#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:35:27 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179755 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/51/7005152.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_7005152
loop_
_publ_author_name
'Louvain, Nicolas'
'Bi, Wenhua'
'Mercier, Nicolas'
'Buzaré, Jean-Yves'
'Legein, Christophe'
'Corbel, Gwenaël'
_publ_section_title
;
 PbnI4n+2(2n+2)- ribbons (n = 3, 5) as dimensional reductions of 2D
 perovskite layers in cystamine cation based hybrids, also
 incorporating iodine molecules or reversible guest water molecules.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              965
_journal_page_last               970
_journal_paper_doi               10.1039/b617225c
_journal_year                    2007
_chemical_formula_moiety         'C24 H88 I22 N12 O2 Pb5 S12'
_chemical_formula_sum            'C24 H88 I22 N12 O2 Pb5 S12'
_chemical_formula_weight         4789.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2006-06-22T11:36:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.3660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.25610(10)
_cell_length_b                   8.77790(10)
_cell_length_c                   25.57040(10)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     5134.74(7)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      353(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            101625
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    15.057
_exptl_absorpt_correction_T_max  0.513
_exptl_absorpt_correction_T_min  0.1784
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.102
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4212
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.5
_refine_diff_density_min         -1.28
_refine_ls_extinction_coef       0.000017(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         14785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0241P)²+36.4307P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                7310
_reflns_number_total             14785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b617225c.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7005152
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
_atom_site_disorder_group
_atom_site_disorder_assembly
Pb1 Pb 1 0 1 0.03522(12) Uani 1 d S . .
Pb2 Pb 0.836922(16) 0.50588(4) 0.856299(13) 0.03826(10) Uani 1 d . . .
Pb3 Pb 0.665008(17) -0.00273(4) 0.731196(15) 0.04450(11) Uani 1 d . . .
I1 I 1.09110(3) -0.07554(8) 0.92392(3) 0.05410(19) Uani 1 d . . .
I2 I 0.93785(3) 0.26415(8) 0.92239(3) 0.05185(19) Uani 1 d . . .
I3 I 0.91703(4) 0.75445(8) 0.93327(3) 0.0681(2) Uani 1 d . . .
I4 I 0.89436(3) 0.56408(10) 0.75223(3) 0.0645(2) Uani 1 d . . .
I5 I 0.75094(4) 0.76302(9) 0.81345(3) 0.0728(3) Uani 1 d . . .
I6 I 0.77023(4) 0.44058(10) 0.95221(3) 0.0654(2) Uani 1 d . . .
I7 I 0.75463(4) 0.26746(9) 0.79154(3) 0.0708(2) Uani 1 d . . .
I8 I 0.74858(3) -0.05916(10) 0.64777(3) 0.0640(2) Uani 1 d . . .
I9 I 0.59502(4) 0.24315(9) 0.65736(3) 0.0662(2) Uani 1 d . . .
I10 I 0.58604(4) 0.02237(11) 0.82140(3) 0.0800(3) Uani 1 d . . .
I11 I 0.58979(4) -0.26305(9) 0.67575(3) 0.0659(2) Uani 1 d . . .
N1 N 0.0210(5) 0.4115(14) 0.7009(4) 0.102(4) Uani 1 d . . .
H1A H 0.0379 0.3229 0.7113 0.153 Uiso 1 calc R . .
H1B H -0.0007 0.4011 0.6687 0.153 Uiso 1 calc R . .
H1C H -0.0015 0.4405 0.7238 0.153 Uiso 1 calc R . .
C1 C 0.0633(9) 0.5196(18) 0.6992(5) 0.129(7) Uani 1 d . . .
H1D H 0.0444 0.6172 0.6907 0.155 Uiso 1 calc R . .
H1E H 0.0841 0.494 0.6707 0.155 Uiso 1 calc R . .
C2 C 0.1061(5) 0.5355(13) 0.7489(4) 0.072(4) Uani 1 d . . .
H2D H 0.1392 0.5932 0.7412 0.087 Uiso 1 calc R . .
H2E H 0.1202 0.4348 0.7603 0.087 Uiso 1 calc R . .
S1 S 0.07995(14) 0.6269(3) 0.80333(11) 0.0604(8) Uani 1 d . . .
S2 S 0.03554(12) 0.4614(3) 0.83539(10) 0.0527(7) Uani 1 d . . .
C3 C 0.0925(4) 0.3630(12) 0.8803(4) 0.053(3) Uani 1 d . . .
H3A H 0.0752 0.276 0.895 0.063 Uiso 1 calc R . .
H3B H 0.1207 0.3243 0.8599 0.063 Uiso 1 calc R . .
C4 C 0.1237(5) 0.4547(12) 0.9245(4) 0.059(3) Uani 1 d . . .
H4A H 0.1443 0.5369 0.9105 0.071 Uiso 1 calc R . .
H4B H 0.1525 0.3915 0.9468 0.071 Uiso 1 calc R . .
N2 N 0.0831(4) 0.5193(10) 0.9570(3) 0.067(3) Uani 1 d . . .
H2A H 0.0611 0.5908 0.9385 0.101 Uiso 1 calc R . .
H2B H 0.1034 0.5602 0.9865 0.101 Uiso 1 calc R . .
H2C H 0.0602 0.4457 0.9657 0.101 Uiso 1 calc R . .
N3 N 0.7357(4) 0.5353(11) 0.6800(3) 0.077(3) Uani 1 d . . .
H3C H 0.7054 0.5873 0.6626 0.115 Uiso 1 calc R . .
H3D H 0.7585 0.5973 0.7022 0.115 Uiso 1 calc R . .
H3E H 0.7229 0.4603 0.6983 0.115 Uiso 1 calc R . .
C5 C 0.7689(6) 0.4716(17) 0.6424(5) 0.094(5) Uani 1 d . . .
H5A H 0.7914 0.553 0.6302 0.113 Uiso 1 calc R . .
H5B H 0.7964 0.3984 0.661 0.113 Uiso 1 calc R . .
C6 C 0.7360(6) 0.3984(15) 0.5970(5) 0.082(4) Uani 1 d . . A
H6A H 0.7196 0.3059 0.6089 0.098 Uiso 1 calc R . .
H6B H 0.763 0.3681 0.574 0.098 Uiso 1 calc R . .
S3 S 0.67948(16) 0.5001(5) 0.55873(13) 0.0878(11) Uani 1 d . . .
S4A S 0.7130(13) 0.646(3) 0.5237(9) 0.181(12) Uani 0.5 d P 1 A
S4B S 0.7231(8) 0.674(2) 0.5215(5) 0.075(3) Uani 0.5 d P 2 A
C7 C 0.7167(8) 0.583(2) 0.4557(5) 0.128(6) Uani 1 d . . .
H7A1 H 0.6772 0.6008 0.4369 0.153 Uiso 1 calc R 1 A
H7B1 H 0.7401 0.6616 0.4432 0.153 Uiso 1 calc R 1 A
H7A2 H 0.6885 0.502 0.4494 0.153 Uiso 1 d R 2 A
H7B2 H 0.7085 0.6607 0.428 0.153 Uiso 1 d R 2 A
C8A C 0.7328(18) 0.455(3) 0.431(3) 0.23(4) Uani 0.55(4) d P 1 A
H8A1 H 0.7265 0.3658 0.4522 0.275 Uiso 0.55(4) calc PR 1 A
H8B1 H 0.7085 0.4445 0.3966 0.275 Uiso 0.55(4) calc PR 1 A
C8B C 0.7753(14) 0.543(4) 0.4650(11) 0.068(12) Uani 0.45(4) d P 2 A
H8A2 H 0.7987 0.6356 0.469 0.081 Uiso 0.45(4) calc PR 2 A
H8B2 H 0.7842 0.487 0.4981 0.081 Uiso 0.45(4) calc PR 2 A
N4 N 0.7895(8) 0.4602(15) 0.4262(9) 0.204(10) Uani 1 d . . .
H4C1 H 0.8 0.3707 0.4145 0.306 Uiso 1 calc R 1 A
H4D1 H 0.8116 0.4806 0.4576 0.306 Uiso 1 calc R 1 A
H4E1 H 0.7943 0.5328 0.4031 0.306 Uiso 1 calc R 1 A
H4C2 H 0.8265 0.4288 0.4325 0.306 Uiso 1 d R 2 A
H4D2 H 0.7835 0.5194 0.3975 0.306 Uiso 1 d R 2 A
H4E2 H 0.7659 0.3798 0.4208 0.306 Uiso 1 d R 2 A
N5 N 0.6135(5) 0.5485(12) 1.0587(4) 0.084(3) Uani 1 d . . .
H5C H 0.5813 0.5935 1.0414 0.126 Uiso 1 calc R . .
H5D H 0.6387 0.6191 1.0735 0.126 Uiso 1 calc R . .
H5E H 0.6042 0.488 1.0838 0.126 Uiso 1 calc R . .
C9 C 0.6396(6) 0.4593(16) 1.0219(5) 0.082(4) Uani 1 d . . .
H9A H 0.6675 0.3888 1.0418 0.099 Uiso 1 calc R . .
H9B H 0.6608 0.5264 1.002 0.099 Uiso 1 calc R . .
C10 C 0.5966(7) 0.3739(15) 0.9850(6) 0.106(5) Uani 1 d . . .
H10A H 0.5761 0.3069 1.0055 0.127 Uiso 1 calc R . .
H10B H 0.6175 0.3099 0.9637 0.127 Uiso 1 calc R . .
S5 S 0.54345(16) 0.4809(6) 0.94075(15) 0.1230(18) Uani 1 d . . .
S6 S 0.58998(18) 0.6248(5) 0.90497(13) 0.0897(11) Uani 1 d . . .
C11 C 0.6083(7) 0.5117(16) 0.8488(6) 0.104(5) Uiso 1 d . . .
H11A H 0.6374 0.5697 0.8344 0.125 Uiso 1 calc R . .
H11B H 0.6276 0.42 0.8641 0.125 Uiso 1 calc R . .
C12 C 0.5628(8) 0.461(2) 0.8014(7) 0.135(6) Uiso 1 d . . .
H12A H 0.5813 0.4226 0.773 0.162 Uiso 1 calc R . .
H12B H 0.5375 0.3829 0.8116 0.162 Uiso 1 calc R . .
N6 N 0.5322(6) 0.5928(17) 0.7865(5) 0.146(5) Uiso 1 d . . .
H6C H 0.5216 0.6355 0.8149 0.219 Uiso 1 calc R . .
H6D H 0.5005 0.571 0.7626 0.219 Uiso 1 calc R . .
H6E H 0.5548 0.6572 0.7724 0.219 Uiso 1 calc R . .
O1 O 0.5278(11) 0.874(3) 1.0020(10) 0.362(13) Uiso 1 d . . .
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'
O O 0.0106 0.006 '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
_geom_angle_publ_flag
I3 Pb1 I3 180 1_545 3_767 ?
I3 Pb1 I1 93.59(2) 1_545 3_757 ?
I3 Pb1 I1 86.41(2) 3_767 3_757 ?
I3 Pb1 I1 86.41(2) 1_545 . ?
I3 Pb1 I1 93.59(2) 3_767 . ?
I1 Pb1 I1 180.0000(10) 3_757 . ?
I3 Pb1 I2 89.748(19) 1_545 . ?
I3 Pb1 I2 90.252(19) 3_767 . ?
I1 Pb1 I2 87.280(17) 3_757 . ?
I1 Pb1 I2 92.720(17) . . ?
I3 Pb1 I2 90.252(19) 1_545 3_757 ?
I3 Pb1 I2 89.748(19) 3_767 3_757 ?
I1 Pb1 I2 92.720(17) 3_757 3_757 ?
I1 Pb1 I2 87.280(17) . 3_757 ?
I2 Pb1 I2 180 . 3_757 ?
I5 Pb2 I7 90.33(3) . . ?
I5 Pb2 I6 91.77(2) . . ?
I7 Pb2 I6 87.16(2) . . ?
I5 Pb2 I4 85.94(2) . . ?
I7 Pb2 I4 88.50(2) . . ?
I6 Pb2 I4 175.08(2) . . ?
I5 Pb2 I3 89.33(2) . . ?
I7 Pb2 I3 174.87(2) . . ?
I6 Pb2 I3 87.73(2) . . ?
I4 Pb2 I3 96.59(2) . . ?
I5 Pb2 I2 169.82(2) . . ?
I7 Pb2 I2 98.59(2) . . ?
I6 Pb2 I2 83.83(2) . . ?
I4 Pb2 I2 99.11(2) . . ?
I3 Pb2 I2 81.35(2) . . ?
I11 Pb3 I9 92.50(2) . . ?
I11 Pb3 I8 86.58(2) . . ?
I9 Pb3 I8 90.98(2) . . ?
I11 Pb3 I10 91.77(2) . . ?
I9 Pb3 I10 94.80(2) . . ?
I8 Pb3 I10 174.05(3) . . ?
I11 Pb3 I5 93.40(2) . 1_545 ?
I9 Pb3 I5 173.83(3) . 1_545 ?
I8 Pb3 I5 87.58(2) . 1_545 ?
I10 Pb3 I5 86.82(2) . 1_545 ?
I11 Pb3 I7 176.33(3) . . ?
I9 Pb3 I7 90.15(2) . . ?
I8 Pb3 I7 90.84(2) . . ?
I10 Pb3 I7 90.54(2) . . ?
I5 Pb3 I7 83.88(2) 1_545 . ?
Pb1 I2 Pb2 162.50(3) . . ?
Pb1 I3 Pb2 175.35(3) 1_565 . ?
Pb2 I5 Pb3 162.14(3) . 1_565 ?
Pb2 I7 Pb3 175.34(3) . . ?
N1 C1 C2 114.6(12) . . ?
C1 C2 S1 116.0(11) . . ?
C2 S1 S2 105.0(4) . . ?
C3 S2 S1 103.3(4) . . ?
C4 C3 S2 115.6(8) . . ?
C3 C4 N2 111.3(9) . . ?
C6 C5 N3 116.4(12) . . ?
C5 C6 S3 117.9(10) . . ?
C6 S3 S4A 107.0(10) . . ?
C6 S3 S4B 104.2(7) . . ?
S4A S3 S4B 3.4(11) . . ?
S3 S4A C7 110.4(14) . . ?
C7 S4B S3 97.4(9) . . ?
C8A C7 C8B 62(2) . . ?
C8A C7 S4A 138(3) . . ?
C8B C7 S4A 97.2(17) . . ?
C8A C7 S4B 142(3) . . ?
C8B C7 S4B 92.1(16) . . ?
S4A C7 S4B 10.9(14) . . ?
N4 C8A C7 112(4) . . ?
N4 C8B C7 112(2) . . ?
C8B N4 C8A 64(3) . . ?
N5 C9 C10 112.5(12) . . ?
C9 C10 S5 117.2(10) . . ?
C10 S5 S6 104.7(5) . . ?
C11 S6 S5 103.6(5) . . ?
C12 C11 S6 123.2(12) . . ?
N6 C12 C11 103.0(15) . . ?
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 I3 3.1775(7) 1_545 ?
Pb1 I3 3.1775(7) 3_767 ?
Pb1 I1 3.1931(7) 3_757 ?
Pb1 I1 3.1931(7) . ?
Pb1 I2 3.2205(6) . ?
Pb1 I2 3.2205(6) 3_757 ?
Pb2 I5 3.0831(8) . ?
Pb2 I7 3.1055(8) . ?
Pb2 I6 3.1808(8) . ?
Pb2 I4 3.2258(8) . ?
Pb2 I3 3.2841(8) . ?
Pb2 I2 3.3824(7) . ?
Pb3 I11 3.0658(8) . ?
Pb3 I9 3.1251(8) . ?
Pb3 I8 3.1726(8) . ?
Pb3 I10 3.2041(9) . ?
Pb3 I5 3.3366(8) 1_545 ?
Pb3 I7 3.3455(8) . ?
I3 Pb1 3.1775(7) 1_565 ?
I5 Pb3 3.3366(8) 1_565 ?
N1 C1 1.373(16) . ?
C1 C2 1.471(18) . ?
C2 S1 1.805(11) . ?
S1 S2 2.038(4) . ?
S2 C3 1.808(10) . ?
C3 C4 1.470(13) . ?
C4 N2 1.480(12) . ?
N3 C5 1.449(14) . ?
C5 C6 1.423(16) . ?
C6 S3 1.737(13) . ?
S3 S4A 1.82(3) . ?
S3 S4B 2.15(2) . ?
S4A C7 1.84(2) . ?
S4B C7 1.85(2) . ?
C7 C8A 1.37(4) . ?
C7 C8B 1.38(3) . ?
C8A N4 1.35(3) . ?
C8B N4 1.32(3) . ?
N5 C9 1.438(14) . ?
C9 C10 1.454(17) . ?
C10 S5 1.785(15) . ?
S5 S6 1.990(5) . ?
S6 C11 1.857(14) . ?
C11 C12 1.52(2) . ?
C12 N6 1.375(19) . ?
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 I4 2_646 0.89 2.83 3.709(12) 172.3
N1 H1B I1 2_656 0.89 2.88 3.743(10) 164.5
N1 H1C S2 . 0.89 2.83 3.422(10) 124.9
N1 H1C I4 1_455 0.89 2.86 3.686(12) 154.2
N2 H2A I1 1_465 0.89 3.05 3.668(9) 128.4
N2 H2B I6 3_667 0.89 3.07 3.782(10) 138.2
N2 H2B I2 3_667 0.89 3.09 3.728(8) 130.5
N2 H2C I3 3_667 0.89 3.09 3.694(8) 126.9
N3 H3C S3 . 0.89 2.72 3.156(10) 111.1
N3 H3C I11 1_565 0.89 3.06 3.812(10) 142.8
N3 H3E I7 . 0.89 2.91 3.661(9) 143.3
N4 H4E2 I6 4_565 0.89 2.92 3.623(13) 136.9
N4 H4D2 I5 4_575 0.89 2.87 3.754(17) 170.6
N4 H4D2 I5 4_575 0.89 2.87 3.754(17) 170.6
N4 H4E2 I6 4_565 0.89 2.92 3.623(13) 136.9
N5 H5C S5 . 0.89 2.75 3.214(10) 113.9
N5 H5D I8 4_566 0.89 2.94 3.535(10) 125.4
N5 H5E I9 4_566 0.89 2.8 3.674(10) 167.2
N6 H6C S6 . 0.89 2.55 3.097(14) 120
N6 H6C I9 2_656 0.89 3.07 3.754(14) 134.7
N6 H6D I10 2_656 0.89 2.7 3.582(14) 171
N6 H6E I11 1_565 0.89 2.83 3.575(14) 142.6
