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_4003376
_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_formula_moiety         'I8 Pb3, C4 H6 O2, 2(C H6 N)'
_chemical_formula_sum            'C6 H18 I8 N2 O2 Pb3'
_chemical_formula_weight         1787.02
_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   difmap
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 101.80(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.822(4)
_cell_length_b                   4.5979(9)
_cell_length_c                   16.653(3)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.0
_cell_volume                     1635.6(6)
_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 0.980
_diffrn_measured_fraction_theta_max 0.951
_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  0.0886
_diffrn_reflns_av_unetI/netI     0.1958
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7812
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.348
_diffrn_reflns_theta_min         1.705
_exptl_absorpt_coefficient_mu    25.955
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.629
_exptl_crystal_description       needle
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.890
_refine_diff_density_min         -3.734
_refine_diff_density_rms         0.559
_refine_ls_extinction_coef       0.00026(2)
_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   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1923
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0862
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1989
_refine_ls_wR_factor_ref         0.2224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1273
_reflns_number_total             1923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b01906_si_002.cif
_cod_data_source_block           igla1
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4003376
_shelx_estimated_absorpt_t_min   0.072
_shelx_estimated_absorpt_t_max   0.779
_shelxl_version_number           2014/6
_shelx_res_checksum              42093
_shelx_hkl_checksum              58075