data_rco1 _vrf_GOODF01_rco1 ; PROBLEM: The least squares goodness of fit parameter lies outside the range 0.80 <> 2.00 Goodness of fit given = 0.752 RESPONSE: The goodness of fit value fell from approximately 1 to 0.752 when the data was treated with the platon squeeze procedure to account for disordered acetonitrile present within the unit cell. ; _vrf_PLAT242_rco1 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C19 RESPONSE: This alert is an artefact of the Cf3 group of which C19 is a part. The adjoined fluorine atoms show a greater thermal motion with respect to C19, as is often observed in CF3 and CMe3 groups, for example. ; #End Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 Fe N6, 3(C2 F6 N O4 S2), 2(C2 H3 N)' _chemical_formula_sum 'C46 H30 F18 Fe N11 O12 S6' _chemical_formula_weight 1519.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 20.3520(5) _cell_length_b 15.4353(4) _cell_length_c 19.6446(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.2570(10) _cell_angle_gamma 90.00 _cell_volume 5981.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 3.64 _cell_measurement_theta_max 59.80 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3052 _exptl_absorpt_coefficient_mu 5.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4949 _exptl_absorpt_correction_T_max 0.6287 _exptl_absorpt_process_details sadabs _exptl_special_details ; rco1 collected, solved and refined by Dr. Zoe R. Turner (Princeton University) ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28724 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 66.39 _reflns_number_total 5145 _reflns_number_gt 4562 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER, APEX II SOFTWARE SUITE' _computing_cell_refinement 'BRUKER, APEX II SOFTWARE SUITE' _computing_data_reduction 'BRUKER, APEX II SOFTWARE SUITE' _computing_structure_solution 'SIR-92 (Giacovazzo, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _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^ > 2\s(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. ; 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 0.106 0.250 79 20 ' ' 2 0.500 -0.106 0.750 79 20 ' ' 3 1.000 0.394 0.750 79 20 ' ' 4 1.000 0.606 0.250 79 20 ' ' _platon_squeeze_details ; The data was treated with the platon/squeeze routine to account for a further 3 molecules of acet0nitrile present within the unit cell. ; _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^)+(0.1225P)^2^+44.4362P] 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 5145 _refine_ls_number_parameters 447 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 0.752 _refine_ls_restrained_S_all 0.758 _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 C1 C 0.35209(16) 0.5203(2) 0.19759(17) 0.0202(7) Uani 1 1 d . . . H1 H 0.3578 0.5643 0.2323 0.024 Uiso 1 1 calc R . . C2 C 0.28788(16) 0.5067(2) 0.15306(18) 0.0233(7) Uani 1 1 d . . . H2 H 0.2506 0.5412 0.1579 0.028 Uiso 1 1 calc R . . C3 C 0.27859(16) 0.4438(2) 0.10248(17) 0.0217(7) Uani 1 1 d . . . H3 H 0.2349 0.4343 0.0724 0.026 Uiso 1 1 calc R . . C4 C 0.33386(15) 0.3934(2) 0.09533(15) 0.0178(6) Uani 1 1 d . . . C5 C 0.33023(16) 0.3251(2) 0.04504(16) 0.0205(7) Uani 1 1 d . . . H5 H 0.2883 0.3131 0.0126 0.025 Uiso 1 1 calc R . . C6 C 0.38565(17) 0.2775(2) 0.04307(17) 0.0219(7) Uani 1 1 d . . . H6 H 0.3816 0.2318 0.0099 0.026 Uiso 1 1 calc R . . C7 C 0.45024(16) 0.2948(2) 0.09012(16) 0.0194(7) Uani 1 1 d . . . C8 C 0.51028(18) 0.2490(2) 0.09118(18) 0.0258(7) Uani 1 1 d . . . H8 H 0.5098 0.2024 0.0595 0.031 Uiso 1 1 calc R . . C9 C 0.56949(18) 0.2720(2) 0.13833(18) 0.0275(8) Uani 1 1 d . . . H9 H 0.6102 0.2415 0.1392 0.033 Uiso 1 1 calc R . . C10 C 0.56970(16) 0.3402(2) 0.18486(17) 0.0220(7) Uani 1 1 d . . . H10 H 0.6110 0.3554 0.2172 0.026 Uiso 1 1 calc R . . C11 C 0.45495(15) 0.3624(2) 0.13842(15) 0.0172(6) Uani 1 1 d . . . C12 C 0.39659(15) 0.4108(2) 0.14185(15) 0.0152(6) Uani 1 1 d . . . C13 C 0.53469(16) 0.5690(2) 0.12930(16) 0.0204(7) Uani 1 1 d . . . H13 H 0.5393 0.5140 0.1092 0.024 Uiso 1 1 calc R . . C14 C 0.54630(17) 0.6441(2) 0.09404(17) 0.0241(7) Uani 1 1 d . . . H14 H 0.5595 0.6396 0.0510 0.029 Uiso 1 1 calc R . . C15 C 0.53870(16) 0.7242(2) 0.12125(18) 0.0241(7) Uani 1 1 d . . . H15 H 0.5468 0.7752 0.0974 0.029 Uiso 1 1 calc R . . C16 C 0.51878(15) 0.7302(2) 0.18476(17) 0.0218(7) Uani 1 1 d . . . C17 C 0.50915(17) 0.8095(2) 0.21885(19) 0.0268(7) Uani 1 1 d . . . H17 H 0.5156 0.8631 0.1977 0.032 Uiso 1 1 calc R . . C18 C 0.50938(15) 0.6522(2) 0.21778(16) 0.0175(6) Uani 1 1 d . . . C19 C 0.20575(19) 0.3662(2) 0.3086(2) 0.0328(8) Uani 1 1 d . . . C20 C 0.2613(2) 0.1156(3) 0.1687(2) 0.0367(9) Uani 1 1 d . . . F1 F 0.21031(19) 0.39311(19) 0.37340(17) 0.0758(10) Uani 1 1 d . A 1 F2 F 0.25835(14) 0.39863(16) 0.28985(19) 0.0614(8) Uani 1 1 d . A 1 F3 F 0.15051(14) 0.39953(17) 0.2687(2) 0.0733(10) Uani 1 1 d . A 1 F4 F 0.29370(14) 0.08200(16) 0.23011(13) 0.0488(6) Uani 1 1 d . . . F5 F 0.30062(16) 0.10917(18) 0.12448(15) 0.0578(8) Uani 1 1 d . . . F6 F 0.20498(14) 0.07039(15) 0.14371(14) 0.0524(7) Uani 1 1 d . . . N1 N 0.40558(13) 0.47294(17) 0.19257(13) 0.0163(5) Uani 1 1 d . . . N2 N 0.51377(12) 0.38505(17) 0.18558(13) 0.0167(5) Uani 1 1 d . . . N3 N 0.51733(12) 0.57287(17) 0.19026(13) 0.0174(6) Uani 1 1 d . . . N4 N 0.18896(14) 0.22430(19) 0.22571(15) 0.0242(6) Uani 1 1 d . . . O1 O 0.27024(12) 0.22324(17) 0.34794(12) 0.0275(5) Uani 1 1 d . . . O2 O 0.14670(12) 0.22392(16) 0.33082(12) 0.0275(5) Uani 1 1 d . . . O3 O 0.30557(12) 0.26884(17) 0.21106(13) 0.0308(6) Uani 1 1 d . . . O4 O 0.20748(12) 0.25557(17) 0.10986(12) 0.0280(5) Uani 1 1 d . . . S1 S 0.20492(4) 0.24741(5) 0.30631(4) 0.0210(2) Uani 1 1 d . A . S2 S 0.24198(4) 0.23000(5) 0.17913(4) 0.0207(2) Uani 1 1 d . A . Fe1 Fe 0.5000 0.47734(4) 0.2500 0.01413(19) Uani 1 2 d S . . C1S C 0.1647(3) 0.8352(4) 0.9932(2) 0.0585(14) Uani 1 1 d . . . H1S1 H 0.1395 0.8020 0.9526 0.088 Uiso 1 1 calc R . . H1S2 H 0.1721 0.7992 1.0355 0.088 Uiso 1 1 calc R . . H1S3 H 0.2085 0.8529 0.9854 0.088 Uiso 1 1 calc R . . C2S C 0.1262(2) 0.9115(3) 1.00211(19) 0.0380(9) Uani 1 1 d . . . N1S N 0.0957(2) 0.9714(3) 1.0081(2) 0.0472(9) Uani 1 1 d . . . F7 F 0.4346(3) 0.8821(4) 0.0506(3) 0.0508(15) Uani 0.437(7) 1 d PD B 1 F8 F 0.3810(3) 0.9995(4) 0.0687(3) 0.0508(15) Uani 0.437(7) 1 d PD B 1 F9 F 0.3361(3) 0.9134(4) -0.0181(3) 0.0508(15) Uani 0.437(7) 1 d PD B 1 F7A F 0.3256(3) 0.9704(5) 0.0197(4) 0.0924(19) Uani 0.563(7) 1 d PD B 2 F8A F 0.4190(3) 0.9727(4) 0.0961(3) 0.0924(19) Uani 0.563(7) 1 d PD B 2 F9A F 0.3930(3) 0.8625(4) 0.0311(4) 0.0924(19) Uani 0.563(7) 1 d PD B 2 S3 S 0.43113(5) 1.00256(7) -0.03533(6) 0.0376(3) Uani 1 1 d . . . O5 O 0.4252(3) 1.0876(4) -0.0218(3) 0.0415(10) Uani 0.534(5) 1 d P . 1 O6 O 0.3891(3) 0.9620(4) -0.0983(3) 0.0415(10) Uani 0.466(5) 1 d P . 1 O5A O 0.4460(3) 0.9473(4) -0.0883(3) 0.0507(17) Uani 0.534(5) 1 d P . 2 O6A O 0.3896(3) 1.0789(4) -0.0624(4) 0.0441(19) Uani 0.466(5) 1 d P . 2 C21 C 0.3919(2) 0.9472(3) 0.0239(3) 0.0534(13) Uani 1 1 d D B . N5 N 0.5000(3) 0.9531(4) -0.0148(4) 0.0352(15) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0208(16) 0.0194(16) 0.0196(16) 0.0009(12) 0.0038(13) 0.0030(12) C2 0.0179(17) 0.0251(17) 0.0272(18) 0.0028(14) 0.0060(14) 0.0049(13) C3 0.0160(15) 0.0253(17) 0.0204(16) 0.0025(13) -0.0017(12) -0.0014(13) C4 0.0177(15) 0.0215(16) 0.0136(14) 0.0055(12) 0.0025(12) -0.0002(12) C5 0.0224(16) 0.0259(17) 0.0133(15) -0.0006(13) 0.0046(12) -0.0050(13) C6 0.0267(17) 0.0243(17) 0.0151(15) -0.0027(13) 0.0055(13) -0.0045(13) C7 0.0215(16) 0.0226(16) 0.0148(15) 0.0005(12) 0.0058(12) 0.0014(13) C8 0.0294(18) 0.0280(18) 0.0216(17) -0.0038(14) 0.0094(14) 0.0049(14) C9 0.0214(17) 0.036(2) 0.0252(18) -0.0059(15) 0.0069(14) 0.0082(14) C10 0.0168(15) 0.0296(18) 0.0187(16) 0.0008(13) 0.0030(13) 0.0012(13) C11 0.0177(15) 0.0212(16) 0.0131(14) 0.0045(12) 0.0044(12) 0.0016(12) C12 0.0174(15) 0.0169(15) 0.0114(14) 0.0016(11) 0.0035(12) -0.0011(12) C13 0.0180(15) 0.0266(17) 0.0163(15) -0.0004(13) 0.0039(12) -0.0023(13) C14 0.0241(17) 0.0303(18) 0.0174(16) 0.0042(14) 0.0043(13) -0.0010(14) C15 0.0196(16) 0.0293(18) 0.0220(17) 0.0085(14) 0.0021(13) -0.0021(13) C16 0.0141(15) 0.0248(18) 0.0232(17) 0.0038(13) -0.0017(13) -0.0015(12) C17 0.0225(17) 0.0217(17) 0.0338(19) 0.0027(15) 0.0025(14) 0.0000(14) C18 0.0103(14) 0.0212(16) 0.0184(15) 0.0007(13) -0.0018(11) 0.0008(12) C19 0.0301(19) 0.0271(19) 0.042(2) -0.0094(16) 0.0100(17) -0.0015(15) C20 0.045(2) 0.035(2) 0.033(2) 0.0042(17) 0.0171(18) 0.0074(18) F1 0.119(3) 0.0481(17) 0.073(2) -0.0318(16) 0.047(2) -0.0045(17) F2 0.0485(15) 0.0274(13) 0.120(3) -0.0180(14) 0.0427(16) -0.0141(11) F3 0.0482(16) 0.0282(13) 0.126(3) 0.0122(15) -0.0119(17) 0.0008(12) F4 0.0616(16) 0.0385(13) 0.0486(15) 0.0153(11) 0.0179(12) 0.0173(12) F5 0.0792(19) 0.0506(16) 0.0573(16) 0.0018(13) 0.0431(15) 0.0219(14) F6 0.0663(17) 0.0284(13) 0.0600(16) -0.0115(11) 0.0105(13) -0.0107(12) N1 0.0157(13) 0.0193(13) 0.0137(13) 0.0012(10) 0.0030(10) -0.0006(10) N2 0.0159(13) 0.0187(13) 0.0150(12) 0.0021(10) 0.0029(10) -0.0004(10) N3 0.0141(12) 0.0206(14) 0.0160(13) 0.0011(10) 0.0007(10) 0.0002(10) N4 0.0203(14) 0.0311(16) 0.0204(14) -0.0026(12) 0.0040(11) -0.0051(12) O1 0.0236(12) 0.0362(14) 0.0207(12) -0.0018(10) 0.0017(10) -0.0023(10) O2 0.0224(12) 0.0366(14) 0.0254(12) -0.0008(10) 0.0094(10) -0.0014(10) O3 0.0249(13) 0.0433(15) 0.0227(12) 0.0041(11) 0.0033(10) -0.0117(11) O4 0.0311(13) 0.0334(14) 0.0176(12) 0.0008(10) 0.0025(10) -0.0034(11) S1 0.0195(4) 0.0238(4) 0.0195(4) -0.0024(3) 0.0044(3) -0.0013(3) S2 0.0205(4) 0.0229(4) 0.0181(4) 0.0001(3) 0.0036(3) -0.0034(3) Fe1 0.0128(3) 0.0181(4) 0.0111(3) 0.000 0.0024(3) 0.000 C1S 0.077(4) 0.070(3) 0.029(2) 0.004(2) 0.015(2) 0.028(3) C2S 0.039(2) 0.054(3) 0.0210(19) -0.0041(17) 0.0078(16) -0.005(2) N1S 0.044(2) 0.055(2) 0.045(2) -0.0110(18) 0.0143(18) -0.0034(19) F7 0.026(2) 0.048(2) 0.075(3) 0.0139(18) 0.0057(17) -0.0004(14) F8 0.026(2) 0.048(2) 0.075(3) 0.0139(18) 0.0057(17) -0.0004(14) F9 0.026(2) 0.048(2) 0.075(3) 0.0139(18) 0.0057(17) -0.0004(14) F7A 0.058(2) 0.120(4) 0.107(3) 0.070(3) 0.035(2) 0.022(2) F8A 0.058(2) 0.120(4) 0.107(3) 0.070(3) 0.035(2) 0.022(2) F9A 0.058(2) 0.120(4) 0.107(3) 0.070(3) 0.035(2) 0.022(2) S3 0.0276(5) 0.0356(5) 0.0467(6) -0.0079(4) 0.0033(4) 0.0107(4) O5 0.033(2) 0.044(2) 0.044(2) -0.0096(19) 0.0020(19) 0.0077(19) O6 0.033(2) 0.044(2) 0.044(2) -0.0096(19) 0.0020(19) 0.0077(19) O5A 0.057(4) 0.042(3) 0.043(3) -0.005(3) -0.006(3) 0.011(3) O6A 0.027(3) 0.020(3) 0.083(5) 0.011(3) 0.009(4) 0.005(2) C21 0.032(2) 0.042(3) 0.077(4) 0.021(3) -0.003(2) 0.0090(19) N5 0.024(3) 0.025(3) 0.058(4) -0.018(3) 0.012(3) -0.002(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.335(4) . ? C1 C2 1.398(5) . ? C2 C3 1.369(5) . ? C3 C4 1.402(5) . ? C4 C12 1.401(4) . ? C4 C5 1.434(5) . ? C5 C6 1.355(5) . ? C6 C7 1.434(5) . ? C7 C8 1.408(5) . ? C7 C11 1.397(5) . ? C8 C9 1.373(5) . ? C9 C10 1.394(5) . ? C10 N2 1.335(4) . ? C11 N2 1.366(4) . ? C11 C12 1.419(4) . ? C12 N1 1.362(4) . ? C13 N3 1.331(4) . ? C13 C14 1.400(5) . ? C14 C15 1.371(5) . ? C15 C16 1.407(5) . ? C16 C18 1.404(5) . ? C16 C17 1.430(5) . ? C17 C17 1.364(7) 2_655 ? C18 N3 1.364(4) . ? C18 C18 1.409(6) 2_655 ? C19 F3 1.307(5) . ? C19 F2 1.314(5) . ? C19 F1 1.320(5) . ? C19 S1 1.835(4) . ? C20 F5 1.322(5) . ? C20 F6 1.328(5) . ? C20 F4 1.330(5) . ? C20 S2 1.831(4) . ? N1 Fe1 1.975(3) . ? N2 Fe1 1.971(3) . ? N3 Fe1 1.970(3) . ? N4 S2 1.580(3) . ? N4 S1 1.577(3) . ? O1 S1 1.428(2) . ? O2 S1 1.431(2) . ? O3 S2 1.424(3) . ? O4 S2 1.425(2) . ? Fe1 N3 1.970(3) 2_655 ? Fe1 N2 1.971(3) 2_655 ? Fe1 N1 1.975(3) 2_655 ? C1S C2S 1.448(7) . ? C2S N1S 1.137(6) . ? F7 C21 1.345(7) . ? F8 C21 1.253(8) . ? F9 C21 1.336(7) . ? F7A C21 1.379(7) . ? F8A C21 1.443(8) . ? F9A C21 1.315(8) . ? S3 O5 1.350(6) . ? S3 O5A 1.434(6) . ? S3 O6 1.461(6) . ? S3 O6A 1.471(6) . ? S3 N5 1.559(6) . ? S3 N5 1.650(6) 5_675 ? S3 C21 1.783(5) . ? O5 N5 1.640(9) 5_675 ? O5A N5 1.587(9) . ? N5 O5 1.640(9) 5_675 ? N5 S3 1.650(6) 5_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.7(3) . . ? C3 C2 C1 120.1(3) . . ? C2 C3 C4 119.7(3) . . ? C12 C4 C3 116.9(3) . . ? C12 C4 C5 118.3(3) . . ? C3 C4 C5 124.7(3) . . ? C6 C5 C4 121.1(3) . . ? C5 C6 C7 121.2(3) . . ? C8 C7 C11 116.8(3) . . ? C8 C7 C6 124.8(3) . . ? C11 C7 C6 118.4(3) . . ? C9 C8 C7 119.6(3) . . ? C8 C9 C10 119.9(3) . . ? N2 C10 C9 122.2(3) . . ? N2 C11 C7 123.6(3) . . ? N2 C11 C12 115.9(3) . . ? C7 C11 C12 120.5(3) . . ? N1 C12 C4 123.3(3) . . ? N1 C12 C11 116.2(3) . . ? C4 C12 C11 120.5(3) . . ? N3 C13 C14 121.5(3) . . ? C15 C14 C13 120.3(3) . . ? C14 C15 C16 119.4(3) . . ? C15 C16 C18 117.0(3) . . ? C15 C16 C17 125.1(3) . . ? C18 C16 C17 117.9(3) . . ? C17 C17 C16 121.3(2) 2_655 . ? N3 C18 C18 116.16(17) . 2_655 ? N3 C18 C16 123.0(3) . . ? C18 C18 C16 120.85(19) 2_655 . ? F3 C19 F2 108.8(4) . . ? F3 C19 F1 107.5(4) . . ? F2 C19 F1 106.4(3) . . ? F3 C19 S1 112.1(3) . . ? F2 C19 S1 112.1(3) . . ? F1 C19 S1 109.7(3) . . ? F5 C20 F6 109.0(3) . . ? F5 C20 F4 108.7(3) . . ? F6 C20 F4 108.7(3) . . ? F5 C20 S2 109.1(3) . . ? F6 C20 S2 111.1(3) . . ? F4 C20 S2 110.3(3) . . ? C1 N1 C12 118.3(3) . . ? C1 N1 Fe1 129.4(2) . . ? C12 N1 Fe1 112.2(2) . . ? C10 N2 C11 117.9(3) . . ? C10 N2 Fe1 129.6(2) . . ? C11 N2 Fe1 112.4(2) . . ? C13 N3 C18 118.7(3) . . ? C13 N3 Fe1 128.9(2) . . ? C18 N3 Fe1 112.3(2) . . ? S2 N4 S1 124.60(18) . . ? O1 S1 O2 118.18(15) . . ? O1 S1 N4 116.64(15) . . ? O2 S1 N4 107.32(15) . . ? O1 S1 C19 104.19(16) . . ? O2 S1 C19 104.37(16) . . ? N4 S1 C19 104.45(17) . . ? O3 S2 O4 119.00(15) . . ? O3 S2 N4 116.40(15) . . ? O4 S2 N4 108.80(15) . . ? O3 S2 C20 105.00(18) . . ? O4 S2 C20 103.23(17) . . ? N4 S2 C20 101.94(17) . . ? N3 Fe1 N3 83.06(15) . 2_655 ? N3 Fe1 N2 94.81(11) . . ? N3 Fe1 N2 176.69(10) 2_655 . ? N3 Fe1 N2 176.69(10) . 2_655 ? N3 Fe1 N2 94.81(11) 2_655 2_655 ? N2 Fe1 N2 87.43(15) . 2_655 ? N3 Fe1 N1 88.70(10) . . ? N3 Fe1 N1 94.26(10) 2_655 . ? N2 Fe1 N1 83.14(10) . . ? N2 Fe1 N1 94.00(10) 2_655 . ? N3 Fe1 N1 94.26(10) . 2_655 ? N3 Fe1 N1 88.70(10) 2_655 2_655 ? N2 Fe1 N1 94.00(10) . 2_655 ? N2 Fe1 N1 83.14(10) 2_655 2_655 ? N1 Fe1 N1 176.06(15) . 2_655 ? N1S C2S C1S 179.0(5) . . ? O5 S3 O5A 140.0(4) . . ? O5 S3 O6 121.4(4) . . ? O5A S3 O6A 114.8(4) . . ? O6 S3 O6A 82.7(4) . . ? O5 S3 N5 122.9(4) . . ? O5A S3 N5 63.9(3) . . ? O6 S3 N5 108.1(3) . . ? O6A S3 N5 152.3(4) . . ? O5 S3 N5 65.4(3) . 5_675 ? O5A S3 N5 112.3(3) . 5_675 ? O6 S3 N5 156.5(4) . 5_675 ? O6A S3 N5 102.2(4) . 5_675 ? N5 S3 N5 58.1(4) . 5_675 ? O5 S3 C21 105.2(3) . . ? O5A S3 C21 113.4(3) . . ? O6 S3 C21 94.9(3) . . ? O6A S3 C21 108.1(3) . . ? N5 S3 C21 96.6(3) . . ? N5 S3 C21 105.1(3) 5_675 . ? S3 O5 N5 66.2(3) . 5_675 ? S3 O5A N5 61.9(3) . . ? F8 C21 F9A 124.5(6) . . ? F8 C21 F9 114.4(5) . . ? F9A C21 F9 70.5(4) . . ? F8 C21 F7 114.6(5) . . ? F9 C21 F7 108.6(5) . . ? F8 C21 F7A 62.2(5) . . ? F9A C21 F7A 104.7(5) . . ? F9 C21 F7A 52.6(4) . . ? F7 C21 F7A 138.1(5) . . ? F9A C21 F8A 100.0(5) . . ? F9 C21 F8A 140.8(6) . . ? F7 C21 F8A 76.6(4) . . ? F7A C21 F8A 96.8(5) . . ? F8 C21 S3 109.6(4) . . ? F9A C21 S3 123.3(5) . . ? F9 C21 S3 103.5(4) . . ? F7 C21 S3 105.2(4) . . ? F7A C21 S3 115.2(4) . . ? F8A C21 S3 112.7(4) . . ? S3 N5 O5A 54.2(3) . . ? S3 N5 O5 168.2(5) . 5_675 ? O5A N5 O5 137.5(5) . 5_675 ? S3 N5 S3 121.9(4) . 5_675 ? O5A N5 S3 149.6(5) . 5_675 ? O5 N5 S3 48.5(3) 5_675 5_675 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.2(5) . . . . ? C1 C2 C3 C4 -0.4(5) . . . . ? C2 C3 C4 C12 0.4(5) . . . . ? C2 C3 C4 C5 179.2(3) . . . . ? C12 C4 C5 C6 1.1(4) . . . . ? C3 C4 C5 C6 -177.8(3) . . . . ? C4 C5 C6 C7 -1.4(5) . . . . ? C5 C6 C7 C8 -179.5(3) . . . . ? C5 C6 C7 C11 0.0(5) . . . . ? C11 C7 C8 C9 -0.1(5) . . . . ? C6 C7 C8 C9 179.4(3) . . . . ? C7 C8 C9 C10 0.2(5) . . . . ? C8 C9 C10 N2 0.0(5) . . . . ? C8 C7 C11 N2 -0.3(5) . . . . ? C6 C7 C11 N2 -179.8(3) . . . . ? C8 C7 C11 C12 -178.7(3) . . . . ? C6 C7 C11 C12 1.8(4) . . . . ? C3 C4 C12 N1 0.2(4) . . . . ? C5 C4 C12 N1 -178.7(3) . . . . ? C3 C4 C12 C11 179.6(3) . . . . ? C5 C4 C12 C11 0.7(4) . . . . ? N2 C11 C12 N1 -1.3(4) . . . . ? C7 C11 C12 N1 177.3(3) . . . . ? N2 C11 C12 C4 179.3(3) . . . . ? C7 C11 C12 C4 -2.1(4) . . . . ? N3 C13 C14 C15 -1.2(5) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C14 C15 C16 C18 1.6(5) . . . . ? C14 C15 C16 C17 179.9(3) . . . . ? C15 C16 C17 C17 -178.9(4) . . . 2_655 ? C18 C16 C17 C17 -0.6(6) . . . 2_655 ? C15 C16 C18 N3 -1.4(4) . . . . ? C17 C16 C18 N3 -179.8(3) . . . . ? C15 C16 C18 C18 178.9(3) . . . 2_655 ? C17 C16 C18 C18 0.4(5) . . . 2_655 ? C2 C1 N1 C12 0.8(5) . . . . ? C2 C1 N1 Fe1 -178.3(2) . . . . ? C4 C12 N1 C1 -0.8(4) . . . . ? C11 C12 N1 C1 179.8(3) . . . . ? C4 C12 N1 Fe1 178.5(2) . . . . ? C11 C12 N1 Fe1 -0.9(3) . . . . ? C9 C10 N2 C11 -0.3(5) . . . . ? C9 C10 N2 Fe1 175.1(3) . . . . ? C7 C11 N2 C10 0.5(4) . . . . ? C12 C11 N2 C10 179.0(3) . . . . ? C7 C11 N2 Fe1 -175.7(2) . . . . ? C12 C11 N2 Fe1 2.8(3) . . . . ? C14 C13 N3 C18 1.4(4) . . . . ? C14 C13 N3 Fe1 -178.9(2) . . . . ? C18 C18 N3 C13 179.7(3) 2_655 . . . ? C16 C18 N3 C13 -0.1(4) . . . . ? C18 C18 N3 Fe1 -0.1(4) 2_655 . . . ? C16 C18 N3 Fe1 -179.8(2) . . . . ? S2 N4 S1 O1 -37.9(3) . . . . ? S2 N4 S1 O2 -173.1(2) . . . . ? S2 N4 S1 C19 76.5(3) . . . . ? F3 C19 S1 O1 175.7(3) . . . . ? F2 C19 S1 O1 53.0(3) . . . . ? F1 C19 S1 O1 -64.9(3) . . . . ? F3 C19 S1 O2 -59.7(3) . . . . ? F2 C19 S1 O2 177.6(3) . . . . ? F1 C19 S1 O2 59.7(3) . . . . ? F3 C19 S1 N4 52.9(3) . . . . ? F2 C19 S1 N4 -69.8(3) . . . . ? F1 C19 S1 N4 172.2(3) . . . . ? S1 N4 S2 O3 -8.0(3) . . . . ? S1 N4 S2 O4 -145.8(2) . . . . ? S1 N4 S2 C20 105.6(2) . . . . ? F5 C20 S2 O3 -64.3(3) . . . . ? F6 C20 S2 O3 175.6(3) . . . . ? F4 C20 S2 O3 55.0(3) . . . . ? F5 C20 S2 O4 61.0(3) . . . . ? F6 C20 S2 O4 -59.1(3) . . . . ? F4 C20 S2 O4 -179.6(3) . . . . ? F5 C20 S2 N4 173.9(3) . . . . ? F6 C20 S2 N4 53.8(3) . . . . ? F4 C20 S2 N4 -66.8(3) . . . . ? C13 N3 Fe1 N1 -85.2(3) . . . . ? C18 N3 Fe1 N1 94.5(2) . . . . ? C13 N3 Fe1 N1 92.2(3) . . . 2_655 ? C18 N3 Fe1 N1 -88.1(2) . . . 2_655 ? C10 N2 Fe1 N2 -83.8(3) . . . 2_655 ? C11 N2 Fe1 N2 91.8(2) . . . 2_655 ? C10 N2 Fe1 N1 -178.2(3) . . . . ? C11 N2 Fe1 N1 -2.6(2) . . . . ? C10 N2 Fe1 N1 -0.9(3) . . . 2_655 ? C11 N2 Fe1 N1 174.7(2) . . . 2_655 ? C1 N1 Fe1 N3 -83.9(3) . . . . ? C12 N1 Fe1 N3 96.9(2) . . . . ? C1 N1 Fe1 N3 -0.9(3) . . . 2_655 ? C12 N1 Fe1 N3 179.9(2) . . . 2_655 ? C1 N1 Fe1 N2 -178.9(3) . . . . ? C12 N1 Fe1 N2 1.9(2) . . . . ? C1 N1 Fe1 N2 94.2(3) . . . 2_655 ? C12 N1 Fe1 N2 -85.0(2) . . . 2_655 ? O5A S3 O5 N5 -95.9(6) . . . 5_675 ? O6 S3 O5 N5 -154.5(4) . . . 5_675 ? O6A S3 O5 N5 -160.0(7) . . . 5_675 ? N5 S3 O5 N5 -8.5(7) . . . 5_675 ? C21 S3 O5 N5 99.9(3) . . . 5_675 ? O5 S3 O5A N5 110.9(6) . . . . ? O6 S3 O5A N5 -159.5(6) . . . . ? O6A S3 O5A N5 149.3(4) . . . . ? N5 S3 O5A N5 33.1(6) 5_675 . . . ? C21 S3 O5A N5 -85.8(4) . . . . ? O5 S3 C21 F8 -11.4(5) . . . . ? O5A S3 C21 F8 179.6(4) . . . . ? O6 S3 C21 F8 -135.9(4) . . . . ? O6A S3 C21 F8 -51.9(5) . . . . ? N5 S3 C21 F8 115.3(4) . . . . ? N5 S3 C21 F8 56.6(4) 5_675 . . . ? O5 S3 C21 F9A -173.6(6) . . . . ? O5A S3 C21 F9A 17.4(6) . . . . ? O6 S3 C21 F9A 61.9(6) . . . . ? O6A S3 C21 F9A 145.9(6) . . . . ? N5 S3 C21 F9A -46.9(6) . . . . ? N5 S3 C21 F9A -105.6(5) 5_675 . . . ? O5 S3 C21 F9 111.0(5) . . . . ? O5A S3 C21 F9 -58.0(5) . . . . ? O6 S3 C21 F9 -13.4(4) . . . . ? O6A S3 C21 F9 70.5(5) . . . . ? N5 S3 C21 F9 -122.3(4) . . . . ? N5 S3 C21 F9 179.0(4) 5_675 . . . ? O5 S3 C21 F7 -135.1(5) . . . . ? O5A S3 C21 F7 55.9(5) . . . . ? O6 S3 C21 F7 100.4(5) . . . . ? O6A S3 C21 F7 -175.6(5) . . . . ? N5 S3 C21 F7 -8.4(5) . . . . ? N5 S3 C21 F7 -67.1(5) 5_675 . . . ? O5 S3 C21 F7A 56.3(6) . . . . ? O5A S3 C21 F7A -112.7(6) . . . . ? O6 S3 C21 F7A -68.2(6) . . . . ? O6A S3 C21 F7A 15.8(6) . . . . ? N5 S3 C21 F7A -177.0(5) . . . . ? N5 S3 C21 F7A 124.3(5) 5_675 . . . ? O5 S3 C21 F8A -53.6(5) . . . . ? O5A S3 C21 F8A 137.4(4) . . . . ? O6 S3 C21 F8A -178.0(4) . . . . ? O6A S3 C21 F8A -94.1(5) . . . . ? N5 S3 C21 F8A 73.1(4) . . . . ? N5 S3 C21 F8A 14.4(5) 5_675 . . . ? O5 S3 N5 O5A -134.3(5) . . . . ? O6 S3 N5 O5A 15.5(5) . . . . ? O6A S3 N5 O5A -94.1(9) . . . . ? N5 S3 N5 O5A -143.4(7) 5_675 . . . ? C21 S3 N5 O5A 112.8(4) . . . . ? O5 S3 N5 O5 42(3) . . . 5_675 ? O5A S3 N5 O5 176(3) . . . 5_675 ? O6 S3 N5 O5 -168(3) . . . 5_675 ? O6A S3 N5 O5 82(3) . . . 5_675 ? N5 S3 N5 O5 33(2) 5_675 . . 5_675 ? C21 S3 N5 O5 -71(3) . . . 5_675 ? O5 S3 N5 S3 9.2(7) . . . 5_675 ? O5A S3 N5 S3 143.4(7) . . . 5_675 ? O6 S3 N5 S3 159.0(5) . . . 5_675 ? O6A S3 N5 S3 49.4(11) . . . 5_675 ? N5 S3 N5 S3 0.0 5_675 . . 5_675 ? C21 S3 N5 S3 -103.7(5) . . . 5_675 ? S3 O5A N5 O5 -178.8(8) . . . 5_675 ? S3 O5A N5 S3 -93.4(9) . . . 5_675 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 'ACTA 50' _diffrn_measured_fraction_theta_full 'ACTA 50' _refine_diff_density_max 1.037 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.080