Solution Processing of Methylammonium Lead Iodide Perovskite from γ-Butyrolactone: Crystallization Mediated by Solvation Equilibrium
Fateev, Sergey A.; Petrov, Andrey A.; Khrustalev, Victor N.; Dorovatovskii, Pavel V.; Zubavichus, Yan V.; Goodilin, Eugene A.; Tarasov, Alexey B.; Chemistry of Materials 30 (2018) 5237–; doi:10.1021/acs.chemmater.8b01906

data_4003375
_publ_section_title
;
 Solution Processing of Methylammonium Lead Iodide Perovskite from
 \g-Butyrolactone: Crystallization Mediated by Solvation Equilibrium
;
_journal_issue                   15
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5237
_journal_paper_doi               10.1021/acs.chemmater.8b01906
_journal_volume                  30
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'I44 Pb18, (C4 H6 O2)x, (C H6 N)y'
_chemical_formula_sum            'I75 Pb50'
_chemical_formula_weight         19875.41
_space_group_crystal_system      cubic
_space_group_IT_number           215
_space_group_name_Hall           'P -4 2 3'
_space_group_name_H-M_alt        'P -4 3 m'
_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                90
_cell_formula_units_Z            1
_cell_length_a                   23.290(3)
_cell_length_b                   23.290(3)
_cell_length_c                   23.290(3)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.9
_cell_measurement_theta_min      3.9
_cell_volume                     12633(3)
_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 0.977
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.2179
_diffrn_reflns_av_unetI/netI     0.1641
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45340
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.428
_diffrn_reflns_theta_min         3.775
_exptl_absorpt_coefficient_mu    19.723
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.613
_exptl_crystal_description       prism
_exptl_crystal_F_000             8075
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         6.678
_refine_diff_density_min         -2.359
_refine_diff_density_rms         0.372
_refine_ls_abs_structure_details
;
 Flack x determined using 600 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.4(4)
_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   0.972
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         4982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.2553
_refine_ls_R_factor_gt           0.1475
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2963
_refine_ls_wR_factor_ref         0.3698
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                2092
_reflns_number_total             4982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b01906_si_004.cif
_cod_data_source_block           framework
_cod_original_cell_volume        12633(4)
_cod_database_code               4003375
_shelx_estimated_absorpt_t_min   0.439
_shelx_estimated_absorpt_t_max   0.439
_shelxl_version_number           2013-4
_shelx_res_checksum              51509
_shelx_hkl_checksum              84356