#------------------------------------------------------------------------------
#$Date: 2020-10-06 13:04:14 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257732 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/91/7059178.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_7059178
loop_
_publ_author_name
'Yin, Wen-Yu'
'Weng, Yi-Gang'
'Jiang, Miao'
'Yu, Shuai-Kang'
'Zhu, Qin-Yu'
'Dai, Jie'
_publ_section_title
;
 (TMT--TTF)[Pb2.6/3□ 0.4/3I2]3: a TTF-intercalated two-dimensional
 hybrid lead iodide: crystal structure and properties
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1263
_journal_page_last               1268
_journal_paper_doi               10.1039/C9NJ04316K
_journal_volume                  44
_journal_year                    2020
_chemical_formula_sum            'C5 H6 I3 Pb1.3 S4'
_chemical_formula_weight         844.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-11-06 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.0050(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5549(14)
_cell_length_b                   4.5007(2)
_cell_length_c                   19.9119(9)
_cell_measurement_reflns_used    8864
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.3
_cell_volume                     1532.66(15)
_computing_cell_refinement       'Bruker ApexII'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'Bruker ApexII'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24096
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.064
_diffrn_reflns_theta_min         2.339
_exptl_absorpt_coefficient_mu    20.839
_exptl_absorpt_correction_T_max  0.124
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.659
_exptl_crystal_description       SHEET
_exptl_crystal_F_000             1462
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.651
_refine_diff_density_min         -1.597
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0175P)²+11.8398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1692
_reflns_number_total             2003
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj04316k2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7059178.cif.

 Adding full bibliography for 7059178.cif.
;
_cod_original_cell_volume        1532.66(14)
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_original_formula_sum        'C5 H6 I3 Pb1.30 S4'
_cod_database_code               7059178
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.103
_shelx_estimated_absorpt_t_max   0.230
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.000000 0.000000 0.000000 0.02981(17) Uani 0.6 4 d S T P . .
Pb2 Pb -0.27706(2) 0.000000 -0.36894(2) 0.02786(10) Uani 1 2 d S T P . .
I1 I -0.08883(3) 0.500000 0.04050(3) 0.03037(14) Uani 1 2 d S T P . .
I2 I -0.13401(3) 0.000000 -0.18143(3) 0.02454(12) Uani 1 2 d S T P . .
I3 I -0.18312(3) 0.500000 -0.39826(3) 0.03098(14) Uani 1 2 d S T P . .
S1 S 0.00228(16) -0.2910(8) -0.39846(16) 0.0353(7) Uani 0.5 1 d . . P A -1
S2 S 0.10685(16) -0.2580(8) -0.46379(16) 0.0358(7) Uani 0.5 1 d . . P A -1
C1 C 0.0845(5) 0(150) -0.3483(5) 0.084(5) Uani 0.5 1 d . . P A -1
C2 C 0.1334(5) 0(150) -0.3780(5) 0.060(3) Uani 0.5 1 d . . P A -1
C3 C 0.0229(6) -0.407(2) -0.4715(6) 0.036(4) Uani 0.5 1 d . . P A -1
S3 S 0.10260(17) -0.1056(7) -0.26172(16) 0.0375(8) Uani 0.5 1 d . . P . .
S4 S 0.21741(16) 0.1476(8) -0.33573(16) 0.0370(7) Uani 0.5 1 d . . P . .
C4 C 0.0241(6) 0.000000 -0.2471(5) 0.050(3) Uani 1 2 d S T P A .
H4A H 0.023228 0.216814 -0.243050 0.075 Uiso 0.5 1 calc R U P . .
H4B H 0.030446 -0.090536 -0.199677 0.075 Uiso 0.5 1 calc R U P . .
H4C H -0.025196 -0.067531 -0.290582 0.075 Uiso 0.5 1 calc R U P . .
C5 C 0.2590(5) 0.000000 -0.3969(5) 0.068(4) Uani 1 2 d S T P A .
H5A H 0.270195 -0.212475 -0.386741 0.102 Uiso 0.5 1 calc R U P . .
H5B H 0.307427 0.106380 -0.384585 0.102 Uiso 0.5 1 calc R U P . .
H5C H 0.221056 0.029319 -0.451265 0.102 Uiso 0.5 1 calc R U 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'
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_
_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
I1 Pb1 I1 89.789(13) . 5_565
I1 Pb1 I1 90.211(13) . 1_545
I1 Pb1 I1 180.000(17) 5_565 1_545
I1 Pb1 I1 180.0 . 5
I1 Pb1 I1 90.211(13) 5_565 5
I1 Pb1 I1 89.789(13) 1_545 5
I1 Pb1 I2 92.091(11) . .
I1 Pb1 I2 87.909(11) 5_565 .
I1 Pb1 I2 92.091(11) 1_545 .
I1 Pb1 I2 87.909(11) 5 .
I1 Pb1 I2 87.908(11) . 5
I1 Pb1 I2 92.092(11) 5_565 5
I1 Pb1 I2 87.908(11) 1_545 5
I1 Pb1 I2 92.092(11) 5 5
I2 Pb1 I2 180.0 . 5
I3 Pb2 I3 91.797(15) . 1_545
I3 Pb2 I1 93.043(14) . 7_454
I3 Pb2 I1 93.043(14) 1_545 7_454
I3 Pb2 I2 173.738(15) . 7_444
I3 Pb2 I2 90.571(9) 1_545 7_444
I1 Pb2 I2 92.620(13) 7_454 7_444
I3 Pb2 I2 90.570(9) . 7_454
I3 Pb2 I2 173.738(15) 1_545 7_454
I1 Pb2 I2 92.620(13) 7_454 7_454
I2 Pb2 I2 86.501(13) 7_444 7_454
I3 Pb2 I2 87.719(14) . .
I3 Pb2 I2 87.719(14) 1_545 .
I1 Pb2 I2 178.904(16) 7_454 .
I2 Pb2 I2 86.583(12) 7_444 .
I2 Pb2 I2 86.583(12) 7_454 .
Pb2 I1 Pb1 89.704(12) 7_454 1_565
Pb2 I1 Pb1 89.704(12) 7_454 .
Pb1 I1 Pb1 90.211(13) 1_565 .
Pb1 I2 Pb2 85.532(11) . 7_444
Pb1 I2 Pb2 85.532(11) . 7_454
Pb2 I2 Pb2 86.502(13) 7_444 7_454
Pb1 I2 Pb2 178.555(16) . .
Pb2 I2 Pb2 93.418(12) 7_444 .
Pb2 I2 Pb2 93.418(12) 7_454 .
Pb2 I3 Pb2 91.798(16) 1_565 .
C3 S1 C1 99(10) . .
C3 S2 C2 99(10) . .
C2 C1 S3 128(10) . .
C2 C1 S1 111(10) . .
S3 C1 S1 93(10) . .
C1 C2 S4 123(10) . .
C1 C2 S2 117(10) . .
S4 C2 S2 119(10) . .
S2 C3 S1 113.7(6) . .
S3 S3 C1 73(10) 6 .
S3 S3 C4 74.35(12) 6 .
C1 S3 C4 109(10) . .
S3 S3 H4A 105.86(17) 6 6
C1 S3 H4A 121(10) . 6
C4 S3 H4A 31.6(3) . 6
S4 S4 C2 65(10) 6 .
S4 S4 C5 69.35(14) 6 .
C2 S4 C5 100(10) . .
S4 S4 H5A 99.4(7) 6 6
C2 S4 H5A 120(10) . 6
C5 S4 H5A 30.8(14) . 6
S3 C4 H4A 109.5 . .
S3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
S3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
S3 C4 H4A 78.24(13) . 6
H4A C4 H4A 169.4 . 6
H4B C4 H4A 60.3 . 6
H4C C4 H4A 73.5 . 6
S3 C4 H4B 123.9(5) . 6
H4A C4 H4B 60.3 . 6
H4B C4 H4B 49.1 . 6
H4C C4 H4B 126.2 . 6
H4A C4 H4B 109.5 6 6
S3 C4 H4C 120.0(11) . 6
H4A C4 H4C 73.5 . 6
H4B C4 H4C 126.2 . 6
H4C C4 H4C 36.1 . 6
H4A C4 H4C 109.5 6 6
H4B C4 H4C 109.5 6 6
S4 C5 H5A 109.5 . .
S4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
S4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
S4 C5 H5A 69.21(15) . 6
H5A C5 H5A 154.7 . 6
H5B C5 H5A 51.7 . 6
H5C C5 H5A 94.0 . 6
S4 C5 H5B 132.7(4) . 6
H5A C5 H5B 51.7 . 6
H5B C5 H5B 58.5 . 6
H5C C5 H5B 117.7 . 6
H5A C5 H5B 109.5 6 6
S4 C5 H5C 115(4) . 6
H5A C5 H5C 94.0 . 6
H5B C5 H5C 117.7 . 6
H5C C5 H5C 15.5 . 6
H5A C5 H5C 109.5 6 6
H5B C5 H5C 109.5 6 6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.1766(4) .
Pb1 I1 3.1766(4) 5_565
Pb1 I1 3.1766(4) 1_545
Pb1 I1 3.1766(4) 5
Pb1 I2 3.2768(5) .
Pb1 I2 3.2768(5) 5
Pb2 I3 3.1337(4) .
Pb2 I3 3.1338(4) 1_545
Pb2 I1 3.1400(6) 7_454
Pb2 I2 3.2843(4) 7_444
Pb2 I2 3.2843(4) 7_454
Pb2 I2 3.4113(6) .
S1 C3 1.766(11) .
S1 C1 2(10) .
S2 C3 1.710(11) .
S2 C2 2(10) .
C1 C2 1(3) .
C1 S3 2(10) .
C2 S4 2(10) .
S3 S3 0.950(6) 6
S3 C4 1.761(8) .
S3 H4A 1.832(9) 6
S4 S4 1.328(7) 6
S4 C5 1.884(9) .
S4 H5A 1.789(12) 6
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C4 H4A 0.980(9) 6
C4 H4B 0.98(5) 6
C4 H4C 0.98(4) 6
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C5 H5A 0.98(5) 6
C5 H5B 0.98(9) 6
C5 H5C 0.98(3) 6
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
S3 C1 C2 S4 -51(100) .
S1 C1 C2 S4 -163(100) .
S3 C1 C2 S2 116(100) .
S1 C1 C2 S2 4(100) .
C2 S2 C3 S1 -4(100) .
C1 S1 C3 S2 6(100) .
C2 C1 S3 S3 104(100) 6
S1 C1 S3 S3 -136(100) 6
C2 C1 S3 C4 170(100) .
S1 C1 S3 C4 -70(100) .
C1 C2 S4 S4 107(100) 6
S2 C2 S4 S4 -60(100) 6
C1 C2 S4 C5 169(100) .
S2 C2 S4 C5 2(100) .
