#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/47/7204757.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_7204757
loop_
_publ_author_name
'Devic, Thomas'
'Canadell, Enric'
'Auban-Senzier, Pascale'
'Batail, Patrick'
_publ_section_title
;
 (EDT-TTF-I2)2PbI3�H2O: an ambient pressure metal with a ??
 donor slab topologyElectronic supplementary information (ESI)
 available: indexed X-ray powder diagram and chemical analysis results
 for [(C2H5)4N]PbI3. See http://www.rsc.org/suppdata/jm/b3/b312493b/
;
_journal_issue                   2
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              135
_journal_paper_doi               10.1039/b312493b
_journal_volume                  14
_journal_year                    2004
_chemical_formula_moiety         '2(C8H4S6I2), PbI3,H2O'
_chemical_formula_sum            'C8 H4 I3.5 O0.5 Pb0.5 S6'
_chemical_formula_weight         848.22
_chemical_name_common            '(EDT-TTF-I2)2, PbI3, H20'
_chemical_name_systematic
; 
 Bis(3,4-diiodo-3',4'-ethylenedithiotetrathiafulvalene), triiodolead(II), 
water
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.29(3)
_cell_angle_beta                 99.88(3)
_cell_angle_gamma                100.13(3)
_cell_formula_units_Z            4
_cell_length_a                   8.0312(16)
_cell_length_b                   12.130(2)
_cell_length_c                   20.777(4)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.05
_cell_volume                     1900.3(7)
_computing_cell_refinement       'CELL, Stoe-IPDS'
_computing_data_collection       'EXPOSE, Stoe-IPDS'
_computing_data_reduction        'INTEGRATE, Stoe-IPDS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       'rotation, phi incr. 1.1'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19480
_diffrn_reflns_theta_full        25.88
_diffrn_reflns_theta_max         25.88
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    10.800
_exptl_absorpt_correction_T_max  0.6805
_exptl_absorpt_correction_T_min  0.3817
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1514
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.038
_refine_diff_density_max         2.591
_refine_diff_density_min         -2.101
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         6881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0382P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                5135
_reflns_number_total             6881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b312493b.txt
_cod_data_source_block           tde242absm
_cod_original_cell_volume        1900.4(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C8 H4 I3.50 O0.50 Pb0.50 S6'
_cod_database_code               7204757
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.5000 0.0000 0.02569(12) Uani 1 2 d S . .
Pb2 Pb -0.5000 0.5000 0.0000 0.02475(12) Uani 1 2 d S . .
I1 I -0.18543(8) 0.71724(4) 0.02536(3) 0.03062(15) Uani 1 1 d . . .
I2 I -0.23129(9) 0.40106(5) 0.09513(3) 0.03354(16) Uani 1 1 d . . .
I3 I 0.33501(9) 0.62885(5) 0.11854(3) 0.03499(16) Uani 1 1 d . . .
I4 I 0.43865(8) 1.08022(5) -0.22755(3) 0.02666(14) Uani 1 1 d . . .
I5 I 0.21995(9) 0.77806(5) -0.21131(3) 0.03023(15) Uani 1 1 d . . .
S1 S 0.2462(3) 0.96531(17) -0.38555(10) 0.0270(5) Uani 1 1 d . . .
S2 S 0.0807(3) 0.73889(18) -0.37009(10) 0.0316(6) Uani 1 1 d . . .
C1 C 0.2824(11) 0.9428(7) -0.3037(4) 0.0213(18) Uani 1 1 d . . .
C2 C 0.2069(12) 0.8404(7) -0.2973(4) 0.025(2) Uani 1 1 d . . .
C3 C 0.1132(12) 0.8284(6) -0.4247(4) 0.025(2) Uani 1 1 d . . .
S3 S 0.0622(3) 0.87741(17) -0.54834(10) 0.0292(5) Uani 1 1 d . . .
S4 S -0.0882(3) 0.65160(17) -0.52716(10) 0.0304(6) Uani 1 1 d . . .
S5 S -0.0616(3) 0.81189(18) -0.69530(10) 0.0300(5) Uani 1 1 d . . .
S6 S -0.2236(4) 0.53824(18) -0.67197(11) 0.0350(6) Uani 1 1 d . . .
C4 C 0.0391(12) 0.7916(7) -0.4921(4) 0.025(2) Uani 1 1 d . . .
C5 C -0.0498(12) 0.7678(7) -0.6201(4) 0.024(2) Uani 1 1 d . . .
C6 C -0.1156(12) 0.6644(7) -0.6101(4) 0.0232(19) Uani 1 1 d . . .
C7 C -0.1606(13) 0.6782(7) -0.7592(4) 0.032(2) Uani 1 1 d . . .
H7A H -0.2089 0.6967 -0.8007 0.038 Uiso 1 1 calc R . .
H7B H -0.0715 0.6361 -0.7682 0.038 Uiso 1 1 calc R . .
C8 C -0.3015(12) 0.6012(8) -0.7396(4) 0.031(2) Uani 1 1 d . . .
H8A H -0.3624 0.5394 -0.7788 0.037 Uiso 1 1 calc R . .
H8B H -0.3841 0.6459 -0.7259 0.037 Uiso 1 1 calc R . .
I40 I -0.04823(8) 1.05405(5) -0.16903(3) 0.02799(14) Uani 1 1 d . . .
I50 I -0.25688(9) 0.76211(5) -0.14541(3) 0.03113(15) Uani 1 1 d . . .
S10 S -0.2472(3) 0.93422(17) -0.32647(10) 0.0289(5) Uani 1 1 d . . .
S20 S -0.4172(3) 0.71277(17) -0.30548(10) 0.0294(5) Uani 1 1 d . . .
S30 S -0.4277(4) 0.84405(18) -0.48626(10) 0.0341(6) Uani 1 1 d . . .
S40 S -0.5954(3) 0.62300(18) -0.46413(10) 0.0326(6) Uani 1 1 d . . .
S50 S -0.5471(4) 0.7764(2) -0.63370(11) 0.0381(6) Uani 1 1 d . . .
S60 S -0.7564(3) 0.51281(18) -0.60675(10) 0.0290(5) Uani 1 1 d . . .
C10 C -0.2045(12) 0.9148(7) -0.2444(4) 0.025(2) Uani 1 1 d . . .
C20 C -0.2814(12) 0.8136(7) -0.2359(4) 0.0226(19) Uani 1 1 d . . .
C30 C -0.3829(12) 0.7967(7) -0.3627(4) 0.0251(19) Uani 1 1 d . . .
C40 C -0.4569(13) 0.7594(7) -0.4291(4) 0.027(2) Uani 1 1 d . . .
C50 C -0.5467(12) 0.7355(7) -0.5575(4) 0.025(2) Uani 1 1 d . . .
C60 C -0.6240(12) 0.6351(7) -0.5478(4) 0.0231(19) Uani 1 1 d . . .
C70 C -0.7240(14) 0.6646(8) -0.6887(4) 0.035(2) Uani 1 1 d . . .
H70A H -0.8320 0.6796 -0.6779 0.042 Uiso 1 1 calc R . .
H70B H -0.7267 0.6690 -0.7349 0.042 Uiso 1 1 calc R . .
C80 C -0.7136(14) 0.5438(8) -0.6840(4) 0.035(2) Uani 1 1 d . . .
H80A H -0.5988 0.5325 -0.6880 0.042 Uiso 1 1 calc R . .
H80B H -0.7963 0.4890 -0.7217 0.042 Uiso 1 1 calc R . .
O1 O 0.744(4) 0.0677(16) -0.0048(10) 0.300(17) Uani 1 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 0.0000 0.0000 '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 0.0060 '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
I2 Pb1 I2 180.00(2) . 2_565 ?
I2 Pb1 I3 96.02(3) . . ?
I2 Pb1 I3 83.98(3) 2_565 . ?
I2 Pb1 I3 83.98(3) . 2_565 ?
I2 Pb1 I3 96.02(3) 2_565 2_565 ?
I3 Pb1 I3 180.0 . 2_565 ?
I2 Pb1 I1 94.92(3) . 2_565 ?
I2 Pb1 I1 85.08(3) 2_565 2_565 ?
I3 Pb1 I1 86.71(3) . 2_565 ?
I3 Pb1 I1 93.29(3) 2_565 2_565 ?
I2 Pb1 I1 85.08(3) . . ?
I2 Pb1 I1 94.92(3) 2_565 . ?
I3 Pb1 I1 93.29(3) . . ?
I3 Pb1 I1 86.71(3) 2_565 . ?
I1 Pb1 I1 180.0 2_565 . ?
I1 Pb2 I1 180.000(15) 2_465 . ?
I1 Pb2 I2 94.65(3) 2_465 . ?
I1 Pb2 I2 85.35(3) . . ?
I1 Pb2 I2 85.35(3) 2_465 2_465 ?
I1 Pb2 I2 94.65(3) . 2_465 ?
I2 Pb2 I2 180.0 . 2_465 ?
I1 Pb2 I3 87.14(3) 2_465 1_455 ?
I1 Pb2 I3 92.86(3) . 1_455 ?
I2 Pb2 I3 96.75(3) . 1_455 ?
I2 Pb2 I3 83.25(3) 2_465 1_455 ?
I1 Pb2 I3 92.86(3) 2_465 2_565 ?
I1 Pb2 I3 87.14(3) . 2_565 ?
I2 Pb2 I3 83.25(3) . 2_565 ?
I2 Pb2 I3 96.75(3) 2_465 2_565 ?
I3 Pb2 I3 180.000(14) 1_455 2_565 ?
Pb2 I1 Pb1 77.20(2) . . ?
Pb1 I2 Pb2 77.13(2) . . ?
Pb1 I3 Pb2 76.94(3) . 1_655 ?
C3 S1 C1 95.6(4) . . ?
C3 S2 C2 95.4(4) . . ?
C2 C1 S1 116.7(6) . . ?
C2 C1 I4 127.0(6) . . ?
S1 C1 I4 116.2(4) . . ?
C1 C2 S2 118.0(6) . . ?
C1 C2 I5 129.0(6) . . ?
S2 C2 I5 113.0(4) . . ?
C4 C3 S2 121.4(6) . . ?
C4 C3 S1 124.3(6) . . ?
S2 C3 S1 114.3(4) . . ?
C4 S3 C5 95.0(4) . . ?
C6 S4 C4 94.7(4) . . ?
C5 S5 C7 102.9(4) . . ?
C6 S6 C8 99.6(4) . . ?
C3 C4 S3 123.5(6) . . ?
C3 C4 S4 121.0(6) . . ?
S3 C4 S4 115.4(4) . . ?
C6 C5 S5 129.4(6) . . ?
C6 C5 S3 117.0(6) . . ?
S5 C5 S3 113.6(5) . . ?
C5 C6 S4 117.5(6) . . ?
C5 C6 S6 127.1(6) . . ?
S4 C6 S6 115.4(5) . . ?
C8 C7 S5 113.6(6) . . ?
C7 C8 S6 113.9(6) . . ?
C10 S10 C30 95.2(4) . . ?
C20 S20 C30 95.2(4) . . ?
C40 S30 C50 95.0(4) . . ?
C40 S40 C60 95.4(4) . . ?
C50 S50 C70 99.8(4) . . ?
C60 S60 C80 100.5(4) . . ?
C20 C10 S10 116.7(6) . . ?
C20 C10 I40 126.2(6) . . ?
S10 C10 I40 117.0(5) . . ?
C10 C20 S20 118.3(6) . . ?
C10 C20 I50 126.5(6) . . ?
S20 C20 I50 115.2(4) . . ?
C40 C30 S20 122.7(7) . . ?
C40 C30 S10 122.7(7) . . ?
S20 C30 S10 114.6(4) . . ?
C30 C40 S30 123.0(7) . . ?
C30 C40 S40 122.1(7) . . ?
S30 C40 S40 114.8(5) . . ?
C60 C50 S30 117.8(6) . . ?
C60 C50 S50 128.7(6) . . ?
S30 C50 S50 113.5(5) . . ?
C50 C60 S60 129.3(6) . . ?
C50 C60 S40 116.7(6) . . ?
S60 C60 S40 114.0(5) . . ?
C80 C70 S50 114.4(7) . . ?
C70 C80 S60 113.6(6) . . ?
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 3.2069(11) . ?
Pb1 I2 3.2069(11) 2_565 ?
Pb1 I3 3.2180(16) . ?
Pb1 I3 3.2180(16) 2_565 ?
Pb1 I1 3.2401(10) 2_565 ?
Pb1 I1 3.2401(10) . ?
Pb2 I1 3.1960(13) 2_465 ?
Pb2 I1 3.1960(13) . ?
Pb2 I2 3.2344(11) . ?
Pb2 I2 3.2344(11) 2_465 ?
Pb2 I3 3.2366(11) 1_455 ?
Pb2 I3 3.2366(11) 2_565 ?
I3 Pb2 3.2366(11) 1_655 ?
I4 C1 2.078(8) . ?
I5 C2 2.078(7) . ?
S1 C3 1.750(8) . ?
S1 C1 1.762(8) . ?
S2 C3 1.750(8) . ?
S2 C2 1.753(8) . ?
C1 C2 1.327(12) . ?
C3 C4 1.366(11) . ?
S3 C4 1.735(8) . ?
S3 C5 1.753(8) . ?
S4 C6 1.744(8) . ?
S4 C4 1.752(8) . ?
S5 C5 1.749(8) . ?
S5 C7 1.815(8) . ?
S6 C6 1.749(8) . ?
S6 C8 1.809(9) . ?
C5 C6 1.345(12) . ?
C7 C8 1.506(14) . ?
I40 C10 2.082(8) . ?
I50 C20 2.093(8) . ?
S10 C10 1.755(8) . ?
S10 C30 1.756(8) . ?
S20 C20 1.736(8) . ?
S20 C30 1.747(9) . ?
S30 C40 1.746(9) . ?
S30 C50 1.755(8) . ?
S40 C40 1.751(9) . ?
S40 C60 1.754(8) . ?
S50 C50 1.756(8) . ?
S50 C70 1.808(10) . ?
S60 C60 1.748(8) . ?
S60 C80 1.799(9) . ?
C10 C20 1.336(12) . ?
C30 C40 1.350(11) . ?
C50 C60 1.339(12) . ?
C70 C80 1.505(13) . ?
