data_publication_text _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'R. H. Holm' _publ_contact_author_address ;Harvard University Department of Chemistry and Chemical Biology 12 Oxford St. Cambridge, MA 02138 ; _publ_contact_author_email holm@chemistry.harvard.edu _publ_contact_author_phone 617-496-3215 _publ_contact_author_fax 617-496-9289 loop_ _publ_author_name _publ_author_address 'Holm, R. H.' ;Harvard University Department of Chemistry and Chemical Biology 12 Oxford St. Cambridge, MA 02138 ; data_ts2018fm _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'tetrakis(Tetrabutylammonium) bis(\m4-sulfido)-hexakis(\m3-sulfido)-tetracyano-bis(hydrogen tris(pyrazolyl)borato-N,N',N")-hexa-iron-di-vanadium acetonitrile solvate' ; _chemical_name_common 'Cyano vanadium edge-bridged-double-cubane' _chemical_melting_point 'not measured' _chemical_formula_moiety '(Bu4N)4((C9H10N6B)2V2Fe6S8(CN)4)(CH3CN)6' _chemical_formula_sum 'C98 H182 B2 Fe6 N26 S8 V2' _chemical_formula_weight 2438.79 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' 'V' 'V' 0.3005 0.5294 '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' _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 18.617(3) _cell_length_b 16.165(3) _cell_length_c 23.299(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.141(2) _cell_angle_gamma 90.00 _cell_volume 6583(2) _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 'primatic plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _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_% ? _diffrn_reflns_number 35065 _diffrn_reflns_av_R_equivalents 0.1926 _diffrn_reflns_av_sigmaI/netI 0.1941 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.02 _reflns_number_total 11575 _reflns_number_gt 5356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0747P)^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 11575 _refine_ls_number_parameters 655 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1945 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2168 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 1.991 _refine_ls_shift/su_mean 0.058 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 C23 C 0.9728(13) 0.4118(15) 1.1055(11) 0.252(14) Uani 1 1 d . . . H23A H 0.9842 0.4571 1.0820 0.378 Uiso 1 1 calc R . . H23B H 1.0166 0.4032 1.1431 0.378 Uiso 1 1 calc R . . H23C H 0.9276 0.4260 1.1159 0.378 Uiso 1 1 calc R . . Fe2 Fe 0.88113(7) 1.03581(8) 0.07047(6) 0.0407(3) Uani 1 1 d . . . Fe3 Fe 0.93901(6) 0.95580(7) -0.00570(6) 0.0372(3) Uani 1 1 d . . . Fe1 Fe 0.96446(7) 0.90634(8) 0.11034(6) 0.0389(3) Uani 1 1 d . . . V1 V 0.82186(8) 0.88594(8) 0.02664(6) 0.0348(4) Uani 1 1 d . . . S1 S 0.93725(12) 0.82491(14) 0.02695(11) 0.0410(6) Uani 1 1 d . . . S2 S 0.82017(12) 1.00766(14) -0.02902(10) 0.0404(6) Uani 1 1 d . . . S3 S 0.85337(12) 0.93364(14) 0.12649(10) 0.0401(6) Uani 1 1 d . . . S4 S 1.01169(12) 1.02945(14) 0.08214(10) 0.0429(6) Uani 1 1 d . . . N4 N 0.7032(4) 0.9113(5) 0.0182(3) 0.0429(19) Uani 1 1 d . . . N8 N 0.7928(4) 0.7669(4) 0.0584(3) 0.0396(18) Uani 1 1 d . . . N6 N 0.7635(4) 0.8278(4) -0.0624(3) 0.0420(18) Uani 1 1 d . . . N9 N 0.8204(4) 0.2675(5) 0.9074(4) 0.050(2) Uani 1 1 d . . . N5 N 0.6985(4) 0.7822(5) -0.0745(4) 0.053(2) Uani 1 1 d . . . N7 N 0.7253(4) 0.7275(5) 0.0306(4) 0.052(2) Uani 1 1 d . . . N3 N 0.6463(4) 0.8546(5) -0.0025(4) 0.051(2) Uani 1 1 d . . . N10 N 0.9143(5) 0.0849(6) 0.2870(4) 0.070(3) Uani 1 1 d . . . C32 C 0.8363(5) 0.0778(6) 0.2385(5) 0.058(3) Uani 1 1 d . . . H32A H 0.8364 0.0281 0.2137 0.070 Uiso 1 1 calc R . . H32B H 0.8289 0.1263 0.2112 0.070 Uiso 1 1 calc R . . C10 C 0.7933(6) 0.6466(7) 0.1049(5) 0.067(3) Uani 1 1 d . . . H10 H 0.8095 0.6019 0.1330 0.080 Uiso 1 1 calc R . . C4 C 0.5963(6) 0.9599(8) 0.0266(5) 0.069(3) Uani 1 1 d . . . H4 H 0.5613 0.9959 0.0357 0.083 Uiso 1 1 calc R . . C26 C 0.9170(6) 0.3983(6) 0.8143(6) 0.071(3) Uani 1 1 d . . . H26A H 0.8743 0.3902 0.7752 0.085 Uiso 1 1 calc R . . H26B H 0.9103 0.4531 0.8307 0.085 Uiso 1 1 calc R . . C1 C 1.0352(5) 0.8670(6) 0.1950(4) 0.043(2) Uani 1 1 d . . . C8 C 0.7803(5) 0.8289(5) -0.1138(4) 0.046(2) Uani 1 1 d . . . H8 H 0.8231 0.8565 -0.1182 0.055 Uiso 1 1 calc R . . C12 C 0.8230(5) 0.1829(6) 0.8804(4) 0.051(3) Uani 1 1 d . . . H12A H 0.8766 0.1717 0.8840 0.061 Uiso 1 1 calc R . . H12B H 0.8088 0.1416 0.9060 0.061 Uiso 1 1 calc R . . C13 C 0.7735(6) 0.1685(6) 0.8152(5) 0.064(3) Uani 1 1 d . . . H13A H 0.7922 0.2027 0.7880 0.076 Uiso 1 1 calc R . . H13B H 0.7204 0.1857 0.8093 0.076 Uiso 1 1 calc R . . C36 C 0.9186(7) 0.1606(7) 0.3258(5) 0.077(4) Uani 1 1 d . . . H36A H 0.8786 0.1560 0.3447 0.092 Uiso 1 1 calc R . . H36B H 0.9688 0.1604 0.3594 0.092 Uiso 1 1 calc R . . C9 C 0.7253(6) 0.6541(7) 0.0572(5) 0.063(3) Uani 1 1 d . . . H9 H 0.6853 0.6144 0.0452 0.076 Uiso 1 1 calc R . . C16 C 0.7416(5) 0.2855(6) 0.9106(5) 0.059(3) Uani 1 1 d . . . H16A H 0.7038 0.2827 0.8686 0.071 Uiso 1 1 calc R . . H16B H 0.7416 0.3430 0.9252 0.071 Uiso 1 1 calc R . . C25 C 0.9126(5) 0.3317(6) 0.8593(5) 0.058(3) Uani 1 1 d . . . H25A H 0.9203 0.2766 0.8439 0.069 Uiso 1 1 calc R . . H25B H 0.9537 0.3407 0.8992 0.069 Uiso 1 1 calc R . . N1 N 1.0690(5) 0.8461(6) 0.2412(4) 0.072(3) Uani 1 1 d . . . C11 C 0.8330(5) 0.7175(6) 0.1033(5) 0.052(3) Uani 1 1 d . . . H11 H 0.8829 0.7297 0.1308 0.063 Uiso 1 1 calc R . . C33 C 0.7678(6) 0.0720(8) 0.2590(5) 0.073(3) Uani 1 1 d . . . H33A H 0.7642 0.1226 0.2817 0.088 Uiso 1 1 calc R . . H33B H 0.7735 0.0239 0.2865 0.088 Uiso 1 1 calc R . . C5 C 0.6724(5) 0.9756(6) 0.0360(4) 0.052(3) Uani 1 1 d . . . H5 H 0.6986 1.0253 0.0527 0.062 Uiso 1 1 calc R . . C6 C 0.6758(6) 0.7568(6) -0.1334(5) 0.065(3) Uani 1 1 d . . . H6 H 0.6314 0.7249 -0.1534 0.078 Uiso 1 1 calc R . . C20 C 0.8813(6) 0.2653(6) 0.9712(5) 0.063(3) Uani 1 1 d . . . H20A H 0.8687 0.2195 0.9944 0.076 Uiso 1 1 calc R . . H20B H 0.9310 0.2520 0.9668 0.076 Uiso 1 1 calc R . . C40 C 0.9703(6) 0.0901(8) 0.2522(5) 0.071(3) Uani 1 1 d . . . H40A H 0.9572 0.1392 0.2252 0.085 Uiso 1 1 calc R . . H40B H 0.9631 0.0406 0.2257 0.085 Uiso 1 1 calc R . . C28 C 0.9314(7) 0.0104(8) 0.3290(5) 0.082(4) Uani 1 1 d . . . H28A H 0.8984 0.0135 0.3544 0.099 Uiso 1 1 calc R . . H28B H 0.9851 0.0148 0.3570 0.099 Uiso 1 1 calc R . . C17 C 0.7146(6) 0.2285(7) 0.9513(5) 0.070(3) Uani 1 1 d . . . H17A H 0.7121 0.1708 0.9365 0.083 Uiso 1 1 calc R . . H17B H 0.7512 0.2306 0.9937 0.083 Uiso 1 1 calc R . . C3 C 0.5814(5) 0.8838(8) 0.0022(5) 0.063(3) Uani 1 1 d . . . H3 H 0.5336 0.8560 -0.0095 0.076 Uiso 1 1 calc R . . C7 C 0.7272(6) 0.7846(7) -0.1597(5) 0.063(3) Uani 1 1 d . . . H7 H 0.7263 0.7753 -0.2002 0.075 Uiso 1 1 calc R . . C37 C 0.9093(7) 0.2434(8) 0.2936(6) 0.089(4) Uani 1 1 d . . . H37A H 0.8666 0.2400 0.2541 0.106 Uiso 1 1 calc R . . H37B H 0.9566 0.2564 0.2850 0.106 Uiso 1 1 calc R . . C24 C 0.8363(5) 0.3343(6) 0.8676(5) 0.061(3) Uani 1 1 d . . . H24A H 0.7961 0.3312 0.8267 0.073 Uiso 1 1 calc R . . H24B H 0.8312 0.3887 0.8854 0.073 Uiso 1 1 calc R . . C29 C 0.9209(7) -0.0742(7) 0.2994(6) 0.085(4) Uani 1 1 d . . . H29A H 0.9459 -0.0754 0.2682 0.102 Uiso 1 1 calc R . . H29B H 0.8657 -0.0852 0.2787 0.102 Uiso 1 1 calc R . . C41 C 1.0550(6) 0.0956(10) 0.2925(6) 0.109(5) Uani 1 1 d . . . H41A H 1.0628 0.1412 0.3224 0.131 Uiso 1 1 calc R . . H41B H 1.0716 0.0433 0.3153 0.131 Uiso 1 1 calc R . . B1 B 0.6644(7) 0.7705(8) -0.0238(6) 0.061(4) Uani 1 1 d . . . C14 C 0.7740(6) 0.0785(6) 0.7979(5) 0.062(3) Uani 1 1 d . . . H14A H 0.8276 0.0588 0.8102 0.074 Uiso 1 1 calc R . . H14B H 0.7476 0.0453 0.8203 0.074 Uiso 1 1 calc R . . N2 N 0.8328(6) 1.2041(7) 0.1153(5) 0.092(3) Uani 1 1 d . . . C2 C 0.8515(6) 1.1469(6) 0.0999(4) 0.054(3) Uani 1 1 d . . . C34 C 0.6957(6) 0.0624(8) 0.2033(6) 0.086(4) Uani 1 1 d . . . H34A H 0.6912 0.1105 0.1760 0.103 Uiso 1 1 calc R . . H34B H 0.7007 0.0122 0.1806 0.103 Uiso 1 1 calc R . . C38 C 0.8932(8) 0.3130(7) 0.3324(6) 0.088(4) Uani 1 1 d . . . H38A H 0.9287 0.3070 0.3750 0.105 Uiso 1 1 calc R . . H38B H 0.9045 0.3667 0.3168 0.105 Uiso 1 1 calc R . . C27 C 0.9914(6) 0.3975(7) 0.8022(6) 0.083(4) Uani 1 1 d . . . H27A H 1.0341 0.4026 0.8410 0.125 Uiso 1 1 calc R . . H27B H 0.9924 0.4441 0.7756 0.125 Uiso 1 1 calc R . . H27C H 0.9960 0.3455 0.7822 0.125 Uiso 1 1 calc R . . C39 C 0.8125(7) 0.3150(8) 0.3326(6) 0.094(4) Uani 1 1 d . . . H39A H 0.7770 0.3246 0.2909 0.141 Uiso 1 1 calc R . . H39B H 0.8074 0.3597 0.3593 0.141 Uiso 1 1 calc R . . H39C H 0.8005 0.2620 0.3476 0.141 Uiso 1 1 calc R . . C42 C 1.1023(7) 0.1116(12) 0.2504(8) 0.122(7) Uani 1 1 d . . . H42A H 1.1572 0.1076 0.2754 0.146 Uiso 1 1 calc R . . H42B H 1.0909 0.0670 0.2194 0.146 Uiso 1 1 calc R . . C30 C 0.9550(8) -0.1403(8) 0.3465(6) 0.105(5) Uani 1 1 d . . . H30A H 0.9341 -0.1347 0.3800 0.126 Uiso 1 1 calc R . . H30B H 1.0111 -0.1321 0.3641 0.126 Uiso 1 1 calc R . . C15 C 0.7351(7) 0.0653(8) 0.7299(6) 0.102(5) Uani 1 1 d . . . H15A H 0.6813 0.0820 0.7179 0.153 Uiso 1 1 calc R . . H15B H 0.7380 0.0066 0.7202 0.153 Uiso 1 1 calc R . . H15C H 0.7607 0.0986 0.7075 0.153 Uiso 1 1 calc R . . C21 C 0.8910(7) 0.3435(9) 1.0089(6) 0.099(5) Uani 1 1 d . . . H21A H 0.8437 0.3547 1.0180 0.119 Uiso 1 1 calc R . . H21B H 0.9004 0.3910 0.9856 0.119 Uiso 1 1 calc R . . C18 C 0.6363(7) 0.2561(8) 0.9497(7) 0.098(5) Uani 1 1 d . . . H18A H 0.6386 0.3151 0.9615 0.118 Uiso 1 1 calc R . . H18B H 0.5996 0.2509 0.9074 0.118 Uiso 1 1 calc R . . C35 C 0.6247(8) 0.0558(9) 0.2185(8) 0.119(5) Uani 1 1 d . . . H35A H 0.6308 0.0120 0.2489 0.179 Uiso 1 1 calc R . . H35B H 0.5815 0.0425 0.1815 0.179 Uiso 1 1 calc R . . H35C H 0.6150 0.1086 0.2352 0.179 Uiso 1 1 calc R . . C2S C 0.8396(9) 0.6202(9) 0.9562(7) 0.119(5) Uani 1 1 d . . . H2S1 H 0.8352 0.6526 0.9195 0.178 Uiso 1 1 calc R . . H2S2 H 0.8899 0.5934 0.9713 0.178 Uiso 1 1 calc R . . H2S3 H 0.8340 0.6569 0.9878 0.178 Uiso 1 1 calc R . . C31 C 0.9386(9) -0.2280(9) 0.3198(7) 0.122(6) Uani 1 1 d . . . H31A H 0.8832 -0.2355 0.3003 0.183 Uiso 1 1 calc R . . H31B H 0.9584 -0.2686 0.3527 0.183 Uiso 1 1 calc R . . H31C H 0.9635 -0.2359 0.2895 0.183 Uiso 1 1 calc R . . C1S C 0.7781(14) 0.5555(13) 0.9406(9) 0.137(7) Uani 1 1 d . . . C43 C 1.0894(10) 0.1897(12) 0.2192(9) 0.143(8) Uani 1 1 d . . . H43A H 1.0404 0.1882 0.1853 0.215 Uiso 1 1 calc R . . H43B H 1.1307 0.2005 0.2031 0.215 Uiso 1 1 calc R . . H43C H 1.0883 0.2338 0.2478 0.215 Uiso 1 1 calc R . . C22 C 0.9574(8) 0.3328(10) 1.0674(7) 0.119(6) Uani 1 1 d . . . H22A H 1.0036 0.3178 1.0579 0.142 Uiso 1 1 calc R . . H22B H 0.9463 0.2871 1.0914 0.142 Uiso 1 1 calc R . . N1S N 0.7295(15) 0.5037(12) 0.9285(11) 0.224(11) Uani 1 1 d . . . C19 C 0.6077(8) 0.2068(10) 0.9915(9) 0.140(7) Uani 1 1 d . . . H19A H 0.6013 0.1489 0.9781 0.210 Uiso 1 1 calc R . . H19B H 0.5583 0.2289 0.9906 0.210 Uiso 1 1 calc R . . H19C H 0.6446 0.2100 1.0332 0.210 Uiso 1 1 calc R . . C3S C 0.5928(7) 0.0530(10) 0.8373(7) 0.088(4) Uani 1 1 d . . . N2S N 0.5755(8) 0.1148(9) 0.8161(8) 0.147(6) Uani 1 1 d . . . C4S C 0.6149(6) -0.0252(7) 0.8666(6) 0.084(4) Uani 1 1 d . . . H4S1 H 0.6208 -0.0654 0.8371 0.125 Uiso 1 1 calc R . . H4S2 H 0.5753 -0.0446 0.8824 0.125 Uiso 1 1 calc R . . H4S3 H 0.6635 -0.0194 0.9005 0.125 Uiso 1 1 calc R . . H1A H 0.624(4) 0.734(4) -0.037(3) 0.018(18) Uiso 1 1 d . . . N3S N 0.852(3) 0.9620(14) 0.4360(16) 0.63(5) Uani 1 1 d D . . C5S C 0.796(2) 0.920(3) 0.423(2) 0.37(3) Uani 1 1 d D . . C6S C 0.734(3) 0.886(3) 0.363(2) 0.48(5) Uani 1 1 d D . . H6S1 H 0.6916 0.8622 0.3733 0.715 Uiso 1 1 calc R . . H6S2 H 0.7571 0.8437 0.3450 0.715 Uiso 1 1 calc R . . H6S3 H 0.7154 0.9318 0.3343 0.715 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C23 0.20(2) 0.28(3) 0.22(3) -0.17(2) 0.01(2) -0.06(2) Fe2 0.0405(7) 0.0430(8) 0.0330(7) -0.0043(6) 0.0054(6) -0.0021(6) Fe3 0.0332(7) 0.0427(8) 0.0282(7) -0.0031(6) 0.0011(5) -0.0046(5) Fe1 0.0322(7) 0.0483(8) 0.0275(7) -0.0007(6) -0.0008(5) 0.0008(6) V1 0.0299(8) 0.0411(9) 0.0246(8) 0.0007(6) -0.0020(6) -0.0015(6) S1 0.0369(12) 0.0438(13) 0.0341(13) -0.0027(10) 0.0015(10) 0.0013(10) S2 0.0358(12) 0.0444(13) 0.0319(13) 0.0032(10) 0.0001(10) -0.0017(10) S3 0.0344(12) 0.0488(14) 0.0313(13) 0.0000(10) 0.0039(10) 0.0005(10) S4 0.0362(12) 0.0534(14) 0.0307(13) -0.0067(11) 0.0008(10) -0.0112(10) N4 0.029(4) 0.055(5) 0.036(5) 0.005(4) 0.000(3) 0.002(4) N8 0.035(4) 0.037(4) 0.041(5) 0.010(3) 0.006(4) -0.001(3) N6 0.046(5) 0.050(5) 0.022(4) -0.006(3) 0.002(3) -0.008(4) N9 0.038(4) 0.046(5) 0.058(6) 0.010(4) 0.005(4) 0.004(3) N5 0.046(5) 0.053(5) 0.048(6) -0.009(4) 0.003(4) -0.021(4) N7 0.051(5) 0.056(5) 0.045(5) 0.004(4) 0.011(4) -0.011(4) N3 0.035(5) 0.065(6) 0.044(5) 0.004(4) 0.000(4) -0.007(4) N10 0.071(6) 0.078(7) 0.048(6) -0.016(5) 0.005(5) 0.006(5) C32 0.054(6) 0.065(7) 0.051(7) -0.016(5) 0.012(5) -0.001(5) C10 0.075(8) 0.062(7) 0.060(8) 0.011(6) 0.018(6) -0.001(6) C4 0.040(6) 0.103(10) 0.065(8) 0.009(7) 0.019(5) 0.022(6) C26 0.060(7) 0.058(7) 0.092(10) 0.023(6) 0.025(7) 0.005(5) C1 0.035(5) 0.057(6) 0.026(5) 0.005(4) -0.002(4) -0.002(4) C8 0.042(5) 0.054(6) 0.035(6) -0.003(5) 0.005(4) -0.007(4) C12 0.047(6) 0.047(6) 0.053(7) 0.014(5) 0.010(5) -0.003(4) C13 0.062(7) 0.056(7) 0.066(8) 0.010(6) 0.013(6) -0.008(5) C36 0.074(8) 0.082(9) 0.064(8) -0.027(7) 0.011(6) -0.003(6) C9 0.072(8) 0.058(7) 0.058(8) -0.006(6) 0.020(6) -0.023(6) C16 0.039(6) 0.055(6) 0.082(9) 0.002(6) 0.018(6) 0.006(5) C25 0.053(6) 0.042(6) 0.074(8) 0.012(5) 0.018(6) 0.002(5) N1 0.056(6) 0.096(7) 0.055(7) 0.017(5) 0.008(5) 0.013(5) C11 0.048(6) 0.050(6) 0.052(7) 0.006(5) 0.009(5) 0.005(5) C33 0.066(8) 0.090(9) 0.070(9) -0.012(7) 0.031(7) 0.003(6) C5 0.034(5) 0.066(7) 0.050(7) 0.011(5) 0.008(5) 0.007(5) C6 0.056(7) 0.075(8) 0.041(7) -0.019(6) -0.012(5) -0.012(6) C20 0.055(7) 0.066(7) 0.060(8) -0.001(6) 0.009(6) 0.006(5) C40 0.052(6) 0.111(10) 0.050(7) -0.036(7) 0.020(6) -0.002(6) C28 0.093(9) 0.092(9) 0.058(8) -0.005(7) 0.021(7) 0.028(7) C17 0.052(7) 0.078(8) 0.074(9) 0.021(6) 0.016(6) 0.010(6) C3 0.031(6) 0.094(9) 0.056(7) 0.006(6) 0.005(5) -0.001(6) C7 0.055(7) 0.086(8) 0.040(7) -0.020(6) 0.009(5) -0.006(6) C37 0.087(9) 0.089(10) 0.110(12) -0.037(9) 0.059(9) -0.021(7) C24 0.050(6) 0.037(6) 0.089(9) 0.008(5) 0.017(6) 0.004(5) C29 0.103(10) 0.076(8) 0.070(9) -0.019(7) 0.023(8) 0.022(7) C41 0.050(7) 0.170(15) 0.097(11) -0.060(10) 0.012(8) -0.012(8) B1 0.050(8) 0.064(9) 0.057(9) 0.002(7) 0.004(7) -0.030(7) C14 0.055(6) 0.070(7) 0.059(8) -0.005(6) 0.017(6) -0.013(5) N2 0.124(9) 0.076(7) 0.077(8) 0.001(6) 0.035(7) 0.016(7) C2 0.072(7) 0.045(6) 0.035(6) -0.005(5) 0.007(5) 0.005(5) C34 0.055(7) 0.107(10) 0.103(11) -0.027(8) 0.036(8) -0.009(7) C38 0.108(11) 0.074(9) 0.085(10) -0.028(7) 0.039(8) -0.001(7) C27 0.079(9) 0.084(9) 0.095(10) 0.030(7) 0.040(8) 0.009(7) C39 0.107(11) 0.085(10) 0.108(12) -0.018(8) 0.060(9) 0.004(8) C42 0.046(8) 0.168(16) 0.147(17) -0.108(14) 0.028(9) -0.027(10) C30 0.128(12) 0.082(10) 0.089(11) -0.002(8) 0.015(9) 0.033(8) C15 0.097(10) 0.091(10) 0.099(12) -0.009(8) 0.011(9) -0.033(8) C21 0.071(8) 0.116(11) 0.095(11) -0.036(9) 0.009(8) 0.000(8) C18 0.061(8) 0.098(10) 0.149(14) 0.040(9) 0.054(9) 0.019(7) C35 0.083(10) 0.117(12) 0.149(16) -0.018(10) 0.029(10) -0.007(9) C2S 0.140(14) 0.095(12) 0.128(15) -0.006(10) 0.055(12) -0.013(10) C31 0.144(14) 0.088(11) 0.129(15) -0.007(10) 0.040(11) 0.009(9) C1S 0.21(2) 0.108(15) 0.105(15) 0.027(12) 0.065(15) 0.052(14) C43 0.135(15) 0.163(17) 0.165(19) -0.104(16) 0.095(14) -0.082(14) C22 0.088(10) 0.167(15) 0.085(12) -0.030(11) 0.010(9) -0.043(10) N1S 0.33(3) 0.121(15) 0.26(3) -0.039(15) 0.14(2) -0.075(16) C19 0.076(10) 0.169(16) 0.20(2) 0.066(14) 0.077(12) 0.015(10) C3S 0.069(8) 0.104(12) 0.082(10) 0.010(9) 0.015(7) 0.007(8) N2S 0.116(11) 0.133(13) 0.179(16) 0.063(12) 0.035(10) 0.028(9) C4S 0.062(7) 0.096(10) 0.076(9) 0.019(8) 0.003(6) -0.003(7) N3S 1.41(12) 0.14(2) 0.84(8) 0.25(3) 1.02(9) 0.33(4) C5S 0.52(7) 0.17(3) 0.65(9) 0.17(5) 0.50(7) 0.11(4) C6S 0.81(13) 0.23(6) 0.60(9) 0.21(6) 0.50(9) 0.11(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 C23 C22 1.52(2) . ? Fe2 C2 2.063(11) . ? Fe2 S2 2.249(3) . ? Fe2 S3 2.272(3) . ? Fe2 S4 2.353(3) . ? Fe2 Fe1 2.5802(18) . ? Fe2 Fe3 2.7018(19) . ? Fe2 V1 2.7117(19) . ? Fe3 S1 2.252(3) . ? Fe3 S2 2.251(3) . ? Fe3 S4 2.280(3) 3_775 ? Fe3 S4 2.352(2) . ? Fe3 Fe3 2.618(2) 3_775 ? Fe3 Fe1 2.7002(19) . ? Fe3 V1 2.7805(19) . ? Fe1 C1 2.059(9) . ? Fe1 S1 2.255(3) . ? Fe1 S3 2.269(3) . ? Fe1 S4 2.359(3) . ? Fe1 V1 2.7192(17) . ? V1 N4 2.187(7) . ? V1 N8 2.194(7) . ? V1 N6 2.195(7) . ? V1 S3 2.326(3) . ? V1 S2 2.351(3) . ? V1 S1 2.362(3) . ? S4 Fe3 2.280(3) 3_775 ? N4 C5 1.323(11) . ? N4 N3 1.358(10) . ? N8 C11 1.324(11) . ? N8 N7 1.358(9) . ? N6 C8 1.337(11) . ? N6 N5 1.361(9) . ? N9 C12 1.512(11) . ? N9 C16 1.521(11) . ? N9 C24 1.518(12) . ? N9 C20 1.529(12) . ? N5 C6 1.352(12) . ? N5 B1 1.534(15) . ? N7 C9 1.337(12) . ? N7 B1 1.544(14) . ? N3 C3 1.335(12) . ? N3 B1 1.525(15) . ? N10 C32 1.506(12) . ? N10 C28 1.515(14) . ? N10 C36 1.507(13) . ? N10 C40 1.527(13) . ? C32 C33 1.510(13) . ? C10 C9 1.374(14) . ? C10 C11 1.372(13) . ? C4 C3 1.343(14) . ? C4 C5 1.380(13) . ? C26 C27 1.506(13) . ? C26 C25 1.524(13) . ? C1 N1 1.098(11) . ? C8 C7 1.380(12) . ? C12 C13 1.501(13) . ? C13 C14 1.511(13) . ? C36 C37 1.514(16) . ? C16 C17 1.526(14) . ? C25 C24 1.498(13) . ? C33 C34 1.519(15) . ? C6 C7 1.376(14) . ? C20 C21 1.514(15) . ? C40 C41 1.536(14) . ? C28 C29 1.513(15) . ? C17 C18 1.514(14) . ? C37 C38 1.536(15) . ? C29 C30 1.506(16) . ? C41 C42 1.55(2) . ? C14 C15 1.513(15) . ? N2 C2 1.092(12) . ? C34 C35 1.486(16) . ? C38 C39 1.505(15) . ? C42 C43 1.44(2) . ? C30 C31 1.535(17) . ? C21 C22 1.503(17) . ? C18 C19 1.490(17) . ? C2S C1S 1.50(3) . ? C1S N1S 1.19(3) . ? C3S N2S 1.111(16) . ? C3S C4S 1.429(17) . ? N3S C5S 1.20(2) . ? C5S C6S 1.57(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe2 S2 114.9(3) . . ? C2 Fe2 S3 107.6(3) . . ? S2 Fe2 S3 108.13(9) . . ? C2 Fe2 S4 112.5(3) . . ? S2 Fe2 S4 104.17(10) . . ? S3 Fe2 S4 109.39(9) . . ? C2 Fe2 Fe1 141.5(3) . . ? S2 Fe2 Fe1 103.56(8) . . ? S3 Fe2 Fe1 55.33(7) . . ? S4 Fe2 Fe1 56.90(7) . . ? C2 Fe2 Fe3 147.9(3) . . ? S2 Fe2 Fe3 53.13(7) . . ? S3 Fe2 Fe3 104.50(8) . . ? S4 Fe2 Fe3 54.92(6) . . ? Fe1 Fe2 Fe3 61.44(5) . . ? C2 Fe2 V1 141.4(3) . . ? S2 Fe2 V1 55.64(7) . . ? S3 Fe2 V1 54.79(7) . . ? S4 Fe2 V1 105.94(8) . . ? Fe1 Fe2 V1 61.78(5) . . ? Fe3 Fe2 V1 61.81(5) . . ? S1 Fe3 S2 107.70(9) . . ? S1 Fe3 S4 114.76(10) . 3_775 ? S2 Fe3 S4 113.53(10) . 3_775 ? S1 Fe3 S4 104.63(9) . . ? S2 Fe3 S4 104.16(10) . . ? S4 Fe3 S4 111.17(8) 3_775 . ? S1 Fe3 Fe3 126.26(9) . 3_775 ? S2 Fe3 Fe3 124.57(10) . 3_775 ? S4 Fe3 Fe3 56.88(7) 3_775 3_775 ? S4 Fe3 Fe3 54.29(7) . 3_775 ? S1 Fe3 Fe1 53.25(7) . . ? S2 Fe3 Fe1 99.85(8) . . ? S4 Fe3 Fe1 146.53(8) 3_775 . ? S4 Fe3 Fe1 55.15(7) . . ? Fe3 Fe3 Fe1 102.30(7) 3_775 . ? S1 Fe3 Fe2 99.92(8) . . ? S2 Fe3 Fe2 53.06(7) . . ? S4 Fe3 Fe2 145.28(8) 3_775 . ? S4 Fe3 Fe2 54.98(7) . . ? Fe3 Fe3 Fe2 101.55(7) 3_775 . ? Fe1 Fe3 Fe2 57.06(5) . . ? S1 Fe3 V1 54.76(7) . . ? S2 Fe3 V1 54.49(7) . . ? S4 Fe3 V1 144.94(8) 3_775 . ? S4 Fe3 V1 103.87(8) . . ? Fe3 Fe3 V1 158.14(8) 3_775 . ? Fe1 Fe3 V1 59.47(5) . . ? Fe2 Fe3 V1 59.27(5) . . ? C1 Fe1 S1 121.7(3) . . ? C1 Fe1 S3 102.7(3) . . ? S1 Fe1 S3 108.01(9) . . ? C1 Fe1 S4 110.5(3) . . ? S1 Fe1 S4 104.31(10) . . ? S3 Fe1 S4 109.30(9) . . ? C1 Fe1 Fe2 134.6(3) . . ? S1 Fe1 Fe2 103.56(8) . . ? S3 Fe1 Fe2 55.44(7) . . ? S4 Fe1 Fe2 56.69(7) . . ? C1 Fe1 Fe3 152.2(3) . . ? S1 Fe1 Fe3 53.15(7) . . ? S3 Fe1 Fe3 104.64(8) . . ? S4 Fe1 Fe3 54.90(6) . . ? Fe2 Fe1 Fe3 61.50(5) . . ? C1 Fe1 V1 142.6(3) . . ? S1 Fe1 V1 55.75(7) . . ? S3 Fe1 V1 54.69(7) . . ? S4 Fe1 V1 105.55(7) . . ? Fe2 Fe1 V1 61.49(5) . . ? Fe3 Fe1 V1 61.73(5) . . ? N4 V1 N8 80.6(3) . . ? N4 V1 N6 80.8(3) . . ? N8 V1 N6 81.0(3) . . ? N4 V1 S3 85.8(2) . . ? N8 V1 S3 87.7(2) . . ? N6 V1 S3 163.7(2) . . ? N4 V1 S2 88.4(2) . . ? N8 V1 S2 164.08(19) . . ? N6 V1 S2 85.9(2) . . ? S3 V1 S2 103.01(10) . . ? N4 V1 S1 165.4(2) . . ? N8 V1 S1 87.83(19) . . ? N6 V1 S1 88.7(2) . . ? S3 V1 S1 102.68(9) . . ? S2 V1 S1 100.99(10) . . ? N4 V1 Fe2 97.7(2) . . ? N8 V1 Fe2 140.5(2) . . ? N6 V1 Fe2 138.0(2) . . ? S3 V1 Fe2 52.95(7) . . ? S2 V1 Fe2 52.15(7) . . ? S1 V1 Fe2 96.90(7) . . ? N4 V1 Fe1 138.4(2) . . ? N8 V1 Fe1 99.07(18) . . ? N6 V1 Fe1 140.6(2) . . ? S3 V1 Fe1 52.76(7) . . ? S2 V1 Fe1 96.80(7) . . ? S1 V1 Fe1 52.12(7) . . ? Fe2 V1 Fe1 56.73(4) . . ? N4 V1 Fe3 139.6(2) . . ? N8 V1 Fe3 138.99(19) . . ? N6 V1 Fe3 95.5(2) . . ? S3 V1 Fe3 100.67(8) . . ? S2 V1 Fe3 51.19(7) . . ? S1 V1 Fe3 51.17(7) . . ? Fe2 V1 Fe3 58.92(5) . . ? Fe1 V1 Fe3 58.80(5) . . ? Fe3 S1 Fe1 73.60(8) . . ? Fe3 S1 V1 74.07(8) . . ? Fe1 S1 V1 72.13(8) . . ? Fe2 S2 Fe3 73.82(8) . . ? Fe2 S2 V1 72.22(8) . . ? Fe3 S2 V1 74.32(8) . . ? Fe1 S3 Fe2 69.24(8) . . ? Fe1 S3 V1 72.55(8) . . ? Fe2 S3 V1 72.26(8) . . ? Fe3 S4 Fe3 68.83(8) 3_775 . ? Fe3 S4 Fe2 125.65(10) 3_775 . ? Fe3 S4 Fe2 70.10(7) . . ? Fe3 S4 Fe1 126.51(11) 3_775 . ? Fe3 S4 Fe1 69.96(7) . . ? Fe2 S4 Fe1 66.41(7) . . ? C5 N4 N3 105.8(7) . . ? C5 N4 V1 130.8(6) . . ? N3 N4 V1 123.1(6) . . ? C11 N8 N7 105.7(7) . . ? C11 N8 V1 131.1(6) . . ? N7 N8 V1 123.1(5) . . ? C8 N6 N5 106.7(7) . . ? C8 N6 V1 130.5(6) . . ? N5 N6 V1 122.9(6) . . ? C12 N9 C16 111.3(7) . . ? C12 N9 C24 110.4(8) . . ? C16 N9 C24 106.7(7) . . ? C12 N9 C20 105.3(7) . . ? C16 N9 C20 111.2(8) . . ? C24 N9 C20 112.0(7) . . ? N6 N5 C6 108.6(8) . . ? N6 N5 B1 118.8(8) . . ? C6 N5 B1 132.6(9) . . ? C9 N7 N8 110.1(8) . . ? C9 N7 B1 131.4(9) . . ? N8 N7 B1 118.5(8) . . ? C3 N3 N4 110.5(8) . . ? C3 N3 B1 130.6(9) . . ? N4 N3 B1 118.9(8) . . ? C32 N10 C28 110.9(9) . . ? C32 N10 C36 110.6(8) . . ? C28 N10 C36 107.6(9) . . ? C32 N10 C40 105.3(8) . . ? C28 N10 C40 110.8(9) . . ? C36 N10 C40 111.6(9) . . ? N10 C32 C33 118.0(9) . . ? C9 C10 C11 104.9(9) . . ? C3 C4 C5 106.7(10) . . ? C27 C26 C25 113.2(8) . . ? N1 C1 Fe1 175.6(9) . . ? N6 C8 C7 111.1(9) . . ? C13 C12 N9 117.7(8) . . ? C12 C13 C14 111.2(8) . . ? C37 C36 N10 116.5(10) . . ? N7 C9 C10 107.8(9) . . ? N9 C16 C17 116.4(8) . . ? C24 C25 C26 110.3(8) . . ? N8 C11 C10 111.3(9) . . ? C32 C33 C34 109.3(9) . . ? N4 C5 C4 109.7(9) . . ? N5 C6 C7 109.3(9) . . ? C21 C20 N9 116.4(9) . . ? N10 C40 C41 115.1(9) . . ? N10 C28 C29 117.3(10) . . ? C18 C17 C16 109.2(9) . . ? N3 C3 C4 107.4(9) . . ? C6 C7 C8 104.3(9) . . ? C36 C37 C38 111.6(11) . . ? C25 C24 N9 116.9(7) . . ? C28 C29 C30 110.8(11) . . ? C42 C41 C40 108.1(11) . . ? N7 B1 N5 107.8(9) . . ? N7 B1 N3 108.5(9) . . ? N5 B1 N3 109.7(9) . . ? C15 C14 C13 111.7(10) . . ? N2 C2 Fe2 176.9(11) . . ? C35 C34 C33 113.6(12) . . ? C39 C38 C37 114.5(10) . . ? C43 C42 C41 115.9(14) . . ? C29 C30 C31 112.7(12) . . ? C20 C21 C22 109.1(11) . . ? C19 C18 C17 112.7(10) . . ? N1S C1S C2S 180(3) . . ? C21 C22 C23 111.3(15) . . ? N2S C3S C4S 177.9(19) . . ? N3S C5S C6S 137(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.919 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.096 data_ts1150sad _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'bis(Tetraethylammoinum) Tetrakis(\m3-sulfido)-triscyano-(hydrogen tri(pyrazolyl)borato-N,N',N")-tri-iron-vanadium' ; _chemical_name_common 'Cyano vanadium single cubane' _chemical_melting_point 'not measured' _chemical_formula_moiety '(Et4N)2 ((C9H10N6B)VFe3S4(CN)3)' _chemical_formula_sum 'C44 H82 B Fe3 N11 S4 V' _chemical_formula_weight 1122.32 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' 'V' 'V' 0.3005 0.5294 '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' _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 11.224(2) _cell_length_b 40.248(7) _cell_length_c 12.602(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.759(3) _cell_angle_gamma 90.00 _cell_volume 5640.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 994 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.46 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2372 _exptl_absorpt_coefficient_mu 1.105 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.604101 _exptl_absorpt_correction_T_max 0.939683 _exptl_absorpt_process_details SADABS _exptl_special_details ; none ; _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_% ? _diffrn_reflns_number 37278 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -52 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 27.89 _reflns_number_total 13357 _reflns_number_gt 7930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^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 13357 _refine_ls_number_parameters 626 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1212 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.2023 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.005 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 B1 B -0.1341(6) 0.14584(15) 0.5910(4) 0.0470(14) Uani 1 1 d . . . C1 C 0.2576(4) 0.21411(13) 0.2704(4) 0.0446(12) Uani 1 1 d . . . C2 C 0.4034(5) 0.07232(13) 0.4452(5) 0.0578(14) Uani 1 1 d . . . C3 C 0.0434(5) 0.09336(13) 0.0754(4) 0.0527(13) Uani 1 1 d . . . C4 C -0.0958(5) 0.21008(13) 0.5980(4) 0.0504(14) Uani 1 1 d . . . H4 H -0.1495 0.2161 0.6468 0.060 Uiso 1 1 calc R . . C5 C -0.0228(5) 0.23168(13) 0.5506(4) 0.0538(14) Uani 1 1 d . . . H5 H -0.0155 0.2550 0.5602 0.065 Uiso 1 1 calc R . . C6 C 0.0370(5) 0.21170(11) 0.4865(4) 0.0438(11) Uani 1 1 d . . . H6 H 0.0937 0.2195 0.4428 0.053 Uiso 1 1 calc R . . C7 C -0.0054(5) 0.10953(12) 0.7378(4) 0.0509(13) Uani 1 1 d . . . H7 H -0.0539 0.1112 0.7938 0.061 Uiso 1 1 calc R . . C8 C 0.1018(5) 0.09247(13) 0.7424(4) 0.0500(13) Uani 1 1 d . . . H8 H 0.1414 0.0803 0.8015 0.060 Uiso 1 1 calc R . . C9 C 0.1395(5) 0.09670(11) 0.6440(4) 0.0431(11) Uani 1 1 d . . . H9 H 0.2112 0.0876 0.6237 0.052 Uiso 1 1 calc R . . C10 C -0.3059(5) 0.11991(15) 0.4583(5) 0.0571(14) Uani 1 1 d . . . H10 H -0.3693 0.1217 0.5008 0.069 Uiso 1 1 calc R . . C11 C -0.3154(5) 0.10697(14) 0.3571(5) 0.0597(15) Uani 1 1 d . . . H11 H -0.3851 0.0980 0.3159 0.072 Uiso 1 1 calc R . . C12 C -0.2015(5) 0.10976(12) 0.3281(4) 0.0482(12) Uani 1 1 d . . . H12 H -0.1797 0.1029 0.2613 0.058 Uiso 1 1 calc R . . C13 C 0.4313(5) 0.29905(15) 0.4043(4) 0.0647(16) Uani 1 1 d . . . H13A H 0.3648 0.2829 0.3882 0.078 Uiso 1 1 calc R . . H13B H 0.4451 0.3093 0.3357 0.078 Uiso 1 1 calc R . . C14 C 0.3892(7) 0.32653(17) 0.4762(5) 0.082(2) Uani 1 1 d . . . H14A H 0.3845 0.3173 0.5483 0.098 Uiso 1 1 calc R . . H14B H 0.4495 0.3446 0.4839 0.098 Uiso 1 1 calc R . . C15 C 0.2699(6) 0.34046(19) 0.4320(6) 0.083(2) Uani 1 1 d . . . H15A H 0.2088 0.3227 0.4309 0.099 Uiso 1 1 calc R . . H15B H 0.2728 0.3474 0.3571 0.099 Uiso 1 1 calc R . . C16 C 0.2282(8) 0.3710(3) 0.4962(9) 0.141(4) Uani 1 1 d . . . H16A H 0.2489 0.3670 0.5732 0.211 Uiso 1 1 calc R . . H16B H 0.1410 0.3738 0.4790 0.211 Uiso 1 1 calc R . . H16C H 0.2688 0.3912 0.4762 0.211 Uiso 1 1 calc R . . C17 C 0.6506(5) 0.30294(16) 0.4751(4) 0.0706(18) Uani 1 1 d . . . H17A H 0.7198 0.2896 0.5085 0.085 Uiso 1 1 calc R . . H17B H 0.6313 0.3193 0.5288 0.085 Uiso 1 1 calc R . . C18 C 0.6883(7) 0.3217(2) 0.3803(5) 0.092(2) Uani 1 1 d . . . H18A H 0.6177 0.3331 0.3410 0.110 Uiso 1 1 calc R . . H18B H 0.7194 0.3058 0.3307 0.110 Uiso 1 1 calc R . . C19 C 0.7869(6) 0.34748(18) 0.4195(6) 0.084(2) Uani 1 1 d . . . H19A H 0.8069 0.3601 0.3568 0.100 Uiso 1 1 calc R . . H19B H 0.7540 0.3634 0.4678 0.100 Uiso 1 1 calc R . . C20 C 0.8977(7) 0.3332(2) 0.4757(7) 0.103(3) Uani 1 1 d . . . H20A H 0.8800 0.3217 0.5404 0.154 Uiso 1 1 calc R . . H20B H 0.9560 0.3510 0.4958 0.154 Uiso 1 1 calc R . . H20C H 0.9313 0.3174 0.4287 0.154 Uiso 1 1 calc R . . C21 C 0.5644(5) 0.25515(16) 0.3624(5) 0.0669(17) Uani 1 1 d . . . H21A H 0.4912 0.2413 0.3464 0.080 Uiso 1 1 calc R . . H21B H 0.5747 0.2675 0.2964 0.080 Uiso 1 1 calc R . . C22 C 0.6708(7) 0.2323(2) 0.3889(7) 0.107(3) Uani 1 1 d . . . H22A H 0.6574 0.2180 0.4499 0.128 Uiso 1 1 calc R . . H22B H 0.7437 0.2458 0.4111 0.128 Uiso 1 1 calc R . . C23 C 0.6913(7) 0.2104(2) 0.2930(8) 0.112(3) Uani 1 1 d . . . H23A H 0.7103 0.2251 0.2345 0.135 Uiso 1 1 calc R . . H23B H 0.7629 0.1964 0.3147 0.135 Uiso 1 1 calc R . . C24 C 0.5907(9) 0.1886(2) 0.2500(9) 0.132(3) Uani 1 1 d . . . H24A H 0.5773 0.1720 0.3040 0.199 Uiso 1 1 calc R . . H24B H 0.6103 0.1773 0.1856 0.199 Uiso 1 1 calc R . . H24C H 0.5178 0.2019 0.2318 0.199 Uiso 1 1 calc R . . C25 C 0.5291(6) 0.26239(16) 0.5533(4) 0.0735(19) Uani 1 1 d . . . H25A H 0.5230 0.2795 0.6088 0.088 Uiso 1 1 calc R . . H25B H 0.6028 0.2493 0.5760 0.088 Uiso 1 1 calc R . . C26 C 0.4200(6) 0.23910(17) 0.5490(5) 0.079(2) Uani 1 1 d . . . H26A H 0.3448 0.2522 0.5341 0.094 Uiso 1 1 calc R . . H26B H 0.4215 0.2227 0.4906 0.094 Uiso 1 1 calc R . . C27 C 0.4226(7) 0.22113(19) 0.6546(5) 0.089(2) Uani 1 1 d . . . H27A H 0.4329 0.2376 0.7135 0.106 Uiso 1 1 calc R . . H27B H 0.3445 0.2098 0.6562 0.106 Uiso 1 1 calc R . . C28 C 0.5225(8) 0.1958(2) 0.6728(7) 0.112(3) Uani 1 1 d . . . H28A H 0.5281 0.1839 0.6059 0.167 Uiso 1 1 calc R . . H28B H 0.5055 0.1800 0.7280 0.167 Uiso 1 1 calc R . . H28C H 0.5988 0.2071 0.6963 0.167 Uiso 1 1 calc R . . C29 C 0.1178(5) 0.97707(16) 0.1974(6) 0.076(2) Uani 0.920(4) 1 d P A 1 H29A H 0.1242 0.9706 0.1226 0.092 Uiso 0.920(4) 1 calc PR A 1 H29B H 0.0832 0.9579 0.2321 0.092 Uiso 0.920(4) 1 calc PR A 1 C30 C 0.0313(6) 1.00621(14) 0.1959(6) 0.0632(18) Uani 0.920(4) 1 d P A 1 H30A H 0.0258 1.0133 0.2703 0.076 Uiso 0.920(4) 1 calc PR A 1 H30B H 0.0625 1.0251 0.1577 0.076 Uiso 0.920(4) 1 calc PR A 1 C31 C -0.0900(6) 0.99715(18) 0.1423(8) 0.096(3) Uani 0.920(4) 1 d P A 1 H31A H -0.1221 0.9789 0.1828 0.115 Uiso 0.920(4) 1 calc PR A 1 H31B H -0.0831 0.9888 0.0695 0.115 Uiso 0.920(4) 1 calc PR A 1 C32 C -0.1789(7) 1.02614(17) 0.1337(7) 0.090(3) Uani 0.920(4) 1 d P A 1 H32A H -0.1890 1.0339 0.2056 0.134 Uiso 0.920(4) 1 calc PR A 1 H32B H -0.2567 1.0188 0.0964 0.134 Uiso 0.920(4) 1 calc PR A 1 H32C H -0.1479 1.0443 0.0934 0.134 Uiso 0.920(4) 1 calc PR A 1 C33 C 0.2430(6) 0.99264(15) 0.3716(5) 0.0622(17) Uani 0.920(4) 1 d P A 1 H33A H 0.2028 1.0145 0.3745 0.075 Uiso 0.920(4) 1 calc PR A 1 H33B H 0.3273 0.9954 0.4053 0.075 Uiso 0.920(4) 1 calc PR A 1 C34 C 0.1813(6) 0.96795(17) 0.4393(7) 0.078(2) Uani 0.920(4) 1 d P A 1 H34A H 0.0974 0.9643 0.4057 0.093 Uiso 0.920(4) 1 calc PR A 1 H34B H 0.2238 0.9464 0.4414 0.093 Uiso 0.920(4) 1 calc PR A 1 C35 C 0.1813(10) 0.9802(3) 0.5483(9) 0.123(4) Uani 0.920(4) 1 d P A 1 H35A H 0.1003 0.9899 0.5489 0.147 Uiso 0.920(4) 1 calc PR A 1 H35B H 0.1834 0.9599 0.5931 0.147 Uiso 0.920(4) 1 calc PR A 1 C36 C 0.2511(15) 0.9999(4) 0.6011(9) 0.226(10) Uani 0.920(4) 1 d P A 1 H36A H 0.2917 0.9887 0.6650 0.340 Uiso 0.920(4) 1 calc PR A 1 H36B H 0.2056 1.0189 0.6228 0.340 Uiso 0.920(4) 1 calc PR A 1 H36C H 0.3112 1.0077 0.5571 0.340 Uiso 0.920(4) 1 calc PR A 1 C37 C 0.3136(7) 0.9528(2) 0.2464(9) 0.137(5) Uani 0.920(4) 1 d PD A 1 H37A H 0.3962 0.9594 0.2766 0.164 Uiso 0.920(4) 1 calc PR A 1 H37B H 0.2855 0.9383 0.3015 0.164 Uiso 0.920(4) 1 calc PR A 1 C38 C 0.3328(12) 0.9310(4) 0.1694(11) 0.209(8) Uani 0.920(4) 1 d PD A 1 H38A H 0.3707 0.9438 0.1158 0.250 Uiso 0.920(4) 1 calc PR A 1 H38B H 0.2524 0.9243 0.1338 0.250 Uiso 0.920(4) 1 calc PR A 1 C39 C 0.4079(14) 0.8980(4) 0.1896(17) 0.259(11) Uani 0.920(4) 1 d PD A 1 H39A H 0.3513 0.8796 0.1974 0.310 Uiso 0.920(4) 1 calc PR A 1 H39B H 0.4465 0.8934 0.1251 0.310 Uiso 0.920(4) 1 calc PR A 1 C40 C 0.4984(14) 0.8977(3) 0.2800(12) 0.165(6) Uani 0.920(4) 1 d PD A 1 H40A H 0.4665 0.9074 0.3416 0.248 Uiso 0.920(4) 1 calc PR A 1 H40B H 0.5677 0.9107 0.2642 0.248 Uiso 0.920(4) 1 calc PR A 1 H40C H 0.5235 0.8747 0.2964 0.248 Uiso 0.920(4) 1 calc PR A 1 C41 C 0.2968(6) 1.0135(2) 0.2041(5) 0.082(3) Uani 0.920(4) 1 d PD A 1 H41A H 0.3784 1.0165 0.2437 0.099 Uiso 0.920(4) 1 calc PR A 1 H41B H 0.2491 1.0328 0.2224 0.099 Uiso 0.920(4) 1 calc PR A 1 C42 C 0.3111(9) 1.0178(3) 0.0820(7) 0.122(4) Uani 0.920(4) 1 d PD A 1 H42A H 0.3673 1.0004 0.0636 0.147 Uiso 0.920(4) 1 calc PR A 1 H42B H 0.2320 1.0131 0.0397 0.147 Uiso 0.920(4) 1 calc PR A 1 C43 C 0.3551(11) 1.0509(3) 0.0439(8) 0.129(4) Uani 0.920(4) 1 d PD A 1 H43A H 0.3461 1.0516 -0.0353 0.155 Uiso 0.920(4) 1 calc PR A 1 H43B H 0.3081 1.0694 0.0692 0.155 Uiso 0.920(4) 1 calc PR A 1 C44 C 0.4767(10) 1.0537(4) 0.0869(8) 0.145(5) Uani 0.920(4) 1 d PD A 1 H44A H 0.4829 1.0598 0.1627 0.218 Uiso 0.920(4) 1 calc PR A 1 H44B H 0.5151 1.0709 0.0479 0.218 Uiso 0.920(4) 1 calc PR A 1 H44C H 0.5171 1.0324 0.0800 0.218 Uiso 0.920(4) 1 calc PR A 1 C38' C 0.4502(10) 0.9612(3) 0.2718(13) 0.155(5) Uani 0.920(4) 1 d P A 2 C39' C 0.5250(10) 0.9278(4) 0.2304(11) 0.148(5) Uani 0.920(4) 1 d P A 2 C42' C 0.4460(11) 1.0062(4) 0.2457(13) 0.176(6) Uani 0.920(4) 1 d P A 2 C43' C 0.4840(19) 1.0423(5) 0.1980(15) 0.246(11) Uani 0.920(4) 1 d P A 2 Fe1 Fe 0.22213(6) 0.166385(17) 0.30645(5) 0.04120(19) Uani 1 1 d . . . Fe2 Fe 0.27851(6) 0.106294(17) 0.38484(6) 0.0433(2) Uani 1 1 d . . . Fe3 Fe 0.10688(7) 0.113470(16) 0.22133(5) 0.04207(19) Uani 1 1 d . . . H1' H -0.204(4) 0.1485(11) 0.647(3) 0.034(11) Uiso 1 1 d . . . N1 N 0.2687(4) 0.24115(12) 0.2504(4) 0.0623(13) Uani 1 1 d . . . N2 N 0.4707(5) 0.05270(14) 0.4775(6) 0.096(2) Uani 1 1 d . . . N3 N 0.0076(5) 0.08249(13) -0.0056(3) 0.0707(15) Uani 1 1 d . . . N4 N -0.0778(3) 0.17927(10) 0.5633(3) 0.0402(9) Uani 1 1 d . . . N5 N 0.0054(3) 0.18014(9) 0.4935(3) 0.0360(8) Uani 1 1 d . . . N6 N -0.0294(4) 0.12340(10) 0.6398(3) 0.0405(9) Uani 1 1 d . . . N7 N 0.0611(3) 0.11549(9) 0.5808(3) 0.0375(8) Uani 1 1 d . . . N8 N -0.1925(3) 0.12963(10) 0.4873(3) 0.0432(9) Uani 1 1 d . . . N9 N -0.1266(3) 0.12344(9) 0.4072(3) 0.0362(8) Uani 1 1 d . . . N10 N 0.5436(4) 0.28002(12) 0.4483(3) 0.0647(14) Uani 1 1 d . . . N11 N 0.2440(4) 0.98367(14) 0.2552(5) 0.0702(17) Uani 0.920(4) 1 d P A 1 S1 S 0.26201(11) 0.15266(3) 0.47996(9) 0.0395(3) Uani 1 1 d . . . S2 S 0.09666(11) 0.08065(3) 0.36512(9) 0.0378(3) Uani 1 1 d . . . S3 S 0.02097(11) 0.16219(3) 0.25619(8) 0.0368(3) Uani 1 1 d . . . S4 S 0.30820(14) 0.12559(4) 0.22203(12) 0.0608(4) Uani 1 1 d . . . V1 V 0.06522(6) 0.134925(16) 0.41940(5) 0.02859(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.049(3) 0.053(3) 0.044(3) 0.005(3) 0.023(3) 0.010(3) C1 0.043(3) 0.050(3) 0.038(2) 0.011(2) -0.006(2) -0.013(2) C2 0.034(3) 0.040(3) 0.102(4) -0.003(3) 0.020(3) -0.003(2) C3 0.080(4) 0.044(3) 0.037(3) -0.003(2) 0.020(3) -0.009(3) C4 0.058(3) 0.056(3) 0.034(2) -0.015(2) -0.005(2) 0.027(3) C5 0.069(4) 0.035(3) 0.051(3) -0.013(2) -0.014(3) 0.012(3) C6 0.055(3) 0.031(2) 0.043(2) -0.008(2) 0.000(2) 0.000(2) C7 0.074(4) 0.049(3) 0.030(2) 0.000(2) 0.010(2) -0.006(3) C8 0.066(4) 0.045(3) 0.036(2) 0.009(2) -0.003(2) -0.001(3) C9 0.050(3) 0.036(3) 0.042(2) 0.001(2) 0.001(2) 0.001(2) C10 0.034(3) 0.071(4) 0.067(4) 0.017(3) 0.009(3) -0.006(3) C11 0.036(3) 0.066(4) 0.074(4) 0.005(3) -0.004(3) -0.018(3) C12 0.047(3) 0.044(3) 0.051(3) 0.002(2) -0.002(2) -0.009(2) C13 0.073(4) 0.068(4) 0.045(3) 0.005(3) -0.020(3) -0.020(3) C14 0.119(6) 0.068(4) 0.052(3) -0.008(3) -0.005(4) -0.020(4) C15 0.078(5) 0.092(5) 0.077(4) -0.024(4) 0.008(4) -0.012(4) C16 0.092(7) 0.150(10) 0.185(10) -0.048(8) 0.034(7) -0.013(6) C17 0.066(4) 0.081(4) 0.057(3) 0.013(3) -0.018(3) -0.035(3) C18 0.097(5) 0.098(6) 0.074(4) 0.031(4) -0.015(4) -0.029(4) C19 0.077(5) 0.083(5) 0.088(5) 0.020(4) 0.004(4) -0.018(4) C20 0.076(5) 0.120(7) 0.113(6) 0.002(5) 0.018(5) -0.018(5) C21 0.056(4) 0.074(4) 0.063(4) 0.005(3) -0.018(3) -0.009(3) C22 0.084(6) 0.120(7) 0.103(6) 0.006(5) -0.041(5) 0.006(5) C23 0.065(5) 0.108(7) 0.154(8) 0.000(6) -0.016(5) 0.016(5) C24 0.136(9) 0.092(7) 0.163(9) 0.000(6) -0.002(7) 0.031(6) C25 0.094(5) 0.071(4) 0.048(3) 0.011(3) -0.019(3) -0.029(4) C26 0.081(5) 0.081(5) 0.067(4) 0.010(3) -0.016(3) -0.035(4) C27 0.096(6) 0.086(5) 0.081(5) 0.018(4) 0.005(4) -0.032(4) C28 0.111(7) 0.097(6) 0.123(7) 0.035(5) 0.004(5) -0.028(5) C29 0.043(4) 0.062(4) 0.125(6) -0.060(4) 0.017(4) -0.008(3) C30 0.064(4) 0.038(3) 0.094(5) -0.016(3) 0.037(4) -0.001(3) C31 0.053(4) 0.052(4) 0.188(9) -0.024(5) 0.033(5) 0.004(3) C32 0.077(5) 0.055(4) 0.148(7) 0.016(5) 0.057(5) 0.014(4) C33 0.057(4) 0.048(4) 0.087(4) -0.024(3) 0.028(3) -0.016(3) C34 0.058(4) 0.050(4) 0.119(6) 0.021(4) -0.014(4) -0.011(3) C35 0.121(8) 0.130(9) 0.128(8) 0.010(7) 0.053(7) -0.067(7) C36 0.33(2) 0.264(18) 0.086(7) 0.011(9) 0.044(10) -0.213(17) C37 0.046(5) 0.121(7) 0.239(12) -0.138(8) 0.000(6) 0.015(4) C38 0.120(11) 0.31(2) 0.187(13) -0.107(14) -0.007(9) 0.037(13) C39 0.123(13) 0.22(2) 0.43(3) -0.05(2) 0.023(17) 0.065(13) C40 0.156(12) 0.101(9) 0.215(14) 0.005(9) -0.059(11) 0.043(8) C41 0.051(4) 0.152(8) 0.049(4) -0.042(4) 0.023(3) -0.036(4) C42 0.099(7) 0.147(10) 0.122(8) -0.031(7) 0.020(6) -0.012(7) C43 0.179(12) 0.115(8) 0.104(7) 0.015(6) 0.056(8) -0.030(8) C44 0.120(9) 0.245(15) 0.077(6) 0.034(8) 0.041(6) 0.036(10) C38' 0.103(8) 0.101(8) 0.254(16) 0.005(9) 0.000(9) 0.018(7) C39' 0.099(8) 0.164(13) 0.178(12) 0.067(10) 0.002(8) -0.013(8) C42' 0.121(10) 0.190(15) 0.225(15) -0.019(12) 0.056(10) -0.043(10) C43' 0.29(2) 0.28(2) 0.187(15) -0.024(15) 0.102(15) -0.144(19) Fe1 0.0460(4) 0.0365(4) 0.0428(4) 0.0008(3) 0.0120(3) -0.0108(3) Fe2 0.0428(4) 0.0363(4) 0.0535(4) -0.0040(3) 0.0167(3) -0.0013(3) Fe3 0.0575(5) 0.0375(4) 0.0336(3) -0.0080(3) 0.0149(3) -0.0084(3) N1 0.062(3) 0.057(3) 0.062(3) 0.021(2) -0.014(2) -0.025(2) N2 0.054(3) 0.057(3) 0.183(7) 0.000(4) 0.035(4) 0.005(3) N3 0.115(4) 0.064(3) 0.036(2) -0.008(2) 0.020(3) -0.018(3) N4 0.049(2) 0.042(2) 0.0298(18) -0.0039(16) 0.0068(17) 0.0093(18) N5 0.047(2) 0.0304(19) 0.0303(18) -0.0037(15) 0.0041(16) 0.0031(16) N6 0.049(2) 0.045(2) 0.0292(18) 0.0032(16) 0.0105(17) 0.0017(18) N7 0.044(2) 0.034(2) 0.0341(19) 0.0031(16) 0.0055(17) 0.0023(17) N8 0.037(2) 0.052(2) 0.042(2) 0.0071(18) 0.0102(18) -0.0010(18) N9 0.040(2) 0.035(2) 0.0339(19) 0.0003(15) 0.0036(16) -0.0048(16) N10 0.073(3) 0.067(3) 0.045(2) 0.009(2) -0.024(2) -0.024(3) N11 0.040(3) 0.075(4) 0.097(4) -0.059(3) 0.015(3) -0.009(3) S1 0.0383(7) 0.0343(6) 0.0447(6) -0.0021(5) 0.0021(5) -0.0066(5) S2 0.0479(7) 0.0266(5) 0.0408(6) -0.0055(4) 0.0125(5) -0.0039(5) S3 0.0470(7) 0.0336(6) 0.0294(5) 0.0015(4) 0.0040(5) -0.0063(5) S4 0.0633(9) 0.0638(9) 0.0631(8) -0.0101(7) 0.0365(7) -0.0114(7) V1 0.0342(4) 0.0251(4) 0.0269(3) -0.0019(3) 0.0058(3) -0.0030(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 B1 N8 1.527(7) . ? B1 N6 1.543(7) . ? B1 N4 1.546(7) . ? C1 N1 1.128(6) . ? C1 Fe1 2.026(5) . ? C2 N2 1.130(7) . ? C2 Fe2 2.031(6) . ? C3 N3 1.133(6) . ? C3 Fe3 2.047(5) . ? C4 N4 1.340(6) . ? C4 C5 1.384(8) . ? C5 C6 1.377(7) . ? C6 N5 1.325(6) . ? C7 N6 1.348(6) . ? C7 C8 1.380(8) . ? C8 C9 1.374(7) . ? C9 N7 1.339(6) . ? C10 N8 1.335(6) . ? C10 C11 1.368(8) . ? C11 C12 1.381(7) . ? C12 N9 1.333(6) . ? C13 N10 1.515(7) . ? C13 C14 1.543(9) . ? C14 C15 1.489(9) . ? C15 C16 1.576(11) . ? C17 N10 1.516(7) . ? C17 C18 1.519(8) . ? C18 C19 1.550(9) . ? C19 C20 1.463(10) . ? C21 C22 1.508(10) . ? C21 N10 1.515(8) . ? C22 C23 1.538(12) . ? C23 C24 1.476(12) . ? C25 N10 1.529(7) . ? C25 C26 1.538(8) . ? C26 C27 1.510(9) . ? C27 C28 1.510(11) . ? C29 C30 1.521(8) . ? C29 N11 1.527(8) . ? C30 C31 1.481(9) . ? C31 C32 1.530(9) . ? C33 N11 1.512(8) . ? C33 C34 1.535(9) . ? C34 C35 1.459(12) . ? C35 C36 1.244(13) . ? C37 C38 1.345(12) . ? C37 N11 1.481(9) . ? C38 C39 1.574(14) . ? C39 C40 1.420(14) . ? C41 N11 1.519(9) . ? C41 C42 1.578(10) . ? C42 C43 1.521(11) . ? C43 C44 1.404(12) . ? C38' C39' 1.703(18) . ? C42' C43' 1.65(2) . ? Fe1 S1 2.2410(13) . ? Fe1 S4 2.2447(16) . ? Fe1 S3 2.2675(14) . ? Fe2 S1 2.2390(13) . ? Fe2 S4 2.2601(16) . ? Fe2 S2 2.2707(14) . ? Fe3 S3 2.2544(14) . ? Fe3 S2 2.2578(13) . ? Fe3 S4 2.3105(17) . ? N4 N5 1.366(5) . ? N5 V1 2.192(3) . ? N6 N7 1.375(5) . ? N7 V1 2.185(3) . ? N8 N9 1.353(5) . ? N9 V1 2.187(4) . ? S1 V1 2.3486(14) . ? S2 V1 2.3301(13) . ? S3 V1 2.3250(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 N8 B1 N6 107.9(4) . . ? N8 B1 N4 108.6(4) . . ? N6 B1 N4 106.7(4) . . ? N1 C1 Fe1 175.0(5) . . ? N2 C2 Fe2 178.0(6) . . ? N3 C3 Fe3 179.3(6) . . ? N4 C4 C5 108.5(4) . . ? C6 C5 C4 104.5(4) . . ? N5 C6 C5 111.4(5) . . ? N6 C7 C8 108.1(4) . . ? C9 C8 C7 105.9(4) . . ? N7 C9 C8 110.4(5) . . ? N8 C10 C11 108.6(5) . . ? C10 C11 C12 104.9(5) . . ? N9 C12 C11 110.5(5) . . ? N10 C13 C14 117.0(4) . . ? C15 C14 C13 112.4(5) . . ? C14 C15 C16 114.6(6) . . ? N10 C17 C18 115.0(4) . . ? C17 C18 C19 110.2(5) . . ? C20 C19 C18 114.5(7) . . ? C22 C21 N10 116.0(5) . . ? C21 C22 C23 111.9(6) . . ? C24 C23 C22 116.2(8) . . ? N10 C25 C26 115.5(4) . . ? C27 C26 C25 109.9(5) . . ? C28 C27 C26 112.5(7) . . ? C30 C29 N11 114.9(5) . . ? C31 C30 C29 111.2(5) . . ? C30 C31 C32 113.3(6) . . ? N11 C33 C34 116.6(5) . . ? C35 C34 C33 111.3(6) . . ? C36 C35 C34 129.6(9) . . ? C38 C37 N11 137.6(12) . . ? C37 C38 C39 124.5(14) . . ? C40 C39 C38 116.6(13) . . ? N11 C41 C42 126.7(6) . . ? C43 C42 C41 119.0(8) . . ? C44 C43 C42 106.8(10) . . ? C1 Fe1 S1 115.65(13) . . ? C1 Fe1 S4 118.53(15) . . ? S1 Fe1 S4 103.89(6) . . ? C1 Fe1 S3 103.08(14) . . ? S1 Fe1 S3 108.32(5) . . ? S4 Fe1 S3 106.81(6) . . ? C2 Fe2 S1 117.61(17) . . ? C2 Fe2 S4 113.09(17) . . ? S1 Fe2 S4 103.45(6) . . ? C2 Fe2 S2 107.44(15) . . ? S1 Fe2 S2 107.42(5) . . ? S4 Fe2 S2 107.30(6) . . ? C3 Fe3 S3 114.38(16) . . ? C3 Fe3 S2 116.13(15) . . ? S3 Fe3 S2 106.44(5) . . ? C3 Fe3 S4 107.96(16) . . ? S3 Fe3 S4 105.04(6) . . ? S2 Fe3 S4 106.02(6) . . ? C4 N4 N5 109.4(4) . . ? C4 N4 B1 130.3(4) . . ? N5 N4 B1 120.2(4) . . ? C6 N5 N4 106.2(4) . . ? C6 N5 V1 131.9(3) . . ? N4 N5 V1 121.9(3) . . ? C7 N6 N7 109.2(4) . . ? C7 N6 B1 130.9(4) . . ? N7 N6 B1 119.9(3) . . ? C9 N7 N6 106.5(4) . . ? C9 N7 V1 131.4(3) . . ? N6 N7 V1 122.1(3) . . ? C10 N8 N9 109.8(4) . . ? C10 N8 B1 130.0(4) . . ? N9 N8 B1 120.2(4) . . ? C12 N9 N8 106.3(4) . . ? C12 N9 V1 131.0(3) . . ? N8 N9 V1 122.7(3) . . ? C17 N10 C21 111.6(5) . . ? C17 N10 C13 111.6(5) . . ? C21 N10 C13 105.9(4) . . ? C17 N10 C25 105.3(4) . . ? C21 N10 C25 110.9(5) . . ? C13 N10 C25 111.7(5) . . ? C37 N11 C33 110.3(7) . . ? C37 N11 C41 113.1(7) . . ? C33 N11 C41 106.1(4) . . ? C37 N11 C29 106.4(5) . . ? C33 N11 C29 112.1(5) . . ? C41 N11 C29 108.9(6) . . ? Fe2 S1 Fe1 72.73(4) . . ? Fe2 S1 V1 73.44(4) . . ? Fe1 S1 V1 72.71(4) . . ? Fe3 S2 Fe2 71.31(4) . . ? Fe3 S2 V1 73.34(4) . . ? Fe2 S2 V1 73.22(4) . . ? Fe3 S3 Fe1 71.53(4) . . ? Fe3 S3 V1 73.50(4) . . ? Fe1 S3 V1 72.68(4) . . ? Fe1 S4 Fe2 72.27(5) . . ? Fe1 S4 Fe3 70.91(5) . . ? Fe2 S4 Fe3 70.55(5) . . ? N7 V1 N9 81.11(14) . . ? N7 V1 N5 81.64(13) . . ? N9 V1 N5 81.38(14) . . ? N7 V1 S3 164.45(11) . . ? N9 V1 S3 86.94(10) . . ? N5 V1 S3 86.78(10) . . ? N7 V1 S2 87.75(10) . . ? N9 V1 S2 88.16(10) . . ? N5 V1 S2 166.10(11) . . ? S3 V1 S2 101.86(5) . . ? N7 V1 S1 86.77(10) . . ? N9 V1 S1 163.92(10) . . ? N5 V1 S1 86.46(11) . . ? S3 V1 S1 102.90(5) . . ? S2 V1 S1 101.96(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.685 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.101 data_ts1151bsad1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'bis(Tetraethylammoinum) Tetrakis(\m3-sulfido)-trisazido-(hydrogen tri(pyrazolyl)borato-N,N',N")-tri-iron-vanadium' ; _chemical_name_common 'Azide vanadium single cubane' _chemical_melting_point 'not measured' _chemical_formula_moiety ' (Et4N)2 ((C9H10N6B)VFe3S4(N3)3)' _chemical_formula_sum 'C25 H50 B Fe3 N17 S4 V' _chemical_formula_weight 946.09 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' 'V' 'V' 0.3005 0.5294 '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' _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 23.671(8) _cell_length_b 34.548(12) _cell_length_c 15.700(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.308(7) _cell_angle_gamma 90.00 _cell_volume 12189(7) _cell_formula_units_Z 12 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 986 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 28.09 _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5868 _exptl_absorpt_coefficient_mu 1.522 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _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_% ? _diffrn_reflns_number 80994 _diffrn_reflns_av_R_equivalents 0.1090 _diffrn_reflns_av_sigmaI/netI 0.1531 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 28.35 _reflns_number_total 29462 _reflns_number_gt 14703 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+11.7127P] 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 29462 _refine_ls_number_parameters 1414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1715 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Fe1 Fe 0.21026(4) 0.36933(2) 0.03026(6) 0.0236(2) Uani 1 1 d . . . Fe2 Fe 0.27682(4) 0.35912(2) 0.20508(6) 0.0244(2) Uani 1 1 d . . . Fe3 Fe 0.18917(4) 0.41240(2) 0.15767(6) 0.0238(2) Uani 1 1 d . . . V1 V 0.15793(4) 0.33451(3) 0.14327(7) 0.0202(2) Uani 1 1 d . . . S1 S 0.11961(7) 0.38444(4) 0.04162(11) 0.0238(4) Uani 1 1 d . . . S2 S 0.23928(7) 0.31254(4) 0.10097(11) 0.0249(4) Uani 1 1 d . . . S3 S 0.20626(7) 0.37066(4) 0.27380(11) 0.0263(4) Uani 1 1 d . . . S4 S 0.27687(7) 0.41260(4) 0.12054(12) 0.0275(4) Uani 1 1 d . . . C1 C 0.0295(3) 0.25305(18) -0.0173(5) 0.0324(17) Uani 1 1 d . . . H1 H -0.0008 0.2343 -0.0225 0.039 Uiso 1 1 calc R . . C2 C 0.0470(3) 0.26732(19) -0.0870(5) 0.0386(18) Uani 1 1 d . . . H2 H 0.0321 0.2604 -0.1486 0.046 Uiso 1 1 calc R . . C3 C 0.0915(3) 0.29415(18) -0.0472(5) 0.0314(16) Uani 1 1 d . . . H3 H 0.1124 0.3090 -0.0784 0.038 Uiso 1 1 calc R . . C4 C 0.1404(3) 0.22640(18) 0.2708(5) 0.0345(17) Uani 1 1 d . . . H4 H 0.1167 0.2051 0.2773 0.041 Uiso 1 1 calc R . . C5 C 0.1995(3) 0.23054(19) 0.3132(5) 0.0373(18) Uani 1 1 d . . . H5 H 0.2249 0.2131 0.3546 0.045 Uiso 1 1 calc R . . C6 C 0.2155(3) 0.26584(18) 0.2836(5) 0.0323(16) Uani 1 1 d . . . H6 H 0.2544 0.2766 0.3022 0.039 Uiso 1 1 calc R . . C7 C -0.0084(3) 0.3198(2) 0.1976(5) 0.0346(17) Uani 1 1 d . . . H7 H -0.0401 0.3036 0.2011 0.041 Uiso 1 1 calc R . . C8 C -0.0051(3) 0.3590(2) 0.2099(5) 0.0369(17) Uani 1 1 d . . . H8 H -0.0333 0.3754 0.2235 0.044 Uiso 1 1 calc R . . C9 C 0.0486(3) 0.36955(19) 0.1981(4) 0.0307(16) Uani 1 1 d . . . H9 H 0.0634 0.3953 0.2028 0.037 Uiso 1 1 calc R . . N1 N 0.2033(3) 0.36722(17) -0.0976(4) 0.0374(15) Uani 1 1 d . . . N2 N 0.1969(3) 0.39201(19) -0.1508(4) 0.0379(15) Uani 1 1 d . . . N3 N 0.1914(4) 0.4155(2) -0.2060(5) 0.073(2) Uani 1 1 d . . . N4 N 0.3518(2) 0.34595(16) 0.2973(4) 0.0355(14) Uani 1 1 d . . . N5 N 0.3602(3) 0.33311(17) 0.3687(5) 0.0508(19) Uani 1 1 d . . . N6 N 0.3714(4) 0.3210(2) 0.4424(6) 0.084(3) Uani 1 1 d . . . N7 N 0.1632(3) 0.46611(16) 0.1717(4) 0.0387(16) Uani 1 1 d . . . N8 N 0.1419(3) 0.48635(19) 0.1092(6) 0.059(2) Uani 1 1 d . . . N9 N 0.1207(4) 0.5083(2) 0.0497(7) 0.101(4) Uani 1 1 d . . . N10 N 0.0621(2) 0.26993(14) 0.0588(4) 0.0269(13) Uani 1 1 d . . . N11 N 0.1003(2) 0.29597(14) 0.0405(3) 0.0232(12) Uani 1 1 d . . . N12 N 0.1209(2) 0.25776(14) 0.2173(4) 0.0269(13) Uani 1 1 d . . . N13 N 0.1675(2) 0.28221(14) 0.2251(4) 0.0278(13) Uani 1 1 d . . . N14 N 0.0408(2) 0.30782(14) 0.1797(4) 0.0284(13) Uani 1 1 d . . . N15 N 0.0768(2) 0.33857(14) 0.1792(4) 0.0265(12) Uani 1 1 d . . . B1 B 0.0592(4) 0.2673(2) 0.1540(6) 0.0317(19) Uani 1 1 d . . . H1A H 0.027(2) 0.2455(15) 0.155(4) 0.021(15) Uiso 1 1 d . . . Fe4 Fe 0.60684(4) 0.37901(3) 0.86893(7) 0.0294(2) Uani 1 1 d . . . Fe5 Fe 0.50878(4) 0.42450(2) 0.81181(7) 0.0280(2) Uani 1 1 d . . . Fe6 Fe 0.53358(4) 0.37479(3) 0.69796(7) 0.0284(2) Uani 1 1 d . . . V2 V 0.49343(4) 0.34634(3) 0.83244(7) 0.0199(2) Uani 1 1 d . . . S5 S 0.57414(7) 0.32407(4) 0.78757(12) 0.0282(4) Uani 1 1 d . . . S6 S 0.54072(7) 0.39159(4) 0.94267(11) 0.0268(4) Uani 1 1 d . . . S7 S 0.44251(7) 0.38624(4) 0.71228(11) 0.0261(4) Uani 1 1 d . . . S8 S 0.59198(8) 0.42719(5) 0.76562(13) 0.0393(5) Uani 1 1 d . . . C10 C 0.3484(3) 0.3345(2) 0.9418(4) 0.0327(16) Uani 1 1 d . . . H10 H 0.3230 0.3186 0.9632 0.039 Uiso 1 1 calc R . . C11 C 0.3495(3) 0.3741(2) 0.9426(5) 0.0356(17) Uani 1 1 d . . . H11 H 0.3253 0.3911 0.9638 0.043 Uiso 1 1 calc R . . C12 C 0.3934(3) 0.38404(18) 0.9058(5) 0.0318(16) Uani 1 1 d . . . H12 H 0.4045 0.4099 0.8978 0.038 Uiso 1 1 calc R . . C13 C 0.3768(3) 0.24978(19) 0.7296(5) 0.0383(19) Uani 1 1 d . . . H13 H 0.3519 0.2296 0.7380 0.046 Uiso 1 1 calc R . . C14 C 0.3893(3) 0.2576(2) 0.6520(6) 0.045(2) Uani 1 1 d . . . H14 H 0.3750 0.2441 0.5967 0.054 Uiso 1 1 calc R . . C15 C 0.4271(3) 0.28931(19) 0.6707(5) 0.0344(17) Uani 1 1 d . . . H15 H 0.4429 0.3015 0.6289 0.041 Uiso 1 1 calc R . . C16 C 0.5007(3) 0.24938(18) 1.0109(5) 0.0324(16) Uani 1 1 d . . . H16 H 0.4808 0.2291 1.0307 0.039 Uiso 1 1 calc R . . C17 C 0.5606(3) 0.25670(18) 1.0418(5) 0.0339(17) Uani 1 1 d . . . H17 H 0.5901 0.2431 1.0870 0.041 Uiso 1 1 calc R . . C18 C 0.5688(3) 0.28853(17) 0.9924(4) 0.0285(15) Uani 1 1 d . . . H18 H 0.6062 0.3002 0.9984 0.034 Uiso 1 1 calc R . . N16 N 0.6865(2) 0.37534(18) 0.9589(4) 0.0423(16) Uani 1 1 d . . . N17 N 0.7062(3) 0.34804(19) 1.0010(5) 0.0435(17) Uani 1 1 d . . . N18 N 0.7289(3) 0.3219(2) 1.0450(5) 0.064(2) Uani 1 1 d . . . N19 N 0.4686(3) 0.47313(17) 0.8225(5) 0.0500(18) Uani 1 1 d . . . N20 N 0.4774(3) 0.50598(19) 0.8294(4) 0.0416(16) Uani 1 1 d . . . N21 N 0.4822(3) 0.53918(18) 0.8369(5) 0.067(2) Uani 1 1 d . . . N22 N 0.5305(3) 0.37013(19) 0.5709(4) 0.0453(16) Uani 1 1 d . . . N23 N 0.5314(3) 0.3962(2) 0.5228(5) 0.0449(17) Uani 1 1 d . . . N24 N 0.5331(3) 0.4214(2) 0.4737(5) 0.073(2) Uani 1 1 d . . . N25 N 0.3898(2) 0.32166(15) 0.9052(4) 0.0273(12) Uani 1 1 d . . . N26 N 0.4182(2) 0.35264(14) 0.8832(3) 0.0237(12) Uani 1 1 d . . . N27 N 0.4063(2) 0.27582(14) 0.7925(4) 0.0283(13) Uani 1 1 d . . . N28 N 0.4379(2) 0.30006(14) 0.7555(4) 0.0261(12) Uani 1 1 d . . . N29 N 0.4747(2) 0.27584(14) 0.9476(4) 0.0276(13) Uani 1 1 d . . . N30 N 0.5170(2) 0.30045(13) 0.9354(3) 0.0232(12) Uani 1 1 d . . . N40 N 0.2081(2) 0.77815(14) -0.0938(4) 0.0265(13) Uani 1 1 d . . . B2 B 0.4093(4) 0.2803(2) 0.8908(6) 0.0325(19) Uani 1 1 d . . . H2A H 0.383(2) 0.2583(15) 0.915(4) 0.024(16) Uiso 1 1 d . . . Fe7 Fe 0.13278(4) 0.86594(2) 0.15507(6) 0.0259(2) Uani 1 1 d . . . Fe8 Fe 0.13775(4) 0.92020(2) 0.03524(7) 0.0262(2) Uani 1 1 d . . . Fe9 Fe 0.05718(4) 0.86382(2) -0.01553(7) 0.0269(2) Uani 1 1 d . . . V3 V 0.17573(4) 0.84572(3) 0.01589(7) 0.0194(2) Uani 1 1 d . . . S9 S 0.21659(7) 0.89029(4) 0.13215(11) 0.0251(4) Uani 1 1 d . . . S10 S 0.11584(7) 0.88689(4) -0.09573(11) 0.0267(4) Uani 1 1 d . . . S11 S 0.10518(7) 0.81326(4) 0.06670(12) 0.0274(4) Uani 1 1 d . . . S12 S 0.05902(7) 0.90917(5) 0.09150(12) 0.0316(4) Uani 1 1 d . . . C19 C 0.1871(3) 0.75137(17) -0.1583(4) 0.0283(16) Uani 1 1 d . . . H19 H 0.2101 0.7321 -0.1750 0.034 Uiso 1 1 calc R . . C20 C 0.1267(3) 0.75657(17) -0.1959(4) 0.0294(16) Uani 1 1 d . . . H20 H 0.1001 0.7422 -0.2434 0.035 Uiso 1 1 calc R . . C21 C 0.1131(3) 0.78732(16) -0.1490(4) 0.0254(15) Uani 1 1 d . . . H21 H 0.0743 0.7976 -0.1595 0.030 Uiso 1 1 calc R . . C22 C 0.3297(3) 0.84512(19) -0.0757(5) 0.0309(16) Uani 1 1 d . . . H22 H 0.3610 0.8313 -0.0879 0.037 Uiso 1 1 calc R . . C23 C 0.3212(3) 0.88433(18) -0.0833(5) 0.0327(16) Uani 1 1 d . . . H23 H 0.3444 0.9029 -0.1022 0.039 Uiso 1 1 calc R . . C24 C 0.2707(3) 0.89110(17) -0.0569(4) 0.0247(14) Uani 1 1 d . . . H24 H 0.2539 0.9159 -0.0545 0.030 Uiso 1 1 calc R . . C25 C 0.3080(3) 0.75746(17) 0.1280(5) 0.0326(17) Uani 1 1 d . . . H25 H 0.3357 0.7388 0.1210 0.039 Uiso 1 1 calc R . . C26 C 0.2948(3) 0.76468(18) 0.2054(5) 0.0351(17) Uani 1 1 d . . . H26 H 0.3108 0.7521 0.2616 0.042 Uiso 1 1 calc R . . C27 C 0.2531(3) 0.79418(18) 0.1844(5) 0.0313(16) Uani 1 1 d . . . H27 H 0.2356 0.8056 0.2253 0.038 Uiso 1 1 calc R . . B3 B 0.2722(3) 0.7862(2) -0.0342(6) 0.0261(17) Uani 1 1 d . . . H3A H 0.307(3) 0.7663(16) -0.048(4) 0.033(18) Uiso 1 1 d . . . N31 N 0.1473(3) 0.85510(19) 0.2819(4) 0.0456(17) Uani 1 1 d . . . N32 N 0.1531(3) 0.8783(2) 0.3392(5) 0.0454(17) Uani 1 1 d . . . N33 N 0.1575(4) 0.8997(2) 0.3982(5) 0.081(3) Uani 1 1 d . . . N34 N 0.1487(3) 0.97630(15) 0.0235(4) 0.0435(17) Uani 1 1 d . . . N35 N 0.1892(3) 0.99302(17) 0.0129(4) 0.0416(16) Uani 1 1 d . . . N36 N 0.2262(3) 1.0126(2) 0.0023(6) 0.084(3) Uani 1 1 d . . . N37 N -0.0205(3) 0.85220(19) -0.1055(5) 0.0436(16) Uani 1 1 d . . . N38 N -0.0288(3) 0.85176(18) -0.1815(5) 0.0459(17) Uani 1 1 d . . . N39 N -0.0389(4) 0.8503(3) -0.2591(6) 0.095(3) Uani 1 1 d . . . N41 N 0.1618(2) 0.80054(13) -0.0874(4) 0.0246(12) Uani 1 1 d . . . N42 N 0.2862(2) 0.82924(14) -0.0480(4) 0.0265(12) Uani 1 1 d . . . N43 N 0.2496(2) 0.85776(13) -0.0356(3) 0.0211(11) Uani 1 1 d . . . N44 N 0.2751(2) 0.78130(14) 0.0637(4) 0.0248(12) Uani 1 1 d . . . N45 N 0.2409(2) 0.80431(14) 0.0985(4) 0.0256(12) Uani 1 1 d . . . N46 N 0.0012(2) 0.00470(14) 0.2509(4) 0.0313(14) Uani 1 1 d . . . C28 C -0.0647(3) -0.0029(2) 0.2030(5) 0.0432(19) Uani 1 1 d . . . H28A H -0.0857 -0.0039 0.2484 0.052 Uiso 1 1 calc R . . H28B H -0.0812 0.0191 0.1626 0.052 Uiso 1 1 calc R . . C29 C -0.0778(4) -0.0398(2) 0.1486(6) 0.066(3) Uani 1 1 d . . . H29A H -0.0602 -0.0383 0.0999 0.099 Uiso 1 1 calc R . . H29B H -0.1210 -0.0432 0.1232 0.099 Uiso 1 1 calc R . . H29C H -0.0608 -0.0619 0.1874 0.099 Uiso 1 1 calc R . . C30 C 0.0285(3) -0.0278(2) 0.3167(5) 0.045(2) Uani 1 1 d . . . H30A H 0.0258 -0.0522 0.2826 0.054 Uiso 1 1 calc R . . H30B H 0.0712 -0.0221 0.3457 0.054 Uiso 1 1 calc R . . C31 C -0.0001(4) -0.0341(3) 0.3891(6) 0.064(3) Uani 1 1 d . . . H31A H 0.0014 -0.0100 0.4227 0.096 Uiso 1 1 calc R . . H31B H 0.0214 -0.0545 0.4300 0.096 Uiso 1 1 calc R . . H31C H -0.0416 -0.0420 0.3616 0.096 Uiso 1 1 calc R . . C32 C 0.0053(4) 0.0432(2) 0.2973(6) 0.067(3) Uani 1 1 d . . . H32A H -0.0186 0.0420 0.3389 0.080 Uiso 1 1 calc R . . H32B H -0.0126 0.0633 0.2517 0.080 Uiso 1 1 calc R . . C33 C 0.0678(5) 0.0555(3) 0.3495(7) 0.097(4) Uani 1 1 d . . . H33A H 0.0879 0.0344 0.3892 0.146 Uiso 1 1 calc R . . H33B H 0.0664 0.0785 0.3854 0.146 Uiso 1 1 calc R . . H33C H 0.0898 0.0616 0.3077 0.146 Uiso 1 1 calc R . . C34 C 0.0360(3) 0.00508(19) 0.1847(5) 0.0375(18) Uani 1 1 d . . . H34A H 0.0784 0.0097 0.2183 0.045 Uiso 1 1 calc R . . H34B H 0.0331 -0.0209 0.1571 0.045 Uiso 1 1 calc R . . C35 C 0.0166(4) 0.0346(2) 0.1107(6) 0.059(2) Uani 1 1 d . . . H35A H -0.0249 0.0298 0.0749 0.089 Uiso 1 1 calc R . . H35B H 0.0420 0.0327 0.0721 0.089 Uiso 1 1 calc R . . H35C H 0.0201 0.0606 0.1368 0.089 Uiso 1 1 calc R . . N47 N 0.1902(2) 0.15576(15) 0.0515(4) 0.0304(13) Uani 1 1 d . . . C36 C 0.2321(3) 0.1734(2) 0.0062(5) 0.0425(19) Uani 1 1 d . . . H36A H 0.2166 0.1677 -0.0589 0.051 Uiso 1 1 calc R . . H36B H 0.2714 0.1607 0.0300 0.051 Uiso 1 1 calc R . . C37 C 0.2407(4) 0.2170(2) 0.0185(6) 0.059(2) Uani 1 1 d . . . H37A H 0.2026 0.2301 -0.0094 0.089 Uiso 1 1 calc R . . H37B H 0.2698 0.2257 -0.0099 0.089 Uiso 1 1 calc R . . H37C H 0.2551 0.2231 0.0827 0.089 Uiso 1 1 calc R . . C38 C 0.1288(3) 0.1739(2) 0.0154(5) 0.044(2) Uani 1 1 d . . . H38A H 0.1033 0.1632 0.0490 0.053 Uiso 1 1 calc R . . H38B H 0.1325 0.2021 0.0271 0.053 Uiso 1 1 calc R . . C39 C 0.0983(4) 0.1676(3) -0.0832(6) 0.073(3) Uani 1 1 d . . . H39A H 0.1186 0.1827 -0.1178 0.109 Uiso 1 1 calc R . . H39B H 0.0568 0.1760 -0.0987 0.109 Uiso 1 1 calc R . . H39C H 0.0997 0.1401 -0.0972 0.109 Uiso 1 1 calc R . . C40 C 0.1875(3) 0.11264(19) 0.0314(5) 0.0423(19) Uani 1 1 d . . . H40A H 0.1770 0.1091 -0.0343 0.051 Uiso 1 1 calc R . . H40B H 0.2275 0.1014 0.0592 0.051 Uiso 1 1 calc R . . C41 C 0.1430(4) 0.0902(2) 0.0644(6) 0.056(2) Uani 1 1 d . . . H41A H 0.1518 0.0944 0.1290 0.084 Uiso 1 1 calc R . . H41B H 0.1460 0.0626 0.0526 0.084 Uiso 1 1 calc R . . H41C H 0.1027 0.0993 0.0328 0.084 Uiso 1 1 calc R . . C42 C 0.2124(3) 0.1632(2) 0.1517(5) 0.046(2) Uani 1 1 d . . . H42A H 0.2097 0.1914 0.1618 0.055 Uiso 1 1 calc R . . H42B H 0.1853 0.1500 0.1793 0.055 Uiso 1 1 calc R . . C43 C 0.2752(4) 0.1501(3) 0.1996(6) 0.075(3) Uani 1 1 d . . . H43A H 0.2782 0.1221 0.1922 0.112 Uiso 1 1 calc R . . H43B H 0.2855 0.1563 0.2636 0.112 Uiso 1 1 calc R . . H43C H 0.3028 0.1635 0.1741 0.112 Uiso 1 1 calc R . . N48 N 0.3667(2) 0.46831(13) 0.4195(4) 0.0257(12) Uani 1 1 d . . . C44 C 0.3714(3) 0.49455(18) 0.4995(5) 0.0359(17) Uani 1 1 d . . . H44A H 0.3347 0.4917 0.5164 0.043 Uiso 1 1 calc R . . H44B H 0.3733 0.5218 0.4808 0.043 Uiso 1 1 calc R . . C45 C 0.4249(3) 0.4866(2) 0.5819(5) 0.049(2) Uani 1 1 d . . . H45A H 0.4208 0.4610 0.6062 0.073 Uiso 1 1 calc R . . H45B H 0.4271 0.5064 0.6276 0.073 Uiso 1 1 calc R . . H45C H 0.4614 0.4873 0.5650 0.073 Uiso 1 1 calc R . . C46 C 0.3756(3) 0.42604(17) 0.4483(5) 0.0348(17) Uani 1 1 d . . . H46A H 0.3728 0.4100 0.3949 0.042 Uiso 1 1 calc R . . H46B H 0.4162 0.4229 0.4909 0.042 Uiso 1 1 calc R . . C47 C 0.3313(3) 0.41105(18) 0.4920(5) 0.0405(19) Uani 1 1 d . . . H47A H 0.3298 0.4288 0.5400 0.061 Uiso 1 1 calc R . . H47B H 0.3437 0.3853 0.5173 0.061 Uiso 1 1 calc R . . H47C H 0.2919 0.4094 0.4471 0.061 Uiso 1 1 calc R . . C48 C 0.3054(3) 0.47260(17) 0.3514(5) 0.0320(16) Uani 1 1 d . . . H48A H 0.2753 0.4651 0.3802 0.038 Uiso 1 1 calc R . . H48B H 0.3019 0.4542 0.3016 0.038 Uiso 1 1 calc R . . C49 C 0.2906(3) 0.5129(2) 0.3123(5) 0.049(2) Uani 1 1 d . . . H49A H 0.2888 0.5309 0.3597 0.074 Uiso 1 1 calc R . . H49B H 0.2519 0.5125 0.2650 0.074 Uiso 1 1 calc R . . H49C H 0.3214 0.5214 0.2868 0.074 Uiso 1 1 calc R . . C50 C 0.4148(3) 0.47988(19) 0.3790(5) 0.0378(18) Uani 1 1 d . . . H50A H 0.4123 0.5082 0.3686 0.045 Uiso 1 1 calc R . . H50B H 0.4541 0.4745 0.4238 0.045 Uiso 1 1 calc R . . C51 C 0.4128(4) 0.4602(2) 0.2921(5) 0.052(2) Uani 1 1 d . . . H51A H 0.4130 0.4320 0.3001 0.078 Uiso 1 1 calc R . . H51B H 0.4476 0.4679 0.2750 0.078 Uiso 1 1 calc R . . H51C H 0.3764 0.4679 0.2448 0.078 Uiso 1 1 calc R . . N49 N 0.1474(2) 0.64886(14) 0.1250(4) 0.0263(12) Uani 1 1 d . . . C52 C 0.1624(3) 0.60667(17) 0.1151(5) 0.0358(17) Uani 1 1 d . . . H52A H 0.1308 0.5953 0.0640 0.043 Uiso 1 1 calc R . . H52B H 0.2001 0.6055 0.1002 0.043 Uiso 1 1 calc R . . C53 C 0.1691(4) 0.5821(2) 0.1976(6) 0.065(3) Uani 1 1 d . . . H53A H 0.2022 0.5920 0.2477 0.097 Uiso 1 1 calc R . . H53B H 0.1772 0.5552 0.1851 0.097 Uiso 1 1 calc R . . H53C H 0.1322 0.5832 0.2134 0.097 Uiso 1 1 calc R . . C54 C 0.0889(3) 0.6534(2) 0.1438(5) 0.0424(19) Uani 1 1 d . . . H54A H 0.0823 0.6813 0.1517 0.051 Uiso 1 1 calc R . . H54B H 0.0922 0.6403 0.2012 0.051 Uiso 1 1 calc R . . C55 C 0.0348(3) 0.6375(3) 0.0723(6) 0.068(3) Uani 1 1 d . . . H55A H 0.0303 0.6506 0.0152 0.102 Uiso 1 1 calc R . . H55B H -0.0008 0.6420 0.0902 0.102 Uiso 1 1 calc R . . H55C H 0.0399 0.6096 0.0653 0.102 Uiso 1 1 calc R . . C56 C 0.1460(3) 0.66878(19) 0.0382(5) 0.0375(18) Uani 1 1 d . . . H56A H 0.1145 0.6566 -0.0117 0.045 Uiso 1 1 calc R . . H56B H 0.1845 0.6641 0.0276 0.045 Uiso 1 1 calc R . . C57 C 0.1347(4) 0.71237(19) 0.0353(6) 0.055(2) Uani 1 1 d . . . H57A H 0.0976 0.7175 0.0484 0.082 Uiso 1 1 calc R . . H57B H 0.1316 0.7223 -0.0245 0.082 Uiso 1 1 calc R . . H57C H 0.1678 0.7252 0.0802 0.082 Uiso 1 1 calc R . . C58 C 0.1946(3) 0.66710(18) 0.2040(4) 0.0316(16) Uani 1 1 d . . . H58A H 0.1844 0.6947 0.2081 0.038 Uiso 1 1 calc R . . H58B H 0.1937 0.6542 0.2598 0.038 Uiso 1 1 calc R . . C59 C 0.2570(3) 0.6647(2) 0.1985(5) 0.048(2) Uani 1 1 d . . . H59A H 0.2687 0.6375 0.1989 0.072 Uiso 1 1 calc R . . H59B H 0.2844 0.6780 0.2502 0.072 Uiso 1 1 calc R . . H59C H 0.2584 0.6770 0.1430 0.072 Uiso 1 1 calc R . . N50 N 0.4444(2) 0.85246(14) 0.2519(4) 0.0309(13) Uani 1 1 d . . . C60 C 0.3975(3) 0.8658(2) 0.1655(4) 0.0378(18) Uani 1 1 d . . . H60A H 0.4118 0.8596 0.1142 0.045 Uiso 1 1 calc R . . H60B H 0.3606 0.8509 0.1578 0.045 Uiso 1 1 calc R . . C61 C 0.3827(3) 0.9087(2) 0.1620(5) 0.050(2) Uani 1 1 d . . . H61A H 0.3680 0.9152 0.2120 0.075 Uiso 1 1 calc R . . H61B H 0.3519 0.9146 0.1051 0.075 Uiso 1 1 calc R . . H61C H 0.4185 0.9238 0.1665 0.075 Uiso 1 1 calc R . . C62 C 0.4480(3) 0.80867(18) 0.2516(5) 0.0426(19) Uani 1 1 d . . . H62A H 0.4759 0.8002 0.3099 0.051 Uiso 1 1 calc R . . H62B H 0.4083 0.7981 0.2472 0.051 Uiso 1 1 calc R . . C63 C 0.4678(4) 0.7910(2) 0.1776(6) 0.056(2) Uani 1 1 d . . . H63A H 0.4386 0.7971 0.1194 0.083 Uiso 1 1 calc R . . H63B H 0.4709 0.7629 0.1854 0.083 Uiso 1 1 calc R . . H63C H 0.5066 0.8016 0.1800 0.083 Uiso 1 1 calc R . . C64 C 0.5035(3) 0.87096(19) 0.2565(5) 0.0351(17) Uani 1 1 d . . . H64A H 0.5133 0.8639 0.2016 0.042 Uiso 1 1 calc R . . H64B H 0.4989 0.8994 0.2566 0.042 Uiso 1 1 calc R . . C65 C 0.5551(3) 0.8596(2) 0.3372(6) 0.060(2) Uani 1 1 d . . . H65A H 0.5467 0.8672 0.3921 0.089 Uiso 1 1 calc R . . H65B H 0.5913 0.8727 0.3348 0.089 Uiso 1 1 calc R . . H65C H 0.5609 0.8315 0.3372 0.089 Uiso 1 1 calc R . . C66 C 0.4279(3) 0.86541(18) 0.3336(4) 0.0293(15) Uani 1 1 d . . . H66A H 0.4562 0.8534 0.3875 0.035 Uiso 1 1 calc R . . H66B H 0.4335 0.8938 0.3399 0.035 Uiso 1 1 calc R . . C67 C 0.3651(3) 0.8560(2) 0.3330(5) 0.0415(19) Uani 1 1 d . . . H67A H 0.3365 0.8693 0.2827 0.062 Uiso 1 1 calc R . . H67B H 0.3598 0.8645 0.3895 0.062 Uiso 1 1 calc R . . H67C H 0.3586 0.8280 0.3264 0.062 Uiso 1 1 calc R . . N51 N 0.2990(2) 0.98843(14) 0.3870(4) 0.0310(14) Uani 1 1 d . . . C68 C 0.2547(3) 0.95775(19) 0.3366(5) 0.0386(18) Uani 1 1 d . . . H68A H 0.2706 0.9451 0.2924 0.046 Uiso 1 1 calc R . . H68B H 0.2513 0.9377 0.3798 0.046 Uiso 1 1 calc R . . C69 C 0.1934(3) 0.9731(2) 0.2881(6) 0.053(2) Uani 1 1 d . . . H69A H 0.1745 0.9819 0.3319 0.079 Uiso 1 1 calc R . . H69B H 0.1693 0.9525 0.2510 0.079 Uiso 1 1 calc R . . H69C H 0.1965 0.9948 0.2497 0.079 Uiso 1 1 calc R . . C70 C 0.2777(3) 1.00746(19) 0.4586(5) 0.0393(18) Uani 1 1 d . . . H70A H 0.2396 1.0208 0.4287 0.047 Uiso 1 1 calc R . . H70B H 0.3070 1.0274 0.4892 0.047 Uiso 1 1 calc R . . C71 C 0.2685(4) 0.9801(2) 0.5295(6) 0.062(2) Uani 1 1 d . . . H71A H 0.2331 0.9642 0.5027 0.093 Uiso 1 1 calc R . . H71B H 0.2631 0.9953 0.5791 0.093 Uiso 1 1 calc R . . H71C H 0.3034 0.9633 0.5522 0.093 Uiso 1 1 calc R . . C72 C 0.3579(3) 0.96797(19) 0.4287(5) 0.0379(18) Uani 1 1 d . . . H72A H 0.3510 0.9455 0.4633 0.045 Uiso 1 1 calc R . . H72B H 0.3719 0.9579 0.3798 0.045 Uiso 1 1 calc R . . C73 C 0.4064(3) 0.9925(2) 0.4897(5) 0.051(2) Uani 1 1 d . . . H73A H 0.4119 1.0158 0.4575 0.077 Uiso 1 1 calc R . . H73B H 0.4436 0.9777 0.5088 0.077 Uiso 1 1 calc R . . H73C H 0.3953 1.0000 0.5425 0.077 Uiso 1 1 calc R . . C74 C 0.3049(4) 1.0204(2) 0.3232(6) 0.049(2) Uani 1 1 d . . . H74A H 0.2674 1.0353 0.3047 0.059 Uiso 1 1 calc R . . H74B H 0.3370 1.0382 0.3567 0.059 Uiso 1 1 calc R . . C75 C 0.3181(4) 1.0075(3) 0.2401(6) 0.068(3) Uani 1 1 d . . . H75A H 0.3547 0.9921 0.2570 0.101 Uiso 1 1 calc R . . H75B H 0.3232 1.0302 0.2059 0.101 Uiso 1 1 calc R . . H75C H 0.2850 0.9917 0.2032 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0214(5) 0.0270(5) 0.0225(5) 0.0005(4) 0.0069(4) -0.0022(4) Fe2 0.0190(5) 0.0262(5) 0.0245(5) 0.0007(4) 0.0020(4) -0.0006(4) Fe3 0.0206(5) 0.0238(4) 0.0256(5) -0.0011(4) 0.0051(4) -0.0001(4) V1 0.0170(5) 0.0228(5) 0.0198(6) -0.0009(5) 0.0044(5) -0.0033(4) S1 0.0197(8) 0.0260(8) 0.0227(9) 0.0019(7) 0.0023(7) -0.0010(6) S2 0.0219(9) 0.0240(8) 0.0284(10) -0.0026(7) 0.0074(7) -0.0005(6) S3 0.0261(9) 0.0307(8) 0.0210(9) -0.0030(7) 0.0059(7) -0.0050(7) S4 0.0224(9) 0.0271(8) 0.0328(10) 0.0008(8) 0.0081(8) -0.0042(6) C1 0.023(4) 0.029(3) 0.041(5) -0.006(3) 0.004(3) -0.007(3) C2 0.036(4) 0.045(4) 0.031(4) -0.006(4) 0.005(4) -0.004(3) C3 0.029(4) 0.039(4) 0.025(4) -0.004(3) 0.007(3) -0.006(3) C4 0.049(5) 0.028(4) 0.030(4) 0.005(3) 0.017(4) -0.001(3) C5 0.052(5) 0.033(4) 0.024(4) 0.007(3) 0.007(4) 0.010(3) C6 0.029(4) 0.036(4) 0.028(4) 0.009(3) 0.002(3) 0.007(3) C7 0.020(4) 0.047(4) 0.038(5) -0.003(4) 0.011(3) -0.010(3) C8 0.027(4) 0.045(4) 0.043(5) -0.003(4) 0.017(4) 0.003(3) C9 0.026(4) 0.036(4) 0.027(4) -0.005(3) 0.005(3) -0.001(3) N1 0.037(4) 0.050(4) 0.026(3) -0.001(3) 0.010(3) -0.004(3) N2 0.035(4) 0.053(4) 0.021(3) -0.009(3) 0.001(3) -0.009(3) N3 0.106(7) 0.061(5) 0.043(5) 0.011(4) 0.009(5) -0.023(4) N4 0.029(3) 0.047(4) 0.024(3) 0.010(3) -0.002(3) 0.009(3) N5 0.054(5) 0.030(3) 0.054(5) -0.006(4) -0.003(4) 0.011(3) N6 0.121(8) 0.065(5) 0.052(6) 0.011(5) 0.005(5) 0.026(5) N7 0.037(4) 0.028(3) 0.045(4) -0.006(3) 0.003(3) 0.006(3) N8 0.041(4) 0.035(4) 0.090(7) -0.023(4) 0.006(4) -0.008(3) N9 0.093(7) 0.051(5) 0.129(9) 0.023(5) -0.011(6) 0.005(5) N10 0.021(3) 0.026(3) 0.030(3) -0.004(3) 0.003(3) -0.009(2) N11 0.018(3) 0.031(3) 0.019(3) -0.003(2) 0.003(2) -0.007(2) N12 0.029(3) 0.023(3) 0.029(3) 0.002(2) 0.009(3) -0.003(2) N13 0.024(3) 0.029(3) 0.032(3) 0.001(3) 0.010(3) -0.006(2) N14 0.024(3) 0.033(3) 0.029(3) -0.005(3) 0.009(3) -0.006(2) N15 0.020(3) 0.029(3) 0.032(3) -0.007(2) 0.011(3) -0.007(2) B1 0.034(5) 0.028(4) 0.037(5) -0.007(4) 0.017(4) -0.015(3) Fe4 0.0225(5) 0.0308(5) 0.0333(6) 0.0042(4) 0.0064(4) -0.0019(4) Fe5 0.0304(6) 0.0229(5) 0.0283(6) 0.0028(4) 0.0057(5) 0.0014(4) Fe6 0.0302(6) 0.0298(5) 0.0271(6) 0.0044(4) 0.0118(5) -0.0011(4) V2 0.0178(6) 0.0200(5) 0.0216(6) 0.0014(5) 0.0055(5) 0.0002(4) S5 0.0252(9) 0.0268(8) 0.0354(11) 0.0030(8) 0.0137(8) 0.0041(7) S6 0.0267(9) 0.0271(8) 0.0234(9) -0.0005(7) 0.0033(7) -0.0029(7) S7 0.0245(9) 0.0271(8) 0.0228(9) 0.0032(7) 0.0019(7) 0.0009(7) S8 0.0390(11) 0.0358(10) 0.0426(12) 0.0069(9) 0.0123(9) -0.0111(8) C10 0.019(4) 0.051(4) 0.028(4) -0.001(3) 0.008(3) -0.006(3) C11 0.018(4) 0.056(5) 0.031(4) -0.008(4) 0.005(3) 0.006(3) C12 0.026(4) 0.030(4) 0.039(4) 0.002(3) 0.009(3) 0.010(3) C13 0.027(4) 0.031(4) 0.050(5) -0.008(4) 0.002(4) -0.017(3) C14 0.044(5) 0.045(4) 0.043(5) -0.018(4) 0.008(4) -0.016(4) C15 0.038(4) 0.044(4) 0.019(4) -0.010(3) 0.007(3) -0.006(3) C16 0.042(5) 0.028(3) 0.028(4) 0.011(3) 0.012(4) 0.007(3) C17 0.042(5) 0.034(4) 0.023(4) 0.009(3) 0.006(3) 0.016(3) C18 0.027(4) 0.029(3) 0.029(4) -0.003(3) 0.008(3) 0.003(3) N16 0.024(3) 0.048(4) 0.048(4) 0.002(3) 0.001(3) 0.002(3) N17 0.021(3) 0.049(4) 0.061(5) -0.010(4) 0.014(3) -0.002(3) N18 0.043(5) 0.057(5) 0.082(6) 0.012(4) 0.004(4) 0.009(3) N19 0.054(4) 0.035(4) 0.053(5) -0.007(3) 0.006(4) 0.008(3) N20 0.039(4) 0.043(4) 0.040(4) 0.006(3) 0.008(3) 0.014(3) N21 0.080(6) 0.034(4) 0.095(7) 0.011(4) 0.040(5) 0.012(3) N22 0.050(4) 0.058(4) 0.035(4) -0.001(3) 0.022(3) -0.007(3) N23 0.030(4) 0.071(5) 0.036(4) 0.008(4) 0.013(3) 0.011(3) N24 0.058(5) 0.109(6) 0.059(5) 0.044(5) 0.029(4) 0.033(4) N25 0.018(3) 0.037(3) 0.028(3) 0.002(3) 0.008(2) -0.002(2) N26 0.019(3) 0.028(3) 0.025(3) 0.004(2) 0.007(2) 0.000(2) N27 0.024(3) 0.026(3) 0.035(4) 0.000(3) 0.009(3) -0.006(2) N28 0.024(3) 0.028(3) 0.028(3) 0.000(2) 0.010(3) -0.003(2) N29 0.028(3) 0.026(3) 0.031(3) 0.004(3) 0.011(3) 0.000(2) N30 0.023(3) 0.020(3) 0.028(3) 0.000(2) 0.009(3) -0.002(2) N40 0.031(3) 0.021(3) 0.031(3) -0.001(2) 0.015(3) 0.004(2) B2 0.030(5) 0.028(4) 0.041(5) 0.004(4) 0.014(4) -0.007(3) Fe7 0.0265(5) 0.0279(5) 0.0242(5) -0.0001(4) 0.0091(4) 0.0028(4) Fe8 0.0257(5) 0.0213(4) 0.0295(6) 0.0003(4) 0.0059(4) 0.0014(4) Fe9 0.0202(5) 0.0277(5) 0.0314(6) -0.0034(4) 0.0063(4) 0.0006(4) V3 0.0170(6) 0.0193(5) 0.0211(6) 0.0001(5) 0.0048(5) 0.0007(4) S9 0.0238(9) 0.0256(8) 0.0231(9) -0.0030(7) 0.0036(7) -0.0018(6) S10 0.0239(9) 0.0282(8) 0.0254(9) 0.0028(7) 0.0038(7) 0.0019(7) S11 0.0255(9) 0.0219(8) 0.0382(11) -0.0022(7) 0.0149(8) -0.0036(6) S12 0.0285(10) 0.0312(9) 0.0372(11) -0.0044(8) 0.0133(8) 0.0072(7) C19 0.041(4) 0.022(3) 0.027(4) -0.005(3) 0.018(3) -0.004(3) C20 0.039(4) 0.027(3) 0.019(4) -0.003(3) 0.006(3) -0.007(3) C21 0.020(3) 0.026(3) 0.027(4) 0.002(3) 0.002(3) -0.005(3) C22 0.019(4) 0.041(4) 0.035(4) -0.003(3) 0.012(3) -0.003(3) C23 0.028(4) 0.035(4) 0.038(5) 0.001(3) 0.015(3) -0.007(3) C24 0.017(3) 0.027(3) 0.025(4) -0.002(3) -0.001(3) -0.002(3) C25 0.023(4) 0.024(3) 0.043(5) 0.005(3) -0.001(3) 0.006(3) C26 0.037(4) 0.034(4) 0.027(4) 0.009(3) 0.000(3) 0.005(3) C27 0.032(4) 0.031(4) 0.030(4) 0.002(3) 0.008(3) -0.001(3) B3 0.019(4) 0.022(4) 0.038(5) 0.003(3) 0.010(4) 0.005(3) N31 0.049(4) 0.060(4) 0.028(4) 0.008(3) 0.012(3) 0.006(3) N32 0.036(4) 0.070(5) 0.028(4) 0.012(4) 0.007(3) -0.013(3) N33 0.122(8) 0.087(6) 0.038(5) -0.007(4) 0.030(5) -0.046(5) N34 0.042(4) 0.026(3) 0.061(5) 0.004(3) 0.013(4) 0.001(3) N35 0.035(4) 0.039(4) 0.049(4) 0.007(3) 0.010(3) 0.003(3) N36 0.045(5) 0.089(6) 0.125(8) 0.032(6) 0.036(5) -0.008(4) N37 0.022(3) 0.068(4) 0.038(4) -0.011(4) 0.006(3) -0.009(3) N38 0.040(4) 0.044(4) 0.046(5) -0.005(4) 0.002(4) -0.014(3) N39 0.099(7) 0.122(8) 0.052(6) -0.014(6) 0.009(5) -0.050(6) N41 0.024(3) 0.022(3) 0.028(3) 0.000(2) 0.007(3) -0.001(2) N42 0.019(3) 0.032(3) 0.030(3) -0.002(3) 0.009(2) 0.001(2) N43 0.018(3) 0.025(3) 0.020(3) 0.001(2) 0.006(2) -0.001(2) N44 0.020(3) 0.025(3) 0.027(3) 0.000(2) 0.004(2) 0.004(2) N45 0.024(3) 0.026(3) 0.029(3) 0.000(2) 0.011(3) 0.000(2) N46 0.026(3) 0.032(3) 0.032(4) -0.007(3) 0.003(3) 0.004(2) C28 0.026(4) 0.068(5) 0.029(4) 0.005(4) -0.002(3) -0.001(4) C29 0.067(6) 0.060(5) 0.048(6) 0.008(5) -0.016(5) -0.030(4) C30 0.035(4) 0.054(5) 0.035(5) 0.005(4) -0.006(4) 0.003(4) C31 0.063(6) 0.083(7) 0.039(5) 0.003(5) 0.007(5) -0.015(5) C32 0.091(8) 0.048(5) 0.062(6) -0.031(5) 0.024(6) 0.007(5) C33 0.111(10) 0.068(7) 0.086(9) -0.041(6) -0.008(7) -0.031(6) C34 0.033(4) 0.038(4) 0.041(5) -0.002(4) 0.011(4) 0.003(3) C35 0.056(6) 0.065(6) 0.056(6) 0.023(5) 0.017(5) 0.006(4) N47 0.033(3) 0.037(3) 0.020(3) -0.003(3) 0.006(3) 0.008(2) C36 0.047(5) 0.046(4) 0.036(5) -0.009(4) 0.017(4) -0.002(4) C37 0.076(7) 0.046(5) 0.055(6) 0.000(4) 0.022(5) -0.012(4) C38 0.027(4) 0.051(5) 0.046(5) -0.013(4) 0.001(4) 0.012(3) C39 0.057(6) 0.084(7) 0.054(6) -0.009(5) -0.016(5) 0.018(5) C40 0.044(5) 0.037(4) 0.044(5) -0.004(4) 0.012(4) 0.005(3) C41 0.068(6) 0.051(5) 0.056(6) -0.010(4) 0.028(5) -0.015(4) C42 0.055(5) 0.061(5) 0.016(4) -0.004(4) 0.005(4) -0.006(4) C43 0.066(7) 0.092(7) 0.046(6) 0.011(5) -0.010(5) 0.005(5) N48 0.020(3) 0.023(3) 0.032(3) 0.000(2) 0.006(3) -0.003(2) C44 0.042(5) 0.031(4) 0.031(4) -0.006(3) 0.008(4) -0.004(3) C45 0.047(5) 0.046(5) 0.041(5) -0.003(4) -0.003(4) -0.012(4) C46 0.036(4) 0.020(3) 0.047(5) -0.002(3) 0.011(4) -0.002(3) C47 0.037(4) 0.029(4) 0.051(5) 0.001(4) 0.007(4) -0.014(3) C48 0.022(4) 0.031(4) 0.039(4) -0.007(3) 0.003(3) -0.003(3) C49 0.035(5) 0.047(5) 0.054(6) 0.009(4) -0.004(4) 0.003(3) C50 0.028(4) 0.039(4) 0.045(5) 0.006(4) 0.009(4) -0.007(3) C51 0.050(5) 0.067(5) 0.052(6) -0.009(5) 0.033(4) -0.010(4) N49 0.028(3) 0.024(3) 0.024(3) -0.007(2) 0.005(3) 0.000(2) C52 0.046(5) 0.026(3) 0.029(4) -0.003(3) 0.003(4) 0.000(3) C53 0.093(7) 0.035(5) 0.058(6) 0.010(4) 0.012(5) 0.003(4) C54 0.033(4) 0.050(4) 0.044(5) 0.000(4) 0.010(4) 0.004(3) C55 0.038(5) 0.082(6) 0.083(8) -0.014(6) 0.017(5) -0.011(4) C56 0.044(5) 0.044(4) 0.023(4) 0.005(3) 0.008(4) 0.003(3) C57 0.071(6) 0.036(4) 0.053(6) 0.017(4) 0.013(5) 0.006(4) C58 0.039(4) 0.028(3) 0.023(4) -0.005(3) 0.005(3) -0.004(3) C59 0.041(5) 0.051(5) 0.047(5) -0.007(4) 0.006(4) -0.005(4) N50 0.032(3) 0.028(3) 0.030(3) -0.007(3) 0.006(3) -0.006(2) C60 0.039(4) 0.053(5) 0.015(4) -0.004(3) 0.000(3) -0.001(3) C61 0.058(6) 0.055(5) 0.031(5) 0.014(4) 0.006(4) 0.008(4) C62 0.053(5) 0.030(4) 0.046(5) -0.001(4) 0.018(4) -0.002(3) C63 0.071(6) 0.038(4) 0.063(6) -0.016(4) 0.029(5) 0.006(4) C64 0.033(4) 0.036(4) 0.036(4) 0.000(3) 0.010(4) 0.001(3) C65 0.035(5) 0.078(6) 0.068(7) -0.008(5) 0.019(5) -0.008(4) C66 0.033(4) 0.032(4) 0.022(4) -0.005(3) 0.006(3) -0.003(3) C67 0.042(5) 0.044(4) 0.044(5) -0.003(4) 0.022(4) -0.007(3) N51 0.026(3) 0.027(3) 0.032(4) -0.004(3) -0.002(3) 0.001(2) C68 0.033(4) 0.040(4) 0.039(5) -0.014(4) 0.007(4) -0.005(3) C69 0.029(5) 0.061(5) 0.058(6) -0.007(5) -0.002(4) -0.001(4) C70 0.041(5) 0.032(4) 0.043(5) -0.010(4) 0.010(4) 0.004(3) C71 0.079(7) 0.066(6) 0.053(6) -0.009(5) 0.036(5) -0.002(5) C72 0.033(4) 0.038(4) 0.041(5) 0.010(4) 0.010(4) 0.011(3) C73 0.037(5) 0.055(5) 0.047(5) 0.007(4) -0.008(4) -0.008(4) C74 0.051(5) 0.037(4) 0.052(6) 0.012(4) 0.007(4) -0.003(4) C75 0.061(6) 0.090(7) 0.054(6) 0.020(5) 0.021(5) -0.004(5) _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 Fe1 N1 1.963(6) . ? Fe1 S2 2.2528(19) . ? Fe1 S1 2.2692(19) . ? Fe1 S4 2.3076(19) . ? Fe2 N4 1.959(6) . ? Fe2 S2 2.2669(19) . ? Fe2 S4 2.2750(19) . ? Fe2 S3 2.290(2) . ? Fe3 N7 1.989(5) . ? Fe3 S1 2.2538(18) . ? Fe3 S3 2.2593(19) . ? Fe3 S4 2.326(2) . ? V1 N15 2.170(5) . ? V1 N13 2.187(5) . ? V1 N11 2.203(5) . ? V1 S1 2.3316(19) . ? V1 S2 2.351(2) . ? V1 S3 2.3655(19) . ? C1 N10 1.336(8) . ? C1 C2 1.377(9) . ? C2 C3 1.394(9) . ? C3 N11 1.327(8) . ? C4 C5 1.355(9) . ? C4 N12 1.360(8) . ? C5 C6 1.399(9) . ? C6 N13 1.341(8) . ? C7 N14 1.345(8) . ? C7 C8 1.368(9) . ? C8 C9 1.390(9) . ? C9 N15 1.343(8) . ? N1 N2 1.172(8) . ? N2 N3 1.164(8) . ? N4 N5 1.163(9) . ? N5 N6 1.178(10) . ? N7 N8 1.181(9) . ? N8 N9 1.185(10) . ? N10 N11 1.370(6) . ? N10 B1 1.520(10) . ? N12 N13 1.365(7) . ? N12 B1 1.522(10) . ? N14 N15 1.363(6) . ? N14 B1 1.555(9) . ? Fe4 N16 1.974(6) . ? Fe4 S6 2.262(2) . ? Fe4 S8 2.273(2) . ? Fe4 S5 2.283(2) . ? Fe5 N19 1.963(6) . ? Fe5 S6 2.260(2) . ? Fe5 S7 2.2604(19) . ? Fe5 S8 2.305(2) . ? Fe6 N22 1.979(6) . ? Fe6 S5 2.2634(19) . ? Fe6 S7 2.271(2) . ? Fe6 S8 2.323(2) . ? V2 N26 2.178(5) . ? V2 N28 2.179(5) . ? V2 N30 2.207(5) . ? V2 S6 2.340(2) . ? V2 S7 2.3416(19) . ? V2 S5 2.363(2) . ? C10 N25 1.355(8) . ? C10 C11 1.369(9) . ? C11 C12 1.382(9) . ? C12 N26 1.334(7) . ? C13 N27 1.356(8) . ? C13 C14 1.367(10) . ? C14 C15 1.385(9) . ? C15 N28 1.328(8) . ? C16 N29 1.348(8) . ? C16 C17 1.370(9) . ? C17 C18 1.394(9) . ? C18 N30 1.336(7) . ? N16 N17 1.162(8) . ? N17 N18 1.160(8) . ? N19 N20 1.153(8) . ? N20 N21 1.155(8) . ? N22 N23 1.179(8) . ? N23 N24 1.172(9) . ? N25 N26 1.366(7) . ? N25 B2 1.538(9) . ? N27 N28 1.368(7) . ? N27 B2 1.531(10) . ? N29 N30 1.372(7) . ? N29 B2 1.534(9) . ? N40 C19 1.346(7) . ? N40 N41 1.371(7) . ? N40 B3 1.537(9) . ? Fe7 N31 1.947(6) . ? Fe7 S11 2.2572(19) . ? Fe7 S12 2.2759(19) . ? Fe7 S9 2.2849(19) . ? Fe8 N34 1.972(6) . ? Fe8 S9 2.2543(19) . ? Fe8 S10 2.270(2) . ? Fe8 S12 2.331(2) . ? Fe9 N37 1.976(6) . ? Fe9 S11 2.2555(19) . ? Fe9 S12 2.288(2) . ? Fe9 S10 2.291(2) . ? V3 N43 2.184(5) . ? V3 N41 2.200(5) . ? V3 N45 2.203(5) . ? V3 S11 2.3494(19) . ? V3 S9 2.3512(19) . ? V3 S10 2.3543(19) . ? C19 C20 1.377(9) . ? C20 C21 1.385(8) . ? C21 N41 1.331(7) . ? C22 N42 1.354(8) . ? C22 C23 1.369(8) . ? C23 C24 1.400(8) . ? C24 N43 1.340(7) . ? C25 N44 1.346(8) . ? C25 C26 1.369(10) . ? C26 C27 1.385(9) . ? C27 N45 1.334(8) . ? B3 N44 1.526(9) . ? B3 N42 1.554(8) . ? N31 N32 1.181(8) . ? N32 N33 1.162(9) . ? N34 N35 1.173(8) . ? N35 N36 1.159(8) . ? N37 N38 1.147(9) . ? N38 N39 1.167(10) . ? N42 N43 1.366(6) . ? N44 N45 1.366(7) . ? N46 C32 1.507(8) . ? N46 C34 1.515(9) . ? N46 C30 1.526(8) . ? N46 C28 1.528(8) . ? C28 C29 1.511(10) . ? C30 C31 1.510(11) . ? C32 C33 1.510(11) . ? C34 C35 1.506(9) . ? N47 C42 1.516(8) . ? N47 C36 1.518(9) . ? N47 C40 1.520(8) . ? N47 C38 1.520(8) . ? C36 C37 1.523(9) . ? C38 C39 1.504(10) . ? C40 C41 1.522(10) . ? C42 C43 1.511(10) . ? N48 C48 1.516(8) . ? N48 C50 1.522(8) . ? N48 C44 1.524(8) . ? N48 C46 1.524(7) . ? C44 C45 1.526(9) . ? C46 C47 1.513(9) . ? C48 C49 1.519(9) . ? C50 C51 1.512(10) . ? N49 C54 1.511(8) . ? N49 C56 1.518(8) . ? N49 C52 1.520(7) . ? N49 C58 1.522(8) . ? C52 C53 1.515(10) . ? C54 C55 1.515(10) . ? C56 C57 1.528(9) . ? C58 C59 1.508(9) . ? N50 C62 1.516(8) . ? N50 C64 1.519(8) . ? N50 C66 1.522(8) . ? N50 C60 1.530(8) . ? C60 C61 1.518(9) . ? C62 C63 1.510(10) . ? C64 C65 1.510(10) . ? C66 C67 1.519(9) . ? N51 C72 1.514(8) . ? N51 C70 1.519(9) . ? N51 C74 1.525(9) . ? N51 C68 1.527(8) . ? C68 C69 1.507(9) . ? C70 C71 1.528(10) . ? C72 C73 1.505(9) . ? C74 C75 1.502(11) . ? 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 Fe1 S2 112.71(18) . . ? N1 Fe1 S1 108.13(18) . . ? S2 Fe1 S1 108.13(7) . . ? N1 Fe1 S4 118.27(18) . . ? S2 Fe1 S4 102.58(7) . . ? S1 Fe1 S4 106.46(7) . . ? N4 Fe2 S2 115.28(18) . . ? N4 Fe2 S4 116.99(18) . . ? S2 Fe2 S4 103.17(7) . . ? N4 Fe2 S3 108.49(19) . . ? S2 Fe2 S3 106.53(7) . . ? S4 Fe2 S3 105.52(7) . . ? N7 Fe3 S1 108.47(18) . . ? N7 Fe3 S3 119.3(2) . . ? S1 Fe3 S3 106.20(7) . . ? N7 Fe3 S4 110.87(19) . . ? S1 Fe3 S4 106.36(7) . . ? S3 Fe3 S4 104.87(7) . . ? N15 V1 N13 80.67(19) . . ? N15 V1 N11 80.47(19) . . ? N13 V1 N11 81.79(19) . . ? N15 V1 S1 86.79(15) . . ? N13 V1 S1 163.65(15) . . ? N11 V1 S1 85.84(14) . . ? N15 V1 S2 164.73(14) . . ? N13 V1 S2 87.49(15) . . ? N11 V1 S2 88.37(14) . . ? S1 V1 S2 102.86(7) . . ? N15 V1 S3 88.13(14) . . ? N13 V1 S3 89.69(15) . . ? N11 V1 S3 166.71(15) . . ? S1 V1 S3 100.41(7) . . ? S2 V1 S3 101.48(7) . . ? Fe3 S1 Fe1 72.14(6) . . ? Fe3 S1 V1 74.65(6) . . ? Fe1 S1 V1 73.10(6) . . ? Fe1 S2 Fe2 74.14(6) . . ? Fe1 S2 V1 73.02(6) . . ? Fe2 S2 V1 74.78(6) . . ? Fe3 S3 Fe2 72.72(6) . . ? Fe3 S3 V1 73.89(6) . . ? Fe2 S3 V1 74.08(6) . . ? Fe2 S4 Fe1 72.95(6) . . ? Fe2 S4 Fe3 71.78(6) . . ? Fe1 S4 Fe3 70.16(6) . . ? N10 C1 C2 108.7(6) . . ? C1 C2 C3 104.8(6) . . ? N11 C3 C2 110.3(6) . . ? C5 C4 N12 108.6(6) . . ? C4 C5 C6 105.9(6) . . ? N13 C6 C5 109.7(6) . . ? N14 C7 C8 108.6(6) . . ? C7 C8 C9 104.8(6) . . ? N15 C9 C8 111.0(6) . . ? N2 N1 Fe1 130.7(5) . . ? N3 N2 N1 177.0(8) . . ? N5 N4 Fe2 130.0(6) . . ? N4 N5 N6 176.7(9) . . ? N8 N7 Fe3 121.8(5) . . ? N7 N8 N9 176.5(9) . . ? C1 N10 N11 109.4(5) . . ? C1 N10 B1 131.5(6) . . ? N11 N10 B1 118.8(5) . . ? C3 N11 N10 106.7(5) . . ? C3 N11 V1 130.4(4) . . ? N10 N11 V1 122.7(4) . . ? C4 N12 N13 109.2(5) . . ? C4 N12 B1 130.3(5) . . ? N13 N12 B1 120.5(5) . . ? C6 N13 N12 106.7(5) . . ? C6 N13 V1 131.3(4) . . ? N12 N13 V1 121.8(4) . . ? C7 N14 N15 110.2(5) . . ? C7 N14 B1 131.4(5) . . ? N15 N14 B1 118.2(5) . . ? C9 N15 N14 105.4(5) . . ? C9 N15 V1 130.6(4) . . ? N14 N15 V1 123.8(4) . . ? N10 B1 N12 108.9(6) . . ? N10 B1 N14 107.8(6) . . ? N12 B1 N14 108.4(5) . . ? N16 Fe4 S6 107.8(2) . . ? N16 Fe4 S8 117.1(2) . . ? S6 Fe4 S8 104.34(8) . . ? N16 Fe4 S5 115.26(19) . . ? S6 Fe4 S5 106.18(7) . . ? S8 Fe4 S5 105.08(8) . . ? N19 Fe5 S6 112.7(2) . . ? N19 Fe5 S7 108.07(19) . . ? S6 Fe5 S7 107.19(7) . . ? N19 Fe5 S8 118.5(2) . . ? S6 Fe5 S8 103.37(8) . . ? S7 Fe5 S8 106.38(8) . . ? N22 Fe6 S5 115.9(2) . . ? N22 Fe6 S7 112.26(19) . . ? S5 Fe6 S7 107.69(7) . . ? N22 Fe6 S8 110.62(19) . . ? S5 Fe6 S8 104.11(8) . . ? S7 Fe6 S8 105.43(7) . . ? N26 V2 N28 81.73(19) . . ? N26 V2 N30 81.45(18) . . ? N28 V2 N30 81.28(19) . . ? N26 V2 S6 85.33(14) . . ? N28 V2 S6 164.93(15) . . ? N30 V2 S6 89.21(14) . . ? N26 V2 S7 87.89(14) . . ? N28 V2 S7 85.25(15) . . ? N30 V2 S7 163.86(14) . . ? S6 V2 S7 102.02(7) . . ? N26 V2 S5 166.41(14) . . ? N28 V2 S5 89.95(14) . . ? N30 V2 S5 86.70(14) . . ? S6 V2 S5 101.20(7) . . ? S7 V2 S5 102.19(7) . . ? Fe6 S5 Fe4 72.98(6) . . ? Fe6 S5 V2 73.04(6) . . ? Fe4 S5 V2 74.11(6) . . ? Fe5 S6 Fe4 73.69(7) . . ? Fe5 S6 V2 73.62(7) . . ? Fe4 S6 V2 74.95(7) . . ? Fe5 S7 Fe6 72.31(6) . . ? Fe5 S7 V2 73.59(6) . . ? Fe6 S7 V2 73.31(6) . . ? Fe4 S8 Fe5 72.65(6) . . ? Fe4 S8 Fe6 72.07(6) . . ? Fe5 S8 Fe6 70.59(6) . . ? N25 C10 C11 108.5(6) . . ? C10 C11 C12 105.0(6) . . ? N26 C12 C11 111.1(6) . . ? N27 C13 C14 108.1(6) . . ? C13 C14 C15 105.9(7) . . ? N28 C15 C14 110.0(7) . . ? N29 C16 C17 108.5(6) . . ? C16 C17 C18 105.0(6) . . ? N30 C18 C17 110.9(6) . . ? N17 N16 Fe4 125.5(5) . . ? N18 N17 N16 176.1(8) . . ? N20 N19 Fe5 140.6(6) . . ? N19 N20 N21 175.0(8) . . ? N23 N22 Fe6 125.5(5) . . ? N24 N23 N22 178.0(8) . . ? C10 N25 N26 109.3(5) . . ? C10 N25 B2 130.9(6) . . ? N26 N25 B2 119.7(5) . . ? C12 N26 N25 106.1(5) . . ? C12 N26 V2 131.1(4) . . ? N25 N26 V2 122.6(4) . . ? C13 N27 N28 108.8(6) . . ? C13 N27 B2 130.7(6) . . ? N28 N27 B2 120.5(5) . . ? C15 N28 N27 107.2(5) . . ? C15 N28 V2 130.9(4) . . ? N27 N28 V2 122.0(4) . . ? C16 N29 N30 109.9(5) . . ? C16 N29 B2 129.9(6) . . ? N30 N29 B2 120.2(5) . . ? C18 N30 N29 105.8(5) . . ? C18 N30 V2 132.8(4) . . ? N29 N30 V2 121.4(4) . . ? C19 N40 N41 109.1(5) . . ? C19 N40 B3 130.0(5) . . ? N41 N40 B3 120.8(5) . . ? N27 B2 N29 107.1(6) . . ? N27 B2 N25 108.8(6) . . ? N29 B2 N25 107.7(5) . . ? N31 Fe7 S11 113.4(2) . . ? N31 Fe7 S12 116.1(2) . . ? S11 Fe7 S12 103.03(7) . . ? N31 Fe7 S9 110.4(2) . . ? S11 Fe7 S9 107.34(7) . . ? S12 Fe7 S9 105.89(7) . . ? N34 Fe8 S9 114.09(19) . . ? N34 Fe8 S10 114.4(2) . . ? S9 Fe8 S10 106.51(7) . . ? N34 Fe8 S12 109.9(2) . . ? S9 Fe8 S12 105.08(8) . . ? S10 Fe8 S12 106.14(7) . . ? N37 Fe9 S11 116.1(2) . . ? N37 Fe9 S12 117.6(2) . . ? S11 Fe9 S12 102.70(8) . . ? N37 Fe9 S10 105.4(2) . . ? S11 Fe9 S10 107.50(7) . . ? S12 Fe9 S10 106.89(7) . . ? N43 V3 N41 79.30(18) . . ? N43 V3 N45 81.24(18) . . ? N41 V3 N45 83.59(19) . . ? N43 V3 S11 162.46(13) . . ? N41 V3 S11 87.33(14) . . ? N45 V3 S11 86.05(14) . . ? N43 V3 S9 88.90(14) . . ? N41 V3 S9 165.19(15) . . ? N45 V3 S9 85.81(14) . . ? S11 V3 S9 102.24(7) . . ? N43 V3 S10 88.52(14) . . ? N41 V3 S10 87.95(14) . . ? N45 V3 S10 167.76(15) . . ? S11 V3 S10 102.42(7) . . ? S9 V3 S10 100.77(7) . . ? Fe8 S9 Fe7 72.51(6) . . ? Fe8 S9 V3 74.03(6) . . ? Fe7 S9 V3 73.47(6) . . ? Fe8 S10 Fe9 71.58(6) . . ? Fe8 S10 V3 73.69(6) . . ? Fe9 S10 V3 73.01(6) . . ? Fe9 S11 Fe7 73.97(6) . . ? Fe9 S11 V3 73.74(6) . . ? Fe7 S11 V3 74.00(6) . . ? Fe7 S12 Fe9 73.01(6) . . ? Fe7 S12 Fe8 71.27(6) . . ? Fe9 S12 Fe8 70.53(6) . . ? N40 C19 C20 108.8(6) . . ? C19 C20 C21 104.7(6) . . ? N41 C21 C20 111.0(6) . . ? N42 C22 C23 108.8(6) . . ? C22 C23 C24 104.9(5) . . ? N43 C24 C23 110.5(5) . . ? N44 C25 C26 108.4(6) . . ? C25 C26 C27 105.5(6) . . ? N45 C27 C26 110.1(6) . . ? N44 B3 N40 108.5(5) . . ? N44 B3 N42 107.5(5) . . ? N40 B3 N42 107.5(5) . . ? N32 N31 Fe7 126.1(5) . . ? N33 N32 N31 176.2(8) . . ? N35 N34 Fe8 129.4(5) . . ? N36 N35 N34 173.8(8) . . ? N38 N37 Fe9 124.3(6) . . ? N37 N38 N39 177.6(9) . . ? C21 N41 N40 106.4(5) . . ? C21 N41 V3 132.4(4) . . ? N40 N41 V3 121.1(4) . . ? C22 N42 N43 109.6(5) . . ? C22 N42 B3 130.5(5) . . ? N43 N42 B3 119.9(5) . . ? C24 N43 N42 106.3(5) . . ? C24 N43 V3 131.4(4) . . ? N42 N43 V3 122.2(4) . . ? C25 N44 N45 109.3(5) . . ? C25 N44 B3 131.0(6) . . ? N45 N44 B3 119.6(5) . . ? C27 N45 N44 106.6(5) . . ? C27 N45 V3 130.9(4) . . ? N44 N45 V3 122.4(4) . . ? C32 N46 C34 111.0(6) . . ? C32 N46 C30 111.9(6) . . ? C34 N46 C30 105.4(5) . . ? C32 N46 C28 106.9(5) . . ? C34 N46 C28 110.8(5) . . ? C30 N46 C28 110.8(5) . . ? C29 C28 N46 114.8(6) . . ? C31 C30 N46 115.0(6) . . ? N46 C32 C33 114.4(7) . . ? C35 C34 N46 115.8(6) . . ? C42 N47 C36 110.8(5) . . ? C42 N47 C40 111.2(5) . . ? C36 N47 C40 106.7(5) . . ? C42 N47 C38 107.2(5) . . ? C36 N47 C38 110.4(6) . . ? C40 N47 C38 110.7(5) . . ? N47 C36 C37 114.7(6) . . ? C39 C38 N47 114.7(6) . . ? C41 C40 N47 114.6(6) . . ? C43 C42 N47 115.5(7) . . ? C48 N48 C50 110.9(5) . . ? C48 N48 C44 109.2(5) . . ? C50 N48 C44 108.5(5) . . ? C48 N48 C46 108.4(5) . . ? C50 N48 C46 108.9(5) . . ? C44 N48 C46 111.0(5) . . ? N48 C44 C45 114.7(6) . . ? C47 C46 N48 114.3(5) . . ? N48 C48 C49 115.0(5) . . ? C51 C50 N48 116.2(5) . . ? C54 N49 C56 111.4(5) . . ? C54 N49 C52 112.2(5) . . ? C56 N49 C52 106.4(5) . . ? C54 N49 C58 106.4(5) . . ? C56 N49 C58 110.3(5) . . ? C52 N49 C58 110.1(5) . . ? C53 C52 N49 114.5(6) . . ? N49 C54 C55 115.5(6) . . ? N49 C56 C57 115.3(6) . . ? C59 C58 N49 114.4(6) . . ? C62 N50 C64 111.6(5) . . ? C62 N50 C66 109.0(5) . . ? C64 N50 C66 108.2(5) . . ? C62 N50 C60 108.9(5) . . ? C64 N50 C60 108.5(5) . . ? C66 N50 C60 110.6(5) . . ? C61 C60 N50 114.9(5) . . ? C63 C62 N50 115.9(6) . . ? C65 C64 N50 114.9(6) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.072 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.118 data_ortho _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(n-ethylammonium) bis(\m~4~-sulfido)-hexakis(\m~3~-sulfido)-tetrafluoro-bis(hydrotris(pyrazolyl) borato)-hexa-iron-di-vanadium acetonitrile solvate dihydrate ; _chemical_name_common 'Fluoride Vanadium edge bridged double cubane' _chemical_melting_point 'none' _chemical_formula_moiety '(Et4N)4[(C9H10N6B)2V2Fe6S8F4](CH3CN)8(H2O)3' _chemical_formula_sum 'C66 H130 B2 F4 Fe6 N24 O3 S8 V2' _chemical_formula_weight 2098.36 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' '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'V' 'V' 0.3005 0.5294 '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' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pnnm ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, z' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' 'x, y, -z' _cell_length_a 14.743(2) _cell_length_b 29.397(4) _cell_length_c 11.0978(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4809.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4336 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 24.58 _exptl_crystal_description plate _exptl_crystal_colour dark _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 2.539 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _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_% ? _diffrn_reflns_number 26410 _diffrn_reflns_av_R_equivalents 0.1610 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.21 _reflns_number_total 4512 _reflns_number_gt 3178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^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 4512 _refine_ls_number_parameters 336 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 5.650 _refine_ls_shift/su_mean 0.077 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 V1 V 0.09952(8) -0.12975(4) 1.0000 0.0312(3) Uani 1 2 d S . . Fe1 Fe 0.17001(6) -0.05396(2) 1.12053(7) 0.0419(3) Uani 1 1 d . . . Fe2 Fe 0.00923(8) -0.04544(3) 1.0000 0.0352(3) Uani 1 2 d S . . S1 S 0.25101(14) -0.10244(6) 1.0000 0.0426(5) Uani 1 2 d S . . S3 S -0.12807(14) -0.00925(6) 1.0000 0.0418(5) Uani 1 2 d S . . S2 S 0.03597(10) -0.08917(4) 1.16448(12) 0.0397(4) Uani 1 1 d . . . N4 N 0.1428(3) -0.18203(14) 0.8710(4) 0.0378(10) Uani 1 1 d . . . B1 B 0.0734(6) -0.2427(3) 1.0000 0.043(2) Uani 1 2 d S . . F1 F 0.2393(3) -0.03074(13) 1.2500(4) 0.0845(14) Uani 1 1 d . . . N3 N 0.1260(3) -0.22718(14) 0.8885(4) 0.0393(10) Uani 1 1 d . . . N1 N -0.0194(4) -0.21868(18) 1.0000 0.0366(14) Uani 1 2 d S . . N2 N -0.0224(4) -0.17234(19) 1.0000 0.0351(14) Uani 1 2 d S . . N5 N 0.4315(4) 0.7544(2) 1.0000 0.0475(16) Uani 1 2 d SD . . C2 C -0.1638(5) -0.2002(3) 1.0000 0.047(2) Uani 1 2 d S . . H2 H -0.2268 -0.2018 1.0000 0.056 Uiso 1 2 calc SR . . C1 C -0.1036(5) -0.2355(3) 1.0000 0.0451(19) Uani 1 2 d S . . H1 H -0.1187 -0.2662 1.0000 0.054 Uiso 1 2 calc SR . . C3 C -0.1102(5) -0.1615(3) 1.0000 0.0402(17) Uani 1 2 d S . . H3 H -0.1325 -0.1319 1.0000 0.048 Uiso 1 2 calc SR . . C4 C 0.1593(4) -0.25081(19) 0.7936(6) 0.0500(15) Uani 1 1 d . . . H4 H 0.1563 -0.2822 0.7846 0.060 Uiso 1 1 calc R . . C6 C 0.1857(4) -0.1791(2) 0.7662(5) 0.0486(14) Uani 1 1 d . . . H6 H 0.2053 -0.1520 0.7317 0.058 Uiso 1 1 calc R . . C5 C 0.1974(4) -0.2220(2) 0.7142(6) 0.0534(16) Uani 1 1 d . . . H5 H 0.2253 -0.2291 0.6414 0.064 Uiso 1 1 calc R . . C8 C 0.4349(8) 0.8136(3) 0.8275(10) 0.119(4) Uani 1 1 d D . . C7 C 0.3733(8) 0.7861(4) 0.9194(12) 0.064(4) Uani 0.50 1 d PD . . N6 N 0.5000 0.0000 1.0000 0.066(3) Uani 1 4 d SD . . N7 N 1.0000 0.0000 0.5000 0.078(4) Uani 1 4 d SD . . C11 C 0.4225(7) 0.6944(3) 0.8343(7) 0.097(3) Uani 1 1 d D . . C10 C 0.3696(9) 0.7290(4) 0.9201(12) 0.065(4) Uani 0.50 1 d PD . . C9 C 0.4978(10) 0.7850(5) 0.9270(15) 0.103(7) Uani 0.50 1 d PD . . C12 C 0.4863(9) 0.7222(5) 0.9200(13) 0.082(5) Uani 0.50 1 d PD . . C19 C 0.9462(13) 0.0831(4) 0.5000 0.116(6) Uani 1 2 d SD . . N1S N 0.2227(16) 0.6396(8) 1.0000 0.54(5) Uani 1 2 d SD . . C14 C 0.5347(9) 0.0575(4) 1.1646(13) 0.138(5) Uani 1 1 d D . . C1S C 0.1464(16) 0.6286(6) 1.0000 0.36(3) Uani 1 2 d SD . . C18 C 0.9708(13) 0.0394(4) 0.4309(11) 0.076(5) Uani 0.50 1 d PD . . C2S C 0.0510(15) 0.6034(11) 1.0000 0.290(19) Uani 1 2 d SD . . H2S1 H 0.0149 0.6144 1.0659 0.434 Uiso 0.50 1 calc PR . . H2S2 H 0.0602 0.5712 1.0087 0.434 Uiso 0.50 1 calc PR . . H2S3 H 0.0202 0.6093 0.9254 0.434 Uiso 0.50 1 calc PR . . C17 C 1.1543(13) 0.0307(9) 0.5000 0.194(11) Uani 1 2 d SD . . C16 C 1.0769(11) 0.0137(6) 0.4060(13) 0.096(6) Uani 0.50 1 d PD . . C13 C 0.4579(10) 0.0374(5) 1.0789(17) 0.101(6) Uani 0.50 1 d PD . . C15 C 0.5752(9) 0.0204(5) 1.0752(16) 0.098(6) Uani 0.50 1 d PD . . C3S C 0.8171(14) 0.6171(6) 0.0000 0.132(7) Uani 1 2 d SD . . N2S N 0.8301(17) 0.6528(7) 0.0000 0.228(13) Uani 1 2 d SD . . H1A H 0.063(4) -0.278(2) 1.0000 0.024(16) Uiso 1 2 d S . . C6S C 0.2289(8) 0.0842(3) 0.2177(10) 0.118(4) Uani 1 1 d D . . H6S1 H 0.2213 0.0860 0.3035 0.177 Uiso 1 1 calc R . . H6S2 H 0.2459 0.0538 0.1958 0.177 Uiso 1 1 calc R . . H6S3 H 0.1730 0.0921 0.1787 0.177 Uiso 1 1 calc R . . C5S C 0.2975(9) 0.1147(4) 0.1813(16) 0.187(9) Uani 1 1 d D . . C4S C 0.821(2) 0.5659(8) 0.0000 0.27(2) Uani 1 2 d SD . . H4S1 H 0.7728 0.5542 -0.0497 0.409 Uiso 0.50 1 calc PR . . H4S2 H 0.8133 0.5549 0.0808 0.409 Uiso 0.50 1 calc PR . . H4S3 H 0.8781 0.5560 -0.0311 0.409 Uiso 0.50 1 calc PR . . N3S N 0.3493(11) 0.1406(5) 0.153(2) 0.295(13) Uani 1 1 d D . . O1 O 0.3824(13) 0.0068(6) 0.3725(14) 0.313(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0401(7) 0.0258(6) 0.0277(6) 0.000 0.000 -0.0002(5) Fe1 0.0531(5) 0.0336(4) 0.0391(5) -0.0042(3) -0.0076(4) -0.0008(3) Fe2 0.0467(7) 0.0242(5) 0.0348(6) 0.000 0.000 -0.0006(4) S1 0.0421(11) 0.0338(9) 0.0518(12) 0.000 0.000 -0.0022(8) S3 0.0465(11) 0.0274(9) 0.0515(12) 0.000 0.000 -0.0011(8) S2 0.0570(9) 0.0332(7) 0.0289(7) -0.0014(5) 0.0031(6) 0.0027(6) N4 0.044(3) 0.034(2) 0.035(2) -0.0034(18) 0.005(2) -0.0014(18) B1 0.047(5) 0.028(4) 0.053(6) 0.000 0.000 0.008(4) F1 0.113(4) 0.065(2) 0.075(3) -0.020(2) -0.048(3) 0.006(2) N3 0.043(3) 0.032(2) 0.044(3) -0.0060(19) 0.000(2) 0.0040(18) N1 0.042(4) 0.026(3) 0.042(4) 0.000 0.000 -0.001(2) N2 0.038(4) 0.030(3) 0.038(3) 0.000 0.000 0.002(2) N5 0.033(4) 0.047(4) 0.062(5) 0.000 0.000 0.003(3) C2 0.034(4) 0.047(4) 0.059(5) 0.000 0.000 -0.005(3) C1 0.046(5) 0.035(4) 0.054(5) 0.000 0.000 -0.008(3) C3 0.036(4) 0.039(4) 0.045(5) 0.000 0.000 0.005(3) C4 0.046(3) 0.042(3) 0.062(4) -0.022(3) -0.010(3) 0.009(3) C6 0.052(4) 0.054(3) 0.040(3) 0.000(3) 0.004(3) 0.002(3) C5 0.052(4) 0.069(4) 0.039(3) -0.015(3) 0.008(3) 0.012(3) C8 0.164(11) 0.078(6) 0.116(8) 0.048(6) 0.011(8) 0.007(6) C7 0.048(7) 0.057(7) 0.085(10) 0.009(7) -0.026(7) 0.010(6) N6 0.042(6) 0.047(6) 0.108(10) 0.000 0.000 -0.009(5) N7 0.123(12) 0.041(6) 0.069(8) 0.000 0.000 0.003(6) C11 0.149(9) 0.085(6) 0.056(5) -0.024(4) 0.005(5) 0.022(6) C10 0.061(8) 0.072(9) 0.063(9) -0.015(7) -0.016(7) -0.001(7) C9 0.076(11) 0.090(11) 0.144(16) -0.018(11) 0.065(11) -0.012(9) C12 0.069(10) 0.085(10) 0.090(11) 0.008(9) 0.051(9) 0.036(8) C19 0.221(18) 0.065(7) 0.061(7) 0.000 0.000 0.052(9) N1S 0.16(2) 0.113(16) 1.35(15) 0.000 0.000 0.000(15) C14 0.149(11) 0.092(7) 0.172(12) -0.056(7) 0.032(10) -0.039(7) C1S 0.85(8) 0.18(2) 0.054(10) 0.000 0.000 0.32(4) C18 0.143(15) 0.046(7) 0.040(7) 0.016(6) -0.004(9) 0.013(8) C2S 0.105(18) 0.40(5) 0.36(5) 0.000 0.000 -0.03(2) C17 0.115(16) 0.19(2) 0.28(3) 0.000 0.000 -0.055(15) C16 0.118(16) 0.107(14) 0.064(10) 0.010(9) 0.013(10) -0.021(11) C13 0.072(11) 0.069(10) 0.162(18) -0.024(10) 0.034(11) 0.000(8) C15 0.059(10) 0.079(11) 0.156(17) -0.001(10) -0.010(10) -0.011(8) C3S 0.181(19) 0.125(14) 0.090(11) 0.000 0.000 -0.056(13) N2S 0.34(3) 0.21(2) 0.131(14) 0.000 0.000 -0.18(2) C6S 0.125(9) 0.082(6) 0.146(10) -0.004(6) -0.054(8) 0.000(6) C5S 0.146(13) 0.070(7) 0.35(2) -0.045(11) -0.137(15) 0.027(7) C4S 0.41(5) 0.30(4) 0.116(17) 0.000 0.000 -0.22(4) N3S 0.163(14) 0.131(12) 0.59(4) -0.046(16) -0.040(18) -0.002(10) O1 0.33(2) 0.33(2) 0.275(17) -0.015(15) 0.035(17) -0.031(18) _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 V1 N2 2.190(6) . ? V1 N4 2.195(4) . ? V1 N4 2.195(4) 8_557 ? V1 S1 2.373(2) . ? V1 S2 2.3733(15) . ? V1 S2 2.3733(15) 8_557 ? V1 Fe1 2.7987(12) . ? V1 Fe1 2.7987(12) 8_557 ? V1 Fe2 2.8131(15) . ? Fe1 F1 1.890(4) . ? Fe1 S2 2.2834(16) . ? Fe1 S1 2.2905(17) . ? Fe1 S3 2.3716(16) 5_557 ? Fe1 Fe1 2.6753(16) 8_557 ? Fe1 Fe2 2.7333(13) . ? Fe2 S2 2.2670(14) 8_557 ? Fe2 S2 2.2670(14) . ? Fe2 S3 2.287(2) . ? Fe2 S3 2.378(2) 5_557 ? Fe2 Fe2 2.6856(19) 5_557 ? Fe2 Fe1 2.7333(13) 8_557 ? S1 Fe1 2.2905(17) 8_557 ? S3 Fe1 2.3716(16) 4 ? S3 Fe1 2.3716(16) 5_557 ? S3 Fe2 2.378(2) 5_557 ? N4 C6 1.327(7) . ? N4 N3 1.364(6) . ? B1 N3 1.530(7) 8_557 ? B1 N3 1.530(7) . ? B1 N1 1.540(11) . ? B1 H1A 1.04(6) . ? N3 C4 1.354(7) . ? N1 C1 1.336(10) . ? N1 N2 1.363(8) . ? N2 C3 1.333(9) . ? N5 C10 1.474(12) 8_557 ? N5 C10 1.474(12) . ? N5 C12 1.530(11) . ? N5 C12 1.530(11) 8_557 ? N5 C7 1.551(11) . ? N5 C7 1.551(11) 8_557 ? N5 C9 1.556(13) 8_557 ? N5 C9 1.556(13) . ? C2 C1 1.366(11) . ? C2 C3 1.383(11) . ? C2 H2 0.9300 . ? C1 H1 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.344(9) . ? C4 H4 0.9300 . ? C6 C5 1.399(8) . ? C6 H6 0.9300 . ? C5 H5 0.9300 . ? C8 C7 1.586(14) . ? C8 C9 1.669(16) . ? C7 C7 1.79(3) 8_557 ? N6 C15 1.512(13) 5_657 ? N6 C15 1.512(13) 4_655 ? N6 C15 1.512(13) . ? N6 C15 1.512(13) 8_557 ? N6 C13 1.536(13) 5_657 ? N6 C13 1.536(13) 4_655 ? N6 C13 1.536(13) . ? N6 C13 1.536(13) 8_557 ? N7 C18 1.454(10) 4_755 ? N7 C18 1.454(10) 5_756 ? N7 C18 1.454(10) . ? N7 C18 1.454(10) 8_556 ? N7 C16 1.592(13) 4_755 ? N7 C16 1.592(14) . ? N7 C16 1.592(13) 5_756 ? N7 C16 1.592(14) 8_556 ? C11 C12 1.566(15) . ? C11 C10 1.598(13) . ? C10 C10 1.77(3) 8_557 ? C9 C9 1.62(3) 8_557 ? C12 C12 1.78(3) 8_557 ? C19 C18 1.539(13) . ? C19 C18 1.539(13) 8_556 ? N1S C1S 1.171(19) . ? C14 C15 1.590(15) . ? C14 C13 1.593(16) . ? C1S C2S 1.589(19) . ? C18 C18 1.53(2) 8_556 ? C18 C16 1.73(2) 4_755 ? C2S H2S1 1.1398 . ? C2S H2S2 1.1333 . ? C2S H2S3 1.1512 . ? C17 C16 1.624(15) . ? C17 C16 1.624(15) 8_556 ? C16 C18 1.73(2) 4_755 ? C13 C13 1.75(4) 8_557 ? C13 C15 1.77(2) 4_655 ? C15 C15 1.67(4) 8_557 ? C15 C13 1.77(2) 4_655 ? C3S N2S 1.065(15) . ? C3S C4S 1.507(18) . ? C6S C5S 1.410(14) . ? C6S H6S1 0.9600 . ? C6S H6S2 0.9600 . ? C6S H6S3 0.9600 . ? C5S N3S 1.124(15) . ? C4S H4S1 1.1231 . ? C4S H4S2 1.1230 . ? C4S H4S3 1.1234 . ? 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 N2 V1 N4 80.68(16) . . ? N2 V1 N4 80.68(16) . 8_557 ? N4 V1 N4 81.4(2) . 8_557 ? N2 V1 S1 164.90(16) . . ? N4 V1 S1 87.90(13) . . ? N4 V1 S1 87.90(13) 8_557 . ? N2 V1 S2 87.91(11) . . ? N4 V1 S2 165.51(12) . . ? N4 V1 S2 88.01(12) 8_557 . ? S1 V1 S2 101.62(6) . . ? N2 V1 S2 87.91(11) . 8_557 ? N4 V1 S2 88.01(12) . 8_557 ? N4 V1 S2 165.51(12) 8_557 8_557 ? S1 V1 S2 101.62(6) . 8_557 ? S2 V1 S2 100.55(8) . 8_557 ? N2 V1 Fe1 139.44(11) . . ? N4 V1 Fe1 139.57(13) . . ? N4 V1 Fe1 97.93(11) 8_557 . ? S1 V1 Fe1 51.78(4) . . ? S2 V1 Fe1 51.60(4) . . ? S2 V1 Fe1 96.55(5) 8_557 . ? N2 V1 Fe1 139.44(11) . 8_557 ? N4 V1 Fe1 97.93(11) . 8_557 ? N4 V1 Fe1 139.57(13) 8_557 8_557 ? S1 V1 Fe1 51.78(4) . 8_557 ? S2 V1 Fe1 96.55(5) . 8_557 ? S2 V1 Fe1 51.60(4) 8_557 8_557 ? Fe1 V1 Fe1 57.10(4) . 8_557 ? N2 V1 Fe2 96.63(15) . . ? N4 V1 Fe2 138.97(11) . . ? N4 V1 Fe2 138.97(11) 8_557 . ? S1 V1 Fe2 98.47(6) . . ? S2 V1 Fe2 50.98(4) . . ? S2 V1 Fe2 50.98(4) 8_557 . ? Fe1 V1 Fe2 58.29(3) . . ? Fe1 V1 Fe2 58.29(3) 8_557 . ? F1 Fe1 S2 117.96(17) . . ? F1 Fe1 S1 112.76(16) . . ? S2 Fe1 S1 107.09(6) . . ? F1 Fe1 S3 106.65(13) . 5_557 ? S2 Fe1 S3 104.47(7) . 5_557 ? S1 Fe1 S3 107.10(5) . 5_557 ? F1 Fe1 Fe1 139.47(16) . 8_557 ? S2 Fe1 Fe1 102.33(4) . 8_557 ? S1 Fe1 Fe1 54.27(3) . 8_557 ? S3 Fe1 Fe1 55.67(3) 5_557 8_557 ? F1 Fe1 Fe2 143.84(14) . . ? S2 Fe1 Fe2 52.81(4) . . ? S1 Fe1 Fe2 102.90(5) . . ? S3 Fe1 Fe2 54.98(5) 5_557 . ? Fe1 Fe1 Fe2 60.70(2) 8_557 . ? F1 Fe1 V1 148.36(13) . . ? S2 Fe1 V1 54.54(4) . . ? S1 Fe1 V1 54.49(6) . . ? S3 Fe1 V1 104.91(5) 5_557 . ? Fe1 Fe1 V1 61.45(2) 8_557 . ? Fe2 Fe1 V1 61.12(3) . . ? S2 Fe2 S2 107.25(7) 8_557 . ? S2 Fe2 S3 114.69(5) 8_557 . ? S2 Fe2 S3 114.69(5) . . ? S2 Fe2 S3 104.78(6) 8_557 5_557 ? S2 Fe2 S3 104.78(6) . 5_557 ? S3 Fe2 S3 109.73(7) . 5_557 ? S2 Fe2 Fe2 125.57(4) 8_557 5_557 ? S2 Fe2 Fe2 125.57(4) . 5_557 ? S3 Fe2 Fe2 56.46(6) . 5_557 ? S3 Fe2 Fe2 53.27(6) 5_557 5_557 ? S2 Fe2 Fe1 101.03(6) 8_557 . ? S2 Fe2 Fe1 53.36(4) . . ? S3 Fe2 Fe1 144.12(4) . . ? S3 Fe2 Fe1 54.76(5) 5_557 . ? Fe2 Fe2 Fe1 100.31(5) 5_557 . ? S2 Fe2 Fe1 53.36(4) 8_557 8_557 ? S2 Fe2 Fe1 101.03(6) . 8_557 ? S3 Fe2 Fe1 144.12(4) . 8_557 ? S3 Fe2 Fe1 54.76(5) 5_557 8_557 ? Fe2 Fe2 Fe1 100.31(5) 5_557 8_557 ? Fe1 Fe2 Fe1 58.60(4) . 8_557 ? S2 Fe2 V1 54.42(4) 8_557 . ? S2 Fe2 V1 54.42(4) . . ? S3 Fe2 V1 145.97(7) . . ? S3 Fe2 V1 104.30(7) 5_557 . ? Fe2 Fe2 V1 157.57(7) 5_557 . ? Fe1 Fe2 V1 60.59(3) . . ? Fe1 Fe2 V1 60.59(3) 8_557 . ? Fe1 S1 Fe1 71.47(7) 8_557 . ? Fe1 S1 V1 73.73(6) 8_557 . ? Fe1 S1 V1 73.73(6) . . ? Fe2 S3 Fe1 126.54(7) . 4 ? Fe2 S3 Fe1 126.54(7) . 5_557 ? Fe1 S3 Fe1 68.67(6) 4 5_557 ? Fe2 S3 Fe2 70.27(7) . 5_557 ? Fe1 S3 Fe2 70.27(5) 4 5_557 ? Fe1 S3 Fe2 70.27(5) 5_557 5_557 ? Fe2 S2 Fe1 73.83(5) . . ? Fe2 S2 V1 74.60(5) . . ? Fe1 S2 V1 73.85(5) . . ? C6 N4 N3 106.0(4) . . ? C6 N4 V1 131.6(4) . . ? N3 N4 V1 122.4(3) . . ? N3 B1 N3 108.0(7) 8_557 . ? N3 B1 N1 108.3(4) 8_557 . ? N3 B1 N1 108.3(4) . . ? N3 B1 H1A 111.6(18) 8_557 . ? N3 B1 H1A 111.6(18) . . ? N1 B1 H1A 109(4) . . ? C4 N3 N4 108.8(4) . . ? C4 N3 B1 131.3(5) . . ? N4 N3 B1 119.8(4) . . ? C1 N1 N2 109.9(6) . . ? C1 N1 B1 131.0(6) . . ? N2 N1 B1 119.2(6) . . ? C3 N2 N1 105.6(6) . . ? C3 N2 V1 131.3(5) . . ? N1 N2 V1 123.0(4) . . ? C10 N5 C10 73.9(12) 8_557 . ? C10 N5 C12 111.2(9) 8_557 . ? C10 N5 C12 70.4(8) . . ? C10 N5 C12 70.4(8) 8_557 8_557 ? C10 N5 C12 111.2(9) . 8_557 ? C12 N5 C12 71.0(12) . 8_557 ? C10 N5 C7 108.0(8) 8_557 . ? C10 N5 C7 67.4(7) . . ? C12 N5 C7 109.2(8) . . ? C12 N5 C7 178.2(9) 8_557 . ? C10 N5 C7 67.4(7) 8_557 8_557 ? C10 N5 C7 108.0(8) . 8_557 ? C12 N5 C7 178.2(9) . 8_557 ? C12 N5 C7 109.2(8) 8_557 8_557 ? C7 N5 C7 70.5(11) . 8_557 ? C10 N5 C9 111.6(9) 8_557 8_557 ? C10 N5 C9 173.8(10) . 8_557 ? C12 N5 C9 109.2(9) . 8_557 ? C12 N5 C9 74.0(8) 8_557 8_557 ? C7 N5 C9 107.5(8) . 8_557 ? C7 N5 C9 72.5(8) 8_557 8_557 ? C10 N5 C9 173.8(10) 8_557 . ? C10 N5 C9 111.6(9) . . ? C12 N5 C9 74.0(8) . . ? C12 N5 C9 109.2(9) 8_557 . ? C7 N5 C9 72.5(8) . . ? C7 N5 C9 107.5(8) 8_557 . ? C9 N5 C9 62.8(14) 8_557 . ? C1 C2 C3 104.7(7) . . ? C1 C2 H2 127.6 . . ? C3 C2 H2 127.6 . . ? N1 C1 C2 108.8(7) . . ? N1 C1 H1 125.6 . . ? C2 C1 H1 125.6 . . ? N2 C3 C2 111.0(7) . . ? N2 C3 H3 124.5 . . ? C2 C3 H3 124.5 . . ? C5 C4 N3 109.8(5) . . ? C5 C4 H4 125.1 . . ? N3 C4 H4 125.1 . . ? N4 C6 C5 111.1(5) . . ? N4 C6 H6 124.4 . . ? C5 C6 H6 124.4 . . ? C4 C5 C6 104.3(5) . . ? C4 C5 H5 127.9 . . ? C6 C5 H5 127.9 . . ? C7 C8 C9 68.7(7) . . ? N5 C7 C8 111.1(8) . . ? N5 C7 C7 54.8(6) . 8_557 ? C8 C7 C7 130.0(7) . 8_557 ? C15 N6 C15 67.0(14) 5_657 4_655 ? C15 N6 C15 180.0(11) 5_657 . ? C15 N6 C15 113.0(14) 4_655 . ? C15 N6 C15 113.0(14) 5_657 8_557 ? C15 N6 C15 180.0(11) 4_655 8_557 ? C15 N6 C15 67.0(14) . 8_557 ? C15 N6 C13 72.4(8) 5_657 5_657 ? C15 N6 C13 109.0(9) 4_655 5_657 ? C15 N6 C13 107.6(8) . 5_657 ? C15 N6 C13 71.0(9) 8_557 5_657 ? C15 N6 C13 109.0(9) 5_657 4_655 ? C15 N6 C13 72.4(8) 4_655 4_655 ? C15 N6 C13 71.0(9) . 4_655 ? C15 N6 C13 107.6(8) 8_557 4_655 ? C13 N6 C13 69.5(15) 5_657 4_655 ? C15 N6 C13 107.6(8) 5_657 . ? C15 N6 C13 71.0(9) 4_655 . ? C15 N6 C13 72.4(8) . . ? C15 N6 C13 109.0(9) 8_557 . ? C13 N6 C13 180.0(11) 5_657 . ? C13 N6 C13 110.5(15) 4_655 . ? C15 N6 C13 71.0(9) 5_657 8_557 ? C15 N6 C13 107.6(8) 4_655 8_557 ? C15 N6 C13 109.0(9) . 8_557 ? C15 N6 C13 72.4(8) 8_557 8_557 ? C13 N6 C13 110.5(15) 5_657 8_557 ? C13 N6 C13 180.000(3) 4_655 8_557 ? C13 N6 C13 69.5(15) . 8_557 ? C18 N7 C18 63.6(10) 4_755 5_756 ? C18 N7 C18 116.4(10) 4_755 . ? C18 N7 C18 180.0(9) 5_756 . ? C18 N7 C18 180.0(9) 4_755 8_556 ? C18 N7 C18 116.4(10) 5_756 8_556 ? C18 N7 C18 63.6(10) . 8_556 ? C18 N7 C16 70.3(9) 4_755 4_755 ? C18 N7 C16 110.8(9) 5_756 4_755 ? C18 N7 C16 69.2(9) . 4_755 ? C18 N7 C16 109.7(9) 8_556 4_755 ? C18 N7 C16 69.2(9) 4_755 . ? C18 N7 C16 109.7(9) 5_756 . ? C18 N7 C16 70.3(9) . . ? C18 N7 C16 110.8(9) 8_556 . ? C16 N7 C16 98.2(12) 4_755 . ? C18 N7 C16 110.8(9) 4_755 5_756 ? C18 N7 C16 70.3(9) 5_756 5_756 ? C18 N7 C16 109.7(9) . 5_756 ? C18 N7 C16 69.2(9) 8_556 5_756 ? C16 N7 C16 81.8(12) 4_755 5_756 ? C16 N7 C16 180.0(13) . 5_756 ? C18 N7 C16 109.7(9) 4_755 8_556 ? C18 N7 C16 69.2(9) 5_756 8_556 ? C18 N7 C16 110.8(9) . 8_556 ? C18 N7 C16 70.3(9) 8_556 8_556 ? C16 N7 C16 180.000(2) 4_755 8_556 ? C16 N7 C16 81.8(12) . 8_556 ? C16 N7 C16 98.2(12) 5_756 8_556 ? C12 C11 C10 66.4(6) . . ? N5 C10 C11 112.3(9) . . ? N5 C10 C10 53.0(6) . 8_557 ? C11 C10 C10 126.6(6) . 8_557 ? N5 C9 C9 58.6(7) . 8_557 ? N5 C9 C8 106.6(9) . . ? C9 C9 C8 131.4(7) 8_557 . ? N5 C12 C11 111.0(9) . . ? N5 C12 C12 54.5(6) . 8_557 ? C11 C12 C12 127.4(6) . 8_557 ? C18 C19 C18 59.7(9) . 8_556 ? C15 C14 C13 68.9(8) . . ? N1S C1S C2S 168(3) . . ? N7 C18 C18 58.2(5) . 8_556 ? N7 C18 C19 118.2(8) . . ? C18 C18 C19 60.1(5) 8_556 . ? N7 C18 C16 59.1(7) . 4_755 ? C18 C18 C16 99.2(6) 8_556 4_755 ? C19 C18 C16 137.3(15) . 4_755 ? C1S C2S H2S1 126.4 . . ? C1S C2S H2S2 125.8 . . ? H2S1 C2S H2S2 88.5 . . ? C1S C2S H2S3 127.4 . . ? H2S1 C2S H2S3 87.7 . . ? H2S2 C2S H2S3 88.3 . . ? C16 C17 C16 79.9(12) . 8_556 ? N7 C16 C17 99.0(10) . . ? N7 C16 C18 51.6(6) . 4_755 ? C17 C16 C18 117.3(15) . 4_755 ? N6 C13 C14 108.6(10) . . ? N6 C13 C13 55.3(7) . 8_557 ? C14 C13 C13 126.7(8) . 8_557 ? N6 C13 C15 53.9(7) . 4_655 ? C14 C13 C15 124.5(13) . 4_655 ? C13 C13 C15 88.7(8) 8_557 4_655 ? N6 C15 C14 110.0(10) . . ? N6 C15 C15 56.5(7) . 8_557 ? C14 C15 C15 128.6(9) . 8_557 ? N6 C15 C13 55.1(7) . 4_655 ? C14 C15 C13 122.7(13) . 4_655 ? C15 C15 C13 91.3(8) 8_557 4_655 ? N2S C3S C4S 168(3) . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? N3S C5S C6S 176.8(16) . . ? C3S C4S H4S1 125.9 . . ? C3S C4S H4S2 125.9 . . ? H4S1 C4S H4S2 89.1 . . ? C3S C4S H4S3 125.9 . . ? H4S1 C4S H4S3 89.1 . . ? H4S2 C4S H4S3 89.1 . . ? C67 C66 N50 116.2(5) . . ? C72 N51 C70 110.9(5) . . ? C72 N51 C74 111.1(5) . . ? C70 N51 C74 107.0(5) . . ? C72 N51 C68 106.8(5) . . ? C70 N51 C68 110.5(5) . . ? C74 N51 C68 110.5(5) . . ? C69 C68 N51 114.5(6) . . ? N51 C70 C71 115.4(6) . . ? C73 C72 N51 115.2(6) . . ? C75 C74 N51 116.3(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.858 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.118 data_ts201fu_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'bis(Tetraethylammoinum) Tetrakis(\m3-sulfido)-trisfluorido-(hydrogen tri(pyrazolyl)borato-N,N',N")-tri-iron-vanadium acetonitrile solvate' ; _chemical_name_common 'Floride vanadium single cubane' _chemical_melting_point 'not measured' _chemical_formula_moiety '(Et4N)2 ((C9H10N6B)VFe3S4F3)(CH3CN)' _chemical_formula_sum 'C27 H53 B F3 Fe3 N9 S4 V' _chemical_formula_weight 918.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'V' 'V' 0.3005 0.5294 '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' _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 10.8425(6) _cell_length_b 16.8430(10) _cell_length_c 21.8996(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.1270(10) _cell_angle_gamma 90.00 _cell_volume 3976.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3489 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.26 _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _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_% ? _diffrn_reflns_number 13493 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8110 _reflns_number_gt 6068 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.6702P] 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 SHELXL _refine_ls_extinction_coef 0.0000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8110 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 15.000 _refine_ls_shift/su_mean 0.036 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 B1 B 0.5623(3) 0.1978(2) 0.60191(14) 0.0325(7) Uani 1 1 d . . . C1 C 0.4560(3) 0.06058(18) 0.61669(14) 0.0369(7) Uani 1 1 d . . . H1 H 0.4141 0.0548 0.5776 0.044 Uiso 1 1 calc R . . C2 C 0.4515(3) 0.00870(18) 0.66398(16) 0.0426(8) Uani 1 1 d . . . H2 H 0.4070 -0.0385 0.6639 0.051 Uiso 1 1 calc R . . C3 C 0.5280(3) 0.04167(17) 0.71250(14) 0.0351(7) Uani 1 1 d . . . H3 H 0.5431 0.0194 0.7515 0.042 Uiso 1 1 calc R . . C4 C 0.7702(3) 0.20248(17) 0.55262(13) 0.0351(7) Uani 1 1 d . . . H4 H 0.7391 0.2034 0.5114 0.042 Uiso 1 1 calc R . . C5 C 0.8927(3) 0.20315(18) 0.57485(14) 0.0400(7) Uani 1 1 d . . . H5 H 0.9608 0.2048 0.5524 0.048 Uiso 1 1 calc R . . C6 C 0.8936(3) 0.20082(17) 0.63822(13) 0.0343(7) Uani 1 1 d . . . H6 H 0.9651 0.2003 0.6658 0.041 Uiso 1 1 calc R . . C7 C 0.4418(3) 0.32751(18) 0.62382(14) 0.0371(7) Uani 1 1 d . . . H7 H 0.3968 0.3337 0.5855 0.045 Uiso 1 1 calc R . . C8 C 0.4356(3) 0.37672(18) 0.67318(15) 0.0423(8) Uani 1 1 d . . . H8 H 0.3870 0.4219 0.6754 0.051 Uiso 1 1 calc R . . C9 C 0.5186(3) 0.34364(17) 0.71934(14) 0.0361(7) Uani 1 1 d . . . H9 H 0.5345 0.3641 0.7588 0.043 Uiso 1 1 calc R . . C10 C 0.2280(3) 0.4313(2) 0.83443(14) 0.0447(8) Uani 1 1 d . . . H10A H 0.1991 0.4833 0.8201 0.054 Uiso 1 1 calc R . . H10B H 0.3180 0.4326 0.8390 0.054 Uiso 1 1 calc R . . C11 C 0.1855(4) 0.3711(2) 0.78586(15) 0.0571(10) Uani 1 1 d . . . H11A H 0.2103 0.3190 0.8001 0.086 Uiso 1 1 calc R . . H11B H 0.2224 0.3828 0.7489 0.086 Uiso 1 1 calc R . . H11C H 0.0968 0.3731 0.7776 0.086 Uiso 1 1 calc R . . C12 C 0.2323(3) 0.33723(19) 0.92277(15) 0.0459(8) Uani 1 1 d . . . H12A H 0.2100 0.3323 0.9643 0.055 Uiso 1 1 calc R . . H12B H 0.1896 0.2953 0.8985 0.055 Uiso 1 1 calc R . . C13 C 0.3704(4) 0.3236(2) 0.92412(19) 0.0711(12) Uani 1 1 d . . . H13A H 0.3929 0.3235 0.8829 0.107 Uiso 1 1 calc R . . H13B H 0.3916 0.2735 0.9432 0.107 Uiso 1 1 calc R . . H13C H 0.4142 0.3653 0.9471 0.107 Uiso 1 1 calc R . . C14 C 0.2360(3) 0.48552(19) 0.93667(16) 0.0475(8) Uani 1 1 d . . . H14A H 0.3258 0.4816 0.9417 0.057 Uiso 1 1 calc R . . H14B H 0.2145 0.5346 0.9150 0.057 Uiso 1 1 calc R . . C15 C 0.1915(3) 0.4906(2) 0.99963(15) 0.0556(9) Uani 1 1 d . . . H15A H 0.1056 0.5056 0.9956 0.083 Uiso 1 1 calc R . . H15B H 0.2395 0.5296 1.0237 0.083 Uiso 1 1 calc R . . H15C H 0.2012 0.4399 1.0195 0.083 Uiso 1 1 calc R . . C16 C 0.0451(3) 0.41334(19) 0.89297(14) 0.0414(8) Uani 1 1 d . . . H16A H 0.0214 0.4033 0.9337 0.050 Uiso 1 1 calc R . . H16B H 0.0169 0.3686 0.8673 0.050 Uiso 1 1 calc R . . C17 C -0.0219(3) 0.4875(2) 0.86752(17) 0.0552(9) Uani 1 1 d . . . H17A H 0.0021 0.5319 0.8936 0.083 Uiso 1 1 calc R . . H17B H -0.1099 0.4796 0.8661 0.083 Uiso 1 1 calc R . . H17C H -0.0004 0.4977 0.8269 0.083 Uiso 1 1 calc R . . C18 C 0.2287(3) 0.92599(19) 0.96215(14) 0.0453(8) Uani 1 1 d . . . H18A H 0.1836 0.9413 0.9962 0.054 Uiso 1 1 calc R . . H18B H 0.1997 0.8737 0.9488 0.054 Uiso 1 1 calc R . . C19 C 0.3639(3) 0.9199(2) 0.98529(15) 0.0555(9) Uani 1 1 d . . . H19A H 0.4107 0.9070 0.9518 0.083 Uiso 1 1 calc R . . H19B H 0.3754 0.8790 1.0159 0.083 Uiso 1 1 calc R . . H19C H 0.3921 0.9697 1.0029 0.083 Uiso 1 1 calc R . . C20 C 0.2444(4) 1.06655(19) 0.92546(15) 0.0540(9) Uani 1 1 d . . . H20A H 0.2180 1.1016 0.8914 0.065 Uiso 1 1 calc R . . H20B H 0.3343 1.0647 0.9294 0.065 Uiso 1 1 calc R . . C21 C 0.2038(4) 1.1026(2) 0.98386(16) 0.0643(11) Uani 1 1 d . . . H21A H 0.1153 1.1088 0.9794 0.096 Uiso 1 1 calc R . . H21B H 0.2424 1.1536 0.9910 0.096 Uiso 1 1 calc R . . H21C H 0.2281 1.0682 1.0180 0.096 Uiso 1 1 calc R . . C22 C 0.0553(3) 0.9884(2) 0.89705(15) 0.0476(8) Uani 1 1 d . . . H22A H 0.0222 1.0055 0.9343 0.057 Uiso 1 1 calc R . . H22B H 0.0347 1.0288 0.8661 0.057 Uiso 1 1 calc R . . C23 C -0.0091(3) 0.9122(2) 0.87559(19) 0.0644(11) Uani 1 1 d . . . H23A H 0.0215 0.8948 0.8383 0.097 Uiso 1 1 calc R . . H23B H -0.0968 0.9212 0.8683 0.097 Uiso 1 1 calc R . . H23C H 0.0071 0.8721 0.9066 0.097 Uiso 1 1 calc R . . C24 C 0.2528(3) 0.9539(2) 0.85370(14) 0.0468(8) Uani 1 1 d . . . H24A H 0.3423 0.9536 0.8630 0.056 Uiso 1 1 calc R . . H24B H 0.2264 0.8996 0.8457 0.056 Uiso 1 1 calc R . . C25 C 0.2199(4) 1.0023(2) 0.79603(15) 0.0635(11) Uani 1 1 d . . . H25A H 0.1314 1.0038 0.7867 0.095 Uiso 1 1 calc R . . H25B H 0.2566 0.9785 0.7625 0.095 Uiso 1 1 calc R . . H25C H 0.2509 1.0554 0.8024 0.095 Uiso 1 1 calc R . . C26 C 0.2278(3) 0.1916(2) 0.63484(18) 0.0465(8) Uani 1 1 d . . . C27 C 0.2643(4) 0.1856(2) 0.70025(17) 0.0557(10) Uani 1 1 d . . . H27A H 0.3101 0.1373 0.7088 0.084 Uiso 1 1 calc R . . H27B H 0.1917 0.1853 0.7217 0.084 Uiso 1 1 calc R . . H27C H 0.3155 0.2302 0.7135 0.084 Uiso 1 1 calc R . . F1 F 0.72484(19) 0.01378(10) 0.89313(8) 0.0541(5) Uani 1 1 d . . . F2 F 1.10835(16) 0.19173(10) 0.82002(8) 0.0445(4) Uani 1 1 d . . . F3 F 0.68963(19) 0.36111(11) 0.90075(8) 0.0550(5) Uani 1 1 d . . . Fe1 Fe 0.74977(4) 0.10973(2) 0.855209(17) 0.03025(12) Uani 1 1 d . . . Fe2 Fe 0.93636(4) 0.19564(2) 0.817371(17) 0.02826(11) Uani 1 1 d . . . Fe3 Fe 0.73931(4) 0.27244(2) 0.860015(17) 0.03082(12) Uani 1 1 d . . . N1 N 0.5308(2) 0.12157(14) 0.63544(10) 0.0302(5) Uani 1 1 d . . . N2 N 0.5767(2) 0.10973(13) 0.69517(10) 0.0284(5) Uani 1 1 d . . . N3 N 0.7021(2) 0.20031(14) 0.60033(10) 0.0304(5) Uani 1 1 d . . . N4 N 0.7785(2) 0.19935(13) 0.65438(10) 0.0295(5) Uani 1 1 d . . . N5 N 0.5233(2) 0.26866(14) 0.63953(10) 0.0308(5) Uani 1 1 d . . . N6 N 0.5722(2) 0.27838(13) 0.69917(10) 0.0291(5) Uani 1 1 d . . . N7 N 0.1846(2) 0.41680(14) 0.89698(11) 0.0351(6) Uani 1 1 d . . . N8 N 0.1953(2) 0.98392(14) 0.90968(11) 0.0369(6) Uani 1 1 d . . . N9 N 0.2006(3) 0.1968(2) 0.58351(16) 0.0675(10) Uani 1 1 d . . . S1 S 0.84479(7) 0.08832(4) 0.76868(3) 0.03029(17) Uani 1 1 d . . . S2 S 0.58250(7) 0.18740(4) 0.82655(3) 0.03370(18) Uani 1 1 d . . . S3 S 0.83442(7) 0.30333(4) 0.77464(3) 0.03082(17) Uani 1 1 d . . . S4 S 0.87938(7) 0.19362(4) 0.91648(3) 0.03209(17) Uani 1 1 d . . . V1 V 0.70644(4) 0.19438(2) 0.744664(19) 0.02400(12) Uani 1 1 d . . . H1A H 0.517(2) 0.2001(15) 0.5544(13) 0.031(8) 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 B1 0.032(2) 0.0417(19) 0.0228(14) 0.0022(13) -0.0029(13) 0.0004(15) C1 0.0270(17) 0.0390(17) 0.0431(17) -0.0135(13) -0.0034(13) -0.0003(13) C2 0.0331(18) 0.0314(16) 0.063(2) -0.0059(15) 0.0028(15) -0.0051(13) C3 0.0334(18) 0.0288(14) 0.0431(16) 0.0002(12) 0.0038(13) -0.0017(12) C4 0.044(2) 0.0368(16) 0.0256(14) 0.0047(12) 0.0065(12) -0.0030(13) C5 0.040(2) 0.0471(19) 0.0351(16) 0.0051(13) 0.0121(14) -0.0010(14) C6 0.0268(19) 0.0419(17) 0.0339(15) 0.0015(12) 0.0021(12) 0.0014(13) C7 0.0259(18) 0.0382(16) 0.0447(17) 0.0125(13) -0.0075(13) 0.0004(13) C8 0.0351(19) 0.0299(16) 0.061(2) 0.0064(14) 0.0021(15) 0.0066(13) C9 0.0361(19) 0.0266(14) 0.0451(17) -0.0040(12) 0.0022(13) 0.0037(13) C10 0.041(2) 0.0487(19) 0.0446(18) 0.0171(15) 0.0068(14) -0.0017(15) C11 0.070(3) 0.066(2) 0.0369(18) 0.0040(17) 0.0140(17) -0.002(2) C12 0.066(3) 0.0363(16) 0.0349(16) 0.0087(13) 0.0041(15) 0.0031(16) C13 0.076(3) 0.072(3) 0.063(3) 0.012(2) -0.005(2) 0.025(2) C14 0.044(2) 0.0350(17) 0.060(2) -0.0018(15) -0.0096(16) -0.0086(15) C15 0.058(2) 0.058(2) 0.046(2) -0.0146(17) -0.0132(16) 0.0041(18) C16 0.039(2) 0.0464(18) 0.0384(16) -0.0050(14) 0.0029(13) -0.0133(15) C17 0.039(2) 0.071(3) 0.053(2) -0.0019(18) -0.0060(16) 0.0036(18) C18 0.057(2) 0.0412(18) 0.0372(17) 0.0104(14) 0.0048(15) 0.0098(16) C19 0.055(2) 0.069(2) 0.0421(19) 0.0113(17) 0.0006(16) 0.0205(19) C20 0.082(3) 0.0350(17) 0.0413(18) 0.0027(14) -0.0108(17) -0.0004(17) C21 0.103(3) 0.043(2) 0.0415(19) -0.0073(15) -0.0174(19) 0.008(2) C22 0.052(2) 0.049(2) 0.0403(17) -0.0009(15) -0.0016(15) 0.0188(16) C23 0.057(3) 0.068(3) 0.066(3) -0.007(2) -0.0077(19) 0.003(2) C24 0.056(2) 0.0492(19) 0.0361(17) 0.0006(14) 0.0075(15) 0.0106(16) C25 0.104(3) 0.056(2) 0.0320(17) 0.0040(16) 0.0117(19) 0.007(2) C26 0.027(2) 0.054(2) 0.060(2) -0.0059(17) 0.0112(16) -0.0018(15) C27 0.054(3) 0.064(2) 0.052(2) 0.0030(18) 0.0188(18) 0.0051(18) F1 0.0925(16) 0.0305(9) 0.0391(10) 0.0056(8) 0.0059(10) -0.0103(10) F2 0.0317(11) 0.0511(11) 0.0505(11) 0.0036(9) 0.0035(8) 0.0022(8) F3 0.0785(15) 0.0357(10) 0.0492(11) -0.0116(8) 0.0001(10) 0.0226(10) Fe1 0.0411(3) 0.0249(2) 0.0238(2) 0.00058(15) -0.00138(17) 0.00001(17) Fe2 0.0305(3) 0.0279(2) 0.02527(19) -0.00054(15) -0.00211(16) 0.00196(17) Fe3 0.0393(3) 0.0255(2) 0.0264(2) -0.00408(15) -0.00249(17) 0.00589(17) N1 0.0249(14) 0.0356(13) 0.0289(12) -0.0054(10) -0.0022(9) -0.0012(10) N2 0.0285(14) 0.0256(11) 0.0303(12) -0.0024(9) -0.0014(10) 0.0001(10) N3 0.0294(14) 0.0389(13) 0.0224(11) 0.0038(9) 0.0003(9) -0.0008(10) N4 0.0287(15) 0.0358(13) 0.0233(11) 0.0008(9) -0.0006(9) -0.0003(10) N5 0.0265(14) 0.0350(13) 0.0296(12) 0.0050(10) -0.0028(10) 0.0003(10) N6 0.0308(15) 0.0290(12) 0.0268(11) 0.0003(9) -0.0005(10) 0.0016(10) N7 0.0378(16) 0.0330(13) 0.0338(13) 0.0039(10) 0.0006(11) -0.0051(11) N8 0.0473(17) 0.0337(13) 0.0291(12) 0.0022(10) 0.0017(11) 0.0081(11) N9 0.043(2) 0.100(3) 0.059(2) -0.0130(19) 0.0014(16) 0.0019(17) S1 0.0371(4) 0.0264(3) 0.0261(3) -0.0033(3) -0.0027(3) 0.0059(3) S2 0.0342(5) 0.0393(4) 0.0279(3) -0.0015(3) 0.0046(3) 0.0011(3) S3 0.0359(4) 0.0250(3) 0.0295(3) 0.0017(3) -0.0058(3) -0.0032(3) S4 0.0409(5) 0.0318(4) 0.0220(3) -0.0014(3) -0.0040(3) 0.0041(3) V1 0.0274(3) 0.0230(2) 0.0207(2) -0.00034(17) -0.00139(17) 0.00027(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N3 1.520(4) . ? B1 N5 1.535(4) . ? B1 N1 1.535(4) . ? B1 H1A 1.10(3) . ? C1 N1 1.346(3) . ? C1 C2 1.360(4) . ? C1 H1 0.9300 . ? C2 C3 1.392(4) . ? C2 H2 0.9300 . ? C3 N2 1.334(3) . ? C3 H3 0.9300 . ? C4 N3 1.343(4) . ? C4 C5 1.366(4) . ? C4 H4 0.9300 . ? C5 C6 1.387(4) . ? C5 H5 0.9300 . ? C6 N4 1.334(4) . ? C6 H6 0.9300 . ? C7 N5 1.348(4) . ? C7 C8 1.369(4) . ? C7 H7 0.9300 . ? C8 C9 1.396(4) . ? C8 H8 0.9300 . ? C9 N6 1.340(4) . ? C9 H9 0.9300 . ? C10 C11 1.506(5) . ? C10 N7 1.515(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.512(5) . ? C12 N7 1.523(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.511(5) . ? C14 N7 1.518(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N7 1.506(4) . ? C16 C17 1.520(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.503(4) . ? C18 N8 1.521(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N8 1.517(4) . ? C20 C21 1.523(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.512(5) . ? C22 N8 1.515(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.513(4) . ? C24 N8 1.520(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N9 1.135(5) . ? C26 C27 1.448(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? F1 Fe1 1.8500(17) . ? F2 Fe2 1.8607(18) . ? F3 Fe3 1.8491(17) . ? Fe1 S2 2.2697(8) . ? Fe1 S1 2.2802(8) . ? Fe1 S4 2.3172(8) . ? Fe1 Fe2 2.6891(6) . ? Fe1 Fe3 2.7454(6) . ? Fe1 V1 2.8056(6) . ? Fe2 S1 2.2724(8) . ? Fe2 S3 2.2730(8) . ? Fe2 S4 2.3196(8) . ? Fe2 Fe3 2.7452(6) . ? Fe2 V1 2.8112(6) . ? Fe3 S4 2.2798(8) . ? Fe3 S2 2.2833(9) . ? Fe3 S3 2.2895(8) . ? Fe3 V1 2.8363(6) . ? N1 N2 1.364(3) . ? N2 V1 2.205(2) . ? N3 N4 1.370(3) . ? N4 V1 2.204(2) . ? N5 N6 1.366(3) . ? N6 V1 2.192(2) . ? S1 V1 2.3557(8) . ? S2 V1 2.3557(9) . ? S3 V1 2.3515(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 B1 N5 108.8(2) . . ? N3 B1 N1 107.9(2) . . ? N5 B1 N1 107.8(2) . . ? N3 B1 H1A 108.8(15) . . ? N5 B1 H1A 111.0(14) . . ? N1 B1 H1A 112.4(14) . . ? N1 C1 C2 109.1(3) . . ? N1 C1 H1 125.4 . . ? C2 C1 H1 125.4 . . ? C1 C2 C3 105.0(3) . . ? C1 C2 H2 127.5 . . ? C3 C2 H2 127.5 . . ? N2 C3 C2 110.3(3) . . ? N2 C3 H3 124.8 . . ? C2 C3 H3 124.8 . . ? N3 C4 C5 108.5(3) . . ? N3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? C4 C5 C6 105.0(3) . . ? C4 C5 H5 127.5 . . ? C6 C5 H5 127.5 . . ? N4 C6 C5 111.0(3) . . ? N4 C6 H6 124.5 . . ? C5 C6 H6 124.5 . . ? N5 C7 C8 109.2(3) . . ? N5 C7 H7 125.4 . . ? C8 C7 H7 125.4 . . ? C7 C8 C9 104.4(3) . . ? C7 C8 H8 127.8 . . ? C9 C8 H8 127.8 . . ? N6 C9 C8 110.9(3) . . ? N6 C9 H9 124.5 . . ? C8 C9 H9 124.5 . . ? C11 C10 N7 115.4(3) . . ? C11 C10 H10A 108.4 . . ? N7 C10 H10A 108.4 . . ? C11 C10 H10B 108.4 . . ? N7 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N7 115.9(3) . . ? C13 C12 H12A 108.3 . . ? N7 C12 H12A 108.3 . . ? C13 C12 H12B 108.3 . . ? N7 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 N7 115.6(3) . . ? C15 C14 H14A 108.4 . . ? N7 C14 H14A 108.4 . . ? C15 C14 H14B 108.4 . . ? N7 C14 H14B 108.4 . . ? H14A C14 H14B 107.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 C17 115.3(3) . . ? N7 C16 H16A 108.4 . . ? C17 C16 H16A 108.4 . . ? N7 C16 H16B 108.4 . . ? C17 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N8 116.3(3) . . ? C19 C18 H18A 108.2 . . ? N8 C18 H18A 108.2 . . ? C19 C18 H18B 108.2 . . ? N8 C18 H18B 108.2 . . ? H18A C18 H18B 107.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N8 C20 C21 115.6(3) . . ? N8 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? N8 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 N8 115.8(3) . . ? C23 C22 H22A 108.3 . . ? N8 C22 H22A 108.3 . . ? C23 C22 H22B 108.3 . . ? N8 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N8 114.4(3) . . ? C25 C24 H24A 108.7 . . ? N8 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? N8 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N9 C26 C27 179.1(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? F1 Fe1 S2 118.49(7) . . ? F1 Fe1 S1 109.61(6) . . ? S2 Fe1 S1 106.25(3) . . ? F1 Fe1 S4 112.42(6) . . ? S2 Fe1 S4 103.06(3) . . ? S1 Fe1 S4 106.13(3) . . ? F1 Fe1 Fe2 139.39(7) . . ? S2 Fe1 Fe2 102.11(3) . . ? S1 Fe1 Fe2 53.66(2) . . ? S4 Fe1 Fe2 54.59(2) . . ? F1 Fe1 Fe3 147.80(6) . . ? S2 Fe1 Fe3 53.14(2) . . ? S1 Fe1 Fe3 102.35(2) . . ? S4 Fe1 Fe3 52.71(2) . . ? Fe2 Fe1 Fe3 60.670(15) . . ? F1 Fe1 V1 144.32(6) . . ? S2 Fe1 V1 54.07(2) . . ? S1 Fe1 V1 54.00(2) . . ? S4 Fe1 V1 103.01(2) . . ? Fe2 Fe1 V1 61.500(15) . . ? Fe3 Fe1 V1 61.444(14) . . ? F2 Fe2 S1 111.88(6) . . ? F2 Fe2 S3 118.87(6) . . ? S1 Fe2 S3 105.82(3) . . ? F2 Fe2 S4 109.66(6) . . ? S1 Fe2 S4 106.31(3) . . ? S3 Fe2 S4 103.34(3) . . ? F2 Fe2 Fe1 139.09(6) . . ? S1 Fe2 Fe1 53.93(2) . . ? S3 Fe2 Fe1 101.98(3) . . ? S4 Fe2 Fe1 54.51(2) . . ? F2 Fe2 Fe3 145.07(6) . . ? S1 Fe2 Fe3 102.57(3) . . ? S3 Fe2 Fe3 53.29(2) . . ? S4 Fe2 Fe3 52.69(2) . . ? Fe1 Fe2 Fe3 60.679(16) . . ? F2 Fe2 V1 147.42(6) . . ? S1 Fe2 V1 53.96(2) . . ? S3 Fe2 V1 53.84(2) . . ? S4 Fe2 V1 102.78(3) . . ? Fe1 Fe2 V1 61.292(15) . . ? Fe3 Fe2 V1 61.376(15) . . ? F3 Fe3 S4 114.84(6) . . ? F3 Fe3 S2 114.60(7) . . ? S4 Fe3 S2 103.82(3) . . ? F3 Fe3 S3 112.97(7) . . ? S4 Fe3 S3 104.08(3) . . ? S2 Fe3 S3 105.38(3) . . ? F3 Fe3 Fe1 147.15(7) . . ? S4 Fe3 Fe1 53.96(2) . . ? S2 Fe3 Fe1 52.69(2) . . ? S3 Fe3 Fe1 99.87(2) . . ? F3 Fe3 Fe2 145.29(7) . . ? S4 Fe3 Fe2 54.02(2) . . ? S2 Fe3 Fe2 100.08(2) . . ? S3 Fe3 Fe2 52.73(2) . . ? Fe1 Fe3 Fe2 58.651(14) . . ? F3 Fe3 V1 142.07(6) . . ? S4 Fe3 V1 103.08(2) . . ? S2 Fe3 V1 53.48(2) . . ? S3 Fe3 V1 53.32(2) . . ? Fe1 Fe3 V1 60.325(14) . . ? Fe2 Fe3 V1 60.459(15) . . ? C1 N1 N2 109.1(2) . . ? C1 N1 B1 130.5(2) . . ? N2 N1 B1 120.3(2) . . ? C3 N2 N1 106.5(2) . . ? C3 N2 V1 131.83(19) . . ? N1 N2 V1 121.69(17) . . ? C4 N3 N4 109.9(2) . . ? C4 N3 B1 130.6(2) . . ? N4 N3 B1 119.5(2) . . ? C6 N4 N3 105.5(2) . . ? C6 N4 V1 132.08(18) . . ? N3 N4 V1 122.42(18) . . ? C7 N5 N6 109.4(2) . . ? C7 N5 B1 130.2(2) . . ? N6 N5 B1 120.4(2) . . ? C9 N6 N5 106.0(2) . . ? C9 N6 V1 132.07(19) . . ? N5 N6 V1 121.89(17) . . ? C16 N7 C10 111.1(2) . . ? C16 N7 C14 111.6(2) . . ? C10 N7 C14 105.3(2) . . ? C16 N7 C12 106.7(2) . . ? C10 N7 C12 110.6(2) . . ? C14 N7 C12 111.7(2) . . ? C22 N8 C20 108.5(2) . . ? C22 N8 C18 108.8(2) . . ? C20 N8 C18 111.5(2) . . ? C22 N8 C24 111.0(2) . . ? C20 N8 C24 108.9(3) . . ? C18 N8 C24 108.1(2) . . ? Fe2 S1 Fe1 72.41(2) . . ? Fe2 S1 V1 74.78(2) . . ? Fe1 S1 V1 74.47(3) . . ? Fe1 S2 Fe3 74.17(3) . . ? Fe1 S2 V1 74.66(3) . . ? Fe3 S2 V1 75.36(3) . . ? Fe2 S3 Fe3 73.98(2) . . ? Fe2 S3 V1 74.85(2) . . ? Fe3 S3 V1 75.33(3) . . ? Fe3 S4 Fe1 73.34(2) . . ? Fe3 S4 Fe2 73.28(2) . . ? Fe1 S4 Fe2 70.89(2) . . ? N6 V1 N4 81.34(8) . . ? N6 V1 N2 80.57(8) . . ? N4 V1 N2 81.49(9) . . ? N6 V1 S3 88.09(6) . . ? N4 V1 S3 88.04(6) . . ? N2 V1 S3 165.56(6) . . ? N6 V1 S2 88.46(6) . . ? N4 V1 S2 166.04(7) . . ? N2 V1 S2 87.49(6) . . ? S3 V1 S2 101.19(3) . . ? N6 V1 S1 165.28(6) . . ? N4 V1 S1 87.18(6) . . ? N2 V1 S1 88.68(6) . . ? S3 V1 S1 100.76(3) . . ? S2 V1 S1 101.16(3) . . ? N6 V1 Fe1 139.66(6) . . ? N4 V1 Fe1 138.66(6) . . ? N2 V1 Fe1 97.75(6) . . ? S3 V1 Fe1 96.68(2) . . ? S2 V1 Fe1 51.27(2) . . ? S1 V1 Fe1 51.54(2) . . ? N6 V1 Fe2 139.33(6) . . ? N4 V1 Fe2 97.48(6) . . ? N2 V1 Fe2 139.81(6) . . ? S3 V1 Fe2 51.30(2) . . ? S2 V1 Fe2 96.47(2) . . ? S1 V1 Fe2 51.26(2) . . ? Fe1 V1 Fe2 57.209(14) . . ? N6 V1 Fe3 96.89(6) . . ? N4 V1 Fe3 139.35(6) . . ? N2 V1 Fe3 138.64(6) . . ? S3 V1 Fe3 51.34(2) . . ? S2 V1 Fe3 51.16(2) . . ? S1 V1 Fe3 97.83(2) . . ? Fe1 V1 Fe3 58.232(15) . . ? Fe2 V1 Fe3 58.165(14) . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 0.469 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.071 data_ebdcn3final _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(n-ethylammonium) bis(\m~4~-sulfido)-hexakis(\m~3~-sulfido)-tetraazido-bis(hydrotris(pyrazolyl) borato)-hexa-iron-di-vanadium acetonitrile solvate ; _chemical_name_common 'Azide vanadium edge bridged double cubane' _chemical_melting_point 'none' _chemical_formula_moiety '(Et4N)4[(C9H10N6B)2V2Fe6S8(N3)4](CH3CN)2' _chemical_formula_sum 'C54 H106 B2 Fe6 N30 S8 V2' _chemical_formula_weight 1890.21 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' 'V' 'V' 0.3005 0.5294 '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' _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 11.867(10) _cell_length_b 20.779(19) _cell_length_c 17.148(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.134(14) _cell_angle_gamma 90.00 _cell_volume 4162(6) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 979 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.484 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5068 _exptl_absorpt_correction_T_max 0.8994 _exptl_absorpt_process_details SADABS _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_% ? _diffrn_reflns_number 23254 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.09 _reflns_number_total 7397 _reflns_number_gt 6185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+5.0561P] 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 7397 _refine_ls_number_parameters 555 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 5.808 _refine_ls_shift/su_mean 0.030 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 S1 S 0.84062(9) 0.11582(5) 0.26596(6) 0.0370(3) Uani 1 1 d . . . S2 S 0.73563(9) 0.01434(5) 0.41385(6) 0.0350(3) Uani 1 1 d . . . S3 S 1.02634(9) 0.08179(5) 0.46023(7) 0.0387(3) Uani 1 1 d . . . S4 S 0.95603(9) -0.04750(5) 0.31380(7) 0.0371(3) Uani 1 1 d . . . V1 V 0.78065(6) 0.00979(3) 0.28600(4) 0.0312(2) Uani 1 1 d . . . Fe1 Fe 0.83717(5) 0.10404(3) 0.39697(4) 0.03474(19) Uani 1 1 d . . . Fe2 Fe 0.99600(5) 0.05876(3) 0.32312(4) 0.03583(19) Uani 1 1 d . . . Fe3 Fe 0.92177(5) -0.01502(3) 0.43397(3) 0.03314(18) Uani 1 1 d . . . N1 N 0.7848(4) 0.1870(2) 0.4389(2) 0.0530(11) Uani 1 1 d . . . N2 N 0.7320(4) 0.2295(2) 0.4061(3) 0.0558(11) Uani 1 1 d . . . N3 N 0.6829(6) 0.2734(3) 0.3772(4) 0.102(2) Uani 1 1 d . . . N4 N 1.1284(3) 0.0855(2) 0.2735(3) 0.0510(10) Uani 1 1 d . . . N5 N 1.1331(4) 0.0837(3) 0.2057(3) 0.0611(12) Uani 1 1 d . . . N6 N 1.1419(5) 0.0809(4) 0.1392(4) 0.107(2) Uani 1 1 d . . . N7 N 0.6104(3) -0.09943(19) 0.2108(2) 0.0425(9) Uani 1 1 d . . . N8 N 0.6941(3) -0.08479(18) 0.2737(2) 0.0382(8) Uani 1 1 d . . . N9 N 0.5326(3) 0.0115(2) 0.1851(2) 0.0466(10) Uani 1 1 d . . . N10 N 0.6061(3) 0.04380(19) 0.2423(2) 0.0399(9) Uani 1 1 d . . . N11 N 0.6787(4) -0.0301(2) 0.1112(2) 0.0468(10) Uani 1 1 d . . . N12 N 0.7741(3) -0.00507(18) 0.1581(2) 0.0405(9) Uani 1 1 d . . . C1 C 0.5773(4) -0.1606(2) 0.2161(3) 0.0498(12) Uani 1 1 d . . . H1 H 0.5209 -0.1821 0.1790 0.060 Uiso 1 1 calc R . . C2 C 0.6375(4) -0.1869(3) 0.2834(3) 0.0520(12) Uani 1 1 d . . . H2 H 0.6315 -0.2293 0.3030 0.062 Uiso 1 1 calc R . . C3 C 0.7100(4) -0.1378(2) 0.3171(3) 0.0449(11) Uani 1 1 d . . . H3 H 0.7637 -0.1418 0.3649 0.054 Uiso 1 1 calc R . . C4 C 0.4313(4) 0.0435(3) 0.1715(3) 0.0535(13) Uani 1 1 d . . . H4 H 0.3657 0.0308 0.1346 0.064 Uiso 1 1 calc R . . C5 C 0.4378(4) 0.0960(3) 0.2185(3) 0.0562(14) Uani 1 1 d . . . H5 H 0.3796 0.1268 0.2215 0.067 Uiso 1 1 calc R . . C6 C 0.5497(4) 0.0948(3) 0.2621(3) 0.0482(12) Uani 1 1 d . . . H6 H 0.5806 0.1261 0.3004 0.058 Uiso 1 1 calc R . . C7 C 0.6961(5) -0.0337(3) 0.0359(3) 0.0588(14) Uani 1 1 d . . . H7 H 0.6431 -0.0497 -0.0078 0.071 Uiso 1 1 calc R . . C8 C 0.8033(6) -0.0104(3) 0.0332(3) 0.0631(15) Uani 1 1 d . . . H8 H 0.8393 -0.0071 -0.0119 0.076 Uiso 1 1 calc R . . C9 C 0.8480(5) 0.0073(2) 0.1105(3) 0.0487(12) Uani 1 1 d . . . H9 H 0.9216 0.0258 0.1270 0.058 Uiso 1 1 calc R . . B1 B 0.5728(5) -0.0484(3) 0.1464(3) 0.0488(14) Uani 1 1 d . . . N13 N 0.6732(4) 0.1022(2) 0.6445(3) 0.0551(11) Uani 1 1 d . . . C10 C 0.5534(5) 0.1186(4) 0.6031(4) 0.0776(19) Uani 1 1 d . . . H10A H 0.5017 0.0828 0.6113 0.093 Uiso 1 1 calc R . . H10B H 0.5273 0.1574 0.6285 0.093 Uiso 1 1 calc R . . C11 C 0.5419(6) 0.1309(4) 0.5157(4) 0.086(2) Uani 1 1 d . . . H11A H 0.5842 0.1700 0.5070 0.128 Uiso 1 1 calc R . . H11B H 0.4608 0.1365 0.4926 0.128 Uiso 1 1 calc R . . H11C H 0.5730 0.0943 0.4904 0.128 Uiso 1 1 calc R . . C12 C 0.7184(5) 0.0449(3) 0.6109(3) 0.0654(16) Uani 1 1 d . . . H12A H 0.7943 0.0347 0.6426 0.078 Uiso 1 1 calc R . . H12B H 0.7300 0.0551 0.5565 0.078 Uiso 1 1 calc R . . C13 C 0.6450(7) -0.0137(3) 0.6076(5) 0.088(2) Uani 1 1 d . . . H13A H 0.6363 -0.0259 0.6614 0.132 Uiso 1 1 calc R . . H13B H 0.6809 -0.0491 0.5831 0.132 Uiso 1 1 calc R . . H13C H 0.5696 -0.0045 0.5760 0.132 Uiso 1 1 calc R . . C14 C 0.6670(6) 0.0927(3) 0.7306(3) 0.0696(16) Uani 1 1 d . . . H14A H 0.6123 0.0574 0.7347 0.084 Uiso 1 1 calc R . . H14B H 0.6351 0.1324 0.7502 0.084 Uiso 1 1 calc R . . C15 C 0.7785(6) 0.0773(4) 0.7849(4) 0.082(2) Uani 1 1 d . . . H15A H 0.8078 0.0360 0.7695 0.123 Uiso 1 1 calc R . . H15B H 0.7655 0.0747 0.8397 0.123 Uiso 1 1 calc R . . H15C H 0.8345 0.1112 0.7807 0.123 Uiso 1 1 calc R . . C16 C 0.7570(6) 0.1562(3) 0.6359(4) 0.081(2) Uani 1 1 d . . . H16A H 0.7556 0.1641 0.5788 0.097 Uiso 1 1 calc R . . H16B H 0.8352 0.1419 0.6594 0.097 Uiso 1 1 calc R . . C17 C 0.7320(10) 0.2201(4) 0.6751(6) 0.135(4) Uani 1 1 d . . . H17A H 0.6543 0.2345 0.6529 0.202 Uiso 1 1 calc R . . H17B H 0.7872 0.2528 0.6651 0.202 Uiso 1 1 calc R . . H17C H 0.7385 0.2137 0.7324 0.202 Uiso 1 1 calc R . . N14 N 0.4699(8) 0.2052(5) 0.0385(7) 0.160(4) Uani 1 1 d . . . C18 C 0.5501(9) 0.1734(4) 0.0467(5) 0.107(3) Uani 1 1 d . . . C19 C 0.6498(8) 0.1338(4) 0.0584(5) 0.105(3) Uani 1 1 d . . . H19A H 0.7092 0.1541 0.0335 0.157 Uiso 1 1 calc R . . H19B H 0.6307 0.0915 0.0343 0.157 Uiso 1 1 calc R . . H19C H 0.6781 0.1286 0.1152 0.157 Uiso 1 1 calc R . . N15 N 0.0995(11) 0.2815(6) 0.4099(8) 0.028(4) Uani 0.351(2) 1 d PD A 1 C20 C 0.0252(8) 0.2476(5) 0.3407(6) 0.081(3) Uani 0.702(5) 1 d PD A 1 H20A H -0.0555 0.2559 0.3453 0.098 Uiso 0.702(5) 1 calc PR A 1 H20B H 0.0381 0.2008 0.3487 0.098 Uiso 0.702(5) 1 calc PR A 1 C21 C 0.037(2) 0.2625(9) 0.2552(10) 0.042(5) Uani 0.351(2) 1 d PD A 1 H21A H 0.0330 0.3092 0.2467 0.062 Uiso 0.351(2) 1 calc PR A 1 H21B H -0.0249 0.2415 0.2189 0.062 Uiso 0.351(2) 1 calc PR A 1 H21C H 0.1110 0.2465 0.2453 0.062 Uiso 0.351(2) 1 calc PR A 1 C22 C 0.2235(10) 0.2781(5) 0.3976(7) 0.078(3) Uani 0.702(5) 1 d PD A 1 H22A H 0.2724 0.2985 0.4437 0.093 Uiso 0.702(5) 1 calc PR A 1 H22B H 0.2308 0.3040 0.3503 0.093 Uiso 0.702(5) 1 calc PR A 1 C23 C 0.2705(14) 0.2104(9) 0.3868(15) 0.051(6) Uani 0.351(2) 1 d PD A 1 H23A H 0.2734 0.1858 0.4359 0.076 Uiso 0.351(2) 1 calc PR A 1 H23B H 0.3478 0.2139 0.3743 0.076 Uiso 0.351(2) 1 calc PR A 1 H23C H 0.2205 0.1885 0.3434 0.076 Uiso 0.351(2) 1 calc PR A 1 C24 C 0.0889(12) 0.2500(6) 0.4855(7) 0.098(4) Uani 0.702(5) 1 d PD A 1 H24A H 0.1064 0.2037 0.4809 0.117 Uiso 0.702(5) 1 calc PR A 1 H24B H 0.0081 0.2533 0.4925 0.117 Uiso 0.702(5) 1 calc PR A 1 C25 C 0.1636(15) 0.2757(11) 0.5599(10) 0.053(5) Uani 0.351(2) 1 d PD A 1 H25A H 0.2439 0.2749 0.5533 0.080 Uiso 0.351(2) 1 calc PR A 1 H25B H 0.1540 0.2487 0.6052 0.080 Uiso 0.351(2) 1 calc PR A 1 H25C H 0.1411 0.3200 0.5693 0.080 Uiso 0.351(2) 1 calc PR A 1 C26 C 0.0755(10) 0.3539(5) 0.4092(10) 0.110(4) Uani 0.702(5) 1 d PD A 1 H26A H 0.1413 0.3763 0.4413 0.132 Uiso 0.702(5) 1 calc PR A 1 H26B H 0.0670 0.3701 0.3542 0.132 Uiso 0.702(5) 1 calc PR A 1 C27 C -0.0323(14) 0.3692(9) 0.4418(13) 0.068(6) Uani 0.351(2) 1 d PD A 1 H27A H -0.0490 0.3337 0.4757 0.102 Uiso 0.351(2) 1 calc PR A 1 H27B H -0.0966 0.3747 0.3979 0.102 Uiso 0.351(2) 1 calc PR A 1 H27C H -0.0210 0.4089 0.4729 0.102 Uiso 0.351(2) 1 calc PR A 1 N15' N 0.1394(11) 0.2754(7) 0.4088(9) 0.028(4) Uani 0.351(2) 1 d PD A 2 C20' C 0.1259(12) 0.3164(6) 0.3382(8) 0.124(5) Uani 0.702(5) 1 d PD A 2 H20C H 0.2023 0.3261 0.3255 0.149 Uiso 0.702(5) 1 calc PR A 2 H20D H 0.0900 0.3576 0.3495 0.149 Uiso 0.702(5) 1 calc PR A 2 C21' C 0.0522(19) 0.2844(8) 0.2667(10) 0.033(4) Uani 0.351(2) 1 d PD A 2 H21D H 0.0891 0.2445 0.2539 0.049 Uiso 0.351(2) 1 calc PR A 2 H21E H 0.0437 0.3136 0.2212 0.049 Uiso 0.351(2) 1 calc PR A 2 H21F H -0.0234 0.2744 0.2791 0.049 Uiso 0.351(2) 1 calc PR A 2 C22' C 0.1934(17) 0.2088(5) 0.3983(8) 0.144(8) Uani 0.702(5) 1 d PD A 2 H22C H 0.1985 0.1848 0.4486 0.173 Uiso 0.702(5) 1 calc PR A 2 H22D H 0.1409 0.1847 0.3572 0.173 Uiso 0.702(5) 1 calc PR A 2 C23' C 0.3074(15) 0.2097(11) 0.3761(17) 0.048(5) Uani 0.351(2) 1 d PD A 2 H23D H 0.3051 0.2357 0.3281 0.071 Uiso 0.351(2) 1 calc PR A 2 H23E H 0.3304 0.1656 0.3660 0.071 Uiso 0.351(2) 1 calc PR A 2 H23F H 0.3627 0.2284 0.4193 0.071 Uiso 0.351(2) 1 calc PR A 2 C24' C 0.2151(14) 0.3064(7) 0.4783(9) 0.155(7) Uani 0.702(5) 1 d PD A 2 H24C H 0.1840 0.3498 0.4854 0.185 Uiso 0.702(5) 1 calc PR A 2 H24D H 0.2917 0.3124 0.4640 0.185 Uiso 0.702(5) 1 calc PR A 2 C25' C 0.232(2) 0.2725(12) 0.5578(11) 0.081(7) Uani 0.351(2) 1 d PD A 2 H25D H 0.1598 0.2737 0.5787 0.121 Uiso 0.351(2) 1 calc PR A 2 H25E H 0.2919 0.2942 0.5949 0.121 Uiso 0.351(2) 1 calc PR A 2 H25F H 0.2535 0.2276 0.5513 0.121 Uiso 0.351(2) 1 calc PR A 2 C26' C 0.0258(16) 0.2685(8) 0.4309(10) 0.171(10) Uani 0.702(5) 1 d PD A 2 H26C H 0.0326 0.2355 0.4730 0.205 Uiso 0.702(5) 1 calc PR A 2 H26D H -0.0261 0.2508 0.3843 0.205 Uiso 0.702(5) 1 calc PR A 2 C27' C -0.0361(16) 0.3284(10) 0.4606(13) 0.074(5) Uani 0.351(2) 1 d PD A 2 H27D H 0.0110 0.3457 0.5087 0.111 Uiso 0.351(2) 1 calc PR A 2 H27E H -0.1107 0.3151 0.4722 0.111 Uiso 0.351(2) 1 calc PR A 2 H27F H -0.0472 0.3615 0.4193 0.111 Uiso 0.351(2) 1 calc PR A 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 S1 0.0332(5) 0.0374(6) 0.0383(6) 0.0039(4) 0.0005(4) 0.0018(4) S2 0.0267(5) 0.0432(6) 0.0340(5) 0.0003(4) 0.0017(4) 0.0032(4) S3 0.0333(6) 0.0322(5) 0.0443(6) 0.0032(4) -0.0101(5) -0.0029(4) S4 0.0238(5) 0.0372(6) 0.0488(6) -0.0053(5) 0.0023(4) 0.0030(4) V1 0.0217(4) 0.0372(4) 0.0328(4) -0.0012(3) -0.0006(3) 0.0017(3) Fe1 0.0309(3) 0.0343(3) 0.0364(3) -0.0005(2) -0.0014(3) 0.0046(2) Fe2 0.0240(3) 0.0369(3) 0.0454(4) -0.0007(3) 0.0028(3) -0.0005(2) Fe3 0.0245(3) 0.0325(3) 0.0384(3) 0.0006(2) -0.0056(3) -0.0002(2) N1 0.067(3) 0.042(2) 0.049(2) -0.0005(19) 0.007(2) 0.014(2) N2 0.054(3) 0.054(3) 0.059(3) -0.001(2) 0.008(2) 0.016(2) N3 0.098(5) 0.082(4) 0.115(5) 0.018(4) -0.010(4) 0.044(4) N4 0.034(2) 0.064(3) 0.057(3) -0.006(2) 0.0119(19) -0.0072(19) N5 0.031(2) 0.085(3) 0.068(3) -0.001(3) 0.010(2) 0.001(2) N6 0.069(4) 0.198(8) 0.059(4) -0.002(4) 0.020(3) 0.004(4) N7 0.0275(18) 0.053(2) 0.046(2) -0.0108(18) 0.0028(16) -0.0056(17) N8 0.0272(18) 0.046(2) 0.0393(19) -0.0026(17) 0.0002(15) -0.0024(16) N9 0.030(2) 0.064(3) 0.041(2) 0.0005(18) -0.0068(17) 0.0021(18) N10 0.0261(18) 0.054(2) 0.0370(19) -0.0004(17) -0.0020(15) 0.0014(16) N11 0.046(2) 0.057(2) 0.0341(19) -0.0066(18) -0.0003(17) -0.0049(19) N12 0.037(2) 0.047(2) 0.0362(19) -0.0044(16) 0.0029(17) -0.0017(17) C1 0.035(2) 0.052(3) 0.064(3) -0.016(2) 0.014(2) -0.011(2) C2 0.041(3) 0.043(3) 0.073(3) -0.004(2) 0.014(3) -0.007(2) C3 0.035(2) 0.047(3) 0.052(3) 0.000(2) 0.004(2) -0.004(2) C4 0.028(2) 0.077(4) 0.049(3) 0.013(3) -0.009(2) 0.005(2) C5 0.032(2) 0.071(4) 0.063(3) 0.011(3) 0.001(2) 0.015(2) C6 0.035(2) 0.055(3) 0.053(3) 0.004(2) 0.003(2) 0.012(2) C7 0.068(4) 0.069(3) 0.037(3) -0.010(2) 0.005(3) -0.006(3) C8 0.080(4) 0.068(4) 0.045(3) -0.005(3) 0.023(3) -0.006(3) C9 0.046(3) 0.051(3) 0.053(3) -0.005(2) 0.019(2) -0.006(2) B1 0.036(3) 0.067(4) 0.041(3) -0.007(3) 0.000(2) -0.005(3) N13 0.041(2) 0.071(3) 0.054(2) 0.000(2) 0.009(2) 0.010(2) C10 0.038(3) 0.098(5) 0.095(5) -0.014(4) 0.004(3) 0.020(3) C11 0.067(4) 0.094(5) 0.084(5) -0.009(4) -0.019(4) 0.018(4) C12 0.055(3) 0.088(4) 0.051(3) -0.012(3) 0.004(3) 0.015(3) C13 0.096(6) 0.073(4) 0.085(5) -0.003(4) -0.009(4) -0.008(4) C14 0.072(4) 0.086(4) 0.055(3) -0.006(3) 0.022(3) 0.006(3) C15 0.094(5) 0.095(5) 0.054(3) 0.001(3) 0.009(3) 0.013(4) C16 0.070(4) 0.088(5) 0.076(4) 0.019(4) -0.006(3) -0.022(4) C17 0.162(10) 0.063(5) 0.152(9) -0.003(5) -0.047(7) -0.007(5) N14 0.114(7) 0.125(7) 0.211(11) 0.042(7) -0.054(7) 0.008(6) C18 0.114(7) 0.068(4) 0.113(6) 0.016(4) -0.049(5) -0.005(5) C19 0.124(7) 0.084(5) 0.088(5) -0.007(4) -0.032(5) 0.024(5) N15 0.000(8) 0.028(6) 0.065(8) 0.003(5) 0.030(6) -0.004(6) C20 0.065(6) 0.067(6) 0.110(8) 0.010(5) 0.009(6) -0.013(5) C21 0.046(10) 0.030(12) 0.045(10) -0.004(8) -0.001(8) -0.023(9) C22 0.080(8) 0.066(6) 0.084(7) -0.006(5) 0.005(6) -0.004(5) C23 0.000(10) 0.065(10) 0.094(16) 0.022(10) 0.029(10) 0.004(9) C24 0.125(10) 0.078(7) 0.103(9) 0.000(6) 0.055(8) -0.017(7) C25 0.053(10) 0.065(11) 0.038(8) -0.014(7) -0.002(8) -0.017(9) C26 0.089(8) 0.052(6) 0.188(14) 0.000(7) 0.023(9) 0.003(5) C27 0.047(10) 0.042(9) 0.116(16) -0.009(10) 0.017(10) 0.016(8) N15' 0.000(8) 0.035(6) 0.053(7) 0.000(5) 0.019(6) -0.006(6) C20' 0.095(9) 0.103(10) 0.173(14) 0.030(10) 0.017(9) 0.001(8) C21' 0.036(9) 0.025(10) 0.029(7) -0.004(6) -0.016(6) -0.009(8) C22' 0.30(3) 0.047(6) 0.078(8) 0.010(6) 0.023(13) -0.006(12) C23' 0.000(9) 0.051(9) 0.103(13) 0.024(8) 0.041(10) 0.004(7) C24' 0.136(13) 0.103(10) 0.195(18) -0.032(11) -0.052(13) 0.008(9) C25' 0.110(19) 0.068(12) 0.049(11) 0.012(9) -0.025(13) -0.010(15) C26' 0.27(3) 0.123(14) 0.099(12) -0.023(10) -0.036(15) 0.076(17) C27' 0.046(10) 0.092(15) 0.085(14) -0.027(13) 0.014(9) 0.003(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 Fe2 2.2651(18) . ? S1 Fe1 2.267(2) . ? S1 V1 2.359(2) . ? S2 Fe3 2.259(2) . ? S2 Fe1 2.266(2) . ? S2 V1 2.348(2) . ? S3 Fe3 2.2809(19) 3_756 ? S3 Fe1 2.361(2) . ? S3 Fe2 2.364(2) . ? S3 Fe3 2.365(2) . ? S4 Fe2 2.258(2) . ? S4 Fe3 2.272(2) . ? S4 V1 2.372(2) . ? V1 N10 2.192(4) . ? V1 N12 2.202(4) . ? V1 N8 2.210(4) . ? V1 Fe2 2.720(2) . ? V1 Fe1 2.7308(19) . ? V1 Fe3 2.831(2) . ? Fe1 N1 2.008(4) . ? Fe1 Fe2 2.6233(18) . ? Fe1 Fe3 2.703(2) . ? Fe2 N4 1.993(4) . ? Fe2 Fe3 2.7072(18) . ? Fe3 S3 2.2809(19) 3_756 ? Fe3 Fe3 2.736(2) 3_756 ? N1 N2 1.168(6) . ? N2 N3 1.147(7) . ? N4 N5 1.174(7) . ? N5 N6 1.165(8) . ? N7 C1 1.338(6) . ? N7 N8 1.366(5) . ? N7 B1 1.540(7) . ? N8 C3 1.323(6) . ? N9 C4 1.357(6) . ? N9 N10 1.369(5) . ? N9 B1 1.525(7) . ? N10 C6 1.330(6) . ? N11 C7 1.345(7) . ? N11 N12 1.370(5) . ? N11 B1 1.535(7) . ? N12 C9 1.324(6) . ? C1 C2 1.361(8) . ? C2 C3 1.393(7) . ? C4 C5 1.351(8) . ? C5 C6 1.405(7) . ? C7 C8 1.370(9) . ? C8 C9 1.389(8) . ? N13 C12 1.465(7) . ? N13 C14 1.504(7) . ? N13 C10 1.513(7) . ? N13 C16 1.524(8) . ? C10 C11 1.504(10) . ? C12 C13 1.491(10) . ? C14 C15 1.513(9) . ? C16 C17 1.541(12) . ? N14 C18 1.146(12) . ? C18 C19 1.426(12) . ? N15 C24 1.477(15) . ? N15 C20 1.521(14) . ? N15 C22 1.525(12) . ? N15 C26 1.530(14) . ? C20 C21 1.530(17) . ? C22 C23 1.536(16) . ? C24 C25 1.516(15) . ? C26 C27 1.517(16) . ? N15' C20' 1.465(15) . ? N15' C26' 1.471(16) . ? N15' C24' 1.505(15) . ? N15' C22' 1.548(15) . ? C20' C21' 1.527(15) . ? C22' C23' 1.469(15) . ? C24' C25' 1.517(17) . ? C26' C27' 1.573(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe2 S1 Fe1 70.73(5) . . ? Fe2 S1 V1 72.03(6) . . ? Fe1 S1 V1 72.32(4) . . ? Fe3 S2 Fe1 73.38(6) . . ? Fe3 S2 V1 75.80(5) . . ? Fe1 S2 V1 72.56(4) . . ? Fe3 S3 Fe1 125.90(6) 3_756 . ? Fe3 S3 Fe2 129.83(7) 3_756 . ? Fe1 S3 Fe2 67.45(4) . . ? Fe3 S3 Fe3 72.13(6) 3_756 . ? Fe1 S3 Fe3 69.78(6) . . ? Fe2 S3 Fe3 69.85(4) . . ? Fe2 S4 Fe3 73.40(4) . . ? Fe2 S4 V1 71.91(6) . . ? Fe3 S4 V1 75.08(5) . . ? N10 V1 N12 80.76(14) . . ? N10 V1 N8 81.89(15) . . ? N12 V1 N8 81.15(14) . . ? N10 V1 S2 87.11(11) . . ? N12 V1 S2 164.04(11) . . ? N8 V1 S2 86.94(10) . . ? N10 V1 S1 86.58(12) . . ? N12 V1 S1 86.82(11) . . ? N8 V1 S1 164.50(10) . . ? S2 V1 S1 102.85(5) . . ? N10 V1 S4 166.75(11) . . ? N12 V1 S4 90.32(11) . . ? N8 V1 S4 87.09(12) . . ? S2 V1 S4 99.69(5) . . ? S1 V1 S4 102.80(7) . . ? N10 V1 Fe2 138.74(12) . . ? N12 V1 Fe2 98.76(11) . . ? N8 V1 Fe2 139.15(10) . . ? S2 V1 Fe2 97.19(5) . . ? S1 V1 Fe2 52.38(3) . . ? S4 V1 Fe2 52.10(6) . . ? N10 V1 Fe1 96.22(11) . . ? N12 V1 Fe1 139.08(11) . . ? N8 V1 Fe1 139.21(11) . . ? S2 V1 Fe1 52.33(5) . . ? S1 V1 Fe1 52.28(6) . . ? S4 V1 Fe1 96.93(5) . . ? Fe2 V1 Fe1 57.53(3) . . ? N10 V1 Fe3 137.68(10) . . ? N12 V1 Fe3 141.13(11) . . ? N8 V1 Fe3 96.61(10) . . ? S2 V1 Fe3 50.68(6) . . ? S1 V1 Fe3 98.89(4) . . ? S4 V1 Fe3 50.85(4) . . ? Fe2 V1 Fe3 58.34(4) . . ? Fe1 V1 Fe3 58.13(5) . . ? N1 Fe1 S2 117.10(15) . . ? N1 Fe1 S1 108.85(13) . . ? S2 Fe1 S1 108.55(5) . . ? N1 Fe1 S3 109.42(14) . . ? S2 Fe1 S3 105.32(6) . . ? S1 Fe1 S3 107.15(6) . . ? N1 Fe1 Fe2 140.78(14) . . ? S2 Fe1 Fe2 102.12(6) . . ? S1 Fe1 Fe2 54.59(4) . . ? S3 Fe1 Fe2 56.33(6) . . ? N1 Fe1 Fe3 145.80(13) . . ? S2 Fe1 Fe3 53.20(6) . . ? S1 Fe1 Fe3 105.11(4) . . ? S3 Fe1 Fe3 55.18(3) . . ? Fe2 Fe1 Fe3 61.07(4) . . ? N1 Fe1 V1 144.28(13) . . ? S2 Fe1 V1 55.11(6) . . ? S1 Fe1 V1 55.39(5) . . ? S3 Fe1 V1 106.07(5) . . ? Fe2 Fe1 V1 61.03(5) . . ? Fe3 Fe1 V1 62.79(6) . . ? N4 Fe2 S4 114.48(14) . . ? N4 Fe2 S1 108.18(15) . . ? S4 Fe2 S1 109.66(6) . . ? N4 Fe2 S3 111.98(14) . . ? S4 Fe2 S3 105.17(5) . . ? S1 Fe2 S3 107.12(5) . . ? N4 Fe2 Fe1 142.48(14) . . ? S4 Fe2 Fe1 103.01(5) . . ? S1 Fe2 Fe1 54.67(6) . . ? S3 Fe2 Fe1 56.22(5) . . ? N4 Fe2 Fe3 146.73(14) . . ? S4 Fe2 Fe3 53.54(5) . . ? S1 Fe2 Fe3 105.05(6) . . ? S3 Fe2 Fe3 55.09(6) . . ? Fe1 Fe2 Fe3 60.92(5) . . ? N4 Fe2 V1 141.57(14) . . ? S4 Fe2 V1 55.99(3) . . ? S1 Fe2 V1 55.58(6) . . ? S3 Fe2 V1 106.31(4) . . ? Fe1 Fe2 V1 61.44(6) . . ? Fe3 Fe2 V1 62.88(4) . . ? S2 Fe3 S4 105.54(5) . . ? S2 Fe3 S3 113.93(5) . 3_756 ? S4 Fe3 S3 118.32(7) . 3_756 ? S2 Fe3 S3 105.40(7) . . ? S4 Fe3 S3 104.70(5) . . ? S3 Fe3 S3 107.87(6) 3_756 . ? S2 Fe3 Fe1 53.43(3) . . ? S4 Fe3 Fe1 100.21(5) . . ? S3 Fe3 Fe1 141.31(5) 3_756 . ? S3 Fe3 Fe1 55.04(6) . . ? S2 Fe3 Fe2 99.79(5) . . ? S4 Fe3 Fe2 53.07(6) . . ? S3 Fe3 Fe2 145.82(5) 3_756 . ? S3 Fe3 Fe2 55.06(5) . . ? Fe1 Fe3 Fe2 58.01(4) . . ? S2 Fe3 Fe3 124.60(6) . 3_756 ? S4 Fe3 Fe3 127.94(7) . 3_756 ? S3 Fe3 Fe3 55.36(6) 3_756 3_756 ? S3 Fe3 Fe3 52.51(4) . 3_756 ? Fe1 Fe3 Fe3 98.94(5) . 3_756 ? Fe2 Fe3 Fe3 101.22(7) . 3_756 ? S2 Fe3 V1 53.53(4) . . ? S4 Fe3 V1 54.07(6) . . ? S3 Fe3 V1 149.10(4) 3_756 . ? S3 Fe3 V1 102.92(5) . . ? Fe1 Fe3 V1 59.08(3) . . ? Fe2 Fe3 V1 58.78(6) . . ? Fe3 Fe3 V1 155.31(5) 3_756 . ? N2 N1 Fe1 130.5(4) . . ? N3 N2 N1 176.2(6) . . ? N5 N4 Fe2 126.3(4) . . ? N6 N5 N4 177.4(6) . . ? C1 N7 N8 109.9(4) . . ? C1 N7 B1 130.6(4) . . ? N8 N7 B1 119.5(4) . . ? C3 N8 N7 105.7(4) . . ? C3 N8 V1 132.0(3) . . ? N7 N8 V1 122.3(3) . . ? C4 N9 N10 108.4(4) . . ? C4 N9 B1 131.3(4) . . ? N10 N9 B1 120.2(4) . . ? C6 N10 N9 106.8(4) . . ? C6 N10 V1 131.1(3) . . ? N9 N10 V1 122.1(3) . . ? C7 N11 N12 109.6(4) . . ? C7 N11 B1 129.6(4) . . ? N12 N11 B1 120.8(4) . . ? C9 N12 N11 106.3(4) . . ? C9 N12 V1 132.5(3) . . ? N11 N12 V1 121.2(3) . . ? N7 C1 C2 108.8(4) . . ? C1 C2 C3 104.5(5) . . ? N8 C3 C2 111.1(4) . . ? C5 C4 N9 109.7(4) . . ? C4 C5 C6 104.6(5) . . ? N10 C6 C5 110.4(5) . . ? N11 C7 C8 108.2(5) . . ? C7 C8 C9 105.2(5) . . ? N12 C9 C8 110.7(5) . . ? N9 B1 N11 108.0(4) . . ? N9 B1 N7 108.9(4) . . ? N11 B1 N7 107.4(4) . . ? C12 N13 C14 111.4(5) . . ? C12 N13 C10 112.2(5) . . ? C14 N13 C10 106.6(5) . . ? C12 N13 C16 105.7(5) . . ? C14 N13 C16 109.7(5) . . ? C10 N13 C16 111.3(5) . . ? C11 C10 N13 114.8(5) . . ? N13 C12 C13 115.2(6) . . ? N13 C14 C15 116.3(5) . . ? N13 C16 C17 114.4(7) . . ? N14 C18 C19 179.0(12) . . ? C24 N15 C20 110.6(10) . . ? C24 N15 C22 109.5(11) . . ? C20 N15 C22 108.1(10) . . ? C24 N15 C26 113.5(12) . . ? C20 N15 C26 111.5(11) . . ? C22 N15 C26 103.1(9) . . ? N15 C20 C21 121.0(10) . . ? N15 C22 C23 116.0(11) . . ? N15 C24 C25 117.1(12) . . ? C27 C26 N15 111.8(11) . . ? C20' N15' C26' 107.3(13) . . ? C20' N15' C24' 111.7(12) . . ? C26' N15' C24' 106.5(14) . . ? C20' N15' C22' 114.3(12) . . ? C26' N15' C22' 111.1(13) . . ? C24' N15' C22' 105.8(12) . . ? N15' C20' C21' 112.0(12) . . ? C23' C22' N15' 116.0(15) . . ? N15' C24' C25' 118.6(15) . . ? N15' C26' C27' 120.5(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.919 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.132 5