#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:00:52 +0100 (mar 22 de mar de 2016) $
#$Revision: 179030 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/28/4122893.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4122893
loop_
_publ_author_name
'Hao, Feng'
'Stoumpos, Constantinos C.'
'Liu, Zhao'
'Chang, Robert P. H.'
'Kanatzidis, Mercouri G.'
_publ_section_title
;
 Controllable Perovskite Crystallization at a Gas--Solid Interface for
 Hole Conductor-Free Solar Cells with Steady Power Conversion Efficiency
 over 10%
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141106073145004
_journal_paper_doi               10.1021/ja509245x
_journal_year                    2014
_chemical_formula_sum            'C H8 I3 N O Pb'
_chemical_formula_weight         637.97
_chemical_name_common            'Methylammonium Lead Iodide Hydrate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.161(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3939(9)
_cell_length_b                   4.6419(2)
_cell_length_c                   11.1181(9)
_cell_measurement_reflns_used    6920
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      1.85
_cell_volume                     526.27(7)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      '180 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5153
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         1.87
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.20
_diffrn_source_voltage           40
_exptl_absorpt_coefficient_mu    24.762
_exptl_absorpt_correction_T_max  0.5037
_exptl_absorpt_correction_T_min  0.1946
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-SHAPE
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    4.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.0716
_exptl_crystal_size_mid          0.0225
_exptl_crystal_size_min          0.0167
_refine_diff_density_max         1.103
_refine_diff_density_min         -2.279
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1604
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0254
_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/[σ²(Fo²)+(0.0243P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0506
_reflns_number_gt                1423
_reflns_number_total             1604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja509245x_si_003.cif
_cod_data_source_block           water_solvate
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4122893
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pb Pb 0.40301(3) 0.2500 0.82018(2) 0.01407(7) Uani 1 2 d S
I1 I 0.13976(4) 0.2500 0.64208(4) 0.01669(10) Uani 1 2 d S
I2 I 0.51662(4) 0.7500 0.67290(4) 0.01601(10) Uani 1 2 d S
I3 I 0.30388(4) 0.7500 0.98567(4) 0.01558(10) Uani 1 2 d S
C C 0.0877(8) 0.2500 0.1713(7) 0.034(2) Uani 1 2 d S
H0A H 0.0392 0.4239 0.1398 0.050 Uiso 0.50 1 calc PR
H0B H 0.0367 0.0792 0.1397 0.050 Uiso 0.50 1 calc PR
H0C H 0.1722 0.2468 0.1447 0.050 Uiso 0.50 2 calc SPR
N N 0.1100(4) 0.2500 0.3057(4) 0.0218(13) Uani 1 2 d S
H0D H 0.1572 0.4087 0.3351 0.033 Uiso 0.50 1 calc PR
H0E H 0.1552 0.0886 0.3350 0.033 Uiso 0.50 1 calc PR
H0F H 0.0315 0.2526 0.3304 0.033 Uiso 0.50 2 calc SPR
O O 0.7604(4) 0.2500 0.5871(4) 0.0190(10) Uani 1 2 d SRD
HW1 H 0.6949 0.2500 0.6367 0.029 Uiso 1 2 d SRD
HW2 H 0.7139 0.2500 0.5052 0.029 Uiso 1 2 d SRD
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb 0.01318(13) 0.01387(12) 0.01405(12) 0.000 -0.00009(8) 0.000
I1 0.0118(2) 0.0191(2) 0.0177(2) 0.000 -0.00067(15) 0.000
I2 0.0150(2) 0.01602(19) 0.0174(2) 0.000 0.00418(16) 0.000
I3 0.0137(2) 0.0172(2) 0.0154(2) 0.000 0.00169(15) 0.000
C 0.026(4) 0.049(5) 0.023(4) 0.000 -0.002(3) 0.000
N 0.020(3) 0.017(3) 0.028(3) 0.000 0.003(2) 0.000
O 0.016(2) 0.022(2) 0.020(2) 0.000 0.0064(19) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
I1 Pb I2 92.371(12) . .
I1 Pb I2 92.371(13) . 1_545
I2 Pb I2 93.159(15) . 1_545
I1 Pb I3 91.411(13) . 1_545
I2 Pb I3 176.074(14) . 1_545
I2 Pb I3 87.737(10) 1_545 1_545
I1 Pb I3 91.411(12) . .
I2 Pb I3 87.737(9) . .
I2 Pb I3 176.074(14) 1_545 .
I3 Pb I3 91.116(14) 1_545 .
I1 Pb I3 179.313(15) . 3_667
I2 Pb I3 87.158(12) . 3_667
I2 Pb I3 87.158(12) 1_545 3_667
I3 Pb I3 89.070(12) 1_545 3_667
I3 Pb I3 89.070(12) . 3_667
Pb I2 Pb 93.160(15) 1_565 .
Pb I3 Pb 91.115(14) . 1_565
Pb I3 Pb 90.930(12) . 3_667
Pb I3 Pb 90.930(12) 1_565 3_667
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb I1 3.0512(6) .
Pb I2 3.1954(4) .
Pb I2 3.1955(4) 1_545
Pb I3 3.2508(4) 1_545
Pb I3 3.2508(4) .
Pb I3 3.3757(6) 3_667
I2 Pb 3.1954(4) 1_565
I3 Pb 3.2509(4) 1_565
I3 Pb 3.3757(6) 3_667
C N 1.467(9) .
