Formamidinium Haloplumbate Intermediates: The Missing Link in a Chain of Hybrid Perovskites Crystallization
Petrov, Andrey A.; Fateev, Sergey A.; Khrustalev, Victor N.; Li, Yumao; Dorovatovskii, Pavel V.; Zubavichus, Yan V.; Goodilin, Eugene A.; Tarasov, Alexey B.; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c02156

data_4003670
_publ_section_title
;
 Formamidinium Haloplumbate Intermediates: The Missing Link in a Chain of
 Hybrid Perovskites Crystallization
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c02156
_journal_year                    2020
_chemical_formula_moiety         'I3 Pb, 2(C3 H7 N O), C H5 N2'
_chemical_formula_sum            'C7 H19 I3 N4 O2 Pb'
_chemical_formula_weight         779.16
_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     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                75.92(3)
_cell_angle_beta                 75.11(3)
_cell_angle_gamma                68.82(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8788(16)
_cell_length_b                   10.497(2)
_cell_length_c                   12.678(3)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      3.2
_cell_volume                     931.6(4)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80246
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_unetI/netI     0.1101
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15000
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.865
_diffrn_reflns_theta_min         3.187
_exptl_absorpt_coefficient_mu    17.453
_exptl_absorpt_correction_T_max  0.560
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.778
_exptl_crystal_description       needle
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.934
_refine_diff_density_min         -3.490
_refine_diff_density_rms         0.370
_refine_ls_extinction_coef       0.0052(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         4035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0559P)^2^+5P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3570
_reflns_number_total             4035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c02156_si_004.cif
_cod_data_source_block           FAPbI_DMF1
_cod_database_code               4003670
_shelx_estimated_absorpt_t_min   0.178
_shelx_estimated_absorpt_t_max   0.621
_shelxl_version_number           2013-4
_shelx_res_checksum              89903
_shelx_hkl_checksum              91189