#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:54:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179459 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/56/4335635.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_4335635
loop_
_publ_author_name
'Constantinos C. Stoumpos'
'Christos D. Malliakas'
'Mercouri G. Kanatzidis'
_publ_contact_author_address
;
   Department of Chemistry
     2145 Sheridan Road
   Northwestern University
   Evanston, IL 60208-3113
           USA
;
_publ_contact_author_email       m-kanatzidis@northwestern.edu
_publ_contact_author_fax         847-491-5937
_publ_contact_author_name        'Mercouri G. Kanatzidis'
_publ_contact_author_phone       847-467-1541
_publ_section_title
;
 Semiconducting Tin and Lead Iodide Perovskites with Organic Cations:
 Phase Transitions, High Mobilities, and Near-Infrared Photoluminescent
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9019
_journal_page_last               9038
_journal_paper_doi               10.1021/ic401215x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         HC(NH2)2PbI3
_chemical_formula_sum            'C H5 I3 N2 Pb'
_chemical_formula_weight         632.96
_chemical_name_common            beta-Formamidinium_Lead_Iodide
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           143
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3'
_symmetry_space_group_name_H-M   'P 3'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   17.7914(8)
_cell_length_b                   17.7914(8)
_cell_length_c                   10.9016(6)
_cell_measurement_reflns_used    4843
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.70
_cell_measurement_theta_min      3.24
_cell_volume                     2988.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19512
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_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    26.159
_exptl_absorpt_correction_T_max  0.3908
_exptl_absorpt_correction_T_min  0.2759
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.221
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.038
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.023
_refine_diff_density_max         3.391
_refine_diff_density_min         -4.496
_refine_diff_density_rms         0.597
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(5)
_refine_ls_extinction_coef       0.000498(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         7026
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.1780
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0994P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.2133
_reflns_number_gt                2012
_reflns_number_total             7026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401215x_si_003_1.cif
_cod_data_source_block           4a_150K
_cod_database_code               4335635
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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
Pb1 Pb 0.33321(3) 0.16653(4) 0.19938(8) 0.03750(12) Uani 1 1 d .
Pb2 Pb 0.50001(3) 0.00004(4) 0.53269(6) 0.02592(9) Uani 1 1 d .
Pb3 Pb 0.16677(4) 0.33354(3) 0.86640(5) 0.03122(12) Uani 1 1 d .
Pb4 Pb 0.3333 0.6667 0.19946(11) 0.03574(18) Uani 1 3 d S
Pb5 Pb 0.6667 0.3333 0.86567(12) 0.0435(2) Uani 1 3 d S
Pb6 Pb 0.0000 0.0000 0.53301(9) 0.01650(13) Uani 1 3 d S
I1 I 0.42090(11) 0.34417(7) 0.34389(11) 0.0908(5) Uani 1 1 d .
I2 I 0.25547(8) 0.24498(9) 0.01035(12) 0.0923(4) Uani 1 1 d .
I3 I 0.32304(8) 0.40942(10) 0.67675(11) 0.0918(6) Uani 1 1 d .
I4 I 0.16544(8) 0.10023(9) 0.36666(14) 0.1024(5) Uani 1 1 d .
I5 I 0.26840(9) 0.50241(8) 0.03318(13) 0.1006(5) Uani 1 1 d .
I6 I 0.60092(9) 0.16746(9) 0.70000(14) 0.1016(5) Uani 1 1 d .
I7 I 0.07985(8) 0.42269(7) 0.71884(12) 0.0929(4) Uani 1 1 d .
I8 I 0.01008(7) 0.25363(10) 0.05100(11) 0.0891(6) Uani 1 1 d D
I9 I 0.41383(9) 0.08997(8) 0.38518(12) 0.0924(4) Uani 1 1 d .
I10 I 0.49839(7) 0.23594(7) 0.03397(15) 0.0810(4) Uani 1 1 d .
I11 I 0.16559(7) 0.56904(8) 0.36757(14) 0.0801(4) Uani 1 1 d .
I12 I 0.07002(8) 0.16783(7) 0.69902(14) 0.0794(4) Uani 1 1 d .
C1 C 0.0380(5) 0.4676(6) 0.0815(9) 0.0357(14) Uiso 1 1 d D
N1 N 0.5024(3) 0.0112(6) 0.0271(4) 0.0357(14) Uiso 1 1 d D
N2 N 0.0637(2) 0.44292(16) 0.1745(4) 0.0357(14) Uiso 1 1 d D
C2 C 0.3268(5) 0.1592(5) 0.6939(10) 0.0248(11) Uiso 1 1 d D
N3 N 0.3070(2) 0.2005(2) 0.6186(4) 0.0248(11) Uiso 1 1 d D
N4 N 0.3660(2) 0.1290(2) 0.7542(5) 0.0248(11) Uiso 1 1 d D
C3 C 0.1344(11) 0.3364(7) 0.4463(16) 0.109(4) Uiso 1 1 d D
N5 N 0.2093(5) 0.4109(3) 0.4464(9) 0.109(4) Uiso 1 1 d D
N6 N 0.0930(6) 0.2640(3) 0.3804(9) 0.109(4) Uiso 1 1 d D
C4 C 0.0000 0.0000 0.009(5) 0.149(12) Uiso 1 3 d SD
N7 N 0.09334(12) 0.0500(18) 0.989(4) 0.149(12) Uiso 0.67 1 d PD
C5 C 0.3333 0.6667 0.752(4) 0.166(15) Uiso 1 3 d SD
N8 N 0.24676(9) 0.6535(2) 0.7838(8) 0.166(15) Uiso 0.67 1 d PD
C6 C 0.6667 0.3333 0.326(4) 0.124(10) Uiso 1 3 d SD
N9 N 0.6287(9) 0.24043(11) 0.305(3) 0.124(10) Uiso 0.67 1 d PD
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'
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
I10 Pb1 I9 90.02(4) . .
I10 Pb1 I1 89.77(4) . .
I9 Pb1 I1 90.46(4) . .
I10 Pb1 I8 90.29(4) . 3
I9 Pb1 I8 90.67(4) . 3
I1 Pb1 I8 178.87(5) . 3
I10 Pb1 I2 88.97(4) . .
I9 Pb1 I2 178.98(4) . .
I1 Pb1 I2 89.41(4) . .
I8 Pb1 I2 89.46(4) 3 .
I10 Pb1 I4 178.65(5) . .
I9 Pb1 I4 90.96(5) . .
I1 Pb1 I4 89.29(4) . .
I8 Pb1 I4 90.64(4) 3 .
I2 Pb1 I4 90.05(4) . .
I11 Pb2 I3 90.06(4) 3 2_655
I11 Pb2 I9 90.41(4) 3 .
I3 Pb2 I9 178.54(4) 2_655 .
I11 Pb2 I7 90.01(4) 3 3
I3 Pb2 I7 90.79(4) 2_655 3
I9 Pb2 I7 90.59(4) . 3
I11 Pb2 I1 88.97(5) 3 2_655
I3 Pb2 I1 89.03(4) 2_655 2_655
I9 Pb2 I1 89.60(4) . 2_655
I7 Pb2 I1 178.96(5) 3 2_655
I11 Pb2 I6 178.95(5) 3 .
I3 Pb2 I6 89.10(5) 2_655 .
I9 Pb2 I6 90.41(4) . .
I7 Pb2 I6 90.64(4) 3 .
I1 Pb2 I6 90.38(4) 2_655 .
I8 Pb3 I12 90.09(4) 1_556 .
I8 Pb3 I2 90.44(4) 1_556 1_556
I12 Pb3 I2 89.79(4) . 1_556
I8 Pb3 I7 90.40(4) 1_556 .
I12 Pb3 I7 89.96(4) . .
I2 Pb3 I7 179.12(4) 1_556 .
I8 Pb3 I3 178.51(5) 1_556 .
I12 Pb3 I3 88.47(4) . .
I2 Pb3 I3 89.19(4) 1_556 .
I7 Pb3 I3 89.96(4) . .
I8 Pb3 I5 91.03(4) 1_556 1_556
I12 Pb3 I5 178.83(5) . 1_556
I2 Pb3 I5 89.85(4) 1_556 1_556
I7 Pb3 I5 90.38(4) . 1_556
I3 Pb3 I5 90.41(4) . 1_556
I5 Pb4 I5 89.79(4) 2_665 .
I5 Pb4 I5 89.79(4) 2_665 3_565
I5 Pb4 I5 89.79(4) . 3_565
I5 Pb4 I11 90.94(3) 2_665 2_665
I5 Pb4 I11 89.23(4) . 2_665
I5 Pb4 I11 178.77(4) 3_565 2_665
I5 Pb4 I11 178.77(4) 2_665 .
I5 Pb4 I11 90.94(3) . .
I5 Pb4 I11 89.22(4) 3_565 .
I11 Pb4 I11 90.06(4) 2_665 .
I5 Pb4 I11 89.22(4) 2_665 3_565
I5 Pb4 I11 178.77(4) . 3_565
I5 Pb4 I11 90.94(3) 3_565 3_565
I11 Pb4 I11 90.06(4) 2_665 3_565
I11 Pb4 I11 90.06(4) . 3_565
I6 Pb5 I6 90.29(5) . 2_655
I6 Pb5 I6 90.29(5) . 3_665
I6 Pb5 I6 90.29(5) 2_655 3_665
I6 Pb5 I10 178.66(4) . 3_666
I6 Pb5 I10 88.86(4) 2_655 3_666
I6 Pb5 I10 90.74(4) 3_665 3_666
I6 Pb5 I10 90.74(4) . 1_556
I6 Pb5 I10 178.67(4) 2_655 1_556
I6 Pb5 I10 88.86(4) 3_665 1_556
I10 Pb5 I10 90.13(5) 3_666 1_556
I6 Pb5 I10 88.86(4) . 2_656
I6 Pb5 I10 90.74(4) 2_655 2_656
I6 Pb5 I10 178.66(4) 3_665 2_656
I10 Pb5 I10 90.13(5) 3_666 2_656
I10 Pb5 I10 90.13(5) 1_556 2_656
I4 Pb6 I4 90.05(4) 2 .
I4 Pb6 I4 90.05(4) 2 3
I4 Pb6 I4 90.05(4) . 3
I4 Pb6 I12 90.57(4) 2 .
I4 Pb6 I12 88.82(4) . .
I4 Pb6 I12 178.71(4) 3 .
I4 Pb6 I12 178.71(4) 2 3
I4 Pb6 I12 90.57(4) . 3
I4 Pb6 I12 88.82(4) 3 3
I12 Pb6 I12 90.56(4) . 3
I4 Pb6 I12 88.82(4) 2 2
I4 Pb6 I12 178.71(4) . 2
I4 Pb6 I12 90.57(4) 3 2
I12 Pb6 I12 90.57(4) . 2
I12 Pb6 I12 90.56(4) 3 2
Pb1 I1 Pb2 169.29(5) . 3_665
Pb3 I2 Pb1 169.30(6) 1_554 .
Pb2 I3 Pb3 169.20(4) 3_665 .
Pb6 I4 Pb1 168.66(6) . .
Pb4 I5 Pb3 168.86(6) . 1_554
Pb5 I6 Pb2 168.89(7) . .
Pb3 I7 Pb2 170.67(5) . 2
Pb3 I8 Pb1 170.87(5) 1_554 2
Pb2 I9 Pb1 170.66(6) . .
Pb1 I10 Pb5 171.45(5) . 1_554
Pb2 I11 Pb4 171.11(6) 2 .
Pb3 I12 Pb6 171.00(5) . .
N2 C1 N1 153.6(9) . 2
N4 C2 N3 164.5(9) . .
N5 C3 N6 139.4(16) . .
N7 C4 N7 117.9(13) 3_554 2_554
N7 C4 N7 117.9(13) 3_554 1_554
N7 C4 N7 117.9(13) 2_554 1_554
N8 C5 N8 114.6(12) . 2_665
N8 C5 N8 114.6(12) . 3_565
N8 C5 N8 114.6(12) 2_665 3_565
N9 C6 N9 117.7(11) . 3_665
N9 C6 N9 117.7(11) . 2_655
N9 C6 N9 117.7(11) 3_665 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I10 3.1279(15) .
Pb1 I9 3.1574(18) .
Pb1 I1 3.1581(13) .
Pb1 I8 3.1658(13) 3
Pb1 I2 3.1682(18) .
Pb1 I4 3.1790(15) .
Pb2 I11 3.1325(14) 3
Pb2 I3 3.1470(13) 2_655
Pb2 I9 3.1544(18) .
Pb2 I7 3.1597(15) 3
Pb2 I1 3.1624(12) 2_655
Pb2 I6 3.1741(14) .
Pb3 I8 3.1431(13) 1_556
Pb3 I12 3.1479(13) .
Pb3 I2 3.1500(18) 1_556
Pb3 I7 3.1539(16) .
Pb3 I3 3.1739(13) .
Pb3 I5 3.1890(13) 1_556
Pb4 I5 3.1280(15) 2_665
Pb4 I5 3.1281(15) .
Pb4 I5 3.1281(15) 3_565
Pb4 I11 3.1778(14) 2_665
Pb4 I11 3.1778(14) .
Pb4 I11 3.1779(14) 3_565
Pb5 I6 3.1444(16) .
Pb5 I6 3.1444(16) 2_655
Pb5 I6 3.1444(16) 3_665
Pb5 I10 3.1850(15) 3_666
Pb5 I10 3.1850(15) 1_556
Pb5 I10 3.1851(15) 2_656
Pb6 I4 3.1437(14) 2
Pb6 I4 3.1438(14) .
Pb6 I4 3.1438(14) 3
Pb6 I12 3.1660(13) .
Pb6 I12 3.1660(13) 3
Pb6 I12 3.1660(13) 2
I1 Pb2 3.1624(12) 3_665
I2 Pb3 3.1501(18) 1_554
I3 Pb2 3.1471(14) 3_665
I5 Pb3 3.1890(13) 1_554
I7 Pb2 3.1597(15) 2
I8 Pb3 3.1431(13) 1_554
I8 Pb1 3.1658(13) 2
I10 Pb5 3.1850(15) 1_554
I11 Pb2 3.1326(14) 2
C1 N2 1.277(11) .
C1 N1 1.289(11) 2
N1 C1 1.289(11) 3
C2 N4 1.256(12) .
C2 N3 1.264(11) .
C3 N5 1.329(12) .
C3 N6 1.331(14) .
C4 N7 1.455(10) 3_554
C4 N7 1.455(10) 2_554
C4 N7 1.455(10) 1_554
N7 C4 1.455(10) 1_556
C5 N8 1.479(10) .
C5 N8 1.479(10) 2_665
C5 N8 1.479(10) 3_565
C6 N9 1.457(9) .
C6 N9 1.457(9) 3_665
C6 N9 1.457(9) 2_655
