Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Giulia Licini' _publ_contact_author_address ; Chemical Sciences University of Padova via Marzolo 1 Padova 35131 ITALY ; _publ_contact_author_email GIULIA.LICINI@UNIPD.IT _publ_section_title ; Stereoselective self-assembly of C3-symmetric Ti(IV) amine triphenolate complexes ; loop_ _publ_author_name 'Giulia Licini' 'Gerald Bernardinelli' 'Andrej Kolarovic' 'E. Peter Kuendig' 'Marta Pontini' ; L.Prins ; 'Thomas M. Seidel' data_SEID _database_code_depnum_ccdc_archive 'CCDC 629066' #-------------------------------------------------------------------- _audit_creation_date 2007-02-01 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 2007-02-01 _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.0.1 #-------------------------------------------------------------------- _chemical_formula_moiety ; (C13 H10 O)6 N2 O Ti2 , (C6 H6)2 , (C H Cl3)0.79 ; _chemical_formula_sum 'C90.79 H72.79 Cl2.36 N2 O7 Ti2' _chemical_formula_weight 1483.4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 13.2828(8) _cell_length_b 15.6644(7) _cell_length_c 18.5844(12) _cell_angle_alpha 90.00000 _cell_angle_beta 105.269(7) _cell_angle_gamma 90.00000 _cell_volume 3730.3(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.32 _exptl_crystal_density_meas nor_measured _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 25.9 _cell_measurement_temperature 200 _exptl_crystal_F_000 1543.4 _exptl_absorpt_coefficient_mu .36 _exptl_crystal_description prism _exptl_crystal_size_max .23 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .12 _exptl_crystal_colour yellow _diffrn_measurement_device_type 'Stoe Ipds' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 6 _exptl_absorpt_correction_type none _diffrn_reflns_number 27925 _reflns_number_total 7259 _reflns_number_gt 3203 _reflns_threshold_expression 'refl observed if Fo > 3.99 \s(Fo)' _diffrn_reflns_theta_max 25.9 _diffrn_reflns_theta_full 25.9 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .084 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .044 _refine_ls_wR_factor_ref .042 _refine_ls_goodness_of_fit_ref 1.33(2) _refine_ls_number_reflns 3234 _refine_ls_number_parameters 483 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.0003(Fo^2^)] _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .022 _refine_diff_density_max .835 _refine_diff_density_min -.722 _refine_ls_extinction_method none _refine_ls_abs_structure_details none _refine_special_details ; Disorders: All the molecules of solvent of inclusion (two molecules of benzene and one of chloroform by complex) are disordered. Both disordered benzene were located around a centre of inversion and have been refined with population parameters fixed to 0.5 and isotropic displacement parameters. The population parameter of the disordered chloroform molecule was refined and converged to a value of 0.394(5) ; _computing_data_collection 'EXPOSE (Stoe & Cie, 1999)' _computing_cell_refinement 'CELL (Stoe & Cie, 1999)' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution SIR97 _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal_gx3 _computing_publication_material xtal_CIFIO loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .002 .002 H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0 Cl Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .132 .159 N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .004 .003 O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .008 .006 Ti Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .248 .446 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ti .41807(6) .50615(6) .40619(4) .0215(4) 1.00000 Uani O1 .4753(3) .4195(2) .36528(16) .0302(17) 1.00000 Uani O2 .4486(3) .61505(19) .38550(16) .0324(18) 1.00000 Uani O3 .29410(18) .4884(3) .42734(14) .0309(16) 1.00000 Uani O4 .50000 .50000 .50000 .025(2) 1.00000 Uani N .3110(3) .5146(3) .28514(17) .0238(18) 1.00000 Uani C1 .4598(4) .3651(3) .3075(3) .026(3) 1.00000 Uani C2 .3657(4) .3677(3) .2512(3) .027(3) 1.00000 Uani C3 .3522(4) .3110(4) .1925(3) .036(3) 1.00000 Uani C4 .4291(5) .2528(4) .1886(3) .042(3) 1.00000 Uani C5 .5217(4) .2514(4) .2443(3) .037(3) 1.00000 Uani C6 .5401(4) .3071(3) .3044(3) .028(3) 1.00000 Uani C7 .6401(4) .3055(3) .3638(3) .027(3) 1.00000 Uani C8 .7338(4) .3010(4) .3440(3) .039(3) 1.00000 Uani C9 .8286(4) .2980(4) .3991(4) .051(4) 1.00000 Uani C10 .8298(4) .2999(4) .4723(4) .049(4) 1.00000 Uani C11 .7377(4) .3050(4) .4930(3) .041(3) 1.00000 Uani C12 .6429(4) .3072(3) .4388(3) .032(3) 1.00000 Uani C13 .2799(4) .4271(3) .2568(3) .028(3) 1.00000 Uani C14 .4430(4) .6726(4) .3308(3) .028(3) 1.00000 Uani C15 .3993(4) .6489(3) .2562(3) .027(3) 1.00000 Uani C16 .3938(4) .7094(4) .2019(3) .035(3) 1.00000 Uani C17 .4295(4) .7919(4) .2193(3) .038(3) 1.00000 Uani C18 .4710(4) .8140(4) .2925(3) .037(3) 1.00000 Uani C19 .4782(3) .7566(3) .3498(3) .027(3) 1.00000 Uani C20 .5207(4) .7798(3) .4297(3) .030(3) 1.00000 Uani C21 .4860(5) .8521(4) .4584(4) .051(4) 1.00000 Uani C22 .5245(6) .8725(4) .5343(5) .065(5) 1.00000 Uani C23 .5969(6) .8202(5) .5801(4) .061(4) 1.00000 Uani C24 .6326(4) .7496(4) .5521(3) .042(3) 1.00000 Uani C25 .5957(4) .7286(4) .4782(3) .036(3) 1.00000 Uani C26 .3670(4) .5576(4) .2367(3) .030(3) 1.00000 Uani C27 .1888(3) .4925(4) .4007(3) .026(3) 1.00000 Uani C28 .1464(4) .5259(3) .3288(3) .030(3) 1.00000 Uani C29 .0380(4) .5270(3) .3016(3) .033(3) 1.00000 Uani C30 -.0247(3) .4969(4) .3436(3) .038(3) 1.00000 Uani C31 .0182(4) .4638(3) .4142(3) .035(3) 1.00000 Uani C32 .1267(4) .4610(3) .4440(3) .028(3) 1.00000 Uani C33 .1730(4) .4227(4) .5187(3) .031(3) 1.00000 Uani C34 .1374(4) .3450(4) .5381(4) .043(4) 1.00000 Uani C35 .1790(5) .3091(4) .6068(4) .058(4) 1.00000 Uani C36 .2582(5) .3505(5) .6579(4) .057(4) 1.00000 Uani C37 .2942(4) .4278(4) .6401(3) .045(4) 1.00000 Uani C38 .2529(4) .4639(3) .5718(3) .034(3) 1.00000 Uani C39 .2155(4) .5641(4) .2851(3) .031(3) 1.00000 Uani C1a .4754(6) .5112(8) .0667(6) .095(5) .50000 Uiso C2a .4143(8) .4434(6) .0653(6) .098(5) .50000 Uiso C3a .3094(8) .4513(7) .0381(7) .090(5) .50000 Uiso C4a .2672(6) .5285(9) .0127(6) .092(6) .50000 Uiso C5a .3278(8) .5958(6) .0138(4) .065(4) .50000 Uiso C6a .4315(10) .5887(7) .0404(6) .113(6) .50000 Uiso C1b .7684(7) .5779(8) .0970(9) .111(6) .50000 Uiso C2b .7814(13) .5207(14) .1554(8) .28(3) .50000 Uiso C3b .7711(10) .4356(11) .1414(9) .117(6) .50000 Uiso C4b .7479(10) .4070(8) .0693(10) .128(7) .50000 Uiso C5b .7346(10) .4633(14) .0115(8) .26(2) .50000 Uiso C6b .7450(10) .5502(11) .0262(8) .165(9) .50000 Uiso Cl1c .5737(4) .6046(3) .1524(3) .070(3) .394(5) Uani Cl2c .6017(8) .4291(4) .1708(4) .168(6) .394(5) Uani Cl3c .7755(4) .5386(7) .1688(4) .162(7) .394(5) Uani C1c .6424(9) .5193(8) .1351(7) .055(4) .394(5) Uiso H3 .28695 .31207 .15278 .05000 1.00000 Uiso H4 .41794 .21278 .14669 .05000 1.00000 Uiso H5 .57568 .21007 .24119 .05000 1.00000 Uiso H8 .73354 .29988 .29121 .05000 1.00000 Uiso H9 .89440 .29444 .38472 .05000 1.00000 Uiso H10 .89645 .29761 .51064 .05000 1.00000 Uiso H11 .73898 .30707 .54596 .05000 1.00000 Uiso H12 .57752 .30991 .45379 .05000 1.00000 Uiso H131 .23244 .43271 .20674 .05000 1.00000 Uiso H132 .24269 .40075 .29015 .05000 1.00000 Uiso H16 .36388 .69386 .14949 .05000 1.00000 Uiso H17 .42512 .83405 .17971 .05000 1.00000 Uiso H18 .49627 .87244 .30435 .05000 1.00000 Uiso H21 .43426 .88925 .42563 .05000 1.00000 Uiso H22 .49981 .92390 .55446 .05000 1.00000 Uiso H23 .62283 .83391 .63327 .05000 1.00000 Uiso H24 .68528 .71336 .58509 .05000 1.00000 Uiso H25 .62180 .67720 .45904 .05000 1.00000 Uiso H261 .32157 .55698 .18572 .05000 1.00000 Uiso H262 .43032 .52454 .23851 .05000 1.00000 Uiso H29 .00630 .54978 .25162 .05000 1.00000 Uiso H30 -.10068 .49870 .32364 .05000 1.00000 Uiso H31 -.02777 .44210 .44356 .05000 1.00000 Uiso H34 .08133 .31518 .50201 .05000 1.00000 Uiso H35 .15250 .25432 .61953 .05000 1.00000 Uiso H36 .28886 .32470 .70682 .05000 1.00000 Uiso H37 .34995 .45740 .67678 .05000 1.00000 Uiso H38 .27937 .51898 .55974 .05000 1.00000 Uiso H391 .17422 .57012 .23319 .05000 1.00000 Uiso H392 .23744 .62071 .30589 .05000 1.00000 Uiso H1a .55118 .50599 .08634 .05000 .50000 Uiso H2a .44500 .38816 .08373 .05000 .50000 Uiso H3a .26407 .40163 .03683 .05000 .50000 Uiso H4a .19140 .53417 -.00653 .05000 .50000 Uiso H5a .29672 .65088 -.00487 .05000 .50000 Uiso H6a .47621 .63869 .04125 .05000 .50000 Uiso H1b .77639 .63919 .10746 .05000 .50000 Uiso H2b .79803 .54158 .20688 .05000 .50000 Uiso H3b .78016 .39497 .18273 .05000 .50000 Uiso H4b .74077 .34562 .05915 .05000 .50000 Uiso H5b .71785 .44254 -.04003 .05000 .50000 Uiso H6b .73532 .59115 -.01495 .05000 .50000 Uiso H1c .62711 .51231 .08091 .05000 .39368 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti .0204(4) .0220(5) .0204(4) -.0004(5) .0026(3) -.0000(5) O1 .0293(17) .030(3) .0259(18) .0054(14) -.0019(14) -.0061(16) O2 .0393(19) .026(2) .0255(18) -.0060(15) -.0032(14) .0041(16) O3 .0214(15) .041(3) .0284(15) -.0005(16) .0030(12) .0061(17) O4 .0203(19) .029(3) .027(2) -.001(3) .0052(16) .003(3) N .0230(17) .021(3) .0241(18) .0010(17) .0012(14) .0007(18) C1 .032(3) .023(3) .024(3) -.001(3) .006(3) -.001(3) C2 .035(3) .016(3) .028(3) -.004(3) .005(3) .001(3) C3 .038(3) .036(4) .028(3) -.003(3) -.002(3) -.007(3) C4 .059(4) .033(4) .035(4) .002(3) .013(3) -.014(3) C5 .041(3) .028(4) .042(4) .002(3) .012(3) -.008(3) C6 .034(3) .023(3) .030(3) .002(3) .011(3) -.001(3) C7 .028(3) .014(3) .037(3) -.001(2) .006(3) -.004(3) C8 .039(4) .035(4) .046(4) .000(3) .017(3) -.007(3) C9 .028(4) .056(5) .073(5) -.000(3) .019(4) .003(4) C10 .035(4) .053(5) .051(4) .000(3) -.002(3) .002(3) C11 .040(4) .042(4) .038(3) .004(3) .003(3) .005(3) C12 .027(3) .027(4) .040(3) .003(3) .006(3) .009(3) C13 .026(3) .032(4) .021(3) -.003(3) -.003(2) -.003(3) C14 .026(3) .030(4) .028(3) .002(3) .004(3) .008(3) C15 .029(3) .025(3) .028(3) .002(3) .008(3) .006(3) C16 .034(3) .040(4) .030(3) .006(3) .006(3) .011(3) C17 .047(4) .029(4) .040(4) .003(3) .014(3) .018(3) C18 .038(3) .025(4) .049(4) .001(3) .015(3) .007(3) C19 .022(3) .019(3) .039(3) .002(2) .007(2) .005(3) C20 .029(3) .024(3) .039(3) -.007(3) .009(3) .001(3) C21 .054(4) .029(4) .069(5) -.002(3) .013(4) -.006(4) C22 .089(6) .039(5) .074(5) -.012(4) .032(5) -.032(4) C23 .071(5) .065(5) .043(4) -.024(4) .007(4) -.021(4) C24 .050(4) .037(4) .032(4) -.016(3) -.000(3) -.006(3) C25 .034(3) .029(4) .043(4) -.011(3) .008(3) .001(3) C26 .033(3) .032(4) .022(3) -.001(3) .002(2) .003(3) C27 .018(2) .024(3) .034(3) .001(3) .0020(18) -.006(3) C28 .024(3) .023(4) .039(3) .0039(19) .003(2) -.002(3) C29 .027(3) .027(4) .041(3) .008(2) .000(3) -.003(3) C30 .019(2) .036(4) .056(3) .000(3) .006(2) -.010(4) C31 .024(3) .036(4) .048(4) -.001(2) .015(3) -.011(3) C32 .025(3) .023(3) .037(3) -.0001(19) .011(3) -.008(3) C33 .030(3) .027(4) .039(3) -.000(3) .016(3) .001(3) C34 .045(4) .034(4) .057(4) -.003(3) .024(3) .004(3) C35 .066(5) .046(5) .071(5) -.003(4) .034(4) .021(4) C36 .067(5) .065(5) .045(4) .013(4) .025(4) .023(4) C37 .044(4) .057(5) .036(4) .004(3) .012(3) .001(3) C38 .033(3) .035(4) .036(3) -.001(3) .015(3) .002(3) C39 .026(3) .032(4) .031(3) .009(3) -.001(3) .007(3) Cl1c .079(3) .055(4) .083(4) .002(3) .036(3) -.001(3) Cl2c .362(11) .054(4) .154(6) .043(5) .185(7) .033(4) Cl3c .054(3) .326(13) .087(4) .038(5) -.017(3) -.093(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance Ti O1 . . 1.818(4) Ti O2 . . 1.818(4) Ti O3 . . 1.812(3) Ti O4 . . 1.7983(7) Ti N . . 2.327(3) Ti Ti . 3_666 3.5965(10) O1 C1 . . 1.344(6) O2 C14 . . 1.346(6) O3 C27 . . 1.357(4) N C13 . . 1.488(6) N C26 . . 1.474(6) N C39 . . 1.486(6) C1 C2 . . 1.403(6) C1 C6 . . 1.414(7) C2 C3 . . 1.382(7) C2 C13 . . 1.495(7) C3 C4 . . 1.385(8) C4 C5 . . 1.383(7) C5 C6 . . 1.387(7) C6 C7 . . 1.486(6) C7 C8 . . 1.390(8) C7 C12 . . 1.386(7) C8 C9 . . 1.398(7) C9 C10 . . 1.358(10) C10 C11 . . 1.378(9) C11 C12 . . 1.391(6) C14 C15 . . 1.405(7) C14 C19 . . 1.410(7) C15 C16 . . 1.372(7) C15 C26 . . 1.510(7) C16 C17 . . 1.385(8) C17 C18 . . 1.370(7) C18 C19 . . 1.378(7) C19 C20 . . 1.487(7) C20 C21 . . 1.382(8) C20 C25 . . 1.405(7) C21 C22 . . 1.405(10) C22 C23 . . 1.375(9) C23 C24 . . 1.361(9) C24 C25 . . 1.371(7) C27 C28 . . 1.405(6) C27 C32 . . 1.387(7) C28 C29 . . 1.396(6) C28 C39 . . 1.502(7) C29 C30 . . 1.367(7) C30 C31 . . 1.386(7) C31 C32 . . 1.402(6) C32 C33 . . 1.489(7) C33 C34 . . 1.388(8) C33 C38 . . 1.401(6) C34 C35 . . 1.370(9) C35 C36 . . 1.380(9) C36 C37 . . 1.375(10) C37 C38 . . 1.366(7) C1a C2a . . 1.332(15) C1a C6a . . 1.379(16) C2a C3a . . 1.357(14) C3a C4a . . 1.364(16) C4a C5a . . 1.322(15) C5a C6a . . 1.340(15) C1b C2b . . 1.38(3) C1b C6b . . 1.34(3) C2b C3b . . 1.36(3) C3b C4b . . 1.37(3) C4b C5b . . 1.37(3) C5b C6b . . 1.39(3) Cl1c C1c . . 1.695(13) Cl2c C1c . . 1.707(14) Cl3c C1c . . 1.739(12) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle O1 Ti O2 . . . 118.11(16) O1 Ti O3 . . . 118.70(15) O1 Ti O4 . . . 98.77(9) O1 Ti N . . . 81.64(13) O1 Ti Ti . . 3_666 98.77(9) O2 Ti O3 . . . 117.14(15) O2 Ti O4 . . . 98.25(10) O2 Ti N . . . 81.72(13) O2 Ti Ti . . 3_666 98.25(9) O3 Ti O4 . . . 97.70(8) O3 Ti N . . . 81.91(12) O3 Ti Ti . . 3_666 97.70(8) O4 Ti N . . . 179.54(9) O4 Ti Ti . . 3_666 .00000 N Ti Ti . . 3_666 179.54(9) Ti O1 C1 . . . 144.6(3) Ti O2 C14 . . . 144.8(3) Ti O3 C27 . . . 145.2(3) Ti O4 Ti . . 3_666 180.0000 Ti N C13 . . . 109.4(3) Ti N C26 . . . 109.8(3) Ti N C39 . . . 109.6(3) C13 N C26 . . . 110.0(4) C13 N C39 . . . 108.9(3) C26 N C39 . . . 109.2(4) O1 C1 C2 . . . 119.7(4) O1 C1 C6 . . . 118.8(4) C2 C1 C6 . . . 121.5(5) C1 C2 C3 . . . 118.3(5) C1 C2 C13 . . . 120.9(4) C3 C2 C13 . . . 120.8(4) C2 C3 C4 . . . 121.4(4) C3 C4 C5 . . . 119.5(5) C4 C5 C6 . . . 121.8(5) C1 C6 C5 . . . 117.4(4) C1 C6 C7 . . . 121.1(4) C5 C6 C7 . . . 121.4(5) C6 C7 C8 . . . 119.5(5) C6 C7 C12 . . . 121.9(5) C8 C7 C12 . . . 118.6(4) C7 C8 C9 . . . 120.3(6) C8 C9 C10 . . . 120.2(6) C9 C10 C11 . . . 120.3(5) C10 C11 C12 . . . 120.0(5) C7 C12 C11 . . . 120.5(5) N C13 C2 . . . 116.9(4) O2 C14 C15 . . . 119.6(4) O2 C14 C19 . . . 119.2(4) C15 C14 C19 . . . 121.1(5) C14 C15 C16 . . . 118.2(5) C14 C15 C26 . . . 120.3(4) C16 C15 C26 . . . 121.4(4) C15 C16 C17 . . . 121.5(5) C16 C17 C18 . . . 119.5(5) C17 C18 C19 . . . 122.0(5) C14 C19 C18 . . . 117.7(5) C14 C19 C20 . . . 119.4(5) C18 C19 C20 . . . 122.9(5) C19 C20 C21 . . . 120.5(5) C19 C20 C25 . . . 121.4(5) C21 C20 C25 . . . 118.2(5) C20 C21 C22 . . . 120.2(5) C21 C22 C23 . . . 119.8(7) C22 C23 C24 . . . 120.3(6) C23 C24 C25 . . . 120.6(5) C20 C25 C24 . . . 120.8(5) N C26 C15 . . . 116.3(4) O3 C27 C28 . . . 118.8(4) O3 C27 C32 . . . 119.0(4) C28 C27 C32 . . . 122.2(4) C27 C28 C29 . . . 117.8(5) C27 C28 C39 . . . 120.9(4) C29 C28 C39 . . . 121.2(4) C28 C29 C30 . . . 120.9(4) C29 C30 C31 . . . 120.7(4) C30 C31 C32 . . . 120.6(5) C27 C32 C31 . . . 117.8(4) C27 C32 C33 . . . 121.5(4) C31 C32 C33 . . . 120.6(5) C32 C33 C34 . . . 120.7(4) C32 C33 C38 . . . 121.4(5) C34 C33 C38 . . . 117.9(5) C33 C34 C35 . . . 121.4(5) C34 C35 C36 . . . 119.7(6) C35 C36 C37 . . . 120.0(6) C36 C37 C38 . . . 120.5(5) C33 C38 C37 . . . 120.6(5) N C39 C28 . . . 115.7(4) C2a C1a C6a . . . 119.8(9) C1a C2a C3a . . . 119.7(9) C2a C3a C4a . . . 119.8(10) C3a C4a C5a . . . 120.6(8) C4a C5a C6a . . . 120.1(10) C1a C6a C5a . . . 120.0(10) C2b C1b C6b . . . 120.6(14) C1b C2b C3b . . . 120.1(14) C2b C3b C4b . . . 119.6(14) C3b C4b C5b . . . 120.5(14) C4b C5b C6b . . . 119.6(14) C1b C6b C5b . . . 119.7(14) Cl1c C1c Cl2c . . . 109.7(8) Cl1c C1c Cl3c . . . 110.0(7) Cl2c C1c Cl3c . . . 113.5(8) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion C26 N C13 C2 . . . . 59.2(5) C39 N C13 C2 . . . . 178.8(4) C13 N C26 C15 . . . . 177.2(4) C39 N C26 C15 . . . . 57.7(4) C13 N C39 C28 . . . . 56.7(5) C26 N C39 C28 . . . . 176.8(4) O1 C1 C2 C3 . . . . 179.9(5) O1 C1 C2 C13 . . . . -3.3(7) C6 C1 C2 C3 . . . . .8(8) C6 C1 C2 C13 . . . . 177.6(5) O1 C1 C6 C5 . . . . 179.7(5) O1 C1 C6 C7 . . . . .1(7) C2 C1 C6 C5 . . . . -1.2(8) C2 C1 C6 C7 . . . . 179.2(5) C1 C2 C3 C4 . . . . .0(8) C13 C2 C3 C4 . . . . -176.7(5) C1 C2 C13 N . . . . 40.9(7) C3 C2 C13 N . . . . -142.4(5) C2 C3 C4 C5 . . . . -.4(9) C3 C4 C5 C6 . . . . .0(9) C4 C5 C6 C1 . . . . .8(8) C4 C5 C6 C7 . . . . -179.6(5) C1 C6 C7 C8 . . . . -135.0(5) C1 C6 C7 C12 . . . . 46.0(7) C5 C6 C7 C8 . . . . 45.4(7) C5 C6 C7 C12 . . . . -133.6(6) C6 C7 C8 C9 . . . . -178.9(5) C12 C7 C8 C9 . . . . .2(8) C6 C7 C12 C11 . . . . 179.5(5) C8 C7 C12 C11 . . . . .5(7) C7 C8 C9 C10 . . . . -.3(9) C8 C9 C10 C11 . . . . -.1(9) C9 C10 C11 C12 . . . . .8(9) C10 C11 C12 C7 . . . . -.9(8) O2 C14 C15 C16 . . . . 179.3(5) O2 C14 C15 C26 . . . . -5.1(7) C19 C14 C15 C16 . . . . 1.4(7) C19 C14 C15 C26 . . . . 177.0(5) O2 C14 C19 C18 . . . . -179.7(5) O2 C14 C19 C20 . . . . .0(7) C15 C14 C19 C18 . . . . -1.8(7) C15 C14 C19 C20 . . . . 178.0(5) C14 C15 C16 C17 . . . . -.3(8) C26 C15 C16 C17 . . . . -175.9(5) C14 C15 C26 N . . . . 43.4(6) C16 C15 C26 N . . . . -141.2(5) C15 C16 C17 C18 . . . . -.3(8) C16 C17 C18 C19 . . . . -.2(8) C17 C18 C19 C14 . . . . 1.2(8) C17 C18 C19 C20 . . . . -178.6(5) C14 C19 C20 C21 . . . . -130.7(6) C14 C19 C20 C25 . . . . 48.3(7) C18 C19 C20 C21 . . . . 49.0(7) C18 C19 C20 C25 . . . . -132.0(6) C19 C20 C21 C22 . . . . 178.4(6) C25 C20 C21 C22 . . . . -.6(9) C19 C20 C25 C24 . . . . -178.6(5) C21 C20 C25 C24 . . . . .4(8) C20 C21 C22 C23 . . . . -.1(11) C21 C22 C23 C24 . . . . 1.1(11) C22 C23 C24 C25 . . . . -1.3(10) C23 C24 C25 C20 . . . . .5(9) O3 C27 C28 C29 . . . . 178.0(4) O3 C27 C28 C39 . . . . -5.9(7) C32 C27 C28 C29 . . . . .4(7) C32 C27 C28 C39 . . . . 176.5(5) O3 C27 C32 C31 . . . . -178.2(5) O3 C27 C32 C33 . . . . -.2(7) C28 C27 C32 C31 . . . . -.5(7) C28 C27 C32 C33 . . . . 177.5(5) C27 C28 C29 C30 . . . . .1(7) C39 C28 C29 C30 . . . . -175.9(5) C27 C28 C39 N . . . . 45.1(6) C29 C28 C39 N . . . . -139.0(4) C28 C29 C30 C31 . . . . -.5(8) C29 C30 C31 C32 . . . . .3(8) C30 C31 C32 C27 . . . . .2(8) C30 C31 C32 C33 . . . . -177.8(5) C27 C32 C33 C34 . . . . -132.2(6) C27 C32 C33 C38 . . . . 48.4(7) C31 C32 C33 C34 . . . . 45.7(7) C31 C32 C33 C38 . . . . -133.7(6) C32 C33 C34 C35 . . . . -179.7(6) C38 C33 C34 C35 . . . . -.3(9) C32 C33 C38 C37 . . . . 179.8(5) C34 C33 C38 C37 . . . . .4(8) C33 C34 C35 C36 . . . . -.3(10) C34 C35 C36 C37 . . . . .8(11) C35 C36 C37 C38 . . . . -.8(10) C36 C37 C38 C33 . . . . .2(9) C6a C1a C2a C3a . . . . -.2(17) C2a C1a C6a C5a . . . . .2(16) C1a C2a C3a C4a . . . . -.2(17) C2a C3a C4a C5a . . . . .4(17) C3a C4a C5a C6a . . . . -.4(16) C4a C5a C6a C1a . . . . .1(15) C6b C1b C2b C3b . . . . 0(3) C2b C1b C6b C5b . . . . -.5(19) C1b C2b C3b C4b . . . . 0(3) C2b C3b C4b C5b . . . . 0(3) C3b C4b C5b C6b . . . . 0(2) C4b C5b C6b C1b . . . . 0(2) #=END==================================================================