#------------------------------------------------------------------------------
#$Date: 2017-02-04 04:12:49 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191346 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/49/4344954.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_4344954
loop_
_publ_author_name
'Stoumpos, Constantinos C.'
'Mao, Lingling'
'Malliakas, Christos D.'
'Kanatzidis, Mercouri G.'
_publ_section_title
;
 Structure-Band Gap Relationships in Hexagonal Polytypes and
 Low-Dimensional Structures of Hybrid Tin Iodide Perovskites.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              56
_journal_page_last               73
_journal_paper_doi               10.1021/acs.inorgchem.6b02764
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         CH3C(NH2)2SnI3
_chemical_formula_sum            'C2 H7 I3 N2 Sn'
_chemical_formula_weight         558.49
_chemical_name_common            'Acetamidinium Tin Iodide'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      160
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_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            9
_cell_length_a                   9.2529(12)
_cell_length_b                   9.2529(12)
_cell_length_c                   35.060(7)
_cell_measurement_reflns_used    2007
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      24.43
_cell_measurement_theta_min      2.60
_cell_volume                     2599.6(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      400(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      ' 235 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  0.0472
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            5274
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.74
_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    10.167
_exptl_absorpt_correction_T_max  0.5557
_exptl_absorpt_correction_T_min  0.3065
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-SHAPE
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             2178
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.495
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.32(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         1197
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0987P)²+12.3255P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1842
_reflns_number_gt                899
_reflns_number_total             1197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02764_si_008.cif
_cod_data_source_block           4b.ACASnI3-400K
_cod_depositor_comments
'Adding full bibliography for 4344944--4344956.cif.'
_cod_original_sg_symbol_Hall     'R3 -2"'
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4344954
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Sn1 Sn 0.0000 0.0000 0.21232(2) 0.09292(3) Uani 1 6 d S T P
Sn2 Sn -0.3333 -0.6667 0.31522(2) 0.09461(3) Uani 1 6 d S T P
Sn3 Sn 0.0000 0.0000 0.09730(2) 0.10348(3) Uani 1 6 d S T P
I1 I -0.02293(2) -0.51146(2) 0.37361(2) 0.14249(3) Uani 1 2 d S T P
I2 I -0.16646(2) 0.16646(2) 0.26452(2) 0.14835(3) Uani 1 2 d S T P
I3 I 0.15288(2) 0.30576(2) 0.15611(2) 0.14793(4) Uani 1 2 d S T P
C1 C -0.3333 0.3333 0.15858(2) 0.4480(18) Uani 1 6 d DS T P
C2 C 0.3333 -0.3333 0.26777(2) 0.3304(8) Uani 1 6 d DS T P
C3 C 0.0000 -1.0000 0.37271(2) 0.4178(16) Uani 1 6 d DS T P
N1 N -0.40373(11) 0.40373(11) 0.15858(2) 0.4480(18) Uani 0.6667 2 d DS T P
C4 C -0.40373(11) 0.40373(11) 0.15858(2) 0.4480(18) Uani 0.3333 2 d S T P
N2 N 0.25879(8) -0.25879(8) 0.26777(2) 0.3304(8) Uani 0.6667 2 d DS T P
C5 C 0.25879(8) -0.25879(8) 0.26777(2) 0.3304(8) Uani 0.3333 2 d S T P
N3 N 0.07414(10) -0.8517(2) 0.37271(2) 0.4178(16) Uani 0.6667 2 d DS T P
C6 C 0.07414(10) -0.8517(2) 0.37271(2) 0.4178(16) Uani 0.3333 2 d S T P
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'
Sn Sn -0.6537 1.4246 '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'
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
I3 Sn1 I3 84.877(10) . 2
I3 Sn1 I3 84.877(10) . 3
I3 Sn1 I3 84.876(10) 2 3
I2 Sn2 I2 92.323(10) 1_545 3_445
I2 Sn2 I2 92.323(10) 1_545 2
I2 Sn2 I2 92.323(10) 3_445 2
I2 Sn2 I1 174.145(5) 1_545 2_445
I2 Sn2 I1 91.731(10) 3_445 2_445
I2 Sn2 I1 91.731(10) 2 2_445
I2 Sn2 I1 91.731(9) 1_545 .
I2 Sn2 I1 174.145(5) 3_445 .
I2 Sn2 I1 91.731(9) 2 .
I1 Sn2 I1 83.925(10) 2_445 .
I2 Sn2 I1 91.730(9) 1_545 3_545
I2 Sn2 I1 91.731(9) 3_445 3_545
I2 Sn2 I1 174.146(5) 2 3_545
I1 Sn2 I1 83.925(10) 2_445 3_545
I1 Sn2 I1 83.925(10) . 3_545
I1 Sn3 I1 84.908(10) 14_444 15_544
I1 Sn3 I1 84.908(11) 14_444 13_554
I1 Sn3 I1 84.906(11) 15_544 13_554
I1 Sn3 I3 178.715(6) 14_444 3
I1 Sn3 I3 96.036(10) 15_544 3
I1 Sn3 I3 96.036(9) 13_554 3
I1 Sn3 I3 96.038(9) 14_444 2
I1 Sn3 I3 96.038(10) 15_544 2
I1 Sn3 I3 178.714(6) 13_554 2
I3 Sn3 I3 83.004(10) 3 2
I1 Sn3 I3 96.039(10) 14_444 .
I1 Sn3 I3 178.714(6) 15_544 .
I1 Sn3 I3 96.038(9) 13_554 .
I3 Sn3 I3 83.004(10) 3 .
I3 Sn3 I3 83.004(10) 2 .
Sn3 I1 Sn2 78.253(13) 7_445 .
Sn1 I3 Sn3 78.892(14) . .
N1 C1 N1 120.0 3_455 2_565
N1 C1 C4 0.00(11) 3_455 3_455
N1 C1 C4 120.0 2_565 3_455
N1 C1 C4 120.0 3_455 2_565
N1 C1 C4 0.000(4) 2_565 2_565
C4 C1 C4 120.0 3_455 2_565
N1 C1 N1 120.0 3_455 .
N1 C1 N1 120.0 2_565 .
C4 C1 N1 120.0 3_455 .
C4 C1 N1 120.0 2_565 .
C5 C2 C5 120.0 3_655 2_545
C5 C2 N2 120.0 3_655 .
C5 C2 N2 120.0 2_545 .
C5 C2 N2 120.0 3_655 2_545
C5 C2 N2 0.0 2_545 2_545
N2 C2 N2 120.0 . 2_545
C5 C2 N2 0.0 3_655 3_655
C5 C2 N2 120.0 2_545 3_655
N2 C2 N2 120.0 . 3_655
N2 C2 N2 120.0 2_545 3_655
C6 C3 N3 120.0 3_645 .
C6 C3 N3 120.0 3_645 2_435
N3 C3 N3 120.000(1) . 2_435
C6 C3 N3 0.0 3_645 3_645
N3 C3 N3 120.000(1) . 3_645
N3 C3 N3 120.0 2_435 3_645
C6 C3 C6 120.002(1) 3_645 2_435
N3 C3 C6 120.0 . 2_435
N3 C3 C6 0.0 2_435 2_435
N3 C3 C6 120.0 3_645 2_435
C1 N1 C4 30.0 . 3_455
C1 N1 C4 30.0 . 2_565
C4 N1 C4 60.0 3_455 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 I3 3.1444(4) .
Sn1 I3 3.1444(4) 2
Sn1 I3 3.1444(4) 3
Sn2 I2 3.2110(4) 1_545
Sn2 I2 3.2110(4) 3_445
Sn2 I2 3.2110(4) 2
Sn2 I1 3.2216(4) 2_445
Sn2 I1 3.2216(4) .
Sn2 I1 3.2216(4) 3_545
Sn3 I1 3.1912(4) 14_444
Sn3 I1 3.1913(4) 15_544
Sn3 I1 3.1913(4) 13_554
Sn3 I3 3.2021(4) 3
Sn3 I3 3.2021(4) 2
Sn3 I3 3.2021(4) .
I1 Sn3 3.1914(4) 7_445
I2 Sn2 3.2111(4) 1_565
C1 N1 1.1282(18) 3_455
C1 N1 1.1282(18) 2_565
C1 C4 1.1283(18) 3_455
C1 C4 1.1283(18) 2_565
C1 N1 1.1282(18) .
C2 C5 1.1947(13) 3_655
C2 C5 1.1947(13) 2_545
C2 N2 1.1947(13) .
C2 N2 1.1947(13) 2_545
C2 N2 1.1947(13) 3_655
C3 C6 1.1881(17) 3_645
C3 N3 1.1882(17) .
C3 N3 1.1882(17) 2_435
C3 N3 1.1882(17) 3_645
C3 C6 1.1882(17) 2_435
N1 C4 1.954(3) 3_455
N1 C4 1.954(3) 2_565
