Crystal Structure of DMF-Intermediate Phases Uncovers the Link Between CH3NH3PbI3 Morphology and Precursor Stoichiometry
Petrov, Andrey A.; Sokolova, Iuliia P.; Belich, Nikolai A.; Peters, Georgy S.; Dorovatovskii, Pavel V.; Zubavichus, Yan V.; Khrustalev, Victor N.; Petrov, Andrey V.; Grätzel, Michael; Goodilin, Eugene A.; Tarasov, Alexey B.; The Journal of Physical Chemistry C 121 (2017) 20739–; doi:10.1021/acs.jpcc.7b08468

data_1547220
_publ_section_title
;
 Crystal Structure of DMF-Intermediate Phases Uncovers the Link Between
 CH3NH3PbI3 Morphology and Precursor Stoichiometry
;
_journal_issue                   38
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              20739
_journal_paper_doi               10.1021/acs.jpcc.7b08468
_journal_volume                  121
_journal_year                    2017
_chemical_formula_moiety         'I3 Pb, C3 H7 N O, C H6 N'
_chemical_formula_sum            'C4 H13 I3 N2 O Pb'
_chemical_formula_weight         693.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 96.75(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.5647(9)
_cell_length_b                   25.446(5)
_cell_length_c                   12.119(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0
_cell_measurement_theta_min      3.0
_cell_volume                     1397.9(5)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
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_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.964
_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  0.0862
_diffrn_reflns_av_unetI/netI     0.1977
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.964
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_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12672
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.371
_diffrn_reflns_theta_min         3.180
_exptl_absorpt_coefficient_mu    21.964
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.293
_exptl_crystal_description       needle
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.20
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_exptl_crystal_size_min          0.01
_refine_diff_density_max         7.387
_refine_diff_density_min         -5.418
_refine_diff_density_rms         0.856
_refine_ls_extinction_coef       0.00042(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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         2953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.1036
_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^)+(0.01P)^2^+100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2260
_refine_ls_wR_factor_ref         0.2459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2142
_reflns_number_total             2953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b08468_si_003.cif
_cod_data_source_block           Phase-II
_cod_depositor_comments
'Adding full bibliography for 1547218--1547220.cif.'
_cod_database_code               1547220
_shelx_estimated_absorpt_t_min   0.094
_shelx_estimated_absorpt_t_max   0.807
_shelxl_version_number           2014/6
_shelx_res_checksum              37111
_shelx_hkl_checksum              48854