#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011903.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_7011903
loop_
_publ_author_name
'Srinivasan S. Kuduva'
'Narcis Avarvari'
'Marc Fourmigué'
_publ_section_title
;
 SbS and SS interactions in the first neutral and oxidized
 diphenylstibino (Ph2Sb--) derivatives of the redox active
 tetrathiafulvalene (TTF) core
;
_journal_issue                   19
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3686
_journal_page_last               3690
_journal_paper_doi               10.1039/b205594p
_journal_year                    2002
_chemical_formula_sum            'C20 H17 S4 Sb'
_chemical_formula_weight         507.33
_chemical_name_common            o-Me2TTF-SbPh2
_chemical_name_systematic
; 
3-(diphenylstibino)3',4'-dimethyltetrathiafulvalene
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7888(16)
_cell_length_b                   38.875(8)
_cell_length_c                   6.8578(14)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.62
_cell_volume                     2073.9(7)
_computing_cell_refinement       'Select, 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      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, Phi incr. 0.6 deg.'
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18941
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  0.9672
_exptl_absorpt_correction_T_min  0.6578
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Faceit, STOE-IPDS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0339
_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)+(0.0451P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                2981
_reflns_number_total             4612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205594p.txt
_cod_data_source_block           ksv1
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7011903
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.78269(4) 0.130631(7) 0.81661(4) 0.05352(10) Uani 1 1 d . . .
S1 S 1.13394(14) 0.08634(3) 0.98126(15) 0.0528(3) Uani 1 1 d . . .
S3 S 1.50444(14) 0.04881(3) 1.09604(15) 0.0541(3) Uani 1 1 d . . .
S4 S 1.44465(15) 0.05975(3) 1.51234(15) 0.0594(3) Uani 1 1 d . . .
C1 C 0.9565(5) 0.11117(10) 1.0438(6) 0.0495(9) Uani 1 1 d . . .
C5 C 1.6628(5) 0.03375(10) 1.2677(6) 0.0508(10) Uani 1 1 d . . .
C3 C 1.2165(5) 0.07982(9) 1.2232(5) 0.0468(9) Uani 1 1 d . . .
C4 C 1.3677(5) 0.06484(10) 1.2692(6) 0.0470(9) Uani 1 1 d . . .
C6 C 1.6350(5) 0.03869(11) 1.4549(6) 0.0526(10) Uani 1 1 d . . .
C6B C 0.6909(6) 0.19869(11) 1.0297(7) 0.0584(11) Uani 1 1 d . . .
H6BA H 0.7779 0.2080 0.9579 0.070 Uiso 1 1 calc R . .
C1B C 0.6513(5) 0.16437(10) 1.0103(6) 0.0509(10) Uani 1 1 d . . .
C6A C 0.8947(6) 0.18996(13) 0.5610(7) 0.0643(12) Uani 1 1 d . . .
H6AA H 0.7901 0.1851 0.4954 0.077 Uiso 1 1 calc R . .
C1A C 0.9516(5) 0.16978(11) 0.7179(6) 0.0513(10) Uani 1 1 d . . .
C7 C 1.8143(6) 0.01610(13) 1.1852(7) 0.0658(12) Uani 1 1 d . . .
H7A H 1.8928 0.0090 1.2898 0.099 Uiso 1 1 calc R . .
H7B H 1.8714 0.0317 1.1014 0.099 Uiso 1 1 calc R . .
H7C H 1.7757 -0.0037 1.1115 0.099 Uiso 1 1 calc R . .
C5A C 0.9932(8) 0.21745(14) 0.5015(7) 0.0737(14) Uani 1 1 d . . .
H5AA H 0.9538 0.2309 0.3964 0.088 Uiso 1 1 calc R . .
C5B C 0.6040(7) 0.21957(13) 1.1535(7) 0.0678(13) Uani 1 1 d . . .
H5BA H 0.6326 0.2427 1.1644 0.081 Uiso 1 1 calc R . .
C2A C 1.1093(6) 0.17728(12) 0.8091(7) 0.0625(12) Uani 1 1 d . . .
H2AA H 1.1497 0.1639 0.9140 0.075 Uiso 1 1 calc R . .
C8 C 1.7495(6) 0.02763(13) 1.6252(7) 0.0648(12) Uani 1 1 d . . .
H8A H 1.8493 0.0164 1.5788 0.097 Uiso 1 1 calc R . .
H8B H 1.6883 0.0120 1.7049 0.097 Uiso 1 1 calc R . .
H8C H 1.7842 0.0474 1.7010 0.097 Uiso 1 1 calc R . .
C4B C 0.4769(8) 0.20650(16) 1.2597(9) 0.0814(16) Uani 1 1 d . . .
H4BA H 0.4186 0.2206 1.3435 0.098 Uiso 1 1 calc R . .
C3B C 0.4348(7) 0.17223(18) 1.2427(9) 0.0846(16) Uani 1 1 d . . .
H3BA H 0.3486 0.1631 1.3164 0.101 Uiso 1 1 calc R . .
C2B C 0.5195(6) 0.15144(14) 1.1176(9) 0.0730(14) Uani 1 1 d . . .
H2BA H 0.4883 0.1284 1.1046 0.088 Uiso 1 1 calc R . .
C3A C 1.2083(7) 0.20435(14) 0.7472(8) 0.0734(14) Uani 1 1 d . . .
H3AA H 1.3156 0.2087 0.8077 0.088 Uiso 1 1 calc R . .
C4A C 1.1464(8) 0.22486(14) 0.5950(8) 0.0741(14) Uani 1 1 d . . .
H4AA H 1.2097 0.2438 0.5566 0.089 Uiso 1 1 calc R . .
S2 S 1.08339(17) 0.09616(4) 1.40134(16) 0.0665(3) Uani 1 1 d . . .
C2 C 0.9358(6) 0.11493(12) 1.2336(6) 0.0596(11) Uani 1 1 d . . .
H2A H 0.8433 0.1275 1.2767 0.072 Uiso 1 1 calc R . .
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'
Sb Sb -0.5866 1.5461 '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
C1A Sb1 C1 96.01(16) . . ?
C1A Sb1 C1B 94.61(16) . . ?
C1 Sb1 C1B 93.95(15) . . ?
C1 S1 C3 95.93(19) . . ?
C4 S3 C5 95.42(19) . . ?
C4 S4 C6 95.2(2) . . ?
C2 C1 S1 115.8(3) . . ?
C2 C1 Sb1 124.6(3) . . ?
S1 C1 Sb1 119.4(2) . . ?
C6 C5 C7 126.9(4) . . ?
C6 C5 S3 117.1(3) . . ?
C7 C5 S3 115.9(3) . . ?
C4 C3 S2 122.4(3) . . ?
C4 C3 S1 124.0(3) . . ?
S2 C3 S1 113.6(2) . . ?
C3 C4 S3 123.6(3) . . ?
C3 C4 S4 121.9(3) . . ?
S3 C4 S4 114.5(2) . . ?
C5 C6 C8 126.5(4) . . ?
C5 C6 S4 117.7(3) . . ?
C8 C6 S4 115.8(3) . . ?
C1B C6B C5B 121.1(5) . . ?
C6B C1B C2B 118.0(4) . . ?
C6B C1B Sb1 122.5(3) . . ?
C2B C1B Sb1 119.5(3) . . ?
C1A C6A C5A 120.2(5) . . ?
C2A C1A C6A 118.3(5) . . ?
C2A C1A Sb1 123.6(3) . . ?
C6A C1A Sb1 118.0(3) . . ?
C4A C5A C6A 120.7(5) . . ?
C4B C5B C6B 120.3(5) . . ?
C1A C2A C3A 121.2(4) . . ?
C5B C4B C3B 119.6(5) . . ?
C2B C3B C4B 120.2(6) . . ?
C3B C2B C1B 120.7(5) . . ?
C4A C3A C2A 119.5(5) . . ?
C5A C4A C3A 120.0(5) . . ?
C2 S2 C3 94.9(2) . . ?
C1 C2 S2 119.5(3) . . ?
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
Sb1 C1A 2.143(5) . ?
Sb1 C1 2.150(4) . ?
Sb1 C1B 2.161(4) . ?
S1 C1 1.756(4) . ?
S1 C3 1.767(4) . ?
S3 C4 1.749(4) . ?
S3 C5 1.762(4) . ?
S4 C4 1.754(4) . ?
S4 C6 1.756(5) . ?
C1 C2 1.327(6) . ?
C5 C6 1.326(6) . ?
C5 C7 1.501(6) . ?
C3 C4 1.337(5) . ?
C3 S2 1.760(4) . ?
C6 C8 1.496(5) . ?
C6B C1B 1.375(6) . ?
C6B C5B 1.376(7) . ?
C1B C2B 1.387(7) . ?
C6A C1A 1.386(6) . ?
C6A C5A 1.389(8) . ?
C1A C2A 1.382(6) . ?
C5A C4A 1.357(8) . ?
C5B C4B 1.357(8) . ?
C2A C3A 1.384(7) . ?
C4B C3B 1.376(9) . ?
C3B C2B 1.372(8) . ?
C3A C4A 1.381(7) . ?
S2 C2 1.745(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652741
