# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'George Shimizu' _publ_contact_author_address ; Department of Chemistry University of Calgary 2500 University Drive NW Calgary Alberta T2N 1N4 CANADA ; _publ_contact_author_email GSHIMIZU@UCALGARY.CA _publ_section_title ; Selective guest inclusion in a non-porous H-bonded host ; loop_ _publ_author_name 'George Shimizu' 'Sean A. Dalrymple' # Attachment '1-Co(NH3)6(C8H8S2O6)1.5(H2O)2.CIF' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 289134' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co(NH3)6(C8H8S2O6)1.5(H2O)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H25 Co N6 O11 S3' _chemical_formula_weight 584.49 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' Co Co 0.3494 0.9721 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5100(2) _cell_length_b 13.2100(3) _cell_length_c 13.8450(4) _cell_angle_alpha 63.9100(11) _cell_angle_beta 84.7360(11) _cell_angle_gamma 86.8150(18) _cell_volume 1228.19(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 302 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9300 _exptl_absorpt_correction_T_max 0.9581 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10516 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5586 _reflns_number_gt 4021 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0754P)^2^+0.4176P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5586 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Co1 Co 0.0000 0.5000 0.0000 0.01543(16) Uani 1 2 d S . . Co2 Co 0.5000 0.0000 1.0000 0.01733(16) Uani 1 2 d S . . S1 S 0.49890(10) 0.39399(7) 0.23345(7) 0.01931(19) Uani 1 1 d . . . S2 S 0.06441(10) -0.06297(7) 0.78214(6) 0.0202(2) Uani 1 1 d . . . S3 S -0.03445(10) 0.28943(7) 0.81001(6) 0.0197(2) Uani 1 1 d . . . O1 O 0.6500(3) 0.3159(2) 0.2549(2) 0.0278(6) Uani 1 1 d . . . O2 O 0.3519(3) 0.3566(2) 0.1947(2) 0.0290(6) Uani 1 1 d . . . O3 O 0.5468(3) 0.5098(2) 0.16170(19) 0.0290(6) Uani 1 1 d . . . O4 O 0.0418(3) -0.1824(2) 0.8540(2) 0.0346(6) Uani 1 1 d . . . O5 O 0.1811(3) -0.0072(2) 0.8215(2) 0.0319(6) Uani 1 1 d . . . O6 O -0.1072(3) -0.0040(2) 0.7559(2) 0.0289(6) Uani 1 1 d . . . O7 O 0.1347(3) 0.3298(2) 0.8230(2) 0.0359(7) Uani 1 1 d . . . O8 O -0.0742(3) 0.1765(2) 0.89195(19) 0.0287(6) Uani 1 1 d . . . O9 O -0.1798(3) 0.3703(2) 0.8032(2) 0.0283(6) Uani 1 1 d . . . O10 O 0.4913(3) 0.3128(2) 0.7543(2) 0.0349(6) Uani 1 1 d . . . O11 O 0.5963(3) -0.1410(2) 0.7996(2) 0.0326(6) Uani 1 1 d . . . N1 N -0.2008(3) 0.4061(2) 0.0082(2) 0.0205(6) Uani 1 1 d . . . H1A H -0.3048 0.4353 0.0254 0.031 Uiso 1 1 calc R . . H1B H -0.1839 0.3346 0.0598 0.031 Uiso 1 1 calc R . . H1C H -0.2065 0.4051 -0.0567 0.031 Uiso 1 1 calc R . . N2 N -0.0181(3) 0.4413(2) 0.1578(2) 0.0188(6) Uani 1 1 d . . . H2A H -0.0327 0.4998 0.1760 0.028 Uiso 1 1 calc R . . H2B H 0.0835 0.4019 0.1843 0.028 Uiso 1 1 calc R . . H2C H -0.1137 0.3951 0.1862 0.028 Uiso 1 1 calc R . . N3 N -0.1700(3) 0.6228(2) -0.0114(2) 0.0206(6) Uani 1 1 d . . . H3A H -0.2536 0.6290 -0.0575 0.031 Uiso 1 1 calc R . . H3B H -0.1103 0.6887 -0.0369 0.031 Uiso 1 1 calc R . . H3C H -0.2249 0.6075 0.0548 0.031 Uiso 1 1 calc R . . N4 N 0.4362(4) -0.1423(2) 1.0007(2) 0.0227(6) Uani 1 1 d . . . H4A H 0.4933 -0.1484 0.9426 0.034 Uiso 1 1 calc R . . H4B H 0.3159 -0.1436 0.9976 0.034 Uiso 1 1 calc R . . H4C H 0.4698 -0.2010 1.0623 0.034 Uiso 1 1 calc R . . N5 N 0.2477(3) 0.0467(2) 0.9952(2) 0.0241(6) Uani 1 1 d . . . H5A H 0.2040 0.0478 0.9356 0.036 Uiso 1 1 calc R . . H5B H 0.2371 0.1168 0.9925 0.036 Uiso 1 1 calc R . . H5C H 0.1846 -0.0029 1.0553 0.036 Uiso 1 1 calc R . . N6 N 0.5270(4) 0.0683(2) 0.8416(2) 0.0211(6) Uani 1 1 d . . . H6A H 0.6378 0.0514 0.8196 0.032 Uiso 1 1 calc R . . H6B H 0.5131 0.1445 0.8151 0.032 Uiso 1 1 calc R . . H6C H 0.4426 0.0408 0.8168 0.032 Uiso 1 1 calc R . . C1 C 0.4141(5) 0.3907(3) 0.3590(3) 0.0262(8) Uani 1 1 d . . . H1D H 0.5092 0.4134 0.3902 0.039 Uiso 1 1 calc R . . H1E H 0.3139 0.4459 0.3468 0.039 Uiso 1 1 calc R . . C2 C 0.3498(5) 0.2757(3) 0.4379(3) 0.0241(7) Uani 1 1 d . . . C3 C 0.1717(5) 0.2466(3) 0.4476(3) 0.0257(8) Uani 1 1 d . . . H3 H 0.0884 0.3012 0.4049 0.039 Uiso 1 1 calc R . . C4 C 0.1136(5) 0.1401(3) 0.5179(3) 0.0253(7) Uani 1 1 d . . . H4 H -0.0088 0.1223 0.5228 0.038 Uiso 1 1 calc R . . C5 C 0.2327(5) 0.0580(3) 0.5821(3) 0.0241(7) Uani 1 1 d . . . C6 C 0.4116(5) 0.0867(3) 0.5727(3) 0.0315(9) Uani 1 1 d . . . H6 H 0.4951 0.0322 0.6152 0.047 Uiso 1 1 calc R . . C7 C 0.4687(5) 0.1942(3) 0.5019(3) 0.0305(8) Uani 1 1 d . . . H7 H 0.5908 0.2125 0.4969 0.046 Uiso 1 1 calc R . . C8 C 0.1718(5) -0.0572(3) 0.6596(3) 0.0279(8) Uani 1 1 d . . . H8A H 0.2764 -0.1095 0.6767 0.042 Uiso 1 1 calc R . . H8B H 0.0878 -0.0835 0.6247 0.042 Uiso 1 1 calc R . . C9 C -0.0100(5) 0.2800(3) 0.6848(3) 0.0254(8) Uani 1 1 d . . . H9A H 0.1014 0.2372 0.6822 0.038 Uiso 1 1 calc R . . H9B H -0.1115 0.2376 0.6808 0.038 Uiso 1 1 calc R . . C10 C -0.0035(5) 0.3931(3) 0.5893(3) 0.0227(7) Uani 1 1 d . . . C11 C 0.1538(5) 0.4547(3) 0.5538(3) 0.0269(8) Uani 1 1 d . . . H11 H 0.2596 0.4242 0.5898 0.040 Uiso 1 1 calc R . . C12 C 0.1567(5) 0.5602(3) 0.4662(3) 0.0265(8) Uani 1 1 d . . . H12 H 0.2645 0.6015 0.4434 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0173(3) 0.0139(3) 0.0140(3) -0.0051(2) 0.0001(2) -0.0026(2) Co2 0.0175(3) 0.0156(3) 0.0196(3) -0.0082(3) -0.0022(2) -0.0011(2) S1 0.0194(4) 0.0176(4) 0.0193(4) -0.0069(3) 0.0013(3) -0.0016(3) S2 0.0227(4) 0.0181(4) 0.0182(4) -0.0063(3) 0.0000(3) -0.0032(3) S3 0.0204(4) 0.0212(4) 0.0172(4) -0.0081(3) -0.0007(3) -0.0013(3) O1 0.0202(12) 0.0245(13) 0.0334(15) -0.0088(11) 0.0020(10) 0.0028(10) O2 0.0238(12) 0.0362(15) 0.0319(14) -0.0183(12) -0.0075(10) -0.0012(10) O3 0.0345(14) 0.0177(13) 0.0260(14) -0.0033(11) 0.0095(10) -0.0043(10) O4 0.0439(15) 0.0174(13) 0.0288(15) 0.0009(11) 0.0080(12) -0.0042(11) O5 0.0294(13) 0.0434(16) 0.0293(15) -0.0207(13) -0.0038(11) -0.0077(11) O6 0.0223(12) 0.0268(14) 0.0353(15) -0.0116(12) -0.0027(10) 0.0006(10) O7 0.0258(13) 0.0579(19) 0.0329(15) -0.0272(14) 0.0018(11) -0.0141(12) O8 0.0348(14) 0.0230(13) 0.0207(13) -0.0033(11) 0.0007(10) 0.0023(10) O9 0.0303(13) 0.0274(14) 0.0283(14) -0.0134(11) -0.0049(10) 0.0070(10) O10 0.0322(14) 0.0227(14) 0.0503(18) -0.0165(13) -0.0048(12) 0.0019(11) O11 0.0324(14) 0.0303(15) 0.0394(16) -0.0199(13) 0.0031(11) -0.0048(11) N1 0.0222(14) 0.0196(15) 0.0172(14) -0.0055(12) -0.0009(11) -0.0033(11) N2 0.0173(13) 0.0203(15) 0.0175(14) -0.0068(12) -0.0001(10) -0.0033(11) N3 0.0221(14) 0.0179(14) 0.0188(14) -0.0053(12) -0.0009(11) -0.0011(11) N4 0.0253(15) 0.0200(15) 0.0248(16) -0.0116(13) -0.0022(12) -0.0012(11) N5 0.0228(14) 0.0246(16) 0.0288(16) -0.0149(13) -0.0046(12) 0.0006(12) N6 0.0233(14) 0.0193(15) 0.0227(15) -0.0107(12) -0.0032(11) -0.0004(11) C1 0.0356(19) 0.0207(18) 0.0216(18) -0.0095(15) 0.0041(14) -0.0033(14) C2 0.0356(19) 0.0214(18) 0.0167(17) -0.0107(15) 0.0036(14) -0.0008(14) C3 0.0309(19) 0.0242(19) 0.0177(18) -0.0060(15) 0.0001(14) 0.0033(14) C4 0.0291(18) 0.0256(19) 0.0190(18) -0.0080(15) -0.0003(14) -0.0017(14) C5 0.0349(19) 0.0196(17) 0.0171(17) -0.0082(14) 0.0031(14) -0.0016(14) C6 0.037(2) 0.024(2) 0.0222(19) -0.0008(16) 0.0006(15) 0.0034(16) C7 0.0288(19) 0.031(2) 0.026(2) -0.0088(17) 0.0025(15) -0.0013(15) C8 0.040(2) 0.0225(19) 0.0207(18) -0.0099(15) 0.0041(15) -0.0011(15) C9 0.0363(19) 0.0211(18) 0.0218(18) -0.0121(15) -0.0028(14) 0.0008(15) C10 0.0346(19) 0.0200(17) 0.0137(17) -0.0082(14) 0.0011(14) -0.0002(14) C11 0.0307(18) 0.029(2) 0.0175(18) -0.0069(15) -0.0016(14) 0.0010(15) C12 0.0302(18) 0.028(2) 0.0224(19) -0.0119(16) 0.0003(14) -0.0037(15) _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 N2 1.965(3) 2_565 ? Co1 N2 1.965(3) . ? Co1 N3 1.967(3) . ? Co1 N3 1.967(3) 2_565 ? Co1 N1 1.969(3) 2_565 ? Co1 N1 1.969(3) . ? Co2 N5 1.958(3) 2_657 ? Co2 N5 1.958(3) . ? Co2 N4 1.961(3) 2_657 ? Co2 N4 1.961(3) . ? Co2 N6 1.965(3) 2_657 ? Co2 N6 1.965(3) . ? S1 O1 1.450(2) . ? S1 O3 1.454(2) . ? S1 O2 1.468(2) . ? S1 C1 1.779(3) . ? S2 O5 1.455(3) . ? S2 O6 1.458(2) . ? S2 O4 1.459(2) . ? S2 C8 1.782(4) . ? S3 O8 1.449(2) . ? S3 O7 1.460(3) . ? S3 O9 1.464(2) . ? S3 C9 1.784(3) . ? C1 C2 1.503(5) . ? C2 C3 1.390(5) . ? C2 C7 1.393(5) . ? C3 C4 1.380(5) . ? C4 C5 1.399(5) . ? C5 C6 1.395(5) . ? C5 C8 1.493(5) . ? C6 C7 1.389(5) . ? C9 C10 1.497(5) . ? C10 C11 1.396(5) . ? C10 C12 1.400(5) 2_566 ? C11 C12 1.388(5) . ? C12 C10 1.400(5) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N2 180.00(6) 2_565 . ? N2 Co1 N3 89.58(11) 2_565 . ? N2 Co1 N3 90.42(11) . . ? N2 Co1 N3 90.42(11) 2_565 2_565 ? N2 Co1 N3 89.58(11) . 2_565 ? N3 Co1 N3 180.0 . 2_565 ? N2 Co1 N1 90.65(11) 2_565 2_565 ? N2 Co1 N1 89.35(11) . 2_565 ? N3 Co1 N1 90.35(11) . 2_565 ? N3 Co1 N1 89.65(11) 2_565 2_565 ? N2 Co1 N1 89.35(11) 2_565 . ? N2 Co1 N1 90.65(11) . . ? N3 Co1 N1 89.65(11) . . ? N3 Co1 N1 90.35(11) 2_565 . ? N1 Co1 N1 180.000(1) 2_565 . ? N5 Co2 N5 180.000(1) 2_657 . ? N5 Co2 N4 90.18(12) 2_657 2_657 ? N5 Co2 N4 89.82(12) . 2_657 ? N5 Co2 N4 89.82(12) 2_657 . ? N5 Co2 N4 90.18(12) . . ? N4 Co2 N4 180.0 2_657 . ? N5 Co2 N6 90.16(12) 2_657 2_657 ? N5 Co2 N6 89.84(12) . 2_657 ? N4 Co2 N6 89.22(12) 2_657 2_657 ? N4 Co2 N6 90.78(12) . 2_657 ? N5 Co2 N6 89.84(12) 2_657 . ? N5 Co2 N6 90.16(12) . . ? N4 Co2 N6 90.78(12) 2_657 . ? N4 Co2 N6 89.22(12) . . ? N6 Co2 N6 180.0 2_657 . ? O1 S1 O3 113.24(14) . . ? O1 S1 O2 111.47(15) . . ? O3 S1 O2 111.58(15) . . ? O1 S1 C1 107.09(16) . . ? O3 S1 C1 107.39(16) . . ? O2 S1 C1 105.58(16) . . ? O5 S2 O6 111.93(15) . . ? O5 S2 O4 113.21(16) . . ? O6 S2 O4 111.68(15) . . ? O5 S2 C8 106.84(17) . . ? O6 S2 C8 106.88(16) . . ? O4 S2 C8 105.77(16) . . ? O8 S3 O7 112.47(16) . . ? O8 S3 O9 112.69(14) . . ? O7 S3 O9 110.74(16) . . ? O8 S3 C9 105.86(16) . . ? O7 S3 C9 107.06(16) . . ? O9 S3 C9 107.62(15) . . ? C2 C1 S1 112.0(2) . . ? C3 C2 C7 118.1(3) . . ? C3 C2 C1 121.3(3) . . ? C7 C2 C1 120.6(3) . . ? C4 C3 C2 121.3(3) . . ? C3 C4 C5 120.8(3) . . ? C6 C5 C4 118.2(3) . . ? C6 C5 C8 120.3(3) . . ? C4 C5 C8 121.5(3) . . ? C7 C6 C5 120.6(3) . . ? C6 C7 C2 121.1(3) . . ? C5 C8 S2 113.3(2) . . ? C10 C9 S3 112.8(2) . . ? C11 C10 C12 118.4(3) . 2_566 ? C11 C10 C9 121.2(3) . . ? C12 C10 C9 120.4(3) 2_566 . ? C12 C11 C10 120.4(3) . . ? C11 C12 C10 121.1(3) . 2_566 ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 S1 C1 C2 -61.5(3) . . . . ? O3 S1 C1 C2 176.6(2) . . . . ? O2 S1 C1 C2 57.4(3) . . . . ? S1 C1 C2 C3 -93.5(4) . . . . ? S1 C1 C2 C7 85.1(4) . . . . ? C7 C2 C3 C4 -0.3(5) . . . . ? C1 C2 C3 C4 178.2(3) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C3 C4 C5 C6 -0.2(5) . . . . ? C3 C4 C5 C8 179.2(3) . . . . ? C4 C5 C6 C7 0.3(5) . . . . ? C8 C5 C6 C7 -179.1(3) . . . . ? C5 C6 C7 C2 -0.5(6) . . . . ? C3 C2 C7 C6 0.5(5) . . . . ? C1 C2 C7 C6 -178.1(3) . . . . ? C6 C5 C8 S2 100.3(4) . . . . ? C4 C5 C8 S2 -79.1(4) . . . . ? O5 S2 C8 C5 -49.8(3) . . . . ? O6 S2 C8 C5 70.2(3) . . . . ? O4 S2 C8 C5 -170.7(3) . . . . ? O8 S3 C9 C10 168.9(2) . . . . ? O7 S3 C9 C10 -70.9(3) . . . . ? O9 S3 C9 C10 48.1(3) . . . . ? S3 C9 C10 C11 80.6(4) . . . . ? S3 C9 C10 C12 -99.0(3) . . . 2_566 ? C12 C10 C11 C12 0.7(6) 2_566 . . . ? C9 C10 C11 C12 -178.9(3) . . . . ? C10 C11 C12 C10 -0.7(6) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.747 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.229 # Attachment '2-Co(NH3)6(C8H8S2O6)1.5(H2O)3(Aniline)0.5.CIF' data_import _database_code_depnum_ccdc_archive 'CCDC 289135' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co(NH3)6(C8H8S2O6)1.5(H2O)3(Aniline)0.5 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H65 Co2 N13 O24 S6' _chemical_formula_weight 1302.17 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' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.567(5) _cell_length_b 15.427(5) _cell_length_c 15.552(5) _cell_angle_alpha 60.837(5) _cell_angle_beta 74.578(5) _cell_angle_gamma 66.910(5) _cell_volume 2795.2(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8399 _exptl_absorpt_correction_T_max 0.8542 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24017 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.1352 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.51 _reflns_number_total 12781 _reflns_number_gt 5800 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1143P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12781 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1659 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.2327 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Co1 Co 1.0000 0.5000 0.5000 0.0159(3) Uani 1 2 d S . . Co2 Co 1.0000 0.0000 1.0000 0.0203(3) Uani 1 2 d S . . Co3 Co 1.0000 0.0000 0.5000 0.0164(3) Uani 1 2 d S . . Co4 Co 1.0000 -0.5000 1.0000 0.0192(3) Uani 1 2 d S . . S1 S 0.79086(10) 0.35291(11) 0.50272(10) 0.0195(3) Uani 1 1 d . . . S2 S 0.76614(11) -0.01590(13) 0.78075(10) 0.0310(4) Uani 1 1 d . . . S3 S 0.18090(11) 0.28196(11) 0.78789(10) 0.0249(4) Uani 1 1 d . . . S4 S 0.80590(11) 0.22504(12) 0.23711(10) 0.0254(4) Uani 1 1 d . . . S5 S 0.23271(11) 0.52977(12) 0.22644(10) 0.0275(4) Uani 1 1 d . . . S6 S 0.78841(10) -0.15469(11) 0.51538(10) 0.0204(3) Uani 1 1 d . . . N1 N 0.8526(3) 0.5599(3) 0.5047(3) 0.0198(10) Uani 1 1 d . . . H1A H 0.8347 0.6119 0.4441 0.030 Uiso 1 1 calc R . . H1B H 0.8298 0.5865 0.5501 0.030 Uiso 1 1 calc R . . H1C H 0.8252 0.5092 0.5219 0.030 Uiso 1 1 calc R . . N2 N 1.0009(3) 0.4689(3) 0.3902(3) 0.0211(10) Uani 1 1 d . . . H2A H 1.0287 0.5114 0.3333 0.032 Uiso 1 1 calc R . . H2B H 0.9370 0.4799 0.3823 0.032 Uiso 1 1 calc R . . H2C H 1.0375 0.4010 0.4045 0.032 Uiso 1 1 calc R . . N3 N 0.9913(3) 0.3599(3) 0.5967(3) 0.0237(11) Uani 1 1 d . . . H3A H 1.0168 0.3159 0.5670 0.036 Uiso 1 1 calc R . . H3B H 0.9261 0.3640 0.6193 0.036 Uiso 1 1 calc R . . H3C H 1.0271 0.3351 0.6482 0.036 Uiso 1 1 calc R . . N4 N 0.9843(4) 0.1460(4) 0.9089(3) 0.0349(13) Uani 1 1 d . . . H4A H 0.9610 0.1615 0.8526 0.052 Uiso 1 1 calc R . . H4B H 1.0446 0.1574 0.8937 0.052 Uiso 1 1 calc R . . H4C H 0.9399 0.1875 0.9377 0.052 Uiso 1 1 calc R . . N5 N 1.0102(4) -0.0265(4) 0.8865(3) 0.0352(13) Uani 1 1 d . . . H5A H 1.0682 -0.0184 0.8481 0.053 Uiso 1 1 calc R . . H5B H 0.9571 0.0194 0.8505 0.053 Uiso 1 1 calc R . . H5C H 1.0101 -0.0929 0.9082 0.053 Uiso 1 1 calc R . . N6 N 1.1477(3) -0.0337(4) 0.9870(3) 0.0299(12) Uani 1 1 d . . . H6A H 1.1657 -0.0290 1.0360 0.045 Uiso 1 1 calc R . . H6B H 1.1676 0.0122 0.9272 0.045 Uiso 1 1 calc R . . H6C H 1.1775 -0.0998 0.9920 0.045 Uiso 1 1 calc R . . N7 N 0.8524(3) 0.0586(3) 0.5050(3) 0.0202(10) Uani 1 1 d . . . H7A H 0.8267 0.0147 0.5028 0.030 Uiso 1 1 calc R . . H7B H 0.8347 0.1221 0.4523 0.030 Uiso 1 1 calc R . . H7C H 0.8278 0.0661 0.5620 0.030 Uiso 1 1 calc R . . N8 N 0.9961(3) 0.0464(4) 0.5988(3) 0.0227(11) Uani 1 1 d . . . H8A H 0.9635 0.0112 0.6566 0.034 Uiso 1 1 calc R . . H8B H 0.9633 0.1162 0.5764 0.034 Uiso 1 1 calc R . . H8C H 1.0598 0.0332 0.6092 0.034 Uiso 1 1 calc R . . N9 N 0.9883(3) -0.1357(3) 0.6055(3) 0.0208(10) Uani 1 1 d . . . H9A H 1.0118 -0.1496 0.6610 0.031 Uiso 1 1 calc R . . H9B H 1.0248 -0.1869 0.5853 0.031 Uiso 1 1 calc R . . H9C H 0.9228 -0.1333 0.6189 0.031 Uiso 1 1 calc R . . N10 N 0.8686(3) -0.4087(4) 1.0236(3) 0.0299(12) Uani 1 1 d . . . H10A H 0.8675 -0.3410 0.9878 0.045 Uiso 1 1 calc R . . H10B H 0.8559 -0.4239 1.0891 0.045 Uiso 1 1 calc R . . H10C H 0.8209 -0.4188 1.0048 0.045 Uiso 1 1 calc R . . N11 N 1.0094(4) -0.3867(4) 0.8683(3) 0.0318(12) Uani 1 1 d . . . H11A H 0.9557 -0.3679 0.8365 0.048 Uiso 1 1 calc R . . H11B H 1.0668 -0.4087 0.8333 0.048 Uiso 1 1 calc R . . H11C H 1.0099 -0.3309 0.8740 0.048 Uiso 1 1 calc R . . N12 N 1.0585(4) -0.4443(4) 1.0538(3) 0.0282(12) Uani 1 1 d . . . H12A H 1.0685 -0.3835 1.0054 0.042 Uiso 1 1 calc R . . H12B H 1.1182 -0.4914 1.0768 0.042 Uiso 1 1 calc R . . H12C H 1.0161 -0.4320 1.1042 0.042 Uiso 1 1 calc R . . N13S N 0.6797(4) 0.5590(4) 0.0121(4) 0.0425(14) Uani 1 1 d . . . C1 C 0.6804(4) 0.3278(4) 0.5042(4) 0.0219(13) Uani 1 1 d . . . H1A' H 0.6867 0.3148 0.4462 0.026 Uiso 1 1 calc . . . H1B' H 0.6750 0.2637 0.5645 0.026 Uiso 1 1 calc . . . C2 C 0.5867(4) 0.4160(4) 0.5023(4) 0.0199(12) Uani 1 1 d . . . C3 C 0.5511(4) 0.4964(5) 0.4134(4) 0.0246(13) Uani 1 1 d . . . H3 H 0.5855 0.4946 0.3529 0.030 Uiso 1 1 calc . . . C4 C 0.5340(4) 0.4206(4) 0.5881(4) 0.0238(13) Uani 1 1 d . . . H4 H 0.5564 0.3658 0.6499 0.029 Uiso 1 1 calc . . . C5 C 0.6601(4) -0.0400(5) 0.7724(4) 0.0337(15) Uani 1 1 d . . . H5A' H 0.6708 -0.0495 0.7116 0.040 Uiso 1 1 calc . . . H5B' H 0.6541 -0.1060 0.8296 0.040 Uiso 1 1 calc . . . C6 C 0.5635(4) 0.0463(5) 0.7705(4) 0.0254(13) Uani 1 1 d . . . C7 C 0.5288(4) 0.1294(5) 0.6826(4) 0.0282(14) Uani 1 1 d . . . H7 H 0.5652 0.1305 0.6217 0.034 Uiso 1 1 calc . . . C8 C 0.4440(5) 0.2093(5) 0.6817(4) 0.0305(15) Uani 1 1 d . . . H8 H 0.4223 0.2657 0.6204 0.037 Uiso 1 1 calc . . . C9 C 0.3886(4) 0.2092(4) 0.7692(4) 0.0237(13) Uani 1 1 d . . . C10 C 0.4205(4) 0.1248(5) 0.8587(4) 0.0304(15) Uani 1 1 d . . . H10 H 0.3829 0.1226 0.9195 0.036 Uiso 1 1 calc . . . C11 C 0.5075(5) 0.0444(5) 0.8578(4) 0.0322(15) Uani 1 1 d . . . H11 H 0.5289 -0.0133 0.9186 0.039 Uiso 1 1 calc . . . C12 C 0.2981(4) 0.3013(5) 0.7700(4) 0.0301(15) Uani 1 1 d . . . H12A' H 0.3015 0.3631 0.7065 0.036 Uiso 1 1 calc . . . H12B' H 0.3017 0.3172 0.8234 0.036 Uiso 1 1 calc . . . C13 C 0.6964(4) 0.1916(4) 0.2508(4) 0.0249(13) Uani 1 1 d . . . H13A H 0.6989 0.1753 0.1959 0.030 Uiso 1 1 calc . . . H13B H 0.6949 0.1286 0.3137 0.030 Uiso 1 1 calc . . . C14 C 0.6033(4) 0.2801(4) 0.2506(4) 0.0239(13) Uani 1 1 d . . . C15 C 0.5678(4) 0.3616(5) 0.1613(4) 0.0258(13) Uani 1 1 d . . . H15 H 0.6007 0.3595 0.1005 0.031 Uiso 1 1 calc . . . C16 C 0.4841(4) 0.4458(4) 0.1616(4) 0.0261(14) Uani 1 1 d . . . H16 H 0.4623 0.5019 0.1002 0.031 Uiso 1 1 calc . . . C17 C 0.4320(4) 0.4505(4) 0.2477(4) 0.0228(13) Uani 1 1 d . . . C18 C 0.4668(4) 0.3691(5) 0.3362(4) 0.0280(14) Uani 1 1 d . . . H18 H 0.4323 0.3708 0.3968 0.034 Uiso 1 1 calc . . . C19 C 0.5507(4) 0.2852(5) 0.3382(4) 0.0287(14) Uani 1 1 d . . . H19 H 0.5729 0.2303 0.3999 0.034 Uiso 1 1 calc . . . C20 C 0.3418(4) 0.5403(5) 0.2468(4) 0.0292(14) Uani 1 1 d . . . H20A H 0.3537 0.6059 0.1940 0.035 Uiso 1 1 calc . . . H20B H 0.3305 0.5439 0.3108 0.035 Uiso 1 1 calc . . . C21 C 0.6779(4) -0.1786(4) 0.5152(4) 0.0265(14) Uani 1 1 d . . . H21A H 0.6860 -0.1951 0.4590 0.032 Uiso 1 1 calc . . . H21B H 0.6695 -0.2402 0.5770 0.032 Uiso 1 1 calc . . . C22 C 0.5850(4) -0.0864(4) 0.5070(4) 0.0254(13) Uani 1 1 d . . . C23 C 0.5522(4) -0.0120(5) 0.4149(4) 0.0257(14) Uani 1 1 d . . . H23 H 0.5872 -0.0192 0.3566 0.031 Uiso 1 1 calc . . . C24 C 0.4676(5) 0.0734(5) 0.4092(4) 0.0295(14) Uani 1 1 d . . . H24 H 0.4451 0.1242 0.3462 0.035 Uiso 1 1 calc . . . C25S C 0.5943(5) 0.6469(6) 0.0105(5) 0.0397(17) Uani 1 1 d . . . C26S C 0.5503(6) 0.6604(6) 0.0977(5) 0.0473(19) Uani 1 1 d . . . H26S H 0.5770 0.6099 0.1589 0.057 Uiso 1 1 calc . . . C27S C 0.4674(6) 0.7479(7) 0.0942(7) 0.062(2) Uani 1 1 d . . . H27S H 0.4378 0.7545 0.1539 0.075 Uiso 1 1 calc . . . C28S C 0.4285(6) 0.8231(7) 0.0083(7) 0.062(2) Uani 1 1 d . . . H28S H 0.3730 0.8822 0.0077 0.074 Uiso 1 1 calc . . . C29S C 0.4703(6) 0.8131(7) -0.0784(6) 0.061(2) Uani 1 1 d . . . H29S H 0.4429 0.8655 -0.1388 0.073 Uiso 1 1 calc . . . C30S C 0.5543(6) 0.7247(6) -0.0780(5) 0.049(2) Uani 1 1 d . . . H30S H 0.5829 0.7191 -0.1382 0.059 Uiso 1 1 calc . . . O1 O 0.7937(3) 0.4512(3) 0.4150(3) 0.0273(9) Uani 1 1 d . . . O2 O 0.7807(3) 0.3642(3) 0.5929(3) 0.0273(9) Uani 1 1 d . . . O3 O 0.8748(3) 0.2647(3) 0.4978(3) 0.0283(10) Uani 1 1 d . . . O4 O 0.7707(3) 0.0813(4) 0.6944(3) 0.0435(12) Uani 1 1 d . . . O5 O 0.7530(3) -0.0091(4) 0.8737(3) 0.0405(12) Uani 1 1 d . . . O6 O 0.8519(3) -0.1058(4) 0.7773(3) 0.0456(13) Uani 1 1 d . . . O7 O 0.1802(3) 0.1864(3) 0.8791(3) 0.0308(10) Uani 1 1 d . . . O8 O 0.1753(3) 0.2690(3) 0.7019(3) 0.0326(10) Uani 1 1 d . . . O9 O 0.1050(3) 0.3749(3) 0.7948(3) 0.0323(10) Uani 1 1 d . . . O10 O 0.8911(3) 0.1332(3) 0.2426(3) 0.0355(11) Uani 1 1 d . . . O11 O 0.8071(3) 0.3146(3) 0.1405(3) 0.0299(10) Uani 1 1 d . . . O12 O 0.7950(3) 0.2530(3) 0.3180(3) 0.0296(10) Uani 1 1 d . . . O14 O 0.2237(3) 0.4269(3) 0.3010(3) 0.0335(10) Uani 1 1 d . . . O15 O 0.2495(3) 0.5392(3) 0.1261(3) 0.0364(11) Uani 1 1 d . . . O16 O 0.1484(3) 0.6166(3) 0.2371(3) 0.0381(11) Uani 1 1 d . . . O17 O 0.7944(3) -0.0606(3) 0.4249(3) 0.0260(9) Uani 1 1 d . . . O18 O 0.7769(3) -0.1375(3) 0.6025(3) 0.0255(9) Uani 1 1 d . . . O19 O 0.8702(3) -0.2470(3) 0.5172(3) 0.0293(10) Uani 1 1 d . . . O20S O 0.7904(3) 0.4639(3) 0.2308(3) 0.0412(12) Uani 1 1 d . . . O21S O 0.8248(3) -0.3250(3) 0.7843(3) 0.0435(12) Uani 1 1 d . . . O22S O 0.8401(4) 0.1769(4) 0.7799(3) 0.0602(15) Uani 1 1 d . . . O23S O 0.8166(4) -0.0573(4) 0.2379(3) 0.0547(14) Uani 1 1 d . . . O24S O 0.9323(3) -0.2165(3) 0.9552(3) 0.0406(12) Uani 1 1 d . . . O25S O 0.1924(4) 0.7534(4) -0.0058(3) 0.0504(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0114(5) 0.0146(6) 0.0215(5) -0.0088(4) -0.0021(4) -0.0022(4) Co2 0.0215(6) 0.0203(6) 0.0210(5) -0.0093(5) -0.0008(4) -0.0085(5) Co3 0.0124(6) 0.0149(6) 0.0217(5) -0.0088(5) -0.0014(4) -0.0030(4) Co4 0.0166(6) 0.0205(6) 0.0216(5) -0.0095(5) -0.0026(4) -0.0059(5) S1 0.0145(7) 0.0198(8) 0.0263(7) -0.0130(6) -0.0015(5) -0.0035(6) S2 0.0193(8) 0.0437(10) 0.0280(8) -0.0183(8) 0.0004(6) -0.0057(7) S3 0.0201(8) 0.0224(8) 0.0275(8) -0.0050(7) -0.0075(6) -0.0062(7) S4 0.0220(8) 0.0217(8) 0.0304(8) -0.0092(7) -0.0078(6) -0.0041(7) S5 0.0184(8) 0.0350(9) 0.0270(8) -0.0148(7) -0.0004(6) -0.0054(7) S6 0.0141(7) 0.0181(8) 0.0294(8) -0.0116(6) -0.0028(6) -0.0032(6) N1 0.015(2) 0.014(2) 0.028(2) -0.007(2) -0.0044(19) -0.004(2) N2 0.017(3) 0.020(3) 0.026(2) -0.011(2) -0.0015(19) -0.004(2) N3 0.022(3) 0.022(3) 0.024(2) -0.008(2) -0.0049(19) -0.005(2) N4 0.033(3) 0.033(3) 0.041(3) -0.013(3) -0.007(2) -0.014(3) N5 0.040(3) 0.034(3) 0.033(3) -0.017(3) -0.005(2) -0.009(3) N6 0.027(3) 0.026(3) 0.030(3) -0.012(2) -0.004(2) 0.000(2) N7 0.016(3) 0.017(3) 0.028(2) -0.011(2) -0.0020(19) -0.005(2) N8 0.015(3) 0.025(3) 0.028(2) -0.014(2) -0.0012(19) -0.003(2) N9 0.013(2) 0.018(3) 0.028(2) -0.010(2) -0.0029(19) -0.001(2) N10 0.030(3) 0.030(3) 0.029(3) -0.012(2) -0.005(2) -0.008(2) N11 0.030(3) 0.032(3) 0.033(3) -0.013(2) -0.004(2) -0.010(2) N12 0.030(3) 0.028(3) 0.031(3) -0.014(2) -0.003(2) -0.011(2) N13S 0.039(4) 0.044(4) 0.052(3) -0.025(3) 0.000(3) -0.018(3) C1 0.017(3) 0.019(3) 0.032(3) -0.015(3) -0.006(2) 0.000(2) C2 0.016(3) 0.020(3) 0.027(3) -0.012(3) -0.003(2) -0.005(2) C3 0.019(3) 0.032(4) 0.020(3) -0.010(3) -0.002(2) -0.007(3) C4 0.013(3) 0.027(3) 0.021(3) -0.006(3) -0.003(2) 0.000(3) C5 0.021(3) 0.036(4) 0.043(4) -0.025(3) 0.007(3) -0.006(3) C6 0.018(3) 0.028(3) 0.037(3) -0.018(3) -0.002(3) -0.008(3) C7 0.026(4) 0.032(4) 0.024(3) -0.013(3) 0.001(2) -0.008(3) C8 0.028(4) 0.031(4) 0.030(3) -0.009(3) 0.000(3) -0.014(3) C9 0.020(3) 0.023(3) 0.031(3) -0.013(3) -0.007(2) -0.006(3) C10 0.027(4) 0.032(4) 0.027(3) -0.015(3) 0.000(3) -0.002(3) C11 0.030(4) 0.024(3) 0.034(3) -0.012(3) -0.006(3) 0.000(3) C12 0.022(3) 0.029(4) 0.043(4) -0.014(3) -0.006(3) -0.012(3) C13 0.018(3) 0.019(3) 0.039(3) -0.014(3) -0.004(2) -0.005(3) C14 0.022(3) 0.020(3) 0.031(3) -0.010(3) -0.008(2) -0.006(3) C15 0.018(3) 0.029(3) 0.033(3) -0.016(3) -0.003(2) -0.007(3) C16 0.020(3) 0.022(3) 0.035(3) -0.012(3) -0.005(3) -0.005(3) C17 0.019(3) 0.025(3) 0.031(3) -0.016(3) -0.005(2) -0.007(3) C18 0.023(3) 0.037(4) 0.029(3) -0.018(3) 0.003(2) -0.013(3) C19 0.027(4) 0.028(4) 0.030(3) -0.007(3) -0.003(3) -0.015(3) C20 0.021(3) 0.031(4) 0.041(3) -0.021(3) 0.005(3) -0.010(3) C21 0.017(3) 0.016(3) 0.043(3) -0.011(3) -0.006(3) -0.003(3) C22 0.016(3) 0.022(3) 0.042(3) -0.014(3) -0.002(3) -0.010(3) C23 0.017(3) 0.028(4) 0.030(3) -0.010(3) -0.003(2) -0.007(3) C24 0.027(4) 0.028(4) 0.030(3) -0.009(3) -0.006(3) -0.008(3) C25S 0.046(5) 0.050(5) 0.044(4) -0.025(4) 0.002(3) -0.032(4) C26S 0.054(5) 0.059(5) 0.043(4) -0.026(4) 0.003(3) -0.032(4) C27S 0.059(6) 0.074(6) 0.088(6) -0.060(5) 0.025(5) -0.042(5) C28S 0.049(5) 0.055(6) 0.096(7) -0.038(5) -0.003(5) -0.025(4) C29S 0.057(6) 0.056(6) 0.075(6) -0.022(5) -0.021(5) -0.022(5) C30S 0.058(5) 0.058(5) 0.046(4) -0.025(4) -0.003(4) -0.030(4) O1 0.023(2) 0.025(2) 0.031(2) -0.0068(19) -0.0046(17) -0.0103(19) O2 0.025(2) 0.036(3) 0.030(2) -0.022(2) 0.0000(17) -0.010(2) O3 0.016(2) 0.028(2) 0.039(2) -0.020(2) -0.0021(17) 0.0016(18) O4 0.034(3) 0.054(3) 0.033(2) -0.007(2) 0.0045(19) -0.024(2) O5 0.031(3) 0.059(3) 0.033(2) -0.030(2) -0.0013(19) -0.004(2) O6 0.021(2) 0.060(3) 0.045(3) -0.031(2) -0.002(2) 0.008(2) O7 0.028(2) 0.024(2) 0.032(2) -0.0039(19) -0.0063(18) -0.0079(19) O8 0.038(3) 0.033(3) 0.029(2) -0.009(2) -0.0149(19) -0.012(2) O9 0.020(2) 0.028(2) 0.040(2) -0.013(2) -0.0046(18) 0.0002(19) O10 0.023(2) 0.032(3) 0.048(3) -0.021(2) -0.0075(19) 0.003(2) O11 0.035(3) 0.024(2) 0.027(2) -0.0050(18) -0.0069(18) -0.010(2) O12 0.035(3) 0.030(2) 0.031(2) -0.0169(19) -0.0107(18) -0.007(2) O14 0.031(3) 0.037(3) 0.033(2) -0.011(2) -0.0003(18) -0.017(2) O15 0.030(3) 0.046(3) 0.027(2) -0.019(2) -0.0012(18) -0.003(2) O16 0.022(2) 0.044(3) 0.045(3) -0.028(2) -0.0031(19) 0.004(2) O17 0.026(2) 0.022(2) 0.029(2) -0.0064(18) -0.0035(17) -0.0118(18) O18 0.025(2) 0.028(2) 0.027(2) -0.0143(18) -0.0044(17) -0.0055(19) O19 0.016(2) 0.023(2) 0.045(2) -0.0195(19) -0.0008(18) 0.0019(18) O20S 0.059(3) 0.031(3) 0.034(2) -0.016(2) 0.008(2) -0.021(2) O21S 0.049(3) 0.037(3) 0.038(3) -0.005(2) -0.019(2) -0.013(2) O22S 0.084(4) 0.040(3) 0.056(3) -0.006(3) -0.039(3) -0.018(3) O23S 0.092(4) 0.053(3) 0.032(2) -0.024(2) 0.020(2) -0.045(3) O24S 0.043(3) 0.031(3) 0.043(3) -0.016(2) -0.008(2) -0.003(2) O25S 0.063(4) 0.041(3) 0.043(3) -0.024(2) -0.002(2) -0.006(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 Co1 N3 1.974(4) 2_766 ? Co1 N3 1.974(4) . ? Co1 N1 1.974(4) . ? Co1 N1 1.974(4) 2_766 ? Co1 N2 1.983(4) 2_766 ? Co1 N2 1.983(4) . ? Co2 N4 1.948(5) . ? Co2 N4 1.948(5) 2_757 ? Co2 N5 1.954(5) . ? Co2 N5 1.954(5) 2_757 ? Co2 N6 1.983(5) 2_757 ? Co2 N6 1.983(5) . ? Co3 N8 1.968(4) 2_756 ? Co3 N8 1.968(4) . ? Co3 N9 1.972(4) 2_756 ? Co3 N9 1.972(4) . ? Co3 N7 1.975(4) . ? Co3 N7 1.975(4) 2_756 ? Co4 N10 1.949(5) 2_747 ? Co4 N10 1.949(5) . ? Co4 N11 1.953(4) . ? Co4 N11 1.953(4) 2_747 ? Co4 N12 1.955(4) 2_747 ? Co4 N12 1.955(4) . ? S1 O3 1.450(4) . ? S1 O2 1.458(4) . ? S1 O1 1.471(4) . ? S1 C1 1.789(6) . ? S2 O5 1.457(4) . ? S2 O4 1.457(4) . ? S2 O6 1.471(4) . ? S2 C5 1.773(6) . ? S3 O9 1.461(4) . ? S3 O7 1.467(4) . ? S3 O8 1.471(4) . ? S3 C12 1.775(6) . ? S4 O10 1.454(4) . ? S4 O11 1.465(4) . ? S4 O12 1.470(4) . ? S4 C13 1.792(6) . ? S5 O15 1.455(4) . ? S5 O16 1.465(4) . ? S5 O14 1.472(4) . ? S5 C20 1.781(6) . ? S6 O19 1.448(4) . ? S6 O18 1.459(4) . ? S6 O17 1.463(4) . ? S6 C21 1.788(6) . ? N13S C25S 1.431(9) . ? C1 C2 1.497(7) . ? C2 C4 1.372(7) . ? C2 C3 1.387(7) . ? C3 C4 1.385(8) 2_666 ? C4 C3 1.385(8) 2_666 ? C5 C6 1.507(8) . ? C6 C11 1.379(8) . ? C6 C7 1.385(8) . ? C7 C8 1.358(8) . ? C8 C9 1.385(8) . ? C9 C10 1.398(8) . ? C9 C12 1.516(8) . ? C10 C11 1.385(8) . ? C13 C14 1.500(8) . ? C14 C15 1.394(7) . ? C14 C19 1.397(8) . ? C15 C16 1.391(8) . ? C16 C17 1.373(7) . ? C17 C18 1.384(8) . ? C17 C20 1.486(8) . ? C18 C19 1.382(8) . ? C21 C22 1.508(8) . ? C22 C23 1.388(7) . ? C22 C24 1.389(8) 2_656 ? C23 C24 1.390(8) . ? C24 C22 1.389(8) 2_656 ? C25S C30S 1.394(9) . ? C25S C26S 1.414(9) . ? C26S C27S 1.403(11) . ? C27S C28S 1.352(11) . ? C28S C29S 1.380(11) . ? C29S C30S 1.430(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 N3 180.0(4) 2_766 . ? N3 Co1 N1 88.47(18) 2_766 . ? N3 Co1 N1 91.53(18) . . ? N3 Co1 N1 91.53(18) 2_766 2_766 ? N3 Co1 N1 88.47(18) . 2_766 ? N1 Co1 N1 180.000(1) . 2_766 ? N3 Co1 N2 90.12(18) 2_766 2_766 ? N3 Co1 N2 89.88(18) . 2_766 ? N1 Co1 N2 90.02(17) . 2_766 ? N1 Co1 N2 89.98(17) 2_766 2_766 ? N3 Co1 N2 89.88(18) 2_766 . ? N3 Co1 N2 90.12(18) . . ? N1 Co1 N2 89.98(17) . . ? N1 Co1 N2 90.02(17) 2_766 . ? N2 Co1 N2 180.000(2) 2_766 . ? N4 Co2 N4 180.0(4) . 2_757 ? N4 Co2 N5 88.3(2) . . ? N4 Co2 N5 91.7(2) 2_757 . ? N4 Co2 N5 91.7(2) . 2_757 ? N4 Co2 N5 88.3(2) 2_757 2_757 ? N5 Co2 N5 180.000(1) . 2_757 ? N4 Co2 N6 88.6(2) . 2_757 ? N4 Co2 N6 91.4(2) 2_757 2_757 ? N5 Co2 N6 89.8(2) . 2_757 ? N5 Co2 N6 90.2(2) 2_757 2_757 ? N4 Co2 N6 91.4(2) . . ? N4 Co2 N6 88.6(2) 2_757 . ? N5 Co2 N6 90.2(2) . . ? N5 Co2 N6 89.8(2) 2_757 . ? N6 Co2 N6 180.0(3) 2_757 . ? N8 Co3 N8 180.00(8) 2_756 . ? N8 Co3 N9 90.86(18) 2_756 2_756 ? N8 Co3 N9 89.14(18) . 2_756 ? N8 Co3 N9 89.14(18) 2_756 . ? N8 Co3 N9 90.86(18) . . ? N9 Co3 N9 180.0(2) 2_756 . ? N8 Co3 N7 91.29(18) 2_756 . ? N8 Co3 N7 88.71(18) . . ? N9 Co3 N7 90.11(17) 2_756 . ? N9 Co3 N7 89.89(17) . . ? N8 Co3 N7 88.71(18) 2_756 2_756 ? N8 Co3 N7 91.29(18) . 2_756 ? N9 Co3 N7 89.89(17) 2_756 2_756 ? N9 Co3 N7 90.11(17) . 2_756 ? N7 Co3 N7 180.0(3) . 2_756 ? N10 Co4 N10 180.0(3) 2_747 . ? N10 Co4 N11 92.6(2) 2_747 . ? N10 Co4 N11 87.4(2) . . ? N10 Co4 N11 87.4(2) 2_747 2_747 ? N10 Co4 N11 92.6(2) . 2_747 ? N11 Co4 N11 180.000(1) . 2_747 ? N10 Co4 N12 88.6(2) 2_747 2_747 ? N10 Co4 N12 91.4(2) . 2_747 ? N11 Co4 N12 89.35(19) . 2_747 ? N11 Co4 N12 90.7(2) 2_747 2_747 ? N10 Co4 N12 91.4(2) 2_747 . ? N10 Co4 N12 88.6(2) . . ? N11 Co4 N12 90.7(2) . . ? N11 Co4 N12 89.3(2) 2_747 . ? N12 Co4 N12 180.000(1) 2_747 . ? O3 S1 O2 113.5(2) . . ? O3 S1 O1 112.0(2) . . ? O2 S1 O1 110.5(2) . . ? O3 S1 C1 106.3(3) . . ? O2 S1 C1 106.7(2) . . ? O1 S1 C1 107.5(2) . . ? O5 S2 O4 112.9(3) . . ? O5 S2 O6 112.0(3) . . ? O4 S2 O6 112.0(3) . . ? O5 S2 C5 108.6(3) . . ? O4 S2 C5 105.8(3) . . ? O6 S2 C5 104.9(3) . . ? O9 S3 O7 112.5(2) . . ? O9 S3 O8 113.4(2) . . ? O7 S3 O8 110.5(2) . . ? O9 S3 C12 105.8(3) . . ? O7 S3 C12 107.7(3) . . ? O8 S3 C12 106.5(3) . . ? O10 S4 O11 112.1(2) . . ? O10 S4 O12 113.2(2) . . ? O11 S4 O12 111.2(2) . . ? O10 S4 C13 106.2(3) . . ? O11 S4 C13 107.0(2) . . ? O12 S4 C13 106.6(3) . . ? O15 S5 O16 111.8(2) . . ? O15 S5 O14 112.3(3) . . ? O16 S5 O14 112.7(3) . . ? O15 S5 C20 106.0(3) . . ? O16 S5 C20 106.4(3) . . ? O14 S5 C20 107.1(3) . . ? O19 S6 O18 113.2(2) . . ? O19 S6 O17 112.9(2) . . ? O18 S6 O17 110.6(2) . . ? O19 S6 C21 105.3(3) . . ? O18 S6 C21 107.8(3) . . ? O17 S6 C21 106.6(2) . . ? C2 C1 S1 112.9(4) . . ? C4 C2 C3 117.9(5) . . ? C4 C2 C1 121.1(5) . . ? C3 C2 C1 121.0(5) . . ? C4 C3 C2 120.8(5) 2_666 . ? C2 C4 C3 121.3(5) . 2_666 ? C6 C5 S2 113.4(5) . . ? C11 C6 C7 118.3(5) . . ? C11 C6 C5 120.0(5) . . ? C7 C6 C5 121.7(5) . . ? C8 C7 C6 121.4(5) . . ? C7 C8 C9 120.7(5) . . ? C8 C9 C10 119.0(5) . . ? C8 C9 C12 121.4(5) . . ? C10 C9 C12 119.5(5) . . ? C11 C10 C9 119.2(5) . . ? C6 C11 C10 121.4(5) . . ? C9 C12 S3 114.6(4) . . ? C14 C13 S4 110.6(4) . . ? C15 C14 C19 117.9(5) . . ? C15 C14 C13 120.2(5) . . ? C19 C14 C13 121.8(5) . . ? C16 C15 C14 119.9(5) . . ? C17 C16 C15 122.2(5) . . ? C16 C17 C18 117.8(5) . . ? C16 C17 C20 121.5(5) . . ? C18 C17 C20 120.7(5) . . ? C19 C18 C17 121.3(5) . . ? C18 C19 C14 120.9(5) . . ? C17 C20 S5 112.0(4) . . ? C22 C21 S6 112.5(4) . . ? C23 C22 C24 119.1(5) . 2_656 ? C23 C22 C21 120.2(5) . . ? C24 C22 C21 120.7(5) 2_656 . ? C22 C23 C24 119.1(5) . . ? C22 C24 C23 121.8(5) 2_656 . ? C30S C25S C26S 117.6(7) . . ? C30S C25S N13S 121.0(6) . . ? C26S C25S N13S 121.4(6) . . ? C27S C26S C25S 120.4(7) . . ? C28S C27S C26S 121.8(8) . . ? C27S C28S C29S 119.4(8) . . ? C28S C29S C30S 120.6(7) . . ? C25S C30S C29S 120.2(7) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 C1 C2 -176.0(4) . . . . ? O2 S1 C1 C2 62.6(4) . . . . ? O1 S1 C1 C2 -56.0(4) . . . . ? S1 C1 C2 C4 -89.6(6) . . . . ? S1 C1 C2 C3 89.5(6) . . . . ? C4 C2 C3 C4 1.0(10) . . . 2_666 ? C1 C2 C3 C4 -178.1(6) . . . 2_666 ? C3 C2 C4 C3 -1.0(10) . . . 2_666 ? C1 C2 C4 C3 178.1(6) . . . 2_666 ? O5 S2 C5 C6 62.4(5) . . . . ? O4 S2 C5 C6 -59.0(5) . . . . ? O6 S2 C5 C6 -177.7(4) . . . . ? S2 C5 C6 C11 -89.2(6) . . . . ? S2 C5 C6 C7 90.3(6) . . . . ? C11 C6 C7 C8 2.5(9) . . . . ? C5 C6 C7 C8 -177.1(6) . . . . ? C6 C7 C8 C9 -0.9(10) . . . . ? C7 C8 C9 C10 -1.0(9) . . . . ? C7 C8 C9 C12 175.4(6) . . . . ? C8 C9 C10 C11 1.2(9) . . . . ? C12 C9 C10 C11 -175.3(6) . . . . ? C7 C6 C11 C10 -2.3(10) . . . . ? C5 C6 C11 C10 177.3(6) . . . . ? C9 C10 C11 C6 0.5(10) . . . . ? C8 C9 C12 S3 103.3(6) . . . . ? C10 C9 C12 S3 -80.3(6) . . . . ? O9 S3 C12 C9 175.3(4) . . . . ? O7 S3 C12 C9 54.7(5) . . . . ? O8 S3 C12 C9 -63.8(5) . . . . ? O10 S4 C13 C14 177.6(4) . . . . ? O11 S4 C13 C14 -62.5(4) . . . . ? O12 S4 C13 C14 56.6(4) . . . . ? S4 C13 C14 C15 84.2(6) . . . . ? S4 C13 C14 C19 -94.5(6) . . . . ? C19 C14 C15 C16 1.8(9) . . . . ? C13 C14 C15 C16 -177.0(5) . . . . ? C14 C15 C16 C17 -2.3(9) . . . . ? C15 C16 C17 C18 1.6(9) . . . . ? C15 C16 C17 C20 -179.1(6) . . . . ? C16 C17 C18 C19 -0.5(9) . . . . ? C20 C17 C18 C19 -179.8(6) . . . . ? C17 C18 C19 C14 0.1(9) . . . . ? C15 C14 C19 C18 -0.7(9) . . . . ? C13 C14 C19 C18 178.0(6) . . . . ? C16 C17 C20 S5 80.3(6) . . . . ? C18 C17 C20 S5 -100.3(6) . . . . ? O15 S5 C20 C17 -66.4(5) . . . . ? O16 S5 C20 C17 174.4(4) . . . . ? O14 S5 C20 C17 53.7(5) . . . . ? O19 S6 C21 C22 -176.4(4) . . . . ? O18 S6 C21 C22 62.5(5) . . . . ? O17 S6 C21 C22 -56.3(5) . . . . ? S6 C21 C22 C23 92.4(6) . . . . ? S6 C21 C22 C24 -86.0(6) . . . 2_656 ? C24 C22 C23 C24 -0.2(10) 2_656 . . . ? C21 C22 C23 C24 -178.6(6) . . . . ? C22 C23 C24 C22 0.2(10) . . . 2_656 ? C30S C25S C26S C27S 1.9(10) . . . . ? N13S C25S C26S C27S 179.1(6) . . . . ? C25S C26S C27S C28S -1.8(12) . . . . ? C26S C27S C28S C29S 1.0(12) . . . . ? C27S C28S C29S C30S -0.4(12) . . . . ? C26S C25S C30S C29S -1.4(10) . . . . ? N13S C25S C30S C29S -178.6(7) . . . . ? C28S C29S C30S C25S 0.7(12) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.029 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.294