Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _journal_coden_Cambridge 186 loop_ _publ_author_name 'Li, Shu-an' 'Tang, Wen-Xia' 'Xia, Jiang' 'Yu, Kai-Bei' _publ_section_title ; Cu(II)-alkoxide promoted carboxyester cleavage: Elucidation of the roles of metal-alkoxide in alkaline phosphatase and tetrahymena ribozyme ; _publ_requested_journal 'J. C. S. Dalton' _publ_contact_author_name 'Wenxia Tang' _publ_contact_author_address ; State Key Laboratory of Coordination Chemistry, Department of Chemistry, Nanjing University, Nanjing 210093, P. R. China ; _publ_contact_author_email wxtang@netra.nju.edu.cn _publ_contact_author_fax '?' _publ_contact_author_phone '?' #============================================================================== data_y729 _database_code_CSD 156015 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H34 Cl4 Cu2 N6 O10' _chemical_formula_weight 691.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.330(2) _cell_length_b 11.6090(10) _cell_length_c 11.310(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.540(10) _cell_angle_gamma 90.00 _cell_volume 1293.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 17.79 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 2.115 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4690 _exptl_absorpt_correction_T_max 0.5346 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.88 _diffrn_reflns_number 3273 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2540 _reflns_number_gt 2144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.1118P] 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 0.0142(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2540 _refine_ls_number_parameters 159 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Cu Cu 0.16947(3) 0.39203(2) 0.17888(2) 0.03077(11) Uani 1 1 d . . . Cl1 Cl 0.06488(7) 0.28108(5) 0.01333(5) 0.04583(17) Uani 1 1 d . . . O1 O -0.02790(18) 0.44652(18) 0.21501(17) 0.0498(4) Uani 1 1 d D . . N1 N 0.24095(19) 0.50077(15) 0.32623(16) 0.0332(4) Uani 1 1 d . . . N2 N 0.2406(2) 0.26594(16) 0.30423(18) 0.0420(5) Uani 1 1 d . . . H2A H 0.1753 0.2414 0.3358 0.050 Uiso 1 1 calc R . . H2B H 0.2696 0.2057 0.2688 0.050 Uiso 1 1 calc R . . N3 N 0.2198(2) 0.51744(17) 0.08035(18) 0.0464(5) Uani 1 1 d . . . H3A H 0.2758 0.4889 0.0401 0.056 Uiso 1 1 calc R . . H3B H 0.1444 0.5432 0.0232 0.056 Uiso 1 1 calc R . . C1 C 0.1289(3) 0.5741(2) 0.3431(3) 0.0453(6) Uani 1 1 d . . . H1A H 0.1080 0.6345 0.2810 0.054 Uiso 1 1 calc R . . H1B H 0.1584 0.6102 0.4242 0.054 Uiso 1 1 calc R . . C2 C 0.0035(3) 0.5039(2) 0.3317(2) 0.0433(6) Uani 1 1 d . . . H2C H 0.0200 0.4484 0.3987 0.052 Uiso 1 1 calc R . . H2D H -0.0710 0.5534 0.3349 0.052 Uiso 1 1 calc R . . C3 C 0.3040(3) 0.4305(2) 0.4382(2) 0.0422(6) Uani 1 1 d . . . H3C H 0.2380 0.4160 0.4819 0.051 Uiso 1 1 calc R . . H3D H 0.3795 0.4724 0.4934 0.051 Uiso 1 1 calc R . . C4 C 0.3541(3) 0.3169(2) 0.4022(2) 0.0450(6) Uani 1 1 d . . . H4A H 0.4314 0.3295 0.3718 0.054 Uiso 1 1 calc R . . H4B H 0.3817 0.2659 0.4733 0.054 Uiso 1 1 calc R . . C5 C 0.3435(3) 0.5727(2) 0.2911(2) 0.0412(5) Uani 1 1 d . . . H5A H 0.4249 0.5276 0.2995 0.049 Uiso 1 1 calc R . . H5B H 0.3680 0.6383 0.3464 0.049 Uiso 1 1 calc R . . C6 C 0.2870(3) 0.6142(2) 0.1591(2) 0.0469(6) Uani 1 1 d . . . H6A H 0.2223 0.6758 0.1549 0.056 Uiso 1 1 calc R . . H6B H 0.3599 0.6440 0.1302 0.056 Uiso 1 1 calc R . . H1O H -0.0993(17) 0.411(2) 0.201(3) 0.069(11) Uiso 1 1 d D . . O2 O -0.2887(2) 0.34881(17) 0.1428(2) 0.0639(6) Uani 1 1 d . . . Cl2 Cl -0.37707(7) 0.41424(5) 0.19267(6) 0.04346(16) Uani 1 1 d . . . O3 O -0.5078(2) 0.36351(18) 0.1590(2) 0.0682(6) Uani 1 1 d . . . O4 O -0.3823(3) 0.52832(19) 0.1523(4) 0.1167(12) Uani 1 1 d . . . O5 O -0.3239(3) 0.4105(3) 0.3235(2) 0.1024(10) 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 Cu 0.03540(17) 0.02934(16) 0.02680(15) 0.00102(10) 0.00821(11) 0.00086(11) Cl1 0.0538(4) 0.0448(3) 0.0373(3) -0.0102(2) 0.0114(3) -0.0050(3) O1 0.0355(10) 0.0701(12) 0.0458(10) -0.0121(9) 0.0153(8) -0.0059(9) N1 0.0308(10) 0.0327(9) 0.0352(9) -0.0026(8) 0.0086(8) 0.0023(8) N2 0.0542(13) 0.0332(10) 0.0390(11) 0.0044(8) 0.0146(10) 0.0080(9) N3 0.0496(13) 0.0504(12) 0.0369(10) 0.0086(9) 0.0095(9) -0.0120(10) C1 0.0443(14) 0.0394(13) 0.0542(14) -0.0090(11) 0.0178(12) 0.0077(11) C2 0.0405(14) 0.0487(14) 0.0457(13) -0.0047(11) 0.0205(11) 0.0085(11) C3 0.0416(14) 0.0525(14) 0.0288(11) -0.0013(10) 0.0050(10) 0.0008(12) C4 0.0446(14) 0.0498(14) 0.0378(12) 0.0134(11) 0.0082(11) 0.0125(12) C5 0.0356(13) 0.0363(12) 0.0492(13) -0.0049(10) 0.0091(11) -0.0041(10) C6 0.0447(14) 0.0380(13) 0.0580(15) 0.0080(11) 0.0157(12) -0.0051(11) O2 0.0662(14) 0.0587(12) 0.0842(15) -0.0158(11) 0.0487(12) -0.0075(11) Cl2 0.0413(3) 0.0382(3) 0.0533(4) -0.0083(3) 0.0179(3) -0.0053(3) O3 0.0494(12) 0.0706(13) 0.0886(16) -0.0237(12) 0.0271(11) -0.0183(10) O4 0.105(2) 0.0404(12) 0.214(4) 0.0230(17) 0.062(2) 0.0030(14) O5 0.092(2) 0.154(3) 0.0548(14) -0.0330(15) 0.0128(13) 0.0058(18) _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 Cu N3 1.9952(19) . ? Cu N2 2.0162(19) . ? Cu N1 2.0432(18) . ? Cu Cl1 2.2611(7) . ? Cu O1 2.2861(19) . ? O1 C2 1.426(3) . ? N1 C3 1.482(3) . ? N1 C5 1.494(3) . ? N1 C1 1.494(3) . ? N2 C4 1.473(3) . ? N3 C6 1.472(3) . ? C1 C2 1.503(4) . ? C3 C4 1.516(3) . ? C5 C6 1.509(3) . ? O2 Cl2 1.428(2) . ? Cl2 O4 1.397(2) . ? Cl2 O5 1.415(2) . ? Cl2 O3 1.417(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu N2 145.22(9) . . ? N3 Cu N1 85.05(8) . . ? N2 Cu N1 84.81(8) . . ? N3 Cu Cl1 95.34(6) . . ? N2 Cu Cl1 98.67(6) . . ? N1 Cu Cl1 172.94(5) . . ? N3 Cu O1 107.12(9) . . ? N2 Cu O1 103.36(8) . . ? N1 Cu O1 78.80(7) . . ? Cl1 Cu O1 94.38(5) . . ? C2 O1 Cu 109.18(14) . . ? C3 N1 C5 111.75(18) . . ? C3 N1 C1 111.26(18) . . ? C5 N1 C1 110.75(18) . . ? C3 N1 Cu 108.33(13) . . ? C5 N1 Cu 103.85(13) . . ? C1 N1 Cu 110.64(14) . . ? C4 N2 Cu 106.05(14) . . ? C6 N3 Cu 111.96(15) . . ? N1 C1 C2 111.20(19) . . ? O1 C2 C1 106.39(19) . . ? N1 C3 C4 110.33(18) . . ? N2 C4 C3 107.00(19) . . ? N1 C5 C6 110.37(19) . . ? N3 C6 C5 109.03(19) . . ? O4 Cl2 O5 109.6(2) . . ? O4 Cl2 O3 111.51(17) . . ? O5 Cl2 O3 107.82(16) . . ? O4 Cl2 O2 109.95(16) . . ? O5 Cl2 O2 107.70(16) . . ? O3 Cl2 O2 110.13(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu O1 C2 -93.45(17) . . . . ? N2 Cu O1 C2 69.59(17) . . . . ? N1 Cu O1 C2 -12.25(15) . . . . ? Cl1 Cu O1 C2 169.59(15) . . . . ? N3 Cu N1 C3 -146.06(16) . . . . ? N2 Cu N1 C3 0.63(15) . . . . ? Cl1 Cu N1 C3 120.4(4) . . . . ? O1 Cu N1 C3 105.38(15) . . . . ? N3 Cu N1 C5 -27.13(14) . . . . ? N2 Cu N1 C5 119.55(14) . . . . ? Cl1 Cu N1 C5 -120.6(4) . . . . ? O1 Cu N1 C5 -135.70(14) . . . . ? N3 Cu N1 C1 91.74(16) . . . . ? N2 Cu N1 C1 -121.58(16) . . . . ? Cl1 Cu N1 C1 -1.8(5) . . . . ? O1 Cu N1 C1 -16.83(15) . . . . ? N3 Cu N2 C4 45.8(2) . . . . ? N1 Cu N2 C4 -27.77(15) . . . . ? Cl1 Cu N2 C4 158.43(14) . . . . ? O1 Cu N2 C4 -104.94(16) . . . . ? N2 Cu N3 C6 -69.6(2) . . . . ? N1 Cu N3 C6 3.86(18) . . . . ? Cl1 Cu N3 C6 176.79(17) . . . . ? O1 Cu N3 C6 80.53(18) . . . . ? C3 N1 C1 C2 -76.0(3) . . . . ? C5 N1 C1 C2 159.1(2) . . . . ? Cu N1 C1 C2 44.5(2) . . . . ? Cu O1 C2 C1 37.4(2) . . . . ? N1 C1 C2 O1 -54.7(3) . . . . ? C5 N1 C3 C4 -87.3(2) . . . . ? C1 N1 C3 C4 148.3(2) . . . . ? Cu N1 C3 C4 26.5(2) . . . . ? Cu N2 C4 C3 48.8(2) . . . . ? N1 C3 C4 N2 -50.6(3) . . . . ? C3 N1 C5 C6 162.78(19) . . . . ? C1 N1 C5 C6 -72.6(2) . . . . ? Cu N1 C5 C6 46.2(2) . . . . ? Cu N3 C6 C5 20.8(3) . . . . ? N1 C5 C6 N3 -45.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.523 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.054