# Copyright The Royal Society of Chemistry, 1998 data_global _publ_contact_author ; Dr Jean-Pierre Costes Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex France ; _publ_contact_author_phone '(33) 0561333152' _publ_contact_author_fax '(33) 0561553003' _publ_contact_author_email costes@lcctoul.lcc-toulouse.fr _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_paper_number 'DALTON 7/08374B' _publ_section_title ; Bridging ability of a novel polydentate ligand (LH~2~) comprising an oxime function. Structures of a mononuclear precursor LNi and a dinuclear (Cu^II^/Cu^II^) complex. Magnetic properties of mononuclear (Ni^II^), (Cu^II^), dinuclear (Cu^II^/Cu^II^), (Ni^II^/Ni^II^), (Ni^II^/Cu^II^), (Cu^II^/Cr^III^) and trinuclear (Cu^II^/Cu^II^/Cu^II^), (Cu^II^/Mn^II^/Cu^II^), (Cu^II^/Zn^II^/Cu^II^) complexes. ; loop_ _publ_author_name _publ_author_address 'Costes, Jean-Pierre' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Dahan, Fran\,coise' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Dupuis, Arnaud' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Laurent, Jean-Pierre' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; data_(3) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C11 H17 N3 Ni O2' _chemical_formula_weight 281.99 _chemical_melting_point ? _chemical_compound_source ? 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' _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 7.2468(11) _cell_length_b 11.2244(12) _cell_length_c 14.6956(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.63(2) _cell_angle_gamma 90.00 _cell_volume 1187.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.58 _cell_measurement_theta_max 16.26 _exptl_crystal_description 'needle' _exptl_crystal_colour 'orange-red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method ? _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 1.627 _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_correction_T_min 0.3323 _exptl_absorpt_correction_T_max 0.6101 _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 'CAD4 Enraf-Nonius' _diffrn_measurement_method \w/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -0.2 _diffrn_reflns_number 2508 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.97 _reflns_number_total 2322 _reflns_number_observed 1262 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4-EXPRESS' _computing_cell_refinement 'CAD4-EXPRESS' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1996)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0199P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2322 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_obs 0.0238 _refine_ls_wR_factor_all 0.0532 _refine_ls_wR_factor_obs 0.0441 _refine_ls_goodness_of_fit_all 0.888 _refine_ls_goodness_of_fit_obs 1.029 _refine_ls_restrained_S_all 0.888 _refine_ls_restrained_S_obs 1.029 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni Ni 0.23028(5) 0.46270(3) 0.48094(2) 0.03660(11) Uani 1 d . . O1 O 0.2343(3) 0.30007(14) 0.47505(12) 0.0492(4) Uani 1 d . . C1 C 0.2915(4) 0.2307(2) 0.5438(2) 0.0489(7) Uani 1 d . . C2 C 0.3513(4) 0.2690(2) 0.6309(2) 0.0541(8) Uani 1 d . . H2 H 0.3848(4) 0.2107(2) 0.6747(2) 0.060 Uiso 1 calc R . C3 C 0.3664(3) 0.3876(2) 0.6598(2) 0.0408(6) Uani 1 d . . C4 C 0.2828(4) 0.1015(2) 0.5199(2) 0.0693(8) Uani 1 d . . H4A H 0.2379(4) 0.0923(2) 0.4563(2) 0.076 Uiso 1 calc R . H4B H 0.2002(4) 0.0616(2) 0.5565(2) 0.076 Uiso 1 calc R . H4C H 0.4046(4) 0.0673(2) 0.5317(2) 0.076 Uiso 1 calc R . C5 C 0.4417(4) 0.4106(3) 0.7586(2) 0.0610(8) Uani 1 d . . H5A H 0.4453(4) 0.4949(3) 0.7699(2) 0.067 Uiso 1 calc R . H5B H 0.5649(4) 0.3785(3) 0.7703(2) 0.067 Uiso 1 calc R . H5C H 0.3628(4) 0.3731(3) 0.7983(2) 0.067 Uiso 1 calc R . N1 N 0.3176(3) 0.4762(2) 0.60327(13) 0.0399(5) Uani 1 d . . C6 C 0.3442(4) 0.5992(2) 0.6366(2) 0.0485(7) Uani 1 d . . H6A H 0.4759(4) 0.6160(2) 0.6497(2) 0.053 Uiso 1 calc R . H6B H 0.2878(4) 0.6088(2) 0.6929(2) 0.053 Uiso 1 calc R . C7 C 0.2575(4) 0.6848(2) 0.5658(2) 0.0564(8) Uani 1 d . . H7A H 0.1427(4) 0.7159(2) 0.5843(2) 0.062 Uiso 1 calc R . H7B H 0.3410(4) 0.7511(2) 0.5597(2) 0.062 Uiso 1 calc R . N2 N 0.2206(3) 0.6240(2) 0.47998(14) 0.0326(5) Uani 1 d . . C8 C 0.1752(3) 0.6744(2) 0.4000(2) 0.0366(6) Uani 1 d . . C9 C 0.1324(3) 0.5920(2) 0.3273(2) 0.0362(6) Uani 1 d . . N3 N 0.1495(3) 0.4806(2) 0.35447(12) 0.0387(5) Uani 1 d . . O2 O 0.1150(3) 0.3933(2) 0.29744(11) 0.0611(6) Uani 1 d . . C10 C 0.1622(4) 0.8055(2) 0.3851(2) 0.0531(7) Uani 1 d . . H10A H 0.1964(4) 0.8460(2) 0.4421(2) 0.058 Uiso 1 calc R . H10B H 0.0371(4) 0.8263(2) 0.3619(2) 0.058 Uiso 1 calc R . H10C H 0.2447(4) 0.8288(2) 0.3417(2) 0.058 Uiso 1 calc R . C11 C 0.0708(4) 0.6257(2) 0.2305(2) 0.0612(8) Uani 1 d . . H11A H 0.0503(4) 0.5550(2) 0.1940(2) 0.067 Uiso 1 calc R . H11B H 0.1651(4) 0.6733(2) 0.2073(2) 0.067 Uiso 1 calc R . H11C H -0.0425(4) 0.6706(2) 0.2277(2) 0.067 Uiso 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 Ni 0.0375(2) 0.0365(2) 0.0358(2) -0.0012(2) 0.00432(12) 0.0006(2) O1 0.0645(12) 0.0379(10) 0.0453(10) -0.0016(9) 0.0070(9) 0.0013(10) C1 0.057(2) 0.0412(15) 0.050(2) 0.0082(13) 0.0143(15) 0.0112(14) C2 0.057(2) 0.051(2) 0.055(2) 0.0150(14) 0.007(2) 0.006(2) C3 0.0270(14) 0.055(2) 0.0401(15) 0.0051(13) 0.0035(11) -0.0012(13) C4 0.094(2) 0.039(2) 0.079(2) 0.015(2) 0.027(2) 0.011(2) C5 0.060(2) 0.084(2) 0.0380(15) 0.0080(14) 0.0030(14) -0.007(2) N1 0.0281(11) 0.0476(13) 0.0443(12) -0.0037(11) 0.0055(10) -0.0054(11) C6 0.055(2) 0.054(2) 0.036(2) -0.0059(13) 0.0022(14) -0.003(2) C7 0.063(2) 0.046(2) 0.057(2) -0.012(2) -0.007(2) 0.011(2) N2 0.0241(11) 0.0413(13) 0.0321(11) -0.0033(11) 0.0021(8) -0.0062(11) C8 0.0276(14) 0.0391(14) 0.044(2) -0.0025(12) 0.0060(12) 0.0015(12) C9 0.0268(14) 0.0417(15) 0.0392(15) 0.0019(12) 0.0005(11) 0.0022(12) N3 0.0373(12) 0.0459(14) 0.0317(11) -0.0089(10) -0.0006(9) -0.0006(11) O2 0.089(2) 0.0491(12) 0.0421(11) -0.0132(9) -0.0044(11) 0.0011(11) C10 0.060(2) 0.037(2) 0.062(2) 0.0028(13) 0.0072(14) 0.0028(14) C11 0.064(2) 0.071(2) 0.045(2) 0.0055(14) -0.0096(14) 0.012(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 Ni N2 1.811(2) . ? Ni O1 1.828(2) . ? Ni N1 1.842(2) . ? Ni N3 1.894(2) . ? O1 C1 1.304(3) . ? C1 C2 1.372(3) . ? C1 C4 1.492(3) . ? C2 C3 1.398(3) . ? C3 N1 1.318(3) . ? C3 C5 1.513(3) . ? N1 C6 1.470(3) . ? C6 C7 1.500(3) . ? C7 N2 1.432(3) . ? N2 C8 1.312(3) . ? C8 C9 1.420(3) . ? C8 C10 1.489(3) . ? C9 N3 1.314(3) . ? C9 C11 1.490(3) . ? N3 O2 1.295(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 N2 Ni O1 176.73(8) . . ? N2 Ni N1 86.20(9) . . ? O1 Ni N1 97.07(9) . . ? N2 Ni N3 83.06(9) . . ? O1 Ni N3 93.69(9) . . ? N1 Ni N3 168.99(9) . . ? C1 O1 Ni 124.4(2) . . ? O1 C1 C2 125.0(2) . . ? O1 C1 C4 113.4(2) . . ? C2 C1 C4 121.6(2) . . ? C1 C2 C3 125.9(2) . . ? N1 C3 C2 121.4(2) . . ? N1 C3 C5 121.1(2) . . ? C2 C3 C5 117.5(2) . . ? C3 N1 C6 118.9(2) . . ? C3 N1 Ni 126.2(2) . . ? C6 N1 Ni 114.9(2) . . ? N1 C6 C7 109.9(2) . . ? N2 C7 C6 109.1(2) . . ? C8 N2 C7 125.8(2) . . ? C8 N2 Ni 116.4(2) . . ? C7 N2 Ni 117.8(2) . . ? N2 C8 C9 113.8(2) . . ? N2 C8 C10 124.3(2) . . ? C9 C8 C10 121.9(2) . . ? N3 C9 C8 112.8(2) . . ? N3 C9 C11 122.6(2) . . ? C8 C9 C11 124.6(2) . . ? O2 N3 C9 121.3(2) . . ? O2 N3 Ni 124.7(2) . . ? C9 N3 Ni 114.0(2) . . ? _refine_diff_density_max 0.193 _refine_diff_density_min -0.181 _refine_diff_density_rms 0.050 #===END data_(8) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H32 Cl Cu2 N5 O7' _chemical_formula_weight 641.07 _chemical_melting_point ? _chemical_compound_source ? 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 P21/c _symmetry_space_group_name_H-M Monoclinic 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 13.401(2) _cell_length_b 9.582(2) _cell_length_c 22.149(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.26(2) _cell_angle_gamma 90.00 _cell_volume 2716.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.048 _cell_measurement_theta_max 14.862 _exptl_crystal_description 'parallelepiped' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method ? _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.680 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.7224 _exptl_absorpt_correction_T_max 0.9996 _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 ? _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -0.2 _diffrn_reflns_number 6139 _diffrn_reflns_av_R_equivalents 0.0123 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.97 _reflns_number_total 5898 _reflns_number_observed 4495 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4-EXPRESS' _computing_cell_refinement 'CAD4-EXPRESS' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1996)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.9168P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5898 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_obs 0.0314 _refine_ls_wR_factor_all 0.0874 _refine_ls_wR_factor_obs 0.0735 _refine_ls_goodness_of_fit_all 0.960 _refine_ls_goodness_of_fit_obs 0.934 _refine_ls_restrained_S_all 0.960 _refine_ls_restrained_S_obs 0.934 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.11632(2) 0.43741(3) 0.590662(14) 0.03547(9) Uani 1 d . . Cu2 Cu 0.34438(2) 0.47159(4) 0.545065(15) 0.04212(10) Uani 1 d . . O1 O 0.22355(14) 0.3174(2) 0.58390(10) 0.0480(5) Uani 1 d . . C1 C 0.2314(2) 0.1895(3) 0.60497(13) 0.0450(6) Uani 1 d . . C2 C 0.1738(2) 0.1302(3) 0.63899(14) 0.0525(7) Uani 1 d . . H2 H 0.1894(2) 0.0377(3) 0.65088(14) 0.058 Uiso 1 calc R . C3 C 0.0919(3) 0.1927(3) 0.65880(15) 0.0528(7) Uani 1 d . . C4 C 0.3146(3) 0.1050(3) 0.5894(2) 0.0693(10) Uani 1 d . . H4A H 0.3481(3) 0.1607(3) 0.5650(2) 0.076 Uiso 1 calc R . H4B H 0.2835(3) 0.0244(3) 0.5653(2) 0.076 Uiso 1 calc R . H4C H 0.3653(3) 0.0758(3) 0.6278(2) 0.076 Uiso 1 calc R . C5 C 0.0486(4) 0.1084(4) 0.7022(2) 0.0810(13) Uani 1 d . . H5A H -0.0058(4) 0.1602(4) 0.7121(2) 0.089 Uiso 1 calc R . H5B H 0.1032(4) 0.0886(4) 0.7405(2) 0.089 Uiso 1 calc R . H5C H 0.0206(4) 0.0224(4) 0.6819(2) 0.089 Uiso 1 calc R . N1 N 0.0566(2) 0.3159(2) 0.63911(12) 0.0485(6) Uani 1 d . . C6 C -0.0186(3) 0.3865(4) 0.6643(2) 0.0722(10) Uani 1 d . . H6A H 0.0165(3) 0.4193(4) 0.7067(2) 0.079 Uiso 1 calc R . H6B H -0.0723(3) 0.3209(4) 0.6668(2) 0.079 Uiso 1 calc R . C7 C -0.0685(2) 0.5081(3) 0.62365(14) 0.0502(7) Uani 1 d . . H7A H -0.1346(2) 0.4795(3) 0.59424(14) 0.055 Uiso 1 calc R . H7B H -0.0821(2) 0.5824(3) 0.64992(14) 0.055 Uiso 1 calc R . N2 N 0.0014(2) 0.5582(2) 0.58884(10) 0.0381(5) Uani 1 d . . C8 C 0.0025(2) 0.6780(3) 0.56466(12) 0.0395(6) Uani 1 d . . C9 C 0.0867(2) 0.7004(3) 0.53570(12) 0.0371(5) Uani 1 d . . C10 C -0.0739(2) 0.7920(4) 0.5645(2) 0.0630(9) Uani 1 d . . H10A H -0.1231(2) 0.7601(4) 0.5853(2) 0.069 Uiso 1 calc R . H10B H -0.1103(2) 0.8171(4) 0.5216(2) 0.069 Uiso 1 calc R . H10C H -0.0372(2) 0.8719(4) 0.5864(2) 0.069 Uiso 1 calc R . C11 C 0.1002(2) 0.8330(3) 0.5036(2) 0.0542(7) Uani 1 d . . H11A H 0.1596(2) 0.8250(3) 0.4881(2) 0.060 Uiso 1 calc R . H11B H 0.1108(2) 0.9087(3) 0.5332(2) 0.060 Uiso 1 calc R . H11C H 0.0387(2) 0.8504(3) 0.4689(2) 0.060 Uiso 1 calc R . N3 N 0.1509(2) 0.5968(2) 0.54236(9) 0.0355(4) Uani 1 d . . O3 O 0.22884(14) 0.6057(2) 0.51712(9) 0.0443(4) Uani 1 d . . O2 O 0.3132(2) 0.4051(3) 0.46208(10) 0.0620(6) Uani 1 d . . C12 C 0.3628(2) 0.3090(3) 0.44098(13) 0.0487(7) Uani 1 d . . C13 C 0.3146(2) 0.2598(4) 0.37901(15) 0.0580(8) Uani 1 d . . H13 H 0.2509(2) 0.2981(4) 0.35606(15) 0.064 Uiso 1 calc R . C14 C 0.3578(3) 0.1589(4) 0.3516(2) 0.0636(9) Uani 1 d . . H14 H 0.3231(3) 0.1280(4) 0.3110(2) 0.070 Uiso 1 calc R . C15 C 0.4532(3) 0.1027(4) 0.3841(2) 0.0688(10) Uani 1 d . . H15 H 0.4834(3) 0.0341(4) 0.3655(2) 0.076 Uiso 1 calc R . C16 C 0.5030(3) 0.1482(4) 0.4437(2) 0.0615(8) Uani 1 d . . H16 H 0.5669(3) 0.1084(4) 0.4653(2) 0.068 Uiso 1 calc R . C17 C 0.4612(2) 0.2538(3) 0.47427(13) 0.0461(6) Uani 1 d . . C18 C 0.5201(2) 0.2957(3) 0.53835(14) 0.0470(7) Uani 1 d . . C19 C 0.6319(2) 0.2483(4) 0.5645(2) 0.0645(9) Uani 1 d . . H19A H 0.6605(2) 0.2835(4) 0.6067(2) 0.071 Uiso 1 calc R . H19B H 0.6720(2) 0.2832(4) 0.5383(2) 0.071 Uiso 1 calc R . H19C H 0.6344(2) 0.1482(4) 0.5652(2) 0.071 Uiso 1 calc R . N4 N 0.4784(2) 0.3722(3) 0.57226(10) 0.0462(5) Uani 1 d . . C20 C 0.5383(2) 0.4090(4) 0.63762(14) 0.0589(8) Uani 1 d . . H20A H 0.5909(2) 0.4782(4) 0.63715(14) 0.065 Uiso 1 calc R . H20B H 0.5735(2) 0.3268(4) 0.65949(14) 0.065 Uiso 1 calc R . C21 C 0.4651(3) 0.4665(4) 0.67163(15) 0.0660(9) Uani 1 d . . H21 H 0.4246(3) 0.3886(4) 0.68094(15) 0.073 Uiso 1 calc R . C22 C 0.5253(3) 0.5337(5) 0.7338(2) 0.0871(14) Uani 1 d . . H22A H 0.4771(3) 0.5699(5) 0.7544(2) 0.096 Uiso 1 calc R . H22B H 0.5675(3) 0.6083(5) 0.7259(2) 0.096 Uiso 1 calc R . H22C H 0.5694(3) 0.4652(5) 0.7605(2) 0.096 Uiso 1 calc R . N5 N 0.3929(2) 0.5620(3) 0.62939(11) 0.0554(6) Uani 1 d . . H5D H 0.4251(2) 0.6432(3) 0.62676(11) 0.061 Uiso 1 calc R . H5E H 0.3382(2) 0.5797(3) 0.64396(11) 0.061 Uiso 1 calc R . Cl Cl 0.21555(6) 0.69545(9) 0.72300(4) 0.0587(2) Uani 1 d . . O4 O 0.2198(2) 0.5572(3) 0.69854(12) 0.0731(7) Uani 1 d . . O5 O 0.1102(2) 0.7445(4) 0.7047(2) 0.1035(11) Uani 1 d . . O6 O 0.2705(3) 0.7814(3) 0.6916(2) 0.1058(11) Uani 1 d . . O7 O 0.2579(3) 0.6991(4) 0.78875(13) 0.1204(13) Uani 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 0.0362(2) 0.0311(2) 0.0429(2) 0.00280(12) 0.01766(13) 0.00915(12) Cu2 0.0352(2) 0.0500(2) 0.0435(2) 0.00255(14) 0.01530(13) 0.01390(14) O1 0.0454(10) 0.0363(10) 0.0691(13) 0.0110(9) 0.0274(9) 0.0148(8) C1 0.0463(14) 0.0362(14) 0.052(2) 0.0049(12) 0.0144(12) 0.0107(11) C2 0.069(2) 0.0341(14) 0.060(2) 0.0077(12) 0.0271(15) 0.0143(13) C3 0.069(2) 0.0406(15) 0.060(2) 0.0065(13) 0.035(2) 0.0050(14) C4 0.060(2) 0.042(2) 0.115(3) 0.014(2) 0.040(2) 0.0190(15) C5 0.127(3) 0.051(2) 0.095(3) 0.027(2) 0.079(3) 0.019(2) N1 0.0578(14) 0.0373(12) 0.0613(14) 0.0009(10) 0.0344(12) 0.0045(10) C6 0.077(2) 0.061(2) 0.091(3) 0.007(2) 0.044(2) 0.015(2) C7 0.0378(13) 0.067(2) 0.050(2) -0.0006(14) 0.0197(12) 0.0040(13) N2 0.0349(10) 0.0417(12) 0.0394(11) -0.0010(9) 0.0135(9) 0.0078(9) C8 0.0340(12) 0.0434(14) 0.0384(13) -0.0063(11) 0.0067(10) 0.0089(11) C9 0.0333(12) 0.0332(12) 0.0439(13) -0.0019(10) 0.0101(10) 0.0081(10) C10 0.056(2) 0.061(2) 0.078(2) 0.008(2) 0.029(2) 0.030(2) C11 0.060(2) 0.0357(14) 0.069(2) 0.0091(13) 0.0224(15) 0.0093(13) N3 0.0381(10) 0.0347(10) 0.0352(10) -0.0010(8) 0.0133(8) 0.0080(8) O3 0.0447(10) 0.0451(10) 0.0509(10) 0.0091(8) 0.0263(8) 0.0147(8) O2 0.0483(11) 0.084(2) 0.0513(11) -0.0109(11) 0.0116(9) 0.0327(11) C12 0.0408(14) 0.061(2) 0.050(2) -0.0036(13) 0.0222(12) 0.0123(13) C13 0.047(2) 0.074(2) 0.055(2) -0.011(2) 0.0183(13) 0.0149(15) C14 0.067(2) 0.067(2) 0.058(2) -0.018(2) 0.021(2) 0.013(2) C15 0.071(2) 0.070(2) 0.068(2) -0.012(2) 0.026(2) 0.027(2) C16 0.057(2) 0.069(2) 0.060(2) 0.002(2) 0.0195(15) 0.032(2) C17 0.0440(14) 0.053(2) 0.0480(15) 0.0097(13) 0.0232(12) 0.0175(12) C18 0.0378(13) 0.053(2) 0.059(2) 0.0209(13) 0.0288(12) 0.0162(12) C19 0.044(2) 0.091(3) 0.066(2) 0.017(2) 0.0261(14) 0.030(2) N4 0.0383(11) 0.0598(15) 0.0447(12) 0.0139(11) 0.0188(9) 0.0149(10) C20 0.044(2) 0.080(2) 0.050(2) 0.008(2) 0.0108(13) 0.015(2) C21 0.061(2) 0.090(3) 0.045(2) -0.001(2) 0.0140(14) 0.011(2) C22 0.084(3) 0.125(4) 0.040(2) -0.013(2) -0.001(2) 0.028(3) N5 0.0489(13) 0.069(2) 0.0481(13) -0.0034(12) 0.0135(11) 0.0149(12) Cl 0.0552(4) 0.0620(5) 0.0556(4) -0.0157(4) 0.0114(3) -0.0074(3) O4 0.075(2) 0.0626(15) 0.073(2) -0.0129(12) 0.0082(13) 0.0017(12) O5 0.069(2) 0.116(3) 0.114(2) -0.051(2) 0.009(2) 0.017(2) O6 0.123(3) 0.055(2) 0.177(3) 0.002(2) 0.101(3) -0.008(2) O7 0.154(3) 0.113(3) 0.058(2) -0.026(2) -0.023(2) 0.003(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 O1 1.881(2) . ? Cu1 N1 1.913(2) . ? Cu1 N2 1.917(2) . ? Cu1 N3 1.996(2) . ? Cu2 O2 1.872(2) . ? Cu2 N4 1.963(2) . ? Cu2 O3 1.965(2) . ? Cu2 N5 1.985(2) . ? Cu2 O1 2.524(2) . ? O1 C1 1.304(3) . ? C1 C2 1.354(4) . ? C1 C4 1.498(4) . ? C2 C3 1.429(4) . ? C3 N1 1.298(4) . ? C3 C5 1.499(4) . ? N1 C6 1.455(4) . ? C6 C7 1.503(5) . ? C7 N2 1.460(3) . ? N2 C8 1.269(3) . ? C8 C9 1.469(3) . ? C8 C10 1.496(3) . ? C9 N3 1.294(3) . ? C9 C11 1.492(4) . ? N3 O3 1.325(3) . ? O2 C12 1.301(3) . ? C12 C13 1.413(4) . ? C12 C17 1.410(4) . ? C13 C14 1.359(4) . ? C14 C15 1.377(5) . ? C15 C16 1.362(5) . ? C16 C17 1.421(4) . ? C17 C18 1.461(4) . ? C18 N4 1.289(3) . ? C18 C19 1.507(4) . ? N4 C20 1.475(4) . ? C20 C21 1.507(4) . ? C21 N5 1.453(4) . ? C21 C22 1.518(5) . ? Cl O7 1.398(3) . ? Cl O6 1.417(3) . ? Cl O5 1.428(3) . ? Cl O4 1.439(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 O1 Cu1 N1 97.43(9) . . ? O1 Cu1 N2 174.44(9) . . ? N1 Cu1 N2 84.95(10) . . ? O1 Cu1 N3 96.93(8) . . ? N1 Cu1 N3 165.64(9) . . ? N2 Cu1 N3 80.78(9) . . ? O2 Cu2 N4 93.07(9) . . ? O2 Cu2 O3 89.29(8) . . ? N4 Cu2 O3 167.79(10) . . ? O2 Cu2 N5 171.08(12) . . ? N4 Cu2 N5 84.76(10) . . ? O3 Cu2 N5 91.06(9) . . ? O2 Cu2 O1 98.99(10) . . ? N4 Cu2 O1 103.44(8) . . ? O3 Cu2 O1 87.99(7) . . ? N5 Cu2 O1 89.94(10) . . ? C1 O1 Cu1 121.9(2) . . ? C1 O1 Cu2 132.8(2) . . ? Cu1 O1 Cu2 104.57(8) . . ? O1 C1 C2 126.5(2) . . ? O1 C1 C4 114.3(3) . . ? C2 C1 C4 119.2(3) . . ? C1 C2 C3 127.7(3) . . ? N1 C3 C2 121.0(3) . . ? N1 C3 C5 122.2(3) . . ? C2 C3 C5 116.8(3) . . ? C3 N1 C6 121.3(3) . . ? C3 N1 Cu1 124.8(2) . . ? C6 N1 Cu1 112.6(2) . . ? N1 C6 C7 111.5(3) . . ? N2 C7 C6 109.2(2) . . ? C8 N2 C7 127.6(2) . . ? C8 N2 Cu1 116.4(2) . . ? C7 N2 Cu1 115.3(2) . . ? N2 C8 C9 115.0(2) . . ? N2 C8 C10 124.6(3) . . ? C9 C8 C10 120.4(2) . . ? N3 C9 C8 114.2(2) . . ? N3 C9 C11 122.5(2) . . ? C8 C9 C11 123.3(2) . . ? C9 N3 O3 118.9(2) . . ? C9 N3 Cu1 113.3(2) . . ? O3 N3 Cu1 127.78(15) . . ? N3 O3 Cu2 118.08(14) . . ? C12 O2 Cu2 127.2(2) . . ? O2 C12 C13 116.7(3) . . ? O2 C12 C17 125.2(3) . . ? C13 C12 C17 118.0(3) . . ? C14 C13 C12 122.6(3) . . ? C13 C14 C15 119.8(3) . . ? C16 C15 C14 119.5(3) . . ? C15 C16 C17 122.7(3) . . ? C16 C17 C12 117.3(3) . . ? C16 C17 C18 118.9(2) . . ? C12 C17 C18 123.8(2) . . ? N4 C18 C17 121.4(2) . . ? N4 C18 C19 120.0(3) . . ? C17 C18 C19 118.6(3) . . ? C18 N4 C20 120.3(2) . . ? C18 N4 Cu2 127.7(2) . . ? C20 N4 Cu2 111.5(2) . . ? N4 C20 C21 109.4(2) . . ? N5 C21 C20 108.4(3) . . ? N5 C21 C22 113.0(3) . . ? C20 C21 C22 111.0(3) . . ? C21 N5 Cu2 107.5(2) . . ? O7 Cl O6 112.8(2) . . ? O7 Cl O5 110.5(2) . . ? O6 Cl O5 106.4(2) . . ? O7 Cl O4 111.5(2) . . ? O6 Cl O4 105.4(2) . . ? O5 Cl O4 110.0(2) . . ? _refine_diff_density_max 0.275 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.062 #===END