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_4003672
_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_absolute_configuration ad
_chemical_formula_moiety         '15(C H5 N2), 3(I9 Pb2)'
_chemical_formula_sum            'C15 H75 I27 N30 Pb6'
_chemical_formula_weight         5345.55
_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_Hall           'P -6'
_space_group_name_H-M_alt        'P -6'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   26.770(3)
_cell_length_b                   26.770(3)
_cell_length_c                   14.860(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      3.3
_cell_volume                     9222.4(19)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1030
_diffrn_reflns_av_unetI/netI     0.1019
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            79929
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.867
_diffrn_reflns_theta_min         3.251
_exptl_absorpt_coefficient_mu    18.942
_exptl_absorpt_correction_T_max  0.555
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.888
_exptl_crystal_description       prism
_exptl_crystal_F_000             6894
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.532
_refine_diff_density_min         -3.757
_refine_diff_density_rms         0.404
_refine_ls_abs_structure_details
;
 Flack x determined using 3773 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.012(6)
_refine_ls_extinction_coef       0.00014(3)
_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   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         13829
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.1230
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2654
_refine_ls_wR_factor_ref         0.2866
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                10126
_reflns_number_total             13829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c02156_si_003.cif
_cod_data_source_block           FA5Pb2I9
_cod_original_cell_volume        9222(3)
_cod_database_code               4003672
_shelx_estimated_absorpt_t_min   0.251
_shelx_estimated_absorpt_t_max   0.598
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2013-4
_shelx_res_checksum              19005
_shelx_hkl_checksum              94130