Directing the Self-Assembly of Conjugated Organic Ammonium Cations in Low-Dimensional Perovskites by Halide Substitution
Denis, Paul-Henry; Mertens, Martijn; Van Gompel, Wouter T. M.; Van Hecke, Kristof; Ruttens, Bart; D’Haen, Jan; Lutsen, Laurence; Vanderzande, Dirk; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.1c01221

data_4003969
_publ_section_title
;
 Directing the Self-Assembly of Conjugated Organic Ammonium Cations in
 Low-Dimensional Perovskites by Halide Substitution
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.1c01221
_journal_year                    2021
_chemical_formula_moiety         'Cl4 Pb, 2(C11 H14 N S2)'
_chemical_formula_sum            'C22 H28 Cl4 N2 Pb S4'
_chemical_formula_weight         797.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-07-28
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5692(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.7740(5)
_cell_length_b                   7.35765(14)
_cell_length_c                   7.86657(15)
_cell_measurement_reflns_used    10166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7770
_cell_measurement_theta_min      3.5410
_cell_volume                     1433.37(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -66.00  33.00   1.00    5.00    --  -41.68  38.00 -90.00   99
  2  \w   -122.00  -1.00   1.00    5.00    --  -41.68 -19.00  90.00  121
  3  \w    -21.00  74.00   1.00    5.00    --   41.68 -77.00  90.00   95
  4  \w     17.00 116.00   1.00    5.00    --   41.68  38.00 -60.00   99
  5  \w     23.00 107.00   1.00   25.00    --  106.01 -94.00 150.00   84
  6  \w     30.00 134.00   1.00   25.00    --  106.01 -30.00 150.00  104
  7  \w     33.00 112.00   1.00   25.00    --  106.01-125.00 -30.00   79
  8  \w     30.00 139.00   1.00   25.00    --  106.01 -77.00-150.00  109
  9  \w    103.00 178.00   1.00   25.00    --  106.01  77.00-120.00   75
 10  \w     78.00 178.00   1.00   25.00    --  106.01  30.00 -90.00  100
 11  \w     23.00 107.00   1.00   25.00    --  106.01 -94.00  90.00   84
 12  \w     33.00 112.00   1.00   25.00    --  106.01-125.00  60.00   79
 13  \w     23.00 107.00   1.00   25.00    --  106.01 -94.00-180.00   84
 14  \w     78.00 178.00   1.00   25.00    --  106.01  30.00 -30.00  100
 15  \w    102.00 178.00   1.00   25.00    --  106.01  87.00-169.00   76
 16  \w     14.00 115.00   1.00    5.00    --   41.68  57.00 -30.00  101
 17  \w     14.00 115.00   1.00    5.00    --   41.68  57.00 120.00  101
 18  \w     14.00 115.00   1.00    5.00    --   41.68  57.00  30.00  101
 19  \w     27.00  98.00   1.00    5.00    --   41.68-125.00  30.00   71
 20  \w     14.00 115.00   1.00    5.00    --   41.68  57.00-150.00  101
 21  \w     80.00 178.00   1.00   25.00    --  106.01  45.00  60.00   98
 22  \w     77.00 178.00   1.00   25.00    --  106.01  61.00 -90.00  101
 23  \w     78.00 178.00   1.00   25.00    --  106.01  30.00 150.00  100
 24  \w     77.00 178.00   1.00   25.00    --  106.01  61.00-150.00  101
 25  \w     76.00 178.00   1.00   25.00    --  106.01  66.00  84.00  102
 26  \w     77.00 178.00   1.00   25.00    --  106.01  61.00   0.00  101
 27  \w     77.00 178.00   1.00   25.00    --  106.01  61.00 -30.00  101
 28  \w     77.00 178.00   1.00   25.00    --  106.01  61.00 150.00  101
 29  \w     77.00 178.00   1.00   25.00    --  106.01  61.00  60.00  101
 30  \w     77.00 178.00   1.00   25.00    --  106.01  61.00-180.00  101
 31  \w     14.00 115.00   1.00    5.00    --   41.68  57.00-120.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0460969000
_diffrn_orient_matrix_UB_12      -0.1229249000
_diffrn_orient_matrix_UB_13      0.0676212000
_diffrn_orient_matrix_UB_21      0.0137136000
_diffrn_orient_matrix_UB_22      0.1401198000
_diffrn_orient_matrix_UB_23      0.1400003000
_diffrn_orient_matrix_UB_31      -0.0394695000
_diffrn_orient_matrix_UB_32      -0.0954504000
_diffrn_orient_matrix_UB_33      0.1191057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            25920
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.861
_diffrn_reflns_theta_min         3.570
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.718
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.848
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0331P)^2^+2.4221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2396
_reflns_number_total             2878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c01221_si_003.cif
_cod_data_source_block           dvdz019b
_cod_database_code               4003969
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H28 Cl4 N2 Pb S4'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              24950
_shelx_hkl_checksum              79597
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.837
_oxdiff_exptl_absorpt_empirical_full_min 0.409