Towards 2D layered hybrid perovskites with enhanced functionality: introducing charge-transfer complexes via self-assembly
Van Gompel, Wouter T.M.; Herckens, Roald; Van Hecke, Kristof; Ruttens, Bart; D'Haen, Jan; Lutsen, Laurence; Vanderzande, Dirk; Chemical Communications  (2019) –; doi:10.1039/C8CC09955C

data_7122921
_publ_section_title
;
 Towards 2D layered hybrid perovskites with enhanced functionality:
 introducing charge-transfer complexes via self-assembly
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09955C
_journal_year                    2019
_chemical_formula_moiety         '2(C20 H20 N), I4 Pb'
_chemical_formula_sum            'C40 H40 I4 N2 Pb'
_chemical_formula_weight         1263.54
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-29
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-30 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.6530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.0798(3)
_cell_length_b                   8.70360(10)
_cell_length_c                   8.76250(10)
_cell_measurement_reflns_used    27910
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.6260
_cell_measurement_theta_min      2.8410
_cell_volume                     1910.67(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.946
_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    -36.00  45.00   1.00    5.00    --   10.40 -85.00 -39.00   81
  2  \w    -46.00  15.00   1.00    5.00    --  -11.11  85.00  79.00   61
  3  \w    -36.00  24.00   1.00    5.00    --  -11.11 -85.00 -39.00   60
  4  \w    -18.00  84.00   1.00    5.00    --   10.40  57.00-180.00  102
  5  \w    -20.00  51.00   1.00    5.00    --   10.40 -99.00-180.00   71
  6  \w    -20.00  30.00   1.00    5.00    --  -11.11 -99.00 120.00   50
  7  \w    -20.00  30.00   1.00    5.00    --  -11.11 -99.00-120.00   50
  8  \w    -20.00  30.00   1.00    5.00    --  -11.11 -99.00 150.00   50
  9  \w    -20.00  30.00   1.00    5.00    --  -11.11 -99.00 -90.00   50
 10  \w    -20.00  30.00   1.00    5.00    --  -11.11 -99.00  60.00   50
 11  \w    -65.00 -20.00   1.00    5.00    --  -11.11 121.00-116.09   45
 12  \w    -67.00 -22.00   1.00    5.00    --  -11.11 124.00 135.79   45
 13  \w    -14.00  85.00   1.00    5.00    --   10.40  38.00  90.00   99
 14  \w    -14.00  15.00   1.00    5.00    --   10.40  38.00   0.00   29
 15  \w    -44.00  65.00   1.00    5.00    --  -11.11  77.00  60.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0000198000
_diffrn_orient_matrix_UB_12      0.0671964000
_diffrn_orient_matrix_UB_13      0.0457980000
_diffrn_orient_matrix_UB_21      -0.0233124000
_diffrn_orient_matrix_UB_22      0.0261394000
_diffrn_orient_matrix_UB_23      -0.0409774000
_diffrn_orient_matrix_UB_31      -0.0160649000
_diffrn_orient_matrix_UB_32      -0.0380007000
_diffrn_orient_matrix_UB_33      0.0528032000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            49790
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.712
_diffrn_reflns_theta_min         2.477
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.677
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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 orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.875
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         5140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+1.5610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4814
_reflns_number_total             5140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09955c2.cif
_cod_data_source_block           dvdz001
_cod_database_code               7122921
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C40 H40 I4 N2 Pb'
_shelx_estimated_absorpt_t_max   0.488
_shelx_estimated_absorpt_t_min   0.201
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              66475
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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 1.589
_oxdiff_exptl_absorpt_empirical_full_min 0.779