Disentangling Second Harmonic Generation from Multiphoton Photoluminescence in Halide Perovskites using Multidimensional Harmonic Generation.
Morrow, Darien J.; Hautzinger, Matthew P.; Lafayette, David P.; Scheeler, Jason M.; Dang, Lianna; Leng, Meiying; Kohler, Daniel D.; Wheaton, Amelia M.; Fu, Yongping; Guzei, Ilia A.; Tang, Jiang; Jin, Song; Wright, John C.; The journal of physical chemistry letters  (2020) 6551–6559; doi:10.1021/acs.jpclett.0c01720

data_8000447
_publ_section_title
;
 Disentangling Second Harmonic Generation from Multiphoton
 Photoluminescence in Halide Perovskites using Multidimensional Harmonic
 Generation.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              6551
_journal_page_last               6559
_journal_paper_doi               10.1021/acs.jpclett.0c01720
_journal_year                    2020
_chemical_formula_moiety         'I7 Pb2, 2(C8 H12 N), C H6 N'
_chemical_formula_sum            'C17 H30 I7 N3 Pb2'
_chemical_formula_weight         1579.12
_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     dual
_audit_creation_date             2019-12-20
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                97.604(16)
_cell_angle_beta                 93.482(11)
_cell_angle_gamma                90.36(2)
_cell_formula_units_Z            2
_cell_length_a                   8.722(3)
_cell_length_b                   8.726(3)
_cell_length_c                   22.533(8)
_cell_measurement_reflns_used    3582
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      30.895
_cell_measurement_theta_min      2.741
_cell_volume                     1696.5(10)
_computing_cell_refinement       'APEX3 Ver. 2018.7-2 (Bruker-AXS, 2018)'
_computing_data_collection       'APEX3 Ver. 2018.7-2 (Bruker-AXS, 2018)'
_computing_data_reduction        'APEX3 Ver. 2018.7-2 (Bruker-AXS, 2018)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_unetI/netI     0.1148
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35179
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.544
_diffrn_reflns_theta_min         1.827
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    16.290
_exptl_absorpt_correction_T_max  0.5143
_exptl_absorpt_correction_T_min  0.4481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1528 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.8713.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.870
_refine_diff_density_min         -4.219
_refine_diff_density_rms         0.424
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         11201
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0052P)^2^+37.1770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6636
_reflns_number_total             11201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz0c01720_si_002.cif
_cod_data_source_block           jin87
_cod_depositor_comments          'Adding full bibliography for 8000447.cif.'
_cod_original_cell_volume        1696.6(10)
_cod_database_code               8000447
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.641
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-N3 = C17A-N3A
 1.525 with sigma of 0.01
 N1-C7 = N1A-C7A
 2.5271 with sigma of 0.01
 N1-C8 = N1A-C8A = C16-N2
 1.5373 with sigma of 0.01
 C7-C8 = C7A-C8A
 1.5294 with sigma of 0.01
 C9-C15
 1.519 with sigma of 0.02
 C16-C15 \\sim C16-C15A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C17) = Uiso(N3) = Uiso(C17A) = Uiso(N3A)
Uanis(I2A) = Uanis(I4)
Uanis(I2) = Uanis(I4A)
Uanis(I3) = Uanis(I5A)
Uanis(I5) = Uanis(I3A)
Uiso(C1) = Uiso(C2) = Uiso(C3) = Uiso(C4) = Uiso(C5) = Uiso(C6) = Uiso(C7) =
Uiso(C8) = Uiso(N1)
Uiso(C1A) = Uiso(C2A) = Uiso(C3A) = Uiso(C4A) = Uiso(C5A) = Uiso(C6A) =
Uiso(C7A) = Uiso(C8A) = Uiso(N1A)
Uiso(C9) = Uiso(C10) = Uiso(C11) = Uiso(C12) = Uiso(C13) = Uiso(C14) = Uiso(C15)
Uiso(C9A) = Uiso(C10A) = Uiso(C11A) = Uiso(C12A) = Uiso(C13A) = Uiso(C14A) =
Uiso(C15A)
Uiso(C16) = Uiso(N2)
4. Others
 Sof(I2A)=Sof(I3A)=Sof(I4A)=Sof(I5A)=1-FVAR(1)
 Sof(I2)=Sof(I3)=Sof(I4)=Sof(I5)=FVAR(1)
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 C1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5)
 C6(0.5) H6(0.5) C7(0.5) H7A(0.5) H7B(0.5) N1A(0.5) H1AA(0.5) H1AB(0.5)
 H1AC(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) C1A(0.5)
 C2A(0.5) H2AA(0.5) C3A(0.5) H3A(0.5) C4A(0.5) H4A(0.5) C5A(0.5) H5A(0.5)
 C6A(0.5) H6A(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H16D(0.5) C15(0.5) H15A(0.5)
 H15B(0.5) C9(0.5) C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5)
 C13(0.5) H13(0.5) C14(0.5) H14(0.5) C9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5)
 H11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5) H13A(0.5) C14A(0.5) H14A(0.5)
 C15A(0.5) H15C(0.5) H15D(0.5) N3(0.5) H3B(0.5) H3C(0.5) H3D(0.5) C17(0.5)
 H17A(0.5) H17B(0.5) H17C(0.5) N3A(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C17A(0.5)
 H17D(0.5) H17E(0.5) H17F(0.5)
5.a Free rotating group:
 C1(C2,C3,C4,C5,C6,C7), C7A(C1A,C2A,C3A,C4A,C5A,C6A), C9(C10,C11,C12,C13,C14),
 C9A(C10A,C11A,C12A,C13A,C14A,C15A)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C8A(H8AA,H8AB), C7A(H7AA,H7AB), C16(H16A,H16B),
 C16(H16C,H16D), C15(H15A,H15B), C15A(H15C,H15D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C2A(H2AA), C3A(H3A), C4A(H4A),
 C5A(H5A), C6A(H6A), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A)
5.d Idealised Me refined with riding coordinates:
 N3A(H3AA,H3AB,H3AC), C17A(H17D,H17E,H17F)
5.e Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N1A(H1AA,H1AB,H1AC), N2(H2A,H2B,H2C), N3(H3B,H3C,H3D),
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              32768
_shelx_hkl_checksum              97529
_olex2_submission_special_instructions 'No special instructions were received'