# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2272 data_Codpdo _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Cl2 Co N6 O18' _chemical_formula_weight 894.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 5.5207(3) _cell_length_b 11.8309(5) _cell_length_c 14.9809(6) _cell_angle_alpha 107.813(2) _cell_angle_beta 95.995(2) _cell_angle_gamma 100.588(2) _cell_volume 902.11(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 459 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type 'SORTAV' _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.903 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Kappa CCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.71 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12296 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.85 _reflns_number_total 4299 _reflns_number_gt 3338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'HKL Denzo $ Maxus' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (1990)' _computing_publication_material 'Siemens SHELXL-97' _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^)+(0.1043P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4299 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1628 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Cl1 Cl -0.32591(15) 0.62042(7) 0.29428(6) 0.0484(2) Uani 1 1 d . . . Co1 Co 0.0000 0.0000 0.0000 0.02320(17) Uani 1 2 d S . . O1 O -0.2511(3) -0.11723(16) 0.04846(14) 0.0309(4) Uani 1 1 d . . . O2 O 0.1108(4) 0.0691(3) 0.30266(17) 0.0574(7) Uani 1 1 d . . . O3 O -0.3448(4) 0.1801(3) 0.19922(16) 0.0617(8) Uani 1 1 d . . . O4 O 0.1658(4) 0.0961(2) 0.13844(14) 0.0404(5) Uani 1 1 d . . . H2 H 0.110(7) 0.069(4) 0.191(3) 0.063(11) Uiso 1 1 d . . . H1 H 0.335(8) 0.121(3) 0.167(3) 0.053(10) Uiso 1 1 d . . . O5 O -0.2506(4) 0.11711(18) 0.02372(16) 0.0329(5) Uani 1 1 d . . . H4 H -0.369(6) 0.112(3) -0.002(2) 0.025(8) Uiso 1 1 d . . . H3 H -0.277(7) 0.156(3) 0.096(3) 0.056(10) Uiso 1 1 d . . . O6 O -0.4181(6) 0.4912(2) 0.2547(2) 0.0777(9) Uani 1 1 d . . . O7 O -0.0618(5) 0.6551(3) 0.3025(2) 0.0835(10) Uani 1 1 d . . . O8 O -0.4391(6) 0.6768(2) 0.2336(2) 0.0682(8) Uani 1 1 d . . . O9 O -0.3895(7) 0.6610(3) 0.3866(2) 0.0900(11) Uani 1 1 d . . . N1 N -0.1924(4) -0.22543(19) 0.03685(16) 0.0284(5) Uani 1 1 d . . . N2 N -0.0617(5) 0.0539(2) 0.35482(18) 0.0400(6) Uani 1 1 d . . . N3 N -0.2491(4) 0.2675(2) 0.28186(16) 0.0372(6) Uani 1 1 d . . . C1 C -0.0231(6) -0.2356(3) 0.1036(2) 0.0374(6) Uani 1 1 d . . . H1A H 0.0433 -0.1695 0.1588 0.045 Uiso 1 1 calc R . . C2 C 0.0520(6) -0.3426(3) 0.0906(2) 0.0385(7) Uani 1 1 d . . . H2A H 0.1675 -0.3489 0.1377 0.046 Uiso 1 1 calc R . . C3 C -0.0415(5) -0.4417(2) 0.0085(2) 0.0316(6) Uani 1 1 d . . . C4 C -0.2221(7) -0.4281(3) -0.0566(3) 0.0513(9) Uani 1 1 d . . . H4A H -0.2957 -0.4938 -0.1113 0.062 Uiso 1 1 calc R . . C5 C -0.2944(6) -0.3202(3) -0.0422(2) 0.0451(8) Uani 1 1 d . . . H5A H -0.4142 -0.3128 -0.0872 0.054 Uiso 1 1 calc R . . C6 C -0.2731(6) -0.0331(3) 0.3176(2) 0.0478(8) Uani 1 1 d . . . H6A H -0.3031 -0.0789 0.2533 0.057 Uiso 1 1 calc R . . C7 C -0.4445(6) -0.0550(3) 0.3733(2) 0.0455(8) Uani 1 1 d . . . H7A H -0.5877 -0.1169 0.3464 0.055 Uiso 1 1 calc R . . C8 C -0.4093(5) 0.0133(3) 0.4692(2) 0.0339(6) Uani 1 1 d . . . C9 C -0.1952(6) 0.1062(3) 0.5038(2) 0.0438(7) Uani 1 1 d . . . H9A H -0.1674 0.1569 0.5669 0.053 Uiso 1 1 calc R . . C10 C -0.0241(6) 0.1248(3) 0.4470(2) 0.0449(7) Uani 1 1 d . . . H10A H 0.1196 0.1869 0.4722 0.054 Uiso 1 1 calc R . . C11 C -0.3778(6) 0.2803(3) 0.3541(2) 0.0400(7) Uani 1 1 d . . . H11A H -0.5319 0.2276 0.3461 0.048 Uiso 1 1 calc R . . C12 C -0.2827(5) 0.3707(3) 0.4394(2) 0.0373(7) Uani 1 1 d . . . H12A H -0.3745 0.3792 0.4887 0.045 Uiso 1 1 calc R . . C13 C -0.0518(5) 0.4503(2) 0.45392(19) 0.0301(6) Uani 1 1 d . . . C14 C 0.0763(5) 0.4325(3) 0.3768(2) 0.0379(7) Uani 1 1 d . . . H14A H 0.2321 0.4829 0.3830 0.046 Uiso 1 1 calc R . . C15 C -0.0255(5) 0.3419(3) 0.2926(2) 0.0409(7) Uani 1 1 d . . . H15A H 0.0614 0.3317 0.2418 0.049 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 Cl1 0.0463(5) 0.0495(5) 0.0393(4) 0.0102(3) -0.0049(3) 0.0007(4) Co1 0.0216(3) 0.0232(3) 0.0239(3) 0.00542(18) 0.00403(18) 0.00719(18) O1 0.0304(9) 0.0242(9) 0.0426(11) 0.0127(8) 0.0105(8) 0.0122(7) O2 0.0402(13) 0.0899(18) 0.0454(13) 0.0322(13) 0.0108(10) 0.0044(12) O3 0.0340(12) 0.0819(18) 0.0337(12) -0.0203(11) 0.0049(10) -0.0049(12) O4 0.0299(11) 0.0562(13) 0.0248(10) 0.0052(9) 0.0028(8) 0.0002(9) O5 0.0250(10) 0.0371(11) 0.0394(11) 0.0113(9) 0.0062(9) 0.0160(8) O6 0.092(2) 0.0492(15) 0.0739(19) 0.0152(14) -0.0277(17) 0.0052(14) O7 0.0457(16) 0.113(3) 0.074(2) 0.0192(19) 0.0025(14) -0.0002(16) O8 0.081(2) 0.0490(14) 0.0651(17) 0.0173(13) -0.0157(15) 0.0109(14) O9 0.095(2) 0.104(3) 0.0464(15) 0.0091(16) 0.0190(16) -0.014(2) N1 0.0285(11) 0.0265(11) 0.0352(12) 0.0150(9) 0.0075(9) 0.0095(9) N2 0.0347(13) 0.0506(15) 0.0370(13) 0.0194(12) 0.0062(11) 0.0067(11) N3 0.0291(12) 0.0448(13) 0.0275(12) -0.0008(10) 0.0033(10) 0.0065(10) C1 0.0485(17) 0.0359(15) 0.0289(14) 0.0080(11) 0.0055(13) 0.0180(13) C2 0.0499(17) 0.0383(15) 0.0307(14) 0.0121(12) -0.0014(13) 0.0222(13) C3 0.0357(14) 0.0255(13) 0.0362(14) 0.0144(11) 0.0020(12) 0.0082(11) C4 0.061(2) 0.0253(14) 0.054(2) 0.0027(13) -0.0228(17) 0.0126(14) C5 0.0466(18) 0.0262(13) 0.0530(19) 0.0090(13) -0.0183(15) 0.0073(13) C6 0.0432(17) 0.0547(19) 0.0327(15) 0.0013(14) 0.0071(13) 0.0029(15) C7 0.0404(16) 0.0430(17) 0.0375(16) -0.0012(13) 0.0065(13) -0.0034(14) C8 0.0341(14) 0.0335(14) 0.0333(14) 0.0103(11) 0.0043(12) 0.0079(11) C9 0.0484(18) 0.0405(16) 0.0322(15) 0.0059(12) 0.0033(13) -0.0027(14) C10 0.0411(17) 0.0449(17) 0.0426(17) 0.0162(14) -0.0001(14) -0.0040(14) C11 0.0305(14) 0.0455(17) 0.0350(15) 0.0044(13) 0.0075(12) 0.0009(12) C12 0.0351(15) 0.0408(15) 0.0297(14) 0.0041(12) 0.0096(12) 0.0038(12) C13 0.0286(13) 0.0322(13) 0.0288(13) 0.0077(11) 0.0050(11) 0.0092(11) C14 0.0261(13) 0.0420(16) 0.0370(15) 0.0032(12) 0.0075(12) 0.0027(12) C15 0.0298(14) 0.0515(17) 0.0336(15) 0.0029(13) 0.0104(12) 0.0068(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 Cl1 O7 1.422(3) . ? Cl1 O9 1.423(3) . ? Cl1 O6 1.430(3) . ? Cl1 O8 1.438(3) . ? Co1 O4 2.052(2) 2 ? Co1 O4 2.052(2) . ? Co1 O5 2.1133(19) . ? Co1 O5 2.1133(19) 2 ? Co1 O1 2.1195(18) . ? Co1 O1 2.1195(18) 2 ? O1 N1 1.342(3) . ? O2 N2 1.315(3) . ? O3 N3 1.327(3) . ? N1 C5 1.339(4) . ? N1 C1 1.344(4) . ? N2 C6 1.343(4) . ? N2 C10 1.350(4) . ? N3 C11 1.341(4) . ? N3 C15 1.341(4) . ? C1 C2 1.368(4) . ? C2 C3 1.384(4) . ? C3 C4 1.386(4) . ? C3 C3 1.491(5) 2_545 ? C4 C5 1.368(4) . ? C6 C7 1.365(5) . ? C7 C8 1.389(4) . ? C8 C9 1.386(4) . ? C8 C8 1.485(5) 2_456 ? C9 C10 1.367(4) . ? C11 C12 1.368(4) . ? C12 C13 1.391(4) . ? C13 C14 1.399(4) . ? C13 C13 1.487(5) 2_566 ? C14 C15 1.363(4) . ? 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 O7 Cl1 O9 108.6(2) . . ? O7 Cl1 O6 112.1(2) . . ? O9 Cl1 O6 108.4(2) . . ? O7 Cl1 O8 108.4(2) . . ? O9 Cl1 O8 110.3(2) . . ? O6 Cl1 O8 108.94(17) . . ? O4 Co1 O4 180.00(12) 2 . ? O4 Co1 O5 94.81(9) 2 . ? O4 Co1 O5 85.19(9) . . ? O4 Co1 O5 85.19(9) 2 2 ? O4 Co1 O5 94.81(9) . 2 ? O5 Co1 O5 180.00(15) . 2 ? O4 Co1 O1 90.55(8) 2 . ? O4 Co1 O1 89.45(8) . . ? O5 Co1 O1 86.74(7) . . ? O5 Co1 O1 93.26(7) 2 . ? O4 Co1 O1 89.45(8) 2 2 ? O4 Co1 O1 90.55(8) . 2 ? O5 Co1 O1 93.26(7) . 2 ? O5 Co1 O1 86.74(7) 2 2 ? O1 Co1 O1 180.00(10) . 2 ? N1 O1 Co1 113.12(13) . . ? C5 N1 O1 120.1(2) . . ? C5 N1 C1 120.8(2) . . ? O1 N1 C1 119.1(2) . . ? O2 N2 C6 120.6(3) . . ? O2 N2 C10 119.8(3) . . ? C6 N2 C10 119.7(3) . . ? O3 N3 C11 119.4(2) . . ? O3 N3 C15 120.0(2) . . ? C11 N3 C15 120.6(2) . . ? N1 C1 C2 120.3(3) . . ? C1 C2 C3 121.0(3) . . ? C2 C3 C4 116.5(3) . . ? C2 C3 C3 122.1(3) . 2_545 ? C4 C3 C3 121.4(3) . 2_545 ? C5 C4 C3 121.5(3) . . ? N1 C5 C4 119.9(3) . . ? N2 C6 C7 120.7(3) . . ? C6 C7 C8 121.4(3) . . ? C9 C8 C7 116.1(3) . . ? C9 C8 C8 122.3(3) . 2_456 ? C7 C8 C8 121.5(3) . 2_456 ? C10 C9 C8 121.3(3) . . ? N2 C10 C9 120.7(3) . . ? N3 C11 C12 120.1(3) . . ? C11 C12 C13 121.4(3) . . ? C12 C13 C14 116.4(2) . . ? C12 C13 C13 121.8(3) . 2_566 ? C14 C13 C13 121.8(3) . 2_566 ? C15 C14 C13 120.5(3) . . ? N3 C15 C14 121.0(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.424 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.127 # END data_Nidpdo _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Cl2 N6 Ni O18' _chemical_formula_weight 894.23 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 5.4646(2) _cell_length_b 11.8165(7) _cell_length_c 15.0889(9) _cell_angle_alpha 108.759(2) _cell_angle_beta 95.400(3) _cell_angle_gamma 100.163(3) _cell_volume 896.12(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type 'SORTAV' _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Kappa CCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.71 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8583 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2225 _reflns_number_gt 1900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'HKL Denzo $ Maxus' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (1990)' _computing_publication_material 'Siemens SHELXL-97' _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^)+(0.0626P)^2^+9.1309P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.010(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2225 _refine_ls_number_parameters 264 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2120 _refine_ls_wR_factor_gt 0.2063 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.183 _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 Cl1 Cl -0.3263(5) 0.6226(2) 0.29352(19) 0.0484(8) Uani 1 1 d . . . Ni1 Ni 0.0000 0.0000 0.0000 0.0218(6) Uani 1 2 d S . . O1 O -0.2522(11) -0.1142(5) 0.0474(4) 0.0306(15) Uani 1 1 d . . . O2 O 0.1068(13) 0.0691(8) 0.2997(5) 0.054(2) Uani 1 1 d . . . O3 O -0.3482(12) 0.1851(7) 0.1957(4) 0.052(2) Uani 1 1 d . . . O4 O 0.1593(11) 0.0961(6) 0.1360(4) 0.0393(17) Uani 1 1 d D . . O5 O -0.2437(11) 0.1163(6) 0.0243(4) 0.0302(15) Uani 1 1 d D . . O6 O -0.4197(19) 0.4924(8) 0.2539(7) 0.083(3) Uani 1 1 d . . . O7 O -0.0627(16) 0.6557(10) 0.3000(7) 0.085(3) Uani 1 1 d . . . O8 O -0.4433(17) 0.6771(7) 0.2337(6) 0.068(2) Uani 1 1 d . . . O9 O -0.3885(19) 0.6671(9) 0.3870(6) 0.086(3) Uani 1 1 d . . . N1 N -0.1911(13) -0.2226(7) 0.0362(5) 0.0284(18) Uani 1 1 d . . . N2 N -0.0639(15) 0.0529(8) 0.3521(6) 0.040(2) Uani 1 1 d . . . N3 N -0.2506(14) 0.2716(7) 0.2795(5) 0.038(2) Uani 1 1 d . . . C1 C -0.0259(18) -0.2329(9) 0.1022(7) 0.035(2) Uani 1 1 d . . . H1A H 0.0375 -0.1662 0.1576 0.042 Uiso 1 1 calc R . . C2 C 0.0527(19) -0.3407(9) 0.0897(7) 0.039(2) Uani 1 1 d . . . H2A H 0.1707 -0.3460 0.1360 0.047 Uiso 1 1 calc R . . C3 C -0.0438(17) -0.4407(8) 0.0086(6) 0.031(2) Uani 1 1 d . . . C4 C -0.223(2) -0.4280(9) -0.0567(8) 0.048(3) Uani 1 1 d . . . H4A H -0.2959 -0.4945 -0.1112 0.058 Uiso 1 1 calc R . . C5 C -0.293(2) -0.3188(9) -0.0422(7) 0.043(3) Uani 1 1 d . . . H5A H -0.4121 -0.3114 -0.0871 0.052 Uiso 1 1 calc R . . C6 C -0.280(2) -0.0318(11) 0.3168(8) 0.048(3) Uani 1 1 d . . . H6A H -0.3142 -0.0773 0.2523 0.058 Uiso 1 1 calc R . . C7 C -0.449(2) -0.0526(10) 0.3730(7) 0.047(3) Uani 1 1 d . . . H7A H -0.5950 -0.1133 0.3463 0.057 Uiso 1 1 calc R . . C8 C -0.4112(18) 0.0130(8) 0.4679(6) 0.032(2) Uani 1 1 d . . . C9 C -0.195(2) 0.1052(10) 0.5031(7) 0.046(3) Uani 1 1 d . . . H9A H -0.1655 0.1548 0.5666 0.055 Uiso 1 1 calc R . . C10 C -0.022(2) 0.1247(9) 0.4458(7) 0.042(3) Uani 1 1 d . . . H10A H 0.1229 0.1866 0.4708 0.050 Uiso 1 1 calc R . . C11 C -0.3784(17) 0.2806(9) 0.3516(6) 0.036(2) Uani 1 1 d . . . H11A H -0.5319 0.2267 0.3433 0.043 Uiso 1 1 calc R . . C12 C -0.2812(18) 0.3708(8) 0.4392(6) 0.034(2) Uani 1 1 d . . . H12A H -0.3716 0.3781 0.4892 0.040 Uiso 1 1 calc R . . C13 C -0.0518(16) 0.4497(8) 0.4526(6) 0.025(2) Uani 1 1 d . . . C14 C 0.0744(17) 0.4343(9) 0.3771(7) 0.039(2) Uani 1 1 d . . . H14A H 0.2330 0.4840 0.3852 0.046 Uiso 1 1 calc R . . C15 C -0.0278(15) 0.3462(9) 0.2880(6) 0.038(3) Uani 1 1 d . . . H15A H 0.0562 0.3397 0.2364 0.046 Uiso 1 1 calc R . . H2 H 0.1085 0.0705 0.1894 0.06(4) Uiso 1 1 d RD . . H1 H 0.3329 0.1226 0.1655 0.10(5) Uiso 1 1 d RD . . H4 H -0.3704 0.1132 -0.0038 0.04(3) Uiso 1 1 d RD . . H3 H -0.2784 0.1581 0.0942 0.29(15) Uiso 1 1 d RD . . 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 Cl1 0.0450(17) 0.0483(17) 0.0407(16) 0.0112(13) -0.0073(12) -0.0026(13) Ni1 0.0200(9) 0.0213(9) 0.0235(9) 0.0061(7) 0.0035(6) 0.0059(6) O1 0.032(4) 0.021(3) 0.044(4) 0.014(3) 0.013(3) 0.011(3) O2 0.040(4) 0.081(6) 0.041(4) 0.029(4) 0.010(3) -0.001(4) O3 0.039(4) 0.061(5) 0.026(4) -0.018(4) 0.000(3) -0.003(4) O4 0.028(4) 0.054(4) 0.022(3) 0.002(3) 0.001(3) -0.004(3) O5 0.024(4) 0.032(4) 0.036(4) 0.010(3) 0.005(3) 0.013(3) O6 0.098(7) 0.050(5) 0.077(6) 0.010(5) -0.035(5) 0.006(5) O7 0.042(5) 0.116(8) 0.079(7) 0.022(6) 0.004(4) -0.001(5) O8 0.084(6) 0.051(5) 0.055(5) 0.013(4) -0.016(5) 0.004(4) O9 0.091(7) 0.093(7) 0.049(5) 0.009(5) 0.018(5) -0.018(6) N1 0.025(4) 0.031(5) 0.031(4) 0.012(4) 0.007(3) 0.008(3) N2 0.028(5) 0.060(6) 0.037(5) 0.029(5) 0.005(4) 0.006(4) N3 0.028(5) 0.043(5) 0.028(5) -0.002(4) -0.002(4) 0.004(4) C1 0.046(6) 0.034(5) 0.024(5) 0.006(4) 0.000(4) 0.016(5) C2 0.051(6) 0.035(6) 0.033(6) 0.013(5) -0.005(5) 0.018(5) C3 0.034(5) 0.024(5) 0.034(5) 0.011(4) -0.001(4) 0.006(4) C4 0.048(7) 0.026(6) 0.058(7) 0.004(5) -0.015(5) 0.006(5) C5 0.047(6) 0.029(6) 0.048(7) 0.015(5) -0.018(5) 0.005(5) C6 0.039(7) 0.060(7) 0.036(6) 0.007(5) 0.007(5) 0.005(6) C7 0.043(6) 0.042(6) 0.042(7) 0.003(5) 0.007(5) -0.006(5) C8 0.037(6) 0.024(5) 0.026(5) 0.003(4) 0.000(4) -0.001(4) C9 0.056(7) 0.043(6) 0.031(6) 0.008(5) 0.002(5) -0.002(5) C10 0.043(6) 0.039(6) 0.035(6) 0.016(5) -0.004(5) -0.010(5) C11 0.022(5) 0.049(6) 0.026(5) 0.004(5) 0.004(4) 0.001(4) C12 0.035(6) 0.037(6) 0.025(5) 0.007(4) 0.004(4) 0.006(5) C13 0.028(5) 0.022(5) 0.028(5) 0.013(4) -0.001(4) 0.005(4) C14 0.021(5) 0.045(6) 0.040(6) 0.007(5) 0.002(4) -0.002(4) C15 0.022(5) 0.056(6) 0.023(5) -0.001(5) 0.001(4) 0.007(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 Cl1 O7 1.410(9) . ? Cl1 O8 1.431(8) . ? Cl1 O9 1.434(9) . ? Cl1 O6 1.435(9) . ? Ni1 O4 2.019(6) . ? Ni1 O4 2.019(6) 2 ? Ni1 O5 2.052(6) 2 ? Ni1 O5 2.052(6) . ? Ni1 O1 2.093(6) 2 ? Ni1 O1 2.093(6) . ? O1 N1 1.343(9) . ? O2 N2 1.305(10) . ? O3 N3 1.333(10) . ? N1 C1 1.330(12) . ? N1 C5 1.338(12) . ? N2 C6 1.342(13) . ? N2 C10 1.368(13) . ? N3 C11 1.334(12) . ? N3 C15 1.340(12) . ? C1 C2 1.377(13) . ? C2 C3 1.379(13) . ? C3 C4 1.384(14) . ? C3 C3 1.512(17) 2_545 ? C4 C5 1.367(14) . ? C6 C7 1.355(15) . ? C7 C8 1.366(13) . ? C8 C9 1.387(14) . ? C8 C8 1.496(19) 2_456 ? C9 C10 1.377(15) . ? C11 C12 1.388(13) . ? C12 C13 1.378(13) . ? C13 C14 1.366(13) . ? C13 C13 1.515(17) 2_566 ? C14 C15 1.399(13) . ? 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 O7 Cl1 O8 108.9(6) . . ? O7 Cl1 O9 108.4(6) . . ? O8 Cl1 O9 110.0(6) . . ? O7 Cl1 O6 112.0(6) . . ? O8 Cl1 O6 108.2(5) . . ? O9 Cl1 O6 109.2(6) . . ? O4 Ni1 O4 180.0(2) . 2 ? O4 Ni1 O5 95.5(3) . 2 ? O4 Ni1 O5 84.5(3) 2 2 ? O4 Ni1 O5 84.5(3) . . ? O4 Ni1 O5 95.5(3) 2 . ? O5 Ni1 O5 180.0(5) 2 . ? O4 Ni1 O1 90.7(2) . 2 ? O4 Ni1 O1 89.3(2) 2 2 ? O5 Ni1 O1 86.8(2) 2 2 ? O5 Ni1 O1 93.2(2) . 2 ? O4 Ni1 O1 89.3(2) . . ? O4 Ni1 O1 90.7(2) 2 . ? O5 Ni1 O1 93.2(2) 2 . ? O5 Ni1 O1 86.8(2) . . ? O1 Ni1 O1 180.0(3) 2 . ? N1 O1 Ni1 112.9(5) . . ? C1 N1 C5 120.5(8) . . ? C1 N1 O1 119.8(7) . . ? C5 N1 O1 119.7(7) . . ? O2 N2 C6 122.1(9) . . ? O2 N2 C10 119.1(8) . . ? C6 N2 C10 118.9(9) . . ? O3 N3 C11 118.8(8) . . ? O3 N3 C15 118.7(7) . . ? C11 N3 C15 122.5(8) . . ? N1 C1 C2 121.0(9) . . ? C1 C2 C3 119.9(9) . . ? C2 C3 C4 117.4(8) . . ? C2 C3 C3 121.3(10) . 2_545 ? C4 C3 C3 121.4(10) . 2_545 ? C5 C4 C3 120.8(9) . . ? N1 C5 C4 120.3(9) . . ? N2 C6 C7 121.5(10) . . ? C6 C7 C8 121.9(10) . . ? C7 C8 C9 116.4(9) . . ? C7 C8 C8 122.7(10) . 2_456 ? C9 C8 C8 120.9(10) . 2_456 ? C10 C9 C8 121.3(9) . . ? N2 C10 C9 119.8(9) . . ? N3 C11 C12 119.7(9) . . ? C13 C12 C11 120.6(9) . . ? C14 C13 C12 117.4(8) . . ? C14 C13 C13 121.9(10) . 2_566 ? C12 C13 C13 120.7(10) . 2_566 ? C13 C14 C15 122.0(9) . . ? N3 C15 C14 117.9(8) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.620 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.119 # END data_Cudpdo _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Cl2 Cu N6 O18' _chemical_formula_weight 899.06 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' '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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 5.3540(2) _cell_length_b 11.8921(4) _cell_length_c 15.2705(6) _cell_angle_alpha 110.739(2) _cell_angle_beta 94.0425(19) _cell_angle_gamma 99.2350(18) _cell_volume 888.91(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light green ' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 461 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type 'SORTAV' _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Kappa CCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.71 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17201 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 27.90 _reflns_number_total 4157 _reflns_number_gt 3381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Kappa CCD' _computing_cell_refinement 'Denzo Scalepack' _computing_data_reduction 'Denzo Maxus' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (1990)' _computing_publication_material 'Siemens SHELXL-97' _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^)+(0.0551P)^2^+0.5393P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4157 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Cl1 Cl -0.34252(13) 0.63312(6) 0.29606(5) 0.04624(18) Uani 1 1 d . . . Cu1 Cu 0.0000 0.0000 0.0000 0.02608(12) Uani 1 2 d S . . O1 O -0.3005(3) -0.11986(14) 0.05868(12) 0.0355(4) Uani 1 1 d . . . O2 O 0.0866(4) 0.0862(2) 0.29537(14) 0.0601(6) Uani 1 1 d . . . O3 O -0.3648(4) 0.2037(2) 0.18927(13) 0.0598(6) Uani 1 1 d . . . O4 O 0.1556(4) 0.0906(2) 0.13074(13) 0.0441(5) Uani 1 1 d . . . H2 H 0.109(8) 0.068(4) 0.165(3) 0.070(13) Uiso 1 1 d . . . H1 H 0.308(8) 0.126(3) 0.154(3) 0.070(11) Uiso 1 1 d . . . O5 O -0.2261(3) 0.11942(16) 0.02119(14) 0.0352(4) Uani 1 1 d . . . H4 H -0.376(7) 0.109(3) -0.016(3) 0.068(11) Uiso 1 1 d . . . H3 H -0.240(5) 0.145(3) 0.077(2) 0.037(8) Uiso 1 1 d . . . O6 O -0.4373(5) 0.5029(2) 0.25560(18) 0.0724(7) Uani 1 1 d . . . O7 O -0.0740(5) 0.6622(3) 0.3006(2) 0.0839(8) Uani 1 1 d . . . O8 O -0.4597(5) 0.6873(2) 0.23817(17) 0.0681(7) Uani 1 1 d . . . O9 O -0.4085(6) 0.6795(3) 0.38953(17) 0.0865(9) Uani 1 1 d . . . N1 N -0.2284(4) -0.22666(17) 0.04383(14) 0.0301(4) Uani 1 1 d . . . N2 N -0.0809(4) 0.0663(2) 0.34991(15) 0.0393(5) Uani 1 1 d . . . N3 N -0.2622(4) 0.2837(2) 0.27470(14) 0.0369(5) Uani 1 1 d . . . C1 C -0.0519(5) -0.2338(2) 0.10727(17) 0.0388(6) Uani 1 1 d . . . H1A H 0.0099 -0.1662 0.1626 0.047 Uiso 1 1 calc R . . C2 C 0.0389(5) -0.3401(2) 0.09152(17) 0.0398(6) Uani 1 1 d . . . H2A H 0.1612 -0.3433 0.1365 0.048 Uiso 1 1 calc R . . C3 C -0.0490(5) -0.4425(2) 0.00963(17) 0.0320(5) Uani 1 1 d . . . C4 C -0.2350(6) -0.4318(2) -0.0536(2) 0.0473(7) Uani 1 1 d . . . H4A H -0.3019 -0.4986 -0.1090 0.057 Uiso 1 1 calc R . . C5 C -0.3220(5) -0.3242(2) -0.0357(2) 0.0441(6) Uani 1 1 d . . . H5A H -0.4463 -0.3189 -0.0790 0.053 Uiso 1 1 calc R . . C6 C -0.3015(5) -0.0151(3) 0.31290(19) 0.0437(6) Uani 1 1 d . . . H6A H -0.3424 -0.0538 0.2476 0.052 Uiso 1 1 calc R . . C7 C -0.4659(5) -0.0416(2) 0.37043(18) 0.0413(6) Uani 1 1 d . . . H7A H -0.6160 -0.0995 0.3435 0.050 Uiso 1 1 calc R . . C8 C -0.4149(5) 0.0160(2) 0.46847(17) 0.0343(5) Uani 1 1 d . . . C9 C -0.1918(5) 0.1049(3) 0.50333(18) 0.0444(6) Uani 1 1 d . . . H9A H -0.1535 0.1496 0.5680 0.053 Uiso 1 1 calc R . . C10 C -0.0280(5) 0.1279(3) 0.44434(19) 0.0462(7) Uani 1 1 d . . . H10A H 0.1217 0.1866 0.4695 0.055 Uiso 1 1 calc R . . C11 C -0.3884(5) 0.2894(2) 0.34871(18) 0.0391(6) Uani 1 1 d . . . H11A H -0.5438 0.2363 0.3400 0.047 Uiso 1 1 calc R . . C12 C -0.2881(5) 0.3736(2) 0.43699(17) 0.0368(5) Uani 1 1 d . . . H12A H -0.3777 0.3772 0.4876 0.044 Uiso 1 1 calc R . . C13 C -0.0544(4) 0.4541(2) 0.45261(15) 0.0300(5) Uani 1 1 d . . . C14 C 0.0687(5) 0.4432(2) 0.37388(17) 0.0369(5) Uani 1 1 d . . . H14A H 0.2253 0.4945 0.3806 0.044 Uiso 1 1 calc R . . C15 C -0.0365(5) 0.3582(3) 0.28624(18) 0.0413(6) Uani 1 1 d . . . H15A H 0.0497 0.3522 0.2345 0.050 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 Cl1 0.0419(4) 0.0496(4) 0.0387(3) 0.0123(3) -0.0046(3) -0.0010(3) Cu1 0.0221(2) 0.0293(2) 0.0239(2) 0.00597(15) 0.00187(14) 0.00635(15) O1 0.0339(9) 0.0280(8) 0.0452(10) 0.0125(7) 0.0031(7) 0.0113(7) O2 0.0438(11) 0.0943(17) 0.0418(11) 0.0337(11) 0.0067(9) -0.0071(11) O3 0.0335(10) 0.0805(15) 0.0290(9) -0.0148(9) 0.0023(8) -0.0083(10) O4 0.0301(10) 0.0638(13) 0.0259(9) 0.0096(9) 0.0015(8) -0.0079(9) O5 0.0319(9) 0.0414(10) 0.0337(10) 0.0119(8) 0.0072(8) 0.0144(7) O6 0.0814(17) 0.0484(13) 0.0738(16) 0.0160(12) -0.0207(13) 0.0041(12) O7 0.0410(13) 0.118(2) 0.0741(17) 0.0251(16) -0.0008(12) -0.0064(14) O8 0.0769(16) 0.0556(13) 0.0663(15) 0.0224(11) -0.0150(12) 0.0087(12) O9 0.0885(19) 0.104(2) 0.0417(13) 0.0116(13) 0.0125(13) -0.0170(16) N1 0.0288(10) 0.0282(9) 0.0362(10) 0.0142(8) 0.0051(8) 0.0081(8) N2 0.0345(11) 0.0483(12) 0.0361(11) 0.0198(10) 0.0027(9) 0.0024(9) N3 0.0262(10) 0.0437(12) 0.0283(10) 0.0000(9) 0.0010(8) 0.0042(9) C1 0.0479(15) 0.0387(13) 0.0280(12) 0.0071(10) 0.0005(10) 0.0179(11) C2 0.0474(15) 0.0415(14) 0.0317(12) 0.0125(11) -0.0031(11) 0.0187(12) C3 0.0348(12) 0.0297(11) 0.0346(12) 0.0154(10) 0.0035(10) 0.0078(9) C4 0.0523(16) 0.0281(12) 0.0499(16) 0.0058(11) -0.0201(13) 0.0073(11) C5 0.0433(15) 0.0322(12) 0.0505(15) 0.0115(12) -0.0156(12) 0.0082(11) C6 0.0405(14) 0.0486(15) 0.0319(13) 0.0063(11) 0.0033(11) 0.0018(12) C7 0.0347(13) 0.0416(14) 0.0352(13) 0.0037(11) 0.0024(10) -0.0012(11) C8 0.0344(12) 0.0321(12) 0.0332(12) 0.0096(10) 0.0029(10) 0.0049(10) C9 0.0488(15) 0.0439(14) 0.0298(12) 0.0089(11) -0.0013(11) -0.0069(12) C10 0.0431(15) 0.0505(16) 0.0371(14) 0.0168(12) -0.0039(11) -0.0103(12) C11 0.0302(12) 0.0441(14) 0.0342(13) 0.0074(11) 0.0042(10) -0.0005(10) C12 0.0325(12) 0.0416(13) 0.0288(11) 0.0079(10) 0.0053(10) -0.0021(10) C13 0.0274(11) 0.0318(11) 0.0274(11) 0.0076(10) 0.0023(9) 0.0050(9) C14 0.0267(11) 0.0429(13) 0.0318(12) 0.0061(10) 0.0036(9) -0.0006(10) C15 0.0289(12) 0.0546(16) 0.0305(12) 0.0061(11) 0.0074(10) 0.0020(11) _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 Cl1 O7 1.414(2) . ? Cl1 O9 1.429(2) . ? Cl1 O8 1.430(2) . ? Cl1 O6 1.436(2) . ? Cu1 O4 1.9480(18) . ? Cu1 O4 1.9480(18) 2 ? Cu1 O5 1.9669(17) 2 ? Cu1 O5 1.9669(17) . ? Cu1 O1 2.4072(17) 2 ? Cu1 O1 2.4072(17) . ? O1 N1 1.334(2) . ? O2 N2 1.315(3) . ? O3 N3 1.327(3) . ? N1 C1 1.340(3) . ? N1 C5 1.342(3) . ? N2 C6 1.343(3) . ? N2 C10 1.350(3) . ? N3 C15 1.339(3) . ? N3 C11 1.344(3) . ? C1 C2 1.374(3) . ? C2 C3 1.387(3) . ? C3 C4 1.390(3) . ? C3 C3 1.483(4) 2_545 ? C4 C5 1.375(4) . ? C6 C7 1.364(4) . ? C7 C8 1.393(3) . ? C8 C9 1.392(4) . ? C8 C8 1.474(5) 2_456 ? C9 C10 1.365(4) . ? C11 C12 1.370(3) . ? C12 C13 1.396(3) . ? C13 C14 1.388(3) . ? C13 C13 1.478(4) 2_566 ? C14 C15 1.372(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Cl1 O9 108.95(17) . . ? O7 Cl1 O8 109.34(18) . . ? O9 Cl1 O8 110.17(19) . . ? O7 Cl1 O6 111.47(18) . . ? O9 Cl1 O6 108.76(18) . . ? O8 Cl1 O6 108.15(14) . . ? O4 Cu1 O4 180.00(7) . 2 ? O4 Cu1 O5 93.16(9) . 2 ? O4 Cu1 O5 86.84(9) 2 2 ? O4 Cu1 O5 86.84(9) . . ? O4 Cu1 O5 93.16(9) 2 . ? O5 Cu1 O5 180.00(9) 2 . ? O4 Cu1 O1 92.70(8) . 2 ? O4 Cu1 O1 87.30(8) 2 2 ? O5 Cu1 O1 88.44(6) 2 2 ? O5 Cu1 O1 91.56(6) . 2 ? O4 Cu1 O1 87.30(8) . . ? O4 Cu1 O1 92.70(8) 2 . ? O5 Cu1 O1 91.56(6) 2 . ? O5 Cu1 O1 88.44(6) . . ? O1 Cu1 O1 180.00(8) 2 . ? N1 O1 Cu1 107.87(13) . . ? O1 N1 C1 119.09(19) . . ? O1 N1 C5 120.6(2) . . ? C1 N1 C5 120.3(2) . . ? O2 N2 C6 120.8(2) . . ? O2 N2 C10 119.3(2) . . ? C6 N2 C10 119.9(2) . . ? O3 N3 C15 120.0(2) . . ? O3 N3 C11 119.3(2) . . ? C15 N3 C11 120.8(2) . . ? N1 C1 C2 120.8(2) . . ? C1 C2 C3 121.0(2) . . ? C2 C3 C4 116.4(2) . . ? C2 C3 C3 122.0(3) . 2_545 ? C4 C3 C3 121.6(3) . 2_545 ? C5 C4 C3 121.2(2) . . ? N1 C5 C4 120.4(2) . . ? N2 C6 C7 120.4(2) . . ? C6 C7 C8 121.8(2) . . ? C9 C8 C7 115.8(2) . . ? C9 C8 C8 122.0(3) . 2_456 ? C7 C8 C8 122.3(3) . 2_456 ? C10 C9 C8 121.2(2) . . ? N2 C10 C9 120.8(2) . . ? N3 C11 C12 120.0(2) . . ? C11 C12 C13 121.5(2) . . ? C14 C13 C12 116.1(2) . . ? C14 C13 C13 122.0(3) . 2_566 ? C12 C13 C13 121.9(3) . 2_566 ? C15 C14 C13 121.2(2) . . ? N3 C15 C14 120.5(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.666 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.066 # END data_Zndpdo _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Cl2 N6 O18 Zn' _chemical_formula_weight 900.89 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' 'Cl' 'Cl' 0.1484 0.1585 '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 5.4888(2) _cell_length_b 11.8617(6) _cell_length_c 15.0146(6) _cell_angle_alpha 108.161(2) _cell_angle_beta 95.599(3) _cell_angle_gamma 100.334(2) _cell_volume 901.39(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type 'SORTAV' _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.864 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'NOINIUS KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.71 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12472 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.87 _reflns_number_total 4300 _reflns_number_gt 3400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'HKL Denzo & Maxus' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (1990)' _computing_publication_material 'Siemens SHELXL-97' _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^)+(0.0642P)^2^+0.7300P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4300 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Cl1 Cl -0.32794(17) 0.62354(9) 0.29444(6) 0.0515(2) Uani 1 1 d . . . Zn1 Zn 0.0000 0.0000 0.0000 0.02819(15) Uani 1 2 d S . . O1 O -0.2575(4) -0.11825(19) 0.04848(16) 0.0341(5) Uani 1 1 d . . . O2 O 0.1092(5) 0.0713(3) 0.3022(2) 0.0666(8) Uani 1 1 d . . . O3 O -0.3475(5) 0.1869(3) 0.19686(18) 0.0702(10) Uani 1 1 d . . . O4 O 0.1652(5) 0.0952(3) 0.13733(17) 0.0468(6) Uani 1 1 d . . . H2 H 0.109(10) 0.072(5) 0.178(4) 0.076(16) Uiso 1 1 d . . . H1 H 0.336(10) 0.126(4) 0.161(3) 0.072(14) Uiso 1 1 d . . . O5 O -0.2470(4) 0.1172(2) 0.02289(18) 0.0366(5) Uani 1 1 d . . . H4 H -0.383(9) 0.115(4) -0.007(3) 0.060(13) Uiso 1 1 d . . . H3 H -0.250(7) 0.154(4) 0.084(3) 0.051(11) Uiso 1 1 d . . . O6 O -0.4195(7) 0.4945(3) 0.2551(2) 0.0809(10) Uani 1 1 d . . . O7 O -0.0633(6) 0.6571(4) 0.3017(3) 0.0861(11) Uani 1 1 d . . . O8 O -0.4424(6) 0.6784(3) 0.2338(2) 0.0713(9) Uani 1 1 d . . . O9 O -0.3919(7) 0.6650(4) 0.3871(2) 0.0913(12) Uani 1 1 d . . . N1 N -0.1974(4) -0.2261(2) 0.03711(18) 0.0312(5) Uani 1 1 d . . . N2 N -0.0627(5) 0.0559(3) 0.3544(2) 0.0466(7) Uani 1 1 d . . . N3 N -0.2501(5) 0.2721(3) 0.27989(19) 0.0429(7) Uani 1 1 d . . . C1 C -0.0285(7) -0.2358(3) 0.1029(2) 0.0414(7) Uani 1 1 d . . . H1A H 0.0366 -0.1696 0.1580 0.050 Uiso 1 1 calc R . . C2 C 0.0500(6) -0.3423(3) 0.0901(2) 0.0409(8) Uani 1 1 d . . . H2A H 0.1676 -0.3477 0.1367 0.049 Uiso 1 1 calc R . . C3 C -0.0434(6) -0.4420(3) 0.0088(2) 0.0345(6) Uani 1 1 d . . . C4 C -0.2263(7) -0.4293(3) -0.0565(3) 0.0517(10) Uani 1 1 d . . . H4A H -0.3007 -0.4950 -0.1109 0.062 Uiso 1 1 calc R . . C5 C -0.2971(6) -0.3205(3) -0.0410(3) 0.0457(8) Uani 1 1 d . . . H5A H -0.4165 -0.3127 -0.0858 0.055 Uiso 1 1 calc R . . C6 C -0.2744(7) -0.0295(4) 0.3174(3) 0.0538(10) Uani 1 1 d . . . H6A H -0.3055 -0.0734 0.2526 0.065 Uiso 1 1 calc R . . C7 C -0.4459(7) -0.0535(4) 0.3727(3) 0.0503(9) Uani 1 1 d . . . H7A H -0.5887 -0.1154 0.3456 0.060 Uiso 1 1 calc R . . C8 C -0.4101(6) 0.0132(3) 0.4689(2) 0.0391(7) Uani 1 1 d . . . C9 C -0.1952(7) 0.1056(4) 0.5039(3) 0.0485(8) Uani 1 1 d . . . H9A H -0.1669 0.1552 0.5673 0.058 Uiso 1 1 calc R . . C10 C -0.0238(7) 0.1251(4) 0.4466(3) 0.0516(9) Uani 1 1 d . . . H10A H 0.1205 0.1866 0.4718 0.062 Uiso 1 1 calc R . . C11 C -0.3792(6) 0.2829(3) 0.3527(2) 0.0436(8) Uani 1 1 d . . . H11A H -0.5336 0.2303 0.3446 0.052 Uiso 1 1 calc R . . C12 C -0.2826(6) 0.3716(3) 0.4392(2) 0.0408(7) Uani 1 1 d . . . H12A H -0.3739 0.3787 0.4890 0.049 Uiso 1 1 calc R . . C13 C -0.0520(5) 0.4511(3) 0.4540(2) 0.0319(6) Uani 1 1 d . . . C14 C 0.0765(6) 0.4356(3) 0.3766(2) 0.0409(7) Uani 1 1 d . . . H14A H 0.2320 0.4864 0.3830 0.049 Uiso 1 1 calc R . . C15 C -0.0253(6) 0.3461(4) 0.2914(2) 0.0458(8) Uani 1 1 d . . . H15A H 0.0629 0.3365 0.2407 0.055 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 Cl1 0.0473(5) 0.0547(6) 0.0421(5) 0.0120(4) -0.0048(4) -0.0009(4) Zn1 0.0248(2) 0.0280(3) 0.0298(3) 0.00619(19) 0.00347(17) 0.00764(18) O1 0.0325(10) 0.0268(11) 0.0455(12) 0.0125(9) 0.0084(9) 0.0110(9) O2 0.0494(15) 0.100(3) 0.0521(16) 0.0357(16) 0.0102(12) 0.0017(15) O3 0.0383(13) 0.095(2) 0.0356(14) -0.0239(14) 0.0049(10) -0.0078(14) O4 0.0325(12) 0.0648(18) 0.0304(12) 0.0068(11) 0.0029(9) -0.0033(11) O5 0.0302(11) 0.0421(13) 0.0381(13) 0.0101(10) 0.0070(9) 0.0151(10) O6 0.093(2) 0.0510(19) 0.078(2) 0.0137(16) -0.0289(18) 0.0033(17) O7 0.0466(16) 0.115(3) 0.077(2) 0.020(2) 0.0011(15) -0.0046(18) O8 0.083(2) 0.0555(19) 0.065(2) 0.0172(15) -0.0123(16) 0.0088(16) O9 0.090(2) 0.113(3) 0.0480(18) 0.0140(19) 0.0171(16) -0.015(2) N1 0.0307(12) 0.0300(13) 0.0362(14) 0.0136(11) 0.0074(10) 0.0092(10) N2 0.0409(15) 0.058(2) 0.0439(17) 0.0232(14) 0.0045(12) 0.0077(14) N3 0.0296(13) 0.0518(18) 0.0325(14) -0.0037(12) 0.0024(10) 0.0052(12) C1 0.0542(19) 0.0396(18) 0.0294(16) 0.0071(13) 0.0021(13) 0.0188(16) C2 0.0507(19) 0.0427(19) 0.0322(17) 0.0135(14) -0.0020(14) 0.0201(16) C3 0.0370(15) 0.0310(16) 0.0370(17) 0.0133(13) 0.0020(12) 0.0098(13) C4 0.057(2) 0.0288(17) 0.056(2) 0.0049(15) -0.0209(17) 0.0100(16) C5 0.0436(18) 0.0334(17) 0.053(2) 0.0120(15) -0.0172(15) 0.0081(14) C6 0.0447(19) 0.059(2) 0.040(2) -0.0011(17) 0.0026(15) 0.0015(18) C7 0.0419(18) 0.049(2) 0.043(2) -0.0011(16) 0.0051(15) -0.0004(16) C8 0.0386(16) 0.0359(17) 0.0391(18) 0.0085(14) 0.0025(13) 0.0083(14) C9 0.051(2) 0.047(2) 0.0385(19) 0.0108(16) 0.0014(15) -0.0031(16) C10 0.0456(19) 0.053(2) 0.047(2) 0.0181(17) -0.0051(15) -0.0090(17) C11 0.0325(15) 0.052(2) 0.0333(17) 0.0022(15) 0.0055(12) -0.0009(14) C12 0.0369(16) 0.047(2) 0.0320(16) 0.0072(14) 0.0075(12) 0.0023(14) C13 0.0297(14) 0.0355(16) 0.0274(15) 0.0065(12) 0.0028(11) 0.0078(12) C14 0.0297(14) 0.047(2) 0.0370(17) 0.0054(14) 0.0062(12) 0.0020(14) C15 0.0316(15) 0.061(2) 0.0335(17) 0.0020(15) 0.0095(13) 0.0037(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 O7 1.419(3) . ? Cl1 O9 1.425(3) . ? Cl1 O8 1.432(3) . ? Cl1 O6 1.430(3) . ? Zn1 O4 2.041(2) 2 ? Zn1 O4 2.041(2) . ? Zn1 O5 2.088(2) . ? Zn1 O5 2.088(2) 2 ? Zn1 O1 2.150(2) 2 ? Zn1 O1 2.150(2) . ? O1 N1 1.342(3) . ? O2 N2 1.308(4) . ? O3 N3 1.323(4) . ? N1 C5 1.329(4) . ? N1 C1 1.334(4) . ? N2 C6 1.336(5) . ? N2 C10 1.345(5) . ? N3 C15 1.341(4) . ? N3 C11 1.346(4) . ? C1 C2 1.371(4) . ? C2 C3 1.383(5) . ? C3 C4 1.395(4) . ? C3 C3 1.492(6) 2_545 ? C4 C5 1.371(5) . ? C6 C7 1.364(5) . ? C7 C8 1.387(5) . ? C8 C9 1.387(5) . ? C8 C8 1.483(7) 2_456 ? C9 C10 1.372(5) . ? C11 C12 1.374(5) . ? C12 C13 1.388(4) . ? C13 C14 1.398(4) . ? C13 C13 1.481(6) 2_566 ? C14 C15 1.370(5) . ? 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 O7 Cl1 O9 108.7(2) . . ? O7 Cl1 O8 108.7(2) . . ? O9 Cl1 O8 110.6(2) . . ? O7 Cl1 O6 111.8(2) . . ? O9 Cl1 O6 108.5(2) . . ? O8 Cl1 O6 108.54(19) . . ? O4 Zn1 O4 180.00(15) 2 . ? O4 Zn1 O5 94.40(10) 2 . ? O4 Zn1 O5 85.61(10) . . ? O4 Zn1 O5 85.60(10) 2 2 ? O4 Zn1 O5 94.39(10) . 2 ? O5 Zn1 O5 180.00(10) . 2 ? O4 Zn1 O1 89.80(10) 2 2 ? O4 Zn1 O1 90.20(10) . 2 ? O5 Zn1 O1 92.62(8) . 2 ? O5 Zn1 O1 87.38(8) 2 2 ? O4 Zn1 O1 90.20(10) 2 . ? O4 Zn1 O1 89.80(10) . . ? O5 Zn1 O1 87.38(8) . . ? O5 Zn1 O1 92.62(8) 2 . ? O1 Zn1 O1 180.00(11) 2 . ? N1 O1 Zn1 113.10(15) . . ? C5 N1 C1 120.5(3) . . ? C5 N1 O1 120.1(2) . . ? C1 N1 O1 119.3(3) . . ? O2 N2 C6 120.6(3) . . ? O2 N2 C10 119.6(3) . . ? C6 N2 C10 119.7(3) . . ? O3 N3 C15 120.5(3) . . ? O3 N3 C11 119.1(3) . . ? C15 N3 C11 120.5(3) . . ? N1 C1 C2 120.6(3) . . ? C1 C2 C3 120.9(3) . . ? C2 C3 C4 116.6(3) . . ? C2 C3 C3 122.3(3) . 2_545 ? C4 C3 C3 121.2(4) . 2_545 ? C5 C4 C3 120.4(3) . . ? N1 C5 C4 120.9(3) . . ? N2 C6 C7 121.3(3) . . ? C6 C7 C8 120.9(3) . . ? C7 C8 C9 116.3(3) . . ? C7 C8 C8 122.0(4) . 2_456 ? C9 C8 C8 121.7(4) . 2_456 ? C10 C9 C8 121.1(3) . . ? N2 C10 C9 120.5(3) . . ? N3 C11 C12 120.0(3) . . ? C11 C12 C13 121.5(3) . . ? C12 C13 C14 116.5(3) . . ? C12 C13 C13 122.1(3) . 2_566 ? C14 C13 C13 121.3(3) . 2_566 ? C15 C14 C13 120.4(3) . . ? N3 C15 C14 121.1(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.636 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.075 # END