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_7711442
_publ_section_title
;
 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         'Br0.4 I3.6 Pb, 2(C6 H10 N3 O2)'
_chemical_formula_sum            'C12 H20 Br0.4 I3.6 N6 O4 Pb'
_chemical_formula_weight         1008.33
_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   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2022-08-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-16 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.658(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1236(9)
_cell_length_b                   9.4686(9)
_cell_length_c                   15.3633(19)
_cell_measurement_reflns_used    2234
_cell_measurement_temperature    227(40)
_cell_measurement_theta_max      26.7270
_cell_measurement_theta_min      2.6440
_cell_volume                     1176.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      227(40)
_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 0.870
_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    -56.00  15.00   1.00   50.00    --  -15.29 106.00 -58.00   71
  2  \w     20.00  56.00   1.00   50.00    --   17.71-106.00-157.00   36
  3  \w    -85.00 -40.00   1.00   50.00    --  -15.29-178.00 -30.00   45
  4  \w     -8.00  38.00   1.00   50.00    --  -15.29  77.00-120.00   46
  5  \w    -49.00   0.00   1.00   50.00    --   17.71 -57.00 150.00   49
  6  \w     -9.00  28.00   1.00   50.00    --   17.71  77.00 120.00   37
  7  \w      1.00  79.00   1.00   50.00    --   17.71  38.00-180.00   78
  8  \w     44.00  90.00   1.00   50.00    --   17.71 178.00-150.00   46
  9  \w     39.00  67.00   1.00   50.00    --   17.71 178.00 150.00   28
 10  \w     -9.00  33.00   1.00   50.00    --   17.71  77.00 -60.00   42
 11  \w     -5.00  22.00   1.00   50.00    --   17.71  77.00  90.00   27
;
_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      -0.0360265000
_diffrn_orient_matrix_UB_12      -0.0231292000
_diffrn_orient_matrix_UB_13      0.0377031000
_diffrn_orient_matrix_UB_21      -0.0103560000
_diffrn_orient_matrix_UB_22      -0.0685273000
_diffrn_orient_matrix_UB_23      -0.0183483000
_diffrn_orient_matrix_UB_31      0.0792839000
_diffrn_orient_matrix_UB_32      -0.0195702000
_diffrn_orient_matrix_UB_33      0.0199385000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3232
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.425
_diffrn_reflns_theta_min         2.665
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.848
_exptl_crystal_description       plate
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.007
_refine_diff_density_min         -2.000
_refine_diff_density_rms         0.267
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         3232
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0579P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.788
_reflns_number_gt                2167
_reflns_number_total             3232
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9063\% 
around [0.98 0.00 -0.18] (reciprocal) or [1.00 -0.00 0.00] (direct)
;
_cod_data_source_file            d2dt03025j2.cif
_cod_data_source_block           shi_5959_ilgu_twin1_hklf4
_cod_original_formula_sum        'C12 H20 Br0.40 I3.60 N6 O4 Pb'
_cod_database_code               7711442
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C11H22I4N6O6Pb
_chemical_oxdiff_usercomment     SV_383
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.338
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.60112
 0.39888
2. Shared sites
{I1, Br1}
{I2, Br2}
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(I2) = Uanis(Br2)
Uanis(I1) = Uanis(Br1)
5. Others
 Fixed Sof: I2(0.9) I1(0.9) Br2(0.1) Br1(0.1)
6.a Ternary CH refined with riding coordinates:
 C2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), N2(H2A), C6(H6)
6.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
6.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              75375
_shelx_hkl_checksum              42346
_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 1.635
_oxdiff_exptl_absorpt_empirical_full_min 0.665
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2