Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Prof Alan Williams' _publ_contact_author_address ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30 quai Ernest Ansermet Geneva 1211 SWITZERLAND ; _publ_contact_author_email Alan.Williams@chiam.unige.ch _publ_contact_author_phone '41 22 379 64 25' _publ_contact_author_fax '41 22 379 68 30' loop_ _publ_author_name _publ_author_address ' Gilles Stupka' ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; ' Ludovic Gremaud' ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; ' Gerald Bernardinelli' ; Laboratoiry of X-ray Crystallography University de Geneva 24, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; ' Alan F. Williams' ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Redox state switching of transition metals by deprotonation of the tridentate ligand 2,6-bis(imidazo-2-yl)pyridine ; data_UPKA _database_code_depnum_ccdc_archive 'CCDC 222687' #--- [Ru(1)2](PF6)2(CH3CN)2(H2O) ---------------------------------------------- _audit_creation_date 2002-10-31 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 2003-10-10 _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.0.1 #------------------------------------------------------------------------ _chemical_formula_moiety '(C11 H9 N5)2 (P F6)2 (C2 H3 N)2 (H2 O) Ru' _chemical_formula_sum 'C26 H26 F12 N12 O P2 Ru' _chemical_formula_weight 913.7 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 8.0276(4) _cell_length_b 9.0574(5) _cell_length_c 25.5753(14) _cell_angle_alpha 95.093(7) _cell_angle_beta 96.757(6) _cell_angle_gamma 97.794(6) _cell_volume 1819.19(18) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_meas not_measured _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 28.06 _cell_measurement_temperature 200 _exptl_absorpt_coefficient_mu .622 _exptl_crystal_description plate _exptl_crystal_size_max .26 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .05 _exptl_crystal_colour violet _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 .8714 _exptl_absorpt_correction_T_max .9689 _diffrn_reflns_number 19580 _reflns_number_total 8123 _reflns_number_gt 5735 _reflns_threshold_expression 'refl observed if Fo > 3.99 \s(Fo)' _diffrn_reflns_theta_max 28.06 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .034 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .045 _refine_ls_wR_factor_ref .045 _refine_ls_goodness_of_fit_ref 1.57(1) _refine_ls_number_reflns 5855 _refine_ls_number_parameters 553 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.00015(Fo^2^)] _refine_ls_hydrogen_treatment refxyz _refine_ls_shift/su_max .10 _refine_diff_density_max .899 _refine_diff_density_min -.99 _refine_ls_extinction_method none _refine_special_details ; Hydrogen treatment: - refxyz for H bound to the N atoms of the ligand - For the other refined with restraints on bond lengths and bond angles and blocked in the last cylcles. Disorders: One of the PF6 (d) is desordered. Two distinct anions have been refined with a common P atomic site, restraints on bond lengths and bond angles, and population parameters of 0.6 and 0.4 for F atoms labelled d and d' respectively. ; _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_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 F Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .014 .01 P Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .09 .095 Ru Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 -1.42 .836 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 Ru .42730(9) .42192(7) .74220(3) .0285(3) 1.00000 Uani N1a .3561(8) .4360(6) .6650(3) .032(3) 1.00000 Uani N2a .6233(9) .3403(6) .7077(3) .033(3) 1.00000 Uani N3a .7246(11) .2730(8) .6343(3) .044(4) 1.00000 Uani N4a .1999(9) .5051(7) .7444(3) .034(3) 1.00000 Uani N5a -.0121(9) .5917(8) .7014(4) .041(4) 1.00000 Uani C1a .4541(10) .3917(7) .6285(3) .033(4) 1.00000 Uani C2a .4070(13) .3984(9) .5748(4) .045(4) 1.00000 Uani C3a .2556(14) .4507(10) .5596(4) .053(5) 1.00000 Uani C4a .1557(12) .4955(9) .5966(4) .048(4) 1.00000 Uani C5a .2085(10) .4893(8) .6500(3) .036(4) 1.00000 Uani C6a .6024(10) .3377(7) .6550(3) .034(4) 1.00000 Uani C7a .7643(11) .2716(8) .7204(4) .041(4) 1.00000 Uani C8a .8256(12) .2301(9) .6751(4) .046(4) 1.00000 Uani C9a .1296(10) .5282(7) .6960(3) .034(4) 1.00000 Uani C10a .1018(11) .5556(8) .7802(4) .039(4) 1.00000 Uani C11a -.0298(12) .6092(9) .7533(4) .045(5) 1.00000 Uani N1b .4939(9) .4101(7) .8192(3) .035(3) 1.00000 Uani N2b .5530(8) .6376(6) .7671(3) .033(3) 1.00000 Uani N3b .6759(10) .8008(8) .8334(4) .050(4) 1.00000 Uani N4b .3254(9) .2029(7) .7498(3) .038(3) 1.00000 Uani N5b .2869(12) .0244(8) .8014(5) .061(5) 1.00000 Uani C1b .5781(11) .5330(9) .8506(3) .041(4) 1.00000 Uani C2b .6255(14) .5274(11) .9042(4) .057(5) 1.00000 Uani C3b .5834(17) .3928(14) .9253(4) .073(7) 1.00000 Uani C4b .4965(14) .2677(11) .8931(4) .060(6) 1.00000 Uani C5b .4499(12) .2794(9) .8404(4) .042(4) 1.00000 Uani C6b .6040(10) .6573(8) .8194(3) .038(4) 1.00000 Uani C7b .5935(11) .7752(8) .7484(4) .041(4) 1.00000 Uani C8b .6689(12) .8741(9) .7893(5) .053(5) 1.00000 Uani C9b .3564(11) .1676(8) .7994(4) .043(4) 1.00000 Uani C10b .2355(12) .0780(9) .7201(4) .051(5) 1.00000 Uani C11b .2122(15) -.0329(10) .7520(5) .064(6) 1.00000 Uani P1c .7772(5) .8133(3) .59513(11) .0637(14) 1.00000 Uani F1c .9141(14) .8652(8) .6438(4) .140(6) 1.00000 Uani F2c .6338(12) .7570(10) .5472(3) .114(6) 1.00000 Uani F3c .8184(18) .9721(9) .5767(4) .151(8) 1.00000 Uani F4c .7482(11) .6542(8) .6163(4) .123(6) 1.00000 Uani F5c .6470(15) .8797(14) .6266(5) .152(8) 1.00000 Uani F6c .9105(14) .7541(11) .5620(5) .146(8) 1.00000 Uani P1d .2089(4) .8190(3) .93081(9) .0523(12) 1.00000 Uani F1d .3191(18) .8077(18) .8830(5) .085(8) .60000 Uani F2d .105(3) .844(3) .9773(5) .117(10) .60000 Uani F3d .3736(19) .910(3) .9660(8) .160(14) .60000 Uani F4d .0505(19) .7344(19) .8960(7) .117(10) .60000 Uani F5d .262(4) .6756(18) .9480(10) .170(17) .60000 Uani F6d .166(4) .970(2) .9126(11) .19(3) .60000 Uani F1d' .341(4) .930(4) .9140(13) .17(3) .40000 Uani F2d' .067(4) .702(3) .9480(13) .15(3) .40000 Uani F3d' .319(3) .818(3) .9829(7) .111(16) .40000 Uani F4d' .095(3) .820(3) .8768(8) .091(13) .40000 Uani F5d' .289(3) .687(3) .9073(10) .111(15) .40000 Uani F6d' .121(4) .947(3) .9533(10) .111(15) .40000 Uani N1e -.078(3) .2068(15) .8462(6) .135(10) 1.00000 Uani C1e -.0123(18) .2593(13) .8852(6) .076(7) 1.00000 Uani C2e .076(2) .3245(14) .9364(6) .092(8) 1.00000 Uani N1f .2443(15) .7522(11) .4789(4) .080(6) 1.00000 Uani C1f .2598(16) .8423(12) .5132(5) .064(6) 1.00000 Uani C2f .2798(18) .9602(14) .5562(6) .086(8) 1.00000 Uani O1w .7331(12) .8991(12) .9414(4) .109(6) 1.00000 Uani H03a .741(13) .264(10) .608(4) .04000 1.00000 Uiso H05a -.056(12) .613(10) .679(4) .04000 1.00000 Uiso H2a .47685 .36700 .54853 .04000 1.00000 Uiso H3a .22004 .45595 .52217 .04000 1.00000 Uiso H4a .04871 .53132 .58552 .04000 1.00000 Uiso H7a .81242 .25556 .75618 .04000 1.00000 Uiso H8a .92473 .17878 .67217 .04000 1.00000 Uiso H10a .12218 .55341 .81866 .04000 1.00000 Uiso H11a -.12078 .65256 .76907 .04000 1.00000 Uiso H03b .705(12) .823(10) .861(4) .04000 1.00000 Uiso H05b .297(12) -.015(10) .826(4) .04000 1.00000 Uiso H2b .68641 .61574 .92667 .04000 1.00000 Uiso H3b .61542 .38576 .96300 .04000 1.00000 Uiso H4b .47076 .17281 .90790 .04000 1.00000 Uiso H7b .57084 .79604 .71137 .04000 1.00000 Uiso H8b .71181 .98026 .78795 .04000 1.00000 Uiso H10b .19564 .06977 .68218 .04000 1.00000 Uiso H11b .15271 -.13509 .74172 .04000 1.00000 Uiso H21e .12874 .25003 .95394 .05000 1.00000 Uiso H22e .16048 .40586 .93169 .05000 1.00000 Uiso H23e -.00443 .36197 .95751 .05000 1.00000 Uiso H21f .27717 .91581 .58955 .05000 1.00000 Uiso H22f .38602 1.02284 .55717 .05000 1.00000 Uiso H23f .18789 1.01940 .55154 .05000 1.00000 Uiso H1w .84679 .93903 .95211 .04000 1.00000 Uiso H2w .66177 .95810 .95885 .04000 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 Ru .0284(4) .0288(3) .0281(3) .0038(2) .0025(3) .00442(19) N1a .033(4) .027(3) .034(4) .002(3) .001(3) .003(3) N2a .036(4) .027(3) .035(4) .003(3) .002(3) .005(3) N3a .046(5) .044(4) .044(4) .011(3) .014(4) -.002(4) N4a .031(4) .033(3) .038(4) .002(3) .006(3) .004(3) N5a .030(4) .039(4) .055(5) .007(3) -.000(4) .009(3) C1a .040(5) .030(4) .028(4) .003(3) .004(4) .003(3) C2a .060(6) .043(4) .032(4) .007(4) .006(4) .002(4) C3a .072(7) .053(5) .034(5) .012(5) -.006(5) .007(4) C4a .053(6) .047(5) .042(5) .014(4) -.008(5) .006(4) C5a .036(5) .034(4) .036(4) .005(3) -.005(4) .006(3) C6a .035(5) .029(4) .036(4) .004(3) .007(4) -.001(3) C7a .035(5) .033(4) .052(5) .008(4) -.004(4) .004(4) C8a .042(6) .039(4) .059(6) .014(4) .005(5) -.001(4) C9a .028(5) .030(4) .043(5) .005(3) -.001(4) .005(3) C10a .033(5) .037(4) .048(5) .002(4) .013(4) .002(4) C11a .038(6) .039(4) .062(6) .007(4) .018(5) .003(4) N1b .030(4) .042(4) .035(4) .008(3) .005(3) .007(3) N2b .033(4) .032(3) .036(4) .006(3) .008(3) .004(3) N3b .050(5) .043(4) .049(5) .002(4) -.000(4) -.016(4) N4b .033(4) .035(3) .047(4) .004(3) .007(4) .009(3) N5b .065(6) .042(4) .083(7) .005(4) .022(6) .031(4) C1b .037(5) .054(5) .031(4) .009(4) .001(4) -.002(4) C2b .063(7) .068(6) .037(5) .015(5) -.003(5) .002(4) C3b .086(9) .101(8) .036(5) .029(7) .002(6) .020(6) C4b .070(8) .066(6) .048(6) .014(5) .010(6) .025(5) C5b .045(6) .048(5) .039(5) .011(4) .009(4) .019(4) C6b .032(5) .041(4) .036(4) .004(3) -.000(4) -.005(3) C7b .039(5) .033(4) .054(5) .006(4) .010(4) .009(4) C8b .049(6) .032(4) .075(7) .003(4) .009(5) -.001(4) C9b .043(6) .036(4) .054(5) .007(4) .013(5) .018(4) C10b .045(6) .037(4) .065(6) -.002(4) .003(5) .001(4) C11b .066(7) .034(5) .090(8) -.003(4) .012(6) .007(5) P1c .095(3) .0535(13) .0485(14) .0314(14) .0062(14) .0132(11) F1c .188(10) .071(5) .126(7) -.028(5) -.076(7) .026(5) F2c .132(8) .149(7) .064(5) .059(6) -.021(5) .008(5) F3c .291(15) .081(5) .109(7) .077(7) .055(8) .046(5) F4c .114(7) .074(4) .156(8) -.031(4) -.065(6) .050(5) F5c .142(10) .212(11) .116(8) .069(8) .047(7) -.006(8) F6c .122(8) .133(7) .190(11) .040(6) .055(8) -.023(7) P1d .0691(19) .0468(12) .0402(12) .0031(11) .0109(12) .0043(10) F1d .087(10) .117(10) .066(7) .030(8) .038(7) .020(7) F2d .109(13) .169(16) .056(8) -.040(12) .042(8) -.023(9) F3d .080(11) .203(17) .16(2) -.032(11) .024(11) -.118(17) F4d .070(9) .165(15) .092(13) -.013(10) .009(9) -.062(11) F5d .25(3) .087(10) .18(3) .043(13) .00(3) .079(13) F6d .27(4) .115(13) .27(3) .119(17) .18(3) .104(17) F1d' .14(3) .15(3) .18(3) -.09(3) -.05(3) .11(3) F2d' .14(3) .105(16) .21(4) -.016(16) .10(3) .04(2) F3d' .17(3) .098(16) .062(11) .045(16) -.042(15) .022(11) F4d' .095(18) .094(14) .073(13) .010(11) -.022(12) .008(11) F5d' .13(2) .112(17) .093(16) .062(16) .010(16) -.020(14) F6d' .13(3) .098(16) .093(17) .064(16) -.030(16) -.050(14) N1e .185(16) .110(10) .095(10) .013(10) -.032(11) .011(8) C1e .091(10) .065(7) .071(8) .008(6) .003(7) .014(6) C2e .115(12) .079(8) .079(9) .008(8) .016(8) .007(7) N1f .115(9) .081(6) .056(6) .043(6) .025(6) .011(5) C1f .080(9) .068(6) .053(6) .028(6) .020(6) .013(5) C2f .093(11) .085(8) .081(9) .010(7) .023(8) -.006(7) O1w .089(7) .138(8) .082(6) .017(6) -.014(6) -.060(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 Ru N1a . . 2.010(6) Ru N2a . . 2.081(7) Ru N4a . . 2.072(7) Ru N1b . . 1.994(7) Ru N2b . . 2.081(6) Ru N4b . . 2.075(6) N1a C1a . . 1.357(11) N1a C5a . . 1.366(11) N2a C6a . . 1.335(10) N2a C7a . . 1.384(11) N3a C6a . . 1.345(12) N3a C8a . . 1.364(12) N3a H03a . . .70(10) N4a C9a . . 1.345(10) N4a C10a . . 1.362(11) N5a C9a . . 1.359(11) N5a C11a . . 1.348(13) N5a H05a . . .69(10) C1a C2a . . 1.390(11) C1a C6a . . 1.463(11) C2a C3a . . 1.389(15) C3a C4a . . 1.380(14) C4a C5a . . 1.389(12) C5a C9a . . 1.440(12) C7a C8a . . 1.352(13) C10a C11a . . 1.361(12) N1b C1b . . 1.361(9) N1b C5b . . 1.366(10) N2b C6b . . 1.341(10) N2b C7b . . 1.385(10) N3b C6b . . 1.347(10) N3b C8b . . 1.357(14) N3b H03b . . .73(9) N4b C9b . . 1.338(12) N4b C10b . . 1.369(10) N5b C9b . . 1.348(11) N5b C11b . . 1.358(15) N5b H05b . . .76(10) C1b C2b . . 1.387(12) C1b C6b . . 1.444(12) C2b C3b . . 1.392(16) C3b C4b . . 1.389(14) C4b C5b . . 1.374(13) C5b C9b . . 1.453(11) C7b C8b . . 1.342(12) C10b C11b . . 1.356(14) P1c F1c . . 1.553(10) P1c F2c . . 1.577(8) P1c F3c . . 1.558(9) P1c F4c . . 1.581(8) P1c F5c . . 1.544(13) P1c F6c . . 1.561(13) P1d F1d . . 1.596(14) P1d F2d . . 1.548(16) P1d F3d . . 1.591(15) P1d F4d . . 1.531(14) P1d F5d . . 1.506(19) P1d F6d . . 1.55(3) P1d F1d' . . 1.49(3) P1d F2d' . . 1.58(3) P1d F3d' . . 1.512(19) P1d F4d' . . 1.57(2) P1d F5d' . . 1.54(3) P1d F6d' . . 1.54(3) N1e C1e . . 1.108(19) C1e C2e . . 1.447(18) N1f C1f . . 1.128(14) C1f C2f . . 1.441(16) 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 N1a Ru N2a . . . 78.2(3) N1a Ru N4a . . . 78.6(3) N1a Ru N1b . . . 178.8(3) N1a Ru N2b . . . 101.5(3) N1a Ru N4b . . . 101.6(3) N2a Ru N4a . . . 156.8(3) N2a Ru N1b . . . 103.0(3) N2a Ru N2b . . . 97.3(3) N2a Ru N4b . . . 88.9(3) N4a Ru N1b . . . 100.3(3) N4a Ru N2b . . . 88.4(3) N4a Ru N4b . . . 94.7(3) N1b Ru N2b . . . 78.2(3) N1b Ru N4b . . . 78.6(3) N2b Ru N4b . . . 156.8(3) Ru N1a C1a . . . 119.8(5) Ru N1a C5a . . . 119.3(6) C1a N1a C5a . . . 120.9(7) Ru N2a C6a . . . 112.7(6) Ru N2a C7a . . . 140.8(6) C6a N2a C7a . . . 106.1(7) C6a N3a C8a . . . 107.5(8) C6a N3a H03a . . . 130(9) C8a N3a H03a . . . 123(9) Ru N4a C9a . . . 112.0(6) Ru N4a C10a . . . 140.1(6) C9a N4a C10a . . . 107.6(7) C9a N5a C11a . . . 108.5(8) C9a N5a H05a . . . 118(9) C11a N5a H05a . . . 133(9) N1a C1a C2a . . . 121.1(8) N1a C1a C6a . . . 109.7(7) C2a C1a C6a . . . 129.2(8) C1a C2a C3a . . . 117.9(9) C2a C3a C4a . . . 121.1(8) C3a C4a C5a . . . 119.3(9) N1a C5a C4a . . . 119.7(8) N1a C5a C9a . . . 109.7(7) C4a C5a C9a . . . 130.6(8) N2a C6a N3a . . . 110.4(7) N2a C6a C1a . . . 119.5(7) N3a C6a C1a . . . 129.9(7) N2a C7a C8a . . . 108.6(8) N3a C8a C7a . . . 107.4(8) N4a C9a N5a . . . 108.2(7) N4a C9a C5a . . . 120.4(7) N5a C9a C5a . . . 131.4(8) N4a C10a C11a . . . 108.3(8) N5a C11a C10a . . . 107.4(8) Ru N1b C1b . . . 120.1(6) Ru N1b C5b . . . 119.7(5) C1b N1b C5b . . . 120.2(7) Ru N2b C6b . . . 112.1(5) Ru N2b C7b . . . 141.2(6) C6b N2b C7b . . . 106.5(6) C6b N3b C8b . . . 108.2(7) C6b N3b H03b . . . 117(7) C8b N3b H03b . . . 134(7) Ru N4b C9b . . . 112.3(5) Ru N4b C10b . . . 140.6(7) C9b N4b C10b . . . 107.1(7) C9b N5b C11b . . . 108.4(9) C9b N5b H05b . . . 123(6) C11b N5b H05b . . . 129(6) N1b C1b C2b . . . 121.1(8) N1b C1b C6b . . . 109.6(7) C2b C1b C6b . . . 129.3(7) C1b C2b C3b . . . 118.2(8) C2b C3b C4b . . . 120.6(9) C3b C4b C5b . . . 119.0(9) N1b C5b C4b . . . 120.8(7) N1b C5b C9b . . . 109.6(7) C4b C5b C9b . . . 129.6(8) N2b C6b N3b . . . 109.2(7) N2b C6b C1b . . . 119.9(6) N3b C6b C1b . . . 130.9(8) N2b C7b C8b . . . 108.4(8) N3b C8b C7b . . . 107.6(7) N4b C9b N5b . . . 109.0(8) N4b C9b C5b . . . 119.7(7) N5b C9b C5b . . . 131.2(9) N4b C10b C11b . . . 108.6(9) N5b C11b C10b . . . 106.9(8) F1c P1c F2c . . . 177.7(6) F1c P1c F3c . . . 87.8(5) F1c P1c F4c . . . 88.4(5) F1c P1c F5c . . . 88.5(6) F1c P1c F6c . . . 91.7(6) F2c P1c F3c . . . 94.0(6) F2c P1c F4c . . . 89.9(5) F2c P1c F5c . . . 90.2(6) F2c P1c F6c . . . 89.7(6) F3c P1c F4c . . . 175.9(6) F3c P1c F5c . . . 86.4(7) F3c P1c F6c . . . 90.6(7) F4c P1c F5c . . . 95.0(6) F4c P1c F6c . . . 88.0(6) F5c P1c F6c . . . 177.0(7) F1d P1d F2d . . . 175.2(10) F1d P1d F3d . . . 87.8(9) F1d P1d F4d . . . 91.5(8) F1d P1d F5d . . . 89.7(12) F1d P1d F6d . . . 87.7(13) F2d P1d F3d . . . 89.8(9) F2d P1d F4d . . . 90.8(9) F2d P1d F5d . . . 94.4(13) F2d P1d F6d . . . 88.1(13) F3d P1d F4d . . . 178.5(10) F3d P1d F5d . . . 89.3(11) F3d P1d F6d . . . 88.2(12) F4d P1d F5d . . . 92.0(11) F4d P1d F6d . . . 90.5(11) F5d P1d F6d . . . 176.5(14) F1d' P1d F2d' . . . 179.3(16) F1d' P1d F3d' . . . 90.1(14) F1d' P1d F4d' . . . 89.8(14) F1d' P1d F5d' . . . 91.7(15) F1d' P1d F6d' . . . 90.5(15) F2d' P1d F3d' . . . 90.6(14) F2d' P1d F4d' . . . 89.5(13) F2d' P1d F5d' . . . 88.5(14) F2d' P1d F6d' . . . 89.3(14) F3d' P1d F4d' . . . 180.0(12) F3d' P1d F5d' . . . 89.4(12) F3d' P1d F6d' . . . 92.3(13) F4d' P1d F5d' . . . 90.6(12) F4d' P1d F6d' . . . 87.7(13) F5d' P1d F6d' . . . 177.2(12) N1e C1e C2e . . . 178.5(16) N1f C1f C2f . . . 178.6(13) 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 C5a N1a C1a C2a . . . . -.4(10) C5a N1a C1a C6a . . . . -179.2(6) C1a N1a C5a C4a . . . . 1.4(10) C1a N1a C5a C9a . . . . -180.0(6) C7a N2a C6a N3a . . . . -.9(8) C7a N2a C6a C1a . . . . 175.0(6) C6a N2a C7a C8a . . . . .3(8) C8a N3a C6a N2a . . . . 1.1(8) C8a N3a C6a C1a . . . . -174.3(7) C6a N3a C8a C7a . . . . -.9(9) C10a N4a C9a N5a . . . . -.4(8) C10a N4a C9a C5a . . . . 178.3(6) C9a N4a C10a C11a . . . . .3(8) C11a N5a C9a N4a . . . . .4(8) C11a N5a C9a C5a . . . . -178.2(7) C9a N5a C11a C10a . . . . -.2(8) N1a C1a C2a C3a . . . . -.5(11) C6a C1a C2a C3a . . . . 178.0(7) N1a C1a C6a N2a . . . . -.9(9) N1a C1a C6a N3a . . . . 174.2(7) C2a C1a C6a N2a . . . . -179.6(7) C2a C1a C6a N3a . . . . -4.5(12) C1a C2a C3a C4a . . . . .4(12) C2a C3a C4a C5a . . . . .6(12) C3a C4a C5a N1a . . . . -1.5(11) C3a C4a C5a C9a . . . . -179.7(8) N1a C5a C9a N4a . . . . -2.1(9) N1a C5a C9a N5a . . . . 176.2(7) C4a C5a C9a N4a . . . . 176.3(7) C4a C5a C9a N5a . . . . -5.4(13) N2a C7a C8a N3a . . . . .4(9) N4a C10a C11a N5a . . . . -.1(9) C5b N1b C1b C2b . . . . 1.9(13) C5b N1b C1b C6b . . . . -177.8(8) C1b N1b C5b C4b . . . . -3.0(14) C1b N1b C5b C9b . . . . 178.0(8) C7b N2b C6b N3b . . . . -.7(10) C7b N2b C6b C1b . . . . 179.6(8) C6b N2b C7b C8b . . . . .5(10) C8b N3b C6b N2b . . . . .6(11) C8b N3b C6b C1b . . . . -179.7(10) C6b N3b C8b C7b . . . . -.3(11) C10b N4b C9b N5b . . . . -.5(11) C10b N4b C9b C5b . . . . -179.6(9) C9b N4b C10b C11b . . . . .1(11) C11b N5b C9b N4b . . . . .8(12) C11b N5b C9b C5b . . . . 179.7(11) C9b N5b C11b C10b . . . . -.7(13) N1b C1b C2b C3b . . . . -.5(15) C6b C1b C2b C3b . . . . 179.2(11) N1b C1b C6b N2b . . . . -2.6(12) N1b C1b C6b N3b . . . . 177.8(9) C2b C1b C6b N2b . . . . 177.6(10) C2b C1b C6b N3b . . . . -2.0(17) C1b C2b C3b C4b . . . . .2(18) C2b C3b C4b C5b . . . . -1.2(19) C3b C4b C5b N1b . . . . 2.6(16) C3b C4b C5b C9b . . . . -178.6(11) N1b C5b C9b N4b . . . . -.6(12) N1b C5b C9b N5b . . . . -179.5(10) C4b C5b C9b N4b . . . . -179.5(10) C4b C5b C9b N5b . . . . 1.6(18) N2b C7b C8b N3b . . . . -.2(11) N4b C10b C11b N5b . . . . .4(13) 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 H03a N1f . . 2_666 0.70(10) 2.23(9) 2.925(12) 171(11) N5a H05a F4c . . 1_455 0.69(9) 2.21(9) 2.880(11) 165(10) N3b H03b O1w . . . 0.73(9) 2.07(9) 2.790(12) 167(10) N5b H05b F1d . . 1_545 0.76(9) 2.27(9) 3.002(17) 163(9) #==END==================================================================== data_STUP _database_code_depnum_ccdc_archive 'CCDC 222688' #--- [Mn(1)2](CF3SO3)2.Et2O ----------------------------------------------- _audit_creation_date 2000-01-13 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 2003-10-10 _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.0.1 _chemical_formula_moiety '(C11 H9 N5)2 Mn (C F3 S O3)2 (C4 H10 O)' _chemical_formula_sum 'C28 H28 F6 Mn N10 O7 S2' _chemical_formula_weight 849.72 _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 13.090(2) _cell_length_b 14.3260(10) _cell_length_c 19.8080(10) _cell_angle_alpha 90.00000 _cell_angle_beta 105.468(5) _cell_angle_gamma 90.00000 _cell_volume 3580.0(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_meas not_measured _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54186 _cell_measurement_reflns_used 36 _cell_measurement_theta_min 21.6 _cell_measurement_theta_max 26.4 _cell_measurement_temperature 200 _exptl_absorpt_coefficient_mu 4.907 _exptl_crystal_description prism _exptl_crystal_size_max .40 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .24 _exptl_crystal_colour colourless _diffrn_measurement_device_type Stoe_Stadi-4_4-circle_diffractometer _diffrn_measurement_method \w-2\q_scans _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'xtal_lsabs (Flack & al. 1992)' _exptl_absorpt_correction_T_min .2951 _exptl_absorpt_correction_T_max .4020 _diffrn_reflns_number 4749 _reflns_number_total 4359 _reflns_number_gt 3281 _reflns_threshold_expression 'refl observed if Fo > 3.99 \s(Fo)' _diffrn_reflns_theta_max 54.15 _diffrn_reflns_theta_full 54.15 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .092 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0. _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .059 _refine_ls_wR_factor_ref .058 _refine_ls_goodness_of_fit_ref 1.81(2) _refine_ls_number_reflns 3281 _refine_ls_number_parameters 488 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.0002(Fo^2^)] _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .0004 _refine_diff_density_max .544 _refine_diff_density_min -.66 _refine_ls_extinction_method none _computing_data_collection Stoe_Stadi-4 _computing_cell_refinement xtal_latcon _computing_data_reduction xtal_REFCAL_LSABS__SORTRF _computing_structure_solution SIR-97 _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal_ORTEP _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 .017 .009 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 .029 .018 O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .047 .032 S Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .319 .557 F Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .069 .053 Mn Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 -.568 2.808 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 Mn .24419(8) .65620(7) .51374(6) .0233(6) 1.00000 Uani N1a .1445(4) .5643(4) .5622(3) .022(3) 1.00000 Uani N2a .0728(4) .7137(4) .4839(3) .028(3) 1.00000 Uani N3a -.0830(4) .7184(4) .5089(3) .029(3) 1.00000 Uani N4a .3460(4) .5353(4) .5649(3) .025(3) 1.00000 Uani N5a .3576(4) .3968(4) .6178(3) .028(3) 1.00000 Uani C1a .0451(5) .5882(5) .5610(3) .022(4) 1.00000 Uani C2a -.0182(5) .5362(5) .5937(4) .028(4) 1.00000 Uani C3a .0265(6) .4555(5) .6284(4) .034(4) 1.00000 Uani C4a .1287(5) .4266(5) .6296(3) .025(4) 1.00000 Uani C5a .1850(5) .4859(5) .5961(4) .024(4) 1.00000 Uani C6a .0120(5) .6721(5) .5199(4) .027(4) 1.00000 Uani C7a .0150(6) .7880(5) .4493(4) .033(4) 1.00000 Uani C8a -.0803(6) .7919(5) .4645(4) .037(5) 1.00000 Uani C9a .2954(5) .4713(5) .5932(4) .024(4) 1.00000 Uani C10a .4462(6) .4988(5) .5727(4) .034(4) 1.00000 Uani C11a .4534(6) .4143(5) .6047(4) .037(5) 1.00000 Uani N1b .2866(4) .7887(4) .4657(3) .024(3) 1.00000 Uani N2b .2766(4) .7659(4) .5967(3) .028(3) 1.00000 Uani N3b .2947(5) .9154(4) .6242(3) .035(4) 1.00000 Uani N4b .2638(4) .6214(4) .4059(3) .025(3) 1.00000 Uani N5b .2699(5) .6733(4) .3008(3) .032(4) 1.00000 Uani C1b .2963(5) .8686(5) .5028(4) .026(4) 1.00000 Uani C2b .3047(6) .9538(5) .4724(4) .036(5) 1.00000 Uani C3b .3009(6) .9553(5) .4029(5) .044(5) 1.00000 Uani C4b .2900(6) .8732(5) .3629(4) .036(5) 1.00000 Uani C5b .2827(5) .7915(5) .3977(4) .023(4) 1.00000 Uani C6b .2919(5) .8522(5) .5742(4) .026(4) 1.00000 Uani C7b .2689(6) .7777(6) .6642(4) .036(5) 1.00000 Uani C8b .2791(6) .8695(6) .6817(4) .040(5) 1.00000 Uani C9b .2718(5) .6967(5) .3675(4) .025(4) 1.00000 Uani C10b .2576(5) .5469(5) .3604(4) .028(4) 1.00000 Uani C11b .2610(6) .5775(5) .2964(4) .037(5) 1.00000 Uani S1c .27305(14) .26102(13) .38038(10) .0354(11) 1.00000 Uani C1c .4093(6) .2266(6) .4257(5) .044(5) 1.00000 Uani O1c .2466(4) .3261(4) .4285(3) .039(3) 1.00000 Uani O2c .2805(4) .3018(4) .3161(3) .053(4) 1.00000 Uani O3c .2168(4) .1734(4) .3728(4) .070(4) 1.00000 Uani F1c .4739(4) .2984(4) .4339(3) .077(4) 1.00000 Uani F2c .4441(4) .1628(4) .3877(3) .072(3) 1.00000 Uani F3c .4134(4) .1900(4) .4864(3) .082(4) 1.00000 Uani S1d -.16790(14) .34906(12) .19153(9) .0311(10) 1.00000 Uani C1d -.0242(6) .3370(6) .2299(5) .048(5) 1.00000 Uani O1d -.2016(4) .4075(3) .2404(3) .038(3) 1.00000 Uani O2d -.1762(4) .3891(4) .1238(3) .048(3) 1.00000 Uani O3d -.2036(4) .2531(3) .1885(3) .035(3) 1.00000 Uani F1d .0230(4) .4192(4) .2346(3) .082(4) 1.00000 Uani F2d .0163(4) .2813(4) .1901(3) .080(4) 1.00000 Uani F3d -.0053(4) .3013(4) .2937(3) .080(4) 1.00000 Uani O1e .5078(5) .5675(4) .8207(3) .058(4) 1.00000 Uani C1e .4926(7) .6092(8) .7542(5) .064(6) 1.00000 Uani C2e .5074(7) .7123(8) .7633(5) .069(6) 1.00000 Uani C3e .4852(7) .4706(7) .8174(5) .070(7) 1.00000 Uani C4e .4932(7) .4366(7) .8893(5) .074(7) 1.00000 Uani H03a -.14777 .70015 .53071 .05000 1.00000 Uiso H05a .33617 .33507 .64275 .05000 1.00000 Uiso H2a -.09804 .55729 .59220 .05000 1.00000 Uiso H3a -.01930 .41372 .65534 .05000 1.00000 Uiso H4a .16300 .36202 .65491 .05000 1.00000 Uiso H7a .04164 .83647 .41528 .05000 1.00000 Uiso H8a -.14265 .84338 .44515 .05000 1.00000 Uiso H10a .48638 .55038 .54918 .05000 1.00000 Uiso H11a .52207 .36917 .61748 .05000 1.00000 Uiso H03b .30635 .98976 .62030 .05000 1.00000 Uiso H05b .27469 .72076 .25920 .05000 1.00000 Uiso H2b .31413 1.01795 .50248 .05000 1.00000 Uiso H3b .30657 1.02157 .37752 .05000 1.00000 Uiso H4b .28621 .87482 .30760 .05000 1.00000 Uiso H7b .25639 .72248 .69815 .05000 1.00000 Uiso H8b .27550 .90060 .73125 .05000 1.00000 Uiso H10b .25179 .48638 .39171 .05000 1.00000 Uiso H11b .25661 .53452 .25081 .05000 1.00000 Uiso H11e .54944 .58119 .72822 .05000 1.00000 Uiso H12e .41211 .59456 .72222 .05000 1.00000 Uiso H21e .45007 .74038 .78907 .05000 1.00000 Uiso H22e .58740 .72701 .79507 .05000 1.00000 Uiso H23e .49526 .74467 .71188 .05000 1.00000 Uiso H31e .40569 .45841 .78421 .05000 1.00000 Uiso H32e .54260 .43374 .79597 .05000 1.00000 Uiso H41e .57311 .44903 .92243 .05000 1.00000 Uiso H42e .43620 .47370 .91067 .05000 1.00000 Uiso H43e .47612 .36226 .88678 .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 Mn .0260(6) .0201(6) .0261(6) -.0010(6) .0106(5) .0038(6) N1a .023(4) .022(4) .020(3) .002(3) .005(3) .000(3) N2a .027(4) .032(4) .027(4) .001(3) .009(3) .011(3) N3a .021(4) .037(4) .030(4) .009(3) .007(3) -.000(3) N4a .024(4) .025(4) .027(4) .005(3) .009(3) .006(3) N5a .025(4) .025(4) .035(4) .001(3) .010(3) .004(3) C1a .028(5) .021(4) .018(4) .001(4) .005(4) -.001(3) C2a .028(4) .030(5) .029(4) -.002(4) .014(4) -.001(4) C3a .038(5) .037(5) .030(5) -.013(4) .013(4) -.003(4) C4a .034(5) .024(4) .019(4) -.002(4) .009(4) .003(3) C5a .023(4) .027(4) .021(4) -.002(4) .006(4) -.005(4) C6a .029(4) .029(5) .023(4) -.002(4) .007(4) -.009(4) C7a .037(5) .030(5) .029(5) .004(4) .006(4) .005(4) C8a .044(5) .035(5) .032(5) .011(4) .010(4) .004(4) C9a .033(5) .020(4) .018(4) .002(4) .008(4) -.000(4) C10a .036(5) .026(5) .043(5) .001(4) .016(4) .010(4) C11a .028(5) .039(5) .048(5) .007(4) .015(4) .005(4) N1b .019(4) .025(4) .027(4) .002(3) .007(3) .003(3) N2b .026(4) .033(4) .024(4) -.003(3) .006(3) .004(3) N3b .043(4) .027(4) .033(4) .003(3) .007(3) -.007(3) N4b .028(4) .020(4) .029(4) -.001(3) .013(3) .004(3) N5b .033(4) .037(4) .028(4) -.002(3) .011(3) .002(3) C1b .023(4) .028(5) .027(4) -.001(4) .006(4) -.003(4) C2b .053(5) .024(5) .036(5) -.004(4) .020(4) .002(4) C3b .062(6) .022(5) .053(6) .001(4) .021(5) .011(4) C4b .051(5) .031(5) .031(5) -.001(4) .016(4) .007(4) C5b .023(4) .023(5) .025(5) .003(4) .011(4) .004(4) C6b .024(4) .030(5) .023(4) .003(4) .005(4) -.003(4) C7b .039(5) .044(6) .027(5) .002(4) .012(4) .002(4) C8b .052(6) .051(6) .020(5) .010(4) .013(4) .002(4) C9b .022(4) .032(5) .023(4) .001(4) .009(4) .001(4) C10b .025(4) .028(5) .035(5) -.005(4) .015(4) -.003(4) C11b .041(5) .026(5) .043(5) -.006(4) .011(4) -.011(4) S1c .0310(11) .0314(12) .0441(12) .0031(9) .0107(9) -.0035(10) C1c .031(5) .046(6) .055(6) -.002(5) .009(5) .001(5) O1c .043(3) .041(4) .039(3) .001(3) .023(3) -.007(3) O2c .067(4) .065(4) .029(3) .021(3) .016(3) -.002(3) O3c .040(4) .031(4) .136(6) -.010(3) .015(4) -.016(4) F1c .034(3) .050(4) .138(5) -.013(3) .007(3) -.011(4) F2c .052(3) .052(3) .120(5) .017(3) .035(3) -.008(4) F3c .072(4) .099(5) .071(4) .019(4) .010(3) .040(4) S1d .0344(11) .0277(11) .0327(11) -.0030(9) .0115(9) -.0045(9) C1d .037(5) .040(6) .069(7) -.005(5) .016(5) -.023(5) O1d .046(3) .028(3) .045(3) -.000(3) .019(3) -.011(3) O2d .076(4) .036(3) .035(3) -.004(3) .021(3) .001(3) O3d .042(3) .024(3) .044(3) -.009(3) .017(3) -.007(3) F1d .048(3) .074(4) .129(5) -.030(3) .029(4) -.044(4) F2d .043(3) .082(4) .119(5) -.002(3) .031(3) -.056(4) F3d .076(4) .079(4) .067(4) .017(3) -.014(3) -.008(3) O1e .058(4) .057(4) .053(4) -.003(3) .006(3) -.003(4) C1e .062(7) .092(8) .036(6) .009(6) .011(5) -.003(6) C2e .041(6) .096(8) .065(7) -.011(6) .008(5) .014(6) C3e .065(7) .058(7) .082(8) .004(6) .010(6) -.014(6) C4e .062(7) .073(7) .081(8) -.005(6) .007(6) .014(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 Mn N1a . . 2.242(6) Mn N2a . . 2.313(6) Mn N4a . . 2.255(5) Mn N1b . . 2.258(6) Mn N2b . . 2.231(6) Mn N4b . . 2.274(6) N1a C1a . . 1.340(9) N1a C5a . . 1.343(8) N2a C6a . . 1.342(10) N2a C7a . . 1.378(8) N3a C6a . . 1.375(9) N3a C8a . . 1.379(9) N4a C9a . . 1.338(9) N4a C10a . . 1.382(9) N5a C9a . . 1.352(8) N5a C11a . . 1.371(10) C1a C2a . . 1.395(10) C1a C6a . . 1.452(9) C2a C3a . . 1.390(9) C3a C4a . . 1.395(10) C4a C5a . . 1.401(10) C5a C9a . . 1.477(10) C7a C8a . . 1.359(11) C10a C11a . . 1.358(10) N1b C1b . . 1.348(8) N1b C5b . . 1.336(9) N2b C6b . . 1.347(9) N2b C7b . . 1.377(9) N3b C6b . . 1.335(9) N3b C8b . . 1.376(10) N4b C9b . . 1.341(9) N4b C10b . . 1.385(9) N5b C9b . . 1.357(9) N5b C11b . . 1.379(9) C1b C2b . . 1.379(10) C1b C6b . . 1.449(10) C2b C3b . . 1.366(11) C3b C4b . . 1.403(10) C4b C5b . . 1.375(10) C5b C9b . . 1.475(9) C7b C8b . . 1.359(11) C10b C11b . . 1.354(11) S1c C1c . . 1.838(8) S1c O1c . . 1.440(6) S1c O2c . . 1.427(6) S1c O3c . . 1.442(6) C1c F1c . . 1.314(9) C1c F2c . . 1.339(10) C1c F3c . . 1.300(10) S1d C1d . . 1.839(8) S1d O1d . . 1.436(6) S1d O2d . . 1.437(5) S1d O3d . . 1.449(5) C1d F1d . . 1.322(10) C1d F2d . . 1.328(11) C1d F3d . . 1.324(11) O1e C1e . . 1.411(11) O1e C3e . . 1.418(11) C1e C2e . . 1.495(15) C3e C4e . . 1.482(14) 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 N1a Mn N2a . . . 71.54(19) N1a Mn N4a . . . 72.43(19) N1a Mn N1b . . . 155.61(19) N1a Mn N2b . . . 96.7(2) N1a Mn N4b . . . 119.86(18) N2a Mn N4a . . . 143.6(2) N2a Mn N1b . . . 85.61(19) N2a Mn N2b . . . 85.32(19) N2a Mn N4b . . . 100.53(18) N4a Mn N1b . . . 130.76(19) N4a Mn N2b . . . 103.68(18) N4a Mn N4b . . . 93.00(19) N1b Mn N2b . . . 72.4(2) N1b Mn N4b . . . 71.73(19) N2b Mn N4b . . . 143.1(2) Mn N1a C1a . . . 121.1(4) Mn N1a C5a . . . 120.6(5) C1a N1a C5a . . . 118.3(6) Mn N2a C6a . . . 112.2(4) Mn N2a C7a . . . 140.2(5) C6a N2a C7a . . . 106.4(6) C6a N3a C8a . . . 107.1(6) Mn N4a C9a . . . 114.5(4) Mn N4a C10a . . . 140.4(5) C9a N4a C10a . . . 104.8(6) C9a N5a C11a . . . 106.3(6) N1a C1a C2a . . . 123.3(6) N1a C1a C6a . . . 111.4(6) C2a C1a C6a . . . 125.3(6) C1a C2a C3a . . . 116.7(7) C2a C3a C4a . . . 122.0(7) C3a C4a C5a . . . 115.8(6) N1a C5a C4a . . . 123.8(6) N1a C5a C9a . . . 111.0(6) C4a C5a C9a . . . 125.2(6) N2a C6a N3a . . . 110.0(6) N2a C6a C1a . . . 122.4(6) N3a C6a C1a . . . 127.6(7) N2a C7a C8a . . . 109.7(7) N3a C8a C7a . . . 106.9(6) N4a C9a N5a . . . 112.0(6) N4a C9a C5a . . . 121.2(6) N5a C9a C5a . . . 126.8(6) N4a C10a C11a . . . 109.6(7) N5a C11a C10a . . . 107.4(6) Mn N1b C1b . . . 118.8(5) Mn N1b C5b . . . 120.2(4) C1b N1b C5b . . . 119.9(6) Mn N2b C6b . . . 114.8(4) Mn N2b C7b . . . 138.8(5) C6b N2b C7b . . . 105.3(6) C6b N3b C8b . . . 108.0(6) Mn N4b C9b . . . 113.7(5) Mn N4b C10b . . . 141.1(5) C9b N4b C10b . . . 104.6(6) C9b N5b C11b . . . 106.6(6) N1b C1b C2b . . . 121.4(7) N1b C1b C6b . . . 111.8(6) C2b C1b C6b . . . 126.7(7) C1b C2b C3b . . . 117.9(7) C2b C3b C4b . . . 121.8(7) C3b C4b C5b . . . 116.2(7) N1b C5b C4b . . . 122.8(6) N1b C5b C9b . . . 110.8(6) C4b C5b C9b . . . 126.4(6) N2b C6b N3b . . . 110.7(6) N2b C6b C1b . . . 121.3(6) N3b C6b C1b . . . 127.8(6) N2b C7b C8b . . . 109.8(7) N3b C8b C7b . . . 106.1(7) N4b C9b N5b . . . 111.7(6) N4b C9b C5b . . . 121.7(6) N5b C9b C5b . . . 126.6(6) N4b C10b C11b . . . 110.4(6) N5b C11b C10b . . . 106.7(7) C1c S1c O1c . . . 102.9(4) C1c S1c O2c . . . 104.9(4) C1c S1c O3c . . . 102.7(4) O1c S1c O2c . . . 114.2(3) O1c S1c O3c . . . 115.2(4) O2c S1c O3c . . . 114.7(4) S1c C1c F1c . . . 111.0(6) S1c C1c F2c . . . 109.9(5) S1c C1c F3c . . . 110.8(6) F1c C1c F2c . . . 107.4(7) F1c C1c F3c . . . 109.6(7) F2c C1c F3c . . . 108.0(7) C1d S1d O1d . . . 103.9(4) C1d S1d O2d . . . 103.8(4) C1d S1d O3d . . . 102.2(4) O1d S1d O2d . . . 115.9(3) O1d S1d O3d . . . 115.3(3) O2d S1d O3d . . . 113.4(3) S1d C1d F1d . . . 110.7(6) S1d C1d F2d . . . 109.7(5) S1d C1d F3d . . . 110.0(6) F1d C1d F2d . . . 108.9(8) F1d C1d F3d . . . 108.2(7) F2d C1d F3d . . . 109.4(7) C1e O1e C3e . . . 113.3(7) O1e C1e C2e . . . 108.8(7) O1e C3e C4e . . . 108.5(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 N2a Mn N1a C1a . . . . -8.7(5) N2a Mn N1a C5a . . . . 174.4(5) N4a Mn N1a C1a . . . . 176.3(5) N4a Mn N1a C5a . . . . -.5(5) N1b Mn N1a C1a . . . . 12.5(7) N1b Mn N1a C5a . . . . -164.3(5) N2b Mn N1a C1a . . . . 74.0(5) N2b Mn N1a C5a . . . . -102.8(5) N4b Mn N1a C1a . . . . -100.5(5) N4b Mn N1a C5a . . . . 82.7(5) N1a Mn N2a C6a . . . . 10.2(4) N1a Mn N2a C7a . . . . 175.5(7) N4a Mn N2a C6a . . . . 18.3(6) N4a Mn N2a C7a . . . . -176.3(6) N1b Mn N2a C6a . . . . -161.2(5) N1b Mn N2a C7a . . . . 4.1(7) N2b Mn N2a C6a . . . . -88.5(5) N2b Mn N2a C7a . . . . 76.9(7) N4b Mn N2a C6a . . . . 128.3(5) N4b Mn N2a C7a . . . . -66.3(7) N1a Mn N4a C9a . . . . 3.4(4) N1a Mn N4a C10a . . . . 175.9(7) N2a Mn N4a C9a . . . . -4.7(6) N2a Mn N4a C10a . . . . 167.8(6) N1b Mn N4a C9a . . . . 174.6(4) N1b Mn N4a C10a . . . . -12.9(8) N2b Mn N4a C9a . . . . 96.1(5) N2b Mn N4a C10a . . . . -91.3(7) N4b Mn N4a C9a . . . . -117.1(5) N4b Mn N4a C10a . . . . 55.4(7) N1a Mn N1b C1b . . . . 57.8(6) N1a Mn N1b C5b . . . . -109.9(6) N2a Mn N1b C1b . . . . 78.0(5) N2a Mn N1b C5b . . . . -89.7(5) N4a Mn N1b C1b . . . . -101.6(5) N4a Mn N1b C5b . . . . 90.7(5) N2b Mn N1b C1b . . . . -8.5(4) N2b Mn N1b C5b . . . . -176.2(5) N4b Mn N1b C1b . . . . -179.4(5) N4b Mn N1b C5b . . . . 12.9(5) N1a Mn N2b C6b . . . . -150.7(5) N1a Mn N2b C7b . . . . 14.8(7) N2a Mn N2b C6b . . . . -80.0(5) N2a Mn N2b C7b . . . . 85.5(7) N4a Mn N2b C6b . . . . 135.8(5) N4a Mn N2b C7b . . . . -58.7(7) N1b Mn N2b C6b . . . . 6.9(5) N1b Mn N2b C7b . . . . 172.4(7) N4b Mn N2b C6b . . . . 21.3(6) N4b Mn N2b C7b . . . . -173.1(6) N1a Mn N4b C9b . . . . 146.0(4) N1a Mn N4b C10b . . . . -22.9(7) N2a Mn N4b C9b . . . . 71.3(5) N2a Mn N4b C10b . . . . -97.5(7) N4a Mn N4b C9b . . . . -142.6(5) N4a Mn N4b C10b . . . . 48.6(7) N1b Mn N4b C9b . . . . -10.4(4) N1b Mn N4b C10b . . . . -179.3(7) N2b Mn N4b C9b . . . . -24.9(6) N2b Mn N4b C10b . . . . 166.2(6) Mn N1a C1a C2a . . . . -176.3(5) Mn N1a C1a C6a . . . . 5.5(7) C5a N1a C1a C2a . . . . .6(9) C5a N1a C1a C6a . . . . -177.6(5) Mn N1a C5a C4a . . . . 177.9(5) Mn N1a C5a C9a . . . . -2.1(7) C1a N1a C5a C4a . . . . 1.0(9) C1a N1a C5a C9a . . . . -179.0(5) Mn N2a C6a N3a . . . . 170.3(4) Mn N2a C6a C1a . . . . -12.1(7) C7a N2a C6a N3a . . . . .0(7) C7a N2a C6a C1a . . . . 177.6(6) Mn N2a C7a C8a . . . . -165.6(5) C6a N2a C7a C8a . . . . .2(7) C8a N3a C6a N2a . . . . -.3(7) C8a N3a C6a C1a . . . . -177.7(6) C6a N3a C8a C7a . . . . .4(7) Mn N4a C9a N5a . . . . 174.8(4) Mn N4a C9a C5a . . . . -6.0(7) C10a N4a C9a N5a . . . . -.3(7) C10a N4a C9a C5a . . . . 178.9(6) Mn N4a C10a C11a . . . . -172.6(5) C9a N4a C10a C11a . . . . .4(7) C11a N5a C9a N4a . . . . .1(7) C11a N5a C9a C5a . . . . -179.0(6) C9a N5a C11a C10a . . . . .2(7) N1a C1a C2a C3a . . . . -.6(9) C6a C1a C2a C3a . . . . 177.4(6) N1a C1a C6a N2a . . . . 5.0(8) N1a C1a C6a N3a . . . . -177.9(6) C2a C1a C6a N2a . . . . -173.1(6) C2a C1a C6a N3a . . . . 4.0(10) C1a C2a C3a C4a . . . . -1.1(10) C2a C3a C4a C5a . . . . 2.5(9) C3a C4a C5a N1a . . . . -2.5(9) C3a C4a C5a C9a . . . . 177.5(6) N1a C5a C9a N4a . . . . 5.5(8) N1a C5a C9a N5a . . . . -175.5(6) C4a C5a C9a N4a . . . . -174.6(6) C4a C5a C9a N5a . . . . 4.4(10) N2a C7a C8a N3a . . . . -.4(8) N4a C10a C11a N5a . . . . -.3(8) Mn N1b C1b C2b . . . . -169.2(5) Mn N1b C1b C6b . . . . 8.3(7) C5b N1b C1b C2b . . . . -1.5(9) C5b N1b C1b C6b . . . . 176.1(6) Mn N1b C5b C4b . . . . 168.8(5) Mn N1b C5b C9b . . . . -12.3(7) C1b N1b C5b C4b . . . . 1.2(10) C1b N1b C5b C9b . . . . -179.9(6) Mn N2b C6b N3b . . . . 170.6(4) Mn N2b C6b C1b . . . . -5.4(8) C7b N2b C6b N3b . . . . .5(7) C7b N2b C6b C1b . . . . -175.6(6) Mn N2b C7b C8b . . . . -166.2(5) C6b N2b C7b C8b . . . . .2(8) C8b N3b C6b N2b . . . . -.9(8) C8b N3b C6b C1b . . . . 174.8(7) C6b N3b C8b C7b . . . . .9(8) Mn N4b C9b N5b . . . . -172.2(4) Mn N4b C9b C5b . . . . 8.5(7) C10b N4b C9b N5b . . . . .6(7) C10b N4b C9b C5b . . . . -178.7(6) Mn N4b C10b C11b . . . . 169.0(5) C9b N4b C10b C11b . . . . -.4(7) C11b N5b C9b N4b . . . . -.5(7) C11b N5b C9b C5b . . . . 178.7(6) C9b N5b C11b C10b . . . . .2(7) N1b C1b C2b C3b . . . . 1.2(10) C6b C1b C2b C3b . . . . -175.9(7) N1b C1b C6b N2b . . . . -1.8(9) N1b C1b C6b N3b . . . . -177.1(6) C2b C1b C6b N2b . . . . 175.6(7) C2b C1b C6b N3b . . . . .3(11) C1b C2b C3b C4b . . . . -.6(11) C2b C3b C4b C5b . . . . .3(11) C3b C4b C5b N1b . . . . -.6(10) C3b C4b C5b C9b . . . . -179.3(7) N1b C5b C9b N4b . . . . 2.1(9) N1b C5b C9b N5b . . . . -177.1(6) C4b C5b C9b N4b . . . . -179.1(7) C4b C5b C9b N5b . . . . 1.8(11) N2b C7b C8b N3b . . . . -.7(8) N4b C10b C11b N5b . . . . .1(8) O1c S1c C1c F1c . . . . -63.3(7) O1c S1c C1c F2c . . . . 178.1(6) O1c S1c C1c F3c . . . . 58.8(6) O2c S1c C1c F1c . . . . 56.5(7) O2c S1c C1c F2c . . . . -62.1(6) O2c S1c C1c F3c . . . . 178.6(6) O3c S1c C1c F1c . . . . 176.7(6) O3c S1c C1c F2c . . . . 58.1(7) O3c S1c C1c F3c . . . . -61.2(7) O1d S1d C1d F1d . . . . -61.8(7) O1d S1d C1d F2d . . . . 178.1(6) O1d S1d C1d F3d . . . . 57.7(6) O2d S1d C1d F1d . . . . 59.9(7) O2d S1d C1d F2d . . . . -60.3(7) O2d S1d C1d F3d . . . . 179.3(6) O3d S1d C1d F1d . . . . 177.9(6) O3d S1d C1d F2d . . . . 57.8(7) O3d S1d C1d F3d . . . . -62.6(6) C3e O1e C1e C2e . . . . 174.1(7) C1e O1e C3e C4e . . . . -174.3(7) 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 H03a O1c . . 3_566 1.08 1.74 2.820(8) 176 N5a H05a O3d . . 4_555 1.08 1.71 2.794(7) 173 N3b H03b O2d . . 4_565 1.08 1.75 2.827(7) 173 N5b H05b O2c . . 2_555 1.08 1.88 2.893(7) 155 #==END==================================================================== data_GILE _database_code_depnum_ccdc_archive 'CCDC 222689' #--- [Mn(1)2](CF3SO3)2 -------------------------------------------------- _audit_creation_date 2000-03-15 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 2003-10-10 _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.0.1 _chemical_formula_moiety '(C11 H9 N5)2 Mn (C F3 S O3)2' _chemical_formula_sum 'C24 H18 F6 Mn N10 O6 S2' _chemical_formula_weight 775.6 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 13.0151(9) _cell_length_b 13.0414(9) _cell_length_c 19.2351(14) _cell_angle_alpha 91.622(8) _cell_angle_beta 105.895(8) _cell_angle_gamma 91.002(8) _cell_volume 3137.7(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_meas not_measured _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 25.96 _cell_measurement_temperature 200 _exptl_absorpt_coefficient_mu 0.646 _exptl_crystal_description prism _exptl_crystal_size_max .40 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .09 _exptl_crystal_colour colourless _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 .8305 _exptl_absorpt_correction_T_max .9451 _diffrn_reflns_number 39439 _reflns_number_total 11429 _reflns_number_gt 6027 _reflns_threshold_expression 'refl observed if Fo > 3.99 \s(Fo)' _diffrn_reflns_theta_max 25.96 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .051 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .037 _refine_ls_wR_factor_ref .037 _refine_ls_goodness_of_fit_ref 1.19(1) _refine_ls_number_reflns 6460 _refine_ls_number_parameters 907 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.0001(Fo^2^)] _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .0004 _refine_diff_density_max .645 _refine_diff_density_min -.416 _refine_ls_extinction_method none _refine_special_details ; Hydrogen treatment: - N-H groups: observed and refined with a fixed value of Uiso. - Other H atoms: calculated ; _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 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 S Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .11 .124 F Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .014 .01 Mn Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .295 .729 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 Mn1 .13079(6) .27084(5) .25704(4) .0320(4) 1.00000 Uani Mn2 .62439(6) .24568(5) .24824(4) .0313(4) 1.00000 Uani N1a .1637(3) .3833(3) .35348(17) .0293(17) 1.00000 Uani N2a .2121(3) .4128(3) .22991(17) .0326(18) 1.00000 Uani N3a .2736(3) .5715(3) .2563(2) .040(2) 1.00000 Uani N4a .0624(3) .2022(3) .34317(18) .0354(18) 1.00000 Uani N5a .0417(4) .2099(3) .4530(2) .042(2) 1.00000 Uani C1a .2100(4) .4749(3) .3500(3) .031(3) 1.00000 Uani C2a .2318(4) .5466(4) .4085(3) .041(3) 1.00000 Uani C3a .2023(4) .5197(4) .4694(3) .044(3) 1.00000 Uani C4a .1541(4) .4253(4) .4734(3) .040(3) 1.00000 Uani C5a .1345(4) .3586(3) .4129(3) .032(3) 1.00000 Uani C6a .2331(4) .4873(3) .2805(3) .030(3) 1.00000 Uani C7a .2406(4) .4509(4) .1714(3) .042(3) 1.00000 Uani C8a .2778(4) .5497(4) .1871(3) .042(3) 1.00000 Uani C9a .0811(4) .2582(3) .4044(3) .032(3) 1.00000 Uani C10a .0095(4) .1148(4) .3537(3) .045(3) 1.00000 Uani C11a -.0033(5) .1184(4) .4220(3) .049(3) 1.00000 Uani N1b .0863(3) .1336(3) .18033(17) .0295(17) 1.00000 Uani N2b -.0214(3) .3063(3) .17385(17) .0334(18) 1.00000 Uani N3b -.1487(4) .2604(3) .0759(2) .039(3) 1.00000 Uani N4b .2607(3) .1527(3) .29072(18) .0373(19) 1.00000 Uani N5b .3147(4) -.0051(3) .2813(3) .044(3) 1.00000 Uani C1b -.0064(4) .1330(3) .1274(2) .031(3) 1.00000 Uani C2b -.0414(4) .0466(4) .0826(3) .036(3) 1.00000 Uani C3b .0217(4) -.0389(3) .0928(3) .037(3) 1.00000 Uani C4b .1168(4) -.0390(3) .1475(3) .036(3) 1.00000 Uani C5b .1458(4) .0497(3) .1902(2) .030(3) 1.00000 Uani C6b -.0601(4) .2311(3) .1258(3) .030(3) 1.00000 Uani C7b -.0879(4) .3872(3) .1531(3) .042(3) 1.00000 Uani C8b -.1670(4) .3603(4) .0928(3) .045(3) 1.00000 Uani C9b .2420(4) .0645(3) .2525(3) .034(3) 1.00000 Uani C10b .3510(4) .1366(4) .3465(3) .049(3) 1.00000 Uani C11b .3846(4) .0397(4) .3413(3) .052(3) 1.00000 Uani N1c .6605(3) .1472(3) .34652(16) .0294(17) 1.00000 Uani N2c .5537(3) .3207(3) .33301(18) .0349(19) 1.00000 Uani N3c .5390(4) .3304(3) .4440(2) .043(3) 1.00000 Uani N4c .7062(3) .1050(3) .22244(17) .0321(18) 1.00000 Uani N5c .7700(4) -.0473(3) .2508(2) .038(2) 1.00000 Uani C1c .7081(4) .0576(3) .3443(2) .031(3) 1.00000 Uani C2c .7339(4) -.0059(4) .4034(3) .044(3) 1.00000 Uani C3c .7053(5) .0272(4) .4655(3) .049(3) 1.00000 Uani C4c .6562(4) .1189(4) .4676(3) .045(3) 1.00000 Uani C5c .6330(4) .1783(3) .4061(2) .031(3) 1.00000 Uani C6c .5777(4) .2751(3) .3959(3) .033(3) 1.00000 Uani C7c .5000(5) .4071(4) .3416(3) .047(3) 1.00000 Uani C8c .4892(5) .4141(4) .4097(3) .050(3) 1.00000 Uani C9c .7302(4) .0377(3) .2741(3) .030(3) 1.00000 Uani C10c .7337(4) .0610(4) .1643(3) .040(3) 1.00000 Uani C11c .7721(4) -.0343(4) .1811(3) .041(3) 1.00000 Uani N1d .5829(3) .3803(3) .17584(17) .0285(17) 1.00000 Uani N2d .7590(3) .3665(3) .28354(18) .0350(18) 1.00000 Uani N3d .8175(4) .5247(3) .2802(2) .039(2) 1.00000 Uani N4d .4705(3) .2055(3) .16564(17) .0337(18) 1.00000 Uani N5d .3422(4) .2473(3) .0702(2) .038(3) 1.00000 Uani C1d .4901(4) .3779(3) .1238(2) .031(3) 1.00000 Uani C2d .4557(4) .4624(3) .0813(3) .036(3) 1.00000 Uani C3d .5214(4) .5507(3) .0948(3) .036(3) 1.00000 Uani C4d .6172(4) .5530(3) .1492(3) .035(3) 1.00000 Uani C5d .6448(4) .4660(3) .1888(2) .029(3) 1.00000 Uani C6d .7414(4) .4534(3) .2500(3) .033(3) 1.00000 Uani C7d .8527(4) .3824(4) .3386(3) .041(3) 1.00000 Uani C8d .8889(4) .4807(4) .3367(3) .046(3) 1.00000 Uani C9d .4332(4) .2794(3) .1191(3) .032(3) 1.00000 Uani C10d .3987(4) .1238(4) .1437(3) .041(3) 1.00000 Uani C11d .3195(4) .1486(4) .0846(3) .044(3) 1.00000 Uani S1e .14585(10) .32445(8) -.08766(6) .0354(6) 1.00000 Uani O1e .2210(3) .3859(3) -.03239(16) .0510(17) 1.00000 Uani O2e .1598(3) .2162(3) -.07967(17) .0477(18) 1.00000 Uani O3e .1288(3) .3609(3) -.15890(16) .0554(19) 1.00000 Uani C1e .0190(5) .3449(4) -.0679(3) .053(3) 1.00000 Uani F1e .0252(4) .3139(3) -.0011(2) .102(3) 1.00000 Uani F2e -.0590(3) .2908(3) -.1129(3) .090(3) 1.00000 Uani F3e -.0071(3) .4423(3) -.07064(19) .075(2) 1.00000 Uani S1f .34748(10) .82487(8) .08626(6) .0355(6) 1.00000 Uani O1f .2729(3) .8819(3) .03241(15) .0484(17) 1.00000 Uani O2f .3336(3) .7160(3) .07514(17) .0466(17) 1.00000 Uani O3f .3637(3) .8637(3) .15842(16) .0572(19) 1.00000 Uani C1f .4746(5) .8500(4) .0668(3) .051(3) 1.00000 Uani F1f .4709(4) .8157(3) .0007(3) .100(3) 1.00000 Uani F2f .5528(3) .8022(3) .1123(3) .089(3) 1.00000 Uani F3f .5003(3) .9492(3) .0714(2) .080(3) 1.00000 Uani S1g -.04515(10) .77844(8) .36316(6) .0373(6) 1.00000 Uani O1g -.1365(3) .7545(3) .30279(16) .0486(17) 1.00000 Uani O2g -.0459(3) .8782(3) .39537(17) .0534(19) 1.00000 Uani O3g -.0163(3) .6978(3) .41447(15) .0486(18) 1.00000 Uani C1g .0664(5) .7855(5) .3229(3) .059(4) 1.00000 Uani F1g .0793(3) .6967(3) .29229(16) .080(3) 1.00000 Uani F2g .0498(4) .8557(3) .2737(2) .099(3) 1.00000 Uani F3g .1559(3) .8099(3) .3730(3) .097(3) 1.00000 Uani S1h .46822(11) .75420(9) .37328(7) .0438(7) 1.00000 Uani O1h .5082(3) .8394(3) .42131(18) .063(3) 1.00000 Uani O2h .4585(3) .6610(3) .40884(18) .059(2) 1.00000 Uani O3h .3753(3) .7717(3) .31383(17) .057(2) 1.00000 Uani C1h .5735(6) .7296(5) .3295(4) .068(4) 1.00000 Uani F1h .5930(4) .8093(3) .29535(18) .093(3) 1.00000 Uani F2h .6636(4) .7072(4) .3785(3) .118(4) 1.00000 Uani F3h .5465(4) .6513(3) .2832(3) .107(3) 1.00000 Uani H03a .289(4) .633(4) .280(3) .05000 1.00000 Uiso H05a .042(4) .229(4) .496(3) .05000 1.00000 Uiso H2a .27010 .62125 .40452 .05000 1.00000 Uiso H3a .21721 .57485 .51585 .05000 1.00000 Uiso H4a .13173 .40371 .52276 .05000 1.00000 Uiso H7a .23296 .40844 .11996 .05000 1.00000 Uiso H8a .30484 .60097 .15113 .05000 1.00000 Uiso H10a -.01589 .05032 .31418 .05000 1.00000 Uiso H11a -.04137 .05882 .44701 .05000 1.00000 Uiso H03b -.186(4) .221(4) .041(3) .05000 1.00000 Uiso H05b .314(4) -.067(4) .262(3) .05000 1.00000 Uiso H2b -.11807 .04727 .04000 .05000 1.00000 Uiso H3b -.00349 -.10806 .05761 .05000 1.00000 Uiso H4b .16706 -.10659 .15673 .05000 1.00000 Uiso H7b -.07834 .46283 .18139 .05000 1.00000 Uiso H8b -.23171 .40821 .06273 .05000 1.00000 Uiso H10b .39130 .19364 .38909 .05000 1.00000 Uiso H11b .45373 .00341 .37766 .05000 1.00000 Uiso H03c .536(5) .310(4) .480(3) .05000 1.00000 Uiso H05c .787(4) -.101(4) .275(3) .05000 1.00000 Uiso H2c .77551 -.07825 .40087 .05000 1.00000 Uiso H3c .72146 -.02266 .51240 .05000 1.00000 Uiso H4c .63383 .14559 .51625 .05000 1.00000 Uiso H7c .47063 .46351 .29923 .05000 1.00000 Uiso H8c .44794 .47420 .43251 .05000 1.00000 Uiso H10c .72475 .09704 .11217 .05000 1.00000 Uiso H11c .80093 -.08905 .14631 .05000 1.00000 Uiso H03d .814(5) .580(4) .269(3) .05000 1.00000 Uiso H05d .302(4) .281(4) .040(3) .05000 1.00000 Uiso H2d .37949 .45925 .03878 .05000 1.00000 Uiso H3d .49768 .61807 .06193 .05000 1.00000 Uiso H4d .66850 .62306 .16017 .05000 1.00000 Uiso H7d .89189 .32469 .37744 .05000 1.00000 Uiso H8d .96101 .51747 .37326 .05000 1.00000 Uiso H10d .40546 .04934 .17001 .05000 1.00000 Uiso H11d .25291 .09891 .05499 .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 Mn1 .0385(5) .0272(4) .0327(4) -.0033(4) .0147(3) -.0036(3) Mn2 .0363(5) .0259(4) .0346(4) .0042(3) .0138(3) .0059(3) N1a .032(3) .0250(17) .0323(19) -.0019(16) .0109(16) -.0015(14) N2a .037(3) .0302(18) .0355(19) -.0026(16) .0182(16) .0002(15) N3a .043(3) .0274(19) .052(3) -.0025(18) .0204(19) .0017(16) N4a .042(3) .0307(18) .037(2) -.0029(17) .0174(17) .0017(15) N5a .050(3) .044(3) .034(2) -.008(2) .0151(19) .0070(17) C1a .028(3) .031(3) .036(3) -.001(2) .0133(19) -.0004(17) C2a .041(4) .035(3) .048(3) -.006(3) .014(3) -.007(2) C3a .051(4) .048(3) .036(3) -.012(3) .015(3) -.013(2) C4a .047(4) .044(3) .030(3) -.008(3) .013(3) -.0044(19) C5a .028(3) .033(3) .035(3) .002(2) .0094(19) .0052(18) C6a .028(3) .024(3) .041(3) .0008(19) .0145(19) .0016(18) C7a .044(4) .051(3) .040(3) -.002(3) .024(3) .003(2) C8a .046(4) .043(3) .045(3) .003(3) .024(3) .010(2) C9a .034(3) .032(3) .032(3) -.001(2) .0134(19) .0058(18) C10a .055(4) .033(3) .051(3) -.014(3) .021(3) -.000(2) C11a .057(4) .042(3) .052(3) -.012(3) .022(3) .008(3) N1b .035(3) .0261(18) .0299(18) -.0003(17) .0137(17) .0018(14) N2b .041(3) .0260(18) .038(2) .0022(17) .0193(17) .0011(15) N3b .044(3) .037(3) .038(3) .0031(19) .0120(19) .0010(16) N4b .036(3) .035(2) .042(3) -.0037(18) .0126(18) -.0041(16) N5b .042(3) .032(2) .057(3) .002(2) .008(2) .0032(18) C1b .040(3) .029(3) .029(3) -.000(2) .018(2) .0026(17) C2b .038(3) .036(3) .035(3) -.005(3) .014(2) -.0033(18) C3b .048(4) .028(3) .039(3) -.005(3) .018(3) -.0072(18) C4b .043(4) .027(3) .041(3) .001(2) .019(3) .0006(18) C5b .036(3) .025(3) .036(3) .002(2) .018(2) .0040(17) C6b .026(3) .034(3) .034(3) -.000(2) .013(2) .0015(18) C7b .054(4) .029(3) .049(3) .008(3) .023(3) .006(2) C8b .045(4) .043(3) .049(3) .013(3) .016(3) .010(3) C9b .034(3) .031(3) .040(3) .003(3) .015(3) .0043(19) C10b .035(4) .050(3) .055(3) -.001(3) .002(3) -.005(3) C11b .032(4) .056(4) .059(4) .001(3) -.005(3) .009(3) N1c .033(3) .0262(18) .0308(18) .0005(16) .0126(16) .0021(14) N2c .036(3) .0330(19) .039(3) .0072(17) .0146(17) .0014(16) N3c .042(3) .052(3) .036(3) .004(3) .013(2) -.0066(19) N4c .036(3) .0295(18) .0347(19) .0055(16) .0159(16) .0051(15) N5c .044(3) .0255(19) .048(3) .0070(18) .0206(19) .0037(16) C1c .034(3) .030(3) .033(3) .000(2) .0126(19) .0054(17) C2c .045(4) .046(3) .046(3) .011(3) .018(3) .015(3) C3c .053(4) .055(3) .042(3) .013(3) .018(3) .018(3) C4c .050(4) .055(3) .034(3) .005(3) .017(3) .002(3) C5c .029(3) .036(3) .030(3) .001(2) .0087(18) -.0015(18) C6c .030(3) .038(3) .031(3) -.001(3) .0108(19) -.0068(19) C7c .047(4) .037(3) .059(4) .014(3) .017(3) -.004(3) C8c .046(4) .047(3) .056(4) .015(3) .014(3) -.007(3) C9c .025(3) .024(3) .044(3) .0029(19) .014(2) .0016(18) C10c .047(4) .041(3) .040(3) .002(3) .025(3) .000(2) C11c .042(4) .044(3) .042(3) .001(3) .020(3) -.005(2) N1d .032(3) .0235(17) .0313(18) .0033(16) .0098(16) .0028(14) N2d .035(3) .0294(18) .042(2) .0018(17) .0128(18) .0047(15) N3d .041(3) .0279(19) .049(3) .002(2) .0126(19) .0006(18) N4d .041(3) .0259(18) .0363(19) .0019(17) .0144(17) .0017(15) N5d .034(3) .041(3) .037(3) .0010(19) .0059(18) -.0011(17) C1d .037(3) .032(3) .028(3) .002(2) .016(2) .0006(17) C2d .043(4) .035(3) .035(3) .012(3) .016(3) .0087(18) C3d .044(4) .030(3) .039(3) .007(3) .017(3) .0086(18) C4d .041(4) .029(3) .039(3) .004(2) .019(3) .0047(18) C5d .031(3) .027(3) .034(3) .0055(19) .0145(19) .0016(17) C6d .037(3) .027(3) .038(3) -.003(2) .017(3) -.0007(18) C7d .038(4) .042(3) .042(3) .006(3) .007(3) .007(2) C8d .041(4) .045(3) .048(3) -.003(3) .007(3) -.003(3) C9d .037(3) .030(3) .031(3) .002(2) .014(2) -.0018(18) C10d .046(4) .031(3) .048(3) -.007(3) .018(3) -.005(2) C11d .048(4) .041(3) .044(3) -.012(3) .013(3) -.007(3) S1e .0371(8) .0353(6) .0364(6) -.0004(6) .0145(5) -.0001(5) O1e .046(3) .0478(18) .0497(19) -.0066(16) -.0020(16) -.0003(15) O2e .046(3) .0373(17) .064(2) .0075(16) .0217(17) .0012(14) O3e .067(3) .067(3) .0347(17) -.0009(19) .0177(16) .0064(15) C1e .053(4) .041(3) .074(4) .007(3) .032(3) .003(3) F1e .125(4) .116(3) .103(3) .025(3) .091(3) .037(3) F2e .037(3) .066(2) .161(4) -.0065(17) .018(3) -.007(3) F3e .071(3) .0445(17) .123(3) .0176(16) .049(2) .0007(16) S1f .0367(8) .0361(6) .0353(6) .0026(6) .0124(5) .0032(5) O1f .047(3) .0476(18) .0437(18) .0078(16) -.0004(16) .0069(14) O2f .041(3) .0387(17) .065(2) .0010(15) .0220(16) .0049(14) O3f .067(3) .069(3) .0364(18) .0092(19) .0158(17) -.0036(15) C1f .047(4) .037(3) .072(4) .000(3) .024(3) -.002(3) F1f .115(4) .106(3) .114(3) -.016(3) .092(3) -.022(3) F2f .040(3) .065(2) .158(4) .0065(17) .019(3) .010(3) F3f .075(3) .0468(18) .134(3) -.0130(17) .053(3) .0041(17) S1g .0483(9) .0328(6) .0358(6) .0048(6) .0193(6) .0054(5) O1g .050(3) .0464(18) .0479(19) .0033(16) .0111(16) .0061(14) O2g .073(3) .0340(17) .057(2) .0069(17) .0235(18) -.0012(14) O3g .070(3) .0377(17) .0427(18) .0098(16) .0218(16) .0116(14) C1g .055(5) .069(4) .061(4) .007(3) .027(3) .008(3) F1g .085(3) .103(3) .063(2) .040(3) .0366(18) .0001(18) F2g .122(4) .105(3) .098(3) .016(3) .074(3) .051(3) F3g .044(3) .135(4) .112(3) -.013(3) .024(3) -.003(3) S1h .0517(9) .0410(7) .0458(7) -.0006(6) .0254(7) .0019(6) O1h .071(3) .057(3) .062(3) -.0050(19) .0219(19) -.0165(17) O2h .069(3) .0500(19) .064(3) -.0057(18) .0270(19) .0152(16) O3h .061(3) .051(2) .058(3) .0017(18) .0133(19) .0030(16) C1h .078(6) .065(4) .076(4) -.008(4) .047(4) -.006(4) F1h .110(4) .104(3) .084(3) -.039(3) .059(3) .0058(19) F2h .064(3) .162(4) .141(4) .036(3) .049(3) .029(3) F3h .148(4) .085(3) .121(3) -.009(3) .094(3) -.038(3) 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 Mn1 N1a . . 2.272(3) Mn1 N2a . . 2.260(4) Mn1 N4a . . 2.281(4) Mn1 N1b . . 2.250(3) Mn1 N2b . . 2.244(4) Mn1 N4b . . 2.281(4) Mn2 N1c . . 2.262(4) Mn2 N2c . . 2.286(4) Mn2 N4c . . 2.247(4) Mn2 N1d . . 2.252(3) Mn2 N2d . . 2.281(4) Mn2 N4d . . 2.233(4) N1a C1a . . 1.341(5) N1a C5a . . 1.344(6) N2a C6a . . 1.325(5) N2a C7a . . 1.380(6) N3a C6a . . 1.358(6) N3a C8a . . 1.369(7) N3a H03a . . .90(5) N4a C9a . . 1.329(5) N4a C10a . . 1.370(6) N5a C9a . . 1.349(6) N5a C11a . . 1.367(6) N5a H05a . . .85(5) C1a C2a . . 1.406(6) C1a C6a . . 1.461(7) C2a C3a . . 1.381(7) C3a C4a . . 1.386(7) C4a C5a . . 1.397(6) C5a C9a . . 1.455(6) C7a C8a . . 1.364(6) C10a C11a . . 1.368(8) N1b C1b . . 1.349(5) N1b C5b . . 1.339(5) N2b C6b . . 1.323(5) N2b C7b . . 1.374(6) N3b C6b . . 1.352(6) N3b C8b . . 1.375(6) N3b H03b . . .86(5) N4b C9b . . 1.329(5) N4b C10b . . 1.382(6) N5b C9b . . 1.341(6) N5b C11b . . 1.367(6) N5b H05b . . .88(5) C1b C2b . . 1.389(6) C1b C6b . . 1.465(6) C2b C3b . . 1.383(6) C3b C4b . . 1.387(6) C4b C5b . . 1.384(6) C5b C9b . . 1.482(6) C7b C8b . . 1.356(6) C10b C11b . . 1.354(7) N1c C1c . . 1.338(5) N1c C5c . . 1.346(6) N2c C6c . . 1.324(6) N2c C7c . . 1.367(6) N3c C6c . . 1.364(7) N3c C8c . . 1.370(6) N3c H03c . . .76(6) N4c C9c . . 1.321(5) N4c C10c . . 1.378(6) N5c C9c . . 1.348(6) N5c C11c . . 1.364(7) N5c H05c . . .84(5) C1c C2c . . 1.395(6) C1c C9c . . 1.472(7) C2c C3c . . 1.403(8) C3c C4c . . 1.371(7) C4c C5c . . 1.397(6) C5c C6c . . 1.456(6) C7c C8c . . 1.355(8) C10c C11c . . 1.362(7) N1d C1d . . 1.341(5) N1d C5d . . 1.343(5) N2d C6d . . 1.312(5) N2d C7d . . 1.386(5) N3d C6d . . 1.344(6) N3d C8d . . 1.368(6) N3d H03d . . .76(5) N4d C9d . . 1.340(5) N4d C10d . . 1.382(6) N5d C9d . . 1.347(6) N5d C11d . . 1.369(6) N5d H05d . . .81(5) C1d C2d . . 1.396(6) C1d C9d . . 1.459(6) C2d C3d . . 1.397(6) C3d C4d . . 1.390(6) C4d C5d . . 1.382(6) C5d C6d . . 1.484(6) C7d C8d . . 1.363(7) C10d C11d . . 1.359(6) S1e O1e . . 1.444(3) S1e O2e . . 1.434(3) S1e O3e . . 1.424(4) S1e C1e . . 1.815(7) C1e F1e . . 1.340(7) C1e F2e . . 1.318(6) C1e F3e . . 1.319(6) S1f O1f . . 1.444(3) S1f O2f . . 1.431(3) S1f O3f . . 1.422(4) S1f C1f . . 1.819(7) C1f F1f . . 1.325(7) C1f F2f . . 1.325(6) C1f F3f . . 1.325(6) S1g O1g . . 1.439(3) S1g O2g . . 1.427(4) S1g O3g . . 1.445(3) S1g C1g . . 1.825(7) C1g F1g . . 1.318(7) C1g F2g . . 1.313(7) C1g F3g . . 1.319(7) S1h O1h . . 1.420(4) S1h O2h . . 1.431(4) S1h O3h . . 1.445(4) S1h C1h . . 1.823(9) C1h F1h . . 1.303(8) C1h F2h . . 1.330(8) C1h F3h . . 1.313(7) 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 N1a Mn1 N2a . . . 71.77(12) N1a Mn1 N4a . . . 71.49(12) N1a Mn1 N1b . . . 165.92(13) N1a Mn1 N2b . . . 111.33(12) N1a Mn1 N4b . . . 103.93(11) N2a Mn1 N4a . . . 143.17(12) N2a Mn1 N1b . . . 122.18(13) N2a Mn1 N2b . . . 90.87(12) N2a Mn1 N4b . . . 106.12(13) N4a Mn1 N1b . . . 94.64(12) N4a Mn1 N2b . . . 99.90(14) N4a Mn1 N4b . . . 85.26(14) N1b Mn1 N2b . . . 72.63(12) N1b Mn1 N4b . . . 71.65(11) N2b Mn1 N4b . . . 144.21(12) N1c Mn2 N2c . . . 71.52(12) N1c Mn2 N4c . . . 72.25(13) N1c Mn2 N1d . . . 162.30(12) N1c Mn2 N2d . . . 100.53(11) N1c Mn2 N4d . . . 114.59(12) N2c Mn2 N4c . . . 143.56(13) N2c Mn2 N1d . . . 91.90(13) N2c Mn2 N2d . . . 86.36(13) N2c Mn2 N4d . . . 97.58(13) N4c Mn2 N1d . . . 124.54(13) N4c Mn2 N2d . . . 103.99(13) N4c Mn2 N4d . . . 93.82(12) N1d Mn2 N2d . . . 71.47(11) N1d Mn2 N4d . . . 72.77(12) N2d Mn2 N4d . . . 144.13(12) Mn1 N1a C1a . . . 119.5(3) Mn1 N1a C5a . . . 119.9(3) C1a N1a C5a . . . 120.5(4) Mn1 N2a C6a . . . 115.2(3) Mn1 N2a C7a . . . 138.2(3) C6a N2a C7a . . . 106.4(4) C6a N3a C8a . . . 107.9(4) C6a N3a H03a . . . 126(4) C8a N3a H03a . . . 125(4) Mn1 N4a C9a . . . 114.7(3) Mn1 N4a C10a . . . 139.1(3) C9a N4a C10a . . . 106.1(4) C9a N5a C11a . . . 107.8(4) C9a N5a H05a . . . 130(4) C11a N5a H05a . . . 122(4) N1a C1a C2a . . . 121.3(4) N1a C1a C6a . . . 111.8(4) C2a C1a C6a . . . 126.9(4) C1a C2a C3a . . . 117.5(4) C2a C3a C4a . . . 121.6(4) C3a C4a C5a . . . 117.4(5) N1a C5a C4a . . . 121.6(4) N1a C5a C9a . . . 111.8(4) C4a C5a C9a . . . 126.5(5) N2a C6a N3a . . . 110.3(4) N2a C6a C1a . . . 121.6(4) N3a C6a C1a . . . 128.1(4) N2a C7a C8a . . . 109.4(4) N3a C8a C7a . . . 106.1(5) N4a C9a N5a . . . 110.6(4) N4a C9a C5a . . . 121.9(4) N5a C9a C5a . . . 127.5(4) N4a C10a C11a . . . 109.4(4) N5a C11a C10a . . . 106.1(5) Mn1 N1b C1b . . . 119.1(3) Mn1 N1b C5b . . . 121.0(3) C1b N1b C5b . . . 119.7(3) Mn1 N2b C6b . . . 114.7(3) Mn1 N2b C7b . . . 139.4(3) C6b N2b C7b . . . 105.8(4) C6b N3b C8b . . . 107.5(4) C6b N3b H03b . . . 124(3) C8b N3b H03b . . . 129(3) Mn1 N4b C9b . . . 115.1(3) Mn1 N4b C10b . . . 139.3(3) C9b N4b C10b . . . 104.9(4) C9b N5b C11b . . . 107.7(4) C9b N5b H05b . . . 123(3) C11b N5b H05b . . . 129(3) N1b C1b C2b . . . 121.1(4) N1b C1b C6b . . . 111.5(4) C2b C1b C6b . . . 127.5(4) C1b C2b C3b . . . 118.5(4) C2b C3b C4b . . . 120.7(4) C3b C4b C5b . . . 117.4(4) N1b C5b C4b . . . 122.6(4) N1b C5b C9b . . . 111.4(4) C4b C5b C9b . . . 125.9(4) N2b C6b N3b . . . 110.9(4) N2b C6b C1b . . . 121.9(4) N3b C6b C1b . . . 127.2(4) N2b C7b C8b . . . 110.1(4) N3b C8b C7b . . . 105.8(4) N4b C9b N5b . . . 111.4(4) N4b C9b C5b . . . 120.7(4) N5b C9b C5b . . . 127.8(4) N4b C10b C11b . . . 110.0(4) N5b C11b C10b . . . 106.1(4) Mn2 N1c C1c . . . 119.3(3) Mn2 N1c C5c . . . 120.1(3) C1c N1c C5c . . . 120.6(4) Mn2 N2c C6c . . . 114.3(3) Mn2 N2c C7c . . . 138.6(4) C6c N2c C7c . . . 106.7(4) C6c N3c C8c . . . 108.0(4) C6c N3c H03c . . . 123(4) C8c N3c H03c . . . 128(4) Mn2 N4c C9c . . . 115.3(3) Mn2 N4c C10c . . . 138.5(3) C9c N4c C10c . . . 105.9(4) C9c N5c C11c . . . 108.4(4) C9c N5c H05c . . . 125(4) C11c N5c H05c . . . 126(4) N1c C1c C2c . . . 122.0(4) N1c C1c C9c . . . 111.9(4) C2c C1c C9c . . . 126.0(4) C1c C2c C3c . . . 117.0(5) C2c C3c C4c . . . 120.9(5) C3c C4c C5c . . . 118.7(5) N1c C5c C4c . . . 120.7(4) N1c C5c C6c . . . 111.7(4) C4c C5c C6c . . . 127.6(5) N2c C6c N3c . . . 109.5(4) N2c C6c C5c . . . 121.9(4) N3c C6c C5c . . . 128.5(4) N2c C7c C8c . . . 110.1(4) N3c C8c C7c . . . 105.7(5) N4c C9c N5c . . . 110.4(4) N4c C9c C1c . . . 121.2(4) N5c C9c C1c . . . 128.3(4) N4c C10c C11c . . . 109.7(4) N5c C11c C10c . . . 105.6(4) Mn2 N1d C1d . . . 119.1(3) Mn2 N1d C5d . . . 120.6(3) C1d N1d C5d . . . 119.9(4) Mn2 N2d C6d . . . 115.3(3) Mn2 N2d C7d . . . 138.1(3) C6d N2d C7d . . . 105.9(4) C6d N3d C8d . . . 107.4(4) C6d N3d H03d . . . 123(4) C8d N3d H03d . . . 129(4) Mn2 N4d C9d . . . 114.6(3) Mn2 N4d C10d . . . 140.0(3) C9d N4d C10d . . . 105.3(4) C9d N5d C11d . . . 108.4(4) C9d N5d H05d . . . 128(4) C11d N5d H05d . . . 123(4) N1d C1d C2d . . . 121.7(4) N1d C1d C9d . . . 111.8(4) C2d C1d C9d . . . 126.4(4) C1d C2d C3d . . . 117.8(4) C2d C3d C4d . . . 120.3(4) C3d C4d C5d . . . 118.1(4) N1d C5d C4d . . . 122.2(4) N1d C5d C6d . . . 111.1(4) C4d C5d C6d . . . 126.7(4) N2d C6d N3d . . . 111.5(4) N2d C6d C5d . . . 121.1(4) N3d C6d C5d . . . 127.4(4) N2d C7d C8d . . . 108.8(4) N3d C8d C7d . . . 106.3(4) N4d C9d N5d . . . 110.4(4) N4d C9d C1d . . . 121.5(4) N5d C9d C1d . . . 128.1(4) N4d C10d C11d . . . 110.1(4) N5d C11d C10d . . . 105.8(4) O1e S1e O2e . . . 113.46(17) O1e S1e O3e . . . 114.4(2) O1e S1e C1e . . . 103.6(3) O2e S1e O3e . . . 116.4(2) O2e S1e C1e . . . 103.2(3) O3e S1e C1e . . . 103.6(3) S1e C1e F1e . . . 109.3(4) S1e C1e F2e . . . 111.4(4) S1e C1e F3e . . . 112.5(4) F1e C1e F2e . . . 107.2(5) F1e C1e F3e . . . 107.8(5) F2e C1e F3e . . . 108.5(4) O1f S1f O2f . . . 113.56(17) O1f S1f O3f . . . 114.3(2) O1f S1f C1f . . . 103.3(3) O2f S1f O3f . . . 116.5(2) O2f S1f C1f . . . 102.8(3) O3f S1f C1f . . . 104.2(3) S1f C1f F1f . . . 110.4(4) S1f C1f F2f . . . 110.9(4) S1f C1f F3f . . . 112.2(4) F1f C1f F2f . . . 107.2(5) F1f C1f F3f . . . 107.8(5) F2f C1f F3f . . . 108.0(4) O1g S1g O2g . . . 114.13(19) O1g S1g O3g . . . 114.73(19) O1g S1g C1g . . . 104.1(3) O2g S1g O3g . . . 114.27(18) O2g S1g C1g . . . 104.0(3) O3g S1g C1g . . . 103.8(3) S1g C1g F1g . . . 111.1(5) S1g C1g F2g . . . 110.3(5) S1g C1g F3g . . . 110.2(5) F1g C1g F2g . . . 108.7(5) F1g C1g F3g . . . 108.0(5) F2g C1g F3g . . . 108.4(5) O1h S1h O2h . . . 114.0(2) O1h S1h O3h . . . 116.3(2) O1h S1h C1h . . . 104.2(3) O2h S1h O3h . . . 112.4(2) O2h S1h C1h . . . 104.2(3) O3h S1h C1h . . . 103.9(3) S1h C1h F1h . . . 111.5(5) S1h C1h F2h . . . 110.2(5) S1h C1h F3h . . . 110.5(5) F1h C1h F2h . . . 107.9(6) F1h C1h F3h . . . 108.7(6) F2h C1h F3h . . . 107.9(6) 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 N2a Mn1 N1a C1a . . . . 1.3(3) N2a Mn1 N1a C5a . . . . 179.8(4) N4a Mn1 N1a C1a . . . . -176.0(4) N4a Mn1 N1a C5a . . . . 2.5(3) N1b Mn1 N1a C1a . . . . 173.8(5) N1b Mn1 N1a C5a . . . . -7.7(7) N2b Mn1 N1a C1a . . . . -82.3(4) N2b Mn1 N1a C5a . . . . 96.2(3) N4b Mn1 N1a C1a . . . . 103.9(3) N4b Mn1 N1a C5a . . . . -77.5(3) N1a Mn1 N2a C6a . . . . -2.2(3) N1a Mn1 N2a C7a . . . . -175.3(5) N4a Mn1 N2a C6a . . . . 2.1(4) N4a Mn1 N2a C7a . . . . -171.0(4) N1b Mn1 N2a C6a . . . . 179.9(3) N1b Mn1 N2a C7a . . . . 6.8(5) N2b Mn1 N2a C6a . . . . 110.0(3) N2b Mn1 N2a C7a . . . . -63.1(5) N4b Mn1 N2a C6a . . . . -101.9(3) N4b Mn1 N2a C7a . . . . 85.0(5) N1a Mn1 N4a C9a . . . . -3.3(3) N1a Mn1 N4a C10a . . . . -179.2(5) N2a Mn1 N4a C9a . . . . -7.6(4) N2a Mn1 N4a C10a . . . . 176.4(4) N1b Mn1 N4a C9a . . . . 174.2(3) N1b Mn1 N4a C10a . . . . -1.7(5) N2b Mn1 N4a C9a . . . . -112.6(3) N2b Mn1 N4a C10a . . . . 71.4(5) N4b Mn1 N4a C9a . . . . 103.1(3) N4b Mn1 N4a C10a . . . . -72.8(5) N1a Mn1 N1b C1b . . . . 104.6(6) N1a Mn1 N1b C5b . . . . -69.7(7) N2a Mn1 N1b C1b . . . . -83.8(4) N2a Mn1 N1b C5b . . . . 101.9(4) N4a Mn1 N1b C1b . . . . 94.9(4) N4a Mn1 N1b C5b . . . . -79.4(4) N2b Mn1 N1b C1b . . . . -4.0(4) N2b Mn1 N1b C5b . . . . -178.4(4) N4b Mn1 N1b C1b . . . . 178.4(4) N4b Mn1 N1b C5b . . . . 4.0(4) N1a Mn1 N2b C6b . . . . -163.6(4) N1a Mn1 N2b C7b . . . . 21.4(6) N2a Mn1 N2b C6b . . . . 125.7(4) N2a Mn1 N2b C7b . . . . -49.3(6) N4a Mn1 N2b C6b . . . . -89.7(4) N4a Mn1 N2b C7b . . . . 95.3(6) N1b Mn1 N2b C6b . . . . 2.1(4) N1b Mn1 N2b C7b . . . . -172.9(6) N4b Mn1 N2b C6b . . . . 6.0(5) N4b Mn1 N2b C7b . . . . -169.1(5) N1a Mn1 N4b C9b . . . . 162.3(4) N1a Mn1 N4b C10b . . . . -6.2(6) N2a Mn1 N4b C9b . . . . -123.0(4) N2a Mn1 N4b C10b . . . . 68.5(6) N4a Mn1 N4b C9b . . . . 92.7(4) N4a Mn1 N4b C10b . . . . -75.8(6) N1b Mn1 N4b C9b . . . . -3.7(4) N1b Mn1 N4b C10b . . . . -172.2(6) N2b Mn1 N4b C9b . . . . -7.6(5) N2b Mn1 N4b C10b . . . . -176.1(5) N2c Mn2 N1c C1c . . . . 175.0(4) N2c Mn2 N1c C5c . . . . -4.1(3) N4c Mn2 N1c C1c . . . . -1.0(3) N4c Mn2 N1c C5c . . . . 179.8(4) N1d Mn2 N1c C1c . . . . -163.8(4) N1d Mn2 N1c C5c . . . . 17.1(6) N2d Mn2 N1c C1c . . . . -102.5(3) N2d Mn2 N1c C5c . . . . 78.4(4) N4d Mn2 N1c C1c . . . . 85.0(4) N4d Mn2 N1c C5c . . . . -94.1(3) N1c Mn2 N2c C6c . . . . 5.7(3) N1c Mn2 N2c C7c . . . . 177.7(5) N4c Mn2 N2c C6c . . . . 12.1(4) N4c Mn2 N2c C7c . . . . -175.9(4) N1d Mn2 N2c C6c . . . . -168.0(3) N1d Mn2 N2c C7c . . . . 4.0(5) N2d Mn2 N2c C6c . . . . -96.7(3) N2d Mn2 N2c C7c . . . . 75.3(5) N4d Mn2 N2c C6c . . . . 119.2(3) N4d Mn2 N2c C7c . . . . -68.8(5) N1c Mn2 N4c C9c . . . . 1.8(3) N1c Mn2 N4c C10c . . . . 175.3(5) N2c Mn2 N4c C9c . . . . -4.6(4) N2c Mn2 N4c C10c . . . . 168.9(4) N1d Mn2 N4c C9c . . . . 175.5(3) N1d Mn2 N4c C10c . . . . -11.0(5) N2d Mn2 N4c C9c . . . . 98.6(3) N2d Mn2 N4c C10c . . . . -87.9(5) N4d Mn2 N4c C9c . . . . -112.8(3) N4d Mn2 N4c C10c . . . . 60.7(5) N1c Mn2 N1d C1d . . . . -113.7(5) N1c Mn2 N1d C5d . . . . 59.8(6) N2c Mn2 N1d C1d . . . . -93.6(4) N2c Mn2 N1d C5d . . . . 79.9(4) N4c Mn2 N1d C1d . . . . 86.4(4) N4c Mn2 N1d C5d . . . . -100.1(4) N2d Mn2 N1d C1d . . . . -179.1(4) N2d Mn2 N1d C5d . . . . -5.6(4) N4d Mn2 N1d C1d . . . . 3.8(4) N4d Mn2 N1d C5d . . . . 177.2(4) N1c Mn2 N2d C6d . . . . -158.0(4) N1c Mn2 N2d C7d . . . . 10.8(5) N2c Mn2 N2d C6d . . . . -87.6(4) N2c Mn2 N2d C7d . . . . 81.2(5) N4c Mn2 N2d C6d . . . . 127.8(4) N4c Mn2 N2d C7d . . . . -63.4(5) N1d Mn2 N2d C6d . . . . 5.7(4) N1d Mn2 N2d C7d . . . . 174.4(5) N4d Mn2 N2d C6d . . . . 10.3(5) N4d Mn2 N2d C7d . . . . 179.1(5) N1c Mn2 N4d C9d . . . . 161.2(3) N1c Mn2 N4d C10d . . . . -22.1(6) N2c Mn2 N4d C9d . . . . 88.1(4) N2c Mn2 N4d C10d . . . . -95.2(5) N4c Mn2 N4d C9d . . . . -126.6(4) N4c Mn2 N4d C10d . . . . 50.1(6) N1d Mn2 N4d C9d . . . . -1.5(4) N1d Mn2 N4d C10d . . . . 175.2(6) N2d Mn2 N4d C9d . . . . -6.2(5) N2d Mn2 N4d C10d . . . . 170.5(5) Mn1 N1a C1a C2a . . . . -179.9(3) Mn1 N1a C1a C6a . . . . -.2(5) C5a N1a C1a C2a . . . . 1.5(6) C5a N1a C1a C6a . . . . -178.7(4) Mn1 N1a C5a C4a . . . . 179.5(4) Mn1 N1a C5a C9a . . . . -1.4(5) C1a N1a C5a C4a . . . . -2.0(6) C1a N1a C5a C9a . . . . 177.2(4) Mn1 N2a C6a N3a . . . . -175.0(3) Mn1 N2a C6a C1a . . . . 3.1(5) C7a N2a C6a N3a . . . . .2(5) C7a N2a C6a C1a . . . . 178.3(4) Mn1 N2a C7a C8a . . . . 172.7(4) C6a N2a C7a C8a . . . . -.8(5) C8a N3a C6a N2a . . . . .4(5) C8a N3a C6a C1a . . . . -177.6(5) H03a N3a C6a N2a . . . . 175(4) H03a N3a C6a C1a . . . . -3(4) C6a N3a C8a C7a . . . . -.9(5) H03a N3a C8a C7a . . . . -175(4) Mn1 N4a C9a N5a . . . . -177.5(3) Mn1 N4a C9a C5a . . . . 4.1(5) C10a N4a C9a N5a . . . . -.3(5) C10a N4a C9a C5a . . . . -178.7(4) Mn1 N4a C10a C11a . . . . 175.9(4) C9a N4a C10a C11a . . . . -.2(5) C11a N5a C9a N4a . . . . .6(5) C11a N5a C9a C5a . . . . 178.9(5) H05a N5a C9a N4a . . . . -179(4) H05a N5a C9a C5a . . . . -1(5) C9a N5a C11a C10a . . . . -.7(6) H05a N5a C11a C10a . . . . 179(4) N1a C1a C2a C3a . . . . -.9(7) C6a C1a C2a C3a . . . . 179.4(5) N1a C1a C6a N2a . . . . -2.0(6) N1a C1a C6a N3a . . . . 175.8(4) C2a C1a C6a N2a . . . . 177.7(5) C2a C1a C6a N3a . . . . -4.5(7) C1a C2a C3a C4a . . . . .8(7) C2a C3a C4a C5a . . . . -1.2(7) C3a C4a C5a N1a . . . . 1.7(7) C3a C4a C5a C9a . . . . -177.2(5) N1a C5a C9a N4a . . . . -1.9(6) N1a C5a C9a N5a . . . . 180.0(4) C4a C5a C9a N4a . . . . 177.2(5) C4a C5a C9a N5a . . . . -1.0(7) N2a C7a C8a N3a . . . . 1.0(6) N4a C10a C11a N5a . . . . .6(6) Mn1 N1b C1b C2b . . . . -174.5(4) Mn1 N1b C1b C6b . . . . 5.0(5) C5b N1b C1b C2b . . . . -.1(7) C5b N1b C1b C6b . . . . 179.4(4) Mn1 N1b C5b C4b . . . . 175.0(4) Mn1 N1b C5b C9b . . . . -3.5(6) C1b N1b C5b C4b . . . . .7(7) C1b N1b C5b C9b . . . . -177.8(4) Mn1 N2b C6b N3b . . . . -177.2(4) Mn1 N2b C6b C1b . . . . -.3(6) C7b N2b C6b N3b . . . . -.5(6) C7b N2b C6b C1b . . . . 176.3(5) Mn1 N2b C7b C8b . . . . 175.7(4) C6b N2b C7b C8b . . . . .4(6) C8b N3b C6b N2b . . . . .5(6) C8b N3b C6b C1b . . . . -176.2(5) H03b N3b C6b N2b . . . . -178(5) H03b N3b C6b C1b . . . . 6(5) C6b N3b C8b C7b . . . . -.2(6) H03b N3b C8b C7b . . . . 178(5) Mn1 N4b C9b N5b . . . . -172.1(4) Mn1 N4b C9b C5b . . . . 3.5(6) C10b N4b C9b N5b . . . . .2(6) C10b N4b C9b C5b . . . . 175.8(5) Mn1 N4b C10b C11b . . . . 168.9(4) C9b N4b C10b C11b . . . . -.3(6) C11b N5b C9b N4b . . . . .0(6) C11b N5b C9b C5b . . . . -175.2(5) H05b N5b C9b N4b . . . . -179(5) H05b N5b C9b C5b . . . . 5(5) C9b N5b C11b C10b . . . . -.2(6) H05b N5b C11b C10b . . . . 179(5) N1b C1b C2b C3b . . . . -.9(7) C6b C1b C2b C3b . . . . 179.7(5) N1b C1b C6b N2b . . . . -3.0(7) N1b C1b C6b N3b . . . . 173.3(5) C2b C1b C6b N2b . . . . 176.4(5) C2b C1b C6b N3b . . . . -7.3(8) C1b C2b C3b C4b . . . . 1.3(8) C2b C3b C4b C5b . . . . -.8(8) C3b C4b C5b N1b . . . . -.2(7) C3b C4b C5b C9b . . . . 178.0(5) N1b C5b C9b N4b . . . . -.2(7) N1b C5b C9b N5b . . . . 174.7(5) C4b C5b C9b N4b . . . . -178.6(5) C4b C5b C9b N5b . . . . -3.7(9) N2b C7b C8b N3b . . . . -.1(6) N4b C10b C11b N5b . . . . .3(7) Mn2 N1c C1c C2c . . . . 179.1(4) Mn2 N1c C1c C9c . . . . .2(5) C5c N1c C1c C2c . . . . -1.8(6) C5c N1c C1c C9c . . . . 179.3(4) Mn2 N1c C5c C4c . . . . -179.1(4) Mn2 N1c C5c C6c . . . . 2.0(5) C1c N1c C5c C4c . . . . 1.8(6) C1c N1c C5c C6c . . . . -177.2(4) Mn2 N2c C6c N3c . . . . 175.2(3) Mn2 N2c C6c C5c . . . . -7.3(5) C7c N2c C6c N3c . . . . .8(5) C7c N2c C6c C5c . . . . 178.2(4) Mn2 N2c C7c C8c . . . . -173.4(4) C6c N2c C7c C8c . . . . -1.0(6) C8c N3c C6c N2c . . . . -.3(5) C8c N3c C6c C5c . . . . -177.5(5) H03c N3c C6c N2c . . . . 168(5) H03c N3c C6c C5c . . . . -9(5) C6c N3c C8c C7c . . . . -.3(6) H03c N3c C8c C7c . . . . -168(5) Mn2 N4c C9c N5c . . . . 174.6(3) Mn2 N4c C9c C1c . . . . -2.5(5) C10c N4c C9c N5c . . . . -1.0(5) C10c N4c C9c C1c . . . . -178.0(4) Mn2 N4c C10c C11c . . . . -172.5(4) C9c N4c C10c C11c . . . . 1.4(5) C11c N5c C9c N4c . . . . .2(5) C11c N5c C9c C1c . . . . 177.0(4) H05c N5c C9c N4c . . . . -176(4) H05c N5c C9c C1c . . . . 0(4) C9c N5c C11c C10c . . . . .7(5) H05c N5c C11c C10c . . . . 177(4) N1c C1c C2c C3c . . . . 1.5(7) C9c C1c C2c C3c . . . . -179.8(4) N1c C1c C9c N4c . . . . 1.6(6) N1c C1c C9c N5c . . . . -174.9(4) C2c C1c C9c N4c . . . . -177.3(4) C2c C1c C9c N5c . . . . 6.3(7) C1c C2c C3c C4c . . . . -1.2(7) C2c C3c C4c C5c . . . . 1.2(7) C3c C4c C5c N1c . . . . -1.5(7) C3c C4c C5c C6c . . . . 177.3(5) N1c C5c C6c N2c . . . . 3.7(6) N1c C5c C6c N3c . . . . -179.3(4) C4c C5c C6c N2c . . . . -175.1(5) C4c C5c C6c N3c . . . . 1.9(8) N2c C7c C8c N3c . . . . .8(6) N4c C10c C11c N5c . . . . -1.3(5) Mn2 N1d C1d C2d . . . . 174.4(4) Mn2 N1d C1d C9d . . . . -5.0(5) C5d N1d C1d C2d . . . . .8(7) C5d N1d C1d C9d . . . . -178.5(4) Mn2 N1d C5d C4d . . . . -174.6(4) Mn2 N1d C5d C6d . . . . 4.6(5) C1d N1d C5d C4d . . . . -1.2(7) C1d N1d C5d C6d . . . . 178.0(4) Mn2 N2d C6d N3d . . . . 171.8(4) Mn2 N2d C6d C5d . . . . -5.7(6) C7d N2d C6d N3d . . . . -.4(6) C7d N2d C6d C5d . . . . -177.9(5) Mn2 N2d C7d C8d . . . . -169.0(4) C6d N2d C7d C8d . . . . .4(6) C8d N3d C6d N2d . . . . .2(6) C8d N3d C6d C5d . . . . 177.5(5) H03d N3d C6d N2d . . . . -173(5) H03d N3d C6d C5d . . . . 5(6) C6d N3d C8d C7d . . . . .1(6) H03d N3d C8d C7d . . . . 172(6) Mn2 N4d C9d N5d . . . . 178.2(3) Mn2 N4d C9d C1d . . . . -.5(6) C10d N4d C9d N5d . . . . .4(6) C10d N4d C9d C1d . . . . -178.3(5) Mn2 N4d C10d C11d . . . . -176.8(4) C9d N4d C10d C11d . . . . .0(6) C11d N5d C9d N4d . . . . -.7(6) C11d N5d C9d C1d . . . . 177.9(5) H05d N5d C9d N4d . . . . 173(5) H05d N5d C9d C1d . . . . -8(6) C9d N5d C11d C10d . . . . .7(6) H05d N5d C11d C10d . . . . -173(5) N1d C1d C2d C3d . . . . .0(7) C9d C1d C2d C3d . . . . 179.3(5) N1d C1d C9d N4d . . . . 3.6(7) N1d C1d C9d N5d . . . . -174.8(5) C2d C1d C9d N4d . . . . -175.7(5) C2d C1d C9d N5d . . . . 5.8(8) C1d C2d C3d C4d . . . . -.5(7) C2d C3d C4d C5d . . . . .1(7) C3d C4d C5d N1d . . . . .7(7) C3d C4d C5d C6d . . . . -178.4(5) N1d C5d C6d N2d . . . . .9(7) N1d C5d C6d N3d . . . . -176.2(5) C4d C5d C6d N2d . . . . -179.9(5) C4d C5d C6d N3d . . . . 3.0(8) N2d C7d C8d N3d . . . . -.3(6) N4d C10d C11d N5d . . . . -.5(6) O1e S1e C1e F1e . . . . -59.8(4) O1e S1e C1e F2e . . . . -178.1(4) O1e S1e C1e F3e . . . . 59.8(4) O2e S1e C1e F1e . . . . 58.7(4) O2e S1e C1e F2e . . . . -59.6(4) O2e S1e C1e F3e . . . . 178.4(4) O3e S1e C1e F1e . . . . -179.5(4) O3e S1e C1e F2e . . . . 62.2(4) O3e S1e C1e F3e . . . . -59.9(4) O1f S1f C1f F1f . . . . -61.2(4) O1f S1f C1f F2f . . . . -179.9(4) O1f S1f C1f F3f . . . . 59.1(4) O2f S1f C1f F1f . . . . 57.1(4) O2f S1f C1f F2f . . . . -61.6(4) O2f S1f C1f F3f . . . . 177.5(4) O3f S1f C1f F1f . . . . 179.1(4) O3f S1f C1f F2f . . . . 60.3(4) O3f S1f C1f F3f . . . . -60.6(4) O1g S1g C1g F1g . . . . -61.9(4) O1g S1g C1g F2g . . . . 58.7(4) O1g S1g C1g F3g . . . . 178.4(4) O2g S1g C1g F1g . . . . 178.3(4) O2g S1g C1g F2g . . . . -61.1(4) O2g S1g C1g F3g . . . . 58.5(5) O3g S1g C1g F1g . . . . 58.5(4) O3g S1g C1g F2g . . . . 179.1(4) O3g S1g C1g F3g . . . . -61.3(5) O1h S1h C1h F1h . . . . -59.2(5) O1h S1h C1h F2h . . . . 60.6(5) O1h S1h C1h F3h . . . . 179.8(4) O2h S1h C1h F1h . . . . -179.0(4) O2h S1h C1h F2h . . . . -59.2(5) O2h S1h C1h F3h . . . . 60.1(5) O3h S1h C1h F1h . . . . 63.1(5) O3h S1h C1h F2h . . . . -177.1(4) O3h S1h C1h F3h . . . . -57.9(5) 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 H03a O3h . . . 0.90(4) 2.11(4) 2.951(4) 157(4) N5a H05a O3g . . 2_566 0.85(5) 2.06(5) 2.890(5) 165(4) N3b H03b O1f . . 2_565 0.86(4) 2.01(4) 2.868(4) 175(4) N5b H05b O3f . . 1_545 0.88(5) 2.42(5) 3.091(5) 134(4) N5b H05b O3h . . 1_545 0.88(5) 2.40(5) 3.065(5) 133(4) N3c H03c O2h . . 2_666 0.76(5) 2.14(5) 2.821(5) 150(5) N5c H05c O1g . . 1_645 0.84(4) 2.16(5) 2.958(4) 157(4) N3d H03d O1g . . 1_655 0.76(5) 2.37(4) 3.042(4) 147(4) N5d H05d O1e . . . 0.81(4) 2.07(4) 2.871(4) 170(5) #==END================================================================ data_GUP3 _database_code_depnum_ccdc_archive 'CCDC 222690' #--- Na2(PPN)[Co(1-2H)2]2(OH)(MeOH)(H2O)2 ------------------------------- _audit_creation_date 2000-11-23 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 2003-10-10 _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.0.1 _chemical_formula_moiety ; ((C11 H7 N5)2 Co)2 Na2 (C36 H30 N P2) (O H) (C H4 O) (H2 O)2 ; _chemical_formula_sum 'C81 H 67 Co2 N21 Na2 O4 P2 ' _chemical_formula_weight 1624.4 _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 12.6715(7) _cell_length_b 13.8632(6) _cell_length_c 21.7372(15) _cell_angle_alpha 90.00000 _cell_angle_beta 93.896(8) _cell_angle_gamma 90.00000 _cell_volume 3809.7(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_meas not_measured _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.75 _cell_measurement_theta_max 26. _cell_measurement_temperature 200 _exptl_absorpt_coefficient_mu .555 _exptl_crystal_description prism _exptl_crystal_size_max .21 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .15 _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 .8924 _exptl_absorpt_correction_T_max .9450 _diffrn_reflns_number 30394 _reflns_number_total 7439 _reflns_number_gt 4735 _reflns_threshold_expression 'refl observed if Fo > 3.99 \s(Fo)' _diffrn_reflns_theta_max 26. _diffrn_reflns_theta_full 26. _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .047 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .049 _refine_ls_wR_factor_ref .051 _refine_ls_goodness_of_fit_ref 1.66(1) _refine_ls_number_reflns 4949 _refine_ls_number_parameters 524 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.0002(Fo^2^)] _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .0009 _refine_diff_density_max .638 _refine_diff_density_min -.764 _refine_ls_extinction_method none _publ_section_exptl_refinement ; Hydrogen treatment: - The coordinates of the H atoms were calculated - The hydrogen atoms of H2O, MeOH and OH- were not observed nor calculated ; _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 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 P Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .09 .095 Na Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .03 .025 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 .99655(5) .54104(4) .75842(3) .0284(3) 1.00000 Uani N1a .9140(3) .6531(3) .76635(13) .0283(16) 1.00000 Uani N2a 1.0821(3) .6014(3) .82374(14) .0293(17) 1.00000 Uani N3a 1.1027(3) .7275(3) .88877(14) .0379(19) 1.00000 Uani N4a .8871(3) .5121(3) .69465(14) .0359(18) 1.00000 Uani N5a .7376(3) .5652(3) .64239(15) .051(3) 1.00000 Uani C1a .9493(4) .7205(3) .80775(16) .031(2) 1.00000 Uani C2a .8968(4) .8089(3) .81054(19) .043(3) 1.00000 Uani C3a .8092(4) .8237(4) .7696(3) .051(3) 1.00000 Uani C4a .7729(4) .7526(4) .7286(2) .050(3) 1.00000 Uani C5a .8280(4) .6659(3) .72767(17) .035(3) 1.00000 Uani C6a 1.0450(3) .6877(3) .84185(16) .029(2) 1.00000 Uani C7a 1.1704(4) .5850(3) .86140(18) .037(3) 1.00000 Uani C8a 1.1822(4) .6620(4) .90086(18) .043(3) 1.00000 Uani C9a .8116(4) .5824(4) .68787(17) .038(3) 1.00000 Uani C10a .8606(4) .4470(4) .65014(19) .051(3) 1.00000 Uani C11a .7694(5) .4790(4) .6186(2) .060(4) 1.00000 Uani N1b 1.0822(3) .4313(3) .74941(14) .0329(18) 1.00000 Uani N2b 1.0834(3) .5927(3) .69751(14) .0333(17) 1.00000 Uani N3b 1.2160(3) .5648(3) .63527(16) .048(3) 1.00000 Uani N4b .9339(3) .4595(3) .81758(13) .0322(17) 1.00000 Uani N5b .9430(3) .3178(3) .86917(15) .0393(19) 1.00000 Uani C1b 1.1580(4) .4357(3) .70855(17) .036(3) 1.00000 Uani C2b 1.2207(4) .3537(4) .7005(2) .045(3) 1.00000 Uani C3b 1.2045(4) .2726(4) .7352(3) .049(3) 1.00000 Uani C4b 1.1269(4) .2707(3) .7775(2) .044(3) 1.00000 Uani C5b 1.0653(4) .3523(3) .78383(18) .035(3) 1.00000 Uani C6b 1.1578(4) .5291(3) .67950(17) .035(3) 1.00000 Uani C7b 1.0943(4) .6724(3) .66254(19) .042(3) 1.00000 Uani C8b 1.1754(4) .6554(4) .62540(19) .049(3) 1.00000 Uani C9b .9806(4) .3715(3) .82415(18) .034(3) 1.00000 Uani C10b .8627(4) .4635(3) .86167(17) .038(3) 1.00000 Uani C11b .8681(4) .3767(4) .89283(19) .043(3) 1.00000 Uani P1c .96402(8) .08631(7) .53923(5) .0282(5) 1.00000 Uani N1c 1.00000 .00000 .50000 .040(3) 1.00000 Uani C1c .8263(4) .1163(3) .52259(16) .031(2) 1.00000 Uani C2c .7565(4) .0459(3) .50077(18) .038(3) 1.00000 Uani C3c .6494(4) .0662(4) .4896(2) .046(3) 1.00000 Uani C4c .6121(4) .1579(4) .50156(19) .048(3) 1.00000 Uani C5c .6810(4) .2289(4) .5226(3) .055(3) 1.00000 Uani C6c .7881(4) .2097(3) .5330(3) .048(3) 1.00000 Uani C7c 1.0394(3) .1928(3) .52443(17) .031(2) 1.00000 Uani C8c 1.0814(4) .2019(3) .46737(18) .042(3) 1.00000 Uani C9c 1.1353(5) .2853(4) .4535(2) .057(3) 1.00000 Uani C10c 1.1464(5) .3594(4) .4955(3) .057(3) 1.00000 Uani C11c 1.1041(4) .3510(4) .5520(3) .051(3) 1.00000 Uani C12c 1.0518(4) .2676(3) .56741(18) .040(3) 1.00000 Uani C13c .9821(3) .0581(3) .62029(17) .034(3) 1.00000 Uani C14c .9226(4) .1027(4) .66392(18) .044(3) 1.00000 Uani C15c .9433(5) .0802(4) .72636(19) .057(3) 1.00000 Uani C16c 1.0209(5) .0146(4) .7443(3) .062(4) 1.00000 Uani C17c 1.0768(4) -.0313(4) .7009(3) .058(3) 1.00000 Uani C18c 1.0585(4) -.0089(3) .63918(19) .043(3) 1.00000 Uani Na .56261(17) .64398(15) .59043(9) .0651(13) 1.00000 Uani O1d .5745(6) .6491(5) .4889(3) .050(4) .50000 Uani O1e .4299(6) .5513(6) .6064(4) .058(5) .50000 Uani C1e .3639(11) .5283(9) .5510(6) .081(9) .50000 Uani O1w .5288(7) .6147(5) .4579(4) .053(5) .50000 Uani O2w .4183(11) .5014(9) .5954(7) .114(5) .50000 Uiso H2a .92351 .86391 .84365 .05000 1.00000 Uiso H3a .76796 .89268 .76987 .05000 1.00000 Uiso H4a .70276 .76456 .69764 .05000 1.00000 Uiso H7a 1.22209 .52226 .86052 .05000 1.00000 Uiso H8a 1.24601 .67014 .93668 .05000 1.00000 Uiso H10a .90356 .38121 .64070 .05000 1.00000 Uiso H11a .72801 .44136 .58010 .05000 1.00000 Uiso H2b 1.28155 .35424 .66731 .05000 1.00000 Uiso H3b 1.25260 .20851 .72920 .05000 1.00000 Uiso H4b 1.11498 .20654 .80516 .05000 1.00000 Uiso H7b 1.04729 .73830 .66365 .05000 1.00000 Uiso H8b 1.20345 .70673 .59218 .05000 1.00000 Uiso H10b .81083 .52388 .87078 .05000 1.00000 Uiso H11b .82011 .35717 .93067 .05000 1.00000 Uiso H2c .78537 -.02615 .49210 .05000 1.00000 Uiso H3c .59525 .01046 .47166 .05000 1.00000 Uiso H4c .52797 .17375 .49403 .05000 1.00000 Uiso H5c .65125 .30105 .53109 .05000 1.00000 Uiso H6c .84222 .26680 .54917 .05000 1.00000 Uiso H8c 1.07241 .14390 .43368 .05000 1.00000 Uiso H9c 1.16858 .29209 .40878 .05000 1.00000 Uiso H10c 1.18929 .42458 .48437 .05000 1.00000 Uiso H11c 1.11121 .41046 .58457 .05000 1.00000 Uiso H12c 1.02062 .26062 .61279 .05000 1.00000 Uiso H14c .86107 .15447 .64958 .05000 1.00000 Uiso H15c .89768 .11471 .76092 .05000 1.00000 Uiso H16c 1.03816 -.00086 .79320 .05000 1.00000 Uiso H17c 1.13559 -.08556 .71524 .05000 1.00000 Uiso H18c 1.10488 -.04395 .60518 .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 .0267(3) .0289(3) .0299(3) -.0003(3) .0028(2) -.0043(3) N1a .0244(18) .0348(17) .0254(16) -.0008(14) .0008(13) .0002(14) N2a .0245(18) .0306(17) .0325(17) .0017(14) .0000(14) .0008(14) N3a .043(3) .0391(18) .0309(18) -.0118(17) -.0011(16) -.0041(15) N4a .038(3) .0418(19) .0283(17) -.0105(16) .0057(14) -.0037(14) N5a .049(3) .072(3) .0309(18) -.032(2) -.0097(16) .0119(18) C1a .033(3) .033(2) .027(2) .0022(18) .0058(17) .0022(17) C2a .052(3) .039(3) .041(3) .013(3) .008(3) -.0003(19) C3a .055(4) .051(3) .049(3) .026(3) .008(3) .008(3) C4a .033(3) .069(4) .047(3) .018(3) .004(2) .015(3) C5a .025(3) .051(3) .029(3) .0001(19) .0020(17) .0077(18) C6a .032(3) .0272(19) .028(2) -.0008(17) -.0001(16) .0013(15) C7a .027(3) .043(3) .040(3) .0006(19) -.0026(18) .0056(19) C8a .035(3) .054(3) .037(3) -.008(3) -.0088(19) .003(2) C9a .031(3) .055(3) .029(3) -.010(3) .0021(17) .0064(19) C10a .065(4) .051(3) .037(3) -.028(3) .011(3) -.012(2) C11a .075(4) .071(4) .032(3) -.047(3) -.012(3) .006(3) N1b .0311(19) .0317(18) .0361(18) -.0042(14) .0034(14) -.0076(14) N2b .0302(19) .0376(18) .0319(17) -.0025(15) .0004(14) -.0054(15) N3b .043(3) .061(3) .040(2) -.0078(19) .0126(16) -.0084(17) N4b .0298(18) .0355(17) .0309(17) -.0014(16) -.0009(13) -.0017(15) N5b .044(3) .0367(19) .0361(19) -.0104(17) -.0070(16) .0036(15) C1b .030(3) .043(3) .034(3) -.0011(18) -.0013(17) -.0126(17) C2b .037(3) .053(3) .043(3) .011(3) -.001(2) -.020(3) C3b .045(3) .048(3) .052(3) .019(3) -.011(3) -.015(3) C4b .047(3) .035(3) .049(3) .009(3) -.009(3) -.0071(19) C5b .033(3) .035(3) .036(3) .0021(19) -.0068(18) -.0055(18) C6b .030(3) .043(3) .033(2) -.0047(19) .0037(17) -.0099(18) C7b .043(3) .043(3) .039(3) -.008(3) .003(2) .0023(19) C8b .051(3) .056(3) .041(3) -.017(3) .011(3) .002(3) C9b .035(3) .032(3) .035(3) -.0048(18) -.0052(18) -.0033(17) C10b .032(3) .046(3) .035(3) -.004(2) .0066(17) -.004(2) C11b .041(3) .052(3) .037(3) -.010(3) .003(2) -.001(2) P1c .0257(6) .0305(5) .0286(5) .0024(5) .0025(4) -.0033(5) N1c .042(4) .035(3) .044(3) .004(3) .009(3) -.003(3) C1c .032(3) .035(3) .0262(19) .0043(18) .0014(16) -.0022(16) C2c .031(3) .044(3) .041(3) .003(2) .0045(17) -.007(2) C3c .033(3) .058(3) .048(3) -.002(3) .0027(19) -.012(3) C4c .034(3) .072(4) .038(3) .011(3) -.0055(19) -.003(3) C5c .041(3) .050(3) .072(4) .018(3) -.011(3) -.010(3) C6c .037(3) .040(3) .063(3) .004(2) -.011(3) -.015(3) C7c .028(3) .037(3) .028(2) .0011(18) -.0030(16) .0024(16) C8c .047(3) .045(3) .035(3) -.006(3) .0046(19) -.0021(19) C9c .075(4) .060(3) .038(3) -.020(3) .010(3) .008(3) C10c .071(4) .051(3) .047(3) -.021(3) -.005(3) .013(3) C11c .064(4) .041(3) .046(3) -.013(3) -.007(3) -.001(2) C12c .046(3) .040(3) .035(3) -.004(2) -.0027(19) -.0005(18) C13c .024(3) .041(3) .038(3) -.0041(18) .0044(17) .0002(17) C14c .037(3) .060(3) .035(3) .000(3) .0063(19) -.003(2) C15c .057(4) .085(4) .030(3) -.011(3) .011(3) -.000(3) C16c .064(4) .083(4) .039(3) -.026(3) -.002(3) .016(3) C17c .055(4) .063(3) .055(3) .001(3) -.013(3) .014(3) C18c .036(3) .048(3) .043(3) -.000(2) -.0032(19) .0042(19) Na .0661(14) .0689(13) .0600(12) .0051(11) .0020(10) .0009(10) O1d .069(5) .049(4) .031(4) .005(4) .003(4) -.007(3) O1e .059(5) .054(5) .061(5) -.022(4) .014(4) -.021(4) C1e .097(10) .068(8) .081(9) -.002(8) .028(8) -.005(7) O1w .080(6) .039(4) .042(4) .009(4) .010(4) .000(3) 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 Co N1a . . 1.888(3) Co N2a . . 1.919(3) Co N4a . . 1.935(4) Co N1b . . 1.887(4) Co N2b . . 1.917(4) Co N4b . . 1.923(4) N1a C1a . . 1.352(5) N1a C5a . . 1.342(5) N2a C6a . . 1.353(5) N2a C7a . . 1.361(5) N3a C6a . . 1.334(5) N3a C8a . . 1.369(6) N4a C9a . . 1.367(6) N4a C10a . . 1.350(6) N5a C9a . . 1.337(6) N5a C11a . . 1.372(7) C1a C2a . . 1.398(6) C1a C6a . . 1.451(6) C2a C3a . . 1.389(7) C3a C4a . . 1.388(7) C4a C5a . . 1.391(7) C5a C9a . . 1.451(6) C7a C8a . . 1.372(6) C10a C11a . . 1.377(7) N1b C1b . . 1.353(6) N1b C5b . . 1.352(5) N2b C6b . . 1.368(5) N2b C7b . . 1.353(6) N3b C6b . . 1.345(6) N3b C8b . . 1.368(6) N4b C9b . . 1.359(5) N4b C10b . . 1.361(5) N5b C9b . . 1.342(5) N5b C11b . . 1.378(6) C1b C2b . . 1.405(6) C1b C6b . . 1.440(6) C2b C3b . . 1.377(7) C3b C4b . . 1.391(7) C4b C5b . . 1.387(6) C5b C9b . . 1.455(6) C7b C8b . . 1.370(7) C10b C11b . . 1.380(6) P1c N1c . . 1.5555(10) P1c C1c . . 1.806(4) P1c C7c . . 1.800(4) P1c C13c . . 1.804(4) C1c C2c . . 1.379(6) C1c C6c . . 1.407(6) C2c C3c . . 1.391(6) C3c C4c . . 1.387(7) C4c C5c . . 1.373(7) C5c C6c . . 1.386(7) C7c C8c . . 1.388(6) C7c C12c . . 1.396(6) C8c C9c . . 1.386(7) C9c C10c . . 1.375(7) C10c C11c . . 1.378(7) C11c C12c . . 1.385(6) C13c C14c . . 1.395(6) C13c C18c . . 1.384(6) C14c C15c . . 1.400(6) C15c C16c . . 1.377(8) C16c C17c . . 1.374(8) C17c C18c . . 1.381(7) 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 N1a Co N2a . . . 82.08(13) N1a Co N4a . . . 82.03(14) N1a Co N1b . . . 178.26(14) N1a Co N2b . . . 95.91(14) N1a Co N4b . . . 99.57(14) N2a Co N4a . . . 164.11(14) N2a Co N1b . . . 97.38(13) N2a Co N2b . . . 91.49(13) N2a Co N4b . . . 89.97(13) N4a Co N1b . . . 98.50(14) N4a Co N2b . . . 89.99(14) N4a Co N4b . . . 92.82(13) N1b Co N2b . . . 82.44(14) N1b Co N4b . . . 82.07(14) N2b Co N4b . . . 164.50(14) Co N1a C1a . . . 118.0(3) Co N1a C5a . . . 118.9(3) C1a N1a C5a . . . 123.0(4) Co N2a C6a . . . 114.3(3) Co N2a C7a . . . 140.6(3) C6a N2a C7a . . . 105.1(3) C6a N3a C8a . . . 103.3(4) Co N4a C9a . . . 113.1(3) Co N4a C10a . . . 141.6(4) C9a N4a C10a . . . 105.1(4) C9a N5a C11a . . . 103.0(4) N1a C1a C2a . . . 119.8(4) N1a C1a C6a . . . 110.5(4) C2a C1a C6a . . . 129.5(4) C1a C2a C3a . . . 117.6(4) C2a C3a C4a . . . 121.5(5) C3a C4a C5a . . . 118.6(4) N1a C5a C4a . . . 119.5(4) N1a C5a C9a . . . 110.2(4) C4a C5a C9a . . . 130.2(4) N2a C6a N3a . . . 113.9(4) N2a C6a C1a . . . 115.0(4) N3a C6a C1a . . . 131.0(4) N2a C7a C8a . . . 107.2(4) N3a C8a C7a . . . 110.5(4) N4a C9a N5a . . . 113.8(4) N4a C9a C5a . . . 115.7(4) N5a C9a C5a . . . 130.4(4) N4a C10a C11a . . . 107.5(4) N5a C11a C10a . . . 110.6(4) Co N1b C1b . . . 118.1(3) Co N1b C5b . . . 118.8(3) C1b N1b C5b . . . 123.1(4) Co N2b C6b . . . 113.3(3) Co N2b C7b . . . 141.1(3) C6b N2b C7b . . . 105.5(4) C6b N3b C8b . . . 103.4(4) Co N4b C9b . . . 113.7(3) Co N4b C10b . . . 140.4(3) C9b N4b C10b . . . 105.5(4) C9b N5b C11b . . . 103.4(4) N1b C1b C2b . . . 118.5(4) N1b C1b C6b . . . 110.4(4) C2b C1b C6b . . . 131.1(4) C1b C2b C3b . . . 119.1(5) C2b C3b C4b . . . 121.1(5) C3b C4b C5b . . . 118.5(4) N1b C5b C4b . . . 119.6(4) N1b C5b C9b . . . 109.6(4) C4b C5b C9b . . . 130.7(4) N2b C6b N3b . . . 112.9(4) N2b C6b C1b . . . 115.8(4) N3b C6b C1b . . . 131.3(4) N2b C7b C8b . . . 107.4(4) N3b C8b C7b . . . 110.8(4) N4b C9b N5b . . . 113.6(4) N4b C9b C5b . . . 115.8(4) N5b C9b C5b . . . 130.5(4) N4b C10b C11b . . . 107.3(4) N5b C11b C10b . . . 110.2(4) N1c P1c C1c . . . 112.47(13) N1c P1c C7c . . . 110.75(14) N1c P1c C13c . . . 110.26(14) C1c P1c C7c . . . 107.03(18) C1c P1c C13c . . . 107.59(18) C7c P1c C13c . . . 108.59(17) P1c N1c P1c . . 3_756 180.0000 P1c C1c C2c . . . 119.6(3) P1c C1c C6c . . . 121.2(3) C2c C1c C6c . . . 119.1(4) C1c C2c C3c . . . 120.8(4) C2c C3c C4c . . . 119.6(4) C3c C4c C5c . . . 120.2(5) C4c C5c C6c . . . 120.6(5) C1c C6c C5c . . . 119.7(4) P1c C7c C8c . . . 118.3(3) P1c C7c C12c . . . 121.7(3) C8c C7c C12c . . . 119.9(4) C7c C8c C9c . . . 119.6(4) C8c C9c C10c . . . 120.5(5) C9c C10c C11c . . . 120.0(5) C10c C11c C12c . . . 120.5(4) C7c C12c C11c . . . 119.4(4) P1c C13c C14c . . . 121.9(3) P1c C13c C18c . . . 118.4(3) C14c C13c C18c . . . 119.7(4) C13c C14c C15c . . . 119.1(5) C14c C15c C16c . . . 120.4(5) C15c C16c C17c . . . 120.2(5) C16c C17c C18c . . . 120.2(5) C13c C18c C17c . . . 120.5(4) 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 C5a N1a C1a C2a . . . . -1.4(6) C5a N1a C1a C6a . . . . -178.4(4) C1a N1a C5a C4a . . . . 1.4(6) C1a N1a C5a C9a . . . . 178.5(4) C7a N2a C6a N3a . . . . -.5(5) C7a N2a C6a C1a . . . . -179.8(4) C6a N2a C7a C8a . . . . .4(5) C8a N3a C6a N2a . . . . .4(5) C8a N3a C6a C1a . . . . 179.6(4) C6a N3a C8a C7a . . . . -.1(5) C10a N4a C9a N5a . . . . 1.0(5) C10a N4a C9a C5a . . . . -174.9(4) C9a N4a C10a C11a . . . . -.9(5) C11a N5a C9a N4a . . . . -.7(5) C11a N5a C9a C5a . . . . 174.5(5) C9a N5a C11a C10a . . . . .1(6) N1a C1a C2a C3a . . . . -.2(6) C6a C1a C2a C3a . . . . 176.2(5) N1a C1a C6a N2a . . . . 3.4(5) N1a C1a C6a N3a . . . . -175.7(4) C2a C1a C6a N2a . . . . -173.2(4) C2a C1a C6a N3a . . . . 7.6(7) C1a C2a C3a C4a . . . . 1.8(7) C2a C3a C4a C5a . . . . -1.8(7) C3a C4a C5a N1a . . . . .2(7) C3a C4a C5a C9a . . . . -176.2(5) N1a C5a C9a N4a . . . . -3.5(5) N1a C5a C9a N5a . . . . -178.7(5) C4a C5a C9a N4a . . . . 173.2(5) C4a C5a C9a N5a . . . . -2.0(8) N2a C7a C8a N3a . . . . -.2(5) N4a C10a C11a N5a . . . . .5(6) C5b N1b C1b C2b . . . . 1.4(6) C5b N1b C1b C6b . . . . -179.3(4) C1b N1b C5b C4b . . . . -.5(6) C1b N1b C5b C9b . . . . 178.5(4) C7b N2b C6b N3b . . . . .6(5) C7b N2b C6b C1b . . . . -177.0(4) C6b N2b C7b C8b . . . . -1.0(5) C8b N3b C6b N2b . . . . -.0(5) C8b N3b C6b C1b . . . . 177.1(4) C6b N3b C8b C7b . . . . -.6(5) C10b N4b C9b N5b . . . . .9(5) C10b N4b C9b C5b . . . . -176.5(4) C9b N4b C10b C11b . . . . -.8(5) C11b N5b C9b N4b . . . . -.5(5) C11b N5b C9b C5b . . . . 176.4(5) C9b N5b C11b C10b . . . . -.0(4) N1b C1b C2b C3b . . . . -1.3(6) C6b C1b C2b C3b . . . . 179.6(5) N1b C1b C6b N2b . . . . -.6(5) N1b C1b C6b N3b . . . . -177.7(4) C2b C1b C6b N2b . . . . 178.6(4) C2b C1b C6b N3b . . . . 1.6(8) C1b C2b C3b C4b . . . . .3(7) C2b C3b C4b C5b . . . . .5(7) C3b C4b C5b N1b . . . . -.5(6) C3b C4b C5b C9b . . . . -179.2(5) N1b C5b C9b N4b . . . . 2.8(5) N1b C5b C9b N5b . . . . -174.1(4) C4b C5b C9b N4b . . . . -178.4(4) C4b C5b C9b N5b . . . . 4.7(8) N2b C7b C8b N3b . . . . 1.0(5) N4b C10b C11b N5b . . . . .5(5) N1c P1c C1c C2c . . . . 26.8(4) N1c P1c C1c C6c . . . . -154.8(3) C7c P1c C1c C2c . . . . 148.7(4) C7c P1c C1c C6c . . . . -33.0(4) C13c P1c C1c C2c . . . . -94.8(4) C13c P1c C1c C6c . . . . 83.5(4) N1c P1c C7c C8c . . . . 27.2(4) N1c P1c C7c C12c . . . . -156.1(3) C1c P1c C7c C8c . . . . -95.8(4) C1c P1c C7c C12c . . . . 81.0(4) C13c P1c C7c C8c . . . . 148.4(4) C13c P1c C7c C12c . . . . -34.9(4) N1c P1c C13c C14c . . . . -155.2(4) N1c P1c C13c C18c . . . . 25.8(4) C1c P1c C13c C14c . . . . -32.2(4) C1c P1c C13c C18c . . . . 148.7(4) C7c P1c C13c C14c . . . . 83.3(4) C7c P1c C13c C18c . . . . -95.7(4) P1c C1c C2c C3c . . . . 177.8(4) C6c C1c C2c C3c . . . . -.6(6) P1c C1c C6c C5c . . . . -176.8(4) C2c C1c C6c C5c . . . . 1.5(7) C1c C2c C3c C4c . . . . -1.2(7) C2c C3c C4c C5c . . . . 1.9(7) C3c C4c C5c C6c . . . . -.9(8) C4c C5c C6c C1c . . . . -.8(8) P1c C7c C8c C9c . . . . 176.8(4) C12c C7c C8c C9c . . . . -.0(7) P1c C7c C12c C11c . . . . -175.4(4) C8c C7c C12c C11c . . . . 1.3(7) C7c C8c C9c C10c . . . . -.7(8) C8c C9c C10c C11c . . . . .2(8) C9c C10c C11c C12c . . . . 1.1(8) C10c C11c C12c C7c . . . . -1.9(7) P1c C13c C14c C15c . . . . -177.6(4) C18c C13c C14c C15c . . . . 1.5(7) P1c C13c C18c C17c . . . . 178.5(4) C14c C13c C18c C17c . . . . -.6(7) C13c C14c C15c C16c . . . . -.3(8) C14c C15c C16c C17c . . . . -1.7(9) C15c C16c C17c C18c . . . . 2.6(8) C16c C17c C18c C13c . . . . -1.5(8) #==END====================================================================