Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge      182

loop_
_publ_author_name
'Mercier, Nicolas'
'Blanchard, Philippe'
'Frere, Pierre'
'Riou, Amedee'
'Zhu, Xu-Hui'

_publ_contact_author_name     	'Dr Nicolas Mercier'  
_publ_contact_author_address 
;
IMMO laboratory
2 Bd lavoisier
Angers
49035
FRANCE
;

_publ_contact_author_email         'nicolas.mercier@univ-angers.fr'
_publ_contact_author_fax           '(33)2.41.73.54.05'
_publ_contact_author_phone         '(33)2.41.73.50.83'

_publ_requested_journal            'Chem. Comm.'
_publ_contact_letter
;
Please consider this CIF submission for publication as a new structure
paper. The figures, chemical structure diagram (scheme), Transfert of 
Copyright Agreement form and structure factors will be sent on receipt 
of your acknowledgement letter
;

_publ_requested_category            FM

_publ_section_title
;
(C4H3SCH2NH3)2(CH3NH3)Pb2I7 : non centrosymmetrical crystal structure of a
bilayer hybrid perovskite
;


_publ_section_references
;
Allen, F.H., Kennard, O. & Taylor, R. (1983).
Acc. Chem. Res.  16, 146-153.

Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A.
(1993) J. Appl. Cryst. 26, 343-350.

Beurskens, P.T., Beurskens, G., Bosman, W.P., de Gelder, R.,
Garciia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M.
(1996) The DIRDIF96 program system,
Technical Report of the Crystallography Laboratory,
University of Nijmegen, The Netherlands.

Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358.

Enraf-Nonius (1994). CAD4Express Software. Enraf-Nonius, Delft,
The Netherlands.

Farrugia, L. J. (1997) ORTEP-3 for Windows, J. Appl. Cryst. 30, 565.

Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, In the press.

Flack, H.D. (1983). Acta Cryst. A39, 876-881.

Harms, K. & Wocadlo, S. (1995) XCAD-4. Program for Processing CAD-4
Diffractometer Data. University of Marburg, Germany.

Johnson, C.K. (1965). ORTEP. Report ORNL-3794. Oak Ridge National
Laboratory, Tennessee, USA.

Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580

LePage, Y. (1987). J. Appl. Cryst. 20, 264-269.

North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst,
A24, 351-359

Orpen, A. G., Brammer, L., Allen, F. H., Kennard, O., Watson, D. G.,
& Taylor, R. (1992). International Tables for Crystallography,
Volume C.

Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure
refinement. University of Gottingen, Germany.

Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure
refinement. University of Gottingen, Germany.

Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3,
edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189.
Oxford University Press.

Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution.
University of Gottingen, Germany.

Spek, A.L. (1990). Acta Cryst. A46, C34

Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr.
34, 824-828

Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr.
35, 281.

Walker, N. &  Stuart, D. (1983). Acta Cryst., A39, 158 - 166.

Wilson, A.J.C. (1992) Ed. International Tables for Crystallography,
Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands.
;
_publ_section_figure_captions
;
Figure 1. View of (I) (50% probability displacement ellipsoids)
;
_publ_section_acknowledgements
;
?
;
_publ_section_table_legends
;
Table 1. Fractional atomic coordinates and equivalent
isotropic displacement parameters (\%A^2^)

Table 2. Selected geometric parameters (\%A ,\% )
;

data_per24b
_database_code_CSD                  187951

_audit_creation_date            2002-07-15T10:04:38-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety                'C11 H19 I7 N3 Pb2 S2'
_chemical_formula_sum                   'C11 H19 I7 N3 Pb2 S2'
_chemical_formula_weight                1560.09

#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting                  orthorhombic
_symmetry_space_group_name_H-M          Aba2
_symmetry_space_group_name_Hall         'A 2 -2ac'
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'

_cell_length_a                          8.838(2)
_cell_length_b                          41.5200(10)
_cell_length_c                          8.769(5)
_cell_angle_alpha                       90
_cell_angle_beta                        90
_cell_angle_gamma                       90
_cell_volume                            3218(2)
_cell_formula_units_Z                   4
_cell_measurement_temperature           293(2)

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description              plate
_exptl_crystal_colour                   red
_exptl_crystal_size_max                 0.3
_exptl_crystal_size_mid                 0.2
_exptl_crystal_size_min                 0.09
_exptl_crystal_density_diffrn           3.22
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    2692
_exptl_absorpt_coefficient_mu           17.3
_exptl_absorpt_correction_type          gaussian
_exptl_absorpt_correction_T_min         0.0152
_exptl_absorpt_correction_T_max         0.2422

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_probe                 x-ray
_diffrn_measurement_device_type         'Enraf Nonius CAD4'
_diffrn_measurement_device              '\k-geometry diffractometer'
_diffrn_measurement_method              'non-profiled omega scans'
_diffrn_standards_number                3
_diffrn_standards_interval_time         60
_diffrn_standards_decay_%               2
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

_diffrn_reflns_number                   5330
_diffrn_reflns_av_R_equivalents         0.0556
_diffrn_reflns_limit_h_min              -12
_diffrn_reflns_limit_h_max              12
_diffrn_reflns_limit_k_min              -60
_diffrn_reflns_limit_k_max              28
_diffrn_reflns_limit_l_min              -8
_diffrn_reflns_limit_l_max              12
_diffrn_reflns_theta_min                2.5
_diffrn_reflns_theta_max                30.97
_diffrn_reflns_theta_full               30.97
_diffrn_measured_fraction_theta_max	0.997
_diffrn_measured_fraction_theta_full	0.997
_reflns_number_total                    2786
_reflns_number_gt                       1854
_reflns_threshold_expression            >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection              'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement              'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction               'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            SHELXL
_refine_ls_extinction_expression
Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef              0.000127(18)
_refine_ls_number_reflns                2786
_refine_ls_number_parameters            122
_refine_ls_number_restraints            1
_refine_ls_R_factor_gt                  0.0344
_refine_ls_wR_factor_ref                0.0933
_refine_ls_goodness_of_fit_ref          0.972
_refine_ls_restrained_S_all             0.972
_refine_ls_shift/su_max                 0
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack          0.43(2)
_refine_diff_density_max                1.742
_refine_diff_density_min                -1.539

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

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_
_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
_atom_site_disorder_group
_atom_site_disorder_assembly
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)


#------------------ MOLECULAR GEOMETRY --------------------------------------#

_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
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_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
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_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

#====end