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_4132395
_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(C18 H16 N O)'
_chemical_formula_sum            'C36 H32 I4 N2 O2 Pb'
_chemical_formula_weight         1239.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                90
_cell_angle_beta                 95.8609(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.4275(3)
_cell_length_b                   12.4001(3)
_cell_length_c                   48.3600(12)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    299
_cell_measurement_theta_max      65.023
_cell_measurement_theta_min      5.518
_cell_volume                     7413.4(3)
_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
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0885
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            29932
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        65.093
_diffrn_reflns_theta_max         65.093
_diffrn_reflns_theta_min         4.596
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    35.267
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1017 before and 0.0697 after correction. The Ratio of minimum to maximum transmission is 0.6496. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.221
_exptl_crystal_description       plate
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.481
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.232
_refine_ls_abs_structure_details
;
 Flack x determined using 2796 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         10598
_refine_ls_number_restraints     602
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0509P)^2^+294.9844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1812
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                9014
_reflns_number_total             10598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b03659_si_004.cif
_cod_data_source_block           4_pyrene_ethyl
_cod_database_code               4132395
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.355
_shelx_estimated_absorpt_t_min   0.097
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.67(3)
 0.33(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C54) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C72) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49, C50, C51, C52
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C55, C56, C57, C58, C59, C60, C61, C62, C63, C64, C65, C66, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C71, C72
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C18, C53, C54
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C35(H35A,H35B), C36(H36A,H36B), C53(H53A,
 H53B), C54(H54A,H54B), C71(H71A,H71B), C72(H72A,H72B)
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),
 C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C30(H30),
  C31(H31), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45),
 C46(H46), C48(H48), C49(H49), C56(H56), C57(H57), C59(H59), C60(H60), C62(H62),
  C63(H63), C64(H64), C66(H66), C67(H67)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C)
;
_shelx_res_checksum              31524
_shelx_hkl_checksum              87812
_olex2_submission_special_instructions 'No special instructions were received'