# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Miao Du' 'Xian-He Bu' 'Ya-Mei Guo' 'Joan Ribas' 'Carmen Diaz' _publ_contact_author_name 'Prof Xian-He Bu' _publ_contact_author_address ; Chemistry Nankai University Nankai University, Tianjin Tianjin 300071 CHINA ; _publ_contact_author_email 'BUXH@NANKAI.EDU.CN' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Proton-controlled inter-conversion of an achiral discrete molecular box versus a chiral interpenetrated double-chain architecture ; data_1 _database_code_CSD 178167 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H88 Cl4 Cu4 N8 O34' _chemical_formula_weight 1717.24 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 Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 13.4001(10) _cell_length_b 13.4001(10) _cell_length_c 34.747(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6239.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6502 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 1.622 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6872 _exptl_absorpt_correction_T_max 0.7374 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6541 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2265 _reflns_number_gt 1449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The ClO4 anions in this structure are disordered and the oxygen atoms refined with isotropic thermal parameters. The hydrogen atoms of the aqua ligand and the carboxylic group can not be determined by difference Fourier syntheses although they should be incorporated in the formula. The occupied factor of the oxygen atom of the aqua ligand is 0.5. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2265 _refine_ls_number_parameters 194 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1843 _refine_ls_R_factor_gt 0.1390 _refine_ls_wR_factor_ref 0.3578 _refine_ls_wR_factor_gt 0.3252 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.097 _refine_ls_shift/su_mean 0.074 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 Cu1 Cu 0.67310(11) 0.57566(11) 0.11651(5) 0.0482(7) Uani 1 1 d . . . Cl1 Cl 0.0000 0.2500 0.0235(3) 0.116(3) Uani 1 2 d SD . . Cl2 Cl 0.5000 0.2500 0.0578(3) 0.101(2) Uani 1 2 d SD . . O1 O 0.5284(8) 0.5833(9) 0.1103(3) 0.069(3) Uani 1 1 d . . . O2 O 0.3829(9) 0.5903(9) 0.0820(3) 0.076(3) Uani 1 1 d . . . N1 N 0.8033(13) 0.4964(13) 0.1287(5) 0.112(7) Uani 1 1 d D . . N2 N 0.7080(8) 0.5863(10) 0.0601(4) 0.074(4) Uani 1 1 d D . . C11 C 0.8190(18) 0.4100(12) 0.1070(7) 0.166(18) Uani 1 1 d D . . H11A H 0.8038 0.3505 0.1218 0.200 Uiso 1 1 calc R . . H11B H 0.8872 0.4062 0.0978 0.200 Uiso 1 1 calc R . . C12 C 0.747(2) 0.424(2) 0.0746(8) 0.18(19) Uani 1 1 d D . . H12A H 0.6836 0.4184 0.0879 0.218 Uiso 1 1 calc R . . H12B H 0.7540 0.3611 0.0610 0.218 Uiso 1 1 calc R . . C13 C 0.721(3) 0.4937(14) 0.0424(8) 0.174(17) Uani 1 1 d D . . H13A H 0.7748 0.4965 0.0237 0.209 Uiso 1 1 calc R . . H13B H 0.6605 0.4726 0.0296 0.209 Uiso 1 1 calc R . . C21 C 0.881(3) 0.5639(17) 0.1218(8) 0.27(3) Uani 1 1 d D . . H21A H 0.9438 0.5273 0.1230 0.324 Uiso 1 1 calc R . . H21B H 0.8820 0.6122 0.1426 0.324 Uiso 1 1 calc R . . C22 C 0.8790(14) 0.620(2) 0.0844(7) 0.144(11) Uani 1 1 d D . . H22A H 0.9183 0.5806 0.0666 0.173 Uiso 1 1 calc R . . H22B H 0.9170 0.6805 0.0890 0.173 Uiso 1 1 calc R . . C23 C 0.7888(15) 0.6528(17) 0.0620(9) 0.141(11) Uani 1 1 d D . . H23A H 0.7650 0.7148 0.0730 0.169 Uiso 1 1 calc R . . H23B H 0.8099 0.6671 0.0358 0.169 Uiso 1 1 calc R . . C41 C 0.6247(9) 0.6318(15) 0.0426(6) 0.105(7) Uani 1 1 d D . . H41A H 0.6407 0.6377 0.0155 0.126 Uiso 1 1 calc R . . H41B H 0.6217 0.6993 0.0526 0.126 Uiso 1 1 calc R . . C42 C 0.5206(10) 0.5914(15) 0.0446(5) 0.110(8) Uani 1 1 d D . . H42A H 0.4782 0.6323 0.0284 0.132 Uiso 1 1 calc R . . H42B H 0.5207 0.5245 0.0339 0.132 Uiso 1 1 calc R . . C43 C 0.4755(9) 0.5872(11) 0.0839(5) 0.061(4) Uani 1 1 d D . . C31 C 0.7997(15) 0.4616(13) 0.1669(6) 0.134(11) Uani 1 1 d D . . H31A H 0.8202 0.5166 0.1832 0.161 Uiso 1 1 calc R . . H31B H 0.8507 0.4106 0.1692 0.161 Uiso 1 1 calc R . . C32 C 0.7059(19) 0.419(2) 0.1843(8) 0.181(16) Uani 1 1 d D . . H32A H 0.6490 0.4578 0.1755 0.218 Uiso 1 1 calc R . . H32B H 0.6971 0.3511 0.1754 0.218 Uiso 1 1 calc R . . C33 C 0.709(6) 0.420(10) 0.2275(8) 0.110 Uiso 1 1 d PD . . O3 O 0.636(2) 0.453(3) 0.2434(9) 0.151 Uiso 1 1 d PD . . O4 O 0.777(2) 0.376(3) 0.2423(10) 0.156 Uiso 1 1 d PD . . O11 O 0.0000 0.2500 0.0649(7) 0.200 Uiso 1 2 d SD . . O12 O -0.012(4) 0.3576(15) 0.0211(16) 0.135 Uiso 0.37 1 d PD . . O13 O 0.099(2) 0.286(4) 0.0161(17) 0.149 Uiso 0.37 1 d PD . . O21 O 0.5000 0.2500 0.0990(6) 0.205(16) Uiso 1 2 d SD . . O22 O 0.403(2) 0.249(3) 0.0401(13) 0.125 Uiso 0.37 1 d PD . . O23 O 0.491(4) 0.3546(18) 0.0478(18) 0.144(16) Uiso 0.37 1 d PD . . O5 O 0.663(2) 0.430(3) 0.1171(12) 0.120(11) Uiso 0.50 1 d P . . 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 Cu1 0.0429(9) 0.0443(9) 0.0574(12) -0.0069(7) 0.0011(6) 0.0013(6) Cl1 0.087(4) 0.132(6) 0.128(8) 0.000 0.000 -0.011(4) Cl2 0.102(5) 0.089(4) 0.112(7) 0.000 0.000 0.015(4) O1 0.055(6) 0.090(8) 0.062(8) -0.004(5) 0.015(5) -0.002(5) O2 0.090(8) 0.107(8) 0.033(7) -0.005(5) -0.003(5) -0.026(6) N1 0.122(15) 0.107(14) 0.106(17) 0.019(11) 0.012(11) 0.052(12) N2 0.039(6) 0.103(10) 0.079(11) -0.005(8) 0.014(6) 0.006(6) C11 0.14(2) 0.049(10) 0.31(5) 0.054(18) 0.10(3) 0.054(13) C12 0.14(3) 0.15(3) 0.25(6) -0.10(4) 0.04(3) -0.03(2) C13 0.30(5) 0.100(18) 0.12(3) 0.005(17) 0.05(3) 0.08(3) C21 0.52(9) 0.090(19) 0.20(4) -0.07(2) 0.12(5) -0.17(4) C22 0.106(17) 0.21(3) 0.12(2) -0.06(2) 0.043(15) -0.076(19) C23 0.15(2) 0.16(3) 0.11(3) 0.047(19) -0.030(18) -0.004(19) C41 0.108(15) 0.110(15) 0.097(18) 0.037(13) 0.049(12) 0.010(12) C42 0.077(11) 0.115(16) 0.14(2) 0.054(14) -0.048(13) -0.006(10) C43 0.028(6) 0.071(8) 0.085(14) -0.017(8) 0.003(7) -0.009(5) C31 0.134(19) 0.050(9) 0.22(3) 0.008(13) -0.034(19) 0.048(11) C32 0.14(2) 0.15(3) 0.25(5) 0.05(3) 0.01(3) -0.07(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.955(11) 12_766 ? Cu1 O1 1.954(11) . ? Cu1 O5 1.95(3) . ? Cu1 N2 2.019(14) . ? Cu1 N1 2.086(16) . ? Cl1 O13 1.438(19) . ? Cl1 O13 1.438(19) 6_454 ? Cl1 O11 1.44(2) . ? Cl1 O12 1.453(19) . ? Cl1 O12 1.453(19) 6_454 ? Cl2 O21 1.433(19) . ? Cl2 O22 1.443(19) . ? Cl2 O22 1.443(19) 6_554 ? Cl2 O23 1.448(19) . ? Cl2 O23 1.448(19) 6_554 ? O1 C43 1.162(18) . ? O2 C43 1.244(17) . ? O2 Cu1 1.955(11) 15_565 ? N1 C11 1.396(10) . ? N1 C21 1.403(10) . ? N1 C31 1.408(10) . ? N2 C13 1.396(10) . ? N2 C23 1.403(10) . ? N2 C41 1.411(9) . ? C11 C12 1.494(10) . ? C12 C13 1.500(10) . ? C21 C22 1.501(10) . ? C22 C23 1.504(10) . ? C41 C42 1.498(10) . ? C42 C43 1.493(10) . ? C31 C32 1.506(10) . ? C32 C33 1.501(11) . ? C33 O4 1.202(12) . ? C33 O3 1.201(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O1 89.4(5) 12_766 . ? O2 Cu1 O5 112.0(12) 12_766 . ? O1 Cu1 O5 89.2(10) . . ? O2 Cu1 N2 151.9(5) 12_766 . ? O1 Cu1 N2 96.9(5) . . ? O5 Cu1 N2 95.5(12) . . ? O2 Cu1 N1 95.2(6) 12_766 . ? O1 Cu1 N1 151.5(6) . . ? O5 Cu1 N1 63.0(11) . . ? N2 Cu1 N1 92.2(6) . . ? O13 Cl1 O13 159(5) . 6_454 ? O13 Cl1 O11 100(2) . . ? O13 Cl1 O11 100(2) 6_454 . ? O13 Cl1 O12 76(3) . . ? O13 Cl1 O12 103(3) 6_454 . ? O11 Cl1 O12 93(2) . . ? O13 Cl1 O12 103(3) . 6_454 ? O13 Cl1 O12 76(3) 6_454 6_454 ? O11 Cl1 O12 93(2) . 6_454 ? O12 Cl1 O12 173(4) . 6_454 ? O21 Cl2 O22 115(2) . . ? O21 Cl2 O22 115(2) . 6_554 ? O22 Cl2 O22 130(4) . 6_554 ? O21 Cl2 O23 104(2) . . ? O22 Cl2 O23 81(2) . . ? O22 Cl2 O23 88(3) 6_554 . ? O21 Cl2 O23 104(2) . 6_554 ? O22 Cl2 O23 88(3) . 6_554 ? O22 Cl2 O23 81(2) 6_554 6_554 ? O23 Cl2 O23 152(5) . 6_554 ? C43 O1 Cu1 134.0(10) . . ? C43 O2 Cu1 109.9(10) . 15_565 ? C11 N1 C21 109.3(19) . . ? C11 N1 C31 103.8(19) . . ? C21 N1 C31 113.6(19) . . ? C11 N1 Cu1 116.0(14) . . ? C21 N1 Cu1 106(2) . . ? C31 N1 Cu1 109.3(12) . . ? C13 N2 C23 119(2) . . ? C13 N2 C41 107(2) . . ? C23 N2 C41 110.8(15) . . ? C13 N2 Cu1 113.2(14) . . ? C23 N2 Cu1 100.4(15) . . ? C41 N2 Cu1 105.4(10) . . ? N1 C11 C12 101.9(17) . . ? C11 C12 C13 142(3) . . ? C11 C12 O5 78.3(19) . . ? C13 C12 O5 115(3) . . ? N2 C13 C12 105(2) . . ? N1 C21 C22 117(2) . . ? C21 C22 C23 128(2) . . ? N2 C23 C22 117.3(17) . . ? N2 C41 C42 124.1(14) . . ? C43 C42 C41 115.7(14) . . ? O1 C43 O2 130.7(15) . . ? O1 C43 C42 118.5(12) . . ? O2 C43 C42 110.8(14) . . ? N1 C31 C32 122(2) . . ? C33 C32 C31 112(5) . . ? O4 C33 O3 127(2) . . ? O4 C33 C32 116.2(15) . . ? O3 C33 C32 116.3(14) . . ? C12 O5 Cu1 89.8(18) . . ? _diffrn_measured_fraction_theta_max 0.820 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.820 _refine_diff_density_max 1.039 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.210 #===END data_2 _database_code_CSD 178168 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 Cl4 Cu3 N4 O18' _chemical_formula_weight 1009.05 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.1565(9) _cell_length_b 13.7346(13) _cell_length_c 27.005(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3767.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15448 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 2.041 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6294 _exptl_absorpt_correction_T_max 0.6857 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15492 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6553 _reflns_number_gt 4489 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms of the protonated water molecules can not be determined by difference Fourier syntheses although they should be incorporated in the formula. ; _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^)+(0.1000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 6553 _refine_ls_number_parameters 478 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1709 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.011 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 Cu1 Cu 0.99794(12) 0.74488(8) 0.66473(3) 0.0439(3) Uani 1 1 d . . . Cu2 Cu 0.75411(11) 0.74600(9) 0.49919(5) 0.0285(2) Uani 1 1 d . . . Cu3 Cu 0.99961(13) 1.03980(6) 0.43655(3) 0.0338(2) Uani 1 1 d . . . Cl3 Cl 0.9567(3) 0.56126(19) 0.66968(10) 0.0648(8) Uani 1 1 d . . . N1 N 1.1396(8) 0.7671(6) 0.7168(3) 0.0385(19) Uani 1 1 d . . . N2 N 0.8649(8) 0.8013(9) 0.7149(3) 0.062(3) Uani 1 1 d . . . N3 N 1.1259(7) 1.1522(6) 0.4296(3) 0.046(2) Uani 1 1 d . . . N4 N 0.8724(7) 1.1094(5) 0.3915(3) 0.0340(17) Uani 1 1 d . . . O1 O 0.8764(6) 0.7566(7) 0.6069(2) 0.051(2) Uani 1 1 d . . . O2 O 0.6963(6) 0.7784(5) 0.5653(2) 0.0389(17) Uani 1 1 d . . . O3 O 0.8806(6) 0.9328(4) 0.4500(3) 0.0404(16) Uani 1 1 d . . . O4 O 0.6936(5) 0.8775(5) 0.4813(2) 0.0346(16) Uani 1 1 d . . . O5 O 0.8133(6) 0.7183(5) 0.4319(2) 0.0354(16) Uani 1 1 d . . . O6 O 0.8163(6) 0.6142(5) 0.5150(3) 0.0377(17) Uani 1 1 d . . . O7 O 1.1293(6) 0.7526(7) 0.6089(2) 0.0466(18) Uani 1 1 d . . . O8 O 1.1255(6) 0.9512(5) 0.4649(3) 0.057(2) Uani 1 1 d . . . C1 C 0.7269(10) 0.7929(12) 0.6962(4) 0.076(4) Uani 1 1 d . . . H1A H 0.7028 0.7246 0.6963 0.091 Uiso 1 1 calc R . . H1B H 0.6693 0.8258 0.7195 0.091 Uiso 1 1 calc R . . C2 C 0.7012(10) 0.8307(12) 0.6483(4) 0.071(4) Uani 1 1 d . . . H2A H 0.7265 0.8988 0.6484 0.085 Uiso 1 1 calc R . . H2B H 0.6067 0.8285 0.6432 0.085 Uiso 1 1 calc R . . C3 C 0.7655(9) 0.7835(7) 0.6043(3) 0.033(2) Uani 1 1 d . . . C4 C 0.7503(9) 1.0506(7) 0.3829(4) 0.046(2) Uani 1 1 d . . . H4A H 0.7729 0.9942 0.3630 0.055 Uiso 1 1 calc R . . H4B H 0.6884 1.0896 0.3641 0.055 Uiso 1 1 calc R . . C5 C 0.6834(8) 1.0160(7) 0.4298(4) 0.044(2) Uani 1 1 d . . . H5A H 0.6727 1.0708 0.4521 0.052 Uiso 1 1 calc R . . H5B H 0.5964 0.9917 0.4216 0.052 Uiso 1 1 calc R . . C6 C 0.7590(8) 0.9376(6) 0.4556(3) 0.031(2) Uani 1 1 d . . . C11 C 0.8618(11) 0.7405(12) 0.7604(4) 0.067(4) Uani 1 1 d . . . H11A H 0.8426 0.6738 0.7511 0.081 Uiso 1 1 calc R . . H11B H 0.7906 0.7630 0.7814 0.081 Uiso 1 1 calc R . . C12 C 0.9889(13) 0.7421(9) 0.7901(3) 0.067(3) Uani 1 1 d . . . H12A H 1.0036 0.8080 0.8018 0.080 Uiso 1 1 calc R . . H12B H 0.9777 0.7010 0.8190 0.080 Uiso 1 1 calc R . . C13 C 1.1067(11) 0.7100(10) 0.7633(4) 0.057(3) Uani 1 1 d . . . H13A H 1.0952 0.6421 0.7543 0.068 Uiso 1 1 calc R . . H13B H 1.1813 0.7137 0.7857 0.068 Uiso 1 1 calc R . . C14 C 0.9058(13) 0.9067(11) 0.7251(5) 0.069(4) Uani 1 1 d . . . H14A H 0.8426 0.9497 0.7093 0.083 Uiso 1 1 calc R . . H14B H 0.9010 0.9181 0.7605 0.083 Uiso 1 1 calc R . . C15 C 1.0379(12) 0.9333(8) 0.7080(4) 0.066(4) Uani 1 1 d . . . H15A H 1.0525 1.0014 0.7158 0.079 Uiso 1 1 calc R . . H15B H 1.0402 0.9270 0.6723 0.079 Uiso 1 1 calc R . . C16 C 1.1517(11) 0.8745(9) 0.7295(5) 0.057(3) Uani 1 1 d . . . H16A H 1.2342 0.8994 0.7165 0.069 Uiso 1 1 calc R . . H16B H 1.1531 0.8823 0.7652 0.069 Uiso 1 1 calc R . . C17 C 1.2517(8) 0.7671(7) 0.6071(3) 0.030(2) Uani 1 1 d . . . C18 C 1.3299(8) 0.7658(8) 0.6551(3) 0.045(2) Uani 1 1 d . . . H18A H 1.4126 0.7327 0.6489 0.053 Uiso 1 1 calc R . . H18B H 1.3506 0.8326 0.6639 0.053 Uiso 1 1 calc R . . C19 C 1.2666(10) 0.7194(10) 0.6983(4) 0.061(3) Uani 1 1 d . . . H19A H 1.3295 0.7186 0.7254 0.073 Uiso 1 1 calc R . . H19B H 1.2473 0.6522 0.6899 0.073 Uiso 1 1 calc R . . C21 C 0.8306(12) 1.2066(8) 0.4123(5) 0.066(3) Uani 1 1 d . . . H21A H 0.7682 1.2362 0.3897 0.079 Uiso 1 1 calc R . . H21B H 0.7854 1.1957 0.4435 0.079 Uiso 1 1 calc R . . C22 C 0.9405(11) 1.2760(9) 0.4209(6) 0.073(4) Uani 1 1 d . . . H22A H 0.9044 1.3324 0.4377 0.087 Uiso 1 1 calc R . . H22B H 0.9713 1.2978 0.3888 0.087 Uiso 1 1 calc R . . C23 C 1.0578(12) 1.2430(7) 0.4496(5) 0.062(3) Uani 1 1 d . . . H23A H 1.0307 1.2304 0.4834 0.074 Uiso 1 1 calc R . . H23B H 1.1213 1.2957 0.4504 0.074 Uiso 1 1 calc R . . C24 C 0.9379(11) 1.1219(10) 0.3420(4) 0.060(3) Uani 1 1 d . . . H24A H 0.9154 1.1855 0.3289 0.071 Uiso 1 1 calc R . . H24B H 0.9033 1.0734 0.3193 0.071 Uiso 1 1 calc R . . C25 C 1.0863(13) 1.1125(16) 0.3437(6) 0.105(7) Uani 1 1 d . . . H25A H 1.1053 1.0438 0.3477 0.127 Uiso 1 1 calc R . . H25B H 1.1183 1.1307 0.3112 0.127 Uiso 1 1 calc R . . C26 C 1.1660(11) 1.1621(10) 0.3783(4) 0.064(3) Uani 1 1 d . . . H26A H 1.1666 1.2307 0.3698 0.076 Uiso 1 1 calc R . . H26B H 1.2556 1.1383 0.3751 0.076 Uiso 1 1 calc R . . C27 C 1.2512(9) 0.9555(7) 0.4694(3) 0.035(2) Uani 1 1 d . . . C28 C 1.3186(9) 1.0499(7) 0.4593(5) 0.057(3) Uani 1 1 d . . . H28A H 1.3953 1.0538 0.4806 0.068 Uiso 1 1 calc R . . H28B H 1.3500 1.0486 0.4254 0.068 Uiso 1 1 calc R . . C29 C 1.2415(9) 1.1393(7) 0.4660(5) 0.057(3) Uani 1 1 d . . . H29A H 1.3001 1.1947 0.4627 0.068 Uiso 1 1 calc R . . H29B H 1.2069 1.1401 0.4995 0.068 Uiso 1 1 calc R . . Cl1 Cl 0.9326(4) 0.0857(3) 0.57141(12) 0.0758(9) Uani 1 1 d D . . O11 O 0.988(2) -0.0078(10) 0.5769(6) 0.242(11) Uani 1 1 d D . . O12 O 0.8872(14) 0.0946(9) 0.5222(4) 0.133(5) Uani 1 1 d D . . O13 O 0.8278(16) 0.0946(18) 0.6061(6) 0.215(9) Uani 1 1 d D . . O14 O 1.0144(17) 0.1683(11) 0.5816(5) 0.184(7) Uani 1 1 d D . . Cl2 Cl 0.4882(4) 0.0635(2) 0.71370(11) 0.0694(7) Uani 1 1 d D . . O21 O 0.6013(13) 0.0881(13) 0.6863(6) 0.172(7) Uani 1 1 d D . . O22 O 0.467(2) 0.1047(16) 0.7610(6) 0.272(13) Uani 1 1 d D . . O23 O 0.3794(18) 0.080(2) 0.6812(9) 0.32(2) Uani 1 1 d D . . O24 O 0.4823(19) -0.0377(7) 0.7216(6) 0.178(6) Uani 1 1 d D . . Cl4 Cl 0.0066(4) 0.6369(2) 0.46457(12) 0.0749(8) Uani 1 1 d . . . O31 O 0.0037(7) 0.7825(3) 0.51234(18) 0.0339(11) Uani 1 1 d . . . O32 O 0.0586(13) 0.4973(7) 0.4252(4) 0.120(4) 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 Cu1 0.0255(5) 0.0850(8) 0.0213(4) -0.0058(5) -0.0017(5) 0.0068(8) Cu2 0.0226(4) 0.0352(5) 0.0276(4) 0.0000(4) -0.0007(3) 0.0018(3) Cu3 0.0255(4) 0.0295(4) 0.0464(5) 0.0145(4) -0.0070(6) -0.0030(6) Cl3 0.107(2) 0.0507(15) 0.0371(13) 0.0041(11) 0.0120(13) 0.0130(13) N1 0.035(4) 0.054(5) 0.027(4) 0.005(4) -0.004(3) 0.008(4) N2 0.028(5) 0.127(10) 0.031(5) -0.016(5) -0.006(4) 0.010(5) N3 0.039(4) 0.038(4) 0.062(6) 0.025(4) -0.011(4) 0.002(3) N4 0.031(4) 0.035(4) 0.035(4) 0.013(3) -0.006(3) -0.005(3) O1 0.023(4) 0.096(6) 0.034(4) -0.015(5) -0.002(3) 0.019(4) O2 0.024(3) 0.061(4) 0.032(4) -0.009(3) -0.010(3) 0.010(3) O3 0.023(3) 0.034(3) 0.064(5) 0.014(3) -0.004(3) -0.005(3) O4 0.023(3) 0.038(4) 0.043(4) 0.006(3) 0.002(3) -0.003(3) O5 0.024(3) 0.058(4) 0.025(3) 0.000(3) -0.002(3) 0.012(3) O6 0.025(3) 0.035(4) 0.053(5) 0.006(3) 0.005(3) -0.006(3) O7 0.025(3) 0.090(6) 0.024(3) -0.002(4) 0.003(2) -0.009(4) O8 0.024(3) 0.046(4) 0.102(6) 0.039(4) -0.016(3) -0.013(3) C1 0.025(5) 0.159(13) 0.043(7) -0.025(8) 0.003(4) -0.002(7) C2 0.029(6) 0.144(12) 0.039(6) -0.020(7) 0.000(5) 0.027(7) C3 0.023(5) 0.046(5) 0.029(5) -0.008(4) -0.003(4) -0.003(4) C4 0.041(5) 0.045(5) 0.051(6) 0.008(5) -0.017(4) -0.011(5) C5 0.018(4) 0.040(5) 0.073(7) 0.017(5) 0.003(4) 0.004(4) C6 0.020(4) 0.032(5) 0.040(5) -0.004(4) 0.000(4) 0.001(4) C11 0.050(7) 0.122(11) 0.029(6) 0.012(7) 0.014(5) -0.011(7) C12 0.068(7) 0.107(8) 0.027(4) 0.002(5) 0.005(6) 0.006(9) C13 0.058(7) 0.089(9) 0.024(5) 0.003(5) 0.000(5) -0.003(6) C14 0.075(9) 0.094(10) 0.038(7) -0.014(7) -0.003(6) 0.029(8) C15 0.100(11) 0.055(6) 0.041(6) 0.001(5) -0.006(6) 0.007(6) C16 0.049(7) 0.077(8) 0.045(6) 0.002(6) -0.004(5) -0.007(6) C17 0.022(5) 0.035(5) 0.031(5) 0.006(4) 0.002(4) 0.004(4) C18 0.023(5) 0.076(7) 0.034(5) -0.011(5) -0.004(4) 0.010(5) C19 0.047(6) 0.111(10) 0.026(5) 0.005(6) -0.013(4) 0.012(6) C21 0.068(8) 0.047(6) 0.083(9) 0.014(6) 0.011(6) 0.008(6) C22 0.048(6) 0.052(7) 0.119(11) 0.002(7) -0.006(7) -0.005(5) C23 0.073(7) 0.029(5) 0.082(8) 0.002(5) -0.019(6) -0.004(5) C24 0.048(6) 0.095(9) 0.035(6) 0.008(6) -0.001(5) -0.012(6) C25 0.063(10) 0.191(19) 0.062(10) -0.036(11) 0.036(7) -0.029(10) C26 0.044(7) 0.088(9) 0.059(8) 0.028(7) -0.004(5) -0.016(6) C27 0.026(5) 0.037(5) 0.042(5) 0.001(4) -0.005(4) -0.002(4) C28 0.033(5) 0.045(6) 0.093(9) 0.023(6) -0.020(5) -0.016(5) C29 0.037(5) 0.043(6) 0.090(9) 0.016(5) -0.023(5) -0.022(5) Cl1 0.098(2) 0.079(2) 0.0509(18) 0.0100(16) -0.0009(17) 0.0180(19) O11 0.32(3) 0.25(2) 0.159(15) -0.045(14) -0.059(18) 0.17(2) O12 0.173(12) 0.102(8) 0.126(11) 0.004(7) -0.057(9) 0.023(8) O13 0.205(18) 0.26(2) 0.183(18) 0.002(16) 0.061(15) 0.039(16) O14 0.210(17) 0.218(15) 0.125(11) -0.033(10) -0.013(12) -0.110(16) Cl2 0.0711(19) 0.0575(15) 0.0796(19) -0.0012(13) 0.0043(19) -0.0122(18) O21 0.132(11) 0.176(15) 0.208(17) -0.006(13) 0.051(11) -0.055(11) O22 0.22(2) 0.25(2) 0.34(3) -0.17(2) 0.08(2) -0.007(18) O23 0.25(2) 0.43(4) 0.28(3) 0.20(3) -0.15(2) -0.21(3) O24 0.188(15) 0.172(13) 0.175(14) 0.021(11) -0.033(14) -0.025(14) Cl4 0.0567(15) 0.0811(18) 0.087(2) 0.0047(14) 0.009(2) -0.005(2) O31 0.036(3) 0.032(2) 0.033(3) 0.002(2) 0.002(3) 0.002(3) O32 0.182(12) 0.080(6) 0.099(8) -0.013(6) 0.020(7) -0.041(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 Cu1 O1 1.998(7) . ? Cu1 O7 2.016(6) . ? Cu1 N1 2.035(8) . ? Cu1 N2 2.064(9) . ? Cu1 Cl3 2.560(3) . ? Cu2 O2 1.931(7) . ? Cu2 O5 1.951(6) . ? Cu2 O6 1.964(6) . ? Cu2 O4 1.968(7) . ? Cu3 O8 1.924(6) . ? Cu3 O3 1.938(6) . ? Cu3 N3 2.016(8) . ? Cu3 N4 2.016(7) . ? N1 C13 1.519(14) . ? N1 C16 1.519(15) . ? N1 C19 1.531(14) . ? N2 C11 1.487(15) . ? N2 C1 1.494(13) . ? N2 C14 1.531(18) . ? N3 C26 1.450(14) . ? N3 C23 1.526(14) . ? N3 C29 1.543(12) . ? N4 C4 1.498(11) . ? N4 C24 1.503(13) . ? N4 C21 1.510(14) . ? O1 C3 1.188(11) . ? O2 C3 1.268(11) . ? O3 C6 1.246(10) . ? O4 C6 1.268(11) . ? O5 C17 1.242(10) 4_466 ? O6 C27 1.238(11) 4_466 ? O7 C17 1.260(10) . ? O8 C27 1.284(10) . ? C1 C2 1.417(17) . ? C2 C3 1.504(14) . ? C4 C5 1.513(14) . ? C5 C6 1.496(12) . ? C11 C12 1.519(16) . ? C12 C13 1.465(16) . ? C14 C15 1.465(18) . ? C15 C16 1.524(16) . ? C17 O5 1.242(10) 4_566 ? C17 C18 1.520(12) . ? C18 C19 1.477(15) . ? C21 C22 1.486(16) . ? C22 C23 1.491(16) . ? C24 C25 1.513(17) . ? C25 C26 1.411(19) . ? C27 O6 1.238(11) 4_566 ? C27 C28 1.491(13) . ? C28 C29 1.468(15) . ? Cl1 O12 1.411(8) . ? Cl1 O11 1.412(9) . ? Cl1 O13 1.422(9) . ? Cl1 O14 1.433(8) . ? Cl2 O21 1.408(8) . ? Cl2 O24 1.408(9) . ? Cl2 O22 1.415(9) . ? Cl2 O23 1.430(9) . ? 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 Cu1 O7 79.6(2) . . ? O1 Cu1 N1 164.9(4) . . ? O7 Cu1 N1 92.4(3) . . ? O1 Cu1 N2 94.5(3) . . ? O7 Cu1 N2 154.7(4) . . ? N1 Cu1 N2 87.3(3) . . ? O1 Cu1 Cl3 91.1(3) . . ? O7 Cu1 Cl3 101.5(3) . . ? N1 Cu1 Cl3 103.1(3) . . ? N2 Cu1 Cl3 103.2(4) . . ? O2 Cu2 O5 177.9(4) . . ? O2 Cu2 O6 96.3(3) . . ? O5 Cu2 O6 85.6(3) . . ? O2 Cu2 O4 85.4(3) . . ? O5 Cu2 O4 92.7(3) . . ? O6 Cu2 O4 178.3(3) . . ? O8 Cu3 O3 81.9(2) . . ? O8 Cu3 N3 95.7(3) . . ? O3 Cu3 N3 174.5(3) . . ? O8 Cu3 N4 165.0(3) . . ? O3 Cu3 N4 94.2(3) . . ? N3 Cu3 N4 89.3(3) . . ? C13 N1 C16 109.5(9) . . ? C13 N1 C19 103.5(8) . . ? C16 N1 C19 114.9(9) . . ? C13 N1 Cu1 109.8(6) . . ? C16 N1 Cu1 111.0(6) . . ? C19 N1 Cu1 107.8(6) . . ? C11 N2 C1 102.5(9) . . ? C11 N2 C14 112.8(10) . . ? C1 N2 C14 112.9(11) . . ? C11 N2 Cu1 110.2(8) . . ? C1 N2 Cu1 111.3(7) . . ? C14 N2 Cu1 107.2(7) . . ? C26 N3 C23 112.9(9) . . ? C26 N3 C29 114.0(8) . . ? C23 N3 C29 102.3(8) . . ? C26 N3 Cu3 109.9(7) . . ? C23 N3 Cu3 107.7(6) . . ? C29 N3 Cu3 109.7(5) . . ? C4 N4 C24 106.9(8) . . ? C4 N4 C21 107.6(8) . . ? C24 N4 C21 110.8(8) . . ? C4 N4 Cu3 111.6(5) . . ? C24 N4 Cu3 107.9(6) . . ? C21 N4 Cu3 112.0(7) . . ? C3 O1 Cu1 131.1(6) . . ? C3 O2 Cu2 127.8(6) . . ? C6 O3 Cu3 126.9(6) . . ? C6 O4 Cu2 124.6(5) . . ? C17 O5 Cu2 127.1(6) 4_466 . ? C27 O6 Cu2 128.0(6) 4_466 . ? C17 O7 Cu1 133.6(6) . . ? C27 O8 Cu3 132.0(6) . . ? C2 C1 N2 116.9(11) . . ? C1 C2 C3 118.9(11) . . ? O1 C3 O2 123.8(9) . . ? O1 C3 C2 120.0(9) . . ? O2 C3 C2 116.2(9) . . ? N4 C4 C5 114.3(8) . . ? C6 C5 C4 112.7(8) . . ? O3 C6 O4 123.5(8) . . ? O3 C6 C5 119.4(8) . . ? O4 C6 C5 117.1(7) . . ? N2 C11 C12 114.2(9) . . ? C13 C12 C11 115.4(9) . . ? C12 C13 N1 115.6(10) . . ? C15 C14 N2 115.3(10) . . ? C14 C15 C16 116.3(10) . . ? N1 C16 C15 111.6(9) . . ? O5 C17 O7 123.8(8) 4_566 . ? O5 C17 C18 117.5(8) 4_566 . ? O7 C17 C18 118.7(8) . . ? C19 C18 C17 116.8(8) . . ? C18 C19 N1 116.0(9) . . ? C22 C21 N4 114.4(10) . . ? C21 C22 C23 119.1(10) . . ? C22 C23 N3 115.2(10) . . ? N4 C24 C25 113.8(11) . . ? C26 C25 C24 123.5(15) . . ? C25 C26 N3 115.2(10) . . ? O6 C27 O8 121.8(8) 4_566 . ? O6 C27 C28 119.3(8) 4_566 . ? O8 C27 C28 118.6(8) . . ? C29 C28 C27 117.4(8) . . ? C28 C29 N3 115.0(9) . . ? O12 Cl1 O11 108.0(8) . . ? O12 Cl1 O13 111.6(11) . . ? O11 Cl1 O13 108.1(13) . . ? O12 Cl1 O14 107.5(8) . . ? O11 Cl1 O14 117.8(11) . . ? O13 Cl1 O14 103.9(12) . . ? O21 Cl2 O24 110.6(11) . . ? O21 Cl2 O22 120.4(12) . . ? O24 Cl2 O22 104.6(12) . . ? O21 Cl2 O23 105.6(12) . . ? O24 Cl2 O23 102.7(13) . . ? O22 Cl2 O23 111.7(17) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.114 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.132 #===END