# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Stuart Batten' _publ_contact_author_email STUART.BATTEN@SCI.MONASH.EDU.AU _publ_section_title ; Variable length ligands: a new class of bridging ligands for supramolecular chemistry and crystal engineering ; loop_ _publ_author_name 'Stuart Batten' 'Martin B. Duriska' 'Suzanne M. Neville' # Attachment 'combined.CIF' #========================================================================== data_A _database_code_depnum_ccdc_archive 'CCDC 735051' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H36 Cl2 Co N4 O4, C H4 O' _chemical_formula_sum 'C25 H40 Cl2 Co N4 O5' _chemical_formula_weight 606.44 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' Cl Cl 0.1484 0.1585 '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 P21/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 10.0871(2) _cell_length_b 16.8016(3) _cell_length_c 17.4116(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.383(1) _cell_angle_gamma 90.00 _cell_volume 2845.19(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 111 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 30.81 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7737 _exptl_absorpt_correction_T_max 0.9031 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 69715 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 30.98 _reflns_number_total 9006 _reflns_number_gt 7732 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _computing_structure_refinement X-SEED _computing_molecular_graphics 'MERCURY 1.4 (Bruno et al., 2002)' _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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^)+(0.0698P)^2^+3.4658P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9006 _refine_ls_number_parameters 324 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1636 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.136 _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 0.27915(4) 0.73330(2) 0.301654(19) 0.02509(10) Uani 1 1 d . . . Cl1 Cl 0.49054(7) 0.74823(4) 0.28650(4) 0.02837(14) Uani 1 1 d . . . O1 O 0.28769(18) 0.49870(10) 0.57330(10) 0.0241(3) Uani 1 1 d . . . N1 N 0.3047(2) 0.35765(12) 0.47772(11) 0.0215(4) Uani 1 1 d . . . C1 C 0.2327(3) 0.57653(15) 0.57257(16) 0.0284(5) Uani 1 1 d . . . H1A H 0.1668 0.5777 0.6057 0.034 Uiso 1 1 calc R . . H1B H 0.1824 0.5911 0.5174 0.034 Uiso 1 1 calc R . . Cl2 Cl 0.09880(8) 0.75990(5) 0.19771(4) 0.04028(18) Uani 1 1 d . . . O2 O 0.57759(18) 0.35023(10) 0.45201(10) 0.0242(3) Uani 1 1 d . . . N2 N 0.2559(2) 0.61770(12) 0.32998(11) 0.0228(4) Uani 1 1 d . . . C2 C 0.1812(3) 0.44113(16) 0.55354(15) 0.0270(5) Uani 1 1 d . . . H2A H 0.1133 0.4567 0.5035 0.032 Uiso 1 1 calc R . . H2B H 0.1333 0.4386 0.5963 0.032 Uiso 1 1 calc R . . O3 O 0.2559(2) 1.08012(12) 0.45195(11) 0.0320(4) Uani 1 1 d . . . N3 N 0.2725(2) 0.79718(13) 0.39928(12) 0.0256(4) Uani 1 1 d . . . C3 C 0.2402(3) 0.36015(15) 0.54332(15) 0.0254(5) Uani 1 1 d . . . H3A H 0.3091 0.3455 0.5933 0.030 Uiso 1 1 calc R . . H3B H 0.1655 0.3201 0.5337 0.030 Uiso 1 1 calc R . . O4 O 0.6250(2) 0.97575(11) 0.67104(11) 0.0318(4) Uani 1 1 d . . . N4 N 0.3320(2) 1.00767(13) 0.61478(13) 0.0283(4) Uani 1 1 d . . . C4 C 0.3817(3) 0.28435(14) 0.47708(15) 0.0257(5) Uani 1 1 d . . . H4A H 0.3163 0.2401 0.4584 0.031 Uiso 1 1 calc R . . H4B H 0.4356 0.2719 0.5321 0.031 Uiso 1 1 calc R . . O5 O -0.1462(10) 0.7699(6) 0.3040(5) 0.200 Uiso 1 1 d D . . H5 H -0.1197 0.7307 0.2820 0.200 Uiso 1 1 calc . . . C5 C 0.4780(3) 0.29019(15) 0.42386(15) 0.0271(5) Uani 1 1 d . . . H5A H 0.5245 0.2384 0.4231 0.033 Uiso 1 1 calc R . . H5B H 0.4248 0.3028 0.3688 0.033 Uiso 1 1 calc R . . C6 C 0.6547(3) 0.36417(16) 0.39592(15) 0.0282(5) Uani 1 1 d . . . H6A H 0.5930 0.3844 0.3457 0.034 Uiso 1 1 calc R . . H6B H 0.6953 0.3135 0.3841 0.034 Uiso 1 1 calc R . . C7 C 0.2083(3) 0.37661(15) 0.40139(14) 0.0256(5) Uani 1 1 d . . . H7A H 0.1132 0.3687 0.4055 0.031 Uiso 1 1 calc R . . H7B H 0.2235 0.3398 0.3602 0.031 Uiso 1 1 calc R . . C8 C 0.2246(2) 0.46112(14) 0.37636(13) 0.0204(4) Uani 1 1 d . . . C9 C 0.3496(2) 0.50034(13) 0.40195(13) 0.0203(4) Uani 1 1 d . . . H9 H 0.4266 0.4741 0.4358 0.024 Uiso 1 1 calc R . . C10 C 0.3612(2) 0.57770(14) 0.37782(13) 0.0210(4) Uani 1 1 d . . . H10 H 0.4474 0.6038 0.3958 0.025 Uiso 1 1 calc R . . C11 C 0.1355(3) 0.57960(16) 0.30413(15) 0.0286(5) Uani 1 1 d . . . H11 H 0.0607 0.6070 0.2696 0.034 Uiso 1 1 calc R . . C12 C 0.1156(3) 0.50229(16) 0.32548(15) 0.0268(5) Uani 1 1 d . . . H12 H 0.0287 0.4773 0.3058 0.032 Uiso 1 1 calc R . . C13 C 0.3540(3) 0.86074(15) 0.42243(15) 0.0287(5) Uani 1 1 d . . . H13 H 0.4159 0.8752 0.3920 0.034 Uiso 1 1 calc R . . C14 C 0.3524(3) 0.90611(15) 0.48823(16) 0.0290(5) Uani 1 1 d . . . H14 H 0.4122 0.9505 0.5026 0.035 Uiso 1 1 calc R . . C15 C 0.2622(3) 0.88616(15) 0.53311(15) 0.0256(5) Uani 1 1 d . . . C16 C 0.1783(3) 0.81994(16) 0.50965(15) 0.0267(5) Uani 1 1 d . . . H16 H 0.1158 0.8042 0.5391 0.032 Uiso 1 1 calc R . . C17 C 0.1865(3) 0.77741(15) 0.44337(16) 0.0280(5) Uani 1 1 d . . . H17 H 0.1289 0.7322 0.4282 0.034 Uiso 1 1 calc R . . C18 C 0.2579(3) 0.93246(18) 0.60683(16) 0.0340(6) Uani 1 1 d . . . H18A H 0.1608 0.9432 0.6054 0.041 Uiso 1 1 calc R . . H18B H 0.2978 0.8993 0.6544 0.041 Uiso 1 1 calc R . . C19 C 0.1838(3) 1.0721(2) 0.37107(19) 0.0433(7) Uani 1 1 d . . . H19A H 0.1070 1.1107 0.3577 0.052 Uiso 1 1 calc R . . H19B H 0.1447 1.0178 0.3614 0.052 Uiso 1 1 calc R . . C20 C 0.1646(3) 1.0719(2) 0.5007(2) 0.0415(7) Uani 1 1 d . . . H20A H 0.1159 1.0203 0.4896 0.050 Uiso 1 1 calc R . . H20B H 0.0951 1.1149 0.4883 0.050 Uiso 1 1 calc R . . C21 C 0.2423(3) 1.07599(19) 0.58746(19) 0.0388(7) Uani 1 1 d . . . H21A H 0.2987 1.1251 0.5966 0.047 Uiso 1 1 calc R . . H21B H 0.1754 1.0798 0.6199 0.047 Uiso 1 1 calc R . . C22 C 0.4170(3) 1.02159(16) 0.69601(15) 0.0322(6) Uani 1 1 d . . . H22A H 0.3588 1.0167 0.7335 0.039 Uiso 1 1 calc R . . H22B H 0.4532 1.0766 0.6999 0.039 Uiso 1 1 calc R . . C23 C 0.5351(3) 0.96481(17) 0.72053(15) 0.0347(6) Uani 1 1 d . . . H23A H 0.5853 0.9744 0.7768 0.042 Uiso 1 1 calc R . . H23B H 0.5004 0.9094 0.7157 0.042 Uiso 1 1 calc R . . C24 C 0.7222(3) 0.91350(19) 0.68058(17) 0.0399(7) Uani 1 1 d . . . H24A H 0.6739 0.8621 0.6661 0.048 Uiso 1 1 calc R . . H24B H 0.7762 0.9105 0.7370 0.048 Uiso 1 1 calc R . . C25 C -0.0625(13) 0.8415(8) 0.2961(7) 0.200 Uiso 1 1 d D . . H25A H -0.1161 0.8761 0.2539 0.300 Uiso 1 1 calc R . . H25B H 0.0216 0.8246 0.2827 0.300 Uiso 1 1 calc R . . H25C H -0.0382 0.8707 0.3466 0.300 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 0.0368(2) 0.02044(17) 0.01769(16) 0.00347(11) 0.00674(13) 0.00466(13) Cl1 0.0385(3) 0.0238(3) 0.0241(3) 0.0028(2) 0.0105(2) 0.0033(2) O1 0.0228(8) 0.0238(8) 0.0250(8) -0.0022(6) 0.0049(6) 0.0026(6) N1 0.0262(10) 0.0182(9) 0.0181(8) 0.0012(6) 0.0025(7) -0.0008(7) C1 0.0277(12) 0.0276(12) 0.0317(13) -0.0011(9) 0.0110(10) 0.0082(9) Cl2 0.0438(4) 0.0422(4) 0.0288(3) 0.0133(3) -0.0010(3) 0.0070(3) O2 0.0295(9) 0.0226(8) 0.0200(8) -0.0035(6) 0.0057(7) 0.0016(6) N2 0.0282(10) 0.0226(9) 0.0167(8) 0.0013(7) 0.0041(7) 0.0034(7) C2 0.0232(12) 0.0321(13) 0.0270(11) -0.0003(9) 0.0091(9) -0.0018(9) O3 0.0261(9) 0.0363(10) 0.0309(10) 0.0028(8) 0.0031(7) 0.0052(7) N3 0.0330(11) 0.0221(10) 0.0228(9) 0.0033(7) 0.0091(8) 0.0065(8) C3 0.0257(12) 0.0260(11) 0.0249(11) 0.0017(9) 0.0075(9) -0.0057(9) O4 0.0414(11) 0.0276(9) 0.0264(9) 0.0066(7) 0.0086(8) -0.0004(8) N4 0.0353(12) 0.0278(11) 0.0249(10) -0.0030(8) 0.0136(9) -0.0042(9) C4 0.0334(13) 0.0172(10) 0.0249(11) -0.0005(8) 0.0051(9) -0.0006(9) C5 0.0362(14) 0.0187(11) 0.0255(11) -0.0055(8) 0.0067(10) 0.0006(9) C6 0.0353(14) 0.0262(12) 0.0247(11) -0.0032(9) 0.0109(10) 0.0029(10) C7 0.0270(12) 0.0250(11) 0.0207(10) -0.0004(8) -0.0006(9) -0.0047(9) C8 0.0225(11) 0.0227(10) 0.0146(9) -0.0009(7) 0.0027(8) -0.0009(8) C9 0.0230(11) 0.0204(10) 0.0158(9) 0.0009(7) 0.0020(8) 0.0019(8) C10 0.0248(11) 0.0213(10) 0.0159(9) -0.0008(7) 0.0036(8) -0.0006(8) C11 0.0253(12) 0.0315(13) 0.0243(11) 0.0066(9) -0.0017(9) 0.0048(9) C12 0.0217(11) 0.0314(13) 0.0234(11) 0.0028(9) -0.0009(9) -0.0015(9) C13 0.0417(15) 0.0222(11) 0.0276(12) 0.0027(9) 0.0187(11) 0.0010(10) C14 0.0383(14) 0.0217(11) 0.0318(13) -0.0020(9) 0.0177(11) -0.0033(10) C15 0.0291(12) 0.0250(11) 0.0241(11) -0.0002(9) 0.0096(9) 0.0005(9) C16 0.0256(12) 0.0286(12) 0.0275(12) 0.0017(9) 0.0099(10) -0.0013(9) C17 0.0302(13) 0.0254(12) 0.0282(12) 0.0003(9) 0.0072(10) -0.0020(9) C18 0.0421(16) 0.0371(15) 0.0288(13) -0.0079(10) 0.0197(12) -0.0130(12) C19 0.0322(15) 0.0510(19) 0.0381(16) 0.0001(13) -0.0059(12) 0.0089(13) C20 0.0248(13) 0.0497(18) 0.0493(18) -0.0020(14) 0.0087(12) 0.0075(12) C21 0.0381(16) 0.0404(16) 0.0430(16) -0.0044(12) 0.0196(13) 0.0058(12) C22 0.0514(17) 0.0283(13) 0.0217(11) -0.0044(9) 0.0182(11) -0.0089(11) C23 0.0559(18) 0.0297(13) 0.0182(11) 0.0026(9) 0.0092(11) -0.0087(12) C24 0.0503(18) 0.0361(15) 0.0243(12) 0.0066(10) -0.0061(12) 0.0073(13) _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 2.026(2) . ? Co1 N2 2.033(2) . ? Co1 Cl1 2.2310(8) . ? Co1 Cl2 2.2445(8) . ? O1 C2 1.418(3) . ? O1 C1 1.419(3) . ? N1 C4 1.457(3) . ? N1 C3 1.458(3) . ? N1 C7 1.459(3) . ? C1 C6 1.501(4) 3_666 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C5 1.416(3) . ? O2 C6 1.420(3) . ? N2 C11 1.341(3) . ? N2 C10 1.343(3) . ? C2 C3 1.514(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C19 1.410(4) . ? O3 C20 1.415(4) . ? N3 C13 1.343(3) . ? N3 C17 1.344(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C24 1.413(4) . ? O4 C23 1.419(3) . ? N4 C18 1.456(3) . ? N4 C21 1.461(4) . ? N4 C22 1.465(3) . ? C4 C5 1.514(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O5 C25 1.497(11) . ? O5 H5 0.8400 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C1 1.501(4) 3_666 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.507(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.387(3) . ? C8 C12 1.398(3) . ? C9 C10 1.381(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.380(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.380(4) . ? C13 H13 0.9500 . ? C14 C15 1.388(4) . ? C14 H14 0.9500 . ? C15 C16 1.392(4) . ? C15 C18 1.511(4) . ? C16 C17 1.378(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.490(5) 3_676 ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.508(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.497(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C19 1.490(5) 3_676 ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 N2 105.72(8) . . ? N3 Co1 Cl1 106.57(7) . . ? N2 Co1 Cl1 108.14(6) . . ? N3 Co1 Cl2 111.76(7) . . ? N2 Co1 Cl2 105.36(6) . . ? Cl1 Co1 Cl2 118.55(3) . . ? C2 O1 C1 110.93(19) . . ? C4 N1 C3 112.33(19) . . ? C4 N1 C7 113.91(19) . . ? C3 N1 C7 112.3(2) . . ? O1 C1 C6 110.6(2) . 3_666 ? O1 C1 H1A 109.5 . . ? C6 C1 H1A 109.5 3_666 . ? O1 C1 H1B 109.5 . . ? C6 C1 H1B 109.5 3_666 . ? H1A C1 H1B 108.1 . . ? C5 O2 C6 110.31(18) . . ? C11 N2 C10 117.8(2) . . ? C11 N2 Co1 121.82(16) . . ? C10 N2 Co1 120.38(16) . . ? O1 C2 C3 110.2(2) . . ? O1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? O1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C19 O3 C20 110.1(2) . . ? C13 N3 C17 117.5(2) . . ? C13 N3 Co1 121.25(17) . . ? C17 N3 Co1 121.23(18) . . ? N1 C3 C2 112.9(2) . . ? N1 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? N1 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C24 O4 C23 111.6(2) . . ? C18 N4 C21 113.1(2) . . ? C18 N4 C22 112.6(2) . . ? C21 N4 C22 110.0(2) . . ? N1 C4 C5 112.3(2) . . ? N1 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N1 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? C25 O5 H5 109.5 . . ? O2 C5 C4 110.24(19) . . ? O2 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? O2 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? O2 C6 C1 110.9(2) . 3_666 ? O2 C6 H6A 109.5 . . ? C1 C6 H6A 109.5 3_666 . ? O2 C6 H6B 109.5 . . ? C1 C6 H6B 109.5 3_666 . ? H6A C6 H6B 108.0 . . ? N1 C7 C8 111.83(19) . . ? N1 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C12 117.6(2) . . ? C9 C8 C7 120.9(2) . . ? C12 C8 C7 121.5(2) . . ? C10 C9 C8 119.5(2) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N2 C10 C9 122.9(2) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C12 122.9(2) . . ? N2 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C8 119.3(2) . . ? C11 C12 H12 120.3 . . ? C8 C12 H12 120.3 . . ? N3 C13 C14 123.2(2) . . ? N3 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C15 119.2(2) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 117.8(2) . . ? C14 C15 C18 121.6(2) . . ? C16 C15 C18 120.5(2) . . ? C17 C16 C15 119.5(2) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? N3 C17 C16 122.8(2) . . ? N3 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? N4 C18 C15 113.4(2) . . ? N4 C18 H18A 108.9 . . ? C15 C18 H18A 108.9 . . ? N4 C18 H18B 108.9 . . ? C15 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O3 C19 C24 110.2(3) . 3_676 ? O3 C19 H19A 109.6 . . ? C24 C19 H19A 109.6 3_676 . ? O3 C19 H19B 109.6 . . ? C24 C19 H19B 109.6 3_676 . ? H19A C19 H19B 108.1 . . ? O3 C20 C21 110.4(2) . . ? O3 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? O3 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? N4 C21 C20 113.8(2) . . ? N4 C21 H21A 108.8 . . ? C20 C21 H21A 108.8 . . ? N4 C21 H21B 108.8 . . ? C20 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? N4 C22 C23 113.0(2) . . ? N4 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? N4 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? O4 C23 C22 109.4(2) . . ? O4 C23 H23A 109.8 . . ? C22 C23 H23A 109.8 . . ? O4 C23 H23B 109.8 . . ? C22 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? O4 C24 C19 109.9(2) . 3_676 ? O4 C24 H24A 109.7 . . ? C19 C24 H24A 109.7 3_676 . ? O4 C24 H24B 109.7 . . ? C19 C24 H24B 109.7 3_676 . ? H24A C24 H24B 108.2 . . ? O5 C25 H25A 109.5 . . ? O5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.549 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.095 #===END #========================================================================== data_B _database_code_depnum_ccdc_archive 'CCDC 735052' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C50 H74 Fe N10 O8 S2, 2(Cl O4), 2(H2 O), C H4 O ; _chemical_formula_sum 'C51 H82 Cl2 Fe N10 O19 S2' _chemical_formula_weight 1330.14 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.2580(6) _cell_length_b 16.8765(7) _cell_length_c 25.9883(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.679(1) _cell_angle_gamma 90.00 _cell_volume 6181.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 111 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 31.95 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7714 _exptl_absorpt_correction_T_max 0.9108 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29767 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 32.00 _reflns_number_total 10736 _reflns_number_gt 8335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _computing_structure_refinement X-SEED _computing_molecular_graphics 'MERCURY 1.4 (Bruno et al., 2002)' _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. There is one perchlorate anion in the asym unit which is disordered over two sites (40:60 ratio free variable), is was refined anisotropically. The hydrogen atoms on the water molecule were located in the difference map but their bond lengths were fixed to 0.95. There is also a methanol solvent molecule, the carbon atom is disordered over two sites by symmetry, thus the hydrogen atoms were not attached. Extra hydrogen bonding details, lengths and angles: N(2)...O(1): 2.778(2) A, N(2)-H(N2)...O(1): 159.1(3)deg, O(1)...O(3): 2.867(2) A, O(1)-H(O1)...O(3): 173.4(3)deg, O(1)...O(4): 2.826(2) A, O(1)-H(O1)...O(4): 170.2(3)deg. ; _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^)+(0.0749P)^2^+9.9820P] 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 10736 _refine_ls_number_parameters 426 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1673 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.077 _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 Fe1 Fe 0.0000 0.05952(2) 0.2500 0.01670(9) Uani 1 2 d S . . Cl1 Cl -0.36587(14) -0.02286(14) 0.10609(14) 0.0393(4) Uani 0.668(9) 1 d P A 2 S1 S 0.26734(5) 0.13508(4) 0.17214(3) 0.03482(15) Uani 1 1 d . . . O1 O 0.15990(11) -0.21467(10) 0.05918(6) 0.0255(3) Uani 1 1 d D . . N1 N 0.45714(12) -0.34592(10) 0.19231(7) 0.0208(3) Uani 1 1 d . . . C1 C 0.34618(14) -0.29232(13) 0.12286(8) 0.0224(4) Uani 1 1 d . . . H1 H 0.2860 -0.2958 0.1016 0.027 Uiso 1 1 calc R . . Cl2 Cl -0.3773(4) -0.0281(3) 0.0874(3) 0.0395(9) Uani 0.332(9) 1 d P A 1 O2 O 0.22268(11) -0.15058(10) 0.17024(6) 0.0283(3) Uani 1 1 d . . . N2 N 0.31077(12) -0.10993(11) 0.08186(7) 0.0229(3) Uani 1 1 d D . . C2 C 0.37307(14) -0.34822(12) 0.16115(8) 0.0220(4) Uani 1 1 d . . . H2 H 0.3303 -0.3900 0.1656 0.026 Uiso 1 1 calc R . . O3 O 0.09049(11) -0.27084(10) 0.15051(6) 0.0285(3) Uani 1 1 d . . . N3 N -0.05934(12) -0.25709(11) 0.05928(7) 0.0229(3) Uani 1 1 d . . . C3 C 0.51704(14) -0.28641(12) 0.18555(8) 0.0223(4) Uani 1 1 d . . . H3 H 0.5766 -0.2841 0.2076 0.027 Uiso 1 1 calc R . . O4 O 0.01378(11) -0.17182(11) -0.02199(6) 0.0289(3) Uani 1 1 d . . . N4 N -0.04350(12) -0.03201(10) 0.19122(7) 0.0193(3) Uani 1 1 d . . . C4 C 0.49578(14) -0.22853(12) 0.14803(9) 0.0229(4) Uani 1 1 d . . . H4 H 0.5401 -0.1878 0.1442 0.027 Uiso 1 1 calc R . . O5 O 0.13534(12) -0.03969(11) 0.01670(7) 0.0317(4) Uani 1 1 d . . . N5 N 0.13837(12) 0.06494(11) 0.22889(7) 0.0236(3) Uani 1 1 d . . . C5 C 0.40827(14) -0.23083(12) 0.11585(8) 0.0220(4) Uani 1 1 d . . . O6 O -0.31813(18) 0.04478(17) 0.09364(12) 0.0691(8) Uani 1 1 d . . . C6 C 0.38575(15) -0.16956(13) 0.07380(9) 0.0247(4) Uani 1 1 d . . . H6A H 0.3651 -0.1973 0.0404 0.030 Uiso 1 1 calc R . . H6B H 0.4448 -0.1406 0.0704 0.030 Uiso 1 1 calc R . . O7 O -0.3333(3) -0.0900(2) 0.07805(14) 0.1013(13) Uani 1 1 d . . . C7 C 0.32856(17) -0.06609(15) 0.13302(10) 0.0314(5) Uani 1 1 d . . . H7A H 0.3952 -0.0475 0.1385 0.038 Uiso 1 1 calc R . . H7B H 0.2874 -0.0186 0.1302 0.038 Uiso 1 1 calc R . . O8 O -0.3428(3) -0.0382(4) 0.16071(17) 0.0776(18) Uani 0.668(9) 1 d P A 2 C8 C 0.31197(16) -0.11159(16) 0.18027(10) 0.0321(5) Uani 1 1 d . . . H8A H 0.3631 -0.1511 0.1893 0.038 Uiso 1 1 calc R . . H8B H 0.3129 -0.0750 0.2101 0.038 Uiso 1 1 calc R . . O9 O -0.4154(17) -0.0387(10) 0.1330(6) 0.168(13) Uani 0.332(9) 1 d P A 1 C9 C 0.21193(17) -0.20687(16) 0.20934(9) 0.0319(5) Uani 1 1 d . . . H9A H 0.2262 -0.1817 0.2440 0.038 Uiso 1 1 calc R . . H9B H 0.2572 -0.2510 0.2079 0.038 Uiso 1 1 calc R . . O10 O -0.4661(2) -0.0121(2) 0.0938(2) 0.0601(17) Uani 0.668(9) 1 d P A 2 C10 C 0.11275(17) -0.23839(16) 0.20155(9) 0.0324(5) Uani 1 1 d . . . H10A H 0.1067 -0.2799 0.2278 0.039 Uiso 1 1 calc R . . H10B H 0.0678 -0.1952 0.2062 0.039 Uiso 1 1 calc R . . O11 O -0.4502(6) -0.0175(5) 0.0450(5) 0.077(4) Uani 0.332(9) 1 d P A 1 C11 C 0.00525(17) -0.31676(15) 0.14508(10) 0.0322(5) Uani 1 1 d . . . H11B H -0.0433 -0.2887 0.1617 0.039 Uiso 1 1 calc R . . H11A H 0.0181 -0.3685 0.1627 0.039 Uiso 1 1 calc R . . O12 O 0.5000 0.0082(3) 0.2500 0.0938(15) Uani 1 2 d S . . C12 C -0.03132(17) -0.32990(14) 0.08821(10) 0.0311(5) Uani 1 1 d . . . H12A H 0.0186 -0.3567 0.0719 0.037 Uiso 1 1 calc R . . H12B H -0.0867 -0.3659 0.0852 0.037 Uiso 1 1 calc R . . C13 C -0.08442(16) -0.27416(15) 0.00379(9) 0.0301(5) Uani 1 1 d . . . H13B H -0.1492 -0.2968 -0.0027 0.036 Uiso 1 1 calc R . . H13A H -0.0401 -0.3144 -0.0064 0.036 Uiso 1 1 calc R . . C14 C -0.08086(16) -0.20172(17) -0.02938(9) 0.0335(5) Uani 1 1 d . . . H14A H -0.1008 -0.2153 -0.0665 0.040 Uiso 1 1 calc R . . H14B H -0.1247 -0.1609 -0.0195 0.040 Uiso 1 1 calc R . . C15 C 0.02134(16) -0.09872(15) -0.04877(9) 0.0297(5) Uani 1 1 d . . . H15B H -0.0238 -0.0596 -0.0381 0.036 Uiso 1 1 calc R . . H15A H 0.0055 -0.1071 -0.0868 0.036 Uiso 1 1 calc R . . C16 C 0.12079(17) -0.06825(15) -0.03568(9) 0.0309(5) Uani 1 1 d . . . H16A H 0.1664 -0.1113 -0.0395 0.037 Uiso 1 1 calc R . . H16B H 0.1314 -0.0249 -0.0598 0.037 Uiso 1 1 calc R . . C17 C 0.22259(18) 0.00162(15) 0.02948(12) 0.0386(6) Uani 1 1 d . . . H17A H 0.2210 0.0323 0.0618 0.046 Uiso 1 1 calc R . . H17B H 0.2292 0.0397 0.0013 0.046 Uiso 1 1 calc R . . C18 C 0.30793(16) -0.05198(14) 0.03719(10) 0.0309(5) Uani 1 1 d . . . H18A H 0.3658 -0.0188 0.0432 0.037 Uiso 1 1 calc R . . H18B H 0.3095 -0.0823 0.0047 0.037 Uiso 1 1 calc R . . C19 C -0.13623(14) -0.21523(13) 0.07968(8) 0.0232(4) Uani 1 1 d . . . H19B H -0.1745 -0.2543 0.0959 0.028 Uiso 1 1 calc R . . H19A H -0.1782 -0.1904 0.0503 0.028 Uiso 1 1 calc R . . C20 C -0.10192(13) -0.15236(12) 0.11907(8) 0.0194(4) Uani 1 1 d . . . C21 C -0.02244(14) -0.10618(13) 0.11503(8) 0.0220(4) Uani 1 1 d . . . H21 H 0.0130 -0.1146 0.0874 0.026 Uiso 1 1 calc R . . C22 C 0.00434(14) -0.04780(12) 0.15178(8) 0.0209(4) Uani 1 1 d . . . H22 H 0.0594 -0.0174 0.1489 0.025 Uiso 1 1 calc R . . C23 C -0.12054(15) -0.07626(13) 0.19445(9) 0.0251(4) Uani 1 1 d . . . H23 H -0.1559 -0.0657 0.2219 0.030 Uiso 1 1 calc R . . C24 C -0.15098(15) -0.13640(14) 0.15995(9) 0.0258(4) Uani 1 1 d . . . H24 H -0.2054 -0.1667 0.1642 0.031 Uiso 1 1 calc R . . C25 C 0.19325(14) 0.09326(12) 0.20556(8) 0.0211(4) Uani 1 1 d . . . C26 C 0.5188(4) -0.0618(3) 0.2253(2) 0.0337(10) Uani 0.50 1 d P . . H1A H 0.141(2) -0.2286(19) 0.0893(9) 0.040 Uiso 1 1 d D . . H1B H 0.1097(17) -0.2013(18) 0.0366(10) 0.040 Uiso 1 1 d D . . H2N H 0.2525(15) -0.1365(17) 0.0792(12) 0.040 Uiso 1 1 d 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 Fe1 0.01782(17) 0.01359(18) 0.01920(18) 0.000 0.00441(13) 0.000 Cl1 0.0264(5) 0.0344(6) 0.0542(12) -0.0140(8) -0.0031(7) 0.0024(4) S1 0.0371(3) 0.0269(3) 0.0458(4) 0.0004(3) 0.0236(3) -0.0068(2) O1 0.0216(7) 0.0292(8) 0.0249(7) 0.0019(6) 0.0011(5) 0.0003(6) N1 0.0224(7) 0.0177(8) 0.0224(8) -0.0004(6) 0.0031(6) 0.0012(6) C1 0.0211(8) 0.0212(9) 0.0243(9) -0.0016(8) 0.0016(7) 0.0027(7) Cl2 0.0425(17) 0.0256(12) 0.052(2) -0.0056(15) 0.0110(16) -0.0017(11) O2 0.0256(7) 0.0337(9) 0.0243(8) -0.0011(6) -0.0008(6) 0.0006(6) N2 0.0212(7) 0.0186(8) 0.0279(9) -0.0004(7) 0.0010(6) 0.0021(6) C2 0.0218(8) 0.0182(9) 0.0258(10) -0.0014(7) 0.0034(7) 0.0006(7) O3 0.0296(8) 0.0304(8) 0.0265(8) 0.0014(7) 0.0069(6) -0.0001(6) N3 0.0245(8) 0.0220(8) 0.0228(8) -0.0060(7) 0.0057(6) -0.0012(7) C3 0.0209(8) 0.0193(9) 0.0259(10) 0.0006(8) 0.0012(7) -0.0002(7) O4 0.0237(7) 0.0402(9) 0.0221(7) 0.0022(7) 0.0010(5) 0.0001(6) N4 0.0216(7) 0.0152(7) 0.0216(8) 0.0020(6) 0.0048(6) 0.0010(6) C4 0.0217(8) 0.0173(9) 0.0296(10) 0.0022(8) 0.0036(7) 0.0012(7) O5 0.0299(8) 0.0321(9) 0.0313(9) -0.0038(7) -0.0016(6) 0.0066(7) N5 0.0226(8) 0.0210(8) 0.0279(9) 0.0014(7) 0.0062(6) -0.0003(6) C5 0.0229(9) 0.0201(9) 0.0237(9) 0.0017(8) 0.0055(7) 0.0059(7) O6 0.0508(14) 0.0700(17) 0.089(2) -0.0122(15) 0.0195(13) -0.0272(12) C6 0.0259(9) 0.0221(10) 0.0265(10) 0.0035(8) 0.0055(7) 0.0050(8) O7 0.105(2) 0.079(2) 0.103(2) -0.0581(19) -0.037(2) 0.0417(19) C7 0.0317(11) 0.0262(11) 0.0357(12) -0.0103(10) 0.0035(9) -0.0029(9) O8 0.059(3) 0.123(5) 0.051(2) -0.004(3) 0.0074(19) 0.045(3) C8 0.0269(10) 0.0383(13) 0.0299(11) -0.0133(10) 0.0005(8) 0.0010(9) O9 0.28(3) 0.158(14) 0.092(11) -0.058(11) 0.127(17) -0.161(18) C9 0.0319(11) 0.0407(14) 0.0222(10) -0.0007(9) 0.0014(8) 0.0104(10) O10 0.0265(14) 0.051(2) 0.099(5) 0.013(2) -0.0037(18) -0.0074(14) C10 0.0337(11) 0.0385(13) 0.0257(11) 0.0046(10) 0.0070(8) 0.0064(10) O11 0.043(4) 0.055(5) 0.123(11) 0.013(5) -0.020(5) -0.003(3) C11 0.0347(11) 0.0239(11) 0.0391(13) 0.0074(10) 0.0095(10) -0.0016(9) O12 0.093(3) 0.109(4) 0.075(3) 0.000 0.000(2) 0.000 C12 0.0321(11) 0.0202(10) 0.0425(13) -0.0018(9) 0.0101(9) -0.0019(8) C13 0.0277(10) 0.0360(12) 0.0270(11) -0.0143(9) 0.0046(8) -0.0055(9) C14 0.0252(10) 0.0527(16) 0.0218(10) -0.0061(10) 0.0012(8) -0.0010(10) C15 0.0290(10) 0.0356(12) 0.0239(10) 0.0019(9) 0.0017(8) 0.0073(9) C16 0.0315(11) 0.0337(12) 0.0269(11) 0.0037(9) 0.0031(8) 0.0049(9) C17 0.0367(12) 0.0226(11) 0.0519(16) 0.0029(11) -0.0081(11) 0.0047(9) C18 0.0278(10) 0.0230(10) 0.0402(13) 0.0091(9) -0.0007(9) -0.0009(8) C19 0.0214(8) 0.0239(10) 0.0248(10) -0.0050(8) 0.0051(7) -0.0030(7) C20 0.0209(8) 0.0175(9) 0.0195(8) -0.0011(7) 0.0017(6) 0.0009(7) C21 0.0239(9) 0.0225(9) 0.0209(9) -0.0011(7) 0.0075(7) -0.0009(7) C22 0.0231(8) 0.0193(9) 0.0212(9) 0.0010(7) 0.0057(7) -0.0026(7) C23 0.0273(10) 0.0230(10) 0.0278(10) -0.0064(8) 0.0127(8) -0.0039(8) C24 0.0252(9) 0.0249(10) 0.0294(11) -0.0056(8) 0.0112(8) -0.0053(8) C25 0.0209(8) 0.0163(9) 0.0262(10) -0.0025(7) 0.0034(7) 0.0004(7) C26 0.032(2) 0.032(2) 0.033(2) -0.011(2) -0.0072(18) 0.0002(19) _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 Fe1 N5 2.1279(18) 2 ? Fe1 N5 2.1280(18) . ? Fe1 N4 2.1951(17) . ? Fe1 N4 2.1952(17) 2 ? Fe1 N1 2.2115(18) 3_455 ? Fe1 N1 2.2116(18) 4 ? Cl1 O6 1.392(4) . ? Cl1 O10 1.428(4) . ? Cl1 O8 1.431(5) . ? Cl1 O7 1.460(4) . ? S1 C25 1.626(2) . ? O1 H1A 0.896(18) . ? O1 H1B 0.885(17) . ? N1 C2 1.342(3) . ? N1 C3 1.347(3) . ? N1 Fe1 2.2116(18) 3_545 ? C1 C2 1.383(3) . ? C1 C5 1.394(3) . ? C1 H1 0.9500 . ? Cl2 O7 1.260(5) . ? Cl2 O9 1.388(10) . ? Cl2 O11 1.408(10) . ? Cl2 O6 1.486(6) . ? O2 C9 1.416(3) . ? O2 C8 1.422(3) . ? N2 C6 1.506(3) . ? N2 C7 1.509(3) . ? N2 C18 1.514(3) . ? N2 H2N 0.937(17) . ? C2 H2 0.9500 . ? O3 C10 1.426(3) . ? O3 C11 1.430(3) . ? N3 C13 1.461(3) . ? N3 C12 1.464(3) . ? N3 C19 1.469(3) . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? O4 C14 1.426(3) . ? O4 C15 1.428(3) . ? N4 C22 1.341(3) . ? N4 C23 1.341(3) . ? C4 C5 1.394(3) . ? C4 H4 0.9500 . ? O5 C17 1.421(3) . ? O5 C16 1.429(3) . ? N5 C25 1.162(3) . ? C5 C6 1.504(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.497(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.496(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.507(4) . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? O12 C26 1.390(7) 2_655 ? O12 C26 1.390(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.501(4) . ? C13 H13B 0.9900 . ? C13 H13A 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.498(3) . ? C15 H15B 0.9900 . ? C15 H15A 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.505(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.504(3) . ? C19 H19B 0.9900 . ? C19 H19A 0.9900 . ? C20 C24 1.384(3) . ? C20 C21 1.392(3) . ? C21 C22 1.385(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.380(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C26 C26 1.464(11) 2_655 ? 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 N5 Fe1 N5 175.07(10) 2 . ? N5 Fe1 N4 91.95(7) 2 . ? N5 Fe1 N4 91.52(7) . . ? N5 Fe1 N4 91.52(7) 2 2 ? N5 Fe1 N4 91.95(7) . 2 ? N4 Fe1 N4 90.55(9) . 2 ? N5 Fe1 N1 88.37(7) 2 3_455 ? N5 Fe1 N1 88.07(7) . 3_455 ? N4 Fe1 N1 90.91(6) . 3_455 ? N4 Fe1 N1 178.54(7) 2 3_455 ? N5 Fe1 N1 88.07(7) 2 4 ? N5 Fe1 N1 88.37(7) . 4 ? N4 Fe1 N1 178.54(7) . 4 ? N4 Fe1 N1 90.91(6) 2 4 ? N1 Fe1 N1 87.63(9) 3_455 4 ? O6 Cl1 O10 110.6(3) . . ? O6 Cl1 O8 109.4(3) . . ? O10 Cl1 O8 108.4(4) . . ? O6 Cl1 O7 108.5(3) . . ? O10 Cl1 O7 111.7(3) . . ? O8 Cl1 O7 108.2(3) . . ? H1A O1 H1B 109(3) . . ? C2 N1 C3 117.96(18) . . ? C2 N1 Fe1 121.24(14) . 3_545 ? C3 N1 Fe1 120.71(13) . 3_545 ? C2 C1 C5 119.30(19) . . ? C2 C1 H1 120.4 . . ? C5 C1 H1 120.4 . . ? O7 Cl2 O9 109.1(11) . . ? O7 Cl2 O11 106.5(6) . . ? O9 Cl2 O11 110.2(12) . . ? O7 Cl2 O6 114.6(4) . . ? O9 Cl2 O6 107.6(6) . . ? O11 Cl2 O6 108.7(5) . . ? C9 O2 C8 111.70(18) . . ? C6 N2 C7 114.94(17) . . ? C6 N2 C18 105.22(17) . . ? C7 N2 C18 109.90(18) . . ? C6 N2 H2N 108(2) . . ? C7 N2 H2N 109(2) . . ? C18 N2 H2N 109.3(19) . . ? N1 C2 C1 122.69(19) . . ? N1 C2 H2 118.7 . . ? C1 C2 H2 118.7 . . ? C10 O3 C11 111.49(18) . . ? C13 N3 C12 110.40(18) . . ? C13 N3 C19 111.49(17) . . ? C12 N3 C19 112.26(18) . . ? N1 C3 C4 122.93(18) . . ? N1 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C14 O4 C15 112.29(18) . . ? C22 N4 C23 116.95(18) . . ? C22 N4 Fe1 123.29(13) . . ? C23 N4 Fe1 119.75(14) . . ? C3 C4 C5 119.01(19) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C17 O5 C16 112.6(2) . . ? C25 N5 Fe1 151.08(17) . . ? C1 C5 C4 118.11(19) . . ? C1 C5 C6 122.47(19) . . ? C4 C5 C6 119.38(19) . . ? C5 C6 N2 115.90(18) . . ? C5 C6 H6A 108.3 . . ? N2 C6 H6A 108.3 . . ? C5 C6 H6B 108.3 . . ? N2 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C8 C7 N2 116.4(2) . . ? C8 C7 H7A 108.2 . . ? N2 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? N2 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? O2 C8 C7 109.56(19) . . ? O2 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O2 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? O2 C9 C10 110.12(18) . . ? O2 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? O2 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? O3 C10 C9 109.61(19) . . ? O3 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? O3 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? O3 C11 C12 109.85(19) . . ? O3 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? O3 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? H11B C11 H11A 108.2 . . ? C26 O12 C26 63.5(5) 2_655 . ? N3 C12 C11 114.02(19) . . ? N3 C12 H12A 108.7 . . ? C11 C12 H12A 108.7 . . ? N3 C12 H12B 108.7 . . ? C11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? N3 C13 C14 112.44(19) . . ? N3 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? N3 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? H13B C13 H13A 107.8 . . ? O4 C14 C13 108.91(19) . . ? O4 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? O4 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? O4 C15 C16 108.92(18) . . ? O4 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? O4 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? H15B C15 H15A 108.3 . . ? O5 C16 C15 109.2(2) . . ? O5 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? O5 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O5 C17 C18 113.4(2) . . ? O5 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? O5 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C17 C18 N2 114.7(2) . . ? C17 C18 H18A 108.6 . . ? N2 C18 H18A 108.6 . . ? C17 C18 H18B 108.6 . . ? N2 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? N3 C19 C20 113.66(16) . . ? N3 C19 H19B 108.8 . . ? C20 C19 H19B 108.8 . . ? N3 C19 H19A 108.8 . . ? C20 C19 H19A 108.8 . . ? H19B C19 H19A 107.7 . . ? C24 C20 C21 117.43(18) . . ? C24 C20 C19 120.64(18) . . ? C21 C20 C19 121.89(18) . . ? C22 C21 C20 119.26(19) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? N4 C22 C21 123.33(18) . . ? N4 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? N4 C23 C24 123.29(19) . . ? N4 C23 H23 118.4 . . ? C24 C23 H23 118.4 . . ? C23 C24 C20 119.74(19) . . ? C23 C24 H24 120.1 . . ? C20 C24 H24 120.1 . . ? N5 C25 S1 178.1(2) . . ? O12 C26 C26 58.2(3) . 2_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.037 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.089 #===END #========================================================================== data_C _database_code_depnum_ccdc_archive 'CCDC 735053' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H36 Ag2 N4 O4, 2(C F3 O3 S)' _chemical_formula_sum 'C26 H36 Ag2 F6 N4 O10 S2' _chemical_formula_weight 958.45 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' F F 0.0171 0.0103 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 26.5762(4) _cell_length_b 26.5762(4) _cell_length_c 26.1635(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16003.4(6) _cell_formula_units_Z 18 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 111 _cell_measurement_theta_min 2.357 _cell_measurement_theta_max 28.278 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8640 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6952 _exptl_absorpt_correction_T_max 0.7359 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker Apex II' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28839 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 31.48 _reflns_number_total 5905 _reflns_number_gt 4709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _computing_structure_refinement X-SEED _computing_molecular_graphics 'MERCURY 1.4 (Bruno et al., 2002)' _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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^)+(0.0908P)^2^+74.4046P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5905 _refine_ls_number_parameters 296 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1799 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.132 _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 Ag1 Ag 0.075281(15) 0.3333 0.0833 0.03027(13) Uani 1 2 d S . . S1 S 0.18229(18) 0.48972(17) 0.28614(13) 0.0435(7) Uani 0.612(6) 1 d P A 1 F1 F 0.2687(3) 0.5389(3) 0.2204(3) 0.088(3) Uani 0.612(6) 1 d P A 1 O1 O -0.03587(19) 0.2929(3) 0.03948(18) 0.0741(14) Uani 1 1 d . . . N1 N 0.01971(15) 0.23359(18) 0.09010(12) 0.0362(8) Uani 1 1 d . . . C1 C -0.0643(4) 0.3278(6) 0.0553(4) 0.118(4) Uani 1 1 d . . . H1A H -0.0458 0.3652 0.0368 0.142 Uiso 1 1 calc R . . H1B H -0.1059 0.3062 0.0459 0.142 Uiso 1 1 calc R . . Ag2 Ag 0.1667 0.3333 0.3333 0.05100(19) Uani 1 2 d S . . S2 S 0.1948(5) 0.4884(5) 0.2885(5) 0.116(5) Uani 0.388(6) 1 d PD A 2 F2 F 0.2913(3) 0.5692(4) 0.2950(5) 0.116(4) Uani 0.612(6) 1 d P A 1 O2 O 0.13874(13) 0.29325(13) 0.04247(10) 0.0310(6) Uani 1 1 d . . . N2 N 0.11560(16) 0.29715(19) 0.26585(13) 0.0423(9) Uani 1 1 d . . . C2 C -0.0670(2) 0.2363(4) 0.05453(19) 0.067(2) Uani 1 1 d . . . H2A H -0.1008 0.2148 0.0316 0.080 Uiso 1 1 calc R . . H2B H -0.0817 0.2341 0.0897 0.080 Uiso 1 1 calc R . . F3 F 0.2402(4) 0.5954(4) 0.2486(5) 0.115(3) Uani 0.612(6) 1 d PU A 1 O3 O 0.1474(4) 0.4733(4) 0.2418(3) 0.0510(17) Uani 0.612(6) 1 d P A 1 C3 C -0.0295(2) 0.2096(3) 0.05290(18) 0.0523(13) Uani 1 1 d . . . H3A H -0.0133 0.2144 0.0180 0.063 Uiso 1 1 calc R . . H3B H -0.0541 0.1674 0.0593 0.063 Uiso 1 1 calc R . . F4 F 0.2667(8) 0.5529(8) 0.3550(7) 0.150(7) Uani 0.388(6) 1 d PDU A 2 O4 O 0.2015(3) 0.4487(4) 0.3001(4) 0.058(2) Uani 0.612(6) 1 d P A 1 C4 C 0.0566(2) 0.2072(2) 0.07953(17) 0.0423(10) Uani 1 1 d . . . H4A H 0.0310 0.1652 0.0731 0.051 Uiso 1 1 calc R . . H4B H 0.0799 0.2112 0.1104 0.051 Uiso 1 1 calc R . . F5 F 0.1823(12) 0.5367(14) 0.3636(11) 0.42(3) Uani 0.388(6) 1 d PDU A 2 O5 O 0.1625(5) 0.5143(5) 0.3251(3) 0.101(3) Uani 0.612(6) 1 d P A 1 C5 C 0.0973(2) 0.2335(2) 0.03474(16) 0.0389(9) Uani 1 1 d . . . H5A H 0.1181 0.2118 0.0290 0.047 Uiso 1 1 calc R . . H5B H 0.0744 0.2295 0.0037 0.047 Uiso 1 1 calc R . . F6 F 0.2379(9) 0.5961(6) 0.3072(9) 0.154(8) Uani 0.388(6) 1 d PD A 2 O6 O 0.1774(14) 0.4371(7) 0.3127(10) 0.171(16) Uani 0.388(6) 1 d PD A 2 C6 C 0.18511(18) 0.30226(18) 0.07576(15) 0.0327(8) Uani 1 1 d . . . H6A H 0.2120 0.2925 0.0580 0.039 Uiso 1 1 calc R . . H6B H 0.1695 0.2772 0.1064 0.039 Uiso 1 1 calc R . . O7 O 0.2505(12) 0.5042(18) 0.2593(14) 0.44(4) Uani 0.388(6) 1 d PDU A 2 C7 C -0.0057(2) 0.2150(2) 0.14278(16) 0.0466(12) Uani 1 1 d . . . H7A H -0.0229 0.1724 0.1459 0.056 Uiso 1 1 calc R . . H7B H -0.0373 0.2240 0.1473 0.056 Uiso 1 1 calc R . . O8 O 0.1581(13) 0.4897(12) 0.2515(10) 0.171(15) Uani 0.388(6) 1 d PDU A 2 C8 C 0.03895(18) 0.2445(2) 0.18475(14) 0.0389(10) Uani 1 1 d . . . C9 C 0.0625(2) 0.2160(2) 0.21090(17) 0.0486(12) Uani 1 1 d . . . H9 H 0.0529 0.1778 0.2012 0.058 Uiso 1 1 calc R . . C10 C 0.1001(3) 0.2430(3) 0.25113(18) 0.0494(12) Uani 1 1 d . . . H10 H 0.1154 0.2225 0.2690 0.059 Uiso 1 1 calc R . . C11 C 0.0938(2) 0.3258(2) 0.24007(16) 0.0406(10) Uani 1 1 d . . . H11 H 0.1054 0.3646 0.2496 0.049 Uiso 1 1 calc R . . C12 C 0.0550(2) 0.3003(2) 0.20000(15) 0.0417(10) Uani 1 1 d . . . H12 H 0.0394 0.3212 0.1831 0.050 Uiso 1 1 calc R . . C13 C 0.2503(5) 0.5520(4) 0.2630(7) 0.092(5) Uani 0.612(6) 1 d P A 1 C14 C 0.2204(10) 0.5448(8) 0.3285(8) 0.177(16) Uiso 0.388(6) 1 d PD A 2 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 Ag1 0.02830(17) 0.0420(3) 0.02508(19) 0.00061(15) 0.00030(7) 0.02100(13) S1 0.0406(13) 0.0488(15) 0.0390(12) -0.0109(10) -0.0091(10) 0.0209(11) F1 0.075(5) 0.073(5) 0.127(7) 0.019(4) 0.041(4) 0.046(4) O1 0.041(2) 0.115(4) 0.067(3) 0.013(3) 0.0001(19) 0.040(3) N1 0.0247(16) 0.048(2) 0.0203(13) -0.0040(13) -0.0030(11) 0.0060(15) C1 0.049(4) 0.189(11) 0.123(7) 0.036(8) -0.006(5) 0.065(6) Ag2 0.0311(3) 0.0774(4) 0.0286(2) -0.0125(2) -0.00663(17) 0.0152(2) S2 0.111(9) 0.113(7) 0.113(7) -0.019(5) -0.052(6) 0.049(6) F2 0.039(4) 0.077(5) 0.196(11) -0.040(6) -0.014(5) 0.002(3) O2 0.0320(14) 0.0391(15) 0.0249(12) -0.0019(10) -0.0023(10) 0.0200(12) N2 0.0315(18) 0.058(2) 0.0245(15) -0.0037(15) -0.0012(13) 0.0126(18) C2 0.026(2) 0.124(6) 0.029(2) -0.004(3) -0.0017(17) 0.021(3) F3 0.101(5) 0.070(4) 0.186(8) 0.023(5) 0.032(5) 0.052(4) O3 0.064(4) 0.063(4) 0.049(3) -0.006(3) -0.015(3) 0.049(4) C3 0.034(2) 0.067(3) 0.030(2) -0.005(2) -0.0090(17) 0.006(2) F4 0.150(10) 0.135(10) 0.159(11) -0.018(8) -0.021(8) 0.067(8) O4 0.045(4) 0.059(5) 0.071(5) 0.021(4) -0.023(3) 0.027(4) C4 0.044(2) 0.036(2) 0.035(2) -0.0060(16) -0.0034(17) 0.011(2) F5 0.43(3) 0.42(3) 0.42(3) -0.005(10) 0.017(10) 0.208(18) O5 0.114(8) 0.115(8) 0.064(5) -0.037(5) 0.014(5) 0.049(6) C5 0.044(2) 0.044(2) 0.0279(17) -0.0099(16) -0.0030(16) 0.021(2) F6 0.175(17) 0.069(9) 0.24(2) -0.001(11) -0.016(16) 0.078(11) O6 0.23(3) 0.050(11) 0.15(2) -0.021(13) -0.06(2) 0.005(16) C6 0.033(2) 0.039(2) 0.0318(17) -0.0013(15) -0.0025(14) 0.0223(18) O7 0.44(4) 0.44(4) 0.44(5) -0.002(10) 0.008(10) 0.22(2) C7 0.035(2) 0.056(3) 0.0247(17) 0.0010(17) 0.0010(15) 0.005(2) O8 0.182(18) 0.166(18) 0.184(18) -0.008(9) -0.024(9) 0.101(12) C8 0.0284(19) 0.048(2) 0.0211(15) 0.0024(15) 0.0028(13) 0.0053(18) C9 0.056(3) 0.045(3) 0.033(2) -0.0028(18) -0.0081(19) 0.016(2) C10 0.055(3) 0.058(3) 0.033(2) -0.002(2) -0.008(2) 0.027(3) C11 0.038(2) 0.048(3) 0.0282(18) -0.0012(16) 0.0039(16) 0.016(2) C12 0.039(2) 0.057(3) 0.0224(16) 0.0021(17) 0.0031(15) 0.019(2) C13 0.048(6) 0.030(5) 0.198(16) -0.009(7) 0.019(8) 0.019(4) _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 Ag1 N1 2.308(4) . ? Ag1 N1 2.307(4) 16_554 ? S1 O3 1.411(8) . ? S1 O5 1.446(9) . ? S1 O4 1.464(8) . ? S1 C13 1.838(12) . ? F1 C13 1.332(17) . ? O1 C2 1.363(9) . ? O1 C1 1.515(12) . ? N1 C4 1.490(7) . ? N1 C3 1.493(5) . ? N1 C7 1.505(5) . ? C1 C1 1.487(19) 16_554 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? Ag2 N2 2.140(4) . ? Ag2 N2 2.140(4) 31 ? S2 O6 1.358(15) . ? S2 O8 1.387(15) . ? S2 O7 1.527(17) . ? S2 C14 1.67(2) . ? F2 C13 1.264(18) . ? O2 C5 1.423(6) . ? O2 C6 1.428(5) . ? N2 C10 1.340(7) . ? N2 C11 1.346(7) . ? C2 C3 1.485(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? F3 C13 1.362(14) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? F4 C14 1.332(18) . ? C4 C5 1.509(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? F5 C14 1.306(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? F6 C14 1.324(17) . ? C6 C6 1.484(8) 16_554 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.517(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.382(7) . ? C8 C12 1.382(7) . ? C9 C10 1.379(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.387(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? 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 Ag1 N1 172.48(19) . 16_554 ? O3 S1 O5 112.7(6) . . ? O3 S1 O4 113.3(5) . . ? O5 S1 O4 120.2(7) . . ? O3 S1 C13 101.9(7) . . ? O5 S1 C13 103.9(6) . . ? O4 S1 C13 101.6(6) . . ? C2 O1 C1 112.5(6) . . ? C4 N1 C3 108.7(4) . . ? C4 N1 C7 108.0(4) . . ? C3 N1 C7 107.6(3) . . ? C4 N1 Ag1 109.4(3) . . ? C3 N1 Ag1 111.2(3) . . ? C7 N1 Ag1 111.9(3) . . ? C1 C1 O1 111.2(7) 16_554 . ? C1 C1 H1A 109.4 16_554 . ? O1 C1 H1A 109.4 . . ? C1 C1 H1B 109.4 16_554 . ? O1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 Ag2 N2 179.993(1) . 31 ? O6 S2 O8 117.4(15) . . ? O6 S2 O7 107.8(15) . . ? O8 S2 O7 103.9(15) . . ? O6 S2 C14 113.1(12) . . ? O8 S2 C14 113.1(13) . . ? O7 S2 C14 99.3(13) . . ? C5 O2 C6 113.3(3) . . ? C10 N2 C11 118.4(4) . . ? C10 N2 Ag2 120.4(3) . . ? C11 N2 Ag2 121.0(3) . . ? O1 C2 C3 109.8(4) . . ? O1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? O1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 N1 115.5(5) . . ? C2 C3 H3A 108.4 . . ? N1 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? N1 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? N1 C4 C5 114.5(4) . . ? N1 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? N1 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? O2 C5 C4 112.5(3) . . ? O2 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? O2 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? O2 C6 C6 107.6(3) . 16_554 ? O2 C6 H6A 110.2 . . ? C6 C6 H6A 110.2 16_554 . ? O2 C6 H6B 110.2 . . ? C6 C6 H6B 110.2 16_554 . ? H6A C6 H6B 108.5 . . ? N1 C7 C8 112.7(4) . . ? N1 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C12 117.7(4) . . ? C9 C8 C7 121.8(5) . . ? C12 C8 C7 120.4(5) . . ? C10 C9 C8 120.1(5) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? N2 C10 C9 122.2(5) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? N2 C11 C12 121.9(5) . . ? N2 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C8 C12 C11 119.8(5) . . ? C8 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? F2 C13 F1 106.5(10) . . ? F2 C13 F3 112.2(11) . . ? F1 C13 F3 104.0(14) . . ? F2 C13 S1 112.9(12) . . ? F1 C13 S1 111.3(8) . . ? F3 C13 S1 109.5(8) . . ? F5 C14 F6 107.9(18) . . ? F5 C14 F4 103.7(17) . . ? F6 C14 F4 103.5(15) . . ? F5 C14 S2 111.0(16) . . ? F6 C14 S2 116.0(14) . . ? F4 C14 S2 113.7(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.556 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.169 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 24 14 ' ' 2 0.000 0.000 0.250 28 17 ' ' 3 0.000 0.000 0.500 24 14 ' ' 4 0.000 0.000 0.750 28 17 ' ' 5 0.333 0.667 0.167 21 13 ' ' 6 0.333 0.667 0.667 21 13 ' ' 7 0.333 0.667 0.917 24 15 ' ' 8 0.333 0.667 0.417 24 15 ' ' 9 0.667 0.333 0.333 21 13 ' ' 10 0.667 0.333 0.583 24 15 ' ' 11 0.667 0.333 0.833 21 13 ' ' 12 0.667 0.333 0.083 24 15 ' ' _platon_squeeze_details ; ; #===END #========================================================================== data_D _database_code_depnum_ccdc_archive 'CCDC 735054' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H38 Fe N8 O4 S4, 2(C H4 O)' _chemical_formula_sum 'C30 H46 Fe N8 O6 S4' _chemical_formula_weight 798.84 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' Fe Fe 0.3463 0.8444 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8825(8) _cell_length_b 10.0056(8) _cell_length_c 10.1091(6) _cell_angle_alpha 103.378(1) _cell_angle_beta 94.538(1) _cell_angle_gamma 96.319(1) _cell_volume 960.89(12) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 254 _cell_measurement_theta_min 2.765 _cell_measurement_theta_max 26.396 _exptl_crystal_description prism _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8793 _exptl_absorpt_correction_T_max 0.9075 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8845 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.42 _reflns_number_total 3927 _reflns_number_gt 3447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0506P)^2^+0.8027P] 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 3927 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Fe1 Fe 0.5000 0.5000 0.5000 0.01963(13) Uani 1 2 d S . . S1 S 0.30948(7) 0.55546(6) 0.05202(6) 0.03281(17) Uani 1 1 d . . . O1 O 0.34357(17) 1.06187(16) 1.03464(16) 0.0261(4) Uani 1 1 d . . . N1 N 0.1752(2) 1.1083(2) 0.8050(2) 0.0241(4) Uani 1 1 d . . . C1 C 0.3463(3) 1.0806(3) 1.1790(2) 0.0307(5) Uani 1 1 d . . . H1A H 0.2993 1.1609 1.2179 0.037 Uiso 1 1 calc R . . H1B H 0.4421 1.0985 1.2220 0.037 Uiso 1 1 calc R . . H1 H 0.155(3) 1.115(3) 0.717(3) 0.037 Uiso 1 1 d . . . S2 S 0.10697(6) 0.15048(6) 0.50090(6) 0.02883(16) Uani 1 1 d . . . O2 O -0.13571(17) 1.06578(17) 0.85037(17) 0.0279(4) Uani 1 1 d . . . N2 N 0.37437(19) 0.65722(19) 0.60078(19) 0.0220(4) Uani 1 1 d . . . C2 C 0.3719(3) 1.1868(3) 0.9939(3) 0.0317(6) Uani 1 1 d . . . H2A H 0.4714 1.2197 1.0114 0.038 Uiso 1 1 calc R . . H2B H 0.3231 1.2589 1.0470 0.038 Uiso 1 1 calc R . . O3 O 0.0196(4) 0.4308(6) 0.1624(5) 0.167(3) Uani 1 1 d . . . H3 H 0.0825 0.4712 0.1290 0.201 Uiso 1 1 calc R . . N3 N 0.4202(2) 0.5192(2) 0.3028(2) 0.0288(5) Uani 1 1 d . . . C3 C 0.3257(2) 1.1614(3) 0.8441(3) 0.0286(5) Uani 1 1 d . . . H3A H 0.3797 1.0933 0.7926 0.034 Uiso 1 1 calc R . . H3B H 0.3461 1.2490 0.8156 0.034 Uiso 1 1 calc R . . N4 N 0.3380(2) 0.3398(2) 0.4997(2) 0.0293(5) Uani 1 1 d . . . C4 C 0.0866(3) 1.2026(3) 0.8865(3) 0.0329(6) Uani 1 1 d . . . H4A H 0.1268 1.2999 0.8965 0.040 Uiso 1 1 calc R . . H4B H 0.0874 1.1856 0.9792 0.040 Uiso 1 1 calc R . . C5 C -0.0605(3) 1.1838(3) 0.8233(3) 0.0349(6) Uani 1 1 d . . . H5A H -0.1033 1.2673 0.8613 0.042 Uiso 1 1 calc R . . H5B H -0.0626 1.1726 0.7232 0.042 Uiso 1 1 calc R . . C6 C -0.2752(3) 1.0482(3) 0.7942(3) 0.0304(5) Uani 1 1 d . . . H6A H -0.2806 1.0408 0.6945 0.037 Uiso 1 1 calc R . . H6B H -0.3197 1.1290 0.8369 0.037 Uiso 1 1 calc R . . C7 C 0.1333(2) 0.9588(2) 0.8073(2) 0.0251(5) Uani 1 1 d . . . H7A H 0.1355 0.9525 0.9037 0.030 Uiso 1 1 calc R . . H7B H 0.0377 0.9302 0.7647 0.030 Uiso 1 1 calc R . . C8 C 0.2224(2) 0.8585(2) 0.7345(2) 0.0239(5) Uani 1 1 d . . . C9 C 0.2628(3) 0.8587(3) 0.6059(3) 0.0293(5) Uani 1 1 d . . . H9 H 0.2381 0.9271 0.5605 0.035 Uiso 1 1 calc R . . C10 C 0.3396(3) 0.7581(2) 0.5441(2) 0.0274(5) Uani 1 1 d . . . H10 H 0.3687 0.7613 0.4574 0.033 Uiso 1 1 calc R . . C11 C 0.3339(2) 0.6564(2) 0.7249(2) 0.0265(5) Uani 1 1 d . . . H11 H 0.3568 0.5847 0.7665 0.032 Uiso 1 1 calc R . . C12 C 0.2605(2) 0.7554(2) 0.7947(3) 0.0266(5) Uani 1 1 d . . . H12 H 0.2364 0.7526 0.8833 0.032 Uiso 1 1 calc R . . C13 C 0.3763(2) 0.5351(2) 0.1987(2) 0.0246(5) Uani 1 1 d . . . C14 C 0.2434(2) 0.2616(2) 0.5016(2) 0.0226(5) Uani 1 1 d . . . C15 C 0.0402(4) 0.4751(5) 0.3076(5) 0.0805(13) Uani 1 1 d . . . H15A H -0.0294 0.4230 0.3467 0.121 Uiso 1 1 calc R . . H15B H 0.0329 0.5743 0.3360 0.121 Uiso 1 1 calc R . . H15C H 0.1315 0.4583 0.3401 0.121 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 Fe1 0.0196(2) 0.0182(2) 0.0205(2) 0.00379(17) 0.00192(17) 0.00165(17) S1 0.0451(4) 0.0283(3) 0.0272(3) 0.0094(2) -0.0001(3) 0.0117(3) O1 0.0299(9) 0.0237(8) 0.0228(9) 0.0018(6) 0.0027(7) 0.0031(7) N1 0.0246(10) 0.0248(10) 0.0223(10) 0.0036(8) 0.0030(8) 0.0040(8) C1 0.0321(13) 0.0314(13) 0.0249(13) 0.0010(10) -0.0029(10) 0.0048(10) S2 0.0262(3) 0.0317(3) 0.0277(3) 0.0102(2) 0.0008(2) -0.0052(2) O2 0.0255(9) 0.0312(9) 0.0299(9) 0.0104(7) 0.0052(7) 0.0083(7) N2 0.0207(9) 0.0212(9) 0.0230(10) 0.0033(7) 0.0022(7) 0.0028(7) C2 0.0315(13) 0.0259(12) 0.0335(14) 0.0040(10) -0.0004(11) -0.0044(10) O3 0.104(3) 0.210(5) 0.121(4) -0.051(3) 0.047(3) -0.096(3) N3 0.0317(11) 0.0294(11) 0.0255(11) 0.0055(8) 0.0026(9) 0.0080(9) C3 0.0250(12) 0.0280(12) 0.0315(13) 0.0068(10) 0.0047(10) -0.0025(9) N4 0.0270(11) 0.0279(10) 0.0324(12) 0.0065(9) 0.0062(9) 0.0001(8) C4 0.0353(14) 0.0260(12) 0.0360(15) 0.0004(10) 0.0130(11) 0.0065(10) C5 0.0322(14) 0.0330(13) 0.0467(16) 0.0162(12) 0.0172(12) 0.0126(11) C6 0.0301(13) 0.0357(13) 0.0275(13) 0.0094(10) 0.0009(10) 0.0105(10) C7 0.0239(11) 0.0236(11) 0.0270(12) 0.0050(9) 0.0021(9) 0.0029(9) C8 0.0212(11) 0.0242(11) 0.0238(12) 0.0022(9) -0.0003(9) 0.0014(9) C9 0.0356(13) 0.0283(12) 0.0269(13) 0.0095(10) 0.0038(10) 0.0113(10) C10 0.0319(13) 0.0279(12) 0.0231(12) 0.0057(9) 0.0042(10) 0.0080(10) C11 0.0274(12) 0.0245(11) 0.0295(13) 0.0102(10) 0.0028(10) 0.0045(9) C12 0.0256(12) 0.0296(12) 0.0257(12) 0.0079(10) 0.0048(10) 0.0040(9) C13 0.0264(12) 0.0179(10) 0.0286(13) 0.0023(9) 0.0055(10) 0.0053(9) C14 0.0251(12) 0.0232(11) 0.0199(11) 0.0043(9) 0.0028(9) 0.0064(9) C15 0.051(2) 0.083(3) 0.105(4) 0.032(3) -0.009(2) -0.012(2) _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 Fe1 N4 2.137(2) . ? Fe1 N4 2.137(2) 2_666 ? Fe1 N3 2.144(2) . ? Fe1 N3 2.144(2) 2_666 ? Fe1 N2 2.2232(18) . ? Fe1 N2 2.2232(18) 2_666 ? S1 C13 1.640(3) . ? O1 C2 1.411(3) . ? O1 C1 1.425(3) . ? N1 C4 1.507(3) . ? N1 C3 1.512(3) . ? N1 C7 1.514(3) . ? N1 H1 0.91(3) . ? C1 C6 1.491(4) 2_577 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? S2 C14 1.649(2) . ? O2 C5 1.418(3) . ? O2 C6 1.425(3) . ? N2 C10 1.333(3) . ? N2 C11 1.348(3) . ? C2 C3 1.502(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C15 1.423(6) . ? O3 H3 0.8400 . ? N3 C13 1.158(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N4 C14 1.156(3) . ? C4 C5 1.514(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C1 1.491(4) 2_577 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.510(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.384(3) . ? C8 C9 1.390(3) . ? C9 C10 1.390(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 N4 Fe1 N4 180.00(8) . 2_666 ? N4 Fe1 N3 91.72(8) . . ? N4 Fe1 N3 88.28(8) 2_666 . ? N4 Fe1 N3 88.28(8) . 2_666 ? N4 Fe1 N3 91.72(8) 2_666 2_666 ? N3 Fe1 N3 180.000(1) . 2_666 ? N4 Fe1 N2 89.63(7) . . ? N4 Fe1 N2 90.37(7) 2_666 . ? N3 Fe1 N2 90.47(7) . . ? N3 Fe1 N2 89.53(7) 2_666 . ? N4 Fe1 N2 90.37(7) . 2_666 ? N4 Fe1 N2 89.63(7) 2_666 2_666 ? N3 Fe1 N2 89.53(7) . 2_666 ? N3 Fe1 N2 90.47(7) 2_666 2_666 ? N2 Fe1 N2 180.000(1) . 2_666 ? C2 O1 C1 113.55(18) . . ? C4 N1 C3 111.55(18) . . ? C4 N1 C7 111.11(19) . . ? C3 N1 C7 115.52(18) . . ? C4 N1 H1 104.0(18) . . ? C3 N1 H1 106.9(19) . . ? C7 N1 H1 106.9(19) . . ? O1 C1 C6 108.04(19) . 2_577 ? O1 C1 H1A 110.1 . . ? C6 C1 H1A 110.1 2_577 . ? O1 C1 H1B 110.1 . . ? C6 C1 H1B 110.1 2_577 . ? H1A C1 H1B 108.4 . . ? C5 O2 C6 111.36(19) . . ? C10 N2 C11 117.26(19) . . ? C10 N2 Fe1 121.98(15) . . ? C11 N2 Fe1 120.72(15) . . ? O1 C2 C3 108.73(19) . . ? O1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C15 O3 H3 109.5 . . ? C13 N3 Fe1 177.19(19) . . ? C2 C3 N1 114.5(2) . . ? C2 C3 H3A 108.6 . . ? N1 C3 H3A 108.6 . . ? C2 C3 H3B 108.6 . . ? N1 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C14 N4 Fe1 174.40(19) . . ? N1 C4 C5 114.0(2) . . ? N1 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.6 . . ? O2 C5 C4 110.6(2) . . ? O2 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? O2 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? O2 C6 C1 108.4(2) . 2_577 ? O2 C6 H6A 110.0 . . ? C1 C6 H6A 110.0 2_577 . ? O2 C6 H6B 110.0 . . ? C1 C6 H6B 110.0 2_577 . ? H6A C6 H6B 108.4 . . ? C8 C7 N1 114.39(19) . . ? C8 C7 H7A 108.7 . . ? N1 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? N1 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C12 C8 C9 117.5(2) . . ? C12 C8 C7 118.7(2) . . ? C9 C8 C7 123.7(2) . . ? C8 C9 C10 119.5(2) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 123.1(2) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N2 C11 C12 123.0(2) . . ? N2 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C8 C12 C11 119.5(2) . . ? C8 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? N3 C13 S1 178.3(2) . . ? N4 C14 S2 178.7(2) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 S1 0.84 2.55 3.372(4) 165.8 . N1 H1 S2 0.91(3) 2.32(3) 3.227(2) 175(3) 1_565 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.810 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.066 #===END #========================================================================== data_E _database_code_depnum_ccdc_archive 'CCDC 735055' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C54 H76 Ba2 Fe N14 O10 S6, 2(C H Cl3) ; _chemical_formula_sum 'C56 H78 Ba2 Cl6 Fe N14 O10 S6' _chemical_formula_weight 1842.91 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmca 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' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y, z-1/2' _cell_length_a 30.6672(13) _cell_length_b 14.4533(5) _cell_length_c 17.3796(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7703.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 111 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 29.71 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 1.627 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7367 _exptl_absorpt_correction_T_max 0.7923 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 68351 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 30.54 _reflns_number_total 6000 _reflns_number_gt 4595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _computing_structure_refinement X-SEED _computing_molecular_graphics 'MERCURY 1.4 (Bruno et al., 2002)' _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. One barium bound water molecule hydrogen atom was located in the diff map (the other generated by symm) and the bond length constr to 0.95. ; _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^)+(0.0683P)^2^+156.9579P] 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 6000 _refine_ls_number_parameters 229 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.2308 _refine_ls_wR_factor_gt 0.2112 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _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 Ba1 Ba 0.2500 0.32468(4) 0.2500 0.02873(18) Uani 1 2 d S . . Fe1 Fe 0.0000 0.0000 0.5000 0.0247(4) Uani 1 4 d S . . S1 S 0.13781(6) 0.13793(15) 0.11574(12) 0.0399(5) Uani 1 1 d . . . O1 O 0.17691(18) 0.3824(3) 0.1693(3) 0.0373(12) Uani 1 1 d . . . N1 N 0.2247(2) 0.1725(4) 0.1519(4) 0.0324(13) Uani 1 1 d . . . C1 C 0.1290(3) 0.3344(5) 0.2690(5) 0.0390(18) Uani 1 1 d . . . H1A H 0.1024 0.3516 0.2981 0.047 Uiso 1 1 calc R . . H1B H 0.1223 0.2781 0.2388 0.047 Uiso 1 1 calc R . . H3 H 0.257(3) 0.562(4) 0.215(4) 0.047 Uiso 1 1 d D . . S2A S 0.0000 0.2270(4) 0.7067(3) 0.113(2) Uani 1 2 d S A 1 O2 O 0.26044(18) 0.3978(4) 0.1029(3) 0.0366(12) Uani 1 1 d . . . N2 N 0.1644(2) 0.3138(4) 0.3236(4) 0.0341(14) Uani 1 1 d . . . C2 C 0.1406(3) 0.4129(6) 0.2140(6) 0.046(2) Uani 1 1 d . . . H2A H 0.1156 0.4273 0.1801 0.055 Uiso 1 1 calc R . . H2B H 0.1484 0.4693 0.2433 0.055 Uiso 1 1 calc R . . O3 O 0.2500 0.5138(5) 0.2500 0.054(2) Uani 1 2 d SD . . N3 N 0.05172(18) 0.0864(4) 0.4456(4) 0.0304(12) Uani 1 1 d . . . C3 C 0.1849(3) 0.4381(5) 0.1035(5) 0.0403(19) Uani 1 1 d . . . H3A H 0.1937 0.5012 0.1192 0.048 Uiso 1 1 calc R . . H3B H 0.1582 0.4428 0.0716 0.048 Uiso 1 1 calc R . . N4 N 0.0000 0.0895(6) 0.5953(6) 0.035(2) Uani 1 2 d S A . C4 C 0.2210(3) 0.3926(6) 0.0582(5) 0.0425(19) Uani 1 1 d . . . H4A H 0.2136 0.3272 0.0478 0.051 Uiso 1 1 calc R . . H4B H 0.2250 0.4247 0.0084 0.051 Uiso 1 1 calc R . . C5 C 0.2984(3) 0.3721(6) 0.0594(5) 0.043(2) Uani 1 1 d . . . H5A H 0.3019 0.4146 0.0151 0.051 Uiso 1 1 calc R . . H5B H 0.2948 0.3085 0.0392 0.051 Uiso 1 1 calc R . . C6 C 0.3376(3) 0.3766(6) 0.1088(5) 0.045(2) Uani 1 1 d . . . H6A H 0.3413 0.4409 0.1272 0.054 Uiso 1 1 calc R . . H6B H 0.3635 0.3605 0.0776 0.054 Uiso 1 1 calc R . . C7 C 0.1651(2) 0.2146(5) 0.3435(4) 0.0293(14) Uani 1 1 d . . . H7A H 0.1895 0.2039 0.3798 0.035 Uiso 1 1 calc R . . H7B H 0.1715 0.1790 0.2962 0.035 Uiso 1 1 calc R . . C8 C 0.1238(2) 0.1755(5) 0.3792(4) 0.0272(14) Uani 1 1 d . . . C9 C 0.1157(2) 0.1797(5) 0.4577(4) 0.0340(16) Uani 1 1 d . . . H9 H 0.1349 0.2129 0.4907 0.041 Uiso 1 1 calc R . . C10 C 0.0797(2) 0.1351(5) 0.4875(4) 0.0326(15) Uani 1 1 d . . . H10 H 0.0745 0.1395 0.5413 0.039 Uiso 1 1 calc R . . C11 C 0.0585(2) 0.0850(5) 0.3687(4) 0.0320(15) Uani 1 1 d . . . H11 H 0.0385 0.0524 0.3370 0.038 Uiso 1 1 calc R . . C12 C 0.0935(2) 0.1290(5) 0.3344(4) 0.0304(14) Uani 1 1 d . . . H12 H 0.0967 0.1273 0.2801 0.036 Uiso 1 1 calc R . . C13 C 0.1885(2) 0.1583(4) 0.1372(4) 0.0277(14) Uani 1 1 d . . . C14 C 0.0000 0.1463(9) 0.6419(7) 0.040(2) Uani 1 2 d S . . Cl1 Cl 0.04548(18) 0.4945(6) 0.3694(7) 0.278(6) Uani 1 1 d . . . Cl2 Cl 0.0000 0.3468(11) 0.4439(10) 0.315(11) Uani 1 2 d S . . C15 C 0.0000 0.436(4) 0.367(3) 0.29(4) Uani 1 2 d S . . H15 H 0.0000 0.4016 0.3172 0.349 Uiso 1 2 calc SR . . 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 Ba1 0.0365(3) 0.0173(3) 0.0323(3) 0.000 0.0148(2) 0.000 Fe1 0.0189(8) 0.0277(10) 0.0275(9) 0.0084(8) 0.000 0.000 S1 0.0345(9) 0.0465(11) 0.0387(10) 0.0048(9) 0.0056(8) 0.0008(8) O1 0.044(3) 0.024(3) 0.044(3) 0.011(2) 0.012(2) 0.008(2) N1 0.039(3) 0.022(3) 0.036(3) 0.002(2) 0.002(3) 0.005(2) C1 0.037(4) 0.036(4) 0.044(4) 0.010(3) 0.012(3) 0.008(3) S2A 0.183(7) 0.078(4) 0.078(3) -0.035(3) 0.000 0.000 O2 0.051(3) 0.025(2) 0.034(3) 0.003(2) 0.017(2) 0.003(2) N2 0.040(3) 0.023(3) 0.039(3) 0.001(3) 0.016(3) -0.002(2) C2 0.044(4) 0.037(4) 0.057(5) 0.015(4) 0.014(4) 0.015(4) O3 0.088(7) 0.020(4) 0.053(5) 0.000 0.030(5) 0.000 N3 0.027(3) 0.030(3) 0.035(3) 0.006(2) 0.001(2) -0.001(2) C3 0.058(5) 0.026(4) 0.037(4) 0.010(3) 0.013(4) 0.013(3) N4 0.031(4) 0.032(5) 0.042(5) 0.003(4) 0.000 0.000 C4 0.055(5) 0.033(4) 0.039(4) 0.006(3) 0.006(4) 0.012(4) C5 0.061(5) 0.030(4) 0.037(4) 0.008(3) 0.023(4) 0.014(4) C6 0.051(5) 0.032(4) 0.051(5) 0.002(4) 0.030(4) 0.002(3) C7 0.030(3) 0.023(3) 0.036(4) 0.006(3) 0.013(3) 0.000(3) C8 0.021(3) 0.025(3) 0.035(4) 0.008(3) 0.011(3) 0.002(2) C9 0.029(3) 0.038(4) 0.035(4) 0.005(3) 0.008(3) -0.004(3) C10 0.031(3) 0.037(4) 0.030(4) 0.001(3) 0.005(3) -0.005(3) C11 0.030(3) 0.033(4) 0.033(4) 0.006(3) 0.003(3) -0.001(3) C12 0.028(3) 0.032(4) 0.031(3) 0.005(3) 0.006(3) 0.001(3) C13 0.038(4) 0.021(3) 0.024(3) 0.010(2) 0.009(3) 0.005(3) C14 0.039(6) 0.045(7) 0.038(6) 0.002(5) 0.000 0.000 Cl1 0.090(3) 0.202(7) 0.542(17) -0.191(10) 0.052(7) -0.030(4) Cl2 0.47(3) 0.236(16) 0.240(16) 0.109(13) 0.000 0.000 C15 0.048(13) 0.60(10) 0.22(4) -0.18(6) 0.000 0.000 _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 Ba1 O3 2.734(8) . ? Ba1 O1 2.772(6) . ? Ba1 O1 2.773(6) 8_545 ? Ba1 O2 2.785(5) . ? Ba1 O2 2.785(5) 8_545 ? Ba1 N1 2.889(6) 8_545 ? Ba1 N1 2.890(6) . ? Ba1 N2 2.923(6) . ? Ba1 N2 2.923(6) 8_545 ? Fe1 N4 2.101(10) . ? Fe1 N4 2.101(10) 9_556 ? Fe1 N3 2.229(6) 9_556 ? Fe1 N3 2.229(6) 11 ? Fe1 N3 2.229(6) 3_556 ? Fe1 N3 2.229(6) . ? S1 C13 1.627(8) . ? O1 C3 1.421(9) . ? O1 C2 1.426(9) . ? N1 C13 1.155(9) . ? C1 N2 1.474(11) . ? C1 C2 1.525(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? S2A C14 1.622(13) . ? O2 C5 1.437(9) . ? O2 C4 1.438(10) . ? N2 C7 1.475(9) . ? N2 C6 1.486(10) 8_545 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 H3 0.95(7) . ? N3 C10 1.327(9) . ? N3 C11 1.353(9) . ? C3 C4 1.509(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N4 C14 1.153(15) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.478(13) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N2 1.486(10) 8_545 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.519(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.389(10) . ? C8 C12 1.387(10) . ? C9 C10 1.381(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.380(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? Cl1 C15 1.63(3) . ? Cl2 C15 1.86(6) . ? C15 Cl1 1.63(3) 11 ? C15 H15 1.0000 . ? 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 O3 Ba1 O1 72.48(11) . . ? O3 Ba1 O1 72.48(11) . 8_545 ? O1 Ba1 O1 145.0(2) . 8_545 ? O3 Ba1 O2 67.69(11) . . ? O1 Ba1 O2 60.95(16) . . ? O1 Ba1 O2 104.89(16) 8_545 . ? O3 Ba1 O2 67.69(11) . 8_545 ? O1 Ba1 O2 104.89(16) . 8_545 ? O1 Ba1 O2 60.95(16) 8_545 8_545 ? O2 Ba1 O2 135.4(2) . 8_545 ? O3 Ba1 N1 139.59(12) . 8_545 ? O1 Ba1 N1 138.15(16) . 8_545 ? O1 Ba1 N1 73.35(16) 8_545 8_545 ? O2 Ba1 N1 143.10(16) . 8_545 ? O2 Ba1 N1 77.20(16) 8_545 8_545 ? O3 Ba1 N1 139.59(12) . . ? O1 Ba1 N1 73.35(16) . . ? O1 Ba1 N1 138.15(16) 8_545 . ? O2 Ba1 N1 77.20(16) . . ? O2 Ba1 N1 143.10(16) 8_545 . ? N1 Ba1 N1 80.8(2) 8_545 . ? O3 Ba1 N2 93.08(11) . . ? O1 Ba1 N2 60.76(17) . . ? O1 Ba1 N2 121.38(17) 8_545 . ? O2 Ba1 N2 121.67(18) . . ? O2 Ba1 N2 61.04(17) 8_545 . ? N1 Ba1 N2 86.70(18) 8_545 . ? N1 Ba1 N2 88.61(18) . . ? O3 Ba1 N2 93.08(11) . 8_545 ? O1 Ba1 N2 121.38(17) . 8_545 ? O1 Ba1 N2 60.76(17) 8_545 8_545 ? O2 Ba1 N2 61.04(17) . 8_545 ? O2 Ba1 N2 121.67(18) 8_545 8_545 ? N1 Ba1 N2 88.61(18) 8_545 8_545 ? N1 Ba1 N2 86.70(18) . 8_545 ? N2 Ba1 N2 173.8(2) . 8_545 ? N4 Fe1 N4 180.000(1) . 9_556 ? N4 Fe1 N3 90.6(2) . 9_556 ? N4 Fe1 N3 89.4(2) 9_556 9_556 ? N4 Fe1 N3 89.4(2) . 11 ? N4 Fe1 N3 90.6(2) 9_556 11 ? N3 Fe1 N3 89.3(3) 9_556 11 ? N4 Fe1 N3 90.6(2) . 3_556 ? N4 Fe1 N3 89.4(2) 9_556 3_556 ? N3 Fe1 N3 90.7(3) 9_556 3_556 ? N3 Fe1 N3 180.0(3) 11 3_556 ? N4 Fe1 N3 89.4(2) . . ? N4 Fe1 N3 90.6(2) 9_556 . ? N3 Fe1 N3 179.999(1) 9_556 . ? N3 Fe1 N3 90.7(3) 11 . ? N3 Fe1 N3 89.3(3) 3_556 . ? C3 O1 C2 113.5(6) . . ? C3 O1 Ba1 116.0(5) . . ? C2 O1 Ba1 116.6(5) . . ? C13 N1 Ba1 121.5(5) . . ? N2 C1 C2 112.4(7) . . ? N2 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N2 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? C5 O2 C4 112.6(6) . . ? C5 O2 Ba1 118.5(4) . . ? C4 O2 Ba1 112.3(4) . . ? C1 N2 C7 111.0(6) . . ? C1 N2 C6 110.8(6) . 8_545 ? C7 N2 C6 114.1(6) . 8_545 ? C1 N2 Ba1 111.7(4) . . ? C7 N2 Ba1 98.2(4) . . ? C6 N2 Ba1 110.5(4) 8_545 . ? O1 C2 C1 107.1(6) . . ? O1 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O1 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? Ba1 O3 H3 137(5) . . ? C10 N3 C11 116.8(6) . . ? C10 N3 Fe1 121.5(5) . . ? C11 N3 Fe1 121.4(5) . . ? O1 C3 C4 107.4(6) . . ? O1 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? O1 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C14 N4 Fe1 172.6(9) . . ? O2 C4 C3 108.2(7) . . ? O2 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O2 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? O2 C5 C6 110.0(6) . . ? O2 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? O2 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C5 C6 N2 113.5(7) . 8_545 ? C5 C6 H6A 108.9 . . ? N2 C6 H6A 108.9 8_545 . ? C5 C6 H6B 108.9 . . ? N2 C6 H6B 108.9 8_545 . ? H6A C6 H6B 107.7 . . ? N2 C7 C8 116.5(6) . . ? N2 C7 H7A 108.2 . . ? C8 C7 H7A 108.2 . . ? N2 C7 H7B 108.2 . . ? C8 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? C9 C8 C12 116.9(6) . . ? C9 C8 C7 122.3(7) . . ? C12 C8 C7 120.7(6) . . ? C10 C9 C8 119.4(7) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N3 C10 C9 124.0(7) . . ? N3 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? N3 C11 C12 122.6(7) . . ? N3 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C8 120.1(7) . . ? C11 C12 H12 120.0 . . ? C8 C12 H12 120.0 . . ? N1 C13 S1 179.4(7) . . ? N4 C14 S2A 179.4(12) . . ? Cl1 C15 Cl1 117(4) . 11 ? Cl1 C15 Cl2 110(2) . . ? Cl1 C15 Cl2 110(2) 11 . ? Cl1 C15 H15 106.2 . . ? Cl1 C15 H15 106.2 11 . ? Cl2 C15 H15 106.1 . . ? 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 N1 0.95(7) 2.02(6) 2.961(8) 173(8) 15 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.775 _refine_diff_density_min -1.575 _refine_diff_density_rms 0.187 #===END #========================================================================== data_F _database_code_depnum_ccdc_archive 'CCDC 735056' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 Ca Cl4 Co N4 O6' _chemical_formula_sum 'C24 H40 Ca Cl4 Co N4 O6' _chemical_formula_weight 721.42 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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 orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 12.474(3) _cell_length_b 13.189(3) _cell_length_c 27.709(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4558.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 111 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 31.34 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8341 _exptl_absorpt_correction_T_max 0.8640 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28839 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5611 _reflns_number_gt 2847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _computing_structure_refinement X-SEED _computing_molecular_graphics 'MERCURY 1.4 (Bruno et al., 2002)' _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5611 _refine_ls_number_parameters 193 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1535 _refine_ls_R_factor_gt 0.1130 _refine_ls_wR_factor_ref 0.3259 _refine_ls_wR_factor_gt 0.3024 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.084 _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 0.5000 0.5000 0.0000 0.0323(3) Uani 1 2 d S . . Cl1 Cl 0.5410(3) 0.3445(3) -0.00419(13) 0.1621(13) Uani 1 1 d . . . O1 O 0.3685(3) 0.4709(4) -0.04583(13) 0.0636(12) Uani 1 1 d . . . N1 N 0.3990(3) 0.4649(3) 0.06079(13) 0.0343(9) Uani 1 1 d . . . C1 C 0.4365(4) 0.4131(4) 0.09821(16) 0.0398(11) Uani 1 1 d . . . H1 H 0.5094 0.3922 0.0979 0.048 Uiso 1 1 calc R . . Ca2 Ca 0.0000 0.25643(9) 0.2500 0.0297(4) Uani 1 2 d S . . Cl2 Cl -0.0933(3) 0.3943(2) 0.21503(11) 0.1452(11) Uani 1 1 d . . . O2 O 0.1480(5) 0.1369(5) 0.24378(16) 0.103(2) Uani 1 1 d U . . N2 N 0.1363(3) 0.2878(3) 0.17359(13) 0.0391(10) Uani 1 1 d . . . C2 C 0.3719(4) 0.3875(4) 0.13892(18) 0.0448(12) Uani 1 1 d . . . H2 H 0.4018 0.3511 0.1653 0.054 Uiso 1 1 calc R . . O3 O -0.0591(3) 0.1859(3) 0.17247(12) 0.0502(10) Uani 1 1 d . . . C3 C 0.2677(4) 0.4156(3) 0.13961(15) 0.0332(10) Uani 1 1 d . . . C4 C 0.2288(4) 0.4711(4) 0.09956(17) 0.0383(11) Uani 1 1 d . . . H4 H 0.1561 0.4926 0.0989 0.046 Uiso 1 1 calc R . . C5 C 0.2948(4) 0.4941(3) 0.06193(18) 0.0380(11) Uani 1 1 d . . . H5 H 0.2668 0.5318 0.0356 0.046 Uiso 1 1 calc R . . C6 C 0.1926(4) 0.3843(3) 0.18027(16) 0.0359(10) Uani 1 1 d . . . H6A H 0.2346 0.3803 0.2105 0.043 Uiso 1 1 calc R . . H6B H 0.1384 0.4384 0.1845 0.043 Uiso 1 1 calc R . . C7 C 0.2073(5) 0.2014(4) 0.1707(3) 0.071(2) Uani 1 1 d . . . H7A H 0.1689 0.1453 0.1544 0.086 Uiso 1 1 calc R . . H7B H 0.2695 0.2198 0.1503 0.086 Uiso 1 1 calc R . . C8 C 0.2452(6) 0.1666(6) 0.2155(4) 0.092(3) Uani 1 1 d . . . H8A H 0.2852 0.2208 0.2323 0.110 Uiso 1 1 calc R . . H8B H 0.2933 0.1076 0.2110 0.110 Uiso 1 1 calc R . . C9 C 0.0651(5) 0.2929(5) 0.13018(17) 0.0587(16) Uani 1 1 d . . . H9A H 0.0218 0.3557 0.1316 0.070 Uiso 1 1 calc R . . H9B H 0.1099 0.2960 0.1007 0.070 Uiso 1 1 calc R . . C10 C -0.0080(5) 0.2040(6) 0.1268(2) 0.075(2) Uani 1 1 d . . . H10A H -0.0632 0.2168 0.1019 0.090 Uiso 1 1 calc R . . H10B H 0.0333 0.1433 0.1171 0.090 Uiso 1 1 calc R . . C11 C -0.1250(5) 0.0995(5) 0.1732(2) 0.072(2) Uani 1 1 d . . . H11A H -0.1037 0.0530 0.1468 0.086 Uiso 1 1 calc R A 1 H11B H -0.2005 0.1197 0.1678 0.086 Uiso 1 1 calc R A 1 C12A C -0.1149(13) 0.0435(11) 0.2229(6) 0.086(4) Uani 0.50 1 d P . 1 H12C H -0.0409 0.0199 0.2294 0.104 Uiso 0.50 1 calc PR . 1 H12D H -0.1656 -0.0140 0.2258 0.104 Uiso 0.50 1 calc PR . 1 C12B C -0.2300(15) 0.1292(16) 0.2046(6) 0.125(8) Uani 0.50 1 d P . 2 H12A H -0.2846 0.0748 0.2062 0.150 Uiso 0.50 1 calc PR . 2 H12B H -0.2629 0.1946 0.1951 0.150 Uiso 0.50 1 calc PR . 2 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 0.0334(6) 0.0436(6) 0.0200(5) 0.0011(3) 0.0068(3) -0.0067(4) Cl1 0.183(3) 0.152(3) 0.151(3) 0.013(2) 0.023(2) -0.014(3) O1 0.047(2) 0.117(4) 0.0269(19) -0.007(2) 0.0059(15) -0.008(2) N1 0.038(2) 0.042(2) 0.0224(18) 0.0044(17) 0.0089(15) -0.0073(18) C1 0.034(3) 0.056(3) 0.030(2) 0.011(2) 0.0095(19) 0.002(2) Ca2 0.0298(7) 0.0340(7) 0.0254(6) 0.000 0.0041(5) 0.000 Cl2 0.160(2) 0.157(3) 0.119(2) 0.0180(18) 0.0186(18) 0.0278(19) O2 0.135(4) 0.127(4) 0.048(3) 0.040(3) 0.039(3) 0.097(4) N2 0.057(3) 0.028(2) 0.033(2) -0.0047(16) 0.0163(18) -0.0092(17) C2 0.051(3) 0.052(3) 0.032(3) 0.008(2) 0.005(2) -0.006(2) O3 0.056(2) 0.060(2) 0.0339(19) -0.0179(16) 0.0135(16) -0.0250(18) C3 0.040(3) 0.034(2) 0.025(2) -0.0008(19) 0.0142(19) -0.007(2) C4 0.029(2) 0.045(3) 0.041(3) -0.007(2) 0.013(2) -0.003(2) C5 0.041(3) 0.036(3) 0.037(3) 0.001(2) 0.002(2) 0.002(2) C6 0.044(3) 0.036(2) 0.028(2) -0.0023(19) 0.0090(19) -0.011(2) C7 0.077(4) 0.036(3) 0.102(6) -0.010(3) 0.066(4) -0.002(3) C8 0.080(5) 0.058(4) 0.136(8) -0.033(5) -0.012(5) 0.028(4) C9 0.075(4) 0.076(4) 0.025(3) -0.014(3) 0.013(2) -0.030(3) C10 0.093(5) 0.095(5) 0.036(3) -0.022(3) 0.019(3) -0.056(4) C11 0.075(4) 0.083(5) 0.057(4) -0.028(3) 0.035(3) -0.045(3) C12A 0.110(12) 0.058(8) 0.091(12) 0.001(8) 0.025(9) 0.009(8) C12B 0.151(17) 0.156(17) 0.068(11) -0.050(11) 0.039(11) -0.073(14) _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 O1 2.110(4) 5_665 ? Co1 O1 2.110(4) . ? Co1 Cl1 2.116(4) 5_665 ? Co1 Cl1 2.116(4) . ? Co1 N1 2.154(3) . ? Co1 N1 2.154(3) 5_665 ? N1 C1 1.327(6) . ? N1 C5 1.356(6) . ? C1 C2 1.427(6) . ? C1 H1 0.9500 . ? Ca2 Cl2 2.366(3) . ? Ca2 Cl2 2.366(3) 4 ? Ca2 O2 2.434(4) 4 ? Ca2 O2 2.434(4) . ? Ca2 O3 2.454(3) 4 ? Ca2 O3 2.454(3) . ? Ca2 N2 2.747(3) 4 ? Ca2 N2 2.747(3) . ? O2 C8 1.496(10) . ? O2 C12A 1.593(16) 4 ? O2 C12B 1.76(2) 4 ? N2 C7 1.445(7) . ? N2 C6 1.466(5) . ? N2 C9 1.497(6) . ? C2 C3 1.351(7) . ? C2 H2 0.9500 . ? O3 C11 1.405(6) . ? O3 C10 1.436(6) . ? C3 C4 1.416(6) . ? C3 C6 1.522(6) . ? C4 C5 1.362(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.406(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.487(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12A 1.569(17) . ? C11 C12B 1.620(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12A O2 1.593(16) 4 ? C12A H12C 0.9900 . ? C12A H12D 0.9900 . ? C12B O2 1.76(2) 4 ? C12B H12A 0.9900 . ? C12B H12B 0.9900 . ? 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 O1 Co1 O1 180.0(2) 5_665 . ? O1 Co1 Cl1 88.76(18) 5_665 5_665 ? O1 Co1 Cl1 91.24(18) . 5_665 ? O1 Co1 Cl1 91.24(18) 5_665 . ? O1 Co1 Cl1 88.76(18) . . ? Cl1 Co1 Cl1 180.0 5_665 . ? O1 Co1 N1 91.34(14) 5_665 . ? O1 Co1 N1 88.66(14) . . ? Cl1 Co1 N1 91.38(14) 5_665 . ? Cl1 Co1 N1 88.62(14) . . ? O1 Co1 N1 88.66(14) 5_665 5_665 ? O1 Co1 N1 91.34(14) . 5_665 ? Cl1 Co1 N1 88.61(14) 5_665 5_665 ? Cl1 Co1 N1 91.39(14) . 5_665 ? N1 Co1 N1 180.0 . 5_665 ? C1 N1 C5 117.8(4) . . ? C1 N1 Co1 121.0(3) . . ? C5 N1 Co1 121.2(3) . . ? N1 C1 C2 122.7(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? Cl2 Ca2 Cl2 79.58(17) . 4 ? Cl2 Ca2 O2 98.8(2) . 4 ? Cl2 Ca2 O2 147.33(13) 4 4 ? Cl2 Ca2 O2 147.33(13) . . ? Cl2 Ca2 O2 98.8(2) 4 . ? O2 Ca2 O2 99.2(4) 4 . ? Cl2 Ca2 O3 142.89(12) . 4 ? Cl2 Ca2 O3 77.59(13) 4 4 ? O2 Ca2 O3 85.43(17) 4 4 ? O2 Ca2 O3 65.70(12) . 4 ? Cl2 Ca2 O3 77.59(13) . . ? Cl2 Ca2 O3 142.89(12) 4 . ? O2 Ca2 O3 65.70(12) 4 . ? O2 Ca2 O3 85.43(17) . . ? O3 Ca2 O3 135.45(19) 4 . ? Cl2 Ca2 N2 84.00(11) . 4 ? Cl2 Ca2 N2 82.70(11) 4 4 ? O2 Ca2 N2 64.75(14) 4 4 ? O2 Ca2 N2 128.44(13) . 4 ? O3 Ca2 N2 64.44(11) 4 4 ? O3 Ca2 N2 123.07(11) . 4 ? Cl2 Ca2 N2 82.70(11) . . ? Cl2 Ca2 N2 84.00(11) 4 . ? O2 Ca2 N2 128.44(13) 4 . ? O2 Ca2 N2 64.75(14) . . ? O3 Ca2 N2 123.07(11) 4 . ? O3 Ca2 N2 64.44(11) . . ? N2 Ca2 N2 162.67(16) 4 . ? C8 O2 C12A 135.7(7) . 4 ? C8 O2 C12B 88.3(7) . 4 ? C12A O2 C12B 68.6(9) 4 4 ? C8 O2 Ca2 118.8(4) . . ? C12A O2 Ca2 105.3(6) 4 . ? C12B O2 Ca2 114.8(6) 4 . ? C7 N2 C6 113.5(4) . . ? C7 N2 C9 110.7(5) . . ? C6 N2 C9 110.3(4) . . ? C7 N2 Ca2 107.7(3) . . ? C6 N2 Ca2 109.3(2) . . ? C9 N2 Ca2 105.0(3) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C11 O3 C10 114.0(4) . . ? C11 O3 Ca2 118.1(3) . . ? C10 O3 Ca2 125.0(3) . . ? C2 C3 C4 117.4(4) . . ? C2 C3 C6 121.9(4) . . ? C4 C3 C6 120.6(4) . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? N1 C5 C4 122.3(4) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N2 C6 C3 115.9(4) . . ? N2 C6 H6A 108.3 . . ? C3 C6 H6A 108.3 . . ? N2 C6 H6B 108.3 . . ? C3 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C8 C7 N2 114.5(5) . . ? C8 C7 H7A 108.6 . . ? N2 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? N2 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 O2 106.0(5) . . ? C7 C8 H8A 110.5 . . ? O2 C8 H8A 110.5 . . ? C7 C8 H8B 110.5 . . ? O2 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? C10 C9 N2 112.3(5) . . ? C10 C9 H9A 109.2 . . ? N2 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? N2 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? O3 C10 C9 110.4(4) . . ? O3 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O3 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? O3 C11 C12A 110.4(8) . . ? O3 C11 C12B 106.5(8) . . ? C12A C11 C12B 73.0(10) . . ? O3 C11 H11A 109.6 . . ? C12A C11 H11A 109.6 . . ? C12B C11 H11A 139.6 . . ? O3 C11 H11B 109.6 . . ? C12A C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C11 C12A O2 97.1(9) . 4 ? C11 C12A H12C 112.3 . . ? O2 C12A H12C 112.3 4 . ? C11 C12A H12D 112.3 . . ? O2 C12A H12D 112.3 4 . ? H12C C12A H12D 109.9 . . ? C11 C12B O2 88.8(10) . 4 ? C11 C12B H12A 113.8 . . ? O2 C12B H12A 113.8 4 . ? C11 C12B H12B 113.8 . . ? O2 C12B H12B 113.8 4 . ? H12A C12B H12B 111.1 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.460 _refine_diff_density_min -1.287 _refine_diff_density_rms 0.244 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.043 0.444 -0.013 1813 1267 ' ' _platon_squeeze_details ; ; #===END #========================================================================== data_G _database_code_depnum_ccdc_archive 'CCDC 735057' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 Cl2 Co K N4 O6, 2(H2 O), (Cl)' _chemical_formula_sum 'C24 H44 Cl3 Co K N4 O8' _chemical_formula_weight 721.01 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 9.4628(1) _cell_length_b 9.9583(1) _cell_length_c 10.5733(2) _cell_angle_alpha 104.956(1) _cell_angle_beta 112.965(1) _cell_angle_gamma 101.559(1) _cell_volume 834.01(2) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 111 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 30.81 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 377 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7525 _exptl_absorpt_correction_T_max 0.8929 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15460 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 30.48 _reflns_number_total 5014 _reflns_number_gt 4300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _computing_structure_refinement X-SEED _computing_molecular_graphics 'MERCURY 1.4 (Bruno et al., 2002)' _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. There is one water molecule in the asym unit which is disordered over two sites (50:50 occupied), all other atoms are ordered. Cl2 was set at half occupancy. The highest residual peak is 0.46 A from CL2. ; _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^)+(0.0739P)^2^+1.7946P] 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 5014 _refine_ls_number_parameters 214 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.075 _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 0.5000 0.0000 0.0000 0.01227(12) Uani 1 2 d S . . K1 K 1.5000 0.5000 1.0000 0.01486(15) Uani 1 2 d S . . Cl1 Cl 0.39939(8) -0.22001(6) 0.04452(6) 0.01835(14) Uani 1 1 d . . . O1 O 1.1931(2) 0.4134(2) 0.9925(2) 0.0186(4) Uani 1 1 d . . . N1 N 1.2006(3) 0.4049(2) 0.7152(2) 0.0149(4) Uani 1 1 d . . . C1 C 1.1766(3) 0.3448(3) 1.0907(3) 0.0188(5) Uani 1 1 d . . . H1A H 1.1689 0.2403 1.0531 0.023 Uiso 1 1 calc R . . H1B H 1.0760 0.3475 1.0981 0.023 Uiso 1 1 calc R . . Cl2 Cl 0.36808(15) 0.11968(14) 0.38995(14) 0.0188(2) Uani 0.50 1 d P . . O2 O 1.5317(2) 0.5759(2) 0.77200(19) 0.0157(3) Uani 1 1 d . . . N2 N 0.7215(3) 0.0734(2) 0.2052(2) 0.0152(4) Uani 1 1 d . . . C2 C 1.0475(3) 0.3571(3) 0.8559(3) 0.0192(5) Uani 1 1 d . . . H2A H 0.9566 0.3757 0.8734 0.023 Uiso 1 1 calc R . . H2B H 1.0189 0.2492 0.8082 0.023 Uiso 1 1 calc R . . O3 O 0.3932(2) 0.1150(2) 0.1109(2) 0.0176(3) Uani 1 1 d D . . C3 C 1.0741(3) 0.4329(3) 0.7561(3) 0.0182(5) Uani 1 1 d . . . H3A H 0.9699 0.3998 0.6644 0.022 Uiso 1 1 calc R . . H3B H 1.1047 0.5407 0.8064 0.022 Uiso 1 1 calc R . . O4A O 1.6138(8) 0.2014(6) 0.6520(6) 0.0291(11) Uani 0.50 1 d PD A 1 C4 C 1.2389(3) 0.5066(3) 0.6447(3) 0.0180(5) Uani 1 1 d . . . H4A H 1.2506 0.6070 0.7037 0.022 Uiso 1 1 calc R . . H4B H 1.1457 0.4759 0.5452 0.022 Uiso 1 1 calc R . . C5 C 1.3922(3) 0.5141(3) 0.6287(3) 0.0187(5) Uani 1 1 d . . . H5A H 1.3853 0.4137 0.5748 0.022 Uiso 1 1 calc R . . H5B H 1.4028 0.5759 0.5709 0.022 Uiso 1 1 calc R . . C6 C 1.6771(3) 0.5735(3) 0.7598(3) 0.0187(5) Uani 1 1 d . . . H6A H 1.6858 0.6204 0.6900 0.022 Uiso 1 1 calc R . . H6B H 1.6722 0.4700 0.7208 0.022 Uiso 1 1 calc R . . C7 C 1.1609(3) 0.2473(3) 0.6269(3) 0.0154(4) Uani 1 1 d . . . H7A H 1.1486 0.1878 0.6863 0.019 Uiso 1 1 calc R . . H7B H 1.2542 0.2371 0.6092 0.019 Uiso 1 1 calc R . . C8 C 1.0074(3) 0.1832(3) 0.4785(3) 0.0149(4) Uani 1 1 d . . . C9 C 0.8547(3) 0.1252(3) 0.4667(3) 0.0177(5) Uani 1 1 d . . . H9 H 0.8447 0.1221 0.5520 0.021 Uiso 1 1 calc R . . C10 C 0.7163(3) 0.0718(3) 0.3301(3) 0.0175(5) Uani 1 1 d . . . H10 H 0.6131 0.0322 0.3247 0.021 Uiso 1 1 calc R . . C11 C 0.8691(3) 0.1265(3) 0.2158(3) 0.0200(5) Uani 1 1 d . . . H11 H 0.8756 0.1271 0.1285 0.024 Uiso 1 1 calc R . . C12 C 1.0129(3) 0.1808(3) 0.3479(3) 0.0203(5) Uani 1 1 d . . . H12 H 1.1148 0.2161 0.3494 0.024 Uiso 1 1 calc R . . O4B O 1.6778(6) 0.1773(7) 0.6853(6) 0.0322(12) Uani 0.50 1 d PD B 2 HO3A H 0.374(5) 0.117(4) 0.187(3) 0.039 Uiso 1 1 d D . . HO3B H 0.408(5) 0.212(2) 0.135(4) 0.039 Uiso 1 1 d D . . HO4A H 1.639(4) 0.218(4) 0.752(2) 0.039 Uiso 1 1 d D . . HO4B H 1.581(3) 0.102(2) 0.648(4) 0.039 Uiso 1 1 d 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 0.0124(2) 0.0108(2) 0.0104(2) 0.00229(16) 0.00383(16) 0.00283(15) K1 0.0149(3) 0.0172(3) 0.0125(3) 0.0064(2) 0.0058(2) 0.0054(3) Cl1 0.0238(3) 0.0120(3) 0.0166(3) 0.0045(2) 0.0087(2) 0.0032(2) O1 0.0168(8) 0.0235(9) 0.0136(8) 0.0086(7) 0.0057(7) 0.0040(7) N1 0.0147(9) 0.0150(9) 0.0122(9) 0.0044(7) 0.0041(7) 0.0044(7) C1 0.0178(11) 0.0227(12) 0.0214(12) 0.0115(10) 0.0116(9) 0.0082(9) Cl2 0.0199(5) 0.0228(6) 0.0263(6) 0.0137(5) 0.0153(5) 0.0167(5) O2 0.0164(8) 0.0177(8) 0.0114(7) 0.0039(6) 0.0065(6) 0.0046(6) N2 0.0145(9) 0.0148(9) 0.0121(9) 0.0032(7) 0.0044(7) 0.0030(7) C2 0.0154(11) 0.0233(12) 0.0147(11) 0.0046(9) 0.0052(9) 0.0053(9) O3 0.0226(9) 0.0157(8) 0.0176(8) 0.0063(7) 0.0115(7) 0.0083(7) C3 0.0177(11) 0.0197(11) 0.0149(10) 0.0054(9) 0.0052(9) 0.0079(9) O4A 0.039(3) 0.022(2) 0.026(3) 0.0096(18) 0.017(2) 0.006(2) C4 0.0184(11) 0.0164(11) 0.0139(10) 0.0061(9) 0.0034(9) 0.0031(9) C5 0.0210(11) 0.0183(11) 0.0107(10) 0.0038(9) 0.0047(9) 0.0023(9) C6 0.0233(12) 0.0240(12) 0.0162(11) 0.0096(9) 0.0131(10) 0.0116(10) C7 0.0148(10) 0.0145(10) 0.0130(10) 0.0042(8) 0.0036(8) 0.0044(8) C8 0.0139(10) 0.0138(10) 0.0120(10) 0.0027(8) 0.0036(8) 0.0030(8) C9 0.0158(11) 0.0214(12) 0.0115(10) 0.0041(9) 0.0054(9) 0.0023(9) C10 0.0145(10) 0.0209(11) 0.0145(10) 0.0050(9) 0.0064(9) 0.0034(9) C11 0.0172(11) 0.0252(13) 0.0131(10) 0.0055(9) 0.0064(9) 0.0017(9) C12 0.0141(11) 0.0269(13) 0.0151(11) 0.0053(10) 0.0061(9) 0.0019(9) O4B 0.023(3) 0.044(3) 0.020(2) 0.004(2) 0.012(2) -0.001(2) _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 O3 2.0979(18) 2_655 ? Co1 O3 2.0979(18) . ? Co1 N2 2.158(2) 2_655 ? Co1 N2 2.158(2) . ? Co1 Cl1 2.4442(6) 2_655 ? Co1 Cl1 2.4442(6) . ? K1 O2 2.8084(17) 2_867 ? K1 O2 2.8084(17) . ? K1 O1 2.8219(18) . ? K1 O1 2.8219(18) 2_867 ? K1 N1 2.964(2) . ? K1 N1 2.964(2) 2_867 ? K1 Cl1 3.1046(6) 1_666 ? K1 Cl1 3.1046(6) 2_756 ? Cl1 K1 3.1046(6) 1_444 ? O1 C2 1.421(3) . ? O1 C1 1.421(3) . ? N1 C4 1.473(3) . ? N1 C3 1.473(3) . ? N1 C7 1.486(3) . ? C1 C6 1.502(4) 2_867 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C5 1.432(3) . ? O2 C6 1.435(3) . ? N2 C11 1.339(3) . ? N2 C10 1.345(3) . ? C2 C3 1.513(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 HO3A 0.886(18) . ? O3 HO3B 0.898(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4A HO4A 0.953(17) . ? O4A HO4B 0.961(17) . ? C4 C5 1.514(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C1 1.502(4) 2_867 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.388(3) . ? C8 C12 1.396(3) . ? C9 C10 1.390(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.388(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? O4B HO4A 0.956(17) . ? O4B HO4B 0.918(18) . ? 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 O3 Co1 O3 180.00(8) 2_655 . ? O3 Co1 N2 90.45(8) 2_655 2_655 ? O3 Co1 N2 89.55(8) . 2_655 ? O3 Co1 N2 89.55(8) 2_655 . ? O3 Co1 N2 90.45(8) . . ? N2 Co1 N2 180.00(11) 2_655 . ? O3 Co1 Cl1 90.84(5) 2_655 2_655 ? O3 Co1 Cl1 89.16(5) . 2_655 ? N2 Co1 Cl1 89.54(6) 2_655 2_655 ? N2 Co1 Cl1 90.46(6) . 2_655 ? O3 Co1 Cl1 89.16(5) 2_655 . ? O3 Co1 Cl1 90.84(5) . . ? N2 Co1 Cl1 90.46(6) 2_655 . ? N2 Co1 Cl1 89.54(6) . . ? Cl1 Co1 Cl1 180.00(2) 2_655 . ? O2 K1 O2 180.000(1) 2_867 . ? O2 K1 O1 58.98(5) 2_867 . ? O2 K1 O1 121.02(5) . . ? O2 K1 O1 121.02(5) 2_867 2_867 ? O2 K1 O1 58.98(5) . 2_867 ? O1 K1 O1 180.0 . 2_867 ? O2 K1 N1 117.65(6) 2_867 . ? O2 K1 N1 62.35(5) . . ? O1 K1 N1 61.01(5) . . ? O1 K1 N1 118.99(5) 2_867 . ? O2 K1 N1 62.35(5) 2_867 2_867 ? O2 K1 N1 117.65(5) . 2_867 ? O1 K1 N1 118.99(5) . 2_867 ? O1 K1 N1 61.01(5) 2_867 2_867 ? N1 K1 N1 180.000(1) . 2_867 ? O2 K1 Cl1 98.94(4) 2_867 1_666 ? O2 K1 Cl1 81.06(4) . 1_666 ? O1 K1 Cl1 73.79(4) . 1_666 ? O1 K1 Cl1 106.21(4) 2_867 1_666 ? N1 K1 Cl1 79.20(4) . 1_666 ? N1 K1 Cl1 100.80(4) 2_867 1_666 ? O2 K1 Cl1 81.06(4) 2_867 2_756 ? O2 K1 Cl1 98.94(4) . 2_756 ? O1 K1 Cl1 106.21(4) . 2_756 ? O1 K1 Cl1 73.79(4) 2_867 2_756 ? N1 K1 Cl1 100.80(4) . 2_756 ? N1 K1 Cl1 79.20(4) 2_867 2_756 ? Cl1 K1 Cl1 180.0 1_666 2_756 ? Co1 Cl1 K1 127.22(2) . 1_444 ? C2 O1 C1 111.6(2) . . ? C2 O1 K1 120.29(14) . . ? C1 O1 K1 118.71(14) . . ? C4 N1 C3 109.3(2) . . ? C4 N1 C7 113.54(19) . . ? C3 N1 C7 113.6(2) . . ? C4 N1 K1 104.71(14) . . ? C3 N1 K1 105.29(14) . . ? C7 N1 K1 109.61(13) . . ? O1 C1 C6 108.6(2) . 2_867 ? O1 C1 H1A 110.0 . . ? C6 C1 H1A 110.0 2_867 . ? O1 C1 H1B 110.0 . . ? C6 C1 H1B 110.0 2_867 . ? H1A C1 H1B 108.4 . . ? C5 O2 C6 110.69(19) . . ? C5 O2 K1 117.82(14) . . ? C6 O2 K1 116.82(14) . . ? C11 N2 C10 117.0(2) . . ? C11 N2 Co1 122.17(17) . . ? C10 N2 Co1 120.79(16) . . ? O1 C2 C3 108.9(2) . . ? O1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? Co1 O3 HO3A 136(2) . . ? Co1 O3 HO3B 126(2) . . ? HO3A O3 HO3B 90(2) . . ? N1 C3 C2 114.4(2) . . ? N1 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? HO4A O4A HO4B 78.4(18) . . ? N1 C4 C5 114.7(2) . . ? N1 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? N1 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? O2 C5 C4 109.8(2) . . ? O2 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? O2 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O2 C6 C1 109.6(2) . 2_867 ? O2 C6 H6A 109.8 . . ? C1 C6 H6A 109.8 2_867 . ? O2 C6 H6B 109.8 . . ? C1 C6 H6B 109.8 2_867 . ? H6A C6 H6B 108.2 . . ? N1 C7 C8 115.11(19) . . ? N1 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C9 C8 C12 116.8(2) . . ? C9 C8 C7 121.4(2) . . ? C12 C8 C7 121.8(2) . . ? C8 C9 C10 119.9(2) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? N2 C10 C9 123.1(2) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N2 C11 C12 123.3(2) . . ? N2 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C8 119.8(2) . . ? C11 C12 H12 120.1 . . ? C8 C12 H12 120.1 . . ? HO4A O4B HO4B 80.4(18) . . ? 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 HO3A Cl2 0.886(18) 2.164(19) 3.041(2) 170(4) . O3 HO3B O2 0.898(18) 1.94(2) 2.826(3) 169(4) 2_766 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.253 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.123 #===END #========================================================================== data_H _database_code_depnum_ccdc_archive 'CCDC 735058' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 Co N6 O6 S2' _chemical_formula_sum 'C26 H40 Co N6 O6 S2' _chemical_formula_weight 655.69 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 monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1581(4) _cell_length_b 18.2060(7) _cell_length_c 10.1529(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.964(1) _cell_angle_gamma 90.00 _cell_volume 1521.96(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 205 _cell_measurement_theta_min 2.496 _cell_measurement_theta_max 26.988 _exptl_crystal_description prism _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7957 _exptl_absorpt_correction_T_max 0.8940 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13984 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.15 _reflns_number_total 3304 _reflns_number_gt 2976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker Apex II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-seed (Barbour, 1999)' _computing_publication_material 'X-seed (Barbour, 1999)' _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. The hydrogen atoms on the cobalt bound water molecule were located in the difference map. The O-H bond lengths were fixed to 0.95. ; _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^)+(0.0229P)^2^+3.1461P] 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 3304 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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 0.0000 0.0000 0.01860(15) Uani 1 2 d S . . S1 S -0.00554(11) 0.16195(5) -0.37070(10) 0.0362(2) Uani 1 1 d . . . O1 O 0.0423(3) 0.48890(12) 0.8193(2) 0.0320(5) Uani 1 1 d . . . N1 N 0.0539(3) 0.36982(14) 0.3133(3) 0.0252(6) Uani 1 1 d . . . C1 C 0.0417(4) 0.61791(18) 0.8450(4) 0.0352(8) Uani 1 1 d . . . H1A H -0.0336 0.6151 0.8911 0.042 Uiso 1 1 calc R . . H1B H 0.1134 0.6609 0.8873 0.042 Uiso 1 1 calc R . . H3AO H 0.308(6) -0.041(3) 0.100(5) 0.072(16) Uiso 1 1 d . . . H3BO H 0.298(5) 0.025(2) 0.059(5) 0.042(13) Uiso 1 1 d . . . O2 O -0.0587(3) 0.37095(12) 0.6166(2) 0.0300(5) Uani 1 1 d . . . N2 N 0.0402(3) 0.10778(13) 0.1038(3) 0.0200(5) Uani 1 1 d . . . C2 C 0.1444(4) 0.54977(18) 0.8839(4) 0.0362(8) Uani 1 1 d . . . H2A H 0.2280 0.5535 0.8471 0.043 Uiso 1 1 calc R . . H2B H 0.2001 0.5438 0.9916 0.043 Uiso 1 1 calc R . . O3 O 0.2467(3) -0.00561(13) 0.0419(3) 0.0245(5) Uani 1 1 d . . . N3 N -0.0446(3) 0.05116(14) -0.1989(3) 0.0262(6) Uani 1 1 d . . . C3 C 0.1303(4) 0.42170(18) 0.8532(4) 0.0339(8) Uani 1 1 d . . . H3A H 0.1784 0.4126 0.9601 0.041 Uiso 1 1 calc R . . H3B H 0.2193 0.4241 0.8230 0.041 Uiso 1 1 calc R . . C4 C 0.0155(4) 0.36151(18) 0.7732(4) 0.0344(8) Uani 1 1 d . . . H4A H 0.0746 0.3142 0.7978 0.041 Uiso 1 1 calc R . . H4B H -0.0708 0.3591 0.8068 0.041 Uiso 1 1 calc R . . C5 C 0.0513(4) 0.36029(19) 0.5549(4) 0.0316(7) Uani 1 1 d . . . H5A H 0.1132 0.3143 0.5924 0.038 Uiso 1 1 calc R . . H5B H 0.1291 0.4017 0.5811 0.038 Uiso 1 1 calc R . . C6 C -0.0474(4) 0.35605(18) 0.3892(4) 0.0289(7) Uani 1 1 d . . . H6A H -0.0973 0.3067 0.3621 0.035 Uiso 1 1 calc R . . H6B H -0.1360 0.3927 0.3574 0.035 Uiso 1 1 calc R . . C7 C 0.1801(4) 0.31385(16) 0.3410(4) 0.0268(7) Uani 1 1 d . . . H7A H 0.2315 0.3025 0.4470 0.032 Uiso 1 1 calc R . . H7B H 0.2649 0.3355 0.3173 0.032 Uiso 1 1 calc R . . C8 C 0.1252(4) 0.24198(16) 0.2574(3) 0.0244(6) Uani 1 1 d . . . C9 C 0.0602(4) 0.18433(17) 0.3032(3) 0.0274(7) Uani 1 1 d . . . H9 H 0.0426 0.1894 0.3883 0.033 Uiso 1 1 calc R . . C10 C 0.0209(4) 0.11908(16) 0.2248(3) 0.0257(6) Uani 1 1 d . . . H10 H -0.0223 0.0802 0.2594 0.031 Uiso 1 1 calc R . . C11 C 0.1008(4) 0.16461(16) 0.0576(3) 0.0250(6) Uani 1 1 d . . . H11 H 0.1147 0.1585 -0.0292 0.030 Uiso 1 1 calc R . . C12 C 0.1435(4) 0.23101(17) 0.1302(3) 0.0266(7) Uani 1 1 d . . . H12 H 0.1855 0.2693 0.0930 0.032 Uiso 1 1 calc R . . C16 C -0.0293(4) 0.09562(16) -0.2729(3) 0.0233(6) 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 0.0235(3) 0.0128(3) 0.0183(3) -0.0005(2) 0.0081(2) -0.0003(2) S1 0.0408(5) 0.0343(5) 0.0368(5) 0.0112(4) 0.0199(4) -0.0003(4) O1 0.0327(12) 0.0245(12) 0.0313(12) -0.0016(9) 0.0069(10) 0.0004(9) N1 0.0293(13) 0.0200(12) 0.0247(13) -0.0039(10) 0.0104(11) 0.0004(10) C1 0.0445(19) 0.0255(16) 0.0266(17) -0.0063(13) 0.0073(15) -0.0003(14) O2 0.0341(12) 0.0270(12) 0.0303(12) -0.0004(9) 0.0152(10) -0.0012(9) N2 0.0245(12) 0.0163(11) 0.0193(12) 0.0000(9) 0.0096(10) 0.0017(9) C2 0.0413(19) 0.0260(17) 0.0297(17) -0.0032(14) 0.0050(15) -0.0056(14) O3 0.0243(11) 0.0161(11) 0.0305(12) 0.0008(9) 0.0096(9) -0.0011(9) N3 0.0345(14) 0.0199(12) 0.0224(13) -0.0019(10) 0.0109(11) -0.0005(11) C3 0.0362(18) 0.0302(17) 0.0322(18) 0.0035(14) 0.0122(15) 0.0047(14) C4 0.0436(19) 0.0282(17) 0.0298(17) 0.0039(14) 0.0145(15) -0.0003(15) C5 0.0294(15) 0.0344(18) 0.0326(17) 0.0035(14) 0.0149(14) -0.0006(14) C6 0.0269(15) 0.0249(16) 0.0351(17) -0.0045(13) 0.0137(14) 0.0007(12) C7 0.0287(15) 0.0215(15) 0.0300(16) -0.0080(12) 0.0127(13) -0.0039(12) C8 0.0244(14) 0.0220(15) 0.0271(15) -0.0060(12) 0.0116(12) 0.0004(12) C9 0.0382(17) 0.0255(16) 0.0241(15) -0.0007(12) 0.0189(14) 0.0002(13) C10 0.0336(16) 0.0181(14) 0.0293(16) 0.0016(12) 0.0173(13) -0.0005(12) C11 0.0286(15) 0.0234(15) 0.0270(15) -0.0033(12) 0.0160(13) -0.0028(12) C12 0.0293(15) 0.0201(15) 0.0321(17) -0.0031(12) 0.0150(13) -0.0049(12) C16 0.0253(14) 0.0218(15) 0.0201(14) 0.0007(12) 0.0076(12) 0.0050(12) _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 2.095(3) . ? Co1 N3 2.095(3) 3 ? Co1 O3 2.111(2) 3 ? Co1 O3 2.111(2) . ? Co1 N2 2.181(2) 3 ? Co1 N2 2.181(2) . ? S1 C16 1.637(3) . ? O1 C2 1.413(4) . ? O1 C3 1.422(4) . ? N1 C6 1.464(4) . ? N1 C1 1.472(4) 3_566 ? N1 C7 1.473(4) . ? C1 N1 1.472(4) 3_566 ? C1 C2 1.501(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C5 1.414(4) . ? O2 C4 1.439(4) . ? N2 C10 1.331(4) . ? N2 C11 1.351(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 H3AO 0.88(5) . ? O3 H3BO 0.70(4) . ? N3 C16 1.154(4) . ? C3 C4 1.490(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.523(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.520(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.383(4) . ? C8 C12 1.388(4) . ? C9 C10 1.387(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.380(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? 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(2) . 3 ? N3 Co1 O3 92.55(10) . 3 ? N3 Co1 O3 87.45(10) 3 3 ? N3 Co1 O3 87.45(10) . . ? N3 Co1 O3 92.55(10) 3 . ? O3 Co1 O3 180.00(13) 3 . ? N3 Co1 N2 90.79(9) . 3 ? N3 Co1 N2 89.21(9) 3 3 ? O3 Co1 N2 90.39(9) 3 3 ? O3 Co1 N2 89.61(9) . 3 ? N3 Co1 N2 89.21(9) . . ? N3 Co1 N2 90.79(9) 3 . ? O3 Co1 N2 89.61(9) 3 . ? O3 Co1 N2 90.39(9) . . ? N2 Co1 N2 180.00(16) 3 . ? C2 O1 C3 111.8(2) . . ? C6 N1 C1 112.9(3) . 3_566 ? C6 N1 C7 114.0(2) . . ? C1 N1 C7 110.8(2) 3_566 . ? N1 C1 C2 114.7(3) 3_566 . ? N1 C1 H1A 108.6 3_566 . ? C2 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 3_566 . ? C2 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C5 O2 C4 112.9(3) . . ? C10 N2 C11 116.3(3) . . ? C10 N2 Co1 121.5(2) . . ? C11 N2 Co1 121.9(2) . . ? O1 C2 C1 108.3(3) . . ? O1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? Co1 O3 H3AO 119(3) . . ? Co1 O3 H3BO 124(4) . . ? H3AO O3 H3BO 104(4) . . ? C16 N3 Co1 155.7(2) . . ? O1 C3 C4 108.1(3) . . ? O1 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? O1 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? O2 C4 C3 113.2(3) . . ? O2 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? O2 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? O2 C5 C6 107.7(3) . . ? O2 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? O2 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? N1 C6 C5 111.5(3) . . ? N1 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N1 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N1 C7 C8 116.7(2) . . ? N1 C7 H7A 108.1 . . ? C8 C7 H7A 108.1 . . ? N1 C7 H7B 108.1 . . ? C8 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C9 C8 C12 116.7(3) . . ? C9 C8 C7 123.5(3) . . ? C12 C8 C7 119.8(3) . . ? C8 C9 C10 119.9(3) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? N2 C10 C9 123.8(3) . . ? N2 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? N2 C11 C12 123.3(3) . . ? N2 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C8 120.1(3) . . ? C11 C12 H12 120.0 . . ? C8 C12 H12 120.0 . . ? N3 C16 S1 176.9(3) . . ? 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 H3AO N1 0.88(5) 2.01(5) 2.879(3) 166(5) 2_545 O3 H3BO O2 0.70(4) 2.23(4) 2.928(3) 174(5) 4_665 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.787 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.074 #===END OF CIF