Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_name 'Dr Gerald Bernardinelli' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address S.G.Telfer ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; A.F.Williams ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; G.Bernardinelli ; Laboratoiry of X-ray Crystallography University de Geneva 24, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; _publ_contact_author_address ; Dr Gerald Bernardinelli Laboratoire de Cristallographie Universite de Geneve 24, quai E. Ansermet CH - 1211 Geneve 4 Switzerland ; _publ_contact_author_email gerald.bernardinelli@cryst.unige.ch _publ_contact_author_fax '41 (22) 702 61 08' _publ_contact_author_phone '41 (22) 702 62 02' data_FLET _database_code_CSD 193595 _audit_creation_date 2001-01-23 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 2001-11-19 _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.0.1 _publ_section_title ; Iron and Cobalt Complexes of 5,5'-di(methylene-N-aminoacidyl)- 2,2'-Bipyridyl Ligands: Ligand Design for Diastereoselectivity and Anion Binding. ; _chemical_name_systematic ; tris(5,5'-di(methyl-N-valine)-2,2'-bipyridyl)cobalt(III)dichloride heptaperchlorate dodecahydrate diethanol ; _chemical_formula_moiety ; Co (C22 H32 N4 O4)3 Cl2 (Cl O4)7 (H2 O)12 (C2 H6 O)2 ; _chemical_formula_sum 'C70 H132 N12 O54 Cl9 Co' _chemical_formula_weight 2384.1 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' 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 14.4363(9) _cell_length_b 20.2358(8) _cell_length_c 20.0112(14) _cell_angle_alpha 90.00000 _cell_angle_beta 110.184(8) _cell_angle_gamma 90.00000 _cell_volume 5486.9(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_meas not_measured _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8001 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 26.0 _cell_measurement_temperature 200 _exptl_absorpt_coefficient_mu .47 _exptl_crystal_description prism _exptl_crystal_size_max .32 _exptl_crystal_size_mid .17 _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 numerical _exptl_absorpt_process_details 'XRED; Stoe & Cie, 1999' _exptl_absorpt_correction_T_min .8811 _exptl_absorpt_correction_T_max .9580 _diffrn_reflns_number 34570 _reflns_number_total 10617 _reflns_number_gt 7000 _reflns_threshold_expression 'refl observed if Fo > 4.0 \s(Fo)' _diffrn_reflns_theta_max 25.97 _diffrn_reflns_av_R_equivalents .058 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .051 _refine_ls_wR_factor_ref .057 _refine_ls_goodness_of_fit_ref 2.39 _refine_ls_number_reflns 7000 _refine_ls_number_parameters 657 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.0002(Fo^2^)] _refine_ls_shift/su_max .00029 _refine_diff_density_max .686 _refine_diff_density_min -.555 _refine_ls_extinction_method none _refine_ls_abs_structure_details Flack_xabs_refined _refine_ls_abs_structure_Flack -.00(3) _refine_special_details ; Calculated excepted for H of OH groups which are refined with restraints on bond lengths and bond angles and blocked on the last cycles ; _computing_data_collection 'EXPOSE (Stoe & Cie, 1999)' _computing_cell_refinement 'CELL (Stoe & Cie, 1999)' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution Multan_87 _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal_gx3 _computing_publication_material xtal_BONDLA_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 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 Cl Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .132 .159 Co Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .299 .973 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 Co .50000 .50000 .00000 .0318(7) 1.00000 Uani O1a 1.1117(5) .5536(4) .1332(4) .060(4) 1.00000 Uani O2a 1.1626(5) .6457(4) .1990(4) .059(4) 1.00000 Uani O3a .2044(6) .2447(4) -.3363(4) .066(5) 1.00000 Uani O4a .0613(7) .2137(5) -.3294(6) .098(6) 1.00000 Uani N1a .6344(4) .4984(5) -.0012(3) .036(3) 1.00000 Uani N2a .4778(6) .4312(4) -.0706(4) .032(4) 1.00000 Uani N3a .9324(5) .5549(4) .1441(4) .041(4) 1.00000 Uani N4a .2223(5) .3489(4) -.2486(4) .041(4) 1.00000 Uani C1a .7081(6) .5373(5) .0350(5) .038(4) 1.00000 Uani C2a .8011(6) .5347(5) .0278(5) .042(5) 1.00000 Uani C3a .8143(6) .4876(6) -.0199(5) .048(5) 1.00000 Uani C4a .7393(7) .4468(5) -.0564(5) .048(5) 1.00000 Uani C5a .6479(6) .4525(5) -.0466(5) .036(4) 1.00000 Uani C6a .5600(6) .4131(5) -.0867(5) .036(4) 1.00000 Uani C7a .5577(6) .3641(5) -.1341(5) .041(4) 1.00000 Uani C8a .4699(8) .3304(5) -.1673(6) .043(5) 1.00000 Uani C9a .3863(6) .3483(4) -.1524(5) .036(4) 1.00000 Uani C10a .3931(6) .3981(4) -.1032(4) .034(4) 1.00000 Uani C11a .8806(6) .5812(5) .0695(5) .048(5) 1.00000 Uani C12a 1.0085(6) .6027(5) .1908(5) .041(5) 1.00000 Uani C13a 1.0993(7) .5979(5) .1705(5) .047(5) 1.00000 Uani C14a 1.0268(7) .5859(6) .2695(6) .056(6) 1.00000 Uani C15a 1.0809(10) .5216(6) .2916(6) .078(7) 1.00000 Uani C16a 1.0813(8) .6423(6) .3207(6) .066(7) 1.00000 Uani C17a .2897(7) .3123(5) -.1839(5) .044(5) 1.00000 Uani C18a .1227(7) .3175(5) -.2798(5) .048(5) 1.00000 Uani C19a .1357(8) .2543(6) -.3178(6) .058(6) 1.00000 Uani C20a .0505(7) .3661(6) -.3309(6) .066(6) 1.00000 Uani C21a .0746(11) .3816(8) -.3964(8) .092(9) 1.00000 Uani C22a -.0563(9) .3426(8) -.3511(8) .098(9) 1.00000 Uani O1b .7188(7) .7087(5) .3811(5) .079(5) 1.00000 Uani O2b .7079(8) .6553(6) .4741(5) .101(7) 1.00000 Uani N1b .5249(6) .5712(5) .0694(5) .038(5) 1.00000 Uani N2b .6857(6) .6031(4) .2990(4) .046(4) 1.00000 Uani C1b .5449(6) .5644(5) .1393(5) .041(5) 1.00000 Uani C2b .5542(6) .6209(5) .1833(5) .046(5) 1.00000 Uani C3b .5414(8) .6828(6) .1513(6) .053(6) 1.00000 Uani C4b .5188(7) .6889(5) .0795(6) .053(6) 1.00000 Uani C5b .5125(6) .6332(5) .0391(5) .042(5) 1.00000 Uani C6b .5766(7) .6110(6) .2615(6) .053(6) 1.00000 Uani C7b .7113(7) .5908(6) .3770(5) .051(5) 1.00000 Uani C8b .7104(8) .6588(7) .4109(6) .058(6) 1.00000 Uani C9b .8105(8) .5548(7) .4069(6) .066(7) 1.00000 Uani C10b .8944(9) .5986(8) .4055(7) .081(8) 1.00000 Uani C11b .8283(10) .5275(8) .4810(7) .088(8) 1.00000 Uani Cl1 .77950(12) .50215(17) .21804(10) .0438(9) 1.00000 Uani Cl1c .78530(18) .72437(14) .18548(16) .0648(15) 1.00000 Uani O1c .7689(8) .6593(5) .1539(7) .101(7) 1.00000 Uani O2c .8882(6) .7392(5) .2103(6) .094(6) 1.00000 Uani O3c .7330(7) .7723(5) .1332(6) .108(7) 1.00000 Uani O4c .7495(7) .7265(6) .2430(5) .103(7) 1.00000 Uani Cl1d .06078(19) .37107(14) -.10708(14) .0595(13) 1.00000 Uani O1d .1471(7) .3937(4) -.1214(5) .085(6) 1.00000 Uani O2d .0018(8) .3303(5) -.1629(5) .092(6) 1.00000 Uani O3d .0904(7) .3357(5) -.0411(5) .083(5) 1.00000 Uani O4d .0041(6) .4276(4) -.1009(5) .068(5) 1.00000 Uani Cl1e .5863(3) .41078(17) .33397(16) .0713(17) 1.00000 Uani O1e .4881(7) .3918(8) .3117(6) .150(10) 1.00000 Uani O2e .5960(10) .4569(6) .2840(6) .119(8) 1.00000 Uani O3e .6511(8) .3597(7) .3368(6) .123(8) 1.00000 Uani O4e .6068(10) .4414(6) .4021(6) .119(8) 1.00000 Uani Cl1f .50000 .23175(19) .00000 .062(2) 1.00000 Uani O1f .4257(9) .2742(7) .0017(6) .143(9) 1.00000 Uani O2f .5398(10) .1956(8) .0593(8) .198(12) 1.00000 Uani O1g .407(3) .5912(15) .3462(16) .143(9) .50000 Uiso O1g' .450(3) .6152(19) .4168(18) .164(11) .50000 Uiso C1g .4004(14) .5672(10) .4027(8) .117(12) 1.00000 Uani C2g .3735(18) .509(3) .422(3) .26(3) 1.00000 Uani O1w .3637(6) .5090(8) .2165(6) .113(7) 1.00000 Uani O2w .2128(8) .4154(7) .2029(6) .114(8) 1.00000 Uani O3w .3191(6) .6424(6) .1665(6) .097(6) 1.00000 Uani O4w .2721(7) .7108(6) .0360(6) .105(7) 1.00000 Uani O5w .7711(14) .2686(8) .4712(7) .172(12) 1.00000 Uani O6w .696(3) .3627(17) .5230(15) .157(10) .50000 Uiso O7w .3162(17) .3352(12) .3417(12) .114(7) .50000 Uiso H02a 1.22422 .64286 .17851 .05000 1.00000 Uiso H04a .06515 .17601 -.36803 .05000 1.00000 Uiso H1a .69606 .57294 .07195 .05000 1.00000 Uiso H3a .88526 .48387 -.02758 .05000 1.00000 Uiso H4a .74990 .41005 -.09284 .05000 1.00000 Uiso H7a .62388 .35170 -.14590 .05000 1.00000 Uiso H8a .46682 .29037 -.20454 .05000 1.00000 Uiso H9a .32769 .41092 -.09051 .05000 1.00000 Uiso H111a .93425 .58670 .04260 .05000 1.00000 Uiso H112a .84800 .62911 .07272 .05000 1.00000 Uiso H031a .87719 .54546 .16878 .05000 1.00000 Uiso H032a .96944 .50886 .14037 .05000 1.00000 Uiso H12a .98358 .65393 .18327 .05000 1.00000 Uiso H14a .95383 .58047 .27368 .05000 1.00000 Uiso H151a 1.15533 .52651 .29011 .05000 1.00000 Uiso H152a 1.08480 .50949 .34560 .05000 1.00000 Uiso H153a 1.04260 .48201 .25572 .05000 1.00000 Uiso H161a 1.08526 .63024 .37468 .05000 1.00000 Uiso H162a 1.15579 .64726 .31919 .05000 1.00000 Uiso H163a 1.04212 .68894 .30467 .05000 1.00000 Uiso H171a .30364 .26280 -.19966 .05000 1.00000 Uiso H172a .25390 .30881 -.14413 .05000 1.00000 Uiso H041a .21280 .39935 -.23299 .05000 1.00000 Uiso H042a .25706 .34982 -.28910 .05000 1.00000 Uiso H18a .09179 .30497 -.23885 .05000 1.00000 Uiso H20a .05916 .41216 -.30112 .05000 1.00000 Uiso H211a .06441 .33734 -.42918 .05000 1.00000 Uiso H212a .02529 .42041 -.42650 .05000 1.00000 Uiso H213a .15074 .39838 -.38200 .05000 1.00000 Uiso H221a -.10559 .38139 -.38121 .05000 1.00000 Uiso H222a -.06647 .29832 -.38389 .05000 1.00000 Uiso H223a -.07378 .33134 -.30357 .05000 1.00000 Uiso H02b .71205 .70480 .49675 .05000 1.00000 Uiso H1b .55409 .51517 .16288 .05000 1.00000 Uiso H3b .54938 .72695 .18401 .05000 1.00000 Uiso H4b .50595 .73757 .05460 .05000 1.00000 Uiso H61b .54451 .65589 .27426 .05000 1.00000 Uiso H62b .52866 .56913 .26042 .05000 1.00000 Uiso H021b .71147 .56141 .27564 .05000 1.00000 Uiso H022b .72272 .64805 .29176 .05000 1.00000 Uiso H7b .65867 .55839 .38875 .05000 1.00000 Uiso H9b .80730 .51264 .37233 .05000 1.00000 Uiso H101b .90153 .63965 .44226 .05000 1.00000 Uiso H102b .96241 .56988 .42227 .05000 1.00000 Uiso H103b .88159 .61823 .35237 .05000 1.00000 Uiso H111b .89632 .49876 .49773 .05000 1.00000 Uiso H112b .83544 .56853 .51772 .05000 1.00000 Uiso H113b .76766 .49585 .48199 .05000 1.00000 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 Co .0284(7) .0262(8) .0386(8) .00000 .0088(6) .00000 O1a .045(4) .054(5) .087(5) -.005(3) .032(4) -.016(4) O2a .045(4) .065(5) .068(5) -.020(4) .020(4) -.010(4) O3a .061(5) .068(6) .064(5) .006(4) .018(4) -.019(4) O4a .081(6) .066(6) .146(8) -.031(5) .039(6) -.044(6) N1a .032(3) .035(4) .036(3) -.001(5) .006(3) .004(5) N2a .030(4) .028(5) .036(5) .005(4) .009(4) .006(4) N3a .031(4) .044(5) .047(5) -.005(3) .013(4) .001(4) N4a .041(4) .030(5) .040(4) .003(3) .000(3) -.004(3) C1a .033(5) .034(5) .044(5) -.001(4) .010(4) .007(4) C2a .033(5) .051(6) .043(5) -.000(4) .013(4) .010(5) C3a .033(4) .067(9) .042(5) .002(5) .013(4) .008(5) C4a .038(5) .058(7) .048(6) .005(5) .015(5) .001(5) C5a .034(4) .039(5) .030(5) .001(4) .007(4) .003(4) C6a .035(4) .032(5) .041(5) .004(4) .012(4) .007(4) C7a .040(5) .042(5) .042(5) .007(4) .015(4) -.002(5) C8a .042(6) .037(6) .045(6) .010(5) .008(5) -.007(5) C9a .038(5) .033(5) .034(5) .001(4) .006(4) -.003(4) C10a .037(4) .027(5) .036(5) -.003(4) .012(4) .004(4) C11a .037(5) .052(6) .050(6) -.010(4) .008(4) .011(5) C12a .030(4) .037(6) .053(6) -.005(4) .011(4) .002(4) C13a .037(5) .045(6) .059(6) -.008(4) .014(5) .008(5) C14a .051(6) .065(7) .052(6) -.012(5) .019(5) .003(5) C15a .091(8) .069(10) .060(7) -.013(6) .009(6) .018(6) C16a .060(7) .069(8) .063(7) -.017(6) .015(6) -.009(6) C17a .049(5) .034(5) .043(5) -.005(4) .009(4) -.003(4) C18a .044(5) .043(6) .049(6) -.000(4) .004(4) -.004(4) C19a .060(7) .051(7) .049(6) -.010(5) .003(5) -.006(5) C20a .048(6) .057(7) .072(7) .008(6) -.007(5) -.012(6) C21a .084(10) .078(10) .079(9) .014(8) -.016(8) .014(7) C22a .050(7) .111(12) .108(11) .018(7) -.004(7) -.031(9) O1b .105(7) .065(6) .069(5) -.001(5) .029(5) -.023(5) O2b .139(9) .113(8) .077(7) -.003(7) .069(6) -.023(6) N1b .026(4) .035(6) .047(6) .000(4) .005(4) -.001(4) N2b .049(5) .043(5) .045(5) -.002(4) .017(4) -.010(4) C1b .030(4) .041(6) .048(6) -.001(4) .010(4) -.015(4) C2b .029(4) .053(7) .052(6) -.001(4) .007(4) -.021(5) C3b .042(6) .046(7) .064(8) .004(5) .008(5) -.019(5) C4b .050(6) .023(5) .077(8) .009(4) .011(5) -.001(5) C5b .033(5) .030(5) .056(5) .002(4) .005(4) -.004(4) C6b .039(5) .061(7) .060(7) -.002(5) .017(5) -.021(5) C7b .049(6) .060(7) .045(6) -.007(5) .017(5) -.012(5) C8b .063(7) .069(8) .046(6) -.008(6) .022(5) -.011(6) C9b .069(7) .081(9) .046(6) .007(6) .014(5) -.007(6) C10b .052(7) .117(13) .071(8) .001(7) .016(6) .010(8) C11b .080(8) .106(12) .070(8) -.010(7) .014(6) .007(7) Cl1 .0439(10) .0372(10) .0536(11) -.0015(14) .0209(8) -.0028(14) Cl1c .0551(14) .0466(15) .103(3) .0022(12) .0403(14) .0107(14) O1c .107(7) .049(6) .172(10) -.009(5) .077(7) -.027(6) O2c .055(5) .074(7) .157(9) -.001(4) .044(5) .025(6) O3c .085(6) .077(7) .151(9) .009(5) .024(6) .046(6) O4c .098(7) .139(9) .092(7) -.033(7) .059(6) -.009(6) Cl1d .0721(15) .0396(14) .0760(16) -.0099(12) .0371(13) -.0042(12) O1d .097(6) .068(6) .123(7) -.025(5) .081(6) -.016(5) O2d .129(8) .060(6) .091(6) -.038(6) .045(6) -.020(5) O3d .099(7) .068(6) .086(6) .003(5) .037(5) .027(5) O4d .067(5) .043(5) .096(6) .006(4) .030(4) -.003(4) Cl1e .0719(18) .075(2) .0716(18) -.0108(15) .0312(14) -.0135(15) O1e .062(6) .277(19) .118(8) -.049(8) .039(6) .019(10) O2e .192(12) .079(7) .112(8) -.040(7) .086(8) -.013(6) O3e .119(9) .165(11) .096(7) .053(8) .052(7) .007(8) O4e .167(11) .111(9) .090(7) -.026(8) .058(7) -.041(6) Cl1f .068(3) .051(3) .058(3) .00000 .0099(18) .00000 O1f .136(10) .158(11) .119(9) .055(9) .023(8) -.058(8) O2f .136(10) .204(16) .183(13) -.046(10) -.035(9) .158(13) C1g .163(16) .133(14) .068(9) -.073(13) .055(10) .005(9) C2g .128(17) .24(4) .41(5) .01(3) .08(3) .16(5) O1w .071(5) .121(10) .131(7) -.002(7) .015(5) -.026(8) O2w .102(7) .132(10) .120(8) .019(7) .054(6) .015(7) O3w .051(5) .126(9) .122(8) -.018(5) .042(5) -.004(6) O4w .086(7) .115(9) .114(8) -.011(6) .035(6) .019(7) O5w .278(19) .143(12) .096(8) .001(12) .066(10) .044(8) 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 _geom_bond_publ_flag Co Cl1 . . 4.8137(15) . Co N1a . . 1.949(6) . Co N2a . . 1.930(8) . Co N1b . . 1.947(9) . Co N1a . 2_655 1.949(6) . Co N2a . 2_655 1.930(8) . Co N1b . 2_655 1.947(9) . O1a C13a . . 1.219(13) . O2a C13a . . 1.318(11) . O2a H02a . . 1.101(8) . O3a C19a . . 1.188(16) . O4a C19a . . 1.307(14) . O4a H04a . . 1.101(11) . N1a C1a . . 1.320(11) . N1a C5a . . 1.361(12) . N2a C6a . . 1.381(13) . N2a C10a . . 1.349(10) . N3a C11a . . 1.517(11) . N3a C12a . . 1.519(10) . N4a C17a . . 1.517(10) . N4a C18a . . 1.498(11) . C1a C2a . . 1.399(13) . C2a C3a . . 1.406(14) . C2a C11a . . 1.496(12) . C3a C4a . . 1.357(12) . C4a C5a . . 1.403(13) . C5a C6a . . 1.479(11) . C6a C7a . . 1.364(13) . C7a C8a . . 1.390(12) . C8a C9a . . 1.389(15) . C9a C10a . . 1.387(12) . C9a C17a . . 1.506(12) . C12a C13a . . 1.504(14) . C12a C14a . . 1.542(14) . C14a C15a . . 1.504(16) . C14a C16a . . 1.554(15) . C18a C19a . . 1.532(15) . C18a C20a . . 1.537(13) . C20a C21a . . 1.50(3) . C20a C22a . . 1.529(16) . O1b C8b . . 1.199(16) . O2b C8b . . 1.280(16) . O2b H02b . . 1.093(11) . N1b C1b . . 1.335(13) . N1b C5b . . 1.378(12) . N2b C6b . . 1.501(11) . N2b C7b . . 1.494(12) . C1b C2b . . 1.420(14) . C2b C3b . . 1.388(16) . C2b C6b . . 1.498(15) . C3b C4b . . 1.365(17) . C4b C5b . . 1.373(14) . C5b C5b . 2_655 1.479(14) . C7b C8b . . 1.536(17) . C7b C9b . . 1.532(15) . C9b C10b . . 1.508(19) . C9b C11b . . 1.519(18) . Cl1c O1c . . 1.445(10) . Cl1c O2c . . 1.427(9) . Cl1c O3c . . 1.435(10) . Cl1c O4c . . 1.415(12) . Cl1d O1d . . 1.445(11) . Cl1d O2d . . 1.413(9) . Cl1d O3d . . 1.432(9) . Cl1d O4d . . 1.437(9) . Cl1e O1e . . 1.385(11) . Cl1e O2e . . 1.410(13) . Cl1e O3e . . 1.381(14) . Cl1e O4e . . 1.432(12) . Cl1f O1f . . 1.385(15) . Cl1f O2f . . 1.343(15) . Cl1f O1f . 2_655 1.385(15) . Cl1f O2f . 2_655 1.343(15) . 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 _geom_angle_publ_flag Cl1 Co Cl1 1_555 1_555 2_655 178.96(6) . N1a Co N2a . . . 83.9(4) . N1a Co N1b . . . 94.7(4) . N1a Co N1a . . 2_655 178.1(5) . N1a Co N2a . . 2_655 94.7(4) . N1a Co N1b . . 2_655 86.7(4) . N2a Co N1b . . . 177.9(4) . N2a Co N1a . . 2_655 94.7(4) . N2a Co N2a . . 2_655 87.7(4) . N2a Co N1b . . 2_655 93.9(4) . N1b Co N1a . . 2_655 86.7(4) . N1b Co N2a . . 2_655 93.9(4) . N1b Co N1b . . 2_655 84.5(4) . N1a Co N2a 2_655 . 2_655 83.9(4) . N1a Co N1b 2_655 . 2_655 94.7(4) . N2a Co N1b 2_655 . 2_655 177.9(4) . C13a O2a H02a . . . 109.2(8) . C19a O4a H04a . . . 108.8(11) . Co N1a C1a . . . 127.0(7) . Co N1a C5a . . . 113.0(6) . C1a N1a C5a . . . 119.9(7) . Co N2a C6a . . . 115.0(6) . Co N2a C10a . . . 127.3(7) . C6a N2a C10a . . . 117.7(8) . C11a N3a C12a . . . 112.9(7) . C11a N3a H031a . . . 108.6(6) . C12a N3a H031a . . . 108.6(7) . C17a N4a C18a . . . 112.9(7) . C17a N4a H041a . . . 108.6(6) . C18a N4a H041a . . . 108.6(7) . N1a C1a C2a . . . 122.8(9) . C1a C2a C3a . . . 117.0(8) . C1a C2a C11a . . . 119.8(9) . C3a C2a C11a . . . 123.1(9) . C2a C3a C4a . . . 120.4(9) . C3a C4a C5a . . . 119.3(9) . N1a C5a C4a . . . 120.4(7) . N1a C5a C6a . . . 115.9(8) . C4a C5a C6a . . . 123.6(8) . N2a C6a C5a . . . 112.1(8) . N2a C6a C7a . . . 122.6(7) . C5a C6a C7a . . . 125.4(8) . C6a C7a C8a . . . 119.3(9) . C7a C8a C9a . . . 119.0(9) . C8a C9a C10a . . . 119.3(8) . C8a C9a C17a . . . 122.1(8) . C10a C9a C17a . . . 118.5(8) . N2a C10a C9a . . . 122.2(9) . N3a C11a C2a . . . 110.6(8) . N3a C12a C13a . . . 107.7(8) . N3a C12a C14a . . . 108.7(8) . C13a C12a C14a . . . 113.8(7) . O1a C13a O2a . . . 125.3(10) . O1a C13a C12a . . . 122.7(9) . O2a C13a C12a . . . 112.0(9) . C12a C14a C15a . . . 112.3(10) . C12a C14a C16a . . . 112.3(9) . C15a C14a C16a . . . 110.4(8) . N4a C17a C9a . . . 110.5(7) . N4a C18a C19a . . . 107.3(8) . N4a C18a C20a . . . 109.8(8) . C19a C18a C20a . . . 112.1(8) . O3a C19a O4a . . . 124.4(11) . O3a C19a C18a . . . 123.3(10) . O4a C19a C18a . . . 112.2(11) . C18a C20a C21a . . . 114.0(10) . C18a C20a C22a . . . 111.6(10) . C21a C20a C22a . . . 110.5(10) . C8b O2b H02b . . . 110.0(11) . Co N1b C1b . . . 126.2(7) . Co N1b C5b . . . 113.3(7) . C1b N1b C5b . . . 120.3(9) . C6b N2b C7b . . . 112.3(8) . C6b N2b H021b . . . 108.8(7) . C7b N2b H021b . . . 108.8(7) . N1b C1b C2b . . . 120.3(9) . C1b C2b C3b . . . 118.2(10) . C1b C2b C6b . . . 118.6(9) . C3b C2b C6b . . . 123.2(10) . C2b C3b C4b . . . 120.8(10) . C3b C4b C5b . . . 119.2(9) . N1b C5b C4b . . . 121.1(9) . N1b C5b C5b . . 2_655 114.4(8) . C4b C5b C5b . . 2_655 124.5(9) . N2b C6b C2b . . . 110.4(9) . N2b C7b C8b . . . 106.0(8) . N2b C7b C9b . . . 110.4(9) . C8b C7b C9b . . . 113.7(8) . O1b C8b O2b . . . 125.4(12) . O1b C8b C7b . . . 121.1(11) . O2b C8b C7b . . . 113.2(11) . C7b C9b C10b . . . 111.2(10) . C7b C9b C11b . . . 112.1(11) . C10b C9b C11b . . . 111.4(9) . O1c Cl1c O2c . . . 109.7(6) . O1c Cl1c O3c . . . 109.4(6) . O1c Cl1c O4c . . . 109.4(8) . O2c Cl1c O3c . . . 109.5(6) . O2c Cl1c O4c . . . 109.8(6) . O3c Cl1c O4c . . . 108.9(7) . O1d Cl1d O2d . . . 110.7(7) . O1d Cl1d O3d . . . 109.7(6) . O1d Cl1d O4d . . . 108.7(5) . O2d Cl1d O3d . . . 110.1(6) . O2d Cl1d O4d . . . 109.1(5) . O3d Cl1d O4d . . . 108.4(6) . O1e Cl1e O2e . . . 107.2(8) . O1e Cl1e O3e . . . 114.2(9) . O1e Cl1e O4e . . . 106.1(8) . O2e Cl1e O3e . . . 107.1(8) . O2e Cl1e O4e . . . 110.5(7) . O3e Cl1e O4e . . . 111.6(7) . O1f Cl1f O2f . . . 114.5(9) . O1f Cl1f O1f . . 2_655 103.2(9) . O1f Cl1f O2f . . 2_655 105.1(8) . O2f Cl1f O1f . . 2_655 105.1(8) . O2f Cl1f O2f . . 2_655 114.0(10) . O1f Cl1f O2f 2_655 . 2_655 114.5(9) . 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 _geom_torsion_publ_flag N2a Co N1a C1a . . . . 177.0(8) . N2a Co N1a C5a . . . . -1.0(6) . N1b Co N1a C1a . . . . -1.5(8) . N1b Co N1a C5a . . . . -179.5(7) . N1a Co N1a C1a 2_655 . . . -139(7) . N1a Co N1a C5a 2_655 . . . 43(7) . N2a Co N1a C1a 2_655 . . . -95.8(8) . N2a Co N1a C5a 2_655 . . . 86.1(7) . N1b Co N1a C1a 2_655 . . . 82.7(8) . N1b Co N1a C5a 2_655 . . . -95.3(7) . N1a Co N2a C6a . . . . 1.4(7) . N1a Co N2a C10a . . . . 178.8(8) . N1b Co N2a C6a . . . . 48(8) . N1b Co N2a C10a . . . . -135(8) . N1a Co N2a C6a 2_655 . . . -177.3(7) . N1a Co N2a C10a 2_655 . . . .1(8) . N2a Co N2a C6a 2_655 . . . -93.6(7) . N2a Co N2a C10a 2_655 . . . 83.8(8) . N1b Co N2a C6a 2_655 . . . 87.7(7) . N1b Co N2a C10a 2_655 . . . -94.9(8) . N1a Co N1b C1b . . . . -97.6(8) . N1a Co N1b C5b . . . . 87.2(7) . N2a Co N1b C1b . . . . -144(8) . N2a Co N1b C5b . . . . 41(8) . N1a Co N1b C1b 2_655 . . . 81.1(8) . N1a Co N1b C5b 2_655 . . . -94.0(7) . N2a Co N1b C1b 2_655 . . . -2.5(8) . N2a Co N1b C5b 2_655 . . . -177.7(7) . N1b Co N1b C1b 2_655 . . . 176.2(8) . N1b Co N1b C5b 2_655 . . . 1.0(7) . N1a Co N1b C5b . . 2_655 2_655 -94.0(7) . N2a Co N1b C5b . . 2_655 2_655 -177.7(7) . N1b Co N1b C5b . . 2_655 2_655 1.0(7) . N1a Co N1b C5b 2_655 . 2_655 2_655 87.2(7) . N2a Co N1b C5b 2_655 . 2_655 2_655 41(8) . H02a O2a C13a O1a . . . . 6.9(13) . H02a O2a C13a C12a . . . . -174.6(7) . H04a O4a C19a O3a . . . . -11.9(14) . H04a O4a C19a C18a . . . . 165.8(8) . Co N1a C1a C2a . . . . -176.5(7) . C5a N1a C1a C2a . . . . 1.4(13) . Co N1a C5a C4a . . . . 177.1(7) . Co N1a C5a C6a . . . . .4(10) . C1a N1a C5a C4a . . . . -1.1(13) . C1a N1a C5a C6a . . . . -177.7(8) . Co N2a C6a C5a . . . . -1.5(9) . Co N2a C6a C7a . . . . 178.4(7) . C10a N2a C6a C5a . . . . -179.2(7) . C10a N2a C6a C7a . . . . .7(12) . Co N2a C10a C9a . . . . -178.6(6) . C6a N2a C10a C9a . . . . -1.3(12) . C12a N3a C11a C2a . . . . -175.4(8) . H031a N3a C11a C2a . . . . -54.9(10) . C11a N3a C12a C13a . . . . -78.0(9) . C11a N3a C12a C14a . . . . 158.2(8) . H031a N3a C12a C13a . . . . 161.5(7) . H031a N3a C12a C14a . . . . 37.7(9) . C18a N4a C17a C9a . . . . -176.7(8) . H041a N4a C17a C9a . . . . -56.2(10) . C17a N4a C18a C19a . . . . -73.4(10) . C17a N4a C18a C20a . . . . 164.6(9) . H041a N4a C18a C19a . . . . 166.1(7) . H041a N4a C18a C20a . . . . 44.1(10) . N1a C1a C2a C3a . . . . -.6(13) . N1a C1a C2a C11a . . . . 178.9(8) . C1a C2a C3a C4a . . . . -.4(13) . C11a C2a C3a C4a . . . . -179.9(9) . C1a C2a C11a N3a . . . . 83.0(10) . C3a C2a C11a N3a . . . . -97.5(11) . C2a C3a C4a C5a . . . . .6(14) . C3a C4a C5a N1a . . . . .1(13) . C3a C4a C5a C6a . . . . 176.5(9) . N1a C5a C6a N2a . . . . .7(11) . N1a C5a C6a C7a . . . . -179.2(8) . C4a C5a C6a N2a . . . . -175.8(8) . C4a C5a C6a C7a . . . . 4.3(14) . N2a C6a C7a C8a . . . . -.8(13) . C5a C6a C7a C8a . . . . 179.1(9) . C6a C7a C8a C9a . . . . 1.4(14) . C7a C8a C9a C10a . . . . -1.9(13) . C7a C8a C9a C17a . . . . -177.5(8) . C8a C9a C10a N2a . . . . 1.9(13) . C17a C9a C10a N2a . . . . 177.6(8) . C8a C9a C17a N4a . . . . -97.7(10) . C10a C9a C17a N4a . . . . 86.7(10) . N3a C12a C13a O1a . . . . -12.8(12) . N3a C12a C13a O2a . . . . 168.6(7) . C14a C12a C13a O1a . . . . 107.8(10) . C14a C12a C13a O2a . . . . -70.7(10) . N3a C12a C14a C15a . . . . 70.0(10) . N3a C12a C14a C16a . . . . -164.9(8) . C13a C12a C14a C15a . . . . -50.1(11) . C13a C12a C14a C16a . . . . 75.1(11) . N4a C18a C19a O3a . . . . -20.3(13) . N4a C18a C19a O4a . . . . 162.0(8) . C20a C18a C19a O3a . . . . 100.3(11) . C20a C18a C19a O4a . . . . -77.5(12) . N4a C18a C20a C21a . . . . 66.6(12) . N4a C18a C20a C22a . . . . -167.4(10) . C19a C18a C20a C21a . . . . -52.5(13) . C19a C18a C20a C22a . . . . 73.6(13) . H02b O2b C8b O1b . . . . 1.8(16) . H02b O2b C8b C7b . . . . 176.4(8) . Co N1b C1b C2b . . . . -175.3(7) . C5b N1b C1b C2b . . . . -.4(13) . Co N1b C5b C4b . . . . 174.4(7) . Co N1b C5b C5b . . . 2_655 -2.7(10) . C1b N1b C5b C4b . . . . -1.1(13) . C1b N1b C5b C5b . . . 2_655 -178.1(8) . C7b N2b C6b C2b . . . . -178.1(8) . H021b N2b C6b C2b . . . . -57.7(10) . C6b N2b C7b C8b . . . . -80.5(10) . C6b N2b C7b C9b . . . . 155.9(9) . H021b N2b C7b C8b . . . . 159.1(8) . H021b N2b C7b C9b . . . . 35.5(10) . N1b C1b C2b C3b . . . . .4(13) . N1b C1b C2b C6b . . . . 179.9(8) . C1b C2b C3b C4b . . . . 1.0(15) . C6b C2b C3b C4b . . . . -178.5(10) . C1b C2b C6b N2b . . . . 84.2(10) . C3b C2b C6b N2b . . . . -96.3(11) . C2b C3b C4b C5b . . . . -2.4(16) . C3b C4b C5b N1b . . . . 2.5(14) . C3b C4b C5b C5b . . . 2_655 179.3(9) . N1b C5b C5b N1b . . 2_655 2_655 3.5(11) . C4b C5b C5b N1b . . 2_655 2_655 -173.4(9) . N2b C7b C8b O1b . . . . -20.7(13) . N2b C7b C8b O2b . . . . 164.4(9) . C9b C7b C8b O1b . . . . 100.7(12) . C9b C7b C8b O2b . . . . -74.1(13) . N2b C7b C9b C10b . . . . 67.7(12) . N2b C7b C9b C11b . . . . -166.8(9) . C8b C7b C9b C10b . . . . -51.3(13) . C8b C7b C9b C11b . . . . 74.1(13) . Co N1b C5b C5b . 2_655 2_655 . -2.7(10) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N3a H031a Cl1 . . . 1.09 2.17 3.234(9) 166 N4a H041a Cl1 2_655 2_655 1_555 1.09 2.10 3.163(8) 164 N2b H021b Cl1 . . . 1.09 2.12 3.185(9) 163 #=END======================================================================