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_4132394
_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(C19 H18 N O)'
_chemical_formula_sum            'C38 H36 I4 N2 O2 Pb'
_chemical_formula_weight         1267.48
_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
_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                 94.9453(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   49.3776(13)
_cell_length_b                   8.4890(2)
_cell_length_c                   9.4480(2)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      29.662
_cell_measurement_theta_min      2.484
_cell_volume                     3945.54(16)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      299.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            71859
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.714
_diffrn_reflns_theta_min         2.164
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.440
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1363 before and 0.0711 after correction. The Ratio of minimum to maximum transmission is 0.6935. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          1.607
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 4635 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0008(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         11170
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0407P)^2^+2.0939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9978
_reflns_number_total             11170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b03659_si_005.cif
_cod_data_source_block           5_pyrenepropylcorrectres
_cod_database_code               4132394
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.029
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.595(4)
 0.405(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 C7-C10 \\sim C8-C11 \\sim C16-C9
 with sigma of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B)
4.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),
 C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C31(H31),
  C32(H32)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              29583
_shelx_hkl_checksum              16709
_olex2_submission_special_instructions 'No special instructions were received'