# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Goldberg, I.' _publ_contact_author_name 'Goldberg, I.' _publ_contact_author_email GOLDBERG@POST.TAU.AC.IL _publ_section_title ; Coordination polymers of flexible tetracarboxylic acids with metal ions. II. Supramolecular assemblies of 5,5'-methylene- and 5,5'-(ethane-1,2-diyl)-bis(oxy)diisophthalic acid ligands with d-transition metals ; # Attachment '- Paper2-CIF_a.txt' data_1 _database_code_depnum_ccdc_archive 'CCDC 779782' #TrackingRef '- Paper2-CIF_a.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H14 O13 Zn, 3(H2 O)' _chemical_formula_sum 'C17 H20 O16 Zn' _chemical_formula_weight 545.70 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 20.7034(4) _cell_length_b 7.5718(2) _cell_length_c 30.7679(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.7486(9) _cell_angle_gamma 90.00 _cell_volume 4817.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4655 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.86 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7007 _exptl_absorpt_correction_T_max 0.8109 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16675 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.86 _reflns_number_total 5583 _reflns_number_gt 3499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The H-atoms of the two protonated carboxylic groups could not be located. Only three molecules of the non-coordinated water solvent could be positioned reliably, though their H-atoms could not be located with high precision. Additional molecules of the water solvent present in the lattice are severely disordered, and could not be modeled at all by discrete atoms. Their contribution to the diffraction pattern was then subtracted by the Squeeze procedure, using the PLATON software (Spek, 2003). ; _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^)+(0.0954P)^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 5583 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.030140(16) 0.24782(5) 0.428744(12) 0.01617(14) Uani 1 1 d . . . O1 O 0.04893(10) 0.2030(3) 0.10817(8) 0.0208(5) Uani 1 1 d . . . O2 O 0.10483(10) 0.3602(4) 0.06228(9) 0.0301(6) Uani 1 1 d . . . C3 C 0.10166(15) 0.2673(4) 0.09489(12) 0.0167(7) Uani 1 1 d . . . C4 C 0.16214(14) 0.2221(4) 0.12220(11) 0.0169(7) Uani 1 1 d . . . C5 C 0.15693(14) 0.1520(4) 0.16329(11) 0.0181(7) Uani 1 1 d . . . H5 H 0.1154 0.1332 0.1743 0.022 Uiso 1 1 calc R . . C6 C 0.21188(14) 0.1089(4) 0.18858(11) 0.0168(7) Uani 1 1 d . . . C7 C 0.27277(14) 0.1349(4) 0.17274(11) 0.0160(7) Uani 1 1 d . . . H7 H 0.3104 0.1029 0.1898 0.019 Uiso 1 1 calc R . . C8 C 0.27822(14) 0.2083(4) 0.13156(11) 0.0153(7) Uani 1 1 d . . . C9 C 0.22325(14) 0.2533(4) 0.10593(11) 0.0164(7) Uani 1 1 d . . . H9 H 0.2271 0.3041 0.0779 0.020 Uiso 1 1 calc R . . C10 C 0.34515(15) 0.2400(4) 0.11579(11) 0.0165(7) Uani 1 1 d . . . O11 O 0.39216(10) 0.1862(3) 0.13971(8) 0.0245(6) Uani 1 1 d . . . O12 O 0.35061(10) 0.3171(3) 0.07987(8) 0.0215(5) Uani 1 1 d . . . O13 O 0.20150(9) 0.0446(3) 0.22986(7) 0.0210(5) Uani 1 1 d . . . C14 C 0.25422(14) -0.0322(5) 0.25379(11) 0.0215(8) Uani 1 1 d . . . H14A H 0.2374 -0.1133 0.2758 0.026 Uiso 1 1 calc R . . H14B H 0.2799 -0.1032 0.2338 0.026 Uiso 1 1 calc R . . O15 O 0.29504(9) 0.0934(3) 0.27492(8) 0.0206(5) Uani 1 1 d . . . C16 C 0.28040(14) 0.1401(4) 0.31727(11) 0.0168(7) Uani 1 1 d . . . C17 C 0.21722(14) 0.1509(4) 0.33061(11) 0.0168(7) Uani 1 1 d . . . H17 H 0.1819 0.1245 0.3109 0.020 Uiso 1 1 calc R . . C18 C 0.20639(15) 0.2011(4) 0.37338(12) 0.0174(7) Uani 1 1 d . . . C19 C 0.25908(14) 0.2379(4) 0.40253(11) 0.0138(7) Uani 1 1 d . . . H19 H 0.2520 0.2697 0.4318 0.017 Uiso 1 1 calc R . . C20 C 0.32128(15) 0.2274(4) 0.38821(12) 0.0170(7) Uani 1 1 d . . . C21 C 0.33196(14) 0.1782(5) 0.34558(11) 0.0181(7) Uani 1 1 d . . . H21 H 0.3748 0.1710 0.3360 0.022 Uiso 1 1 calc R . . C22 C 0.37883(15) 0.2623(4) 0.41928(12) 0.0184(7) Uani 1 1 d . . . O23 O 0.36940(11) 0.2817(3) 0.45875(8) 0.0243(6) Uani 1 1 d . . . O24 O 0.43433(10) 0.2683(3) 0.40310(8) 0.0212(6) Uani 1 1 d . . . C25 C 0.13829(15) 0.2149(4) 0.38741(13) 0.0188(8) Uani 1 1 d . . . O26 O 0.09287(10) 0.1866(3) 0.36044(8) 0.0244(6) Uani 1 1 d . . . O27 O 0.12929(11) 0.2548(3) 0.42691(8) 0.0189(5) Uani 1 1 d . . . O28 O 0.02071(12) 0.2943(4) 0.49338(8) 0.0302(6) Uani 1 1 d . . . H28A H 0.0524 0.2309 0.5094 0.045 Uiso 1 1 d R . . H28B H -0.0190 0.2339 0.4991 0.045 Uiso 1 1 d R . . O29 O 0.03039(10) 0.5198(3) 0.41645(9) 0.0274(6) Uani 1 1 d . . . H29A H 0.0596 0.5554 0.3949 0.041 Uiso 1 1 d R . . H29B H -0.0038 0.5833 0.4146 0.041 Uiso 1 1 d R . . O30 O 0.03583(10) -0.0313(3) 0.44135(8) 0.0232(6) Uani 1 1 d . . . H30A H 0.0707 -0.0862 0.4285 0.035 Uiso 1 1 d R . . H30B H 0.0014 -0.1004 0.4294 0.035 Uiso 1 1 d R . . O31 O 0.29845(11) 0.4701(4) 0.00301(8) 0.0315(6) Uani 1 1 d . . . H31A H 0.3221 0.5540 -0.0149 0.047 Uiso 1 1 d R . . H31B H 0.3148 0.4791 0.0349 0.047 Uiso 1 1 d R . . O32 O 0.33332(13) 0.0456(4) 0.01300(10) 0.0435(7) Uani 1 1 d . . . H32A H 0.3434 -0.0756 0.0228 0.065 Uiso 1 1 d R . . H32B H 0.3481 0.1500 0.0302 0.065 Uiso 1 1 d R . . O33 O 0.49531(12) 0.4120(4) 0.16395(10) 0.0428(7) Uani 1 1 d . . . H33A H 0.4613 0.3253 0.1617 0.064 Uiso 1 1 d R . . H33B H 0.4750 0.5351 0.1608 0.064 Uiso 1 1 d 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 Zn 0.0101(2) 0.0206(2) 0.0178(2) -0.00136(16) 0.00043(15) -0.00053(14) O1 0.0106(11) 0.0287(14) 0.0230(14) 0.0070(11) 0.0005(9) -0.0026(9) O2 0.0166(12) 0.0443(18) 0.0298(16) 0.0181(13) 0.0033(10) 0.0025(11) C3 0.0110(15) 0.0191(19) 0.0201(18) 0.0014(15) 0.0013(13) 0.0018(12) C4 0.0119(15) 0.0183(19) 0.0203(19) 0.0015(14) -0.0001(13) 0.0009(12) C5 0.0147(15) 0.0172(19) 0.022(2) -0.0025(14) 0.0024(13) -0.0013(12) C6 0.0216(16) 0.0142(17) 0.0148(18) 0.0020(14) 0.0024(13) -0.0021(13) C7 0.0141(15) 0.0148(17) 0.0188(19) -0.0019(13) -0.0008(13) -0.0001(12) C8 0.0129(15) 0.0168(18) 0.0164(18) 0.0001(13) 0.0040(13) -0.0003(12) C9 0.0118(15) 0.0182(18) 0.0190(18) 0.0011(14) -0.0001(13) 0.0017(12) C10 0.0165(16) 0.0160(17) 0.0171(18) -0.0026(15) 0.0017(13) 0.0007(12) O11 0.0124(11) 0.0318(14) 0.0295(15) 0.0055(12) 0.0022(10) 0.0028(10) O12 0.0177(11) 0.0216(13) 0.0253(15) 0.0016(11) 0.0036(10) -0.0009(10) O13 0.0161(11) 0.0284(14) 0.0182(14) 0.0048(11) -0.0004(9) -0.0035(10) C14 0.0214(17) 0.022(2) 0.021(2) -0.0002(16) -0.0003(14) 0.0005(14) O15 0.0176(11) 0.0276(14) 0.0167(13) -0.0035(10) 0.0021(9) -0.0003(9) C16 0.0206(16) 0.0154(18) 0.0144(18) 0.0019(14) 0.0012(13) -0.0010(13) C17 0.0148(15) 0.0149(19) 0.0204(19) 0.0012(14) -0.0020(13) -0.0011(12) C18 0.0146(15) 0.0165(17) 0.0212(19) 0.0005(14) 0.0022(13) 0.0009(12) C19 0.0138(15) 0.0162(17) 0.0116(16) 0.0019(13) 0.0025(12) 0.0009(12) C20 0.0140(15) 0.0169(18) 0.0201(19) -0.0008(14) 0.0010(13) 0.0004(12) C21 0.0134(15) 0.0181(17) 0.023(2) 0.0008(15) 0.0031(13) 0.0003(13) C22 0.0109(15) 0.0195(19) 0.0245(19) 0.0000(15) -0.0022(13) 0.0000(12) O23 0.0185(12) 0.0377(16) 0.0165(14) -0.0081(11) -0.0002(10) 0.0031(10) O24 0.0093(11) 0.0294(15) 0.0248(14) -0.0028(10) -0.0006(9) 0.0001(9) C25 0.0105(15) 0.0165(19) 0.030(2) -0.0009(14) 0.0019(14) -0.0012(12) O26 0.0135(11) 0.0293(14) 0.0303(15) -0.0026(12) 0.0002(10) -0.0012(10) O27 0.0132(11) 0.0211(13) 0.0230(14) -0.0053(10) 0.0056(10) 0.0003(9) O28 0.0230(13) 0.0507(18) 0.0170(14) -0.0044(12) 0.0019(10) -0.0009(11) O29 0.0159(11) 0.0201(14) 0.0470(18) 0.0033(12) 0.0095(11) 0.0017(9) O30 0.0146(11) 0.0217(13) 0.0334(16) -0.0016(11) 0.0006(10) 0.0008(9) O31 0.0292(13) 0.0379(16) 0.0270(16) 0.0067(12) -0.0009(11) -0.0062(11) O32 0.0503(17) 0.0329(17) 0.047(2) 0.0005(14) 0.0013(14) 0.0035(13) O33 0.0376(15) 0.0404(18) 0.050(2) 0.0038(15) 0.0004(13) -0.0030(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 Zn O1 1.976(2) 2 ? Zn O28 2.038(3) . ? Zn O27 2.057(2) . ? Zn O29 2.094(2) . ? Zn O30 2.151(2) . ? O1 C3 1.280(4) . ? O1 Zn 1.976(2) 2 ? O2 C3 1.230(4) . ? C3 C4 1.513(5) . ? C4 C5 1.380(5) . ? C4 C9 1.403(4) . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 O13 1.386(4) . ? C6 C7 1.387(4) . ? C7 C8 1.393(5) . ? C7 H7 0.9500 . ? C8 C9 1.395(4) . ? C8 C10 1.509(4) . ? C9 H9 0.9500 . ? C10 O11 1.259(4) . ? C10 O12 1.260(4) . ? O13 C14 1.412(4) . ? C14 O15 1.410(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C16 1.398(4) . ? C16 C21 1.375(4) . ? C16 C17 1.392(4) . ? C17 C18 1.398(5) . ? C17 H17 0.9500 . ? C18 C19 1.407(5) . ? C18 C25 1.498(4) . ? C19 C20 1.383(4) . ? C19 H19 0.9500 . ? C20 C21 1.391(5) . ? C20 C22 1.515(5) . ? C21 H21 0.9500 . ? C22 O23 1.248(4) . ? C22 O24 1.275(4) . ? C25 O26 1.242(4) . ? C25 O27 1.275(4) . ? O28 H28A 0.9341 . ? O28 H28B 0.9633 . ? O29 H29A 0.9583 . ? O29 H29B 0.8554 . ? O30 H30A 0.9364 . ? O30 H30B 0.9445 . ? O31 H31A 0.9861 . ? O31 H31B 1.0253 . ? O32 H32A 0.9862 . ? O32 H32B 0.9915 . ? O33 H33A 0.9621 . ? O33 H33B 1.0255 . ? 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 Zn O28 118.36(10) 2 . ? O1 Zn O27 142.07(10) 2 . ? O28 Zn O27 99.48(10) . . ? O1 Zn O29 94.27(10) 2 . ? O28 Zn O29 90.43(10) . . ? O27 Zn O29 87.62(8) . . ? O1 Zn O30 88.37(9) 2 . ? O28 Zn O30 90.05(10) . . ? O27 Zn O30 89.09(8) . . ? O29 Zn O30 176.72(8) . . ? C3 O1 Zn 116.5(2) . 2 ? O2 C3 O1 123.9(3) . . ? O2 C3 C4 120.5(3) . . ? O1 C3 C4 115.6(3) . . ? C5 C4 C9 120.2(3) . . ? C5 C4 C3 119.8(3) . . ? C9 C4 C3 120.0(3) . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 O13 116.0(3) . . ? C5 C6 C7 120.3(3) . . ? O13 C6 C7 123.7(3) . . ? C6 C7 C8 119.4(3) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 120.8(3) . . ? C9 C8 C10 121.1(3) . . ? C7 C8 C10 118.1(3) . . ? C8 C9 C4 118.8(3) . . ? C8 C9 H9 120.6 . . ? C4 C9 H9 120.6 . . ? O11 C10 O12 124.3(3) . . ? O11 C10 C8 117.1(3) . . ? O12 C10 C8 118.6(3) . . ? C6 O13 C14 118.2(2) . . ? O15 C14 O13 113.2(3) . . ? O15 C14 H14A 108.9 . . ? O13 C14 H14A 108.9 . . ? O15 C14 H14B 108.9 . . ? O13 C14 H14B 108.9 . . ? H14A C14 H14B 107.8 . . ? C16 O15 C14 116.7(2) . . ? C21 C16 C17 120.9(3) . . ? C21 C16 O15 116.5(3) . . ? C17 C16 O15 122.6(3) . . ? C16 C17 C18 119.3(3) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 C25 119.1(3) . . ? C19 C18 C25 121.0(3) . . ? C20 C19 C18 119.4(3) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 C22 120.3(3) . . ? C21 C20 C22 119.1(3) . . ? C16 C21 C20 120.0(3) . . ? C16 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? O23 C22 O24 124.2(3) . . ? O23 C22 C20 118.7(3) . . ? O24 C22 C20 117.2(3) . . ? O26 C25 O27 122.5(3) . . ? O26 C25 C18 119.2(3) . . ? O27 C25 C18 118.3(3) . . ? C25 O27 Zn 102.22(19) . . ? Zn O28 H28A 109.2 . . ? Zn O28 H28B 102.6 . . ? H28A O28 H28B 104.0 . . ? Zn O29 H29A 114.1 . . ? Zn O29 H29B 123.7 . . ? H29A O29 H29B 110.1 . . ? Zn O30 H30A 113.4 . . ? Zn O30 H30B 116.1 . . ? H30A O30 H30B 100.0 . . ? H31A O31 H31B 110.0 . . ? H32A O32 H32B 121.5 . . ? H33A O33 H33B 108.6 . . ? # 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 0.500 -0.030 0.250 191 54 ' ' 2 1.000 0.009 0.250 191 54 ' ' 3 0.500 0.000 0.750 191 54 ' ' 4 1.000 -0.101 0.750 191 54 ' ' _platon_squeeze_details ; ; 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 O28 H28A O23 0.93 1.85 2.712(3) 151 7_556 O28 H28B O30 0.96 2.43 3.098(4) 126 5_556 O29 H29A O11 0.96 1.79 2.722(3) 163 4 O29 H29B O24 0.86 1.92 2.754(3) 165 3_455 O30 H30A O12 0.94 1.82 2.724(3) 162 4_545 O30 H30B O24 0.94 1.86 2.805(3) 177 3_445 O31 H31A O23 0.99 1.80 2.781(3) 173 6_565 O31 H31B O12 1.03 1.97 2.803(3) 137 . O32 H32A O27 0.99 2.07 2.954(4) 149 4_545 O32 H32B O12 0.99 1.98 2.918(4) 156 . O33 H33A O11 0.96 1.88 2.808(4) 162 . O33 H33B O26 1.03 1.90 2.844(4) 151 4 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.163 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.120 #==============================END=================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 779783' #TrackingRef '- Paper2-CIF_a.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H19 N O13 Zn2, 2(H2 O)' _chemical_formula_sum 'C22 H23 N O15 Zn2' _chemical_formula_weight 672.15 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8788(2) _cell_length_b 30.1049(6) _cell_length_c 8.5449(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.3600(14) _cell_angle_gamma 90.00 _cell_volume 2606.27(9) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5570 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.89 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5143 _exptl_absorpt_correction_T_max 0.6457 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19477 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.89 _reflns_number_total 6089 _reflns_number_gt 4258 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0833P)^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 6089 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.33259(4) 0.063122(13) 0.00261(5) 0.01805(13) Uani 1 1 d . . . Zn2 Zn 1.33374(4) 0.147369(13) 0.55442(5) 0.01993(13) Uani 1 1 d . . . O1 O 1.1916(2) 0.39591(8) 0.5131(3) 0.0200(5) Uani 1 1 d . . . O2 O 1.0524(2) 0.44369(9) 0.3422(4) 0.0340(7) Uani 1 1 d . . . C3 C 1.0742(3) 0.40967(11) 0.4267(4) 0.0190(7) Uani 1 1 d . . . C4 C 0.9621(3) 0.38058(11) 0.4328(4) 0.0183(7) Uani 1 1 d . . . C5 C 0.8318(3) 0.39420(11) 0.3505(4) 0.0193(7) Uani 1 1 d . . . H5 H 0.8132 0.4221 0.2950 0.023 Uiso 1 1 calc R . . C6 C 0.7292(3) 0.36661(11) 0.3504(4) 0.0184(7) Uani 1 1 d . . . C7 C 0.7554(3) 0.32530(11) 0.4291(4) 0.0179(7) Uani 1 1 d . . . H7 H 0.6850 0.3060 0.4248 0.022 Uiso 1 1 calc R . . C8 C 0.8858(3) 0.31259(11) 0.5141(4) 0.0172(7) Uani 1 1 d . . . C9 C 0.9882(3) 0.34022(11) 0.5161(4) 0.0188(7) Uani 1 1 d . . . H9 H 1.0770 0.3314 0.5751 0.023 Uiso 1 1 calc R . . C10 C 0.5877(3) 0.38023(11) 0.2571(4) 0.0190(7) Uani 1 1 d . . . O11 O 0.5003(2) 0.35025(7) 0.2442(3) 0.0211(5) Uani 1 1 d . . . O12 O 0.5607(2) 0.41818(8) 0.1970(3) 0.0227(5) Uani 1 1 d . . . O13 O 0.9219(2) 0.27194(7) 0.5941(3) 0.0192(5) Uani 1 1 d . . . C14 C 0.8242(3) 0.24779(11) 0.6316(4) 0.0189(7) Uani 1 1 d . . . H14A H 0.8685 0.2261 0.7216 0.023 Uiso 1 1 calc R . . H14B H 0.7743 0.2687 0.6757 0.023 Uiso 1 1 calc R . . O15 O 0.7342(2) 0.22483(7) 0.4934(3) 0.0192(5) Uani 1 1 d . . . C16 C 0.7744(3) 0.18450(10) 0.4497(4) 0.0169(7) Uani 1 1 d . . . C17 C 0.6745(3) 0.15717(11) 0.3459(4) 0.0184(7) Uani 1 1 d . . . H17 H 0.5849 0.1660 0.3148 0.022 Uiso 1 1 calc R . . C18 C 0.7051(3) 0.11711(11) 0.2876(4) 0.0169(7) Uani 1 1 d . . . C19 C 0.8356(3) 0.10311(11) 0.3389(4) 0.0187(7) Uani 1 1 d . . . H19 H 0.8568 0.0754 0.3017 0.022 Uiso 1 1 calc R . . C20 C 0.9350(3) 0.13013(11) 0.4454(4) 0.0183(7) Uani 1 1 d . . . C21 C 0.9050(3) 0.17149(11) 0.4974(4) 0.0201(7) Uani 1 1 d . . . H21 H 0.9736 0.1905 0.5647 0.024 Uiso 1 1 calc R . . C22 C 1.0776(3) 0.11583(12) 0.4986(4) 0.0203(7) Uani 1 1 d . . . O23 O 1.1635(2) 0.14531(8) 0.5799(3) 0.0225(5) Uani 1 1 d . . . O24 O 1.1060(2) 0.07867(8) 0.4617(3) 0.0270(6) Uani 1 1 d . . . O25 O 1.3392(3) 0.10426(11) 0.3795(4) 0.0431(8) Uani 1 1 d . . . H25A H 1.4118 0.1037 0.3414 0.052 Uiso 1 1 d . . . H25B H 1.2636 0.1009 0.2794 0.052 Uiso 1 1 d . . . N26 N 1.3285(3) 0.21258(10) 0.4880(4) 0.0229(7) Uani 1 1 d . . . C27 C 1.4404(4) 0.23669(12) 0.5322(5) 0.0270(8) Uani 1 1 d . . . H27 H 1.5227 0.2221 0.5848 0.032 Uiso 1 1 calc R . . C28 C 1.4394(4) 0.28210(12) 0.5034(5) 0.0264(8) Uani 1 1 d . . . H28 H 1.5200 0.2981 0.5354 0.032 Uiso 1 1 calc R . . C29 C 1.3214(4) 0.30365(12) 0.4283(5) 0.0279(9) Uani 1 1 d . . . H29 H 1.3188 0.3348 0.4092 0.033 Uiso 1 1 calc R . . C30 C 1.2053(4) 0.27889(13) 0.3806(5) 0.0289(9) Uani 1 1 d . . . H30 H 1.1220 0.2927 0.3263 0.035 Uiso 1 1 calc R . . C31 C 1.2137(4) 0.23368(12) 0.4137(5) 0.0255(8) Uani 1 1 d . . . H31 H 1.1343 0.2169 0.3823 0.031 Uiso 1 1 calc R . . C32 C 0.5962(3) 0.08882(11) 0.1664(4) 0.0182(7) Uani 1 1 d . . . O33 O 0.6239(2) 0.05485(8) 0.1056(3) 0.0214(5) Uani 1 1 d . . . O34 O 0.4781(2) 0.10321(7) 0.1329(3) 0.0197(5) Uani 1 1 d . . . O35 O 0.3288(3) 0.04224(9) -0.2209(3) 0.0369(7) Uani 1 1 d . . . H35A H 0.2421 0.0513 -0.3044 0.044 Uiso 1 1 d . . . H35B H 0.4100 0.0567 -0.2230 0.044 Uiso 1 1 d . . . O36 O 0.3446(3) 0.00960(10) 0.1491(4) 0.0413(7) Uani 1 1 d . . . H36A H 0.4327 0.0084 0.2397 0.050 Uiso 1 1 d . . . H36B H 0.2688 0.0066 0.1866 0.050 Uiso 1 1 d . . . O37 O 0.6055(3) 0.02808(10) 0.4521(3) 0.0391(7) Uani 1 1 d . . . H37A H 0.6848 0.0187 0.5244 0.047 Uiso 1 1 d . . . H37B H 0.5928 0.0418 0.5366 0.047 Uiso 1 1 d . . . O38 O 0.1462(3) 0.00106(9) 0.3240(4) 0.0379(7) Uani 1 1 d . . . H38A H 0.1031 0.0255 0.3518 0.046 Uiso 1 1 d . . . H38B H 0.0757 -0.0203 0.2657 0.046 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0123(2) 0.0182(2) 0.0209(2) -0.00163(16) 0.00270(17) 0.00035(15) Zn2 0.0113(2) 0.0217(2) 0.0231(2) -0.00183(17) 0.00189(17) 0.00050(16) O1 0.0119(12) 0.0214(12) 0.0237(13) 0.0019(10) 0.0029(10) -0.0009(9) O2 0.0167(14) 0.0303(15) 0.0476(18) 0.0196(13) 0.0027(13) -0.0002(11) C3 0.0128(17) 0.0215(17) 0.0202(18) -0.0020(14) 0.0028(14) -0.0005(14) C4 0.0150(17) 0.0184(16) 0.0197(18) -0.0034(14) 0.0043(14) -0.0028(14) C5 0.0153(18) 0.0206(17) 0.0197(18) 0.0015(14) 0.0035(14) 0.0010(14) C6 0.0167(18) 0.0201(17) 0.0175(18) -0.0061(14) 0.0052(14) -0.0008(14) C7 0.0126(17) 0.0197(17) 0.0200(18) -0.0036(14) 0.0042(14) -0.0035(13) C8 0.0149(17) 0.0196(17) 0.0157(17) -0.0012(14) 0.0038(14) 0.0011(13) C9 0.0127(17) 0.0203(17) 0.0195(18) -0.0018(14) 0.0011(14) 0.0024(13) C10 0.0130(17) 0.0232(18) 0.0207(18) -0.0010(14) 0.0059(14) 0.0005(14) O11 0.0118(12) 0.0238(13) 0.0225(13) 0.0044(10) -0.0001(10) -0.0029(10) O12 0.0134(12) 0.0221(13) 0.0280(14) 0.0024(11) 0.0022(10) 0.0008(10) O13 0.0125(12) 0.0194(12) 0.0225(13) 0.0035(10) 0.0023(10) 0.0002(10) C14 0.0184(18) 0.0184(17) 0.0199(18) -0.0011(14) 0.0071(15) -0.0025(14) O15 0.0118(12) 0.0184(12) 0.0240(13) -0.0035(10) 0.0025(10) 0.0006(10) C16 0.0170(18) 0.0148(16) 0.0169(17) 0.0004(13) 0.0039(14) 0.0010(13) C17 0.0118(17) 0.0230(18) 0.0177(17) 0.0007(14) 0.0021(14) 0.0031(13) C18 0.0149(17) 0.0190(16) 0.0149(17) 0.0009(13) 0.0031(14) -0.0016(13) C19 0.0149(18) 0.0176(16) 0.0226(19) 0.0001(14) 0.0057(15) 0.0005(13) C20 0.0105(16) 0.0201(17) 0.0218(18) 0.0028(14) 0.0027(14) 0.0000(13) C21 0.0131(17) 0.0204(17) 0.0240(19) -0.0005(15) 0.0032(14) -0.0045(14) C22 0.0147(18) 0.0236(18) 0.0189(18) 0.0011(15) 0.0017(14) -0.0012(14) O23 0.0120(12) 0.0245(13) 0.0272(14) -0.0090(11) 0.0026(10) -0.0009(10) O24 0.0145(13) 0.0230(13) 0.0389(16) -0.0061(12) 0.0044(11) 0.0030(11) O25 0.0323(17) 0.060(2) 0.0326(17) -0.0095(15) 0.0073(14) -0.0005(15) N26 0.0174(16) 0.0232(16) 0.0248(16) 0.0021(13) 0.0039(13) -0.0003(12) C27 0.0167(19) 0.030(2) 0.031(2) 0.0030(17) 0.0048(16) 0.0010(15) C28 0.022(2) 0.029(2) 0.026(2) 0.0007(16) 0.0062(16) -0.0055(16) C29 0.035(2) 0.0221(18) 0.028(2) 0.0031(16) 0.0131(18) 0.0015(17) C30 0.024(2) 0.032(2) 0.027(2) 0.0065(17) 0.0048(17) 0.0045(17) C31 0.0163(19) 0.029(2) 0.027(2) 0.0037(16) 0.0016(16) 0.0012(15) C32 0.0137(17) 0.0214(17) 0.0181(18) 0.0034(14) 0.0041(14) -0.0023(14) O33 0.0173(13) 0.0219(13) 0.0234(13) -0.0034(10) 0.0056(11) -0.0002(10) O34 0.0110(12) 0.0217(12) 0.0222(13) -0.0022(10) 0.0013(10) -0.0007(9) O35 0.0289(16) 0.0432(17) 0.0363(17) -0.0083(14) 0.0090(13) -0.0016(13) O36 0.0360(18) 0.0411(18) 0.0452(18) 0.0089(14) 0.0128(15) 0.0054(14) O37 0.0372(17) 0.0555(19) 0.0198(14) -0.0068(13) 0.0044(12) -0.0030(15) O38 0.0269(15) 0.0315(15) 0.0550(19) -0.0173(14) 0.0143(14) -0.0053(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 Zn1 O34 1.979(2) . ? Zn1 O1 1.995(2) 4_465 ? Zn1 O35 1.997(3) . ? Zn1 O36 2.015(3) . ? Zn2 O23 1.942(2) . ? Zn2 O11 1.944(2) 4_666 ? Zn2 O25 1.997(3) . ? Zn2 N26 2.039(3) . ? O1 C3 1.289(4) . ? O1 Zn1 1.995(2) 4_666 ? O2 C3 1.225(4) . ? C3 C4 1.518(5) . ? C4 C9 1.384(5) . ? C4 C5 1.395(5) . ? C5 C6 1.391(5) . ? C5 H5 0.9500 . ? C6 C7 1.393(5) . ? C6 C10 1.509(5) . ? C7 C8 1.391(5) . ? C7 H7 0.9500 . ? C8 C9 1.386(5) . ? C8 O13 1.387(4) . ? C9 H9 0.9500 . ? C10 O12 1.243(4) . ? C10 O11 1.286(4) . ? O11 Zn2 1.944(2) 4_465 ? O13 C14 1.418(4) . ? C14 O15 1.409(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C16 1.387(4) . ? C16 C21 1.384(5) . ? C16 C17 1.394(5) . ? C17 C18 1.391(5) . ? C17 H17 0.9500 . ? C18 C19 1.390(4) . ? C18 C32 1.519(5) . ? C19 C20 1.394(5) . ? C19 H19 0.9500 . ? C20 C21 1.400(5) . ? C20 C22 1.512(5) . ? C21 H21 0.9500 . ? C22 O24 1.232(4) . ? C22 O23 1.293(4) . ? O25 H25A 0.9575 . ? O25 H25B 0.9522 . ? N26 C31 1.337(4) . ? N26 C27 1.348(5) . ? C27 C28 1.389(5) . ? C27 H27 0.9500 . ? C28 C29 1.372(5) . ? C28 H28 0.9500 . ? C29 C30 1.394(5) . ? C29 H29 0.9500 . ? C30 C31 1.386(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 O33 1.233(4) . ? C32 O34 1.285(4) . ? O35 H35A 0.9915 . ? O35 H35B 0.9911 . ? O36 H36A 0.9894 . ? O36 H36B 0.9915 . ? O37 H37A 0.9039 . ? O37 H37B 0.8852 . ? O38 H38A 0.9480 . ? O38 H38B 0.9861 . ? 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 O34 Zn1 O1 93.90(10) . 4_465 ? O34 Zn1 O35 117.63(11) . . ? O1 Zn1 O35 119.27(10) 4_465 . ? O34 Zn1 O36 106.29(11) . . ? O1 Zn1 O36 110.08(11) 4_465 . ? O35 Zn1 O36 108.46(12) . . ? O23 Zn2 O11 123.00(10) . 4_666 ? O23 Zn2 O25 110.66(11) . . ? O11 Zn2 O25 112.06(11) 4_666 . ? O23 Zn2 N26 97.51(11) . . ? O11 Zn2 N26 96.89(11) 4_666 . ? O25 Zn2 N26 115.02(12) . . ? C3 O1 Zn1 113.2(2) . 4_666 ? O2 C3 O1 123.0(3) . . ? O2 C3 C4 121.1(3) . . ? O1 C3 C4 115.9(3) . . ? C9 C4 C5 119.8(3) . . ? C9 C4 C3 120.5(3) . . ? C5 C4 C3 119.7(3) . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 120.6(3) . . ? C5 C6 C10 120.1(3) . . ? C7 C6 C10 119.2(3) . . ? C8 C7 C6 119.2(3) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C9 C8 O13 116.2(3) . . ? C9 C8 C7 120.2(3) . . ? O13 C8 C7 123.5(3) . . ? C4 C9 C8 120.5(3) . . ? C4 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? O12 C10 O11 123.6(3) . . ? O12 C10 C6 120.7(3) . . ? O11 C10 C6 115.7(3) . . ? C10 O11 Zn2 118.7(2) . 4_465 ? C8 O13 C14 117.6(3) . . ? O15 C14 O13 114.3(3) . . ? O15 C14 H14A 108.7 . . ? O13 C14 H14A 108.7 . . ? O15 C14 H14B 108.7 . . ? O13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C16 O15 C14 117.7(3) . . ? C21 C16 O15 124.0(3) . . ? C21 C16 C17 119.9(3) . . ? O15 C16 C17 116.1(3) . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 C32 119.9(3) . . ? C17 C18 C32 120.1(3) . . ? C18 C19 C20 119.3(3) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C21 120.7(3) . . ? C19 C20 C22 119.8(3) . . ? C21 C20 C22 119.4(3) . . ? C16 C21 C20 119.4(3) . . ? C16 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? O24 C22 O23 124.1(3) . . ? O24 C22 C20 120.5(3) . . ? O23 C22 C20 115.4(3) . . ? C22 O23 Zn2 119.6(2) . . ? Zn2 O25 H25A 121.3 . . ? Zn2 O25 H25B 119.4 . . ? H25A O25 H25B 104.0 . . ? C31 N26 C27 118.0(3) . . ? C31 N26 Zn2 121.1(2) . . ? C27 N26 Zn2 120.6(2) . . ? N26 C27 C28 122.2(3) . . ? N26 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C29 C28 C27 119.6(4) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 118.6(4) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C31 C30 C29 118.7(4) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? N26 C31 C30 122.9(3) . . ? N26 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? O33 C32 O34 124.3(3) . . ? O33 C32 C18 120.1(3) . . ? O34 C32 C18 115.5(3) . . ? C32 O34 Zn1 116.7(2) . . ? Zn1 O35 H35A 106.5 . . ? Zn1 O35 H35B 99.8 . . ? H35A O35 H35B 119.2 . . ? Zn1 O36 H36A 110.0 . . ? Zn1 O36 H36B 113.7 . . ? H36A O36 H36B 115.2 . . ? H37A O37 H37B 89.0 . . ? H38A O38 H38B 105.5 . . ? 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 O25 H25A O34 0.96 2.15 3.007(4) 148 1_655 O25 H25B O1 0.95 2.12 2.953(4) 145 4_565 O35 H35A O24 0.99 2.17 3.105(4) 157 1_454 O35 H35B O12 0.99 2.13 3.092(4) 163 4_565 O36 H36A O37 0.99 2.17 3.118(4) 160 . O36 H36B O38 0.99 2.08 3.050(4) 166 . O37 H37A O38 0.90 1.92 2.821(4) 179 3_656 O37 H37B O12 0.89 1.95 2.824(4) 169 4_566 O38 H38A O24 0.95 1.85 2.722(4) 152 1_455 O38 H38B O2 0.99 1.74 2.726(4) 178 2_645 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.381 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.118 #============================END================================= data_3 _database_code_depnum_ccdc_archive 'CCDC 779784' #TrackingRef '- Paper2-CIF_a.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H24 Mn3 N2 O22' _chemical_formula_sum 'C40 H24 Mn3 N2 O22' _chemical_formula_weight 1049.45 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' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 28.0246(6) _cell_length_b 12.3747(3) _cell_length_c 14.1946(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.4888(11) _cell_angle_gamma 90.00 _cell_volume 4640.60(18) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4904 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.86 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2116 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8087 _exptl_absorpt_correction_T_max 0.9165 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17293 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.86 _reflns_number_total 5508 _reflns_number_gt 3309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The acetonitrile ligand is partially disordered; its H-atoms were not included in the structure factor calculations. The lattice includes also disordered non-coordinated methanol and water solvent, which could not be modelled reliably by discrete atoms. The contribution of the disordered solvent was subtracted from the diffraction data by the Squeeze method, using the PLATON software (Spek, 2003). ; _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^)+(0.0872P)^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 5508 _refine_ls_number_parameters 306 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 Mn1 Mn 0.12397(2) 0.10600(4) 0.99640(4) 0.03070(17) Uani 1 1 d . . . Mn2 Mn 0.2500 0.2500 0.0000 0.02073(17) Uani 1 2 d S . . O3 O 0.12171(9) 0.1691(2) 0.85934(18) 0.0382(6) Uani 1 1 d . . . O4 O 0.18605(9) 0.28030(18) 0.86587(17) 0.0335(5) Uani 1 1 d . . . C5 C 0.14281(13) 0.2424(2) 0.8244(2) 0.0271(7) Uani 1 1 d . . . C6 C 0.11202(12) 0.2855(2) 0.7231(2) 0.0259(7) Uani 1 1 d . . . C7 C 0.06188(12) 0.2509(3) 0.6783(2) 0.0286(7) Uani 1 1 d . . . H7 H 0.0475 0.2002 0.7113 0.034 Uiso 1 1 calc R . . C8 C 0.03341(12) 0.2915(3) 0.5853(2) 0.0282(7) Uani 1 1 d . . . C9 C -0.01983(13) 0.2551(3) 0.5372(3) 0.0302(7) Uani 1 1 d . . . O10 O -0.04444(9) 0.30911(18) 0.45659(16) 0.0336(6) Uani 1 1 d . . . H10 H -0.0818 0.2923 0.4417 0.040 Uiso 1 1 d R . . O11 O -0.03863(10) 0.1820(2) 0.5698(2) 0.0529(8) Uani 1 1 d . . . C12 C 0.05423(12) 0.3668(2) 0.5358(2) 0.0272(7) Uani 1 1 d . . . H12 H 0.0348 0.3934 0.4716 0.033 Uiso 1 1 calc R . . C13 C 0.10332(12) 0.4016(2) 0.5820(2) 0.0265(7) Uani 1 1 d . . . C14 C 0.13243(13) 0.3611(2) 0.6747(2) 0.0268(7) Uani 1 1 d . . . H14 H 0.1663 0.3850 0.7050 0.032 Uiso 1 1 calc R . . O15 O 0.12668(9) 0.47795(17) 0.54109(15) 0.0292(5) Uani 1 1 d . . . C16 C 0.10088(14) 0.5149(2) 0.4436(2) 0.0298(7) Uani 1 1 d . . . H16A H 0.1174 0.5815 0.4311 0.036 Uiso 1 1 calc R . . H16B H 0.0656 0.5333 0.4377 0.036 Uiso 1 1 calc R . . O17 O 0.10033(8) 0.43727(18) 0.37086(16) 0.0293(5) Uani 1 1 d . . . C18 C 0.14391(12) 0.4293(2) 0.3455(2) 0.0246(7) Uani 1 1 d . . . C19 C 0.18917(12) 0.4779(2) 0.3988(2) 0.0281(7) Uani 1 1 d . . . H19 H 0.1924 0.5163 0.4586 0.034 Uiso 1 1 calc R . . C20 C 0.23003(12) 0.4702(2) 0.3641(2) 0.0279(7) Uani 1 1 d . . . C21 C 0.27824(13) 0.5299(3) 0.4187(3) 0.0327(8) Uani 1 1 d . . . O22 O 0.27946(9) 0.58871(17) 0.49190(18) 0.0373(6) Uani 1 1 d . . . O23 O 0.31550(9) 0.51998(19) 0.38900(19) 0.0410(6) Uani 1 1 d . . . C24 C 0.22573(12) 0.4128(2) 0.2771(2) 0.0261(7) Uani 1 1 d . . . H24 H 0.2536 0.4080 0.2535 0.031 Uiso 1 1 calc R . . C25 C 0.18012(12) 0.3626(2) 0.2256(2) 0.0230(7) Uani 1 1 d . . . C26 C 0.17630(12) 0.3027(2) 0.1311(2) 0.0239(7) Uani 1 1 d . . . O27 O 0.13594(8) 0.24904(17) 0.08803(15) 0.0272(5) Uani 1 1 d . . . O28 O 0.21250(9) 0.3089(2) 0.09975(18) 0.0406(6) Uani 1 1 d . . . C29 C 0.13941(12) 0.3704(2) 0.2592(2) 0.0233(6) Uani 1 1 d . . . H29 H 0.1084 0.3356 0.2237 0.028 Uiso 1 1 calc R . . O30 O 0.11120(13) -0.0463(2) 0.91165(18) 0.0565(8) Uani 1 1 d . . . C31 C 0.1106(2) -0.1520(3) 0.9535(4) 0.0680(14) Uani 1 1 d . . . H31A H 0.1454 -0.1756 0.9886 0.102 Uiso 1 1 calc R . . H31B H 0.0942 -0.2032 0.8998 0.102 Uiso 1 1 calc R . . H31C H 0.0918 -0.1493 1.0006 0.102 Uiso 1 1 calc R . . N32 N 0.08487(17) 0.0327(3) 1.0979(4) 0.0436(13) Uani 1 1 d U . . C33 C 0.05233(16) 0.0395(3) 1.1392(3) 0.0483(10) Uani 1 1 d U . . C34 C 0.0240(4) 0.0304(9) 1.2015(8) 0.075(4) Uani 1 1 d U . . 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 Mn1 0.0349(3) 0.0241(3) 0.0264(3) -0.0006(2) 0.0014(2) 0.0000(2) Mn2 0.0187(3) 0.0225(3) 0.0206(3) -0.0015(3) 0.0059(3) 0.0006(3) O3 0.0284(13) 0.0433(14) 0.0356(13) 0.0129(11) 0.0011(11) -0.0063(11) O4 0.0276(13) 0.0313(12) 0.0333(12) 0.0058(10) -0.0008(10) -0.0032(10) C5 0.0302(18) 0.0215(15) 0.0267(16) 0.0000(13) 0.0055(14) 0.0024(13) C6 0.0258(17) 0.0230(14) 0.0258(16) -0.0002(13) 0.0045(13) -0.0001(13) C7 0.0255(18) 0.0287(16) 0.0295(16) 0.0035(14) 0.0063(14) -0.0006(13) C8 0.0254(18) 0.0294(16) 0.0277(17) 0.0015(14) 0.0058(14) -0.0021(13) C9 0.0272(18) 0.0285(17) 0.0323(18) 0.0045(14) 0.0063(14) -0.0011(14) O10 0.0235(13) 0.0418(13) 0.0319(12) 0.0083(11) 0.0043(10) -0.0023(10) O11 0.0273(14) 0.0553(17) 0.0626(18) 0.0336(15) -0.0030(13) -0.0088(12) C12 0.0277(18) 0.0274(16) 0.0257(16) 0.0031(13) 0.0079(14) 0.0004(13) C13 0.0292(18) 0.0244(15) 0.0291(16) -0.0023(13) 0.0140(14) -0.0047(13) C14 0.0258(17) 0.0253(15) 0.0289(17) -0.0048(14) 0.0085(14) -0.0019(13) O15 0.0345(13) 0.0291(12) 0.0240(11) -0.0004(9) 0.0098(10) -0.0083(10) C16 0.042(2) 0.0247(16) 0.0265(16) 0.0006(14) 0.0166(15) 0.0041(14) O17 0.0298(13) 0.0322(12) 0.0291(12) -0.0047(10) 0.0140(10) -0.0034(10) C18 0.0233(17) 0.0244(15) 0.0269(16) -0.0010(13) 0.0095(13) 0.0009(12) C19 0.0319(19) 0.0233(15) 0.0261(16) -0.0041(13) 0.0057(14) 0.0004(13) C20 0.0243(17) 0.0229(15) 0.0337(17) 0.0007(14) 0.0060(14) -0.0011(13) C21 0.0291(19) 0.0224(16) 0.0378(19) 0.0018(15) -0.0005(15) -0.0010(13) O22 0.0339(14) 0.0247(11) 0.0382(13) -0.0080(11) -0.0083(11) 0.0008(10) O23 0.0256(13) 0.0363(14) 0.0561(16) -0.0040(12) 0.0069(12) -0.0041(10) C24 0.0254(17) 0.0213(15) 0.0319(17) -0.0009(13) 0.0101(14) -0.0006(12) C25 0.0256(17) 0.0197(14) 0.0237(15) 0.0002(12) 0.0085(13) 0.0007(12) C26 0.0230(17) 0.0202(15) 0.0271(16) 0.0012(13) 0.0068(14) 0.0027(12) O27 0.0224(12) 0.0303(12) 0.0257(11) -0.0073(9) 0.0038(9) 0.0008(9) O28 0.0318(14) 0.0537(16) 0.0437(14) -0.0229(13) 0.0223(12) -0.0087(12) C29 0.0234(17) 0.0222(14) 0.0227(15) -0.0008(12) 0.0056(13) -0.0036(12) O30 0.108(3) 0.0244(12) 0.0332(14) -0.0006(11) 0.0188(15) -0.0130(14) C31 0.119(4) 0.027(2) 0.068(3) 0.002(2) 0.046(3) -0.014(2) N32 0.055(3) 0.0370(18) 0.046(4) -0.020(2) 0.026(3) -0.021(2) C33 0.046(2) 0.047(2) 0.046(2) -0.015(2) 0.017(2) -0.0172(18) C34 0.084(10) 0.055(9) 0.074(9) -0.021(7) 0.024(8) -0.004(7) _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 Mn1 O3 2.078(2) . ? Mn1 O27 2.156(2) 1_556 ? Mn1 O23 2.194(2) 4_546 ? Mn1 O30 2.200(3) . ? Mn1 N32 2.270(3) . ? Mn1 O11 2.447(3) 2_556 ? Mn2 O28 2.152(2) 7 ? Mn2 O28 2.153(2) . ? Mn2 O4 2.168(2) 7_556 ? Mn2 O4 2.168(2) 1_554 ? Mn2 O22 2.178(2) 6_565 ? Mn2 O22 2.178(2) 4_545 ? O3 C5 1.270(4) . ? O4 C5 1.249(4) . ? O4 Mn2 2.168(2) 1_556 ? C5 C6 1.506(4) . ? C6 C14 1.391(4) . ? C6 C7 1.402(4) . ? C7 C8 1.389(4) . ? C7 H7 0.9500 . ? C8 C12 1.406(4) . ? C8 C9 1.488(5) . ? C9 O11 1.214(4) . ? C9 O10 1.306(4) . ? O10 H10 1.0188 . ? O11 Mn1 2.447(3) 2_556 ? C12 C13 1.380(4) . ? C12 H12 0.9500 . ? C13 O15 1.383(4) . ? C13 C14 1.390(4) . ? C14 H14 0.9500 . ? O15 C16 1.407(4) . ? C16 O17 1.407(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O17 C18 1.387(4) . ? C18 C19 1.380(4) . ? C18 C29 1.394(4) . ? C19 C20 1.393(5) . ? C19 H19 0.9500 . ? C20 C24 1.394(5) . ? C20 C21 1.508(5) . ? C21 O22 1.260(4) . ? C21 O23 1.255(4) . ? O22 Mn2 2.178(2) 4 ? O23 Mn1 2.194(2) 4_556 ? C24 C25 1.390(4) . ? C24 H24 0.9500 . ? C25 C29 1.379(4) . ? C25 C26 1.505(4) . ? C26 O28 1.239(4) . ? C26 O27 1.277(4) . ? O27 Mn1 2.156(2) 1_554 ? C29 H29 0.9500 . ? O30 C31 1.439(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N32 C33 1.241(5) . ? C33 C34 1.376(10) . ? 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 Mn1 O27 101.91(9) . 1_556 ? O3 Mn1 O23 130.62(10) . 4_546 ? O27 Mn1 O23 91.42(9) 1_556 4_546 ? O3 Mn1 O30 82.04(10) . . ? O27 Mn1 O30 176.03(9) 1_556 . ? O23 Mn1 O30 86.23(10) 4_546 . ? O3 Mn1 N32 150.95(15) . . ? O27 Mn1 N32 87.48(11) 1_556 . ? O23 Mn1 N32 75.70(14) 4_546 . ? O30 Mn1 N32 88.84(12) . . ? O3 Mn1 O11 77.02(10) . 2_556 ? O27 Mn1 O11 81.45(8) 1_556 2_556 ? O23 Mn1 O11 152.35(11) 4_546 2_556 ? O30 Mn1 O11 99.18(11) . 2_556 ? N32 Mn1 O11 77.31(15) . 2_556 ? O28 Mn2 O28 180.0 7 . ? O28 Mn2 O4 94.42(9) 7 7_556 ? O28 Mn2 O4 85.58(9) . 7_556 ? O28 Mn2 O4 85.58(9) 7 1_554 ? O28 Mn2 O4 94.42(9) . 1_554 ? O4 Mn2 O4 179.998(1) 7_556 1_554 ? O28 Mn2 O22 89.93(10) 7 6_565 ? O28 Mn2 O22 90.07(10) . 6_565 ? O4 Mn2 O22 89.31(8) 7_556 6_565 ? O4 Mn2 O22 90.69(8) 1_554 6_565 ? O28 Mn2 O22 90.07(10) 7 4_545 ? O28 Mn2 O22 89.93(10) . 4_545 ? O4 Mn2 O22 90.69(8) 7_556 4_545 ? O4 Mn2 O22 89.31(8) 1_554 4_545 ? O22 Mn2 O22 180.0 6_565 4_545 ? C5 O3 Mn1 139.6(2) . . ? C5 O4 Mn2 137.5(2) . 1_556 ? O4 C5 O3 126.1(3) . . ? O4 C5 C6 118.3(3) . . ? O3 C5 C6 115.7(3) . . ? C14 C6 C7 119.8(3) . . ? C14 C6 C5 120.7(3) . . ? C7 C6 C5 119.5(3) . . ? C8 C7 C6 119.4(3) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C12 120.8(3) . . ? C7 C8 C9 119.8(3) . . ? C12 C8 C9 119.4(3) . . ? O11 C9 O10 123.1(3) . . ? O11 C9 C8 123.2(3) . . ? O10 C9 C8 113.8(3) . . ? C9 O10 H10 106.5 . . ? C9 O11 Mn1 129.3(2) . 2_556 ? C13 C12 C8 118.9(3) . . ? C13 C12 H12 120.6 . . ? C8 C12 H12 120.6 . . ? O15 C13 C12 123.4(3) . . ? O15 C13 C14 115.7(3) . . ? C12 C13 C14 120.9(3) . . ? C6 C14 C13 120.1(3) . . ? C6 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C13 O15 C16 118.4(2) . . ? O15 C16 O17 112.1(2) . . ? O15 C16 H16A 109.2 . . ? O17 C16 H16A 109.2 . . ? O15 C16 H16B 109.2 . . ? O17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 O17 C16 116.4(2) . . ? C19 C18 O17 123.6(3) . . ? C19 C18 C29 120.5(3) . . ? O17 C18 C29 115.8(3) . . ? C18 C19 C20 119.3(3) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C24 120.7(3) . . ? C19 C20 C21 119.1(3) . . ? C24 C20 C21 120.2(3) . . ? O22 C21 O23 122.4(3) . . ? O22 C21 C20 118.7(3) . . ? O23 C21 C20 118.9(3) . . ? C21 O22 Mn2 131.8(2) . 4 ? C21 O23 Mn1 103.2(2) . 4_556 ? C25 C24 C20 119.1(3) . . ? C25 C24 H24 120.4 . . ? C20 C24 H24 120.4 . . ? C29 C25 C24 120.6(3) . . ? C29 C25 C26 121.4(3) . . ? C24 C25 C26 118.0(3) . . ? O28 C26 O27 124.1(3) . . ? O28 C26 C25 117.8(3) . . ? O27 C26 C25 118.1(3) . . ? C26 O27 Mn1 130.5(2) . 1_554 ? C26 O28 Mn2 148.6(2) . . ? C25 C29 C18 119.8(3) . . ? C25 C29 H29 120.1 . . ? C18 C29 H29 120.1 . . ? C31 O30 Mn1 125.1(2) . . ? O30 C31 H31A 109.5 . . ? O30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 N32 Mn1 149.3(4) . . ? N32 C33 C34 166.1(7) . . ? 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 O10 H10 O27 1.02 1.53 2.539(3) 170 2 # 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 0.250 0.250 0.500 132 37 ' ' 2 0.250 -0.250 1.000 132 37 ' ' 3 0.500 -0.099 0.250 68 11 ' ' 4 0.500 0.099 0.750 68 11 ' ' 5 0.750 0.250 0.000 132 37 ' ' 6 0.750 -0.250 0.500 132 37 ' ' 7 0.000 0.401 0.250 68 11 ' ' 8 0.000 0.599 0.750 68 11 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.581 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.091 #==================================END====================== data_4 _database_code_depnum_ccdc_archive 'CCDC 779785' #TrackingRef '- Paper2-CIF_a.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H8 Co2 O12' _chemical_formula_sum 'C17 H8 Co2 O12' _chemical_formula_weight 522.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 10.2067(4) _cell_length_b 11.1297(6) _cell_length_c 13.9251(5) _cell_angle_alpha 112.663(3) _cell_angle_beta 104.574(3) _cell_angle_gamma 94.7960(17) _cell_volume 1383.57(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5094 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.20 _exptl_crystal_description plates _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7065 _exptl_absorpt_correction_T_max 0.8856 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16280 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.1030 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.20 _reflns_number_total 5917 _reflns_number_gt 3463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contained several molecules of severely disordered solvent (MeOH and water), which could not be modeled reliably by discrete atoms. Its contribution to the diffraction pattern was thus subtracted by the Squeeze technique, using the PLATON software (Spek, 2003). ; _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^)+(0.0489P)^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 5917 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 0.50570(5) -0.13633(5) -0.49098(4) 0.02417(15) Uani 1 1 d . . . Co2 Co 0.38618(5) 0.07824(5) -0.30240(4) 0.02200(15) Uani 1 1 d . . . O3 O 0.6695(2) -0.0370(3) -0.34347(19) 0.0283(6) Uani 1 1 d . . . O4 O 0.5940(3) 0.1212(3) -0.22402(19) 0.0307(6) Uani 1 1 d . . . C5 C 0.6877(4) 0.0691(4) -0.2578(3) 0.0281(9) Uani 1 1 d . . . C6 C 0.8345(4) 0.1379(4) -0.1914(3) 0.0269(9) Uani 1 1 d . . . C7 C 0.9415(4) 0.1016(4) -0.2348(3) 0.0276(9) Uani 1 1 d . . . H7 H 0.9215 0.0333 -0.3065 0.033 Uiso 1 1 calc R . . C8 C 1.0771(4) 0.1651(4) -0.1736(3) 0.0271(9) Uani 1 1 d . . . C9 C 1.1927(4) 0.1284(4) -0.2210(3) 0.0256(9) Uani 1 1 d . . . O10 O 1.3145(2) 0.1553(2) -0.15888(18) 0.0256(6) Uani 1 1 d . . . O11 O 1.1633(3) 0.0693(3) -0.32451(18) 0.0307(6) Uani 1 1 d . . . C12 C 1.1072(4) 0.2671(4) -0.0687(3) 0.0247(8) Uani 1 1 d . . . H12 H 1.2001 0.3093 -0.0257 0.030 Uiso 1 1 calc R . . C13 C 0.9990(4) 0.3055(4) -0.0286(3) 0.0250(8) Uani 1 1 d . . . C14 C 0.8623(4) 0.2421(4) -0.0881(3) 0.0268(9) Uani 1 1 d . . . H14 H 0.7894 0.2692 -0.0592 0.032 Uiso 1 1 calc R . . O15 O 1.0401(3) 0.4127(2) 0.07443(18) 0.0283(6) Uani 1 1 d . . . C16 C 0.9353(4) 0.4603(4) 0.1195(3) 0.0295(9) Uani 1 1 d . . . H16A H 0.8595 0.4700 0.0643 0.035 Uiso 1 1 calc R . . H16B H 0.9729 0.5477 0.1831 0.035 Uiso 1 1 calc R . . O17 O 0.8865(3) 0.3626(3) 0.15274(19) 0.0307(6) Uani 1 1 d . . . C18 C 0.7997(4) 0.3972(4) 0.2172(3) 0.0244(8) Uani 1 1 d . . . C19 C 0.7595(4) 0.3014(4) 0.2499(3) 0.0248(8) Uani 1 1 d . . . H19 H 0.7889 0.2191 0.2260 0.030 Uiso 1 1 calc R . . C20 C 0.6762(3) 0.3250(3) 0.3175(3) 0.0202(8) Uani 1 1 d . . . C21 C 0.6290(4) 0.2189(4) 0.3494(3) 0.0255(8) Uani 1 1 d . . . O22 O 0.5787(3) 0.2531(3) 0.42769(19) 0.0306(6) Uani 1 1 d . . . O23 O 0.6436(3) 0.1036(2) 0.29532(19) 0.0306(6) Uani 1 1 d . . . C24 C 0.6373(4) 0.4481(4) 0.3539(3) 0.0230(8) Uani 1 1 d . . . H24 H 0.5842 0.4674 0.4031 0.028 Uiso 1 1 calc R . . C25 C 0.6758(4) 0.5424(4) 0.3187(3) 0.0229(8) Uani 1 1 d . . . C26 C 0.6277(4) 0.6718(4) 0.3532(3) 0.0230(8) Uani 1 1 d . . . O27 O 0.6137(3) 0.7192(2) 0.44884(18) 0.0280(6) Uani 1 1 d . . . O28 O 0.6055(3) 0.7264(3) 0.28907(19) 0.0304(6) Uani 1 1 d . . . C29 C 0.7555(4) 0.5167(4) 0.2480(3) 0.0238(8) Uani 1 1 d . . . H29 H 0.7791 0.5797 0.2215 0.029 Uiso 1 1 calc R . . O30 O 0.3932(3) 0.0105(2) -0.45646(17) 0.0240(6) Uani 1 1 d . . . O31 O 0.3313(3) -0.2497(3) -0.6380(2) 0.0383(7) 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 0.0297(3) 0.0237(3) 0.0263(3) 0.0107(2) 0.0190(2) 0.0098(2) Co2 0.0243(3) 0.0231(3) 0.0240(3) 0.0101(2) 0.0154(2) 0.0076(2) O3 0.0237(14) 0.0315(16) 0.0321(14) 0.0111(12) 0.0146(11) 0.0098(12) O4 0.0248(14) 0.0375(16) 0.0318(14) 0.0099(12) 0.0180(11) 0.0109(13) C5 0.032(2) 0.030(2) 0.029(2) 0.0143(17) 0.0165(17) 0.0088(18) C6 0.023(2) 0.031(2) 0.029(2) 0.0112(17) 0.0149(16) 0.0063(17) C7 0.023(2) 0.029(2) 0.0302(19) 0.0075(16) 0.0155(16) 0.0085(17) C8 0.032(2) 0.029(2) 0.0258(19) 0.0099(17) 0.0194(16) 0.0095(18) C9 0.026(2) 0.024(2) 0.030(2) 0.0091(17) 0.0164(17) 0.0053(17) O10 0.0224(15) 0.0288(15) 0.0278(13) 0.0098(11) 0.0142(11) 0.0070(12) O11 0.0304(15) 0.0342(16) 0.0223(14) 0.0028(11) 0.0138(11) 0.0083(12) C12 0.026(2) 0.024(2) 0.0275(19) 0.0100(16) 0.0155(15) 0.0059(16) C13 0.033(2) 0.020(2) 0.0246(19) 0.0068(15) 0.0182(16) 0.0073(17) C14 0.025(2) 0.030(2) 0.033(2) 0.0138(17) 0.0194(16) 0.0057(17) O15 0.0323(15) 0.0293(15) 0.0264(13) 0.0068(11) 0.0216(11) 0.0083(12) C16 0.042(3) 0.025(2) 0.033(2) 0.0119(17) 0.0279(18) 0.0137(19) O17 0.0436(17) 0.0259(15) 0.0401(14) 0.0173(12) 0.0334(13) 0.0164(13) C18 0.028(2) 0.028(2) 0.0201(18) 0.0071(15) 0.0179(15) 0.0075(17) C19 0.026(2) 0.025(2) 0.0240(18) 0.0087(16) 0.0117(15) 0.0074(17) C20 0.0198(19) 0.021(2) 0.0217(17) 0.0086(15) 0.0101(14) 0.0070(16) C21 0.021(2) 0.031(2) 0.031(2) 0.0156(17) 0.0146(16) 0.0093(17) O22 0.0405(17) 0.0284(15) 0.0308(14) 0.0121(11) 0.0240(12) 0.0082(13) O23 0.0457(17) 0.0218(15) 0.0354(14) 0.0122(12) 0.0286(12) 0.0134(13) C24 0.028(2) 0.025(2) 0.0226(18) 0.0097(15) 0.0184(15) 0.0078(17) C25 0.029(2) 0.023(2) 0.0257(18) 0.0135(15) 0.0159(15) 0.0136(17) C26 0.020(2) 0.021(2) 0.035(2) 0.0152(16) 0.0140(16) 0.0057(16) O27 0.0381(16) 0.0276(15) 0.0290(13) 0.0142(11) 0.0218(11) 0.0154(13) O28 0.0444(17) 0.0283(16) 0.0324(14) 0.0176(12) 0.0236(12) 0.0176(13) C29 0.027(2) 0.026(2) 0.0239(18) 0.0108(16) 0.0165(15) 0.0096(17) O30 0.0320(15) 0.0227(14) 0.0268(13) 0.0131(11) 0.0183(11) 0.0127(12) O31 0.0372(17) 0.0408(18) 0.0391(15) 0.0192(13) 0.0123(12) 0.0060(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 O30 2.051(2) . ? Co1 O27 2.056(2) 1_544 ? Co1 O22 2.071(3) 2_655 ? Co1 O3 2.110(2) . ? Co1 O30 2.119(2) 2_654 ? Co1 O31 2.180(3) . ? Co2 O30 2.004(2) . ? Co2 O4 2.045(3) . ? Co2 O23 2.065(3) 2_655 ? Co2 O28 2.102(3) 2_665 ? Co2 O10 2.187(2) 1_455 ? Co2 O11 2.206(3) 1_455 ? Co2 C9 2.514(4) 1_455 ? O3 C5 1.272(4) . ? O4 C5 1.258(4) . ? C5 C6 1.500(5) . ? C6 C7 1.392(5) . ? C6 C14 1.396(5) . ? C7 C8 1.385(5) . ? C7 H7 0.9500 . ? C8 C12 1.398(5) . ? C8 C9 1.503(5) . ? C9 O10 1.258(4) . ? C9 O11 1.272(4) . ? C9 Co2 2.514(4) 1_655 ? O10 Co2 2.187(2) 1_655 ? O11 Co2 2.206(3) 1_655 ? C12 C13 1.385(5) . ? C12 H12 0.9500 . ? C13 C14 1.391(5) . ? C13 O15 1.397(4) . ? C14 H14 0.9500 . ? O15 C16 1.412(4) . ? C16 O17 1.435(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O17 C18 1.390(4) . ? C18 C19 1.380(5) . ? C18 C29 1.383(5) . ? C19 C20 1.389(5) . ? C19 H19 0.9500 . ? C20 C24 1.396(5) . ? C20 C21 1.497(5) . ? C21 O23 1.257(4) . ? C21 O22 1.262(4) . ? O22 Co1 2.071(3) 2_655 ? O23 Co2 2.065(3) 2_655 ? C24 C25 1.386(5) . ? C24 H24 0.9500 . ? C25 C29 1.392(5) . ? C25 C26 1.499(5) . ? C26 O28 1.249(4) . ? C26 O27 1.280(4) . ? O27 Co1 2.056(2) 1_566 ? O28 Co2 2.102(3) 2_665 ? C29 H29 0.9500 . ? O30 Co1 2.119(2) 2_654 ? 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 O30 Co1 O27 169.94(9) . 1_544 ? O30 Co1 O22 99.14(10) . 2_655 ? O27 Co1 O22 88.58(10) 1_544 2_655 ? O30 Co1 O3 94.72(9) . . ? O27 Co1 O3 91.57(10) 1_544 . ? O22 Co1 O3 91.02(10) 2_655 . ? O30 Co1 O30 81.93(10) . 2_654 ? O27 Co1 O30 90.93(9) 1_544 2_654 ? O22 Co1 O30 175.11(10) 2_655 2_654 ? O3 Co1 O30 84.14(9) . 2_654 ? O30 Co1 O31 86.57(10) . . ? O27 Co1 O31 87.77(10) 1_544 . ? O22 Co1 O31 84.42(10) 2_655 . ? O3 Co1 O31 175.40(10) . . ? O30 Co1 O31 100.42(10) 2_654 . ? O30 Co2 O4 98.15(10) . . ? O30 Co2 O23 97.30(9) . 2_655 ? O4 Co2 O23 93.66(11) . 2_655 ? O30 Co2 O28 91.96(9) . 2_665 ? O4 Co2 O28 90.51(11) . 2_665 ? O23 Co2 O28 169.19(9) 2_655 2_665 ? O30 Co2 O10 162.44(10) . 1_455 ? O4 Co2 O10 98.72(9) . 1_455 ? O23 Co2 O10 86.46(9) 2_655 1_455 ? O28 Co2 O10 83.05(9) 2_665 1_455 ? O30 Co2 O11 102.60(9) . 1_455 ? O4 Co2 O11 159.05(9) . 1_455 ? O23 Co2 O11 86.57(10) 2_655 1_455 ? O28 Co2 O11 85.98(10) 2_665 1_455 ? O10 Co2 O11 60.37(9) 1_455 1_455 ? O30 Co2 C9 132.71(11) . 1_455 ? O4 Co2 C9 128.67(11) . 1_455 ? O23 Co2 C9 87.11(11) 2_655 1_455 ? O28 Co2 C9 82.51(11) 2_665 1_455 ? O10 Co2 C9 30.02(10) 1_455 1_455 ? O11 Co2 C9 30.38(10) 1_455 1_455 ? C5 O3 Co1 133.4(2) . . ? C5 O4 Co2 129.1(2) . . ? O4 C5 O3 125.9(4) . . ? O4 C5 C6 117.3(3) . . ? O3 C5 C6 116.8(3) . . ? C7 C6 C14 120.3(3) . . ? C7 C6 C5 120.0(3) . . ? C14 C6 C5 119.6(3) . . ? C8 C7 C6 120.1(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C12 120.3(3) . . ? C7 C8 C9 120.3(3) . . ? C12 C8 C9 119.4(3) . . ? O10 C9 O11 121.7(3) . . ? O10 C9 C8 120.1(3) . . ? O11 C9 C8 118.2(3) . . ? O10 C9 Co2 60.47(17) . 1_655 ? O11 C9 Co2 61.32(18) . 1_655 ? C8 C9 Co2 176.8(3) . 1_655 ? C9 O10 Co2 89.51(19) . 1_655 ? C9 O11 Co2 88.3(2) . 1_655 ? C13 C12 C8 118.8(4) . . ? C13 C12 H12 120.6 . . ? C8 C12 H12 120.6 . . ? C12 C13 C14 121.8(3) . . ? C12 C13 O15 114.1(3) . . ? C14 C13 O15 124.1(3) . . ? C13 C14 C6 118.6(3) . . ? C13 C14 H14 120.7 . . ? C6 C14 H14 120.7 . . ? C13 O15 C16 117.5(3) . . ? O15 C16 O17 105.5(3) . . ? O15 C16 H16A 110.6 . . ? O17 C16 H16A 110.6 . . ? O15 C16 H16B 110.6 . . ? O17 C16 H16B 110.6 . . ? H16A C16 H16B 108.8 . . ? C18 O17 C16 116.7(3) . . ? C19 C18 C29 121.4(3) . . ? C19 C18 O17 114.3(3) . . ? C29 C18 O17 124.3(3) . . ? C18 C19 C20 120.2(3) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C24 118.8(3) . . ? C19 C20 C21 119.9(3) . . ? C24 C20 C21 121.2(3) . . ? O23 C21 O22 126.1(4) . . ? O23 C21 C20 116.5(3) . . ? O22 C21 C20 117.3(3) . . ? C21 O22 Co1 129.1(2) . 2_655 ? C21 O23 Co2 136.1(2) . 2_655 ? C25 C24 C20 120.4(3) . . ? C25 C24 H24 119.8 . . ? C20 C24 H24 119.8 . . ? C24 C25 C29 120.6(3) . . ? C24 C25 C26 120.2(3) . . ? C29 C25 C26 119.1(3) . . ? O28 C26 O27 124.5(3) . . ? O28 C26 C25 119.1(3) . . ? O27 C26 C25 116.5(3) . . ? C26 O27 Co1 127.3(2) . 1_566 ? C26 O28 Co2 136.7(2) . 2_665 ? C18 C29 C25 118.5(3) . . ? C18 C29 H29 120.8 . . ? C25 C29 H29 120.8 . . ? Co2 O30 Co1 112.38(11) . . ? Co2 O30 Co1 120.60(12) . 2_654 ? Co1 O30 Co1 98.07(10) . 2_654 ? # 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 -0.020 -0.017 -0.012 607 232 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.20 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.645 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.098 #=====================================END======================= data_5 _database_code_depnum_ccdc_archive 'CCDC 779786' #TrackingRef '- Paper2-CIF_a.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H12 Ag2 O11' _chemical_formula_sum 'C17 H12 Ag2 O11' _chemical_formula_weight 608.01 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' Ag Ag -0.8971 1.1015 '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' _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 8.55940(10) _cell_length_b 9.7574(2) _cell_length_c 11.5046(2) _cell_angle_alpha 67.7013(9) _cell_angle_beta 81.9196(8) _cell_angle_gamma 71.4140(11) _cell_volume 842.41(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2992 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.82 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 2.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5338 _exptl_absorpt_correction_T_max 0.7154 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scan' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9318 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.82 _reflns_number_total 3942 _reflns_number_gt 3329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^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 3572 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.08382(3) 0.10835(3) 0.91956(2) 0.01856(10) Uani 1 1 d . . . Ag2 Ag -0.39436(3) 0.05990(3) 0.90372(2) 0.01931(10) Uani 1 1 d . . . O1 O -0.8152(3) -0.6079(3) 0.9834(2) 0.0228(6) Uani 1 1 d . . . H1 H -0.8829 -0.6677 1.0166 0.034 Uiso 1 1 d R . . O2 O -0.7351(3) -0.7175(3) 0.8366(2) 0.0202(5) Uani 1 1 d . . . C3 C -0.7351(4) -0.6199(4) 0.8795(3) 0.0165(7) Uani 1 1 d . . . C4 C -0.6417(4) -0.5045(4) 0.8194(3) 0.0135(6) Uani 1 1 d . . . C5 C -0.6395(4) -0.4018(4) 0.8771(3) 0.0143(7) Uani 1 1 d . . . H5 H -0.6998 -0.4035 0.9533 0.017 Uiso 1 1 calc R . . C6 C -0.5474(4) -0.2971(4) 0.8210(3) 0.0119(6) Uani 1 1 d . . . C7 C -0.5434(4) -0.1878(4) 0.8824(3) 0.0126(6) Uani 1 1 d . . . O8 O -0.6053(3) -0.2072(3) 0.9918(2) 0.0153(5) Uani 1 1 d . . . O9 O -0.4748(3) -0.0821(3) 0.8222(2) 0.0173(5) Uani 1 1 d . . . C10 C -0.4581(4) -0.2967(4) 0.7097(3) 0.0127(6) Uani 1 1 d . . . H10 H -0.3956 -0.2254 0.6714 0.015 Uiso 1 1 calc R . . C11 C -0.4605(4) -0.4006(4) 0.6548(3) 0.0123(6) Uani 1 1 d . . . C12 C -0.5530(4) -0.5035(4) 0.7082(3) 0.0143(7) Uani 1 1 d . . . H12 H -0.5560 -0.5728 0.6693 0.017 Uiso 1 1 calc R . . O13 O -0.3729(3) -0.4109(3) 0.5462(2) 0.0153(5) Uani 1 1 d . . . C14 C -0.2484(4) -0.3369(4) 0.5053(3) 0.0155(7) Uani 1 1 d . . . H14A H -0.2946 -0.2255 0.4924 0.019 Uiso 1 1 calc R . . H14B H -0.1987 -0.3469 0.4247 0.019 Uiso 1 1 calc R . . O15 O -0.1261(3) -0.4105(3) 0.6010(2) 0.0144(5) Uani 1 1 d . . . C16 C -0.0317(4) -0.3173(4) 0.6007(3) 0.0125(6) Uani 1 1 d . . . C17 C 0.0780(4) -0.2766(4) 0.5016(3) 0.0149(7) Uani 1 1 d . . . H17 H 0.0891 -0.3111 0.4332 0.018 Uiso 1 1 calc R . . C18 C 0.1711(4) -0.1846(4) 0.5046(3) 0.0136(7) Uani 1 1 d . . . C19 C 0.2845(4) -0.1384(4) 0.3953(3) 0.0144(7) Uani 1 1 d . . . O20 O 0.3727(3) -0.0536(3) 0.4055(2) 0.0174(5) Uani 1 1 d . . . H20 H 0.4175 -0.0041 0.3324 0.026 Uiso 1 1 d R . . O21 O 0.2911(3) -0.1749(3) 0.3040(2) 0.0179(5) Uani 1 1 d . . . C22 C 0.1528(4) -0.1307(4) 0.6035(3) 0.0129(6) Uani 1 1 d . . . H22 H 0.2150 -0.0656 0.6033 0.015 Uiso 1 1 calc R . . C23 C 0.0430(4) -0.1726(4) 0.7021(3) 0.0120(6) Uani 1 1 d . . . C24 C 0.0233(4) -0.1099(4) 0.8060(3) 0.0124(6) Uani 1 1 d . . . O25 O 0.0739(3) 0.1517(3) 1.1017(2) 0.0152(5) Uani 1 1 d . . . O26 O 0.1027(3) -0.0163(3) 0.7935(2) 0.0166(5) Uani 1 1 d . . . C27 C -0.0489(4) -0.2677(4) 0.7014(3) 0.0136(6) Uani 1 1 d . . . H27 H -0.1226 -0.2982 0.7694 0.016 Uiso 1 1 calc R . . O28 O -0.1486(3) 0.3489(3) 0.8532(3) 0.0256(6) Uani 1 1 d . . . H28A H -0.2381 0.3155 0.8837 0.038 Uiso 1 1 d R . . H28B H -0.1594 0.4138 0.7725 0.038 Uiso 1 1 d 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 Ag1 0.02554(16) 0.02099(16) 0.01782(16) -0.01287(12) 0.00459(11) -0.01306(13) Ag2 0.03033(17) 0.02259(16) 0.01490(15) -0.01263(12) 0.00762(11) -0.01687(13) O1 0.0333(14) 0.0251(13) 0.0231(14) -0.0162(11) 0.0133(11) -0.0222(12) O2 0.0243(13) 0.0203(12) 0.0226(13) -0.0123(11) 0.0075(10) -0.0130(11) C3 0.0189(16) 0.0154(16) 0.0156(17) -0.0063(14) -0.0007(13) -0.0043(14) C4 0.0158(15) 0.0117(15) 0.0136(16) -0.0044(13) -0.0015(13) -0.0042(13) C5 0.0159(16) 0.0144(16) 0.0123(16) -0.0032(13) 0.0002(12) -0.0060(14) C6 0.0126(14) 0.0096(14) 0.0135(16) -0.0033(12) -0.0006(12) -0.0039(13) C7 0.0129(15) 0.0107(15) 0.0151(16) -0.0058(13) -0.0024(12) -0.0023(13) O8 0.0199(12) 0.0187(12) 0.0132(12) -0.0097(10) 0.0041(9) -0.0103(10) O9 0.0260(13) 0.0184(12) 0.0142(12) -0.0086(10) 0.0061(10) -0.0149(11) C10 0.0127(15) 0.0131(15) 0.0142(16) -0.0059(13) -0.0011(12) -0.0043(13) C11 0.0110(14) 0.0153(16) 0.0126(16) -0.0060(13) -0.0006(12) -0.0050(13) C12 0.0111(15) 0.0178(16) 0.0161(17) -0.0087(14) -0.0011(12) -0.0032(14) O13 0.0162(11) 0.0221(12) 0.0154(12) -0.0125(10) 0.0055(9) -0.0112(10) C14 0.0178(16) 0.0195(17) 0.0130(16) -0.0070(13) 0.0014(13) -0.0095(15) O15 0.0164(11) 0.0154(11) 0.0154(12) -0.0061(10) 0.0004(9) -0.0095(10) C16 0.0123(15) 0.0125(15) 0.0148(16) -0.0058(13) 0.0011(12) -0.0058(13) C17 0.0182(16) 0.0164(16) 0.0126(16) -0.0068(13) -0.0019(13) -0.0055(14) C18 0.0144(15) 0.0133(15) 0.0121(16) -0.0038(13) 0.0006(12) -0.0038(14) C19 0.0155(15) 0.0146(16) 0.0138(16) -0.0050(13) -0.0039(13) -0.0040(14) O20 0.0210(12) 0.0232(13) 0.0143(12) -0.0084(10) 0.0057(10) -0.0152(11) O21 0.0215(12) 0.0228(13) 0.0152(12) -0.0094(10) 0.0052(10) -0.0133(11) C22 0.0139(15) 0.0108(14) 0.0132(16) -0.0027(12) -0.0021(12) -0.0037(13) C23 0.0129(15) 0.0140(15) 0.0099(15) -0.0048(13) -0.0002(12) -0.0041(13) C24 0.0124(15) 0.0121(15) 0.0130(16) -0.0054(13) -0.0022(12) -0.0019(13) O25 0.0222(12) 0.0186(12) 0.0100(11) -0.0081(10) 0.0055(9) -0.0117(10) O26 0.0197(12) 0.0222(12) 0.0160(12) -0.0125(10) 0.0066(10) -0.0128(11) C27 0.0132(15) 0.0168(16) 0.0126(16) -0.0078(13) 0.0020(12) -0.0047(14) O28 0.0266(14) 0.0271(14) 0.0240(14) -0.0076(12) 0.0030(11) -0.0125(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 Ag1 O26 2.181(2) . ? Ag1 O25 2.276(2) . ? Ag1 O28 2.478(3) . ? Ag1 O2 2.497(2) 1_665 ? Ag1 Ag1 2.8588(5) 2_557 ? Ag1 Ag2 3.1778(4) 2_557 ? Ag2 O8 2.194(2) 2_457 ? Ag2 O9 2.247(2) . ? Ag2 O21 2.399(2) 2_556 ? Ag2 Ag2 2.7929(5) 2_457 ? Ag2 Ag1 3.1778(4) 2_557 ? O1 C3 1.318(4) . ? O1 H1 0.8988 . ? O2 C3 1.227(4) . ? O2 Ag1 2.497(2) 1_445 ? C3 C4 1.488(5) . ? C4 C12 1.391(5) . ? C4 C5 1.402(5) . ? C5 C6 1.398(4) . ? C5 H5 0.9500 . ? C6 C10 1.395(5) . ? C6 C7 1.496(5) . ? C7 O8 1.264(4) . ? C7 O9 1.272(4) . ? O8 Ag2 2.194(2) 2_457 ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 C12 1.383(4) . ? C11 O13 1.385(4) . ? C12 H12 0.9500 . ? O13 C14 1.403(4) . ? C14 O15 1.439(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C16 1.395(4) . ? C16 C17 1.390(5) . ? C16 C27 1.389(5) . ? C17 C18 1.389(5) . ? C17 H17 0.9500 . ? C18 C22 1.395(5) . ? C18 C19 1.494(5) . ? C19 O21 1.219(4) . ? C19 O20 1.328(4) . ? O20 H20 0.8983 . ? O21 Ag2 2.399(2) 2_556 ? C22 C23 1.389(4) . ? C22 H22 0.9500 . ? C23 C27 1.397(5) . ? C23 C24 1.504(5) . ? C24 O26 1.259(4) . ? C24 O25 1.275(4) 2_557 ? O25 C24 1.275(4) 2_557 ? C27 H27 0.9500 . ? O28 H28A 0.9012 . ? O28 H28B 0.9011 . ? 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 O26 Ag1 O25 159.48(9) . . ? O26 Ag1 O28 108.65(9) . . ? O25 Ag1 O28 85.97(9) . . ? O26 Ag1 O2 109.06(8) . 1_665 ? O25 Ag1 O2 85.79(8) . 1_665 ? O28 Ag1 O2 85.61(9) . 1_665 ? O26 Ag1 Ag1 83.12(6) . 2_557 ? O25 Ag1 Ag1 79.90(6) . 2_557 ? O28 Ag1 Ag1 101.04(6) . 2_557 ? O2 Ag1 Ag1 163.70(6) 1_665 2_557 ? O26 Ag1 Ag2 108.22(6) . 2_557 ? O25 Ag1 Ag2 60.83(6) . 2_557 ? O28 Ag1 Ag2 142.31(6) . 2_557 ? O2 Ag1 Ag2 75.33(6) 1_665 2_557 ? Ag1 Ag1 Ag2 90.775(12) 2_557 2_557 ? O8 Ag2 O9 161.98(9) 2_457 . ? O8 Ag2 O21 106.55(8) 2_457 2_556 ? O9 Ag2 O21 85.59(8) . 2_556 ? O8 Ag2 Ag2 85.05(6) 2_457 2_457 ? O9 Ag2 Ag2 79.75(6) . 2_457 ? O21 Ag2 Ag2 159.96(6) 2_556 2_457 ? O8 Ag2 Ag1 72.44(6) 2_457 2_557 ? O9 Ag2 Ag1 117.60(6) . 2_557 ? O21 Ag2 Ag1 106.37(6) 2_556 2_557 ? Ag2 Ag2 Ag1 92.577(13) 2_457 2_557 ? C3 O1 H1 115.4 . . ? C3 O2 Ag1 123.6(2) . 1_445 ? O2 C3 O1 123.8(3) . . ? O2 C3 C4 122.8(3) . . ? O1 C3 C4 113.4(3) . . ? C12 C4 C5 120.8(3) . . ? C12 C4 C3 119.3(3) . . ? C5 C4 C3 119.9(3) . . ? C6 C5 C4 119.1(3) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C10 C6 C5 120.0(3) . . ? C10 C6 C7 120.6(3) . . ? C5 C6 C7 119.4(3) . . ? O8 C7 O9 123.6(3) . . ? O8 C7 C6 118.4(3) . . ? O9 C7 C6 118.0(3) . . ? C7 O8 Ag2 123.0(2) . 2_457 ? C7 O9 Ag2 126.1(2) . . ? C11 C10 C6 120.0(3) . . ? C11 C10 H10 120.0 . . ? C6 C10 H10 120.0 . . ? C12 C11 O13 115.3(3) . . ? C12 C11 C10 120.7(3) . . ? O13 C11 C10 124.0(3) . . ? C11 C12 C4 119.4(3) . . ? C11 C12 H12 120.3 . . ? C4 C12 H12 120.3 . . ? C11 O13 C14 117.4(2) . . ? O13 C14 O15 107.3(2) . . ? O13 C14 H14A 110.2 . . ? O15 C14 H14A 110.2 . . ? O13 C14 H14B 110.2 . . ? O15 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? C16 O15 C14 113.9(2) . . ? C17 C16 C27 121.1(3) . . ? C17 C16 O15 120.1(3) . . ? C27 C16 O15 118.7(3) . . ? C16 C17 C18 118.8(3) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C17 C18 C22 120.9(3) . . ? C17 C18 C19 117.8(3) . . ? C22 C18 C19 121.2(3) . . ? O21 C19 O20 123.8(3) . . ? O21 C19 C18 121.4(3) . . ? O20 C19 C18 114.7(3) . . ? C19 O20 H20 113.9 . . ? C19 O21 Ag2 128.1(2) . 2_556 ? C23 C22 C18 119.7(3) . . ? C23 C22 H22 120.2 . . ? C18 C22 H22 120.2 . . ? C22 C23 C27 119.9(3) . . ? C22 C23 C24 118.5(3) . . ? C27 C23 C24 121.6(3) . . ? O26 C24 O25 124.6(3) . 2_557 ? O26 C24 C23 116.8(3) . . ? O25 C24 C23 118.5(3) 2_557 . ? C24 O25 Ag1 123.7(2) 2_557 . ? C24 O26 Ag1 125.3(2) . . ? C16 C27 C23 119.5(3) . . ? C16 C27 H27 120.2 . . ? C23 C27 H27 120.2 . . ? Ag1 O28 H28A 103.4 . . ? Ag1 O28 H28B 121.5 . . ? H28A O28 H28B 112.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O25 0.90 1.79 2.625(3) 153.5 1_445 O20 H20 O9 0.90 1.73 2.615(3) 168.0 2_556 O28 H28A O8 0.90 2.04 2.908(3) 160.0 2_457 O28 H28B O15 0.90 2.12 2.989(3) 161.1 1_565 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.268 _refine_diff_density_min -1.222 _refine_diff_density_rms 0.138 #========================END================================ data_6 _database_code_depnum_ccdc_archive 'CCDC 779787' #TrackingRef '- Paper2-CIF_a.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Cd O10' _chemical_formula_sum 'C18 H12 Cd O10' _chemical_formula_weight 500.68 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 13.8667(4) _cell_length_b 14.8068(4) _cell_length_c 14.6050(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.1755(12) _cell_angle_gamma 90.00 _cell_volume 2735.72(13) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3349 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour colorless _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 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8182 _exptl_absorpt_correction_T_max 0.8848 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23187 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.87 _reflns_number_total 3256 _reflns_number_gt 2925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains an unidetified amount of severely disordered solvent (methanol, or a mixture of methanol and DMF), which could not be modeled by discrete atoms. Its contribution to the diffraction pattern was thus subtracted by the Squeeze procedure using the PLATON software (Spek, 2003). ; _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^)+(0.0701P)^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 SHELXL _refine_ls_extinction_coef 0.0017(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3256 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Cd Cd 0.0000 0.568598(13) 0.2500 0.03365(12) Uani 1 2 d S . . O1 O 0.12361(17) 0.45098(15) 0.24514(17) 0.0543(5) Uani 1 1 d . . . O2 O 0.13184(14) 0.49622(12) 0.39049(15) 0.0515(4) Uani 1 1 d . . . C3 C 0.1633(2) 0.44707(16) 0.3387(2) 0.0441(6) Uani 1 1 d . . . C4 C 0.25142(18) 0.38059(16) 0.39089(19) 0.0446(5) Uani 1 1 d . . . C5 C 0.28441(18) 0.32196(16) 0.33439(19) 0.0434(5) Uani 1 1 d . . . H5 H 0.2524 0.3243 0.2632 0.052 Uiso 1 1 calc R . . C6 C 0.36458(18) 0.26015(15) 0.3834(2) 0.0448(5) Uani 1 1 d . . . C7 C 0.40246(18) 0.19693(16) 0.3246(2) 0.0482(6) Uani 1 1 d . . . O8 O 0.36710(17) 0.19967(16) 0.23323(17) 0.0637(6) Uani 1 1 d . . . O9 O 0.47186(15) 0.13917(12) 0.37516(16) 0.0569(5) Uani 1 1 d . . . H9 H 0.5126 0.1546 0.3467 0.068 Uiso 1 1 d R . . C10 C 0.41051(17) 0.25649(15) 0.4878(2) 0.0461(6) Uani 1 1 d . . . H10 H 0.4649 0.2139 0.5211 0.055 Uiso 1 1 calc R . . C11 C 0.37744(19) 0.31448(16) 0.54315(19) 0.0465(6) Uani 1 1 d . . . C12 C 0.29716(19) 0.37679(16) 0.4950(2) 0.0480(6) Uani 1 1 d . . . H12 H 0.2740 0.4163 0.5331 0.058 Uiso 1 1 calc R . . O13 O 0.41851(15) 0.31570(12) 0.64593(14) 0.0554(5) Uani 1 1 d . . . C14 C 0.4919(2) 0.24513(19) 0.6947(2) 0.0573(7) Uani 1 1 d . . . H14A H 0.5598 0.2561 0.6895 0.069 Uiso 1 1 calc R . . H14B H 0.4635 0.1862 0.6633 0.069 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 Cd 0.02899(15) 0.02784(15) 0.03399(16) 0.000 0.00262(10) 0.000 O1 0.0459(11) 0.0529(10) 0.0538(12) 0.0028(9) 0.0098(9) 0.0218(9) O2 0.0453(9) 0.0418(9) 0.0576(11) -0.0022(8) 0.0111(8) 0.0194(7) C3 0.0331(12) 0.0347(11) 0.0544(16) 0.0008(10) 0.0076(11) 0.0101(9) C4 0.0351(11) 0.0338(11) 0.0545(14) -0.0029(10) 0.0077(10) 0.0131(9) C5 0.0353(11) 0.0382(11) 0.0470(13) -0.0042(10) 0.0070(10) 0.0100(9) C6 0.0339(11) 0.0321(11) 0.0583(15) -0.0059(10) 0.0087(10) 0.0070(9) C7 0.0335(11) 0.0350(12) 0.0709(18) -0.0106(11) 0.0161(11) 0.0021(9) O8 0.0581(11) 0.0666(13) 0.0569(12) -0.0149(10) 0.0139(10) 0.0185(10) O9 0.0535(10) 0.0371(9) 0.0802(14) -0.0022(9) 0.0275(10) 0.0171(8) C10 0.0346(11) 0.0330(11) 0.0596(15) -0.0003(10) 0.0080(10) 0.0088(9) C11 0.0389(12) 0.0389(12) 0.0476(13) -0.0009(10) 0.0035(10) 0.0053(9) C12 0.0418(12) 0.0372(12) 0.0556(15) -0.0077(10) 0.0105(11) 0.0091(10) O13 0.0548(10) 0.0461(10) 0.0476(10) -0.0023(8) 0.0030(8) 0.0101(8) C14 0.0536(15) 0.0448(14) 0.0543(16) 0.0005(12) 0.0026(13) 0.0059(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 Cd O9 2.274(2) 4 ? Cd O9 2.274(2) 3_455 ? Cd O2 2.3724(18) . ? Cd O2 2.3724(18) 2 ? Cd O1 2.4649(19) 2 ? Cd O1 2.4649(19) . ? Cd O8 2.618(2) 3_455 ? Cd O8 2.618(2) 4 ? O1 C3 1.248(4) . ? O2 C3 1.250(3) . ? C3 C4 1.510(3) . ? C4 C12 1.388(4) . ? C4 C5 1.397(3) . ? C5 C6 1.391(3) . ? C5 H5 0.9500 . ? C6 C10 1.392(4) . ? C6 C7 1.503(3) . ? C7 O8 1.219(4) . ? C7 O9 1.273(3) . ? O8 Cd 2.618(2) 3_545 ? O9 Cd 2.274(2) 3_545 ? O9 H9 0.8574 . ? C10 C11 1.380(4) . ? C10 H10 0.9500 . ? C11 O13 1.370(3) . ? C11 C12 1.394(3) . ? C12 H12 0.9500 . ? O13 C14 1.428(3) . ? C14 C14 1.535(6) 2_656 ? C14 H14A 0.9900 . ? C14 H14B 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 O9 Cd O9 125.28(10) 4 3_455 ? O9 Cd O2 125.29(7) 4 . ? O9 Cd O2 80.64(6) 3_455 . ? O9 Cd O2 80.65(6) 4 2 ? O9 Cd O2 125.29(7) 3_455 2 ? O2 Cd O2 126.29(9) . 2 ? O9 Cd O1 134.28(7) 4 2 ? O9 Cd O1 87.20(8) 3_455 2 ? O2 Cd O1 87.40(7) . 2 ? O2 Cd O1 53.64(7) 2 2 ? O9 Cd O1 87.21(8) 4 . ? O9 Cd O1 134.28(7) 3_455 . ? O2 Cd O1 53.64(7) . . ? O2 Cd O1 87.40(7) 2 . ? O1 Cd O1 90.09(12) 2 . ? O9 Cd O8 85.99(7) 4 3_455 ? O9 Cd O8 52.30(7) 3_455 3_455 ? O2 Cd O8 132.80(6) . 3_455 ? O2 Cd O8 89.45(7) 2 3_455 ? O1 Cd O8 93.17(10) 2 3_455 ? O1 Cd O8 172.89(7) . 3_455 ? O9 Cd O8 52.30(7) 4 4 ? O9 Cd O8 85.99(7) 3_455 4 ? O2 Cd O8 89.45(7) . 4 ? O2 Cd O8 132.80(6) 2 4 ? O1 Cd O8 172.89(7) 2 4 ? O1 Cd O8 93.17(10) . 4 ? O8 Cd O8 84.31(11) 3_455 4 ? C3 O1 Cd 90.09(16) . . ? C3 O2 Cd 94.37(16) . . ? O1 C3 O2 121.9(2) . . ? O1 C3 C4 119.1(2) . . ? O2 C3 C4 119.0(3) . . ? C12 C4 C5 120.5(2) . . ? C12 C4 C3 119.4(2) . . ? C5 C4 C3 120.0(2) . . ? C6 C5 C4 119.4(2) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C10 120.0(2) . . ? C5 C6 C7 120.6(2) . . ? C10 C6 C7 119.4(2) . . ? O8 C7 O9 121.8(2) . . ? O8 C7 C6 121.8(2) . . ? O9 C7 C6 116.4(3) . . ? C7 O8 Cd 85.45(16) . 3_545 ? C7 O9 Cd 100.38(18) . 3_545 ? C7 O9 H9 91.8 . . ? C11 C10 C6 120.3(2) . . ? C11 C10 H10 119.8 . . ? C6 C10 H10 119.8 . . ? O13 C11 C10 124.1(2) . . ? O13 C11 C12 115.6(2) . . ? C10 C11 C12 120.3(2) . . ? C4 C12 C11 119.4(2) . . ? C4 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C11 O13 C14 115.4(2) . . ? O13 C14 C14 107.0(2) . 2_656 ? O13 C14 H14A 110.3 . . ? C14 C14 H14A 110.3 2_656 . ? O13 C14 H14B 110.3 . . ? C14 C14 H14B 110.3 2_656 . ? H14A C14 H14B 108.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9 O8 0.86 2.49 3.345(3) 179 2_655 # 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 -0.012 -0.007 -0.010 1194 297 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.095 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.082 #=======================END============================================= data_7 _database_code_depnum_ccdc_archive 'CCDC 779788' #TrackingRef '- Paper2-CIF_a.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 N3 O13 Zn2, C3 H7 N O' _chemical_formula_sum 'C30 H38 N4 O14 Zn2' _chemical_formula_weight 809.38 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.10990(10) _cell_length_b 13.89090(10) _cell_length_c 22.4850(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3470.03(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4456 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6299 _exptl_absorpt_correction_T_max 0.7596 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24555 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.87 _reflns_number_total 8172 _reflns_number_gt 6691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(9) _refine_ls_number_reflns 8172 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.36789(3) -0.14083(2) 0.347009(14) 0.01257(8) Uani 1 1 d . . . Zn2 Zn 0.13414(3) -0.01874(2) 0.438606(15) 0.01516(9) Uani 1 1 d . . . O1 O -0.1847(2) 0.51390(14) 0.53604(10) 0.0191(5) Uani 1 1 d . . . C2 C -0.1135(3) 0.58277(19) 0.52909(14) 0.0155(6) Uani 1 1 d . . . O3 O -0.07900(19) 0.64054(14) 0.56973(9) 0.0171(4) Uani 1 1 d . . . C4 C -0.0590(3) 0.5975(2) 0.46877(14) 0.0153(6) Uani 1 1 d . . . C5 C -0.0838(3) 0.53259(19) 0.42346(13) 0.0155(6) Uani 1 1 d . . . H5 H -0.1379 0.4808 0.4303 0.019 Uiso 1 1 calc R . . C6 C -0.0299(3) 0.5431(2) 0.36815(14) 0.0176(7) Uani 1 1 d . . . C7 C 0.0509(3) 0.61795(19) 0.35715(14) 0.0157(6) Uani 1 1 d . . . H7 H 0.0895 0.6240 0.3196 0.019 Uiso 1 1 calc R . . C8 C 0.0735(3) 0.68401(19) 0.40297(13) 0.0136(6) Uani 1 1 d . . . C9 C 0.0170(3) 0.6750(2) 0.45739(14) 0.0148(6) Uani 1 1 d . . . H9 H 0.0302 0.7221 0.4873 0.018 Uiso 1 1 calc R . . C10 C 0.1576(3) 0.76778(19) 0.39303(13) 0.0121(6) Uani 1 1 d . . . O11 O 0.22900(18) 0.76623(13) 0.34912(10) 0.0155(4) Uani 1 1 d . . . O12 O 0.15065(19) 0.83391(12) 0.43126(9) 0.0163(4) Uani 1 1 d . . . O13 O -0.0621(2) 0.47430(15) 0.32737(9) 0.0215(5) Uani 1 1 d . . . C14 C 0.0053(3) 0.4704(2) 0.27362(13) 0.0168(6) Uani 1 1 d . . . H14A H 0.0926 0.4670 0.2823 0.020 Uiso 1 1 calc R . . H14B H -0.0102 0.5283 0.2491 0.020 Uiso 1 1 calc R . . C15 C -0.0351(3) 0.38128(18) 0.24141(14) 0.0153(6) Uani 1 1 d . . . H15A H -0.1236 0.3835 0.2364 0.018 Uiso 1 1 calc R . . H15B H 0.0016 0.3804 0.2013 0.018 Uiso 1 1 calc R . . O16 O -0.00326(19) 0.29495(14) 0.27204(10) 0.0168(5) Uani 1 1 d . . . C17 C 0.1133(3) 0.26332(19) 0.26766(13) 0.0150(6) Uani 1 1 d . . . C18 C 0.1345(3) 0.17561(18) 0.29637(12) 0.0143(6) Uani 1 1 d . . . H18 H 0.0720 0.1460 0.3187 0.017 Uiso 1 1 calc R . . C19 C 0.2458(3) 0.1318(2) 0.29248(13) 0.0139(6) Uani 1 1 d . . . C20 C 0.3399(3) 0.1774(2) 0.26224(13) 0.0157(7) Uani 1 1 d . . . H20 H 0.4167 0.1477 0.2596 0.019 Uiso 1 1 calc R . . C21 C 0.3198(3) 0.26735(19) 0.23600(13) 0.0142(6) Uani 1 1 d . . . C22 C 0.2062(3) 0.3091(2) 0.23782(14) 0.0157(6) Uani 1 1 d . . . H22 H 0.1922 0.3690 0.2186 0.019 Uiso 1 1 calc R . . C23 C 0.4184(3) 0.3212(2) 0.20432(14) 0.0171(7) Uani 1 1 d . . . O24 O 0.52267(19) 0.28128(14) 0.20224(10) 0.0185(5) Uani 1 1 d . . . O25 O 0.3948(2) 0.40024(15) 0.18114(10) 0.0232(5) Uani 1 1 d . . . C26 C 0.2587(3) 0.0339(2) 0.31999(13) 0.0152(6) Uani 1 1 d . . . O27 O 0.3550(2) -0.01293(13) 0.30940(9) 0.0184(4) Uani 1 1 d . . . O28 O 0.17270(18) 0.00158(13) 0.34945(10) 0.0163(4) Uani 1 1 d . . . O29 O -0.0501(2) -0.02244(16) 0.41609(11) 0.0280(6) Uani 1 1 d . . . C30 C -0.1045(3) -0.1017(2) 0.41506(15) 0.0225(8) Uani 1 1 d . . . H30 H -0.0606 -0.1562 0.4016 0.027 Uiso 1 1 calc R . . N31 N -0.2165(3) -0.11580(18) 0.43095(13) 0.0213(6) Uani 1 1 d . . . C32 C -0.2684(3) -0.2125(2) 0.43005(16) 0.0242(7) Uani 1 1 d . . . H32A H -0.2212 -0.2536 0.4034 0.036 Uiso 1 1 calc R . . H32B H -0.3517 -0.2092 0.4158 0.036 Uiso 1 1 calc R . . H32C H -0.2671 -0.2395 0.4703 0.036 Uiso 1 1 calc R . . C33 C -0.2901(3) -0.0370(3) 0.45316(19) 0.0348(9) Uani 1 1 d . . . H33A H -0.3061 -0.0466 0.4956 0.052 Uiso 1 1 calc R . . H33B H -0.3664 -0.0351 0.4313 0.052 Uiso 1 1 calc R . . H33C H -0.2472 0.0240 0.4475 0.052 Uiso 1 1 calc R . . O34 O 0.0729(2) -0.04386(16) 0.52519(10) 0.0308(6) Uani 1 1 d . . . C35 C 0.0773(3) 0.0118(2) 0.56758(15) 0.0286(8) Uani 1 1 d . . . H35 H 0.1255 0.0680 0.5637 0.034 Uiso 1 1 calc R . . N36 N 0.0197(3) -0.00137(19) 0.61805(13) 0.0312(7) Uani 1 1 d . . . C37 C -0.0616(5) -0.0827(3) 0.6266(2) 0.0497(12) Uani 1 1 d . . . H37A H -0.0630 -0.1220 0.5904 0.075 Uiso 1 1 calc R . . H37B H -0.1429 -0.0588 0.6349 0.075 Uiso 1 1 calc R . . H37C H -0.0335 -0.1218 0.6601 0.075 Uiso 1 1 calc R . . C38 C 0.0350(5) 0.0646(3) 0.66800(17) 0.0531(14) Uani 1 1 d . . . H38A H 0.0860 0.1187 0.6558 0.080 Uiso 1 1 calc R . . H38B H 0.0733 0.0305 0.7012 0.080 Uiso 1 1 calc R . . H38C H -0.0438 0.0889 0.6806 0.080 Uiso 1 1 calc R . . O39 O 0.1256(2) 0.12831(14) 0.45184(10) 0.0233(5) Uani 1 1 d . . . C40 C 0.2129(3) 0.1821(2) 0.44422(15) 0.0231(7) Uani 1 1 d . . . H40 H 0.2906 0.1540 0.4410 0.028 Uiso 1 1 calc R . . N41 N 0.2036(3) 0.27672(18) 0.44035(14) 0.0288(7) Uani 1 1 d . . . C42 C 0.3084(5) 0.3363(3) 0.4286(3) 0.0662(17) Uani 1 1 d . . . H42A H 0.3788 0.2951 0.4223 0.099 Uiso 1 1 calc R . . H42B H 0.3230 0.3788 0.4627 0.099 Uiso 1 1 calc R . . H42C H 0.2941 0.3753 0.3930 0.099 Uiso 1 1 calc R . . C43 C 0.0867(4) 0.3227(2) 0.44362(19) 0.0383(10) Uani 1 1 d . . . H43A H 0.0603 0.3406 0.4035 0.057 Uiso 1 1 calc R . . H43B H 0.0923 0.3806 0.4684 0.057 Uiso 1 1 calc R . . H43C H 0.0284 0.2780 0.4612 0.057 Uiso 1 1 calc R . . O44 O 0.4582(3) 0.6921(3) 0.08734(16) 0.0669(10) Uani 1 1 d . . . C45 C 0.4127(4) 0.6509(3) 0.12972(19) 0.0413(10) Uani 1 1 d . . . H45 H 0.4615 0.6067 0.1511 0.050 Uiso 1 1 calc R . . N46 N 0.3000(3) 0.6632(2) 0.14819(15) 0.0371(8) Uani 1 1 d . . . C47 C 0.2526(5) 0.6121(3) 0.1992(2) 0.0583(15) Uani 1 1 d . . . H47A H 0.3162 0.5725 0.2168 0.088 Uiso 1 1 calc R . . H47B H 0.1858 0.5707 0.1866 0.088 Uiso 1 1 calc R . . H47C H 0.2235 0.6586 0.2287 0.088 Uiso 1 1 calc R . . C48 C 0.2152(5) 0.7259(3) 0.1163(2) 0.0621(14) Uani 1 1 d . . . H48A H 0.2555 0.7544 0.0817 0.093 Uiso 1 1 calc R . . H48B H 0.1875 0.7771 0.1429 0.093 Uiso 1 1 calc R . . H48C H 0.1460 0.6878 0.1029 0.093 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 Zn1 0.01386(17) 0.00982(14) 0.01404(17) 0.00067(12) 0.00096(16) 0.00038(14) Zn2 0.01640(17) 0.01135(15) 0.01774(18) -0.00070(12) 0.00249(16) 0.00056(15) O1 0.0208(12) 0.0109(10) 0.0257(12) 0.0020(9) 0.0076(10) -0.0008(9) C2 0.0137(17) 0.0103(13) 0.0226(17) 0.0002(11) 0.0022(13) 0.0026(11) O3 0.0188(11) 0.0194(10) 0.0131(11) 0.0006(9) 0.0004(9) -0.0024(9) C4 0.0131(16) 0.0129(14) 0.0199(17) 0.0016(12) 0.0013(13) 0.0030(12) C5 0.0161(15) 0.0108(14) 0.0195(17) 0.0005(11) -0.0004(13) -0.0004(12) C6 0.0198(17) 0.0134(14) 0.0196(17) -0.0044(12) 0.0002(13) -0.0004(12) C7 0.0153(15) 0.0145(14) 0.0172(17) 0.0018(11) 0.0021(13) 0.0006(11) C8 0.0161(16) 0.0087(13) 0.0159(16) 0.0013(11) -0.0005(13) 0.0010(12) C9 0.0134(16) 0.0119(14) 0.0189(17) -0.0017(11) -0.0005(13) 0.0011(11) C10 0.0126(17) 0.0113(13) 0.0124(15) 0.0022(10) -0.0005(12) 0.0008(11) O11 0.0166(11) 0.0126(9) 0.0172(11) 0.0005(8) 0.0022(10) -0.0006(8) O12 0.0218(12) 0.0102(9) 0.0170(11) -0.0012(8) 0.0015(10) -0.0038(8) O13 0.0244(13) 0.0197(11) 0.0205(12) -0.0079(9) 0.0081(10) -0.0087(10) C14 0.0207(17) 0.0142(15) 0.0156(16) 0.0020(12) 0.0012(13) 0.0016(13) C15 0.0159(16) 0.0144(15) 0.0157(16) -0.0010(11) 0.0001(13) 0.0050(12) O16 0.0149(11) 0.0105(10) 0.0249(13) 0.0036(8) 0.0019(9) 0.0030(8) C17 0.0148(17) 0.0149(13) 0.0152(15) -0.0051(11) 0.0004(12) 0.0038(12) C18 0.0141(14) 0.0116(12) 0.0173(15) 0.0031(10) 0.0035(14) -0.0041(13) C19 0.0183(16) 0.0124(13) 0.0109(15) 0.0015(11) -0.0011(12) -0.0017(12) C20 0.0162(17) 0.0131(13) 0.0176(17) 0.0013(11) -0.0007(12) -0.0002(11) C21 0.0181(16) 0.0112(13) 0.0133(16) -0.0005(11) -0.0012(12) -0.0013(12) C22 0.0185(17) 0.0098(14) 0.0189(17) 0.0023(11) -0.0004(13) 0.0005(12) C23 0.0179(17) 0.0149(14) 0.0184(17) -0.0015(12) 0.0003(14) 0.0001(13) O24 0.0163(12) 0.0141(10) 0.0252(13) 0.0000(9) 0.0061(10) -0.0008(9) O25 0.0228(14) 0.0152(10) 0.0316(13) 0.0085(9) 0.0041(10) -0.0031(9) C26 0.0182(17) 0.0141(14) 0.0133(16) 0.0002(12) -0.0036(13) -0.0002(12) O27 0.0191(12) 0.0135(9) 0.0228(12) 0.0038(8) 0.0046(10) 0.0032(10) O28 0.0160(11) 0.0154(10) 0.0174(11) 0.0032(8) -0.0015(9) -0.0026(8) O29 0.0158(12) 0.0196(11) 0.0484(16) 0.0034(10) 0.0060(11) -0.0013(10) C30 0.0198(19) 0.0207(16) 0.0270(19) 0.0035(13) 0.0009(14) 0.0032(13) N31 0.0191(14) 0.0195(13) 0.0252(16) 0.0008(11) 0.0016(12) -0.0023(11) C32 0.0212(18) 0.0209(16) 0.030(2) 0.0050(14) 0.0023(15) -0.0007(13) C33 0.022(2) 0.0247(18) 0.057(3) -0.0015(17) 0.0143(18) -0.0012(15) O34 0.0464(16) 0.0227(12) 0.0232(14) -0.0030(10) 0.0107(12) 0.0004(11) C35 0.0311(19) 0.0269(17) 0.028(2) -0.0010(15) 0.0011(16) 0.0014(15) N36 0.048(2) 0.0291(16) 0.0168(15) 0.0028(12) 0.0037(14) 0.0105(14) C37 0.075(3) 0.036(2) 0.038(3) 0.0051(18) 0.015(2) -0.004(2) C38 0.090(4) 0.049(3) 0.021(2) -0.0077(17) 0.001(2) 0.014(3) O39 0.0261(13) 0.0146(10) 0.0291(13) -0.0039(8) 0.0023(11) 0.0033(10) C40 0.030(2) 0.0154(15) 0.0234(19) -0.0029(13) 0.0004(16) 0.0038(14) N41 0.0402(19) 0.0125(13) 0.0338(18) 0.0015(12) 0.0061(16) 0.0021(12) C42 0.062(3) 0.023(2) 0.114(5) -0.002(2) 0.044(3) -0.010(2) C43 0.049(3) 0.0185(17) 0.047(3) 0.0008(16) -0.003(2) 0.0102(16) O44 0.053(2) 0.093(3) 0.055(2) 0.0012(19) 0.0172(18) -0.021(2) C45 0.035(2) 0.053(2) 0.036(2) -0.0092(19) -0.0003(19) -0.007(2) N46 0.038(2) 0.0359(17) 0.037(2) 0.0067(15) 0.0124(17) 0.0037(14) C47 0.078(4) 0.040(2) 0.056(3) 0.010(2) 0.036(3) 0.008(2) C48 0.067(4) 0.048(3) 0.071(4) 0.018(2) 0.008(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.963(2) 3_556 ? Zn1 O24 1.969(2) 4_645 ? Zn1 O27 1.9728(19) . ? Zn1 O11 2.012(2) 1_545 ? Zn2 O12 2.0617(18) 1_545 ? Zn2 O39 2.0663(19) . ? Zn2 O28 2.069(2) . ? Zn2 O1 2.093(2) 3_556 ? Zn2 O34 2.092(2) . ? Zn2 O29 2.109(2) . ? O1 C2 1.251(4) . ? O1 Zn2 2.093(2) 3_456 ? C2 O3 1.275(4) . ? C2 C4 1.499(4) . ? O3 Zn1 1.963(2) 3_456 ? C4 C5 1.388(4) . ? C4 C9 1.392(4) . ? C5 C6 1.388(4) . ? C5 H5 0.9500 . ? C6 O13 1.371(4) . ? C6 C7 1.396(4) . ? C7 C8 1.402(4) . ? C7 H7 0.9500 . ? C8 C9 1.381(4) . ? C8 C10 1.509(4) . ? C9 H9 0.9500 . ? C10 O12 1.260(3) . ? C10 O11 1.267(3) . ? O11 Zn1 2.012(2) 1_565 ? O12 Zn2 2.0618(18) 1_565 ? O13 C14 1.423(4) . ? C14 C15 1.503(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O16 1.428(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C17 1.371(4) . ? C17 C22 1.385(4) . ? C17 C18 1.399(4) . ? C18 C19 1.381(4) . ? C18 H18 0.9500 . ? C19 C20 1.399(4) . ? C19 C26 1.501(4) . ? C20 C21 1.399(4) . ? C20 H20 0.9500 . ? C21 C22 1.390(4) . ? C21 C23 1.505(4) . ? C22 H22 0.9500 . ? C23 O25 1.244(4) . ? C23 O24 1.285(4) . ? O24 Zn1 1.969(2) 4_655 ? C26 O28 1.246(4) . ? C26 O27 1.275(4) . ? O29 C30 1.257(4) . ? C30 N31 1.309(4) . ? C30 H30 0.9500 . ? N31 C33 1.455(4) . ? N31 C32 1.462(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O34 C35 1.229(4) . ? C35 N36 1.316(5) . ? C35 H35 0.9500 . ? N36 C37 1.458(5) . ? N36 C38 1.459(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O39 C40 1.237(4) . ? C40 N41 1.321(4) . ? C40 H40 0.9500 . ? N41 C43 1.449(5) . ? N41 C42 1.453(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O44 C45 1.221(5) . ? C45 N46 1.330(5) . ? C45 H45 0.9500 . ? N46 C47 1.448(5) . ? N46 C48 1.470(6) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 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 O3 Zn1 O24 110.61(9) 3_556 4_645 ? O3 Zn1 O27 115.39(9) 3_556 . ? O24 Zn1 O27 107.38(9) 4_645 . ? O3 Zn1 O11 102.08(9) 3_556 1_545 ? O24 Zn1 O11 97.72(8) 4_645 1_545 ? O27 Zn1 O11 122.15(9) . 1_545 ? O12 Zn2 O39 175.58(9) 1_545 . ? O12 Zn2 O28 92.25(8) 1_545 . ? O39 Zn2 O28 90.82(8) . . ? O12 Zn2 O1 88.17(8) 1_545 3_556 ? O39 Zn2 O1 88.48(9) . 3_556 ? O28 Zn2 O1 93.46(8) . 3_556 ? O12 Zn2 O34 86.44(8) 1_545 . ? O39 Zn2 O34 90.91(9) . . ? O28 Zn2 O34 172.66(10) . . ? O1 Zn2 O34 93.72(10) 3_556 . ? O12 Zn2 O29 92.46(9) 1_545 . ? O39 Zn2 O29 90.80(9) . . ? O28 Zn2 O29 88.38(9) . . ? O1 Zn2 O29 178.03(9) 3_556 . ? O34 Zn2 O29 84.46(10) . . ? C2 O1 Zn2 128.13(19) . 3_456 ? O1 C2 O3 125.6(3) . . ? O1 C2 C4 118.2(3) . . ? O3 C2 C4 116.2(3) . . ? C2 O3 Zn1 126.47(19) . 3_456 ? C5 C4 C9 119.2(3) . . ? C5 C4 C2 119.7(3) . . ? C9 C4 C2 121.1(3) . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? O13 C6 C5 114.5(3) . . ? O13 C6 C7 124.6(3) . . ? C5 C6 C7 120.9(3) . . ? C8 C7 C6 118.2(3) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? C9 C8 C7 120.7(3) . . ? C9 C8 C10 118.8(3) . . ? C7 C8 C10 120.4(3) . . ? C8 C9 C4 120.5(3) . . ? C8 C9 H9 119.7 . . ? C4 C9 H9 119.7 . . ? O12 C10 O11 125.6(3) . . ? O12 C10 C8 115.0(2) . . ? O11 C10 C8 119.3(2) . . ? C10 O11 Zn1 119.19(18) . 1_565 ? C10 O12 Zn2 141.60(18) . 1_565 ? C6 O13 C14 117.2(2) . . ? O13 C14 C15 106.5(2) . . ? O13 C14 H14A 110.4 . . ? C15 C14 H14A 110.4 . . ? O13 C14 H14B 110.4 . . ? C15 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? O16 C15 C14 112.7(2) . . ? O16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? O16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C17 O16 C15 117.9(2) . . ? O16 C17 C22 126.2(3) . . ? O16 C17 C18 113.9(3) . . ? C22 C17 C18 119.9(3) . . ? C19 C18 C17 120.3(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.0(3) . . ? C18 C19 C26 117.3(3) . . ? C20 C19 C26 122.7(3) . . ? C19 C20 C21 119.4(3) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 120.3(3) . . ? C22 C21 C23 117.9(3) . . ? C20 C21 C23 121.8(3) . . ? C21 C22 C17 120.0(3) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? O25 C23 O24 123.8(3) . . ? O25 C23 C21 118.9(3) . . ? O24 C23 C21 117.3(3) . . ? C23 O24 Zn1 109.90(18) . 4_655 ? O28 C26 O27 124.0(3) . . ? O28 C26 C19 118.2(3) . . ? O27 C26 C19 117.7(3) . . ? C26 O27 Zn1 116.14(18) . . ? C26 O28 Zn2 136.3(2) . . ? C30 O29 Zn2 119.5(2) . . ? O29 C30 N31 125.7(3) . . ? O29 C30 H30 117.2 . . ? N31 C30 H30 117.2 . . ? C30 N31 C33 121.0(3) . . ? C30 N31 C32 120.5(3) . . ? C33 N31 C32 118.4(3) . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N31 C33 H33A 109.5 . . ? N31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 O34 Zn2 127.2(2) . . ? O34 C35 N36 124.2(3) . . ? O34 C35 H35 117.9 . . ? N36 C35 H35 117.9 . . ? C35 N36 C37 121.5(3) . . ? C35 N36 C38 121.3(3) . . ? C37 N36 C38 117.2(3) . . ? N36 C37 H37A 109.5 . . ? N36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N36 C38 H38A 109.5 . . ? N36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 O39 Zn2 122.8(2) . . ? O39 C40 N41 123.3(3) . . ? O39 C40 H40 118.4 . . ? N41 C40 H40 118.4 . . ? C40 N41 C43 120.4(3) . . ? C40 N41 C42 121.1(3) . . ? C43 N41 C42 118.4(3) . . ? N41 C42 H42A 109.5 . . ? N41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N41 C43 H43A 109.5 . . ? N41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O44 C45 N46 125.0(4) . . ? O44 C45 H45 117.5 . . ? N46 C45 H45 117.5 . . ? C45 N46 C47 121.8(4) . . ? C45 N46 C48 121.8(4) . . ? C47 N46 C48 116.3(4) . . ? N46 C47 H47A 109.5 . . ? N46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N46 C48 H48A 109.5 . . ? N46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? # start Validation Reply Form _vrf_PLAT220_7 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.45 Ratio RESPONSE: Atoms of the metal-coordinated as well as the non-coordinated DMF molecules reveal relatively large-amplitudes ADP's. ; _vrf_PLAT222_7 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.82 Ratio RESPONSE: Atoms of the metal-coordinated as well as the non-coordinated DMF molecules reveal relatively large-amplitudes ADP's. ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.648 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.086 #==============================END====================================== # Attachment '- Paper2-CIF_b.txt' data_8 _database_code_depnum_ccdc_archive 'CCDC 779789' #TrackingRef '- Paper2-CIF_b.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Ni2 O12' _chemical_formula_sum 'C18 H12 Ni2 O12' _chemical_formula_weight 537.70 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' Ni Ni 0.3393 1.1124 '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' _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 10.0777(2) _cell_length_b 11.0012(2) _cell_length_c 15.0573(3) _cell_angle_alpha 72.9490(12) _cell_angle_beta 77.0468(11) _cell_angle_gamma 81.3705(10) _cell_volume 1548.98(5) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5375 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 27.85 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 1.258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6672 _exptl_absorpt_correction_T_max 0.7870 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16652 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.85 _reflns_number_total 7277 _reflns_number_gt 5054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Uncoordinated molecules of the water solvent incorporated into the coordination polymeric grid was found severely disordered and could not be modeled by discrete. Thie contribution to the diffraction pattern was Squeezed by the PLATON software (Spek, 2003). The number of residual electrons within these voids was assessed to be 199, which corresponds to about 20 water molecules. ; _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^)+(0.0577P)^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 7277 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.50391(3) -0.35831(3) 0.49232(2) 0.02207(9) Uani 1 1 d . . . Ni2 Ni 0.36319(3) -0.40881(3) 0.32499(2) 0.02137(9) Uani 1 1 d . . . O1 O 0.33188(19) -0.21843(14) 0.31620(12) 0.0304(4) Uani 1 1 d . . . O2 O 0.40344(19) -0.18693(15) 0.43859(12) 0.0310(4) Uani 1 1 d . . . C3 C 0.3471(2) -0.1508(2) 0.36751(17) 0.0252(5) Uani 1 1 d . . . C4 C 0.2924(2) -0.0129(2) 0.34145(16) 0.0223(5) Uani 1 1 d . . . C5 C 0.3383(2) 0.0751(2) 0.37525(16) 0.0234(5) Uani 1 1 d . . . H5 H 0.4009 0.0473 0.4174 0.028 Uiso 1 1 calc R . . C6 C 0.2925(2) 0.2035(2) 0.34739(17) 0.0230(5) Uani 1 1 d . . . C7 C 0.3515(2) 0.2993(2) 0.37661(18) 0.0258(5) Uani 1 1 d . . . O8 O 0.37719(17) 0.26515(15) 0.45973(12) 0.0269(4) Uani 1 1 d . . . O9 O 0.3732(2) 0.40387(15) 0.31654(12) 0.0327(4) Uani 1 1 d . . . C10 C 0.1943(3) 0.2445(2) 0.28884(17) 0.0257(5) Uani 1 1 d . . . H10 H 0.1621 0.3322 0.2702 0.031 Uiso 1 1 calc R . . C11 C 0.1451(2) 0.1549(2) 0.25873(16) 0.0244(5) Uani 1 1 d . . . C12 C 0.1952(3) 0.0287(2) 0.28324(17) 0.0255(5) Uani 1 1 d . . . H12 H 0.1633 -0.0310 0.2603 0.031 Uiso 1 1 calc R . . O13 O 0.04759(19) 0.18151(15) 0.20364(13) 0.0345(5) Uani 1 1 d . . . C14 C -0.0210(3) 0.3080(2) 0.17930(17) 0.0271(6) Uani 1 1 d . . . H14A H 0.0402 0.3728 0.1749 0.033 Uiso 1 1 calc R . . H14B H -0.1039 0.3166 0.2276 0.033 Uiso 1 1 calc R . . C15 C -0.0588(2) 0.3251(2) 0.08491(17) 0.0261(5) Uani 1 1 d . . . H15A H -0.1058 0.2517 0.0860 0.031 Uiso 1 1 calc R . . H15B H -0.1201 0.4041 0.0685 0.031 Uiso 1 1 calc R . . O16 O 0.06554(19) 0.3328(2) 0.01902(13) 0.0379(5) Uani 1 1 d . . . C17 C 0.0653(3) 0.3437(2) -0.07425(17) 0.0285(6) Uani 1 1 d . . . C18 C 0.1929(3) 0.3486(2) -0.13217(18) 0.0287(6) Uani 1 1 d . . . H18 H 0.2717 0.3441 -0.1062 0.034 Uiso 1 1 calc R . . C19 C 0.2069(3) 0.3601(2) -0.22872(17) 0.0261(5) Uani 1 1 d . . . C20 C 0.3443(3) 0.3634(2) -0.29169(17) 0.0268(5) Uani 1 1 d . . . O21 O 0.35319(17) 0.33552(16) -0.36837(12) 0.0289(4) Uani 1 1 d . . . O22 O 0.43953(17) 0.39591(16) -0.26364(12) 0.0286(4) Uani 1 1 d . . . C23 C 0.0889(3) 0.3694(2) -0.26584(18) 0.0285(6) Uani 1 1 d . . . H23 H 0.0968 0.3784 -0.3315 0.034 Uiso 1 1 calc R . . C24 C -0.0380(2) 0.3655(2) -0.20816(16) 0.0233(5) Uani 1 1 d . . . C25 C -0.1628(3) 0.3780(2) -0.24983(18) 0.0255(6) Uani 1 1 d . . . O26 O -0.14896(18) 0.40866(16) -0.33997(12) 0.0303(4) Uani 1 1 d . . . O27 O -0.27902(17) 0.36109(15) -0.19753(12) 0.0265(4) Uani 1 1 d . . . C28 C -0.0527(3) 0.3526(2) -0.11064(17) 0.0265(5) Uani 1 1 d . . . H28 H -0.1404 0.3499 -0.0707 0.032 Uiso 1 1 calc R . . O29 O 0.38875(16) -0.46819(14) 0.45857(11) 0.0230(4) Uani 1 1 d . . . O30 O 0.35506(19) -0.35974(17) 0.61726(13) 0.0371(5) Uani 1 1 d . . . H30A H 0.3869 -0.4102 0.6678 0.056 Uiso 1 1 d R . . H30B H 0.3592 -0.3966 0.5710 0.056 Uiso 1 1 d 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 Ni1 0.03082(18) 0.01654(16) 0.02447(17) -0.00554(12) -0.01927(14) 0.00182(12) Ni2 0.02833(18) 0.01655(16) 0.02469(17) -0.00403(12) -0.01916(14) -0.00053(12) O1 0.0505(11) 0.0152(8) 0.0337(9) -0.0051(7) -0.0291(9) 0.0006(8) O2 0.0481(11) 0.0194(8) 0.0343(10) -0.0074(7) -0.0314(9) 0.0059(8) C3 0.0300(13) 0.0202(12) 0.0301(13) -0.0036(10) -0.0193(12) -0.0028(10) C4 0.0297(13) 0.0173(11) 0.0235(12) -0.0038(9) -0.0145(11) -0.0019(9) C5 0.0301(13) 0.0213(12) 0.0234(12) -0.0040(9) -0.0180(11) -0.0010(10) C6 0.0291(13) 0.0175(11) 0.0272(12) -0.0065(9) -0.0168(11) 0.0012(10) C7 0.0301(13) 0.0146(11) 0.0367(14) -0.0058(10) -0.0203(12) 0.0043(10) O8 0.0392(10) 0.0223(8) 0.0276(9) -0.0070(7) -0.0254(8) 0.0010(7) O9 0.0566(12) 0.0162(9) 0.0338(10) -0.0051(7) -0.0291(9) -0.0024(8) C10 0.0356(14) 0.0190(12) 0.0270(12) -0.0045(10) -0.0213(12) 0.0031(10) C11 0.0317(13) 0.0239(12) 0.0230(12) -0.0032(9) -0.0209(11) -0.0016(10) C12 0.0358(14) 0.0196(12) 0.0274(13) -0.0058(10) -0.0186(12) -0.0036(10) O13 0.0484(12) 0.0201(9) 0.0454(11) -0.0057(8) -0.0386(10) 0.0036(8) C14 0.0333(14) 0.0262(13) 0.0249(12) -0.0060(10) -0.0188(12) 0.0062(10) C15 0.0273(13) 0.0255(13) 0.0280(13) -0.0040(10) -0.0172(11) 0.0014(10) O16 0.0297(10) 0.0654(13) 0.0235(9) -0.0115(9) -0.0144(8) -0.0059(9) C17 0.0339(14) 0.0317(14) 0.0239(12) -0.0056(10) -0.0175(12) -0.0008(11) C18 0.0297(14) 0.0323(14) 0.0292(13) -0.0057(11) -0.0203(12) -0.0008(11) C19 0.0298(13) 0.0234(12) 0.0280(13) -0.0060(10) -0.0141(11) 0.0000(10) C20 0.0325(14) 0.0228(12) 0.0282(13) -0.0037(10) -0.0187(12) 0.0016(10) O21 0.0342(10) 0.0308(9) 0.0269(9) -0.0082(7) -0.0147(8) -0.0045(8) O22 0.0305(10) 0.0318(9) 0.0284(9) -0.0078(7) -0.0146(8) -0.0054(7) C23 0.0351(15) 0.0279(13) 0.0271(13) -0.0068(10) -0.0177(12) -0.0006(11) C24 0.0300(13) 0.0202(12) 0.0239(12) -0.0038(9) -0.0179(11) -0.0006(10) C25 0.0331(15) 0.0190(12) 0.0321(13) -0.0069(10) -0.0239(13) 0.0003(10) O26 0.0364(10) 0.0345(10) 0.0253(9) -0.0044(7) -0.0215(8) -0.0037(8) O27 0.0300(10) 0.0276(9) 0.0259(9) -0.0030(7) -0.0186(8) -0.0034(7) C28 0.0291(13) 0.0262(13) 0.0265(13) -0.0050(10) -0.0142(11) 0.0000(10) O29 0.0336(9) 0.0150(8) 0.0256(8) -0.0037(6) -0.0212(8) 0.0021(7) O30 0.0486(12) 0.0360(11) 0.0320(10) -0.0128(8) -0.0211(10) 0.0076(9) _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 Ni1 O29 2.0279(14) . ? Ni1 O2 2.0333(15) . ? Ni1 O8 2.0488(15) 2_656 ? Ni1 O21 2.0613(18) 2_655 ? Ni1 O29 2.0668(14) 2_646 ? Ni1 O30 2.1246(19) . ? Ni1 H30B 1.6806 . ? Ni2 O29 1.9874(14) . ? Ni2 O22 2.0027(18) 2_655 ? Ni2 O1 2.0400(15) . ? Ni2 O9 2.0877(15) 1_545 ? Ni2 O26 2.1196(17) 2 ? Ni2 O27 2.1640(14) 2 ? Ni2 C25 2.464(2) 2 ? O1 C3 1.264(3) . ? O2 C3 1.257(3) . ? C3 C4 1.503(3) . ? C4 C5 1.392(3) . ? C4 C12 1.397(3) . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 C10 1.409(3) . ? C6 C7 1.495(3) . ? C7 O9 1.252(3) . ? C7 O8 1.271(3) . ? O8 Ni1 2.0488(15) 2_656 ? O9 Ni2 2.0877(15) 1_565 ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 O13 1.369(2) . ? C11 C12 1.375(3) . ? C12 H12 0.9500 . ? O13 C14 1.441(3) . ? C14 C15 1.505(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O16 1.409(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C17 1.374(3) . ? C17 C18 1.381(4) . ? C17 C28 1.396(3) . ? C18 C19 1.398(3) . ? C18 H18 0.9500 . ? C19 C23 1.401(3) . ? C19 C20 1.491(4) . ? C20 O21 1.260(3) . ? C20 O22 1.265(3) . ? O21 Ni1 2.0613(18) 2_655 ? O22 Ni2 2.0026(18) 2_655 ? C23 C24 1.375(4) . ? C23 H23 0.9500 . ? C24 C28 1.409(3) . ? C24 C25 1.498(3) . ? C25 O27 1.262(3) . ? C25 O26 1.279(3) . ? C25 Ni2 2.464(2) 2 ? O26 Ni2 2.1197(17) 2 ? O27 Ni2 2.1641(14) 2 ? C28 H28 0.9500 . ? O29 Ni1 2.0668(14) 2_646 ? O30 H30A 0.8934 . ? O30 H30B 0.8936 . ? 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 O29 Ni1 O2 97.05(6) . . ? O29 Ni1 O8 173.17(6) . 2_656 ? O2 Ni1 O8 88.72(6) . 2_656 ? O29 Ni1 O21 95.29(7) . 2_655 ? O2 Ni1 O21 90.48(7) . 2_655 ? O8 Ni1 O21 88.30(7) 2_656 2_655 ? O29 Ni1 O29 82.89(6) . 2_646 ? O2 Ni1 O29 177.60(7) . 2_646 ? O8 Ni1 O29 91.50(6) 2_656 2_646 ? O21 Ni1 O29 87.14(7) 2_655 2_646 ? O29 Ni1 O30 88.73(7) . . ? O2 Ni1 O30 84.24(7) . . ? O8 Ni1 O30 88.22(7) 2_656 . ? O21 Ni1 O30 173.73(7) 2_655 . ? O29 Ni1 O30 98.16(7) 2_646 . ? O29 Ni1 H30B 65.0 . . ? O2 Ni1 H30B 87.9 . . ? O8 Ni1 H30B 111.7 2_656 . ? O21 Ni1 H30B 159.9 2_655 . ? O29 Ni1 H30B 94.2 2_646 . ? O30 Ni1 H30B 23.7 . . ? O29 Ni2 O22 97.57(7) . 2_655 ? O29 Ni2 O1 96.98(6) . . ? O22 Ni2 O1 92.19(7) 2_655 . ? O29 Ni2 O9 91.74(6) . 1_545 ? O22 Ni2 O9 91.54(7) 2_655 1_545 ? O1 Ni2 O9 169.97(6) . 1_545 ? O29 Ni2 O26 102.26(7) . 2 ? O22 Ni2 O26 160.02(6) 2_655 2 ? O1 Ni2 O26 87.84(7) . 2 ? O9 Ni2 O26 85.49(7) 1_545 2 ? O29 Ni2 O27 163.98(7) . 2 ? O22 Ni2 O27 97.99(7) 2_655 2 ? O1 Ni2 O27 86.21(6) . 2 ? O9 Ni2 O27 84.06(6) 1_545 2 ? O26 Ni2 O27 62.07(6) 2 2 ? O29 Ni2 C25 133.43(8) . 2 ? O22 Ni2 C25 128.76(8) 2_655 2 ? O1 Ni2 C25 86.82(7) . 2 ? O9 Ni2 C25 83.59(7) 1_545 2 ? O26 Ni2 C25 31.28(8) 2 2 ? O27 Ni2 C25 30.79(8) 2 2 ? C3 O1 Ni2 134.47(14) . . ? C3 O2 Ni1 129.57(15) . . ? O2 C3 O1 126.8(2) . . ? O2 C3 C4 116.18(19) . . ? O1 C3 C4 117.04(18) . . ? C5 C4 C12 119.2(2) . . ? C5 C4 C3 120.17(18) . . ? C12 C4 C3 120.62(19) . . ? C6 C5 C4 120.04(19) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C10 120.3(2) . . ? C5 C6 C7 119.90(18) . . ? C10 C6 C7 119.76(19) . . ? O9 C7 O8 126.4(2) . . ? O9 C7 C6 117.09(19) . . ? O8 C7 C6 116.5(2) . . ? C7 O8 Ni1 124.55(16) . 2_656 ? C7 O9 Ni2 133.77(16) . 1_565 ? C11 C10 C6 119.1(2) . . ? C11 C10 H10 120.5 . . ? C6 C10 H10 120.5 . . ? O13 C11 C12 114.73(19) . . ? O13 C11 C10 125.0(2) . . ? C12 C11 C10 120.31(19) . . ? C11 C12 C4 121.0(2) . . ? C11 C12 H12 119.5 . . ? C4 C12 H12 119.5 . . ? C11 O13 C14 120.28(17) . . ? O13 C14 C15 106.01(18) . . ? O13 C14 H14A 110.5 . . ? C15 C14 H14A 110.5 . . ? O13 C14 H14B 110.5 . . ? C15 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? O16 C15 C14 105.75(18) . . ? O16 C15 H15A 110.6 . . ? C14 C15 H15A 110.6 . . ? O16 C15 H15B 110.6 . . ? C14 C15 H15B 110.6 . . ? H15A C15 H15B 108.7 . . ? C17 O16 C15 119.67(18) . . ? O16 C17 C18 114.72(19) . . ? O16 C17 C28 124.2(2) . . ? C18 C17 C28 121.1(2) . . ? C17 C18 C19 120.5(2) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C23 118.8(2) . . ? C18 C19 C20 121.0(2) . . ? C23 C19 C20 120.3(2) . . ? O21 C20 O22 126.5(2) . . ? O21 C20 C19 116.6(2) . . ? O22 C20 C19 116.9(2) . . ? C20 O21 Ni1 134.39(16) . 2_655 ? C20 O22 Ni2 129.34(16) . 2_655 ? C24 C23 C19 120.6(2) . . ? C24 C23 H23 119.7 . . ? C19 C23 H23 119.7 . . ? C23 C24 C28 120.9(2) . . ? C23 C24 C25 119.6(2) . . ? C28 C24 C25 119.5(2) . . ? O27 C25 O26 120.72(19) . . ? O27 C25 C24 121.0(2) . . ? O26 C25 C24 118.3(2) . . ? O27 C25 Ni2 61.38(10) . 2 ? O26 C25 Ni2 59.35(11) . 2 ? C24 C25 Ni2 176.87(19) . 2 ? C25 O26 Ni2 89.37(15) . 2 ? C25 O27 Ni2 87.83(12) . 2 ? C17 C28 C24 118.2(2) . . ? C17 C28 H28 120.9 . . ? C24 C28 H28 120.9 . . ? Ni2 O29 Ni1 113.90(8) . . ? Ni2 O29 Ni1 120.68(8) . 2_646 ? Ni1 O29 Ni1 97.11(6) . 2_646 ? Ni1 O30 H30A 110.1 . . ? Ni1 O30 H30B 49.1 . . ? H30A O30 H30B 114.8 . . ? 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 O30 H30A O22 0.89 2.12 2.887(2) 143 1_546 O30 H30B O29 0.89 2.02 2.904(2) 173 . # 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 -0.023 0.001 0.006 782 199 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.639 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.077 #=================================END================================== data_9 _database_code_depnum_ccdc_archive 'CCDC 779790' #TrackingRef '- Paper2-CIF_b.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H26 Ag4 O21, H2 O' _chemical_formula_sum 'C36 H28 Ag4 O22' _chemical_formula_weight 1244.06 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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4803(2) _cell_length_b 17.8109(2) _cell_length_c 13.2541(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.7111(6) _cell_angle_gamma 90.00 _cell_volume 3534.60(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8179 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.87 _exptl_crystal_description rods _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 2.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5019 _exptl_absorpt_correction_T_max 0.8038 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32567 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.87 _reflns_number_total 8351 _reflns_number_gt 6330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^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 8351 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.003 _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 0.587101(18) 0.482769(16) 0.49146(2) 0.01947(8) Uani 1 1 d . . . Ag2 Ag 0.656526(18) 0.558578(17) 0.72256(2) 0.02139(8) Uani 1 1 d . . . Ag3 Ag 0.163913(19) 0.085962(16) 0.78317(2) 0.02171(9) Uani 1 1 d . . . Ag4 Ag 0.094015(19) 0.013007(16) 0.54567(2) 0.02088(9) Uani 1 1 d . . . O1 O 0.53465(17) 0.36944(15) 0.4972(2) 0.0223(6) Uani 1 1 d . . . O2 O 0.39261(17) 0.39524(15) 0.49555(19) 0.0183(5) Uani 1 1 d . . . C3 C 0.4571(2) 0.3504(2) 0.4976(3) 0.0160(7) Uani 1 1 d . . . C4 C 0.4391(2) 0.2678(2) 0.5003(2) 0.0154(7) Uani 1 1 d . . . C5 C 0.3570(2) 0.2416(2) 0.5108(2) 0.0161(7) Uani 1 1 d . . . H5 H 0.3111 0.2758 0.5155 0.019 Uiso 1 1 calc R . . C6 C 0.3432(2) 0.1645(2) 0.5142(3) 0.0156(7) Uani 1 1 d . . . C7 C 0.2554(2) 0.1355(2) 0.5252(3) 0.0165(7) Uani 1 1 d . . . O8 O 0.19473(17) 0.18862(15) 0.5175(2) 0.0219(6) Uani 1 1 d . . . H8 H 0.1450 0.1690 0.5159 0.033 Uiso 1 1 calc R . . O9 O 0.24138(17) 0.06909(16) 0.5396(2) 0.0239(6) Uani 1 1 d . . . C10 C 0.4086(2) 0.1137(2) 0.5056(2) 0.0158(7) Uani 1 1 d . . . H10 H 0.3984 0.0613 0.5089 0.019 Uiso 1 1 calc R . . C11 C 0.4897(2) 0.1402(2) 0.4921(2) 0.0152(7) Uani 1 1 d . . . C12 C 0.5056(2) 0.2174(2) 0.4916(2) 0.0154(7) Uani 1 1 d . . . H12 H 0.5618 0.2355 0.4852 0.018 Uiso 1 1 calc R . . O13 O 0.54722(16) 0.08494(14) 0.47694(19) 0.0189(5) Uani 1 1 d . . . C14 C 0.6358(2) 0.1046(2) 0.4699(3) 0.0171(7) Uani 1 1 d . . . H14A H 0.6346 0.1553 0.4390 0.021 Uiso 1 1 calc R . . H14B H 0.6553 0.0687 0.4231 0.021 Uiso 1 1 calc R . . C15 C 0.7016(2) 0.1037(2) 0.5747(3) 0.0179(7) Uani 1 1 d . . . H15A H 0.6985 0.0548 0.6092 0.021 Uiso 1 1 calc R . . H15B H 0.7629 0.1098 0.5660 0.021 Uiso 1 1 calc R . . O16 O 0.68209(16) 0.16392(15) 0.63923(19) 0.0195(5) Uani 1 1 d . . . C17 C 0.7521(2) 0.2109(2) 0.6833(2) 0.0151(7) Uani 1 1 d . . . C18 C 0.7315(2) 0.2864(2) 0.6903(2) 0.0156(7) Uani 1 1 d . . . H18 H 0.6713 0.3030 0.6680 0.019 Uiso 1 1 calc R . . C19 C 0.8002(2) 0.3381(2) 0.7306(3) 0.0159(7) Uani 1 1 d . . . C20 C 0.7817(2) 0.4200(2) 0.7344(3) 0.0145(7) Uani 1 1 d . . . O21 O 0.70013(16) 0.44067(15) 0.7143(2) 0.0186(5) Uani 1 1 d . . . O22 O 0.84678(16) 0.46465(15) 0.75580(19) 0.0180(5) Uani 1 1 d . . . C23 C 0.8889(2) 0.3125(2) 0.7616(2) 0.0153(7) Uani 1 1 d . . . H23 H 0.9362 0.3472 0.7863 0.018 Uiso 1 1 calc R . . C24 C 0.9072(2) 0.2373(2) 0.7562(2) 0.0145(7) Uani 1 1 d . . . C25 C 1.0007(2) 0.2075(2) 0.7831(2) 0.0155(7) Uani 1 1 d . . . O26 O 1.01781(17) 0.14180(15) 0.7750(2) 0.0219(6) Uani 1 1 d . . . O27 O 1.06237(16) 0.26053(15) 0.8132(2) 0.0203(6) Uani 1 1 d . . . H27 H 1.1124 0.2437 0.8103 0.030 Uiso 1 1 calc R . . C28 C 0.8389(2) 0.1858(2) 0.7190(2) 0.0156(7) Uani 1 1 d . . . H28 H 0.8519 0.1337 0.7182 0.019 Uiso 1 1 calc R . . O29 O 0.21071(16) 0.20521(15) 0.77526(19) 0.0187(5) Uani 1 1 d . . . O30 O 0.34741(16) 0.17965(15) 0.75554(18) 0.0174(5) Uani 1 1 d . . . C31 C 0.2859(2) 0.2245(2) 0.7628(2) 0.0157(7) Uani 1 1 d . . . C32 C 0.3029(2) 0.3069(2) 0.7535(3) 0.0156(7) Uani 1 1 d . . . C33 C 0.3871(2) 0.3312(2) 0.7474(2) 0.0144(7) Uani 1 1 d . . . H33 H 0.4332 0.2959 0.7478 0.017 Uiso 1 1 calc R . . C34 C 0.4028(2) 0.4077(2) 0.7406(3) 0.0157(7) Uani 1 1 d . . . C35 C 0.4929(2) 0.4347(2) 0.7339(3) 0.0164(7) Uani 1 1 d . . . O36 O 0.51048(17) 0.50105(16) 0.7257(2) 0.0230(6) Uani 1 1 d . . . O37 O 0.55028(17) 0.37968(15) 0.73421(19) 0.0192(5) Uani 1 1 d . . . H37 H 0.5992 0.3978 0.7296 0.029 Uiso 1 1 calc R . . C38 C 0.3368(2) 0.4600(2) 0.7402(3) 0.0170(7) Uani 1 1 d . . . H38 H 0.3488 0.5121 0.7364 0.020 Uiso 1 1 calc R . . C39 C 0.2522(2) 0.4356(2) 0.7454(3) 0.0158(7) Uani 1 1 d . . . C40 C 0.2349(2) 0.3593(2) 0.7511(3) 0.0153(7) Uani 1 1 d . . . H40 H 0.1770 0.3427 0.7533 0.018 Uiso 1 1 calc R . . O41 O 0.19079(16) 0.49212(15) 0.7430(2) 0.0184(5) Uani 1 1 d . . . C42 C 0.1050(2) 0.4748(2) 0.7600(3) 0.0179(8) Uani 1 1 d . . . H42A H 0.0891 0.5134 0.8060 0.021 Uiso 1 1 calc R . . H42B H 0.1079 0.4256 0.7956 0.021 Uiso 1 1 calc R . . C43 C 0.0343(2) 0.4722(2) 0.6586(3) 0.0191(8) Uani 1 1 d . . . H43A H -0.0251 0.4649 0.6722 0.023 Uiso 1 1 calc R . . H43B H 0.0335 0.5201 0.6205 0.023 Uiso 1 1 calc R . . O44 O 0.05388(16) 0.41042(15) 0.5965(2) 0.0216(6) Uani 1 1 d . . . C45 C -0.0148(2) 0.3603(2) 0.5570(3) 0.0161(7) Uani 1 1 d . . . C46 C 0.0086(2) 0.2853(2) 0.5544(2) 0.0157(7) Uani 1 1 d . . . H46 H 0.0694 0.2706 0.5773 0.019 Uiso 1 1 calc R . . C47 C -0.0576(2) 0.2314(2) 0.5181(2) 0.0155(7) Uani 1 1 d . . . C48 C -0.0363(2) 0.1496(2) 0.5173(3) 0.0156(7) Uani 1 1 d . . . O49 O 0.04564(16) 0.13031(15) 0.53692(19) 0.0196(5) Uani 1 1 d . . . O50 O -0.10067(17) 0.10447(15) 0.4978(2) 0.0203(6) Uani 1 1 d . . . C51 C -0.1468(2) 0.2542(2) 0.4823(2) 0.0139(7) Uani 1 1 d . . . H51 H -0.1923 0.2179 0.4575 0.017 Uiso 1 1 calc R . . C52 C -0.1688(2) 0.3295(2) 0.4831(3) 0.0156(7) Uani 1 1 d . . . C53 C -0.2630(2) 0.3559(2) 0.4434(3) 0.0171(7) Uani 1 1 d . . . O54 O -0.28456(17) 0.42100(15) 0.4471(2) 0.0228(6) Uani 1 1 d . . . O55 O -0.31863(17) 0.30050(16) 0.4028(2) 0.0240(6) Uani 1 1 d . . . H55 H -0.3675 0.3186 0.3688 0.036 Uiso 1 1 calc R . . C56 C -0.1032(2) 0.3838(2) 0.5214(3) 0.0169(7) Uani 1 1 d . . . H56 H -0.1185 0.4354 0.5230 0.020 Uiso 1 1 calc R . . O57 O 0.1970(2) 0.0953(2) 0.9746(2) 0.0487(10) Uani 1 1 d . . . H57A H 0.1596 0.0701 1.0044 0.050 Uiso 1 1 d R . . H57B H 0.2548 0.0894 1.0085 0.050 Uiso 1 1 d R . . O58 O 0.53462(19) 0.3266(2) 0.2631(2) 0.0359(8) Uani 1 1 d . . . H58A H 0.4752 0.3304 0.2542 0.050 Uiso 1 1 d R . . H58B H 0.5516 0.3347 0.2040 0.050 Uiso 1 1 d 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 Ag1 0.01844(16) 0.01190(16) 0.02927(16) 0.00074(11) 0.00829(12) -0.00014(11) Ag2 0.01941(16) 0.01158(16) 0.03469(17) -0.00066(11) 0.00964(12) -0.00023(11) Ag3 0.01784(16) 0.01242(16) 0.03550(17) -0.00107(11) 0.00796(12) 0.00033(11) Ag4 0.01802(16) 0.01330(16) 0.03207(16) 0.00062(11) 0.00771(12) 0.00063(11) O1 0.0175(14) 0.0150(15) 0.0374(15) 0.0009(11) 0.0122(11) -0.0014(11) O2 0.0153(13) 0.0152(14) 0.0251(12) 0.0002(10) 0.0064(10) -0.0027(11) C3 0.0177(18) 0.0147(19) 0.0154(16) -0.0008(13) 0.0040(13) 0.0004(15) C4 0.0170(18) 0.0156(19) 0.0136(15) 0.0004(13) 0.0040(13) 0.0020(15) C5 0.0153(18) 0.018(2) 0.0150(15) -0.0006(13) 0.0043(13) 0.0015(15) C6 0.0151(18) 0.0142(19) 0.0173(16) 0.0015(13) 0.0036(13) -0.0025(14) C7 0.0176(18) 0.016(2) 0.0152(16) 0.0008(13) 0.0028(13) -0.0010(15) O8 0.0147(13) 0.0166(15) 0.0350(14) 0.0030(11) 0.0075(11) -0.0023(11) O9 0.0147(13) 0.0188(16) 0.0389(15) 0.0009(12) 0.0084(11) -0.0031(11) C10 0.0171(18) 0.016(2) 0.0142(16) 0.0005(13) 0.0033(13) 0.0003(14) C11 0.0143(17) 0.0153(19) 0.0156(16) -0.0020(13) 0.0028(13) -0.0013(14) C12 0.0150(17) 0.0146(19) 0.0160(16) -0.0007(13) 0.0031(13) -0.0033(14) O13 0.0123(12) 0.0144(14) 0.0309(13) -0.0024(11) 0.0070(10) 0.0018(10) C14 0.0129(17) 0.0152(19) 0.0243(17) -0.0011(14) 0.0068(14) -0.0015(14) C15 0.0178(18) 0.0121(19) 0.0228(17) -0.0042(14) 0.0034(14) 0.0008(15) O16 0.0136(13) 0.0175(14) 0.0271(13) -0.0075(11) 0.0046(10) -0.0016(11) C17 0.0125(17) 0.017(2) 0.0170(16) -0.0028(13) 0.0055(13) -0.0008(14) C18 0.0136(17) 0.018(2) 0.0153(15) 0.0009(13) 0.0033(13) 0.0002(14) C19 0.0188(19) 0.0135(19) 0.0170(16) 0.0022(13) 0.0076(14) 0.0006(15) C20 0.0118(17) 0.0156(19) 0.0179(16) 0.0017(13) 0.0071(13) 0.0006(14) O21 0.0136(13) 0.0138(14) 0.0304(13) -0.0013(10) 0.0092(10) 0.0015(10) O22 0.0138(13) 0.0096(13) 0.0315(13) 0.0045(10) 0.0074(10) -0.0006(10) C23 0.0128(17) 0.020(2) 0.0141(15) 0.0015(13) 0.0045(13) -0.0007(14) C24 0.0123(17) 0.0165(19) 0.0148(15) 0.0035(13) 0.0040(13) 0.0004(14) C25 0.0147(17) 0.018(2) 0.0136(15) 0.0027(13) 0.0035(13) 0.0018(15) O26 0.0162(13) 0.0164(15) 0.0325(14) -0.0008(11) 0.0053(11) 0.0037(11) O27 0.0116(13) 0.0168(15) 0.0324(13) -0.0049(11) 0.0057(11) 0.0012(11) C28 0.0139(17) 0.017(2) 0.0173(16) 0.0004(13) 0.0060(13) 0.0011(14) O29 0.0151(13) 0.0128(14) 0.0303(13) 0.0004(10) 0.0100(10) -0.0026(10) O30 0.0184(13) 0.0098(13) 0.0244(13) -0.0025(10) 0.0063(10) -0.0001(10) C31 0.0173(18) 0.0149(19) 0.0144(15) -0.0007(13) 0.0031(13) -0.0002(15) C32 0.0130(17) 0.017(2) 0.0160(16) 0.0005(13) 0.0030(13) 0.0005(14) C33 0.0136(17) 0.0151(19) 0.0149(15) -0.0003(13) 0.0046(13) 0.0008(14) C34 0.0151(18) 0.017(2) 0.0155(16) -0.0003(13) 0.0042(13) -0.0003(15) C35 0.0149(18) 0.020(2) 0.0135(15) 0.0013(13) 0.0025(13) 0.0010(15) O36 0.0162(14) 0.0186(16) 0.0348(14) 0.0046(11) 0.0078(11) -0.0006(11) O37 0.0147(13) 0.0173(14) 0.0279(13) -0.0008(11) 0.0093(11) -0.0024(11) C38 0.0197(19) 0.0116(19) 0.0195(16) 0.0009(14) 0.0046(14) -0.0015(15) C39 0.0149(18) 0.0143(19) 0.0165(15) -0.0007(13) 0.0005(13) 0.0018(14) C40 0.0130(17) 0.0155(19) 0.0181(16) -0.0003(13) 0.0056(13) -0.0012(14) O41 0.0092(12) 0.0142(14) 0.0317(13) -0.0020(11) 0.0047(10) 0.0000(10) C42 0.0116(18) 0.018(2) 0.0267(18) -0.0021(15) 0.0094(14) -0.0009(14) C43 0.0143(18) 0.018(2) 0.0253(18) -0.0013(15) 0.0057(14) 0.0012(15) O44 0.0138(13) 0.0189(15) 0.0325(14) -0.0100(11) 0.0064(11) -0.0023(11) C45 0.0147(17) 0.018(2) 0.0165(16) 0.0009(14) 0.0060(13) 0.0013(14) C46 0.0131(17) 0.017(2) 0.0169(16) -0.0010(13) 0.0036(13) 0.0008(14) C47 0.0135(17) 0.0174(19) 0.0167(16) 0.0010(14) 0.0059(13) 0.0024(14) C48 0.0146(18) 0.0158(19) 0.0176(16) -0.0011(14) 0.0062(13) 0.0003(15) O49 0.0108(13) 0.0138(14) 0.0347(14) 0.0007(11) 0.0066(10) 0.0013(10) O50 0.0145(13) 0.0137(14) 0.0323(14) -0.0016(11) 0.0054(10) -0.0008(11) C51 0.0130(17) 0.0165(19) 0.0133(15) 0.0005(13) 0.0054(13) 0.0001(14) C52 0.0164(18) 0.0152(19) 0.0165(16) -0.0003(13) 0.0062(13) -0.0003(14) C53 0.0178(19) 0.017(2) 0.0186(16) 0.0034(14) 0.0084(14) -0.0012(15) O54 0.0172(13) 0.0168(15) 0.0359(14) 0.0024(11) 0.0094(11) 0.0036(11) O55 0.0133(13) 0.0245(16) 0.0316(14) 0.0011(12) 0.0007(11) 0.0012(12) C56 0.0165(18) 0.018(2) 0.0186(16) -0.0007(14) 0.0084(14) 0.0008(15) O57 0.0308(18) 0.085(3) 0.0293(16) 0.0033(17) 0.0050(14) 0.0126(19) O58 0.0189(15) 0.059(2) 0.0287(15) 0.0056(14) 0.0033(12) -0.0019(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O1 2.184(3) . ? Ag1 O2 2.196(3) 3_666 ? Ag1 O54 2.469(2) 1_655 ? Ag1 Ag1 2.8303(5) 3_666 ? Ag1 Ag2 3.2693(4) . ? Ag2 O30 2.179(3) 2_656 ? Ag2 O21 2.217(3) . ? Ag2 O36 2.492(3) . ? Ag2 Ag3 2.8420(4) 2_656 ? Ag3 O22 2.218(3) 2_646 ? Ag3 O29 2.255(3) . ? Ag3 O26 2.448(2) 1_455 ? Ag3 O57 2.463(3) . ? Ag3 Ag2 2.8421(4) 2_646 ? Ag3 Ag4 3.3224(4) . ? Ag4 O50 2.180(3) 3_556 ? Ag4 O49 2.212(3) . ? Ag4 O9 2.510(3) . ? Ag4 Ag4 2.8919(6) 3_556 ? O1 C3 1.249(4) . ? O2 C3 1.274(4) . ? O2 Ag1 2.196(3) 3_666 ? C3 C4 1.499(5) . ? C4 C5 1.394(5) . ? C4 C12 1.392(5) . ? C5 C6 1.391(5) . ? C5 H5 0.9500 . ? C6 C10 1.384(5) . ? C6 C7 1.496(5) . ? C7 O9 1.226(5) . ? C7 O8 1.319(4) . ? O8 H8 0.8400 . ? C10 C11 1.395(5) . ? C10 H10 0.9500 . ? C11 O13 1.376(4) . ? C11 C12 1.397(5) . ? C12 H12 0.9500 . ? O13 C14 1.441(4) . ? C14 C15 1.500(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O16 1.451(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C17 1.377(4) . ? C17 C28 1.381(5) . ? C17 C18 1.390(5) . ? C18 C19 1.405(5) . ? C18 H18 0.9500 . ? C19 C23 1.406(5) . ? C19 C20 1.490(5) . ? C20 O22 1.258(4) . ? C20 O21 1.277(4) . ? O22 Ag3 2.218(3) 2_656 ? C23 C24 1.374(5) . ? C23 H23 0.9500 . ? C24 C28 1.392(5) . ? C24 C25 1.497(5) . ? C25 O26 1.210(5) . ? C25 O27 1.331(4) . ? O26 Ag3 2.448(2) 1_655 ? O27 H27 0.8400 . ? C28 H28 0.9500 . ? O29 C31 1.265(4) . ? O30 C31 1.264(4) . ? O30 Ag2 2.179(3) 2_646 ? C31 C32 1.502(5) . ? C32 C33 1.396(5) . ? C32 C40 1.401(5) . ? C33 C34 1.390(5) . ? C33 H33 0.9500 . ? C34 C38 1.382(5) . ? C34 C35 1.498(5) . ? C35 O36 1.224(5) . ? C35 O37 1.322(4) . ? O37 H37 0.8400 . ? C38 C39 1.398(5) . ? C38 H38 0.9500 . ? C39 O41 1.380(4) . ? C39 C40 1.390(5) . ? C40 H40 0.9500 . ? O41 C42 1.435(4) . ? C42 C43 1.503(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O44 1.452(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O44 C45 1.385(4) . ? C45 C46 1.386(5) . ? C45 C56 1.394(5) . ? C46 C47 1.397(5) . ? C46 H46 0.9500 . ? C47 C51 1.402(5) . ? C47 C48 1.495(5) . ? C48 O50 1.255(4) . ? C48 O49 1.275(4) . ? O50 Ag4 2.180(3) 3_556 ? C51 C52 1.385(5) . ? C51 H51 0.9500 . ? C52 C56 1.400(5) . ? C52 C53 1.496(5) . ? C53 O54 1.211(5) . ? C53 O55 1.330(4) . ? O54 Ag1 2.469(2) 1_455 ? O55 H55 0.8400 . ? C56 H56 0.9500 . ? O57 H57A 0.9001 . ? O57 H57B 0.8996 . ? O58 H58A 0.8997 . ? O58 H58B 0.8997 . ? 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 Ag1 O2 163.48(9) . 3_666 ? O1 Ag1 O54 85.71(9) . 1_655 ? O2 Ag1 O54 110.60(9) 3_666 1_655 ? O1 Ag1 Ag1 80.06(7) . 3_666 ? O2 Ag1 Ag1 84.22(7) 3_666 3_666 ? O54 Ag1 Ag1 163.00(7) 1_655 3_666 ? O1 Ag1 Ag2 112.69(7) . . ? O2 Ag1 Ag2 60.75(6) 3_666 . ? O54 Ag1 Ag2 108.31(6) 1_655 . ? Ag1 Ag1 Ag2 85.911(13) 3_666 . ? O30 Ag2 O21 164.42(9) 2_656 . ? O30 Ag2 O36 110.39(9) 2_656 . ? O21 Ag2 O36 84.28(9) . . ? O30 Ag2 Ag3 83.94(6) 2_656 2_656 ? O21 Ag2 Ag3 81.32(6) . 2_656 ? O36 Ag2 Ag3 165.60(7) . 2_656 ? O30 Ag2 Ag1 121.33(6) 2_656 . ? O21 Ag2 Ag1 66.08(7) . . ? O36 Ag2 Ag1 76.24(6) . . ? Ag3 Ag2 Ag1 97.869(11) 2_656 . ? O22 Ag3 O29 155.86(9) 2_646 . ? O22 Ag3 O26 111.84(9) 2_646 1_455 ? O29 Ag3 O26 85.38(9) . 1_455 ? O22 Ag3 O57 106.82(12) 2_646 . ? O29 Ag3 O57 89.95(12) . . ? O26 Ag3 O57 88.06(10) 1_455 . ? O22 Ag3 Ag2 80.93(6) 2_646 2_646 ? O29 Ag3 Ag2 80.35(6) . 2_646 ? O26 Ag3 Ag2 165.36(7) 1_455 2_646 ? O57 Ag3 Ag2 95.17(7) . 2_646 ? O22 Ag3 Ag4 53.93(6) 2_646 . ? O29 Ag3 Ag4 110.82(6) . . ? O26 Ag3 Ag4 92.42(6) 1_455 . ? O57 Ag3 Ag4 159.20(10) . . ? Ag2 Ag3 Ag4 89.599(11) 2_646 . ? O50 Ag4 O49 158.55(10) 3_556 . ? O50 Ag4 O9 105.62(9) 3_556 . ? O49 Ag4 O9 85.46(9) . . ? O50 Ag4 Ag4 81.12(7) 3_556 3_556 ? O49 Ag4 Ag4 80.68(6) . 3_556 ? O9 Ag4 Ag4 151.25(6) . 3_556 ? O50 Ag4 Ag3 126.87(7) 3_556 . ? O49 Ag4 Ag3 72.83(7) . . ? O9 Ag4 Ag3 78.15(6) . . ? Ag4 Ag4 Ag3 120.683(14) 3_556 . ? C3 O1 Ag1 128.2(2) . . ? C3 O2 Ag1 121.6(2) . 3_666 ? O1 C3 O2 125.3(3) . . ? O1 C3 C4 116.9(3) . . ? O2 C3 C4 117.8(3) . . ? C5 C4 C12 120.4(3) . . ? C5 C4 C3 120.7(3) . . ? C12 C4 C3 118.9(3) . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C10 C6 C5 121.4(3) . . ? C10 C6 C7 118.9(3) . . ? C5 C6 C7 119.7(3) . . ? O9 C7 O8 123.6(3) . . ? O9 C7 C6 123.4(3) . . ? O8 C7 C6 113.0(3) . . ? C7 O8 H8 109.5 . . ? C7 O9 Ag4 126.0(2) . . ? C6 C10 C11 119.4(3) . . ? C6 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? O13 C11 C10 114.4(3) . . ? O13 C11 C12 125.6(3) . . ? C10 C11 C12 120.0(3) . . ? C4 C12 C11 119.9(3) . . ? C4 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C11 O13 C14 119.8(3) . . ? O13 C14 C15 111.8(3) . . ? O13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? O13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? O16 C15 C14 110.1(3) . . ? O16 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? O16 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.2 . . ? C17 O16 C15 116.2(3) . . ? C28 C17 O16 122.8(3) . . ? C28 C17 C18 120.7(3) . . ? O16 C17 C18 116.6(3) . . ? C17 C18 C19 119.6(3) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C23 C19 C18 119.2(3) . . ? C23 C19 C20 119.2(3) . . ? C18 C19 C20 121.4(3) . . ? O22 C20 O21 123.8(3) . . ? O22 C20 C19 118.5(3) . . ? O21 C20 C19 117.6(3) . . ? C20 O21 Ag2 124.1(2) . . ? C20 O22 Ag3 123.8(2) . 2_656 ? C24 C23 C19 119.9(3) . . ? C24 C23 H23 120.0 . . ? C19 C23 H23 120.0 . . ? C23 C24 C28 120.9(3) . . ? C23 C24 C25 122.2(3) . . ? C28 C24 C25 116.9(3) . . ? O26 C25 O27 123.8(3) . . ? O26 C25 C24 122.8(3) . . ? O27 C25 C24 113.4(3) . . ? C25 O26 Ag3 127.6(2) . 1_655 ? C25 O27 H27 109.5 . . ? C17 C28 C24 119.6(3) . . ? C17 C28 H28 120.2 . . ? C24 C28 H28 120.2 . . ? C31 O29 Ag3 125.4(2) . . ? C31 O30 Ag2 124.6(2) . 2_646 ? O30 C31 O29 125.0(3) . . ? O30 C31 C32 117.4(3) . . ? O29 C31 C32 117.5(3) . . ? C33 C32 C40 120.0(3) . . ? C33 C32 C31 119.6(3) . . ? C40 C32 C31 120.4(3) . . ? C34 C33 C32 119.3(3) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C38 C34 C33 121.3(3) . . ? C38 C34 C35 118.8(3) . . ? C33 C34 C35 119.9(3) . . ? O36 C35 O37 123.5(3) . . ? O36 C35 C34 123.1(3) . . ? O37 C35 C34 113.4(3) . . ? C35 O36 Ag2 128.4(2) . . ? C35 O37 H37 109.5 . . ? C34 C38 C39 119.4(3) . . ? C34 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? O41 C39 C40 125.0(3) . . ? O41 C39 C38 114.8(3) . . ? C40 C39 C38 120.2(3) . . ? C39 C40 C32 119.8(3) . . ? C39 C40 H40 120.1 . . ? C32 C40 H40 120.1 . . ? C39 O41 C42 119.9(3) . . ? O41 C42 C43 111.0(3) . . ? O41 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? O41 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? O44 C43 C42 108.7(3) . . ? O44 C43 H43A 109.9 . . ? C42 C43 H43A 109.9 . . ? O44 C43 H43B 109.9 . . ? C42 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? C45 O44 C43 116.9(3) . . ? O44 C45 C46 116.8(3) . . ? O44 C45 C56 121.8(3) . . ? C46 C45 C56 121.4(3) . . ? C45 C46 C47 119.8(3) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C46 C47 C51 119.4(3) . . ? C46 C47 C48 121.9(3) . . ? C51 C47 C48 118.7(3) . . ? O50 C48 O49 124.5(3) . . ? O50 C48 C47 117.4(3) . . ? O49 C48 C47 118.1(3) . . ? C48 O49 Ag4 124.8(2) . . ? C48 O50 Ag4 125.5(2) . 3_556 ? C52 C51 C47 120.0(3) . . ? C52 C51 H51 120.0 . . ? C47 C51 H51 120.0 . . ? C51 C52 C56 121.0(3) . . ? C51 C52 C53 121.3(3) . . ? C56 C52 C53 117.6(3) . . ? O54 C53 O55 124.8(3) . . ? O54 C53 C52 122.7(3) . . ? O55 C53 C52 112.5(3) . . ? C53 O54 Ag1 133.1(2) . 1_455 ? C53 O55 H55 109.5 . . ? C45 C56 C52 118.3(3) . . ? C45 C56 H56 120.9 . . ? C52 C56 H56 120.9 . . ? Ag3 O57 H57A 115.5 . . ? Ag3 O57 H57B 115.3 . . ? H57A O57 H57B 113.0 . . ? H58A O58 H58B 113.0 . . ? 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 O57 H57B O2 0.90 2.20 2.975(4) 144 4_566 O57 H57A O44 0.90 2.30 3.057(4) 141 4_566 O58 H58A O30 0.90 1.99 2.876(4) 168 4_565 O58 H58B O16 0.90 2.39 3.137(4) 141 4_565 O8 H8 O49 0.84 1.77 2.603(3) 170 . O27 H27 O29 0.84 1.83 2.661(3) 168 1_655 O37 H37 O21 0.84 1.80 2.635(3) 176 . O55 H55 O58 0.84 1.79 2.583(4) 157 1_455 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.104 _refine_diff_density_min -1.730 _refine_diff_density_rms 0.167 #=====================================END========================== data_10 _database_code_depnum_ccdc_archive 'CCDC 779791' #TrackingRef '- Paper2-CIF_b.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H26 N4 O11 Zn2, C2 H6 O S, H2 O' _chemical_formula_sum 'C39 H34 N4 O13 S Zn2' _chemical_formula_weight 929.50 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.4370(2) _cell_length_b 14.6990(2) _cell_length_c 17.5061(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.3792(10) _cell_angle_gamma 90.00 _cell_volume 3989.97(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9156 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.88 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.326 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6904 _exptl_absorpt_correction_T_max 0.7763 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34714 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.88 _reflns_number_total 9442 _reflns_number_gt 5828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The polymeric lattice contains molecules of DMSO and disordered molecules of water as crystallization solvent. Three of the disordered water species could not be reliably modeled by discrete atoms. Their contribution was thus subtracted by the Squeeze procedure, using the PLATON software (Spek, 2003). ; _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^)+(0.0874P)^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 9434 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0882 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.47174(2) 0.15165(3) -0.351786(19) 0.03069(12) Uani 1 1 d . . . Zn2 Zn 0.00351(2) -0.35395(3) -0.17637(2) 0.03808(13) Uani 1 1 d . . . O1 O 0.44417(14) 0.14641(15) -0.24691(11) 0.0326(5) Uani 1 1 d . . . O2 O 0.33667(15) 0.04449(17) -0.28575(12) 0.0425(6) Uani 1 1 d . . . C3 C 0.39014(19) 0.0923(2) -0.23330(16) 0.0299(7) Uani 1 1 d . . . C4 C 0.39194(18) 0.0843(2) -0.14683(15) 0.0283(7) Uani 1 1 d . . . C5 C 0.41762(18) 0.1560(2) -0.09286(16) 0.0282(7) Uani 1 1 d . . . H5 H 0.4331 0.2127 -0.1102 0.034 Uiso 1 1 calc R . . C6 C 0.42052(19) 0.1444(2) -0.01297(17) 0.0307(7) Uani 1 1 d . . . C7 C 0.44256(19) 0.2221(2) 0.04630(16) 0.0327(7) Uani 1 1 d . . . O8 O 0.42663(14) 0.21354(17) 0.11151(12) 0.0384(5) Uani 1 1 d . . . O9 O 0.47427(14) 0.29404(16) 0.02934(12) 0.0372(5) Uani 1 1 d . . . C10 C 0.39939(19) 0.0602(2) 0.01272(17) 0.0323(7) Uani 1 1 d . . . H10 H 0.4023 0.0519 0.0674 0.039 Uiso 1 1 calc R . . C11 C 0.37435(19) -0.0107(2) -0.04179(17) 0.0321(7) Uani 1 1 d . . . C12 C 0.36898(19) 0.0014(2) -0.12178(16) 0.0306(7) Uani 1 1 d . . . H12 H 0.3496 -0.0470 -0.1595 0.037 Uiso 1 1 calc R . . O13 O 0.34966(14) -0.09633(16) -0.02320(12) 0.0397(6) Uani 1 1 d . . . C14 C 0.3724(2) -0.1191(3) 0.05914(18) 0.0415(8) Uani 1 1 d . . . H14A H 0.4335 -0.1024 0.0868 0.050 Uiso 1 1 calc R . . H14B H 0.3673 -0.1858 0.0641 0.050 Uiso 1 1 calc R . . O15 O 0.32075(14) -0.07550(17) 0.09829(12) 0.0412(6) Uani 1 1 d . . . C16 C 0.24255(19) -0.1145(2) 0.09060(16) 0.0298(7) Uani 1 1 d . . . C17 C 0.2084(2) -0.0941(2) 0.15153(16) 0.0302(7) Uani 1 1 d . . . H17 H 0.2382 -0.0533 0.1936 0.036 Uiso 1 1 calc R . . C18 C 0.13182(18) -0.1326(2) 0.15126(16) 0.0255(6) Uani 1 1 d . . . C19 C 0.0990(2) -0.1111(3) 0.21985(18) 0.0379(8) Uani 1 1 d . . . O20 O 0.03211(15) -0.15253(17) 0.22154(13) 0.0414(6) Uani 1 1 d . . . O21 O 0.1389(2) -0.0575(3) 0.27202(18) 0.0440(13) Uani 1 1 d . . . C22 C 0.08810(18) -0.1924(2) 0.08956(15) 0.0256(6) Uani 1 1 d . . . H22 H 0.0369 -0.2215 0.0907 0.031 Uiso 1 1 calc R . . C23 C 0.11969(18) -0.2094(2) 0.02608(16) 0.0259(6) Uani 1 1 d . . . C24 C 0.07068(19) -0.2687(2) -0.04378(16) 0.0293(7) Uani 1 1 d . . . O25 O 0.09004(14) -0.26422(16) -0.10789(11) 0.0371(5) Uani 1 1 d . . . O26 O 0.01092(15) -0.31900(17) -0.03897(12) 0.0397(6) Uani 1 1 d . . . C27 C 0.19749(19) -0.1709(2) 0.02688(16) 0.0302(7) Uani 1 1 d . . . H27 H 0.2196 -0.1832 -0.0158 0.036 Uiso 1 1 calc R . . N28 N 0.53098(18) 0.02279(19) -0.34727(15) 0.0368(6) Uani 1 1 d . . . C29 C 0.5502(2) -0.0276(2) -0.27947(19) 0.0422(8) Uani 1 1 d . . . H29 H 0.5176 -0.0176 -0.2445 0.051 Uiso 1 1 calc R . . C30 C 0.6138(2) -0.0925(2) -0.25744(18) 0.0403(8) Uani 1 1 d . . . H30 H 0.6245 -0.1258 -0.2086 0.048 Uiso 1 1 calc R . . C31 C 0.6622(2) -0.1087(2) -0.30771(18) 0.0360(7) Uani 1 1 d . . . C32 C 0.6396(2) -0.0606(2) -0.37993(18) 0.0394(8) Uani 1 1 d . . . H32 H 0.6690 -0.0717 -0.4175 0.047 Uiso 1 1 calc R . . C33 C 0.5752(2) 0.0026(2) -0.39704(18) 0.0397(8) Uani 1 1 d . . . H33 H 0.5609 0.0341 -0.4472 0.048 Uiso 1 1 calc R . . C34 C 0.7395(2) -0.1694(2) -0.28107(18) 0.0336(7) Uani 1 1 d . . . C35 C 0.7456(2) -0.2388(2) -0.22577(19) 0.0395(8) Uani 1 1 d . . . H35 H 0.6990 -0.2507 -0.2064 0.047 Uiso 1 1 calc R . . C36 C 0.8194(2) -0.2903(3) -0.1992(2) 0.0416(8) Uani 1 1 d . . . H36 H 0.8218 -0.3380 -0.1618 0.050 Uiso 1 1 calc R . . N37 N 0.88852(17) -0.27748(19) -0.22283(15) 0.0358(6) Uani 1 1 d . . . C38 C 0.8816(2) -0.2112(3) -0.2775(2) 0.0458(9) Uani 1 1 d . . . H38 H 0.9285 -0.2012 -0.2968 0.055 Uiso 1 1 calc R . . C39 C 0.8096(3) -0.1574(3) -0.3069(2) 0.0490(10) Uani 1 1 d . . . H39 H 0.8080 -0.1113 -0.3454 0.059 Uiso 1 1 calc R . . N40 N 0.59873(16) 0.21085(18) -0.29616(14) 0.0312(6) Uani 1 1 d . . . C41 C 0.6595(2) 0.2081(2) -0.33148(17) 0.0338(7) Uani 1 1 d . . . H41 H 0.6510 0.1689 -0.3766 0.041 Uiso 1 1 calc R . . C42 C 0.73444(19) 0.2598(2) -0.30535(17) 0.0303(7) Uani 1 1 d . . . H42 H 0.7762 0.2552 -0.3319 0.036 Uiso 1 1 calc R . . C43 C 0.74769(19) 0.3185(2) -0.23981(17) 0.0293(7) Uani 1 1 d . . . C44 C 0.6849(2) 0.3195(2) -0.20228(17) 0.0336(7) Uani 1 1 d . . . H44 H 0.6922 0.3574 -0.1565 0.040 Uiso 1 1 calc R . . C45 C 0.6121(2) 0.2656(2) -0.23156(17) 0.0333(7) Uani 1 1 d . . . H45 H 0.5701 0.2674 -0.2051 0.040 Uiso 1 1 calc R . . C46 C 0.82162(19) 0.3825(2) -0.21531(17) 0.0300(7) Uani 1 1 d . . . C47 C 0.8464(2) 0.4283(2) -0.14134(17) 0.0336(7) Uani 1 1 d . . . H47 H 0.8215 0.4124 -0.1013 0.040 Uiso 1 1 calc R . . C48 C 0.9067(2) 0.4965(2) -0.12648(17) 0.0329(7) Uani 1 1 d . . . H48 H 0.9223 0.5268 -0.0757 0.040 Uiso 1 1 calc R . . N49 N 0.94464(17) 0.52242(18) -0.17987(14) 0.0328(6) Uani 1 1 d . . . C50 C 0.9259(2) 0.4735(2) -0.24879(19) 0.0422(8) Uani 1 1 d . . . H50 H 0.9556 0.4873 -0.2856 0.051 Uiso 1 1 calc R . . C51 C 0.8663(2) 0.4050(2) -0.26814(19) 0.0420(8) Uani 1 1 d . . . H51 H 0.8552 0.3727 -0.3175 0.050 Uiso 1 1 calc R . . O52 O 0.34076(15) 0.10568(19) -0.42311(13) 0.0480(6) Uani 1 1 d . . . H52A H 0.3323 0.0799 -0.3795 0.072 Uiso 1 1 d R . . H52B H 0.3055 0.1536 -0.4419 0.072 Uiso 1 1 d R . . S53 S 0.21669(6) 0.14874(8) 0.02846(6) 0.0517(3) Uani 1 1 d . . . O54 O 0.21463(17) 0.2507(2) 0.02121(16) 0.0584(7) Uani 1 1 d . . . C55 C 0.1215(3) 0.1152(3) 0.0504(3) 0.0652(12) Uani 1 1 d . . . H55A H 0.1291 0.1288 0.1072 0.098 Uiso 1 1 calc R . . H55B H 0.1120 0.0497 0.0409 0.098 Uiso 1 1 calc R . . H55C H 0.0716 0.1487 0.0152 0.098 Uiso 1 1 calc R . . C56 C 0.1834(3) 0.1071(4) -0.0730(2) 0.0682(12) Uani 1 1 d . . . H56A H 0.2267 0.1233 -0.0980 0.102 Uiso 1 1 calc R . . H56B H 0.1279 0.1343 -0.1040 0.102 Uiso 1 1 calc R . . H56C H 0.1775 0.0407 -0.0726 0.102 Uiso 1 1 calc R . . O57 O 0.08422(18) 0.36904(19) -0.05843(15) 0.0564(7) Uani 1 1 d . . . H57A H 0.1385 0.3474 -0.0387 0.085 Uiso 1 1 d R . . H57B H 0.0515 0.3512 -0.0288 0.085 Uiso 1 1 d 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 Zn1 0.0335(2) 0.0368(2) 0.02419(18) 0.00341(14) 0.01271(15) -0.00083(16) Zn2 0.0400(2) 0.0449(3) 0.0378(2) -0.01517(17) 0.02423(18) -0.01652(18) O1 0.0342(12) 0.0420(14) 0.0243(10) -0.0012(9) 0.0135(9) -0.0071(10) O2 0.0496(14) 0.0505(15) 0.0254(11) -0.0065(10) 0.0097(10) -0.0183(12) C3 0.0294(16) 0.0381(19) 0.0251(14) -0.0007(13) 0.0128(12) -0.0015(14) C4 0.0236(15) 0.0417(19) 0.0207(13) -0.0016(12) 0.0086(11) -0.0042(13) C5 0.0237(15) 0.0353(18) 0.0269(14) -0.0020(12) 0.0101(11) -0.0011(13) C6 0.0240(15) 0.043(2) 0.0266(14) -0.0039(13) 0.0105(12) -0.0048(13) C7 0.0283(16) 0.044(2) 0.0234(14) -0.0054(13) 0.0054(12) -0.0011(14) O8 0.0410(13) 0.0510(16) 0.0270(10) -0.0088(10) 0.0163(9) -0.0060(11) O9 0.0440(13) 0.0411(14) 0.0261(10) -0.0048(9) 0.0112(9) -0.0039(11) C10 0.0299(16) 0.044(2) 0.0260(14) -0.0005(13) 0.0131(12) -0.0065(14) C11 0.0267(16) 0.042(2) 0.0313(15) 0.0038(13) 0.0144(12) -0.0036(14) C12 0.0291(16) 0.0386(19) 0.0265(14) -0.0037(13) 0.0123(12) -0.0067(14) O13 0.0433(13) 0.0448(15) 0.0356(11) 0.0020(10) 0.0190(10) -0.0106(11) C14 0.0331(18) 0.056(2) 0.0358(17) 0.0162(16) 0.0124(14) -0.0025(16) O15 0.0352(12) 0.0604(17) 0.0293(11) -0.0015(10) 0.0125(9) -0.0206(11) C16 0.0288(16) 0.0367(18) 0.0237(14) 0.0056(12) 0.0084(12) -0.0070(13) C17 0.0348(16) 0.0284(18) 0.0242(14) 0.0010(12) 0.0058(12) -0.0012(13) C18 0.0260(15) 0.0265(16) 0.0233(14) 0.0026(11) 0.0072(11) 0.0038(12) C19 0.0363(18) 0.052(2) 0.0278(16) -0.0020(15) 0.0144(14) 0.0130(16) O20 0.0442(14) 0.0553(16) 0.0333(12) 0.0112(10) 0.0244(10) 0.0141(12) O21 0.0466(19) 0.054(3) 0.031(2) -0.009(2) 0.0127(15) -0.0118(18) C22 0.0248(14) 0.0302(17) 0.0233(13) 0.0023(12) 0.0099(11) -0.0010(12) C23 0.0255(15) 0.0282(17) 0.0236(13) 0.0026(11) 0.0075(11) 0.0026(12) C24 0.0305(16) 0.0307(18) 0.0258(14) -0.0016(12) 0.0082(12) 0.0008(13) O25 0.0435(13) 0.0440(14) 0.0264(10) -0.0050(9) 0.0152(9) -0.0053(11) O26 0.0407(13) 0.0460(14) 0.0342(11) -0.0083(10) 0.0150(10) -0.0155(11) C27 0.0318(16) 0.0393(19) 0.0224(14) 0.0011(12) 0.0128(12) -0.0017(14) N28 0.0464(16) 0.0339(16) 0.0319(13) -0.0007(11) 0.0155(12) -0.0050(13) C29 0.050(2) 0.044(2) 0.0368(17) 0.0050(15) 0.0197(15) 0.0029(17) C30 0.048(2) 0.046(2) 0.0302(16) 0.0066(14) 0.0179(14) 0.0019(17) C31 0.0447(19) 0.0345(19) 0.0325(16) 0.0006(14) 0.0178(14) -0.0065(15) C32 0.051(2) 0.043(2) 0.0301(16) 0.0005(14) 0.0225(15) 0.0017(17) C33 0.051(2) 0.042(2) 0.0262(15) 0.0002(14) 0.0133(14) -0.0017(17) C34 0.0395(18) 0.0340(19) 0.0291(15) -0.0038(13) 0.0139(13) -0.0016(14) C35 0.0366(18) 0.045(2) 0.0429(18) 0.0077(15) 0.0210(14) -0.0039(16) C36 0.042(2) 0.046(2) 0.0410(18) 0.0130(15) 0.0197(15) 0.0000(17) N37 0.0411(16) 0.0370(17) 0.0341(13) -0.0031(12) 0.0191(12) -0.0065(13) C38 0.050(2) 0.047(2) 0.054(2) 0.0070(17) 0.0355(18) 0.0007(18) C39 0.067(3) 0.044(2) 0.051(2) 0.0156(17) 0.0401(19) 0.0081(19) N40 0.0316(14) 0.0354(16) 0.0263(12) 0.0032(11) 0.0091(10) 0.0020(11) C41 0.0359(17) 0.041(2) 0.0260(14) -0.0004(13) 0.0117(13) 0.0029(14) C42 0.0333(17) 0.0307(18) 0.0293(15) 0.0015(13) 0.0136(12) 0.0024(13) C43 0.0321(16) 0.0286(17) 0.0272(14) 0.0067(12) 0.0101(12) 0.0032(13) C44 0.0398(18) 0.0381(19) 0.0241(14) 0.0008(13) 0.0121(13) 0.0006(15) C45 0.0364(17) 0.0367(19) 0.0294(15) 0.0054(13) 0.0143(13) 0.0007(14) C46 0.0316(16) 0.0278(17) 0.0304(15) 0.0045(12) 0.0099(12) 0.0020(13) C47 0.0387(18) 0.0380(19) 0.0275(15) 0.0035(13) 0.0154(13) 0.0018(15) C48 0.0353(17) 0.0383(19) 0.0249(14) -0.0033(13) 0.0095(12) -0.0010(14) N49 0.0355(14) 0.0334(16) 0.0315(13) -0.0013(11) 0.0139(11) -0.0003(12) C50 0.055(2) 0.042(2) 0.0381(17) -0.0075(15) 0.0274(16) -0.0140(17) C51 0.055(2) 0.045(2) 0.0352(17) -0.0122(15) 0.0264(15) -0.0112(17) O52 0.0465(14) 0.0643(18) 0.0295(11) 0.0035(11) 0.0078(10) -0.0092(13) S53 0.0383(5) 0.0626(7) 0.0491(5) 0.0049(4) 0.0078(4) 0.0093(4) O54 0.0501(16) 0.0583(19) 0.0641(17) 0.0041(14) 0.0154(13) 0.0044(13) C55 0.050(2) 0.070(3) 0.071(3) 0.010(2) 0.014(2) 0.006(2) C56 0.056(3) 0.083(3) 0.056(2) -0.006(2) 0.006(2) 0.013(2) O57 0.0559(16) 0.066(2) 0.0558(15) 0.0100(13) 0.0297(13) 0.0035(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 Zn1 O1 2.0332(19) . ? Zn1 N28 2.119(3) . ? Zn1 O8 2.139(2) 4_565 ? Zn1 N40 2.171(3) . ? Zn1 O52 2.206(2) . ? Zn1 O9 2.242(2) 4_565 ? Zn1 C7 2.508(3) 4_565 ? Zn2 O20 1.995(2) 4 ? Zn2 O25 2.017(2) . ? Zn2 N49 2.050(3) 1_445 ? Zn2 N37 2.116(3) 1_455 ? Zn2 O26 2.423(2) . ? Zn2 C24 2.545(3) . ? O1 C3 1.272(4) . ? O2 C3 1.255(4) . ? C3 C4 1.509(4) . ? C4 C5 1.385(4) . ? C4 C12 1.389(4) . ? C5 C6 1.394(4) . ? C5 H5 0.9500 . ? C6 C10 1.399(4) . ? C6 C7 1.504(4) . ? C7 O9 1.257(4) . ? C7 O8 1.259(3) . ? C7 Zn1 2.508(3) 4_566 ? O8 Zn1 2.139(2) 4_566 ? O9 Zn1 2.242(2) 4_566 ? C10 C11 1.381(4) . ? C10 H10 0.9500 . ? C11 C12 1.385(4) . ? C11 O13 1.393(4) . ? C12 H12 0.9500 . ? O13 C14 1.404(4) . ? C14 O15 1.410(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C16 1.373(3) . ? C16 C27 1.390(4) . ? C16 C17 1.392(4) . ? C17 C18 1.379(4) . ? C17 H17 0.9500 . ? C18 C22 1.393(4) . ? C18 C19 1.505(4) . ? C19 O21 1.219(4) . ? C19 O20 1.266(4) . ? O20 Zn2 1.995(2) 4_556 ? C22 C23 1.397(4) . ? C22 H22 0.9500 . ? C23 C27 1.394(4) . ? C23 C24 1.500(4) . ? C24 O26 1.254(4) . ? C24 O25 1.266(3) . ? C27 H27 0.9500 . ? N28 C33 1.340(4) . ? N28 C29 1.345(4) . ? C29 C30 1.372(5) . ? C29 H29 0.9500 . ? C30 C31 1.389(4) . ? C30 H30 0.9500 . ? C31 C32 1.387(4) . ? C31 C34 1.494(5) . ? C32 C33 1.365(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.382(5) . ? C34 C35 1.387(5) . ? C35 C36 1.374(5) . ? C35 H35 0.9500 . ? C36 N37 1.346(4) . ? C36 H36 0.9500 . ? N37 C38 1.344(4) . ? N37 Zn2 2.116(3) 1_655 ? C38 C39 1.374(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? N40 C41 1.339(4) . ? N40 C45 1.346(4) . ? C41 C42 1.389(4) . ? C41 H41 0.9500 . ? C42 C43 1.394(4) . ? C42 H42 0.9500 . ? C43 C44 1.395(4) . ? C43 C46 1.483(4) . ? C44 C45 1.385(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.398(4) . ? C46 C47 1.395(4) . ? C47 C48 1.372(4) . ? C47 H47 0.9500 . ? C48 N49 1.340(4) . ? C48 H48 0.9500 . ? N49 C50 1.350(4) . ? N49 Zn2 2.050(3) 1_665 ? C50 C51 1.366(5) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? O52 H52A 0.9035 . ? O52 H52B 0.9022 . ? S53 O54 1.504(3) . ? S53 C56 1.784(4) . ? S53 C55 1.799(4) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? O57 H57A 0.9019 . ? O57 H57B 0.9008 . ? 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 Zn1 N28 99.77(9) . . ? O1 Zn1 O8 98.49(8) . 4_565 ? N28 Zn1 O8 161.55(9) . 4_565 ? O1 Zn1 N40 94.55(9) . . ? N28 Zn1 N40 88.85(10) . . ? O8 Zn1 N40 87.09(9) 4_565 . ? O1 Zn1 O52 91.81(8) . . ? N28 Zn1 O52 95.59(10) . . ? O8 Zn1 O52 86.44(10) 4_565 . ? N40 Zn1 O52 171.53(9) . . ? O1 Zn1 O9 158.42(9) . 4_565 ? N28 Zn1 O9 101.72(9) . 4_565 ? O8 Zn1 O9 60.17(8) 4_565 4_565 ? N40 Zn1 O9 87.84(8) . 4_565 ? O52 Zn1 O9 84.20(8) . 4_565 ? O1 Zn1 C7 128.55(10) . 4_565 ? N28 Zn1 C7 131.68(10) . 4_565 ? O8 Zn1 C7 30.13(9) 4_565 4_565 ? N40 Zn1 C7 87.19(9) . 4_565 ? O52 Zn1 C7 84.47(10) . 4_565 ? O9 Zn1 C7 30.04(9) 4_565 4_565 ? O20 Zn2 O25 99.90(9) 4 . ? O20 Zn2 N49 105.35(9) 4 1_445 ? O25 Zn2 N49 146.11(9) . 1_445 ? O20 Zn2 N37 94.38(10) 4 1_455 ? O25 Zn2 N37 104.18(10) . 1_455 ? N49 Zn2 N37 96.13(10) 1_445 1_455 ? O20 Zn2 O26 158.42(8) 4 . ? O25 Zn2 O26 58.53(8) . . ? N49 Zn2 O26 94.89(9) 1_445 . ? N37 Zn2 O26 90.76(9) 1_455 . ? O20 Zn2 C24 129.32(10) 4 . ? O25 Zn2 C24 29.42(9) . . ? N49 Zn2 C24 121.41(10) 1_445 . ? N37 Zn2 C24 98.68(10) 1_455 . ? O26 Zn2 C24 29.11(8) . . ? C3 O1 Zn1 124.86(18) . . ? O2 C3 O1 125.2(3) . . ? O2 C3 C4 117.8(3) . . ? O1 C3 C4 117.0(3) . . ? C5 C4 C12 120.4(3) . . ? C5 C4 C3 121.6(3) . . ? C12 C4 C3 118.0(3) . . ? C4 C5 C6 119.5(3) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C5 C6 C10 120.1(3) . . ? C5 C6 C7 121.3(3) . . ? C10 C6 C7 118.6(3) . . ? O9 C7 O8 121.7(3) . . ? O9 C7 C6 120.0(3) . . ? O8 C7 C6 118.3(3) . . ? O9 C7 Zn1 63.20(16) . 4_566 ? O8 C7 Zn1 58.48(16) . 4_566 ? C6 C7 Zn1 176.4(2) . 4_566 ? C7 O8 Zn1 91.4(2) . 4_566 ? C7 O9 Zn1 86.77(17) . 4_566 ? C11 C10 C6 119.7(3) . . ? C11 C10 H10 120.2 . . ? C6 C10 H10 120.2 . . ? C10 C11 C12 120.4(3) . . ? C10 C11 O13 124.3(3) . . ? C12 C11 O13 115.2(3) . . ? C11 C12 C4 119.9(3) . . ? C11 C12 H12 120.0 . . ? C4 C12 H12 120.0 . . ? C11 O13 C14 117.1(3) . . ? O13 C14 O15 113.1(3) . . ? O13 C14 H14A 109.0 . . ? O15 C14 H14A 109.0 . . ? O13 C14 H14B 109.0 . . ? O15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 O15 C14 117.3(3) . . ? O15 C16 C27 124.1(3) . . ? O15 C16 C17 115.9(3) . . ? C27 C16 C17 120.0(3) . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C22 119.8(3) . . ? C17 C18 C19 118.7(3) . . ? C22 C18 C19 121.5(3) . . ? O21 C19 O20 123.3(3) . . ? O21 C19 C18 119.1(3) . . ? O20 C19 C18 117.5(3) . . ? C19 O20 Zn2 117.5(2) . 4_556 ? C23 C22 C18 119.9(3) . . ? C23 C22 H22 120.1 . . ? C18 C22 H22 120.1 . . ? C27 C23 C22 120.1(3) . . ? C27 C23 C24 119.1(3) . . ? C22 C23 C24 120.8(3) . . ? O26 C24 O25 121.5(3) . . ? O26 C24 C23 120.6(3) . . ? O25 C24 C23 117.9(3) . . ? O26 C24 Zn2 70.04(16) . . ? O25 C24 Zn2 51.51(14) . . ? C23 C24 Zn2 169.3(2) . . ? C24 O25 Zn2 99.07(19) . . ? C24 O26 Zn2 80.84(16) . . ? C23 C27 C16 119.5(3) . . ? C23 C27 H27 120.2 . . ? C16 C27 H27 120.2 . . ? C33 N28 C29 115.6(3) . . ? C33 N28 Zn1 121.0(2) . . ? C29 N28 Zn1 119.7(2) . . ? N28 C29 C30 124.4(3) . . ? N28 C29 H29 117.8 . . ? C30 C29 H29 117.8 . . ? C29 C30 C31 119.0(3) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C32 C31 C30 117.0(3) . . ? C32 C31 C34 122.1(3) . . ? C30 C31 C34 120.7(3) . . ? C33 C32 C31 120.0(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? N28 C33 C32 123.8(3) . . ? N28 C33 H33 118.1 . . ? C32 C33 H33 118.1 . . ? C39 C34 C35 116.6(3) . . ? C39 C34 C31 122.4(3) . . ? C35 C34 C31 120.9(3) . . ? C36 C35 C34 119.5(3) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? N37 C36 C35 124.0(3) . . ? N37 C36 H36 118.0 . . ? C35 C36 H36 118.0 . . ? C36 N37 C38 116.1(3) . . ? C36 N37 Zn2 123.0(2) . 1_655 ? C38 N37 Zn2 120.8(2) . 1_655 ? N37 C38 C39 122.9(3) . . ? N37 C38 H38 118.6 . . ? C39 C38 H38 118.6 . . ? C38 C39 C34 120.8(3) . . ? C38 C39 H39 119.6 . . ? C34 C39 H39 119.6 . . ? C41 N40 C45 117.9(3) . . ? C41 N40 Zn1 122.3(2) . . ? C45 N40 Zn1 118.8(2) . . ? N40 C41 C42 123.2(3) . . ? N40 C41 H41 118.4 . . ? C42 C41 H41 118.4 . . ? C43 C42 C41 119.3(3) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C42 C43 C44 117.1(3) . . ? C42 C43 C46 121.3(3) . . ? C44 C43 C46 121.3(3) . . ? C45 C44 C43 120.2(3) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? N40 C45 C44 122.2(3) . . ? N40 C45 H45 118.9 . . ? C44 C45 H45 118.9 . . ? C51 C46 C47 116.4(3) . . ? C51 C46 C43 121.2(3) . . ? C47 C46 C43 122.2(3) . . ? C48 C47 C46 119.9(3) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? N49 C48 C47 123.4(3) . . ? N49 C48 H48 118.3 . . ? C47 C48 H48 118.3 . . ? C48 N49 C50 116.8(3) . . ? C48 N49 Zn2 123.8(2) . 1_665 ? C50 N49 Zn2 117.7(2) . 1_665 ? N49 C50 C51 123.1(3) . . ? N49 C50 H50 118.4 . . ? C51 C50 H50 118.4 . . ? C50 C51 C46 120.1(3) . . ? C50 C51 H51 120.0 . . ? C46 C51 H51 120.0 . . ? Zn1 O52 H52A 92.5 . . ? Zn1 O52 H52B 110.8 . . ? H52A O52 H52B 112.1 . . ? O54 S53 C56 105.5(2) . . ? O54 S53 C55 107.1(2) . . ? C56 S53 C55 96.8(2) . . ? S53 C55 H55A 109.5 . . ? S53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? S53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? S53 C56 H56A 109.5 . . ? S53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? S53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? H57A O57 H57B 112.4 . . ? 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 O52 H52A O2 0.90 1.70 2.589(3) 167 . O52 H52B O54 0.90 2.00 2.892(4) 172 4_565 O57 H57A O54 0.90 1.95 2.753(4) 147 . O57 H57B O26 0.90 1.87 2.768(3) 176 3 # 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 0.299 -0.098 0.503 56 19 ' ' 2 0.701 0.097 0.497 56 19 ' ' 3 0.970 0.042 0.083 9 1 ' ' 4 0.700 0.402 0.997 56 19 ' ' 5 0.970 0.458 0.583 9 1 ' ' 6 0.299 0.597 1.003 56 19 ' ' 7 0.030 0.542 0.417 9 1 ' ' 8 0.030 0.958 0.917 9 1 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.014 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.086 #=======================END================================= data_11 _database_code_depnum_ccdc_archive 'CCDC 779792' #TrackingRef '- Paper2-CIF_b.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H14 Ag2 N O10' _chemical_formula_sum 'C22 H14 Ag2 N O10' _chemical_formula_weight 668.08 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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7679(2) _cell_length_b 10.6578(4) _cell_length_c 12.8283(3) _cell_angle_alpha 78.834(2) _cell_angle_beta 73.855(2) _cell_angle_gamma 80.3001(12) _cell_volume 993.41(5) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4415 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 27.88 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 654 _exptl_absorpt_coefficient_mu 2.039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6297 _exptl_absorpt_correction_T_max 0.8221 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18547 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4699 _reflns_number_gt 3680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The two silver ions reveal twofold disorder. The disordered positions of each atom are represented by Ag1a and Ag1b, and Ag2a and Ag2b sites. ; _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^+1.4635P] 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 4699 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 Ag1A Ag 1.1356(10) -0.0375(2) 0.1176(3) 0.0254(5) Uani 0.56(2) 1 d P . . Ag1B Ag 1.0796(15) -0.0358(3) 0.1286(3) 0.0249(8) Uani 0.44(2) 1 d P . . Ag2A Ag 1.4163(6) 0.1335(3) -0.04690(14) 0.0227(4) Uani 0.572(13) 1 d P . . Ag2B Ag 1.3603(8) 0.1045(5) -0.0323(3) 0.0243(7) Uani 0.428(13) 1 d P . . O3 O 1.0829(3) 0.1366(2) 0.19462(18) 0.0209(5) Uani 1 1 d . . . O4 O 1.3283(3) 0.2273(2) 0.09153(17) 0.0218(5) Uani 1 1 d . . . C5 C 1.1885(4) 0.2243(3) 0.1683(2) 0.0156(6) Uani 1 1 d . . . C6 C 1.1382(4) 0.3324(3) 0.2337(2) 0.0158(6) Uani 1 1 d . . . C7 C 1.2554(4) 0.4257(3) 0.2132(2) 0.0163(6) Uani 1 1 d . . . H7 H 1.3683 0.4183 0.1603 0.020 Uiso 1 1 calc R . . C8 C 1.2051(4) 0.5294(3) 0.2709(2) 0.0153(6) Uani 1 1 d . . . C9 C 1.3281(4) 0.6311(3) 0.2435(2) 0.0177(6) Uani 1 1 d . . . O10 O 1.4658(3) 0.6310(2) 0.1697(2) 0.0271(5) Uani 1 1 d . . . O11 O 1.2693(3) 0.7231(2) 0.30574(18) 0.0223(5) Uani 1 1 d . . . H11 H 1.3269 0.7865 0.2774 0.033 Uiso 1 1 calc R . . C12 C 1.0396(4) 0.5418(3) 0.3479(2) 0.0158(6) Uani 1 1 d . . . H12 H 1.0062 0.6125 0.3875 0.019 Uiso 1 1 calc R . . C13 C 0.9235(4) 0.4493(3) 0.3662(2) 0.0154(6) Uani 1 1 d . . . C14 C 0.9715(4) 0.3453(3) 0.3095(2) 0.0154(6) Uani 1 1 d . . . H14 H 0.8907 0.2830 0.3224 0.018 Uiso 1 1 calc R . . O15 O 0.7584(3) 0.47077(19) 0.44144(17) 0.0183(4) Uani 1 1 d . . . C16 C 0.6492(4) 0.3709(3) 0.4725(2) 0.0172(6) Uani 1 1 d . . . H16A H 0.5523 0.3855 0.5394 0.021 Uiso 1 1 calc R . . H16B H 0.7221 0.2874 0.4885 0.021 Uiso 1 1 calc R . . O17 O 0.5722(3) 0.36922(19) 0.38338(16) 0.0161(4) Uani 1 1 d . . . C18 C 0.4940(4) 0.2582(3) 0.3947(2) 0.0147(6) Uani 1 1 d . . . C19 C 0.3634(4) 0.2180(3) 0.4871(2) 0.0171(6) Uani 1 1 d . . . H19 H 0.3251 0.2662 0.5464 0.020 Uiso 1 1 calc R . . C20 C 0.2876(4) 0.1060(3) 0.4932(2) 0.0152(6) Uani 1 1 d . . . C21 C 0.1559(4) 0.0616(3) 0.5976(2) 0.0172(6) Uani 1 1 d . . . O22 O 0.0956(3) -0.0485(2) 0.59858(18) 0.0200(4) Uani 1 1 d . . . H22 H 0.0333 -0.0734 0.6619 0.030 Uiso 1 1 calc R . . O23 O 0.1110(3) 0.1194(2) 0.67580(18) 0.0233(5) Uani 1 1 d . . . C24 C 0.3400(4) 0.0376(3) 0.4055(2) 0.0167(6) Uani 1 1 d . . . H24 H 0.2845 -0.0365 0.4088 0.020 Uiso 1 1 calc R . . C25 C 0.4736(4) 0.0771(3) 0.3126(2) 0.0156(6) Uani 1 1 d . . . C26 C 0.5525(4) 0.1875(3) 0.3075(2) 0.0159(6) Uani 1 1 d . . . H26 H 0.6453 0.2144 0.2451 0.019 Uiso 1 1 calc R . . C27 C 0.5342(4) 0.0057(3) 0.2166(3) 0.0208(6) Uani 1 1 d . . . O28 O 0.6734(3) 0.0295(2) 0.14362(18) 0.0244(5) Uani 1 1 d . . . O29 O 0.4368(3) -0.0777(2) 0.21232(18) 0.0244(5) Uani 1 1 d . . . N30 N 1.0878(4) -0.2158(3) 0.0730(2) 0.0254(6) Uani 1 1 d . . . C31 C 1.2092(5) -0.2775(3) -0.0023(3) 0.0302(8) Uani 1 1 d . . . H31 H 1.3201 -0.2434 -0.0369 0.036 Uiso 1 1 calc R . . C32 C 1.1810(5) -0.3890(3) -0.0324(3) 0.0265(7) Uani 1 1 d . . . H32 H 1.2718 -0.4298 -0.0861 0.032 Uiso 1 1 calc R . . C33 C 1.0194(4) -0.4411(3) 0.0161(2) 0.0176(6) Uani 1 1 d . . . C34 C 0.8944(4) -0.3779(3) 0.0958(3) 0.0213(6) Uani 1 1 d . . . H34 H 0.7825 -0.4101 0.1317 0.026 Uiso 1 1 calc R . . C35 C 0.9331(5) -0.2679(3) 0.1227(3) 0.0240(7) Uani 1 1 d . . . H35 H 0.8471 -0.2273 0.1786 0.029 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 Ag1A 0.0343(14) 0.0167(3) 0.0268(6) -0.0104(3) -0.0036(8) -0.0067(6) Ag1B 0.039(2) 0.0174(4) 0.0189(6) -0.0094(3) -0.0012(9) -0.0091(8) Ag2A 0.0319(9) 0.0199(5) 0.0148(3) -0.0081(3) -0.0006(4) -0.0015(6) Ag2B 0.0329(13) 0.0235(9) 0.0167(5) -0.0127(5) -0.0033(7) 0.0023(9) O3 0.0279(12) 0.0154(10) 0.0213(11) -0.0093(9) -0.0042(9) -0.0040(9) O4 0.0268(12) 0.0204(11) 0.0156(10) -0.0094(9) 0.0016(9) 0.0001(9) C5 0.0193(14) 0.0137(13) 0.0128(13) -0.0041(11) -0.0035(11) 0.0017(11) C6 0.0185(14) 0.0153(14) 0.0144(13) -0.0034(11) -0.0046(11) -0.0024(11) C7 0.0176(14) 0.0183(14) 0.0128(13) -0.0015(11) -0.0034(11) -0.0034(12) C8 0.0169(14) 0.0177(14) 0.0130(13) -0.0060(11) -0.0041(11) -0.0019(11) C9 0.0158(15) 0.0217(15) 0.0173(14) -0.0071(12) -0.0045(12) -0.0019(12) O10 0.0199(12) 0.0274(12) 0.0329(13) -0.0157(10) 0.0060(10) -0.0084(10) O11 0.0257(12) 0.0226(11) 0.0212(11) -0.0092(9) -0.0013(9) -0.0113(9) C12 0.0198(14) 0.0159(14) 0.0130(13) -0.0075(11) -0.0026(11) -0.0026(11) C13 0.0133(13) 0.0157(14) 0.0158(14) -0.0045(11) -0.0004(11) -0.0014(11) C14 0.0154(14) 0.0143(13) 0.0162(14) -0.0060(11) -0.0013(11) -0.0021(11) O15 0.0166(10) 0.0159(10) 0.0216(11) -0.0105(8) 0.0029(8) -0.0044(8) C16 0.0179(14) 0.0187(14) 0.0167(14) -0.0052(11) -0.0028(11) -0.0069(12) O17 0.0197(10) 0.0148(10) 0.0143(10) -0.0027(8) -0.0031(8) -0.0051(8) C18 0.0156(14) 0.0104(13) 0.0192(14) -0.0031(11) -0.0067(11) 0.0002(11) C19 0.0187(14) 0.0152(14) 0.0174(14) -0.0049(11) -0.0043(12) -0.0001(11) C20 0.0133(13) 0.0140(13) 0.0183(14) -0.0035(11) -0.0041(11) -0.0002(11) C21 0.0166(14) 0.0153(14) 0.0207(15) -0.0045(12) -0.0057(12) -0.0008(11) O22 0.0232(11) 0.0167(11) 0.0200(11) -0.0034(9) -0.0021(9) -0.0076(9) O23 0.0280(12) 0.0191(11) 0.0215(11) -0.0094(9) 0.0021(9) -0.0061(9) C24 0.0182(14) 0.0120(13) 0.0208(15) -0.0033(11) -0.0066(12) -0.0006(11) C25 0.0176(14) 0.0161(14) 0.0140(13) -0.0055(11) -0.0062(11) 0.0029(11) C26 0.0165(14) 0.0152(14) 0.0153(14) -0.0047(11) -0.0026(11) -0.0003(11) C27 0.0277(17) 0.0145(14) 0.0195(15) -0.0049(12) -0.0078(13) 0.0051(12) O28 0.0325(13) 0.0194(11) 0.0181(11) -0.0081(9) 0.0017(10) -0.0020(10) O29 0.0375(13) 0.0185(11) 0.0195(11) -0.0091(9) -0.0041(10) -0.0078(10) N30 0.0447(17) 0.0136(12) 0.0202(13) -0.0041(10) -0.0077(12) -0.0092(12) C31 0.048(2) 0.0205(16) 0.0195(16) -0.0056(13) 0.0049(15) -0.0158(15) C32 0.0344(19) 0.0188(15) 0.0214(16) -0.0079(13) 0.0093(14) -0.0122(14) C33 0.0259(16) 0.0124(14) 0.0139(13) -0.0021(11) -0.0055(12) -0.0005(12) C34 0.0204(15) 0.0197(15) 0.0257(16) -0.0116(13) -0.0077(13) 0.0044(12) C35 0.0295(17) 0.0187(15) 0.0259(16) -0.0113(13) -0.0095(14) 0.0049(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 Ag1A O3 2.195(3) . ? Ag1A N30 2.203(4) . ? Ag1A Ag2B 2.632(10) . ? Ag1A Ag2A 3.134(8) . ? Ag1B N30 2.159(4) . ? Ag1B O3 2.174(3) . ? Ag1B O23 2.606(7) 2_656 ? Ag1B Ag2B 2.941(11) . ? Ag2A Ag2B 0.546(3) . ? Ag2A O4 2.098(2) . ? Ag2A O29 2.252(3) 2_755 ? Ag2A Ag2B 2.9952(14) 2_855 ? Ag2A Ag2A 3.087(3) 2_855 ? Ag2B O4 2.185(3) . ? Ag2B O28 2.296(4) 2_755 ? Ag2B O29 2.445(5) 2_755 ? Ag2B C27 2.705(3) 2_755 ? Ag2B Ag2A 2.9952(14) 2_855 ? Ag2B Ag2B 3.001(3) 2_855 ? O3 C5 1.282(4) . ? O4 C5 1.247(4) . ? C5 C6 1.491(4) . ? C6 C14 1.391(4) . ? C6 C7 1.399(4) . ? C7 C8 1.391(4) . ? C7 H7 0.9500 . ? C8 C12 1.390(4) . ? C8 C9 1.492(4) . ? C9 O10 1.215(4) . ? C9 O11 1.325(4) . ? O11 H11 0.8400 . ? C12 C13 1.390(4) . ? C12 H12 0.9500 . ? C13 O15 1.388(3) . ? C13 C14 1.385(4) . ? C14 H14 0.9500 . ? O15 C16 1.402(3) . ? C16 O17 1.434(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O17 C18 1.384(3) . ? C18 C19 1.378(4) . ? C18 C26 1.398(4) . ? C19 C20 1.398(4) . ? C19 H19 0.9500 . ? C20 C24 1.388(4) . ? C20 C21 1.490(4) . ? C21 O23 1.217(4) . ? C21 O22 1.332(4) . ? O22 H22 0.8400 . ? O23 Ag1B 2.606(7) 2_656 ? C24 C25 1.393(4) . ? C24 H24 0.9500 . ? C25 C26 1.398(4) . ? C25 C27 1.496(4) . ? C26 H26 0.9500 . ? C27 O28 1.245(4) . ? C27 O29 1.279(4) . ? C27 Ag2B 2.705(3) 2_755 ? O28 Ag2B 2.296(4) 2_755 ? O29 Ag2A 2.252(3) 2_755 ? O29 Ag2B 2.445(5) 2_755 ? N30 C31 1.336(5) . ? N30 C35 1.349(5) . ? C31 C32 1.386(4) . ? C31 H31 0.9500 . ? C32 C33 1.392(5) . ? C32 H32 0.9500 . ? C33 C34 1.391(4) . ? C33 C33 1.495(6) 2_745 ? C34 C35 1.385(4) . ? C34 H34 0.9500 . ? C35 H35 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 O3 Ag1A N30 159.6(4) . . ? O3 Ag1A Ag2B 80.71(15) . . ? N30 Ag1A Ag2B 116.8(2) . . ? O3 Ag1A Ag2A 78.34(15) . . ? N30 Ag1A Ag2A 119.8(2) . . ? N30 Ag1B O3 175.3(3) . . ? N30 Ag1B O23 91.8(2) . 2_656 ? O3 Ag1B O23 85.93(17) . 2_656 ? N30 Ag1B Ag2B 107.0(3) . . ? O3 Ag1B Ag2B 74.1(2) . . ? O23 Ag1B Ag2B 155.7(2) 2_656 . ? Ag2B Ag2A O4 91.8(2) . . ? Ag2B Ag2A O29 104.4(3) . 2_755 ? O4 Ag2A O29 163.5(3) . 2_755 ? O4 Ag2A Ag2B 102.37(7) . 2_855 ? O29 Ag2A Ag2B 82.39(9) 2_755 2_855 ? O4 Ag2A Ag2A 102.33(8) . 2_855 ? O29 Ag2A Ag2A 85.14(7) 2_755 2_855 ? O4 Ag2A Ag1A 76.25(14) . . ? O29 Ag2A Ag1A 120.23(18) 2_755 . ? Ag2B Ag2A Ag1A 75.3(2) 2_855 . ? Ag2A Ag2A Ag1A 65.70(19) 2_855 . ? Ag2A Ag2B O4 73.7(3) . . ? Ag2A Ag2B O28 118.5(3) . 2_755 ? O4 Ag2B O28 167.0(4) . 2_755 ? Ag2A Ag2B O29 63.1(3) . 2_755 ? O4 Ag2B O29 136.7(4) . 2_755 ? O28 Ag2B O29 55.42(8) 2_755 2_755 ? Ag2A Ag2B Ag1A 154.5(2) . . ? O4 Ag2B Ag1A 86.99(17) . . ? O28 Ag2B Ag1A 82.4(3) 2_755 . ? O29 Ag2B Ag1A 134.9(2) 2_755 . ? Ag2A Ag2B C27 91.3(3) . 2_755 ? O4 Ag2B C27 164.7(4) . 2_755 ? O28 Ag2B C27 27.28(9) 2_755 2_755 ? O29 Ag2B C27 28.17(9) 2_755 2_755 ? Ag1A Ag2B C27 108.2(2) . 2_755 ? Ag2A Ag2B Ag1B 157.3(2) . . ? O4 Ag2B Ag1B 86.41(18) . . ? O28 Ag2B Ag1B 82.3(2) 2_755 . ? O29 Ag2B Ag1B 136.4(2) 2_755 . ? Ag1A Ag2B Ag1B 5.76(10) . . ? C27 Ag2B Ag1B 108.8(2) 2_755 . ? Ag2A Ag2B Ag2A 94.6(3) . 2_855 ? O4 Ag2B Ag2A 103.05(9) . 2_855 ? O28 Ag2B Ag2A 81.07(15) 2_755 2_855 ? O29 Ag2B Ag2A 84.02(11) 2_755 2_855 ? Ag1A Ag2B Ag2A 73.4(2) . 2_855 ? C27 Ag2B Ag2A 80.59(7) 2_755 2_855 ? Ag1B Ag2B Ag2A 79.1(3) . 2_855 ? Ag2A Ag2B Ag2B 84.1(3) . 2_855 ? O4 Ag2B Ag2B 100.03(13) . 2_855 ? O28 Ag2B Ag2B 86.10(15) 2_755 2_855 ? O29 Ag2B Ag2B 79.27(16) 2_755 2_855 ? Ag1A Ag2B Ag2B 83.0(3) . 2_855 ? C27 Ag2B Ag2B 80.85(8) 2_755 2_855 ? Ag1B Ag2B Ag2B 88.8(3) . 2_855 ? C5 O3 Ag1B 134.0(3) . . ? C5 O3 Ag1A 124.1(3) . . ? C5 O4 Ag2A 131.6(3) . . ? C5 O4 Ag2B 117.2(3) . . ? O4 C5 O3 125.2(3) . . ? O4 C5 C6 117.5(3) . . ? O3 C5 C6 117.3(3) . . ? C14 C6 C7 120.0(3) . . ? C14 C6 C5 120.5(3) . . ? C7 C6 C5 119.4(3) . . ? C8 C7 C6 119.4(3) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C12 C8 C7 120.8(3) . . ? C12 C8 C9 120.8(3) . . ? C7 C8 C9 118.4(3) . . ? O10 C9 O11 123.6(3) . . ? O10 C9 C8 123.3(3) . . ? O11 C9 C8 113.2(2) . . ? C9 O11 H11 109.5 . . ? C8 C12 C13 119.1(3) . . ? C8 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? O15 C13 C14 123.5(3) . . ? O15 C13 C12 115.7(2) . . ? C14 C13 C12 120.8(3) . . ? C6 C14 C13 119.8(3) . . ? C6 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C13 O15 C16 116.7(2) . . ? O15 C16 O17 107.9(2) . . ? O15 C16 H16A 110.1 . . ? O17 C16 H16A 110.1 . . ? O15 C16 H16B 110.1 . . ? O17 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? C18 O17 C16 112.8(2) . . ? C19 C18 O17 122.2(3) . . ? C19 C18 C26 120.7(3) . . ? O17 C18 C26 117.1(3) . . ? C18 C19 C20 119.5(3) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C24 C20 C19 120.2(3) . . ? C24 C20 C21 122.1(3) . . ? C19 C20 C21 117.6(3) . . ? O23 C21 O22 123.1(3) . . ? O23 C21 C20 122.9(3) . . ? O22 C21 C20 114.0(3) . . ? C21 O22 H22 109.5 . . ? C21 O23 Ag1B 125.8(2) . 2_656 ? C20 C24 C25 120.3(3) . . ? C20 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 119.5(3) . . ? C24 C25 C27 121.8(3) . . ? C26 C25 C27 118.6(3) . . ? C25 C26 C18 119.7(3) . . ? C25 C26 H26 120.2 . . ? C18 C26 H26 120.2 . . ? O28 C27 O29 122.2(3) . . ? O28 C27 C25 120.1(3) . . ? O29 C27 C25 117.7(3) . . ? O28 C27 Ag2B 57.7(2) . 2_755 ? O29 C27 Ag2B 64.6(2) . 2_755 ? C25 C27 Ag2B 175.2(2) . 2_755 ? C27 O28 Ag2B 95.0(3) . 2_755 ? C27 O29 Ag2A 99.8(2) . 2_755 ? C27 O29 Ag2B 87.3(3) . 2_755 ? C31 N30 C35 117.3(3) . . ? C31 N30 Ag1B 132.4(4) . . ? C35 N30 Ag1B 110.1(3) . . ? C31 N30 Ag1A 122.2(3) . . ? C35 N30 Ag1A 120.4(3) . . ? N30 C31 C32 123.1(3) . . ? N30 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? C31 C32 C33 119.9(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 116.9(3) . . ? C34 C33 C33 121.3(4) . 2_745 ? C32 C33 C33 121.8(3) . 2_745 ? C35 C34 C33 120.0(3) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? N30 C35 C34 122.7(3) . . ? N30 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11 O29 0.84 1.75 2.591(3) 176 1_665 O22 H22 O3 0.84 1.86 2.696(3) 174 2_656 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.606 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.128 #========================END=================================== data_12 _database_code_depnum_ccdc_archive 'CCDC 779793' #TrackingRef '- Paper2-CIF_b.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 Co N2 O10' _chemical_formula_sum 'C28 H20 Co N2 O10' _chemical_formula_weight 603.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 20.2908(13) _cell_length_b 9.9513(6) _cell_length_c 14.5720(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.450(3) _cell_angle_gamma 90.00 _cell_volume 2634.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2812 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.32 _exptl_crystal_description parallelpiped _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9003 _exptl_absorpt_correction_T_max 0.9651 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16150 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.32 _reflns_number_total 2672 _reflns_number_gt 2123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+2.4315P] 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 2672 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.077 _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 Co Co 0.0000 0.04339(5) 0.2500 0.01985(18) Uani 1 2 d S . . O1 O 0.01770(10) 0.1315(2) 0.14085(15) 0.0261(5) Uani 1 1 d . . . O2 O 0.10417(11) 0.21428(19) 0.28495(15) 0.0235(5) Uani 1 1 d . . . C3 C 0.07161(15) 0.2100(3) 0.1887(2) 0.0219(6) Uani 1 1 d . . . C4 C 0.09275(15) 0.3052(3) 0.1265(2) 0.0216(6) Uani 1 1 d . . . C5 C 0.15489(15) 0.3859(3) 0.1735(2) 0.0228(6) Uani 1 1 d . . . H5 H 0.1852 0.3788 0.2452 0.027 Uiso 1 1 calc R . . C6 C 0.17255(15) 0.4763(3) 0.1161(2) 0.0219(6) Uani 1 1 d . . . C7 C 0.24155(15) 0.5565(3) 0.1699(2) 0.0239(6) Uani 1 1 d . . . O8 O 0.25802(11) 0.6313(2) 0.10748(16) 0.0311(5) Uani 1 1 d . . . H8 H 0.3101 0.6648 0.1468 0.037 Uiso 1 1 d R . . O9 O 0.27882(11) 0.5533(2) 0.26161(16) 0.0343(5) Uani 1 1 d . . . C10 C 0.12845(15) 0.4889(3) 0.0103(2) 0.0223(6) Uani 1 1 d . . . H10 H 0.1408 0.5513 -0.0289 0.027 Uiso 1 1 calc R . . C11 C 0.06623(15) 0.4081(3) -0.0362(2) 0.0219(6) Uani 1 1 d . . . C12 C 0.04857(15) 0.3165(3) 0.0216(2) 0.0219(6) Uani 1 1 d . . . H12 H 0.0061 0.2615 -0.0108 0.026 Uiso 1 1 calc R . . O13 O 0.01895(10) 0.41095(19) -0.13873(15) 0.0247(5) Uani 1 1 d . . . C14 C 0.03109(15) 0.5160(3) -0.1972(2) 0.0216(6) Uani 1 1 d . . . H14A H 0.0782 0.5007 -0.2005 0.026 Uiso 1 1 calc R . . H14B H 0.0338 0.6040 -0.1640 0.026 Uiso 1 1 calc R . . N15 N 0.08477(12) -0.0792(2) 0.33936(18) 0.0213(5) Uani 1 1 d . . . C16 C 0.12116(16) -0.0525(3) 0.4399(2) 0.0285(7) Uani 1 1 d . . . H16 H 0.1022 0.0148 0.4678 0.034 Uiso 1 1 calc R . . C17 C 0.18500(16) -0.1183(3) 0.5047(2) 0.0287(7) Uani 1 1 d . . . H17 H 0.2082 -0.0972 0.5757 0.034 Uiso 1 1 calc R . . C18 C 0.21521(15) -0.2147(3) 0.4665(2) 0.0204(6) Uani 1 1 d . . . C19 C 0.17745(16) -0.2425(3) 0.3619(2) 0.0275(7) Uani 1 1 d . . . H19 H 0.1958 -0.3080 0.3318 0.033 Uiso 1 1 calc R . . C20 C 0.11304(16) -0.1740(3) 0.3022(2) 0.0281(7) Uani 1 1 d . . . H20 H 0.0877 -0.1954 0.2313 0.034 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 Co 0.0192(3) 0.0213(3) 0.0172(3) 0.000 0.0064(2) 0.000 O1 0.0220(11) 0.0288(11) 0.0257(11) 0.0025(9) 0.0090(9) -0.0030(9) O2 0.0254(10) 0.0256(11) 0.0207(11) 0.0021(9) 0.0113(9) 0.0049(9) C3 0.0202(15) 0.0224(15) 0.0256(16) 0.0032(12) 0.0124(13) 0.0050(12) C4 0.0202(14) 0.0233(15) 0.0218(16) -0.0007(12) 0.0097(12) 0.0044(12) C5 0.0214(15) 0.0271(15) 0.0194(15) -0.0026(12) 0.0085(13) 0.0019(12) C6 0.0215(15) 0.0237(15) 0.0226(16) -0.0027(12) 0.0118(13) -0.0002(12) C7 0.0246(15) 0.0258(15) 0.0223(16) -0.0034(13) 0.0112(13) -0.0013(13) O8 0.0272(11) 0.0409(13) 0.0218(11) 0.0022(10) 0.0079(9) -0.0105(10) O9 0.0347(12) 0.0467(13) 0.0189(12) -0.0061(10) 0.0096(10) -0.0150(11) C10 0.0225(15) 0.0221(14) 0.0235(16) 0.0013(12) 0.0113(13) 0.0007(12) C11 0.0217(15) 0.0236(14) 0.0195(15) -0.0013(12) 0.0082(12) 0.0010(12) C12 0.0218(15) 0.0200(14) 0.0237(16) -0.0021(12) 0.0100(13) -0.0007(12) O13 0.0259(11) 0.0258(11) 0.0174(11) 0.0017(8) 0.0053(9) -0.0047(9) C14 0.0251(15) 0.0209(14) 0.0189(15) 0.0004(11) 0.0099(13) 0.0009(11) N15 0.0205(12) 0.0226(13) 0.0210(13) 0.0003(10) 0.0094(11) -0.0013(10) C16 0.0285(16) 0.0335(16) 0.0239(16) -0.0001(14) 0.0118(13) 0.0080(14) C17 0.0301(17) 0.0357(17) 0.0183(16) 0.0025(13) 0.0091(14) 0.0085(14) C18 0.0206(14) 0.0199(14) 0.0214(15) 0.0025(12) 0.0100(12) -0.0013(11) C19 0.0259(16) 0.0297(16) 0.0238(16) -0.0032(13) 0.0081(13) 0.0067(13) C20 0.0261(16) 0.0313(16) 0.0198(16) -0.0025(13) 0.0038(13) 0.0033(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 Co O1 1.984(2) 2 ? Co O1 1.984(2) . ? Co N15 2.036(2) . ? Co N15 2.036(2) 2 ? O1 C3 1.270(3) . ? O2 C3 1.257(3) . ? C3 C4 1.501(4) . ? C4 C5 1.391(4) . ? C4 C12 1.390(4) . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C6 C10 1.402(4) . ? C6 C7 1.495(4) . ? C7 O9 1.207(3) . ? C7 O8 1.329(3) . ? O8 H8 1.0087 . ? C10 C11 1.392(4) . ? C10 H10 0.9500 . ? C11 O13 1.370(3) . ? C11 C12 1.392(4) . ? C12 H12 0.9500 . ? O13 C14 1.437(3) . ? C14 C14 1.493(5) 2_554 ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? N15 C20 1.338(4) . ? N15 C16 1.340(4) . ? C16 C17 1.382(4) . ? C16 H16 0.9500 . ? C17 C18 1.382(4) . ? C17 H17 0.9500 . ? C18 C19 1.395(4) . ? C18 C18 1.487(5) 7_546 ? C19 C20 1.384(4) . ? C19 H19 0.9500 . ? C20 H20 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 O1 Co O1 127.57(12) 2 . ? O1 Co N15 98.91(9) 2 . ? O1 Co N15 111.98(8) . . ? O1 Co N15 111.98(8) 2 2 ? O1 Co N15 98.91(9) . 2 ? N15 Co N15 106.41(13) . 2 ? C3 O1 Co 104.51(18) . . ? O2 C3 O1 122.0(3) . . ? O2 C3 C4 120.2(3) . . ? O1 C3 C4 117.7(3) . . ? C5 C4 C12 119.6(3) . . ? C5 C4 C3 120.5(3) . . ? C12 C4 C3 119.9(3) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C10 120.9(3) . . ? C5 C6 C7 117.8(3) . . ? C10 C6 C7 121.3(3) . . ? O9 C7 O8 123.2(3) . . ? O9 C7 C6 123.0(3) . . ? O8 C7 C6 113.8(2) . . ? C7 O8 H8 108.4 . . ? C11 C10 C6 118.7(3) . . ? C11 C10 H10 120.6 . . ? C6 C10 H10 120.6 . . ? O13 C11 C10 124.2(3) . . ? O13 C11 C12 115.4(2) . . ? C10 C11 C12 120.4(3) . . ? C4 C12 C11 120.3(3) . . ? C4 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C11 O13 C14 116.1(2) . . ? O13 C14 C14 108.8(2) . 2_554 ? O13 C14 H14A 109.9 . . ? C14 C14 H14A 109.9 2_554 . ? O13 C14 H14B 109.9 . . ? C14 C14 H14B 109.9 2_554 . ? H14A C14 H14B 108.3 . . ? C20 N15 C16 117.1(2) . . ? C20 N15 Co 123.8(2) . . ? C16 N15 Co 118.50(19) . . ? N15 C16 C17 123.0(3) . . ? N15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 116.8(3) . . ? C17 C18 C18 121.7(3) . 7_546 ? C19 C18 C18 121.5(3) . 7_546 ? C20 C19 C18 119.7(3) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? N15 C20 C19 123.2(3) . . ? N15 C20 H20 118.4 . . ? C19 C20 H20 118.4 . . ? 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 O8 H8 O2 1.01 1.65 2.656(3) 177 4 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.295 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.072 #=========================================END======================== data_ka13 _database_code_depnum_ccdc_archive 'CCDC 779794' #TrackingRef '- Paper2-CIF_b.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 Co2 N2 O12' _chemical_formula_sum 'C30 H26 Co2 N2 O12' _chemical_formula_weight 724.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 13.5405(3) _cell_length_b 21.5306(5) _cell_length_c 13.5016(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.7777(13) _cell_angle_gamma 90.00 _cell_volume 3787.89(15) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4354 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.90 _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7366 _exptl_absorpt_correction_T_max 0.8358 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16647 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.90 _reflns_number_total 7833 _reflns_number_gt 6458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains also severely disordered molecules of the water solvent, which could not mo0deled reliably by discrete atoms. Their contribution to the diffraction patter was subtracted by the Squeeze technique, using the PLATON software (Spek, 2003). The bipyridyl species are also disordered, and some of their atoms were assigned isotropic ADP's. The structure represents a racemic twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.3994P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.465(14) _refine_ls_number_reflns 7833 _refine_ls_number_parameters 484 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 Co1A Co -0.2111(3) 0.0000 0.6422(3) 0.01424(16) Uani 1 2 d S . . Co1B Co -0.0577(3) 0.0000 0.8327(3) 0.01443(16) Uani 1 2 d S . . Co2 Co -0.0270(3) 0.27231(3) 0.2131(3) 0.02416(14) Uani 1 1 d . . . O1 O -0.1263(4) 0.34222(14) 0.2436(4) 0.0344(7) Uani 1 1 d . . . H1A H -0.1871 0.3344 0.2104 0.052 Uiso 1 1 d R . . H1B H -0.1210 0.3433 0.3182 0.052 Uiso 1 1 d R . . O2 O 0.0611(3) 0.19856(15) 0.1800(4) 0.0335(7) Uani 1 1 d . . . H2a H 0.1109 0.2003 0.1535 0.050 Uiso 1 1 d R . . H2b H 0.0880 0.1764 0.2462 0.050 Uiso 1 1 d R . . O3 O -0.0036(3) 0.06546(16) 0.7526(4) 0.0321(8) Uani 1 1 d . . . O4 O -0.1240(3) 0.06640(15) 0.6019(4) 0.0277(7) Uani 1 1 d . . . C5 C -0.0417(4) 0.0847(2) 0.6621(4) 0.0220(9) Uani 1 1 d . . . C6 C 0.0166(4) 0.1347(2) 0.6251(4) 0.0216(9) Uani 1 1 d . . . C7 C 0.0396(4) 0.2064(2) 0.4977(4) 0.0206(8) Uani 1 1 d . . . C8 C -0.0176(4) 0.1600(2) 0.5273(4) 0.0222(8) Uani 1 1 d . . . H8 H -0.0796 0.1458 0.4811 0.027 Uiso 1 1 calc R . . C9 C 0.0066(4) 0.2318(2) 0.3892(4) 0.0291(10) Uani 1 1 d . . . O10 O -0.0696(3) 0.21039(16) 0.3250(4) 0.0324(7) Uani 1 1 d . . . O11 O 0.0606(3) 0.27520(15) 0.3657(4) 0.0313(7) Uani 1 1 d . . . C12 C 0.1295(4) 0.2293(2) 0.5632(4) 0.0230(8) Uani 1 1 d . . . H12 H 0.1656 0.2624 0.5424 0.028 Uiso 1 1 calc R . . C13 C 0.1658(4) 0.2024(2) 0.6609(4) 0.0199(8) Uani 1 1 d . . . C14 C 0.1101(4) 0.1558(2) 0.6919(4) 0.0208(8) Uani 1 1 d . . . H14 H 0.1348 0.1379 0.7584 0.025 Uiso 1 1 calc R . . O15 O 0.2549(3) 0.21818(14) 0.7311(4) 0.0236(6) Uani 1 1 d . . . C16 C 0.3165(4) 0.2659(2) 0.7050(4) 0.0224(9) Uani 1 1 d . . . H16A H 0.2825 0.3068 0.7029 0.027 Uiso 1 1 calc R . . H16B H 0.3278 0.2577 0.6368 0.027 Uiso 1 1 calc R . . C17 C 0.4161(4) 0.2651(2) 0.7870(4) 0.0218(9) Uani 1 1 d . . . H17A H 0.4567 0.3029 0.7833 0.026 Uiso 1 1 calc R . . H17B H 0.4044 0.2627 0.8562 0.026 Uiso 1 1 calc R . . O18 O 0.4674(3) 0.21090(16) 0.7663(4) 0.0332(8) Uani 1 1 d . . . C19 C 0.5656(4) 0.2001(2) 0.8258(4) 0.0244(9) Uani 1 1 d . . . C20 C 0.6151(4) 0.1503(2) 0.7932(4) 0.0275(9) Uani 1 1 d . . . H20 H 0.5809 0.1269 0.7343 0.033 Uiso 1 1 calc R . . C21 C 0.7143(4) 0.1356(2) 0.8475(4) 0.0240(9) Uani 1 1 d . . . C22 C 0.7708(4) 0.0857(2) 0.8100(4) 0.0254(9) Uani 1 1 d . . . O23 O 0.8545(3) 0.06712(17) 0.8684(4) 0.0381(9) Uani 1 1 d . . . O24 O 0.7313(3) 0.06460(16) 0.7213(4) 0.0331(8) Uani 1 1 d . . . C25 C 0.7655(4) 0.17072(19) 0.9349(4) 0.0179(8) Uani 1 1 d . . . H25 H 0.8336 0.1606 0.9726 0.022 Uiso 1 1 calc R . . C26 C 0.7144(4) 0.22033(19) 0.9644(4) 0.0197(8) Uani 1 1 d . . . C27 C 0.7701(4) 0.25890(18) 1.0534(4) 0.0198(8) Uani 1 1 d . . . O28 O 0.7208(3) 0.29555(14) 1.0961(4) 0.0298(7) Uani 1 1 d . . . O29 O 0.8675(3) 0.25391(15) 1.0789(4) 0.0254(6) Uani 1 1 d . . . C30 C 0.6136(4) 0.2348(2) 0.9107(4) 0.0212(9) Uani 1 1 d . . . H30 H 0.5787 0.2682 0.9325 0.025 Uiso 1 1 calc R . . N31A N 0.0715(5) 0.3301(2) 0.1635(5) 0.037(2) Uani 0.50 1 d PG . 1 C32A C 0.1728(5) 0.3351(2) 0.2223(4) 0.0308(19) Uani 0.50 1 d PG . 1 H32A H 0.1989 0.3072 0.2779 0.037 Uiso 0.50 1 calc PR . 1 C33A C 0.2359(4) 0.3808(3) 0.1998(4) 0.0248(17) Uani 0.50 1 d PG . 1 H33A H 0.3052 0.3842 0.2400 0.030 Uiso 0.50 1 calc PR . 1 C34A C 0.1977(4) 0.4215(2) 0.1185(4) 0.0252(18) Uani 0.50 1 d PG . 1 C35A C 0.0964(4) 0.4165(2) 0.0597(4) 0.0260(18) Uani 0.50 1 d PG . 1 H35A H 0.0703 0.4444 0.0042 0.031 Uiso 0.50 1 calc PR . 1 C36A C 0.0333(4) 0.3708(2) 0.0822(4) 0.0102(13) Uani 0.50 1 d PG . 1 H36A H -0.0360 0.3674 0.0421 0.022 Uiso 0.50 1 calc PR . 1 C37A C 0.2705(6) 0.4719(4) 0.0972(7) 0.0266(18) Uani 0.50 1 d P . 1 H37A H 0.3377 0.4611 0.1451 0.032 Uiso 0.50 1 calc PR . 1 H37B H 0.2767 0.4611 0.0279 0.032 Uiso 0.50 1 calc PR . 1 N38 N 0.0673(4) 0.0000 0.9613(4) 0.0184(10) Uani 1 2 d S . . C39A C 0.1401(7) 0.0448(6) 0.9796(7) 0.040(2) Uani 0.58 1 d P . 1 H39A H 0.1320 0.0779 0.9315 0.048 Uiso 0.58 1 calc PR . 1 C40A C 0.2270(7) 0.0457(4) 1.0653(8) 0.047(2) Uani 0.58 1 d P . 1 H40A H 0.2783 0.0767 1.0721 0.057 Uiso 0.58 1 calc PR . 1 C41 C 0.2354(5) 0.0000 1.1393(5) 0.0241(13) Uani 1 2 d S . 1 C42 C 0.3223(5) 0.0000 1.2396(5) 0.0270(13) Uani 1 2 d S . 1 H42A H 0.3155 0.0372 1.2804 0.032 Uiso 0.50 1 calc PR . 1 H42B H 0.3155 -0.0372 1.2804 0.032 Uiso 0.50 1 calc PR . 1 C43 C 0.4290(5) 0.0000 1.2209(5) 0.0334(15) Uani 1 2 d S . 1 H43A H 0.4362 -0.0372 1.1802 0.040 Uiso 0.50 1 calc PR . 1 H43B H 0.4362 0.0372 1.1802 0.040 Uiso 0.50 1 calc PR . 1 C44 C 0.5145(5) 0.0000 1.3219(5) 0.0289(14) Uani 1 2 d S . 1 C45 C 0.5540(4) -0.0542(2) 1.3698(4) 0.0378(11) Uani 1 1 d . . 1 H45 H 0.5274 -0.0929 1.3408 0.045 Uiso 1 1 calc R . 1 C46 C 0.6326(4) -0.0529(2) 1.4603(4) 0.0345(10) Uani 1 1 d . . 1 H46 H 0.6613 -0.0910 1.4902 0.041 Uiso 1 1 calc R . 1 N47 N 0.6689(4) 0.0000 1.5065(4) 0.0169(10) Uani 1 2 d S . 1 N31B N 0.0534(3) 0.3407(2) 0.1473(3) 0.0220(14) Uani 0.50 1 d PG . 2 C32B C 0.1539(3) 0.3547(2) 0.2012(3) 0.0305(19) Uani 0.50 1 d PG . 2 H32B H 0.1847 0.3344 0.2645 0.037 Uiso 0.50 1 calc PR . 2 C33B C 0.2093(3) 0.3983(3) 0.1623(3) 0.034(2) Uani 0.50 1 d PG . 2 H33B H 0.2780 0.4078 0.1992 0.040 Uiso 0.50 1 calc PR . 2 C34B C 0.1642(3) 0.4279(2) 0.0696(3) 0.0244(17) Uani 0.50 1 d PG . 2 C35B C 0.0637(4) 0.4140(3) 0.0157(3) 0.033(2) Uani 0.50 1 d PG . 2 H35B H 0.0329 0.4343 -0.0476 0.040 Uiso 0.50 1 calc PR . 2 C36B C 0.0083(3) 0.3704(3) 0.0546(3) 0.046(2) Uani 0.50 1 d PG . 2 H36B H -0.0603 0.3609 0.0177 0.055 Uiso 0.50 1 calc PR . 2 C37B C 0.2253(7) 0.4758(4) 0.0256(7) 0.035(2) Uani 0.50 1 d P . 2 H37C H 0.2979 0.4645 0.0570 0.042 Uiso 0.50 1 calc PR . 2 H37D H 0.2111 0.4645 -0.0480 0.042 Uiso 0.50 1 calc PR . 2 C39B C 0.0804(7) 0.0446(5) 1.0314(7) 0.032(2) Uani 0.42 1 d P . 2 H39B H 0.0311 0.0771 1.0200 0.038 Uiso 0.42 1 calc PR . 2 C40B C 0.1603(7) 0.0469(5) 1.1192(7) 0.036(3) Uani 0.42 1 d P . 2 H40B H 0.1987 0.0787 1.1614 0.043 Uiso 0.42 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 Co1A 0.0100(3) 0.0193(4) 0.0122(3) 0.000 0.0010(3) 0.000 Co1B 0.0099(3) 0.0183(4) 0.0140(3) 0.000 0.0013(3) 0.000 Co2 0.0193(2) 0.0325(3) 0.0189(2) 0.0002(2) 0.0023(2) -0.0070(2) O1 0.0302(15) 0.0385(17) 0.0294(15) -0.0111(16) -0.0005(13) -0.0052(15) O2 0.0226(14) 0.0393(19) 0.0422(18) 0.0109(15) 0.0151(14) 0.0020(13) O3 0.0347(17) 0.036(2) 0.0235(16) 0.0109(14) 0.0038(14) -0.0114(15) O4 0.0252(15) 0.0291(19) 0.0294(16) 0.0014(14) 0.0086(14) -0.0099(14) C5 0.0188(19) 0.024(2) 0.027(2) 0.0002(18) 0.0118(18) 0.0009(17) C6 0.0201(18) 0.024(2) 0.0220(19) -0.0036(17) 0.0086(16) -0.0084(17) C7 0.0148(17) 0.026(2) 0.0218(18) 0.0061(16) 0.0059(15) -0.0050(15) C8 0.0202(18) 0.024(2) 0.0204(19) -0.0032(16) 0.0030(15) -0.0055(16) C9 0.0222(19) 0.039(3) 0.030(2) 0.0083(19) 0.0129(18) -0.0059(19) O10 0.0260(14) 0.052(2) 0.0166(13) -0.0026(13) 0.0018(12) -0.0191(14) O11 0.0265(16) 0.039(2) 0.0215(15) 0.0091(13) -0.0050(13) -0.0156(13) C12 0.0172(17) 0.026(2) 0.0257(19) 0.0044(18) 0.0059(16) -0.0069(17) C13 0.0154(17) 0.023(2) 0.0207(18) 0.0014(16) 0.0048(15) -0.0036(15) C14 0.0186(18) 0.027(2) 0.0152(18) 0.0063(16) 0.0019(15) -0.0038(16) O15 0.0160(12) 0.0314(17) 0.0217(14) 0.0072(12) 0.0023(11) -0.0064(12) C16 0.0125(16) 0.031(3) 0.0240(19) 0.0033(17) 0.0052(15) -0.0029(17) C17 0.0144(17) 0.028(2) 0.0225(18) -0.0023(17) 0.0045(16) -0.0003(16) O18 0.0136(13) 0.047(2) 0.0346(17) -0.0118(15) -0.0010(12) 0.0075(13) C19 0.0135(17) 0.033(3) 0.0229(19) -0.0054(18) -0.0011(16) 0.0005(17) C20 0.025(2) 0.033(3) 0.025(2) -0.0093(19) 0.0074(17) 0.0014(19) C21 0.0208(19) 0.028(3) 0.025(2) -0.0095(18) 0.0086(17) -0.0039(17) C22 0.0188(19) 0.027(3) 0.032(2) 0.0009(19) 0.0087(18) 0.0064(17) O23 0.0222(16) 0.048(2) 0.0400(19) -0.0149(17) 0.0018(15) 0.0125(15) O24 0.0322(17) 0.035(2) 0.0329(18) -0.0086(15) 0.0104(14) 0.0056(15) C25 0.0132(16) 0.021(2) 0.0200(18) -0.0007(15) 0.0051(14) 0.0047(14) C26 0.0185(18) 0.020(2) 0.0204(18) 0.0025(15) 0.0050(15) -0.0029(15) C27 0.0223(18) 0.019(2) 0.0211(18) -0.0003(15) 0.0113(16) -0.0013(16) O28 0.0203(14) 0.0342(18) 0.0361(16) -0.0112(13) 0.0099(13) -0.0018(12) O29 0.0187(14) 0.0355(17) 0.0211(14) -0.0087(13) 0.0040(12) -0.0023(13) C30 0.0177(18) 0.024(2) 0.0223(19) 0.0010(17) 0.0058(16) 0.0040(17) N31A 0.054(5) 0.037(5) 0.021(4) 0.009(3) 0.013(4) 0.012(4) C32A 0.035(4) 0.028(5) 0.025(4) 0.006(4) 0.001(4) 0.010(4) C33A 0.031(4) 0.026(5) 0.016(4) 0.007(3) 0.004(3) 0.001(3) C34A 0.013(3) 0.057(6) 0.004(3) 0.000(3) 0.001(3) 0.010(3) C35A 0.033(4) 0.027(5) 0.025(4) 0.010(3) 0.020(4) 0.013(4) C36A 0.015(3) 0.006(3) 0.012(3) 0.002(2) 0.009(3) 0.004(2) C37A 0.022(4) 0.031(4) 0.025(4) 0.001(3) 0.003(3) -0.001(3) N38 0.014(2) 0.024(3) 0.013(2) 0.000 -0.0024(18) 0.000 C39A 0.043(5) 0.028(5) 0.035(4) 0.004(4) -0.010(4) 0.000(4) C40A 0.032(4) 0.041(5) 0.054(5) 0.003(4) -0.013(4) -0.005(4) C41 0.017(3) 0.032(4) 0.017(3) 0.000 -0.005(2) 0.000 C42 0.018(3) 0.034(4) 0.026(3) 0.000 0.000(2) 0.000 C43 0.028(3) 0.053(5) 0.016(3) 0.000 0.000(2) 0.000 C44 0.029(3) 0.038(4) 0.020(3) 0.000 0.007(3) 0.000 C45 0.030(2) 0.026(3) 0.042(3) -0.014(2) -0.015(2) -0.0003(19) C46 0.036(2) 0.023(2) 0.031(2) -0.0081(19) -0.0135(19) 0.0053(19) N47 0.013(2) 0.015(3) 0.016(2) 0.000 -0.0058(18) 0.000 N31B 0.019(3) 0.015(3) 0.034(3) -0.008(3) 0.005(3) -0.009(2) C32B 0.017(3) 0.033(5) 0.030(4) 0.012(4) -0.013(3) -0.007(3) C33B 0.028(4) 0.054(6) 0.015(4) 0.001(4) -0.001(3) -0.010(4) C34B 0.024(4) 0.025(4) 0.030(4) -0.007(3) 0.018(3) -0.004(3) C35B 0.044(5) 0.038(5) 0.023(4) -0.003(4) 0.016(4) -0.003(4) C36B 0.028(4) 0.055(7) 0.044(5) 0.006(5) -0.009(4) -0.010(4) C37B 0.039(4) 0.022(4) 0.054(5) 0.001(4) 0.027(4) -0.003(3) C39B 0.025(5) 0.034(6) 0.036(5) -0.011(4) 0.008(4) 0.013(4) C40B 0.019(4) 0.066(8) 0.023(5) -0.016(5) 0.005(4) 0.015(5) _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 Co1A O4 2.021(3) . ? Co1A O4 2.021(3) 2 ? Co1A O24 2.033(3) 2_455 ? Co1A O24 2.033(3) 1_455 ? Co1A N47 2.092(4) 1_454 ? Co1B O23 2.012(3) 2_455 ? Co1B O23 2.012(3) 1_455 ? Co1B O3 2.031(3) . ? Co1B O3 2.031(3) 2 ? Co1B N38 2.069(4) . ? Co2 O29 2.018(3) 1_454 ? Co2 N31A 2.064(3) . ? Co2 O11 2.080(3) . ? Co2 O2 2.105(3) . ? Co2 O1 2.132(3) . ? Co2 N31B 2.162(3) . ? Co2 O10 2.206(3) . ? Co2 C9 2.455(4) . ? O3 C5 1.260(5) . ? O4 C5 1.251(5) . ? C5 C6 1.498(6) . ? C6 C8 1.387(6) . ? C6 C14 1.415(5) . ? C7 C12 1.386(5) . ? C7 C8 1.387(5) . ? C7 C9 1.513(6) . ? C8 H8 0.9500 . ? C9 O10 1.242(5) . ? C9 O11 1.278(5) . ? C12 C13 1.402(6) . ? C12 H12 0.9500 . ? C13 O15 1.359(5) . ? C13 C14 1.387(5) . ? C14 H14 0.9500 . ? O15 C16 1.426(5) . ? C16 C17 1.495(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O18 1.425(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O18 C19 1.373(5) . ? C19 C30 1.376(6) . ? C19 C20 1.398(6) . ? C20 C21 1.380(6) . ? C20 H20 0.9500 . ? C21 C25 1.414(6) . ? C21 C22 1.486(6) . ? C22 O24 1.256(5) . ? C22 O23 1.256(5) . ? O23 Co1B 2.012(3) 1_655 ? O24 Co1A 2.033(3) 1_655 ? C25 C26 1.389(5) . ? C25 H25 0.9500 . ? C26 C30 1.395(5) . ? C26 C27 1.486(5) . ? C27 O28 1.270(5) . ? C27 O29 1.273(5) . ? O29 Co2 2.018(3) 1_656 ? C30 H30 0.9500 . ? N31A C32A 1.3900 . ? N31A C36A 1.3900 . ? C32A C33A 1.3900 . ? C32A H32A 0.9500 . ? C33A C34A 1.3900 . ? C33A H33A 0.9500 . ? C34A C35A 1.3900 . ? C34A C37A 1.544(9) . ? C35A C36A 1.3900 . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? C37A C37A 1.212(17) 2_565 ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? N38 C39B 1.325(9) 2 ? N38 C39B 1.325(9) . ? N38 C39A 1.352(6) . ? N38 C39A 1.352(6) 2 ? C39A C40A 1.408(11) . ? C39A H39A 0.9500 . ? C40A C41 1.384(10) . ? C40A H40A 0.9500 . ? C41 C40A 1.384(10) 2 ? C41 C42 1.534(8) . ? C42 C43 1.533(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.530(8) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.370(6) 2 ? C44 C45 1.370(6) . ? C45 C46 1.385(6) . ? C45 H45 0.9500 . ? C46 N47 1.327(5) . ? C46 H46 0.9500 . ? N47 C46 1.327(5) 2 ? N47 Co1A 2.092(4) 1_656 ? N31B C32B 1.3900 . ? N31B C36B 1.3900 . ? C32B C33B 1.3900 . ? C32B H32B 0.9500 . ? C33B C34B 1.3900 . ? C33B H33B 0.9500 . ? C34B C35B 1.3900 . ? C34B C37B 1.538(8) . ? C35B C36B 1.3900 . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? C39B C40B 1.371(13) . ? C39B H39B 0.9500 . ? C40B H40B 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 O4 Co1A O4 90.07(18) . 2 ? O4 Co1A O24 163.90(13) . 2_455 ? O4 Co1A O24 89.57(12) 2 2_455 ? O4 Co1A O24 89.57(12) . 1_455 ? O4 Co1A O24 163.90(13) 2 1_455 ? O24 Co1A O24 86.36(19) 2_455 1_455 ? O4 Co1A N47 97.76(13) . 1_454 ? O4 Co1A N47 97.76(13) 2 1_454 ? O24 Co1A N47 98.23(13) 2_455 1_454 ? O24 Co1A N47 98.23(13) 1_455 1_454 ? O23 Co1B O23 91.8(2) 2_455 1_455 ? O23 Co1B O3 161.53(13) 2_455 . ? O23 Co1B O3 87.21(14) 1_455 . ? O23 Co1B O3 87.21(14) 2_455 2 ? O23 Co1B O3 161.53(13) 1_455 2 ? O3 Co1B O3 87.9(2) . 2 ? O23 Co1B N38 101.61(13) 2_455 . ? O23 Co1B N38 101.61(13) 1_455 . ? O3 Co1B N38 96.64(13) . . ? O3 Co1B N38 96.65(13) 2 . ? O29 Co2 N31A 100.90(15) 1_454 . ? O29 Co2 O11 165.68(11) 1_454 . ? N31A Co2 O11 93.36(15) . . ? O29 Co2 O2 88.00(12) 1_454 . ? N31A Co2 O2 86.13(16) . . ? O11 Co2 O2 91.68(13) . . ? O29 Co2 O1 88.98(12) 1_454 . ? N31A Co2 O1 97.71(16) . . ? O11 Co2 O1 90.42(13) . . ? O2 Co2 O1 175.51(13) . . ? O29 Co2 N31B 94.43(13) 1_454 . ? N31A Co2 N31B 9.46(16) . . ? O11 Co2 N31B 99.88(13) . . ? O2 Co2 N31B 92.79(14) . . ? O1 Co2 N31B 90.76(14) . . ? O29 Co2 O10 104.08(11) 1_454 . ? N31A Co2 O10 154.00(14) . . ? O11 Co2 O10 61.61(11) . . ? O2 Co2 O10 87.60(12) . . ? O1 Co2 O10 89.90(13) . . ? N31B Co2 O10 161.49(12) . . ? O29 Co2 C9 134.36(13) 1_454 . ? N31A Co2 C9 124.19(16) . . ? O11 Co2 C9 31.35(13) . . ? O2 Co2 C9 88.34(14) . . ? O1 Co2 C9 91.39(14) . . ? N31B Co2 C9 131.18(14) . . ? O10 Co2 C9 30.30(12) . . ? C5 O3 Co1B 129.2(3) . . ? C5 O4 Co1A 122.0(3) . . ? O4 C5 O3 125.8(4) . . ? O4 C5 C6 117.8(4) . . ? O3 C5 C6 116.4(4) . . ? C8 C6 C14 119.3(4) . . ? C8 C6 C5 122.1(4) . . ? C14 C6 C5 118.6(4) . . ? C12 C7 C8 122.3(4) . . ? C12 C7 C9 117.8(3) . . ? C8 C7 C9 119.9(4) . . ? C6 C8 C7 119.3(4) . . ? C6 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? O10 C9 O11 121.4(4) . . ? O10 C9 C7 120.8(4) . . ? O11 C9 C7 117.8(4) . . ? O10 C9 Co2 63.7(2) . . ? O11 C9 Co2 57.9(2) . . ? C7 C9 Co2 173.7(3) . . ? C9 O10 Co2 86.0(2) . . ? C9 O11 Co2 90.8(3) . . ? C7 C12 C13 118.5(4) . . ? C7 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? O15 C13 C14 115.0(3) . . ? O15 C13 C12 124.8(4) . . ? C14 C13 C12 120.2(4) . . ? C13 C14 C6 120.4(3) . . ? C13 C14 H14 119.8 . . ? C6 C14 H14 119.8 . . ? C13 O15 C16 118.4(3) . . ? O15 C16 C17 106.2(3) . . ? O15 C16 H16A 110.5 . . ? C17 C16 H16A 110.5 . . ? O15 C16 H16B 110.5 . . ? C17 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? O18 C17 C16 104.7(3) . . ? O18 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? O18 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? C19 O18 C17 118.0(3) . . ? O18 C19 C30 124.0(4) . . ? O18 C19 C20 114.7(4) . . ? C30 C19 C20 121.4(4) . . ? C21 C20 C19 119.4(4) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C25 120.4(4) . . ? C20 C21 C22 120.1(4) . . ? C25 C21 C22 119.3(4) . . ? O24 C22 O23 124.2(4) . . ? O24 C22 C21 117.4(4) . . ? O23 C22 C21 118.4(4) . . ? C22 O23 Co1B 124.7(3) . 1_655 ? C22 O24 Co1A 128.5(3) . 1_655 ? C26 C25 C21 118.8(3) . . ? C26 C25 H25 120.6 . . ? C21 C25 H25 120.6 . . ? C25 C26 C30 121.1(4) . . ? C25 C26 C27 118.6(3) . . ? C30 C26 C27 120.3(4) . . ? O28 C27 O29 124.3(3) . . ? O28 C27 C26 120.0(3) . . ? O29 C27 C26 115.6(3) . . ? C27 O29 Co2 130.9(2) . 1_656 ? C19 C30 C26 119.0(4) . . ? C19 C30 H30 120.5 . . ? C26 C30 H30 120.5 . . ? C32A N31A C36A 120.0 . . ? C32A N31A Co2 119.1(2) . . ? C36A N31A Co2 120.1(2) . . ? C33A C32A N31A 120.0 . . ? C33A C32A H32A 120.0 . . ? N31A C32A H32A 120.0 . . ? C34A C33A C32A 120.0 . . ? C34A C33A H33A 120.0 . . ? C32A C33A H33A 120.0 . . ? C33A C34A C35A 120.0 . . ? C33A C34A C37A 118.1(4) . . ? C35A C34A C37A 121.9(4) . . ? C36A C35A C34A 120.0 . . ? C36A C35A H35A 120.0 . . ? C34A C35A H35A 120.0 . . ? C35A C36A N31A 120.0 . . ? C35A C36A H36A 120.0 . . ? N31A C36A H36A 120.0 . . ? C37A C37A C34A 134.6(4) 2_565 . ? C37A C37A H37A 103.5 2_565 . ? C34A C37A H37A 103.5 . . ? C37A C37A H37B 103.5 2_565 . ? C34A C37A H37B 103.5 . . ? H37A C37A H37B 105.3 . . ? C39B N38 C39A 115.9(5) . 2 ? C39B N38 Co1B 121.2(4) 2 . ? C39B N38 Co1B 121.2(4) . . ? C39A N38 Co1B 122.8(4) . . ? C39A N38 Co1B 122.8(4) 2 . ? N38 C39A C40A 124.3(6) . . ? N38 C39A H39A 117.8 . . ? C40A C39A H39A 117.8 . . ? C41 C40A C39A 118.0(7) . . ? C41 C40A H40A 121.0 . . ? C39A C40A H40A 121.0 . . ? C40A C41 C42 122.0(5) . . ? C40A C41 C42 122.0(5) 2 . ? C43 C42 C41 112.7(4) . . ? C43 C42 H42A 109.0 . . ? C41 C42 H42A 109.0 . . ? C43 C42 H42B 109.0 . . ? C41 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 111.8(4) . . ? C44 C43 H43A 109.3 . . ? C42 C43 H43A 109.3 . . ? C44 C43 H43B 109.3 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 107.9 . . ? C45 C44 C45 116.7(6) 2 . ? C45 C44 C43 121.7(3) 2 . ? C45 C44 C43 121.7(3) . . ? C44 C45 C46 120.5(4) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? N47 C46 C45 122.0(4) . . ? N47 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? C46 N47 C46 118.2(5) . 2 ? C46 N47 Co1A 120.8(3) . 1_656 ? C46 N47 Co1A 120.8(3) 2 1_656 ? C32B N31B C36B 120.0 . . ? C32B N31B Co2 117.6(2) . . ? C36B N31B Co2 122.4(2) . . ? N31B C32B C33B 120.0 . . ? N31B C32B H32B 120.0 . . ? C33B C32B H32B 120.0 . . ? C34B C33B C32B 120.0 . . ? C34B C33B H33B 120.0 . . ? C32B C33B H33B 120.0 . . ? C35B C34B C33B 120.0 . . ? C35B C34B C37B 119.7(5) . . ? C33B C34B C37B 120.3(5) . . ? C34B C35B C36B 120.0 . . ? C34B C35B H35B 120.0 . . ? C36B C35B H35B 120.0 . . ? C35B C36B N31B 120.0 . . ? C35B C36B H36B 120.0 . . ? N31B C36B H36B 120.0 . . ? C37B C37B H37C 104.2 2_565 . ? C34B C37B H37C 104.2 . . ? C37B C37B H37D 104.2 2_565 . ? C34B C37B H37D 104.2 . . ? H37C C37B H37D 105.5 . . ? N38 C39B C40B 124.3(7) . . ? N38 C39B H39B 117.8 . . ? C40B C39B H39B 117.8 . . ? C39B C40B H40B 136.0 . . ? 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 O1 H1A O28 0.84 1.89 2.650(4) 148 1_454 O2 H2A O28 0.85 1.86 2.703(4) 179 4_454 # 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 0.250 0.000 0.539 479 193 ' ' 2 -0.250 0.500 0.539 479 193 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.918 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.081 #=======================================END==========================