Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email alan.Williams@chiam.unige.ch _publ_contact_author_name 'Prof Alan Williams' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30 quai Ernest Ansermet Geneva CH 1211 SWITZERLAND ; _publ_contact_author_phone '+41 22 702 64 25' _publ_section_title ; Crystal structures of dicarboxy-2,2'-bipyridyl complexes: the role of hydrogen bonding and stacking interactions ; loop_ _publ_author_name _publ_author_address C.J.Matthews ; Department of Chemistry and Physics Nottingham Trent University Clifton Lane Nottingham UK NG11 8NS ; M.R.J.Elsegood ; Chemistry Department Loughborough University Loughborough Leicester UK LE11 3TU ; G.Bernardinelli ; Laboratoiry of X-ray Crystallography University de Geneva 24, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; 'William Clegg' ; University Chemistry Laboratories School of Natural Sciences University of Newcastle Newcastle upon Tyne UK NE1 7RU ; ; A.F.Williams ; ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; data_MATH _database_code_depnum_ccdc_archive 'CCDC 209930' _chemical_name_common ;Rhodium(iii) tris(2,2'-bipirydine-5,5'-dicarboxylic acid) hexa-aquo ; #--------------------------------------------- Compound [Rh(1H)3].6H2O --- _audit_creation_date 1997-03-21 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 2003-03-04 _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.0.1 #------------------------------------------------------------------------ _chemical_name_systematic ; Rhodium(III) tris(2,2'-bipirydine-5,5'-dicarboxylic acid) hexa-aquo ; _chemical_formula_moiety 'Rh, (C12 H7 N2 O4)3, (H2 O)6' _chemical_formula_sum 'C36 H33 N6 O18 Rh' _chemical_formula_weight 940.6 _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 13.596(3) _cell_length_b 13.6180(10) _cell_length_c 13.661(2) _cell_angle_alpha 70.430(10) _cell_angle_beta 63.340(10) _cell_angle_gamma 75.530(10) _cell_volume 2114.9(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_meas not_measured _diffrn_radiation_type 'Cu K/a' _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 27 _cell_measurement_theta_min 17 _cell_measurement_theta_max 30 _cell_measurement_temperature 220 _exptl_absorpt_coefficient_mu 3.978 _exptl_crystal_description prism _exptl_crystal_size_max .22 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .046 _exptl_crystal_colour yellow _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 .52847 _exptl_absorpt_correction_T_max .841959 _diffrn_reflns_number 4661 _reflns_number_total 4355 _reflns_number_gt 3839 _reflns_threshold_expression 'refl observed if Fo > 3.99 \s(Fo)' _diffrn_reflns_theta_max 49.99 _diffrn_reflns_theta_full 49.99 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .018 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 2 _diffrn_standards_interval_time 45 _diffrn_standards_decay_% 1.5 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .056 _refine_ls_wR_factor_ref .071 _refine_ls_goodness_of_fit_ref 1.913 _refine_ls_number_reflns 3839 _refine_ls_number_parameters 623 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.0005(Fo^2^)] _refine_ls_hydrogen_treatment refxyz _refine_ls_shift/su_max .0022 _refine_diff_density_max 1.406 _refine_diff_density_min -.578 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 7475(747) _refine_ls_abs_structure_details none _refine_special_details ; Hydrogen treatment: Hydrogen atom of the bipyridines were observed and refined with a fixed value of Uiso. Hydrogen atoms of the carboxyl groups and water molecules were not observed. ; _computing_data_collection Stoe_Stadi-4 _computing_cell_refinement xtal_LATCON _computing_data_reduction xtal_REFCAL_LSABS__SORTRF _computing_structure_solution Multan_87 _computing_structure_refinement xtal_CRYLSQ _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 O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .047 .032 N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .029 .018 Rh Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 -.077 3.605 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 Rh .29596(5) .25004(5) .77491(5) .0204(8) 1.00000 Uani O1a .1681(6) .5988(5) .9375(6) .056(9) 1.00000 Uani O2a .0280(7) .5681(6) 1.1085(7) .069(11) 1.00000 Uani O3a .2192(9) -.1361(7) .7784(8) .097(14) 1.00000 Uani O4a .1341(7) -.2207(6) .9588(7) .070(11) 1.00000 Uani N1a .2031(5) .2994(5) .9180(6) .023(8) 1.00000 Uani N2a .2094(6) .1241(5) .8724(6) .025(9) 1.00000 Uani C1a .1935(8) .3960(7) .9295(8) .029(11) 1.00000 Uani C2a .1192(8) .4269(7) 1.0254(8) .041(12) 1.00000 Uani C3a .0561(10) .3524(8) 1.1169(9) .054(14) 1.00000 Uani C4a .0662(9) .2539(8) 1.1070(9) .050(13) 1.00000 Uani C5a .1377(8) .2288(7) 1.0067(7) .031(11) 1.00000 Uani C6a .1493(7) .1268(7) .9836(8) .029(11) 1.00000 Uani C7a .1026(8) .0399(7) 1.0651(8) .034(12) 1.00000 Uani C8a .1133(8) -.0494(7) 1.0347(9) .036(12) 1.00000 Uani C9a .1682(7) -.0497(7) .9202(8) .033(12) 1.00000 Uani C10a .2176(7) .0378(7) .8434(8) .027(11) 1.00000 Uani C11a .1037(10) .5383(8) 1.0279(9) .053(14) 1.00000 Uani C12a .1772(9) -.1437(8) .8806(11) .049(14) 1.00000 Uani O1b .4485(6) .1534(6) 1.1157(6) .062(10) 1.00000 Uani O2b .6155(6) .0583(6) 1.0625(6) .060(10) 1.00000 Uani O3b .3081(8) .1638(8) .3937(8) .098(15) 1.00000 Uani O4b .4826(8) .1301(8) .2855(7) .082(12) 1.00000 Uani N1b .4242(6) .1737(5) .8194(6) .024(9) 1.00000 Uani N2b .3935(6) .1896(5) .6386(6) .024(8) 1.00000 Uani C1b .4330(8) .1659(8) .9158(8) .033(12) 1.00000 Uani C2b .5290(8) .1230(8) .9331(8) .038(12) 1.00000 Uani C3b .6180(9) .0885(10) .8481(9) .053(15) 1.00000 Uani C4b .6119(9) .0961(9) .7482(9) .049(14) 1.00000 Uani C5b .5122(7) .1381(7) .7367(7) .029(11) 1.00000 Uani C6b .4957(7) .1466(7) .6349(7) .025(10) 1.00000 Uani C7b .5745(8) .1146(8) .5420(8) .037(12) 1.00000 Uani C8b .5476(9) .1197(8) .4532(9) .041(13) 1.00000 Uani C9b .4416(8) .1556(7) .4620(8) .034(12) 1.00000 Uani C10b .3669(8) .1917(7) .5539(8) .029(11) 1.00000 Uani C11b .5350(9) .1100(9) 1.0450(8) .046(14) 1.00000 Uani C12b .4067(10) .1531(9) .3720(9) .050(15) 1.00000 Uani O1c .6718(5) .4096(5) .6680(6) .052(9) 1.00000 Uani O2c .6538(6) .5847(6) .5994(7) .060(10) 1.00000 Uani O3c -.1000(6) .2573(7) .7322(8) .074(12) 1.00000 Uani O4c -.1466(6) .4249(6) .6531(7) .058(10) 1.00000 Uani N1c .3713(5) .3824(5) .6919(6) .023(8) 1.00000 Uani N2c .1844(6) .3426(5) .7105(6) .024(8) 1.00000 Uani C1c .4690(7) .3963(7) .6873(8) .030(11) 1.00000 Uani C2c .5090(7) .4921(7) .6432(7) .032(11) 1.00000 Uani C3c .4434(8) .5782(8) .6051(9) .037(12) 1.00000 Uani C4c .3445(8) .5658(8) .6065(8) .035(12) 1.00000 Uani C5c .3098(7) .4672(7) .6499(7) .027(11) 1.00000 Uani C6c .2076(7) .4427(7) .6570(7) .025(10) 1.00000 Uani C7c .1377(8) .5145(8) .6133(9) .039(13) 1.00000 Uani C8c .0433(8) .4851(8) .6228(9) .038(12) 1.00000 Uani C9c .0194(7) .3853(7) .6754(7) .029(11) 1.00000 Uani C10c .0918(7) .3139(8) .7195(8) .028(11) 1.00000 Uani C11c .6202(8) .4989(9) .6364(9) .044(13) 1.00000 Uani C12c -.0831(8) .3495(9) .6889(9) .046(14) 1.00000 Uani O1w .1833(11) -.2267(11) .6377(13) .16(3) 1.00000 Uani O2w .1555(10) .3315(9) .4263(14) .16(3) 1.00000 Uani O3w .1328(13) .0822(12) .6407(13) .18(3) 1.00000 Uani O4w .3994(13) .466(3) .9404(15) .31(5) 1.00000 Uani O5w .415(3) .637(3) .888(4) .21(7) .50000 Uani O6w -.0147(19) .7696(15) .6092(18) .11(4) .50000 Uani O7w -.1051(19) .1075(16) .6529(19) .13(4) .50000 Uani O8w .195(3) .111(3) .261(4) .25(9) .50000 Uani H1a .233(8) .443(8) .865(9) .05000 1.00000 Uiso H3a .030(8) .376(7) 1.189(9) .05000 1.00000 Uiso H4a .033(8) .202(8) 1.167(9) .05000 1.00000 Uiso H7a .062(8) .037(7) 1.144(9) .05000 1.00000 Uiso H8a .092(8) -.104(8) 1.077(9) .05000 1.00000 Uiso H10a .256(8) .025(8) .772(9) .05000 1.00000 Uiso H1b .381(9) .182(8) .964(9) .05000 1.00000 Uiso H3b .674(8) .047(8) .861(8) .05000 1.00000 Uiso H4b .668(8) .065(7) .690(9) .05000 1.00000 Uiso H7b .642(8) .087(8) .532(9) .05000 1.00000 Uiso H8b .605(8) .100(7) .391(9) .05000 1.00000 Uiso H10b .300(8) .221(8) .553(8) .05000 1.00000 Uiso H1c .509(8) .338(8) .720(8) .05000 1.00000 Uiso H3c .475(8) .638(8) .565(8) .05000 1.00000 Uiso H4c .296(8) .624(8) .585(8) .05000 1.00000 Uiso H7c .162(9) .569(8) .581(9) .05000 1.00000 Uiso H8c .005(8) .530(8) .593(9) .05000 1.00000 Uiso H10c .080(8) .240(8) .759(8) .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 Rh .0199(5) .0215(5) .0203(5) -.0025(3) -.0088(3) -.0048(3) O1a .069(5) .032(4) .044(5) -.022(4) .008(4) -.013(4) O2a .094(7) .047(5) .048(5) -.015(5) -.004(5) -.023(4) O3a .143(9) .068(6) .062(7) -.054(6) .015(6) -.042(5) O4a .099(7) .029(5) .074(6) -.021(5) -.013(5) -.023(5) N1a .022(4) .025(5) .024(5) -.005(4) -.008(4) -.009(4) N2a .026(4) .021(5) .026(5) -.004(4) -.011(4) -.003(4) C1a .031(6) .026(6) .026(6) -.007(5) -.008(5) -.005(5) C2a .050(7) .031(6) .037(7) -.008(5) -.006(6) -.017(6) C3a .075(8) .039(7) .029(6) -.020(6) .008(6) -.015(6) C4a .068(8) .030(7) .031(7) -.020(6) .007(6) -.009(5) C5a .039(6) .026(6) .026(6) -.012(5) -.009(5) -.004(5) C6a .029(6) .027(6) .031(6) -.005(5) -.012(5) -.008(5) C7a .043(6) .025(6) .029(6) -.010(5) -.010(5) -.004(5) C8a .040(6) .019(6) .041(7) -.003(5) -.015(6) -.000(5) C9a .026(6) .024(6) .051(7) -.003(5) -.014(5) -.015(5) C10a .032(6) .023(6) .032(6) .000(5) -.017(5) -.013(5) C11a .074(8) .038(7) .038(7) -.011(6) -.004(7) -.023(6) C12a .053(7) .030(7) .062(9) -.013(6) -.012(7) -.017(7) O1b .054(5) .101(6) .040(5) .027(5) -.026(4) -.045(5) O2b .051(5) .095(6) .049(5) .010(5) -.039(4) -.023(5) O3b .079(7) .163(10) .099(8) .032(7) -.066(6) -.084(7) O4b .085(6) .135(8) .042(5) .014(6) -.037(5) -.044(6) N1b .027(5) .024(4) .020(5) .001(4) -.012(4) -.006(4) N2b .027(5) .024(4) .024(5) -.003(4) -.014(4) -.004(4) C1b .035(7) .037(6) .030(7) -.000(5) -.013(5) -.016(5) C2b .032(6) .055(7) .034(6) .009(5) -.022(6) -.019(5) C3b .039(7) .083(9) .043(7) .024(6) -.028(6) -.030(7) C4b .033(7) .082(9) .039(7) .015(6) -.017(6) -.033(6) C5b .033(6) .029(6) .022(6) .001(5) -.012(5) -.008(5) C6b .025(6) .029(5) .022(6) -.001(4) -.009(5) -.009(4) C7b .031(6) .050(7) .034(6) .008(5) -.019(6) -.017(5) C8b .042(7) .047(7) .029(6) .004(5) -.013(6) -.014(5) C9b .041(7) .037(6) .027(6) .002(5) -.016(5) -.015(5) C10b .036(6) .026(6) .027(6) -.002(5) -.018(6) -.004(5) C11b .051(8) .065(8) .031(6) -.007(6) -.028(6) -.009(6) C12b .057(8) .062(8) .039(7) .011(6) -.032(7) -.018(6) O1c .035(4) .041(5) .083(6) -.007(4) -.040(4) .005(4) O2c .043(5) .042(5) .097(6) -.018(4) -.036(5) -.000(5) O3c .063(6) .054(6) .115(7) -.027(5) -.063(6) .017(5) O4c .038(5) .058(5) .082(6) -.015(4) -.042(5) .011(5) N1c .018(4) .031(5) .022(4) -.007(4) -.008(4) -.007(4) N2c .020(5) .031(5) .020(4) -.006(4) -.007(4) -.005(4) C1c .025(6) .033(6) .027(6) -.004(5) -.009(5) -.003(5) C2c .026(6) .039(6) .027(6) -.010(5) -.007(5) -.007(5) C3c .035(6) .027(6) .045(7) -.015(5) -.016(6) .004(5) C4c .030(6) .028(6) .047(7) -.007(5) -.022(5) .003(5) C5c .022(5) .029(6) .031(6) .005(5) -.016(5) -.007(5) C6c .023(5) .024(6) .026(5) -.005(5) -.008(5) -.005(5) C7c .036(7) .035(6) .041(7) -.010(6) -.019(6) .006(5) C8c .026(6) .044(7) .042(7) -.000(5) -.022(5) .001(6) C9c .025(6) .035(6) .026(5) -.007(5) -.010(5) -.004(5) C10c .022(6) .035(6) .027(6) -.004(5) -.008(5) -.008(5) C11c .040(7) .050(8) .051(7) -.024(6) -.020(6) -.008(6) C12c .037(7) .060(8) .045(7) -.010(6) -.025(6) -.004(6) O1w .116(10) .156(12) .197(14) -.000(9) -.038(10) -.083(11) O2w .102(9) .108(9) .267(18) .001(7) -.069(11) -.053(10) O3w .203(15) .195(14) .178(14) -.076(12) -.115(13) -.001(11) O4w .119(12) .56(4) .200(17) -.178(18) -.095(13) .11(2) O5w .16(3) .14(3) .43(6) .03(2) -.18(4) -.13(4) O6w .16(2) .085(14) .104(16) .015(13) -.079(15) -.020(12) O7w .16(2) .107(16) .109(17) -.068(15) -.007(15) -.045(13) O8w .19(3) .24(4) .46(6) .16(3) -.24(4) -.24(4) 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 Rh N1a . . 2.027(7) Rh N2a . . 2.043(7) Rh N1b . . 2.028(8) Rh N2b . . 2.042(7) Rh N1c . . 2.023(7) Rh N2c . . 2.040(8) O1a C11a . . 1.295(11) O2a C11a . . 1.229(13) O3a C12a . . 1.227(16) O4a C12a . . 1.257(12) N1a C1a . . 1.344(13) N1a C5a . . 1.366(10) N2a C6a . . 1.373(11) N2a C10a . . 1.325(14) C1a C2a . . 1.373(13) C2a C3a . . 1.397(12) C2a C11a . . 1.488(15) C3a C4a . . 1.360(17) C4a C5a . . 1.375(14) C5a C6a . . 1.480(14) C6a C7a . . 1.380(11) C7a C8a . . 1.366(16) C8a C9a . . 1.399(15) C9a C10a . . 1.380(11) C9a C12a . . 1.506(18) O1b C11b . . 1.296(12) O2b C11b . . 1.220(14) O3b C12b . . 1.217(18) O4b C12b . . 1.245(13) N1b C1b . . 1.342(15) N1b C5b . . 1.345(10) N2b C6b . . 1.351(12) N2b C10b . . 1.348(15) C1b C2b . . 1.380(15) C2b C3b . . 1.362(13) C2b C11b . . 1.515(18) C3b C4b . . 1.372(19) C4b C5b . . 1.390(15) C5b C6b . . 1.468(16) C6b C7b . . 1.366(12) C7b C8b . . 1.393(19) C8b C9b . . 1.365(15) C9b C10b . . 1.367(13) C9b C12b . . 1.51(2) O1c C11c . . 1.285(12) O2c C11c . . 1.223(14) O3c C12c . . 1.226(14) O4c C12c . . 1.281(13) N1c C1c . . 1.359(14) N1c C5c . . 1.366(11) N2c C6c . . 1.354(11) N2c C10c . . 1.351(14) C1c C2c . . 1.376(14) C2c C3c . . 1.388(13) C2c C11c . . 1.497(16) C3c C4c . . 1.388(17) C4c C5c . . 1.382(13) C5c C6c . . 1.463(15) C6c C7c . . 1.367(14) C7c C8c . . 1.377(18) C8c C9c . . 1.352(13) C9c C10c . . 1.393(13) C9c C12c . . 1.504(17) 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 Rh N2a . . . 80.7(3) N1a Rh N1b . . . 96.3(3) N1a Rh N2b . . . 175.5(3) N1a Rh N1c . . . 93.2(3) N1a Rh N2c . . . 87.4(3) N2a Rh N1b . . . 89.9(3) N2a Rh N2b . . . 96.5(3) N2a Rh N1c . . . 173.9(3) N2a Rh N2c . . . 98.9(3) N1b Rh N2b . . . 80.0(4) N1b Rh N1c . . . 91.5(3) N1b Rh N2c . . . 171.0(3) N2b Rh N1c . . . 89.6(3) N2b Rh N2c . . . 96.6(3) N1c Rh N2c . . . 80.1(3) Rh N1a C1a . . . 126.3(5) Rh N1a C5a . . . 115.1(7) C1a N1a C5a . . . 118.3(7) Rh N2a C6a . . . 113.4(7) Rh N2a C10a . . . 127.1(5) C6a N2a C10a . . . 118.8(7) N1a C1a C2a . . . 122.7(8) C1a C2a C3a . . . 118.1(10) C1a C2a C11a . . . 120.0(8) C3a C2a C11a . . . 121.8(9) C2a C3a C4a . . . 119.7(10) C3a C4a C5a . . . 119.7(9) N1a C5a C4a . . . 121.3(9) N1a C5a C6a . . . 114.3(8) C4a C5a C6a . . . 124.4(8) N2a C6a C5a . . . 115.1(7) N2a C6a C7a . . . 120.9(9) C5a C6a C7a . . . 124.0(9) C6a C7a C8a . . . 119.8(9) C7a C8a C9a . . . 119.2(8) C8a C9a C10a . . . 118.2(10) C8a C9a C12a . . . 121.7(8) C10a C9a C12a . . . 120.0(9) N2a C10a C9a . . . 122.8(9) O1a C11a O2a . . . 124.9(10) O1a C11a C2a . . . 115.3(9) O2a C11a C2a . . . 119.6(9) O3a C12a O4a . . . 127.1(13) O3a C12a C9a . . . 118.4(9) O4a C12a C9a . . . 114.3(11) Rh N1b C1b . . . 126.6(6) Rh N1b C5b . . . 114.2(7) C1b N1b C5b . . . 118.8(8) Rh N2b C6b . . . 114.1(7) Rh N2b C10b . . . 126.8(6) C6b N2b C10b . . . 119.0(8) N1b C1b C2b . . . 122.5(8) C1b C2b C3b . . . 118.3(12) C1b C2b C11b . . . 121.4(9) C3b C2b C11b . . . 120.3(10) C2b C3b C4b . . . 120.7(11) C3b C4b C5b . . . 118.5(9) N1b C5b C4b . . . 121.4(10) N1b C5b C6b . . . 115.8(9) C4b C5b C6b . . . 122.9(8) N2b C6b C5b . . . 114.7(7) N2b C6b C7b . . . 120.7(10) C5b C6b C7b . . . 124.7(9) C6b C7b C8b . . . 119.9(10) C7b C8b C9b . . . 118.8(9) C8b C9b C10b . . . 119.3(12) C8b C9b C12b . . . 120.2(9) C10b C9b C12b . . . 120.5(10) N2b C10b C9b . . . 122.1(10) O1b C11b O2b . . . 126.3(12) O1b C11b C2b . . . 114.5(10) O2b C11b C2b . . . 119.2(9) O3b C12b O4b . . . 125.3(16) O3b C12b C9b . . . 118.3(10) O4b C12b C9b . . . 116.0(12) Rh N1c C1c . . . 125.7(6) Rh N1c C5c . . . 115.1(6) C1c N1c C5c . . . 118.6(8) Rh N2c C6c . . . 114.1(7) Rh N2c C10c . . . 126.5(6) C6c N2c C10c . . . 119.4(8) N1c C1c C2c . . . 123.3(8) C1c C2c C3c . . . 117.4(10) C1c C2c C11c . . . 119.5(8) C3c C2c C11c . . . 123.2(9) C2c C3c C4c . . . 120.5(10) C3c C4c C5c . . . 119.4(9) N1c C5c C4c . . . 120.8(10) N1c C5c C6c . . . 114.0(8) C4c C5c C6c . . . 125.2(8) N2c C6c C5c . . . 116.0(8) N2c C6c C7c . . . 120.5(10) C5c C6c C7c . . . 123.5(8) C6c C7c C8c . . . 120.0(9) C7c C8c C9c . . . 120.2(10) C8c C9c C10c . . . 118.6(10) C8c C9c C12c . . . 122.2(9) C10c C9c C12c . . . 119.2(9) N2c C10c C9c . . . 121.4(9) O1c C11c O2c . . . 127.1(11) O1c C11c C2c . . . 114.0(10) O2c C11c C2c . . . 118.9(9) O3c C12c O4c . . . 126.6(12) O3c C12c C9c . . . 120.8(10) O4c C12c C9c . . . 112.6(10) 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 Rh N1a C1a . . . . -170.2(9) N2a Rh N1a C5a . . . . 3.8(7) N1b Rh N1a C1a . . . . 101.0(9) N1b Rh N1a C5a . . . . -85.0(7) N1c Rh N1a C1a . . . . 9.1(9) N1c Rh N1a C5a . . . . -176.9(7) N2c Rh N1a C1a . . . . -70.8(9) N2c Rh N1a C5a . . . . 103.3(7) N1a Rh N2a C6a . . . . -9.3(7) N1a Rh N2a C10a . . . . -179.7(9) N1b Rh N2a C6a . . . . 87.1(7) N1b Rh N2a C10a . . . . -83.3(9) N2b Rh N2a C6a . . . . 167.0(7) N2b Rh N2a C10a . . . . -3.3(9) N2c Rh N2a C6a . . . . -95.2(7) N2c Rh N2a C10a . . . . 94.4(9) N1a Rh N1b C1b . . . . -.4(8) N1a Rh N1b C5b . . . . -172.9(7) N2a Rh N1b C1b . . . . -81.0(8) N2a Rh N1b C5b . . . . 106.4(7) N2b Rh N1b C1b . . . . -177.7(8) N2b Rh N1b C5b . . . . 9.8(6) N1c Rh N1b C1b . . . . 93.0(8) N1c Rh N1b C5b . . . . -79.5(7) N2a Rh N2b C6b . . . . -98.4(6) N2a Rh N2b C10b . . . . 83.6(7) N1b Rh N2b C6b . . . . -9.7(6) N1b Rh N2b C10b . . . . 172.4(7) N1c Rh N2b C6b . . . . 81.9(6) N1c Rh N2b C10b . . . . -96.1(7) N2c Rh N2b C6b . . . . 161.8(6) N2c Rh N2b C10b . . . . -16.1(7) N1a Rh N1c C1c . . . . 92.8(8) N1a Rh N1c C5c . . . . -78.7(7) N1b Rh N1c C1c . . . . -3.6(8) N1b Rh N1c C5c . . . . -175.1(7) N2b Rh N1c C1c . . . . -83.6(8) N2b Rh N1c C5c . . . . 104.9(7) N2c Rh N1c C1c . . . . 179.6(8) N2c Rh N1c C5c . . . . 8.2(7) N1a Rh N2c C6c . . . . 88.1(6) N1a Rh N2c C10c . . . . -89.9(8) N2a Rh N2c C6c . . . . 168.3(6) N2a Rh N2c C10c . . . . -9.7(8) N2b Rh N2c C6c . . . . -94.0(6) N2b Rh N2c C10c . . . . 88.0(8) N1c Rh N2c C6c . . . . -5.6(6) N1c Rh N2c C10c . . . . 176.4(8) Rh N1a C1a C2a . . . . 172.3(9) C5a N1a C1a C2a . . . . -1.5(16) Rh N1a C5a C4a . . . . -176.7(9) Rh N1a C5a C6a . . . . 2.0(11) C1a N1a C5a C4a . . . . -2.2(16) C1a N1a C5a C6a . . . . 176.5(9) Rh N2a C6a C5a . . . . 13.1(11) Rh N2a C6a C7a . . . . -168.1(9) C10a N2a C6a C5a . . . . -175.7(9) C10a N2a C6a C7a . . . . 3.1(15) Rh N2a C10a C9a . . . . 169.9(8) C6a N2a C10a C9a . . . . .1(15) N1a C1a C2a C3a . . . . 4.0(18) N1a C1a C2a C11a . . . . -173.1(11) C1a C2a C3a C4a . . . . -3(2) C11a C2a C3a C4a . . . . 174.2(13) C1a C2a C11a O1a . . . . -3.3(19) C1a C2a C11a O2a . . . . 171.3(13) C3a C2a C11a O1a . . . . 179.7(13) C3a C2a C11a O2a . . . . -6(3) C2a C3a C4a C5a . . . . 0(2) C3a C4a C5a N1a . . . . 3.2(19) C3a C4a C5a C6a . . . . -175.3(12) N1a C5a C6a N2a . . . . -10.1(13) N1a C5a C6a C7a . . . . 171.2(10) C4a C5a C6a N2a . . . . 168.5(11) C4a C5a C6a C7a . . . . -10.2(18) N2a C6a C7a C8a . . . . -1.9(16) C5a C6a C7a C8a . . . . 176.8(11) C6a C7a C8a C9a . . . . -2.4(17) C7a C8a C9a C10a . . . . 5.4(16) C7a C8a C9a C12a . . . . -176.6(11) C8a C9a C10a N2a . . . . -4.3(16) C12a C9a C10a N2a . . . . 177.6(10) C8a C9a C12a O3a . . . . 174.7(12) C8a C9a C12a O4a . . . . -1.7(16) C10a C9a C12a O3a . . . . -7.3(17) C10a C9a C12a O4a . . . . 176.3(11) Rh N1b C1b C2b . . . . -172.1(8) C5b N1b C1b C2b . . . . .1(14) Rh N1b C5b C4b . . . . 171.6(8) Rh N1b C5b C6b . . . . -8.3(10) C1b N1b C5b C4b . . . . -1.5(13) C1b N1b C5b C6b . . . . 178.5(8) Rh N2b C6b C5b . . . . 8.1(9) Rh N2b C6b C7b . . . . -172.0(7) C10b N2b C6b C5b . . . . -173.8(8) C10b N2b C6b C7b . . . . 6.1(12) Rh N2b C10b C9b . . . . 175.1(7) C6b N2b C10b C9b . . . . -2.8(12) N1b C1b C2b C3b . . . . .7(16) N1b C1b C2b C11b . . . . -176.8(9) C1b C2b C3b C4b . . . . -.3(17) C11b C2b C3b C4b . . . . 177.3(11) C1b C2b C11b O1b . . . . -7.9(15) C1b C2b C11b O2b . . . . 169.5(11) C3b C2b C11b O1b . . . . 174.6(11) C3b C2b C11b O2b . . . . -7.9(17) C2b C3b C4b C5b . . . . -1.1(18) C3b C4b C5b N1b . . . . 2.0(16) C3b C4b C5b C6b . . . . -178.0(10) N1b C5b C6b N2b . . . . .1(11) N1b C5b C6b C7b . . . . -179.8(9) C4b C5b C6b N2b . . . . -179.9(9) C4b C5b C6b C7b . . . . .2(15) N2b C6b C7b C8b . . . . -4.4(14) C5b C6b C7b C8b . . . . 175.5(9) C6b C7b C8b C9b . . . . -.8(15) C7b C8b C9b C10b . . . . 4.0(14) C7b C8b C9b C12b . . . . -174.6(9) C8b C9b C10b N2b . . . . -2.3(14) C12b C9b C10b N2b . . . . 176.2(8) C8b C9b C12b O3b . . . . 164.3(10) C8b C9b C12b O4b . . . . -9.1(14) C10b C9b C12b O3b . . . . -14.2(15) C10b C9b C12b O4b . . . . 172.4(9) Rh N1c C1c C2c . . . . -170.6(7) C5c N1c C1c C2c . . . . .6(14) Rh N1c C5c C4c . . . . 170.3(7) Rh N1c C5c C6c . . . . -9.2(10) C1c N1c C5c C4c . . . . -1.8(13) C1c N1c C5c C6c . . . . 178.7(8) Rh N2c C6c C5c . . . . 2.4(10) Rh N2c C6c C7c . . . . -177.6(8) C10c N2c C6c C5c . . . . -179.5(8) C10c N2c C6c C7c . . . . .5(13) Rh N2c C10c C9c . . . . 177.6(7) C6c N2c C10c C9c . . . . -.3(13) N1c C1c C2c C3c . . . . 2.0(15) N1c C1c C2c C11c . . . . -177.0(9) C1c C2c C3c C4c . . . . -3.4(15) C11c C2c C3c C4c . . . . 175.5(10) C1c C2c C11c O1c . . . . 3.8(14) C1c C2c C11c O2c . . . . -178.4(10) C3c C2c C11c O1c . . . . -175.1(10) C3c C2c C11c O2c . . . . 2.7(16) C2c C3c C4c C5c . . . . 2.3(15) C3c C4c C5c N1c . . . . .4(15) C3c C4c C5c C6c . . . . 179.8(10) N1c C5c C6c N2c . . . . 4.4(12) N1c C5c C6c C7c . . . . -175.6(9) C4c C5c C6c N2c . . . . -175.0(9) C4c C5c C6c C7c . . . . 4.9(15) N2c C6c C7c C8c . . . . -.4(15) C5c C6c C7c C8c . . . . 179.6(10) C6c C7c C8c C9c . . . . .1(16) C7c C8c C9c C10c . . . . .2(15) C7c C8c C9c C12c . . . . 179.4(10) C8c C9c C10c N2c . . . . -.1(14) C12c C9c C10c N2c . . . . -179.3(9) C8c C9c C12c O3c . . . . 176.5(11) C8c C9c C12c O4c . . . . -4.7(15) C10c C9c C12c O3c . . . . -4.3(16) C10c C9c C12c O4c . . . . 174.5(9) #==END================================================================== data_cjm2a _database_code_depnum_ccdc_archive 'CCDC 209931' _chemical_name_common ;Ruthenium(iii) tris(2,2'-bipyridine-5,5'-dicarboxylic acid) 2.6-hydrate ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C36 H22 N6 O12 Ru,2.5 H2 O' _chemical_formula_sum 'C36 H27 N6 O14.50 Ru' _chemical_formula_weight 876.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 14.605(2) _cell_length_b 12.503(2) _cell_length_c 19.601(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.147(4) _cell_angle_gamma 90.00 _cell_volume 3551.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 3170 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 28.00 _exptl_crystal_description brick _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.489 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9139 _diffrn_reflns_av_R_equivalents 0.1152 _diffrn_reflns_av_sigmaI/netI 0.1353 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3128 _reflns_number_gt 2073 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00044(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3128 _refine_ls_number_parameters 271 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.2500 0.22038(5) 0.5000 0.0158(2) Uani 1 2 d S . . N1 N 0.3367(3) 0.0920(3) 0.48883(18) 0.0159(9) Uani 1 1 d . . . N2 N 0.3246(2) 0.2118(3) 0.59660(17) 0.0172(9) Uani 1 1 d . . . C1 C 0.3321(3) 0.0296(3) 0.4321(2) 0.0175(11) Uani 1 1 d . . . H1 H 0.3050 0.0579 0.3894 0.021 Uiso 1 1 calc R . . C2 C 0.3655(3) -0.0740(4) 0.4342(2) 0.0207(12) Uani 1 1 d . . . C3 C 0.4071(3) -0.1147(4) 0.4962(2) 0.0250(12) Uani 1 1 d . . . H3 H 0.4289 -0.1864 0.4988 0.030 Uiso 1 1 calc R . . C4 C 0.4167(3) -0.0512(4) 0.5538(2) 0.0241(12) Uani 1 1 d . . . H4 H 0.4466 -0.0775 0.5963 0.029 Uiso 1 1 calc R . . C5 C 0.3814(3) 0.0530(4) 0.5488(2) 0.0191(11) Uani 1 1 d . . . C6 C 0.3816(3) 0.1263(4) 0.6083(2) 0.0180(11) Uani 1 1 d . . . C7 C 0.4385(3) 0.1128(4) 0.6695(2) 0.0295(13) Uani 1 1 d . . . H7 H 0.4783 0.0526 0.6759 0.035 Uiso 1 1 calc R . . C8 C 0.4369(4) 0.1875(4) 0.7211(3) 0.0340(14) Uani 1 1 d . . . H8 H 0.4761 0.1800 0.7633 0.041 Uiso 1 1 calc R . . C9 C 0.3775(3) 0.2732(4) 0.7105(2) 0.0239(11) Uani 1 1 d . . . C10 C 0.3231(3) 0.2819(4) 0.6481(2) 0.0190(10) Uani 1 1 d . . . H10 H 0.2821 0.3410 0.6412 0.023 Uiso 1 1 calc R . . C11 C 0.3495(3) -0.1427(4) 0.3700(3) 0.0255(12) Uani 1 1 d . . . C12 C 0.3749(4) 0.3571(4) 0.7644(3) 0.0281(13) Uani 1 1 d . . . O1 O 0.3217(2) -0.0988(3) 0.31389(16) 0.0344(10) Uani 1 1 d . . . O2 O 0.3613(3) -0.2410(3) 0.37833(18) 0.0435(11) Uani 1 1 d . . . O3 O 0.3030(2) 0.4196(3) 0.75306(17) 0.0314(9) Uani 1 1 d . . . H3O H 0.3148 0.4786 0.7727 0.047 Uiso 1 1 calc R . . O4 O 0.4346(3) 0.3657(3) 0.81279(19) 0.0580(13) Uani 1 1 d . . . N3 N 0.3287(3) 0.3475(3) 0.47488(18) 0.0164(9) Uani 1 1 d . . . C13 C 0.2923(3) 0.4466(4) 0.4828(2) 0.0183(12) Uani 1 1 d . . . C14 C 0.3301(4) 0.5386(4) 0.4593(3) 0.0265(13) Uani 1 1 d . . . H14 H 0.3022 0.6061 0.4648 0.032 Uiso 1 1 calc R . . C15 C 0.4093(4) 0.5309(4) 0.4276(3) 0.0330(14) Uani 1 1 d . . . H15 H 0.4361 0.5931 0.4105 0.040 Uiso 1 1 calc R . . C16 C 0.4492(3) 0.4309(4) 0.4209(2) 0.0223(12) Uani 1 1 d . . . C17 C 0.4063(3) 0.3420(4) 0.4444(2) 0.0193(12) Uani 1 1 d . . . H17 H 0.4328 0.2737 0.4388 0.023 Uiso 1 1 calc R . . C18 C 0.5351(4) 0.4237(4) 0.3880(3) 0.0317(14) Uani 1 1 d . . . O5 O 0.5712(2) 0.3282(3) 0.39039(18) 0.0331(9) Uani 1 1 d . . . H5O H 0.6150 0.3267 0.3663 0.050 Uiso 1 1 calc R . . O6 O 0.5668(3) 0.5001(3) 0.3619(3) 0.0655(14) Uani 1 1 d . . . O1W O 0.6957(3) 0.3095(5) 0.3136(2) 0.0734(16) Uani 1 1 d D . . H1WA H 0.685(5) 0.345(5) 0.277(2) 0.110 Uiso 1 1 d D . . H1WB H 0.7503(19) 0.304(6) 0.333(4) 0.110 Uiso 1 1 d D . . O2W O 0.8893(16) 0.3990(18) 0.2505(12) 0.114(8) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0216(3) 0.0148(3) 0.0091(3) 0.000 -0.0055(2) 0.000 N1 0.020(2) 0.017(2) 0.009(2) 0.0021(17) -0.0033(19) -0.0032(18) N2 0.022(2) 0.018(2) 0.011(2) 0.0007(19) -0.0002(17) 0.001(2) C1 0.017(3) 0.023(3) 0.012(3) 0.002(2) -0.001(2) -0.002(2) C2 0.029(3) 0.017(3) 0.015(3) -0.002(2) -0.004(2) -0.002(2) C3 0.030(3) 0.019(3) 0.024(3) 0.002(2) -0.005(3) 0.003(2) C4 0.027(3) 0.025(3) 0.018(3) 0.003(2) -0.007(2) 0.003(2) C5 0.020(3) 0.023(3) 0.013(3) -0.001(2) -0.002(2) -0.002(2) C6 0.018(3) 0.024(3) 0.012(3) -0.001(2) -0.001(2) -0.003(2) C7 0.033(3) 0.036(3) 0.017(3) -0.003(2) -0.008(3) 0.014(3) C8 0.040(3) 0.041(4) 0.017(3) -0.003(2) -0.011(3) 0.006(3) C9 0.029(3) 0.027(3) 0.015(2) -0.005(2) -0.002(2) 0.000(3) C10 0.022(3) 0.017(2) 0.017(2) 0.001(2) -0.003(2) 0.000(3) C11 0.028(3) 0.020(3) 0.027(3) -0.003(2) -0.005(3) 0.001(2) C12 0.034(3) 0.030(3) 0.020(3) -0.004(2) 0.003(3) 0.001(3) O1 0.060(3) 0.024(2) 0.0162(19) -0.0003(16) -0.0096(19) 0.0059(18) O2 0.071(3) 0.021(2) 0.034(2) -0.0018(16) -0.011(2) 0.0104(19) O3 0.043(2) 0.028(2) 0.021(2) -0.0116(16) -0.0062(19) 0.0017(19) O4 0.066(3) 0.066(3) 0.032(2) -0.027(2) -0.032(2) 0.020(2) N3 0.017(2) 0.020(2) 0.009(2) -0.0002(17) -0.0099(19) -0.0024(19) C13 0.022(3) 0.016(3) 0.015(3) -0.001(2) -0.006(2) -0.001(2) C14 0.033(3) 0.018(3) 0.026(3) 0.002(2) -0.007(3) -0.001(3) C15 0.042(4) 0.023(3) 0.034(3) 0.006(3) 0.003(3) -0.009(3) C16 0.020(3) 0.030(3) 0.016(3) 0.005(2) -0.004(2) -0.004(3) C17 0.021(3) 0.023(3) 0.012(3) 0.005(2) -0.006(2) 0.002(2) C18 0.037(4) 0.030(3) 0.027(3) 0.001(3) -0.003(3) 0.001(3) O5 0.028(2) 0.042(2) 0.031(2) 0.0017(17) 0.0079(18) 0.0020(18) O6 0.062(3) 0.042(3) 0.104(4) 0.025(3) 0.052(3) -0.002(2) O1W 0.063(3) 0.121(4) 0.041(3) 0.034(3) 0.024(3) 0.048(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.073(4) . ? Ru1 N1 2.073(4) 2_556 ? Ru1 N2 2.066(3) . ? Ru1 N2 2.066(3) 2_556 ? Ru1 N3 2.057(4) . ? Ru1 N3 2.057(4) 2_556 ? N1 C1 1.353(5) . ? N1 C5 1.362(5) . ? N2 C6 1.357(5) . ? N2 C10 1.340(5) . ? C1 C2 1.382(6) . ? C2 C3 1.386(6) . ? C2 C11 1.518(6) . ? C3 C4 1.374(6) . ? C4 C5 1.399(6) . ? C5 C6 1.482(6) . ? C6 C7 1.382(6) . ? C7 C8 1.380(6) . ? C8 C9 1.378(6) . ? C9 C10 1.378(6) . ? C9 C12 1.493(6) . ? C11 O1 1.251(5) . ? C11 O2 1.249(5) . ? C12 O3 1.305(6) . ? C12 O4 1.209(6) . ? N3 C13 1.365(5) . ? N3 C17 1.346(5) . ? C13 C13 1.480(9) 2_556 ? C13 C14 1.379(6) . ? C14 C15 1.383(7) . ? C15 C16 1.393(6) . ? C16 C17 1.383(6) . ? C16 C18 1.483(7) . ? C18 O5 1.303(6) . ? C18 O6 1.203(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N1 78.5(2) . 2_556 ? N1 Ru1 N2 78.29(14) . . ? N1 Ru1 N2 78.29(14) 2_556 2_556 ? N1 Ru1 N2 97.02(14) 2_556 . ? N1 Ru1 N2 97.02(14) . 2_556 ? N1 Ru1 N3 101.89(14) . . ? N1 Ru1 N3 172.13(14) 2_556 . ? N1 Ru1 N3 101.89(14) 2_556 2_556 ? N1 Ru1 N3 172.13(14) . 2_556 ? N2 Ru1 N2 174.0(2) . 2_556 ? N2 Ru1 N3 90.74(14) . . ? N2 Ru1 N3 93.88(14) 2_556 . ? N2 Ru1 N3 90.74(14) 2_556 2_556 ? N2 Ru1 N3 93.88(14) . 2_556 ? N3 Ru1 N3 78.8(2) . 2_556 ? Ru1 N1 C1 124.4(3) . . ? Ru1 N1 C5 114.8(3) . . ? C1 N1 C5 118.2(4) . . ? Ru1 N2 C6 116.0(3) . . ? Ru1 N2 C10 126.9(3) . . ? C6 N2 C10 117.1(4) . . ? N1 C1 C2 122.4(4) . . ? C1 C2 C3 119.0(4) . . ? C1 C2 C11 119.2(4) . . ? C3 C2 C11 121.6(4) . . ? C2 C3 C4 119.8(4) . . ? C3 C4 C5 118.8(4) . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 114.3(4) . . ? C4 C5 C6 123.8(4) . . ? N2 C6 C5 114.4(4) . . ? N2 C6 C7 122.2(4) . . ? C5 C6 C7 123.3(4) . . ? C6 C7 C8 119.4(5) . . ? C7 C8 C9 118.9(5) . . ? C8 C9 C10 118.6(4) . . ? C8 C9 C12 120.7(4) . . ? C10 C9 C12 120.7(5) . . ? N2 C10 C9 123.7(4) . . ? C2 C11 O1 118.7(4) . . ? C2 C11 O2 116.3(4) . . ? O1 C11 O2 124.9(5) . . ? C9 C12 O3 113.0(4) . . ? C9 C12 O4 122.5(5) . . ? O3 C12 O4 124.5(5) . . ? Ru1 N3 C13 115.9(3) . . ? Ru1 N3 C17 126.4(3) . . ? C13 N3 C17 117.3(4) . . ? N3 C13 C13 114.3(3) . 2_556 ? N3 C13 C14 122.8(4) . . ? C13 C13 C14 122.9(3) 2_556 . ? C13 C14 C15 118.9(5) . . ? C14 C15 C16 119.2(5) . . ? C15 C16 C17 118.5(5) . . ? C15 C16 C18 118.8(5) . . ? C17 C16 C18 122.7(5) . . ? N3 C17 C16 123.3(5) . . ? C16 C18 O5 113.6(5) . . ? C16 C18 O6 121.9(5) . . ? O5 C18 O6 124.5(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3O O1 0.84 1.70 2.536(4) 171.5 8 O5 H5O O1W 0.84 1.68 2.512(6) 172.6 . O1W H1WA O1 0.839(10) 1.91(2) 2.732(5) 167(7) 4 O1W H1WB O2 0.840(10) 1.92(3) 2.726(6) 160(8) 6_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.603 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.115 #==END================================================================== data_cjm1 _database_code_depnum_ccdc_archive 'CCDC 209932' _chemical_name_common ;Cobalt(iii) tris(2,2'-bipyridine-4,4'-dicarboxylic acid) hexahydrate ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C36 H21 Co N6 O12,6 H2 O' _chemical_formula_sum 'C36 H33 Co N6 O18' _chemical_formula_weight 896.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8979(8) _cell_length_b 18.2150(14) _cell_length_c 20.7718(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.149(2) _cell_angle_gamma 90.00 _cell_volume 3697.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 8539 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 28.11 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22868 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.53 _reflns_number_total 8434 _reflns_number_gt 5808 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.4659P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8434 _refine_ls_number_parameters 590 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.48665(3) 0.253513(15) 0.054050(13) 0.01096(8) Uani 1 1 d . . . N1 N 0.36097(17) 0.17118(9) 0.04105(8) 0.0125(4) Uani 1 1 d . . . N2 N 0.57642(17) 0.20188(9) -0.00929(8) 0.0127(4) Uani 1 1 d . . . C1 C 0.2553(2) 0.15754(12) 0.07266(10) 0.0162(5) Uani 1 1 d . . . H1 H 0.2286 0.1943 0.1006 0.019 Uiso 1 1 calc R . . C2 C 0.1844(2) 0.09228(11) 0.06610(10) 0.0159(5) Uani 1 1 d . . . H2 H 0.1108 0.0845 0.0896 0.019 Uiso 1 1 calc R . . C3 C 0.2205(2) 0.03786(11) 0.02522(10) 0.0146(5) Uani 1 1 d . . . C4 C 0.3257(2) 0.05307(11) -0.00996(10) 0.0152(5) Uani 1 1 d . . . H4 H 0.3501 0.0182 -0.0401 0.018 Uiso 1 1 calc R . . C5 C 0.3943(2) 0.11933(11) -0.00075(10) 0.0140(5) Uani 1 1 d . . . C6 C 0.5083(2) 0.14104(11) -0.03407(10) 0.0131(4) Uani 1 1 d . . . C7 C 0.5393(2) 0.10609(12) -0.08875(10) 0.0155(5) Uani 1 1 d . . . H7 H 0.4926 0.0625 -0.1045 0.019 Uiso 1 1 calc R . . C8 C 0.6401(2) 0.13573(12) -0.12030(10) 0.0159(5) Uani 1 1 d . . . C9 C 0.7104(2) 0.19734(12) -0.09475(10) 0.0171(5) Uani 1 1 d . . . H9 H 0.7799 0.2182 -0.1157 0.020 Uiso 1 1 calc R . . C10 C 0.6783(2) 0.22834(12) -0.03825(10) 0.0150(5) Uani 1 1 d . . . H10 H 0.7296 0.2693 -0.0195 0.018 Uiso 1 1 calc R . . C11 C 0.1507(2) -0.03742(12) 0.01942(10) 0.0151(5) Uani 1 1 d . . . O1 O 0.07582(15) -0.05185(8) 0.06120(7) 0.0187(3) Uani 1 1 d . . . O2 O 0.17513(15) -0.07818(8) -0.02573(7) 0.0200(4) Uani 1 1 d . . . C12 C 0.6669(2) 0.10188(13) -0.18335(11) 0.0204(5) Uani 1 1 d . . . O3 O 0.62501(19) 0.03532(9) -0.19023(8) 0.0336(4) Uani 1 1 d . . . H3 H 0.6321 0.0206 -0.2279 0.050 Uiso 1 1 calc R . . O4 O 0.71956(18) 0.13786(10) -0.22244(8) 0.0325(4) Uani 1 1 d . . . N3 N 0.40329(17) 0.30841(9) -0.02174(8) 0.0124(4) Uani 1 1 d . . . N4 N 0.61692(17) 0.33418(9) 0.06396(8) 0.0118(4) Uani 1 1 d . . . C13 C 0.2953(2) 0.28703(12) -0.06537(10) 0.0167(5) Uani 1 1 d . . . H13 H 0.2438 0.2455 -0.0560 0.020 Uiso 1 1 calc R . . C14 C 0.2571(2) 0.32407(12) -0.12376(11) 0.0189(5) Uani 1 1 d . . . H14 H 0.1805 0.3081 -0.1540 0.023 Uiso 1 1 calc R . . C15 C 0.3319(2) 0.38455(12) -0.13746(10) 0.0176(5) Uani 1 1 d . . . C16 C 0.4421(2) 0.40693(12) -0.09205(10) 0.0164(5) Uani 1 1 d . . . H16 H 0.4937 0.4489 -0.1003 0.020 Uiso 1 1 calc R . . C17 C 0.4766(2) 0.36801(11) -0.03481(10) 0.0133(4) Uani 1 1 d . . . C18 C 0.5953(2) 0.38413(11) 0.01482(10) 0.0136(4) Uani 1 1 d . . . C19 C 0.6832(2) 0.44287(11) 0.01206(10) 0.0160(5) Uani 1 1 d . . . H19 H 0.6668 0.4768 -0.0230 0.019 Uiso 1 1 calc R . . C20 C 0.7952(2) 0.45183(11) 0.06075(10) 0.0149(5) Uani 1 1 d . . . C21 C 0.8137(2) 0.40146(11) 0.11174(11) 0.0176(5) Uani 1 1 d . . . H21 H 0.8881 0.4069 0.1464 0.021 Uiso 1 1 calc R . . C22 C 0.7236(2) 0.34354(12) 0.11178(10) 0.0171(5) Uani 1 1 d . . . H22 H 0.7377 0.3093 0.1467 0.020 Uiso 1 1 calc R . . C23 C 0.2994(2) 0.42719(13) -0.20057(11) 0.0222(5) Uani 1 1 d . . . O5 O 0.20871(18) 0.40570(10) -0.24396(8) 0.0341(4) Uani 1 1 d . . . O6 O 0.37206(19) 0.48379(10) -0.20250(8) 0.0406(5) Uani 1 1 d . . . C24 C 0.8929(2) 0.51611(12) 0.05913(10) 0.0167(5) Uani 1 1 d . . . O7 O 0.85259(16) 0.56865(8) 0.02275(8) 0.0242(4) Uani 1 1 d . . . O8 O 1.00543(16) 0.50945(8) 0.09560(8) 0.0275(4) Uani 1 1 d . . . N5 N 0.39009(17) 0.30249(9) 0.11521(8) 0.0123(4) Uani 1 1 d . . . N6 N 0.57580(17) 0.20294(9) 0.13073(8) 0.0124(4) Uani 1 1 d . . . C25 C 0.2913(2) 0.35348(12) 0.10015(11) 0.0163(5) Uani 1 1 d . . . H25 H 0.2654 0.3680 0.0560 0.020 Uiso 1 1 calc R . . C26 C 0.2271(2) 0.38502(12) 0.14780(11) 0.0184(5) Uani 1 1 d . . . H26 H 0.1560 0.4200 0.1364 0.022 Uiso 1 1 calc R . . C27 C 0.2674(2) 0.36511(12) 0.21230(11) 0.0182(5) Uani 1 1 d . . . C28 C 0.3716(2) 0.31435(12) 0.22764(11) 0.0175(5) Uani 1 1 d . . . H28 H 0.4026 0.3013 0.2718 0.021 Uiso 1 1 calc R . . C29 C 0.4304(2) 0.28267(12) 0.17822(10) 0.0135(4) Uani 1 1 d . . . C30 C 0.5357(2) 0.22601(12) 0.18728(10) 0.0135(4) Uani 1 1 d . . . C31 C 0.5941(2) 0.19716(12) 0.24665(11) 0.0169(5) Uani 1 1 d . . . H31 H 0.5636 0.2127 0.2856 0.020 Uiso 1 1 calc R . . C32 C 0.6976(2) 0.14528(12) 0.24923(11) 0.0182(5) Uani 1 1 d . . . C33 C 0.7356(2) 0.12105(12) 0.19101(11) 0.0192(5) Uani 1 1 d . . . H33 H 0.8047 0.0848 0.1914 0.023 Uiso 1 1 calc R . . C34 C 0.6712(2) 0.15045(12) 0.13273(11) 0.0163(5) Uani 1 1 d . . . H34 H 0.6954 0.1329 0.0930 0.020 Uiso 1 1 calc R . . C35 C 0.2023(2) 0.39831(13) 0.26644(12) 0.0232(5) Uani 1 1 d . . . O9 O 0.08282(16) 0.42597(10) 0.24489(8) 0.0280(4) Uani 1 1 d . . . H9A H 0.0538 0.4486 0.2752 0.042 Uiso 1 1 calc R . . O10 O 0.25777(19) 0.39645(13) 0.32213(9) 0.0508(6) Uani 1 1 d . . . C36 C 0.7640(2) 0.11720(13) 0.31457(11) 0.0235(5) Uani 1 1 d . . . O11 O 0.71469(18) 0.12859(10) 0.36311(8) 0.0334(4) Uani 1 1 d . . . O12 O 0.87633(19) 0.08166(11) 0.31076(8) 0.0394(5) Uani 1 1 d . . . H12 H 0.9092 0.0652 0.3477 0.059 Uiso 1 1 calc R . . O1W O -0.05184(19) -0.18437(11) 0.07451(10) 0.0337(5) Uani 1 1 d . . . H1WA H -0.019(3) -0.1464(17) 0.0687(15) 0.050 Uiso 1 1 d . . . H1WB H -0.026(3) -0.1937(17) 0.1148(15) 0.050 Uiso 1 1 d . . . O2W O 0.07378(19) -0.20984(10) -0.08437(9) 0.0320(4) Uani 1 1 d . . . H2WB H 0.050(3) -0.2394(16) -0.0609(15) 0.048 Uiso 1 1 d . . . H2WA H 0.093(3) -0.1696(16) -0.0645(15) 0.048 Uiso 1 1 d . . . O3W O 0.9458(2) 0.23094(12) -0.19947(10) 0.0448(6) Uani 1 1 d . . . H3WA H 0.879(3) 0.2008(19) -0.2129(17) 0.067 Uiso 1 1 d . . . H3WB H 0.977(4) 0.2438(19) -0.2297(17) 0.067 Uiso 1 1 d . . . O4W O 0.0850(2) 0.27734(11) -0.29681(10) 0.0401(5) Uani 1 1 d . . . H4WA H 0.102(3) 0.3195(18) -0.2811(16) 0.060 Uiso 1 1 d . . . H4WB H 0.039(3) 0.2834(18) -0.3345(16) 0.060 Uiso 1 1 d . . . O5W O 1.0190(2) 0.69097(12) 0.00687(11) 0.0459(6) Uani 1 1 d . . . H5WA H 0.985(3) 0.651(2) 0.0182(16) 0.069 Uiso 1 1 d . . . H5WB H 1.001(4) 0.722(2) 0.0328(17) 0.069 Uiso 1 1 d . . . O6W O -0.01983(18) 0.50618(10) 0.32367(8) 0.0246(4) Uani 1 1 d . . . H6WB H -0.091(3) 0.5285(15) 0.3013(13) 0.037 Uiso 1 1 d . . . H6WA H -0.037(3) 0.4914(15) 0.3571(14) 0.037 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01230(15) 0.01104(14) 0.00952(14) 0.00039(12) 0.00167(10) -0.00109(12) N1 0.0140(9) 0.0112(9) 0.0123(9) 0.0013(7) 0.0023(7) -0.0002(7) N2 0.0122(9) 0.0134(9) 0.0126(9) 0.0004(7) 0.0020(7) 0.0006(7) C1 0.0167(11) 0.0169(12) 0.0160(11) -0.0001(9) 0.0051(9) 0.0021(9) C2 0.0164(11) 0.0166(12) 0.0157(11) 0.0007(9) 0.0058(9) -0.0004(9) C3 0.0142(11) 0.0147(11) 0.0141(11) 0.0026(9) 0.0000(9) -0.0021(9) C4 0.0179(12) 0.0142(11) 0.0140(11) -0.0008(9) 0.0042(9) -0.0002(9) C5 0.0151(11) 0.0150(11) 0.0115(11) 0.0018(9) 0.0008(9) -0.0007(9) C6 0.0159(11) 0.0121(11) 0.0110(10) 0.0024(8) 0.0010(9) -0.0007(9) C7 0.0156(11) 0.0145(11) 0.0164(11) -0.0029(9) 0.0019(9) -0.0008(9) C8 0.0179(12) 0.0175(12) 0.0123(11) 0.0004(9) 0.0023(9) 0.0038(9) C9 0.0154(11) 0.0205(12) 0.0160(11) 0.0022(9) 0.0048(9) -0.0009(9) C10 0.0144(11) 0.0156(11) 0.0149(11) 0.0000(8) 0.0017(9) -0.0016(8) C11 0.0133(11) 0.0141(11) 0.0170(11) 0.0013(9) -0.0010(9) 0.0006(9) O1 0.0197(8) 0.0167(8) 0.0210(8) 0.0010(6) 0.0073(7) -0.0049(6) O2 0.0241(9) 0.0154(8) 0.0222(9) -0.0041(7) 0.0082(7) -0.0026(7) C12 0.0186(12) 0.0262(13) 0.0168(12) -0.0045(10) 0.0036(10) -0.0005(10) O3 0.0465(11) 0.0320(10) 0.0256(10) -0.0158(8) 0.0156(9) -0.0078(9) O4 0.0418(11) 0.0395(11) 0.0192(9) -0.0038(8) 0.0147(8) -0.0063(9) N3 0.0131(9) 0.0117(9) 0.0122(9) 0.0006(7) 0.0011(7) -0.0008(7) N4 0.0133(9) 0.0120(9) 0.0101(9) 0.0004(7) 0.0015(7) -0.0002(7) C13 0.0152(11) 0.0168(11) 0.0175(12) 0.0020(9) 0.0011(9) -0.0032(9) C14 0.0176(12) 0.0220(12) 0.0152(11) 0.0016(9) -0.0031(9) -0.0023(10) C15 0.0170(12) 0.0212(12) 0.0145(11) 0.0026(9) 0.0020(9) 0.0021(9) C16 0.0168(11) 0.0157(11) 0.0163(11) 0.0025(9) 0.0019(9) -0.0015(9) C17 0.0132(11) 0.0126(11) 0.0146(11) -0.0003(9) 0.0032(9) -0.0010(8) C18 0.0146(11) 0.0141(11) 0.0120(11) -0.0002(8) 0.0015(9) -0.0009(9) C19 0.0193(12) 0.0133(11) 0.0147(11) 0.0030(9) 0.0002(9) 0.0000(9) C20 0.0153(11) 0.0144(11) 0.0143(11) -0.0019(9) 0.0005(9) -0.0010(9) C21 0.0182(12) 0.0167(12) 0.0158(12) -0.0003(9) -0.0038(9) -0.0015(9) C22 0.0201(12) 0.0177(12) 0.0126(11) 0.0015(9) 0.0001(9) 0.0010(9) C23 0.0231(13) 0.0242(13) 0.0186(12) 0.0077(10) 0.0012(10) -0.0006(10) O5 0.0378(11) 0.0371(11) 0.0219(10) 0.0105(8) -0.0126(8) -0.0117(9) O6 0.0509(12) 0.0403(11) 0.0254(10) 0.0179(9) -0.0096(9) -0.0221(10) C24 0.0206(12) 0.0134(11) 0.0156(11) -0.0027(9) 0.0019(10) -0.0021(9) O7 0.0238(9) 0.0188(9) 0.0272(9) 0.0089(7) -0.0044(7) -0.0040(7) O8 0.0233(9) 0.0203(9) 0.0331(10) 0.0017(7) -0.0134(8) -0.0060(7) N5 0.0123(9) 0.0121(9) 0.0122(9) 0.0004(7) 0.0008(7) 0.0002(7) N6 0.0126(9) 0.0123(9) 0.0125(9) 0.0005(7) 0.0026(7) -0.0001(7) C25 0.0160(11) 0.0167(11) 0.0155(11) 0.0029(9) 0.0004(9) 0.0030(9) C26 0.0168(12) 0.0188(12) 0.0193(12) 0.0004(9) 0.0018(10) 0.0060(9) C27 0.0166(12) 0.0222(12) 0.0165(12) -0.0028(9) 0.0049(10) 0.0012(9) C28 0.0176(11) 0.0216(12) 0.0125(11) 0.0001(9) 0.0004(9) 0.0028(9) C29 0.0138(11) 0.0139(11) 0.0124(11) 0.0016(9) 0.0003(9) -0.0012(9) C30 0.0119(11) 0.0147(11) 0.0137(11) 0.0006(8) 0.0014(9) 0.0002(8) C31 0.0175(12) 0.0211(12) 0.0121(11) 0.0011(9) 0.0023(9) 0.0019(9) C32 0.0181(12) 0.0168(11) 0.0192(12) 0.0041(9) 0.0015(10) 0.0022(9) C33 0.0179(12) 0.0195(12) 0.0204(12) 0.0014(9) 0.0039(10) 0.0060(9) C34 0.0160(11) 0.0166(11) 0.0169(11) -0.0001(9) 0.0046(9) 0.0019(9) C35 0.0217(13) 0.0285(14) 0.0197(13) -0.0013(10) 0.0041(11) 0.0069(10) O9 0.0294(10) 0.0370(11) 0.0186(9) -0.0016(8) 0.0067(8) 0.0168(8) O10 0.0344(11) 0.0960(18) 0.0205(10) -0.0162(11) -0.0005(9) 0.0297(11) C36 0.0265(14) 0.0222(13) 0.0204(13) 0.0026(10) -0.0004(11) 0.0058(10) O11 0.0358(11) 0.0464(12) 0.0176(9) 0.0089(8) 0.0037(8) 0.0147(9) O12 0.0405(11) 0.0535(13) 0.0228(10) 0.0071(9) 0.0007(9) 0.0306(10) O1W 0.0342(11) 0.0293(11) 0.0358(11) 0.0047(9) 0.0004(9) -0.0155(9) O2W 0.0387(11) 0.0251(11) 0.0311(11) -0.0024(8) 0.0026(9) -0.0046(9) O3W 0.0526(14) 0.0500(14) 0.0313(12) 0.0035(10) 0.0053(10) -0.0142(10) O4W 0.0483(13) 0.0327(11) 0.0362(12) 0.0022(10) -0.0024(10) -0.0017(10) O5W 0.0586(14) 0.0356(12) 0.0494(14) -0.0091(10) 0.0267(11) -0.0215(11) O6W 0.0294(10) 0.0284(10) 0.0171(9) 0.0046(7) 0.0068(8) 0.0098(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.9398(17) . ? Co1 N2 1.9433(17) . ? Co1 N3 1.9354(17) . ? Co1 N4 1.9440(17) . ? Co1 N5 1.9261(17) . ? Co1 N6 1.9279(17) . ? N1 C1 1.343(3) . ? N1 C5 1.359(3) . ? N2 C6 1.355(3) . ? N2 C10 1.343(3) . ? C1 C2 1.376(3) . ? C2 C3 1.388(3) . ? C3 C4 1.391(3) . ? C3 C11 1.532(3) . ? C4 C5 1.383(3) . ? C5 C6 1.469(3) . ? C6 C7 1.378(3) . ? C7 C8 1.387(3) . ? C8 C9 1.381(3) . ? C8 C12 1.509(3) . ? C9 C10 1.384(3) . ? C11 O1 1.255(2) . ? C11 O2 1.250(2) . ? C12 O3 1.282(3) . ? C12 O4 1.223(3) . ? N3 C13 1.344(3) . ? N3 C17 1.357(2) . ? N4 C18 1.359(3) . ? N4 C22 1.341(3) . ? C13 C14 1.387(3) . ? C14 C15 1.382(3) . ? C15 C16 1.385(3) . ? C15 C23 1.514(3) . ? C16 C17 1.380(3) . ? C17 C18 1.464(3) . ? C18 C19 1.386(3) . ? C19 C20 1.386(3) . ? C20 C21 1.391(3) . ? C20 C24 1.522(3) . ? C21 C22 1.382(3) . ? C23 O5 1.230(3) . ? C23 O6 1.261(3) . ? C24 O7 1.245(3) . ? C24 O8 1.250(3) . ? N5 C25 1.349(3) . ? N5 C29 1.355(3) . ? N6 C30 1.365(3) . ? N6 C34 1.340(3) . ? C25 C26 1.384(3) . ? C26 C27 1.384(3) . ? C27 C28 1.384(3) . ? C27 C35 1.508(3) . ? C28 C29 1.384(3) . ? C29 C30 1.457(3) . ? C30 C31 1.380(3) . ? C31 C32 1.389(3) . ? C32 C33 1.394(3) . ? C32 C36 1.501(3) . ? C33 C34 1.383(3) . ? C35 O9 1.298(3) . ? C35 O10 1.199(3) . ? C36 O11 1.206(3) . ? C36 O12 1.300(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N2 83.33(7) . . ? N1 Co1 N3 96.04(7) . . ? N1 Co1 N4 177.36(7) . . ? N1 Co1 N5 94.32(7) . . ? N1 Co1 N6 86.83(7) . . ? N2 Co1 N3 83.17(7) . . ? N2 Co1 N4 94.04(7) . . ? N2 Co1 N5 177.41(7) . . ? N2 Co1 N6 97.45(7) . . ? N3 Co1 N4 83.42(7) . . ? N3 Co1 N5 96.03(7) . . ? N3 Co1 N6 177.12(7) . . ? N4 Co1 N5 88.30(7) . . ? N4 Co1 N6 93.72(7) . . ? N5 Co1 N6 83.47(7) . . ? Co1 N1 C1 127.36(15) . . ? Co1 N1 C5 114.25(13) . . ? C1 N1 C5 118.09(18) . . ? Co1 N2 C6 113.55(13) . . ? Co1 N2 C10 125.90(14) . . ? C6 N2 C10 119.11(18) . . ? N1 C1 C2 122.4(2) . . ? C1 C2 C3 120.1(2) . . ? C2 C3 C4 117.7(2) . . ? C2 C3 C11 122.05(19) . . ? C4 C3 C11 120.19(19) . . ? C3 C4 C5 119.5(2) . . ? N1 C5 C4 122.07(19) . . ? N1 C5 C6 113.39(18) . . ? C4 C5 C6 124.55(19) . . ? N2 C6 C5 114.46(18) . . ? N2 C6 C7 121.89(19) . . ? C5 C6 C7 123.52(19) . . ? C6 C7 C8 118.7(2) . . ? C7 C8 C9 119.4(2) . . ? C7 C8 C12 119.3(2) . . ? C9 C8 C12 121.2(2) . . ? C8 C9 C10 119.2(2) . . ? N2 C10 C9 121.6(2) . . ? C3 C11 O1 116.20(19) . . ? C3 C11 O2 116.87(18) . . ? O1 C11 O2 126.9(2) . . ? C8 C12 O3 112.6(2) . . ? C8 C12 O4 120.6(2) . . ? O3 C12 O4 126.7(2) . . ? Co1 N3 C13 126.09(14) . . ? Co1 N3 C17 113.81(13) . . ? C13 N3 C17 119.34(18) . . ? Co1 N4 C18 113.83(13) . . ? Co1 N4 C22 127.27(14) . . ? C18 N4 C22 118.87(18) . . ? N3 C13 C14 121.7(2) . . ? C13 C14 C15 119.2(2) . . ? C14 C15 C16 118.9(2) . . ? C14 C15 C23 122.7(2) . . ? C16 C15 C23 118.3(2) . . ? C15 C16 C17 119.7(2) . . ? N3 C17 C16 121.08(19) . . ? N3 C17 C18 114.47(18) . . ? C16 C17 C18 124.39(19) . . ? N4 C18 C17 114.05(18) . . ? N4 C18 C19 121.54(19) . . ? C17 C18 C19 124.36(19) . . ? C18 C19 C20 119.69(19) . . ? C19 C20 C21 118.10(19) . . ? C19 C20 C24 120.77(19) . . ? C21 C20 C24 121.11(19) . . ? C20 C21 C22 119.8(2) . . ? N4 C22 C21 122.0(2) . . ? C15 C23 O5 120.1(2) . . ? C15 C23 O6 113.8(2) . . ? O5 C23 O6 126.2(2) . . ? C20 C24 O7 117.48(19) . . ? C20 C24 O8 114.84(19) . . ? O7 C24 O8 127.7(2) . . ? Co1 N5 C25 125.69(15) . . ? Co1 N5 C29 114.38(13) . . ? C25 N5 C29 119.92(18) . . ? Co1 N6 C30 113.98(13) . . ? Co1 N6 C34 126.47(14) . . ? C30 N6 C34 119.54(18) . . ? N5 C25 C26 121.2(2) . . ? C25 C26 C27 119.3(2) . . ? C26 C27 C28 119.2(2) . . ? C26 C27 C35 121.7(2) . . ? C28 C27 C35 119.1(2) . . ? C27 C28 C29 119.6(2) . . ? N5 C29 C28 120.74(19) . . ? N5 C29 C30 114.08(18) . . ? C28 C29 C30 125.16(19) . . ? N6 C30 C29 114.00(18) . . ? N6 C30 C31 120.95(19) . . ? C29 C30 C31 125.05(19) . . ? C30 C31 C32 119.7(2) . . ? C31 C32 C33 118.8(2) . . ? C31 C32 C36 118.8(2) . . ? C33 C32 C36 122.5(2) . . ? C32 C33 C34 119.1(2) . . ? N6 C34 C33 121.9(2) . . ? C27 C35 O9 111.8(2) . . ? C27 C35 O10 121.6(2) . . ? O9 C35 O10 126.6(2) . . ? C32 C36 O11 121.3(2) . . ? C32 C36 O12 111.8(2) . . ? O11 C36 O12 126.9(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O6 0.84 1.59 2.422(2) 171.3 2_644 O9 H9A O6W 0.84 1.70 2.525(2) 168.0 . O12 H12 O8 0.84 1.68 2.482(2) 159.4 2_745 O1W H1WA O1 0.78(3) 1.98(3) 2.759(2) 175(3) . O1W H1WB O3W 0.85(3) 1.93(3) 2.773(3) 168(3) 3_655 O2W H2WB O5W 0.79(3) 1.95(3) 2.734(3) 171(3) 1_445 O2W H2WA O2 0.85(3) 1.97(3) 2.802(2) 168(3) . O3W H3WA O4 0.87(3) 1.93(3) 2.789(3) 166(3) . O3W H3WB O4W 0.78(3) 1.98(3) 2.754(3) 170(4) 1_655 O4W H4WA O5 0.84(3) 1.98(3) 2.783(3) 160(3) . O4W H4WB O2W 0.85(3) 1.87(3) 2.717(3) 175(3) 2_554 O5W H5WA O7 0.86(4) 2.00(4) 2.821(2) 161(3) . O5W H5WB O1W 0.82(4) 2.02(4) 2.817(3) 164(3) 1_665 O6W H6WB O5 0.88(3) 1.94(3) 2.798(2) 164(2) 3_565 _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.500 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.067 #==END=================================================================