#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:51:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180359 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/28/7202875.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_7202875
loop_
_publ_author_name
'Alberola, Antonio'
'Llusar, Rosa'
'Triguero, Sonia'
'Vicent, Cristian'
'Sokolov, Maxim N.'
'Gómez-García, Carlos'
_publ_section_title
;
 Structural diversity in charge transfer salts based on Mo3S7 and
 Mo3S4Se3 clusters complexes and bis(ethylenedithio)tetrathiafulvalene
 (ET)
;
_journal_issue                   32
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              3440
_journal_paper_doi               10.1039/b703551a
_journal_volume                  17
_journal_year                    2007
_chemical_formula_sum            'C12 H11 Cl6 Mo3 N S15'
_chemical_formula_weight         1150.64
_chemical_name_systematic
;
?
;
_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                105.133(2)
_cell_angle_beta                 92.035(2)
_cell_angle_gamma                99.297(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0467(10)
_cell_length_b                   11.3217(12)
_cell_length_c                   14.8607(15)
_cell_measurement_reflns_used    13381
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.89
_cell_volume                     1604.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.1283
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9263
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    2.643
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0325P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                3432
_reflns_number_total             5652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b703551a.txt
_cod_data_source_block           (ET)2[Mo3S7Cl6]2CH3CN
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7202875
#BEGIN Tags that were not found in dictionaries:
_ratio_of_minimum_to_maximum_apparent_transmision 0.906055
#END Tags that were not found in dictionaries
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
Mo1 Mo -0.13239(8) 0.67136(8) 0.26857(5) 0.0193(2) Uani 1 1 d . . .
Mo2 Mo 0.10308(8) 0.58703(8) 0.29791(6) 0.0234(2) Uani 1 1 d . . .
Mo3 Mo 0.07999(8) 0.70830(8) 0.16005(6) 0.0206(2) Uani 1 1 d . . .
S1 S 0.0805(2) 0.7964(2) 0.32203(17) 0.0260(6) Uani 1 1 d . . .
S2 S -0.1163(2) 0.4588(2) 0.25748(18) 0.0276(6) Uani 1 1 d . . .
S3 S -0.0955(3) 0.5629(3) 0.39165(18) 0.0314(6) Uani 1 1 d . . .
S4 S -0.1459(2) 0.6036(2) 0.10095(16) 0.0257(6) Uani 1 1 d . . .
S5 S -0.1335(2) 0.7905(3) 0.15046(17) 0.0281(6) Uani 1 1 d . . .
S6 S 0.1331(2) 0.5042(2) 0.13553(17) 0.0265(6) Uani 1 1 d . . .
S7 S 0.2902(2) 0.6366(3) 0.20224(19) 0.0320(7) Uani 1 1 d . . .
Cl1 Cl -0.2040(2) 0.8405(2) 0.38468(17) 0.0336(6) Uani 1 1 d . . .
Cl2 Cl -0.3820(2) 0.6008(3) 0.24472(17) 0.0340(6) Uani 1 1 d . . .
Cl3 Cl 0.2498(3) 0.6811(3) 0.44193(19) 0.0510(8) Uani 1 1 d . . .
Cl4 Cl 0.1791(3) 0.3959(3) 0.3166(2) 0.0481(8) Uani 1 1 d . . .
Cl5 Cl 0.2115(3) 0.9103(3) 0.16459(18) 0.0378(7) Uani 1 1 d . . .
Cl6 Cl 0.1190(2) 0.6772(3) -0.01333(17) 0.0329(6) Uani 1 1 d . . .
S10 S 0.4360(3) 0.6114(3) 0.62604(18) 0.0345(7) Uani 1 1 d . . .
S11 S 0.5907(3) 0.6787(2) 0.48393(18) 0.0316(6) Uani 1 1 d . . .
S12 S 0.4449(4) 0.8675(3) 0.7410(2) 0.0602(10) Uani 1 1 d . . .
S13 S 0.6292(3) 0.9503(3) 0.5706(2) 0.0427(8) Uani 1 1 d . . .
C10 C 0.5063(8) 0.5635(8) 0.5248(7) 0.023(2) Uani 1 1 d . . .
C11 C 0.4893(10) 0.7674(9) 0.6428(7) 0.031(3) Uani 1 1 d . . .
C12 C 0.5624(9) 0.8001(9) 0.5754(7) 0.026(2) Uani 1 1 d . . .
C13 C 0.4117(12) 0.9841(11) 0.6852(8) 0.050(3) Uani 1 1 d . . .
H13A H 0.3480 0.9459 0.6309 0.060 Uiso 1 1 calc R . .
H13B H 0.3710 1.0459 0.7282 0.060 Uiso 1 1 calc R . .
C14 C 0.5393(11) 1.0462(10) 0.6558(7) 0.042(3) Uani 1 1 d . . .
H14A H 0.6006 1.0848 0.7114 0.050 Uiso 1 1 calc R . .
H14B H 0.5175 1.1123 0.6307 0.050 Uiso 1 1 calc R . .
S20 S 0.8055(3) 1.0221(2) 1.05345(18) 0.0314(6) Uani 1 1 d . . .
S21 S 0.8834(2) 0.8302(2) 0.90893(18) 0.0284(6) Uani 1 1 d . . .
S22 S 0.5242(3) 0.8947(3) 1.0499(2) 0.0473(8) Uani 1 1 d . . .
S23 S 0.6113(2) 0.6744(3) 0.86422(18) 0.0316(6) Uani 1 1 d . . .
C20 C 0.9314(8) 0.9650(9) 0.9901(6) 0.025(2) Uani 1 1 d . . .
C21 C 0.7157(8) 0.8080(9) 0.9315(6) 0.019(2) Uani 1 1 d . . .
C22 C 0.6804(9) 0.9005(9) 1.0022(7) 0.027(2) Uani 1 1 d . . .
C23 C 0.4661(11) 0.6655(13) 0.9311(8) 0.066(4) Uani 1 1 d . . .
H23A H 0.3954 0.6943 0.9009 0.079 Uiso 1 1 calc R . .
H23B H 0.4340 0.5784 0.9266 0.079 Uiso 1 1 calc R . .
C24 C 0.4800(12) 0.7323(12) 1.0289(8) 0.056(4) Uani 1 1 d . . .
H24A H 0.5487 0.7031 1.0607 0.067 Uiso 1 1 calc R . .
H24B H 0.3952 0.7134 1.0557 0.067 Uiso 1 1 calc R . .
C100 C 1.0118(15) 0.1545(14) 0.4168(9) 0.078(5) Uani 1 1 d . . .
C101 C 0.9612(14) 0.1151(13) 0.3230(10) 0.064(4) Uani 1 1 d . . .
N1 N 0.9183(16) 0.0786(16) 0.2447(9) 0.126(6) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'
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
S1 Mo1 S4 108.47(9) . . ?
S1 Mo1 S2 108.91(9) . . ?
S4 Mo1 S2 83.85(9) . . ?
S1 Mo1 Cl1 81.00(9) . . ?
S4 Mo1 Cl1 135.49(9) . . ?
S2 Mo1 Cl1 135.53(9) . . ?
S1 Mo1 S5 84.79(9) . . ?
S4 Mo1 S5 49.21(9) . . ?
S2 Mo1 S5 132.68(9) . . ?
Cl1 Mo1 S5 90.48(9) . . ?
S1 Mo1 Cl2 161.06(9) . . ?
S4 Mo1 Cl2 83.33(8) . . ?
S2 Mo1 Cl2 86.61(9) . . ?
Cl1 Mo1 Cl2 80.27(9) . . ?
S5 Mo1 Cl2 92.60(9) . . ?
S1 Mo1 S3 87.30(9) . . ?
S4 Mo1 S3 132.24(10) . . ?
S2 Mo1 S3 48.55(9) . . ?
Cl1 Mo1 S3 90.54(9) . . ?
S5 Mo1 S3 171.76(9) . . ?
Cl2 Mo1 S3 95.63(9) . . ?
S1 Mo1 Mo2 54.22(7) . . ?
S4 Mo1 Mo2 96.30(6) . . ?
S2 Mo1 Mo2 54.93(6) . . ?
Cl1 Mo1 Mo2 121.80(7) . . ?
S5 Mo1 Mo2 116.49(7) . . ?
Cl2 Mo1 Mo2 141.15(8) . . ?
S3 Mo1 Mo2 56.41(6) . . ?
S1 Mo1 Mo3 54.04(6) . . ?
S4 Mo1 Mo3 54.92(6) . . ?
S2 Mo1 Mo3 94.76(6) . . ?
Cl1 Mo1 Mo3 123.05(7) . . ?
S5 Mo1 Mo3 56.32(6) . . ?
Cl2 Mo1 Mo3 137.65(7) . . ?
S3 Mo1 Mo3 116.70(7) . . ?
Mo2 Mo1 Mo3 60.30(3) . . ?
S1 Mo2 S2 109.00(9) . . ?
S1 Mo2 S6 108.03(9) . . ?
S2 Mo2 S6 83.61(9) . . ?
S1 Mo2 Cl3 79.90(10) . . ?
S2 Mo2 Cl3 135.56(10) . . ?
S6 Mo2 Cl3 136.49(10) . . ?
S1 Mo2 S7 85.20(9) . . ?
S2 Mo2 S7 132.17(10) . . ?
S6 Mo2 S7 48.85(9) . . ?
Cl3 Mo2 S7 91.11(10) . . ?
S1 Mo2 Cl4 161.72(10) . . ?
S2 Mo2 Cl4 85.15(10) . . ?
S6 Mo2 Cl4 84.46(9) . . ?
Cl3 Mo2 Cl4 81.87(11) . . ?
S7 Mo2 Cl4 93.81(9) . . ?
S1 Mo2 S3 87.48(9) . . ?
S2 Mo2 S3 48.70(9) . . ?
S6 Mo2 S3 132.14(9) . . ?
Cl3 Mo2 S3 89.98(10) . . ?
S7 Mo2 S3 172.29(10) . . ?
Cl4 Mo2 S3 93.89(9) . . ?
S1 Mo2 Mo1 54.15(6) . . ?
S2 Mo2 Mo1 55.08(6) . . ?
S6 Mo2 Mo1 95.77(6) . . ?
Cl3 Mo2 Mo1 120.71(8) . . ?
S7 Mo2 Mo1 116.48(7) . . ?
Cl4 Mo2 Mo1 139.75(8) . . ?
S3 Mo2 Mo1 56.74(6) . . ?
S1 Mo2 Mo3 53.92(6) . . ?
S2 Mo2 Mo3 94.69(7) . . ?
S6 Mo2 Mo3 54.59(6) . . ?
Cl3 Mo2 Mo3 122.37(9) . . ?
S7 Mo2 Mo3 56.51(6) . . ?
Cl4 Mo2 Mo3 138.64(8) . . ?
S3 Mo2 Mo3 116.80(7) . . ?
Mo1 Mo2 Mo3 60.06(3) . . ?
S1 Mo3 S6 108.23(9) . . ?
S1 Mo3 S4 108.29(9) . . ?
S6 Mo3 S4 85.53(9) . . ?
S1 Mo3 Cl5 83.30(9) . . ?
S6 Mo3 Cl5 133.86(9) . . ?
S4 Mo3 Cl5 134.34(9) . . ?
S1 Mo3 S5 84.57(8) . . ?
S6 Mo3 S5 134.17(9) . . ?
S4 Mo3 S5 49.08(9) . . ?
Cl5 Mo3 S5 90.39(9) . . ?
S1 Mo3 S7 84.75(9) . . ?
S6 Mo3 S7 48.67(9) . . ?
S4 Mo3 S7 133.77(10) . . ?
Cl5 Mo3 S7 90.23(9) . . ?
S5 Mo3 S7 169.15(9) . . ?
S1 Mo3 Cl6 162.82(10) . . ?
S6 Mo3 Cl6 84.33(9) . . ?
S4 Mo3 Cl6 83.81(8) . . ?
Cl5 Mo3 Cl6 79.52(9) . . ?
S5 Mo3 Cl6 95.09(8) . . ?
S7 Mo3 Cl6 95.67(8) . . ?
S1 Mo3 Mo1 53.98(6) . . ?
S6 Mo3 Mo1 95.60(7) . . ?
S4 Mo3 Mo1 54.81(6) . . ?
Cl5 Mo3 Mo1 124.58(7) . . ?
S5 Mo3 Mo1 56.03(6) . . ?
S7 Mo3 Mo1 115.37(7) . . ?
Cl6 Mo3 Mo1 138.37(7) . . ?
S1 Mo3 Mo2 53.93(7) . . ?
S6 Mo3 Mo2 54.78(6) . . ?
S4 Mo3 Mo2 95.74(7) . . ?
Cl5 Mo3 Mo2 124.16(7) . . ?
S5 Mo3 Mo2 115.54(7) . . ?
S7 Mo3 Mo2 55.82(6) . . ?
Cl6 Mo3 Mo2 138.89(7) . . ?
Mo1 Mo3 Mo2 59.64(3) . . ?
Mo1 S1 Mo3 71.98(8) . . ?
Mo1 S1 Mo2 71.63(8) . . ?
Mo3 S1 Mo2 72.15(8) . . ?
S3 S2 Mo2 68.14(11) . . ?
S3 S2 Mo1 68.35(11) . . ?
Mo2 S2 Mo1 69.99(8) . . ?
S2 S3 Mo2 63.16(10) . . ?
S2 S3 Mo1 63.10(10) . . ?
Mo2 S3 Mo1 66.85(7) . . ?
S5 S4 Mo1 67.41(10) . . ?
S5 S4 Mo3 67.61(10) . . ?
Mo1 S4 Mo3 70.27(7) . . ?
S4 S5 Mo1 63.37(10) . . ?
S4 S5 Mo3 63.31(9) . . ?
Mo1 S5 Mo3 67.65(7) . . ?
S7 S6 Mo3 68.37(11) . . ?
S7 S6 Mo2 67.61(11) . . ?
Mo3 S6 Mo2 70.63(7) . . ?
S6 S7 Mo2 63.54(10) . . ?
S6 S7 Mo3 62.96(9) . . ?
Mo2 S7 Mo3 67.67(6) . . ?
C10 S10 C11 97.1(5) . . ?
C10 S11 C12 96.0(5) . . ?
C11 S12 C13 96.3(5) . . ?
C12 S13 C14 102.9(5) . . ?
C10 C10 S10 122.9(10) 2_666 . ?
C10 C10 S11 121.9(10) 2_666 . ?
S10 C10 S11 115.3(5) . . ?
C12 C11 S10 115.8(7) . . ?
C12 C11 S12 126.2(8) . . ?
S10 C11 S12 118.1(6) . . ?
C11 C12 S11 115.9(8) . . ?
C11 C12 S13 127.2(8) . . ?
S11 C12 S13 116.9(5) . . ?
C14 C13 S12 110.9(8) . . ?
C13 C14 S13 117.5(8) . . ?
C22 S20 C20 96.1(5) . . ?
C20 S21 C21 96.9(4) . . ?
C22 S22 C24 98.5(5) . . ?
C21 S23 C23 102.4(5) . . ?
C20 C20 S21 125.3(9) 2_777 . ?
C20 C20 S20 119.2(10) 2_777 . ?
S21 C20 S20 115.6(5) . . ?
C22 C21 S21 115.0(7) . . ?
C22 C21 S23 127.5(7) . . ?
S21 C21 S23 117.5(5) . . ?
C21 C22 S20 116.3(7) . . ?
C21 C22 S22 125.3(8) . . ?
S20 C22 S22 118.1(6) . . ?
C24 C23 S23 118.9(8) . . ?
C23 C24 S22 113.8(10) . . ?
N1 C101 C100 178.0(17) . . ?
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
Mo1 S1 2.350(3) . ?
Mo1 S4 2.399(2) . ?
Mo1 S2 2.401(3) . ?
Mo1 Cl1 2.444(3) . ?
Mo1 S5 2.478(3) . ?
Mo1 Cl2 2.489(2) . ?
Mo1 S3 2.502(3) . ?
Mo1 Mo2 2.7517(11) . ?
Mo1 Mo3 2.7634(11) . ?
Mo2 S1 2.352(3) . ?
Mo2 S2 2.397(3) . ?
Mo2 S6 2.399(3) . ?
Mo2 Cl3 2.443(3) . ?
Mo2 S7 2.478(3) . ?
Mo2 Cl4 2.485(3) . ?
Mo2 S3 2.493(3) . ?
Mo2 Mo3 2.7702(12) . ?
Mo3 S1 2.352(3) . ?
Mo3 S6 2.393(3) . ?
Mo3 S4 2.403(3) . ?
Mo3 Cl5 2.433(3) . ?
Mo3 S5 2.486(2) . ?
Mo3 S7 2.498(3) . ?
Mo3 Cl6 2.561(3) . ?
S2 S3 2.018(4) . ?
S4 S5 2.032(4) . ?
S6 S7 2.018(4) . ?
S10 C10 1.682(9) . ?
S10 C11 1.710(11) . ?
S11 C10 1.697(10) . ?
S11 C12 1.731(10) . ?
S12 C11 1.720(10) . ?
S12 C13 1.799(11) . ?
S13 C12 1.745(10) . ?
S13 C14 1.810(10) . ?
C10 C10 1.417(18) 2_666 ?
C11 C12 1.355(13) . ?
C13 C14 1.496(15) . ?
S20 C22 1.698(10) . ?
S20 C20 1.713(9) . ?
S21 C20 1.666(10) . ?
S21 C21 1.720(8) . ?
S22 C22 1.743(9) . ?
S22 C24 1.761(13) . ?
S23 C21 1.735(9) . ?
S23 C23 1.799(10) . ?
C20 C20 1.452(17) 2_777 ?
C21 C22 1.378(12) . ?
C23 C24 1.443(15) . ?
C100 C101 1.398(17) . ?
C101 N1 1.168(16) . ?
