# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'Konstantin Shuvaev' ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'Louise Dawe' ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'Laurence K Thompson' ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; _publ_contact_author_name 'Konstantin Shuvaev' _publ_contact_author_email KSHUVAEV@MUN.CA _publ_section_title ; Formation of unusual molecular rectangles and squares containing low spin and high spin Co(II) and Fe(II) centers ; _publ_contact_author_address ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; _publ_contact_author_fax 1-709-737-3702 _publ_contact_author_phone 1-709-737-8750 # Attachment 'KS_Paper_Submission_CIF_Revised2.cif' data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 743062' #TrackingRef 'KS_Paper_Submission_CIF_Revised2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 Co4 N24 O4, 2 (C F3 O3 S), 5 (C H4 O)' _chemical_formula_sum 'C67 H78 Co4 F6 N24 O15 S2' _chemical_formula_weight 1873.35 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.230(9) _cell_length_b 11.985(4) _cell_length_c 27.967(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.532(7) _cell_angle_gamma 90.00 _cell_volume 8222(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 16625 _cell_measurement_theta_min 2.5307 _cell_measurement_theta_max 30.6790 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3848 _exptl_absorpt_coefficient_mu 0.934 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9686 _exptl_absorpt_correction_T_min 0.8975 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 53299 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8511 _reflns_number_gt 7695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+26.2140P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8511 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1931 _refine_ls_wR_factor_gt 0.1853 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 -0.026 986 206 'Disordered CH3OH-See Details' 2 0.000 0.500 0.240 986 206 'Disordered CH3OH-See Details' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 412 electrons per unit cell in two voids (total volume 1972 ^A^3); that is 103 electrons per formula unit. Disordered solvent lattice methanol molecules were present prior to the application of Squeeze, however, a satisfactory point atom model could not be achieved. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.31623(2) 0.85134(4) 0.099240(17) 0.03201(16) Uani 1 1 d . . . Co2 Co 0.35344(2) 0.60161(4) 0.029279(18) 0.03322(16) Uani 1 1 d . . . S1 S 0.12278(4) 0.84224(9) 0.18977(4) 0.0432(3) Uani 1 1 d . . . F1 F 0.04817(13) 0.7321(3) 0.22228(10) 0.0662(8) Uani 1 1 d . . . F2 F 0.09120(15) 0.6342(3) 0.17940(13) 0.0743(9) Uani 1 1 d . . . F3 F 0.03042(12) 0.7510(3) 0.14399(10) 0.0658(8) Uani 1 1 d . . . O1 O 0.35814(11) 0.7609(2) 0.06513(9) 0.0355(6) Uani 1 1 d . . . O2 O 0.30540(14) 0.9584(3) 0.04877(11) 0.0478(7) Uani 1 1 d . . . O3 O 0.14038(15) 0.8304(3) 0.14436(13) 0.0600(9) Uani 1 1 d . . . O4 O 0.09441(13) 0.9438(3) 0.19440(11) 0.0501(7) Uani 1 1 d . . . O5 O 0.16204(15) 0.8110(3) 0.23383(13) 0.0624(9) Uani 1 1 d . . . N1 N 0.29256(13) 0.9560(3) 0.14161(11) 0.0348(7) Uani 1 1 d . . . N2 N 0.38485(14) 0.9111(3) 0.12717(13) 0.0402(7) Uani 1 1 d . . . N3 N 0.42700(14) 0.8781(3) 0.10863(14) 0.0441(8) Uani 1 1 d . . . N4 N 0.44464(14) 0.7655(3) 0.04838(13) 0.0431(8) Uani 1 1 d . . . N5 N 0.42272(14) 0.6768(3) 0.01929(12) 0.0381(7) Uani 1 1 d . . . N6 N 0.37896(13) 0.4978(3) -0.02319(12) 0.0375(7) Uani 1 1 d . . . N7 N 0.31189(14) 0.7312(3) 0.14295(12) 0.0390(7) Uani 1 1 d . . . N8 N 0.24754(14) 0.8016(3) 0.06569(12) 0.0392(7) Uani 1 1 d . . . N9 N 0.22387(16) 0.8633(4) 0.02477(13) 0.0548(11) Uani 1 1 d . . . N10 N 0.24946(19) 1.0319(4) -0.01902(19) 0.0683(13) Uani 1 1 d . . . N11 N 0.20239(19) 1.0083(4) -0.04472(19) 0.0730(14) Uani 1 1 d . . . N12 N 0.10664(18) 0.9771(4) -0.09751(14) 0.0574(11) Uani 1 1 d . . . C1 C 0.24204(16) 0.9734(3) 0.14686(14) 0.0381(8) Uani 1 1 d . . . H1 H 0.2131 0.9295 0.1282 0.046 Uiso 1 1 calc R . . C2 C 0.23038(18) 1.0535(4) 0.17858(15) 0.0439(9) Uani 1 1 d . . . H2 H 0.1940 1.0654 0.1815 0.053 Uiso 1 1 calc R . . C3 C 0.27299(19) 1.1156(4) 0.20596(16) 0.0466(10) Uani 1 1 d . . . H3 H 0.2662 1.1710 0.2281 0.056 Uiso 1 1 calc R . . C4 C 0.32516(18) 1.0971(3) 0.20104(15) 0.0425(9) Uani 1 1 d . . . H4 H 0.3546 1.1392 0.2200 0.051 Uiso 1 1 calc R . . C5 C 0.33491(17) 1.0170(3) 0.16846(14) 0.0384(8) Uani 1 1 d . . . C6 C 0.38805(17) 0.9917(4) 0.15917(16) 0.0437(9) Uani 1 1 d . . . C7 C 0.43908(19) 1.0522(5) 0.1814(2) 0.0600(13) Uani 1 1 d . . . H5 H 0.4304 1.1291 0.1888 0.072 Uiso 1 1 calc R . . H6 H 0.4629 1.0528 0.1583 0.072 Uiso 1 1 calc R . . H7 H 0.4577 1.0148 0.2119 0.072 Uiso 1 1 calc R . . C8 C 0.40936(16) 0.8007(3) 0.07359(14) 0.0378(8) Uani 1 1 d . . . C9 C 0.44811(16) 0.6390(4) -0.01259(14) 0.0387(8) Uani 1 1 d . . . C10 C 0.49775(18) 0.6921(4) -0.02340(15) 0.0439(9) Uani 1 1 d . . . H8 H 0.5188 0.7288 0.0063 0.053 Uiso 1 1 calc R . . H9 H 0.4867 0.7476 -0.0496 0.053 Uiso 1 1 calc R . . H10 H 0.5202 0.6348 -0.0340 0.053 Uiso 1 1 calc R . . C11 C 0.42275(16) 0.5390(3) -0.03842(14) 0.0383(8) Uani 1 1 d . . . C12 C 0.44126(18) 0.4882(4) -0.07591(15) 0.0440(9) Uani 1 1 d . . . H11 H 0.4711 0.5187 -0.0869 0.053 Uiso 1 1 calc R . . C13 C 0.4155(2) 0.3919(4) -0.09722(16) 0.0501(11) Uani 1 1 d . . . H12 H 0.4276 0.3560 -0.1230 0.060 Uiso 1 1 calc R . . C14 C 0.3724(2) 0.3488(4) -0.08100(16) 0.0494(10) Uani 1 1 d . . . H13 H 0.3550 0.2820 -0.0947 0.059 Uiso 1 1 calc R . . C15 C 0.35496(18) 0.4050(4) -0.04401(16) 0.0445(9) Uani 1 1 d . . . H14 H 0.3247 0.3761 -0.0331 0.053 Uiso 1 1 calc R . . C16 C 0.3485(2) 0.6997(4) 0.18317(15) 0.0509(11) Uani 1 1 d . . . H15 H 0.3816 0.7401 0.1937 0.061 Uiso 1 1 calc R . . C17 C 0.3377(3) 0.6057(5) 0.21016(18) 0.0696(17) Uani 1 1 d . . . H16 H 0.3637 0.5817 0.2386 0.084 Uiso 1 1 calc R . . C18 C 0.2893(3) 0.5498(5) 0.1947(2) 0.0704(16) Uani 1 1 d . . . H17 H 0.2819 0.4870 0.2128 0.084 Uiso 1 1 calc R . . C19 C 0.2519(3) 0.5828(4) 0.1540(2) 0.0614(14) Uani 1 1 d . . . H18 H 0.2182 0.5445 0.1436 0.074 Uiso 1 1 calc R . . C20 C 0.26400(19) 0.6736(4) 0.12786(17) 0.0474(10) Uani 1 1 d . . . C21 C 0.22735(17) 0.7157(4) 0.08303(17) 0.0462(10) Uani 1 1 d . . . C22 C 0.17264(19) 0.6668(4) 0.0598(2) 0.0597(13) Uani 1 1 d . . . H19 H 0.1729 0.5867 0.0669 0.072 Uiso 1 1 calc R . . H20 H 0.1647 0.6783 0.0242 0.072 Uiso 1 1 calc R . . H21 H 0.1446 0.7035 0.0733 0.072 Uiso 1 1 calc R . . C23 C 0.2598(2) 0.9470(4) 0.01951(17) 0.0529(11) Uani 1 1 d . . . C24 C 0.1891(3) 1.0841(5) -0.0828(2) 0.0714(18) Uani 1 1 d . . . C25 C 0.2217(3) 1.1809(6) -0.0942(2) 0.084(2) Uani 1 1 d . . . H22 H 0.2606 1.1643 -0.0831 0.101 Uiso 1 1 calc R . . H23 H 0.2130 1.2476 -0.0773 0.101 Uiso 1 1 calc R . . H24 H 0.2126 1.1942 -0.1298 0.101 Uiso 1 1 calc R . . C26 C 0.1345(2) 1.0587(5) -0.11312(19) 0.0644(15) Uani 1 1 d . . . C27 C 0.1126(3) 1.1146(6) -0.1575(2) 0.081(2) Uani 1 1 d . . . H25 H 0.1324 1.1732 -0.1682 0.098 Uiso 1 1 calc R . . C28 C 0.0629(3) 1.0844(7) -0.1851(2) 0.098(3) Uani 1 1 d . . . H26 H 0.0477 1.1219 -0.2150 0.117 Uiso 1 1 calc R . . C29 C 0.0351(3) 1.0012(7) -0.1698(2) 0.085(2) Uani 1 1 d . . . H27 H 0.0004 0.9794 -0.1890 0.103 Uiso 1 1 calc R . . C30 C 0.0578(2) 0.9470(6) -0.12541(18) 0.0673(16) Uani 1 1 d . . . H28 H 0.0383 0.8878 -0.1148 0.081 Uiso 1 1 calc R . . C31 C 0.0708(2) 0.7345(4) 0.18351(16) 0.0511(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0342(3) 0.0364(3) 0.0247(3) -0.00131(19) 0.0055(2) -0.0054(2) Co2 0.0359(3) 0.0366(3) 0.0276(3) 0.00175(19) 0.0083(2) -0.0012(2) S1 0.0449(6) 0.0425(6) 0.0404(5) 0.0046(4) 0.0063(4) -0.0025(4) F1 0.078(2) 0.077(2) 0.0479(15) 0.0056(14) 0.0233(14) -0.0220(16) F2 0.097(2) 0.0462(16) 0.076(2) -0.0062(15) 0.0131(18) -0.0080(16) F3 0.0629(18) 0.082(2) 0.0440(15) 0.0033(14) -0.0039(13) -0.0181(15) O1 0.0382(14) 0.0387(14) 0.0298(13) -0.0026(11) 0.0081(10) -0.0056(11) O2 0.0631(19) 0.0454(16) 0.0371(15) 0.0068(13) 0.0165(14) -0.0001(14) O3 0.067(2) 0.061(2) 0.060(2) 0.0000(17) 0.0313(18) -0.0086(17) O4 0.0615(19) 0.0424(16) 0.0432(16) -0.0014(13) 0.0057(14) 0.0025(14) O5 0.061(2) 0.0537(19) 0.062(2) 0.0086(17) -0.0079(17) -0.0006(16) N1 0.0405(17) 0.0373(16) 0.0252(14) 0.0006(12) 0.0050(12) -0.0051(13) N2 0.0395(17) 0.0428(18) 0.0382(17) -0.0086(14) 0.0087(14) -0.0090(14) N3 0.0386(18) 0.0463(19) 0.049(2) -0.0110(16) 0.0131(15) -0.0062(15) N4 0.0443(19) 0.0459(19) 0.0429(18) -0.0085(15) 0.0181(15) -0.0080(15) N5 0.0407(18) 0.0414(17) 0.0346(16) 0.0011(14) 0.0138(14) -0.0024(14) N6 0.0396(17) 0.0422(18) 0.0307(15) 0.0022(13) 0.0081(13) 0.0060(14) N7 0.0473(19) 0.0423(18) 0.0293(15) 0.0007(13) 0.0125(14) -0.0014(15) N8 0.0379(17) 0.0428(18) 0.0371(17) -0.0126(14) 0.0093(14) -0.0041(14) N9 0.050(2) 0.078(3) 0.0293(17) -0.0181(18) -0.0047(15) 0.025(2) N10 0.061(3) 0.065(3) 0.091(3) -0.031(3) 0.042(3) -0.029(2) N11 0.060(3) 0.086(3) 0.083(3) -0.042(3) 0.038(2) -0.019(2) N12 0.073(3) 0.069(3) 0.0367(19) 0.0190(18) 0.0261(19) 0.033(2) C1 0.038(2) 0.045(2) 0.0300(18) -0.0007(16) 0.0067(15) -0.0051(16) C2 0.047(2) 0.050(2) 0.037(2) -0.0034(18) 0.0130(17) -0.0006(19) C3 0.058(3) 0.044(2) 0.038(2) -0.0047(18) 0.0122(19) -0.001(2) C4 0.050(2) 0.041(2) 0.0330(19) -0.0066(16) 0.0018(17) -0.0052(18) C5 0.044(2) 0.038(2) 0.0311(18) -0.0057(15) 0.0037(16) -0.0073(16) C6 0.040(2) 0.046(2) 0.044(2) -0.0145(18) 0.0075(17) -0.0127(18) C7 0.039(2) 0.068(3) 0.068(3) -0.033(3) 0.004(2) -0.012(2) C8 0.038(2) 0.041(2) 0.0349(19) -0.0022(16) 0.0095(15) -0.0094(16) C9 0.0357(19) 0.050(2) 0.0305(18) 0.0080(16) 0.0082(15) 0.0038(17) C10 0.046(2) 0.053(2) 0.035(2) 0.0058(18) 0.0146(17) -0.0012(19) C11 0.040(2) 0.046(2) 0.0288(18) 0.0075(16) 0.0074(15) 0.0092(17) C12 0.048(2) 0.052(2) 0.035(2) 0.0015(18) 0.0154(17) 0.0105(19) C13 0.061(3) 0.055(3) 0.035(2) -0.0008(19) 0.013(2) 0.012(2) C14 0.057(3) 0.050(3) 0.039(2) -0.0064(19) 0.008(2) -0.002(2) C15 0.046(2) 0.048(2) 0.038(2) -0.0044(18) 0.0083(18) 0.0026(19) C16 0.066(3) 0.058(3) 0.0280(19) 0.0051(18) 0.0088(19) 0.013(2) C17 0.100(4) 0.078(4) 0.032(2) 0.010(2) 0.020(3) 0.037(3) C18 0.104(5) 0.050(3) 0.072(4) 0.001(3) 0.052(4) -0.007(3) C19 0.082(4) 0.048(3) 0.067(3) 0.001(2) 0.044(3) -0.006(2) C20 0.054(3) 0.044(2) 0.052(3) -0.0072(19) 0.028(2) -0.0104(19) C21 0.036(2) 0.051(2) 0.054(2) -0.022(2) 0.0145(18) -0.0043(18) C22 0.043(2) 0.062(3) 0.076(3) -0.030(3) 0.017(2) -0.018(2) C23 0.073(3) 0.055(3) 0.038(2) 0.002(2) 0.027(2) 0.010(2) C24 0.112(5) 0.066(3) 0.049(3) 0.036(3) 0.045(3) 0.040(3) C25 0.081(4) 0.115(5) 0.056(3) 0.029(3) 0.014(3) 0.022(4) C26 0.080(4) 0.072(3) 0.048(3) 0.028(3) 0.030(3) 0.037(3) C27 0.108(5) 0.088(4) 0.060(3) 0.039(3) 0.045(4) 0.049(4) C28 0.095(5) 0.138(7) 0.064(4) 0.055(4) 0.026(4) 0.071(5) C29 0.074(4) 0.134(6) 0.051(3) 0.029(4) 0.021(3) 0.053(4) C30 0.060(3) 0.103(4) 0.041(2) 0.009(3) 0.014(2) 0.035(3) C31 0.065(3) 0.050(3) 0.039(2) 0.0004(19) 0.012(2) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N8 1.865(3) . ? Co1 N2 1.867(3) . ? Co1 O2 1.880(3) . ? Co1 N7 1.908(3) . ? Co1 N1 1.914(3) . ? Co1 O1 1.917(3) . ? Co2 N5 2.043(3) . ? Co2 N11 2.047(5) 7_565 ? Co2 N6 2.135(3) . ? Co2 O1 2.146(3) . ? Co2 N12 2.156(4) 7_565 ? Co2 N9 2.210(4) 7_565 ? S1 O4 1.433(3) . ? S1 O5 1.438(3) . ? S1 O3 1.447(4) . ? S1 C31 1.820(5) . ? F1 C31 1.338(5) . ? F2 C31 1.323(6) . ? F3 C31 1.331(5) . ? O1 C8 1.346(5) . ? O2 C23 1.254(6) . ? N1 C1 1.333(5) . ? N1 C5 1.366(5) . ? N2 C6 1.307(5) . ? N2 N3 1.347(5) . ? N3 C8 1.347(5) . ? N4 C8 1.327(5) . ? N4 N5 1.374(5) . ? N5 C9 1.295(5) . ? N6 C15 1.333(5) . ? N6 C11 1.366(5) . ? N7 C16 1.332(5) . ? N7 C20 1.370(6) . ? N8 C21 1.293(6) . ? N8 N9 1.376(5) . ? N9 C23 1.382(7) . ? N9 Co2 2.210(4) 7_565 ? N10 N11 1.268(6) . ? N10 C23 1.460(7) . ? N11 C24 1.380(7) . ? N11 Co2 2.047(5) 7_565 ? N12 C26 1.336(7) . ? N12 C30 1.345(7) . ? N12 Co2 2.156(4) 7_565 ? C1 C2 1.384(6) . ? C1 H1 0.9500 . ? C2 C3 1.383(6) . ? C2 H2 0.9500 . ? C3 C4 1.373(6) . ? C3 H3 0.9500 . ? C4 C5 1.384(6) . ? C4 H4 0.9500 . ? C5 C6 1.456(6) . ? C6 C7 1.482(6) . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C7 H7 0.9800 . ? C9 C11 1.467(6) . ? C9 C10 1.497(6) . ? C10 H8 0.9800 . ? C10 H9 0.9800 . ? C10 H10 0.9800 . ? C11 C12 1.385(6) . ? C12 C13 1.389(7) . ? C12 H11 0.9500 . ? C13 C14 1.372(7) . ? C13 H12 0.9500 . ? C14 C15 1.390(6) . ? C14 H13 0.9500 . ? C15 H14 0.9500 . ? C16 C17 1.418(8) . ? C16 H15 0.9500 . ? C17 C18 1.369(9) . ? C17 H16 0.9500 . ? C18 C19 1.358(9) . ? C18 H17 0.9500 . ? C19 C20 1.383(7) . ? C19 H18 0.9500 . ? C20 C21 1.462(7) . ? C21 C22 1.500(6) . ? C22 H19 0.9800 . ? C22 H20 0.9800 . ? C22 H21 0.9800 . ? C24 C26 1.472(9) . ? C24 C25 1.498(9) . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C25 H24 0.9800 . ? C26 C27 1.405(7) . ? C27 C28 1.359(11) . ? C27 H25 0.9500 . ? C28 C29 1.343(11) . ? C28 H26 0.9500 . ? C29 C30 1.399(7) . ? C29 H27 0.9500 . ? C30 H28 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Co1 N2 173.95(16) . . ? N8 Co1 O2 83.44(15) . . ? N2 Co1 O2 90.58(15) . . ? N8 Co1 N7 83.98(15) . . ? N2 Co1 N7 101.99(15) . . ? O2 Co1 N7 167.42(15) . . ? N8 Co1 N1 97.64(14) . . ? N2 Co1 N1 83.28(14) . . ? O2 Co1 N1 90.35(14) . . ? N7 Co1 N1 91.42(14) . . ? N8 Co1 O1 97.15(13) . . ? N2 Co1 O1 81.94(13) . . ? O2 Co1 O1 90.73(13) . . ? N7 Co1 O1 90.74(13) . . ? N1 Co1 O1 165.19(12) . . ? N5 Co2 N11 164.95(19) . 7_565 ? N5 Co2 N6 75.99(13) . . ? N11 Co2 N6 95.92(15) 7_565 . ? N5 Co2 O1 73.51(12) . . ? N11 Co2 O1 116.04(14) 7_565 . ? N6 Co2 O1 147.86(12) . . ? N5 Co2 N12 94.40(16) . 7_565 ? N11 Co2 N12 74.6(2) 7_565 7_565 ? N6 Co2 N12 101.52(14) . 7_565 ? O1 Co2 N12 90.72(14) . 7_565 ? N5 Co2 N9 117.96(16) . 7_565 ? N11 Co2 N9 74.1(2) 7_565 7_565 ? N6 Co2 N9 90.03(13) . 7_565 ? O1 Co2 N9 95.38(13) . 7_565 ? N12 Co2 N9 147.49(18) 7_565 7_565 ? O4 S1 O5 113.7(2) . . ? O4 S1 O3 115.1(2) . . ? O5 S1 O3 115.8(2) . . ? O4 S1 C31 104.3(2) . . ? O5 S1 C31 103.5(2) . . ? O3 S1 C31 102.0(2) . . ? C8 O1 Co1 109.3(2) . . ? C8 O1 Co2 110.1(2) . . ? Co1 O1 Co2 139.37(14) . . ? C23 O2 Co1 111.4(3) . . ? C1 N1 C5 120.0(3) . . ? C1 N1 Co1 128.0(3) . . ? C5 N1 Co1 112.0(3) . . ? C6 N2 N3 123.6(3) . . ? C6 N2 Co1 118.2(3) . . ? N3 N2 Co1 117.7(3) . . ? C8 N3 N2 109.0(3) . . ? C8 N4 N5 109.5(3) . . ? C9 N5 N4 118.9(3) . . ? C9 N5 Co2 121.1(3) . . ? N4 N5 Co2 119.9(2) . . ? C15 N6 C11 118.9(4) . . ? C15 N6 Co2 127.4(3) . . ? C11 N6 Co2 113.5(3) . . ? C16 N7 C20 120.3(4) . . ? C16 N7 Co1 128.5(3) . . ? C20 N7 Co1 111.2(3) . . ? C21 N8 N9 127.4(4) . . ? C21 N8 Co1 117.9(3) . . ? N9 N8 Co1 114.7(3) . . ? N8 N9 C23 108.1(4) . . ? N8 N9 Co2 144.4(3) . 7_565 ? C23 N9 Co2 106.6(3) . 7_565 ? N11 N10 C23 104.2(4) . . ? N10 N11 C24 108.4(5) . . ? N10 N11 Co2 128.6(5) . 7_565 ? C24 N11 Co2 122.1(4) . 7_565 ? C26 N12 C30 119.2(5) . . ? C26 N12 Co2 115.9(4) . 7_565 ? C30 N12 Co2 124.8(4) . 7_565 ? N1 C1 C2 122.1(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 118.3(4) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C4 C3 C2 119.8(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.0(4) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 119.8(4) . . ? N1 C5 C6 115.1(3) . . ? C4 C5 C6 125.1(4) . . ? N2 C6 C5 111.4(3) . . ? N2 C6 C7 123.9(4) . . ? C5 C6 C7 124.7(4) . . ? C6 C7 H5 109.5 . . ? C6 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C6 C7 H7 109.5 . . ? H5 C7 H7 109.5 . . ? H6 C7 H7 109.5 . . ? N4 C8 O1 122.0(3) . . ? N4 C8 N3 117.2(3) . . ? O1 C8 N3 120.8(3) . . ? N5 C9 C11 113.3(4) . . ? N5 C9 C10 124.2(4) . . ? C11 C9 C10 122.5(4) . . ? C9 C10 H8 109.5 . . ? C9 C10 H9 109.5 . . ? H8 C10 H9 109.5 . . ? C9 C10 H10 109.5 . . ? H8 C10 H10 109.5 . . ? H9 C10 H10 109.5 . . ? N6 C11 C12 121.2(4) . . ? N6 C11 C9 115.7(3) . . ? C12 C11 C9 123.1(4) . . ? C11 C12 C13 118.9(4) . . ? C11 C12 H11 120.6 . . ? C13 C12 H11 120.6 . . ? C14 C13 C12 119.9(4) . . ? C14 C13 H12 120.0 . . ? C12 C13 H12 120.0 . . ? C13 C14 C15 118.5(4) . . ? C13 C14 H13 120.8 . . ? C15 C14 H13 120.8 . . ? N6 C15 C14 122.6(4) . . ? N6 C15 H14 118.7 . . ? C14 C15 H14 118.7 . . ? N7 C16 C17 119.6(5) . . ? N7 C16 H15 120.2 . . ? C17 C16 H15 120.2 . . ? C18 C17 C16 119.2(5) . . ? C18 C17 H16 120.4 . . ? C16 C17 H16 120.4 . . ? C19 C18 C17 121.0(5) . . ? C19 C18 H17 119.5 . . ? C17 C18 H17 119.5 . . ? C18 C19 C20 118.5(6) . . ? C18 C19 H18 120.8 . . ? C20 C19 H18 120.8 . . ? N7 C20 C19 121.4(5) . . ? N7 C20 C21 115.2(4) . . ? C19 C20 C21 123.4(5) . . ? N8 C21 C20 111.7(4) . . ? N8 C21 C22 123.5(5) . . ? C20 C21 C22 124.7(4) . . ? C21 C22 H19 109.5 . . ? C21 C22 H20 109.5 . . ? H19 C22 H20 109.5 . . ? C21 C22 H21 109.5 . . ? H19 C22 H21 109.5 . . ? H20 C22 H21 109.5 . . ? O2 C23 N9 122.3(4) . . ? O2 C23 N10 112.6(4) . . ? N9 C23 N10 125.1(5) . . ? N11 C24 C26 109.5(5) . . ? N11 C24 C25 129.0(6) . . ? C26 C24 C25 121.5(4) . . ? C24 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C25 H24 109.5 . . ? H22 C25 H24 109.5 . . ? H23 C25 H24 109.5 . . ? N12 C26 C27 120.6(6) . . ? N12 C26 C24 117.2(4) . . ? C27 C26 C24 122.2(6) . . ? C28 C27 C26 119.6(7) . . ? C28 C27 H25 120.2 . . ? C26 C27 H25 120.2 . . ? C29 C28 C27 119.9(5) . . ? C29 C28 H26 120.1 . . ? C27 C28 H26 120.1 . . ? C28 C29 C30 119.4(7) . . ? C28 C29 H27 120.3 . . ? C30 C29 H27 120.3 . . ? N12 C30 C29 121.2(6) . . ? N12 C30 H28 119.4 . . ? C29 C30 H28 119.4 . . ? F2 C31 F3 107.5(4) . . ? F2 C31 F1 107.4(4) . . ? F3 C31 F1 106.7(4) . . ? F2 C31 S1 111.5(4) . . ? F3 C31 S1 111.6(3) . . ? F1 C31 S1 111.8(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.680 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.099 data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 743063' #TrackingRef 'KS_Paper_Submission_CIF_Revised2.cif' # start Validation Reply Form _vrf_CHEMW03_Compound2 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: One disordered triflate anion and 13 disordered lattice solvent water molecules were removed via the Platon Squeeze procedure. These were included in the formula for the calculation of intensive properties (for example, molecular weight and density). ; _vrf_PLAT043_Compound2 ; PROBLEM: Check Reported Molecular Weight ................ 2011.58 RESPONSE: One disordered triflate anion and 13 disordered lattice solvent water molecules were removed via the Platon Squeeze procedure. These were included in the formula for the calculation of intensive properties (for example, molecular weight and density). ; _vrf_PLAT044_Compound2 ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: One disordered triflate anion and 13 disordered lattice solvent water molecules were removed via the Platon Squeeze procedure. These were included in the formula for the calculation of intensive properties (for example, molecular weight and density). ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C15 H14 N6 S), 2(C15 H15 N6 S), 4Co, 2(C F3 O3 S), 13(H2 O)' _chemical_formula_sum 'C62 H84 Co4 F6 N24 O19 S6' _chemical_formula_weight 2011.58 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.950(3) _cell_length_b 27.769(6) _cell_length_c 13.903(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.404(5) _cell_angle_gamma 90.00 _cell_volume 4487.9(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 17601 _cell_measurement_theta_min 2.5033 _cell_measurement_theta_max 30.9251 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2068 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_correction_T_min 0.8974 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite-Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 20154 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.50 _reflns_number_total 9406 _reflns_number_gt 6308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.002 -0.008 0.500 1557 422 '1(C F3 O3 S), 13(H2 O)' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 422 electrons per unit cell in one void (total volume 1557 ^A^3); that is 211 electrons per formula unit. One very badly disordered triflate anion, and several disordered solvent lattice water molecules were present prior to the application of Squeeze, however, despite numerous attempts at modeling, a satisfactory point atom model could not be achieved. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9406 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.2044 _refine_ls_wR_factor_gt 0.1877 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.63103(5) 0.42607(2) 0.18093(4) 0.03840(18) Uani 1 1 d . . . Co2 Co 0.37227(5) 0.52537(2) 0.20316(4) 0.03884(18) Uani 1 1 d . . . S1 S 0.54122(9) 0.49263(4) 0.20479(8) 0.0412(3) Uani 1 1 d . . . S2 S 0.75385(10) 0.47303(4) 0.12373(8) 0.0413(3) Uani 1 1 d . . . S3 S 0.7117(2) 0.2500 0.47738(17) 0.0740(6) Uani 1 2 d S . . F1 F 0.9076(3) 0.28790(13) 0.5748(3) 0.0937(12) Uani 1 1 d . . . F2 F 0.9189(6) 0.2500 0.4451(5) 0.116(2) Uani 1 2 d S . . O1 O 0.6766(7) 0.2500 0.5703(5) 0.101(2) Uani 1 2 d S . . O2 O 0.6899(4) 0.20545(15) 0.4254(4) 0.0979(15) Uani 1 1 d . . . N1 N 0.7394(3) 0.37362(13) 0.1866(3) 0.0432(9) Uani 1 1 d . . . N2 N 0.7060(3) 0.43229(13) 0.3167(3) 0.0404(8) Uani 1 1 d . . . N3 N 0.6754(3) 0.46470(14) 0.3813(3) 0.0419(8) Uani 1 1 d . . . N4 N 0.5513(3) 0.52706(13) 0.3862(3) 0.0441(9) Uani 1 1 d . . . N5 N 0.4578(3) 0.54983(13) 0.3273(3) 0.0417(8) Uani 1 1 d . . . N6 N 0.2843(3) 0.58375(13) 0.2076(3) 0.0464(9) Uani 1 1 d . . . N7 N 0.5069(3) 0.38402(12) 0.2025(3) 0.0413(8) Uani 1 1 d . . . N8 N 0.5491(3) 0.41993(13) 0.0476(3) 0.0423(9) Uani 1 1 d . . . N9 N 0.5829(3) 0.44135(13) -0.0284(3) 0.0422(8) Uani 1 1 d . . . N10 N 0.7081(3) 0.49188(13) -0.0742(3) 0.0428(9) Uani 1 1 d . . . N11 N 0.8034(3) 0.51992(13) -0.0415(3) 0.0431(9) Uani 1 1 d . . . N12 N 0.7239(3) 0.52164(13) -0.2654(3) 0.0436(9) Uani 1 1 d . . . C1 C 0.7608(4) 0.34731(17) 0.1119(4) 0.0509(12) Uani 1 1 d . . . H1 H 0.7094 0.3499 0.0488 0.061 Uiso 1 1 calc R . . C2 C 0.8528(5) 0.31693(17) 0.1220(4) 0.0587(14) Uani 1 1 d . . . H2 H 0.8657 0.2995 0.0668 0.070 Uiso 1 1 calc R . . C3 C 0.9266(5) 0.31203(18) 0.2141(5) 0.0618(14) Uani 1 1 d . . . H3 H 0.9915 0.2914 0.2231 0.074 Uiso 1 1 calc R . . C4 C 0.9048(4) 0.33732(16) 0.2920(4) 0.0527(12) Uani 1 1 d . . . H4 H 0.9525 0.3330 0.3563 0.063 Uiso 1 1 calc R . . C5 C 0.8131(4) 0.36923(16) 0.2774(4) 0.0455(11) Uani 1 1 d . . . C6 C 0.7869(4) 0.40139(16) 0.3518(3) 0.0455(11) Uani 1 1 d . . . C7 C 0.8509(4) 0.39891(18) 0.4578(4) 0.0528(12) Uani 1 1 d . . . H5 H 0.8752 0.3657 0.4745 0.063 Uiso 1 1 calc R . . H6 H 0.8007 0.4097 0.5002 0.063 Uiso 1 1 calc R . . H7 H 0.9188 0.4198 0.4681 0.063 Uiso 1 1 calc R . . C8 C 0.5921(4) 0.49406(16) 0.3347(3) 0.0397(10) Uani 1 1 d . . . C9 C 0.4186(4) 0.58887(18) 0.3608(3) 0.0477(11) Uani 1 1 d . . . C10 C 0.4716(5) 0.6086(2) 0.4595(4) 0.0675(15) Uani 1 1 d . . . H8 H 0.5470 0.6223 0.4589 0.081 Uiso 1 1 calc R . . H9 H 0.4811 0.5827 0.5088 0.081 Uiso 1 1 calc R . . H10 H 0.4220 0.6337 0.4764 0.081 Uiso 1 1 calc R . . C11 C 0.3211(4) 0.60986(17) 0.2913(4) 0.0514(12) Uani 1 1 d . . . C12 C 0.2710(6) 0.6535(2) 0.3065(4) 0.0777(19) Uani 1 1 d . . . H11 H 0.2950 0.6707 0.3669 0.093 Uiso 1 1 calc R . . C13 C 0.1848(6) 0.6711(2) 0.2303(5) 0.090(2) Uani 1 1 d . . . H12 H 0.1505 0.7014 0.2377 0.108 Uiso 1 1 calc R . . C14 C 0.1480(5) 0.6456(2) 0.1441(4) 0.0755(18) Uani 1 1 d . . . H13 H 0.0888 0.6577 0.0919 0.091 Uiso 1 1 calc R . . C15 C 0.2001(5) 0.60165(18) 0.1358(4) 0.0583(13) Uani 1 1 d . . . H14 H 0.1749 0.5835 0.0768 0.070 Uiso 1 1 calc R . . C16 C 0.4953(4) 0.36486(17) 0.2876(4) 0.0526(12) Uani 1 1 d . . . H15 H 0.5534 0.3705 0.3459 0.063 Uiso 1 1 calc R . . C17 C 0.4006(4) 0.3369(2) 0.2935(4) 0.0613(14) Uani 1 1 d . . . H16 H 0.3934 0.3239 0.3550 0.074 Uiso 1 1 calc R . . C18 C 0.3181(5) 0.3286(2) 0.2090(4) 0.0606(14) Uani 1 1 d . . . H17 H 0.2525 0.3097 0.2113 0.073 Uiso 1 1 calc R . . C19 C 0.3303(4) 0.34761(18) 0.1212(4) 0.0535(12) Uani 1 1 d . . . H18 H 0.2728 0.3420 0.0624 0.064 Uiso 1 1 calc R . . C20 C 0.4260(4) 0.37493(17) 0.1179(3) 0.0462(11) Uani 1 1 d . . . C21 C 0.4525(4) 0.39621(16) 0.0308(3) 0.0460(11) Uani 1 1 d . . . C22 C 0.3748(4) 0.39179(19) -0.0696(4) 0.0554(13) Uani 1 1 d . . . H19 H 0.3333 0.3611 -0.0746 0.066 Uiso 1 1 calc R . . H20 H 0.4205 0.3929 -0.1196 0.066 Uiso 1 1 calc R . . H21 H 0.3195 0.4184 -0.0804 0.066 Uiso 1 1 calc R . . C23 C 0.6756(4) 0.46854(15) 0.0014(3) 0.0409(10) Uani 1 1 d . . . C24 C 0.8478(4) 0.54407(17) -0.1027(3) 0.0463(11) Uani 1 1 d . . . C25 C 0.9519(4) 0.5728(2) -0.0491(4) 0.0595(14) Uani 1 1 d . . . H22 H 0.9892 0.5561 0.0120 0.071 Uiso 1 1 calc R . . H23 H 0.9272 0.6049 -0.0331 0.071 Uiso 1 1 calc R . . H24 H 1.0064 0.5759 -0.0917 0.071 Uiso 1 1 calc R . . C26 C 0.8150(4) 0.54760(18) -0.2105(4) 0.0476(11) Uani 1 1 d . . . C27 C 0.8789(5) 0.5780(2) -0.2577(4) 0.0649(15) Uani 1 1 d . . . H25 H 0.9424 0.5952 -0.2193 0.078 Uiso 1 1 calc R . . C28 C 0.8509(5) 0.5833(3) -0.3593(4) 0.081(2) Uani 1 1 d . . . H26 H 0.8932 0.6043 -0.3914 0.097 Uiso 1 1 calc R . . C29 C 0.7597(4) 0.5569(2) -0.4122(4) 0.0668(16) Uani 1 1 d . . . H27 H 0.7390 0.5591 -0.4823 0.080 Uiso 1 1 calc R . . C30 C 0.6985(4) 0.52751(16) -0.3637(3) 0.0460(11) Uani 1 1 d . . . H28 H 0.6347 0.5104 -0.4020 0.055 Uiso 1 1 calc R . . C31 C 0.8656(8) 0.2500 0.5203(6) 0.064(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0421(3) 0.0453(3) 0.0289(3) -0.0023(2) 0.0104(2) -0.0023(3) Co2 0.0445(4) 0.0453(4) 0.0276(3) -0.0029(2) 0.0101(2) 0.0003(3) S1 0.0465(6) 0.0503(6) 0.0272(5) -0.0033(4) 0.0097(5) 0.0011(5) S2 0.0442(6) 0.0484(6) 0.0326(6) -0.0016(4) 0.0116(5) -0.0045(5) S3 0.1009(17) 0.0555(12) 0.0653(14) 0.000 0.0187(12) 0.000 F1 0.113(3) 0.075(2) 0.089(3) -0.017(2) 0.016(2) -0.005(2) F2 0.148(6) 0.135(5) 0.085(4) 0.000 0.068(4) 0.000 O1 0.140(6) 0.081(4) 0.096(5) 0.000 0.056(5) 0.000 O2 0.121(4) 0.057(2) 0.100(4) -0.020(2) -0.008(3) -0.009(3) N1 0.053(2) 0.0410(19) 0.041(2) 0.0013(16) 0.0207(18) 0.0035(17) N2 0.041(2) 0.0421(19) 0.039(2) -0.0030(16) 0.0120(16) -0.0033(17) N3 0.042(2) 0.054(2) 0.0293(19) -0.0042(16) 0.0085(15) -0.0067(18) N4 0.046(2) 0.053(2) 0.0307(19) -0.0030(16) 0.0042(16) -0.0001(18) N5 0.043(2) 0.051(2) 0.0328(19) -0.0032(16) 0.0121(16) 0.0024(17) N6 0.052(2) 0.050(2) 0.040(2) -0.0010(17) 0.0151(18) 0.0104(18) N7 0.050(2) 0.044(2) 0.0329(19) -0.0058(15) 0.0148(16) -0.0089(17) N8 0.041(2) 0.047(2) 0.040(2) -0.0014(16) 0.0125(17) 0.0027(17) N9 0.049(2) 0.045(2) 0.035(2) -0.0053(16) 0.0142(16) -0.0013(17) N10 0.049(2) 0.047(2) 0.034(2) -0.0040(16) 0.0130(17) -0.0006(18) N11 0.045(2) 0.049(2) 0.035(2) -0.0050(16) 0.0091(16) -0.0074(17) N12 0.047(2) 0.053(2) 0.032(2) -0.0027(16) 0.0124(16) 0.0027(18) C1 0.059(3) 0.052(3) 0.045(3) -0.007(2) 0.017(2) -0.012(2) C2 0.071(4) 0.046(3) 0.071(4) -0.006(3) 0.041(3) -0.001(3) C3 0.057(3) 0.047(3) 0.084(4) -0.009(3) 0.022(3) 0.004(2) C4 0.044(3) 0.038(2) 0.073(4) 0.011(2) 0.007(2) -0.002(2) C5 0.044(2) 0.041(2) 0.053(3) 0.005(2) 0.014(2) -0.004(2) C6 0.042(2) 0.047(3) 0.045(3) -0.001(2) 0.006(2) -0.009(2) C7 0.054(3) 0.053(3) 0.045(3) 0.009(2) -0.002(2) 0.004(2) C8 0.042(2) 0.048(2) 0.029(2) 0.0006(18) 0.0080(18) -0.007(2) C9 0.052(3) 0.057(3) 0.035(2) -0.009(2) 0.013(2) -0.006(2) C10 0.095(4) 0.063(3) 0.041(3) -0.013(2) 0.010(3) 0.012(3) C11 0.058(3) 0.053(3) 0.039(3) -0.011(2) 0.002(2) 0.009(2) C12 0.116(5) 0.059(3) 0.048(3) -0.009(3) 0.001(3) 0.031(4) C13 0.130(6) 0.074(4) 0.064(4) -0.009(3) 0.016(4) 0.048(4) C14 0.087(4) 0.084(4) 0.051(3) -0.018(3) 0.008(3) 0.029(4) C15 0.070(3) 0.059(3) 0.040(3) -0.011(2) 0.000(2) 0.016(3) C16 0.062(3) 0.060(3) 0.037(3) -0.006(2) 0.014(2) -0.009(2) C17 0.058(3) 0.077(4) 0.054(3) 0.005(3) 0.024(3) -0.017(3) C18 0.059(3) 0.075(4) 0.049(3) 0.000(3) 0.014(2) -0.022(3) C19 0.054(3) 0.058(3) 0.045(3) -0.007(2) 0.007(2) -0.014(2) C20 0.047(3) 0.054(3) 0.038(3) -0.006(2) 0.009(2) -0.006(2) C21 0.056(3) 0.040(2) 0.041(3) -0.0044(19) 0.009(2) -0.001(2) C22 0.056(3) 0.060(3) 0.045(3) 0.000(2) 0.003(2) -0.008(2) C23 0.050(3) 0.042(2) 0.033(2) -0.0029(18) 0.0144(19) 0.009(2) C24 0.049(3) 0.053(3) 0.039(3) -0.003(2) 0.016(2) -0.002(2) C25 0.058(3) 0.082(4) 0.040(3) -0.003(2) 0.015(2) -0.020(3) C26 0.041(2) 0.062(3) 0.041(3) 0.000(2) 0.012(2) -0.005(2) C27 0.061(3) 0.093(4) 0.041(3) 0.001(3) 0.011(2) -0.025(3) C28 0.073(4) 0.125(5) 0.042(3) 0.017(3) 0.007(3) -0.046(4) C29 0.056(3) 0.105(5) 0.036(3) 0.015(3) 0.006(2) -0.009(3) C30 0.047(3) 0.049(3) 0.042(3) -0.005(2) 0.010(2) -0.006(2) C31 0.097(6) 0.051(4) 0.046(4) 0.000 0.020(4) 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 Co1 N8 1.893(4) . ? Co1 N2 1.900(4) . ? Co1 N1 1.938(4) . ? Co1 N7 1.965(4) . ? Co1 S1 2.2006(13) . ? Co1 S2 2.2422(12) . ? Co2 N10 1.889(4) 3_665 ? Co2 N5 1.915(4) . ? Co2 N6 1.941(4) . ? Co2 N12 2.058(4) 3_665 ? Co2 S1 2.2095(13) . ? S1 C8 1.768(4) . ? S2 C23 1.745(5) . ? S3 O2 1.426(4) 4_565 ? S3 O2 1.426(4) . ? S3 O1 1.448(7) . ? S3 C31 1.798(9) . ? F1 C31 1.326(6) . ? F2 C31 1.344(9) . ? N1 C1 1.342(6) . ? N1 C5 1.368(6) . ? N2 C6 1.301(6) . ? N2 N3 1.379(5) . ? N3 C8 1.332(6) . ? N4 C8 1.324(5) . ? N4 N5 1.377(5) . ? N5 C9 1.309(6) . ? N6 C15 1.337(6) . ? N6 C11 1.356(6) . ? N7 C16 1.334(6) . ? N7 C20 1.362(6) . ? N8 C21 1.302(6) . ? N8 N9 1.352(5) . ? N9 C23 1.325(6) . ? N10 C23 1.365(6) . ? N10 N11 1.368(5) . ? N10 Co2 1.889(4) 3_665 ? N11 C24 1.290(6) . ? N12 C30 1.340(6) . ? N12 C26 1.379(6) . ? N12 Co2 2.058(4) 3_665 ? C1 C2 1.367(7) . ? C1 H1 0.9500 . ? C2 C3 1.383(8) . ? C2 H2 0.9500 . ? C3 C4 1.365(7) . ? C3 H3 0.9500 . ? C4 C5 1.387(6) . ? C4 H4 0.9500 . ? C5 C6 1.455(6) . ? C6 C7 1.496(6) . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C7 H7 0.9800 . ? C9 C11 1.452(7) . ? C9 C10 1.476(6) . ? C10 H8 0.9800 . ? C10 H9 0.9800 . ? C10 H10 0.9800 . ? C11 C12 1.390(7) . ? C12 C13 1.385(8) . ? C12 H11 0.9500 . ? C13 C14 1.373(8) . ? C13 H12 0.9500 . ? C14 C15 1.388(7) . ? C14 H13 0.9500 . ? C15 H14 0.9500 . ? C16 C17 1.389(7) . ? C16 H15 0.9500 . ? C17 C18 1.367(7) . ? C17 H16 0.9500 . ? C18 C19 1.369(7) . ? C18 H17 0.9500 . ? C19 C20 1.383(6) . ? C19 H18 0.9500 . ? C20 C21 1.447(6) . ? C21 C22 1.491(6) . ? C22 H19 0.9800 . ? C22 H20 0.9800 . ? C22 H21 0.9800 . ? C24 C26 1.462(6) . ? C24 C25 1.519(6) . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C25 H24 0.9800 . ? C26 C27 1.399(7) . ? C27 C28 1.381(7) . ? C27 H25 0.9500 . ? C28 C29 1.376(8) . ? C28 H26 0.9500 . ? C29 C30 1.373(7) . ? C29 H27 0.9500 . ? C30 H28 0.9500 . ? C31 F1 1.326(6) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Co1 N2 177.06(15) . . ? N8 Co1 N1 99.26(16) . . ? N2 Co1 N1 82.62(16) . . ? N8 Co1 N7 81.86(15) . . ? N2 Co1 N7 95.79(15) . . ? N1 Co1 N7 93.91(15) . . ? N8 Co1 S1 93.65(11) . . ? N2 Co1 S1 84.72(11) . . ? N1 Co1 S1 165.83(12) . . ? N7 Co1 S1 93.67(11) . . ? N8 Co1 S2 86.43(12) . . ? N2 Co1 S2 95.91(11) . . ? N1 Co1 S2 88.02(11) . . ? N7 Co1 S2 168.29(11) . . ? S1 Co1 S2 86.98(5) . . ? N10 Co2 N5 173.27(16) 3_665 . ? N10 Co2 N6 94.70(17) 3_665 . ? N5 Co2 N6 81.66(16) . . ? N10 Co2 N12 91.59(15) 3_665 3_665 ? N5 Co2 N12 94.56(15) . 3_665 ? N6 Co2 N12 99.04(15) . 3_665 ? N10 Co2 S1 99.65(12) 3_665 . ? N5 Co2 S1 80.87(11) . . ? N6 Co2 S1 147.53(13) . . ? N12 Co2 S1 109.44(11) 3_665 . ? C8 S1 Co1 96.23(15) . . ? C8 S1 Co2 95.66(15) . . ? Co1 S1 Co2 145.13(6) . . ? C23 S2 Co1 93.27(16) . . ? O2 S3 O2 120.3(4) 4_565 . ? O2 S3 O1 113.3(3) 4_565 . ? O2 S3 O1 113.3(3) . . ? O2 S3 C31 102.7(3) 4_565 . ? O2 S3 C31 102.7(3) . . ? O1 S3 C31 100.9(4) . . ? C1 N1 C5 117.9(4) . . ? C1 N1 Co1 128.6(3) . . ? C5 N1 Co1 112.7(3) . . ? C6 N2 N3 118.2(4) . . ? C6 N2 Co1 116.8(3) . . ? N3 N2 Co1 124.8(3) . . ? C8 N3 N2 111.3(4) . . ? C8 N4 N5 110.2(3) . . ? C9 N5 N4 118.4(4) . . ? C9 N5 Co2 117.1(3) . . ? N4 N5 Co2 124.3(3) . . ? C15 N6 C11 118.7(4) . . ? C15 N6 Co2 127.3(3) . . ? C11 N6 Co2 113.8(3) . . ? C16 N7 C20 119.6(4) . . ? C16 N7 Co1 127.6(3) . . ? C20 N7 Co1 112.8(3) . . ? C21 N8 N9 119.7(4) . . ? C21 N8 Co1 117.2(3) . . ? N9 N8 Co1 123.0(3) . . ? C23 N9 N8 112.7(4) . . ? C23 N10 N11 112.2(4) . . ? C23 N10 Co2 115.9(3) . 3_665 ? N11 N10 Co2 131.3(3) . 3_665 ? C24 N11 N10 121.0(4) . . ? C30 N12 C26 117.6(4) . . ? C30 N12 Co2 119.3(3) . 3_665 ? C26 N12 Co2 123.0(3) . 3_665 ? N1 C1 C2 123.4(5) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 118.7(5) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 119.0(5) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.2(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 120.7(5) . . ? N1 C5 C6 113.8(4) . . ? C4 C5 C6 125.6(5) . . ? N2 C6 C5 113.7(4) . . ? N2 C6 C7 124.5(4) . . ? C5 C6 C7 121.8(4) . . ? C6 C7 H5 109.5 . . ? C6 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C6 C7 H7 109.5 . . ? H5 C7 H7 109.5 . . ? H6 C7 H7 109.5 . . ? N4 C8 N3 119.2(4) . . ? N4 C8 S1 119.0(3) . . ? N3 C8 S1 121.6(3) . . ? N5 C9 C11 113.2(4) . . ? N5 C9 C10 121.7(4) . . ? C11 C9 C10 125.1(4) . . ? C9 C10 H8 109.5 . . ? C9 C10 H9 109.5 . . ? H8 C10 H9 109.5 . . ? C9 C10 H10 109.5 . . ? H8 C10 H10 109.5 . . ? H9 C10 H10 109.5 . . ? N6 C11 C12 122.1(4) . . ? N6 C11 C9 114.1(4) . . ? C12 C11 C9 123.8(4) . . ? C13 C12 C11 117.5(5) . . ? C13 C12 H11 121.3 . . ? C11 C12 H11 121.3 . . ? C14 C13 C12 121.1(5) . . ? C14 C13 H12 119.4 . . ? C12 C13 H12 119.4 . . ? C13 C14 C15 117.8(5) . . ? C13 C14 H13 121.1 . . ? C15 C14 H13 121.1 . . ? N6 C15 C14 122.7(5) . . ? N6 C15 H14 118.7 . . ? C14 C15 H14 118.7 . . ? N7 C16 C17 121.9(5) . . ? N7 C16 H15 119.1 . . ? C17 C16 H15 119.1 . . ? C18 C17 C16 118.6(5) . . ? C18 C17 H16 120.7 . . ? C16 C17 H16 120.7 . . ? C17 C18 C19 119.8(5) . . ? C17 C18 H17 120.1 . . ? C19 C18 H17 120.1 . . ? C18 C19 C20 120.1(5) . . ? C18 C19 H18 120.0 . . ? C20 C19 H18 120.0 . . ? N7 C20 C19 120.0(4) . . ? N7 C20 C21 113.5(4) . . ? C19 C20 C21 126.5(4) . . ? N8 C21 C20 114.4(4) . . ? N8 C21 C22 122.9(4) . . ? C20 C21 C22 122.7(4) . . ? C21 C22 H19 109.5 . . ? C21 C22 H20 109.5 . . ? H19 C22 H20 109.5 . . ? C21 C22 H21 109.5 . . ? H19 C22 H21 109.5 . . ? H20 C22 H21 109.5 . . ? N9 C23 N10 113.4(4) . . ? N9 C23 S2 124.4(3) . . ? N10 C23 S2 122.1(4) . . ? N11 C24 C26 131.1(4) . . ? N11 C24 C25 111.3(4) . . ? C26 C24 C25 117.5(4) . . ? C24 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C25 H24 109.5 . . ? H22 C25 H24 109.5 . . ? H23 C25 H24 109.5 . . ? N12 C26 C27 120.2(4) . . ? N12 C26 C24 121.4(4) . . ? C27 C26 C24 118.4(4) . . ? C28 C27 C26 121.0(5) . . ? C28 C27 H25 119.5 . . ? C26 C27 H25 119.5 . . ? C29 C28 C27 117.6(5) . . ? C29 C28 H26 121.2 . . ? C27 C28 H26 121.2 . . ? C30 C29 C28 120.0(5) . . ? C30 C29 H27 120.0 . . ? C28 C29 H27 120.0 . . ? N12 C30 C29 123.5(4) . . ? N12 C30 H28 118.2 . . ? C29 C30 H28 118.2 . . ? F1 C31 F1 105.1(7) 4_565 . ? F1 C31 F2 105.1(5) 4_565 . ? F1 C31 F2 105.1(5) . . ? F1 C31 S3 114.3(5) 4_565 . ? F1 C31 S3 114.3(5) . . ? F2 C31 S3 112.0(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.608 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.090 data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 743064' #TrackingRef 'KS_Paper_Submission_CIF_Revised2.cif' # start Validation Reply Form _vrf_LABEL01_Compound3 ; PROBLEM: An _atom_site_label occurs more than once in the atom list. RESPONSE: This refers to F8 and F9, which appear in both PARTs of a disordered triflate. ; _vrf_PLAT431_Compound3 ; PROBLEM: Short Inter HL..A Contact F4 .. F15 .. 1.87 Ang. RESPONSE: F(14-16) and C(66) are part of a disordered triflate anion with occupancy of 0.25. ; _vrf_PLAT432_Compound3 ; PROBLEM: Short Inter X...Y Contact F4 .. C66 .. 2.31 Ang. RESPONSE: F(14-16) and C(66) are part of a disordered triflate anion with occupancy of 0.25. ; _vrf_PLAT070_Compound3 ; PROBLEM: Duplicate Atomic Label on INPUT ................ F8 RESPONSE: This refers to F8 and F9, which appear in both PARTs of a disordered triflate. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C15 H14 N6 O), 4Fe, 4(C F3 S O3), 2(C H3 O H)' _chemical_formula_sum 'C66 H64 F12 Fe4 N24 O18 S4' _chemical_formula_weight 2060.99 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.767(2) _cell_length_b 14.043(3) _cell_length_c 21.488(4) _cell_angle_alpha 89.440(7) _cell_angle_beta 80.884(5) _cell_angle_gamma 89.425(7) _cell_volume 4101.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 15560 _cell_measurement_theta_min 2.8804 _cell_measurement_theta_max 30.8064 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9552 _exptl_absorpt_correction_T_min 0.9006 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite-Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 38297 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 26.50 _reflns_number_total 16776 _reflns_number_gt 13984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One of the triflate anions and both lattice solvent methanol molecules exhibited unsatisfactory anisotropic temperature factors, even with the use of (ISOR) restraints, and was therefore refined isotropically. Two of the other triflate anions were disordered, and refined with PART commands. [S(3), F(7-9), C(63) and O(11-13)] are present at 50% occupancy while [S(4), F(8-10), C(64) and O(14-16)] are also present at 50% occupancy. [S(5), F(11-13), C(65) and O(17-19)] are present at 75% occupancy while [S(6), F(14-16), C(66) and O(20-22)] are present at 25% occupancy. Distance (DFIX) and angle (DANG) restraints were used for both of these disordered triflates in order to achieve reasonable geometric parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1798P)^2^+19.8051P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16776 _refine_ls_number_parameters 1086 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.1310 _refine_ls_R_factor_gt 0.1177 _refine_ls_wR_factor_ref 0.3323 _refine_ls_wR_factor_gt 0.3177 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.48014(7) 0.26067(7) 0.26931(5) 0.0334(3) Uani 1 1 d . . . Fe2 Fe 0.24571(7) 0.39400(7) 0.24447(4) 0.0318(3) Uani 1 1 d . . . Fe3 Fe 0.37059(7) 0.02314(7) 0.22308(5) 0.0327(3) Uani 1 1 d . . . Fe4 Fe 0.12118(7) 0.15211(7) 0.23856(5) 0.0338(3) Uani 1 1 d . . . S1 S 0.78407(15) 0.68197(13) 0.07447(9) 0.0410(4) Uani 1 1 d . . . S2 S 0.3405(4) 0.6672(4) 0.4901(3) 0.1293(16) Uiso 1 1 d D . . S3 S 0.8100(4) 0.1716(5) 0.0763(2) 0.0585(12) Uiso 0.50 1 d PD A 1 C63 C 0.8534(12) 0.2979(11) 0.0613(8) 0.091(8) Uiso 0.50 1 d PD A 1 F7 F 0.7965(11) 0.3359(11) 0.1217(7) 0.094(4) Uiso 0.50 1 d PD A 1 F8 F 0.8212(12) 0.3286(11) 0.0218(7) 0.095(5) Uiso 0.50 1 d PD A 1 F9 F 0.9306(11) 0.3019(12) 0.0665(8) 0.089(5) Uiso 0.50 1 d PD A 1 O11 O 0.8527(11) 0.1322(10) 0.0158(6) 0.073(4) Uiso 0.50 1 d PD A 1 O12 O 0.7067(10) 0.1688(13) 0.0839(9) 0.094(5) Uiso 0.50 1 d PD A 1 O13 O 0.8556(9) 0.1343(8) 0.1237(5) 0.051(3) Uiso 0.50 1 d PD A 1 S4 S 0.7839(4) 0.2112(4) 0.0736(3) 0.0611(12) Uiso 0.50 1 d PD B 2 C64 C 0.8807(8) 0.2628(7) 0.0273(5) 0.045(3) Uiso 0.50 1 d PD B 2 F8 F 0.8525(7) 0.3513(6) -0.0003(5) 0.048(2) Uiso 0.50 1 d PD B 2 F9 F 0.9632(8) 0.2903(8) 0.0569(5) 0.048(3) Uiso 0.50 1 d PD B 2 F10 F 0.9258(7) 0.2099(7) -0.0266(5) 0.058(2) Uiso 0.50 1 d PD B 2 O14 O 0.7593(9) 0.2738(9) 0.1256(5) 0.054(3) Uiso 0.50 1 d PD B 2 O15 O 0.7082(11) 0.2088(12) 0.0353(7) 0.083(4) Uiso 0.50 1 d PD B 2 O16 O 0.8157(12) 0.1215(10) 0.0844(8) 0.078(4) Uiso 0.50 1 d PD B 2 S5 S 0.2132(3) 0.1517(3) 0.55972(18) 0.0675(9) Uiso 0.75 1 d PD C 3 C65 C 0.2182(10) 0.2733(9) 0.5797(6) 0.076(4) Uiso 0.75 1 d PD C 3 F11 F 0.2136(8) 0.2820(8) 0.6446(5) 0.102(3) Uiso 0.75 1 d PD C 3 F12 F 0.3048(7) 0.3130(7) 0.5515(5) 0.091(3) Uiso 0.75 1 d PD C 3 F13 F 0.1379(8) 0.3256(8) 0.5622(6) 0.104(3) Uiso 0.75 1 d PD C 3 O17 O 0.2235(7) 0.1593(7) 0.4928(4) 0.066(2) Uiso 0.75 1 d PD C 3 O18 O 0.1180(7) 0.1235(8) 0.5904(5) 0.081(3) Uiso 0.75 1 d PD C 3 O19 O 0.2947(7) 0.1153(7) 0.5837(5) 0.078(3) Uiso 0.75 1 d PD C 3 S6 S 0.2508(7) 0.2445(6) 0.5827(4) 0.0471(18) Uiso 0.25 1 d PD D 4 C66 C 0.2275(17) 0.3615(12) 0.5630(11) 0.061(9) Uiso 0.25 1 d PD D 4 F14 F 0.308(2) 0.389(2) 0.5180(14) 0.116(11) Uiso 0.25 1 d PD D 4 F15 F 0.221(2) 0.4286(17) 0.6098(12) 0.094(8) Uiso 0.25 1 d PD D 4 F16 F 0.1439(16) 0.3701(19) 0.5361(13) 0.081(7) Uiso 0.25 1 d PD D 4 O20 O 0.3398(17) 0.251(2) 0.6048(15) 0.090(10) Uiso 0.25 1 d PD D 4 O21 O 0.175(3) 0.209(3) 0.6269(18) 0.17(2) Uiso 0.25 1 d PD D 4 O22 O 0.2562(19) 0.2019(16) 0.5219(9) 0.059(6) Uiso 0.25 1 d PD D 4 F1 F 0.8445(6) 0.5083(5) 0.0819(3) 0.093(2) Uani 1 1 d . . . F2 F 0.9590(5) 0.6078(7) 0.0500(3) 0.100(3) Uani 1 1 d . . . F3 F 0.8636(6) 0.5649(6) -0.0136(3) 0.100(3) Uani 1 1 d . . . F4 F 0.2386(10) 0.5241(10) 0.5481(6) 0.174(5) Uiso 1 1 d D . . F5 F 0.2923(14) 0.5149(13) 0.4348(8) 0.244(8) Uiso 1 1 d D . . F6 F 0.3959(16) 0.5114(17) 0.5023(12) 0.326(12) Uiso 1 1 d D . . O1 O 0.3395(3) 0.3185(4) 0.2981(2) 0.0341(10) Uani 1 1 d . . . O2 O 0.2442(4) 0.0827(4) 0.2684(2) 0.0367(11) Uani 1 1 d . . . O3 O 0.4337(4) 0.1535(3) 0.2105(2) 0.0346(10) Uani 1 1 d . . . O4 O 0.2019(4) 0.2710(3) 0.1991(2) 0.0353(10) Uani 1 1 d . . . O5 O 0.6886(5) 0.6448(5) 0.0687(3) 0.0629(17) Uani 1 1 d . . . O6 O 0.8028(5) 0.6932(4) 0.1376(3) 0.0518(14) Uani 1 1 d . . . O7 O 0.8123(5) 0.7609(4) 0.0332(3) 0.0555(15) Uani 1 1 d . . . O8 O 0.2574(6) 0.7004(6) 0.4683(4) 0.088(2) Uiso 1 1 d D . . O9 O 0.3612(12) 0.6885(12) 0.5511(5) 0.177(6) Uiso 1 1 d D . . O10 O 0.4185(9) 0.6713(11) 0.4406(6) 0.160(5) Uiso 1 1 d D . . O23 O 0.4667(5) 0.3013(4) 0.0026(3) 0.0541(14) Uiso 1 1 d . . . O24 O 0.1723(18) 0.7046(17) 0.3670(12) 0.122(7) Uiso 0.50 1 d P . . O25 O 0.1999(18) 0.9532(17) 0.4976(12) 0.125(7) Uiso 0.50 1 d P . . N1 N 0.6004(4) 0.1750(4) 0.2919(3) 0.0368(13) Uani 1 1 d . . . N2 N 0.4413(4) 0.2225(4) 0.3644(3) 0.0362(13) Uani 1 1 d . . . N3 N 0.3529(4) 0.2565(5) 0.3951(3) 0.0396(14) Uani 1 1 d . . . N4 N 0.2164(5) 0.3448(5) 0.3835(3) 0.0390(14) Uani 1 1 d . . . N5 N 0.1749(4) 0.3947(4) 0.3388(3) 0.0364(13) Uani 1 1 d . . . N6 N 0.1110(4) 0.4775(4) 0.2443(3) 0.0370(13) Uani 1 1 d . . . N7 N 0.5000(4) -0.0406(4) 0.2104(3) 0.0359(13) Uani 1 1 d . . . N8 N 0.3811(4) -0.0065(4) 0.3080(3) 0.0355(13) Uani 1 1 d . . . N9 N 0.3056(5) 0.0218(5) 0.3555(3) 0.0423(15) Uani 1 1 d . . . N10 N 0.1604(5) 0.1040(5) 0.3687(3) 0.0497(17) Uani 1 1 d . . . N11 N 0.0941(5) 0.1508(5) 0.3389(3) 0.0419(14) Uani 1 1 d . . . N12 N -0.0144(5) 0.2345(4) 0.2676(3) 0.0406(14) Uani 1 1 d . . . N13 N 0.5558(4) 0.3937(4) 0.2769(3) 0.0374(13) Uani 1 1 d . . . N14 N 0.5185(4) 0.3121(4) 0.1772(3) 0.0341(12) Uani 1 1 d . . . N15 N 0.4868(5) 0.2596(4) 0.1303(3) 0.0390(14) Uani 1 1 d . . . N16 N 0.4075(5) 0.1266(4) 0.1076(3) 0.0394(14) Uani 1 1 d . . . N17 N 0.3645(4) 0.0458(4) 0.1366(3) 0.0369(13) Uani 1 1 d . . . N18 N 0.3000(4) -0.0913(4) 0.2042(3) 0.0410(14) Uani 1 1 d . . . N19 N 0.3311(4) 0.5245(4) 0.2363(3) 0.0337(12) Uani 1 1 d . . . N20 N 0.2943(4) 0.4123(4) 0.1470(3) 0.0339(12) Uani 1 1 d . . . N21 N 0.2631(5) 0.3515(4) 0.1052(3) 0.0357(13) Uani 1 1 d . . . N22 N 0.1738(5) 0.2152(4) 0.1039(3) 0.0376(13) Uani 1 1 d . . . N23 N 0.1262(4) 0.1431(4) 0.1390(3) 0.0334(12) Uani 1 1 d . . . N24 N 0.0401(4) 0.0241(4) 0.2227(3) 0.0357(13) Uani 1 1 d . . . C1 C 0.6782(6) 0.1480(6) 0.2505(4) 0.0423(17) Uani 1 1 d . . . H1 H 0.6821 0.1674 0.2077 0.051 Uiso 1 1 calc R . . C2 C 0.7532(6) 0.0927(6) 0.2676(4) 0.0481(19) Uani 1 1 d . . . H2 H 0.8088 0.0758 0.2375 0.058 Uiso 1 1 calc R . . C3 C 0.7460(6) 0.0629(7) 0.3288(4) 0.053(2) Uani 1 1 d . . . H3 H 0.7961 0.0238 0.3416 0.064 Uiso 1 1 calc R . . C4 C 0.6643(6) 0.0902(6) 0.3729(4) 0.0489(19) Uani 1 1 d . . . H4 H 0.6589 0.0713 0.4158 0.059 Uiso 1 1 calc R . . C5 C 0.5923(6) 0.1447(5) 0.3524(4) 0.0403(16) Uani 1 1 d . . . C6 C 0.5019(6) 0.1741(5) 0.3937(3) 0.0394(16) Uani 1 1 d . . . C7 C 0.4804(7) 0.1474(7) 0.4623(4) 0.060(3) Uani 1 1 d . . . H5 H 0.5035 0.1978 0.4874 0.072 Uiso 1 1 calc R . . H6 H 0.5143 0.0875 0.4693 0.072 Uiso 1 1 calc R . . H7 H 0.4093 0.1394 0.4748 0.072 Uiso 1 1 calc R . . C8 C 0.3001(5) 0.3083(5) 0.3567(3) 0.0340(14) Uani 1 1 d . . . C9 C 0.0972(6) 0.4458(6) 0.3553(4) 0.0429(17) Uani 1 1 d . . . C10 C 0.0479(7) 0.4612(8) 0.4217(4) 0.061(2) Uani 1 1 d . . . H8 H -0.0022 0.4123 0.4334 0.073 Uiso 1 1 calc R . . H9 H 0.0166 0.5243 0.4251 0.073 Uiso 1 1 calc R . . H10 H 0.0969 0.4570 0.4501 0.073 Uiso 1 1 calc R . . C11 C 0.0597(6) 0.4940(6) 0.3022(4) 0.0429(17) Uani 1 1 d . . . C12 C -0.0246(7) 0.5509(7) 0.3108(5) 0.062(3) Uani 1 1 d . . . H11 H -0.0597 0.5620 0.3519 0.075 Uiso 1 1 calc R . . C13 C -0.0566(7) 0.5913(7) 0.2581(5) 0.059(2) Uani 1 1 d . . . H12 H -0.1131 0.6317 0.2630 0.071 Uiso 1 1 calc R . . C14 C -0.0066(6) 0.5728(6) 0.1995(5) 0.051(2) Uani 1 1 d . . . H13 H -0.0291 0.5980 0.1631 0.062 Uiso 1 1 calc R . . C15 C 0.0774(6) 0.5166(6) 0.1939(4) 0.0438(17) Uani 1 1 d . . . H14 H 0.1130 0.5050 0.1530 0.053 Uiso 1 1 calc R . . C16 C 0.5638(6) -0.0511(6) 0.1570(4) 0.0443(18) Uani 1 1 d . . . H15 H 0.5472 -0.0248 0.1191 0.053 Uiso 1 1 calc R . . C17 C 0.6523(6) -0.0983(7) 0.1546(5) 0.054(2) Uani 1 1 d . . . H16 H 0.6955 -0.1050 0.1157 0.065 Uiso 1 1 calc R . . C18 C 0.6771(6) -0.1356(7) 0.2093(5) 0.058(2) Uani 1 1 d . . . H17 H 0.7378 -0.1686 0.2088 0.070 Uiso 1 1 calc R . . C19 C 0.6133(6) -0.1247(6) 0.2647(4) 0.0486(19) Uani 1 1 d . . . H18 H 0.6297 -0.1502 0.3029 0.058 Uiso 1 1 calc R . . C20 C 0.5262(5) -0.0772(5) 0.2650(4) 0.0393(16) Uani 1 1 d . . . C21 C 0.4540(5) -0.0578(5) 0.3218(3) 0.0383(15) Uani 1 1 d . . . C22 C 0.4655(6) -0.0926(6) 0.3856(4) 0.0485(19) Uani 1 1 d . . . H19 H 0.5009 -0.0452 0.4064 0.058 Uiso 1 1 calc R . . H20 H 0.5028 -0.1526 0.3821 0.058 Uiso 1 1 calc R . . H21 H 0.4004 -0.1030 0.4106 0.058 Uiso 1 1 calc R . . C23 C 0.2394(6) 0.0686(5) 0.3290(3) 0.0382(15) Uani 1 1 d . . . C24 C 0.0188(6) 0.1922(6) 0.3710(4) 0.051(2) Uani 1 1 d . . . C25 C -0.0001(10) 0.1910(12) 0.4401(5) 0.102(5) Uani 1 1 d . . . H22 H -0.0404 0.1358 0.4550 0.123 Uiso 1 1 calc R . . H23 H -0.0351 0.2495 0.4552 0.123 Uiso 1 1 calc R . . H24 H 0.0625 0.1871 0.4562 0.123 Uiso 1 1 calc R . . C26 C -0.0443(6) 0.2409(6) 0.3304(4) 0.0474(19) Uani 1 1 d . . . C27 C -0.1288(7) 0.2893(8) 0.3549(5) 0.066(3) Uani 1 1 d . . . H25 H -0.1519 0.2894 0.3990 0.079 Uiso 1 1 calc R . . C28 C -0.1796(7) 0.3382(7) 0.3129(6) 0.069(3) Uani 1 1 d . . . H26 H -0.2375 0.3732 0.3287 0.083 Uiso 1 1 calc R . . C29 C -0.1475(7) 0.3365(7) 0.2495(5) 0.062(3) Uani 1 1 d . . . H27 H -0.1807 0.3716 0.2211 0.074 Uiso 1 1 calc R . . C30 C -0.0650(6) 0.2819(6) 0.2280(4) 0.0490(19) Uani 1 1 d . . . H28 H -0.0432 0.2778 0.1839 0.059 Uiso 1 1 calc R . . C31 C 0.5675(6) 0.4382(6) 0.3301(4) 0.0465(18) Uani 1 1 d . . . H29 H 0.5421 0.4091 0.3694 0.056 Uiso 1 1 calc R . . C32 C 0.6155(7) 0.5259(6) 0.3305(4) 0.054(2) Uani 1 1 d . . . H30 H 0.6216 0.5560 0.3690 0.065 Uiso 1 1 calc R . . C33 C 0.6534(6) 0.5670(6) 0.2739(4) 0.0496(19) Uani 1 1 d . . . H31 H 0.6880 0.6254 0.2727 0.060 Uiso 1 1 calc R . . C34 C 0.6407(6) 0.5223(6) 0.2182(4) 0.0457(18) Uani 1 1 d . . . H32 H 0.6666 0.5500 0.1786 0.055 Uiso 1 1 calc R . . C35 C 0.5901(5) 0.4377(5) 0.2209(3) 0.0386(16) Uani 1 1 d . . . C36 C 0.5667(5) 0.3888(5) 0.1638(3) 0.0362(15) Uani 1 1 d . . . C37 C 0.5959(6) 0.4283(6) 0.0994(4) 0.0469(18) Uani 1 1 d . . . H33 H 0.6604 0.4025 0.0812 0.056 Uiso 1 1 calc R . . H34 H 0.5996 0.4979 0.1015 0.056 Uiso 1 1 calc R . . H35 H 0.5471 0.4108 0.0730 0.056 Uiso 1 1 calc R . . C38 C 0.4397(5) 0.1763(5) 0.1510(3) 0.0376(15) Uani 1 1 d . . . C39 C 0.3281(6) -0.0183(6) 0.1032(4) 0.0438(17) Uani 1 1 d . . . C40 C 0.3305(8) -0.0086(7) 0.0338(5) 0.061(2) Uani 1 1 d . . . H36 H 0.2709 0.0247 0.0255 0.073 Uiso 1 1 calc R . . H37 H 0.3338 -0.0719 0.0148 0.073 Uiso 1 1 calc R . . H38 H 0.3885 0.0280 0.0154 0.073 Uiso 1 1 calc R . . C41 C 0.2871(6) -0.0972(6) 0.1427(4) 0.0453(18) Uani 1 1 d . . . C42 C 0.2366(6) -0.1732(6) 0.1220(5) 0.054(2) Uani 1 1 d . . . H39 H 0.2293 -0.1772 0.0789 0.065 Uiso 1 1 calc R . . C43 C 0.1974(7) -0.2420(7) 0.1638(6) 0.067(3) Uani 1 1 d . . . H40 H 0.1635 -0.2944 0.1499 0.080 Uiso 1 1 calc R . . C44 C 0.2079(7) -0.2340(7) 0.2261(6) 0.061(2) Uani 1 1 d . . . H41 H 0.1796 -0.2799 0.2562 0.073 Uiso 1 1 calc R . . C45 C 0.2594(6) -0.1594(6) 0.2443(5) 0.052(2) Uani 1 1 d . . . H42 H 0.2670 -0.1554 0.2874 0.062 Uiso 1 1 calc R . . C46 C 0.3576(5) 0.5746(5) 0.2831(3) 0.0374(15) Uani 1 1 d . . . H43 H 0.3345 0.5553 0.3253 0.045 Uiso 1 1 calc R . . C47 C 0.4176(6) 0.6540(6) 0.2727(4) 0.0434(17) Uani 1 1 d . . . H44 H 0.4333 0.6892 0.3073 0.052 Uiso 1 1 calc R . . C48 C 0.4541(6) 0.6811(6) 0.2119(4) 0.0430(17) Uani 1 1 d . . . H45 H 0.4969 0.7340 0.2037 0.052 Uiso 1 1 calc R . . C49 C 0.4267(6) 0.6292(5) 0.1622(4) 0.0399(16) Uani 1 1 d . . . H46 H 0.4494 0.6471 0.1197 0.048 Uiso 1 1 calc R . . C50 C 0.3665(5) 0.5519(5) 0.1759(3) 0.0351(14) Uani 1 1 d . . . C51 C 0.3383(5) 0.4916(5) 0.1255(3) 0.0368(15) Uani 1 1 d . . . C52 C 0.3537(6) 0.5212(6) 0.0590(4) 0.0443(18) Uani 1 1 d . . . H47 H 0.4171 0.4964 0.0380 0.053 Uiso 1 1 calc R . . H48 H 0.3533 0.5908 0.0562 0.053 Uiso 1 1 calc R . . H49 H 0.3008 0.4959 0.0385 0.053 Uiso 1 1 calc R . . C53 C 0.2155(5) 0.2815(5) 0.1376(3) 0.0325(14) Uani 1 1 d . . . C54 C 0.0814(5) 0.0765(5) 0.1142(4) 0.0371(15) Uani 1 1 d . . . C55 C 0.0742(7) 0.0659(7) 0.0465(4) 0.051(2) Uani 1 1 d . . . H50 H 0.0153 0.0994 0.0372 0.062 Uiso 1 1 calc R . . H51 H 0.0699 -0.0018 0.0367 0.062 Uiso 1 1 calc R . . H52 H 0.1327 0.0930 0.0208 0.062 Uiso 1 1 calc R . . C56 C 0.0338(5) 0.0054(5) 0.1616(4) 0.0380(16) Uani 1 1 d . . . C57 C -0.0139(5) -0.0743(5) 0.1440(4) 0.0416(17) Uani 1 1 d . . . H53 H -0.0191 -0.0851 0.1011 0.050 Uiso 1 1 calc R . . C58 C -0.0537(6) -0.1381(6) 0.1909(4) 0.0471(19) Uani 1 1 d . . . H54 H -0.0850 -0.1943 0.1802 0.056 Uiso 1 1 calc R . . C59 C -0.0474(6) -0.1192(6) 0.2519(4) 0.0495(19) Uani 1 1 d . . . H55 H -0.0755 -0.1614 0.2846 0.059 Uiso 1 1 calc R . . C60 C 0.0005(6) -0.0377(5) 0.2661(4) 0.0440(17) Uani 1 1 d . . . H56 H 0.0051 -0.0256 0.3089 0.053 Uiso 1 1 calc R . . C61 C 0.8676(8) 0.5860(8) 0.0459(4) 0.065(3) Uani 1 1 d . . . C62 C 0.3021(16) 0.5487(12) 0.4940(10) 0.200(11) Uiso 1 1 d D . . C67 C 0.4902(9) 0.2186(9) -0.0303(6) 0.079(3) Uiso 1 1 d . . . H57 H 0.5129 0.1704 -0.0024 0.095 Uiso 1 1 calc R . . H58 H 0.5425 0.2311 -0.0659 0.095 Uiso 1 1 calc R . . H59 H 0.4319 0.1952 -0.0461 0.095 Uiso 1 1 calc R . . C68 C 0.0853(17) 0.7608(17) 0.3830(11) 0.073(6) Uiso 0.50 1 d P . . H60 H 0.0840 0.8114 0.3514 0.088 Uiso 0.50 1 calc PR . . H61 H 0.0847 0.7892 0.4245 0.088 Uiso 0.50 1 calc PR . . H62 H 0.0274 0.7204 0.3840 0.088 Uiso 0.50 1 calc PR . . C69 C 0.1148(16) 1.0015(16) 0.4785(11) 0.068(5) Uiso 0.50 1 d P . . H63 H 0.1363 1.0410 0.4411 0.082 Uiso 0.50 1 calc PR . . H64 H 0.0830 1.0419 0.5129 0.082 Uiso 0.50 1 calc PR . . H65 H 0.0679 0.9541 0.4686 0.082 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0321(5) 0.0388(6) 0.0293(5) 0.0013(4) -0.0047(4) 0.0017(4) Fe2 0.0356(5) 0.0330(5) 0.0275(5) -0.0008(4) -0.0074(4) 0.0020(4) Fe3 0.0332(5) 0.0330(5) 0.0312(5) 0.0002(4) -0.0030(4) 0.0029(4) Fe4 0.0346(5) 0.0342(5) 0.0333(5) 0.0004(4) -0.0081(4) 0.0016(4) S1 0.0481(11) 0.0386(9) 0.0366(9) -0.0021(7) -0.0069(8) -0.0045(8) F1 0.140(7) 0.058(4) 0.088(5) -0.011(3) -0.043(5) 0.033(4) F2 0.058(4) 0.188(8) 0.053(4) -0.002(4) -0.011(3) 0.035(4) F3 0.131(6) 0.117(6) 0.059(4) -0.035(4) -0.037(4) 0.070(5) O1 0.034(3) 0.044(3) 0.024(2) 0.0028(19) -0.0044(18) 0.006(2) O2 0.035(3) 0.039(3) 0.035(3) 0.001(2) -0.002(2) 0.004(2) O3 0.036(3) 0.038(3) 0.029(2) -0.0002(19) -0.0018(19) 0.000(2) O4 0.044(3) 0.032(2) 0.032(2) 0.0022(19) -0.010(2) -0.001(2) O5 0.054(4) 0.067(4) 0.071(4) 0.009(3) -0.020(3) -0.013(3) O6 0.063(4) 0.057(3) 0.035(3) -0.005(2) -0.007(3) -0.001(3) O7 0.072(4) 0.052(3) 0.044(3) 0.000(3) -0.013(3) -0.013(3) N1 0.036(3) 0.036(3) 0.038(3) -0.004(2) -0.007(2) 0.002(2) N2 0.033(3) 0.043(3) 0.032(3) 0.004(2) -0.007(2) 0.005(2) N3 0.035(3) 0.051(4) 0.032(3) 0.001(3) -0.005(2) 0.014(3) N4 0.040(3) 0.050(4) 0.027(3) -0.002(3) -0.007(2) 0.013(3) N5 0.037(3) 0.041(3) 0.032(3) -0.003(2) -0.007(2) 0.007(2) N6 0.037(3) 0.037(3) 0.040(3) -0.001(2) -0.014(3) 0.002(2) N7 0.033(3) 0.038(3) 0.035(3) -0.004(2) 0.000(2) -0.001(2) N8 0.032(3) 0.034(3) 0.040(3) 0.003(2) -0.006(2) 0.003(2) N9 0.042(3) 0.050(4) 0.033(3) 0.003(3) 0.000(3) 0.014(3) N10 0.049(4) 0.065(4) 0.033(3) 0.006(3) -0.003(3) 0.023(3) N11 0.035(3) 0.044(3) 0.047(4) 0.002(3) -0.006(3) 0.012(3) N12 0.036(3) 0.038(3) 0.051(4) 0.001(3) -0.014(3) 0.003(3) N13 0.036(3) 0.042(3) 0.036(3) 0.002(3) -0.013(2) 0.004(3) N14 0.034(3) 0.035(3) 0.032(3) -0.001(2) -0.003(2) -0.001(2) N15 0.049(4) 0.038(3) 0.030(3) -0.004(2) -0.007(3) -0.007(3) N16 0.046(4) 0.041(3) 0.033(3) 0.000(2) -0.012(3) -0.001(3) N17 0.032(3) 0.037(3) 0.042(3) -0.001(2) -0.005(2) 0.000(2) N18 0.031(3) 0.038(3) 0.052(4) 0.004(3) -0.001(3) 0.006(2) N19 0.033(3) 0.035(3) 0.034(3) -0.003(2) -0.010(2) 0.003(2) N20 0.037(3) 0.031(3) 0.034(3) 0.001(2) -0.009(2) -0.001(2) N21 0.042(3) 0.034(3) 0.032(3) -0.004(2) -0.008(2) -0.005(2) N22 0.043(3) 0.040(3) 0.033(3) 0.000(2) -0.014(3) -0.005(3) N23 0.032(3) 0.034(3) 0.034(3) -0.002(2) -0.005(2) -0.003(2) N24 0.035(3) 0.033(3) 0.039(3) 0.000(2) -0.006(2) 0.001(2) C1 0.036(4) 0.049(4) 0.041(4) 0.002(3) -0.003(3) 0.001(3) C2 0.041(4) 0.050(5) 0.052(5) -0.009(4) -0.006(3) 0.008(3) C3 0.040(4) 0.062(5) 0.058(5) 0.004(4) -0.009(4) 0.012(4) C4 0.048(5) 0.062(5) 0.036(4) 0.003(4) -0.005(3) 0.014(4) C5 0.044(4) 0.042(4) 0.037(4) -0.002(3) -0.011(3) 0.006(3) C6 0.042(4) 0.042(4) 0.034(4) 0.003(3) -0.007(3) 0.009(3) C7 0.064(6) 0.078(6) 0.037(4) 0.005(4) -0.006(4) 0.033(5) C8 0.035(4) 0.037(4) 0.031(3) -0.001(3) -0.007(3) 0.006(3) C9 0.038(4) 0.051(4) 0.040(4) -0.006(3) -0.008(3) 0.011(3) C10 0.061(6) 0.082(7) 0.039(4) -0.009(4) -0.007(4) 0.029(5) C11 0.039(4) 0.047(4) 0.044(4) -0.006(3) -0.012(3) 0.007(3) C12 0.050(5) 0.074(6) 0.062(6) -0.008(5) -0.008(4) 0.034(5) C13 0.051(5) 0.068(6) 0.061(6) -0.007(5) -0.015(4) 0.023(4) C14 0.048(5) 0.049(5) 0.061(5) 0.005(4) -0.024(4) 0.005(4) C15 0.044(4) 0.042(4) 0.048(4) 0.002(3) -0.018(3) 0.003(3) C16 0.036(4) 0.043(4) 0.053(5) -0.014(3) -0.005(3) 0.001(3) C17 0.041(4) 0.063(5) 0.056(5) -0.020(4) 0.001(4) 0.007(4) C18 0.030(4) 0.066(6) 0.079(7) -0.033(5) -0.009(4) 0.010(4) C19 0.036(4) 0.050(5) 0.062(5) -0.009(4) -0.014(4) -0.001(3) C20 0.035(4) 0.033(4) 0.050(4) -0.005(3) -0.007(3) -0.002(3) C21 0.038(4) 0.040(4) 0.038(4) 0.001(3) -0.010(3) 0.004(3) C22 0.042(4) 0.056(5) 0.049(5) 0.005(4) -0.013(3) 0.007(4) C23 0.042(4) 0.041(4) 0.029(3) -0.003(3) -0.002(3) 0.005(3) C24 0.050(5) 0.056(5) 0.043(4) -0.003(4) 0.000(4) 0.014(4) C25 0.087(9) 0.161(14) 0.050(6) 0.007(7) 0.012(6) 0.071(9) C26 0.046(4) 0.039(4) 0.058(5) -0.010(4) -0.011(4) 0.008(3) C27 0.053(5) 0.079(7) 0.065(6) -0.025(5) -0.010(4) 0.026(5) C28 0.051(5) 0.066(6) 0.095(8) -0.026(6) -0.029(5) 0.029(5) C29 0.061(6) 0.051(5) 0.082(7) -0.010(5) -0.036(5) 0.014(4) C30 0.043(4) 0.048(5) 0.060(5) -0.006(4) -0.021(4) 0.006(3) C31 0.054(5) 0.049(5) 0.040(4) 0.004(3) -0.019(3) 0.007(4) C32 0.070(6) 0.047(5) 0.048(5) -0.010(4) -0.019(4) 0.010(4) C33 0.050(5) 0.042(4) 0.061(5) 0.001(4) -0.019(4) -0.001(3) C34 0.045(4) 0.041(4) 0.052(5) 0.000(3) -0.010(3) -0.002(3) C35 0.033(4) 0.045(4) 0.036(4) -0.002(3) -0.002(3) 0.003(3) C36 0.033(4) 0.042(4) 0.033(3) 0.001(3) -0.003(3) 0.001(3) C37 0.053(5) 0.048(4) 0.039(4) 0.008(3) -0.006(3) -0.006(4) C38 0.036(4) 0.041(4) 0.036(4) -0.005(3) -0.006(3) 0.001(3) C39 0.038(4) 0.039(4) 0.056(5) -0.009(3) -0.013(3) -0.001(3) C40 0.072(6) 0.055(5) 0.061(6) -0.005(4) -0.024(5) -0.012(5) C41 0.036(4) 0.038(4) 0.062(5) -0.002(3) -0.007(3) 0.004(3) C42 0.047(5) 0.039(4) 0.078(6) -0.013(4) -0.012(4) 0.000(4) C43 0.043(5) 0.039(5) 0.118(10) 0.000(5) -0.012(5) -0.002(4) C44 0.045(5) 0.046(5) 0.089(7) 0.005(5) -0.002(5) 0.001(4) C45 0.040(4) 0.041(4) 0.069(6) 0.011(4) 0.009(4) 0.007(3) C46 0.043(4) 0.039(4) 0.031(3) -0.004(3) -0.008(3) 0.004(3) C47 0.046(4) 0.042(4) 0.046(4) -0.013(3) -0.019(3) -0.001(3) C48 0.046(4) 0.038(4) 0.047(4) -0.006(3) -0.012(3) -0.005(3) C49 0.043(4) 0.044(4) 0.035(4) 0.001(3) -0.012(3) -0.002(3) C50 0.039(4) 0.029(3) 0.038(4) 0.001(3) -0.009(3) 0.002(3) C51 0.037(4) 0.034(4) 0.040(4) 0.002(3) -0.009(3) -0.004(3) C52 0.054(5) 0.043(4) 0.038(4) 0.003(3) -0.014(3) -0.011(3) C53 0.038(4) 0.028(3) 0.033(3) -0.003(3) -0.010(3) -0.001(3) C54 0.032(4) 0.038(4) 0.042(4) -0.009(3) -0.010(3) 0.001(3) C55 0.058(5) 0.059(5) 0.039(4) -0.006(4) -0.013(4) -0.010(4) C56 0.025(3) 0.036(4) 0.053(4) -0.001(3) -0.008(3) 0.005(3) C57 0.032(4) 0.041(4) 0.054(5) -0.009(3) -0.013(3) 0.000(3) C58 0.037(4) 0.035(4) 0.068(5) -0.002(4) -0.004(4) 0.002(3) C59 0.047(5) 0.040(4) 0.060(5) 0.007(4) -0.006(4) 0.001(3) C60 0.041(4) 0.039(4) 0.051(5) 0.004(3) -0.005(3) 0.006(3) C61 0.079(7) 0.077(7) 0.041(5) -0.018(5) -0.018(4) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N14 2.090(6) . ? Fe1 N2 2.095(6) . ? Fe1 O1 2.096(5) . ? Fe1 O3 2.141(5) . ? Fe1 N1 2.151(6) . ? Fe1 N13 2.168(6) . ? Fe2 N5 2.105(6) . ? Fe2 N20 2.109(6) . ? Fe2 O1 2.129(5) . ? Fe2 O4 2.130(5) . ? Fe2 N19 2.178(6) . ? Fe2 N6 2.184(6) . ? Fe3 N8 1.895(6) . ? Fe3 N17 1.897(6) . ? Fe3 N18 1.965(7) . ? Fe3 N7 1.967(6) . ? Fe3 O3 2.031(5) . ? Fe3 O2 2.031(5) . ? Fe4 O4 2.110(5) . ? Fe4 O2 2.127(5) . ? Fe4 N11 2.128(7) . ? Fe4 N23 2.134(6) . ? Fe4 N24 2.183(6) . ? Fe4 N12 2.194(6) . ? S1 O7 1.430(6) . ? S1 O6 1.431(6) . ? S1 O5 1.443(7) . ? S1 C61 1.811(11) . ? S2 O8 1.378(7) . ? S2 O10 1.387(9) . ? S2 O9 1.421(9) . ? S2 C62 1.749(15) . ? S3 O13 1.374(11) . ? S3 O12 1.407(13) . ? S3 O11 1.451(12) . ? S3 C63 1.886(15) . ? C63 F9 1.50(2) . ? C63 F8 1.517(19) . ? C63 F7 1.506(17) . ? S4 O16 1.359(13) . ? S4 O14 1.425(11) . ? S4 O15 1.427(13) . ? S4 C64 1.696(11) . ? C64 F10 1.434(9) . ? C64 F9 1.444(9) . ? C64 F8 1.448(9) . ? S5 O19 1.397(10) . ? S5 O17 1.426(9) . ? S5 O18 1.429(10) . ? S5 C65 1.769(12) . ? C65 F12 1.369(13) . ? C65 F11 1.393(14) . ? C65 F13 1.419(14) . ? S6 O20 1.385(17) . ? S6 O21 1.386(18) . ? S6 O22 1.434(16) . ? S6 C66 1.733(16) . ? C66 F16 1.371(18) . ? C66 F15 1.378(18) . ? C66 F14 1.406(19) . ? F1 C61 1.342(13) . ? F2 C61 1.316(13) . ? F3 C61 1.324(10) . ? F4 C62 1.384(16) . ? F5 C62 1.387(16) . ? F6 C62 1.426(18) . ? O1 C8 1.297(8) . ? O2 C23 1.308(9) . ? O3 C38 1.306(9) . ? O4 C53 1.312(8) . ? O23 C67 1.376(13) . ? O24 C68 1.43(3) . ? O25 C69 1.46(3) . ? N1 C1 1.334(9) . ? N1 C5 1.352(9) . ? N2 C6 1.304(9) . ? N2 N3 1.372(8) . ? N3 C8 1.381(9) . ? N4 C8 1.308(9) . ? N4 N5 1.376(8) . ? N5 C9 1.287(9) . ? N6 C11 1.350(10) . ? N6 C15 1.353(9) . ? N7 C16 1.339(10) . ? N7 C20 1.374(10) . ? N8 C21 1.300(9) . ? N8 N9 1.393(8) . ? N9 C23 1.315(10) . ? N10 N11 1.358(9) . ? N10 C23 1.364(9) . ? N11 C24 1.287(10) . ? N12 C30 1.349(10) . ? N12 C26 1.350(11) . ? N13 C31 1.341(10) . ? N13 C35 1.366(10) . ? N14 C36 1.277(9) . ? N14 N15 1.382(8) . ? N15 C38 1.378(10) . ? N16 C38 1.304(9) . ? N16 N17 1.381(9) . ? N17 C39 1.309(10) . ? N18 C45 1.347(10) . ? N18 C41 1.365(11) . ? N19 C46 1.333(9) . ? N19 C50 1.364(9) . ? N20 C51 1.318(9) . ? N20 N21 1.364(8) . ? N21 C53 1.317(9) . ? N22 N23 1.366(8) . ? N22 C53 1.371(9) . ? N23 C54 1.290(9) . ? N24 C60 1.323(10) . ? N24 C56 1.359(10) . ? C1 C2 1.380(11) . ? C1 H1 0.9500 . ? C2 C3 1.365(12) . ? C2 H2 0.9500 . ? C3 C4 1.403(12) . ? C3 H3 0.9500 . ? C4 C5 1.370(11) . ? C4 H4 0.9500 . ? C5 C6 1.469(10) . ? C6 C7 1.500(11) . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C7 H7 0.9800 . ? C9 C11 1.480(11) . ? C9 C10 1.496(11) . ? C10 H8 0.9800 . ? C10 H9 0.9800 . ? C10 H10 0.9800 . ? C11 C12 1.392(11) . ? C12 C13 1.392(13) . ? C12 H11 0.9500 . ? C13 C14 1.362(13) . ? C13 H12 0.9500 . ? C14 C15 1.384(11) . ? C14 H13 0.9500 . ? C15 H14 0.9500 . ? C16 C17 1.375(12) . ? C16 H15 0.9500 . ? C17 C18 1.374(14) . ? C17 H16 0.9500 . ? C18 C19 1.372(13) . ? C18 H17 0.9500 . ? C19 C20 1.365(11) . ? C19 H18 0.9500 . ? C20 C21 1.473(10) . ? C21 C22 1.483(10) . ? C22 H19 0.9800 . ? C22 H20 0.9800 . ? C22 H21 0.9800 . ? C24 C25 1.466(13) . ? C24 C26 1.483(12) . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C25 H24 0.9800 . ? C26 C27 1.374(12) . ? C27 C28 1.399(14) . ? C27 H25 0.9500 . ? C28 C29 1.363(16) . ? C28 H26 0.9500 . ? C29 C30 1.384(12) . ? C29 H27 0.9500 . ? C30 H28 0.9500 . ? C31 C32 1.404(12) . ? C31 H29 0.9500 . ? C32 C33 1.368(13) . ? C32 H30 0.9500 . ? C33 C34 1.394(12) . ? C33 H31 0.9500 . ? C34 C35 1.380(11) . ? C34 H32 0.9500 . ? C35 C36 1.492(10) . ? C36 C37 1.482(10) . ? C37 H33 0.9800 . ? C37 H34 0.9800 . ? C37 H35 0.9800 . ? C39 C41 1.452(12) . ? C39 C40 1.491(13) . ? C40 H36 0.9800 . ? C40 H37 0.9800 . ? C40 H38 0.9800 . ? C41 C42 1.393(12) . ? C42 C43 1.367(14) . ? C42 H39 0.9500 . ? C43 C44 1.376(16) . ? C43 H40 0.9500 . ? C44 C45 1.365(14) . ? C44 H41 0.9500 . ? C45 H42 0.9500 . ? C46 C47 1.389(11) . ? C46 H43 0.9500 . ? C47 C48 1.376(12) . ? C47 H44 0.9500 . ? C48 C49 1.401(10) . ? C48 H45 0.9500 . ? C49 C50 1.373(10) . ? C49 H46 0.9500 . ? C50 C51 1.482(10) . ? C51 C52 1.468(10) . ? C52 H47 0.9800 . ? C52 H48 0.9800 . ? C52 H49 0.9800 . ? C54 C55 1.484(11) . ? C54 C56 1.498(11) . ? C55 H50 0.9800 . ? C55 H51 0.9800 . ? C55 H52 0.9800 . ? C56 C57 1.389(10) . ? C57 C58 1.390(12) . ? C57 H53 0.9500 . ? C58 C59 1.357(13) . ? C58 H54 0.9500 . ? C59 C60 1.387(12) . ? C59 H55 0.9500 . ? C60 H56 0.9500 . ? C67 H57 0.9800 . ? C67 H58 0.9800 . ? C67 H59 0.9800 . ? C68 H60 0.9800 . ? C68 H61 0.9800 . ? C68 H62 0.9800 . ? C69 H63 0.9800 . ? C69 H64 0.9800 . ? C69 H65 0.9800 . ? 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 N14 Fe1 N2 174.6(2) . . ? N14 Fe1 O1 103.5(2) . . ? N2 Fe1 O1 74.1(2) . . ? N14 Fe1 O3 74.7(2) . . ? N2 Fe1 O3 110.2(2) . . ? O1 Fe1 O3 95.57(19) . . ? N14 Fe1 N1 108.2(2) . . ? N2 Fe1 N1 74.3(2) . . ? O1 Fe1 N1 148.4(2) . . ? O3 Fe1 N1 93.1(2) . . ? N14 Fe1 N13 74.1(2) . . ? N2 Fe1 N13 101.2(2) . . ? O1 Fe1 N13 94.6(2) . . ? O3 Fe1 N13 148.6(2) . . ? N1 Fe1 N13 93.6(2) . . ? N5 Fe2 N20 168.6(2) . . ? N5 Fe2 O1 73.3(2) . . ? N20 Fe2 O1 118.0(2) . . ? N5 Fe2 O4 109.0(2) . . ? N20 Fe2 O4 73.0(2) . . ? O1 Fe2 O4 95.13(19) . . ? N5 Fe2 N19 103.4(2) . . ? N20 Fe2 N19 74.9(2) . . ? O1 Fe2 N19 95.2(2) . . ? O4 Fe2 N19 147.5(2) . . ? N5 Fe2 N6 74.5(2) . . ? N20 Fe2 N6 94.2(2) . . ? O1 Fe2 N6 147.7(2) . . ? O4 Fe2 N6 97.4(2) . . ? N19 Fe2 N6 90.0(2) . . ? N8 Fe3 N17 176.4(3) . . ? N8 Fe3 N18 98.1(3) . . ? N17 Fe3 N18 80.1(3) . . ? N8 Fe3 N7 80.4(2) . . ? N17 Fe3 N7 96.6(3) . . ? N18 Fe3 N7 94.0(2) . . ? N8 Fe3 O3 102.8(2) . . ? N17 Fe3 O3 79.1(2) . . ? N18 Fe3 O3 159.0(2) . . ? N7 Fe3 O3 91.5(2) . . ? N8 Fe3 O2 79.3(2) . . ? N17 Fe3 O2 103.8(2) . . ? N18 Fe3 O2 91.2(2) . . ? N7 Fe3 O2 159.6(2) . . ? O3 Fe3 O2 90.6(2) . . ? O4 Fe4 O2 94.72(19) . . ? O4 Fe4 N11 113.8(2) . . ? O2 Fe4 N11 73.4(2) . . ? O4 Fe4 N23 73.8(2) . . ? O2 Fe4 N23 111.7(2) . . ? N11 Fe4 N23 171.0(2) . . ? O4 Fe4 N24 147.7(2) . . ? O2 Fe4 N24 97.3(2) . . ? N11 Fe4 N24 98.4(2) . . ? N23 Fe4 N24 73.9(2) . . ? O4 Fe4 N12 94.1(2) . . ? O2 Fe4 N12 146.0(2) . . ? N11 Fe4 N12 73.0(2) . . ? N23 Fe4 N12 102.2(2) . . ? N24 Fe4 N12 92.5(2) . . ? O7 S1 O6 115.0(4) . . ? O7 S1 O5 113.3(4) . . ? O6 S1 O5 115.4(4) . . ? O7 S1 C61 105.4(5) . . ? O6 S1 C61 102.2(4) . . ? O5 S1 C61 103.5(5) . . ? O8 S2 O10 108.1(8) . . ? O8 S2 O9 122.7(9) . . ? O10 S2 O9 117.0(10) . . ? O8 S2 C62 93.9(9) . . ? O10 S2 C62 105.6(9) . . ? O9 S2 C62 105.7(10) . . ? O13 S3 O12 118.3(10) . . ? O13 S3 O11 110.7(9) . . ? O12 S3 O11 110.3(10) . . ? O13 S3 C63 107.8(8) . . ? O12 S3 C63 110.0(10) . . ? O11 S3 C63 97.9(8) . . ? F9 C63 F8 97.0(11) . . ? F9 C63 F7 117.2(13) . . ? F8 C63 F7 120.2(12) . . ? F9 C63 S3 104.0(10) . . ? F8 C63 S3 124.1(11) . . ? F7 C63 S3 94.7(10) . . ? O16 S4 O14 118.9(9) . . ? O16 S4 O15 110.5(10) . . ? O14 S4 O15 111.7(9) . . ? O16 S4 C64 104.6(9) . . ? O14 S4 C64 105.1(7) . . ? O15 S4 C64 104.8(8) . . ? F10 C64 F9 103.4(9) . . ? F10 C64 F8 103.0(9) . . ? F9 C64 F8 103.0(8) . . ? F10 C64 S4 116.6(8) . . ? F9 C64 S4 117.4(8) . . ? F8 C64 S4 111.7(8) . . ? O19 S5 O17 116.0(6) . . ? O19 S5 O18 117.5(7) . . ? O17 S5 O18 115.0(6) . . ? O19 S5 C65 100.9(7) . . ? O17 S5 C65 100.3(6) . . ? O18 S5 C65 103.3(7) . . ? F12 C65 F11 107.5(11) . . ? F12 C65 F13 109.5(11) . . ? F11 C65 F13 107.5(11) . . ? F12 C65 S5 110.9(9) . . ? F11 C65 S5 109.9(9) . . ? F13 C65 S5 111.4(9) . . ? O20 S6 O21 114(2) . . ? O20 S6 O22 115.2(17) . . ? O21 S6 O22 113(2) . . ? O20 S6 C66 102.4(15) . . ? O21 S6 C66 111(2) . . ? O22 S6 C66 99.4(12) . . ? F16 C66 F15 107.2(19) . . ? F16 C66 F14 108(2) . . ? F15 C66 F14 105(2) . . ? F16 C66 S6 112.1(17) . . ? F15 C66 S6 117.8(18) . . ? F14 C66 S6 106.1(17) . . ? C8 O1 Fe1 118.0(4) . . ? C8 O1 Fe2 112.4(4) . . ? Fe1 O1 Fe2 129.6(2) . . ? C23 O2 Fe3 108.9(4) . . ? C23 O2 Fe4 116.6(4) . . ? Fe3 O2 Fe4 134.4(3) . . ? C38 O3 Fe3 107.7(4) . . ? C38 O3 Fe1 115.5(4) . . ? Fe3 O3 Fe1 136.6(2) . . ? C53 O4 Fe4 118.0(4) . . ? C53 O4 Fe2 111.7(4) . . ? Fe4 O4 Fe2 129.4(2) . . ? C1 N1 C5 119.3(6) . . ? C1 N1 Fe1 124.8(5) . . ? C5 N1 Fe1 115.9(5) . . ? C6 N2 N3 122.0(6) . . ? C6 N2 Fe1 120.9(5) . . ? N3 N2 Fe1 117.0(4) . . ? N2 N3 C8 113.6(6) . . ? C8 N4 N5 108.6(6) . . ? C9 N5 N4 120.0(6) . . ? C9 N5 Fe2 120.6(5) . . ? N4 N5 Fe2 119.2(4) . . ? C11 N6 C15 118.2(7) . . ? C11 N6 Fe2 114.3(5) . . ? C15 N6 Fe2 127.4(5) . . ? C16 N7 C20 117.8(7) . . ? C16 N7 Fe3 128.7(6) . . ? C20 N7 Fe3 113.5(5) . . ? C21 N8 N9 120.1(6) . . ? C21 N8 Fe3 120.9(5) . . ? N9 N8 Fe3 118.9(4) . . ? C23 N9 N8 108.1(6) . . ? N11 N10 C23 113.9(6) . . ? C24 N11 N10 120.2(7) . . ? C24 N11 Fe4 122.7(6) . . ? N10 N11 Fe4 117.1(5) . . ? C30 N12 C26 119.2(7) . . ? C30 N12 Fe4 125.0(6) . . ? C26 N12 Fe4 115.7(5) . . ? C31 N13 C35 117.9(7) . . ? C31 N13 Fe1 127.0(5) . . ? C35 N13 Fe1 115.1(5) . . ? C36 N14 N15 120.6(6) . . ? C36 N14 Fe1 123.0(5) . . ? N15 N14 Fe1 116.3(4) . . ? C38 N15 N14 114.6(6) . . ? C38 N16 N17 107.2(6) . . ? C39 N17 N16 119.9(7) . . ? C39 N17 Fe3 120.5(5) . . ? N16 N17 Fe3 119.3(5) . . ? C45 N18 C41 117.7(8) . . ? C45 N18 Fe3 128.4(7) . . ? C41 N18 Fe3 113.8(5) . . ? C46 N19 C50 118.1(6) . . ? C46 N19 Fe2 127.1(5) . . ? C50 N19 Fe2 114.7(5) . . ? C51 N20 N21 118.8(6) . . ? C51 N20 Fe2 120.1(5) . . ? N21 N20 Fe2 119.8(4) . . ? C53 N21 N20 107.9(5) . . ? N23 N22 C53 115.0(6) . . ? C54 N23 N22 122.3(6) . . ? C54 N23 Fe4 121.5(5) . . ? N22 N23 Fe4 116.1(4) . . ? C60 N24 C56 117.7(7) . . ? C60 N24 Fe4 126.6(6) . . ? C56 N24 Fe4 115.6(5) . . ? N1 C1 C2 122.3(7) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 118.6(8) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.8(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 118.4(8) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 121.6(7) . . ? N1 C5 C6 115.4(6) . . ? C4 C5 C6 123.0(7) . . ? N2 C6 C5 113.3(6) . . ? N2 C6 C7 123.8(7) . . ? C5 C6 C7 122.9(7) . . ? C6 C7 H5 109.5 . . ? C6 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C6 C7 H7 109.5 . . ? H5 C7 H7 109.5 . . ? H6 C7 H7 109.5 . . ? O1 C8 N4 126.2(6) . . ? O1 C8 N3 117.2(6) . . ? N4 C8 N3 116.5(6) . . ? N5 C9 C11 114.1(7) . . ? N5 C9 C10 125.3(7) . . ? C11 C9 C10 120.5(7) . . ? C9 C10 H8 109.5 . . ? C9 C10 H9 109.5 . . ? H8 C10 H9 109.5 . . ? C9 C10 H10 109.5 . . ? H8 C10 H10 109.5 . . ? H9 C10 H10 109.5 . . ? N6 C11 C12 121.7(8) . . ? N6 C11 C9 115.9(7) . . ? C12 C11 C9 122.4(8) . . ? C13 C12 C11 118.8(9) . . ? C13 C12 H11 120.6 . . ? C11 C12 H11 120.6 . . ? C14 C13 C12 119.7(8) . . ? C14 C13 H12 120.2 . . ? C12 C13 H12 120.2 . . ? C13 C14 C15 118.9(8) . . ? C13 C14 H13 120.5 . . ? C15 C14 H13 120.5 . . ? N6 C15 C14 122.7(8) . . ? N6 C15 H14 118.7 . . ? C14 C15 H14 118.7 . . ? N7 C16 C17 122.8(8) . . ? N7 C16 H15 118.6 . . ? C17 C16 H15 118.6 . . ? C18 C17 C16 118.9(8) . . ? C18 C17 H16 120.6 . . ? C16 C17 H16 120.6 . . ? C19 C18 C17 119.3(8) . . ? C19 C18 H17 120.4 . . ? C17 C18 H17 120.4 . . ? C20 C19 C18 120.0(9) . . ? C20 C19 H18 120.0 . . ? C18 C19 H18 120.0 . . ? C19 C20 N7 121.2(7) . . ? C19 C20 C21 124.7(8) . . ? N7 C20 C21 114.0(6) . . ? N8 C21 C20 110.8(7) . . ? N8 C21 C22 125.8(7) . . ? C20 C21 C22 123.4(7) . . ? C21 C22 H19 109.5 . . ? C21 C22 H20 109.5 . . ? H19 C22 H20 109.5 . . ? C21 C22 H21 109.5 . . ? H19 C22 H21 109.5 . . ? H20 C22 H21 109.5 . . ? O2 C23 N9 124.8(6) . . ? O2 C23 N10 118.7(7) . . ? N9 C23 N10 116.4(6) . . ? N11 C24 C25 122.7(8) . . ? N11 C24 C26 112.5(7) . . ? C25 C24 C26 124.7(8) . . ? C24 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C25 H24 109.5 . . ? H22 C25 H24 109.5 . . ? H23 C25 H24 109.5 . . ? N12 C26 C27 121.6(8) . . ? N12 C26 C24 116.1(7) . . ? C27 C26 C24 122.2(9) . . ? C26 C27 C28 117.8(10) . . ? C26 C27 H25 121.1 . . ? C28 C27 H25 121.1 . . ? C29 C28 C27 121.1(9) . . ? C29 C28 H26 119.4 . . ? C27 C28 H26 119.4 . . ? C28 C29 C30 117.7(9) . . ? C28 C29 H27 121.1 . . ? C30 C29 H27 121.1 . . ? N12 C30 C29 122.2(9) . . ? N12 C30 H28 118.9 . . ? C29 C30 H28 118.9 . . ? N13 C31 C32 123.0(8) . . ? N13 C31 H29 118.5 . . ? C32 C31 H29 118.5 . . ? C33 C32 C31 118.5(8) . . ? C33 C32 H30 120.8 . . ? C31 C32 H30 120.8 . . ? C32 C33 C34 119.3(8) . . ? C32 C33 H31 120.4 . . ? C34 C33 H31 120.4 . . ? C35 C34 C33 119.6(8) . . ? C35 C34 H32 120.2 . . ? C33 C34 H32 120.2 . . ? N13 C35 C34 121.7(7) . . ? N13 C35 C36 115.2(7) . . ? C34 C35 C36 123.1(7) . . ? N14 C36 C37 125.2(7) . . ? N14 C36 C35 112.6(6) . . ? C37 C36 C35 122.2(7) . . ? C36 C37 H33 109.5 . . ? C36 C37 H34 109.5 . . ? H33 C37 H34 109.5 . . ? C36 C37 H35 109.5 . . ? H33 C37 H35 109.5 . . ? H34 C37 H35 109.5 . . ? N16 C38 O3 126.4(7) . . ? N16 C38 N15 115.5(6) . . ? O3 C38 N15 118.0(6) . . ? N17 C39 C41 110.9(7) . . ? N17 C39 C40 122.8(8) . . ? C41 C39 C40 126.3(7) . . ? C39 C40 H36 109.5 . . ? C39 C40 H37 109.5 . . ? H36 C40 H37 109.5 . . ? C39 C40 H38 109.5 . . ? H36 C40 H38 109.5 . . ? H37 C40 H38 109.5 . . ? N18 C41 C42 120.8(8) . . ? N18 C41 C39 114.4(7) . . ? C42 C41 C39 124.7(9) . . ? C43 C42 C41 120.0(10) . . ? C43 C42 H39 120.0 . . ? C41 C42 H39 120.0 . . ? C42 C43 C44 118.9(9) . . ? C42 C43 H40 120.6 . . ? C44 C43 H40 120.6 . . ? C45 C44 C43 119.4(9) . . ? C45 C44 H41 120.3 . . ? C43 C44 H41 120.3 . . ? N18 C45 C44 123.2(10) . . ? N18 C45 H42 118.4 . . ? C44 C45 H42 118.4 . . ? N19 C46 C47 122.6(7) . . ? N19 C46 H43 118.7 . . ? C47 C46 H43 118.7 . . ? C48 C47 C46 119.3(7) . . ? C48 C47 H44 120.3 . . ? C46 C47 H44 120.3 . . ? C47 C48 C49 118.6(7) . . ? C47 C48 H45 120.7 . . ? C49 C48 H45 120.7 . . ? C50 C49 C48 119.0(7) . . ? C50 C49 H46 120.5 . . ? C48 C49 H46 120.5 . . ? N19 C50 C49 122.4(7) . . ? N19 C50 C51 116.0(6) . . ? C49 C50 C51 121.6(7) . . ? N20 C51 C52 124.1(7) . . ? N20 C51 C50 113.3(6) . . ? C52 C51 C50 122.5(6) . . ? C51 C52 H47 109.5 . . ? C51 C52 H48 109.5 . . ? H47 C52 H48 109.5 . . ? C51 C52 H49 109.5 . . ? H47 C52 H49 109.5 . . ? H48 C52 H49 109.5 . . ? O4 C53 N21 126.1(6) . . ? O4 C53 N22 117.1(6) . . ? N21 C53 N22 116.7(6) . . ? N23 C54 C55 126.7(7) . . ? N23 C54 C56 113.1(7) . . ? C55 C54 C56 120.2(7) . . ? C54 C55 H50 109.5 . . ? C54 C55 H51 109.5 . . ? H50 C55 H51 109.5 . . ? C54 C55 H52 109.5 . . ? H50 C55 H52 109.5 . . ? H51 C55 H52 109.5 . . ? N24 C56 C57 122.2(7) . . ? N24 C56 C54 115.7(6) . . ? C57 C56 C54 122.0(7) . . ? C56 C57 C58 118.3(8) . . ? C56 C57 H53 120.9 . . ? C58 C57 H53 120.9 . . ? C59 C58 C57 119.4(8) . . ? C59 C58 H54 120.3 . . ? C57 C58 H54 120.3 . . ? C58 C59 C60 119.1(8) . . ? C58 C59 H55 120.4 . . ? C60 C59 H55 120.4 . . ? N24 C60 C59 123.2(8) . . ? N24 C60 H56 118.4 . . ? C59 C60 H56 118.4 . . ? F2 C61 F3 108.0(9) . . ? F2 C61 F1 107.4(9) . . ? F3 C61 F1 109.0(9) . . ? F2 C61 S1 111.1(8) . . ? F3 C61 S1 112.3(7) . . ? F1 C61 S1 108.9(7) . . ? F4 C62 F5 122.9(17) . . ? F4 C62 F6 105.6(18) . . ? F5 C62 F6 102.2(18) . . ? F4 C62 S2 115.0(13) . . ? F5 C62 S2 111.4(14) . . ? F6 C62 S2 94.2(14) . . ? O23 C67 H57 109.5 . . ? O23 C67 H58 109.5 . . ? H57 C67 H58 109.5 . . ? O23 C67 H59 109.5 . . ? H57 C67 H59 109.5 . . ? H58 C67 H59 109.5 . . ? O24 C68 H60 109.5 . . ? O24 C68 H61 109.5 . . ? H60 C68 H61 109.5 . . ? O24 C68 H62 109.5 . . ? H60 C68 H62 109.5 . . ? H61 C68 H62 109.5 . . ? O25 C69 H63 109.5 . . ? O25 C69 H64 109.5 . . ? H63 C69 H64 109.5 . . ? O25 C69 H65 109.5 . . ? H63 C69 H65 109.5 . . ? H64 C69 H65 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.089 _refine_diff_density_min -2.185 _refine_diff_density_rms 0.159 data_Compound4 _database_code_depnum_ccdc_archive 'CCDC 743065' #TrackingRef 'KS_Paper_Submission_CIF_Revised2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 Fe4 N24 S4, 2(C F3 O3 S), 2(H2 O)' _chemical_formula_sum 'C62 H62 F6 Fe4 N24 O8 S6' _chemical_formula_weight 1801.07 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' F F 0.0171 0.0103 '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 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.487(9) _cell_length_b 18.419(5) _cell_length_c 14.466(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.027(5) _cell_angle_gamma 90.00 _cell_volume 7428(4) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 15189 _cell_measurement_theta_min 2.4733 _cell_measurement_theta_max 30.7377 _exptl_crystal_description Prism _exptl_crystal_colour Black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3680 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9734 _exptl_absorpt_correction_T_min 0.8537 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite-Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 46757 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7678 _reflns_number_gt 7264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The triflate anion present in the asymmetric unit was refined using the shelxl PART instruction, with [S(3), F(1-3), O(1-3) and C(31)] making up a 0.65 occupancy component and [S(4), F(4-6), O(4-6) and C(32)] making up the remaining 0.35 occupancy component. It should be noted that while the triflate atoms in this model are all isotropic, this was not a trivial assignment. Distance (DFIX) and angle (DANG) restraints were used, however, while refinement with ISOR and SIMU restraints was attempted at great length, satisfactory anisotropic temperature factors could not be achieved. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1538P)^2^+95.5155P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7678 _refine_ls_number_parameters 498 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.1050 _refine_ls_wR_factor_ref 0.2798 _refine_ls_wR_factor_gt 0.2767 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S3 S 0.21258(19) 0.4347(3) 0.6554(4) 0.0902(13) Uiso 0.65 1 d PD A 1 F1 F 0.1566(7) 0.4219(14) 0.4728(17) 0.250(11) Uiso 0.65 1 d PD A 1 F2 F 0.2014(8) 0.3361(9) 0.5107(16) 0.213(9) Uiso 0.65 1 d PD A 1 F3 F 0.2304(7) 0.4453(11) 0.4894(14) 0.192(8) Uiso 0.65 1 d PD A 1 O1 O 0.1742(6) 0.4000(10) 0.6794(13) 0.134(6) Uiso 0.65 1 d PD A 1 O2 O 0.2033(9) 0.5100(9) 0.6415(17) 0.183(9) Uiso 0.65 1 d PD A 1 O3 O 0.2630(5) 0.4232(10) 0.7129(12) 0.133(6) Uiso 0.65 1 d PD A 1 C31 C 0.2040(5) 0.4087(7) 0.5398(8) 0.061(3) Uiso 0.65 1 d PD A 1 S4 S 0.2267(4) 0.4351(6) 0.7125(9) 0.110(3) Uiso 0.35 1 d PD B 2 F4 F 0.1915(7) 0.5421(9) 0.7729(15) 0.100(6) Uiso 0.35 1 d PD B 2 F5 F 0.1804(11) 0.4360(15) 0.8325(18) 0.163(11) Uiso 0.35 1 d PD B 2 F6 F 0.1372(7) 0.4637(13) 0.6756(16) 0.121(8) Uiso 0.35 1 d PD B 2 O4 O 0.2117(8) 0.3629(10) 0.6691(16) 0.093(6) Uiso 0.35 1 d PD B 2 O5 O 0.2391(11) 0.4877(14) 0.6528(19) 0.120(9) Uiso 0.35 1 d PD B 2 O6 O 0.2622(9) 0.4308(16) 0.8121(15) 0.132(10) Uiso 0.35 1 d PD B 2 C32 C 0.1808(6) 0.4701(11) 0.7459(14) 0.069(7) Uiso 0.35 1 d PD B 2 O7 O 0.1160(10) 0.4798(14) 0.749(3) 0.151(12) Uani 0.40 1 d P C 3 O8 O 0.0431(8) 0.5159(10) 0.7243(16) 0.160(8) Uani 0.60 1 d P D 4 Fe1 Fe 0.09208(3) 0.21204(4) 0.90532(6) 0.0322(3) Uani 1 1 d . . . Fe2 Fe 0.04884(3) 0.18587(4) 0.60527(6) 0.0317(3) Uani 1 1 d . . . S1 S 0.05219(5) 0.21643(7) 0.75090(11) 0.0312(3) Uani 1 1 d . . . S2 S 0.03062(5) 0.17201(7) 0.95299(11) 0.0308(3) Uani 1 1 d . . . N1 N 0.12252(18) 0.2369(3) 1.0455(4) 0.0380(11) Uani 1 1 d . . . N2 N 0.0790(2) 0.3147(3) 0.9001(4) 0.0389(12) Uani 1 1 d . . . N3 N 0.0634(2) 0.3548(3) 0.8157(4) 0.0466(14) Uani 1 1 d . . . N4 N 0.0507(2) 0.3411(3) 0.6504(4) 0.0439(13) Uani 1 1 d . . . N5 N 0.0492(2) 0.2889(3) 0.5821(4) 0.0392(12) Uani 1 1 d . . . N6 N 0.04800(18) 0.1839(3) 0.4691(4) 0.0377(11) Uani 1 1 d . . . N7 N 0.15649(18) 0.2157(3) 0.8922(4) 0.0381(12) Uani 1 1 d . . . N8 N 0.10509(17) 0.1088(3) 0.9075(4) 0.0317(10) Uani 1 1 d . . . N9 N 0.07122(17) 0.0554(2) 0.8976(4) 0.0304(10) Uani 1 1 d . . . N10 N -0.00868(17) 0.0424(3) 0.8785(4) 0.0315(10) Uani 1 1 d . . . N11 N -0.04810(16) 0.0818(3) 0.8768(4) 0.0295(10) Uani 1 1 d . . . N12 N -0.11769(19) 0.1673(3) 0.8647(4) 0.0404(12) Uani 1 1 d . . . C1 C 0.1495(2) 0.1945(4) 1.1181(5) 0.0398(14) Uani 1 1 d . . . H1 H 0.1573 0.1470 1.1026 0.048 Uiso 1 1 calc R . . C2 C 0.1662(2) 0.2169(4) 1.2141(5) 0.0470(16) Uani 1 1 d . . . H2 H 0.1854 0.1856 1.2638 0.056 Uiso 1 1 calc R . . C3 C 0.1545(3) 0.2862(4) 1.2370(6) 0.0523(18) Uani 1 1 d . . . H3 H 0.1648 0.3026 1.3028 0.063 Uiso 1 1 calc R . . C4 C 0.1277(3) 0.3309(4) 1.1623(6) 0.0539(18) Uani 1 1 d . . . H4 H 0.1200 0.3788 1.1767 0.065 Uiso 1 1 calc R . . C5 C 0.1121(3) 0.3063(4) 1.0677(6) 0.0459(16) Uani 1 1 d . . . C6 C 0.0867(3) 0.3500(4) 0.9829(6) 0.0489(17) Uani 1 1 d . . . C7 C 0.0752(4) 0.4275(4) 0.9882(7) 0.075(3) Uani 1 1 d . . . H5 H 0.0667 0.4363 1.0473 0.090 Uiso 1 1 calc R . . H6 H 0.0481 0.4407 0.9304 0.090 Uiso 1 1 calc R . . H7 H 0.1032 0.4570 0.9903 0.090 Uiso 1 1 calc R . . C8 C 0.0550(2) 0.3128(3) 0.7369(5) 0.0394(14) Uani 1 1 d . . . C9 C 0.0506(3) 0.3106(3) 0.4974(5) 0.0442(15) Uani 1 1 d . . . C10 C 0.0508(4) 0.3891(4) 0.4695(7) 0.067(2) Uani 1 1 d . . . H8 H 0.0658 0.4182 0.5283 0.080 Uiso 1 1 calc R . . H9 H 0.0178 0.4057 0.4381 0.080 Uiso 1 1 calc R . . H10 H 0.0690 0.3948 0.4240 0.080 Uiso 1 1 calc R . . C11 C 0.0513(2) 0.2513(4) 0.4314(5) 0.0432(15) Uani 1 1 d . . . C12 C 0.0572(3) 0.2586(5) 0.3403(6) 0.0549(19) Uani 1 1 d . . . H11 H 0.0603 0.3054 0.3155 0.066 Uiso 1 1 calc R . . C13 C 0.0585(3) 0.1967(5) 0.2857(6) 0.0536(18) Uani 1 1 d . . . H12 H 0.0627 0.2008 0.2235 0.064 Uiso 1 1 calc R . . C14 C 0.0538(2) 0.1302(4) 0.3232(5) 0.0462(15) Uani 1 1 d . . . H13 H 0.0541 0.0876 0.2864 0.055 Uiso 1 1 calc R . . C15 C 0.0485(2) 0.1247(4) 0.4150(5) 0.0402(14) Uani 1 1 d . . . H14 H 0.0451 0.0780 0.4400 0.048 Uiso 1 1 calc R . . C16 C 0.1802(3) 0.2745(4) 0.8790(6) 0.0488(17) Uani 1 1 d . . . H15 H 0.1649 0.3204 0.8728 0.059 Uiso 1 1 calc R . . C17 C 0.2266(3) 0.2710(5) 0.8738(6) 0.057(2) Uani 1 1 d . . . H16 H 0.2422 0.3133 0.8619 0.068 Uiso 1 1 calc R . . C18 C 0.2492(3) 0.2033(5) 0.8866(7) 0.059(2) Uani 1 1 d . . . H17 H 0.2812 0.1991 0.8862 0.070 Uiso 1 1 calc R . . C19 C 0.2246(2) 0.1430(4) 0.8998(6) 0.0490(17) Uani 1 1 d . . . H18 H 0.2395 0.0967 0.9079 0.059 Uiso 1 1 calc R . . C20 C 0.1781(2) 0.1498(4) 0.9013(5) 0.0385(13) Uani 1 1 d . . . C21 C 0.1483(2) 0.0889(3) 0.9085(4) 0.0329(12) Uani 1 1 d . . . C22 C 0.1643(2) 0.0121(4) 0.9114(5) 0.0416(14) Uani 1 1 d . . . H19 H 0.1878 0.0078 0.8770 0.050 Uiso 1 1 calc R . . H20 H 0.1366 -0.0189 0.8797 0.050 Uiso 1 1 calc R . . H21 H 0.1790 -0.0031 0.9796 0.050 Uiso 1 1 calc R . . C23 C 0.0307(2) 0.0828(3) 0.9034(4) 0.0309(11) Uani 1 1 d . . . C24 C -0.0889(2) 0.0476(3) 0.8615(4) 0.0319(12) Uani 1 1 d . . . C25 C -0.0940(2) -0.0323(3) 0.8530(5) 0.0397(13) Uani 1 1 d . . . H22 H -0.1020 -0.0465 0.7843 0.048 Uiso 1 1 calc R . . H23 H -0.1197 -0.0481 0.8777 0.048 Uiso 1 1 calc R . . H24 H -0.0638 -0.0553 0.8915 0.048 Uiso 1 1 calc R . . C26 C -0.1290(2) 0.0949(4) 0.8567(5) 0.0376(13) Uani 1 1 d . . . C27 C -0.1749(3) 0.0705(5) 0.8456(6) 0.0511(17) Uani 1 1 d . . . H25 H -0.1822 0.0202 0.8387 0.061 Uiso 1 1 calc R . . C28 C -0.2096(3) 0.1207(6) 0.8449(8) 0.069(3) Uani 1 1 d . . . H26 H -0.2414 0.1054 0.8371 0.083 Uiso 1 1 calc R . . C29 C -0.1976(3) 0.1945(5) 0.8557(8) 0.068(3) Uani 1 1 d . . . H27 H -0.2210 0.2295 0.8576 0.082 Uiso 1 1 calc R . . C30 C -0.1519(2) 0.2157(4) 0.8636(6) 0.0513(18) Uani 1 1 d . . . H28 H -0.1442 0.2659 0.8684 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O7 0.11(2) 0.096(18) 0.24(4) -0.02(2) 0.06(2) -0.066(16) O8 0.162(18) 0.103(13) 0.167(18) 0.034(12) -0.013(14) 0.057(12) Fe1 0.0291(4) 0.0199(4) 0.0456(5) -0.0002(3) 0.0094(4) -0.0045(3) Fe2 0.0291(4) 0.0217(4) 0.0447(5) 0.0017(3) 0.0127(4) -0.0041(3) S1 0.0308(7) 0.0178(6) 0.0441(8) 0.0003(5) 0.0111(6) -0.0029(5) S2 0.0287(7) 0.0198(6) 0.0437(8) -0.0013(5) 0.0119(6) 0.0004(5) N1 0.030(2) 0.029(3) 0.053(3) -0.004(2) 0.011(2) -0.008(2) N2 0.043(3) 0.020(2) 0.049(3) 0.000(2) 0.008(2) -0.006(2) N3 0.064(4) 0.019(2) 0.051(3) 0.002(2) 0.011(3) -0.005(2) N4 0.055(3) 0.020(2) 0.055(3) 0.000(2) 0.015(3) -0.008(2) N5 0.043(3) 0.022(2) 0.048(3) 0.003(2) 0.010(2) -0.004(2) N6 0.029(2) 0.035(3) 0.047(3) 0.003(2) 0.010(2) -0.004(2) N7 0.029(2) 0.034(3) 0.046(3) -0.001(2) 0.006(2) -0.007(2) N8 0.028(2) 0.022(2) 0.045(3) 0.0012(19) 0.011(2) -0.0038(18) N9 0.028(2) 0.021(2) 0.044(3) 0.0035(19) 0.0133(19) -0.0016(18) N10 0.026(2) 0.023(2) 0.047(3) -0.0008(19) 0.013(2) 0.0008(18) N11 0.024(2) 0.026(2) 0.040(2) -0.0030(19) 0.0114(18) 0.0009(17) N12 0.035(3) 0.039(3) 0.052(3) 0.003(2) 0.020(2) 0.009(2) C1 0.032(3) 0.039(3) 0.047(3) 0.006(3) 0.011(3) -0.005(3) C2 0.035(3) 0.055(4) 0.046(4) 0.006(3) 0.007(3) -0.010(3) C3 0.051(4) 0.051(4) 0.051(4) -0.007(3) 0.011(3) -0.023(3) C4 0.059(4) 0.038(4) 0.060(4) -0.012(3) 0.013(4) -0.012(3) C5 0.046(4) 0.030(3) 0.058(4) -0.005(3) 0.012(3) -0.009(3) C6 0.059(4) 0.027(3) 0.057(4) -0.004(3) 0.014(3) -0.008(3) C7 0.115(8) 0.030(4) 0.071(6) -0.016(4) 0.018(5) 0.002(4) C8 0.043(3) 0.017(3) 0.051(4) 0.004(2) 0.005(3) -0.003(2) C9 0.049(4) 0.027(3) 0.053(4) 0.006(3) 0.012(3) -0.013(3) C10 0.096(7) 0.037(4) 0.067(5) 0.015(4) 0.024(5) -0.021(4) C11 0.042(3) 0.039(3) 0.049(4) 0.004(3) 0.015(3) -0.012(3) C12 0.058(4) 0.055(5) 0.051(4) 0.014(3) 0.016(3) -0.019(4) C13 0.054(4) 0.062(5) 0.049(4) 0.008(3) 0.021(3) -0.007(4) C14 0.042(4) 0.049(4) 0.051(4) 0.001(3) 0.020(3) -0.001(3) C15 0.040(3) 0.035(3) 0.049(4) 0.000(3) 0.019(3) 0.002(3) C16 0.036(3) 0.040(4) 0.064(4) 0.003(3) 0.008(3) -0.017(3) C17 0.045(4) 0.060(5) 0.068(5) -0.003(4) 0.021(4) -0.029(4) C18 0.037(4) 0.069(5) 0.070(5) -0.003(4) 0.016(3) -0.018(4) C19 0.030(3) 0.056(4) 0.060(4) -0.001(3) 0.013(3) -0.004(3) C20 0.028(3) 0.041(3) 0.046(3) 0.000(3) 0.011(2) -0.006(2) C21 0.026(3) 0.031(3) 0.040(3) 0.003(2) 0.010(2) 0.002(2) C22 0.033(3) 0.033(3) 0.059(4) 0.002(3) 0.016(3) 0.005(2) C23 0.029(3) 0.021(2) 0.044(3) 0.001(2) 0.014(2) 0.001(2) C24 0.025(3) 0.031(3) 0.040(3) 0.004(2) 0.013(2) -0.002(2) C25 0.034(3) 0.036(3) 0.048(3) 0.002(3) 0.012(3) -0.008(2) C26 0.028(3) 0.039(3) 0.047(3) 0.002(3) 0.015(2) 0.003(2) C27 0.036(3) 0.054(4) 0.065(4) 0.010(4) 0.020(3) 0.000(3) C28 0.027(3) 0.088(7) 0.096(7) 0.014(5) 0.024(4) 0.013(4) C29 0.039(4) 0.069(6) 0.101(7) 0.010(5) 0.031(4) 0.027(4) C30 0.033(3) 0.052(4) 0.068(5) -0.001(3) 0.016(3) 0.018(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 S3 O2 1.416(15) . ? S3 O1 1.438(13) . ? S3 O3 1.464(13) . ? S3 C31 1.678(11) . ? F1 C31 1.439(16) . ? F2 C31 1.396(15) . ? F3 C31 1.399(15) . ? S4 O5 1.423(16) . ? S4 O4 1.475(15) . ? S4 O6 1.481(16) . ? S4 C32 1.705(15) . ? F4 C32 1.388(17) . ? F5 C32 1.404(17) . ? F6 C32 1.362(17) . ? Fe1 N2 1.927(5) . ? Fe1 N8 1.938(5) . ? Fe1 N7 1.970(6) . ? Fe1 N1 1.985(6) . ? Fe1 S1 2.1604(18) . ? Fe1 S2 2.2624(17) . ? Fe2 N5 1.927(5) . ? Fe2 N11 1.935(5) 2_556 ? Fe2 N6 1.962(6) . ? Fe2 N12 1.963(6) 2_556 ? Fe2 S1 2.1516(19) . ? Fe2 S2 2.2310(17) 2_556 ? S1 C8 1.791(6) . ? S2 C23 1.794(6) . ? S2 Fe2 2.2310(17) 2_556 ? N1 C1 1.341(9) . ? N1 C5 1.377(9) . ? N2 C6 1.315(9) . ? N2 N3 1.372(8) . ? N3 C8 1.333(9) . ? N4 C8 1.323(9) . ? N4 N5 1.368(8) . ? N5 C9 1.304(9) . ? N6 C15 1.345(8) . ? N6 C11 1.373(8) . ? N7 C16 1.336(8) . ? N7 C20 1.358(9) . ? N8 C21 1.321(7) . ? N8 N9 1.375(6) . ? N9 C23 1.323(7) . ? N10 C23 1.328(7) . ? N10 N11 1.364(6) . ? N11 C24 1.313(7) . ? N11 Fe2 1.935(5) 2_556 ? N12 C30 1.341(8) . ? N12 C26 1.370(9) . ? N12 Fe2 1.963(6) 2_556 ? C1 C2 1.377(10) . ? C1 H1 0.9500 . ? C2 C3 1.390(11) . ? C2 H2 0.9500 . ? C3 C4 1.383(12) . ? C3 H3 0.9500 . ? C4 C5 1.371(11) . ? C4 H4 0.9500 . ? C5 C6 1.455(11) . ? C6 C7 1.475(10) . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C7 H7 0.9800 . ? C9 C11 1.456(10) . ? C9 C10 1.501(9) . ? C10 H8 0.9800 . ? C10 H9 0.9800 . ? C10 H10 0.9800 . ? C11 C12 1.389(10) . ? C12 C13 1.394(12) . ? C12 H11 0.9500 . ? C13 C14 1.366(11) . ? C13 H12 0.9500 . ? C14 C15 1.390(10) . ? C14 H13 0.9500 . ? C15 H14 0.9500 . ? C16 C17 1.394(11) . ? C16 H15 0.9500 . ? C17 C18 1.397(13) . ? C17 H16 0.9500 . ? C18 C19 1.374(11) . ? C18 H17 0.9500 . ? C19 C20 1.382(9) . ? C19 H18 0.9500 . ? C20 C21 1.450(8) . ? C21 C22 1.488(8) . ? C22 H19 0.9800 . ? C22 H20 0.9800 . ? C22 H21 0.9800 . ? C24 C26 1.452(8) . ? C24 C25 1.480(8) . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C25 H24 0.9800 . ? C26 C27 1.384(9) . ? C27 C28 1.377(11) . ? C27 H25 0.9500 . ? C28 C29 1.399(14) . ? C28 H26 0.9500 . ? C29 C30 1.374(11) . ? C29 H27 0.9500 . ? C30 H28 0.9500 . ? 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 O2 S3 O1 109.9(13) . . ? O2 S3 O3 109.6(12) . . ? O1 S3 O3 122.2(11) . . ? O2 S3 C31 100.3(11) . . ? O1 S3 C31 103.9(9) . . ? O3 S3 C31 108.6(9) . . ? F2 C31 F3 107.0(14) . . ? F2 C31 F1 90.7(14) . . ? F3 C31 F1 98.7(14) . . ? F2 C31 S3 123.3(13) . . ? F3 C31 S3 116.9(12) . . ? F1 C31 S3 114.8(13) . . ? O5 S4 O4 117.1(16) . . ? O5 S4 O6 112.8(17) . . ? O4 S4 O6 112.6(16) . . ? O5 S4 C32 107.4(15) . . ? O4 S4 C32 107.8(12) . . ? O6 S4 C32 96.9(14) . . ? F6 C32 F4 111.4(17) . . ? F6 C32 F5 110.3(19) . . ? F4 C32 F5 104.1(18) . . ? F6 C32 S4 113.6(16) . . ? F4 C32 S4 108.2(14) . . ? F5 C32 S4 108.8(16) . . ? N2 Fe1 N8 178.7(2) . . ? N2 Fe1 N7 98.6(2) . . ? N8 Fe1 N7 81.0(2) . . ? N2 Fe1 N1 80.3(2) . . ? N8 Fe1 N1 100.9(2) . . ? N7 Fe1 N1 87.8(2) . . ? N2 Fe1 S1 83.59(17) . . ? N8 Fe1 S1 95.26(16) . . ? N7 Fe1 S1 96.66(17) . . ? N1 Fe1 S1 163.77(17) . . ? N2 Fe1 S2 99.28(18) . . ? N8 Fe1 S2 81.34(15) . . ? N7 Fe1 S2 159.02(17) . . ? N1 Fe1 S2 84.50(16) . . ? S1 Fe1 S2 96.15(6) . . ? N5 Fe2 N11 177.8(2) . 2_556 ? N5 Fe2 N6 81.0(2) . . ? N11 Fe2 N6 96.8(2) 2_556 . ? N5 Fe2 N12 98.5(2) . 2_556 ? N11 Fe2 N12 81.6(2) 2_556 2_556 ? N6 Fe2 N12 83.8(2) . 2_556 ? N5 Fe2 S1 84.90(18) . . ? N11 Fe2 S1 97.28(15) 2_556 . ? N6 Fe2 S1 165.78(16) . . ? N12 Fe2 S1 96.60(18) 2_556 . ? N5 Fe2 S2 96.37(17) . 2_556 ? N11 Fe2 S2 83.16(14) 2_556 2_556 ? N6 Fe2 S2 87.17(16) . 2_556 ? N12 Fe2 S2 161.21(18) 2_556 2_556 ? S1 Fe2 S2 96.15(6) . 2_556 ? C8 S1 Fe2 97.9(2) . . ? C8 S1 Fe1 97.1(2) . . ? Fe2 S1 Fe1 146.97(8) . . ? C23 S2 Fe2 95.31(19) . 2_556 ? C23 S2 Fe1 94.02(19) . . ? Fe2 S2 Fe1 134.00(8) 2_556 . ? C1 N1 C5 118.5(6) . . ? C1 N1 Fe1 128.4(5) . . ? C5 N1 Fe1 113.1(5) . . ? C6 N2 N3 116.9(5) . . ? C6 N2 Fe1 118.5(5) . . ? N3 N2 Fe1 124.6(4) . . ? C8 N3 N2 111.4(5) . . ? C8 N4 N5 112.1(5) . . ? C9 N5 N4 117.3(5) . . ? C9 N5 Fe2 118.0(5) . . ? N4 N5 Fe2 124.6(4) . . ? C15 N6 C11 119.1(6) . . ? C15 N6 Fe2 126.9(5) . . ? C11 N6 Fe2 113.8(5) . . ? C16 N7 C20 119.1(6) . . ? C16 N7 Fe1 127.5(5) . . ? C20 N7 Fe1 113.4(4) . . ? C21 N8 N9 117.9(5) . . ? C21 N8 Fe1 117.2(4) . . ? N9 N8 Fe1 124.5(4) . . ? C23 N9 N8 111.1(5) . . ? C23 N10 N11 111.8(5) . . ? C24 N11 N10 118.5(5) . . ? C24 N11 Fe2 116.7(4) . 2_556 ? N10 N11 Fe2 124.9(4) . 2_556 ? C30 N12 C26 119.0(6) . . ? C30 N12 Fe2 127.2(5) . 2_556 ? C26 N12 Fe2 113.2(4) . 2_556 ? N1 C1 C2 122.8(7) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 118.6(7) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 119.0(7) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C5 C4 C3 120.1(7) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 N1 120.9(7) . . ? C4 C5 C6 124.8(7) . . ? N1 C5 C6 114.2(6) . . ? N2 C6 C5 112.5(6) . . ? N2 C6 C7 123.4(7) . . ? C5 C6 C7 123.8(7) . . ? C6 C7 H5 109.5 . . ? C6 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C6 C7 H7 109.5 . . ? H5 C7 H7 109.5 . . ? H6 C7 H7 109.5 . . ? N4 C8 N3 121.0(5) . . ? N4 C8 S1 120.2(5) . . ? N3 C8 S1 118.8(5) . . ? N5 C9 C11 113.4(6) . . ? N5 C9 C10 123.6(7) . . ? C11 C9 C10 123.0(7) . . ? C9 C10 H8 109.5 . . ? C9 C10 H9 109.5 . . ? H8 C10 H9 109.5 . . ? C9 C10 H10 109.5 . . ? H8 C10 H10 109.5 . . ? H9 C10 H10 109.5 . . ? N6 C11 C12 120.7(7) . . ? N6 C11 C9 113.6(6) . . ? C12 C11 C9 125.6(7) . . ? C11 C12 C13 119.6(7) . . ? C11 C12 H11 120.2 . . ? C13 C12 H11 120.2 . . ? C14 C13 C12 118.8(7) . . ? C14 C13 H12 120.6 . . ? C12 C13 H12 120.6 . . ? C13 C14 C15 120.2(7) . . ? C13 C14 H13 119.9 . . ? C15 C14 H13 119.9 . . ? N6 C15 C14 121.5(6) . . ? N6 C15 H14 119.3 . . ? C14 C15 H14 119.3 . . ? N7 C16 C17 122.6(7) . . ? N7 C16 H15 118.7 . . ? C17 C16 H15 118.7 . . ? C16 C17 C18 117.9(7) . . ? C16 C17 H16 121.1 . . ? C18 C17 H16 121.1 . . ? C19 C18 C17 119.2(7) . . ? C19 C18 H17 120.4 . . ? C17 C18 H17 120.4 . . ? C18 C19 C20 120.0(7) . . ? C18 C19 H18 120.0 . . ? C20 C19 H18 120.0 . . ? N7 C20 C19 121.1(6) . . ? N7 C20 C21 114.9(5) . . ? C19 C20 C21 124.0(6) . . ? N8 C21 C20 113.0(5) . . ? N8 C21 C22 124.0(5) . . ? C20 C21 C22 122.9(5) . . ? C21 C22 H19 109.5 . . ? C21 C22 H20 109.5 . . ? H19 C22 H20 109.5 . . ? C21 C22 H21 109.5 . . ? H19 C22 H21 109.5 . . ? H20 C22 H21 109.5 . . ? N9 C23 N10 119.8(5) . . ? N9 C23 S2 119.6(4) . . ? N10 C23 S2 120.4(4) . . ? N11 C24 C26 114.0(5) . . ? N11 C24 C25 123.7(5) . . ? C26 C24 C25 122.3(5) . . ? C24 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C25 H24 109.5 . . ? H22 C25 H24 109.5 . . ? H23 C25 H24 109.5 . . ? N12 C26 C27 121.8(6) . . ? N12 C26 C24 114.1(5) . . ? C27 C26 C24 124.0(6) . . ? C28 C27 C26 118.6(8) . . ? C28 C27 H25 120.7 . . ? C26 C27 H25 120.7 . . ? C27 C28 C29 119.5(7) . . ? C27 C28 H26 120.2 . . ? C29 C28 H26 120.2 . . ? C30 C29 C28 119.3(7) . . ? C30 C29 H27 120.4 . . ? C28 C29 H27 120.4 . . ? N12 C30 C29 121.7(8) . . ? N12 C30 H28 119.1 . . ? C29 C30 H28 119.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.838 _refine_diff_density_min -2.257 _refine_diff_density_rms 0.158 # Attachment 'Supplementary_CIF_for_Compound_2.cif' data_Compound2-Not-Squeezed _database_code_depnum_ccdc_archive 'CCDC 749347' _publ_section_abstract ; Please see full paper. ; # start Validation Reply Form _vrf_PLAT430_Compound2-Not-Squeezed ; PROBLEM: Short Inter D...A Contact O8 .. O9 .. 1.36 Ang. RESPONSE: These are partial occupancy lattice solvent molecules. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C15 H14 S N6)2 (C15 H15 S N6)2 Co4] (C F3 S O3)2 (H2 O)5.8' _chemical_formula_sum 'C62 H69.60 Co4 F6 N24 O11.80 S6' _chemical_formula_weight 1881.87 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.950(3) _cell_length_b 27.769(6) _cell_length_c 13.903(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.404(5) _cell_angle_gamma 90.00 _cell_volume 4487.9(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 17601 _cell_measurement_theta_min 2.5033 _cell_measurement_theta_max 30.9251 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1924 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_correction_T_min 0.8974 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 20154 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.50 _reflns_number_total 9406 _reflns_number_gt 7285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _refine_special_details ; This structure was refined two ways - one SQUEEZED (which appears in the paper), and also, against the original reflection data. This .cif reflects the results against the original data, and is intended to support the presence of a difficult-to-model triflate anion, that was omitted from the SQUEEZED model. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1470P)^2^+14.1008P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9406 _refine_ls_number_parameters 584 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.3221 _refine_ls_wR_factor_gt 0.3015 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.63121(8) 0.42601(4) 0.18106(7) 0.0374(3) Uani 1 1 d . . . Co2 Co 0.37232(8) 0.52536(4) 0.20311(7) 0.0376(3) Uani 1 1 d . . . S1 S 0.54118(16) 0.49266(7) 0.20468(13) 0.0398(4) Uani 1 1 d . . . S2 S 0.75374(16) 0.47292(7) 0.12360(13) 0.0405(4) Uani 1 1 d . . . S3 S 0.9332(3) 0.7500 0.0194(3) 0.0720(10) Uani 1 2 d SD . . S4 S 0.7118(4) 0.2500 0.4777(3) 0.0732(10) Uani 1 2 d SD . . F1 F 0.7528(8) 0.7500 0.0922(10) 0.138(5) Uani 1 2 d SD . . F2 F 0.8749(14) 0.8026(6) 0.1385(14) 0.139(8) Uani 0.50 1 d PD . 1 F3 F 0.9223(12) 0.7500 0.2080(9) 0.168(7) Uani 1 2 d SD . 2 F4 F 0.9205(10) 0.2500 0.4454(7) 0.106(3) Uani 1 2 d SD . . F5 F 0.9060(6) 0.2883(2) 0.5755(5) 0.093(2) Uani 1 1 d D . . O1 O 0.9075(14) 0.8024(6) 0.003(3) 0.176(16) Uani 0.50 1 d PD A 3 O2 O 0.8708(16) 0.7705(10) -0.0648(11) 0.137(17) Uani 0.50 1 d PD . 4 O3 O 1.0528(7) 0.7500 0.0603(7) 0.057(2) Uani 1 2 d SD A . O4 O 0.6888(8) 0.2054(3) 0.4262(7) 0.096(3) Uani 1 1 d D . . O5 O 0.6771(12) 0.2500 0.5694(9) 0.103(4) Uani 1 2 d SD . . O6 O 0.253(4) 0.2500 0.512(4) 0.158(16) Uiso 0.40 2 d SP . . O7 O 0.174(2) 0.2500 0.366(2) 0.197(18) Uani 0.60 2 d SP . . O8 O 0.5865(18) 0.2500 0.1671(15) 0.065(5) Uani 0.50 2 d SP B 5 O9 O 0.5307(19) 0.2500 0.070(2) 0.059(6) Uani 0.35 2 d SP C 6 O10 O 0.5890(16) 0.2500 0.0075(13) 0.099(10) Uani 0.45 2 d SP D 7 O11 O 0.553(2) 0.2500 -0.098(2) 0.131(11) Uani 0.50 2 d SP E 8 O12 O 0.9246(19) 0.5277(8) 0.3720(14) 0.048(6) Uani 0.25 1 d P F 9 O13 O 0.9308(13) 0.5669(7) 0.3192(10) 0.079(5) Uani 0.50 1 d P G 10 O14 O 0.897(2) 0.6086(13) 0.3472(19) 0.072(9) Uani 0.25 1 d P H 11 O15 O 0.8545(15) 0.6096(9) 0.4102(13) 0.137(9) Uani 0.50 1 d P I 12 N1 N 0.7394(6) 0.3738(2) 0.1867(5) 0.0434(15) Uani 1 1 d . . . N2 N 0.7058(5) 0.4324(2) 0.3162(5) 0.0389(13) Uani 1 1 d . . . N3 N 0.6754(5) 0.4646(2) 0.3807(4) 0.0406(14) Uani 1 1 d . . . N4 N 0.5519(5) 0.5270(2) 0.3864(4) 0.0422(14) Uani 1 1 d . . . N5 N 0.4578(5) 0.5498(2) 0.3267(4) 0.0407(14) Uani 1 1 d . . . N6 N 0.2840(6) 0.5838(2) 0.2075(5) 0.0451(15) Uani 1 1 d . . . N7 N 0.5067(5) 0.3842(2) 0.2025(4) 0.0409(14) Uani 1 1 d . . . N8 N 0.5486(5) 0.4199(2) 0.0477(5) 0.0407(14) Uani 1 1 d . . . N9 N 0.5822(6) 0.4417(2) -0.0287(5) 0.0425(14) Uani 1 1 d . . . N10 N 0.7081(5) 0.4920(2) -0.0745(5) 0.0412(14) Uani 1 1 d . . . N11 N 0.8028(5) 0.5197(2) -0.0410(5) 0.0434(15) Uani 1 1 d . . . N12 N 0.7240(5) 0.5219(2) -0.2649(4) 0.0411(14) Uani 1 1 d . . . C1 C 0.7596(8) 0.3477(3) 0.1119(6) 0.052(2) Uani 1 1 d . . . H1 H 0.7075 0.3501 0.0491 0.063 Uiso 1 1 calc R . . C2 C 0.8542(8) 0.3169(3) 0.1221(7) 0.057(2) Uani 1 1 d . . . H2 H 0.8679 0.2998 0.0668 0.068 Uiso 1 1 calc R . . C3 C 0.9261(8) 0.3119(3) 0.2129(8) 0.060(2) Uani 1 1 d . . . H3 H 0.9909 0.2912 0.2220 0.072 Uiso 1 1 calc R . . C4 C 0.9038(7) 0.3375(3) 0.2919(7) 0.053(2) Uani 1 1 d . . . H4 H 0.9513 0.3331 0.3563 0.063 Uiso 1 1 calc R . . C5 C 0.8133(7) 0.3691(3) 0.2774(6) 0.0429(17) Uani 1 1 d . . . C6 C 0.7868(7) 0.4018(3) 0.3519(6) 0.0455(18) Uani 1 1 d . . . C7 C 0.8490(7) 0.3987(3) 0.4583(6) 0.051(2) Uani 1 1 d . . . H5 H 0.8730 0.3653 0.4746 0.061 Uiso 1 1 calc R . . H6 H 0.7977 0.4091 0.5001 0.061 Uiso 1 1 calc R . . H7 H 0.9169 0.4196 0.4701 0.061 Uiso 1 1 calc R . . C8 C 0.5923(6) 0.4939(3) 0.3349(5) 0.0376(15) Uani 1 1 d . . . C9 C 0.4184(7) 0.5890(3) 0.3605(6) 0.0444(17) Uani 1 1 d . . . C10 C 0.4714(10) 0.6084(3) 0.4601(6) 0.067(3) Uani 1 1 d . . . H8 H 0.5468 0.6222 0.4599 0.080 Uiso 1 1 calc R . . H9 H 0.4806 0.5824 0.5089 0.080 Uiso 1 1 calc R . . H10 H 0.4216 0.6335 0.4772 0.080 Uiso 1 1 calc R . . C11 C 0.3209(7) 0.6099(3) 0.2913(6) 0.0497(19) Uani 1 1 d . . . C12 C 0.2695(10) 0.6530(4) 0.3065(7) 0.078(3) Uani 1 1 d . . . H11 H 0.2928 0.6695 0.3677 0.093 Uiso 1 1 calc R . . C13 C 0.1841(11) 0.6715(4) 0.2315(8) 0.088(4) Uani 1 1 d . . . H12 H 0.1489 0.7015 0.2397 0.106 Uiso 1 1 calc R . . C14 C 0.1499(9) 0.6457(4) 0.1434(8) 0.074(3) Uani 1 1 d . . . H13 H 0.0931 0.6582 0.0898 0.089 Uiso 1 1 calc R . . C15 C 0.2003(8) 0.6016(3) 0.1357(6) 0.056(2) Uani 1 1 d . . . H14 H 0.1744 0.5832 0.0772 0.067 Uiso 1 1 calc R . . C16 C 0.4960(8) 0.3654(3) 0.2879(6) 0.054(2) Uani 1 1 d . . . H15 H 0.5538 0.3713 0.3463 0.064 Uiso 1 1 calc R . . C17 C 0.4005(8) 0.3369(3) 0.2931(7) 0.059(2) Uani 1 1 d . . . H16 H 0.3934 0.3236 0.3543 0.071 Uiso 1 1 calc R . . C18 C 0.3176(8) 0.3284(4) 0.2082(6) 0.058(2) Uani 1 1 d . . . H17 H 0.2523 0.3093 0.2101 0.070 Uiso 1 1 calc R . . C19 C 0.3301(7) 0.3479(3) 0.1216(6) 0.052(2) Uani 1 1 d . . . H18 H 0.2724 0.3427 0.0628 0.063 Uiso 1 1 calc R . . C20 C 0.4260(7) 0.3750(3) 0.1180(6) 0.0453(18) Uani 1 1 d . . . C21 C 0.4518(7) 0.3962(3) 0.0307(6) 0.0432(17) Uani 1 1 d . . . C22 C 0.3751(7) 0.3919(3) -0.0691(6) 0.055(2) Uani 1 1 d . . . H19 H 0.3335 0.3612 -0.0743 0.066 Uiso 1 1 calc R . . H20 H 0.4212 0.3930 -0.1189 0.066 Uiso 1 1 calc R . . H21 H 0.3199 0.4185 -0.0801 0.066 Uiso 1 1 calc R . . C23 C 0.6755(7) 0.4682(3) 0.0011(5) 0.0404(16) Uani 1 1 d . . . C24 C 0.8486(7) 0.5439(3) -0.1032(6) 0.0452(18) Uani 1 1 d . . . C25 C 0.9514(7) 0.5731(4) -0.0488(6) 0.059(2) Uani 1 1 d . . . H22 H 0.9888 0.5565 0.0124 0.071 Uiso 1 1 calc R . . H23 H 0.9255 0.6050 -0.0328 0.071 Uiso 1 1 calc R . . H24 H 1.0063 0.5767 -0.0909 0.071 Uiso 1 1 calc R . . C26 C 0.8148(7) 0.5474(3) -0.2103(6) 0.0466(18) Uani 1 1 d . . . C27 C 0.8782(9) 0.5775(4) -0.2591(7) 0.067(3) Uani 1 1 d . . . H25 H 0.9424 0.5946 -0.2215 0.081 Uiso 1 1 calc R . . C28 C 0.8491(9) 0.5826(5) -0.3599(7) 0.081(4) Uani 1 1 d . . . H26 H 0.8912 0.6038 -0.3921 0.097 Uiso 1 1 calc R . . C29 C 0.7601(8) 0.5572(4) -0.4120(7) 0.065(3) Uani 1 1 d . . . H27 H 0.7396 0.5596 -0.4821 0.078 Uiso 1 1 calc R . . C30 C 0.6988(7) 0.5279(3) -0.3641(6) 0.0467(18) Uani 1 1 d . . . H28 H 0.6350 0.5108 -0.4026 0.056 Uiso 1 1 calc R . . C31 C 0.8672(11) 0.7500 0.1128(11) 0.137(11) Uani 1 2 d SD . . C32 C 0.8629(11) 0.2500 0.5204(9) 0.064(4) Uani 1 2 d SD . . 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 Co1 0.0413(6) 0.0433(6) 0.0287(5) -0.0027(4) 0.0103(4) -0.0021(4) Co2 0.0430(6) 0.0438(6) 0.0270(5) -0.0030(4) 0.0100(4) 0.0007(4) S1 0.0443(10) 0.0495(10) 0.0263(8) -0.0031(7) 0.0093(7) 0.0009(8) S2 0.0431(10) 0.0478(10) 0.0319(9) -0.0009(7) 0.0112(7) -0.0040(8) S3 0.0500(18) 0.110(3) 0.0505(19) 0.000 0.0006(15) 0.000 S4 0.101(3) 0.0539(19) 0.064(2) 0.000 0.018(2) 0.000 F1 0.050(5) 0.211(14) 0.162(12) 0.000 0.041(6) 0.000 F2 0.111(12) 0.182(18) 0.137(16) -0.115(15) 0.057(11) -0.012(12) F3 0.112(10) 0.32(2) 0.089(10) 0.000 0.045(8) 0.000 F4 0.118(8) 0.134(9) 0.077(7) 0.000 0.050(6) 0.000 F5 0.106(5) 0.076(4) 0.089(5) -0.017(4) 0.007(4) -0.012(4) O1 0.050(9) 0.099(15) 0.33(4) 0.13(2) -0.061(16) -0.008(10) O2 0.087(11) 0.26(5) 0.052(9) 0.036(13) -0.001(8) 0.071(18) O3 0.053(5) 0.057(5) 0.059(5) 0.000 0.010(4) 0.000 O4 0.114(7) 0.062(4) 0.098(6) -0.025(4) -0.003(5) -0.010(4) O5 0.130(11) 0.092(8) 0.108(10) 0.000 0.068(9) 0.000 O7 0.078(15) 0.43(6) 0.096(19) 0.000 0.057(14) 0.000 O8 0.097(14) 0.038(9) 0.072(13) 0.000 0.045(11) 0.000 O9 0.038(12) 0.078(17) 0.064(17) 0.000 0.017(11) 0.000 O10 0.037(10) 0.24(3) 0.021(9) 0.000 0.004(8) 0.000 O11 0.072(16) 0.17(3) 0.12(2) 0.000 -0.040(15) 0.000 O12 0.057(13) 0.061(13) 0.026(10) -0.010(9) 0.009(9) -0.048(11) O13 0.076(10) 0.121(13) 0.039(7) -0.019(8) 0.011(6) -0.038(10) O14 0.045(13) 0.13(3) 0.043(14) 0.051(17) 0.019(11) 0.008(15) O15 0.090(12) 0.24(3) 0.074(11) 0.104(15) 0.016(10) -0.006(14) N1 0.054(4) 0.041(3) 0.040(3) 0.000(3) 0.020(3) 0.003(3) N2 0.042(3) 0.039(3) 0.037(3) 0.001(3) 0.012(3) -0.002(3) N3 0.042(3) 0.052(4) 0.028(3) -0.002(3) 0.008(2) -0.004(3) N4 0.045(3) 0.049(4) 0.031(3) -0.003(3) 0.005(3) -0.001(3) N5 0.043(3) 0.050(4) 0.031(3) -0.004(3) 0.011(3) 0.002(3) N6 0.054(4) 0.048(4) 0.035(3) 0.000(3) 0.013(3) 0.008(3) N7 0.049(3) 0.043(3) 0.034(3) -0.003(3) 0.017(3) -0.007(3) N8 0.043(3) 0.044(3) 0.037(3) -0.003(3) 0.014(3) 0.002(3) N9 0.053(4) 0.044(3) 0.033(3) -0.004(3) 0.015(3) -0.002(3) N10 0.046(3) 0.045(3) 0.035(3) -0.004(3) 0.014(3) -0.003(3) N11 0.045(3) 0.051(4) 0.035(3) -0.004(3) 0.012(3) -0.004(3) N12 0.042(3) 0.049(4) 0.033(3) -0.005(3) 0.010(3) -0.003(3) C1 0.058(5) 0.058(5) 0.043(4) -0.007(4) 0.017(4) -0.014(4) C2 0.068(6) 0.040(4) 0.072(6) -0.006(4) 0.036(5) 0.005(4) C3 0.050(5) 0.046(5) 0.085(7) -0.007(5) 0.017(5) 0.004(4) C4 0.044(4) 0.033(4) 0.076(6) 0.008(4) 0.004(4) -0.001(3) C5 0.047(4) 0.036(4) 0.048(4) 0.002(3) 0.015(3) -0.003(3) C6 0.044(4) 0.046(4) 0.045(4) -0.002(3) 0.008(3) -0.010(4) C7 0.055(5) 0.053(5) 0.040(4) 0.010(4) -0.001(4) 0.001(4) C8 0.038(4) 0.045(4) 0.029(3) 0.001(3) 0.008(3) -0.003(3) C9 0.047(4) 0.049(4) 0.036(4) -0.009(3) 0.008(3) -0.004(4) C10 0.100(8) 0.059(5) 0.039(5) -0.014(4) 0.012(5) 0.009(5) C11 0.060(5) 0.051(4) 0.036(4) -0.009(3) 0.006(4) 0.004(4) C12 0.117(9) 0.061(6) 0.049(6) -0.009(4) 0.007(6) 0.030(6) C13 0.125(10) 0.076(7) 0.058(6) -0.016(5) 0.010(6) 0.039(7) C14 0.080(7) 0.085(7) 0.053(6) -0.015(5) 0.006(5) 0.026(6) C15 0.059(5) 0.066(6) 0.039(4) -0.013(4) 0.002(4) 0.011(4) C16 0.061(5) 0.065(5) 0.037(4) -0.004(4) 0.016(4) -0.012(4) C17 0.059(5) 0.071(6) 0.053(5) 0.006(4) 0.024(4) -0.016(5) C18 0.063(5) 0.070(6) 0.046(5) -0.001(4) 0.019(4) -0.025(5) C19 0.053(5) 0.061(5) 0.041(4) -0.007(4) 0.007(4) -0.007(4) C20 0.046(4) 0.053(4) 0.036(4) -0.008(3) 0.007(3) -0.003(4) C21 0.050(4) 0.043(4) 0.035(4) -0.005(3) 0.007(3) -0.005(4) C22 0.057(5) 0.061(5) 0.042(5) 0.003(4) 0.001(4) -0.008(4) C23 0.047(4) 0.046(4) 0.031(4) -0.005(3) 0.015(3) 0.006(3) C24 0.048(4) 0.053(4) 0.036(4) -0.005(3) 0.012(3) -0.002(4) C25 0.050(5) 0.087(7) 0.041(5) -0.005(4) 0.012(4) -0.022(5) C26 0.044(4) 0.058(5) 0.041(4) 0.000(4) 0.015(3) -0.002(4) C27 0.066(6) 0.092(7) 0.045(5) -0.001(5) 0.014(4) -0.032(5) C28 0.073(7) 0.126(10) 0.041(5) 0.019(6) 0.007(5) -0.043(7) C29 0.063(6) 0.096(7) 0.036(5) 0.011(5) 0.010(4) -0.014(5) C30 0.047(4) 0.056(5) 0.038(4) -0.005(3) 0.011(3) -0.013(4) C31 0.050(10) 0.28(4) 0.081(14) 0.000 0.024(9) 0.000 C32 0.096(11) 0.050(7) 0.050(7) 0.000 0.023(7) 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 Co1 N2 1.892(6) . ? Co1 N8 1.895(6) . ? Co1 N1 1.933(6) . ? Co1 N7 1.964(6) . ? Co1 S1 2.203(2) . ? Co1 S2 2.241(2) . ? Co2 N10 1.886(6) 3_665 ? Co2 N5 1.908(6) . ? Co2 N6 1.946(6) . ? Co2 N12 2.061(6) 3_665 ? Co2 S1 2.208(2) . ? S1 C8 1.771(7) . ? S2 C23 1.748(8) . ? S3 O2 1.359(13) . ? S3 O2 1.359(13) 4_575 ? S3 O3 1.410(8) . ? S3 O1 1.495(14) 4_575 ? S3 O1 1.495(14) . ? S3 C31 1.669(13) . ? S4 O4 1.425(7) 4_565 ? S4 O4 1.425(7) . ? S4 O5 1.428(11) . ? S4 C32 1.766(13) . ? F1 C31 1.330(14) . ? F2 C31 1.502(14) . ? F3 C31 1.334(15) . ? F4 C32 1.377(12) . ? F5 C32 1.343(9) . ? O2 O2 1.14(5) 4_575 ? N1 C1 1.334(10) . ? N1 C5 1.368(10) . ? N2 C6 1.298(10) . ? N2 N3 1.374(8) . ? N3 C8 1.326(9) . ? N4 C8 1.324(9) . ? N4 N5 1.386(8) . ? N5 C9 1.316(10) . ? N6 C15 1.333(10) . ? N6 C11 1.356(10) . ? N7 C16 1.330(10) . ? N7 C20 1.360(9) . ? N8 C21 1.305(10) . ? N8 N9 1.360(8) . ? N9 C23 1.320(10) . ? N10 N11 1.358(9) . ? N10 C23 1.371(9) . ? N10 Co2 1.886(6) 3_665 ? N11 C24 1.310(10) . ? N12 C30 1.351(10) . ? N12 C26 1.369(10) . ? N12 Co2 2.061(6) 3_665 ? C1 C2 1.398(12) . ? C1 H1 0.9500 . ? C2 C3 1.359(13) . ? C2 H2 0.9500 . ? C3 C4 1.384(13) . ? C3 H3 0.9500 . ? C4 C5 1.371(11) . ? C4 H4 0.9500 . ? C5 C6 1.466(11) . ? C6 C7 1.496(11) . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C7 H7 0.9800 . ? C9 C11 1.449(11) . ? C9 C10 1.483(11) . ? C10 H8 0.9800 . ? C10 H9 0.9800 . ? C10 H10 0.9800 . ? C11 C12 1.384(12) . ? C12 C13 1.379(14) . ? C12 H11 0.9500 . ? C13 C14 1.397(14) . ? C13 H12 0.9500 . ? C14 C15 1.379(13) . ? C14 H13 0.9500 . ? C15 H14 0.9500 . ? C16 C17 1.403(12) . ? C16 H15 0.9500 . ? C17 C18 1.373(12) . ? C17 H16 0.9500 . ? C18 C19 1.359(12) . ? C18 H17 0.9500 . ? C19 C20 1.382(11) . ? C19 H18 0.9500 . ? C20 C21 1.445(11) . ? C21 C22 1.480(10) . ? C22 H19 0.9800 . ? C22 H20 0.9800 . ? C22 H21 0.9800 . ? C24 C26 1.453(11) . ? C24 C25 1.521(11) . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C25 H24 0.9800 . ? C26 C27 1.403(12) . ? C27 C28 1.371(13) . ? C27 H25 0.9500 . ? C28 C29 1.341(13) . ? C28 H26 0.9500 . ? C29 C30 1.368(12) . ? C29 H27 0.9500 . ? C30 H28 0.9500 . ? C31 F2 1.502(14) 4_575 ? C32 F5 1.343(9) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N8 176.9(3) . . ? N2 Co1 N1 82.7(3) . . ? N8 Co1 N1 99.5(3) . . ? N2 Co1 N7 96.0(3) . . ? N8 Co1 N7 81.7(3) . . ? N1 Co1 N7 94.2(3) . . ? N2 Co1 S1 84.67(19) . . ? N8 Co1 S1 93.40(19) . . ? N1 Co1 S1 165.9(2) . . ? N7 Co1 S1 93.45(19) . . ? N2 Co1 S2 95.90(19) . . ? N8 Co1 S2 86.5(2) . . ? N1 Co1 S2 88.0(2) . . ? N7 Co1 S2 168.11(19) . . ? S1 Co1 S2 86.95(8) . . ? N10 Co2 N5 173.3(3) 3_665 . ? N10 Co2 N6 94.7(3) 3_665 . ? N5 Co2 N6 81.7(3) . . ? N10 Co2 N12 91.3(3) 3_665 3_665 ? N5 Co2 N12 94.9(3) . 3_665 ? N6 Co2 N12 99.1(3) . 3_665 ? N10 Co2 S1 99.7(2) 3_665 . ? N5 Co2 S1 80.79(19) . . ? N6 Co2 S1 147.6(2) . . ? N12 Co2 S1 109.38(19) 3_665 . ? C8 S1 Co1 96.0(3) . . ? C8 S1 Co2 95.7(2) . . ? Co1 S1 Co2 145.14(10) . . ? C23 S2 Co1 93.3(3) . . ? O2 S3 O2 50(2) . 4_575 ? O2 S3 O3 130.6(10) . . ? O2 S3 O3 130.6(10) 4_575 . ? O2 S3 O1 102.9(19) . 4_575 ? O2 S3 O1 53.6(13) 4_575 4_575 ? O3 S3 O1 102.4(6) . 4_575 ? O2 S3 O1 53.6(13) . . ? O2 S3 O1 102.9(19) 4_575 . ? O3 S3 O1 102.4(6) . . ? O1 S3 O1 153.8(15) 4_575 . ? O2 S3 C31 113.9(10) . . ? O2 S3 C31 113.9(10) 4_575 . ? O3 S3 C31 107.7(6) . . ? O1 S3 C31 90.1(14) 4_575 . ? O1 S3 C31 90.1(14) . . ? O4 S4 O4 120.7(8) 4_565 . ? O4 S4 O5 112.7(5) 4_565 . ? O4 S4 O5 112.7(5) . . ? O4 S4 C32 103.4(5) 4_565 . ? O4 S4 C32 103.4(4) . . ? O5 S4 C32 100.7(7) . . ? O2 O2 S3 65.2(12) 4_575 . ? C1 N1 C5 118.2(7) . . ? C1 N1 Co1 128.0(6) . . ? C5 N1 Co1 113.0(5) . . ? C6 N2 N3 117.6(6) . . ? C6 N2 Co1 117.2(5) . . ? N3 N2 Co1 125.0(5) . . ? C8 N3 N2 111.6(6) . . ? C8 N4 N5 109.8(6) . . ? C9 N5 N4 118.1(6) . . ? C9 N5 Co2 117.1(5) . . ? N4 N5 Co2 124.6(5) . . ? C15 N6 C11 119.0(7) . . ? C15 N6 Co2 127.1(6) . . ? C11 N6 Co2 113.6(5) . . ? C16 N7 C20 120.1(7) . . ? C16 N7 Co1 127.0(6) . . ? C20 N7 Co1 113.0(5) . . ? C21 N8 N9 119.5(6) . . ? C21 N8 Co1 117.5(5) . . ? N9 N8 Co1 122.9(5) . . ? C23 N9 N8 112.6(6) . . ? N11 N10 C23 111.9(6) . . ? N11 N10 Co2 132.1(5) . 3_665 ? C23 N10 Co2 115.5(5) . 3_665 ? C24 N11 N10 120.4(6) . . ? C30 N12 C26 117.6(7) . . ? C30 N12 Co2 119.3(5) . 3_665 ? C26 N12 Co2 123.1(5) . 3_665 ? N1 C1 C2 122.8(8) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.5(8) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.3(8) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 120.1(9) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 121.0(8) . . ? N1 C5 C6 113.2(7) . . ? C4 C5 C6 125.8(8) . . ? N2 C6 C5 113.5(7) . . ? N2 C6 C7 124.8(7) . . ? C5 C6 C7 121.6(7) . . ? C6 C7 H5 109.5 . . ? C6 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C6 C7 H7 109.5 . . ? H5 C7 H7 109.5 . . ? H6 C7 H7 109.5 . . ? N4 C8 N3 119.5(6) . . ? N4 C8 S1 119.0(5) . . ? N3 C8 S1 121.4(5) . . ? N5 C9 C11 113.1(7) . . ? N5 C9 C10 121.6(7) . . ? C11 C9 C10 125.3(7) . . ? C9 C10 H8 109.5 . . ? C9 C10 H9 109.5 . . ? H8 C10 H9 109.5 . . ? C9 C10 H10 109.5 . . ? H8 C10 H10 109.5 . . ? H9 C10 H10 109.5 . . ? N6 C11 C12 121.6(8) . . ? N6 C11 C9 114.2(7) . . ? C12 C11 C9 124.2(8) . . ? C13 C12 C11 119.0(9) . . ? C13 C12 H11 120.5 . . ? C11 C12 H11 120.5 . . ? C12 C13 C14 119.0(10) . . ? C12 C13 H12 120.5 . . ? C14 C13 H12 120.5 . . ? C15 C14 C13 118.7(9) . . ? C15 C14 H13 120.6 . . ? C13 C14 H13 120.6 . . ? N6 C15 C14 122.4(8) . . ? N6 C15 H14 118.8 . . ? C14 C15 H14 118.8 . . ? N7 C16 C17 121.0(8) . . ? N7 C16 H15 119.5 . . ? C17 C16 H15 119.5 . . ? C18 C17 C16 119.1(8) . . ? C18 C17 H16 120.5 . . ? C16 C17 H16 120.5 . . ? C19 C18 C17 119.2(8) . . ? C19 C18 H17 120.4 . . ? C17 C18 H17 120.4 . . ? C18 C19 C20 120.7(8) . . ? C18 C19 H18 119.6 . . ? C20 C19 H18 119.6 . . ? N7 C20 C19 119.9(7) . . ? N7 C20 C21 113.8(7) . . ? C19 C20 C21 126.3(7) . . ? N8 C21 C20 114.0(7) . . ? N8 C21 C22 122.8(7) . . ? C20 C21 C22 123.2(7) . . ? C21 C22 H19 109.5 . . ? C21 C22 H20 109.5 . . ? H19 C22 H20 109.5 . . ? C21 C22 H21 109.5 . . ? H19 C22 H21 109.5 . . ? H20 C22 H21 109.5 . . ? N9 C23 N10 113.4(7) . . ? N9 C23 S2 124.7(6) . . ? N10 C23 S2 121.9(6) . . ? N11 C24 C26 130.7(7) . . ? N11 C24 C25 111.0(7) . . ? C26 C24 C25 118.3(7) . . ? C24 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C25 H24 109.5 . . ? H22 C25 H24 109.5 . . ? H23 C25 H24 109.5 . . ? N12 C26 C27 119.2(7) . . ? N12 C26 C24 122.0(7) . . ? C27 C26 C24 118.9(8) . . ? C28 C27 C26 121.3(9) . . ? C28 C27 H25 119.4 . . ? C26 C27 H25 119.4 . . ? C29 C28 C27 118.6(9) . . ? C29 C28 H26 120.7 . . ? C27 C28 H26 120.7 . . ? C28 C29 C30 119.9(8) . . ? C28 C29 H27 120.1 . . ? C30 C29 H27 120.1 . . ? N12 C30 C29 123.5(8) . . ? N12 C30 H28 118.3 . . ? C29 C30 H28 118.3 . . ? F1 C31 F3 117.5(13) . . ? F1 C31 F2 93.2(9) . 4_575 ? F3 C31 F2 77.0(10) . 4_575 ? F1 C31 F2 93.1(9) . . ? F3 C31 F2 77.0(10) . . ? F2 C31 F2 153(2) 4_575 . ? F1 C31 S3 118.7(12) . . ? F3 C31 S3 123.9(11) . . ? F2 C31 S3 99.8(9) 4_575 . ? F2 C31 S3 99.8(9) . . ? F5 C32 F5 104.9(10) 4_565 . ? F5 C32 F4 103.9(8) 4_565 . ? F5 C32 F4 103.9(8) . . ? F5 C32 S4 114.8(6) 4_565 . ? F5 C32 S4 114.8(6) . . ? F4 C32 S4 113.4(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.739 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.155