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_7711440
_publ_section_title
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 Chiral 2D organic-inorganic hybrid perovskites based upon L-histidine
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03025J
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         'I4 Pb, 2(C6 H10 N3 O2), H0.44 O0.22'
_chemical_formula_sum            'C12 H20.44 I4 N6 O4.22 Pb'
_chemical_formula_weight         1031.09
_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     dual
_audit_creation_date             2022-08-22
_audit_creation_method
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Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
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_audit_update_record
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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                   8.3053(15)
_cell_length_b                   9.5330(18)
_cell_length_c                   30.667(6)
_cell_measurement_reflns_used    1352
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8380
_cell_measurement_theta_min      2.6240
_cell_volume                     2428.0(8)
_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(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 0.855
_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    -42.00  14.00   1.00  100.00    --  -15.13 107.00   5.00   56
  2  \w      8.00  86.00   1.00  100.00    --   17.71  28.00 167.00   78
  3  \w     -8.00  54.00   1.00  100.00    --   17.71 -99.00   0.00   62
  4  \w     -2.00  37.00   1.00  100.00    --   17.71  77.00-120.00   39
;
_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      0.0602789000
_diffrn_orient_matrix_UB_12      0.0526138000
_diffrn_orient_matrix_UB_13      0.0010323000
_diffrn_orient_matrix_UB_21      0.0554602000
_diffrn_orient_matrix_UB_22      -0.0496076000
_diffrn_orient_matrix_UB_23      0.0084676000
_diffrn_orient_matrix_UB_31      0.0248047000
_diffrn_orient_matrix_UB_32      -0.0170540000
_diffrn_orient_matrix_UB_33      -0.0214891000
_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  0.0649
_diffrn_reflns_av_unetI/netI     0.1008
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            6398
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.448
_diffrn_reflns_theta_min         2.657
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.063
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64977
_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 light red'
_exptl_crystal_density_diffrn    2.821
_exptl_crystal_description       prism
_exptl_crystal_F_000             1849
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.248
_refine_ls_abs_structure_details
;
 Flack x determined using 503 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2787
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0524
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.706
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.787
_reflns_number_gt                1752
_reflns_number_total             2787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03025j2.cif
_cod_data_source_block           shi_5165_ilgu_autored
_cod_database_code               7711440
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H10N2O4Pb1I2
_chemical_oxdiff_usercomment     SV354
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.644
_olex2_refinement_description
;
1. Restrained distances
 C6-C4 = N3-C6 = N3-C5 = N2-C5 = N2-C4
 1.35 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) = Uanis(N2) = Uanis(C5) = Uanis(N3) = Uanis(C6)
3. Others
 Fixed Sof: O3(0.11) H3C(0.22)
4.a Riding coordinates:
 O1(H1), O3(H3C)
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:
 N3(H3), C5(H5), C6(H6)
4.e Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              2096
_shelx_hkl_checksum              44370
_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 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.760