Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yozo Miura' _publ_contact_author_address ; Graduate School of Engineering Osaka City University Sumiyoshi-ku Osaka 558-8585 JAPAN ; _publ_contact_author_email MIURA@A-CHEM.ENG.OSAKA-CU.AC.JP _publ_section_title ; Syntheses and magnetic properties of Cu(II)(hfac)2 and Mn(II)(hfac)2 complexes of 4-pyridyl-substituted thioaminyl radicals ; loop_ _publ_author_name 'Yozo Miura' 'Ikumi Kato' 'Yoshio Teki' #Compound Cu(hfac)2(1)2 data_crystalclear _database_code_depnum_ccdc_archive 'CCDC 251883' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C62 H40 Cl4 Cu F12 N4 O8 S2' _chemical_formula_sum 'C62 H40 Cl4 Cu F12 N4 O8 S2' _chemical_formula_weight 1466.44 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.786(6) _cell_length_b 9.362(6) _cell_length_c 19.669(15) _cell_angle_alpha 80.087(16) _cell_angle_beta 88.99(2) _cell_angle_gamma 80.506(19) _cell_volume 1571.8(19) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3439 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Platelet _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 741 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8597 _exptl_absorpt_correction_T_max 0.9669 _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.6199 _diffrn_reflns_number 12250 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.00 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.561 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.074 _reflns_number_total 6779 _reflns_number_gt 5341 _reflns_threshold_expression >2sigma(I) _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0231P)^2^+4.2540P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6779 _refine_ls_number_parameters 460 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1295 _refine_ls_R_factor_gt 0.0998 _refine_ls_wR_factor_ref 0.1778 _refine_ls_wR_factor_gt 0.1636 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.197 _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 Cu1 Cu 1.0000 0.5000 0.5000 0.0356(2) Uani 1 2 d S . . S1 S 1.46448(16) 0.12025(16) 0.74346(7) 0.0434(3) Uani 1 1 d . . . Cl1 Cl 2.0265(2) -0.1515(2) 0.65418(9) 0.0799(6) Uani 1 1 d . . . Cl2 Cl 0.76229(16) 0.51754(19) 0.89231(8) 0.0597(4) Uani 1 1 d . . . N1 N 1.4316(5) 0.2158(5) 0.8048(2) 0.0388(10) Uani 1 1 d . . . N2 N 1.1225(4) 0.3737(5) 0.57972(19) 0.0368(9) Uani 1 1 d . . . O1 O 1.8764(4) 0.1046(5) 1.06931(18) 0.0513(10) Uani 1 1 d . . . O2 O 1.6486(4) 0.1993(4) 1.10989(16) 0.0439(9) Uani 1 1 d . . . C1 C 1.5136(5) 0.1868(5) 0.8662(2) 0.0333(10) Uani 1 1 d . . . C2 C 1.6649(5) 0.1067(5) 0.8784(2) 0.0349(10) Uani 1 1 d . . . C3 C 1.7335(5) 0.0939(6) 0.9426(2) 0.0366(11) Uani 1 1 d . . . H3A H 1.8331 0.0393 0.9512 0.044 Uiso 1 1 calc R . . C4 C 1.6574(5) 0.1605(5) 0.9945(2) 0.0346(10) Uani 1 1 d . . . C5 C 1.5077(6) 0.2381(5) 0.9835(2) 0.0363(11) Uani 1 1 d . . . H5A H 1.4569 0.2816 1.0192 0.044 Uiso 1 1 calc R . . C6 C 1.4326(5) 0.2518(5) 0.9201(2) 0.0345(10) Uani 1 1 d . . . C7 C 1.7564(5) 0.0424(6) 0.8229(2) 0.0350(11) Uani 1 1 d . . . C8 C 1.8142(6) 0.1332(6) 0.7682(3) 0.0439(12) Uani 1 1 d . . . H8A H 1.7950 0.2357 0.7661 0.053 Uiso 1 1 calc R . . C9 C 1.8997(6) 0.0736(7) 0.7169(3) 0.0479(13) Uani 1 1 d . . . H9A H 1.9409 0.1347 0.6808 0.057 Uiso 1 1 calc R . . C10 C 1.9233(6) -0.0763(7) 0.7197(3) 0.0519(15) Uani 1 1 d . . . C11 C 1.8666(7) -0.1680(7) 0.7731(3) 0.0519(14) Uani 1 1 d . . . H11A H 1.8835 -0.2702 0.7744 0.062 Uiso 1 1 calc R . . C12 C 1.7848(6) -0.1079(6) 0.8247(3) 0.0453(13) Uani 1 1 d . . . H12A H 1.7478 -0.1701 0.8618 0.054 Uiso 1 1 calc R . . C13 C 1.2692(5) 0.3234(5) 0.9113(2) 0.0349(11) Uani 1 1 d . . . C14 C 1.2170(6) 0.4606(6) 0.9276(3) 0.0405(12) Uani 1 1 d . . . H14A H 1.2881 0.5126 0.9435 0.049 Uiso 1 1 calc R . . C15 C 1.0626(6) 0.5238(6) 0.9213(3) 0.0439(12) Uani 1 1 d . . . H15A H 1.0291 0.6179 0.9320 0.053 Uiso 1 1 calc R . . C16 C 0.9597(6) 0.4454(6) 0.8990(3) 0.0408(12) Uani 1 1 d . . . C17 C 1.0067(6) 0.3093(6) 0.8826(3) 0.0479(13) Uani 1 1 d . . . H17A H 0.9347 0.2575 0.8673 0.057 Uiso 1 1 calc R . . C18 C 1.1613(6) 0.2481(6) 0.8887(3) 0.0446(12) Uani 1 1 d . . . H18A H 1.1940 0.1543 0.8774 0.054 Uiso 1 1 calc R . . C19 C 1.7418(6) 0.1501(6) 1.0607(2) 0.0375(11) Uani 1 1 d . . . C20 C 1.7232(6) 0.1974(7) 1.1756(3) 0.0488(14) Uani 1 1 d . . . H20A H 1.8164 0.2427 1.1681 0.059 Uiso 1 1 calc R . . H20B H 1.7526 0.0961 1.1997 0.059 Uiso 1 1 calc R . . C21 C 1.6086(7) 0.2830(8) 1.2171(3) 0.0651(18) Uani 1 1 d . . . H21A H 1.5837 0.3838 1.1934 0.098 Uiso 1 1 calc R . . H21B H 1.6526 0.2812 1.2622 0.098 Uiso 1 1 calc R . . H21C H 1.5156 0.2391 1.2225 0.098 Uiso 1 1 calc R . . C22 C 1.3214(5) 0.2187(6) 0.6842(2) 0.0349(11) Uani 1 1 d . . . C23 C 1.2381(6) 0.3537(6) 0.6905(2) 0.0418(12) Uani 1 1 d . . . H23A H 1.2472 0.3943 0.7305 0.050 Uiso 1 1 calc R . . C24 C 1.1411(6) 0.4282(6) 0.6372(2) 0.0428(12) Uani 1 1 d . . . H24A H 1.0856 0.5211 0.6412 0.051 Uiso 1 1 calc R . . C25 C 1.2002(6) 0.2405(6) 0.5751(3) 0.0409(12) Uani 1 1 d . . . H25A H 1.1863 0.2009 0.5353 0.049 Uiso 1 1 calc R . . C26 C 1.2989(6) 0.1589(6) 0.6256(2) 0.0416(12) Uani 1 1 d . . . H26A H 1.3504 0.0649 0.6209 0.050 Uiso 1 1 calc R . . O4 O 0.8692(4) 0.3140(4) 0.48961(19) 0.0480(9) Uani 1 1 d . . . O3 O 0.8363(4) 0.5639(4) 0.56517(17) 0.0418(8) Uani 1 1 d . . . C27 C 0.7319(6) 0.4969(6) 0.5902(3) 0.0477(13) Uani 1 1 d . A . C29 C 0.7597(7) 0.2914(6) 0.5266(3) 0.0486(13) Uani 1 1 d D B . C28 C 0.6883(8) 0.3721(8) 0.5754(3) 0.068(2) Uani 1 1 d . . . H28A H 0.6045 0.3381 0.5997 0.082 Uiso 1 1 calc R . . C30 C 0.6450(8) 0.5657(7) 0.6462(3) 0.078(2) Uani 1 1 d D . . C31 C 0.6913(8) 0.1555(7) 0.5176(3) 0.083(2) Uani 1 1 d D . . F1A F 0.653(2) 0.7084(10) 0.6458(12) 0.065(3) Uani 0.48 1 d PD A 1 F2A F 0.4854(10) 0.5670(13) 0.6421(6) 0.101(4) Uani 0.48 1 d PD A 1 F3A F 0.707(2) 0.515(4) 0.7111(6) 0.128(5) Uani 0.48 1 d PD A 1 F1B F 0.607(2) 0.7135(10) 0.6289(12) 0.065(3) Uani 0.47 1 d PD A 2 F2B F 0.5499(15) 0.4862(12) 0.6842(7) 0.101(4) Uani 0.47 1 d PD A 2 F3B F 0.753(2) 0.542(4) 0.6988(7) 0.128(5) Uani 0.47 1 d PD A 2 F1C F 0.735(7) 0.639(10) 0.682(4) 0.065(3) Uani 0.05 1 d PD A 3 F2C F 0.496(4) 0.629(10) 0.622(4) 0.101(4) Uani 0.05 1 d PD A 3 F3C F 0.62(2) 0.446(8) 0.695(5) 0.128(5) Uani 0.05 1 d PD A 3 F4A F 0.6771(8) 0.0641(10) 0.5796(4) 0.071(2) Uani 0.58 1 d PD B 1 F5A F 0.5399(11) 0.1827(11) 0.4967(11) 0.103(3) Uani 0.58 1 d PD B 1 F6A F 0.7796(14) 0.0559(12) 0.4852(6) 0.139(5) Uani 0.58 1 d PD B 1 F4B F 0.618(2) 0.096(3) 0.5758(11) 0.071(2) Uani 0.27 1 d PD B 2 F6B F 0.8263(19) 0.054(2) 0.5172(14) 0.139(5) Uani 0.27 1 d PD B 2 F4C F 0.750(3) 0.026(2) 0.5614(14) 0.071(2) Uani 0.15 1 d PD B 3 F6C F 0.696(6) 0.174(4) 0.4455(6) 0.139(5) Uani 0.15 1 d PD B 3 F5B F 0.672(3) 0.140(3) 0.4506(6) 0.103(3) Uani 0.27 1 d PD B 2 F5C F 0.540(4) 0.222(5) 0.500(5) 0.103(3) Uani 0.15 1 d PD B 3 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 Cu1 0.0356(4) 0.0459(5) 0.0257(4) -0.0104(4) 0.0007(3) -0.0038(4) S1 0.0492(7) 0.0447(8) 0.0361(7) -0.0128(6) -0.0106(6) 0.0006(6) Cl1 0.0823(12) 0.0971(15) 0.0647(11) -0.0399(10) 0.0288(9) -0.0032(10) Cl2 0.0370(7) 0.0712(11) 0.0663(10) -0.0028(8) 0.0009(6) -0.0044(7) N1 0.044(2) 0.043(3) 0.029(2) -0.0079(18) -0.0053(17) -0.0021(19) N2 0.040(2) 0.045(3) 0.025(2) -0.0096(18) -0.0001(16) -0.0031(19) O1 0.048(2) 0.065(3) 0.039(2) -0.0157(19) -0.0127(17) 0.0037(19) O2 0.045(2) 0.061(2) 0.0262(17) -0.0136(16) -0.0006(14) -0.0062(17) C1 0.039(3) 0.033(3) 0.027(2) -0.0057(19) -0.0013(19) -0.004(2) C2 0.039(3) 0.034(3) 0.031(2) -0.007(2) 0.0007(19) -0.003(2) C3 0.035(2) 0.041(3) 0.032(2) -0.005(2) -0.0033(19) -0.001(2) C4 0.042(3) 0.032(3) 0.029(2) -0.006(2) -0.0016(19) -0.004(2) C5 0.044(3) 0.039(3) 0.028(2) -0.011(2) 0.000(2) -0.007(2) C6 0.040(3) 0.031(3) 0.031(2) -0.004(2) 0.000(2) -0.004(2) C7 0.034(2) 0.043(3) 0.029(2) -0.012(2) -0.0046(19) -0.002(2) C8 0.053(3) 0.046(3) 0.037(3) -0.016(2) 0.004(2) -0.014(3) C9 0.055(3) 0.055(4) 0.038(3) -0.015(3) 0.007(2) -0.018(3) C10 0.048(3) 0.071(4) 0.039(3) -0.021(3) 0.007(2) -0.005(3) C11 0.060(3) 0.043(3) 0.050(3) -0.015(3) 0.002(3) 0.005(3) C12 0.050(3) 0.042(3) 0.042(3) -0.010(2) 0.004(2) 0.000(2) C13 0.040(3) 0.035(3) 0.029(2) -0.003(2) 0.0024(19) -0.006(2) C14 0.038(3) 0.042(3) 0.045(3) -0.013(2) 0.001(2) -0.010(2) C15 0.044(3) 0.041(3) 0.047(3) -0.009(2) 0.005(2) -0.007(2) C16 0.035(3) 0.048(3) 0.037(3) 0.000(2) -0.002(2) -0.007(2) C17 0.044(3) 0.055(4) 0.050(3) -0.015(3) 0.001(2) -0.017(3) C18 0.050(3) 0.041(3) 0.047(3) -0.014(2) 0.004(2) -0.011(2) C19 0.043(3) 0.039(3) 0.031(2) -0.005(2) -0.001(2) -0.007(2) C20 0.054(3) 0.066(4) 0.028(3) -0.011(3) -0.004(2) -0.013(3) C21 0.070(4) 0.089(5) 0.040(3) -0.029(3) 0.000(3) -0.007(4) C22 0.035(2) 0.040(3) 0.030(2) -0.006(2) -0.0022(19) -0.008(2) C23 0.052(3) 0.048(3) 0.028(2) -0.015(2) -0.007(2) -0.008(3) C24 0.050(3) 0.049(3) 0.030(2) -0.015(2) -0.006(2) 0.001(2) C25 0.045(3) 0.043(3) 0.037(3) -0.017(2) 0.000(2) -0.004(2) C26 0.050(3) 0.044(3) 0.033(3) -0.013(2) -0.002(2) -0.006(2) O4 0.048(2) 0.057(2) 0.045(2) -0.0201(18) 0.0098(17) -0.0124(18) O3 0.045(2) 0.046(2) 0.0362(19) -0.0117(16) 0.0029(15) -0.0097(17) C27 0.054(3) 0.054(4) 0.038(3) -0.018(3) 0.008(2) -0.009(3) C29 0.055(3) 0.050(3) 0.046(3) -0.014(3) 0.004(3) -0.019(3) C28 0.074(4) 0.076(5) 0.069(4) -0.037(4) 0.041(4) -0.035(4) C30 0.099(6) 0.083(6) 0.067(5) -0.039(4) 0.043(4) -0.033(5) C31 0.111(6) 0.090(6) 0.067(5) -0.042(4) 0.043(5) -0.049(5) F1A 0.058(11) 0.076(3) 0.065(10) -0.037(3) -0.001(5) 0.006(3) F2A 0.111(8) 0.088(8) 0.128(10) -0.062(6) 0.095(7) -0.054(6) F3A 0.263(14) 0.087(12) 0.032(5) -0.011(5) 0.064(7) -0.022(10) F1B 0.058(11) 0.076(3) 0.065(10) -0.037(3) -0.001(5) 0.006(3) F2B 0.111(8) 0.088(8) 0.128(10) -0.062(6) 0.095(7) -0.054(6) F3B 0.263(14) 0.087(12) 0.032(5) -0.011(5) 0.064(7) -0.022(10) F1C 0.058(11) 0.076(3) 0.065(10) -0.037(3) -0.001(5) 0.006(3) F2C 0.111(8) 0.088(8) 0.128(10) -0.062(6) 0.095(7) -0.054(6) F3C 0.263(14) 0.087(12) 0.032(5) -0.011(5) 0.064(7) -0.022(10) F4A 0.049(7) 0.051(6) 0.115(4) -0.024(4) 0.030(5) -0.008(5) F5A 0.114(5) 0.097(7) 0.117(6) -0.019(7) -0.037(4) -0.071(5) F6A 0.217(11) 0.112(6) 0.147(12) -0.119(8) 0.112(9) -0.111(7) F4B 0.049(7) 0.051(6) 0.115(4) -0.024(4) 0.030(5) -0.008(5) F6B 0.217(11) 0.112(6) 0.147(12) -0.119(8) 0.112(9) -0.111(7) F4C 0.049(7) 0.051(6) 0.115(4) -0.024(4) 0.030(5) -0.008(5) F6C 0.217(11) 0.112(6) 0.147(12) -0.119(8) 0.112(9) -0.111(7) F5B 0.114(5) 0.097(7) 0.117(6) -0.019(7) -0.037(4) -0.071(5) F5C 0.114(5) 0.097(7) 0.117(6) -0.019(7) -0.037(4) -0.071(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.996(3) . ? Cu1 O3 1.996(3) 2_766 ? Cu1 N2 2.004(4) . ? Cu1 N2 2.004(4) 2_766 ? Cu1 O4 2.277(4) 2_766 ? Cu1 O4 2.277(4) . ? S1 N1 1.617(4) . ? S1 C22 1.758(5) . ? Cl1 C10 1.743(5) . ? Cl2 C16 1.753(5) . ? N1 C1 1.380(6) . ? N2 C25 1.336(6) . ? N2 C24 1.340(6) . ? O1 C19 1.193(6) . ? O2 C19 1.349(6) . ? O2 C20 1.455(6) . ? C1 C2 1.416(6) . ? C1 C6 1.433(6) . ? C2 C3 1.386(7) . ? C2 C7 1.496(6) . ? C3 C4 1.391(6) . ? C3 H3A 0.9400 . ? C4 C5 1.394(7) . ? C4 C19 1.491(7) . ? C5 C6 1.398(7) . ? C5 H5A 0.9400 . ? C6 C13 1.481(7) . ? C7 C12 1.382(7) . ? C7 C8 1.394(7) . ? C8 C9 1.387(7) . ? C8 H8A 0.9400 . ? C9 C10 1.376(8) . ? C9 H9A 0.9400 . ? C10 C11 1.379(8) . ? C11 C12 1.379(7) . ? C11 H11A 0.9400 . ? C12 H12A 0.9400 . ? C13 C14 1.381(7) . ? C13 C18 1.391(7) . ? C14 C15 1.385(7) . ? C14 H14A 0.9400 . ? C15 C16 1.376(7) . ? C15 H15A 0.9400 . ? C16 C17 1.365(8) . ? C17 C18 1.383(7) . ? C17 H17A 0.9400 . ? C18 H18A 0.9400 . ? C20 C21 1.501(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.377(7) . ? C22 C26 1.395(7) . ? C23 C24 1.377(7) . ? C23 H23A 0.9400 . ? C24 H24A 0.9400 . ? C25 C26 1.368(7) . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? O4 C29 1.220(6) . ? O3 C27 1.243(6) . ? C27 C28 1.365(8) . ? C27 C30 1.505(8) . ? C29 C28 1.399(8) . ? C29 C31 1.532(7) . ? C28 H28A 0.9400 . ? C30 F2B 1.343(8) . ? C30 F1A 1.347(9) . ? C30 F1B 1.353(9) . ? C30 F3A 1.374(9) . ? C30 F3B 1.384(10) . ? C30 F3C 1.397(11) . ? C30 F1C 1.397(10) . ? C30 F2C 1.400(11) . ? C30 F2A 1.404(8) . ? C31 F6A 1.351(8) . ? C31 F5B 1.366(10) . ? C31 F5A 1.369(8) . ? C31 F4B 1.380(10) . ? C31 F4A 1.381(8) . ? C31 F4C 1.386(10) . ? C31 F6B 1.393(10) . ? C31 F5C 1.395(10) . ? C31 F6C 1.400(10) . ? F6C F5C 1.77(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 O3 179.998(1) . 2_766 ? O3 Cu1 N2 89.63(16) . . ? O3 Cu1 N2 90.37(16) 2_766 . ? O3 Cu1 N2 90.37(16) . 2_766 ? O3 Cu1 N2 89.63(16) 2_766 2_766 ? N2 Cu1 N2 179.998(1) . 2_766 ? O3 Cu1 O4 92.81(14) . 2_766 ? O3 Cu1 O4 87.19(14) 2_766 2_766 ? N2 Cu1 O4 89.39(16) . 2_766 ? N2 Cu1 O4 90.61(16) 2_766 2_766 ? O3 Cu1 O4 87.19(14) . . ? O3 Cu1 O4 92.81(14) 2_766 . ? N2 Cu1 O4 90.61(16) . . ? N2 Cu1 O4 89.39(16) 2_766 . ? O4 Cu1 O4 180.0 2_766 . ? N1 S1 C22 99.3(2) . . ? C1 N1 S1 124.5(4) . . ? C25 N2 C24 118.0(4) . . ? C25 N2 Cu1 121.8(3) . . ? C24 N2 Cu1 119.9(4) . . ? C19 O2 C20 115.6(4) . . ? N1 C1 C2 126.7(4) . . ? N1 C1 C6 113.3(4) . . ? C2 C1 C6 120.0(4) . . ? C3 C2 C1 119.2(4) . . ? C3 C2 C7 118.8(4) . . ? C1 C2 C7 121.9(4) . . ? C2 C3 C4 121.1(5) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C3 C4 C5 120.3(4) . . ? C3 C4 C19 118.2(4) . . ? C5 C4 C19 121.4(4) . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C13 120.0(4) . . ? C1 C6 C13 121.3(4) . . ? C12 C7 C8 118.9(5) . . ? C12 C7 C2 120.6(4) . . ? C8 C7 C2 120.5(5) . . ? C9 C8 C7 120.5(5) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C10 C9 C8 119.1(5) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? C9 C10 C11 121.2(5) . . ? C9 C10 Cl1 119.3(4) . . ? C11 C10 Cl1 119.4(5) . . ? C12 C11 C10 119.2(6) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C7 121.0(5) . . ? C11 C12 H12A 119.5 . . ? C7 C12 H12A 119.5 . . ? C14 C13 C18 118.0(5) . . ? C14 C13 C6 122.5(4) . . ? C18 C13 C6 119.4(5) . . ? C13 C14 C15 121.8(5) . . ? C13 C14 H14A 119.1 . . ? C15 C14 H14A 119.1 . . ? C16 C15 C14 118.4(5) . . ? C16 C15 H15A 120.8 . . ? C14 C15 H15A 120.8 . . ? C17 C16 C15 121.5(5) . . ? C17 C16 Cl2 118.0(4) . . ? C15 C16 Cl2 120.5(4) . . ? C16 C17 C18 119.4(5) . . ? C16 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C17 C18 C13 120.9(5) . . ? C17 C18 H18A 119.6 . . ? C13 C18 H18A 119.6 . . ? O1 C19 O2 123.7(5) . . ? O1 C19 C4 124.2(5) . . ? O2 C19 C4 112.1(4) . . ? O2 C20 C21 106.8(5) . . ? O2 C20 H20A 110.4 . . ? C21 C20 H20A 110.4 . . ? O2 C20 H20B 110.4 . . ? C21 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C26 118.9(5) . . ? C23 C22 S1 123.8(4) . . ? C26 C22 S1 117.2(4) . . ? C22 C23 C24 118.7(5) . . ? C22 C23 H23A 120.7 . . ? C24 C23 H23A 120.7 . . ? N2 C24 C23 122.8(5) . . ? N2 C24 H24A 118.6 . . ? C23 C24 H24A 118.6 . . ? N2 C25 C26 123.1(5) . . ? N2 C25 H25A 118.4 . . ? C26 C25 H25A 118.4 . . ? C25 C26 C22 118.4(5) . . ? C25 C26 H26A 120.8 . . ? C22 C26 H26A 120.8 . . ? C29 O4 Cu1 120.7(3) . . ? C27 O3 Cu1 127.5(4) . . ? O3 C27 C28 130.0(5) . . ? O3 C27 C30 113.0(5) . . ? C28 C27 C30 117.0(5) . . ? O4 C29 C28 129.2(5) . . ? O4 C29 C31 114.8(5) . . ? C28 C29 C31 116.0(5) . . ? C27 C28 C29 124.5(5) . . ? C27 C28 H28A 117.7 . . ? C29 C28 H28A 117.7 . . ? F2B C30 F1A 126.5(13) . . ? F2B C30 F1B 121.0(14) . . ? F1A C30 F1B 22.1(9) . . ? F2B C30 F3A 70.6(11) . . ? F1A C30 F3A 96.1(17) . . ? F1B C30 F3A 115.6(18) . . ? F2B C30 F3B 93.4(11) . . ? F1A C30 F3B 83.4(17) . . ? F1B C30 F3B 105.3(17) . . ? F3A C30 F3B 22.9(13) . . ? F2B C30 F3C 28(7) . . ? F1A C30 F3C 137(5) . . ? F1B C30 F3C 143(5) . . ? F3A C30 F3C 51(7) . . ? F3B C30 F3C 72(7) . . ? F2B C30 F1C 116(4) . . ? F1A C30 F1C 46(4) . . ? F1B C30 F1C 68(4) . . ? F3A C30 F1C 54(5) . . ? F3B C30 F1C 38(4) . . ? F3C C30 F1C 104(8) . . ? F2B C30 F2C 74(4) . . ? F1A C30 F2C 81(4) . . ? F1B C30 F2C 60(4) . . ? F3A C30 F2C 133(4) . . ? F3B C30 F2C 147(4) . . ? F3C C30 F2C 102(8) . . ? F1C C30 F2C 122(5) . . ? F2B C30 F2A 47.7(7) . . ? F1A C30 F2A 102.4(10) . . ? F1B C30 F2A 84.6(11) . . ? F3A C30 F2A 114.1(10) . . ? F3B C30 F2A 135.7(10) . . ? F3C C30 F2A 75(8) . . ? F1C C30 F2A 133(3) . . ? F2C C30 F2A 27(4) . . ? F2B C30 C27 116.5(7) . . ? F1A C30 C27 116.1(13) . . ? F1B C30 C27 112.6(13) . . ? F3A C30 C27 114.1(15) . . ? F3B C30 C27 103.3(14) . . ? F3C C30 C27 104(4) . . ? F1C C30 C27 113(3) . . ? F2C C30 C27 109(4) . . ? F2A C30 C27 112.4(6) . . ? F6A C31 F5B 54.9(12) . . ? F6A C31 F5A 113.0(9) . . ? F5B C31 F5A 66.9(14) . . ? F6A C31 F4B 114.8(13) . . ? F5B C31 F4B 128.9(16) . . ? F5A C31 F4B 77.6(14) . . ? F6A C31 F4A 97.7(8) . . ? F5B C31 F4A 132.5(11) . . ? F5A C31 F4A 98.6(10) . . ? F4B C31 F4A 23.1(8) . . ? F6A C31 F4C 66.5(14) . . ? F5B C31 F4C 114.6(17) . . ? F5A C31 F4C 120.5(14) . . ? F4B C31 F4C 55.4(12) . . ? F4A C31 F4C 33.2(11) . . ? F6A C31 F6B 31.8(9) . . ? F5B C31 F6B 86.0(14) . . ? F5A C31 F6B 141.9(11) . . ? F4B C31 F6B 102.4(15) . . ? F4A C31 F6B 79.9(13) . . ? F4C C31 F6B 47.0(15) . . ? F6A C31 F5C 126(3) . . ? F5B C31 F5C 75(4) . . ? F5A C31 F5C 16(2) . . ? F4B C31 F5C 81(4) . . ? F4A C31 F5C 104(4) . . ? F4C C31 F5C 131(4) . . ? F6B C31 F5C 157(3) . . ? F6A C31 F6C 59(2) . . ? F5B C31 F6C 16.6(16) . . ? F5A C31 F6C 75(3) . . ? F4B C31 F6C 145(2) . . ? F4A C31 F6C 148.1(15) . . ? F4C C31 F6C 124(2) . . ? F6B C31 F6C 86(3) . . ? F5C C31 F6C 79(4) . . ? F6A C31 C29 116.9(7) . . ? F5B C31 C29 114.7(9) . . ? F5A C31 C29 115.2(6) . . ? F4B C31 C29 113.3(15) . . ? F4A C31 C29 112.3(7) . . ? F4C C31 C29 115.8(14) . . ? F6B C31 C29 100.0(11) . . ? F5C C31 C29 100(2) . . ? F6C C31 C29 98.2(14) . . ? C31 F6C F5C 50(2) . . ? C31 F5C F6C 51(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 S1 N1 C1 -179.8(4) . . . . ? O3 Cu1 N2 C25 140.8(4) . . . . ? O3 Cu1 N2 C25 -39.2(4) 2_766 . . . ? N2 Cu1 N2 C25 10(39) 2_766 . . . ? O4 Cu1 N2 C25 -126.4(4) 2_766 . . . ? O4 Cu1 N2 C25 53.6(4) . . . . ? O3 Cu1 N2 C24 -46.1(4) . . . . ? O3 Cu1 N2 C24 133.9(4) 2_766 . . . ? N2 Cu1 N2 C24 -177(39) 2_766 . . . ? O4 Cu1 N2 C24 46.7(4) 2_766 . . . ? O4 Cu1 N2 C24 -133.3(4) . . . . ? S1 N1 C1 C2 22.5(7) . . . . ? S1 N1 C1 C6 -159.8(4) . . . . ? N1 C1 C2 C3 176.8(5) . . . . ? C6 C1 C2 C3 -0.8(7) . . . . ? N1 C1 C2 C7 0.2(8) . . . . ? C6 C1 C2 C7 -177.4(4) . . . . ? C1 C2 C3 C4 -1.2(7) . . . . ? C7 C2 C3 C4 175.5(5) . . . . ? C2 C3 C4 C5 2.0(8) . . . . ? C2 C3 C4 C19 -176.2(5) . . . . ? C3 C4 C5 C6 -0.8(7) . . . . ? C19 C4 C5 C6 177.4(5) . . . . ? C4 C5 C6 C1 -1.1(7) . . . . ? C4 C5 C6 C13 174.7(4) . . . . ? N1 C1 C6 C5 -176.0(4) . . . . ? C2 C1 C6 C5 1.9(7) . . . . ? N1 C1 C6 C13 8.2(7) . . . . ? C2 C1 C6 C13 -173.9(4) . . . . ? C3 C2 C7 C12 74.3(6) . . . . ? C1 C2 C7 C12 -109.1(6) . . . . ? C3 C2 C7 C8 -105.9(6) . . . . ? C1 C2 C7 C8 70.7(6) . . . . ? C12 C7 C8 C9 -0.5(8) . . . . ? C2 C7 C8 C9 179.7(5) . . . . ? C7 C8 C9 C10 1.7(8) . . . . ? C8 C9 C10 C11 -1.5(9) . . . . ? C8 C9 C10 Cl1 178.4(4) . . . . ? C9 C10 C11 C12 0.0(9) . . . . ? Cl1 C10 C11 C12 -179.9(4) . . . . ? C10 C11 C12 C7 1.3(9) . . . . ? C8 C7 C12 C11 -1.0(8) . . . . ? C2 C7 C12 C11 178.8(5) . . . . ? C5 C6 C13 C14 52.2(7) . . . . ? C1 C6 C13 C14 -132.1(5) . . . . ? C5 C6 C13 C18 -124.7(5) . . . . ? C1 C6 C13 C18 51.0(7) . . . . ? C18 C13 C14 C15 -0.7(7) . . . . ? C6 C13 C14 C15 -177.7(5) . . . . ? C13 C14 C15 C16 1.0(8) . . . . ? C14 C15 C16 C17 -0.7(8) . . . . ? C14 C15 C16 Cl2 178.2(4) . . . . ? C15 C16 C17 C18 0.2(8) . . . . ? Cl2 C16 C17 C18 -178.8(4) . . . . ? C16 C17 C18 C13 0.0(8) . . . . ? C14 C13 C18 C17 0.2(8) . . . . ? C6 C13 C18 C17 177.3(5) . . . . ? C20 O2 C19 O1 1.4(7) . . . . ? C20 O2 C19 C4 -178.1(4) . . . . ? C3 C4 C19 O1 9.9(8) . . . . ? C5 C4 C19 O1 -168.4(5) . . . . ? C3 C4 C19 O2 -170.7(4) . . . . ? C5 C4 C19 O2 11.1(7) . . . . ? C19 O2 C20 C21 168.9(5) . . . . ? N1 S1 C22 C23 11.5(5) . . . . ? N1 S1 C22 C26 -172.4(4) . . . . ? C26 C22 C23 C24 -3.2(7) . . . . ? S1 C22 C23 C24 172.9(4) . . . . ? C25 N2 C24 C23 1.1(8) . . . . ? Cu1 N2 C24 C23 -172.3(4) . . . . ? C22 C23 C24 N2 1.1(8) . . . . ? C24 N2 C25 C26 -1.1(7) . . . . ? Cu1 N2 C25 C26 172.2(4) . . . . ? N2 C25 C26 C22 -1.0(8) . . . . ? C23 C22 C26 C25 3.1(7) . . . . ? S1 C22 C26 C25 -173.2(4) . . . . ? O3 Cu1 O4 C29 -7.8(4) . . . . ? O3 Cu1 O4 C29 172.2(4) 2_766 . . . ? N2 Cu1 O4 C29 81.8(4) . . . . ? N2 Cu1 O4 C29 -98.2(4) 2_766 . . . ? O4 Cu1 O4 C29 74(34) 2_766 . . . ? O3 Cu1 O3 C27 51(11) 2_766 . . . ? N2 Cu1 O3 C27 -81.4(5) . . . . ? N2 Cu1 O3 C27 98.6(5) 2_766 . . . ? O4 Cu1 O3 C27 -170.7(5) 2_766 . . . ? O4 Cu1 O3 C27 9.3(5) . . . . ? Cu1 O3 C27 C28 -8.0(10) . . . . ? Cu1 O3 C27 C30 170.6(4) . . . . ? Cu1 O4 C29 C28 4.9(9) . . . . ? Cu1 O4 C29 C31 -175.4(4) . . . . ? O3 C27 C28 C29 0.8(12) . . . . ? C30 C27 C28 C29 -177.8(6) . . . . ? O4 C29 C28 C27 0.3(12) . . . . ? C31 C29 C28 C27 -179.4(7) . . . . ? O3 C27 C30 F2B -168.4(10) . . . . ? C28 C27 C30 F2B 10.5(12) . . . . ? O3 C27 C30 F1A 21.6(10) . . . . ? C28 C27 C30 F1A -159.6(8) . . . . ? O3 C27 C30 F1B 45.5(10) . . . . ? C28 C27 C30 F1B -135.7(9) . . . . ? O3 C27 C30 F3A -88.9(13) . . . . ? C28 C27 C30 F3A 89.9(14) . . . . ? O3 C27 C30 F3B -67.6(14) . . . . ? C28 C27 C30 F3B 111.2(14) . . . . ? O3 C27 C30 F3C -142(8) . . . . ? C28 C27 C30 F3C 37(8) . . . . ? O3 C27 C30 F1C -29(5) . . . . ? C28 C27 C30 F1C 150(5) . . . . ? O3 C27 C30 F2C 110(4) . . . . ? C28 C27 C30 F2C -71(4) . . . . ? O3 C27 C30 F2A 139.0(7) . . . . ? C28 C27 C30 F2A -42.1(10) . . . . ? O4 C29 C31 F6A 17.0(11) . . . . ? C28 C29 C31 F6A -163.3(9) . . . . ? O4 C29 C31 F5B -44.5(16) . . . . ? C28 C29 C31 F5B 135.2(15) . . . . ? O4 C29 C31 F5A -119.3(12) . . . . ? C28 C29 C31 F5A 60.4(13) . . . . ? O4 C29 C31 F4B 153.8(10) . . . . ? C28 C29 C31 F4B -26.4(12) . . . . ? O4 C29 C31 F4A 128.8(6) . . . . ? C28 C29 C31 F4A -51.5(8) . . . . ? O4 C29 C31 F4C 92.5(14) . . . . ? C28 C29 C31 F4C -87.8(15) . . . . ? O4 C29 C31 F6B 45.6(13) . . . . ? C28 C29 C31 F6B -134.6(13) . . . . ? O4 C29 C31 F5C -122(4) . . . . ? C28 C29 C31 F5C 58(4) . . . . ? O4 C29 C31 F6C -42(2) . . . . ? C28 C29 C31 F6C 138(2) . . . . ? F6A C31 F6C F5C 145(2) . . . . ? F5B C31 F6C F5C 74(11) . . . . ? F5A C31 F6C F5C 16(2) . . . . ? F4B C31 F6C F5C 56(4) . . . . ? F4A C31 F6C F5C 98(5) . . . . ? F4C C31 F6C F5C 133(3) . . . . ? F6B C31 F6C F5C 162(2) . . . . ? C29 C31 F6C F5C -98(2) . . . . ? F6A C31 F5C F6C -37(3) . . . . ? F5B C31 F5C F6C -16.6(17) . . . . ? F5A C31 F5C F6C -74(18) . . . . ? F4B C31 F5C F6C -151.1(19) . . . . ? F4A C31 F5C F6C -147.5(16) . . . . ? F4C C31 F5C F6C -126(4) . . . . ? F6B C31 F5C F6C -51(10) . . . . ? C29 C31 F5C F6C 96.6(14) . . . . ? #Compound Mn(hfac)2(2)2 data__kato2 _database_code_depnum_ccdc_archive 'CCDC 251884' _audit_creation_date 'Wed Aug 31 08:54:57 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C68 H38 Cl6 F12 Mn N4 O4 S2 ' _chemical_formula_moiety 'C68 H38 Cl6 F12 Mn N4 O4 S2 ' _chemical_formula_weight 1534.83 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 19.950(2) _cell_length_b 6.1000(4) _cell_length_c 29.270(3) _cell_angle_alpha 90 _cell_angle_beta 111.160(4) _cell_angle_gamma 90 _cell_volume 3321.8(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6205 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 223.2 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour Blue _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.040 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1546.00 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.977 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 25861 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9860 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9860 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 33 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7486 _reflns_number_gt 5334 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1202 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7486 _refine_ls_number_parameters 439 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.68 _refine_diff_density_min -0.54 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Mn Mn 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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(1) Mn 1.0000 0.0000 0.5000 0.0243(1) Uani 1.00 2 d S . . Cl(1) Cl 1.29422(5) -1.0944(2) 0.78611(3) 0.0610(3) Uani 1.00 1 d . . . Cl(2) Cl 1.88194(5) -0.9698(3) 0.72104(5) 0.1029(4) Uani 1.00 1 d . . . Cl(3) Cl 1.34143(5) 0.1232(1) 0.43373(3) 0.0501(2) Uani 1.00 1 d . . . S(1) S 1.29048(4) -0.6326(1) 0.62391(3) 0.0308(2) Uani 1.00 1 d . . . F(1) F 1.21480(9) 0.2957(3) 0.48766(7) 0.0599(6) Uani 1.00 1 d . . . F(2) F 1.1747(1) 0.3506(3) 0.40984(7) 0.0567(6) Uani 1.00 1 d . . . F(3) F 1.1399(1) 0.5555(3) 0.45669(8) 0.0556(6) Uani 1.00 1 d . . . F(4) F 1.0645(1) -0.3286(4) 0.34902(9) 0.0916(9) Uani 1.00 1 d . . . F(5) F 0.9628(2) -0.1784(4) 0.32069(8) 0.0977(9) Uani 1.00 1 d . . . F(6) F 0.9780(1) -0.4610(3) 0.36533(7) 0.0628(7) Uani 1.00 1 d . . . O(1) O 1.06892(9) 0.2198(3) 0.47846(7) 0.0305(5) Uani 1.00 1 d . . . O(2) O 0.99051(10) -0.1616(3) 0.43159(7) 0.0324(5) Uani 1.00 1 d . . . N(1) N 1.3549(1) -0.5187(4) 0.61070(8) 0.0282(6) Uani 1.00 1 d . . . N(2) N 1.1003(1) -0.1951(4) 0.54213(8) 0.0290(6) Uani 1.00 1 d . . . C(1) C 1.4241(1) -0.5952(4) 0.62629(9) 0.0246(6) Uani 1.00 1 d . . . C(2) C 1.4570(1) -0.7478(4) 0.66522(9) 0.0248(6) Uani 1.00 1 d . . . C(3) C 1.5283(1) -0.8009(4) 0.67689(9) 0.0281(7) Uani 1.00 1 d . . . C(4) C 1.5711(1) -0.7121(4) 0.65275(9) 0.0274(7) Uani 1.00 1 d . . . C(5) C 1.5391(1) -0.5608(4) 0.61531(10) 0.0289(7) Uani 1.00 1 d . . . C(6) C 1.4675(1) -0.5013(4) 0.60159(9) 0.0259(6) Uani 1.00 1 d . . . C(7) C 1.4179(1) -0.8395(4) 0.69567(9) 0.0257(7) Uani 1.00 1 d . . . C(8) C 1.3851(1) -1.0438(4) 0.68590(10) 0.0325(8) Uani 1.00 1 d . . . C(9) C 1.3473(2) -1.1234(5) 0.7138(1) 0.0381(8) Uani 1.00 1 d . . . C(10) C 1.3431(1) -0.9979(5) 0.7515(1) 0.0377(8) Uani 1.00 1 d . . . C(11) C 1.3762(2) -0.7977(5) 0.7629(1) 0.0408(9) Uani 1.00 1 d . . . C(12) C 1.4141(1) -0.7191(5) 0.73486(10) 0.0335(8) Uani 1.00 1 d . . . C(13) C 1.6476(1) -0.7765(5) 0.66748(9) 0.0293(7) Uani 1.00 1 d . . . C(14) C 1.6710(1) -0.9803(5) 0.6895(1) 0.0364(8) Uani 1.00 1 d . . . C(15) C 1.7427(2) -1.0398(6) 0.7056(1) 0.0455(9) Uani 1.00 1 d . . . C(16) C 1.7917(2) -0.8961(7) 0.6993(1) 0.053(1) Uani 1.00 1 d . . . C(17) C 1.7708(2) -0.6967(6) 0.6766(1) 0.052(1) Uani 1.00 1 d . . . C(18) C 1.6986(1) -0.6377(5) 0.6608(1) 0.0410(8) Uani 1.00 1 d . . . C(19) C 1.4353(1) -0.3453(4) 0.56039(9) 0.0272(7) Uani 1.00 1 d . . . C(20) C 1.4654(1) -0.1396(4) 0.56138(10) 0.0314(7) Uani 1.00 1 d . . . C(21) C 1.4361(2) 0.0065(5) 0.5226(1) 0.0359(8) Uani 1.00 1 d . . . C(22) C 1.3772(2) -0.0565(5) 0.48266(10) 0.0347(8) Uani 1.00 1 d . . . C(23) C 1.3463(2) -0.2593(5) 0.4810(1) 0.0382(8) Uani 1.00 1 d . . . C(24) C 1.3749(1) -0.4022(5) 0.5199(1) 0.0349(8) Uani 1.00 1 d . . . C(25) C 1.2194(1) -0.4559(4) 0.59166(9) 0.0264(7) Uani 1.00 1 d . . . C(26) C 1.2279(1) -0.2531(5) 0.5737(1) 0.0318(7) Uani 1.00 1 d . . . C(27) C 1.1678(1) -0.1294(4) 0.5498(1) 0.0327(7) Uani 1.00 1 d . . . C(28) C 1.0929(1) -0.3930(5) 0.5596(1) 0.0310(7) Uani 1.00 1 d . . . C(29) C 1.1503(1) -0.5266(4) 0.58507(10) 0.0318(7) Uani 1.00 1 d . . . C(30) C 1.0942(1) 0.1932(4) 0.44526(10) 0.0289(7) Uani 1.00 1 d . . . C(31) C 1.0760(2) 0.0392(5) 0.4085(1) 0.0359(8) Uani 1.00 1 d . . . C(32) C 1.0249(1) -0.1232(4) 0.40431(10) 0.0321(7) Uani 1.00 1 d . . . C(33) C 1.1561(2) 0.3504(5) 0.4494(1) 0.0389(9) Uani 1.00 1 d . . . C(34) C 1.0061(2) -0.2732(5) 0.3594(1) 0.0465(10) Uani 1.00 1 d . . . H(3A) H 1.5496 -0.9026 0.7026 0.0332 Uiso 1.00 1 calc . . . H(5A) H 1.5673 -0.4965 0.5989 0.0341 Uiso 1.00 1 calc . . . H(8A) H 1.3886 -1.1294 0.6599 0.0392 Uiso 1.00 1 calc . . . H(9A) H 1.3246 -1.2624 0.7069 0.0451 Uiso 1.00 1 calc . . . H(11A) H 1.3732 -0.7141 0.7895 0.0478 Uiso 1.00 1 calc . . . H(12A) H 1.4379 -0.5818 0.7427 0.0396 Uiso 1.00 1 calc . . . H(14A) H 1.6369 -1.0797 0.6933 0.0429 Uiso 1.00 1 calc . . . H(15A) H 1.7579 -1.1781 0.7208 0.0539 Uiso 1.00 1 calc . . . H(17A) H 1.8051 -0.6012 0.6717 0.0625 Uiso 1.00 1 calc . . . H(18A) H 1.6839 -0.5005 0.6452 0.0482 Uiso 1.00 1 calc . . . H(20A) H 1.5063 -0.0979 0.5886 0.0375 Uiso 1.00 1 calc . . . H(21A) H 1.4566 0.1481 0.5236 0.0422 Uiso 1.00 1 calc . . . H(23A) H 1.3055 -0.3007 0.4536 0.0456 Uiso 1.00 1 calc . . . H(24A) H 1.3532 -0.5412 0.5191 0.0409 Uiso 1.00 1 calc . . . H(26A) H 1.2744 -0.1997 0.5778 0.0376 Uiso 1.00 1 calc . . . H(27A) H 1.1744 0.0108 0.5381 0.0384 Uiso 1.00 1 calc . . . H(28A) H 1.0457 -0.4445 0.5543 0.0364 Uiso 1.00 1 calc . . . H(29A) H 1.1426 -0.6641 0.5978 0.0374 Uiso 1.00 1 calc . . . H(31A) H 1.0987 0.0436 0.3851 0.0426 Uiso 1.00 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0177(3) 0.0301(3) 0.0259(3) 0.0028(2) 0.0090(2) 0.0043(2) Cl(1) 0.0570(6) 0.0849(7) 0.0533(5) -0.0131(5) 0.0345(5) 0.0094(5) Cl(2) 0.0321(5) 0.176(1) 0.1071(9) 0.0464(7) 0.0330(5) 0.0878(9) Cl(3) 0.0619(5) 0.0520(5) 0.0345(4) 0.0169(4) 0.0152(4) 0.0183(4) S(1) 0.0206(3) 0.0328(4) 0.0376(4) 0.0048(3) 0.0086(3) 0.0098(3) F(1) 0.0299(10) 0.076(1) 0.068(1) -0.0134(9) 0.0105(9) 0.006(1) F(2) 0.060(1) 0.064(1) 0.064(1) -0.0196(10) 0.043(1) -0.004(1) F(3) 0.064(1) 0.035(1) 0.078(1) -0.0128(9) 0.037(1) -0.0060(9) F(4) 0.100(2) 0.108(2) 0.096(2) -0.030(2) 0.071(2) -0.052(2) F(5) 0.153(2) 0.065(2) 0.033(1) -0.008(2) -0.018(1) 0.000(1) F(6) 0.100(2) 0.045(1) 0.055(1) -0.028(1) 0.042(1) -0.0170(9) O(1) 0.0269(10) 0.033(1) 0.034(1) -0.0004(8) 0.0143(8) 0.0017(8) O(2) 0.032(1) 0.036(1) 0.032(1) -0.0040(8) 0.0143(8) -0.0003(8) N(1) 0.022(1) 0.032(1) 0.030(1) 0.0021(9) 0.0100(9) 0.0019(10) N(2) 0.023(1) 0.032(1) 0.031(1) 0.0034(9) 0.0095(10) 0.0031(10) C(1) 0.020(1) 0.027(1) 0.024(1) 0.003(1) 0.006(1) -0.002(1) C(2) 0.024(1) 0.026(1) 0.022(1) 0.001(1) 0.005(1) 0.000(1) C(3) 0.026(1) 0.032(1) 0.024(1) 0.004(1) 0.006(1) 0.002(1) C(4) 0.022(1) 0.033(1) 0.024(1) 0.002(1) 0.005(1) -0.003(1) C(5) 0.023(1) 0.034(1) 0.029(1) 0.001(1) 0.008(1) 0.001(1) C(6) 0.025(1) 0.028(1) 0.022(1) 0.001(1) 0.006(1) -0.001(1) C(7) 0.020(1) 0.033(1) 0.022(1) 0.004(1) 0.004(1) 0.003(1) C(8) 0.035(2) 0.030(2) 0.032(1) 0.003(1) 0.012(1) -0.001(1) C(9) 0.038(2) 0.033(2) 0.044(2) -0.004(1) 0.016(1) 0.004(1) C(10) 0.033(2) 0.050(2) 0.031(2) 0.000(1) 0.014(1) 0.009(1) C(11) 0.040(2) 0.054(2) 0.031(2) 0.001(1) 0.015(1) -0.004(1) C(12) 0.032(2) 0.039(2) 0.027(1) -0.002(1) 0.008(1) -0.003(1) C(13) 0.021(1) 0.042(2) 0.022(1) 0.004(1) 0.005(1) 0.000(1) C(14) 0.030(2) 0.045(2) 0.031(1) 0.007(1) 0.008(1) 0.006(1) C(15) 0.040(2) 0.060(2) 0.037(2) 0.022(2) 0.014(1) 0.014(2) C(16) 0.026(2) 0.093(3) 0.043(2) 0.022(2) 0.015(1) 0.026(2) C(17) 0.026(2) 0.084(3) 0.050(2) 0.002(2) 0.016(1) 0.023(2) C(18) 0.026(1) 0.057(2) 0.038(2) 0.005(1) 0.009(1) 0.013(1) C(19) 0.024(1) 0.034(1) 0.024(1) 0.004(1) 0.009(1) 0.002(1) C(20) 0.030(1) 0.035(2) 0.027(1) -0.002(1) 0.008(1) -0.004(1) C(21) 0.043(2) 0.030(1) 0.037(2) 0.001(1) 0.017(1) 0.003(1) C(22) 0.037(2) 0.041(2) 0.029(1) 0.011(1) 0.016(1) 0.010(1) C(23) 0.031(2) 0.048(2) 0.029(1) 0.001(1) 0.003(1) 0.003(1) C(24) 0.030(1) 0.036(2) 0.036(2) -0.003(1) 0.009(1) 0.002(1) C(25) 0.020(1) 0.032(1) 0.026(1) 0.005(1) 0.007(1) 0.002(1) C(26) 0.021(1) 0.035(2) 0.037(2) -0.001(1) 0.007(1) 0.001(1) C(27) 0.026(1) 0.028(1) 0.042(2) 0.001(1) 0.010(1) 0.008(1) C(28) 0.023(1) 0.036(2) 0.036(2) 0.001(1) 0.012(1) 0.003(1) C(29) 0.026(1) 0.034(2) 0.036(2) 0.003(1) 0.012(1) 0.007(1) C(30) 0.022(1) 0.033(1) 0.033(1) 0.002(1) 0.011(1) 0.006(1) C(31) 0.041(2) 0.038(2) 0.036(2) -0.007(1) 0.023(1) -0.005(1) C(32) 0.035(2) 0.033(2) 0.029(1) 0.001(1) 0.013(1) 0.003(1) C(33) 0.035(2) 0.042(2) 0.044(2) -0.006(1) 0.019(1) 0.002(1) C(34) 0.060(2) 0.048(2) 0.037(2) -0.015(2) 0.023(2) -0.005(2) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 2.0' _computing_publication_material 'teXsan Ver. 2.0' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) O(1) 2.171(2) . . yes Mn(1) O(1) 2.171(2) . 3_756 yes Mn(1) O(2) 2.178(2) . . yes Mn(1) O(2) 2.178(2) . 3_756 yes Mn(1) N(2) 2.272(2) . . yes Mn(1) N(2) 2.272(2) . 3_756 yes Cl(1) C(10) 1.742(3) . . yes Cl(2) C(16) 1.738(3) . . yes Cl(3) C(22) 1.739(3) . . yes S(1) N(1) 1.626(2) . . yes S(1) C(25) 1.760(3) . . yes F(1) C(33) 1.337(3) . . yes F(2) C(33) 1.338(3) . . yes F(3) C(33) 1.329(3) . . yes F(4) C(34) 1.349(4) . . yes F(5) C(34) 1.288(4) . . yes F(6) C(34) 1.314(4) . . yes O(1) C(30) 1.257(3) . . yes O(2) C(32) 1.248(3) . . yes N(1) C(1) 1.369(3) . . yes N(2) C(27) 1.343(3) . . yes N(2) C(28) 1.340(3) . . yes C(1) C(2) 1.434(3) . . yes C(1) C(6) 1.432(3) . . yes C(2) C(3) 1.376(3) . . yes C(2) C(7) 1.489(3) . . yes C(3) C(4) 1.398(4) . . yes C(3) H(3A) 0.948 . . no C(4) C(5) 1.398(4) . . yes C(4) C(13) 1.481(3) . . yes C(5) C(6) 1.386(3) . . yes C(5) H(5A) 0.948 . . no C(6) C(19) 1.488(3) . . yes C(7) C(8) 1.389(4) . . yes C(7) C(12) 1.387(4) . . yes C(8) C(9) 1.384(4) . . yes C(8) H(8A) 0.945 . . no C(9) C(10) 1.371(4) . . yes C(9) H(9A) 0.948 . . no C(10) C(11) 1.371(4) . . yes C(11) C(12) 1.387(4) . . yes C(11) H(11A) 0.951 . . no C(12) H(12A) 0.948 . . no C(13) C(14) 1.400(4) . . yes C(13) C(18) 1.391(4) . . yes C(14) C(15) 1.384(4) . . yes C(14) H(14A) 0.948 . . no C(15) C(16) 1.374(5) . . yes C(15) H(15A) 0.951 . . no C(16) C(17) 1.377(5) . . yes C(17) C(18) 1.391(4) . . yes C(17) H(17A) 0.949 . . no C(18) H(18A) 0.948 . . no C(19) C(20) 1.388(4) . . yes C(19) C(24) 1.394(4) . . yes C(20) C(21) 1.395(4) . . yes C(20) H(20A) 0.947 . . no C(21) C(22) 1.380(4) . . yes C(21) H(21A) 0.951 . . no C(22) C(23) 1.375(4) . . yes C(23) C(24) 1.383(4) . . yes C(23) H(23A) 0.948 . . no C(24) H(24A) 0.949 . . no C(25) C(26) 1.378(4) . . yes C(25) C(29) 1.390(4) . . yes C(26) C(27) 1.375(4) . . yes C(26) H(26A) 0.948 . . no C(27) H(27A) 0.948 . . no C(28) C(29) 1.384(4) . . yes C(28) H(28A) 0.950 . . no C(29) H(29A) 0.952 . . no C(30) C(31) 1.374(4) . . yes C(30) C(33) 1.533(4) . . yes C(31) C(32) 1.394(4) . . yes C(31) H(31A) 0.949 . . no C(32) C(34) 1.533(4) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Mn(1) O(1) 180.0 . . 3_756 yes O(1) Mn(1) O(2) 82.32(7) . . . yes O(1) Mn(1) O(2) 97.68(7) . . 3_756 yes O(1) Mn(1) N(2) 87.41(7) . . . yes O(1) Mn(1) N(2) 92.59(7) . . 3_756 yes O(1) Mn(1) O(2) 97.68(7) 3_756 . . yes O(1) Mn(1) O(2) 82.32(7) 3_756 . 3_756 yes O(1) Mn(1) N(2) 92.59(7) 3_756 . . yes O(1) Mn(1) N(2) 87.41(7) 3_756 . 3_756 yes O(2) Mn(1) O(2) 180.0 . . 3_756 yes O(2) Mn(1) N(2) 91.66(7) . . . yes O(2) Mn(1) N(2) 88.34(7) . . 3_756 yes O(2) Mn(1) N(2) 88.34(7) 3_756 . . yes O(2) Mn(1) N(2) 91.66(7) 3_756 . 3_756 yes N(2) Mn(1) N(2) 180.0 . . 3_756 yes N(1) S(1) C(25) 99.4(1) . . . yes Mn(1) O(1) C(30) 128.2(2) . . . yes Mn(1) O(2) C(32) 128.1(2) . . . yes S(1) N(1) C(1) 124.3(2) . . . yes Mn(1) N(2) C(27) 124.6(2) . . . yes Mn(1) N(2) C(28) 118.8(2) . . . yes C(27) N(2) C(28) 116.5(2) . . . yes N(1) C(1) C(2) 127.1(2) . . . yes N(1) C(1) C(6) 114.5(2) . . . yes C(2) C(1) C(6) 118.3(2) . . . yes C(1) C(2) C(3) 119.1(2) . . . yes C(1) C(2) C(7) 122.1(2) . . . yes C(3) C(2) C(7) 118.7(2) . . . yes C(2) C(3) C(4) 123.2(2) . . . yes C(2) C(3) H(3A) 118.5 . . . no C(4) C(3) H(3A) 118.2 . . . no C(3) C(4) C(5) 117.6(2) . . . yes C(3) C(4) C(13) 120.2(2) . . . yes C(5) C(4) C(13) 122.2(2) . . . yes C(4) C(5) C(6) 122.0(2) . . . yes C(4) C(5) H(5A) 119.0 . . . no C(6) C(5) H(5A) 119.0 . . . no C(1) C(6) C(5) 119.8(2) . . . yes C(1) C(6) C(19) 120.1(2) . . . yes C(5) C(6) C(19) 120.1(2) . . . yes C(2) C(7) C(8) 121.6(2) . . . yes C(2) C(7) C(12) 119.5(2) . . . yes C(8) C(7) C(12) 118.9(2) . . . yes C(7) C(8) C(9) 120.7(3) . . . yes C(7) C(8) H(8A) 119.7 . . . no C(9) C(8) H(8A) 119.6 . . . no C(8) C(9) C(10) 119.0(3) . . . yes C(8) C(9) H(9A) 120.4 . . . no C(10) C(9) H(9A) 120.6 . . . no Cl(1) C(10) C(9) 119.3(2) . . . yes Cl(1) C(10) C(11) 118.8(2) . . . yes C(9) C(10) C(11) 121.9(3) . . . yes C(10) C(11) C(12) 118.9(3) . . . yes C(10) C(11) H(11A) 120.6 . . . no C(12) C(11) H(11A) 120.5 . . . no C(7) C(12) C(11) 120.7(3) . . . yes C(7) C(12) H(12A) 119.7 . . . no C(11) C(12) H(12A) 119.7 . . . no C(4) C(13) C(14) 120.4(2) . . . yes C(4) C(13) C(18) 121.8(2) . . . yes C(14) C(13) C(18) 117.7(2) . . . yes C(13) C(14) C(15) 121.4(3) . . . yes C(13) C(14) H(14A) 119.2 . . . no C(15) C(14) H(14A) 119.3 . . . no C(14) C(15) C(16) 119.0(3) . . . yes C(14) C(15) H(15A) 120.5 . . . no C(16) C(15) H(15A) 120.5 . . . no Cl(2) C(16) C(15) 118.6(3) . . . yes Cl(2) C(16) C(17) 119.9(3) . . . yes C(15) C(16) C(17) 121.5(3) . . . yes C(16) C(17) C(18) 119.0(3) . . . yes C(16) C(17) H(17A) 120.3 . . . no C(18) C(17) H(17A) 120.6 . . . no C(13) C(18) C(17) 121.3(3) . . . yes C(13) C(18) H(18A) 119.3 . . . no C(17) C(18) H(18A) 119.4 . . . no C(6) C(19) C(20) 120.3(2) . . . yes C(6) C(19) C(24) 121.2(2) . . . yes C(20) C(19) C(24) 118.5(2) . . . yes C(19) C(20) C(21) 120.6(2) . . . yes C(19) C(20) H(20A) 119.7 . . . no C(21) C(20) H(20A) 119.7 . . . no C(20) C(21) C(22) 119.4(3) . . . yes C(20) C(21) H(21A) 120.3 . . . no C(22) C(21) H(21A) 120.4 . . . no Cl(3) C(22) C(21) 119.5(2) . . . yes Cl(3) C(22) C(23) 119.5(2) . . . yes C(21) C(22) C(23) 120.9(3) . . . yes C(22) C(23) C(24) 119.4(3) . . . yes C(22) C(23) H(23A) 120.4 . . . no C(24) C(23) H(23A) 120.2 . . . no C(19) C(24) C(23) 121.1(3) . . . yes C(19) C(24) H(24A) 119.4 . . . no C(23) C(24) H(24A) 119.5 . . . no S(1) C(25) C(26) 124.6(2) . . . yes S(1) C(25) C(29) 116.8(2) . . . yes C(26) C(25) C(29) 118.6(2) . . . yes C(25) C(26) C(27) 118.8(2) . . . yes C(25) C(26) H(26A) 120.6 . . . no C(27) C(26) H(26A) 120.6 . . . no N(2) C(27) C(26) 124.0(2) . . . yes N(2) C(27) H(27A) 118.0 . . . no C(26) C(27) H(27A) 118.0 . . . no N(2) C(28) C(29) 123.5(2) . . . yes N(2) C(28) H(28A) 118.4 . . . no C(29) C(28) H(28A) 118.1 . . . no C(25) C(29) C(28) 118.6(2) . . . yes C(25) C(29) H(29A) 120.7 . . . no C(28) C(29) H(29A) 120.7 . . . no O(1) C(30) C(31) 128.7(2) . . . yes O(1) C(30) C(33) 113.3(2) . . . yes C(31) C(30) C(33) 117.9(2) . . . yes C(30) C(31) C(32) 122.3(2) . . . yes C(30) C(31) H(31A) 119.0 . . . no C(32) C(31) H(31A) 118.7 . . . no O(2) C(32) C(31) 129.0(3) . . . yes O(2) C(32) C(34) 114.6(2) . . . yes C(31) C(32) C(34) 116.4(2) . . . yes F(1) C(33) F(2) 107.0(2) . . . yes F(1) C(33) F(3) 106.9(3) . . . yes F(1) C(33) C(30) 110.3(2) . . . yes F(2) C(33) F(3) 107.3(2) . . . yes F(2) C(33) C(30) 113.5(2) . . . yes F(3) C(33) C(30) 111.5(2) . . . yes F(4) C(34) F(5) 105.9(3) . . . yes F(4) C(34) F(6) 104.8(3) . . . yes F(4) C(34) C(32) 112.3(3) . . . yes F(5) C(34) F(6) 108.9(3) . . . yes F(5) C(34) C(32) 111.4(3) . . . yes F(6) C(34) C(32) 113.0(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mn(1) O(1) C(30) C(31) 12.2(4) . . . . yes Mn(1) O(1) C(30) C(33) -164.4(2) . . . . yes Mn(1) O(1) C(30) C(31) -12.2(4) . 3_756 3_756 3_756 yes Mn(1) O(1) C(30) C(33) 164.4(2) . 3_756 3_756 3_756 yes Mn(1) O(2) C(32) C(31) -3.5(4) . . . . yes Mn(1) O(2) C(32) C(34) 178.3(2) . . . . yes Mn(1) O(2) C(32) C(31) 3.5(4) . 3_756 3_756 3_756 yes Mn(1) O(2) C(32) C(34) -178.3(2) . 3_756 3_756 3_756 yes Mn(1) N(2) C(27) C(26) -177.3(2) . . . . yes Mn(1) N(2) C(27) H(27A) 2.7 . . . . no Mn(1) N(2) C(28) C(29) 178.9(2) . . . . yes Mn(1) N(2) C(28) H(28A) -1.0 . . . . no Mn(1) N(2) C(27) C(26) 177.3(2) . 3_756 3_756 3_756 yes Mn(1) N(2) C(27) H(27A) -2.7 . 3_756 3_756 3_756 no Mn(1) N(2) C(28) C(29) -178.9(2) . 3_756 3_756 3_756 yes Mn(1) N(2) C(28) H(28A) 1.0 . 3_756 3_756 3_756 no Cl(1) C(10) C(9) C(8) 178.8(2) . . . . yes Cl(1) C(10) C(9) H(9A) -1.0 . . . . no Cl(1) C(10) C(11) C(12) -179.0(2) . . . . yes Cl(1) C(10) C(11) H(11A) 0.9 . . . . no Cl(2) C(16) C(15) C(14) 178.4(2) . . . . yes Cl(2) C(16) C(15) H(15A) -1.6 . . . . no Cl(2) C(16) C(17) C(18) -177.9(3) . . . . yes Cl(2) C(16) C(17) H(17A) 2.1 . . . . no Cl(3) C(22) C(21) C(20) -178.9(2) . . . . yes Cl(3) C(22) C(21) H(21A) 1.2 . . . . no Cl(3) C(22) C(23) C(24) 179.8(2) . . . . yes Cl(3) C(22) C(23) H(23A) -0.7 . . . . no S(1) N(1) C(1) C(2) -16.6(4) . . . . yes S(1) N(1) C(1) C(6) 166.4(2) . . . . yes S(1) C(25) C(26) C(27) -178.9(2) . . . . yes S(1) C(25) C(26) H(26A) 1.0 . . . . no S(1) C(25) C(29) C(28) -179.6(2) . . . . yes S(1) C(25) C(29) H(29A) 0.4 . . . . no F(1) C(33) C(30) O(1) 71.2(3) . . . . yes F(1) C(33) C(30) C(31) -105.8(3) . . . . yes F(2) C(33) C(30) O(1) -168.7(2) . . . . yes F(2) C(33) C(30) C(31) 14.2(4) . . . . yes F(3) C(33) C(30) O(1) -47.4(3) . . . . yes F(3) C(33) C(30) C(31) 135.5(3) . . . . yes F(4) C(34) C(32) O(2) -141.5(3) . . . . yes F(4) C(34) C(32) C(31) 40.1(4) . . . . yes F(5) C(34) C(32) O(2) 99.9(3) . . . . yes F(5) C(34) C(32) C(31) -78.5(4) . . . . yes F(6) C(34) C(32) O(2) -23.2(4) . . . . yes F(6) C(34) C(32) C(31) 158.4(3) . . . . yes O(1) Mn(1) O(2) C(32) 8.4(2) . . . . yes O(1) Mn(1) O(2) C(32) 171.6(2) . . 3_756 3_756 yes O(1) Mn(1) N(2) C(27) 9.3(2) . . . . yes O(1) Mn(1) N(2) C(28) -168.6(2) . . . . yes O(1) Mn(1) N(2) C(27) 170.7(2) . . 3_756 3_756 yes O(1) Mn(1) N(2) C(28) -11.4(2) . . 3_756 3_756 yes O(1) C(30) C(31) C(32) -2.3(5) . . . . yes O(1) C(30) C(31) H(31A) 177.4 . . . . no O(2) Mn(1) O(1) C(30) -12.4(2) . . . . yes O(2) Mn(1) O(1) C(30) -167.6(2) . . 3_756 3_756 yes O(2) Mn(1) N(2) C(27) 91.6(2) . . . . yes O(2) Mn(1) N(2) C(28) -86.4(2) . . . . yes O(2) Mn(1) N(2) C(27) 88.4(2) . . 3_756 3_756 yes O(2) Mn(1) N(2) C(28) -93.6(2) . . 3_756 3_756 yes O(2) C(32) C(31) C(30) -2.5(5) . . . . yes O(2) C(32) C(31) H(31A) 177.9 . . . . no N(1) S(1) C(25) C(26) -15.1(3) . . . . yes N(1) S(1) C(25) C(29) 166.3(2) . . . . yes N(1) C(1) C(2) C(3) -177.9(2) . . . . yes N(1) C(1) C(2) C(7) -2.0(4) . . . . yes N(1) C(1) C(6) C(5) 177.9(2) . . . . yes N(1) C(1) C(6) C(19) -3.8(3) . . . . yes N(2) Mn(1) O(1) C(30) 79.6(2) . . . . yes N(2) Mn(1) O(1) C(30) 100.4(2) . . 3_756 3_756 yes N(2) Mn(1) O(2) C(32) -78.8(2) . . . . yes N(2) Mn(1) O(2) C(32) -101.2(2) . . 3_756 3_756 yes N(2) C(27) C(26) C(25) -1.0(4) . . . . yes N(2) C(27) C(26) H(26A) 179.2 . . . . no N(2) C(28) C(29) C(25) -2.0(4) . . . . yes N(2) C(28) C(29) H(29A) 178.0 . . . . no C(1) N(1) S(1) C(25) -178.8(2) . . . . yes C(1) C(2) C(3) C(4) 0.4(4) . . . . yes C(1) C(2) C(3) H(3A) -179.7 . . . . no C(1) C(2) C(7) C(8) 97.5(3) . . . . yes C(1) C(2) C(7) C(12) -82.7(3) . . . . yes C(1) C(6) C(5) C(4) 0.3(4) . . . . yes C(1) C(6) C(5) H(5A) -179.4 . . . . no C(1) C(6) C(19) C(20) 125.6(3) . . . . yes C(1) C(6) C(19) C(24) -55.0(4) . . . . yes C(2) C(1) C(6) C(5) 0.7(4) . . . . yes C(2) C(1) C(6) C(19) 178.9(2) . . . . yes C(2) C(3) C(4) C(5) 0.6(4) . . . . yes C(2) C(3) C(4) C(13) 179.7(2) . . . . yes C(2) C(7) C(8) C(9) -178.2(2) . . . . yes C(2) C(7) C(8) H(8A) 1.8 . . . . no C(2) C(7) C(12) C(11) 178.0(2) . . . . yes C(2) C(7) C(12) H(12A) -2.2 . . . . no C(3) C(2) C(1) C(6) -1.0(4) . . . . yes C(3) C(2) C(7) C(8) -86.6(3) . . . . yes C(3) C(2) C(7) C(12) 93.2(3) . . . . yes C(3) C(4) C(5) C(6) -1.0(4) . . . . yes C(3) C(4) C(5) H(5A) 178.8 . . . . no C(3) C(4) C(13) C(14) 26.4(4) . . . . yes C(3) C(4) C(13) C(18) -152.6(3) . . . . yes C(4) C(3) C(2) C(7) -175.6(2) . . . . yes C(4) C(5) C(6) C(19) -177.9(2) . . . . yes C(4) C(13) C(14) C(15) -177.0(3) . . . . yes C(4) C(13) C(14) H(14A) 3.1 . . . . no C(4) C(13) C(18) C(17) 177.5(3) . . . . yes C(4) C(13) C(18) H(18A) -2.7 . . . . no C(5) C(4) C(3) H(3A) -179.4 . . . . no C(5) C(4) C(13) C(14) -154.5(3) . . . . yes C(5) C(4) C(13) C(18) 26.5(4) . . . . yes C(5) C(6) C(19) C(20) -56.2(3) . . . . yes C(5) C(6) C(19) C(24) 123.2(3) . . . . yes C(6) C(1) C(2) C(7) 174.8(2) . . . . yes C(6) C(5) C(4) C(13) 179.9(2) . . . . yes C(6) C(19) C(20) C(21) 179.1(2) . . . . yes C(6) C(19) C(20) H(20A) -0.8 . . . . no C(6) C(19) C(24) C(23) -178.1(3) . . . . yes C(6) C(19) C(24) H(24A) 1.9 . . . . no C(7) C(2) C(3) H(3A) 4.3 . . . . no C(7) C(8) C(9) C(10) -0.4(4) . . . . yes C(7) C(8) C(9) H(9A) 179.5 . . . . no C(7) C(12) C(11) C(10) 0.7(4) . . . . yes C(7) C(12) C(11) H(11A) -179.2 . . . . no C(8) C(7) C(12) C(11) -2.2(4) . . . . yes C(8) C(7) C(12) H(12A) 177.6 . . . . no C(8) C(9) C(10) C(11) -1.1(5) . . . . yes C(9) C(8) C(7) C(12) 2.0(4) . . . . yes C(9) C(10) C(11) C(12) 1.0(5) . . . . yes C(9) C(10) C(11) H(11A) -179.1 . . . . no C(10) C(9) C(8) H(8A) 179.7 . . . . no C(10) C(11) C(12) H(12A) -179.1 . . . . no C(11) C(10) C(9) H(9A) 179.0 . . . . no C(12) C(7) C(8) H(8A) -178.0 . . . . no C(13) C(4) C(3) H(3A) -0.2 . . . . no C(13) C(4) C(5) H(5A) -0.3 . . . . no C(13) C(14) C(15) C(16) -0.7(5) . . . . yes C(13) C(14) C(15) H(15A) 179.3 . . . . no C(13) C(18) C(17) C(16) -0.3(5) . . . . yes C(13) C(18) C(17) H(17A) 179.7 . . . . no C(14) C(13) C(18) C(17) -1.6(4) . . . . yes C(14) C(13) C(18) H(18A) 178.3 . . . . no C(14) C(15) C(16) C(17) -1.2(5) . . . . yes C(15) C(14) C(13) C(18) 2.1(4) . . . . yes C(15) C(16) C(17) C(18) 1.7(5) . . . . yes C(15) C(16) C(17) H(17A) -178.3 . . . . no C(16) C(15) C(14) H(14A) 179.2 . . . . no C(16) C(17) C(18) H(18A) 179.9 . . . . no C(17) C(16) C(15) H(15A) 178.8 . . . . no C(18) C(13) C(14) H(14A) -177.8 . . . . no C(19) C(6) C(5) H(5A) 2.3 . . . . no C(19) C(20) C(21) C(22) -0.8(4) . . . . yes C(19) C(20) C(21) H(21A) 179.1 . . . . no C(19) C(24) C(23) C(22) -1.1(4) . . . . yes C(19) C(24) C(23) H(23A) 179.4 . . . . no C(20) C(19) C(24) C(23) 1.3(4) . . . . yes C(20) C(19) C(24) H(24A) -178.7 . . . . no C(20) C(21) C(22) C(23) 1.0(4) . . . . yes C(21) C(20) C(19) C(24) -0.3(4) . . . . yes C(21) C(22) C(23) C(24) -0.1(4) . . . . yes C(21) C(22) C(23) H(23A) 179.5 . . . . no C(22) C(21) C(20) H(20A) 179.1 . . . . no C(22) C(23) C(24) H(24A) 178.9 . . . . no C(23) C(22) C(21) H(21A) -178.9 . . . . no C(24) C(19) C(20) H(20A) 179.8 . . . . no C(25) C(26) C(27) H(27A) 179.0 . . . . no C(25) C(29) C(28) H(28A) 177.9 . . . . no C(26) C(25) C(29) C(28) 1.7(4) . . . . yes C(26) C(25) C(29) H(29A) -178.3 . . . . no C(26) C(27) N(2) C(28) 0.7(4) . . . . yes C(27) N(2) C(28) C(29) 0.8(4) . . . . yes C(27) N(2) C(28) H(28A) -179.2 . . . . no C(27) C(26) C(25) C(29) -0.3(4) . . . . yes C(28) N(2) C(27) H(27A) -179.3 . . . . no C(29) C(25) C(26) H(26A) 179.6 . . . . no C(30) C(31) C(32) C(34) 175.7(3) . . . . yes C(32) C(31) C(30) C(33) 174.2(3) . . . . yes C(33) C(30) C(31) H(31A) -6.1 . . . . no C(34) C(32) C(31) H(31A) -4.0 . . . . no H(8A) C(8) C(9) H(9A) -0.5 . . . . no H(11A) C(11) C(12) H(12A) 1.0 . . . . no H(14A) C(14) C(15) H(15A) -0.8 . . . . no H(17A) C(17) C(18) H(18A) -0.2 . . . . no H(20A) C(20) C(21) H(21A) -1.0 . . . . no H(23A) C(23) C(24) H(24A) -0.6 . . . . no H(26A) C(26) C(27) H(27A) -0.8 . . . . no H(28A) C(28) C(29) H(29A) -2.1 . . . . no H(28A) C(28) C(29) H(29A) -2.1 . . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(11) 3.411(3) . 2_746 ? Cl(1) F(5) 3.435(3) . 4_535 ? Cl(1) C(10) 3.549(3) . 2_746 ? Cl(1) C(29) 3.550(3) . 2_746 ? Cl(1) F(6) 3.578(2) . 4_535 ? Cl(2) F(4) 3.200(3) . 3_846 ? Cl(2) C(3) 3.514(3) . 2_846 ? F(1) C(25) 3.372(3) . 1_565 ? F(1) C(24) 3.510(3) . 1_565 ? F(2) F(4) 3.001(4) . 1_565 ? F(3) C(32) 2.986(3) . 1_565 ? F(3) F(4) 3.045(3) . 1_565 ? F(3) C(27) 3.216(4) . 1_565 ? F(3) N(2) 3.258(3) . 1_565 ? F(3) O(2) 3.290(3) . 1_565 ? F(3) C(34) 3.292(4) . 1_565 ? F(3) C(31) 3.319(4) . 1_565 ? F(3) F(6) 3.370(3) . 1_565 ? F(3) C(26) 3.441(3) . 1_565 ? F(3) C(28) 3.478(3) . 1_565 ? F(4) C(33) 3.455(4) . 1_545 ? F(5) C(10) 3.196(4) . 4_434 ? F(5) C(9) 3.370(4) . 4_434 ? F(5) C(12) 3.372(4) . 4_444 ? F(5) C(11) 3.489(4) . 4_444 ? F(6) C(28) 3.141(3) . 3_746 ? F(6) C(11) 3.300(4) . 4_434 ? F(6) C(29) 3.370(3) . 3_746 ? F(6) C(30) 3.374(3) . 1_545 ? F(6) C(10) 3.455(4) . 4_434 ? F(6) C(31) 3.596(4) . 1_545 ? O(1) C(28) 3.261(3) . 1_565 ? O(1) C(29) 3.333(3) . 1_565 ? O(2) C(28) 3.245(3) . 3_746 ? O(2) C(29) 3.280(3) . 3_746 ? N(1) C(8) 3.556(3) . 1_565 ? C(21) C(21) 3.267(6) . 3_856 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------