#------------------------------------------------------------------------------
#$Date: 2019-11-28 14:33:19 +0100 (jue 28 de nov de 2019) $
#$Revision: 244040 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/55/7125562.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_7125562
loop_
_publ_author_name
'Zhu, Xu-Hui'
'Mercier, Nicolas'
'Riou, Amédée'
'Blanchard, Philippe'
'Frère, Pierre'
_publ_section_title
;
 (C4H3SCH2NH3)2(CH3NH3)Pb2I7: non-centrosymmetrical crystal structure of a
 bilayer hybrid perovskite.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2160
_journal_page_last               2161
_journal_paper_doi               10.1039/b205543k
_journal_year                    2002
_chemical_formula_moiety         'C11 H19 I7 N3 Pb2 S2'
_chemical_formula_sum            'C11 H19 I7 N3 Pb2 S2'
_chemical_formula_weight         1560.09
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A e a 2'
_audit_creation_date             2002-07-15T10:04:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.838(2)
_cell_length_b                   41.5200(10)
_cell_length_c                   8.769(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3218(2)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5330
_diffrn_reflns_theta_full        30.97
_diffrn_reflns_theta_max         30.97
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    17.3
_exptl_absorpt_correction_T_max  0.2422
_exptl_absorpt_correction_T_min  0.0152
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.22
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2692
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.742
_refine_diff_density_min         -1.539
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.43(2)
_refine_ls_extinction_coef       0.000127(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2786
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0433P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                1854
_reflns_number_total             2786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205543k.txt
_cod_data_source_block           per24b
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_original_sg_symbol_H-M      Aba2
_cod_database_code               7125562
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-x, -y, z'
'x, y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'
'-x, -y+1/2, z+1/2'
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_calc_flag
_atom_site_refinement_flags
S1 S -0.0331(16) 0.2139(2) -0.3811(14) 0.139(6) Uani 0.64(3) d P
C3A C -0.0331(16) 0.2139(2) -0.3811(14) 0.139(6) Uani 0.36(3) d P
N1 N -0.0682(17) 0.1390(4) -0.5735(14) 0.068(4) Uani 1 d .
H1A H -0.0726 0.1178 -0.5613 0.102 Uiso 1 calc R
H1B H -0.0417 0.1435 -0.6691 0.102 Uiso 1 calc R
H1C H -0.1584 0.1476 -0.5539 0.102 Uiso 1 calc R
C2 C 0.057(2) 0.1888(5) -0.483(3) 0.077(5) Uani 1 d .
C1 C 0.046(3) 0.1527(4) -0.467(3) 0.087(6) Uani 1 d .
H1D H 0.1439 0.1431 -0.4876 0.105 Uiso 1 calc R
H1E H 0.018 0.1474 -0.363 0.105 Uiso 1 calc R
C3 C 0.163(2) 0.2066(4) -0.600(2) 0.145(8) Uani 0.64(3) d P
H3 H 0.2275 0.1986 -0.6749 0.174 Uiso 0.64(3) calc PR
S1A S 0.163(2) 0.2066(4) -0.600(2) 0.145(8) Uani 0.36(3) d P
C4 C 0.128(5) 0.2416(7) -0.549(4) 0.152(16) Uani 1 d .
H4 H 0.1759 0.2593 -0.5925 0.183 Uiso 1 calc R
C5 C 0.026(5) 0.2446(7) -0.440(4) 0.141(15) Uani 1 d .
H5 H -0.006 0.2645 -0.4042 0.169 Uiso 1 calc R
C6 C 0 0 0.451(7) 0.22(5) Uani 1 d S
N2 N -0.062(7) -0.0115(9) 0.552(8) 0.16(3) Uani 0.5 d P
Pb1 Pb -0.00130(6) 0.078612(10) 0.00119(18) 0.03460(11) Uani 1 d .
I2 I -0.19537(12) 0.07517(3) -0.30465(11) 0.0523(3) Uani 1 d .
I1 I 0 0 -0.0041(4) 0.0551(3) Uani 1 d S
I4 I 0.20085(12) 0.07861(3) 0.29965(11) 0.0574(3) Uani 1 d .
I3 I -0.03356(12) 0.15378(2) 0.01461(18) 0.0593(3) Uani 1 d .
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
S1 0.195(14) 0.053(5) 0.169(10) -0.017(6) 0.037(9) 0.013(6)
C3A 0.195(14) 0.053(5) 0.169(10) -0.017(6) 0.037(9) 0.013(6)
N1 0.060(9) 0.066(10) 0.078(9) 0.008(7) 0.014(7) -0.002(8)
C2 0.068(10) 0.082(12) 0.081(11) -0.021(12) 0.010(11) -0.007(10)
C1 0.089(13) 0.049(9) 0.125(18) -0.028(13) -0.025(13) 0.008(10)
C3 0.129(14) 0.129(14) 0.177(16) 0.013(11) 0.026(10) -0.046(11)
S1A 0.129(14) 0.129(14) 0.177(16) 0.013(11) 0.026(10) -0.046(11)
C4 0.21(4) 0.08(2) 0.16(3) 0.05(2) -0.07(3) -0.09(2)
C5 0.21(4) 0.057(16) 0.16(3) 0.005(17) 0.04(2) 0.020(19)
C6 0.47(14) 0.05(3) 0.13(4) 0 0 -0.12(5)
N2 0.21(6) 0.04(2) 0.23(7) -0.04(3) -0.14(5) 0.05(3)
Pb1 0.03204(17) 0.0409(2) 0.03088(16) 0.0004(3) 0.00011(13) -0.00094(19)
I2 0.0482(6) 0.0617(7) 0.0471(7) 0.0003(5) -0.0225(4) 0.0021(4)
I1 0.0677(7) 0.0333(5) 0.0644(7) 0 0 0.0031(7)
I4 0.0457(6) 0.0799(9) 0.0464(7) -0.0093(5) -0.0208(4) 0.0114(5)
I3 0.0711(7) 0.0347(4) 0.0720(7) 0.0040(6) -0.0033(8) -0.0048(4)
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 0 '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'
S S 0.1246 0.1234 '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_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-4 12 -2
-1 -13 -3
-3 -7 5
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
C5 S1 C2 101.0(18) . .
C1 C2 C3 124.4(18) . .
C1 C2 S1 124.5(18) . .
C3 C2 S1 111.0(15) . .
N1 C1 C2 111.2(17) . .
C4 C3 C2 98(2) . .
C5 C4 C3 116(2) . .
C4 C5 S1 115(3) . .
N2 C6 N2 79(6) 4 .
C6 N2 N2 51(3) . 4
I3 Pb1 I4 91.17(4) . .
I3 Pb1 I2 87.02(3) . 7_445
I4 Pb1 I2 91.90(7) . 7_445
I3 Pb1 I2 91.56(4) . .
I4 Pb1 I2 176.90(4) . .
I2 Pb1 I2 89.70(4) 7_445 .
I3 Pb1 I4 95.54(3) . 7_544
I4 Pb1 I4 89.33(4) . 7_544
I2 Pb1 I4 177.14(4) 7_445 7_544
I2 Pb1 I4 88.96(6) . 7_544
I3 Pb1 I1 174.81(3) . .
I4 Pb1 I1 90.55(5) . .
I2 Pb1 I1 88.03(4) 7_445 .
I2 Pb1 I1 86.85(5) . .
I4 Pb1 I1 89.38(4) 7_544 .
Pb1 I2 Pb1 154.50(6) 7_444 .
Pb1 I1 Pb1 178.38(12) . 4
Pb1 I4 Pb1 157.97(6) . 7_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C5 1.47(4) .
S1 C2 1.59(2) .
N1 C1 1.49(2) .
C2 C1 1.51(3) .
C2 C3 1.57(3) .
C3 C4 1.55(4) .
C4 C5 1.32(5) .
C6 N2 1.15(8) 4
C6 N2 1.15(8) .
N2 N2 1.46(12) 4
Pb1 I3 3.1361(10) .
Pb1 I4 3.169(2) .
Pb1 I2 3.1790(16) 7_445
Pb1 I2 3.187(2) .
Pb1 I4 3.1898(17) 7_544
Pb1 I1 3.2643(4) .
I2 Pb1 3.1790(16) 7_444
I1 Pb1 3.2643(4) 4
I4 Pb1 3.1898(17) 7_545
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A I2 . 0.89 3.06 3.722(14) 132.6
N1 H1A I4 1_554 0.89 3.16 3.631(16) 115.5
N1 H1B I3 1_554 0.89 2.81 3.676(13) 165.7
N1 H1C I3 7_444 0.89 2.8 3.655(15) 161.7
