# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c4
_database_code_depnum_ccdc_archive 'CCDC 1537775'
_audit_update_record             
;
2017-03-14 deposited with the CCDC.
2017-04-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?CH3NH3?0.85[CH(NH2)2]0.15PbI3
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            CN1.15H5.85PbI3
_chemical_formula_weight         621.91

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'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   pm-3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   6.3191(2)
_cell_length_b                   6.3191(2)
_cell_length_c                   6.3191(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     252.328(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    300.00(10)
_cell_measurement_reflns_used    1811
_cell_measurement_theta_min      0.28972
_cell_measurement_theta_max      1.00000

_exptl_crystal_description       bulk
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             261
_exptl_absorpt_coefficient_mu    25.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.28972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;                                                         
CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.         
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300.00(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2576
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0127
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.56
_diffrn_reflns_theta_max         29.57
_reflns_number_total             100
_reflns_number_gt                100
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0480P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         100
_refine_ls_number_parameters     7
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0608
_refine_ls_wR_factor_gt          0.0608
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_restrained_S_all      1.179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.0000 0.0000 0.0000 0.0304(3) Uani 1 48 d S . .
I2 I 0.0000 0.0000 -0.5000 0.1180(8) Uani 1 16 d S . .
C1 C 0.5000 -0.5000 0.5000 0.19(4) Uiso 1 48 d SD . .
N1 N 0.5000 -0.5000 0.289(3) 0.16(6) Uiso 0.19 8 d SPD . .

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
Pb1 0.0304(3) 0.0304(3) 0.0304(3) 0.000 0.000 0.000
I2 0.1660(12) 0.1660(12) 0.0221(5) 0.000 0.000 0.000

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.1596(1) 9_565 ?
Pb1 I2 3.1596(1) . ?
Pb1 I2 3.1596(1) 1_556 ?
Pb1 I2 3.1596(1) 5 ?
Pb1 I2 3.1596(1) 5_655 ?
Pb1 I2 3.1596(1) 9 ?
I2 Pb1 3.1596(1) 1_554 ?
C1 N1 1.34(2) 29_655 ?
C1 N1 1.34(2) 33_556 ?
C1 N1 1.34(2) . ?
C1 N1 1.34(2) 25_646 ?
C1 N1 1.34(2) 5_546 ?
C1 N1 1.34(2) 9_645 ?
N1 N1 1.89(3) 29_655 ?
N1 N1 1.89(3) 33_556 ?
N1 N1 1.89(3) 5_546 ?
N1 N1 1.89(3) 9_645 ?

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
_geom_angle_publ_flag
I2 Pb1 I2 90.0 9_565 . ?
I2 Pb1 I2 90.0 9_565 1_556 ?
I2 Pb1 I2 180.0 . 1_556 ?
I2 Pb1 I2 90.0 9_565 5 ?
I2 Pb1 I2 90.0 . 5 ?
I2 Pb1 I2 90.0 1_556 5 ?
I2 Pb1 I2 90.0 9_565 5_655 ?
I2 Pb1 I2 90.0 . 5_655 ?
I2 Pb1 I2 90.0 1_556 5_655 ?
I2 Pb1 I2 180.0 5 5_655 ?
I2 Pb1 I2 180.0 9_565 9 ?
I2 Pb1 I2 90.0 . 9 ?
I2 Pb1 I2 90.0 1_556 9 ?
I2 Pb1 I2 90.0 5 9 ?
I2 Pb1 I2 90.0 5_655 9 ?
Pb1 I2 Pb1 180.0 1_554 . ?
N1 C1 N1 90.000(2) 29_655 33_556 ?
N1 C1 N1 90.000(1) 29_655 . ?
N1 C1 N1 90.000(1) 33_556 . ?
N1 C1 N1 90.000(1) 29_655 25_646 ?
N1 C1 N1 90.000(1) 33_556 25_646 ?
N1 C1 N1 180.000(2) . 25_646 ?
N1 C1 N1 180.000(1) 29_655 5_546 ?
N1 C1 N1 90.000(1) 33_556 5_546 ?
N1 C1 N1 90.0 . 5_546 ?
N1 C1 N1 90.0 25_646 5_546 ?
N1 C1 N1 90.000(1) 29_655 9_645 ?
N1 C1 N1 180.000(1) 33_556 9_645 ?
N1 C1 N1 90.000(3) . 9_645 ?
N1 C1 N1 90.0 25_646 9_645 ?
N1 C1 N1 90.000(4) 5_546 9_645 ?
C1 N1 N1 45.0 . 29_655 ?
C1 N1 N1 45.0 . 33_556 ?
N1 N1 N1 60.0 29_655 33_556 ?
C1 N1 N1 45.0 . 5_546 ?
N1 N1 N1 90.0 29_655 5_546 ?
N1 N1 N1 60.000(1) 33_556 5_546 ?
C1 N1 N1 45.0 . 9_645 ?
N1 N1 N1 60.000(1) 29_655 9_645 ?
N1 N1 N1 90.0 33_556 9_645 ?
N1 N1 N1 60.000(1) 5_546 9_645 ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        29.57
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.488
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.329
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c4-2-final-2
_database_code_depnum_ccdc_archive 'CCDC 1537762'
_audit_update_record             
;
2017-03-14 deposited with the CCDC.
2017-04-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[CH(NH2)2]0.85[CH3NH3]0.15PbI3'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[CH(NH2)2]0.85[CH3NH3]0.15PbI3'
_chemical_formula_sum            CN1.85H5.15PbI3
_chemical_formula_weight         631.01

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'
Pb Pb -3.3944 10.1111 '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'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   pm-3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   6.3749(4)
_cell_length_b                   6.3749(4)
_cell_length_c                   6.3749(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     259.07(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    300.00(10)
_cell_measurement_reflns_used    327
_cell_measurement_theta_min      5.5640
_cell_measurement_theta_max      29.2560

_exptl_crystal_description       bulk
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             265
_exptl_absorpt_coefficient_mu    25.144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_T_max  1.923
_exptl_absorpt_process_details   
;                                                                
CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)        
Empirical absorption correction using spherical harmonics,       
 implemented in SCALE3 ABSPACK scaling algorithm.                
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300.00(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            407
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         5.54
_diffrn_reflns_theta_max         26.04
_reflns_number_total             76
_reflns_number_gt                76
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0391P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         76
_refine_ls_number_parameters     7
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0595
_refine_ls_wR_factor_gt          0.0595
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_restrained_S_all      1.192
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.0000 0.0000 0.0000 0.0312(5) Uani 1 48 d S . .
I1 I 0.0000 0.0000 0.5000 0.0883(8) Uani 1 16 d S . .
C1 C 0.5000 -0.5000 0.5000 0.18(5) Uiso 1 48 d SD . .
N1 N 0.5000 -0.5000 0.290(3) 0.19(5) Uiso 0.31 8 d SPD . .

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
Pb1 0.0312(5) 0.0312(5) 0.0312(5) 0.000 0.000 0.000
I1 0.1212(11) 0.1212(11) 0.0224(7) 0.000 0.000 0.000

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.1874(2) 9 ?
Pb1 I1 3.1874(2) . ?
Pb1 I1 3.1874(2) 1_554 ?
Pb1 I1 3.1874(2) 5_455 ?
Pb1 I1 3.1874(2) 5 ?
Pb1 I1 3.1874(2) 9_545 ?
I1 Pb1 3.1874(2) 1_556 ?
C1 N1 1.34(2) 33_556 ?
C1 N1 1.34(2) . ?
C1 N1 1.34(2) 25_646 ?
C1 N1 1.34(2) 5_546 ?
C1 N1 1.34(2) 29_655 ?
C1 N1 1.34(2) 9_645 ?
N1 N1 1.90(3) 33_556 ?
N1 N1 1.90(3) 29_655 ?
N1 N1 1.90(3) 5_546 ?
N1 N1 1.90(3) 9_645 ?

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
_geom_angle_publ_flag
I1 Pb1 I1 90.0 9 . ?
I1 Pb1 I1 90.0 9 1_554 ?
I1 Pb1 I1 180.0 . 1_554 ?
I1 Pb1 I1 90.0 9 5_455 ?
I1 Pb1 I1 90.0 . 5_455 ?
I1 Pb1 I1 90.0 1_554 5_455 ?
I1 Pb1 I1 90.0 9 5 ?
I1 Pb1 I1 90.0 . 5 ?
I1 Pb1 I1 90.0 1_554 5 ?
I1 Pb1 I1 180.0 5_455 5 ?
I1 Pb1 I1 180.0 9 9_545 ?
I1 Pb1 I1 90.0 . 9_545 ?
I1 Pb1 I1 90.0 1_554 9_545 ?
I1 Pb1 I1 90.0 5_455 9_545 ?
I1 Pb1 I1 90.0 5 9_545 ?
Pb1 I1 Pb1 180.0 1_556 . ?
N1 C1 N1 90.000(1) 33_556 . ?
N1 C1 N1 90.000(1) 33_556 25_646 ?
N1 C1 N1 180.000(2) . 25_646 ?
N1 C1 N1 90.000(2) 33_556 5_546 ?
N1 C1 N1 90.0 . 5_546 ?
N1 C1 N1 90.0 25_646 5_546 ?
N1 C1 N1 90.000(2) 33_556 29_655 ?
N1 C1 N1 90.0 . 29_655 ?
N1 C1 N1 90.0 25_646 29_655 ?
N1 C1 N1 180.000(2) 5_546 29_655 ?
N1 C1 N1 180.000(1) 33_556 9_645 ?
N1 C1 N1 90.000(3) . 9_645 ?
N1 C1 N1 90.0 25_646 9_645 ?
N1 C1 N1 90.000(4) 5_546 9_645 ?
N1 C1 N1 90.000(1) 29_655 9_645 ?
C1 N1 N1 45.0 . 33_556 ?
C1 N1 N1 45.0 . 29_655 ?
N1 N1 N1 60.000(1) 33_556 29_655 ?
C1 N1 N1 45.0 . 5_546 ?
N1 N1 N1 60.000(1) 33_556 5_546 ?
N1 N1 N1 90.0 29_655 5_546 ?
C1 N1 N1 45.0 . 9_645 ?
N1 N1 N1 90.0 33_556 9_645 ?
N1 N1 N1 60.0 29_655 9_645 ?
N1 N1 N1 60.000(1) 5_546 9_645 ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.255
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_45-6
_database_code_depnum_ccdc_archive 'CCDC 1532918'
_audit_update_record             
;
2017-02-15 deposited with the CCDC.
2017-04-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Formamidinium Lead Iodide'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         CH(NH2)2PbI3
_chemical_formula_sum            'C H5 I3 N2 Pb'
_chemical_formula_weight         632.96

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'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   P-43m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'

_cell_length_a                   6.3691(2)
_cell_length_b                   6.3691(2)
_cell_length_c                   6.3691(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     258.365(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    1697
_cell_measurement_theta_min      4.5010
_cell_measurement_theta_max      29.2920

_exptl_crystal_description       cuboid
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             266
_exptl_absorpt_coefficient_mu    25.214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.40833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2719
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.53
_diffrn_reflns_theta_max         29.52
_reflns_number_total             165
_reflns_number_gt                165
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0190P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_number_reflns         165
_refine_ls_number_parameters     8
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0125
_refine_ls_R_factor_gt           0.0125
_refine_ls_wR_factor_ref         0.0343
_refine_ls_wR_factor_gt          0.0343
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_restrained_S_all      2.525
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.0000 0.0000 0.0000 0.0336(3) Uani 1 24 d S . .
I2 I 0.962(2) 0.0000 0.5000 0.066(3) Uani 0.25 2 d SP . .
N4 N 0.4500 0.3095 0.5500 0.120(17) Uiso 0.17 2 d SPD . .
C3 C 0.5000 0.5000 0.5000 0.120(17) Uiso 1 24 d SD . .

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
Pb1 0.0336(3) 0.0336(3) 0.0336(3) 0.000 0.000 0.000
I2 0.090(6) 0.084(5) 0.0248(5) 0.003(2) 0.000 0.000

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.1935(12) 22_656 ?
Pb1 I2 3.1935(12) 21_554 ?
Pb1 I2 3.1935(12) 1_554 ?
Pb1 I2 3.1935(12) 18_755 ?
Pb1 I2 3.1935(12) 2_755 ?
Pb1 I2 3.1935(12) 5_545 ?
Pb1 I2 3.1935(12) 17_545 ?
Pb1 I2 3.1935(12) 14_665 ?
Pb1 I2 3.1935(12) 6_665 ?
Pb1 I2 3.1935(12) 9_644 ?
Pb1 I2 3.1935(12) 13_644 ?
Pb1 I2 3.1935(12) 10_656 ?
I2 I2 0.34(2) 14_665 ?
I2 I2 0.34(2) 13_645 ?
I2 I2 0.48(3) 2_755 ?
I2 Pb1 3.1935(12) 1_556 ?
N4 N4 0.9009 3_656 ?
N4 N4 1.2651 8_656 ?
N4 N4 1.2651 11_566 ?
N4 C3 1.2940 . ?
N4 N4 1.8846 6_566 ?
N4 N4 1.8846 12_665 ?
N4 N4 1.8846 9 ?
N4 N4 1.8846 5 ?
C3 N4 1.2940 10_656 ?
C3 N4 1.2940 6_566 ?
C3 N4 1.2940 2_665 ?
C3 N4 1.2940 11_566 ?
C3 N4 1.2940 5 ?
C3 N4 1.2940 3_656 ?
C3 N4 1.2940 7_665 ?
C3 N4 1.2940 9 ?
C3 N4 1.2940 12_665 ?
C3 N4 1.2940 8_656 ?
C3 N4 1.2940 4_566 ?

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
_geom_angle_publ_flag
I2 Pb1 I2 180.0 22_656 21_554 ?
I2 Pb1 I2 98.6(6) 22_656 1_554 ?
I2 Pb1 I2 81.4(6) 21_554 1_554 ?
I2 Pb1 I2 85.7(3) 22_656 18_755 ?
I2 Pb1 I2 94.3(3) 21_554 18_755 ?
I2 Pb1 I2 90.32(4) 1_554 18_755 ?
I2 Pb1 I2 81.4(6) 22_656 2_755 ?
I2 Pb1 I2 98.6(6) 21_554 2_755 ?
I2 Pb1 I2 180.0 1_554 2_755 ?
I2 Pb1 I2 89.68(4) 18_755 2_755 ?
I2 Pb1 I2 173.9(4) 22_656 5_545 ?
I2 Pb1 I2 6.1(4) 21_554 5_545 ?
I2 Pb1 I2 85.7(3) 1_554 5_545 ?
I2 Pb1 I2 98.6(6) 18_755 5_545 ?
I2 Pb1 I2 94.3(3) 2_755 5_545 ?
I2 Pb1 I2 94.3(3) 22_656 17_545 ?
I2 Pb1 I2 85.7(3) 21_554 17_545 ?
I2 Pb1 I2 89.68(4) 1_554 17_545 ?
I2 Pb1 I2 180.0(6) 18_755 17_545 ?
I2 Pb1 I2 90.32(4) 2_755 17_545 ?
I2 Pb1 I2 81.4(6) 5_545 17_545 ?
I2 Pb1 I2 85.7(3) 22_656 14_665 ?
I2 Pb1 I2 94.3(3) 21_554 14_665 ?
I2 Pb1 I2 173.9(4) 1_554 14_665 ?
I2 Pb1 I2 85.7(3) 18_755 14_665 ?
I2 Pb1 I2 6.1(4) 2_755 14_665 ?
I2 Pb1 I2 90.32(4) 5_545 14_665 ?
I2 Pb1 I2 94.3(3) 17_545 14_665 ?
I2 Pb1 I2 6.1(4) 22_656 6_665 ?
I2 Pb1 I2 173.9(4) 21_554 6_665 ?
I2 Pb1 I2 94.3(3) 1_554 6_665 ?
I2 Pb1 I2 81.4(6) 18_755 6_665 ?
I2 Pb1 I2 85.7(3) 2_755 6_665 ?
I2 Pb1 I2 180.0 5_545 6_665 ?
I2 Pb1 I2 98.6(6) 17_545 6_665 ?
I2 Pb1 I2 89.68(4) 14_665 6_665 ?
I2 Pb1 I2 90.32(4) 22_656 9_644 ?
I2 Pb1 I2 89.68(4) 21_554 9_644 ?
I2 Pb1 I2 85.7(3) 1_554 9_644 ?
I2 Pb1 I2 173.9(4) 18_755 9_644 ?
I2 Pb1 I2 94.3(3) 2_755 9_644 ?
I2 Pb1 I2 85.7(3) 5_545 9_644 ?
I2 Pb1 I2 6.1(4) 17_545 9_644 ?
I2 Pb1 I2 98.6(6) 14_665 9_644 ?
I2 Pb1 I2 94.3(3) 6_665 9_644 ?
I2 Pb1 I2 94.3(3) 22_656 13_644 ?
I2 Pb1 I2 85.7(3) 21_554 13_644 ?
I2 Pb1 I2 6.1(4) 1_554 13_644 ?
I2 Pb1 I2 94.3(3) 18_755 13_644 ?
I2 Pb1 I2 173.9(4) 2_755 13_644 ?
I2 Pb1 I2 89.68(4) 5_545 13_644 ?
I2 Pb1 I2 85.7(3) 17_545 13_644 ?
I2 Pb1 I2 180.0 14_665 13_644 ?
I2 Pb1 I2 90.32(4) 6_665 13_644 ?
I2 Pb1 I2 81.4(6) 9_644 13_644 ?
I2 Pb1 I2 89.68(4) 22_656 10_656 ?
I2 Pb1 I2 90.32(4) 21_554 10_656 ?
I2 Pb1 I2 94.3(3) 1_554 10_656 ?
I2 Pb1 I2 6.1(4) 18_755 10_656 ?
I2 Pb1 I2 85.7(3) 2_755 10_656 ?
I2 Pb1 I2 94.3(3) 5_545 10_656 ?
I2 Pb1 I2 173.9(4) 17_545 10_656 ?
I2 Pb1 I2 81.4(6) 14_665 10_656 ?
I2 Pb1 I2 85.7(3) 6_665 10_656 ?
I2 Pb1 I2 180.0 9_644 10_656 ?
I2 Pb1 I2 98.6(6) 13_644 10_656 ?
I2 I2 I2 90.000(8) 14_665 13_645 ?
I2 I2 I2 45.000(4) 14_665 2_755 ?
I2 I2 I2 45.000(3) 13_645 2_755 ?
I2 I2 Pb1 86.96(19) 14_665 1_556 ?
I2 I2 Pb1 86.96(19) 13_645 1_556 ?
I2 I2 Pb1 85.7(3) 2_755 1_556 ?
I2 I2 Pb1 86.96(19) 14_665 . ?
I2 I2 Pb1 86.96(19) 13_645 . ?
I2 I2 Pb1 85.7(3) 2_755 . ?
Pb1 I2 Pb1 171.4(6) 1_556 . ?
N4 N4 N4 120.0 3_656 8_656 ?
N4 N4 N4 120.0 3_656 11_566 ?
N4 N4 N4 60.0 8_656 11_566 ?
N4 N4 C3 69.6 3_656 . ?
N4 N4 C3 60.7 8_656 . ?
N4 N4 C3 60.7 11_566 . ?
N4 N4 N4 95.5 3_656 6_566 ?
N4 N4 N4 24.5 8_656 6_566 ?
N4 N4 N4 70.4 11_566 6_566 ?
C3 N4 N4 43.3 . 6_566 ?
N4 N4 N4 35.5 3_656 12_665 ?
N4 N4 N4 84.5 8_656 12_665 ?
N4 N4 N4 103.8 11_566 12_665 ?
C3 N4 N4 43.3 . 12_665 ?
N4 N4 N4 60.0 6_566 12_665 ?
N4 N4 N4 95.5 3_656 9 ?
N4 N4 N4 70.4 8_656 9 ?
N4 N4 N4 24.5 11_566 9 ?
C3 N4 N4 43.3 . 9 ?
N4 N4 N4 70.2 6_566 9 ?
N4 N4 N4 83.4 12_665 9 ?
N4 N4 N4 35.5 3_656 5 ?
N4 N4 N4 103.8 8_656 5 ?
N4 N4 N4 84.5 11_566 5 ?
C3 N4 N4 43.3 . 5 ?
N4 N4 N4 83.4 6_566 5 ?
N4 N4 N4 39.2 12_665 5 ?
N4 N4 N4 60.0 9 5 ?
N4 C3 N4 58.5 10_656 6_566 ?
N4 C3 N4 58.5 10_656 2_665 ?
N4 C3 N4 58.5 6_566 2_665 ?
N4 C3 N4 151.5 10_656 11_566 ?
N4 C3 N4 93.5 6_566 11_566 ?
N4 C3 N4 113.6 2_665 11_566 ?
N4 C3 N4 113.6 10_656 . ?
N4 C3 N4 93.5 6_566 . ?
N4 C3 N4 151.5 2_665 . ?
N4 C3 N4 58.5 11_566 . ?
N4 C3 N4 93.5 10_656 5 ?
N4 C3 N4 151.5 6_566 5 ?
N4 C3 N4 113.6 2_665 5 ?
N4 C3 N4 113.6 11_566 5 ?
N4 C3 N4 93.5 . 5 ?
N4 C3 N4 93.5 10_656 3_656 ?
N4 C3 N4 113.6 6_566 3_656 ?
N4 C3 N4 151.5 2_665 3_656 ?
N4 C3 N4 93.5 11_566 3_656 ?
N4 C3 N4 40.7 . 3_656 ?
N4 C3 N4 58.5 5 3_656 ?
N4 C3 N4 113.6 10_656 7_665 ?
N4 C3 N4 151.5 6_566 7_665 ?
N4 C3 N4 93.5 2_665 7_665 ?
N4 C3 N4 93.5 11_566 7_665 ?
N4 C3 N4 113.6 . 7_665 ?
N4 C3 N4 40.7 5 7_665 ?
N4 C3 N4 93.5 3_656 7_665 ?
N4 C3 N4 151.5 10_656 9 ?
N4 C3 N4 113.6 6_566 9 ?
N4 C3 N4 93.5 2_665 9 ?
N4 C3 N4 40.7 11_566 9 ?
N4 C3 N4 93.5 . 9 ?
N4 C3 N4 93.5 5 9 ?
N4 C3 N4 113.6 3_656 9 ?
N4 C3 N4 58.5 7_665 9 ?
N4 C3 N4 40.7 10_656 12_665 ?
N4 C3 N4 93.5 6_566 12_665 ?
N4 C3 N4 93.5 2_665 12_665 ?
N4 C3 N4 151.5 11_566 12_665 ?
N4 C3 N4 93.5 . 12_665 ?
N4 C3 N4 58.5 5 12_665 ?
N4 C3 N4 58.5 3_656 12_665 ?
N4 C3 N4 93.5 7_665 12_665 ?
N4 C3 N4 151.5 9 12_665 ?
N4 C3 N4 93.5 10_656 8_656 ?
N4 C3 N4 40.7 6_566 8_656 ?
N4 C3 N4 93.5 2_665 8_656 ?
N4 C3 N4 58.5 11_566 8_656 ?
N4 C3 N4 58.5 . 8_656 ?
N4 C3 N4 151.5 5 8_656 ?
N4 C3 N4 93.5 3_656 8_656 ?
N4 C3 N4 151.5 7_665 8_656 ?
N4 C3 N4 93.5 9 8_656 ?
N4 C3 N4 113.6 12_665 8_656 ?
N4 C3 N4 93.5 10_656 4_566 ?
N4 C3 N4 93.5 6_566 4_566 ?
N4 C3 N4 40.7 2_665 4_566 ?
N4 C3 N4 93.5 11_566 4_566 ?
N4 C3 N4 151.5 . 4_566 ?
N4 C3 N4 93.5 5 4_566 ?
N4 C3 N4 151.5 3_656 4_566 ?
N4 C3 N4 58.5 7_665 4_566 ?
N4 C3 N4 58.5 9 4_566 ?
N4 C3 N4 113.6 12_665 4_566 ?
N4 C3 N4 113.6 8_656 4_566 ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        29.52
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.083
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
