# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Narcis Avarvari' _publ_contact_author_address ; Laboratoire Chimie, Ingenierie Moleculaire et Materiaux UMR - 6200 CNRS Universite d'Angers UFR Sciences ANGERS 49045 FRANCE ; _publ_contact_author_email NARCIS.AVARVARI@UNIV-ANGERS.FR _publ_section_title ; O***S versus N***S Intramolecular Nonbonded Interactions in Neutral and Radical Cation Salts of TTF-Oxazoline Derivatives: Synthesis, Theoretical Investigations, Crystalline Structures, and Physical Properties ; loop_ _publ_author_name 'Narcis Avarvari' 'Manuel Almeida' 'Enric Canadell' 'Rodolphe Clerac' 'Marc Fourmigue' ; E.B.Lopes ; 'Augustin Madalan' 'Celine Rethore' data_[1a]2Mo6Cl14 _database_code_depnum_ccdc_archive 'CCDC 632613' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((R/S)-EDT-TTF(SMe)-oxazoline)2(Mo6Cl14) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 Cl14 Mo6 N2 O2 S14' _chemical_formula_weight 1919.27 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.563 _cell_length_b 12.095 _cell_length_c 13.129 _cell_angle_alpha 73.31 _cell_angle_beta 69.31 _cell_angle_gamma 88.65 _cell_volume 1355.6 _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 84 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 926 _exptl_absorpt_coefficient_mu 2.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.707320 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area_detector _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14042 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.1478 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6449 _reflns_number_gt 3167 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.4436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6449 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1620 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 C1 C 0.0250(9) 0.3156(6) 0.3526(7) 0.038(2) Uani 1 1 d . . . C2 C 0.0679(8) 0.4204(6) 0.2686(6) 0.034(2) Uani 1 1 d . . . C3 C 0.1433(9) 0.4389(6) 0.4343(6) 0.036(2) Uani 1 1 d . . . C4 C 0.2082(9) 0.4734(6) 0.5015(7) 0.038(2) Uani 1 1 d . . . C5 C 0.3004(9) 0.4760(6) 0.6597(6) 0.038(2) Uani 1 1 d . . . C6 C 0.3505(8) 0.5812(6) 0.5801(6) 0.0320(19) Uani 1 1 d . . . C7 C 0.4168(14) 0.5395(9) 0.7975(8) 0.088(4) Uani 1 1 d . . . H7A H 0.3804 0.5353 0.8776 0.106 Uiso 1 1 calc R . . H7B H 0.5222 0.5260 0.7767 0.106 Uiso 1 1 calc R . . C8 C 0.4110(16) 0.6514(8) 0.7391(9) 0.111(5) Uani 1 1 d . . . H8A H 0.4788 0.6989 0.7528 0.133 Uiso 1 1 calc R . . H8B H 0.3106 0.6724 0.7739 0.133 Uiso 1 1 calc R . . C9 C -0.0512(10) 0.2112(6) 0.3541(7) 0.045(2) Uani 1 1 d . . . C10 C -0.1547(13) 0.0962(7) 0.2927(8) 0.080(4) Uani 1 1 d . . . H10A H -0.1048 0.0571 0.2362 0.096 Uiso 1 1 calc R . . H10B H -0.2587 0.1012 0.2989 0.096 Uiso 1 1 calc R . . C11 C -0.1445(16) 0.0311(9) 0.4079(10) 0.105(5) Uani 1 1 d . . . H11 H -0.0647 -0.0206 0.3910 0.126 Uiso 1 1 calc R . . C12 C -0.2627(15) -0.0372(10) 0.4907(9) 0.114(5) Uani 1 1 d . . . H12A H -0.2369 -0.0723 0.5564 0.170 Uiso 1 1 calc R . . H12B H -0.2900 -0.0965 0.4641 0.170 Uiso 1 1 calc R . . H12C H -0.3459 0.0085 0.5108 0.170 Uiso 1 1 calc R . . C13 C 0.1373(11) 0.5956(8) 0.0695(7) 0.077(4) Uani 1 1 d . . . H13A H 0.1304 0.6237 -0.0046 0.115 Uiso 1 1 calc R . . H13B H 0.2409 0.5935 0.0617 0.115 Uiso 1 1 calc R . . H13C H 0.0905 0.6463 0.1138 0.115 Uiso 1 1 calc R . . N1 N -0.0807(11) 0.1221(7) 0.4375(7) 0.099(4) Uani 1 1 d . . . O1 O -0.0798(7) 0.2116(4) 0.2610(5) 0.0589(18) Uani 1 1 d . . . S1 S 0.0537(3) 0.30159(16) 0.47808(19) 0.0473(6) Uani 1 1 d . . . S2 S 0.1556(2) 0.52374(17) 0.30061(17) 0.0404(6) Uani 1 1 d . . . S3 S 0.1979(3) 0.38286(16) 0.63057(17) 0.0426(6) Uani 1 1 d . . . S4 S 0.3040(2) 0.60675(16) 0.45914(16) 0.0365(5) Uani 1 1 d . . . S5 S 0.3267(3) 0.42132(19) 0.7884(2) 0.0573(7) Uani 1 1 d . . . S6 S 0.4536(3) 0.69428(19) 0.58724(18) 0.0510(7) Uani 1 1 d . . . S7 S 0.0461(3) 0.45579(19) 0.13839(19) 0.0505(7) Uani 1 1 d . . . Mo1 Mo 0.30168(8) 0.94196(5) 0.07532(5) 0.0296(2) Uani 1 1 d . . . Mo2 Mo 0.53652(8) 0.93878(5) 0.13281(5) 0.0300(2) Uani 1 1 d . . . Mo3 Mo 0.45280(8) 1.13554(5) 0.03680(5) 0.0305(2) Uani 1 1 d . . . Cl1 Cl 0.3010(2) 1.01565(17) 0.23209(16) 0.0432(6) Uani 1 1 d . . . Cl2 Cl 0.3919(2) 0.75907(15) 0.16246(16) 0.0405(6) Uani 1 1 d . . . Cl3 Cl 0.3217(2) 0.87447(15) -0.08971(15) 0.0381(5) Uani 1 1 d . . . Cl4 Cl 0.2321(2) 1.13077(15) -0.01879(17) 0.0386(5) Uani 1 1 d . . . Cl5 Cl 0.3978(3) 1.31844(17) 0.0806(2) 0.0525(6) Uani 1 1 d . . . Cl6 Cl 0.0419(2) 0.86175(17) 0.17568(19) 0.0502(6) Uani 1 1 d . . . Cl7 Cl 0.5805(3) 0.85385(18) 0.30863(17) 0.0511(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(6) 0.040(5) 0.047(5) -0.019(4) -0.016(5) 0.008(4) C2 0.022(5) 0.046(5) 0.038(5) -0.021(4) -0.011(4) 0.001(4) C3 0.033(6) 0.029(4) 0.042(5) -0.005(4) -0.014(4) -0.001(4) C4 0.037(6) 0.035(4) 0.042(5) -0.009(4) -0.018(4) 0.003(4) C5 0.026(5) 0.048(5) 0.029(5) -0.004(4) -0.004(4) 0.008(4) C6 0.026(5) 0.049(5) 0.030(5) -0.022(4) -0.011(4) 0.009(4) C7 0.133(12) 0.088(8) 0.053(7) -0.014(6) -0.048(8) -0.025(8) C8 0.245(17) 0.052(7) 0.093(9) -0.028(6) -0.125(11) 0.022(8) C9 0.067(7) 0.026(4) 0.054(6) -0.012(4) -0.034(5) -0.003(4) C10 0.136(11) 0.034(5) 0.088(8) -0.021(5) -0.059(8) -0.010(6) C11 0.180(15) 0.061(7) 0.095(9) 0.000(7) -0.090(10) -0.041(8) C12 0.143(13) 0.111(10) 0.085(9) -0.021(8) -0.040(9) -0.065(9) C13 0.091(9) 0.080(7) 0.041(6) 0.000(5) -0.013(6) -0.027(6) N1 0.181(11) 0.050(5) 0.107(7) -0.005(5) -0.111(8) -0.032(6) O1 0.090(6) 0.037(3) 0.067(4) -0.013(3) -0.050(4) 0.002(3) S1 0.0659(19) 0.0276(11) 0.0576(15) -0.0096(10) -0.0353(14) -0.0008(11) S2 0.0428(16) 0.0397(11) 0.0379(13) -0.0092(10) -0.0147(12) -0.0079(10) S3 0.0539(17) 0.0291(11) 0.0446(13) -0.0032(10) -0.0233(12) -0.0008(10) S4 0.0422(15) 0.0353(11) 0.0308(11) -0.0059(9) -0.0142(11) -0.0072(10) S5 0.081(2) 0.0495(13) 0.0478(15) -0.0052(11) -0.0388(15) 0.0134(13) S6 0.0585(18) 0.0543(14) 0.0431(13) -0.0135(11) -0.0215(13) -0.0150(12) S7 0.0543(18) 0.0575(14) 0.0472(14) -0.0182(11) -0.0249(13) -0.0023(12) Mo1 0.0289(5) 0.0306(4) 0.0256(4) -0.0017(3) -0.0104(4) -0.0058(3) Mo2 0.0343(5) 0.0317(4) 0.0229(4) -0.0013(3) -0.0141(4) -0.0046(3) Mo3 0.0348(5) 0.0290(4) 0.0291(4) -0.0063(3) -0.0149(4) -0.0018(3) Cl1 0.0401(15) 0.0579(13) 0.0281(11) -0.0139(10) -0.0069(10) -0.0009(11) Cl2 0.0461(15) 0.0318(10) 0.0360(12) 0.0061(9) -0.0178(11) -0.0115(10) Cl3 0.0464(15) 0.0362(10) 0.0377(12) -0.0075(9) -0.0242(11) -0.0073(10) Cl4 0.0367(14) 0.0355(10) 0.0453(12) -0.0063(9) -0.0213(11) 0.0024(9) Cl5 0.0587(17) 0.0453(12) 0.0738(16) -0.0348(12) -0.0350(14) 0.0161(11) Cl6 0.0274(14) 0.0519(12) 0.0571(14) -0.0101(11) -0.0029(12) -0.0108(10) Cl7 0.0660(18) 0.0567(13) 0.0322(12) 0.0026(10) -0.0315(12) -0.0039(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 C2 1.375(10) . ? C1 C9 1.465(9) . ? C1 S1 1.725(8) . ? C2 S7 1.724(7) . ? C2 S2 1.745(7) . ? C3 C4 1.396(10) . ? C3 S2 1.724(7) . ? C3 S1 1.731(6) . ? C4 S3 1.703(8) . ? C4 S4 1.716(7) . ? C5 C6 1.361(9) . ? C5 S3 1.715(7) . ? C5 S5 1.734(8) . ? C6 S4 1.739(7) . ? C6 S6 1.748(7) . ? C7 C8 1.361(13) . ? C7 S5 1.740(9) . ? C8 S6 1.804(10) . ? C9 N1 1.248(10) . ? C9 O1 1.342(9) . ? C10 O1 1.462(9) . ? C10 C11 1.527(13) . ? C11 C12 1.343(13) . ? C11 N1 1.477(10) . ? C13 S7 1.753(8) . ? Mo1 Cl6 2.432(2) . ? Mo1 Cl4 2.465(2) . ? Mo1 Cl1 2.4648(19) . ? Mo1 Cl2 2.470(2) . ? Mo1 Cl3 2.4726(19) . ? Mo1 Mo3 2.6055(8) . ? Mo1 Mo2 2.6060(9) . ? Mo1 Mo2 2.6067(9) 2_675 ? Mo1 Mo3 2.6086(10) 2_675 ? Mo2 Cl7 2.4216(19) . ? Mo2 Cl2 2.4624(17) . ? Mo2 Cl3 2.4758(17) 2_675 ? Mo2 Cl4 2.478(2) 2_675 ? Mo2 Cl1 2.481(2) . ? Mo2 Mo3 2.6003(8) 2_675 ? Mo2 Mo3 2.6064(9) . ? Mo2 Mo1 2.6067(9) 2_675 ? Mo3 Cl5 2.442(2) . ? Mo3 Cl2 2.470(2) 2_675 ? Mo3 Cl4 2.472(2) . ? Mo3 Cl1 2.473(2) . ? Mo3 Cl3 2.479(2) 2_675 ? Mo3 Mo2 2.6003(8) 2_675 ? Mo3 Mo1 2.6086(10) 2_675 ? Cl2 Mo3 2.470(2) 2_675 ? Cl3 Mo2 2.4758(17) 2_675 ? Cl3 Mo3 2.479(2) 2_675 ? Cl4 Mo2 2.478(2) 2_675 ? 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 C2 C1 C9 128.7(7) . . ? C2 C1 S1 118.4(5) . . ? C9 C1 S1 112.8(6) . . ? C1 C2 S7 126.7(5) . . ? C1 C2 S2 114.4(6) . . ? S7 C2 S2 118.9(4) . . ? C4 C3 S2 123.6(5) . . ? C4 C3 S1 121.0(6) . . ? S2 C3 S1 115.3(4) . . ? C3 C4 S3 121.1(5) . . ? C3 C4 S4 122.5(6) . . ? S3 C4 S4 116.4(4) . . ? C6 C5 S3 116.8(6) . . ? C6 C5 S5 128.8(6) . . ? S3 C5 S5 114.5(4) . . ? C5 C6 S4 116.4(5) . . ? C5 C6 S6 127.1(6) . . ? S4 C6 S6 116.5(4) . . ? C8 C7 S5 123.8(8) . . ? C7 C8 S6 120.8(8) . . ? N1 C9 O1 121.1(7) . . ? N1 C9 C1 120.5(7) . . ? O1 C9 C1 118.3(7) . . ? O1 C10 C11 105.5(7) . . ? C12 C11 N1 116.6(10) . . ? C12 C11 C10 120.2(11) . . ? N1 C11 C10 102.9(7) . . ? C9 N1 C11 106.7(7) . . ? C9 O1 C10 103.2(6) . . ? C1 S1 C3 95.2(4) . . ? C3 S2 C2 96.6(3) . . ? C4 S3 C5 95.7(3) . . ? C4 S4 C6 94.7(4) . . ? C5 S5 C7 102.7(4) . . ? C6 S6 C8 99.2(4) . . ? C2 S7 C13 103.1(4) . . ? Cl6 Mo1 Cl4 93.11(8) . . ? Cl6 Mo1 Cl1 92.25(7) . . ? Cl4 Mo1 Cl1 89.68(7) . . ? Cl6 Mo1 Cl2 91.32(7) . . ? Cl4 Mo1 Cl2 175.56(7) . . ? Cl1 Mo1 Cl2 89.94(7) . . ? Cl6 Mo1 Cl3 91.99(7) . . ? Cl4 Mo1 Cl3 89.96(7) . . ? Cl1 Mo1 Cl3 175.76(7) . . ? Cl2 Mo1 Cl3 90.09(7) . . ? Cl6 Mo1 Mo3 135.95(6) . . ? Cl4 Mo1 Mo3 58.28(5) . . ? Cl1 Mo1 Mo3 58.31(5) . . ? Cl2 Mo1 Mo3 117.97(5) . . ? Cl3 Mo1 Mo3 118.11(5) . . ? Cl6 Mo1 Mo2 134.45(6) . . ? Cl4 Mo1 Mo2 118.28(5) . . ? Cl1 Mo1 Mo2 58.52(6) . . ? Cl2 Mo1 Mo2 57.97(5) . . ? Cl3 Mo1 Mo2 118.15(6) . . ? Mo3 Mo1 Mo2 60.02(2) . . ? Cl6 Mo1 Mo2 135.70(6) . 2_675 ? Cl4 Mo1 Mo2 58.42(5) . 2_675 ? Cl1 Mo1 Mo2 118.15(5) . 2_675 ? Cl2 Mo1 Mo2 118.08(6) . 2_675 ? Cl3 Mo1 Mo2 58.27(4) . 2_675 ? Mo3 Mo1 Mo2 59.85(2) . 2_675 ? Mo2 Mo1 Mo2 89.84(3) . 2_675 ? Cl6 Mo1 Mo3 134.18(6) . 2_675 ? Cl4 Mo1 Mo3 118.37(6) . 2_675 ? Cl1 Mo1 Mo3 118.32(6) . 2_675 ? Cl2 Mo1 Mo3 58.14(5) . 2_675 ? Cl3 Mo1 Mo3 58.34(5) . 2_675 ? Mo3 Mo1 Mo3 89.87(3) . 2_675 ? Mo2 Mo1 Mo3 59.82(3) . 2_675 ? Mo2 Mo1 Mo3 59.97(3) 2_675 2_675 ? Cl7 Mo2 Cl2 90.62(7) . . ? Cl7 Mo2 Cl3 93.63(6) . 2_675 ? Cl2 Mo2 Cl3 175.75(7) . 2_675 ? Cl7 Mo2 Cl4 92.45(8) . 2_675 ? Cl2 Mo2 Cl4 90.23(7) . 2_675 ? Cl3 Mo2 Cl4 89.58(7) 2_675 2_675 ? Cl7 Mo2 Cl1 92.29(8) . . ? Cl2 Mo2 Cl1 89.73(7) . . ? Cl3 Mo2 Cl1 90.12(7) 2_675 . ? Cl4 Mo2 Cl1 175.26(7) 2_675 . ? Cl7 Mo2 Mo3 133.97(6) . 2_675 ? Cl2 Mo2 Mo3 58.34(5) . 2_675 ? Cl3 Mo2 Mo3 118.19(5) 2_675 2_675 ? Cl4 Mo2 Mo3 58.19(5) 2_675 2_675 ? Cl1 Mo2 Mo3 118.02(5) . 2_675 ? Cl7 Mo2 Mo1 133.79(6) . . ? Cl2 Mo2 Mo1 58.25(5) . . ? Cl3 Mo2 Mo1 118.30(5) 2_675 . ? Cl4 Mo2 Mo1 118.31(5) 2_675 . ? Cl1 Mo2 Mo1 57.90(5) . . ? Mo3 Mo2 Mo1 60.14(3) 2_675 . ? Cl7 Mo2 Mo3 135.98(6) . . ? Cl2 Mo2 Mo3 118.21(6) . . ? Cl3 Mo2 Mo3 58.33(5) 2_675 . ? Cl4 Mo2 Mo3 117.95(5) 2_675 . ? Cl1 Mo2 Mo3 58.11(5) . . ? Mo3 Mo2 Mo3 90.03(3) 2_675 . ? Mo1 Mo2 Mo3 59.98(2) . . ? Cl7 Mo2 Mo1 136.03(6) . 2_675 ? Cl2 Mo2 Mo1 118.37(5) . 2_675 ? Cl3 Mo2 Mo1 58.15(5) 2_675 2_675 ? Cl4 Mo2 Mo1 57.92(5) 2_675 2_675 ? Cl1 Mo2 Mo1 118.14(5) . 2_675 ? Mo3 Mo2 Mo1 60.05(2) 2_675 2_675 ? Mo1 Mo2 Mo1 90.16(3) . 2_675 ? Mo3 Mo2 Mo1 60.05(3) . 2_675 ? Cl5 Mo3 Cl2 90.64(8) . 2_675 ? Cl5 Mo3 Cl4 92.97(7) . . ? Cl2 Mo3 Cl4 90.19(7) 2_675 . ? Cl5 Mo3 Cl1 93.89(8) . . ? Cl2 Mo3 Cl1 175.46(7) 2_675 . ? Cl4 Mo3 Cl1 89.32(7) . . ? Cl5 Mo3 Cl3 91.50(7) . 2_675 ? Cl2 Mo3 Cl3 89.92(7) 2_675 2_675 ? Cl4 Mo3 Cl3 175.53(7) . 2_675 ? Cl1 Mo3 Cl3 90.22(7) . 2_675 ? Cl5 Mo3 Mo2 134.30(6) . 2_675 ? Cl2 Mo3 Mo2 58.04(4) 2_675 2_675 ? Cl4 Mo3 Mo2 58.42(5) . 2_675 ? Cl1 Mo3 Mo2 118.08(5) . 2_675 ? Cl3 Mo3 Mo2 118.11(6) 2_675 2_675 ? Cl5 Mo3 Mo1 136.66(7) . . ? Cl2 Mo3 Mo1 118.12(5) 2_675 . ? Cl4 Mo3 Mo1 58.01(5) . . ? Cl1 Mo3 Mo1 58.00(5) . . ? Cl3 Mo3 Mo1 118.18(5) 2_675 . ? Mo2 Mo3 Mo1 60.10(2) 2_675 . ? Cl5 Mo3 Mo2 135.68(6) . . ? Cl2 Mo3 Mo2 118.08(6) 2_675 . ? Cl4 Mo3 Mo2 117.99(5) . . ? Cl1 Mo3 Mo2 58.41(6) . . ? Cl3 Mo3 Mo2 58.20(4) 2_675 . ? Mo2 Mo3 Mo2 89.97(3) 2_675 . ? Mo1 Mo3 Mo2 60.00(2) . . ? Cl5 Mo3 Mo1 133.20(6) . 2_675 ? Cl2 Mo3 Mo1 58.12(6) 2_675 2_675 ? Cl4 Mo3 Mo1 118.44(6) . 2_675 ? Cl1 Mo3 Mo1 118.38(6) . 2_675 ? Cl3 Mo3 Mo1 58.09(5) 2_675 2_675 ? Mo2 Mo3 Mo1 60.04(3) 2_675 2_675 ? Mo1 Mo3 Mo1 90.13(3) . 2_675 ? Mo2 Mo3 Mo1 59.98(3) . 2_675 ? Mo1 Cl1 Mo3 63.69(5) . . ? Mo1 Cl1 Mo2 63.59(5) . . ? Mo3 Cl1 Mo2 63.48(5) . . ? Mo2 Cl2 Mo1 63.79(5) . . ? Mo2 Cl2 Mo3 63.63(5) . 2_675 ? Mo1 Cl2 Mo3 63.74(5) . 2_675 ? Mo1 Cl3 Mo2 63.58(4) . 2_675 ? Mo1 Cl3 Mo3 63.58(5) . 2_675 ? Mo2 Cl3 Mo3 63.47(5) 2_675 2_675 ? Mo1 Cl4 Mo3 63.72(5) . . ? Mo1 Cl4 Mo2 63.66(6) . 2_675 ? Mo3 Cl4 Mo2 63.38(5) . 2_675 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.826 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.171 # Attachment '1a_4Mo6Cl14.cif' data_[1a]4Mo6Cl14 _database_code_depnum_ccdc_archive 'CCDC 632614' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((R/S)-EDT-TTF(SMe)-oxazoline)4(Mo6Cl14) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H52 Cl14 Mo6 N4 O4 S28' _chemical_formula_weight 2766.60 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' 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.392 _cell_length_b 13.868 _cell_length_c 18.026 _cell_angle_alpha 91.19 _cell_angle_beta 102.84 _cell_angle_gamma 107.28 _cell_volume 2408.1 _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 122 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1362 _exptl_absorpt_coefficient_mu 1.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.684934 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area_detector _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46952 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11018 _reflns_number_gt 5548 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+1.8955P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11018 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1425 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1354 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.56599(5) 0.01169(4) 0.10498(3) 0.04166(16) Uani 1 1 d . . . Mo2 Mo 0.32095(5) -0.04728(4) 0.01133(3) 0.04633(17) Uani 1 1 d . . . Mo3 Mo 0.50801(6) -0.13070(4) -0.00512(3) 0.04667(16) Uani 1 1 d . . . Cl1 Cl 0.3993(2) -0.15746(13) 0.10499(9) 0.0647(5) Uani 1 1 d . . . Cl2 Cl 0.74084(18) -0.06740(16) 0.08284(9) 0.0684(5) Uani 1 1 d . . . Cl3 Cl 0.38691(16) 0.09021(13) 0.11529(8) 0.0529(4) Uani 1 1 d . . . Cl4 Cl 0.72311(17) 0.17983(14) 0.09360(9) 0.0644(5) Uani 1 1 d . . . Cl5 Cl 0.65156(17) 0.02947(14) 0.24653(8) 0.0577(5) Uani 1 1 d . . . Cl6 Cl 0.5200(3) -0.30279(16) -0.01053(12) 0.0986(8) Uani 1 1 d . . . Cl7 Cl 0.08518(18) -0.1121(2) 0.02497(11) 0.1023(9) Uani 1 1 d . . . S1 S 1.02961(15) -0.21924(12) 0.46707(9) 0.0457(4) Uani 1 1 d . . . S2 S 0.78609(15) -0.17777(12) 0.37265(8) 0.0445(4) Uani 1 1 d . . . S3 S 1.00200(17) -0.09525(13) 0.61208(9) 0.0533(4) Uani 1 1 d . . . S4 S 0.76220(16) -0.05069(12) 0.51707(9) 0.0498(4) Uani 1 1 d . . . S5 S 0.9953(2) 0.00753(17) 0.75409(10) 0.0825(7) Uani 1 1 d . . . S6 S 0.7072(2) 0.06157(15) 0.63947(12) 0.0742(6) Uani 1 1 d . . . S7 S 0.79730(18) -0.28968(13) 0.23125(9) 0.0578(5) Uani 1 1 d . . . C1 C 0.9806(6) -0.2646(4) 0.3710(3) 0.0432(15) Uani 1 1 d . . . C2 C 0.8640(6) -0.2490(4) 0.3262(3) 0.0419(14) Uani 1 1 d . . . C3 C 0.9013(5) -0.1628(4) 0.4611(3) 0.0391(14) Uani 1 1 d . . . C4 C 0.8905(6) -0.1079(4) 0.5231(3) 0.0411(14) Uani 1 1 d . . . C5 C 0.9204(7) -0.0257(5) 0.6567(4) 0.0567(18) Uani 1 1 d . . . C6 C 0.8103(7) -0.0045(4) 0.6125(3) 0.0484(16) Uani 1 1 d . . . C7 C 0.8854(10) 0.0801(9) 0.7775(5) 0.125(4) Uani 1 1 d . . . H7A H 0.8912 0.0798 0.8319 0.150 Uiso 1 1 calc R . . H7B H 0.9253 0.1499 0.7678 0.150 Uiso 1 1 calc R . . C8 C 0.7441(11) 0.0488(7) 0.7394(5) 0.106(3) Uani 1 1 d . . . H8A H 0.6978 0.0876 0.7632 0.128 Uiso 1 1 calc R . . H8B H 0.7041 -0.0219 0.7470 0.128 Uiso 1 1 calc R . . C9 C 1.0652(6) -0.3199(5) 0.3433(4) 0.0455(15) Uani 1 1 d . . . C10 C 1.2548(8) -0.3649(6) 0.3585(5) 0.077(2) Uani 1 1 d . . . H10A H 1.2749 -0.4232 0.3813 0.092 Uiso 1 1 calc R . . H10B H 1.3416 -0.3136 0.3582 0.092 Uiso 1 1 calc R . . C11 C 1.1622(8) -0.3955(6) 0.2772(5) 0.080(2) Uani 1 1 d . . . H11 H 1.1226 -0.4696 0.2696 0.096 Uiso 1 1 calc R . . C12 C 1.2390(12) -0.3597(10) 0.2158(7) 0.156(5) Uani 1 1 d . . . H12A H 1.1760 -0.3806 0.1664 0.234 Uiso 1 1 calc R . . H12B H 1.3131 -0.3887 0.2198 0.234 Uiso 1 1 calc R . . H12C H 1.2765 -0.2871 0.2222 0.234 Uiso 1 1 calc R . . C13 C 0.6384(7) -0.2595(6) 0.2112(4) 0.076(2) Uani 1 1 d . . . H13A H 0.5914 -0.2801 0.1585 0.114 Uiso 1 1 calc R . . H13B H 0.6578 -0.1877 0.2210 0.114 Uiso 1 1 calc R . . H13C H 0.5807 -0.2945 0.2432 0.114 Uiso 1 1 calc R . . N1 N 1.0482(6) -0.3500(4) 0.2770(4) 0.0686(17) Uani 1 1 d . . . O1 O 1.1744(5) -0.3256(4) 0.3993(3) 0.0688(13) Uani 1 1 d . . . S8 S 1.20373(16) -0.63719(13) 0.38930(9) 0.0499(4) Uani 1 1 d . . . S9 S 1.44705(15) -0.68623(12) 0.47803(9) 0.0469(4) Uani 1 1 d . . . S10 S 1.18119(16) -0.51776(12) 0.53444(9) 0.0476(4) Uani 1 1 d . . . S11 S 1.42649(16) -0.55717(12) 0.62907(9) 0.0491(4) Uani 1 1 d . . . S12 S 1.13286(19) -0.39799(15) 0.65413(12) 0.0705(6) Uani 1 1 d . . . S13 S 1.42592(19) -0.44414(15) 0.76905(11) 0.0702(5) Uani 1 1 d . . . S14 S 1.48873(16) -0.79183(13) 0.34134(10) 0.0545(4) Uani 1 1 d . . . C14 C 1.2871(6) -0.7009(4) 0.3398(4) 0.0454(15) Uani 1 1 d . . . C15 C 1.3966(5) -0.7255(4) 0.3800(3) 0.0404(14) Uani 1 1 d . . . C16 C 1.3210(5) -0.6258(4) 0.4768(3) 0.0393(14) Uani 1 1 d . . . C17 C 1.3128(5) -0.5732(4) 0.5394(3) 0.0403(14) Uani 1 1 d . . . C18 C 1.2360(6) -0.4663(4) 0.6298(3) 0.0453(15) Uani 1 1 d . . . C19 C 1.3482(6) -0.4840(4) 0.6727(4) 0.0484(16) Uani 1 1 d . . . C20 C 1.2054(10) -0.3635(9) 0.7522(5) 0.111(3) Uani 1 1 d . . . H20A H 1.2669 -0.2944 0.7576 0.133 Uiso 1 1 calc R . . H20B H 1.1303 -0.3620 0.7755 0.133 Uiso 1 1 calc R . . C21 C 1.2768(13) -0.4181(10) 0.7947(6) 0.140(5) Uani 1 1 d . . . H21A H 1.2105 -0.4833 0.7974 0.168 Uiso 1 1 calc R . . H21B H 1.3097 -0.3844 0.8461 0.168 Uiso 1 1 calc R . . C22 C 1.2239(6) -0.7169(6) 0.2581(4) 0.0604(19) Uani 1 1 d . . . C24 C 1.0921(11) -0.7126(9) 0.1451(5) 0.117(4) Uani 1 1 d . . . H24 H 0.9969 -0.7587 0.1289 0.140 Uiso 1 1 calc R . . C23 C 1.1925(8) -0.7665(7) 0.1355(4) 0.093(3) Uani 1 1 d . . . H23A H 1.1444 -0.8340 0.1100 0.112 Uiso 1 1 calc R . . H23B H 1.2553 -0.7292 0.1060 0.112 Uiso 1 1 calc R . . C25 C 1.1092(18) -0.6235(10) 0.0993(7) 0.213(8) Uani 1 1 d . . . H25A H 1.0455 -0.5882 0.1065 0.320 Uiso 1 1 calc R . . H25B H 1.0906 -0.6461 0.0462 0.320 Uiso 1 1 calc R . . H25C H 1.2026 -0.5786 0.1158 0.320 Uiso 1 1 calc R . . C26 C 1.6091(7) -0.8107(6) 0.4240(4) 0.074(2) Uani 1 1 d . . . H26A H 1.6654 -0.8471 0.4082 0.111 Uiso 1 1 calc R . . H26B H 1.5587 -0.8490 0.4579 0.111 Uiso 1 1 calc R . . H26C H 1.6674 -0.7461 0.4498 0.111 Uiso 1 1 calc R . . N2 N 1.1265(7) -0.6811(6) 0.2284(4) 0.100(3) Uani 1 1 d . . . O2 O 1.2673(4) -0.7712(4) 0.2129(3) 0.0629(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0471(3) 0.0573(4) 0.0226(3) -0.0051(2) 0.0041(2) 0.0229(3) Mo2 0.0415(3) 0.0663(4) 0.0291(3) -0.0097(3) 0.0074(2) 0.0152(3) Mo3 0.0652(4) 0.0493(4) 0.0302(3) -0.0036(2) 0.0094(3) 0.0266(3) Cl1 0.0948(13) 0.0598(12) 0.0418(10) 0.0068(8) 0.0258(9) 0.0201(10) Cl2 0.0743(12) 0.1096(15) 0.0364(9) -0.0067(9) -0.0011(8) 0.0622(11) Cl3 0.0615(10) 0.0741(12) 0.0327(8) -0.0075(7) 0.0124(7) 0.0352(9) Cl4 0.0599(10) 0.0740(12) 0.0446(10) -0.0246(8) 0.0118(8) 0.0014(9) Cl5 0.0710(11) 0.0925(13) 0.0167(7) -0.0057(7) -0.0016(7) 0.0455(10) Cl6 0.178(2) 0.0633(14) 0.0705(14) 0.0013(11) 0.0264(14) 0.0641(15) Cl7 0.0479(11) 0.176(2) 0.0586(13) -0.0390(14) 0.0177(9) -0.0014(12) S1 0.0411(9) 0.0530(10) 0.0388(9) 0.0033(7) 0.0044(7) 0.0119(7) S2 0.0438(9) 0.0509(10) 0.0360(9) -0.0001(7) 0.0063(7) 0.0130(7) S3 0.0537(10) 0.0575(11) 0.0369(9) 0.0008(8) 0.0044(7) 0.0049(8) S4 0.0500(9) 0.0517(11) 0.0452(10) -0.0017(8) 0.0145(7) 0.0101(8) S5 0.1036(16) 0.0860(15) 0.0354(10) -0.0088(10) 0.0147(10) -0.0018(12) S6 0.0909(14) 0.0585(12) 0.0792(14) -0.0055(10) 0.0500(12) 0.0110(10) S7 0.0666(11) 0.0562(11) 0.0412(10) -0.0039(8) 0.0050(8) 0.0116(9) C1 0.044(4) 0.039(4) 0.041(4) 0.001(3) 0.010(3) 0.006(3) C2 0.041(3) 0.041(4) 0.039(3) 0.009(3) 0.013(3) 0.003(3) C3 0.035(3) 0.046(4) 0.031(3) 0.001(3) 0.007(2) 0.003(3) C4 0.045(3) 0.037(4) 0.032(3) 0.006(3) 0.005(3) 0.002(3) C5 0.073(5) 0.046(4) 0.038(4) -0.007(3) 0.025(4) -0.008(3) C6 0.062(4) 0.036(4) 0.040(4) 0.003(3) 0.021(3) -0.002(3) C7 0.113(8) 0.169(10) 0.062(6) -0.045(6) 0.046(6) -0.017(7) C8 0.150(10) 0.094(7) 0.081(7) 0.000(5) 0.065(7) 0.019(7) C9 0.041(4) 0.049(4) 0.046(4) 0.009(3) 0.012(3) 0.012(3) C10 0.065(5) 0.067(5) 0.101(7) 0.002(5) 0.023(5) 0.023(4) C11 0.084(6) 0.074(6) 0.095(7) -0.001(5) 0.040(5) 0.033(5) C12 0.149(10) 0.216(14) 0.138(10) 0.014(9) 0.098(9) 0.060(10) C13 0.084(5) 0.094(6) 0.043(4) -0.001(4) -0.005(4) 0.031(5) N1 0.067(4) 0.067(4) 0.080(5) -0.001(4) 0.024(3) 0.029(3) O1 0.064(3) 0.079(4) 0.068(3) -0.001(3) 0.014(3) 0.030(3) S8 0.0451(9) 0.0549(11) 0.0535(10) -0.0046(8) 0.0082(8) 0.0245(8) S9 0.0435(9) 0.0442(10) 0.0547(10) -0.0010(8) 0.0102(7) 0.0177(7) S10 0.0459(9) 0.0512(10) 0.0487(10) -0.0024(8) 0.0100(7) 0.0207(8) S11 0.0439(9) 0.0495(10) 0.0527(10) -0.0006(8) 0.0070(7) 0.0163(8) S12 0.0609(11) 0.0784(14) 0.0761(14) -0.0240(10) 0.0127(10) 0.0322(10) S13 0.0592(11) 0.0750(14) 0.0570(12) -0.0210(10) -0.0041(9) 0.0072(10) S14 0.0449(9) 0.0508(11) 0.0703(12) -0.0090(9) 0.0121(8) 0.0207(8) C14 0.036(3) 0.039(4) 0.058(4) -0.013(3) 0.012(3) 0.007(3) C15 0.031(3) 0.029(3) 0.057(4) -0.008(3) 0.010(3) 0.003(3) C16 0.038(3) 0.031(3) 0.049(4) 0.000(3) 0.011(3) 0.010(3) C17 0.033(3) 0.028(3) 0.056(4) 0.001(3) 0.011(3) 0.003(2) C18 0.032(3) 0.046(4) 0.051(4) -0.010(3) 0.005(3) 0.008(3) C19 0.039(4) 0.041(4) 0.056(4) -0.009(3) 0.010(3) 0.000(3) C20 0.101(7) 0.164(10) 0.080(7) -0.027(7) 0.013(5) 0.070(7) C21 0.203(12) 0.200(13) 0.069(7) -0.010(7) 0.039(8) 0.137(11) C22 0.040(4) 0.083(5) 0.058(5) -0.019(4) 0.004(3) 0.025(4) C24 0.121(8) 0.165(10) 0.077(7) -0.035(7) -0.020(6) 0.097(8) C23 0.082(6) 0.152(9) 0.050(5) -0.036(5) -0.010(4) 0.066(6) C25 0.44(3) 0.159(13) 0.099(10) 0.019(9) 0.073(13) 0.171(16) C26 0.063(5) 0.088(6) 0.079(5) -0.009(4) 0.007(4) 0.045(4) N2 0.093(5) 0.152(7) 0.065(4) -0.042(4) -0.027(4) 0.089(5) O2 0.048(3) 0.078(3) 0.060(3) -0.026(2) 0.002(2) 0.026(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cl3 2.4563(15) . ? Mo1 Cl4 2.4601(18) . ? Mo1 Cl1 2.4678(18) . ? Mo1 Cl2 2.4805(16) . ? Mo1 Cl5 2.4895(14) . ? Mo1 Mo2 2.6072(7) . ? Mo1 Mo3 2.6075(7) . ? Mo1 Mo2 2.6103(7) 2_655 ? Mo1 Mo3 2.6111(7) 2_655 ? Mo2 Cl7 2.4167(18) . ? Mo2 Cl2 2.4613(18) 2_655 ? Mo2 Cl1 2.4664(18) . ? Mo2 Cl3 2.4740(16) . ? Mo2 Cl4 2.4773(17) 2_655 ? Mo2 Mo3 2.5995(8) 2_655 ? Mo2 Mo3 2.6045(7) . ? Mo2 Mo1 2.6103(7) 2_655 ? Mo3 Cl6 2.428(2) . ? Mo3 Cl4 2.4610(18) 2_655 ? Mo3 Cl3 2.4694(15) 2_655 ? Mo3 Cl2 2.4726(18) . ? Mo3 Cl1 2.4764(16) . ? Mo3 Mo2 2.5995(8) 2_655 ? Mo3 Mo1 2.6111(7) 2_655 ? Cl2 Mo2 2.4613(18) 2_655 ? Cl3 Mo3 2.4694(15) 2_655 ? Cl4 Mo3 2.4610(17) 2_655 ? Cl4 Mo2 2.4773(17) 2_655 ? S1 C3 1.721(6) . ? S1 C1 1.739(6) . ? S2 C3 1.735(6) . ? S2 C2 1.754(6) . ? S3 C4 1.728(6) . ? S3 C5 1.747(7) . ? S4 C4 1.728(6) . ? S4 C6 1.732(6) . ? S5 C5 1.746(7) . ? S5 C7 1.837(11) . ? S6 C6 1.738(7) . ? S6 C8 1.781(9) . ? S7 C2 1.711(6) . ? S7 C13 1.784(7) . ? C1 C2 1.377(8) . ? C1 C9 1.480(8) . ? C3 C4 1.383(8) . ? C5 C6 1.355(9) . ? C7 C8 1.406(12) . ? C9 N1 1.215(8) . ? C9 O1 1.364(7) . ? C10 O1 1.438(8) . ? C10 C11 1.535(11) . ? C11 N1 1.498(9) . ? C11 C12 1.513(11) . ? S8 C16 1.737(6) . ? S8 C14 1.759(6) . ? S9 C16 1.748(6) . ? S9 C15 1.752(6) . ? S10 C17 1.745(6) . ? S10 C18 1.749(6) . ? S11 C17 1.744(6) . ? S11 C19 1.746(6) . ? S12 C18 1.743(6) . ? S12 C20 1.756(9) . ? S13 C19 1.745(6) . ? S13 C21 1.841(10) . ? S14 C15 1.744(6) . ? S14 C26 1.798(7) . ? C14 C15 1.346(8) . ? C14 C22 1.457(9) . ? C16 C17 1.363(8) . ? C18 C19 1.340(8) . ? C20 C21 1.347(12) . ? C22 N2 1.275(8) . ? C22 O2 1.331(7) . ? C24 N2 1.488(10) . ? C24 C23 1.489(11) . ? C24 C25 1.489(14) . ? C23 O2 1.451(8) . ? 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 Cl3 Mo1 Cl4 89.37(6) . . ? Cl3 Mo1 Cl1 89.87(6) . . ? Cl4 Mo1 Cl1 175.23(6) . . ? Cl3 Mo1 Cl2 175.22(5) . . ? Cl4 Mo1 Cl2 89.94(7) . . ? Cl1 Mo1 Cl2 90.44(7) . . ? Cl3 Mo1 Cl5 90.97(5) . . ? Cl4 Mo1 Cl5 92.25(6) . . ? Cl1 Mo1 Cl5 92.47(6) . . ? Cl2 Mo1 Cl5 93.79(5) . . ? Cl3 Mo1 Mo2 58.41(4) . . ? Cl4 Mo1 Mo2 117.72(5) . . ? Cl1 Mo1 Mo2 58.08(5) . . ? Cl2 Mo1 Mo2 117.98(5) . . ? Cl5 Mo1 Mo2 134.39(4) . . ? Cl3 Mo1 Mo3 118.32(4) . . ? Cl4 Mo1 Mo3 118.14(4) . . ? Cl1 Mo1 Mo3 58.33(4) . . ? Cl2 Mo1 Mo3 58.09(4) . . ? Cl5 Mo1 Mo3 136.03(5) . . ? Mo2 Mo1 Mo3 59.93(2) . . ? Cl3 Mo1 Mo2 118.06(4) . 2_655 ? Cl4 Mo1 Mo2 58.41(4) . 2_655 ? Cl1 Mo1 Mo2 118.07(4) . 2_655 ? Cl2 Mo1 Mo2 57.76(4) . 2_655 ? Cl5 Mo1 Mo2 135.91(5) . 2_655 ? Mo2 Mo1 Mo2 89.68(2) . 2_655 ? Mo3 Mo1 Mo2 59.76(2) . 2_655 ? Cl3 Mo1 Mo3 58.23(4) . 2_655 ? Cl4 Mo1 Mo3 57.97(5) . 2_655 ? Cl1 Mo1 Mo3 117.82(5) . 2_655 ? Cl2 Mo1 Mo3 117.59(5) . 2_655 ? Cl5 Mo1 Mo3 134.26(5) . 2_655 ? Mo2 Mo1 Mo3 59.76(2) . 2_655 ? Mo3 Mo1 Mo3 89.71(2) . 2_655 ? Mo2 Mo1 Mo3 59.843(19) 2_655 2_655 ? Cl7 Mo2 Cl2 92.08(8) . 2_655 ? Cl7 Mo2 Cl1 91.80(8) . . ? Cl2 Mo2 Cl1 176.12(6) 2_655 . ? Cl7 Mo2 Cl3 93.39(6) . . ? Cl2 Mo2 Cl3 90.16(6) 2_655 . ? Cl1 Mo2 Cl3 89.49(6) . . ? Cl7 Mo2 Cl4 91.75(7) . 2_655 ? Cl2 Mo2 Cl4 89.98(6) 2_655 2_655 ? Cl1 Mo2 Cl4 90.02(6) . 2_655 ? Cl3 Mo2 Cl4 174.86(6) . 2_655 ? Cl7 Mo2 Mo3 135.79(7) . 2_655 ? Cl2 Mo2 Mo3 58.42(5) 2_655 2_655 ? Cl1 Mo2 Mo3 118.31(5) . 2_655 ? Cl3 Mo2 Mo3 58.19(4) . 2_655 ? Cl4 Mo2 Mo3 117.80(5) 2_655 2_655 ? Cl7 Mo2 Mo3 134.18(7) . . ? Cl2 Mo2 Mo3 118.55(4) 2_655 . ? Cl1 Mo2 Mo3 58.39(4) . . ? Cl3 Mo2 Mo3 117.77(4) . . ? Cl4 Mo2 Mo3 57.86(4) 2_655 . ? Mo3 Mo2 Mo3 90.03(2) 2_655 . ? Cl7 Mo2 Mo1 135.28(5) . . ? Cl2 Mo2 Mo1 118.61(5) 2_655 . ? Cl1 Mo2 Mo1 58.13(5) . . ? Cl3 Mo2 Mo1 57.75(4) . . ? Cl4 Mo2 Mo1 117.89(5) 2_655 . ? Mo3 Mo2 Mo1 60.20(2) 2_655 . ? Mo3 Mo2 Mo1 60.043(19) . . ? Cl7 Mo2 Mo1 134.39(5) . 2_655 ? Cl2 Mo2 Mo1 58.47(4) 2_655 2_655 ? Cl1 Mo2 Mo1 118.47(5) . 2_655 ? Cl3 Mo2 Mo1 118.23(5) . 2_655 ? Cl4 Mo2 Mo1 57.76(4) 2_655 2_655 ? Mo3 Mo2 Mo1 60.07(2) 2_655 2_655 ? Mo3 Mo2 Mo1 60.095(19) . 2_655 ? Mo1 Mo2 Mo1 90.32(2) . 2_655 ? Cl6 Mo3 Cl4 92.73(8) . 2_655 ? Cl6 Mo3 Cl3 92.63(7) . 2_655 ? Cl4 Mo3 Cl3 89.04(6) 2_655 2_655 ? Cl6 Mo3 Cl2 91.68(8) . . ? Cl4 Mo3 Cl2 175.54(7) 2_655 . ? Cl3 Mo3 Cl2 90.01(6) 2_655 . ? Cl6 Mo3 Cl1 92.07(7) . . ? Cl4 Mo3 Cl1 90.17(6) 2_655 . ? Cl3 Mo3 Cl1 175.26(6) 2_655 . ? Cl2 Mo3 Cl1 90.42(6) . . ? Cl6 Mo3 Mo2 134.82(7) . 2_655 ? Cl4 Mo3 Mo2 117.97(5) 2_655 2_655 ? Cl3 Mo3 Mo2 58.36(4) 2_655 2_655 ? Cl2 Mo3 Mo2 58.00(5) . 2_655 ? Cl1 Mo3 Mo2 118.16(5) . 2_655 ? Cl6 Mo3 Mo2 135.20(7) . . ? Cl4 Mo3 Mo2 58.47(4) 2_655 . ? Cl3 Mo3 Mo2 117.79(4) 2_655 . ? Cl2 Mo3 Mo2 118.38(4) . . ? Cl1 Mo3 Mo2 58.02(5) . . ? Mo2 Mo3 Mo2 89.97(2) 2_655 . ? Cl6 Mo3 Mo1 134.24(6) . . ? Cl4 Mo3 Mo1 118.48(5) 2_655 . ? Cl3 Mo3 Mo1 118.51(5) 2_655 . ? Cl2 Mo3 Mo1 58.38(4) . . ? Cl1 Mo3 Mo1 58.01(4) . . ? Mo2 Mo3 Mo1 60.17(2) 2_655 . ? Mo2 Mo3 Mo1 60.029(19) . . ? Cl6 Mo3 Mo1 135.47(6) . 2_655 ? Cl4 Mo3 Mo1 57.94(5) 2_655 2_655 ? Cl3 Mo3 Mo1 57.74(4) 2_655 2_655 ? Cl2 Mo3 Mo1 118.03(5) . 2_655 ? Cl1 Mo3 Mo1 118.06(5) . 2_655 ? Mo2 Mo3 Mo1 60.05(2) 2_655 2_655 ? Mo2 Mo3 Mo1 60.062(19) . 2_655 ? Mo1 Mo3 Mo1 90.29(2) . 2_655 ? Mo2 Cl1 Mo1 63.79(4) . . ? Mo2 Cl1 Mo3 63.60(4) . . ? Mo1 Cl1 Mo3 63.66(4) . . ? Mo2 Cl2 Mo3 63.59(4) 2_655 . ? Mo2 Cl2 Mo1 63.77(4) 2_655 . ? Mo3 Cl2 Mo1 63.53(4) . . ? Mo1 Cl3 Mo3 64.02(4) . 2_655 ? Mo1 Cl3 Mo2 63.85(4) . . ? Mo3 Cl3 Mo2 63.45(4) 2_655 . ? Mo1 Cl4 Mo3 64.09(4) . 2_655 ? Mo1 Cl4 Mo2 63.83(4) . 2_655 ? Mo3 Cl4 Mo2 63.66(4) 2_655 2_655 ? C3 S1 C1 94.9(3) . . ? C3 S2 C2 95.6(3) . . ? C4 S3 C5 94.7(3) . . ? C4 S4 C6 95.5(3) . . ? C5 S5 C7 100.3(4) . . ? C6 S6 C8 99.3(4) . . ? C2 S7 C13 102.6(3) . . ? C2 C1 C9 124.2(6) . . ? C2 C1 S1 118.1(5) . . ? C9 C1 S1 117.7(5) . . ? C1 C2 S7 125.1(5) . . ? C1 C2 S2 114.9(4) . . ? S7 C2 S2 119.9(3) . . ? C4 C3 S1 122.1(4) . . ? C4 C3 S2 121.5(4) . . ? S1 C3 S2 116.4(3) . . ? C3 C4 S4 122.2(4) . . ? C3 C4 S3 121.9(5) . . ? S4 C4 S3 116.0(3) . . ? C6 C5 S5 128.9(5) . . ? C6 C5 S3 117.2(5) . . ? S5 C5 S3 114.0(5) . . ? C5 C6 S4 116.7(5) . . ? C5 C6 S6 128.3(5) . . ? S4 C6 S6 115.0(4) . . ? C8 C7 S5 118.3(7) . . ? C7 C8 S6 115.8(6) . . ? N1 C9 O1 122.5(6) . . ? N1 C9 C1 124.7(6) . . ? O1 C9 C1 112.6(6) . . ? O1 C10 C11 104.3(6) . . ? N1 C11 C12 112.8(7) . . ? N1 C11 C10 103.7(6) . . ? C12 C11 C10 113.2(8) . . ? C9 N1 C11 104.7(6) . . ? C9 O1 C10 103.5(5) . . ? C16 S8 C14 94.5(3) . . ? C16 S9 C15 95.6(3) . . ? C17 S10 C18 95.3(3) . . ? C17 S11 C19 95.3(3) . . ? C18 S12 C20 102.6(4) . . ? C19 S13 C21 97.5(4) . . ? C15 S14 C26 103.2(3) . . ? C15 C14 C22 130.0(5) . . ? C15 C14 S8 118.3(5) . . ? C22 C14 S8 111.7(4) . . ? C14 C15 S14 124.7(5) . . ? C14 C15 S9 116.0(4) . . ? S14 C15 S9 119.3(3) . . ? C17 C16 S8 121.2(4) . . ? C17 C16 S9 123.4(4) . . ? S8 C16 S9 115.5(3) . . ? C16 C17 S11 124.3(4) . . ? C16 C17 S10 120.8(4) . . ? S11 C17 S10 114.8(3) . . ? C19 C18 S12 129.7(5) . . ? C19 C18 S10 117.1(5) . . ? S12 C18 S10 113.2(3) . . ? C18 C19 S13 127.6(5) . . ? C18 C19 S11 117.4(5) . . ? S13 C19 S11 115.0(4) . . ? C21 C20 S12 120.9(8) . . ? C20 C21 S13 121.8(8) . . ? N2 C22 O2 118.8(6) . . ? N2 C22 C14 121.7(6) . . ? O2 C22 C14 119.5(6) . . ? N2 C24 C23 105.1(6) . . ? N2 C24 C25 111.6(9) . . ? C23 C24 C25 109.7(10) . . ? O2 C23 C24 104.4(6) . . ? C22 N2 C24 105.3(6) . . ? C22 O2 C23 106.0(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.856 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.113