data_(Et4N)4[Tp2Mo2Fe6S8(N3)4]2MeCN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety (Et4N)4[Tp2Mo2Fe6S8(N3)4]2MeCN _chemical_formula_sum 'C54 H106 B2 Fe6 Mo2 N30 S8' _chemical_formula_weight 1980.77 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' 'B' 'B' 0.0013 0.0007 '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' 'Fe' 'Fe' 0.3463 0.8444 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.882(2) _cell_length_b 20.771(4) _cell_length_c 17.159(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.818(4) _cell_angle_gamma 90.00 _cell_volume 4172.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour black _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2036 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ? _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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 30085 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.30 _reflns_number_total 10328 _reflns_number_gt 7076 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0218P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10328 _refine_ls_number_parameters 639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _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 0.718360(19) 0.007659(11) 0.713299(13) 0.02560(6) Uani 1 1 d . . . Fe1 Fe 0.50457(3) 0.055115(18) 0.67469(2) 0.03119(10) Uani 1 1 d . . . Fe2 Fe 0.66114(3) 0.099700(18) 0.60143(2) 0.02932(10) Uani 1 1 d . . . Fe3 Fe 0.58100(3) -0.015562(17) 0.56935(2) 0.02829(9) Uani 1 1 d . . . S1 S 0.54437(6) -0.05191(3) 0.68881(4) 0.03260(17) Uani 1 1 d . . . S2 S 0.65719(6) 0.11453(3) 0.73283(4) 0.03129(16) Uani 1 1 d . . . S3 S 0.76960(6) 0.01122(3) 0.58620(4) 0.03004(16) Uani 1 1 d . . . S4 S 0.46958(6) 0.08144(3) 0.53743(4) 0.03367(17) Uani 1 1 d . . . N1 N 0.89498(19) 0.04307(11) 0.75863(13) 0.0330(6) Uani 1 1 d . . . N2 N 0.9679(2) 0.01069(11) 0.81491(14) 0.0360(6) Uani 1 1 d . . . N3 N 0.7261(2) -0.00666(11) 0.84402(13) 0.0337(6) Uani 1 1 d . . . N4 N 0.8215(2) -0.03135(11) 0.88988(14) 0.0380(6) Uani 1 1 d . . . N5 N 0.80772(19) -0.08808(10) 0.72805(14) 0.0314(5) Uani 1 1 d . . . N6 N 0.8907(2) -0.10121(11) 0.79137(14) 0.0339(6) Uani 1 1 d . . . N7 N 0.3707(2) 0.08222(12) 0.72464(17) 0.0429(6) Uani 1 1 d . . . N8 N 0.3678(2) 0.08035(13) 0.7916(2) 0.0494(7) Uani 1 1 d . . . N9 N 0.3615(3) 0.07824(18) 0.8593(2) 0.0815(11) Uani 1 1 d . . . N10 N 0.7129(2) 0.18337(11) 0.55814(15) 0.0398(6) Uani 1 1 d . . . N11 N 0.7652(2) 0.22475(13) 0.58948(16) 0.0473(7) Uani 1 1 d . . . N12 N 0.8169(3) 0.26888(16) 0.6183(2) 0.0939(13) Uani 1 1 d . . . N13 N 0.8262(2) 0.10473(11) 0.35482(14) 0.0373(6) Uani 1 1 d . . . N14 N 0.3893(3) 0.22261(12) 0.08582(17) 0.0501(7) Uani 1 1 d . . . N15 N 1.0314(4) 0.1997(2) 0.9617(3) 0.1252(18) Uani 1 1 d . . . B1 B 0.9269(3) -0.04963(18) 0.8543(2) 0.0411(9) Uani 1 1 d . . . C1 C 0.9523(3) 0.09374(16) 0.7384(2) 0.0408(8) Uani 1 1 d . . . C2 C 1.0618(3) 0.09473(17) 0.7816(2) 0.0459(8) Uani 1 1 d . . . C3 C 1.0684(3) 0.04201(16) 0.8284(2) 0.0423(8) Uani 1 1 d . . . C4 C 0.6530(3) 0.00574(15) 0.8927(2) 0.0410(8) Uani 1 1 d . . . C5 C 0.6987(3) -0.01147(16) 0.9691(2) 0.0513(9) Uani 1 1 d . . . C6 C 0.8043(3) -0.03496(16) 0.96533(19) 0.0466(9) Uani 1 1 d . . . C7 C 0.7919(3) -0.14180(15) 0.6858(2) 0.0390(7) Uani 1 1 d . . . C8 C 0.8635(3) -0.19020(15) 0.7210(2) 0.0432(8) Uani 1 1 d . . . C9 C 0.9239(3) -0.16284(15) 0.7873(2) 0.0396(8) Uani 1 1 d . . . C10 C 0.8346(3) 0.0926(2) 0.2692(2) 0.0519(9) Uani 1 1 d . . . C11 C 0.7238(3) 0.07978(17) 0.21519(19) 0.0605(10) Uani 1 1 d . . . H11A H 0.6905 0.0408 0.2311 0.091 Uiso 1 1 calc R . . H11B H 0.7374 0.0752 0.1619 0.091 Uiso 1 1 calc R . . H11C H 0.6724 0.1151 0.2179 0.091 Uiso 1 1 calc R . . C12 C 0.9464(3) 0.1185(2) 0.3979(2) 0.0549(10) Uani 1 1 d . . . C13 C 0.9574(4) 0.1317(2) 0.4838(3) 0.0613(11) Uani 1 1 d . . . C14 C 0.7777(3) 0.04682(17) 0.3908(2) 0.0429(8) Uani 1 1 d . . . C15 C 0.8476(4) -0.01290(19) 0.3968(3) 0.0621(11) Uani 1 1 d . . . C16 C 0.7469(4) 0.16039(19) 0.3623(2) 0.0566(10) Uani 1 1 d . . . C17 C 0.7766(4) 0.22214(17) 0.3243(3) 0.0974(16) Uani 1 1 d . . . H17A H 0.8537 0.2342 0.3458 0.146 Uiso 1 1 calc R . . H17B H 0.7254 0.2556 0.3347 0.146 Uiso 1 1 calc R . . H17C H 0.7696 0.2160 0.2683 0.146 Uiso 1 1 calc R . . C18 C 0.4748(4) 0.2554(2) 0.1506(3) 0.0337(11) Uani 0.60 1 d P A 1 H18A H 0.4655 0.3016 0.1448 0.040 Uiso 0.60 1 calc PR A 1 H18B H 0.5514 0.2449 0.1422 0.040 Uiso 0.60 1 calc PR A 1 C19 C 0.4641(14) 0.2365(8) 0.2383(7) 0.060(3) Uani 0.60 1 d P A 1 H19A H 0.3872 0.2438 0.2464 0.090 Uiso 0.60 1 calc PR A 1 H19B H 0.5155 0.2625 0.2746 0.090 Uiso 0.60 1 calc PR A 1 H19C H 0.4831 0.1919 0.2471 0.090 Uiso 0.60 1 calc PR A 1 C20 C 0.4089(5) 0.2533(3) 0.0084(3) 0.0405(14) Uani 0.60 1 d P A 1 H20A H 0.3901 0.2987 0.0098 0.049 Uiso 0.60 1 calc PR A 1 H20B H 0.4896 0.2502 0.0056 0.049 Uiso 0.60 1 calc PR A 1 C21 C 0.3418(8) 0.2246(7) -0.0662(8) 0.062(3) Uani 0.60 1 d P A 1 H21A H 0.3594 0.1796 -0.0685 0.093 Uiso 0.60 1 calc PR A 1 H21B H 0.3618 0.2461 -0.1114 0.093 Uiso 0.60 1 calc PR A 1 H21C H 0.2616 0.2298 -0.0659 0.093 Uiso 0.60 1 calc PR A 1 C22 C 0.2750(4) 0.2233(2) 0.0997(3) 0.0341(11) Uani 0.60 1 d P A 1 H22A H 0.2733 0.1978 0.1468 0.041 Uiso 0.60 1 calc PR A 1 H22B H 0.2293 0.2005 0.0561 0.041 Uiso 0.60 1 calc PR A 1 C23 C 0.2120(15) 0.2868(7) 0.1103(10) 0.095(6) Uani 0.60 1 d P A 1 H23A H 0.2403 0.3045 0.1616 0.142 Uiso 0.60 1 calc PR A 1 H23B H 0.1316 0.2786 0.1056 0.142 Uiso 0.60 1 calc PR A 1 H23C H 0.2248 0.3169 0.0703 0.142 Uiso 0.60 1 calc PR A 1 C24 C 0.4274(4) 0.1491(2) 0.0842(3) 0.0426(13) Uani 0.60 1 d P A 1 H24A H 0.4334 0.1326 0.1377 0.051 Uiso 0.60 1 calc PR A 1 H24B H 0.3658 0.1258 0.0518 0.051 Uiso 0.60 1 calc PR A 1 C25 C 0.5334(8) 0.1322(3) 0.0561(5) 0.068(2) Uani 0.60 1 d P A 1 H25A H 0.5258 0.1421 0.0008 0.103 Uiso 0.60 1 calc PR A 1 H25B H 0.5482 0.0870 0.0641 0.103 Uiso 0.60 1 calc PR A 1 H25C H 0.5957 0.1565 0.0850 0.103 Uiso 0.60 1 calc PR A 1 C181 C 0.3818(10) 0.1869(5) 0.1577(7) 0.087(4) Uani 0.40 1 d P A 2 H18C H 0.4103 0.1434 0.1543 0.104 Uiso 0.40 1 calc PR A 2 H18D H 0.3033 0.1847 0.1662 0.104 Uiso 0.40 1 calc PR A 2 C191 C 0.455(2) 0.2236(13) 0.2245(13) 0.088(8) Uani 0.40 1 d P A 2 H19D H 0.5125 0.2476 0.2038 0.132 Uiso 0.40 1 calc PR A 2 H19E H 0.4912 0.1937 0.2636 0.132 Uiso 0.40 1 calc PR A 2 H19F H 0.4079 0.2526 0.2482 0.132 Uiso 0.40 1 calc PR A 2 C201 C 0.2896(10) 0.1946(5) 0.0241(7) 0.088(4) Uani 0.40 1 d P A 2 H20C H 0.3027 0.1491 0.0170 0.106 Uiso 0.40 1 calc PR A 2 H20D H 0.2185 0.1992 0.0441 0.106 Uiso 0.40 1 calc PR A 2 C211 C 0.2787(16) 0.2289(11) -0.0567(11) 0.108(7) Uani 0.40 1 d P A 2 H21D H 0.3532 0.2343 -0.0704 0.162 Uiso 0.40 1 calc PR A 2 H21E H 0.2439 0.2703 -0.0535 0.162 Uiso 0.40 1 calc PR A 2 H21F H 0.2322 0.2034 -0.0964 0.162 Uiso 0.40 1 calc PR A 2 C221 C 0.3176(12) 0.2958(5) 0.1017(7) 0.079(4) Uani 0.40 1 d P A 2 H22C H 0.3619 0.3163 0.1477 0.095 Uiso 0.40 1 calc PR A 2 H22D H 0.3225 0.3236 0.0569 0.095 Uiso 0.40 1 calc PR A 2 C231 C 0.2297(16) 0.2962(9) 0.1101(16) 0.074(7) Uani 0.40 1 d P A 2 H23D H 0.2139 0.2578 0.1374 0.112 Uiso 0.40 1 calc PR A 2 H23E H 0.1806 0.2980 0.0595 0.112 Uiso 0.40 1 calc PR A 2 H23F H 0.2164 0.3332 0.1408 0.112 Uiso 0.40 1 calc PR A 2 C241 C 0.4776(12) 0.2395(5) 0.0576(10) 0.112(6) Uani 0.40 1 d P A 2 H24C H 0.5278 0.2651 0.0961 0.134 Uiso 0.40 1 calc PR A 2 H24D H 0.4553 0.2653 0.0104 0.134 Uiso 0.40 1 calc PR A 2 C251 C 0.5447(12) 0.1739(6) 0.0360(10) 0.101(5) Uani 0.40 1 d P A 2 H25D H 0.5402 0.1415 0.0752 0.151 Uiso 0.40 1 calc PR A 2 H25E H 0.6233 0.1839 0.0351 0.151 Uiso 0.40 1 calc PR A 2 H25F H 0.5094 0.1582 -0.0150 0.151 Uiso 0.40 1 calc PR A 2 C26 C 0.9514(4) 0.17122(19) 0.9548(3) 0.0814(15) Uani 1 1 d . . . C27 C 0.8461(4) 0.13606(19) 0.9440(3) 0.0966(16) Uani 1 1 d . . . H27A H 0.8172 0.1317 0.8885 0.145 Uiso 1 1 calc R . . H27B H 0.7915 0.1588 0.9689 0.145 Uiso 1 1 calc R . . H27C H 0.8591 0.0941 0.9674 0.145 Uiso 1 1 calc R . . H1 H 0.994(2) -0.0679(11) 0.8992(15) 0.030(7) Uiso 1 1 d . . . H2 H 0.918(3) 0.1225(13) 0.7027(18) 0.048(10) Uiso 1 1 d . . . H3 H 1.120(3) 0.1237(13) 0.7741(18) 0.053(10) Uiso 1 1 d . . . H4 H 1.130(3) 0.0264(13) 0.8678(17) 0.044(9) Uiso 1 1 d . . . H5 H 0.584(2) 0.0203(13) 0.8728(17) 0.036(9) Uiso 1 1 d . . . H6 H 0.661(3) -0.0104(13) 1.0088(18) 0.048(9) Uiso 1 1 d . . . H7 H 0.861(3) -0.0541(13) 1.0031(18) 0.046(9) Uiso 1 1 d . . . H8 H 0.742(2) -0.1422(11) 0.6408(14) 0.019(7) Uiso 1 1 d . . . H9 H 0.870(2) -0.2309(12) 0.7064(15) 0.031(8) Uiso 1 1 d . . . H10 H 0.977(2) -0.1797(12) 0.8273(16) 0.031(8) Uiso 1 1 d . . . H13 H 0.972(3) 0.1536(14) 0.3721(18) 0.056(10) Uiso 1 1 d . . . H14 H 0.988(3) 0.0824(14) 0.3876(18) 0.048(10) Uiso 1 1 d . . . H15 H 0.929(3) 0.0991(15) 0.5117(19) 0.058(11) Uiso 1 1 d . . . H16 H 1.034(3) 0.1372(16) 0.501(2) 0.071(12) Uiso 1 1 d . . . H17 H 0.923(3) 0.1689(18) 0.496(2) 0.083(15) Uiso 1 1 d . . . H18 H 0.744(3) 0.1656(15) 0.419(2) 0.074(12) Uiso 1 1 d . . . H19 H 0.677(3) 0.1472(14) 0.3405(19) 0.049(10) Uiso 1 1 d . . . H22 H 0.885(3) 0.0550(16) 0.271(2) 0.076(12) Uiso 1 1 d . . . H23 H 0.870(3) 0.1309(15) 0.2515(19) 0.062(10) Uiso 1 1 d . . . H25 H 0.706(2) 0.0421(13) 0.3612(17) 0.039(8) Uiso 1 1 d . . . H26 H 0.768(3) 0.0610(13) 0.4401(18) 0.045(9) Uiso 1 1 d . . . H27 H 0.870(3) -0.0271(16) 0.350(2) 0.071(13) Uiso 1 1 d . . . H28 H 0.919(3) -0.0095(15) 0.4294(19) 0.056(11) Uiso 1 1 d . . . H29 H 0.810(3) -0.0487(16) 0.422(2) 0.077(12) 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 0.02295(12) 0.02810(12) 0.02383(13) 0.00064(10) -0.00145(9) -0.00109(10) Fe1 0.0251(2) 0.0293(2) 0.0374(3) 0.00030(18) 0.00059(18) 0.00014(18) Fe2 0.0319(2) 0.0269(2) 0.0269(2) 0.00021(17) -0.00148(18) -0.00276(18) Fe3 0.0262(2) 0.0253(2) 0.0296(2) -0.00078(17) -0.00627(17) 0.00043(17) S1 0.0259(4) 0.0295(4) 0.0406(4) 0.0042(3) 0.0007(3) -0.0027(3) S2 0.0324(4) 0.0297(4) 0.0297(4) -0.0036(3) -0.0005(3) -0.0012(3) S3 0.0286(4) 0.0343(4) 0.0257(4) -0.0004(3) 0.0002(3) -0.0009(3) S4 0.0345(4) 0.0257(3) 0.0351(4) -0.0035(3) -0.0105(3) 0.0039(3) N1 0.0267(13) 0.0402(14) 0.0290(14) -0.0023(11) -0.0038(11) -0.0029(11) N2 0.0301(13) 0.0442(14) 0.0300(13) -0.0013(11) -0.0056(11) -0.0008(12) N3 0.0345(14) 0.0374(13) 0.0288(13) 0.0029(11) 0.0046(11) 0.0002(11) N4 0.0440(16) 0.0421(14) 0.0249(14) 0.0041(11) -0.0026(12) 0.0057(12) N5 0.0273(13) 0.0332(13) 0.0313(14) 0.0018(11) -0.0019(11) 0.0043(11) N6 0.0295(13) 0.0378(13) 0.0329(14) 0.0048(11) 0.0008(11) 0.0033(11) N7 0.0345(15) 0.0529(16) 0.0418(17) 0.0064(13) 0.0083(14) 0.0040(13) N8 0.0309(15) 0.0534(17) 0.064(2) -0.0011(16) 0.0098(16) -0.0012(13) N9 0.071(2) 0.127(3) 0.048(2) -0.002(2) 0.0158(19) -0.003(2) N10 0.0488(17) 0.0349(14) 0.0339(15) 0.0022(12) 0.0014(13) -0.0101(13) N11 0.0515(18) 0.0465(17) 0.0443(18) 0.0070(14) 0.0096(15) -0.0051(15) N12 0.107(3) 0.075(2) 0.095(3) -0.015(2) 0.004(2) -0.050(2) N13 0.0317(14) 0.0423(14) 0.0374(15) 0.0045(12) 0.0048(12) -0.0033(12) N14 0.062(2) 0.0370(15) 0.0475(18) 0.0072(13) -0.0030(16) -0.0188(15) N15 0.087(3) 0.104(3) 0.161(5) -0.037(3) -0.045(3) 0.000(3) B1 0.0349(19) 0.053(2) 0.031(2) 0.0062(17) -0.0059(16) 0.0055(18) C1 0.0343(18) 0.0438(19) 0.043(2) -0.0023(16) 0.0024(16) -0.0088(16) C2 0.0343(18) 0.052(2) 0.050(2) -0.0119(17) 0.0016(16) -0.0140(17) C3 0.0280(16) 0.057(2) 0.0379(19) -0.0121(16) -0.0060(15) 0.0003(16) C4 0.045(2) 0.0375(18) 0.0413(19) 0.0052(15) 0.0106(16) 0.0009(16) C5 0.069(3) 0.054(2) 0.035(2) 0.0091(17) 0.0200(19) 0.004(2) C6 0.061(2) 0.046(2) 0.0297(19) 0.0079(15) 0.0009(18) 0.0022(18) C7 0.0340(18) 0.0363(17) 0.044(2) 0.0012(15) -0.0019(16) -0.0004(15) C8 0.0383(19) 0.0298(17) 0.061(2) 0.0024(16) 0.0075(17) 0.0050(15) C9 0.0297(17) 0.0399(18) 0.049(2) 0.0147(16) 0.0067(16) 0.0057(15) C10 0.057(2) 0.063(2) 0.040(2) 0.0072(18) 0.0210(19) -0.002(2) C11 0.075(3) 0.072(2) 0.034(2) -0.0020(18) 0.0084(19) -0.012(2) C12 0.038(2) 0.062(3) 0.063(3) 0.010(2) 0.0039(19) -0.012(2) C13 0.049(2) 0.063(3) 0.063(3) 0.005(2) -0.015(2) -0.013(2) C14 0.0354(19) 0.056(2) 0.035(2) 0.0076(17) -0.0006(16) -0.0076(17) C15 0.072(3) 0.047(2) 0.061(3) 0.006(2) -0.007(2) 0.003(2) C16 0.059(3) 0.058(2) 0.046(2) -0.0083(19) -0.010(2) 0.015(2) C17 0.136(4) 0.045(2) 0.093(4) 0.004(2) -0.031(3) 0.002(3) C18 0.034(3) 0.035(3) 0.030(3) 0.002(2) -0.002(2) -0.014(2) C19 0.065(7) 0.088(8) 0.023(4) 0.016(6) -0.006(4) -0.012(5) C20 0.042(3) 0.037(3) 0.040(4) 0.007(3) -0.001(3) 0.003(3) C21 0.072(6) 0.053(5) 0.058(6) -0.003(4) -0.001(5) 0.007(5) C22 0.025(3) 0.033(3) 0.041(3) 0.002(2) -0.004(2) -0.005(2) C23 0.104(12) 0.077(8) 0.090(9) 0.045(7) -0.023(7) -0.021(7) C24 0.039(3) 0.020(2) 0.064(4) 0.001(2) -0.003(3) 0.002(2) C25 0.070(6) 0.056(5) 0.073(6) 0.002(4) -0.005(4) 0.011(4) C181 0.091(9) 0.058(6) 0.109(10) 0.022(7) 0.007(8) -0.010(6) C191 0.053(9) 0.103(13) 0.090(15) -0.053(9) -0.040(8) 0.030(9) C201 0.083(9) 0.067(7) 0.114(11) 0.008(7) 0.013(8) -0.004(6) C211 0.21(2) 0.070(9) 0.033(7) 0.012(6) -0.002(14) -0.007(15) C221 0.131(12) 0.042(6) 0.063(7) 0.009(5) 0.013(8) -0.011(8) C231 0.016(5) 0.022(6) 0.17(2) -0.015(8) -0.015(8) 0.008(5) C241 0.128(13) 0.033(6) 0.194(19) -0.007(8) 0.086(13) -0.017(7) C251 0.052(7) 0.135(13) 0.118(13) -0.038(11) 0.023(8) -0.014(10) C26 0.094(4) 0.042(2) 0.089(3) -0.010(2) -0.039(3) 0.005(2) C27 0.127(4) 0.065(3) 0.082(3) 0.013(2) -0.027(3) -0.029(3) _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 N1 2.235(2) . ? Mo1 N5 2.248(2) . ? Mo1 N3 2.249(2) . ? Mo1 S3 2.3632(8) . ? Mo1 S2 2.3771(8) . ? Mo1 S1 2.3844(8) . ? Mo1 Fe1 2.6998(6) . ? Mo1 Fe2 2.7123(6) . ? Mo1 Fe3 2.7608(6) . ? Fe1 N7 2.011(3) . ? Fe1 S1 2.2771(9) . ? Fe1 S2 2.2779(8) . ? Fe1 S4 2.3843(9) . ? Fe1 Fe2 2.5877(6) . ? Fe1 Fe3 2.6089(6) . ? Fe2 N10 2.026(2) . ? Fe2 S2 2.2840(9) . ? Fe2 S3 2.2850(8) . ? Fe2 S4 2.3828(9) . ? Fe2 Fe3 2.6005(6) . ? Fe3 S3 2.2789(9) . ? Fe3 S4 2.2837(8) 3_656 ? Fe3 S1 2.2945(9) . ? Fe3 S4 2.4218(8) . ? Fe3 Fe3 2.8679(9) 3_656 ? S4 Fe3 2.2837(8) 3_656 ? N1 C1 1.332(4) . ? N1 N2 1.361(3) . ? N2 C3 1.344(4) . ? N2 B1 1.542(4) . ? N3 C4 1.329(4) . ? N3 N4 1.365(3) . ? N4 C6 1.347(4) . ? N4 B1 1.531(4) . ? N5 C7 1.326(4) . ? N5 N6 1.364(3) . ? N6 C9 1.345(4) . ? N6 B1 1.530(4) . ? N7 N8 1.157(4) . ? N8 N9 1.177(4) . ? N10 N11 1.140(3) . ? N11 N12 1.165(4) . ? N13 C16 1.511(4) . ? N13 C10 1.510(4) . ? N13 C14 1.511(4) . ? N13 C12 1.519(4) . ? N14 C241 1.277(12) . ? N14 C22 1.419(5) . ? N14 C181 1.455(10) . ? N14 C20 1.527(6) . ? N14 C18 1.531(5) . ? N14 C201 1.561(12) . ? N14 C24 1.594(5) . ? N14 C221 1.786(11) . ? N15 C26 1.108(5) . ? C1 C2 1.383(4) . ? C2 C3 1.353(5) . ? C4 C5 1.377(5) . ? C5 C6 1.357(5) . ? C7 C8 1.387(4) . ? C8 C9 1.361(5) . ? C10 C11 1.499(5) . ? C12 C13 1.483(6) . ? C14 C15 1.486(5) . ? C16 C17 1.507(5) . ? C18 C19 1.581(11) . ? C20 C21 1.510(15) . ? C22 C23 1.542(16) . ? C24 C25 1.466(10) . ? C181 C191 1.52(3) . ? C201 C211 1.54(2) . ? C221 C231 1.08(2) . ? C241 C251 1.651(16) . ? C26 C27 1.433(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 N1 Mo1 N5 81.64(8) . . ? N1 Mo1 N3 79.64(8) . . ? N5 Mo1 N3 80.35(8) . . ? N1 Mo1 S3 86.36(6) . . ? N5 Mo1 S3 86.59(6) . . ? N3 Mo1 S3 162.06(6) . . ? N1 Mo1 S2 86.28(6) . . ? N5 Mo1 S2 163.73(6) . . ? N3 Mo1 S2 86.81(6) . . ? S3 Mo1 S2 103.53(3) . . ? N1 Mo1 S1 165.18(6) . . ? N5 Mo1 S1 86.53(6) . . ? N3 Mo1 S1 89.65(6) . . ? S3 Mo1 S1 101.87(3) . . ? S2 Mo1 S1 103.45(3) . . ? N1 Mo1 Fe1 138.91(6) . . ? N5 Mo1 Fe1 139.21(6) . . ? N3 Mo1 Fe1 99.77(6) . . ? S3 Mo1 Fe1 98.15(2) . . ? S2 Mo1 Fe1 52.85(2) . . ? S1 Mo1 Fe1 52.77(2) . . ? N1 Mo1 Fe2 96.98(6) . . ? N5 Mo1 Fe2 139.44(6) . . ? N3 Mo1 Fe2 139.62(6) . . ? S3 Mo1 Fe2 52.97(2) . . ? S2 Mo1 Fe2 52.83(2) . . ? S1 Mo1 Fe2 97.81(2) . . ? Fe1 Mo1 Fe2 57.126(13) . . ? N1 Mo1 Fe3 138.22(6) . . ? N5 Mo1 Fe3 98.16(6) . . ? N3 Mo1 Fe3 141.87(6) . . ? S3 Mo1 Fe3 52.11(2) . . ? S2 Mo1 Fe3 98.10(2) . . ? S1 Mo1 Fe3 52.35(2) . . ? Fe1 Mo1 Fe3 57.067(14) . . ? Fe2 Mo1 Fe3 56.728(15) . . ? N7 Fe1 S1 113.13(7) . . ? N7 Fe1 S2 106.86(8) . . ? S1 Fe1 S2 110.30(3) . . ? N7 Fe1 S4 109.83(8) . . ? S1 Fe1 S4 109.09(3) . . ? S2 Fe1 S4 107.46(3) . . ? N7 Fe1 Fe2 142.47(7) . . ? S1 Fe1 Fe2 104.34(3) . . ? S2 Fe1 Fe2 55.55(2) . . ? S4 Fe1 Fe2 57.09(2) . . ? N7 Fe1 Fe3 147.84(8) . . ? S1 Fe1 Fe3 55.52(2) . . ? S2 Fe1 Fe3 105.25(3) . . ? S4 Fe1 Fe3 57.82(2) . . ? Fe2 Fe1 Fe3 60.053(17) . . ? N7 Fe1 Mo1 140.98(8) . . ? S1 Fe1 Mo1 56.49(2) . . ? S2 Fe1 Mo1 56.28(2) . . ? S4 Fe1 Mo1 108.93(2) . . ? Fe2 Fe1 Mo1 61.680(17) . . ? Fe3 Fe1 Mo1 62.643(15) . . ? N10 Fe2 S2 107.74(7) . . ? N10 Fe2 S3 115.82(8) . . ? S2 Fe2 S3 109.16(3) . . ? N10 Fe2 S4 107.06(8) . . ? S2 Fe2 S4 107.31(3) . . ? S3 Fe2 S4 109.41(3) . . ? N10 Fe2 Fe1 140.64(7) . . ? S2 Fe2 Fe1 55.33(2) . . ? S3 Fe2 Fe1 103.53(3) . . ? S4 Fe2 Fe1 57.15(3) . . ? N10 Fe2 Fe3 146.63(7) . . ? S2 Fe2 Fe3 105.34(2) . . ? S3 Fe2 Fe3 55.16(2) . . ? S4 Fe2 Fe3 57.96(2) . . ? Fe1 Fe2 Fe3 60.379(16) . . ? N10 Fe2 Mo1 143.98(8) . . ? S2 Fe2 Mo1 56.03(2) . . ? S3 Fe2 Mo1 55.66(2) . . ? S4 Fe2 Mo1 108.57(2) . . ? Fe1 Fe2 Mo1 61.194(16) . . ? Fe3 Fe2 Mo1 62.576(16) . . ? S3 Fe3 S4 111.50(3) . 3_656 ? S3 Fe3 S1 107.41(3) . . ? S4 Fe3 S1 117.10(3) 3_656 . ? S3 Fe3 S4 108.26(3) . . ? S4 Fe3 S4 104.96(3) 3_656 . ? S1 Fe3 S4 107.23(3) . . ? S3 Fe3 Fe2 55.37(2) . . ? S4 Fe3 Fe2 139.31(3) 3_656 . ? S1 Fe3 Fe2 103.43(2) . . ? S4 Fe3 Fe2 56.51(2) . . ? S3 Fe3 Fe1 103.04(2) . . ? S4 Fe3 Fe1 144.88(3) 3_656 . ? S1 Fe3 Fe1 54.89(2) . . ? S4 Fe3 Fe1 56.43(2) . . ? Fe2 Fe3 Fe1 59.569(16) . . ? S3 Fe3 Mo1 54.93(2) . . ? S4 Fe3 Mo1 148.98(2) 3_656 . ? S1 Fe3 Mo1 55.36(2) . . ? S4 Fe3 Mo1 105.90(2) . . ? Fe2 Fe3 Mo1 60.696(13) . . ? Fe1 Fe3 Mo1 60.290(17) . . ? S3 Fe3 Fe3 123.82(3) . 3_656 ? S4 Fe3 Fe3 54.67(2) 3_656 3_656 ? S1 Fe3 Fe3 127.79(3) . 3_656 ? S4 Fe3 Fe3 50.29(2) . 3_656 ? Fe2 Fe3 Fe3 97.92(2) . 3_656 ? Fe1 Fe3 Fe3 100.63(2) . 3_656 ? Mo1 Fe3 Fe3 156.03(2) . 3_656 ? Fe1 S1 Fe3 69.59(2) . . ? Fe1 S1 Mo1 70.74(2) . . ? Fe3 S1 Mo1 72.29(2) . . ? Fe1 S2 Fe2 69.12(3) . . ? Fe1 S2 Mo1 70.86(2) . . ? Fe2 S2 Mo1 71.14(2) . . ? Fe3 S3 Fe2 69.47(3) . . ? Fe3 S3 Mo1 72.96(2) . . ? Fe2 S3 Mo1 71.37(2) . . ? Fe3 S4 Fe2 124.41(4) 3_656 . ? Fe3 S4 Fe1 129.26(3) 3_656 . ? Fe2 S4 Fe1 65.75(2) . . ? Fe3 S4 Fe3 75.04(3) 3_656 . ? Fe2 S4 Fe3 65.53(2) . . ? Fe1 S4 Fe3 65.75(2) . . ? C1 N1 N2 106.5(2) . . ? C1 N1 Mo1 131.4(2) . . ? N2 N1 Mo1 122.09(17) . . ? C3 N2 N1 108.8(2) . . ? C3 N2 B1 130.9(3) . . ? N1 N2 B1 120.1(2) . . ? C4 N3 N4 106.1(2) . . ? C4 N3 Mo1 133.0(2) . . ? N4 N3 Mo1 120.90(17) . . ? C6 N4 N3 109.1(3) . . ? C6 N4 B1 129.6(3) . . ? N3 N4 B1 121.2(2) . . ? C7 N5 N6 106.4(2) . . ? C7 N5 Mo1 131.5(2) . . ? N6 N5 Mo1 121.98(17) . . ? C9 N6 N5 109.1(2) . . ? C9 N6 B1 130.8(3) . . ? N5 N6 B1 120.0(2) . . ? N8 N7 Fe1 125.0(2) . . ? N7 N8 N9 178.1(4) . . ? N11 N10 Fe2 130.5(2) . . ? N10 N11 N12 176.7(4) . . ? C16 N13 C10 110.9(3) . . ? C16 N13 C14 106.7(3) . . ? C10 N13 C14 111.0(3) . . ? C16 N13 C12 111.2(3) . . ? C10 N13 C12 107.0(3) . . ? C14 N13 C12 110.1(3) . . ? C241 N14 C22 158.9(7) . . ? C241 N14 C181 129.3(9) . . ? C22 N14 C181 70.4(5) . . ? C241 N14 C20 45.5(7) . . ? C22 N14 C20 115.7(4) . . ? C181 N14 C20 172.3(6) . . ? C241 N14 C18 70.5(8) . . ? C22 N14 C18 114.2(4) . . ? C181 N14 C18 75.0(5) . . ? C20 N14 C18 105.4(3) . . ? C241 N14 C201 115.0(9) . . ? C22 N14 C201 58.7(5) . . ? C181 N14 C201 103.7(6) . . ? C20 N14 C201 77.0(5) . . ? C18 N14 C201 172.3(5) . . ? C241 N14 C24 90.1(5) . . ? C22 N14 C24 107.2(3) . . ? C181 N14 C24 65.5(5) . . ? C20 N14 C24 107.4(4) . . ? C18 N14 C24 106.4(3) . . ? C201 N14 C24 79.4(4) . . ? C241 N14 C221 105.6(6) . . ? C22 N14 C221 58.0(4) . . ? C181 N14 C221 101.9(6) . . ? C20 N14 C221 85.6(4) . . ? C18 N14 C221 77.6(5) . . ? C201 N14 C221 95.4(6) . . ? C24 N14 C221 164.2(5) . . ? N6 B1 N4 107.7(3) . . ? N6 B1 N2 109.3(3) . . ? N4 B1 N2 108.3(3) . . ? N1 C1 C2 110.4(3) . . ? C3 C2 C1 105.1(3) . . ? N2 C3 C2 109.2(3) . . ? N3 C4 C5 110.7(3) . . ? C6 C5 C4 105.4(3) . . ? N4 C6 C5 108.6(3) . . ? N5 C7 C8 110.7(3) . . ? C9 C8 C7 104.9(3) . . ? N6 C9 C8 108.9(3) . . ? C11 C10 N13 115.8(3) . . ? C13 C12 N13 115.8(3) . . ? C15 C14 N13 116.4(3) . . ? C17 C16 N13 114.8(3) . . ? N14 C18 C19 115.4(6) . . ? C21 C20 N14 115.8(7) . . ? N14 C22 C23 121.8(7) . . ? C25 C24 N14 119.8(4) . . ? N14 C181 C191 105.9(12) . . ? C211 C201 N14 112.1(10) . . ? C231 C221 N14 121.7(12) . . ? N14 C241 C251 108.6(8) . . ? N15 C26 C27 178.1(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.666 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.074 #--------------------------------END data_(et4n)2[tpmofe3s4(n3)3] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Et4N)2[TpMoFe3S4(N3)3] ' _chemical_formula_sum 'C25 H50 B Fe3 Mo N17 S4' _chemical_formula_weight 991.36 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' 'B' 'B' 0.0013 0.0007 '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' 'Fe' 'Fe' 0.3463 0.8444 '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 10.6920(17) _cell_length_b 34.707(6) _cell_length_c 10.9322(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.902(4) _cell_angle_gamma 90.00 _cell_volume 4051.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark black ' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.605 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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_% none _diffrn_reflns_number 29261 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 28.31 _reflns_number_total 10050 _reflns_number_gt 6084 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0425P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10050 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 0.70251(3) 0.155627(11) 0.77829(3) 0.02584(9) Uani 1 1 d . . . Fe1 Fe 0.89551(6) 0.140469(19) 0.94207(6) 0.03392(16) Uani 1 1 d . . . Fe2 Fe 0.92586(5) 0.131381(18) 0.69926(6) 0.02987(15) Uani 1 1 d . . . Fe3 Fe 0.78398(6) 0.081873(19) 0.82030(6) 0.04046(18) Uani 1 1 d . . . S1 S 0.69485(11) 0.11953(4) 0.96199(10) 0.0430(3) Uani 1 1 d . . . S2 S 0.89912(9) 0.18720(3) 0.79942(10) 0.0297(2) Uani 1 1 d . . . S3 S 0.73652(10) 0.10708(3) 0.63300(10) 0.0305(2) Uani 1 1 d . . . S4 S 0.99897(11) 0.09059(4) 0.85323(12) 0.0434(3) Uani 1 1 d . . . N1 N 0.6600(3) 0.19435(10) 0.6190(3) 0.0305(8) Uani 1 1 d . . . N2 N 0.5590(3) 0.21845(10) 0.6132(4) 0.0369(9) Uani 1 1 d . . . N3 N 0.4987(3) 0.14506(11) 0.7460(3) 0.0353(9) Uani 1 1 d . . . N4 N 0.4177(3) 0.17420(11) 0.7146(4) 0.0406(10) Uani 1 1 d . . . N5 N 0.6227(3) 0.20461(11) 0.8832(3) 0.0381(9) Uani 1 1 d . . . N6 N 0.5269(3) 0.22615(12) 0.8354(4) 0.0457(11) Uani 1 1 d . . . N7 N 0.9557(4) 0.15778(14) 1.1070(4) 0.0578(13) Uani 1 1 d . . . N8 N 0.8932(5) 0.1631(3) 1.1859(5) 0.142(4) Uani 1 1 d . . . N9 N 0.8348(11) 0.1478(4) 1.2766(10) 0.090(4) Uani 0.50 1 d P . . N91 N 0.8273(11) 0.1874(3) 1.2534(8) 0.067(3) Uani 0.50 1 d P . . N10 N 1.0299(4) 0.13707(13) 0.5577(4) 0.0452(10) Uani 1 1 d . . . N11 N 1.0733(4) 0.11423(14) 0.4933(4) 0.0476(11) Uani 1 1 d . . . N12 N 1.1202(5) 0.09244(18) 0.4291(5) 0.0871(19) Uani 1 1 d . . . N13 N 0.7351(6) 0.02751(14) 0.8285(5) 0.0868(19) Uani 1 1 d . . . N14 N 0.6863(5) 0.00597(14) 0.7646(5) 0.0635(13) Uani 1 1 d . . . N15 N 0.6347(7) -0.01742(18) 0.7060(6) 0.107(2) Uani 1 1 d . . . N16 N 0.3366(3) 0.14637(10) 0.1801(3) 0.0360(9) Uani 1 1 d . . . N17 N 0.7940(5) 0.02297(17) 1.2712(6) 0.0858(19) Uani 1 1 d . . . B1 B 0.4611(5) 0.21636(17) 0.7096(6) 0.0463(15) Uani 1 1 d . . . C1 C 0.7168(4) 0.19827(13) 0.5122(4) 0.0364(11) Uani 1 1 d . . . H1 H 0.7881 0.1849 0.4912 0.044 Uiso 1 1 calc R . . C2 C 0.6533(5) 0.22513(14) 0.4385(5) 0.0502(14) Uani 1 1 d . . . H2 H 0.6727 0.2333 0.3607 0.060 Uiso 1 1 calc R . . C3 C 0.5555(5) 0.23705(14) 0.5059(5) 0.0501(14) Uani 1 1 d . . . H3 H 0.4958 0.2553 0.4808 0.060 Uiso 1 1 calc R . . C4 C 0.4323(4) 0.11251(15) 0.7393(4) 0.0417(12) Uani 1 1 d . . . H4 H 0.4645 0.0881 0.7569 0.050 Uiso 1 1 calc R . . C5 C 0.3092(4) 0.12000(15) 0.7028(5) 0.0466(13) Uani 1 1 d . . . H5 H 0.2444 0.1023 0.6912 0.056 Uiso 1 1 calc R . . C6 C 0.3034(4) 0.15898(16) 0.6872(5) 0.0491(14) Uani 1 1 d . . . H6 H 0.2323 0.1728 0.6619 0.059 Uiso 1 1 calc R . . C7 C 0.6548(5) 0.21980(16) 0.9923(4) 0.0514(14) Uani 1 1 d . . . H7 H 0.7197 0.2107 1.0444 0.062 Uiso 1 1 calc R . . C8 C 0.5799(5) 0.25050(18) 1.0177(6) 0.0685(19) Uani 1 1 d . . . H8 H 0.5825 0.2657 1.0879 0.082 Uiso 1 1 calc R . . C9 C 0.5010(5) 0.25376(16) 0.9169(6) 0.0638(18) Uani 1 1 d . . . H9 H 0.4385 0.2723 0.9059 0.077 Uiso 1 1 calc R . . C10 C 0.2696(4) 0.10872(13) 0.1550(4) 0.0429(12) Uani 1 1 d . . . H10A H 0.1850 0.1144 0.1240 0.052 Uiso 1 1 calc R . . H10B H 0.2635 0.0952 0.2321 0.052 Uiso 1 1 calc R . . C11 C 0.3293(6) 0.08204(14) 0.0654(5) 0.0626(16) Uani 1 1 d . . . H11A H 0.3204 0.0928 -0.0155 0.094 Uiso 1 1 calc R . . H11B H 0.2888 0.0574 0.0664 0.094 Uiso 1 1 calc R . . H11C H 0.4166 0.0790 0.0885 0.094 Uiso 1 1 calc R . . C12 C 0.4643(4) 0.14018(16) 0.2430(5) 0.0536(14) Uani 1 1 d . . . H12A H 0.5142 0.1248 0.1898 0.064 Uiso 1 1 calc R . . H12B H 0.5052 0.1650 0.2530 0.064 Uiso 1 1 calc R . . C13 C 0.4646(6) 0.12080(19) 0.3667(6) 0.079(2) Uani 1 1 d . . . H13A H 0.4233 0.1371 0.4231 0.118 Uiso 1 1 calc R . . H13B H 0.5494 0.1164 0.3964 0.118 Uiso 1 1 calc R . . H13C H 0.4213 0.0966 0.3591 0.118 Uiso 1 1 calc R . . C14 C 0.2532(4) 0.16980(14) 0.2593(5) 0.0459(13) Uani 1 1 d . . . H14A H 0.2457 0.1564 0.3365 0.055 Uiso 1 1 calc R . . H14B H 0.1703 0.1711 0.2193 0.055 Uiso 1 1 calc R . . C15 C 0.2989(5) 0.21054(17) 0.2859(6) 0.083(2) Uani 1 1 d . . . H15A H 0.3836 0.2097 0.3194 0.125 Uiso 1 1 calc R . . H15B H 0.2464 0.2224 0.3437 0.125 Uiso 1 1 calc R . . H15C H 0.2956 0.2252 0.2113 0.125 Uiso 1 1 calc R . . C16 C 0.3575(4) 0.16689(14) 0.0604(5) 0.0448(12) Uani 1 1 d . . . H16A H 0.4014 0.1908 0.0785 0.054 Uiso 1 1 calc R . . H16B H 0.4117 0.1510 0.0126 0.054 Uiso 1 1 calc R . . C17 C 0.2416(5) 0.17580(15) -0.0164(5) 0.0567(14) Uani 1 1 d . . . H17A H 0.2079 0.1524 -0.0514 0.085 Uiso 1 1 calc R . . H17B H 0.2615 0.1932 -0.0807 0.085 Uiso 1 1 calc R . . H17C H 0.1808 0.1875 0.0337 0.085 Uiso 1 1 calc R . . C18 C 0.6710(8) 0.03601(17) 1.2097(6) 0.088(2) Uani 1 1 d . A . H18A H 0.6099 0.0389 1.2717 0.106 Uiso 1 1 calc R . . H18B H 0.6830 0.0611 1.1733 0.106 Uiso 1 1 calc R . . C19 C 0.6188(9) 0.0091(2) 1.1121(6) 0.136(4) Uani 1 1 d . . . H19A H 0.6810 0.0044 1.0535 0.203 Uiso 1 1 calc R A . H19B H 0.5462 0.0205 1.0716 0.203 Uiso 1 1 calc R . . H19C H 0.5960 -0.0149 1.1489 0.203 Uiso 1 1 calc R . . C20 C 0.7791(8) -0.0159(2) 1.3182(8) 0.113(3) Uani 1 1 d . A . H20A H 0.8586 -0.0243 1.3560 0.135 Uiso 1 1 calc R . . H20B H 0.7589 -0.0330 1.2498 0.135 Uiso 1 1 calc R . . C21 C 0.6775(11) -0.0202(2) 1.4124(7) 0.149(4) Uani 1 1 d . . . H21A H 0.6974 -0.0039 1.4815 0.224 Uiso 1 1 calc R A . H21B H 0.6739 -0.0465 1.4390 0.224 Uiso 1 1 calc R . . H21C H 0.5977 -0.0128 1.3753 0.224 Uiso 1 1 calc R . . C22 C 0.8704(9) 0.0307(3) 1.1425(8) 0.046(2) Uani 0.50 1 d P A 1 H22A H 0.8588 0.0088 1.0880 0.055 Uiso 1 1 calc R A 1 H22B H 0.8364 0.0533 1.1008 0.055 Uiso 1 1 calc R A 1 C23 C 0.9908(7) 0.0358(3) 1.1696(7) 0.139(4) Uani 1 1 d . A 1 H23A H 1.0023 0.0581 1.2208 0.208 Uiso 1 1 calc R A 1 H23B H 1.0339 0.0394 1.0955 0.208 Uiso 1 1 calc R A 1 H23C H 1.0239 0.0135 1.2121 0.208 Uiso 1 1 calc R A 1 C221 C 0.9171(11) 0.0100(3) 1.2296(11) 0.061(3) Uani 0.50 1 d P A 2 C24 C 0.8251(6) 0.0517(2) 1.3707(8) 0.122(4) Uani 1 1 d . A 1 H24A H 0.9067 0.0463 1.4097 0.146 Uiso 1 1 calc R A 1 H24B H 0.7631 0.0509 1.4324 0.146 Uiso 1 1 calc R A 1 C25 C 0.8251(10) 0.0972(3) 1.2993(9) 0.050(3) Uani 0.50 1 d P A 1 H25A H 0.8840 0.0972 1.2359 0.076 Uiso 1 1 calc R A 1 H25B H 0.8484 0.1166 1.3588 0.076 Uiso 1 1 calc R A 1 H25C H 0.7428 0.1027 1.2643 0.076 Uiso 1 1 calc R A 1 C251 C 0.9295(14) 0.0262(4) 1.5048(11) 0.081(4) Uani 0.50 1 d P 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 0.02000(17) 0.0337(2) 0.02364(17) -0.00004(16) -0.00090(13) -0.00290(16) Fe1 0.0282(3) 0.0450(4) 0.0279(3) 0.0029(3) -0.0055(3) -0.0036(3) Fe2 0.0230(3) 0.0340(4) 0.0323(3) -0.0013(3) -0.0005(2) 0.0010(3) Fe3 0.0419(4) 0.0365(4) 0.0417(4) 0.0102(3) -0.0109(3) -0.0095(3) S1 0.0348(6) 0.0650(9) 0.0288(6) 0.0123(6) -0.0020(5) -0.0138(6) S2 0.0225(5) 0.0326(6) 0.0335(6) -0.0016(5) -0.0013(4) -0.0037(5) S3 0.0269(5) 0.0338(6) 0.0304(6) -0.0023(5) -0.0029(4) -0.0012(5) S4 0.0393(7) 0.0393(7) 0.0502(8) 0.0031(6) -0.0131(6) 0.0064(6) N1 0.0283(19) 0.027(2) 0.035(2) 0.0042(16) -0.0061(16) 0.0004(16) N2 0.0288(19) 0.031(2) 0.050(2) -0.0023(18) -0.0109(17) 0.0047(17) N3 0.0217(17) 0.048(2) 0.036(2) -0.0021(18) 0.0000(15) -0.0011(17) N4 0.0185(18) 0.048(2) 0.056(3) -0.016(2) 0.0013(17) 0.0024(18) N5 0.027(2) 0.048(2) 0.040(2) -0.0138(18) 0.0052(17) -0.0062(18) N6 0.0202(19) 0.053(3) 0.064(3) -0.025(2) 0.0062(18) 0.0009(18) N7 0.038(2) 0.102(4) 0.032(2) -0.001(2) -0.0094(19) -0.012(2) N8 0.056(4) 0.338(12) 0.031(3) -0.044(5) 0.003(3) -0.027(5) N9 0.090(8) 0.117(11) 0.063(7) -0.001(7) 0.008(6) 0.008(8) N91 0.116(9) 0.040(6) 0.046(6) -0.003(4) 0.017(6) -0.002(6) N10 0.033(2) 0.057(3) 0.046(3) 0.001(2) 0.0076(19) -0.004(2) N11 0.034(2) 0.081(4) 0.029(2) 0.003(2) 0.0051(18) -0.009(2) N12 0.063(3) 0.141(6) 0.059(3) -0.037(4) 0.017(3) -0.002(3) N13 0.119(5) 0.047(3) 0.089(4) 0.031(3) -0.044(4) -0.040(3) N14 0.066(3) 0.052(3) 0.071(4) 0.015(3) -0.011(3) -0.014(3) N15 0.135(6) 0.084(5) 0.101(5) -0.017(4) 0.000(4) -0.046(4) N16 0.0283(19) 0.036(2) 0.044(2) -0.0056(17) 0.0025(16) 0.0015(17) N17 0.066(4) 0.064(4) 0.130(5) -0.058(4) 0.038(4) -0.017(3) B1 0.029(3) 0.048(4) 0.061(4) -0.015(3) -0.003(3) 0.001(3) C1 0.033(2) 0.042(3) 0.034(3) 0.003(2) 0.000(2) -0.005(2) C2 0.059(3) 0.047(3) 0.045(3) 0.020(2) -0.006(3) -0.010(3) C3 0.044(3) 0.037(3) 0.066(4) 0.010(3) -0.028(3) 0.000(2) C4 0.036(3) 0.045(3) 0.044(3) 0.001(2) -0.001(2) -0.011(2) C5 0.023(2) 0.054(3) 0.063(3) -0.012(3) 0.002(2) -0.013(2) C6 0.020(2) 0.063(4) 0.064(4) -0.023(3) -0.003(2) -0.002(2) C7 0.042(3) 0.072(4) 0.041(3) -0.021(3) 0.011(2) -0.025(3) C8 0.045(3) 0.090(5) 0.072(4) -0.055(4) 0.019(3) -0.020(3) C9 0.034(3) 0.060(4) 0.099(5) -0.039(3) 0.012(3) -0.002(3) C10 0.049(3) 0.040(3) 0.040(3) -0.001(2) 0.002(2) -0.002(2) C11 0.071(4) 0.040(3) 0.078(4) -0.013(3) 0.012(3) 0.005(3) C12 0.032(3) 0.065(4) 0.063(4) -0.016(3) -0.002(2) 0.008(3) C13 0.066(4) 0.100(5) 0.068(4) 0.003(4) -0.020(3) 0.006(4) C14 0.031(2) 0.053(3) 0.053(3) -0.019(3) 0.004(2) 0.004(2) C15 0.059(4) 0.067(4) 0.122(6) -0.053(4) -0.010(4) 0.012(3) C16 0.040(3) 0.039(3) 0.057(3) 0.003(2) 0.012(2) -0.003(2) C17 0.062(4) 0.055(4) 0.054(3) 0.012(3) 0.009(3) 0.006(3) C18 0.147(7) 0.049(4) 0.073(5) 0.014(3) 0.051(5) 0.021(4) C19 0.215(10) 0.144(8) 0.044(4) -0.030(5) -0.036(5) 0.108(7) C20 0.138(7) 0.082(6) 0.109(7) -0.050(5) -0.073(6) 0.052(5) C21 0.315(15) 0.063(5) 0.070(6) 0.016(4) 0.013(7) -0.003(7) C22 0.049(6) 0.052(7) 0.036(5) -0.006(5) -0.001(5) 0.017(5) C23 0.096(6) 0.254(12) 0.066(5) 0.000(6) 0.007(5) -0.088(7) C221 0.061(7) 0.060(8) 0.063(8) 0.012(6) 0.015(6) 0.002(6) C24 0.065(4) 0.110(6) 0.191(9) -0.117(7) 0.021(5) -0.011(4) C25 0.065(7) 0.041(6) 0.045(6) -0.009(5) 0.000(5) -0.007(5) C251 0.120(11) 0.077(9) 0.043(7) 0.008(6) -0.023(7) 0.011(8) _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 N3 2.220(3) . ? Mo1 N1 2.228(3) . ? Mo1 N5 2.243(4) . ? Mo1 S3 2.3564(12) . ? Mo1 S2 2.3716(11) . ? Mo1 S1 2.3719(12) . ? Mo1 Fe2 2.7141(8) . ? Mo1 Fe1 2.7142(7) . ? Mo1 Fe3 2.7353(9) . ? Fe1 N7 1.977(4) . ? Fe1 S2 2.2517(13) . ? Fe1 S1 2.2860(13) . ? Fe1 S4 2.2963(14) . ? Fe1 Fe3 2.6775(10) . ? Fe1 Fe2 2.7089(10) . ? Fe2 N10 1.961(4) . ? Fe2 S2 2.2507(13) . ? Fe2 S3 2.2772(12) . ? Fe2 S4 2.3057(14) . ? Fe2 Fe3 2.6847(9) . ? Fe3 N13 1.961(5) . ? Fe3 S3 2.2606(13) . ? Fe3 S1 2.2728(15) . ? Fe3 S4 2.3283(14) . ? N1 C1 1.350(5) . ? N1 N2 1.365(4) . ? N2 C3 1.337(6) . ? N2 B1 1.525(7) . ? N3 C4 1.334(5) . ? N3 N4 1.364(5) . ? N4 C6 1.351(5) . ? N4 B1 1.537(7) . ? N5 C7 1.333(5) . ? N5 N6 1.352(5) . ? N6 C9 1.347(6) . ? N6 B1 1.551(7) . ? N7 N8 1.133(6) . ? N8 N9 1.310(13) . ? N8 N91 1.345(11) . ? N10 N11 1.172(5) . ? N11 N12 1.163(6) . ? N13 N14 1.132(6) . ? N14 N15 1.157(7) . ? N16 C10 1.509(5) . ? N16 C14 1.512(5) . ? N16 C12 1.513(6) . ? N16 C16 1.516(6) . ? N17 C20 1.457(9) . ? N17 C221 1.484(12) . ? N17 C24 1.501(7) . ? N17 C18 1.516(9) . ? N17 C22 1.683(10) . ? C1 C2 1.387(6) . ? C2 C3 1.374(7) . ? C4 C5 1.380(6) . ? C5 C6 1.365(7) . ? C7 C8 1.370(7) . ? C8 C9 1.358(8) . ? C10 C11 1.512(6) . ? C12 C13 1.509(7) . ? C14 C15 1.519(7) . ? C16 C17 1.494(7) . ? C18 C19 1.504(9) . ? C20 C21 1.541(11) . ? C22 C23 1.318(10) . ? C24 C25 1.762(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 N3 Mo1 N1 79.37(13) . . ? N3 Mo1 N5 79.10(13) . . ? N1 Mo1 N5 82.79(14) . . ? N3 Mo1 S3 87.62(10) . . ? N1 Mo1 S3 86.39(10) . . ? N5 Mo1 S3 164.19(10) . . ? N3 Mo1 S2 161.77(10) . . ? N1 Mo1 S2 86.69(9) . . ? N5 Mo1 S2 87.61(9) . . ? S3 Mo1 S2 103.28(4) . . ? N3 Mo1 S1 88.38(10) . . ? N1 Mo1 S1 164.97(10) . . ? N5 Mo1 S1 86.39(11) . . ? S3 Mo1 S1 101.90(5) . . ? S2 Mo1 S1 103.30(4) . . ? N3 Mo1 Fe2 140.39(10) . . ? N1 Mo1 Fe2 94.96(9) . . ? N5 Mo1 Fe2 139.58(9) . . ? S3 Mo1 Fe2 52.80(3) . . ? S2 Mo1 Fe2 52.00(3) . . ? S1 Mo1 Fe2 100.05(4) . . ? N3 Mo1 Fe1 141.28(10) . . ? N1 Mo1 Fe1 138.65(9) . . ? N5 Mo1 Fe1 96.07(10) . . ? S3 Mo1 Fe1 99.67(3) . . ? S2 Mo1 Fe1 52.03(3) . . ? S1 Mo1 Fe1 52.90(3) . . ? Fe2 Mo1 Fe1 59.87(2) . . ? N3 Mo1 Fe3 100.00(10) . . ? N1 Mo1 Fe3 138.28(9) . . ? N5 Mo1 Fe3 138.54(10) . . ? S3 Mo1 Fe3 52.07(3) . . ? S2 Mo1 Fe3 98.21(3) . . ? S1 Mo1 Fe3 52.26(4) . . ? Fe2 Mo1 Fe3 59.03(2) . . ? Fe1 Mo1 Fe3 58.86(2) . . ? N7 Fe1 S2 113.36(15) . . ? N7 Fe1 S1 105.88(13) . . ? S2 Fe1 S1 110.12(5) . . ? N7 Fe1 S4 118.24(14) . . ? S2 Fe1 S4 102.98(5) . . ? S1 Fe1 S4 105.97(5) . . ? N7 Fe1 Fe3 143.18(14) . . ? S2 Fe1 Fe3 103.04(4) . . ? S1 Fe1 Fe3 53.80(4) . . ? S4 Fe1 Fe3 55.18(4) . . ? N7 Fe1 Fe2 151.56(13) . . ? S2 Fe1 Fe2 53.00(3) . . ? S1 Fe1 Fe2 102.47(4) . . ? S4 Fe1 Fe2 54.10(4) . . ? Fe3 Fe1 Fe2 59.79(2) . . ? N7 Fe1 Mo1 138.11(14) . . ? S2 Fe1 Mo1 56.13(3) . . ? S1 Fe1 Mo1 55.85(3) . . ? S4 Fe1 Mo1 103.51(4) . . ? Fe3 Fe1 Mo1 60.97(2) . . ? Fe2 Fe1 Mo1 60.06(2) . . ? N10 Fe2 S2 112.85(13) . . ? N10 Fe2 S3 108.48(12) . . ? S2 Fe2 S3 109.93(4) . . ? N10 Fe2 S4 116.94(13) . . ? S2 Fe2 S4 102.72(5) . . ? S3 Fe2 S4 105.54(5) . . ? N10 Fe2 Fe3 144.16(13) . . ? S2 Fe2 Fe3 102.84(4) . . ? S3 Fe2 Fe3 53.44(3) . . ? S4 Fe2 Fe3 54.99(4) . . ? N10 Fe2 Fe1 149.59(12) . . ? S2 Fe2 Fe1 53.03(3) . . ? S3 Fe2 Fe1 101.90(4) . . ? S4 Fe2 Fe1 53.78(4) . . ? Fe3 Fe2 Fe1 59.52(2) . . ? N10 Fe2 Mo1 139.77(13) . . ? S2 Fe2 Mo1 56.14(3) . . ? S3 Fe2 Mo1 55.51(3) . . ? S4 Fe2 Mo1 103.25(4) . . ? Fe3 Fe2 Mo1 60.88(2) . . ? Fe1 Fe2 Mo1 60.07(2) . . ? N13 Fe3 S3 111.45(16) . . ? N13 Fe3 S1 113.6(2) . . ? S3 Fe3 S1 108.19(5) . . ? N13 Fe3 S4 112.41(18) . . ? S3 Fe3 S4 105.33(5) . . ? S1 Fe3 S4 105.35(5) . . ? N13 Fe3 Fe1 145.18(16) . . ? S3 Fe3 Fe1 103.31(4) . . ? S1 Fe3 Fe1 54.26(4) . . ? S4 Fe3 Fe1 54.07(4) . . ? N13 Fe3 Fe2 142.8(2) . . ? S3 Fe3 Fe2 54.01(3) . . ? S1 Fe3 Fe2 103.58(4) . . ? S4 Fe3 Fe2 54.20(4) . . ? Fe1 Fe3 Fe2 60.69(3) . . ? N13 Fe3 Mo1 145.56(18) . . ? S3 Fe3 Mo1 55.30(3) . . ? S1 Fe3 Mo1 55.62(4) . . ? S4 Fe3 Mo1 102.00(4) . . ? Fe1 Fe3 Mo1 60.18(2) . . ? Fe2 Fe3 Mo1 60.09(2) . . ? Fe3 S1 Fe1 71.93(4) . . ? Fe3 S1 Mo1 72.12(4) . . ? Fe1 S1 Mo1 71.25(4) . . ? Fe2 S2 Fe1 73.98(4) . . ? Fe2 S2 Mo1 71.86(4) . . ? Fe1 S2 Mo1 71.84(4) . . ? Fe3 S3 Fe2 72.55(4) . . ? Fe3 S3 Mo1 72.63(4) . . ? Fe2 S3 Mo1 71.69(4) . . ? Fe1 S4 Fe2 72.12(4) . . ? Fe1 S4 Fe3 70.75(4) . . ? Fe2 S4 Fe3 70.81(4) . . ? C1 N1 N2 106.7(4) . . ? C1 N1 Mo1 130.8(3) . . ? N2 N1 Mo1 122.4(3) . . ? C3 N2 N1 108.9(4) . . ? C3 N2 B1 129.7(4) . . ? N1 N2 B1 120.5(4) . . ? C4 N3 N4 106.5(3) . . ? C4 N3 Mo1 131.6(3) . . ? N4 N3 Mo1 121.5(3) . . ? C6 N4 N3 108.8(4) . . ? C6 N4 B1 129.4(4) . . ? N3 N4 B1 121.8(3) . . ? C7 N5 N6 106.4(4) . . ? C7 N5 Mo1 132.0(4) . . ? N6 N5 Mo1 121.5(3) . . ? C9 N6 N5 108.4(4) . . ? C9 N6 B1 130.1(5) . . ? N5 N6 B1 121.5(4) . . ? N8 N7 Fe1 124.5(4) . . ? N7 N8 N9 146.4(12) . . ? N7 N8 N91 150.0(11) . . ? N9 N8 N91 63.6(6) . . ? N11 N10 Fe2 131.6(4) . . ? N12 N11 N10 177.5(6) . . ? N14 N13 Fe3 136.3(5) . . ? N13 N14 N15 175.5(7) . . ? C10 N16 C14 106.3(3) . . ? C10 N16 C12 111.7(4) . . ? C14 N16 C12 111.1(4) . . ? C10 N16 C16 109.8(4) . . ? C14 N16 C16 111.1(4) . . ? C12 N16 C16 106.9(4) . . ? C20 N17 C221 86.6(7) . . ? C20 N17 C24 112.6(7) . . ? C221 N17 C24 104.9(7) . . ? C20 N17 C18 109.0(5) . . ? C221 N17 C18 135.9(7) . . ? C24 N17 C18 106.2(5) . . ? C20 N17 C22 120.6(6) . . ? C221 N17 C22 46.9(5) . . ? C24 N17 C22 113.6(6) . . ? C18 N17 C22 91.7(6) . . ? N2 B1 N4 106.8(4) . . ? N2 B1 N6 107.9(4) . . ? N4 B1 N6 107.5(4) . . ? N1 C1 C2 110.0(4) . . ? C3 C2 C1 104.8(4) . . ? N2 C3 C2 109.7(4) . . ? N3 C4 C5 110.7(5) . . ? C6 C5 C4 105.0(4) . . ? N4 C6 C5 109.0(4) . . ? N5 C7 C8 111.2(5) . . ? C9 C8 C7 104.3(5) . . ? N6 C9 C8 109.7(5) . . ? N16 C10 C11 115.8(4) . . ? C13 C12 N16 115.6(4) . . ? N16 C14 C15 114.6(4) . . ? C17 C16 N16 115.3(4) . . ? C19 C18 N17 114.3(5) . . ? N17 C20 C21 114.7(6) . . ? C23 C22 N17 110.1(7) . . ? N17 C24 C25 106.2(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.745 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.090 #--------------------------------END data_(Et4N)3[Tp2Mo2Fe6S8(SPh)4]MeCN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (Et4N)3[Tp2Mo2Fe6S8(SPh)4]MeCN _chemical_formula_sum 'C68 H103 B2 Fe6 Mo2 N16 S12' _chemical_formula_weight 2077.98 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' 'B' 'B' 0.0013 0.0007 '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' 'Fe' 'Fe' 0.3463 0.8444 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.333(3) _cell_length_b 13.935(3) _cell_length_c 15.016(3) _cell_angle_alpha 84.84(3) _cell_angle_beta 72.41(3) _cell_angle_gamma 70.77(3) _cell_volume 2322.6(8) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark green ' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1065 _exptl_absorpt_coefficient_mu 1.485 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ? _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_% none _diffrn_reflns_number 14160 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.1790 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9083 _reflns_number_gt 4135 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0599P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9083 _refine_ls_number_parameters 575 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1365 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.810 _refine_ls_shift/su_max 3.593 _refine_ls_shift/su_mean 0.368 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 C22 C 0.388(2) 0.727(2) 0.1863(17) 0.108(8) Uani 0.50 1 d P . . H22 H 0.3859 0.7934 0.1711 0.129 Uiso 0.50 1 calc PR . . C23 C 0.292(2) 0.7029(15) 0.248(2) 0.136(11) Uani 0.50 1 d P . . H23 H 0.2199 0.7559 0.2676 0.163 Uiso 0.50 1 calc PR . . C24 C 0.292(2) 0.6068(16) 0.2847(17) 0.105(9) Uani 0.50 1 d P . . H24 H 0.2237 0.5986 0.3277 0.126 Uiso 0.50 1 calc PR . . C25 C 0.468(2) 0.6599(16) 0.1560(17) 0.120(10) Uani 0.50 1 d P . . H25 H 0.5291 0.6742 0.1090 0.144 Uiso 0.50 1 calc PR . . Mo1 Mo 0.10078(6) 0.27369(5) 0.32511(5) 0.03668(19) Uani 1 1 d . . . Fe1 Fe 0.00540(9) 0.43747(7) 0.43853(7) 0.0371(3) Uani 1 1 d . . . Fe2 Fe 0.14471(9) 0.26455(8) 0.49341(7) 0.0393(3) Uani 1 1 d . . . Fe3 Fe 0.24425(10) 0.37241(8) 0.35443(8) 0.0434(3) Uani 1 1 d . . . S1 S -0.03898(17) 0.29241(14) 0.47641(13) 0.0390(5) Uani 1 1 d . . . S2 S 0.09696(18) 0.44324(14) 0.28538(14) 0.0426(5) Uani 1 1 d . . . S3 S 0.28669(18) 0.20183(14) 0.35787(14) 0.0457(5) Uani 1 1 d . . . S4 S -0.15666(17) 0.57437(14) 0.48800(14) 0.0410(5) Uani 1 1 d . . . S5 S 0.2073(2) 0.14544(16) 0.59670(17) 0.0599(6) Uani 1 1 d . . . S6 S 0.4222(2) 0.4057(2) 0.2916(2) 0.0861(9) Uani 1 1 d . . . N1 N 0.0908(5) 0.1170(5) 0.3253(5) 0.0450(17) Uani 1 1 d . . . N2 N 0.0711(5) 0.0787(5) 0.2521(4) 0.0442(16) Uani 1 1 d . . . N3 N -0.0563(6) 0.3047(5) 0.2688(4) 0.0415(16) Uani 1 1 d . . . N4 N -0.0574(6) 0.2409(5) 0.2051(4) 0.0439(16) Uani 1 1 d . . . N5 N 0.1999(6) 0.2332(5) 0.1748(4) 0.0459(17) Uani 1 1 d . . . N6 N 0.1631(6) 0.1803(5) 0.1240(4) 0.0484(17) Uani 1 1 d . . . N7 N 0.5744(7) 0.2278(7) 0.5334(6) 0.086(3) Uani 1 1 d . . . N8 N 1.0000 0.5000 1.0000 0.064(3) Uani 1 2 d S . . N9 N 0.3798(17) 0.9781(14) 0.1719(11) 0.103(6) Uani 0.50 1 d PD . . B1 B 0.0506(9) 0.1466(8) 0.1684(7) 0.049(3) Uani 1 1 d . . . H1 H 0.036(6) 0.110(5) 0.123(5) 0.059 Uiso 1 1 calc . . . C1 C 0.0973(7) 0.0444(6) 0.3904(6) 0.049(2) Uani 1 1 d . . . H1A H 0.1101 0.0496 0.4475 0.058 Uiso 1 1 calc R . . C2 C 0.0819(7) -0.0405(6) 0.3590(6) 0.055(2) Uani 1 1 d . . . H2 H 0.0836 -0.1016 0.3900 0.066 Uiso 1 1 calc R . . C3 C 0.0639(7) -0.0152(6) 0.2737(6) 0.053(2) Uani 1 1 d . . . H3 H 0.0491 -0.0562 0.2363 0.063 Uiso 1 1 calc R . . C4 C -0.1636(7) 0.3746(6) 0.2895(6) 0.050(2) Uani 1 1 d . . . H4 H -0.1871 0.4286 0.3307 0.060 Uiso 1 1 calc R . . C5 C -0.2357(8) 0.3581(7) 0.2433(6) 0.060(2) Uani 1 1 d . . . H5 H -0.3147 0.3962 0.2469 0.071 Uiso 1 1 calc R . . C6 C -0.1657(8) 0.2732(7) 0.1906(6) 0.058(2) Uani 1 1 d . . . H6 H -0.1894 0.2423 0.1507 0.070 Uiso 1 1 calc R . . C7 C 0.2979(7) 0.2497(6) 0.1184(6) 0.055(2) Uani 1 1 d . . . H7 H 0.3411 0.2850 0.1352 0.066 Uiso 1 1 calc R . . C8 C 0.3264(8) 0.2078(7) 0.0325(6) 0.062(3) Uani 1 1 d . . . H8 H 0.3913 0.2084 -0.0188 0.075 Uiso 1 1 calc R . . C9 C 0.2401(8) 0.1648(7) 0.0372(6) 0.065(3) Uani 1 1 d . . . H9 H 0.2353 0.1306 -0.0112 0.078 Uiso 1 1 calc R . . C10 C 0.1172(9) 0.1686(7) 0.7050(8) 0.074(3) Uani 1 1 d . . . C11 C 0.1439(11) 0.1060(10) 0.7802(8) 0.100(4) Uani 1 1 d . . . H11 H 0.2166 0.0535 0.7671 0.119 Uiso 1 1 calc R . . C12 C 0.0725(17) 0.1159(15) 0.8696(9) 0.138(8) Uani 1 1 d . . . H12 H 0.0987 0.0712 0.9142 0.165 Uiso 1 1 calc R . . C13 C -0.0348(19) 0.1881(17) 0.8959(11) 0.155(10) Uani 1 1 d . . . H13 H -0.0850 0.1923 0.9567 0.186 Uiso 1 1 calc R . . C14 C -0.0690(14) 0.2597(12) 0.8243(10) 0.144(7) Uani 1 1 d . . . H14 H -0.1411 0.3128 0.8390 0.172 Uiso 1 1 calc R . . C15 C 0.0112(11) 0.2467(9) 0.7302(7) 0.090(4) Uani 1 1 d . . . H15 H -0.0101 0.2931 0.6850 0.108 Uiso 1 1 calc R . . C28 C 0.4437(8) 0.2830(7) 0.5516(7) 0.076(3) Uani 1 1 d . . . H28A H 0.4063 0.2384 0.5353 0.092 Uiso 1 1 calc R . . H28B H 0.4336 0.3413 0.5108 0.092 Uiso 1 1 calc R . . C29 C 0.3775(10) 0.3200(8) 0.6528(7) 0.108(4) Uani 1 1 d . . . H29A H 0.3882 0.2632 0.6942 0.162 Uiso 1 1 calc R . . H29B H 0.2935 0.3514 0.6593 0.162 Uiso 1 1 calc R . . H29C H 0.4093 0.3685 0.6682 0.162 Uiso 1 1 calc R . . C30 C 0.6011(10) 0.1371(8) 0.5930(8) 0.093(4) Uani 1 1 d . . . H30A H 0.5710 0.1585 0.6581 0.112 Uiso 1 1 calc R . . H30B H 0.6873 0.1056 0.5783 0.112 Uiso 1 1 calc R . . C31 C 0.5458(12) 0.0604(9) 0.5796(11) 0.154(6) Uani 1 1 d . . . H31A H 0.4649 0.0774 0.6196 0.230 Uiso 1 1 calc R . . H31B H 0.5915 -0.0059 0.5948 0.230 Uiso 1 1 calc R . . H31C H 0.5457 0.0608 0.5156 0.230 Uiso 1 1 calc R . . C32 C 0.6399(11) 0.2994(12) 0.5577(10) 0.142(6) Uani 1 1 d . . . H32A H 0.6182 0.3055 0.6251 0.171 Uiso 1 1 calc R . . H32B H 0.7258 0.2657 0.5358 0.171 Uiso 1 1 calc R . . C33 C 0.6126(15) 0.4077(11) 0.5168(13) 0.221(11) Uani 1 1 d . . . H33A H 0.6264 0.4035 0.4506 0.332 Uiso 1 1 calc R . . H33B H 0.6640 0.4406 0.5288 0.332 Uiso 1 1 calc R . . H33C H 0.5303 0.4461 0.5456 0.332 Uiso 1 1 calc R . . C34 C 0.6305(11) 0.2016(8) 0.4312(8) 0.121(5) Uani 1 1 d . . . H34A H 0.6182 0.2641 0.3958 0.146 Uiso 1 1 calc R . . H34B H 0.5893 0.1615 0.4132 0.146 Uiso 1 1 calc R . . C35 C 0.7665(9) 0.1420(7) 0.4042(8) 0.124(5) Uani 1 1 d . . . H35A H 0.8082 0.1810 0.4217 0.186 Uiso 1 1 calc R . . H35B H 0.7961 0.1299 0.3379 0.186 Uiso 1 1 calc R . . H35C H 0.7794 0.0782 0.4361 0.186 Uiso 1 1 calc R . . C36 C 0.8972(17) 0.5551(14) 0.9548(14) 0.070(5) Uani 0.50 1 d P . 1 C37 C 0.8031(10) 0.4938(9) 0.9837(8) 0.104(4) Uani 1 1 d . A 1 H37A H 0.8450 0.4225 0.9724 0.156 Uiso 1 1 calc R A 1 H37B H 0.7475 0.5168 0.9473 0.156 Uiso 1 1 calc R A 1 H37C H 0.7602 0.5051 1.0489 0.156 Uiso 1 1 calc R A 1 C40 C 1.1297(10) 0.3898(8) 0.8547(7) 0.108(4) Uani 1 1 d . . 1 H40A H 1.0865 0.4505 0.8286 0.162 Uiso 1 1 calc R . 1 H40B H 1.1264 0.3314 0.8275 0.162 Uiso 1 1 calc R . 1 H40C H 1.2119 0.3871 0.8415 0.162 Uiso 1 1 calc R . 1 C41 C 1.0680(18) 0.3905(13) 0.9698(13) 0.070(6) Uani 0.50 1 d P . 1 C38 C 0.9224(18) 0.4354(14) 1.0286(15) 0.083(7) Uani 0.50 1 d P . 2 H38A H 0.9602 0.3624 1.0212 0.100 Uiso 0.50 1 calc PR . 2 H38B H 0.8435 0.4609 1.0191 0.100 Uiso 0.50 1 calc PR . 2 C39 C 1.052(2) 0.5082(15) 0.8948(11) 0.089(7) Uani 0.50 1 d P . 2 H39A H 0.9995 0.5488 0.8595 0.106 Uiso 0.50 1 calc PR . 2 H39B H 1.1165 0.4501 0.8616 0.106 Uiso 0.50 1 calc PR . 2 C42 C 0.4841(17) 0.948(3) 0.1686(14) 0.24(5) Uani 0.50 1 d PD . . C43 C 0.6073(17) 0.887(2) 0.1834(15) 0.30(4) Uani 0.50 1 d PD . . H43A H 0.5956 0.8467 0.2386 0.448 Uiso 0.50 1 calc PR . . H43B H 0.6471 0.9335 0.1905 0.448 Uiso 0.50 1 calc PR . . H43C H 0.6557 0.8435 0.1303 0.448 Uiso 0.50 1 calc PR . . C16 C 0.5104(18) 0.335(2) 0.1976(18) 0.102(8) Uani 0.50 1 d P . . C17 C 0.655(3) 0.185(3) 0.063(3) 0.173(14) Uani 0.50 1 d P . . H17 H 0.7091 0.1417 0.0136 0.207 Uiso 0.50 1 calc PR . . C18 C 0.635(3) 0.147(3) 0.125(2) 0.109(10) Uani 0.50 1 d P . . H18 H 0.6623 0.0763 0.1294 0.131 Uiso 0.50 1 calc PR . . C19 C 0.561(2) 0.215(2) 0.2052(18) 0.107(8) Uani 0.50 1 d P . . H19 H 0.5417 0.1856 0.2638 0.128 Uiso 0.50 1 calc PR . . C20 C 0.622(2) 0.280(3) 0.0380(17) 0.152(12) Uani 0.50 1 d P . . H20 H 0.6469 0.2925 -0.0256 0.183 Uiso 0.50 1 calc PR . . C21 C 0.539(2) 0.381(2) 0.106(2) 0.157(11) Uani 0.50 1 d P . . H21 H 0.5173 0.4491 0.0898 0.188 Uiso 0.50 1 calc PR . . C26 C 0.4002(14) 0.5197(12) 0.2552(14) 0.060(5) Uani 0.50 1 d P . . C27 C 0.487(2) 0.557(2) 0.1797(19) 0.131(10) Uani 0.50 1 d P . . H27 H 0.5583 0.5091 0.1467 0.157 Uiso 0.50 1 calc PR . . 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 C22 0.10(2) 0.15(2) 0.11(2) 0.015(18) -0.041(16) -0.089(19) C23 0.12(2) 0.020(12) 0.27(4) -0.020(17) -0.11(2) 0.024(13) C24 0.091(18) 0.072(14) 0.15(2) -0.020(15) 0.007(15) -0.049(13) C25 0.095(18) 0.041(13) 0.14(2) 0.009(14) 0.070(15) -0.010(12) Mo1 0.0472(4) 0.0281(4) 0.0343(4) 0.0006(3) -0.0102(3) -0.0130(3) Fe1 0.0460(7) 0.0266(6) 0.0393(6) -0.0002(5) -0.0162(5) -0.0087(5) Fe2 0.0483(7) 0.0279(6) 0.0395(7) 0.0017(5) -0.0147(5) -0.0080(5) Fe3 0.0481(7) 0.0364(6) 0.0472(7) 0.0012(5) -0.0138(5) -0.0159(5) S1 0.0473(12) 0.0315(10) 0.0362(11) 0.0006(9) -0.0092(9) -0.0124(9) S2 0.0583(13) 0.0340(11) 0.0407(12) 0.0064(9) -0.0183(10) -0.0194(10) S3 0.0462(13) 0.0357(11) 0.0485(13) -0.0031(10) -0.0093(10) -0.0074(9) S4 0.0465(12) 0.0291(10) 0.0480(12) 0.0000(9) -0.0193(9) -0.0078(9) S5 0.0722(17) 0.0430(13) 0.0707(17) 0.0220(12) -0.0343(13) -0.0196(12) S6 0.0493(16) 0.0785(19) 0.118(2) 0.0220(18) -0.0084(15) -0.0237(14) N1 0.050(4) 0.033(4) 0.046(4) -0.003(3) -0.005(3) -0.014(3) N2 0.055(4) 0.035(4) 0.042(4) -0.003(3) -0.009(3) -0.016(3) N3 0.052(4) 0.040(4) 0.036(4) 0.000(3) -0.012(3) -0.020(3) N4 0.050(5) 0.047(4) 0.040(4) 0.003(3) -0.014(3) -0.023(3) N5 0.056(5) 0.042(4) 0.043(4) -0.005(3) -0.011(3) -0.022(3) N6 0.067(5) 0.039(4) 0.040(4) 0.001(3) -0.014(4) -0.020(3) N7 0.067(6) 0.096(7) 0.072(6) 0.016(5) -0.005(5) -0.015(5) N8 0.083(8) 0.060(7) 0.057(7) 0.014(6) -0.022(6) -0.035(6) N9 0.093(16) 0.119(14) 0.051(10) 0.008(10) -0.014(10) 0.018(12) B1 0.064(8) 0.054(7) 0.035(6) -0.001(5) -0.012(5) -0.029(6) C1 0.058(6) 0.033(5) 0.048(5) -0.006(4) -0.009(4) -0.011(4) C2 0.069(6) 0.032(5) 0.059(6) 0.004(4) -0.012(5) -0.017(4) C3 0.066(6) 0.033(5) 0.056(6) -0.008(4) -0.005(5) -0.022(4) C4 0.050(6) 0.044(5) 0.057(6) 0.006(4) -0.016(4) -0.016(4) C5 0.052(6) 0.071(6) 0.058(6) 0.000(5) -0.025(5) -0.015(5) C6 0.060(6) 0.072(6) 0.058(6) 0.007(5) -0.026(5) -0.036(5) C7 0.052(6) 0.069(6) 0.046(5) -0.004(5) -0.007(4) -0.028(5) C8 0.062(6) 0.078(7) 0.038(5) -0.003(5) 0.011(4) -0.032(5) C9 0.084(7) 0.067(6) 0.034(5) -0.015(5) -0.002(5) -0.023(5) C10 0.069(7) 0.049(6) 0.114(9) 0.000(6) -0.037(6) -0.023(5) C11 0.135(10) 0.132(10) 0.073(8) 0.041(8) -0.065(8) -0.075(9) C12 0.219(19) 0.23(2) 0.050(9) 0.049(11) -0.065(11) -0.173(18) C13 0.25(2) 0.22(2) 0.065(10) -0.016(13) -0.007(14) -0.19(2) C14 0.181(15) 0.136(14) 0.104(11) -0.067(11) 0.050(11) -0.103(12) C15 0.128(10) 0.086(8) 0.062(7) -0.014(6) -0.006(7) -0.056(8) C28 0.050(6) 0.064(6) 0.098(8) 0.024(6) -0.026(6) 0.002(5) C29 0.101(9) 0.111(9) 0.072(8) 0.005(7) -0.023(7) 0.014(7) C30 0.095(9) 0.081(8) 0.082(8) 0.021(7) -0.029(7) -0.002(7) C31 0.139(13) 0.076(9) 0.247(19) 0.027(11) -0.081(12) -0.020(9) C32 0.103(11) 0.200(17) 0.147(13) -0.028(13) -0.026(9) -0.081(11) C33 0.25(2) 0.087(11) 0.27(2) -0.014(13) 0.045(17) -0.086(12) C34 0.144(12) 0.067(8) 0.088(9) 0.003(7) 0.032(8) -0.009(7) C35 0.091(9) 0.052(7) 0.150(11) -0.010(7) 0.062(8) -0.008(6) C36 0.079(15) 0.064(12) 0.080(15) 0.031(11) -0.046(12) -0.027(11) C37 0.099(9) 0.126(10) 0.104(10) 0.010(8) -0.048(7) -0.044(8) C40 0.135(11) 0.093(9) 0.076(8) -0.029(7) -0.014(7) -0.017(8) C41 0.091(16) 0.046(11) 0.061(13) -0.021(10) 0.007(11) -0.027(11) C38 0.082(16) 0.047(12) 0.14(2) 0.027(13) -0.056(14) -0.035(11) C39 0.17(2) 0.078(14) 0.015(9) -0.001(10) -0.020(11) -0.046(15) C42 0.09(3) 0.43(8) 0.000(11) -0.03(2) 0.008(15) 0.15(4) C43 0.48(8) 0.44(8) 0.05(2) -0.12(4) 0.11(4) -0.39(8) C16 0.044(14) 0.17(2) 0.12(2) -0.009(19) -0.025(13) -0.063(16) C17 0.12(2) 0.27(4) 0.20(4) 0.03(3) -0.08(2) -0.14(3) C18 0.10(2) 0.17(3) 0.07(2) 0.01(2) -0.036(18) -0.060(19) C19 0.076(16) 0.20(3) 0.075(19) 0.007(19) -0.029(14) -0.072(17) C20 0.10(2) 0.39(4) 0.015(15) -0.05(2) 0.030(13) -0.16(2) C21 0.15(2) 0.25(3) 0.15(3) 0.07(3) -0.05(2) -0.17(2) C26 0.027(10) 0.040(10) 0.114(16) -0.021(10) -0.026(10) -0.001(8) C27 0.044(16) 0.16(3) 0.15(3) 0.00(2) 0.010(15) -0.013(16) _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 C22 C25 1.12(3) . ? C22 C23 1.39(3) . ? C23 C24 1.40(3) . ? C24 C26 1.46(2) . ? C25 C27 1.41(3) . ? Mo1 N1 2.226(6) . ? Mo1 N5 2.239(6) . ? Mo1 N3 2.242(6) . ? Mo1 S3 2.363(2) . ? Mo1 S2 2.373(2) . ? Mo1 S1 2.376(2) . ? Mo1 Fe1 2.6857(15) . ? Mo1 Fe3 2.7203(14) . ? Mo1 Fe2 2.7241(14) . ? Fe1 S2 2.242(2) . ? Fe1 S4 2.243(2) . ? Fe1 S1 2.246(2) . ? Fe1 S4 2.394(2) 2_566 ? Fe1 Fe1 2.596(2) 2_566 ? Fe1 Fe2 2.6850(18) . ? Fe1 Fe3 2.7005(18) . ? Fe2 S1 2.258(2) . ? Fe2 S3 2.265(2) . ? Fe2 S5 2.274(3) . ? Fe2 S4 2.344(2) 2_566 ? Fe2 Fe3 2.6878(18) . ? Fe3 S3 2.259(2) . ? Fe3 S2 2.263(2) . ? Fe3 S6 2.293(3) . ? Fe3 S4 2.358(2) 2_566 ? S4 Fe2 2.344(2) 2_566 ? S4 Fe3 2.358(2) 2_566 ? S4 Fe1 2.394(2) 2_566 ? S5 C10 1.658(11) . ? S6 C26 1.597(17) . ? S6 C16 1.66(2) . ? N1 C1 1.343(9) . ? N1 N2 1.380(8) . ? N2 C3 1.345(9) . ? N2 B1 1.535(12) . ? N3 C4 1.325(9) . ? N3 N4 1.369(8) . ? N4 C6 1.340(10) . ? N4 B1 1.529(12) . ? N5 C7 1.327(9) . ? N5 N6 1.364(8) . ? N6 C9 1.347(9) . ? N6 B1 1.552(11) . ? N7 C30 1.486(12) . ? N7 C28 1.490(11) . ? N7 C34 1.503(12) . ? N7 C32 1.599(14) . ? N8 C38 1.470(17) 2_767 ? N8 C38 1.470(17) . ? N8 C41 1.513(17) . ? N8 C41 1.513(17) 2_767 ? N8 C39 1.525(16) . ? N8 C39 1.525(15) 2_767 ? N8 C36 1.563(18) . ? N8 C36 1.563(18) 2_767 ? N9 C42 1.202(6) . ? C1 C2 1.400(10) . ? C2 C3 1.361(11) . ? C4 C5 1.364(11) . ? C5 C6 1.362(11) . ? C7 C8 1.361(10) . ? C8 C9 1.367(11) . ? C10 C15 1.369(13) . ? C10 C11 1.415(14) . ? C11 C12 1.355(16) . ? C12 C13 1.34(2) . ? C13 C14 1.46(2) . ? C14 C15 1.446(14) . ? C28 C29 1.535(12) . ? C30 C31 1.499(14) . ? C32 C33 1.546(19) . ? C34 C35 1.549(14) . ? C36 C37 1.596(19) . ? C36 C41 1.64(2) 2_767 ? C40 C41 1.664(19) . ? C41 C36 1.64(2) 2_767 ? C38 C39 1.61(2) 2_767 ? C39 C38 1.61(2) 2_767 ? C42 C43 1.548(6) . ? C16 C21 1.46(3) . ? C16 C19 1.60(3) . ? C17 C18 1.03(4) . ? C17 C20 1.31(4) . ? C18 C19 1.47(4) . ? C20 C21 1.65(4) . ? C26 C27 1.49(3) . ? 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 C25 C22 C23 115(3) . . ? C24 C23 C22 126(2) . . ? C23 C24 C26 119.8(19) . . ? C22 C25 C27 129(2) . . ? N1 Mo1 N5 81.4(2) . . ? N1 Mo1 N3 80.0(2) . . ? N5 Mo1 N3 80.9(2) . . ? N1 Mo1 S3 87.98(18) . . ? N5 Mo1 S3 87.57(18) . . ? N3 Mo1 S3 164.44(16) . . ? N1 Mo1 S2 163.92(19) . . ? N5 Mo1 S2 87.00(17) . . ? N3 Mo1 S2 87.19(16) . . ? S3 Mo1 S2 102.67(8) . . ? N1 Mo1 S1 86.25(16) . . ? N5 Mo1 S1 163.85(16) . . ? N3 Mo1 S1 86.80(16) . . ? S3 Mo1 S1 102.40(8) . . ? S2 Mo1 S1 102.87(8) . . ? N1 Mo1 Fe1 138.49(16) . . ? N5 Mo1 Fe1 139.17(16) . . ? N3 Mo1 Fe1 95.75(16) . . ? S3 Mo1 Fe1 99.80(6) . . ? S2 Mo1 Fe1 52.18(6) . . ? S1 Mo1 Fe1 52.24(6) . . ? N1 Mo1 Fe3 140.12(17) . . ? N5 Mo1 Fe3 96.86(16) . . ? N3 Mo1 Fe3 139.37(15) . . ? S3 Mo1 Fe3 52.19(6) . . ? S2 Mo1 Fe3 52.23(6) . . ? S1 Mo1 Fe3 99.28(6) . . ? Fe1 Mo1 Fe3 59.93(4) . . ? N1 Mo1 Fe2 97.15(18) . . ? N5 Mo1 Fe2 139.82(17) . . ? N3 Mo1 Fe2 138.77(15) . . ? S3 Mo1 Fe2 52.29(6) . . ? S2 Mo1 Fe2 98.91(6) . . ? S1 Mo1 Fe2 52.02(6) . . ? Fe1 Mo1 Fe2 59.51(4) . . ? Fe3 Mo1 Fe2 59.17(4) . . ? S2 Fe1 S4 112.22(9) . . ? S2 Fe1 S1 111.66(8) . . ? S4 Fe1 S1 111.63(8) . . ? S2 Fe1 S4 104.38(8) . 2_566 ? S4 Fe1 S4 112.01(7) . 2_566 ? S1 Fe1 S4 104.46(8) . 2_566 ? S2 Fe1 Fe1 123.77(8) . 2_566 ? S4 Fe1 Fe1 58.77(7) . 2_566 ? S1 Fe1 Fe1 123.29(8) . 2_566 ? S4 Fe1 Fe1 53.24(6) 2_566 2_566 ? S2 Fe1 Fe2 103.52(8) . . ? S4 Fe1 Fe2 144.20(7) . . ? S1 Fe1 Fe2 53.63(6) . . ? S4 Fe1 Fe2 54.60(6) 2_566 . ? Fe1 Fe1 Fe2 99.59(7) 2_566 . ? S2 Fe1 Mo1 56.71(6) . . ? S4 Fe1 Mo1 144.11(7) . . ? S1 Fe1 Mo1 56.76(6) . . ? S4 Fe1 Mo1 103.88(6) 2_566 . ? Fe1 Fe1 Mo1 157.12(7) 2_566 . ? Fe2 Fe1 Mo1 60.96(4) . . ? S2 Fe1 Fe3 53.53(7) . . ? S4 Fe1 Fe3 144.98(7) . . ? S1 Fe1 Fe3 103.32(7) . . ? S4 Fe1 Fe3 54.73(6) 2_566 . ? Fe1 Fe1 Fe3 100.08(7) 2_566 . ? Fe2 Fe1 Fe3 59.88(5) . . ? Mo1 Fe1 Fe3 60.67(4) . . ? S1 Fe2 S3 109.45(9) . . ? S1 Fe2 S5 118.87(9) . . ? S3 Fe2 S5 101.27(9) . . ? S1 Fe2 S4 105.72(8) . 2_566 ? S3 Fe2 S4 105.24(8) . 2_566 ? S5 Fe2 S4 115.37(9) . 2_566 ? S1 Fe2 Fe1 53.19(6) . . ? S3 Fe2 Fe1 102.43(8) . . ? S5 Fe2 Fe1 156.27(8) . . ? S4 Fe2 Fe1 56.37(6) 2_566 . ? S1 Fe2 Fe3 103.36(7) . . ? S3 Fe2 Fe3 53.44(6) . . ? S5 Fe2 Fe3 136.91(8) . . ? S4 Fe2 Fe3 55.37(6) 2_566 . ? Fe1 Fe2 Fe3 60.35(5) . . ? S1 Fe2 Mo1 56.02(6) . . ? S3 Fe2 Mo1 55.62(6) . . ? S5 Fe2 Mo1 138.90(8) . . ? S4 Fe2 Mo1 104.13(7) 2_566 . ? Fe1 Fe2 Mo1 59.54(4) . . ? Fe3 Fe2 Mo1 60.35(4) . . ? S3 Fe3 S2 109.72(9) . . ? S3 Fe3 S6 107.42(10) . . ? S2 Fe3 S6 117.69(10) . . ? S3 Fe3 S4 104.99(9) . 2_566 ? S2 Fe3 S4 104.92(8) . 2_566 ? S6 Fe3 S4 111.42(11) . 2_566 ? S3 Fe3 Fe2 53.66(6) . . ? S2 Fe3 Fe2 102.85(7) . . ? S6 Fe3 Fe2 139.45(10) . . ? S4 Fe3 Fe2 54.89(6) 2_566 . ? S3 Fe3 Fe1 102.13(7) . . ? S2 Fe3 Fe1 52.82(6) . . ? S6 Fe3 Fe1 150.24(9) . . ? S4 Fe3 Fe1 56.01(6) 2_566 . ? Fe2 Fe3 Fe1 59.78(5) . . ? S3 Fe3 Mo1 55.73(6) . . ? S2 Fe3 Mo1 55.97(6) . . ? S6 Fe3 Mo1 144.18(10) . . ? S4 Fe3 Mo1 103.86(7) 2_566 . ? Fe2 Fe3 Mo1 60.49(4) . . ? Fe1 Fe3 Mo1 59.40(4) . . ? Fe1 S1 Fe2 73.18(7) . . ? Fe1 S1 Mo1 71.00(7) . . ? Fe2 S1 Mo1 71.95(7) . . ? Fe1 S2 Fe3 73.65(8) . . ? Fe1 S2 Mo1 71.11(7) . . ? Fe3 S2 Mo1 71.81(7) . . ? Fe3 S3 Fe2 72.91(8) . . ? Fe3 S3 Mo1 72.08(7) . . ? Fe2 S3 Mo1 72.09(7) . . ? Fe1 S4 Fe2 123.11(9) . 2_566 ? Fe1 S4 Fe3 123.88(10) . 2_566 ? Fe2 S4 Fe3 69.74(7) 2_566 2_566 ? Fe1 S4 Fe1 67.99(7) . 2_566 ? Fe2 S4 Fe1 69.03(7) 2_566 2_566 ? Fe3 S4 Fe1 69.26(7) 2_566 2_566 ? C10 S5 Fe2 113.1(4) . . ? C26 S6 C16 104.0(13) . . ? C26 S6 Fe3 111.2(6) . . ? C16 S6 Fe3 113.2(7) . . ? C1 N1 N2 106.7(6) . . ? C1 N1 Mo1 130.9(5) . . ? N2 N1 Mo1 122.3(5) . . ? C3 N2 N1 108.9(7) . . ? C3 N2 B1 131.1(7) . . ? N1 N2 B1 119.7(6) . . ? C4 N3 N4 105.6(6) . . ? C4 N3 Mo1 132.5(5) . . ? N4 N3 Mo1 121.7(5) . . ? C6 N4 N3 108.5(6) . . ? C6 N4 B1 130.7(7) . . ? N3 N4 B1 120.6(7) . . ? C7 N5 N6 106.8(6) . . ? C7 N5 Mo1 131.9(5) . . ? N6 N5 Mo1 121.3(4) . . ? C9 N6 N5 108.6(6) . . ? C9 N6 B1 130.3(7) . . ? N5 N6 B1 121.1(6) . . ? C30 N7 C28 113.4(7) . . ? C30 N7 C34 111.9(8) . . ? C28 N7 C34 109.8(9) . . ? C30 N7 C32 104.7(10) . . ? C28 N7 C32 110.2(9) . . ? C34 N7 C32 106.5(8) . . ? C38 N8 C38 180.000(3) 2_767 . ? C38 N8 C41 111.8(10) 2_767 . ? C38 N8 C41 68.2(10) . . ? C38 N8 C41 68.2(10) 2_767 2_767 ? C38 N8 C41 111.8(10) . 2_767 ? C41 N8 C41 180.0(14) . 2_767 ? C38 N8 C39 64.8(10) 2_767 . ? C38 N8 C39 115.2(10) . . ? C41 N8 C39 77.1(10) . . ? C41 N8 C39 102.9(10) 2_767 . ? C38 N8 C39 115.2(10) 2_767 2_767 ? C38 N8 C39 64.8(10) . 2_767 ? C41 N8 C39 102.9(10) . 2_767 ? C41 N8 C39 77.1(10) 2_767 2_767 ? C39 N8 C39 180.000(4) . 2_767 ? C38 N8 C36 102.1(10) 2_767 . ? C38 N8 C36 77.9(10) . . ? C41 N8 C36 115.4(10) . . ? C41 N8 C36 64.6(10) 2_767 . ? C39 N8 C36 70.1(11) . . ? C39 N8 C36 109.9(11) 2_767 . ? C38 N8 C36 77.9(10) 2_767 2_767 ? C38 N8 C36 102.1(10) . 2_767 ? C41 N8 C36 64.6(10) . 2_767 ? C41 N8 C36 115.4(10) 2_767 2_767 ? C39 N8 C36 109.9(11) . 2_767 ? C39 N8 C36 70.1(11) 2_767 2_767 ? C36 N8 C36 180.000(4) . 2_767 ? N4 B1 N2 108.0(7) . . ? N4 B1 N6 108.7(7) . . ? N2 B1 N6 108.0(8) . . ? N1 C1 C2 109.4(8) . . ? C3 C2 C1 105.8(7) . . ? N2 C3 C2 109.1(7) . . ? N3 C4 C5 112.1(8) . . ? C6 C5 C4 104.2(8) . . ? N4 C6 C5 109.6(8) . . ? N5 C7 C8 110.5(7) . . ? C7 C8 C9 105.9(7) . . ? N6 C9 C8 108.2(7) . . ? C15 C10 C11 114.0(11) . . ? C15 C10 S5 124.4(9) . . ? C11 C10 S5 121.7(9) . . ? C12 C11 C10 125.5(15) . . ? C13 C12 C11 122.2(19) . . ? C12 C13 C14 116.7(16) . . ? C15 C14 C13 118.9(16) . . ? C10 C15 C14 122.5(13) . . ? N7 C28 C29 114.8(9) . . ? N7 C30 C31 112.3(10) . . ? C33 C32 N7 116.6(13) . . ? N7 C34 C35 114.4(11) . . ? N8 C36 C37 107.2(11) . . ? N8 C36 C41 56.2(10) . 2_767 ? C37 C36 C41 123.9(14) . 2_767 ? N8 C41 C36 59.2(9) . 2_767 ? N8 C41 C40 107.3(12) . . ? C36 C41 C40 124.0(13) 2_767 . ? N8 C38 C39 59.3(9) . 2_767 ? N8 C39 C38 56.0(8) . 2_767 ? N9 C42 C43 164(3) . . ? C21 C16 C19 118(2) . . ? C21 C16 S6 121(3) . . ? C19 C16 S6 120(2) . . ? C18 C17 C20 134(5) . . ? C17 C18 C19 114(4) . . ? C18 C19 C16 124(2) . . ? C17 C20 C21 128(3) . . ? C16 C21 C20 102(2) . . ? C24 C26 C27 106.3(18) . . ? C24 C26 S6 127.9(15) . . ? C27 C26 S6 125.7(16) . . ? C25 C27 C26 123(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.879 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.112 #--------------------------------END data_(Et4N)3[Tp2Mo2Fe6S9(SPh)2]5.5MeCN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ' not measure ' _chemical_formula_moiety (Et4N)3[Tp2Mo2Fe6S9(SPh)2]5.5MeCN _chemical_formula_sum 'C65 H106.50 B2 Fe6 Mo2 N20.50 S11' _chemical_formula_weight 2076.47 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' 'B' 'B' 0.0013 0.0007 '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' 'Fe' 'Fe' 0.3463 0.8444 '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 P21/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 18.114(3) _cell_length_b 17.997(3) _cell_length_c 27.898(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.602(4) _cell_angle_gamma 90.00 _cell_volume 9091(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark black ' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4264 _exptl_absorpt_coefficient_mu 1.497 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ? _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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 29208 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.1891 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15216 _reflns_number_gt 6591 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0364P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15216 _refine_ls_number_parameters 996 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 0.850 _refine_ls_restrained_S_all 0.850 _refine_ls_shift/su_max 7.135 _refine_ls_shift/su_mean 0.160 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 0.23340(4) 0.06230(4) 0.45911(3) 0.0352(2) Uani 1 1 d . . . Mo2 Mo 0.26426(4) 0.42543(4) 0.58062(3) 0.0357(2) Uani 1 1 d . . . Fe1 Fe 0.22591(6) 0.19262(7) 0.41008(4) 0.0383(3) Uani 1 1 d . . . Fe2 Fe 0.31816(6) 0.17926(7) 0.48777(4) 0.0357(3) Uani 1 1 d . . . Fe3 Fe 0.16734(6) 0.18388(7) 0.49674(4) 0.0349(3) Uani 1 1 d . . . Fe4 Fe 0.25509(6) 0.41460(7) 0.48416(5) 0.0409(3) Uani 1 1 d . . . Fe5 Fe 0.33071(6) 0.30970(7) 0.53475(4) 0.0362(3) Uani 1 1 d . . . Fe6 Fe 0.17896(6) 0.31663(7) 0.54053(4) 0.0362(3) Uani 1 1 d . . . S1 S 0.32876(11) 0.12155(13) 0.41644(8) 0.0422(6) Uani 1 1 d . . . S2 S 0.12633(11) 0.12520(12) 0.42968(8) 0.0388(6) Uani 1 1 d . . . S3 S 0.24820(11) 0.11015(12) 0.53708(8) 0.0368(6) Uani 1 1 d . . . S4 S 0.36199(11) 0.42982(13) 0.52599(8) 0.0422(6) Uani 1 1 d . . . S5 S 0.15701(11) 0.43882(13) 0.53023(8) 0.0421(6) Uani 1 1 d . . . S6 S 0.26250(11) 0.29840(12) 0.60113(8) 0.0381(6) Uani 1 1 d . . . S7 S 0.24356(11) 0.28492(12) 0.47053(9) 0.0382(6) Uani 1 1 d . . . S8 S 0.41966(11) 0.22690(13) 0.52268(9) 0.0429(6) Uani 1 1 d . . . S9 S 0.08226(11) 0.24006(13) 0.53968(9) 0.0453(7) Uani 1 1 d . . . S10 S 0.20739(14) 0.27840(15) 0.35049(10) 0.0614(8) Uani 1 1 d . . . S11 S 0.25848(16) 0.46333(19) 0.40914(11) 0.0847(10) Uani 1 1 d . . . N1 N 0.2219(4) -0.0158(4) 0.3965(3) 0.047(2) Uani 1 1 d . . . N2 N 0.2210(4) -0.0905(5) 0.4024(3) 0.054(2) Uani 1 1 d . . . N3 N 0.3155(4) -0.0242(4) 0.4816(3) 0.046(2) Uani 1 1 d . . . N4 N 0.2998(4) -0.0987(4) 0.4770(3) 0.052(2) Uani 1 1 d . . . N5 N 0.1559(3) -0.0201(4) 0.4906(3) 0.046(2) Uani 1 1 d . . . N6 N 0.1624(4) -0.0953(4) 0.4814(3) 0.054(2) Uani 1 1 d . . . N7 N 0.2688(3) 0.5510(4) 0.5842(3) 0.0389(18) Uani 1 1 d . . . N8 N 0.2711(3) 0.5865(4) 0.6272(3) 0.0381(18) Uani 1 1 d . . . N9 N 0.1892(4) 0.4444(4) 0.6420(3) 0.0427(19) Uani 1 1 d . . . N10 N 0.2033(4) 0.4952(4) 0.6767(3) 0.046(2) Uani 1 1 d . . . N11 N 0.3489(3) 0.4428(4) 0.6389(3) 0.0395(18) Uani 1 1 d . . . N12 N 0.3397(4) 0.4913(4) 0.6756(3) 0.049(2) Uani 1 1 d . . . N13 N 0.9860(4) 0.3606(4) 0.4012(3) 0.045(2) Uani 1 1 d . . . N14 N 0.4651(4) 0.3315(5) 0.3661(3) 0.057(2) Uani 1 1 d . . . N15 N 0.4618(4) 0.0851(5) 0.6503(3) 0.058(2) Uani 1 1 d . . . N16 N 0.2953(8) 0.8535(9) 0.6491(6) 0.150(6) Uani 1 1 d . . . N17 N 0.0856(8) 0.5595(14) 0.2691(8) 0.296(14) Uani 1 1 d . . . C60 C 0.965(2) 1.0004(19) 0.3272(7) 0.36(3) Uani 1 1 d . . . H60A H 0.9180 0.9777 0.3215 0.543 Uiso 1 1 calc R . . H60B H 0.9954 0.9931 0.2997 0.543 Uiso 1 1 calc R . . H60C H 0.9591 1.0526 0.3327 0.543 Uiso 1 1 calc R . . N19 N 0.3450(5) 0.2123(6) 0.7687(4) 0.089(3) Uani 1 1 d . . . C64 C 0.1283(8) 0.1815(10) 0.6694(7) 0.162(7) Uani 1 1 d . . . H64A H 0.1638 0.2176 0.6806 0.243 Uiso 1 1 calc R . . H64B H 0.1174 0.1894 0.6359 0.243 Uiso 1 1 calc R . . H64C H 0.1482 0.1325 0.6740 0.243 Uiso 1 1 calc R . . B1 B 0.2258(7) -0.1234(6) 0.4527(5) 0.065(4) Uani 1 1 d . . . H1 H 0.224(4) -0.178(5) 0.451(3) 0.078 Uiso 1 1 calc . . . B2 B 0.2725(6) 0.5451(7) 0.6739(4) 0.047(3) Uani 1 1 d . . . H2 H 0.275(4) 0.580(4) 0.701(3) 0.056 Uiso 1 1 calc . . . C1 C 0.2147(5) -0.0054(6) 0.3501(4) 0.060(3) Uani 1 1 d . . . H1A H 0.2139 0.0410 0.3355 0.072 Uiso 1 1 calc R . . C2 C 0.2086(6) -0.0717(6) 0.3258(4) 0.068(3) Uani 1 1 d . . . H2A H 0.2027 -0.0783 0.2928 0.081 Uiso 1 1 calc R . . C3 C 0.2131(5) -0.1245(7) 0.3592(5) 0.072(3) Uani 1 1 d . . . H3 H 0.2111 -0.1755 0.3539 0.087 Uiso 1 1 calc R . . C4 C 0.3826(5) -0.0205(5) 0.5000(3) 0.047(3) Uani 1 1 d . . . H4 H 0.4072 0.0238 0.5067 0.056 Uiso 1 1 calc R . . C5 C 0.4129(5) -0.0899(5) 0.5083(3) 0.054(3) Uani 1 1 d . . . H5 H 0.4593 -0.1014 0.5213 0.064 Uiso 1 1 calc R . . C6 C 0.3593(6) -0.1374(6) 0.4930(4) 0.069(3) Uani 1 1 d . . . H6 H 0.3630 -0.1889 0.4935 0.083 Uiso 1 1 calc R . . C7 C 0.0946(5) -0.0130(6) 0.5151(3) 0.055(3) Uani 1 1 d . . . H7 H 0.0765 0.0321 0.5260 0.066 Uiso 1 1 calc R . . C8 C 0.0609(5) -0.0803(6) 0.5224(4) 0.072(3) Uani 1 1 d . . . H8 H 0.0173 -0.0892 0.5382 0.087 Uiso 1 1 calc R . . C9 C 0.1053(5) -0.1310(6) 0.5013(4) 0.070(3) Uani 1 1 d . . . H9 H 0.0976 -0.1821 0.5008 0.084 Uiso 1 1 calc R . . C10 C 0.2693(4) 0.6022(5) 0.5492(3) 0.041(2) Uani 1 1 d . . . H10 H 0.2679 0.5925 0.5165 0.050 Uiso 1 1 calc R . . C11 C 0.2723(4) 0.6721(5) 0.5704(4) 0.049(3) Uani 1 1 d . . . H11 H 0.2741 0.7177 0.5548 0.058 Uiso 1 1 calc R . . C12 C 0.2720(4) 0.6603(5) 0.6186(4) 0.050(3) Uani 1 1 d . . . H12 H 0.2723 0.6973 0.6419 0.060 Uiso 1 1 calc R . . C13 C 0.1274(4) 0.4082(5) 0.6548(4) 0.050(3) Uani 1 1 d . . . H13 H 0.1057 0.3689 0.6381 0.060 Uiso 1 1 calc R . . C14 C 0.1015(5) 0.4384(6) 0.6964(3) 0.056(3) Uani 1 1 d . . . H14 H 0.0592 0.4250 0.7124 0.068 Uiso 1 1 calc R . . C15 C 0.1514(5) 0.4924(5) 0.7093(3) 0.052(3) Uani 1 1 d . . . H15 H 0.1492 0.5222 0.7364 0.062 Uiso 1 1 calc R . . C16 C 0.4110(5) 0.4061(5) 0.6498(4) 0.050(3) Uani 1 1 d . . . H16 H 0.4308 0.3690 0.6308 0.060 Uiso 1 1 calc R . . C17 C 0.4421(5) 0.4299(6) 0.6926(4) 0.061(3) Uani 1 1 d . . . H17 H 0.4852 0.4129 0.7078 0.073 Uiso 1 1 calc R . . C18 C 0.3955(6) 0.4839(6) 0.7078(4) 0.059(3) Uani 1 1 d . . . H18 H 0.4015 0.5112 0.7359 0.071 Uiso 1 1 calc R . . C19 C 0.1784(5) 0.2327(6) 0.2996(4) 0.061(3) Uani 1 1 d . . . C20 C 0.1360(5) 0.1690(6) 0.2996(4) 0.056(3) Uani 1 1 d . . . H20 H 0.1224 0.1489 0.3288 0.068 Uiso 1 1 calc R . . C21 C 0.1131(6) 0.1341(8) 0.2577(5) 0.089(4) Uani 1 1 d . . . H21 H 0.0858 0.0904 0.2594 0.107 Uiso 1 1 calc R . . C22 C 0.1297(6) 0.1624(7) 0.2139(5) 0.094(4) Uani 1 1 d . . . H22 H 0.1147 0.1392 0.1854 0.112 Uiso 1 1 calc R . . C23 C 0.1718(6) 0.2303(8) 0.2143(5) 0.099(4) Uani 1 1 d . . . H23 H 0.1853 0.2511 0.1854 0.119 Uiso 1 1 calc R . . C24 C 0.1921(7) 0.2642(7) 0.2553(4) 0.087(4) Uani 1 1 d . . . H24 H 0.2159 0.3100 0.2540 0.104 Uiso 1 1 calc R . . C25 C 0.2976(8) 0.5524(7) 0.4170(4) 0.083(4) Uani 1 1 d . . . C26 C 0.3721(9) 0.5624(7) 0.4322(5) 0.107(5) Uani 1 1 d . . . H26 H 0.3999 0.5206 0.4402 0.128 Uiso 1 1 calc R . . C31 C 0.9676(5) 0.3839(5) 0.3503(4) 0.061(3) Uani 1 1 d . . . H31A H 0.9227 0.3586 0.3399 0.073 Uiso 1 1 calc R . . H31B H 0.9572 0.4368 0.3503 0.073 Uiso 1 1 calc R . . C32 C 1.0257(5) 0.3691(6) 0.3144(4) 0.078(3) Uani 1 1 d . . . H32A H 1.0720 0.3893 0.3259 0.117 Uiso 1 1 calc R . . H32B H 1.0118 0.3922 0.2845 0.117 Uiso 1 1 calc R . . H32C H 1.0306 0.3165 0.3098 0.117 Uiso 1 1 calc R . . C33 C 1.0538(4) 0.4018(5) 0.4197(4) 0.055(3) Uani 1 1 d . . . H33A H 1.0955 0.3877 0.4007 0.066 Uiso 1 1 calc R . . H33B H 1.0645 0.3866 0.4525 0.066 Uiso 1 1 calc R . . C34 C 1.0454(5) 0.4857(5) 0.4183(4) 0.080(4) Uani 1 1 d . . . H34A H 1.0450 0.5023 0.3856 0.120 Uiso 1 1 calc R . . H34B H 1.0861 0.5083 0.4356 0.120 Uiso 1 1 calc R . . H34C H 1.0000 0.4996 0.4327 0.120 Uiso 1 1 calc R . . C35 C 0.9207(5) 0.3763(6) 0.4309(4) 0.063(3) Uani 1 1 d . . . H35A H 0.8796 0.3468 0.4186 0.076 Uiso 1 1 calc R . . H35B H 0.9075 0.4281 0.4267 0.076 Uiso 1 1 calc R . . C36 C 0.9299(5) 0.3612(6) 0.4839(3) 0.067(3) Uani 1 1 d . . . H36A H 0.9492 0.3120 0.4887 0.101 Uiso 1 1 calc R . . H36B H 0.8829 0.3653 0.4987 0.101 Uiso 1 1 calc R . . H36C H 0.9636 0.3968 0.4980 0.101 Uiso 1 1 calc R . . C37 C 1.0059(4) 0.2788(5) 0.4031(3) 0.053(3) Uani 1 1 d . . . H37A H 1.0169 0.2654 0.4362 0.063 Uiso 1 1 calc R . . H37B H 1.0505 0.2713 0.3853 0.063 Uiso 1 1 calc R . . C38 C 0.9464(5) 0.2259(5) 0.3832(4) 0.072(3) Uani 1 1 d . . . H38A H 0.9023 0.2316 0.4011 0.109 Uiso 1 1 calc R . . H38B H 0.9637 0.1756 0.3859 0.109 Uiso 1 1 calc R . . H38C H 0.9360 0.2374 0.3501 0.109 Uiso 1 1 calc R . . C39 C 0.4717(6) 0.3821(7) 0.3233(4) 0.089(4) Uani 1 1 d . . . H39A H 0.4801 0.3522 0.2950 0.107 Uiso 1 1 calc R . . H39B H 0.5143 0.4142 0.3282 0.107 Uiso 1 1 calc R . . C40 C 0.4023(6) 0.4306(7) 0.3143(4) 0.112(5) Uani 1 1 d . . . H40A H 0.3938 0.4604 0.3421 0.169 Uiso 1 1 calc R . . H40B H 0.3603 0.3991 0.3081 0.169 Uiso 1 1 calc R . . H40C H 0.4096 0.4622 0.2872 0.169 Uiso 1 1 calc R . . C41 C 0.4570(5) 0.3703(6) 0.4111(4) 0.076(3) Uani 1 1 d . . . H41A H 0.4492 0.3334 0.4358 0.092 Uiso 1 1 calc R . . H41B H 0.4126 0.4002 0.4086 0.092 Uiso 1 1 calc R . . C42 C 0.5203(5) 0.4207(6) 0.4283(5) 0.107(5) Uani 1 1 d . . . H42A H 0.5594 0.3910 0.4421 0.160 Uiso 1 1 calc R . . H42B H 0.5027 0.4547 0.4520 0.160 Uiso 1 1 calc R . . H42C H 0.5385 0.4482 0.4016 0.160 Uiso 1 1 calc R . . C43 C 0.5363(5) 0.2856(7) 0.3676(4) 0.088(4) Uani 1 1 d . . . H43A H 0.5393 0.2582 0.3378 0.105 Uiso 1 1 calc R . . H43B H 0.5781 0.3193 0.3695 0.105 Uiso 1 1 calc R . . C44 C 0.5427(5) 0.2315(6) 0.4089(4) 0.081(4) Uani 1 1 d . . . H44A H 0.5434 0.2583 0.4386 0.122 Uiso 1 1 calc R . . H44B H 0.5875 0.2034 0.4064 0.122 Uiso 1 1 calc R . . H44C H 0.5011 0.1983 0.4077 0.122 Uiso 1 1 calc R . . C45 C 0.3997(5) 0.2809(6) 0.3592(4) 0.078(4) Uani 1 1 d . . . H45A H 0.3551 0.3106 0.3607 0.093 Uiso 1 1 calc R . . H45B H 0.3994 0.2461 0.3858 0.093 Uiso 1 1 calc R . . C46 C 0.3966(6) 0.2356(7) 0.3113(4) 0.097(4) Uani 1 1 d . . . H46A H 0.3982 0.2692 0.2846 0.145 Uiso 1 1 calc R . . H46B H 0.3517 0.2073 0.3093 0.145 Uiso 1 1 calc R . . H46C H 0.4381 0.2025 0.3105 0.145 Uiso 1 1 calc R . . C47 C 0.5178(5) 0.0874(6) 0.6116(3) 0.070(3) Uani 1 1 d . . . H47A H 0.5114 0.1332 0.5936 0.084 Uiso 1 1 calc R . . H47B H 0.5083 0.0465 0.5896 0.084 Uiso 1 1 calc R . . C48 C 0.5992(5) 0.0825(7) 0.6306(4) 0.105(5) Uani 1 1 d . . . H48A H 0.6115 0.1267 0.6483 0.158 Uiso 1 1 calc R . . H48B H 0.6315 0.0779 0.6040 0.158 Uiso 1 1 calc R . . H48C H 0.6050 0.0399 0.6511 0.158 Uiso 1 1 calc R . . C49 C 0.4694(6) 0.0155(6) 0.6789(4) 0.076(3) Uani 1 1 d . . . H49A H 0.4288 0.0127 0.7007 0.091 Uiso 1 1 calc R . . H49B H 0.5148 0.0182 0.6981 0.091 Uiso 1 1 calc R . . C50 C 0.4706(7) -0.0567(7) 0.6490(4) 0.122(5) Uani 1 1 d . . . H50A H 0.4301 -0.0563 0.6260 0.183 Uiso 1 1 calc R . . H50B H 0.4659 -0.0988 0.6698 0.183 Uiso 1 1 calc R . . H50C H 0.5163 -0.0599 0.6325 0.183 Uiso 1 1 calc R . . C51 C 0.4735(5) 0.1487(6) 0.6854(4) 0.072(3) Uani 1 1 d . . . H51A H 0.4383 0.1437 0.7108 0.086 Uiso 1 1 calc R . . H51B H 0.5226 0.1444 0.6999 0.086 Uiso 1 1 calc R . . C52 C 0.4654(6) 0.2246(6) 0.6638(4) 0.091(4) Uani 1 1 d . . . H52A H 0.5006 0.2306 0.6390 0.137 Uiso 1 1 calc R . . H52B H 0.4741 0.2615 0.6881 0.137 Uiso 1 1 calc R . . H52C H 0.4163 0.2303 0.6504 0.137 Uiso 1 1 calc R . . C53 C 0.3853(5) 0.0903(6) 0.6251(3) 0.066(3) Uani 1 1 d . . . H53A H 0.3842 0.1345 0.6051 0.079 Uiso 1 1 calc R . . H53B H 0.3790 0.0477 0.6041 0.079 Uiso 1 1 calc R . . C54 C 0.3203(5) 0.0934(7) 0.6584(4) 0.087(4) Uani 1 1 d . . . H54A H 0.3192 0.0488 0.6772 0.131 Uiso 1 1 calc R . . H54B H 0.2752 0.0976 0.6397 0.131 Uiso 1 1 calc R . . H54C H 0.3255 0.1356 0.6792 0.131 Uiso 1 1 calc R . . C55 C 0.2529(10) 0.8928(11) 0.6254(9) 0.151(8) Uani 1 1 d . . . C56 C 0.2125(11) 0.9297(10) 0.6020(8) 0.243(15) Uani 1 1 d . . . H56A H 0.1902 0.9001 0.5769 0.365 Uiso 1 1 calc R . . H56B H 0.2396 0.9698 0.5881 0.365 Uiso 1 1 calc R . . H56C H 0.1748 0.9496 0.6218 0.365 Uiso 1 1 calc R . . C57 C 0.1413(10) 0.5447(13) 0.2691(7) 0.168(9) Uani 1 1 d . . . C58 C 0.2109(9) 0.5359(17) 0.2835(8) 0.34(2) Uani 1 1 d . . . H58A H 0.2378 0.5809 0.2778 0.517 Uiso 1 1 calc R . . H58B H 0.2325 0.4959 0.2659 0.517 Uiso 1 1 calc R . . H58C H 0.2130 0.5245 0.3171 0.517 Uiso 1 1 calc R . . C59 C 0.9909(19) 0.9763(15) 0.3570(7) 0.225(18) Uani 1 1 d . . . N18 N 1.0301(8) 0.9384(10) 0.3918(5) 0.157(6) Uani 1 1 d . . . C61 C 0.3155(6) 0.2616(7) 0.7548(4) 0.063(3) Uani 1 1 d . . . C62 C 0.2764(6) 0.3303(6) 0.7384(4) 0.088(4) Uani 1 1 d . . . H62A H 0.3006 0.3730 0.7523 0.132 Uiso 1 1 calc R . . H62B H 0.2261 0.3287 0.7484 0.132 Uiso 1 1 calc R . . H62C H 0.2773 0.3335 0.7041 0.132 Uiso 1 1 calc R . . C63 C 0.059(3) 0.1893(18) 0.6971(10) 0.60(3) Uani 1 1 d . . . C67 C 0.9358(13) 0.3083(19) 0.6210(11) 0.109(13) Uani 0.50 1 d P . . H67A H 0.9883 0.3015 0.6221 0.163 Uiso 0.50 1 calc PR . . H67B H 0.9244 0.3581 0.6109 0.163 Uiso 0.50 1 calc PR . . H67C H 0.9136 0.2736 0.5988 0.163 Uiso 0.50 1 calc PR . . C68 C 0.910(3) 0.297(3) 0.663(2) 0.20(3) Uani 0.50 1 d P . . N21 N 0.9326(18) 0.250(2) 0.6701(14) 0.169(19) Uani 0.50 1 d P . . C29 C 0.282(2) 0.665(2) 0.4086(9) 0.33(3) Uani 1 1 d . . . H29 H 0.2490 0.7043 0.4061 0.401 Uiso 1 1 calc R . . C30 C 0.250(2) 0.6049(11) 0.3991(12) 0.31(2) Uani 1 1 d . . . H30 H 0.2042 0.5977 0.3836 0.376 Uiso 1 1 calc R . . C28 C 0.3584(18) 0.6923(8) 0.4229(7) 0.222(19) Uani 1 1 d . . . H28 H 0.3715 0.7422 0.4230 0.267 Uiso 1 1 calc R . . C27 C 0.4076(8) 0.6348(10) 0.4360(5) 0.135(7) Uani 1 1 d . . . H27 H 0.4565 0.6422 0.4459 0.162 Uiso 1 1 calc R . . N51 N 0.1161(18) 0.201(2) 0.7335(13) 0.156(12) Uiso 0.50 1 d P . . N20 N 0.084(3) 0.233(3) 0.738(2) 0.31(4) Uiso 0.50 1 d P . . 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 0.0306(4) 0.0359(4) 0.0391(5) 0.0011(4) 0.0017(4) 0.0017(4) Mo2 0.0296(4) 0.0355(5) 0.0419(5) -0.0015(4) -0.0012(4) -0.0010(4) Fe1 0.0346(7) 0.0411(8) 0.0393(8) 0.0057(7) 0.0018(6) 0.0018(6) Fe2 0.0257(7) 0.0384(7) 0.0431(9) 0.0028(7) 0.0022(6) 0.0004(6) Fe3 0.0274(7) 0.0354(7) 0.0421(8) -0.0008(7) 0.0025(6) -0.0002(6) Fe4 0.0338(7) 0.0453(8) 0.0434(9) 0.0035(7) -0.0025(6) -0.0021(6) Fe5 0.0263(7) 0.0403(8) 0.0419(9) 0.0004(7) -0.0003(6) -0.0018(6) Fe6 0.0276(7) 0.0372(8) 0.0435(9) -0.0032(7) -0.0015(6) 0.0008(6) S1 0.0362(13) 0.0476(15) 0.0431(16) 0.0029(13) 0.0103(12) 0.0033(11) S2 0.0311(12) 0.0401(14) 0.0451(16) 0.0000(12) -0.0022(11) 0.0019(10) S3 0.0278(12) 0.0446(14) 0.0381(15) 0.0041(12) 0.0025(11) 0.0005(10) S4 0.0308(12) 0.0477(15) 0.0481(16) -0.0010(13) 0.0039(11) -0.0070(11) S5 0.0333(12) 0.0409(14) 0.0518(16) -0.0032(13) -0.0057(12) 0.0025(11) S6 0.0326(12) 0.0369(13) 0.0449(16) 0.0013(12) 0.0015(11) 0.0009(10) S7 0.0277(11) 0.0401(13) 0.0468(16) 0.0051(12) 0.0010(11) 0.0004(11) S8 0.0254(12) 0.0482(15) 0.0551(17) 0.0017(13) -0.0003(12) 0.0021(11) S9 0.0262(12) 0.0470(15) 0.0630(18) -0.0087(13) 0.0088(12) -0.0047(11) S10 0.0617(17) 0.0577(18) 0.064(2) 0.0010(15) -0.0059(15) -0.0060(14) S11 0.072(2) 0.103(3) 0.079(2) 0.027(2) -0.0077(18) -0.0092(18) N1 0.051(5) 0.051(6) 0.040(6) -0.003(4) -0.004(4) 0.012(4) N2 0.054(5) 0.051(6) 0.056(7) -0.007(5) -0.002(5) 0.013(4) N3 0.047(5) 0.038(5) 0.051(6) 0.003(4) -0.002(4) 0.011(4) N4 0.058(6) 0.036(5) 0.064(6) 0.007(4) 0.002(5) 0.015(4) N5 0.031(4) 0.045(5) 0.062(6) 0.010(4) 0.005(4) -0.002(4) N6 0.058(5) 0.035(5) 0.070(6) 0.005(4) 0.009(5) -0.003(4) N7 0.037(4) 0.045(5) 0.034(5) 0.001(4) -0.008(4) 0.008(4) N8 0.033(4) 0.040(5) 0.040(5) -0.007(4) -0.008(4) 0.000(4) N9 0.041(4) 0.043(5) 0.044(5) -0.005(4) 0.008(4) 0.006(4) N10 0.044(5) 0.056(5) 0.038(5) -0.009(4) 0.007(4) 0.008(4) N11 0.030(4) 0.040(5) 0.048(5) 0.000(4) -0.012(4) 0.000(4) N12 0.054(5) 0.050(5) 0.042(6) -0.009(5) -0.006(5) -0.007(4) N13 0.031(4) 0.051(5) 0.054(6) 0.002(4) -0.008(4) 0.001(4) N14 0.035(5) 0.060(6) 0.075(7) -0.005(5) -0.003(5) -0.001(4) N15 0.068(6) 0.061(6) 0.044(6) 0.009(5) 0.006(5) 0.009(5) N16 0.130(13) 0.138(15) 0.186(17) -0.015(11) 0.068(12) -0.013(9) N17 0.084(11) 0.40(3) 0.40(3) 0.22(3) 0.021(15) 0.001(16) C60 0.59(5) 0.40(4) 0.09(2) 0.06(2) -0.10(3) -0.32(4) N19 0.086(8) 0.080(8) 0.098(9) 0.018(6) -0.017(6) 0.025(6) C64 0.118(13) 0.113(15) 0.25(2) 0.039(18) -0.011(14) -0.032(11) B1 0.079(10) 0.020(6) 0.094(12) -0.007(8) -0.011(9) -0.007(7) B2 0.041(7) 0.066(9) 0.031(8) -0.017(6) -0.012(6) 0.011(6) C1 0.059(7) 0.073(8) 0.047(8) -0.011(7) 0.003(6) 0.007(6) C2 0.100(9) 0.064(8) 0.038(7) -0.022(7) -0.010(6) 0.016(7) C3 0.073(8) 0.066(8) 0.076(9) -0.025(8) -0.018(7) 0.005(7) C4 0.040(6) 0.050(6) 0.050(7) 0.003(5) 0.000(5) 0.014(5) C5 0.057(7) 0.046(6) 0.059(7) 0.007(6) 0.000(6) 0.018(6) C6 0.101(9) 0.038(6) 0.069(8) 0.010(6) 0.005(7) 0.014(7) C7 0.046(6) 0.064(7) 0.055(7) 0.011(6) 0.004(5) -0.004(5) C8 0.046(6) 0.073(8) 0.098(10) 0.031(8) -0.007(6) -0.029(6) C9 0.058(7) 0.060(7) 0.091(10) 0.025(7) -0.009(7) -0.021(6) C10 0.030(5) 0.049(6) 0.045(7) -0.002(5) -0.003(5) 0.000(5) C11 0.036(5) 0.034(6) 0.075(8) -0.004(6) -0.008(6) -0.013(4) C12 0.036(5) 0.038(6) 0.075(8) -0.023(6) -0.003(6) -0.010(5) C13 0.039(6) 0.048(6) 0.063(8) 0.007(5) -0.002(5) 0.009(5) C14 0.051(6) 0.065(7) 0.054(7) -0.004(6) 0.011(6) 0.004(6) C15 0.063(7) 0.055(7) 0.038(7) -0.008(5) 0.010(6) 0.007(6) C16 0.041(6) 0.038(6) 0.072(8) -0.008(5) -0.001(6) 0.002(5) C17 0.055(7) 0.060(7) 0.067(8) -0.004(6) -0.025(6) 0.010(6) C18 0.066(7) 0.059(7) 0.051(8) -0.002(6) -0.020(6) -0.015(6) C19 0.046(6) 0.085(8) 0.052(8) -0.004(7) -0.013(6) -0.001(6) C20 0.056(7) 0.072(8) 0.040(7) -0.002(6) -0.011(6) -0.006(6) C21 0.079(9) 0.130(12) 0.058(9) 0.014(9) -0.021(8) -0.011(8) C22 0.097(10) 0.100(11) 0.082(11) -0.004(8) -0.027(8) -0.021(8) C23 0.094(10) 0.128(13) 0.076(11) 0.024(9) -0.014(8) -0.041(9) C24 0.120(11) 0.121(11) 0.018(7) 0.018(7) -0.018(7) -0.032(9) C25 0.096(9) 0.093(11) 0.061(9) 0.006(7) -0.004(8) 0.020(9) C26 0.162(14) 0.061(9) 0.099(11) 0.018(8) 0.040(11) -0.008(10) C31 0.069(7) 0.041(6) 0.072(9) 0.010(6) -0.026(7) 0.001(5) C32 0.077(8) 0.099(9) 0.057(8) 0.015(7) -0.003(7) 0.010(7) C33 0.038(6) 0.057(7) 0.069(8) -0.011(6) -0.025(5) -0.001(5) C34 0.073(7) 0.061(8) 0.104(10) -0.024(7) -0.023(7) -0.006(6) C35 0.033(6) 0.065(7) 0.090(9) -0.020(7) -0.015(6) 0.019(5) C36 0.065(7) 0.070(8) 0.067(8) -0.015(6) 0.004(6) 0.019(6) C37 0.034(5) 0.054(7) 0.069(8) 0.002(6) -0.015(5) 0.007(5) C38 0.081(8) 0.042(6) 0.093(9) 0.004(6) -0.026(7) -0.007(6) C39 0.095(9) 0.097(10) 0.075(9) 0.044(8) 0.019(8) -0.011(8) C40 0.083(8) 0.119(11) 0.134(12) 0.077(10) -0.009(8) 0.037(9) C41 0.059(7) 0.061(7) 0.109(11) -0.007(8) -0.001(7) -0.004(6) C42 0.041(6) 0.076(9) 0.203(15) -0.035(10) -0.011(8) -0.025(6) C43 0.063(8) 0.121(11) 0.081(9) 0.012(8) 0.016(7) -0.007(7) C44 0.093(9) 0.065(8) 0.087(9) 0.018(7) 0.025(8) 0.009(7) C45 0.053(7) 0.075(8) 0.107(10) 0.007(7) 0.024(7) -0.020(6) C46 0.088(9) 0.107(10) 0.095(10) -0.033(8) 0.000(8) -0.010(8) C47 0.079(8) 0.083(8) 0.050(7) 0.003(6) 0.022(6) 0.010(6) C48 0.052(7) 0.165(14) 0.099(10) -0.006(10) 0.011(7) 0.019(8) C49 0.081(8) 0.077(9) 0.071(9) 0.018(7) 0.012(7) 0.021(7) C50 0.176(13) 0.069(9) 0.123(12) 0.004(9) 0.029(11) 0.029(9) C51 0.058(7) 0.104(10) 0.053(8) -0.026(7) -0.003(6) 0.016(7) C52 0.091(9) 0.058(8) 0.122(11) 0.005(8) -0.027(8) 0.001(7) C53 0.076(8) 0.070(8) 0.051(7) 0.011(6) -0.001(6) -0.004(6) C54 0.077(8) 0.132(11) 0.054(8) 0.012(7) 0.014(7) -0.009(7) C55 0.114(18) 0.13(2) 0.21(3) 0.022(16) 0.024(17) -0.007(12) C56 0.27(2) 0.113(15) 0.34(3) 0.138(17) -0.23(2) -0.079(15) C57 0.079(12) 0.27(2) 0.158(18) 0.007(16) 0.039(14) 0.006(17) C58 0.094(14) 0.72(6) 0.22(3) -0.10(3) -0.001(16) 0.03(3) C59 0.39(5) 0.19(3) 0.09(2) -0.048(19) 0.06(3) -0.18(3) N18 0.164(12) 0.198(16) 0.107(13) 0.007(11) -0.011(11) 0.030(11) C61 0.057(8) 0.102(10) 0.031(7) 0.009(7) 0.002(6) 0.000(7) C62 0.108(10) 0.085(9) 0.071(9) 0.023(7) 0.015(7) 0.018(8) C63 1.41(10) 0.26(3) 0.14(3) -0.01(2) 0.19(4) -0.22(5) C67 0.067(16) 0.11(2) 0.15(3) -0.03(3) 0.06(2) -0.001(16) C68 0.16(4) 0.19(5) 0.23(6) -0.08(5) -0.13(4) 0.12(4) N21 0.08(2) 0.22(4) 0.21(4) -0.16(3) -0.08(2) 0.07(2) C29 0.50(7) 0.43(6) 0.070(17) -0.01(3) -0.03(3) 0.33(6) C30 0.32(3) 0.085(15) 0.53(5) 0.04(2) 0.03(3) 0.13(2) C28 0.55(6) 0.012(7) 0.105(18) 0.005(9) 0.07(2) 0.007(17) C27 0.166(14) 0.142(15) 0.100(12) -0.039(12) 0.075(11) -0.087(13) _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 N3 2.232(7) . ? Mo1 N5 2.238(7) . ? Mo1 N1 2.247(8) . ? Mo1 S3 2.348(2) . ? Mo1 S2 2.372(2) . ? Mo1 S1 2.378(2) . ? Mo1 Fe2 2.7128(14) . ? Mo1 Fe1 2.7166(15) . ? Mo1 Fe3 2.7188(14) . ? Mo2 N11 2.226(7) . ? Mo2 N9 2.242(6) . ? Mo2 N7 2.264(7) . ? Mo2 S6 2.357(2) . ? Mo2 S4 2.369(2) . ? Mo2 S5 2.378(2) . ? Mo2 Fe4 2.6984(15) . ? Mo2 Fe6 2.7157(15) . ? Mo2 Fe5 2.7405(14) . ? Fe1 S2 2.254(2) . ? Fe1 S1 2.263(2) . ? Fe1 S10 2.287(3) . ? Fe1 S7 2.382(3) . ? Fe1 Fe3 2.6718(17) . ? Fe1 Fe2 2.7102(18) . ? Fe2 S8 2.228(3) . ? Fe2 S1 2.258(3) . ? Fe2 S3 2.268(2) . ? Fe2 S7 2.374(2) . ? Fe2 Fe5 2.6950(18) . ? Fe2 Fe3 2.7516(15) . ? Fe3 S9 2.222(2) . ? Fe3 S3 2.254(2) . ? Fe3 S2 2.256(3) . ? Fe3 S7 2.409(2) . ? Fe3 Fe6 2.6889(18) . ? Fe4 S4 2.250(3) . ? Fe4 S5 2.264(2) . ? Fe4 S11 2.272(3) . ? Fe4 S7 2.373(3) . ? Fe4 Fe5 2.7063(18) . ? Fe4 Fe6 2.7577(17) . ? Fe5 S8 2.227(2) . ? Fe5 S4 2.250(3) . ? Fe5 S6 2.264(2) . ? Fe5 S7 2.396(3) . ? Fe5 Fe6 2.7609(15) . ? Fe6 S9 2.228(2) . ? Fe6 S5 2.252(3) . ? Fe6 S6 2.261(3) . ? Fe6 S7 2.374(3) . ? S10 C19 1.710(10) . ? S11 C25 1.764(14) . ? N1 C1 1.310(11) . ? N1 N2 1.354(10) . ? N2 C3 1.356(12) . ? N2 B1 1.524(15) . ? N3 C4 1.307(10) . ? N3 N4 1.376(9) . ? N4 C6 1.349(11) . ? N4 B1 1.549(14) . ? N5 C7 1.327(10) . ? N5 N6 1.383(9) . ? N6 C9 1.351(10) . ? N6 B1 1.506(14) . ? N7 C10 1.342(10) . ? N7 N8 1.358(9) . ? N8 C12 1.349(10) . ? N8 B2 1.502(13) . ? N9 C13 1.352(9) . ? N9 N10 1.352(9) . ? N10 C15 1.326(9) . ? N10 B2 1.545(13) . ? N11 C16 1.332(9) . ? N11 N12 1.359(9) . ? N12 C18 1.340(10) . ? N12 B2 1.554(12) . ? N13 C35 1.490(10) . ? N13 C31 1.507(11) . ? N13 C33 1.513(10) . ? N13 C37 1.516(10) . ? N14 C41 1.448(12) . ? N14 C39 1.510(11) . ? N14 C45 1.503(11) . ? N14 C43 1.531(12) . ? N15 C49 1.490(11) . ? N15 C47 1.502(10) . ? N15 C51 1.518(12) . ? N15 C53 1.539(11) . ? N16 C55 1.22(2) . ? N17 C57 1.045(17) . ? C60 C59 1.04(4) . ? N19 C61 1.101(12) . ? C64 C63 1.51(4) . ? C1 C2 1.376(12) . ? C2 C3 1.333(13) . ? C4 C5 1.382(11) . ? C5 C6 1.353(12) . ? C7 C8 1.373(12) . ? C8 C9 1.360(13) . ? C10 C11 1.391(11) . ? C11 C12 1.360(12) . ? C13 C14 1.375(11) . ? C14 C15 1.367(12) . ? C16 C17 1.375(12) . ? C17 C18 1.362(12) . ? C19 C20 1.381(12) . ? C19 C24 1.390(13) . ? C20 C21 1.381(13) . ? C21 C22 1.367(14) . ? C22 C23 1.439(15) . ? C23 C24 1.338(14) . ? C25 C30 1.37(2) . ? C25 C26 1.415(15) . ? C26 C27 1.455(16) . ? C31 C32 1.498(11) . ? C33 C34 1.518(12) . ? C35 C36 1.507(12) . ? C37 C38 1.530(11) . ? C39 C40 1.545(12) . ? C41 C42 1.528(12) . ? C43 C44 1.509(13) . ? C45 C46 1.566(13) . ? C47 C48 1.556(11) . ? C49 C50 1.543(14) . ? C51 C52 1.498(13) . ? C53 C54 1.520(11) . ? C55 C56 1.17(2) . ? C57 C58 1.321(19) . ? C59 N18 1.37(3) . ? C61 C62 1.490(14) . ? C63 N51 1.45(5) . ? C63 N20 1.45(8) . ? C67 C68 1.29(7) . ? C68 N21 0.96(6) . ? C29 C30 1.25(5) . ? C29 C28 1.51(5) . ? C28 C27 1.41(2) . ? N51 N20 0.83(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 N3 Mo1 N5 81.2(3) . . ? N3 Mo1 N1 80.1(3) . . ? N5 Mo1 N1 81.1(3) . . ? N3 Mo1 S3 86.4(2) . . ? N5 Mo1 S3 86.3(2) . . ? N1 Mo1 S3 162.8(2) . . ? N3 Mo1 S2 164.2(2) . . ? N5 Mo1 S2 86.36(18) . . ? N1 Mo1 S2 88.4(2) . . ? S3 Mo1 S2 102.52(8) . . ? N3 Mo1 S1 88.04(19) . . ? N5 Mo1 S1 165.0(2) . . ? N1 Mo1 S1 86.8(2) . . ? S3 Mo1 S1 103.51(8) . . ? S2 Mo1 S1 102.19(8) . . ? N3 Mo1 Fe2 95.2(2) . . ? N5 Mo1 Fe2 139.0(2) . . ? N1 Mo1 Fe2 138.9(2) . . ? S3 Mo1 Fe2 52.65(6) . . ? S2 Mo1 Fe2 100.50(6) . . ? S1 Mo1 Fe2 52.15(6) . . ? N3 Mo1 Fe1 140.14(19) . . ? N5 Mo1 Fe1 138.30(18) . . ? N1 Mo1 Fe1 98.4(2) . . ? S3 Mo1 Fe1 98.78(7) . . ? S2 Mo1 Fe1 52.05(6) . . ? S1 Mo1 Fe1 52.23(6) . . ? Fe2 Mo1 Fe1 59.89(4) . . ? N3 Mo1 Fe3 138.6(2) . . ? N5 Mo1 Fe3 95.39(19) . . ? N1 Mo1 Fe3 140.45(19) . . ? S3 Mo1 Fe3 52.21(6) . . ? S2 Mo1 Fe3 52.07(6) . . ? S1 Mo1 Fe3 99.56(7) . . ? Fe2 Mo1 Fe3 60.88(4) . . ? Fe1 Mo1 Fe3 58.89(4) . . ? N11 Mo2 N9 80.8(3) . . ? N11 Mo2 N7 78.7(3) . . ? N9 Mo2 N7 80.5(3) . . ? N11 Mo2 S6 88.41(19) . . ? N9 Mo2 S6 87.14(19) . . ? N7 Mo2 S6 163.4(2) . . ? N11 Mo2 S4 87.35(18) . . ? N9 Mo2 S4 165.0(2) . . ? N7 Mo2 S4 88.21(18) . . ? S6 Mo2 S4 101.77(8) . . ? N11 Mo2 S5 162.23(19) . . ? N9 Mo2 S5 86.13(19) . . ? N7 Mo2 S5 87.30(18) . . ? S6 Mo2 S5 103.03(8) . . ? S4 Mo2 S5 103.25(8) . . ? N11 Mo2 Fe4 139.55(17) . . ? N9 Mo2 Fe4 138.62(18) . . ? N7 Mo2 Fe4 96.8(2) . . ? S6 Mo2 Fe4 99.86(7) . . ? S4 Mo2 Fe4 52.21(6) . . ? S5 Mo2 Fe4 52.51(6) . . ? N11 Mo2 Fe6 140.75(18) . . ? N9 Mo2 Fe6 94.24(19) . . ? N7 Mo2 Fe6 139.24(18) . . ? S6 Mo2 Fe6 52.36(6) . . ? S4 Mo2 Fe6 100.72(7) . . ? S5 Mo2 Fe6 51.95(6) . . ? Fe4 Mo2 Fe6 61.24(4) . . ? N11 Mo2 Fe5 98.36(19) . . ? N9 Mo2 Fe5 139.13(19) . . ? N7 Mo2 Fe5 139.81(18) . . ? S6 Mo2 Fe5 52.08(6) . . ? S4 Mo2 Fe5 51.62(6) . . ? S5 Mo2 Fe5 99.39(6) . . ? Fe4 Mo2 Fe5 59.67(4) . . ? Fe6 Mo2 Fe5 60.79(4) . . ? S2 Fe1 S1 109.85(9) . . ? S2 Fe1 S10 115.95(10) . . ? S1 Fe1 S10 122.84(10) . . ? S2 Fe1 S7 107.22(9) . . ? S1 Fe1 S7 104.17(9) . . ? S10 Fe1 S7 93.32(10) . . ? S2 Fe1 Fe3 53.71(7) . . ? S1 Fe1 Fe3 104.05(8) . . ? S10 Fe1 Fe3 130.07(9) . . ? S7 Fe1 Fe3 56.59(6) . . ? S2 Fe1 Fe2 103.77(8) . . ? S1 Fe1 Fe2 53.08(7) . . ? S10 Fe1 Fe2 135.72(9) . . ? S7 Fe1 Fe2 55.13(6) . . ? Fe3 Fe1 Fe2 61.49(4) . . ? S2 Fe1 Mo1 56.09(6) . . ? S1 Fe1 Mo1 56.16(6) . . ? S10 Fe1 Mo1 162.41(9) . . ? S7 Fe1 Mo1 103.99(7) . . ? Fe3 Fe1 Mo1 60.60(4) . . ? Fe2 Fe1 Mo1 59.98(4) . . ? S8 Fe2 S1 118.22(9) . . ? S8 Fe2 S3 114.47(10) . . ? S1 Fe2 S3 110.19(9) . . ? S8 Fe2 S7 103.80(9) . . ? S1 Fe2 S7 104.59(9) . . ? S3 Fe2 S7 103.74(8) . . ? S8 Fe2 Fe5 52.77(7) . . ? S1 Fe2 Fe5 145.21(8) . . ? S3 Fe2 Fe5 102.92(8) . . ? S7 Fe2 Fe5 55.99(7) . . ? S8 Fe2 Fe1 142.97(8) . . ? S1 Fe2 Fe1 53.25(7) . . ? S3 Fe2 Fe1 101.02(7) . . ? S7 Fe2 Fe1 55.41(7) . . ? Fe5 Fe2 Fe1 110.69(6) . . ? S8 Fe2 Mo1 151.74(8) . . ? S1 Fe2 Mo1 56.27(6) . . ? S3 Fe2 Mo1 55.38(7) . . ? S7 Fe2 Mo1 104.33(7) . . ? Fe5 Fe2 Mo1 149.15(5) . . ? Fe1 Fe2 Mo1 60.12(4) . . ? S8 Fe2 Fe3 139.28(8) . . ? S1 Fe2 Fe3 101.72(7) . . ? S3 Fe2 Fe3 52.29(6) . . ? S7 Fe2 Fe3 55.48(6) . . ? Fe5 Fe2 Fe3 89.99(5) . . ? Fe1 Fe2 Fe3 58.57(4) . . ? Mo1 Fe2 Fe3 59.67(4) . . ? S9 Fe3 S3 116.72(10) . . ? S9 Fe3 S2 116.28(9) . . ? S3 Fe3 S2 109.44(9) . . ? S9 Fe3 S7 103.43(9) . . ? S3 Fe3 S7 103.06(9) . . ? S2 Fe3 S7 106.26(9) . . ? S9 Fe3 Fe1 139.48(9) . . ? S3 Fe3 Fe1 102.56(7) . . ? S2 Fe3 Fe1 53.64(6) . . ? S7 Fe3 Fe1 55.63(7) . . ? S9 Fe3 Fe6 52.94(7) . . ? S3 Fe3 Fe6 104.75(8) . . ? S2 Fe3 Fe6 144.34(8) . . ? S7 Fe3 Fe6 55.18(7) . . ? Fe1 Fe3 Fe6 109.32(6) . . ? S9 Fe3 Mo1 153.36(8) . . ? S3 Fe3 Mo1 55.40(6) . . ? S2 Fe3 Mo1 56.04(6) . . ? S7 Fe3 Mo1 103.19(6) . . ? Fe1 Fe3 Mo1 60.52(4) . . ? Fe6 Fe3 Mo1 149.41(5) . . ? S9 Fe3 Fe2 140.20(9) . . ? S3 Fe3 Fe2 52.75(6) . . ? S2 Fe3 Fe2 102.43(7) . . ? S7 Fe3 Fe2 54.29(6) . . ? Fe1 Fe3 Fe2 59.94(4) . . ? Fe6 Fe3 Fe2 90.17(5) . . ? Mo1 Fe3 Fe2 59.45(4) . . ? S4 Fe4 S5 111.10(10) . . ? S4 Fe4 S11 112.69(10) . . ? S5 Fe4 S11 119.38(11) . . ? S4 Fe4 S7 105.87(9) . . ? S5 Fe4 S7 102.32(9) . . ? S11 Fe4 S7 103.68(12) . . ? S4 Fe4 Mo2 56.35(6) . . ? S5 Fe4 Mo2 56.46(7) . . ? S11 Fe4 Mo2 152.67(11) . . ? S7 Fe4 Mo2 103.51(8) . . ? S4 Fe4 Fe5 53.03(7) . . ? S5 Fe4 Fe5 103.42(8) . . ? S11 Fe4 Fe5 136.34(9) . . ? S7 Fe4 Fe5 55.84(7) . . ? Mo2 Fe4 Fe5 60.93(4) . . ? S4 Fe4 Fe6 102.65(8) . . ? S5 Fe4 Fe6 52.16(7) . . ? S11 Fe4 Fe6 143.04(10) . . ? S7 Fe4 Fe6 54.51(6) . . ? Mo2 Fe4 Fe6 59.69(4) . . ? Fe5 Fe4 Fe6 60.69(4) . . ? S8 Fe5 S4 116.16(9) . . ? S8 Fe5 S6 118.51(10) . . ? S4 Fe5 S6 108.67(9) . . ? S8 Fe5 S7 103.11(9) . . ? S4 Fe5 S7 105.08(9) . . ? S6 Fe5 S7 103.40(9) . . ? S8 Fe5 Fe2 52.79(7) . . ? S4 Fe5 Fe2 143.34(8) . . ? S6 Fe5 Fe2 106.20(8) . . ? S7 Fe5 Fe2 55.22(6) . . ? S8 Fe5 Fe4 138.22(9) . . ? S4 Fe5 Fe4 53.02(7) . . ? S6 Fe5 Fe4 102.09(7) . . ? S7 Fe5 Fe4 55.02(6) . . ? Fe2 Fe5 Fe4 108.63(6) . . ? S8 Fe5 Mo2 155.25(8) . . ? S4 Fe5 Mo2 55.65(6) . . ? S6 Fe5 Mo2 55.21(6) . . ? S7 Fe5 Mo2 101.64(7) . . ? Fe2 Fe5 Mo2 148.97(5) . . ? Fe4 Fe5 Mo2 59.39(4) . . ? S8 Fe5 Fe6 139.89(8) . . ? S4 Fe5 Fe6 102.54(7) . . ? S6 Fe5 Fe6 52.36(6) . . ? S7 Fe5 Fe6 54.26(6) . . ? Fe2 Fe5 Fe6 89.84(5) . . ? Fe4 Fe5 Fe6 60.57(4) . . ? Mo2 Fe5 Fe6 59.16(4) . . ? S9 Fe6 S5 117.82(9) . . ? S9 Fe6 S6 115.32(10) . . ? S5 Fe6 S6 110.44(9) . . ? S9 Fe6 S7 104.35(9) . . ? S5 Fe6 S7 102.65(9) . . ? S6 Fe6 S7 104.19(9) . . ? S9 Fe6 Fe3 52.71(7) . . ? S5 Fe6 Fe3 142.98(9) . . ? S6 Fe6 Fe3 104.66(7) . . ? S7 Fe6 Fe3 56.41(6) . . ? S9 Fe6 Mo2 152.66(8) . . ? S5 Fe6 Mo2 56.28(6) . . ? S6 Fe6 Mo2 55.64(6) . . ? S7 Fe6 Mo2 102.95(7) . . ? Fe3 Fe6 Mo2 149.78(5) . . ? S9 Fe6 Fe4 142.63(9) . . ? S5 Fe6 Fe4 52.56(6) . . ? S6 Fe6 Fe4 100.62(7) . . ? S7 Fe6 Fe4 54.46(6) . . ? Fe3 Fe6 Fe4 110.06(6) . . ? Mo2 Fe6 Fe4 59.07(4) . . ? S9 Fe6 Fe5 139.03(8) . . ? S5 Fe6 Fe5 102.08(7) . . ? S6 Fe6 Fe5 52.45(6) . . ? S7 Fe6 Fe5 55.01(6) . . ? Fe3 Fe6 Fe5 89.92(5) . . ? Mo2 Fe6 Fe5 60.05(4) . . ? Fe4 Fe6 Fe5 58.73(4) . . ? Fe2 S1 Fe1 73.67(8) . . ? Fe2 S1 Mo1 71.58(7) . . ? Fe1 S1 Mo1 71.61(7) . . ? Fe1 S2 Fe3 72.66(8) . . ? Fe1 S2 Mo1 71.86(7) . . ? Fe3 S2 Mo1 71.90(7) . . ? Fe3 S3 Fe2 74.97(8) . . ? Fe3 S3 Mo1 72.40(8) . . ? Fe2 S3 Mo1 71.97(7) . . ? Fe5 S4 Fe4 73.95(8) . . ? Fe5 S4 Mo2 72.73(7) . . ? Fe4 S4 Mo2 71.44(7) . . ? Fe6 S5 Fe4 75.28(8) . . ? Fe6 S5 Mo2 71.77(7) . . ? Fe4 S5 Mo2 71.03(7) . . ? Fe6 S6 Fe5 75.20(8) . . ? Fe6 S6 Mo2 72.00(7) . . ? Fe5 S6 Mo2 72.71(7) . . ? Fe4 S7 Fe6 71.03(7) . . ? Fe4 S7 Fe2 135.09(11) . . ? Fe6 S7 Fe2 108.46(10) . . ? Fe4 S7 Fe1 143.97(12) . . ? Fe6 S7 Fe1 133.66(10) . . ? Fe2 S7 Fe1 69.47(7) . . ? Fe4 S7 Fe5 69.14(8) . . ? Fe6 S7 Fe5 70.72(8) . . ? Fe2 S7 Fe5 68.79(7) . . ? Fe1 S7 Fe5 137.01(10) . . ? Fe4 S7 Fe3 137.93(10) . . ? Fe6 S7 Fe3 68.41(7) . . ? Fe2 S7 Fe3 70.23(7) . . ? Fe1 S7 Fe3 67.78(7) . . ? Fe5 S7 Fe3 106.54(10) . . ? Fe5 S8 Fe2 74.45(7) . . ? Fe3 S9 Fe6 74.35(7) . . ? C19 S10 Fe1 108.3(4) . . ? C25 S11 Fe4 104.9(4) . . ? C1 N1 N2 105.1(8) . . ? C1 N1 Mo1 133.1(7) . . ? N2 N1 Mo1 121.8(7) . . ? C3 N2 N1 109.9(9) . . ? C3 N2 B1 130.1(10) . . ? N1 N2 B1 119.9(8) . . ? C4 N3 N4 106.0(7) . . ? C4 N3 Mo1 132.8(6) . . ? N4 N3 Mo1 121.2(6) . . ? C6 N4 N3 108.0(8) . . ? C6 N4 B1 132.1(9) . . ? N3 N4 B1 119.7(8) . . ? C7 N5 N6 105.4(7) . . ? C7 N5 Mo1 133.0(7) . . ? N6 N5 Mo1 121.2(5) . . ? C9 N6 N5 108.7(8) . . ? C9 N6 B1 131.5(9) . . ? N5 N6 B1 119.8(7) . . ? C10 N7 N8 108.6(7) . . ? C10 N7 Mo2 130.8(6) . . ? N8 N7 Mo2 120.6(5) . . ? C12 N8 N7 107.8(8) . . ? C12 N8 B2 130.1(9) . . ? N7 N8 B2 122.1(7) . . ? C13 N9 N10 106.0(7) . . ? C13 N9 Mo2 130.8(7) . . ? N10 N9 Mo2 123.0(5) . . ? C15 N10 N9 110.0(8) . . ? C15 N10 B2 130.5(8) . . ? N9 N10 B2 119.6(7) . . ? C16 N11 N12 105.6(7) . . ? C16 N11 Mo2 131.0(7) . . ? N12 N11 Mo2 122.9(6) . . ? C18 N12 N11 109.4(7) . . ? C18 N12 B2 131.2(9) . . ? N11 N12 B2 119.3(8) . . ? C35 N13 C31 108.3(7) . . ? C35 N13 C33 111.4(7) . . ? C31 N13 C33 109.9(7) . . ? C35 N13 C37 110.8(7) . . ? C31 N13 C37 110.5(7) . . ? C33 N13 C37 105.9(6) . . ? C41 N14 C39 114.1(9) . . ? C41 N14 C45 107.7(7) . . ? C39 N14 C45 110.1(8) . . ? C41 N14 C43 109.9(8) . . ? C39 N14 C43 105.2(7) . . ? C45 N14 C43 109.7(8) . . ? C49 N15 C47 110.7(8) . . ? C49 N15 C51 106.2(8) . . ? C47 N15 C51 111.0(8) . . ? C49 N15 C53 111.4(8) . . ? C47 N15 C53 106.7(7) . . ? C51 N15 C53 110.8(7) . . ? N6 B1 N2 109.4(9) . . ? N6 B1 N4 109.6(9) . . ? N2 B1 N4 108.5(9) . . ? N8 B2 N10 109.8(8) . . ? N8 B2 N12 109.3(8) . . ? N10 B2 N12 105.9(8) . . ? N1 C1 C2 111.6(10) . . ? C3 C2 C1 105.7(10) . . ? C2 C3 N2 107.6(10) . . ? N3 C4 C5 112.3(9) . . ? C6 C5 C4 103.9(9) . . ? N4 C6 C5 109.8(9) . . ? N5 C7 C8 111.9(9) . . ? C9 C8 C7 105.0(9) . . ? N6 C9 C8 109.0(9) . . ? N7 C10 C11 108.2(8) . . ? C12 C11 C10 106.1(9) . . ? N8 C12 C11 109.3(9) . . ? N9 C13 C14 109.8(9) . . ? C15 C14 C13 105.3(8) . . ? N10 C15 C14 108.9(8) . . ? N11 C16 C17 111.5(9) . . ? C18 C17 C16 104.4(9) . . ? N12 C18 C17 109.1(9) . . ? C20 C19 C24 117.0(10) . . ? C20 C19 S10 123.8(9) . . ? C24 C19 S10 119.0(9) . . ? C19 C20 C21 122.1(11) . . ? C22 C21 C20 121.4(12) . . ? C21 C22 C23 116.0(12) . . ? C24 C23 C22 121.9(13) . . ? C23 C24 C19 121.4(12) . . ? C30 C25 C26 127.7(19) . . ? C30 C25 S11 109.5(17) . . ? C26 C25 S11 122.0(10) . . ? C25 C26 C27 123.5(14) . . ? C32 C31 N13 116.1(8) . . ? N13 C33 C34 113.6(7) . . ? N13 C35 C36 116.4(8) . . ? N13 C37 C38 115.2(7) . . ? N14 C39 C40 112.7(8) . . ? N14 C41 C42 117.7(8) . . ? C44 C43 N14 114.6(8) . . ? N14 C45 C46 115.7(8) . . ? N15 C47 C48 114.0(8) . . ? N15 C49 C50 114.9(9) . . ? C52 C51 N15 114.7(9) . . ? C54 C53 N15 115.3(8) . . ? C56 C55 N16 179(3) . . ? N17 C57 C58 161(3) . . ? C60 C59 N18 172(4) . . ? N19 C61 C62 176.9(14) . . ? N51 C63 C64 77(4) . . ? N51 C63 N20 33(3) . . ? C64 C63 N20 102(5) . . ? N21 C68 C67 99(6) . . ? C30 C29 C28 139(4) . . ? C29 C30 C25 103(4) . . ? C27 C28 C29 113.4(19) . . ? C28 C27 C26 111.3(16) . . ? N20 N51 C63 73(5) . . ? N51 N20 C63 73(5) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.137 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.098 #--------------------------------END data_(Et4N)2.75[Tp2Mo2Fe6S8.75(SEt)2.25]2.5MeCN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ' not measured' _chemical_formula_moiety (Et4N)2.75[Tp2Mo2Fe6S8.75(SEt)2.25]2.5MeCN _chemical_formula_sum 'C48.50 H93.75 B2 Fe6 Mo2 N18 S11' _chemical_formula_weight 1812.97 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' 'B' 'B' 0.0013 0.0007 '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' 'Fe' 'Fe' 0.3463 0.8444 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.938(4) _cell_length_b 17.094(4) _cell_length_c 18.600(5) _cell_angle_alpha 79.331(5) _cell_angle_beta 78.884(5) _cell_angle_gamma 64.905(5) _cell_volume 4191.6(18) _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 ? _exptl_crystal_colour 'Dark green ' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1926 _exptl_absorpt_coefficient_mu 1.614 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ? _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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23553 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14667 _reflns_number_gt 8652 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0905P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14667 _refine_ls_number_parameters 812 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0990 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.818 _refine_ls_shift/su_mean 0.011 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 0.54200(4) 0.63845(4) 0.21448(4) 0.04430(19) Uani 1 1 d . . . Mo2 Mo -0.00062(5) 0.91711(4) 0.26998(4) 0.0508(2) Uani 1 1 d . . . Fe1 Fe 0.40659(7) 0.56553(6) 0.25090(6) 0.0408(3) Uani 1 1 d . A . Fe2 Fe 0.36108(8) 0.71230(6) 0.16259(6) 0.0447(3) Uani 1 1 d . . . Fe3 Fe 0.37029(7) 0.71006(7) 0.30431(7) 0.0496(3) Uani 1 1 d . . . Fe4 Fe 0.06609(7) 0.74213(6) 0.29209(6) 0.0433(3) Uani 1 1 d . . . Fe5 Fe 0.16066(8) 0.81509(6) 0.18423(6) 0.0461(3) Uani 1 1 d . . . Fe6 Fe 0.17287(7) 0.81592(7) 0.32426(6) 0.0455(3) Uani 1 1 d . . . S1 S 0.48322(14) 0.58162(12) 0.13435(11) 0.0451(5) Uani 1 1 d . . . S2 S 0.49194(14) 0.57851(13) 0.33350(11) 0.0499(5) Uani 1 1 d . . . S3 S 0.42946(14) 0.78550(12) 0.20831(13) 0.0551(5) Uani 1 1 d . . . S4 S 0.00542(16) 0.82267(13) 0.18727(13) 0.0584(6) Uani 1 1 d . . . S5 S 0.02259(15) 0.82662(12) 0.38381(12) 0.0540(5) Uani 1 1 d . . . S6 S 0.15364(15) 0.92893(12) 0.23435(13) 0.0535(5) Uani 1 1 d . . . S7 S 0.26033(17) 0.79179(13) 0.07531(12) 0.0583(5) Uani 1 1 d . . . S8 S 0.2832(2) 0.7787(3) 0.4076(2) 0.0595(9) Uani 0.75 1 d P . . S81 S 0.2966(7) 0.8206(7) 0.3808(6) 0.051(2) Uani 0.25 1 d P . . S9 S 0.24423(13) 0.68538(11) 0.26271(10) 0.0401(4) Uani 1 1 d . . . S10 S 0.35802(16) 0.45206(13) 0.27677(13) 0.0583(6) Uani 1 1 d . . . S11 S 0.01558(14) 0.63212(12) 0.34023(12) 0.0497(5) Uani 1 1 d . . . N1 N 0.6850(4) 0.5169(4) 0.2119(4) 0.0492(16) Uani 1 1 d . . . N2 N 0.7763(4) 0.5201(4) 0.1956(4) 0.0590(19) Uani 1 1 d . . . N3 N 0.6319(5) 0.6773(4) 0.1142(4) 0.0550(18) Uani 1 1 d . . . N4 N 0.7304(5) 0.6610(4) 0.1143(4) 0.064(2) Uani 1 1 d . . . N5 N 0.6340(4) 0.6776(4) 0.2707(4) 0.0536(17) Uani 1 1 d . . . N6 N 0.7337(4) 0.6588(4) 0.2468(4) 0.0583(19) Uani 1 1 d . . . N7 N -0.1628(5) 0.9480(4) 0.2984(5) 0.081(3) Uani 1 1 d . . . N8 N -0.2337(6) 1.0324(5) 0.2971(7) 0.108(4) Uani 1 1 d . . . N9 N -0.0621(7) 1.0278(5) 0.1820(6) 0.089(3) Uani 1 1 d . . . N10 N -0.1471(8) 1.1012(5) 0.2004(8) 0.121(5) Uani 1 1 d . . . N11 N -0.0464(5) 1.0284(4) 0.3361(5) 0.072(2) Uani 1 1 d . . . N12 N -0.1328(6) 1.1013(5) 0.3283(6) 0.099(3) Uani 1 1 d . . . N13 N 0.2266(5) 0.5526(4) 0.0328(4) 0.0549(17) Uani 1 1 d . . . N14 N 0.2305(5) 0.5349(5) 0.5228(4) 0.068(2) Uani 1 1 d . . . N15 N 0.3216(11) 0.0098(10) 0.9460(9) 0.120(5) Uiso 0.75 1 d P . . N16 N 0.0862(12) 0.2727(11) 0.1170(10) 0.205(8) Uani 1 1 d . . . N31 N 0.390(3) -0.024(3) 0.308(2) 0.255(19) Uiso 0.50 1 d P . . N111 N 0.201(2) 0.040(2) 0.499(2) 0.192(15) Uani 0.50 1 d P . . B1 B 0.7857(8) 0.6104(6) 0.1790(7) 0.066(3) Uani 1 1 d . . . B2 B -0.2033(10) 1.1081(8) 0.2752(12) 0.111(6) Uani 1 1 d . . . C1 C 0.7019(6) 0.4330(5) 0.2257(5) 0.054(2) Uani 1 1 d . . . H1 H 0.6523 0.4117 0.2379 0.064 Uiso 1 1 calc R . . C2 C 0.8021(6) 0.3820(5) 0.2195(5) 0.065(2) Uani 1 1 d . . . H2 H 0.8328 0.3216 0.2265 0.078 Uiso 1 1 calc R . . C3 C 0.8485(6) 0.4406(5) 0.2003(5) 0.065(2) Uani 1 1 d . . . H3 H 0.9167 0.4265 0.1925 0.077 Uiso 1 1 calc R . . C4 C 0.6061(7) 0.7233(5) 0.0508(5) 0.065(2) Uani 1 1 d . . . H4 H 0.5428 0.7434 0.0368 0.077 Uiso 1 1 calc R . . C5 C 0.6850(8) 0.7377(6) 0.0078(6) 0.071(3) Uani 1 1 d . . . H5 H 0.6858 0.7680 -0.0392 0.086 Uiso 1 1 calc R . . C6 C 0.7620(7) 0.6975(6) 0.0496(6) 0.072(3) Uani 1 1 d . . . H6 H 0.8260 0.6957 0.0356 0.086 Uiso 1 1 calc R . . C7 C 0.6098(6) 0.7217(5) 0.3268(5) 0.060(2) Uani 1 1 d . . . H7 H 0.5462 0.7433 0.3529 0.072 Uiso 1 1 calc R . . C8 C 0.6918(6) 0.7325(5) 0.3428(5) 0.060(2) Uani 1 1 d . . . H8 H 0.6948 0.7598 0.3805 0.072 Uiso 1 1 calc R . . C9 C 0.7669(6) 0.6925(5) 0.2888(5) 0.063(2) Uani 1 1 d . . . H9 H 0.8314 0.6896 0.2828 0.076 Uiso 1 1 calc R . . C10 C -0.2121(7) 0.8968(6) 0.3161(7) 0.100(4) Uani 1 1 d . . . H10 H -0.1834 0.8365 0.3182 0.120 Uiso 1 1 calc R . . C11 C -0.3144(8) 0.9481(7) 0.3313(10) 0.146(7) Uani 1 1 d . . . H11 H -0.3657 0.9293 0.3473 0.176 Uiso 1 1 calc R . . C12 C -0.3216(8) 1.0303(7) 0.3175(10) 0.142(7) Uani 1 1 d . . . H12 H -0.3812 1.0793 0.3218 0.171 Uiso 1 1 calc R . . C13 C -0.0285(11) 1.0333(7) 0.1083(9) 0.119(5) Uani 1 1 d . . . H13 H 0.0268 0.9906 0.0854 0.143 Uiso 1 1 calc R . . C14 C -0.0901(16) 1.1133(12) 0.0716(14) 0.178(11) Uani 1 1 d . . . H14 H -0.0837 1.1355 0.0222 0.214 Uiso 1 1 calc R . . C15 C -0.1589(13) 1.1478(11) 0.1262(13) 0.152(10) Uani 1 1 d . . . H15 H -0.2133 1.2001 0.1178 0.182 Uiso 1 1 calc R . . C16 C -0.0054(8) 1.0370(6) 0.3909(7) 0.084(3) Uani 1 1 d . . . H16 H 0.0542 0.9967 0.4071 0.100 Uiso 1 1 calc R . . C17 C -0.0648(11) 1.1147(8) 0.4195(9) 0.117(5) Uani 1 1 d . . . H17 H -0.0540 1.1366 0.4577 0.141 Uiso 1 1 calc R . . C18 C -0.1423(10) 1.1518(7) 0.3794(10) 0.126(6) Uani 1 1 d . . . H18 H -0.1952 1.2052 0.3862 0.152 Uiso 1 1 calc R . . C19 C 0.4793(12) 0.3576(8) 0.2650(10) 0.114(5) Uani 1 1 d . A 1 H19A H 0.5090 0.3616 0.2140 0.137 Uiso 1 1 calc R A 1 H19B H 0.5236 0.3604 0.2955 0.137 Uiso 1 1 calc R A 1 C20 C 0.472(2) 0.2787(13) 0.283(2) 0.27(2) Uani 0.70 1 d P A 1 H20A H 0.4922 0.2539 0.3314 0.400 Uiso 0.70 1 calc PR A 1 H20B H 0.5140 0.2402 0.2477 0.400 Uiso 0.70 1 calc PR A 1 H20C H 0.4039 0.2869 0.2842 0.400 Uiso 0.70 1 calc PR A 1 C201 C 0.510(6) 0.330(5) 0.316(3) 0.15(3) Uani 0.30 1 d P B 2 C21 C 0.0647(7) 0.5596(5) 0.2703(5) 0.066(2) Uani 1 1 d . . . H21A H 0.0372 0.5900 0.2250 0.080 Uiso 1 1 calc R . . H21B H 0.1365 0.5406 0.2607 0.080 Uiso 1 1 calc R . . C22 C 0.0394(9) 0.4816(6) 0.2939(6) 0.101(4) Uani 1 1 d . . . H22A H 0.0727 0.4478 0.3356 0.151 Uiso 1 1 calc R . . H22B H 0.0606 0.4467 0.2540 0.151 Uiso 1 1 calc R . . H22C H -0.0314 0.5005 0.3073 0.151 Uiso 1 1 calc R . . C23 C 0.1785(7) 0.4937(6) 0.0229(5) 0.070(3) Uani 1 1 d . . . H23A H 0.1359 0.5222 -0.0156 0.084 Uiso 1 1 calc R . . H23B H 0.2307 0.4407 0.0058 0.084 Uiso 1 1 calc R . . C24 C 0.1181(8) 0.4692(7) 0.0896(6) 0.099(4) Uani 1 1 d . . . H24A H 0.1591 0.4410 0.1285 0.148 Uiso 1 1 calc R . . H24B H 0.0932 0.4304 0.0779 0.148 Uiso 1 1 calc R . . H24C H 0.0632 0.5206 0.1053 0.148 Uiso 1 1 calc R . . C25 C 0.2808(6) 0.5686(6) -0.0417(5) 0.063(2) Uani 1 1 d . . . H25A H 0.2321 0.6004 -0.0757 0.076 Uiso 1 1 calc R . . H25B H 0.3232 0.5129 -0.0594 0.076 Uiso 1 1 calc R . . C26 C 0.3444(6) 0.6184(6) -0.0436(5) 0.069(3) Uani 1 1 d . . . H26A H 0.3050 0.6712 -0.0217 0.103 Uiso 1 1 calc R . . H26B H 0.3688 0.6322 -0.0939 0.103 Uiso 1 1 calc R . . H26C H 0.3997 0.5835 -0.0166 0.103 Uiso 1 1 calc R . . C27 C 0.1474(6) 0.6390(5) 0.0611(5) 0.066(2) Uani 1 1 d . . . H27A H 0.1215 0.6256 0.1116 0.079 Uiso 1 1 calc R . . H27B H 0.1811 0.6764 0.0620 0.079 Uiso 1 1 calc R . . C28 C 0.0627(8) 0.6885(7) 0.0195(7) 0.111(4) Uani 1 1 d . . . H28A H 0.0864 0.6931 -0.0322 0.166 Uiso 1 1 calc R . . H28B H 0.0277 0.7456 0.0349 0.166 Uiso 1 1 calc R . . H28C H 0.0185 0.6592 0.0286 0.166 Uiso 1 1 calc R . . C29 C 0.2993(7) 0.5098(6) 0.0913(5) 0.074(3) Uani 1 1 d . . . H29A H 0.3274 0.5502 0.0960 0.089 Uiso 1 1 calc R . . H29B H 0.2611 0.5017 0.1384 0.089 Uiso 1 1 calc R . . C30 C 0.3832(7) 0.4246(7) 0.0775(6) 0.091(3) Uani 1 1 d . . . H30A H 0.3569 0.3827 0.0757 0.136 Uiso 1 1 calc R . . H30B H 0.4241 0.4050 0.1166 0.136 Uiso 1 1 calc R . . H30C H 0.4225 0.4314 0.0313 0.136 Uiso 1 1 calc R . . C31 C 0.2602(8) 0.5477(9) 0.5912(6) 0.105(4) Uani 1 1 d . . . H31A H 0.3071 0.4923 0.6118 0.126 Uiso 1 1 calc R . . H31B H 0.2017 0.5674 0.6275 0.126 Uiso 1 1 calc R . . C32 C 0.3074(10) 0.6129(8) 0.5763(7) 0.125(5) Uani 1 1 d . . . H32A H 0.2561 0.6708 0.5741 0.187 Uiso 1 1 calc R . . H32B H 0.3501 0.6054 0.5301 0.187 Uiso 1 1 calc R . . H32C H 0.3458 0.6040 0.6152 0.187 Uiso 1 1 calc R . . C33 C 0.3125(8) 0.5124(7) 0.4617(5) 0.086(3) Uani 1 1 d . . . H33A H 0.3352 0.5592 0.4484 0.104 Uiso 1 1 calc R . . H33B H 0.2878 0.5070 0.4191 0.104 Uiso 1 1 calc R . . C34 C 0.4029(8) 0.4255(7) 0.4817(6) 0.095(4) Uani 1 1 d . . . H34A H 0.4210 0.4270 0.5281 0.142 Uiso 1 1 calc R . . H34B H 0.4585 0.4190 0.4440 0.142 Uiso 1 1 calc R . . H34C H 0.3845 0.3773 0.4854 0.142 Uiso 1 1 calc R . . C35 C 0.1882(9) 0.4673(8) 0.5463(7) 0.115(5) Uani 1 1 d . . . H35A H 0.1303 0.4889 0.5828 0.138 Uiso 1 1 calc R . . H35B H 0.2374 0.4155 0.5697 0.138 Uiso 1 1 calc R . . C37 C 0.1511(7) 0.6196(7) 0.4927(6) 0.094(4) Uani 1 1 d . . . H37A H 0.1793 0.6628 0.4787 0.113 Uiso 1 1 calc R . . H37B H 0.1334 0.6102 0.4486 0.113 Uiso 1 1 calc R . . C38 C 0.0578(8) 0.6553(8) 0.5459(7) 0.130(6) Uani 1 1 d . . . H38A H 0.0265 0.6149 0.5575 0.195 Uiso 1 1 calc R . . H38B H 0.0128 0.7098 0.5239 0.195 Uiso 1 1 calc R . . H38C H 0.0745 0.6639 0.5903 0.195 Uiso 1 1 calc R . . C39 C 0.0771(9) 0.2254(8) 0.1601(9) 0.110(5) Uani 1 1 d . . . C40 C 0.0541(11) 0.1632(8) 0.2135(14) 0.259(15) Uani 1 1 d . . . H40A H -0.0137 0.1719 0.2133 0.388 Uiso 1 1 calc R . . H40B H 0.0627 0.1700 0.2615 0.388 Uiso 1 1 calc R . . H40C H 0.0978 0.1056 0.2017 0.388 Uiso 1 1 calc R . . C44 C 0.3904(13) 0.0577(11) 0.9107(10) 0.115(5) Uiso 0.75 1 d P . . H44A H 0.3881 0.0941 0.9458 0.138 Uiso 0.75 1 calc PR . . H44B H 0.4582 0.0142 0.9038 0.138 Uiso 0.75 1 calc PR . . C45 C 0.1998(13) 0.0974(12) 0.9597(11) 0.130(6) Uiso 0.75 1 d P . . H45A H 0.2036 0.1407 0.9847 0.156 Uiso 0.75 1 calc PR . . H45B H 0.1771 0.1251 0.9123 0.156 Uiso 0.75 1 calc PR . . C46 C 0.3694(14) 0.1110(12) 0.8414(11) 0.140(7) Uiso 0.75 1 d P . . H46A H 0.3000 0.1303 0.8369 0.210 Uiso 0.75 1 calc PR . . H46B H 0.4092 0.0777 0.8017 0.210 Uiso 0.75 1 calc PR . . H46C H 0.3848 0.1605 0.8394 0.210 Uiso 0.75 1 calc PR . . C55 C 0.1585(9) 0.4430(8) 0.4837(8) 0.117(5) Uani 1 1 d . . . H55A H 0.1144 0.4946 0.4575 0.175 Uiso 1 1 calc R . . H55B H 0.1251 0.4049 0.5029 0.175 Uiso 1 1 calc R . . H55C H 0.2169 0.4140 0.4508 0.175 Uiso 1 1 calc R . . C54 C 0.1357(19) 0.0665(16) 0.9997(15) 0.203(11) Uiso 0.75 1 d P . . H54A H 0.0879 0.0709 0.9697 0.304 Uiso 0.75 1 calc PR . . H54B H 0.1019 0.0997 1.0406 0.304 Uiso 0.75 1 calc PR . . H54C H 0.1709 0.0067 1.0179 0.304 Uiso 0.75 1 calc PR . . C112 C 0.233(5) 0.153(4) 0.405(4) 0.32(4) Uani 0.50 1 d P . . H11A H 0.2539 0.1789 0.4361 0.482 Uiso 0.50 1 calc PR . . H11B H 0.1955 0.1969 0.3691 0.482 Uiso 0.50 1 calc PR . . H11C H 0.2899 0.1100 0.3801 0.482 Uiso 0.50 1 calc PR . . C114 C 0.184(2) 0.121(4) 0.439(4) 0.25(3) Uani 0.50 1 d P . . C121 C 0.3318(18) 0.0160(16) 1.0856(14) 0.201(11) Uiso 0.75 1 d P . . H12A H 0.3892 0.0295 1.0790 0.301 Uiso 0.75 1 calc PR . . H12B H 0.3231 -0.0110 1.1350 0.301 Uiso 0.75 1 calc PR . . H12C H 0.2737 0.0686 1.0773 0.301 Uiso 0.75 1 calc PR . . C122 C 0.3483(19) -0.0535(17) 1.0242(14) 0.196(11) Uiso 0.75 1 d P . . H12D H 0.4165 -0.0965 1.0190 0.235 Uiso 0.75 1 calc PR . . H12E H 0.3039 -0.0833 1.0399 0.235 Uiso 0.75 1 calc PR . . C123 C 0.285(3) -0.034(3) 0.912(2) 0.33(2) Uiso 0.75 1 d P . . H12F H 0.2624 -0.0024 0.8656 0.395 Uiso 0.75 1 calc PR . . H12G H 0.2325 -0.0469 0.9438 0.395 Uiso 0.75 1 calc PR . . C124 C 0.4029(19) -0.1321(16) 0.8996(15) 0.208(11) Uiso 0.75 1 d P . . H12H H 0.4587 -0.1165 0.8934 0.312 Uiso 0.75 1 calc PR . . H12I H 0.4042 -0.1566 0.8567 0.312 Uiso 0.75 1 calc PR . . H12J H 0.4064 -0.1742 0.9422 0.312 Uiso 0.75 1 calc PR . . C154 C 0.322(2) 0.863(3) 0.411(2) 0.12(2) Uani 0.25 1 d PD . . C155 C 0.383(3) 0.846(4) 0.475(2) 0.14(3) Uani 0.25 1 d PD . . C156 C 0.341(3) 0.023(3) 0.256(2) 0.173(14) Uiso 0.50 1 d P . . C159 C 0.364(4) 0.103(3) 0.199(3) 0.24(2) Uiso 0.50 1 d P . . 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 0.0336(3) 0.0465(4) 0.0549(5) -0.0142(3) -0.0012(3) -0.0166(3) Mo2 0.0417(4) 0.0316(3) 0.0765(6) 0.0020(3) -0.0211(3) -0.0100(3) Fe1 0.0356(5) 0.0422(5) 0.0426(7) -0.0060(5) -0.0038(5) -0.0139(5) Fe2 0.0443(6) 0.0440(6) 0.0480(7) -0.0072(5) -0.0029(5) -0.0206(5) Fe3 0.0333(6) 0.0573(7) 0.0570(8) -0.0184(6) -0.0083(5) -0.0112(5) Fe4 0.0395(6) 0.0343(5) 0.0540(7) 0.0003(5) -0.0128(5) -0.0121(5) Fe5 0.0525(7) 0.0391(6) 0.0477(7) -0.0003(5) -0.0132(5) -0.0184(5) Fe6 0.0373(6) 0.0434(6) 0.0516(7) -0.0107(5) -0.0114(5) -0.0078(5) S1 0.0445(10) 0.0492(10) 0.0447(12) -0.0114(9) 0.0020(8) -0.0227(9) S2 0.0367(10) 0.0641(12) 0.0466(13) -0.0068(10) -0.0091(9) -0.0162(9) S3 0.0453(11) 0.0447(10) 0.0791(16) -0.0171(10) -0.0058(10) -0.0188(9) S4 0.0647(13) 0.0455(11) 0.0728(16) 0.0090(10) -0.0373(11) -0.0241(10) S5 0.0489(11) 0.0440(10) 0.0594(14) -0.0074(9) -0.0008(10) -0.0115(9) S6 0.0519(12) 0.0405(10) 0.0719(15) -0.0066(10) -0.0102(10) -0.0214(9) S7 0.0738(14) 0.0585(12) 0.0425(13) 0.0059(10) -0.0143(10) -0.0285(11) S8 0.0467(18) 0.075(2) 0.054(2) -0.0205(18) -0.0096(16) -0.0154(18) S81 0.032(4) 0.062(6) 0.048(6) -0.016(5) -0.005(4) -0.003(4) S9 0.0351(9) 0.0386(9) 0.0426(11) -0.0021(8) -0.0093(8) -0.0103(8) S10 0.0568(13) 0.0571(12) 0.0606(15) -0.0042(10) -0.0037(10) -0.0250(11) S11 0.0448(11) 0.0496(11) 0.0546(13) 0.0018(9) -0.0087(9) -0.0211(9) N1 0.039(3) 0.045(4) 0.065(5) -0.015(3) -0.005(3) -0.017(3) N2 0.038(4) 0.059(4) 0.081(5) -0.023(4) 0.004(3) -0.019(3) N3 0.043(4) 0.052(4) 0.071(5) -0.011(4) 0.006(3) -0.024(3) N4 0.053(4) 0.064(4) 0.082(6) -0.024(4) 0.012(4) -0.034(4) N5 0.034(3) 0.057(4) 0.075(5) -0.023(4) -0.009(3) -0.016(3) N6 0.033(3) 0.058(4) 0.090(6) -0.020(4) -0.006(3) -0.020(3) N7 0.042(4) 0.041(4) 0.153(8) -0.002(4) -0.024(5) -0.010(3) N8 0.042(5) 0.044(4) 0.229(12) -0.010(6) -0.036(6) -0.004(4) N9 0.105(7) 0.052(5) 0.128(9) 0.038(5) -0.083(6) -0.041(5) N10 0.087(7) 0.039(5) 0.245(15) 0.046(7) -0.106(9) -0.024(5) N11 0.047(4) 0.039(4) 0.120(7) -0.019(4) 0.006(4) -0.010(3) N12 0.050(5) 0.038(4) 0.192(11) -0.020(5) -0.003(6) -0.006(4) N13 0.051(4) 0.063(4) 0.056(5) -0.021(3) 0.001(3) -0.024(3) N14 0.045(4) 0.102(6) 0.043(4) 0.015(4) -0.010(3) -0.025(4) N16 0.189(15) 0.219(17) 0.215(18) 0.056(14) -0.002(12) -0.134(14) N111 0.13(2) 0.18(3) 0.26(4) -0.05(3) 0.04(2) -0.07(2) B1 0.055(6) 0.052(6) 0.097(9) -0.017(6) -0.009(6) -0.023(5) B2 0.056(8) 0.058(7) 0.21(2) 0.015(10) -0.036(10) -0.020(6) C1 0.046(5) 0.056(5) 0.062(6) -0.014(4) -0.006(4) -0.020(4) C2 0.057(5) 0.048(5) 0.084(7) -0.012(4) -0.015(5) -0.012(4) C3 0.038(4) 0.058(5) 0.086(7) -0.028(5) -0.004(4) -0.001(4) C4 0.068(6) 0.053(5) 0.075(7) -0.014(5) 0.007(5) -0.031(5) C5 0.094(7) 0.066(6) 0.066(7) -0.007(5) 0.011(6) -0.051(6) C6 0.068(6) 0.066(6) 0.093(8) -0.027(5) 0.024(6) -0.045(5) C7 0.053(5) 0.047(4) 0.082(7) -0.017(4) -0.007(4) -0.019(4) C8 0.051(5) 0.050(5) 0.088(7) -0.015(5) -0.021(5) -0.021(4) C9 0.045(5) 0.047(5) 0.103(8) -0.005(5) -0.020(5) -0.021(4) C10 0.045(5) 0.049(5) 0.195(14) -0.006(7) -0.023(7) -0.011(5) C11 0.055(7) 0.075(8) 0.30(2) 0.010(10) -0.039(9) -0.028(6) C12 0.046(6) 0.065(7) 0.30(2) -0.023(10) -0.035(9) -0.001(6) C13 0.161(13) 0.075(8) 0.145(13) 0.055(8) -0.096(11) -0.065(8) C14 0.22(2) 0.113(16) 0.24(3) 0.105(16) -0.15(2) -0.099(17) C15 0.134(14) 0.076(10) 0.27(3) 0.088(14) -0.151(16) -0.059(11) C16 0.086(7) 0.061(6) 0.108(9) -0.032(6) -0.009(6) -0.026(6) C17 0.108(10) 0.079(8) 0.158(14) -0.063(9) 0.020(10) -0.027(8) C18 0.083(9) 0.051(6) 0.232(18) -0.062(9) 0.033(10) -0.020(6) C19 0.110(10) 0.067(8) 0.150(16) 0.003(10) -0.011(12) -0.029(7) C20 0.18(3) 0.058(14) 0.49(6) -0.05(2) -0.02(3) 0.024(15) C201 0.19(7) 0.22(7) 0.09(4) -0.10(5) 0.06(4) -0.13(6) C21 0.067(6) 0.070(6) 0.068(6) -0.011(5) 0.007(5) -0.039(5) C22 0.167(12) 0.086(7) 0.080(8) -0.010(6) 0.006(7) -0.089(8) C23 0.065(6) 0.074(6) 0.086(7) -0.034(5) 0.002(5) -0.036(5) C24 0.099(8) 0.100(8) 0.111(10) -0.043(7) 0.033(7) -0.061(7) C25 0.062(5) 0.088(6) 0.044(5) -0.019(5) 0.002(4) -0.033(5) C26 0.066(6) 0.075(6) 0.065(7) -0.012(5) 0.011(5) -0.035(5) C27 0.069(6) 0.061(5) 0.065(6) -0.025(5) 0.012(5) -0.025(5) C28 0.080(8) 0.084(8) 0.149(12) -0.001(8) -0.028(8) -0.013(7) C29 0.063(6) 0.095(7) 0.070(7) -0.016(6) -0.012(5) -0.033(6) C30 0.069(7) 0.095(8) 0.088(8) -0.021(6) -0.008(6) -0.011(6) C31 0.076(7) 0.146(11) 0.045(7) -0.006(7) -0.022(5) 0.003(7) C32 0.131(11) 0.126(11) 0.114(11) -0.047(9) -0.071(9) -0.013(9) C33 0.097(8) 0.132(9) 0.044(6) -0.022(6) 0.002(5) -0.058(8) C34 0.080(7) 0.114(9) 0.070(8) -0.022(6) 0.017(6) -0.025(7) C35 0.075(8) 0.115(10) 0.112(11) 0.053(8) -0.021(7) -0.022(7) C37 0.074(7) 0.116(9) 0.084(8) 0.040(7) -0.038(6) -0.039(7) C38 0.059(7) 0.134(11) 0.141(12) 0.045(9) 0.005(7) -0.017(7) C39 0.077(8) 0.079(8) 0.167(15) -0.003(8) -0.013(8) -0.031(7) C40 0.112(12) 0.060(8) 0.56(4) 0.079(15) -0.053(18) -0.031(9) C55 0.108(10) 0.103(9) 0.158(14) 0.036(9) -0.056(9) -0.064(8) C112 0.34(9) 0.34(8) 0.34(9) -0.12(6) 0.10(7) -0.22(7) C114 0.057(18) 0.25(6) 0.41(9) -0.22(6) 0.11(3) -0.03(3) C154 0.04(2) 0.16(4) 0.18(5) -0.16(4) -0.02(2) -0.01(2) C155 0.04(2) 0.23(6) 0.13(4) -0.16(4) -0.03(2) 0.03(3) _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 N5 2.241(6) . ? Mo1 N3 2.249(6) . ? Mo1 N1 2.261(6) . ? Mo1 S3 2.354(2) . ? Mo1 S2 2.384(2) . ? Mo1 S1 2.388(2) . ? Mo1 Fe3 2.7038(13) . ? Mo1 Fe1 2.7206(13) . ? Mo1 Fe2 2.7368(14) . ? Mo2 N7 2.225(7) . ? Mo2 N11 2.245(7) . ? Mo2 N9 2.250(8) . ? Mo2 S6 2.355(2) . ? Mo2 S5 2.369(2) . ? Mo2 S4 2.392(2) . ? Mo2 Fe4 2.6987(13) . ? Mo2 Fe6 2.6996(13) . ? Mo2 Fe5 2.7154(14) . ? Fe1 S2 2.271(2) . ? Fe1 S1 2.275(2) . ? Fe1 S10 2.288(2) . ? Fe1 S9 2.424(2) . ? Fe1 Fe2 2.6292(16) . ? Fe1 Fe3 2.6361(16) . ? Fe2 S7 2.267(2) . ? Fe2 S3 2.268(2) . ? Fe2 S1 2.281(2) . ? Fe2 S9 2.416(2) . ? Fe2 Fe3 2.6584(18) . ? Fe2 Fe5 2.7472(16) . ? Fe3 S2 2.262(2) . ? Fe3 S3 2.267(2) . ? Fe3 S8 2.310(4) . ? Fe3 S81 2.332(10) . ? Fe3 S9 2.383(2) . ? Fe3 Fe6 2.7219(15) . ? Fe4 S5 2.260(2) . ? Fe4 S4 2.269(2) . ? Fe4 S11 2.286(2) . ? Fe4 S9 2.401(2) . ? Fe4 Fe6 2.6167(15) . ? Fe4 Fe5 2.6554(15) . ? Fe5 S4 2.257(2) . ? Fe5 S7 2.261(2) . ? Fe5 S6 2.264(2) . ? Fe5 S9 2.400(2) . ? Fe5 Fe6 2.6487(17) . ? Fe6 S5 2.251(2) . ? Fe6 S6 2.265(2) . ? Fe6 S8 2.292(4) . ? Fe6 S81 2.332(10) . ? Fe6 S9 2.426(2) . ? S8 S81 0.868(10) . ? S8 C154 1.78(4) . ? S81 C154 1.20(3) . ? S10 C19 1.853(15) . ? S11 C21 1.796(9) . ? N1 C1 1.330(9) . ? N1 N2 1.362(8) . ? N2 C3 1.329(9) . ? N2 B1 1.578(11) . ? N3 C4 1.316(11) . ? N3 N4 1.376(9) . ? N4 C6 1.347(11) . ? N4 B1 1.507(14) . ? N5 C7 1.304(10) . ? N5 N6 1.382(8) . ? N6 C9 1.320(10) . ? N6 B1 1.531(13) . ? N7 C10 1.329(11) . ? N7 N8 1.380(9) . ? N8 C12 1.309(13) . ? N8 B2 1.508(15) . ? N9 C13 1.366(16) . ? N9 N10 1.394(14) . ? N10 C15 1.46(2) . ? N10 B2 1.48(2) . ? N11 C16 1.344(13) . ? N11 N12 1.372(9) . ? N12 C18 1.347(16) . ? N12 B2 1.53(2) . ? N13 C25 1.506(10) . ? N13 C23 1.515(10) . ? N13 C29 1.545(11) . ? N13 C27 1.556(9) . ? N14 C33 1.472(11) . ? N14 C35 1.500(14) . ? N14 C31 1.505(13) . ? N14 C37 1.521(11) . ? N15 C123 1.37(4) . ? N15 C44 1.553(19) . ? N15 C122 1.65(3) . ? N15 C45 1.81(2) . ? N16 C39 1.061(16) . ? N31 C156 1.26(5) . ? N111 C114 1.57(7) . ? C1 C2 1.370(11) . ? C2 C3 1.404(11) . ? C4 C5 1.380(11) . ? C5 C6 1.370(14) . ? C7 C8 1.406(11) . ? C8 C9 1.379(12) . ? C10 C11 1.404(14) . ? C11 C12 1.343(14) . ? C13 C14 1.42(2) . ? C14 C15 1.32(3) . ? C16 C17 1.384(13) . ? C17 C18 1.354(19) . ? C19 C20 1.38(3) . ? C21 C22 1.502(11) . ? C23 C24 1.491(12) . ? C25 C26 1.512(11) . ? C27 C28 1.463(14) . ? C29 C30 1.491(12) . ? C31 C32 1.515(16) . ? C33 C34 1.567(14) . ? C35 C55 1.504(17) . ? C37 C38 1.505(14) . ? C39 C40 1.422(18) . ? C44 C46 1.44(2) . ? C45 C54 1.32(2) . ? C112 C114 1.12(6) . ? C121 C122 1.71(3) . ? C123 C124 1.86(4) . ? C154 C155 1.561(19) . ? C156 C159 1.68(5) . ? 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 N5 Mo1 N3 81.1(3) . . ? N5 Mo1 N1 79.8(2) . . ? N3 Mo1 N1 79.5(2) . . ? N5 Mo1 S3 86.27(17) . . ? N3 Mo1 S3 87.01(17) . . ? N1 Mo1 S3 161.87(15) . . ? N5 Mo1 S2 86.73(19) . . ? N3 Mo1 S2 163.53(19) . . ? N1 Mo1 S2 87.52(17) . . ? S3 Mo1 S2 103.28(8) . . ? N5 Mo1 S1 165.28(17) . . ? N3 Mo1 S1 87.49(19) . . ? N1 Mo1 S1 89.12(17) . . ? S3 Mo1 S1 102.42(8) . . ? S2 Mo1 S1 102.51(7) . . ? N5 Mo1 Fe3 95.71(16) . . ? N3 Mo1 Fe3 139.69(17) . . ? N1 Mo1 Fe3 139.86(17) . . ? S3 Mo1 Fe3 52.70(6) . . ? S2 Mo1 Fe3 52.33(5) . . ? S1 Mo1 Fe3 99.01(6) . . ? N5 Mo1 Fe1 138.84(18) . . ? N3 Mo1 Fe1 139.80(18) . . ? N1 Mo1 Fe1 99.94(15) . . ? S3 Mo1 Fe1 98.18(6) . . ? S2 Mo1 Fe1 52.33(5) . . ? S1 Mo1 Fe1 52.40(5) . . ? Fe3 Mo1 Fe1 58.15(4) . . ? N5 Mo1 Fe2 138.38(16) . . ? N3 Mo1 Fe2 98.10(19) . . ? N1 Mo1 Fe2 141.40(16) . . ? S3 Mo1 Fe2 52.27(6) . . ? S2 Mo1 Fe2 98.37(6) . . ? S1 Mo1 Fe2 52.32(5) . . ? Fe3 Mo1 Fe2 58.50(4) . . ? Fe1 Mo1 Fe2 57.60(4) . . ? N7 Mo2 N11 80.0(3) . . ? N7 Mo2 N9 79.6(3) . . ? N11 Mo2 N9 81.2(3) . . ? N7 Mo2 S6 163.24(18) . . ? N11 Mo2 S6 87.38(18) . . ? N9 Mo2 S6 87.6(2) . . ? N7 Mo2 S5 87.5(2) . . ? N11 Mo2 S5 86.2(2) . . ? N9 Mo2 S5 163.3(3) . . ? S6 Mo2 S5 102.77(8) . . ? N7 Mo2 S4 87.7(2) . . ? N11 Mo2 S4 164.3(2) . . ? N9 Mo2 S4 87.1(2) . . ? S6 Mo2 S4 102.53(8) . . ? S5 Mo2 S4 103.09(8) . . ? N7 Mo2 Fe4 97.89(17) . . ? N11 Mo2 Fe4 138.7(2) . . ? N9 Mo2 Fe4 139.5(2) . . ? S6 Mo2 Fe4 98.87(5) . . ? S5 Mo2 Fe4 52.48(6) . . ? S4 Mo2 Fe4 52.51(6) . . ? N7 Mo2 Fe6 139.6(2) . . ? N11 Mo2 Fe6 97.4(2) . . ? N9 Mo2 Fe6 140.3(2) . . ? S6 Mo2 Fe6 52.70(6) . . ? S5 Mo2 Fe6 52.24(6) . . ? S4 Mo2 Fe6 98.26(6) . . ? Fe4 Mo2 Fe6 57.99(3) . . ? N7 Mo2 Fe5 139.7(2) . . ? N11 Mo2 Fe5 139.77(18) . . ? N9 Mo2 Fe5 97.5(3) . . ? S6 Mo2 Fe5 52.46(6) . . ? S5 Mo2 Fe5 99.22(6) . . ? S4 Mo2 Fe5 51.98(6) . . ? Fe4 Mo2 Fe5 58.74(3) . . ? Fe6 Mo2 Fe5 58.57(4) . . ? S2 Fe1 S1 109.90(8) . . ? S2 Fe1 S10 117.04(9) . . ? S1 Fe1 S10 115.26(9) . . ? S2 Fe1 S9 105.75(8) . . ? S1 Fe1 S9 108.24(8) . . ? S10 Fe1 S9 99.30(8) . . ? S2 Fe1 Fe2 104.55(7) . . ? S1 Fe1 Fe2 54.86(6) . . ? S10 Fe1 Fe2 136.96(8) . . ? S9 Fe1 Fe2 56.95(5) . . ? S2 Fe1 Fe3 54.28(6) . . ? S1 Fe1 Fe3 104.03(6) . . ? S10 Fe1 Fe3 139.14(7) . . ? S9 Fe1 Fe3 56.01(5) . . ? Fe2 Fe1 Fe3 60.65(5) . . ? S2 Fe1 Mo1 56.18(6) . . ? S1 Fe1 Mo1 56.25(5) . . ? S10 Fe1 Mo1 154.59(7) . . ? S9 Fe1 Mo1 106.11(6) . . ? Fe2 Fe1 Mo1 61.51(4) . . ? Fe3 Fe1 Mo1 60.60(4) . . ? S7 Fe2 S3 114.80(9) . . ? S7 Fe2 S1 116.79(9) . . ? S3 Fe2 S1 108.66(8) . . ? S7 Fe2 S9 101.81(8) . . ? S3 Fe2 S9 105.47(8) . . ? S1 Fe2 S9 108.31(7) . . ? S7 Fe2 Fe1 140.94(7) . . ? S3 Fe2 Fe1 103.12(8) . . ? S1 Fe2 Fe1 54.65(6) . . ? S9 Fe2 Fe1 57.23(5) . . ? S7 Fe2 Fe3 139.30(8) . . ? S3 Fe2 Fe3 54.09(7) . . ? S1 Fe2 Fe3 103.17(7) . . ? S9 Fe2 Fe3 55.78(6) . . ? Fe1 Fe2 Fe3 59.81(4) . . ? S7 Fe2 Mo1 152.26(7) . . ? S3 Fe2 Mo1 55.15(6) . . ? S1 Fe2 Mo1 55.94(6) . . ? S9 Fe2 Mo1 105.83(6) . . ? Fe1 Fe2 Mo1 60.89(4) . . ? Fe3 Fe2 Mo1 60.13(4) . . ? S7 Fe2 Fe5 52.55(7) . . ? S3 Fe2 Fe5 102.86(7) . . ? S1 Fe2 Fe5 147.68(7) . . ? S9 Fe2 Fe5 54.95(5) . . ? Fe1 Fe2 Fe5 111.42(5) . . ? Fe3 Fe2 Fe5 89.40(5) . . ? Mo1 Fe2 Fe5 148.80(5) . . ? S2 Fe3 S3 110.22(8) . . ? S2 Fe3 S8 112.01(12) . . ? S3 Fe3 S8 118.45(13) . . ? S2 Fe3 S81 124.5(3) . . ? S3 Fe3 S81 96.9(3) . . ? S8 Fe3 S81 21.6(2) . . ? S2 Fe3 S9 107.39(8) . . ? S3 Fe3 S9 106.60(9) . . ? S8 Fe3 S9 101.07(11) . . ? S81 Fe3 S9 109.7(2) . . ? S2 Fe3 Fe1 54.60(6) . . ? S3 Fe3 Fe1 102.95(7) . . ? S8 Fe3 Fe1 137.96(12) . . ? S81 Fe3 Fe1 158.8(3) . . ? S9 Fe3 Fe1 57.48(5) . . ? S2 Fe3 Fe2 103.89(7) . . ? S3 Fe3 Fe2 54.14(6) . . ? S8 Fe3 Fe2 142.61(11) . . ? S81 Fe3 Fe2 130.8(3) . . ? S9 Fe3 Fe2 56.95(6) . . ? Fe1 Fe3 Fe2 59.55(4) . . ? S2 Fe3 Mo1 56.53(6) . . ? S3 Fe3 Mo1 55.70(6) . . ? S8 Fe3 Mo1 150.96(10) . . ? S81 Fe3 Mo1 138.7(3) . . ? S9 Fe3 Mo1 107.82(6) . . ? Fe1 Fe3 Mo1 61.24(3) . . ? Fe2 Fe3 Mo1 61.37(4) . . ? S2 Fe3 Fe6 147.12(7) . . ? S3 Fe3 Fe6 102.18(7) . . ? S8 Fe3 Fe6 53.45(9) . . ? S81 Fe3 Fe6 54.3(2) . . ? S9 Fe3 Fe6 56.27(5) . . ? Fe1 Fe3 Fe6 113.23(5) . . ? Fe2 Fe3 Fe6 90.38(5) . . ? Mo1 Fe3 Fe6 150.57(6) . . ? S5 Fe4 S4 110.83(9) . . ? S5 Fe4 S11 105.23(9) . . ? S4 Fe4 S11 116.75(9) . . ? S5 Fe4 S9 107.97(8) . . ? S4 Fe4 S9 105.42(8) . . ? S11 Fe4 S9 110.43(7) . . ? S5 Fe4 Fe6 54.39(6) . . ? S4 Fe4 Fe6 104.00(7) . . ? S11 Fe4 Fe6 139.17(8) . . ? S9 Fe4 Fe6 57.62(5) . . ? S5 Fe4 Fe5 103.92(7) . . ? S4 Fe4 Fe5 53.88(6) . . ? S11 Fe4 Fe5 150.67(7) . . ? S9 Fe4 Fe5 56.41(5) . . ? Fe6 Fe4 Fe5 60.31(4) . . ? S5 Fe4 Mo2 56.23(6) . . ? S4 Fe4 Mo2 56.79(6) . . ? S11 Fe4 Mo2 142.22(7) . . ? S9 Fe4 Mo2 106.84(6) . . ? Fe6 Fe4 Mo2 61.02(4) . . ? Fe5 Fe4 Mo2 60.94(4) . . ? S4 Fe5 S7 116.48(10) . . ? S4 Fe5 S6 109.99(9) . . ? S7 Fe5 S6 113.77(9) . . ? S4 Fe5 S9 105.83(8) . . ? S7 Fe5 S9 102.46(8) . . ? S6 Fe5 S9 107.32(9) . . ? S4 Fe5 Fe6 103.32(8) . . ? S7 Fe5 Fe6 139.49(8) . . ? S6 Fe5 Fe6 54.22(7) . . ? S9 Fe5 Fe6 57.17(6) . . ? S4 Fe5 Fe4 54.28(6) . . ? S7 Fe5 Fe4 142.64(7) . . ? S6 Fe5 Fe4 102.55(7) . . ? S9 Fe5 Fe4 56.45(5) . . ? Fe6 Fe5 Fe4 59.12(4) . . ? S4 Fe5 Mo2 56.62(7) . . ? S7 Fe5 Mo2 151.14(7) . . ? S6 Fe5 Mo2 55.56(6) . . ? S9 Fe5 Mo2 106.35(6) . . ? Fe6 Fe5 Mo2 60.42(4) . . ? Fe4 Fe5 Mo2 60.32(4) . . ? S4 Fe5 Fe2 145.58(7) . . ? S7 Fe5 Fe2 52.73(7) . . ? S6 Fe5 Fe2 103.59(7) . . ? S9 Fe5 Fe2 55.49(5) . . ? Fe6 Fe5 Fe2 90.03(5) . . ? Fe4 Fe5 Fe2 111.45(5) . . ? Mo2 Fe5 Fe2 149.85(6) . . ? S5 Fe6 S6 109.64(8) . . ? S5 Fe6 S8 109.97(12) . . ? S6 Fe6 S8 121.78(13) . . ? S5 Fe6 S81 123.7(3) . . ? S6 Fe6 S81 100.2(3) . . ? S8 Fe6 S81 21.6(2) . . ? S5 Fe6 S9 107.43(8) . . ? S6 Fe6 S9 106.45(8) . . ? S8 Fe6 S9 100.31(11) . . ? S81 Fe6 S9 108.2(2) . . ? S5 Fe6 Fe4 54.70(7) . . ? S6 Fe6 Fe4 103.73(7) . . ? S8 Fe6 Fe4 133.94(12) . . ? S81 Fe6 Fe4 154.6(3) . . ? S9 Fe6 Fe4 56.73(5) . . ? S5 Fe6 Fe5 104.38(8) . . ? S6 Fe6 Fe5 54.20(6) . . ? S8 Fe6 Fe5 143.31(10) . . ? S81 Fe6 Fe5 131.6(3) . . ? S9 Fe6 Fe5 56.25(5) . . ? Fe4 Fe6 Fe5 60.57(4) . . ? S5 Fe6 Mo2 56.29(6) . . ? S6 Fe6 Mo2 55.81(6) . . ? S8 Fe6 Mo2 152.90(10) . . ? S81 Fe6 Mo2 142.7(3) . . ? S9 Fe6 Mo2 106.11(6) . . ? Fe4 Fe6 Mo2 60.99(4) . . ? Fe5 Fe6 Mo2 61.01(4) . . ? S5 Fe6 Fe3 144.75(7) . . ? S6 Fe6 Fe3 104.93(7) . . ? S8 Fe6 Fe3 54.04(9) . . ? S81 Fe6 Fe3 54.3(2) . . ? S9 Fe6 Fe3 54.79(5) . . ? Fe4 Fe6 Fe3 110.48(5) . . ? Fe5 Fe6 Fe3 90.14(5) . . ? Mo2 Fe6 Fe3 150.81(6) . . ? Fe1 S1 Fe2 70.49(6) . . ? Fe1 S1 Mo1 71.35(7) . . ? Fe2 S1 Mo1 71.74(6) . . ? Fe3 S2 Fe1 71.12(7) . . ? Fe3 S2 Mo1 71.13(7) . . ? Fe1 S2 Mo1 71.49(7) . . ? Fe3 S3 Fe2 71.77(7) . . ? Fe3 S3 Mo1 71.60(7) . . ? Fe2 S3 Mo1 72.58(6) . . ? Fe5 S4 Fe4 71.85(7) . . ? Fe5 S4 Mo2 71.40(7) . . ? Fe4 S4 Mo2 70.70(7) . . ? Fe6 S5 Fe4 70.91(7) . . ? Fe6 S5 Mo2 71.46(7) . . ? Fe4 S5 Mo2 71.29(7) . . ? Fe5 S6 Fe6 71.58(7) . . ? Fe5 S6 Mo2 71.98(6) . . ? Fe6 S6 Mo2 71.48(6) . . ? Fe5 S7 Fe2 74.71(8) . . ? S81 S8 C154 36.5(16) . . ? S81 S8 Fe6 81.8(8) . . ? C154 S8 Fe6 112.7(13) . . ? S81 S8 Fe3 80.6(7) . . ? C154 S8 Fe3 107.9(13) . . ? Fe6 S8 Fe3 72.52(11) . . ? S8 S81 C154 118(3) . . ? S8 S81 Fe3 77.8(8) . . ? C154 S81 Fe3 137.9(17) . . ? S8 S81 Fe6 76.6(8) . . ? C154 S81 Fe6 147.1(17) . . ? Fe3 S81 Fe6 71.4(3) . . ? Fe3 S9 Fe5 105.30(8) . . ? Fe3 S9 Fe4 132.92(9) . . ? Fe5 S9 Fe4 67.15(6) . . ? Fe3 S9 Fe2 67.27(6) . . ? Fe5 S9 Fe2 69.56(6) . . ? Fe4 S9 Fe2 135.89(9) . . ? Fe3 S9 Fe1 66.51(6) . . ? Fe5 S9 Fe1 134.13(9) . . ? Fe4 S9 Fe1 151.81(9) . . ? Fe2 S9 Fe1 65.81(6) . . ? Fe3 S9 Fe6 68.94(6) . . ? Fe5 S9 Fe6 66.58(6) . . ? Fe4 S9 Fe6 65.65(6) . . ? Fe2 S9 Fe6 104.08(7) . . ? Fe1 S9 Fe6 134.64(9) . . ? C19 S10 Fe1 101.6(5) . . ? C21 S11 Fe4 104.0(3) . . ? C1 N1 N2 106.0(6) . . ? C1 N1 Mo1 131.8(5) . . ? N2 N1 Mo1 122.2(4) . . ? C3 N2 N1 111.0(6) . . ? C3 N2 B1 128.6(7) . . ? N1 N2 B1 120.3(6) . . ? C4 N3 N4 106.9(7) . . ? C4 N3 Mo1 131.4(6) . . ? N4 N3 Mo1 121.4(6) . . ? C6 N4 N3 108.0(8) . . ? C6 N4 B1 129.9(8) . . ? N3 N4 B1 122.1(7) . . ? C7 N5 N6 106.5(6) . . ? C7 N5 Mo1 130.9(5) . . ? N6 N5 Mo1 122.6(5) . . ? C9 N6 N5 108.9(7) . . ? C9 N6 B1 130.6(7) . . ? N5 N6 B1 120.4(7) . . ? C10 N7 N8 106.5(7) . . ? C10 N7 Mo2 131.2(6) . . ? N8 N7 Mo2 122.2(5) . . ? C12 N8 N7 108.5(8) . . ? C12 N8 B2 130.9(9) . . ? N7 N8 B2 120.5(8) . . ? C13 N9 N10 112.1(9) . . ? C13 N9 Mo2 128.2(8) . . ? N10 N9 Mo2 119.6(9) . . ? N9 N10 C15 98.0(13) . . ? N9 N10 B2 122.8(10) . . ? C15 N10 B2 138.6(12) . . ? C16 N11 N12 107.4(8) . . ? C16 N11 Mo2 130.8(6) . . ? N12 N11 Mo2 121.7(7) . . ? C18 N12 N11 106.9(11) . . ? C18 N12 B2 132.1(11) . . ? N11 N12 B2 120.6(9) . . ? C25 N13 C23 105.8(6) . . ? C25 N13 C29 110.9(6) . . ? C23 N13 C29 111.3(7) . . ? C25 N13 C27 111.7(6) . . ? C23 N13 C27 111.4(6) . . ? C29 N13 C27 105.9(7) . . ? C33 N14 C35 113.2(9) . . ? C33 N14 C31 113.3(8) . . ? C35 N14 C31 106.0(9) . . ? C33 N14 C37 104.6(7) . . ? C35 N14 C37 109.8(7) . . ? C31 N14 C37 109.9(8) . . ? C123 N15 C44 128(2) . . ? C123 N15 C122 102(2) . . ? C44 N15 C122 117.3(16) . . ? C123 N15 C45 92(2) . . ? C44 N15 C45 103.4(12) . . ? C122 N15 C45 110.1(14) . . ? N4 B1 N6 108.7(7) . . ? N4 B1 N2 107.7(8) . . ? N6 B1 N2 107.2(8) . . ? N10 B2 N8 108.9(13) . . ? N10 B2 N12 107.6(10) . . ? N8 B2 N12 108.4(12) . . ? N1 C1 C2 111.0(7) . . ? C1 C2 C3 105.2(7) . . ? N2 C3 C2 106.9(7) . . ? N3 C4 C5 111.1(9) . . ? C6 C5 C4 104.7(9) . . ? N4 C6 C5 109.2(8) . . ? N5 C7 C8 111.5(7) . . ? C9 C8 C7 103.0(8) . . ? N6 C9 C8 110.0(7) . . ? N7 C10 C11 109.2(8) . . ? C12 C11 C10 104.6(10) . . ? N8 C12 C11 111.0(10) . . ? N9 C13 C14 110.4(16) . . ? C15 C14 C13 101(2) . . ? C14 C15 N10 118.0(18) . . ? N11 C16 C17 110.0(11) . . ? C18 C17 C16 104.5(13) . . ? N12 C18 C17 111.2(10) . . ? C20 C19 S10 113.5(15) . . ? C22 C21 S11 111.0(6) . . ? C24 C23 N13 116.1(8) . . ? N13 C25 C26 115.4(7) . . ? C28 C27 N13 117.2(8) . . ? C30 C29 N13 116.7(8) . . ? N14 C31 C32 112.7(9) . . ? N14 C33 C34 112.7(8) . . ? N14 C35 C55 113.5(9) . . ? C38 C37 N14 114.4(8) . . ? N16 C39 C40 173(2) . . ? C46 C44 N15 117.7(16) . . ? C54 C45 N15 109.9(17) . . ? C112 C114 N111 136(7) . . ? N15 C122 C121 104.4(17) . . ? N15 C123 C124 97(3) . . ? S81 C154 C155 136(4) . . ? S81 C154 S8 25.5(12) . . ? C155 C154 S8 114(4) . . ? N31 C156 C159 125(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.888 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.113 #--------------------------------END data_(Et4N)4[Tp2Mo2Fe6S8(C4H5N2)4]3MeCN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ' not measured ' _chemical_formula_moiety (Et4N)4[Tp2Mo2Fe6S8(C4H5N2)4]3MeCN _chemical_formula_sum 'C72 H119 B2 Fe6 Mo2 N27 S8' _chemical_formula_weight 2168.44 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' 'B' 'B' 0.0013 0.0007 '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' 'Fe' 'Fe' 0.3463 0.8444 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.960(3) _cell_length_b 14.424(4) _cell_length_c 15.357(4) _cell_angle_alpha 102.785(5) _cell_angle_beta 99.337(5) _cell_angle_gamma 97.038(5) _cell_volume 2514.5(11) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark green ' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.288 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 14006 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8794 _reflns_number_gt 6856 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0781P)^2^+2.8015P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8794 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.423 _refine_ls_shift/su_mean 0.009 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 N18 N 1.007(3) 0.606(2) 0.379(2) 0.068(8) Uiso 0.17 1 d P . . Mo1 Mo 0.44181(3) 0.21376(3) 0.19401(2) 0.03488(13) Uani 1 1 d . . . Fe1 Fe 0.60504(6) 0.21925(5) 0.08960(5) 0.03984(18) Uani 1 1 d . . . Fe2 Fe 0.46997(6) 0.05474(4) 0.07421(4) 0.03732(17) Uani 1 1 d . . . Fe3 Fe 0.39169(6) 0.18940(4) 0.00755(4) 0.03930(18) Uani 1 1 d . . . S1 S 0.60446(10) 0.13435(8) 0.19815(8) 0.0414(3) Uani 1 1 d . . . S2 S 0.48448(10) 0.32952(8) 0.10950(8) 0.0408(3) Uani 1 1 d . . . S3 S 0.29548(10) 0.10035(8) 0.08568(8) 0.0415(3) Uani 1 1 d . . . S4 S 0.53489(13) 0.10557(8) -0.05300(8) 0.0486(3) Uani 1 1 d . . . N1 N 0.3057(4) 0.2988(3) 0.2378(3) 0.0460(9) Uani 1 1 d . . . N2 N 0.2984(4) 0.3276(3) 0.3270(3) 0.0552(11) Uani 1 1 d . . . N3 N 0.5457(4) 0.3152(3) 0.3231(3) 0.0482(10) Uani 1 1 d . . . N4 N 0.5014(4) 0.3394(3) 0.4000(3) 0.0567(11) Uani 1 1 d . . . N5 N 0.3901(4) 0.1388(3) 0.2976(3) 0.0461(10) Uani 1 1 d . . . N6 N 0.3649(4) 0.1876(3) 0.3771(3) 0.0537(11) Uani 1 1 d . . . N7 N 0.3109(5) 0.1928(4) -0.1172(3) 0.0732(15) Uani 1 1 d . . . N8 N 0.2543(7) 0.1369(7) -0.3707(5) 0.129(3) Uani 1 1 d . . . N9 N 0.7556(4) 0.2707(4) 0.0625(4) 0.0683(14) Uani 1 1 d . . . N11 N 0.5987(4) 0.3450(3) 0.7869(3) 0.0535(11) Uani 1 1 d . . . N12 N 0.9730(4) 0.0780(3) 0.2348(4) 0.0652(13) Uani 1 1 d . . . N13 N 0.8258(10) 0.1811(9) 0.5513(9) 0.175(5) Uani 1 1 d . . . N16 N 1.021(4) 0.518(4) 0.434(3) 0.119(15) Uiso 0.17 1 d P . . N17 N 1.024(4) 0.457(3) 0.499(3) 0.098(12) Uiso 0.17 1 d P . . B1 B 0.3771(7) 0.2980(5) 0.4004(4) 0.0609(17) Uani 1 1 d . . . H1 H 0.358(5) 0.322(4) 0.460(4) 0.073 Uiso 1 1 calc . . . C1 C 0.2299(4) 0.3386(4) 0.1922(4) 0.0531(13) Uani 1 1 d . . . H1A H 0.2156 0.3301 0.1294 0.064 Uiso 1 1 calc R . . C2 C 0.1740(5) 0.3957(4) 0.2522(5) 0.0627(16) Uani 1 1 d . . . H2 H 0.1181 0.4322 0.2376 0.075 Uiso 1 1 calc R . . C3 C 0.2188(5) 0.3861(4) 0.3353(4) 0.0586(14) Uani 1 1 d . . . H3 H 0.1983 0.4149 0.3895 0.070 Uiso 1 1 calc R . . C4 C 0.6554(5) 0.3565(4) 0.3441(4) 0.0583(14) Uani 1 1 d . . . H4 H 0.7062 0.3515 0.3041 0.070 Uiso 1 1 calc R . . C5 C 0.6833(6) 0.4086(5) 0.4352(4) 0.0755(18) Uani 1 1 d . . . H5 H 0.7539 0.4445 0.4669 0.091 Uiso 1 1 calc R . . C6 C 0.5837(6) 0.3952(5) 0.4671(4) 0.0726(18) Uani 1 1 d . . . H6 H 0.5746 0.4208 0.5262 0.087 Uiso 1 1 calc R . . C7 C 0.3734(5) 0.0456(4) 0.2970(4) 0.0528(13) Uani 1 1 d . . . H7 H 0.3852 -0.0036 0.2506 0.063 Uiso 1 1 calc R . . C8 C 0.3358(6) 0.0319(5) 0.3752(4) 0.0675(16) Uani 1 1 d . . . H8 H 0.3179 -0.0260 0.3911 0.081 Uiso 1 1 calc R . . C9 C 0.3313(6) 0.1232(5) 0.4236(4) 0.0665(16) Uani 1 1 d . . . H9 H 0.3087 0.1384 0.4795 0.080 Uiso 1 1 calc R . . C10 C 0.2318(5) 0.2371(5) -0.1471(4) 0.0690(17) Uani 1 1 d . . . C11 C 0.1840(8) 0.3002(6) -0.0702(5) 0.100(2) Uani 1 1 d . . . H11A H 0.1318 0.2597 -0.0476 0.149 Uiso 1 1 calc R . . H11B H 0.1442 0.3459 -0.0941 0.149 Uiso 1 1 calc R . . H11C H 0.2463 0.3340 -0.0216 0.149 Uiso 1 1 calc R . . C12 C 0.1803(7) 0.2409(6) -0.2311(5) 0.096(3) Uani 1 1 d . . . H12A H 0.1915 0.3074 -0.2354 0.116 Uiso 1 1 calc R . . H12B H 0.0984 0.2195 -0.2390 0.116 Uiso 1 1 calc R . . C13 C 0.2259(8) 0.1786(8) -0.3097(6) 0.118(4) Uani 1 1 d . . . C14 C 0.8274(5) 0.3521(7) 0.0907(6) 0.094(3) Uani 1 1 d . . . C15 C 0.8016(8) 0.4281(6) 0.1646(7) 0.115(3) Uani 1 1 d . . . C16 C 0.9346(8) 0.3583(10) 0.0462(8) 0.148(5) Uani 1 1 d . . . C18 C 0.5534(6) 0.4226(5) 0.7466(4) 0.0764(19) Uani 1 1 d . . . H18A H 0.5930 0.4846 0.7847 0.092 Uiso 1 1 calc R . . H18B H 0.5739 0.4165 0.6872 0.092 Uiso 1 1 calc R . . C19 C 0.4276(7) 0.4235(5) 0.7355(6) 0.105(3) Uani 1 1 d . . . H19A H 0.3868 0.3650 0.6936 0.157 Uiso 1 1 calc R . . H19B H 0.4096 0.4776 0.7123 0.157 Uiso 1 1 calc R . . H19C H 0.4052 0.4285 0.7934 0.157 Uiso 1 1 calc R . . C20 C 0.5801(6) 0.3561(4) 0.8841(4) 0.0725(17) Uani 1 1 d . . . H20A H 0.4981 0.3480 0.8830 0.087 Uiso 1 1 calc R . . H20B H 0.6091 0.3044 0.9071 0.087 Uiso 1 1 calc R . . C21 C 0.6353(8) 0.4499(5) 0.9495(4) 0.088(2) Uani 1 1 d . . . H21A H 0.7157 0.4614 0.9480 0.132 Uiso 1 1 calc R . . H21B H 0.6260 0.4474 1.0099 0.132 Uiso 1 1 calc R . . H21C H 0.5997 0.5011 0.9326 0.132 Uiso 1 1 calc R . . C22 C 0.5313(7) 0.2446(5) 0.7380(5) 0.090(2) Uani 1 1 d . . . H22A H 0.5617 0.1982 0.7685 0.108 Uiso 1 1 calc R . . H22B H 0.4519 0.2436 0.7446 0.108 Uiso 1 1 calc R . . C23 C 0.5336(9) 0.2126(7) 0.6400(6) 0.124(3) Uani 1 1 d . . . H23A H 0.4892 0.2493 0.6068 0.186 Uiso 1 1 calc R . . H23B H 0.5016 0.1455 0.6182 0.186 Uiso 1 1 calc R . . H23C H 0.6115 0.2224 0.6314 0.186 Uiso 1 1 calc R . . C24 C 0.7213(6) 0.3499(6) 0.7823(6) 0.089(2) Uani 1 1 d . . . H24A H 0.7628 0.4108 0.8216 0.107 Uiso 1 1 calc R . . H24B H 0.7296 0.3500 0.7205 0.107 Uiso 1 1 calc R . . C25 C 0.7785(8) 0.2678(8) 0.8099(7) 0.129(4) Uani 1 1 d . . . H25A H 0.7595 0.2593 0.8663 0.193 Uiso 1 1 calc R . . H25B H 0.8603 0.2839 0.8173 0.193 Uiso 1 1 calc R . . H25C H 0.7513 0.2092 0.7634 0.193 Uiso 1 1 calc R . . C26 C 0.9110(7) 0.0311(6) 0.2937(6) 0.090(2) Uani 1 1 d . . . H26A H 0.8433 0.0603 0.3019 0.108 Uiso 1 1 calc R . . H26B H 0.8854 -0.0365 0.2635 0.108 Uiso 1 1 calc R . . C27 C 0.9811(9) 0.0391(8) 0.3826(7) 0.133(4) Uani 1 1 d . . . H27A H 1.0446 0.0052 0.3753 0.199 Uiso 1 1 calc R . . H27B H 0.9355 0.0115 0.4193 0.199 Uiso 1 1 calc R . . H27C H 1.0096 0.1058 0.4117 0.199 Uiso 1 1 calc R . . C28 C 1.0795(5) 0.0360(5) 0.2181(5) 0.0739(18) Uani 1 1 d . . . H28A H 1.1142 0.0674 0.1770 0.089 Uiso 1 1 calc R . . H28B H 1.1341 0.0510 0.2754 0.089 Uiso 1 1 calc R . . C29 C 1.0599(7) -0.0706(5) 0.1789(7) 0.108(3) Uani 1 1 d . . . H29A H 1.0206 -0.1025 0.2167 0.162 Uiso 1 1 calc R . . H29B H 1.1325 -0.0920 0.1764 0.162 Uiso 1 1 calc R . . H29C H 1.0141 -0.0858 0.1186 0.162 Uiso 1 1 calc R . . C30 C 0.8853(5) 0.0604(5) 0.1434(5) 0.0743(18) Uani 1 1 d . . . H30A H 0.8612 -0.0085 0.1191 0.089 Uiso 1 1 calc R . . H30B H 0.8180 0.0880 0.1559 0.089 Uiso 1 1 calc R . . C31 C 0.9309(7) 0.1022(6) 0.0713(5) 0.088(2) Uani 1 1 d . . . H31A H 0.9552 0.1704 0.0944 0.131 Uiso 1 1 calc R . . H31B H 0.8713 0.0900 0.0181 0.131 Uiso 1 1 calc R . . H31C H 0.9949 0.0726 0.0556 0.131 Uiso 1 1 calc R . . C32 C 1.0108(5) 0.1858(4) 0.2731(4) 0.0602(14) Uani 1 1 d . . . H32A H 1.0695 0.1961 0.3275 0.072 Uiso 1 1 calc R . . H32B H 1.0461 0.2115 0.2289 0.072 Uiso 1 1 calc R . . C33 C 0.9182(5) 0.2424(4) 0.2967(5) 0.0727(17) Uani 1 1 d . . . H33A H 0.8604 0.2346 0.2432 0.109 Uiso 1 1 calc R . . H33B H 0.9507 0.3093 0.3200 0.109 Uiso 1 1 calc R . . H33C H 0.8842 0.2194 0.3421 0.109 Uiso 1 1 calc R . . C34 C 0.7472(9) 0.1500(8) 0.4956(7) 0.104(3) Uani 1 1 d . . . C35 C 0.6542(8) 0.1037(9) 0.4284(5) 0.124(4) Uani 1 1 d . . . H35A H 0.6485 0.1362 0.3800 0.186 Uiso 1 1 calc R . . H35B H 0.5854 0.1043 0.4531 0.186 Uiso 1 1 calc R . . H35C H 0.6637 0.0383 0.4050 0.186 Uiso 1 1 calc R . . C36 C 0.9778(16) 0.5755(14) 0.4331(13) 0.101(5) Uiso 0.50 1 d P . . C37 C 0.9204(13) 0.6543(11) 0.4295(10) 0.081(4) Uiso 0.50 1 d P . . C17 C 0.904(2) 0.490(2) 0.1726(17) 0.145(8) Uiso 0.50 1 d P . . C171 C 0.972(2) 0.442(2) 0.0807(18) 0.146(8) Uiso 0.50 1 d P . . N101 N 0.977(2) 0.564(2) 0.201(2) 0.205(10) Uiso 0.50 1 d P . . N10 N 1.036(2) 0.527(2) 0.1097(19) 0.199(10) Uiso 0.50 1 d P . . 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 0.0431(2) 0.0294(2) 0.0330(2) 0.00585(15) 0.00958(16) 0.00976(16) Fe1 0.0450(4) 0.0337(3) 0.0473(4) 0.0167(3) 0.0152(3) 0.0105(3) Fe2 0.0545(4) 0.0268(3) 0.0355(3) 0.0090(3) 0.0191(3) 0.0092(3) Fe3 0.0500(4) 0.0311(3) 0.0363(4) 0.0102(3) 0.0066(3) 0.0037(3) S1 0.0474(7) 0.0393(6) 0.0437(6) 0.0164(5) 0.0127(5) 0.0148(5) S2 0.0504(7) 0.0271(5) 0.0447(6) 0.0088(5) 0.0078(5) 0.0084(5) S3 0.0469(7) 0.0362(6) 0.0405(6) 0.0080(5) 0.0116(5) 0.0020(5) S4 0.0815(9) 0.0293(6) 0.0445(7) 0.0136(5) 0.0311(6) 0.0124(6) N1 0.056(3) 0.041(2) 0.043(2) 0.0078(18) 0.0148(19) 0.0132(19) N2 0.071(3) 0.046(2) 0.050(3) 0.0010(19) 0.023(2) 0.019(2) N3 0.055(3) 0.042(2) 0.041(2) 0.0033(18) 0.0001(19) 0.010(2) N4 0.076(3) 0.050(3) 0.036(2) -0.0038(19) 0.006(2) 0.013(2) N5 0.058(3) 0.047(2) 0.038(2) 0.0099(18) 0.0184(18) 0.014(2) N6 0.066(3) 0.060(3) 0.038(2) 0.009(2) 0.020(2) 0.015(2) N7 0.072(3) 0.074(3) 0.065(3) 0.032(3) -0.012(3) -0.013(3) N8 0.124(6) 0.190(9) 0.067(5) 0.033(5) 0.031(4) -0.017(6) N9 0.042(3) 0.086(4) 0.093(4) 0.057(3) 0.015(2) 0.006(3) N11 0.062(3) 0.048(2) 0.051(3) 0.015(2) 0.009(2) 0.009(2) N12 0.052(3) 0.057(3) 0.094(4) 0.023(3) 0.030(3) 0.008(2) N13 0.145(10) 0.182(11) 0.180(11) 0.039(9) 0.024(8) -0.023(8) B1 0.078(5) 0.062(4) 0.043(3) 0.001(3) 0.020(3) 0.021(4) C1 0.049(3) 0.050(3) 0.067(3) 0.023(3) 0.017(3) 0.011(2) C2 0.052(3) 0.051(3) 0.097(5) 0.022(3) 0.036(3) 0.022(3) C3 0.064(4) 0.044(3) 0.071(4) 0.002(3) 0.030(3) 0.018(3) C4 0.062(4) 0.043(3) 0.058(3) 0.003(2) -0.005(3) 0.008(3) C5 0.081(5) 0.060(4) 0.065(4) -0.001(3) -0.013(3) 0.003(3) C6 0.094(5) 0.066(4) 0.043(3) -0.006(3) -0.002(3) 0.013(4) C7 0.065(3) 0.053(3) 0.049(3) 0.020(2) 0.019(3) 0.013(3) C8 0.087(4) 0.071(4) 0.061(4) 0.036(3) 0.028(3) 0.022(3) C9 0.081(4) 0.084(4) 0.044(3) 0.027(3) 0.025(3) 0.014(3) C10 0.069(4) 0.067(4) 0.064(4) 0.034(3) -0.013(3) -0.014(3) C11 0.120(7) 0.086(5) 0.084(5) 0.013(4) 0.001(5) 0.020(5) C12 0.086(5) 0.118(6) 0.078(5) 0.059(5) -0.019(4) -0.024(5) C13 0.111(7) 0.168(9) 0.056(5) 0.051(6) -0.008(4) -0.057(6) C14 0.044(4) 0.153(8) 0.100(6) 0.090(6) -0.009(3) -0.012(4) C15 0.127(8) 0.085(6) 0.106(7) 0.044(5) -0.036(6) -0.041(5) C16 0.087(6) 0.199(12) 0.139(9) 0.084(9) -0.024(6) -0.064(7) C18 0.107(6) 0.064(4) 0.058(4) 0.022(3) 0.009(3) 0.012(4) C19 0.094(6) 0.064(4) 0.128(7) 0.000(4) -0.035(5) 0.026(4) C20 0.099(5) 0.063(4) 0.069(4) 0.033(3) 0.030(4) 0.017(3) C21 0.150(7) 0.057(4) 0.060(4) 0.017(3) 0.009(4) 0.032(4) C22 0.100(6) 0.054(4) 0.098(6) -0.004(4) 0.001(4) 0.010(4) C23 0.149(9) 0.103(7) 0.096(7) -0.005(5) -0.002(6) 0.024(6) C24 0.072(5) 0.090(5) 0.109(6) 0.027(4) 0.025(4) 0.012(4) C25 0.103(7) 0.143(9) 0.133(8) 0.019(7) -0.006(6) 0.053(6) C26 0.084(5) 0.091(5) 0.118(7) 0.051(5) 0.050(5) 0.014(4) C27 0.133(8) 0.170(10) 0.126(8) 0.069(8) 0.067(7) 0.023(7) C28 0.060(4) 0.077(4) 0.104(5) 0.039(4) 0.036(4) 0.027(3) C29 0.105(6) 0.075(5) 0.173(9) 0.043(5) 0.073(6) 0.041(5) C30 0.048(3) 0.062(4) 0.099(5) -0.003(3) 0.007(3) 0.005(3) C31 0.084(5) 0.093(5) 0.079(5) 0.013(4) 0.006(4) 0.018(4) C32 0.049(3) 0.058(3) 0.064(4) 0.010(3) 0.003(3) -0.007(3) C33 0.065(4) 0.056(4) 0.085(5) 0.002(3) 0.005(3) 0.007(3) C34 0.103(7) 0.127(8) 0.103(7) 0.060(6) 0.038(6) 0.013(6) C35 0.106(7) 0.215(12) 0.065(5) 0.057(6) 0.015(5) 0.036(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 N5 2.236(4) . ? Mo1 N1 2.255(4) . ? Mo1 N3 2.256(4) . ? Mo1 S1 2.3746(13) . ? Mo1 S3 2.3782(13) . ? Mo1 S2 2.3869(12) . ? Mo1 Fe2 2.6984(9) . ? Mo1 Fe1 2.7244(9) . ? Mo1 Fe3 2.7620(10) . ? Fe1 N9 2.004(4) . ? Fe1 S1 2.2768(13) . ? Fe1 S2 2.2786(13) . ? Fe1 S4 2.3803(15) . ? Fe1 Fe3 2.5946(11) . ? Fe1 Fe2 2.6429(10) . ? Fe2 S4 2.2548(14) 2_655 ? Fe2 S1 2.2616(15) . ? Fe2 S3 2.2854(15) . ? Fe2 S4 2.4380(13) . ? Fe2 Fe3 2.5907(10) . ? Fe2 Fe2 2.7243(13) 2_655 ? Fe3 N7 2.015(5) . ? Fe3 S3 2.2762(13) . ? Fe3 S2 2.2921(14) . ? Fe3 S4 2.4055(15) . ? S4 Fe2 2.2548(14) 2_655 ? N1 C1 1.319(6) . ? N1 N2 1.361(6) . ? N2 C3 1.349(7) . ? N2 B1 1.519(9) . ? N3 C4 1.329(7) . ? N3 N4 1.365(6) . ? N4 C6 1.336(7) . ? N4 B1 1.534(9) . ? N5 C7 1.332(6) . ? N5 N6 1.366(5) . ? N6 C9 1.352(7) . ? N6 B1 1.537(8) . ? N7 C10 1.284(8) . ? N8 C13 1.123(12) . ? N9 C14 1.309(10) . ? N11 C24 1.473(8) . ? N11 C18 1.508(7) . ? N11 C20 1.522(7) . ? N11 C22 1.532(8) . ? N12 C26 1.481(8) . ? N12 C28 1.510(7) . ? N12 C32 1.518(7) . ? N12 C30 1.560(8) . ? N13 C34 1.133(13) . ? N16 C36 1.03(5) . ? N18 C36 1.10(3) . ? N18 C37 1.53(3) . ? N18 N16 1.68(6) . ? N16 N17 1.24(6) 2_766 ? N16 N17 1.47(6) . ? N17 C36 1.23(4) 2_766 ? N17 N16 1.24(6) 2_766 ? N17 N17 1.42(8) 2_766 ? C1 C2 1.404(7) . ? C2 C3 1.346(9) . ? C4 C5 1.398(8) . ? C5 C6 1.369(10) . ? C7 C8 1.394(7) . ? C8 C9 1.374(9) . ? C10 C12 1.353(8) . ? C10 C11 1.556(10) . ? C12 C13 1.554(14) . ? C14 C15 1.494(13) . ? C14 C16 1.550(13) . ? C15 C17 1.40(3) . ? C16 C171 1.20(3) . ? C18 C19 1.489(10) . ? C20 C21 1.497(9) . ? C22 C23 1.479(11) . ? C24 C25 1.541(11) . ? C26 C27 1.454(12) . ? C28 C29 1.496(10) . ? C30 C31 1.516(10) . ? C32 C33 1.499(8) . ? C34 C35 1.374(13) . ? C36 N17 1.23(4) 2_766 ? C36 C37 1.41(2) . ? C17 N101 1.24(3) . ? C171 N10 1.30(3) . ? 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 C36 N18 C37 62.2(19) . . ? C36 N18 N16 37(2) . . ? C37 N18 N16 99(3) . . ? N5 Mo1 N1 80.35(15) . . ? N5 Mo1 N3 79.52(16) . . ? N1 Mo1 N3 80.49(15) . . ? N5 Mo1 S1 87.53(11) . . ? N1 Mo1 S1 161.97(11) . . ? N3 Mo1 S1 84.24(11) . . ? N5 Mo1 S3 86.65(12) . . ? N1 Mo1 S3 88.85(11) . . ? N3 Mo1 S3 163.74(12) . . ? S1 Mo1 S3 103.81(5) . . ? N5 Mo1 S2 164.84(11) . . ? N1 Mo1 S2 86.74(11) . . ? N3 Mo1 S2 90.60(11) . . ? S1 Mo1 S2 103.02(4) . . ? S3 Mo1 S2 101.08(5) . . ? N5 Mo1 Fe2 96.57(10) . . ? N1 Mo1 Fe2 141.89(11) . . ? N3 Mo1 Fe2 136.72(11) . . ? S1 Mo1 Fe2 52.48(4) . . ? S3 Mo1 Fe2 53.06(4) . . ? S2 Mo1 Fe2 98.50(4) . . ? N5 Mo1 Fe1 139.86(11) . . ? N1 Mo1 Fe1 139.18(10) . . ? N3 Mo1 Fe1 97.66(12) . . ? S1 Mo1 Fe1 52.50(3) . . ? S3 Mo1 Fe1 98.43(4) . . ? S2 Mo1 Fe1 52.44(3) . . ? Fe2 Mo1 Fe1 58.33(2) . . ? N5 Mo1 Fe3 138.22(11) . . ? N1 Mo1 Fe3 101.31(10) . . ? N3 Mo1 Fe3 142.22(11) . . ? S1 Mo1 Fe3 96.63(3) . . ? S3 Mo1 Fe3 51.92(3) . . ? S2 Mo1 Fe3 52.25(3) . . ? Fe2 Mo1 Fe3 56.63(2) . . ? Fe1 Mo1 Fe3 56.44(3) . . ? N9 Fe1 S1 119.08(14) . . ? N9 Fe1 S2 113.95(16) . . ? S1 Fe1 S2 109.80(5) . . ? N9 Fe1 S4 97.04(18) . . ? S1 Fe1 S4 106.38(5) . . ? S2 Fe1 S4 109.19(5) . . ? N9 Fe1 Fe3 135.33(14) . . ? S1 Fe1 Fe3 104.04(4) . . ? S2 Fe1 Fe3 55.66(4) . . ? S4 Fe1 Fe3 57.64(4) . . ? N9 Fe1 Fe2 141.05(17) . . ? S1 Fe1 Fe2 54.12(4) . . ? S2 Fe1 Fe2 102.98(4) . . ? S4 Fe1 Fe2 57.79(3) . . ? Fe3 Fe1 Fe2 59.28(3) . . ? N9 Fe1 Mo1 154.22(18) . . ? S1 Fe1 Mo1 55.83(3) . . ? S2 Fe1 Mo1 56.14(3) . . ? S4 Fe1 Mo1 108.67(4) . . ? Fe3 Fe1 Mo1 62.51(3) . . ? Fe2 Fe1 Mo1 60.34(2) . . ? S4 Fe2 S1 110.01(5) 2_655 . ? S4 Fe2 S3 113.02(5) 2_655 . ? S1 Fe2 S3 110.69(5) . . ? S4 Fe2 S4 109.15(4) 2_655 . ? S1 Fe2 S4 104.96(5) . . ? S3 Fe2 S4 108.69(5) . . ? S4 Fe2 Fe3 145.22(5) 2_655 . ? S1 Fe2 Fe3 104.60(4) . . ? S3 Fe2 Fe3 55.23(4) . . ? S4 Fe2 Fe3 57.06(4) . . ? S4 Fe2 Fe1 143.72(5) 2_655 . ? S1 Fe2 Fe1 54.65(4) . . ? S3 Fe2 Fe1 103.26(4) . . ? S4 Fe2 Fe1 55.70(4) . . ? Fe3 Fe2 Fe1 59.43(3) . . ? S4 Fe2 Mo1 142.96(4) 2_655 . ? S1 Fe2 Mo1 56.38(3) . . ? S3 Fe2 Mo1 56.27(3) . . ? S4 Fe2 Mo1 107.77(4) . . ? Fe3 Fe2 Mo1 62.92(3) . . ? Fe1 Fe2 Mo1 61.33(3) . . ? S4 Fe2 Fe2 57.71(4) 2_655 2_655 ? S1 Fe2 Fe2 120.95(5) . 2_655 ? S3 Fe2 Fe2 127.61(5) . 2_655 ? S4 Fe2 Fe2 51.43(4) . 2_655 ? Fe3 Fe2 Fe2 101.14(4) . 2_655 ? Fe1 Fe2 Fe2 99.37(4) . 2_655 ? Mo1 Fe2 Fe2 159.01(4) . 2_655 ? N7 Fe3 S3 117.56(15) . . ? N7 Fe3 S2 120.01(15) . . ? S3 Fe3 S2 107.28(5) . . ? N7 Fe3 S4 92.41(18) . . ? S3 Fe3 S4 110.13(5) . . ? S2 Fe3 S4 107.86(5) . . ? N7 Fe3 Fe2 133.31(17) . . ? S3 Fe3 Fe2 55.56(4) . . ? S2 Fe3 Fe2 104.22(4) . . ? S4 Fe3 Fe2 58.27(3) . . ? N7 Fe3 Fe1 134.51(16) . . ? S3 Fe3 Fe1 105.04(4) . . ? S2 Fe3 Fe1 55.17(4) . . ? S4 Fe3 Fe1 56.70(4) . . ? Fe2 Fe3 Fe1 61.29(3) . . ? N7 Fe3 Mo1 160.84(18) . . ? S3 Fe3 Mo1 55.32(4) . . ? S2 Fe3 Mo1 55.43(3) . . ? S4 Fe3 Mo1 106.73(4) . . ? Fe2 Fe3 Mo1 60.45(2) . . ? Fe1 Fe3 Mo1 61.05(2) . . ? Fe2 S1 Fe1 71.23(4) . . ? Fe2 S1 Mo1 71.14(4) . . ? Fe1 S1 Mo1 71.67(4) . . ? Fe1 S2 Fe3 69.17(4) . . ? Fe1 S2 Mo1 71.41(4) . . ? Fe3 S2 Mo1 72.32(4) . . ? Fe3 S3 Fe2 69.21(4) . . ? Fe3 S3 Mo1 72.76(4) . . ? Fe2 S3 Mo1 70.67(4) . . ? Fe2 S4 Fe1 123.99(6) 2_655 . ? Fe2 S4 Fe3 123.51(6) 2_655 . ? Fe1 S4 Fe3 65.66(4) . . ? Fe2 S4 Fe2 70.85(4) 2_655 . ? Fe1 S4 Fe2 66.52(4) . . ? Fe3 S4 Fe2 64.67(4) . . ? C1 N1 N2 106.4(4) . . ? C1 N1 Mo1 131.7(3) . . ? N2 N1 Mo1 121.6(3) . . ? C3 N2 N1 109.5(5) . . ? C3 N2 B1 129.4(5) . . ? N1 N2 B1 121.0(4) . . ? C4 N3 N4 106.9(4) . . ? C4 N3 Mo1 130.9(4) . . ? N4 N3 Mo1 122.0(3) . . ? C6 N4 N3 109.1(5) . . ? C6 N4 B1 130.6(5) . . ? N3 N4 B1 120.2(4) . . ? C7 N5 N6 106.8(4) . . ? C7 N5 Mo1 131.0(3) . . ? N6 N5 Mo1 122.2(3) . . ? C9 N6 N5 108.7(4) . . ? C9 N6 B1 130.9(5) . . ? N5 N6 B1 120.4(4) . . ? C10 N7 Fe3 134.6(5) . . ? C14 N9 Fe1 135.4(6) . . ? C24 N11 C18 108.4(5) . . ? C24 N11 C20 111.6(5) . . ? C18 N11 C20 111.0(5) . . ? C24 N11 C22 110.9(5) . . ? C18 N11 C22 112.0(5) . . ? C20 N11 C22 103.0(5) . . ? C26 N12 C28 112.4(5) . . ? C26 N12 C32 113.5(5) . . ? C28 N12 C32 106.8(4) . . ? C26 N12 C30 105.1(5) . . ? C28 N12 C30 110.3(5) . . ? C32 N12 C30 108.8(5) . . ? C36 N16 N17 65(4) . 2_766 ? C36 N16 N17 127(5) . . ? N17 N16 N17 63(4) 2_766 . ? C36 N16 N18 39(2) . . ? N17 N16 N18 103(4) 2_766 . ? N17 N16 N18 166(5) . . ? C36 N17 N16 49(3) 2_766 2_766 ? C36 N17 N17 116(5) 2_766 2_766 ? N16 N17 N17 67(4) 2_766 2_766 ? C36 N17 N16 166(4) 2_766 . ? N16 N17 N16 117(4) 2_766 . ? N17 N17 N16 51(3) 2_766 . ? N2 B1 N4 108.2(5) . . ? N2 B1 N6 109.0(5) . . ? N4 B1 N6 108.1(5) . . ? N1 C1 C2 110.3(5) . . ? C3 C2 C1 105.0(5) . . ? C2 C3 N2 108.8(5) . . ? N3 C4 C5 110.1(6) . . ? C6 C5 C4 104.6(6) . . ? N4 C6 C5 109.3(6) . . ? N5 C7 C8 110.8(5) . . ? C9 C8 C7 104.3(5) . . ? N6 C9 C8 109.3(5) . . ? N7 C10 C12 134.1(8) . . ? N7 C10 C11 113.5(6) . . ? C12 C10 C11 112.5(7) . . ? C10 C12 C13 113.9(8) . . ? N8 C13 C12 174.8(11) . . ? N9 C14 C15 117.7(6) . . ? N9 C14 C16 116.0(10) . . ? C15 C14 C16 126.3(9) . . ? C17 C15 C14 93.7(13) . . ? C171 C16 C14 97.3(19) . . ? C19 C18 N11 117.1(6) . . ? C21 C20 N11 115.6(5) . . ? C23 C22 N11 115.7(7) . . ? N11 C24 C25 115.5(7) . . ? C27 C26 N12 112.8(7) . . ? C29 C28 N12 115.1(6) . . ? C31 C30 N12 114.6(5) . . ? C33 C32 N12 116.0(5) . . ? N13 C34 C35 174.5(13) . . ? N16 C36 N18 104(4) . . ? N16 C36 N17 66(3) . 2_766 ? N18 C36 N17 163(3) . 2_766 ? N16 C36 C37 178(4) . . ? N18 C36 C37 74(2) . . ? N17 C36 C37 116(3) 2_766 . ? C36 C37 N18 43.8(13) . . ? N101 C17 C15 158(3) . . ? C16 C171 N10 165(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.876 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.101 #--------------------------------END data_(Et4N)3[Tp2Mo2Fe6S8(OMe)3](2DMF)(C6H14) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ' not measured ' _chemical_formula_moiety (Et4N)3[Tp2Mo2Fe6S8(OMe)3](2DMF)(C6H14) _chemical_formula_sum 'C57 H131 B2 Fe6 Mo2 N17 O5 S8' _chemical_formula_weight 1939.64 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 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 28.932(8) _cell_length_b 20.688(6) _cell_length_c 31.443(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.398(6) _cell_angle_gamma 90.00 _cell_volume 16857(8) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'Dark black ' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7728 _exptl_absorpt_coefficient_mu 1.538 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ? _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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 36516 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 22.50 _reflns_number_total 11016 _reflns_number_gt 6729 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0959P)^2^+221.9146P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11016 _refine_ls_number_parameters 842 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1294 _refine_ls_R_factor_gt 0.0799 _refine_ls_wR_factor_ref 0.2323 _refine_ls_wR_factor_gt 0.2126 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 3.600 _refine_ls_shift/su_mean 0.127 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 0.90291(5) 0.18516(6) 0.99454(4) 0.0488(4) Uani 1 1 d . . . Mo2 Mo 0.80604(5) 0.23139(6) 0.72841(4) 0.0501(4) Uani 1 1 d . . . Fe1 Fe 0.84061(8) 0.24127(9) 0.91162(7) 0.0499(5) Uani 1 1 d . . . Fe2 Fe 0.91597(7) 0.16889(9) 0.91283(7) 0.0463(5) Uani 1 1 d . . . Fe3 Fe 0.93559(8) 0.28269(10) 0.95664(7) 0.0539(6) Uani 1 1 d . . . Fe4 Fe 0.80305(8) 0.25502(9) 0.81165(7) 0.0504(5) Uani 1 1 d . . . Fe5 Fe 0.88055(7) 0.18686(9) 0.81441(7) 0.0470(5) Uani 1 1 d . . . Fe6 Fe 0.87337(8) 0.31367(9) 0.79394(7) 0.0525(6) Uani 1 1 d . . . S1 S 0.84646(13) 0.13371(17) 0.92302(13) 0.0503(9) Uani 1 1 d . . . S2 S 0.87362(15) 0.29479(18) 0.98208(13) 0.0582(10) Uani 1 1 d . . . S3 S 0.98104(13) 0.19019(19) 0.98698(13) 0.0562(10) Uani 1 1 d . . . S4 S 0.79609(14) 0.15528(17) 0.78020(13) 0.0530(9) Uani 1 1 d . . . S5 S 0.78641(15) 0.33126(17) 0.75512(13) 0.0569(10) Uani 1 1 d . . . S6 S 0.89710(13) 0.23556(18) 0.75730(13) 0.0526(9) Uani 1 1 d . . . S7 S 0.89097(13) 0.27254(16) 0.87101(13) 0.0500(9) Uani 1 1 d . . . S8 S 0.93674(14) 0.11327(17) 0.86228(14) 0.0572(10) Uani 1 1 d . . . O1 O 0.7735(4) 0.2692(5) 0.8579(4) 0.063(3) Uani 1 1 d . . . O2 O 0.9150(4) 0.3891(5) 0.8104(4) 0.071(3) Uani 1 1 d . . . O3 O 0.9753(4) 0.3566(5) 0.9604(4) 0.079(3) Uani 1 1 d . . . O8 O 0.2842(15) 0.956(2) 0.4921(14) 0.133(14) Uiso 0.50 1 d P . . O14 O -0.0060(8) 0.4124(10) 0.8943(7) 0.177(7) Uiso 1 1 d . . . O16 O 0.186(5) 0.781(7) 0.478(5) 0.69(9) Uiso 0.50 1 d P . . O17 O 0.1074(12) 0.7149(17) 0.7586(11) 0.314(13) Uiso 1 1 d . . . N1 N 0.8435(4) 0.1672(6) 1.0207(4) 0.056(3) Uani 1 1 d . . . N2 N 0.8560(5) 0.1357(7) 1.0631(5) 0.072(4) Uani 1 1 d . . . N3 N 0.9271(4) 0.0847(6) 1.0249(4) 0.055(3) Uani 1 1 d . . . N4 N 0.9286(4) 0.0665(6) 1.0666(4) 0.063(3) Uani 1 1 d . . . N5 N 0.9487(5) 0.2089(6) 1.0719(4) 0.057(3) Uani 1 1 d . . . N6 N 0.9453(5) 0.1715(7) 1.1059(5) 0.070(4) Uani 1 1 d . . . N7 N 0.7214(5) 0.2177(5) 0.6805(4) 0.054(3) Uani 1 1 d . . . N8 N 0.7028(5) 0.2082(6) 0.6328(5) 0.067(4) Uani 1 1 d . . . N9 N 0.8086(5) 0.1501(6) 0.6833(4) 0.060(3) Uani 1 1 d . . . N10 N 0.7793(5) 0.1503(7) 0.6359(5) 0.072(4) Uani 1 1 d . . . N11 N 0.7984(5) 0.2896(6) 0.6648(4) 0.057(3) Uani 1 1 d . . . N12 N 0.7701(5) 0.2658(7) 0.6193(5) 0.071(4) Uani 1 1 d . . . N13 N 0.8454(6) 0.4903(6) 0.8856(5) 0.078(4) Uani 1 1 d . . . N14 N 0.6491(4) 0.4347(6) 0.6451(4) 0.063(3) Uani 1 1 d . . . N15 N 0.0711(7) 0.2490(14) 0.8876(7) 0.144(9) Uani 1 1 d . . . N16 N 0.2258(15) 0.952(2) 0.5015(13) 0.122(12) Uiso 0.50 1 d P . . N17 N 0.2559(12) 1.0107(14) 0.5344(10) 0.086(9) Uiso 0.50 1 d P . . B1 B 0.9116(8) 0.1144(11) 1.0945(7) 0.071(6) Uani 1 1 d . . . H1A H 0.914(6) 0.094(7) 1.124(5) 0.085 Uiso 1 1 calc . . . B2 B 0.7402(8) 0.2047(12) 0.6104(8) 0.077(6) Uani 1 1 d . . . H2A H 0.722(6) 0.196(8) 0.576(6) 0.092 Uiso 1 1 calc . . . C1 C 0.7950(7) 0.1829(7) 1.0037(6) 0.068(4) Uani 1 1 d . . . H1 H 0.7765 0.2045 0.9751 0.082 Uiso 1 1 calc R . . C2 C 0.7741(7) 0.1628(9) 1.0344(7) 0.085(5) Uani 1 1 d . . . H2 H 0.7406 0.1680 1.0305 0.103 Uiso 1 1 calc R . . C3 C 0.8143(7) 0.1340(9) 1.0708(7) 0.086(6) Uani 1 1 d . . . H3 H 0.8130 0.1158 1.0973 0.104 Uiso 1 1 calc R . . C4 C 0.9455(5) 0.0368(7) 1.0098(6) 0.061(4) Uani 1 1 d . . . H4 H 0.9494 0.0378 0.9820 0.073 Uiso 1 1 calc R . . C5 C 0.9583(6) -0.0148(9) 1.0399(7) 0.085(6) Uani 1 1 d . . . H5 H 0.9710 -0.0548 1.0367 0.102 Uiso 1 1 calc R . . C6 C 0.9482(6) 0.0057(9) 1.0751(8) 0.092(6) Uani 1 1 d . . . H6 H 0.9540 -0.0185 1.1020 0.110 Uiso 1 1 calc R . . C16 C 0.9819(6) 0.2591(9) 1.0939(6) 0.081(5) Uani 1 1 d . . . H16 H 0.9910 0.2919 1.0789 0.097 Uiso 1 1 calc R . . C17 C 0.9998(8) 0.2519(13) 1.1436(6) 0.108(7) Uani 1 1 d . . . H17 H 1.0222 0.2789 1.1675 0.129 Uiso 1 1 calc R . . C18 C 0.9765(8) 0.1955(13) 1.1485(7) 0.105(7) Uani 1 1 d . . . H18 H 0.9818 0.1772 1.1774 0.126 Uiso 1 1 calc R . . C19 C 0.6800(6) 0.2200(8) 0.6884(5) 0.061(4) Uani 1 1 d . . . H19 H 0.6813 0.2268 0.7182 0.073 Uiso 1 1 calc R . . C20 C 0.6358(6) 0.2112(7) 0.6483(6) 0.069(5) Uani 1 1 d . . . H20 H 0.6023 0.2102 0.6451 0.083 Uiso 1 1 calc R . . C21 C 0.6517(6) 0.2041(7) 0.6125(6) 0.066(4) Uani 1 1 d . . . H21 H 0.6303 0.1976 0.5804 0.079 Uiso 1 1 calc R . . C22 C 0.8393(5) 0.0981(7) 0.6941(6) 0.059(4) Uani 1 1 d . . . H22 H 0.8639 0.0873 0.7245 0.070 Uiso 1 1 calc R . . C23 C 0.8289(7) 0.0621(8) 0.6528(7) 0.080(5) Uani 1 1 d . . . H23 H 0.8441 0.0237 0.6501 0.096 Uiso 1 1 calc R . . C24 C 0.7906(7) 0.0975(9) 0.6170(7) 0.082(5) Uani 1 1 d . . . H24 H 0.7751 0.0866 0.5849 0.098 Uiso 1 1 calc R . . C25 C 0.8162(6) 0.3463(9) 0.6617(6) 0.069(4) Uani 1 1 d . . . H25 H 0.8378 0.3713 0.6875 0.083 Uiso 1 1 calc R . . C26 C 0.7984(7) 0.3642(11) 0.6144(7) 0.086(6) Uani 1 1 d . . . H26 H 0.8052 0.4023 0.6025 0.103 Uiso 1 1 calc R . . C27 C 0.7683(8) 0.3127(13) 0.5889(7) 0.100(7) Uani 1 1 d . . . H27 H 0.7498 0.3108 0.5561 0.120 Uiso 1 1 calc R . . C28 C 0.7334(9) 0.2453(11) 0.8511(7) 0.118(10) Uani 1 1 d . . . H28A H 0.7338 0.2002 0.8441 0.178 Uiso 1 1 calc R . . H28B H 0.7059 0.2664 0.8248 0.178 Uiso 1 1 calc R . . H28C H 0.7281 0.2500 0.8790 0.178 Uiso 1 1 calc R . . H40A H 0.7458 0.4719 0.6508 0.178 Uiso 1 1 d R . . H40B H 0.7426 0.5450 0.6623 0.178 Uiso 1 1 d R . . H40C H 0.7439 0.4916 0.6982 0.178 Uiso 1 1 d R . . C29 C 0.9159(8) 0.4302(9) 0.7769(7) 0.109(7) Uani 1 1 d . . . H29A H 0.9305 0.4084 0.7587 0.163 Uiso 1 1 calc R . . H29B H 0.9365 0.4673 0.7922 0.163 Uiso 1 1 calc R . . H29C H 0.8814 0.4437 0.7562 0.163 Uiso 1 1 calc R . . C30 C 1.0080(8) 0.3789(9) 1.0027(7) 0.107(7) Uani 1 1 d . . . H30A H 0.9891 0.3955 1.0188 0.161 Uiso 1 1 calc R . . H30B H 1.0285 0.4128 0.9988 0.161 Uiso 1 1 calc R . . H30C H 1.0302 0.3445 1.0210 0.161 Uiso 1 1 calc R . . C31 C 0.8967(7) 0.4800(8) 0.8850(7) 0.084(5) Uani 1 1 d . . . H31A H 0.9192 0.4572 0.9138 0.101 Uiso 1 1 calc R . . H31B H 0.8913 0.4520 0.8584 0.101 Uiso 1 1 calc R . . C32 C 0.9240(7) 0.5390(10) 0.8813(7) 0.108(7) Uani 1 1 d . . . H32A H 0.9263 0.5695 0.9051 0.162 Uiso 1 1 calc R . . H32B H 0.9054 0.5578 0.8504 0.162 Uiso 1 1 calc R . . H32C H 0.9582 0.5276 0.8860 0.162 Uiso 1 1 calc R . . C33 C 0.8202(7) 0.4274(8) 0.8813(7) 0.091(6) Uani 1 1 d . . . H33A H 0.8159 0.4079 0.8517 0.110 Uiso 1 1 calc R . . H33B H 0.8438 0.4000 0.9068 0.110 Uiso 1 1 calc R . . C34 C 0.7712(7) 0.4252(9) 0.8824(9) 0.126(9) Uani 1 1 d . . . H34A H 0.7462 0.4490 0.8559 0.189 Uiso 1 1 calc R . . H34B H 0.7743 0.4442 0.9114 0.189 Uiso 1 1 calc R . . H34C H 0.7602 0.3811 0.8806 0.189 Uiso 1 1 calc R . . C35 C 0.8542(8) 0.5233(8) 0.9329(6) 0.092(6) Uani 1 1 d . . . H35A H 0.8711 0.5645 0.9352 0.110 Uiso 1 1 calc R . . H35B H 0.8210 0.5318 0.9323 0.110 Uiso 1 1 calc R . . C36 C 0.8861(9) 0.4842(9) 0.9761(7) 0.110(7) Uani 1 1 d . . . H36A H 0.9182 0.4729 0.9759 0.165 Uiso 1 1 calc R . . H36B H 0.8677 0.4456 0.9762 0.165 Uiso 1 1 calc R . . H36C H 0.8929 0.5092 1.0040 0.165 Uiso 1 1 calc R . . C37 C 0.8096(8) 0.5332(9) 0.8461(7) 0.099(6) Uani 1 1 d . . . H37A H 0.7775 0.5371 0.8487 0.119 Uiso 1 1 calc R . . H37B H 0.8248 0.5760 0.8508 0.119 Uiso 1 1 calc R . . C38 C 0.7972(9) 0.5113(9) 0.7965(7) 0.126(8) Uani 1 1 d . . . H38A H 0.7759 0.4734 0.7890 0.189 Uiso 1 1 calc R . . H38B H 0.8286 0.5016 0.7945 0.189 Uiso 1 1 calc R . . H38C H 0.7791 0.5451 0.7744 0.189 Uiso 1 1 calc R . . C39 C 0.6744(7) 0.4963(8) 0.6406(7) 0.089(6) Uani 1 1 d . . . H39A H 0.6632 0.5042 0.6070 0.107 Uiso 1 1 calc R . . H39B H 0.6610 0.5314 0.6524 0.107 Uiso 1 1 calc R . . C40 C 0.7313(8) 0.5002(9) 0.6647(8) 0.107(7) Uani 1 1 d . . . C41 C 0.6632(6) 0.4224(8) 0.6966(6) 0.077(5) Uani 1 1 d . . . H41A H 0.7001 0.4141 0.7131 0.092 Uiso 1 1 calc R . . H41B H 0.6458 0.3834 0.6988 0.092 Uiso 1 1 calc R . . C42 C 0.6504(7) 0.4762(10) 0.7223(6) 0.102(6) Uani 1 1 d . . . H42A H 0.6139 0.4839 0.7071 0.153 Uiso 1 1 calc R . . H42B H 0.6683 0.5149 0.7214 0.153 Uiso 1 1 calc R . . H42C H 0.6610 0.4638 0.7548 0.153 Uiso 1 1 calc R . . C43 C 0.5914(6) 0.4435(8) 0.6170(6) 0.079(5) Uani 1 1 d . . . H43A H 0.5834 0.4520 0.5841 0.094 Uiso 1 1 calc R . . H43B H 0.5808 0.4809 0.6291 0.094 Uiso 1 1 calc R . . C44 C 0.5601(6) 0.3831(10) 0.6194(8) 0.119(8) Uani 1 1 d . . . H44A H 0.5704 0.3720 0.6520 0.178 Uiso 1 1 calc R . . H44B H 0.5669 0.3474 0.6035 0.178 Uiso 1 1 calc R . . H44C H 0.5239 0.3930 0.6042 0.178 Uiso 1 1 calc R . . C45 C 0.6679(6) 0.3773(7) 0.6273(6) 0.070(5) Uani 1 1 d . . . H45A H 0.7053 0.3773 0.6430 0.084 Uiso 1 1 calc R . . H45B H 0.6565 0.3381 0.6368 0.084 Uiso 1 1 calc R . . C46 C 0.6504(8) 0.3748(10) 0.5747(7) 0.112(7) Uani 1 1 d . . . H46A H 0.6627 0.4123 0.5649 0.169 Uiso 1 1 calc R . . H46B H 0.6133 0.3739 0.5586 0.169 Uiso 1 1 calc R . . H46C H 0.6638 0.3366 0.5669 0.169 Uiso 1 1 calc R . . C47 C 0.0240(9) 0.2827(13) 0.8556(9) 0.119(8) Uani 1 1 d . . . H47A H 0.0148 0.3136 0.8738 0.143 Uiso 1 1 calc R . . H47B H -0.0039 0.2515 0.8420 0.143 Uiso 1 1 calc R . . C48 C 0.0291(10) 0.3179(15) 0.8158(10) 0.175(12) Uani 1 1 d . . . H48A H 0.0631 0.3361 0.8274 0.262 Uiso 1 1 calc R . . H48B H 0.0039 0.3518 0.8041 0.262 Uiso 1 1 calc R . . H48C H 0.0236 0.2881 0.7906 0.262 Uiso 1 1 calc R . . C49 C 0.0889(11) 0.2045(18) 0.8606(12) 0.178(13) Uani 1 1 d . . . H49A H 0.1167 0.1779 0.8829 0.214 Uiso 1 1 calc R . . H49B H 0.1023 0.2298 0.8426 0.214 Uiso 1 1 calc R . . C50 C 0.0426(12) 0.1575(14) 0.8242(12) 0.178(13) Uani 1 1 d . . . H50A H 0.0140 0.1835 0.8032 0.267 Uiso 1 1 calc R . . H50B H 0.0315 0.1293 0.8421 0.267 Uiso 1 1 calc R . . H50C H 0.0551 0.1322 0.8059 0.267 Uiso 1 1 calc R . . C51 C 0.1176(8) 0.295(2) 0.9219(17) 0.35(4) Uani 1 1 d . . . H51A H 0.1493 0.2700 0.9368 0.418 Uiso 1 1 calc R . . H51B H 0.1227 0.3296 0.9038 0.418 Uiso 1 1 calc R . . C52 C 0.104(2) 0.321(4) 0.958(2) 0.49(8) Uani 1 1 d . . . H52A H 0.1132 0.2902 0.9834 0.740 Uiso 1 1 calc R . . H52B H 0.0677 0.3292 0.9442 0.740 Uiso 1 1 calc R . . H52C H 0.1227 0.3604 0.9702 0.740 Uiso 1 1 calc R . . C53 C 0.0536(11) 0.217(2) 0.9190(11) 0.27(3) Uani 1 1 d . . . H53A H 0.0419 0.2498 0.9341 0.323 Uiso 1 1 calc R . . H53B H 0.0242 0.1901 0.9000 0.323 Uiso 1 1 calc R . . C54 C 0.0934(16) 0.177(4) 0.9564(17) 0.47(6) Uani 1 1 d . . . H54A H 0.1131 0.2027 0.9838 0.709 Uiso 1 1 calc R . . H54B H 0.1160 0.1584 0.9446 0.709 Uiso 1 1 calc R . . H54C H 0.0769 0.1423 0.9651 0.709 Uiso 1 1 calc R . . C63 C 0.133(2) 0.612(3) 0.763(2) 0.17(2) Uiso 0.50 1 d P . . C67 C 0.2038(13) 1.0037(16) 0.5141(11) 0.169(11) Uiso 1 1 d . . . C70 C 0.2909(15) 0.989(2) 0.5235(15) 0.094(12) Uiso 0.50 1 d P . . C88 C 0.279(2) 1.060(3) 0.585(2) 0.17(2) Uiso 0.50 1 d P . . C90 C 0.277(2) 0.928(3) 0.502(2) 0.14(2) Uiso 0.50 1 d P . . C94 C 0.1065(15) 0.836(2) 0.7691(13) 0.228(15) Uiso 1 1 d . . . C99 C 0.1410(15) 0.682(2) 0.9056(14) 0.099(12) Uiso 0.50 1 d P . . C108 C 0.097(2) 0.648(3) 0.7689(19) 0.149(19) Uiso 0.50 1 d P . . C109 C 0.124(3) 0.598(4) 0.895(2) 0.19(3) Uiso 0.50 1 d P . . C110 C 0.085(3) 0.590(4) 0.895(3) 0.22(3) Uiso 0.50 1 d P . . C111 C 0.196(3) 0.883(4) 0.483(3) 0.22(3) Uiso 0.50 1 d P . . C112 C 0.073(3) 0.515(5) 0.888(3) 0.25(4) Uiso 0.50 1 d P . . C113 C 0.077(4) 0.513(5) 0.845(4) 0.32(5) Uiso 0.50 1 d P . . C114 C 0.040(4) 0.450(5) 0.902(3) 0.26(4) Uiso 0.50 1 d P . . C116 C 0.051(4) 0.908(5) 0.755(3) 0.27(4) Uiso 0.50 1 d P . . C117 C 0.011(2) 0.918(2) 0.754(3) 0.21(2) Uiso 0.50 1 d P . . C118 C 0.0897(16) 0.773(2) 0.7777(14) 0.226(16) 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 0.0416(7) 0.0479(8) 0.0533(8) 0.0086(6) 0.0178(6) 0.0064(6) Mo2 0.0446(7) 0.0455(7) 0.0535(8) 0.0004(6) 0.0158(6) 0.0066(6) Fe1 0.0491(12) 0.0422(12) 0.0534(12) 0.0055(9) 0.0182(11) 0.0069(10) Fe2 0.0414(11) 0.0380(11) 0.0532(12) 0.0070(9) 0.0154(10) 0.0051(9) Fe3 0.0526(13) 0.0484(12) 0.0535(13) 0.0014(10) 0.0169(11) -0.0086(10) Fe4 0.0488(12) 0.0438(12) 0.0530(13) 0.0025(9) 0.0177(11) 0.0087(10) Fe5 0.0443(11) 0.0365(11) 0.0547(12) 0.0025(9) 0.0171(10) 0.0057(9) Fe6 0.0543(13) 0.0386(11) 0.0601(13) 0.0015(10) 0.0215(11) 0.0033(10) S1 0.042(2) 0.045(2) 0.057(2) 0.0010(17) 0.0158(18) 0.0010(17) S2 0.063(2) 0.048(2) 0.059(2) 0.0037(18) 0.024(2) 0.0020(19) S3 0.038(2) 0.069(3) 0.057(2) 0.0135(19) 0.0169(18) 0.0050(19) S4 0.049(2) 0.047(2) 0.058(2) -0.0027(17) 0.0191(19) 0.0008(18) S5 0.058(2) 0.041(2) 0.062(2) 0.0084(18) 0.018(2) 0.0178(18) S6 0.044(2) 0.054(2) 0.055(2) 0.0010(18) 0.0178(18) 0.0024(18) S7 0.048(2) 0.040(2) 0.055(2) 0.0072(17) 0.0162(18) 0.0062(17) S8 0.056(2) 0.043(2) 0.070(3) 0.0072(18) 0.025(2) 0.0093(18) O1 0.063(7) 0.066(7) 0.057(7) 0.010(5) 0.022(6) 0.016(6) O2 0.091(8) 0.046(6) 0.076(7) 0.002(5) 0.037(6) -0.016(6) O3 0.081(8) 0.070(7) 0.065(7) -0.007(6) 0.014(6) -0.037(6) N1 0.048(8) 0.056(8) 0.071(9) 0.018(6) 0.031(7) 0.020(6) N2 0.059(9) 0.090(10) 0.087(10) 0.037(8) 0.049(8) 0.031(7) N3 0.041(7) 0.063(8) 0.058(8) 0.025(7) 0.019(6) 0.016(6) N4 0.051(8) 0.068(9) 0.067(9) 0.028(7) 0.023(7) 0.009(7) N5 0.058(8) 0.062(8) 0.052(8) 0.013(7) 0.025(7) 0.008(7) N6 0.068(9) 0.096(11) 0.040(8) 0.008(8) 0.018(7) 0.007(8) N7 0.062(8) 0.039(7) 0.057(9) 0.008(6) 0.022(7) 0.011(6) N8 0.047(8) 0.074(9) 0.066(9) -0.004(7) 0.013(7) 0.008(7) N9 0.060(8) 0.066(8) 0.053(8) 0.000(6) 0.024(7) 0.012(7) N10 0.052(8) 0.093(11) 0.073(10) -0.022(8) 0.028(8) -0.013(8) N11 0.055(8) 0.049(8) 0.065(9) -0.002(6) 0.024(7) 0.008(6) N12 0.061(9) 0.095(11) 0.067(10) 0.003(9) 0.036(8) 0.003(8) N13 0.089(10) 0.053(9) 0.089(11) 0.012(8) 0.037(9) 0.010(8) N14 0.047(8) 0.057(8) 0.063(9) 0.006(6) 0.006(7) -0.002(6) N15 0.067(12) 0.27(3) 0.098(14) 0.068(16) 0.037(12) -0.005(15) B1 0.077(14) 0.079(14) 0.069(13) 0.023(11) 0.043(12) 0.005(12) B2 0.051(12) 0.106(18) 0.061(13) 0.001(12) 0.015(11) 0.002(12) C1 0.082(13) 0.050(10) 0.085(12) 0.007(9) 0.048(11) 0.011(9) C2 0.072(12) 0.077(13) 0.116(16) 0.006(11) 0.050(13) 0.007(10) C3 0.091(14) 0.087(13) 0.107(15) 0.037(11) 0.068(13) 0.030(11) C4 0.055(10) 0.048(9) 0.085(12) 0.014(9) 0.037(9) 0.011(8) C5 0.069(12) 0.067(12) 0.142(18) 0.020(12) 0.069(13) 0.032(9) C6 0.067(12) 0.075(13) 0.129(17) 0.056(12) 0.039(12) 0.041(10) C16 0.058(11) 0.101(14) 0.079(13) -0.009(11) 0.026(10) -0.017(10) C17 0.090(15) 0.18(2) 0.046(12) -0.009(12) 0.026(11) -0.009(15) C18 0.085(15) 0.17(2) 0.078(16) 0.035(15) 0.051(14) 0.018(15) C19 0.046(9) 0.080(11) 0.050(10) 0.012(8) 0.016(9) 0.009(8) C20 0.044(10) 0.054(10) 0.096(13) 0.012(9) 0.019(11) 0.008(8) C21 0.053(11) 0.047(9) 0.075(11) -0.004(8) 0.007(10) 0.002(8) C22 0.049(9) 0.050(9) 0.074(11) -0.015(8) 0.025(8) 0.000(8) C23 0.069(12) 0.062(11) 0.115(16) -0.022(11) 0.047(12) -0.011(10) C24 0.073(12) 0.089(14) 0.087(13) -0.041(12) 0.039(12) -0.026(11) C25 0.060(11) 0.078(13) 0.081(13) 0.003(10) 0.043(10) 0.004(9) C26 0.061(12) 0.110(16) 0.092(15) 0.026(13) 0.039(11) 0.014(11) C27 0.074(13) 0.16(2) 0.071(13) 0.032(15) 0.033(12) 0.003(14) C28 0.14(2) 0.15(2) 0.076(14) 0.014(14) 0.049(16) 0.09(2) C29 0.112(17) 0.088(14) 0.116(17) 0.009(13) 0.041(14) -0.023(13) C30 0.118(17) 0.065(12) 0.117(17) 0.002(12) 0.032(15) -0.019(12) C31 0.091(14) 0.066(12) 0.115(15) 0.017(10) 0.064(12) 0.004(10) C32 0.089(14) 0.109(16) 0.133(18) -0.028(13) 0.056(14) -0.030(12) C33 0.108(16) 0.046(10) 0.129(17) 0.004(10) 0.061(14) -0.005(10) C34 0.088(14) 0.062(12) 0.26(3) -0.008(15) 0.106(18) -0.015(11) C35 0.140(18) 0.051(10) 0.085(13) -0.003(10) 0.050(13) -0.010(11) C36 0.17(2) 0.078(13) 0.090(15) -0.014(11) 0.059(15) -0.001(14) C37 0.118(17) 0.060(12) 0.098(15) -0.007(11) 0.029(13) -0.012(11) C38 0.15(2) 0.073(13) 0.105(17) 0.007(12) 0.015(16) -0.022(14) C39 0.087(14) 0.057(11) 0.133(17) 0.004(11) 0.059(13) -0.007(10) C40 0.089(15) 0.079(14) 0.15(2) 0.001(13) 0.056(14) -0.018(12) C41 0.054(10) 0.075(11) 0.085(13) 0.009(10) 0.016(10) -0.003(9) C42 0.097(15) 0.112(16) 0.090(14) -0.028(12) 0.035(12) 0.016(12) C43 0.056(10) 0.075(12) 0.082(12) -0.004(9) 0.009(10) 0.025(9) C44 0.052(11) 0.107(16) 0.17(2) -0.040(15) 0.021(13) -0.017(11) C45 0.071(11) 0.037(9) 0.095(13) -0.010(8) 0.029(10) 0.011(8) C46 0.127(18) 0.103(16) 0.114(18) 0.011(13) 0.059(15) 0.039(14) C47 0.106(19) 0.14(2) 0.116(19) -0.008(16) 0.056(17) 0.025(16) C48 0.11(2) 0.22(3) 0.17(3) 0.04(2) 0.05(2) 0.07(2) C49 0.11(2) 0.23(4) 0.21(4) 0.01(3) 0.09(3) 0.01(2) C50 0.20(3) 0.16(3) 0.25(4) -0.01(3) 0.16(3) 0.03(2) C51 0.021(12) 0.46(7) 0.45(7) 0.39(6) 0.01(2) -0.01(2) C52 0.21(6) 0.69(16) 0.58(11) -0.53(12) 0.17(7) -0.10(7) C53 0.11(2) 0.54(7) 0.14(3) 0.11(4) 0.03(2) -0.13(3) C54 0.16(4) 0.90(16) 0.26(5) 0.31(8) 0.00(4) -0.17(6) _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 N5 2.246(12) . ? Mo1 N1 2.242(11) . ? Mo1 N3 2.264(11) . ? Mo1 S1 2.365(4) . ? Mo1 S3 2.378(4) . ? Mo1 S2 2.392(4) . ? Mo1 Fe1 2.686(2) . ? Mo1 Fe3 2.718(2) . ? Mo1 Fe2 2.778(2) . ? Mo2 N9 2.222(12) . ? Mo2 N7 2.252(12) . ? Mo2 N11 2.260(13) . ? Mo2 S4 2.373(4) . ? Mo2 S6 2.376(4) . ? Mo2 S5 2.392(4) . ? Mo2 Fe4 2.702(2) . ? Mo2 Fe6 2.714(2) . ? Mo2 Fe5 2.761(2) . ? Fe1 O1 2.010(11) . ? Fe1 S1 2.248(4) . ? Fe1 S2 2.273(4) . ? Fe1 S7 2.414(4) . ? Fe1 Fe3 2.613(3) . ? Fe1 Fe2 2.631(3) . ? Fe1 Fe4 2.847(3) . ? Fe2 S8 2.250(4) . ? Fe2 S1 2.291(4) . ? Fe2 S3 2.296(4) . ? Fe2 S7 2.451(4) . ? Fe2 Fe3 2.658(3) . ? Fe2 Fe5 2.819(3) . ? Fe3 O3 1.884(10) . ? Fe3 S3 2.277(4) . ? Fe3 S2 2.279(5) . ? Fe3 S7 2.423(4) . ? Fe4 O1 2.009(11) . ? Fe4 S4 2.258(4) . ? Fe4 S5 2.262(4) . ? Fe4 S7 2.422(4) . ? Fe4 Fe5 2.617(3) . ? Fe4 Fe6 2.632(3) . ? Fe5 S8 2.247(4) . ? Fe5 S4 2.284(4) . ? Fe5 S6 2.288(4) . ? Fe5 S7 2.434(4) . ? Fe5 Fe6 2.687(3) . ? Fe6 O2 1.899(10) . ? Fe6 S6 2.261(4) . ? Fe6 S5 2.285(4) . ? Fe6 S7 2.399(4) . ? O1 C28 1.19(2) . ? O2 C29 1.362(19) . ? O3 C30 1.33(2) . ? O8 C70 1.14(5) . ? O14 C114 1.47(9) . ? O16 C111 2.11(15) . ? O17 C108 1.48(6) . ? O17 C118 1.53(4) . ? N1 C1 1.301(18) . ? N1 N2 1.379(15) . ? N2 C3 1.334(19) . ? N2 B1 1.53(2) . ? N3 C4 1.311(17) . ? N3 N4 1.348(15) . ? N4 C6 1.358(19) . ? N4 B1 1.54(2) . ? N5 N6 1.358(16) . ? N5 C16 1.374(19) . ? N6 C18 1.34(2) . ? N6 B1 1.47(2) . ? N7 C19 1.327(17) . ? N7 N8 1.365(15) . ? N8 C21 1.329(18) . ? N8 B2 1.53(2) . ? N9 C22 1.340(17) . ? N9 N10 1.346(16) . ? N10 C24 1.35(2) . ? N10 B2 1.54(2) . ? N11 C25 1.304(19) . ? N11 N12 1.383(17) . ? N12 C27 1.35(2) . ? N12 B2 1.49(3) . ? N13 C33 1.47(2) . ? N13 C31 1.51(2) . ? N13 C37 1.50(2) . ? N13 C35 1.55(2) . ? N14 C41 1.505(19) . ? N14 C39 1.508(19) . ? N14 C43 1.512(18) . ? N14 C45 1.514(18) . ? N15 C47 1.46(3) . ? N15 C53 1.45(3) . ? N15 C49 1.49(3) . ? N15 C51 1.60(5) . ? N16 C111 1.63(8) . ? N16 C67 1.39(4) . ? N16 C90 1.57(7) . ? N17 C70 1.29(4) . ? N17 C67 1.36(4) . ? N17 C88 1.74(6) . ? C1 C2 1.41(2) . ? C2 C3 1.35(2) . ? C4 C5 1.36(2) . ? C5 C6 1.33(2) . ? C16 C17 1.42(2) . ? C17 C18 1.39(3) . ? C19 C20 1.352(19) . ? C20 C21 1.40(2) . ? C22 C23 1.41(2) . ? C23 C24 1.39(2) . ? C25 C26 1.39(2) . ? C26 C27 1.38(3) . ? C31 C32 1.49(2) . ? C33 C34 1.43(2) . ? C35 C36 1.50(2) . ? C37 C38 1.51(2) . ? C39 C40 1.48(2) . ? C41 C42 1.52(2) . ? C43 C44 1.57(2) . ? C45 C46 1.50(2) . ? C47 C48 1.51(3) . ? C49 C50 1.64(4) . ? C51 C52 1.46(6) . ? C53 C54 1.49(5) . ? C63 C108 1.38(7) . ? C94 C118 1.46(5) . ? C94 C116 2.08(9) . ? C99 C109 1.80(8) . ? C109 C110 1.13(9) . ? C110 C112 1.59(11) . ? C112 C113 1.41(12) . ? C112 C114 1.81(11) . ? C116 C117 1.18(10) . ? C117 C117 0.56(12) 2_556 ? 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 N5 Mo1 N1 79.5(4) . . ? N5 Mo1 N3 79.7(4) . . ? N1 Mo1 N3 80.6(4) . . ? N5 Mo1 S1 162.5(3) . . ? N1 Mo1 S1 87.5(3) . . ? N3 Mo1 S1 86.6(3) . . ? N5 Mo1 S3 88.3(3) . . ? N1 Mo1 S3 164.1(3) . . ? N3 Mo1 S3 87.3(3) . . ? S1 Mo1 S3 102.11(14) . . ? N5 Mo1 S2 88.0(3) . . ? N1 Mo1 S2 86.8(3) . . ? N3 Mo1 S2 163.8(3) . . ? S1 Mo1 S2 103.09(13) . . ? S3 Mo1 S2 103.03(14) . . ? N5 Mo1 Fe1 140.8(3) . . ? N1 Mo1 Fe1 97.7(3) . . ? N3 Mo1 Fe1 139.0(3) . . ? S1 Mo1 Fe1 52.40(10) . . ? S3 Mo1 Fe1 98.13(11) . . ? S2 Mo1 Fe1 52.79(10) . . ? N5 Mo1 Fe3 99.2(3) . . ? N1 Mo1 Fe3 139.2(3) . . ? N3 Mo1 Fe3 139.8(3) . . ? S1 Mo1 Fe3 98.33(11) . . ? S3 Mo1 Fe3 52.57(10) . . ? S2 Mo1 Fe3 52.50(11) . . ? Fe1 Mo1 Fe3 57.84(7) . . ? N5 Mo1 Fe2 140.4(3) . . ? N1 Mo1 Fe2 139.5(3) . . ? N3 Mo1 Fe2 97.8(3) . . ? S1 Mo1 Fe2 52.15(10) . . ? S3 Mo1 Fe2 52.17(10) . . ? S2 Mo1 Fe2 98.47(11) . . ? Fe1 Mo1 Fe2 57.54(6) . . ? Fe3 Mo1 Fe2 57.84(6) . . ? N9 Mo2 N7 79.2(4) . . ? N9 Mo2 N11 81.7(4) . . ? N7 Mo2 N11 79.9(4) . . ? N9 Mo2 S4 89.1(3) . . ? N7 Mo2 S4 87.0(3) . . ? N11 Mo2 S4 165.2(3) . . ? N9 Mo2 S6 85.8(3) . . ? N7 Mo2 S6 162.2(3) . . ? N11 Mo2 S6 88.6(3) . . ? S4 Mo2 S6 102.35(13) . . ? N9 Mo2 S5 163.4(3) . . ? N7 Mo2 S5 89.2(3) . . ? N11 Mo2 S5 84.6(3) . . ? S4 Mo2 S5 102.23(14) . . ? S6 Mo2 S5 103.32(14) . . ? N9 Mo2 Fe4 141.3(3) . . ? N7 Mo2 Fe4 100.2(3) . . ? N11 Mo2 Fe4 136.8(3) . . ? S4 Mo2 Fe4 52.36(10) . . ? S6 Mo2 Fe4 97.51(11) . . ? S5 Mo2 Fe4 52.30(10) . . ? N9 Mo2 Fe6 138.0(3) . . ? N7 Mo2 Fe6 141.9(3) . . ? N11 Mo2 Fe6 95.3(3) . . ? S4 Mo2 Fe6 99.22(11) . . ? S6 Mo2 Fe6 52.23(10) . . ? S5 Mo2 Fe6 52.71(10) . . ? Fe4 Mo2 Fe6 58.15(7) . . ? N9 Mo2 Fe5 98.1(3) . . ? N7 Mo2 Fe5 139.2(3) . . ? N11 Mo2 Fe5 140.5(3) . . ? S4 Mo2 Fe5 52.17(10) . . ? S6 Mo2 Fe5 52.23(10) . . ? S5 Mo2 Fe5 98.52(11) . . ? Fe4 Mo2 Fe5 57.24(6) . . ? Fe6 Mo2 Fe5 58.77(6) . . ? O1 Fe1 S1 113.3(3) . . ? O1 Fe1 S2 120.6(3) . . ? S1 Fe1 S2 110.96(15) . . ? O1 Fe1 S7 93.6(3) . . ? S1 Fe1 S7 109.22(15) . . ? S2 Fe1 S7 107.12(16) . . ? O1 Fe1 Fe3 138.7(3) . . ? S1 Fe1 Fe3 104.57(12) . . ? S2 Fe1 Fe3 55.07(12) . . ? S7 Fe1 Fe3 57.46(11) . . ? O1 Fe1 Fe2 131.3(3) . . ? S1 Fe1 Fe2 55.33(11) . . ? S2 Fe1 Fe2 106.07(13) . . ? S7 Fe1 Fe2 57.93(10) . . ? Fe3 Fe1 Fe2 60.91(8) . . ? O1 Fe1 Mo1 157.0(3) . . ? S1 Fe1 Mo1 56.44(10) . . ? S2 Fe1 Mo1 56.94(11) . . ? S7 Fe1 Mo1 109.09(11) . . ? Fe3 Fe1 Mo1 61.69(7) . . ? Fe2 Fe1 Mo1 62.99(7) . . ? O1 Fe1 Fe4 44.9(3) . . ? S1 Fe1 Fe4 103.86(12) . . ? S2 Fe1 Fe4 144.72(13) . . ? S7 Fe1 Fe4 54.05(10) . . ? Fe3 Fe1 Fe4 111.01(9) . . ? Fe2 Fe1 Fe4 88.85(8) . . ? Mo1 Fe1 Fe4 151.27(9) . . ? S8 Fe2 S1 117.58(16) . . ? S8 Fe2 S3 117.36(16) . . ? S1 Fe2 S3 107.07(15) . . ? S8 Fe2 S7 100.15(15) . . ? S1 Fe2 S7 106.56(14) . . ? S3 Fe2 S7 106.86(15) . . ? S8 Fe2 Fe1 139.53(13) . . ? S1 Fe2 Fe1 53.82(11) . . ? S3 Fe2 Fe1 101.86(13) . . ? S7 Fe2 Fe1 56.58(10) . . ? S8 Fe2 Fe3 139.15(14) . . ? S1 Fe2 Fe3 101.97(12) . . ? S3 Fe2 Fe3 54.13(12) . . ? S7 Fe2 Fe3 56.44(10) . . ? Fe1 Fe2 Fe3 59.21(8) . . ? S8 Fe2 Mo1 154.71(13) . . ? S1 Fe2 Mo1 54.59(10) . . ? S3 Fe2 Mo1 54.91(10) . . ? S7 Fe2 Mo1 105.14(11) . . ? Fe1 Fe2 Mo1 59.47(6) . . ? Fe3 Fe2 Mo1 59.94(7) . . ? S8 Fe2 Fe5 51.15(11) . . ? S1 Fe2 Fe5 106.39(12) . . ? S3 Fe2 Fe5 145.41(13) . . ? S7 Fe2 Fe5 54.47(10) . . ? Fe1 Fe2 Fe5 90.84(8) . . ? Fe3 Fe2 Fe5 109.98(9) . . ? Mo1 Fe2 Fe5 150.07(9) . . ? O3 Fe3 S3 115.7(4) . . ? O3 Fe3 S2 116.2(4) . . ? S3 Fe3 S2 110.08(15) . . ? O3 Fe3 S7 98.6(3) . . ? S3 Fe3 S7 108.41(15) . . ? S2 Fe3 S7 106.62(15) . . ? O3 Fe3 Fe1 139.9(4) . . ? S3 Fe3 Fe1 102.93(13) . . ? S2 Fe3 Fe1 54.84(12) . . ? S7 Fe3 Fe1 57.13(11) . . ? O3 Fe3 Fe2 137.3(4) . . ? S3 Fe3 Fe2 54.78(12) . . ? S2 Fe3 Fe2 105.01(13) . . ? S7 Fe3 Fe2 57.45(10) . . ? Fe1 Fe3 Fe2 59.88(7) . . ? O3 Fe3 Mo1 153.6(3) . . ? S3 Fe3 Mo1 56.03(10) . . ? S2 Fe3 Mo1 56.37(11) . . ? S7 Fe3 Mo1 107.80(11) . . ? Fe1 Fe3 Mo1 60.47(7) . . ? Fe2 Fe3 Mo1 62.22(7) . . ? O1 Fe4 S4 117.8(4) . . ? O1 Fe4 S5 117.1(3) . . ? S4 Fe4 S5 110.28(16) . . ? O1 Fe4 S7 93.4(3) . . ? S4 Fe4 S7 109.45(14) . . ? S5 Fe4 S7 106.55(15) . . ? O1 Fe4 Fe5 133.5(3) . . ? S4 Fe4 Fe5 55.29(11) . . ? S5 Fe4 Fe5 106.36(13) . . ? S7 Fe4 Fe5 57.60(10) . . ? O1 Fe4 Fe6 134.7(3) . . ? S4 Fe4 Fe6 104.80(13) . . ? S5 Fe4 Fe6 55.04(12) . . ? S7 Fe4 Fe6 56.50(11) . . ? Fe5 Fe4 Fe6 61.57(8) . . ? O1 Fe4 Mo2 159.2(3) . . ? S4 Fe4 Mo2 56.32(11) . . ? S5 Fe4 Mo2 56.79(11) . . ? S7 Fe4 Mo2 107.37(12) . . ? Fe5 Fe4 Mo2 62.53(7) . . ? Fe6 Fe4 Mo2 61.17(7) . . ? O1 Fe4 Fe1 44.9(3) . . ? S4 Fe4 Fe1 107.95(12) . . ? S5 Fe4 Fe1 141.31(13) . . ? S7 Fe4 Fe1 53.80(10) . . ? Fe5 Fe4 Fe1 90.49(8) . . ? Fe6 Fe4 Fe1 109.15(9) . . ? Mo2 Fe4 Fe1 152.96(9) . . ? S8 Fe5 S4 115.18(16) . . ? S8 Fe5 S6 118.86(16) . . ? S4 Fe5 S6 108.04(15) . . ? S8 Fe5 S7 100.73(15) . . ? S4 Fe5 S7 108.15(14) . . ? S6 Fe5 S7 104.60(14) . . ? S8 Fe5 Fe4 137.83(14) . . ? S4 Fe5 Fe4 54.35(11) . . ? S6 Fe5 Fe4 102.23(12) . . ? S7 Fe5 Fe4 57.16(10) . . ? S8 Fe5 Fe6 141.05(14) . . ? S4 Fe5 Fe6 102.35(12) . . ? S6 Fe5 Fe6 53.33(11) . . ? S7 Fe5 Fe6 55.62(10) . . ? Fe4 Fe5 Fe6 59.48(7) . . ? S8 Fe5 Mo2 154.05(13) . . ? S4 Fe5 Mo2 55.13(10) . . ? S6 Fe5 Mo2 55.18(10) . . ? S7 Fe5 Mo2 105.19(11) . . ? Fe4 Fe5 Mo2 60.23(6) . . ? Fe6 Fe5 Mo2 59.75(6) . . ? S8 Fe5 Fe2 51.22(11) . . ? S4 Fe5 Fe2 105.66(12) . . ? S6 Fe5 Fe2 144.99(13) . . ? S7 Fe5 Fe2 55.04(10) . . ? Fe4 Fe5 Fe2 89.74(8) . . ? Fe6 Fe5 Fe2 110.09(9) . . ? Mo2 Fe5 Fe2 149.73(9) . . ? O2 Fe6 S6 115.3(3) . . ? O2 Fe6 S5 115.4(3) . . ? S6 Fe6 S5 110.68(16) . . ? O2 Fe6 S7 101.1(3) . . ? S6 Fe6 S7 106.56(14) . . ? S5 Fe6 S7 106.55(15) . . ? O2 Fe6 Fe4 141.1(3) . . ? S6 Fe6 Fe4 102.52(12) . . ? S5 Fe6 Fe4 54.22(11) . . ? S7 Fe6 Fe4 57.31(10) . . ? O2 Fe6 Fe5 140.0(3) . . ? S6 Fe6 Fe5 54.25(11) . . ? S5 Fe6 Fe5 103.47(12) . . ? S7 Fe6 Fe5 56.83(10) . . ? Fe4 Fe6 Fe5 58.94(7) . . ? O2 Fe6 Mo2 151.3(3) . . ? S6 Fe6 Mo2 56.16(10) . . ? S5 Fe6 Mo2 56.38(11) . . ? S7 Fe6 Mo2 107.63(12) . . ? Fe4 Fe6 Mo2 60.68(7) . . ? Fe5 Fe6 Mo2 61.49(7) . . ? Fe1 S1 Fe2 70.85(12) . . ? Fe1 S1 Mo1 71.17(12) . . ? Fe2 S1 Mo1 73.26(12) . . ? Fe1 S2 Fe3 70.09(13) . . ? Fe1 S2 Mo1 70.27(12) . . ? Fe3 S2 Mo1 71.13(12) . . ? Fe3 S3 Fe2 71.09(12) . . ? Fe3 S3 Mo1 71.40(12) . . ? Fe2 S3 Mo1 72.92(12) . . ? Fe4 S4 Fe5 70.36(12) . . ? Fe4 S4 Mo2 71.32(12) . . ? Fe5 S4 Mo2 72.70(12) . . ? Fe4 S5 Fe6 70.74(12) . . ? Fe4 S5 Mo2 70.91(11) . . ? Fe6 S5 Mo2 70.91(11) . . ? Fe6 S6 Fe5 72.42(13) . . ? Fe6 S6 Mo2 71.62(12) . . ? Fe5 S6 Mo2 72.59(12) . . ? Fe6 S7 Fe1 136.24(17) . . ? Fe6 S7 Fe3 149.39(17) . . ? Fe1 S7 Fe3 65.41(12) . . ? Fe6 S7 Fe4 66.18(11) . . ? Fe1 S7 Fe4 72.14(12) . . ? Fe3 S7 Fe4 136.69(18) . . ? Fe6 S7 Fe5 67.55(12) . . ? Fe1 S7 Fe5 106.50(15) . . ? Fe3 S7 Fe5 135.01(16) . . ? Fe4 S7 Fe5 65.24(11) . . ? Fe6 S7 Fe2 137.03(17) . . ? Fe1 S7 Fe2 65.49(11) . . ? Fe3 S7 Fe2 66.11(11) . . ? Fe4 S7 Fe2 103.94(15) . . ? Fe5 S7 Fe2 70.49(11) . . ? Fe5 S8 Fe2 77.63(13) . . ? C28 O1 Fe1 122.1(13) . . ? C28 O1 Fe4 120.3(14) . . ? Fe1 O1 Fe4 90.2(5) . . ? C29 O2 Fe6 122.0(11) . . ? C30 O3 Fe3 119.3(11) . . ? C108 O17 C118 121(4) . . ? C1 N1 N2 106.8(12) . . ? C1 N1 Mo1 132.1(11) . . ? N2 N1 Mo1 121.1(9) . . ? C3 N2 N1 108.5(13) . . ? C3 N2 B1 130.6(14) . . ? N1 N2 B1 120.7(12) . . ? C4 N3 N4 107.4(12) . . ? C4 N3 Mo1 129.9(10) . . ? N4 N3 Mo1 122.5(10) . . ? N3 N4 C6 106.3(14) . . ? N3 N4 B1 119.6(13) . . ? C6 N4 B1 134.1(15) . . ? N6 N5 C16 108.2(13) . . ? N6 N5 Mo1 120.9(10) . . ? C16 N5 Mo1 130.9(11) . . ? C18 N6 N5 109.0(15) . . ? C18 N6 B1 128.4(17) . . ? N5 N6 B1 122.6(14) . . ? C19 N7 N8 105.4(12) . . ? C19 N7 Mo2 132.3(10) . . ? N8 N7 Mo2 122.2(9) . . ? C21 N8 N7 110.2(14) . . ? C21 N8 B2 129.8(15) . . ? N7 N8 B2 120.0(13) . . ? C22 N9 N10 107.6(12) . . ? C22 N9 Mo2 130.7(10) . . ? N10 N9 Mo2 121.5(10) . . ? C24 N10 N9 109.3(15) . . ? C24 N10 B2 128.6(16) . . ? N9 N10 B2 122.1(14) . . ? C25 N11 N12 108.4(13) . . ? C25 N11 Mo2 131.2(12) . . ? N12 N11 Mo2 120.4(10) . . ? C27 N12 N11 107.2(16) . . ? C27 N12 B2 130.0(17) . . ? N11 N12 B2 121.6(14) . . ? C33 N13 C31 109.0(13) . . ? C33 N13 C37 108.5(14) . . ? C31 N13 C37 113.1(14) . . ? C33 N13 C35 110.0(14) . . ? C31 N13 C35 109.3(14) . . ? C37 N13 C35 106.9(13) . . ? C41 N14 C39 109.5(12) . . ? C41 N14 C43 110.7(13) . . ? C39 N14 C43 107.3(12) . . ? C41 N14 C45 107.1(12) . . ? C39 N14 C45 111.0(12) . . ? C43 N14 C45 111.3(12) . . ? C47 N15 C53 101(2) . . ? C47 N15 C49 111(2) . . ? C53 N15 C49 115(3) . . ? C47 N15 C51 115(3) . . ? C53 N15 C51 105(2) . . ? C49 N15 C51 111(3) . . ? C111 N16 C67 123(4) . . ? C111 N16 C90 94(4) . . ? C67 N16 C90 143(4) . . ? C70 N17 C67 133(3) . . ? C70 N17 C88 115(4) . . ? C67 N17 C88 113(3) . . ? N6 B1 N2 108.6(15) . . ? N6 B1 N4 108.0(14) . . ? N2 B1 N4 109.0(15) . . ? N12 B2 N10 106.9(14) . . ? N12 B2 N8 110.0(16) . . ? N10 B2 N8 107.4(15) . . ? N1 C1 C2 110.8(15) . . ? C3 C2 C1 104.0(15) . . ? N2 C3 C2 109.9(15) . . ? N3 C4 C5 111.6(15) . . ? C6 C5 C4 103.7(15) . . ? C5 C6 N4 111.0(16) . . ? N5 C16 C17 107.9(17) . . ? C18 C17 C16 104.7(18) . . ? N6 C18 C17 110.1(17) . . ? N7 C19 C20 112.2(14) . . ? C19 C20 C21 104.6(14) . . ? N8 C21 C20 107.6(14) . . ? N9 C22 C23 110.2(15) . . ? C24 C23 C22 103.6(15) . . ? N10 C24 C23 109.3(16) . . ? N11 C25 C26 110.3(17) . . ? C27 C26 C25 104.7(18) . . ? N12 C27 C26 109.2(18) . . ? C32 C31 N13 116.5(15) . . ? C34 C33 N13 118.7(15) . . ? C36 C35 N13 113.9(14) . . ? C38 C37 N13 115.9(16) . . ? C40 C39 N14 118.4(15) . . ? N14 C41 C42 115.8(14) . . ? N14 C43 C44 112.7(13) . . ? C46 C45 N14 115.7(13) . . ? N15 C47 C48 113.2(19) . . ? N15 C49 C50 113(2) . . ? C52 C51 N15 108(3) . . ? C54 C53 N15 114(3) . . ? N17 C67 N16 70(3) . . ? O8 C70 N17 126(4) . . ? C118 C94 C116 113(4) . . ? C63 C108 O17 103(5) . . ? C110 C109 C99 109(8) . . ? C109 C110 C112 107(9) . . ? N16 C111 O16 159(7) . . ? C113 C112 C110 93(8) . . ? C113 C112 C114 119(9) . . ? C110 C112 C114 143(8) . . ? O14 C114 C112 153(7) . . ? C94 C116 C117 143(8) . . ? C117 C117 C116 156(10) 2_556 . ? C94 C118 O17 116(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.369 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.143 #--------------------------------END data_(Et4N)2[Tp2Mo2Fe6S7(OMe)4]MeCN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ' not measured ' _chemical_formula_moiety (Et4N)2[Tp2Mo2Fe6S7(OMe)4]MeCN _chemical_formula_sum 'C40 H87 B2 Fe6 Mo2 N15 O4 S7' _chemical_formula_weight 1615.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 P21/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 19.989(7) _cell_length_b 16.420(6) _cell_length_c 23.472(9) _cell_angle_alpha 90.00 _cell_angle_beta 112.549(8) _cell_angle_gamma 90.00 _cell_volume 7115(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark black' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 1.777 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ? _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 APEX ' _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_% none _diffrn_reflns_number 24070 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0764 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 20.00 _reflns_number_total 6637 _reflns_number_gt 4874 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1405P)^2^+162.4500P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6637 _refine_ls_number_parameters 689 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0983 _refine_ls_wR_factor_ref 0.2797 _refine_ls_wR_factor_gt 0.2625 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 1.181 _refine_ls_shift/su_mean 0.027 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 -0.07865(11) 0.05300(10) 0.65979(9) 0.0351(6) Uani 1 1 d . A 1 Mo2 Mo 0.10686(11) 0.45533(11) 0.73247(9) 0.0373(6) Uani 1 1 d . A 1 Fe1 Fe -0.16203(17) 0.19019(18) 0.62353(15) 0.0377(9) Uani 1 1 d . . . Fe2 Fe -0.05124(17) 0.19111(18) 0.72764(15) 0.0378(9) Uani 1 1 d . A . Fe3 Fe -0.02998(16) 0.18847(17) 0.62613(14) 0.0337(8) Uani 1 1 d . A . Fe4 Fe -0.04052(18) 0.45462(18) 0.66998(15) 0.0399(9) Uani 1 1 d . . . Fe5 Fe 0.01917(18) 0.34746(19) 0.75599(15) 0.0413(9) Uani 1 1 d . A . Fe6 Fe 0.03929(17) 0.33738(17) 0.65462(14) 0.0346(8) Uani 1 1 d . A . S1 S -0.1228(3) 0.1157(3) 0.5605(3) 0.0377(14) Uani 1 1 d . A . S2 S -0.1518(3) 0.1142(3) 0.7085(3) 0.0426(15) Uani 1 1 d . A . S3 S 0.0354(3) 0.1166(3) 0.7118(3) 0.0408(15) Uani 1 1 d . . . S4 S 0.0408(3) 0.4660(3) 0.6235(3) 0.0396(15) Uani 1 1 d . A . S5 S 0.0157(3) 0.4835(4) 0.7726(3) 0.0481(16) Uani 1 1 d . A . S6 S 0.1256(3) 0.3131(3) 0.7497(3) 0.0444(16) Uani 1 1 d . . . S7 S -0.0784(3) 0.3086(3) 0.6583(3) 0.0358(14) Uani 1 1 d . A . O1 O 0.0292(8) 0.2528(8) 0.5926(6) 0.037(4) Uani 1 1 d . . . O2 O -0.0152(8) 0.2632(9) 0.8004(8) 0.054(4) Uani 1 1 d . . . O3 O -0.2513(9) 0.2461(10) 0.5835(9) 0.061(5) Uani 1 1 d . A . O4 O -0.1320(8) 0.5047(9) 0.6320(8) 0.056(4) Uani 1 1 d . A . N1 N -0.0173(11) -0.0315(9) 0.6213(9) 0.048(5) Uani 1 1 d . . . N2 N -0.0250(12) -0.1145(12) 0.6223(9) 0.054(6) Uani 1 1 d . A . N3 N -0.1667(13) -0.0400(11) 0.6197(9) 0.050(5) Uani 1 1 d . . . N4 N -0.1477(14) -0.1232(12) 0.6244(11) 0.061(6) Uani 1 1 d . A . N5 N -0.0406(11) -0.0401(12) 0.7355(10) 0.049(5) Uani 1 1 d . . . N6 N -0.0421(13) -0.1218(12) 0.7209(11) 0.064(6) Uani 1 1 d . A . N7 N 0.1276(12) 0.5899(11) 0.7299(9) 0.055(6) Uani 1 1 d . . . N8 N 0.1988(12) 0.6189(12) 0.7545(9) 0.054(6) Uani 1 1 d . A . N9 N 0.1862(10) 0.4737(11) 0.8279(10) 0.047(5) Uani 1 1 d . . . N10 N 0.2472(12) 0.5206(12) 0.8416(10) 0.055(6) Uani 1 1 d . A . N11 N 0.2072(10) 0.4475(10) 0.7135(9) 0.046(5) Uani 1 1 d . . . N12 N 0.2677(12) 0.4933(11) 0.7443(10) 0.057(6) Uani 1 1 d . A . N13 N 0.7575(14) 0.3848(17) 0.7374(13) 0.093(8) Uani 1 1 d . . . N14 N 0.8080(11) 0.3889(11) 0.4563(9) 0.056(6) Uani 1 1 d . . . N22 N 0.185(3) 0.732(4) 0.915(3) 0.12(2) Uiso 0.50 1 d P . . B1 B -0.072(3) -0.1485(18) 0.6557(18) 0.073(12) Uani 1 1 d . . . H1 H -0.070(14) -0.208(18) 0.655(12) 0.087 Uiso 1 1 calc . . . B2 B 0.2626(19) 0.561(2) 0.7918(17) 0.065(10) Uani 1 1 d . . . H2 H 0.308(14) 0.591(16) 0.809(12) 0.078 Uiso 1 1 calc . . . C1 C 0.0836(14) 0.2240(13) 0.5792(11) 0.050(7) Uani 1 1 d . A . H1A H 0.0866 0.2539 0.5451 0.075 Uiso 1 1 calc R . . H1B H 0.0753 0.1674 0.5683 0.075 Uiso 1 1 calc R . . H1C H 0.1282 0.2298 0.6144 0.075 Uiso 1 1 calc R . . C2 C 0.035(2) 0.2342(19) 0.8578(12) 0.120(16) Uani 1 1 d . A . H2A H 0.0144 0.2378 0.8883 0.180 Uiso 1 1 calc R . . H2B H 0.0785 0.2667 0.8704 0.180 Uiso 1 1 calc R . . H2C H 0.0471 0.1785 0.8534 0.180 Uiso 1 1 calc R . . C3 C -0.307(2) 0.205(2) 0.5514(18) 0.106(13) Uani 1 1 d . . . H3A H -0.2995 0.1801 0.5175 0.159 Uiso 1 1 calc R A . H3B H -0.3484 0.2406 0.5360 0.159 Uiso 1 1 calc R . . H3C H -0.3158 0.1637 0.5767 0.159 Uiso 1 1 calc R . . C4 C -0.1375(17) 0.5905(16) 0.6347(14) 0.083(9) Uani 1 1 d . . . H4A H -0.1089 0.6090 0.6757 0.125 Uiso 1 1 calc R A . H4B H -0.1872 0.6055 0.6244 0.125 Uiso 1 1 calc R . . H4C H -0.1201 0.6153 0.6060 0.125 Uiso 1 1 calc R . . C5 C -0.2358(18) -0.0354(16) 0.5850(13) 0.060(8) Uani 1 1 d . A . H5 H -0.2615 0.0131 0.5735 0.072 Uiso 1 1 calc R . . C6 C -0.2652(18) -0.111(2) 0.5678(13) 0.077(9) Uani 1 1 d . . . H6 H -0.3136 -0.1232 0.5459 0.092 Uiso 1 1 calc R A . C7 C -0.209(2) -0.163(2) 0.5895(16) 0.081(10) Uani 1 1 d . A . H7 H -0.2120 -0.2183 0.5815 0.097 Uiso 1 1 calc R . . C8 C 0.0228(14) -0.0189(14) 0.5886(12) 0.050(7) Uani 1 1 d . A . H8 H 0.0358 0.0326 0.5800 0.060 Uiso 1 1 calc R . . C9 C 0.0425(16) -0.0874(18) 0.5692(12) 0.070(9) Uani 1 1 d . . . H9 H 0.0696 -0.0932 0.5449 0.084 Uiso 1 1 calc R A . C10 C 0.0131(16) -0.1489(18) 0.5942(12) 0.066(8) Uani 1 1 d . A . H10 H 0.0195 -0.2046 0.5913 0.079 Uiso 1 1 calc R . . C11 C -0.0129(14) -0.0340(17) 0.7946(15) 0.065(8) Uani 1 1 d . A . H11 H -0.0090 0.0146 0.8160 0.078 Uiso 1 1 calc R . . C12 C 0.0107(18) -0.1097(19) 0.8230(15) 0.077(9) Uani 1 1 d . . . H12 H 0.0359 -0.1211 0.8646 0.092 Uiso 1 1 calc R A . C13 C -0.0130(16) -0.1633(18) 0.7735(18) 0.078(10) Uani 1 1 d . A . H13 H -0.0091 -0.2197 0.7765 0.094 Uiso 1 1 calc R . . C14 C 0.0833(13) 0.6536(14) 0.7078(12) 0.055(7) Uani 1 1 d . A . H14 H 0.0330 0.6523 0.6892 0.066 Uiso 1 1 calc R . . C15 C 0.1278(19) 0.7224(15) 0.7180(13) 0.070(8) Uani 1 1 d . . . H15 H 0.1120 0.7755 0.7068 0.084 Uiso 1 1 calc R A . C16 C 0.1955(17) 0.6993(15) 0.7461(12) 0.059(7) Uani 1 1 d . A . H16 H 0.2353 0.7340 0.7584 0.071 Uiso 1 1 calc R . . C17 C 0.1832(18) 0.4474(14) 0.8826(15) 0.081(10) Uani 1 1 d . A . H17 H 0.1473 0.4162 0.8881 0.097 Uiso 1 1 calc R . . C18 C 0.2481(18) 0.4791(18) 0.9290(12) 0.076(10) Uani 1 1 d . . . H18 H 0.2628 0.4715 0.9714 0.091 Uiso 1 1 calc R A . C19 C 0.2856(15) 0.5233(15) 0.8996(15) 0.060(7) Uani 1 1 d . A . H19 H 0.3299 0.5496 0.9186 0.072 Uiso 1 1 calc R . . C20 C 0.2306(13) 0.3939(14) 0.6810(11) 0.043(6) Uani 1 1 d . A . H20 H 0.2020 0.3535 0.6554 0.052 Uiso 1 1 calc R . . C21 C 0.3028(13) 0.4074(16) 0.6911(12) 0.052(7) Uani 1 1 d . . . H21 H 0.3302 0.3789 0.6734 0.062 Uiso 1 1 calc R A . C22 C 0.3266(14) 0.4719(16) 0.7329(13) 0.061(8) Uani 1 1 d . A . H22 H 0.3726 0.4948 0.7493 0.073 Uiso 1 1 calc R . . C23 C 0.771(2) 0.461(3) 0.7794(16) 0.133(18) Uani 1 1 d . . . H23A H 0.7300 0.4977 0.7622 0.160 Uiso 1 1 calc R . . H23B H 0.7733 0.4440 0.8198 0.160 Uiso 1 1 calc R . . C24 C 0.839(2) 0.505(3) 0.786(3) 0.22(4) Uani 1 1 d . . . H24A H 0.8800 0.4749 0.8136 0.324 Uiso 1 1 calc R . . H24B H 0.8386 0.5581 0.8032 0.324 Uiso 1 1 calc R . . H24C H 0.8422 0.5101 0.7467 0.324 Uiso 1 1 calc R . . C25 C 0.823(2) 0.334(3) 0.7603(18) 0.130(16) Uani 1 1 d . . . H25A H 0.8653 0.3686 0.7667 0.156 Uiso 1 1 calc R . . H25B H 0.8209 0.2939 0.7295 0.156 Uiso 1 1 calc R . . C26 C 0.833(2) 0.289(3) 0.825(2) 0.146(17) Uani 1 1 d . . . H26A H 0.8534 0.3263 0.8587 0.219 Uiso 1 1 calc R . . H26B H 0.8650 0.2431 0.8311 0.219 Uiso 1 1 calc R . . H26C H 0.7868 0.2705 0.8232 0.219 Uiso 1 1 calc R . . C27 C 0.691(2) 0.342(3) 0.736(2) 0.142(19) Uani 1 1 d . . . H27A H 0.6503 0.3789 0.7216 0.170 Uiso 1 1 calc R . . H27B H 0.6981 0.3251 0.7777 0.170 Uiso 1 1 calc R . . C28 C 0.674(3) 0.265(3) 0.693(3) 0.18(2) Uani 1 1 d . . . H28A H 0.7173 0.2448 0.6908 0.268 Uiso 1 1 calc R . . H28B H 0.6398 0.2795 0.6530 0.268 Uiso 1 1 calc R . . H28C H 0.6526 0.2235 0.7103 0.268 Uiso 1 1 calc R . . C29 C 0.744(2) 0.413(3) 0.6697(16) 0.124(15) Uani 1 1 d . . . H29A H 0.7905 0.4295 0.6687 0.149 Uiso 1 1 calc R . . H29B H 0.7278 0.3661 0.6426 0.149 Uiso 1 1 calc R . . C30 C 0.691(2) 0.481(4) 0.644(2) 0.21(3) Uani 1 1 d . . . H30A H 0.6644 0.4891 0.6705 0.312 Uiso 1 1 calc R . . H30B H 0.6578 0.4674 0.6035 0.312 Uiso 1 1 calc R . . H30C H 0.7164 0.5302 0.6431 0.312 Uiso 1 1 calc R . . C31 C 0.8188(14) 0.4735(16) 0.4329(13) 0.064(8) Uani 1 1 d . . . H31A H 0.8478 0.4672 0.4082 0.077 Uiso 1 1 calc R . . H31B H 0.7718 0.4942 0.4060 0.077 Uiso 1 1 calc R . . C32 C 0.8528(17) 0.5333(14) 0.4799(12) 0.071(8) Uani 1 1 d . . . H32A H 0.8315 0.5314 0.5102 0.107 Uiso 1 1 calc R . . H32B H 0.8459 0.5865 0.4616 0.107 Uiso 1 1 calc R . . H32C H 0.9037 0.5218 0.4993 0.107 Uiso 1 1 calc R . . C33 C 0.8812(14) 0.3542(16) 0.4940(11) 0.060(7) Uani 1 1 d . . . H33A H 0.8744 0.3004 0.5079 0.072 Uiso 1 1 calc R . . H33B H 0.9031 0.3879 0.5304 0.072 Uiso 1 1 calc R . . C34 C 0.9351(17) 0.3471(18) 0.4616(15) 0.086(10) Uani 1 1 d . . . H34A H 0.9647 0.2996 0.4764 0.129 Uiso 1 1 calc R . . H34B H 0.9654 0.3947 0.4704 0.129 Uiso 1 1 calc R . . H34C H 0.9089 0.3427 0.4178 0.129 Uiso 1 1 calc R . . C35 C 0.7643(18) 0.393(2) 0.4976(14) 0.092(11) Uani 1 1 d . . . H35A H 0.7909 0.4248 0.5342 0.110 Uiso 1 1 calc R . . H35B H 0.7580 0.3385 0.5107 0.110 Uiso 1 1 calc R . . C36 C 0.688(2) 0.433(2) 0.462(3) 0.26(4) Uani 1 1 d . . . H36A H 0.6927 0.4777 0.4379 0.389 Uiso 1 1 calc R . . H36B H 0.6688 0.4523 0.4917 0.389 Uiso 1 1 calc R . . H36C H 0.6555 0.3932 0.4360 0.389 Uiso 1 1 calc R . . C37 C 0.7737(17) 0.3397(17) 0.4017(13) 0.071(8) Uani 1 1 d . . . H37A H 0.8013 0.3454 0.3757 0.086 Uiso 1 1 calc R . . H37B H 0.7257 0.3615 0.3790 0.086 Uiso 1 1 calc R . . C38 C 0.766(2) 0.2438(17) 0.4131(16) 0.127(16) Uani 1 1 d . . . H38A H 0.7626 0.2363 0.4525 0.190 Uiso 1 1 calc R . . H38B H 0.8076 0.2153 0.4125 0.190 Uiso 1 1 calc R . . H38C H 0.7230 0.2229 0.3813 0.190 Uiso 1 1 calc R . . C113 C 0.136(4) 0.672(5) 0.885(3) 0.11(2) Uiso 0.50 1 d P . . C114 C 0.022(6) 0.642(7) 0.941(5) 0.19(4) Uiso 0.50 1 d P . . 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 0.0526(13) 0.0152(10) 0.0456(13) 0.0022(9) 0.0279(11) -0.0001(9) Mo2 0.0462(13) 0.0209(11) 0.0417(13) -0.0015(9) 0.0133(10) -0.0017(9) Fe1 0.044(2) 0.0223(17) 0.052(2) 0.0042(15) 0.0246(17) 0.0018(15) Fe2 0.050(2) 0.0249(18) 0.045(2) 0.0001(15) 0.0247(17) 0.0011(15) Fe3 0.045(2) 0.0186(17) 0.044(2) 0.0026(14) 0.0236(17) -0.0005(14) Fe4 0.051(2) 0.0208(18) 0.047(2) -0.0001(15) 0.0174(17) 0.0039(16) Fe5 0.053(2) 0.0273(18) 0.046(2) -0.0027(16) 0.0224(18) -0.0043(16) Fe6 0.045(2) 0.0195(17) 0.040(2) -0.0018(14) 0.0170(16) -0.0059(15) S1 0.053(4) 0.027(3) 0.037(3) 0.000(3) 0.022(3) -0.002(3) S2 0.056(4) 0.030(3) 0.057(4) 0.000(3) 0.038(3) 0.000(3) S3 0.045(4) 0.024(3) 0.057(4) 0.010(3) 0.023(3) 0.009(3) S4 0.052(4) 0.023(3) 0.039(3) 0.002(3) 0.011(3) -0.003(3) S5 0.061(4) 0.032(3) 0.054(4) -0.006(3) 0.025(3) 0.003(3) S6 0.052(4) 0.024(3) 0.054(4) 0.002(3) 0.018(3) 0.001(3) S7 0.044(3) 0.024(3) 0.043(4) 0.004(3) 0.020(3) -0.001(3) O1 0.047(9) 0.026(8) 0.046(9) -0.001(7) 0.026(8) 0.002(7) O2 0.050(10) 0.045(10) 0.064(13) -0.002(9) 0.020(9) -0.010(8) O3 0.036(10) 0.041(11) 0.105(15) -0.007(10) 0.027(10) -0.018(9) O4 0.055(10) 0.032(10) 0.076(12) -0.003(9) 0.018(9) 0.000(8) N1 0.095(16) 0.000(11) 0.066(14) -0.002(9) 0.048(13) -0.003(10) N2 0.089(16) 0.035(14) 0.043(13) 0.004(10) 0.031(13) 0.020(12) N3 0.089(18) 0.023(13) 0.046(13) -0.010(10) 0.034(14) -0.015(12) N4 0.083(19) 0.027(14) 0.092(18) 0.000(12) 0.054(16) -0.012(14) N5 0.071(14) 0.039(15) 0.041(14) 0.019(10) 0.025(12) 0.012(11) N6 0.104(18) 0.023(14) 0.078(18) 0.022(14) 0.050(15) 0.002(12) N7 0.074(16) 0.025(12) 0.065(14) -0.023(11) 0.025(13) -0.022(13) N8 0.073(16) 0.023(14) 0.062(14) -0.012(10) 0.020(13) -0.018(11) N9 0.043(13) 0.026(11) 0.066(16) 0.005(11) 0.014(11) 0.001(11) N10 0.068(16) 0.033(13) 0.041(16) -0.003(11) -0.003(13) 0.004(12) N11 0.064(13) 0.011(10) 0.062(13) -0.004(10) 0.022(12) -0.020(11) N12 0.081(17) 0.017(11) 0.069(15) -0.014(11) 0.024(13) -0.022(12) N13 0.09(2) 0.10(2) 0.11(2) -0.011(18) 0.060(18) 0.025(17) N14 0.075(16) 0.024(11) 0.057(14) 0.024(11) 0.014(13) 0.003(11) B1 0.13(4) 0.010(16) 0.08(3) -0.014(18) 0.05(3) -0.01(2) B2 0.06(2) 0.04(2) 0.07(3) -0.008(19) -0.005(19) 0.012(17) C1 0.08(2) 0.016(12) 0.053(16) 0.005(11) 0.029(15) -0.014(13) C2 0.24(4) 0.09(2) 0.030(18) -0.026(17) 0.05(2) -0.11(3) C3 0.13(3) 0.07(2) 0.16(4) 0.06(2) 0.10(3) 0.03(2) C4 0.11(3) 0.05(2) 0.09(2) -0.006(17) 0.03(2) 0.003(17) C5 0.08(2) 0.037(18) 0.056(18) 0.000(14) 0.024(18) -0.032(17) C6 0.07(2) 0.10(3) 0.07(2) -0.012(19) 0.030(18) -0.04(2) C7 0.09(3) 0.06(2) 0.11(3) -0.04(2) 0.06(2) -0.04(2) C8 0.084(19) 0.022(14) 0.075(18) -0.011(13) 0.064(17) -0.001(13) C9 0.10(2) 0.07(2) 0.063(19) 0.013(17) 0.063(19) 0.045(19) C10 0.10(2) 0.052(18) 0.051(17) -0.014(15) 0.034(17) 0.007(17) C11 0.069(19) 0.052(19) 0.08(2) 0.026(17) 0.031(17) -0.002(15) C12 0.12(3) 0.05(2) 0.07(2) 0.028(19) 0.04(2) 0.006(19) C13 0.08(2) 0.039(18) 0.14(3) 0.04(2) 0.06(2) 0.007(17) C14 0.049(16) 0.023(15) 0.077(19) 0.018(13) 0.007(14) 0.023(15) C15 0.10(3) 0.019(16) 0.08(2) -0.003(14) 0.02(2) -0.001(17) C16 0.07(2) 0.022(18) 0.065(19) -0.022(13) 0.006(17) -0.023(15) C17 0.11(3) 0.009(13) 0.08(2) -0.002(15) -0.01(2) 0.011(15) C18 0.11(3) 0.054(19) 0.033(16) -0.005(15) 0.000(19) 0.039(19) C19 0.060(18) 0.032(16) 0.07(2) -0.002(15) 0.007(19) -0.004(14) C20 0.054(18) 0.024(13) 0.055(16) 0.008(12) 0.024(14) 0.004(12) C21 0.039(17) 0.054(18) 0.069(18) -0.007(15) 0.027(14) -0.010(13) C22 0.039(16) 0.059(19) 0.09(2) -0.007(17) 0.032(16) 0.000(14) C23 0.15(4) 0.17(4) 0.09(3) -0.02(3) 0.07(3) 0.11(3) C24 0.11(3) 0.22(6) 0.35(8) -0.22(6) 0.11(4) -0.09(4) C25 0.11(3) 0.19(4) 0.12(3) 0.02(3) 0.08(3) 0.08(3) C26 0.19(5) 0.12(4) 0.15(4) 0.01(3) 0.09(4) 0.07(3) C27 0.12(3) 0.15(4) 0.23(5) 0.04(4) 0.15(4) 0.01(3) C28 0.19(5) 0.11(3) 0.32(7) -0.09(4) 0.19(5) -0.06(3) C29 0.10(3) 0.20(5) 0.07(3) 0.02(3) 0.03(2) -0.01(3) C30 0.11(3) 0.37(8) 0.17(4) 0.19(5) 0.09(3) 0.13(5) C31 0.054(17) 0.055(18) 0.09(2) 0.010(17) 0.036(16) -0.007(14) C32 0.13(3) 0.027(15) 0.07(2) 0.002(14) 0.049(19) -0.016(16) C33 0.074(19) 0.052(17) 0.037(15) 0.016(13) 0.002(15) -0.011(15) C34 0.10(2) 0.07(2) 0.10(2) 0.037(19) 0.06(2) 0.047(19) C35 0.11(3) 0.11(3) 0.07(2) -0.02(2) 0.06(2) -0.05(2) C36 0.11(3) 0.08(3) 0.66(14) -0.10(5) 0.23(6) -0.03(3) C37 0.09(2) 0.07(2) 0.054(19) -0.001(16) 0.030(17) 0.006(17) C38 0.20(4) 0.04(2) 0.09(2) 0.015(18) 0.01(3) -0.05(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N5 2.244(19) . ? Mo1 N3 2.25(2) . ? Mo1 N1 2.257(18) . ? Mo1 S3 2.375(6) . ? Mo1 S1 2.386(6) . ? Mo1 S2 2.395(6) . ? Mo1 Fe3 2.666(3) . ? Mo1 Fe2 2.704(4) . ? Mo1 Fe1 2.737(4) . ? Mo2 N9 2.21(2) . ? Mo2 N11 2.22(2) . ? Mo2 N7 2.253(19) . ? Mo2 S6 2.376(6) . ? Mo2 S4 2.393(6) . ? Mo2 S5 2.395(6) . ? Mo2 Fe6 2.650(4) . ? Mo2 Fe5 2.694(4) . ? Mo2 Fe4 2.742(4) . ? Fe1 O3 1.904(17) . ? Fe1 S1 2.279(6) . ? Fe1 S2 2.294(6) . ? Fe1 S7 2.488(6) . ? Fe1 Fe2 2.593(5) . ? Fe1 Fe3 2.617(4) . ? Fe2 O2 1.974(16) . ? Fe2 S3 2.264(6) . ? Fe2 S2 2.268(6) . ? Fe2 S7 2.448(6) . ? Fe2 Fe3 2.576(4) . ? Fe2 Fe5 2.880(4) . ? Fe3 O1 1.961(14) . ? Fe3 S1 2.247(6) . ? Fe3 S3 2.263(6) . ? Fe3 S7 2.441(6) . ? Fe3 Fe6 2.763(4) . ? Fe4 O4 1.888(16) . ? Fe4 S5 2.283(7) . ? Fe4 S4 2.286(7) . ? Fe4 S7 2.498(6) . ? Fe4 Fe5 2.598(5) . ? Fe4 Fe6 2.612(4) . ? Fe5 O2 2.006(16) . ? Fe5 S6 2.259(7) . ? Fe5 S5 2.274(7) . ? Fe5 S7 2.458(7) . ? Fe5 Fe6 2.566(5) . ? Fe6 O1 1.964(14) . ? Fe6 S4 2.239(6) . ? Fe6 S6 2.272(7) . ? Fe6 S7 2.434(6) . ? O1 C1 1.33(3) . ? O2 C2 1.42(3) . ? O3 C3 1.27(4) . ? O4 C4 1.42(3) . ? N1 C8 1.32(3) . ? N1 N2 1.37(2) . ? N2 C10 1.31(3) . ? N2 B1 1.54(4) . ? N3 C5 1.31(3) . ? N3 N4 1.41(3) . ? N4 C7 1.35(4) . ? N4 B1 1.47(5) . ? N5 C11 1.29(3) . ? N5 N6 1.38(3) . ? N6 C13 1.33(4) . ? N6 B1 1.48(4) . ? N7 C14 1.34(3) . ? N7 N8 1.40(3) . ? N8 C16 1.33(3) . ? N8 B2 1.57(4) . ? N9 N10 1.37(3) . ? N9 C17 1.38(4) . ? N10 C19 1.28(3) . ? N10 B2 1.47(4) . ? N11 C20 1.36(3) . ? N11 N12 1.37(3) . ? N12 C22 1.35(3) . ? N12 B2 1.60(4) . ? N13 C25 1.47(4) . ? N13 C27 1.50(4) . ? N13 C23 1.55(4) . ? N13 C29 1.58(4) . ? N14 C37 1.45(3) . ? N14 C33 1.50(3) . ? N14 C35 1.53(3) . ? N14 C31 1.54(3) . ? N22 C113 1.38(9) . ? C5 C6 1.36(4) . ? C6 C7 1.35(4) . ? C8 C9 1.33(3) . ? C9 C10 1.41(4) . ? C11 C12 1.40(4) . ? C12 C13 1.39(4) . ? C14 C15 1.40(3) . ? C15 C16 1.31(4) . ? C17 C18 1.43(4) . ? C18 C19 1.40(4) . ? C20 C21 1.39(3) . ? C21 C22 1.40(3) . ? C23 C24 1.50(5) . ? C25 C26 1.64(5) . ? C27 C28 1.56(5) . ? C29 C30 1.51(5) . ? C31 C32 1.44(3) . ? C33 C34 1.54(3) . ? C35 C36 1.57(5) . ? C37 C38 1.61(4) . ? C113 C114 3.08(13) . ? 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 N5 Mo1 N3 80.9(8) . . ? N5 Mo1 N1 80.0(7) . . ? N3 Mo1 N1 82.7(7) . . ? N5 Mo1 S3 85.8(6) . . ? N3 Mo1 S3 163.3(6) . . ? N1 Mo1 S3 85.1(5) . . ? N5 Mo1 S1 162.4(6) . . ? N3 Mo1 S1 87.0(5) . . ? N1 Mo1 S1 85.9(5) . . ? S3 Mo1 S1 103.5(2) . . ? N5 Mo1 S2 89.5(5) . . ? N3 Mo1 S2 87.8(5) . . ? N1 Mo1 S2 166.9(5) . . ? S3 Mo1 S2 102.2(2) . . ? S1 Mo1 S2 102.8(2) . . ? N5 Mo1 Fe3 138.7(6) . . ? N3 Mo1 Fe3 139.4(5) . . ? N1 Mo1 Fe3 94.5(5) . . ? S3 Mo1 Fe3 52.97(15) . . ? S1 Mo1 Fe3 52.46(15) . . ? S2 Mo1 Fe3 98.64(16) . . ? N5 Mo1 Fe2 100.1(6) . . ? N3 Mo1 Fe2 140.0(5) . . ? N1 Mo1 Fe2 137.1(5) . . ? S3 Mo1 Fe2 52.47(15) . . ? S1 Mo1 Fe2 97.41(16) . . ? S2 Mo1 Fe2 52.39(16) . . ? Fe3 Mo1 Fe2 57.33(10) . . ? N5 Mo1 Fe1 142.0(5) . . ? N3 Mo1 Fe1 98.2(6) . . ? N1 Mo1 Fe1 137.8(5) . . ? S3 Mo1 Fe1 98.48(16) . . ? S1 Mo1 Fe1 52.28(15) . . ? S2 Mo1 Fe1 52.61(16) . . ? Fe3 Mo1 Fe1 57.92(10) . . ? Fe2 Mo1 Fe1 56.94(10) . . ? N9 Mo2 N11 81.9(7) . . ? N9 Mo2 N7 79.9(8) . . ? N11 Mo2 N7 82.1(7) . . ? N9 Mo2 S6 87.5(5) . . ? N11 Mo2 S6 83.2(5) . . ? N7 Mo2 S6 161.8(6) . . ? N9 Mo2 S4 163.6(6) . . ? N11 Mo2 S4 87.8(5) . . ? N7 Mo2 S4 86.1(6) . . ? S6 Mo2 S4 103.9(2) . . ? N9 Mo2 S5 86.2(5) . . ? N11 Mo2 S5 166.6(5) . . ? N7 Mo2 S5 89.8(6) . . ? S6 Mo2 S5 102.5(2) . . ? S4 Mo2 S5 102.4(2) . . ? N9 Mo2 Fe6 140.8(5) . . ? N11 Mo2 Fe6 94.6(5) . . ? N7 Mo2 Fe6 138.5(5) . . ? S6 Mo2 Fe6 53.42(17) . . ? S4 Mo2 Fe6 52.42(15) . . ? S5 Mo2 Fe6 98.56(18) . . ? N9 Mo2 Fe5 98.8(6) . . ? N11 Mo2 Fe5 135.4(4) . . ? N7 Mo2 Fe5 142.3(6) . . ? S6 Mo2 Fe5 52.48(16) . . ? S4 Mo2 Fe5 97.55(17) . . ? S5 Mo2 Fe5 52.67(16) . . ? Fe6 Mo2 Fe5 57.39(10) . . ? N9 Mo2 Fe4 138.4(5) . . ? N11 Mo2 Fe4 139.5(5) . . ? N7 Mo2 Fe4 99.3(6) . . ? S6 Mo2 Fe4 98.84(17) . . ? S4 Mo2 Fe4 52.33(16) . . ? S5 Mo2 Fe4 52.24(17) . . ? Fe6 Mo2 Fe4 57.92(10) . . ? Fe5 Mo2 Fe4 57.09(11) . . ? O3 Fe1 S1 115.4(6) . . ? O3 Fe1 S2 116.5(6) . . ? S1 Fe1 S2 109.5(2) . . ? O3 Fe1 S7 99.8(5) . . ? S1 Fe1 S7 106.1(2) . . ? S2 Fe1 S7 108.4(2) . . ? O3 Fe1 Fe2 139.7(6) . . ? S1 Fe1 Fe2 103.4(2) . . ? S2 Fe1 Fe2 54.87(18) . . ? S7 Fe1 Fe2 57.54(16) . . ? O3 Fe1 Fe3 139.7(5) . . ? S1 Fe1 Fe3 54.11(17) . . ? S2 Fe1 Fe3 102.8(2) . . ? S7 Fe1 Fe3 57.06(15) . . ? Fe2 Fe1 Fe3 59.26(12) . . ? O3 Fe1 Mo1 153.4(5) . . ? S1 Fe1 Mo1 55.92(16) . . ? S2 Fe1 Mo1 56.03(16) . . ? S7 Fe1 Mo1 106.80(17) . . ? Fe2 Fe1 Mo1 60.89(10) . . ? Fe3 Fe1 Mo1 59.69(10) . . ? O2 Fe2 S3 114.7(5) . . ? O2 Fe2 S2 120.5(5) . . ? S3 Fe2 S2 110.0(2) . . ? O2 Fe2 S7 91.0(5) . . ? S3 Fe2 S7 107.7(2) . . ? S2 Fe2 S7 110.7(2) . . ? O2 Fe2 Fe3 132.5(5) . . ? S3 Fe2 Fe3 55.31(17) . . ? S2 Fe2 Fe3 104.8(2) . . ? S7 Fe2 Fe3 58.07(16) . . ? O2 Fe2 Fe1 135.7(5) . . ? S3 Fe2 Fe1 105.8(2) . . ? S2 Fe2 Fe1 55.85(18) . . ? S7 Fe2 Fe1 59.07(16) . . ? Fe3 Fe2 Fe1 60.82(12) . . ? O2 Fe2 Mo1 159.6(5) . . ? S3 Fe2 Mo1 56.29(17) . . ? S2 Fe2 Mo1 56.79(16) . . ? S7 Fe2 Mo1 109.03(18) . . ? Fe3 Fe2 Mo1 60.60(10) . . ? Fe1 Fe2 Mo1 62.17(11) . . ? O2 Fe2 Fe5 44.1(5) . . ? S3 Fe2 Fe5 100.53(19) . . ? S2 Fe2 Fe5 149.3(2) . . ? S7 Fe2 Fe5 54.22(16) . . ? Fe3 Fe2 Fe5 89.39(13) . . ? Fe1 Fe2 Fe5 112.82(14) . . ? Mo1 Fe2 Fe5 148.69(14) . . ? O1 Fe3 S1 118.5(5) . . ? O1 Fe3 S3 113.9(5) . . ? S1 Fe3 S3 112.0(2) . . ? O1 Fe3 S7 93.4(4) . . ? S1 Fe3 S7 108.7(2) . . ? S3 Fe3 S7 108.0(2) . . ? O1 Fe3 Fe2 134.4(4) . . ? S1 Fe3 Fe2 104.93(19) . . ? S3 Fe3 Fe2 55.34(17) . . ? S7 Fe3 Fe2 58.33(16) . . ? O1 Fe3 Fe1 138.0(4) . . ? S1 Fe3 Fe1 55.24(17) . . ? S3 Fe3 Fe1 105.07(19) . . ? S7 Fe3 Fe1 58.82(16) . . ? Fe2 Fe3 Fe1 59.92(12) . . ? O1 Fe3 Mo1 155.9(4) . . ? S1 Fe3 Mo1 57.35(16) . . ? S3 Fe3 Mo1 56.91(16) . . ? S7 Fe3 Mo1 110.46(17) . . ? Fe2 Fe3 Mo1 62.07(10) . . ? Fe1 Fe3 Mo1 62.39(10) . . ? O1 Fe3 Fe6 45.3(4) . . ? S1 Fe3 Fe6 147.3(2) . . ? S3 Fe3 Fe6 100.4(2) . . ? S7 Fe3 Fe6 55.35(15) . . ? Fe2 Fe3 Fe6 90.36(13) . . ? Fe1 Fe3 Fe6 113.80(14) . . ? Mo1 Fe3 Fe6 150.77(15) . . ? O4 Fe4 S5 113.8(5) . . ? O4 Fe4 S4 118.4(5) . . ? S5 Fe4 S4 109.5(3) . . ? O4 Fe4 S7 99.7(5) . . ? S5 Fe4 S7 108.8(2) . . ? S4 Fe4 S7 105.5(2) . . ? O4 Fe4 Fe5 137.3(5) . . ? S5 Fe4 Fe5 55.07(18) . . ? S4 Fe4 Fe5 103.17(19) . . ? S7 Fe4 Fe5 57.65(16) . . ? O4 Fe4 Fe6 142.0(5) . . ? S5 Fe4 Fe6 102.7(2) . . ? S4 Fe4 Fe6 53.92(16) . . ? S7 Fe4 Fe6 56.83(15) . . ? Fe5 Fe4 Fe6 59.01(12) . . ? O4 Fe4 Mo2 153.9(5) . . ? S5 Fe4 Mo2 56.05(17) . . ? S4 Fe4 Mo2 55.97(17) . . ? S7 Fe4 Mo2 106.35(17) . . ? Fe5 Fe4 Mo2 60.53(11) . . ? Fe6 Fe4 Mo2 59.28(10) . . ? O2 Fe5 S6 112.4(5) . . ? O2 Fe5 S5 123.3(5) . . ? S6 Fe5 S5 110.4(3) . . ? O2 Fe5 S7 89.9(5) . . ? S6 Fe5 S7 107.7(2) . . ? S5 Fe5 S7 110.4(2) . . ? O2 Fe5 Fe6 130.1(5) . . ? S6 Fe5 Fe6 55.74(18) . . ? S5 Fe5 Fe6 104.4(2) . . ? S7 Fe5 Fe6 57.89(16) . . ? O2 Fe5 Fe4 136.4(5) . . ? S6 Fe5 Fe4 106.4(2) . . ? S5 Fe5 Fe4 55.41(19) . . ? S7 Fe5 Fe4 59.13(16) . . ? Fe6 Fe5 Fe4 60.77(12) . . ? O2 Fe5 Mo2 160.0(5) . . ? S6 Fe5 Mo2 56.50(16) . . ? S5 Fe5 Mo2 56.91(18) . . ? S7 Fe5 Mo2 108.99(17) . . ? Fe6 Fe5 Mo2 60.45(10) . . ? Fe4 Fe5 Mo2 62.38(11) . . ? O2 Fe5 Fe2 43.2(5) . . ? S6 Fe5 Fe2 98.69(19) . . ? S5 Fe5 Fe2 150.6(2) . . ? S7 Fe5 Fe2 53.87(15) . . ? Fe6 Fe5 Fe2 87.98(13) . . ? Fe4 Fe5 Fe2 112.71(15) . . ? Mo2 Fe5 Fe2 146.87(14) . . ? O1 Fe6 S4 115.8(4) . . ? O1 Fe6 S6 115.3(5) . . ? S4 Fe6 S6 112.7(2) . . ? O1 Fe6 S7 93.6(4) . . ? S4 Fe6 S7 109.2(2) . . ? S6 Fe6 S7 108.2(2) . . ? O1 Fe6 Fe5 136.4(4) . . ? S4 Fe6 Fe5 105.55(19) . . ? S6 Fe6 Fe5 55.28(18) . . ? S7 Fe6 Fe5 58.84(17) . . ? O1 Fe6 Fe4 136.7(4) . . ? S4 Fe6 Fe4 55.58(18) . . ? S6 Fe6 Fe4 105.5(2) . . ? S7 Fe6 Fe4 59.22(16) . . ? Fe5 Fe6 Fe4 60.22(12) . . ? O1 Fe6 Mo2 155.2(4) . . ? S4 Fe6 Mo2 57.89(16) . . ? S6 Fe6 Mo2 57.10(16) . . ? S7 Fe6 Mo2 111.21(18) . . ? Fe5 Fe6 Mo2 62.17(11) . . ? Fe4 Fe6 Mo2 62.80(11) . . ? O1 Fe6 Fe3 45.2(4) . . ? S4 Fe6 Fe3 145.5(2) . . ? S6 Fe6 Fe3 101.74(19) . . ? S7 Fe6 Fe3 55.60(15) . . ? Fe5 Fe6 Fe3 92.25(13) . . ? Fe4 Fe6 Fe3 114.19(14) . . ? Mo2 Fe6 Fe3 152.80(15) . . ? Fe3 S1 Fe1 70.64(19) . . ? Fe3 S1 Mo1 70.19(18) . . ? Fe1 S1 Mo1 71.80(18) . . ? Fe2 S2 Fe1 69.28(19) . . ? Fe2 S2 Mo1 70.82(18) . . ? Fe1 S2 Mo1 71.36(18) . . ? Fe3 S3 Fe2 69.35(19) . . ? Fe3 S3 Mo1 70.12(19) . . ? Fe2 S3 Mo1 71.24(19) . . ? Fe6 S4 Fe4 70.50(19) . . ? Fe6 S4 Mo2 69.69(18) . . ? Fe4 S4 Mo2 71.70(19) . . ? Fe5 S5 Fe4 69.5(2) . . ? Fe5 S5 Mo2 70.42(19) . . ? Fe4 S5 Mo2 71.7(2) . . ? Fe5 S6 Fe6 69.0(2) . . ? Fe5 S6 Mo2 71.02(19) . . ? Fe6 S6 Mo2 69.48(18) . . ? Fe6 S7 Fe3 69.05(17) . . ? Fe6 S7 Fe2 101.8(2) . . ? Fe3 S7 Fe2 63.60(16) . . ? Fe6 S7 Fe5 63.27(17) . . ? Fe3 S7 Fe5 103.4(2) . . ? Fe2 S7 Fe5 71.90(19) . . ? Fe6 S7 Fe1 132.6(2) . . ? Fe3 S7 Fe1 64.12(16) . . ? Fe2 S7 Fe1 63.39(16) . . ? Fe5 S7 Fe1 134.5(2) . . ? Fe6 S7 Fe4 63.95(16) . . ? Fe3 S7 Fe4 132.1(2) . . ? Fe2 S7 Fe4 134.6(3) . . ? Fe5 S7 Fe4 63.22(17) . . ? Fe1 S7 Fe4 157.4(3) . . ? C1 O1 Fe3 125.2(12) . . ? C1 O1 Fe6 124.5(14) . . ? Fe3 O1 Fe6 89.5(6) . . ? C2 O2 Fe2 120.7(16) . . ? C2 O2 Fe5 117.6(15) . . ? Fe2 O2 Fe5 92.7(7) . . ? C3 O3 Fe1 118.7(18) . . ? C4 O4 Fe4 119.3(17) . . ? C8 N1 N2 105.2(17) . . ? C8 N1 Mo1 132.9(14) . . ? N2 N1 Mo1 121.4(15) . . ? C10 N2 N1 109(2) . . ? C10 N2 B1 133(2) . . ? N1 N2 B1 118(2) . . ? C5 N3 N4 107(2) . . ? C5 N3 Mo1 133.8(17) . . ? N4 N3 Mo1 118.8(18) . . ? C7 N4 N3 105(2) . . ? C7 N4 B1 134(3) . . ? N3 N4 B1 121(2) . . ? C11 N5 N6 108(2) . . ? C11 N5 Mo1 132.5(18) . . ? N6 N5 Mo1 119.8(16) . . ? C13 N6 N5 108(2) . . ? C13 N6 B1 132(3) . . ? N5 N6 B1 120(2) . . ? C14 N7 N8 108.1(18) . . ? C14 N7 Mo2 132.4(18) . . ? N8 N7 Mo2 119.5(15) . . ? C16 N8 N7 107(2) . . ? C16 N8 B2 132(2) . . ? N7 N8 B2 120(2) . . ? N10 N9 C17 108(2) . . ? N10 N9 Mo2 122.8(17) . . ? C17 N9 Mo2 129.1(18) . . ? C19 N10 N9 113(2) . . ? C19 N10 B2 127(3) . . ? N9 N10 B2 120(2) . . ? C20 N11 N12 103.0(19) . . ? C20 N11 Mo2 133.0(15) . . ? N12 N11 Mo2 123.1(15) . . ? C22 N12 N11 114.4(19) . . ? C22 N12 B2 128(2) . . ? N11 N12 B2 118(2) . . ? C25 N13 C27 114(3) . . ? C25 N13 C23 108(3) . . ? C27 N13 C23 109(3) . . ? C25 N13 C29 108(2) . . ? C27 N13 C29 108(3) . . ? C23 N13 C29 109(3) . . ? C37 N14 C33 109(2) . . ? C37 N14 C35 113(2) . . ? C33 N14 C35 108(2) . . ? C37 N14 C31 105.7(19) . . ? C33 N14 C31 108.2(19) . . ? C35 N14 C31 112(2) . . ? N4 B1 N6 111(3) . . ? N4 B1 N2 111(3) . . ? N6 B1 N2 110(3) . . ? N10 B2 N8 110(3) . . ? N10 B2 N12 109(2) . . ? N8 B2 N12 107(2) . . ? N3 C5 C6 111(3) . . ? C7 C6 C5 105(3) . . ? C6 C7 N4 111(3) . . ? N1 C8 C9 113(2) . . ? C8 C9 C10 104(2) . . ? N2 C10 C9 108(2) . . ? N5 C11 C12 112(3) . . ? C13 C12 C11 103(3) . . ? N6 C13 C12 110(2) . . ? N7 C14 C15 106(2) . . ? C16 C15 C14 108(2) . . ? C15 C16 N8 110(2) . . ? N9 C17 C18 104(3) . . ? C19 C18 C17 108(3) . . ? N10 C19 C18 107(2) . . ? N11 C20 C21 111(2) . . ? C20 C21 C22 107(2) . . ? N12 C22 C21 104(2) . . ? C24 C23 N13 113(3) . . ? N13 C25 C26 112(3) . . ? N13 C27 C28 112(3) . . ? C30 C29 N13 116(3) . . ? C32 C31 N14 116(2) . . ? N14 C33 C34 117(2) . . ? N14 C35 C36 111(3) . . ? N14 C37 C38 116(2) . . ? N22 C113 C114 114(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.035 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.208 #--------------------------------END data_(Et4N)2[Tp2Mo2Fe6S8Br4](C4H10O) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ' not measured ' _chemical_formula_moiety (Et4N)2[Tp2Mo2Fe6S8Br4](C4H10O) _chemical_formula_sum 'C42 H80 B2 Br4 Fe6 Mo2 N14 O2 S8' _chemical_formula_weight 1937.80 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' _symmetry_cell_setting orthrhombic _symmetry_space_group_name_H-M Pbam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' _cell_length_a 15.359(3) _cell_length_b 19.810(4) _cell_length_c 11.806(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3592.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark green ' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 4.009 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.67 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 25172 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4664 _reflns_number_gt 3338 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0553P)^2^+2.2443P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4664 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 0.81706(3) 0.13908(2) 0.5000 0.02486(13) Uani 1 2 d S . . Fe1 Fe 0.95800(5) 0.05684(4) 0.5000 0.02514(18) Uani 1 2 d S . . Fe2 Fe 0.81056(4) 0.02102(3) 0.38782(5) 0.02875(15) Uani 1 1 d . . . S1 S 0.90382(7) 0.10504(5) 0.34410(9) 0.0290(2) Uani 1 1 d . . . S2 S 0.70231(9) 0.05998(7) 0.5000 0.0328(3) Uani 1 2 d S . . S3 S 1.10356(9) 0.04998(7) 0.5000 0.0280(3) Uani 1 2 d S . . Br1 Br 0.74805(3) -0.03792(3) 0.23342(5) 0.04952(16) Uani 1 1 d . . . O1 O 0.4140(6) 0.2182(4) 0.0000 0.109(3) Uani 1 2 d S . . B1 B 0.7557(5) 0.3010(4) 0.5000 0.0404(18) Uani 1 2 d S . . N1 N 0.8944(3) 0.2346(2) 0.5000 0.0296(11) Uani 1 2 d S . . N2 N 0.8559(3) 0.2957(2) 0.5000 0.0343(12) Uani 1 2 d S . . N3 N 0.7373(2) 0.19804(17) 0.3780(3) 0.0349(8) Uani 1 1 d . . . N4 N 0.7199(2) 0.26494(17) 0.3950(3) 0.0385(9) Uani 1 1 d . . . N5 N 0.5000 0.0000 0.0000 0.067(3) Uani 1 4 d S . . N6 N 1.0000 1.0000 0.0000 0.075(3) Uani 1 4 d S . . C1 C 0.9799(4) 0.2461(3) 0.5000 0.0374(14) Uani 1 2 d S . . C2 C 0.9968(5) 0.3145(3) 0.5000 0.0450(17) Uani 1 2 d S . . C3 C 0.9168(5) 0.3436(3) 0.5000 0.0441(17) Uani 1 2 d S . . C4 C 0.6983(3) 0.1807(3) 0.2817(5) 0.0427(11) Uani 1 1 d . . . C5 C 0.6552(4) 0.2365(3) 0.2371(5) 0.0533(14) Uani 1 1 d . . . C6 C 0.6706(4) 0.2874(3) 0.3099(5) 0.0495(13) Uani 1 1 d . . . C7 C 0.5380(7) -0.0405(7) 0.1012(10) 0.063(3) Uani 0.50 1 d P . . C8 C 0.499(2) -0.0198(8) 0.2165(10) 0.077(6) Uani 0.50 1 d P . . C9 C 0.6061(14) 0.0305(17) 0.0000 0.104(9) Uani 0.50 2 d SP . . C10 C 0.6127(14) 0.0971(9) 0.0000 0.154(7) Uani 1 2 d S . . C11 C 0.9369(9) 1.0364(7) 0.0697(11) 0.075(4) Uani 0.50 1 d P . . C12 C 0.8674(7) 1.0802(7) 0.0000 0.098(4) Uani 1 2 d S . . C13 C 0.9523(9) 0.9496(9) 0.0886(10) 0.085(5) Uani 0.50 1 d P . . C14 C 0.9045(8) 0.8916(7) 0.0000 0.131(5) Uani 1 2 d S . . C15 C 0.4047(6) 0.2166(4) 0.2022(6) 0.088(2) Uani 1 1 d . . . H15A H 0.4382 0.1757 0.2037 0.132 Uiso 1 1 calc R . . H15B H 0.3650 0.2170 0.2649 0.132 Uiso 1 1 calc R . . H15C H 0.4432 0.2547 0.2076 0.132 Uiso 1 1 calc R . . C16 C 0.3582(10) 0.2202(8) 0.1012(9) 0.218(8) Uani 1 1 d . . . H16A H 0.3246 0.2617 0.1003 0.261 Uiso 1 1 calc R . . H16B H 0.3175 0.1828 0.0981 0.261 Uiso 1 1 calc R . . C18 C 0.498(3) 0.0691(15) 0.0000 0.138(13) Uani 0.50 2 d SP . . H1 H 0.703(3) 0.142(3) 0.262(4) 0.036(13) Uiso 1 1 d . . . H2 H 0.626(4) 0.234(3) 0.173(5) 0.053(16) Uiso 1 1 d . . . H3 H 0.652(3) 0.325(2) 0.312(4) 0.030(12) Uiso 1 1 d . . . H4 H 1.027(5) 0.210(3) 0.5000 0.045(19) Uiso 1 2 d S . . H5 H 1.049(5) 0.337(4) 0.5000 0.05(2) Uiso 1 2 d S . . H6 H 0.745(3) 0.354(3) 0.5000 0.022(14) Uiso 1 2 d S . . H7 H 0.894(4) 0.383(4) 0.5000 0.037(18) Uiso 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 0.0218(2) 0.0170(2) 0.0358(3) 0.000 0.000 0.00327(18) Fe1 0.0207(4) 0.0155(3) 0.0393(5) 0.000 0.000 0.0009(3) Fe2 0.0251(3) 0.0215(3) 0.0396(3) -0.0024(2) -0.0030(3) 0.0003(2) S1 0.0300(5) 0.0216(5) 0.0354(5) 0.0003(4) 0.0018(4) 0.0016(4) S2 0.0212(7) 0.0254(7) 0.0517(9) 0.000 0.000 0.0013(5) S3 0.0216(7) 0.0162(6) 0.0463(8) 0.000 0.000 -0.0003(5) Br1 0.0502(3) 0.0450(3) 0.0533(3) -0.0096(2) -0.0168(2) -0.0030(2) O1 0.139(7) 0.106(6) 0.083(5) 0.000 0.000 0.042(5) B1 0.039(4) 0.021(3) 0.061(5) 0.000 0.000 0.004(3) N1 0.029(3) 0.016(2) 0.043(3) 0.000 0.000 0.0047(18) N2 0.040(3) 0.018(2) 0.045(3) 0.000 0.000 0.001(2) N3 0.0297(19) 0.0247(17) 0.050(2) 0.0008(16) -0.0056(17) 0.0049(14) N4 0.0331(19) 0.0237(18) 0.059(2) 0.0051(17) -0.0031(18) 0.0077(15) N5 0.052(6) 0.105(9) 0.045(5) 0.000 0.000 0.042(6) N6 0.052(6) 0.113(9) 0.060(6) 0.000 0.000 -0.002(6) C1 0.033(3) 0.031(3) 0.048(4) 0.000 0.000 -0.005(3) C2 0.035(4) 0.035(4) 0.065(5) 0.000 0.000 -0.010(3) C3 0.054(4) 0.018(3) 0.061(5) 0.000 0.000 -0.006(3) C4 0.043(3) 0.034(3) 0.051(3) 0.003(2) -0.009(2) 0.003(2) C5 0.048(3) 0.054(3) 0.058(3) 0.005(3) -0.016(3) 0.007(3) C6 0.049(3) 0.030(3) 0.069(4) 0.010(3) -0.007(3) 0.011(2) C7 0.034(6) 0.102(10) 0.054(7) 0.011(7) -0.007(5) 0.015(6) C8 0.071(8) 0.113(19) 0.047(6) 0.005(7) -0.011(8) 0.005(17) C9 0.061(13) 0.19(3) 0.059(12) 0.000 0.000 0.054(16) C10 0.194(19) 0.126(14) 0.140(14) 0.000 0.000 -0.031(14) C11 0.076(9) 0.098(11) 0.051(7) -0.026(7) 0.018(6) -0.011(7) C12 0.078(7) 0.124(10) 0.094(8) 0.000 0.000 0.026(7) C13 0.073(9) 0.136(14) 0.046(7) 0.046(8) 0.008(6) -0.005(9) C14 0.079(8) 0.102(10) 0.212(17) 0.000 0.000 -0.017(7) C15 0.122(7) 0.093(5) 0.050(4) -0.011(4) 0.005(4) 0.007(5) C16 0.316(19) 0.263(18) 0.074(7) 0.007(8) 0.049(10) 0.164(15) C18 0.22(4) 0.10(2) 0.10(2) 0.000 0.000 0.09(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N3 2.222(4) 6_556 ? Mo1 N3 2.222(4) . ? Mo1 N1 2.234(5) . ? Mo1 S2 2.3584(15) . ? Mo1 S1 2.3702(11) 6_556 ? Mo1 S1 2.3702(11) . ? Mo1 Fe2 2.6896(8) . ? Mo1 Fe2 2.6896(8) 6_556 ? Mo1 Fe1 2.7093(9) . ? Fe1 S1 2.2342(12) 6_556 ? Fe1 S1 2.2342(12) . ? Fe1 S3 2.2397(16) . ? Fe1 S3 2.3178(15) 5_756 ? Fe1 Fe1 2.5954(15) 5_756 ? Fe1 Fe2 2.7177(9) . ? Fe1 Fe2 2.7176(9) 6_556 ? Fe2 S1 2.2557(12) . ? Fe2 S2 2.2613(13) . ? Fe2 S3 2.3392(12) 5_756 ? Fe2 Br1 2.3681(8) . ? Fe2 Fe2 2.6487(13) 6_556 ? S2 Fe2 2.2613(13) 6_556 ? S3 Fe1 2.3178(15) 5_756 ? S3 Fe2 2.3392(12) 2_755 ? S3 Fe2 2.3392(12) 5_756 ? O1 C16 1.471(12) 6 ? O1 C16 1.471(12) . ? B1 N4 1.533(6) . ? B1 N4 1.533(6) 6_556 ? B1 N2 1.543(9) . ? N1 C1 1.334(8) . ? N1 N2 1.346(6) . ? N2 C3 1.332(8) . ? N3 C4 1.331(6) . ? N3 N4 1.367(5) . ? N4 C6 1.334(6) . ? N5 C18 1.37(3) . ? N5 C18 1.37(3) 5_655 ? N5 C7 1.553(11) 2_655 ? N5 C7 1.553(11) 5_655 ? N5 C7 1.553(11) . ? N5 C7 1.553(11) 6 ? N5 C9 1.74(3) . ? N5 C9 1.74(3) 5_655 ? N6 C11 1.462(13) 6 ? N6 C11 1.462(13) . ? N6 C11 1.462(13) 2_775 ? N6 C11 1.462(13) 5_775 ? N6 C13 1.622(12) 2_775 ? N6 C13 1.622(12) 5_775 ? N6 C13 1.622(12) 6 ? N6 C13 1.622(12) . ? C1 C2 1.380(9) . ? C2 C3 1.357(10) . ? C4 C5 1.392(8) . ? C5 C6 1.345(8) . ? C7 C18 1.44(3) 5_655 ? C7 C8 1.54(2) . ? C7 C8 1.90(2) 2_655 ? C7 C7 1.98(2) 2_655 ? C8 C8 0.79(3) 2_655 ? C8 C7 1.90(2) 2_655 ? C9 C10 1.32(3) . ? C9 C18 1.82(4) . ? C10 C18 1.84(4) . ? C11 C12 1.603(17) . ? C11 C11 1.64(2) 6 ? C11 C13 1.739(18) 2_775 ? C12 C11 1.603(17) 6 ? C13 C14 1.718(18) . ? C13 C11 1.739(18) 2_775 ? C14 C13 1.718(18) 6 ? C15 C16 1.392(14) . ? C18 C7 1.44(3) 5_655 ? C18 C7 1.44(3) 2_655 ? 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 N3 Mo1 N3 80.8(2) 6_556 . ? N3 Mo1 N1 81.24(13) 6_556 . ? N3 Mo1 N1 81.24(13) . . ? N3 Mo1 S2 86.41(10) 6_556 . ? N3 Mo1 S2 86.41(10) . . ? N1 Mo1 S2 163.75(12) . . ? N3 Mo1 S1 87.50(10) 6_556 6_556 ? N3 Mo1 S1 164.28(10) . 6_556 ? N1 Mo1 S1 86.69(8) . 6_556 ? S2 Mo1 S1 103.36(4) . 6_556 ? N3 Mo1 S1 164.28(10) 6_556 . ? N3 Mo1 S1 87.50(10) . . ? N1 Mo1 S1 86.69(8) . . ? S2 Mo1 S1 103.36(4) . . ? S1 Mo1 S1 101.89(5) 6_556 . ? N3 Mo1 Fe2 139.08(9) 6_556 . ? N3 Mo1 Fe2 96.75(10) . . ? N1 Mo1 Fe2 139.14(8) . . ? S2 Mo1 Fe2 52.73(3) . . ? S1 Mo1 Fe2 98.96(3) 6_556 . ? S1 Mo1 Fe2 52.49(3) . . ? N3 Mo1 Fe2 96.75(10) 6_556 6_556 ? N3 Mo1 Fe2 139.08(9) . 6_556 ? N1 Mo1 Fe2 139.14(8) . 6_556 ? S2 Mo1 Fe2 52.73(3) . 6_556 ? S1 Mo1 Fe2 52.49(3) 6_556 6_556 ? S1 Mo1 Fe2 98.96(3) . 6_556 ? Fe2 Mo1 Fe2 59.00(3) . 6_556 ? N3 Mo1 Fe1 139.16(10) 6_556 . ? N3 Mo1 Fe1 139.16(10) . . ? N1 Mo1 Fe1 94.86(12) . . ? S2 Mo1 Fe1 101.39(4) . . ? S1 Mo1 Fe1 51.66(3) 6_556 . ? S1 Mo1 Fe1 51.66(3) . . ? Fe2 Mo1 Fe1 60.45(2) . . ? Fe2 Mo1 Fe1 60.45(2) 6_556 . ? S1 Fe1 S1 110.93(6) 6_556 . ? S1 Fe1 S3 113.44(4) 6_556 . ? S1 Fe1 S3 113.44(4) . . ? S1 Fe1 S3 103.78(4) 6_556 5_756 ? S1 Fe1 S3 103.78(4) . 5_756 ? S3 Fe1 S3 110.60(5) . 5_756 ? S1 Fe1 Fe1 123.78(3) 6_556 5_756 ? S1 Fe1 Fe1 123.78(3) . 5_756 ? S3 Fe1 Fe1 56.72(4) . 5_756 ? S3 Fe1 Fe1 53.88(4) 5_756 5_756 ? S1 Fe1 Mo1 56.32(3) 6_556 . ? S1 Fe1 Mo1 56.32(3) . . ? S3 Fe1 Mo1 146.52(5) . . ? S3 Fe1 Mo1 102.89(5) 5_756 . ? Fe1 Fe1 Mo1 156.77(5) 5_756 . ? S1 Fe1 Fe2 101.69(4) 6_556 . ? S1 Fe1 Fe2 53.11(3) . . ? S3 Fe1 Fe2 144.67(3) . . ? S3 Fe1 Fe2 54.67(3) 5_756 . ? Fe1 Fe1 Fe2 100.81(4) 5_756 . ? Mo1 Fe1 Fe2 59.42(2) . . ? S1 Fe1 Fe2 53.11(3) 6_556 6_556 ? S1 Fe1 Fe2 101.69(4) . 6_556 ? S3 Fe1 Fe2 144.67(3) . 6_556 ? S3 Fe1 Fe2 54.66(3) 5_756 6_556 ? Fe1 Fe1 Fe2 100.81(4) 5_756 6_556 ? Mo1 Fe1 Fe2 59.42(2) . 6_556 ? Fe2 Fe1 Fe2 58.33(3) . 6_556 ? S1 Fe2 S2 110.43(5) . . ? S1 Fe2 S3 102.43(5) . 5_756 ? S2 Fe2 S3 106.75(4) . 5_756 ? S1 Fe2 Br1 116.43(4) . . ? S2 Fe2 Br1 108.72(4) . . ? S3 Fe2 Br1 111.59(4) 5_756 . ? S1 Fe2 Fe2 103.23(3) . 6_556 ? S2 Fe2 Fe2 54.15(3) . 6_556 ? S3 Fe2 Fe2 55.52(2) 5_756 6_556 ? Br1 Fe2 Fe2 140.33(2) . 6_556 ? S1 Fe2 Mo1 56.46(3) . . ? S2 Fe2 Mo1 56.09(4) . . ? S3 Fe2 Mo1 102.90(4) 5_756 . ? Br1 Fe2 Mo1 145.37(3) . . ? Fe2 Fe2 Mo1 60.502(15) 6_556 . ? S1 Fe2 Fe1 52.39(3) . . ? S2 Fe2 Fe1 103.78(4) . . ? S3 Fe2 Fe1 53.93(4) 5_756 . ? Br1 Fe2 Fe1 147.32(3) . . ? Fe2 Fe2 Fe1 60.836(17) 6_556 . ? Mo1 Fe2 Fe1 60.14(2) . . ? Fe1 S1 Fe2 74.50(4) . . ? Fe1 S1 Mo1 72.02(4) . . ? Fe2 S1 Mo1 71.05(4) . . ? Fe2 S2 Fe2 71.70(5) . 6_556 ? Fe2 S2 Mo1 71.18(4) . . ? Fe2 S2 Mo1 71.18(4) 6_556 . ? Fe1 S3 Fe1 69.40(5) . 5_756 ? Fe1 S3 Fe2 126.82(5) . 2_755 ? Fe1 S3 Fe2 71.40(4) 5_756 2_755 ? Fe1 S3 Fe2 126.82(5) . 5_756 ? Fe1 S3 Fe2 71.40(4) 5_756 5_756 ? Fe2 S3 Fe2 68.96(5) 2_755 5_756 ? C16 O1 C16 108.5(13) 6 . ? N4 B1 N4 108.0(5) . 6_556 ? N4 B1 N2 109.1(4) . . ? N4 B1 N2 109.1(4) 6_556 . ? C1 N1 N2 106.2(5) . . ? C1 N1 Mo1 131.9(4) . . ? N2 N1 Mo1 121.9(4) . . ? C3 N2 N1 109.4(5) . . ? C3 N2 B1 130.7(5) . . ? N1 N2 B1 119.9(5) . . ? C4 N3 N4 106.7(4) . . ? C4 N3 Mo1 131.8(3) . . ? N4 N3 Mo1 121.5(3) . . ? C6 N4 N3 108.9(4) . . ? C6 N4 B1 131.1(4) . . ? N3 N4 B1 120.0(4) . . ? C18 N5 C18 180(3) . 5_655 ? C18 N5 C7 58.4(8) . 2_655 ? C18 N5 C7 121.6(8) 5_655 2_655 ? C18 N5 C7 58.4(8) . 5_655 ? C18 N5 C7 121.6(8) 5_655 5_655 ? C7 N5 C7 100.6(9) 2_655 5_655 ? C18 N5 C7 121.6(8) . . ? C18 N5 C7 58.4(8) 5_655 . ? C7 N5 C7 79.4(9) 2_655 . ? C7 N5 C7 180.0(11) 5_655 . ? C18 N5 C7 121.6(8) . 6 ? C18 N5 C7 58.4(8) 5_655 6 ? C7 N5 C7 180.0(11) 2_655 6 ? C7 N5 C7 79.4(9) 5_655 6 ? C7 N5 C7 100.6(9) . 6 ? C18 N5 C9 70.7(18) . . ? C18 N5 C9 109.3(18) 5_655 . ? C7 N5 C9 99.9(7) 2_655 . ? C7 N5 C9 99.9(7) 5_655 . ? C7 N5 C9 80.1(7) . . ? C7 N5 C9 80.1(7) 6 . ? C18 N5 C9 109.3(18) . 5_655 ? C18 N5 C9 70.7(18) 5_655 5_655 ? C7 N5 C9 80.1(7) 2_655 5_655 ? C7 N5 C9 80.1(7) 5_655 5_655 ? C7 N5 C9 99.9(7) . 5_655 ? C7 N5 C9 99.9(7) 6 5_655 ? C9 N5 C9 180(2) . 5_655 ? C11 N6 C11 68.5(12) 6 . ? C11 N6 C11 180.0(10) 6 2_775 ? C11 N6 C11 111.5(12) . 2_775 ? C11 N6 C11 111.5(12) 6 5_775 ? C11 N6 C11 180.0(10) . 5_775 ? C11 N6 C11 68.5(12) 2_775 5_775 ? C11 N6 C13 111.0(8) 6 2_775 ? C11 N6 C13 68.4(7) . 2_775 ? C11 N6 C13 69.0(8) 2_775 2_775 ? C11 N6 C13 111.6(7) 5_775 2_775 ? C11 N6 C13 68.4(7) 6 5_775 ? C11 N6 C13 111.0(8) . 5_775 ? C11 N6 C13 111.6(7) 2_775 5_775 ? C11 N6 C13 69.0(8) 5_775 5_775 ? C13 N6 C13 80.4(11) 2_775 5_775 ? C11 N6 C13 69.0(8) 6 6 ? C11 N6 C13 111.6(7) . 6 ? C11 N6 C13 111.0(8) 2_775 6 ? C11 N6 C13 68.4(7) 5_775 6 ? C13 N6 C13 180.000(3) 2_775 6 ? C13 N6 C13 99.6(11) 5_775 6 ? C11 N6 C13 111.6(7) 6 . ? C11 N6 C13 69.0(8) . . ? C11 N6 C13 68.4(7) 2_775 . ? C11 N6 C13 111.0(8) 5_775 . ? C13 N6 C13 99.6(11) 2_775 . ? C13 N6 C13 180.000(3) 5_775 . ? C13 N6 C13 80.4(11) 6 . ? N1 C1 C2 110.6(6) . . ? C3 C2 C1 104.3(6) . . ? N2 C3 C2 109.5(6) . . ? N3 C4 C5 109.4(5) . . ? C6 C5 C4 105.6(5) . . ? N4 C6 C5 109.3(4) . . ? C18 C7 C8 133.3(19) 5_655 . ? C18 C7 N5 54.4(11) 5_655 . ? C8 C7 N5 113.2(11) . . ? C18 C7 C8 137.0(16) 5_655 2_655 ? C8 C7 C8 23.7(10) . 2_655 ? N5 C7 C8 96.6(9) . 2_655 ? C18 C7 C7 95.2(11) 5_655 2_655 ? C8 C7 C7 63.6(8) . 2_655 ? N5 C7 C7 50.3(5) . 2_655 ? C8 C7 C7 46.8(7) 2_655 2_655 ? C8 C8 C7 104(2) 2_655 . ? C8 C8 C7 52.2(18) 2_655 2_655 ? C7 C8 C7 69.5(9) . 2_655 ? C10 C9 N5 114.8(17) . . ? C10 C9 C18 69.6(17) . . ? N5 C9 C18 45.2(13) . . ? C9 C10 C18 68.1(14) . . ? N6 C11 C12 114.9(8) . . ? N6 C11 C11 55.8(6) . 6 ? C12 C11 C11 59.1(5) . 6 ? N6 C11 C13 60.1(7) . 2_775 ? C12 C11 C13 129.2(12) . 2_775 ? C11 C11 C13 97.4(6) 6 2_775 ? C11 C12 C11 61.7(9) . 6 ? N6 C13 C14 102.2(8) . . ? N6 C13 C11 51.4(6) . 2_775 ? C14 C13 C11 116.5(12) . 2_775 ? C13 C14 C13 75.0(9) 6 . ? C15 C16 O1 113.2(11) . . ? N5 C18 C7 67.2(14) . 5_655 ? N5 C18 C7 67.2(14) . 2_655 ? C7 C18 C7 113(3) 5_655 2_655 ? N5 C18 C9 64.2(15) . . ? C7 C18 C9 100.8(13) 5_655 . ? C7 C18 C9 100.8(13) 2_655 . ? N5 C18 C10 106.5(18) . . ? C7 C18 C10 119.3(15) 5_655 . ? C7 C18 C10 119.3(15) 2_655 . ? C9 C18 C10 42.3(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.800 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.143 #--------------------------------END data_(Et4N)2[Tp2Mo2Fe6S8Cl4]4MeCN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ' not measured ' _chemical_formula_moiety (Et4N)2[Tp2Mo2Fe6S8Cl4]4MeCN _chemical_formula_sum 'C42 H72 B2 Cl4 Fe6 Mo2 N18 S8' _chemical_formula_weight 1776.06 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' 'B' 'B' 0.0013 0.0007 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 orthrhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 15.070(3) _cell_length_b 19.824(4) _cell_length_c 23.695(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7079(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ' black ' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 1.966 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17606 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.99 _reflns_number_total 2871 _reflns_number_gt 2473 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0615P)^2^+26.1334P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2871 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.002 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 0.18395(4) 0.14066(3) 0.0000 0.0266(2) Uani 1 2 d S . . Fe1 Fe 0.04170(7) 0.05749(5) 0.0000 0.0326(3) Uani 1 2 d S . . Fe2 Fe 0.19217(5) 0.02261(4) 0.05634(3) 0.0336(2) Uani 1 1 d . . . S1 S 0.09617(9) 0.10617(6) 0.07762(6) 0.0362(3) Uani 1 1 d . . . S2 S 0.30124(12) 0.06221(9) 0.0000 0.0321(4) Uani 1 2 d S . . S3 S -0.10557(12) 0.04855(9) 0.0000 0.0368(5) Uani 1 2 d S . . Cl1 Cl 0.25147(12) -0.03355(8) 0.12838(7) 0.0586(5) Uani 1 1 d . . . N1 N 0.1037(4) 0.2352(3) 0.0000 0.0339(15) Uani 1 2 d S . . N2 N 0.1419(4) 0.2968(3) 0.0000 0.0382(16) Uani 1 2 d S . . N3 N 0.2641(3) 0.2005(2) 0.06103(19) 0.0346(10) Uani 1 1 d . . . N4 N 0.2803(3) 0.2678(2) 0.0522(2) 0.0395(11) Uani 1 1 d . . . N5 N 0.0000 1.0000 0.2500 0.060(3) Uani 1 4 d S . . N6 N 0.5000 0.0000 0.2500 0.099(5) Uani 1 4 d S . . N7 N 0.3944(12) 0.7863(11) 0.1412(7) 0.096(7) Uani 0.50 1 d P . . N8 N 0.325(2) 0.8320(19) 0.2459(10) 0.095(13) Uani 0.25 1 d P . . B1 B 0.2446(6) 0.3028(4) 0.0000 0.041(2) Uani 1 2 d S . . C1 C 0.0160(5) 0.2462(4) 0.0000 0.047(2) Uani 1 2 d S . . C2 C -0.0019(7) 0.3139(4) 0.0000 0.059(3) Uani 1 2 d S . . C3 C 0.0802(7) 0.3451(5) 0.0000 0.057(3) Uani 1 2 d S . . C4 C 0.3026(4) 0.1852(4) 0.1094(3) 0.0451(17) Uani 1 1 d . . . C5 C 0.3427(5) 0.2403(4) 0.1326(3) 0.0548(17) Uani 1 1 d . . . C6 C 0.3275(4) 0.2910(4) 0.0964(3) 0.0517(17) Uani 1 1 d . . . C7 C 0.0554(8) 0.9560(6) 0.2104(5) 0.080(4) Uani 0.70 1 d P . . C8 C 0.0606(19) 1.0423(16) 0.2093(11) 0.083(9) Uani 0.30 1 d P . . C9 C 0.1167(7) 0.9052(6) 0.2472(6) 0.125(4) Uani 1 1 d . . . C10 C 0.524(3) 0.0420(19) 0.186(2) 0.111(16) Uani 0.25 1 d P . . C101 C 0.4609(18) 0.0564(19) 0.221(2) 0.117(19) Uani 0.25 1 d P . . C11 C 0.5000 0.0000 0.1386(11) 0.084(7) Uani 0.50 2 d SP . . C12 C 0.4055(14) 0.0000 0.2500 0.091(8) Uani 0.50 2 d SP . . C13 C 0.3624(12) -0.0735(9) 0.2611(8) 0.085(5) Uani 0.50 1 d P . . C14 C 0.4247(12) 0.7717(8) 0.1826(14) 0.173(12) Uani 0.75 1 d P . . C15 C 0.4584(14) 0.7558(11) 0.2355(7) 0.092(7) Uani 0.50 1 d P . . C16 C 0.3531(15) 0.8081(12) 0.2104(14) 0.130(11) Uani 0.50 1 d P . . H1 H 0.107(6) 0.385(5) 0.0000 0.05(3) Uiso 1 2 d S . . H3 H 0.263(5) 0.349(4) 0.0000 0.04(2) Uiso 1 2 d S . . H4 H 0.341(4) 0.331(3) 0.094(2) 0.031(15) Uiso 1 1 d . . . H6 H 0.301(3) 0.155(3) 0.120(2) 0.011(15) Uiso 1 1 d . . . H7 H -0.033(6) 0.209(4) 0.0000 0.05(2) Uiso 1 2 d S . . H8 H 0.359(4) 0.241(3) 0.168(3) 0.045(18) Uiso 1 1 d . . . H9 H -0.056(7) 0.324(5) 0.0000 0.07(3) Uiso 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 0.0201(3) 0.0184(3) 0.0412(4) 0.000 0.000 -0.0032(2) Fe1 0.0197(6) 0.0177(5) 0.0602(8) 0.000 0.000 -0.0021(4) Fe2 0.0264(4) 0.0251(4) 0.0492(5) 0.0053(3) 0.0006(3) -0.0012(3) S1 0.0310(7) 0.0268(7) 0.0507(9) 0.0004(6) 0.0083(6) -0.0026(5) S2 0.0209(9) 0.0252(9) 0.0501(12) 0.000 0.000 -0.0013(7) S3 0.0202(9) 0.0183(9) 0.0719(14) 0.000 0.000 -0.0005(7) Cl1 0.0619(11) 0.0535(9) 0.0603(10) 0.0187(8) -0.0104(8) 0.0006(8) N1 0.027(3) 0.018(3) 0.057(4) 0.000 0.000 -0.003(3) N2 0.035(4) 0.016(3) 0.064(5) 0.000 0.000 0.002(3) N3 0.029(2) 0.027(2) 0.047(3) -0.003(2) -0.003(2) -0.0047(19) N4 0.031(3) 0.028(2) 0.060(3) -0.006(2) -0.003(2) -0.009(2) N5 0.043(6) 0.088(8) 0.050(7) 0.000 0.000 0.000 N6 0.064(9) 0.089(10) 0.142(15) 0.000 0.000 0.000 N7 0.084(11) 0.140(16) 0.064(10) -0.033(9) -0.054(9) 0.027(10) N8 0.11(2) 0.14(3) 0.026(12) -0.005(15) 0.029(13) 0.09(2) B1 0.036(5) 0.016(4) 0.069(7) 0.000 0.000 -0.010(4) C1 0.027(5) 0.037(5) 0.078(6) 0.000 0.000 0.004(4) C2 0.035(5) 0.036(5) 0.105(8) 0.000 0.000 0.012(4) C3 0.048(6) 0.030(5) 0.092(8) 0.000 0.000 0.003(4) C4 0.045(4) 0.034(4) 0.056(5) 0.006(3) -0.008(3) -0.007(3) C5 0.056(4) 0.059(4) 0.050(4) -0.008(4) -0.018(3) -0.004(3) C6 0.044(4) 0.042(4) 0.069(5) -0.017(4) -0.008(3) -0.012(3) C7 0.070(8) 0.099(9) 0.072(8) -0.001(7) 0.029(6) 0.014(7) C8 0.077(19) 0.12(2) 0.052(15) 0.048(16) 0.018(13) 0.008(17) C9 0.096(8) 0.126(9) 0.154(11) 0.037(8) 0.022(7) 0.051(7) C10 0.10(3) 0.08(2) 0.16(4) 0.06(3) 0.07(3) 0.01(2) C101 0.023(14) 0.12(3) 0.21(4) 0.13(3) 0.00(2) 0.012(16) C11 0.053(13) 0.13(2) 0.070(16) 0.000 0.000 -0.029(15) C12 0.035(11) 0.14(2) 0.099(19) -0.004(18) 0.000 0.000 C13 0.078(12) 0.086(11) 0.091(13) -0.002(10) 0.007(10) -0.007(9) C14 0.104(14) 0.065(9) 0.35(4) -0.051(17) 0.135(19) -0.025(10) C15 0.103(15) 0.132(17) 0.041(9) 0.041(10) -0.003(8) 0.010(11) C16 0.072(15) 0.107(17) 0.21(3) 0.09(2) -0.052(18) -0.012(13) _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 N3 2.227(4) . ? Mo1 N3 2.227(4) 10 ? Mo1 N1 2.231(6) . ? Mo1 S2 2.3544(19) . ? Mo1 S1 2.3665(14) 10 ? Mo1 S1 2.3665(14) . ? Mo1 Fe2 2.6972(9) . ? Mo1 Fe2 2.6972(9) 10 ? Mo1 Fe1 2.7045(11) . ? Fe1 S3 2.226(2) . ? Fe1 S1 2.2334(16) . ? Fe1 S1 2.2334(16) 10 ? Fe1 S3 2.312(2) 9 ? Fe1 Fe1 2.6029(19) 9 ? Fe1 Fe2 2.7208(12) . ? Fe1 Fe2 2.7208(12) 10 ? Fe2 Cl1 2.2251(17) . ? Fe2 S1 2.2563(15) . ? Fe2 S2 2.2584(16) . ? Fe2 S3 2.3400(16) 9 ? Fe2 Fe2 2.6702(17) 10 ? S2 Fe2 2.2584(16) 10 ? S3 Fe1 2.312(2) 9 ? S3 Fe2 2.3400(16) 9 ? S3 Fe2 2.3400(16) 2 ? N1 C1 1.340(10) . ? N1 N2 1.349(8) . ? N2 C3 1.335(11) . ? N2 B1 1.552(12) . ? N3 C4 1.319(8) . ? N3 N4 1.372(6) . ? N4 C6 1.349(8) . ? N4 B1 1.516(7) . ? N5 C7 1.529(11) 8_465 ? N5 C7 1.529(11) 2_575 ? N5 C7 1.529(11) . ? N5 C7 1.529(11) 7_445 ? N5 C8 1.57(2) 7_445 ? N5 C8 1.57(2) . ? N5 C8 1.57(2) 2_575 ? N5 C8 1.57(2) 8_465 ? N6 C12 1.42(2) 2_655 ? N6 C12 1.42(2) . ? N6 C101 1.43(2) 7_545 ? N6 C101 1.43(2) . ? N6 C101 1.43(2) 2_655 ? N6 C101 1.43(2) 8_445 ? N6 C10 1.77(4) 7_545 ? N6 C10 1.77(4) 2_655 ? N6 C10 1.77(4) . ? N6 C10 1.77(4) 8_445 ? N7 C14 1.12(3) . ? N7 C16 1.80(4) . ? N8 C16 1.06(4) . ? B1 N4 1.516(7) 10 ? C1 C2 1.369(12) . ? C2 C3 1.383(14) . ? C4 C5 1.364(10) . ? C5 C6 1.341(10) . ? C7 C9 1.621(16) . ? C7 C8 1.71(3) . ? C7 C8 1.75(3) 2_575 ? C7 C8 1.90(3) 8_465 ? C8 C9 1.69(3) 8_465 ? C8 C7 1.75(3) 2_575 ? C8 C7 1.90(3) 8_465 ? C9 C8 1.69(3) 8_465 ? C10 C101 1.30(5) . ? C10 C11 1.44(5) . ? C10 C10 1.81(8) 2_655 ? C10 C12 2.03(5) 2_655 ? C101 C12 1.55(3) . ? C101 C13 1.58(4) 8_445 ? C101 C101 1.80(8) 7_545 ? C11 C10 1.44(5) 2_655 ? C12 C101 1.55(3) 8_445 ? C12 C13 1.617(19) 8_445 ? C12 C13 1.617(19) . ? C12 C10 2.03(5) 7_545 ? C12 C10 2.03(5) 2_655 ? C13 C101 1.58(4) 8_445 ? C14 C15 1.39(3) . ? C14 C16 1.45(3) . ? C15 C15 1.43(4) 7_545 ? C15 C16 1.99(3) . ? 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 N3 Mo1 N3 81.0(2) . 10 ? N3 Mo1 N1 81.15(16) . . ? N3 Mo1 N1 81.15(16) 10 . ? N3 Mo1 S2 86.84(12) . . ? N3 Mo1 S2 86.84(12) 10 . ? N1 Mo1 S2 164.17(16) . . ? N3 Mo1 S1 164.15(12) . 10 ? N3 Mo1 S1 87.27(12) 10 10 ? N1 Mo1 S1 86.55(10) . 10 ? S2 Mo1 S1 103.22(5) . 10 ? N3 Mo1 S1 87.27(12) . . ? N3 Mo1 S1 164.15(12) 10 . ? N1 Mo1 S1 86.55(10) . . ? S2 Mo1 S1 103.22(5) . . ? S1 Mo1 S1 102.01(7) 10 . ? N3 Mo1 Fe2 96.66(12) . . ? N3 Mo1 Fe2 139.37(12) 10 . ? N1 Mo1 Fe2 138.94(10) . . ? S2 Mo1 Fe2 52.58(4) . . ? S1 Mo1 Fe2 99.19(4) 10 . ? S1 Mo1 Fe2 52.43(4) . . ? N3 Mo1 Fe2 139.37(12) . 10 ? N3 Mo1 Fe2 96.66(12) 10 10 ? N1 Mo1 Fe2 138.94(10) . 10 ? S2 Mo1 Fe2 52.58(4) . 10 ? S1 Mo1 Fe2 52.43(4) 10 10 ? S1 Mo1 Fe2 99.19(4) . 10 ? Fe2 Mo1 Fe2 59.34(4) . 10 ? N3 Mo1 Fe1 139.01(12) . . ? N3 Mo1 Fe1 139.01(12) 10 . ? N1 Mo1 Fe1 94.74(15) . . ? S2 Mo1 Fe1 101.09(5) . . ? S1 Mo1 Fe1 51.74(4) 10 . ? S1 Mo1 Fe1 51.74(4) . . ? Fe2 Mo1 Fe1 60.49(3) . . ? Fe2 Mo1 Fe1 60.49(3) 10 . ? S3 Fe1 S1 113.63(5) . . ? S3 Fe1 S1 113.63(5) . 10 ? S1 Fe1 S1 110.88(8) . 10 ? S3 Fe1 S3 110.04(6) . 9 ? S1 Fe1 S3 103.88(5) . 9 ? S1 Fe1 S3 103.88(5) 10 9 ? S3 Fe1 Fe1 56.56(6) . 9 ? S1 Fe1 Fe1 123.77(4) . 9 ? S1 Fe1 Fe1 123.77(4) 10 9 ? S3 Fe1 Fe1 53.48(6) 9 9 ? S3 Fe1 Mo1 147.00(6) . . ? S1 Fe1 Mo1 56.30(4) . . ? S1 Fe1 Mo1 56.30(4) 10 . ? S3 Fe1 Mo1 102.97(6) 9 . ? Fe1 Fe1 Mo1 156.44(6) 9 . ? S3 Fe1 Fe2 144.15(4) . . ? S1 Fe1 Fe2 53.08(4) . . ? S1 Fe1 Fe2 101.98(5) 10 . ? S3 Fe1 Fe2 54.69(4) 9 . ? Fe1 Fe1 Fe2 100.37(5) 9 . ? Mo1 Fe1 Fe2 59.62(3) . . ? S3 Fe1 Fe2 144.15(4) . 10 ? S1 Fe1 Fe2 101.98(5) . 10 ? S1 Fe1 Fe2 53.08(4) 10 10 ? S3 Fe1 Fe2 54.69(4) 9 10 ? Fe1 Fe1 Fe2 100.37(5) 9 10 ? Mo1 Fe1 Fe2 59.62(3) . 10 ? Fe2 Fe1 Fe2 58.77(4) . 10 ? Cl1 Fe2 S1 116.96(7) . . ? Cl1 Fe2 S2 109.58(7) . . ? S1 Fe2 S2 110.09(6) . . ? Cl1 Fe2 S3 111.10(6) . 9 ? S1 Fe2 S3 102.26(6) . 9 ? S2 Fe2 S3 106.15(5) . 9 ? Cl1 Fe2 Fe2 140.09(5) . 10 ? S1 Fe2 Fe2 102.91(4) . 10 ? S2 Fe2 Fe2 53.76(3) . 10 ? S3 Fe2 Fe2 55.21(3) 9 10 ? Cl1 Fe2 Mo1 146.33(6) . . ? S1 Fe2 Mo1 56.23(4) . . ? S2 Fe2 Mo1 55.89(5) . . ? S3 Fe2 Mo1 102.42(5) 9 . ? Fe2 Fe2 Mo1 60.332(19) 10 . ? Cl1 Fe2 Fe1 146.96(6) . . ? S1 Fe2 Fe1 52.32(4) . . ? S2 Fe2 Fe1 103.19(5) . . ? S3 Fe2 Fe1 53.73(5) 9 . ? Fe2 Fe2 Fe1 60.61(2) 10 . ? Mo1 Fe2 Fe1 59.89(3) . . ? Fe1 S1 Fe2 74.60(5) . . ? Fe1 S1 Mo1 71.96(5) . . ? Fe2 S1 Mo1 71.34(5) . . ? Fe2 S2 Fe2 72.48(7) 10 . ? Fe2 S2 Mo1 71.53(5) 10 . ? Fe2 S2 Mo1 71.53(5) . . ? Fe1 S3 Fe1 69.96(6) . 9 ? Fe1 S3 Fe2 127.15(6) . 9 ? Fe1 S3 Fe2 71.58(5) 9 9 ? Fe1 S3 Fe2 127.15(6) . 2 ? Fe1 S3 Fe2 71.58(5) 9 2 ? Fe2 S3 Fe2 69.58(6) 9 2 ? C1 N1 N2 105.9(6) . . ? C1 N1 Mo1 132.2(5) . . ? N2 N1 Mo1 121.9(5) . . ? C3 N2 N1 110.5(7) . . ? C3 N2 B1 129.8(7) . . ? N1 N2 B1 119.7(6) . . ? C4 N3 N4 106.2(5) . . ? C4 N3 Mo1 132.8(4) . . ? N4 N3 Mo1 121.0(3) . . ? C6 N4 N3 107.9(5) . . ? C6 N4 B1 131.6(5) . . ? N3 N4 B1 120.5(5) . . ? C7 N5 C7 110.4(9) 8_465 2_575 ? C7 N5 C7 113.8(10) 8_465 . ? C7 N5 C7 104.3(10) 2_575 . ? C7 N5 C7 104.3(10) 8_465 7_445 ? C7 N5 C7 113.8(10) 2_575 7_445 ? C7 N5 C7 110.4(9) . 7_445 ? C7 N5 C8 68.7(10) 8_465 7_445 ? C7 N5 C8 75.8(12) 2_575 7_445 ? C7 N5 C8 177.1(13) . 7_445 ? C7 N5 C8 67.1(12) 7_445 7_445 ? C7 N5 C8 75.8(12) 8_465 . ? C7 N5 C8 68.7(10) 2_575 . ? C7 N5 C8 67.1(12) . . ? C7 N5 C8 177.1(13) 7_445 . ? C8 N5 C8 115(2) 7_445 . ? C7 N5 C8 177.1(13) 8_465 2_575 ? C7 N5 C8 67.1(12) 2_575 2_575 ? C7 N5 C8 68.7(10) . 2_575 ? C7 N5 C8 75.8(12) 7_445 2_575 ? C8 N5 C8 109(2) 7_445 2_575 ? C8 N5 C8 104(2) . 2_575 ? C7 N5 C8 67.1(12) 8_465 8_465 ? C7 N5 C8 177.1(13) 2_575 8_465 ? C7 N5 C8 75.8(12) . 8_465 ? C7 N5 C8 68.7(10) 7_445 8_465 ? C8 N5 C8 104(2) 7_445 8_465 ? C8 N5 C8 109(2) . 8_465 ? C8 N5 C8 115(2) 2_575 8_465 ? C12 N6 C12 180.000(1) 2_655 . ? C12 N6 C101 65.7(11) 2_655 7_545 ? C12 N6 C101 114.3(11) . 7_545 ? C12 N6 C101 114.3(11) 2_655 . ? C12 N6 C101 65.7(11) . . ? C101 N6 C101 78(4) 7_545 . ? C12 N6 C101 65.7(11) 2_655 2_655 ? C12 N6 C101 114.3(11) . 2_655 ? C101 N6 C101 131(2) 7_545 2_655 ? C101 N6 C101 124(4) . 2_655 ? C12 N6 C101 114.3(11) 2_655 8_445 ? C12 N6 C101 65.7(11) . 8_445 ? C101 N6 C101 124(4) 7_545 8_445 ? C101 N6 C101 131(2) . 8_445 ? C101 N6 C101 78(4) 2_655 8_445 ? C12 N6 C10 101.8(15) 2_655 7_545 ? C12 N6 C10 78.2(15) . 7_545 ? C101 N6 C10 47(2) 7_545 7_545 ? C101 N6 C10 87(3) . 7_545 ? C101 N6 C10 149(3) 2_655 7_545 ? C101 N6 C10 83(2) 8_445 7_545 ? C12 N6 C10 101.8(15) 2_655 2_655 ? C12 N6 C10 78.2(15) . 2_655 ? C101 N6 C10 149(3) 7_545 2_655 ? C101 N6 C10 83(2) . 2_655 ? C101 N6 C10 47(2) 2_655 2_655 ? C101 N6 C10 87(3) 8_445 2_655 ? C10 N6 C10 156(3) 7_545 2_655 ? C12 N6 C10 78.2(15) 2_655 . ? C12 N6 C10 101.8(15) . . ? C101 N6 C10 87(3) 7_545 . ? C101 N6 C10 47(2) . . ? C101 N6 C10 83(2) 2_655 . ? C101 N6 C10 149(3) 8_445 . ? C10 N6 C10 124(3) 7_545 . ? C10 N6 C10 62(3) 2_655 . ? C12 N6 C10 78.2(15) 2_655 8_445 ? C12 N6 C10 101.8(15) . 8_445 ? C101 N6 C10 83(2) 7_545 8_445 ? C101 N6 C10 149(3) . 8_445 ? C101 N6 C10 87(3) 2_655 8_445 ? C101 N6 C10 47(2) 8_445 8_445 ? C10 N6 C10 62(3) 7_545 8_445 ? C10 N6 C10 124(3) 2_655 8_445 ? C10 N6 C10 156(3) . 8_445 ? C14 N7 C16 53.6(13) . . ? N4 B1 N4 109.2(7) . 10 ? N4 B1 N2 108.5(4) . . ? N4 B1 N2 108.5(4) 10 . ? N1 C1 C2 110.7(8) . . ? C1 C2 C3 105.2(8) . . ? N2 C3 C2 107.6(8) . . ? N3 C4 C5 111.1(7) . . ? C6 C5 C4 105.5(6) . . ? C5 C6 N4 109.3(6) . . ? N5 C7 C9 109.6(9) . . ? N5 C7 C8 57.6(9) . . ? C9 C7 C8 127.1(14) . . ? N5 C7 C8 56.8(8) . 2_575 ? C9 C7 C8 126.2(15) . 2_575 ? C8 C7 C8 91.5(17) . 2_575 ? N5 C7 C8 53.1(10) . 8_465 ? C9 C7 C8 56.7(11) . 8_465 ? C8 C7 C8 89.7(13) . 8_465 ? C8 C7 C8 93.2(12) 2_575 8_465 ? N5 C8 C9 104.2(15) . 8_465 ? N5 C8 C7 55.3(10) . . ? C9 C8 C7 128.9(17) 8_465 . ? N5 C8 C7 54.5(10) . 2_575 ? C9 C8 C7 118.6(19) 8_465 2_575 ? C7 C8 C7 88.5(16) . 2_575 ? N5 C8 C7 51.1(8) . 8_465 ? C9 C8 C7 53.2(10) 8_465 8_465 ? C7 C8 C7 90.0(12) . 8_465 ? C7 C8 C7 86.8(12) 2_575 8_465 ? C7 C9 C8 70.1(9) . 8_465 ? C101 C10 C11 116(4) . . ? C101 C10 N6 53.1(17) . . ? C11 C10 N6 110(2) . . ? C101 C10 C10 85(3) . 2_655 ? C11 C10 C10 51.1(14) . 2_655 ? N6 C10 C10 59.1(16) . 2_655 ? C101 C10 C12 89(3) . 2_655 ? C11 C10 C12 118(2) . 2_655 ? N6 C10 C12 43.4(11) . 2_655 ? C10 C10 C12 80.4(18) 2_655 2_655 ? C10 C101 N6 80(2) . . ? C10 C101 C12 121(4) . . ? N6 C101 C12 56.8(12) . . ? C10 C101 C13 155(4) . 8_445 ? N6 C101 C13 115(2) . 8_445 ? C12 C101 C13 62.2(14) . 8_445 ? C10 C101 C101 90(3) . 7_545 ? N6 C101 C101 51.2(19) . 7_545 ? C12 C101 C101 91(3) . 7_545 ? C13 C101 C101 115(4) 8_445 7_545 ? C10 C11 C10 78(3) . 2_655 ? N6 C12 C101 57.4(11) . . ? N6 C12 C101 57.4(11) . 8_445 ? C101 C12 C101 115(2) . 8_445 ? N6 C12 C13 113.7(10) . 8_445 ? C101 C12 C13 59.7(13) . 8_445 ? C101 C12 C13 159(2) 8_445 8_445 ? N6 C12 C13 113.7(10) . . ? C101 C12 C13 159(2) . . ? C101 C12 C13 59.7(13) 8_445 . ? C13 C12 C13 132.7(19) 8_445 . ? N6 C12 C10 58.5(11) . 7_545 ? C101 C12 C10 76(2) . 7_545 ? C101 C12 C10 72(2) 8_445 7_545 ? C13 C12 C10 87.8(14) 8_445 7_545 ? C13 C12 C10 117.3(15) . 7_545 ? N6 C12 C10 58.5(11) . 2_655 ? C101 C12 C10 72(2) . 2_655 ? C101 C12 C10 76(2) 8_445 2_655 ? C13 C12 C10 117.3(15) 8_445 2_655 ? C13 C12 C10 87.8(14) . 2_655 ? C10 C12 C10 117(2) 7_545 2_655 ? C101 C13 C12 58.1(13) 8_445 . ? N7 C14 C15 177(2) . . ? N7 C14 C16 88(2) . . ? C15 C14 C16 89(2) . . ? C14 C15 C15 139(2) . 7_545 ? C14 C15 C16 47.1(13) . . ? C15 C15 C16 147.6(11) 7_545 . ? N8 C16 C14 152(3) . . ? N8 C16 N7 166(3) . . ? C14 C16 N7 38.3(17) . . ? N8 C16 C15 108(3) . . ? C14 C16 C15 44.3(15) . . ? N7 C16 C15 82.6(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.979 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.123 #===END