Resolving Rotational Stacking Disorder and Electronic Level Alignment in a 2D Oligothiophene-Based Lead Iodide Perovskite
Jana, Manoj K.; Liu, Chi; Lidin, Sven; Dirkes, David J.; You, Wei; Blum, Volker; Mitzi, David B.; Chemistry of Materials 31 (2019) 8523–; doi:10.1021/acs.chemmater.9b03208

data_4003005
_publ_section_title
;
 Resolving Rotational Stacking Disorder and Electronic Level Alignment in
 a 2D Oligothiophene-Based Lead Iodide Perovskite
;
_journal_issue                   20
_journal_name_full               'Chemistry of Materials'
_journal_page_first              8523
_journal_paper_doi               10.1021/acs.chemmater.9b03208
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         '0.5(I8 Pb2), C12 H18 N2 S2'
_chemical_formula_sum            'C12 H18 I4 N2 Pb S2'
_chemical_formula_weight         969.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7847(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.7184(13)
_cell_length_b                   6.1756(3)
_cell_length_c                   12.2470(5)
_cell_measurement_reflns_used    9091
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      3.33
_cell_volume                     2245.02(17)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2289
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.399
_diffrn_reflns_theta_min         3.744
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.198
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.5
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.867
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.081
_refine_diff_density_max         5.229
_refine_diff_density_min         -3.662
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2289
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1029P)^2^+43.6952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2025
_refine_ls_wR_factor_ref         0.2168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1415
_reflns_number_total             2289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b03208_si_002.cif
_cod_data_source_block           AE2TbI4
_cod_database_code               4003005
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.414
_shelx_estimated_absorpt_t_min   0.104
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.727(13)
 0.273(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
3. Rigid body (RIGU) restrains
 C9, S1, C7, C8, C15, C16, C18, C20, C10, C19, C11, C17, N6, N9, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: I3(0.25) I4(0.25) I5(0.5) C7(0.5) C8(0.5) H9BC(0.5) H9BD(0.5)
 H9AA(0.5) H9AB(0.5) C10(0.5) H10(0.5) C11(0.5) H11(0.5) C15(0.5) C16(0.5)
 C17(0.5) H17A(0.5) H17B(0.5) C18(0.5) H18(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 C20(0.5) H20(0.5) N6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) N9(0.25) H9A(0.25)
 H9B(0.25) H9C(0.25) N10(0.25) H10A(0.25) H10B(0.25) H10C(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9BC,H9BD), C9(H9AA,H9AB), C17(H17A,H17B), C19(H19A,H19B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C18(H18), C20(H20)
5.c Idealised Me refined as rotating group:
 N6(H6A,H6B,H6C), N9(H9A,H9B,H9C), N10(H10A,H10B,H10C)
;
_shelx_res_checksum              10862
_shelx_hkl_checksum              11101
_olex2_submission_original_sample_id '[AE2T]PbI4'
_olex2_submission_special_instructions 'No special instructions were received'