# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peter Junk' _publ_contact_author_email peter.junk@sci.monash.edu.au loop_ _publ_author_name G.B.Deacon P.C.Junk A.Urbatsch # Attachment - revised ttfpz.cif' #Divalent metal complexes (Ca, Sr, Ba, Yb) of the unsymmetrical 3 #(2' thienyl) 5 (trifluoromethyl)pyrazolate ligand #Glen B. Deacon, Peter C. Junk and Aron Urbatsch data_compound1 _database_code_depnum_ccdc_archive 'CCDC 794838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Yb(ttfpz)2(thf)4] ; _chemical_name_common (Yb(ttfpz)2(thf)4) _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 F6 N4 O4 S2 Yb' _chemical_formula_sum 'C32 H40 F6 N4 O4 S2 Yb' _chemical_formula_weight 895.84 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.2265(3) _cell_length_b 9.9967(2) _cell_length_c 19.4434(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3542.68(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 102651 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 2.831 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4838 _exptl_absorpt_correction_T_max 0.6761 _exptl_absorpt_process_details SADABS _exptl_special_details ; Thiophene groups were disordered over two positions, their occupancies were freely refined against each other (45:55 for S(1) and 70:30 for S(2)). Both parts of the disordered groups were restrained using DFIX and DANG commands. Both components of the disorder of thiophene S(2) were restrained using SIMU. Two of the thf ligands (O(1) and O(3)) were also disordered over two positions. Their occupancies were freely refined against each other (62:38 and 70:30). The TWIN command was employed and the BASF factor was refined to be approximately 0.15. ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102651 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8102 _reflns_number_gt 7738 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_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 0.144(7) _refine_ls_number_reflns 8102 _refine_ls_number_parameters 546 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.073 _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 Yb1 Yb 0.127485(6) 0.288649(10) 0.17493(2) 0.02106(4) Uani 1 1 d . D . S1 S -0.1162(3) 0.3864(4) -0.05934(19) 0.0451(12) Uani 0.452(6) 1 d PD A 1 S1A S -0.0390(3) 0.5419(4) 0.0314(3) 0.0266(8) Uani 0.548(6) 1 d PD A 2 S2 S 0.27992(16) 0.55572(19) 0.33105(17) 0.0270(6) Uani 0.696(5) 1 d PU B 1 S2A S 0.3875(3) 0.3786(6) 0.3936(4) 0.0228(13) Uani 0.304(5) 1 d PDU B 2 F1 F 0.01317(19) -0.1382(3) -0.0052(2) 0.0780(10) Uani 1 1 d . E . F2 F 0.12332(15) -0.0856(4) 0.0019(2) 0.0648(12) Uani 1 1 d . E . F3 F 0.0632(3) -0.1249(3) 0.09421(18) 0.1140(18) Uani 1 1 d . E . F4 F 0.24415(16) -0.1264(3) 0.36166(18) 0.0636(8) Uani 1 1 d . E . F5 F 0.13360(15) -0.0797(4) 0.3417(3) 0.0606(11) Uani 1 1 d . E . F6 F 0.2040(2) -0.1274(3) 0.25952(16) 0.0735(10) Uani 1 1 d . E . O1 O 0.19801(12) 0.4768(3) 0.12612(13) 0.0275(5) Uani 1 1 d . D . O2 O 0.23511(13) 0.1901(3) 0.11130(13) 0.0293(6) Uani 1 1 d . . . O3 O 0.01880(14) 0.1951(3) 0.23791(14) 0.0326(6) Uani 1 1 d . . . O4 O 0.05797(11) 0.4889(3) 0.21404(14) 0.0299(6) Uani 1 1 d . . . N1 N 0.04019(15) 0.2814(3) 0.07390(15) 0.0222(6) Uani 1 1 d . . . N2 N 0.06855(16) 0.1563(3) 0.08421(16) 0.0273(6) Uani 1 1 d . D . N3 N 0.21603(15) 0.2878(3) 0.27588(16) 0.0214(6) Uani 1 1 d . . . N4 N 0.18733(14) 0.1627(3) 0.26759(15) 0.0207(6) Uani 1 1 d . D . C1 C -0.00855(17) 0.2731(3) 0.02214(17) 0.0212(7) Uani 1 1 d . A . C2 C -0.01197(19) 0.1426(4) -0.00272(19) 0.0261(7) Uani 1 1 d . . . H2 H -0.0411 0.1085 -0.0393 0.031 Uiso 1 1 calc R E . C3 C 0.03702(19) 0.0752(4) 0.0384(2) 0.0275(8) Uani 1 1 d . D . C4 C -0.04735(17) 0.3902(3) -0.00260(17) 0.0241(7) Uani 1 1 d D . . C5 C -0.0339(13) 0.5244(12) 0.0239(14) 0.047(10) Uani 0.452(6) 1 d PD A 1 H5 H 0.0027 0.5510 0.0559 0.056 Uiso 0.452(6) 1 calc PR A 1 C5A C -0.0883(4) 0.3952(10) -0.0675(5) 0.024(2) Uani 0.548(6) 1 d PD A 2 H5A H -0.0979 0.3224 -0.0976 0.029 Uiso 0.548(6) 1 calc PR A 2 C6 C -0.0888(10) 0.6089(11) -0.0091(7) 0.027(3) Uani 0.452(6) 1 d PD A 1 H6 H -0.0938 0.7006 0.0028 0.033 Uiso 0.452(6) 1 calc PR A 1 C6A C -0.1115(5) 0.5345(9) -0.0769(5) 0.039(3) Uani 0.548(6) 1 d PD A 2 H6A H -0.1413 0.5618 -0.1145 0.047 Uiso 0.548(6) 1 calc PR A 2 C7 C -0.1316(7) 0.5529(10) -0.0564(6) 0.036(4) Uani 0.452(6) 1 d PD A 1 H7 H -0.1657 0.5996 -0.0844 0.044 Uiso 0.452(6) 1 calc PR A 1 C7A C -0.0881(7) 0.6204(10) -0.0291(5) 0.028(3) Uani 0.548(6) 1 d PD A 2 H7A H -0.0981 0.7137 -0.0294 0.033 Uiso 0.548(6) 1 calc PR A 2 C8 C 0.0588(2) -0.0672(4) 0.0352(2) 0.0420(10) Uani 1 1 d . . . C9 C 0.26860(17) 0.2803(3) 0.32477(16) 0.0192(6) Uani 1 1 d . B . C10 C 0.27437(18) 0.1491(4) 0.34900(19) 0.0244(7) Uani 1 1 d . . . H10 H 0.3065 0.1150 0.3832 0.029 Uiso 1 1 calc R E . C11 C 0.22241(17) 0.0814(3) 0.31152(18) 0.0227(7) Uani 1 1 d . D . C12 C 0.30947(17) 0.3978(3) 0.34719(16) 0.0213(7) Uani 1 1 d D . . C13 C 0.3716(6) 0.4049(13) 0.3861(7) 0.026(2) Uani 0.696(5) 1 d PU B 1 H13 H 0.3970 0.3276 0.4018 0.032 Uiso 0.696(5) 1 calc PR B 1 C13A C 0.2945(14) 0.5395(11) 0.3329(17) 0.040(6) Uani 0.304(5) 1 d PDU B 2 H13A H 0.2549 0.5750 0.3069 0.048 Uiso 0.304(5) 1 calc PR B 2 C14 C 0.3949(10) 0.5342(10) 0.4011(12) 0.030(2) Uani 0.696(5) 1 d PU B 1 H14 H 0.4384 0.5544 0.4261 0.036 Uiso 0.696(5) 1 calc PR B 1 C14A C 0.3530(16) 0.6145(16) 0.3669(18) 0.034(5) Uani 0.304(5) 1 d PDU B 2 H14A H 0.3554 0.7094 0.3646 0.041 Uiso 0.304(5) 1 calc PR B 2 C15 C 0.3480(7) 0.6287(9) 0.3758(7) 0.029(2) Uani 0.696(5) 1 d PU B 1 H15 H 0.3532 0.7224 0.3824 0.034 Uiso 0.696(5) 1 calc PR B 1 C15A C 0.403(2) 0.5436(13) 0.401(3) 0.027(4) Uani 0.304(5) 1 d PDU B 2 H15A H 0.4418 0.5816 0.4269 0.032 Uiso 0.304(5) 1 calc PR B 2 C16 C 0.2017(2) -0.0612(4) 0.3168(2) 0.0328(8) Uani 1 1 d . . . C17 C 0.1769(2) 0.5601(4) 0.0698(2) 0.0459(10) Uani 1 1 d . . . H17A H 0.1355 0.6178 0.0840 0.055 Uiso 1 1 calc R C 1 H17B H 0.1601 0.5035 0.0312 0.055 Uiso 1 1 calc R C 1 C18 C 0.2367(5) 0.6423(16) 0.0473(10) 0.071(5) Uani 0.70(3) 1 d P D 1 H18A H 0.2203 0.7334 0.0347 0.085 Uiso 0.70(3) 1 calc PR D 1 H18B H 0.2633 0.6017 0.0081 0.085 Uiso 0.70(3) 1 calc PR D 1 C18A C 0.2306(7) 0.6907(15) 0.0836(11) 0.024(4) Uani 0.30(3) 1 d P D 2 H18C H 0.2472 0.7301 0.0396 0.029 Uiso 0.30(3) 1 calc PR D 2 H18D H 0.2044 0.7602 0.1104 0.029 Uiso 0.30(3) 1 calc PR D 2 C19 C 0.2876(2) 0.6426(4) 0.1194(3) 0.0539(13) Uani 1 1 d . . . H19A H 0.3399 0.6622 0.1101 0.065 Uiso 1 1 calc R D 1 H19B H 0.2684 0.7052 0.1545 0.065 Uiso 1 1 calc R D 1 C20 C 0.27522(17) 0.4997(4) 0.1383(2) 0.0332(9) Uani 1 1 d . D . H20A H 0.3056 0.4398 0.1095 0.040 Uiso 1 1 calc R . . H20B H 0.2876 0.4841 0.1873 0.040 Uiso 1 1 calc R . . C21 C 0.2415(2) 0.1911(4) 0.0367(2) 0.0314(8) Uani 1 1 d . . . H21A H 0.2623 0.2769 0.0205 0.038 Uiso 1 1 calc R . . H21B H 0.1929 0.1776 0.0149 0.038 Uiso 1 1 calc R . . C22 C 0.2929(2) 0.0752(4) 0.0200(2) 0.0370(9) Uani 1 1 d . . . H22A H 0.2651 -0.0081 0.0110 0.044 Uiso 1 1 calc R . . H22B H 0.3240 0.0959 -0.0204 0.044 Uiso 1 1 calc R . . C23 C 0.3385(3) 0.0630(6) 0.0844(2) 0.0595(14) Uani 1 1 d . . . H23A H 0.3566 -0.0296 0.0903 0.071 Uiso 1 1 calc R . . H23B H 0.3810 0.1246 0.0828 0.071 Uiso 1 1 calc R . . C24 C 0.2886(3) 0.0994(6) 0.1400(2) 0.0577(14) Uani 1 1 d . . . H24A H 0.2641 0.0187 0.1585 0.069 Uiso 1 1 calc R . . H24B H 0.3159 0.1433 0.1778 0.069 Uiso 1 1 calc R . . C25 C -0.0364(5) 0.1083(12) 0.2052(4) 0.031(2) Uani 0.62(2) 1 d P E 1 H25A H -0.0139 0.0243 0.1884 0.037 Uiso 0.62(2) 1 calc PR E 1 H25B H -0.0605 0.1544 0.1662 0.037 Uiso 0.62(2) 1 calc PR E 1 C25A C -0.0548(7) 0.1664(17) 0.2153(7) 0.025(3) Uani 0.38(2) 1 d P E 2 H25C H -0.0575 0.1612 0.1645 0.029 Uiso 0.38(2) 1 calc PR E 2 H25D H -0.0897 0.2353 0.2317 0.029 Uiso 0.38(2) 1 calc PR E 2 C26 C -0.0900(5) 0.0811(13) 0.2623(5) 0.038(2) Uani 0.62(2) 1 d P E 1 H26A H -0.1179 -0.0024 0.2540 0.046 Uiso 0.62(2) 1 calc PR E 1 H26B H -0.1248 0.1563 0.2682 0.046 Uiso 0.62(2) 1 calc PR E 1 C26A C -0.0705(11) 0.0342(19) 0.2472(9) 0.039(4) Uani 0.38(2) 1 d P E 2 H26C H -0.0429 -0.0393 0.2249 0.047 Uiso 0.38(2) 1 calc PR E 2 H26D H -0.1235 0.0131 0.2475 0.047 Uiso 0.38(2) 1 calc PR E 2 C27 C -0.0396(2) 0.0678(4) 0.3235(2) 0.0404(9) Uani 1 1 d . . . H27A H -0.0666 0.0797 0.3673 0.049 Uiso 1 1 calc R E 1 H27B H -0.0145 -0.0201 0.3239 0.049 Uiso 1 1 calc R E 1 C28 C 0.01377(19) 0.1802(4) 0.31146(19) 0.0275(7) Uani 1 1 d . E . H28A H -0.0042 0.2638 0.3329 0.033 Uiso 1 1 calc R . . H28B H 0.0623 0.1581 0.3312 0.033 Uiso 1 1 calc R . . C29 C -0.02122(17) 0.4994(4) 0.2149(2) 0.0286(8) Uani 1 1 d . E . H29A H -0.0417 0.4588 0.2572 0.034 Uiso 1 1 calc R . . H29B H -0.0429 0.4543 0.1744 0.034 Uiso 1 1 calc R . . C30 C -0.0362(2) 0.6480(4) 0.2130(2) 0.0359(8) Uani 1 1 d . . . H30A H -0.0352 0.6825 0.1653 0.043 Uiso 1 1 calc R E . H30B H -0.0842 0.6695 0.2341 0.043 Uiso 1 1 calc R . . C31 C 0.0262(3) 0.7040(4) 0.2548(3) 0.0455(11) Uani 1 1 d . E . H31A H 0.0380 0.7964 0.2403 0.055 Uiso 1 1 calc R . . H31B H 0.0140 0.7042 0.3044 0.055 Uiso 1 1 calc R . . C32 C 0.0892(2) 0.6109(5) 0.2402(3) 0.0520(12) Uani 1 1 d . E . H32A H 0.1226 0.6510 0.2057 0.062 Uiso 1 1 calc R . . H32B H 0.1173 0.5931 0.2827 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01705(6) 0.02447(6) 0.02166(7) 0.00180(10) -0.00331(8) -0.00056(4) S1 0.045(3) 0.049(2) 0.041(2) -0.0053(16) -0.0282(17) 0.0055(18) S1A 0.0283(18) 0.0285(12) 0.0231(13) -0.0007(10) 0.0039(11) 0.0026(10) S2 0.0198(11) 0.0222(8) 0.0390(10) 0.0010(6) -0.0053(9) -0.0016(6) S2A 0.017(2) 0.027(3) 0.024(2) 0.0064(17) -0.0063(18) 0.000(2) F1 0.083(2) 0.0362(15) 0.115(3) -0.0219(17) -0.013(2) -0.0086(15) F2 0.058(2) 0.052(2) 0.084(3) -0.012(2) 0.0102(14) 0.0165(13) F3 0.239(5) 0.0427(19) 0.060(2) 0.0206(17) 0.026(3) 0.056(3) F4 0.0709(18) 0.0289(13) 0.091(2) 0.0190(14) -0.0297(17) 0.0021(13) F5 0.0390(17) 0.0305(18) 0.112(3) 0.0129(18) 0.0213(15) -0.0093(11) F6 0.129(3) 0.0371(15) 0.0544(18) -0.0184(14) 0.0273(18) -0.0256(17) O1 0.0197(11) 0.0344(13) 0.0286(13) 0.0068(11) -0.0022(9) 0.0003(10) O2 0.0262(12) 0.0389(14) 0.0229(13) -0.0010(11) -0.0002(10) 0.0079(11) O3 0.0245(12) 0.0474(16) 0.0260(14) 0.0087(11) -0.0035(10) -0.0126(11) O4 0.0197(11) 0.0332(14) 0.0369(15) -0.0091(11) 0.0000(10) 0.0035(10) N1 0.0218(14) 0.0240(15) 0.0207(14) 0.0019(11) 0.0008(11) 0.0016(11) N2 0.0262(14) 0.0223(14) 0.0335(17) 0.0004(13) -0.0021(13) 0.0005(12) N3 0.0195(13) 0.0216(15) 0.0229(15) 0.0019(11) -0.0019(11) -0.0011(10) N4 0.0195(12) 0.0196(13) 0.0231(14) 0.0005(11) -0.0020(11) -0.0019(11) C1 0.0180(15) 0.0270(17) 0.0187(16) -0.0014(13) 0.0043(12) -0.0034(13) C2 0.0247(16) 0.0252(17) 0.0285(19) -0.0045(14) -0.0006(14) -0.0096(14) C3 0.0274(17) 0.0241(17) 0.0312(19) -0.0009(15) 0.0010(14) -0.0089(14) C4 0.0190(15) 0.0264(17) 0.0267(18) 0.0021(14) 0.0003(13) -0.0039(13) C5 0.018(7) 0.075(17) 0.047(15) 0.008(9) 0.002(7) 0.026(8) C5A 0.010(4) 0.024(4) 0.039(5) 0.004(3) 0.000(4) 0.001(3) C6 0.045(7) 0.018(5) 0.019(7) 0.001(4) 0.014(5) -0.004(4) C6A 0.022(5) 0.049(6) 0.045(6) 0.022(5) -0.015(4) -0.003(4) C7 0.023(7) 0.058(8) 0.029(7) -0.006(6) -0.009(5) 0.025(6) C7A 0.018(5) 0.035(5) 0.030(8) 0.021(4) 0.012(5) 0.011(4) C8 0.042(2) 0.028(2) 0.056(3) -0.0045(19) -0.002(2) -0.0041(17) C9 0.0169(14) 0.0254(17) 0.0154(15) 0.0006(12) 0.0022(12) 0.0046(12) C10 0.0232(16) 0.0253(17) 0.0247(17) 0.0018(14) 0.0002(14) 0.0059(14) C11 0.0220(15) 0.0210(16) 0.0253(17) -0.0006(14) 0.0034(13) 0.0028(12) C12 0.0198(14) 0.0264(17) 0.0177(15) 0.0010(13) 0.0040(12) -0.0025(13) C13 0.027(5) 0.029(5) 0.024(4) 0.002(3) -0.012(3) 0.014(3) C13A 0.021(10) 0.060(11) 0.040(10) -0.001(8) 0.015(7) 0.000(7) C14 0.023(5) 0.040(4) 0.028(4) 0.002(4) -0.012(4) -0.003(4) C14A 0.030(8) 0.039(9) 0.034(8) -0.004(7) 0.017(6) -0.009(7) C15 0.032(4) 0.020(3) 0.033(5) 0.000(3) 0.007(4) 0.002(3) C15A 0.016(7) 0.034(7) 0.030(7) 0.000(6) 0.005(6) -0.014(6) C16 0.0324(19) 0.0233(18) 0.043(2) 0.0003(16) -0.0016(16) 0.0014(14) C17 0.050(2) 0.036(2) 0.052(3) 0.0179(19) -0.017(2) -0.0042(18) C18 0.056(5) 0.067(8) 0.088(10) 0.049(8) -0.014(5) -0.012(5) C18A 0.023(6) 0.022(7) 0.028(10) 0.005(6) -0.003(5) -0.005(5) C19 0.033(2) 0.033(2) 0.095(4) -0.011(2) 0.018(2) -0.0064(18) C20 0.0210(17) 0.047(3) 0.031(2) 0.0053(17) -0.0030(14) -0.0082(16) C21 0.0306(19) 0.039(2) 0.0244(19) 0.0033(15) 0.0031(16) 0.0038(16) C22 0.035(2) 0.042(2) 0.034(2) -0.0093(19) 0.0062(17) 0.0014(18) C23 0.060(3) 0.077(3) 0.042(2) 0.005(2) 0.005(2) 0.042(3) C24 0.053(3) 0.081(4) 0.039(2) 0.005(2) -0.001(2) 0.044(3) C25 0.031(4) 0.034(5) 0.027(3) -0.006(3) 0.005(3) -0.008(3) C25A 0.018(6) 0.027(7) 0.028(6) 0.000(5) -0.009(4) -0.013(5) C26 0.031(4) 0.054(6) 0.030(4) -0.011(4) 0.011(3) -0.019(4) C26A 0.044(9) 0.049(9) 0.023(7) -0.011(6) -0.006(6) -0.013(7) C27 0.050(2) 0.044(2) 0.027(2) 0.0074(18) 0.0098(17) -0.0073(19) C28 0.0239(17) 0.0354(19) 0.0231(18) -0.0052(15) -0.0010(14) 0.0049(15) C29 0.0212(16) 0.035(2) 0.029(2) 0.0016(14) 0.0016(14) 0.0013(14) C30 0.0344(19) 0.038(2) 0.035(2) -0.0018(17) 0.0014(16) 0.0090(17) C31 0.044(2) 0.045(3) 0.048(3) -0.022(2) 0.004(2) 0.0012(19) C32 0.033(2) 0.060(3) 0.064(3) -0.038(2) -0.004(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N2 2.453(3) . ? Yb1 N4 2.454(3) . ? Yb1 O1 2.468(3) . ? Yb1 O4 2.488(2) . ? Yb1 O3 2.510(2) . ? Yb1 O2 2.520(2) . ? Yb1 N1 2.529(3) . ? Yb1 N3 2.541(3) . ? S1 C4 1.671(4) . ? S1 C7 1.689(9) . ? S1A C4 1.661(5) . ? S1A C7A 1.675(8) . ? S2 C15 1.682(10) . ? S2 C12 1.697(4) . ? S2A C15A 1.679(10) . ? S2A C12 1.694(6) . ? F1 C8 1.345(5) . ? F2 C8 1.355(5) . ? F3 C8 1.288(6) . ? F4 C16 1.335(5) . ? F5 C16 1.346(5) . ? F6 C16 1.296(5) . ? O1 C17 1.428(4) . ? O1 C20 1.446(4) . ? O2 C24 1.444(5) . ? O2 C21 1.454(5) . ? O3 C28 1.441(4) . ? O3 C25A 1.441(10) . ? O3 C25 1.472(8) . ? O4 C32 1.438(5) . ? O4 C29 1.447(4) . ? N1 C1 1.345(5) . ? N1 N2 1.368(4) . ? N2 C3 1.334(5) . ? N3 C9 1.352(4) . ? N3 N4 1.365(4) . ? N4 C11 1.341(4) . ? C1 C2 1.392(5) . ? C1 C4 1.450(5) . ? C2 C3 1.376(5) . ? C3 C8 1.478(5) . ? C4 C5 1.457(10) . ? C4 C5A 1.468(8) . ? C5 C6 1.458(9) . ? C5A C6A 1.467(8) . ? C6 C7 1.330(9) . ? C6A C7A 1.334(9) . ? C9 C10 1.397(5) . ? C9 C12 1.458(4) . ? C10 C11 1.373(5) . ? C11 C16 1.478(5) . ? C12 C13 1.365(11) . ? C12 C13A 1.469(10) . ? C13 C14 1.392(15) . ? C13A C14A 1.463(10) . ? C14 C15 1.366(10) . ? C14A C15A 1.328(10) . ? C17 C18 1.434(9) . ? C17 C18A 1.653(15) . ? C18 C19 1.680(16) . ? C18A C19 1.339(15) . ? C19 C20 1.492(6) . ? C21 C22 1.526(5) . ? C22 C23 1.507(6) . ? C23 C24 1.458(6) . ? C25 C26 1.504(13) . ? C25A C26A 1.49(2) . ? C26 C27 1.510(11) . ? C26A C27 1.621(15) . ? C27 C28 1.504(5) . ? C29 C30 1.511(5) . ? C30 C31 1.506(6) . ? C31 C32 1.505(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Yb1 N4 116.49(8) . . ? N2 Yb1 O1 111.26(10) . . ? N4 Yb1 O1 116.22(8) . . ? N2 Yb1 O4 115.51(9) . . ? N4 Yb1 O4 114.50(9) . . ? O1 Yb1 O4 76.68(8) . . ? N2 Yb1 O3 78.70(9) . . ? N4 Yb1 O3 78.54(9) . . ? O1 Yb1 O3 151.99(9) . . ? O4 Yb1 O3 75.46(9) . . ? N2 Yb1 O2 77.12(9) . . ? N4 Yb1 O2 79.28(9) . . ? O1 Yb1 O2 72.75(8) . . ? O4 Yb1 O2 149.42(8) . . ? O3 Yb1 O2 135.10(8) . . ? N2 Yb1 N1 31.83(9) . . ? N4 Yb1 N1 146.66(9) . . ? O1 Yb1 N1 92.91(8) . . ? O4 Yb1 N1 86.56(8) . . ? O3 Yb1 N1 82.63(9) . . ? O2 Yb1 N1 95.58(9) . . ? N2 Yb1 N3 146.30(9) . . ? N4 Yb1 N3 31.66(9) . . ? O1 Yb1 N3 88.20(8) . . ? O4 Yb1 N3 95.16(9) . . ? O3 Yb1 N3 97.08(9) . . ? O2 Yb1 N3 83.31(9) . . ? N1 Yb1 N3 178.14(8) . . ? C4 S1 C7 94.6(5) . . ? C4 S1A C7A 95.7(4) . . ? C15 S2 C12 94.2(3) . . ? C15A S2A C12 94.2(8) . . ? C17 O1 C20 107.2(3) . . ? C17 O1 Yb1 126.8(2) . . ? C20 O1 Yb1 124.4(2) . . ? C24 O2 C21 109.6(3) . . ? C24 O2 Yb1 125.6(2) . . ? C21 O2 Yb1 123.3(2) . . ? C28 O3 C25A 102.9(6) . . ? C28 O3 C25 108.9(4) . . ? C25A O3 C25 27.8(5) . . ? C28 O3 Yb1 125.0(2) . . ? C25A O3 Yb1 131.3(5) . . ? C25 O3 Yb1 123.2(3) . . ? C32 O4 C29 109.2(3) . . ? C32 O4 Yb1 126.1(2) . . ? C29 O4 Yb1 124.7(2) . . ? C1 N1 N2 107.6(3) . . ? C1 N1 Yb1 176.9(2) . . ? N2 N1 Yb1 71.01(18) . . ? C3 N2 N1 107.2(3) . . ? C3 N2 Yb1 175.0(3) . . ? N1 N2 Yb1 77.15(19) . . ? C9 N3 N4 107.7(3) . . ? C9 N3 Yb1 173.5(2) . . ? N4 N3 Yb1 70.63(16) . . ? C11 N4 N3 107.3(3) . . ? C11 N4 Yb1 172.1(2) . . ? N3 N4 Yb1 77.71(17) . . ? N1 C1 C2 110.4(3) . . ? N1 C1 C4 121.3(3) . . ? C2 C1 C4 128.3(3) . . ? C3 C2 C1 103.2(3) . . ? N2 C3 C2 111.7(3) . . ? N2 C3 C8 119.9(3) . . ? C2 C3 C8 128.4(3) . . ? C1 C4 C5 123.0(7) . . ? C1 C4 C5A 124.1(5) . . ? C5 C4 C5A 111.0(8) . . ? C1 C4 S1A 124.1(3) . . ? C5 C4 S1A 5.0(15) . . ? C5A C4 S1A 111.0(5) . . ? C1 C4 S1 124.5(3) . . ? C5 C4 S1 112.4(6) . . ? C5A C4 S1 18.4(3) . . ? S1A C4 S1 110.7(3) . . ? C4 C5 C6 105.2(9) . . ? C6A C5A C4 106.6(7) . . ? C7 C6 C5 117.5(9) . . ? C7A C6A C5A 115.7(8) . . ? C6 C7 S1 109.9(7) . . ? C6A C7A S1A 111.0(7) . . ? F3 C8 F1 108.8(4) . . ? F3 C8 F2 108.0(4) . . ? F1 C8 F2 100.8(4) . . ? F3 C8 C3 114.2(4) . . ? F1 C8 C3 111.6(4) . . ? F2 C8 C3 112.6(4) . . ? N3 C9 C10 110.1(3) . . ? N3 C9 C12 121.8(3) . . ? C10 C9 C12 128.1(3) . . ? C11 C10 C9 103.4(3) . . ? N4 C11 C10 111.6(3) . . ? N4 C11 C16 120.5(3) . . ? C10 C11 C16 127.9(3) . . ? C13 C12 C9 129.2(6) . . ? C13 C12 C13A 102.1(10) . . ? C9 C12 C13A 128.7(8) . . ? C13 C12 S2A 9.6(7) . . ? C9 C12 S2A 119.8(3) . . ? C13A C12 S2A 111.5(8) . . ? C13 C12 S2 108.5(6) . . ? C9 C12 S2 122.1(2) . . ? C13A C12 S2 7.8(11) . . ? S2A C12 S2 118.0(3) . . ? C12 C13 C14 114.7(8) . . ? C14A C13A C12 105.8(10) . . ? C15 C14 C13 112.1(8) . . ? C15A C14A C13A 116.8(12) . . ? C14 C15 S2 110.4(7) . . ? C14A C15A S2A 111.6(11) . . ? F6 C16 F4 107.1(4) . . ? F6 C16 F5 105.6(4) . . ? F4 C16 F5 103.4(4) . . ? F6 C16 C11 115.1(3) . . ? F4 C16 C11 111.6(3) . . ? F5 C16 C11 113.1(3) . . ? O1 C17 C18 111.3(5) . . ? O1 C17 C18A 100.2(6) . . ? C18 C17 C18A 31.5(6) . . ? C17 C18 C19 99.5(8) . . ? C19 C18A C17 105.0(9) . . ? C18A C19 C20 110.8(7) . . ? C18A C19 C18 30.7(6) . . ? C20 C19 C18 97.0(5) . . ? O1 C20 C19 105.0(3) . . ? O2 C21 C22 104.9(3) . . ? C23 C22 C21 102.9(3) . . ? C24 C23 C22 104.6(4) . . ? O2 C24 C23 106.9(4) . . ? O3 C25 C26 103.4(7) . . ? O3 C25A C26A 103.2(12) . . ? C25 C26 C27 101.6(7) . . ? C25A C26A C27 97.6(11) . . ? C28 C27 C26 101.8(5) . . ? C28 C27 C26A 103.7(6) . . ? C26 C27 C26A 23.9(6) . . ? O3 C28 C27 105.8(3) . . ? O4 C29 C30 104.5(3) . . ? C31 C30 C29 102.5(3) . . ? C32 C31 C30 104.1(3) . . ? O4 C32 C31 106.8(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.393 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.081 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 794839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Ca(ttfpz)2(thf)4] ; _chemical_name_common (Ca(ttfpz)2(thf)4) _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 Ca F6 N4 O4 S2' _chemical_formula_sum 'C32 H40 Ca F6 N4 O4 S2' _chemical_formula_weight 762.88 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.1794(3) _cell_length_b 9.9826(2) _cell_length_c 19.4586(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3531.30(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 42699 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.370 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8972 _exptl_absorpt_correction_T_max 0.9640 _exptl_absorpt_process_details SADABS _exptl_special_details ; Thiophene groups were disordered over two positions, their occupancies were freely refined against each other (48:52 for S(1) and 70:30 for S(2)). Both parts of the disordered groups were restrained using DFIX and DANG commands, they were also FLATtened. EADP constraints were applied on disordered atoms C(5) and C(13A) with atoms C(5A) and C(13) respectively used as reference. Thiophene rings S(1), S(1A) and S(2A) were also restrained using SIMU. Thf-molecules O(1,2 and 3) were also disordered and the occupancies of the involved atoms were freely refined against each other (refined occupancies were 40:60 (O(1)), 70:30 (O(2)) and 52:48 (O(3))). SIMU and DFIX restraints were also applied on some involved atoms. Additionally, the structure was inverted. ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42699 _diffrn_reflns_av_R_equivalents 0.1090 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7644 _reflns_number_gt 5730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_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 0.08(6) _refine_ls_number_reflns 7644 _refine_ls_number_parameters 546 _refine_ls_number_restraints 148 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.003 _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 Ca1 Ca 0.87232(5) 0.71284(8) 0.82513(6) 0.0215(2) Uani 1 1 d . D . S1 S 1.0383(3) 0.4551(3) 0.9680(2) 0.0268(10) Uani 0.482(5) 1 d PDU A 2 S1A S 1.1152(2) 0.6138(4) 1.0583(2) 0.0503(13) Uani 0.518(5) 1 d PDU A 1 S2 S 0.72057(14) 0.4416(2) 0.66979(17) 0.0264(6) Uani 0.702(5) 1 d P B 1 S2A S 0.6126(4) 0.6187(8) 0.6073(5) 0.0294(17) Uani 0.298(5) 1 d PDU B 2 F1 F 0.9858(3) 1.1365(4) 1.0042(3) 0.0870(16) Uani 1 1 d . F . F2 F 0.8776(2) 1.0864(4) 0.9985(3) 0.0750(14) Uani 1 1 d . F . F3 F 0.9354(5) 1.1250(5) 0.9064(3) 0.149(3) Uani 1 1 d . F . F4 F 0.7553(2) 1.1249(3) 0.6389(3) 0.0719(14) Uani 1 1 d . F . F5 F 0.86572(18) 1.0786(3) 0.6576(3) 0.0652(13) Uani 1 1 d . F . F6 F 0.7969(3) 1.1256(4) 0.7414(2) 0.0856(16) Uani 1 1 d . F . O1 O 0.80265(18) 0.5278(4) 0.87325(19) 0.0281(8) Uani 1 1 d . D . O2 O 0.76562(19) 0.8117(4) 0.88768(18) 0.0306(9) Uani 1 1 d D . . O3 O 0.97928(19) 0.8071(4) 0.76256(19) 0.0331(9) Uani 1 1 d . . . O4 O 0.94124(19) 0.5169(4) 0.7860(2) 0.0311(9) Uani 1 1 d . . . N1 N 0.9590(2) 0.7187(4) 0.9247(2) 0.0231(9) Uani 1 1 d . . . N2 N 0.9309(2) 0.8424(4) 0.9141(2) 0.0265(10) Uani 1 1 d . D . N3 N 0.7844(2) 0.7106(4) 0.7254(2) 0.0213(8) Uani 1 1 d . . . N4 N 0.8132(2) 0.8365(4) 0.7334(2) 0.0215(9) Uani 1 1 d . D . C1 C 1.0080(2) 0.7261(4) 0.9770(2) 0.0188(10) Uani 1 1 d . A . C2 C 1.0106(3) 0.8572(5) 1.0008(3) 0.0264(12) Uani 1 1 d . . . H2 H 1.0396 0.8916 1.0374 0.032 Uiso 1 1 calc R F . C3 C 0.9624(3) 0.9257(5) 0.9602(3) 0.0275(12) Uani 1 1 d . D . C4 C 1.0463(2) 0.6103(4) 1.0013(2) 0.0256(11) Uani 1 1 d D . . C5 C 1.0890(6) 0.6081(12) 1.0655(6) 0.026(2) Uani 0.482(5) 1 d PDU A 2 H5 H 1.0992 0.6823 1.0946 0.031 Uiso 0.482(5) 1 calc PR A 2 C5A C 1.0338(9) 0.4760(11) 0.9742(8) 0.026(2) Uani 0.52 1 d PDU A 1 H5A H 0.9989 0.4506 0.9403 0.031 Uiso 0.518(5) 1 calc PR A 1 C6 C 1.1127(6) 0.4692(11) 1.0760(6) 0.028(3) Uani 0.482(5) 1 d PDU A 2 H6 H 1.1428 0.4439 1.1138 0.033 Uiso 0.482(5) 1 calc PR A 2 C6A C 1.0859(9) 0.3882(12) 1.0098(7) 0.034(3) Uani 0.518(5) 1 d PDU A 1 H6A H 1.0881 0.2948 1.0009 0.041 Uiso 0.518(5) 1 calc PR A 1 C7 C 1.0897(9) 0.3808(11) 1.0296(6) 0.029(3) Uani 0.482(5) 1 d PDU A 2 H7 H 1.1007 0.2878 1.0309 0.035 Uiso 0.482(5) 1 calc PR A 2 C7A C 1.1301(7) 0.4468(10) 1.0555(7) 0.044(3) Uani 0.518(5) 1 d PDU A 1 H7A H 1.1652 0.4008 1.0829 0.053 Uiso 0.518(5) 1 calc PR A 1 C8 C 0.9415(3) 1.0674(6) 0.9642(4) 0.0470(17) Uani 1 1 d . . . C9 C 0.7317(2) 0.7182(4) 0.6765(3) 0.0211(10) Uani 1 1 d . B . C10 C 0.7257(3) 0.8473(5) 0.6516(3) 0.0251(11) Uani 1 1 d . . . H10 H 0.6938 0.8804 0.6168 0.030 Uiso 1 1 calc R F . C11 C 0.7780(3) 0.9173(4) 0.6899(3) 0.0247(11) Uani 1 1 d . D . C12 C 0.6910(2) 0.5999(4) 0.6536(2) 0.0194(10) Uani 1 1 d D . . C13 C 0.6298(7) 0.5978(15) 0.6126(9) 0.026(2) Uani 0.702(5) 1 d P B 1 H13 H 0.6061 0.6763 0.5960 0.031 Uiso 0.702(5) 1 calc PR B 1 C13A C 0.7080(14) 0.4582(12) 0.6665(16) 0.026(2) Uani 0.30 1 d PDU B 2 H13A H 0.7491 0.4230 0.6907 0.031 Uiso 0.298(5) 1 calc PR B 2 C14 C 0.6051(7) 0.4644(11) 0.5972(7) 0.028(3) Uani 0.702(5) 1 d P B 1 H14 H 0.5622 0.4438 0.5715 0.033 Uiso 0.702(5) 1 calc PR B 1 C14A C 0.6484(17) 0.3826(17) 0.635(2) 0.030(5) Uani 0.298(5) 1 d PDU B 2 H14A H 0.6477 0.2875 0.6348 0.036 Uiso 0.298(5) 1 calc PR B 2 C15 C 0.6518(8) 0.3709(10) 0.6246(7) 0.026(3) Uani 0.702(5) 1 d P B 1 H15 H 0.6461 0.2770 0.6188 0.032 Uiso 0.702(5) 1 calc PR B 1 C15A C 0.5950(16) 0.4535(15) 0.605(2) 0.032(5) Uani 0.298(5) 1 d PDU B 2 H15A H 0.5523 0.4153 0.5847 0.039 Uiso 0.298(5) 1 calc PR B 2 C16 C 0.7991(3) 1.0592(5) 0.6838(3) 0.0353(14) Uani 1 1 d . . . C17 C 0.8260(4) 0.4404(5) 0.9274(4) 0.0467(15) Uani 1 1 d U . . H17A H 0.8183 0.4826 0.9728 0.056 Uiso 1 1 calc R C 1 H17B H 0.8787 0.4174 0.9224 0.056 Uiso 1 1 calc R C 1 C18 C 0.7755(7) 0.3101(15) 0.9189(11) 0.038(5) Uani 0.41(3) 1 d PD D 1 H18A H 0.8015 0.2385 0.8935 0.045 Uiso 0.41(3) 1 calc PR D 1 H18B H 0.7595 0.2751 0.9641 0.045 Uiso 0.41(3) 1 calc PR D 1 C18A C 0.7629(6) 0.3614(17) 0.9508(9) 0.048(3) Uani 0.59(3) 1 d PU D 2 H18C H 0.7368 0.4054 0.9894 0.058 Uiso 0.59(3) 1 calc PR D 2 H18D H 0.7775 0.2697 0.9645 0.058 Uiso 0.59(3) 1 calc PR D 2 C19 C 0.7134(3) 0.3616(6) 0.8797(4) 0.0508(17) Uani 1 1 d DU . . H19A H 0.6678 0.3528 0.9071 0.061 Uiso 1 1 calc R D 1 H19B H 0.7074 0.3085 0.8371 0.061 Uiso 1 1 calc R D 1 C20 C 0.7255(3) 0.5045(6) 0.8618(3) 0.0351(15) Uani 1 1 d . D . H20A H 0.7125 0.5216 0.8132 0.042 Uiso 1 1 calc R . . H20B H 0.6954 0.5635 0.8915 0.042 Uiso 1 1 calc R . . C21 C 0.7587(3) 0.8114(5) 0.9614(3) 0.0317(12) Uani 1 1 d . F . H21A H 0.8074 0.8244 0.9832 0.038 Uiso 1 1 calc R . . H21B H 0.7380 0.7251 0.9774 0.038 Uiso 1 1 calc R . . C22 C 0.7080(3) 0.9249(6) 0.9798(3) 0.0397(12) Uani 1 1 d U . . H22A H 0.7350 1.0102 0.9856 0.048 Uiso 1 1 calc R E 1 H22B H 0.6795 0.9055 1.0220 0.048 Uiso 1 1 calc R E 1 C23 C 0.6573(7) 0.927(2) 0.9143(6) 0.039(2) Uani 0.71(4) 1 d PU F 1 H23A H 0.6169 0.8613 0.9184 0.047 Uiso 0.71(4) 1 calc PR F 1 H23B H 0.6360 1.0175 0.9070 0.047 Uiso 0.71(4) 1 calc PR F 1 C25 C 1.0493(9) 0.848(2) 0.7862(8) 0.038(3) Uani 0.52(3) 1 d PU F 1 H25A H 1.0427 0.9080 0.8264 0.045 Uiso 0.52(3) 1 calc PR F 1 H25B H 1.0772 0.7687 0.8015 0.045 Uiso 0.52(3) 1 calc PR F 1 C25A C 1.0326(9) 0.8998(17) 0.7960(8) 0.033(3) Uani 0.48(3) 1 d PU F 2 H25C H 1.0060 0.9637 0.8259 0.040 Uiso 0.48(3) 1 calc PR F 2 H25D H 1.0673 0.8481 0.8249 0.040 Uiso 0.48(3) 1 calc PR F 2 C26 C 1.0901(8) 0.9157(18) 0.7365(7) 0.037(2) Uani 0.52(3) 1 d PU F 1 H26A H 1.1336 0.8624 0.7228 0.044 Uiso 0.52(3) 1 calc PR F 1 H26B H 1.1069 1.0037 0.7540 0.044 Uiso 0.52(3) 1 calc PR F 1 C26A C 1.0676(12) 0.963(2) 0.7504(9) 0.048(3) Uani 0.48(3) 1 d PU F 2 H26C H 1.1202 0.9377 0.7529 0.058 Uiso 0.48(3) 1 calc PR F 2 H26D H 1.0637 1.0600 0.7596 0.058 Uiso 0.48(3) 1 calc PR F 2 C27 C 1.0383(3) 0.9332(6) 0.6770(3) 0.0426(13) Uani 1 1 d U . . H27A H 1.0641 0.9237 0.6325 0.051 Uiso 1 1 calc R F 1 H27B H 1.0133 1.0212 0.6786 0.051 Uiso 1 1 calc R F 1 C28 C 0.9849(3) 0.8195(5) 0.6889(3) 0.0284(12) Uani 1 1 d . F . H28A H 0.9364 0.8404 0.6684 0.034 Uiso 1 1 calc R . . H28B H 1.0037 0.7355 0.6683 0.034 Uiso 1 1 calc R . . C29 C 1.0200(3) 0.5047(5) 0.7861(3) 0.0292(14) Uani 1 1 d . F . H29A H 1.0413 0.5479 0.8274 0.035 Uiso 1 1 calc R . . H29B H 1.0414 0.5469 0.7447 0.035 Uiso 1 1 calc R . . C30 C 1.0350(3) 0.3555(5) 0.7866(3) 0.0370(13) Uani 1 1 d . . . H30A H 1.0831 0.3346 0.7652 0.044 Uiso 1 1 calc R F . H30B H 1.0341 0.3191 0.8339 0.044 Uiso 1 1 calc R . . C31 C 0.9723(3) 0.3019(6) 0.7444(3) 0.0468(17) Uani 1 1 d . F . H31A H 0.9850 0.3016 0.6949 0.056 Uiso 1 1 calc R . . H31B H 0.9596 0.2095 0.7586 0.056 Uiso 1 1 calc R . . C32 C 0.9104(3) 0.3954(7) 0.7584(4) 0.0548(19) Uani 1 1 d . F . H32A H 0.8832 0.4147 0.7154 0.066 Uiso 1 1 calc R . . H32B H 0.8758 0.3551 0.7918 0.066 Uiso 1 1 calc R . . C24A C 0.7223(16) 0.926(2) 0.8613(14) 0.039(4) Uani 0.29(4) 1 d PDU F 2 H24A H 0.6926 0.8980 0.8212 0.047 Uiso 0.29(4) 1 calc PR F 2 H24B H 0.7556 0.9994 0.8467 0.047 Uiso 0.29(4) 1 calc PR F 2 C23A C 0.6733(19) 0.973(4) 0.9180(15) 0.041(3) Uani 0.29(4) 1 d PDU F 2 H23C H 0.6698 1.0718 0.9183 0.049 Uiso 0.29(4) 1 calc PR F 2 H23D H 0.6233 0.9348 0.9130 0.049 Uiso 0.29(4) 1 calc PR F 2 C24 C 0.7075(7) 0.8916(18) 0.8587(7) 0.041(3) Uani 0.71(4) 1 d PU F 1 H24C H 0.6811 0.8402 0.8229 0.050 Uiso 0.71(4) 1 calc PR F 1 H24D H 0.7281 0.9735 0.8374 0.050 Uiso 0.71(4) 1 calc PR F 1 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 Ca1 0.0144(4) 0.0287(4) 0.0213(4) 0.0017(5) -0.0024(4) -0.0009(4) S1 0.0270(19) 0.0288(16) 0.0247(19) -0.0002(13) 0.0079(14) 0.0070(13) S1A 0.051(3) 0.054(2) 0.045(2) -0.0076(17) -0.0293(19) 0.0121(19) S2 0.0173(13) 0.0265(9) 0.0354(13) 0.0002(9) -0.0032(10) -0.0010(7) S2A 0.013(3) 0.046(4) 0.030(3) 0.002(3) -0.008(3) -0.001(2) F1 0.093(4) 0.039(2) 0.129(5) -0.019(2) -0.017(3) -0.014(2) F2 0.068(3) 0.051(2) 0.106(4) -0.011(2) 0.015(3) 0.022(2) F3 0.336(10) 0.054(3) 0.058(3) 0.027(3) 0.045(5) 0.091(4) F4 0.072(3) 0.0371(19) 0.106(4) 0.024(2) -0.032(3) -0.0011(19) F5 0.041(2) 0.0378(19) 0.117(4) 0.016(2) 0.023(2) -0.0087(15) F6 0.155(5) 0.042(2) 0.060(3) -0.016(2) 0.035(3) -0.034(3) O1 0.0159(19) 0.0381(18) 0.030(2) 0.0027(17) 0.0001(16) 0.0005(15) O2 0.026(2) 0.045(2) 0.021(2) 0.0016(16) -0.0030(16) 0.0092(15) O3 0.021(2) 0.052(2) 0.026(2) 0.0088(18) -0.0060(16) -0.0123(16) O4 0.017(2) 0.0401(19) 0.036(2) -0.0119(17) -0.0001(16) 0.0029(15) N1 0.016(2) 0.026(2) 0.027(2) -0.0031(18) 0.0002(18) -0.0062(16) N2 0.024(2) 0.027(2) 0.028(3) 0.0029(19) 0.000(2) 0.0002(17) N3 0.021(2) 0.0236(19) 0.019(2) -0.0018(16) -0.0020(18) -0.0037(16) N4 0.013(2) 0.027(2) 0.025(2) 0.0009(17) -0.0007(18) -0.0002(15) C1 0.013(2) 0.030(2) 0.014(2) 0.000(2) 0.0052(19) -0.0083(17) C2 0.023(3) 0.031(2) 0.025(3) -0.008(2) -0.002(2) -0.012(2) C3 0.021(3) 0.032(2) 0.029(3) -0.004(2) 0.001(2) -0.007(2) C4 0.018(3) 0.042(3) 0.017(3) 0.003(2) 0.004(2) -0.007(2) C5 0.009(4) 0.037(3) 0.033(4) 0.010(3) -0.002(3) 0.006(3) C5A 0.009(4) 0.037(3) 0.033(4) 0.010(3) -0.002(3) 0.006(3) C6 0.010(5) 0.041(5) 0.032(6) 0.009(5) -0.005(4) 0.000(4) C6A 0.031(6) 0.044(5) 0.028(6) -0.010(5) 0.002(5) 0.009(5) C7 0.017(5) 0.034(5) 0.036(7) 0.014(5) 0.006(5) 0.007(4) C7A 0.042(6) 0.051(6) 0.040(6) -0.012(5) -0.008(5) 0.023(5) C8 0.030(3) 0.035(3) 0.076(5) -0.003(3) 0.001(3) -0.004(3) C9 0.011(2) 0.032(2) 0.020(3) 0.000(2) 0.003(2) 0.0014(18) C10 0.020(3) 0.030(2) 0.025(3) 0.001(2) -0.002(2) 0.003(2) C11 0.019(3) 0.025(2) 0.030(3) -0.001(2) 0.005(2) 0.0041(19) C12 0.012(2) 0.024(2) 0.022(3) 0.008(2) 0.005(2) -0.0011(17) C13 0.009(4) 0.037(3) 0.033(4) 0.010(3) -0.002(3) 0.006(3) C13A 0.009(4) 0.037(3) 0.033(4) 0.010(3) -0.002(3) 0.006(3) C14 0.013(5) 0.052(5) 0.018(5) -0.003(4) 0.003(4) -0.012(4) C14A 0.020(8) 0.036(8) 0.033(8) 0.005(7) 0.006(7) 0.004(7) C15 0.034(6) 0.027(4) 0.018(6) -0.002(4) 0.006(4) -0.014(4) C15A 0.019(8) 0.044(8) 0.034(8) 0.004(7) 0.000(8) 0.002(7) C16 0.028(3) 0.031(3) 0.046(4) 0.001(3) 0.001(3) 0.003(2) C17 0.043(3) 0.042(3) 0.055(4) 0.021(3) -0.008(3) 0.000(3) C18 0.048(10) 0.013(7) 0.052(12) 0.008(7) 0.011(8) 0.003(6) C18A 0.029(5) 0.042(5) 0.074(6) 0.019(5) -0.007(5) 0.002(4) C19 0.031(3) 0.039(3) 0.081(5) -0.003(3) 0.010(3) -0.005(2) C20 0.024(3) 0.051(4) 0.030(4) 0.009(2) -0.001(3) -0.012(2) C21 0.023(3) 0.045(3) 0.028(3) 0.007(2) 0.004(2) 0.001(2) C22 0.036(3) 0.047(3) 0.036(3) -0.008(3) 0.004(2) 0.001(2) C23 0.026(4) 0.053(4) 0.038(3) -0.002(4) 0.001(3) 0.016(3) C25 0.028(6) 0.058(6) 0.028(5) -0.001(5) -0.012(4) -0.021(5) C25A 0.022(6) 0.037(7) 0.041(7) -0.022(6) 0.012(5) -0.008(5) C26 0.030(4) 0.054(5) 0.027(4) -0.006(4) 0.001(3) -0.013(4) C26A 0.047(7) 0.055(7) 0.044(7) 0.002(6) -0.003(6) -0.014(6) C27 0.041(3) 0.054(3) 0.032(3) 0.000(3) 0.011(2) -0.006(2) C28 0.024(3) 0.038(3) 0.023(3) 0.001(2) 0.004(2) 0.007(2) C29 0.005(3) 0.045(3) 0.038(4) 0.003(2) -0.002(2) 0.0033(19) C30 0.037(3) 0.040(3) 0.034(3) 0.000(3) 0.001(3) 0.009(2) C31 0.033(3) 0.056(4) 0.051(4) -0.025(3) -0.004(3) -0.004(3) C32 0.032(4) 0.064(4) 0.069(5) -0.042(4) -0.003(3) 0.005(3) C24A 0.038(7) 0.046(7) 0.034(7) -0.001(6) 0.005(6) 0.001(6) C23A 0.039(5) 0.046(5) 0.037(5) -0.006(5) 0.001(5) 0.002(5) C24 0.025(5) 0.061(5) 0.037(4) -0.002(4) -0.001(4) 0.020(4) _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 Ca1 N2 2.410(4) . ? Ca1 N4 2.422(4) . ? Ca1 O1 2.428(4) . ? Ca1 O4 2.444(4) . ? Ca1 O3 2.480(4) . ? Ca1 O2 2.494(4) . ? Ca1 N1 2.497(4) . ? Ca1 N3 2.513(4) . ? S1 C4 1.685(5) . ? S1 C7 1.690(8) . ? S1A C4 1.673(5) . ? S1A C7A 1.690(8) . ? S2 C15 1.683(11) . ? S2 C12 1.698(5) . ? S2A C15A 1.680(10) . ? S2A C12 1.697(6) . ? F1 C8 1.317(7) . ? F2 C8 1.352(7) . ? F3 C8 1.269(8) . ? F4 C16 1.352(7) . ? F5 C16 1.328(6) . ? F6 C16 1.302(7) . ? O1 C17 1.431(6) . ? O1 C20 1.439(6) . ? O2 C24 1.439(10) . ? O2 C21 1.441(6) . ? O2 C24A 1.479(10) . ? O3 C25 1.414(13) . ? O3 C28 1.443(6) . ? O3 C25A 1.489(15) . ? O4 C29 1.438(6) . ? O4 C32 1.440(7) . ? N1 N2 1.352(5) . ? N1 C1 1.354(6) . ? N2 C3 1.350(7) . ? N3 C9 1.354(6) . ? N3 N4 1.370(5) . ? N4 C11 1.332(6) . ? C1 C2 1.389(7) . ? C1 C4 1.431(6) . ? C2 C3 1.363(8) . ? C3 C8 1.467(8) . ? C4 C5A 1.458(9) . ? C4 C5 1.470(9) . ? C5 C6 1.466(9) . ? C5A C6A 1.464(9) . ? C6 C7 1.331(9) . ? C6A C7A 1.333(9) . ? C9 C10 1.382(7) . ? C9 C12 1.462(6) . ? C10 C11 1.395(7) . ? C11 C16 1.473(7) . ? C12 C13 1.371(14) . ? C12 C13A 1.470(10) . ? C13 C14 1.436(17) . ? C13A C14A 1.460(10) . ? C14 C15 1.370(12) . ? C14A C15A 1.333(10) . ? C17 C18A 1.464(12) . ? C17 C18 1.601(15) . ? C18 C19 1.456(9) . ? C18A C19 1.652(16) . ? C19 C20 1.484(8) . ? C21 C22 1.503(7) . ? C22 C23A 1.44(3) . ? C22 C23 1.572(14) . ? C23 C24 1.460(12) . ? C25 C26 1.391(17) . ? C25A C26A 1.26(2) . ? C26 C27 1.503(14) . ? C26A C27 1.553(18) . ? C27 C28 1.511(7) . ? C29 C30 1.514(7) . ? C30 C31 1.504(8) . ? C31 C32 1.488(8) . ? C24A C23A 1.492(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ca1 N4 116.90(12) . . ? N2 Ca1 O1 111.21(14) . . ? N4 Ca1 O1 116.13(13) . . ? N2 Ca1 O4 115.27(13) . . ? N4 Ca1 O4 113.92(14) . . ? O1 Ca1 O4 77.23(11) . . ? N2 Ca1 O3 78.61(14) . . ? N4 Ca1 O3 78.04(13) . . ? O1 Ca1 O3 152.53(13) . . ? O4 Ca1 O3 75.44(13) . . ? N2 Ca1 O2 77.33(13) . . ? N4 Ca1 O2 79.21(12) . . ? O1 Ca1 O2 72.97(12) . . ? O4 Ca1 O2 150.17(13) . . ? O3 Ca1 O2 134.38(11) . . ? N2 Ca1 N1 31.91(13) . . ? N4 Ca1 N1 147.11(13) . . ? O1 Ca1 N1 92.74(13) . . ? O4 Ca1 N1 86.41(13) . . ? O3 Ca1 N1 82.96(13) . . ? O2 Ca1 N1 95.90(13) . . ? N2 Ca1 N3 147.19(13) . . ? N4 Ca1 N3 32.15(12) . . ? O1 Ca1 N3 87.67(12) . . ? O4 Ca1 N3 94.49(13) . . ? O3 Ca1 N3 97.06(12) . . ? O2 Ca1 N3 83.43(12) . . ? N1 Ca1 N3 179.08(12) . . ? C4 S1 C7 94.8(5) . . ? C4 S1A C7A 94.5(5) . . ? C15 S2 C12 93.4(4) . . ? C15A S2A C12 93.8(8) . . ? C17 O1 C20 107.7(4) . . ? C17 O1 Ca1 126.3(3) . . ? C20 O1 Ca1 124.9(3) . . ? C24 O2 C21 109.1(6) . . ? C24 O2 C24A 17.3(13) . . ? C21 O2 C24A 107.5(12) . . ? C24 O2 Ca1 126.8(5) . . ? C21 O2 Ca1 123.6(3) . . ? C24A O2 Ca1 123.4(11) . . ? C25 O3 C28 103.5(7) . . ? C25 O3 C25A 24.7(7) . . ? C28 O3 C25A 109.5(7) . . ? C25 O3 Ca1 131.0(6) . . ? C28 O3 Ca1 125.2(3) . . ? C25A O3 Ca1 122.1(6) . . ? C29 O4 C32 108.5(4) . . ? C29 O4 Ca1 125.3(3) . . ? C32 O4 Ca1 126.2(3) . . ? N2 N1 C1 108.2(4) . . ? N2 N1 Ca1 70.5(3) . . ? C1 N1 Ca1 177.2(3) . . ? C3 N2 N1 107.6(4) . . ? C3 N2 Ca1 174.4(4) . . ? N1 N2 Ca1 77.6(3) . . ? C9 N3 N4 107.4(4) . . ? C9 N3 Ca1 173.2(3) . . ? N4 N3 Ca1 70.3(2) . . ? C11 N4 N3 107.5(4) . . ? C11 N4 Ca1 171.8(3) . . ? N3 N4 Ca1 77.6(2) . . ? N1 C1 C2 109.0(4) . . ? N1 C1 C4 121.7(4) . . ? C2 C1 C4 129.3(4) . . ? C3 C2 C1 104.9(4) . . ? N2 C3 C2 110.4(4) . . ? N2 C3 C8 121.3(5) . . ? C2 C3 C8 128.3(5) . . ? C1 C4 C5A 123.2(6) . . ? C1 C4 C5 123.4(6) . . ? C5A C4 C5 112.1(8) . . ? C1 C4 S1A 124.5(4) . . ? C5A C4 S1A 112.1(6) . . ? C5 C4 S1A 16.7(5) . . ? C1 C4 S1 125.0(4) . . ? C5A C4 S1 4.2(9) . . ? C5 C4 S1 111.0(5) . . ? S1A C4 S1 109.8(3) . . ? C6 C5 C4 106.7(8) . . ? C4 C5A C6A 106.1(9) . . ? C7 C6 C5 116.1(9) . . ? C7A C6A C5A 116.3(10) . . ? C6 C7 S1 111.4(7) . . ? C6A C7A S1A 111.0(8) . . ? F3 C8 F1 109.9(6) . . ? F3 C8 F2 107.4(6) . . ? F1 C8 F2 99.3(6) . . ? F3 C8 C3 114.4(6) . . ? F1 C8 C3 112.2(5) . . ? F2 C8 C3 112.6(5) . . ? N3 C9 C10 110.8(4) . . ? N3 C9 C12 121.8(4) . . ? C10 C9 C12 127.4(4) . . ? C9 C10 C11 103.0(4) . . ? N4 C11 C10 111.3(4) . . ? N4 C11 C16 120.5(5) . . ? C10 C11 C16 128.0(5) . . ? C13 C12 C9 126.9(7) . . ? C13 C12 C13A 104.8(12) . . ? C9 C12 C13A 128.3(9) . . ? C13 C12 S2A 8.0(9) . . ? C9 C12 S2A 119.8(4) . . ? C13A C12 S2A 111.9(9) . . ? C13 C12 S2 110.5(7) . . ? C9 C12 S2 122.4(3) . . ? C13A C12 S2 6.4(10) . . ? S2A C12 S2 117.8(4) . . ? C12 C13 C14 112.9(10) . . ? C14A C13A C12 105.6(11) . . ? C15 C14 C13 110.9(9) . . ? C15A C14A C13A 116.8(13) . . ? C14 C15 S2 112.2(7) . . ? C14A C15A S2A 111.7(11) . . ? F6 C16 F5 106.5(5) . . ? F6 C16 F4 107.0(5) . . ? F5 C16 F4 102.6(5) . . ? F6 C16 C11 114.4(5) . . ? F5 C16 C11 114.1(5) . . ? F4 C16 C11 111.4(5) . . ? O1 C17 C18A 109.0(6) . . ? O1 C17 C18 104.4(6) . . ? C18A C17 C18 31.3(7) . . ? C19 C18 C17 102.2(8) . . ? C17 C18A C19 99.5(8) . . ? C18 C19 C20 110.3(7) . . ? C18 C19 C18A 30.4(6) . . ? C20 C19 C18A 96.7(7) . . ? O1 C20 C19 105.3(5) . . ? O2 C21 C22 106.8(4) . . ? C23A C22 C21 108.7(12) . . ? C23A C22 C23 20.2(13) . . ? C21 C22 C23 100.3(6) . . ? C24 C23 C22 103.3(7) . . ? C26 C25 O3 113.3(10) . . ? C26A C25A O3 109.4(12) . . ? C25 C26 C27 104.9(9) . . ? C25A C26A C27 112.3(12) . . ? C26 C27 C28 101.4(7) . . ? C26 C27 C26A 25.6(7) . . ? C28 C27 C26A 102.8(7) . . ? O3 C28 C27 105.2(4) . . ? O4 C29 C30 105.3(4) . . ? C31 C30 C29 102.1(5) . . ? C32 C31 C30 104.5(5) . . ? O4 C32 C31 107.6(5) . . ? O2 C24A C23A 107.6(17) . . ? C22 C23A C24A 104.6(18) . . ? O2 C24 C23 107.7(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.639 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.076 #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 794840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Sr(ttfpz)2(thf)4] ; _chemical_name_common (Sr(ttfpz)2(thf)4) _chemical_melting_point ? _chemical_formula_moiety ; C32 H40 F6 N4 O4 S2 Sr ; _chemical_formula_sum 'C32 H40 F6 N4 O4 S2 Sr' _chemical_formula_weight 810.42 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.4622(3) _cell_length_b 10.0965(2) _cell_length_c 19.3001(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3597.61(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 38893 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.687 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6315 _exptl_absorpt_correction_T_max 0.7859 _exptl_absorpt_process_details SADABS _exptl_special_details ; Thiophene groups were disordered over two positions, their occupancies were freely refined against each other (59:41 for S(1) and 76:24 for S(2)). Both disordered groups were restrained using the SIMU command. SIMU was also applied on thf molecules O(1) and O(3). Carbon atoms C(25) and C(26) of thf molecule O(3) are disordered over two positions, their occupancy was freely refined against each other (64:36). The distance between C(23) and C(24) was restrained using the DFIX command. The distance between C(14A) and C(15A) was restrained using the SADI command using atoms C(6) and C(7) as reference. ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38893 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8209 _reflns_number_gt 7086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_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 -0.008(4) _refine_ls_number_reflns 8209 _refine_ls_number_parameters 535 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.036 _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 Sr1 Sr 0.128191(10) 0.292624(17) 0.17511(2) 0.02103(5) Uani 1 1 d . C . N3 N 0.21952(10) 0.2847(2) 0.28023(11) 0.0219(4) Uani 1 1 d . . . N1 N 0.03715(10) 0.2838(2) 0.07032(11) 0.0235(4) Uani 1 1 d . . . C9 C 0.27354(12) 0.2776(2) 0.32720(12) 0.0206(5) Uani 1 1 d . A . N4 N 0.19035(10) 0.1610(2) 0.27264(11) 0.0224(5) Uani 1 1 d . . . C1 C -0.01300(12) 0.2773(2) 0.01911(12) 0.0218(5) Uani 1 1 d . B . C2 C -0.01780(14) 0.1478(3) -0.00555(14) 0.0284(6) Uani 1 1 d . . . H2 H -0.0482 0.1145 -0.0412 0.034 Uiso 1 1 calc R . . N2 N 0.06484(11) 0.1598(2) 0.07938(12) 0.0275(5) Uani 1 1 d . . . C10 C 0.28025(13) 0.1482(3) 0.35131(13) 0.0240(5) Uani 1 1 d . . . H10 H 0.3134 0.1146 0.3846 0.029 Uiso 1 1 calc R . . C11 C 0.22747(13) 0.0808(2) 0.31556(13) 0.0244(5) Uani 1 1 d . . . C3 C 0.03208(14) 0.0793(3) 0.03400(14) 0.0261(6) Uani 1 1 d . . . C4 C -0.05076(13) 0.3945(3) -0.00403(13) 0.0252(5) Uani 1 1 d U . . C16 C 0.20747(15) -0.0608(3) 0.32071(16) 0.0340(6) Uani 1 1 d . . . S2 S 0.28387(11) 0.55131(17) 0.32949(13) 0.0277(4) Uani 0.766(4) 1 d P A 3 C5 C -0.0467(10) 0.5256(18) 0.0197(10) 0.035(3) Uani 0.420(4) 1 d PU B 1 H5 H -0.0151 0.5495 0.0565 0.042 Uiso 0.420(4) 1 calc PR B 1 F5 F 0.14040(10) -0.0810(2) 0.34520(12) 0.0557(6) Uani 1 1 d . . . O2 O 0.23732(9) 0.1890(2) 0.11011(10) 0.0342(5) Uani 1 1 d . . . S1 S -0.1183(2) 0.3924(6) -0.0622(3) 0.0456(10) Uani 0.420(4) 1 d PU B 1 F4 F 0.25022(12) -0.12578(19) 0.36485(13) 0.0656(6) Uani 1 1 d . . . C21 C 0.24244(15) 0.1816(3) 0.03524(14) 0.0323(6) Uani 1 1 d . . . H21A H 0.2614 0.2656 0.0161 0.039 Uiso 1 1 calc R . . H21B H 0.1943 0.1640 0.0146 0.039 Uiso 1 1 calc R . . C13 C 0.3774(5) 0.4067(10) 0.3882(6) 0.036(2) Uani 0.766(4) 1 d PU A 3 H13 H 0.4028 0.3316 0.4052 0.043 Uiso 0.766(4) 1 calc PR A 3 F6 F 0.21019(13) -0.1258(2) 0.26168(12) 0.0707(7) Uani 1 1 d . . . C22 C 0.29399(15) 0.0684(3) 0.02006(15) 0.0384(7) Uani 1 1 d . . . H22A H 0.2671 -0.0145 0.0105 0.046 Uiso 1 1 calc R . . H22B H 0.3253 0.0891 -0.0201 0.046 Uiso 1 1 calc R . . C24 C 0.29288(19) 0.1088(5) 0.14048(17) 0.0762(14) Uani 1 1 d D . . H24A H 0.2709 0.0351 0.1671 0.091 Uiso 1 1 calc R . . H24B H 0.3227 0.1625 0.1725 0.091 Uiso 1 1 calc R . . C8 C 0.05305(16) -0.0612(3) 0.03011(17) 0.0405(7) Uani 1 1 d . . . F1 F 0.00821(11) -0.13069(19) -0.01102(12) 0.0651(6) Uani 1 1 d . . . C23 C 0.3375(2) 0.0567(4) 0.08495(17) 0.0710(12) Uani 1 1 d D . . H23A H 0.3501 -0.0370 0.0940 0.085 Uiso 1 1 calc R . . H23B H 0.3829 0.1083 0.0809 0.085 Uiso 1 1 calc R . . O1 O 0.20199(9) 0.4834(2) 0.12216(11) 0.0330(5) Uani 1 1 d . . . O3 O 0.01690(10) 0.1988(2) 0.24084(10) 0.0373(5) Uani 1 1 d . . . C15 C 0.3561(4) 0.6233(11) 0.3721(6) 0.0273(16) Uani 0.766(4) 1 d P A 3 H15 H 0.3641 0.7161 0.3754 0.033 Uiso 0.766(4) 1 calc PR A 3 C20 C 0.27841(13) 0.5047(3) 0.13289(17) 0.0360(8) Uani 1 1 d . . . H20A H 0.3074 0.4509 0.1002 0.043 Uiso 1 1 calc R . . H20B H 0.2924 0.4812 0.1808 0.043 Uiso 1 1 calc R . . C6 C -0.0881(13) 0.615(2) -0.0109(8) 0.032(3) Uani 0.420(4) 1 d PDU B 1 H6 H -0.0867 0.7070 -0.0012 0.038 Uiso 0.420(4) 1 calc PR B 1 C28 C 0.01356(14) 0.1730(3) 0.31394(14) 0.0319(6) Uani 1 1 d . C . H28A H -0.0032 0.2525 0.3393 0.038 Uiso 1 1 calc R . . H28B H 0.0618 0.1471 0.3319 0.038 Uiso 1 1 calc R . . C25 C -0.0371(6) 0.1081(13) 0.2035(5) 0.034(2) Uani 0.362(14) 1 d PU C 5 H25A H -0.0599 0.1529 0.1635 0.041 Uiso 0.362(14) 1 calc PR C 5 H25B H -0.0141 0.0247 0.1880 0.041 Uiso 0.362(14) 1 calc PR C 5 F2 F 0.11839(10) -0.0803(2) 0.00100(13) 0.0607(6) Uani 1 1 d . . . C14 C 0.4003(7) 0.5294(10) 0.4005(6) 0.029(2) Uani 0.766(4) 1 d PU A 3 H14 H 0.4427 0.5494 0.4263 0.035 Uiso 0.766(4) 1 calc PR A 3 C19 C 0.28967(16) 0.6484(3) 0.1200(2) 0.0525(9) Uani 1 1 d U . . H19A H 0.3390 0.6657 0.1021 0.063 Uiso 1 1 calc R . . H19B H 0.2823 0.7005 0.1629 0.063 Uiso 1 1 calc R . . C27 C -0.04051(16) 0.0595(3) 0.32217(15) 0.0396(7) Uani 1 1 d U . . H27A H -0.0164 -0.0279 0.3190 0.048 Uiso 1 1 calc R C 5 H27B H -0.0673 0.0657 0.3665 0.048 Uiso 1 1 calc R C 5 C26 C -0.0898(8) 0.0847(14) 0.2603(8) 0.039(3) Uani 0.362(14) 1 d PU C 5 H26A H -0.1208 0.0069 0.2504 0.047 Uiso 0.362(14) 1 calc PR C 5 H26B H -0.1209 0.1632 0.2679 0.047 Uiso 0.362(14) 1 calc PR C 5 C17 C 0.18206(17) 0.5658(3) 0.06520(18) 0.0509(8) Uani 1 1 d U . . H17A H 0.1313 0.5961 0.0701 0.061 Uiso 1 1 calc R . . H17B H 0.1867 0.5168 0.0210 0.061 Uiso 1 1 calc R . . O4 O 0.05950(9) 0.50100(19) 0.21476(11) 0.0348(5) Uani 1 1 d . . . C30 C -0.03319(15) 0.6597(3) 0.21565(15) 0.0370(7) Uani 1 1 d . . . H30A H -0.0336 0.6934 0.1675 0.044 Uiso 1 1 calc R C . H30B H -0.0799 0.6815 0.2382 0.044 Uiso 1 1 calc R . . C29 C -0.01843(14) 0.5123(3) 0.21770(17) 0.0327(7) Uani 1 1 d . C . H29A H -0.0375 0.4728 0.2610 0.039 Uiso 1 1 calc R . . H29B H -0.0411 0.4673 0.1776 0.039 Uiso 1 1 calc R . . C32 C 0.09166(16) 0.6244(3) 0.23730(19) 0.0520(9) Uani 1 1 d . C . H32A H 0.1211 0.6636 0.1997 0.062 Uiso 1 1 calc R . . H32B H 0.1233 0.6094 0.2780 0.062 Uiso 1 1 calc R . . C7 C -0.1340(7) 0.5565(17) -0.0589(7) 0.037(3) Uani 0.420(4) 1 d PDU B 1 H7 H -0.1690 0.6023 -0.0859 0.044 Uiso 0.420(4) 1 calc PR B 1 C31 C 0.02998(17) 0.7150(3) 0.25602(18) 0.0460(8) Uani 1 1 d . C . H31A H 0.0405 0.8074 0.2420 0.055 Uiso 1 1 calc R . . H31B H 0.0203 0.7127 0.3065 0.055 Uiso 1 1 calc R . . S1A S -0.03750(16) 0.5446(3) 0.03198(15) 0.0237(5) Uani 0.580(4) 1 d P B 2 C5A C -0.0935(5) 0.4025(15) -0.0643(8) 0.040(3) Uani 0.580(4) 1 d PU B 2 H5A H -0.1049 0.3299 -0.0936 0.048 Uiso 0.580(4) 1 calc PR B 2 C7A C -0.0934(9) 0.6204(15) -0.0286(6) 0.031(3) Uani 0.580(4) 1 d PU B 2 H7A H -0.1051 0.7120 -0.0280 0.037 Uiso 0.580(4) 1 calc PR B 2 C12 C 0.31391(12) 0.3940(2) 0.34889(12) 0.0212(5) Uani 1 1 d U . . C13A C 0.2967(15) 0.521(3) 0.3348(18) 0.033(5) Uani 0.234(4) 1 d PU A 4 H13A H 0.2577 0.5437 0.3050 0.039 Uiso 0.234(4) 1 calc PR A 4 S2A S 0.3880(4) 0.3775(8) 0.3947(5) 0.0286(16) Uani 0.234(4) 1 d P A 4 C14A C 0.3400(14) 0.615(3) 0.367(2) 0.028(5) Uani 0.234(4) 1 d PDU A 4 H14A H 0.3305 0.7079 0.3668 0.033 Uiso 0.234(4) 1 calc PR A 4 C15A C 0.399(2) 0.556(4) 0.399(2) 0.029(6) Uani 0.234(4) 1 d PDU A 4 H15A H 0.4384 0.6017 0.4199 0.035 Uiso 0.234(4) 1 calc PR A 4 C6A C -0.1175(5) 0.5377(11) -0.0750(5) 0.038(2) Uani 0.580(4) 1 d PU B 2 H6A H -0.1479 0.5635 -0.1123 0.046 Uiso 0.580(4) 1 calc PR B 2 C25A C -0.0542(3) 0.1734(7) 0.2165(3) 0.0276(16) Uani 0.638(14) 1 d P C 6 H25C H -0.0553 0.1684 0.1653 0.033 Uiso 0.638(14) 1 calc PR C 6 H25D H -0.0883 0.2431 0.2320 0.033 Uiso 0.638(14) 1 calc PR C 6 C26A C -0.0732(4) 0.0405(8) 0.2487(4) 0.0386(17) Uani 0.638(14) 1 d P C 6 H26C H -0.0499 -0.0338 0.2237 0.046 Uiso 0.638(14) 1 calc PR C 6 H26D H -0.1262 0.0262 0.2504 0.046 Uiso 0.638(14) 1 calc PR C 6 C18 C 0.2331(2) 0.6816(4) 0.0666(3) 0.0927(18) Uani 1 1 d U . . H18A H 0.2070 0.7637 0.0796 0.111 Uiso 1 1 calc R . . H18B H 0.2557 0.6946 0.0206 0.111 Uiso 1 1 calc R . . F3 F 0.05528(16) -0.1214(2) 0.09073(12) 0.0847(8) 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 Sr1 0.01737(9) 0.02392(9) 0.02179(9) 0.00066(13) -0.00326(10) -0.00020(9) N3 0.0184(9) 0.0235(11) 0.0239(10) 0.0008(9) -0.0010(8) 0.0006(8) N1 0.0224(10) 0.0253(12) 0.0228(10) 0.0006(9) -0.0028(8) -0.0004(8) C9 0.0174(11) 0.0269(13) 0.0176(11) -0.0006(10) 0.0026(9) 0.0039(9) N4 0.0199(10) 0.0211(11) 0.0261(11) -0.0002(9) -0.0016(8) -0.0009(8) C1 0.0166(11) 0.0311(14) 0.0178(11) 0.0013(10) 0.0021(9) -0.0061(10) C2 0.0252(13) 0.0303(15) 0.0296(14) -0.0012(12) -0.0044(11) -0.0085(11) N2 0.0256(11) 0.0270(12) 0.0299(12) -0.0008(10) -0.0029(9) -0.0014(9) C10 0.0217(12) 0.0259(13) 0.0245(13) 0.0010(10) 0.0003(10) 0.0040(10) C11 0.0226(12) 0.0237(13) 0.0268(13) 0.0008(11) 0.0040(10) 0.0037(10) C3 0.0265(13) 0.0260(14) 0.0258(13) 0.0008(11) -0.0017(10) -0.0054(10) C4 0.0187(12) 0.0337(15) 0.0232(12) 0.0012(11) -0.0016(9) -0.0038(10) C16 0.0340(15) 0.0271(15) 0.0408(16) -0.0034(13) 0.0006(12) 0.0014(11) S2 0.0214(8) 0.0219(7) 0.0398(8) 0.0026(6) -0.0058(6) -0.0001(5) C5 0.024(5) 0.057(6) 0.026(6) 0.000(5) -0.011(4) -0.011(4) F5 0.0455(11) 0.0320(11) 0.0895(17) 0.0108(10) 0.0147(10) -0.0090(8) O2 0.0277(9) 0.0468(13) 0.0279(10) -0.0067(9) -0.0031(8) 0.0130(8) S1 0.048(2) 0.0479(18) 0.0413(15) -0.0049(13) -0.0242(18) 0.0086(19) F4 0.0710(12) 0.0300(10) 0.0958(17) 0.0167(11) -0.0315(12) 0.0041(9) C21 0.0305(14) 0.0399(17) 0.0264(13) 0.0014(12) 0.0031(11) 0.0009(12) C13 0.040(4) 0.031(4) 0.037(4) 0.007(3) -0.001(2) 0.015(2) F6 0.1187(18) 0.0368(12) 0.0566(13) -0.0164(10) 0.0230(12) -0.0218(12) C22 0.0383(16) 0.0438(18) 0.0331(16) -0.0063(14) 0.0072(13) 0.0028(13) C24 0.058(2) 0.129(4) 0.0415(19) -0.016(2) -0.0130(16) 0.063(2) C8 0.0415(17) 0.0309(17) 0.0489(18) -0.0002(14) -0.0063(14) -0.0069(13) F1 0.0702(13) 0.0361(11) 0.0890(17) -0.0165(11) -0.0167(12) -0.0111(10) C23 0.076(2) 0.093(3) 0.044(2) -0.006(2) -0.0061(18) 0.055(2) O1 0.0237(9) 0.0395(11) 0.0357(11) 0.0097(9) -0.0019(8) -0.0039(8) O3 0.0242(9) 0.0557(13) 0.0320(10) 0.0123(10) -0.0053(8) -0.0120(9) C15 0.015(3) 0.032(3) 0.034(3) 0.000(2) 0.001(3) -0.012(2) C20 0.0194(13) 0.054(2) 0.0350(17) 0.0057(13) -0.0007(12) -0.0060(12) C6 0.027(5) 0.039(6) 0.030(6) -0.007(5) -0.004(5) -0.004(4) C28 0.0240(13) 0.0421(16) 0.0295(14) -0.0048(12) 0.0003(11) 0.0027(11) C25 0.035(5) 0.027(5) 0.040(4) -0.017(4) 0.003(3) -0.010(4) F2 0.0514(12) 0.0430(12) 0.0876(17) -0.0108(11) 0.0043(10) 0.0100(9) C14 0.032(3) 0.028(5) 0.027(3) -0.001(3) -0.012(2) -0.003(3) C19 0.0343(16) 0.0412(19) 0.082(3) -0.0093(17) 0.0113(16) -0.0056(14) C27 0.0517(18) 0.0389(17) 0.0282(14) 0.0042(13) 0.0067(13) -0.0061(13) C26 0.043(5) 0.034(6) 0.039(5) -0.011(4) 0.003(4) -0.020(4) C17 0.0509(18) 0.0482(19) 0.0535(19) 0.0198(16) -0.0146(15) -0.0064(15) O4 0.0261(9) 0.0370(12) 0.0414(12) -0.0091(8) -0.0007(8) 0.0047(8) C30 0.0337(15) 0.0393(16) 0.0381(16) 0.0009(13) -0.0001(12) 0.0100(12) C29 0.0277(14) 0.0333(16) 0.0371(18) 0.0035(12) 0.0061(12) 0.0035(11) C32 0.0400(17) 0.052(2) 0.064(2) -0.0280(17) -0.0047(15) 0.0017(14) C7 0.029(5) 0.044(5) 0.038(5) -0.001(4) -0.003(4) 0.014(4) C31 0.0489(18) 0.0396(18) 0.0495(19) -0.0126(15) 0.0023(14) 0.0060(14) S1A 0.0211(10) 0.0279(9) 0.0222(10) -0.0027(6) -0.0009(8) 0.0006(6) C5A 0.031(5) 0.033(3) 0.056(4) 0.007(3) -0.006(4) -0.002(4) C7A 0.023(4) 0.028(4) 0.042(6) 0.013(4) 0.004(4) 0.013(3) C12 0.0186(11) 0.0263(13) 0.0186(11) -0.0005(10) 0.0016(9) 0.0006(10) C13A 0.024(10) 0.042(11) 0.033(8) 0.009(8) -0.009(7) 0.004(7) S2A 0.027(2) 0.026(3) 0.033(2) 0.004(2) -0.0078(18) -0.008(2) C14A 0.024(10) 0.022(9) 0.038(8) 0.010(6) 0.000(7) 0.004(7) C15A 0.022(10) 0.024(10) 0.043(9) 0.011(8) 0.003(8) -0.013(7) C6A 0.026(4) 0.043(4) 0.046(5) 0.009(3) -0.012(3) 0.002(3) C25A 0.023(2) 0.035(4) 0.025(2) 0.005(2) -0.0057(17) -0.008(2) C26A 0.046(4) 0.035(4) 0.035(4) 0.002(3) -0.010(3) -0.014(3) C18 0.045(2) 0.088(3) 0.145(5) 0.078(3) -0.013(2) -0.012(2) F3 0.160(2) 0.0388(13) 0.0559(14) 0.0161(11) 0.0120(15) 0.0233(14) _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 Sr1 N2 2.565(2) . ? Sr1 O1 2.5709(18) . ? Sr1 O4 2.5730(19) . ? Sr1 N4 2.574(2) . ? Sr1 O2 2.5939(18) . ? Sr1 O3 2.5939(18) . ? Sr1 N1 2.631(2) . ? Sr1 N3 2.639(2) . ? N3 C9 1.350(3) . ? N3 N4 1.367(3) . ? N1 C1 1.356(3) . ? N1 N2 1.363(3) . ? C9 C10 1.392(3) . ? C9 C12 1.453(3) . ? N4 C11 1.346(3) . ? C1 C2 1.394(4) . ? C1 C4 1.445(3) . ? C2 C3 1.382(4) . ? N2 C3 1.339(3) . ? C10 C11 1.375(3) . ? C11 C16 1.480(4) . ? C3 C8 1.473(4) . ? C4 C5 1.402(17) . ? C4 C5A 1.408(13) . ? C4 S1 1.678(5) . ? C4 S1A 1.685(4) . ? C16 F6 1.316(4) . ? C16 F4 1.334(3) . ? C16 F5 1.341(3) . ? S2 C12 1.723(3) . ? S2 C15 1.728(8) . ? C5 C6 1.32(3) . ? O2 C24 1.432(4) . ? O2 C21 1.450(3) . ? S1 C7 1.683(17) . ? C21 C22 1.516(4) . ? C13 C14 1.330(16) . ? C13 C12 1.402(10) . ? C22 C23 1.493(4) . ? C24 C23 1.450(3) . ? C8 F3 1.319(4) . ? C8 F1 1.344(3) . ? C8 F2 1.345(4) . ? O1 C17 1.427(3) . ? O1 C20 1.442(3) . ? O3 C25A 1.418(4) . ? O3 C28 1.436(3) . ? O3 C25 1.534(8) . ? C15 C14 1.365(11) . ? C20 C19 1.487(4) . ? C6 C7 1.39(2) . ? C28 C27 1.528(4) . ? C25 C26 1.483(19) . ? C19 C18 1.505(5) . ? C27 C26 1.523(15) . ? C27 C26A 1.553(8) . ? C17 C18 1.503(5) . ? O4 C29 1.444(3) . ? O4 C32 1.447(4) . ? C30 C31 1.510(4) . ? C30 C29 1.513(4) . ? C32 C31 1.505(4) . ? S1A C7A 1.738(12) . ? C5A C6A 1.450(18) . ? C7A C6A 1.303(17) . ? C12 C13A 1.34(2) . ? C12 S2A 1.637(8) . ? C13A C14A 1.39(4) . ? S2A C15A 1.82(4) . ? C14A C15A 1.39(2) . ? C25A C26A 1.519(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Sr1 O1 110.30(7) . . ? N2 Sr1 O4 114.64(7) . . ? O1 Sr1 O4 76.52(6) . . ? N2 Sr1 N4 117.41(6) . . ? O1 Sr1 N4 116.17(6) . . ? O4 Sr1 N4 115.10(7) . . ? N2 Sr1 O2 78.17(6) . . ? O1 Sr1 O2 72.44(6) . . ? O4 Sr1 O2 148.93(6) . . ? N4 Sr1 O2 78.42(6) . . ? N2 Sr1 O3 78.48(7) . . ? O1 Sr1 O3 152.59(7) . . ? O4 Sr1 O3 76.27(7) . . ? N4 Sr1 O3 78.87(6) . . ? O2 Sr1 O3 134.79(6) . . ? N2 Sr1 N1 30.39(7) . . ? O1 Sr1 N1 93.35(6) . . ? O4 Sr1 N1 86.64(6) . . ? N4 Sr1 N1 146.04(6) . . ? O2 Sr1 N1 96.36(6) . . ? O3 Sr1 N1 81.81(6) . . ? N2 Sr1 N3 146.01(7) . . ? O1 Sr1 N3 89.42(6) . . ? O4 Sr1 N3 96.38(6) . . ? N4 Sr1 N3 30.37(6) . . ? O2 Sr1 N3 82.14(6) . . ? O3 Sr1 N3 96.83(6) . . ? N1 Sr1 N3 176.32(5) . . ? C9 N3 N4 108.36(19) . . ? C9 N3 Sr1 171.91(16) . . ? N4 N3 Sr1 72.17(12) . . ? C1 N1 N2 107.7(2) . . ? C1 N1 Sr1 176.49(16) . . ? N2 N1 Sr1 72.12(12) . . ? N3 C9 C10 109.8(2) . . ? N3 C9 C12 122.0(2) . . ? C10 C9 C12 128.1(2) . . ? C11 N4 N3 106.45(19) . . ? C11 N4 Sr1 170.96(17) . . ? N3 N4 Sr1 77.45(12) . . ? N1 C1 C2 109.8(2) . . ? N1 C1 C4 121.0(2) . . ? C2 C1 C4 129.2(2) . . ? C3 C2 C1 103.8(2) . . ? C3 N2 N1 107.7(2) . . ? C3 N2 Sr1 173.84(19) . . ? N1 N2 Sr1 77.49(13) . . ? C11 C10 C9 103.5(2) . . ? N4 C11 C10 111.8(2) . . ? N4 C11 C16 119.7(2) . . ? C10 C11 C16 128.4(2) . . ? N2 C3 C2 111.0(2) . . ? N2 C3 C8 120.0(2) . . ? C2 C3 C8 129.0(2) . . ? C5 C4 C5A 104.2(10) . . ? C5 C4 C1 130.3(8) . . ? C5A C4 C1 124.9(7) . . ? C5 C4 S1 105.7(8) . . ? C5A C4 S1 14.4(6) . . ? C1 C4 S1 123.7(3) . . ? C5 C4 S1A 7.7(9) . . ? C5A C4 S1A 111.8(7) . . ? C1 C4 S1A 122.6(2) . . ? S1 C4 S1A 113.3(3) . . ? F6 C16 F4 106.6(3) . . ? F6 C16 F5 105.3(2) . . ? F4 C16 F5 104.3(3) . . ? F6 C16 C11 114.5(2) . . ? F4 C16 C11 111.7(2) . . ? F5 C16 C11 113.7(2) . . ? C12 S2 C15 92.1(4) . . ? C6 C5 C4 117.8(15) . . ? C24 O2 C21 109.4(2) . . ? C24 O2 Sr1 125.91(17) . . ? C21 O2 Sr1 123.61(15) . . ? C4 S1 C7 95.2(6) . . ? O2 C21 C22 105.8(2) . . ? C14 C13 C12 116.6(7) . . ? C23 C22 C21 103.6(2) . . ? O2 C24 C23 108.0(3) . . ? F3 C8 F1 107.6(3) . . ? F3 C8 F2 106.1(3) . . ? F1 C8 F2 103.4(3) . . ? F3 C8 C3 114.0(3) . . ? F1 C8 C3 111.8(2) . . ? F2 C8 C3 113.3(2) . . ? C24 C23 C22 106.6(3) . . ? C17 O1 C20 106.0(2) . . ? C17 O1 Sr1 127.32(16) . . ? C20 O1 Sr1 124.99(16) . . ? C25A O3 C28 104.6(2) . . ? C25A O3 C25 30.0(4) . . ? C28 O3 C25 109.0(4) . . ? C25A O3 Sr1 129.6(2) . . ? C28 O3 Sr1 125.50(15) . . ? C25 O3 Sr1 120.2(4) . . ? C14 C15 S2 111.1(9) . . ? O1 C20 C19 105.0(2) . . ? C5 C6 C7 111.3(18) . . ? O3 C28 C27 105.4(2) . . ? C26 C25 O3 100.1(8) . . ? C13 C14 C15 112.7(10) . . ? C20 C19 C18 103.6(3) . . ? C26 C27 C28 100.6(6) . . ? C26 C27 C26A 21.9(4) . . ? C28 C27 C26A 104.5(3) . . ? C25 C26 C27 102.4(10) . . ? O1 C17 C18 106.1(3) . . ? C29 O4 C32 109.2(2) . . ? C29 O4 Sr1 124.56(16) . . ? C32 O4 Sr1 126.24(15) . . ? C31 C30 C29 102.2(2) . . ? O4 C29 C30 104.8(2) . . ? O4 C32 C31 106.6(2) . . ? C6 C7 S1 109.7(14) . . ? C32 C31 C30 103.6(2) . . ? C4 S1A C7A 91.8(5) . . ? C4 C5A C6A 110.1(11) . . ? C6A C7A S1A 112.5(10) . . ? C13A C12 C13 102.7(14) . . ? C13A C12 C9 126.1(14) . . ? C13 C12 C9 131.2(4) . . ? C13A C12 S2A 113.8(14) . . ? C13 C12 S2A 11.1(6) . . ? C9 C12 S2A 120.1(3) . . ? C13A C12 S2 5.2(14) . . ? C13 C12 S2 107.6(4) . . ? C9 C12 S2 121.17(19) . . ? S2A C12 S2 118.7(3) . . ? C12 C13A C14A 115(2) . . ? C12 S2A C15A 90.9(12) . . ? C15A C14A C13A 111(3) . . ? C14A C15A S2A 109(3) . . ? C7A C6A C5A 113.7(11) . . ? O3 C25A C26A 103.7(5) . . ? C25A C26A C27 100.1(5) . . ? C17 C18 C19 105.9(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.431 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.051 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 794841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Ba(ttfpz)2(thf)4] ; _chemical_name_common (Ba(ttfpz)2(thf)4) _chemical_melting_point ? _chemical_formula_moiety ; C32 H40 Ba F6 N4 O4 S2 ; _chemical_formula_sum 'C32 H40 Ba F6 N4 O4 S2' _chemical_formula_weight 860.14 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.7660(3) _cell_length_b 10.2146(2) _cell_length_c 19.2620(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3692.28(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 94905 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 1.259 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7038 _exptl_absorpt_correction_T_max 0.8336 _exptl_absorpt_process_details SADABS _exptl_special_details ; Disordered thiophene groups S(1) and S(2) and molecule thf O(1) were restrained using SIMU. C-C and C-S distances in thiophene S(1) were restrained with DFIX and DANG on atoms C(4), C(5) and C(5), S(1) respectively. Atoms C(23) and C(24) as well as atoms C(25) and C(26) of thf-molecules O(2) and O(3) respectively are disordered over two positions, their occupancies were refined to be approximately 60:40 and 56:44 respectively. Additionally, the TWIN command was used and the BASF value was refined to be 0.53. ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94905 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8484 _reflns_number_gt 8041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_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 0.539(17) _refine_ls_number_reflns 8484 _refine_ls_number_parameters 481 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.148 _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 Ba1 Ba 0.128557(9) 0.299686(18) 0.17547(3) 0.02437(7) Uani 1 1 d . B . S1 S -0.04095(8) 0.54162(17) 0.02852(9) 0.0539(4) Uani 1 1 d D B . S2 S 0.28862(6) 0.54125(12) 0.32916(8) 0.0401(3) Uani 1 1 d . B . F1 F 0.0030(2) -0.1231(3) -0.0169(2) 0.0657(10) Uani 1 1 d . B . F2 F 0.1118(2) -0.0747(4) -0.0031(2) 0.0643(10) Uani 1 1 d . B . F3 F 0.0476(3) -0.1132(4) 0.0863(2) 0.0878(16) Uani 1 1 d . B . F4 F 0.2577(2) -0.1291(3) 0.3647(3) 0.0789(14) Uani 1 1 d . B . F5 F 0.1494(2) -0.0856(3) 0.3461(2) 0.0614(10) Uani 1 1 d . B . F6 F 0.2183(3) -0.1252(4) 0.2618(2) 0.0802(14) Uani 1 1 d . B . O1 O 0.20596(18) 0.4979(4) 0.1176(2) 0.0458(9) Uani 1 1 d . . . O2 O 0.2416(2) 0.1925(4) 0.10597(19) 0.0463(10) Uani 1 1 d . . . O3 O 0.0119(2) 0.2079(4) 0.2455(2) 0.0484(10) Uani 1 1 d . . . O4 O 0.0592(2) 0.5228(4) 0.2149(2) 0.0481(9) Uani 1 1 d . . . N1 N 0.03238(19) 0.2856(4) 0.0651(2) 0.0278(7) Uani 1 1 d . . . N2 N 0.0598(2) 0.1635(4) 0.0740(2) 0.0318(8) Uani 1 1 d . B . N3 N 0.22420(18) 0.2795(3) 0.28554(19) 0.0244(7) Uani 1 1 d . . . N4 N 0.19590(18) 0.1574(4) 0.27762(19) 0.0265(7) Uani 1 1 d . B . C1 C -0.0181(2) 0.2793(4) 0.0148(2) 0.0265(8) Uani 1 1 d . B . C2 C -0.0237(2) 0.1517(5) -0.0103(2) 0.0324(9) Uani 1 1 d . . . H2 H -0.0540 0.1188 -0.0457 0.039 Uiso 1 1 calc R B . C3 C 0.0264(2) 0.0839(5) 0.0298(2) 0.0315(9) Uani 1 1 d . B . C4 C -0.0555(2) 0.3961(5) -0.0080(2) 0.0296(9) Uani 1 1 d DU . . C5 C -0.1090(2) 0.4078(3) -0.06515(17) 0.0229(8) Uani 1 1 d DU B . H5A H -0.1281 0.3393 -0.0928 0.028 Uiso 1 1 calc R . . C6 C -0.1260(3) 0.5504(7) -0.0694(4) 0.0571(17) Uani 1 1 d DU . . H6A H -0.1580 0.5858 -0.1027 0.069 Uiso 1 1 calc R B . C7 C -0.0930(3) 0.6223(5) -0.0235(3) 0.0423(12) Uani 1 1 d DU B . H7A H -0.0990 0.7145 -0.0207 0.051 Uiso 1 1 calc R . . C8 C 0.0467(3) -0.0558(5) 0.0259(3) 0.0435(11) Uani 1 1 d . . . C9 C 0.2787(2) 0.2712(4) 0.3306(2) 0.0224(7) Uani 1 1 d . B . C10 C 0.2871(2) 0.1427(4) 0.3530(2) 0.0283(8) Uani 1 1 d . . . H10 H 0.3213 0.1085 0.3845 0.034 Uiso 1 1 calc R B . C11 C 0.2337(2) 0.0771(4) 0.3184(2) 0.0284(8) Uani 1 1 d . B . C12 C 0.3183(2) 0.3875(4) 0.3512(2) 0.0235(7) Uani 1 1 d U . . C13 C 0.3846(3) 0.3898(5) 0.3918(2) 0.0281(9) Uani 1 1 d U B . H13 H 0.4100 0.3167 0.4095 0.034 Uiso 1 1 calc R . . C14 C 0.4031(3) 0.5285(5) 0.3990(3) 0.0403(11) Uani 1 1 d DU . . H14 H 0.4451 0.5559 0.4224 0.048 Uiso 1 1 calc R B . C15 C 0.3580(3) 0.6138(5) 0.3711(3) 0.0403(11) Uani 1 1 d DU B . H15 H 0.3639 0.7060 0.3742 0.048 Uiso 1 1 calc R . . C16 C 0.2153(3) -0.0636(5) 0.3223(3) 0.0403(11) Uani 1 1 d . . . C17 C 0.1874(4) 0.5741(7) 0.0579(4) 0.0659(17) Uani 1 1 d U . . H17A H 0.1364 0.5990 0.0595 0.079 Uiso 1 1 calc R . . H17B H 0.1961 0.5237 0.0148 0.079 Uiso 1 1 calc R . . C18 C 0.2331(5) 0.6925(8) 0.0599(6) 0.082(2) Uani 1 1 d U . . H18A H 0.2049 0.7706 0.0729 0.099 Uiso 1 1 calc R . . H18B H 0.2555 0.7081 0.0141 0.099 Uiso 1 1 calc R . . C19 C 0.2909(3) 0.6624(7) 0.1161(5) 0.0660(18) Uani 1 1 d U . . H19A H 0.3394 0.6826 0.0989 0.079 Uiso 1 1 calc R . . H19B H 0.2820 0.7122 0.1593 0.079 Uiso 1 1 calc R . . C20 C 0.2812(3) 0.5181(6) 0.1272(3) 0.0475(13) Uani 1 1 d . . . H20A H 0.3091 0.4672 0.0929 0.057 Uiso 1 1 calc R . . H20B H 0.2961 0.4924 0.1745 0.057 Uiso 1 1 calc R . . C21 C 0.2431(3) 0.1767(6) 0.0313(3) 0.0388(10) Uani 1 1 d . B . H21A H 0.2595 0.2581 0.0084 0.047 Uiso 1 1 calc R . . H21B H 0.1952 0.1541 0.0134 0.047 Uiso 1 1 calc R . . C22 C 0.2952(3) 0.0657(6) 0.0186(3) 0.0454(12) Uani 1 1 d . . . H22A H 0.2697 -0.0188 0.0148 0.054 Uiso 1 1 calc R A 1 H22B H 0.3224 0.0807 -0.0247 0.054 Uiso 1 1 calc R A 1 C23 C 0.3444(10) 0.065(2) 0.0807(10) 0.055(4) Uani 0.60(3) 1 d P B 1 H23A H 0.3819 0.1332 0.0767 0.065 Uiso 0.60(3) 1 calc PR B 1 H23B H 0.3670 -0.0213 0.0877 0.065 Uiso 0.60(3) 1 calc PR B 1 C23A C 0.3232(15) 0.032(2) 0.0930(12) 0.041(5) Uani 0.40(3) 1 d P B 2 H23C H 0.2950 -0.0393 0.1148 0.050 Uiso 0.40(3) 1 calc PR B 2 H23D H 0.3742 0.0070 0.0926 0.050 Uiso 0.40(3) 1 calc PR B 2 C24 C 0.2915(8) 0.0973(18) 0.1388(6) 0.047(4) Uani 0.60(3) 1 d P B 1 H24A H 0.2659 0.0176 0.1541 0.057 Uiso 0.60(3) 1 calc PR B 1 H24B H 0.3160 0.1368 0.1791 0.057 Uiso 0.60(3) 1 calc PR B 1 C24A C 0.3111(7) 0.161(2) 0.1280(7) 0.030(4) Uani 0.40(3) 1 d P B 2 H24C H 0.3137 0.1527 0.1791 0.036 Uiso 0.40(3) 1 calc PR B 2 H24D H 0.3461 0.2272 0.1123 0.036 Uiso 0.40(3) 1 calc PR B 2 C25 C -0.0575(7) 0.1869(11) 0.2205(7) 0.022(3) Uani 0.56(5) 1 d P B 3 H25A H -0.0588 0.1924 0.1692 0.027 Uiso 0.56(5) 1 calc PR B 3 H25B H -0.0909 0.2524 0.2400 0.027 Uiso 0.56(5) 1 calc PR B 3 C25A C -0.048(2) 0.146(6) 0.2055(17) 0.089(12) Uani 0.44(5) 1 d P B 4 H25C H -0.0812 0.2126 0.1876 0.107 Uiso 0.44(5) 1 calc PR B 4 H25D H -0.0293 0.0937 0.1660 0.107 Uiso 0.44(5) 1 calc PR B 4 C26 C -0.0776(12) 0.044(2) 0.2460(10) 0.036(4) Uani 0.56(5) 1 d P B 3 H26A H -0.1298 0.0289 0.2471 0.043 Uiso 0.56(5) 1 calc PR B 3 H26B H -0.0541 -0.0252 0.2182 0.043 Uiso 0.56(5) 1 calc PR B 3 C26A C -0.077(2) 0.075(5) 0.248(2) 0.084(14) Uani 0.44(5) 1 d P B 4 H26C H -0.0814 -0.0132 0.2269 0.100 Uiso 0.44(5) 1 calc PR B 4 H26D H -0.1263 0.1083 0.2543 0.100 Uiso 0.44(5) 1 calc PR B 4 C27 C -0.0451(3) 0.0575(5) 0.3196(3) 0.0412(11) Uani 1 1 d . . . H27A H -0.0824 0.0823 0.3534 0.049 Uiso 1 1 calc R B 3 H27B H -0.0238 -0.0267 0.3345 0.049 Uiso 1 1 calc R B 3 C28 C 0.0115(3) 0.1626(6) 0.3160(3) 0.0420(11) Uani 1 1 d . B . H28A H 0.0000 0.2353 0.3481 0.050 Uiso 1 1 calc R . . H28B H 0.0587 0.1263 0.3287 0.050 Uiso 1 1 calc R . . C29 C -0.0169(3) 0.5334(6) 0.2209(3) 0.0446(12) Uani 1 1 d . B . H29A H -0.0337 0.4953 0.2652 0.053 Uiso 1 1 calc R . . H29B H -0.0409 0.4880 0.1819 0.053 Uiso 1 1 calc R . . C30 C -0.0313(3) 0.6793(6) 0.2185(3) 0.0490(13) Uani 1 1 d . . . H30A H -0.0343 0.7112 0.1700 0.059 Uiso 1 1 calc R B . H30B H -0.0760 0.7016 0.2431 0.059 Uiso 1 1 calc R . . C31 C 0.0327(3) 0.7353(6) 0.2552(3) 0.0531(14) Uani 1 1 d . B . H31A H 0.0419 0.8266 0.2405 0.064 Uiso 1 1 calc R . . H31B H 0.0263 0.7330 0.3062 0.064 Uiso 1 1 calc R . . C32 C 0.0920(3) 0.6459(6) 0.2328(4) 0.0554(15) Uani 1 1 d . B . H32A H 0.1173 0.6830 0.1922 0.066 Uiso 1 1 calc R . . H32B H 0.1268 0.6338 0.2710 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.02041(10) 0.02778(11) 0.02491(11) -0.00012(14) -0.00347(12) 0.00058(7) S1 0.0474(8) 0.0600(9) 0.0543(8) -0.0020(7) 0.0042(6) 0.0038(6) S2 0.0337(6) 0.0317(6) 0.0549(7) 0.0033(5) -0.0057(5) -0.0026(4) F1 0.076(3) 0.0413(18) 0.080(3) -0.0167(18) -0.016(2) -0.0126(17) F2 0.058(2) 0.049(2) 0.087(3) -0.0101(19) 0.002(2) 0.0103(18) F3 0.167(5) 0.045(2) 0.051(2) 0.0149(18) 0.015(3) 0.012(3) F4 0.082(3) 0.0297(16) 0.125(4) 0.021(2) -0.042(3) 0.0018(17) F5 0.057(2) 0.0360(17) 0.091(3) 0.0090(17) 0.016(2) -0.0149(16) F6 0.135(4) 0.0380(19) 0.067(3) -0.0217(18) 0.028(3) -0.023(2) O1 0.0348(17) 0.054(2) 0.049(2) 0.0185(18) -0.0023(15) -0.0114(16) O2 0.0340(18) 0.072(3) 0.0329(18) -0.0157(17) -0.0048(15) 0.0205(17) O3 0.0281(17) 0.073(3) 0.044(2) 0.0139(19) -0.0025(15) -0.0124(16) O4 0.0392(18) 0.044(2) 0.061(2) -0.0158(18) 0.0047(17) 0.0078(16) N1 0.0233(17) 0.0340(19) 0.0260(17) 0.0009(14) -0.0022(14) -0.0018(13) N2 0.0280(18) 0.0356(19) 0.0319(19) -0.0047(16) -0.0021(15) 0.0000(15) N3 0.0200(15) 0.0268(16) 0.0265(16) 0.0010(13) -0.0022(13) -0.0007(12) N4 0.0251(16) 0.0236(16) 0.0308(18) -0.0003(14) -0.0005(14) -0.0004(13) C1 0.0222(18) 0.037(2) 0.0199(18) -0.0009(15) 0.0001(14) -0.0059(16) C2 0.030(2) 0.038(2) 0.029(2) 0.0017(18) -0.0047(17) -0.0091(18) C3 0.033(2) 0.032(2) 0.029(2) 0.0023(18) 0.0002(17) -0.0072(18) C4 0.0241(19) 0.038(2) 0.0264(19) 0.0012(17) -0.0048(15) -0.0059(17) C5 0.041(2) 0.0140(16) 0.0142(16) 0.0050(13) -0.0070(16) 0.0084(15) C6 0.044(3) 0.067(4) 0.061(4) 0.025(3) -0.025(3) -0.006(2) C7 0.030(3) 0.038(3) 0.058(3) -0.001(2) 0.009(2) 0.005(2) C8 0.050(3) 0.033(2) 0.048(3) -0.003(2) -0.006(2) -0.004(2) C9 0.0218(17) 0.0243(17) 0.0211(17) -0.0010(15) 0.0029(14) 0.0025(14) C10 0.028(2) 0.028(2) 0.029(2) 0.0019(16) 0.0001(16) 0.0072(16) C11 0.028(2) 0.027(2) 0.030(2) 0.0011(17) 0.0034(16) 0.0034(16) C12 0.0233(18) 0.0249(18) 0.0223(18) 0.0027(14) -0.0009(14) 0.0036(14) C13 0.025(2) 0.031(2) 0.027(2) -0.0045(17) 0.0039(17) -0.0085(17) C14 0.040(3) 0.043(3) 0.038(2) -0.005(2) -0.011(2) -0.008(2) C15 0.037(2) 0.026(2) 0.057(3) -0.004(2) 0.011(2) -0.0076(18) C16 0.042(3) 0.029(2) 0.050(3) 0.000(2) 0.001(2) 0.0025(19) C17 0.063(4) 0.070(4) 0.065(4) 0.023(3) -0.020(3) -0.009(3) C18 0.068(4) 0.073(4) 0.106(5) 0.035(4) 0.006(4) -0.007(3) C19 0.047(3) 0.053(3) 0.098(5) -0.015(3) 0.022(3) -0.012(3) C20 0.031(2) 0.065(3) 0.047(3) 0.003(3) 0.002(2) -0.005(2) C21 0.033(2) 0.052(3) 0.031(2) 0.000(2) 0.0003(19) 0.006(2) C22 0.054(3) 0.050(3) 0.032(3) -0.007(2) 0.005(2) 0.004(2) C23 0.057(9) 0.061(10) 0.046(7) 0.010(6) 0.015(6) 0.015(7) C23A 0.056(14) 0.038(10) 0.030(9) -0.004(7) -0.003(8) 0.021(8) C24 0.050(6) 0.051(8) 0.042(5) -0.001(5) 0.006(4) 0.018(6) C24A 0.026(6) 0.042(9) 0.023(5) 0.001(5) -0.004(4) 0.003(6) C25 0.014(4) 0.031(5) 0.022(5) -0.001(3) 0.001(3) 0.003(3) C25A 0.060(17) 0.15(3) 0.052(13) 0.004(16) -0.006(10) -0.05(2) C26 0.051(7) 0.029(8) 0.029(6) 0.004(4) 0.000(5) -0.019(5) C26A 0.11(2) 0.05(2) 0.088(19) 0.017(13) -0.051(16) -0.052(15) C27 0.052(3) 0.037(2) 0.034(2) 0.003(2) 0.008(2) -0.005(2) C28 0.029(2) 0.059(3) 0.038(3) 0.000(2) -0.0009(19) 0.001(2) C29 0.040(3) 0.049(3) 0.045(3) 0.001(2) 0.012(2) 0.003(2) C30 0.043(3) 0.047(3) 0.057(3) 0.003(2) 0.010(2) 0.012(2) C31 0.060(4) 0.043(3) 0.057(4) -0.016(3) 0.000(3) 0.014(3) C32 0.046(3) 0.043(3) 0.077(4) -0.021(3) 0.000(3) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 N2 2.724(4) . ? Ba1 O1 2.730(3) . ? Ba1 O4 2.732(4) . ? Ba1 O2 2.736(3) . ? Ba1 O3 2.736(4) . ? Ba1 N4 2.753(4) . ? Ba1 N3 2.786(4) . ? Ba1 N1 2.792(4) . ? S1 C7 1.623(6) . ? S1 C4 1.667(5) . ? S2 C15 1.702(5) . ? S2 C12 1.720(4) . ? F1 C8 1.353(6) . ? F2 C8 1.357(7) . ? F3 C8 1.303(7) . ? F4 C16 1.322(7) . ? F5 C16 1.337(6) . ? F6 C16 1.326(7) . ? O1 C17 1.432(7) . ? O1 C20 1.439(6) . ? O2 C24A 1.410(12) . ? O2 C21 1.447(6) . ? O2 C24 1.491(11) . ? O3 C25 1.406(14) . ? O3 C28 1.435(7) . ? O3 C25A 1.50(3) . ? O4 C29 1.436(6) . ? O4 C32 1.442(7) . ? N1 C1 1.357(5) . ? N1 N2 1.360(5) . ? N2 C3 1.332(6) . ? N3 C9 1.344(5) . ? N3 N4 1.364(5) . ? N4 C11 1.338(6) . ? C1 C2 1.395(7) . ? C1 C4 1.452(6) . ? C2 C3 1.401(7) . ? C3 C8 1.479(7) . ? C4 C5 1.496(5) . ? C5 C6 1.493(8) . ? C6 C7 1.305(7) . ? C9 C10 1.390(6) . ? C9 C12 1.457(5) . ? C10 C11 1.378(6) . ? C11 C16 1.481(6) . ? C12 C13 1.468(6) . ? C13 C14 1.466(7) . ? C14 C15 1.328(7) . ? C17 C18 1.483(10) . ? C18 C19 1.563(12) . ? C19 C20 1.500(9) . ? C21 C22 1.517(7) . ? C22 C23 1.51(2) . ? C22 C23A 1.57(2) . ? C23 C24 1.53(2) . ? C23A C24A 1.50(3) . ? C25 C26 1.59(3) . ? C25A C26A 1.22(5) . ? C26 C27 1.55(2) . ? C26A C27 1.52(4) . ? C27 C28 1.512(7) . ? C29 C30 1.515(8) . ? C30 C31 1.507(9) . ? C31 C32 1.503(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 N2 Ba1 O1 109.75(13) . . ? N2 Ba1 O4 113.56(12) . . ? O1 Ba1 O4 75.43(13) . . ? N2 Ba1 O2 79.15(11) . . ? O1 Ba1 O2 71.61(12) . . ? O4 Ba1 O2 147.03(13) . . ? N2 Ba1 O3 78.44(12) . . ? O1 Ba1 O3 151.75(13) . . ? O4 Ba1 O3 76.56(13) . . ? O2 Ba1 O3 136.38(12) . . ? N2 Ba1 N4 117.42(10) . . ? O1 Ba1 N4 116.04(11) . . ? O4 Ba1 N4 117.41(12) . . ? O2 Ba1 N4 77.45(11) . . ? O3 Ba1 N4 80.46(11) . . ? N2 Ba1 N3 144.44(11) . . ? O1 Ba1 N3 91.31(11) . . ? O4 Ba1 N3 99.04(11) . . ? O2 Ba1 N3 80.99(11) . . ? O3 Ba1 N3 96.60(11) . . ? N4 Ba1 N3 28.50(10) . . ? N2 Ba1 N1 28.51(11) . . ? O1 Ba1 N1 94.09(11) . . ? O4 Ba1 N1 86.95(11) . . ? O2 Ba1 N1 96.19(11) . . ? O3 Ba1 N1 80.82(11) . . ? N4 Ba1 N1 144.43(11) . . ? N3 Ba1 N1 172.79(9) . . ? C7 S1 C4 95.4(2) . . ? C15 S2 C12 91.8(2) . . ? C17 O1 C20 105.3(4) . . ? C17 O1 Ba1 127.0(3) . . ? C20 O1 Ba1 125.2(3) . . ? C24A O2 C21 104.8(6) . . ? C24A O2 C24 30.9(6) . . ? C21 O2 C24 109.6(5) . . ? C24A O2 Ba1 131.4(5) . . ? C21 O2 Ba1 123.1(3) . . ? C24 O2 Ba1 122.7(5) . . ? C25 O3 C28 105.6(6) . . ? C25 O3 C25A 21(2) . . ? C28 O3 C25A 110.1(12) . . ? C25 O3 Ba1 128.7(6) . . ? C28 O3 Ba1 125.5(3) . . ? C25A O3 Ba1 119.4(14) . . ? C29 O4 C32 109.9(4) . . ? C29 O4 Ba1 124.0(3) . . ? C32 O4 Ba1 126.2(3) . . ? C1 N1 N2 108.1(4) . . ? C1 N1 Ba1 176.0(3) . . ? N2 N1 Ba1 73.0(2) . . ? C3 N2 N1 107.5(4) . . ? C3 N2 Ba1 172.7(3) . . ? N1 N2 Ba1 78.5(2) . . ? C9 N3 N4 108.1(3) . . ? C9 N3 Ba1 170.6(3) . . ? N4 N3 Ba1 74.4(2) . . ? C11 N4 N3 106.7(3) . . ? C11 N4 Ba1 170.3(3) . . ? N3 N4 Ba1 77.1(2) . . ? N1 C1 C2 110.1(4) . . ? N1 C1 C4 121.0(4) . . ? C2 C1 C4 128.8(4) . . ? C1 C2 C3 102.7(4) . . ? N2 C3 C2 111.5(4) . . ? N2 C3 C8 120.0(4) . . ? C2 C3 C8 128.4(4) . . ? C1 C4 C5 127.8(4) . . ? C1 C4 S1 121.7(3) . . ? C5 C4 S1 110.4(3) . . ? C6 C5 C4 105.1(3) . . ? C7 C6 C5 114.3(5) . . ? C6 C7 S1 114.7(5) . . ? F3 C8 F1 108.9(5) . . ? F3 C8 F2 107.0(5) . . ? F1 C8 F2 102.8(5) . . ? F3 C8 C3 113.1(5) . . ? F1 C8 C3 111.4(5) . . ? F2 C8 C3 113.0(4) . . ? N3 C9 C10 110.3(4) . . ? N3 C9 C12 120.9(4) . . ? C10 C9 C12 128.8(4) . . ? C11 C10 C9 103.1(4) . . ? N4 C11 C10 111.8(4) . . ? N4 C11 C16 120.1(4) . . ? C10 C11 C16 128.1(4) . . ? C9 C12 C13 126.1(4) . . ? C9 C12 S2 120.8(3) . . ? C13 C12 S2 113.1(3) . . ? C14 C13 C12 105.5(4) . . ? C15 C14 C13 116.4(4) . . ? C14 C15 S2 113.2(4) . . ? F4 C16 F6 106.1(5) . . ? F4 C16 F5 105.1(5) . . ? F6 C16 F5 105.1(5) . . ? F4 C16 C11 112.5(4) . . ? F6 C16 C11 113.9(5) . . ? F5 C16 C11 113.3(4) . . ? O1 C17 C18 106.3(6) . . ? C17 C18 C19 105.1(6) . . ? C20 C19 C18 101.9(6) . . ? O1 C20 C19 104.0(5) . . ? O2 C21 C22 104.9(4) . . ? C23 C22 C21 105.5(8) . . ? C23 C22 C23A 21.6(8) . . ? C21 C22 C23A 103.6(9) . . ? C22 C23 C24 100.4(13) . . ? C24A C23A C22 99.5(15) . . ? O2 C24 C23 103.8(12) . . ? O2 C24A C23A 101.9(15) . . ? O3 C25 C26 104.8(11) . . ? C26A C25A O3 104(3) . . ? C27 C26 C25 96.1(15) . . ? C25A C26A C27 120(3) . . ? C28 C27 C26A 98.8(15) . . ? C28 C27 C26 107.3(9) . . ? C26A C27 C26 12(2) . . ? O3 C28 C27 106.1(4) . . ? O4 C29 C30 104.4(4) . . ? C31 C30 C29 102.5(5) . . ? C32 C31 C30 103.0(5) . . ? O4 C32 C31 106.3(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.042 _refine_diff_density_min -1.242 _refine_diff_density_rms 0.093 #===END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 794842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Ca(ttfpz)2(dme)2] ; _chemical_name_common (Ca(ttfpz)2(dme)2) _chemical_melting_point ? _chemical_formula_moiety ; C24 H28 Ca F6 N4 O4 S2 ; _chemical_formula_sum 'C24 H28 Ca F6 N4 O4 S2' _chemical_formula_weight 654.70 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 7.7619(2) _cell_length_b 18.9930(6) _cell_length_c 19.8639(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.6190(10) _cell_angle_gamma 90.00 _cell_volume 2887.20(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 39058 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9174 _exptl_absorpt_correction_T_max 0.9575 _exptl_absorpt_process_details SADABS _exptl_special_details ; The EADP constraint was applied on atom C13 with atom C5 as reference. ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39058 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6611 _reflns_number_gt 5867 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6611 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1221 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.51741(5) 0.08112(2) 0.30344(2) 0.01349(11) Uani 1 1 d . . . S1 S 0.33340(9) 0.25267(3) 0.44274(3) 0.02840(15) Uani 1 1 d . . . S2 S 0.70124(9) 0.01533(3) 0.09993(3) 0.03067(16) Uani 1 1 d . . . F1 F 0.2845(3) 0.29139(10) 0.09307(9) 0.0620(6) Uani 1 1 d . . . F4 F 0.7983(4) -0.19630(9) 0.38794(10) 0.0665(7) Uani 1 1 d . . . F2 F 0.1282(3) 0.19845(11) 0.09150(8) 0.0530(5) Uani 1 1 d . . . F5 F 0.6194(3) -0.12384(14) 0.42040(10) 0.0714(7) Uani 1 1 d . . . F3 F 0.4043(3) 0.18906(10) 0.09842(8) 0.0459(4) Uani 1 1 d . . . F6 F 0.8885(3) -0.10214(11) 0.43813(9) 0.0576(5) Uani 1 1 d . . . O1 O 0.6549(2) 0.11914(8) 0.41635(8) 0.0205(3) Uani 1 1 d . . . O2 O 0.7862(2) 0.14728(8) 0.30394(8) 0.0201(3) Uani 1 1 d . . . O3 O 0.2860(2) 0.01629(9) 0.23141(8) 0.0231(3) Uani 1 1 d . . . O4 O 0.30905(19) 0.02655(8) 0.36954(8) 0.0193(3) Uani 1 1 d . . . N1 N 0.3675(2) 0.19411(10) 0.30053(9) 0.0186(4) Uani 1 1 d . . . N3 N 0.6802(2) -0.00845(9) 0.25118(9) 0.0159(3) Uani 1 1 d . . . N2 N 0.3804(2) 0.17833(10) 0.23445(9) 0.0203(4) Uani 1 1 d . . . N4 N 0.6771(2) -0.02794(10) 0.31704(9) 0.0176(4) Uani 1 1 d . . . C17 C 0.6618(4) 0.07725(15) 0.47607(12) 0.0347(6) Uani 1 1 d . . . H17A H 0.7740 0.0525 0.4853 0.052 Uiso 1 1 calc R . . H17B H 0.5664 0.0428 0.4691 0.052 Uiso 1 1 calc R . . H17C H 0.6496 0.1076 0.5149 0.052 Uiso 1 1 calc R . . C3 C 0.2996(3) 0.23024(12) 0.19570(11) 0.0209(4) Uani 1 1 d . . . C11 C 0.7434(3) -0.09319(11) 0.32480(11) 0.0174(4) Uani 1 1 d . . . C18 C 0.7974(3) 0.16750(13) 0.42229(12) 0.0259(5) Uani 1 1 d . . . H18A H 0.9091 0.1423 0.4365 0.031 Uiso 1 1 calc R . . H18B H 0.7854 0.2036 0.4572 0.031 Uiso 1 1 calc R . . C2 C 0.2328(3) 0.28036(11) 0.23485(11) 0.0212(4) Uani 1 1 d . . . H2 H 0.1701 0.3220 0.2200 0.025 Uiso 1 1 calc R . . C10 C 0.7912(3) -0.11794(11) 0.26489(11) 0.0179(4) Uani 1 1 d . . . H10 H 0.8412 -0.1621 0.2567 0.021 Uiso 1 1 calc R . . C19 C 0.7962(3) 0.20209(13) 0.35400(13) 0.0266(5) Uani 1 1 d . . . H19A H 0.6943 0.2339 0.3432 0.032 Uiso 1 1 calc R . . H19B H 0.9040 0.2301 0.3546 0.032 Uiso 1 1 calc R . . C1 C 0.2790(3) 0.25530(11) 0.30105(11) 0.0166(4) Uani 1 1 d . . . C9 C 0.7476(3) -0.06189(11) 0.21955(10) 0.0151(4) Uani 1 1 d . . . C20 C 0.8307(4) 0.17095(15) 0.24076(13) 0.0326(6) Uani 1 1 d . . . H20A H 0.7487 0.2078 0.2214 0.049 Uiso 1 1 calc R . . H20B H 0.8242 0.1313 0.2088 0.049 Uiso 1 1 calc R . . H20C H 0.9498 0.1900 0.2488 0.049 Uiso 1 1 calc R . . C8 C 0.2807(4) 0.22723(14) 0.12037(13) 0.0328(6) Uani 1 1 d . . . C16 C 0.7602(3) -0.12878(13) 0.39176(12) 0.0247(5) Uani 1 1 d . . . C21 C 0.2288(3) 0.02825(14) 0.16036(12) 0.0290(5) Uani 1 1 d . . . H21A H 0.2052 -0.0170 0.1369 0.044 Uiso 1 1 calc R . . H21B H 0.3199 0.0534 0.1414 0.044 Uiso 1 1 calc R . . H21C H 0.1217 0.0566 0.1539 0.044 Uiso 1 1 calc R . . C4 C 0.2408(3) 0.28574(11) 0.36440(11) 0.0170(4) Uani 1 1 d . . . C12 C 0.7733(3) -0.05645(11) 0.14875(10) 0.0163(4) Uani 1 1 d . . . C22 C 0.1601(3) -0.02113(12) 0.26202(12) 0.0222(5) Uani 1 1 d . . . H22A H 0.1273 -0.0655 0.2370 0.027 Uiso 1 1 calc R . . H22B H 0.0535 0.0077 0.2612 0.027 Uiso 1 1 calc R . . C5 C 0.1258(3) 0.34175(11) 0.37066(10) 0.0163(3) Uani 1 1 d . . . H5 H 0.0635 0.3679 0.3336 0.020 Uiso 1 1 calc R . . C13 C 0.8606(3) -0.10890(12) 0.11154(10) 0.0163(3) Uani 1 1 d . . . H13 H 0.9074 -0.1530 0.1282 0.020 Uiso 1 1 calc R . . C23 C 0.2435(3) -0.03658(12) 0.33459(12) 0.0214(4) Uani 1 1 d . . . H23A H 0.1562 -0.0586 0.3591 0.026 Uiso 1 1 calc R . . H23B H 0.3406 -0.0704 0.3346 0.026 Uiso 1 1 calc R . . C6 C 0.1165(3) 0.35359(13) 0.44167(13) 0.0277(5) Uani 1 1 d . . . H6 H 0.0443 0.3886 0.4568 0.033 Uiso 1 1 calc R . . C14 C 0.8605(3) -0.07930(14) 0.04367(13) 0.0287(5) Uani 1 1 d . . . H14 H 0.9128 -0.1030 0.0101 0.034 Uiso 1 1 calc R . . C24 C 0.1740(3) 0.06755(13) 0.39185(13) 0.0281(5) Uani 1 1 d . . . H24A H 0.0907 0.0832 0.3521 0.042 Uiso 1 1 calc R . . H24B H 0.2259 0.1087 0.4173 0.042 Uiso 1 1 calc R . . H24C H 0.1130 0.0388 0.4214 0.042 Uiso 1 1 calc R . . C7 C 0.2203(4) 0.31017(13) 0.48484(13) 0.0307(5) Uani 1 1 d . . . H7 H 0.2291 0.3116 0.5331 0.037 Uiso 1 1 calc R . . C15 C 0.7813(3) -0.01604(14) 0.03175(12) 0.0295(5) Uani 1 1 d . . . H15 H 0.7716 0.0082 -0.0105 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.01328(19) 0.0134(2) 0.0137(2) -0.00064(14) 0.00188(14) 0.00052(14) S1 0.0393(3) 0.0233(3) 0.0225(3) 0.0010(2) 0.0048(2) 0.0075(2) S2 0.0387(4) 0.0306(3) 0.0234(3) 0.0029(2) 0.0073(3) 0.0049(3) F1 0.1261(19) 0.0343(10) 0.0260(9) 0.0164(7) 0.0136(10) 0.0073(11) F4 0.137(2) 0.0280(9) 0.0356(10) 0.0137(8) 0.0179(11) 0.0236(11) F2 0.0568(11) 0.0693(13) 0.0260(8) -0.0081(8) -0.0137(8) -0.0004(10) F5 0.0465(11) 0.121(2) 0.0536(12) 0.0562(13) 0.0285(9) 0.0277(12) F3 0.0645(12) 0.0510(11) 0.0255(8) 0.0008(7) 0.0173(8) 0.0084(9) F6 0.0718(13) 0.0684(13) 0.0248(8) 0.0107(8) -0.0148(8) -0.0143(11) O1 0.0219(7) 0.0225(8) 0.0160(7) -0.0017(6) 0.0000(6) -0.0030(6) O2 0.0220(7) 0.0196(8) 0.0197(8) -0.0023(6) 0.0060(6) -0.0053(6) O3 0.0197(8) 0.0298(9) 0.0186(8) -0.0006(6) -0.0007(6) -0.0082(6) O4 0.0185(7) 0.0187(7) 0.0217(8) -0.0032(6) 0.0058(6) -0.0012(6) N1 0.0202(9) 0.0186(9) 0.0163(9) 0.0001(7) 0.0006(7) 0.0032(7) N3 0.0157(8) 0.0169(8) 0.0153(8) 0.0003(7) 0.0035(6) 0.0015(6) N2 0.0243(9) 0.0209(9) 0.0153(9) 0.0012(7) 0.0019(7) 0.0021(7) N4 0.0191(8) 0.0199(9) 0.0142(8) 0.0009(7) 0.0034(7) 0.0029(7) C17 0.0400(15) 0.0446(16) 0.0171(11) 0.0045(11) -0.0019(10) -0.0072(12) C3 0.0253(11) 0.0184(10) 0.0181(10) 0.0048(8) 0.0013(8) -0.0011(8) C11 0.0171(9) 0.0172(10) 0.0180(10) 0.0013(8) 0.0029(8) 0.0000(8) C18 0.0216(11) 0.0310(13) 0.0244(11) -0.0108(10) 0.0019(9) -0.0054(9) C2 0.0245(11) 0.0145(10) 0.0231(11) 0.0043(8) -0.0006(8) -0.0006(8) C10 0.0197(10) 0.0144(10) 0.0198(10) -0.0001(8) 0.0038(8) 0.0008(8) C19 0.0270(12) 0.0212(11) 0.0323(13) -0.0084(9) 0.0068(10) -0.0090(9) C1 0.0157(9) 0.0127(9) 0.0206(10) 0.0012(8) 0.0005(8) -0.0012(7) C9 0.0120(9) 0.0168(10) 0.0164(10) -0.0015(8) 0.0019(7) -0.0021(7) C20 0.0371(14) 0.0355(14) 0.0279(13) 0.0021(11) 0.0134(11) -0.0103(11) C8 0.0487(16) 0.0278(13) 0.0207(12) 0.0044(10) 0.0025(11) 0.0039(11) C16 0.0277(11) 0.0273(12) 0.0196(11) 0.0056(9) 0.0055(9) 0.0042(9) C21 0.0314(13) 0.0350(13) 0.0186(11) 0.0000(10) -0.0019(9) -0.0068(10) C4 0.0160(9) 0.0139(9) 0.0204(10) 0.0013(8) 0.0012(8) -0.0017(7) C12 0.0160(9) 0.0166(10) 0.0161(10) -0.0016(8) 0.0021(7) -0.0018(7) C22 0.0171(10) 0.0237(11) 0.0250(11) -0.0005(9) 0.0013(8) -0.0053(8) C5 0.0117(6) 0.0238(8) 0.0138(6) -0.0028(5) 0.0031(5) -0.0040(5) C13 0.0117(6) 0.0238(8) 0.0138(6) -0.0028(5) 0.0031(5) -0.0040(5) C23 0.0210(10) 0.0180(10) 0.0248(11) -0.0004(8) 0.0026(8) -0.0049(8) C6 0.0258(11) 0.0238(12) 0.0346(13) -0.0089(10) 0.0085(10) 0.0010(9) C14 0.0320(13) 0.0315(13) 0.0256(12) -0.0081(10) 0.0130(10) -0.0032(10) C24 0.0302(12) 0.0266(12) 0.0310(13) 0.0004(10) 0.0153(10) 0.0060(10) C7 0.0403(14) 0.0273(13) 0.0262(12) -0.0041(10) 0.0106(10) 0.0003(10) C15 0.0369(14) 0.0345(14) 0.0177(11) 0.0021(10) 0.0064(10) -0.0011(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 Ca1 N4 2.4058(18) . ? Ca1 O1 2.4272(15) . ? Ca1 O2 2.4343(15) . ? Ca1 N2 2.4352(19) . ? Ca1 O3 2.4356(15) . ? Ca1 N1 2.4374(18) . ? Ca1 N3 2.4511(18) . ? Ca1 O4 2.4746(15) . ? Ca1 C19 3.200(2) . ? Ca1 C23 3.216(2) . ? S1 C7 1.705(3) . ? S1 C4 1.720(2) . ? S2 C15 1.690(3) . ? S2 C12 1.712(2) . ? F1 C8 1.336(3) . ? F4 C16 1.321(3) . ? F2 C8 1.342(3) . ? F5 C16 1.318(3) . ? F3 C8 1.333(3) . ? F6 C16 1.338(3) . ? O1 C17 1.422(3) . ? O1 C18 1.427(3) . ? O2 C20 1.429(3) . ? O2 C19 1.433(3) . ? O3 C22 1.424(3) . ? O3 C21 1.425(3) . ? O4 C24 1.434(3) . ? O4 C23 1.436(3) . ? N1 C1 1.351(3) . ? N1 N2 1.366(3) . ? N3 C9 1.345(3) . ? N3 N4 1.364(2) . ? N2 C3 1.341(3) . ? N4 C11 1.341(3) . ? C3 C2 1.384(3) . ? C3 C8 1.480(3) . ? C11 C10 1.387(3) . ? C11 C16 1.478(3) . ? C18 C19 1.506(4) . ? C2 C1 1.388(3) . ? C10 C9 1.399(3) . ? C1 C4 1.460(3) . ? C9 C12 1.457(3) . ? C4 C5 1.408(3) . ? C12 C13 1.472(3) . ? C22 C23 1.507(3) . ? C5 C6 1.442(3) . ? C13 C14 1.461(3) . ? C6 C7 1.354(4) . ? C14 C15 1.353(4) . ? 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 N4 Ca1 O1 90.77(6) . . ? N4 Ca1 O2 91.08(6) . . ? O1 Ca1 O2 66.32(5) . . ? N4 Ca1 N2 152.16(6) . . ? O1 Ca1 N2 112.19(6) . . ? O2 Ca1 N2 84.51(6) . . ? N4 Ca1 O3 86.92(6) . . ? O1 Ca1 O3 149.38(6) . . ? O2 Ca1 O3 144.20(5) . . ? N2 Ca1 O3 80.96(6) . . ? N4 Ca1 N1 174.70(6) . . ? O1 Ca1 N1 83.94(6) . . ? O2 Ca1 N1 87.20(6) . . ? N2 Ca1 N1 32.57(6) . . ? O3 Ca1 N1 97.40(6) . . ? N4 Ca1 N3 32.59(6) . . ? O1 Ca1 N3 114.80(6) . . ? O2 Ca1 N3 81.82(6) . . ? N2 Ca1 N3 119.71(6) . . ? O3 Ca1 N3 77.42(6) . . ? N1 Ca1 N3 151.53(6) . . ? N4 Ca1 O4 87.13(6) . . ? O1 Ca1 O4 81.94(5) . . ? O2 Ca1 O4 148.18(5) . . ? N2 Ca1 O4 110.70(6) . . ? O3 Ca1 O4 67.46(5) . . ? N1 Ca1 O4 91.69(6) . . ? N3 Ca1 O4 111.28(6) . . ? N4 Ca1 C19 105.92(6) . . ? O1 Ca1 C19 47.67(6) . . ? O2 Ca1 C19 25.05(6) . . ? N2 Ca1 C19 80.85(7) . . ? O3 Ca1 C19 160.21(6) . . ? N1 Ca1 C19 70.76(6) . . ? N3 Ca1 C19 105.18(6) . . ? O4 Ca1 C19 126.99(6) . . ? N4 Ca1 C23 74.02(6) . . ? O1 Ca1 C23 103.40(6) . . ? O2 Ca1 C23 162.16(6) . . ? N2 Ca1 C23 113.25(6) . . ? O3 Ca1 C23 46.77(6) . . ? N1 Ca1 C23 106.75(6) . . ? N3 Ca1 C23 90.19(6) . . ? O4 Ca1 C23 25.17(5) . . ? C19 Ca1 C23 150.78(6) . . ? C7 S1 C4 92.20(12) . . ? C15 S2 C12 92.53(12) . . ? C17 O1 C18 111.76(18) . . ? C17 O1 Ca1 123.63(14) . . ? C18 O1 Ca1 118.88(13) . . ? C20 O2 C19 112.84(18) . . ? C20 O2 Ca1 119.44(14) . . ? C19 O2 Ca1 108.94(12) . . ? C22 O3 C21 112.34(17) . . ? C22 O3 Ca1 119.52(13) . . ? C21 O3 Ca1 125.33(14) . . ? C24 O4 C23 112.61(17) . . ? C24 O4 Ca1 120.85(13) . . ? C23 O4 Ca1 107.68(12) . . ? C1 N1 N2 108.37(17) . . ? C1 N1 Ca1 177.05(15) . . ? N2 N1 Ca1 73.62(11) . . ? C9 N3 N4 108.31(17) . . ? C9 N3 Ca1 171.93(14) . . ? N4 N3 Ca1 71.88(10) . . ? C3 N2 N1 106.73(18) . . ? C3 N2 Ca1 177.78(16) . . ? N1 N2 Ca1 73.80(11) . . ? C11 N4 N3 107.04(17) . . ? C11 N4 Ca1 171.59(15) . . ? N3 N4 Ca1 75.53(11) . . ? N2 C3 C2 111.51(19) . . ? N2 C3 C8 120.7(2) . . ? C2 C3 C8 127.7(2) . . ? N4 C11 C10 111.54(19) . . ? N4 C11 C16 120.05(19) . . ? C10 C11 C16 128.4(2) . . ? O1 C18 C19 108.56(18) . . ? C3 C2 C1 103.57(19) . . ? C11 C10 C9 102.95(18) . . ? O2 C19 C18 107.44(19) . . ? O2 C19 Ca1 46.01(9) . . ? C18 C19 Ca1 82.62(13) . . ? N1 C1 C2 109.82(19) . . ? N1 C1 C4 121.60(19) . . ? C2 C1 C4 128.6(2) . . ? N3 C9 C10 110.15(18) . . ? N3 C9 C12 121.62(19) . . ? C10 C9 C12 128.18(19) . . ? F3 C8 F1 107.3(2) . . ? F3 C8 F2 105.7(2) . . ? F1 C8 F2 106.0(2) . . ? F3 C8 C3 113.4(2) . . ? F1 C8 C3 111.7(2) . . ? F2 C8 C3 112.3(2) . . ? F5 C16 F4 107.7(2) . . ? F5 C16 F6 104.6(2) . . ? F4 C16 F6 105.0(2) . . ? F5 C16 C11 113.6(2) . . ? F4 C16 C11 112.3(2) . . ? F6 C16 C11 113.0(2) . . ? C5 C4 C1 126.77(19) . . ? C5 C4 S1 111.80(16) . . ? C1 C4 S1 121.40(16) . . ? C9 C12 C13 125.86(19) . . ? C9 C12 S2 121.25(16) . . ? C13 C12 S2 112.89(15) . . ? O3 C22 C23 106.87(17) . . ? C4 C5 C6 109.90(19) . . ? C14 C13 C12 105.89(19) . . ? O4 C23 C22 111.15(18) . . ? O4 C23 Ca1 47.15(9) . . ? C22 C23 Ca1 82.67(12) . . ? C7 C6 C5 113.8(2) . . ? C15 C14 C13 115.7(2) . . ? C6 C7 S1 112.33(19) . . ? C14 C15 S2 112.97(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.277 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.075 #===END data_compound6 _database_code_depnum_ccdc_archive 'CCDC 794843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Sr(ttfpz)2(dme)2] ; _chemical_name_common (Sr(ttfpz)2(dme)2) _chemical_melting_point ? _chemical_formula_moiety ; C24 H28 F6 N4 O4 S2 Sr ; _chemical_formula_sum 'C24 H28 F6 N4 O4 S2 Sr' _chemical_formula_weight 702.24 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' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 7.9180(16) _cell_length_b 19.131(4) _cell_length_c 19.896(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.82(3) _cell_angle_gamma 90.00 _cell_volume 2978.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 13014 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour coulourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 2.025 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5376 _exptl_absorpt_correction_T_max 0.8630 _exptl_absorpt_process_details SADABS _exptl_special_details ; The data set showed twinning. Initial indexing for the two components of the twin was carried out using CELL NOW within the APEX2 software package. Multi-component integration was carried out using SAINT+. Scaling and empirical absorption corrections were then applied using TWINABS. The structure was solved as above using a HKLF 5 command with a resulting BASF parameter of 0.318. ; _diffrn_ambient_temperature 173(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13014 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1715 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.55 _reflns_number_total 13019 _reflns_number_gt 8145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13019 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1598 _refine_ls_R_factor_gt 0.0983 _refine_ls_wR_factor_ref 0.2119 _refine_ls_wR_factor_gt 0.1889 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.51837(7) 0.08082(3) 0.30296(2) 0.01748(14) Uani 1 1 d . . . S1 S 0.3198(2) 0.25417(9) 0.44107(8) 0.0374(5) Uani 1 1 d . . . S2 S 0.7070(2) 0.01164(10) 0.10176(8) 0.0371(4) Uani 1 1 d . . . F1 F 0.2695(8) 0.2905(3) 0.0922(2) 0.101(2) Uani 1 1 d . . . F2 F 0.1189(7) 0.1984(3) 0.0952(2) 0.0854(17) Uani 1 1 d . . . F3 F 0.3854(6) 0.1900(3) 0.0977(2) 0.0689(15) Uani 1 1 d . . . F4 F 0.8042(9) -0.2000(3) 0.3864(3) 0.120(3) Uani 1 1 d . . . F5 F 0.6242(7) -0.1340(4) 0.4167(3) 0.123(3) Uani 1 1 d . . . F6 F 0.8794(8) -0.1082(3) 0.4361(2) 0.102(2) Uani 1 1 d . . . O1 O 0.6635(5) 0.1213(2) 0.4197(2) 0.0298(10) Uani 1 1 d . . . O2 O 0.8015(5) 0.1487(2) 0.3072(2) 0.0302(10) Uani 1 1 d . . . O3 O 0.2763(5) 0.0135(2) 0.23066(19) 0.0292(10) Uani 1 1 d . . . O4 O 0.2976(5) 0.0232(2) 0.37048(19) 0.0246(10) Uani 1 1 d . . . N1 N 0.3660(6) 0.2005(3) 0.3001(2) 0.0256(12) Uani 1 1 d . . . N2 N 0.3758(7) 0.1841(3) 0.2338(2) 0.0279(12) Uani 1 1 d . . . N3 N 0.6830(6) -0.0160(2) 0.2506(2) 0.0195(10) Uani 1 1 d . . . N4 N 0.6779(6) -0.0360(3) 0.3162(2) 0.0226(11) Uani 1 1 d . . . C1 C 0.2727(7) 0.2599(3) 0.3010(3) 0.0240(14) Uani 1 1 d . . . C2 C 0.2221(7) 0.2820(3) 0.2344(3) 0.0253(14) Uani 1 1 d . . . H2 H 0.1554 0.3219 0.2192 0.030 Uiso 1 1 calc R . . C3 C 0.2895(8) 0.2337(3) 0.1955(3) 0.0296(15) Uani 1 1 d . . . C4 C 0.2332(7) 0.2892(3) 0.3632(3) 0.0222(13) Uani 1 1 d . . . C5 C 0.1267(7) 0.3439(3) 0.3721(3) 0.0278(15) Uani 1 1 d . . . H5 H 0.0692 0.3713 0.3358 0.033 Uiso 1 1 calc R . . C6 C 0.1122(8) 0.3547(4) 0.4408(3) 0.0381(17) Uani 1 1 d . . . H6 H 0.0407 0.3896 0.4556 0.046 Uiso 1 1 calc R . . C7 C 0.2092(9) 0.3111(4) 0.4837(3) 0.0422(18) Uani 1 1 d . . . H7 H 0.2153 0.3121 0.5317 0.051 Uiso 1 1 calc R . . C8 C 0.2685(11) 0.2275(4) 0.1208(3) 0.0463(19) Uani 1 1 d . . . C9 C 0.7535(6) -0.0675(3) 0.2194(3) 0.0161(12) Uani 1 1 d . . . C10 C 0.7972(7) -0.1229(3) 0.2641(3) 0.0255(14) Uani 1 1 d . . . H10 H 0.8486 -0.1662 0.2555 0.031 Uiso 1 1 calc R . . C11 C 0.7482(7) -0.0999(3) 0.3239(3) 0.0219(13) Uani 1 1 d . . . C12 C 0.7789(7) -0.0611(3) 0.1483(3) 0.0205(13) Uani 1 1 d . . . C13 C 0.8612(7) -0.1073(3) 0.1101(3) 0.0235(14) Uani 1 1 d . . . H13 H 0.9099 -0.1507 0.1263 0.028 Uiso 1 1 calc R . . C14 C 0.8623(8) -0.0805(4) 0.0434(3) 0.0388(17) Uani 1 1 d . . . H14 H 0.9117 -0.1049 0.0096 0.047 Uiso 1 1 calc R . . C15 C 0.7872(9) -0.0176(4) 0.0325(3) 0.0428(19) Uani 1 1 d . . . H15 H 0.7799 0.0075 -0.0091 0.051 Uiso 1 1 calc R . . C16 C 0.7633(9) -0.1347(4) 0.3896(3) 0.0360(17) Uani 1 1 d . . . C17 C 0.6584(10) 0.0811(4) 0.4802(3) 0.062(2) Uani 1 1 d . . . H17A H 0.7675 0.0568 0.4929 0.093 Uiso 1 1 calc R . . H17B H 0.5657 0.0468 0.4718 0.093 Uiso 1 1 calc R . . H17C H 0.6385 0.1123 0.5172 0.093 Uiso 1 1 calc R . . C18 C 0.8015(8) 0.1695(4) 0.4242(3) 0.0423(19) Uani 1 1 d . . . H18A H 0.9108 0.1446 0.4387 0.051 Uiso 1 1 calc R . . H18B H 0.7886 0.2056 0.4587 0.051 Uiso 1 1 calc R . . C19 C 0.8041(9) 0.2030(3) 0.3575(3) 0.0403(18) Uani 1 1 d . . . H19A H 0.7033 0.2338 0.3460 0.048 Uiso 1 1 calc R . . H19B H 0.9085 0.2318 0.3589 0.048 Uiso 1 1 calc R . . C20 C 0.8440(10) 0.1735(4) 0.2447(3) 0.048(2) Uani 1 1 d . . . H20A H 0.7637 0.2103 0.2266 0.073 Uiso 1 1 calc R . . H20B H 0.8374 0.1348 0.2120 0.073 Uiso 1 1 calc R . . H20C H 0.9605 0.1924 0.2522 0.073 Uiso 1 1 calc R . . C21 C 0.2189(8) 0.0257(4) 0.1608(3) 0.0369(17) Uani 1 1 d . . . H21A H 0.1968 -0.0191 0.1372 0.055 Uiso 1 1 calc R . . H21B H 0.3067 0.0514 0.1412 0.055 Uiso 1 1 calc R . . H21C H 0.1133 0.0533 0.1556 0.055 Uiso 1 1 calc R . . C22 C 0.1580(7) -0.0245(4) 0.2632(3) 0.0347(17) Uani 1 1 d . . . H22A H 0.1276 -0.0688 0.2386 0.042 Uiso 1 1 calc R . . H22B H 0.0523 0.0032 0.2630 0.042 Uiso 1 1 calc R . . C23 C 0.2371(8) -0.0394(3) 0.3342(3) 0.0304(15) Uani 1 1 d . . . H23A H 0.1520 -0.0626 0.3583 0.036 Uiso 1 1 calc R . . H23B H 0.3340 -0.0720 0.3338 0.036 Uiso 1 1 calc R . . C24 C 0.1620(9) 0.0628(4) 0.3916(4) 0.0442(19) Uani 1 1 d . . . H24A H 0.0874 0.0808 0.3514 0.066 Uiso 1 1 calc R . . H24B H 0.2098 0.1020 0.4200 0.066 Uiso 1 1 calc R . . H24C H 0.0956 0.0327 0.4177 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr1 0.0153(2) 0.0183(3) 0.0185(2) -0.0021(3) 0.0016(2) 0.0004(2) S1 0.0518(12) 0.0302(10) 0.0297(9) 0.0027(8) 0.0047(8) 0.0107(8) S2 0.0465(11) 0.0387(11) 0.0278(9) 0.0043(8) 0.0108(8) 0.0082(8) F1 0.219(7) 0.052(3) 0.033(3) 0.024(2) 0.019(3) 0.008(4) F2 0.085(4) 0.124(5) 0.038(3) -0.016(3) -0.021(3) -0.008(4) F3 0.094(4) 0.083(4) 0.034(2) -0.004(2) 0.022(2) 0.018(3) F4 0.256(9) 0.048(3) 0.062(3) 0.028(3) 0.039(4) 0.051(4) F5 0.066(4) 0.220(7) 0.092(4) 0.109(5) 0.041(3) 0.028(4) F6 0.139(5) 0.121(5) 0.031(3) 0.029(3) -0.034(3) -0.046(4) O1 0.034(3) 0.030(3) 0.023(2) -0.0012(19) -0.0018(19) -0.004(2) O2 0.030(2) 0.030(3) 0.032(2) -0.006(2) 0.010(2) -0.011(2) O3 0.020(2) 0.043(3) 0.022(2) -0.003(2) -0.0070(18) -0.011(2) O4 0.023(2) 0.025(2) 0.028(2) -0.0052(19) 0.0107(18) -0.0015(18) N1 0.025(3) 0.027(3) 0.025(3) 0.003(2) 0.003(2) 0.008(2) N2 0.037(3) 0.023(3) 0.024(3) 0.001(2) 0.006(2) 0.000(3) N3 0.021(3) 0.019(3) 0.019(2) 0.001(2) 0.004(2) 0.004(2) N4 0.021(3) 0.026(3) 0.019(3) 0.001(2) -0.001(2) 0.000(2) C1 0.021(3) 0.019(3) 0.031(3) 0.006(3) -0.001(3) -0.004(2) C2 0.029(4) 0.022(3) 0.023(3) 0.007(3) 0.001(3) 0.002(3) C3 0.043(4) 0.025(4) 0.020(3) 0.005(3) -0.001(3) -0.009(3) C4 0.017(3) 0.018(3) 0.030(3) 0.002(3) -0.001(3) -0.008(3) C5 0.015(3) 0.022(4) 0.046(4) -0.003(3) 0.002(3) -0.002(3) C6 0.036(4) 0.032(4) 0.050(4) -0.011(4) 0.016(3) 0.002(3) C7 0.060(5) 0.037(4) 0.033(4) -0.006(3) 0.016(4) 0.002(4) C8 0.074(6) 0.033(4) 0.031(4) 0.009(3) 0.006(4) 0.001(4) C9 0.015(3) 0.014(3) 0.018(3) -0.004(2) -0.001(2) -0.002(2) C10 0.023(3) 0.025(4) 0.031(3) -0.004(3) 0.013(3) 0.000(3) C11 0.021(3) 0.021(3) 0.023(3) 0.001(2) 0.000(2) 0.001(3) C12 0.019(3) 0.018(3) 0.024(3) -0.002(2) 0.004(3) -0.004(2) C13 0.021(3) 0.028(4) 0.024(3) -0.004(3) 0.011(3) -0.006(3) C14 0.044(4) 0.045(5) 0.028(4) -0.020(4) 0.009(3) -0.008(4) C15 0.061(5) 0.046(5) 0.025(4) 0.002(3) 0.018(3) -0.004(4) C16 0.041(4) 0.045(5) 0.024(3) 0.007(3) 0.011(3) 0.005(4) C17 0.076(6) 0.083(7) 0.023(4) 0.003(4) -0.002(4) -0.018(5) C18 0.024(4) 0.052(5) 0.049(5) -0.026(4) 0.001(3) -0.006(3) C19 0.046(5) 0.025(4) 0.051(5) -0.012(3) 0.011(4) -0.015(3) C20 0.053(5) 0.048(5) 0.047(5) 0.012(4) 0.019(4) -0.011(4) C21 0.039(4) 0.045(5) 0.024(4) -0.001(3) -0.003(3) -0.014(3) C22 0.019(4) 0.037(4) 0.046(4) 0.001(3) -0.002(3) -0.006(3) C23 0.032(4) 0.021(4) 0.038(4) -0.001(3) 0.007(3) -0.010(3) C24 0.037(4) 0.051(5) 0.047(4) -0.001(4) 0.015(4) 0.001(4) _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 Sr1 O1 2.549(4) . ? Sr1 O3 2.560(4) . ? Sr1 N4 2.562(5) . ? Sr1 N2 2.568(5) . ? Sr1 N3 2.574(5) . ? Sr1 O2 2.581(4) . ? Sr1 N1 2.584(5) . ? Sr1 O4 2.606(4) . ? S1 C7 1.703(7) . ? S1 C4 1.730(6) . ? S2 C15 1.699(7) . ? S2 C12 1.719(6) . ? F1 C8 1.333(8) . ? F2 C8 1.337(9) . ? F3 C8 1.308(8) . ? F4 C16 1.295(8) . ? F5 C16 1.298(7) . ? F6 C16 1.302(8) . ? O1 C18 1.421(7) . ? O1 C17 1.433(7) . ? O2 C20 1.420(7) . ? O2 C19 1.440(7) . ? O3 C21 1.414(6) . ? O3 C22 1.418(7) . ? O4 C24 1.428(7) . ? O4 C23 1.443(7) . ? N1 C1 1.358(7) . ? N1 N2 1.369(6) . ? N2 C3 1.337(7) . ? N3 C9 1.333(6) . ? N3 N4 1.367(6) . ? N4 C11 1.341(7) . ? C1 C2 1.390(8) . ? C1 C4 1.437(8) . ? C2 C3 1.366(8) . ? C3 C8 1.474(9) . ? C4 C5 1.373(8) . ? C5 C6 1.404(9) . ? C6 C7 1.347(9) . ? C9 C10 1.392(8) . ? C9 C12 1.465(7) . ? C10 C11 1.377(8) . ? C11 C16 1.457(8) . ? C12 C13 1.391(8) . ? C13 C14 1.425(8) . ? C14 C15 1.346(9) . ? C18 C19 1.478(9) . ? C22 C23 1.482(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 O1 Sr1 O3 149.18(13) . . ? O1 Sr1 N4 91.44(14) . . ? O3 Sr1 N4 86.19(14) . . ? O1 Sr1 N2 110.75(14) . . ? O3 Sr1 N2 81.74(15) . . ? N4 Sr1 N2 153.63(15) . . ? O1 Sr1 N3 113.68(14) . . ? O3 Sr1 N3 78.04(14) . . ? N4 Sr1 N3 30.86(13) . . ? N2 Sr1 N3 123.02(15) . . ? O1 Sr1 O2 63.20(13) . . ? O3 Sr1 O2 147.49(13) . . ? N4 Sr1 O2 91.36(14) . . ? N2 Sr1 O2 86.49(15) . . ? N3 Sr1 O2 83.35(14) . . ? O1 Sr1 N1 83.95(14) . . ? O3 Sr1 N1 97.27(14) . . ? N4 Sr1 N1 175.30(15) . . ? N2 Sr1 N1 30.82(14) . . ? N3 Sr1 N1 153.10(15) . . ? O2 Sr1 N1 87.43(14) . . ? O1 Sr1 O4 84.43(13) . . ? O3 Sr1 O4 64.76(12) . . ? N4 Sr1 O4 86.40(14) . . ? N2 Sr1 O4 109.07(14) . . ? N3 Sr1 O4 109.01(14) . . ? O2 Sr1 O4 147.50(12) . . ? N1 Sr1 O4 92.18(14) . . ? C7 S1 C4 92.0(3) . . ? C15 S2 C12 92.1(3) . . ? C18 O1 C17 114.5(5) . . ? C18 O1 Sr1 119.3(4) . . ? C17 O1 Sr1 122.4(4) . . ? C20 O2 C19 112.8(5) . . ? C20 O2 Sr1 117.4(4) . . ? C19 O2 Sr1 107.8(3) . . ? C21 O3 C22 113.5(4) . . ? C21 O3 Sr1 124.7(4) . . ? C22 O3 Sr1 119.4(3) . . ? C24 O4 C23 112.3(5) . . ? C24 O4 Sr1 121.4(4) . . ? C23 O4 Sr1 106.9(3) . . ? C1 N1 N2 108.3(5) . . ? C1 N1 Sr1 174.2(4) . . ? N2 N1 Sr1 73.9(3) . . ? C3 N2 N1 106.8(5) . . ? C3 N2 Sr1 174.5(4) . . ? N1 N2 Sr1 75.2(3) . . ? C9 N3 N4 108.1(4) . . ? C9 N3 Sr1 174.2(4) . . ? N4 N3 Sr1 74.0(3) . . ? C11 N4 N3 107.0(4) . . ? C11 N4 Sr1 174.9(4) . . ? N3 N4 Sr1 75.1(3) . . ? N1 C1 C2 108.7(5) . . ? N1 C1 C4 121.8(5) . . ? C2 C1 C4 129.4(6) . . ? C3 C2 C1 104.7(5) . . ? N2 C3 C2 111.5(5) . . ? N2 C3 C8 119.2(6) . . ? C2 C3 C8 129.2(6) . . ? C5 C4 C1 128.8(5) . . ? C5 C4 S1 110.3(5) . . ? C1 C4 S1 120.8(4) . . ? C4 C5 C6 112.4(6) . . ? C7 C6 C5 113.7(6) . . ? C6 C7 S1 111.6(5) . . ? F3 C8 F1 107.1(7) . . ? F3 C8 F2 105.8(6) . . ? F1 C8 F2 106.0(7) . . ? F3 C8 C3 115.0(6) . . ? F1 C8 C3 110.6(6) . . ? F2 C8 C3 111.9(6) . . ? N3 C9 C10 110.3(5) . . ? N3 C9 C12 121.1(5) . . ? C10 C9 C12 128.6(5) . . ? C11 C10 C9 103.5(5) . . ? N4 C11 C10 111.1(5) . . ? N4 C11 C16 119.6(5) . . ? C10 C11 C16 129.3(6) . . ? C13 C12 C9 128.3(5) . . ? C13 C12 S2 111.4(4) . . ? C9 C12 S2 120.3(4) . . ? C12 C13 C14 110.5(6) . . ? C15 C14 C13 114.0(6) . . ? C14 C15 S2 112.0(5) . . ? F4 C16 F5 105.4(7) . . ? F4 C16 F6 104.8(6) . . ? F5 C16 F6 104.7(6) . . ? F4 C16 C11 112.6(6) . . ? F5 C16 C11 114.2(6) . . ? F6 C16 C11 114.3(6) . . ? O1 C18 C19 110.0(5) . . ? O2 C19 C18 108.0(5) . . ? O3 C22 C23 108.8(5) . . ? O4 C23 C22 112.1(5) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.708 _refine_diff_density_min -1.488 _refine_diff_density_rms 0.163 #===END data_compound7 _database_code_depnum_ccdc_archive 'CCDC 794844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Yb(ttfpz)2(dme)2] ; _chemical_name_common (Yb(ttfpz)2(dme)2) _chemical_melting_point ? _chemical_formula_moiety 'C24 H28 F6 N4 O4 S2 Yb' _chemical_formula_sum 'C24 H28 F6 N4 O4 S2 Yb' _chemical_formula_weight 787.66 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 11.4592(4) _cell_length_b 13.7915(5) _cell_length_c 18.5391(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.903(2) _cell_angle_gamma 90.00 _cell_volume 2929.55(18) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 71741 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 3.410 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1988 _exptl_absorpt_correction_T_max 0.4277 _exptl_absorpt_process_details SADABS _exptl_special_details ; Thiophene group S(2) was disordered over two positions, its occupancy was freely refined to be 80:20. The disordered part of that disorder was restrained using DFIX and DANG commands. Atoms C(13A), C(14A) and C(15A) were restrained using SIMU. Dme-oxygen atom O(3) and neighbouring C-atoms were disordered over two positions, their occupancy was freely refined to be appr. 55:45. Also, DFIX was used to restraint the distance between C(23A) and O(4). EADP C6 C5 was also applied. ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71741 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6715 _reflns_number_gt 6512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6715 _refine_ls_number_parameters 443 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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 Yb1 Yb 0.352727(10) 0.482376(8) 0.176162(6) 0.01388(4) Uani 1 1 d . . . S1 S 0.14825(8) 0.68241(8) 0.02346(5) 0.0395(2) Uani 1 1 d . B . S2 S 0.35610(13) 0.55942(14) 0.41271(10) 0.0285(5) Uani 0.793(5) 1 d P A 1 F1 F 0.64242(19) 0.83897(15) 0.20426(13) 0.0417(5) Uani 1 1 d . . . F2 F 0.7170(2) 0.7068(2) 0.17277(19) 0.0772(10) Uani 1 1 d . . . F3 F 0.6172(3) 0.7133(2) 0.26792(14) 0.0764(11) Uani 1 1 d . . . F4 F -0.16110(17) 0.52803(18) 0.21478(13) 0.0437(6) Uani 1 1 d . . . F5 F -0.0577(2) 0.4475(2) 0.14173(16) 0.0626(8) Uani 1 1 d . . . F6 F -0.06082(18) 0.60252(19) 0.13660(12) 0.0448(6) Uani 1 1 d . . . O1 O 0.30628(18) 0.31425(15) 0.21835(11) 0.0207(4) Uani 1 1 d . B . O2 O 0.48393(17) 0.42456(15) 0.27546(11) 0.0211(4) Uani 1 1 d . B . O3 O 0.5146(8) 0.3875(7) 0.1214(7) 0.0185(17) Uani 0.55(4) 1 d P B 3 O4 O 0.2862(2) 0.39822(18) 0.06417(11) 0.0291(5) Uani 1 1 d D B . N1 N 0.3696(2) 0.63790(18) 0.11493(13) 0.0196(5) Uani 1 1 d . B . N2 N 0.4648(2) 0.63477(18) 0.16028(13) 0.0201(5) Uani 1 1 d . B . N3 N 0.2210(2) 0.52896(17) 0.27184(12) 0.0162(5) Uani 1 1 d . B . N4 N 0.1499(2) 0.51873(17) 0.21241(13) 0.0174(5) Uani 1 1 d . B . C1 C 0.3620(2) 0.7276(2) 0.08653(14) 0.0179(5) Uani 1 1 d . . . C2 C 0.4538(2) 0.7847(2) 0.11242(15) 0.0192(5) Uani 1 1 d . B . H2 H 0.4706 0.8504 0.1013 0.023 Uiso 1 1 calc R . . C3 C 0.5147(2) 0.7230(2) 0.15819(15) 0.0193(5) Uani 1 1 d . . . C4 C 0.2693(2) 0.7537(2) 0.03554(15) 0.0189(5) Uani 1 1 d . B . C5 C 0.2716(3) 0.8389(2) -0.01442(16) 0.0251(5) Uani 1 1 d . . . H5 H 0.3308 0.8867 -0.0188 0.030 Uiso 1 1 calc R B . C6 C 0.1604(3) 0.8313(2) -0.05524(16) 0.0251(5) Uani 1 1 d . B . H6 H 0.1377 0.8786 -0.0900 0.030 Uiso 1 1 calc R . . C7 C 0.0930(3) 0.7546(3) -0.0411(2) 0.0387(8) Uani 1 1 d . . . H7 H 0.0208 0.7424 -0.0653 0.046 Uiso 1 1 calc R B . C8 C 0.6212(3) 0.7447(2) 0.20115(18) 0.0284(7) Uani 1 1 d . B . C9 C 0.1540(2) 0.5479(2) 0.32918(15) 0.0175(5) Uani 1 1 d . . . C10 C 0.0366(2) 0.5509(2) 0.30774(16) 0.0214(6) Uani 1 1 d . B . H10 H -0.0296 0.5631 0.3365 0.026 Uiso 1 1 calc R . . C11 C 0.0401(2) 0.5318(2) 0.23455(16) 0.0196(6) Uani 1 1 d . . . C12 C 0.2059(2) 0.5628(2) 0.40014(15) 0.0190(5) Uani 1 1 d D A . C13 C 0.1548(6) 0.5824(7) 0.4643(5) 0.0307(18) Uani 0.793(5) 1 d P A 1 H13 H 0.0727 0.5885 0.4695 0.037 Uiso 0.793(5) 1 calc PR A 1 C14 C 0.2354(8) 0.593(2) 0.5225(5) 0.0342(19) Uani 0.793(5) 1 d P A 1 H14 H 0.2131 0.6054 0.5708 0.041 Uiso 0.793(5) 1 calc PR A 1 C15 C 0.3468(7) 0.5841(17) 0.5020(5) 0.032(2) Uani 0.793(5) 1 d P A 1 H15 H 0.4123 0.5907 0.5336 0.039 Uiso 0.793(5) 1 calc PR A 1 C16 C -0.0583(3) 0.5270(2) 0.18220(19) 0.0287(7) Uani 1 1 d . B . C17 C 0.1892(3) 0.2806(2) 0.20791(19) 0.0284(7) Uani 1 1 d . . . H17A H 0.1850 0.2116 0.2201 0.043 Uiso 1 1 calc R B . H17B H 0.1654 0.2900 0.1574 0.043 Uiso 1 1 calc R . . H17C H 0.1370 0.3173 0.2391 0.043 Uiso 1 1 calc R . . C18 C 0.3477(3) 0.2968(2) 0.29004(16) 0.0256(6) Uani 1 1 d . . . H18A H 0.3384 0.2274 0.3023 0.031 Uiso 1 1 calc R B . H18B H 0.3022 0.3356 0.3246 0.031 Uiso 1 1 calc R . . C19 C 0.4736(3) 0.3246(2) 0.29471(18) 0.0269(7) Uani 1 1 d . B . H19A H 0.5040 0.3143 0.3444 0.032 Uiso 1 1 calc R . . H19B H 0.5196 0.2841 0.2615 0.032 Uiso 1 1 calc R . . C20 C 0.5982(3) 0.4605(3) 0.2878(2) 0.0374(9) Uani 1 1 d . . . H20A H 0.6172 0.4572 0.3395 0.056 Uiso 1 1 calc R B . H20B H 0.6024 0.5280 0.2716 0.056 Uiso 1 1 calc R . . H20C H 0.6540 0.4212 0.2610 0.056 Uiso 1 1 calc R . . C21 C 0.6208(11) 0.4240(10) 0.0897(7) 0.029(2) Uani 0.55(4) 1 d P B 3 H21A H 0.6833 0.3761 0.0960 0.043 Uiso 0.55(4) 1 calc PR B 3 H21B H 0.6436 0.4847 0.1135 0.043 Uiso 0.55(4) 1 calc PR B 3 H21C H 0.6074 0.4360 0.0381 0.043 Uiso 0.55(4) 1 calc PR B 3 C22 C 0.4673(16) 0.3076(10) 0.0817(7) 0.020(2) Uani 0.55(4) 1 d P B 3 H22A H 0.4315 0.2609 0.1154 0.024 Uiso 0.55(4) 1 calc PR B 3 H22B H 0.5307 0.2738 0.0562 0.024 Uiso 0.55(4) 1 calc PR B 3 C23 C 0.3771(17) 0.3420(10) 0.0282(8) 0.024(3) Uani 0.55(4) 1 d P B 3 H23A H 0.4148 0.3827 -0.0087 0.028 Uiso 0.55(4) 1 calc PR B 3 H23B H 0.3413 0.2854 0.0035 0.028 Uiso 0.55(4) 1 calc PR B 3 C24 C 0.1837(4) 0.4184(3) 0.0232(2) 0.0454(10) Uani 1 1 d . . . H24A H 0.2027 0.4619 -0.0167 0.068 Uiso 1 1 calc R B . H24B H 0.1261 0.4496 0.0541 0.068 Uiso 1 1 calc R . . H24C H 0.1513 0.3578 0.0040 0.068 Uiso 1 1 calc R . . C13A C 0.3294(10) 0.577(2) 0.4195(12) 0.032(6) Uani 0.207(5) 1 d PDU A 2 H13A H 0.3942 0.5782 0.3881 0.038 Uiso 0.207(5) 1 calc PR A 2 S2A S 0.1156(6) 0.5780(7) 0.4717(4) 0.0262(16) Uani 0.207(5) 1 d PDU A 2 C14A C 0.331(2) 0.589(7) 0.4979(15) 0.030(6) Uani 0.207(5) 1 d PDU A 2 H14A H 0.4016 0.5922 0.5250 0.036 Uiso 0.207(5) 1 calc PR A 2 C15A C 0.2274(19) 0.597(9) 0.5298(15) 0.024(5) Uani 0.207(5) 1 d PDU A 2 H15A H 0.2182 0.6110 0.5795 0.029 Uiso 0.207(5) 1 calc PR A 2 O3A O 0.5066(12) 0.4091(15) 0.0991(11) 0.034(3) Uani 0.45(4) 1 d P B 4 C23A C 0.364(3) 0.358(2) 0.0147(15) 0.057(8) Uani 0.45(4) 1 d PD B 4 H23C H 0.3905 0.4066 -0.0204 0.068 Uiso 0.45(4) 1 calc PR B 4 H23D H 0.3272 0.3028 -0.0118 0.068 Uiso 0.45(4) 1 calc PR B 4 C22A C 0.460(2) 0.324(2) 0.0610(15) 0.050(6) Uani 0.45(4) 1 d P B 4 H22C H 0.5212 0.2939 0.0317 0.060 Uiso 0.45(4) 1 calc PR B 4 H22D H 0.4314 0.2758 0.0960 0.060 Uiso 0.45(4) 1 calc PR B 4 C21A C 0.6226(15) 0.4040(19) 0.1165(17) 0.052(5) Uani 0.45(4) 1 d P B 4 H21D H 0.6369 0.3481 0.1480 0.078 Uiso 0.45(4) 1 calc PR B 4 H21E H 0.6465 0.4635 0.1415 0.078 Uiso 0.45(4) 1 calc PR B 4 H21F H 0.6678 0.3968 0.0723 0.078 Uiso 0.45(4) 1 calc PR B 4 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 Yb1 0.01494(6) 0.01525(7) 0.01148(6) -0.00094(4) 0.00142(4) -0.00121(4) S1 0.0317(4) 0.0509(6) 0.0360(5) 0.0027(4) -0.0014(4) -0.0035(4) S2 0.0249(6) 0.0429(11) 0.0176(7) -0.0026(5) -0.0027(5) -0.0007(7) F1 0.0383(12) 0.0284(11) 0.0579(14) 0.0017(10) -0.0177(10) -0.0120(9) F2 0.0285(13) 0.088(2) 0.114(3) -0.049(2) -0.0264(14) 0.0255(13) F3 0.097(2) 0.088(2) 0.0432(14) 0.0349(14) -0.0444(15) -0.0580(18) F4 0.0138(9) 0.0660(16) 0.0513(14) 0.0140(11) -0.0031(9) -0.0041(9) F5 0.0433(14) 0.0636(17) 0.0796(19) -0.0419(15) -0.0337(13) 0.0107(12) F6 0.0307(11) 0.0662(16) 0.0370(12) 0.0217(11) -0.0135(9) -0.0091(10) O1 0.0213(10) 0.0190(10) 0.0218(10) 0.0034(8) 0.0024(8) -0.0034(8) O2 0.0176(10) 0.0213(11) 0.0244(10) 0.0034(8) -0.0017(8) 0.0007(8) O3 0.019(2) 0.025(3) 0.012(4) -0.005(2) 0.007(3) -0.002(2) O4 0.0370(13) 0.0339(13) 0.0163(10) -0.0053(9) -0.0019(9) -0.0083(10) N1 0.0211(12) 0.0213(12) 0.0164(11) 0.0027(9) 0.0004(9) -0.0014(9) N2 0.0201(12) 0.0216(12) 0.0185(11) 0.0012(9) -0.0007(9) -0.0032(9) N3 0.0155(11) 0.0175(12) 0.0156(11) -0.0018(9) -0.0009(9) 0.0012(9) N4 0.0148(11) 0.0188(12) 0.0185(11) -0.0020(9) -0.0024(9) 0.0006(9) C1 0.0189(13) 0.0209(14) 0.0141(12) 0.0000(10) 0.0045(10) -0.0001(11) C2 0.0206(13) 0.0190(14) 0.0181(13) 0.0010(10) 0.0025(10) -0.0015(11) C3 0.0207(14) 0.0188(14) 0.0185(13) 0.0001(11) 0.0028(11) -0.0011(11) C4 0.0200(13) 0.0197(14) 0.0170(13) -0.0032(10) 0.0017(10) 0.0006(11) C5 0.0304(12) 0.0214(11) 0.0232(10) -0.0029(8) -0.0156(9) 0.0104(9) C6 0.0304(12) 0.0214(11) 0.0232(10) -0.0029(8) -0.0156(9) 0.0104(9) C7 0.0334(19) 0.040(2) 0.042(2) -0.0101(16) -0.0131(15) 0.0059(16) C8 0.0288(16) 0.0238(16) 0.0323(17) 0.0029(13) -0.0065(13) -0.0019(13) C9 0.0179(13) 0.0157(13) 0.0188(13) -0.0001(10) 0.0032(10) 0.0005(10) C10 0.0153(13) 0.0238(15) 0.0251(14) 0.0003(12) 0.0034(11) 0.0014(11) C11 0.0151(13) 0.0181(14) 0.0256(15) 0.0001(11) -0.0020(11) -0.0003(10) C12 0.0217(14) 0.0175(14) 0.0177(13) 0.0013(10) 0.0010(11) 0.0018(11) C13 0.030(4) 0.038(3) 0.024(3) 0.003(2) 0.007(3) 0.011(4) C14 0.054(4) 0.032(4) 0.016(3) -0.003(4) 0.002(3) 0.011(4) C15 0.039(3) 0.033(5) 0.023(3) 0.003(3) -0.008(2) 0.001(4) C16 0.0187(15) 0.0325(18) 0.0347(18) -0.0005(14) -0.0047(13) -0.0012(12) C17 0.0246(15) 0.0223(15) 0.0384(18) 0.0038(13) 0.0008(13) -0.0071(12) C18 0.0309(16) 0.0230(15) 0.0228(15) 0.0078(12) 0.0023(12) -0.0018(12) C19 0.0310(16) 0.0227(16) 0.0268(16) 0.0086(12) -0.0038(13) 0.0025(13) C20 0.0269(17) 0.043(2) 0.042(2) 0.0142(16) -0.0161(15) -0.0099(15) C21 0.026(4) 0.036(5) 0.024(5) -0.007(4) 0.016(4) -0.007(3) C22 0.026(4) 0.022(4) 0.012(5) -0.010(3) 0.006(4) 0.004(3) C23 0.045(6) 0.019(4) 0.007(5) -0.006(3) 0.003(5) -0.003(3) C24 0.051(2) 0.056(3) 0.0289(18) 0.0051(17) -0.0166(17) -0.019(2) C13A 0.053(12) 0.035(10) 0.007(7) -0.005(6) 0.006(8) 0.025(9) S2A 0.030(4) 0.034(3) 0.015(2) -0.0005(18) 0.005(2) 0.011(3) C14A 0.043(10) 0.031(9) 0.017(8) 0.001(8) -0.004(8) 0.014(9) C15A 0.030(8) 0.029(8) 0.014(7) -0.004(7) 0.002(7) 0.013(7) O3A 0.033(4) 0.047(7) 0.023(6) -0.014(5) 0.012(4) -0.007(4) C23A 0.062(12) 0.097(18) 0.012(8) -0.013(9) 0.006(7) -0.024(11) C22A 0.045(9) 0.073(15) 0.033(12) -0.035(9) 0.013(10) -0.013(9) C21A 0.031(6) 0.068(11) 0.058(12) -0.027(9) 0.026(8) -0.004(7) _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 Yb1 N3 2.434(2) . ? Yb1 N1 2.436(2) . ? Yb1 N4 2.481(2) . ? Yb1 N2 2.483(2) . ? Yb1 O4 2.488(2) . ? Yb1 O2 2.490(2) . ? Yb1 O3 2.498(9) . ? Yb1 O3A 2.500(12) . ? Yb1 O1 2.507(2) . ? S1 C7 1.674(4) . ? S1 C4 1.712(3) . ? S2 C15 1.695(7) . ? S2 C12 1.734(3) . ? F1 C8 1.324(4) . ? F2 C8 1.331(4) . ? F3 C8 1.313(4) . ? F4 C16 1.333(4) . ? F5 C16 1.329(4) . ? F6 C16 1.342(4) . ? O1 C18 1.425(4) . ? O1 C17 1.430(4) . ? O2 C20 1.415(4) . ? O2 C19 1.429(4) . ? O3 C22 1.43(2) . ? O3 C21 1.451(18) . ? O4 C23A 1.404(17) . ? O4 C24 1.416(4) . ? O4 C23 1.468(13) . ? N1 C1 1.346(4) . ? N1 N2 1.368(3) . ? N2 C3 1.346(4) . ? N3 C9 1.346(3) . ? N3 N4 1.367(3) . ? N4 C11 1.342(4) . ? C1 C2 1.393(4) . ? C1 C4 1.456(4) . ? C2 C3 1.383(4) . ? C3 C8 1.477(4) . ? C4 C5 1.497(4) . ? C5 C6 1.476(4) . ? C6 C7 1.338(5) . ? C9 C10 1.397(4) . ? C9 C12 1.450(4) . ? C10 C11 1.383(4) . ? C11 C16 1.477(4) . ? C12 C13 1.361(9) . ? C12 C13A 1.468(10) . ? C12 S2A 1.708(6) . ? C13 C14 1.418(10) . ? C14 C15 1.344(9) . ? C18 C19 1.494(4) . ? C22 C23 1.50(2) . ? C13A C14A 1.465(10) . ? S2A C15A 1.680(10) . ? C14A C15A 1.333(10) . ? O3A C21A 1.36(3) . ? O3A C22A 1.46(3) . ? C23A C22A 1.46(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 N3 Yb1 N1 99.32(8) . . ? N3 Yb1 N4 32.29(8) . . ? N1 Yb1 N4 91.71(8) . . ? N3 Yb1 N2 101.01(8) . . ? N1 Yb1 N2 32.27(8) . . ? N4 Yb1 N2 110.47(8) . . ? N3 Yb1 O4 123.08(8) . . ? N1 Yb1 O4 92.72(8) . . ? N4 Yb1 O4 92.53(8) . . ? N2 Yb1 O4 116.63(8) . . ? N3 Yb1 O2 85.41(7) . . ? N1 Yb1 O2 125.11(7) . . ? N4 Yb1 O2 114.95(7) . . ? N2 Yb1 O2 92.94(7) . . ? O4 Yb1 O2 129.89(8) . . ? N3 Yb1 O3 155.1(3) . . ? N1 Yb1 O3 102.0(3) . . ? N4 Yb1 O3 157.0(2) . . ? N2 Yb1 O3 90.4(2) . . ? O4 Yb1 O3 68.7(3) . . ? O2 Yb1 O3 71.9(3) . . ? N3 Yb1 O3A 167.0(6) . . ? N1 Yb1 O3A 91.6(6) . . ? N4 Yb1 O3A 155.3(3) . . ? N2 Yb1 O3A 84.5(4) . . ? O4 Yb1 O3A 62.9(4) . . ? O2 Yb1 O3A 82.5(6) . . ? O3 Yb1 O3A 11.9(4) . . ? N3 Yb1 O1 83.08(7) . . ? N1 Yb1 O1 168.13(7) . . ? N4 Yb1 O1 84.14(7) . . ? N2 Yb1 O1 158.85(7) . . ? O4 Yb1 O1 76.41(7) . . ? O2 Yb1 O1 66.53(7) . . ? O3 Yb1 O1 78.7(3) . . ? O3A Yb1 O1 87.7(5) . . ? C7 S1 C4 92.77(17) . . ? C15 S2 C12 92.8(3) . . ? C18 O1 C17 111.7(2) . . ? C18 O1 Yb1 112.21(17) . . ? C17 O1 Yb1 117.46(18) . . ? C20 O2 C19 112.2(2) . . ? C20 O2 Yb1 123.65(19) . . ? C19 O2 Yb1 116.24(17) . . ? C22 O3 C21 112.0(10) . . ? C22 O3 Yb1 109.6(8) . . ? C21 O3 Yb1 128.0(8) . . ? C23A O4 C24 104.8(14) . . ? C23A O4 C23 14.3(16) . . ? C24 O4 C23 116.7(8) . . ? C23A O4 Yb1 122.9(14) . . ? C24 O4 Yb1 126.6(2) . . ? C23 O4 Yb1 114.5(7) . . ? C1 N1 N2 108.4(2) . . ? C1 N1 Yb1 170.4(2) . . ? N2 N1 Yb1 75.76(15) . . ? C3 N2 N1 106.8(2) . . ? C3 N2 Yb1 171.8(2) . . ? N1 N2 Yb1 71.96(14) . . ? C9 N3 N4 108.5(2) . . ? C9 N3 Yb1 174.0(2) . . ? N4 N3 Yb1 75.75(14) . . ? C11 N4 N3 106.8(2) . . ? C11 N4 Yb1 175.6(2) . . ? N3 N4 Yb1 71.96(14) . . ? N1 C1 C2 109.9(3) . . ? N1 C1 C4 121.5(3) . . ? C2 C1 C4 128.5(3) . . ? C3 C2 C1 103.6(3) . . ? N2 C3 C2 111.3(3) . . ? N2 C3 C8 121.0(3) . . ? C2 C3 C8 127.7(3) . . ? C1 C4 C5 125.2(3) . . ? C1 C4 S1 121.6(2) . . ? C5 C4 S1 113.1(2) . . ? C6 C5 C4 103.8(3) . . ? C7 C6 C5 116.9(3) . . ? C6 C7 S1 113.4(3) . . ? F3 C8 F1 107.0(3) . . ? F3 C8 F2 106.5(3) . . ? F1 C8 F2 104.5(3) . . ? F3 C8 C3 113.6(3) . . ? F1 C8 C3 111.8(3) . . ? F2 C8 C3 112.8(3) . . ? N3 C9 C10 109.8(2) . . ? N3 C9 C12 120.9(2) . . ? C10 C9 C12 129.3(3) . . ? C11 C10 C9 103.4(2) . . ? N4 C11 C10 111.5(3) . . ? N4 C11 C16 120.2(3) . . ? C10 C11 C16 128.3(3) . . ? C13 C12 C9 130.2(4) . . ? C13 C12 C13A 100.8(9) . . ? C9 C12 C13A 128.4(9) . . ? C13 C12 S2A 12.2(6) . . ? C9 C12 S2A 118.6(4) . . ? C13A C12 S2A 112.8(8) . . ? C13 C12 S2 109.1(4) . . ? C9 C12 S2 120.7(2) . . ? C13A C12 S2 11.3(10) . . ? S2A C12 S2 120.7(3) . . ? C12 C13 C14 113.7(6) . . ? C15 C14 C13 112.6(6) . . ? C14 C15 S2 111.7(5) . . ? F5 C16 F4 106.1(3) . . ? F5 C16 F6 106.6(3) . . ? F4 C16 F6 105.5(3) . . ? F5 C16 C11 113.4(3) . . ? F4 C16 C11 111.9(3) . . ? F6 C16 C11 112.8(3) . . ? O1 C18 C19 108.5(2) . . ? O2 C19 C18 108.5(2) . . ? O3 C22 C23 110.4(11) . . ? O4 C23 C22 110.7(10) . . ? C14A C13A C12 104.5(11) . . ? C15A S2A C12 93.0(8) . . ? C15A C14A C13A 117.1(13) . . ? C14A C15A S2A 112.1(12) . . ? C21A O3A C22A 114.9(16) . . ? C21A O3A Yb1 125.4(16) . . ? C22A O3A Yb1 110.0(12) . . ? O4 C23A C22A 102.7(18) . . ? C23A C22A O3A 108(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.380 _refine_diff_density_min -1.656 _refine_diff_density_rms 0.096 #===END data_compound8 _database_code_depnum_ccdc_archive 'CCDC 794845' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Ba(ttfpz)2(dme)3] ; _chemical_name_common (Ba(ttfpz)2(dme)3) _chemical_melting_point ? _chemical_formula_moiety 'C28 H38 Ba F6 N4 O6 S2' _chemical_formula_sum 'C28 H38 Ba F6 N4 O6 S2' _chemical_formula_weight 842.08 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.2283(3) _cell_length_b 19.7677(3) _cell_length_c 36.8700(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.2920(10) _cell_angle_gamma 90.00 _cell_volume 14457.7(4) _cell_formula_units_Z 16 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 112788 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6784 _exptl_absorpt_coefficient_mu 1.288 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6985 _exptl_absorpt_correction_T_max 0.8302 _exptl_absorpt_process_details SADABS _exptl_special_details ; Thiophene groups were disordered over two positions, their occupancies were freely refined against each other. Their occupancies were refined to be 64:36 for S(2), 73:27 for S(3) and 74:26 for S(4). All disordered parts were restrained using DFIX, DANG and FLAT restraints. SIMU restraints were placed on thiophene groups S(2), S(3), S(3A), S(4) and S(4A). ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112788 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16611 _reflns_number_gt 14000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16611 _refine_ls_number_parameters 970 _refine_ls_number_restraints 122 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba1 Ba 0.361346(6) 0.522856(6) 0.129340(3) 0.01978(4) Uani 1 1 d . . . Ba2 Ba 0.392544(6) 0.036150(6) 0.116359(3) 0.01803(4) Uani 1 1 d . . . S1 S 0.52950(4) 0.36059(3) 0.17675(2) 0.04238(17) Uani 1 1 d . . . S2 S 0.43623(13) 0.37829(15) 0.04013(9) 0.0444(8) Uani 0.643(4) 1 d P A 1 S2A S 0.3567(4) 0.2752(4) 0.0098(2) 0.0328(12) Uani 0.357(4) 1 d PD A 2 S3 S 0.31304(8) -0.10807(9) 0.26057(4) 0.0407(5) Uani 0.731(3) 1 d PDU B 1 S3A S 0.3635(5) -0.1404(3) 0.20364(19) 0.0628(18) Uani 0.269(3) 1 d PDU B 2 S4 S 0.20372(7) -0.10997(7) 0.10306(4) 0.0514(5) Uani 0.741(4) 1 d PU C 1 S4A S 0.1849(4) -0.2057(3) 0.04212(17) 0.0308(11) Uani 0.259(4) 1 d PDU C 2 F1 F 0.62612(8) 0.69504(8) 0.17318(6) 0.0686(6) Uani 1 1 d . . . F2 F 0.52835(9) 0.71128(8) 0.18510(5) 0.0562(5) Uani 1 1 d . . . F3 F 0.54010(9) 0.70505(8) 0.12939(5) 0.0581(5) Uani 1 1 d . . . F4 F 0.13824(8) 0.29451(9) 0.09217(6) 0.0634(5) Uani 1 1 d . . . F5 F 0.12558(9) 0.39980(9) 0.09782(7) 0.0744(6) Uani 1 1 d . . . F6 F 0.18000(9) 0.34467(11) 0.14239(5) 0.0686(6) Uani 1 1 d . . . F7 F 0.27705(14) 0.18427(9) 0.24356(6) 0.0999(9) Uani 1 1 d . . . F8 F 0.27708(8) 0.20979(7) 0.18744(5) 0.0477(4) Uani 1 1 d . . . F9 F 0.36909(10) 0.20757(8) 0.22638(5) 0.0684(6) Uani 1 1 d . . . F10 F 0.43462(9) -0.16763(11) -0.00903(5) 0.0721(6) Uani 1 1 d . . . F11 F 0.50364(9) -0.14635(12) 0.04056(5) 0.0767(7) Uani 1 1 d . . . F12 F 0.46587(11) -0.06741(10) 0.00476(7) 0.0830(7) Uani 1 1 d . . . O1 O 0.29071(8) 0.56971(9) 0.05855(4) 0.0346(4) Uani 1 1 d . . . O2 O 0.42900(8) 0.54610(9) 0.06679(5) 0.0348(4) Uani 1 1 d . . . O3 O 0.23300(8) 0.57000(8) 0.14471(4) 0.0317(4) Uani 1 1 d . . . O4 O 0.32584(9) 0.66392(8) 0.13144(5) 0.0372(4) Uani 1 1 d . . . O5 O 0.36496(9) 0.42503(8) 0.18670(5) 0.0347(4) Uani 1 1 d . . . O6 O 0.37638(9) 0.56014(8) 0.20689(4) 0.0334(4) Uani 1 1 d . . . O7 O 0.25603(8) 0.07730(9) 0.09212(5) 0.0357(4) Uani 1 1 d . . . O8 O 0.34559(8) 0.10127(8) 0.04435(4) 0.0285(4) Uani 1 1 d . . . O9 O 0.50566(7) 0.07751(8) 0.08833(4) 0.0269(4) Uani 1 1 d . . . O10 O 0.43819(8) 0.17262(8) 0.12003(4) 0.0271(4) Uani 1 1 d . . . O11 O 0.47187(8) -0.07699(7) 0.14880(4) 0.0265(4) Uani 1 1 d . . . O12 O 0.51201(8) 0.05121(8) 0.17723(4) 0.0292(4) Uani 1 1 d . . . N1 N 0.49698(9) 0.50880(9) 0.15653(5) 0.0243(4) Uani 1 1 d . . . N2 N 0.49014(9) 0.57718(9) 0.15333(5) 0.0274(4) Uani 1 1 d . . . N3 N 0.32544(9) 0.41077(9) 0.08526(5) 0.0244(4) Uani 1 1 d . . . N4 N 0.27231(10) 0.41472(9) 0.10292(5) 0.0263(4) Uani 1 1 d . . . N5 N 0.34849(9) 0.01425(9) 0.18095(5) 0.0237(4) Uani 1 1 d . . . N6 N 0.34341(10) 0.08304(9) 0.17934(5) 0.0244(4) Uani 1 1 d . . . N7 N 0.33172(9) -0.07176(9) 0.07500(5) 0.0224(4) Uani 1 1 d . . . N8 N 0.38914(9) -0.06491(9) 0.06141(5) 0.0243(4) Uani 1 1 d . . . C1 C 0.56298(11) 0.49457(11) 0.16887(6) 0.0226(5) Uani 1 1 d . . . C2 C 0.60011(12) 0.55424(12) 0.17379(6) 0.0271(5) Uani 1 1 d . . . H2 H 0.6473 0.5596 0.1823 0.032 Uiso 1 1 calc R . . C3 C 0.55219(12) 0.60373(12) 0.16348(6) 0.0275(5) Uani 1 1 d . . . C4 C 0.58598(11) 0.42540(12) 0.17688(6) 0.0254(5) Uani 1 1 d . . . C5 C 0.65225(12) 0.40248(12) 0.18710(6) 0.0252(5) Uani 1 1 d . . . H5 H 0.6910 0.4303 0.1887 0.030 Uiso 1 1 calc R . . C6 C 0.65411(15) 0.33217(14) 0.19474(8) 0.0431(7) Uani 1 1 d . . . H6 H 0.6948 0.3076 0.2023 0.052 Uiso 1 1 calc R . . C7 C 0.59289(16) 0.30354(14) 0.19026(8) 0.0478(7) Uani 1 1 d . . . H7 H 0.5857 0.2568 0.1942 0.057 Uiso 1 1 calc R . . C8 C 0.56170(13) 0.67780(13) 0.16276(8) 0.0374(6) Uani 1 1 d . . . C9 C 0.31660(11) 0.35598(11) 0.06322(6) 0.0215(5) Uani 1 1 d . A . C10 C 0.25728(11) 0.32300(11) 0.06620(6) 0.0235(5) Uani 1 1 d . . . H10 H 0.2386 0.2832 0.0538 0.028 Uiso 1 1 calc R . . C11 C 0.23199(11) 0.36172(11) 0.09150(6) 0.0223(5) Uani 1 1 d . . . C12 C 0.36466(12) 0.33790(12) 0.04031(6) 0.0273(5) Uani 1 1 d D . . C13 C 0.3559(8) 0.2841(8) 0.0168(4) 0.024(2) Uani 0.643(4) 1 d PU A 1 H13 H 0.3182 0.2545 0.0136 0.029 Uiso 0.643(4) 1 calc PR A 1 C13A C 0.4289(7) 0.3758(9) 0.0432(5) 0.060(9) Uani 0.357(4) 1 d PD A 2 H13A H 0.4445 0.4129 0.0590 0.072 Uiso 0.357(4) 1 calc PR A 2 C14 C 0.4126(6) 0.2775(7) -0.0031(4) 0.0366(18) Uani 0.643(4) 1 d PU A 1 H14 H 0.4154 0.2438 -0.0211 0.044 Uiso 0.643(4) 1 calc PR A 1 C14A C 0.4624(9) 0.3430(9) 0.0163(6) 0.041(4) Uani 0.357(4) 1 d PD A 2 H14A H 0.5049 0.3582 0.0123 0.049 Uiso 0.357(4) 1 calc PR A 2 C15 C 0.4598(5) 0.3258(5) 0.0078(3) 0.040(2) Uani 0.643(4) 1 d PU A 1 H15 H 0.5005 0.3301 -0.0013 0.048 Uiso 0.643(4) 1 calc PR A 1 C15A C 0.4310(8) 0.2909(10) -0.0026(6) 0.040(5) Uani 0.357(4) 1 d PD A 2 H15A H 0.4483 0.2659 -0.0207 0.048 Uiso 0.357(4) 1 calc PR A 2 C16 C 0.17015(12) 0.35008(12) 0.10580(8) 0.0332(6) Uani 1 1 d . . . C17 C 0.32742(11) -0.00680(11) 0.21161(6) 0.0218(5) Uani 1 1 d . B . C18 C 0.30743(12) 0.04812(12) 0.22997(6) 0.0270(5) Uani 1 1 d . . . H18 H 0.2900 0.0483 0.2521 0.032 Uiso 1 1 calc R . . C19 C 0.31861(12) 0.10260(11) 0.20869(6) 0.0250(5) Uani 1 1 d . . . C20 C 0.33161(12) -0.07749(12) 0.22202(7) 0.0336(6) Uani 1 1 d D . . C21 C 0.3511(5) -0.1286(4) 0.1992(3) 0.061(3) Uani 0.731(3) 1 d PDU B 1 H21 H 0.3609 -0.1226 0.1752 0.074 Uiso 0.731(3) 1 calc PR B 3 C21A C 0.3106(9) -0.0977(7) 0.2570(4) 0.045(4) Uani 0.269(3) 1 d PDU B 2 H21A H 0.2911 -0.0696 0.2729 0.054 Uiso 0.269(3) 1 calc PR B 4 C22 C 0.3533(4) -0.1926(3) 0.2197(2) 0.0849(19) Uani 0.731(3) 1 d PDU B 1 H22 H 0.3670 -0.2340 0.2104 0.102 Uiso 0.731(3) 1 calc PR B 3 C22A C 0.3260(9) -0.1696(6) 0.2616(4) 0.048(3) Uani 0.269(3) 1 d PDU B 2 H22A H 0.3158 -0.1948 0.2818 0.057 Uiso 0.269(3) 1 calc PR B 4 C23 C 0.3343(3) -0.1883(2) 0.25272(18) 0.0606(18) Uani 0.731(3) 1 d PDU B 1 H23 H 0.3331 -0.2251 0.2691 0.073 Uiso 0.731(3) 1 calc PR B 3 C23A C 0.3554(11) -0.1979(6) 0.2360(4) 0.055(3) Uani 0.269(3) 1 d PDU B 2 H23A H 0.3695 -0.2438 0.2360 0.066 Uiso 0.269(3) 1 calc PR B 4 C24 C 0.31026(16) 0.17499(13) 0.21638(8) 0.0408(7) Uani 1 1 d . . . C25 C 0.29856(11) -0.12710(11) 0.05970(6) 0.0229(5) Uani 1 1 d . C . C26 C 0.33493(12) -0.15772(12) 0.03596(6) 0.0282(5) Uani 1 1 d . . . H26 H 0.3240 -0.1976 0.0217 0.034 Uiso 1 1 calc R . . C27 C 0.39062(12) -0.11660(12) 0.03795(6) 0.0259(5) Uani 1 1 d . . . C28 C 0.23363(12) -0.14633(12) 0.06789(6) 0.0272(5) Uani 1 1 d D . . C29 C 0.1896(5) -0.1935(5) 0.0515(2) 0.041(2) Uani 0.741(4) 1 d PU C 1 H29 H 0.1982 -0.2211 0.0318 0.049 Uiso 0.741(4) 1 calc PR C 5 C29A C 0.1929(6) -0.1009(7) 0.0880(3) 0.061(5) Uani 0.259(4) 1 d PDU C 2 H29A H 0.2038 -0.0574 0.0983 0.074 Uiso 0.259(4) 1 calc PR C 6 C30 C 0.1300(5) -0.1991(6) 0.0656(4) 0.0430(16) Uani 0.741(4) 1 d PU C 1 H30 H 0.0930 -0.2275 0.0556 0.052 Uiso 0.741(4) 1 calc PR C 5 C30A C 0.1315(8) -0.1419(9) 0.0874(5) 0.054(4) Uani 0.259(4) 1 d PDU C 2 H30A H 0.0990 -0.1292 0.1016 0.064 Uiso 0.259(4) 1 calc PR C 6 C31 C 0.1326(3) -0.1579(3) 0.09554(16) 0.0407(14) Uani 0.741(4) 1 d PU C 1 H31 H 0.0990 -0.1562 0.1103 0.049 Uiso 0.741(4) 1 calc PR C 5 C31A C 0.1231(14) -0.1971(17) 0.0664(11) 0.043(4) Uani 0.259(4) 1 d PDU C 2 H31A H 0.0867 -0.2278 0.0652 0.051 Uiso 0.259(4) 1 calc PR C 6 C32 C 0.44781(14) -0.12481(14) 0.01913(7) 0.0369(6) Uani 1 1 d . . . C33 C 0.22054(13) 0.55188(16) 0.05198(8) 0.0469(8) Uani 1 1 d . . . H33A H 0.1964 0.5766 0.0304 0.070 Uiso 1 1 calc R . . H33B H 0.2017 0.5637 0.0737 0.070 Uiso 1 1 calc R . . H33C H 0.2157 0.5031 0.0474 0.070 Uiso 1 1 calc R . . C34 C 0.32037(13) 0.54997(15) 0.02826(7) 0.0386(6) Uani 1 1 d . . . H34A H 0.2939 0.5687 0.0050 0.046 Uiso 1 1 calc R . . H34B H 0.3201 0.5000 0.0262 0.046 Uiso 1 1 calc R . . C35 C 0.39099(14) 0.57542(15) 0.03408(7) 0.0412(7) Uani 1 1 d . . . H35A H 0.4113 0.5633 0.0126 0.049 Uiso 1 1 calc R . . H35B H 0.3913 0.6253 0.0364 0.049 Uiso 1 1 calc R . . C36 C 0.49967(13) 0.55489(17) 0.06886(8) 0.0466(7) Uani 1 1 d . . . H36A H 0.5122 0.5371 0.0463 0.070 Uiso 1 1 calc R . . H36B H 0.5245 0.5305 0.0904 0.070 Uiso 1 1 calc R . . H36C H 0.5108 0.6031 0.0713 0.070 Uiso 1 1 calc R . . C37 C 0.21065(14) 0.52282(14) 0.16884(7) 0.0395(6) Uani 1 1 d . . . H37A H 0.2424 0.5223 0.1926 0.059 Uiso 1 1 calc R . . H37B H 0.2083 0.4776 0.1578 0.059 Uiso 1 1 calc R . . H37C H 0.1659 0.5360 0.1727 0.059 Uiso 1 1 calc R . . C38 C 0.23142(14) 0.63742(14) 0.15764(8) 0.0446(7) Uani 1 1 d . . . H38A H 0.2596 0.6414 0.1827 0.053 Uiso 1 1 calc R . . H38B H 0.1846 0.6503 0.1589 0.053 Uiso 1 1 calc R . . C39 C 0.25765(14) 0.68272(14) 0.13168(9) 0.0504(8) Uani 1 1 d . . . H39A H 0.2299 0.6783 0.1065 0.060 Uiso 1 1 calc R . . H39B H 0.2558 0.7304 0.1397 0.060 Uiso 1 1 calc R . . C40 C 0.35614(16) 0.70731(15) 0.10869(9) 0.0564(9) Uani 1 1 d . . . H40A H 0.3304 0.7055 0.0833 0.085 Uiso 1 1 calc R . . H40B H 0.4025 0.6926 0.1091 0.085 Uiso 1 1 calc R . . H40C H 0.3564 0.7538 0.1180 0.085 Uiso 1 1 calc R . . C41 C 0.34481(14) 0.35613(12) 0.18302(9) 0.0427(7) Uani 1 1 d . . . H41A H 0.3814 0.3274 0.1960 0.064 Uiso 1 1 calc R . . H41B H 0.3346 0.3438 0.1568 0.064 Uiso 1 1 calc R . . H41C H 0.3046 0.3496 0.1937 0.064 Uiso 1 1 calc R . . C42 C 0.38050(17) 0.44442(15) 0.22409(7) 0.0498(8) Uani 1 1 d . . . H42A H 0.4108 0.4102 0.2382 0.060 Uiso 1 1 calc R . . H42B H 0.3385 0.4454 0.2341 0.060 Uiso 1 1 calc R . . C43 C 0.41205(19) 0.50891(16) 0.22936(8) 0.0583(9) Uani 1 1 d . . . H43A H 0.4166 0.5221 0.2556 0.070 Uiso 1 1 calc R . . H43B H 0.4580 0.5054 0.2240 0.070 Uiso 1 1 calc R . . C44 C 0.40293(16) 0.62506(14) 0.21804(8) 0.0488(8) Uani 1 1 d . . . H44A H 0.3935 0.6359 0.2425 0.073 Uiso 1 1 calc R . . H44B H 0.3818 0.6590 0.2001 0.073 Uiso 1 1 calc R . . H44C H 0.4518 0.6250 0.2193 0.073 Uiso 1 1 calc R . . C45 C 0.20809(14) 0.0857(2) 0.11554(9) 0.0640(10) Uani 1 1 d . . . H45A H 0.2018 0.1341 0.1197 0.096 Uiso 1 1 calc R . . H45B H 0.2246 0.0632 0.1393 0.096 Uiso 1 1 calc R . . H45C H 0.1650 0.0657 0.1037 0.096 Uiso 1 1 calc R . . C46 C 0.23475(13) 0.10777(14) 0.05712(8) 0.0407(7) Uani 1 1 d . . . H46A H 0.2386 0.1576 0.0595 0.049 Uiso 1 1 calc R . . H46B H 0.1869 0.0964 0.0473 0.049 Uiso 1 1 calc R . . C47 C 0.27707(12) 0.08331(14) 0.03123(7) 0.0352(6) Uani 1 1 d . . . H47A H 0.2731 0.0335 0.0288 0.042 Uiso 1 1 calc R . . H47B H 0.2610 0.1035 0.0065 0.042 Uiso 1 1 calc R . . C48 C 0.38427(13) 0.08956(14) 0.01649(7) 0.0339(6) Uani 1 1 d . . . H48A H 0.3828 0.0414 0.0102 0.051 Uiso 1 1 calc R . . H48B H 0.4311 0.1032 0.0258 0.051 Uiso 1 1 calc R . . H48C H 0.3655 0.1161 -0.0056 0.051 Uiso 1 1 calc R . . C49 C 0.55274(13) 0.02459(14) 0.08703(8) 0.0382(6) Uani 1 1 d . . . H49A H 0.5793 0.0350 0.0682 0.057 Uiso 1 1 calc R . . H49B H 0.5285 -0.0181 0.0808 0.057 Uiso 1 1 calc R . . H49C H 0.5829 0.0204 0.1112 0.057 Uiso 1 1 calc R . . C50 C 0.53704(12) 0.13995(13) 0.10002(7) 0.0341(6) Uani 1 1 d . . . H50A H 0.5695 0.1521 0.0842 0.041 Uiso 1 1 calc R . . H50B H 0.5619 0.1363 0.1259 0.041 Uiso 1 1 calc R . . C51 C 0.48384(13) 0.19283(12) 0.09722(7) 0.0337(6) Uani 1 1 d . . . H51A H 0.5044 0.2370 0.1056 0.040 Uiso 1 1 calc R . . H51B H 0.4597 0.1975 0.0712 0.040 Uiso 1 1 calc R . . C52 C 0.38506(14) 0.22015(13) 0.11898(8) 0.0407(7) Uani 1 1 d . . . H52A H 0.4041 0.2648 0.1263 0.061 Uiso 1 1 calc R . . H52B H 0.3563 0.2059 0.1361 0.061 Uiso 1 1 calc R . . H52C H 0.3582 0.2225 0.0938 0.061 Uiso 1 1 calc R . . C53 C 0.47172(14) -0.14282(12) 0.13290(7) 0.0351(6) Uani 1 1 d . . . H53A H 0.5119 -0.1483 0.1220 0.053 Uiso 1 1 calc R . . H53B H 0.4312 -0.1483 0.1136 0.053 Uiso 1 1 calc R . . H53C H 0.4719 -0.1771 0.1521 0.053 Uiso 1 1 calc R . . C54 C 0.52931(12) -0.06845(13) 0.17775(7) 0.0322(6) Uani 1 1 d . . . H54A H 0.5702 -0.0626 0.1671 0.039 Uiso 1 1 calc R . . H54B H 0.5355 -0.1091 0.1937 0.039 Uiso 1 1 calc R . . C55 C 0.51946(13) -0.00766(12) 0.20015(6) 0.0310(6) Uani 1 1 d . . . H55A H 0.4788 -0.0137 0.2110 0.037 Uiso 1 1 calc R . . H55B H 0.5588 -0.0021 0.2207 0.037 Uiso 1 1 calc R . . C56 C 0.51272(15) 0.11068(13) 0.19945(7) 0.0401(7) Uani 1 1 d . . . H56A H 0.4769 0.1077 0.2138 0.060 Uiso 1 1 calc R . . H56B H 0.5053 0.1506 0.1834 0.060 Uiso 1 1 calc R . . H56C H 0.5565 0.1145 0.2163 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.02056(7) 0.01943(7) 0.01824(7) -0.00052(5) 0.00111(5) -0.00321(5) Ba2 0.01912(7) 0.01871(6) 0.01661(6) -0.00106(5) 0.00436(5) -0.00088(5) S1 0.0383(4) 0.0319(4) 0.0553(5) 0.0066(3) 0.0050(3) -0.0039(3) S2 0.0375(10) 0.0420(14) 0.0615(16) -0.0087(11) 0.0285(10) -0.0108(9) S2A 0.046(2) 0.0300(18) 0.022(2) -0.0129(15) 0.0049(17) 0.0125(14) S3 0.0373(7) 0.0431(9) 0.0362(7) 0.0212(5) -0.0061(5) -0.0149(6) S3A 0.117(4) 0.020(2) 0.070(3) 0.0148(19) 0.064(3) 0.028(2) S4 0.0435(7) 0.0684(8) 0.0483(10) -0.0284(7) 0.0236(7) -0.0272(6) S4A 0.0340(19) 0.029(2) 0.029(3) -0.0062(17) 0.0052(18) -0.0142(14) F1 0.0376(9) 0.0351(9) 0.1253(17) -0.0094(10) -0.0036(10) -0.0157(8) F2 0.0754(12) 0.0268(8) 0.0714(12) -0.0084(8) 0.0264(10) -0.0007(8) F3 0.0845(13) 0.0333(9) 0.0539(11) 0.0099(8) 0.0071(10) -0.0145(9) F4 0.0491(10) 0.0550(11) 0.0951(15) -0.0297(10) 0.0362(10) -0.0319(9) F5 0.0380(10) 0.0597(12) 0.1341(19) 0.0241(12) 0.0380(11) 0.0183(9) F6 0.0475(11) 0.1189(17) 0.0451(11) 0.0001(11) 0.0228(9) -0.0247(11) F7 0.202(3) 0.0396(11) 0.0873(16) 0.0001(10) 0.1008(18) 0.0317(13) F8 0.0525(10) 0.0264(8) 0.0613(11) 0.0073(7) 0.0038(8) 0.0125(7) F9 0.0821(13) 0.0258(9) 0.0812(13) -0.0123(8) -0.0237(11) -0.0008(9) F10 0.0588(12) 0.1038(16) 0.0605(12) -0.0536(11) 0.0288(10) -0.0096(11) F11 0.0420(10) 0.142(2) 0.0462(11) -0.0090(12) 0.0094(9) 0.0391(12) F12 0.0887(15) 0.0660(13) 0.1194(19) 0.0105(13) 0.0819(15) 0.0086(11) O1 0.0312(9) 0.0447(11) 0.0245(9) 0.0061(8) -0.0032(7) -0.0081(8) O2 0.0303(9) 0.0465(11) 0.0269(9) 0.0044(8) 0.0042(7) -0.0122(8) O3 0.0320(9) 0.0338(9) 0.0295(9) -0.0062(7) 0.0062(8) -0.0014(7) O4 0.0348(10) 0.0254(9) 0.0474(11) 0.0069(8) -0.0017(8) 0.0006(7) O5 0.0462(11) 0.0256(9) 0.0298(9) 0.0066(7) 0.0015(8) -0.0030(8) O6 0.0410(10) 0.0300(9) 0.0252(9) -0.0047(7) -0.0032(8) 0.0030(8) O7 0.0208(9) 0.0562(12) 0.0307(9) -0.0040(8) 0.0068(7) 0.0053(8) O8 0.0236(8) 0.0391(10) 0.0219(8) 0.0004(7) 0.0020(7) -0.0011(7) O9 0.0213(8) 0.0307(9) 0.0291(9) 0.0011(7) 0.0058(7) -0.0007(7) O10 0.0309(9) 0.0256(8) 0.0255(8) 0.0046(7) 0.0074(7) -0.0004(7) O11 0.0269(8) 0.0224(8) 0.0286(9) 0.0017(7) 0.0013(7) 0.0043(7) O12 0.0366(10) 0.0292(9) 0.0194(8) 0.0007(7) -0.0001(7) -0.0029(7) N1 0.0242(10) 0.0231(10) 0.0248(10) -0.0007(8) 0.0030(8) -0.0018(8) N2 0.0252(10) 0.0234(10) 0.0323(11) -0.0027(8) 0.0023(9) -0.0026(8) N3 0.0264(10) 0.0260(10) 0.0227(10) -0.0018(8) 0.0094(8) -0.0056(8) N4 0.0286(11) 0.0242(10) 0.0280(10) -0.0039(8) 0.0103(9) -0.0064(8) N5 0.0283(10) 0.0192(9) 0.0255(10) -0.0010(8) 0.0101(8) 0.0009(8) N6 0.0309(11) 0.0208(10) 0.0229(10) 0.0016(8) 0.0090(8) 0.0004(8) N7 0.0228(10) 0.0233(10) 0.0215(10) -0.0025(8) 0.0056(8) -0.0007(8) N8 0.0230(10) 0.0278(10) 0.0234(10) -0.0024(8) 0.0073(8) 0.0015(8) C1 0.0214(11) 0.0290(12) 0.0174(11) -0.0018(9) 0.0035(9) -0.0015(9) C2 0.0222(12) 0.0330(13) 0.0255(12) -0.0029(10) 0.0035(10) -0.0046(10) C3 0.0270(12) 0.0261(12) 0.0288(13) -0.0033(10) 0.0039(10) -0.0048(10) C4 0.0271(12) 0.0279(12) 0.0207(11) -0.0011(9) 0.0037(10) -0.0013(10) C5 0.0262(12) 0.0298(12) 0.0192(11) 0.0008(9) 0.0036(9) 0.0055(10) C6 0.0447(17) 0.0398(16) 0.0409(16) 0.0034(12) -0.0011(13) 0.0158(13) C7 0.062(2) 0.0272(14) 0.0523(18) 0.0083(13) 0.0067(15) 0.0039(14) C8 0.0317(14) 0.0305(14) 0.0481(17) -0.0037(12) 0.0029(13) -0.0053(11) C9 0.0244(12) 0.0208(11) 0.0186(11) 0.0017(9) 0.0025(9) 0.0030(9) C10 0.0243(12) 0.0184(11) 0.0255(12) -0.0013(9) -0.0003(10) 0.0008(9) C11 0.0217(11) 0.0204(11) 0.0245(12) 0.0014(9) 0.0036(9) -0.0008(9) C12 0.0290(13) 0.0288(13) 0.0242(12) 0.0048(10) 0.0052(10) 0.0060(10) C13 0.028(3) 0.031(5) 0.016(5) -0.013(3) 0.012(3) 0.009(3) C13A 0.094(18) 0.052(13) 0.044(10) -0.015(8) 0.037(10) 0.028(10) C14 0.042(4) 0.036(4) 0.034(3) -0.004(3) 0.012(3) 0.011(3) C14A 0.044(6) 0.043(9) 0.045(10) -0.009(6) 0.031(6) 0.003(5) C15 0.046(4) 0.045(6) 0.037(5) -0.001(4) 0.028(3) 0.012(3) C15A 0.043(12) 0.049(13) 0.029(6) -0.001(8) 0.010(8) 0.018(8) C16 0.0278(13) 0.0287(13) 0.0438(16) -0.0016(11) 0.0088(12) -0.0024(11) C17 0.0202(11) 0.0222(11) 0.0233(11) 0.0025(9) 0.0047(9) -0.0015(9) C18 0.0335(13) 0.0297(13) 0.0206(11) 0.0029(10) 0.0120(10) 0.0040(10) C19 0.0330(13) 0.0217(11) 0.0217(11) 0.0008(9) 0.0089(10) 0.0043(10) C20 0.0267(13) 0.0247(13) 0.0501(16) 0.0107(11) 0.0092(12) -0.0022(10) C21 0.081(5) 0.010(3) 0.111(6) 0.026(3) 0.065(4) 0.016(3) C21A 0.082(7) 0.009(5) 0.047(6) 0.009(4) 0.024(6) 0.016(5) C22 0.096(4) 0.030(3) 0.140(5) 0.026(3) 0.051(4) 0.017(2) C22A 0.088(6) 0.016(5) 0.047(5) 0.008(4) 0.032(5) 0.012(4) C23 0.043(3) 0.031(3) 0.104(5) 0.041(3) 0.005(3) -0.004(2) C23A 0.106(6) 0.016(4) 0.055(4) 0.014(4) 0.043(4) 0.023(4) C24 0.0629(19) 0.0249(13) 0.0375(15) -0.0018(11) 0.0172(14) 0.0082(13) C25 0.0289(12) 0.0224(11) 0.0166(11) -0.0011(9) 0.0021(9) -0.0009(9) C26 0.0403(14) 0.0227(12) 0.0210(12) -0.0061(9) 0.0045(10) 0.0003(10) C27 0.0294(13) 0.0282(12) 0.0199(11) -0.0009(9) 0.0038(10) 0.0038(10) C28 0.0324(13) 0.0286(12) 0.0203(12) -0.0024(10) 0.0049(10) -0.0048(10) C29 0.051(4) 0.039(4) 0.032(4) -0.008(3) 0.004(3) -0.009(3) C29A 0.046(7) 0.135(11) 0.001(5) -0.001(6) -0.002(5) -0.054(7) C30 0.045(4) 0.040(3) 0.042(3) -0.006(3) 0.002(3) -0.019(3) C30A 0.049(7) 0.094(9) 0.023(6) 0.011(6) 0.019(5) -0.043(6) C31 0.043(2) 0.048(3) 0.037(3) -0.005(2) 0.021(2) -0.021(2) C31A 0.040(7) 0.064(8) 0.026(7) 0.004(7) 0.012(6) -0.027(7) C32 0.0380(15) 0.0444(16) 0.0300(14) -0.0073(12) 0.0107(12) 0.0080(12) C33 0.0302(14) 0.073(2) 0.0324(15) 0.0123(14) -0.0069(12) -0.0082(14) C34 0.0412(16) 0.0504(17) 0.0213(12) 0.0078(11) -0.0012(11) -0.0105(13) C35 0.0448(16) 0.0506(17) 0.0275(14) 0.0078(12) 0.0053(12) -0.0135(13) C36 0.0342(15) 0.070(2) 0.0379(16) 0.0002(14) 0.0120(13) -0.0125(14) C37 0.0385(15) 0.0544(18) 0.0285(14) -0.0033(12) 0.0137(12) -0.0050(13) C38 0.0301(14) 0.0435(16) 0.0585(19) -0.0169(14) 0.0047(13) 0.0060(12) C39 0.0369(16) 0.0300(15) 0.078(2) 0.0002(15) -0.0052(15) 0.0072(12) C40 0.059(2) 0.0344(16) 0.072(2) 0.0173(15) 0.0043(17) -0.0120(14) C41 0.0436(16) 0.0235(13) 0.0614(19) 0.0089(13) 0.0111(14) 0.0014(12) C42 0.079(2) 0.0446(17) 0.0250(14) 0.0115(12) 0.0093(14) 0.0110(16) C43 0.086(2) 0.0537(19) 0.0260(15) 0.0010(13) -0.0123(15) 0.0062(18) C44 0.0597(19) 0.0397(16) 0.0399(16) -0.0157(13) -0.0076(14) -0.0028(14) C45 0.0282(16) 0.118(3) 0.0500(19) -0.018(2) 0.0167(14) 0.0063(18) C46 0.0242(13) 0.0467(17) 0.0494(17) 0.0062(13) 0.0028(12) 0.0087(12) C47 0.0274(13) 0.0465(16) 0.0272(13) 0.0050(11) -0.0056(11) -0.0005(11) C48 0.0341(14) 0.0443(15) 0.0234(12) 0.0016(11) 0.0057(11) 0.0012(12) C49 0.0272(13) 0.0472(16) 0.0414(15) -0.0007(13) 0.0098(12) 0.0066(12) C50 0.0296(13) 0.0403(15) 0.0339(14) -0.0016(11) 0.0099(11) -0.0117(11) C51 0.0422(15) 0.0304(13) 0.0307(13) 0.0028(11) 0.0124(12) -0.0101(11) C52 0.0521(17) 0.0268(13) 0.0465(17) 0.0034(12) 0.0177(14) 0.0073(12) C53 0.0445(16) 0.0222(12) 0.0387(15) 0.0003(11) 0.0087(12) 0.0061(11) C54 0.0263(13) 0.0353(14) 0.0327(14) 0.0080(11) 0.0001(11) 0.0040(10) C55 0.0295(13) 0.0379(14) 0.0227(12) 0.0073(10) -0.0019(10) -0.0004(11) C56 0.0534(17) 0.0351(15) 0.0265(14) -0.0061(11) -0.0053(12) -0.0041(13) _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 Ba1 N1 2.7446(18) . ? Ba1 N3 2.7596(18) . ? Ba1 N2 2.7964(18) . ? Ba1 N4 2.8417(18) . ? Ba1 O5 2.8562(16) . ? Ba1 O1 2.8725(15) . ? Ba1 O4 2.8844(16) . ? Ba1 O6 2.9103(16) . ? Ba1 O3 2.9166(17) . ? Ba1 O2 2.9392(17) . ? Ba2 N5 2.7356(19) . ? Ba2 N7 2.7667(18) . ? Ba2 O9 2.8104(15) . ? Ba2 N8 2.8366(18) . ? Ba2 O10 2.8460(15) . ? Ba2 O7 2.8495(16) . ? Ba2 N6 2.8535(19) . ? Ba2 O11 2.8733(14) . ? Ba2 O8 2.9360(15) . ? Ba2 O12 2.9736(15) . ? S1 C7 1.707(3) . ? S1 C4 1.716(2) . ? S2 C12 1.654(3) . ? S2 C15 1.718(8) . ? S2A C12 1.659(6) . ? S2A C15A 1.685(9) . ? S3 C20 1.654(3) . ? S3 C23 1.683(5) . ? S3A C20 1.610(6) . ? S3A C23A 1.679(9) . ? S4 C28 1.695(3) . ? S4 C31 1.700(5) . ? S4A C31A 1.682(10) . ? S4A C28 1.698(5) . ? F1 C8 1.329(3) . ? F2 C8 1.338(3) . ? F3 C8 1.336(3) . ? F4 C16 1.323(3) . ? F5 C16 1.327(3) . ? F6 C16 1.329(3) . ? F7 C24 1.324(3) . ? F8 C24 1.335(3) . ? F9 C24 1.340(3) . ? F10 C32 1.326(3) . ? F11 C32 1.316(3) . ? F12 C32 1.333(3) . ? O1 C34 1.422(3) . ? O1 C33 1.436(3) . ? O2 C35 1.421(3) . ? O2 C36 1.427(3) . ? O3 C38 1.418(3) . ? O3 C37 1.422(3) . ? O4 C40 1.420(3) . ? O4 C39 1.430(3) . ? O5 C42 1.406(3) . ? O5 C41 1.421(3) . ? O6 C43 1.414(3) . ? O6 C44 1.421(3) . ? O7 C46 1.413(3) . ? O7 C45 1.429(3) . ? O8 C47 1.421(3) . ? O8 C48 1.427(3) . ? O9 C50 1.416(3) . ? O9 C49 1.422(3) . ? O10 C52 1.422(3) . ? O10 C51 1.423(3) . ? O11 C54 1.426(3) . ? O11 C53 1.427(3) . ? O12 C55 1.429(3) . ? O12 C56 1.431(3) . ? N1 C1 1.353(3) . ? N1 N2 1.361(3) . ? N2 C3 1.344(3) . ? N3 C9 1.345(3) . ? N3 N4 1.363(3) . ? N4 C11 1.344(3) . ? N5 C17 1.350(3) . ? N5 N6 1.364(2) . ? N6 C19 1.336(3) . ? N7 C25 1.348(3) . ? N7 N8 1.359(3) . ? N8 C27 1.343(3) . ? C1 C2 1.391(3) . ? C1 C4 1.456(3) . ? C2 C3 1.377(3) . ? C3 C8 1.478(3) . ? C4 C5 1.395(3) . ? C5 C6 1.417(3) . ? C6 C7 1.342(4) . ? C9 C10 1.389(3) . ? C9 C12 1.452(3) . ? C10 C11 1.380(3) . ? C11 C16 1.468(3) . ? C12 C13 1.360(11) . ? C12 C13A 1.485(9) . ? C13 C14 1.485(15) . ? C13A C14A 1.460(10) . ? C14 C15 1.354(11) . ? C14A C15A 1.332(9) . ? C17 C18 1.381(3) . ? C17 C20 1.447(3) . ? C18 C19 1.377(3) . ? C19 C24 1.475(3) . ? C20 C21 1.420(7) . ? C20 C21A 1.489(10) . ? C21 C22 1.472(7) . ? C21A C22A 1.458(9) . ? C22 C23 1.347(6) . ? C22A C23A 1.336(9) . ? C25 C26 1.388(3) . ? C25 C28 1.455(3) . ? C26 C27 1.379(3) . ? C27 C32 1.470(4) . ? C28 C29 1.349(8) . ? C28 C29A 1.507(9) . ? C29 C30 1.408(10) . ? C29A C30A 1.479(9) . ? C30 C31 1.365(8) . ? C30A C31A 1.329(10) . ? C34 C35 1.490(4) . ? C38 C39 1.482(4) . ? C42 C43 1.422(4) . ? C46 C47 1.483(4) . ? C50 C51 1.489(4) . ? C54 C55 1.493(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 N1 Ba1 N3 105.24(5) . . ? N1 Ba1 N2 28.43(5) . . ? N3 Ba1 N2 128.03(6) . . ? N1 Ba1 N4 124.77(5) . . ? N3 Ba1 N4 28.13(5) . . ? N2 Ba1 N4 152.37(5) . . ? N1 Ba1 O5 77.42(5) . . ? N3 Ba1 O5 81.84(5) . . ? N2 Ba1 O5 97.97(5) . . ? N4 Ba1 O5 70.56(5) . . ? N1 Ba1 O1 130.42(5) . . ? N3 Ba1 O1 72.37(5) . . ? N2 Ba1 O1 115.49(5) . . ? N4 Ba1 O1 76.23(5) . . ? O5 Ba1 O1 145.81(5) . . ? N1 Ba1 O4 108.93(5) . . ? N3 Ba1 O4 138.92(5) . . ? N2 Ba1 O4 80.89(5) . . ? N4 Ba1 O4 126.30(5) . . ? O5 Ba1 O4 127.24(5) . . ? O1 Ba1 O4 68.31(5) . . ? N1 Ba1 O6 76.23(5) . . ? N3 Ba1 O6 138.30(5) . . ? N2 Ba1 O6 71.36(5) . . ? N4 Ba1 O6 117.68(5) . . ? O5 Ba1 O6 57.41(5) . . ? O1 Ba1 O6 138.48(5) . . ? O4 Ba1 O6 72.99(5) . . ? N1 Ba1 O3 145.65(5) . . ? N3 Ba1 O3 103.26(5) . . ? N2 Ba1 O3 128.72(5) . . ? N4 Ba1 O3 77.20(5) . . ? O5 Ba1 O3 88.11(5) . . ? O1 Ba1 O3 76.71(5) . . ? O4 Ba1 O3 56.64(5) . . ? O6 Ba1 O3 69.75(5) . . ? N1 Ba1 O2 73.55(5) . . ? N3 Ba1 O2 76.86(5) . . ? N2 Ba1 O2 68.90(5) . . ? N4 Ba1 O2 102.11(5) . . ? O5 Ba1 O2 137.61(5) . . ? O1 Ba1 O2 57.44(5) . . ? O4 Ba1 O2 91.52(5) . . ? O6 Ba1 O2 139.13(5) . . ? O3 Ba1 O2 132.18(5) . . ? N5 Ba2 N7 99.92(5) . . ? N5 Ba2 O9 142.52(5) . . ? N7 Ba2 O9 109.14(5) . . ? N5 Ba2 N8 122.95(5) . . ? N7 Ba2 N8 28.03(5) . . ? O9 Ba2 N8 81.37(5) . . ? N5 Ba2 O10 105.45(5) . . ? N7 Ba2 O10 149.56(5) . . ? O9 Ba2 O10 57.44(5) . . ? N8 Ba2 O10 131.60(5) . . ? N5 Ba2 O7 81.79(5) . . ? N7 Ba2 O7 75.42(5) . . ? O9 Ba2 O7 127.62(5) . . ? N8 Ba2 O7 95.20(5) . . ? O10 Ba2 O7 91.70(5) . . ? N5 Ba2 N6 28.15(5) . . ? N7 Ba2 N6 120.72(5) . . ? O9 Ba2 N6 130.03(5) . . ? N8 Ba2 N6 147.82(5) . . ? O10 Ba2 N6 79.33(5) . . ? O7 Ba2 N6 72.05(5) . . ? N5 Ba2 O11 76.41(5) . . ? N7 Ba2 O11 77.36(5) . . ? O9 Ba2 O11 87.19(4) . . ? N8 Ba2 O11 71.49(5) . . ? O10 Ba2 O11 124.65(4) . . ? O7 Ba2 O11 141.32(5) . . ? N6 Ba2 O11 99.74(5) . . ? N5 Ba2 O8 138.91(5) . . ? N7 Ba2 O8 79.01(5) . . ? O9 Ba2 O8 71.48(4) . . ? N8 Ba2 O8 72.82(5) . . ? O10 Ba2 O8 70.85(4) . . ? O7 Ba2 O8 57.94(5) . . ? N6 Ba2 O8 119.40(5) . . ? O11 Ba2 O8 140.63(5) . . ? N5 Ba2 O12 73.38(5) . . ? N7 Ba2 O12 134.52(5) . . ? O9 Ba2 O12 69.42(4) . . ? N8 Ba2 O12 120.80(5) . . ? O10 Ba2 O12 70.19(4) . . ? O7 Ba2 O12 143.38(5) . . ? N6 Ba2 O12 73.40(5) . . ? O11 Ba2 O12 57.23(4) . . ? O8 Ba2 O12 135.22(4) . . ? C7 S1 C4 91.76(13) . . ? C12 S2 C15 94.2(4) . . ? C12 S2A C15A 94.2(7) . . ? C20 S3 C23 95.0(2) . . ? C20 S3A C23A 97.0(5) . . ? C28 S4 C31 93.2(2) . . ? C31A S4A C28 92.5(7) . . ? C34 O1 C33 110.80(19) . . ? C34 O1 Ba1 114.44(14) . . ? C33 O1 Ba1 111.93(14) . . ? C35 O2 C36 111.5(2) . . ? C35 O2 Ba1 118.17(15) . . ? C36 O2 Ba1 126.32(14) . . ? C38 O3 C37 112.0(2) . . ? C38 O3 Ba1 116.43(14) . . ? C37 O3 Ba1 108.43(14) . . ? C40 O4 C39 112.0(2) . . ? C40 O4 Ba1 115.44(17) . . ? C39 O4 Ba1 119.79(14) . . ? C42 O5 C41 111.1(2) . . ? C42 O5 Ba1 120.65(15) . . ? C41 O5 Ba1 127.82(15) . . ? C43 O6 C44 110.9(2) . . ? C43 O6 Ba1 109.73(15) . . ? C44 O6 Ba1 118.30(16) . . ? C46 O7 C45 112.4(2) . . ? C46 O7 Ba2 120.76(14) . . ? C45 O7 Ba2 125.07(16) . . ? C47 O8 C48 110.51(18) . . ? C47 O8 Ba2 108.63(13) . . ? C48 O8 Ba2 117.00(13) . . ? C50 O9 C49 112.86(18) . . ? C50 O9 Ba2 119.36(14) . . ? C49 O9 Ba2 113.40(14) . . ? C52 O10 C51 111.89(18) . . ? C52 O10 Ba2 112.86(14) . . ? C51 O10 Ba2 118.69(13) . . ? C54 O11 C53 110.58(18) . . ? C54 O11 Ba2 121.76(13) . . ? C53 O11 Ba2 125.64(13) . . ? C55 O12 C56 110.03(18) . . ? C55 O12 Ba2 109.93(12) . . ? C56 O12 Ba2 115.45(14) . . ? C1 N1 N2 108.21(18) . . ? C1 N1 Ba1 173.65(15) . . ? N2 N1 Ba1 77.90(11) . . ? C3 N2 N1 106.85(18) . . ? C3 N2 Ba1 177.78(16) . . ? N1 N2 Ba1 73.67(11) . . ? C9 N3 N4 108.10(18) . . ? C9 N3 Ba1 172.31(15) . . ? N4 N3 Ba1 79.28(11) . . ? C11 N4 N3 107.02(18) . . ? C11 N4 Ba1 177.42(16) . . ? N3 N4 Ba1 72.59(11) . . ? C17 N5 N6 108.08(18) . . ? C17 N5 Ba2 171.14(15) . . ? N6 N5 Ba2 80.74(12) . . ? C19 N6 N5 106.87(18) . . ? C19 N6 Ba2 177.46(15) . . ? N5 N6 Ba2 71.12(11) . . ? C25 N7 N8 108.52(18) . . ? C25 N7 Ba2 170.97(15) . . ? N8 N7 Ba2 78.84(11) . . ? C27 N8 N7 106.88(18) . . ? C27 N8 Ba2 174.56(15) . . ? N7 N8 Ba2 73.12(11) . . ? N1 C1 C2 109.8(2) . . ? N1 C1 C4 121.2(2) . . ? C2 C1 C4 128.8(2) . . ? C3 C2 C1 103.5(2) . . ? N2 C3 C2 111.6(2) . . ? N2 C3 C8 120.0(2) . . ? C2 C3 C8 128.4(2) . . ? C5 C4 C1 127.7(2) . . ? C5 C4 S1 111.25(17) . . ? C1 C4 S1 120.96(17) . . ? C4 C5 C6 111.0(2) . . ? C7 C6 C5 113.7(2) . . ? C6 C7 S1 112.3(2) . . ? F1 C8 F3 106.8(2) . . ? F1 C8 F2 106.2(2) . . ? F3 C8 F2 104.7(2) . . ? F1 C8 C3 111.9(2) . . ? F3 C8 C3 113.3(2) . . ? F2 C8 C3 113.3(2) . . ? N3 C9 C10 110.2(2) . . ? N3 C9 C12 121.7(2) . . ? C10 C9 C12 128.2(2) . . ? C11 C10 C9 103.52(19) . . ? N4 C11 C10 111.2(2) . . ? N4 C11 C16 121.2(2) . . ? C10 C11 C16 127.6(2) . . ? C13 C12 C9 122.9(7) . . ? C13 C12 C13A 116.4(9) . . ? C9 C12 C13A 120.6(6) . . ? C13 C12 S2 112.3(7) . . ? C9 C12 S2 124.7(2) . . ? C13A C12 S2 4.6(7) . . ? C13 C12 S2A 3.9(10) . . ? C9 C12 S2A 126.2(4) . . ? C13A C12 S2A 113.2(7) . . ? S2 C12 S2A 109.1(3) . . ? C12 C13 C14 111.5(12) . . ? C14A C13A C12 104.0(9) . . ? C15 C14 C13 111.1(10) . . ? C15A C14A C13A 117.5(12) . . ? C14 C15 S2 110.8(8) . . ? C14A C15A S2A 111.0(10) . . ? F4 C16 F5 105.7(2) . . ? F4 C16 F6 106.5(2) . . ? F5 C16 F6 104.2(2) . . ? F4 C16 C11 112.4(2) . . ? F5 C16 C11 113.2(2) . . ? F6 C16 C11 114.1(2) . . ? N5 C17 C18 109.82(19) . . ? N5 C17 C20 120.5(2) . . ? C18 C17 C20 129.5(2) . . ? C19 C18 C17 103.8(2) . . ? N6 C19 C18 111.4(2) . . ? N6 C19 C24 120.8(2) . . ? C18 C19 C24 127.7(2) . . ? C21 C20 C17 122.6(4) . . ? C21 C20 C21A 118.8(6) . . ? C17 C20 C21A 118.5(5) . . ? C21 C20 S3A 11.5(6) . . ? C17 C20 S3A 129.9(3) . . ? C21A C20 S3A 111.3(6) . . ? C21 C20 S3 112.7(4) . . ? C17 C20 S3 124.7(2) . . ? C21A C20 S3 6.6(6) . . ? S3A C20 S3 104.9(3) . . ? C20 C21 C22 106.8(6) . . ? C22A C21A C20 105.8(9) . . ? C23 C22 C21 115.2(6) . . ? C23A C22A C21A 116.1(10) . . ? C22 C23 S3 110.0(4) . . ? C22A C23A S3A 109.7(8) . . ? F7 C24 F8 106.5(2) . . ? F7 C24 F9 106.2(2) . . ? F8 C24 F9 104.7(2) . . ? F7 C24 C19 112.0(2) . . ? F8 C24 C19 113.9(2) . . ? F9 C24 C19 113.0(2) . . ? N7 C25 C26 109.7(2) . . ? N7 C25 C28 121.4(2) . . ? C26 C25 C28 128.9(2) . . ? C27 C26 C25 103.7(2) . . ? N8 C27 C26 111.2(2) . . ? N8 C27 C32 120.5(2) . . ? C26 C27 C32 128.3(2) . . ? C29 C28 C25 129.2(5) . . ? C29 C28 C29A 104.8(7) . . ? C25 C28 C29A 123.3(5) . . ? C29 C28 S4 109.5(5) . . ? C25 C28 S4 121.35(17) . . ? C29A C28 S4 19.9(5) . . ? C29 C28 S4A 8.5(6) . . ? C25 C28 S4A 120.9(3) . . ? C29A C28 S4A 111.9(5) . . ? S4 C28 S4A 117.8(3) . . ? C28 C29 C30 115.2(6) . . ? C30A C29A C28 101.8(9) . . ? C31 C30 C29 110.6(6) . . ? C31A C30A C29A 118.0(12) . . ? C30 C31 S4 111.2(5) . . ? C30A C31A S4A 111.7(11) . . ? F11 C32 F10 106.3(2) . . ? F11 C32 F12 104.1(2) . . ? F10 C32 F12 105.1(2) . . ? F11 C32 C27 114.5(2) . . ? F10 C32 C27 112.6(2) . . ? F12 C32 C27 113.3(2) . . ? O1 C34 C35 109.5(2) . . ? O2 C35 C34 109.2(2) . . ? O3 C38 C39 108.4(2) . . ? O4 C39 C38 108.3(2) . . ? O5 C42 C43 112.8(2) . . ? O6 C43 C42 113.5(3) . . ? O7 C46 C47 109.8(2) . . ? O8 C47 C46 110.3(2) . . ? O9 C50 C51 108.42(19) . . ? O10 C51 C50 107.80(19) . . ? O11 C54 C55 109.38(19) . . ? O12 C55 C54 109.78(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.841 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.074 #===END