# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_Rodriguez_Dieguez _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ; Structural and Magnetic Properties and Biological Activity against T. Cruzi of Three Novel Multidimensional Complexes with 5-Methyl-1,2,4-Triazolo[1,5-a]Pyrimidin-7(4H)-one ; _publ_contact_author_name 'Antonio Rodriquez-Dieguez' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, c/ Severo Ochoa s/n, 18071 Granada, Spain ; _publ_contact_author_email antonio5@ugr.es _publ_contact_author_phone '34 958 243236' _publ_contact_author_fax '34 958 248526' loop_ _publ_author_name _publ_author_address A.B.Caballero ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, c/ Severo Ochoa s/n, 18071 Granada, Spain ; A.Rodriquez-Dieguez ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, c/ Severo Ochoa s/n, 18071 Granada, Spain ; L.Lezama ; Departamento de Qu\'imica Inorg\'anica, Universidad del Pa\'is Vasco, Apdo. 644, E-48080, Bilbao, Spain ; E.Barea ; Instituto de Biolog\'ia Molecular y Celular, Universidad Miguel Hern\'andez, 03202 Elche, Spain ; J.M.Salas ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, c/ Severo Ochoa s/n, 18071 Granada, Spain ; data_compound1 _database_code_depnum_ccdc_archive 'CCDC 780316' #TrackingRef '- Rodriguez_Dieguez.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 Cl2 Cu N8 O14' _chemical_formula_weight 634.80 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' 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' 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 P21/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 14.166(5) _cell_length_b 13.435(5) _cell_length_c 13.405(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.357(5) _cell_angle_gamma 90.00 _cell_volume 2492.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2804 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 23.35 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13111 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4355 _reflns_number_gt 3759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker APEXII' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1154P)^2^+1.7200P] 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 4355 _refine_ls_number_parameters 376 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _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 Cu1 Cu 0.34513(3) 0.57228(3) 0.25674(3) 0.0352(2) Uani 1 1 d . . . O1W O 0.2612(3) 0.6951(3) 0.2196(3) 0.0577(9) Uani 1 1 d . . . O2W O 0.4725(3) 0.6685(3) 0.2841(3) 0.0586(9) Uani 1 1 d D . . O3W O 0.4170(4) 0.4479(3) 0.2916(3) 0.0718(13) Uani 1 1 d . . . O71A O 0.1932(2) 0.4756(3) 0.1780(2) 0.0541(8) Uani 1 1 d . . . O71B O 0.2179(3) 0.5342(3) 0.6836(2) 0.0773(11) Uani 1 1 d . . . N3B N 0.3187(2) 0.5748(2) 0.3953(2) 0.0378(8) Uani 1 1 d . . . N3A N 0.3613(3) 0.5585(3) -0.0532(3) 0.0449(9) Uani 1 1 d . . . N1B N 0.3389(3) 0.6099(4) 0.5626(3) 0.0563(10) Uani 1 1 d . . . N1A N 0.3486(2) 0.5554(3) 0.1106(3) 0.0399(8) Uani 1 1 d . . . N8B N 0.2606(2) 0.5473(3) 0.5308(2) 0.0419(8) Uani 1 1 d . . . N8A N 0.2688(2) 0.5126(2) 0.0503(2) 0.0348(7) Uani 1 1 d . . . N4B N 0.1800(3) 0.4680(3) 0.3848(3) 0.0398(9) Uani 1 1 d . . . N4A N 0.2060(3) 0.4816(3) -0.1199(3) 0.0414(8) Uani 1 1 d . . . C2B C 0.3693(3) 0.6232(4) 0.4796(3) 0.0488(11) Uani 1 1 d . . . H2B H 0.4223 0.6632 0.4773 0.059 Uiso 1 1 calc R . . C2A C 0.4002(3) 0.5817(3) 0.0444(3) 0.0459(10) Uani 1 1 d . . . H2A H 0.4593 0.6140 0.0636 0.055 Uiso 1 1 calc R . . C3AB C 0.2503(3) 0.5279(3) 0.4307(3) 0.0355(8) Uani 1 1 d . . . C3AA C 0.2782(3) 0.5165(3) -0.0477(3) 0.0393(9) Uani 1 1 d . . . C5B C 0.1181(3) 0.4251(3) 0.4382(3) 0.0443(10) Uani 1 1 d . . . C5A C 0.1248(3) 0.4434(3) -0.0936(3) 0.0413(9) Uani 1 1 d . . . C51B C 0.0438(4) 0.3572(4) 0.3796(4) 0.0645(14) Uani 1 1 d . . . H51A H 0.0276 0.3074 0.4245 0.097 Uiso 1 1 calc R . . H51B H 0.0687 0.3256 0.3264 0.097 Uiso 1 1 calc R . . H51C H -0.0130 0.3947 0.3499 0.097 Uiso 1 1 calc R . . C51A C 0.0473(4) 0.4105(4) -0.1822(4) 0.0616(13) Uani 1 1 d . . . H51D H -0.0091 0.3912 -0.1581 0.092 Uiso 1 1 calc R . . H51E H 0.0702 0.3548 -0.2153 0.092 Uiso 1 1 calc R . . H51F H 0.0314 0.4643 -0.2299 0.092 Uiso 1 1 calc R . . C6B C 0.1299(4) 0.4459(4) 0.5396(3) 0.0512(11) Uani 1 1 d . . . H6B H 0.0880 0.4162 0.5754 0.061 Uiso 1 1 calc R . . C6A C 0.1178(3) 0.4370(3) 0.0052(3) 0.0430(10) Uani 1 1 d . . . H6A H 0.0630 0.4080 0.0204 0.052 Uiso 1 1 calc R . . C7B C 0.2013(3) 0.5093(4) 0.5930(3) 0.0519(11) Uani 1 1 d . . . C7A C 0.1904(3) 0.4725(3) 0.0859(3) 0.0404(9) Uani 1 1 d . . . Cl2 Cl 0.10913(8) 0.76551(8) 0.42001(8) 0.0476(3) Uani 1 1 d . . . O8 O 0.1295(4) 0.7969(4) 0.5248(3) 0.1089(17) Uani 1 1 d . . . O7 O 0.0365(4) 0.8300(4) 0.3706(4) 0.1121(18) Uani 1 1 d . . . O6 O 0.1921(5) 0.7798(4) 0.3816(6) 0.131(2) Uani 1 1 d . . . O9 O 0.0803(3) 0.6657(3) 0.4103(4) 0.0869(13) Uani 1 1 d . . . Cl1 Cl 0.35204(10) 0.26059(10) 0.47681(14) 0.0734(4) Uani 1 1 d . . . O3 O 0.4031(7) 0.1835(5) 0.5236(6) 0.179(4) Uani 1 1 d . . . O2 O 0.2643(5) 0.2424(5) 0.4490(13) 0.267(8) Uani 1 1 d . . . O4 O 0.3749(5) 0.3541(4) 0.5138(9) 0.207(5) Uani 1 1 d . . . O5 O 0.3816(19) 0.2702(14) 0.3944(14) 0.397(13) Uani 1 1 d . . . O4W O 0.5647(3) 0.3730(3) 0.2241(3) 0.0483(8) Uani 1 1 d . . . H4B H 0.178(3) 0.463(4) 0.339(4) 0.029(13) Uiso 1 1 d . . . H31W H 0.454(5) 0.438(5) 0.272(5) 0.06(2) Uiso 1 1 d . . . H22W H 0.465(3) 0.726(4) 0.298(4) 0.044(14) Uiso 1 1 d . . . H4A H 0.206(3) 0.489(3) -0.176(3) 0.031(11) Uiso 1 1 d . . . H41W H 0.596(5) 0.388(5) 0.268(6) 0.08(3) Uiso 1 1 d . . . H21W H 0.528(3) 0.653(5) 0.323(4) 0.09(2) Uiso 1 1 d D . . H11W H 0.236(4) 0.718(4) 0.260(5) 0.062(18) Uiso 1 1 d . . . H42W H 0.581(5) 0.397(5) 0.178(6) 0.08(2) Uiso 1 1 d . . . H32W H 0.385(5) 0.415(4) 0.317(5) 0.07(2) Uiso 1 1 d . . . H12W H 0.237(5) 0.711(6) 0.157(6) 0.10(2) Uiso 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 0.0390(3) 0.0453(3) 0.0230(3) 0.00096(17) 0.0104(2) 0.00116(19) O1W 0.065(2) 0.069(2) 0.040(2) 0.0058(17) 0.0131(17) 0.0211(18) O2W 0.049(2) 0.056(2) 0.067(2) 0.0003(18) 0.0036(17) -0.0074(16) O3W 0.090(3) 0.069(3) 0.073(3) 0.029(2) 0.053(3) 0.035(2) O71A 0.0606(19) 0.080(2) 0.0268(16) -0.0022(14) 0.0206(13) -0.0151(17) O71B 0.097(3) 0.116(3) 0.0242(17) -0.0059(18) 0.0224(17) -0.026(2) N3B 0.0390(18) 0.053(2) 0.0220(16) -0.0024(13) 0.0082(13) 0.0001(14) N3A 0.045(2) 0.062(2) 0.0314(19) 0.0024(15) 0.0164(15) -0.0055(16) N1B 0.053(2) 0.086(3) 0.0283(19) -0.0040(19) 0.0049(16) -0.018(2) N1A 0.0418(19) 0.052(2) 0.0275(17) -0.0005(14) 0.0118(14) -0.0036(15) N8B 0.0434(19) 0.061(2) 0.0214(16) -0.0034(15) 0.0076(14) -0.0035(16) N8A 0.0397(17) 0.0439(18) 0.0233(15) 0.0002(13) 0.0124(13) -0.0028(14) N4B 0.049(2) 0.052(2) 0.0205(19) -0.0038(16) 0.0118(16) -0.0023(16) N4A 0.055(2) 0.050(2) 0.0217(18) 0.0006(15) 0.0130(15) -0.0051(16) C2B 0.044(2) 0.074(3) 0.029(2) -0.007(2) 0.0069(17) -0.013(2) C2A 0.042(2) 0.064(3) 0.034(2) 0.0000(19) 0.0146(18) -0.0064(19) C3AB 0.039(2) 0.046(2) 0.0222(18) 0.0039(15) 0.0085(15) 0.0057(17) C3AA 0.048(2) 0.044(2) 0.029(2) 0.0023(16) 0.0154(17) 0.0038(18) C5B 0.049(2) 0.049(2) 0.037(2) 0.0017(17) 0.0151(19) -0.0014(18) C5A 0.051(2) 0.041(2) 0.032(2) 0.0010(16) 0.0076(18) -0.0050(17) C51B 0.075(3) 0.071(3) 0.053(3) -0.008(2) 0.025(3) -0.026(3) C51A 0.065(3) 0.070(3) 0.045(3) -0.003(2) 0.000(2) -0.021(2) C6B 0.058(3) 0.068(3) 0.034(2) 0.006(2) 0.024(2) -0.006(2) C6A 0.047(2) 0.045(2) 0.040(2) 0.0005(17) 0.0164(19) -0.0077(18) C7B 0.062(3) 0.073(3) 0.024(2) 0.0023(19) 0.0148(19) -0.007(2) C7A 0.046(2) 0.050(2) 0.029(2) -0.0009(17) 0.0167(17) -0.0022(18) Cl2 0.0540(6) 0.0439(6) 0.0476(6) -0.0028(4) 0.0167(5) 0.0036(4) O8 0.122(4) 0.132(4) 0.060(3) -0.019(3) -0.009(3) -0.022(3) O7 0.126(4) 0.112(4) 0.093(3) 0.011(3) 0.011(3) 0.063(3) O6 0.138(5) 0.092(3) 0.203(7) -0.041(4) 0.124(5) -0.022(3) O9 0.084(3) 0.057(2) 0.120(4) -0.013(2) 0.021(3) -0.0135(19) Cl1 0.0606(8) 0.0564(8) 0.1024(12) 0.0173(7) 0.0158(7) -0.0009(6) O3 0.249(9) 0.090(4) 0.169(7) 0.009(4) -0.018(6) 0.057(5) O2 0.078(4) 0.099(5) 0.62(2) -0.073(8) 0.067(8) -0.023(4) O4 0.128(5) 0.069(3) 0.356(13) -0.011(5) -0.099(6) 0.005(3) O5 0.66(4) 0.33(2) 0.278(18) 0.093(15) 0.28(2) -0.01(2) O4W 0.0507(19) 0.066(2) 0.0284(17) 0.0005(16) 0.0096(15) 0.0004(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3W 1.961(4) . ? Cu1 N3B 1.972(3) . ? Cu1 N1A 1.984(3) . ? Cu1 O1W 2.032(4) . ? Cu1 O2W 2.185(4) . ? O1W H11W 0.77(6) . ? O1W H12W 0.86(8) . ? O2W H22W 0.81(5) . ? O2W H21W 0.87(2) . ? O3W H31W 0.64(7) . ? O3W H32W 0.77(6) . ? O71A C7A 1.228(5) . ? O71B C7B 1.232(5) . ? N3B C3AB 1.326(5) . ? N3B C2B 1.367(5) . ? N3A C3AA 1.322(5) . ? N3A C2A 1.342(6) . ? N1B C2B 1.288(5) . ? N1B N8B 1.385(5) . ? N1A C2A 1.313(5) . ? N1A N8A 1.367(5) . ? N8B C3AB 1.343(5) . ? N8B C7B 1.401(5) . ? N8A C3AA 1.349(5) . ? N8A C7A 1.406(5) . ? N4B C3AB 1.326(6) . ? N4B C5B 1.371(6) . ? N4B H4B 0.61(5) . ? N4A C3AA 1.334(5) . ? N4A C5A 1.372(6) . ? N4A H4A 0.77(4) . ? C2B H2B 0.9300 . ? C2A H2A 0.9300 . ? C5B C6B 1.364(6) . ? C5B C51B 1.484(7) . ? C5A C6A 1.352(6) . ? C5A C51A 1.501(6) . ? C51B H51A 0.9600 . ? C51B H51B 0.9600 . ? C51B H51C 0.9600 . ? C51A H51D 0.9600 . ? C51A H51E 0.9600 . ? C51A H51F 0.9600 . ? C6B C7B 1.396(7) . ? C6B H6B 0.9300 . ? C6A C7A 1.407(6) . ? C6A H6A 0.9300 . ? Cl2 O6 1.394(5) . ? Cl2 O7 1.399(5) . ? Cl2 O9 1.399(4) . ? Cl2 O8 1.436(5) . ? Cl1 O2 1.243(7) . ? Cl1 O5 1.269(14) . ? Cl1 O3 1.340(6) . ? Cl1 O4 1.363(6) . ? O4W H41W 0.68(7) . ? O4W H42W 0.77(7) . ? 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 O3W Cu1 N3B 89.04(16) . . ? O3W Cu1 N1A 90.97(17) . . ? N3B Cu1 N1A 169.16(14) . . ? O3W Cu1 O1W 175.7(2) . . ? N3B Cu1 O1W 89.88(15) . . ? N1A Cu1 O1W 89.30(16) . . ? O3W Cu1 O2W 95.5(2) . . ? N3B Cu1 O2W 98.50(15) . . ? N1A Cu1 O2W 92.29(14) . . ? O1W Cu1 O2W 88.82(16) . . ? Cu1 O1W H11W 119(4) . . ? Cu1 O1W H12W 122(5) . . ? H11W O1W H12W 116(7) . . ? Cu1 O2W H22W 117(4) . . ? Cu1 O2W H21W 125(5) . . ? H22W O2W H21W 104(6) . . ? Cu1 O3W H31W 120(6) . . ? Cu1 O3W H32W 106(5) . . ? H31W O3W H32W 132(7) . . ? C3AB N3B C2B 102.9(3) . . ? C3AB N3B Cu1 129.1(3) . . ? C2B N3B Cu1 128.0(3) . . ? C3AA N3A C2A 103.2(3) . . ? C2B N1B N8B 102.2(3) . . ? C2A N1A N8A 102.9(3) . . ? C2A N1A Cu1 140.5(3) . . ? N8A N1A Cu1 116.1(2) . . ? C3AB N8B N1B 109.5(3) . . ? C3AB N8B C7B 125.0(4) . . ? N1B N8B C7B 125.5(3) . . ? C3AA N8A N1A 108.5(3) . . ? C3AA N8A C7A 126.5(3) . . ? N1A N8A C7A 125.0(3) . . ? C3AB N4B C5B 120.9(4) . . ? C3AB N4B H4B 114(5) . . ? C5B N4B H4B 125(5) . . ? C3AA N4A C5A 120.0(3) . . ? C3AA N4A H4A 121(3) . . ? C5A N4A H4A 119(3) . . ? N1B C2B N3B 115.9(4) . . ? N1B C2B H2B 122.1 . . ? N3B C2B H2B 122.1 . . ? N1A C2A N3A 115.1(4) . . ? N1A C2A H2A 122.5 . . ? N3A C2A H2A 122.5 . . ? N3B C3AB N4B 131.0(3) . . ? N3B C3AB N8B 109.5(3) . . ? N4B C3AB N8B 119.5(4) . . ? N3A C3AA N4A 131.5(4) . . ? N3A C3AA N8A 110.2(4) . . ? N4A C3AA N8A 118.3(4) . . ? C6B C5B N4B 118.6(4) . . ? C6B C5B C51B 125.2(4) . . ? N4B C5B C51B 116.2(4) . . ? C6A C5A N4A 121.1(4) . . ? C6A C5A C51A 124.2(4) . . ? N4A C5A C51A 114.7(4) . . ? C5B C51B H51A 109.5 . . ? C5B C51B H51B 109.5 . . ? H51A C51B H51B 109.5 . . ? C5B C51B H51C 109.5 . . ? H51A C51B H51C 109.5 . . ? H51B C51B H51C 109.5 . . ? C5A C51A H51D 109.5 . . ? C5A C51A H51E 109.5 . . ? H51D C51A H51E 109.5 . . ? C5A C51A H51F 109.5 . . ? H51D C51A H51F 109.5 . . ? H51E C51A H51F 109.5 . . ? C5B C6B C7B 123.9(4) . . ? C5B C6B H6B 118.1 . . ? C7B C6B H6B 118.1 . . ? C5A C6A C7A 122.5(4) . . ? C5A C6A H6A 118.8 . . ? C7A C6A H6A 118.8 . . ? O71B C7B C6B 129.4(4) . . ? O71B C7B N8B 118.4(4) . . ? C6B C7B N8B 112.2(4) . . ? O71A C7A N8A 118.1(4) . . ? O71A C7A C6A 130.2(4) . . ? N8A C7A C6A 111.7(3) . . ? O6 Cl2 O7 109.5(4) . . ? O6 Cl2 O9 110.5(3) . . ? O7 Cl2 O9 112.2(3) . . ? O6 Cl2 O8 108.2(4) . . ? O7 Cl2 O8 104.8(3) . . ? O9 Cl2 O8 111.5(3) . . ? O2 Cl1 O5 104.7(14) . . ? O2 Cl1 O3 113.1(6) . . ? O5 Cl1 O3 103.9(11) . . ? O2 Cl1 O4 115.8(5) . . ? O5 Cl1 O4 97.3(9) . . ? O3 Cl1 O4 118.7(5) . . ? H41W O4W H42W 108(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.011 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.100 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 780317' #TrackingRef 'Rodriguez-Dieguez.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 Cl2 Cu N16 O14' _chemical_formula_weight 899.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/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 11.752(2) _cell_length_b 11.663(2) _cell_length_c 12.921(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.396(2) _cell_angle_gamma 90.00 _cell_volume 1736.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2799 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.19 _exptl_crystal_description prismatic _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 918 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9072 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3056 _reflns_number_gt 2621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker APEXII' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0814P)^2^+0.4205P] 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 3056 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.5000 0.0000 0.02552(19) Uani 1 2 d S . . Cl1 Cl 0.75166(7) 0.59372(8) 0.24679(7) 0.0468(3) Uani 1 1 d . . . O71B O -0.04445(19) 0.13642(16) 0.36231(15) 0.0348(5) Uani 1 1 d . . . O1W O 0.1619(2) 0.4448(2) 0.0285(2) 0.0359(5) Uani 1 1 d . . . C6B C 0.0629(3) 0.3073(2) 0.4165(2) 0.0328(7) Uani 1 1 d . . . H6B H 0.0857 0.2851 0.4867 0.039 Uiso 1 1 calc R . . C51B C 0.1728(3) 0.4898(3) 0.4623(3) 0.0430(8) Uani 1 1 d . . . H51A H 0.1244 0.5321 0.5006 0.064 Uiso 1 1 calc R . . H51B H 0.2125 0.5422 0.4243 0.064 Uiso 1 1 calc R . . H51C H 0.2287 0.4462 0.5110 0.064 Uiso 1 1 calc R . . C7B C -0.0081(2) 0.2324(2) 0.3463(2) 0.0285(6) Uani 1 1 d . . . O2 O 0.8080(3) 0.4878(3) 0.2737(3) 0.0958(12) Uani 1 1 d . . . O3 O 0.6420(3) 0.5908(3) 0.2716(3) 0.0951(12) Uani 1 1 d . . . O4 O 0.7440(4) 0.6226(4) 0.1409(3) 0.1211(16) Uani 1 1 d . . . O5 O 0.8174(4) 0.6806(4) 0.3062(3) 0.1258(16) Uani 1 1 d . . . N8B N -0.0394(2) 0.27886(19) 0.24483(17) 0.0273(5) Uani 1 1 d . . . N3B N -0.0386(2) 0.39176(19) 0.10973(17) 0.0283(5) Uani 1 1 d . . . N1B N -0.1100(2) 0.2263(2) 0.16152(18) 0.0337(6) Uani 1 1 d . . . N4B N 0.0700(2) 0.4446(2) 0.28306(19) 0.0293(6) Uani 1 1 d . . . C3AB C 0.0018(2) 0.3783(2) 0.2125(2) 0.0256(6) Uani 1 1 d . . . C5B C 0.0996(3) 0.4105(2) 0.3865(2) 0.0320(7) Uani 1 1 d . . . C2B C -0.1070(3) 0.2970(2) 0.0839(2) 0.0331(7) Uani 1 1 d . . . H2B H -0.1484 0.2840 0.0158 0.040 Uiso 1 1 calc R . . O71A O 0.2996(2) 0.7021(3) 0.1213(2) 0.0697(8) Uani 1 1 d . . . N8A N 0.3660(2) 0.5812(2) 0.2579(2) 0.0404(6) Uani 1 1 d . . . N4A N 0.4635(3) 0.6453(3) 0.4217(2) 0.0445(7) Uani 1 1 d . . . C6A C 0.3946(3) 0.7779(3) 0.2862(3) 0.0493(8) Uani 1 1 d . . . H6A H 0.3873 0.8540 0.2644 0.059 Uiso 1 1 calc R . . C3AA C 0.4235(3) 0.5585(3) 0.3568(3) 0.0409(8) Uani 1 1 d . . . N3A N 0.4285(3) 0.4469(3) 0.3750(2) 0.0468(7) Uani 1 1 d . . . N1A N 0.3310(3) 0.4796(3) 0.2083(2) 0.0498(8) Uani 1 1 d . . . C7A C 0.3486(3) 0.6918(3) 0.2130(3) 0.0479(8) Uani 1 1 d . . . C2A C 0.3702(3) 0.4043(3) 0.2808(3) 0.0533(9) Uani 1 1 d . . . H2A H 0.3593 0.3260 0.2692 0.064 Uiso 1 1 calc R . . C5A C 0.4487(3) 0.7550(3) 0.3866(3) 0.0457(8) Uani 1 1 d . . . C51A C 0.4973(4) 0.8466(4) 0.4647(4) 0.0723(12) Uani 1 1 d . . . H51D H 0.4914 0.9197 0.4298 0.108 Uiso 1 1 calc R . . H51E H 0.5774 0.8303 0.4935 0.108 Uiso 1 1 calc R . . H51F H 0.4543 0.8483 0.5206 0.108 Uiso 1 1 calc R . . H4B H 0.084(2) 0.505(2) 0.264(2) 0.020(8) Uiso 1 1 d . . . H12W H 0.189(4) 0.440(4) -0.022(4) 0.069(15) Uiso 1 1 d . . . H11W H 0.201(4) 0.463(4) 0.068(4) 0.047(14) Uiso 1 1 d . . . H4A H 0.493(3) 0.629(4) 0.478(3) 0.051(12) Uiso 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 0.0376(3) 0.0228(3) 0.0151(3) 0.00324(17) 0.0027(2) 0.00109(18) Cl1 0.0444(5) 0.0571(6) 0.0402(5) -0.0017(4) 0.0116(4) 0.0031(4) O71B 0.0547(13) 0.0245(10) 0.0252(11) 0.0073(9) 0.0081(9) -0.0005(9) O1W 0.0392(13) 0.0410(13) 0.0242(12) -0.0019(11) -0.0014(12) 0.0023(11) C6B 0.0474(17) 0.0291(15) 0.0206(14) 0.0055(12) 0.0032(12) 0.0036(13) C51B 0.058(2) 0.0356(18) 0.0300(18) 0.0016(13) -0.0032(16) -0.0048(14) C7B 0.0380(15) 0.0287(15) 0.0193(13) 0.0044(12) 0.0072(12) 0.0075(12) O2 0.103(3) 0.090(3) 0.098(3) 0.0075(19) 0.026(2) 0.047(2) O3 0.0665(19) 0.100(2) 0.135(3) 0.008(2) 0.059(2) 0.0116(17) O4 0.108(3) 0.212(5) 0.0467(19) 0.023(3) 0.0244(18) 0.054(3) O5 0.152(4) 0.099(3) 0.108(3) -0.004(2) -0.020(3) -0.057(3) N8B 0.0376(13) 0.0229(11) 0.0205(12) 0.0024(9) 0.0032(10) -0.0001(10) N3B 0.0412(14) 0.0256(12) 0.0171(11) 0.0046(9) 0.0034(10) 0.0010(10) N1B 0.0479(15) 0.0288(13) 0.0230(12) -0.0007(10) 0.0040(11) -0.0049(11) N4B 0.0426(14) 0.0226(13) 0.0223(12) 0.0037(11) 0.0052(11) -0.0018(11) C3AB 0.0325(14) 0.0232(13) 0.0212(14) 0.0027(11) 0.0059(12) 0.0032(11) C5B 0.0409(16) 0.0320(15) 0.0223(15) 0.0029(12) 0.0040(12) 0.0078(13) C2B 0.0465(17) 0.0297(15) 0.0211(15) 0.0018(12) 0.0016(13) -0.0016(13) O71A 0.0695(18) 0.089(2) 0.0401(15) 0.0110(15) -0.0157(13) -0.0017(16) N8A 0.0353(14) 0.0527(17) 0.0295(14) -0.0040(13) -0.0025(11) -0.0039(12) N4A 0.0497(17) 0.0520(18) 0.0274(16) -0.0023(14) -0.0030(13) -0.0075(13) C6A 0.0462(19) 0.050(2) 0.049(2) 0.0048(17) 0.0027(16) -0.0009(16) C3AA 0.0344(16) 0.056(2) 0.0306(17) -0.0054(16) 0.0015(13) -0.0026(15) N3A 0.0517(17) 0.0469(17) 0.0374(16) -0.0031(13) -0.0021(13) -0.0042(13) N1A 0.0473(17) 0.0595(19) 0.0380(17) -0.0138(15) -0.0027(14) -0.0048(14) C7A 0.0379(17) 0.064(2) 0.038(2) 0.0052(17) -0.0006(15) -0.0005(16) C2A 0.053(2) 0.056(2) 0.047(2) -0.0146(18) 0.0011(18) -0.0071(18) C5A 0.0422(18) 0.052(2) 0.0410(19) -0.0038(17) 0.0032(15) -0.0082(15) C51A 0.098(3) 0.061(3) 0.054(2) -0.010(2) 0.004(2) -0.022(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 O1W 1.973(2) . ? Cu1 O1W 1.973(2) 3_565 ? Cu1 N3B 2.016(2) . ? Cu1 N3B 2.016(2) 3_565 ? Cu1 O71B 2.3670(19) 4_565 ? Cu1 O71B 2.3670(19) 2 ? Cl1 O3 1.389(3) . ? Cl1 O4 1.395(3) . ? Cl1 O5 1.407(4) . ? Cl1 O2 1.413(3) . ? O71B C7B 1.230(3) . ? O71B Cu1 2.3670(19) 2_545 ? C6B C5B 1.362(4) . ? C6B C7B 1.408(4) . ? C51B C5B 1.491(4) . ? C7B N8B 1.399(3) . ? N8B C3AB 1.354(3) . ? N8B N1B 1.368(3) . ? N3B C3AB 1.328(3) . ? N3B C2B 1.369(4) . ? N1B C2B 1.304(4) . ? N4B C3AB 1.336(4) . ? N4B C5B 1.372(4) . ? O71A C7A 1.217(4) . ? N8A C3AA 1.348(4) . ? N8A N1A 1.372(4) . ? N8A C7A 1.412(5) . ? N4A C3AA 1.340(4) . ? N4A C5A 1.358(5) . ? C6A C5A 1.354(5) . ? C6A C7A 1.412(5) . ? C3AA N3A 1.322(5) . ? N3A C2A 1.367(4) . ? N1A C2A 1.301(5) . ? C5A C51A 1.502(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Cu1 O1W 180.0 . 3_565 ? O1W Cu1 N3B 90.39(10) . . ? O1W Cu1 N3B 89.61(10) 3_565 . ? O1W Cu1 N3B 89.61(10) . 3_565 ? O1W Cu1 N3B 90.39(10) 3_565 3_565 ? N3B Cu1 N3B 180.00(10) . 3_565 ? O1W Cu1 O71B 89.00(10) . 4_565 ? O1W Cu1 O71B 91.00(10) 3_565 4_565 ? N3B Cu1 O71B 93.49(8) . 4_565 ? N3B Cu1 O71B 86.51(8) 3_565 4_565 ? O1W Cu1 O71B 91.00(10) . 2 ? O1W Cu1 O71B 89.00(10) 3_565 2 ? N3B Cu1 O71B 86.51(8) . 2 ? N3B Cu1 O71B 93.49(8) 3_565 2 ? O71B Cu1 O71B 180.00(11) 4_565 2 ? O3 Cl1 O4 110.5(2) . . ? O3 Cl1 O5 109.0(3) . . ? O4 Cl1 O5 106.5(3) . . ? O3 Cl1 O2 109.5(2) . . ? O4 Cl1 O2 112.8(3) . . ? O5 Cl1 O2 108.4(3) . . ? C7B O71B Cu1 134.88(19) . 2_545 ? C5B C6B C7B 123.1(3) . . ? O71B C7B N8B 118.3(2) . . ? O71B C7B C6B 129.6(3) . . ? N8B C7B C6B 112.1(2) . . ? C3AB N8B N1B 109.9(2) . . ? C3AB N8B C7B 125.3(2) . . ? N1B N8B C7B 124.7(2) . . ? C3AB N3B C2B 103.0(2) . . ? C3AB N3B Cu1 133.79(19) . . ? C2B N3B Cu1 122.50(18) . . ? C2B N1B N8B 102.5(2) . . ? C3AB N4B C5B 120.0(2) . . ? N3B C3AB N4B 131.4(2) . . ? N3B C3AB N8B 109.4(2) . . ? N4B C3AB N8B 119.2(2) . . ? C6B C5B N4B 120.0(3) . . ? C6B C5B C51B 122.4(3) . . ? N4B C5B C51B 117.6(3) . . ? N1B C2B N3B 115.3(2) . . ? C3AA N8A N1A 108.7(3) . . ? C3AA N8A C7A 125.0(3) . . ? N1A N8A C7A 126.2(3) . . ? C3AA N4A C5A 119.8(3) . . ? C5A C6A C7A 123.2(3) . . ? N3A C3AA N4A 129.4(3) . . ? N3A C3AA N8A 111.0(3) . . ? N4A C3AA N8A 119.6(3) . . ? C3AA N3A C2A 101.7(3) . . ? C2A N1A N8A 102.5(3) . . ? O71A C7A N8A 119.5(3) . . ? O71A C7A C6A 128.8(4) . . ? N8A C7A C6A 111.7(3) . . ? N1A C2A N3A 116.1(3) . . ? C6A C5A N4A 120.7(3) . . ? C6A C5A C51A 123.2(3) . . ? N4A C5A C51A 116.0(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.840 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.074 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 780318' #TrackingRef 'Rodriguez-Dieguez.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H15 Cl2 Co N4 O14' _chemical_formula_weight 497.05 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pmn21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 12.923(5) _cell_length_b 6.542(5) _cell_length_c 10.446(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 883.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3102 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 23.40 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 1.354 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.572 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9737 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.20 _reflns_number_total 2149 _reflns_number_gt 1948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker APEXII' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0926P)^2^+0.8821P] 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 0.98(3) _refine_ls_number_reflns 2149 _refine_ls_number_parameters 163 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1504 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.65650(11) 0.31211(6) 0.0280(2) Uani 1 2 d S . . O1W O 0.1577(3) 0.6617(5) 0.3105(7) 0.0527(10) Uani 1 1 d D . . O2W O 0.0000 0.5886(11) 0.1172(6) 0.0434(14) Uani 1 2 d S . . 071A O 0.0000 0.7189(8) 0.5145(5) 0.0387(11) Uani 1 2 d S . . N1A N 0.0000 0.9917(7) 0.3219(7) 0.0304(10) Uani 1 2 d S . . N8A N 0.0000 1.0420(8) 0.4488(5) 0.0270(10) Uani 1 2 d S . . C2A C 0.0000 1.1745(9) 0.2662(7) 0.0307(13) Uani 1 2 d S . . H2A H 0.0000 1.1908 0.1778 0.037 Uiso 1 2 calc SR . . C7A C 0.0000 0.9037(9) 0.5475(6) 0.0299(13) Uani 1 2 d S . . C6A C 0.0000 0.9905(9) 0.6682(6) 0.0331(14) Uani 1 2 d S . . H6A H 0.0000 0.9060 0.7398 0.040 Uiso 1 2 calc SR . . C5A C 0.0000 1.1992(10) 0.6846(7) 0.0364(15) Uani 1 2 d S . . C51A C 0.0000 1.3039(10) 0.8113(10) 0.0490(18) Uani 1 2 d S . . H51A H -0.0450 1.4205 0.8080 0.073 Uiso 0.50 1 calc PR . . H51B H 0.0690 1.3478 0.8316 0.073 Uiso 0.50 1 calc PR . . H51C H -0.0239 1.2110 0.8760 0.073 Uiso 0.50 1 calc PR . . Cl1B Cl 0.29272(10) 1.1081(3) 0.46473(16) 0.0483(4) Uani 1 1 d . . . O2B O 0.3632(13) 0.987(2) 0.5179(11) 0.203(7) Uani 1 1 d . . . O5B O 0.2562(7) 1.0435(11) 0.3450(6) 0.103(2) Uani 1 1 d . . . O4B O 0.3493(12) 1.285(2) 0.4489(11) 0.204(8) Uani 1 1 d . . . O3W O 0.2731(7) 1.3993(11) 0.1697(7) 0.094(2) Uani 1 1 d . . . O3B O 0.2191(8) 1.127(3) 0.5504(13) 0.208(10) Uani 1 1 d . . . N3A N 0.0000 1.3351(8) 0.3481(5) 0.0316(13) Uani 1 2 d S . . N4A N 0.0000 1.3225(7) 0.5808(6) 0.0307(12) Uani 1 2 d S . . C3AA C 0.0000 1.2462(9) 0.4625(6) 0.0256(11) Uani 1 2 d S . . H11W H 0.200(5) 0.765(9) 0.293(10) 0.08(2) Uiso 1 1 d D . . H31W H 0.227(8) 1.449(12) 0.099(11) 0.09(3) Uiso 1 1 d D . . H32W H 0.240(5) 1.278(11) 0.138(7) 0.046(17) Uiso 1 1 d D . . H12W H 0.198(5) 0.582(11) 0.263(7) 0.07(3) Uiso 1 1 d D . . H22W H 0.034(7) 0.635(13) 0.085(9) 0.08(4) Uiso 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 Co1 0.0412(4) 0.0122(3) 0.0305(4) 0.0010(4) 0.000 0.000 O1W 0.0430(18) 0.0304(16) 0.085(3) -0.009(2) 0.006(3) -0.0028(14) O2W 0.056(4) 0.039(4) 0.036(3) 0.009(3) 0.000 0.000 071A 0.071(3) 0.009(2) 0.036(3) 0.0009(19) 0.000 0.000 N1A 0.047(3) 0.016(2) 0.029(2) 0.001(3) 0.000 0.000 N8A 0.040(3) 0.014(2) 0.027(2) 0.001(2) 0.000 0.000 C2A 0.050(4) 0.016(3) 0.027(3) -0.002(2) 0.000 0.000 C7A 0.043(3) 0.015(3) 0.032(3) 0.004(2) 0.000 0.000 C6A 0.049(4) 0.020(3) 0.030(3) 0.008(3) 0.000 0.000 C5A 0.053(4) 0.023(3) 0.033(3) 0.001(3) 0.000 0.000 C51A 0.089(5) 0.028(3) 0.029(3) 0.008(4) 0.000 0.000 Cl1B 0.0457(7) 0.0513(8) 0.0480(7) -0.0063(6) -0.0013(6) -0.0049(6) O2B 0.240(13) 0.224(13) 0.144(9) -0.056(9) -0.080(9) 0.159(12) O5B 0.159(6) 0.080(4) 0.070(4) -0.006(3) -0.031(4) -0.058(4) O4B 0.284(15) 0.207(12) 0.120(7) 0.070(8) -0.107(9) -0.186(12) O3W 0.143(7) 0.070(4) 0.069(4) -0.003(3) 0.013(4) 0.021(4) O3B 0.079(6) 0.42(3) 0.131(8) -0.080(12) 0.037(6) -0.018(8) N3A 0.053(3) 0.016(2) 0.026(3) 0.0042(18) 0.000 0.000 N4A 0.052(3) 0.010(2) 0.030(3) 0.0012(19) 0.000 0.000 C3AA 0.035(3) 0.013(3) 0.028(3) 0.000(3) 0.000 0.000 _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 Co1 O1W 2.038(4) . ? Co1 O1W 2.038(4) 3 ? Co1 O2W 2.084(7) . ? Co1 N3A 2.136(6) 1_545 ? Co1 071A 2.154(5) . ? Co1 N1A 2.195(5) . ? O1W H11W 0.89(2) . ? O1W H12W 0.89(2) . ? O2W H22W 0.63(9) . ? 071A C7A 1.257(8) . ? N1A C2A 1.330(8) . ? N1A N8A 1.366(9) . ? N8A C3AA 1.343(8) . ? N8A C7A 1.372(8) . ? C2A N3A 1.355(8) . ? C2A H2A 0.9300 . ? C7A C6A 1.382(10) . ? C6A C5A 1.376(9) . ? C6A H6A 0.9300 . ? C5A N4A 1.352(9) . ? C5A C51A 1.490(12) . ? C51A H51A 0.9600 . ? C51A H51B 0.9600 . ? C51A H51C 0.9600 . ? Cl1B O3B 1.312(10) . ? Cl1B O2B 1.330(9) . ? Cl1B O4B 1.377(9) . ? Cl1B O5B 1.402(6) . ? O3W H31W 1.00(11) . ? O3W H32W 0.96(7) . ? N3A C3AA 1.329(8) . ? N3A Co1 2.136(6) 1_565 ? N4A C3AA 1.333(8) . ? 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 O1W Co1 O1W 177.9(3) . 3 ? O1W Co1 O2W 89.8(2) . . ? O1W Co1 O2W 89.8(2) 3 . ? O1W Co1 N3A 91.02(10) . 1_545 ? O1W Co1 N3A 91.02(10) 3 1_545 ? O2W Co1 N3A 87.8(3) . 1_545 ? O1W Co1 071A 90.3(2) . . ? O1W Co1 071A 90.3(2) 3 . ? O2W Co1 071A 178.6(3) . . ? N3A Co1 071A 90.79(19) 1_545 . ? O1W Co1 N1A 89.06(10) . . ? O1W Co1 N1A 89.06(10) 3 . ? O2W Co1 N1A 105.0(3) . . ? N3A Co1 N1A 167.2(2) 1_545 . ? 071A Co1 N1A 76.4(2) . . ? Co1 O1W H11W 129(5) . . ? Co1 O1W H12W 126(5) . . ? H11W O1W H12W 88(8) . . ? Co1 O2W H22W 115(9) . . ? C7A 071A Co1 116.8(4) . . ? C2A N1A N8A 102.0(5) . . ? C2A N1A Co1 151.4(5) . . ? N8A N1A Co1 106.6(4) . . ? C3AA N8A N1A 110.1(5) . . ? C3AA N8A C7A 125.1(6) . . ? N1A N8A C7A 124.8(5) . . ? N1A C2A N3A 114.9(6) . . ? N1A C2A H2A 122.5 . . ? N3A C2A H2A 122.5 . . ? 071A C7A N8A 115.4(6) . . ? 071A C7A C6A 130.1(6) . . ? N8A C7A C6A 114.5(6) . . ? C5A C6A C7A 121.4(6) . . ? C5A C6A H6A 119.3 . . ? C7A C6A H6A 119.3 . . ? N4A C5A C6A 119.5(6) . . ? N4A C5A C51A 116.0(6) . . ? C6A C5A C51A 124.6(6) . . ? C5A C51A H51A 109.5 . . ? C5A C51A H51B 109.5 . . ? H51A C51A H51B 109.5 . . ? C5A C51A H51C 109.5 . . ? H51A C51A H51C 109.5 . . ? H51B C51A H51C 109.5 . . ? O3B Cl1B O2B 105.6(11) . . ? O3B Cl1B O4B 112.8(10) . . ? O2B Cl1B O4B 100.8(11) . . ? O3B Cl1B O5B 113.1(7) . . ? O2B Cl1B O5B 115.1(6) . . ? O4B Cl1B O5B 108.9(5) . . ? H31W O3W H32W 76(5) . . ? C3AA N3A C2A 103.2(5) . . ? C3AA N3A Co1 126.1(4) . 1_565 ? C2A N3A Co1 130.7(5) . 1_565 ? C3AA N4A C5A 121.3(5) . . ? N3A C3AA N4A 132.0(5) . . ? N3A C3AA N8A 109.8(5) . . ? N4A C3AA N8A 118.1(5) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.724 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.091