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_4132392
_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         'I8 Pb2, 4(C13 H16 N O), C4 H6 O2'
_chemical_formula_sum            'C56 H70 I8 N4 O6 Pb2'
_chemical_formula_weight         2324.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                101.0957(19)
_cell_angle_beta                 104.0738(19)
_cell_angle_gamma                90.7065(18)
_cell_formula_units_Z            2
_cell_length_a                   12.4181(3)
_cell_length_b                   12.5652(4)
_cell_length_c                   23.8888(7)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      65.364
_cell_measurement_theta_min      3.705
_cell_volume                     3541.18(18)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      299.11
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37685
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        65.461
_diffrn_reflns_theta_max         65.461
_diffrn_reflns_theta_min         3.591
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    36.869
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1089 before and 0.0636 after correction. The Ratio of minimum to maximum transmission is 0.6331. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.180
_exptl_crystal_description       plate
_exptl_crystal_F_000             2140
_exptl_crystal_recrystallization_method
'Crystals were prepared by dissolving 2:1 Cattion:lead (II) iodide in GBL and vapor diffusion of DCM.'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.355
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         11746
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+3.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8702
_reflns_number_total             11746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b03659_si_003.cif
_cod_data_source_block           3_napthyl_propyl_gbl
_cod_database_code               4132392
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.260
_shelx_estimated_absorpt_t_min   0.043
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C56-C54 \\sim C55-C57
 with sigma of 0.001
 O5-C56 \\sim O5-C55
 with sigma of 0.02
 O5-C54 \\sim O5-C57
 with sigma of 0.02
 C54-C57 \\sim C54-C56
 with sigma of 0.001
 C57-C55 \\sim C57-C54
 with sigma of 0.02
 C38-C37 \\sim C39A-C38 \\sim N3A-C39A \\sim N3-C39 \\sim C39-C38
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 N3, N3A, C37, C38, C39, C39A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, O6, C54, C55, H55A, H55B, C56, H56A, H56B, C57, H57A, H57B
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
4. Others
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H13C)=Sof(H13D)=1-FVAR(1)
 Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(H13A)=Sof(H13B)=FVAR(1)
 Sof(N3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(H38C)=Sof(H38D)=Sof(C39A)=
 Sof(H39C)=Sof(H39D)=1-FVAR(2)
 Sof(N3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C13(H13C,H13D), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C37(H37A,H37B), C38(H38A,H38B),
 C38(H38C,H38D), C39(H39A,H39B), C39A(H39C,H39D), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42), C43(H43),
 C45(H45), C46(H46), C47(H47), C48(H48)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N1A(H1AA,H1AB,H1AC), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C),
 N3A(H3AA,H3AB,H3AC), N4(H4A,H4B,H4C)
;
_shelx_res_checksum              68245
_shelx_hkl_checksum              33312
_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'