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_1547218
_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         'I5 Pb, C3 H7 N O, 3(C H6 N)'
_chemical_formula_sum            'C6 H25 I5 N4 O Pb'
_chemical_formula_weight         1011.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                111.18(3)
_cell_angle_beta                 101.11(3)
_cell_angle_gamma                109.80(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1714(15)
_cell_length_b                   11.335(3)
_cell_length_c                   12.394(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.0
_cell_measurement_theta_min      4.0
_cell_volume                     1170.0(7)
_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 0.893
_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  0.0888
_diffrn_reflns_av_unetI/netI     0.1917
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18171
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.385
_diffrn_reflns_theta_min         3.946
_exptl_absorpt_coefficient_mu    19.169
_exptl_absorpt_correction_T_max  0.120
_exptl_absorpt_correction_T_min  0.060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.870
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         12.269
_refine_diff_density_min         -5.771
_refine_diff_density_rms         0.915
_refine_ls_extinction_coef       0.0031(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   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         4757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.1219
_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^+160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2715
_refine_ls_wR_factor_ref         0.2847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3786
_reflns_number_total             4757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b08468_si_004.cif
_cod_data_source_block           Pb2I5MAH
_cod_depositor_comments
'Adding full bibliography for 1547218--1547220.cif.'
_cod_database_code               1547218
_shelx_estimated_absorpt_t_min   0.156
_shelx_estimated_absorpt_t_max   0.243
_shelxl_version_number           2014/6
_shelx_res_checksum              88290
_shelx_hkl_checksum              29175