# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2007 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Rosa Llusar' _publ_contact_author_address ; Departament de Quimica Fisica i Analitica Universitat Jaume I Campus de Riu Sec Castellon 12071 SPAIN ; _publ_contact_author_email LLUSAR@QFA.UJI.ES _publ_section_title ; Structural Diversity in Charge Transfer Salts Based on Mo3S7 and Mo3S4Se3 Clusters Complexes and Bis(ethylendithio)tetrathiafulvalene (ET) ; loop_ _publ_author_name 'Rosa Llusar' 'Antonio Alberola Catalan' 'Carlos Gomez-Garcia' 'Maxim Sokolov' 'Sonia Triguero' ; C.Vicent ; data_(n-Bu4N)2[Mo3S7(tdas)3]0.5H2O _database_code_depnum_ccdc_archive 'CCDC 639723' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H73 Mo3 N8 O0.50 S16' _chemical_formula_weight 1450.82 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' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.817(5) _cell_length_b 14.767(2) _cell_length_c 29.597(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.763(4) _cell_angle_gamma 90.00 _cell_volume 12233(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5944 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _Ratio_of_minimum_to_maximum_apparent_transmission 0.945544 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48900 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17706 _reflns_number_gt 9408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0608P)^2^+27.9675P] 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 17706 _refine_ls_number_parameters 591 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1309 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.033 _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 Mo1 Mo 0.340217(17) 0.55695(3) 0.100136(15) 0.04282(12) Uani 1 1 d . . . Mo2 Mo 0.300419(18) 0.68200(3) 0.148518(15) 0.04447(12) Uani 1 1 d . . . Mo3 Mo 0.245684(16) 0.60554(3) 0.068195(15) 0.04230(12) Uani 1 1 d . . . S1 S 0.27823(5) 0.52794(8) 0.13827(4) 0.0454(3) Uani 1 1 d . . . S2 S 0.36867(6) 0.70942(10) 0.11642(5) 0.0571(4) Uani 1 1 d . . . S3 S 0.38522(6) 0.62962(10) 0.17369(5) 0.0595(4) Uani 1 1 d . . . S6 S 0.25658(5) 0.76654(9) 0.08229(5) 0.0523(3) Uani 1 1 d . . . S7 S 0.21310(6) 0.71071(9) 0.11951(5) 0.0557(4) Uani 1 1 d . . . S4 S 0.30604(5) 0.61932(9) 0.02457(4) 0.0494(3) Uani 1 1 d . . . S5 S 0.28572(5) 0.48885(9) 0.02927(5) 0.0520(3) Uani 1 1 d . . . S9 S 0.41457(6) 0.53566(11) 0.07003(6) 0.0640(4) Uani 1 1 d . . . S8 S 0.36063(6) 0.40700(10) 0.13501(5) 0.0601(4) Uani 1 1 d . . . S12 S 0.32075(8) 0.83426(10) 0.18542(6) 0.0729(5) Uani 1 1 d . . . S11 S 0.28801(6) 0.63951(9) 0.22524(5) 0.0555(4) Uani 1 1 d . . . S15 S 0.18864(6) 0.65636(11) -0.00609(5) 0.0643(4) Uani 1 1 d . . . S14 S 0.18318(6) 0.49293(10) 0.06964(5) 0.0598(4) Uani 1 1 d . . . S10 S 0.47948(10) 0.2921(2) 0.10718(11) 0.1406(12) Uani 1 1 d . . . S13 S 0.31783(9) 0.84012(13) 0.32261(6) 0.0937(7) Uani 1 1 d . . . S16 S 0.08579(8) 0.46706(15) -0.05461(8) 0.1065(8) Uani 1 1 d . . . N1 N 0.4322(3) 0.2957(4) 0.1302(2) 0.107(2) Uani 1 1 d . . . N2 N 0.4736(2) 0.3938(5) 0.0817(2) 0.100(2) Uani 1 1 d . . . N4 N 0.3269(2) 0.8826(3) 0.27410(19) 0.0857(18) Uani 1 1 d . . . N3 N 0.3025(2) 0.7365(3) 0.30399(16) 0.0706(15) Uani 1 1 d . . . N5 N 0.1108(2) 0.4387(4) -0.0004(2) 0.0873(18) Uani 1 1 d . . . N6 N 0.1185(2) 0.5565(4) -0.05926(19) 0.0819(17) Uani 1 1 d . . . C1 C 0.4117(2) 0.3744(4) 0.1184(2) 0.0662(16) Uani 1 1 d . . . C2 C 0.4353(2) 0.4303(5) 0.0906(2) 0.0683(17) Uani 1 1 d . . . C4 C 0.3175(2) 0.8185(4) 0.2425(2) 0.0602(15) Uani 1 1 d . . . C3 C 0.3035(2) 0.7339(4) 0.25950(18) 0.0531(13) Uani 1 1 d . . . C5 C 0.1451(2) 0.4985(4) 0.0140(2) 0.0614(15) Uani 1 1 d . . . C6 C 0.1490(2) 0.5666(4) -0.0191(2) 0.0606(15) Uani 1 1 d . . . N10 N 0.36193(17) 0.1515(3) 0.23438(15) 0.0563(12) Uani 1 1 d . . . C100 C 0.3639(2) 0.1034(4) 0.2801(2) 0.0645(16) Uani 1 1 d . . . H10A H 0.3359 0.1204 0.2909 0.077 Uiso 1 1 calc R . . H10B H 0.3622 0.0387 0.2744 0.077 Uiso 1 1 calc R . . C101 C 0.4072(3) 0.1223(6) 0.3183(2) 0.093(2) Uani 1 1 d . . . H10C H 0.4084 0.1858 0.3269 0.111 Uiso 1 1 calc R . . H10D H 0.4360 0.1075 0.3083 0.111 Uiso 1 1 calc R . . C102 C 0.4035(4) 0.0640(8) 0.3592(3) 0.137(4) Uani 1 1 d D . . H10E H 0.3795 0.0909 0.3732 0.165 Uiso 1 1 calc R . . H10F H 0.3913 0.0054 0.3471 0.165 Uiso 1 1 calc R . . C103 C 0.4457(4) 0.0484(12) 0.3961(4) 0.239(9) Uani 1 1 d D . . H10G H 0.4378 0.0099 0.4193 0.358 Uiso 1 1 calc R . . H10H H 0.4575 0.1052 0.4099 0.358 Uiso 1 1 calc R . . H10I H 0.4698 0.0199 0.3835 0.358 Uiso 1 1 calc R . . C104 C 0.4040(2) 0.1269(4) 0.2146(2) 0.0672(17) Uani 1 1 d . . . H10J H 0.4328 0.1486 0.2359 0.081 Uiso 1 1 calc R . . H10K H 0.4009 0.1592 0.1856 0.081 Uiso 1 1 calc R . . C105 C 0.4105(3) 0.0274(5) 0.2057(3) 0.084(2) Uani 1 1 d . . . H10L H 0.4136 -0.0062 0.2344 0.101 Uiso 1 1 calc R . . H10M H 0.3825 0.0050 0.1835 0.101 Uiso 1 1 calc R . . C106 C 0.4537(3) 0.0115(6) 0.1872(3) 0.097(2) Uani 1 1 d . . . H10N H 0.4816 0.0333 0.2098 0.117 Uiso 1 1 calc R . . H10O H 0.4508 0.0465 0.1589 0.117 Uiso 1 1 calc R . . C107 C 0.4612(4) -0.0873(7) 0.1768(3) 0.131(4) Uani 1 1 d . . . H10P H 0.4893 -0.0931 0.1648 0.197 Uiso 1 1 calc R . . H10Q H 0.4339 -0.1092 0.1541 0.197 Uiso 1 1 calc R . . H10R H 0.4652 -0.1222 0.2048 0.197 Uiso 1 1 calc R . . C108 C 0.3154(2) 0.1206(4) 0.20178(19) 0.0627(15) Uani 1 1 d . . . H10S H 0.3168 0.0555 0.1980 0.075 Uiso 1 1 calc R . . H10T H 0.2894 0.1332 0.2165 0.075 Uiso 1 1 calc R . . C109 C 0.3038(3) 0.1641(5) 0.1537(2) 0.081(2) Uani 1 1 d . . . H10U H 0.2969 0.2279 0.1564 0.098 Uiso 1 1 calc R . . H10V H 0.3311 0.1592 0.1401 0.098 Uiso 1 1 calc R . . C110 C 0.2613(3) 0.1182(6) 0.1225(2) 0.090(2) Uani 1 1 d . . . H11A H 0.2368 0.1108 0.1397 0.107 Uiso 1 1 calc R . . H11B H 0.2484 0.1580 0.0964 0.107 Uiso 1 1 calc R . . C111 C 0.2708(3) 0.0283(6) 0.1039(3) 0.104(3) Uani 1 1 d . . . H11C H 0.2414 0.0029 0.0862 0.156 Uiso 1 1 calc R . . H11D H 0.2846 -0.0114 0.1292 0.156 Uiso 1 1 calc R . . H11E H 0.2926 0.0354 0.0841 0.156 Uiso 1 1 calc R . . C112 C 0.3639(2) 0.2528(4) 0.2408(2) 0.0629(16) Uani 1 1 d . . . H11F H 0.3945 0.2682 0.2611 0.076 Uiso 1 1 calc R . . H11G H 0.3626 0.2806 0.2108 0.076 Uiso 1 1 calc R . . C113 C 0.3252(3) 0.2943(4) 0.2605(3) 0.081(2) Uani 1 1 d . . . H11H H 0.3242 0.2637 0.2893 0.097 Uiso 1 1 calc R . . H11I H 0.2946 0.2858 0.2387 0.097 Uiso 1 1 calc R . . C114 C 0.3338(3) 0.3945(5) 0.2699(3) 0.095(2) Uani 1 1 d . . . H11J H 0.3660 0.4030 0.2888 0.114 Uiso 1 1 calc R . . H11K H 0.3316 0.4255 0.2406 0.114 Uiso 1 1 calc R . . C115 C 0.2997(4) 0.4365(5) 0.2939(3) 0.111(3) Uani 1 1 d . . . H11L H 0.3079 0.4990 0.3002 0.166 Uiso 1 1 calc R . . H11M H 0.3011 0.4053 0.3227 0.166 Uiso 1 1 calc R . . H11N H 0.2679 0.4324 0.2745 0.166 Uiso 1 1 calc R . . N20 N 0.58320(19) 0.6452(4) 0.07222(17) 0.0680(14) Uani 1 1 d . . . C200 C 0.5885(3) 0.6519(6) 0.1242(2) 0.095(2) Uani 1 1 d . . . H20A H 0.5884 0.7154 0.1325 0.114 Uiso 1 1 calc R . . H20B H 0.6195 0.6274 0.1396 0.114 Uiso 1 1 calc R . . C201 C 0.5500(4) 0.6031(8) 0.1433(3) 0.139(4) Uani 1 1 d . . . H20C H 0.5516 0.5384 0.1382 0.167 Uiso 1 1 calc R . . H20D H 0.5186 0.6243 0.1273 0.167 Uiso 1 1 calc R . . C202 C 0.5587(5) 0.6227(10) 0.1963(4) 0.167(5) Uani 1 1 d . . . H20E H 0.5404 0.5799 0.2099 0.201 Uiso 1 1 calc R . . H20F H 0.5922 0.6130 0.2108 0.201 Uiso 1 1 calc R . . C203 C 0.5462(7) 0.7107(13) 0.2065(5) 0.275(12) Uani 1 1 d . . . H20G H 0.5599 0.7237 0.2387 0.413 Uiso 1 1 calc R . . H20H H 0.5120 0.7155 0.2004 0.413 Uiso 1 1 calc R . . H20I H 0.5581 0.7531 0.1874 0.413 Uiso 1 1 calc R . . C204 C 0.6254(2) 0.6957(4) 0.0623(2) 0.0719(18) Uani 1 1 d . . . H20J H 0.6247 0.7569 0.0740 0.086 Uiso 1 1 calc R . . H20K H 0.6543 0.6673 0.0802 0.086 Uiso 1 1 calc R . . C205 C 0.6292(2) 0.7017(4) 0.0128(2) 0.0699(17) Uani 1 1 d . . . H20L H 0.6032 0.7377 -0.0052 0.084 Uiso 1 1 calc R . . H20M H 0.6273 0.6416 -0.0008 0.084 Uiso 1 1 calc R . . C206 C 0.6768(3) 0.7451(5) 0.0115(2) 0.084(2) Uani 1 1 d . . . H20N H 0.6804 0.8006 0.0296 0.101 Uiso 1 1 calc R . . H20O H 0.7024 0.7046 0.0262 0.101 Uiso 1 1 calc R . . C207 C 0.6818(3) 0.7665(6) -0.0360(3) 0.103(3) Uani 1 1 d . . . H20P H 0.7118 0.7964 -0.0341 0.154 Uiso 1 1 calc R . . H20Q H 0.6562 0.8055 -0.0512 0.154 Uiso 1 1 calc R . . H20R H 0.6808 0.7114 -0.0534 0.154 Uiso 1 1 calc R . . C208 C 0.5371(3) 0.6858(5) 0.0453(3) 0.083(2) Uani 1 1 d . . . H20S H 0.5109 0.6515 0.0521 0.100 Uiso 1 1 calc R . . H20T H 0.5355 0.6786 0.0124 0.100 Uiso 1 1 calc R . . C209 C 0.5294(4) 0.7870(6) 0.0548(4) 0.142(4) Uani 1 1 d D . . H20U H 0.5590 0.8197 0.0565 0.171 Uiso 1 1 calc R . . H20V H 0.5212 0.7929 0.0846 0.171 Uiso 1 1 calc R . . C210 C 0.4876(5) 0.8312(9) 0.0147(5) 0.186(6) Uani 1 1 d D . . H21A H 0.4859 0.8965 0.0175 0.223 Uiso 1 1 calc R . . H21B H 0.4900 0.8148 -0.0164 0.223 Uiso 1 1 calc R . . C211 C 0.4477(6) 0.7836(10) 0.0292(8) 0.301(12) Uani 1 1 d D . . H21C H 0.4178 0.8007 0.0089 0.452 Uiso 1 1 calc R . . H21D H 0.4478 0.8000 0.0606 0.452 Uiso 1 1 calc R . . H21E H 0.4520 0.7193 0.0274 0.452 Uiso 1 1 calc R . . C212 C 0.5827(3) 0.5466(4) 0.0567(2) 0.0751(18) Uani 1 1 d . . . H21F H 0.5757 0.5446 0.0230 0.090 Uiso 1 1 calc R . . H21G H 0.5571 0.5150 0.0664 0.090 Uiso 1 1 calc R . . C213 C 0.6299(3) 0.4969(6) 0.0764(4) 0.119(3) Uani 1 1 d . . . H21H H 0.6386 0.5028 0.1100 0.143 Uiso 1 1 calc R . . H21I H 0.6551 0.5238 0.0642 0.143 Uiso 1 1 calc R . . C214 C 0.6245(4) 0.3943(7) 0.0627(4) 0.150(5) Uani 1 1 d . . . H21J H 0.6080 0.3895 0.0302 0.180 Uiso 1 1 calc R . . H21K H 0.6560 0.3681 0.0662 0.180 Uiso 1 1 calc R . . C215 C 0.5994(4) 0.3443(8) 0.0894(4) 0.153(4) Uani 1 1 d . . . H21L H 0.6005 0.2811 0.0820 0.230 Uiso 1 1 calc R . . H21M H 0.5668 0.3642 0.0827 0.230 Uiso 1 1 calc R . . H21N H 0.6138 0.3532 0.1218 0.230 Uiso 1 1 calc R . . O10 O 0.5000 0.310(2) 0.2500 0.385(16) Uani 1 2 d S . . 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 0.0492(3) 0.0409(2) 0.0406(2) 0.00535(18) 0.01517(19) 0.00437(19) Mo2 0.0578(3) 0.0358(2) 0.0428(2) 0.00170(18) 0.0181(2) -0.0005(2) Mo3 0.0483(3) 0.0387(2) 0.0425(2) 0.00290(18) 0.0160(2) 0.00341(19) S1 0.0582(8) 0.0372(6) 0.0445(7) 0.0036(5) 0.0196(6) 0.0001(6) S2 0.0643(10) 0.0512(8) 0.0600(8) 0.0028(6) 0.0229(7) -0.0105(7) S3 0.0621(10) 0.0629(9) 0.0518(8) 0.0033(7) 0.0102(7) -0.0024(7) S6 0.0671(9) 0.0396(7) 0.0526(8) 0.0067(6) 0.0192(7) 0.0070(6) S7 0.0639(9) 0.0498(8) 0.0610(8) 0.0013(6) 0.0300(7) 0.0092(7) S4 0.0584(9) 0.0495(7) 0.0444(7) 0.0091(6) 0.0202(6) 0.0081(6) S5 0.0643(9) 0.0460(7) 0.0473(7) -0.0009(6) 0.0165(7) 0.0062(6) S9 0.0633(10) 0.0693(10) 0.0664(9) 0.0140(8) 0.0292(8) 0.0109(8) S8 0.0705(10) 0.0529(8) 0.0629(9) 0.0181(7) 0.0280(8) 0.0180(7) S12 0.1206(15) 0.0408(8) 0.0618(9) -0.0032(7) 0.0307(10) -0.0145(8) S11 0.0782(11) 0.0455(7) 0.0474(7) 0.0006(6) 0.0244(7) -0.0053(7) S15 0.0614(10) 0.0700(10) 0.0583(9) 0.0158(7) 0.0079(7) 0.0036(8) S14 0.0622(10) 0.0572(9) 0.0617(9) 0.0019(7) 0.0181(7) -0.0109(7) S10 0.112(2) 0.152(2) 0.175(3) 0.075(2) 0.0704(19) 0.0862(18) S13 0.142(2) 0.0787(12) 0.0550(10) -0.0161(9) 0.0127(11) -0.0125(12) S16 0.0893(15) 0.0814(13) 0.1203(17) -0.0130(12) -0.0315(13) -0.0029(11) N1 0.104(5) 0.098(5) 0.126(6) 0.047(4) 0.042(4) 0.056(4) N2 0.078(4) 0.128(6) 0.102(5) 0.026(4) 0.033(4) 0.041(4) N4 0.122(5) 0.055(3) 0.074(4) -0.016(3) 0.010(3) -0.012(3) N3 0.094(4) 0.070(3) 0.046(3) -0.003(2) 0.014(3) -0.005(3) N5 0.072(4) 0.068(4) 0.109(5) -0.007(3) -0.005(3) -0.007(3) N6 0.075(4) 0.083(4) 0.074(4) -0.003(3) -0.008(3) 0.014(3) C1 0.064(4) 0.071(4) 0.065(4) 0.018(3) 0.019(3) 0.019(3) C2 0.054(4) 0.092(5) 0.059(4) 0.009(3) 0.013(3) 0.024(3) C4 0.072(4) 0.048(3) 0.057(3) 0.000(3) 0.010(3) 0.001(3) C3 0.059(4) 0.052(3) 0.047(3) 0.000(2) 0.011(3) 0.004(3) C5 0.054(4) 0.055(3) 0.071(4) -0.010(3) 0.007(3) 0.004(3) C6 0.054(4) 0.060(4) 0.064(4) -0.006(3) 0.008(3) 0.012(3) N10 0.055(3) 0.059(3) 0.052(3) 0.008(2) 0.008(2) -0.011(2) C100 0.075(4) 0.061(4) 0.061(4) 0.016(3) 0.022(3) -0.004(3) C101 0.087(6) 0.127(7) 0.058(4) 0.022(4) 0.005(4) -0.007(5) C102 0.123(8) 0.209(11) 0.075(6) 0.056(6) 0.015(5) -0.003(8) C103 0.159(13) 0.36(2) 0.207(14) 0.187(15) 0.066(11) 0.063(14) C104 0.063(4) 0.076(4) 0.063(4) 0.009(3) 0.016(3) -0.014(3) C105 0.074(5) 0.092(5) 0.091(5) -0.008(4) 0.028(4) -0.002(4) C106 0.075(5) 0.129(7) 0.085(5) -0.003(5) 0.016(4) 0.011(5) C107 0.119(8) 0.139(9) 0.136(8) -0.026(7) 0.030(7) 0.034(7) C108 0.064(4) 0.060(4) 0.061(4) 0.002(3) 0.009(3) -0.013(3) C109 0.089(6) 0.075(4) 0.074(4) 0.014(4) 0.010(4) 0.003(4) C110 0.076(5) 0.121(7) 0.064(4) 0.007(4) 0.001(4) 0.002(5) C111 0.123(7) 0.111(6) 0.068(5) -0.011(4) 0.004(5) 0.010(6) C112 0.068(4) 0.055(3) 0.061(3) 0.012(3) 0.006(3) -0.013(3) C113 0.083(5) 0.060(4) 0.098(5) 0.007(4) 0.018(4) -0.014(4) C114 0.128(7) 0.061(4) 0.106(6) 0.015(4) 0.049(6) 0.006(4) C115 0.146(9) 0.077(5) 0.110(7) 0.014(5) 0.033(6) -0.004(5) N20 0.061(3) 0.073(3) 0.066(3) -0.010(3) 0.008(3) 0.007(3) C200 0.086(6) 0.137(7) 0.060(4) -0.022(4) 0.014(4) -0.011(5) C201 0.147(10) 0.199(11) 0.084(6) -0.026(6) 0.051(6) -0.025(8) C202 0.169(12) 0.253(16) 0.098(8) -0.008(9) 0.069(8) 0.012(11) C203 0.33(3) 0.36(3) 0.140(12) 0.002(14) 0.070(14) 0.22(2) C204 0.062(4) 0.069(4) 0.081(5) -0.008(3) 0.009(4) -0.002(3) C205 0.072(5) 0.059(4) 0.073(4) 0.005(3) 0.006(3) 0.007(3) C206 0.078(5) 0.080(5) 0.089(5) 0.012(4) 0.011(4) 0.003(4) C207 0.105(7) 0.107(6) 0.102(6) 0.021(5) 0.037(5) 0.001(5) C208 0.063(4) 0.076(5) 0.103(5) -0.019(4) 0.006(4) 0.014(4) C209 0.090(7) 0.098(7) 0.223(12) -0.035(7) 0.006(8) 0.023(6) C210 0.142(12) 0.149(11) 0.279(18) -0.040(12) 0.074(13) 0.024(10) C211 0.25(2) 0.174(16) 0.50(4) -0.015(19) 0.14(2) 0.124(16) C212 0.084(5) 0.072(4) 0.071(4) 0.002(3) 0.022(4) 0.006(4) C213 0.094(7) 0.104(7) 0.162(9) 0.049(6) 0.034(6) 0.033(5) C214 0.188(11) 0.141(9) 0.156(9) 0.079(8) 0.111(9) 0.096(8) C215 0.128(10) 0.141(9) 0.192(12) 0.051(9) 0.041(9) 0.014(7) O10 0.082(9) 0.78(5) 0.263(19) 0.000 -0.027(11) 0.000 _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 S1 2.3679(14) . ? Mo1 S4 2.4024(14) . ? Mo1 S2 2.4054(15) . ? Mo1 S8 2.4548(14) . ? Mo1 S3 2.4958(16) . ? Mo1 S5 2.5120(15) . ? Mo1 S9 2.5282(16) . ? Mo1 Mo2 2.7490(7) . ? Mo1 Mo3 2.7575(8) . ? Mo2 S1 2.3631(13) . ? Mo2 S6 2.4121(14) . ? Mo2 S2 2.4131(15) . ? Mo2 S11 2.4625(14) . ? Mo2 S7 2.4940(17) . ? Mo2 S3 2.5016(17) . ? Mo2 S12 2.5075(15) . ? Mo2 Mo3 2.7623(7) . ? Mo3 S1 2.3597(13) . ? Mo3 S4 2.4088(14) . ? Mo3 S6 2.4214(14) . ? Mo3 S14 2.4594(15) . ? Mo3 S5 2.5021(14) . ? Mo3 S7 2.5058(14) . ? Mo3 S15 2.5257(16) . ? S2 S3 2.026(2) . ? S6 S7 2.030(2) . ? S4 S5 2.0281(19) . ? S9 C2 1.725(7) . ? S8 C1 1.726(6) . ? S12 C4 1.731(6) . ? S11 C3 1.719(6) . ? S15 C6 1.732(6) . ? S14 C5 1.751(6) . ? S10 N1 1.664(7) . ? S10 N2 1.670(7) . ? S13 N4 1.644(6) . ? S13 N3 1.651(5) . ? S16 N6 1.647(6) . ? S16 N5 1.649(6) . ? N1 C1 1.314(8) . ? N2 C2 1.312(8) . ? N4 C4 1.312(7) . ? N3 C3 1.324(7) . ? N5 C5 1.318(8) . ? N6 C6 1.308(8) . ? C1 C2 1.445(9) . ? C4 C3 1.439(8) . ? C5 C6 1.427(8) . ? N10 C104 1.509(8) . ? N10 C112 1.507(7) . ? N10 C100 1.517(7) . ? N10 C108 1.523(7) . ? C100 C101 1.497(9) . ? C101 C102 1.509(10) . ? C102 C103 1.446(8) . ? C104 C105 1.513(9) . ? C105 C106 1.492(10) . ? C106 C107 1.518(11) . ? C108 C109 1.525(8) . ? C109 C110 1.508(9) . ? C110 C111 1.489(10) . ? C112 C113 1.504(9) . ? C113 C114 1.516(9) . ? C114 C115 1.479(11) . ? N20 C208 1.502(8) . ? N20 C200 1.512(8) . ? N20 C204 1.513(8) . ? N20 C212 1.526(8) . ? C200 C201 1.539(12) . ? C201 C202 1.556(12) . ? C202 C203 1.400(17) . ? C204 C205 1.499(9) . ? C205 C206 1.521(9) . ? C206 C207 1.480(9) . ? C208 C209 1.545(10) . ? C209 C210 1.614(9) . ? C210 C211 1.494(9) . ? C212 C213 1.535(10) . ? C213 C214 1.567(13) . ? C214 C215 1.402(12) . ? 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 108.93(5) . . ? S1 Mo1 S2 109.49(5) . . ? S4 Mo1 S2 82.67(5) . . ? S1 Mo1 S8 76.64(5) . . ? S4 Mo1 S8 137.85(5) . . ? S2 Mo1 S8 136.39(6) . . ? S1 Mo1 S3 87.50(5) . . ? S4 Mo1 S3 131.30(5) . . ? S2 Mo1 S3 48.79(5) . . ? S8 Mo1 S3 89.90(6) . . ? S1 Mo1 S5 86.15(5) . . ? S4 Mo1 S5 48.68(5) . . ? S2 Mo1 S5 131.12(5) . . ? S8 Mo1 S5 91.69(5) . . ? S3 Mo1 S5 172.91(5) . . ? S1 Mo1 S9 160.75(5) . . ? S4 Mo1 S9 85.05(5) . . ? S2 Mo1 S9 84.84(5) . . ? S8 Mo1 S9 84.12(5) . . ? S3 Mo1 S9 93.03(6) . . ? S5 Mo1 S9 94.00(5) . . ? S1 Mo1 Mo2 54.39(3) . . ? S4 Mo1 Mo2 95.62(4) . . ? S2 Mo1 Mo2 55.35(4) . . ? S8 Mo1 Mo2 118.35(4) . . ? S3 Mo1 Mo2 56.73(4) . . ? S5 Mo1 Mo2 116.65(4) . . ? S9 Mo1 Mo2 139.52(4) . . ? S1 Mo1 Mo3 54.18(4) . . ? S4 Mo1 Mo3 55.14(4) . . ? S2 Mo1 Mo3 94.99(4) . . ? S8 Mo1 Mo3 119.81(4) . . ? S3 Mo1 Mo3 116.94(4) . . ? S5 Mo1 Mo3 56.47(3) . . ? S9 Mo1 Mo3 139.68(4) . . ? Mo2 Mo1 Mo3 60.217(17) . . ? S1 Mo2 S6 108.70(5) . . ? S1 Mo2 S2 109.39(5) . . ? S6 Mo2 S2 84.92(5) . . ? S1 Mo2 S11 77.22(4) . . ? S6 Mo2 S11 135.92(5) . . ? S2 Mo2 S11 135.77(6) . . ? S1 Mo2 S7 84.23(5) . . ? S6 Mo2 S7 48.84(5) . . ? S2 Mo2 S7 133.31(5) . . ? S11 Mo2 S7 90.27(5) . . ? S1 Mo2 S3 87.47(5) . . ? S6 Mo2 S3 133.44(5) . . ? S2 Mo2 S3 48.65(5) . . ? S11 Mo2 S3 89.57(5) . . ? S7 Mo2 S3 171.52(5) . . ? S1 Mo2 S12 161.31(5) . . ? S6 Mo2 S12 84.99(6) . . ? S2 Mo2 S12 83.87(6) . . ? S11 Mo2 S12 84.09(5) . . ? S7 Mo2 S12 96.28(6) . . ? S3 Mo2 S12 92.13(6) . . ? S1 Mo2 Mo1 54.56(3) . . ? S6 Mo2 Mo1 97.30(4) . . ? S2 Mo2 Mo1 55.08(4) . . ? S11 Mo2 Mo1 118.64(4) . . ? S7 Mo2 Mo1 116.53(4) . . ? S3 Mo2 Mo1 56.53(4) . . ? S12 Mo2 Mo1 138.25(5) . . ? S1 Mo2 Mo3 54.15(3) . . ? S6 Mo2 Mo3 55.30(4) . . ? S2 Mo2 Mo3 94.69(4) . . ? S11 Mo2 Mo3 120.73(4) . . ? S7 Mo2 Mo3 56.67(3) . . ? S3 Mo2 Mo3 116.57(4) . . ? S12 Mo2 Mo3 140.16(5) . . ? Mo1 Mo2 Mo3 60.044(18) . . ? S1 Mo3 S4 108.99(5) . . ? S1 Mo3 S6 108.49(5) . . ? S4 Mo3 S6 85.92(5) . . ? S1 Mo3 S14 78.23(5) . . ? S4 Mo3 S14 133.77(5) . . ? S6 Mo3 S14 136.59(5) . . ? S1 Mo3 S5 86.55(5) . . ? S4 Mo3 S5 48.74(5) . . ? S6 Mo3 S5 134.46(5) . . ? S14 Mo3 S5 87.84(5) . . ? S1 Mo3 S7 84.04(5) . . ? S4 Mo3 S7 134.02(5) . . ? S6 Mo3 S7 48.62(5) . . ? S14 Mo3 S7 91.55(5) . . ? S5 Mo3 S7 170.50(5) . . ? S1 Mo3 S15 161.74(5) . . ? S4 Mo3 S15 84.93(5) . . ? S6 Mo3 S15 83.63(5) . . ? S14 Mo3 S15 83.60(5) . . ? S5 Mo3 S15 94.57(5) . . ? S7 Mo3 S15 94.78(6) . . ? S1 Mo3 Mo1 54.46(3) . . ? S4 Mo3 Mo1 54.92(4) . . ? S6 Mo3 Mo1 96.85(4) . . ? S14 Mo3 Mo1 119.08(4) . . ? S5 Mo3 Mo1 56.81(4) . . ? S7 Mo3 Mo1 115.82(4) . . ? S15 Mo3 Mo1 139.55(4) . . ? S1 Mo3 Mo2 54.26(3) . . ? S4 Mo3 Mo2 95.13(4) . . ? S6 Mo3 Mo2 54.99(4) . . ? S14 Mo3 Mo2 122.14(4) . . ? S5 Mo3 Mo2 116.51(4) . . ? S7 Mo3 Mo2 56.26(4) . . ? S15 Mo3 Mo2 138.40(4) . . ? Mo1 Mo3 Mo2 59.739(17) . . ? Mo3 S1 Mo2 71.59(4) . . ? Mo3 S1 Mo1 71.36(4) . . ? Mo2 S1 Mo1 71.05(4) . . ? S3 S2 Mo1 67.93(6) . . ? S3 S2 Mo2 67.96(6) . . ? Mo1 S2 Mo2 69.57(4) . . ? S2 S3 Mo1 63.27(6) . . ? S2 S3 Mo2 63.39(6) . . ? Mo1 S3 Mo2 66.75(4) . . ? S7 S6 Mo2 67.68(6) . . ? S7 S6 Mo3 67.86(6) . . ? Mo2 S6 Mo3 69.71(4) . . ? S6 S7 Mo2 63.47(6) . . ? S6 S7 Mo3 63.52(5) . . ? Mo2 S7 Mo3 67.08(4) . . ? S5 S4 Mo1 68.48(5) . . ? S5 S4 Mo3 68.03(6) . . ? Mo1 S4 Mo3 69.94(4) . . ? S4 S5 Mo3 63.23(5) . . ? S4 S5 Mo1 62.84(6) . . ? Mo3 S5 Mo1 66.73(4) . . ? C2 S9 Mo1 103.8(2) . . ? C1 S8 Mo1 105.5(2) . . ? C4 S12 Mo2 104.10(19) . . ? C3 S11 Mo2 105.25(19) . . ? C6 S15 Mo3 103.0(2) . . ? C5 S14 Mo3 104.5(2) . . ? N1 S10 N2 98.8(3) . . ? N4 S13 N3 98.5(3) . . ? N6 S16 N5 99.2(3) . . ? C1 N1 S10 106.2(5) . . ? C2 N2 S10 106.1(5) . . ? C4 N4 S13 107.3(4) . . ? C3 N3 S13 106.9(4) . . ? C5 N5 S16 105.3(5) . . ? C6 N6 S16 106.9(5) . . ? N1 C1 C2 114.5(6) . . ? N1 C1 S8 122.1(5) . . ? C2 C1 S8 123.5(5) . . ? N2 C2 C1 114.5(6) . . ? N2 C2 S9 122.5(6) . . ? C1 C2 S9 123.1(5) . . ? N4 C4 C3 113.9(5) . . ? N4 C4 S12 123.3(5) . . ? C3 C4 S12 122.8(4) . . ? N3 C3 C4 113.3(5) . . ? N3 C3 S11 123.1(4) . . ? C4 C3 S11 123.6(4) . . ? N5 C5 C6 115.3(6) . . ? N5 C5 S14 121.8(5) . . ? C6 C5 S14 123.0(5) . . ? N6 C6 C5 113.4(6) . . ? N6 C6 S15 123.7(5) . . ? C5 C6 S15 122.9(5) . . ? C104 N10 C112 106.2(4) . . ? C104 N10 C100 111.7(5) . . ? C112 N10 C100 111.0(4) . . ? C104 N10 C108 110.4(5) . . ? C112 N10 C108 112.2(5) . . ? C100 N10 C108 105.5(4) . . ? C101 C100 N10 115.8(5) . . ? C100 C101 C102 107.1(6) . . ? C103 C102 C101 119.1(9) . . ? N10 C104 C105 116.5(5) . . ? C106 C105 C104 111.5(6) . . ? C105 C106 C107 113.4(8) . . ? C109 C108 N10 115.5(5) . . ? C110 C109 C108 110.4(6) . . ? C111 C110 C109 115.6(7) . . ? C113 C112 N10 116.4(5) . . ? C112 C113 C114 111.5(6) . . ? C115 C114 C113 113.6(7) . . ? C208 N20 C200 112.1(6) . . ? C208 N20 C204 110.5(5) . . ? C200 N20 C204 105.9(5) . . ? C208 N20 C212 106.0(5) . . ? C200 N20 C212 111.1(5) . . ? C204 N20 C212 111.2(5) . . ? N20 C200 C201 115.9(6) . . ? C200 C201 C202 109.1(9) . . ? C203 C202 C201 113.7(12) . . ? C205 C204 N20 118.0(5) . . ? C204 C205 C206 109.0(6) . . ? C207 C206 C205 113.9(6) . . ? N20 C208 C209 115.8(6) . . ? C208 C209 C210 111.8(8) . . ? C211 C210 C209 95.1(12) . . ? N20 C212 C213 113.4(6) . . ? C212 C213 C214 109.8(8) . . ? C215 C214 C213 113.4(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.847 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.103 #===END data_(ET)2[Mo3S7(tdas)3] _database_code_depnum_ccdc_archive 'CCDC 639724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 Mo3 N6 S32' _chemical_formula_weight 1726.19 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4374(6) _cell_length_b 21.6924(9) _cell_length_c 17.2853(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.7440(10) _cell_angle_gamma 90.00 _cell_volume 5258.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5547 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 30.61 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 2.011 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _Ratio_of_minimum_to_maximum_apparent_transmission 0.806894 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42508 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 30.00 _reflns_number_total 15163 _reflns_number_gt 11719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0517P)^2^+0.0000P] 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 15163 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 0.235112(15) 0.303542(10) 0.540353(13) 0.01748(5) Uani 1 1 d . . . Mo2 Mo 0.245986(15) 0.225542(10) 0.668642(12) 0.01546(5) Uani 1 1 d . . . Mo3 Mo 0.240835(15) 0.177887(10) 0.518793(13) 0.01704(5) Uani 1 1 d . . . S1 S 0.36475(4) 0.23821(3) 0.59685(4) 0.01802(12) Uani 1 1 d . . . S2 S 0.12085(5) 0.30020(3) 0.62286(4) 0.02165(13) Uani 1 1 d . . . S3 S 0.24584(5) 0.34093(3) 0.67832(4) 0.02135(13) Uani 1 1 d . . . S4 S 0.11382(5) 0.24508(3) 0.45055(4) 0.02293(14) Uani 1 1 d . . . S5 S 0.23316(5) 0.25350(4) 0.40977(4) 0.02703(15) Uani 1 1 d . . . S6 S 0.13049(5) 0.15151(3) 0.59882(4) 0.02097(13) Uani 1 1 d . . . S7 S 0.26136(5) 0.11331(3) 0.64238(4) 0.02087(13) Uani 1 1 d . . . S8 S 0.14477(5) 0.39834(4) 0.48410(5) 0.03251(17) Uani 1 1 d . . . S9 S 0.37591(5) 0.36055(3) 0.52422(4) 0.02477(14) Uani 1 1 d . . . S10 S 0.31577(8) 0.52854(4) 0.41786(7) 0.0571(3) Uani 1 1 d . . . S11 S 0.39474(5) 0.22105(3) 0.77517(4) 0.01957(13) Uani 1 1 d . . . S12 S 0.16780(5) 0.21084(4) 0.78261(4) 0.02667(15) Uani 1 1 d . . . S13 S 0.35568(6) 0.15201(4) 0.98581(5) 0.03529(18) Uani 1 1 d . . . S14 S 0.15343(5) 0.09601(4) 0.42643(4) 0.02717(15) Uani 1 1 d . . . S15 S 0.38349(5) 0.13454(4) 0.48377(4) 0.02775(15) Uani 1 1 d . . . S16 S 0.31617(7) 0.03174(5) 0.27957(5) 0.0484(3) Uani 1 1 d . . . N1 N 0.3859(2) 0.47082(13) 0.45626(17) 0.0419(7) Uani 1 1 d . . . N2 N 0.2131(2) 0.50045(13) 0.42823(18) 0.0443(7) Uani 1 1 d . . . N3 N 0.41969(18) 0.17675(11) 0.92478(14) 0.0275(5) Uani 1 1 d . . . N4 N 0.24816(18) 0.16438(13) 0.92791(15) 0.0322(6) Uani 1 1 d . . . N5 N 0.3884(2) 0.06995(15) 0.35212(16) 0.0445(8) Uani 1 1 d . . . N6 N 0.21557(19) 0.04207(12) 0.30764(14) 0.0318(6) Uani 1 1 d . . . C1 C 0.3311(2) 0.42905(14) 0.47787(17) 0.0288(6) Uani 1 1 d . . . C2 C 0.2320(2) 0.44583(14) 0.46189(17) 0.0294(6) Uani 1 1 d . . . C3 C 0.35904(19) 0.19426(12) 0.85840(15) 0.0207(5) Uani 1 1 d . . . C4 C 0.2609(2) 0.18752(12) 0.86032(16) 0.0225(5) Uani 1 1 d . . . C5 C 0.3360(2) 0.09140(15) 0.39882(17) 0.0288(6) Uani 1 1 d . . . C6 C 0.2363(2) 0.07512(13) 0.37346(16) 0.0251(6) Uani 1 1 d . . . S20 S 0.13596(5) 0.38842(3) 1.07735(4) 0.02188(13) Uani 1 1 d . . . S21 S 0.15815(5) 0.28784(3) 0.97139(4) 0.02359(14) Uani 1 1 d . . . S22 S 0.14780(6) 0.30904(3) 1.21906(4) 0.02715(15) Uani 1 1 d . . . S23 S 0.17509(6) 0.18924(3) 1.08898(5) 0.03351(18) Uani 1 1 d . . . S24 S 0.10802(5) 0.48377(3) 0.93296(4) 0.02515(14) Uani 1 1 d . . . S25 S 0.12718(6) 0.38479(3) 0.82515(4) 0.03162(17) Uani 1 1 d . . . S26 S 0.02980(5) 0.57532(3) 0.80850(4) 0.02378(14) Uani 1 1 d . . . S27 S 0.06754(10) 0.45731(4) 0.67844(5) 0.0581(3) Uani 1 1 d . . . C20 C 0.12745(19) 0.40688(12) 0.92032(15) 0.0215(5) Uani 1 1 d . . . C21 C 0.14145(19) 0.36529(12) 0.98339(15) 0.0210(5) Uani 1 1 d . . . C22 C 0.15048(19) 0.31479(12) 1.11876(15) 0.0203(5) Uani 1 1 d . . . C23 C 0.16056(19) 0.26784(12) 1.06953(16) 0.0218(5) Uani 1 1 d . . . C24 C 0.1053(2) 0.23051(13) 1.21645(16) 0.0243(6) Uani 1 1 d . . . H24A H 0.0963 0.2196 1.2686 0.029 Uiso 1 1 calc R . . H24B H 0.0438 0.2277 1.1788 0.029 Uiso 1 1 calc R . . C25 C 0.1731(2) 0.18479(13) 1.19304(17) 0.0266(6) Uani 1 1 d . . . H25A H 0.1547 0.1434 1.2046 0.032 Uiso 1 1 calc R . . H25B H 0.2369 0.1922 1.2252 0.032 Uiso 1 1 calc R . . C26 C 0.07543(19) 0.50137(12) 0.83198(15) 0.0215(5) Uani 1 1 d . . . C27 C 0.0874(2) 0.45579(13) 0.78184(16) 0.0284(6) Uani 1 1 d . . . C28 C -0.0081(2) 0.57095(13) 0.70099(16) 0.0258(6) Uani 1 1 d . . . H28A H -0.0683 0.5489 0.6867 0.031 Uiso 1 1 calc R . . H28B H -0.0192 0.6124 0.6798 0.031 Uiso 1 1 calc R . . C29 C 0.0626(3) 0.53934(15) 0.66233(18) 0.0368(8) Uani 1 1 d . . . H29A H 0.1254 0.5567 0.6835 0.044 Uiso 1 1 calc R . . H29B H 0.0452 0.5474 0.6055 0.044 Uiso 1 1 calc R . . S30 S 0.13572(6) 0.98117(3) 0.58011(4) 0.02970(16) Uani 1 1 d . . . S31 S 0.09540(6) 0.85428(3) 0.61591(4) 0.02762(15) Uani 1 1 d . . . S32 S 0.11840(7) 1.03250(4) 0.73451(5) 0.03743(19) Uani 1 1 d . . . S33 S 0.04712(5) 0.88139(4) 0.76846(4) 0.02869(15) Uani 1 1 d . . . S34 S 0.13259(6) 0.93469(3) 0.39562(4) 0.02798(15) Uani 1 1 d . . . S35 S 0.10076(5) 0.80919(3) 0.44562(4) 0.02610(14) Uani 1 1 d . . . S36 S 0.12009(6) 0.90250(4) 0.22727(5) 0.03430(17) Uani 1 1 d . . . S37 S 0.07861(6) 0.75209(4) 0.28899(5) 0.03518(18) Uani 1 1 d . . . C30 C 0.1185(2) 0.88617(13) 0.47097(16) 0.0245(6) Uani 1 1 d . . . C31 C 0.11715(19) 0.90627(13) 0.54695(16) 0.0233(5) Uani 1 1 d . . . C32 C 0.1102(2) 0.96772(13) 0.67254(16) 0.0252(6) Uani 1 1 d . . . C33 C 0.08639(19) 0.90966(13) 0.68734(16) 0.0229(5) Uani 1 1 d . . . C34 C 0.1062(2) 0.99720(15) 0.82661(18) 0.0343(7) Uani 1 1 d . . . H34A H 0.1645 0.9753 0.8507 0.041 Uiso 1 1 calc R . . H34B H 0.0973 1.0292 0.8634 0.041 Uiso 1 1 calc R . . C35 C 0.0230(2) 0.95284(14) 0.81364(18) 0.0311(7) Uani 1 1 d . . . H35A H -0.0326 0.9722 0.7797 0.037 Uiso 1 1 calc R . . H35B H 0.0084 0.9440 0.8645 0.037 Uiso 1 1 calc R . . C36 C 0.1165(2) 0.87783(14) 0.32279(17) 0.0276(6) Uani 1 1 d . . . C37 C 0.1016(2) 0.81939(14) 0.34583(17) 0.0265(6) Uani 1 1 d . . . C38 C 0.0450(3) 0.84395(19) 0.16962(19) 0.0443(9) Uani 1 1 d . . . H38A H -0.0187 0.8475 0.1784 0.053 Uiso 1 1 calc R . . H38B H 0.0405 0.8513 0.1135 0.053 Uiso 1 1 calc R . . C39 C 0.0811(3) 0.77883(19) 0.1901(2) 0.0495(10) Uani 1 1 d . . . H39A H 0.1462 0.7764 0.1844 0.059 Uiso 1 1 calc R . . H39B H 0.0431 0.7509 0.1515 0.059 Uiso 1 1 calc R . . 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 0.01620(10) 0.02033(11) 0.01563(10) 0.00235(8) 0.00321(8) -0.00112(8) Mo2 0.01436(10) 0.01770(11) 0.01501(10) 0.00037(8) 0.00489(7) 0.00002(8) Mo3 0.01323(10) 0.02168(11) 0.01618(10) -0.00233(8) 0.00346(7) -0.00057(8) S1 0.0144(3) 0.0236(3) 0.0161(3) -0.0002(2) 0.0037(2) -0.0018(2) S2 0.0172(3) 0.0243(3) 0.0245(3) 0.0024(3) 0.0071(2) 0.0029(2) S3 0.0227(3) 0.0202(3) 0.0214(3) -0.0013(2) 0.0058(2) 0.0009(2) S4 0.0167(3) 0.0290(4) 0.0211(3) 0.0004(3) 0.0005(2) -0.0001(3) S5 0.0237(3) 0.0414(4) 0.0159(3) 0.0012(3) 0.0046(2) -0.0044(3) S6 0.0159(3) 0.0234(3) 0.0241(3) -0.0005(2) 0.0058(2) -0.0023(2) S7 0.0189(3) 0.0193(3) 0.0245(3) 0.0009(2) 0.0054(2) 0.0004(2) S8 0.0274(4) 0.0323(4) 0.0369(4) 0.0153(3) 0.0057(3) 0.0048(3) S9 0.0229(3) 0.0288(4) 0.0227(3) 0.0024(3) 0.0055(3) -0.0067(3) S10 0.0660(7) 0.0311(5) 0.0732(7) 0.0186(5) 0.0146(5) -0.0125(4) S11 0.0177(3) 0.0247(3) 0.0168(3) 0.0015(2) 0.0050(2) -0.0011(2) S12 0.0193(3) 0.0405(4) 0.0225(3) 0.0053(3) 0.0097(3) 0.0023(3) S13 0.0388(4) 0.0447(5) 0.0242(4) 0.0141(3) 0.0111(3) 0.0060(4) S14 0.0211(3) 0.0330(4) 0.0280(4) -0.0123(3) 0.0069(3) -0.0047(3) S15 0.0169(3) 0.0405(4) 0.0258(3) -0.0097(3) 0.0049(3) 0.0024(3) S16 0.0380(5) 0.0750(7) 0.0327(4) -0.0257(4) 0.0092(4) 0.0102(5) N1 0.0472(18) 0.0334(15) 0.0443(17) 0.0063(12) 0.0094(13) -0.0150(13) N2 0.0555(19) 0.0273(15) 0.0485(18) 0.0122(13) 0.0090(14) 0.0014(13) N3 0.0291(13) 0.0328(14) 0.0216(12) 0.0051(10) 0.0081(10) 0.0020(10) N4 0.0318(14) 0.0415(15) 0.0265(13) 0.0112(11) 0.0133(10) 0.0037(11) N5 0.0295(15) 0.070(2) 0.0342(15) -0.0208(14) 0.0084(12) 0.0088(14) N6 0.0334(14) 0.0383(15) 0.0226(12) -0.0081(11) 0.0048(10) 0.0050(11) C1 0.0365(17) 0.0272(15) 0.0211(14) -0.0003(11) 0.0038(12) -0.0084(12) C2 0.0391(17) 0.0247(15) 0.0234(14) 0.0039(11) 0.0056(12) -0.0046(12) C3 0.0254(13) 0.0208(13) 0.0172(12) -0.0003(10) 0.0077(10) 0.0019(10) C4 0.0268(14) 0.0216(13) 0.0214(13) 0.0033(10) 0.0102(10) 0.0024(11) C5 0.0225(14) 0.0402(17) 0.0231(14) -0.0049(12) 0.0042(11) 0.0064(12) C6 0.0260(14) 0.0260(14) 0.0232(14) -0.0019(11) 0.0054(11) 0.0039(11) S20 0.0267(3) 0.0201(3) 0.0195(3) 0.0029(2) 0.0067(2) 0.0029(3) S21 0.0332(4) 0.0199(3) 0.0183(3) 0.0026(2) 0.0074(3) 0.0016(3) S22 0.0386(4) 0.0258(4) 0.0189(3) 0.0041(3) 0.0104(3) 0.0026(3) S23 0.0537(5) 0.0214(3) 0.0314(4) 0.0071(3) 0.0218(4) 0.0082(3) S24 0.0345(4) 0.0204(3) 0.0196(3) 0.0034(2) 0.0045(3) 0.0017(3) S25 0.0511(5) 0.0251(4) 0.0206(3) 0.0059(3) 0.0123(3) 0.0137(3) S26 0.0266(3) 0.0210(3) 0.0230(3) 0.0041(2) 0.0046(3) 0.0033(3) S27 0.1191(10) 0.0359(5) 0.0196(4) 0.0071(3) 0.0173(5) 0.0335(5) C20 0.0235(13) 0.0220(13) 0.0195(13) 0.0045(10) 0.0063(10) 0.0024(10) C21 0.0230(13) 0.0218(13) 0.0184(12) 0.0018(10) 0.0055(10) 0.0002(10) C22 0.0226(13) 0.0209(13) 0.0181(12) 0.0059(10) 0.0059(10) 0.0031(10) C23 0.0225(13) 0.0240(14) 0.0202(13) 0.0075(10) 0.0073(10) 0.0018(10) C24 0.0234(14) 0.0309(15) 0.0192(13) 0.0057(11) 0.0063(10) -0.0028(11) C25 0.0279(15) 0.0248(14) 0.0266(14) 0.0083(11) 0.0056(11) 0.0002(11) C26 0.0228(13) 0.0225(13) 0.0197(12) 0.0049(10) 0.0064(10) 0.0015(10) C27 0.0419(18) 0.0250(14) 0.0205(13) 0.0080(11) 0.0117(12) 0.0095(12) C28 0.0294(15) 0.0250(14) 0.0207(13) 0.0049(11) 0.0014(11) 0.0025(11) C29 0.052(2) 0.0359(17) 0.0244(15) 0.0115(13) 0.0119(14) 0.0143(15) S30 0.0427(4) 0.0244(4) 0.0247(3) 0.0020(3) 0.0135(3) -0.0051(3) S31 0.0347(4) 0.0242(4) 0.0248(3) 0.0035(3) 0.0087(3) -0.0037(3) S32 0.0583(6) 0.0285(4) 0.0308(4) -0.0020(3) 0.0211(4) -0.0074(4) S33 0.0304(4) 0.0311(4) 0.0268(4) 0.0071(3) 0.0113(3) -0.0020(3) S34 0.0350(4) 0.0266(4) 0.0232(3) 0.0027(3) 0.0088(3) 0.0019(3) S35 0.0259(3) 0.0257(3) 0.0273(4) 0.0007(3) 0.0075(3) -0.0002(3) S36 0.0393(4) 0.0406(4) 0.0253(4) 0.0009(3) 0.0122(3) 0.0005(3) S37 0.0331(4) 0.0352(4) 0.0363(4) -0.0100(3) 0.0065(3) 0.0018(3) C30 0.0222(14) 0.0271(14) 0.0240(14) 0.0024(11) 0.0054(10) 0.0006(11) C31 0.0236(13) 0.0215(13) 0.0236(13) 0.0043(10) 0.0034(10) 0.0007(10) C32 0.0264(14) 0.0266(14) 0.0229(13) -0.0004(11) 0.0065(11) -0.0024(11) C33 0.0217(13) 0.0269(14) 0.0199(13) 0.0039(10) 0.0048(10) -0.0020(11) C34 0.0470(19) 0.0329(17) 0.0247(15) -0.0004(12) 0.0121(13) 0.0035(14) C35 0.0328(16) 0.0335(17) 0.0309(16) 0.0090(12) 0.0151(13) 0.0087(13) C36 0.0242(14) 0.0349(16) 0.0243(14) -0.0031(12) 0.0071(11) 0.0046(12) C37 0.0213(14) 0.0329(16) 0.0254(14) -0.0057(11) 0.0057(11) 0.0042(11) C38 0.0385(19) 0.068(3) 0.0277(17) 0.0036(16) 0.0112(14) -0.0169(17) C39 0.050(2) 0.065(3) 0.040(2) -0.0255(18) 0.0252(17) -0.0237(19) _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 S1 2.3657(7) . ? Mo1 S4 2.4067(7) . ? Mo1 S2 2.4245(7) . ? Mo1 S9 2.4512(7) . ? Mo1 S3 2.4887(7) . ? Mo1 S5 2.4987(7) . ? Mo1 S8 2.5046(8) . ? Mo1 Mo3 2.7550(3) . ? Mo1 Mo2 2.7640(3) . ? Mo2 S1 2.3594(7) . ? Mo2 S2 2.4153(7) . ? Mo2 S6 2.4207(7) . ? Mo2 S11 2.4766(7) . ? Mo2 S7 2.4961(7) . ? Mo2 S3 2.5087(7) . ? Mo2 S12 2.5127(7) . ? Mo2 Mo3 2.7734(3) . ? Mo3 S1 2.3635(7) . ? Mo3 S6 2.4137(7) . ? Mo3 S4 2.4189(7) . ? Mo3 S15 2.4668(7) . ? Mo3 S5 2.4809(8) . ? Mo3 S7 2.5125(7) . ? Mo3 S14 2.5177(7) . ? S2 S3 2.0332(9) . ? S4 S5 2.0189(10) . ? S6 S7 2.0364(9) . ? S8 C2 1.739(3) . ? S9 C1 1.739(3) . ? S10 N1 1.647(3) . ? S10 N2 1.651(3) . ? S11 C3 1.739(3) . ? S12 C4 1.735(3) . ? S13 N3 1.649(2) . ? S13 N4 1.657(3) . ? S14 C6 1.731(3) . ? S15 C5 1.739(3) . ? S16 N5 1.651(3) . ? S16 N6 1.652(3) . ? N1 C1 1.314(4) . ? N2 C2 1.319(4) . ? N3 C3 1.323(3) . ? N4 C4 1.324(3) . ? N5 C5 1.316(4) . ? N6 C6 1.318(4) . ? C1 C2 1.438(4) . ? C3 C4 1.432(4) . ? C5 C6 1.445(4) . ? S20 C21 1.720(3) . ? S20 C22 1.743(3) . ? S21 C21 1.717(3) . ? S21 C23 1.743(3) . ? S22 C22 1.748(3) . ? S22 C24 1.808(3) . ? S23 C23 1.741(3) . ? S23 C25 1.809(3) . ? S24 C20 1.714(3) . ? S24 C26 1.739(3) . ? S25 C20 1.713(3) . ? S25 C27 1.749(3) . ? S26 C26 1.745(3) . ? S26 C28 1.811(3) . ? S27 C27 1.742(3) . ? S27 C29 1.800(3) . ? C20 C21 1.392(4) . ? C22 C23 1.357(4) . ? C24 C25 1.514(4) . ? C26 C27 1.353(4) . ? C28 C29 1.511(4) . ? S30 C31 1.723(3) . ? S30 C32 1.748(3) . ? S31 C31 1.723(3) . ? S31 C33 1.750(3) . ? S32 C32 1.754(3) . ? S32 C34 1.813(3) . ? S33 C33 1.744(3) . ? S33 C35 1.806(3) . ? S34 C30 1.724(3) . ? S34 C36 1.738(3) . ? S35 C30 1.730(3) . ? S35 C37 1.742(3) . ? S36 C36 1.748(3) . ? S36 C38 1.808(4) . ? S37 C37 1.747(3) . ? S37 C39 1.813(4) . ? C30 C31 1.388(4) . ? C32 C33 1.346(4) . ? C34 C35 1.513(4) . ? C36 C37 1.361(4) . ? C38 C39 1.518(6) . ? 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 109.49(2) . . ? S1 Mo1 S2 108.75(2) . . ? S4 Mo1 S2 82.60(2) . . ? S1 Mo1 S9 75.70(2) . . ? S4 Mo1 S9 133.51(3) . . ? S2 Mo1 S9 141.31(3) . . ? S1 Mo1 S3 86.37(2) . . ? S4 Mo1 S3 131.29(2) . . ? S2 Mo1 S3 48.87(2) . . ? S9 Mo1 S3 94.60(2) . . ? S1 Mo1 S5 87.17(2) . . ? S4 Mo1 S5 48.56(2) . . ? S2 Mo1 S5 130.93(3) . . ? S9 Mo1 S5 87.02(2) . . ? S3 Mo1 S5 172.73(3) . . ? S1 Mo1 S8 160.06(3) . . ? S4 Mo1 S8 87.15(3) . . ? S2 Mo1 S8 83.60(3) . . ? S9 Mo1 S8 84.90(3) . . ? S3 Mo1 S8 90.72(3) . . ? S5 Mo1 S8 96.48(3) . . ? S1 Mo1 Mo3 54.334(17) . . ? S4 Mo1 Mo3 55.393(18) . . ? S2 Mo1 Mo3 95.533(18) . . ? S9 Mo1 Mo3 115.56(2) . . ? S3 Mo1 Mo3 117.066(18) . . ? S5 Mo1 Mo3 56.100(19) . . ? S8 Mo1 Mo3 142.13(2) . . ? S1 Mo1 Mo2 54.094(16) . . ? S4 Mo1 Mo2 95.097(19) . . ? S2 Mo1 Mo2 55.017(17) . . ? S9 Mo1 Mo2 120.631(19) . . ? S3 Mo1 Mo2 56.767(17) . . ? S5 Mo1 Mo2 116.43(2) . . ? S8 Mo1 Mo2 137.66(2) . . ? Mo3 Mo1 Mo2 60.333(8) . . ? S1 Mo2 S2 109.27(2) . . ? S1 Mo2 S6 108.40(2) . . ? S2 Mo2 S6 84.75(2) . . ? S1 Mo2 S11 77.61(2) . . ? S2 Mo2 S11 135.97(2) . . ? S6 Mo2 S11 135.85(2) . . ? S1 Mo2 S7 84.88(2) . . ? S2 Mo2 S7 133.34(2) . . ? S6 Mo2 S7 48.91(2) . . ? S11 Mo2 S7 89.89(2) . . ? S1 Mo2 S3 86.05(2) . . ? S2 Mo2 S3 48.73(2) . . ? S6 Mo2 S3 133.14(2) . . ? S11 Mo2 S3 90.23(2) . . ? S7 Mo2 S3 170.69(2) . . ? S1 Mo2 S12 160.94(2) . . ? S2 Mo2 S12 84.35(2) . . ? S6 Mo2 S12 85.53(2) . . ? S11 Mo2 S12 83.33(2) . . ? S7 Mo2 S12 95.44(3) . . ? S3 Mo2 S12 93.82(2) . . ? S1 Mo2 Mo1 54.307(17) . . ? S2 Mo2 Mo1 55.331(17) . . ? S6 Mo2 Mo1 96.030(18) . . ? S11 Mo2 Mo1 119.638(17) . . ? S7 Mo2 Mo1 116.214(18) . . ? S3 Mo2 Mo1 56.077(16) . . ? S12 Mo2 Mo1 139.13(2) . . ? S1 Mo2 Mo3 54.110(16) . . ? S2 Mo2 Mo3 95.273(18) . . ? S6 Mo2 Mo3 54.875(17) . . ? S11 Mo2 Mo3 120.388(18) . . ? S7 Mo2 Mo3 56.660(16) . . ? S3 Mo2 Mo3 115.717(17) . . ? S12 Mo2 Mo3 140.14(2) . . ? Mo1 Mo2 Mo3 59.674(8) . . ? S1 Mo3 S6 108.50(2) . . ? S1 Mo3 S4 109.15(2) . . ? S6 Mo3 S4 83.99(2) . . ? S1 Mo3 S15 77.78(2) . . ? S6 Mo3 S15 138.89(3) . . ? S4 Mo3 S15 133.66(3) . . ? S1 Mo3 S5 87.63(2) . . ? S6 Mo3 S5 132.50(3) . . ? S4 Mo3 S5 48.64(2) . . ? S15 Mo3 S5 87.41(3) . . ? S1 Mo3 S7 84.43(2) . . ? S6 Mo3 S7 48.78(2) . . ? S4 Mo3 S7 132.31(2) . . ? S15 Mo3 S7 93.41(2) . . ? S5 Mo3 S7 171.66(2) . . ? S1 Mo3 S14 161.79(2) . . ? S6 Mo3 S14 84.06(2) . . ? S4 Mo3 S14 84.73(3) . . ? S15 Mo3 S14 84.11(2) . . ? S5 Mo3 S14 93.41(3) . . ? S7 Mo3 S14 94.93(3) . . ? S1 Mo3 Mo1 54.407(17) . . ? S6 Mo3 Mo1 96.428(18) . . ? S4 Mo3 Mo1 54.979(18) . . ? S15 Mo3 Mo1 117.64(2) . . ? S5 Mo3 Mo1 56.719(19) . . ? S7 Mo3 Mo1 115.969(18) . . ? S14 Mo3 Mo1 139.21(2) . . ? S1 Mo3 Mo2 53.971(16) . . ? S6 Mo3 Mo2 55.112(17) . . ? S4 Mo3 Mo2 94.579(18) . . ? S15 Mo3 Mo2 122.182(19) . . ? S5 Mo3 Mo2 116.71(2) . . ? S7 Mo3 Mo2 56.095(17) . . ? S14 Mo3 Mo2 138.88(2) . . ? Mo1 Mo3 Mo2 59.993(8) . . ? Mo2 S1 Mo3 71.919(19) . . ? Mo2 S1 Mo1 71.599(19) . . ? Mo3 S1 Mo1 71.260(19) . . ? S3 S2 Mo2 68.03(3) . . ? S3 S2 Mo1 67.21(3) . . ? Mo2 S2 Mo1 69.652(19) . . ? S2 S3 Mo1 63.92(3) . . ? S2 S3 Mo2 63.24(3) . . ? Mo1 S3 Mo2 67.156(18) . . ? S5 S4 Mo1 68.10(3) . . ? S5 S4 Mo3 67.28(3) . . ? Mo1 S4 Mo3 69.628(19) . . ? S4 S5 Mo3 64.07(3) . . ? S4 S5 Mo1 63.34(3) . . ? Mo3 S5 Mo1 67.180(19) . . ? S7 S6 Mo3 68.14(3) . . ? S7 S6 Mo2 67.48(3) . . ? Mo3 S6 Mo2 70.013(19) . . ? S6 S7 Mo2 63.62(3) . . ? S6 S7 Mo3 63.08(3) . . ? Mo2 S7 Mo3 67.245(18) . . ? C2 S8 Mo1 103.57(11) . . ? C1 S9 Mo1 104.82(11) . . ? N1 S10 N2 99.05(14) . . ? C3 S11 Mo2 104.66(9) . . ? C4 S12 Mo2 103.53(9) . . ? N3 S13 N4 98.51(12) . . ? C6 S14 Mo3 102.40(10) . . ? C5 S15 Mo3 103.15(10) . . ? N5 S16 N6 98.63(13) . . ? C1 N1 S10 106.6(2) . . ? C2 N2 S10 106.4(2) . . ? C3 N3 S13 107.0(2) . . ? C4 N4 S13 106.7(2) . . ? C5 N5 S16 106.9(2) . . ? C6 N6 S16 107.0(2) . . ? N1 C1 C2 114.2(3) . . ? N1 C1 S9 122.5(3) . . ? C2 C1 S9 123.3(2) . . ? N2 C2 C1 113.8(3) . . ? N2 C2 S8 123.0(3) . . ? C1 C2 S8 123.2(2) . . ? N3 C3 C4 113.9(2) . . ? N3 C3 S11 123.2(2) . . ? C4 C3 S11 122.8(2) . . ? N4 C4 C3 113.9(2) . . ? N4 C4 S12 123.3(2) . . ? C3 C4 S12 122.8(2) . . ? N5 C5 C6 113.8(3) . . ? N5 C5 S15 122.6(2) . . ? C6 C5 S15 123.5(2) . . ? N6 C6 C5 113.6(3) . . ? N6 C6 S14 123.7(2) . . ? C5 C6 S14 122.6(2) . . ? C21 S20 C22 95.30(13) . . ? C21 S21 C23 95.56(13) . . ? C22 S22 C24 97.47(13) . . ? C23 S23 C25 102.40(13) . . ? C20 S24 C26 95.69(13) . . ? C20 S25 C27 95.18(13) . . ? C26 S26 C28 101.30(13) . . ? C27 S27 C29 99.69(14) . . ? C21 C20 S25 122.5(2) . . ? C21 C20 S24 121.9(2) . . ? S25 C20 S24 115.57(15) . . ? C20 C21 S21 122.5(2) . . ? C20 C21 S20 121.3(2) . . ? S21 C21 S20 116.04(15) . . ? C23 C22 S20 116.8(2) . . ? C23 C22 S22 126.8(2) . . ? S20 C22 S22 116.36(15) . . ? C22 C23 S23 129.8(2) . . ? C22 C23 S21 116.3(2) . . ? S23 C23 S21 113.91(15) . . ? C25 C24 S22 112.74(19) . . ? C24 C25 S23 113.25(19) . . ? C27 C26 S24 115.9(2) . . ? C27 C26 S26 128.4(2) . . ? S24 C26 S26 115.63(15) . . ? C26 C27 S27 129.0(2) . . ? C26 C27 S25 116.6(2) . . ? S27 C27 S25 114.40(16) . . ? C29 C28 S26 114.0(2) . . ? C28 C29 S27 112.7(2) . . ? C31 S30 C32 95.55(14) . . ? C31 S31 C33 95.46(13) . . ? C32 S32 C34 101.02(14) . . ? C33 S33 C35 100.30(14) . . ? C30 S34 C36 95.42(14) . . ? C30 S35 C37 95.33(14) . . ? C36 S36 C38 99.03(15) . . ? C37 S37 C39 102.66(16) . . ? C31 C30 S34 123.6(2) . . ? C31 C30 S35 120.6(2) . . ? S34 C30 S35 115.78(16) . . ? C30 C31 S31 119.6(2) . . ? C30 C31 S30 125.1(2) . . ? S31 C31 S30 115.26(16) . . ? C33 C32 S30 116.7(2) . . ? C33 C32 S32 128.1(2) . . ? S30 C32 S32 115.22(16) . . ? C32 C33 S33 128.9(2) . . ? C32 C33 S31 116.3(2) . . ? S33 C33 S31 114.76(16) . . ? C35 C34 S32 112.2(2) . . ? C34 C35 S33 112.5(2) . . ? C37 C36 S34 116.9(2) . . ? C37 C36 S36 127.1(2) . . ? S34 C36 S36 115.98(18) . . ? C36 C37 S35 116.5(2) . . ? C36 C37 S37 129.5(2) . . ? S35 C37 S37 113.93(18) . . ? C39 C38 S36 113.4(3) . . ? C38 C39 S37 115.8(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.702 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.137 #===END data_(TBA)ET[Mo3S4Se3Br6] _database_code_depnum_ccdc_archive 'CCDC 639725' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 Br6 Mo3 N S12 Se3' _chemical_formula_weight 1759.50 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _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 12.903(7) _cell_length_b 13.733(8) _cell_length_c 17.658(11) _cell_angle_alpha 92.982(15) _cell_angle_beta 109.882(14) _cell_angle_gamma 117.707(13) _cell_volume 2521(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1674 _exptl_absorpt_coefficient_mu 8.177 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _Ratio_of_minimum_to_maximum_apparent_transmission 0.695309 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11769 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.2223 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8552 _reflns_number_gt 3895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0886P)^2^+0.0000P] 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 8552 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1883 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2360 _refine_ls_wR_factor_gt 0.1686 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Mo1 Mo 0.52572(16) 0.96077(15) 0.25929(12) 0.0257(5) Uani 1 1 d . . . Mo2 Mo 0.33921(17) 0.75429(15) 0.26637(12) 0.0258(5) Uani 1 1 d . . . Mo3 Mo 0.34687(16) 0.95410(15) 0.31680(11) 0.0242(5) Uani 1 1 d . . . Br1 Br 0.5223(3) 1.0016(2) 0.11607(16) 0.0542(8) Uani 1 1 d . . . Br2 Br 0.7781(2) 1.0817(2) 0.30428(16) 0.0417(6) Uani 1 1 d . . . Br3 Br 0.1605(3) 0.5944(2) 0.13013(17) 0.0552(7) Uani 1 1 d . . . Br4 Br 0.3222(2) 0.57638(19) 0.32620(16) 0.0430(6) Uani 1 1 d . . . Br5 Br 0.1736(2) 1.0050(2) 0.23717(16) 0.0445(7) Uani 1 1 d . . . Br6 Br 0.3484(2) 1.0594(2) 0.45011(15) 0.0428(6) Uani 1 1 d . . . S1 S 0.3017(5) 0.8702(4) 0.1812(3) 0.0301(13) Uani 1 1 d . . . S2 S 0.5687(5) 0.8378(5) 0.3400(4) 0.0337(14) Uani 1 1 d . . . S3 S 0.3566(5) 0.8234(5) 0.4010(3) 0.0299(13) Uani 1 1 d . . . S4 S 0.5762(5) 1.0609(5) 0.3946(4) 0.0324(14) Uani 1 1 d . . . Se1 Se 0.5044(2) 0.7679(2) 0.20818(15) 0.0387(6) Uani 1 1 d . . . Se2 Se 0.1624(2) 0.75355(19) 0.30633(15) 0.0356(6) Uani 1 1 d . . . Se3 Se 0.5180(2) 1.14212(19) 0.29985(16) 0.0387(6) Uani 1 1 d . . . S10 S 1.0127(5) 0.3989(5) 0.3720(4) 0.0326(14) Uani 1 1 d . . . S11 S 1.2368(5) 0.5743(5) 0.5173(4) 0.0335(14) Uani 1 1 d . . . S12 S 0.8887(5) 0.5601(5) 0.3517(4) 0.0347(14) Uani 1 1 d . . . S13 S 1.1120(5) 0.7288(5) 0.5003(4) 0.0348(14) Uani 1 1 d . . . S14 S 0.7717(6) 0.7063(6) 0.3177(5) 0.060(2) Uani 1 1 d . . . S15 S 1.3790(6) 0.4558(5) 0.5496(4) 0.0443(16) Uani 1 1 d . . . S16 S 1.1162(5) 0.2492(5) 0.3671(4) 0.0398(15) Uani 1 1 d . . . S17 S 1.0309(7) 0.9033(6) 0.4791(4) 0.0535(19) Uani 1 1 d . . . C1 C 1.0330(18) 0.5966(16) 0.4307(12) 0.024(5) Uiso 1 1 d . . . C2 C 1.0878(17) 0.5294(15) 0.4399(11) 0.017(4) Uiso 1 1 d . . . C3 C 1.1352(19) 0.3714(17) 0.4175(13) 0.029(5) Uiso 1 1 d . . . C4 C 1.2395(19) 0.4565(17) 0.4885(13) 0.031(5) Uiso 1 1 d . . . C5 C 0.8926(19) 0.6867(17) 0.3801(13) 0.031(5) Uiso 1 1 d . . . C6 C 0.998(2) 0.7666(18) 0.4500(14) 0.034(5) Uiso 1 1 d . . . C7 C 1.287(2) 0.288(2) 0.4076(15) 0.052(7) Uiso 1 1 d . . . H7A H 1.2923 0.2238 0.3866 0.063 Uiso 1 1 calc R . . H7B H 1.3347 0.3513 0.3877 0.063 Uiso 1 1 calc R . . C8 C 1.348(2) 0.3185(19) 0.5007(14) 0.044(6) Uiso 1 1 d . . . H8A H 1.4282 0.3196 0.5191 0.053 Uiso 1 1 calc R . . H8B H 1.2916 0.2598 0.5199 0.053 Uiso 1 1 calc R . . C9 C 0.862(3) 0.851(2) 0.313(2) 0.085(10) Uiso 1 1 d . . . H9A H 0.8672 0.8481 0.2590 0.102 Uiso 1 1 calc R . . H9B H 0.8131 0.8865 0.3133 0.102 Uiso 1 1 calc R . . C10 C 0.9943(9) 0.9267(8) 0.3767(6) 0.057(7) Uiso 1 1 d . . . H10A H 1.0123 1.0042 0.3815 0.068 Uiso 1 1 calc R . . H10B H 1.0531 0.9210 0.3567 0.068 Uiso 1 1 calc R . . N1 N 0.0045(9) 0.2201(8) 0.0821(6) 0.026(10) Uiso 0.50 1 d PR A 1 C100 C 0.1412(9) 0.3086(8) 0.1524(6) 0.070(17) Uiso 0.50 1 d PR A 1 C101 C 0.2397(9) 0.2783(8) 0.1613(6) 0.058(15) Uiso 0.50 1 d PR A 1 C102 C 0.3469(9) 0.3380(8) 0.2497(6) 0.36(10) Uiso 0.50 1 d PR A 1 C103 C 0.4830(9) 0.3907(8) 0.2503(6) 0.28(9) Uiso 0.50 1 d PR A 1 C104 C -0.0556(9) 0.1061(8) 0.1098(6) 0.09(2) Uiso 0.50 1 d PR A 1 C105 C -0.1880(9) 0.0214(8) 0.0521(6) 0.047(13) Uiso 0.50 1 d PR A 1 C106 C -0.2439(9) -0.0773(8) 0.0915(6) 0.09(2) Uiso 0.50 1 d PR A 1 C107 C -0.3528(9) -0.1963(8) 0.0543(6) 0.044(12) Uiso 0.50 1 d PR A 1 C108 C -0.0858(9) 0.2713(8) 0.0690(6) 0.067(17) Uiso 0.50 1 d PR A 1 C109 C -0.1040(9) 0.2960(8) 0.1439(6) 0.10(2) Uiso 0.50 1 d PR A 1 C110 C -0.2319(9) 0.2940(8) 0.1178(6) 0.12(3) Uiso 0.50 1 d PR A 1 C111 C -0.2845(9) 0.3399(8) 0.1623(6) 0.12(3) Uiso 0.50 1 d PR A 1 C112 C 0.0060(9) 0.1961(8) -0.0056(6) 0.059(15) Uiso 0.50 1 d PR A 1 C113 C 0.0555(9) 0.2968(8) -0.0377(6) 0.14(3) Uiso 0.50 1 d PR A 1 C114 C 0.0918(9) 0.2702(8) -0.1078(6) 0.13(3) Uiso 0.50 1 d PR A 1 C115 C 0.1414(9) 0.3764(8) -0.1439(6) 0.10(2) Uiso 0.50 1 d PR A 1 N2 N 0.0114(9) 0.2259(8) 0.0676(6) 0.11(3) Uiso 0.50 1 d PR B 2 C200 C 0.1335(9) 0.2186(8) 0.1183(6) 0.15(3) Uiso 0.50 1 d PR B 2 C201 C 0.2515(9) 0.3303(8) 0.1623(6) 0.08(2) Uiso 0.50 1 d PR B 2 C202 C 0.3583(9) 0.3180(8) 0.2016(6) 0.043(12) Uiso 0.50 1 d PR B 2 C203 C 0.5084(9) 0.3827(8) 0.2425(6) 0.14(4) Uiso 0.50 1 d PR B 2 C204 C -0.1022(9) 0.1032(8) 0.0123(6) 0.13(3) Uiso 0.50 1 d PR B 2 C205 C -0.1393(9) 0.0194(8) 0.0609(6) 0.11(3) Uiso 0.50 1 d PR B 2 C206 C -0.2799(9) -0.0764(8) 0.0103(6) 0.11(3) Uiso 0.50 1 d PR B 2 C207 C -0.3762(9) -0.1838(8) 0.0158(6) 0.077(18) Uiso 0.50 1 d PR B 2 C208 C -0.0305(9) 0.2695(8) 0.1299(6) 0.071(17) Uiso 0.50 1 d PR B 2 C209 C -0.1505(9) 0.2696(8) 0.0891(6) 0.062(16) Uiso 0.50 1 d PR B 2 C210 C -0.1933(9) 0.2950(8) 0.1554(6) 0.31(9) Uiso 0.50 1 d PR B 2 C211 C -0.3156(9) 0.2917(8) 0.1480(6) 0.12(3) Uiso 0.50 1 d PR B 2 C212 C 0.0312(9) 0.3015(8) 0.0039(6) 0.11(2) Uiso 0.50 1 d PR B 2 C213 C 0.0652(9) 0.2642(8) -0.0586(6) 0.14(3) Uiso 0.50 1 d PR B 2 C214 C 0.1226(9) 0.3630(8) -0.0981(6) 0.10(2) Uiso 0.50 1 d PR B 2 C215 C 0.2110(9) 0.3963(8) -0.1404(6) 0.13(3) Uiso 0.50 1 d PR B 2 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 0.0251(10) 0.0227(11) 0.0314(12) 0.0110(9) 0.0141(9) 0.0117(9) Mo2 0.0268(10) 0.0215(11) 0.0292(12) 0.0089(9) 0.0127(9) 0.0115(9) Mo3 0.0235(10) 0.0220(11) 0.0279(12) 0.0076(9) 0.0104(9) 0.0123(9) Br1 0.0557(16) 0.071(2) 0.0423(17) 0.0310(15) 0.0294(14) 0.0293(15) Br2 0.0307(13) 0.0384(15) 0.0589(18) 0.0184(13) 0.0242(13) 0.0154(11) Br3 0.0594(17) 0.0307(15) 0.0480(18) 0.0004(13) 0.0049(14) 0.0155(13) Br4 0.0520(15) 0.0280(14) 0.0471(17) 0.0170(12) 0.0216(13) 0.0177(12) Br5 0.0431(14) 0.0518(17) 0.0471(16) 0.0193(13) 0.0145(13) 0.0329(13) Br6 0.0494(15) 0.0488(16) 0.0418(16) 0.0076(13) 0.0169(13) 0.0353(13) S1 0.038(3) 0.025(3) 0.029(3) 0.009(3) 0.013(3) 0.017(3) S2 0.032(3) 0.038(4) 0.033(4) 0.012(3) 0.015(3) 0.018(3) S3 0.032(3) 0.030(3) 0.025(3) 0.005(3) 0.013(3) 0.013(3) S4 0.028(3) 0.030(3) 0.033(4) 0.004(3) 0.012(3) 0.011(3) Se1 0.0457(14) 0.0402(15) 0.0408(16) 0.0112(12) 0.0251(13) 0.0248(12) Se2 0.0267(12) 0.0370(14) 0.0446(16) 0.0174(12) 0.0198(12) 0.0133(11) Se3 0.0399(14) 0.0233(13) 0.0480(17) 0.0128(12) 0.0156(13) 0.0139(11) S10 0.032(3) 0.028(3) 0.035(4) 0.004(3) 0.012(3) 0.015(3) S11 0.028(3) 0.027(3) 0.037(4) 0.002(3) 0.011(3) 0.010(3) S12 0.036(3) 0.023(3) 0.038(4) 0.005(3) 0.010(3) 0.014(3) S13 0.032(3) 0.027(3) 0.039(4) 0.000(3) 0.018(3) 0.009(3) S14 0.041(4) 0.060(5) 0.080(6) 0.026(4) 0.022(4) 0.028(4) S15 0.035(3) 0.045(4) 0.053(4) 0.013(3) 0.012(3) 0.024(3) S16 0.037(3) 0.033(4) 0.045(4) 0.004(3) 0.016(3) 0.016(3) S17 0.088(5) 0.044(4) 0.057(5) 0.019(4) 0.043(4) 0.046(4) _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 S1 2.360(6) . ? Mo1 S2 2.404(6) . ? Mo1 S4 2.407(6) . ? Mo1 Br1 2.609(3) . ? Mo1 Se1 2.610(3) . ? Mo1 Se3 2.611(3) . ? Mo1 Br2 2.659(3) . ? Mo1 Mo2 2.783(3) . ? Mo1 Mo3 2.788(3) . ? Mo2 S1 2.346(6) . ? Mo2 S3 2.409(6) . ? Mo2 S2 2.418(6) . ? Mo2 Se1 2.602(3) . ? Mo2 Se2 2.603(3) . ? Mo2 Br3 2.626(3) . ? Mo2 Br4 2.657(3) . ? Mo2 Mo3 2.787(3) . ? Mo3 S1 2.354(6) . ? Mo3 S4 2.405(6) . ? Mo3 S3 2.410(6) . ? Mo3 Se2 2.615(3) . ? Mo3 Se3 2.619(3) . ? Mo3 Br5 2.623(3) . ? Mo3 Br6 2.687(3) . ? S2 Se1 2.178(6) . ? S3 Se2 2.177(6) . ? S4 Se3 2.174(6) . ? S10 C2 1.720(19) . ? S10 C3 1.74(2) . ? S11 C4 1.69(2) . ? S11 C2 1.722(19) . ? S12 C1 1.72(2) . ? S12 C5 1.76(2) . ? S13 C1 1.74(2) . ? S13 C6 1.75(2) . ? S14 C5 1.72(2) . ? S14 C9 1.80(3) . ? S15 C4 1.76(2) . ? S15 C8 1.83(2) . ? S16 C3 1.73(2) . ? S16 C7 1.86(2) . ? S17 C6 1.73(2) . ? S17 C10 1.793(12) . ? C1 C2 1.39(2) . ? C3 C4 1.41(3) . ? C5 C6 1.38(3) . ? C7 C8 1.50(3) . ? C9 C10 1.48(3) . ? N1 C112 1.5750 . ? N1 C100 1.5778 . ? N1 C108 1.5810 . ? N1 C104 1.5819 . ? C100 C101 1.4745 . ? C101 C102 1.5379 . ? C102 C103 1.5527 . ? C104 C105 1.4681 . ? C105 C106 1.5406 . ? C106 C107 1.4842 . ? C108 C109 1.4697 . ? C109 C110 1.5414 . ? C110 C111 1.4782 . ? C112 C113 1.4656 . ? C113 C114 1.5464 . ? C114 C115 1.5640 . ? N2 C212 1.5752 . ? N2 C200 1.5782 . ? N2 C204 1.5812 . ? N2 C208 1.5820 . ? C200 C201 1.4749 . ? C201 C202 1.4086 . ? C202 C203 1.5637 . ? C204 C205 1.4701 . ? C205 C206 1.5417 . ? C206 C207 1.4558 . ? C208 C209 1.4685 . ? C209 C210 1.5408 . ? C210 C211 1.5179 . ? C212 C213 1.4661 . ? C213 C214 1.5468 . ? C214 C215 1.4830 . ? 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 S2 108.35(19) . . ? S1 Mo1 S4 108.01(19) . . ? S2 Mo1 S4 80.6(2) . . ? S1 Mo1 Br1 80.50(15) . . ? S2 Mo1 Br1 136.14(16) . . ? S4 Mo1 Br1 138.96(17) . . ? S1 Mo1 Se1 86.74(15) . . ? S2 Mo1 Se1 51.30(15) . . ? S4 Mo1 Se1 131.75(16) . . ? Br1 Mo1 Se1 87.85(10) . . ? S1 Mo1 Se3 86.51(15) . . ? S2 Mo1 Se3 131.64(17) . . ? S4 Mo1 Se3 51.16(15) . . ? Br1 Mo1 Se3 90.86(10) . . ? Se1 Mo1 Se3 173.25(11) . . ? S1 Mo1 Br2 162.36(16) . . ? S2 Mo1 Br2 85.69(15) . . ? S4 Mo1 Br2 84.32(15) . . ? Br1 Mo1 Br2 81.95(9) . . ? Se1 Mo1 Br2 94.37(9) . . ? Se3 Mo1 Br2 92.01(10) . . ? S1 Mo1 Mo2 53.51(14) . . ? S2 Mo1 Mo2 54.98(14) . . ? S4 Mo1 Mo2 94.27(15) . . ? Br1 Mo1 Mo2 120.41(10) . . ? Se1 Mo1 Mo2 57.60(8) . . ? Se3 Mo1 Mo2 117.88(10) . . ? Br2 Mo1 Mo2 140.12(9) . . ? S1 Mo1 Mo3 53.63(14) . . ? S2 Mo1 Mo3 93.79(14) . . ? S4 Mo1 Mo3 54.57(14) . . ? Br1 Mo1 Mo3 122.70(10) . . ? Se1 Mo1 Mo3 117.59(9) . . ? Se3 Mo1 Mo3 57.93(7) . . ? Br2 Mo1 Mo3 138.20(10) . . ? Mo2 Mo1 Mo3 60.04(7) . . ? S1 Mo2 S3 107.9(2) . . ? S1 Mo2 S2 108.4(2) . . ? S3 Mo2 S2 82.91(19) . . ? S1 Mo2 Se1 87.21(15) . . ? S3 Mo2 Se1 134.11(16) . . ? S2 Mo2 Se1 51.27(15) . . ? S1 Mo2 Se2 84.33(15) . . ? S3 Mo2 Se2 51.31(14) . . ? S2 Mo2 Se2 133.89(17) . . ? Se1 Mo2 Se2 171.32(11) . . ? S1 Mo2 Br3 81.56(16) . . ? S3 Mo2 Br3 137.09(16) . . ? S2 Mo2 Br3 135.01(17) . . ? Se1 Mo2 Br3 86.93(11) . . ? Se2 Mo2 Br3 89.89(11) . . ? S1 Mo2 Br4 163.53(17) . . ? S3 Mo2 Br4 82.44(15) . . ? S2 Mo2 Br4 85.18(15) . . ? Se1 Mo2 Br4 94.60(9) . . ? Se2 Mo2 Br4 92.96(9) . . ? Br3 Mo2 Br4 82.19(10) . . ? S1 Mo2 Mo1 53.99(15) . . ? S3 Mo2 Mo1 96.03(15) . . ? S2 Mo2 Mo1 54.53(14) . . ? Se1 Mo2 Mo1 57.86(8) . . ? Se2 Mo2 Mo1 117.69(10) . . ? Br3 Mo2 Mo1 121.02(10) . . ? Br4 Mo2 Mo1 139.37(10) . . ? S1 Mo2 Mo3 53.76(15) . . ? S3 Mo2 Mo3 54.68(14) . . ? S2 Mo2 Mo3 93.52(16) . . ? Se1 Mo2 Mo3 117.88(9) . . ? Se2 Mo2 Mo3 57.92(7) . . ? Br3 Mo2 Mo3 124.32(10) . . ? Br4 Mo2 Mo3 136.81(10) . . ? Mo1 Mo2 Mo3 60.07(7) . . ? S1 Mo3 S4 108.3(2) . . ? S1 Mo3 S3 107.67(19) . . ? S4 Mo3 S3 83.80(19) . . ? S1 Mo3 Se2 83.92(15) . . ? S4 Mo3 Se2 134.59(16) . . ? S3 Mo3 Se2 51.16(15) . . ? S1 Mo3 Se3 86.46(15) . . ? S4 Mo3 Se3 51.07(15) . . ? S3 Mo3 Se3 134.72(16) . . ? Se2 Mo3 Se3 170.18(11) . . ? S1 Mo3 Br5 82.92(15) . . ? S4 Mo3 Br5 134.77(17) . . ? S3 Mo3 Br5 135.74(15) . . ? Se2 Mo3 Br5 89.22(10) . . ? Se3 Mo3 Br5 87.64(10) . . ? S1 Mo3 Br6 164.95(16) . . ? S4 Mo3 Br6 83.34(15) . . ? S3 Mo3 Br6 82.58(15) . . ? Se2 Mo3 Br6 94.75(10) . . ? Se3 Mo3 Br6 94.03(10) . . ? Br5 Mo3 Br6 82.08(10) . . ? S1 Mo3 Mo2 53.50(14) . . ? S4 Mo3 Mo2 94.20(15) . . ? S3 Mo3 Mo2 54.66(14) . . ? Se2 Mo3 Mo2 57.52(8) . . ? Se3 Mo3 Mo2 117.45(10) . . ? Br5 Mo3 Mo2 124.66(10) . . ? Br6 Mo3 Mo2 137.11(9) . . ? S1 Mo3 Mo1 53.85(14) . . ? S4 Mo3 Mo1 54.62(15) . . ? S3 Mo3 Mo1 95.89(14) . . ? Se2 Mo3 Mo1 117.11(9) . . ? Se3 Mo3 Mo1 57.65(8) . . ? Br5 Mo3 Mo1 122.66(10) . . ? Br6 Mo3 Mo1 137.69(10) . . ? Mo2 Mo3 Mo1 59.89(6) . . ? Mo2 S1 Mo3 72.75(17) . . ? Mo2 S1 Mo1 72.50(17) . . ? Mo3 S1 Mo1 72.52(17) . . ? Se1 S2 Mo1 69.23(18) . . ? Se1 S2 Mo2 68.75(18) . . ? Mo1 S2 Mo2 70.50(16) . . ? Se2 S3 Mo3 69.29(17) . . ? Se2 S3 Mo2 68.94(17) . . ? Mo3 S3 Mo2 70.65(16) . . ? Se3 S4 Mo3 69.56(18) . . ? Se3 S4 Mo1 69.29(18) . . ? Mo3 S4 Mo1 70.81(17) . . ? S2 Se1 Mo2 59.98(16) . . ? S2 Se1 Mo1 59.48(16) . . ? Mo2 Se1 Mo1 64.54(7) . . ? S3 Se2 Mo2 59.74(16) . . ? S3 Se2 Mo3 59.55(16) . . ? Mo2 Se2 Mo3 64.56(8) . . ? S4 Se3 Mo1 59.55(16) . . ? S4 Se3 Mo3 59.37(16) . . ? Mo1 Se3 Mo3 64.41(8) . . ? C2 S10 C3 95.6(10) . . ? C4 S11 C2 95.1(10) . . ? C1 S12 C5 96.3(10) . . ? C1 S13 C6 96.0(10) . . ? C5 S14 C9 101.2(12) . . ? C4 S15 C8 102.9(11) . . ? C3 S16 C7 99.6(10) . . ? C6 S17 C10 96.2(8) . . ? C2 C1 S12 124.2(15) . . ? C2 C1 S13 120.4(15) . . ? S12 C1 S13 115.4(11) . . ? C1 C2 S10 121.5(15) . . ? C1 C2 S11 121.9(15) . . ? S10 C2 S11 116.6(10) . . ? C4 C3 S16 129.5(16) . . ? C4 C3 S10 114.2(15) . . ? S16 C3 S10 116.2(12) . . ? C3 C4 S11 118.4(16) . . ? C3 C4 S15 126.2(16) . . ? S11 C4 S15 115.3(12) . . ? C6 C5 S14 124.8(17) . . ? C6 C5 S12 116.1(16) . . ? S14 C5 S12 119.0(13) . . ? C5 C6 S17 122.8(17) . . ? C5 C6 S13 116.1(16) . . ? S17 C6 S13 120.5(13) . . ? C8 C7 S16 111.1(16) . . ? C7 C8 S15 114.6(17) . . ? C10 C9 S14 119.6(19) . . ? C9 C10 S17 117.7(14) . . ? C112 N1 C100 113.4 . . ? C112 N1 C108 104.9 . . ? C100 N1 C108 108.9 . . ? C112 N1 C104 110.9 . . ? C100 N1 C104 109.6 . . ? C108 N1 C104 108.9 . . ? C101 C100 N1 113.9 . . ? C100 C101 C102 108.7 . . ? C101 C102 C103 112.4 . . ? C105 C104 N1 114.0 . . ? C104 C105 C106 109.6 . . ? C107 C106 C105 131.8 . . ? C109 C108 N1 113.5 . . ? C108 C109 C110 109.1 . . ? C111 C110 C109 133.4 . . ? C113 C112 N1 114.6 . . ? C112 C113 C114 109.0 . . ? C113 C114 C115 109.3 . . ? C212 N2 C200 113.4 . . ? C212 N2 C204 104.9 . . ? C200 N2 C204 108.9 . . ? C212 N2 C208 110.9 . . ? C200 N2 C208 109.6 . . ? C204 N2 C208 108.9 . . ? C201 C200 N2 113.9 . . ? C202 C201 C200 111.0 . . ? C201 C202 C203 144.0 . . ? C205 C204 N2 113.5 . . ? C204 C205 C206 109.1 . . ? C207 C206 C205 140.2 . . ? C209 C208 N2 114.0 . . ? C208 C209 C210 109.6 . . ? C211 C210 C209 131.7 . . ? C213 C212 N2 114.6 . . ? C212 C213 C214 109.0 . . ? C215 C214 C213 135.6 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.474 _refine_diff_density_min -1.301 _refine_diff_density_rms 0.333 #===END data_(ET)2[Mo3S7Cl6]2CH3CN _database_code_depnum_ccdc_archive 'CCDC 639726' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H11 Cl6 Mo3 N S15' _chemical_formula_weight 1150.64 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' _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 10.0467(10) _cell_length_b 11.3217(12) _cell_length_c 14.8607(15) _cell_angle_alpha 105.133(2) _cell_angle_beta 92.035(2) _cell_angle_gamma 99.297(3) _cell_volume 1604.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13381 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 2.643 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _Ratio_of_minimum_to_maximum_apparent_transmision 0.906055 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 9263 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.1283 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5652 _reflns_number_gt 3432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0325P)^2^+0.0000P] 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 5652 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.000 _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 -0.13239(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_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 0.0148(4) 0.0240(5) 0.0201(5) 0.0074(4) 0.0013(3) 0.0036(4) Mo2 0.0165(4) 0.0302(6) 0.0273(5) 0.0140(4) 0.0013(4) 0.0050(4) Mo3 0.0155(4) 0.0251(6) 0.0223(5) 0.0087(4) 0.0018(4) 0.0026(4) S1 0.0189(13) 0.0279(16) 0.0276(14) 0.0040(12) -0.0030(11) 0.0004(11) S2 0.0214(13) 0.0275(16) 0.0350(15) 0.0108(13) 0.0054(11) 0.0034(11) S3 0.0300(14) 0.0415(18) 0.0284(15) 0.0188(13) 0.0058(12) 0.0061(13) S4 0.0208(13) 0.0307(17) 0.0253(14) 0.0073(12) 0.0012(11) 0.0042(11) S5 0.0259(14) 0.0337(17) 0.0291(14) 0.0131(13) 0.0001(11) 0.0108(12) S6 0.0212(13) 0.0273(16) 0.0339(15) 0.0105(13) 0.0066(11) 0.0083(12) S7 0.0169(13) 0.0427(19) 0.0400(16) 0.0164(14) 0.0041(12) 0.0064(12) Cl1 0.0374(15) 0.0313(17) 0.0320(15) 0.0049(12) 0.0105(12) 0.0104(12) Cl2 0.0172(12) 0.0453(18) 0.0370(15) 0.0091(13) 0.0022(11) 0.0019(12) Cl3 0.0380(16) 0.076(3) 0.0399(17) 0.0184(16) -0.0149(13) 0.0103(16) Cl4 0.0414(17) 0.057(2) 0.061(2) 0.0332(17) 0.0114(15) 0.0229(15) Cl5 0.0383(15) 0.0335(17) 0.0419(16) 0.0192(14) -0.0054(13) -0.0056(13) Cl6 0.0292(14) 0.0379(17) 0.0323(15) 0.0123(13) 0.0059(12) 0.0028(12) S10 0.0428(17) 0.0313(17) 0.0318(15) 0.0115(13) 0.0149(13) 0.0057(13) S11 0.0368(16) 0.0223(16) 0.0320(15) 0.0036(12) 0.0117(12) -0.0010(12) S12 0.106(3) 0.038(2) 0.0404(19) 0.0072(16) 0.0318(19) 0.024(2) S13 0.0500(18) 0.0232(17) 0.0480(19) 0.0016(14) 0.0121(15) -0.0020(14) C10 0.012(5) 0.017(6) 0.043(6) 0.008(5) 0.002(4) 0.010(4) C11 0.037(6) 0.023(6) 0.032(6) 0.005(5) 0.002(5) 0.004(5) C12 0.022(5) 0.022(6) 0.035(6) 0.009(5) 0.003(5) 0.003(4) C13 0.074(9) 0.038(8) 0.046(7) 0.009(6) 0.018(7) 0.035(7) C14 0.049(7) 0.030(7) 0.039(7) -0.007(6) -0.006(6) 0.013(6) S20 0.0335(15) 0.0241(16) 0.0319(15) 0.0020(12) 0.0049(12) 0.0004(12) S21 0.0236(14) 0.0279(16) 0.0308(15) 0.0031(12) 0.0028(11) 0.0042(12) S22 0.0380(17) 0.0362(19) 0.066(2) 0.0063(16) 0.0292(16) 0.0096(14) S23 0.0231(14) 0.0274(16) 0.0367(16) -0.0033(13) 0.0028(12) 0.0018(12) C20 0.020(5) 0.025(6) 0.031(6) 0.009(5) 0.006(5) 0.001(4) C21 0.011(5) 0.019(6) 0.023(5) 0.001(4) -0.001(4) -0.002(4) C22 0.026(5) 0.022(6) 0.036(6) 0.015(5) 0.010(5) 0.002(5) C23 0.029(7) 0.076(11) 0.062(9) -0.015(8) 0.019(6) -0.027(7) C24 0.048(8) 0.057(10) 0.063(9) 0.023(8) 0.018(7) -0.002(7) C100 0.113(12) 0.067(11) 0.042(8) 0.018(8) -0.030(8) -0.018(9) C101 0.078(10) 0.062(11) 0.052(9) 0.023(8) 0.010(8) -0.001(8) N1 0.160(14) 0.149(16) 0.057(9) 0.046(10) -0.034(9) -0.032(11) _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 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) . ? 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) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.789 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.179 #===END data_(ET)8(Mo3S7Cl6)2ClCH3CN _database_code_depnum_ccdc_archive 'CCDC 639727' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H35 Cl6.50 Mo3 N S39' _chemical_formula_weight 2322.30 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' _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 11.8603(9) _cell_length_b 17.3577(13) _cell_length_c 20.8821(15) _cell_angle_alpha 69.390(2) _cell_angle_beta 88.139(2) _cell_angle_gamma 73.734(2) _cell_volume 3852.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2309 _exptl_absorpt_coefficient_mu 1.800 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _Ratio_of_minimum_to_maximum_apparent_transmission 0.928086 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31354 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.1687 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 30.00 _reflns_number_total 21770 _reflns_number_gt 10055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0386P)^2^+3.9911P] 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 21770 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1759 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1124 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.000 _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 -0.09883(5) 0.25797(4) 0.49127(3) 0.02299(14) Uani 1 1 d . . . Mo2 Mo 0.13817(5) 0.18392(4) 0.52983(3) 0.02737(15) Uani 1 1 d . . . Mo3 Mo 0.05759(5) 0.23999(4) 0.39376(3) 0.02467(15) Uani 1 1 d . . . S1 S 0.04965(16) 0.32741(12) 0.45944(9) 0.0297(4) Uani 1 1 d . . . S2 S -0.10558(16) 0.18231(12) 0.41573(9) 0.0308(4) Uani 1 1 d . . . S3 S -0.15550(16) 0.31206(13) 0.36657(9) 0.0326(4) Uani 1 1 d . . . S4 S -0.01342(17) 0.11768(12) 0.57364(9) 0.0339(4) Uani 1 1 d . . . S5 S -0.01402(17) 0.21228(13) 0.61001(9) 0.0373(5) Uani 1 1 d . . . S6 S 0.17046(17) 0.09673(12) 0.46063(9) 0.0347(5) Uani 1 1 d . . . S7 S 0.26937(17) 0.18034(14) 0.43423(11) 0.0426(5) Uani 1 1 d . . . Cl1 Cl -0.28906(16) 0.22493(13) 0.52374(9) 0.0402(5) Uani 1 1 d . . . Cl2 Cl -0.21050(15) 0.39733(12) 0.50030(9) 0.0332(4) Uani 1 1 d . . . Cl3 Cl 0.26486(18) 0.24848(15) 0.57230(12) 0.0563(6) Uani 1 1 d . . . Cl4 Cl 0.26022(19) 0.05128(14) 0.62183(11) 0.0541(6) Uani 1 1 d . . . Cl5 Cl 0.07741(18) 0.18074(13) 0.29887(9) 0.0429(5) Uani 1 1 d . . . Cl6 Cl 0.09019(18) 0.36421(13) 0.30080(9) 0.0444(5) Uani 1 1 d . . . Cl7 Cl 0.0000 0.0000 0.5000 0.0630(9) Uani 1 2 d S . . S10 S 0.12948(19) 0.28208(15) 0.99833(10) 0.0461(6) Uani 1 1 d . . . S11 S 0.33351(18) 0.34461(15) 0.95378(10) 0.0427(5) Uani 1 1 d . . . S12 S 0.18537(19) 0.23392(17) 1.14605(10) 0.0553(7) Uani 1 1 d . . . S13 S 0.4255(2) 0.3153(2) 1.09085(11) 0.0700(8) Uani 1 1 d . . . S14 S 0.03663(19) 0.33907(15) 0.83980(10) 0.0448(5) Uani 1 1 d . . . S15 S 0.24315(18) 0.39829(15) 0.79608(9) 0.0426(5) Uani 1 1 d . . . S16 S -0.06333(18) 0.37994(15) 0.70128(10) 0.0466(6) Uani 1 1 d . . . S17 S 0.17905(19) 0.46020(15) 0.64884(10) 0.0470(6) Uani 1 1 d . . . C10 C 0.1669(6) 0.3525(5) 0.8638(3) 0.0331(17) Uani 1 1 d . . . C11 C 0.2063(6) 0.3277(5) 0.9307(3) 0.0342(18) Uani 1 1 d . . . C12 C 0.2254(6) 0.2774(5) 1.0622(4) 0.0361(19) Uani 1 1 d . . . C13 C 0.3179(6) 0.3073(5) 1.0416(4) 0.0384(19) Uani 1 1 d . . . C14 C 0.2851(12) 0.2574(11) 1.1907(5) 0.145(7) Uani 1 1 d . . . H14A H 0.2388 0.3059 1.2021 0.173 Uiso 1 1 calc R . . H14B H 0.3057 0.2092 1.2339 0.173 Uiso 1 1 calc R . . C15 C 0.3820(11) 0.2744(10) 1.1728(5) 0.122(6) Uani 1 1 d . . . H15A H 0.4430 0.2212 1.1955 0.146 Uiso 1 1 calc R . . H15B H 0.3891 0.3136 1.1949 0.146 Uiso 1 1 calc R . . C16 C 0.0508(6) 0.3804(5) 0.7525(3) 0.0331(17) Uani 1 1 d . . . C17 C 0.1440(6) 0.4092(5) 0.7317(3) 0.0297(16) Uani 1 1 d . . . C18 C -0.0453(7) 0.4534(6) 0.6199(4) 0.051(2) Uani 1 1 d . . . H18A H -0.0947 0.4501 0.5855 0.061 Uiso 1 1 calc R . . H18B H -0.0729 0.5111 0.6207 0.061 Uiso 1 1 calc R . . C19 C 0.0788(7) 0.4384(6) 0.5988(4) 0.048(2) Uani 1 1 d . . . H19A H 0.0777 0.4744 0.5511 0.058 Uiso 1 1 calc R . . H19B H 0.1089 0.3791 0.6020 0.058 Uiso 1 1 calc R . . S20 S 0.63341(19) 0.15910(15) 1.01324(10) 0.0468(6) Uani 1 1 d . . . S21 S 0.85064(18) 0.20570(15) 0.96996(10) 0.0445(5) Uani 1 1 d . . . S22 S 0.6834(2) 0.11860(17) 1.16020(11) 0.0610(7) Uani 1 1 d . . . S23 S 0.9419(2) 0.17581(16) 1.10851(11) 0.0515(6) Uani 1 1 d . . . S24 S 0.54535(18) 0.21380(14) 0.85275(10) 0.0430(5) Uani 1 1 d . . . S25 S 0.76119(17) 0.26310(15) 0.81112(10) 0.0427(5) Uani 1 1 d . . . S26 S 0.43999(18) 0.26949(17) 0.71221(10) 0.0526(6) Uani 1 1 d . . . S27 S 0.69736(18) 0.33111(15) 0.66320(10) 0.0451(6) Uani 1 1 d . . . C20 C 0.6785(6) 0.2230(5) 0.8783(4) 0.0369(18) Uani 1 1 d . . . C21 C 0.7151(7) 0.1996(5) 0.9457(4) 0.0365(18) Uani 1 1 d . . . C22 C 0.7283(7) 0.1551(5) 1.0772(4) 0.040(2) Uani 1 1 d . . . C23 C 0.8265(7) 0.1761(5) 1.0570(4) 0.0386(19) Uani 1 1 d . . . C24 C 0.7943(8) 0.1300(6) 1.2117(4) 0.064(3) Uani 1 1 d . . . H24A H 0.7737 0.1892 1.2091 0.077 Uiso 1 1 calc R . . H24B H 0.7925 0.0944 1.2592 0.077 Uiso 1 1 calc R . . C25 C 0.9171(8) 0.1060(6) 1.1906(4) 0.051(2) Uani 1 1 d . . . H25A H 0.9356 0.0481 1.1901 0.061 Uiso 1 1 calc R . . H25B H 0.9710 0.1053 1.2249 0.061 Uiso 1 1 calc R . . C26 C 0.5576(7) 0.2615(5) 0.7649(4) 0.0360(18) Uani 1 1 d . . . C27 C 0.6558(6) 0.2854(5) 0.7453(4) 0.0337(18) Uani 1 1 d . . . C28 C 0.5040(8) 0.2910(7) 0.6307(4) 0.062(3) Uani 1 1 d . . . H28A H 0.5596 0.2380 0.6307 0.075 Uiso 1 1 calc R . . H28B H 0.4419 0.3073 0.5952 0.075 Uiso 1 1 calc R . . C29 C 0.5638(7) 0.3566(6) 0.6122(4) 0.049(2) Uani 1 1 d . . . H29A H 0.5102 0.4086 0.6154 0.059 Uiso 1 1 calc R . . H29B H 0.5821 0.3690 0.5647 0.059 Uiso 1 1 calc R . . S30 S 0.64730(18) 0.91210(15) 1.03201(10) 0.0459(6) Uani 1 1 d . . . S31 S 0.86103(18) 0.96459(15) 0.99576(10) 0.0459(5) Uani 1 1 d . . . S32 S 0.7010(2) 0.84916(19) 1.18016(11) 0.0671(8) Uani 1 1 d . . . S33 S 0.9568(2) 0.91259(17) 1.13665(11) 0.0565(7) Uani 1 1 d . . . S34 S 0.57630(17) 0.96550(15) 0.86908(10) 0.0437(5) Uani 1 1 d . . . S35 S 0.78929(18) 1.01874(15) 0.83702(10) 0.0441(5) Uani 1 1 d . . . S36 S 0.4930(2) 1.01052(19) 0.72586(11) 0.0609(7) Uani 1 1 d . . . S37 S 0.7494(2) 1.07431(17) 0.68797(11) 0.0572(7) Uani 1 1 d . . . C30 C 0.7025(6) 0.9767(5) 0.8996(3) 0.0337(18) Uani 1 1 d . . . C31 C 0.7334(6) 0.9528(5) 0.9682(4) 0.0353(18) Uani 1 1 d . . . C32 C 0.7456(7) 0.8951(5) 1.0995(4) 0.0382(19) Uani 1 1 d . . . C33 C 0.8451(6) 0.9184(5) 1.0822(3) 0.0304(17) Uani 1 1 d . . . C34 C 0.8011(9) 0.8641(9) 1.2328(5) 0.092(4) Uani 1 1 d . . . H34A H 0.7620 0.9173 1.2400 0.110 Uiso 1 1 calc R . . H34B H 0.8094 0.8184 1.2771 0.110 Uiso 1 1 calc R . . C35 C 0.9114(13) 0.8674(10) 1.2163(5) 0.137(7) Uani 1 1 d . . . H35A H 0.9602 0.8082 1.2334 0.164 Uiso 1 1 calc R . . H35B H 0.9353 0.8949 1.2445 0.164 Uiso 1 1 calc R . . C36 C 0.6011(6) 1.0063(5) 0.7825(4) 0.0369(19) Uani 1 1 d . . . C37 C 0.7000(6) 1.0313(5) 0.7681(3) 0.0349(18) Uani 1 1 d . . . C38 C 0.5507(9) 1.0500(7) 0.6447(4) 0.064(3) Uani 1 1 d . . . H38A H 0.5199 1.0291 0.6136 0.076 Uiso 1 1 calc R . . H38B H 0.5195 1.1121 0.6271 0.076 Uiso 1 1 calc R . . C39 C 0.6802(8) 1.0285(6) 0.6415(4) 0.052(2) Uani 1 1 d . . . H39A H 0.6982 1.0487 0.5939 0.063 Uiso 1 1 calc R . . H39B H 0.7131 0.9665 0.6599 0.063 Uiso 1 1 calc R . . S40 S 0.24682(17) 0.48370(14) 0.21638(9) 0.0405(5) Uani 1 1 d . . . S41 S 0.45326(17) 0.54458(14) 0.17715(10) 0.0390(5) Uani 1 1 d . . . S42 S 0.32313(19) 0.39777(15) 0.36411(10) 0.0481(6) Uani 1 1 d . . . S43 S 0.56931(18) 0.47544(15) 0.31454(11) 0.0474(6) Uani 1 1 d . . . S44 S 0.16253(18) 0.54046(15) 0.05808(10) 0.0460(6) Uani 1 1 d . . . S45 S 0.37343(18) 0.59515(15) 0.01723(10) 0.0442(5) Uani 1 1 d . . . S46 S 0.0824(2) 0.56136(17) -0.08040(12) 0.0567(6) Uani 1 1 d . . . S47 S 0.3368(2) 0.62783(16) -0.12900(10) 0.0502(6) Uani 1 1 d . . . C40 C 0.2901(6) 0.5546(5) 0.0832(4) 0.0330(17) Uani 1 1 d . . . C41 C 0.3254(6) 0.5317(5) 0.1502(4) 0.0335(17) Uani 1 1 d . . . C42 C 0.3529(6) 0.4576(5) 0.2823(3) 0.0341(18) Uani 1 1 d . . . C43 C 0.4469(6) 0.4877(5) 0.2631(3) 0.0293(16) Uani 1 1 d . . . C44 C 0.4264(8) 0.4158(7) 0.4152(4) 0.067(3) Uani 1 1 d . . . H44A H 0.3982 0.4747 0.4134 0.080 Uiso 1 1 calc R . . H44B H 0.4275 0.3787 0.4626 0.080 Uiso 1 1 calc R . . C45 C 0.5457(8) 0.4005(6) 0.3943(4) 0.065(3) Uani 1 1 d . . . H45A H 0.5705 0.3436 0.3917 0.078 Uiso 1 1 calc R . . H45B H 0.5964 0.4003 0.4300 0.078 Uiso 1 1 calc R . . C46 C 0.1891(7) 0.5675(5) -0.0282(4) 0.0371(19) Uani 1 1 d . . . C47 C 0.2849(7) 0.5939(5) -0.0475(3) 0.0359(18) Uani 1 1 d . . . C48 C 0.1141(8) 0.6249(7) -0.1624(4) 0.069(3) Uani 1 1 d . . . H48A H 0.0691 0.6180 -0.1969 0.082 Uiso 1 1 calc R . . H48B H 0.0862 0.6847 -0.1666 0.082 Uiso 1 1 calc R . . C49 C 0.2395(9) 0.6062(7) -0.1784(4) 0.069(3) Uani 1 1 d . . . H49A H 0.2433 0.6394 -0.2263 0.082 Uiso 1 1 calc R . . H49B H 0.2680 0.5460 -0.1728 0.082 Uiso 1 1 calc R . . C100 C 0.5989(11) 0.1368(8) 0.4123(6) 0.093(4) Uiso 1 1 d . . . C101 C 0.5948(11) 0.1988(8) 0.3433(7) 0.094(4) Uiso 1 1 d . . . N100 N 0.6017(8) 0.2510(6) 0.2949(5) 0.090(3) Uiso 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 0.0201(3) 0.0307(4) 0.0160(3) -0.0042(3) -0.0005(2) -0.0092(3) Mo2 0.0224(3) 0.0343(4) 0.0249(3) -0.0113(3) -0.0053(2) -0.0057(3) Mo3 0.0227(3) 0.0321(4) 0.0199(3) -0.0069(3) 0.0024(2) -0.0121(3) S1 0.0279(10) 0.0325(11) 0.0319(10) -0.0112(8) 0.0012(8) -0.0139(8) S2 0.0308(10) 0.0414(12) 0.0243(9) -0.0100(8) 0.0008(7) -0.0189(9) S3 0.0273(10) 0.0417(12) 0.0226(9) -0.0042(8) -0.0037(7) -0.0093(9) S4 0.0369(11) 0.0346(12) 0.0244(9) -0.0020(8) -0.0016(8) -0.0117(9) S5 0.0398(11) 0.0471(13) 0.0207(9) -0.0115(9) -0.0046(8) -0.0056(10) S6 0.0372(11) 0.0352(12) 0.0297(10) -0.0117(9) -0.0026(8) -0.0064(9) S7 0.0228(10) 0.0572(15) 0.0510(13) -0.0222(11) 0.0057(9) -0.0132(10) Cl1 0.0317(10) 0.0521(13) 0.0337(10) -0.0067(9) 0.0087(8) -0.0190(9) Cl2 0.0289(9) 0.0386(11) 0.0316(10) -0.0121(8) 0.0044(7) -0.0097(8) Cl3 0.0384(12) 0.0650(16) 0.0774(16) -0.0388(13) -0.0178(11) -0.0132(11) Cl4 0.0481(13) 0.0548(15) 0.0432(12) -0.0105(11) -0.0219(10) 0.0039(11) Cl5 0.0516(12) 0.0550(14) 0.0276(10) -0.0198(9) 0.0073(9) -0.0176(10) Cl6 0.0525(13) 0.0539(13) 0.0294(10) -0.0053(9) 0.0097(9) -0.0327(11) Cl7 0.092(3) 0.0394(19) 0.063(2) -0.0135(16) -0.0006(19) -0.0335(18) S10 0.0439(12) 0.0735(16) 0.0262(10) -0.0121(10) 0.0042(9) -0.0326(12) S11 0.0419(12) 0.0635(15) 0.0255(10) -0.0106(10) 0.0029(9) -0.0264(11) S12 0.0435(13) 0.097(2) 0.0246(11) -0.0100(11) 0.0043(9) -0.0348(13) S13 0.0499(14) 0.136(3) 0.0340(12) -0.0216(14) 0.0033(11) -0.0535(16) S14 0.0463(12) 0.0686(16) 0.0265(10) -0.0121(10) 0.0057(9) -0.0338(12) S15 0.0460(12) 0.0652(15) 0.0237(10) -0.0101(10) 0.0020(9) -0.0339(11) S16 0.0428(12) 0.0660(16) 0.0311(11) -0.0046(10) -0.0049(9) -0.0314(11) S17 0.0452(12) 0.0681(16) 0.0244(10) -0.0007(10) -0.0003(9) -0.0313(11) C10 0.038(4) 0.038(5) 0.027(4) -0.011(3) 0.002(3) -0.018(4) C11 0.036(4) 0.045(5) 0.025(4) -0.011(3) 0.006(3) -0.019(4) C12 0.025(4) 0.053(5) 0.026(4) -0.012(4) 0.001(3) -0.008(4) C13 0.026(4) 0.056(6) 0.027(4) -0.009(4) -0.005(3) -0.008(4) C14 0.156(13) 0.31(2) 0.046(7) -0.068(10) 0.038(8) -0.186(15) C15 0.096(9) 0.264(18) 0.035(6) -0.047(9) 0.011(6) -0.107(11) C16 0.035(4) 0.041(5) 0.020(4) -0.009(3) 0.000(3) -0.009(4) C17 0.032(4) 0.034(4) 0.019(3) -0.002(3) 0.002(3) -0.012(3) C18 0.050(5) 0.064(6) 0.040(5) -0.014(4) -0.004(4) -0.024(5) C19 0.058(6) 0.062(6) 0.032(4) -0.022(4) -0.003(4) -0.021(5) S20 0.0421(12) 0.0663(16) 0.0340(11) -0.0104(11) 0.0056(9) -0.0288(11) S21 0.0403(12) 0.0686(16) 0.0279(10) -0.0125(10) 0.0030(9) -0.0267(11) S22 0.0467(14) 0.087(2) 0.0318(12) -0.0007(12) 0.0074(10) -0.0182(13) S23 0.0491(13) 0.0722(17) 0.0379(12) -0.0172(11) -0.0017(10) -0.0272(12) S24 0.0370(11) 0.0623(15) 0.0295(10) -0.0078(10) 0.0021(9) -0.0250(11) S25 0.0299(11) 0.0664(15) 0.0309(11) -0.0094(10) 0.0026(8) -0.0226(10) S26 0.0366(12) 0.0931(19) 0.0297(11) -0.0099(11) 0.0047(9) -0.0372(12) S27 0.0356(11) 0.0754(17) 0.0297(11) -0.0129(10) 0.0062(9) -0.0322(11) C20 0.028(4) 0.047(5) 0.036(4) -0.013(4) 0.008(3) -0.015(4) C21 0.036(4) 0.044(5) 0.028(4) -0.009(4) 0.003(3) -0.014(4) C22 0.040(5) 0.046(5) 0.026(4) -0.006(4) 0.005(3) -0.008(4) C23 0.042(5) 0.042(5) 0.029(4) -0.008(4) 0.002(4) -0.015(4) C24 0.081(7) 0.076(7) 0.032(5) -0.019(5) 0.007(5) -0.016(6) C25 0.061(6) 0.060(6) 0.033(5) -0.014(4) -0.009(4) -0.020(5) C26 0.037(4) 0.041(5) 0.030(4) -0.009(4) -0.001(3) -0.015(4) C27 0.026(4) 0.045(5) 0.028(4) -0.009(3) 0.002(3) -0.011(4) C28 0.066(6) 0.092(8) 0.045(5) -0.023(5) 0.004(5) -0.048(6) C29 0.050(5) 0.063(6) 0.035(5) -0.008(4) -0.001(4) -0.030(5) S30 0.0381(12) 0.0734(16) 0.0275(10) -0.0086(10) 0.0017(9) -0.0302(11) S31 0.0407(12) 0.0691(16) 0.0285(11) -0.0087(10) -0.0020(9) -0.0275(11) S32 0.0751(18) 0.102(2) 0.0255(11) -0.0067(12) 0.0059(11) -0.0496(16) S33 0.0459(13) 0.0868(19) 0.0422(13) -0.0294(13) -0.0113(10) -0.0179(13) S34 0.0351(11) 0.0718(16) 0.0252(10) -0.0107(10) 0.0024(8) -0.0251(11) S35 0.0365(11) 0.0652(15) 0.0279(10) -0.0066(10) -0.0002(9) -0.0234(11) S36 0.0432(13) 0.114(2) 0.0275(11) -0.0206(13) -0.0015(10) -0.0320(14) S37 0.0566(15) 0.0893(19) 0.0278(11) -0.0107(11) 0.0107(10) -0.0381(14) C30 0.029(4) 0.045(5) 0.025(4) -0.009(3) -0.002(3) -0.011(4) C31 0.030(4) 0.051(5) 0.027(4) -0.014(4) -0.003(3) -0.015(4) C32 0.041(5) 0.050(5) 0.023(4) -0.010(4) 0.003(3) -0.015(4) C33 0.028(4) 0.036(5) 0.025(4) -0.010(3) -0.004(3) -0.006(3) C34 0.056(7) 0.178(13) 0.036(6) -0.049(7) 0.003(5) -0.010(8) C35 0.194(16) 0.210(16) 0.022(5) 0.024(7) -0.028(7) -0.163(14) C36 0.032(4) 0.044(5) 0.026(4) -0.007(3) -0.004(3) -0.003(4) C37 0.032(4) 0.050(5) 0.020(4) -0.011(3) 0.002(3) -0.008(4) C38 0.079(7) 0.085(8) 0.036(5) -0.020(5) 0.002(5) -0.038(6) C39 0.067(6) 0.068(7) 0.037(5) -0.028(5) 0.019(4) -0.032(5) S40 0.0364(11) 0.0585(14) 0.0248(10) -0.0038(9) -0.0011(8) -0.0249(10) S41 0.0335(11) 0.0536(14) 0.0316(10) -0.0118(9) 0.0023(8) -0.0198(10) S42 0.0465(13) 0.0647(16) 0.0280(11) -0.0011(10) -0.0043(9) -0.0274(12) S43 0.0304(11) 0.0677(16) 0.0422(12) -0.0159(11) -0.0060(9) -0.0149(11) S44 0.0412(12) 0.0665(16) 0.0340(11) -0.0114(11) -0.0010(9) -0.0293(11) S45 0.0431(12) 0.0697(16) 0.0268(10) -0.0124(10) 0.0042(9) -0.0334(11) S46 0.0491(14) 0.0783(18) 0.0469(14) -0.0190(12) -0.0119(11) -0.0276(13) S47 0.0527(14) 0.0709(17) 0.0283(11) -0.0158(11) 0.0041(10) -0.0227(12) C40 0.030(4) 0.044(5) 0.028(4) -0.014(3) 0.004(3) -0.013(4) C41 0.033(4) 0.043(5) 0.030(4) -0.015(4) 0.005(3) -0.018(4) C42 0.034(4) 0.037(5) 0.025(4) -0.006(3) -0.010(3) -0.006(4) C43 0.025(4) 0.034(4) 0.028(4) -0.015(3) -0.001(3) 0.000(3) C44 0.066(7) 0.102(9) 0.028(5) -0.011(5) -0.004(4) -0.033(6) C45 0.066(7) 0.074(7) 0.039(5) 0.002(5) -0.023(5) -0.019(6) C46 0.040(5) 0.033(5) 0.032(4) -0.005(3) -0.010(3) -0.010(4) C47 0.045(5) 0.037(5) 0.022(4) -0.009(3) 0.002(3) -0.007(4) C48 0.056(6) 0.100(9) 0.041(5) -0.014(5) -0.017(5) -0.022(6) C49 0.083(8) 0.105(9) 0.032(5) -0.030(5) 0.001(5) -0.041(7) _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 S1 2.3547(19) . ? Mo1 S4 2.3868(19) . ? Mo1 S2 2.3970(19) . ? Mo1 S5 2.4736(18) . ? Mo1 Cl2 2.4801(19) . ? Mo1 S3 2.4807(18) . ? Mo1 Cl1 2.4962(19) . ? Mo1 Mo3 2.7501(8) . ? Mo1 Mo2 2.7560(8) . ? Mo2 S1 2.350(2) . ? Mo2 S4 2.388(2) . ? Mo2 S6 2.3883(19) . ? Mo2 Cl3 2.456(2) . ? Mo2 S5 2.488(2) . ? Mo2 S7 2.498(2) . ? Mo2 Cl4 2.507(2) . ? Mo2 Mo3 2.7645(8) . ? Mo3 S1 2.3600(19) . ? Mo3 S2 2.3795(19) . ? Mo3 S6 2.395(2) . ? Mo3 Cl6 2.4573(19) . ? Mo3 S3 2.4691(19) . ? Mo3 S7 2.482(2) . ? Mo3 Cl5 2.5115(19) . ? S2 S3 2.035(3) . ? S4 S5 2.036(3) . ? S6 S7 2.034(3) . ? S10 C11 1.727(7) . ? S10 C12 1.747(7) . ? S11 C11 1.729(7) . ? S11 C13 1.740(7) . ? S12 C14 1.745(11) . ? S12 C12 1.754(7) . ? S13 C13 1.729(8) . ? S13 C15 1.730(10) . ? S14 C16 1.729(7) . ? S14 C10 1.740(7) . ? S15 C10 1.726(7) . ? S15 C17 1.739(7) . ? S16 C16 1.755(7) . ? S16 C18 1.778(8) . ? S17 C17 1.742(7) . ? S17 C19 1.805(8) . ? C10 C11 1.364(9) . ? C12 C13 1.338(10) . ? C14 C15 1.277(14) . ? C16 C17 1.337(10) . ? C18 C19 1.501(11) . ? S20 C21 1.737(8) . ? S20 C22 1.745(8) . ? S21 C21 1.743(8) . ? S21 C23 1.745(7) . ? S22 C22 1.745(7) . ? S22 C24 1.821(10) . ? S23 C23 1.766(8) . ? S23 C25 1.788(8) . ? S24 C26 1.748(7) . ? S24 C20 1.749(8) . ? S25 C20 1.738(7) . ? S25 C27 1.750(7) . ? S26 C26 1.749(8) . ? S26 C28 1.801(9) . ? S27 C27 1.738(7) . ? S27 C29 1.795(8) . ? C20 C21 1.368(10) . ? C22 C23 1.328(10) . ? C24 C25 1.495(11) . ? C26 C27 1.348(10) . ? C28 C29 1.440(11) . ? S30 C31 1.723(8) . ? S30 C32 1.748(8) . ? S31 C31 1.726(7) . ? S31 C33 1.726(7) . ? S32 C32 1.728(8) . ? S32 C34 1.773(11) . ? S33 C35 1.712(10) . ? S33 C33 1.733(7) . ? S34 C30 1.731(7) . ? S34 C36 1.743(7) . ? S35 C30 1.721(7) . ? S35 C37 1.729(7) . ? S36 C36 1.741(8) . ? S36 C38 1.783(9) . ? S37 C37 1.733(7) . ? S37 C39 1.790(8) . ? C30 C31 1.374(9) . ? C32 C33 1.349(10) . ? C34 C35 1.354(14) . ? C36 C37 1.351(10) . ? C38 C39 1.481(12) . ? S40 C41 1.736(7) . ? S40 C42 1.742(7) . ? S41 C43 1.729(7) . ? S41 C41 1.733(7) . ? S42 C42 1.744(7) . ? S42 C44 1.808(9) . ? S43 C43 1.753(7) . ? S43 C45 1.787(9) . ? S44 C40 1.725(7) . ? S44 C46 1.738(8) . ? S45 C40 1.729(7) . ? S45 C47 1.748(7) . ? S46 C46 1.745(8) . ? S46 C48 1.775(9) . ? S47 C47 1.747(7) . ? S47 C49 1.769(9) . ? C40 C41 1.357(9) . ? C42 C43 1.351(10) . ? C44 C45 1.447(12) . ? C46 C47 1.341(10) . ? C48 C49 1.485(12) . ? C100 C101 1.456(16) . ? C101 N100 1.115(14) . ? 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 108.44(7) . . ? S1 Mo1 S2 108.60(6) . . ? S4 Mo1 S2 84.11(7) . . ? S1 Mo1 S5 85.34(7) . . ? S4 Mo1 S5 49.48(7) . . ? S2 Mo1 S5 133.29(7) . . ? S1 Mo1 Cl2 82.55(6) . . ? S4 Mo1 Cl2 133.61(6) . . ? S2 Mo1 Cl2 136.30(6) . . ? S5 Mo1 Cl2 88.60(6) . . ? S1 Mo1 S3 85.52(7) . . ? S4 Mo1 S3 133.08(7) . . ? S2 Mo1 S3 49.28(6) . . ? S5 Mo1 S3 170.74(7) . . ? Cl2 Mo1 S3 91.68(6) . . ? S1 Mo1 Cl1 164.01(7) . . ? S4 Mo1 Cl1 84.01(7) . . ? S2 Mo1 Cl1 82.07(6) . . ? S5 Mo1 Cl1 95.98(7) . . ? Cl2 Mo1 Cl1 81.55(7) . . ? S3 Mo1 Cl1 93.21(6) . . ? S1 Mo1 Mo3 54.41(5) . . ? S4 Mo1 Mo3 95.45(5) . . ? S2 Mo1 Mo3 54.55(5) . . ? S5 Mo1 Mo3 116.70(5) . . ? Cl2 Mo1 Mo3 124.66(5) . . ? S3 Mo1 Mo3 56.05(5) . . ? Cl1 Mo1 Mo3 136.28(5) . . ? S1 Mo1 Mo2 54.07(5) . . ? S4 Mo1 Mo2 54.76(5) . . ? S2 Mo1 Mo2 95.35(5) . . ? S5 Mo1 Mo2 56.51(5) . . ? Cl2 Mo1 Mo2 122.94(5) . . ? S3 Mo1 Mo2 116.24(5) . . ? Cl1 Mo1 Mo2 138.65(5) . . ? Mo3 Mo1 Mo2 60.27(2) . . ? S1 Mo2 S4 108.55(7) . . ? S1 Mo2 S6 108.58(7) . . ? S4 Mo2 S6 84.35(7) . . ? S1 Mo2 Cl3 82.79(7) . . ? S4 Mo2 Cl3 136.20(8) . . ? S6 Mo2 Cl3 133.29(8) . . ? S1 Mo2 S5 85.11(7) . . ? S4 Mo2 S5 49.30(7) . . ? S6 Mo2 S5 133.29(7) . . ? Cl3 Mo2 S5 91.79(8) . . ? S1 Mo2 S7 84.87(7) . . ? S4 Mo2 S7 133.04(7) . . ? S6 Mo2 S7 49.12(7) . . ? Cl3 Mo2 S7 89.06(8) . . ? S5 Mo2 S7 169.75(7) . . ? S1 Mo2 Cl4 163.48(7) . . ? S4 Mo2 Cl4 81.28(7) . . ? S6 Mo2 Cl4 85.16(7) . . ? Cl3 Mo2 Cl4 81.04(8) . . ? S5 Mo2 Cl4 92.05(7) . . ? S7 Mo2 Cl4 98.16(8) . . ? S1 Mo2 Mo1 54.22(5) . . ? S4 Mo2 Mo1 54.73(5) . . ? S6 Mo2 Mo1 95.51(5) . . ? Cl3 Mo2 Mo1 124.93(6) . . ? S5 Mo2 Mo1 56.01(5) . . ? S7 Mo2 Mo1 115.66(5) . . ? Cl4 Mo2 Mo1 135.54(6) . . ? S1 Mo2 Mo3 54.22(5) . . ? S4 Mo2 Mo3 95.06(5) . . ? S6 Mo2 Mo3 54.82(5) . . ? Cl3 Mo2 Mo3 123.42(7) . . ? S5 Mo2 Mo3 115.69(5) . . ? S7 Mo2 Mo3 56.00(5) . . ? Cl4 Mo2 Mo3 139.93(6) . . ? Mo1 Mo2 Mo3 59.76(2) . . ? S1 Mo3 S2 109.02(7) . . ? S1 Mo3 S6 108.02(7) . . ? S2 Mo3 S6 84.46(7) . . ? S1 Mo3 Cl6 82.99(7) . . ? S2 Mo3 Cl6 132.03(7) . . ? S6 Mo3 Cl6 137.27(7) . . ? S1 Mo3 S3 85.67(7) . . ? S2 Mo3 S3 49.59(7) . . ? S6 Mo3 S3 133.68(7) . . ? Cl6 Mo3 S3 87.19(7) . . ? S1 Mo3 S7 85.03(7) . . ? S2 Mo3 S7 133.43(7) . . ? S6 Mo3 S7 49.24(7) . . ? Cl6 Mo3 S7 92.78(7) . . ? S3 Mo3 S7 170.63(7) . . ? S1 Mo3 Cl5 164.50(7) . . ? S2 Mo3 Cl5 82.14(7) . . ? S6 Mo3 Cl5 83.23(7) . . ? Cl6 Mo3 Cl5 81.52(7) . . ? S3 Mo3 Cl5 94.20(7) . . ? S7 Mo3 Cl5 95.06(7) . . ? S1 Mo3 Mo1 54.23(5) . . ? S2 Mo3 Mo1 55.14(5) . . ? S6 Mo3 Mo1 95.50(5) . . ? Cl6 Mo3 Mo1 122.28(6) . . ? S3 Mo3 Mo1 56.45(4) . . ? S7 Mo3 Mo1 116.43(5) . . ? Cl5 Mo3 Mo1 137.07(5) . . ? S1 Mo3 Mo2 53.90(5) . . ? S2 Mo3 Mo2 95.54(5) . . ? S6 Mo3 Mo2 54.58(5) . . ? Cl6 Mo3 Mo2 125.82(5) . . ? S3 Mo3 Mo2 116.33(5) . . ? S7 Mo3 Mo2 56.57(5) . . ? Cl5 Mo3 Mo2 137.67(5) . . ? Mo1 Mo3 Mo2 59.97(2) . . ? Mo2 S1 Mo1 71.71(6) . . ? Mo2 S1 Mo3 71.87(6) . . ? Mo1 S1 Mo3 71.37(5) . . ? S3 S2 Mo3 67.50(8) . . ? S3 S2 Mo1 67.50(7) . . ? Mo3 S2 Mo1 70.31(5) . . ? S2 S3 Mo3 62.91(7) . . ? S2 S3 Mo1 63.22(7) . . ? Mo3 S3 Mo1 67.50(5) . . ? S5 S4 Mo1 67.48(8) . . ? S5 S4 Mo2 67.91(8) . . ? Mo1 S4 Mo2 70.51(6) . . ? S4 S5 Mo1 63.04(7) . . ? S4 S5 Mo2 62.79(7) . . ? Mo1 S5 Mo2 67.49(5) . . ? S7 S6 Mo2 68.26(8) . . ? S7 S6 Mo3 67.60(8) . . ? Mo2 S6 Mo3 70.61(6) . . ? S6 S7 Mo3 63.16(7) . . ? S6 S7 Mo2 62.62(8) . . ? Mo3 S7 Mo2 67.43(5) . . ? C11 S10 C12 95.3(4) . . ? C11 S11 C13 95.6(4) . . ? C14 S12 C12 99.7(5) . . ? C13 S13 C15 101.7(5) . . ? C16 S14 C10 95.3(4) . . ? C10 S15 C17 96.1(3) . . ? C16 S16 C18 101.6(4) . . ? C17 S17 C19 101.0(4) . . ? C11 C10 S15 122.8(6) . . ? C11 C10 S14 122.7(6) . . ? S15 C10 S14 114.4(4) . . ? C10 C11 S10 122.6(6) . . ? C10 C11 S11 122.1(6) . . ? S10 C11 S11 115.2(4) . . ? C13 C12 S10 117.0(6) . . ? C13 C12 S12 128.6(6) . . ? S10 C12 S12 114.4(4) . . ? C12 C13 S13 128.6(6) . . ? C12 C13 S11 116.9(5) . . ? S13 C13 S11 114.5(4) . . ? C15 C14 S12 129.6(9) . . ? C14 C15 S13 128.4(9) . . ? C17 C16 S14 117.9(5) . . ? C17 C16 S16 127.7(5) . . ? S14 C16 S16 114.4(4) . . ? C16 C17 S15 116.2(5) . . ? C16 C17 S17 129.4(6) . . ? S15 C17 S17 114.4(4) . . ? C19 C18 S16 114.8(6) . . ? C18 C19 S17 114.9(6) . . ? C21 S20 C22 95.4(4) . . ? C21 S21 C23 94.4(4) . . ? C22 S22 C24 102.9(4) . . ? C23 S23 C25 100.7(4) . . ? C26 S24 C20 95.3(4) . . ? C20 S25 C27 96.0(4) . . ? C26 S26 C28 100.5(4) . . ? C27 S27 C29 101.3(4) . . ? C21 C20 S25 122.8(6) . . ? C21 C20 S24 122.7(6) . . ? S25 C20 S24 114.5(4) . . ? C20 C21 S20 123.1(6) . . ? C20 C21 S21 121.9(6) . . ? S20 C21 S21 115.0(4) . . ? C23 C22 S20 116.5(6) . . ? C23 C22 S22 128.8(6) . . ? S20 C22 S22 114.6(5) . . ? C22 C23 S21 118.4(6) . . ? C22 C23 S23 127.8(6) . . ? S21 C23 S23 113.8(4) . . ? C25 C24 S22 114.5(6) . . ? C24 C25 S23 114.7(6) . . ? C27 C26 S24 117.6(6) . . ? C27 C26 S26 127.6(6) . . ? S24 C26 S26 114.8(4) . . ? C26 C27 S27 129.3(6) . . ? C26 C27 S25 116.3(6) . . ? S27 C27 S25 114.3(4) . . ? C29 C28 S26 116.4(6) . . ? C28 C29 S27 115.6(6) . . ? C31 S30 C32 95.0(4) . . ? C31 S31 C33 95.6(4) . . ? C32 S32 C34 101.4(5) . . ? C35 S33 C33 102.9(5) . . ? C30 S34 C36 95.9(4) . . ? C30 S35 C37 96.3(4) . . ? C36 S36 C38 102.3(4) . . ? C37 S37 C39 99.0(4) . . ? C31 C30 S35 121.9(6) . . ? C31 C30 S34 123.4(6) . . ? S35 C30 S34 114.7(4) . . ? C30 C31 S30 123.1(6) . . ? C30 C31 S31 121.4(6) . . ? S30 C31 S31 115.5(4) . . ? C33 C32 S32 129.0(6) . . ? C33 C32 S30 116.7(5) . . ? S32 C32 S30 114.3(5) . . ? C32 C33 S31 117.0(5) . . ? C32 C33 S33 127.7(6) . . ? S31 C33 S33 115.2(4) . . ? C35 C34 S32 123.5(8) . . ? C34 C35 S33 127.6(9) . . ? C37 C36 S36 128.7(6) . . ? C37 C36 S34 116.2(5) . . ? S36 C36 S34 115.1(5) . . ? C36 C37 S35 117.0(5) . . ? C36 C37 S37 127.5(6) . . ? S35 C37 S37 115.5(4) . . ? C39 C38 S36 118.3(6) . . ? C38 C39 S37 113.5(6) . . ? C41 S40 C42 96.1(4) . . ? C43 S41 C41 95.5(3) . . ? C42 S42 C44 99.7(4) . . ? C43 S43 C45 101.0(4) . . ? C40 S44 C46 95.5(4) . . ? C40 S45 C47 95.2(4) . . ? C46 S46 C48 100.6(4) . . ? C47 S47 C49 101.6(4) . . ? C41 C40 S44 122.4(6) . . ? C41 C40 S45 122.3(6) . . ? S44 C40 S45 115.2(4) . . ? C40 C41 S41 123.5(6) . . ? C40 C41 S40 122.1(6) . . ? S41 C41 S40 114.3(4) . . ? C43 C42 S40 115.4(5) . . ? C43 C42 S42 128.5(5) . . ? S40 C42 S42 116.1(4) . . ? C42 C43 S41 118.1(5) . . ? C42 C43 S43 128.4(6) . . ? S41 C43 S43 113.4(4) . . ? C45 C44 S42 114.9(7) . . ? C44 C45 S43 116.4(7) . . ? C47 C46 S44 117.1(6) . . ? C47 C46 S46 127.7(6) . . ? S44 C46 S46 115.2(5) . . ? C46 C47 S47 129.6(6) . . ? C46 C47 S45 116.7(6) . . ? S47 C47 S45 113.7(5) . . ? C49 C48 S46 116.5(7) . . ? C48 C49 S47 116.7(7) . . ? N100 C101 C100 169.5(15) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.023 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.151 #===END