# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Chaudhuri, Nirmalendu Ray' 'Dalai, Sudipta' 'Mostafa, Golam' 'Mukherjee, Partha Sarathi' 'Rentschler, E.' _publ_contact_author_name 'Prof Nirmalendu Ray Chaudhuri' _publ_contact_author_address ; Department of Chemistry Indian Association for the Cultivation of Science Jadavpur Calcutta 700 032 INDIA ; _publ_contact_author_email 'JCNRC@MAHENDRA.IACS.RES.IN' _publ_section_title ; Synthesis, Crystal Structure, and Magnetic Properties of Two Cu(II) Polynuclear Complexes With End-toEnd Zaido as Bridging Ligand ; data_Complex_1 _database_code_CSD 167671 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H17 Cu N5 O2, 2(H2 O)' _chemical_formula_sum 'C13 H21 Cu N5 O4' _chemical_formula_weight 374.90 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.497(6) _cell_length_b 9.410(2) _cell_length_c 18.232(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.01(3) _cell_angle_gamma 90.00 _cell_volume 1604.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description parallelopiped _exptl_crystal_colour Green _exptl_crystal_size_max .40 _exptl_crystal_size_mid .31 _exptl_crystal_size_min .27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.389 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.847 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'AFC-7S diffractometer' _diffrn_measurement_method '\w-2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6242 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 32.50 _reflns_number_total 5727 _reflns_number_gt 2744 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+2.0546P] 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 5727 _refine_ls_number_parameters 220 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1381 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.006 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.87270(5) 0.36631(5) 0.18375(3) 0.03407(14) Uani 1 1 d . . . N1 N 0.8833(4) 0.5563(3) 0.14256(18) 0.0369(7) Uani 1 1 d . . . N2 N 0.7181(3) 0.4559(3) 0.23829(18) 0.0344(6) Uani 1 1 d . . . N3 N 0.8210(5) 0.1763(4) 0.2142(3) 0.0554(11) Uani 1 1 d . . . N4 N 0.8822(3) 0.0664(4) 0.21111(18) 0.0374(7) Uani 1 1 d . . . N5 N 0.9378(4) -0.0422(4) 0.2092(2) 0.0501(9) Uani 1 1 d . . . O1 O 1.0054(3) 0.2899(3) 0.12578(16) 0.0413(6) Uani 1 1 d . . . O2 O 0.4759(3) 0.3996(4) 0.31265(19) 0.0534(8) Uani 1 1 d . . . C1 C 1.0990(4) 0.3654(4) 0.0961(2) 0.0346(7) Uani 1 1 d . . . C2 C 1.2071(5) 0.2911(5) 0.0681(2) 0.0446(9) Uani 1 1 d . . . H2 H 1.2085 0.1923 0.0701 0.053 Uiso 1 1 calc R . . C3 C 1.3111(5) 0.3614(6) 0.0377(2) 0.0507(11) Uani 1 1 d . . . H3 H 1.3826 0.3099 0.0208 0.061 Uiso 1 1 calc R . . C4 C 1.3091(5) 0.5097(6) 0.0324(2) 0.0545(12) Uani 1 1 d . . . H4 H 1.3797 0.5574 0.0126 0.065 Uiso 1 1 calc R . . C5 C 1.2017(5) 0.5838(5) 0.0567(2) 0.0459(10) Uani 1 1 d . . . H5 H 1.1984 0.6821 0.0515 0.055 Uiso 1 1 calc R . . C6 C 1.0963(4) 0.5154(4) 0.0895(2) 0.0379(8) Uani 1 1 d . . . C7 C 0.9838(4) 0.6023(4) 0.1103(2) 0.0392(9) Uani 1 1 d . . . H7 H 0.9845 0.6988 0.0994 0.047 Uiso 1 1 calc R . . C8 C 0.7715(5) 0.6531(3) 0.1595(3) 0.0427(9) Uani 1 1 d . . . H8A H 0.6858 0.6440 0.1221 0.051 Uiso 1 1 calc R . . H8B H 0.8042 0.7508 0.1598 0.051 Uiso 1 1 calc R . . C9 C 0.7404(4) 0.6130(4) 0.2347(2) 0.0401(9) Uani 1 1 d . . . H9A H 0.8196 0.6412 0.2730 0.048 Uiso 1 1 calc R . . H9B H 0.6553 0.6624 0.2438 0.048 Uiso 1 1 calc R . . C10 C 0.7309(4) 0.4046(5) 0.3168(2) 0.0401(9) Uani 1 1 d . . . H10A H 0.8189 0.4411 0.3457 0.048 Uiso 1 1 calc R . . H10B H 0.7368 0.3017 0.3172 0.048 Uiso 1 1 calc R . . C11 C 0.6082(5) 0.4493(6) 0.3529(3) 0.0510(11) Uani 1 1 d . . . H11A H 0.6218 0.4122 0.4033 0.061 Uiso 1 1 calc R . . H11B H 0.6059 0.5522 0.3558 0.061 Uiso 1 1 calc R . . C12 C 0.4534(4) 0.4558(5) 0.2388(2) 0.0460(10) Uani 1 1 d . . . H12A H 0.4478 0.5586 0.2408 0.055 Uiso 1 1 calc R . . H12B H 0.3635 0.4206 0.2114 0.055 Uiso 1 1 calc R . . C13 C 0.5731(4) 0.4135(5) 0.1990(2) 0.0449(9) Uani 1 1 d . . . H13A H 0.5711 0.3112 0.1925 0.054 Uiso 1 1 calc R . . H13B H 0.5565 0.4563 0.1499 0.054 Uiso 1 1 calc R . . O3 O 0.6322(5) 0.9801(8) 0.0458(3) 0.112(2) Uani 1 1 d D . . H3WA H 0.616(10) 1.082(3) 0.044(5) 0.134 Uiso 1 1 d D . . H3WB H 0.634(9) 0.937(9) 0.093(2) 0.134 Uiso 1 1 d D . . O4 O 0.8915(4) 0.0825(4) 0.0178(2) 0.0652(10) Uani 1 1 d D . . H4WA H 0.926(6) 0.148(5) 0.055(2) 0.078 Uiso 1 1 d D . . H4WB H 0.837(5) 0.018(5) 0.039(3) 0.078 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0378(2) 0.0268(2) 0.0385(2) 0.0010(2) 0.00924(17) 0.0020(2) N1 0.0391(17) 0.0331(15) 0.0375(17) -0.0030(13) 0.0039(14) -0.0008(13) N2 0.0303(15) 0.0315(14) 0.0390(16) -0.0029(13) -0.0009(13) 0.0013(12) N3 0.059(2) 0.0295(15) 0.087(3) 0.0087(18) 0.039(2) 0.0081(16) N4 0.0374(17) 0.0402(18) 0.0367(16) 0.0021(14) 0.0119(14) -0.0036(14) N5 0.047(2) 0.0293(16) 0.070(3) -0.0073(17) -0.0016(18) 0.0064(15) O1 0.0458(16) 0.0317(13) 0.0490(16) -0.0001(12) 0.0151(13) 0.0033(12) O2 0.0406(16) 0.062(2) 0.0588(19) -0.0045(16) 0.0131(14) -0.0018(15) C1 0.0351(18) 0.0364(17) 0.0311(16) 0.0000(15) 0.0021(14) -0.0020(16) C2 0.047(2) 0.050(2) 0.036(2) 0.0018(18) 0.0064(18) 0.009(2) C3 0.044(2) 0.071(3) 0.037(2) 0.001(2) 0.0090(17) 0.001(2) C4 0.046(3) 0.078(3) 0.040(2) 0.004(2) 0.0107(19) -0.014(2) C5 0.050(2) 0.049(2) 0.038(2) 0.0013(18) 0.0066(18) -0.014(2) C6 0.039(2) 0.040(2) 0.0327(18) 0.0007(16) 0.0014(15) -0.0057(16) C7 0.046(2) 0.0317(18) 0.0378(19) 0.0018(15) 0.0002(16) -0.0030(15) C8 0.044(2) 0.0161(15) 0.065(3) 0.0041(15) 0.0027(19) 0.0059(13) C9 0.039(2) 0.0317(19) 0.050(2) -0.0096(16) 0.0070(17) 0.0037(15) C10 0.039(2) 0.050(2) 0.0323(18) 0.0028(16) 0.0085(16) 0.0060(17) C11 0.041(2) 0.066(3) 0.047(2) -0.011(2) 0.0086(19) 0.002(2) C12 0.036(2) 0.051(2) 0.051(2) -0.002(2) 0.0088(18) 0.0021(18) C13 0.037(2) 0.050(2) 0.043(2) -0.0047(19) -0.0042(17) -0.0011(18) O3 0.061(3) 0.206(7) 0.068(3) 0.022(4) 0.013(2) -0.014(4) O4 0.070(2) 0.060(2) 0.067(2) -0.0170(19) 0.0174(19) -0.0110(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu O1 1.920(3) . . yes Cu N1 1.948(3) . . yes Cu N2 2.089(3) . . yes Cu N3 1.960(4) . . yes Cu N5 2.563(4) . 2_755 yes O1 C1 1.325(5) . . no O2 C11 1.420(6) . . no O2 C12 1.428(5) . . no O3 H3WA 0.97(3) . . no O3 H3WB 0.95(5) . . no O4 H4WA 0.93(4) . . no O4 H4WB 0.92(5) . . no N1 C8 1.472(6) . . no N1 C7 1.280(5) . . no N2 C9 1.496(5) . . no N2 C13 1.492(5) . . no N2 C10 1.495(5) . . no N3 N4 1.192(5) . . yes N4 N5 1.154(5) . . yes C1 C6 1.416(5) . . no C1 C2 1.409(6) . . no C2 C3 1.382(7) . . no C3 C4 1.399(8) . . no C4 C5 1.371(7) . . no C5 C6 1.408(6) . . no C6 C7 1.447(5) . . no C8 C9 1.500(6) . . no C10 C11 1.495(6) . . no C12 C13 1.505(6) . . no C2 H2 0.9304 . . no C3 H3 0.9293 . . no C4 H4 0.9303 . . no C5 H5 0.9298 . . no C7 H7 0.9298 . . no C8 H8B 0.9701 . . no C8 H8A 0.9705 . . no C9 H9B 0.9713 . . no C9 H9A 0.9701 . . no C10 H10A 0.9700 . . no C10 H10B 0.9699 . . no C11 H11A 0.9704 . . no C11 H11B 0.9702 . . no C12 H12B 0.9695 . . no C12 H12A 0.9698 . . no C13 H13A 0.9697 . . no C13 H13B 0.9692 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu N1 92.79(14) . . . yes O1 Cu N2 175.09(13) . . . yes O1 Cu N3 92.01(17) . . . yes O1 Cu N5 95.96(13) . . 2_755 yes N1 Cu N2 84.31(14) . . . yes N1 Cu N3 168.11(19) . . . yes N2 Cu N3 90.11(17) . . . yes N1 Cu N5 84.77(13) . . 2_755 yes N2 Cu N5 87.74(12) . . 2_755 yes N3 Cu N5 105.55(18) . . 2_755 yes Cu O1 C1 125.1(2) . . . no C11 O2 C12 109.8(4) . . . no H3WA O3 H3WB 116(7) . . . no H4WA O4 H4WB 106(4) . . . no Cu N1 C8 113.5(3) . . . no C7 N1 C8 120.6(3) . . . no Cu N1 C7 125.4(3) . . . no Cu N2 C13 109.3(2) . . . no Cu N2 C9 105.2(2) . . . no Cu N2 C10 112.2(2) . . . no C10 N2 C13 106.7(3) . . . no C9 N2 C13 111.7(3) . . . no C9 N2 C10 111.9(3) . . . no Cu N3 N4 129.0(4) . . . yes N3 N4 N5 177.6(4) . . . yes Cu N5 N4 122.6(3) 2_745 . . yes O1 C1 C2 117.7(4) . . . no O1 C1 C6 124.4(3) . . . no C2 C1 C6 117.9(4) . . . no C1 C2 C3 121.6(4) . . . no C2 C3 C4 120.2(4) . . . no C3 C4 C5 119.1(4) . . . no C4 C5 C6 121.9(4) . . . no C1 C6 C5 119.2(4) . . . no C1 C6 C7 123.0(3) . . . no C5 C6 C7 117.7(4) . . . no N1 C7 C6 124.9(3) . . . no N1 C8 C9 107.5(3) . . . no N2 C9 C8 109.9(3) . . . no N2 C10 C11 113.0(4) . . . no O2 C11 C10 111.6(4) . . . no O2 C12 C13 110.8(3) . . . no N2 C13 C12 114.2(3) . . . no C3 C2 H2 119.18 . . . no C1 C2 H2 119.21 . . . no C4 C3 H3 119.95 . . . no C2 C3 H3 119.84 . . . no C5 C4 H4 120.45 . . . no C3 C4 H4 120.41 . . . no C4 C5 H5 119.13 . . . no C6 C5 H5 118.97 . . . no N1 C7 H7 117.51 . . . no C6 C7 H7 117.56 . . . no C9 C8 H8A 110.22 . . . no C9 C8 H8B 110.30 . . . no H8A C8 H8B 108.43 . . . no N1 C8 H8B 110.23 . . . no N1 C8 H8A 110.21 . . . no C8 C9 H9A 109.75 . . . no N2 C9 H9A 109.67 . . . no N2 C9 H9B 109.70 . . . no H9A C9 H9B 108.07 . . . no C8 C9 H9B 109.73 . . . no N2 C10 H10B 108.93 . . . no N2 C10 H10A 108.94 . . . no H10A C10 H10B 107.83 . . . no C11 C10 H10A 108.97 . . . no C11 C10 H10B 109.03 . . . no C10 C11 H11A 109.27 . . . no C10 C11 H11B 109.36 . . . no H11A C11 H11B 107.94 . . . no O2 C11 H11A 109.34 . . . no O2 C11 H11B 109.31 . . . no C13 C12 H12A 109.45 . . . no O2 C12 H12A 109.52 . . . no O2 C12 H12B 109.48 . . . no H12A C12 H12B 108.12 . . . no C13 C12 H12B 109.43 . . . no N2 C13 H13B 108.71 . . . no N2 C13 H13A 108.72 . . . no H13A C13 H13B 107.64 . . . no C12 C13 H13A 108.73 . . . no C12 C13 H13B 108.68 . . . no _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 32.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.678 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.108 #END# data_Complex_2 _database_code_CSD 167672 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H17 Cl Cu N6 O4' _chemical_formula_sum 'C11 H17 Cl Cu N6 O4' _chemical_formula_weight 396.30 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 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0852(10) _cell_length_b 16.2398(18) _cell_length_c 10.8913(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.881(2) _cell_angle_gamma 90.00 _cell_volume 1595.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description parallelopiped _exptl_crystal_colour Green _exptl_crystal_size_max .20 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 1.565 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w-2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9550 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 28.25 _reflns_number_total 3611 _reflns_number_gt 2571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 software' _computing_cell_refinement 'Enraf-Nonius CAD4 software' _computing_data_reduction 'Enraf-Nonius CAD4 software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (1994)' _computing_publication_material 'PLATON99 (A.L. Spek, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0533P)^2^+0.7367P] 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 3611 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.33428(4) 0.14836(2) 0.94084(4) 0.03812(15) Uani 1 1 d . . . N1 N 0.2513(3) 0.12341(16) 1.1024(3) 0.0363(6) Uani 1 1 d . . . N2 N 0.1169(3) 0.14219(17) 0.8775(3) 0.0420(7) Uani 1 1 d . . . N3 N 0.4065(3) 0.15472(17) 0.7691(3) 0.0431(7) Uani 1 1 d . . . N4 N 0.5365(3) 0.14591(19) 1.0287(3) 0.0497(8) Uani 1 1 d . . . N5 N 0.6137(3) 0.0867(2) 1.0321(3) 0.0438(7) Uani 1 1 d . . . N6 N 0.6944(4) 0.0318(3) 1.0364(4) 0.0732(11) Uani 1 1 d . . . C1 C 0.3247(4) 0.1136(2) 1.2148(3) 0.0425(8) Uani 1 1 d . . . H1 H 0.4248 0.1270 1.2279 0.051 Uiso 1 1 calc R . . C2 C 0.2559(4) 0.0840(2) 1.3127(3) 0.0501(9) Uani 1 1 d . . . H2 H 0.3099 0.0770 1.3901 0.060 Uiso 1 1 calc R . . C3 C 0.1085(5) 0.0650(2) 1.2952(4) 0.0531(10) Uani 1 1 d . . . H3 H 0.0614 0.0448 1.3602 0.064 Uiso 1 1 calc R . . C4 C 0.0296(4) 0.0764(2) 1.1788(4) 0.0499(9) Uani 1 1 d . . . H4 H -0.0712 0.0648 1.1645 0.060 Uiso 1 1 calc R . . C5 C 0.1052(4) 0.1051(2) 1.0858(3) 0.0388(7) Uani 1 1 d . . . C6 C 0.0364(4) 0.1200(2) 0.9583(4) 0.0442(8) Uani 1 1 d . . . H6 H -0.0651 0.1131 0.9376 0.053 Uiso 1 1 calc R . . C7 C 0.0481(4) 0.1623(3) 0.7519(4) 0.0547(10) Uani 1 1 d . . . H7A H 0.0285 0.2210 0.7462 0.066 Uiso 1 1 calc R . . H7B H -0.0458 0.1337 0.7354 0.066 Uiso 1 1 calc R . . C8 C 0.1465(5) 0.1383(3) 0.6570(4) 0.0635(12) Uani 1 1 d . . . H8A H 0.0942 0.1483 0.5754 0.076 Uiso 1 1 calc R . . H8B H 0.1664 0.0797 0.6641 0.076 Uiso 1 1 calc R . . C9 C 0.2923(5) 0.1838(3) 0.6680(4) 0.0575(10) Uani 1 1 d . . . H9A H 0.3331 0.1791 0.5900 0.069 Uiso 1 1 calc R . . H9B H 0.2733 0.2417 0.6813 0.069 Uiso 1 1 calc R . . C10 C 0.5345(5) 0.2118(3) 0.7725(4) 0.0660(12) Uani 1 1 d . . . H10A H 0.6107 0.1949 0.8362 0.099 Uiso 1 1 calc R . . H10B H 0.5030 0.2667 0.7894 0.099 Uiso 1 1 calc R . . H10C H 0.5727 0.2109 0.6940 0.099 Uiso 1 1 calc R . . C11 C 0.4578(5) 0.0714(2) 0.7380(4) 0.0568(10) Uani 1 1 d . . . H11A H 0.3764 0.0334 0.7344 0.085 Uiso 1 1 calc R . . H11B H 0.5351 0.0538 0.8003 0.085 Uiso 1 1 calc R . . H11C H 0.4951 0.0730 0.6592 0.085 Uiso 1 1 calc R . . Cl Cl 0.22840(10) 0.36356(5) 0.94022(8) 0.0447(2) Uani 1 1 d . . . O2 O 0.3221(4) 0.29599(18) 0.9766(3) 0.0854(11) Uani 1 1 d . . . O1 O 0.2301(5) 0.3767(3) 0.8115(3) 0.1005(12) Uani 1 1 d . . . O4 O 0.0808(4) 0.3424(3) 0.9539(4) 0.1106(14) Uani 1 1 d . . . O3 O 0.2780(6) 0.4330(2) 1.0053(4) 0.1340(19) 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 0.0354(2) 0.0428(2) 0.0349(2) -0.00146(18) -0.00120(16) 0.00186(18) N1 0.0375(15) 0.0307(14) 0.0396(16) -0.0013(11) -0.0002(12) 0.0010(11) N2 0.0418(16) 0.0413(16) 0.0397(16) -0.0036(13) -0.0083(13) 0.0050(13) N3 0.0512(17) 0.0384(16) 0.0397(16) -0.0007(13) 0.0057(13) -0.0009(13) N4 0.0395(16) 0.0541(19) 0.0531(19) -0.0029(15) -0.0045(14) 0.0008(15) N5 0.0317(14) 0.057(2) 0.0420(17) -0.0041(14) -0.0004(12) -0.0013(15) N6 0.053(2) 0.079(3) 0.083(3) -0.023(2) -0.0127(19) 0.0178(19) C1 0.0413(19) 0.0419(19) 0.042(2) -0.0023(16) -0.0033(16) 0.0021(15) C2 0.062(2) 0.049(2) 0.038(2) 0.0049(16) -0.0001(17) 0.0036(18) C3 0.066(3) 0.047(2) 0.049(2) 0.0052(17) 0.0166(19) -0.0016(19) C4 0.045(2) 0.051(2) 0.056(2) -0.0016(18) 0.0124(18) -0.0060(17) C5 0.0377(17) 0.0335(17) 0.0442(19) -0.0037(15) 0.0001(14) 0.0012(14) C6 0.0352(18) 0.0453(19) 0.049(2) -0.0069(16) -0.0066(16) 0.0033(15) C7 0.054(2) 0.063(3) 0.043(2) -0.0008(18) -0.0129(17) 0.0106(19) C8 0.068(3) 0.076(3) 0.042(2) -0.010(2) -0.013(2) 0.010(2) C9 0.078(3) 0.054(2) 0.040(2) 0.0053(18) 0.003(2) 0.011(2) C10 0.072(3) 0.065(3) 0.064(3) 0.005(2) 0.019(2) -0.021(2) C11 0.070(3) 0.048(2) 0.053(2) -0.0044(18) 0.010(2) 0.0130(19) Cl 0.0465(5) 0.0441(5) 0.0430(5) -0.0041(4) 0.0027(4) 0.0070(4) O2 0.088(2) 0.0449(17) 0.111(3) -0.0071(17) -0.036(2) 0.0110(15) O1 0.120(3) 0.126(3) 0.059(2) 0.024(2) 0.026(2) 0.021(2) O4 0.059(2) 0.176(4) 0.100(3) 0.003(3) 0.022(2) 0.003(2) O3 0.161(4) 0.061(2) 0.160(4) -0.053(2) -0.060(3) 0.021(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 Cu N4 1.968(3) . ? Cu N2 2.015(3) . ? Cu N1 2.037(3) . ? Cu N3 2.058(3) . ? Cu O2 2.434(3) . ? N1 C1 1.331(4) . ? N1 C5 1.351(4) . ? N2 C6 1.262(5) . ? N2 C7 1.471(4) . ? N3 C11 1.484(4) . ? N3 C10 1.485(5) . ? N3 C9 1.496(5) . ? N4 N5 1.188(4) . ? N5 N6 1.152(4) . ? C1 C2 1.386(5) . ? C2 C3 1.365(5) . ? C3 C4 1.392(5) . ? C4 C5 1.372(5) . ? C5 C6 1.472(5) . ? C7 C8 1.497(6) . ? C8 C9 1.508(6) . ? Cl O3 1.378(3) . ? Cl O4 1.409(4) . ? Cl O2 1.416(3) . ? Cl O1 1.420(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 N4 Cu N2 170.17(13) . . ? N4 Cu N1 89.81(12) . . ? N2 Cu N1 80.59(12) . . ? N4 Cu N3 93.56(13) . . ? N2 Cu N3 95.60(12) . . ? N1 Cu N3 170.70(11) . . ? N4 Cu O2 89.99(12) . . ? N2 Cu O2 92.42(11) . . ? N1 Cu O2 91.66(12) . . ? N3 Cu O2 97.00(12) . . ? C1 N1 C5 118.2(3) . . ? C1 N1 Cu 128.4(2) . . ? C5 N1 Cu 112.8(2) . . ? C6 N2 C7 119.7(3) . . ? C6 N2 Cu 113.7(2) . . ? C7 N2 Cu 126.7(3) . . ? C11 N3 C10 108.0(3) . . ? C11 N3 C9 109.2(3) . . ? C10 N3 C9 107.1(3) . . ? C11 N3 Cu 107.7(2) . . ? C10 N3 Cu 110.0(2) . . ? C9 N3 Cu 114.6(2) . . ? N5 N4 Cu 123.0(2) . . ? N6 N5 N4 176.7(4) . . ? N1 C1 C2 121.8(3) . . ? C3 C2 C1 119.7(3) . . ? C2 C3 C4 119.1(4) . . ? C5 C4 C3 118.0(3) . . ? N1 C5 C4 123.1(3) . . ? N1 C5 C6 112.9(3) . . ? C4 C5 C6 124.0(3) . . ? N2 C6 C5 119.2(3) . . ? N2 C7 C8 111.2(3) . . ? C7 C8 C9 114.1(3) . . ? N3 C9 C8 115.4(3) . . ? O3 Cl O4 113.7(3) . . ? O3 Cl O2 109.9(2) . . ? O4 Cl O2 109.2(2) . . ? O3 Cl O1 110.1(3) . . ? O4 Cl O1 105.3(3) . . ? O2 Cl O1 108.4(2) . . ? Cl O2 Cu 139.10(18) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.482 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.070 #END#