Enhanced Out-of-Plane Conductivity and Photovoltaic Performance in n = 1 Layered Perovskites through Organic Cation Design.
Passarelli, James V.; Fairfield, Daniel J.; Sather, Nicholas A.; Hendricks, Mark P.; Sai, Hiroaki; Stern, Charlotte L.; Stupp, Samuel I.; Journal of the American Chemical Society 140 (2018) 7313–7323; doi:10.1021/jacs.8b03659

data_4132397
_publ_section_title
;
 Enhanced Out-of-Plane Conductivity and Photovoltaic Performance in n = 1
 Layered Perovskites through Organic Cation Design.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7313
_journal_page_last               7323
_journal_paper_doi               10.1021/jacs.8b03659
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'I4 Pb, 2(C20 H20 N O)'
_chemical_formula_sum            'C40 H40 I4 N2 O2 Pb'
_chemical_formula_weight         1295.53
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.318(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   53.3048(16)
_cell_length_b                   6.1727(2)
_cell_length_c                   12.5651(4)
_cell_measurement_reflns_used    4266
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      65.079
_cell_measurement_theta_min      7.048
_cell_volume                     4134.3(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      299.18
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14074
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        65.194
_diffrn_reflns_theta_max         65.194
_diffrn_reflns_theta_min         7.048
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    31.655
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1393 before and 0.0723 after correction. The Ratio of minimum to maximum transmission is 0.5385. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_description       plate
_exptl_crystal_F_000             2416
_exptl_crystal_preparation
'Crystals were prepared by dissolving 2:1 Cattion:lead (II) iodide in GBL and vapor diffusion of DCM.'
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.445
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3425
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+17.9666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2234
_reflns_number_total             3425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b03659_si_006.cif
_cod_data_source_block           6_pyrene_butyl
_cod_database_code               4132397
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.450
_shelx_estimated_absorpt_t_min   0.040
_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. Restrained distances
 N1-C20 \\sim C20-C19 \\sim C18-C19
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: I2(0.5) I3(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
5.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)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              14307
_shelx_hkl_checksum              28719
_olex2_exptl_crystal_mounting_method
'Crystals were mounted onto a kapton loop using grease to secure crystals.'
_olex2_submission_special_instructions 'No special instructions were received'