Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Davies, Sian C.' 'Hughes, David L.' 'Richards, Raymond L.' 'Sanders, John' _publ_contact_author_name 'David L Hughes' _publ_contact_author_address ; David L Hughes Department of Biological Chemistry John Innes Centre Norwich NR4 7UH UNITED KINGDOM ; _publ_contact_author_email 'DAVID.HUGHES@BBSRC.AC.UK' _publ_section_title ; Dinuclear iron and vanadium complexes of the N(CH2CH2S)3 3-ligand with bridging oxide, nitride or cyanide ; data_roger29 _database_code_CSD 169282 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 1' _chemical_formula_moiety '2(C8 H20 N), C12 H24 Fe2 N2 O S6, C2 H3 N' _chemical_formula_structural '(NEt4)2[(Fe{N(CH2CH2S)3})2(mu-O)]' _chemical_formula_analytical ? _chemical_formula_sum 'C30 H67 Fe2 N5 O S6' _chemical_formula_weight 817.95 _chemical_melting_point ? _chemical_compound_source ? 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' #(no. 14) 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 16.9292(15) _cell_length_b 11.2912(10) _cell_length_c 22.060(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.207(7) _cell_angle_gamma 90.00 _cell_volume 4213.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'square and hexagonal prisms' _exptl_crystal_colour 'Reddish brown' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method ? _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.993 _exptl_absorpt_correction_T_max 0.987 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 11.0 _diffrn_reflns_number 8213 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25 _reflns_number_total 7390 _reflns_number_observed 4389 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+1.1454P] 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 ; Coordinates were of idealised positions and set to ride on the parent carbon atoms. Isotropic thermal parameters of the ethylene hydrogens were set to be 1.2 x Ueq of the parent carbon atoms and those of the methyl hydrogens were set to be 1.5 x Ueq of the parent atoms. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7390 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_obs 0.0417 _refine_ls_wR_factor_all 0.1095 _refine_ls_wR_factor_obs 0.0889 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.137 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.137 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.63936(3) 0.82137(5) 0.12970(2) 0.04016(15) Uani 1 d . . S1 S 0.62911(6) 0.76820(11) 0.02684(4) 0.0606(3) Uani 1 d . . C11 C 0.5246(3) 0.7488(5) 0.0130(2) 0.0757(14) Uani 1 d . . H11A H 0.5120(3) 0.7647(5) -0.0295(2) 0.091 Uiso 0.80 calc PR 1 H11B H 0.5113(3) 0.6667(5) 0.0206(2) 0.091 Uiso 0.80 calc PR 1 H11C H 0.5046(3) 0.8167(5) -0.0098(2) 0.091 Uiso 0.20 calc PR 2 H11D H 0.5165(3) 0.6795(5) -0.0125(2) 0.091 Uiso 0.20 calc PR 2 C12 C 0.4754(3) 0.8238(7) 0.0495(2) 0.075(2) Uani 0.80 d P 1 H12A H 0.4208(3) 0.7989(7) 0.0435(2) 0.090 Uiso 0.80 calc PR 1 H12B H 0.4790(3) 0.9046(7) 0.0349(2) 0.090 Uiso 0.80 calc PR 1 C12B C 0.4763(11) 0.7346(20) 0.0680(9) 0.048(5) Uiso 0.20 d P 2 H12C H 0.4207(11) 0.7415(20) 0.0561(9) 0.057 Uiso 0.20 calc PR 2 H12D H 0.4849(11) 0.6559(20) 0.0846(9) 0.057 Uiso 0.20 calc PR 2 S2 S 0.60570(6) 0.67956(10) 0.20235(5) 0.0566(3) Uani 1 d . . C21 C 0.4999(3) 0.6851(5) 0.2018(2) 0.092(2) Uani 1 d . . H21A H 0.4802(3) 0.6081(5) 0.2137(2) 0.110 Uiso 0.80 calc PR 1 H21B H 0.4841(3) 0.7421(5) 0.2319(2) 0.110 Uiso 0.80 calc PR 1 H21C H 0.4793(3) 0.6182(5) 0.1786(2) 0.110 Uiso 0.20 calc PR 2 H21D H 0.4833(3) 0.6757(5) 0.2431(2) 0.110 Uiso 0.20 calc PR 2 C22 C 0.4629(3) 0.7173(7) 0.1428(3) 0.099(3) Uani 0.80 d P 1 H22A H 0.4684(3) 0.6514(7) 0.1151(3) 0.118 Uiso 0.80 calc PR 1 H22B H 0.4069(3) 0.7298(7) 0.1478(3) 0.118 Uiso 0.80 calc PR 1 C22B C 0.4644(11) 0.7930(18) 0.1768(9) 0.043(5) Uiso 0.20 d P 2 H22C H 0.4754(11) 0.8582(18) 0.2045(9) 0.052 Uiso 0.20 calc PR 2 H22D H 0.4075(11) 0.7831(18) 0.1730(9) 0.052 Uiso 0.20 calc PR 2 S3 S 0.61522(7) 1.01889(10) 0.15355(6) 0.0680(3) Uani 1 d . . C31 C 0.5110(3) 1.0356(5) 0.1370(3) 0.096(2) Uani 1 d . . H31A H 0.4908(3) 1.0966(5) 0.1632(3) 0.115 Uiso 0.80 calc PR 1 H31B H 0.5034(3) 1.0627(5) 0.0954(3) 0.115 Uiso 0.80 calc PR 1 H31C H 0.4844(3) 1.0355(5) 0.1751(3) 0.115 Uiso 0.20 calc PR 2 H31D H 0.5025(3) 1.1128(5) 0.1186(3) 0.115 Uiso 0.20 calc PR 2 C32 C 0.4647(4) 0.9275(7) 0.1447(4) 0.096(2) Uani 0.80 d P 1 H32A H 0.4615(4) 0.9114(7) 0.1877(4) 0.115 Uiso 0.80 calc PR 1 H32B H 0.4113(4) 0.9414(7) 0.1287(4) 0.115 Uiso 0.80 calc PR 1 C32B C 0.4742(11) 0.9501(17) 0.0987(9) 0.044(5) Uiso 0.20 d P 2 H32C H 0.4888(11) 0.9649(17) 0.0573(9) 0.053 Uiso 0.20 calc PR 2 H32D H 0.4173(11) 0.9593(17) 0.1002(9) 0.053 Uiso 0.20 calc PR 2 N10 N 0.4958(2) 0.8229(3) 0.11537(14) 0.0533(8) Uani 1 d . . O12 O 0.74492(13) 0.8153(2) 0.14292(11) 0.0527(7) Uani 1 d . . Fe2 Fe 0.84900(3) 0.83081(5) 0.13335(2) 0.03973(15) Uani 1 d . . S4 S 0.85180(6) 0.75606(11) 0.03453(4) 0.0574(3) Uani 1 d . . C41 C 0.9567(3) 0.7538(5) 0.0203(2) 0.084(2) Uani 1 d . . H41A H 0.9781(3) 0.6772(5) 0.0322(2) 0.101 Uiso 0.90 calc PR 3 H41B H 0.9636(3) 0.7630(5) -0.0229(2) 0.101 Uiso 0.90 calc PR 3 H41C H 0.9657(3) 0.6878(5) -0.0068(2) 0.101 Uiso 0.10 calc PR 4 H41D H 0.9684(3) 0.8254(5) -0.0019(2) 0.101 Uiso 0.10 calc PR 4 C42 C 1.0024(3) 0.8481(6) 0.0533(2) 0.080(2) Uani 0.90 d P 3 H42A H 1.0582(3) 0.8355(6) 0.0473(2) 0.095 Uiso 0.90 calc PR 3 H42B H 0.9882(3) 0.9241(6) 0.0355(2) 0.095 Uiso 0.90 calc PR 3 C42B C 1.0109(22) 0.7454(38) 0.0668(17) 0.046(9) Uiso 0.10 d P 4 H42C H 1.0638(22) 0.7561(38) 0.0522(17) 0.055 Uiso 0.10 calc PR 4 H42D H 1.0080(22) 0.6682(38) 0.0859(17) 0.055 Uiso 0.10 calc PR 4 S5 S 0.90037(6) 0.70635(10) 0.21055(5) 0.0588(3) Uani 1 d . . C51 C 1.0051(3) 0.7319(5) 0.2105(2) 0.092(2) Uani 1 d . . H51A H 1.0182(3) 0.7966(5) 0.2380(2) 0.111 Uiso 0.90 calc PR 3 H51B H 1.0322(3) 0.6617(5) 0.2257(2) 0.111 Uiso 0.90 calc PR 3 H51C H 1.0252(3) 0.7465(5) 0.2516(2) 0.111 Uiso 0.10 calc PR 4 H51D H 1.0314(3) 0.6623(5) 0.1952(2) 0.111 Uiso 0.10 calc PR 4 C52 C 1.0340(3) 0.7606(6) 0.1500(2) 0.091(2) Uani 0.90 d P 3 H52A H 1.0888(3) 0.7850(6) 0.1546(2) 0.109 Uiso 0.90 calc PR 3 H52B H 1.0324(3) 0.6891(6) 0.1256(2) 0.109 Uiso 0.90 calc PR 3 C52B C 1.0218(3) 0.8361(6) 0.1714(2) 0.097(21) Uiso 0.10 d PR 4 H52C H 1.0092(3) 0.9057(6) 0.1949(2) 0.117 Uiso 0.10 calc PR 4 H52D H 1.0786(3) 0.8372(6) 0.1670(2) 0.117 Uiso 0.10 calc PR 4 S6 S 0.86120(7) 1.03487(10) 0.15178(5) 0.0644(3) Uani 1 d . . C61 C 0.9599(3) 1.0677(5) 0.1299(3) 0.091(2) Uani 1 d . . H61A H 0.9588(3) 1.0855(5) 0.0868(3) 0.109 Uiso 0.90 calc PR 3 H61B H 0.9785(3) 1.1378(5) 0.1514(3) 0.109 Uiso 0.90 calc PR 3 H61C H 0.9585(3) 1.1412(5) 0.1071(3) 0.109 Uiso 0.10 calc PR 4 H61D H 0.9924(3) 1.0811(5) 0.1664(3) 0.109 Uiso 0.10 calc PR 4 C62 C 1.0158(3) 0.9706(6) 0.1422(3) 0.095(2) Uani 0.90 d P 3 H62A H 1.0242(3) 0.9629(6) 0.1858(3) 0.113 Uiso 0.90 calc PR 3 H62B H 1.0661(3) 0.9912(6) 0.1254(3) 0.113 Uiso 0.90 calc PR 3 C62B C 1.0006(19) 0.9730(28) 0.0916(15) 0.029(7) Uiso 0.10 d P 4 H62C H 0.9785(19) 0.9752(28) 0.0503(15) 0.035 Uiso 0.10 calc PR 4 H62D H 1.0566(19) 0.9905(28) 0.0903(15) 0.035 Uiso 0.10 calc PR 4 N20 N 0.9900(2) 0.8532(3) 0.11699(14) 0.0541(9) Uani 1 d . . N7 N 0.2491(2) 0.3792(3) 0.15522(12) 0.0510(8) Uani 1 d . . C71 C 0.3221(3) 0.4031(5) 0.1198(2) 0.084(2) Uani 1 d . . H71A H 0.3179(3) 0.3591(5) 0.0820(2) 0.101 Uiso 1 calc R . H71B H 0.3233(3) 0.4867(5) 0.1096(2) 0.101 Uiso 1 calc R . C72 C 0.3988(3) 0.3711(6) 0.1523(3) 0.118(2) Uani 1 d . . H72A H 0.4420(3) 0.3889(6) 0.1269(3) 0.176 Uiso 1 calc R . H72B H 0.3990(3) 0.2880(6) 0.1616(3) 0.176 Uiso 1 calc R . H72C H 0.4043(3) 0.4158(6) 0.1893(3) 0.176 Uiso 1 calc R . C73 C 0.2455(3) 0.2502(4) 0.1748(2) 0.0638(12) Uani 1 d . . H73A H 0.2901(3) 0.2343(4) 0.2025(2) 0.077 Uiso 1 calc R . H73B H 0.1977(3) 0.2384(4) 0.1969(2) 0.077 Uiso 1 calc R . C74 C 0.2464(3) 0.1605(5) 0.1234(2) 0.102(2) Uani 1 d . . H74A H 0.2440(3) 0.0819(5) 0.1398(2) 0.153 Uiso 1 calc R . H74B H 0.2942(3) 0.1695(5) 0.1018(2) 0.153 Uiso 1 calc R . H74C H 0.2016(3) 0.1736(5) 0.0962(2) 0.153 Uiso 1 calc R . C75 C 0.2498(3) 0.4504(4) 0.2135(2) 0.0604(12) Uani 1 d . . H75A H 0.2026(3) 0.4312(4) 0.2351(2) 0.072 Uiso 1 calc R . H75B H 0.2950(3) 0.4259(4) 0.2388(2) 0.072 Uiso 1 calc R . C76 C 0.2534(3) 0.5827(4) 0.2056(2) 0.089(2) Uani 1 d . . H76A H 0.2536(3) 0.6203(4) 0.2446(2) 0.133 Uiso 1 calc R . H76B H 0.2081(3) 0.6087(4) 0.1817(2) 0.133 Uiso 1 calc R . H76C H 0.3007(3) 0.6034(4) 0.1854(2) 0.133 Uiso 1 calc R . C77 C 0.1786(3) 0.4121(5) 0.1147(2) 0.084(2) Uani 1 d . . H77A H 0.1839(3) 0.4944(5) 0.1029(2) 0.101 Uiso 1 calc R . H77B H 0.1798(3) 0.3647(5) 0.0780(2) 0.101 Uiso 1 calc R . C78 C 0.1001(3) 0.3962(6) 0.1416(3) 0.128(2) Uani 1 d . . H78A H 0.0592(3) 0.4193(6) 0.1126(3) 0.192 Uiso 1 calc R . H78B H 0.0973(3) 0.4445(6) 0.1773(3) 0.192 Uiso 1 calc R . H78C H 0.0932(3) 0.3146(6) 0.1524(3) 0.192 Uiso 1 calc R . N8 N 0.7487(2) 0.4015(3) 0.1222(2) 0.0582(9) Uani 1 d . . C81 C 0.7064(3) 0.4923(4) 0.0825(2) 0.0684(12) Uani 1 d . . H81A H 0.7449(3) 0.5491(4) 0.0689(2) 0.082 Uiso 1 calc R . H81B H 0.6693(3) 0.5349(4) 0.1068(2) 0.082 Uiso 1 calc R . C82 C 0.6617(4) 0.4421(6) 0.0271(3) 0.137(3) Uani 1 d . . H82A H 0.6368(4) 0.5055(6) 0.0046(3) 0.206 Uiso 1 calc R . H82B H 0.6222(4) 0.3875(6) 0.0399(3) 0.206 Uiso 1 calc R . H82C H 0.6980(4) 0.4017(6) 0.0019(3) 0.206 Uiso 1 calc R . C83 C 0.6938(3) 0.3036(4) 0.1391(2) 0.0736(13) Uani 1 d . . H83A H 0.6751(3) 0.2635(4) 0.1024(2) 0.088 Uiso 1 calc R . H83B H 0.7231(3) 0.2464(4) 0.1639(2) 0.088 Uiso 1 calc R . C84 C 0.6237(4) 0.3444(5) 0.1730(3) 0.154(3) Uani 1 d . . H84A H 0.5914(4) 0.2774(5) 0.1822(3) 0.230 Uiso 1 calc R . H84B H 0.5934(4) 0.3994(5) 0.1484(3) 0.230 Uiso 1 calc R . H84C H 0.6415(4) 0.3823(5) 0.2100(3) 0.230 Uiso 1 calc R . C85 C 0.7785(4) 0.4698(5) 0.1766(3) 0.113(2) Uani 1 d . . H85A H 0.7342(4) 0.5070(5) 0.1956(3) 0.136 Uiso 1 calc R . H85B H 0.8136(4) 0.5319(5) 0.1636(3) 0.136 Uiso 1 calc R . C86 C 0.8222(6) 0.3922(7) 0.2225(4) 0.256(7) Uani 1 d . . H86A H 0.8401(6) 0.4395(7) 0.2565(4) 0.384 Uiso 1 calc R . H86B H 0.8668(6) 0.3564(7) 0.2042(4) 0.384 Uiso 1 calc R . H86C H 0.7874(6) 0.3315(7) 0.2362(4) 0.384 Uiso 1 calc R . C87 C 0.8128(3) 0.3400(4) 0.0885(3) 0.121(2) Uani 1 d . . H87A H 0.7892(3) 0.3007(4) 0.0531(3) 0.146 Uiso 1 calc R . H87B H 0.8370(3) 0.2799(4) 0.1145(3) 0.146 Uiso 1 calc R . C88 C 0.8771(4) 0.4254(6) 0.0680(5) 0.219(5) Uani 1 d . . H88A H 0.9162(4) 0.3820(6) 0.0468(5) 0.328 Uiso 1 calc R . H88B H 0.9015(4) 0.4634(6) 0.1028(5) 0.328 Uiso 1 calc R . H88C H 0.8537(4) 0.4842(6) 0.0415(5) 0.328 Uiso 1 calc R . N91 N 0.2372(3) 0.7911(6) 0.0729(3) 0.133(2) Uani 1 d . . C92 C 0.2462(3) 0.8647(5) 0.0398(2) 0.0753(14) Uani 1 d . . C93 C 0.2607(3) 0.9568(5) -0.0033(2) 0.094(2) Uani 1 d . . H93A H 0.2215(13) 1.0177(16) 0.0000(11) 0.142 Uiso 1 calc R . H93B H 0.2580(21) 0.9244(8) -0.0435(3) 0.142 Uiso 1 calc R . H93C H 0.3123(9) 0.9898(22) 0.0049(10) 0.142 Uiso 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 0.0393(3) 0.0398(3) 0.0417(3) -0.0040(3) 0.0050(2) -0.0019(3) S1 0.0607(7) 0.0776(8) 0.0441(6) -0.0111(6) 0.0081(5) -0.0082(6) C11 0.069(3) 0.098(4) 0.059(3) -0.013(3) -0.011(2) 0.000(3) C12 0.051(3) 0.102(5) 0.070(4) 0.004(4) -0.018(3) 0.007(4) S2 0.0644(7) 0.0534(6) 0.0524(6) 0.0083(5) 0.0056(5) 0.0011(6) C21 0.069(3) 0.122(5) 0.085(4) 0.033(3) 0.013(3) -0.021(3) C22 0.053(4) 0.132(7) 0.109(6) 0.048(5) -0.009(4) -0.042(4) S3 0.0760(8) 0.0393(6) 0.0886(8) -0.0106(6) 0.0034(6) -0.0019(6) C31 0.097(4) 0.068(4) 0.120(4) -0.017(3) -0.019(3) 0.037(3) C32 0.056(4) 0.118(7) 0.114(6) -0.029(5) 0.002(4) 0.021(4) N10 0.045(2) 0.060(2) 0.055(2) -0.001(2) 0.004(2) -0.002(2) O12 0.0326(13) 0.066(2) 0.059(2) -0.0131(14) 0.0034(11) -0.0029(13) Fe2 0.0379(3) 0.0418(3) 0.0396(3) -0.0020(2) 0.0031(2) -0.0031(3) S4 0.0576(6) 0.0716(8) 0.0433(5) -0.0121(5) 0.0030(5) 0.0034(6) C41 0.079(3) 0.103(4) 0.073(3) -0.021(3) 0.034(3) -0.002(3) C42 0.057(3) 0.121(5) 0.062(3) 0.013(3) 0.021(2) -0.014(3) S5 0.0588(7) 0.0629(7) 0.0545(6) 0.0152(5) -0.0002(5) -0.0081(6) C51 0.054(3) 0.128(5) 0.094(4) 0.044(4) -0.009(3) 0.008(3) C52 0.050(3) 0.132(6) 0.091(4) 0.033(4) 0.011(3) 0.032(4) S6 0.0741(8) 0.0429(6) 0.0763(8) -0.0042(6) 0.0064(6) -0.0038(6) C61 0.102(4) 0.061(3) 0.110(4) 0.000(3) 0.014(3) -0.032(3) C62 0.059(4) 0.107(5) 0.118(5) -0.012(4) 0.010(3) -0.034(4) N20 0.046(2) 0.067(2) 0.050(2) 0.003(2) 0.0052(15) -0.004(2) N7 0.063(2) 0.060(2) 0.030(2) 0.000(2) 0.0040(15) 0.002(2) C71 0.111(4) 0.085(4) 0.060(3) 0.007(3) 0.050(3) 0.004(3) C72 0.074(4) 0.119(5) 0.163(6) 0.030(5) 0.048(4) 0.003(4) C73 0.075(3) 0.070(3) 0.047(2) 0.009(2) 0.005(2) 0.000(3) C74 0.155(6) 0.071(4) 0.080(4) -0.014(3) 0.006(4) -0.008(4) C75 0.074(3) 0.070(3) 0.037(2) -0.006(2) 0.005(2) -0.001(2) C76 0.124(5) 0.069(4) 0.074(3) -0.009(3) 0.005(3) 0.000(3) C77 0.106(4) 0.090(4) 0.055(3) 0.002(3) -0.027(3) 0.010(3) C78 0.074(4) 0.142(6) 0.164(6) 0.019(5) -0.042(4) 0.009(4) N8 0.048(2) 0.032(2) 0.095(3) 0.004(2) 0.002(2) 0.002(2) C81 0.082(3) 0.040(3) 0.084(3) 0.006(2) 0.007(3) 0.010(2) C82 0.226(8) 0.097(5) 0.086(4) 0.001(4) -0.043(5) 0.024(5) C83 0.085(3) 0.043(3) 0.094(3) 0.005(2) 0.015(3) -0.010(2) C84 0.167(6) 0.080(4) 0.223(8) -0.020(5) 0.128(6) -0.039(4) C85 0.127(5) 0.060(3) 0.147(5) -0.013(4) -0.076(4) 0.010(3) C86 0.371(14) 0.118(6) 0.259(10) 0.001(7) -0.249(11) 0.036(8) C87 0.077(4) 0.050(3) 0.241(8) -0.004(4) 0.057(4) 0.012(3) C88 0.108(5) 0.092(5) 0.467(16) 0.009(7) 0.160(8) 0.007(4) N91 0.127(5) 0.138(5) 0.135(5) 0.052(4) 0.028(4) 0.003(4) C92 0.061(3) 0.089(4) 0.077(3) -0.001(3) 0.005(3) 0.010(3) C93 0.132(5) 0.068(4) 0.083(4) 0.008(3) -0.007(3) 0.010(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 Fe1 O12 1.801(2) . ? Fe1 S3 2.3311(12) . ? Fe1 S1 2.3471(11) . ? Fe1 S2 2.3511(11) . ? Fe1 N10 2.439(3) . ? S1 C11 1.798(4) . ? C11 C12 1.454(7) . ? C11 C12B 1.50(2) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C11 H11C 0.97 . ? C11 H11D 0.97 . ? C12 N10 1.480(6) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C12B N10 1.47(2) . ? C12B H12C 0.97 . ? C12B H12D 0.97 . ? S2 C21 1.791(5) . ? C21 C22B 1.46(2) . ? C21 C22 1.469(7) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C21 H21C 0.97 . ? C21 H21D 0.97 . ? C22 N10 1.457(7) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C22B N10 1.51(2) . ? C22B H22C 0.97 . ? C22B H22D 0.97 . ? S3 C31 1.797(5) . ? C31 C32B 1.41(2) . ? C31 C32 1.465(8) . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C31 H31C 0.97 . ? C31 H31D 0.97 . ? C32 N10 1.454(7) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? C32B N10 1.52(2) . ? C32B H32C 0.97 . ? C32B H32D 0.97 . ? O12 Fe2 1.791(2) . ? Fe2 S4 2.3398(11) . ? Fe2 S6 2.3475(12) . ? Fe2 S5 2.3488(12) . ? Fe2 N20 2.440(3) . ? S4 C41 1.816(4) . ? C41 C42B 1.35(4) . ? C41 C42 1.490(7) . ? C41 H41A 0.97 . ? C41 H41B 0.97 . ? C41 H41C 0.97 . ? C41 H41D 0.97 . ? C42 N20 1.431(5) . ? C42 H42A 0.97 . ? C42 H42B 0.97 . ? C42B N20 1.69(4) . ? C42B H42C 0.97 . ? C42B H42D 0.97 . ? S5 C51 1.796(5) . ? C51 C52 1.476(6) . ? C51 C52B 1.493(7) . ? C51 H51A 0.97 . ? C51 H51B 0.97 . ? C51 H51C 0.97 . ? C51 H51D 0.97 . ? C52 N20 1.462(6) . ? C52 H52A 0.97 . ? C52 H52B 0.97 . ? C52B N20 1.312(6) . ? C52B H52C 0.97 . ? C52B H52D 0.97 . ? S6 C61 1.796(5) . ? C61 C62 1.468(7) . ? C61 C62B 1.54(3) . ? C61 H61A 0.97 . ? C61 H61B 0.97 . ? C61 H61C 0.97 . ? C61 H61D 0.97 . ? C62 N20 1.497(7) . ? C62 H62A 0.97 . ? C62 H62B 0.97 . ? C62B N20 1.48(3) . ? C62B H62C 0.97 . ? C62B H62D 0.97 . ? N7 C77 1.510(5) . ? N7 C71 1.512(5) . ? N7 C75 1.517(4) . ? N7 C73 1.521(5) . ? C71 C72 1.504(7) . ? C71 H71A 0.97 . ? C71 H71B 0.97 . ? C72 H72A 0.96 . ? C72 H72B 0.96 . ? C72 H72C 0.96 . ? C73 C74 1.521(6) . ? C73 H73A 0.97 . ? C73 H73B 0.97 . ? C74 H74A 0.96 . ? C74 H74B 0.96 . ? C74 H74C 0.96 . ? C75 C76 1.505(6) . ? C75 H75A 0.97 . ? C75 H75B 0.97 . ? C76 H76A 0.96 . ? C76 H76B 0.96 . ? C76 H76C 0.96 . ? C77 C78 1.486(7) . ? C77 H77A 0.97 . ? C77 H77B 0.97 . ? C78 H78A 0.96 . ? C78 H78B 0.96 . ? C78 H78C 0.96 . ? N8 C85 1.496(6) . ? N8 C83 1.501(5) . ? N8 C87 1.508(6) . ? N8 C81 1.512(5) . ? C81 C82 1.521(7) . ? C81 H81A 0.97 . ? C81 H81B 0.97 . ? C82 H82A 0.96 . ? C82 H82B 0.96 . ? C82 H82C 0.96 . ? C83 C84 1.498(7) . ? C83 H83A 0.97 . ? C83 H83B 0.97 . ? C84 H84A 0.96 . ? C84 H84B 0.96 . ? C84 H84C 0.96 . ? C85 C86 1.512(7) . ? C85 H85A 0.97 . ? C85 H85B 0.97 . ? C86 H86A 0.96 . ? C86 H86B 0.96 . ? C86 H86C 0.96 . ? C87 C88 1.535(7) . ? C87 H87A 0.97 . ? C87 H87B 0.97 . ? C88 H88A 0.96 . ? C88 H88B 0.96 . ? C88 H88C 0.96 . ? N91 C92 1.120(6) . ? C92 C93 1.436(7) . ? C93 H93A 0.96 . ? C93 H93B 0.96 . ? C93 H93C 0.96 . ? 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 O12 Fe1 S3 100.46(9) . . ? O12 Fe1 S1 100.53(8) . . ? S3 Fe1 S1 117.12(5) . . ? O12 Fe1 S2 97.38(9) . . ? S3 Fe1 S2 116.65(5) . . ? S1 Fe1 S2 118.29(5) . . ? O12 Fe1 N10 177.40(12) . . ? S3 Fe1 N10 80.79(9) . . ? S1 Fe1 N10 80.81(8) . . ? S2 Fe1 N10 80.02(8) . . ? C11 S1 Fe1 103.38(15) . . ? C12 C11 S1 114.6(4) . . ? C12B C11 S1 116.1(8) . . ? C12 C11 H11A 108.6(3) . . ? S1 C11 H11A 108.62(15) . . ? C12 C11 H11B 108.6(4) . . ? S1 C11 H11B 108.6(2) . . ? H11A C11 H11B 107.6 . . ? C12B C11 H11C 108.3(9) . . ? S1 C11 H11C 108.3(2) . . ? C12B C11 H11D 108.3(8) . . ? S1 C11 H11D 108.3(2) . . ? H11C C11 H11D 107.4 . . ? C11 C12 N10 115.0(4) . . ? C11 C12 H12A 108.5(3) . . ? N10 C12 H12A 108.5(3) . . ? C11 C12 H12B 108.5(4) . . ? N10 C12 H12B 108.5(3) . . ? H12A C12 H12B 107.5 . . ? N10 C12B C11 112.9(13) . . ? N10 C12B H12C 109.0(8) . . ? C11 C12B H12C 109.0(8) . . ? N10 C12B H12D 109.0(9) . . ? C11 C12B H12D 109.0(9) . . ? H12C C12B H12D 107.8 . . ? C21 S2 Fe1 103.9(2) . . ? C22B C21 S2 115.4(8) . . ? C22 C21 S2 114.0(4) . . ? C22 C21 H21A 108.8(4) . . ? S2 C21 H21A 108.8(2) . . ? C22 C21 H21B 108.8(4) . . ? S2 C21 H21B 108.8(2) . . ? H21A C21 H21B 107.7 . . ? C22B C21 H21C 108.4(9) . . ? S2 C21 H21C 108.4(2) . . ? C22B C21 H21D 108.4(8) . . ? S2 C21 H21D 108.4(2) . . ? H21C C21 H21D 107.5 . . ? N10 C22 C21 114.5(5) . . ? N10 C22 H22A 108.6(4) . . ? C21 C22 H22A 108.6(5) . . ? N10 C22 H22B 108.6(3) . . ? C21 C22 H22B 108.6(3) . . ? H22A C22 H22B 107.6 . . ? C21 C22B N10 111.8(12) . . ? C21 C22B H22C 109.3(9) . . ? N10 C22B H22C 109.3(8) . . ? C21 C22B H22D 109.3(8) . . ? N10 C22B H22D 109.3(8) . . ? H22C C22B H22D 107.9 . . ? C31 S3 Fe1 103.5(2) . . ? C32B C31 S3 117.2(8) . . ? C32 C31 S3 114.5(4) . . ? C32 C31 H31A 108.6(4) . . ? S3 C31 H31A 108.6(2) . . ? C32 C31 H31B 108.6(4) . . ? S3 C31 H31B 108.6(2) . . ? H31A C31 H31B 107.6 . . ? C32B C31 H31C 108.0(9) . . ? S3 C31 H31C 108.0(2) . . ? C32B C31 H31D 108.0(8) . . ? S3 C31 H31D 108.0(2) . . ? H31C C31 H31D 107.2 . . ? N10 C32 C31 114.8(5) . . ? N10 C32 H32A 108.6(4) . . ? C31 C32 H32A 108.6(4) . . ? N10 C32 H32B 108.6(3) . . ? C31 C32 H32B 108.6(3) . . ? H32A C32 H32B 107.5 . . ? C31 C32B N10 113.8(13) . . ? C31 C32B H32C 108.8(9) . . ? N10 C32B H32C 108.8(8) . . ? C31 C32B H32D 108.8(8) . . ? N10 C32B H32D 108.8(7) . . ? H32C C32B H32D 107.7 . . ? C32 N10 C22 109.2(5) . . ? C32 N10 C12 110.8(5) . . ? C22 N10 C12 109.6(5) . . ? C12B N10 C22B 114.1(12) . . ? C12B N10 C32B 114.9(12) . . ? C22B N10 C32B 109.7(11) . . ? C32 N10 Fe1 108.9(3) . . ? C22 N10 Fe1 109.6(3) . . ? C12B N10 Fe1 106.4(8) . . ? C12 N10 Fe1 108.7(3) . . ? C22B N10 Fe1 105.4(8) . . ? C32B N10 Fe1 105.5(7) . . ? Fe2 O12 Fe1 162.1(2) . . ? O12 Fe2 S4 97.46(8) . . ? O12 Fe2 S6 98.99(9) . . ? S4 Fe2 S6 120.70(5) . . ? O12 Fe2 S5 101.20(9) . . ? S4 Fe2 S5 116.07(5) . . ? S6 Fe2 S5 115.73(4) . . ? O12 Fe2 N20 178.23(11) . . ? S4 Fe2 N20 81.05(8) . . ? S6 Fe2 N20 81.03(9) . . ? S5 Fe2 N20 80.34(8) . . ? C41 S4 Fe2 102.8(2) . . ? C42B C41 S4 120.6(16) . . ? C42 C41 S4 113.5(3) . . ? C42 C41 H41A 108.9(3) . . ? S4 C41 H41A 108.9(2) . . ? C42 C41 H41B 108.9(3) . . ? S4 C41 H41B 108.9(2) . . ? H41A C41 H41B 107.7 . . ? C42B C41 H41C 107.2(17) . . ? S4 C41 H41C 107.2(2) . . ? C42B C41 H41D 107.2(19) . . ? S4 C41 H41D 107.2(2) . . ? H41C C41 H41D 106.8 . . ? N20 C42 C41 114.5(4) . . ? N20 C42 H42A 108.6(2) . . ? C41 C42 H42A 108.6(3) . . ? N20 C42 H42B 108.6(3) . . ? C41 C42 H42B 108.6(3) . . ? H42A C42 H42B 107.6 . . ? C41 C42B N20 107.0(24) . . ? C41 C42B H42C 110.3(16) . . ? N20 C42B H42C 110.3(13) . . ? C41 C42B H42D 110.3(18) . . ? N20 C42B H42D 110.3(14) . . ? H42C C42B H42D 108.6 . . ? C51 S5 Fe2 104.0(2) . . ? C52 C51 S5 113.4(3) . . ? C52B C51 S5 109.7(3) . . ? C52 C51 H51A 108.9(4) . . ? S5 C51 H51A 108.9(2) . . ? C52 C51 H51B 108.9(3) . . ? S5 C51 H51B 108.9(2) . . ? H51A C51 H51B 107.7 . . ? C52B C51 H51C 109.7(3) . . ? S5 C51 H51C 109.7(2) . . ? C52B C51 H51D 109.7(3) . . ? S5 C51 H51D 109.7(2) . . ? H51C C51 H51D 108.2 . . ? N20 C52 C51 115.3(4) . . ? N20 C52 H52A 108.5(3) . . ? C51 C52 H52A 108.5(3) . . ? N20 C52 H52B 108.5(3) . . ? C51 C52 H52B 108.5(4) . . ? H52A C52 H52B 107.5 . . ? N20 C52B C51 124.3(6) . . ? N20 C52B H52C 106.2(3) . . ? C51 C52B H52C 106.2(3) . . ? N20 C52B H52D 106.2(3) . . ? C51 C52B H52D 106.2(2) . . ? H52C C52B H52D 106.4 . . ? C61 S6 Fe2 103.5(2) . . ? C62 C61 S6 113.3(4) . . ? C62B C61 S6 116.4(12) . . ? C62 C61 H61A 108.9(4) . . ? S6 C61 H61A 108.9(2) . . ? C62 C61 H61B 108.9(3) . . ? S6 C61 H61B 108.9(2) . . ? H61A C61 H61B 107.7 . . ? C62B C61 H61C 108.2(12) . . ? S6 C61 H61C 108.2(2) . . ? C62B C61 H61D 108.2(13) . . ? S6 C61 H61D 108.2(2) . . ? H61C C61 H61D 107.3 . . ? C61 C62 N20 114.5(4) . . ? C61 C62 H62A 108.6(4) . . ? N20 C62 H62A 108.6(3) . . ? C61 C62 H62B 108.6(3) . . ? N20 C62 H62B 108.6(3) . . ? H62A C62 H62B 107.6 . . ? N20 C62B C61 111.3(20) . . ? N20 C62B H62C 109.4(13) . . ? C61 C62B H62C 109.4(13) . . ? N20 C62B H62D 109.4(12) . . ? C61 C62B H62D 109.4(12) . . ? H62C C62B H62D 108.0 . . ? C42 N20 C52 111.7(4) . . ? C52B N20 C62B 115.5(14) . . ? C42 N20 C62 110.4(4) . . ? C52 N20 C62 108.2(4) . . ? C52B N20 C42B 113.8(14) . . ? C62B N20 C42B 112.2(19) . . ? C52B N20 Fe2 102.7(3) . . ? C42 N20 Fe2 108.8(3) . . ? C52 N20 Fe2 109.6(3) . . ? C62B N20 Fe2 106.5(12) . . ? C62 N20 Fe2 108.1(3) . . ? C42B N20 Fe2 104.7(13) . . ? C77 N7 C71 107.0(3) . . ? C77 N7 C75 110.6(3) . . ? C71 N7 C75 111.3(3) . . ? C77 N7 C73 111.4(3) . . ? C71 N7 C73 111.2(3) . . ? C75 N7 C73 105.4(3) . . ? C72 C71 N7 114.7(4) . . ? C72 C71 H71A 108.6(3) . . ? N7 C71 H71A 108.6(2) . . ? C72 C71 H71B 108.6(3) . . ? N7 C71 H71B 108.6(2) . . ? H71A C71 H71B 107.6 . . ? C71 C72 H72A 109.5(3) . . ? C71 C72 H72B 109.5(3) . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5(3) . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 N7 115.1(3) . . ? C74 C73 H73A 108.5(3) . . ? N7 C73 H73A 108.5(2) . . ? C74 C73 H73B 108.5(3) . . ? N7 C73 H73B 108.5(2) . . ? H73A C73 H73B 107.5 . . ? C73 C74 H74A 109.5(3) . . ? C73 C74 H74B 109.5(3) . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5(3) . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 N7 115.2(3) . . ? C76 C75 H75A 108.5(3) . . ? N7 C75 H75A 108.5(2) . . ? C76 C75 H75B 108.5(3) . . ? N7 C75 H75B 108.5(2) . . ? H75A C75 H75B 107.5 . . ? C75 C76 H76A 109.5(2) . . ? C75 C76 H76B 109.5(3) . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5(3) . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 N7 115.5(4) . . ? C78 C77 H77A 108.4(3) . . ? N7 C77 H77A 108.4(2) . . ? C78 C77 H77B 108.4(3) . . ? N7 C77 H77B 108.4(2) . . ? H77A C77 H77B 107.5 . . ? C77 C78 H78A 109.5(3) . . ? C77 C78 H78B 109.5(3) . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5(3) . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C85 N8 C83 111.9(4) . . ? C85 N8 C87 114.0(4) . . ? C83 N8 C87 104.3(3) . . ? C85 N8 C81 104.7(3) . . ? C83 N8 C81 111.0(3) . . ? C87 N8 C81 111.1(4) . . ? N8 C81 C82 115.0(4) . . ? N8 C81 H81A 108.5(2) . . ? C82 C81 H81A 108.5(3) . . ? N8 C81 H81B 108.5(2) . . ? C82 C81 H81B 108.5(3) . . ? H81A C81 H81B 107.5 . . ? C81 C82 H82A 109.5(3) . . ? C81 C82 H82B 109.5(3) . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5(3) . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 N8 114.0(4) . . ? C84 C83 H83A 108.7(4) . . ? N8 C83 H83A 108.7(2) . . ? C84 C83 H83B 108.7(4) . . ? N8 C83 H83B 108.7(2) . . ? H83A C83 H83B 107.6 . . ? C83 C84 H84A 109.5(3) . . ? C83 C84 H84B 109.5(4) . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5(4) . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N8 C85 C86 112.4(5) . . ? N8 C85 H85A 109.1(3) . . ? C86 C85 H85A 109.1(5) . . ? N8 C85 H85B 109.1(3) . . ? C86 C85 H85B 109.1(5) . . ? H85A C85 H85B 107.9 . . ? C85 C86 H86A 109.5(4) . . ? C85 C86 H86B 109.5(5) . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5(5) . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N8 C87 C88 112.8(4) . . ? N8 C87 H87A 109.0(3) . . ? C88 C87 H87A 109.0(5) . . ? N8 C87 H87B 109.0(3) . . ? C88 C87 H87B 109.0(4) . . ? H87A C87 H87B 107.8 . . ? C87 C88 H88A 109.5(3) . . ? C87 C88 H88B 109.5(5) . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5(4) . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? N91 C92 C93 177.7(6) . . ? C92 C93 H93A 109.5(3) . . ? C92 C93 H93B 109.5(3) . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5(3) . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? _refine_diff_density_max 0.318 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.058 #===END data_roger23 _database_code_CSD 169283 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 2' _chemical_formula_moiety 'C8 H20 N, C12 H24 N3 S6 V2, C2 H3 N' _chemical_formula_structural '(NEt4)[(V{N(CH2CH2S)3})2(mu-N)].MeCN' _chemical_formula_analytical ? _chemical_formula_sum 'C22 H47 N5 S6 V2' _chemical_formula_weight 675.89 _chemical_melting_point ? _chemical_compound_source ? 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' 'V' 'V' 0.3005 0.5294 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a a ' # (equiv. to no. 56) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 15.587(8) _cell_length_b 17.7284(15) _cell_length_c 24.016(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6636.4(36) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 10 _exptl_crystal_description 'large needles' _exptl_crystal_colour black _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method ? _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.961 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.57 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 21.3 _diffrn_reflns_number 4531 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.1036 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 22.0 _reflns_number_total 4061 _reflns_number_observed 1740 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1094P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4060 _refine_ls_number_parameters 338 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1463 _refine_ls_R_factor_obs 0.0663 _refine_ls_wR_factor_all 0.2239 _refine_ls_wR_factor_obs 0.1642 _refine_ls_goodness_of_fit_all 0.966 _refine_ls_goodness_of_fit_obs 1.131 _refine_ls_restrained_S_all 0.967 _refine_ls_restrained_S_obs 1.132 _refine_ls_shift/esd_max 0.055 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V1 V 0.20353(10) 0.48137(9) 0.32755(6) 0.0536(5) Uani 1 d . . N10 N 0.1313(6) 0.4228(5) 0.2588(3) 0.076(3) Uani 1 d . . S11 S 0.0980(2) 0.5690(2) 0.31981(13) 0.0826(9) Uani 1 d . . C12 C 0.0304(8) 0.5306(8) 0.2648(6) 0.121(5) Uani 1 d . . H12A H -0.0171(8) 0.5033(8) 0.2813(6) 0.145 Uiso 1 calc R . H12B H 0.0070(8) 0.5717(8) 0.2429(6) 0.145 Uiso 1 calc R . C13 C 0.0805(11) 0.4782(10) 0.2272(6) 0.150(6) Uani 1 d . . H13A H 0.0409(11) 0.4517(10) 0.2030(6) 0.181 Uiso 1 calc R . H13B H 0.1186(11) 0.5078(10) 0.2040(6) 0.181 Uiso 1 calc R . S14 S 0.1771(3) 0.3745(2) 0.37645(12) 0.0983(12) Uani 1 d . . C15 C 0.1180(11) 0.3173(7) 0.3264(6) 0.133(6) Uani 1 d . . H15A H 0.1570(11) 0.2814(7) 0.3094(6) 0.160 Uiso 1 calc R . H15B H 0.0740(11) 0.2890(7) 0.3459(6) 0.160 Uiso 1 calc R . C16 C 0.0777(11) 0.3629(9) 0.2827(6) 0.140(6) Uani 1 d . . H16A H 0.0263(11) 0.3859(9) 0.2979(6) 0.168 Uiso 1 calc R . H16B H 0.0600(11) 0.3295(9) 0.2528(6) 0.168 Uiso 1 calc R . S17 S 0.3120(2) 0.4828(2) 0.26493(12) 0.0935(11) Uani 1 d . . C18 C 0.2665(9) 0.4329(9) 0.2049(5) 0.123(5) Uani 1 d . . H18A H 0.2481(9) 0.4695(9) 0.1773(5) 0.148 Uiso 1 calc R . H18B H 0.3106(9) 0.4016(9) 0.1881(5) 0.148 Uiso 1 calc R . C19 C 0.1925(10) 0.3849(9) 0.2209(5) 0.129(5) Uani 1 d . . H19A H 0.1623(10) 0.3695(9) 0.1875(5) 0.155 Uiso 1 calc R . H19B H 0.2139(10) 0.3397(9) 0.2389(5) 0.155 Uiso 1 calc R . N12 N 0.2609(5) 0.5296(4) 0.3808(3) 0.063(2) Uani 1 d . . V2 V 0.31588(11) 0.57955(11) 0.43438(6) 0.0697(6) Uani 1 d . . N20 N 0.3814(7) 0.6440(7) 0.5035(5) 0.103(4) Uani 1 d D . S21 S 0.3161(2) 0.4841(2) 0.49768(13) 0.1055(12) Uani 1 d . . C22 C 0.3676(13) 0.5272(10) 0.5570(6) 0.142(7) Uani 1 d . . H22A H 0.3396(13) 0.5094(10) 0.5906(6) 0.171 Uiso 0.80 calc PR 1 H22B H 0.4268(13) 0.5103(10) 0.5583(6) 0.171 Uiso 0.80 calc PR 1 C23A C 0.3668(17) 0.6066(19) 0.5573(6) 0.195(16) Uani 0.80 d P 1 H23A H 0.4104(17) 0.6239(19) 0.5831(6) 0.233 Uiso 0.80 calc PR 1 H23B H 0.3117(17) 0.6231(19) 0.5716(6) 0.233 Uiso 0.80 calc PR 1 C23B C 0.4273(30) 0.5828(21) 0.5337(21) 0.057(13) Uiso 0.20 d PD 2 S24 S 0.2155(2) 0.6726(2) 0.44016(13) 0.0980(11) Uani 1 d . . C25 C 0.2580(11) 0.7333(9) 0.4947(6) 0.133(6) Uani 1 d . . H25A H 0.2440(11) 0.7854(9) 0.4863(6) 0.160 Uiso 0.80 calc PR 1 H25B H 0.2314(11) 0.7204(9) 0.5299(6) 0.160 Uiso 0.80 calc PR 1 C26A C 0.3523(17) 0.7249(16) 0.4994(10) 0.183(11) Uani 0.80 d P 1 H26A H 0.3718(17) 0.7521(16) 0.5320(10) 0.219 Uiso 0.80 calc PR 1 H26B H 0.3790(17) 0.7479(16) 0.4671(10) 0.219 Uiso 0.80 calc PR 1 C26B C 0.3077(32) 0.6715(28) 0.5405(22) 0.054(13) Uiso 0.20 d P 2 S27 S 0.4391(2) 0.6015(2) 0.38600(13) 0.1039(12) Uani 1 d . . C28 C 0.5032(9) 0.6548(9) 0.4339(6) 0.134(6) Uani 1 d . . H28A H 0.5618(9) 0.6365(9) 0.4320(6) 0.160 Uiso 0.80 calc PR 1 H28B H 0.5035(9) 0.7071(9) 0.4220(6) 0.160 Uiso 0.80 calc PR 1 C29A C 0.4752(15) 0.6517(14) 0.4907(9) 0.133(8) Uani 0.80 d P 1 H29A H 0.4954(15) 0.6972(14) 0.5090(9) 0.159 Uiso 0.80 calc PR 1 H29B H 0.5045(15) 0.6096(14) 0.5082(9) 0.159 Uiso 0.80 calc PR 1 C29B C 0.4463(51) 0.6937(38) 0.4767(30) 0.080(23) Uiso 0.20 d P 2 N3 N 0.2861(8) 0.7500 0.2500 0.081(4) Uani 1 d S . C31A C 0.3322(22) 0.8212(13) 0.2531(11) 0.218(17) Uani 0.79(3) d P . C31B C 0.2382(15) 0.7312(13) 0.3009(10) 0.177(14) Uani 0.79(3) d P . C31C C 0.3355(33) 0.7209(28) 0.3000(21) 0.070(22) Uiso 0.21(3) d P . C31D C 0.2298(47) 0.6867(38) 0.2361(29) 0.104(28) Uiso 0.21(3) d P . C32A C 0.3671(27) 0.8292(23) 0.3114(18) 0.177(14) Uiso 0.50 d P . C32B C 0.1443(25) 0.7579(26) 0.2915(16) 0.163(14) Uiso 0.50 d P . C32C C 0.4275(20) 0.7752(18) 0.3052(13) 0.137(11) Uiso 0.50 d P . C32D C 0.2254(34) 0.6724(27) 0.1688(18) 0.196(19) Uiso 0.50 d P . C32E C 0.1682(28) 0.6957(23) 0.1825(17) 0.149(13) Uiso 0.50 d P . N4 N 0.5000 0.5000 0.0000 0.092(4) Uani 1 d S . C41A C 0.5924(17) 0.4720(14) -0.0083(10) 0.098(8) Uiso 0.50 d P . C41B C 0.4369(17) 0.4386(15) -0.0086(11) 0.101(8) Uiso 0.50 d P . C41C C 0.5089(19) 0.5354(16) 0.0572(12) 0.114(9) Uiso 0.50 d P . C41D C 0.4703(17) 0.5591(15) -0.0464(11) 0.103(8) Uiso 0.50 d P . C42A C 0.4531(12) 0.3790(10) 0.0467(9) 0.201(9) Uani 1 d . . C42B C 0.5941(11) 0.4379(12) -0.0713(7) 0.178(8) Uani 1 d . . C5 C 0.5940(13) 0.6448(15) 0.6261(9) 0.181(9) Uani 1 d . . C51 C 0.6066(19) 0.7106(21) 0.6529(13) 0.235(12) Uani 1 d . . N52A N 0.6245(27) 0.7482(28) 0.7040(17) 0.230(17) Uiso 0.50 d P . N52B N 0.6393(40) 0.7771(35) 0.6551(29) 0.301(31) Uiso 0.50 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0587(10) 0.0561(10) 0.0461(9) 0.0008(8) 0.0023(8) -0.0052(9) N10 0.079(6) 0.092(7) 0.058(6) -0.013(5) -0.005(5) -0.030(6) S11 0.068(2) 0.083(2) 0.097(2) 0.001(2) -0.017(2) 0.005(2) C12 0.087(10) 0.138(13) 0.137(13) -0.010(11) -0.037(9) 0.001(9) C13 0.160(15) 0.185(17) 0.106(11) -0.025(12) -0.081(12) -0.010(14) S14 0.157(3) 0.064(2) 0.074(2) 0.013(2) 0.022(2) -0.004(2) C15 0.222(18) 0.066(9) 0.111(11) 0.008(8) 0.019(12) -0.051(10) C16 0.178(16) 0.137(13) 0.105(11) -0.030(10) 0.005(11) -0.104(13) S17 0.080(2) 0.128(3) 0.072(2) -0.014(2) 0.019(2) -0.017(2) C18 0.120(11) 0.181(15) 0.069(8) -0.027(9) 0.031(8) -0.019(11) C19 0.147(14) 0.156(13) 0.084(9) -0.042(9) 0.032(10) -0.052(12) N12 0.060(5) 0.079(6) 0.048(5) -0.004(4) 0.000(4) 0.009(5) V2 0.0671(12) 0.0933(14) 0.0486(10) -0.0138(10) -0.0029(9) -0.0044(10) N20 0.092(9) 0.117(10) 0.101(9) -0.048(8) -0.021(7) -0.005(7) S21 0.119(3) 0.131(3) 0.067(2) 0.012(2) -0.016(2) -0.001(2) C22 0.214(20) 0.155(15) 0.059(9) -0.034(10) -0.032(10) -0.003(15) C23A 0.200(27) 0.367(43) 0.017(9) -0.039(17) 0.009(12) -0.174(32) S24 0.106(2) 0.101(2) 0.087(2) -0.023(2) 0.011(2) 0.014(2) C25 0.159(14) 0.124(13) 0.116(11) -0.067(10) 0.030(11) -0.015(11) C26A 0.163(24) 0.211(30) 0.174(23) -0.079(22) -0.031(20) -0.063(24) S27 0.080(2) 0.153(3) 0.079(2) -0.031(2) 0.013(2) -0.022(2) C28 0.102(11) 0.179(15) 0.121(12) -0.057(11) -0.009(10) -0.054(11) C29A 0.137(21) 0.153(22) 0.109(17) -0.024(15) -0.049(15) -0.044(17) N3 0.079(9) 0.053(8) 0.110(11) 0.022(8) 0.000 0.000 C31A 0.360(43) 0.142(19) 0.154(22) 0.040(17) -0.036(25) -0.156(23) C31B 0.159(23) 0.165(22) 0.208(25) 0.123(20) 0.088(19) 0.057(17) N4 0.107(11) 0.088(10) 0.080(9) -0.029(8) -0.032(8) 0.001(9) C42A 0.210(19) 0.126(13) 0.266(21) 0.070(14) -0.123(17) -0.065(14) C42B 0.149(15) 0.248(21) 0.138(13) -0.097(14) -0.011(12) 0.033(14) C5 0.135(15) 0.231(25) 0.177(19) -0.036(17) -0.050(14) 0.008(17) C51 0.201(27) 0.261(39) 0.243(33) -0.036(28) -0.034(23) 0.045(29) _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 N12 1.779(7) . ? V1 N10 2.253(8) . ? V1 S17 2.263(3) . ? V1 S14 2.267(3) . ? V1 S11 2.270(3) . ? N10 C16 1.467(14) . ? N10 C13 1.47(2) . ? N10 C19 1.479(14) . ? S11 C12 1.821(13) . ? C12 C13 1.51(2) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? S14 C15 1.822(14) . ? C15 C16 1.47(2) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 H16A 0.97 . ? C16 H16B 0.97 . ? S17 C18 1.834(12) . ? C18 C19 1.48(2) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 H19A 0.97 . ? C19 H19B 0.97 . ? N12 V2 1.782(7) . ? V2 N20 2.260(10) . ? V2 S21 2.274(4) . ? V2 S24 2.277(4) . ? V2 S27 2.279(4) . ? N20 C23A 1.47(2) . ? N20 C29B 1.49(7) . ? N20 C23B 1.49(2) . ? N20 C29A 1.50(2) . ? N20 C26A 1.51(3) . ? N20 C26B 1.53(5) . ? S21 C22 1.805(15) . ? C22 C23A 1.41(3) . ? C22 C23B 1.47(5) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23A H23A 0.97 . ? C23A H23B 0.97 . ? S24 C25 1.820(13) . ? C25 C26A 1.48(3) . ? C25 C26B 1.74(5) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26A H26A 0.97 . ? C26A H26B 0.97 . ? S27 C28 1.792(12) . ? C28 C29A 1.43(2) . ? C28 C29B 1.52(8) . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? C29A H29A 0.97 . ? C29A H29B 0.97 . ? N3 C31A 1.45(2) . ? N3 C31A 1.45(2) 2_565 ? N3 C31D 1.46(7) 2_565 ? N3 C31D 1.46(7) . ? N3 C31B 1.47(2) 2_565 ? N3 C31B 1.47(2) . ? N3 C31C 1.52(5) . ? N3 C31C 1.52(5) 2_565 ? C31A C31C 1.48(5) 2_565 ? C31A C32A 1.51(4) . ? C31A C31D 1.62(7) 2_565 ? C31B C31C 1.53(5) . ? C31B C32B 1.55(4) . ? C31B C31D 1.71(7) 2_565 ? C31B C32E 1.74(4) 2_565 ? C31B C31D 1.75(7) . ? C31B C32D 1.87(5) 2_565 ? C31C C31A 1.48(5) 2_565 ? C31C C32C 1.73(5) . ? C31C C32A 2.00(6) . ? C31D C31A 1.62(7) 2_565 ? C31D C32E 1.61(8) . ? C31D C32D 1.64(8) . ? C31D C31B 1.71(7) 2_565 ? C31D C32B 1.78(8) 2_565 ? C32A C32C 1.35(4) . ? C32B C32E 1.10(5) 2_565 ? C32B C31D 1.78(8) 2_565 ? C32B C32D 2.01(6) 2_565 ? C32B C32B 2.01(8) 2_565 ? C32D C32E 1.04(5) . ? C32D C31B 1.87(5) 2_565 ? C32D C32B 2.01(6) 2_565 ? C32E C32B 1.10(5) 2_565 ? C32E C31B 1.74(4) 2_565 ? N4 C41B 1.48(3) 5_665 ? N4 C41B 1.48(3) . ? N4 C41C 1.52(3) 5_665 ? N4 C41C 1.52(3) . ? N4 C41A 1.54(3) 5_665 ? N4 C41A 1.54(3) . ? N4 C41D 1.60(3) 5_665 ? N4 C41D 1.60(3) . ? C41A C42B 1.63(3) . ? C41A C41B 1.70(3) 5_665 ? C41A C41D 1.73(3) 5_665 ? C41A C41C 1.97(4) 5_665 ? C41B C41C 1.51(3) 5_665 ? C41B C41A 1.70(3) 5_665 ? C41B C42A 1.72(3) . ? C41B C41D 1.96(4) 5_665 ? C41C C41B 1.51(3) 5_665 ? C41C C42B 1.71(3) 5_665 ? C41C C41D 1.73(4) 5_665 ? C41C C41A 1.97(4) 5_665 ? C41D C42A 1.62(3) 5_665 ? C41D C41A 1.73(3) 5_665 ? C41D C41C 1.73(4) 5_665 ? C41D C41B 1.96(4) 5_665 ? C42A C41D 1.62(3) 5_665 ? C42B C41C 1.71(3) 5_665 ? C5 C51 1.35(3) . ? C51 N52B 1.29(5) . ? C51 N52A 1.42(5) . ? N52A N52B 1.30(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 V1 N10 178.6(3) . . ? N12 V1 S17 95.5(3) . . ? N10 V1 S17 83.7(2) . . ? N12 V1 S14 96.9(3) . . ? N10 V1 S14 84.5(3) . . ? S17 V1 S14 119.29(14) . . ? N12 V1 S11 95.4(3) . . ? N10 V1 S11 83.9(3) . . ? S17 V1 S11 118.65(14) . . ? S14 V1 S11 118.85(14) . . ? C16 N10 C13 112.2(12) . . ? C16 N10 C19 106.2(10) . . ? C13 N10 C19 109.6(11) . . ? C16 N10 V1 109.3(7) . . ? C13 N10 V1 109.8(7) . . ? C19 N10 V1 109.7(7) . . ? C12 S11 V1 102.9(5) . . ? C13 C12 S11 111.3(9) . . ? C13 C12 H12A 109.4(9) . . ? S11 C12 H12A 109.4(5) . . ? C13 C12 H12B 109.4(8) . . ? S11 C12 H12B 109.4(5) . . ? H12A C12 H12B 108.0 . . ? N10 C13 C12 112.4(11) . . ? N10 C13 H13A 109.1(7) . . ? C12 C13 H13A 109.1(7) . . ? N10 C13 H13B 109.1(8) . . ? C12 C13 H13B 109.1(9) . . ? H13A C13 H13B 107.9 . . ? C15 S14 V1 102.4(4) . . ? C16 C15 S14 112.4(9) . . ? C16 C15 H15A 109.1(9) . . ? S14 C15 H15A 109.1(6) . . ? C16 C15 H15B 109.1(9) . . ? S14 C15 H15B 109.1(5) . . ? H15A C15 H15B 107.8 . . ? C15 C16 N10 115.8(13) . . ? C15 C16 H16A 108.3(9) . . ? N10 C16 H16A 108.3(8) . . ? C15 C16 H16B 108.3(7) . . ? N10 C16 H16B 108.3(6) . . ? H16A C16 H16B 107.4 . . ? C18 S17 V1 103.2(4) . . ? C19 C18 S17 111.9(8) . . ? C19 C18 H18A 109.2(9) . . ? S17 C18 H18A 109.2(5) . . ? C19 C18 H18B 109.2(8) . . ? S17 C18 H18B 109.2(5) . . ? H18A C18 H18B 107.9 . . ? N10 C19 C18 113.6(11) . . ? N10 C19 H19A 108.8(6) . . ? C18 C19 H19A 108.8(7) . . ? N10 C19 H19B 108.8(7) . . ? C18 C19 H19B 108.8(9) . . ? H19A C19 H19B 107.7 . . ? V1 N12 V2 178.4(5) . . ? N12 V2 N20 178.1(4) . . ? N12 V2 S21 96.5(3) . . ? N20 V2 S21 83.3(4) . . ? N12 V2 S24 94.2(3) . . ? N20 V2 S24 84.2(3) . . ? S21 V2 S24 119.92(14) . . ? N12 V2 S27 97.0(3) . . ? N20 V2 S27 84.7(3) . . ? S21 V2 S27 117.8(2) . . ? S24 V2 S27 119.1(2) . . ? C29B N20 C23B 108.4(36) . . ? C23A N20 C29A 111.8(17) . . ? C23A N20 C26A 116.2(19) . . ? C29A N20 C26A 101.1(16) . . ? C29B N20 C26B 124.9(34) . . ? C23B N20 C26B 108.1(30) . . ? C23A N20 V2 110.3(10) . . ? C29B N20 V2 106.7(29) . . ? C23B N20 V2 101.9(20) . . ? C29A N20 V2 109.6(9) . . ? C26A N20 V2 107.2(10) . . ? C26B N20 V2 104.4(20) . . ? C22 S21 V2 102.4(6) . . ? C23A C22 S21 115.0(13) . . ? C23B C22 S21 105.3(22) . . ? C23A C22 H22A 108.5(12) . . ? S21 C22 H22A 108.5(6) . . ? C23A C22 H22B 108.5(15) . . ? S21 C22 H22B 108.5(6) . . ? H22A C22 H22B 107.5 . . ? C22 C23A N20 116.5(18) . . ? C22 C23A H23A 108.1(13) . . ? N20 C23A H23A 108.2(8) . . ? C22 C23A H23B 108.2(15) . . ? N20 C23A H23B 108.2(15) . . ? H23A C23A H23B 107.3 . . ? C22 C23B N20 111.8(30) . . ? C25 S24 V2 102.9(6) . . ? C26A C25 S24 110.8(12) . . ? C26B C25 S24 104.2(18) . . ? C26A C25 H25A 109.5(14) . . ? S24 C25 H25A 109.5(6) . . ? C26A C25 H25B 109.5(13) . . ? S24 C25 H25B 109.5(5) . . ? H25A C25 H25B 108.1 . . ? C25 C26A N20 113.5(18) . . ? C25 C26A H26A 108.9(11) . . ? N20 C26A H26A 108.9(9) . . ? C25 C26A H26B 108.9(14) . . ? N20 C26A H26B 108.9(12) . . ? H26A C26A H26B 107.7 . . ? N20 C26B C25 99.7(30) . . ? C28 S27 V2 103.5(5) . . ? C29A C28 S27 114.9(12) . . ? C29B C28 S27 110.3(30) . . ? C29A C28 H28A 108.5(13) . . ? S27 C28 H28A 108.5(5) . . ? C29A C28 H28B 108.6(14) . . ? S27 C28 H28B 108.5(6) . . ? H28A C28 H28B 107.5 . . ? C28 C29A N20 119.7(15) . . ? C28 C29A H29A 107.4(11) . . ? N20 C29A H29A 107.4(10) . . ? C28 C29A H29B 107.4(14) . . ? N20 C29A H29B 107.4(12) . . ? H29A C29A H29B 106.9 . . ? N20 C29B C28 114.9(45) . . ? C31A N3 C31A 120.8(31) . 2_565 ? C31A N3 C31D 67.6(27) . 2_565 ? C31A N3 C31D 166.8(34) 2_565 2_565 ? C31A N3 C31D 166.8(34) . . ? C31A N3 C31D 67.6(27) 2_565 . ? C31D N3 C31D 106.3(59) 2_565 . ? C31A N3 C31B 95.5(14) . 2_565 ? C31A N3 C31B 113.9(17) 2_565 2_565 ? C31D N3 C31B 73.2(28) 2_565 2_565 ? C31D N3 C31B 71.3(29) . 2_565 ? C31A N3 C31B 113.9(17) . . ? C31A N3 C31B 95.5(14) 2_565 . ? C31D N3 C31B 71.3(29) 2_565 . ? C31D N3 C31B 73.2(28) . . ? C31B N3 C31B 119.0(21) 2_565 . ? C31A N3 C31C 90.2(22) . . ? C31A N3 C31C 59.6(20) 2_565 . ? C31D N3 C31C 112.6(35) 2_565 . ? C31D N3 C31C 103.0(35) . . ? C31B N3 C31C 173.1(23) 2_565 . ? C31B N3 C31C 61.5(20) . . ? C31A N3 C31C 59.6(20) . 2_565 ? C31A N3 C31C 90.2(22) 2_565 2_565 ? C31D N3 C31C 103.0(34) 2_565 2_565 ? C31D N3 C31C 112.6(35) . 2_565 ? C31B N3 C31C 61.5(20) 2_565 2_565 ? C31B N3 C31C 173.1(23) . 2_565 ? C31C N3 C31C 118.9(40) . 2_565 ? N3 C31A C31C 62.3(22) . 2_565 ? N3 C31A C32A 107.9(21) . . ? C31C C31A C32A 146.5(37) 2_565 . ? N3 C31A C31D 56.4(24) . 2_565 ? C31C C31A C31D 97.4(36) 2_565 2_565 ? C32A C31A C31D 102.4(36) . 2_565 ? N3 C31B C31C 60.7(20) . . ? N3 C31B C32B 106.7(20) . . ? C31C C31B C32B 165.6(27) . . ? N3 C31B C31D 54.1(25) . 2_565 ? C31C C31B C31D 99.7(33) . 2_565 ? C32B C31B C31D 66.0(29) . 2_565 ? N3 C31B C32E 109.9(16) . 2_565 ? C31C C31B C32E 135.5(33) . 2_565 ? C32B C31B C32E 38.4(17) . 2_565 ? C31D C31B C32E 55.8(26) 2_565 2_565 ? N3 C31B C31D 53.2(23) . . ? C31C C31B C31D 90.4(33) . . ? C32B C31B C31D 86.4(34) . . ? C31D C31B C31D 85.2(37) 2_565 . ? C32E C31B C31D 119.6(33) 2_565 . ? N3 C31B C32D 99.8(19) . 2_565 ? C31C C31B C32D 102.7(31) . 2_565 ? C32B C31B C32D 71.2(22) . 2_565 ? C31D C31B C32D 54.3(27) 2_565 2_565 ? C32E C31B C32D 33.1(17) 2_565 2_565 ? C31D C31B C32D 138.7(30) . 2_565 ? C31A C31C N3 58.1(21) 2_565 . ? C31A C31C C31B 92.2(34) 2_565 . ? N3 C31C C31B 57.7(20) . . ? C31A C31C C32C 111.9(36) 2_565 . ? N3 C31C C32C 106.8(30) . . ? C31B C31C C32C 139.0(37) . . ? C31A C31C C32A 127.7(34) 2_565 . ? N3 C31C C32A 84.7(26) . . ? C31B C31C C32A 97.4(31) . . ? C32C C31C C32A 41.6(17) . . ? N3 C31D C31A 56.0(26) . 2_565 ? N3 C31D C32E 117.7(47) . . ? C31A C31D C32E 136.2(52) 2_565 . ? N3 C31D C32D 111.7(47) . . ? C31A C31D C32D 100.7(46) 2_565 . ? C32E C31D C32D 37.2(25) . . ? N3 C31D C31B 54.6(24) . 2_565 ? C31A C31D C31B 94.7(37) 2_565 2_565 ? C32E C31D C31B 63.1(31) . 2_565 ? C32D C31D C31B 67.8(34) . 2_565 ? N3 C31D C31B 53.6(24) . . ? C31A C31D C31B 79.8(35) 2_565 . ? C32E C31D C31B 135.2(51) . . ? C32D C31D C31B 162.0(50) . . ? C31B C31D C31B 94.2(36) 2_565 . ? N3 C31D C32B 96.4(41) . 2_565 ? C31A C31D C32B 147.4(47) 2_565 2_565 ? C32E C31D C32B 37.3(23) . 2_565 ? C32D C31D C32B 71.8(36) . 2_565 ? C31B C31D C32B 52.8(25) 2_565 2_565 ? C31B C31D C32B 97.9(39) . 2_565 ? C32C C32A C31A 94.8(32) . . ? C32C C32A C31C 58.4(25) . . ? C31A C32A C31C 72.2(24) . . ? C32E C32B C31B 80.0(35) 2_565 . ? C32E C32B C31D 63.0(36) 2_565 2_565 ? C31B C32B C31D 61.2(26) . 2_565 ? C32E C32B C32D 19.2(31) 2_565 2_565 ? C31B C32B C32D 61.7(20) . 2_565 ? C31D C32B C32D 50.7(26) 2_565 2_565 ? C32E C32B C32B 131.9(45) 2_565 2_565 ? C31B C32B C32B 95.8(21) . 2_565 ? C31D C32B C32B 73.1(28) 2_565 2_565 ? C32D C32B C32B 123.8(24) 2_565 2_565 ? C32A C32C C31C 79.9(29) . . ? C32E C32D C31D 70.2(43) . . ? C32E C32D C31B 66.7(37) . 2_565 ? C31D C32D C31B 57.9(29) . 2_565 ? C32E C32D C32B 20.4(32) . 2_565 ? C31D C32D C32B 57.5(31) . 2_565 ? C31B C32D C32B 47.1(16) 2_565 2_565 ? C32D C32E C32B 140.3(61) . 2_565 ? C32D C32E C31D 72.6(42) . . ? C32B C32E C31D 79.7(41) 2_565 . ? C32D C32E C31B 80.2(40) . 2_565 ? C32B C32E C31B 61.5(30) 2_565 2_565 ? C31D C32E C31B 61.1(27) . 2_565 ? C41B N4 C41B 179.996(4) 5_665 . ? C41B N4 C41C 119.4(13) 5_665 5_665 ? C41B N4 C41C 60.6(13) . 5_665 ? C41B N4 C41C 60.6(13) 5_665 . ? C41B N4 C41C 119.4(13) . . ? C41C N4 C41C 179.998(5) 5_665 . ? C41B N4 C41A 111.5(13) 5_665 5_665 ? C41B N4 C41A 68.5(13) . 5_665 ? C41C N4 C41A 99.5(15) 5_665 5_665 ? C41C N4 C41A 80.5(15) . 5_665 ? C41B N4 C41A 68.5(13) 5_665 . ? C41B N4 C41A 111.5(13) . . ? C41C N4 C41A 80.5(15) 5_665 . ? C41C N4 C41A 99.5(15) . . ? C41A N4 C41A 179.998(3) 5_665 . ? C41B N4 C41D 101.1(13) 5_665 5_665 ? C41B N4 C41D 78.9(13) . 5_665 ? C41C N4 C41D 112.8(13) 5_665 5_665 ? C41C N4 C41D 67.2(13) . 5_665 ? C41A N4 C41D 113.1(12) 5_665 5_665 ? C41A N4 C41D 66.9(12) . 5_665 ? C41B N4 C41D 78.9(13) 5_665 . ? C41B N4 C41D 101.1(13) . . ? C41C N4 C41D 67.2(13) 5_665 . ? C41C N4 C41D 112.8(13) . . ? C41A N4 C41D 66.9(12) 5_665 . ? C41A N4 C41D 113.1(12) . . ? C41D N4 C41D 179.997(5) 5_665 . ? N4 C41A C42B 104.8(16) . . ? N4 C41A C41B 54.2(13) . 5_665 ? C42B C41A C41B 124.9(20) . 5_665 ? N4 C41A C41D 58.3(13) . 5_665 ? C42B C41A C41D 126.7(19) . 5_665 ? C41B C41A C41D 87.9(17) 5_665 5_665 ? N4 C41A C41C 49.3(12) . 5_665 ? C42B C41A C41C 55.6(12) . 5_665 ? C41B C41A C41C 89.4(18) 5_665 5_665 ? C41D C41A C41C 88.8(17) 5_665 5_665 ? N4 C41B C41C 60.8(15) . 5_665 ? N4 C41B C41A 57.3(13) . 5_665 ? C41C C41B C41A 92.8(20) 5_665 5_665 ? N4 C41B C42A 104.2(16) . . ? C41C C41B C42A 134.6(22) 5_665 . ? C41A C41B C42A 115.4(18) 5_665 . ? N4 C41B C41D 53.1(12) . 5_665 ? C41C C41B C41D 95.8(19) 5_665 5_665 ? C41A C41B C41D 91.0(17) 5_665 5_665 ? C42A C41B C41D 51.8(11) . 5_665 ? C41B C41C N4 58.6(15) 5_665 . ? C41B C41C C42B 126.5(22) 5_665 5_665 ? N4 C41C C42B 102.0(17) . 5_665 ? C41B C41C C41D 94.4(20) 5_665 5_665 ? N4 C41C C41D 58.7(14) . 5_665 ? C42B C41C C41D 118.4(20) 5_665 5_665 ? C41B C41C C41A 90.5(18) 5_665 5_665 ? N4 C41C C41A 50.2(12) . 5_665 ? C42B C41C C41A 52.0(12) 5_665 5_665 ? C41D C41C C41A 89.8(17) 5_665 5_665 ? N4 C41D C42A 103.5(16) . 5_665 ? N4 C41D C41A 54.9(13) . 5_665 ? C42A C41D C41A 129.4(20) 5_665 5_665 ? N4 C41D C41C 54.1(13) . 5_665 ? C42A C41D C41C 121.3(20) 5_665 5_665 ? C41A C41D C41C 84.9(18) 5_665 5_665 ? N4 C41D C41B 47.9(11) . 5_665 ? C42A C41D C41B 56.3(13) 5_665 5_665 ? C41A C41D C41B 84.9(16) 5_665 5_665 ? C41C C41D C41B 89.0(18) 5_665 5_665 ? C41D C42A C41B 71.9(15) 5_665 . ? C41A C42B C41C 72.4(14) . 5_665 ? N52B C51 N52A 57.1(32) . . ? N52B C51 C5 150.8(50) . . ? N52A C51 C5 147.7(38) . . ? N52B N52A C51 56.1(31) . . ? C51 N52B N52A 66.8(38) . . ? _refine_diff_density_max 0.473 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.074 #===END data_roger14x _database_code_CSD 169284 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 4' _chemical_formula_moiety 'C16 H36 N, C13 H24 N3 S6 V2, 2(C2 H3 N)' _chemical_formula_structural '(NBu4)[{N(CH2CH2S)3}VCNV{N(CH2CH2S)3}].2MeCN' _chemical_formula_analytical ? _chemical_formula_sum 'C33 H66 N6 S6 V2' _chemical_formula_weight 841.16 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' #(no. 4) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6163(14) _cell_length_b 17.384(2) _cell_length_c 11.3268(13) _cell_angle_alpha 90.00 _cell_angle_beta 100.518(10) _cell_angle_gamma 90.00 _cell_volume 2248.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'subhedral plate' _exptl_crystal_colour 'Dark orange-brown' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method ? _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.094 _exptl_absorpt_correction_T_max 0.112 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD 4-circle diffractometer' _diffrn_measurement_method bisecting _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 6 _diffrn_reflns_number 2819 _diffrn_reflns_av_R_equivalents 0.01840 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 20 _reflns_number_total 2167 _reflns_number_observed 1677 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.4733P] 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 ; Coordinates were set to ride on the parent carbon atoms, those of the methyl hydrogens in rotating groups and those of the ethyl hydrogens in idealised positions. Thermal parameters of the ethyl hydrogens were set to be 1.2 x Ueq of the parent carbon atoms and those of the methyl hydrogens were set to be 1.5 x Ueq. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(9) _refine_ls_number_reflns 2167 _refine_ls_number_parameters 428 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_obs 0.0371 _refine_ls_wR_factor_all 0.1034 _refine_ls_wR_factor_obs 0.0898 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_goodness_of_fit_obs 1.105 _refine_ls_restrained_S_all 1.090 _refine_ls_restrained_S_obs 1.116 _refine_ls_shift/esd_max 0.425 _refine_ls_shift/esd_mean 0.089 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V1 V 0.1226(3) 0.28013(13) 0.2663(3) 0.0546(8) Uani 1 d . . S11 S 0.2631(5) 0.2839(3) 0.4347(4) 0.0703(14) Uani 1 d . . S14 S -0.0701(4) 0.2901(3) 0.2821(5) 0.0711(15) Uani 1 d . . S17 S 0.1740(4) 0.2982(3) 0.0814(4) 0.070(2) Uani 1 d . . N10 N 0.1257(13) 0.4081(6) 0.2786(12) 0.050(4) Uani 1 d . . C12 C 0.2728(20) 0.3862(12) 0.4518(17) 0.079(6) Uani 1 d . . H12A H 0.2246(20) 0.4014(12) 0.5094(17) 0.094 Uiso 0.50 calc PR 1 H12B H 0.3531(20) 0.3991(12) 0.4864(17) 0.094 Uiso 0.50 calc PR 1 H12C H 0.2944(20) 0.3970(12) 0.5370(17) 0.094 Uiso 0.50 calc PR 2 H12D H 0.3372(20) 0.4035(12) 0.4148(17) 0.094 Uiso 0.50 calc PR 2 C15 C -0.0844(15) 0.3977(10) 0.2905(17) 0.073(6) Uani 1 d . . H15A H -0.1101(15) 0.4185(10) 0.2106(17) 0.087 Uiso 0.50 calc PR 1 H15B H -0.1424(15) 0.4108(10) 0.3389(17) 0.087 Uiso 0.50 calc PR 1 H15C H -0.1622(15) 0.4128(10) 0.2505(17) 0.087 Uiso 0.50 calc PR 2 H15D H -0.0752(15) 0.4131(10) 0.3740(17) 0.087 Uiso 0.50 calc PR 2 C18 C 0.1834(16) 0.4022(11) 0.0763(14) 0.060(5) Uani 1 d . . H18A H 0.2624(16) 0.4186(11) 0.1102(14) 0.072 Uiso 0.50 calc PR 1 H18B H 0.1654(16) 0.4196(11) -0.0064(14) 0.072 Uiso 0.50 calc PR 1 H18C H 0.2445(16) 0.4166(11) 0.0324(14) 0.072 Uiso 0.50 calc PR 2 H18D H 0.1099(16) 0.4225(11) 0.0330(14) 0.072 Uiso 0.50 calc PR 2 C13A C 0.2355(23) 0.4358(16) 0.3357(27) 0.080(8) Uiso 0.50 d P 1 H13A H 0.2301(23) 0.4897(16) 0.3564(27) 0.095 Uiso 0.50 calc PR 1 H13B H 0.2924(23) 0.4306(16) 0.2832(27) 0.095 Uiso 0.50 calc PR 1 C16A C 0.0254(19) 0.4297(13) 0.3422(19) 0.054(6) Uiso 0.50 d P 1 H16A H 0.0451(19) 0.4131(13) 0.4252(19) 0.065 Uiso 0.50 calc PR 1 H16B H 0.0181(19) 0.4853(13) 0.3422(19) 0.065 Uiso 0.50 calc PR 1 C19A C 0.0963(20) 0.4379(12) 0.1481(17) 0.051(5) Uiso 0.50 d P 1 H19A H 0.0169(20) 0.4236(12) 0.1122(17) 0.061 Uiso 0.50 calc PR 1 H19B H 0.1022(20) 0.4936(12) 0.1471(17) 0.061 Uiso 0.50 calc PR 1 C13B C 0.1672(16) 0.4362(12) 0.4026(17) 0.022(5) Uiso 0.50 d P 2 H13C H 0.1066(16) 0.4305(12) 0.4506(17) 0.027 Uiso 0.50 calc PR 2 H13D H 0.1894(16) 0.4900(12) 0.4022(17) 0.027 Uiso 0.50 calc PR 2 C16B C 0.0070(19) 0.4392(13) 0.2318(16) 0.022(5) Uiso 0.50 d P 2 H16C H -0.0116(19) 0.4324(13) 0.1455(16) 0.027 Uiso 0.50 calc PR 2 H16D H 0.0054(19) 0.4939(13) 0.2489(16) 0.027 Uiso 0.50 calc PR 2 C19B C 0.2098(16) 0.4383(12) 0.2009(16) 0.024(5) Uiso 0.50 d P 2 H19C H 0.2896(16) 0.4264(12) 0.2386(16) 0.029 Uiso 0.50 calc PR 2 H19D H 0.2025(16) 0.4938(12) 0.1939(16) 0.029 Uiso 0.50 calc PR 2 C/N1 N 0.1222(13) 0.1601(11) 0.2564(14) 0.054(4) Uani 0.92 d P . C/N2 N 0.1262(16) 0.0937(11) 0.2602(16) 0.072(5) Uani 0.92 d P . V2 V 0.1223(3) -0.02613(13) 0.2654(3) 0.0529(8) Uani 1 d . . S21 S 0.2619(5) -0.0287(4) 0.4369(5) 0.080(2) Uani 1 d . . S24 S -0.0716(5) -0.0350(3) 0.2834(5) 0.076(2) Uani 1 d . . S27 S 0.1710(5) -0.0433(3) 0.0819(4) 0.072(2) Uani 1 d . . N20 N 0.1227(10) -0.1434(8) 0.2741(10) 0.055(4) Uani 1 d . . C22 C 0.2807(17) -0.1316(10) 0.4680(17) 0.073(6) Uani 1 d . . H22A H 0.3531(17) -0.1500(10) 0.4468(17) 0.088 Uiso 1 calc R . H22B H 0.2821(17) -0.1421(10) 0.5524(17) 0.088 Uiso 1 calc R . C23 C 0.1809(31) -0.1678(10) 0.3944(24) 0.191(14) Uani 1 d . . H23A H 0.1202(31) -0.1686(10) 0.4429(24) 0.230 Uiso 1 calc R . H23B H 0.2034(31) -0.2210(10) 0.3860(24) 0.230 Uiso 1 calc R . C25 C -0.0889(19) -0.1343(11) 0.2875(16) 0.077(6) Uani 1 d . . H25A H -0.0925(19) -0.1499(11) 0.3690(16) 0.092 Uiso 1 calc R . H25B H -0.1624(19) -0.1484(11) 0.2368(16) 0.092 Uiso 1 calc R . C26 C 0.0078(23) -0.1761(12) 0.2467(27) 0.163(13) Uani 1 d . . H26A H 0.0115(23) -0.2273(12) 0.2810(27) 0.196 Uiso 1 calc R . H26B H -0.0126(23) -0.1818(12) 0.1602(27) 0.196 Uiso 1 calc R . C28 C 0.1761(22) -0.1478(13) 0.0736(21) 0.091(7) Uani 1 d . . H28A H 0.1033(22) -0.1673(13) 0.0274(21) 0.109 Uiso 1 calc R . H28B H 0.2398(22) -0.1637(13) 0.0344(21) 0.109 Uiso 1 calc R . C29 C 0.1946(29) -0.1797(15) 0.2010(26) 0.179(20) Uani 1.00(6) d . . H29A H 0.1780(29) -0.2344(15) 0.1975(26) 0.215 Uiso 1 calc R . H29B H 0.2761(29) -0.1731(15) 0.2381(26) 0.215 Uiso 1 calc R . N3 N 0.4997(5) 0.6308(13) 0.7897(5) 0.064(2) Uani 1 d . . C31 C 0.4263(18) 0.6990(9) 0.8107(14) 0.064(5) Uani 1 d D . H31A H 0.4152(18) 0.6982(9) 0.8935(14) 0.077 Uiso 1 calc R . H31B H 0.3499(18) 0.6941(9) 0.7599(14) 0.077 Uiso 1 calc R . C312 C 0.4784(17) 0.7753(9) 0.7859(19) 0.080(6) Uani 1 d D . H31C H 0.4752(17) 0.7815(9) 0.7002(19) 0.096 Uiso 1 calc R . H31D H 0.5597(17) 0.7776(9) 0.8255(19) 0.096 Uiso 1 calc R . C313 C 0.4096(15) 0.8384(10) 0.8322(21) 0.091(6) Uani 1 d D . H31E H 0.3272(15) 0.8311(10) 0.7994(21) 0.110 Uiso 1 calc R . H31F H 0.4194(15) 0.8338(10) 0.9188(21) 0.110 Uiso 1 calc R . C314 C 0.4444(19) 0.9178(11) 0.8018(23) 0.126(10) Uani 1 d D . H31G H 0.3961(94) 0.9547(12) 0.8327(124) 0.189 Uiso 1 calc R . H31H H 0.4345(137) 0.9231(31) 0.7162(24) 0.189 Uiso 1 calc R . H31I H 0.5249(43) 0.9265(35) 0.8371(127) 0.189 Uiso 1 calc R . C32 C 0.4294(17) 0.5588(10) 0.8090(18) 0.082(6) Uani 1 d D . H32A H 0.4114(17) 0.5618(10) 0.8892(18) 0.098 Uiso 1 calc R . H32B H 0.3555(17) 0.5613(10) 0.7531(18) 0.098 Uiso 1 calc R . C322 C 0.4820(16) 0.4806(9) 0.7958(19) 0.078(6) Uani 1 d D . H32C H 0.4980(16) 0.4756(9) 0.7151(19) 0.093 Uiso 1 calc R . H32D H 0.5560(16) 0.4768(9) 0.8513(19) 0.093 Uiso 1 calc R . C323 C 0.4041(16) 0.4155(9) 0.8194(19) 0.099(8) Uani 1 d D . H32E H 0.3927(16) 0.4189(9) 0.9019(19) 0.119 Uiso 1 calc R . H32F H 0.3281(16) 0.4219(9) 0.7681(19) 0.119 Uiso 1 calc R . C324 C 0.4493(21) 0.3368(9) 0.7988(23) 0.119(9) Uani 1 d D . H32G H 0.3932(60) 0.2989(10) 0.8126(139) 0.178 Uiso 1 calc R . H32H H 0.5219(68) 0.3283(35) 0.8530(95) 0.178 Uiso 1 calc R . H32I H 0.4618(133) 0.3329(31) 0.7175(44) 0.178 Uiso 1 calc R . C33 C 0.6163(6) 0.6296(14) 0.8763(6) 0.068(2) Uani 1 d D . H33A H 0.6602(6) 0.5851(14) 0.8575(6) 0.082 Uiso 1 calc R . H33B H 0.6601(6) 0.6750(14) 0.8617(6) 0.082 Uiso 1 calc R . C332 C 0.6110(7) 0.6269(17) 1.0078(7) 0.089(3) Uani 1 d D . H33C H 0.5677(7) 0.5816(17) 1.0243(7) 0.107 Uiso 1 calc R . H33D H 0.5695(7) 0.6719(17) 1.0289(7) 0.107 Uiso 1 calc R . C333 C 0.7316(7) 0.6248(21) 1.0837(8) 0.103(3) Uani 1 d D . H33E H 0.7696(7) 0.5775(21) 1.0667(8) 0.123 Uiso 1 calc R . H33F H 0.7767(7) 0.6672(21) 1.0599(8) 0.123 Uiso 1 calc R . C334 C 0.7355(11) 0.6297(19) 1.2151(9) 0.151(6) Uani 1 d D . H33G H 0.8128(32) 0.6172(78) 1.2566(9) 0.226 Uiso 1 calc R . H33H H 0.6803(83) 0.5941(55) 1.2378(19) 0.226 Uiso 1 calc R . H33I H 0.7159(112) 0.6810(26) 1.2358(19) 0.226 Uiso 1 calc R . C34 C 0.5272(8) 0.6287(15) 0.6648(7) 0.086(3) Uani 1 d D . H34A H 0.5821(8) 0.5871(15) 0.6609(7) 0.104 Uiso 1 calc R . H34B H 0.5663(8) 0.6763(15) 0.6512(7) 0.104 Uiso 1 calc R . C342 C 0.4236(10) 0.6182(18) 0.5634(8) 0.132(6) Uani 1 d D . H34C H 0.3742(10) 0.6635(18) 0.5561(8) 0.158 Uiso 1 calc R . H34D H 0.3774(10) 0.5743(18) 0.5795(8) 0.158 Uiso 1 calc R . C343 C 0.4702(16) 0.6055(10) 0.4484(10) 0.170(9) Uani 1 d D . H34E H 0.5550(16) 0.6044(10) 0.4684(10) 0.204 Uiso 1 calc R . H34F H 0.4447(16) 0.5551(10) 0.4175(10) 0.204 Uiso 1 calc R . C344 C 0.4370(20) 0.6607(11) 0.3531(13) 0.223(12) Uani 1 d D . H34G H 0.3545(37) 0.6708(88) 0.3432(124) 0.334 Uiso 1 calc R . H34H H 0.4548(167) 0.6405(50) 0.2797(41) 0.334 Uiso 1 calc R . H34I H 0.4796(131) 0.7077(42) 0.3732(84) 0.334 Uiso 1 calc R . N41 N 0.1041(11) 0.6243(18) 0.3250(13) 0.151(5) Uani 1 d . . C42 C 0.0528(12) 0.6249(17) 0.4043(15) 0.122(5) Uani 1 d . . C43 C -0.0132(13) 0.6310(18) 0.4946(10) 0.152(6) Uani 1 d . . H43A H -0.0813(46) 0.6618(53) 0.4669(32) 0.228 Uiso 1 calc R . H43B H 0.0331(30) 0.6547(53) 0.5640(31) 0.228 Uiso 1 calc R . H43C H -0.0369(76) 0.5806(20) 0.5154(65) 0.228 Uiso 1 calc R . N51 N 0.3044(11) 0.6267(31) 0.0601(11) 0.192(7) Uani 1 d . . C52 C 0.2100(13) 0.6308(23) 0.0288(9) 0.106(4) Uani 1 d . . C53 C 0.0863(12) 0.6248(19) -0.0033(10) 0.138(6) Uani 1 d . . H53A H 0.0564(24) 0.6685(67) -0.0512(174) 0.206 Uiso 1 calc R . H53B H 0.0528(18) 0.6235(137) 0.0680(12) 0.206 Uiso 1 calc R . H53C H 0.0663(13) 0.5786(67) -0.0486(176) 0.206 Uiso 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 V1 0.047(2) 0.051(2) 0.064(2) -0.001(2) 0.0059(15) -0.003(2) S11 0.073(3) 0.069(3) 0.067(3) 0.004(3) 0.008(2) 0.009(3) S14 0.060(3) 0.063(3) 0.092(4) 0.013(3) 0.020(3) -0.003(3) S17 0.069(4) 0.069(3) 0.070(3) -0.007(3) 0.005(3) 0.012(3) N10 0.071(10) 0.003(4) 0.071(9) -0.007(5) 0.000(8) -0.011(5) C12 0.084(14) 0.110(17) 0.041(9) -0.011(9) 0.008(9) -0.016(12) C15 0.037(10) 0.054(10) 0.121(15) 0.009(9) -0.001(9) 0.019(8) C18 0.056(11) 0.090(14) 0.038(10) 0.011(9) 0.016(9) 0.013(9) C/N1 0.042(9) 0.059(14) 0.061(10) 0.012(9) 0.010(7) 0.005(9) C/N2 0.081(14) 0.046(13) 0.087(14) 0.012(10) 0.009(10) 0.000(10) V2 0.054(2) 0.050(2) 0.054(2) -0.006(2) 0.0090(14) -0.009(2) S21 0.080(4) 0.079(4) 0.069(3) -0.007(3) -0.020(3) -0.013(3) S24 0.054(3) 0.067(3) 0.111(4) 0.000(3) 0.022(3) 0.003(3) S27 0.082(4) 0.086(4) 0.049(3) -0.002(3) 0.016(2) -0.015(3) N20 0.025(7) 0.110(11) 0.031(6) -0.008(6) 0.011(5) 0.002(7) C22 0.064(11) 0.074(12) 0.065(10) -0.008(8) -0.034(9) 0.001(9) C23 0.343(38) 0.031(10) 0.155(20) 0.015(11) -0.072(20) -0.012(14) C25 0.089(13) 0.088(14) 0.065(11) 0.004(9) 0.046(10) 0.024(10) C26 0.107(16) 0.066(12) 0.299(34) 0.009(14) -0.009(18) -0.022(10) C28 0.099(18) 0.076(15) 0.102(17) -0.005(12) 0.027(14) 0.013(12) C29 0.263(37) 0.105(17) 0.189(31) 0.001(15) 0.091(24) 0.053(17) N3 0.059(4) 0.067(5) 0.067(4) -0.002(10) 0.017(4) -0.019(11) C31 0.068(12) 0.078(14) 0.049(11) 0.000(9) 0.021(9) 0.023(12) C312 0.071(14) 0.079(15) 0.090(13) -0.012(12) 0.012(10) 0.004(13) C313 0.044(10) 0.096(15) 0.143(18) -0.009(13) 0.042(11) 0.000(11) C314 0.072(15) 0.132(22) 0.149(21) -0.008(17) -0.046(14) 0.021(14) C32 0.042(11) 0.076(15) 0.131(17) -0.004(13) 0.022(11) -0.004(11) C322 0.054(12) 0.077(14) 0.103(14) -0.023(12) 0.018(10) -0.023(12) C323 0.093(15) 0.099(17) 0.093(13) 0.017(12) -0.017(11) -0.046(14) C324 0.135(20) 0.040(11) 0.192(23) 0.018(13) 0.061(16) -0.022(11) C33 0.047(5) 0.062(6) 0.093(6) -0.020(13) 0.007(5) 0.024(11) C332 0.074(6) 0.102(7) 0.085(7) 0.034(15) -0.001(5) -0.012(16) C333 0.092(7) 0.106(8) 0.101(8) -0.016(18) -0.008(6) -0.002(20) C334 0.153(11) 0.177(14) 0.104(9) -0.074(18) -0.022(8) 0.021(24) C34 0.110(7) 0.088(7) 0.071(6) 0.021(14) 0.042(6) 0.047(15) C342 0.164(11) 0.161(16) 0.065(7) 0.009(14) 0.004(8) 0.038(19) C343 0.293(22) 0.125(22) 0.076(9) -0.006(10) -0.006(12) 0.058(14) C344 0.339(31) 0.189(27) 0.174(17) 0.050(17) 0.139(20) 0.060(20) N41 0.170(11) 0.083(8) 0.220(13) -0.019(22) 0.091(10) -0.042(19) C42 0.138(11) 0.051(8) 0.181(15) -0.039(20) 0.038(10) -0.027(18) C43 0.236(15) 0.127(12) 0.117(9) -0.023(20) 0.097(10) 0.049(26) N51 0.119(9) 0.338(21) 0.132(10) 0.031(32) 0.053(8) 0.032(36) C52 0.116(10) 0.130(12) 0.068(7) -0.021(19) 0.006(7) -0.022(26) C53 0.160(12) 0.102(10) 0.125(9) -0.007(18) -0.042(9) 0.059(20) _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 C/N1 2.09(2) . ? V1 N10 2.229(10) . ? V1 S11 2.274(6) . ? V1 S14 2.284(6) . ? V1 S17 2.302(6) . ? S11 C12 1.79(2) . ? S14 C15 1.88(2) . ? S17 C18 1.81(2) . ? N10 C13A 1.41(3) . ? N10 C13B 1.48(2) . ? N10 C16B 1.49(3) . ? N10 C19B 1.52(2) . ? N10 C16A 1.52(2) . ? N10 C19A 1.54(2) . ? C12 C13B 1.52(3) . ? C12 C13A 1.57(3) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C12 H12C 0.97 . ? C12 H12D 0.97 . ? C15 C16A 1.42(3) . ? C15 C16B 1.53(3) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C15 H15C 0.97 . ? C15 H15D 0.97 . ? C18 C19B 1.52(3) . ? C18 C19A 1.54(3) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C18 H18C 0.97 . ? C18 H18D 0.97 . ? C13A H13A 0.97 . ? C13A H13B 0.97 . ? C16A H16A 0.97 . ? C16A H16B 0.97 . ? C19A H19A 0.97 . ? C19A H19B 0.97 . ? C13B H13C 0.97 . ? C13B H13D 0.97 . ? C16B H16C 0.97 . ? C16B H16D 0.97 . ? C19B H19C 0.97 . ? C19B H19D 0.97 . ? C/N1 C/N2 1.157(8) . ? C/N2 V2 2.08(2) . ? V2 N20 2.041(14) . ? V2 S27 2.270(5) . ? V2 S21 2.293(6) . ? V2 S24 2.304(6) . ? S21 C22 1.83(2) . ? S24 C25 1.74(2) . ? S27 C28 1.82(2) . ? N20 C29 1.43(3) . ? N20 C26 1.43(3) . ? N20 C23 1.47(3) . ? C22 C23 1.44(3) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C25 C26 1.48(3) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C28 C29 1.52(3) . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? N3 C31 1.50(3) . ? N3 C34 1.506(9) . ? N3 C33 1.521(9) . ? N3 C32 1.53(3) . ? C31 C312 1.505(9) . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C312 C313 1.507(10) . ? C312 H31C 0.97 . ? C312 H31D 0.97 . ? C313 C314 1.496(10) . ? C313 H31E 0.97 . ? C313 H31F 0.97 . ? C314 H31G 0.96 . ? C314 H31H 0.96 . ? C314 H31I 0.9601(14) . ? C32 C322 1.508(9) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? C322 C323 1.503(10) . ? C322 H32C 0.97 . ? C322 H32D 0.97 . ? C323 C324 1.499(10) . ? C323 H32E 0.97 . ? C323 H32F 0.97 . ? C324 H32G 0.96 . ? C324 H32H 0.96 . ? C324 H32I 0.96 . ? C33 C332 1.503(8) . ? C33 H33A 0.97 . ? C33 H33B 0.97 . ? C332 C333 1.505(8) . ? C332 H33C 0.97 . ? C332 H33D 0.97 . ? C333 C334 1.483(9) . ? C333 H33E 0.97 . ? C333 H33F 0.97 . ? C334 H33G 0.9600(10) . ? C334 H33H 0.96 . ? C334 H33I 0.96 . ? C34 C342 1.515(9) . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C342 C343 1.516(10) . ? C342 H34C 0.97 . ? C342 H34D 0.97 . ? C343 C344 1.443(10) . ? C343 H34E 0.97 . ? C343 H34F 0.97 . ? C344 H34G 0.96 . ? C344 H34H 0.96 . ? C344 H34I 0.96 . ? N41 C42 1.17(2) . ? C42 C43 1.39(2) . ? C43 H43A 0.96 . ? C43 H43B 0.96 . ? C43 H43C 0.96 . ? N51 C52 1.092(14) . ? C52 C53 1.42(2) . ? C53 H53A 0.96 . ? C53 H53B 0.96 . ? C53 H53C 0.96 . ? 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 C/N1 V1 N10 179.1(5) . . ? C/N1 V1 S11 93.9(4) . . ? N10 V1 S11 85.3(4) . . ? C/N1 V1 S14 95.0(4) . . ? N10 V1 S14 85.7(4) . . ? S11 V1 S14 119.7(2) . . ? C/N1 V1 S17 94.9(4) . . ? N10 V1 S17 85.2(4) . . ? S11 V1 S17 119.5(2) . . ? S14 V1 S17 118.8(2) . . ? C12 S11 V1 98.1(7) . . ? C15 S14 V1 100.1(6) . . ? C18 S17 V1 101.1(5) . . ? C13B N10 C16B 109.7(13) . . ? C13B N10 C19B 107.6(13) . . ? C16B N10 C19B 108.7(13) . . ? C13A N10 C16A 114.0(16) . . ? C13A N10 C19A 110.4(17) . . ? C16A N10 C19A 108.4(15) . . ? C13A N10 V1 111.9(14) . . ? C13B N10 V1 112.8(10) . . ? C16B N10 V1 109.7(11) . . ? C19B N10 V1 108.2(10) . . ? C16A N10 V1 105.7(11) . . ? C19A N10 V1 106.1(10) . . ? C13B C12 S11 119.8(14) . . ? C13A C12 S11 117.0(16) . . ? C13A C12 H12A 108.3(14) . . ? S11 C12 H12A 108.1(7) . . ? C13A C12 H12B 107.9(12) . . ? S11 C12 H12B 107.9(7) . . ? H12A C12 H12B 107.3 . . ? C13B C12 H12C 107.4(10) . . ? S11 C12 H12C 107.4(6) . . ? C13B C12 H12D 107.4(10) . . ? S11 C12 H12D 107.3(7) . . ? H12C C12 H12D 107.0 . . ? C16A C15 S14 109.3(13) . . ? C16B C15 S14 111.8(13) . . ? C16A C15 H15A 109.7(11) . . ? S14 C15 H15A 109.8(6) . . ? C16A C15 H15B 109.9(11) . . ? S14 C15 H15B 109.9(6) . . ? H15A C15 H15B 108.3 . . ? C16B C15 H15C 109.3(10) . . ? S14 C15 H15C 109.3(5) . . ? C16B C15 H15D 109.2(10) . . ? S14 C15 H15D 109.3(6) . . ? H15C C15 H15D 107.9 . . ? C19B C18 S17 112.6(13) . . ? C19A C18 S17 109.6(13) . . ? C19A C18 H18A 109.8(10) . . ? S17 C18 H18A 109.9(6) . . ? C19A C18 H18B 109.6(9) . . ? S17 C18 H18B 109.7(5) . . ? H18A C18 H18B 108.2 . . ? C19B C18 H18C 109.2(10) . . ? S17 C18 H18C 109.2(5) . . ? C19B C18 H18D 108.9(10) . . ? S17 C18 H18D 109.0(6) . . ? H18C C18 H18D 107.9 . . ? N10 C13A C12 106.7(19) . . ? N10 C13A H13A 110.2(13) . . ? C12 C13A H13A 110.2(14) . . ? N10 C13A H13B 110.4(14) . . ? C12 C13A H13B 110.7(13) . . ? H13A C13A H13B 108.6 . . ? C15 C16A N10 114.6(16) . . ? C15 C16A H16A 108.5(11) . . ? N10 C16A H16A 108.7(10) . . ? C15 C16A H16B 108.6(11) . . ? N10 C16A H16B 108.6(9) . . ? H16A C16A H16B 107.6 . . ? C18 C19A N10 108.6(15) . . ? C18 C19A H19A 110.0(10) . . ? N10 C19A H19A 109.8(10) . . ? C18 C19A H19B 110.1(10) . . ? N10 C19A H19B 110.0(8) . . ? H19A C19A H19B 108.4 . . ? N10 C13B C12 105.1(14) . . ? N10 C13B H13C 110.7(9) . . ? C12 C13B H13C 110.7(10) . . ? N10 C13B H13D 110.7(9) . . ? C12 C13B H13D 110.8(10) . . ? H13C C13B H13D 108.8 . . ? N10 C16B C15 110.2(15) . . ? N10 C16B H16C 109.4(9) . . ? C15 C16B H16C 109.5(10) . . ? N10 C16B H16D 109.8(9) . . ? C15 C16B H16D 109.7(10) . . ? H16C C16B H16D 108.1 . . ? N10 C19B C18 110.6(15) . . ? N10 C19B H19C 109.6(9) . . ? C18 C19B H19C 109.4(10) . . ? N10 C19B H19D 109.5(9) . . ? C18 C19B H19D 109.7(11) . . ? H19C C19B H19D 108.1 . . ? C/N2 C/N1 V1 174.7(20) . . ? C/N1 C/N2 V2 176.5(21) . . ? N20 V2 C/N2 178.4(6) . . ? N20 V2 S27 85.1(4) . . ? C/N2 V2 S27 95.5(5) . . ? N20 V2 S21 86.8(4) . . ? C/N2 V2 S21 91.6(5) . . ? S27 V2 S21 121.2(2) . . ? N20 V2 S24 85.5(4) . . ? C/N2 V2 S24 95.5(5) . . ? S27 V2 S24 118.9(2) . . ? S21 V2 S24 118.3(3) . . ? C22 S21 V2 102.9(6) . . ? C25 S24 V2 100.9(7) . . ? C28 S27 V2 101.2(7) . . ? C29 N20 C26 108.7(18) . . ? C29 N20 C23 101.0(18) . . ? C26 N20 C23 109.9(17) . . ? C29 N20 V2 114.2(13) . . ? C26 N20 V2 113.1(12) . . ? C23 N20 V2 109.2(10) . . ? C23 C22 S21 105.1(13) . . ? C23 C22 H22A 110.7(16) . . ? S21 C22 H22A 110.8(7) . . ? C23 C22 H22B 110.7(14) . . ? S21 C22 H22B 110.7(6) . . ? H22A C22 H22B 108.8 . . ? C22 C23 N20 126.6(18) . . ? C22 C23 H23A 105.6(16) . . ? N20 C23 H23A 105.6(15) . . ? C22 C23 H23B 105.7(12) . . ? N20 C23 H23B 105.8(10) . . ? H23A C23 H23B 106.1 . . ? C26 C25 S24 112.4(14) . . ? C26 C25 H25A 109.3(13) . . ? S24 C25 H25A 109.1(6) . . ? C26 C25 H25B 109.0(12) . . ? S24 C25 H25B 109.1(7) . . ? H25A C25 H25B 107.9 . . ? N20 C26 C25 117.9(18) . . ? N20 C26 H26A 107.6(11) . . ? C25 C26 H26A 107.7(12) . . ? N20 C26 H26B 108.1(13) . . ? C25 C26 H26B 108.0(13) . . ? H26A C26 H26B 107.1 . . ? C29 C28 S27 108.3(16) . . ? C29 C28 H28A 110.2(16) . . ? S27 C28 H28A 110.2(8) . . ? C29 C28 H28B 109.9(13) . . ? S27 C28 H28B 109.9(7) . . ? H28A C28 H28B 108.4 . . ? N20 C29 C28 113.1(20) . . ? N20 C29 H29A 109.1(13) . . ? C28 C29 H29A 108.8(14) . . ? N20 C29 H29B 108.9(15) . . ? C28 C29 H29B 109.1(16) . . ? H29A C29 H29B 107.7 . . ? C31 N3 C34 113.0(14) . . ? C31 N3 C33 111.9(14) . . ? C34 N3 C33 106.8(6) . . ? C31 N3 C32 106.8(5) . . ? C34 N3 C32 109.0(15) . . ? C33 N3 C32 109.4(15) . . ? N3 C31 C312 114.0(15) . . ? N3 C31 H31A 108.6(7) . . ? C312 C31 H31A 108.9(9) . . ? N3 C31 H31B 108.8(8) . . ? C312 C31 H31B 108.8(11) . . ? H31A C31 H31B 107.7 . . ? C31 C312 C313 108.7(15) . . ? C31 C312 H31C 110.0(10) . . ? C313 C312 H31C 110.1(12) . . ? C31 C312 H31D 110.0(11) . . ? C313 C312 H31D 109.8(11) . . ? H31C C312 H31D 108.3 . . ? C314 C313 C312 114.1(15) . . ? C314 C313 H31E 108.6(10) . . ? C312 C313 H31E 108.6(11) . . ? C314 C313 H31F 108.8(12) . . ? C312 C313 H31F 108.8(12) . . ? H31E C313 H31F 107.6 . . ? C313 C314 H31G 109.5(12) . . ? C313 C314 H31H 109.6(12) . . ? H31G C314 H31H 109.5 . . ? C313 C314 H31I 109.3(10) . . ? H31G C314 H31I 109.46(8) . . ? H31H C314 H31I 109.5(2) . . ? C322 C32 N3 119.0(15) . . ? C322 C32 H32A 107.5(10) . . ? N3 C32 H32A 107.7(8) . . ? C322 C32 H32B 107.5(11) . . ? N3 C32 H32B 107.6(8) . . ? H32A C32 H32B 107.0 . . ? C323 C322 C32 113.2(15) . . ? C323 C322 H32C 108.9(11) . . ? C32 C322 H32C 108.9(10) . . ? C323 C322 H32D 109.1(11) . . ? C32 C322 H32D 108.9(11) . . ? H32C C322 H32D 107.8 . . ? C324 C323 C322 114.8(15) . . ? C324 C323 H32E 108.5(11) . . ? C322 C323 H32E 108.5(11) . . ? C324 C323 H32F 108.7(11) . . ? C322 C323 H32F 108.6(11) . . ? H32E C323 H32F 107.5 . . ? C323 C324 H32G 109.4(10) . . ? C323 C324 H32H 109.6(11) . . ? H32G C324 H32H 109.5 . . ? C323 C324 H32I 109.4(11) . . ? H32G C324 H32I 109.47(7) . . ? H32H C324 H32I 109.47(8) . . ? C332 C33 N3 116.5(6) . . ? C332 C33 H33A 108.0(12) . . ? N3 C33 H33A 107.9(10) . . ? C332 C33 H33B 108.3(12) . . ? N3 C33 H33B 108.4(11) . . ? H33A C33 H33B 107.3 . . ? C33 C332 C333 111.3(7) . . ? C33 C332 H33C 109.6(12) . . ? C333 C332 H33C 109.6(16) . . ? C33 C332 H33D 109.2(12) . . ? C333 C332 H33D 109.1(16) . . ? H33C C332 H33D 108.0 . . ? C334 C333 C332 115.2(8) . . ? C334 C333 H33E 108.1(16) . . ? C332 C333 H33E 108.2(16) . . ? C334 C333 H33F 108.8(15) . . ? C332 C333 H33F 108.7(15) . . ? H33E C333 H33F 107.5 . . ? C333 C334 H33G 109.6(7) . . ? C333 C334 H33H 109.8(14) . . ? H33G C334 H33H 109.5 . . ? C333 C334 H33I 109.1(18) . . ? H33G C334 H33I 109.47(7) . . ? H33H C334 H33I 109.5 . . ? N3 C34 C342 116.1(7) . . ? N3 C34 H34A 108.0(10) . . ? C342 C34 H34A 108.1(12) . . ? N3 C34 H34B 108.6(11) . . ? C342 C34 H34B 108.4(13) . . ? H34A C34 H34B 107.4 . . ? C34 C342 C343 108.1(10) . . ? C34 C342 H34C 109.9(13) . . ? C343 C342 H34C 110.0(10) . . ? C34 C342 H34D 110.2(12) . . ? C343 C342 H34D 110.3(13) . . ? H34C C342 H34D 108.4 . . ? C344 C343 C342 117.2(11) . . ? C344 C343 H34E 108.1(13) . . ? C342 C343 H34E 108.1(8) . . ? C344 C343 H34F 108.0(11) . . ? C342 C343 H34F 107.8(13) . . ? H34E C343 H34F 107.2 . . ? C343 C344 H34G 109.6(12) . . ? C343 C344 H34H 109.4(8) . . ? H34G C344 H34H 109.47(5) . . ? C343 C344 H34I 109.4(12) . . ? H34G C344 H34I 109.47(7) . . ? H34H C344 H34I 109.47(8) . . ? N41 C42 C43 175.3(32) . . ? C42 C43 H43A 109.6(13) . . ? C42 C43 H43B 109.5(10) . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.3(17) . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N51 C52 C53 171.2(51) . . ? C52 C53 H53A 108.7(21) . . ? C52 C53 H53B 109.5(7) . . ? H53A C53 H53B 109.47(6) . . ? C52 C53 H53C 110.2(20) . . ? H53A C53 H53C 109.44(14) . . ? H53B C53 H53C 109.5 . . ? _refine_diff_density_max 0.301 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.043 #===END data_roger49 _database_code_CSD 169285 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 6' _chemical_formula_moiety 'C8 H20 N, C7 H12 Fe N2 S3' _chemical_formula_structural (NEt4)[Fe(CN)(N{CH2CH2S}3)] _chemical_formula_analytical ? _chemical_formula_sum 'C15 H32 Fe N3 S3' _chemical_formula_weight 406.47 _chemical_melting_point ? _chemical_compound_source ? 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' 'Fe' 'Fe' 0.3463 0.8444 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c m' #(no. 57) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9215(9) _cell_length_b 14.1773(14) _cell_length_c 15.7017(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1986.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description needles _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method ? _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.174 _exptl_absorpt_correction_T_max 0.209 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 1.3 _diffrn_reflns_number 2209 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25.0 _reflns_number_total 1821 _reflns_number_observed 1031 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'isostructural with Co analogue' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; Hydrogen coordinates were of idealised positions and set to ride on the parent carbon atoms. All isotropic thermal displacement parameters were set to be 1.2 x Ueq of the parent atoms. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1821 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_obs 0.0460 _refine_ls_wR_factor_all 0.1232 _refine_ls_wR_factor_obs 0.0994 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.128 _refine_ls_restrained_S_all 1.021 _refine_ls_restrained_S_obs 1.128 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.15999(9) 0.06447(6) 0.2500 0.0412(3) Uani 1 d S . S1 S 0.1472(2) 0.21849(11) 0.2500 0.0605(5) Uani 1 d S . S2 S 0.1562(2) -0.01137(10) 0.37107(8) 0.0711(4) Uani 1 d . . N4 N -0.0693(5) 0.0617(3) 0.2500 0.0371(11) Uani 1 d S . C5 C 0.3751(8) 0.0690(5) 0.2500 0.073(2) Uani 1 d S . N5 N 0.4977(7) 0.0735(6) 0.2500 0.117(3) Uani 1 d S . C14 C -0.0542(7) 0.2353(4) 0.2500 0.072(2) Uani 1 d S . H14A H -0.0795(7) 0.2887(4) 0.2859 0.086 Uiso 0.50 calc PR . H14B H -0.0878(7) 0.2491(4) 0.1926 0.086 Uiso 0.50 calc PR . C41 C -0.1301(8) 0.1521(5) 0.2810(6) 0.057(3) Uani 0.50 d P . H41A H -0.2348(8) 0.1560(5) 0.2647(6) 0.068 Uiso 0.50 calc PR . H41B H -0.1259(8) 0.1523(5) 0.3427(6) 0.068 Uiso 0.50 calc PR . C24 C -0.0431(6) -0.0264(4) 0.3855(3) 0.0726(15) Uani 1 d . . H24A H -0.0627(6) -0.0882(4) 0.4094(3) 0.087 Uiso 0.50 calc PR 1 H24B H -0.0799(6) 0.0206(4) 0.4253(3) 0.087 Uiso 0.50 calc PR 1 H24C H -0.0725(6) -0.0882(4) 0.3650(3) 0.087 Uiso 0.50 calc PR 2 H24D H -0.0668(6) -0.0230(4) 0.4457(3) 0.087 Uiso 0.50 calc PR 2 C42 C -0.1231(10) -0.0169(7) 0.3043(6) 0.059(2) Uani 0.50 d P 1 H42A H -0.2287(10) -0.0074(7) 0.3161(6) 0.070 Uiso 0.50 calc PR 1 H42B H -0.1132(10) -0.0754(7) 0.2729(6) 0.070 Uiso 0.50 calc PR 1 C43 C -0.1271(11) 0.0452(7) 0.1598(6) 0.055(2) Uani 0.50 d P 2 H43A H -0.2315(11) 0.0264(7) 0.1625(6) 0.065 Uiso 0.50 calc PR 2 H43B H -0.1217(11) 0.1040(7) 0.1282(6) 0.065 Uiso 0.50 calc PR 2 N6 N 0.4802(6) 0.2500 0.5000 0.0510(13) Uani 1 d S . C61 C 0.4799(18) 0.2690(12) 0.6009(10) 0.062(4) Uiso 0.30 d P 3 H61A H 0.5603(18) 0.3131(12) 0.6130(10) 0.075 Uiso 0.30 calc PR 3 H61B H 0.3867(18) 0.3007(12) 0.6147(10) 0.075 Uiso 0.30 calc PR 3 C62 C 0.4954(17) 0.1929(11) 0.6572(11) 0.076(5) Uiso 0.35 d P 3 H62A H 0.4930(17) 0.2157(11) 0.7148(11) 0.091 Uiso 0.35 calc PR 3 H62B H 0.5891(17) 0.1617(11) 0.6469(11) 0.091 Uiso 0.35 calc PR 3 H62C H 0.4146(17) 0.1493(11) 0.6486(11) 0.091 Uiso 0.35 calc PR 3 C67 C 0.3467(18) 0.1934(11) 0.4800(11) 0.058(4) Uiso 0.30 d P 4 H67A H 0.3485(18) 0.1358(11) 0.5132(11) 0.069 Uiso 0.30 calc PR 4 H67B H 0.3485(18) 0.1762(11) 0.4202(11) 0.069 Uiso 0.30 calc PR 4 C65 C 0.6198(16) 0.1963(11) 0.4801(11) 0.053(4) Uiso 0.30 d P 4 H65A H 0.6194(16) 0.1799(11) 0.4201(11) 0.063 Uiso 0.30 calc PR 4 H65B H 0.6194(16) 0.1380(11) 0.5124(11) 0.063 Uiso 0.30 calc PR 4 C63 C 0.4769(27) 0.3549(18) 0.4667(15) 0.080(6) Uiso 0.30 d P 5 H63A H 0.3886(27) 0.3870(18) 0.4881(15) 0.096 Uiso 0.30 calc PR 5 H63B H 0.5649(27) 0.3886(18) 0.4865(15) 0.096 Uiso 0.30 calc PR 5 C64 C 0.4741(23) 0.3527(15) 0.3670(14) 0.081(6) Uiso 0.30 d P 5 H64A H 0.4720(23) 0.4161(15) 0.3455(14) 0.097 Uiso 0.30 calc PR 5 H64B H 0.3864(23) 0.3196(15) 0.3480(14) 0.097 Uiso 0.30 calc PR 5 H64C H 0.5621(23) 0.3212(15) 0.3464(14) 0.097 Uiso 0.30 calc PR 5 C61B C 0.4777(29) 0.1653(17) 0.4368(16) 0.065(7) Uiso 0.20 d P 6 H61C H 0.3840(29) 0.1653(17) 0.4054(16) 0.078 Uiso 0.20 calc PR 6 H61D H 0.5591(29) 0.1716(17) 0.3962(16) 0.078 Uiso 0.20 calc PR 6 C62B C 0.4937(35) 0.0744(22) 0.4844(21) 0.090(9) Uiso 0.20 d P 6 H62D H 0.4919(35) 0.0227(22) 0.4449(21) 0.108 Uiso 0.20 calc PR 6 H62E H 0.4123(35) 0.0680(22) 0.5240(21) 0.108 Uiso 0.20 calc PR 6 H62F H 0.5870(35) 0.0742(22) 0.5148(21) 0.108 Uiso 0.20 calc PR 6 C67B C 0.3442(27) 0.2611(20) 0.5462(16) 0.060(6) Uiso 0.20 d P 7 H67C H 0.3455(27) 0.3235(20) 0.5715(16) 0.073 Uiso 0.20 calc PR 7 H67D H 0.3455(27) 0.2161(20) 0.5926(16) 0.073 Uiso 0.20 calc PR 7 C65B C 0.6118(24) 0.2595(20) 0.5449(15) 0.054(6) Uiso 0.20 d P 7 H65C H 0.6098(24) 0.2131(20) 0.5904(15) 0.065 Uiso 0.20 calc PR 7 H65D H 0.6098(24) 0.3211(20) 0.5718(15) 0.065 Uiso 0.20 calc PR 7 C63B C 0.4800(26) 0.3359(14) 0.4321(16) 0.037(6) Uiso 0.20 d P 8 H63C H 0.5740(26) 0.3334(14) 0.4011(16) 0.045 Uiso 0.20 calc PR 8 H63D H 0.4007(26) 0.3236(14) 0.3913(16) 0.045 Uiso 0.20 calc PR 8 C64B C 0.4617(35) 0.4276(23) 0.4614(21) 0.053(7) Uiso 0.15 d P 8 H64D H 0.4639(35) 0.4704(23) 0.4141(21) 0.064 Uiso 0.15 calc PR 8 H64E H 0.5413(35) 0.4428(23) 0.5002(21) 0.064 Uiso 0.15 calc PR 8 H64F H 0.3672(35) 0.4329(23) 0.4902(21) 0.064 Uiso 0.15 calc PR 8 C68 C 0.1953(7) 0.2500 0.5000 0.077(2) Uani 1 d S . H68A H 0.1105(7) 0.2112 0.4862 0.093 Uiso 0.30 calc PR 4 H68B H 0.1923(7) 0.3066 0.4664 0.093 Uiso 0.30 calc PR 4 H68C H 0.1923(7) 0.2661 0.5594 0.093 Uiso 0.30 calc PR 4 H68D H 0.1145(7) 0.2595 0.5395 0.093 Uiso 0.20 calc PR 7 H68E H 0.1887(7) 0.1877 0.4763 0.093 Uiso 0.20 calc PR 7 H68F H 0.1887(7) 0.2957 0.4551 0.093 Uiso 0.20 calc PR 7 C66 C 0.7633(7) 0.2500 0.5000 0.072(2) Uani 1 d S . H66A H 0.8483(7) 0.2116 0.4858 0.087 Uiso 0.30 calc PR 4 H66B H 0.7660(7) 0.2651 0.5596 0.087 Uiso 0.30 calc PR 4 H66C H 0.7660(7) 0.3071 0.4672 0.087 Uiso 0.30 calc PR 4 H66D H 0.8426(7) 0.2586 0.5406 0.087 Uiso 0.20 calc PR 7 H66E H 0.7712(7) 0.2970 0.4563 0.087 Uiso 0.20 calc PR 7 H66F H 0.7712(7) 0.1884 0.4750 0.087 Uiso 0.20 calc PR 7 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 Fe 0.0332(4) 0.0457(5) 0.0446(5) 0.000 0.000 -0.0011(5) S1 0.0496(10) 0.0482(9) 0.0836(12) 0.000 0.000 -0.0092(9) S2 0.0618(8) 0.0931(10) 0.0584(8) 0.0202(7) -0.0107(8) 0.0061(8) N4 0.028(2) 0.040(3) 0.043(3) 0.000 0.000 0.000(2) C5 0.038(4) 0.078(5) 0.102(6) 0.000 0.000 -0.005(4) N5 0.044(4) 0.116(6) 0.191(9) 0.000 0.000 -0.012(4) C14 0.058(4) 0.045(4) 0.113(6) 0.000 0.000 0.007(4) C41 0.037(4) 0.048(4) 0.084(8) -0.005(4) 0.011(4) 0.009(4) C24 0.075(4) 0.092(4) 0.051(3) 0.014(3) 0.013(3) -0.010(3) C42 0.038(5) 0.066(6) 0.071(7) -0.001(6) 0.016(5) -0.009(5) C43 0.050(6) 0.061(6) 0.053(6) 0.009(5) -0.022(5) 0.000(5) N6 0.039(3) 0.055(3) 0.059(3) -0.012(3) 0.000 0.000 C68 0.036(4) 0.101(6) 0.095(6) 0.021(5) 0.000 0.000 C66 0.040(4) 0.103(6) 0.074(5) -0.018(5) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C5 1.920(7) . ? Fe N4 2.046(4) . ? Fe S2 2.1842(13) 6_556 ? Fe S2 2.1842(13) . ? Fe S1 2.187(2) . ? S1 C14 1.812(7) . ? S2 C24 1.805(5) . ? N4 C41 1.474(8) . ? N4 C41 1.474(8) 6_556 ? N4 C42 1.483(9) 6_556 ? N4 C42 1.483(9) . ? N4 C43 1.526(9) . ? N4 C43 1.526(9) 6_556 ? C5 N5 1.095(8) . ? C14 C41 1.444(9) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C41 H41A 0.97 . ? C41 H41B 0.97 . ? C24 C43 1.448(10) 6_556 ? C24 C42 1.466(10) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C24 H24C 0.97 . ? C24 H24D 0.97 . ? C42 H42A 0.97 . ? C42 H42B 0.97 . ? C43 C24 1.448(10) 6_556 ? C43 H43A 0.97 . ? C43 H43B 0.97 . ? N6 C65B 1.38(2) . ? N6 C65B 1.38(2) 3_556 ? N6 C67B 1.42(2) 3_556 ? N6 C67B 1.42(2) . ? N6 C67 1.47(2) . ? N6 C67 1.47(2) 3_556 ? N6 C65 1.49(2) 3_556 ? N6 C65 1.493(15) . ? N6 C61B 1.56(2) . ? N6 C61B 1.56(2) 3_556 ? N6 C63 1.58(2) 3_556 ? N6 C63 1.58(2) . ? C61 C62 1.40(2) . ? C61 H61A 0.97 . ? C61 H61B 0.97 . ? C62 H62A 0.96 . ? C62 H62B 0.96 . ? C62 H62C 0.96 . ? C67 C68 1.60(2) . ? C67 H67A 0.97 . ? C67 H67B 0.97 . ? C65 C66 1.522(15) . ? C65 H65A 0.97 . ? C65 H65B 0.97 . ? C63 C64 1.57(3) . ? C63 H63A 0.97 . ? C63 H63B 0.97 . ? C64 H64A 0.96 . ? C64 H64B 0.96 . ? C64 H64C 0.96 . ? C61B C62B 1.50(4) . ? C61B H61C 0.97 . ? C61B H61D 0.97 . ? C62B H62D 0.96 . ? C62B H62E 0.96 . ? C62B H62F 0.96 . ? C67B C68 1.52(2) . ? C67B H67C 0.97 . ? C67B H67D 0.97 . ? C65B C66 1.53(2) . ? C65B H65C 0.97 . ? C65B H65D 0.97 . ? C63B C64B 1.39(4) . ? C63B H63C 0.97 . ? C63B H63D 0.97 . ? C64B H64D 0.96 . ? C64B H64E 0.96 . ? C64B H64F 0.96 . ? C68 H68A 0.96 . ? C68 H68B 0.96 . ? C68 H68C 0.96 . ? C68 H68D 0.96 . ? C68 H68E 0.96 . ? C68 H68F 0.96 . ? C66 H66A 0.96 . ? C66 H66B 0.96 . ? C66 H66C 0.96 . ? C66 H66D 0.96 . ? C66 H66E 0.96 . ? C66 H66F 0.96 . ? 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 C5 Fe N4 179.2(3) . . ? C5 Fe S2 91.85(12) . 6_556 ? N4 Fe S2 88.56(8) . 6_556 ? C5 Fe S2 91.85(12) . . ? N4 Fe S2 88.57(8) . . ? S2 Fe S2 120.99(8) 6_556 . ? C5 Fe S1 91.1(2) . . ? N4 Fe S1 88.10(14) . . ? S2 Fe S1 119.39(4) 6_556 . ? S2 Fe S1 119.39(4) . . ? C14 S1 Fe 100.6(2) . . ? C24 S2 Fe 100.5(2) . . ? C41 N4 C41 38.5(7) . 6_556 ? C41 N4 C42 136.4(6) . 6_556 ? C41 N4 C42 110.2(5) 6_556 6_556 ? C41 N4 C42 110.2(5) . . ? C41 N4 C42 136.4(6) 6_556 . ? C42 N4 C42 70.3(9) 6_556 . ? C41 N4 C43 108.4(6) . . ? C41 N4 C43 72.7(5) 6_556 . ? C41 N4 C43 72.7(5) . 6_556 ? C41 N4 C43 108.4(6) 6_556 6_556 ? C43 N4 C43 136.5(8) . 6_556 ? C41 N4 Fe 110.6(4) . . ? C41 N4 Fe 110.6(4) 6_556 . ? C42 N4 Fe 109.7(4) 6_556 . ? C42 N4 Fe 109.7(4) . . ? C43 N4 Fe 109.9(4) . . ? C43 N4 Fe 109.9(4) 6_556 . ? N5 C5 Fe 178.7(8) . . ? C41 C14 S1 110.9(5) . . ? C41 C14 H14A 109.5(3) . . ? S1 C14 H14A 109.5(2) . . ? C41 C14 H14B 109.5(4) . . ? S1 C14 H14B 109.45(3) . . ? H14A C14 H14B 108.0 . . ? C14 C41 N4 115.2(6) . . ? C14 C41 H41A 108.5(4) . . ? N4 C41 H41A 108.5(3) . . ? C14 C41 H41B 108.5(4) . . ? N4 C41 H41B 108.5(4) . . ? H41A C41 H41B 107.5 . . ? C43 C24 S2 111.4(5) 6_556 . ? C42 C24 S2 111.1(4) . . ? C42 C24 H24A 109.4(5) . . ? S2 C24 H24A 109.4(2) . . ? C42 C24 H24B 109.4(5) . . ? S2 C24 H24B 109.4(2) . . ? H24A C24 H24B 108.0 . . ? C43 C24 H24C 109.3(5) 6_556 . ? S2 C24 H24C 109.3(2) . . ? C43 C24 H24D 109.3(4) 6_556 . ? S2 C24 H24D 109.3(2) . . ? H24C C24 H24D 108.0 . . ? C24 C42 N4 114.3(7) . . ? C24 C42 H42A 108.7(4) . . ? N4 C42 H42A 108.7(4) . . ? C24 C42 H42B 108.7(5) . . ? N4 C42 H42B 108.7(4) . . ? H42A C42 H42B 107.6 . . ? C24 C43 N4 112.9(7) 6_556 . ? C24 C43 H43A 109.0(4) 6_556 . ? N4 C43 H43A 109.0(4) . . ? C24 C43 H43B 109.0(5) 6_556 . ? N4 C43 H43B 109.0(4) . . ? H43A C43 H43B 107.8 . . ? C65B N6 C65B 62.9(20) . 3_556 ? C65B N6 C67B 179.2(17) . 3_556 ? C65B N6 C67B 117.1(13) 3_556 3_556 ? C65B N6 C67B 117.1(13) . . ? C65B N6 C67B 179.2(17) 3_556 . ? C67B N6 C67B 62.9(20) 3_556 . ? C67 N6 C67 71.7(12) . 3_556 ? C67 N6 C65 177.6(9) . 3_556 ? C67 N6 C65 110.7(8) 3_556 3_556 ? C67 N6 C65 110.7(8) . . ? C67 N6 C65 177.6(9) 3_556 . ? C65 N6 C65 66.9(12) 3_556 . ? C61B N6 C61B 178.3(20) . 3_556 ? C63 N6 C63 177.8(18) 3_556 . ? C62 C61 N6 119.6(13) . . ? C62 C61 H61A 107.4(10) . . ? N6 C61 H61A 107.4(6) . . ? C62 C61 H61B 107.4(10) . . ? N6 C61 H61B 107.4(6) . . ? H61A C61 H61B 107.0 . . ? C61 C62 H62A 109.5(10) . . ? C61 C62 H62B 109.5(10) . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5(10) . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N6 C67 C68 111.6(9) . . ? N6 C67 H67A 109.3(7) . . ? C68 C67 H67A 109.3(6) . . ? N6 C67 H67B 109.3(7) . . ? C68 C67 H67B 109.3(6) . . ? H67A C67 H67B 108.0 . . ? N6 C65 C66 113.8(10) . . ? N6 C65 H65A 108.8(6) . . ? C66 C65 H65A 108.8(6) . . ? N6 C65 H65B 108.8(7) . . ? C66 C65 H65B 108.8(7) . . ? H65A C65 H65B 107.7 . . ? C64 C63 N6 108.2(19) . . ? C64 C63 H63A 110.0(13) . . ? N6 C63 H63A 110.0(9) . . ? C64 C63 H63B 110.0(12) . . ? N6 C63 H63B 110.0(9) . . ? H63A C63 H63B 108.4 . . ? C63 C64 H64A 109.5(13) . . ? C63 C64 H64B 109.5(12) . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5(13) . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62B C61B N6 110.1(20) . . ? C62B C61B H61C 109.6(16) . . ? N6 C61B H61C 109.6(10) . . ? C62B C61B H61D 109.6(16) . . ? N6 C61B H61D 109.6(10) . . ? H61C C61B H61D 108.2 . . ? C61B C62B H62D 109.5(16) . . ? C61B C62B H62E 109.5(16) . . ? H62D C62B H62E 109.5 . . ? C61B C62B H62F 109.5(16) . . ? H62D C62B H62F 109.5 . . ? H62E C62B H62F 109.5 . . ? N6 C67B C68 119.4(16) . . ? N6 C67B H67C 107.5(11) . . ? C68 C67B H67C 107.5(10) . . ? N6 C67B H67D 107.5(11) . . ? C68 C67B H67D 107.5(10) . . ? H67C C67B H67D 107.0 . . ? N6 C65B C66 120.5(16) . . ? N6 C65B H65C 107.2(11) . . ? C66 C65B H65C 107.2(10) . . ? N6 C65B H65D 107.2(11) . . ? C66 C65B H65D 107.2(10) . . ? H65C C65B H65D 106.8 . . ? C64B C63B N6 119.1(23) . . ? C64B C63B H63C 107.6(16) . . ? N6 C63B H63C 107.6(8) . . ? C64B C63B H63D 107.6(17) . . ? N6 C63B H63D 107.6(8) . . ? H63C C63B H63D 107.0 . . ? C63B C64B H64D 109.5(18) . . ? C63B C64B H64E 109.5(17) . . ? H64D C64B H64E 109.5 . . ? C63B C64B H64F 109.5(16) . . ? H64D C64B H64F 109.5 . . ? H64E C64B H64F 109.5 . . ? C67 C68 H68A 109.5(6) . . ? C67 C68 H68B 109.5(6) . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5(6) . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67B C68 H68D 109.5(9) . . ? C67B C68 H68E 109.5(10) . . ? H68D C68 H68E 109.5 . . ? C67B C68 H68F 109.5(10) . . ? H68D C68 H68F 109.5 . . ? H68E C68 H68F 109.5 . . ? C65 C66 H66A 109.5(6) . . ? C65 C66 H66B 109.5(6) . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5(7) . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65B C66 H66D 109.5(9) . . ? C65B C66 H66E 109.5(10) . . ? H66D C66 H66E 109.5 . . ? C65B C66 H66F 109.5(10) . . ? H66D C66 H66F 109.5 . . ? H66E C66 H66F 109.5 . . ? _refine_diff_density_max 0.520 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.064 #===END