#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:42:49 +0200 (lun 05 de jul de 2021) $
#$Revision: 267189 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/72/7707262.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_7707262
loop_
_publ_author_name
'Yin, Wen-Yu'
'Weng, Yi-Gang'
'Ren, Zhou-Hong'
'Zhang, Zhi-Ruo'
'Zhu, Qin-Yu'
'Dai, Jie'
_publ_section_title
;
 Tetrathiafulvalene-based double metal lead iodides: structures and
 electrical properties.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8120
_journal_page_last               8126
_journal_paper_doi               10.1039/d1dt00631b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'Cu2 I10 Pb2, 5(C6 H4 S4), 0.5(H4 O2)'
_chemical_formula_sum            'C30 H22 Cu2 I10 O Pb2 S20'
_chemical_formula_weight         2850.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-03-15
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.02.10 svn.rb'16c95d35' for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-04-19 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                86.986(4)
_cell_angle_beta                 70.722(4)
_cell_angle_gamma                80.970(4)
_cell_formula_units_Z            1
_cell_length_a                   10.9196(19)
_cell_length_b                   11.281(2)
_cell_length_c                   13.700(2)
_cell_measurement_reflns_used    7639
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.41
_cell_volume                     1573.2(5)
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      213.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7015
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         1.575
_exptl_absorpt_coefficient_mu    11.600
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4979
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.008
_exptl_crystal_description       rod
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.878
_refine_diff_density_min         -2.520
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         7015
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0744P)²+10.2386P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5679
_reflns_number_total             7015
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00631b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7707262--7707265.cif.'
_cod_original_cell_volume        1573.3(5)
_cod_database_code               7707262
_shelx_shelxl_version_number     2018/3
_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_max   0.457
_shelx_estimated_absorpt_t_min   0.205
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.855(3)
 0.145(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Rigid body (RIGU) restrains
 S9, C13, C14, S10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
 Fixed Uiso: O1(0.07)
5.a Riding coordinates:
 O1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_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
Cu1 Cu 0.05330(16) 0.80206(15) 0.01916(12) 0.0519(4) Uani 1 1 d . . . . .
Pb1 Pb 0.19394(4) 0.98964(3) -0.18644(3) 0.02797(12) Uani 1 1 d . . . . .
I1 I -0.13165(6) 0.71332(6) 0.14895(5) 0.03035(16) Uani 1 1 d . . . . .
I2 I 0.17952(6) 0.70475(6) -0.15365(5) 0.03174(16) Uani 1 1 d . . . . .
I3 I 0.14353(7) 0.97340(6) 0.07867(5) 0.03099(16) Uani 1 1 d . . . . .
I4 I 0.16848(7) 0.99666(6) -0.40034(6) 0.03600(17) Uani 1 1 d . . . . .
I5 I 0.49021(8) 0.98522(7) -0.25717(7) 0.0436(2) Uani 1 1 d . . . . .
S1 S -0.0089(3) 0.4470(3) 0.3237(2) 0.0344(6) Uani 1 1 d . . . . .
S2 S 0.1885(3) 0.3501(3) 0.4185(2) 0.0391(6) Uani 1 1 d . . . . .
S3 S 0.0809(3) 0.7119(2) 0.3166(2) 0.0347(6) Uani 1 1 d . . . . .
S4 S 0.2746(3) 0.6100(3) 0.4129(2) 0.0349(6) Uani 1 1 d . . . . .
S5 S 0.2130(3) 0.4309(2) 0.0812(2) 0.0331(6) Uani 1 1 d . . . . .
S6 S 0.4045(3) 0.3032(2) 0.1718(2) 0.0322(6) Uani 1 1 d . . . . .
S7 S 0.3262(3) 0.6763(2) 0.0846(2) 0.0331(6) Uani 1 1 d . . . . .
S8 S 0.5133(2) 0.5516(2) 0.1796(2) 0.0347(6) Uani 1 1 d . . . . .
S9 S 0.5615(3) 0.3278(2) 0.4171(2) 0.0363(6) Uani 1 1 d . . . . .
S10 S 0.3581(2) 0.4039(2) 0.6159(2) 0.0299(5) Uani 1 1 d . . . . .
C1 C -0.0001(12) 0.2980(11) 0.3565(9) 0.042(3) Uani 1 1 d . . . . .
H1 H -0.055908 0.249601 0.343884 0.051 Uiso 1 1 calc R U . . .
C2 C 0.0907(14) 0.2531(12) 0.4013(10) 0.048(3) Uani 1 1 d . . . . .
H2 H 0.099884 0.172391 0.422160 0.057 Uiso 1 1 calc R U . . .
C3 C 0.1149(9) 0.4728(9) 0.3685(8) 0.028(2) Uani 1 1 d . . . . .
C4 C 0.1544(9) 0.5858(9) 0.3650(8) 0.027(2) Uani 1 1 d . . . . .
C5 C 0.1729(11) 0.8097(10) 0.3440(9) 0.038(2) Uani 1 1 d . . . . .
H5 H 0.160353 0.891957 0.328523 0.045 Uiso 1 1 calc R U . . .
C6 C 0.2628(11) 0.7630(10) 0.3881(9) 0.039(3) Uani 1 1 d . . . . .
H6 H 0.316457 0.810626 0.404683 0.046 Uiso 1 1 calc R U . . .
C7 C 0.2139(12) 0.2785(10) 0.0996(10) 0.041(3) Uani 1 1 d . . . . .
H7 H 0.155460 0.238227 0.081465 0.049 Uiso 1 1 calc R U . . .
C8 C 0.3010(11) 0.2204(10) 0.1406(9) 0.038(3) Uani 1 1 d . . . . .
H8 H 0.306495 0.137191 0.152317 0.045 Uiso 1 1 calc R U . . .
C9 C 0.3389(10) 0.4381(9) 0.1287(8) 0.029(2) Uani 1 1 d . . . . .
C10 C 0.3900(9) 0.5435(9) 0.1290(8) 0.028(2) Uani 1 1 d . . . . .
C11 C 0.4303(11) 0.7594(10) 0.1117(10) 0.039(3) Uani 1 1 d . . . . .
H11 H 0.426294 0.841943 0.096661 0.047 Uiso 1 1 calc R U . . .
C12 C 0.5167(11) 0.7034(10) 0.1547(10) 0.039(3) Uani 1 1 d . . . . .
H12 H 0.576458 0.744149 0.170726 0.047 Uiso 1 1 calc R U . . .
C13 C 0.4710(13) 0.2268(12) 0.4879(11) 0.049(3) Uani 1 1 d . . . . .
H13 H 0.485361 0.147539 0.464007 0.059 Uiso 1 1 calc R U . . .
C14 C 0.3811(12) 0.2578(10) 0.5756(11) 0.042(2) Uani 1 1 d . . . . .
H14 H 0.330015 0.201956 0.615987 0.051 Uiso 1 1 calc R U . . .
C15 C 0.4832(8) 0.4435(8) 0.5075(7) 0.0216(18) Uani 1 1 d . . . . .
O1 O 0.500000 0.000000 0.500000 0.070 Uiso 1 2 d S U P . .
H1A H 0.515100 -0.028080 0.439310 0.105 Uiso 0.5 1 d R U P . .
H1B H 0.573210 -0.000540 0.510980 0.105 Uiso 0.5 1 d 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'
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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
I1 Cu1 I2 121.95(6) . . y
I1 Cu1 I3 118.23(6) . . y
I2 Cu1 I3 118.77(6) . . y
I2 Pb1 I1 161.83(2) . 2_575 y
I4 Pb1 I1 96.28(2) . 2_575 y
I4 Pb1 I2 94.56(2) . . y
I4 Pb1 I5 96.58(3) . . y
I5 Pb1 I1 93.17(2) . 2_575 y
I5 Pb1 I2 100.03(2) . . y
Cu1 I1 Pb1 72.86(4) . 2_575 ?
Cu1 I2 Pb1 73.79(4) . . ?
C1 S1 C3 95.1(5) . . ?
C3 S2 C2 95.1(6) . . ?
C4 S3 C5 95.2(5) . . ?
C4 S4 C6 96.0(5) . . ?
C9 S5 C7 95.3(5) . . ?
C9 S6 C8 94.0(5) . . ?
C10 S7 C11 94.6(5) . . ?
C10 S8 C12 94.9(5) . . ?
C13 S9 C15 93.4(6) . . ?
C14 S10 C15 93.2(6) . . ?
C2 C1 S1 117.1(9) . . ?
C1 C2 S2 117.1(10) . . ?
S2 C3 S1 115.6(6) . . ?
C4 C3 S1 123.1(8) . . ?
C4 C3 S2 121.3(7) . . ?
S4 C4 S3 115.2(6) . . ?
C3 C4 S3 122.5(7) . . ?
C3 C4 S4 122.2(8) . . ?
C6 C5 S3 117.2(9) . . ?
C5 C6 S4 116.4(9) . . ?
C8 C7 S5 117.1(8) . . ?
C7 C8 S6 117.9(9) . . ?
S5 C9 S6 115.7(5) . . ?
C10 C9 S5 122.7(8) . . ?
C10 C9 S6 121.5(8) . . ?
S7 C10 S8 115.9(6) . . ?
C9 C10 S7 121.2(8) . . ?
C9 C10 S8 122.7(8) . . ?
C12 C11 S7 118.0(9) . . ?
C11 C12 S8 116.5(8) . . ?
C14 C13 S9 120.2(11) . . ?
C13 C14 S10 118.2(11) . . ?
S10 C15 S9 115.0(5) . . ?
C15 C15 S9 122.0(10) 2_666 . ?
C15 C15 S10 122.9(10) 2_666 . ?
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
Cu1 I1 2.5138(16) . y
Cu1 I2 2.5205(16) . y
Cu1 I3 2.5818(16) . y
Pb1 I1 3.3452(9) 2_575 y
Pb1 I2 3.2429(9) . y
Pb1 I4 3.0294(10) . y
Pb1 I5 3.0482(10) . y
S1 C1 1.713(12) . ?
S1 C3 1.727(10) . ?
S2 C2 1.718(13) . ?
S2 C3 1.717(10) . ?
S3 C4 1.733(10) . ?
S3 C5 1.734(11) . ?
S4 C4 1.710(10) . ?
S4 C6 1.734(12) . ?
S5 C7 1.723(12) . ?
S5 C9 1.719(10) . ?
S6 C8 1.738(11) . ?
S6 C9 1.738(10) . ?
S7 C10 1.720(11) . ?
S7 C11 1.720(11) . ?
S8 C10 1.721(10) . ?
S8 C12 1.732(12) . ?
S9 C13 1.680(16) . ?
S9 C15 1.758(9) . ?
S10 C14 1.720(11) . ?
S10 C15 1.748(10) . ?
C1 C2 1.352(17) . ?
C3 C4 1.402(14) . ?
C5 C6 1.343(16) . ?
C7 C8 1.329(16) . ?
C9 C10 1.390(13) . ?
C11 C12 1.334(16) . ?
C13 C14 1.299(19) . ?
C15 C15 1.367(18) 2_666 ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S2 -0.9(15) . . . . ?
S1 C3 C4 S3 0.9(13) . . . . ?
S1 C3 C4 S4 178.3(6) . . . . ?
S2 C3 C4 S3 -179.2(6) . . . . ?
S2 C3 C4 S4 -1.7(13) . . . . ?
S3 C5 C6 S4 -0.4(13) . . . . ?
S5 C7 C8 S6 0.2(14) . . . . ?
S5 C9 C10 S7 2.0(13) . . . . ?
S5 C9 C10 S8 178.3(6) . . . . ?
S6 C9 C10 S7 179.0(6) . . . . ?
S6 C9 C10 S8 -4.6(13) . . . . ?
S7 C11 C12 S8 -0.5(14) . . . . ?
S9 C13 C14 S10 0.2(14) . . . . ?
C1 S1 C3 S2 1.4(7) . . . . ?
C1 S1 C3 C4 -178.7(9) . . . . ?
C2 S2 C3 S1 -1.8(7) . . . . ?
C2 S2 C3 C4 178.3(9) . . . . ?
C3 S1 C1 C2 -0.3(11) . . . . ?
C3 S2 C2 C1 1.6(11) . . . . ?
C4 S3 C5 C6 0.5(10) . . . . ?
C4 S4 C6 C5 0.0(10) . . . . ?
C5 S3 C4 S4 -0.5(7) . . . . ?
C5 S3 C4 C3 177.1(9) . . . . ?
C6 S4 C4 S3 0.4(7) . . . . ?
C6 S4 C4 C3 -177.3(9) . . . . ?
C7 S5 C9 S6 -0.7(7) . . . . ?
C7 S5 C9 C10 176.5(9) . . . . ?
C8 S6 C9 S5 0.7(7) . . . . ?
C8 S6 C9 C10 -176.5(9) . . . . ?
C9 S5 C7 C8 0.3(11) . . . . ?
C9 S6 C8 C7 -0.6(11) . . . . ?
C10 S7 C11 C12 -0.8(11) . . . . ?
C10 S8 C12 C11 1.5(10) . . . . ?
C11 S7 C10 S8 1.8(7) . . . . ?
C11 S7 C10 C9 178.4(9) . . . . ?
C12 S8 C10 S7 -2.0(7) . . . . ?
C12 S8 C10 C9 -178.6(9) . . . . ?
C13 S9 C15 S10 -1.3(6) . . . . ?
C13 S9 C15 C15 179.8(11) . . . 2_666 ?
C14 S10 C15 S9 1.4(6) . . . . ?
C14 S10 C15 C15 -179.7(11) . . . 2_666 ?
C15 S9 C13 C14 0.7(10) . . . . ?
C15 S10 C14 C13 -1.0(10) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.855(3)
2 0.145(3)
