# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ma Antonia Mendiola' _publ_contact_author_email ANTONIA.MENDIOLA@UAM.ES _publ_section_title ; Structural diversity of benzil bis(benzoylhydrazone): Mononuclear, binuclear and trinuclear complexes ; loop_ _publ_author_name 'Ma Antonia Mendiola' 'Elena Lopez-Torres' # Attachment 'LH2a.cif' data_bbhz _database_code_depnum_ccdc_archive 'CCDC 710840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 N4 O2' _chemical_formula_sum 'C28 H22 N4 O2' _chemical_formula_weight 446.50 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.4854(6) _cell_length_b 11.4782(4) _cell_length_c 9.7608(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.877(2) _cell_angle_gamma 90.00 _cell_volume 2171.60(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6128 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 32.60 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9785 _exptl_absorpt_correction_T_max 0.9920 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24984 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 29.57 _reflns_number_total 3002 _reflns_number_gt 2181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0503P)^2^+2.0478P] 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 3002 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 O1 O 0.11926(5) 0.53912(8) -0.01126(9) 0.0184(2) Uani 1 1 d . . . C1 C 0.11530(6) 0.54588(11) 0.11268(13) 0.0145(2) Uani 1 1 d . . . N1 N 0.07556(6) 0.47159(10) 0.18219(11) 0.0157(2) Uani 1 1 d . . . H1 H 0.0800(9) 0.4706(16) 0.272(2) 0.029(5) Uiso 1 1 d . . . N2 N 0.03778(5) 0.38768(9) 0.10747(11) 0.0147(2) Uani 1 1 d . . . C11 C 0.15367(7) 0.63704(11) 0.19884(13) 0.0149(3) Uani 1 1 d . . . C16 C 0.13270(7) 0.67721(11) 0.32272(13) 0.0172(3) Uani 1 1 d . . . H16 H 0.0948 0.6438 0.3581 0.021 Uiso 1 1 calc R . . C15 C 0.16846(7) 0.76690(12) 0.39314(14) 0.0207(3) Uani 1 1 d . . . H15 H 0.1542 0.7939 0.4754 0.025 Uiso 1 1 calc R . . C14 C 0.22537(8) 0.81666(12) 0.34185(15) 0.0225(3) Uani 1 1 d . . . H14 H 0.2492 0.8767 0.3898 0.027 Uiso 1 1 calc R . . C13 C 0.24675(7) 0.77686(12) 0.21923(15) 0.0227(3) Uani 1 1 d . . . H13 H 0.2852 0.8097 0.1850 0.027 Uiso 1 1 calc R . . C12 C 0.21081(7) 0.68790(12) 0.14747(14) 0.0199(3) Uani 1 1 d . . . H12 H 0.2249 0.6620 0.0645 0.024 Uiso 1 1 calc R . . C2 C 0.00161(6) 0.31686(11) 0.17318(12) 0.0138(2) Uani 1 1 d . . . C21 C -0.03733(6) 0.22320(11) 0.09548(13) 0.0145(3) Uani 1 1 d . . . C22 C -0.02442(7) 0.19267(12) -0.03819(13) 0.0181(3) Uani 1 1 d . . . H22 H 0.0096 0.2317 -0.0804 0.022 Uiso 1 1 calc R . . C23 C -0.06198(7) 0.10462(12) -0.10822(14) 0.0201(3) Uani 1 1 d . . . H23 H -0.0530 0.0849 -0.1971 0.024 Uiso 1 1 calc R . . C24 C -0.11286(7) 0.04576(12) -0.04628(14) 0.0198(3) Uani 1 1 d . . . H24 H -0.1382 -0.0128 -0.0938 0.024 Uiso 1 1 calc R . . C25 C -0.12567(7) 0.07449(12) 0.08609(14) 0.0208(3) Uani 1 1 d . . . H25 H -0.1596 0.0348 0.1279 0.025 Uiso 1 1 calc R . . C26 C -0.08813(7) 0.16240(12) 0.15692(14) 0.0182(3) Uani 1 1 d . . . H26 H -0.0969 0.1810 0.2462 0.022 Uiso 1 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 O1 0.0241(5) 0.0190(5) 0.0128(4) -0.0005(3) 0.0054(3) -0.0016(4) C1 0.0150(6) 0.0140(6) 0.0148(6) 0.0004(4) 0.0032(4) 0.0020(5) N1 0.0199(6) 0.0163(5) 0.0110(5) -0.0004(4) 0.0023(4) -0.0029(4) N2 0.0157(5) 0.0139(5) 0.0145(5) -0.0009(4) 0.0022(4) 0.0001(4) C11 0.0169(6) 0.0144(6) 0.0135(6) 0.0013(4) 0.0021(4) 0.0006(5) C16 0.0211(6) 0.0152(6) 0.0158(6) 0.0015(5) 0.0044(5) 0.0021(5) C15 0.0288(7) 0.0179(6) 0.0152(6) -0.0016(5) 0.0009(5) 0.0040(6) C14 0.0250(7) 0.0166(6) 0.0242(7) -0.0010(5) -0.0054(5) -0.0003(6) C13 0.0190(7) 0.0216(7) 0.0275(7) 0.0012(6) 0.0025(5) -0.0038(6) C12 0.0209(7) 0.0207(7) 0.0186(6) 0.0006(5) 0.0052(5) -0.0018(5) C2 0.0152(6) 0.0133(6) 0.0132(6) -0.0006(4) 0.0023(4) 0.0023(5) C21 0.0152(6) 0.0138(6) 0.0144(6) 0.0012(4) 0.0011(4) 0.0011(5) C22 0.0199(6) 0.0191(7) 0.0158(6) -0.0006(5) 0.0045(5) -0.0013(5) C23 0.0247(7) 0.0201(7) 0.0156(6) -0.0032(5) 0.0021(5) 0.0009(6) C24 0.0219(7) 0.0159(6) 0.0207(6) -0.0012(5) -0.0017(5) -0.0015(5) C25 0.0210(7) 0.0198(7) 0.0219(7) 0.0023(5) 0.0032(5) -0.0051(5) C26 0.0205(6) 0.0193(6) 0.0154(6) -0.0007(5) 0.0041(5) -0.0017(5) _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 O1 C1 1.2225(15) . ? C1 N1 1.3764(16) . ? C1 C11 1.4942(18) . ? N1 N2 1.3753(15) . ? N1 H1 0.871(19) . ? N2 C2 1.2891(16) . ? C11 C16 1.3938(17) . ? C11 C12 1.3951(18) . ? C16 C15 1.3854(19) . ? C16 H16 0.9300 . ? C15 C14 1.386(2) . ? C15 H15 0.9300 . ? C14 C13 1.385(2) . ? C14 H14 0.9300 . ? C13 C12 1.3869(19) . ? C13 H13 0.9300 . ? C12 H12 0.9300 . ? C2 C21 1.4794(17) . ? C2 C2 1.507(2) 2 ? C21 C26 1.3958(18) . ? C21 C22 1.3984(17) . ? C22 C23 1.3862(19) . ? C22 H22 0.9300 . ? C23 C24 1.3885(19) . ? C23 H23 0.9300 . ? C24 C25 1.3807(19) . ? C24 H24 0.9300 . ? C25 C26 1.3885(19) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? 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 C1 N1 122.97(12) . . ? O1 C1 C11 121.51(12) . . ? N1 C1 C11 115.51(11) . . ? N2 N1 C1 118.03(11) . . ? N2 N1 H1 121.1(12) . . ? C1 N1 H1 120.0(12) . . ? C2 N2 N1 117.91(11) . . ? C16 C11 C12 119.27(12) . . ? C16 C11 C1 123.07(12) . . ? C12 C11 C1 117.55(11) . . ? C15 C16 C11 119.94(12) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C16 C15 C14 120.49(13) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C13 C14 C15 119.94(13) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C13 C12 119.89(13) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C12 C11 120.46(13) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? N2 C2 C21 118.75(11) . . ? N2 C2 C2 125.14(11) . 2 ? C21 C2 C2 116.02(9) . 2 ? C26 C21 C22 118.60(12) . . ? C26 C21 C2 119.47(11) . . ? C22 C21 C2 121.92(11) . . ? C23 C22 C21 120.43(12) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.30(13) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 119.79(13) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.20(13) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.67(13) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 N1 N2 -1.28(18) . . . . ? C11 C1 N1 N2 178.47(11) . . . . ? C1 N1 N2 C2 178.75(11) . . . . ? O1 C1 C11 C16 155.10(13) . . . . ? N1 C1 C11 C16 -24.65(18) . . . . ? O1 C1 C11 C12 -21.23(19) . . . . ? N1 C1 C11 C12 159.02(12) . . . . ? C12 C11 C16 C15 0.1(2) . . . . ? C1 C11 C16 C15 -176.12(12) . . . . ? C11 C16 C15 C14 -0.5(2) . . . . ? C16 C15 C14 C13 0.1(2) . . . . ? C15 C14 C13 C12 0.5(2) . . . . ? C14 C13 C12 C11 -0.8(2) . . . . ? C16 C11 C12 C13 0.5(2) . . . . ? C1 C11 C12 C13 176.96(12) . . . . ? N1 N2 C2 C21 -177.73(11) . . . . ? N1 N2 C2 C2 -1.33(19) . . . 2 ? N2 C2 C21 C26 -165.95(12) . . . . ? C2 C2 C21 C26 17.31(18) 2 . . . ? N2 C2 C21 C22 14.58(19) . . . . ? C2 C2 C21 C22 -162.16(13) 2 . . . ? C26 C21 C22 C23 0.7(2) . . . . ? C2 C21 C22 C23 -179.86(12) . . . . ? C21 C22 C23 C24 0.0(2) . . . . ? C22 C23 C24 C25 -0.5(2) . . . . ? C23 C24 C25 C26 0.4(2) . . . . ? C24 C25 C26 C21 0.3(2) . . . . ? C22 C21 C26 C25 -0.8(2) . . . . ? C2 C21 C26 C25 179.69(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.871(19) 2.178(19) 3.0285(14) 165.1(16) 6_566 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.398 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.052 # Attachment 'LH2b.cif' data_datos_0ma _database_code_depnum_ccdc_archive 'CCDC 710841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 N4 O2' _chemical_formula_sum 'C28 H22 N4 O2' _chemical_formula_weight 446.50 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4953(13) _cell_length_b 7.5979(14) _cell_length_c 12.975(3) _cell_angle_alpha 92.021(7) _cell_angle_beta 96.286(8) _cell_angle_gamma 90.381(7) _cell_volume 538.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3715 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 30.89 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 234 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9780 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7558 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2336 _reflns_number_gt 2023 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0204P)^2^+1.1627P] 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 2336 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1550 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _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 C1 C 0.9634(4) 0.8791(3) 0.63838(19) 0.0154(5) Uani 1 1 d . . . C11 C 0.9593(4) 0.8218(3) 0.74678(18) 0.0144(5) Uani 1 1 d . . . C12 C 1.1622(5) 0.8761(3) 0.8143(2) 0.0193(5) Uani 1 1 d . . . C13 C 1.1762(5) 0.8402(4) 0.9171(2) 0.0231(6) Uani 1 1 d . . . C14 C 0.9899(5) 0.7506(4) 0.9557(2) 0.0244(6) Uani 1 1 d . . . C15 C 0.7883(5) 0.6983(4) 0.8898(2) 0.0238(6) Uani 1 1 d . . . C16 C 0.7705(5) 0.7338(3) 0.7859(2) 0.0194(5) Uani 1 1 d . . . C2 C 0.5722(4) 0.5778(3) 0.48972(19) 0.0152(5) Uani 1 1 d . . . C21 C 0.5722(4) 0.6306(3) 0.38133(18) 0.0129(5) Uani 1 1 d . . . C26 C 0.3836(5) 0.7301(3) 0.3347(2) 0.0176(5) Uani 1 1 d . . . C25 C 0.3802(5) 0.7693(3) 0.2321(2) 0.0204(6) Uani 1 1 d . . . C24 C 0.5618(5) 0.7092(3) 0.1755(2) 0.0204(5) Uani 1 1 d . . . C23 C 0.7497(5) 0.6110(3) 0.2216(2) 0.0204(5) Uani 1 1 d . . . C22 C 0.7554(5) 0.5730(3) 0.3248(2) 0.0165(5) Uani 1 1 d . . . N1 N 0.8281(4) 0.7965(3) 0.55684(17) 0.0165(5) Uani 1 1 d . . . N2 N 0.6928(4) 0.6507(3) 0.56987(16) 0.0157(4) Uani 1 1 d . . . O1 O 1.0924(3) 1.0035(2) 0.62132(14) 0.0220(4) Uani 1 1 d . . . H1 H 0.841(5) 0.840(4) 0.499(3) 0.020(8) Uiso 1 1 d . . . H12 H 1.287(5) 0.934(4) 0.785(2) 0.017(7) Uiso 1 1 d . . . H13 H 1.323(6) 0.875(5) 0.960(3) 0.032(9) Uiso 1 1 d . . . H14 H 1.001(6) 0.722(5) 1.028(3) 0.034(9) Uiso 1 1 d . . . H15 H 0.644(6) 0.645(5) 0.919(3) 0.033(9) Uiso 1 1 d . . . H16 H 0.633(6) 0.691(4) 0.738(2) 0.022(8) Uiso 1 1 d . . . H26 H 0.255(6) 0.768(4) 0.373(2) 0.021(8) Uiso 1 1 d . . . H25 H 0.250(6) 0.835(4) 0.196(2) 0.020(8) Uiso 1 1 d . . . H24 H 0.554(6) 0.733(5) 0.103(3) 0.032(9) Uiso 1 1 d . . . H23 H 0.879(6) 0.570(4) 0.184(3) 0.030(9) Uiso 1 1 d . . . H22 H 0.885(6) 0.507(4) 0.359(3) 0.031(9) 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 C1 0.0169(12) 0.0125(11) 0.0166(12) 0.0002(9) 0.0008(9) -0.0021(9) C11 0.0176(12) 0.0108(11) 0.0144(12) -0.0014(9) 0.0001(9) 0.0001(9) C12 0.0181(12) 0.0186(12) 0.0204(13) 0.0021(10) -0.0016(10) -0.0036(10) C13 0.0238(14) 0.0254(14) 0.0188(13) 0.0001(10) -0.0039(10) -0.0034(11) C14 0.0310(15) 0.0265(14) 0.0156(13) 0.0001(10) 0.0015(11) -0.0034(11) C15 0.0275(14) 0.0264(14) 0.0180(13) -0.0024(11) 0.0060(11) -0.0064(11) C16 0.0181(12) 0.0212(13) 0.0184(12) -0.0042(10) 0.0012(10) -0.0058(10) C2 0.0169(12) 0.0120(11) 0.0170(12) 0.0009(9) 0.0030(9) -0.0005(9) C21 0.0139(11) 0.0108(11) 0.0135(11) -0.0007(8) 0.0006(8) -0.0050(8) C26 0.0173(12) 0.0153(12) 0.0202(13) 0.0014(9) 0.0017(10) -0.0006(9) C25 0.0208(13) 0.0172(12) 0.0218(13) 0.0043(10) -0.0049(10) -0.0014(10) C24 0.0270(14) 0.0190(13) 0.0146(12) 0.0016(10) 0.0004(10) -0.0063(10) C23 0.0233(13) 0.0200(13) 0.0189(13) -0.0013(10) 0.0078(10) -0.0032(10) C22 0.0153(12) 0.0154(12) 0.0180(12) 0.0016(9) -0.0011(9) -0.0003(9) N1 0.0217(11) 0.0148(10) 0.0126(10) 0.0032(8) -0.0012(8) -0.0076(8) N2 0.0169(10) 0.0128(10) 0.0173(10) 0.0005(8) 0.0013(8) -0.0045(8) O1 0.0262(10) 0.0190(9) 0.0195(9) 0.0030(7) -0.0039(7) -0.0119(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.218(3) . ? C1 N1 1.357(3) . ? C1 C11 1.489(3) . ? C11 C16 1.383(3) . ? C11 C12 1.391(3) . ? C12 C13 1.365(4) . ? C12 H12 0.94(3) . ? C13 C14 1.374(4) . ? C13 H13 0.96(4) . ? C14 C15 1.371(4) . ? C14 H14 0.96(4) . ? C15 C16 1.377(4) . ? C15 H15 1.00(3) . ? C16 H16 0.97(3) . ? C2 N2 1.277(3) . ? C2 C2 1.469(5) 2_666 ? C2 C21 1.476(3) . ? C21 C22 1.374(3) . ? C21 C26 1.385(3) . ? C26 C25 1.372(4) . ? C26 H26 0.95(3) . ? C25 C24 1.374(4) . ? C25 H25 0.96(3) . ? C24 C23 1.374(4) . ? C24 H24 0.96(3) . ? C23 C22 1.376(4) . ? C23 H23 0.95(3) . ? C22 H22 0.95(3) . ? N1 N2 1.356(3) . ? N1 H1 0.84(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 C1 N1 118.3(2) . . ? O1 C1 C11 119.6(2) . . ? N1 C1 C11 122.1(2) . . ? C16 C11 C12 118.9(2) . . ? C16 C11 C1 126.6(2) . . ? C12 C11 C1 114.3(2) . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12 123.3(18) . . ? C11 C12 H12 116.2(18) . . ? C12 C13 C14 120.6(3) . . ? C12 C13 H13 118(2) . . ? C14 C13 H13 122(2) . . ? C15 C14 C13 119.2(3) . . ? C15 C14 H14 120(2) . . ? C13 C14 H14 121(2) . . ? C14 C15 C16 121.0(3) . . ? C14 C15 H15 119.5(19) . . ? C16 C15 H15 119(2) . . ? C15 C16 C11 119.8(2) . . ? C15 C16 H16 121.2(19) . . ? C11 C16 H16 118.9(18) . . ? N2 C2 C2 114.8(3) . 2_666 ? N2 C2 C21 126.8(2) . . ? C2 C2 C21 118.4(3) 2_666 . ? C22 C21 C26 119.8(2) . . ? C22 C21 C2 119.5(2) . . ? C26 C21 C2 120.7(2) . . ? C25 C26 C21 119.7(2) . . ? C25 C26 H26 120.2(19) . . ? C21 C26 H26 120.1(19) . . ? C26 C25 C24 120.3(2) . . ? C26 C25 H25 122.2(18) . . ? C24 C25 H25 117.4(18) . . ? C25 C24 C23 120.1(2) . . ? C25 C24 H24 120(2) . . ? C23 C24 H24 120(2) . . ? C24 C23 C22 119.8(2) . . ? C24 C23 H23 121(2) . . ? C22 C23 H23 119(2) . . ? C21 C22 C23 120.3(2) . . ? C21 C22 H22 118(2) . . ? C23 C22 H22 122(2) . . ? N2 N1 C1 121.1(2) . . ? N2 N1 H1 124(2) . . ? C1 N1 H1 115(2) . . ? C2 N2 N1 118.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C11 C16 154.5(3) . . . . ? N1 C1 C11 C16 -25.9(4) . . . . ? O1 C1 C11 C12 -20.7(3) . . . . ? N1 C1 C11 C12 158.9(2) . . . . ? C16 C11 C12 C13 1.1(4) . . . . ? C1 C11 C12 C13 176.7(2) . . . . ? C11 C12 C13 C14 -0.2(4) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C11 0.7(4) . . . . ? C12 C11 C16 C15 -1.3(4) . . . . ? C1 C11 C16 C15 -176.3(3) . . . . ? N2 C2 C21 C22 83.2(3) . . . . ? C2 C2 C21 C22 -94.4(3) 2_666 . . . ? N2 C2 C21 C26 -100.0(3) . . . . ? C2 C2 C21 C26 82.4(3) 2_666 . . . ? C22 C21 C26 C25 0.5(4) . . . . ? C2 C21 C26 C25 -176.3(2) . . . . ? C21 C26 C25 C24 0.4(4) . . . . ? C26 C25 C24 C23 -0.7(4) . . . . ? C25 C24 C23 C22 0.1(4) . . . . ? C26 C21 C22 C23 -1.2(4) . . . . ? C2 C21 C22 C23 175.7(2) . . . . ? C24 C23 C22 C21 0.9(4) . . . . ? O1 C1 N1 N2 175.8(2) . . . . ? C11 C1 N1 N2 -3.8(4) . . . . ? C2 C2 N2 N1 -179.2(2) 2_666 . . . ? C21 C2 N2 N1 3.1(4) . . . . ? C1 N1 N2 C2 -179.1(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.84(3) 2.06(3) 2.882(3) 166(3) 2_776 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.297 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.066 # Attachment 'Complex_1.cif' data_el9 _database_code_depnum_ccdc_archive 'CCDC 710842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 N4 Ni O2' _chemical_formula_sum 'C28 H20 N4 Ni O2' _chemical_formula_weight 503.19 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 Orthorhombic _symmetry_space_group_name_H-M 'Pbcn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 26.762(2) _cell_length_b 12.3139(9) _cell_length_c 6.7859(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2236.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4888 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 22.83 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8058 _exptl_absorpt_correction_T_max 0.9562 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33938 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.02 _reflns_number_total 2215 _reflns_number_gt 1629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0616P)^2^+0.1460P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2215 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.193 _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 Ni1 Ni 0.5000 -0.04266(4) 0.2500 0.02134(18) Uani 1 2 d S . . N2 N 0.45562(8) 0.06583(18) 0.2155(3) 0.0225(5) Uani 1 1 d . . . N1 N 0.40729(8) 0.03629(17) 0.1703(3) 0.0223(5) Uani 1 1 d . . . O1 O 0.44457(7) -0.13302(15) 0.2121(3) 0.0255(5) Uani 1 1 d . . . C2 C 0.47332(10) 0.1650(2) 0.2203(3) 0.0210(6) Uani 1 1 d . . . C21 C 0.44513(10) 0.2618(2) 0.1573(4) 0.0215(6) Uani 1 1 d . . . C22 C 0.39505(10) 0.2761(2) 0.2100(4) 0.0248(6) Uani 1 1 d . . . H22 H 0.3790 0.2244 0.2873 0.030 Uiso 1 1 calc R . . C23 C 0.36950(10) 0.3671(2) 0.1472(4) 0.0246(6) Uani 1 1 d . . . H23 H 0.3364 0.3773 0.1850 0.030 Uiso 1 1 calc R . . C24 C 0.39263(10) 0.4433(2) 0.0282(4) 0.0264(6) Uani 1 1 d . . . H24 H 0.3752 0.5046 -0.0131 0.032 Uiso 1 1 calc R . . C25 C 0.44188(10) 0.4278(2) -0.0291(4) 0.0268(6) Uani 1 1 d . . . H25 H 0.4572 0.4779 -0.1119 0.032 Uiso 1 1 calc R . . C26 C 0.46819(10) 0.3383(2) 0.0363(4) 0.0243(6) Uani 1 1 d . . . H26 H 0.5014 0.3291 -0.0006 0.029 Uiso 1 1 calc R . . C1 C 0.40611(10) -0.0716(2) 0.1772(4) 0.0231(6) Uani 1 1 d . . . C11 C 0.35739(10) -0.1246(2) 0.1414(4) 0.0229(6) Uani 1 1 d . . . C16 C 0.35251(11) -0.2354(2) 0.1781(4) 0.0276(7) Uani 1 1 d . . . H16 H 0.3794 -0.2747 0.2274 0.033 Uiso 1 1 calc R . . C15 C 0.30753(11) -0.2868(3) 0.1409(4) 0.0315(7) Uani 1 1 d . . . H15 H 0.3043 -0.3608 0.1651 0.038 Uiso 1 1 calc R . . C14 C 0.26735(12) -0.2290(2) 0.0681(4) 0.0334(7) Uani 1 1 d . . . H14 H 0.2373 -0.2640 0.0425 0.040 Uiso 1 1 calc R . . C13 C 0.27209(11) -0.1185(2) 0.0333(4) 0.0335(7) Uani 1 1 d . . . H13 H 0.2451 -0.0794 -0.0156 0.040 Uiso 1 1 calc R . . C12 C 0.31672(10) -0.0661(2) 0.0710(4) 0.0280(7) Uani 1 1 d . . . H12 H 0.3196 0.0082 0.0492 0.034 Uiso 1 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 Ni1 0.0226(3) 0.0212(3) 0.0202(3) 0.000 0.0050(2) 0.000 N2 0.0259(13) 0.0276(13) 0.0140(11) 0.0009(9) 0.0015(9) -0.0005(10) N1 0.0242(12) 0.0245(12) 0.0181(11) -0.0005(9) 0.0018(10) -0.0027(10) O1 0.0249(10) 0.0240(10) 0.0276(11) 0.0022(8) 0.0072(8) 0.0000(8) C2 0.0261(15) 0.0237(14) 0.0133(13) -0.0013(11) 0.0021(11) -0.0005(12) C21 0.0265(15) 0.0239(14) 0.0140(13) -0.0027(11) -0.0038(11) -0.0029(12) C22 0.0302(16) 0.0255(14) 0.0187(14) -0.0014(11) 0.0012(11) -0.0028(12) C23 0.0216(14) 0.0289(15) 0.0233(15) -0.0037(12) -0.0035(12) 0.0000(12) C24 0.0310(17) 0.0252(15) 0.0229(14) 0.0016(12) -0.0114(12) 0.0003(12) C25 0.0294(16) 0.0279(15) 0.0231(15) 0.0041(12) -0.0073(12) -0.0074(12) C26 0.0244(15) 0.0285(14) 0.0200(13) 0.0006(12) -0.0049(11) -0.0043(12) C1 0.0286(16) 0.0284(15) 0.0123(12) -0.0007(11) 0.0074(12) -0.0005(13) C11 0.0275(15) 0.0266(15) 0.0146(13) -0.0010(11) 0.0074(11) -0.0035(12) C16 0.0274(16) 0.0314(16) 0.0241(14) 0.0034(12) 0.0095(12) -0.0014(13) C15 0.0377(18) 0.0302(16) 0.0266(16) 0.0008(13) 0.0130(13) -0.0081(14) C14 0.0327(17) 0.0383(17) 0.0292(16) 0.0009(14) 0.0017(14) -0.0122(14) C13 0.0315(16) 0.0382(16) 0.0307(16) 0.0038(14) -0.0057(13) -0.0064(14) C12 0.0332(17) 0.0286(15) 0.0221(14) 0.0018(12) -0.0017(12) -0.0044(13) _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 Ni1 N2 1.803(2) 3_655 ? Ni1 N2 1.803(2) . ? Ni1 O1 1.8721(19) . ? Ni1 O1 1.8721(19) 3_655 ? N2 C2 1.310(3) . ? N2 N1 1.378(3) . ? N1 C1 1.329(3) . ? O1 C1 1.299(3) . ? C2 C21 1.475(4) . ? C2 C2 1.484(5) 3_655 ? C21 C26 1.393(4) . ? C21 C22 1.398(4) . ? C22 C23 1.380(4) . ? C22 H22 0.9300 . ? C23 C24 1.384(4) . ? C23 H23 0.9300 . ? C24 C25 1.387(4) . ? C24 H24 0.9300 . ? C25 C26 1.381(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C1 C11 1.478(4) . ? C11 C12 1.390(4) . ? C11 C16 1.393(4) . ? C16 C15 1.383(4) . ? C16 H16 0.9300 . ? C15 C14 1.381(4) . ? C15 H15 0.9300 . ? C14 C13 1.387(4) . ? C14 H14 0.9300 . ? C13 C12 1.382(4) . ? C13 H13 0.9300 . ? C12 H12 0.9300 . ? 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 Ni1 N2 84.37(14) 3_655 . ? N2 Ni1 O1 168.61(9) 3_655 . ? N2 Ni1 O1 84.29(9) . . ? N2 Ni1 O1 84.29(9) 3_655 3_655 ? N2 Ni1 O1 168.61(9) . 3_655 ? O1 Ni1 O1 107.07(12) . 3_655 ? C2 N2 N1 126.2(2) . . ? C2 N2 Ni1 116.69(19) . . ? N1 N2 Ni1 116.85(17) . . ? C1 N1 N2 106.2(2) . . ? C1 O1 Ni1 107.86(16) . . ? N2 C2 C21 124.2(2) . . ? N2 C2 C2 110.77(16) . 3_655 ? C21 C2 C2 124.83(15) . 3_655 ? C26 C21 C22 119.4(3) . . ? C26 C21 C2 119.4(2) . . ? C22 C21 C2 121.2(2) . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.6(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 119.7(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 120.2(3) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C21 120.2(3) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? O1 C1 N1 124.7(3) . . ? O1 C1 C11 118.1(2) . . ? N1 C1 C11 117.2(2) . . ? C12 C11 C16 119.7(3) . . ? C12 C11 C1 121.2(2) . . ? C16 C11 C1 119.1(3) . . ? C15 C16 C11 119.8(3) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N2 C2 2.93(13) 3_655 . . . ? O1 Ni1 N2 C2 -178.1(2) . . . . ? O1 Ni1 N2 C2 -2.5(6) 3_655 . . . ? N2 Ni1 N2 N1 177.6(2) 3_655 . . . ? O1 Ni1 N2 N1 -3.43(17) . . . . ? O1 Ni1 N2 N1 172.2(4) 3_655 . . . ? C2 N2 N1 C1 178.2(2) . . . . ? Ni1 N2 N1 C1 4.0(3) . . . . ? N2 Ni1 O1 C1 7.2(5) 3_655 . . . ? N2 Ni1 O1 C1 1.78(16) . . . . ? O1 Ni1 O1 C1 -177.32(19) 3_655 . . . ? N1 N2 C2 C21 -6.6(4) . . . . ? Ni1 N2 C2 C21 167.54(19) . . . . ? N1 N2 C2 C2 178.6(2) . . . 3_655 ? Ni1 N2 C2 C2 -7.3(3) . . . 3_655 ? N2 C2 C21 C26 -133.9(3) . . . . ? C2 C2 C21 C26 40.2(4) 3_655 . . . ? N2 C2 C21 C22 43.4(4) . . . . ? C2 C2 C21 C22 -142.5(3) 3_655 . . . ? C26 C21 C22 C23 -2.0(4) . . . . ? C2 C21 C22 C23 -179.3(2) . . . . ? C21 C22 C23 C24 1.5(4) . . . . ? C22 C23 C24 C25 0.3(4) . . . . ? C23 C24 C25 C26 -1.7(4) . . . . ? C24 C25 C26 C21 1.2(4) . . . . ? C22 C21 C26 C25 0.6(4) . . . . ? C2 C21 C26 C25 178.0(2) . . . . ? Ni1 O1 C1 N1 0.1(3) . . . . ? Ni1 O1 C1 C11 179.82(18) . . . . ? N2 N1 C1 O1 -2.6(3) . . . . ? N2 N1 C1 C11 177.7(2) . . . . ? O1 C1 C11 C12 -169.1(2) . . . . ? N1 C1 C11 C12 10.7(4) . . . . ? O1 C1 C11 C16 10.5(4) . . . . ? N1 C1 C11 C16 -169.8(2) . . . . ? C12 C11 C16 C15 1.1(4) . . . . ? C1 C11 C16 C15 -178.4(2) . . . . ? C11 C16 C15 C14 -0.1(4) . . . . ? C16 C15 C14 C13 -0.4(4) . . . . ? C15 C14 C13 C12 0.0(5) . . . . ? C14 C13 C12 C11 0.9(4) . . . . ? C16 C11 C12 C13 -1.5(4) . . . . ? C1 C11 C12 C13 178.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.404 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.159 # Attachment 'Complex_2.cif' data_datos_0m _database_code_depnum_ccdc_archive 'CCDC 710843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H40 N8 O4 Pb2' _chemical_formula_sum 'C56 H40 N8 O4 Pb2' _chemical_formula_weight 1303.34 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.544(6) _cell_length_b 11.924(3) _cell_length_c 20.901(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.231(11) _cell_angle_gamma 90.00 _cell_volume 4594(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9933 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.38 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 7.380 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4040 _exptl_absorpt_correction_T_max 0.7092 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66588 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 26.02 _reflns_number_total 9040 _reflns_number_gt 6465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0491P)^2^+2.2043P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9040 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 Pb1 Pb 0.681681(14) -0.07932(2) 0.186214(12) 0.02199(9) Uani 1 1 d . . . Pb2 Pb 0.540760(15) 0.16863(3) 0.189499(13) 0.02470(9) Uani 1 1 d . . . C1 C 0.8467(4) -0.0940(6) 0.1443(3) 0.0214(16) Uani 1 1 d . . . C2 C 0.8197(4) -0.0310(6) 0.3003(3) 0.0213(16) Uani 1 1 d . . . C3 C 0.7543(4) -0.0255(6) 0.3367(3) 0.0213(16) Uani 1 1 d . . . C4 C 0.5690(4) -0.0304(6) 0.3015(4) 0.0256(17) Uani 1 1 d . . . C5 C 0.7185(4) 0.1993(6) 0.2242(3) 0.0265(17) Uani 1 1 d . . . C6 C 0.5991(4) 0.2680(6) 0.3335(3) 0.0207(15) Uani 1 1 d . . . C7 C 0.5204(4) 0.2609(6) 0.3347(3) 0.0230(16) Uani 1 1 d . . . C8 C 0.3753(4) 0.1726(6) 0.2265(3) 0.0203(15) Uani 1 1 d . . . C11 C 0.9106(4) -0.1076(6) 0.1062(3) 0.0247(17) Uani 1 1 d . . . C12 C 0.8998(4) -0.1544(7) 0.0452(3) 0.0308(18) Uani 1 1 d . . . H12 H 0.8523 -0.1747 0.0273 0.037 Uiso 1 1 calc R . . C13 C 0.9590(5) -0.1719(7) 0.0101(4) 0.037(2) Uani 1 1 d . . . H13 H 0.9523 -0.2073 -0.0308 0.044 Uiso 1 1 calc R . . C14 C 1.0276(5) -0.1370(7) 0.0356(4) 0.037(2) Uani 1 1 d . . . H14 H 1.0678 -0.1474 0.0116 0.044 Uiso 1 1 calc R . . C15 C 1.0376(4) -0.0889(7) 0.0938(4) 0.038(2) Uani 1 1 d . . . H15 H 1.0848 -0.0654 0.1108 0.046 Uiso 1 1 calc R . . C16 C 0.9791(4) -0.0731(7) 0.1297(4) 0.0315(18) Uani 1 1 d . . . H16 H 0.9867 -0.0381 0.1708 0.038 Uiso 1 1 calc R . . C21 C 0.8927(4) -0.0068(6) 0.3339(3) 0.0213(16) Uani 1 1 d . . . C22 C 0.9331(4) 0.0801(6) 0.3129(4) 0.0272(17) Uani 1 1 d . . . H22 H 0.9157 0.1191 0.2747 0.033 Uiso 1 1 calc R . . C23 C 0.9989(4) 0.1120(7) 0.3466(4) 0.0327(19) Uani 1 1 d . . . H23 H 1.0252 0.1738 0.3323 0.039 Uiso 1 1 calc R . . C24 C 1.0253(4) 0.0531(7) 0.4008(4) 0.036(2) Uani 1 1 d . . . H24 H 1.0700 0.0745 0.4241 0.043 Uiso 1 1 calc R . . C25 C 0.9875(4) -0.0360(7) 0.4212(4) 0.0308(19) Uani 1 1 d . . . H25 H 1.0071 -0.0787 0.4573 0.037 Uiso 1 1 calc R . . C26 C 0.9205(4) -0.0640(6) 0.3889(3) 0.0248(17) Uani 1 1 d . . . H26 H 0.8932 -0.1233 0.4048 0.030 Uiso 1 1 calc R . . C31 C 0.7650(4) -0.0001(6) 0.4070(3) 0.0231(16) Uani 1 1 d . . . C32 C 0.7947(4) 0.1015(7) 0.4284(4) 0.035(2) Uani 1 1 d . . . H32 H 0.8044 0.1578 0.3983 0.043 Uiso 1 1 calc R . . C33 C 0.8103(4) 0.1210(8) 0.4940(4) 0.040(2) Uani 1 1 d . . . H33 H 0.8304 0.1909 0.5085 0.049 Uiso 1 1 calc R . . C34 C 0.7972(4) 0.0409(8) 0.5377(4) 0.042(2) Uani 1 1 d . . . H34 H 0.8102 0.0535 0.5823 0.051 Uiso 1 1 calc R . . C35 C 0.7650(4) -0.0583(8) 0.5168(4) 0.039(2) Uani 1 1 d . . . H35 H 0.7535 -0.1133 0.5470 0.047 Uiso 1 1 calc R . . C36 C 0.7495(4) -0.0769(7) 0.4521(3) 0.0323(19) Uani 1 1 d . . . H36 H 0.7274 -0.1458 0.4380 0.039 Uiso 1 1 calc R . . C41 C 0.5034(4) -0.0492(6) 0.3380(3) 0.0237(16) Uani 1 1 d . . . C42 C 0.5118(4) -0.0688(7) 0.4038(4) 0.035(2) Uani 1 1 d . . . H42 H 0.5589 -0.0696 0.4269 0.042 Uiso 1 1 calc R . . C43 C 0.4510(4) -0.0873(7) 0.4357(4) 0.037(2) Uani 1 1 d . . . H43 H 0.4565 -0.1001 0.4808 0.044 Uiso 1 1 calc R . . C44 C 0.3824(4) -0.0869(7) 0.4021(4) 0.035(2) Uani 1 1 d . . . H44 H 0.3409 -0.0996 0.4241 0.042 Uiso 1 1 calc R . . C45 C 0.3742(4) -0.0682(6) 0.3362(4) 0.0277(18) Uani 1 1 d . . . H45 H 0.3272 -0.0687 0.3131 0.033 Uiso 1 1 calc R . . C46 C 0.4344(4) -0.0486(6) 0.3041(4) 0.0309(19) Uani 1 1 d . . . H46 H 0.4287 -0.0348 0.2591 0.037 Uiso 1 1 calc R . . C51 C 0.7924(4) 0.2364(6) 0.2084(3) 0.0242(17) Uani 1 1 d . . . C56 C 0.8241(4) 0.1825(7) 0.1596(4) 0.0317(18) Uani 1 1 d . . . H56 H 0.7987 0.1240 0.1360 0.038 Uiso 1 1 calc R . . C55 C 0.8925(4) 0.2134(7) 0.1451(4) 0.036(2) Uani 1 1 d . . . H55 H 0.9140 0.1764 0.1116 0.043 Uiso 1 1 calc R . . C54 C 0.9282(5) 0.2962(8) 0.1787(4) 0.043(2) Uani 1 1 d . . . H54 H 0.9758 0.3156 0.1697 0.052 Uiso 1 1 calc R . . C53 C 0.8970(4) 0.3530(7) 0.2257(4) 0.039(2) Uani 1 1 d . . . H53 H 0.9219 0.4139 0.2476 0.047 Uiso 1 1 calc R . . C52 C 0.8292(4) 0.3215(7) 0.2413(4) 0.0354(19) Uani 1 1 d . . . H52 H 0.8083 0.3590 0.2749 0.042 Uiso 1 1 calc R . . C61 C 0.6463(4) 0.3153(6) 0.3900(3) 0.0222(16) Uani 1 1 d . . . C66 C 0.6963(4) 0.3996(6) 0.3819(3) 0.0263(17) Uani 1 1 d . . . H66 H 0.7008 0.4280 0.3401 0.032 Uiso 1 1 calc R . . C65 C 0.7399(4) 0.4426(7) 0.4351(4) 0.0335(19) Uani 1 1 d . . . H65 H 0.7751 0.4983 0.4287 0.040 Uiso 1 1 calc R . . C64 C 0.7329(4) 0.4057(7) 0.4960(4) 0.035(2) Uani 1 1 d . . . H64 H 0.7623 0.4366 0.5317 0.042 Uiso 1 1 calc R . . C63 C 0.6813(4) 0.3210(7) 0.5054(4) 0.0330(19) Uani 1 1 d . . . H63 H 0.6753 0.2951 0.5474 0.040 Uiso 1 1 calc R . . C62 C 0.6394(4) 0.2764(6) 0.4517(4) 0.0281(17) Uani 1 1 d . . . H62 H 0.6057 0.2183 0.4575 0.034 Uiso 1 1 calc R . . C71 C 0.4817(4) 0.3036(6) 0.3886(3) 0.0260(17) Uani 1 1 d . . . C72 C 0.4848(4) 0.4164(7) 0.4052(4) 0.0334(19) Uani 1 1 d . . . H72 H 0.5163 0.4649 0.3852 0.040 Uiso 1 1 calc R . . C73 C 0.4434(5) 0.4592(8) 0.4498(4) 0.045(2) Uani 1 1 d . . . H73 H 0.4443 0.5371 0.4596 0.054 Uiso 1 1 calc R . . C74 C 0.3988(5) 0.3845(10) 0.4814(4) 0.055(3) Uani 1 1 d . . . H74 H 0.3690 0.4120 0.5121 0.066 Uiso 1 1 calc R . . C75 C 0.3993(5) 0.2727(8) 0.4669(4) 0.042(2) Uani 1 1 d . . . H75 H 0.3726 0.2221 0.4903 0.051 Uiso 1 1 calc R . . C76 C 0.4374(4) 0.2324(7) 0.4197(4) 0.034(2) Uani 1 1 d . . . H76 H 0.4336 0.1555 0.4079 0.041 Uiso 1 1 calc R . . C81 C 0.2930(4) 0.1701(6) 0.2235(4) 0.0266(17) Uani 1 1 d . . . C82 C 0.2588(4) 0.1648(7) 0.2802(4) 0.0326(19) Uani 1 1 d . . . H82 H 0.2871 0.1662 0.3209 0.039 Uiso 1 1 calc R . . C83 C 0.1838(4) 0.1574(7) 0.2772(5) 0.041(2) Uani 1 1 d . . . H83 H 0.1608 0.1511 0.3155 0.049 Uiso 1 1 calc R . . C84 C 0.1434(5) 0.1591(7) 0.2184(4) 0.040(2) Uani 1 1 d . . . H84 H 0.0920 0.1575 0.2161 0.048 Uiso 1 1 calc R . . C85 C 0.1761(5) 0.1632(7) 0.1631(5) 0.046(2) Uani 1 1 d . . . H85 H 0.1473 0.1638 0.1226 0.055 Uiso 1 1 calc R . . C86 C 0.2517(4) 0.1666(6) 0.1655(4) 0.0315(18) Uani 1 1 d . . . H86 H 0.2742 0.1665 0.1268 0.038 Uiso 1 1 calc R . . N1 N 0.8669(3) -0.0698(5) 0.2067(3) 0.0206(13) Uani 1 1 d . . . N2 N 0.8073(3) -0.0569(5) 0.2400(3) 0.0199(13) Uani 1 1 d . . . N3 N 0.6910(3) -0.0441(5) 0.3043(3) 0.0248(14) Uani 1 1 d . . . N4 N 0.6324(3) -0.0458(5) 0.3388(3) 0.0268(15) Uani 1 1 d . . . N5 N 0.6976(3) 0.2475(5) 0.2759(3) 0.0273(14) Uani 1 1 d . . . N6 N 0.6245(3) 0.2323(5) 0.2820(3) 0.0211(13) Uani 1 1 d . . . N7 N 0.4815(3) 0.2214(5) 0.2824(3) 0.0254(14) Uani 1 1 d . . . N8 N 0.4066(3) 0.2212(5) 0.2799(3) 0.0264(14) Uani 1 1 d . . . O1 O 0.7829(3) -0.1028(5) 0.1162(2) 0.0311(13) Uani 1 1 d . . . O2 O 0.5602(2) -0.0074(4) 0.2406(2) 0.0238(11) Uani 1 1 d . . . O3 O 0.6803(2) 0.1286(4) 0.1855(2) 0.0228(11) Uani 1 1 d . . . O4 O 0.4058(3) 0.1320(5) 0.1815(2) 0.0325(13) 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 Pb1 0.01640(14) 0.02630(17) 0.02317(14) -0.00116(12) 0.00176(10) -0.00127(12) Pb2 0.01934(15) 0.03227(18) 0.02227(14) -0.00121(12) 0.00128(11) 0.00221(13) C1 0.020(4) 0.021(4) 0.025(4) 0.005(3) 0.007(3) 0.000(3) C2 0.017(4) 0.023(4) 0.026(4) 0.001(3) 0.008(3) 0.003(3) C3 0.021(4) 0.023(4) 0.020(4) 0.005(3) 0.002(3) 0.001(3) C4 0.017(4) 0.028(4) 0.033(4) -0.007(3) 0.006(3) -0.006(3) C5 0.024(4) 0.029(5) 0.026(4) 0.003(3) 0.001(3) 0.002(3) C6 0.019(4) 0.014(4) 0.028(4) 0.003(3) 0.004(3) 0.002(3) C7 0.019(4) 0.026(4) 0.024(4) 0.005(3) 0.003(3) 0.002(3) C8 0.012(3) 0.025(4) 0.023(4) 0.002(3) -0.001(3) 0.000(3) C11 0.025(4) 0.022(4) 0.029(4) 0.000(3) 0.011(3) 0.004(3) C12 0.027(4) 0.042(5) 0.024(4) 0.006(3) 0.004(3) 0.004(4) C13 0.045(5) 0.044(5) 0.024(4) -0.003(4) 0.016(4) 0.016(4) C14 0.032(5) 0.044(5) 0.037(5) 0.001(4) 0.015(4) 0.006(4) C15 0.024(4) 0.055(6) 0.035(5) 0.005(4) 0.008(4) 0.003(4) C16 0.023(4) 0.035(5) 0.037(4) -0.005(4) 0.002(3) 0.000(4) C21 0.015(4) 0.027(4) 0.024(4) -0.005(3) 0.008(3) 0.002(3) C22 0.016(4) 0.033(5) 0.033(4) 0.003(3) 0.001(3) 0.006(3) C23 0.019(4) 0.033(5) 0.048(5) -0.006(4) 0.009(4) 0.002(4) C24 0.012(4) 0.050(6) 0.045(5) -0.016(4) -0.001(3) 0.005(4) C25 0.023(4) 0.044(5) 0.025(4) -0.004(4) -0.003(3) 0.009(4) C26 0.025(4) 0.030(4) 0.021(4) -0.002(3) 0.007(3) 0.004(3) C31 0.014(4) 0.034(5) 0.021(4) -0.003(3) 0.005(3) 0.002(3) C32 0.029(5) 0.034(5) 0.043(5) -0.008(4) 0.001(4) 0.014(4) C33 0.019(4) 0.052(6) 0.049(5) -0.026(5) -0.002(4) 0.007(4) C34 0.023(5) 0.076(7) 0.029(4) -0.004(5) 0.006(4) 0.017(5) C35 0.028(5) 0.061(6) 0.029(4) 0.007(4) 0.007(4) 0.000(4) C36 0.023(4) 0.048(5) 0.026(4) -0.002(4) 0.005(3) -0.006(4) C41 0.022(4) 0.026(4) 0.023(4) 0.000(3) 0.002(3) -0.002(3) C42 0.028(5) 0.042(5) 0.037(5) 0.005(4) 0.009(4) 0.000(4) C43 0.032(5) 0.053(6) 0.029(4) 0.005(4) 0.015(4) 0.004(4) C44 0.027(4) 0.034(5) 0.048(5) 0.007(4) 0.019(4) -0.003(4) C45 0.018(4) 0.016(4) 0.050(5) -0.002(3) 0.006(3) 0.001(3) C46 0.019(4) 0.028(5) 0.047(5) 0.004(4) 0.007(4) -0.002(3) C51 0.021(4) 0.032(5) 0.021(4) 0.008(3) 0.005(3) 0.006(3) C56 0.030(4) 0.029(5) 0.036(4) 0.002(4) 0.001(4) 0.003(4) C55 0.033(5) 0.046(5) 0.031(4) 0.015(4) 0.011(4) 0.004(4) C54 0.024(5) 0.060(6) 0.047(5) 0.026(5) 0.006(4) -0.012(4) C53 0.029(5) 0.042(5) 0.047(5) 0.003(4) 0.004(4) -0.014(4) C52 0.029(5) 0.039(5) 0.038(5) -0.005(4) 0.006(4) -0.001(4) C61 0.012(4) 0.028(4) 0.026(4) -0.006(3) -0.002(3) 0.002(3) C66 0.027(4) 0.029(4) 0.024(4) 0.002(3) 0.007(3) 0.000(3) C65 0.028(5) 0.034(5) 0.037(5) -0.005(4) 0.000(4) -0.004(4) C64 0.028(4) 0.043(5) 0.031(4) -0.009(4) -0.007(3) 0.005(4) C63 0.032(5) 0.039(5) 0.027(4) 0.008(4) -0.002(3) 0.015(4) C62 0.021(4) 0.027(4) 0.037(4) -0.001(3) 0.005(3) 0.001(3) C71 0.022(4) 0.030(5) 0.026(4) 0.002(3) 0.001(3) 0.008(3) C72 0.028(4) 0.039(5) 0.032(4) -0.004(4) -0.001(3) 0.010(4) C73 0.031(5) 0.059(6) 0.046(5) -0.016(5) 0.004(4) 0.011(5) C74 0.030(5) 0.098(9) 0.036(5) -0.015(5) 0.001(4) 0.022(5) C75 0.035(5) 0.057(6) 0.035(5) 0.008(4) 0.005(4) 0.009(5) C76 0.025(4) 0.046(5) 0.031(4) 0.005(4) 0.002(3) 0.010(4) C81 0.023(4) 0.020(4) 0.036(4) 0.004(3) -0.003(3) 0.003(3) C82 0.028(4) 0.034(5) 0.036(4) 0.001(4) 0.004(3) 0.000(4) C83 0.027(5) 0.034(5) 0.064(6) -0.006(4) 0.011(4) -0.005(4) C84 0.030(5) 0.032(5) 0.059(6) -0.002(4) 0.006(4) 0.005(4) C85 0.032(5) 0.039(6) 0.062(6) -0.006(5) -0.018(4) 0.000(4) C86 0.026(4) 0.024(4) 0.044(5) -0.005(4) 0.001(4) 0.003(4) N1 0.017(3) 0.027(3) 0.019(3) 0.001(3) 0.007(2) 0.000(3) N2 0.016(3) 0.028(4) 0.016(3) 0.003(2) 0.002(2) 0.000(3) N3 0.017(3) 0.034(4) 0.024(3) 0.001(3) 0.006(3) -0.003(3) N4 0.016(3) 0.041(4) 0.025(3) -0.003(3) 0.009(3) -0.001(3) N5 0.016(3) 0.036(4) 0.030(3) 0.000(3) 0.005(3) -0.002(3) N6 0.017(3) 0.026(3) 0.021(3) -0.005(3) 0.006(2) -0.003(3) N7 0.012(3) 0.034(4) 0.031(3) -0.004(3) 0.004(3) 0.001(3) N8 0.020(3) 0.030(4) 0.030(3) 0.000(3) 0.005(3) -0.002(3) O1 0.017(3) 0.055(4) 0.021(3) 0.000(2) 0.000(2) 0.002(3) O2 0.020(3) 0.032(3) 0.021(3) -0.001(2) 0.007(2) -0.002(2) O3 0.019(3) 0.030(3) 0.019(2) -0.003(2) 0.002(2) -0.007(2) O4 0.023(3) 0.046(3) 0.027(3) -0.009(3) -0.001(2) -0.004(3) _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 Pb1 O3 2.479(5) . ? Pb1 N2 2.489(6) . ? Pb1 N3 2.492(6) . ? Pb1 O1 2.518(5) . ? Pb1 O2 2.767(5) . ? Pb2 O2 2.365(5) . ? Pb2 N7 2.417(6) . ? Pb2 N6 2.465(6) . ? Pb2 O4 2.528(5) . ? Pb2 O3 2.642(5) . ? C1 O1 1.266(8) . ? C1 N1 1.349(9) . ? C1 C11 1.507(9) . ? C2 N2 1.293(8) . ? C2 C21 1.484(10) . ? C2 C3 1.501(9) . ? C3 N3 1.309(9) . ? C3 C31 1.493(9) . ? C4 O2 1.295(8) . ? C4 N4 1.350(9) . ? C4 C41 1.522(10) . ? C5 O3 1.319(9) . ? C5 N5 1.319(9) . ? C5 C51 1.511(10) . ? C6 N6 1.294(8) . ? C6 C7 1.464(10) . ? C6 C61 1.502(9) . ? C7 N7 1.329(9) . ? C7 C71 1.489(10) . ? C8 O4 1.247(8) . ? C8 N8 1.333(9) . ? C8 C81 1.522(10) . ? C11 C16 1.374(10) . ? C11 C12 1.386(10) . ? C12 C13 1.400(10) . ? C13 C14 1.389(11) . ? C14 C15 1.339(11) . ? C15 C16 1.398(10) . ? C21 C22 1.377(10) . ? C21 C26 1.388(10) . ? C22 C23 1.393(10) . ? C23 C24 1.378(11) . ? C24 C25 1.366(11) . ? C25 C26 1.389(10) . ? C31 C36 1.366(10) . ? C31 C32 1.385(11) . ? C32 C33 1.390(11) . ? C33 C34 1.361(12) . ? C34 C35 1.374(12) . ? C35 C36 1.371(10) . ? C41 C42 1.386(10) . ? C41 C46 1.394(10) . ? C42 C43 1.389(10) . ? C43 C44 1.385(11) . ? C44 C45 1.386(11) . ? C45 C46 1.383(10) . ? C51 C52 1.366(11) . ? C51 C56 1.390(10) . ? C56 C55 1.386(11) . ? C55 C54 1.343(12) . ? C54 C53 1.374(12) . ? C53 C52 1.384(11) . ? C61 C62 1.388(10) . ? C61 C66 1.390(10) . ? C66 C65 1.399(10) . ? C65 C64 1.366(11) . ? C64 C63 1.419(11) . ? C63 C62 1.399(10) . ? C71 C72 1.389(11) . ? C71 C76 1.391(11) . ? C72 C73 1.370(11) . ? C73 C74 1.425(13) . ? C74 C75 1.366(13) . ? C75 C76 1.363(11) . ? C81 C86 1.363(10) . ? C81 C82 1.404(10) . ? C82 C83 1.388(11) . ? C83 C84 1.367(12) . ? C84 C85 1.363(12) . ? C85 C86 1.397(11) . ? N1 N2 1.378(7) . ? N3 N4 1.367(8) . ? N5 N6 1.387(8) . ? N7 N8 1.384(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 O3 Pb1 N2 84.46(17) . . ? O3 Pb1 N3 80.61(17) . . ? N2 Pb1 N3 64.76(18) . . ? O3 Pb1 O1 96.63(16) . . ? N2 Pb1 O1 63.52(17) . . ? N3 Pb1 O1 128.22(17) . . ? O3 Pb1 O2 71.61(14) . . ? N2 Pb1 O2 123.04(16) . . ? N3 Pb1 O2 60.85(16) . . ? O1 Pb1 O2 164.72(15) . . ? O2 Pb2 N7 85.91(18) . . ? O2 Pb2 N6 82.38(18) . . ? N7 Pb2 N6 65.95(19) . . ? O2 Pb2 O4 88.71(17) . . ? N7 Pb2 O4 64.21(18) . . ? N6 Pb2 O4 129.82(17) . . ? O2 Pb2 O3 75.65(15) . . ? N7 Pb2 O3 127.24(17) . . ? N6 Pb2 O3 62.89(16) . . ? O4 Pb2 O3 158.86(17) . . ? O1 C1 N1 127.9(6) . . ? O1 C1 C11 119.7(6) . . ? N1 C1 C11 112.4(6) . . ? N2 C2 C21 124.3(6) . . ? N2 C2 C3 115.8(6) . . ? C21 C2 C3 119.8(6) . . ? N3 C3 C31 123.9(6) . . ? N3 C3 C2 117.4(6) . . ? C31 C3 C2 118.7(6) . . ? O2 C4 N4 127.3(6) . . ? O2 C4 C41 120.1(6) . . ? N4 C4 C41 112.5(6) . . ? O3 C5 N5 126.6(7) . . ? O3 C5 C51 119.5(6) . . ? N5 C5 C51 113.9(6) . . ? N6 C6 C7 116.7(6) . . ? N6 C6 C61 122.9(6) . . ? C7 C6 C61 120.3(6) . . ? N7 C7 C6 117.4(6) . . ? N7 C7 C71 118.7(6) . . ? C6 C7 C71 123.7(6) . . ? O4 C8 N8 127.6(6) . . ? O4 C8 C81 119.8(6) . . ? N8 C8 C81 112.7(6) . . ? C16 C11 C12 119.1(7) . . ? C16 C11 C1 121.8(7) . . ? C12 C11 C1 119.0(7) . . ? C11 C12 C13 119.9(8) . . ? C14 C13 C12 119.5(7) . . ? C15 C14 C13 120.5(7) . . ? C14 C15 C16 120.4(8) . . ? C11 C16 C15 120.5(7) . . ? C22 C21 C26 117.9(7) . . ? C22 C21 C2 119.7(6) . . ? C26 C21 C2 122.3(6) . . ? C21 C22 C23 121.4(7) . . ? C24 C23 C22 119.3(8) . . ? C25 C24 C23 120.3(7) . . ? C24 C25 C26 119.9(7) . . ? C21 C26 C25 121.0(7) . . ? C36 C31 C32 118.0(7) . . ? C36 C31 C3 121.8(7) . . ? C32 C31 C3 120.1(7) . . ? C31 C32 C33 119.8(8) . . ? C34 C33 C32 120.7(8) . . ? C33 C34 C35 119.7(8) . . ? C36 C35 C34 119.3(8) . . ? C31 C36 C35 122.3(8) . . ? C42 C41 C46 120.2(7) . . ? C42 C41 C4 120.8(7) . . ? C46 C41 C4 119.0(6) . . ? C41 C42 C43 119.5(8) . . ? C44 C43 C42 120.4(8) . . ? C43 C44 C45 120.0(7) . . ? C46 C45 C44 120.2(8) . . ? C45 C46 C41 119.8(8) . . ? C52 C51 C56 119.0(7) . . ? C52 C51 C5 121.6(7) . . ? C56 C51 C5 119.4(7) . . ? C55 C56 C51 120.5(8) . . ? C54 C55 C56 119.5(8) . . ? C55 C54 C53 121.0(8) . . ? C54 C53 C52 119.9(8) . . ? C51 C52 C53 120.0(8) . . ? C62 C61 C66 119.0(6) . . ? C62 C61 C6 120.0(7) . . ? C66 C61 C6 121.0(6) . . ? C61 C66 C65 120.3(7) . . ? C64 C65 C66 121.1(8) . . ? C65 C64 C63 119.4(7) . . ? C62 C63 C64 118.9(7) . . ? C61 C62 C63 121.2(7) . . ? C72 C71 C76 119.1(7) . . ? C72 C71 C7 120.6(7) . . ? C76 C71 C7 120.1(7) . . ? C73 C72 C71 121.3(8) . . ? C72 C73 C74 118.6(9) . . ? C75 C74 C73 119.3(8) . . ? C76 C75 C74 121.4(9) . . ? C75 C76 C71 120.1(8) . . ? C86 C81 C82 119.1(7) . . ? C86 C81 C8 120.1(7) . . ? C82 C81 C8 120.7(7) . . ? C83 C82 C81 120.4(8) . . ? C84 C83 C82 119.2(8) . . ? C85 C84 C83 120.8(8) . . ? C84 C85 C86 120.5(8) . . ? C81 C86 C85 119.8(8) . . ? C1 N1 N2 111.0(5) . . ? C2 N2 N1 116.9(6) . . ? C2 N2 Pb1 121.6(4) . . ? N1 N2 Pb1 121.5(4) . . ? C3 N3 N4 116.8(6) . . ? C3 N3 Pb1 120.1(4) . . ? N4 N3 Pb1 123.1(4) . . ? C4 N4 N3 112.7(6) . . ? C5 N5 N6 113.2(6) . . ? C6 N6 N5 118.8(6) . . ? C6 N6 Pb2 119.9(5) . . ? N5 N6 Pb2 120.5(4) . . ? C7 N7 N8 119.0(6) . . ? C7 N7 Pb2 120.0(4) . . ? N8 N7 Pb2 120.8(4) . . ? C8 N8 N7 112.1(6) . . ? C1 O1 Pb1 116.1(4) . . ? C4 O2 Pb2 128.9(4) . . ? C4 O2 Pb1 108.4(4) . . ? Pb2 O2 Pb1 100.40(15) . . ? C5 O3 Pb1 129.1(4) . . ? C5 O3 Pb2 109.1(4) . . ? Pb1 O3 Pb2 100.94(16) . . ? C8 O4 Pb2 114.1(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.626 _refine_diff_density_min -1.991 _refine_diff_density_rms 0.358 # Attachment 'Complex_4.cif' data_el20 _database_code_depnum_ccdc_archive 'CCDC 710844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H60 N12 O6 Zn3' _chemical_formula_sum 'C84 H60 N12 O6 Zn3' _chemical_formula_weight 1529.55 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 15.6131(12) _cell_length_b 18.2359(15) _cell_length_c 25.3841(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.908(4) _cell_angle_gamma 90.00 _cell_volume 7218.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9530 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 25.05 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8169 _exptl_absorpt_correction_T_max 0.9020 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 134872 _diffrn_reflns_av_R_equivalents 0.0870 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.84 _reflns_number_total 13936 _reflns_number_gt 9843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0565P)^2^+2.8973P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13936 _refine_ls_number_parameters 946 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _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 Zn1 Zn -0.10374(2) 0.81844(2) 0.248052(14) 0.01642(10) Uani 1 1 d . . . Zn2 Zn 0.17326(2) 0.819505(19) 0.183729(14) 0.01560(10) Uani 1 1 d . . . Zn3 Zn -0.06450(2) 0.774979(19) 0.071388(14) 0.01616(10) Uani 1 1 d . . . C1 C -0.1850(2) 0.78705(17) 0.33879(13) 0.0192(7) Uani 1 1 d . . . C2 C 0.0186(2) 0.73339(18) 0.32046(13) 0.0197(7) Uani 1 1 d . . . C3 C 0.0773(2) 0.73773(18) 0.27633(13) 0.0187(7) Uani 1 1 d . . . C4 C 0.0628(2) 0.91174(17) 0.23107(12) 0.0168(7) Uani 1 1 d . . . C5 C 0.3488(2) 0.79917(17) 0.18333(13) 0.0177(7) Uani 1 1 d . . . C6 C 0.2048(2) 0.68795(17) 0.11711(13) 0.0185(7) Uani 1 1 d . . . C7 C 0.1102(2) 0.69138(17) 0.10623(12) 0.0170(7) Uani 1 1 d . . . C8 C 0.0675(2) 0.87234(17) 0.08260(12) 0.0159(7) Uani 1 1 d . . . C9 C -0.1444(2) 0.70086(17) -0.01186(12) 0.0163(7) Uani 1 1 d . . . C10 C -0.1845(2) 0.66359(17) 0.11581(13) 0.0185(7) Uani 1 1 d . . . C11 C -0.1556(2) 0.69471(17) 0.16722(13) 0.0169(7) Uani 1 1 d . . . C12 C -0.1460(2) 0.87918(17) 0.15189(13) 0.0175(7) Uani 1 1 d . . . C13 C -0.2538(2) 0.77897(18) 0.37617(14) 0.0224(8) Uani 1 1 d . . . C14 C -0.3373(2) 0.7967(2) 0.35974(16) 0.0321(9) Uani 1 1 d . . . H14 H -0.3492 0.8164 0.3255 0.038 Uiso 1 1 calc R . . C15 C -0.4030(2) 0.7856(2) 0.39309(18) 0.0392(10) Uani 1 1 d . . . H15 H -0.4601 0.7973 0.3814 0.047 Uiso 1 1 calc R . . C16 C -0.3873(3) 0.7583(2) 0.44237(17) 0.0353(10) Uani 1 1 d . . . H16 H -0.4331 0.7504 0.4649 0.042 Uiso 1 1 calc R . . C17 C -0.3039(3) 0.74196(19) 0.45950(16) 0.0339(10) Uani 1 1 d . . . H17 H -0.2924 0.7240 0.4943 0.041 Uiso 1 1 calc R . . C18 C -0.2376(2) 0.75163(19) 0.42654(14) 0.0258(8) Uani 1 1 d . . . H18 H -0.1807 0.7395 0.4384 0.031 Uiso 1 1 calc R . . C21 C 0.0512(2) 0.7030(2) 0.37191(14) 0.0249(8) Uani 1 1 d . . . C22 C 0.0072(2) 0.6482(2) 0.39660(15) 0.0343(9) Uani 1 1 d . . . H22 H -0.0426 0.6272 0.3796 0.041 Uiso 1 1 calc R . . C23 C 0.0352(3) 0.6239(3) 0.44594(17) 0.0480(12) Uani 1 1 d . . . H23 H 0.0056 0.5854 0.4625 0.058 Uiso 1 1 calc R . . C24 C 0.1062(3) 0.6555(3) 0.47129(18) 0.0574(14) Uani 1 1 d . . . H24 H 0.1247 0.6395 0.5056 0.069 Uiso 1 1 calc R . . C25 C 0.1499(3) 0.7094(3) 0.44723(17) 0.0525(13) Uani 1 1 d . . . H25 H 0.1989 0.7310 0.4648 0.063 Uiso 1 1 calc R . . C26 C 0.1231(2) 0.7331(2) 0.39698(15) 0.0355(10) Uani 1 1 d . . . H26 H 0.1544 0.7701 0.3799 0.043 Uiso 1 1 calc R . . C31 C 0.1362(2) 0.67514(17) 0.27149(13) 0.0192(7) Uani 1 1 d . . . C32 C 0.1058(2) 0.60454(18) 0.27910(14) 0.0247(8) Uani 1 1 d . . . H32 H 0.0484 0.5971 0.2885 0.030 Uiso 1 1 calc R . . C33 C 0.1593(2) 0.54519(19) 0.27295(14) 0.0291(9) Uani 1 1 d . . . H33 H 0.1382 0.4969 0.2779 0.035 Uiso 1 1 calc R . . C34 C 0.2424(2) 0.5552(2) 0.25975(14) 0.0302(9) Uani 1 1 d . . . H34 H 0.2786 0.5141 0.2549 0.036 Uiso 1 1 calc R . . C35 C 0.2732(2) 0.6253(2) 0.25351(14) 0.0262(8) Uani 1 1 d . . . H35 H 0.3311 0.6326 0.2448 0.031 Uiso 1 1 calc R . . C36 C 0.2207(2) 0.68456(19) 0.25988(13) 0.0208(7) Uani 1 1 d . . . H36 H 0.2429 0.7327 0.2562 0.025 Uiso 1 1 calc R . . C41 C 0.0193(2) 0.98341(18) 0.23600(13) 0.0200(7) Uani 1 1 d . . . C42 C 0.0434(2) 1.03930(18) 0.20303(14) 0.0218(8) Uani 1 1 d . . . H42 H 0.0843 1.0299 0.1774 0.026 Uiso 1 1 calc R . . C43 C 0.0089(2) 1.10831(19) 0.20687(14) 0.0247(8) Uani 1 1 d . . . H43 H 0.0256 1.1462 0.1839 0.030 Uiso 1 1 calc R . . C44 C -0.0496(2) 1.12211(19) 0.24401(15) 0.0283(8) Uani 1 1 d . . . H44 H -0.0733 1.1699 0.2469 0.034 Uiso 1 1 calc R . . C45 C -0.0744(2) 1.0671(2) 0.27729(15) 0.0312(9) Uani 1 1 d . . . H45 H -0.1150 1.0771 0.3030 0.037 Uiso 1 1 calc R . . C46 C -0.0404(2) 0.99730(19) 0.27329(13) 0.0242(8) Uani 1 1 d . . . H46 H -0.0579 0.9592 0.2959 0.029 Uiso 1 1 calc R . . C51 C 0.4422(2) 0.81041(18) 0.19218(14) 0.0214(7) Uani 1 1 d . . . C52 C 0.4721(2) 0.85764(18) 0.23134(14) 0.0240(8) Uani 1 1 d . . . H52 H 0.4325 0.8824 0.2523 0.029 Uiso 1 1 calc R . . C53 C 0.5589(2) 0.8692(2) 0.24037(15) 0.0321(9) Uani 1 1 d . . . H53 H 0.5787 0.9009 0.2681 0.039 Uiso 1 1 calc R . . C54 C 0.6168(2) 0.8354(2) 0.20968(17) 0.0366(10) Uani 1 1 d . . . H54 H 0.6765 0.8444 0.2153 0.044 Uiso 1 1 calc R . . C55 C 0.5872(2) 0.7881(2) 0.17067(17) 0.0392(10) Uani 1 1 d . . . H55 H 0.6269 0.7640 0.1494 0.047 Uiso 1 1 calc R . . C56 C 0.5009(2) 0.7754(2) 0.16215(16) 0.0333(9) Uani 1 1 d . . . H56 H 0.4814 0.7422 0.1353 0.040 Uiso 1 1 calc R . . C61 C 0.2541(2) 0.63121(17) 0.09067(13) 0.0194(7) Uani 1 1 d . . . C62 C 0.3250(2) 0.59789(18) 0.11567(15) 0.0242(8) Uani 1 1 d . . . H62 H 0.3414 0.6106 0.1511 0.029 Uiso 1 1 calc R . . C63 C 0.3718(2) 0.54661(19) 0.08962(16) 0.0302(9) Uani 1 1 d . . . H63 H 0.4200 0.5239 0.1072 0.036 Uiso 1 1 calc R . . C64 C 0.3491(2) 0.5283(2) 0.03865(17) 0.0348(10) Uani 1 1 d . . . H64 H 0.3821 0.4934 0.0207 0.042 Uiso 1 1 calc R . . C65 C 0.2784(2) 0.5602(2) 0.01313(16) 0.0329(9) Uani 1 1 d . . . H65 H 0.2628 0.5473 -0.0223 0.039 Uiso 1 1 calc R . . C66 C 0.2307(2) 0.61080(18) 0.03921(14) 0.0245(8) Uani 1 1 d . . . H66 H 0.1813 0.6320 0.0219 0.029 Uiso 1 1 calc R . . C71 C 0.0653(2) 0.62047(17) 0.10017(13) 0.0177(7) Uani 1 1 d . . . C72 C 0.0825(2) 0.56610(18) 0.13718(14) 0.0236(8) Uani 1 1 d . . . H72 H 0.1232 0.5744 0.1656 0.028 Uiso 1 1 calc R . . C73 C 0.0405(2) 0.50000(19) 0.13272(16) 0.0304(9) Uani 1 1 d . . . H73 H 0.0520 0.4628 0.1583 0.037 Uiso 1 1 calc R . . C74 C -0.0181(2) 0.48743(19) 0.09145(17) 0.0342(10) Uani 1 1 d . . . H74 H -0.0476 0.4419 0.0890 0.041 Uiso 1 1 calc R . . C75 C -0.0341(2) 0.54041(19) 0.05379(16) 0.0297(9) Uani 1 1 d . . . H75 H -0.0744 0.5315 0.0252 0.036 Uiso 1 1 calc R . . C76 C 0.0086(2) 0.60659(18) 0.05771(14) 0.0215(8) Uani 1 1 d . . . H76 H -0.0010 0.6428 0.0311 0.026 Uiso 1 1 calc R . . C81 C 0.1074(2) 0.94573(17) 0.08493(12) 0.0190(7) Uani 1 1 d . . . C82 C 0.0578(2) 1.00464(18) 0.06646(13) 0.0220(8) Uani 1 1 d . . . H82 H 0.0011 0.9966 0.0523 0.026 Uiso 1 1 calc R . . C83 C 0.0909(2) 1.07455(19) 0.06865(14) 0.0274(8) Uani 1 1 d . . . H83 H 0.0569 1.1147 0.0560 0.033 Uiso 1 1 calc R . . C84 C 0.1725(3) 1.08644(19) 0.08894(15) 0.0312(9) Uani 1 1 d . . . H84 H 0.1944 1.1350 0.0914 0.037 Uiso 1 1 calc R . . C85 C 0.2233(2) 1.02809(19) 0.10595(14) 0.0272(8) Uani 1 1 d . . . H85 H 0.2804 1.0366 0.1192 0.033 Uiso 1 1 calc R . . C86 C 0.1913(2) 0.95790(18) 0.10374(13) 0.0208(7) Uani 1 1 d . . . H86 H 0.2265 0.9178 0.1150 0.025 Uiso 1 1 calc R . . C91 C -0.1656(2) 0.67713(17) -0.06639(13) 0.0190(7) Uani 1 1 d . . . C92 C -0.1347(2) 0.71603(18) -0.10797(13) 0.0200(7) Uani 1 1 d . . . H92 H -0.0993 0.7577 -0.1013 0.024 Uiso 1 1 calc R . . C93 C -0.1548(2) 0.69487(19) -0.15877(14) 0.0245(8) Uani 1 1 d . . . H93 H -0.1324 0.7216 -0.1871 0.029 Uiso 1 1 calc R . . C94 C -0.2070(2) 0.63546(19) -0.16927(14) 0.0266(8) Uani 1 1 d . . . H94 H -0.2213 0.6215 -0.2047 0.032 Uiso 1 1 calc R . . C95 C -0.2382(2) 0.5965(2) -0.12838(14) 0.0301(9) Uani 1 1 d . . . H95 H -0.2743 0.5553 -0.1355 0.036 Uiso 1 1 calc R . . C96 C -0.2178(2) 0.61643(18) -0.07693(14) 0.0256(8) Uani 1 1 d . . . H96 H -0.2392 0.5888 -0.0487 0.031 Uiso 1 1 calc R . . C101 C -0.2529(2) 0.60742(18) 0.11218(13) 0.0198(7) Uani 1 1 d . . . C102 C -0.3311(2) 0.6254(2) 0.08772(14) 0.0269(8) Uani 1 1 d . . . H102 H -0.3406 0.6739 0.0750 0.032 Uiso 1 1 calc R . . C103 C -0.3954(2) 0.5743(2) 0.08152(15) 0.0333(9) Uani 1 1 d . . . H103 H -0.4490 0.5875 0.0648 0.040 Uiso 1 1 calc R . . C104 C -0.3820(3) 0.5043(2) 0.09958(15) 0.0363(10) Uani 1 1 d . . . H104 H -0.4262 0.4688 0.0949 0.044 Uiso 1 1 calc R . . C105 C -0.3051(3) 0.4853(2) 0.12437(15) 0.0334(9) Uani 1 1 d . . . H105 H -0.2963 0.4368 0.1372 0.040 Uiso 1 1 calc R . . C106 C -0.2406(2) 0.53666(19) 0.13066(14) 0.0264(8) Uani 1 1 d . . . H106 H -0.1873 0.5234 0.1478 0.032 Uiso 1 1 calc R . . C116 C -0.1624(2) 0.64893(17) 0.21522(13) 0.0179(7) Uani 1 1 d . . . C115 C -0.2279(2) 0.66225(18) 0.24829(13) 0.0215(8) Uani 1 1 d . . . H116 H -0.2677 0.7006 0.2403 0.026 Uiso 1 1 calc R . . C114 C -0.2361(2) 0.6203(2) 0.29290(14) 0.0279(8) Uani 1 1 d . . . H115 H -0.2815 0.6298 0.3155 0.034 Uiso 1 1 calc R . . C113 C -0.1793(2) 0.5652(2) 0.30470(14) 0.0291(9) Uani 1 1 d . . . H114 H -0.1855 0.5358 0.3351 0.035 Uiso 1 1 calc R . . C112 C -0.1131(2) 0.5526(2) 0.27247(15) 0.0307(9) Uani 1 1 d . . . H113 H -0.0724 0.5153 0.2813 0.037 Uiso 1 1 calc R . . C111 C -0.1050(2) 0.59352(19) 0.22729(14) 0.0253(8) Uani 1 1 d . . . H112 H -0.0599 0.5834 0.2046 0.030 Uiso 1 1 calc R . . C121 C -0.1640(2) 0.93594(18) 0.11138(13) 0.0196(7) Uani 1 1 d . . . C122 C -0.1449(2) 1.00790(18) 0.12424(14) 0.0219(8) Uani 1 1 d . . . H122 H -0.1179 1.0192 0.1576 0.026 Uiso 1 1 calc R . . C123 C -0.1646(2) 1.06305(19) 0.08908(14) 0.0275(8) Uani 1 1 d . . . H123 H -0.1487 1.1122 0.0973 0.033 Uiso 1 1 calc R . . C124 C -0.2074(3) 1.0469(2) 0.04192(15) 0.0398(11) Uani 1 1 d . . . H124 H -0.2226 1.0851 0.0178 0.048 Uiso 1 1 calc R . . C125 C -0.2281(3) 0.9759(2) 0.02961(15) 0.0448(12) Uani 1 1 d . . . H125 H -0.2583 0.9650 -0.0029 0.054 Uiso 1 1 calc R . . C126 C -0.2056(3) 0.9204(2) 0.06380(14) 0.0311(9) Uani 1 1 d . . . H126 H -0.2187 0.8710 0.0546 0.037 Uiso 1 1 calc R . . N1 N -0.11308(17) 0.75247(15) 0.35183(11) 0.0205(6) Uani 1 1 d . . . N2 N -0.05799(17) 0.75751(14) 0.31211(10) 0.0181(6) Uani 1 1 d . . . N3 N 0.08260(16) 0.79112(14) 0.24337(10) 0.0170(6) Uani 1 1 d . . . N4 N 0.02621(16) 0.85086(14) 0.24797(10) 0.0162(6) Uani 1 1 d . . . N5 N 0.32625(16) 0.74111(14) 0.15448(11) 0.0196(6) Uani 1 1 d . . . N6 N 0.23890(17) 0.73761(14) 0.14774(11) 0.0184(6) Uani 1 1 d . . . N7 N 0.06529(17) 0.75073(14) 0.10068(10) 0.0156(6) Uani 1 1 d . . . N8 N 0.10620(17) 0.81826(14) 0.11003(11) 0.0181(6) Uani 1 1 d . . . N9 N -0.18036(17) 0.66383(14) 0.02621(10) 0.0185(6) Uani 1 1 d . . . N10 N -0.15221(16) 0.69037(14) 0.07413(10) 0.0167(6) Uani 1 1 d . . . N11 N -0.13227(16) 0.76142(14) 0.17654(10) 0.0168(6) Uani 1 1 d . . . N12 N -0.13124(17) 0.81111(14) 0.13440(10) 0.0171(6) Uani 1 1 d . . . O1 O -0.20037(14) 0.82458(12) 0.29688(9) 0.0224(5) Uani 1 1 d . . . O6 O -0.14980(14) 0.89670(12) 0.19939(9) 0.0200(5) Uani 1 1 d . . . O2 O 0.13565(13) 0.91379(11) 0.21187(9) 0.0192(5) Uani 1 1 d . . . O3 O 0.29755(14) 0.84413(12) 0.20355(9) 0.0212(5) Uani 1 1 d . . . O4 O -0.00017(14) 0.86414(12) 0.05410(9) 0.0202(5) Uani 1 1 d . . . O5 O -0.09272(14) 0.75427(12) -0.00490(9) 0.0208(5) 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 Zn1 0.0161(2) 0.0181(2) 0.0147(2) 0.00039(15) -0.00234(15) 0.00137(15) Zn2 0.01505(19) 0.01560(19) 0.0159(2) -0.00157(15) -0.00206(15) 0.00140(15) Zn3 0.01656(19) 0.01595(19) 0.0156(2) -0.00024(15) -0.00267(15) -0.00177(15) C1 0.0208(18) 0.0178(17) 0.0189(18) -0.0018(14) -0.0011(15) -0.0035(14) C2 0.0182(17) 0.0225(18) 0.0180(18) 0.0032(14) -0.0034(14) -0.0011(14) C3 0.0140(16) 0.0223(18) 0.0192(18) 0.0004(14) -0.0063(14) -0.0026(13) C4 0.0186(17) 0.0167(17) 0.0146(17) -0.0047(13) -0.0059(14) 0.0007(13) C5 0.0184(17) 0.0198(17) 0.0147(17) 0.0033(14) -0.0016(14) -0.0008(14) C6 0.0187(17) 0.0149(17) 0.0217(18) 0.0007(14) -0.0003(14) 0.0017(13) C7 0.0205(17) 0.0180(17) 0.0125(17) -0.0008(13) 0.0006(14) -0.0008(14) C8 0.0144(16) 0.0196(17) 0.0135(16) 0.0005(13) -0.0008(14) 0.0004(13) C9 0.0177(16) 0.0154(16) 0.0155(17) 0.0007(13) -0.0023(14) 0.0020(13) C10 0.0204(17) 0.0146(16) 0.0201(18) -0.0005(13) -0.0014(15) 0.0006(13) C11 0.0132(16) 0.0175(17) 0.0196(18) 0.0020(13) -0.0013(14) -0.0002(13) C12 0.0151(16) 0.0170(17) 0.0201(19) 0.0011(14) -0.0008(14) 0.0000(13) C13 0.0224(18) 0.0188(18) 0.026(2) -0.0069(15) 0.0040(15) -0.0016(14) C14 0.025(2) 0.033(2) 0.038(2) 0.0000(18) 0.0032(18) 0.0025(17) C15 0.019(2) 0.041(2) 0.059(3) -0.009(2) 0.011(2) -0.0027(17) C16 0.038(2) 0.023(2) 0.047(3) -0.0086(18) 0.023(2) -0.0072(17) C17 0.048(3) 0.021(2) 0.034(2) -0.0044(16) 0.014(2) -0.0062(18) C18 0.029(2) 0.0253(19) 0.024(2) -0.0026(15) 0.0045(16) -0.0015(16) C21 0.0208(18) 0.033(2) 0.0206(19) 0.0039(15) 0.0003(15) 0.0062(15) C22 0.029(2) 0.041(2) 0.032(2) 0.0126(19) -0.0029(18) -0.0009(18) C23 0.042(3) 0.060(3) 0.041(3) 0.029(2) -0.005(2) -0.005(2) C24 0.038(3) 0.096(4) 0.038(3) 0.035(3) -0.006(2) -0.003(3) C25 0.028(2) 0.095(4) 0.033(3) 0.020(3) -0.010(2) -0.009(2) C26 0.022(2) 0.058(3) 0.025(2) 0.0111(19) -0.0029(17) -0.0085(19) C31 0.0226(18) 0.0182(17) 0.0162(17) 0.0031(14) -0.0048(14) 0.0045(14) C32 0.0271(19) 0.0236(19) 0.0228(19) 0.0045(15) -0.0049(16) 0.0013(15) C33 0.040(2) 0.0175(18) 0.028(2) 0.0018(15) -0.0125(18) 0.0037(16) C34 0.036(2) 0.029(2) 0.024(2) -0.0021(16) -0.0076(17) 0.0172(17) C35 0.0222(19) 0.034(2) 0.0222(19) 0.0041(16) -0.0037(15) 0.0108(16) C36 0.0204(17) 0.0242(18) 0.0173(18) 0.0072(14) -0.0044(14) 0.0033(14) C41 0.0174(17) 0.0220(18) 0.0200(18) -0.0049(14) -0.0055(14) 0.0013(14) C42 0.0193(17) 0.0209(18) 0.0247(19) -0.0029(14) -0.0022(15) -0.0008(14) C43 0.0247(19) 0.0204(18) 0.028(2) 0.0008(15) -0.0039(16) -0.0009(15) C44 0.029(2) 0.0189(18) 0.036(2) -0.0026(16) -0.0044(17) 0.0052(15) C45 0.035(2) 0.031(2) 0.028(2) -0.0009(17) 0.0023(17) 0.0096(17) C46 0.0263(19) 0.0245(19) 0.0222(19) 0.0001(15) 0.0036(16) 0.0031(15) C51 0.0165(17) 0.0206(18) 0.027(2) 0.0000(15) -0.0032(15) -0.0008(14) C52 0.0215(18) 0.0208(18) 0.029(2) -0.0006(15) -0.0046(16) 0.0028(15) C53 0.029(2) 0.030(2) 0.036(2) 0.0012(17) -0.0143(18) -0.0030(17) C54 0.0207(19) 0.036(2) 0.052(3) 0.004(2) -0.0074(19) -0.0011(17) C55 0.0181(19) 0.048(3) 0.052(3) -0.010(2) 0.0034(19) 0.0037(18) C56 0.025(2) 0.034(2) 0.041(2) -0.0117(18) -0.0003(18) -0.0024(17) C61 0.0173(17) 0.0166(17) 0.0242(19) -0.0014(14) 0.0021(14) -0.0030(14) C62 0.0218(18) 0.0178(17) 0.033(2) -0.0018(15) 0.0001(16) -0.0001(14) C63 0.0240(19) 0.0219(19) 0.045(3) -0.0017(17) 0.0078(18) 0.0016(16) C64 0.031(2) 0.024(2) 0.051(3) -0.0093(18) 0.016(2) 0.0004(17) C65 0.038(2) 0.031(2) 0.031(2) -0.0097(17) 0.0096(19) -0.0072(18) C66 0.0260(19) 0.0213(18) 0.026(2) -0.0006(15) 0.0019(16) -0.0043(15) C71 0.0140(16) 0.0158(16) 0.0236(18) -0.0025(14) 0.0023(14) 0.0005(13) C72 0.0216(18) 0.0218(18) 0.027(2) 0.0032(15) 0.0019(15) 0.0039(15) C73 0.027(2) 0.0205(19) 0.044(2) 0.0083(17) 0.0046(18) 0.0000(16) C74 0.030(2) 0.0137(18) 0.059(3) -0.0061(18) 0.005(2) -0.0056(15) C75 0.0248(19) 0.0221(19) 0.041(2) -0.0102(17) -0.0064(17) 0.0029(15) C76 0.0189(17) 0.0184(17) 0.027(2) -0.0030(14) -0.0034(15) 0.0020(14) C81 0.0239(18) 0.0181(17) 0.0147(17) 0.0008(13) -0.0019(14) -0.0006(14) C82 0.0241(18) 0.0232(18) 0.0184(18) 0.0028(14) -0.0031(15) 0.0000(15) C83 0.035(2) 0.0188(18) 0.028(2) 0.0042(15) -0.0043(17) 0.0013(16) C84 0.044(2) 0.0177(18) 0.031(2) -0.0005(16) -0.0008(19) -0.0079(17) C85 0.027(2) 0.030(2) 0.024(2) 0.0014(16) -0.0059(16) -0.0100(16) C86 0.0231(18) 0.0218(18) 0.0170(18) 0.0031(14) -0.0038(15) -0.0005(14) C91 0.0212(17) 0.0169(17) 0.0184(18) -0.0002(14) -0.0033(14) 0.0037(14) C92 0.0180(17) 0.0214(18) 0.0203(19) 0.0015(14) -0.0025(15) 0.0048(14) C93 0.029(2) 0.0235(19) 0.0206(19) 0.0056(15) -0.0001(16) 0.0024(15) C94 0.035(2) 0.028(2) 0.0163(18) -0.0034(15) -0.0042(16) -0.0009(17) C95 0.041(2) 0.0229(19) 0.025(2) -0.0054(16) -0.0049(18) -0.0086(17) C96 0.036(2) 0.0203(18) 0.0203(19) -0.0011(15) -0.0001(16) -0.0059(16) C101 0.0216(18) 0.0207(17) 0.0173(18) -0.0015(14) 0.0029(15) -0.0058(14) C102 0.027(2) 0.028(2) 0.025(2) -0.0015(16) 0.0033(16) -0.0040(16) C103 0.029(2) 0.042(2) 0.029(2) -0.0059(18) -0.0014(17) -0.0120(18) C104 0.040(2) 0.037(2) 0.033(2) -0.0111(18) 0.0129(19) -0.0214(19) C105 0.047(3) 0.023(2) 0.032(2) -0.0036(16) 0.013(2) -0.0109(18) C106 0.030(2) 0.0238(19) 0.025(2) -0.0031(15) 0.0042(16) -0.0004(16) C116 0.0191(17) 0.0161(16) 0.0180(18) -0.0014(13) -0.0035(14) -0.0045(14) C115 0.0217(18) 0.0191(17) 0.0235(19) 0.0017(14) -0.0005(15) -0.0003(14) C114 0.030(2) 0.031(2) 0.023(2) 0.0024(16) 0.0015(16) -0.0083(17) C113 0.031(2) 0.029(2) 0.026(2) 0.0074(16) -0.0020(17) -0.0080(17) C112 0.032(2) 0.027(2) 0.033(2) 0.0068(17) -0.0069(18) -0.0001(17) C111 0.0242(19) 0.0258(19) 0.026(2) 0.0018(15) 0.0013(16) 0.0022(15) C121 0.0196(17) 0.0213(18) 0.0179(18) 0.0009(14) 0.0013(14) 0.0032(14) C122 0.0214(18) 0.0209(18) 0.0235(19) -0.0018(15) 0.0013(15) 0.0025(14) C123 0.036(2) 0.0179(18) 0.029(2) 0.0032(15) 0.0044(17) 0.0022(16) C124 0.066(3) 0.032(2) 0.022(2) 0.0086(17) 0.001(2) 0.019(2) C125 0.081(3) 0.032(2) 0.019(2) -0.0036(17) -0.018(2) 0.013(2) C126 0.047(2) 0.0231(19) 0.022(2) -0.0023(15) -0.0120(18) 0.0061(17) N1 0.0184(15) 0.0251(15) 0.0181(15) 0.0030(12) 0.0011(12) 0.0007(12) N2 0.0182(15) 0.0201(15) 0.0158(15) -0.0005(11) -0.0002(12) 0.0001(12) N3 0.0163(14) 0.0151(14) 0.0191(15) -0.0008(11) -0.0041(12) 0.0036(11) N4 0.0158(14) 0.0157(14) 0.0169(15) 0.0002(11) -0.0015(11) 0.0040(11) N5 0.0131(14) 0.0205(15) 0.0248(16) -0.0025(12) -0.0029(12) -0.0002(11) N6 0.0155(14) 0.0196(15) 0.0200(15) 0.0017(12) -0.0010(12) 0.0015(11) N7 0.0192(14) 0.0145(13) 0.0130(14) 0.0019(11) -0.0011(12) -0.0009(11) N8 0.0175(14) 0.0137(14) 0.0225(16) -0.0006(11) -0.0032(12) -0.0019(11) N9 0.0204(14) 0.0189(14) 0.0158(15) -0.0036(11) -0.0036(12) -0.0009(12) N10 0.0175(14) 0.0167(14) 0.0156(15) -0.0012(11) -0.0035(12) 0.0002(11) N11 0.0149(14) 0.0175(14) 0.0177(15) 0.0033(11) -0.0010(12) 0.0004(11) N12 0.0206(14) 0.0163(14) 0.0139(14) 0.0036(11) -0.0032(12) 0.0015(11) O1 0.0184(12) 0.0253(13) 0.0234(13) 0.0017(10) -0.0004(10) 0.0032(10) O6 0.0243(13) 0.0192(12) 0.0162(12) -0.0012(10) -0.0022(10) 0.0047(10) O2 0.0182(12) 0.0156(12) 0.0238(13) -0.0044(9) 0.0015(10) -0.0014(9) O3 0.0167(12) 0.0218(12) 0.0247(13) -0.0059(10) -0.0019(10) 0.0020(10) O4 0.0184(12) 0.0195(12) 0.0219(13) 0.0033(10) -0.0062(10) -0.0020(10) O5 0.0249(13) 0.0191(12) 0.0182(13) 0.0001(10) -0.0010(10) -0.0079(10) _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 Zn1 O6 1.997(2) . ? Zn1 O1 2.004(2) . ? Zn1 N2 2.066(3) . ? Zn1 N4 2.113(3) . ? Zn1 N11 2.120(3) . ? Zn2 O2 1.963(2) . ? Zn2 O3 2.030(2) . ? Zn2 N6 2.052(3) . ? Zn2 N8 2.097(3) . ? Zn2 N3 2.187(3) . ? Zn3 O4 1.972(2) . ? Zn3 O5 2.000(2) . ? Zn3 N12 2.061(3) . ? Zn3 N10 2.066(3) . ? Zn3 N7 2.168(3) . ? C1 O1 1.277(4) . ? C1 N1 1.315(4) . ? C1 C13 1.477(5) . ? C2 N2 1.281(4) . ? C2 C21 1.485(5) . ? C2 C3 1.486(5) . ? C3 N3 1.289(4) . ? C3 C31 1.474(4) . ? C4 O2 1.261(4) . ? C4 N4 1.330(4) . ? C4 C41 1.481(4) . ? C5 O3 1.272(4) . ? C5 N5 1.325(4) . ? C5 C51 1.479(4) . ? C6 N6 1.291(4) . ? C6 C61 1.472(4) . ? C6 C7 1.491(4) . ? C7 N7 1.293(4) . ? C7 C71 1.475(4) . ? C8 O4 1.259(4) . ? C8 N8 1.334(4) . ? C8 C81 1.476(4) . ? C9 O5 1.271(4) . ? C9 N9 1.327(4) . ? C9 C91 1.472(4) . ? C10 N10 1.291(4) . ? C10 C11 1.473(5) . ? C10 C101 1.479(4) . ? C11 N11 1.288(4) . ? C11 C116 1.485(4) . ? C12 O6 1.252(4) . ? C12 N12 1.342(4) . ? C12 C121 1.476(4) . ? C13 C18 1.384(5) . ? C13 C14 1.387(5) . ? C14 C15 1.377(5) . ? C14 H14 0.9500 . ? C15 C16 1.357(6) . ? C15 H15 0.9500 . ? C16 C17 1.383(6) . ? C16 H16 0.9500 . ? C17 C18 1.375(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C21 C26 1.376(5) . ? C21 C22 1.380(5) . ? C22 C23 1.379(5) . ? C22 H22 0.9500 . ? C23 C24 1.379(6) . ? C23 H23 0.9500 . ? C24 C25 1.360(6) . ? C24 H24 0.9500 . ? C25 C26 1.391(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C36 1.378(5) . ? C31 C32 1.389(5) . ? C32 C33 1.380(5) . ? C32 H32 0.9500 . ? C33 C34 1.369(5) . ? C33 H33 0.9500 . ? C34 C35 1.377(5) . ? C34 H34 0.9500 . ? C35 C36 1.371(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.383(5) . ? C41 C46 1.385(5) . ? C42 C43 1.374(5) . ? C42 H42 0.9500 . ? C43 C44 1.369(5) . ? C43 H43 0.9500 . ? C44 C45 1.380(5) . ? C44 H44 0.9500 . ? C45 C46 1.385(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C56 1.377(5) . ? C51 C52 1.378(5) . ? C52 C53 1.380(5) . ? C52 H52 0.9500 . ? C53 C54 1.370(5) . ? C53 H53 0.9500 . ? C54 C55 1.375(6) . ? C54 H54 0.9500 . ? C55 C56 1.375(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C62 1.388(5) . ? C61 C66 1.389(5) . ? C62 C63 1.376(5) . ? C62 H62 0.9500 . ? C63 C64 1.366(5) . ? C63 H63 0.9500 . ? C64 C65 1.379(5) . ? C64 H64 0.9500 . ? C65 C66 1.377(5) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C72 1.383(5) . ? C71 C76 1.383(5) . ? C72 C73 1.374(5) . ? C72 H72 0.9500 . ? C73 C74 1.375(5) . ? C73 H73 0.9500 . ? C74 C75 1.373(5) . ? C74 H74 0.9500 . ? C75 C76 1.380(5) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C86 1.389(5) . ? C81 C82 1.392(5) . ? C82 C83 1.376(5) . ? C82 H82 0.9500 . ? C83 C84 1.368(5) . ? C83 H83 0.9500 . ? C84 C85 1.383(5) . ? C84 H84 0.9500 . ? C85 C86 1.374(5) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C91 C92 1.379(5) . ? C91 C96 1.392(5) . ? C92 C93 1.367(5) . ? C92 H92 0.9500 . ? C93 C94 1.374(5) . ? C93 H93 0.9500 . ? C94 C95 1.368(5) . ? C94 H94 0.9500 . ? C95 C96 1.378(5) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C101 C102 1.381(5) . ? C101 C106 1.383(5) . ? C102 C103 1.372(5) . ? C102 H102 0.9500 . ? C103 C104 1.369(6) . ? C103 H103 0.9500 . ? C104 C105 1.371(6) . ? C104 H104 0.9500 . ? C105 C106 1.379(5) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C116 C111 1.375(5) . ? C116 C115 1.377(5) . ? C115 C114 1.378(5) . ? C115 H116 0.9500 . ? C114 C113 1.364(5) . ? C114 H115 0.9500 . ? C113 C112 1.369(5) . ? C113 H114 0.9500 . ? C112 C111 1.380(5) . ? C112 H113 0.9500 . ? C111 H112 0.9500 . ? C121 C126 1.371(5) . ? C121 C122 1.381(5) . ? C122 C123 1.369(5) . ? C122 H122 0.9500 . ? C123 C124 1.373(5) . ? C123 H123 0.9500 . ? C124 C125 1.367(6) . ? C124 H124 0.9500 . ? C125 C126 1.368(5) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? N1 N2 1.361(4) . ? N3 N4 1.409(3) . ? N5 N6 1.367(4) . ? N7 N8 1.402(3) . ? N9 N10 1.361(4) . ? N11 N12 1.403(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 O6 Zn1 O1 94.81(9) . . ? O6 Zn1 N2 165.92(10) . . ? O1 Zn1 N2 77.55(10) . . ? O6 Zn1 N4 96.61(10) . . ? O1 Zn1 N4 137.56(10) . . ? N2 Zn1 N4 81.82(10) . . ? O6 Zn1 N11 76.56(9) . . ? O1 Zn1 N11 115.15(10) . . ? N2 Zn1 N11 117.34(10) . . ? N4 Zn1 N11 107.25(10) . . ? O2 Zn2 O3 90.91(9) . . ? O2 Zn2 N6 164.76(10) . . ? O3 Zn2 N6 77.21(10) . . ? O2 Zn2 N8 100.90(10) . . ? O3 Zn2 N8 130.63(10) . . ? N6 Zn2 N8 80.39(10) . . ? O2 Zn2 N3 74.89(9) . . ? O3 Zn2 N3 121.67(9) . . ? N6 Zn2 N3 119.44(10) . . ? N8 Zn2 N3 107.68(10) . . ? O4 Zn3 O5 91.71(9) . . ? O4 Zn3 N12 101.09(10) . . ? O5 Zn3 N12 135.77(10) . . ? O4 Zn3 N10 165.66(10) . . ? O5 Zn3 N10 77.16(10) . . ? N12 Zn3 N10 81.41(10) . . ? O4 Zn3 N7 76.51(9) . . ? O5 Zn3 N7 116.72(10) . . ? N12 Zn3 N7 107.43(10) . . ? N10 Zn3 N7 116.46(10) . . ? O1 C1 N1 126.1(3) . . ? O1 C1 C13 118.4(3) . . ? N1 C1 C13 115.5(3) . . ? N2 C2 C21 123.3(3) . . ? N2 C2 C3 117.6(3) . . ? C21 C2 C3 119.1(3) . . ? N3 C3 C31 118.0(3) . . ? N3 C3 C2 126.3(3) . . ? C31 C3 C2 115.6(3) . . ? O2 C4 N4 124.1(3) . . ? O2 C4 C41 115.7(3) . . ? N4 C4 C41 120.2(3) . . ? O3 C5 N5 125.6(3) . . ? O3 C5 C51 119.0(3) . . ? N5 C5 C51 115.3(3) . . ? N6 C6 C61 124.0(3) . . ? N6 C6 C7 117.2(3) . . ? C61 C6 C7 118.8(3) . . ? N7 C7 C71 118.1(3) . . ? N7 C7 C6 125.6(3) . . ? C71 C7 C6 116.3(3) . . ? O4 C8 N8 123.8(3) . . ? O4 C8 C81 118.1(3) . . ? N8 C8 C81 118.1(3) . . ? O5 C9 N9 125.3(3) . . ? O5 C9 C91 117.9(3) . . ? N9 C9 C91 116.8(3) . . ? N10 C10 C11 117.8(3) . . ? N10 C10 C101 121.4(3) . . ? C11 C10 C101 120.6(3) . . ? N11 C11 C10 126.7(3) . . ? N11 C11 C116 114.3(3) . . ? C10 C11 C116 118.6(3) . . ? O6 C12 N12 124.9(3) . . ? O6 C12 C121 118.4(3) . . ? N12 C12 C121 116.6(3) . . ? C18 C13 C14 119.1(3) . . ? C18 C13 C1 121.7(3) . . ? C14 C13 C1 119.2(3) . . ? C15 C14 C13 119.9(4) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 121.0(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.5(4) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 120.4(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C13 120.0(4) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C26 C21 C22 119.5(3) . . ? C26 C21 C2 119.5(3) . . ? C22 C21 C2 120.9(3) . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.1(4) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.1(4) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C36 C31 C32 118.9(3) . . ? C36 C31 C3 121.9(3) . . ? C32 C31 C3 119.2(3) . . ? C33 C32 C31 119.9(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.6(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.6(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 120.2(3) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C31 120.8(3) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C42 C41 C46 119.5(3) . . ? C42 C41 C4 117.3(3) . . ? C46 C41 C4 123.1(3) . . ? C43 C42 C41 120.8(3) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 119.6(3) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C45 120.4(3) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C46 120.2(3) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 119.5(3) . . ? C45 C46 H46 120.3 . . ? C41 C46 H46 120.3 . . ? C56 C51 C52 118.6(3) . . ? C56 C51 C5 122.0(3) . . ? C52 C51 C5 119.4(3) . . ? C51 C52 C53 120.6(3) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C54 C53 C52 120.5(4) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C53 C54 C55 119.0(4) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? C56 C55 C54 120.7(4) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C55 C56 C51 120.6(4) . . ? C55 C56 H56 119.7 . . ? C51 C56 H56 119.7 . . ? C62 C61 C66 118.6(3) . . ? C62 C61 C6 121.5(3) . . ? C66 C61 C6 119.9(3) . . ? C63 C62 C61 120.6(3) . . ? C63 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C64 C63 C62 120.2(4) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C63 C64 C65 120.3(3) . . ? C63 C64 H64 119.9 . . ? C65 C64 H64 119.9 . . ? C66 C65 C64 119.8(4) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C61 120.6(3) . . ? C65 C66 H66 119.7 . . ? C61 C66 H66 119.7 . . ? C72 C71 C76 119.5(3) . . ? C72 C71 C7 118.9(3) . . ? C76 C71 C7 121.6(3) . . ? C73 C72 C71 119.9(3) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C72 C73 C74 120.3(3) . . ? C72 C73 H73 119.8 . . ? C74 C73 H73 119.8 . . ? C75 C74 C73 120.3(3) . . ? C75 C74 H74 119.9 . . ? C73 C74 H74 119.9 . . ? C74 C75 C76 119.7(3) . . ? C74 C75 H75 120.2 . . ? C76 C75 H75 120.2 . . ? C75 C76 C71 120.3(3) . . ? C75 C76 H76 119.9 . . ? C71 C76 H76 119.9 . . ? C86 C81 C82 119.4(3) . . ? C86 C81 C8 123.2(3) . . ? C82 C81 C8 117.4(3) . . ? C83 C82 C81 120.0(3) . . ? C83 C82 H82 120.0 . . ? C81 C82 H82 120.0 . . ? C84 C83 C82 120.2(3) . . ? C84 C83 H83 119.9 . . ? C82 C83 H83 119.9 . . ? C83 C84 C85 120.3(3) . . ? C83 C84 H84 119.9 . . ? C85 C84 H84 119.9 . . ? C86 C85 C84 120.2(3) . . ? C86 C85 H85 119.9 . . ? C84 C85 H85 119.9 . . ? C85 C86 C81 119.8(3) . . ? C85 C86 H86 120.1 . . ? C81 C86 H86 120.1 . . ? C92 C91 C96 119.1(3) . . ? C92 C91 C9 119.8(3) . . ? C96 C91 C9 121.1(3) . . ? C93 C92 C91 120.3(3) . . ? C93 C92 H92 119.9 . . ? C91 C92 H92 119.9 . . ? C92 C93 C94 120.7(3) . . ? C92 C93 H93 119.6 . . ? C94 C93 H93 119.6 . . ? C95 C94 C93 119.6(3) . . ? C95 C94 H94 120.2 . . ? C93 C94 H94 120.2 . . ? C94 C95 C96 120.5(3) . . ? C94 C95 H95 119.7 . . ? C96 C95 H95 119.7 . . ? C95 C96 C91 119.8(3) . . ? C95 C96 H96 120.1 . . ? C91 C96 H96 120.1 . . ? C102 C101 C106 118.6(3) . . ? C102 C101 C10 118.9(3) . . ? C106 C101 C10 122.5(3) . . ? C103 C102 C101 121.0(3) . . ? C103 C102 H102 119.5 . . ? C101 C102 H102 119.5 . . ? C104 C103 C102 119.7(4) . . ? C104 C103 H103 120.1 . . ? C102 C103 H103 120.1 . . ? C103 C104 C105 120.4(4) . . ? C103 C104 H104 119.8 . . ? C105 C104 H104 119.8 . . ? C104 C105 C106 119.9(4) . . ? C104 C105 H105 120.1 . . ? C106 C105 H105 120.1 . . ? C105 C106 C101 120.4(4) . . ? C105 C106 H106 119.8 . . ? C101 C106 H106 119.8 . . ? C111 C116 C115 119.3(3) . . ? C111 C116 C11 121.5(3) . . ? C115 C116 C11 119.2(3) . . ? C116 C115 C114 120.4(3) . . ? C116 C115 H116 119.8 . . ? C114 C115 H116 119.8 . . ? C113 C114 C115 120.2(3) . . ? C113 C114 H115 119.9 . . ? C115 C114 H115 119.9 . . ? C114 C113 C112 119.7(3) . . ? C114 C113 H114 120.2 . . ? C112 C113 H114 120.2 . . ? C113 C112 C111 120.6(3) . . ? C113 C112 H113 119.7 . . ? C111 C112 H113 119.7 . . ? C116 C111 C112 119.8(3) . . ? C116 C111 H112 120.1 . . ? C112 C111 H112 120.1 . . ? C126 C121 C122 119.5(3) . . ? C126 C121 C12 122.2(3) . . ? C122 C121 C12 118.1(3) . . ? C123 C122 C121 120.3(3) . . ? C123 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? C122 C123 C124 119.6(3) . . ? C122 C123 H123 120.2 . . ? C124 C123 H123 120.2 . . ? C125 C124 C123 120.1(4) . . ? C125 C124 H124 119.9 . . ? C123 C124 H124 119.9 . . ? C124 C125 C126 120.4(4) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C125 C126 C121 120.0(4) . . ? C125 C126 H126 120.0 . . ? C121 C126 H126 120.0 . . ? C1 N1 N2 110.1(3) . . ? C2 N2 N1 118.3(3) . . ? C2 N2 Zn1 126.7(2) . . ? N1 N2 Zn1 114.40(19) . . ? C3 N3 N4 118.0(3) . . ? C3 N3 Zn2 133.9(2) . . ? N4 N3 Zn2 107.66(18) . . ? C4 N4 N3 109.8(2) . . ? C4 N4 Zn1 131.5(2) . . ? N3 N4 Zn1 112.81(18) . . ? C5 N5 N6 110.0(3) . . ? C6 N6 N5 119.1(3) . . ? C6 N6 Zn2 125.4(2) . . ? N5 N6 Zn2 115.3(2) . . ? C7 N7 N8 118.5(3) . . ? C7 N7 Zn3 134.4(2) . . ? N8 N7 Zn3 106.78(17) . . ? C8 N8 N7 111.8(2) . . ? C8 N8 Zn2 130.5(2) . . ? N7 N8 Zn2 111.28(18) . . ? C9 N9 N10 109.9(3) . . ? C10 N10 N9 118.4(3) . . ? C10 N10 Zn3 126.7(2) . . ? N9 N10 Zn3 114.83(19) . . ? C11 N11 N12 118.9(3) . . ? C11 N11 Zn1 131.7(2) . . ? N12 N11 Zn1 109.03(18) . . ? C12 N12 N11 109.7(3) . . ? C12 N12 Zn3 130.9(2) . . ? N11 N12 Zn3 114.28(18) . . ? C1 O1 Zn1 111.7(2) . . ? C12 O6 Zn1 112.3(2) . . ? C4 O2 Zn2 114.03(19) . . ? C5 O3 Zn2 111.8(2) . . ? C8 O4 Zn3 113.1(2) . . ? C9 O5 Zn3 112.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 N3 39.5(5) . . . . ? C21 C2 C3 N3 -139.4(3) . . . . ? N2 C2 C3 C31 -142.2(3) . . . . ? C21 C2 C3 C31 38.9(4) . . . . ? N6 C6 C7 N7 36.3(5) . . . . ? C61 C6 C7 N7 -140.7(3) . . . . ? N6 C6 C7 C71 -145.2(3) . . . . ? C61 C6 C7 C71 37.8(4) . . . . ? N10 C10 C11 N11 31.7(5) . . . . ? C101 C10 C11 N11 -143.9(3) . . . . ? N10 C10 C11 C116 -156.0(3) . . . . ? C101 C10 C11 C116 28.5(4) . . . . ? O1 C1 C13 C18 -167.4(3) . . . . ? N1 C1 C13 C18 14.2(5) . . . . ? O1 C1 C13 C14 15.0(5) . . . . ? N1 C1 C13 C14 -163.3(3) . . . . ? C18 C13 C14 C15 -1.2(5) . . . . ? C1 C13 C14 C15 176.4(3) . . . . ? C13 C14 C15 C16 0.7(6) . . . . ? C14 C15 C16 C17 0.7(6) . . . . ? C15 C16 C17 C18 -1.6(6) . . . . ? C16 C17 C18 C13 1.1(5) . . . . ? C14 C13 C18 C17 0.3(5) . . . . ? C1 C13 C18 C17 -177.2(3) . . . . ? N2 C2 C21 C26 -123.5(4) . . . . ? C3 C2 C21 C26 55.3(5) . . . . ? N2 C2 C21 C22 52.2(5) . . . . ? C3 C2 C21 C22 -129.0(4) . . . . ? C26 C21 C22 C23 -0.1(6) . . . . ? C2 C21 C22 C23 -175.8(4) . . . . ? C21 C22 C23 C24 1.5(7) . . . . ? C22 C23 C24 C25 -1.5(8) . . . . ? C23 C24 C25 C26 0.1(8) . . . . ? C22 C21 C26 C25 -1.3(6) . . . . ? C2 C21 C26 C25 174.4(4) . . . . ? C24 C25 C26 C21 1.3(7) . . . . ? N3 C3 C31 C36 39.8(5) . . . . ? C2 C3 C31 C36 -138.6(3) . . . . ? N3 C3 C31 C32 -140.5(3) . . . . ? C2 C3 C31 C32 41.1(4) . . . . ? C36 C31 C32 C33 -2.5(5) . . . . ? C3 C31 C32 C33 177.8(3) . . . . ? C31 C32 C33 C34 0.5(5) . . . . ? C32 C33 C34 C35 1.2(5) . . . . ? C33 C34 C35 C36 -0.7(5) . . . . ? C34 C35 C36 C31 -1.4(5) . . . . ? C32 C31 C36 C35 3.0(5) . . . . ? C3 C31 C36 C35 -177.4(3) . . . . ? O2 C4 C41 C42 23.7(4) . . . . ? N4 C4 C41 C42 -158.5(3) . . . . ? O2 C4 C41 C46 -153.2(3) . . . . ? N4 C4 C41 C46 24.6(5) . . . . ? C46 C41 C42 C43 0.1(5) . . . . ? C4 C41 C42 C43 -176.9(3) . . . . ? C41 C42 C43 C44 0.4(5) . . . . ? C42 C43 C44 C45 -0.4(5) . . . . ? C43 C44 C45 C46 -0.2(6) . . . . ? C44 C45 C46 C41 0.7(5) . . . . ? C42 C41 C46 C45 -0.6(5) . . . . ? C4 C41 C46 C45 176.2(3) . . . . ? O3 C5 C51 C56 -164.4(3) . . . . ? N5 C5 C51 C56 16.0(5) . . . . ? O3 C5 C51 C52 15.1(5) . . . . ? N5 C5 C51 C52 -164.5(3) . . . . ? C56 C51 C52 C53 -0.3(5) . . . . ? C5 C51 C52 C53 -179.9(3) . . . . ? C51 C52 C53 C54 1.6(6) . . . . ? C52 C53 C54 C55 -1.8(6) . . . . ? C53 C54 C55 C56 0.6(6) . . . . ? C54 C55 C56 C51 0.7(6) . . . . ? C52 C51 C56 C55 -0.8(6) . . . . ? C5 C51 C56 C55 178.7(4) . . . . ? N6 C6 C61 C62 38.2(5) . . . . ? C7 C6 C61 C62 -144.9(3) . . . . ? N6 C6 C61 C66 -140.7(3) . . . . ? C7 C6 C61 C66 36.1(4) . . . . ? C66 C61 C62 C63 1.0(5) . . . . ? C6 C61 C62 C63 -177.9(3) . . . . ? C61 C62 C63 C64 0.4(5) . . . . ? C62 C63 C64 C65 -0.9(5) . . . . ? C63 C64 C65 C66 0.1(6) . . . . ? C64 C65 C66 C61 1.4(5) . . . . ? C62 C61 C66 C65 -1.9(5) . . . . ? C6 C61 C66 C65 177.1(3) . . . . ? N7 C7 C71 C72 -133.5(3) . . . . ? C6 C7 C71 C72 47.9(4) . . . . ? N7 C7 C71 C76 48.3(4) . . . . ? C6 C7 C71 C76 -130.3(3) . . . . ? C76 C71 C72 C73 -2.7(5) . . . . ? C7 C71 C72 C73 179.1(3) . . . . ? C71 C72 C73 C74 0.4(5) . . . . ? C72 C73 C74 C75 1.1(6) . . . . ? C73 C74 C75 C76 -0.3(6) . . . . ? C74 C75 C76 C71 -2.0(5) . . . . ? C72 C71 C76 C75 3.5(5) . . . . ? C7 C71 C76 C75 -178.3(3) . . . . ? O4 C8 C81 C86 -163.6(3) . . . . ? N8 C8 C81 C86 15.2(5) . . . . ? O4 C8 C81 C82 15.5(4) . . . . ? N8 C8 C81 C82 -165.8(3) . . . . ? C86 C81 C82 C83 -2.3(5) . . . . ? C8 C81 C82 C83 178.6(3) . . . . ? C81 C82 C83 C84 0.0(5) . . . . ? C82 C83 C84 C85 1.9(6) . . . . ? C83 C84 C85 C86 -1.5(6) . . . . ? C84 C85 C86 C81 -0.8(5) . . . . ? C82 C81 C86 C85 2.7(5) . . . . ? C8 C81 C86 C85 -178.3(3) . . . . ? O5 C9 C91 C92 -4.7(4) . . . . ? N9 C9 C91 C92 176.0(3) . . . . ? O5 C9 C91 C96 176.3(3) . . . . ? N9 C9 C91 C96 -3.0(5) . . . . ? C96 C91 C92 C93 -0.4(5) . . . . ? C9 C91 C92 C93 -179.4(3) . . . . ? C91 C92 C93 C94 1.1(5) . . . . ? C92 C93 C94 C95 -0.9(5) . . . . ? C93 C94 C95 C96 0.1(6) . . . . ? C94 C95 C96 C91 0.6(6) . . . . ? C92 C91 C96 C95 -0.5(5) . . . . ? C9 C91 C96 C95 178.5(3) . . . . ? N10 C10 C101 C102 -63.2(4) . . . . ? C11 C10 C101 C102 112.2(4) . . . . ? N10 C10 C101 C106 114.4(4) . . . . ? C11 C10 C101 C106 -70.2(4) . . . . ? C106 C101 C102 C103 -0.3(5) . . . . ? C10 C101 C102 C103 177.4(3) . . . . ? C101 C102 C103 C104 -0.3(5) . . . . ? C102 C103 C104 C105 0.8(6) . . . . ? C103 C104 C105 C106 -0.7(6) . . . . ? C104 C105 C106 C101 0.1(5) . . . . ? C102 C101 C106 C105 0.4(5) . . . . ? C10 C101 C106 C105 -177.2(3) . . . . ? N11 C11 C116 C111 -109.8(4) . . . . ? C10 C11 C116 C111 77.0(4) . . . . ? N11 C11 C116 C115 70.4(4) . . . . ? C10 C11 C116 C115 -102.9(4) . . . . ? C111 C116 C115 C114 -0.3(5) . . . . ? C11 C116 C115 C114 179.6(3) . . . . ? C116 C115 C114 C113 0.1(5) . . . . ? C115 C114 C113 C112 1.1(5) . . . . ? C114 C113 C112 C111 -2.0(6) . . . . ? C115 C116 C111 C112 -0.7(5) . . . . ? C11 C116 C111 C112 179.5(3) . . . . ? C113 C112 C111 C116 1.8(6) . . . . ? O6 C12 C121 C126 -144.3(3) . . . . ? N12 C12 C121 C126 32.2(5) . . . . ? O6 C12 C121 C122 29.8(4) . . . . ? N12 C12 C121 C122 -153.7(3) . . . . ? C126 C121 C122 C123 -2.2(5) . . . . ? C12 C121 C122 C123 -176.5(3) . . . . ? C121 C122 C123 C124 3.2(5) . . . . ? C122 C123 C124 C125 -1.8(6) . . . . ? C123 C124 C125 C126 -0.7(7) . . . . ? C124 C125 C126 C121 1.8(7) . . . . ? C122 C121 C126 C125 -0.4(6) . . . . ? C12 C121 C126 C125 173.7(4) . . . . ? O1 C1 N1 N2 -4.5(5) . . . . ? C13 C1 N1 N2 173.7(3) . . . . ? C21 C2 N2 N1 -2.5(5) . . . . ? C3 C2 N2 N1 178.6(3) . . . . ? C21 C2 N2 Zn1 167.4(2) . . . . ? C3 C2 N2 Zn1 -11.4(4) . . . . ? C1 N1 N2 C2 172.8(3) . . . . ? C1 N1 N2 Zn1 1.7(3) . . . . ? O6 Zn1 N2 C2 -111.7(4) . . . . ? O1 Zn1 N2 C2 -169.8(3) . . . . ? N4 Zn1 N2 C2 -27.1(3) . . . . ? N11 Zn1 N2 C2 78.1(3) . . . . ? O6 Zn1 N2 N1 58.6(5) . . . . ? O1 Zn1 N2 N1 0.4(2) . . . . ? N4 Zn1 N2 N1 143.1(2) . . . . ? N11 Zn1 N2 N1 -111.6(2) . . . . ? C31 C3 N3 N4 179.9(3) . . . . ? C2 C3 N3 N4 -1.9(5) . . . . ? C31 C3 N3 Zn2 -9.1(5) . . . . ? C2 C3 N3 Zn2 169.2(2) . . . . ? O2 Zn2 N3 C3 -145.9(3) . . . . ? O3 Zn2 N3 C3 -64.3(3) . . . . ? N6 Zn2 N3 C3 28.5(3) . . . . ? N8 Zn2 N3 C3 117.3(3) . . . . ? O2 Zn2 N3 N4 25.87(17) . . . . ? O3 Zn2 N3 N4 107.40(18) . . . . ? N6 Zn2 N3 N4 -159.77(17) . . . . ? N8 Zn2 N3 N4 -70.99(19) . . . . ? O2 C4 N4 N3 2.8(4) . . . . ? C41 C4 N4 N3 -174.9(3) . . . . ? O2 C4 N4 Zn1 -147.4(3) . . . . ? C41 C4 N4 Zn1 34.9(4) . . . . ? C3 N3 N4 C4 150.6(3) . . . . ? Zn2 N3 N4 C4 -22.7(3) . . . . ? C3 N3 N4 Zn1 -53.3(3) . . . . ? Zn2 N3 N4 Zn1 133.49(13) . . . . ? O6 Zn1 N4 C4 13.0(3) . . . . ? O1 Zn1 N4 C4 -91.5(3) . . . . ? N2 Zn1 N4 C4 -152.8(3) . . . . ? N11 Zn1 N4 C4 91.0(3) . . . . ? O6 Zn1 N4 N3 -136.43(19) . . . . ? O1 Zn1 N4 N3 118.99(19) . . . . ? N2 Zn1 N4 N3 57.68(19) . . . . ? N11 Zn1 N4 N3 -58.5(2) . . . . ? O3 C5 N5 N6 2.2(4) . . . . ? C51 C5 N5 N6 -178.3(3) . . . . ? C61 C6 N6 N5 3.5(5) . . . . ? C7 C6 N6 N5 -173.4(3) . . . . ? C61 C6 N6 Zn2 178.1(2) . . . . ? C7 C6 N6 Zn2 1.3(4) . . . . ? C5 N5 N6 C6 174.5(3) . . . . ? C5 N5 N6 Zn2 -0.6(3) . . . . ? O2 Zn2 N6 C6 -135.7(4) . . . . ? O3 Zn2 N6 C6 -175.2(3) . . . . ? N8 Zn2 N6 C6 -39.5(3) . . . . ? N3 Zn2 N6 C6 65.4(3) . . . . ? O2 Zn2 N6 N5 39.1(5) . . . . ? O3 Zn2 N6 N5 -0.4(2) . . . . ? N8 Zn2 N6 N5 135.3(2) . . . . ? N3 Zn2 N6 N5 -119.8(2) . . . . ? C71 C7 N7 N8 175.6(3) . . . . ? C6 C7 N7 N8 -6.0(5) . . . . ? C71 C7 N7 Zn3 -11.8(5) . . . . ? C6 C7 N7 Zn3 166.6(2) . . . . ? O4 Zn3 N7 C7 -149.4(3) . . . . ? O5 Zn3 N7 C7 -64.4(3) . . . . ? N12 Zn3 N7 C7 113.0(3) . . . . ? N10 Zn3 N7 C7 24.0(3) . . . . ? O4 Zn3 N7 N8 23.78(18) . . . . ? O5 Zn3 N7 N8 108.82(18) . . . . ? N12 Zn3 N7 N8 -73.81(19) . . . . ? N10 Zn3 N7 N8 -162.74(17) . . . . ? O4 C8 N8 N7 3.6(4) . . . . ? C81 C8 N8 N7 -175.1(3) . . . . ? O4 C8 N8 Zn2 -145.2(3) . . . . ? C81 C8 N8 Zn2 36.1(4) . . . . ? C7 N7 N8 C8 153.0(3) . . . . ? Zn3 N7 N8 C8 -21.5(3) . . . . ? C7 N7 N8 Zn2 -52.0(3) . . . . ? Zn3 N7 N8 Zn2 133.54(13) . . . . ? O2 Zn2 N8 C8 16.3(3) . . . . ? O3 Zn2 N8 C8 -84.5(3) . . . . ? N6 Zn2 N8 C8 -148.3(3) . . . . ? N3 Zn2 N8 C8 93.7(3) . . . . ? O2 Zn2 N8 N7 -132.67(19) . . . . ? O3 Zn2 N8 N7 126.58(18) . . . . ? N6 Zn2 N8 N7 62.77(19) . . . . ? N3 Zn2 N8 N7 -55.2(2) . . . . ? O5 C9 N9 N10 -1.5(4) . . . . ? C91 C9 N9 N10 177.8(3) . . . . ? C11 C10 N10 N9 -177.9(3) . . . . ? C101 C10 N10 N9 -2.3(4) . . . . ? C11 C10 N10 Zn3 -1.2(4) . . . . ? C101 C10 N10 Zn3 174.3(2) . . . . ? C9 N9 N10 C10 176.0(3) . . . . ? C9 N9 N10 Zn3 -1.0(3) . . . . ? O4 Zn3 N10 C10 -134.9(4) . . . . ? O5 Zn3 N10 C10 -174.8(3) . . . . ? N12 Zn3 N10 C10 -33.7(3) . . . . ? N7 Zn3 N10 C10 71.5(3) . . . . ? O4 Zn3 N10 N9 41.8(5) . . . . ? O5 Zn3 N10 N9 2.0(2) . . . . ? N12 Zn3 N10 N9 143.0(2) . . . . ? N7 Zn3 N10 N9 -111.7(2) . . . . ? C10 C11 N11 N12 -1.7(5) . . . . ? C116 C11 N11 N12 -174.3(3) . . . . ? C10 C11 N11 Zn1 171.5(2) . . . . ? C116 C11 N11 Zn1 -1.1(4) . . . . ? O6 Zn1 N11 C11 -149.7(3) . . . . ? O1 Zn1 N11 C11 -60.6(3) . . . . ? N2 Zn1 N11 C11 27.9(3) . . . . ? N4 Zn1 N11 C11 117.5(3) . . . . ? O6 Zn1 N11 N12 24.04(18) . . . . ? O1 Zn1 N11 N12 113.06(18) . . . . ? N2 Zn1 N11 N12 -158.40(18) . . . . ? N4 Zn1 N11 N12 -68.8(2) . . . . ? O6 C12 N12 N11 7.9(4) . . . . ? C121 C12 N12 N11 -168.3(3) . . . . ? O6 C12 N12 Zn3 -144.5(3) . . . . ? C121 C12 N12 Zn3 39.2(4) . . . . ? C11 N11 N12 C12 150.8(3) . . . . ? Zn1 N11 N12 C12 -23.8(3) . . . . ? C11 N11 N12 Zn3 -51.7(3) . . . . ? Zn1 N11 N12 Zn3 133.65(14) . . . . ? O4 Zn3 N12 C12 15.0(3) . . . . ? O5 Zn3 N12 C12 -89.2(3) . . . . ? N10 Zn3 N12 C12 -150.7(3) . . . . ? N7 Zn3 N12 C12 94.2(3) . . . . ? O4 Zn3 N12 N11 -136.5(2) . . . . ? O5 Zn3 N12 N11 119.3(2) . . . . ? N10 Zn3 N12 N11 57.8(2) . . . . ? N7 Zn3 N12 N11 -57.3(2) . . . . ? N1 C1 O1 Zn1 5.0(4) . . . . ? C13 C1 O1 Zn1 -173.2(2) . . . . ? O6 Zn1 O1 C1 -170.5(2) . . . . ? N2 Zn1 O1 C1 -2.5(2) . . . . ? N4 Zn1 O1 C1 -65.3(3) . . . . ? N11 Zn1 O1 C1 112.1(2) . . . . ? N12 C12 O6 Zn1 13.9(4) . . . . ? C121 C12 O6 Zn1 -169.9(2) . . . . ? O1 Zn1 O6 C12 -135.0(2) . . . . ? N2 Zn1 O6 C12 168.6(4) . . . . ? N4 Zn1 O6 C12 85.9(2) . . . . ? N11 Zn1 O6 C12 -20.3(2) . . . . ? N4 C4 O2 Zn2 22.1(4) . . . . ? C41 C4 O2 Zn2 -160.1(2) . . . . ? O3 Zn2 O2 C4 -148.0(2) . . . . ? N6 Zn2 O2 C4 173.7(3) . . . . ? N8 Zn2 O2 C4 80.3(2) . . . . ? N3 Zn2 O2 C4 -25.3(2) . . . . ? N5 C5 O3 Zn2 -2.6(4) . . . . ? C51 C5 O3 Zn2 177.9(2) . . . . ? O2 Zn2 O3 C5 -168.9(2) . . . . ? N6 Zn2 O3 C5 1.4(2) . . . . ? N8 Zn2 O3 C5 -63.7(2) . . . . ? N3 Zn2 O3 C5 118.3(2) . . . . ? N8 C8 O4 Zn3 19.2(4) . . . . ? C81 C8 O4 Zn3 -162.2(2) . . . . ? O5 Zn3 O4 C8 -140.0(2) . . . . ? N12 Zn3 O4 C8 82.6(2) . . . . ? N10 Zn3 O4 C8 -178.7(4) . . . . ? N7 Zn3 O4 C8 -22.9(2) . . . . ? N9 C9 O5 Zn3 3.2(4) . . . . ? C91 C9 O5 Zn3 -176.1(2) . . . . ? O4 Zn3 O5 C9 -173.4(2) . . . . ? N12 Zn3 O5 C9 -65.6(3) . . . . ? N10 Zn3 O5 C9 -2.6(2) . . . . ? N7 Zn3 O5 C9 110.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.84 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.954 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.198 # Attachment 'Complex_5.cif' data_el23 _database_code_depnum_ccdc_archive 'CCDC 710845' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H60 Cu3 N12 O6' _chemical_formula_sum 'C84 H60 Cu3 N12 O6' _chemical_formula_weight 1524.06 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 15.7016(5) _cell_length_b 18.2981(6) _cell_length_c 25.5157(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.6550(10) _cell_angle_gamma 90.00 _cell_volume 7323.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8832 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 24.02 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3132 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8013 _exptl_absorpt_correction_T_max 0.9130 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 118416 _diffrn_reflns_av_R_equivalents 0.1258 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.04 _reflns_number_total 14433 _reflns_number_gt 9164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0952P)^2^+4.9527P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14433 _refine_ls_number_parameters 946 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1814 _refine_ls_wR_factor_gt 0.1429 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.18019(3) 0.17780(3) 0.17273(2) 0.01408(15) Uani 1 1 d . . . Cu2 Cu -0.08287(4) 0.22086(3) 0.06914(2) 0.01435(15) Uani 1 1 d . . . Cu3 Cu -0.09594(4) 0.17513(3) 0.25363(2) 0.01451(15) Uani 1 1 d . . . N1 N 0.3277(2) 0.2562(2) 0.14825(16) 0.0193(9) Uani 1 1 d . . . N2 N 0.2390(2) 0.2593(2) 0.14254(15) 0.0170(9) Uani 1 1 d . . . N3 N 0.0613(2) 0.2530(2) 0.10134(14) 0.0136(8) Uani 1 1 d . . . N4 N 0.1004(2) 0.1850(2) 0.10895(15) 0.0154(9) Uani 1 1 d . . . N5 N -0.1872(2) 0.3317(2) 0.02489(15) 0.0168(9) Uani 1 1 d . . . N6 N -0.1589(2) 0.3046(2) 0.07296(15) 0.0150(9) Uani 1 1 d . . . N7 N -0.1291(2) 0.2401(2) 0.17770(15) 0.0159(9) Uani 1 1 d . . . N8 N -0.1282(2) 0.1892(2) 0.13634(15) 0.0154(9) Uani 1 1 d . . . N9 N -0.1151(2) 0.2420(2) 0.35206(16) 0.0198(9) Uani 1 1 d . . . N10 N -0.0583(2) 0.2373(2) 0.31189(15) 0.0171(9) Uani 1 1 d . . . N11 N 0.0823(2) 0.2127(2) 0.24170(15) 0.0144(9) Uani 1 1 d . . . N12 N 0.0283(2) 0.1522(2) 0.24508(15) 0.0139(8) Uani 1 1 d . . . O1 O 0.2968(2) 0.15825(18) 0.20206(13) 0.0183(7) Uani 1 1 d . . . O2 O -0.01043(19) 0.13841(17) 0.05673(12) 0.0160(7) Uani 1 1 d . . . O3 O -0.0925(2) 0.24544(17) -0.00535(12) 0.0168(7) Uani 1 1 d . . . O4 O -0.1405(2) 0.10354(17) 0.20252(12) 0.0159(7) Uani 1 1 d . . . O5 O -0.2026(2) 0.17922(18) 0.29181(13) 0.0182(7) Uani 1 1 d . . . O6 O 0.13505(19) 0.09137(17) 0.20382(13) 0.0159(7) Uani 1 1 d . . . C1 C 0.3495(3) 0.2013(3) 0.17998(19) 0.0184(11) Uani 1 1 d . . . C2 C 0.2040(3) 0.3127(3) 0.11497(17) 0.0140(10) Uani 1 1 d . . . C3 C 0.1087(3) 0.3113(3) 0.10599(18) 0.0147(10) Uani 1 1 d . . . C4 C 0.0599(3) 0.1316(3) 0.08247(17) 0.0133(10) Uani 1 1 d . . . C5 C -0.1474(3) 0.2975(3) -0.01292(19) 0.0157(10) Uani 1 1 d . . . C6 C -0.1854(3) 0.3356(3) 0.11502(19) 0.0159(10) Uani 1 1 d . . . C7 C -0.1546(3) 0.3065(3) 0.16659(19) 0.0163(10) Uani 1 1 d . . . C8 C -0.1409(3) 0.1210(3) 0.15442(19) 0.0174(11) Uani 1 1 d . . . C9 C -0.1884(3) 0.2124(3) 0.3355(2) 0.0178(11) Uani 1 1 d . . . C10 C 0.0172(3) 0.2669(3) 0.31944(19) 0.0170(10) Uani 1 1 d . . . C11 C 0.0762(3) 0.2648(3) 0.27578(18) 0.0154(10) Uani 1 1 d . . . C12 C 0.0640(3) 0.0919(3) 0.22619(18) 0.0153(10) Uani 1 1 d . . . C13 C 0.4426(3) 0.1896(3) 0.1899(2) 0.0208(11) Uani 1 1 d . . . C14 C 0.5018(3) 0.2246(3) 0.1595(2) 0.0308(13) Uani 1 1 d . . . H14 H 0.4835 0.2566 0.1330 0.037 Uiso 1 1 calc R . . C15 C 0.5883(4) 0.2117(3) 0.1689(3) 0.0368(15) Uani 1 1 d . . . H15 H 0.6280 0.2349 0.1486 0.044 Uiso 1 1 calc R . . C16 C 0.6156(3) 0.1639(3) 0.2087(2) 0.0329(14) Uani 1 1 d . . . H16 H 0.6735 0.1550 0.2147 0.039 Uiso 1 1 calc R . . C17 C 0.5581(3) 0.1300(3) 0.2389(2) 0.0295(13) Uani 1 1 d . . . H17 H 0.5769 0.0988 0.2658 0.035 Uiso 1 1 calc R . . C18 C 0.4720(3) 0.1420(3) 0.2295(2) 0.0216(11) Uani 1 1 d . . . H18 H 0.4330 0.1180 0.2498 0.026 Uiso 1 1 calc R . . C21 C 0.2535(3) 0.3702(3) 0.09000(19) 0.0162(10) Uani 1 1 d . . . C22 C 0.3255(3) 0.4026(3) 0.1152(2) 0.0191(11) Uani 1 1 d . . . H22 H 0.3418 0.3889 0.1493 0.023 Uiso 1 1 calc R . . C23 C 0.3725(3) 0.4547(3) 0.0897(2) 0.0247(12) Uani 1 1 d . . . H23 H 0.4197 0.4762 0.1070 0.030 Uiso 1 1 calc R . . C24 C 0.3498(3) 0.4750(3) 0.0388(2) 0.0277(13) Uani 1 1 d . . . H24 H 0.3828 0.5087 0.0216 0.033 Uiso 1 1 calc R . . C25 C 0.2782(3) 0.4454(3) 0.0134(2) 0.0252(12) Uani 1 1 d . . . H25 H 0.2623 0.4599 -0.0206 0.030 Uiso 1 1 calc R . . C26 C 0.2299(3) 0.3935(3) 0.03915(19) 0.0206(11) Uani 1 1 d . . . H26 H 0.1813 0.3741 0.0222 0.025 Uiso 1 1 calc R . . C31 C 0.0652(3) 0.3830(3) 0.10056(18) 0.0147(10) Uani 1 1 d . . . C32 C 0.0856(3) 0.4385(3) 0.1365(2) 0.0217(11) Uani 1 1 d . . . H32 H 0.1269 0.4309 0.1632 0.026 Uiso 1 1 calc R . . C33 C 0.0434(3) 0.5058(3) 0.1321(2) 0.0279(13) Uani 1 1 d . . . H33 H 0.0568 0.5428 0.1560 0.033 Uiso 1 1 calc R . . C34 C -0.0175(3) 0.5174(3) 0.0926(2) 0.0320(14) Uani 1 1 d . . . H34 H -0.0460 0.5619 0.0901 0.038 Uiso 1 1 calc R . . C35 C -0.0365(3) 0.4624(3) 0.0562(2) 0.0271(13) Uani 1 1 d . . . H35 H -0.0778 0.4703 0.0295 0.033 Uiso 1 1 calc R . . C36 C 0.0055(3) 0.3961(3) 0.0597(2) 0.0195(11) Uani 1 1 d . . . H36 H -0.0062 0.3601 0.0346 0.023 Uiso 1 1 calc R . . C41 C 0.1016(3) 0.0581(3) 0.08175(18) 0.0171(10) Uani 1 1 d . . . C42 C 0.0519(3) -0.0018(3) 0.06413(18) 0.0170(10) Uani 1 1 d . . . H42 H -0.0045 0.0055 0.0526 0.020 Uiso 1 1 calc R . . C43 C 0.0859(3) -0.0711(3) 0.0638(2) 0.0225(11) Uani 1 1 d . . . H43 H 0.0524 -0.1101 0.0519 0.027 Uiso 1 1 calc R . . C44 C 0.1697(3) -0.0830(3) 0.0810(2) 0.0246(12) Uani 1 1 d . . . H44 H 0.1919 -0.1301 0.0813 0.030 Uiso 1 1 calc R . . C45 C 0.2206(3) -0.0248(3) 0.0978(2) 0.0237(12) Uani 1 1 d . . . H45 H 0.2768 -0.0329 0.1094 0.028 Uiso 1 1 calc R . . C46 C 0.1871(3) 0.0461(3) 0.09719(19) 0.0193(11) Uani 1 1 d . . . H46 H 0.2218 0.0853 0.1071 0.023 Uiso 1 1 calc R . . C51 C -0.1700(3) 0.3195(3) -0.06790(18) 0.0159(10) Uani 1 1 d . . . C52 C -0.1381(3) 0.2804(3) -0.10942(19) 0.0179(11) Uani 1 1 d . . . H52 H -0.1020 0.2409 -0.1026 0.021 Uiso 1 1 calc R . . C53 C -0.1596(3) 0.2997(3) -0.1606(2) 0.0211(11) Uani 1 1 d . . . H53 H -0.1380 0.2732 -0.1881 0.025 Uiso 1 1 calc R . . C54 C -0.2136(3) 0.3590(3) -0.1712(2) 0.0240(12) Uani 1 1 d . . . H54 H -0.2288 0.3718 -0.2057 0.029 Uiso 1 1 calc R . . C55 C -0.2441(4) 0.3982(3) -0.1303(2) 0.0266(12) Uani 1 1 d . . . H55 H -0.2793 0.4383 -0.1372 0.032 Uiso 1 1 calc R . . C56 C -0.2231(3) 0.3790(3) -0.07904(19) 0.0223(11) Uani 1 1 d . . . H56 H -0.2446 0.4059 -0.0517 0.027 Uiso 1 1 calc R . . C61 C -0.2499(3) 0.3949(3) 0.11217(19) 0.0201(11) Uani 1 1 d . . . C62 C -0.3299(3) 0.3799(3) 0.08730(19) 0.0246(12) Uani 1 1 d . . . H62 H -0.3412 0.3336 0.0737 0.030 Uiso 1 1 calc R . . C63 C -0.3921(4) 0.4337(4) 0.0829(2) 0.0370(16) Uani 1 1 d . . . H63 H -0.4449 0.4235 0.0665 0.044 Uiso 1 1 calc R . . C64 C -0.3751(4) 0.5022(4) 0.1028(2) 0.0411(17) Uani 1 1 d . . . H64 H -0.4167 0.5383 0.0996 0.049 Uiso 1 1 calc R . . C65 C -0.2969(4) 0.5183(3) 0.1276(2) 0.0361(15) Uani 1 1 d . . . H65 H -0.2863 0.5648 0.1410 0.043 Uiso 1 1 calc R . . C66 C -0.2347(4) 0.4647(3) 0.1323(2) 0.0281(13) Uani 1 1 d . . . H66 H -0.1823 0.4754 0.1490 0.034 Uiso 1 1 calc R . . C69 C 0.1436(4) 0.3007(4) 0.4456(2) 0.0410(17) Uani 1 1 d . . . H69 H 0.1924 0.2825 0.4631 0.049 Uiso 1 1 calc R . . C71 C -0.1626(3) 0.3529(3) 0.21438(19) 0.0173(10) Uani 1 1 d . . . C72 C -0.2318(3) 0.3422(3) 0.2455(2) 0.0220(11) Uani 1 1 d . . . H72 H -0.2718 0.3064 0.2365 0.026 Uiso 1 1 calc R . . C73 C -0.2416(3) 0.3845(3) 0.2900(2) 0.0254(12) Uani 1 1 d . . . H73 H -0.2881 0.3770 0.3107 0.030 Uiso 1 1 calc R . . C74 C -0.1815(3) 0.4382(3) 0.3037(2) 0.0235(12) Uani 1 1 d . . . H74 H -0.1882 0.4678 0.3328 0.028 Uiso 1 1 calc R . . C75 C -0.1121(3) 0.4468(3) 0.2734(2) 0.0272(13) Uani 1 1 d . . . H75 H -0.0709 0.4814 0.2831 0.033 Uiso 1 1 calc R . . C76 C -0.1018(3) 0.4055(3) 0.2289(2) 0.0235(12) Uani 1 1 d . . . H76 H -0.0547 0.4126 0.2087 0.028 Uiso 1 1 calc R . . C81 C -0.1636(3) 0.0640(3) 0.11511(18) 0.0144(10) Uani 1 1 d . . . C82 C -0.2115(3) 0.0792(3) 0.0692(2) 0.0258(12) Uani 1 1 d . . . H82 H -0.2266 0.1272 0.0611 0.031 Uiso 1 1 calc R . . C83 C -0.2367(4) 0.0232(3) 0.0359(2) 0.0304(13) Uani 1 1 d . . . H83 H -0.2706 0.0334 0.0059 0.036 Uiso 1 1 calc R . . C84 C -0.2121(4) -0.0478(3) 0.0466(2) 0.0267(13) Uani 1 1 d . . . H84 H -0.2278 -0.0850 0.0233 0.032 Uiso 1 1 calc R . . C85 C -0.1638(3) -0.0637(3) 0.0921(2) 0.0222(11) Uani 1 1 d . . . H85 H -0.1469 -0.1115 0.0994 0.027 Uiso 1 1 calc R . . C86 C -0.1412(3) -0.0082(3) 0.1267(2) 0.0184(11) Uani 1 1 d . . . H86 H -0.1108 -0.0190 0.1578 0.022 Uiso 1 1 calc R . . C91 C -0.2595(3) 0.2215(3) 0.3716(2) 0.0205(11) Uani 1 1 d . . . C92 C -0.2456(3) 0.2446(3) 0.4231(2) 0.0263(12) Uani 1 1 d . . . H92 H -0.1904 0.2543 0.4361 0.032 Uiso 1 1 calc R . . C93 C -0.3140(4) 0.2534(3) 0.4555(2) 0.0301(13) Uani 1 1 d . . . H93 H -0.3044 0.2688 0.4900 0.036 Uiso 1 1 calc R . . C94 C -0.3961(4) 0.2390(3) 0.4362(3) 0.0361(15) Uani 1 1 d . . . H94 H -0.4418 0.2449 0.4577 0.043 Uiso 1 1 calc R . . C95 C -0.4102(4) 0.2159(3) 0.3849(3) 0.0368(15) Uani 1 1 d . . . H95 H -0.4655 0.2061 0.3721 0.044 Uiso 1 1 calc R . . C96 C -0.3426(3) 0.2071(3) 0.3523(2) 0.0314(13) Uani 1 1 d . . . H96 H -0.3525 0.1917 0.3178 0.038 Uiso 1 1 calc R . . C101 C 0.0456(3) 0.3006(3) 0.3709(2) 0.0210(11) Uani 1 1 d . . . C102 C 0.1196(3) 0.2744(3) 0.3963(2) 0.0278(13) Uani 1 1 d . . . H102 H 0.1527 0.2395 0.3803 0.033 Uiso 1 1 calc R . . C103 C 0.0960(4) 0.3536(4) 0.4692(3) 0.051(2) Uani 1 1 d . . . H103 H 0.1130 0.3713 0.5022 0.062 Uiso 1 1 calc R . . C104 C 0.0241(4) 0.3799(4) 0.4442(3) 0.0487(19) Uani 1 1 d . . . H104 H -0.0077 0.4158 0.4601 0.058 Uiso 1 1 calc R . . C105 C -0.0023(4) 0.3535(3) 0.3948(2) 0.0316(14) Uani 1 1 d . . . H105 H -0.0518 0.3714 0.3779 0.038 Uiso 1 1 calc R . . C111 C 0.1346(3) 0.3281(3) 0.27130(19) 0.0168(10) Uani 1 1 d . . . C112 C 0.2178(3) 0.3177(3) 0.25687(18) 0.0173(10) Uani 1 1 d . . . H112 H 0.2378 0.2709 0.2506 0.021 Uiso 1 1 calc R . . C113 C 0.2711(3) 0.3777(3) 0.25182(19) 0.0229(12) Uani 1 1 d . . . H113 H 0.3267 0.3705 0.2420 0.027 Uiso 1 1 calc R . . C114 C 0.2426(3) 0.4480(3) 0.2612(2) 0.0253(12) Uani 1 1 d . . . H114 H 0.2784 0.4879 0.2571 0.030 Uiso 1 1 calc R . . C115 C 0.1601(3) 0.4580(3) 0.2768(2) 0.0254(12) Uani 1 1 d . . . H115 H 0.1404 0.5048 0.2835 0.031 Uiso 1 1 calc R . . C116 C 0.1067(3) 0.3987(3) 0.2826(2) 0.0202(11) Uani 1 1 d . . . H116 H 0.0519 0.4059 0.2940 0.024 Uiso 1 1 calc R . . C121 C 0.0245(3) 0.0185(3) 0.23359(19) 0.0158(10) Uani 1 1 d . . . C122 C 0.0489(3) -0.0371(3) 0.19975(19) 0.0166(10) Uani 1 1 d . . . H122 H 0.0869 -0.0272 0.1738 0.020 Uiso 1 1 calc R . . C123 C 0.0160(3) -0.1075(3) 0.2051(2) 0.0203(11) Uani 1 1 d . . . H123 H 0.0316 -0.1443 0.1823 0.024 Uiso 1 1 calc R . . C124 C -0.0396(3) -0.1225(3) 0.2440(2) 0.0229(12) Uani 1 1 d . . . H124 H -0.0612 -0.1695 0.2477 0.027 Uiso 1 1 calc R . . C125 C -0.0630(3) -0.0671(3) 0.2777(2) 0.0241(12) Uani 1 1 d . . . H125 H -0.1003 -0.0772 0.3041 0.029 Uiso 1 1 calc R . . C126 C -0.0314(3) 0.0032(3) 0.27257(19) 0.0199(11) Uani 1 1 d . . . H126 H -0.0477 0.0400 0.2952 0.024 Uiso 1 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 Cu1 0.0134(3) 0.0123(3) 0.0164(3) 0.0021(2) -0.0008(2) -0.0014(2) Cu2 0.0157(3) 0.0128(3) 0.0146(3) 0.0003(2) 0.0007(2) 0.0025(2) Cu3 0.0135(3) 0.0149(3) 0.0151(3) -0.0020(2) 0.0001(2) -0.0015(2) N1 0.013(2) 0.019(2) 0.025(2) 0.0059(19) -0.0023(17) -0.0031(17) N2 0.016(2) 0.016(2) 0.019(2) -0.0013(18) -0.0007(17) -0.0004(17) N3 0.021(2) 0.0088(19) 0.011(2) 0.0000(16) 0.0007(16) 0.0048(17) N4 0.015(2) 0.010(2) 0.020(2) 0.0002(17) -0.0031(17) -0.0018(16) N5 0.019(2) 0.016(2) 0.015(2) 0.0022(18) -0.0008(17) 0.0024(17) N6 0.016(2) 0.014(2) 0.015(2) 0.0030(17) -0.0004(16) -0.0003(16) N7 0.015(2) 0.016(2) 0.017(2) -0.0008(18) 0.0015(16) 0.0014(17) N8 0.018(2) 0.014(2) 0.014(2) -0.0010(17) 0.0020(16) 0.0025(17) N9 0.015(2) 0.022(2) 0.023(2) -0.0014(19) 0.0061(17) -0.0034(18) N10 0.017(2) 0.018(2) 0.017(2) -0.0018(18) 0.0053(17) 0.0015(17) N11 0.0114(19) 0.014(2) 0.018(2) 0.0020(18) 0.0003(16) -0.0008(16) N12 0.013(2) 0.011(2) 0.017(2) -0.0014(17) -0.0015(16) -0.0031(16) O1 0.0179(18) 0.0178(18) 0.0192(18) 0.0033(15) -0.0004(14) -0.0026(14) O2 0.0146(17) 0.0147(17) 0.0186(18) -0.0029(15) -0.0015(14) 0.0007(14) O3 0.0182(17) 0.0144(17) 0.0178(17) 0.0001(14) 0.0010(14) 0.0055(14) O4 0.0207(18) 0.0140(17) 0.0128(17) 0.0020(14) -0.0018(13) -0.0039(14) O5 0.0142(17) 0.0204(18) 0.0200(18) -0.0050(16) 0.0022(14) -0.0035(14) O6 0.0138(17) 0.0122(17) 0.0216(18) 0.0009(14) 0.0020(14) 0.0010(13) C1 0.017(3) 0.016(3) 0.022(3) -0.002(2) -0.003(2) 0.000(2) C2 0.017(2) 0.014(2) 0.011(2) -0.002(2) -0.0016(19) 0.000(2) C3 0.019(2) 0.012(2) 0.012(2) 0.000(2) -0.0012(19) -0.003(2) C4 0.014(2) 0.014(2) 0.012(2) 0.002(2) 0.0057(19) 0.0016(19) C5 0.017(2) 0.011(2) 0.019(3) -0.002(2) 0.001(2) -0.0037(19) C6 0.018(2) 0.013(2) 0.017(2) -0.001(2) 0.002(2) 0.000(2) C7 0.016(2) 0.015(3) 0.019(3) -0.002(2) 0.001(2) 0.0012(19) C8 0.011(2) 0.020(3) 0.021(3) 0.002(2) 0.0029(19) 0.002(2) C9 0.017(3) 0.013(3) 0.024(3) 0.002(2) 0.002(2) 0.001(2) C10 0.015(2) 0.015(3) 0.021(3) -0.001(2) 0.001(2) 0.000(2) C11 0.015(2) 0.015(3) 0.017(2) -0.003(2) -0.0008(19) 0.0020(19) C12 0.015(2) 0.016(3) 0.015(2) 0.006(2) -0.0019(19) 0.001(2) C13 0.013(2) 0.018(3) 0.031(3) 0.000(2) -0.002(2) -0.002(2) C14 0.020(3) 0.032(3) 0.040(3) 0.012(3) -0.004(2) 0.000(2) C15 0.021(3) 0.039(4) 0.051(4) 0.005(3) 0.006(3) -0.006(3) C16 0.017(3) 0.035(3) 0.046(4) -0.009(3) -0.006(3) 0.005(2) C17 0.024(3) 0.025(3) 0.038(3) -0.001(3) -0.012(3) 0.005(2) C18 0.023(3) 0.017(3) 0.025(3) -0.002(2) -0.003(2) -0.001(2) C21 0.017(2) 0.011(2) 0.021(3) -0.002(2) 0.007(2) 0.0025(19) C22 0.020(3) 0.017(3) 0.021(3) 0.002(2) 0.000(2) 0.002(2) C23 0.021(3) 0.020(3) 0.034(3) 0.000(2) 0.006(2) -0.001(2) C24 0.027(3) 0.020(3) 0.037(3) 0.003(3) 0.018(3) 0.001(2) C25 0.029(3) 0.023(3) 0.024(3) 0.007(2) 0.008(2) 0.006(2) C26 0.022(3) 0.023(3) 0.017(3) -0.001(2) 0.000(2) 0.001(2) C31 0.014(2) 0.014(2) 0.017(2) 0.003(2) 0.0057(19) -0.0010(19) C32 0.022(3) 0.018(3) 0.025(3) 0.003(2) 0.004(2) 0.003(2) C33 0.028(3) 0.017(3) 0.039(3) -0.005(3) 0.008(3) -0.001(2) C34 0.028(3) 0.015(3) 0.053(4) 0.006(3) 0.007(3) 0.009(2) C35 0.024(3) 0.023(3) 0.035(3) 0.012(3) -0.001(2) 0.001(2) C36 0.019(3) 0.017(3) 0.023(3) 0.002(2) 0.002(2) -0.002(2) C41 0.022(3) 0.014(3) 0.015(2) -0.002(2) 0.003(2) 0.001(2) C42 0.019(2) 0.017(3) 0.016(2) -0.001(2) 0.003(2) -0.002(2) C43 0.031(3) 0.015(3) 0.022(3) -0.005(2) 0.004(2) -0.004(2) C44 0.031(3) 0.015(3) 0.027(3) -0.003(2) 0.003(2) 0.006(2) C45 0.022(3) 0.029(3) 0.020(3) 0.001(2) 0.000(2) 0.007(2) C46 0.021(3) 0.019(3) 0.018(3) -0.002(2) -0.003(2) 0.005(2) C51 0.016(2) 0.014(2) 0.017(2) 0.003(2) -0.0011(19) -0.002(2) C52 0.013(2) 0.016(3) 0.025(3) -0.002(2) 0.001(2) -0.003(2) C53 0.028(3) 0.018(3) 0.017(3) -0.003(2) 0.002(2) -0.004(2) C54 0.034(3) 0.022(3) 0.016(3) -0.001(2) -0.004(2) -0.002(2) C55 0.037(3) 0.018(3) 0.024(3) 0.004(2) -0.003(2) 0.007(2) C56 0.033(3) 0.017(3) 0.016(3) -0.005(2) 0.000(2) 0.004(2) C61 0.029(3) 0.019(3) 0.013(2) 0.004(2) 0.011(2) 0.009(2) C62 0.024(3) 0.031(3) 0.019(3) 0.006(2) 0.004(2) 0.009(2) C63 0.030(3) 0.055(4) 0.026(3) 0.015(3) 0.009(2) 0.022(3) C64 0.049(4) 0.039(4) 0.037(4) 0.017(3) 0.019(3) 0.030(3) C65 0.063(4) 0.021(3) 0.027(3) 0.002(3) 0.027(3) 0.014(3) C66 0.039(3) 0.023(3) 0.024(3) 0.005(2) 0.013(2) 0.008(3) C69 0.021(3) 0.072(5) 0.030(3) -0.013(3) -0.004(2) 0.000(3) C71 0.018(2) 0.012(2) 0.021(3) 0.002(2) -0.001(2) 0.005(2) C72 0.023(3) 0.020(3) 0.023(3) -0.005(2) 0.003(2) 0.002(2) C73 0.025(3) 0.027(3) 0.025(3) -0.004(2) 0.005(2) 0.005(2) C74 0.028(3) 0.023(3) 0.020(3) -0.009(2) -0.003(2) 0.008(2) C75 0.027(3) 0.021(3) 0.033(3) -0.008(3) -0.009(2) -0.001(2) C76 0.018(3) 0.022(3) 0.030(3) -0.003(2) 0.004(2) 0.000(2) C81 0.015(2) 0.015(2) 0.013(2) -0.003(2) 0.0032(19) -0.0055(19) C82 0.033(3) 0.022(3) 0.022(3) 0.002(2) -0.006(2) -0.004(2) C83 0.045(4) 0.031(3) 0.014(3) -0.002(2) -0.009(2) -0.007(3) C84 0.038(3) 0.020(3) 0.022(3) -0.007(2) 0.002(2) -0.011(2) C85 0.026(3) 0.015(3) 0.026(3) -0.004(2) 0.009(2) -0.004(2) C86 0.016(2) 0.018(3) 0.022(3) 0.001(2) -0.001(2) -0.003(2) C91 0.022(3) 0.012(2) 0.029(3) -0.002(2) 0.007(2) -0.005(2) C92 0.023(3) 0.023(3) 0.034(3) 0.001(3) 0.011(2) 0.000(2) C93 0.041(3) 0.024(3) 0.026(3) 0.005(3) 0.017(3) 0.005(3) C94 0.029(3) 0.018(3) 0.064(4) 0.009(3) 0.028(3) 0.006(2) C95 0.022(3) 0.034(3) 0.056(4) 0.002(3) 0.012(3) -0.003(3) C96 0.020(3) 0.030(3) 0.045(4) -0.005(3) 0.004(3) -0.004(2) C101 0.017(3) 0.024(3) 0.022(3) -0.009(2) 0.004(2) -0.005(2) C102 0.019(3) 0.037(3) 0.027(3) -0.010(3) 0.001(2) -0.005(2) C103 0.029(3) 0.084(5) 0.040(4) -0.040(4) -0.005(3) -0.012(4) C104 0.035(4) 0.058(5) 0.053(4) -0.039(4) -0.002(3) 0.001(3) C105 0.024(3) 0.035(3) 0.036(3) -0.020(3) 0.002(2) -0.001(3) C111 0.018(2) 0.014(2) 0.018(3) -0.001(2) -0.001(2) -0.001(2) C112 0.019(2) 0.018(3) 0.015(2) -0.005(2) -0.0023(19) -0.001(2) C113 0.019(3) 0.029(3) 0.021(3) -0.002(2) 0.001(2) -0.007(2) C114 0.027(3) 0.024(3) 0.025(3) 0.001(2) -0.005(2) -0.014(2) C115 0.030(3) 0.016(3) 0.030(3) -0.003(2) -0.005(2) 0.000(2) C116 0.020(3) 0.016(3) 0.024(3) -0.004(2) 0.000(2) -0.001(2) C121 0.016(2) 0.014(2) 0.018(2) -0.002(2) -0.0016(19) -0.0014(19) C122 0.014(2) 0.018(3) 0.017(2) 0.003(2) -0.0020(19) 0.001(2) C123 0.021(3) 0.012(3) 0.028(3) -0.004(2) -0.002(2) 0.000(2) C124 0.025(3) 0.011(2) 0.031(3) 0.005(2) -0.005(2) -0.004(2) C125 0.026(3) 0.023(3) 0.023(3) 0.004(2) 0.006(2) -0.006(2) C126 0.024(3) 0.016(3) 0.021(3) 0.002(2) 0.006(2) -0.001(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 O6 1.920(3) . ? Cu1 N2 1.933(4) . ? Cu1 O1 1.979(3) . ? Cu1 N4 2.011(4) . ? Cu1 N11 2.473(4) . ? Cu2 O2 1.924(3) . ? Cu2 N6 1.947(4) . ? Cu2 O3 1.952(3) . ? Cu2 N8 1.974(4) . ? Cu2 N3 2.444(4) . ? Cu3 N10 1.942(4) . ? Cu3 O4 1.955(3) . ? Cu3 O5 1.978(3) . ? Cu3 N12 2.016(4) . ? Cu3 N7 2.312(4) . ? N1 C1 1.326(6) . ? N1 N2 1.394(5) . ? N2 C2 1.311(6) . ? N3 C3 1.304(6) . ? N3 N4 1.397(5) . ? N4 C4 1.332(6) . ? N5 C5 1.330(6) . ? N5 N6 1.377(5) . ? N6 C6 1.300(6) . ? N7 C7 1.307(6) . ? N7 N8 1.409(5) . ? N8 C8 1.348(6) . ? N9 C9 1.324(6) . ? N9 N10 1.392(5) . ? N10 C10 1.311(6) . ? N11 C11 1.298(6) . ? N11 N12 1.399(5) . ? N12 C12 1.339(6) . ? O1 C1 1.290(6) . ? O2 C4 1.265(5) . ? O3 C5 1.293(6) . ? O4 C8 1.268(6) . ? O5 C9 1.280(6) . ? O6 C12 1.277(5) . ? C1 C13 1.488(7) . ? C2 C21 1.470(6) . ? C2 C3 1.503(6) . ? C3 C31 1.482(6) . ? C4 C41 1.497(6) . ? C5 C51 1.486(7) . ? C6 C7 1.480(7) . ? C6 C61 1.483(7) . ? C7 C71 1.496(7) . ? C8 C81 1.479(7) . ? C9 C91 1.488(7) . ? C10 C11 1.481(6) . ? C10 C101 1.500(7) . ? C11 C111 1.484(7) . ? C12 C121 1.496(6) . ? C13 C14 1.394(7) . ? C13 C18 1.398(7) . ? C14 C15 1.388(7) . ? C15 C16 1.393(8) . ? C16 C17 1.363(8) . ? C17 C18 1.380(7) . ? C21 C26 1.399(7) . ? C21 C22 1.405(7) . ? C22 C23 1.387(7) . ? C23 C24 1.380(8) . ? C24 C25 1.381(8) . ? C25 C26 1.399(7) . ? C31 C36 1.391(7) . ? C31 C32 1.395(7) . ? C32 C33 1.399(7) . ? C33 C34 1.374(8) . ? C34 C35 1.392(8) . ? C35 C36 1.382(7) . ? C41 C46 1.398(7) . ? C41 C42 1.407(7) . ? C42 C43 1.375(7) . ? C43 C44 1.385(7) . ? C44 C45 1.387(7) . ? C45 C46 1.399(7) . ? C51 C52 1.390(7) . ? C51 C56 1.393(7) . ? C52 C53 1.380(7) . ? C53 C54 1.396(7) . ? C54 C55 1.372(7) . ? C55 C56 1.379(7) . ? C61 C66 1.393(7) . ? C61 C62 1.408(7) . ? C62 C63 1.387(7) . ? C63 C64 1.374(9) . ? C64 C65 1.386(9) . ? C65 C66 1.386(8) . ? C69 C103 1.378(9) . ? C69 C102 1.384(8) . ? C71 C72 1.388(7) . ? C71 C76 1.394(7) . ? C72 C73 1.388(7) . ? C73 C74 1.397(7) . ? C74 C75 1.374(7) . ? C75 C76 1.380(7) . ? C81 C82 1.390(7) . ? C81 C86 1.395(7) . ? C82 C83 1.378(7) . ? C83 C84 1.380(8) . ? C84 C85 1.389(7) . ? C85 C86 1.381(7) . ? C91 C92 1.389(7) . ? C91 C96 1.398(7) . ? C92 C93 1.395(7) . ? C93 C94 1.384(8) . ? C94 C95 1.386(9) . ? C95 C96 1.387(8) . ? C101 C105 1.384(7) . ? C101 C102 1.389(7) . ? C103 C104 1.359(9) . ? C104 C105 1.395(8) . ? C111 C112 1.386(7) . ? C111 C116 1.399(7) . ? C112 C113 1.390(7) . ? C113 C114 1.386(7) . ? C114 C115 1.386(7) . ? C115 C116 1.381(7) . ? C121 C126 1.385(7) . ? C121 C122 1.399(7) . ? C122 C123 1.396(7) . ? C123 C124 1.380(7) . ? C124 C125 1.391(7) . ? C125 C126 1.387(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 O6 Cu1 N2 173.07(15) . . ? O6 Cu1 O1 92.74(13) . . ? N2 Cu1 O1 80.74(15) . . ? O6 Cu1 N4 99.23(15) . . ? N2 Cu1 N4 85.31(16) . . ? O1 Cu1 N4 148.06(15) . . ? O6 Cu1 N11 70.43(13) . . ? N2 Cu1 N11 114.11(15) . . ? O1 Cu1 N11 111.85(13) . . ? N4 Cu1 N11 100.07(14) . . ? O2 Cu2 N6 173.38(15) . . ? O2 Cu2 O3 92.30(13) . . ? N6 Cu2 O3 81.23(15) . . ? O2 Cu2 N8 98.74(15) . . ? N6 Cu2 N8 86.64(16) . . ? O3 Cu2 N8 154.02(15) . . ? O2 Cu2 N3 72.46(13) . . ? N6 Cu2 N3 110.74(14) . . ? O3 Cu2 N3 107.48(13) . . ? N8 Cu2 N3 98.28(14) . . ? N10 Cu3 O4 171.84(15) . . ? N10 Cu3 O5 80.52(15) . . ? O4 Cu3 O5 93.94(13) . . ? N10 Cu3 N12 86.72(16) . . ? O4 Cu3 N12 96.15(14) . . ? O5 Cu3 N12 155.03(15) . . ? N10 Cu3 N7 112.90(15) . . ? O4 Cu3 N7 74.09(13) . . ? O5 Cu3 N7 103.32(14) . . ? N12 Cu3 N7 101.40(15) . . ? C1 N1 N2 108.8(4) . . ? C2 N2 N1 118.6(4) . . ? C2 N2 Cu1 126.4(3) . . ? N1 N2 Cu1 114.9(3) . . ? C3 N3 N4 118.1(4) . . ? C3 N3 Cu2 138.0(3) . . ? N4 N3 Cu2 103.1(3) . . ? C4 N4 N3 112.7(4) . . ? C4 N4 Cu1 128.8(3) . . ? N3 N4 Cu1 115.1(3) . . ? C5 N5 N6 109.5(4) . . ? C6 N6 N5 118.4(4) . . ? C6 N6 Cu2 127.3(3) . . ? N5 N6 Cu2 114.3(3) . . ? C7 N7 N8 117.8(4) . . ? C7 N7 Cu3 135.6(3) . . ? N8 N7 Cu3 106.1(3) . . ? C8 N8 N7 110.4(4) . . ? C8 N8 Cu2 129.4(3) . . ? N7 N8 Cu2 118.2(3) . . ? C9 N9 N10 108.5(4) . . ? C10 N10 N9 118.2(4) . . ? C10 N10 Cu3 126.6(3) . . ? N9 N10 Cu3 114.7(3) . . ? C11 N11 N12 118.4(4) . . ? C11 N11 Cu1 137.3(3) . . ? N12 N11 Cu1 103.8(3) . . ? C12 N12 N11 111.3(4) . . ? C12 N12 Cu3 129.3(3) . . ? N11 N12 Cu3 115.8(3) . . ? C1 O1 Cu1 109.0(3) . . ? C4 O2 Cu2 120.0(3) . . ? C5 O3 Cu2 109.6(3) . . ? C8 O4 Cu3 117.5(3) . . ? C9 O5 Cu3 109.3(3) . . ? C12 O6 Cu1 121.7(3) . . ? O1 C1 N1 125.3(4) . . ? O1 C1 C13 118.9(4) . . ? N1 C1 C13 115.8(4) . . ? N2 C2 C21 123.3(4) . . ? N2 C2 C3 117.3(4) . . ? C21 C2 C3 119.3(4) . . ? N3 C3 C31 117.3(4) . . ? N3 C3 C2 126.0(4) . . ? C31 C3 C2 116.7(4) . . ? O2 C4 N4 125.2(4) . . ? O2 C4 C41 117.0(4) . . ? N4 C4 C41 117.8(4) . . ? O3 C5 N5 124.8(4) . . ? O3 C5 C51 118.0(4) . . ? N5 C5 C51 117.2(4) . . ? N6 C6 C7 118.2(4) . . ? N6 C6 C61 121.5(4) . . ? C7 C6 C61 120.1(4) . . ? N7 C7 C6 127.7(4) . . ? N7 C7 C71 112.8(4) . . ? C6 C7 C71 119.0(4) . . ? O4 C8 N8 124.8(4) . . ? O4 C8 C81 117.9(4) . . ? N8 C8 C81 117.1(4) . . ? O5 C9 N9 125.8(4) . . ? O5 C9 C91 119.1(4) . . ? N9 C9 C91 115.0(4) . . ? N10 C10 C11 118.1(4) . . ? N10 C10 C101 122.0(4) . . ? C11 C10 C101 119.9(4) . . ? N11 C11 C10 126.3(4) . . ? N11 C11 C111 117.1(4) . . ? C10 C11 C111 116.6(4) . . ? O6 C12 N12 123.8(4) . . ? O6 C12 C121 115.2(4) . . ? N12 C12 C121 120.8(4) . . ? C14 C13 C18 118.9(5) . . ? C14 C13 C1 121.0(5) . . ? C18 C13 C1 120.1(5) . . ? C15 C14 C13 119.9(5) . . ? C14 C15 C16 119.9(5) . . ? C17 C16 C15 120.6(5) . . ? C16 C17 C18 119.9(5) . . ? C17 C18 C13 120.9(5) . . ? C26 C21 C22 117.9(4) . . ? C26 C21 C2 119.8(4) . . ? C22 C21 C2 122.3(4) . . ? C23 C22 C21 120.7(5) . . ? C24 C23 C22 120.3(5) . . ? C23 C24 C25 120.4(5) . . ? C24 C25 C26 119.5(5) . . ? C25 C26 C21 121.1(5) . . ? C36 C31 C32 119.6(4) . . ? C36 C31 C3 120.9(4) . . ? C32 C31 C3 119.5(4) . . ? C31 C32 C33 119.6(5) . . ? C34 C33 C32 120.4(5) . . ? C33 C34 C35 119.8(5) . . ? C36 C35 C34 120.4(5) . . ? C35 C36 C31 120.1(5) . . ? C46 C41 C42 118.6(4) . . ? C46 C41 C4 123.5(4) . . ? C42 C41 C4 117.9(4) . . ? C43 C42 C41 120.7(5) . . ? C42 C43 C44 120.4(5) . . ? C43 C44 C45 120.1(5) . . ? C44 C45 C46 119.8(5) . . ? C41 C46 C45 120.2(5) . . ? C52 C51 C56 118.7(4) . . ? C52 C51 C5 120.1(4) . . ? C56 C51 C5 121.2(4) . . ? C53 C52 C51 120.6(5) . . ? C52 C53 C54 120.1(5) . . ? C55 C54 C53 119.3(5) . . ? C54 C55 C56 120.8(5) . . ? C55 C56 C51 120.5(5) . . ? C66 C61 C62 118.6(5) . . ? C66 C61 C6 123.2(5) . . ? C62 C61 C6 118.3(5) . . ? C63 C62 C61 120.6(5) . . ? C64 C63 C62 119.6(6) . . ? C63 C64 C65 121.0(5) . . ? C64 C65 C66 119.6(6) . . ? C65 C66 C61 120.6(6) . . ? C103 C69 C102 120.7(6) . . ? C72 C71 C76 119.3(5) . . ? C72 C71 C7 119.0(4) . . ? C76 C71 C7 121.7(4) . . ? C71 C72 C73 120.7(5) . . ? C72 C73 C74 119.7(5) . . ? C75 C74 C73 119.0(5) . . ? C74 C75 C76 121.8(5) . . ? C75 C76 C71 119.5(5) . . ? C82 C81 C86 119.3(4) . . ? C82 C81 C8 122.3(4) . . ? C86 C81 C8 118.3(4) . . ? C83 C82 C81 120.0(5) . . ? C82 C83 C84 120.5(5) . . ? C83 C84 C85 120.0(5) . . ? C86 C85 C84 119.6(5) . . ? C85 C86 C81 120.5(5) . . ? C92 C91 C96 119.6(5) . . ? C92 C91 C9 122.1(5) . . ? C96 C91 C9 118.4(5) . . ? C91 C92 C93 120.3(5) . . ? C94 C93 C92 119.8(6) . . ? C93 C94 C95 120.0(5) . . ? C94 C95 C96 120.5(6) . . ? C95 C96 C91 119.7(6) . . ? C105 C101 C102 119.8(5) . . ? C105 C101 C10 121.8(5) . . ? C102 C101 C10 118.3(5) . . ? C69 C102 C101 119.4(5) . . ? C104 C103 C69 120.0(6) . . ? C103 C104 C105 120.5(6) . . ? C101 C105 C104 119.6(6) . . ? C112 C111 C116 119.2(4) . . ? C112 C111 C11 120.4(4) . . ? C116 C111 C11 120.3(4) . . ? C111 C112 C113 119.7(5) . . ? C114 C113 C112 121.1(5) . . ? C115 C114 C113 119.0(5) . . ? C116 C115 C114 120.5(5) . . ? C115 C116 C111 120.4(5) . . ? C126 C121 C122 119.9(4) . . ? C126 C121 C12 123.5(4) . . ? C122 C121 C12 116.6(4) . . ? C123 C122 C121 119.8(5) . . ? C124 C123 C122 120.2(5) . . ? C123 C124 C125 119.6(5) . . ? C126 C125 C124 120.8(5) . . ? C121 C126 C125 119.7(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.138 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.229