(4NPEA)<sub>2</sub>PbI<sub>4</sub> (4NPEA = 4-Nitrophenylethylammonium): Structural, NMR, and Optical Properties of a 3 ×3 Corrugated 2D Hybrid Perovskite.
Tremblay, Marie-Hélène; Thouin, Félix; Leisen, Johannes; Bacsa, John; Srimath Kandada, Ajay Ram; Hoffman, Justin M.; Kanatzidis, Mercouri G.; Mohite, Aditya D.; Silva, Carlos; Barlow, Stephen; Marder, Seth R.; Journal of the American Chemical Society 141 (2019) 4521–4525; doi:10.1021/jacs.8b13207

data_4128938
_publ_section_title
;
 (4NPEA)<sub>2</sub>PbI<sub>4</sub> (4NPEA = 4-Nitrophenylethylammonium):
 Structural, NMR, and Optical Properties of a 3 \\times 3 Corrugated 2D
 Hybrid Perovskite.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4521
_journal_page_last               4525
_journal_paper_doi               10.1021/jacs.8b13207
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.13(Br32 Pb8), 2(C8 H11 N2 O2)'
_chemical_formula_sum            'C16 H22 Br4 N4 O4 Pb'
_chemical_formula_weight         861.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-20
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.290(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2912(5)
_cell_length_b                   19.4228(4)
_cell_length_c                   11.7888(3)
_cell_measurement_reflns_used    33711
_cell_measurement_temperature    108(6)
_cell_measurement_theta_max      37.9870
_cell_measurement_theta_min      1.9130
_cell_volume                     4835.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      108(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w      1.00  68.00   0.50   14.72    --   25.84-112.00 150.00  134
  2  \w     53.00  91.00   0.50   14.72    --   25.84-178.00 -60.00   76
  3  \w     35.00  60.00   0.50   14.72    --   25.84 -99.00-180.00   50
  4  \w    -15.00  20.00   0.50   14.72    --   25.84 -99.00-180.00   70
  5  \w     48.00  98.00   0.50   14.72    --   25.84  77.00 -60.00  100
  6  \w     39.00  98.00   0.50   14.72    --   25.84 178.00  90.00  118
  7  \w     45.00  71.00   0.50   14.72    --   25.84 178.00 120.00   52
  8  \w     49.00  84.00   0.50   14.72    --   25.84 178.00  60.00   70
  9  \w      2.00  99.00   0.50   14.72    --   25.84  77.00-120.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0008640000
_diffrn_orient_matrix_UB_12      -0.0342711000
_diffrn_orient_matrix_UB_13      -0.0205109000
_diffrn_orient_matrix_UB_21      0.0165460000
_diffrn_orient_matrix_UB_22      -0.0105320000
_diffrn_orient_matrix_UB_23      0.0531811000
_diffrn_orient_matrix_UB_31      -0.0292376000
_diffrn_orient_matrix_UB_32      -0.0069766000
_diffrn_orient_matrix_UB_33      0.0205940000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            84119
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.061
_diffrn_reflns_theta_min         2.646
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.616
_exptl_absorpt_correction_T_max  0.520
_exptl_absorpt_correction_T_min  0.068
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             3200
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by ---'
_exptl_crystal_size_max          0.299
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.434
_refine_diff_density_min         -2.253
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         24781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+6.9630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18256
_reflns_number_total             24781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13207_si_003.cif
_cod_data_source_block           mht-iv-49-i_2
_cod_original_cell_volume        4835.70(19)
_cod_database_code               4128938
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C128  H176  Br32  N32  O32  Pb8  '
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2DA,H2DB,H2DC} of N2D, All C(H,H) groups
 At 1.5 times of:
  {H2CB,H2CC,H2CD} of N2C, {H2A,H2B,H2C} of N2, {H2BB,H2BC,H2BD} of N2B
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C7B(H7BA,H7BB), C8B(H8BA,H8BB), C7C(H7CA,H7CB),
 C8C(H8CA,H8CB), C7D(H7DA,H7DB), C8D(H8DA,H8DB)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C2B(H2BA), C3B(H3B), C5B(H5B), C6B(H6B),
 C2C(H2CA), C3C(H3C), C5C(H5C), C6C(H6C), C2D(H2D), C3D(H3D), C5D(H5D), C6D(H6D)
2.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N2B(H2BB,H2BC,H2BD), N2C(H2CB,H2CC,H2CD), N2D(H2DA,H2DB,H2DC)
;
_shelx_res_checksum              45629
_shelx_hkl_checksum              70516
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a None'
_olex2_submission_original_sample_id MHT-IV-49-I
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.364
_oxdiff_exptl_absorpt_empirical_full_min 0.750
_oxdiff_exptl_absorpt_spherical_max 0.216
_oxdiff_exptl_absorpt_spherical_min 0.179