Guanidinium-Formamidinium Lead Iodide: A Layered Perovskite-Related Compound with Red Luminescence at Room Temperature.
Nazarenko, Olga; Kotyrba, Martin R.; Yakunin, Sergii; Aebli, Marcel; Rainò, Gabriele; Benin, Bogdan M.; Wörle, Michael; Kovalenko, Maksym V.; Journal of the American Chemical Society 140 (2018) 3850–3853; doi:10.1021/jacs.8b00194

data_4132015
_publ_section_title
;
 Guanidinium-Formamidinium Lead Iodide: A Layered Perovskite-Related
 Compound with Red Luminescence at Room Temperature.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3850
_journal_page_last               3853
_journal_paper_doi               10.1021/jacs.8b00194
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.17(I24 Pb6), C H6 N3, 0.5(C2 H10 N4)'
_chemical_formula_sum            'C2 H11 I4 N5 Pb'
_chemical_formula_weight         819.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.9408(14)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   26.948(2)
_cell_length_b                   12.8189(11)
_cell_length_c                   14.4080(12)
_cell_measurement_reflns_used    5067
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.172
_cell_measurement_theta_min      2.549
_cell_volume                     4678.8(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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      298
_diffrn_detector                 'Bruker SMART CCD 1K area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21673
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         1.503
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.710
_exptl_absorpt_correction_T_max  0.1924
_exptl_absorpt_correction_T_min  0.0707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1431 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.3883. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.492
_exptl_crystal_description       needle
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.848
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         5009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+60.4763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3914
_reflns_number_total             5009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00194_si_001.cif
_cod_data_source_block           c2m_cor_1_3
_cod_original_cell_volume        4678.7(7)
_cod_database_code               4132015
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(N9) = Uiso(N9) = Uiso(N8) = Uiso(N8) = Uiso(N7) = Uiso(N7) = Uiso(C4) =
Uiso(C4)
Uiso(N12) = Uiso(C5) = Uiso(N11) = Uiso(N10)
Uiso(N13) = Uiso(N15) = Uiso(N14) = Uiso(N16)
Uiso(C6) = Uiso(C7)
3. Others
 Sof(N15)=Sof(H15A)=Sof(H15B)=Sof(N16)=Sof(H16A)=Sof(H16B)=Sof(C7)=Sof(H7)=0.5*
 (1-FVAR(2))
 Sof(N14)=Sof(H14A)=Sof(H14B)=Sof(C6)=Sof(H6)=Sof(N13)=Sof(H13A)=Sof(H13B)=0.5*
 FVAR(2)
 Fixed Sof: N9(0.5) H9A(0.5) H9B(0.5) N7(0.5) H7A(0.5) H7B(0.5) N8(0.5)
 H8A(0.5) H8B(0.5) C4(0.5) H5A(0.5) H5B(0.5) N3(0.5) H3A(0.5) H3B(0.5) N4(0.5)
 H4A(0.5) H4B(0.5) C2(0.5) H2(0.5) N1(0.5) H1A(0.5) H1B(0.5) N2(0.5) H2A(0.5)
 H2B(0.5) C1(0.5) H1(0.5) N12(0.5) H12A(0.5) H12B(0.5) N10(0.5) H10A(0.5)
 H10B(0.5) N11(0.5) H11A(0.5) H11B(0.5) C5(0.5)
4.a Free rotating group:
 N9(N7,N8,C4), N14(C6,N13), N3(N4,C2), N1(N2,C1), N12(N10,N11,C5), N15(N16,C7)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C1(H1), C7(H7)
4.c X=CH2 refined with riding coordinates:
 N9(H9A,H9B), N7(H7A,H7B), N8(H8A,H8B), N14(H14A,H14B), N13(H13A,H13B), N5(H5A,
 H5B), N6(H6A,H6B), N3(H3A,H3B), N4(H4A,H4B), N1(H1A,H1B), N2(H2A,H2B),
 N12(H12A,H12B), N10(H10A,H10B), N11(H11A,H11B), N15(H15A,H15B), N16(H16A,H16B)
;
_shelx_res_checksum              86090
_shelx_hkl_checksum              85337
_olex2_submission_special_instructions 'No special instructions were received'