Solid state transformation of the crystalline monohydrate (CH3NH3)PbI3(H2O) to the (CH3NH3)PbI3 perovskite
Gregory H. Imler; Xia Li; Bolei Xu; Graham E. Dobereiner; Hai-Lung Dai; Yi Rao; Bradford B. Wayland; Chem.Commun. 51 (2015) 11290–; doi:10.1039/C5cc03741G

data_7117405
_publ_section_title
;
 Solid state transformation of the crystalline monohydrate
 (CH3NH3)PbI3(H2O) to the (CH3NH3)PbI3 perovskite
;
_journal_name_full               Chem.Commun.
_journal_page_first              11290
_journal_paper_doi               10.1039/C5cc03741G
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C H8 I3 N O Pb'
_chemical_formula_sum            'C H8 I3 N O Pb'
_chemical_formula_weight         637.97
_chemical_melting_point          ?
_chemical_name_systematic        'Methylammonium Lead Triiodide Hydrate'
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-08 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.251(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.469(2)
_cell_length_b                   4.6557(9)
_cell_length_c                   11.214(2)
_cell_measurement_reflns_used    5416
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.007
_cell_measurement_theta_min      2.436
_cell_volume                     536.07(17)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       COSMO
_computing_data_reduction        'SADABS (Bruker-AXS)'
_computing_molecular_graphics    XP
_computing_publication_material  'APEX2 report generator (Bruker-AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Kappa APEX II DUO'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6477
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    24.311
_exptl_absorpt_correction_T_max  0.1214
_exptl_absorpt_correction_T_min  0.0210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    6535 Corrected reflections written to file mo_2214_0m.hkl
 Estimated minimum and maximum transmission:  0.3456  0.7456
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.2000
 Lambda/2 correction factor = 0.0015
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    3.953
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             540
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: \g-Butyrolactone (GBL)'
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.247
_refine_diff_density_min         -2.162
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       0.0048(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   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1430
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.7814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                1405
_reflns_number_total             1430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc03741g2.cif
_cod_data_source_block           solve
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not determined' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3392 2015-05-12 13:50:21Z andrius 
;
_cod_original_cell_volume        536.05(19)
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7117405