data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr George Britovsek' _publ_contact_author_address ; Department of Chemistry Imperial College London Exhibition Road South Kensington London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email G.BRITOVSEK@IMPERIAL.AC.UK _publ_section_title ; Synthesis of Iron(II), Manganese(II) Cobalt(II) and Ruthenium(II) Complexes Containing Tridentate Nitrogen Ligands and their Application in the Catalytic Oxidation of Alkanes ; loop_ _publ_author_name 'George Britovsek' 'Jason England' 'Stefan K. Spitzmesser' 'Andrew J. P. White' 'David J. Williams' data_[Fe(1)(OTf)2] _database_code_depnum_ccdc_archive 'CCDC 246556' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Fe(1)(OTf)2]' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H45 N3 O6 F6 S2 Cl2 Fe' _chemical_formula_weight 920.62 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 26.783(3) _cell_length_b 9.0389(11) _cell_length_c 17.712(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4288.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 3.95 _cell_measurement_theta_max 12.49 _exptl_crystal_description blocks _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.67 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method ? _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.6267 _exptl_absorpt_correction_T_max 0.6920 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 42.75 _diffrn_reflns_number 3864 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3864 _reflns_number_observed 2693 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 311 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 3553 _refine_ls_number_parameters 506 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_obs 0.0492 _refine_ls_wR_factor_all 0.1231 _refine_ls_wR_factor_obs 0.1045 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.050 _refine_ls_restrained_S_obs 1.101 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.86722(3) 0.25139(13) 0.92826(6) 0.0394(2) Uani 1 d . . N1 N 0.8394(2) 0.0389(6) 0.9469(3) 0.0389(13) Uani 1 d . . C2 C 0.8538(3) -0.0334(8) 1.0089(4) 0.044(2) Uani 1 d . . C3 C 0.8268(3) -0.1551(9) 1.0337(4) 0.054(2) Uani 1 d . . H3A H 0.8371(3) -0.2076(9) 1.0761(4) 0.065 Uiso 1 calc R . C4 C 0.7849(3) -0.1970(10) 0.9949(5) 0.064(2) Uani 1 d . . H4A H 0.7657(3) -0.2759(10) 1.0119(5) 0.076 Uiso 1 calc R . C5 C 0.7715(3) -0.1219(7) 0.9309(5) 0.052(2) Uani 1 d . . H5A H 0.7431(3) -0.1494(7) 0.9041(5) 0.062 Uiso 1 calc R . C6 C 0.8005(2) -0.0050(7) 0.9068(4) 0.040(2) Uani 1 d . . C7 C 0.8996(3) 0.0276(9) 1.0436(4) 0.049(2) Uani 1 d . . N7 N 0.9153(2) 0.1504(7) 1.0163(4) 0.0481(14) Uani 1 d . . C8 C 0.9259(4) -0.0623(11) 1.1032(6) 0.077(3) Uani 1 d . . H8A H 0.9229(4) -0.1656(11) 1.0913(6) 0.116 Uiso 1 d R . H8B H 0.9109(4) -0.0434(11) 1.1515(6) 0.116 Uiso 1 d R . H8C H 0.9605(4) -0.0353(11) 1.1047(6) 0.116 Uiso 1 d R . C9 C 0.7939(3) 0.0798(9) 0.8346(4) 0.044(2) Uani 1 d . . N9 N 0.8197(2) 0.1965(6) 0.8280(3) 0.0395(13) Uani 1 d . . C10 C 0.7592(4) 0.0145(11) 0.7760(5) 0.070(2) Uani 1 d . . H10A H 0.7254(4) 0.0208(11) 0.7936(5) 0.105 Uiso 1 d R . H10B H 0.7678(4) -0.0873(11) 0.7676(5) 0.105 Uiso 1 d R . H10C H 0.7624(4) 0.0685(11) 0.7296(5) 0.105 Uiso 1 d R . C11 C 0.9631(3) 0.2091(8) 1.0422(4) 0.051(2) Uani 1 d . . C12 C 0.9650(3) 0.3052(11) 1.1042(5) 0.064(2) Uani 1 d . . C13 C 1.0120(4) 0.3574(12) 1.1247(5) 0.072(2) Uani 1 d . . H13A H 1.0147(4) 0.4195(12) 1.1664(5) 0.086 Uiso 1 calc R . C14 C 1.0546(4) 0.3203(12) 1.0855(7) 0.084(3) Uani 1 d . . H14A H 1.0855(4) 0.3576(12) 1.1001(7) 0.101 Uiso 1 calc R . C15 C 1.0509(3) 0.2283(14) 1.0251(6) 0.081(3) Uani 1 d . . H15A H 1.0798(3) 0.2016(14) 0.9994(6) 0.097 Uiso 1 calc R . C16 C 1.0049(3) 0.1721(12) 0.9999(5) 0.066(2) Uani 1 d . . C17 C 0.9190(4) 0.3497(15) 1.1477(6) 0.085(3) Uani 1 d . . H17A H 0.8897(4) 0.3176(15) 1.1189(6) 0.102 Uiso 1 calc R . C18 C 0.9152(7) 0.5149(16) 1.1595(8) 0.120(5) Uani 1 d . . H18A H 0.8854(7) 0.5370(16) 1.1874(8) 0.180 Uiso 1 calc R . H18B H 0.9140(7) 0.5637(16) 1.1114(8) 0.180 Uiso 1 calc R . H18C H 0.9437(7) 0.5490(16) 1.1872(8) 0.180 Uiso 1 calc R . C19 C 0.9178(8) 0.2704(22) 1.2254(9) 0.158(7) Uani 1 d . . H19A H 0.8884(8) 0.2996(22) 1.2525(9) 0.237 Uiso 1 calc R . H19B H 0.9469(8) 0.2972(22) 1.2539(9) 0.237 Uiso 1 calc R . H19C H 0.9174(8) 0.1652(22) 1.2178(9) 0.237 Uiso 1 calc R . C20 C 1.0030(3) 0.0734(13) 0.9304(9) 0.097(4) Uani 1 d . . H20A H 0.9684(3) 0.0705(13) 0.9128(9) 0.117 Uiso 1 calc R . C21 C 1.0179(7) -0.0836(17) 0.9527(10) 0.153(8) Uani 1 d . . H21A H 0.9973(7) -0.1165(17) 0.9937(10) 0.230 Uiso 1 calc R . H21B H 1.0523(7) -0.0846(17) 0.9682(10) 0.230 Uiso 1 calc R . H21C H 1.0136(7) -0.1484(17) 0.9102(10) 0.230 Uiso 1 calc R . C22 C 1.0351(7) 0.1282(22) 0.8657(8) 0.140(6) Uani 1 d . . H22A H 1.0323(7) 0.0613(22) 0.8238(8) 0.211 Uiso 1 calc R . H22B H 1.0693(7) 0.1333(22) 0.8817(8) 0.211 Uiso 1 calc R . H22C H 1.0241(7) 0.2249(22) 0.8506(8) 0.211 Uiso 1 calc R . C23 C 0.8190(3) 0.2804(8) 0.7586(4) 0.042(2) Uani 1 d . . C24 C 0.8595(3) 0.2627(10) 0.7089(3) 0.052(2) Uani 1 d . . C25 C 0.8594(4) 0.3417(13) 0.6417(5) 0.076(3) Uani 1 d . . H25A H 0.8860(4) 0.3321(13) 0.6083(5) 0.091 Uiso 1 calc R . C26 C 0.8204(4) 0.4338(13) 0.6242(5) 0.079(3) Uani 1 d . . H26A H 0.8204(4) 0.4854(13) 0.5787(5) 0.095 Uiso 1 calc R . C27 C 0.7815(4) 0.4497(11) 0.6732(5) 0.070(2) Uani 1 d . . H27A H 0.7555(4) 0.5128(11) 0.6604(5) 0.084 Uiso 1 calc R . C28 C 0.7795(3) 0.3754(10) 0.7414(4) 0.059(2) Uani 1 d . . C29 C 0.9022(3) 0.1580(12) 0.7257(5) 0.067(2) Uani 1 d . . H29A H 0.9026(3) 0.1395(12) 0.7802(5) 0.080 Uiso 1 calc R . C30 C 0.9527(4) 0.2249(18) 0.7039(8) 0.106(4) Uani 1 d . . H30A H 0.9789(4) 0.1557(18) 0.7152(8) 0.159 Uiso 1 calc R . H30B H 0.9580(4) 0.3145(18) 0.7319(8) 0.159 Uiso 1 calc R . H30C H 0.9530(4) 0.2466(18) 0.6508(8) 0.159 Uiso 1 calc R . C31 C 0.8946(6) 0.0090(14) 0.6856(9) 0.110(4) Uani 1 d . . H31A H 0.9221(6) -0.0555(14) 0.6971(9) 0.165 Uiso 1 calc R . H31B H 0.8929(6) 0.0246(14) 0.6321(9) 0.165 Uiso 1 calc R . H31C H 0.8641(6) -0.0354(14) 0.7028(9) 0.165 Uiso 1 calc R . C32 C 0.7356(4) 0.4013(12) 0.7945(5) 0.068(2) Uani 1 d . . H32A H 0.7384(4) 0.3316(12) 0.8367(5) 0.082 Uiso 1 calc R . C33 C 0.6858(4) 0.3750(18) 0.7557(8) 0.107(5) Uani 1 d . . H33A H 0.6848(4) 0.2759(18) 0.7362(8) 0.161 Uiso 1 calc R . H33B H 0.6820(4) 0.4440(18) 0.7149(8) 0.161 Uiso 1 calc R . H33C H 0.6592(4) 0.3884(18) 0.7913(8) 0.161 Uiso 1 calc R . C34 C 0.7384(5) 0.5558(14) 0.8257(9) 0.110(4) Uani 1 d . . H34A H 0.7701(5) 0.5700(14) 0.8500(9) 0.165 Uiso 1 calc R . H34B H 0.7121(5) 0.5702(14) 0.8618(9) 0.165 Uiso 1 calc R . H34C H 0.7348(5) 0.6258(14) 0.7853(9) 0.165 Uiso 1 calc R . S1 S 0.78875(8) 0.3595(3) 1.05840(12) 0.0579(5) Uani 1 d . . O11 O 0.8134(2) 0.3722(7) 0.9860(3) 0.0637(15) Uani 1 d . . O12 O 0.7899(3) 0.4935(8) 1.1008(4) 0.085(2) Uani 1 d . . O13 O 0.8006(3) 0.2255(8) 1.0978(4) 0.081(2) Uani 1 d . . C35 C 0.7241(4) 0.3367(13) 1.0321(6) 0.079(3) Uani 1 d . . F11 F 0.6964(3) 0.3107(9) 1.0914(5) 0.118(3) Uani 1 d . . F12 F 0.7181(3) 0.2240(10) 0.9868(5) 0.123(3) Uani 1 d . . F13 F 0.7066(3) 0.4561(11) 0.9977(5) 0.132(3) Uani 1 d . . S2 S 0.93821(10) 0.5391(3) 0.8972(2) 0.0763(7) Uani 1 d . . O21 O 0.9127(3) 0.4003(7) 0.8842(4) 0.076(2) Uani 1 d . . O22 O 0.9856(3) 0.5401(11) 0.8681(9) 0.148(5) Uani 1 d . . O23 O 0.9305(6) 0.5974(12) 0.9696(5) 0.155(5) Uani 1 d . . C36 C 0.9048(4) 0.6637(11) 0.8391(6) 0.076(3) Uani 1 d . . F21 F 0.9221(5) 0.7959(9) 0.8415(7) 0.183(6) Uani 1 d . . F22 F 0.8577(4) 0.6666(15) 0.8542(7) 0.184(5) Uani 1 d . . F23 F 0.9042(4) 0.6197(10) 0.7668(4) 0.126(3) Uani 1 d . . C40 C 0.6003(4) -0.0741(19) 0.9216(9) 0.129(5) Uani 1 d . . H40A H 0.5880(4) -0.0415(19) 0.9704(9) 0.154 Uiso 1 calc R . H40B H 0.5717(4) -0.0988(19) 0.8905(9) 0.154 Uiso 1 calc R . Cl1 Cl 0.63629(13) -0.2284(7) 0.9337(4) 0.149(2) Uani 1 d . . Cl2 Cl 0.6332(2) 0.0701(7) 0.8794(4) 0.172(2) Uani 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 Fe 0.0445(4) 0.0322(3) 0.0415(3) 0.0032(5) -0.0036(6) -0.0059(5) N1 0.046(3) 0.029(3) 0.042(3) 0.002(2) -0.002(2) -0.003(2) C2 0.047(4) 0.041(4) 0.043(3) 0.006(3) 0.004(3) -0.001(3) C3 0.072(5) 0.040(4) 0.050(4) 0.009(3) -0.003(3) -0.009(4) C4 0.068(5) 0.047(4) 0.076(5) 0.006(4) 0.009(4) -0.022(4) C5 0.055(4) 0.040(3) 0.059(4) 0.001(5) -0.007(4) -0.012(3) C6 0.040(3) 0.032(3) 0.047(4) -0.008(3) 0.005(3) -0.005(3) C7 0.061(4) 0.045(4) 0.040(3) -0.003(3) -0.009(3) 0.004(4) N7 0.052(3) 0.047(4) 0.046(3) -0.001(3) -0.009(3) -0.002(3) C8 0.086(6) 0.062(6) 0.084(6) 0.027(5) -0.028(5) -0.002(5) C9 0.041(3) 0.054(4) 0.038(3) -0.010(3) -0.009(3) 0.004(3) N9 0.044(3) 0.040(3) 0.035(3) 0.000(2) -0.001(2) -0.002(2) C10 0.088(6) 0.059(5) 0.064(5) -0.003(5) -0.021(5) -0.011(5) C11 0.055(4) 0.047(5) 0.049(4) 0.005(3) -0.020(3) -0.004(3) C12 0.068(5) 0.063(5) 0.060(5) -0.004(4) -0.021(4) -0.003(4) C13 0.074(6) 0.070(6) 0.071(5) -0.015(5) -0.023(5) -0.006(5) C14 0.072(6) 0.078(6) 0.101(7) 0.007(6) -0.035(6) -0.022(5) C15 0.046(4) 0.105(9) 0.091(6) -0.002(7) -0.007(4) -0.016(5) C16 0.054(5) 0.079(6) 0.065(5) -0.001(5) -0.012(4) 0.006(5) C17 0.068(6) 0.101(8) 0.085(6) -0.021(7) -0.013(5) -0.007(6) C18 0.167(14) 0.101(10) 0.093(8) -0.003(8) 0.001(9) 0.028(10) C19 0.206(18) 0.145(16) 0.123(11) 0.000(12) 0.077(12) -0.018(15) C20 0.047(4) 0.112(8) 0.133(9) -0.049(9) 0.006(7) -0.007(5) C21 0.215(19) 0.096(10) 0.148(16) -0.034(10) 0.048(13) -0.031(12) C22 0.160(14) 0.166(17) 0.096(9) -0.032(11) 0.033(10) 0.005(13) C23 0.055(4) 0.038(4) 0.034(3) -0.003(3) -0.009(3) -0.003(3) C24 0.064(4) 0.052(4) 0.040(3) -0.003(4) 0.004(3) -0.002(4) C25 0.074(5) 0.096(7) 0.058(4) 0.027(5) 0.004(4) -0.003(6) C26 0.084(6) 0.094(7) 0.058(5) 0.037(5) 0.001(4) 0.001(6) C27 0.079(6) 0.062(5) 0.069(5) 0.019(5) -0.022(5) 0.009(5) C28 0.069(5) 0.055(5) 0.052(4) -0.004(4) -0.018(4) 0.003(4) C29 0.066(5) 0.083(7) 0.052(4) 0.008(5) 0.013(4) 0.009(5) C30 0.078(6) 0.134(12) 0.106(8) 0.031(9) 0.025(6) 0.014(7) C31 0.129(10) 0.077(8) 0.125(10) -0.010(8) -0.020(9) 0.028(8) C32 0.072(6) 0.073(6) 0.059(5) 0.003(5) -0.006(4) 0.022(5) C33 0.055(6) 0.148(13) 0.119(9) 0.035(10) -0.006(6) 0.008(7) C34 0.115(10) 0.084(8) 0.131(11) -0.031(8) 0.025(8) 0.018(7) S1 0.0678(12) 0.0512(10) 0.0548(10) 0.0029(11) 0.0168(10) 0.0032(10) O11 0.064(3) 0.062(4) 0.065(3) 0.001(3) 0.016(3) 0.006(3) O12 0.111(6) 0.070(4) 0.072(4) -0.016(4) 0.024(4) -0.005(4) O13 0.084(4) 0.073(5) 0.084(4) 0.024(4) 0.017(4) 0.009(4) C35 0.085(7) 0.075(7) 0.078(6) 0.007(6) 0.019(5) 0.013(6) F11 0.080(4) 0.129(6) 0.145(6) 0.020(5) 0.052(4) 0.002(4) F12 0.103(5) 0.141(7) 0.124(6) -0.029(6) -0.008(4) -0.036(5) F13 0.088(4) 0.148(7) 0.161(8) 0.058(6) 0.009(5) 0.034(5) S2 0.0746(14) 0.0588(13) 0.096(2) 0.0205(14) -0.0184(12) -0.0246(12) O21 0.086(4) 0.054(4) 0.088(4) 0.016(4) 0.009(4) -0.028(3) O22 0.052(4) 0.105(7) 0.286(15) 0.047(9) -0.008(6) -0.016(4) O23 0.282(15) 0.109(8) 0.075(5) -0.003(5) -0.054(8) -0.037(9) C36 0.097(7) 0.052(6) 0.078(6) 0.000(5) 0.013(5) 0.005(5) F21 0.262(13) 0.064(5) 0.225(11) 0.042(6) -0.100(11) -0.033(6) F22 0.119(7) 0.222(12) 0.212(11) 0.018(10) 0.029(7) 0.090(8) F23 0.184(8) 0.115(6) 0.080(4) 0.019(5) -0.006(5) 0.002(6) C40 0.079(6) 0.190(15) 0.117(9) -0.054(12) 0.023(8) -0.012(8) Cl1 0.091(2) 0.190(4) 0.167(3) -0.014(4) 0.000(3) 0.011(3) Cl2 0.125(3) 0.174(5) 0.217(5) -0.034(4) 0.030(4) -0.008(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 Fe O21 1.976(6) . ? Fe O11 2.077(6) . ? Fe N1 2.087(5) . ? Fe N7 2.219(6) . ? Fe N9 2.241(5) . ? N1 C6 1.321(8) . ? N1 C2 1.335(9) . ? C2 C3 1.387(11) . ? C2 C7 1.478(10) . ? C3 C4 1.370(12) . ? C4 C5 1.369(13) . ? C5 C6 1.379(9) . ? C6 C9 1.501(10) . ? C7 N7 1.282(10) . ? C7 C8 1.507(11) . ? N7 C11 1.459(9) . ? C9 N9 1.265(9) . ? C9 C10 1.513(11) . ? N9 C23 1.445(9) . ? C11 C16 1.388(12) . ? C11 C12 1.401(12) . ? C12 C13 1.392(13) . ? C12 C17 1.508(14) . ? C13 C14 1.38(2) . ? C14 C15 1.36(2) . ? C15 C16 1.405(12) . ? C16 C20 1.52(2) . ? C17 C18 1.51(2) . ? C17 C19 1.55(2) . ? C20 C22 1.52(2) . ? C20 C21 1.53(2) . ? C23 C28 1.395(11) . ? C23 C24 1.406(10) . ? C24 C25 1.388(12) . ? C24 C29 1.514(12) . ? C25 C26 1.371(14) . ? C26 C27 1.363(13) . ? C27 C28 1.383(12) . ? C28 C32 1.525(13) . ? C29 C30 1.532(15) . ? C29 C31 1.54(2) . ? C32 C34 1.50(2) . ? C32 C33 1.519(15) . ? S1 O12 1.425(7) . ? S1 O13 1.433(7) . ? S1 O11 1.447(6) . ? S1 C35 1.804(12) . ? C35 F12 1.307(13) . ? C35 F11 1.308(12) . ? C35 F13 1.325(13) . ? S2 O22 1.371(9) . ? S2 O23 1.401(11) . ? S2 O21 1.446(7) . ? S2 C36 1.769(11) . ? C36 F21 1.282(13) . ? C36 F22 1.291(14) . ? C36 F23 1.341(13) . ? C40 Cl1 1.71(2) . ? C40 Cl2 1.74(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Fe O11 105.3(3) . . ? O21 Fe N1 155.5(3) . . ? O11 Fe N1 99.1(2) . . ? O21 Fe N7 101.5(3) . . ? O11 Fe N7 105.9(2) . . ? N1 Fe N7 73.6(2) . . ? O21 Fe N9 100.9(3) . . ? O11 Fe N9 96.4(2) . . ? N1 Fe N9 73.6(2) . . ? N7 Fe N9 142.7(2) . . ? C6 N1 C2 121.6(6) . . ? C6 N1 Fe 118.2(4) . . ? C2 N1 Fe 118.5(5) . . ? N1 C2 C3 119.9(7) . . ? N1 C2 C7 113.5(6) . . ? C3 C2 C7 126.6(6) . . ? C4 C3 C2 119.1(7) . . ? C5 C4 C3 119.6(7) . . ? C4 C5 C6 119.3(7) . . ? N1 C6 C5 120.4(6) . . ? N1 C6 C9 113.4(6) . . ? C5 C6 C9 126.1(7) . . ? N7 C7 C2 116.0(6) . . ? N7 C7 C8 125.3(7) . . ? C2 C7 C8 118.5(7) . . ? C7 N7 C11 119.0(6) . . ? C7 N7 Fe 115.5(5) . . ? C11 N7 Fe 125.4(5) . . ? N9 C9 C6 116.1(6) . . ? N9 C9 C10 126.6(7) . . ? C6 C9 C10 117.2(7) . . ? C9 N9 C23 120.6(6) . . ? C9 N9 Fe 114.9(5) . . ? C23 N9 Fe 124.4(4) . . ? C16 C11 C12 122.8(7) . . ? C16 C11 N7 116.8(7) . . ? C12 C11 N7 120.3(7) . . ? C13 C12 C11 116.7(9) . . ? C13 C12 C17 120.9(9) . . ? C11 C12 C17 122.4(8) . . ? C14 C13 C12 122.3(9) . . ? C15 C14 C13 119.1(9) . . ? C14 C15 C16 122.4(10) . . ? C11 C16 C15 116.7(8) . . ? C11 C16 C20 123.5(8) . . ? C15 C16 C20 119.8(8) . . ? C12 C17 C18 113.0(11) . . ? C12 C17 C19 110.3(11) . . ? C18 C17 C19 109.4(12) . . ? C22 C20 C16 113.7(10) . . ? C22 C20 C21 110.6(12) . . ? C16 C20 C21 109.1(13) . . ? C28 C23 C24 121.2(7) . . ? C28 C23 N9 121.2(7) . . ? C24 C23 N9 117.5(6) . . ? C25 C24 C23 118.4(8) . . ? C25 C24 C29 119.4(7) . . ? C23 C24 C29 122.1(7) . . ? C26 C25 C24 120.6(9) . . ? C27 C26 C25 120.0(8) . . ? C26 C27 C28 122.4(8) . . ? C27 C28 C23 117.4(8) . . ? C27 C28 C32 119.6(8) . . ? C23 C28 C32 123.0(7) . . ? C24 C29 C30 111.8(9) . . ? C24 C29 C31 111.0(8) . . ? C30 C29 C31 110.3(10) . . ? C34 C32 C33 110.8(10) . . ? C34 C32 C28 109.3(9) . . ? C33 C32 C28 112.0(8) . . ? O12 S1 O13 117.2(4) . . ? O12 S1 O11 112.9(4) . . ? O13 S1 O11 113.4(4) . . ? O12 S1 C35 104.7(5) . . ? O13 S1 C35 104.0(5) . . ? O11 S1 C35 102.5(4) . . ? S1 O11 Fe 135.3(4) . . ? F12 C35 F11 106.4(10) . . ? F12 C35 F13 108.0(10) . . ? F11 C35 F13 108.3(9) . . ? F12 C35 S1 111.5(7) . . ? F11 C35 S1 110.9(8) . . ? F13 C35 S1 111.4(9) . . ? O22 S2 O23 118.5(9) . . ? O22 S2 O21 112.6(6) . . ? O23 S2 O21 113.7(6) . . ? O22 S2 C36 104.2(6) . . ? O23 S2 C36 102.6(6) . . ? O21 S2 C36 102.8(5) . . ? S2 O21 Fe 145.0(5) . . ? F21 C36 F22 109.1(12) . . ? F21 C36 F23 108.2(11) . . ? F22 C36 F23 101.1(11) . . ? F21 C36 S2 113.1(9) . . ? F22 C36 S2 112.7(9) . . ? F23 C36 S2 111.9(8) . . ? Cl1 C40 Cl2 112.3(7) . . ? _refine_diff_density_max 0.298 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.053 #===END data_[Fe(1)(OTf)(CH3CN)](SbF6) _database_code_depnum_ccdc_archive 'CCDC 246557' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Fe(1)(OTf)(CH3CN)](SbF6)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H50 N4 O3 F9 S Cl4 Fe Sb' _chemical_formula_weight 1133.28 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' 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' F F 0.0727 0.0534 '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' Cl Cl 0.3639 0.7018 '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' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.4010(10) _cell_length_b 12.6433(6) _cell_length_c 21.1155(15) _cell_angle_alpha 90.00 _cell_angle_beta 116.516(4) _cell_angle_gamma 90.00 _cell_volume 4873.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 11.13 _cell_measurement_theta_max 22.48 _exptl_crystal_description needles _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method ? _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 9.846 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.2468 _exptl_absorpt_correction_T_max 0.6825 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7437 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 60.00 _reflns_number_total 7207 _reflns_number_observed 5706 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 368 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0971P)^2^+9.8667P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00037(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6839 _refine_ls_number_parameters 596 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_obs 0.0589 _refine_ls_wR_factor_all 0.1660 _refine_ls_wR_factor_obs 0.1495 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.042 _refine_ls_restrained_S_obs 1.066 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.73071(4) 0.25441(6) 0.96258(4) 0.0195(2) Uani 1 d . . N1 N 0.7716(2) 0.2400(3) 1.0719(2) 0.0218(9) Uani 1 d . . C2 C 0.8332(3) 0.1859(4) 1.1087(3) 0.0219(11) Uani 1 d . . C3 C 0.8666(3) 0.1861(5) 1.1823(3) 0.0290(12) Uani 1 d . . H3A H 0.9104(3) 0.1473(5) 1.2083(3) 0.035 Uiso 1 calc R . C4 C 0.8349(3) 0.2440(5) 1.2165(3) 0.0330(13) Uani 1 d . . H4A H 0.8571(3) 0.2455(5) 1.2668(3) 0.040 Uiso 1 calc R . C5 C 0.7704(3) 0.3002(5) 1.1782(3) 0.0299(12) Uani 1 d . . H5A H 0.7481(3) 0.3401(5) 1.2015(3) 0.036 Uiso 1 calc R . C6 C 0.7397(3) 0.2958(4) 1.1045(3) 0.0239(11) Uani 1 d . . C7 C 0.8601(3) 0.1290(4) 1.0630(3) 0.0226(11) Uani 1 d . . N7 N 0.8221(2) 0.1439(3) 0.9965(2) 0.0226(9) Uani 1 d . . C8 C 0.9257(3) 0.0594(5) 1.0977(3) 0.0327(13) Uani 1 d . . H8A H 0.9164(3) 0.0054(5) 1.1260(3) 0.049 Uiso 1 d R . H8B H 0.9681(3) 0.1023(5) 1.1286(3) 0.049 Uiso 1 d R . H8C H 0.9359(3) 0.0251(5) 1.0615(3) 0.049 Uiso 1 d R . C9 C 0.6688(3) 0.3443(4) 1.0557(3) 0.0252(11) Uani 1 d . . N9 N 0.6503(2) 0.3298(3) 0.9891(2) 0.0222(9) Uani 1 d . . C10 C 0.6246(3) 0.4008(5) 1.0850(3) 0.0353(14) Uani 1 d . . H10A H 0.6481(3) 0.4683(5) 1.1055(3) 0.053 Uiso 1 d R . H10B H 0.6210(3) 0.3573(5) 1.1217(3) 0.053 Uiso 1 d R . H10C H 0.5754(3) 0.4142(5) 1.0470(3) 0.053 Uiso 1 d R . C11 C 0.8398(3) 0.0919(4) 0.9449(3) 0.0240(11) Uani 1 d . . C12 C 0.8964(3) 0.1319(4) 0.9307(3) 0.0294(12) Uani 1 d . . C13 C 0.9053(3) 0.0842(5) 0.8759(3) 0.0359(14) Uani 1 d . . H13A H 0.9420(3) 0.1102(5) 0.8640(3) 0.043 Uiso 1 calc R . C14 C 0.8625(4) 0.0006(6) 0.8381(3) 0.044(2) Uani 1 d . . H14A H 0.8707(4) -0.0312(6) 0.8015(3) 0.053 Uiso 1 calc R . C15 C 0.8075(4) -0.0372(6) 0.8537(4) 0.046(2) Uani 1 d . . H15A H 0.7780(4) -0.0947(6) 0.8272(4) 0.055 Uiso 1 calc R . C16 C 0.7948(3) 0.0070(5) 0.9067(3) 0.0348(13) Uani 1 d . . C17 C 0.9444(3) 0.2234(5) 0.9712(3) 0.0328(13) Uani 1 d . . H17A H 0.9286(3) 0.2469(5) 1.0075(3) 0.039 Uiso 1 calc R . C18 C 0.9363(4) 0.3171(5) 0.9224(4) 0.0419(15) Uani 1 d . . H18A H 0.9680(4) 0.3751(5) 0.9501(4) 0.063 Uiso 1 calc R . H18B H 0.8853(4) 0.3409(5) 0.9001(4) 0.063 Uiso 1 calc R . H18C H 0.9505(4) 0.2952(5) 0.8857(4) 0.063 Uiso 1 calc R . C19 C 1.0253(3) 0.1890(6) 1.0101(4) 0.045(2) Uani 1 d . . H19A H 1.0555(3) 0.2493(6) 1.0360(4) 0.067 Uiso 1 calc R . H19B H 1.0416(3) 0.1636(6) 0.9756(4) 0.067 Uiso 1 calc R . H19C H 1.0303(3) 0.1320(6) 1.0435(4) 0.067 Uiso 1 calc R . C20 C 0.7373(4) -0.0376(5) 0.9269(4) 0.0423(15) Uani 1 d . . H20A H 0.7204(4) 0.0221(5) 0.9470(4) 0.051 Uiso 1 calc R . C21 C 0.7719(5) -0.1201(7) 0.9855(5) 0.066(2) Uani 1 d . . H21A H 0.8153(5) -0.0897(7) 1.0246(5) 0.100 Uiso 1 calc R . H21B H 0.7864(5) -0.1821(7) 0.9667(5) 0.100 Uiso 1 calc R . H21C H 0.7364(5) -0.1413(7) 1.0025(5) 0.100 Uiso 1 calc R . C22 C 0.6698(4) -0.0824(6) 0.8653(4) 0.056(2) Uani 1 d . . H22A H 0.6357(4) -0.1093(6) 0.8826(4) 0.084 Uiso 1 calc R . H22B H 0.6844(4) -0.1402(6) 0.8433(4) 0.084 Uiso 1 calc R . H22C H 0.6459(4) -0.0266(6) 0.8303(4) 0.084 Uiso 1 calc R . C23 C 0.5791(3) 0.3618(4) 0.9361(3) 0.0230(11) Uani 1 d . . C24 C 0.5273(3) 0.2809(5) 0.9057(3) 0.0295(12) Uani 1 d . . C25 C 0.4578(3) 0.3097(6) 0.8540(3) 0.0392(15) Uani 1 d . . H25A H 0.4209(3) 0.2572(6) 0.8337(3) 0.047 Uiso 1 calc R . C26 C 0.4421(3) 0.4130(5) 0.8319(3) 0.041(2) Uani 1 d . . H26A H 0.3946(3) 0.4307(5) 0.7964(3) 0.049 Uiso 1 calc R . C27 C 0.4942(3) 0.4911(5) 0.8606(3) 0.0348(14) Uani 1 d . . H27A H 0.4827(3) 0.5617(5) 0.8440(3) 0.042 Uiso 1 calc R . C28 C 0.5640(3) 0.4668(5) 0.9141(3) 0.0284(12) Uani 1 d . . C29 C 0.5454(3) 0.1678(5) 0.9320(4) 0.0382(14) Uani 1 d . . H29A H 0.5996(3) 0.1592(5) 0.9513(4) 0.046 Uiso 1 calc R . C30 C 0.5097(5) 0.0855(6) 0.8733(5) 0.060(2) Uani 1 d . . H30A H 0.5233(5) 0.0144(6) 0.8934(5) 0.090 Uiso 1 calc R . H30B H 0.5266(5) 0.0961(6) 0.8370(5) 0.090 Uiso 1 calc R . H30C H 0.4563(5) 0.0933(6) 0.8520(5) 0.090 Uiso 1 calc R . C31 C 0.5256(5) 0.1475(6) 0.9932(5) 0.060(2) Uani 1 d . . H31A H 0.5377(5) 0.0742(6) 1.0094(5) 0.091 Uiso 1 calc R . H31B H 0.4731(5) 0.1595(6) 0.9768(5) 0.091 Uiso 1 calc R . H31C H 0.5536(5) 0.1958(6) 1.0324(5) 0.091 Uiso 1 calc R . C32 C 0.6205(3) 0.5556(5) 0.9456(3) 0.0348(13) Uani 1 d . . H32A H 0.6651(3) 0.5255(5) 0.9856(3) 0.042 Uiso 1 calc R . C33 C 0.5916(4) 0.6451(6) 0.9747(4) 0.054(2) Uani 1 d . . H33A H 0.6289(4) 0.7005(6) 0.9944(4) 0.081 Uiso 1 calc R . H33B H 0.5801(4) 0.6175(6) 1.0119(4) 0.081 Uiso 1 calc R . H33C H 0.5472(4) 0.6748(6) 0.9365(4) 0.081 Uiso 1 calc R . C34 C 0.6430(4) 0.5988(6) 0.8900(4) 0.051(2) Uani 1 d . . H34A H 0.6614(4) 0.5408(6) 0.8717(4) 0.076 Uiso 1 calc R . H34B H 0.6814(4) 0.6522(6) 0.9119(4) 0.076 Uiso 1 calc R . H34C H 0.6003(4) 0.6310(6) 0.8510(4) 0.076 Uiso 1 calc R . N35 N 0.7835(3) 0.3908(4) 0.9591(2) 0.0308(11) Uani 1 d . . C36 C 0.8155(4) 0.4654(5) 0.9617(4) 0.0385(14) Uani 1 d . . C37 C 0.8586(5) 0.5595(6) 0.9662(6) 0.072(3) Uani 1 d . . H37A H 0.8287(5) 0.6094(6) 0.9289(6) 0.108 Uiso 1 d R . H37B H 0.9019(5) 0.5396(6) 0.9602(6) 0.108 Uiso 1 d R . H37C H 0.8740(5) 0.5930(6) 1.0125(6) 0.108 Uiso 1 d R . S S 0.66983(8) 0.23046(12) 0.79497(7) 0.0306(3) Uani 1 d . . O11 O 0.6664(2) 0.2149(3) 0.8627(2) 0.0329(9) Uani 1 d . . O12 O 0.6580(2) 0.1351(4) 0.7556(2) 0.0408(10) Uani 1 d . . O13 O 0.7297(3) 0.2966(4) 0.8013(2) 0.0507(12) Uani 1 d . . C38 C 0.5883(4) 0.3079(6) 0.7441(3) 0.045(2) Uani 1 d . . F11 F 0.5824(3) 0.3264(4) 0.6801(2) 0.0744(15) Uani 1 d . . F12 F 0.5882(3) 0.3984(4) 0.7744(3) 0.0706(14) Uani 1 d . . F13 F 0.5278(2) 0.2551(4) 0.7359(2) 0.0686(13) Uani 1 d . . Sb Sb 0.98874(3) 0.59170(4) 0.81278(3) 0.0577(2) Uani 1 d . . F1 F 1.0006(4) 0.4440(5) 0.8169(4) 0.103(2) Uani 1 d . . F2 F 0.9417(7) 0.5810(7) 0.8689(6) 0.176(5) Uani 1 d . . F3 F 0.8992(3) 0.5758(5) 0.7303(4) 0.110(2) Uani 1 d . . F4 F 1.0348(4) 0.5977(6) 0.7550(3) 0.102(2) Uani 1 d . . F5 F 1.0765(4) 0.6100(6) 0.8914(3) 0.128(3) Uani 1 d . . F6 F 0.9766(4) 0.7363(5) 0.8089(4) 0.097(2) Uani 1 d . . C40 C 0.7439(6) 0.5140(10) 0.7183(7) 0.093(3) Uani 1 d . . H40A H 0.7403(6) 0.4439(10) 0.7374(7) 0.112 Uiso 1 calc R . H40B H 0.7965(6) 0.5276(10) 0.7327(7) 0.112 Uiso 1 calc R . Cl1 Cl 0.6990(2) 0.5073(4) 0.6267(2) 0.1401(15) Uani 1 d . . Cl2 Cl 0.7138(3) 0.6055(5) 0.7565(2) 0.173(2) Uani 1 d . . C50 C 0.8110(35) 0.8096(59) 0.6584(38) 0.254(31) Uani 0.60 d PU . C50' C 0.8165(17) 0.8313(29) 0.5887(14) 0.082(7) Uani 0.40 d PU . Cl3 Cl 0.8884(7) 0.7596(6) 0.6246(4) 0.141(3) Uani 0.47 d PU . Cl4 Cl 0.7912(9) 0.9111(14) 0.6232(9) 0.176(6) Uani 0.43 d PU . Cl5 Cl 0.7620(10) 0.8006(11) 0.6872(7) 0.124(4) Uani 0.32 d PU . Cl6 Cl 0.7470(9) 0.8701(16) 0.6696(8) 0.148(6) Uani 0.30 d PU . Cl7 Cl 0.8003(9) 0.9171(18) 0.5930(10) 0.104(5) Uani 0.26 d PU . Cl8 Cl 0.8480(14) 0.8354(21) 0.6696(12) 0.131(6) Uani 0.22 d PU . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0215(4) 0.0278(4) 0.0088(4) -0.0005(3) 0.0063(3) 0.0005(3) N1 0.023(2) 0.031(2) 0.011(2) 0.001(2) 0.008(2) 0.001(2) C2 0.021(2) 0.030(3) 0.015(3) 0.001(2) 0.008(2) -0.001(2) C3 0.022(3) 0.046(3) 0.017(3) 0.010(2) 0.006(2) 0.004(2) C4 0.034(3) 0.051(4) 0.014(3) 0.001(2) 0.011(2) 0.000(3) C5 0.029(3) 0.048(3) 0.013(3) -0.003(2) 0.010(2) -0.002(2) C6 0.024(3) 0.033(3) 0.018(3) -0.002(2) 0.013(2) -0.002(2) C7 0.022(3) 0.027(3) 0.019(3) 0.003(2) 0.010(2) -0.002(2) N7 0.027(2) 0.025(2) 0.017(2) -0.003(2) 0.011(2) -0.002(2) C8 0.036(3) 0.037(3) 0.024(3) 0.003(2) 0.012(3) 0.012(3) C9 0.025(3) 0.032(3) 0.021(3) -0.001(2) 0.013(2) -0.001(2) N9 0.023(2) 0.030(2) 0.013(2) -0.001(2) 0.007(2) -0.002(2) C10 0.034(3) 0.051(4) 0.024(3) 0.001(3) 0.016(3) 0.012(3) C11 0.026(3) 0.029(3) 0.016(3) 0.003(2) 0.008(2) 0.008(2) C12 0.034(3) 0.032(3) 0.022(3) 0.006(2) 0.012(2) 0.011(2) C13 0.041(3) 0.046(4) 0.026(3) 0.004(3) 0.020(3) 0.011(3) C14 0.054(4) 0.054(4) 0.029(3) -0.008(3) 0.022(3) 0.012(3) C15 0.055(4) 0.044(4) 0.040(4) -0.016(3) 0.022(3) 0.000(3) C16 0.044(3) 0.030(3) 0.029(3) -0.007(2) 0.015(3) -0.001(3) C17 0.034(3) 0.039(3) 0.029(3) 0.005(3) 0.016(3) 0.003(2) C18 0.044(4) 0.046(4) 0.040(4) 0.008(3) 0.023(3) 0.003(3) C19 0.035(3) 0.053(4) 0.043(4) 0.010(3) 0.014(3) 0.008(3) C20 0.044(4) 0.038(3) 0.044(4) -0.012(3) 0.020(3) -0.009(3) C21 0.073(5) 0.068(5) 0.053(5) 0.007(4) 0.024(4) -0.020(4) C22 0.054(4) 0.054(4) 0.054(5) -0.007(4) 0.018(4) -0.016(3) C23 0.025(3) 0.032(3) 0.012(2) -0.004(2) 0.008(2) 0.002(2) C24 0.027(3) 0.039(3) 0.022(3) -0.003(2) 0.009(2) -0.003(2) C25 0.023(3) 0.058(4) 0.027(3) -0.009(3) 0.004(2) -0.005(3) C26 0.027(3) 0.060(4) 0.026(3) -0.003(3) 0.002(3) 0.009(3) C27 0.036(3) 0.046(4) 0.024(3) 0.006(3) 0.015(3) 0.015(3) C28 0.027(3) 0.038(3) 0.021(3) 0.000(2) 0.012(2) 0.003(2) C29 0.035(3) 0.032(3) 0.044(4) -0.003(3) 0.014(3) -0.005(2) C30 0.059(5) 0.046(4) 0.073(6) -0.024(4) 0.027(4) -0.015(4) C31 0.078(5) 0.048(4) 0.064(5) 0.003(4) 0.040(5) -0.006(4) C32 0.034(3) 0.029(3) 0.040(3) 0.002(3) 0.015(3) 0.000(2) C33 0.058(4) 0.041(4) 0.062(5) -0.012(3) 0.025(4) 0.003(3) C34 0.047(4) 0.047(4) 0.060(5) 0.013(3) 0.025(4) 0.002(3) N35 0.031(2) 0.039(3) 0.023(2) -0.002(2) 0.014(2) -0.001(2) C36 0.040(3) 0.036(4) 0.046(4) -0.005(3) 0.025(3) -0.001(3) C37 0.066(5) 0.045(4) 0.117(8) -0.013(5) 0.051(6) -0.017(4) S 0.0330(7) 0.0452(8) 0.0135(6) -0.0053(6) 0.0104(5) -0.0044(6) O11 0.033(2) 0.053(2) 0.012(2) -0.007(2) 0.009(2) -0.007(2) O12 0.054(3) 0.047(2) 0.021(2) -0.009(2) 0.015(2) -0.001(2) O13 0.049(3) 0.074(3) 0.036(3) -0.012(2) 0.025(2) -0.024(2) C38 0.051(4) 0.056(4) 0.020(3) -0.002(3) 0.009(3) 0.003(3) F11 0.100(4) 0.092(4) 0.027(2) 0.021(2) 0.025(2) 0.036(3) F12 0.095(4) 0.056(3) 0.056(3) -0.007(2) 0.029(3) 0.022(2) F13 0.036(2) 0.102(4) 0.054(3) -0.006(2) 0.007(2) 0.006(2) Sb 0.0634(3) 0.0673(4) 0.0541(3) -0.0312(2) 0.0367(3) -0.0312(3) F1 0.104(5) 0.074(4) 0.124(6) -0.029(4) 0.046(4) -0.023(3) F2 0.296(13) 0.132(6) 0.238(11) -0.067(7) 0.244(11) -0.086(7) F3 0.059(3) 0.115(5) 0.136(6) -0.059(4) 0.025(4) -0.026(3) F4 0.093(4) 0.147(6) 0.093(4) -0.040(4) 0.067(4) -0.039(4) F5 0.140(6) 0.105(5) 0.064(4) -0.007(3) -0.021(4) -0.048(4) F6 0.095(4) 0.071(4) 0.121(5) -0.031(3) 0.046(4) -0.018(3) C40 0.064(6) 0.103(8) 0.119(10) 0.019(7) 0.046(6) -0.001(5) Cl1 0.111(3) 0.187(4) 0.108(3) 0.007(3) 0.035(2) 0.036(3) Cl2 0.147(4) 0.250(6) 0.117(3) 0.017(3) 0.054(3) 0.107(4) C50 0.264(37) 0.258(36) 0.241(35) -0.017(19) 0.113(23) 0.002(20) C50' 0.098(15) 0.119(17) 0.048(11) -0.030(11) 0.048(11) -0.024(13) Cl3 0.245(10) 0.102(5) 0.092(5) -0.025(4) 0.088(6) -0.019(6) Cl4 0.145(10) 0.178(12) 0.145(11) 0.028(9) 0.009(8) 0.085(9) Cl5 0.192(11) 0.116(8) 0.112(8) -0.012(6) 0.111(8) -0.047(8) Cl6 0.130(9) 0.149(11) 0.096(8) -0.020(8) -0.012(7) 0.051(9) Cl7 0.081(7) 0.130(11) 0.110(10) 0.070(9) 0.049(7) 0.026(7) Cl8 0.143(13) 0.150(14) 0.111(11) 0.001(10) 0.067(10) 0.017(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O11 1.988(4) . ? Fe N35 2.051(5) . ? Fe N1 2.083(4) . ? Fe N9 2.176(4) . ? Fe N7 2.179(4) . ? N1 C2 1.335(7) . ? N1 C6 1.339(7) . ? C2 C3 1.391(8) . ? C2 C7 1.488(7) . ? C3 C4 1.378(8) . ? C4 C5 1.392(8) . ? C5 C6 1.396(8) . ? C6 C9 1.483(8) . ? C7 N7 1.280(7) . ? C7 C8 1.493(8) . ? N7 C11 1.450(7) . ? C9 N9 1.295(7) . ? C9 C10 1.486(8) . ? N9 C23 1.441(7) . ? C11 C16 1.409(8) . ? C11 C12 1.409(8) . ? C12 C13 1.386(8) . ? C12 C17 1.511(9) . ? C13 C14 1.376(10) . ? C14 C15 1.388(10) . ? C15 C16 1.375(9) . ? C16 C20 1.524(9) . ? C17 C18 1.529(8) . ? C17 C19 1.542(8) . ? C20 C22 1.519(10) . ? C20 C21 1.529(11) . ? C23 C28 1.395(8) . ? C23 C24 1.402(8) . ? C24 C25 1.398(8) . ? C24 C29 1.519(9) . ? C25 C26 1.375(10) . ? C26 C27 1.377(10) . ? C27 C28 1.401(8) . ? C28 C32 1.532(8) . ? C29 C30 1.530(9) . ? C29 C31 1.538(10) . ? C32 C33 1.527(9) . ? C32 C34 1.537(9) . ? N35 C36 1.134(8) . ? C36 C37 1.457(10) . ? S O12 1.423(5) . ? S O13 1.436(5) . ? S O11 1.475(4) . ? S C38 1.813(7) . ? C38 F12 1.311(8) . ? C38 F11 1.322(8) . ? C38 F13 1.343(9) . ? Sb F5 1.834(6) . ? Sb F2 1.834(6) . ? Sb F6 1.841(6) . ? Sb F4 1.843(5) . ? Sb F1 1.880(6) . ? Sb F3 1.890(6) . ? C40 Cl2 1.676(13) . ? C40 Cl1 1.732(13) . ? C50 Cl8 0.76(7) . ? C50 Cl5 1.39(7) . ? C50 Cl4 1.45(8) . ? C50 C50' 1.55(8) . ? C50 Cl6 1.62(7) . ? C50 Cl7 1.88(8) . ? C50 Cl3 2.10(7) . ? C50' Cl7 1.15(4) . ? C50' Cl4 1.47(3) . ? C50' Cl8 1.53(3) . ? C50' Cl3 1.60(4) . ? Cl3 Cl8 1.79(2) . ? Cl4 Cl7 0.74(2) . ? Cl4 Cl8 1.49(3) . ? Cl4 Cl6 1.68(3) . ? Cl4 Cl5 2.20(2) . ? Cl5 Cl6 0.95(2) . ? Cl5 Cl8 2.00(3) . ? Cl6 Cl8 2.11(3) . ? Cl6 Cl7 2.39(3) . ? Cl7 Cl8 1.80(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Fe N35 106.4(2) . . ? O11 Fe N1 154.5(2) . . ? N35 Fe N1 99.0(2) . . ? O11 Fe N9 99.6(2) . . ? N35 Fe N9 96.2(2) . . ? N1 Fe N9 74.2(2) . . ? O11 Fe N7 104.5(2) . . ? N35 Fe N7 99.5(2) . . ? N1 Fe N7 73.7(2) . . ? N9 Fe N7 146.0(2) . . ? C2 N1 C6 121.3(4) . . ? C2 N1 Fe 119.7(3) . . ? C6 N1 Fe 118.5(3) . . ? N1 C2 C3 120.8(5) . . ? N1 C2 C7 113.3(4) . . ? C3 C2 C7 125.9(5) . . ? C4 C3 C2 118.5(5) . . ? C3 C4 C5 120.6(5) . . ? C4 C5 C6 117.7(5) . . ? N1 C6 C5 121.0(5) . . ? N1 C6 C9 114.0(5) . . ? C5 C6 C9 124.9(5) . . ? N7 C7 C2 115.0(5) . . ? N7 C7 C8 126.6(5) . . ? C2 C7 C8 118.4(5) . . ? C7 N7 C11 121.8(4) . . ? C7 N7 Fe 117.7(3) . . ? C11 N7 Fe 120.5(3) . . ? N9 C9 C6 114.7(5) . . ? N9 C9 C10 125.7(5) . . ? C6 C9 C10 119.6(5) . . ? C9 N9 C23 120.5(4) . . ? C9 N9 Fe 116.9(4) . . ? C23 N9 Fe 122.5(3) . . ? C16 C11 C12 122.6(5) . . ? C16 C11 N7 117.2(5) . . ? C12 C11 N7 119.9(5) . . ? C13 C12 C11 116.4(6) . . ? C13 C12 C17 120.8(5) . . ? C11 C12 C17 122.7(5) . . ? C14 C13 C12 122.2(6) . . ? C13 C14 C15 119.9(6) . . ? C16 C15 C14 121.3(6) . . ? C15 C16 C11 117.6(6) . . ? C15 C16 C20 121.8(6) . . ? C11 C16 C20 120.6(5) . . ? C12 C17 C18 111.4(5) . . ? C12 C17 C19 110.7(5) . . ? C18 C17 C19 110.2(5) . . ? C22 C20 C16 114.5(6) . . ? C22 C20 C21 110.7(6) . . ? C16 C20 C21 110.0(6) . . ? C28 C23 C24 122.2(5) . . ? C28 C23 N9 121.4(5) . . ? C24 C23 N9 116.3(5) . . ? C25 C24 C23 117.5(6) . . ? C25 C24 C29 121.8(5) . . ? C23 C24 C29 120.6(5) . . ? C26 C25 C24 120.9(6) . . ? C25 C26 C27 121.0(6) . . ? C26 C27 C28 120.3(6) . . ? C23 C28 C27 118.0(5) . . ? C23 C28 C32 122.8(5) . . ? C27 C28 C32 119.1(5) . . ? C24 C29 C30 113.3(6) . . ? C24 C29 C31 110.6(5) . . ? C30 C29 C31 111.0(6) . . ? C33 C32 C28 111.5(5) . . ? C33 C32 C34 110.2(6) . . ? C28 C32 C34 110.6(5) . . ? C36 N35 Fe 175.6(5) . . ? N35 C36 C37 178.4(7) . . ? O12 S O13 117.6(3) . . ? O12 S O11 112.5(3) . . ? O13 S O11 113.2(3) . . ? O12 S C38 103.9(3) . . ? O13 S C38 105.0(3) . . ? O11 S C38 102.6(3) . . ? S O11 Fe 134.5(3) . . ? F12 C38 F11 109.0(6) . . ? F12 C38 F13 107.2(6) . . ? F11 C38 F13 107.3(6) . . ? F12 C38 S 112.5(5) . . ? F11 C38 S 110.0(5) . . ? F13 C38 S 110.8(5) . . ? F5 Sb F2 90.3(5) . . ? F5 Sb F6 88.4(3) . . ? F2 Sb F6 90.2(3) . . ? F5 Sb F4 90.8(4) . . ? F2 Sb F4 177.9(3) . . ? F6 Sb F4 91.6(3) . . ? F5 Sb F1 91.7(3) . . ? F2 Sb F1 89.5(4) . . ? F6 Sb F1 179.7(3) . . ? F4 Sb F1 88.7(3) . . ? F5 Sb F3 178.3(3) . . ? F2 Sb F3 91.0(5) . . ? F6 Sb F3 90.5(3) . . ? F4 Sb F3 87.9(3) . . ? F1 Sb F3 89.4(3) . . ? Cl2 C40 Cl1 116.5(7) . . ? Cl8 C50 Cl5 135.3(87) . . ? Cl8 C50 Cl4 77.8(70) . . ? Cl5 C50 Cl4 102.0(49) . . ? Cl8 C50 C50' 74.7(67) . . ? Cl5 C50 C50' 143.4(54) . . ? Cl4 C50 C50' 58.5(33) . . ? Cl8 C50 Cl6 120.5(82) . . ? Cl5 C50 Cl6 35.8(19) . . ? Cl4 C50 Cl6 66.3(34) . . ? C50' C50 Cl6 117.4(52) . . ? Cl8 C50 Cl7 72.0(68) . . ? Cl5 C50 Cl7 120.7(48) . . ? Cl4 C50 Cl7 21.1(16) . . ? C50' C50 Cl7 37.7(22) . . ? Cl6 C50 Cl7 85.9(37) . . ? Cl8 C50 Cl3 56.0(57) . . ? Cl5 C50 Cl3 157.3(53) . . ? Cl4 C50 Cl3 99.9(41) . . ? C50' C50 Cl3 49.2(26) . . ? Cl6 C50 Cl3 165.9(52) . . ? Cl7 C50 Cl3 80.0(29) . . ? Cl7 C50' Cl4 29.9(11) . . ? Cl7 C50' Cl8 82.6(18) . . ? Cl4 C50' Cl8 59.3(13) . . ? Cl7 C50' C50 86.9(31) . . ? Cl4 C50' C50 57.3(28) . . ? Cl8 C50' C50 28.4(25) . . ? Cl7 C50' Cl3 137.2(24) . . ? Cl4 C50' Cl3 127.4(18) . . ? Cl8 C50' Cl3 69.7(17) . . ? C50 C50' Cl3 83.7(34) . . ? C50' Cl3 Cl8 53.5(11) . . ? C50' Cl3 C50 47.2(22) . . ? Cl8 Cl3 C50 20.5(20) . . ? Cl7 Cl4 C50 114.3(41) . . ? Cl7 Cl4 C50' 50.7(25) . . ? C50 Cl4 C50' 64.2(31) . . ? Cl7 Cl4 Cl8 102.3(26) . . ? C50 Cl4 Cl8 29.8(27) . . ? C50' Cl4 Cl8 62.6(17) . . ? Cl7 Cl4 Cl6 159.2(33) . . ? C50 Cl4 Cl6 61.8(31) . . ? C50' Cl4 Cl6 118.4(20) . . ? Cl8 Cl4 Cl6 83.1(14) . . ? Cl7 Cl4 Cl5 146.2(33) . . ? C50 Cl4 Cl5 38.1(29) . . ? C50' Cl4 Cl5 96.9(17) . . ? Cl8 Cl4 Cl5 62.0(13) . . ? Cl6 Cl4 Cl5 23.8(6) . . ? Cl6 Cl5 C50 85.5(34) . . ? Cl6 Cl5 Cl8 83.0(19) . . ? C50 Cl5 Cl8 15.4(30) . . ? Cl6 Cl5 Cl4 45.6(16) . . ? C50 Cl5 Cl4 40.0(32) . . ? Cl8 Cl5 Cl4 41.0(8) . . ? Cl5 Cl6 C50 58.7(27) . . ? Cl5 Cl6 Cl4 110.6(19) . . ? C50 Cl6 Cl4 52.0(29) . . ? Cl5 Cl6 Cl8 70.4(17) . . ? C50 Cl6 Cl8 18.0(26) . . ? Cl4 Cl6 Cl8 44.4(9) . . ? Cl5 Cl6 Cl7 109.3(18) . . ? C50 Cl6 Cl7 51.6(30) . . ? Cl4 Cl6 Cl7 6.3(10) . . ? Cl8 Cl6 Cl7 46.5(9) . . ? Cl4 Cl7 C50' 99.4(28) . . ? Cl4 Cl7 Cl8 53.9(19) . . ? C50' Cl7 Cl8 57.9(17) . . ? Cl4 Cl7 C50 44.6(29) . . ? C50' Cl7 C50 55.4(24) . . ? Cl8 Cl7 C50 23.6(21) . . ? Cl4 Cl7 Cl6 14.5(24) . . ? C50' Cl7 Cl6 93.0(15) . . ? Cl8 Cl7 Cl6 58.3(9) . . ? C50 Cl7 Cl6 42.5(22) . . ? C50 Cl8 Cl4 72.3(68) . . ? C50 Cl8 C50' 76.9(67) . . ? Cl4 Cl8 C50' 58.1(17) . . ? C50 Cl8 Cl3 103.5(68) . . ? Cl4 Cl8 Cl3 113.8(15) . . ? C50' Cl8 Cl3 56.8(15) . . ? C50 Cl8 Cl7 84.4(71) . . ? Cl4 Cl8 Cl7 23.8(10) . . ? C50' Cl8 Cl7 39.4(15) . . ? Cl3 Cl8 Cl7 91.3(12) . . ? C50 Cl8 Cl5 29.3(62) . . ? Cl4 Cl8 Cl5 77.0(14) . . ? C50' Cl8 Cl5 103.5(18) . . ? Cl3 Cl8 Cl5 129.2(16) . . ? Cl7 Cl8 Cl5 97.3(13) . . ? C50 Cl8 Cl6 41.5(63) . . ? Cl4 Cl8 Cl6 52.5(11) . . ? C50' Cl8 Cl6 94.8(17) . . ? Cl3 Cl8 Cl6 142.6(16) . . ? Cl7 Cl8 Cl6 75.1(11) . . ? Cl5 Cl8 Cl6 26.6(6) . . ? _refine_diff_density_max 0.913 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.099 #===END data_[Fe(2)(CH3CN)3](SbF6)2 _database_code_depnum_ccdc_archive 'CCDC 246558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Fe(2)(CH3CN)3](SbF6)2' _chemical_formula_sum 'C32 H38 Cl2 F12 Fe N6 Sb2' _chemical_formula_weight 1104.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 12.356(4) _cell_length_b 22.688(6) _cell_length_c 15.762(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.16(4) _cell_angle_gamma 90.00 _cell_volume 4284(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 12.56 _exptl_crystal_description blocks _exptl_crystal_colour Red _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 1.794 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6939 _exptl_absorpt_correction_T_max 0.9127 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3956 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3956 _reflns_number_gt 3599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0394 _refine_ls_wR_factor_obs+ 0.0942 _refine_ls_abs_structure_Flack+ 0.06(6) _refine_ls_R_factor_obs- 0.0411 _refine_ls_wR_factor_obs- 0.0986 _refine_ls_abs_structure_Flack- 0.94(6) _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^)+(0.0536P)^2^+7.6517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00002(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 3956 _refine_ls_number_parameters 531 _refine_ls_number_restraints 386 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.043 _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 Fe Fe 0.59434(9) 0.37404(4) 0.63657(7) 0.0322(2) Uani 1 1 d . . . N1 N 0.6815(5) 0.4222(3) 0.5594(4) 0.0336(13) Uani 1 1 d . . . C2 C 0.7260(7) 0.4744(3) 0.5912(5) 0.0356(16) Uani 1 1 d . . . C3 C 0.8102(8) 0.4996(4) 0.5587(6) 0.0440(19) Uani 1 1 d . . . H3A H 0.8409 0.5362 0.5799 0.053 Uiso 1 1 calc R . . C4 C 0.8473(8) 0.4706(4) 0.4959(7) 0.052(2) Uani 1 1 d . . . H4A H 0.9055 0.4870 0.4749 0.062 Uiso 1 1 calc R . . C5 C 0.8002(8) 0.4168(4) 0.4620(6) 0.048(2) Uani 1 1 d . . . H5A H 0.8234 0.3975 0.4167 0.057 Uiso 1 1 calc R . . C6 C 0.7184(7) 0.3933(3) 0.4979(5) 0.0360(17) Uani 1 1 d . . . C7 C 0.6797(7) 0.4988(3) 0.6619(5) 0.0339(16) Uani 1 1 d . . . N7 N 0.6148(6) 0.4647(3) 0.6916(4) 0.0364(15) Uani 1 1 d . . . C8 C 0.7073(8) 0.5614(4) 0.6901(6) 0.046(2) Uani 1 1 d . . . H8A H 0.6675 0.5723 0.7338 0.069 Uiso 1 1 calc R . . H8B H 0.6852 0.5873 0.6400 0.069 Uiso 1 1 calc R . . H8C H 0.7870 0.5650 0.7149 0.069 Uiso 1 1 calc R . . C9 C 0.6646(7) 0.3344(4) 0.4759(5) 0.0406(18) Uani 1 1 d . . . N9 N 0.6048(6) 0.3162(3) 0.5254(5) 0.0391(15) Uani 1 1 d . . . C10 C 0.6847(10) 0.3014(4) 0.3969(7) 0.055(2) Uani 1 1 d . . . H10A H 0.6378 0.2665 0.3861 0.082 Uiso 1 1 calc R . . H10B H 0.7625 0.2897 0.4083 0.082 Uiso 1 1 calc R . . H10C H 0.6667 0.3268 0.3459 0.082 Uiso 1 1 calc R . . C11 C 0.5552(7) 0.4853(3) 0.7544(5) 0.0342(16) Uani 1 1 d . . . C12 C 0.5849(7) 0.4633(4) 0.8388(6) 0.0397(18) Uani 1 1 d . . . C13 C 0.5265(8) 0.4816(4) 0.9002(7) 0.048(2) Uani 1 1 d . . . H13A H 0.5459 0.4667 0.9576 0.057 Uiso 1 1 calc R . . C14 C 0.4410(9) 0.5215(4) 0.8758(7) 0.056(2) Uani 1 1 d . . . H14A H 0.4024 0.5340 0.9172 0.067 Uiso 1 1 calc R . . C15 C 0.4102(8) 0.5438(4) 0.7906(7) 0.050(2) Uani 1 1 d . . . H15A H 0.3507 0.5707 0.7752 0.060 Uiso 1 1 calc R . . C16 C 0.4672(8) 0.5265(4) 0.7275(6) 0.0434(19) Uani 1 1 d . . . C17 C 0.6785(9) 0.4177(4) 0.8659(6) 0.051(2) Uani 1 1 d . . . H17A H 0.6545 0.3805 0.8372 0.077 Uiso 1 1 calc R . . H17B H 0.6959 0.4123 0.9288 0.077 Uiso 1 1 calc R . . H17C H 0.7445 0.4315 0.8489 0.077 Uiso 1 1 calc R . . C18 C 0.4308(9) 0.5504(4) 0.6379(7) 0.055(2) Uani 1 1 d . . . H18A H 0.4457 0.5217 0.5966 0.082 Uiso 1 1 calc R . . H18B H 0.4714 0.5864 0.6338 0.082 Uiso 1 1 calc R . . H18C H 0.3514 0.5587 0.6246 0.082 Uiso 1 1 calc R . . C19 C 0.5504(8) 0.2593(3) 0.5108(6) 0.0399(18) Uani 1 1 d . . . C20 C 0.4428(8) 0.2571(4) 0.4567(6) 0.046(2) Uani 1 1 d . . . C21 C 0.3863(10) 0.2025(5) 0.4495(8) 0.064(3) Uani 1 1 d . . . H21A H 0.3132 0.1994 0.4143 0.077 Uiso 1 1 calc R . . C22 C 0.4372(11) 0.1543(5) 0.4934(8) 0.062(3) Uani 1 1 d . . . H22A H 0.3980 0.1185 0.4891 0.075 Uiso 1 1 calc R . . C23 C 0.5451(10) 0.1571(4) 0.5438(8) 0.058(3) Uani 1 1 d . . . H23A H 0.5802 0.1226 0.5699 0.070 Uiso 1 1 calc R . . C24 C 0.6035(9) 0.2104(4) 0.5567(7) 0.049(2) Uani 1 1 d . . . C25 C 0.3855(11) 0.3087(5) 0.4042(7) 0.066(3) Uani 1 1 d . . . H25A H 0.4108 0.3123 0.3509 0.098 Uiso 1 1 calc R . . H25B H 0.4033 0.3445 0.4384 0.098 Uiso 1 1 calc R . . H25C H 0.3054 0.3025 0.3896 0.098 Uiso 1 1 calc R . . C26 C 0.7184(10) 0.2133(5) 0.6136(9) 0.067(3) Uani 1 1 d . . . H26A H 0.7396 0.1749 0.6393 0.101 Uiso 1 1 calc R . . H26B H 0.7208 0.2420 0.6597 0.101 Uiso 1 1 calc R . . H26C H 0.7697 0.2250 0.5790 0.101 Uiso 1 1 calc R . . N27 N 0.4211(6) 0.3972(3) 0.5922(5) 0.0438(16) Uani 1 1 d . . . C28 C 0.3301(8) 0.4084(4) 0.5863(6) 0.047(2) Uani 1 1 d . . . C29 C 0.2127(10) 0.4238(6) 0.5786(8) 0.074(3) Uani 1 1 d . . . H29A H 0.1989 0.4636 0.5562 0.110 Uiso 1 1 calc R . . H29B H 0.1966 0.4214 0.6357 0.110 Uiso 1 1 calc R . . H29C H 0.1651 0.3966 0.5388 0.110 Uiso 1 1 calc R . . N30 N 0.5401(7) 0.3063(3) 0.7083(5) 0.0457(17) Uani 1 1 d . . . C31 C 0.5061(9) 0.2642(4) 0.7299(6) 0.049(2) Uani 1 1 d . . . C32 C 0.4603(13) 0.2090(5) 0.7549(9) 0.078(4) Uani 1 1 d . . . H32A H 0.4795 0.1767 0.7210 0.117 Uiso 1 1 calc R . . H32B H 0.3797 0.2122 0.7436 0.117 Uiso 1 1 calc R . . H32C H 0.4913 0.2016 0.8167 0.117 Uiso 1 1 calc R . . N33 N 0.7703(6) 0.3534(3) 0.7058(5) 0.0416(16) Uani 1 1 d . . . C34 C 0.8632(8) 0.3475(4) 0.7310(6) 0.0415(18) Uani 1 1 d . . . C35 C 0.9843(9) 0.3398(6) 0.7608(9) 0.066(3) Uani 1 1 d . . . H35A H 1.0151 0.3322 0.7108 0.099 Uiso 1 1 calc R . . H35B H 1.0006 0.3069 0.8011 0.099 Uiso 1 1 calc R . . H35C H 1.0175 0.3754 0.7902 0.099 Uiso 1 1 calc R . . Sb1 Sb 0.05592(5) 0.52774(3) 0.80552(4) 0.05099(18) Uani 1 1 d . . . F11 F 0.0773(9) 0.4897(4) 0.9143(5) 0.097(3) Uani 1 1 d . . . F12 F 0.1409(7) 0.4710(3) 0.7654(5) 0.086(2) Uani 1 1 d . . . F13 F -0.0723(7) 0.4793(3) 0.7684(6) 0.087(2) Uani 1 1 d . . . F14 F -0.0325(7) 0.5827(3) 0.8469(6) 0.085(2) Uani 1 1 d . . . F15 F 0.1750(7) 0.5769(5) 0.8439(8) 0.116(4) Uani 1 1 d U . . F16 F 0.0207(9) 0.5642(4) 0.6969(5) 0.098(3) Uani 1 1 d . . . Sb2 Sb 0.07912(7) 0.23155(4) 0.54899(5) 0.0664(2) Uani 1 1 d D . . F21 F 0.0206(12) 0.2090(5) 0.6430(7) 0.126(5) Uani 0.748(14) 1 d PDU A 1 F22 F 0.0740(13) 0.3089(4) 0.5828(9) 0.149(7) Uani 0.748(14) 1 d PDU A 1 F23 F 0.2193(9) 0.2214(7) 0.6145(9) 0.162(8) Uani 0.748(14) 1 d PDU A 1 F24 F 0.0715(12) 0.1522(4) 0.5152(7) 0.121(5) Uani 0.748(14) 1 d PDU A 1 F25 F -0.0681(8) 0.2403(6) 0.4808(8) 0.123(5) Uani 0.748(14) 1 d PDU A 1 F26 F 0.1286(11) 0.2520(6) 0.4526(7) 0.134(6) Uani 0.748(14) 1 d PDU A 1 F21' F 0.095(3) 0.2231(14) 0.6681(9) 0.119(15) Uiso 0.252(14) 1 d PD A 2 F22' F -0.017(2) 0.2937(11) 0.547(2) 0.15(2) Uiso 0.252(14) 1 d PD A 2 F23' F 0.199(2) 0.2825(12) 0.570(2) 0.16(2) Uiso 0.252(14) 1 d PD A 2 F24' F 0.177(2) 0.1684(10) 0.5517(19) 0.102(12) Uiso 0.252(14) 1 d PD A 2 F25' F -0.039(2) 0.1793(13) 0.528(2) 0.21(3) Uiso 0.252(14) 1 d PD A 2 F26' F 0.065(3) 0.2386(14) 0.4302(9) 0.14(2) Uiso 0.252(14) 1 d PD A 2 C40 C 0.8251(11) 0.1265(6) 0.3533(11) 0.086(4) Uani 1 1 d . . . H40A H 0.9025 0.1376 0.3805 0.103 Uiso 1 1 calc R . . H40B H 0.8259 0.0869 0.3288 0.103 Uiso 1 1 calc R . . Cl1 Cl 0.7718(3) 0.17452(18) 0.2704(2) 0.0824(9) Uani 1 1 d . . . Cl2 Cl 0.7496(5) 0.1250(2) 0.4336(3) 0.1136(16) 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 Fe 0.0345(5) 0.0267(5) 0.0389(6) 0.0011(4) 0.0159(4) -0.0011(4) N1 0.029(3) 0.031(3) 0.041(3) 0.004(3) 0.010(3) -0.003(3) C2 0.043(4) 0.025(3) 0.041(4) 0.002(3) 0.015(3) -0.001(3) C3 0.049(5) 0.041(4) 0.045(5) 0.003(4) 0.016(4) -0.009(4) C4 0.051(5) 0.053(5) 0.059(5) 0.004(4) 0.029(4) -0.015(4) C5 0.056(6) 0.047(5) 0.049(5) 0.008(4) 0.030(4) 0.002(4) C6 0.037(4) 0.032(4) 0.042(4) 0.003(3) 0.014(3) 0.004(3) C7 0.033(4) 0.030(4) 0.040(4) 0.003(3) 0.009(3) 0.002(3) N7 0.037(4) 0.034(3) 0.038(3) 0.004(3) 0.009(3) 0.007(3) C8 0.048(5) 0.032(4) 0.059(5) -0.003(4) 0.014(4) -0.006(4) C9 0.046(5) 0.038(4) 0.042(4) -0.006(3) 0.018(4) -0.003(4) N9 0.047(4) 0.033(3) 0.039(3) 0.001(3) 0.015(3) -0.004(3) C10 0.072(7) 0.046(5) 0.060(6) -0.012(4) 0.043(5) -0.003(5) C11 0.035(4) 0.028(4) 0.040(4) -0.003(3) 0.009(3) -0.001(3) C12 0.040(4) 0.044(5) 0.038(4) -0.011(3) 0.014(3) -0.006(4) C13 0.046(5) 0.048(5) 0.050(5) -0.016(4) 0.015(4) -0.006(4) C14 0.059(6) 0.050(5) 0.066(6) -0.020(5) 0.029(5) 0.001(5) C15 0.040(4) 0.043(5) 0.070(6) -0.016(4) 0.020(4) 0.005(4) C16 0.046(5) 0.030(4) 0.057(5) -0.003(4) 0.018(4) -0.004(4) C17 0.059(6) 0.048(5) 0.043(5) 0.001(4) 0.005(4) 0.002(4) C18 0.053(5) 0.043(5) 0.071(6) 0.006(4) 0.020(5) 0.015(4) C19 0.053(5) 0.029(4) 0.044(4) -0.007(3) 0.024(4) -0.002(3) C20 0.054(5) 0.041(5) 0.046(5) -0.008(4) 0.016(4) -0.006(4) C21 0.060(6) 0.061(6) 0.074(7) -0.018(6) 0.021(5) -0.019(5) C22 0.079(8) 0.045(5) 0.068(6) 0.001(5) 0.029(6) -0.022(5) C23 0.079(8) 0.032(4) 0.068(6) 0.002(4) 0.027(6) -0.001(5) C24 0.066(6) 0.029(4) 0.057(5) 0.002(4) 0.027(5) -0.006(4) C25 0.067(7) 0.062(6) 0.059(6) -0.006(5) -0.002(5) -0.008(5) C26 0.075(8) 0.042(5) 0.082(8) -0.006(5) 0.013(6) 0.016(5) N27 0.040(4) 0.044(4) 0.047(4) -0.001(3) 0.009(3) 0.002(3) C28 0.053(6) 0.054(5) 0.036(4) 0.006(4) 0.016(4) 0.006(4) C29 0.052(6) 0.098(10) 0.071(7) 0.017(7) 0.017(6) 0.008(6) N30 0.050(4) 0.045(4) 0.049(4) 0.008(3) 0.024(4) -0.005(3) C31 0.066(6) 0.042(5) 0.047(5) 0.004(4) 0.027(5) 0.000(4) C32 0.115(11) 0.038(5) 0.093(9) 0.022(6) 0.047(8) -0.014(6) N33 0.043(4) 0.039(4) 0.046(4) 0.005(3) 0.016(3) 0.006(3) C34 0.044(5) 0.035(4) 0.044(4) 0.002(3) 0.009(4) 0.003(3) C35 0.041(5) 0.069(7) 0.089(8) 0.006(6) 0.019(5) 0.019(5) Sb1 0.0503(3) 0.0520(4) 0.0540(3) -0.0051(3) 0.0191(3) 0.0082(3) F11 0.120(7) 0.107(6) 0.065(4) 0.013(4) 0.028(5) 0.034(6) F12 0.095(6) 0.078(5) 0.093(5) -0.024(4) 0.036(4) 0.024(4) F13 0.078(5) 0.062(4) 0.117(6) 0.008(4) 0.016(5) -0.009(4) F14 0.098(5) 0.061(4) 0.124(6) 0.006(4) 0.077(5) 0.018(4) F15 0.059(4) 0.121(7) 0.177(9) -0.077(7) 0.049(5) -0.040(5) F16 0.149(8) 0.072(5) 0.076(5) 0.022(4) 0.029(5) -0.008(5) Sb2 0.0740(5) 0.0609(4) 0.0646(4) -0.0065(4) 0.0176(4) -0.0102(4) F21 0.164(13) 0.130(10) 0.110(9) 0.008(8) 0.082(9) 0.000(10) F22 0.207(15) 0.070(7) 0.160(12) -0.039(7) 0.028(12) -0.019(9) F23 0.101(10) 0.207(16) 0.150(13) 0.035(12) -0.021(9) 0.001(10) F24 0.183(13) 0.074(7) 0.100(8) -0.020(6) 0.024(9) 0.025(8) F25 0.071(7) 0.137(11) 0.143(11) 0.009(9) -0.008(7) 0.006(7) F26 0.114(11) 0.195(14) 0.106(9) 0.075(9) 0.051(8) 0.029(10) C40 0.060(7) 0.076(8) 0.115(11) -0.034(8) 0.011(7) -0.004(6) Cl1 0.0663(18) 0.097(2) 0.087(2) 0.0026(18) 0.0243(16) -0.0017(17) Cl2 0.138(4) 0.124(3) 0.068(2) 0.007(2) 0.005(2) -0.042(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 Fe N30 2.112(7) . ? Fe N1 2.115(6) . ? Fe N27 2.149(8) . ? Fe N9 2.218(7) . ? Fe N7 2.222(7) . ? Fe N33 2.231(8) . ? N1 C6 1.339(11) . ? N1 C2 1.349(10) . ? C2 C3 1.390(12) . ? C2 C7 1.479(11) . ? C3 C4 1.358(13) . ? C4 C5 1.402(14) . ? C5 C6 1.381(12) . ? C6 C9 1.495(11) . ? C7 N7 1.283(11) . ? C7 C8 1.502(11) . ? N7 C11 1.449(10) . ? C9 N9 1.267(11) . ? C9 C10 1.525(11) . ? N9 C19 1.450(10) . ? C11 C12 1.385(12) . ? C11 C16 1.417(12) . ? C12 C13 1.404(13) . ? C12 C17 1.532(13) . ? C13 C14 1.373(15) . ? C14 C15 1.399(15) . ? C15 C16 1.408(13) . ? C16 C18 1.475(14) . ? C19 C20 1.394(14) . ? C19 C24 1.397(13) . ? C20 C21 1.413(14) . ? C20 C25 1.506(15) . ? C21 C22 1.363(17) . ? C22 C23 1.377(17) . ? C23 C24 1.397(13) . ? C24 C26 1.483(16) . ? N27 C28 1.134(12) . ? C28 C29 1.467(15) . ? N30 C31 1.128(12) . ? C31 C32 1.468(13) . ? N33 C34 1.126(12) . ? C34 C35 1.465(13) . ? Sb1 F15 1.827(7) . ? Sb1 F16 1.854(7) . ? Sb1 F12 1.866(7) . ? Sb1 F14 1.876(6) . ? Sb1 F11 1.879(8) . ? Sb1 F13 1.899(8) . ? Sb2 F23 1.801(10) . ? Sb2 F26 1.830(9) . ? Sb2 F22' 1.836(13) . ? Sb2 F22 1.839(9) . ? Sb2 F26' 1.845(13) . ? Sb2 F21' 1.848(13) . ? Sb2 F23' 1.848(13) . ? Sb2 F25' 1.850(13) . ? Sb2 F24' 1.868(13) . ? Sb2 F21 1.872(9) . ? Sb2 F24 1.874(9) . ? Sb2 F25 1.883(9) . ? C40 Cl1 1.704(17) . ? C40 Cl2 1.748(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N30 Fe N1 163.1(3) . . ? N30 Fe N27 86.0(3) . . ? N1 Fe N27 107.1(3) . . ? N30 Fe N9 94.6(3) . . ? N1 Fe N9 73.4(3) . . ? N27 Fe N9 97.7(3) . . ? N30 Fe N7 119.0(3) . . ? N1 Fe N7 73.8(3) . . ? N27 Fe N7 84.9(3) . . ? N9 Fe N7 146.4(3) . . ? N30 Fe N33 89.1(3) . . ? N1 Fe N33 79.5(3) . . ? N27 Fe N33 170.0(3) . . ? N9 Fe N33 91.4(3) . . ? N7 Fe N33 89.9(3) . . ? C6 N1 C2 121.2(7) . . ? C6 N1 Fe 118.3(5) . . ? C2 N1 Fe 117.3(5) . . ? N1 C2 C3 120.0(7) . . ? N1 C2 C7 114.3(7) . . ? C3 C2 C7 125.8(7) . . ? C4 C3 C2 119.0(8) . . ? C3 C4 C5 121.2(8) . . ? C6 C5 C4 117.1(8) . . ? N1 C6 C5 121.4(8) . . ? N1 C6 C9 113.3(7) . . ? C5 C6 C9 125.3(8) . . ? N7 C7 C2 116.1(7) . . ? N7 C7 C8 125.4(8) . . ? C2 C7 C8 118.5(7) . . ? C7 N7 C11 121.5(7) . . ? C7 N7 Fe 116.0(6) . . ? C11 N7 Fe 122.5(5) . . ? N9 C9 C6 116.1(7) . . ? N9 C9 C10 125.4(8) . . ? C6 C9 C10 118.5(7) . . ? C9 N9 C19 120.6(7) . . ? C9 N9 Fe 116.7(6) . . ? C19 N9 Fe 122.6(5) . . ? C12 C11 C16 122.0(8) . . ? C12 C11 N7 118.7(7) . . ? C16 C11 N7 119.3(7) . . ? C11 C12 C13 119.7(9) . . ? C11 C12 C17 121.1(8) . . ? C13 C12 C17 119.2(9) . . ? C14 C13 C12 119.5(10) . . ? C13 C14 C15 121.1(9) . . ? C14 C15 C16 120.8(9) . . ? C15 C16 C11 116.9(9) . . ? C15 C16 C18 119.0(9) . . ? C11 C16 C18 124.1(8) . . ? C20 C19 C24 123.1(8) . . ? C20 C19 N9 117.7(8) . . ? C24 C19 N9 119.0(8) . . ? C19 C20 C21 117.3(9) . . ? C19 C20 C25 124.0(9) . . ? C21 C20 C25 118.7(10) . . ? C22 C21 C20 120.4(11) . . ? C21 C22 C23 121.1(10) . . ? C22 C23 C24 121.2(10) . . ? C23 C24 C19 116.8(10) . . ? C23 C24 C26 120.7(10) . . ? C19 C24 C26 122.4(9) . . ? C28 N27 Fe 166.0(8) . . ? N27 C28 C29 179.3(12) . . ? C31 N30 Fe 165.3(8) . . ? N30 C31 C32 178.1(12) . . ? C34 N33 Fe 169.8(7) . . ? N33 C34 C35 178.1(11) . . ? F15 Sb1 F16 91.3(5) . . ? F15 Sb1 F12 93.4(4) . . ? F16 Sb1 F12 91.1(4) . . ? F15 Sb1 F14 88.3(4) . . ? F16 Sb1 F14 90.0(4) . . ? F12 Sb1 F14 178.0(4) . . ? F15 Sb1 F11 93.2(5) . . ? F16 Sb1 F11 174.7(5) . . ? F12 Sb1 F11 91.6(4) . . ? F14 Sb1 F11 87.2(4) . . ? F15 Sb1 F13 177.0(4) . . ? F16 Sb1 F13 89.1(4) . . ? F12 Sb1 F13 89.6(4) . . ? F14 Sb1 F13 88.8(4) . . ? F11 Sb1 F13 86.3(4) . . ? F23 Sb2 F26 92.2(5) . . ? F23 Sb2 F22' 129.3(11) . . ? F26 Sb2 F22' 97.7(11) . . ? F23 Sb2 F22 93.0(5) . . ? F26 Sb2 F22 92.3(5) . . ? F22' Sb2 F22 37.3(11) . . ? F23 Sb2 F26' 115.6(11) . . ? F26 Sb2 F26' 26.3(11) . . ? F22' Sb2 F26' 90.8(7) . . ? F22 Sb2 F26' 102.1(11) . . ? F23 Sb2 F21' 63.6(10) . . ? F26 Sb2 F21' 153.4(11) . . ? F22' Sb2 F21' 90.4(7) . . ? F22 Sb2 F21' 78.9(11) . . ? F26' Sb2 F21' 178.8(9) . . ? F23 Sb2 F23' 50.0(11) . . ? F26 Sb2 F23' 64.8(11) . . ? F22' Sb2 F23' 90.5(7) . . ? F22 Sb2 F23' 55.5(11) . . ? F26' Sb2 F23' 90.1(7) . . ? F21' Sb2 F23' 89.9(7) . . ? F23 Sb2 F25' 129.0(11) . . ? F26 Sb2 F25' 115.1(11) . . ? F22' Sb2 F25' 90.5(7) . . ? F22 Sb2 F25' 125.5(11) . . ? F26' Sb2 F25' 90.0(7) . . ? F21' Sb2 F25' 89.9(7) . . ? F23' Sb2 F25' 178.9(9) . . ? F23 Sb2 F24' 50.4(10) . . ? F26 Sb2 F24' 82.4(10) . . ? F22' Sb2 F24' 179.7(10) . . ? F22 Sb2 F24' 142.4(10) . . ? F26' Sb2 F24' 89.4(7) . . ? F21' Sb2 F24' 89.4(7) . . ? F23' Sb2 F24' 89.3(7) . . ? F25' Sb2 F24' 89.6(7) . . ? F23 Sb2 F21 90.9(5) . . ? F26 Sb2 F21 176.5(6) . . ? F22' Sb2 F21 81.5(11) . . ? F22 Sb2 F21 89.1(5) . . ? F26' Sb2 F21 150.3(11) . . ? F21' Sb2 F21 30.1(10) . . ? F23' Sb2 F21 118.5(11) . . ? F25' Sb2 F21 61.6(11) . . ? F24' Sb2 F21 98.4(10) . . ? F23 Sb2 F24 90.8(5) . . ? F26 Sb2 F24 90.7(5) . . ? F22' Sb2 F24 138.2(11) . . ? F22 Sb2 F24 175.1(6) . . ? F26' Sb2 F24 79.0(11) . . ? F21' Sb2 F24 100.1(10) . . ? F23' Sb2 F24 129.4(11) . . ? F25' Sb2 F24 49.6(11) . . ? F24' Sb2 F24 42.0(10) . . ? F21 Sb2 F24 87.7(5) . . ? F23 Sb2 F25 178.7(6) . . ? F26 Sb2 F25 88.4(5) . . ? F22' Sb2 F25 51.7(11) . . ? F22 Sb2 F25 88.2(5) . . ? F26' Sb2 F25 64.8(11) . . ? F21' Sb2 F25 116.1(10) . . ? F23' Sb2 F25 131.3(11) . . ? F25' Sb2 F25 49.7(11) . . ? F24' Sb2 F25 128.6(10) . . ? F21 Sb2 F25 88.5(5) . . ? F24 Sb2 F25 88.0(5) . . ? Cl1 C40 Cl2 113.2(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.947 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.081 #===END data_[Ru(2)(CH3CN)3](SbF6)2 _database_code_depnum_ccdc_archive 'CCDC 246559' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Ru(2)(CH3CN)3](SbF6)2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32.38 H38.75 Cl2.75 F12 N6 Ru Sb2' _chemical_formula_weight 1182.00 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' N N 0.0311 0.0180 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.823(3) _cell_length_b 37.885(3) _cell_length_c 15.047(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.268(15) _cell_angle_gamma 90.00 _cell_volume 8965.9(26) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.97 _cell_measurement_theta_max 23.93 _exptl_crystal_description prisms _exptl_crystal_colour 'Dark orange' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method ? _exptl_crystal_F_000 4606 _exptl_absorpt_coefficient_mu 14.420 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0916 _exptl_absorpt_correction_T_max 0.5502 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11865 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.1001 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 57.04 _reflns_number_total 11338 _reflns_number_observed 6871 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1352 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+74.5426P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000044(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9986 _refine_ls_number_parameters 1175 _refine_ls_number_restraints 2010 _refine_ls_R_factor_all 0.1341 _refine_ls_R_factor_obs 0.0693 _refine_ls_wR_factor_all 0.1972 _refine_ls_wR_factor_obs 0.1481 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_goodness_of_fit_obs 1.127 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.049 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.16898(6) 0.36499(2) 0.55546(7) 0.0300(3) Uani 1 d . . N1 N 0.2344(7) 0.3908(2) 0.6517(8) 0.040(3) Uani 1 d . . C2 C 0.3167(10) 0.3975(4) 0.6435(9) 0.042(4) Uani 1 d U . C3 C 0.3665(11) 0.4128(4) 0.7134(10) 0.053(4) Uani 1 d . . H3A H 0.4235(11) 0.4177(4) 0.7090(10) 0.063 Uiso 1 calc R . C4 C 0.3297(12) 0.4211(4) 0.7918(12) 0.068(5) Uani 1 d . . H4A H 0.3620(12) 0.4316(4) 0.8401(12) 0.081 Uiso 1 calc R . C5 C 0.2472(11) 0.4136(4) 0.7956(10) 0.057(4) Uani 1 d . . H5A H 0.2227(11) 0.4195(4) 0.8471(10) 0.068 Uiso 1 calc R . C6 C 0.1983(8) 0.3979(3) 0.7275(8) 0.031(3) Uani 1 d U . C7 C 0.3434(9) 0.3869(4) 0.5576(9) 0.041(3) Uani 1 d U . N7 N 0.2837(7) 0.3723(3) 0.5005(7) 0.035(3) Uani 1 d . . C8 C 0.4323(10) 0.3937(5) 0.5366(13) 0.070(5) Uani 1 d . . H8A H 0.4714(11) 0.3886(30) 0.5884(27) 0.104 Uiso 1 calc R . H8B H 0.4378(23) 0.4179(9) 0.5199(78) 0.104 Uiso 1 calc R . H8C H 0.4446(28) 0.3787(23) 0.4881(54) 0.104 Uiso 1 calc R . C9 C 0.1070(10) 0.3870(3) 0.7180(11) 0.047(4) Uani 1 d . . N9 N 0.0783(7) 0.3716(3) 0.6475(6) 0.034(3) Uani 1 d U . C10 C 0.0581(12) 0.3957(5) 0.7996(11) 0.071(5) Uani 1 d . . H10A H 0.0474(72) 0.4206(7) 0.8013(50) 0.107 Uiso 1 calc R . H10B H 0.0918(35) 0.3887(30) 0.8537(12) 0.107 Uiso 1 calc R . H10C H 0.0051(36) 0.3832(26) 0.7943(43) 0.107 Uiso 1 calc R . C11 C 0.2998(9) 0.3659(3) 0.4100(9) 0.041(3) Uani 1 d . . C12 C 0.3001(11) 0.3949(4) 0.3525(11) 0.059(4) Uani 1 d . . C13 C 0.3082(14) 0.3879(7) 0.2634(14) 0.094(7) Uani 1 d . . H13A H 0.3081(14) 0.4064(7) 0.2228(14) 0.113 Uiso 1 calc R . C14 C 0.3163(17) 0.3533(7) 0.2342(15) 0.108(8) Uani 1 d . . H14A H 0.3199(17) 0.3490(7) 0.1739(15) 0.130 Uiso 1 calc R . C15 C 0.3189(14) 0.3265(6) 0.2903(15) 0.090(6) Uani 1 d U . H15A H 0.3258(14) 0.3038(6) 0.2689(15) 0.109 Uiso 1 calc R . C16 C 0.3116(11) 0.3315(4) 0.3822(12) 0.064(5) Uani 1 d . . C17 C 0.2963(13) 0.4328(5) 0.3809(12) 0.075(6) Uani 1 d . . H17A H 0.2891(89) 0.4339(5) 0.4434(24) 0.112 Uiso 1 calc R . H17B H 0.2491(52) 0.4442(10) 0.3469(65) 0.112 Uiso 1 calc R . H17C H 0.3481(36) 0.4445(10) 0.3706(85) 0.112 Uiso 1 calc R . C18 C 0.3196(13) 0.3011(4) 0.4450(14) 0.080(6) Uani 1 d . . H18A H 0.3673(55) 0.3048(18) 0.4892(58) 0.121 Uiso 1 calc R . H18B H 0.3280(91) 0.2798(7) 0.4124(20) 0.121 Uiso 1 calc R . H18C H 0.2686(37) 0.2991(23) 0.4739(71) 0.121 Uiso 1 calc R . C19 C -0.0113(9) 0.3648(4) 0.6312(9) 0.042(3) Uani 1 d U . C20 C -0.0395(12) 0.3302(5) 0.6366(13) 0.071(5) Uani 1 d . . C21 C -0.1286(13) 0.3248(6) 0.6203(13) 0.082(6) Uani 1 d U . H21A H -0.1516(13) 0.3024(6) 0.6261(13) 0.098 Uiso 1 calc R . C22 C -0.1800(16) 0.3528(8) 0.5961(17) 0.107(8) Uani 1 d U . H22A H -0.2380(16) 0.3489(8) 0.5829(17) 0.128 Uiso 1 calc R . C23 C -0.1506(16) 0.3859(7) 0.5904(14) 0.100(7) Uani 1 d U . H23A H -0.1883(16) 0.4042(7) 0.5744(14) 0.120 Uiso 1 calc R . C24 C -0.0646(10) 0.3928(6) 0.6082(12) 0.068(5) Uani 1 d . . C25 C 0.0228(14) 0.3013(4) 0.6661(15) 0.088(7) Uani 1 d . . H25A H 0.0572(64) 0.3085(16) 0.7195(56) 0.132 Uiso 1 calc R . H25B H 0.0587(64) 0.2969(27) 0.6197(42) 0.132 Uiso 1 calc R . H25C H -0.0075(14) 0.2802(12) 0.6777(97) 0.132 Uiso 1 calc R . C26 C -0.0383(14) 0.4312(5) 0.6094(13) 0.092(7) Uani 1 d U . H26A H 0.0171(44) 0.4333(7) 0.5894(101) 0.137 Uiso 1 calc R . H26B H -0.0366(98) 0.4403(13) 0.6692(23) 0.137 Uiso 1 calc R . H26C H -0.0785(56) 0.4445(9) 0.5704(81) 0.137 Uiso 1 calc R . N27 N 0.2162(7) 0.3214(3) 0.6208(8) 0.044(3) Uani 1 d . . C28 C 0.2427(11) 0.2978(4) 0.6582(12) 0.060(5) Uani 1 d . . C29 C 0.2824(14) 0.2668(4) 0.7045(14) 0.087(7) Uani 1 d . . H29A H 0.3254(66) 0.2745(5) 0.7504(67) 0.131 Uiso 1 calc R . H29B H 0.3078(83) 0.2523(21) 0.6624(24) 0.131 Uiso 1 calc R . H29C H 0.2399(22) 0.2535(22) 0.7309(85) 0.131 Uiso 1 calc R . N30 N 0.1100(7) 0.3340(3) 0.4555(8) 0.041(3) Uani 1 d . . C31 C 0.0907(10) 0.3171(4) 0.3945(12) 0.057(4) Uani 1 d . . C32 C 0.0642(15) 0.2943(5) 0.3172(13) 0.093(7) Uani 1 d . . H32A H 0.0676(96) 0.3073(14) 0.2630(13) 0.140 Uiso 1 calc R . H32B H 0.0068(36) 0.2866(33) 0.3200(56) 0.140 Uiso 1 calc R . H32C H 0.1010(63) 0.2741(22) 0.3184(60) 0.140 Uiso 1 calc R . N33 N 0.1211(7) 0.4074(3) 0.4853(8) 0.041(3) Uani 1 d . . C34 C 0.0949(11) 0.4301(4) 0.4458(11) 0.059(4) Uani 1 d . . C35 C 0.0585(17) 0.4607(5) 0.3955(15) 0.106(8) Uani 1 d . . H35A H 0.0930(63) 0.4665(29) 0.3489(75) 0.158 Uiso 1 calc R . H35B H 0.0566(104) 0.4805(14) 0.4350(28) 0.158 Uiso 1 calc R . H35C H 0.0019(44) 0.4552(17) 0.3695(98) 0.158 Uiso 1 calc R . Ru' Ru 0.69483(6) 0.12686(2) 0.59957(7) 0.0318(3) Uani 1 d . . N1' N 0.7441(6) 0.1334(2) 0.4914(6) 0.028(2) Uani 1 d U . C2' C 0.8149(9) 0.1526(3) 0.4871(10) 0.042(4) Uani 1 d . . C3' C 0.8562(10) 0.1539(4) 0.4072(10) 0.051(4) Uani 1 d . . H3'A H 0.9069(10) 0.1661(4) 0.4052(10) 0.061 Uiso 1 calc R . C4' C 0.8183(11) 0.1364(4) 0.3339(10) 0.061(5) Uani 1 d . . H4'A H 0.8418(11) 0.1376(4) 0.2800(10) 0.074 Uiso 1 calc R . C5' C 0.7463(10) 0.1173(4) 0.3395(9) 0.049(4) Uani 1 d U . H5'A H 0.7229(10) 0.1045(4) 0.2900(9) 0.058 Uiso 1 calc R . C6' C 0.7082(8) 0.1166(3) 0.4149(7) 0.024(3) Uani 1 d U . C7' C 0.8436(9) 0.1693(3) 0.5752(10) 0.042(4) Uani 1 d . . N7' N 0.7928(7) 0.1629(3) 0.6388(7) 0.038(3) Uani 1 d . . C8' C 0.9193(11) 0.1926(4) 0.5822(12) 0.068(5) Uani 1 d . . H8'1 H 0.9205(42) 0.2055(24) 0.5275(32) 0.102 Uiso 1 calc R . H8'2 H 0.9698(11) 0.1785(5) 0.5929(82) 0.102 Uiso 1 calc R . H8'3 H 0.9167(41) 0.2088(22) 0.6308(53) 0.102 Uiso 1 calc R . C9' C 0.6351(8) 0.0951(3) 0.4309(8) 0.026(3) Uani 1 d U . N9' N 0.6141(7) 0.0962(3) 0.5115(8) 0.040(3) Uani 1 d . . C10' C 0.5854(10) 0.0744(4) 0.3583(9) 0.052(4) Uani 1 d . . H10D H 0.6213(20) 0.0568(17) 0.3363(46) 0.078 Uiso 1 calc R . H10E H 0.5649(54) 0.0900(6) 0.3105(30) 0.078 Uiso 1 calc R . H10F H 0.5381(37) 0.0632(21) 0.3817(19) 0.078 Uiso 1 calc R . C11' C 0.8075(10) 0.1838(4) 0.7151(10) 0.048(4) Uani 1 d . . C12' C 0.7845(12) 0.2198(5) 0.7139(14) 0.068(5) Uani 1 d . . C13' C 0.7969(16) 0.2399(6) 0.7898(18) 0.102(8) Uani 1 d . . H13B H 0.7827(16) 0.2637(6) 0.7884(18) 0.123 Uiso 1 calc R . C14' C 0.8307(18) 0.2242(7) 0.8678(19) 0.116(8) Uani 1 d U . H14B H 0.8397(18) 0.2384(7) 0.9185(19) 0.139 Uiso 1 calc R . C15' C 0.8520(15) 0.1896(6) 0.8762(13) 0.093(7) Uani 1 d U . H15B H 0.8747(15) 0.1801(6) 0.9306(13) 0.111 Uiso 1 calc R . C16' C 0.8376(11) 0.1680(5) 0.7957(11) 0.067(5) Uani 1 d . . C17' C 0.7479(15) 0.2370(5) 0.6279(19) 0.109(9) Uani 1 d . . H17D H 0.7294(105) 0.2191(5) 0.5849(44) 0.164 Uiso 1 calc R . H17E H 0.7907(35) 0.2513(37) 0.6051(64) 0.164 Uiso 1 calc R . H17F H 0.7004(70) 0.2515(37) 0.6389(30) 0.164 Uiso 1 calc R . C18' C 0.8632(15) 0.1284(6) 0.8043(11) 0.095(7) Uani 1 d . . H18D H 0.8155(33) 0.1139(6) 0.7825(98) 0.142 Uiso 1 calc R . H18E H 0.8803(98) 0.1228(12) 0.8659(18) 0.142 Uiso 1 calc R . H18F H 0.9096(68) 0.1239(11) 0.7697(87) 0.142 Uiso 1 calc R . C19' C 0.5383(10) 0.0780(4) 0.5358(11) 0.051(4) Uani 1 d . . C20' C 0.5502(17) 0.0448(6) 0.5780(13) 0.091(8) Uani 1 d . . C21' C 0.4748(22) 0.0289(7) 0.6072(19) 0.125(9) Uani 1 d U . H21B H 0.4778(22) 0.0073(7) 0.6366(19) 0.150 Uiso 1 calc R . C22' C 0.4029(19) 0.0454(7) 0.5914(17) 0.110(8) Uani 1 d U . H22B H 0.3556(19) 0.0338(7) 0.6090(17) 0.132 Uiso 1 calc R . C23' C 0.3881(14) 0.0777(7) 0.5521(16) 0.098(7) Uani 1 d U . H23B H 0.3343(14) 0.0880(7) 0.5467(16) 0.118 Uiso 1 calc R . C24' C 0.4586(13) 0.0950(6) 0.5199(14) 0.083(7) Uani 1 d . . C25' C 0.6324(18) 0.0261(5) 0.5875(15) 0.108(9) Uani 1 d U . H25D H 0.6236(23) 0.0018(12) 0.6023(118) 0.162 Uiso 1 calc R . H25E H 0.6699(42) 0.0369(30) 0.6341(80) 0.162 Uiso 1 calc R . H25F H 0.6573(56) 0.0274(40) 0.5321(38) 0.162 Uiso 1 calc R . C26' C 0.4451(12) 0.1290(6) 0.4699(18) 0.105(8) Uani 1 d U . H26D H 0.4387(111) 0.1478(9) 0.5113(21) 0.157 Uiso 1 calc R . H26E H 0.3948(63) 0.1273(17) 0.4283(85) 0.157 Uiso 1 calc R . H26F H 0.4933(52) 0.1337(24) 0.4380(94) 0.157 Uiso 1 calc R . N27' N 0.7780(8) 0.0866(3) 0.6209(7) 0.038(3) Uani 1 d . . C28' C 0.8252(11) 0.0650(4) 0.6299(11) 0.054(4) Uani 1 d . . C29' C 0.8838(14) 0.0335(5) 0.6390(12) 0.088(7) Uani 1 d U . H29D H 0.8791(72) 0.0206(23) 0.5837(36) 0.132 Uiso 1 calc R . H29E H 0.8683(64) 0.0184(21) 0.6859(71) 0.132 Uiso 1 calc R . H29F H 0.9414(18) 0.0413(6) 0.6533(99) 0.132 Uiso 1 calc R . N30' N 0.6404(8) 0.1143(3) 0.7104(8) 0.046(3) Uani 1 d U . C31' C 0.6042(12) 0.1040(5) 0.7673(11) 0.065(5) Uani 1 d U . C32' C 0.5521(16) 0.0890(7) 0.8333(17) 0.132(11) Uani 1 d . . H32D H 0.4963(44) 0.0993(43) 0.8252(96) 0.197 Uiso 1 calc R . H32E H 0.5782(73) 0.0940(49) 0.8925(17) 0.197 Uiso 1 calc R . H32F H 0.5478(117) 0.0639(10) 0.8250(96) 0.197 Uiso 1 calc R . N33' N 0.6117(7) 0.1675(3) 0.5786(7) 0.036(3) Uani 1 d . . C34' C 0.5671(12) 0.1898(4) 0.5676(13) 0.068(5) Uani 1 d . . C35' C 0.5017(15) 0.2182(5) 0.5503(17) 0.106(8) Uani 1 d . . H35D H 0.4816(80) 0.2187(30) 0.4878(24) 0.160 Uiso 1 calc R . H35E H 0.5265(34) 0.2406(8) 0.5679(109) 0.160 Uiso 1 calc R . H35F H 0.4549(53) 0.2135(25) 0.5842(90) 0.160 Uiso 1 calc R . Sb10 Sb 0.84646(8) 0.01487(3) 0.35172(9) 0.0688(4) Uani 1 d D . F11 F 0.8060(14) 0.0416(5) 0.2546(10) 0.133(9) Uani 0.60 d PDU 1 F12 F 0.7545(12) 0.0272(5) 0.4045(16) 0.172(15) Uani 0.60 d PD 1 F13 F 0.9008(14) 0.0540(5) 0.4003(16) 0.183(14) Uani 0.60 d PD 1 F14 F 0.9398(12) 0.0049(7) 0.2959(15) 0.175(13) Uani 0.60 d PD 1 F15 F 0.7924(15) -0.0231(5) 0.2998(16) 0.186(14) Uani 0.60 d PD 1 F16 F 0.8877(16) -0.0112(5) 0.4460(11) 0.145(10) Uani 0.60 d PDU 1 F11' F 0.8651(20) 0.0500(6) 0.2771(17) 0.120(13) Uiso 0.40 d PD 2 F12' F 0.7389(13) 0.0099(9) 0.2971(21) 0.208(22) Uiso 0.40 d PD 2 F13' F 0.8073(19) 0.0463(6) 0.4289(15) 0.097(9) Uiso 0.40 d PD 2 F14' F 0.9516(13) 0.0197(9) 0.4098(22) 0.237(26) Uiso 0.40 d PD 2 F15' F 0.8842(21) -0.0174(6) 0.2792(17) 0.117(11) Uiso 0.40 d PD 2 F16' F 0.8240(21) -0.0203(6) 0.4294(18) 0.138(15) Uiso 0.40 d PD 2 Sb20 Sb 0.77084(8) 0.01051(3) 0.88155(8) 0.0660(4) Uani 1 d D . F21 F 0.7385(14) 0.0045(6) 0.7645(9) 0.117(8) Uani 0.55 d PDU 1 F22 F 0.8417(16) -0.0260(5) 0.8811(15) 0.187(14) Uani 0.55 d PDU 1 F23 F 0.6856(15) -0.0184(7) 0.9100(14) 0.171(13) Uani 0.55 d PDU 1 F24 F 0.6979(16) 0.0473(6) 0.8846(18) 0.256(20) Uani 0.55 d PDU 1 F25 F 0.8544(15) 0.0406(6) 0.8575(16) 0.206(21) Uani 0.55 d PD 1 F26 F 0.8013(12) 0.0166(5) 1.0012(9) 0.083(5) Uani 0.55 d PDU 1 F21' F 0.6706(13) 0.0113(7) 0.8137(17) 0.163(14) Uiso 0.45 d PD 2 F22' F 0.8129(16) -0.0191(6) 0.8010(16) 0.123(10) Uiso 0.45 d PD 2 F23' F 0.7366(16) -0.0279(5) 0.9392(15) 0.103(10) Uiso 0.45 d PD 2 F24' F 0.7333(18) 0.0395(6) 0.9608(17) 0.148(13) Uiso 0.45 d PD 2 F25' F 0.8073(18) 0.0475(6) 0.8193(18) 0.141(15) Uiso 0.45 d PD 2 F26' F 0.8741(13) 0.0080(8) 0.9470(18) 0.197(18) Uiso 0.45 d PD 2 Sb30 Sb 0.17405(9) 0.19812(3) 0.47598(9) 0.0747(4) Uani 1 d D . F31 F 0.0662(11) 0.1819(7) 0.4380(17) 0.111(10) Uani 0.50 d PDU 1 F32 F 0.2012(17) 0.1949(7) 0.3622(12) 0.155(11) Uani 0.50 d PDU 1 F33 F 0.2093(16) 0.1511(4) 0.4928(15) 0.114(8) Uani 0.50 d PDU 1 F34 F 0.1455(17) 0.1976(6) 0.5901(11) 0.112(8) Uani 0.50 d PDU 1 F35 F 0.1406(16) 0.2428(4) 0.4605(17) 0.138(9) Uani 0.50 d PDU 1 F36 F 0.2821(12) 0.2117(7) 0.5147(18) 0.138(12) Uani 0.50 d PDU 1 F31' F 0.0650(12) 0.1947(7) 0.4225(17) 0.126(11) Uani 0.50 d PDU 2 F32' F 0.2000(18) 0.1553(5) 0.4389(18) 0.164(12) Uani 0.50 d PDU 2 F33' F 0.1378(16) 0.1807(6) 0.5795(12) 0.102(8) Uani 0.50 d PDU 2 F34' F 0.1467(16) 0.2430(4) 0.5188(16) 0.124(9) Uani 0.50 d PDU 2 F35' F 0.2061(16) 0.2195(6) 0.3779(13) 0.136(10) Uani 0.50 d PDU 2 F36' F 0.2810(11) 0.2032(7) 0.5342(17) 0.124(10) Uani 0.50 d PDU 2 Sb40 Sb 0.54032(11) 0.18914(3) 0.24709(11) 0.0923(5) Uani 1 d D . F41 F 0.4625(14) 0.1870(7) 0.1518(13) 0.194(14) Uani 0.65 d PDU 1 F42 F 0.6235(13) 0.1773(8) 0.1793(13) 0.189(13) Uani 0.65 d PD 1 F43 F 0.5258(18) 0.1439(4) 0.2715(18) 0.219(16) Uani 0.65 d PD 1 F44 F 0.4620(12) 0.2028(8) 0.3176(14) 0.190(13) Uani 0.65 d PD 1 F45 F 0.5609(19) 0.2351(4) 0.2225(16) 0.210(15) Uani 0.65 d PD 1 F46 F 0.6212(14) 0.1925(6) 0.3446(12) 0.178(13) Uani 0.65 d PD 1 F41' F 0.4905(28) 0.2266(9) 0.2942(26) 0.214(33) Uiso 0.35 d PD 2 F42' F 0.5824(24) 0.1754(10) 0.3570(15) 0.158(23) Uiso 0.35 d PD 2 F43' F 0.6321(20) 0.2144(11) 0.2336(28) 0.219(29) Uiso 0.35 d PD 2 F44' F 0.4926(23) 0.2025(10) 0.1370(16) 0.131(17) Uiso 0.35 d PD 2 F45' F 0.4435(20) 0.1638(12) 0.2593(29) 0.223(29) Uiso 0.35 d PD 2 F46' F 0.5843(27) 0.1511(8) 0.1989(24) 0.152(18) Uiso 0.35 d PD 2 C40 C 0.3714(13) -0.0276(5) 0.8896(17) 0.098(7) Uani 1 d . . H40A H 0.3654(13) -0.0195(5) 0.9497(17) 0.117 Uiso 1 calc R . H40B H 0.3245(13) -0.0180(5) 0.8500(17) 0.117 Uiso 1 calc R . Cl1 Cl 0.3660(3) -0.07289(14) 0.8869(4) 0.0845(14) Uani 1 d . . Cl2 Cl 0.4671(5) -0.0118(2) 0.8572(6) 0.142(3) Uani 1 d . . C50 C 0.1050(16) 0.1009(6) 0.6270(14) 0.102(8) Uani 1 d . . H50A H 0.1309(16) 0.0777(6) 0.6325(14) 0.122 Uiso 1 calc R . H50B H 0.1473(16) 0.1174(6) 0.6105(14) 0.122 Uiso 1 calc R . Cl3 Cl 0.0725(6) 0.1130(2) 0.7271(5) 0.144(3) Uani 1 d . . Cl4 Cl 0.0183(6) 0.1001(2) 0.5432(5) 0.140(3) Uani 1 d . . C60 C 0.3871(17) -0.1966(13) 0.1435(15) 0.126(16) Uani 0.60 d PDU 1 H60A H 0.3448(17) -0.1808(13) 0.1633(15) 0.151 Uiso 0.60 calc PR 1 H60B H 0.3738(17) -0.2205(13) 0.1609(15) 0.151 Uiso 0.60 calc PR 1 Cl5 Cl 0.4872(7) -0.1848(3) 0.1909(10) 0.141(5) Uani 0.60 d PD 1 Cl6 Cl 0.3868(13) -0.1940(5) 0.0275(10) 0.195(7) Uani 0.60 d PD 1 C60' C 0.4087(190) -0.2029(26) 0.1016(46) 0.189(119) Uiso 0.15 d PD 2 H60C H 0.3667(190) -0.2217(26) 0.0962(46) 0.227 Uiso 0.15 calc PR 2 H60D H 0.4600(190) -0.2113(26) 0.0785(46) 0.227 Uiso 0.15 calc PR 2 Cl5' Cl 0.4303(28) -0.1895(9) 0.2131(24) 0.088(10) Uiso 0.15 d PD 2 Cl6' Cl 0.3693(43) -0.1652(18) 0.0437(33) 0.162(23) Uiso 0.15 d PD 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0290(6) 0.0290(5) 0.0318(6) 0.0026(4) 0.0020(4) -0.0042(4) N1 0.036(7) 0.028(5) 0.055(8) 0.006(5) 0.003(6) -0.010(5) C2 0.057(10) 0.049(7) 0.018(8) 0.005(6) -0.010(7) -0.005(7) C3 0.055(11) 0.060(9) 0.042(10) 0.002(7) -0.004(8) -0.007(8) C4 0.064(13) 0.070(11) 0.061(13) -0.010(9) -0.028(10) -0.001(9) C5 0.055(12) 0.080(11) 0.032(9) -0.006(8) -0.010(8) -0.010(9) C6 0.035(5) 0.035(4) 0.024(5) 0.001(4) 0.011(4) 0.001(4) C7 0.048(9) 0.056(8) 0.021(8) -0.004(6) 0.015(6) -0.002(7) N7 0.047(7) 0.038(6) 0.023(7) -0.005(5) 0.014(5) -0.005(5) C8 0.041(10) 0.091(12) 0.081(13) 0.000(10) 0.026(10) -0.026(9) C9 0.053(10) 0.034(7) 0.055(11) 0.009(7) 0.009(8) 0.012(7) N9 0.054(7) 0.033(5) 0.015(6) 0.005(4) 0.001(5) -0.011(5) C10 0.077(13) 0.099(13) 0.047(11) 0.003(9) 0.046(10) 0.015(10) C11 0.040(8) 0.047(8) 0.034(9) -0.003(7) -0.004(6) -0.018(7) C12 0.067(12) 0.075(11) 0.036(11) 0.004(8) 0.013(8) -0.013(9) C13 0.104(18) 0.127(19) 0.053(15) 0.010(12) 0.016(12) -0.047(15) C14 0.143(24) 0.132(21) 0.054(15) -0.011(14) 0.028(14) -0.039(18) C15 0.110(14) 0.088(12) 0.081(13) -0.036(10) 0.041(11) -0.031(11) C16 0.061(12) 0.073(11) 0.061(12) -0.016(9) 0.022(9) -0.036(9) C17 0.086(15) 0.080(12) 0.061(13) 0.030(10) 0.019(11) -0.002(10) C18 0.095(15) 0.049(9) 0.108(16) -0.012(10) 0.058(13) -0.011(9) C19 0.037(8) 0.067(8) 0.025(7) -0.006(6) 0.017(6) -0.011(7) C20 0.057(12) 0.085(13) 0.076(13) -0.014(10) 0.023(10) -0.029(10) C21 0.086(12) 0.102(12) 0.065(11) -0.038(9) 0.044(10) -0.044(10) C22 0.077(13) 0.146(16) 0.099(14) -0.034(13) 0.015(12) -0.016(13) C23 0.094(14) 0.141(15) 0.068(12) -0.003(11) 0.017(11) 0.026(12) C24 0.023(9) 0.120(16) 0.063(12) -0.004(10) 0.013(8) 0.016(9) C25 0.115(18) 0.042(9) 0.115(17) 0.012(10) 0.046(15) -0.014(10) C26 0.103(16) 0.112(15) 0.068(13) 0.040(11) 0.051(12) 0.050(13) N27 0.036(7) 0.046(7) 0.049(8) 0.003(6) -0.001(6) 0.000(6) C28 0.068(12) 0.037(8) 0.078(13) 0.009(8) 0.021(10) 0.002(8) C29 0.106(17) 0.062(11) 0.093(15) 0.020(10) 0.006(13) 0.036(11) N30 0.040(7) 0.045(7) 0.039(8) 0.000(6) 0.009(6) -0.005(6) C31 0.041(10) 0.046(9) 0.076(13) 0.002(9) -0.030(9) 0.010(7) C32 0.114(19) 0.078(13) 0.080(15) -0.044(11) -0.024(13) 0.000(12) N33 0.026(7) 0.040(6) 0.051(8) 0.011(6) -0.020(6) -0.007(5) C34 0.068(12) 0.055(10) 0.053(11) 0.013(8) 0.004(9) 0.005(9) C35 0.153(24) 0.072(12) 0.088(16) 0.043(12) -0.003(16) 0.031(14) Ru' 0.0313(6) 0.0383(5) 0.0269(6) 0.0001(4) 0.0085(4) -0.0043(4) N1' 0.028(4) 0.034(4) 0.020(4) -0.005(3) 0.000(3) 0.001(3) C2' 0.031(8) 0.043(7) 0.050(10) 0.012(7) 0.004(7) 0.002(6) C3' 0.046(10) 0.073(10) 0.036(10) 0.003(8) 0.015(8) -0.023(8) C4' 0.069(12) 0.092(12) 0.028(10) 0.015(8) 0.027(8) -0.009(10) C5' 0.057(9) 0.065(8) 0.023(8) 0.016(6) 0.003(7) -0.002(7) C6' 0.031(5) 0.031(4) 0.013(4) 0.003(3) 0.009(4) 0.002(4) C7' 0.038(9) 0.048(8) 0.043(10) -0.008(7) 0.014(7) -0.002(6) N7' 0.037(7) 0.059(7) 0.018(6) -0.011(5) 0.006(5) -0.008(5) C8' 0.056(11) 0.076(11) 0.074(13) -0.005(9) 0.013(10) -0.027(9) C9' 0.035(5) 0.031(4) 0.015(5) 0.001(3) 0.010(4) -0.002(4) N9' 0.040(7) 0.034(6) 0.045(8) 0.010(5) -0.004(6) -0.012(5) C10' 0.058(11) 0.063(9) 0.032(9) -0.017(7) -0.007(8) -0.009(8) C11' 0.061(11) 0.064(9) 0.025(9) -0.011(7) 0.027(8) -0.027(8) C12' 0.065(13) 0.061(11) 0.083(14) -0.024(10) 0.031(11) -0.026(9) C13' 0.105(20) 0.086(15) 0.116(21) -0.034(14) 0.013(16) -0.037(14) C14' 0.133(17) 0.116(15) 0.101(15) -0.051(13) 0.022(13) -0.022(13) C15' 0.108(14) 0.139(14) 0.036(10) -0.004(10) 0.024(10) -0.024(12) C16' 0.047(11) 0.116(15) 0.038(11) -0.003(10) 0.006(8) -0.038(10) C17' 0.096(18) 0.055(11) 0.180(28) -0.023(14) 0.030(19) -0.007(11) C18' 0.133(20) 0.131(19) 0.021(10) 0.006(10) 0.017(11) -0.017(15) C19' 0.047(10) 0.059(9) 0.052(10) -0.017(7) 0.023(8) -0.027(8) C20' 0.133(21) 0.088(14) 0.055(13) -0.019(11) 0.022(13) -0.069(15) C21' 0.153(18) 0.104(14) 0.118(16) 0.006(12) 0.012(15) -0.050(14) C22' 0.113(15) 0.120(15) 0.104(15) -0.029(12) 0.042(13) -0.061(13) C23' 0.068(12) 0.127(14) 0.105(14) -0.068(12) 0.034(11) -0.015(11) C24' 0.067(14) 0.111(16) 0.079(14) -0.058(12) 0.038(12) -0.048(12) C25' 0.165(23) 0.066(12) 0.083(15) 0.038(11) -0.030(15) -0.033(14) C26' 0.041(11) 0.101(15) 0.167(21) -0.036(15) -0.011(13) -0.003(11) N27' 0.045(8) 0.052(7) 0.019(6) 0.012(5) 0.007(5) 0.005(6) C28' 0.050(11) 0.066(10) 0.051(11) -0.015(8) 0.022(9) -0.007(9) C29' 0.118(17) 0.102(13) 0.051(12) 0.041(10) 0.039(11) 0.058(12) N30' 0.044(7) 0.074(8) 0.022(7) -0.022(5) 0.009(6) 0.000(6) C31' 0.076(11) 0.089(10) 0.036(10) -0.014(8) 0.032(9) 0.016(9) C32' 0.135(22) 0.148(21) 0.132(23) 0.057(17) 0.105(19) 0.015(17) N33' 0.043(7) 0.038(6) 0.026(6) -0.009(5) -0.004(5) -0.001(6) C34' 0.061(12) 0.039(9) 0.103(15) -0.028(9) 0.005(11) 0.001(9) C35' 0.111(20) 0.066(12) 0.138(22) -0.001(13) -0.009(17) 0.025(12) Sb10 0.0628(8) 0.0735(7) 0.0705(8) -0.0152(6) 0.0088(6) 0.0122(6) F11 0.142(20) 0.202(21) 0.047(12) 0.070(13) -0.024(12) 0.011(17) F12 0.126(21) 0.129(19) 0.291(41) -0.015(21) 0.150(26) -0.007(16) F13 0.154(28) 0.114(19) 0.258(37) -0.036(21) -0.089(26) -0.035(18) F14 0.083(18) 0.252(33) 0.202(32) 0.005(25) 0.078(20) 0.059(20) F15 0.164(29) 0.131(20) 0.245(36) -0.103(22) -0.056(26) -0.030(19) F16 0.219(28) 0.132(17) 0.078(14) 0.040(13) -0.013(16) 0.041(19) Sb20 0.0754(9) 0.0557(6) 0.0655(8) 0.0088(5) 0.0019(6) -0.0056(6) F21 0.132(16) 0.171(16) 0.044(10) 0.028(11) -0.005(11) -0.017(13) F22 0.264(32) 0.162(22) 0.134(22) 0.037(18) 0.015(22) 0.103(22) F23 0.163(25) 0.209(25) 0.145(23) 0.017(20) 0.037(20) -0.118(21) F24 0.229(32) 0.233(30) 0.301(36) 0.043(28) 0.008(28) 0.152(26) F25 0.216(44) 0.166(29) 0.266(49) 0.006(31) 0.158(42) -0.076(29) F26 0.102(10) 0.102(9) 0.046(8) -0.019(7) 0.019(7) -0.007(8) Sb30 0.0660(9) 0.0783(8) 0.0796(9) 0.0146(7) 0.0065(7) -0.0217(6) F31 0.077(16) 0.127(19) 0.130(21) -0.008(17) 0.010(15) -0.041(14) F32 0.159(20) 0.185(21) 0.123(18) 0.013(17) 0.032(16) -0.047(19) F33 0.140(19) 0.106(16) 0.102(18) -0.002(14) 0.041(16) 0.024(15) F34 0.159(19) 0.108(16) 0.075(14) -0.014(12) 0.040(14) -0.020(15) F35 0.147(12) 0.130(12) 0.136(12) 0.020(9) 0.010(9) -0.005(9) F36 0.120(20) 0.151(20) 0.133(20) -0.004(17) -0.031(17) -0.041(17) F31' 0.138(22) 0.139(21) 0.100(18) 0.040(16) 0.011(17) -0.007(17) F32' 0.171(21) 0.139(19) 0.175(22) -0.041(18) -0.006(20) -0.004(18) F33' 0.111(11) 0.105(11) 0.092(11) 0.015(8) 0.019(8) -0.010(8) F34' 0.130(12) 0.121(11) 0.121(11) -0.016(8) 0.014(9) 0.008(9) F35' 0.165(21) 0.127(18) 0.118(19) 0.025(16) 0.030(17) -0.069(17) F36' 0.100(19) 0.129(19) 0.138(21) 0.023(17) -0.009(18) -0.015(16) Sb40 0.1090(13) 0.0671(8) 0.0989(11) 0.0225(7) 0.0033(9) -0.0061(8) F41 0.168(25) 0.231(27) 0.161(23) -0.007(20) -0.077(20) 0.002(23) F42 0.195(28) 0.306(37) 0.083(17) -0.029(20) 0.089(19) -0.018(27) F43 0.223(35) 0.091(16) 0.345(47) 0.088(22) 0.047(34) -0.022(19) F44 0.073(17) 0.322(42) 0.172(27) -0.002(30) 0.001(18) 0.021(23) F45 0.325(44) 0.097(16) 0.205(30) 0.090(18) 0.019(30) -0.034(22) F46 0.224(35) 0.161(24) 0.129(22) 0.008(18) -0.073(22) 0.005(25) C40 0.070(15) 0.100(15) 0.127(20) 0.005(14) 0.024(14) 0.027(12) Cl1 0.062(3) 0.102(3) 0.090(4) 0.002(3) 0.010(3) 0.005(3) Cl2 0.123(6) 0.114(5) 0.200(8) 0.006(5) 0.069(6) -0.013(4) C50 0.137(22) 0.095(15) 0.081(17) 0.010(12) 0.046(16) -0.002(14) Cl3 0.174(8) 0.151(6) 0.113(6) 0.016(5) 0.045(5) 0.013(5) Cl4 0.150(7) 0.146(6) 0.120(6) 0.021(5) -0.005(5) -0.028(5) C60 0.114(22) 0.138(22) 0.129(22) 0.000(17) 0.028(18) -0.016(17) Cl5 0.076(7) 0.133(9) 0.218(15) -0.020(9) 0.032(9) -0.016(7) Cl6 0.233(21) 0.208(17) 0.135(13) 0.010(12) -0.017(13) 0.062(15) _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 Ru N1 1.950(11) . ? Ru N27 2.021(12) . ? Ru N33 2.024(11) . ? Ru N30 2.050(13) . ? Ru N7 2.094(10) . ? Ru N9 2.115(10) . ? N1 C2 1.35(2) . ? N1 C6 1.36(2) . ? C2 C3 1.37(2) . ? C2 C7 1.46(2) . ? C3 C4 1.41(2) . ? C4 C5 1.34(2) . ? C5 C6 1.35(2) . ? C6 C9 1.50(2) . ? C7 N7 1.33(2) . ? C7 C8 1.50(2) . ? N7 C11 1.43(2) . ? C9 N9 1.25(2) . ? C9 C10 1.56(2) . ? N9 C19 1.43(2) . ? C11 C16 1.39(2) . ? C11 C12 1.40(2) . ? C12 C13 1.39(3) . ? C12 C17 1.50(2) . ? C13 C14 1.39(3) . ? C14 C15 1.32(3) . ? C15 C16 1.41(3) . ? C16 C18 1.48(2) . ? C19 C24 1.38(2) . ? C19 C20 1.39(2) . ? C20 C21 1.42(3) . ? C20 C25 1.51(3) . ? C21 C22 1.36(3) . ? C22 C23 1.34(3) . ? C23 C24 1.38(3) . ? C24 C26 1.51(3) . ? N27 C28 1.12(2) . ? C28 C29 1.47(2) . ? N30 C31 1.13(2) . ? C31 C32 1.47(2) . ? N33 C34 1.10(2) . ? C34 C35 1.47(2) . ? Ru' N1' 1.896(9) . ? Ru' N30' 2.015(12) . ? Ru' N27' 2.018(12) . ? Ru' N33' 2.028(12) . ? Ru' N9' 2.090(11) . ? Ru' N7' 2.101(11) . ? N1' C2' 1.34(2) . ? N1' C6' 1.381(15) . ? C2' C3' 1.43(2) . ? C2' C7' 1.49(2) . ? C3' C4' 1.37(2) . ? C4' C5' 1.36(2) . ? C5' C6' 1.34(2) . ? C6' C9' 1.45(2) . ? C7' N7' 1.34(2) . ? C7' C8' 1.48(2) . ? N7' C11' 1.39(2) . ? C9' N9' 1.29(2) . ? C9' C10' 1.50(2) . ? N9' C19' 1.46(2) . ? C11' C16' 1.39(2) . ? C11' C12' 1.41(2) . ? C12' C13' 1.37(3) . ? C12' C17' 1.51(3) . ? C13' C14' 1.37(3) . ? C14' C15' 1.36(3) . ? C15' C16' 1.46(3) . ? C16' C18' 1.56(3) . ? C19' C20' 1.41(3) . ? C19' C24' 1.41(3) . ? C20' C21' 1.45(3) . ? C20' C25' 1.47(3) . ? C21' C22' 1.30(4) . ? C22' C23' 1.37(3) . ? C23' C24' 1.42(3) . ? C24' C26' 1.49(3) . ? N27' C28' 1.10(2) . ? C28' C29' 1.51(2) . ? N30' C31' 1.15(2) . ? C31' C32' 1.47(2) . ? N33' C34' 1.10(2) . ? C34' C35' 1.50(3) . ? Sb10 F15' 1.79(2) . ? Sb10 F11' 1.79(2) . ? Sb10 F16 1.792(13) . ? Sb10 F12 1.794(13) . ? Sb10 F14' 1.80(2) . ? Sb10 F15 1.806(14) . ? Sb10 F12' 1.82(2) . ? Sb10 F14 1.817(13) . ? Sb10 F13' 1.82(2) . ? Sb10 F13 1.825(14) . ? Sb10 F16' 1.83(2) . ? Sb10 F11 1.835(12) . ? Sb20 F24' 1.77(2) . ? Sb20 F22 1.78(2) . ? Sb20 F21' 1.79(2) . ? Sb20 F21 1.794(14) . ? Sb20 F23' 1.81(2) . ? Sb20 F25 1.811(15) . ? Sb20 F25' 1.81(2) . ? Sb20 F24 1.81(2) . ? Sb20 F26' 1.82(2) . ? Sb20 F23 1.825(14) . ? Sb20 F26 1.826(13) . ? Sb20 F22' 1.83(2) . ? Sb30 F32' 1.78(2) . ? Sb30 F35 1.78(2) . ? Sb30 F35' 1.803(15) . ? Sb30 F32 1.81(2) . ? Sb30 F36 1.82(2) . ? Sb30 F34 1.822(14) . ? Sb30 F31' 1.83(2) . ? Sb30 F36' 1.83(2) . ? Sb30 F33' 1.840(15) . ? Sb30 F31 1.845(15) . ? Sb30 F33 1.874(15) . ? Sb30 F34' 1.887(15) . ? Sb40 F43' 1.77(2) . ? Sb40 F43 1.771(14) . ? Sb40 F41 1.787(15) . ? Sb40 F46' 1.79(2) . ? Sb40 F42' 1.79(2) . ? Sb40 F44 1.79(2) . ? Sb40 F41' 1.81(2) . ? Sb40 F42 1.806(14) . ? Sb40 F45 1.816(14) . ? Sb40 F44' 1.82(2) . ? Sb40 F45' 1.83(2) . ? Sb40 F46 1.843(15) . ? C40 Cl1 1.72(2) . ? C40 Cl2 1.74(2) . ? C50 Cl3 1.71(2) . ? C50 Cl4 1.76(3) . ? C60 Cl5 1.72(2) . ? C60 Cl6 1.75(2) . ? C60' Cl5' 1.75(2) . ? C60' Cl6' 1.75(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru N27 84.8(5) . . ? N1 Ru N33 97.3(4) . . ? N27 Ru N33 177.6(5) . . ? N1 Ru N30 174.1(5) . . ? N27 Ru N30 90.3(5) . . ? N33 Ru N30 87.5(5) . . ? N1 Ru N7 79.3(4) . . ? N27 Ru N7 90.6(4) . . ? N33 Ru N7 88.9(4) . . ? N30 Ru N7 97.5(4) . . ? N1 Ru N9 78.3(4) . . ? N27 Ru N9 91.1(4) . . ? N33 Ru N9 90.3(4) . . ? N30 Ru N9 105.1(4) . . ? N7 Ru N9 157.3(4) . . ? C2 N1 C6 122.7(12) . . ? C2 N1 Ru 117.9(9) . . ? C6 N1 Ru 119.0(9) . . ? N1 C2 C3 119.4(14) . . ? N1 C2 C7 113.9(12) . . ? C3 C2 C7 126.7(14) . . ? C2 C3 C4 118.8(15) . . ? C5 C4 C3 118.8(16) . . ? C4 C5 C6 122.5(16) . . ? C5 C6 N1 117.7(13) . . ? C5 C6 C9 131.3(13) . . ? N1 C6 C9 110.9(12) . . ? N7 C7 C2 115.8(12) . . ? N7 C7 C8 123.5(13) . . ? C2 C7 C8 120.6(14) . . ? C7 N7 C11 119.9(11) . . ? C7 N7 Ru 112.7(8) . . ? C11 N7 Ru 127.2(9) . . ? N9 C9 C6 117.8(13) . . ? N9 C9 C10 127.1(15) . . ? C6 C9 C10 115.1(14) . . ? C9 N9 C19 119.2(12) . . ? C9 N9 Ru 113.6(10) . . ? C19 N9 Ru 126.5(8) . . ? C16 C11 C12 122.7(14) . . ? C16 C11 N7 119.2(13) . . ? C12 C11 N7 118.0(12) . . ? C13 C12 C11 117.2(17) . . ? C13 C12 C17 117.9(17) . . ? C11 C12 C17 124.8(14) . . ? C12 C13 C14 120.4(20) . . ? C15 C14 C13 121.3(21) . . ? C14 C15 C16 121.7(20) . . ? C11 C16 C15 116.6(17) . . ? C11 C16 C18 122.7(15) . . ? C15 C16 C18 120.6(17) . . ? C24 C19 C20 123.3(15) . . ? C24 C19 N9 118.2(13) . . ? C20 C19 N9 118.4(14) . . ? C19 C20 C21 116.4(19) . . ? C19 C20 C25 119.8(16) . . ? C21 C20 C25 123.6(17) . . ? C22 C21 C20 119.1(20) . . ? C23 C22 C21 122.9(24) . . ? C22 C23 C24 120.4(24) . . ? C19 C24 C23 117.7(20) . . ? C19 C24 C26 125.3(16) . . ? C23 C24 C26 116.7(19) . . ? C28 N27 Ru 178.8(13) . . ? N27 C28 C29 176.4(18) . . ? C31 N30 Ru 168.1(13) . . ? N30 C31 C32 178.0(20) . . ? C34 N33 Ru 178.8(13) . . ? N33 C34 C35 178.2(19) . . ? N1' Ru' N30' 173.6(4) . . ? N1' Ru' N27' 85.0(4) . . ? N30' Ru' N27' 91.2(4) . . ? N1' Ru' N33' 95.1(4) . . ? N30' Ru' N33' 88.8(5) . . ? N27' Ru' N33' 179.7(5) . . ? N1' Ru' N9' 78.9(4) . . ? N30' Ru' N9' 96.2(4) . . ? N27' Ru' N9' 91.3(5) . . ? N33' Ru' N9' 89.0(4) . . ? N1' Ru' N7' 78.3(4) . . ? N30' Ru' N7' 106.8(4) . . ? N27' Ru' N7' 89.9(5) . . ? N33' Ru' N7' 89.8(4) . . ? N9' Ru' N7' 156.9(4) . . ? C2' N1' C6' 118.6(10) . . ? C2' N1' Ru' 122.3(9) . . ? C6' N1' Ru' 119.0(7) . . ? N1' C2' C3' 121.2(13) . . ? N1' C2' C7' 111.2(11) . . ? C3' C2' C7' 127.5(12) . . ? C4' C3' C2' 117.4(13) . . ? C5' C4' C3' 120.3(13) . . ? C6' C5' C4' 121.3(14) . . ? C5' C6' N1' 120.9(12) . . ? C5' C6' C9' 126.2(12) . . ? N1' C6' C9' 112.4(9) . . ? N7' C7' C8' 127.0(13) . . ? N7' C7' C2' 114.2(12) . . ? C8' C7' C2' 118.7(12) . . ? C7' N7' C11' 115.3(11) . . ? C7' N7' Ru' 113.6(8) . . ? C11' N7' Ru' 130.7(8) . . ? N9' C9' C6' 115.4(11) . . ? N9' C9' C10' 122.2(11) . . ? C6' C9' C10' 122.4(11) . . ? C9' N9' C19' 121.4(12) . . ? C9' N9' Ru' 114.2(8) . . ? C19' N9' Ru' 124.4(9) . . ? C16' C11' N7' 118.9(14) . . ? C16' C11' C12' 119.5(15) . . ? N7' C11' C12' 121.3(15) . . ? C13' C12' C11' 120.9(22) . . ? C13' C12' C17' 118.9(20) . . ? C11' C12' C17' 120.2(16) . . ? C12' C13' C14' 118.8(23) . . ? C15' C14' C13' 124.6(22) . . ? C14' C15' C16' 116.7(21) . . ? C11' C16' C15' 119.3(19) . . ? C11' C16' C18' 123.4(15) . . ? C15' C16' C18' 117.2(17) . . ? C20' C19' C24' 123.7(17) . . ? C20' C19' N9' 117.4(16) . . ? C24' C19' N9' 118.8(14) . . ? C19' C20' C21' 115.6(25) . . ? C19' C20' C25' 122.9(17) . . ? C21' C20' C25' 121.4(23) . . ? C22' C21' C20' 118.8(26) . . ? C21' C22' C23' 128.0(24) . . ? C22' C23' C24' 117.0(23) . . ? C19' C24' C23' 116.8(22) . . ? C19' C24' C26' 123.7(15) . . ? C23' C24' C26' 119.5(22) . . ? C28' N27' Ru' 177.2(11) . . ? N27' C28' C29' 175.1(19) . . ? C31' N30' Ru' 171.6(13) . . ? N30' C31' C32' 174.2(22) . . ? C34' N33' Ru' 179.4(12) . . ? N33' C34' C35' 175.9(19) . . ? F15' Sb10 F11' 92.1(9) . . ? F16 Sb10 F12 92.0(8) . . ? F15' Sb10 F14' 90.8(9) . . ? F11' Sb10 F14' 91.2(9) . . ? F16 Sb10 F15 91.1(8) . . ? F12 Sb10 F15 91.7(8) . . ? F15' Sb10 F12' 90.7(9) . . ? F11' Sb10 F12' 90.2(9) . . ? F14' Sb10 F12' 177.9(12) . . ? F16 Sb10 F14 90.4(8) . . ? F12 Sb10 F14 176.8(9) . . ? F15 Sb10 F14 90.3(8) . . ? F15' Sb10 F13' 177.6(10) . . ? F11' Sb10 F13' 90.3(8) . . ? F14' Sb10 F13' 89.1(9) . . ? F12' Sb10 F13' 89.3(9) . . ? F16 Sb10 F13 90.8(8) . . ? F12 Sb10 F13 88.9(8) . . ? F15 Sb10 F13 177.9(9) . . ? F14 Sb10 F13 89.0(8) . . ? F15' Sb10 F16' 89.6(9) . . ? F11' Sb10 F16' 177.9(10) . . ? F14' Sb10 F16' 89.9(9) . . ? F12' Sb10 F16' 88.6(9) . . ? F13' Sb10 F16' 88.0(8) . . ? F16 Sb10 F11 179.0(9) . . ? F12 Sb10 F11 88.9(8) . . ? F15 Sb10 F11 89.2(8) . . ? F14 Sb10 F11 88.7(7) . . ? F13 Sb10 F11 88.8(7) . . ? F24' Sb20 F21' 91.9(9) . . ? F22 Sb20 F21 90.6(8) . . ? F24' Sb20 F23' 92.1(9) . . ? F21' Sb20 F23' 89.6(9) . . ? F22 Sb20 F25 90.8(9) . . ? F21 Sb20 F25 91.1(8) . . ? F24' Sb20 F25' 91.0(9) . . ? F21' Sb20 F25' 90.3(9) . . ? F23' Sb20 F25' 176.9(10) . . ? F22 Sb20 F24 178.6(10) . . ? F21 Sb20 F24 90.5(8) . . ? F25 Sb20 F24 90.1(8) . . ? F24' Sb20 F26' 90.8(9) . . ? F21' Sb20 F26' 177.3(10) . . ? F23' Sb20 F26' 89.9(9) . . ? F25' Sb20 F26' 90.1(9) . . ? F22 Sb20 F23 91.0(8) . . ? F21 Sb20 F23 90.9(8) . . ? F25 Sb20 F23 177.3(10) . . ? F24 Sb20 F23 88.1(9) . . ? F22 Sb20 F26 90.2(7) . . ? F21 Sb20 F26 178.7(8) . . ? F25 Sb20 F26 89.9(8) . . ? F24 Sb20 F26 88.8(8) . . ? F23 Sb20 F26 88.1(7) . . ? F24' Sb20 F22' 178.3(11) . . ? F21' Sb20 F22' 89.8(9) . . ? F23' Sb20 F22' 88.4(8) . . ? F25' Sb20 F22' 88.4(8) . . ? F26' Sb20 F22' 87.5(9) . . ? F32' Sb30 F35' 93.3(9) . . ? F35 Sb30 F32 92.2(8) . . ? F35 Sb30 F36 91.7(8) . . ? F32 Sb30 F36 90.6(9) . . ? F35 Sb30 F34 91.9(8) . . ? F32 Sb30 F34 175.5(9) . . ? F36 Sb30 F34 91.3(8) . . ? F32' Sb30 F31' 92.1(9) . . ? F35' Sb30 F31' 90.5(8) . . ? F32' Sb30 F36' 90.8(9) . . ? F35' Sb30 F36' 90.9(8) . . ? F31' Sb30 F36' 176.7(10) . . ? F32' Sb30 F33' 92.4(8) . . ? F35' Sb30 F33' 174.3(9) . . ? F31' Sb30 F33' 88.9(8) . . ? F36' Sb30 F33' 89.4(8) . . ? F35 Sb30 F31 91.3(8) . . ? F32 Sb30 F31 89.5(8) . . ? F36 Sb30 F31 177.0(10) . . ? F34 Sb30 F31 88.4(8) . . ? F35 Sb30 F33 179.8(9) . . ? F32 Sb30 F33 88.0(8) . . ? F36 Sb30 F33 88.3(8) . . ? F34 Sb30 F33 87.9(7) . . ? F31 Sb30 F33 88.7(8) . . ? F32' Sb30 F34' 178.3(10) . . ? F35' Sb30 F34' 88.3(8) . . ? F31' Sb30 F34' 88.5(8) . . ? F36' Sb30 F34' 88.6(8) . . ? F33' Sb30 F34' 86.0(8) . . ? F43 Sb40 F41 91.7(8) . . ? F43' Sb40 F46' 91.6(10) . . ? F43' Sb40 F42' 92.1(10) . . ? F46' Sb40 F42' 91.0(10) . . ? F43 Sb40 F44 92.4(8) . . ? F41 Sb40 F44 91.6(8) . . ? F43' Sb40 F41' 91.2(10) . . ? F46' Sb40 F41' 177.0(12) . . ? F42' Sb40 F41' 90.0(10) . . ? F43 Sb40 F42 89.8(8) . . ? F41 Sb40 F42 91.0(8) . . ? F44 Sb40 F42 176.6(9) . . ? F43 Sb40 F45 177.1(10) . . ? F41 Sb40 F45 90.1(8) . . ? F44 Sb40 F45 89.7(8) . . ? F42 Sb40 F45 88.0(8) . . ? F43' Sb40 F44' 90.5(10) . . ? F46' Sb40 F44' 89.8(10) . . ? F42' Sb40 F44' 177.2(12) . . ? F41' Sb40 F44' 89.0(10) . . ? F43' Sb40 F45' 178.5(12) . . ? F46' Sb40 F45' 89.1(10) . . ? F42' Sb40 F45' 89.2(10) . . ? F41' Sb40 F45' 88.1(10) . . ? F44' Sb40 F45' 88.2(10) . . ? F43 Sb40 F46 89.8(8) . . ? F41 Sb40 F46 178.5(9) . . ? F44 Sb40 F46 88.5(8) . . ? F42 Sb40 F46 88.9(8) . . ? F45 Sb40 F46 88.4(8) . . ? Cl1 C40 Cl2 112.2(11) . . ? Cl3 C50 Cl4 110.6(14) . . ? Cl5 C60 Cl6 107.5(16) . . ? Cl5' C60' Cl6' 105.1(23) . . ? _refine_diff_density_max 0.693 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.136 #===END data_[Mn(2)(OTf)2(H2O)] _database_code_depnum_ccdc_archive 'CCDC 246560' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn(2)(OTf)2(H2O)]' _chemical_formula_sum 'C28 H31 Cl2 F6 Mn N3 O7 S2' _chemical_formula_weight 825.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9005(16) _cell_length_b 12.7266(16) _cell_length_c 22.4334(17) _cell_angle_alpha 90.00 _cell_angle_beta 91.068(8) _cell_angle_gamma 90.00 _cell_volume 3682.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.05 _cell_measurement_theta_max 12.50 _exptl_crystal_description prisms _exptl_crystal_colour Orange/yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1684 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.7439 _exptl_absorpt_correction_T_max 0.8198 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.94 _diffrn_reflns_number 6797 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6487 _reflns_number_gt 4511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6487 _refine_ls_number_parameters 469 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.022 _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 Mn Mn 0.44627(4) 0.32219(4) 0.64488(2) 0.02652(13) Uani 1 1 d . . . N1 N 0.4009(2) 0.16181(19) 0.62174(11) 0.0262(5) Uani 1 1 d . . . C2 C 0.4744(3) 0.0944(2) 0.60579(13) 0.0275(6) Uani 1 1 d . . . C3 C 0.4482(3) -0.0021(3) 0.58026(15) 0.0350(8) Uani 1 1 d . . . H3A H 0.5003 -0.0489 0.5684 0.042 Uiso 1 1 calc R . . C4 C 0.3455(3) -0.0281(3) 0.57257(17) 0.0397(8) Uani 1 1 d . . . H4A H 0.3269 -0.0931 0.5557 0.048 Uiso 1 1 calc R . . C5 C 0.2694(3) 0.0419(3) 0.58975(16) 0.0361(8) Uani 1 1 d . . . H5A H 0.1988 0.0247 0.5856 0.043 Uiso 1 1 calc R . . C6 C 0.3005(3) 0.1384(3) 0.61331(13) 0.0277(6) Uani 1 1 d . . . C7 C 0.5831(3) 0.1295(3) 0.61913(14) 0.0299(7) Uani 1 1 d . . . N7 N 0.5939(2) 0.2209(2) 0.64256(12) 0.0298(6) Uani 1 1 d . . . C8 C 0.6703(3) 0.0554(3) 0.6059(2) 0.0483(10) Uani 1 1 d . . . H8A H 0.7360 0.0896 0.6147 0.072 Uiso 1 1 calc R . . H8B H 0.6670 0.0356 0.5642 0.072 Uiso 1 1 calc R . . H8C H 0.6642 -0.0070 0.6305 0.072 Uiso 1 1 calc R . . C9 C 0.2268(3) 0.2229(2) 0.63224(14) 0.0276(6) Uani 1 1 d . . . N9 N 0.2690(2) 0.3092(2) 0.65014(12) 0.0287(6) Uani 1 1 d . . . C10 C 0.1127(3) 0.2008(3) 0.62910(18) 0.0401(8) Uani 1 1 d . . . H10A H 0.0747 0.2645 0.6380 0.060 Uiso 1 1 calc R . . H10B H 0.0959 0.1469 0.6579 0.060 Uiso 1 1 calc R . . H10C H 0.0937 0.1767 0.5893 0.060 Uiso 1 1 calc R . . C11 C 0.6947(3) 0.2547(3) 0.66423(17) 0.0378(8) Uani 1 1 d . . . C12 C 0.7490(3) 0.3297(3) 0.6315(2) 0.0500(10) Uani 1 1 d . . . C13 C 0.8438(4) 0.3648(4) 0.6554(3) 0.0726(16) Uani 1 1 d . . . H13A H 0.8824 0.4145 0.6341 0.087 Uiso 1 1 calc R . . C14 C 0.8815(4) 0.3290(5) 0.7086(3) 0.0793(18) Uani 1 1 d . . . H14A H 0.9449 0.3545 0.7239 0.095 Uiso 1 1 calc R . . C15 C 0.8261(4) 0.2546(5) 0.7403(3) 0.0692(15) Uani 1 1 d . . . H15A H 0.8534 0.2290 0.7766 0.083 Uiso 1 1 calc R . . C16 C 0.7315(3) 0.2175(4) 0.71936(19) 0.0490(10) Uani 1 1 d . . . C17 C 0.7091(4) 0.3679(4) 0.5722(3) 0.0682(14) Uani 1 1 d . . . H17A H 0.7040 0.3092 0.5447 0.102 Uiso 1 1 calc R . . H17B H 0.7563 0.4200 0.5566 0.102 Uiso 1 1 calc R . . H17C H 0.6411 0.3991 0.5769 0.102 Uiso 1 1 calc R . . C18 C 0.6718(4) 0.1385(4) 0.7553(2) 0.0602(12) Uani 1 1 d . . . H18A H 0.7079 0.1258 0.7929 0.090 Uiso 1 1 calc R . . H18B H 0.6659 0.0732 0.7332 0.090 Uiso 1 1 calc R . . H18C H 0.6030 0.1658 0.7629 0.090 Uiso 1 1 calc R . . C19 C 0.2078(2) 0.3923(3) 0.67458(15) 0.0298(7) Uani 1 1 d . . . C20 C 0.1733(3) 0.3838(3) 0.73317(16) 0.0341(7) Uani 1 1 d . . . C21 C 0.1255(3) 0.4723(3) 0.75766(18) 0.0451(9) Uani 1 1 d . . . H21A H 0.1025 0.4693 0.7971 0.054 Uiso 1 1 calc R . . C22 C 0.1112(3) 0.5633(3) 0.7257(2) 0.0529(11) Uani 1 1 d . . . H22A H 0.0799 0.6219 0.7434 0.063 Uiso 1 1 calc R . . C23 C 0.1427(4) 0.5682(3) 0.6682(2) 0.0523(10) Uani 1 1 d . . . H23A H 0.1308 0.6302 0.6463 0.063 Uiso 1 1 calc R . . C24 C 0.1919(3) 0.4840(3) 0.64076(18) 0.0413(8) Uani 1 1 d . . . C25 C 0.1862(3) 0.2858(3) 0.76937(17) 0.0458(9) Uani 1 1 d . . . H25A H 0.1355 0.2341 0.7563 0.069 Uiso 1 1 calc R . . H25B H 0.1762 0.3018 0.8111 0.069 Uiso 1 1 calc R . . H25C H 0.2555 0.2579 0.7642 0.069 Uiso 1 1 calc R . . C26 C 0.2245(4) 0.4909(4) 0.5769(2) 0.0571(11) Uani 1 1 d . . . H26A H 0.1823 0.4437 0.5527 0.086 Uiso 1 1 calc R . . H26B H 0.2968 0.4712 0.5740 0.086 Uiso 1 1 calc R . . H26C H 0.2152 0.5624 0.5627 0.086 Uiso 1 1 calc R . . S30 S 0.45199(7) 0.41695(8) 0.78627(4) 0.0387(2) Uani 1 1 d . . . O31 O 0.4611(2) 0.33375(19) 0.74202(10) 0.0377(5) Uani 1 1 d . . . O32 O 0.4263(3) 0.5175(2) 0.76096(14) 0.0625(9) Uani 1 1 d . . . O33 O 0.3953(3) 0.3884(3) 0.83769(13) 0.0612(8) Uani 1 1 d . . . C30 C 0.5839(4) 0.4342(5) 0.8140(2) 0.0664(14) Uani 1 1 d . . . F31 F 0.5865(3) 0.5090(4) 0.8550(2) 0.1174(18) Uani 1 1 d . . . F32 F 0.6185(3) 0.3467(4) 0.83954(19) 0.1077(15) Uani 1 1 d . . . F33 F 0.6469(3) 0.4579(4) 0.7711(2) 0.1109(16) Uani 1 1 d . . . S40 S 0.47165(9) 0.30693(7) 0.48783(4) 0.0433(2) Uani 1 1 d . . . O41 O 0.4395(2) 0.3474(2) 0.54492(11) 0.0431(6) Uani 1 1 d . . . O42 O 0.5219(3) 0.2067(2) 0.49154(14) 0.0624(9) Uani 1 1 d . . . O43 O 0.5195(3) 0.3832(3) 0.45078(14) 0.0708(10) Uani 1 1 d . . . C40 C 0.3487(5) 0.2776(4) 0.4498(2) 0.0663(14) Uani 1 1 d . . . F41 F 0.3652(4) 0.2340(3) 0.39694(14) 0.1052(14) Uani 1 1 d . . . F42 F 0.2937(3) 0.3634(3) 0.44028(18) 0.0978(12) Uani 1 1 d . . . F43 F 0.2926(4) 0.2109(4) 0.48055(18) 0.1126(16) Uani 1 1 d . . . O50 O 0.4768(3) 0.4846(2) 0.64400(13) 0.0512(8) Uani 1 1 d D . . H50A H 0.469(5) 0.524(4) 0.6769(15) 0.076(17) Uiso 1 1 d D . . H50B H 0.472(5) 0.529(5) 0.611(3) 0.09(2) Uiso 1 1 d . . . C60 C -0.0930(13) 0.2259(11) 0.4747(8) 0.157(7) Uani 0.75 1 d PU A 1 H60A H -0.1599 0.2614 0.4785 0.189 Uiso 0.75 1 calc PR A 1 H60B H -0.0894 0.2017 0.4333 0.189 Uiso 0.75 1 calc PR A 1 Cl1 Cl -0.0972(3) 0.1317(4) 0.51193(14) 0.1227(12) Uani 0.75 1 d P A 1 Cl2 Cl 0.0062(3) 0.3264(3) 0.48406(17) 0.1723(14) Uani 1 1 d . . . C60' C -0.0121(18) 0.2079(17) 0.4622(10) 0.061(5) Uiso 0.25 1 d P A 2 H60C H -0.0735 0.2148 0.4361 0.073 Uiso 0.25 1 calc PR A 2 H60D H 0.0456 0.1971 0.4351 0.073 Uiso 0.25 1 calc PR A 2 Cl1' Cl -0.026(2) 0.101(2) 0.4880(10) 0.263(11) Uani 0.25 1 d PU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.0300(2) 0.0205(2) 0.0291(2) -0.00287(19) 0.00266(17) -0.0001(2) N1 0.0306(14) 0.0229(13) 0.0250(12) 0.0006(10) -0.0010(10) 0.0008(11) C2 0.0376(17) 0.0232(14) 0.0219(14) 0.0011(12) 0.0037(12) 0.0037(13) C3 0.044(2) 0.0264(16) 0.0346(18) -0.0052(13) 0.0053(15) 0.0036(14) C4 0.052(2) 0.0259(16) 0.0408(19) -0.0104(14) -0.0016(16) -0.0055(15) C5 0.0368(19) 0.0317(17) 0.0396(19) -0.0037(14) -0.0032(15) -0.0039(14) C6 0.0343(17) 0.0278(15) 0.0210(14) -0.0005(12) 0.0000(12) -0.0023(13) C7 0.0331(17) 0.0292(16) 0.0274(15) -0.0023(13) 0.0042(13) 0.0055(14) N7 0.0281(14) 0.0288(13) 0.0325(14) -0.0009(11) 0.0003(11) 0.0013(11) C8 0.040(2) 0.044(2) 0.061(3) -0.0159(19) 0.0018(18) 0.0135(18) C9 0.0298(16) 0.0280(15) 0.0248(15) 0.0029(12) 0.0006(12) 0.0006(13) N9 0.0297(13) 0.0290(13) 0.0275(13) -0.0019(11) 0.0016(10) 0.0021(11) C10 0.0306(18) 0.041(2) 0.048(2) -0.0060(16) -0.0036(15) -0.0027(15) C11 0.0266(17) 0.0391(19) 0.048(2) -0.0111(16) 0.0015(15) 0.0013(14) C12 0.035(2) 0.047(2) 0.069(3) -0.015(2) 0.0136(18) -0.0069(17) C13 0.037(2) 0.067(3) 0.114(5) -0.024(3) 0.018(3) -0.017(2) C14 0.033(2) 0.104(4) 0.100(4) -0.049(4) -0.007(3) -0.006(3) C15 0.041(2) 0.098(4) 0.069(3) -0.027(3) -0.013(2) 0.012(3) C16 0.037(2) 0.060(2) 0.050(2) -0.0176(19) -0.0053(17) 0.0087(18) C17 0.056(3) 0.063(3) 0.086(4) 0.018(3) 0.021(3) -0.007(2) C18 0.059(3) 0.076(3) 0.046(2) 0.007(2) -0.009(2) 0.007(2) C19 0.0237(15) 0.0294(16) 0.0361(17) -0.0070(13) -0.0019(13) 0.0020(13) C20 0.0237(16) 0.0413(19) 0.0373(18) -0.0076(15) 0.0002(13) -0.0015(14) C21 0.036(2) 0.054(2) 0.045(2) -0.0220(18) 0.0060(16) -0.0006(17) C22 0.045(2) 0.046(2) 0.068(3) -0.021(2) 0.002(2) 0.0122(18) C23 0.054(2) 0.0344(19) 0.068(3) -0.0016(18) -0.003(2) 0.0157(18) C24 0.041(2) 0.0359(19) 0.047(2) 0.0008(16) 0.0010(16) 0.0074(16) C25 0.050(2) 0.051(2) 0.0372(19) -0.0010(16) 0.0067(17) -0.0015(18) C26 0.067(3) 0.053(2) 0.052(2) 0.014(2) 0.008(2) 0.024(2) S30 0.0393(5) 0.0453(5) 0.0315(4) -0.0096(4) -0.0001(3) 0.0000(4) O31 0.0477(14) 0.0346(13) 0.0308(12) -0.0017(10) -0.0009(10) -0.0025(11) O32 0.092(3) 0.0458(16) 0.0499(17) -0.0145(13) 0.0020(16) 0.0133(17) O33 0.0546(18) 0.093(2) 0.0366(15) -0.0091(15) 0.0056(13) -0.0055(17) C30 0.044(2) 0.083(4) 0.071(3) -0.038(3) -0.006(2) 0.000(2) F31 0.064(2) 0.149(4) 0.138(4) -0.103(3) -0.023(2) -0.003(2) F32 0.080(2) 0.140(4) 0.101(3) -0.036(3) -0.045(2) 0.042(2) F33 0.0560(19) 0.130(3) 0.148(4) -0.056(3) 0.033(2) -0.039(2) S40 0.0763(7) 0.0272(4) 0.0269(4) 0.0003(3) 0.0096(4) 0.0034(4) O41 0.0667(18) 0.0359(13) 0.0268(12) -0.0027(10) 0.0063(11) 0.0057(12) O42 0.106(3) 0.0369(15) 0.0451(16) -0.0077(12) 0.0095(17) 0.0210(16) O43 0.113(3) 0.0543(19) 0.0456(17) 0.0136(14) 0.0193(18) -0.0111(19) C40 0.111(4) 0.049(2) 0.039(2) 0.0022(19) -0.011(3) 0.001(3) F41 0.173(4) 0.094(2) 0.0479(17) -0.0245(17) -0.032(2) 0.006(3) F42 0.114(3) 0.084(2) 0.093(2) 0.0010(19) -0.037(2) 0.020(2) F43 0.131(3) 0.123(3) 0.083(2) 0.033(2) -0.035(2) -0.070(3) O50 0.093(2) 0.0252(12) 0.0358(14) -0.0003(11) 0.0047(14) -0.0091(13) C60 0.156(13) 0.109(9) 0.203(16) -0.054(10) -0.083(12) 0.047(9) Cl1 0.117(2) 0.164(3) 0.0861(17) 0.0111(18) -0.0278(16) -0.049(2) Cl2 0.161(3) 0.172(3) 0.181(3) 0.049(2) -0.069(2) -0.023(2) Cl1' 0.271(18) 0.338(19) 0.178(13) -0.063(14) -0.094(13) -0.032(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn O50 2.104(3) . ? Mn N1 2.183(3) . ? Mn O31 2.189(2) . ? Mn O41 2.266(3) . ? Mn N9 2.298(3) . ? Mn N7 2.301(3) . ? N1 C2 1.333(4) . ? N1 C6 1.338(4) . ? C2 C3 1.394(5) . ? C2 C7 1.496(5) . ? C3 C4 1.373(6) . ? C4 C5 1.385(5) . ? C5 C6 1.393(5) . ? C6 C9 1.502(5) . ? C7 N7 1.283(4) . ? C7 C8 1.502(5) . ? N7 C11 1.445(5) . ? C9 N9 1.286(4) . ? C9 C10 1.499(5) . ? N9 C19 1.436(4) . ? C11 C16 1.399(6) . ? C11 C12 1.400(6) . ? C12 C13 1.401(7) . ? C12 C17 1.498(7) . ? C13 C14 1.358(9) . ? C14 C15 1.390(9) . ? C15 C16 1.383(7) . ? C16 C18 1.508(7) . ? C19 C20 1.400(5) . ? C19 C24 1.405(5) . ? C20 C21 1.402(5) . ? C20 C25 1.496(6) . ? C21 C22 1.373(7) . ? C22 C23 1.361(7) . ? C23 C24 1.395(6) . ? C24 C26 1.503(6) . ? S30 O33 1.425(3) . ? S30 O32 1.436(3) . ? S30 O31 1.458(3) . ? S30 C30 1.814(5) . ? C30 F33 1.307(7) . ? C30 F31 1.324(6) . ? C30 F32 1.325(7) . ? S40 O43 1.426(3) . ? S40 O42 1.432(3) . ? S40 O41 1.448(3) . ? S40 C40 1.826(6) . ? C40 F42 1.318(7) . ? C40 F43 1.319(7) . ? C40 F41 1.329(6) . ? C60 Cl1 1.463(17) . ? C60 Cl2 1.819(16) . ? Cl2 C60' 1.60(2) . ? C60' Cl1' 1.49(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O50 Mn N1 164.89(11) . . ? O50 Mn O31 86.01(10) . . ? N1 Mn O31 108.52(9) . . ? O50 Mn O41 81.67(10) . . ? N1 Mn O41 83.80(9) . . ? O31 Mn O41 167.67(9) . . ? O50 Mn N9 104.96(12) . . ? N1 Mn N9 71.47(10) . . ? O31 Mn N9 91.29(10) . . ? O41 Mn N9 92.36(10) . . ? O50 Mn N7 113.25(12) . . ? N1 Mn N7 71.90(10) . . ? O31 Mn N7 90.17(10) . . ? O41 Mn N7 94.22(10) . . ? N9 Mn N7 141.78(10) . . ? C2 N1 C6 120.7(3) . . ? C2 N1 Mn 118.5(2) . . ? C6 N1 Mn 119.7(2) . . ? N1 C2 C3 120.6(3) . . ? N1 C2 C7 115.0(3) . . ? C3 C2 C7 124.4(3) . . ? C4 C3 C2 119.3(3) . . ? C3 C4 C5 119.8(3) . . ? C4 C5 C6 118.1(3) . . ? N1 C6 C5 121.4(3) . . ? N1 C6 C9 114.6(3) . . ? C5 C6 C9 124.0(3) . . ? N7 C7 C2 116.6(3) . . ? N7 C7 C8 125.0(3) . . ? C2 C7 C8 118.4(3) . . ? C7 N7 C11 119.9(3) . . ? C7 N7 Mn 115.7(2) . . ? C11 N7 Mn 124.4(2) . . ? N9 C9 C10 125.8(3) . . ? N9 C9 C6 115.7(3) . . ? C10 C9 C6 118.6(3) . . ? C9 N9 C19 121.0(3) . . ? C9 N9 Mn 117.5(2) . . ? C19 N9 Mn 121.5(2) . . ? C16 C11 C12 122.0(4) . . ? C16 C11 N7 119.0(4) . . ? C12 C11 N7 118.8(4) . . ? C11 C12 C13 117.3(5) . . ? C11 C12 C17 121.3(4) . . ? C13 C12 C17 121.4(5) . . ? C14 C13 C12 121.7(5) . . ? C13 C14 C15 119.9(4) . . ? C16 C15 C14 121.2(5) . . ? C15 C16 C11 117.9(5) . . ? C15 C16 C18 120.2(5) . . ? C11 C16 C18 122.0(4) . . ? C20 C19 C24 121.8(3) . . ? C20 C19 N9 119.2(3) . . ? C24 C19 N9 118.8(3) . . ? C19 C20 C21 117.1(4) . . ? C19 C20 C25 122.7(3) . . ? C21 C20 C25 120.2(3) . . ? C22 C21 C20 122.0(4) . . ? C23 C22 C21 119.6(4) . . ? C22 C23 C24 122.0(4) . . ? C23 C24 C19 117.5(4) . . ? C23 C24 C26 120.9(4) . . ? C19 C24 C26 121.6(3) . . ? O33 S30 O32 115.4(2) . . ? O33 S30 O31 114.53(19) . . ? O32 S30 O31 113.52(16) . . ? O33 S30 C30 104.2(2) . . ? O32 S30 C30 103.7(3) . . ? O31 S30 C30 103.54(19) . . ? S30 O31 Mn 136.05(15) . . ? F33 C30 F31 109.8(5) . . ? F33 C30 F32 107.6(5) . . ? F31 C30 F32 107.4(5) . . ? F33 C30 S30 111.5(4) . . ? F31 C30 S30 109.7(3) . . ? F32 C30 S30 110.7(4) . . ? O43 S40 O42 116.1(2) . . ? O43 S40 O41 114.04(19) . . ? O42 S40 O41 113.72(17) . . ? O43 S40 C40 104.4(2) . . ? O42 S40 C40 103.5(2) . . ? O41 S40 C40 103.0(2) . . ? S40 O41 Mn 144.93(17) . . ? F42 C40 F43 108.6(6) . . ? F42 C40 F41 107.2(4) . . ? F43 C40 F41 107.3(5) . . ? F42 C40 S40 111.5(4) . . ? F43 C40 S40 111.6(3) . . ? F41 C40 S40 110.5(5) . . ? Cl1 C60 Cl2 122.9(8) . . ? C60' Cl2 C60 37.2(9) . . ? Cl1' C60' Cl2 139.3(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.409 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.067 #===END