Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Peter James Steel' 'Christopher J. Sumby' _publ_contact_author_name 'Prof Peter James Steel' _publ_contact_author_address ; Department of Chemistry University of Canterbury Private Bag 4800 Christchurch NEW ZEALAND ; _publ_contact_author_email P.STEEL@CHEM.CATERBURY.AC.NZ _publ_section_title ; Coordination chemistry of di-2-pyridylmethane and related bridging ligands with silver(I), copper(II), palladium(II) and zinc(II) ; data_Compound-7 _database_code_CSD 216634 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H10 Ag N3 O3' _chemical_formula_weight 340.09 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' Ag Ag -0.8971 1.1015 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 5.477(3) _cell_length_b 8.370(5) _cell_length_c 12.711(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.762(10) _cell_angle_gamma 90.00 _cell_volume 581.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 2336 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.12 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 1.737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.613267 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 4893 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.47 _reflns_number_total 1175 _reflns_number_gt 861 _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^)+(0.1019P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1175 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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 Ag1 Ag 1.0000 0.24619(6) 0.2500 0.0300(3) Uani 1 2 d S . . C1 C 0.5000 0.4824(9) 0.2500 0.0287(16) Uani 1 2 d S . . H1A H 0.3583 0.5501 0.2485 0.034 Uiso 1 1 d R . . N11 N 0.6810(9) 0.2859(5) 0.1342(4) 0.0251(10) Uani 1 1 d . . . C12 C 0.4902(9) 0.3827(6) 0.1496(3) 0.0238(11) Uani 1 1 d . . . C13 C 0.2911(9) 0.3932(6) 0.0762(4) 0.0277(11) Uani 1 1 d . . . H13A H 0.1572 0.4610 0.0890 0.033 Uiso 1 1 calc R . . C14 C 0.2891(11) 0.3030(7) -0.0169(4) 0.0302(12) Uani 1 1 d . . . H14A H 0.1536 0.3075 -0.0675 0.036 Uiso 1 1 calc R . . C15 C 0.4897(11) 0.2069(7) -0.0334(5) 0.0315(13) Uani 1 1 d . . . H15A H 0.4957 0.1471 -0.0967 0.038 Uiso 1 1 calc R . . C16 C 0.6802(10) 0.1991(7) 0.0431(4) 0.0288(12) Uani 1 1 d . . . H16A H 0.8151 0.1311 0.0320 0.035 Uiso 1 1 calc R . . N21 N 1.0000 -0.1161(8) 0.2500 0.0347(16) Uani 1 2 d S . . O22 O 0.9191(9) -0.0397(5) 0.3256(3) 0.0480(11) Uani 1 1 d . . . O23 O 1.0000 -0.2664(6) 0.2500 0.0464(18) Uani 1 2 d S . . 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 Ag1 0.0281(4) 0.0361(4) 0.0241(4) 0.000 -0.0113(2) 0.000 C1 0.036(4) 0.024(4) 0.026(4) 0.000 -0.001(3) 0.000 N11 0.024(2) 0.034(2) 0.016(2) -0.0006(16) -0.0072(18) -0.0017(17) C12 0.032(3) 0.025(2) 0.014(2) 0.0038(18) -0.005(2) -0.001(2) C13 0.027(3) 0.033(3) 0.023(3) 0.007(2) -0.003(2) 0.001(2) C14 0.027(3) 0.043(3) 0.020(3) 0.005(2) -0.010(2) -0.007(2) C15 0.037(3) 0.034(3) 0.023(3) 0.001(2) -0.007(3) -0.007(2) C16 0.030(3) 0.034(3) 0.022(3) -0.004(2) -0.004(2) 0.000(2) N21 0.041(4) 0.037(4) 0.024(3) 0.000 -0.017(3) 0.000 O22 0.070(3) 0.043(2) 0.031(2) -0.0029(18) 0.006(2) -0.007(2) O23 0.055(4) 0.035(4) 0.045(4) 0.000 -0.026(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N11 2.234(5) . ? Ag1 N11 2.234(5) 2_755 ? C1 C12 1.523(6) . ? C1 C12 1.523(6) 2_655 ? N11 C12 1.347(6) . ? N11 C16 1.367(7) . ? C12 C13 1.391(7) . ? C13 C14 1.403(8) . ? C14 C15 1.388(10) . ? C15 C16 1.380(8) . ? N21 O23 1.259(7) . ? N21 O22 1.259(5) . ? N21 O22 1.259(5) 2_755 ? 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 N11 Ag1 N11 162.9(2) . 2_755 ? C12 C1 C12 113.5(6) . 2_655 ? C12 N11 C16 118.9(5) . . ? C12 N11 Ag1 125.0(3) . . ? C16 N11 Ag1 116.0(4) . . ? N11 C12 C13 121.5(5) . . ? N11 C12 C1 117.8(4) . . ? C13 C12 C1 120.7(4) . . ? C12 C13 C14 119.6(5) . . ? C15 C14 C13 118.4(5) . . ? C16 C15 C14 119.4(5) . . ? N11 C16 C15 122.1(5) . . ? O23 N21 O22 120.5(3) . . ? O23 N21 O22 120.5(3) . 2_755 ? O22 N21 O22 119.0(7) . 2_755 ? 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 N11 Ag1 N11 C12 -50.4(4) 2_755 . . . ? N11 Ag1 N11 C16 132.2(4) 2_755 . . . ? C16 N11 C12 C13 1.5(7) . . . . ? Ag1 N11 C12 C13 -175.9(4) . . . . ? C16 N11 C12 C1 -177.9(5) . . . . ? Ag1 N11 C12 C1 4.7(6) . . . . ? C12 C1 C12 N11 -62.1(4) 2_655 . . . ? C12 C1 C12 C13 118.5(5) 2_655 . . . ? N11 C12 C13 C14 -0.9(7) . . . . ? C1 C12 C13 C14 178.4(5) . . . . ? C12 C13 C14 C15 -0.9(8) . . . . ? C13 C14 C15 C16 2.0(8) . . . . ? C12 N11 C16 C15 -0.3(8) . . . . ? Ag1 N11 C16 C15 177.3(4) . . . . ? C14 C15 C16 N11 -1.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.719 _refine_diff_density_min -1.722 _refine_diff_density_rms 0.211 data_Compound-11 _database_code_CSD 216635 _chemical_name_common 11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H49 Cu6 N19 O26' _chemical_formula_weight 1761.36 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.473(4) _cell_length_b 24.872(7) _cell_length_c 20.202(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.596(4) _cell_angle_gamma 90.00 _cell_volume 6932(3) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 7515 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.28 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 1.901 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.4499 _exptl_absorpt_correction_T_max 0.5727 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 50777 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.38 _reflns_number_total 14005 _reflns_number_gt 8660 _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^)+(0.0261P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14005 _refine_ls_number_parameters 971 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.900 _refine_ls_shift/su_max 0.002 _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 0.35172(2) 0.423140(13) 0.310914(16) 0.02110(9) Uani 1 1 d . . . Cu2 Cu 0.18326(3) 0.422216(13) 0.186273(16) 0.02123(9) Uani 1 1 d . . . Cu3 Cu 0.20889(3) 0.299490(13) 0.287088(16) 0.02280(9) Uani 1 1 d . . . Cu4 Cu 0.34566(3) 0.307998(13) 0.200771(16) 0.02269(9) Uani 1 1 d . . . Cu5 Cu -0.03680(3) 0.365350(13) 0.093608(17) 0.02512(9) Uani 1 1 d . . . Cu6 Cu 0.58017(3) 0.374580(14) 0.393269(17) 0.02696(10) Uani 1 1 d . . . N1 N 0.25823(18) 0.30412(8) 0.38976(11) 0.0236(6) Uani 1 1 d . . . C2 C 0.3556(2) 0.30818(10) 0.41461(13) 0.0222(7) Uani 1 1 d . . . C3 C 0.4020(2) 0.31270(11) 0.48550(13) 0.0318(8) Uani 1 1 d . . . H3A H 0.4707 0.3146 0.5028 0.038 Uiso 1 1 calc R . . C4 C 0.3462(3) 0.31434(11) 0.53069(15) 0.0362(8) Uani 1 1 d . . . H4A H 0.3766 0.3174 0.5793 0.043 Uiso 1 1 calc R . . C5 C 0.2463(3) 0.31157(11) 0.50475(15) 0.0353(8) Uani 1 1 d . . . H5A H 0.2073 0.3136 0.5350 0.042 Uiso 1 1 calc R . . C6 C 0.2039(2) 0.30572(10) 0.43373(14) 0.0292(7) Uani 1 1 d . . . H6A H 0.1354 0.3028 0.4156 0.035 Uiso 1 1 calc R . . C10 C 0.4105(2) 0.31081(11) 0.35964(13) 0.0228(7) Uani 1 1 d . . . O11 O 0.44295(13) 0.36412(7) 0.35706(8) 0.0205(4) Uani 1 1 d . . . O12 O 0.34622(13) 0.29507(7) 0.29632(8) 0.0226(5) Uani 1 1 d . . . N11 N 0.58550(18) 0.29641(9) 0.39896(11) 0.0299(6) Uani 1 1 d . . . C12 C 0.4974(2) 0.27261(11) 0.37899(13) 0.0253(7) Uani 1 1 d . . . C13 C 0.4889(3) 0.21697(12) 0.37753(14) 0.0403(9) Uani 1 1 d . . . H13A H 0.4269 0.2004 0.3636 0.048 Uiso 1 1 calc R . . C14 C 0.5726(3) 0.18589(13) 0.39669(17) 0.0592(12) Uani 1 1 d . . . H14A H 0.5683 0.1478 0.3970 0.071 Uiso 1 1 calc R . . C15 C 0.6621(3) 0.21077(14) 0.41527(17) 0.0611(12) Uani 1 1 d . . . H15A H 0.7199 0.1900 0.4271 0.073 Uiso 1 1 calc R . . C16 C 0.6666(2) 0.26595(13) 0.41647(15) 0.0452(9) Uani 1 1 d . . . H16A H 0.7281 0.2831 0.4299 0.054 Uiso 1 1 calc R . . N21 N 0.29450(17) 0.31525(8) 0.09802(11) 0.0221(6) Uani 1 1 d . . . C22 C 0.1966(2) 0.31512(10) 0.07347(13) 0.0207(7) Uani 1 1 d . . . C23 C 0.1489(2) 0.32187(10) 0.00314(13) 0.0270(7) Uani 1 1 d . . . H23A H 0.0801 0.3213 -0.0138 0.032 Uiso 1 1 calc R . . C24 C 0.2038(3) 0.32949(11) -0.04195(14) 0.0340(8) Uani 1 1 d . . . H24A H 0.1725 0.3340 -0.0902 0.041 Uiso 1 1 calc R . . C25 C 0.3034(3) 0.33043(11) -0.01667(15) 0.0350(8) Uani 1 1 d . . . H25A H 0.3415 0.3363 -0.0470 0.042 Uiso 1 1 calc R . . C26 C 0.3470(2) 0.32274(11) 0.05354(14) 0.0311(8) Uani 1 1 d . . . H26A H 0.4157 0.3227 0.0711 0.037 Uiso 1 1 calc R . . C30 C 0.1423(2) 0.31068(10) 0.12901(13) 0.0208(7) Uani 1 1 d . . . O31 O 0.21036(13) 0.29554(7) 0.19121(8) 0.0214(4) Uani 1 1 d . . . O32 O 0.10069(13) 0.36116(7) 0.13472(8) 0.0206(4) Uani 1 1 d . . . N31 N -0.02886(17) 0.28696(9) 0.08513(11) 0.0247(6) Uani 1 1 d . . . C32 C 0.0629(2) 0.26785(11) 0.10857(12) 0.0214(7) Uani 1 1 d . . . C33 C 0.0818(2) 0.21304(11) 0.11285(13) 0.0255(7) Uani 1 1 d . . . H33A H 0.1465 0.2003 0.1302 0.031 Uiso 1 1 calc R . . C34 C 0.0050(2) 0.17705(12) 0.09150(14) 0.0334(8) Uani 1 1 d . . . H34A H 0.0165 0.1394 0.0935 0.040 Uiso 1 1 calc R . . C35 C -0.0885(2) 0.19693(12) 0.06723(15) 0.0378(8) Uani 1 1 d . . . H35A H -0.1420 0.1730 0.0520 0.045 Uiso 1 1 calc R . . C36 C -0.1035(2) 0.25187(12) 0.06534(14) 0.0338(8) Uani 1 1 d . . . H36A H -0.1679 0.2653 0.0497 0.041 Uiso 1 1 calc R . . N41 N 0.31924(17) 0.44204(8) 0.39656(10) 0.0218(6) Uani 1 1 d . . . C42 C 0.2247(2) 0.44058(10) 0.39376(13) 0.0203(7) Uani 1 1 d . . . C43 C 0.1956(2) 0.44800(11) 0.45227(13) 0.0275(7) Uani 1 1 d . . . H43A H 0.1288 0.4473 0.4491 0.033 Uiso 1 1 calc R . . C44 C 0.2654(2) 0.45643(11) 0.51560(14) 0.0323(8) Uani 1 1 d . . . H44A H 0.2471 0.4608 0.5567 0.039 Uiso 1 1 calc R . . C45 C 0.3622(2) 0.45843(11) 0.51835(14) 0.0297(8) Uani 1 1 d . . . H45A H 0.4108 0.4647 0.5612 0.036 Uiso 1 1 calc R . . C46 C 0.3874(2) 0.45116(10) 0.45803(13) 0.0266(7) Uani 1 1 d . . . H46A H 0.4537 0.4526 0.4599 0.032 Uiso 1 1 calc R . . C50 C 0.1541(2) 0.43169(10) 0.31993(13) 0.0201(7) Uani 1 1 d . . . O51 O 0.07065(14) 0.40730(8) 0.33122(9) 0.0331(5) Uani 1 1 d . . . H51 H 0.0296 0.4004 0.2928 0.050 Uiso 1 1 calc R . . O52 O 0.19648(13) 0.39876(7) 0.28105(8) 0.0196(4) Uani 1 1 d . . . N51 N 0.14260(16) 0.49147(8) 0.22137(11) 0.0226(6) Uani 1 1 d . . . C52 C 0.12687(19) 0.48698(10) 0.28354(13) 0.0202(6) Uani 1 1 d . . . C53 C 0.0885(2) 0.52908(11) 0.31216(14) 0.0301(7) Uani 1 1 d . . . H53A H 0.0787 0.5252 0.3563 0.036 Uiso 1 1 calc R . . C54 C 0.0645(2) 0.57704(12) 0.27512(15) 0.0371(8) Uani 1 1 d . . . H54A H 0.0366 0.6059 0.2932 0.045 Uiso 1 1 calc R . . C55 C 0.0819(2) 0.58194(12) 0.21193(15) 0.0361(8) Uani 1 1 d . . . H55A H 0.0679 0.6147 0.1866 0.043 Uiso 1 1 calc R . . C56 C 0.1200(2) 0.53876(11) 0.18580(14) 0.0301(8) Uani 1 1 d . . . H56A H 0.1307 0.5421 0.1418 0.036 Uiso 1 1 calc R . . N61 N 0.21421(18) 0.44991(8) 0.10336(11) 0.0229(6) Uani 1 1 d . . . C62 C 0.3078(2) 0.45522(10) 0.10701(14) 0.0238(7) Uani 1 1 d . . . C63 C 0.3370(2) 0.46897(11) 0.04990(14) 0.0325(8) Uani 1 1 d . . . H63A H 0.4039 0.4727 0.0542 0.039 Uiso 1 1 calc R . . C64 C 0.2678(3) 0.47721(12) -0.01320(15) 0.0406(9) Uani 1 1 d . . . H64A H 0.2863 0.4864 -0.0530 0.049 Uiso 1 1 calc R . . C65 C 0.1712(3) 0.47188(11) -0.01761(14) 0.0351(8) Uani 1 1 d . . . H65A H 0.1224 0.4772 -0.0607 0.042 Uiso 1 1 calc R . . C66 C 0.1464(2) 0.45869(10) 0.04127(14) 0.0290(7) Uani 1 1 d . . . H66A H 0.0798 0.4557 0.0382 0.035 Uiso 1 1 calc R . . C70 C 0.3800(2) 0.44501(11) 0.17997(14) 0.0239(7) Uani 1 1 d . . . O71 O 0.46833(16) 0.42753(9) 0.16918(11) 0.0446(6) Uani 1 1 d . . . H71 H 0.4973 0.4065 0.2012 0.067 Uiso 1 1 calc R . . O72 O 0.34184(13) 0.40659(7) 0.21488(8) 0.0204(4) Uani 1 1 d . . . N71 N 0.37773(16) 0.49807(8) 0.28172(11) 0.0248(6) Uani 1 1 d . . . C72 C 0.3989(2) 0.49855(11) 0.22132(14) 0.0259(7) Uani 1 1 d . . . C73 C 0.4387(2) 0.54374(12) 0.19942(16) 0.0451(9) Uani 1 1 d . . . H73A H 0.4529 0.5434 0.1565 0.054 Uiso 1 1 calc R . . C74 C 0.4571(3) 0.58913(13) 0.24106(18) 0.0545(11) Uani 1 1 d . . . H74A H 0.4856 0.6201 0.2276 0.065 Uiso 1 1 calc R . . C75 C 0.4335(2) 0.58878(12) 0.30275(17) 0.0452(9) Uani 1 1 d . . . H75A H 0.4445 0.6197 0.3316 0.054 Uiso 1 1 calc R . . C76 C 0.3941(2) 0.54324(11) 0.32158(15) 0.0326(8) Uani 1 1 d . . . H76A H 0.3778 0.5433 0.3637 0.039 Uiso 1 1 calc R . . N110 N 0.5228(3) 0.26407(17) 0.21910(15) 0.0654(11) Uani 1 1 d . . . O111 O 0.48534(15) 0.31235(9) 0.21519(10) 0.0404(6) Uani 1 1 d . . . O112 O 0.6112(2) 0.26041(15) 0.23924(14) 0.1161(14) Uani 1 1 d . . . O113 O 0.4665(2) 0.22570(11) 0.20151(13) 0.0733(9) Uani 1 1 d . . . N120 N 0.0583(2) 0.23321(11) 0.27091(12) 0.0352(7) Uani 1 1 d . . . O121 O 0.06962(14) 0.28556(8) 0.27211(9) 0.0304(5) Uani 1 1 d . . . O122 O -0.02420(18) 0.21500(10) 0.25442(13) 0.0615(8) Uani 1 1 d . . . O123 O 0.13231(18) 0.20474(8) 0.28648(10) 0.0445(6) Uani 1 1 d . . . N130 N -0.08199(19) 0.44099(12) 0.17145(14) 0.0400(7) Uani 1 1 d . . . O131 O -0.04140(15) 0.44166(7) 0.12197(10) 0.0342(5) Uani 1 1 d . . . O132 O -0.10924(18) 0.48331(10) 0.19025(12) 0.0596(7) Uani 1 1 d . . . O133 O -0.08875(17) 0.39605(9) 0.19797(11) 0.0520(7) Uani 1 1 d . . . N140 N 0.6261(2) 0.45489(12) 0.32538(14) 0.0460(8) Uani 1 1 d . . . O141 O 0.57183(15) 0.45094(8) 0.36606(11) 0.0370(5) Uani 1 1 d . . . O142 O 0.64898(19) 0.50007(10) 0.31054(12) 0.0734(9) Uani 1 1 d . . . O143 O 0.65231(19) 0.41180(11) 0.30427(12) 0.0643(8) Uani 1 1 d . . . N150 N -0.1608(2) 0.39540(9) -0.02412(13) 0.0333(7) Uani 1 1 d . . . O151 O -0.17172(14) 0.37218(7) 0.03131(10) 0.0327(5) Uani 1 1 d . . . O152 O -0.07587(16) 0.40371(8) -0.02525(10) 0.0390(6) Uani 1 1 d . . . O153 O -0.23336(16) 0.40792(8) -0.07131(11) 0.0476(6) Uani 1 1 d . . . N160 N 0.6957(2) 0.40255(9) 0.51650(13) 0.0347(7) Uani 1 1 d . . . O161 O 0.71270(14) 0.38634(8) 0.45977(10) 0.0362(5) Uani 1 1 d . . . O162 O 0.76451(16) 0.41503(8) 0.56697(11) 0.0518(7) Uani 1 1 d . . . O163 O 0.60958(16) 0.40487(8) 0.51682(10) 0.0390(6) Uani 1 1 d . . . C81 C 0.1089(3) 0.55944(17) 0.5994(3) 0.1124(19) Uani 1 1 d U . . H81A H 0.1611 0.5626 0.6433 0.169 Uiso 1 1 calc R . . H81B H 0.0530 0.5806 0.6019 0.169 Uiso 1 1 calc R . . H81C H 0.1315 0.5729 0.5614 0.169 Uiso 1 1 calc R . . C82 C 0.0804(3) 0.5026(2) 0.5866(2) 0.0767(14) Uani 1 1 d . . . N83 N 0.0603(3) 0.45922(16) 0.5773(2) 0.0971(14) Uani 1 1 d . . . C85 C 0.8422(3) 0.30742(16) 0.3048(2) 0.0850(14) Uani 1 1 d . . . H85A H 0.8816 0.3118 0.2734 0.128 Uiso 1 1 calc R . . H85B H 0.8265 0.3428 0.3198 0.128 Uiso 1 1 calc R . . H85C H 0.7822 0.2884 0.2807 0.128 Uiso 1 1 calc R . . C86 C 0.8954(4) 0.2770(3) 0.3643(3) 0.1042(19) Uani 1 1 d . . . N87 N 0.9338(4) 0.2514(3) 0.4093(2) 0.202(3) Uani 1 1 d U . . C91 C 0.7472(3) 0.31749(16) 0.6832(2) 0.0803(14) Uani 1 1 d D . . H91A H 0.7509 0.3555 0.6716 0.120 Uiso 1 1 calc R . . H91B H 0.8123 0.3018 0.6964 0.120 Uiso 1 1 calc R . . H91C H 0.7200 0.3143 0.7219 0.120 Uiso 1 1 calc R . . C92 C 0.6849(3) 0.28895(19) 0.6227(2) 0.0699(13) Uani 1 1 d D . . N93 N 0.6376(3) 0.26747(19) 0.5761(2) 0.1127(17) Uani 1 1 d D . . C95 C 0.6549(6) 0.1195(4) 0.6215(4) 0.222(5) Uani 1 1 d . . . H95A H 0.6656 0.0912 0.6567 0.333 Uiso 1 1 calc R . . H95B H 0.6249 0.1507 0.6364 0.333 Uiso 1 1 calc R . . H95C H 0.7172 0.1301 0.6156 0.333 Uiso 1 1 calc R . . C96 C 0.5909(8) 0.0994(4) 0.5554(5) 0.171(5) Uani 1 1 d U . . N97 N 0.5279(7) 0.0858(3) 0.4935(5) 0.234(5) Uani 1 1 d U . . C100 C 0.6196(8) 0.5897(4) 0.1332(6) 0.109(5) Uani 0.387(4) 1 d PDU A 1 H10A H 0.6357 0.6047 0.0932 0.163 Uiso 0.387(4) 1 d PR A 1 H10B H 0.5671 0.6107 0.1418 0.163 Uiso 0.387(4) 1 d PR A 1 H10C H 0.5987 0.5523 0.1235 0.163 Uiso 0.387(4) 1 d PR A 1 C101 C 0.7008(9) 0.5911(5) 0.1933(7) 0.079(4) Uani 0.387(4) 1 d PDU A 1 N102 N 0.7685(6) 0.5819(3) 0.2384(4) 0.162(3) Uani 0.387(4) 1 d PDU A 1 C105 C 0.7685(6) 0.5819(3) 0.2384(4) 0.162(3) Uani 0.61 1 d PDU A 2 H10D H 0.7817 0.5450 0.2558 0.243 Uiso 0.613(4) 1 d PR A 2 H10E H 0.8286 0.5983 0.2353 0.243 Uiso 0.613(4) 1 d PR A 2 H10F H 0.7205 0.5813 0.1923 0.243 Uiso 0.613(4) 1 d PR A 2 C106 C 0.7324(5) 0.6119(3) 0.2837(4) 0.060(2) Uani 0.613(4) 1 d PD A 2 N107 N 0.7131(4) 0.6343(2) 0.3245(3) 0.090(2) Uani 0.613(4) 1 d PD A 2 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 0.0250(2) 0.01825(19) 0.01989(17) -0.00091(14) 0.00654(16) 0.00214(16) Cu2 0.0275(2) 0.01703(19) 0.01844(17) 0.00002(14) 0.00582(16) -0.00053(16) Cu3 0.0255(2) 0.0229(2) 0.01935(18) 0.00046(15) 0.00587(16) -0.00281(16) Cu4 0.0224(2) 0.0249(2) 0.02069(18) -0.00235(15) 0.00630(16) 0.00140(16) Cu5 0.0226(2) 0.0233(2) 0.02585(19) 0.00096(15) 0.00196(17) -0.00040(16) Cu6 0.0212(2) 0.0263(2) 0.0298(2) -0.00331(16) 0.00227(17) 0.00257(17) N1 0.0335(17) 0.0169(13) 0.0234(13) 0.0024(10) 0.0132(12) -0.0003(12) C2 0.033(2) 0.0114(15) 0.0232(15) 0.0021(12) 0.0097(14) -0.0020(13) C3 0.044(2) 0.0271(18) 0.0208(15) 0.0011(13) 0.0047(15) -0.0062(15) C4 0.058(3) 0.0272(18) 0.0210(16) 0.0000(13) 0.0087(17) -0.0066(17) C5 0.056(3) 0.0271(18) 0.0317(18) 0.0006(14) 0.0267(18) -0.0017(17) C6 0.036(2) 0.0216(17) 0.0324(17) 0.0028(13) 0.0141(16) -0.0004(15) C10 0.0267(18) 0.0198(16) 0.0195(14) -0.0013(12) 0.0034(13) -0.0018(14) O11 0.0193(11) 0.0175(10) 0.0222(10) 0.0025(8) 0.0026(9) 0.0023(9) O12 0.0216(12) 0.0263(11) 0.0184(10) -0.0018(8) 0.0041(9) -0.0009(9) N11 0.0309(17) 0.0261(14) 0.0266(13) -0.0032(11) -0.0005(12) 0.0132(13) C12 0.030(2) 0.0221(17) 0.0187(15) -0.0008(12) -0.0008(14) 0.0052(14) C13 0.053(2) 0.0260(19) 0.0326(18) -0.0013(14) -0.0004(17) 0.0014(17) C14 0.085(3) 0.025(2) 0.047(2) -0.0047(16) -0.012(2) 0.023(2) C15 0.059(3) 0.044(2) 0.057(2) -0.0152(19) -0.018(2) 0.031(2) C16 0.031(2) 0.047(2) 0.046(2) -0.0087(17) -0.0058(17) 0.0193(17) N21 0.0257(16) 0.0191(13) 0.0235(13) -0.0048(10) 0.0103(12) -0.0024(11) C22 0.0302(19) 0.0100(14) 0.0240(15) -0.0034(11) 0.0113(14) -0.0012(13) C23 0.031(2) 0.0258(17) 0.0220(15) -0.0017(12) 0.0053(15) 0.0000(14) C24 0.057(3) 0.0241(18) 0.0212(16) 0.0006(13) 0.0118(17) -0.0009(16) C25 0.055(3) 0.0288(19) 0.0301(17) -0.0047(14) 0.0254(18) -0.0058(17) C26 0.033(2) 0.0306(18) 0.0345(17) -0.0070(14) 0.0172(16) -0.0075(15) C30 0.0214(17) 0.0209(16) 0.0181(14) -0.0011(12) 0.0028(13) 0.0009(13) O31 0.0212(12) 0.0241(11) 0.0183(10) -0.0001(8) 0.0050(9) 0.0009(9) O32 0.0195(12) 0.0164(10) 0.0236(10) -0.0047(8) 0.0031(9) 0.0001(8) N31 0.0229(15) 0.0223(14) 0.0260(13) -0.0014(10) 0.0028(11) -0.0052(12) C32 0.0283(19) 0.0229(16) 0.0124(13) -0.0006(11) 0.0053(13) -0.0026(14) C33 0.032(2) 0.0226(17) 0.0225(15) 0.0001(12) 0.0088(14) 0.0014(14) C34 0.047(2) 0.0218(17) 0.0328(17) -0.0016(13) 0.0148(17) -0.0074(16) C35 0.040(2) 0.0300(19) 0.0400(19) -0.0050(15) 0.0067(17) -0.0183(17) C36 0.026(2) 0.038(2) 0.0345(18) -0.0006(15) 0.0047(15) -0.0058(16) N41 0.0238(16) 0.0190(13) 0.0220(12) -0.0023(10) 0.0057(11) 0.0026(11) C42 0.0264(19) 0.0115(14) 0.0225(15) 0.0003(11) 0.0066(14) 0.0004(13) C43 0.0272(19) 0.0298(18) 0.0274(16) -0.0009(13) 0.0115(15) 0.0038(14) C44 0.045(2) 0.0316(19) 0.0231(16) -0.0029(13) 0.0149(16) 0.0049(16) C45 0.035(2) 0.0266(18) 0.0226(16) -0.0028(13) 0.0019(15) 0.0039(15) C46 0.0245(19) 0.0250(17) 0.0272(16) -0.0046(13) 0.0031(14) 0.0021(14) C50 0.0170(17) 0.0218(16) 0.0226(15) -0.0010(12) 0.0074(13) -0.0024(13) O51 0.0290(14) 0.0397(13) 0.0309(11) -0.0030(10) 0.0097(10) -0.0075(11) O52 0.0233(12) 0.0170(10) 0.0188(9) 0.0009(8) 0.0066(9) 0.0017(9) N51 0.0272(16) 0.0168(13) 0.0223(12) -0.0011(10) 0.0052(11) 0.0007(11) C52 0.0161(17) 0.0205(16) 0.0225(15) -0.0021(12) 0.0040(13) -0.0018(13) C53 0.029(2) 0.0306(19) 0.0307(17) -0.0065(14) 0.0095(15) 0.0029(15) C54 0.038(2) 0.0274(18) 0.044(2) -0.0098(15) 0.0100(17) 0.0083(16) C55 0.045(2) 0.0219(18) 0.0364(18) 0.0037(14) 0.0045(16) 0.0087(16) C56 0.037(2) 0.0235(17) 0.0264(16) 0.0023(13) 0.0048(15) 0.0034(15) N61 0.0311(16) 0.0164(13) 0.0195(12) 0.0004(10) 0.0050(12) 0.0002(11) C62 0.033(2) 0.0146(15) 0.0253(15) 0.0002(12) 0.0117(15) 0.0028(14) C63 0.041(2) 0.0308(18) 0.0300(17) 0.0035(14) 0.0180(16) -0.0023(15) C64 0.064(3) 0.035(2) 0.0311(18) 0.0069(15) 0.0266(19) 0.0003(19) C65 0.055(3) 0.0242(18) 0.0208(16) 0.0038(13) 0.0040(16) 0.0024(17) C66 0.036(2) 0.0206(17) 0.0276(16) 0.0018(13) 0.0055(15) 0.0006(14) C70 0.0228(19) 0.0245(17) 0.0270(16) 0.0035(13) 0.0114(14) 0.0020(14) O71 0.0380(15) 0.0522(16) 0.0495(15) 0.0132(11) 0.0220(12) 0.0100(12) O72 0.0232(12) 0.0191(10) 0.0197(10) 0.0004(8) 0.0079(9) -0.0003(9) N71 0.0271(16) 0.0193(13) 0.0262(13) 0.0005(10) 0.0054(12) 0.0007(11) C72 0.0228(19) 0.0234(17) 0.0292(16) 0.0032(13) 0.0045(14) -0.0023(14) C73 0.057(3) 0.040(2) 0.0394(19) 0.0045(16) 0.0154(18) -0.0179(19) C74 0.070(3) 0.035(2) 0.052(2) 0.0039(17) 0.009(2) -0.0264(19) C75 0.060(3) 0.0212(19) 0.045(2) -0.0046(15) 0.0027(19) -0.0088(17) C76 0.035(2) 0.0242(18) 0.0337(17) -0.0049(14) 0.0035(15) -0.0037(15) N110 0.047(3) 0.113(3) 0.0309(17) -0.016(2) 0.0054(17) 0.039(2) O111 0.0231(13) 0.0526(15) 0.0468(14) -0.0094(11) 0.0126(11) 0.0041(12) O112 0.048(2) 0.217(4) 0.071(2) -0.030(2) -0.0004(17) 0.074(2) O113 0.107(3) 0.0549(19) 0.0468(16) -0.0058(14) 0.0062(17) 0.0402(17) N120 0.043(2) 0.0399(19) 0.0263(14) -0.0070(13) 0.0166(14) -0.0165(16) O121 0.0316(13) 0.0267(12) 0.0347(12) -0.0036(9) 0.0126(10) -0.0067(10) O122 0.0496(18) 0.0649(18) 0.0762(18) -0.0241(14) 0.0282(15) -0.0372(15) O123 0.0611(18) 0.0307(14) 0.0401(13) 0.0044(10) 0.0128(12) 0.0016(12) N130 0.0325(19) 0.0441(19) 0.0356(16) -0.0077(14) -0.0013(14) 0.0088(15) O131 0.0353(14) 0.0258(12) 0.0384(12) -0.0015(10) 0.0067(11) 0.0045(10) O132 0.0626(19) 0.0543(17) 0.0594(16) -0.0192(13) 0.0148(14) 0.0208(14) O133 0.0636(19) 0.0504(16) 0.0450(14) 0.0074(12) 0.0209(13) 0.0042(14) N140 0.047(2) 0.046(2) 0.0350(17) 0.0072(15) -0.0022(15) -0.0113(17) O141 0.0316(14) 0.0278(13) 0.0505(14) 0.0004(10) 0.0107(12) -0.0014(10) O142 0.085(2) 0.0569(19) 0.0701(18) 0.0214(14) 0.0110(16) -0.0283(16) O143 0.086(2) 0.0623(19) 0.0556(16) -0.0094(14) 0.0384(15) -0.0082(16) N150 0.0377(19) 0.0214(15) 0.0308(15) 0.0001(12) -0.0049(14) -0.0038(13) O151 0.0263(13) 0.0321(12) 0.0335(12) 0.0099(10) -0.0001(10) -0.0016(10) O152 0.0324(15) 0.0494(15) 0.0328(12) 0.0039(10) 0.0061(11) -0.0086(12) O153 0.0435(16) 0.0377(14) 0.0427(14) 0.0124(11) -0.0154(12) -0.0045(11) N160 0.039(2) 0.0224(15) 0.0353(16) 0.0008(12) 0.0002(15) 0.0008(14) O161 0.0231(13) 0.0430(14) 0.0370(13) -0.0042(10) 0.0010(10) 0.0021(10) O162 0.0454(16) 0.0463(15) 0.0432(14) -0.0079(11) -0.0173(12) -0.0034(12) O163 0.0340(16) 0.0444(14) 0.0375(13) -0.0020(10) 0.0089(12) 0.0020(12) C81 0.076(4) 0.079(4) 0.205(6) -0.045(4) 0.078(4) -0.024(3) C82 0.056(3) 0.081(4) 0.118(4) -0.015(3) 0.063(3) -0.006(3) N83 0.108(4) 0.071(3) 0.139(4) -0.011(3) 0.079(3) -0.019(3) C85 0.086(4) 0.066(3) 0.099(4) -0.008(3) 0.023(3) 0.002(3) C86 0.080(4) 0.178(6) 0.067(3) 0.007(4) 0.041(3) 0.039(4) N87 0.184(6) 0.360(8) 0.086(4) 0.074(4) 0.077(4) 0.160(6) C91 0.052(3) 0.081(3) 0.105(4) 0.029(3) 0.019(3) -0.001(2) C92 0.056(3) 0.089(4) 0.069(3) 0.033(3) 0.025(3) 0.025(3) N93 0.105(4) 0.150(4) 0.067(3) 0.000(3) 0.002(3) 0.031(3) C95 0.131(8) 0.330(13) 0.253(11) 0.073(10) 0.131(8) 0.072(8) C96 0.171(11) 0.178(9) 0.228(10) 0.079(9) 0.156(8) 0.059(8) N97 0.281(11) 0.133(5) 0.420(12) 0.036(8) 0.305(10) 0.013(6) C100 0.144(12) 0.076(8) 0.172(12) 0.077(8) 0.146(10) 0.065(8) C101 0.099(12) 0.053(7) 0.116(11) -0.007(8) 0.079(9) 0.002(8) N102 0.199(8) 0.117(5) 0.215(8) 0.009(5) 0.131(6) -0.021(5) C105 0.199(8) 0.117(5) 0.215(8) 0.009(5) 0.131(6) -0.021(5) C106 0.063(5) 0.053(4) 0.080(5) -0.033(4) 0.045(4) -0.034(4) N107 0.081(5) 0.084(5) 0.112(5) -0.044(4) 0.042(4) -0.033(4) _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 O72 1.9457(17) . ? Cu1 N41 1.982(2) . ? Cu1 O11 2.0057(17) . ? Cu1 N71 2.024(2) . ? Cu1 O52 2.2272(19) . ? Cu1 Cu2 2.9281(8) . ? Cu2 O52 1.9549(17) . ? Cu2 N61 1.984(2) . ? Cu2 O32 2.0166(17) . ? Cu2 N51 2.017(2) . ? Cu2 O72 2.2251(19) . ? Cu3 O12 1.9425(19) . ? Cu3 O31 1.9459(17) . ? Cu3 O121 1.976(2) . ? Cu3 N1 1.982(2) . ? Cu3 Cu4 3.0151(8) . ? Cu4 O31 1.9338(19) . ? Cu4 O12 1.9545(17) . ? Cu4 O111 1.956(2) . ? Cu4 N21 1.990(2) . ? Cu5 O32 1.9135(18) . ? Cu5 N31 1.964(2) . ? Cu5 O151 1.9849(19) . ? Cu5 O131 1.9894(19) . ? Cu6 O11 1.9154(18) . ? Cu6 N11 1.948(2) . ? Cu6 O141 1.971(2) . ? Cu6 O161 2.003(2) . ? N1 C2 1.349(3) . ? N1 C6 1.354(3) . ? C2 C3 1.390(3) . ? C2 C10 1.550(4) . ? C3 C4 1.391(4) . ? C4 C5 1.383(4) . ? C5 C6 1.387(4) . ? C10 O12 1.391(3) . ? C10 O11 1.413(3) . ? C10 C12 1.530(4) . ? N11 C16 1.351(3) . ? N11 C12 1.352(3) . ? C12 C13 1.389(4) . ? C13 C14 1.390(4) . ? C14 C15 1.381(5) . ? C15 C16 1.374(4) . ? N21 C22 1.352(3) . ? N21 C26 1.353(3) . ? C22 C23 1.390(3) . ? C22 C30 1.556(4) . ? C23 C24 1.392(4) . ? C24 C25 1.377(4) . ? C25 C26 1.380(4) . ? C30 O31 1.394(3) . ? C30 O32 1.412(3) . ? C30 C32 1.530(4) . ? N31 C36 1.352(3) . ? N31 C32 1.354(3) . ? C32 C33 1.388(3) . ? C33 C34 1.391(4) . ? C34 C35 1.384(4) . ? C35 C36 1.382(4) . ? N41 C46 1.351(3) . ? N41 C42 1.352(3) . ? C42 C43 1.382(4) . ? C42 C50 1.548(3) . ? C43 C44 1.386(4) . ? C44 C45 1.386(4) . ? C45 C46 1.386(4) . ? C50 O52 1.398(3) . ? C50 O51 1.430(3) . ? C50 C52 1.553(3) . ? N51 C52 1.347(3) . ? N51 C56 1.366(3) . ? C52 C53 1.390(4) . ? C53 C54 1.395(4) . ? C54 C55 1.379(4) . ? C55 C56 1.382(4) . ? N61 C62 1.341(3) . ? N61 C66 1.357(3) . ? C62 C63 1.386(4) . ? C62 C70 1.548(4) . ? C63 C64 1.378(4) . ? C64 C65 1.380(4) . ? C65 C66 1.382(4) . ? C70 O72 1.397(3) . ? C70 O71 1.428(3) . ? C70 C72 1.552(4) . ? N71 C72 1.345(3) . ? N71 C76 1.361(3) . ? C72 C73 1.394(4) . ? C73 C74 1.385(4) . ? C74 C75 1.389(4) . ? C75 C76 1.372(4) . ? N110 O112 1.223(4) . ? N110 O113 1.235(4) . ? N110 O111 1.310(4) . ? N120 O122 1.225(3) . ? N120 O123 1.242(3) . ? N120 O121 1.312(3) . ? N130 O132 1.224(3) . ? N130 O133 1.256(3) . ? N130 O131 1.304(3) . ? N140 O142 1.234(3) . ? N140 O143 1.254(3) . ? N140 O141 1.301(3) . ? N150 O153 1.226(3) . ? N150 O152 1.253(3) . ? N150 O151 1.312(3) . ? N160 O162 1.231(3) . ? N160 O163 1.249(3) . ? N160 O161 1.307(3) . ? C81 C82 1.472(6) . ? C82 N83 1.119(5) . ? C85 C86 1.432(6) . ? C86 N87 1.111(6) . ? C91 C92 1.464(5) . ? C92 N93 1.117(5) . ? C95 C96 1.464(11) . ? C96 N97 1.350(12) . ? C100 C101 1.413(9) . ? C101 N102 1.142(8) . ? C106 N107 1.099(6) . ? 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 O72 Cu1 N41 162.82(9) . . ? O72 Cu1 O11 98.53(7) . . ? N41 Cu1 O11 93.69(8) . . ? O72 Cu1 N71 82.43(8) . . ? N41 Cu1 N71 98.63(9) . . ? O11 Cu1 N71 130.92(8) . . ? O72 Cu1 O52 84.74(7) . . ? N41 Cu1 O52 79.34(8) . . ? O11 Cu1 O52 113.27(7) . . ? N71 Cu1 O52 115.66(8) . . ? O72 Cu1 Cu2 49.44(5) . . ? N41 Cu1 Cu2 113.39(7) . . ? O11 Cu1 Cu2 130.84(5) . . ? N71 Cu1 Cu2 86.36(6) . . ? O52 Cu1 Cu2 41.87(4) . . ? O52 Cu2 N61 161.90(9) . . ? O52 Cu2 O32 98.53(7) . . ? N61 Cu2 O32 94.31(8) . . ? O52 Cu2 N51 82.13(8) . . ? N61 Cu2 N51 99.48(9) . . ? O32 Cu2 N51 129.37(8) . . ? O52 Cu2 O72 84.59(7) . . ? N61 Cu2 O72 78.55(8) . . ? O32 Cu2 O72 113.98(7) . . ? N51 Cu2 O72 116.45(8) . . ? O52 Cu2 Cu1 49.50(5) . . ? N61 Cu2 Cu1 112.43(7) . . ? O32 Cu2 Cu1 131.26(5) . . ? N51 Cu2 Cu1 86.94(6) . . ? O72 Cu2 Cu1 41.64(4) . . ? O12 Cu3 O31 76.94(7) . . ? O12 Cu3 O121 166.27(8) . . ? O31 Cu3 O121 98.99(7) . . ? O12 Cu3 N1 82.43(9) . . ? O31 Cu3 N1 159.31(9) . . ? O121 Cu3 N1 101.45(9) . . ? O12 Cu3 Cu4 39.46(5) . . ? O31 Cu3 Cu4 38.86(5) . . ? O121 Cu3 Cu4 137.84(5) . . ? N1 Cu3 Cu4 120.61(7) . . ? O31 Cu4 O12 76.94(7) . . ? O31 Cu4 O111 173.41(9) . . ? O12 Cu4 O111 99.58(8) . . ? O31 Cu4 N21 82.19(8) . . ? O12 Cu4 N21 159.10(9) . . ? O111 Cu4 N21 101.08(9) . . ? O31 Cu4 Cu3 39.14(5) . . ? O12 Cu4 Cu3 39.17(5) . . ? O111 Cu4 Cu3 138.36(6) . . ? N21 Cu4 Cu3 120.48(7) . . ? O32 Cu5 N31 84.44(8) . . ? O32 Cu5 O151 167.04(8) . . ? N31 Cu5 O151 95.86(9) . . ? O32 Cu5 O131 92.75(8) . . ? N31 Cu5 O131 168.61(9) . . ? O151 Cu5 O131 89.36(8) . . ? O11 Cu6 N11 84.55(9) . . ? O11 Cu6 O141 93.17(8) . . ? N11 Cu6 O141 167.54(9) . . ? O11 Cu6 O161 161.47(8) . . ? N11 Cu6 O161 95.35(9) . . ? O141 Cu6 O161 90.68(8) . . ? C2 N1 C6 120.2(2) . . ? C2 N1 Cu3 113.52(18) . . ? C6 N1 Cu3 126.2(2) . . ? N1 C2 C3 121.0(3) . . ? N1 C2 C10 116.1(2) . . ? C3 C2 C10 122.8(3) . . ? C2 C3 C4 118.9(3) . . ? C5 C4 C3 119.9(3) . . ? C4 C5 C6 118.8(3) . . ? N1 C6 C5 121.3(3) . . ? O12 C10 O11 111.6(2) . . ? O12 C10 C12 109.2(2) . . ? O11 C10 C12 109.6(2) . . ? O12 C10 C2 107.6(2) . . ? O11 C10 C2 108.3(2) . . ? C12 C10 C2 110.6(2) . . ? C10 O11 Cu6 115.57(15) . . ? C10 O11 Cu1 121.61(16) . . ? Cu6 O11 Cu1 122.62(9) . . ? C10 O12 Cu3 116.90(16) . . ? C10 O12 Cu4 131.61(16) . . ? Cu3 O12 Cu4 101.37(8) . . ? C16 N11 C12 119.9(3) . . ? C16 N11 Cu6 126.2(2) . . ? C12 N11 Cu6 113.73(18) . . ? N11 C12 C13 120.8(3) . . ? N11 C12 C10 115.7(2) . . ? C13 C12 C10 123.5(3) . . ? C12 C13 C14 119.0(3) . . ? C15 C14 C13 119.5(3) . . ? C16 C15 C14 119.2(3) . . ? N11 C16 C15 121.5(3) . . ? C22 N21 C26 119.5(2) . . ? C22 N21 Cu4 113.61(18) . . ? C26 N21 Cu4 126.8(2) . . ? N21 C22 C23 121.1(3) . . ? N21 C22 C30 115.9(2) . . ? C23 C22 C30 122.8(3) . . ? C22 C23 C24 118.7(3) . . ? C25 C24 C23 120.1(3) . . ? C24 C25 C26 118.7(3) . . ? N21 C26 C25 121.9(3) . . ? O31 C30 O32 111.7(2) . . ? O31 C30 C32 108.9(2) . . ? O32 C30 C32 109.6(2) . . ? O31 C30 C22 107.2(2) . . ? O32 C30 C22 108.5(2) . . ? C32 C30 C22 110.9(2) . . ? C30 O31 Cu4 117.69(16) . . ? C30 O31 Cu3 131.80(16) . . ? Cu4 O31 Cu3 102.00(8) . . ? C30 O32 Cu5 115.25(15) . . ? C30 O32 Cu2 120.71(15) . . ? Cu5 O32 Cu2 124.01(9) . . ? C36 N31 C32 119.2(2) . . ? C36 N31 Cu5 127.2(2) . . ? C32 N31 Cu5 113.28(18) . . ? N31 C32 C33 121.4(3) . . ? N31 C32 C30 115.3(2) . . ? C33 C32 C30 123.3(3) . . ? C32 C33 C34 119.3(3) . . ? C35 C34 C33 119.0(3) . . ? C36 C35 C34 119.4(3) . . ? N31 C36 C35 121.7(3) . . ? C46 N41 C42 119.4(2) . . ? C46 N41 Cu1 122.8(2) . . ? C42 N41 Cu1 117.45(17) . . ? N41 C42 C43 121.8(3) . . ? N41 C42 C50 114.1(2) . . ? C43 C42 C50 124.0(3) . . ? C42 C43 C44 119.0(3) . . ? C43 C44 C45 119.2(3) . . ? C46 C45 C44 119.5(3) . . ? N41 C46 C45 121.1(3) . . ? O52 C50 O51 112.1(2) . . ? O52 C50 C42 110.5(2) . . ? O51 C50 C42 104.5(2) . . ? O52 C50 C52 110.2(2) . . ? O51 C50 C52 110.2(2) . . ? C42 C50 C52 109.2(2) . . ? C50 O52 Cu2 116.46(14) . . ? C50 O52 Cu1 105.45(14) . . ? Cu2 O52 Cu1 88.63(7) . . ? C52 N51 C56 118.7(2) . . ? C52 N51 Cu2 113.98(17) . . ? C56 N51 Cu2 126.84(18) . . ? N51 C52 C53 121.8(2) . . ? N51 C52 C50 115.1(2) . . ? C53 C52 C50 123.1(2) . . ? C52 C53 C54 119.1(3) . . ? C55 C54 C53 119.1(3) . . ? C54 C55 C56 119.3(3) . . ? N51 C56 C55 121.9(3) . . ? C62 N61 C66 118.1(2) . . ? C62 N61 Cu2 118.04(18) . . ? C66 N61 Cu2 123.5(2) . . ? N61 C62 C63 122.4(3) . . ? N61 C62 C70 114.6(2) . . ? C63 C62 C70 123.0(3) . . ? C64 C63 C62 119.2(3) . . ? C63 C64 C65 119.0(3) . . ? C64 C65 C66 119.3(3) . . ? N61 C66 C65 122.0(3) . . ? O72 C70 O71 112.2(2) . . ? O72 C70 C62 109.7(2) . . ? O71 C70 C62 106.4(2) . . ? O72 C70 C72 110.3(2) . . ? O71 C70 C72 108.9(2) . . ? C62 C70 C72 109.3(2) . . ? C70 O72 Cu1 115.95(15) . . ? C70 O72 Cu2 106.49(15) . . ? Cu1 O72 Cu2 88.92(7) . . ? C72 N71 C76 118.9(2) . . ? C72 N71 Cu1 112.71(17) . . ? C76 N71 Cu1 127.04(19) . . ? N71 C72 C73 121.6(3) . . ? N71 C72 C70 115.4(2) . . ? C73 C72 C70 122.9(3) . . ? C74 C73 C72 119.1(3) . . ? C73 C74 C75 119.0(3) . . ? C76 C75 C74 119.3(3) . . ? N71 C76 C75 122.0(3) . . ? O112 N110 O113 124.8(4) . . ? O112 N110 O111 117.4(4) . . ? O113 N110 O111 117.7(3) . . ? N110 O111 Cu4 110.4(2) . . ? O122 N120 O123 123.6(3) . . ? O122 N120 O121 118.5(3) . . ? O123 N120 O121 117.9(3) . . ? N120 O121 Cu3 107.02(18) . . ? O132 N130 O133 124.0(3) . . ? O132 N130 O131 119.3(3) . . ? O133 N130 O131 116.7(3) . . ? N130 O131 Cu5 105.70(17) . . ? O142 N140 O143 124.4(3) . . ? O142 N140 O141 118.7(3) . . ? O143 N140 O141 116.9(3) . . ? N140 O141 Cu6 104.55(18) . . ? O153 N150 O152 124.0(3) . . ? O153 N150 O151 118.6(3) . . ? O152 N150 O151 117.4(2) . . ? N150 O151 Cu5 103.26(17) . . ? O162 N160 O163 122.9(3) . . ? O162 N160 O161 119.0(3) . . ? O163 N160 O161 118.1(2) . . ? N160 O161 Cu6 103.71(18) . . ? N83 C82 C81 178.9(6) . . ? N87 C86 C85 176.7(8) . . ? N93 C92 C91 179.4(6) . . ? N97 C96 C95 174.3(12) . . ? N102 C101 C100 166.3(15) . . ? 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 O72 Cu1 Cu2 O52 140.71(9) . . . . ? N41 Cu1 Cu2 O52 -38.30(9) . . . . ? O11 Cu1 Cu2 O52 79.51(10) . . . . ? N71 Cu1 Cu2 O52 -136.14(9) . . . . ? O72 Cu1 Cu2 N61 -38.03(9) . . . . ? N41 Cu1 Cu2 N61 142.96(10) . . . . ? O11 Cu1 Cu2 N61 -99.22(10) . . . . ? N71 Cu1 Cu2 N61 45.12(9) . . . . ? O52 Cu1 Cu2 N61 -178.74(9) . . . . ? O72 Cu1 Cu2 O32 80.03(9) . . . . ? N41 Cu1 Cu2 O32 -98.99(9) . . . . ? O11 Cu1 Cu2 O32 18.83(10) . . . . ? N71 Cu1 Cu2 O32 163.17(9) . . . . ? O52 Cu1 Cu2 O32 -60.69(9) . . . . ? O72 Cu1 Cu2 N51 -137.02(9) . . . . ? N41 Cu1 Cu2 N51 43.96(9) . . . . ? O11 Cu1 Cu2 N51 161.78(9) . . . . ? N71 Cu1 Cu2 N51 -53.88(9) . . . . ? O52 Cu1 Cu2 N51 82.26(9) . . . . ? N41 Cu1 Cu2 O72 -179.02(9) . . . . ? O11 Cu1 Cu2 O72 -61.20(9) . . . . ? N71 Cu1 Cu2 O72 83.15(9) . . . . ? O52 Cu1 Cu2 O72 -140.71(9) . . . . ? O12 Cu3 Cu4 O31 160.26(11) . . . . ? O121 Cu3 Cu4 O31 0.93(12) . . . . ? N1 Cu3 Cu4 O31 176.60(11) . . . . ? O31 Cu3 Cu4 O12 -160.26(11) . . . . ? O121 Cu3 Cu4 O12 -159.33(12) . . . . ? N1 Cu3 Cu4 O12 16.34(11) . . . . ? O12 Cu3 Cu4 O111 -10.31(13) . . . . ? O31 Cu3 Cu4 O111 -170.57(13) . . . . ? O121 Cu3 Cu4 O111 -169.65(13) . . . . ? N1 Cu3 Cu4 O111 6.02(12) . . . . ? O12 Cu3 Cu4 N21 173.61(11) . . . . ? O31 Cu3 Cu4 N21 13.35(11) . . . . ? O121 Cu3 Cu4 N21 14.28(11) . . . . ? N1 Cu3 Cu4 N21 -170.05(10) . . . . ? O12 Cu3 N1 C2 6.95(17) . . . . ? O31 Cu3 N1 C2 2.6(3) . . . . ? O121 Cu3 N1 C2 173.60(17) . . . . ? Cu4 Cu3 N1 C2 -3.4(2) . . . . ? O12 Cu3 N1 C6 -175.9(2) . . . . ? O31 Cu3 N1 C6 179.7(2) . . . . ? O121 Cu3 N1 C6 -9.3(2) . . . . ? Cu4 Cu3 N1 C6 173.69(18) . . . . ? C6 N1 C2 C3 1.6(4) . . . . ? Cu3 N1 C2 C3 178.93(19) . . . . ? C6 N1 C2 C10 -175.0(2) . . . . ? Cu3 N1 C2 C10 2.4(3) . . . . ? N1 C2 C3 C4 -1.6(4) . . . . ? C10 C2 C3 C4 174.8(2) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C6 1.7(4) . . . . ? C2 N1 C6 C5 0.1(4) . . . . ? Cu3 N1 C6 C5 -176.88(19) . . . . ? C4 C5 C6 N1 -1.7(4) . . . . ? N1 C2 C10 O12 -14.4(3) . . . . ? C3 C2 C10 O12 169.1(2) . . . . ? N1 C2 C10 O11 106.3(2) . . . . ? C3 C2 C10 O11 -70.2(3) . . . . ? N1 C2 C10 C12 -133.6(2) . . . . ? C3 C2 C10 C12 49.9(3) . . . . ? O12 C10 O11 Cu6 -131.73(18) . . . . ? C12 C10 O11 Cu6 -10.6(2) . . . . ? C2 C10 O11 Cu6 110.0(2) . . . . ? O12 C10 O11 Cu1 43.2(3) . . . . ? C12 C10 O11 Cu1 164.31(15) . . . . ? C2 C10 O11 Cu1 -75.0(2) . . . . ? N11 Cu6 O11 C10 7.61(16) . . . . ? O141 Cu6 O11 C10 175.32(16) . . . . ? O161 Cu6 O11 C10 -83.0(3) . . . . ? N11 Cu6 O11 Cu1 -167.28(11) . . . . ? O141 Cu6 O11 Cu1 0.43(11) . . . . ? O161 Cu6 O11 Cu1 102.1(2) . . . . ? O72 Cu1 O11 C10 -78.75(17) . . . . ? N41 Cu1 O11 C10 89.14(18) . . . . ? N71 Cu1 O11 C10 -166.09(16) . . . . ? O52 Cu1 O11 C10 9.16(19) . . . . ? Cu2 Cu1 O11 C10 -36.43(19) . . . . ? O72 Cu1 O11 Cu6 95.84(10) . . . . ? N41 Cu1 O11 Cu6 -96.28(11) . . . . ? N71 Cu1 O11 Cu6 8.49(15) . . . . ? O52 Cu1 O11 Cu6 -176.25(8) . . . . ? Cu2 Cu1 O11 Cu6 138.15(7) . . . . ? O11 C10 O12 Cu3 -98.3(2) . . . . ? C12 C10 O12 Cu3 140.45(18) . . . . ? C2 C10 O12 Cu3 20.4(2) . . . . ? O11 C10 O12 Cu4 40.0(3) . . . . ? C12 C10 O12 Cu4 -81.3(3) . . . . ? C2 C10 O12 Cu4 158.68(16) . . . . ? O31 Cu3 O12 C10 162.06(18) . . . . ? O121 Cu3 O12 C10 -123.8(3) . . . . ? N1 Cu3 O12 C10 -16.37(17) . . . . ? Cu4 Cu3 O12 C10 149.5(2) . . . . ? O31 Cu3 O12 Cu4 12.56(7) . . . . ? O121 Cu3 O12 Cu4 86.7(3) . . . . ? N1 Cu3 O12 Cu4 -165.86(9) . . . . ? O31 Cu4 O12 C10 -155.4(2) . . . . ? O111 Cu4 O12 C10 30.3(2) . . . . ? N21 Cu4 O12 C10 -158.3(2) . . . . ? Cu3 Cu4 O12 C10 -142.7(2) . . . . ? O31 Cu4 O12 Cu3 -12.64(7) . . . . ? O111 Cu4 O12 Cu3 173.07(9) . . . . ? N21 Cu4 O12 Cu3 -15.6(3) . . . . ? O11 Cu6 N11 C16 173.8(2) . . . . ? O141 Cu6 N11 C16 93.8(5) . . . . ? O161 Cu6 N11 C16 -24.8(2) . . . . ? O11 Cu6 N11 C12 -2.18(18) . . . . ? O141 Cu6 N11 C12 -82.1(5) . . . . ? O161 Cu6 N11 C12 159.21(19) . . . . ? C16 N11 C12 C13 1.3(4) . . . . ? Cu6 N11 C12 C13 177.5(2) . . . . ? C16 N11 C12 C10 -179.5(2) . . . . ? Cu6 N11 C12 C10 -3.2(3) . . . . ? O12 C10 C12 N11 131.4(2) . . . . ? O11 C10 C12 N11 8.9(3) . . . . ? C2 C10 C12 N11 -110.4(3) . . . . ? O12 C10 C12 C13 -49.4(3) . . . . ? O11 C10 C12 C13 -171.9(2) . . . . ? C2 C10 C12 C13 68.8(3) . . . . ? N11 C12 C13 C14 -0.3(4) . . . . ? C10 C12 C13 C14 -179.4(3) . . . . ? C12 C13 C14 C15 -1.4(5) . . . . ? C13 C14 C15 C16 2.0(5) . . . . ? C12 N11 C16 C15 -0.7(5) . . . . ? Cu6 N11 C16 C15 -176.4(2) . . . . ? C14 C15 C16 N11 -0.9(5) . . . . ? O31 Cu4 N21 C22 7.64(17) . . . . ? O12 Cu4 N21 C22 10.5(3) . . . . ? O111 Cu4 N21 C22 -178.17(17) . . . . ? Cu3 Cu4 N21 C22 -0.8(2) . . . . ? O31 Cu4 N21 C26 -175.9(2) . . . . ? O12 Cu4 N21 C26 -173.0(2) . . . . ? O111 Cu4 N21 C26 -1.7(2) . . . . ? Cu3 Cu4 N21 C26 175.62(19) . . . . ? C26 N21 C22 C23 0.8(4) . . . . ? Cu4 N21 C22 C23 177.54(19) . . . . ? C26 N21 C22 C30 -175.4(2) . . . . ? Cu4 N21 C22 C30 1.3(3) . . . . ? N21 C22 C23 C24 -0.8(4) . . . . ? C30 C22 C23 C24 175.2(2) . . . . ? C22 C23 C24 C25 -0.2(4) . . . . ? C23 C24 C25 C26 1.1(4) . . . . ? C22 N21 C26 C25 0.1(4) . . . . ? Cu4 N21 C26 C25 -176.1(2) . . . . ? C24 C25 C26 N21 -1.1(4) . . . . ? N21 C22 C30 O31 -13.3(3) . . . . ? C23 C22 C30 O31 170.5(2) . . . . ? N21 C22 C30 O32 107.4(2) . . . . ? C23 C22 C30 O32 -68.8(3) . . . . ? N21 C22 C30 C32 -132.1(2) . . . . ? C23 C22 C30 C32 51.7(3) . . . . ? O32 C30 O31 Cu4 -98.5(2) . . . . ? C32 C30 O31 Cu4 140.24(17) . . . . ? C22 C30 O31 Cu4 20.2(2) . . . . ? O32 C30 O31 Cu3 43.1(3) . . . . ? C32 C30 O31 Cu3 -78.1(3) . . . . ? C22 C30 O31 Cu3 161.82(15) . . . . ? O12 Cu4 O31 C30 164.44(18) . . . . ? O111 Cu4 O31 C30 -136.8(6) . . . . ? N21 Cu4 O31 C30 -16.63(17) . . . . ? Cu3 Cu4 O31 C30 151.8(2) . . . . ? O12 Cu4 O31 Cu3 12.65(7) . . . . ? O111 Cu4 O31 Cu3 71.4(7) . . . . ? N21 Cu4 O31 Cu3 -168.41(9) . . . . ? O12 Cu3 O31 C30 -158.6(2) . . . . ? O121 Cu3 O31 C30 34.8(2) . . . . ? N1 Cu3 O31 C30 -154.1(2) . . . . ? Cu4 Cu3 O31 C30 -145.8(2) . . . . ? O12 Cu3 O31 Cu4 -12.73(7) . . . . ? O121 Cu3 O31 Cu4 -179.37(8) . . . . ? N1 Cu3 O31 Cu4 -8.3(3) . . . . ? O31 C30 O32 Cu5 -136.24(17) . . . . ? C32 C30 O32 Cu5 -15.5(2) . . . . ? C22 C30 O32 Cu5 105.8(2) . . . . ? O31 C30 O32 Cu2 41.6(3) . . . . ? C32 C30 O32 Cu2 162.38(14) . . . . ? C22 C30 O32 Cu2 -76.4(2) . . . . ? N31 Cu5 O32 C30 10.17(16) . . . . ? O151 Cu5 O32 C30 -81.8(4) . . . . ? O131 Cu5 O32 C30 179.10(16) . . . . ? N31 Cu5 O32 Cu2 -167.59(11) . . . . ? O151 Cu5 O32 Cu2 100.5(3) . . . . ? O131 Cu5 O32 Cu2 1.34(11) . . . . ? O52 Cu2 O32 C30 -77.85(17) . . . . ? N61 Cu2 O32 C30 89.36(18) . . . . ? N51 Cu2 O32 C30 -164.64(16) . . . . ? O72 Cu2 O32 C30 9.99(18) . . . . ? Cu1 Cu2 O32 C30 -35.75(19) . . . . ? O52 Cu2 O32 Cu5 99.79(10) . . . . ? N61 Cu2 O32 Cu5 -93.00(11) . . . . ? N51 Cu2 O32 Cu5 13.00(15) . . . . ? O72 Cu2 O32 Cu5 -172.37(8) . . . . ? Cu1 Cu2 O32 Cu5 141.89(7) . . . . ? O32 Cu5 N31 C36 171.8(2) . . . . ? O151 Cu5 N31 C36 -21.2(2) . . . . ? O131 Cu5 N31 C36 95.6(5) . . . . ? O32 Cu5 N31 C32 -1.58(17) . . . . ? O151 Cu5 N31 C32 165.40(18) . . . . ? O131 Cu5 N31 C32 -77.7(5) . . . . ? C36 N31 C32 C33 -0.2(4) . . . . ? Cu5 N31 C32 C33 173.79(19) . . . . ? C36 N31 C32 C30 179.4(2) . . . . ? Cu5 N31 C32 C30 -6.6(3) . . . . ? O31 C30 C32 N31 136.7(2) . . . . ? O32 C30 C32 N31 14.3(3) . . . . ? C22 C30 C32 N31 -105.5(3) . . . . ? O31 C30 C32 C33 -43.7(3) . . . . ? O32 C30 C32 C33 -166.2(2) . . . . ? C22 C30 C32 C33 74.1(3) . . . . ? N31 C32 C33 C34 1.1(4) . . . . ? C30 C32 C33 C34 -178.4(2) . . . . ? C32 C33 C34 C35 -0.7(4) . . . . ? C33 C34 C35 C36 -0.6(4) . . . . ? C32 N31 C36 C35 -1.2(4) . . . . ? Cu5 N31 C36 C35 -174.2(2) . . . . ? C34 C35 C36 N31 1.6(4) . . . . ? O72 Cu1 N41 C46 -174.2(2) . . . . ? O11 Cu1 N41 C46 50.4(2) . . . . ? N71 Cu1 N41 C46 -81.9(2) . . . . ? O52 Cu1 N41 C46 163.4(2) . . . . ? Cu2 Cu1 N41 C46 -171.69(18) . . . . ? O72 Cu1 N41 C42 12.1(4) . . . . ? O11 Cu1 N41 C42 -123.25(18) . . . . ? N71 Cu1 N41 C42 104.40(19) . . . . ? O52 Cu1 N41 C42 -10.25(17) . . . . ? Cu2 Cu1 N41 C42 14.6(2) . . . . ? C46 N41 C42 C43 -0.2(4) . . . . ? Cu1 N41 C42 C43 173.7(2) . . . . ? C46 N41 C42 C50 178.1(2) . . . . ? Cu1 N41 C42 C50 -8.0(3) . . . . ? N41 C42 C43 C44 -0.9(4) . . . . ? C50 C42 C43 C44 -179.0(2) . . . . ? C42 C43 C44 C45 1.5(4) . . . . ? C43 C44 C45 C46 -1.0(4) . . . . ? C42 N41 C46 C45 0.7(4) . . . . ? Cu1 N41 C46 C45 -172.80(19) . . . . ? C44 C45 C46 N41 -0.1(4) . . . . ? N41 C42 C50 O52 33.3(3) . . . . ? C43 C42 C50 O52 -148.4(2) . . . . ? N41 C42 C50 O51 154.1(2) . . . . ? C43 C42 C50 O51 -27.7(3) . . . . ? N41 C42 C50 C52 -88.0(3) . . . . ? C43 C42 C50 C52 90.2(3) . . . . ? O51 C50 O52 Cu2 109.57(19) . . . . ? C42 C50 O52 Cu2 -134.28(17) . . . . ? C52 C50 O52 Cu2 -13.5(3) . . . . ? O51 C50 O52 Cu1 -154.12(16) . . . . ? C42 C50 O52 Cu1 -38.0(2) . . . . ? C52 C50 O52 Cu1 82.8(2) . . . . ? N61 Cu2 O52 C50 110.4(3) . . . . ? O32 Cu2 O52 C50 -114.92(17) . . . . ? N51 Cu2 O52 C50 13.90(17) . . . . ? O72 Cu2 O52 C50 131.60(17) . . . . ? Cu1 Cu2 O52 C50 106.60(18) . . . . ? N61 Cu2 O52 Cu1 3.8(3) . . . . ? O32 Cu2 O52 Cu1 138.48(6) . . . . ? N51 Cu2 O52 Cu1 -92.70(8) . . . . ? O72 Cu2 O52 Cu1 25.00(6) . . . . ? O72 Cu1 O52 C50 -146.01(15) . . . . ? N41 Cu1 O52 C50 27.51(15) . . . . ? O11 Cu1 O52 C50 116.95(14) . . . . ? N71 Cu1 O52 C50 -67.02(16) . . . . ? Cu2 Cu1 O52 C50 -117.12(16) . . . . ? O72 Cu1 O52 Cu2 -28.89(7) . . . . ? N41 Cu1 O52 Cu2 144.63(8) . . . . ? O11 Cu1 O52 Cu2 -125.93(7) . . . . ? N71 Cu1 O52 Cu2 50.10(9) . . . . ? O52 Cu2 N51 C52 -11.08(19) . . . . ? N61 Cu2 N51 C52 -172.84(19) . . . . ? O32 Cu2 N51 C52 83.5(2) . . . . ? O72 Cu2 N51 C52 -90.99(19) . . . . ? Cu1 Cu2 N51 C52 -60.60(19) . . . . ? O52 Cu2 N51 C56 176.7(2) . . . . ? N61 Cu2 N51 C56 14.9(2) . . . . ? O32 Cu2 N51 C56 -88.7(2) . . . . ? O72 Cu2 N51 C56 96.8(2) . . . . ? Cu1 Cu2 N51 C56 127.2(2) . . . . ? C56 N51 C52 C53 -0.1(4) . . . . ? Cu2 N51 C52 C53 -173.0(2) . . . . ? C56 N51 C52 C50 179.6(2) . . . . ? Cu2 N51 C52 C50 6.7(3) . . . . ? O52 C50 C52 N51 4.1(3) . . . . ? O51 C50 C52 N51 -120.1(2) . . . . ? C42 C50 C52 N51 125.7(3) . . . . ? O52 C50 C52 C53 -176.2(2) . . . . ? O51 C50 C52 C53 59.6(3) . . . . ? C42 C50 C52 C53 -54.7(3) . . . . ? N51 C52 C53 C54 0.8(4) . . . . ? C50 C52 C53 C54 -178.9(3) . . . . ? C52 C53 C54 C55 -1.7(4) . . . . ? C53 C54 C55 C56 1.9(5) . . . . ? C52 N51 C56 C55 0.3(4) . . . . ? Cu2 N51 C56 C55 172.2(2) . . . . ? C54 C55 C56 N51 -1.2(5) . . . . ? O52 Cu2 N61 C62 10.7(4) . . . . ? O32 Cu2 N61 C62 -124.49(19) . . . . ? N51 Cu2 N61 C62 104.40(19) . . . . ? O72 Cu2 N61 C62 -10.88(18) . . . . ? Cu1 Cu2 N61 C62 13.8(2) . . . . ? O52 Cu2 N61 C66 -176.0(2) . . . . ? O32 Cu2 N61 C66 48.8(2) . . . . ? N51 Cu2 N61 C66 -82.3(2) . . . . ? O72 Cu2 N61 C66 162.4(2) . . . . ? Cu1 Cu2 N61 C66 -172.92(18) . . . . ? C66 N61 C62 C63 -0.3(4) . . . . ? Cu2 N61 C62 C63 173.3(2) . . . . ? C66 N61 C62 C70 179.4(2) . . . . ? Cu2 N61 C62 C70 -7.0(3) . . . . ? N61 C62 C63 C64 -0.4(4) . . . . ? C70 C62 C63 C64 179.9(3) . . . . ? C62 C63 C64 C65 0.4(4) . . . . ? C63 C64 C65 C66 0.3(4) . . . . ? C62 N61 C66 C65 1.1(4) . . . . ? Cu2 N61 C66 C65 -172.2(2) . . . . ? C64 C65 C66 N61 -1.1(4) . . . . ? N61 C62 C70 O72 31.9(3) . . . . ? C63 C62 C70 O72 -148.4(3) . . . . ? N61 C62 C70 O71 153.5(2) . . . . ? C63 C62 C70 O71 -26.8(3) . . . . ? N61 C62 C70 C72 -89.2(3) . . . . ? C63 C62 C70 C72 90.6(3) . . . . ? O71 C70 O72 Cu1 107.6(2) . . . . ? C62 C70 O72 Cu1 -134.39(17) . . . . ? C72 C70 O72 Cu1 -14.0(3) . . . . ? O71 C70 O72 Cu2 -155.36(17) . . . . ? C62 C70 O72 Cu2 -37.4(2) . . . . ? C72 C70 O72 Cu2 83.1(2) . . . . ? N41 Cu1 O72 C70 110.9(3) . . . . ? O11 Cu1 O72 C70 -114.24(18) . . . . ? N71 Cu1 O72 C70 16.16(18) . . . . ? O52 Cu1 O72 C70 132.96(17) . . . . ? Cu2 Cu1 O72 C70 107.85(18) . . . . ? N41 Cu1 O72 Cu2 3.1(3) . . . . ? O11 Cu1 O72 Cu2 137.91(6) . . . . ? N71 Cu1 O72 Cu2 -91.69(8) . . . . ? O52 Cu1 O72 Cu2 25.11(6) . . . . ? O52 Cu2 O72 C70 -145.73(15) . . . . ? N61 Cu2 O72 C70 27.68(15) . . . . ? O32 Cu2 O72 C70 117.32(15) . . . . ? N51 Cu2 O72 C70 -67.31(16) . . . . ? Cu1 Cu2 O72 C70 -116.80(16) . . . . ? O52 Cu2 O72 Cu1 -28.93(7) . . . . ? N61 Cu2 O72 Cu1 144.48(8) . . . . ? O32 Cu2 O72 Cu1 -125.87(7) . . . . ? N51 Cu2 O72 Cu1 49.49(9) . . . . ? O72 Cu1 N71 C72 -14.93(19) . . . . ? N41 Cu1 N71 C72 -177.60(19) . . . . ? O11 Cu1 N71 C72 79.8(2) . . . . ? O52 Cu1 N71 C72 -95.3(2) . . . . ? Cu2 Cu1 N71 C72 -64.48(19) . . . . ? O72 Cu1 N71 C76 178.8(2) . . . . ? N41 Cu1 N71 C76 16.2(2) . . . . ? O11 Cu1 N71 C76 -86.4(3) . . . . ? O52 Cu1 N71 C76 98.4(2) . . . . ? Cu2 Cu1 N71 C76 129.3(2) . . . . ? C76 N71 C72 C73 1.2(4) . . . . ? Cu1 N71 C72 C73 -166.3(2) . . . . ? C76 N71 C72 C70 178.8(2) . . . . ? Cu1 N71 C72 C70 11.3(3) . . . . ? O72 C70 C72 N71 1.2(3) . . . . ? O71 C70 C72 N71 -122.3(3) . . . . ? C62 C70 C72 N71 121.9(3) . . . . ? O72 C70 C72 C73 178.7(3) . . . . ? O71 C70 C72 C73 55.2(4) . . . . ? C62 C70 C72 C73 -60.6(4) . . . . ? N71 C72 C73 C74 0.3(5) . . . . ? C70 C72 C73 C74 -177.1(3) . . . . ? C72 C73 C74 C75 -1.4(5) . . . . ? C73 C74 C75 C76 1.2(5) . . . . ? C72 N71 C76 C75 -1.4(4) . . . . ? Cu1 N71 C76 C75 164.0(2) . . . . ? C74 C75 C76 N71 0.3(5) . . . . ? O112 N110 O111 Cu4 -168.3(2) . . . . ? O113 N110 O111 Cu4 12.4(4) . . . . ? O31 Cu4 O111 N110 23.3(8) . . . . ? O12 Cu4 O111 N110 80.89(19) . . . . ? N21 Cu4 O111 N110 -95.98(19) . . . . ? Cu3 Cu4 O111 N110 87.47(19) . . . . ? O122 N120 O121 Cu3 -171.9(2) . . . . ? O123 N120 O121 Cu3 7.9(3) . . . . ? O12 Cu3 O121 N120 13.9(4) . . . . ? O31 Cu3 O121 N120 85.43(16) . . . . ? N1 Cu3 O121 N120 -91.36(16) . . . . ? Cu4 Cu3 O121 N120 84.84(16) . . . . ? O132 N130 O131 Cu5 -167.4(2) . . . . ? O133 N130 O131 Cu5 14.1(3) . . . . ? O32 Cu5 O131 N130 -108.44(17) . . . . ? N31 Cu5 O131 N130 -33.1(6) . . . . ? O151 Cu5 O131 N130 84.35(17) . . . . ? O142 N140 O141 Cu6 -166.8(2) . . . . ? O143 N140 O141 Cu6 12.7(3) . . . . ? O11 Cu6 O141 N140 -121.82(17) . . . . ? N11 Cu6 O141 N140 -42.8(5) . . . . ? O161 Cu6 O141 N140 76.31(18) . . . . ? O153 N150 O151 Cu5 -175.9(2) . . . . ? O152 N150 O151 Cu5 3.7(3) . . . . ? O32 Cu5 O151 N150 -18.3(4) . . . . ? N31 Cu5 O151 N150 -108.92(16) . . . . ? O131 Cu5 O151 N150 81.23(16) . . . . ? O162 N160 O161 Cu6 -177.4(2) . . . . ? O163 N160 O161 Cu6 2.3(3) . . . . ? O11 Cu6 O161 N160 -16.1(3) . . . . ? N11 Cu6 O161 N160 -104.90(17) . . . . ? O141 Cu6 O161 N160 86.01(17) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.432 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.064 #===END data_Compound-12 _database_code_CSD 216636 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 12 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 Ag N5 O3' _chemical_formula_weight 508.28 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 15.948(6) _cell_length_b 11.544(5) _cell_length_c 13.420(5) _cell_angle_alpha 90.00 _cell_angle_beta 121.083(5) _cell_angle_gamma 90.00 _cell_volume 2116.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.924407 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst., (1995) A 51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 13344 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3870 _reflns_number_gt 3445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0189P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.63(2) _refine_ls_number_reflns 3870 _refine_ls_number_parameters 281 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0407 _refine_ls_wR_factor_gt 0.0396 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 Ag1 Ag 0.348977(16) 0.556294(16) 0.359937(17) 0.03215(6) Uani 1 1 d . . . C1 C 0.3392(2) 0.4254(3) 0.5912(3) 0.0265(8) Uani 1 1 d . . . H1A H 0.3295 0.3862 0.6510 0.032 Uiso 1 1 calc R . . C2 C 0.4015(3) 0.5347(3) 0.6492(3) 0.0263(7) Uani 1 1 d . . . H2A H 0.4212 0.5663 0.5949 0.032 Uiso 1 1 calc R . . N11 N 0.2311(2) 0.5307(3) 0.4092(3) 0.0320(8) Uani 1 1 d . . . C12 C 0.2388(3) 0.4553(3) 0.4904(3) 0.0280(7) Uani 1 1 d . . . C13 C 0.1558(2) 0.4044(3) 0.4813(3) 0.0395(8) Uani 1 1 d . . . H13A H 0.1622 0.3500 0.5380 0.047 Uiso 1 1 calc R . . C14 C 0.0658(3) 0.4332(3) 0.3912(4) 0.0508(10) Uani 1 1 d . . . H14A H 0.0090 0.3980 0.3836 0.061 Uiso 1 1 calc R . . C15 C 0.0572(3) 0.5138(4) 0.3105(4) 0.0475(10) Uani 1 1 d . . . H15A H -0.0053 0.5370 0.2483 0.057 Uiso 1 1 calc R . . C16 C 0.1421(3) 0.5602(3) 0.3227(4) 0.0439(11) Uani 1 1 d . . . H16A H 0.1367 0.6152 0.2670 0.053 Uiso 1 1 calc R . . N21 N 0.4393(2) 0.3844(3) 0.5062(3) 0.0297(7) Uani 1 1 d . . . C22 C 0.3930(2) 0.3404(3) 0.5575(3) 0.0267(7) Uani 1 1 d . . . C23 C 0.3919(3) 0.2232(3) 0.5774(3) 0.0413(10) Uani 1 1 d . . . H23A H 0.3589 0.1943 0.6144 0.050 Uiso 1 1 calc R . . C24 C 0.4398(3) 0.1486(3) 0.5422(3) 0.0517(11) Uani 1 1 d . . . H24A H 0.4386 0.0674 0.5530 0.062 Uiso 1 1 calc R . . C25 C 0.4891(3) 0.1930(3) 0.4917(3) 0.0450(10) Uani 1 1 d . . . H25A H 0.5233 0.1437 0.4679 0.054 Uiso 1 1 calc R . . C26 C 0.4875(3) 0.3111(3) 0.4766(3) 0.0374(9) Uani 1 1 d . . . H26A H 0.5227 0.3422 0.4433 0.045 Uiso 1 1 calc R . . N31 N 0.4857(3) 0.4376(2) 0.8385(3) 0.0319(9) Uani 1 1 d . . . C32 C 0.4944(2) 0.5011(3) 0.7601(3) 0.0278(7) Uani 1 1 d . . . C33 C 0.5868(3) 0.5321(3) 0.7808(3) 0.0425(9) Uani 1 1 d . . . H33A H 0.5927 0.5749 0.7243 0.051 Uiso 1 1 calc R . . C34 C 0.6688(3) 0.5003(4) 0.8831(4) 0.0533(11) Uani 1 1 d . . . H34A H 0.7319 0.5221 0.8984 0.064 Uiso 1 1 calc R . . C35 C 0.6596(3) 0.4362(3) 0.9640(3) 0.0484(9) Uani 1 1 d . . . H35A H 0.7155 0.4137 1.0356 0.058 Uiso 1 1 calc R . . C36 C 0.5666(3) 0.4062(4) 0.9373(3) 0.0399(10) Uani 1 1 d . . . H36A H 0.5596 0.3610 0.9917 0.048 Uiso 1 1 calc R . . N41 N 0.2930(2) 0.6013(3) 0.7150(3) 0.0316(7) Uani 1 1 d . . . C42 C 0.3463(2) 0.6301(3) 0.6692(3) 0.0250(7) Uani 1 1 d . . . C43 C 0.3542(2) 0.7445(3) 0.6410(3) 0.0392(8) Uani 1 1 d . . . H43A H 0.3930 0.7631 0.6083 0.047 Uiso 1 1 calc R . . C44 C 0.3046(3) 0.8297(3) 0.6617(3) 0.0432(10) Uani 1 1 d . . . H44A H 0.3097 0.9082 0.6443 0.052 Uiso 1 1 calc R . . C45 C 0.2479(3) 0.8011(3) 0.7074(3) 0.0413(9) Uani 1 1 d . . . H45A H 0.2122 0.8586 0.7208 0.050 Uiso 1 1 calc R . . C46 C 0.2440(3) 0.6869(3) 0.7333(4) 0.0390(9) Uani 1 1 d . . . H46A H 0.2052 0.6668 0.7656 0.047 Uiso 1 1 calc R . . N10 N 0.3143(3) 0.8204(3) 0.3026(4) 0.0389(9) Uani 1 1 d . . . O11 O 0.3766(3) 0.7838(3) 0.4001(3) 0.0612(10) Uani 1 1 d . . . O12 O 0.2505(2) 0.7525(2) 0.2313(2) 0.0594(7) Uani 1 1 d . . . O13 O 0.31663(19) 0.92144(19) 0.2738(2) 0.0628(7) 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 Ag1 0.03776(12) 0.03280(10) 0.03174(10) 0.00174(18) 0.02210(9) 0.00253(18) C1 0.029(2) 0.0270(18) 0.0241(17) -0.0001(13) 0.0139(16) -0.0025(13) C2 0.033(2) 0.0238(17) 0.0249(18) -0.0032(14) 0.0171(17) -0.0055(14) N11 0.0270(18) 0.0385(17) 0.0282(18) 0.0013(14) 0.0125(15) 0.0057(14) C12 0.032(2) 0.0260(18) 0.0312(19) -0.0049(15) 0.0203(17) -0.0014(15) C13 0.036(2) 0.0375(18) 0.047(2) -0.0066(16) 0.0226(18) -0.0056(16) C14 0.039(3) 0.050(3) 0.063(3) -0.014(2) 0.026(2) -0.0078(19) C15 0.029(2) 0.056(3) 0.047(3) -0.007(2) 0.012(2) 0.006(2) C16 0.043(3) 0.050(3) 0.039(3) 0.0046(18) 0.022(2) 0.0117(19) N21 0.0365(18) 0.0318(17) 0.0288(15) 0.0060(13) 0.0225(14) 0.0079(15) C22 0.0274(19) 0.0264(19) 0.0206(15) -0.0048(12) 0.0084(15) 0.0008(14) C23 0.060(3) 0.025(2) 0.050(2) 0.0022(17) 0.036(2) 0.0017(19) C24 0.073(3) 0.026(2) 0.057(3) 0.0055(18) 0.034(2) 0.009(2) C25 0.055(3) 0.042(2) 0.037(2) 0.0019(15) 0.0230(19) 0.0150(18) C26 0.037(2) 0.043(2) 0.037(2) 0.0062(15) 0.0226(18) 0.0091(17) N31 0.033(2) 0.0302(17) 0.031(2) 0.0019(13) 0.0153(17) 0.0055(13) C32 0.0292(19) 0.0266(18) 0.0267(18) -0.0082(14) 0.0137(16) -0.0003(14) C33 0.042(3) 0.052(2) 0.037(2) -0.0079(18) 0.023(2) -0.007(2) C34 0.027(2) 0.074(3) 0.054(3) -0.009(2) 0.017(2) -0.009(2) C35 0.035(2) 0.059(3) 0.040(2) 0.0008(18) 0.0109(18) 0.0059(18) C36 0.036(2) 0.038(2) 0.036(2) 0.0021(16) 0.0115(18) 0.0074(17) N41 0.0301(17) 0.0345(16) 0.0329(16) -0.0010(12) 0.0183(15) 0.0053(14) C42 0.029(2) 0.0244(18) 0.0168(15) 0.0005(13) 0.0081(15) 0.0022(14) C43 0.044(2) 0.0347(19) 0.0377(19) -0.0029(15) 0.0200(18) -0.0035(16) C44 0.046(2) 0.027(2) 0.047(2) 0.0019(17) 0.0175(19) 0.0044(18) C45 0.043(2) 0.035(2) 0.038(2) -0.0010(17) 0.0155(18) 0.0111(19) C46 0.036(2) 0.044(2) 0.039(2) 0.0029(17) 0.0208(18) 0.0065(18) N10 0.046(2) 0.0335(19) 0.055(2) 0.0026(16) 0.0387(19) 0.0073(15) O11 0.071(3) 0.0566(19) 0.055(2) 0.0196(16) 0.0319(18) 0.0060(17) O12 0.0739(19) 0.0475(16) 0.0665(18) -0.0125(13) 0.0432(16) -0.0106(14) O13 0.0678(18) 0.0322(14) 0.0881(19) 0.0188(12) 0.0400(16) 0.0048(12) _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 Ag1 N11 2.312(4) . ? Ag1 N31 2.343(4) 2_564 ? Ag1 N41 2.469(3) 2_564 ? Ag1 N21 2.635(3) . ? C1 C12 1.508(5) . ? C1 C22 1.518(4) . ? C1 C2 1.545(4) . ? C2 C32 1.511(4) . ? C2 C42 1.517(4) . ? N11 C16 1.333(5) . ? N11 C12 1.350(4) . ? C12 C13 1.395(5) . ? C13 C14 1.357(5) . ? C14 C15 1.379(6) . ? C15 C16 1.384(6) . ? N21 C26 1.335(4) . ? N21 C22 1.342(4) . ? C22 C23 1.381(4) . ? C23 C24 1.386(5) . ? C24 C25 1.376(5) . ? C25 C26 1.377(5) . ? N31 C36 1.337(5) . ? N31 C32 1.347(5) . ? N31 Ag1 2.343(4) 2_565 ? C32 C33 1.399(5) . ? C33 C34 1.370(5) . ? C34 C35 1.383(6) . ? C35 C36 1.378(5) . ? N41 C42 1.324(4) . ? N41 C46 1.359(4) . ? N41 Ag1 2.469(3) 2_565 ? C42 C43 1.397(4) . ? C43 C44 1.378(5) . ? C44 C45 1.370(6) . ? C45 C46 1.372(5) . ? N10 O13 1.235(4) . ? N10 O11 1.240(3) . ? N10 O12 1.249(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 N11 Ag1 N31 170.04(12) . 2_564 ? N11 Ag1 N41 96.59(10) . 2_564 ? N31 Ag1 N41 84.62(10) 2_564 2_564 ? N11 Ag1 N21 84.44(10) . . ? N31 Ag1 N21 85.92(10) 2_564 . ? N41 Ag1 N21 82.44(8) 2_564 . ? C12 C1 C22 112.4(3) . . ? C12 C1 C2 111.9(3) . . ? C22 C1 C2 111.3(3) . . ? C32 C2 C42 112.1(3) . . ? C32 C2 C1 109.6(3) . . ? C42 C2 C1 113.6(3) . . ? C16 N11 C12 118.7(4) . . ? C16 N11 Ag1 112.1(3) . . ? C12 N11 Ag1 124.4(2) . . ? N11 C12 C13 120.9(3) . . ? N11 C12 C1 118.9(3) . . ? C13 C12 C1 120.1(3) . . ? C14 C13 C12 119.6(4) . . ? C13 C14 C15 119.7(4) . . ? C14 C15 C16 118.3(4) . . ? N11 C16 C15 122.7(4) . . ? C26 N21 C22 117.8(3) . . ? C26 N21 Ag1 115.6(2) . . ? C22 N21 Ag1 115.7(2) . . ? N21 C22 C23 122.4(3) . . ? N21 C22 C1 117.0(3) . . ? C23 C22 C1 120.6(3) . . ? C22 C23 C24 118.6(3) . . ? C25 C24 C23 119.5(3) . . ? C24 C25 C26 118.0(3) . . ? N21 C26 C25 123.7(3) . . ? C36 N31 C32 119.1(4) . . ? C36 N31 Ag1 111.6(3) . 2_565 ? C32 N31 Ag1 123.9(2) . 2_565 ? N31 C32 C33 120.5(3) . . ? N31 C32 C2 117.7(3) . . ? C33 C32 C2 121.8(3) . . ? C34 C33 C32 119.6(4) . . ? C33 C34 C35 119.7(4) . . ? C36 C35 C34 117.9(3) . . ? N31 C36 C35 123.2(4) . . ? C42 N41 C46 117.9(3) . . ? C42 N41 Ag1 119.6(2) . 2_565 ? C46 N41 Ag1 113.7(3) . 2_565 ? N41 C42 C43 122.1(3) . . ? N41 C42 C2 118.0(3) . . ? C43 C42 C2 119.8(3) . . ? C44 C43 C42 118.7(3) . . ? C45 C44 C43 119.9(4) . . ? C44 C45 C46 118.1(4) . . ? N41 C46 C45 123.3(4) . . ? O13 N10 O11 121.0(4) . . ? O13 N10 O12 119.9(4) . . ? O11 N10 O12 119.1(3) . . ? 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 C12 C1 C2 C32 171.2(3) . . . . ? C22 C1 C2 C32 -62.1(3) . . . . ? C12 C1 C2 C42 45.0(3) . . . . ? C22 C1 C2 C42 171.7(3) . . . . ? N31 Ag1 N11 C16 -165.3(5) 2_564 . . . ? N41 Ag1 N11 C16 -68.9(3) 2_564 . . . ? N21 Ag1 N11 C16 -150.6(3) . . . . ? N31 Ag1 N11 C12 -10.6(9) 2_564 . . . ? N41 Ag1 N11 C12 85.9(3) 2_564 . . . ? N21 Ag1 N11 C12 4.2(3) . . . . ? C16 N11 C12 C13 3.1(5) . . . . ? Ag1 N11 C12 C13 -150.1(3) . . . . ? C16 N11 C12 C1 -177.5(3) . . . . ? Ag1 N11 C12 C1 29.2(4) . . . . ? C22 C1 C12 N11 -77.3(4) . . . . ? C2 C1 C12 N11 48.8(4) . . . . ? C22 C1 C12 C13 102.1(3) . . . . ? C2 C1 C12 C13 -131.8(3) . . . . ? N11 C12 C13 C14 -1.6(5) . . . . ? C1 C12 C13 C14 179.1(3) . . . . ? C12 C13 C14 C15 -1.1(6) . . . . ? C13 C14 C15 C16 2.1(6) . . . . ? C12 N11 C16 C15 -2.0(6) . . . . ? Ag1 N11 C16 C15 154.3(3) . . . . ? C14 C15 C16 N11 -0.6(6) . . . . ? N11 Ag1 N21 C26 143.9(3) . . . . ? N31 Ag1 N21 C26 -38.6(3) 2_564 . . . ? N41 Ag1 N21 C26 46.5(3) 2_564 . . . ? N11 Ag1 N21 C22 0.3(3) . . . . ? N31 Ag1 N21 C22 177.8(3) 2_564 . . . ? N41 Ag1 N21 C22 -97.1(3) 2_564 . . . ? C26 N21 C22 C23 -1.6(5) . . . . ? Ag1 N21 C22 C23 141.2(3) . . . . ? C26 N21 C22 C1 179.6(3) . . . . ? Ag1 N21 C22 C1 -37.6(4) . . . . ? C12 C1 C22 N21 82.4(4) . . . . ? C2 C1 C22 N21 -44.1(4) . . . . ? C12 C1 C22 C23 -96.5(4) . . . . ? C2 C1 C22 C23 137.1(3) . . . . ? N21 C22 C23 C24 -0.5(6) . . . . ? C1 C22 C23 C24 178.3(3) . . . . ? C22 C23 C24 C25 1.7(6) . . . . ? C23 C24 C25 C26 -0.9(6) . . . . ? C22 N21 C26 C25 2.6(6) . . . . ? Ag1 N21 C26 C25 -140.2(3) . . . . ? C24 C25 C26 N21 -1.4(6) . . . . ? C36 N31 C32 C33 1.2(5) . . . . ? Ag1 N31 C32 C33 153.0(3) 2_565 . . . ? C36 N31 C32 C2 179.8(3) . . . . ? Ag1 N31 C32 C2 -28.3(4) 2_565 . . . ? C42 C2 C32 N31 74.5(4) . . . . ? C1 C2 C32 N31 -52.6(4) . . . . ? C42 C2 C32 C33 -106.9(4) . . . . ? C1 C2 C32 C33 125.9(3) . . . . ? N31 C32 C33 C34 -1.9(5) . . . . ? C2 C32 C33 C34 179.5(3) . . . . ? C32 C33 C34 C35 1.1(6) . . . . ? C33 C34 C35 C36 0.4(6) . . . . ? C32 N31 C36 C35 0.4(6) . . . . ? Ag1 N31 C36 C35 -154.7(3) 2_565 . . . ? C34 C35 C36 N31 -1.1(6) . . . . ? C46 N41 C42 C43 0.8(5) . . . . ? Ag1 N41 C42 C43 -144.6(3) 2_565 . . . ? C46 N41 C42 C2 179.7(3) . . . . ? Ag1 N41 C42 C2 34.3(4) 2_565 . . . ? C32 C2 C42 N41 -78.7(4) . . . . ? C1 C2 C42 N41 46.2(4) . . . . ? C32 C2 C42 C43 100.2(4) . . . . ? C1 C2 C42 C43 -134.9(3) . . . . ? N41 C42 C43 C44 -0.1(5) . . . . ? C2 C42 C43 C44 -179.0(3) . . . . ? C42 C43 C44 C45 -0.9(6) . . . . ? C43 C44 C45 C46 1.2(6) . . . . ? C42 N41 C46 C45 -0.5(6) . . . . ? Ag1 N41 C46 C45 146.9(3) 2_565 . . . ? C44 C45 C46 N41 -0.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.296 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.048 #===END data_Compound-13 _database_code_CSD 216637 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 13 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H42 Ag2 B2 F8 N10' _chemical_formula_weight 1148.28 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 9.225(3) _cell_length_b 15.448(6) _cell_length_c 16.892(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.551(5) _cell_angle_gamma 90.00 _cell_volume 2404.8(15) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 5492 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.58 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.824184 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 27747 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4818 _reflns_number_gt 2844 _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^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4818 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _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 Ag1 Ag 0.62638(9) -0.03962(4) -0.08186(3) 0.0364(2) Uani 0.6983(19) 1 d P . 1 Ag1' Ag 0.5314(3) -0.06334(8) -0.10016(7) 0.0487(7) Uani 0.3017(19) 1 d P . 2 C1 C 0.6890(5) 0.1719(4) -0.0735(3) 0.0824(18) Uani 1 1 d . . . H1A H 0.7111 0.2346 -0.0813 0.099 Uiso 1 1 calc R . . C2 C 0.63330(19) 0.17190(13) 0.00053(11) 0.0823(17) Uani 1 1 d . . . H2A H 0.6056 0.1102 0.0092 0.099 Uiso 1 1 calc R . . N11 N 0.52235(19) 0.07399(13) -0.15185(11) 0.0438(8) Uani 1 1 d R . . C12 C 0.58141(19) 0.15348(13) -0.14369(11) 0.0413(9) Uani 1 1 d R . . C13 C 0.55110(19) 0.21854(13) -0.19699(11) 0.0547(12) Uani 1 1 d R . . H13A H 0.5929 0.2743 -0.1896 0.066 Uiso 1 1 calc R . . C14 C 0.4583(5) 0.2015(3) -0.2619(3) 0.0661(14) Uani 1 1 d . . . H14A H 0.4358 0.2454 -0.2999 0.079 Uiso 1 1 calc R . . C15 C 0.3998(4) 0.1208(3) -0.2704(3) 0.0621(13) Uani 1 1 d . . . H15A H 0.3359 0.1076 -0.3144 0.074 Uiso 1 1 calc R . . C16 C 0.4344(4) 0.0593(3) -0.2148(3) 0.0525(11) Uani 1 1 d . . . H16A H 0.3936 0.0031 -0.2214 0.063 Uiso 1 1 calc R . . N21 N 0.8411(3) 0.0416(2) -0.08099(18) 0.0508(9) Uani 1 1 d . . . C22 C 0.8363(4) 0.1299(3) -0.0854(2) 0.0504(11) Uani 1 1 d . . . C23 C 0.9556(5) 0.1797(3) -0.1022(2) 0.0528(11) Uani 1 1 d . . . H23A H 0.9482 0.2410 -0.1040 0.063 Uiso 1 1 calc R . . C24 C 1.0849(4) 0.1399(3) -0.1161(2) 0.0495(10) Uani 1 1 d . . . H24A H 1.1673 0.1731 -0.1287 0.059 Uiso 1 1 calc R . . C25 C 1.0936(4) 0.0514(2) -0.1116(2) 0.0499(11) Uani 1 1 d . . . H25A H 1.1824 0.0226 -0.1203 0.060 Uiso 1 1 calc R . . C26 C 0.9715(4) 0.0049(3) -0.0941(2) 0.0528(11) Uani 1 1 d . . . H26A H 0.9791 -0.0563 -0.0910 0.063 Uiso 1 1 calc R . . N31 N 0.7241(3) 0.1359(2) 0.13005(19) 0.0466(8) Uani 1 1 d . . . C32 C 0.7349(4) 0.1936(3) 0.0729(2) 0.0429(10) Uani 1 1 d . . . C33 C 0.8276(4) 0.2646(3) 0.0787(3) 0.0542(11) Uani 1 1 d . . . H33A H 0.8308 0.3054 0.0368 0.065 Uiso 1 1 calc R . . C34 C 0.9159(4) 0.2747(3) 0.1474(3) 0.0590(12) Uani 1 1 d . . . H34A H 0.9802 0.3225 0.1536 0.071 Uiso 1 1 calc R . . C35 C 0.9069(4) 0.2134(3) 0.2054(2) 0.0542(11) Uani 1 1 d . . . H35A H 0.9672 0.2168 0.2524 0.065 Uiso 1 1 calc R . . C36 C 0.8100(4) 0.1475(3) 0.1948(2) 0.0507(10) Uani 1 1 d . . . H36A H 0.8031 0.1068 0.2366 0.061 Uiso 1 1 calc R . . N41 N 0.3806(3) 0.17796(19) 0.03755(17) 0.0394(7) Uani 1 1 d . . . C42 C 0.4889(4) 0.2230(3) 0.0099(2) 0.0444(10) Uani 1 1 d . . . C43 C 0.4733(5) 0.3094(3) -0.0094(3) 0.0653(13) Uani 1 1 d . . . H43A H 0.5532 0.3405 -0.0288 0.078 Uiso 1 1 calc R . . C44 C 0.3431(5) 0.3508(3) -0.0007(2) 0.0643(13) Uani 1 1 d . . . H44A H 0.3322 0.4104 -0.0134 0.077 Uiso 1 1 calc R . . C45 C 0.2278(4) 0.3034(2) 0.0272(2) 0.0466(10) Uani 1 1 d . . . H45A H 0.1354 0.3292 0.0330 0.056 Uiso 1 1 calc R . . C46 C 0.2522(4) 0.2186(2) 0.0459(2) 0.0406(9) Uani 1 1 d . . . H46A H 0.1744 0.1862 0.0660 0.049 Uiso 1 1 calc R . . B1 B 0.1662(7) 0.5519(3) 0.0942(3) 0.0616(15) Uani 1 1 d . . . F1 F 0.0577(4) 0.61327(18) 0.10683(19) 0.1213(12) Uani 1 1 d . . . F2 F 0.2924(4) 0.5839(2) 0.12726(18) 0.1233(13) Uani 1 1 d . . . F3 F 0.1811(4) 0.54128(18) 0.01411(16) 0.1115(11) Uani 1 1 d . . . F4 F 0.1306(3) 0.47623(14) 0.13006(15) 0.0723(7) Uani 1 1 d . . . C50 C 0.7740(7) 0.0121(4) -0.3215(3) 0.124(3) Uani 1 1 d . . . H50A H 0.7261 0.0008 -0.3734 0.186 Uiso 1 1 calc R . . H50B H 0.8790 0.0164 -0.3271 0.186 Uiso 1 1 calc R . . H50C H 0.7376 0.0666 -0.3002 0.186 Uiso 1 1 calc R . . C51 C 0.7432(5) -0.0578(3) -0.2681(3) 0.0655(13) Uani 1 1 d . . . N52 N 0.7198(6) -0.1090(3) -0.2252(3) 0.1034(16) 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 Ag1 0.0397(4) 0.0273(2) 0.0430(3) 0.0052(2) 0.0093(2) 0.0012(3) Ag1' 0.0770(16) 0.0328(6) 0.0370(7) -0.0012(5) 0.0109(7) -0.0047(7) C1 0.058(3) 0.134(5) 0.054(3) -0.050(3) -0.016(2) 0.052(3) C2 0.039(2) 0.161(5) 0.047(3) -0.010(3) 0.003(2) 0.040(3) N11 0.055(2) 0.0413(18) 0.036(2) 0.0083(16) 0.0103(16) 0.0097(16) C12 0.037(2) 0.049(2) 0.038(2) -0.009(2) 0.0006(17) 0.0140(18) C13 0.047(2) 0.037(2) 0.082(4) 0.002(2) 0.018(2) 0.0014(19) C14 0.066(3) 0.081(4) 0.052(3) 0.032(3) 0.008(2) 0.026(3) C15 0.050(3) 0.090(4) 0.046(3) -0.004(3) -0.010(2) 0.012(3) C16 0.045(2) 0.052(3) 0.061(3) -0.006(2) 0.010(2) -0.015(2) N21 0.0359(17) 0.074(2) 0.042(2) 0.0113(19) 0.0076(14) 0.0141(18) C22 0.059(3) 0.066(3) 0.024(2) -0.017(2) -0.0092(19) 0.042(2) C23 0.063(3) 0.046(2) 0.049(3) -0.011(2) -0.007(2) 0.009(2) C24 0.057(3) 0.047(3) 0.045(3) -0.002(2) 0.009(2) 0.006(2) C25 0.043(2) 0.042(2) 0.066(3) 0.000(2) 0.018(2) 0.0110(18) C26 0.042(2) 0.038(2) 0.079(3) 0.005(2) 0.016(2) 0.0130(18) N31 0.0499(19) 0.049(2) 0.041(2) -0.0107(17) 0.0080(16) 0.0005(16) C32 0.032(2) 0.064(3) 0.032(2) -0.004(2) 0.0047(17) 0.017(2) C33 0.059(3) 0.055(3) 0.050(3) 0.012(2) 0.020(2) 0.011(2) C34 0.055(3) 0.055(3) 0.069(3) -0.019(3) 0.020(2) -0.012(2) C35 0.048(2) 0.074(3) 0.040(3) -0.020(2) -0.004(2) 0.009(2) C36 0.066(3) 0.048(3) 0.038(3) 0.003(2) 0.004(2) 0.011(2) N41 0.0436(18) 0.0435(18) 0.0311(18) 0.0026(15) 0.0025(14) 0.0122(15) C42 0.036(2) 0.069(3) 0.028(2) -0.003(2) 0.0014(17) 0.013(2) C43 0.054(3) 0.076(3) 0.069(3) 0.000(3) 0.032(2) -0.013(3) C44 0.100(4) 0.039(2) 0.055(3) 0.008(2) 0.015(3) 0.006(2) C45 0.042(2) 0.049(2) 0.049(3) -0.002(2) 0.0036(19) 0.0200(19) C46 0.034(2) 0.048(2) 0.040(2) -0.0036(19) 0.0027(17) -0.0042(18) B1 0.105(4) 0.035(3) 0.045(3) -0.004(2) 0.009(3) -0.001(3) F1 0.194(4) 0.0602(19) 0.110(3) -0.0007(17) 0.010(2) 0.051(2) F2 0.145(3) 0.150(3) 0.076(2) 0.001(2) 0.010(2) -0.092(3) F3 0.208(4) 0.079(2) 0.0484(19) -0.0054(15) 0.0089(19) 0.013(2) F4 0.0739(16) 0.0425(14) 0.101(2) 0.0233(14) 0.0098(14) -0.0014(12) C50 0.179(7) 0.082(4) 0.118(5) 0.024(4) 0.090(5) 0.007(4) C51 0.093(4) 0.056(3) 0.049(3) -0.007(2) 0.024(3) -0.005(3) N52 0.175(5) 0.069(3) 0.070(3) 0.009(3) 0.042(3) -0.006(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 Ag1 N41 2.266(3) 3_655 ? Ag1 N11 2.302(2) . ? Ag1 N21 2.344(3) . ? Ag1' N41 2.199(3) 3_655 ? Ag1' N11 2.294(2) . ? Ag1' N31 2.638(4) 3_655 ? C1 C2 1.373(5) . ? C1 C22 1.528(5) . ? C1 C12 1.538(4) . ? C2 C32 1.544(4) . ? C2 C42 1.562(4) . ? N11 C16 1.327(4) . ? N11 C12 1.3480 . ? C12 C13 1.3698 . ? C13 C14 1.386(5) . ? C14 C15 1.364(6) . ? C15 C16 1.365(6) . ? N21 C26 1.357(4) . ? N21 C22 1.366(5) . ? C22 C23 1.383(6) . ? C23 C24 1.371(5) . ? C24 C25 1.371(5) . ? C25 C26 1.379(5) . ? N31 C32 1.322(5) . ? N31 C36 1.334(5) . ? N31 Ag1' 2.638(4) 3_655 ? C32 C33 1.391(5) . ? C33 C34 1.395(6) . ? C34 C35 1.368(6) . ? C35 C36 1.362(5) . ? N41 C42 1.320(5) . ? N41 C46 1.354(4) . ? N41 Ag1' 2.199(3) 3_655 ? N41 Ag1 2.266(3) 3_655 ? C42 C43 1.380(5) . ? C43 C44 1.374(6) . ? C44 C45 1.390(5) . ? C45 C46 1.363(5) . ? B1 F2 1.362(6) . ? B1 F4 1.363(5) . ? B1 F3 1.376(6) . ? B1 F1 1.402(6) . ? C50 C51 1.442(7) . ? C51 N52 1.101(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Ag1 N11 150.62(10) 3_655 . ? N41 Ag1 N21 122.62(11) 3_655 . ? N11 Ag1 N21 85.87(10) . . ? N41 Ag1' N11 159.05(16) 3_655 . ? N41 Ag1' N31 93.31(13) 3_655 3_655 ? N11 Ag1' N31 107.64(12) . 3_655 ? C2 C1 C22 119.4(3) . . ? C2 C1 C12 116.6(3) . . ? C22 C1 C12 111.5(3) . . ? C1 C2 C32 118.8(3) . . ? C1 C2 C42 116.6(3) . . ? C32 C2 C42 107.5(2) . . ? C16 N11 C12 117.9(2) . . ? C16 N11 Ag1' 99.0(2) . . ? C12 N11 Ag1' 142.73(8) . . ? C16 N11 Ag1 120.4(2) . . ? C12 N11 Ag1 118.99(6) . . ? Ag1' N11 Ag1 24.80(5) . . ? N11 C12 C13 122.1 . . ? N11 C12 C1 119.4(2) . . ? C13 C12 C1 118.5(2) . . ? C12 C13 C14 118.8(2) . . ? C15 C14 C13 118.9(4) . . ? C14 C15 C16 119.0(4) . . ? N11 C16 C15 123.2(4) . . ? C26 N21 C22 115.8(3) . . ? C26 N21 Ag1 122.0(3) . . ? C22 N21 Ag1 120.6(2) . . ? N21 C22 C23 122.9(3) . . ? N21 C22 C1 116.3(4) . . ? C23 C22 C1 120.8(4) . . ? C24 C23 C22 119.4(4) . . ? C25 C24 C23 119.1(4) . . ? C24 C25 C26 119.0(3) . . ? N21 C26 C25 123.8(4) . . ? C32 N31 C36 116.5(3) . . ? C32 N31 Ag1' 104.1(2) . 3_655 ? C36 N31 Ag1' 135.0(3) . 3_655 ? N31 C32 C33 123.1(4) . . ? N31 C32 C2 111.6(3) . . ? C33 C32 C2 125.3(4) . . ? C32 C33 C34 118.8(4) . . ? C35 C34 C33 117.7(4) . . ? C36 C35 C34 118.9(4) . . ? N31 C36 C35 124.9(4) . . ? C42 N41 C46 118.2(3) . . ? C42 N41 Ag1' 109.0(2) . 3_655 ? C46 N41 Ag1' 129.0(3) . 3_655 ? C42 N41 Ag1 130.3(2) . 3_655 ? C46 N41 Ag1 111.4(2) . 3_655 ? Ag1' N41 Ag1 25.48(6) 3_655 3_655 ? N41 C42 C43 121.4(3) . . ? N41 C42 C2 115.6(3) . . ? C43 C42 C2 123.0(4) . . ? C44 C43 C42 120.5(4) . . ? C43 C44 C45 118.5(4) . . ? C46 C45 C44 117.6(3) . . ? N41 C46 C45 123.9(3) . . ? F2 B1 F4 110.3(4) . . ? F2 B1 F3 109.0(5) . . ? F4 B1 F3 111.8(4) . . ? F2 B1 F1 107.2(4) . . ? F4 B1 F1 108.9(4) . . ? F3 B1 F1 109.5(4) . . ? N52 C51 C50 177.4(5) . . ? 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 C22 C1 C2 C32 43.6(6) . . . . ? C12 C1 C2 C32 -177.6(3) . . . . ? C22 C1 C2 C42 174.8(4) . . . . ? C12 C1 C2 C42 -46.3(5) . . . . ? N41 Ag1' N11 C16 148.2(3) 3_655 . . . ? N31 Ag1' N11 C16 -33.8(2) 3_655 . . . ? N41 Ag1' N11 C12 -24.0(3) 3_655 . . . ? N31 Ag1' N11 C12 154.07(9) 3_655 . . . ? N41 Ag1' N11 Ag1 -3.4(3) 3_655 . . . ? N31 Ag1' N11 Ag1 174.69(12) 3_655 . . . ? N41 Ag1 N11 C16 -30.7(3) 3_655 . . . ? N21 Ag1 N11 C16 136.1(2) . . . . ? N41 Ag1 N11 C12 168.29(16) 3_655 . . . ? N21 Ag1 N11 C12 -24.96(8) . . . . ? N41 Ag1 N11 Ag1' 2.40(18) 3_655 . . . ? N21 Ag1 N11 Ag1' 169.14(11) . . . . ? C16 N11 C12 C13 1.3(2) . . . . ? Ag1' N11 C12 C13 172.49(9) . . . . ? Ag1 N11 C12 C13 162.77(5) . . . . ? C16 N11 C12 C1 -177.4(3) . . . . ? Ag1' N11 C12 C1 -6.16(18) . . . . ? Ag1 N11 C12 C1 -15.88(17) . . . . ? C2 C1 C12 N11 -67.9(4) . . . . ? C22 C1 C12 N11 74.0(4) . . . . ? C2 C1 C12 C13 113.4(4) . . . . ? C22 C1 C12 C13 -104.7(4) . . . . ? N11 C12 C13 C14 -0.9(2) . . . . ? C1 C12 C13 C14 177.7(3) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C13 C14 C15 C16 0.0(6) . . . . ? C12 N11 C16 C15 -1.0(4) . . . . ? Ag1' N11 C16 C15 -175.6(3) . . . . ? Ag1 N11 C16 C15 -162.2(3) . . . . ? C14 C15 C16 N11 0.4(6) . . . . ? N41 Ag1 N21 C26 34.6(3) 3_655 . . . ? N11 Ag1 N21 C26 -137.7(3) . . . . ? N41 Ag1 N21 C22 -160.5(3) 3_655 . . . ? N11 Ag1 N21 C22 27.1(3) . . . . ? C26 N21 C22 C23 0.1(5) . . . . ? Ag1 N21 C22 C23 -165.7(3) . . . . ? C26 N21 C22 C1 178.1(3) . . . . ? Ag1 N21 C22 C1 12.3(4) . . . . ? C2 C1 C22 N21 70.9(5) . . . . ? C12 C1 C22 N21 -69.8(5) . . . . ? C2 C1 C22 C23 -111.1(5) . . . . ? C12 C1 C22 C23 108.2(4) . . . . ? N21 C22 C23 C24 0.8(6) . . . . ? C1 C22 C23 C24 -177.1(3) . . . . ? C22 C23 C24 C25 -1.3(6) . . . . ? C23 C24 C25 C26 0.8(6) . . . . ? C22 N21 C26 C25 -0.6(6) . . . . ? Ag1 N21 C26 C25 165.0(3) . . . . ? C24 C25 C26 N21 0.1(7) . . . . ? C36 N31 C32 C33 -1.4(5) . . . . ? Ag1' N31 C32 C33 158.6(3) 3_655 . . . ? C36 N31 C32 C2 178.5(3) . . . . ? Ag1' N31 C32 C2 -21.4(3) 3_655 . . . ? C1 C2 C32 N31 -130.7(4) . . . . ? C42 C2 C32 N31 94.1(3) . . . . ? C1 C2 C32 C33 49.2(5) . . . . ? C42 C2 C32 C33 -86.0(4) . . . . ? N31 C32 C33 C34 1.4(6) . . . . ? C2 C32 C33 C34 -178.5(3) . . . . ? C32 C33 C34 C35 0.4(6) . . . . ? C33 C34 C35 C36 -2.0(6) . . . . ? C32 N31 C36 C35 -0.4(5) . . . . ? Ag1' N31 C36 C35 -152.5(3) 3_655 . . . ? C34 C35 C36 N31 2.1(6) . . . . ? C46 N41 C42 C43 0.7(5) . . . . ? Ag1' N41 C42 C43 -159.3(3) 3_655 . . . ? Ag1 N41 C42 C43 -175.5(3) 3_655 . . . ? C46 N41 C42 C2 -179.1(3) . . . . ? Ag1' N41 C42 C2 20.9(3) 3_655 . . . ? Ag1 N41 C42 C2 4.6(5) 3_655 . . . ? C1 C2 C42 N41 123.8(4) . . . . ? C32 C2 C42 N41 -99.9(3) . . . . ? C1 C2 C42 C43 -56.0(5) . . . . ? C32 C2 C42 C43 80.3(4) . . . . ? N41 C42 C43 C44 -0.5(6) . . . . ? C2 C42 C43 C44 179.3(3) . . . . ? C42 C43 C44 C45 -0.5(6) . . . . ? C43 C44 C45 C46 1.3(6) . . . . ? C42 N41 C46 C45 0.2(5) . . . . ? Ag1' N41 C46 C45 155.6(3) 3_655 . . . ? Ag1 N41 C46 C45 177.1(3) 3_655 . . . ? C44 C45 C46 N41 -1.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.808 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.068 #===END data_Compound-14 _database_code_CSD 216638 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 14 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34 Cu2 N8 O16' _chemical_formula_weight 841.69 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 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 27.086(13) _cell_length_b 10.055(5) _cell_length_c 14.324(7) _cell_angle_alpha 90.00 _cell_angle_beta 119.938(6) _cell_angle_gamma 90.00 _cell_volume 3380(3) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.880043 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst (1995) A 51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 21145 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.41 _reflns_number_total 3438 _reflns_number_gt 2812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0416P)^2^+0.3794P] 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 3438 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.093 _refine_ls_shift/su_mean 0.008 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 0.124906(9) 0.60046(2) 0.341710(17) 0.02183(8) Uani 1 1 d . . . C1 C 0.23826(7) 0.73446(17) 0.53920(14) 0.0188(4) Uani 1 1 d . . . H1A H 0.2673 0.7685 0.6118 0.023 Uiso 1 1 calc R . . N1' N 0.13289(6) 0.75985(15) 0.43076(12) 0.0210(3) Uani 1 1 d . A . N1" N 0.18927(7) 0.51707(15) 0.47283(12) 0.0226(3) Uani 1 1 d . A . C2' C 0.18309(7) 0.80842(18) 0.50825(14) 0.0196(4) Uani 1 1 d . . . C2" C 0.23330(8) 0.58526(18) 0.55160(15) 0.0207(4) Uani 1 1 d . . . C3' C 0.18516(9) 0.92501(19) 0.56227(17) 0.0293(5) Uani 1 1 d . A . H3'A H 0.2208 0.9606 0.6149 0.035 Uiso 1 1 calc R . . C3" C 0.27417(9) 0.5214(2) 0.64376(16) 0.0299(4) Uani 1 1 d . A . H3"A H 0.3054 0.5700 0.6979 0.036 Uiso 1 1 calc R . . C4' C 0.13497(10) 0.9892(2) 0.53901(18) 0.0366(5) Uani 1 1 d . . . H4'A H 0.1359 1.0703 0.5740 0.044 Uiso 1 1 calc R A . C4" C 0.26927(10) 0.3863(2) 0.65661(18) 0.0386(5) Uani 1 1 d . . . H4"A H 0.2969 0.3415 0.7196 0.046 Uiso 1 1 calc R A . C5' C 0.08394(9) 0.9340(2) 0.46482(18) 0.0358(5) Uani 1 1 d . A . H5'A H 0.0490 0.9737 0.4505 0.043 Uiso 1 1 calc R . . C5" C 0.22380(10) 0.3181(2) 0.57684(18) 0.0371(5) Uani 1 1 d . A . H5"A H 0.2194 0.2255 0.5841 0.045 Uiso 1 1 calc R . . C6' C 0.08408(8) 0.8205(2) 0.41148(16) 0.0293(4) Uani 1 1 d . . . H6'A H 0.0487 0.7833 0.3593 0.035 Uiso 1 1 calc R A . C6" C 0.18468(9) 0.38566(19) 0.48626(18) 0.0325(5) Uani 1 1 d . . . H6"A H 0.1533 0.3381 0.4312 0.039 Uiso 1 1 calc R A . N10 N 0.15205(8) 0.42829(17) 0.21787(12) 0.0263(4) Uani 1 1 d . . . O11 O 0.1109(5) 0.4502(9) 0.2437(7) 0.0306(13) Uani 0.75(5) 1 d P A 1 O12 O 0.1952(4) 0.486(2) 0.2612(11) 0.064(3) Uani 0.75(5) 1 d P A 1 O11' O 0.1261(16) 0.433(3) 0.254(2) 0.035(4) Uani 0.25(5) 1 d P A 2 O12' O 0.1814(16) 0.539(4) 0.227(3) 0.054(6) Uani 0.25(5) 1 d P A 2 O13 O 0.14403(9) 0.33444(19) 0.15560(13) 0.0632(6) Uani 1 1 d . A . N20 N 0.07803(7) 0.75770(16) 0.16060(13) 0.0277(4) Uani 1 1 d . . . O21 O 0.0593(7) 0.6928(17) 0.2177(14) 0.0238(18) Uani 0.61(7) 1 d P A 1 O22 O 0.1301(5) 0.7495(17) 0.1920(11) 0.0359(19) Uani 0.61(7) 1 d P A 1 O21' O 0.0625(11) 0.676(3) 0.202(2) 0.027(3) Uani 0.39(7) 1 d P A 2 O22' O 0.1292(10) 0.790(5) 0.207(2) 0.051(6) Uani 0.39(7) 1 d P A 2 O23 O 0.04314(7) 0.81366(16) 0.07765(12) 0.0452(4) Uani 1 1 d . A . O31 O 0.05343(6) 0.4931(2) 0.34972(12) 0.0378(4) Uani 1 1 d . A . H31 H 0.0337(12) 0.515(3) 0.317(2) 0.057 Uiso 1 1 d . . . C31 C 0.04519(10) 0.4775(3) 0.44030(17) 0.0420(6) Uani 1 1 d . . . H31A H 0.0107 0.4249 0.4191 0.063 Uiso 1 1 calc R A . H31B H 0.0411 0.5652 0.4655 0.063 Uiso 1 1 calc R . . H31C H 0.0782 0.4317 0.4984 0.063 Uiso 1 1 calc R . . O41 O 0.0611(3) 0.1992(8) 0.2592(8) 0.070(3) Uani 0.533(18) 1 d P B 1 H41 H 0.0666 0.2687 0.2331 0.104 Uiso 0.533(18) 1 calc PR B 1 C41 C 0.0686(3) 0.0940(12) 0.2122(7) 0.061(2) Uani 0.533(18) 1 d P B 1 H41A H 0.1093 0.0815 0.2388 0.091 Uiso 0.533(18) 1 calc PR B 1 H41B H 0.0486 0.1076 0.1340 0.091 Uiso 0.533(18) 1 calc PR B 1 H41C H 0.0532 0.0150 0.2289 0.091 Uiso 0.533(18) 1 calc PR B 1 O41' O 0.0489(3) 0.2237(6) 0.2957(7) 0.0486(18) Uani 0.467(18) 1 d P B 2 H41' H 0.0148 0.2215 0.2809 0.073 Uiso 0.467(18) 1 calc PR B 2 C41' C 0.0546(8) 0.1547(12) 0.2098(13) 0.089(4) Uani 0.467(18) 1 d P B 2 H41D H 0.0854 0.1956 0.2028 0.133 Uiso 0.467(18) 1 calc PR B 2 H41E H 0.0187 0.1625 0.1412 0.133 Uiso 0.467(18) 1 calc PR B 2 H41F H 0.0632 0.0606 0.2285 0.133 Uiso 0.467(18) 1 calc PR B 2 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 0.02199(13) 0.02132(13) 0.02124(13) -0.00200(10) 0.01008(10) -0.00297(9) C1 0.0174(9) 0.0194(9) 0.0198(9) -0.0011(7) 0.0094(8) -0.0025(7) N1' 0.0203(8) 0.0228(8) 0.0221(8) 0.0025(7) 0.0122(7) 0.0021(6) N1" 0.0253(8) 0.0193(8) 0.0256(8) 0.0012(7) 0.0146(7) 0.0004(7) C2' 0.0226(9) 0.0188(9) 0.0227(9) 0.0023(7) 0.0153(8) -0.0008(7) C2" 0.0207(9) 0.0219(10) 0.0251(9) 0.0019(8) 0.0156(8) 0.0021(7) C3' 0.0334(11) 0.0248(11) 0.0365(11) -0.0072(9) 0.0225(10) -0.0052(8) C3" 0.0262(10) 0.0348(12) 0.0273(10) 0.0045(9) 0.0121(9) 0.0025(9) C4' 0.0458(13) 0.0276(11) 0.0503(14) -0.0060(10) 0.0344(12) 0.0029(10) C4" 0.0429(13) 0.0367(13) 0.0388(12) 0.0190(10) 0.0224(11) 0.0157(11) C5' 0.0346(12) 0.0371(12) 0.0441(13) 0.0041(10) 0.0259(11) 0.0129(10) C5" 0.0476(14) 0.0196(10) 0.0508(14) 0.0092(10) 0.0296(12) 0.0059(10) C6' 0.0225(10) 0.0358(12) 0.0298(10) 0.0034(9) 0.0132(9) 0.0051(9) C6" 0.0371(12) 0.0193(10) 0.0431(12) -0.0024(9) 0.0214(10) -0.0038(9) N10 0.0253(10) 0.0358(10) 0.0154(8) 0.0015(7) 0.0082(8) 0.0146(8) O11 0.021(3) 0.039(2) 0.037(2) -0.0149(15) 0.018(2) -0.001(2) O12 0.041(2) 0.104(7) 0.057(4) -0.021(4) 0.033(3) -0.010(3) O11' 0.018(9) 0.030(7) 0.063(8) -0.023(5) 0.025(7) -0.010(6) O12' 0.045(10) 0.072(11) 0.060(9) 0.002(9) 0.037(9) -0.010(8) O13 0.0936(15) 0.0544(12) 0.0371(10) -0.0035(9) 0.0293(10) 0.0356(11) N20 0.0320(10) 0.0222(9) 0.0271(9) 0.0004(7) 0.0135(8) -0.0019(7) O21 0.027(2) 0.034(3) 0.017(4) 0.001(3) 0.016(2) 0.002(2) O22 0.028(3) 0.036(4) 0.046(3) -0.001(3) 0.020(2) -0.009(2) O21' 0.024(4) 0.047(7) 0.016(5) -0.007(4) 0.015(3) -0.012(4) O22' 0.039(5) 0.059(13) 0.039(6) 0.015(7) 0.008(3) -0.026(7) O23 0.0488(10) 0.0446(10) 0.0318(8) 0.0150(7) 0.0123(8) 0.0080(8) O31 0.0262(9) 0.0583(11) 0.0256(8) 0.0075(7) 0.0104(7) -0.0107(8) C31 0.0388(13) 0.0569(15) 0.0339(12) 0.0104(11) 0.0207(11) -0.0046(11) O41 0.072(3) 0.047(4) 0.109(6) 0.011(4) 0.060(4) -0.005(3) C41 0.050(4) 0.058(6) 0.085(4) -0.019(4) 0.041(3) -0.008(3) O41' 0.050(3) 0.033(2) 0.079(4) -0.005(2) 0.044(3) -0.008(2) C41' 0.115(9) 0.037(6) 0.173(13) -0.045(6) 0.115(10) -0.023(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 Cu1 O11 1.967(8) . ? Cu1 N1' 1.9917(16) . ? Cu1 O21' 2.01(2) . ? Cu1 N1" 2.0003(17) . ? Cu1 O21 2.006(15) . ? Cu1 O11' 2.11(3) . ? Cu1 O31 2.2692(18) . ? C1 C2" 1.524(2) . ? C1 C2' 1.523(2) . ? C1 C1 1.574(3) 7_566 ? N1' C2' 1.346(2) . ? N1' C6' 1.353(2) . ? N1" C2" 1.350(2) . ? N1" C6" 1.350(2) . ? C2' C3' 1.390(3) . ? C2" C3" 1.386(3) . ? C3' C4' 1.387(3) . ? C3" C4" 1.386(3) . ? C4' C5' 1.372(3) . ? C4" C5" 1.374(3) . ? C5' C6' 1.375(3) . ? C5" C6" 1.377(3) . ? N10 O11' 1.06(3) . ? N10 O12 1.169(6) . ? N10 O13 1.241(2) . ? N10 O12' 1.34(2) . ? N10 O11 1.357(12) . ? N20 O21' 1.21(2) . ? N20 O23 1.225(2) . ? N20 O22' 1.244(17) . ? N20 O22 1.251(12) . ? N20 O21 1.330(18) . ? O31 C31 1.431(3) . ? O41 C41 1.323(8) . ? O41' C41' 1.486(10) . ? 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 O11 Cu1 N1' 175.0(4) . . ? O11 Cu1 O21' 79.2(11) . . ? N1' Cu1 O21' 95.9(11) . . ? O11 Cu1 N1" 96.7(3) . . ? N1' Cu1 N1" 88.32(7) . . ? O21' Cu1 N1" 175.1(11) . . ? O11 Cu1 O21 87.3(7) . . ? N1' Cu1 O21 87.7(6) . . ? O21' Cu1 O21 9.3(9) . . ? N1" Cu1 O21 175.6(6) . . ? O11 Cu1 O11' 10.5(8) . . ? N1' Cu1 O11' 173.7(9) . . ? O21' Cu1 O11' 87.8(15) . . ? N1" Cu1 O11' 87.8(10) . . ? O21 Cu1 O11' 96.4(12) . . ? O11 Cu1 O31 78.7(3) . . ? N1' Cu1 O31 99.97(7) . . ? O21' Cu1 O31 85.0(7) . . ? N1" Cu1 O31 96.82(7) . . ? O21 Cu1 O31 82.1(5) . . ? O11' Cu1 O31 85.4(8) . . ? C2" C1 C2' 112.56(14) . . ? C2" C1 C1 111.65(17) . 7_566 ? C2' C1 C1 112.48(18) . 7_566 ? C2' N1' C6' 119.13(16) . . ? C2' N1' Cu1 124.19(12) . . ? C6' N1' Cu1 116.68(13) . . ? C2" N1" C6" 118.93(17) . . ? C2" N1" Cu1 124.36(13) . . ? C6" N1" Cu1 116.42(14) . . ? N1' C2' C3' 120.55(16) . . ? N1' C2' C1 120.21(15) . . ? C3' C2' C1 119.23(16) . . ? N1" C2" C3" 120.87(18) . . ? N1" C2" C1 119.66(16) . . ? C3" C2" C1 119.48(17) . . ? C4' C3' C2' 119.76(19) . . ? C4" C3" C2" 119.8(2) . . ? C5' C4' C3' 119.0(2) . . ? C5" C4" C3" 119.0(2) . . ? C4' C5' C6' 119.04(19) . . ? C4" C5" C6" 119.08(19) . . ? N1' C6' C5' 122.27(19) . . ? N1" C6" C5" 122.4(2) . . ? O11' N10 O12 116.6(13) . . ? O11' N10 O13 117.8(13) . . ? O12 N10 O13 122.0(4) . . ? O11' N10 O12' 114.6(14) . . ? O12 N10 O12' 31.1(11) . . ? O13 N10 O12' 126.0(7) . . ? O11' N10 O11 13(2) . . ? O12 N10 O11 121.0(5) . . ? O13 N10 O11 116.5(4) . . ? O12' N10 O11 111.5(12) . . ? N10 O11 Cu1 115.3(6) . . ? N10 O11' Cu1 122.8(17) . . ? O21' N20 O23 120.1(12) . . ? O21' N20 O22' 118.8(14) . . ? O23 N20 O22' 121.0(10) . . ? O21' N20 O22 112.6(13) . . ? O23 N20 O22 124.4(6) . . ? O22' N20 O22 22(2) . . ? O21' N20 O21 13.7(17) . . ? O23 N20 O21 118.4(7) . . ? O22' N20 O21 117.6(11) . . ? O22 N20 O21 117.1(8) . . ? N20 O21 Cu1 109.2(10) . . ? N20 O21' Cu1 114.7(16) . . ? C31 O31 Cu1 128.40(14) . . ? 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 O11 Cu1 N1' C2' -151(3) . . . . ? O21' Cu1 N1' C2' -139.7(8) . . . . ? N1" Cu1 N1' C2' 37.74(14) . . . . ? O21 Cu1 N1' C2' -144.0(5) . . . . ? O11' Cu1 N1' C2' -14(8) . . . . ? O31 Cu1 N1' C2' 134.37(14) . . . . ? O11 Cu1 N1' C6' 30(3) . . . . ? O21' Cu1 N1' C6' 41.1(8) . . . . ? N1" Cu1 N1' C6' -141.44(13) . . . . ? O21 Cu1 N1' C6' 36.8(5) . . . . ? O11' Cu1 N1' C6' 167(8) . . . . ? O31 Cu1 N1' C6' -44.80(14) . . . . ? O11 Cu1 N1" C2" 148.2(3) . . . . ? N1' Cu1 N1" C2" -32.54(14) . . . . ? O21' Cu1 N1" C2" 116(9) . . . . ? O21 Cu1 N1" C2" -56(6) . . . . ? O11' Cu1 N1" C2" 142.5(7) . . . . ? O31 Cu1 N1" C2" -132.39(14) . . . . ? O11 Cu1 N1" C6" -38.0(3) . . . . ? N1' Cu1 N1" C6" 141.20(14) . . . . ? O21' Cu1 N1" C6" -70(9) . . . . ? O21 Cu1 N1" C6" 117(6) . . . . ? O11' Cu1 N1" C6" -43.7(7) . . . . ? O31 Cu1 N1" C6" 41.36(15) . . . . ? C6' N1' C2' C3' -4.8(3) . . . . ? Cu1 N1' C2' C3' 176.03(13) . . . . ? C6' N1' C2' C1 173.98(15) . . . . ? Cu1 N1' C2' C1 -5.2(2) . . . . ? C2" C1 C2' N1' -44.9(2) . . . . ? C1 C1 C2' N1' 82.3(2) 7_566 . . . ? C2" C1 C2' C3' 133.92(17) . . . . ? C1 C1 C2' C3' -98.9(2) 7_566 . . . ? C6" N1" C2" C3" 1.7(3) . . . . ? Cu1 N1" C2" C3" 175.32(13) . . . . ? C6" N1" C2" C1 -178.30(16) . . . . ? Cu1 N1" C2" C1 -4.7(2) . . . . ? C2' C1 C2" N1" 50.1(2) . . . . ? C1 C1 C2" N1" -77.5(2) 7_566 . . . ? C2' C1 C2" C3" -129.89(17) . . . . ? C1 C1 C2" C3" 102.5(2) 7_566 . . . ? N1' C2' C3' C4' 2.4(3) . . . . ? C1 C2' C3' C4' -176.41(17) . . . . ? N1" C2" C3" C4" -1.4(3) . . . . ? C1 C2" C3" C4" 178.61(17) . . . . ? C2' C3' C4' C5' 1.8(3) . . . . ? C2" C3" C4" C5" 0.3(3) . . . . ? C3' C4' C5' C6' -3.4(3) . . . . ? C3" C4" C5" C6" 0.4(3) . . . . ? C2' N1' C6' C5' 3.2(3) . . . . ? Cu1 N1' C6' C5' -177.63(15) . . . . ? C4' C5' C6' N1' 1.0(3) . . . . ? C2" N1" C6" C5" -1.0(3) . . . . ? Cu1 N1" C6" C5" -175.07(16) . . . . ? C4" C5" C6" N1" -0.1(3) . . . . ? O11' N10 O11 Cu1 81(7) . . . . ? O12 N10 O11 Cu1 8.1(11) . . . . ? O13 N10 O11 Cu1 -179.6(3) . . . . ? O12' N10 O11 Cu1 -25.1(18) . . . . ? N1' Cu1 O11 N10 119(3) . . . . ? O21' Cu1 O11 N10 107.6(10) . . . . ? N1" Cu1 O11 N10 -69.7(6) . . . . ? O21 Cu1 O11 N10 112.1(8) . . . . ? O11' Cu1 O11 N10 -37(5) . . . . ? O31 Cu1 O11 N10 -165.4(7) . . . . ? O12 N10 O11' Cu1 31(3) . . . . ? O13 N10 O11' Cu1 -170.2(15) . . . . ? O12' N10 O11' Cu1 -4(2) . . . . ? O11 N10 O11' Cu1 -83(8) . . . . ? O11 Cu1 O11' N10 124(7) . . . . ? N1' Cu1 O11' N10 -37(10) . . . . ? O21' Cu1 O11' N10 89(3) . . . . ? N1" Cu1 O11' N10 -89(3) . . . . ? O21 Cu1 O11' N10 93(3) . . . . ? O31 Cu1 O11' N10 174(3) . . . . ? O21' N20 O21 Cu1 75(7) . . . . ? O23 N20 O21 Cu1 175.7(5) . . . . ? O22' N20 O21 Cu1 -24(3) . . . . ? O22 N20 O21 Cu1 0.4(10) . . . . ? O11 Cu1 O21 N20 -87.0(11) . . . . ? N1' Cu1 O21 N20 93.7(11) . . . . ? O21' Cu1 O21 N20 -59(7) . . . . ? N1" Cu1 O21 N20 117(6) . . . . ? O11' Cu1 O21 N20 -81.5(13) . . . . ? O31 Cu1 O21 N20 -165.9(12) . . . . ? O23 N20 O21' Cu1 -177.1(10) . . . . ? O22' N20 O21' Cu1 -1.8(17) . . . . ? O22 N20 O21' Cu1 21(2) . . . . ? O21 N20 O21' Cu1 -90(8) . . . . ? O11 Cu1 O21' N20 -106(3) . . . . ? N1' Cu1 O21' N20 75(3) . . . . ? N1" Cu1 O21' N20 -73(10) . . . . ? O21 Cu1 O21' N20 103(8) . . . . ? O11' Cu1 O21' N20 -100(3) . . . . ? O31 Cu1 O21' N20 175(3) . . . . ? O11 Cu1 O31 C31 144.1(4) . . . . ? N1' Cu1 O31 C31 -40.84(19) . . . . ? O21' Cu1 O31 C31 -136.0(11) . . . . ? N1" Cu1 O31 C31 48.66(19) . . . . ? O21 Cu1 O31 C31 -127.1(6) . . . . ? O11' Cu1 O31 C31 135.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.301 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.051 #===END data_Compound-16 _database_code_CSD 216639 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 16 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 N4 O8 Zn2' _chemical_formula_weight 705.32 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.898(3) _cell_length_b 7.975(3) _cell_length_c 18.728(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.104(4) _cell_angle_gamma 90.00 _cell_volume 1469.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.32 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.710345 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 18324 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2975 _reflns_number_gt 2458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0317P)^2^+1.3759P] 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 2975 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Zn Zn 0.23217(3) 0.81312(3) 0.110789(14) 0.02696(10) Uani 1 1 d . . . C1 C 0.0061(2) 0.9170(3) -0.02218(11) 0.0219(5) Uani 1 1 d . . . H1A H -0.059(2) 0.926(3) -0.0666(13) 0.024(6) Uiso 1 1 d . . . N11 N 0.25431(19) 0.8604(2) 0.00132(10) 0.0248(4) Uani 1 1 d . . . C12 C 0.1479(2) 0.9002(3) -0.04723(12) 0.0229(5) Uani 1 1 d . . . C13 C 0.1654(2) 0.9305(3) -0.11910(12) 0.0284(5) Uani 1 1 d . . . H13A H 0.0894 0.9574 -0.1525 0.034 Uiso 1 1 calc R . . C14 C 0.2947(3) 0.9212(3) -0.14160(13) 0.0328(6) Uani 1 1 d . . . H14A H 0.3079 0.9409 -0.1904 0.039 Uiso 1 1 calc R . . C15 C 0.4044(3) 0.8826(3) -0.09154(14) 0.0342(6) Uani 1 1 d . . . H15A H 0.4939 0.8774 -0.1053 0.041 Uiso 1 1 calc R . . C16 C 0.3803(2) 0.8517(3) -0.02126(13) 0.0300(5) Uani 1 1 d . . . H16A H 0.4550 0.8233 0.0127 0.036 Uiso 1 1 calc R . . N21 N 0.03511(19) 0.7244(2) 0.08111(10) 0.0245(4) Uani 1 1 d . . . C22 C -0.0412(2) 0.7695(3) 0.01975(12) 0.0232(5) Uani 1 1 d . . . C23 C -0.1649(2) 0.6919(3) -0.00263(13) 0.0291(5) Uani 1 1 d . . . H23A H -0.2158 0.7238 -0.0464 0.035 Uiso 1 1 calc R . . C24 C -0.2123(3) 0.5678(3) 0.04005(14) 0.0347(6) Uani 1 1 d . . . H24A H -0.2969 0.5144 0.0263 0.042 Uiso 1 1 calc R . . C25 C -0.1348(3) 0.5223(3) 0.10328(14) 0.0330(6) Uani 1 1 d . . . H25A H -0.1656 0.4379 0.1335 0.040 Uiso 1 1 calc R . . C26 C -0.0119(2) 0.6020(3) 0.12145(12) 0.0292(5) Uani 1 1 d . . . H26A H 0.0418 0.5690 0.1642 0.035 Uiso 1 1 calc R . . O30 O 0.30577(18) 0.6140(3) 0.16084(11) 0.0449(5) Uani 1 1 d . . . C31 C 0.4332(2) 0.6079(3) 0.15810(13) 0.0304(5) Uani 1 1 d . . . O31 O 0.4961(2) 0.7204(3) 0.13023(14) 0.0718(7) Uani 1 1 d . . . C32 C 0.5100(3) 0.4658(4) 0.19785(15) 0.0409(6) Uani 1 1 d . . . H32A H 0.6015 0.4583 0.1826 0.061 Uiso 1 1 calc R . . H32B H 0.4617 0.3601 0.1870 0.061 Uiso 1 1 calc R . . H32C H 0.5165 0.4871 0.2496 0.061 Uiso 1 1 calc R . . O40 O 0.26388(17) 1.0438(2) 0.14691(9) 0.0333(4) Uani 1 1 d . . . C41 C 0.1915(2) 1.0602(3) 0.20032(12) 0.0297(5) Uani 1 1 d . . . O41 O 0.12624(18) 0.9421(2) 0.22243(10) 0.0397(4) Uani 1 1 d . . . C42 C 0.1884(3) 1.2316(3) 0.23410(14) 0.0370(6) Uani 1 1 d . . . H42A H 0.0969 1.2543 0.2472 0.055 Uiso 1 1 calc R . . H42B H 0.2126 1.3164 0.1998 0.055 Uiso 1 1 calc R . . H42C H 0.2537 1.2354 0.2773 0.055 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 Zn 0.02605(15) 0.02842(16) 0.02615(15) 0.00324(12) 0.00153(10) -0.00061(11) C1 0.0226(11) 0.0230(12) 0.0204(11) 0.0018(9) 0.0035(9) -0.0008(9) N11 0.0248(10) 0.0221(9) 0.0279(10) -0.0021(8) 0.0052(8) -0.0025(7) C12 0.0257(11) 0.0181(11) 0.0256(11) -0.0012(9) 0.0053(9) -0.0026(9) C13 0.0333(12) 0.0258(12) 0.0265(12) 0.0007(10) 0.0046(10) -0.0004(10) C14 0.0390(14) 0.0323(13) 0.0294(13) 0.0017(10) 0.0143(11) -0.0006(11) C15 0.0304(13) 0.0338(13) 0.0405(14) -0.0021(11) 0.0141(11) -0.0026(10) C16 0.0262(12) 0.0303(13) 0.0336(13) -0.0013(10) 0.0037(10) -0.0018(10) N21 0.0272(10) 0.0233(10) 0.0236(9) 0.0007(8) 0.0060(8) 0.0010(8) C22 0.0254(11) 0.0215(11) 0.0233(11) -0.0030(9) 0.0061(9) 0.0013(9) C23 0.0295(12) 0.0277(12) 0.0299(12) -0.0023(10) 0.0016(10) -0.0043(10) C24 0.0345(13) 0.0292(13) 0.0412(14) -0.0035(11) 0.0076(11) -0.0111(11) C25 0.0397(14) 0.0242(12) 0.0378(14) 0.0026(10) 0.0159(11) -0.0043(10) C26 0.0351(13) 0.0270(12) 0.0271(12) 0.0042(10) 0.0106(10) 0.0038(10) O30 0.0322(10) 0.0457(11) 0.0559(12) 0.0147(10) 0.0008(9) 0.0089(8) C31 0.0324(13) 0.0330(13) 0.0256(12) 0.0027(10) 0.0022(10) 0.0010(10) O31 0.0595(15) 0.0791(18) 0.0779(17) 0.0354(14) 0.0121(13) -0.0031(13) C32 0.0315(13) 0.0429(16) 0.0477(16) 0.0016(13) 0.0022(12) 0.0084(12) O40 0.0361(9) 0.0383(10) 0.0254(9) -0.0030(8) 0.0027(7) 0.0017(8) C41 0.0277(12) 0.0342(13) 0.0261(12) -0.0019(10) -0.0032(10) 0.0024(10) O41 0.0426(10) 0.0354(10) 0.0415(10) -0.0058(8) 0.0062(8) -0.0093(8) C42 0.0435(15) 0.0337(14) 0.0344(14) -0.0024(11) 0.0071(12) 0.0012(11) _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 Zn O30 1.9458(19) . ? Zn O40 1.9735(18) . ? Zn N21 2.094(2) . ? Zn N11 2.119(2) . ? C1 C22 1.516(3) . ? C1 C12 1.532(3) . ? C1 C1 1.574(4) 3_575 ? N11 C12 1.354(3) . ? N11 C16 1.360(3) . ? C12 C13 1.396(3) . ? C13 C14 1.391(3) . ? C14 C15 1.391(4) . ? C15 C16 1.384(3) . ? N21 C26 1.347(3) . ? N21 C22 1.355(3) . ? C22 C23 1.396(3) . ? C23 C24 1.385(3) . ? C24 C25 1.389(4) . ? C25 C26 1.382(3) . ? O30 C31 1.269(3) . ? C31 O31 1.238(3) . ? C31 C32 1.516(4) . ? O40 C41 1.297(3) . ? C41 O41 1.237(3) . ? C41 C42 1.508(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 O30 Zn O40 123.91(8) . . ? O30 Zn N21 98.20(8) . . ? O40 Zn N21 121.04(7) . . ? O30 Zn N11 122.66(8) . . ? O40 Zn N11 97.85(7) . . ? N21 Zn N11 89.57(7) . . ? C22 C1 C12 115.71(18) . . ? C22 C1 C1 109.5(2) . 3_575 ? C12 C1 C1 111.1(2) . 3_575 ? C12 N11 C16 118.45(19) . . ? C12 N11 Zn 122.59(14) . . ? C16 N11 Zn 118.96(16) . . ? N11 C12 C13 121.4(2) . . ? N11 C12 C1 119.16(19) . . ? C13 C12 C1 119.4(2) . . ? C14 C13 C12 119.7(2) . . ? C13 C14 C15 119.0(2) . . ? C16 C15 C14 118.6(2) . . ? N11 C16 C15 122.9(2) . . ? C26 N21 C22 118.3(2) . . ? C26 N21 Zn 117.61(16) . . ? C22 N21 Zn 123.72(15) . . ? N21 C22 C23 122.0(2) . . ? N21 C22 C1 118.05(19) . . ? C23 C22 C1 119.8(2) . . ? C24 C23 C22 118.9(2) . . ? C23 C24 C25 119.2(2) . . ? C26 C25 C24 118.8(2) . . ? N21 C26 C25 122.8(2) . . ? C31 O30 Zn 109.53(16) . . ? O31 C31 O30 122.4(2) . . ? O31 C31 C32 120.0(2) . . ? O30 C31 C32 117.2(2) . . ? C41 O40 Zn 106.10(15) . . ? O41 C41 O40 122.1(2) . . ? O41 C41 C42 121.0(2) . . ? O40 C41 C42 116.9(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 O30 Zn N11 C12 129.23(17) . . . . ? O40 Zn N11 C12 -91.55(17) . . . . ? N21 Zn N11 C12 29.75(17) . . . . ? O30 Zn N11 C16 -51.18(19) . . . . ? O40 Zn N11 C16 88.04(17) . . . . ? N21 Zn N11 C16 -150.66(17) . . . . ? C16 N11 C12 C13 0.5(3) . . . . ? Zn N11 C12 C13 -179.92(16) . . . . ? C16 N11 C12 C1 -177.72(19) . . . . ? Zn N11 C12 C1 1.9(3) . . . . ? C22 C1 C12 N11 -52.4(3) . . . . ? C1 C1 C12 N11 73.2(3) 3_575 . . . ? C22 C1 C12 C13 129.3(2) . . . . ? C1 C1 C12 C13 -105.0(3) 3_575 . . . ? N11 C12 C13 C14 -0.5(3) . . . . ? C1 C12 C13 C14 177.7(2) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? C13 C14 C15 C16 1.2(4) . . . . ? C12 N11 C16 C15 0.3(3) . . . . ? Zn N11 C16 C15 -179.26(19) . . . . ? C14 C15 C16 N11 -1.2(4) . . . . ? O30 Zn N21 C26 25.16(17) . . . . ? O40 Zn N21 C26 -112.96(16) . . . . ? N11 Zn N21 C26 148.12(17) . . . . ? O30 Zn N21 C22 -147.25(17) . . . . ? O40 Zn N21 C22 74.63(18) . . . . ? N11 Zn N21 C22 -24.28(17) . . . . ? C26 N21 C22 C23 -0.6(3) . . . . ? Zn N21 C22 C23 171.74(16) . . . . ? C26 N21 C22 C1 174.92(19) . . . . ? Zn N21 C22 C1 -12.7(3) . . . . ? C12 C1 C22 N21 58.6(3) . . . . ? C1 C1 C22 N21 -67.8(3) 3_575 . . . ? C12 C1 C22 C23 -125.7(2) . . . . ? C1 C1 C22 C23 107.8(3) 3_575 . . . ? N21 C22 C23 C24 1.4(3) . . . . ? C1 C22 C23 C24 -174.0(2) . . . . ? C22 C23 C24 C25 -0.9(4) . . . . ? C23 C24 C25 C26 -0.4(4) . . . . ? C22 N21 C26 C25 -0.7(3) . . . . ? Zn N21 C26 C25 -173.57(18) . . . . ? C24 C25 C26 N21 1.2(4) . . . . ? O40 Zn O30 C31 -70.60(19) . . . . ? N21 Zn O30 C31 152.96(17) . . . . ? N11 Zn O30 C31 58.2(2) . . . . ? Zn O30 C31 O31 3.4(3) . . . . ? Zn O30 C31 C32 176.75(18) . . . . ? O30 Zn O40 C41 -72.87(17) . . . . ? N21 Zn O40 C41 54.37(17) . . . . ? N11 Zn O40 C41 148.62(15) . . . . ? Zn O40 C41 O41 4.1(3) . . . . ? Zn O40 C41 C42 -175.08(17) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.580 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.060 #===END data_Compound-17 _database_code_CSD 216640 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 17 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H10 Ag N3 O3' _chemical_formula_weight 340.09 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' Ag Ag -0.8971 1.1015 '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 9.478(3) _cell_length_b 14.189(4) _cell_length_c 9.136(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.702(4) _cell_angle_gamma 90.00 _cell_volume 1149.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 5009 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.38 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.857764 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 11743 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 26.39 _reflns_number_total 2245 _reflns_number_gt 1795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0326P)^2^+0.5163P] 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 2245 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Ag Ag -0.00249(3) 0.163154(18) 0.05043(3) 0.03335(10) Uani 1 1 d . . . C1 C 0.1272(3) 0.3605(2) -0.0624(4) 0.0308(7) Uani 1 1 d . . . H1A H 0.1626 0.3688 0.0526 0.037 Uiso 1 1 calc R . . H1B H 0.1607 0.4163 -0.1064 0.037 Uiso 1 1 calc R . . N1 N 0.1596(3) 0.18839(18) -0.0657(3) 0.0259(6) Uani 1 1 d . . . C2 C 0.2037(3) 0.2741(2) -0.0977(3) 0.0244(6) Uani 1 1 d . . . C3 C 0.3203(3) 0.2832(2) -0.1540(4) 0.0289(7) Uani 1 1 d . . . H3A H 0.3501 0.3438 -0.1761 0.035 Uiso 1 1 calc R . . C4 C 0.3937(3) 0.2037(2) -0.1781(4) 0.0323(7) Uani 1 1 d . . . H4A H 0.4747 0.2094 -0.2159 0.039 Uiso 1 1 calc R . . C5 C 0.3479(3) 0.1158(2) -0.1466(4) 0.0311(7) Uani 1 1 d . . . H5A H 0.3963 0.0602 -0.1624 0.037 Uiso 1 1 calc R . . C6 C 0.2308(3) 0.1114(2) -0.0920(3) 0.0307(7) Uani 1 1 d . . . H6A H 0.1980 0.0511 -0.0716 0.037 Uiso 1 1 calc R . . N11 N -0.1151(3) 0.34707(16) -0.2788(3) 0.0249(5) Uani 1 1 d . . . C12 C -0.0428(3) 0.3590(2) -0.1239(4) 0.0264(7) Uani 1 1 d . . . C13 C -0.1237(4) 0.3752(2) -0.0261(4) 0.0330(7) Uani 1 1 d . . . H13A H -0.0721 0.3826 0.0832 0.040 Uiso 1 1 calc R . . C14 C -0.2797(4) 0.3807(2) -0.0876(4) 0.0362(8) Uani 1 1 d . . . H14A H -0.3357 0.3927 -0.0215 0.043 Uiso 1 1 calc R . . C15 C -0.3519(3) 0.3684(2) -0.2456(4) 0.0309(7) Uani 1 1 d . . . H15A H -0.4587 0.3723 -0.2911 0.037 Uiso 1 1 calc R . . C16 C -0.2667(3) 0.3504(2) -0.3362(4) 0.0294(7) Uani 1 1 d . . . H16A H -0.3171 0.3397 -0.4450 0.035 Uiso 1 1 calc R . . N20 N 0.2596(3) -0.05888(19) 0.2093(3) 0.0304(6) Uani 1 1 d . . . O21 O 0.2684(3) -0.14546(15) 0.1914(3) 0.0397(6) Uani 1 1 d . . . O22 O 0.1321(3) -0.01995(17) 0.1579(3) 0.0463(6) Uani 1 1 d . . . O23 O 0.3746(3) -0.01184(18) 0.2772(3) 0.0550(7) 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 Ag 0.03154(15) 0.04307(17) 0.03204(14) 0.00002(12) 0.01940(11) -0.00543(12) C1 0.0283(16) 0.0317(19) 0.0331(17) -0.0045(13) 0.0116(14) -0.0014(13) N1 0.0235(13) 0.0323(15) 0.0238(13) 0.0027(10) 0.0105(10) 0.0006(11) C2 0.0218(14) 0.0288(17) 0.0205(14) 0.0011(12) 0.0047(12) 0.0000(13) C3 0.0251(16) 0.0300(18) 0.0323(16) 0.0058(13) 0.0110(13) -0.0024(13) C4 0.0238(15) 0.044(2) 0.0322(17) 0.0016(15) 0.0145(14) 0.0006(15) C5 0.0296(16) 0.0335(19) 0.0305(16) -0.0001(14) 0.0108(14) 0.0057(14) C6 0.0325(17) 0.0290(18) 0.0302(16) 0.0018(13) 0.0107(14) -0.0007(14) N11 0.0236(12) 0.0262(14) 0.0279(13) 0.0006(10) 0.0128(11) 0.0024(11) C12 0.0280(15) 0.0231(17) 0.0305(16) 0.0012(12) 0.0135(13) 0.0042(12) C13 0.0379(18) 0.0351(18) 0.0303(16) -0.0041(14) 0.0175(15) 0.0002(15) C14 0.0365(18) 0.0403(19) 0.042(2) -0.0016(16) 0.0268(16) 0.0033(16) C15 0.0254(16) 0.0313(18) 0.0392(18) 0.0052(14) 0.0154(14) 0.0029(13) C16 0.0290(16) 0.0312(19) 0.0296(16) 0.0033(13) 0.0124(13) 0.0000(14) N20 0.0367(16) 0.0338(16) 0.0257(13) 0.0006(11) 0.0172(12) -0.0034(13) O21 0.0423(14) 0.0284(14) 0.0484(14) -0.0071(10) 0.0161(12) 0.0020(10) O22 0.0384(14) 0.0359(14) 0.0625(16) 0.0088(12) 0.0151(12) 0.0100(11) O23 0.0406(15) 0.0470(16) 0.0730(18) -0.0121(14) 0.0146(13) -0.0146(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 Ag N1 2.183(2) . ? Ag N11 2.184(2) 4_566 ? C1 C12 1.507(4) . ? C1 C2 1.515(4) . ? N1 C6 1.349(4) . ? N1 C2 1.351(4) . ? C2 C3 1.380(4) . ? C3 C4 1.383(4) . ? C4 C5 1.383(5) . ? C5 C6 1.371(4) . ? N11 C16 1.345(4) . ? N11 C12 1.347(4) . ? N11 Ag 2.184(2) 4_565 ? C12 C13 1.387(4) . ? C13 C14 1.386(4) . ? C14 C15 1.373(5) . ? C15 C16 1.370(4) . ? N20 O23 1.241(3) . ? N20 O21 1.246(3) . ? N20 O22 1.258(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 N1 Ag N11 164.46(9) . 4_566 ? C12 C1 C2 115.9(2) . . ? C6 N1 C2 118.6(3) . . ? C6 N1 Ag 115.8(2) . . ? C2 N1 Ag 125.25(19) . . ? N1 C2 C3 120.9(3) . . ? N1 C2 C1 118.3(3) . . ? C3 C2 C1 120.7(3) . . ? C2 C3 C4 119.9(3) . . ? C5 C4 C3 119.3(3) . . ? C6 C5 C4 118.1(3) . . ? N1 C6 C5 123.2(3) . . ? C16 N11 C12 118.8(2) . . ? C16 N11 Ag 116.63(19) . 4_565 ? C12 N11 Ag 124.26(19) . 4_565 ? N11 C12 C13 120.4(3) . . ? N11 C12 C1 118.3(3) . . ? C13 C12 C1 121.2(3) . . ? C14 C13 C12 120.1(3) . . ? C15 C14 C13 118.9(3) . . ? C16 C15 C14 118.6(3) . . ? N11 C16 C15 123.2(3) . . ? O23 N20 O21 120.5(3) . . ? O23 N20 O22 120.5(3) . . ? O21 N20 O22 118.9(3) . . ? 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 N11 Ag N1 C6 103.2(4) 4_566 . . . ? N11 Ag N1 C2 -69.9(4) 4_566 . . . ? C6 N1 C2 C3 -0.9(4) . . . . ? Ag N1 C2 C3 171.9(2) . . . . ? C6 N1 C2 C1 -177.8(3) . . . . ? Ag N1 C2 C1 -5.0(4) . . . . ? C12 C1 C2 N1 -49.8(4) . . . . ? C12 C1 C2 C3 133.3(3) . . . . ? N1 C2 C3 C4 -0.1(4) . . . . ? C1 C2 C3 C4 176.8(3) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C2 N1 C6 C5 1.4(4) . . . . ? Ag N1 C6 C5 -172.1(2) . . . . ? C4 C5 C6 N1 -0.9(5) . . . . ? C16 N11 C12 C13 -0.6(4) . . . . ? Ag N11 C12 C13 172.8(2) 4_565 . . . ? C16 N11 C12 C1 -176.7(3) . . . . ? Ag N11 C12 C1 -3.2(4) 4_565 . . . ? C2 C1 C12 N11 -57.3(4) . . . . ? C2 C1 C12 C13 126.7(3) . . . . ? N11 C12 C13 C14 -0.9(5) . . . . ? C1 C12 C13 C14 175.0(3) . . . . ? C12 C13 C14 C15 0.9(5) . . . . ? C13 C14 C15 C16 0.6(5) . . . . ? C12 N11 C16 C15 2.2(4) . . . . ? Ag N11 C16 C15 -171.7(2) 4_565 . . . ? C14 C15 C16 N11 -2.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.969 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.077 #===END data_Compound-18 _database_code_CSD 216641 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 18 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cl2 N2 O2 Pd' _chemical_formula_weight 393.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 9.106(3) _cell_length_b 11.784(5) _cell_length_c 12.625(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.509(15) _cell_angle_gamma 90.00 _cell_volume 1354.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 4157 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 26.35 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.930 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.831089 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 9676 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.45 _reflns_number_total 2761 _reflns_number_gt 2233 _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^)+(0.0323P)^2^+1.3477P] 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 2761 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _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 Pd1 Pd 0.19478(3) 0.57256(2) 0.22801(2) 0.02226(10) Uani 1 1 d . . . Cl1 Cl -0.03268(10) 0.60972(10) 0.15330(8) 0.0363(2) Uani 1 1 d . . . Cl2 Cl 0.09252(10) 0.51637(9) 0.38319(7) 0.0312(2) Uani 1 1 d . . . C1 C 0.4574(4) 0.7292(3) 0.2185(3) 0.0237(8) Uani 1 1 d . . . O1 O 0.3307(3) 0.7782(2) 0.2650(2) 0.0359(7) Uiso 1 1 d . . . O2 O 0.5718(3) 0.8048(3) 0.2199(2) 0.0402(7) Uiso 1 1 d . . . H2A H 0.5470 0.8634 0.1859 0.060 Uiso 1 1 calc R . . C3 C 0.3496(5) 0.8025(4) 0.3780(3) 0.0457(11) Uiso 1 1 d . . . H3A H 0.2589 0.8356 0.4045 0.069 Uiso 1 1 calc R . . H3B H 0.4307 0.8563 0.3889 0.069 Uiso 1 1 calc R . . H3C H 0.3718 0.7320 0.4163 0.069 Uiso 1 1 calc R . . N11 N 0.2950(3) 0.6252(3) 0.0951(2) 0.0230(7) Uani 1 1 d . . . C12 C 0.4101(4) 0.6964(3) 0.1058(3) 0.0251(8) Uani 1 1 d . . . C13 C 0.4836(4) 0.7331(3) 0.0184(3) 0.0322(9) Uani 1 1 d . . . H13A H 0.5638 0.7842 0.0264 0.039 Uiso 1 1 calc R . . C14 C 0.4396(5) 0.6949(4) -0.0823(3) 0.0366(10) Uani 1 1 d . . . H14A H 0.4894 0.7194 -0.1434 0.044 Uiso 1 1 calc R . . C15 C 0.3222(4) 0.6207(4) -0.0914(3) 0.0334(9) Uani 1 1 d . . . H15A H 0.2906 0.5926 -0.1588 0.040 Uiso 1 1 calc R . . C16 C 0.2524(4) 0.5884(3) -0.0015(3) 0.0293(9) Uani 1 1 d . . . H16A H 0.1709 0.5383 -0.0077 0.035 Uiso 1 1 calc R . . N21 N 0.4010(3) 0.5414(2) 0.2891(2) 0.0209(6) Uani 1 1 d . . . C22 C 0.5051(4) 0.6224(3) 0.2780(3) 0.0225(8) Uani 1 1 d . . . C23 C 0.6457(4) 0.6058(3) 0.3177(3) 0.0283(9) Uani 1 1 d . . . H23A H 0.7188 0.6623 0.3086 0.034 Uiso 1 1 calc R . . C24 C 0.6798(4) 0.5059(4) 0.3709(3) 0.0340(10) Uani 1 1 d . . . H24A H 0.7754 0.4940 0.4009 0.041 Uiso 1 1 calc R . . C25 C 0.5735(4) 0.4246(4) 0.3796(3) 0.0328(9) Uani 1 1 d . . . H25A H 0.5956 0.3548 0.4142 0.039 Uiso 1 1 calc R . . C26 C 0.4348(4) 0.4440(3) 0.3382(3) 0.0274(9) Uani 1 1 d . . . H26A H 0.3616 0.3871 0.3446 0.033 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 Pd1 0.02037(15) 0.02648(16) 0.01998(15) -0.00062(13) 0.00145(11) -0.00333(13) Cl1 0.0232(4) 0.0492(7) 0.0362(5) -0.0031(5) -0.0039(4) -0.0001(4) Cl2 0.0316(5) 0.0381(6) 0.0243(5) -0.0013(4) 0.0085(4) -0.0066(4) C1 0.0210(17) 0.025(2) 0.0252(19) 0.0012(16) 0.0016(15) -0.0067(15) N11 0.0240(15) 0.0241(17) 0.0208(15) 0.0013(13) -0.0019(13) -0.0018(13) C12 0.0276(18) 0.025(2) 0.0225(18) 0.0032(16) 0.0012(16) 0.0024(16) C13 0.036(2) 0.028(2) 0.032(2) 0.0027(18) 0.0083(18) -0.0035(17) C14 0.048(2) 0.038(3) 0.024(2) 0.0071(19) 0.0104(19) 0.001(2) C15 0.042(2) 0.039(2) 0.0196(19) -0.0006(18) -0.0003(18) 0.0028(19) C16 0.033(2) 0.030(2) 0.0246(19) -0.0008(17) -0.0024(17) -0.0029(17) N21 0.0235(15) 0.0202(16) 0.0190(15) -0.0027(12) 0.0008(13) 0.0007(12) C22 0.0242(18) 0.024(2) 0.0197(17) -0.0038(16) 0.0026(15) -0.0010(15) C23 0.0244(19) 0.030(2) 0.030(2) -0.0055(17) 0.0016(17) -0.0017(16) C24 0.026(2) 0.043(3) 0.032(2) -0.007(2) -0.0024(18) 0.0105(19) C25 0.040(2) 0.032(2) 0.027(2) 0.0045(19) 0.0010(18) 0.0088(19) C26 0.034(2) 0.020(2) 0.0277(19) 0.0018(16) 0.0033(17) 0.0013(16) _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 Pd1 N11 2.028(3) . ? Pd1 N21 2.044(3) . ? Pd1 Cl2 2.2891(11) . ? Pd1 Cl1 2.2953(12) . ? C1 O2 1.370(4) . ? C1 O1 1.430(4) . ? C1 C22 1.524(5) . ? C1 C12 1.525(5) . ? O1 C3 1.460(5) . ? N11 C16 1.342(5) . ? N11 C12 1.346(5) . ? C12 C13 1.376(5) . ? C13 C14 1.397(5) . ? C14 C15 1.384(6) . ? C15 C16 1.369(5) . ? N21 C26 1.337(4) . ? N21 C22 1.355(5) . ? C22 C23 1.377(5) . ? C23 C24 1.387(6) . ? C24 C25 1.368(6) . ? C25 C26 1.372(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Pd1 N21 86.44(12) . . ? N11 Pd1 Cl2 176.91(8) . . ? N21 Pd1 Cl2 90.89(9) . . ? N11 Pd1 Cl1 91.29(9) . . ? N21 Pd1 Cl1 177.74(8) . . ? Cl2 Pd1 Cl1 91.37(4) . . ? O2 C1 O1 110.7(3) . . ? O2 C1 C22 108.9(3) . . ? O1 C1 C22 110.7(3) . . ? O2 C1 C12 111.9(3) . . ? O1 C1 C12 105.9(3) . . ? C22 C1 C12 108.7(3) . . ? C1 O1 C3 113.9(3) . . ? C16 N11 C12 119.9(3) . . ? C16 N11 Pd1 121.8(3) . . ? C12 N11 Pd1 118.3(2) . . ? N11 C12 C13 120.6(3) . . ? N11 C12 C1 116.8(3) . . ? C13 C12 C1 122.5(3) . . ? C12 C13 C14 119.6(4) . . ? C15 C14 C13 118.8(4) . . ? C16 C15 C14 118.7(4) . . ? N11 C16 C15 122.3(4) . . ? C26 N21 C22 119.9(3) . . ? C26 N21 Pd1 121.8(2) . . ? C22 N21 Pd1 118.2(2) . . ? N21 C22 C23 120.6(3) . . ? N21 C22 C1 116.2(3) . . ? C23 C22 C1 123.2(3) . . ? C22 C23 C24 119.4(4) . . ? C25 C24 C23 118.9(4) . . ? C24 C25 C26 119.9(4) . . ? N21 C26 C25 121.2(4) . . ? 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 O2 C1 O1 C3 -65.6(4) . . . . ? C22 C1 O1 C3 55.3(4) . . . . ? C12 C1 O1 C3 172.9(3) . . . . ? N21 Pd1 N11 C16 131.2(3) . . . . ? Cl2 Pd1 N11 C16 161.8(15) . . . . ? Cl1 Pd1 N11 C16 -48.8(3) . . . . ? N21 Pd1 N11 C12 -46.8(3) . . . . ? Cl2 Pd1 N11 C12 -16.3(19) . . . . ? Cl1 Pd1 N11 C12 133.2(3) . . . . ? C16 N11 C12 C13 0.8(5) . . . . ? Pd1 N11 C12 C13 178.8(3) . . . . ? C16 N11 C12 C1 -176.7(3) . . . . ? Pd1 N11 C12 C1 1.4(4) . . . . ? O2 C1 C12 N11 -177.9(3) . . . . ? O1 C1 C12 N11 -57.1(4) . . . . ? C22 C1 C12 N11 61.8(4) . . . . ? O2 C1 C12 C13 4.7(5) . . . . ? O1 C1 C12 C13 125.4(4) . . . . ? C22 C1 C12 C13 -115.6(4) . . . . ? N11 C12 C13 C14 -0.9(6) . . . . ? C1 C12 C13 C14 176.5(4) . . . . ? C12 C13 C14 C15 0.1(6) . . . . ? C13 C14 C15 C16 0.7(6) . . . . ? C12 N11 C16 C15 0.1(6) . . . . ? Pd1 N11 C16 C15 -177.9(3) . . . . ? C14 C15 C16 N11 -0.8(6) . . . . ? N11 Pd1 N21 C26 -132.8(3) . . . . ? Cl2 Pd1 N21 C26 48.8(3) . . . . ? Cl1 Pd1 N21 C26 -131(2) . . . . ? N11 Pd1 N21 C22 46.7(3) . . . . ? Cl2 Pd1 N21 C22 -131.7(2) . . . . ? Cl1 Pd1 N21 C22 48(2) . . . . ? C26 N21 C22 C23 -0.5(5) . . . . ? Pd1 N21 C22 C23 180.0(3) . . . . ? C26 N21 C22 C1 178.5(3) . . . . ? Pd1 N21 C22 C1 -1.1(4) . . . . ? O2 C1 C22 N21 176.3(3) . . . . ? O1 C1 C22 N21 54.4(4) . . . . ? C12 C1 C22 N21 -61.5(4) . . . . ? O2 C1 C22 C23 -4.7(5) . . . . ? O1 C1 C22 C23 -126.7(3) . . . . ? C12 C1 C22 C23 117.4(4) . . . . ? N21 C22 C23 C24 -1.1(5) . . . . ? C1 C22 C23 C24 -180.0(3) . . . . ? C22 C23 C24 C25 2.1(6) . . . . ? C23 C24 C25 C26 -1.6(6) . . . . ? C22 N21 C26 C25 1.0(5) . . . . ? Pd1 N21 C26 C25 -179.5(3) . . . . ? C24 C25 C26 N21 0.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.664 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.092 #===END data_Compound-19 _database_code_CSD 216642 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 19 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H22 Cu N6 O11' _chemical_formula_weight 610.00 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 Cc 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' _cell_length_a 8.000(2) _cell_length_b 32.264(8) _cell_length_c 9.563(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.962(3) _cell_angle_gamma 90.00 _cell_volume 2444.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 6890 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 26.34 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.845185 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 15172 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0125 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 26.34 _reflns_number_total 4267 _reflns_number_gt 4177 _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^)+(0.0462P)^2^+2.1694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(8) _refine_ls_number_reflns 4267 _refine_ls_number_parameters 361 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.21917(3) 0.128744(7) 0.01299(3) 0.01935(8) Uani 1 1 d . . . C1 C 0.0855(3) 0.04888(7) -0.0722(3) 0.0203(5) Uani 1 1 d . . . O2 O 0.2553(2) 0.05544(5) -0.00759(18) 0.0213(4) Uani 1 1 d . . . H2A H 0.2641 0.0474 0.0747 0.032 Uiso 1 1 d R . . O3 O 0.0479(2) 0.00725(5) -0.09650(19) 0.0246(4) Uani 1 1 d . . . H3A H 0.1085 -0.0010 -0.1195 0.037 Uiso 1 1 d R . . N11 N 0.1150(3) 0.11492(6) -0.1855(2) 0.0203(4) Uani 1 1 d . . . C12 C 0.0640(3) 0.07535(7) -0.2052(3) 0.0197(5) Uani 1 1 d . . . C13 C -0.0098(3) 0.06081(8) -0.3359(3) 0.0246(5) Uani 1 1 d . . . H13A H -0.0449 0.0328 -0.3480 0.030 Uiso 1 1 calc R . . C14 C -0.0308(4) 0.08812(9) -0.4477(3) 0.0312(6) Uani 1 1 d . . . H14A H -0.0807 0.0790 -0.5383 0.037 Uiso 1 1 calc R . . C15 C 0.0214(4) 0.12926(8) -0.4278(3) 0.0298(7) Uani 1 1 d . . . H15A H 0.0068 0.1484 -0.5040 0.036 Uiso 1 1 calc R . . C16 C 0.0946(3) 0.14143(9) -0.2953(3) 0.0257(5) Uani 1 1 d . . . H16A H 0.1317 0.1693 -0.2810 0.031 Uiso 1 1 calc R . . N21 N 0.0110(3) 0.10368(6) 0.0791(2) 0.0204(4) Uani 1 1 d . . . C22 C -0.0352(3) 0.06610(7) 0.0240(3) 0.0192(5) Uani 1 1 d . . . C23 C -0.1809(3) 0.04628(8) 0.0503(3) 0.0245(5) Uani 1 1 d . . . H23A H -0.2125 0.0203 0.0082 0.029 Uiso 1 1 calc R . . C24 C -0.2798(3) 0.06537(8) 0.1399(3) 0.0297(6) Uani 1 1 d . . . H24A H -0.3787 0.0521 0.1624 0.036 Uiso 1 1 calc R . . C25 C -0.2327(3) 0.10396(9) 0.1962(3) 0.0290(5) Uani 1 1 d . . . H25A H -0.3001 0.1176 0.2565 0.035 Uiso 1 1 calc R . . C26 C -0.0868(4) 0.12246(9) 0.1637(3) 0.0259(6) Uani 1 1 d . . . H26A H -0.0550 0.1489 0.2019 0.031 Uiso 1 1 calc R . . C31 C 0.3651(3) 0.20857(7) 0.0653(3) 0.0223(5) Uani 1 1 d . . . O32 O 0.1968(2) 0.20043(5) -0.0025(2) 0.0227(4) Uani 1 1 d . . . H32A H 0.1191 0.2115 0.0556 0.034 Uiso 1 1 d R . . O33 O 0.3969(2) 0.25069(5) 0.0828(2) 0.0278(4) Uani 1 1 d . . . H33A H 0.3932 0.2552 -0.0116 0.042 Uiso 1 1 d R . . N41 N 0.4324(3) 0.14716(6) -0.0590(2) 0.0204(4) Uani 1 1 d . . . C42 C 0.4814(3) 0.18646(7) -0.0244(3) 0.0213(5) Uani 1 1 d . . . C43 C 0.6269(3) 0.20350(8) -0.0622(3) 0.0271(5) Uani 1 1 d . . . H43A H 0.6620 0.2306 -0.0325 0.033 Uiso 1 1 calc R . . C44 C 0.7200(3) 0.18003(9) -0.1444(3) 0.0306(6) Uani 1 1 d . . . H44A H 0.8191 0.1912 -0.1741 0.037 Uiso 1 1 calc R . . C45 C 0.6688(3) 0.14011(9) -0.1836(3) 0.0285(5) Uani 1 1 d . . . H45A H 0.7316 0.1238 -0.2406 0.034 Uiso 1 1 calc R . . C46 C 0.5233(4) 0.12448(8) -0.1378(3) 0.0241(6) Uani 1 1 d . . . H46A H 0.4879 0.0971 -0.1632 0.029 Uiso 1 1 calc R . . N51 N 0.3234(3) 0.14862(6) 0.2074(2) 0.0219(4) Uani 1 1 d . . . C52 C 0.3884(3) 0.18743(7) 0.2098(3) 0.0225(5) Uani 1 1 d . . . C53 C 0.4720(4) 0.20529(8) 0.3312(3) 0.0306(6) Uani 1 1 d . . . H53A H 0.5173 0.2325 0.3299 0.037 Uiso 1 1 calc R . . C54 C 0.4879(4) 0.18224(9) 0.4558(3) 0.0364(7) Uani 1 1 d . . . H54A H 0.5446 0.1935 0.5411 0.044 Uiso 1 1 calc R . . C55 C 0.4202(4) 0.14273(9) 0.4537(3) 0.0328(7) Uani 1 1 d . . . H55A H 0.4300 0.1266 0.5376 0.039 Uiso 1 1 calc R . . C56 C 0.3374(4) 0.12686(7) 0.3272(3) 0.0264(6) Uani 1 1 d . . . H56A H 0.2897 0.0999 0.3262 0.032 Uiso 1 1 calc R . . N60 N 0.4004(3) 0.26515(7) 0.7301(3) 0.0370(6) Uani 1 1 d . . . O61 O 0.4552(3) 0.26691(8) 0.6150(3) 0.0524(6) Uani 1 1 d . . . O62 O 0.2936(3) 0.23720(8) 0.7373(3) 0.0594(7) Uani 1 1 d . . . O63 O 0.4486(6) 0.28872(8) 0.8270(3) 0.0844(12) Uani 1 1 d . . . N70 N 0.0187(3) 0.45737(6) 0.0613(3) 0.0306(5) Uani 1 1 d . . . O71 O 0.0717(3) 0.45976(7) -0.0565(2) 0.0420(5) Uani 1 1 d . . . O72 O -0.1360(3) 0.45120(7) 0.0642(3) 0.0406(5) Uani 1 1 d . . . O73 O 0.1173(3) 0.46154(8) 0.1724(3) 0.0503(6) Uani 1 1 d . . . O80 O 0.3013(2) 0.01537(5) 0.2445(2) 0.0285(4) Uani 1 1 d . . . H80A H 0.3275 -0.0059 0.2109 0.043 Uiso 1 1 d R . . H80B H 0.3866 0.0220 0.3119 0.043 Uiso 1 1 d 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 0.02225(13) 0.01872(12) 0.01763(13) -0.00045(12) 0.00467(9) -0.00287(11) C1 0.0199(11) 0.0184(10) 0.0229(12) -0.0024(9) 0.0044(9) -0.0027(8) O2 0.0219(9) 0.0210(7) 0.0210(9) 0.0035(6) 0.0028(6) -0.0001(6) O3 0.0281(9) 0.0152(8) 0.0320(10) -0.0028(7) 0.0092(8) -0.0002(6) N11 0.0222(10) 0.0199(9) 0.0197(11) 0.0021(8) 0.0057(8) -0.0025(8) C12 0.0186(10) 0.0207(10) 0.0209(12) 0.0004(9) 0.0068(9) 0.0016(8) C13 0.0276(12) 0.0236(11) 0.0226(13) -0.0058(9) 0.0032(10) -0.0014(9) C14 0.0343(14) 0.0387(14) 0.0195(13) -0.0029(10) -0.0003(11) 0.0009(11) C15 0.0337(15) 0.0332(15) 0.0229(15) 0.0082(10) 0.0055(11) 0.0043(10) C16 0.0278(13) 0.0262(12) 0.0241(14) 0.0044(11) 0.0069(10) 0.0004(10) N21 0.0236(10) 0.0210(9) 0.0172(10) 0.0003(7) 0.0048(8) 0.0008(7) C22 0.0219(11) 0.0174(9) 0.0186(11) 0.0041(8) 0.0033(9) -0.0012(8) C23 0.0225(12) 0.0246(11) 0.0265(13) 0.0026(9) 0.0037(10) -0.0026(9) C24 0.0228(12) 0.0363(14) 0.0316(15) 0.0087(11) 0.0098(10) -0.0008(10) C25 0.0283(13) 0.0387(13) 0.0222(13) 0.0015(11) 0.0118(10) 0.0076(11) C26 0.0286(16) 0.0292(13) 0.0198(15) -0.0003(11) 0.0035(12) 0.0041(10) C31 0.0251(12) 0.0179(10) 0.0243(13) 0.0003(9) 0.0045(10) -0.0001(9) O32 0.0228(10) 0.0224(7) 0.0230(10) 0.0013(7) 0.0035(7) 0.0001(7) O33 0.0379(10) 0.0184(8) 0.0276(10) -0.0013(7) 0.0059(8) -0.0033(7) N41 0.0229(10) 0.0202(9) 0.0185(10) 0.0010(8) 0.0039(8) 0.0005(7) C42 0.0244(12) 0.0216(10) 0.0176(11) 0.0030(9) 0.0021(9) 0.0011(9) C43 0.0252(13) 0.0264(12) 0.0295(14) 0.0048(10) 0.0026(10) -0.0024(9) C44 0.0231(13) 0.0379(14) 0.0317(15) 0.0059(11) 0.0069(11) -0.0015(10) C45 0.0236(13) 0.0377(13) 0.0247(14) 0.0009(11) 0.0051(10) 0.0058(10) C46 0.0243(15) 0.0265(13) 0.0216(15) -0.0011(10) 0.0039(12) 0.0021(10) N51 0.0260(10) 0.0195(10) 0.0208(11) 0.0009(8) 0.0054(8) 0.0016(7) C52 0.0234(11) 0.0215(11) 0.0235(12) -0.0017(9) 0.0061(9) -0.0008(8) C53 0.0397(15) 0.0238(12) 0.0276(14) -0.0049(10) 0.0019(11) -0.0036(10) C54 0.0510(17) 0.0329(14) 0.0227(14) -0.0046(11) -0.0035(12) -0.0009(12) C55 0.0463(17) 0.0299(14) 0.0217(15) 0.0013(11) 0.0032(12) 0.0015(12) C56 0.0302(14) 0.0245(13) 0.0258(15) 0.0000(10) 0.0087(11) -0.0028(9) N60 0.0474(15) 0.0317(12) 0.0334(14) 0.0111(10) 0.0110(11) 0.0113(11) O61 0.0463(14) 0.0705(16) 0.0439(14) 0.0014(12) 0.0186(11) -0.0169(12) O62 0.0519(15) 0.0624(16) 0.0651(18) 0.0253(13) 0.0124(13) -0.0136(12) O63 0.175(4) 0.0318(12) 0.0383(15) 0.0022(10) -0.0131(18) 0.0103(16) N70 0.0299(12) 0.0263(10) 0.0370(13) 0.0019(9) 0.0098(10) 0.0015(9) O71 0.0385(11) 0.0518(13) 0.0388(12) -0.0020(9) 0.0167(9) -0.0015(9) O72 0.0315(11) 0.0388(10) 0.0552(14) -0.0104(9) 0.0188(10) -0.0036(8) O73 0.0389(12) 0.0714(16) 0.0398(13) 0.0080(12) 0.0025(10) -0.0008(11) O80 0.0352(10) 0.0255(9) 0.0262(10) 0.0041(7) 0.0097(8) 0.0020(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 2.014(2) . ? Cu1 N41 2.015(2) . ? Cu1 N21 2.029(2) . ? Cu1 N51 2.033(2) . ? Cu1 O32 2.3229(16) . ? Cu1 O2 2.3942(17) . ? C1 O3 1.389(3) . ? C1 O2 1.428(3) . ? C1 C12 1.522(3) . ? C1 C22 1.528(3) . ? N11 C12 1.346(3) . ? N11 C16 1.347(3) . ? C12 C13 1.388(3) . ? C13 C14 1.377(4) . ? C14 C15 1.397(4) . ? C15 C16 1.378(4) . ? N21 C26 1.345(4) . ? N21 C22 1.353(3) . ? C22 C23 1.383(3) . ? C23 C24 1.388(4) . ? C24 C25 1.388(4) . ? C25 C26 1.384(5) . ? C31 O33 1.388(3) . ? C31 O32 1.435(3) . ? C31 C42 1.527(3) . ? C31 C52 1.529(4) . ? N41 C46 1.336(4) . ? N41 C42 1.355(3) . ? C42 C43 1.379(4) . ? C43 C44 1.382(4) . ? C44 C45 1.388(4) . ? C45 C46 1.394(5) . ? N51 C56 1.335(4) . ? N51 C52 1.355(3) . ? C52 C53 1.383(4) . ? C53 C54 1.395(4) . ? C54 C55 1.384(4) . ? C55 C56 1.394(4) . ? N60 O63 1.219(4) . ? N60 O61 1.242(3) . ? N60 O62 1.251(4) . ? N70 O73 1.240(3) . ? N70 O72 1.257(3) . ? N70 O71 1.259(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 N11 Cu1 N41 90.15(8) . . ? N11 Cu1 N21 87.42(8) . . ? N41 Cu1 N21 173.59(8) . . ? N11 Cu1 N51 174.38(8) . . ? N41 Cu1 N51 87.70(9) . . ? N21 Cu1 N51 95.24(8) . . ? N11 Cu1 O32 98.19(7) . . ? N41 Cu1 O32 75.29(7) . . ? N21 Cu1 O32 110.93(8) . . ? N51 Cu1 O32 76.25(7) . . ? N11 Cu1 O2 75.09(7) . . ? N41 Cu1 O2 98.37(7) . . ? N21 Cu1 O2 75.27(7) . . ? N51 Cu1 O2 110.36(7) . . ? O32 Cu1 O2 170.93(7) . . ? O3 C1 O2 112.75(19) . . ? O3 C1 C12 113.9(2) . . ? O2 C1 C12 105.60(18) . . ? O3 C1 C22 108.20(19) . . ? O2 C1 C22 109.17(19) . . ? C12 C1 C22 106.95(18) . . ? C1 O2 Cu1 93.63(12) . . ? C12 N11 C16 119.5(2) . . ? C12 N11 Cu1 114.84(16) . . ? C16 N11 Cu1 125.70(18) . . ? N11 C12 C13 122.0(2) . . ? N11 C12 C1 114.7(2) . . ? C13 C12 C1 123.2(2) . . ? C14 C13 C12 118.3(2) . . ? C13 C14 C15 120.0(2) . . ? C16 C15 C14 118.5(3) . . ? N11 C16 C15 121.8(3) . . ? C26 N21 C22 119.2(2) . . ? C26 N21 Cu1 125.36(19) . . ? C22 N21 Cu1 115.32(16) . . ? N21 C22 C23 122.4(2) . . ? N21 C22 C1 113.5(2) . . ? C23 C22 C1 124.1(2) . . ? C22 C23 C24 118.3(2) . . ? C25 C24 C23 119.4(2) . . ? C26 C25 C24 119.4(3) . . ? N21 C26 C25 121.3(3) . . ? O33 C31 O32 112.23(18) . . ? O33 C31 C42 114.1(2) . . ? O32 C31 C42 105.50(19) . . ? O33 C31 C52 109.3(2) . . ? O32 C31 C52 108.4(2) . . ? C42 C31 C52 106.95(19) . . ? C31 O32 Cu1 95.41(12) . . ? C46 N41 C42 119.3(2) . . ? C46 N41 Cu1 125.71(18) . . ? C42 N41 Cu1 115.02(16) . . ? N41 C42 C43 122.4(2) . . ? N41 C42 C31 113.3(2) . . ? C43 C42 C31 124.2(2) . . ? C42 C43 C44 118.1(2) . . ? C43 C44 C45 120.0(2) . . ? C44 C45 C46 118.6(3) . . ? N41 C46 C45 121.5(2) . . ? C56 N51 C52 119.0(2) . . ? C56 N51 Cu1 126.42(17) . . ? C52 N51 Cu1 114.51(17) . . ? N51 C52 C53 122.6(2) . . ? N51 C52 C31 113.5(2) . . ? C53 C52 C31 123.9(2) . . ? C52 C53 C54 118.1(2) . . ? C55 C54 C53 119.3(2) . . ? C54 C55 C56 119.3(3) . . ? N51 C56 C55 121.7(2) . . ? O63 N60 O61 122.1(3) . . ? O63 N60 O62 123.7(3) . . ? O61 N60 O62 114.2(3) . . ? O73 N70 O72 120.6(3) . . ? O73 N70 O71 120.4(2) . . ? O72 N70 O71 119.0(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 O3 C1 O2 Cu1 -176.56(18) . . . . ? C12 C1 O2 Cu1 58.40(16) . . . . ? C22 C1 O2 Cu1 -56.28(16) . . . . ? N11 Cu1 O2 C1 -46.11(14) . . . . ? N41 Cu1 O2 C1 -134.02(14) . . . . ? N21 Cu1 O2 C1 45.14(13) . . . . ? N51 Cu1 O2 C1 135.33(13) . . . . ? O32 Cu1 O2 C1 -89.0(4) . . . . ? N41 Cu1 N11 C12 122.34(17) . . . . ? N21 Cu1 N11 C12 -51.72(17) . . . . ? N51 Cu1 N11 C12 -170.2(8) . . . . ? O32 Cu1 N11 C12 -162.50(17) . . . . ? O2 Cu1 N11 C12 23.72(16) . . . . ? N41 Cu1 N11 C16 -57.3(2) . . . . ? N21 Cu1 N11 C16 128.6(2) . . . . ? N51 Cu1 N11 C16 10.2(10) . . . . ? O32 Cu1 N11 C16 17.8(2) . . . . ? O2 Cu1 N11 C16 -155.9(2) . . . . ? C16 N11 C12 C13 -0.1(4) . . . . ? Cu1 N11 C12 C13 -179.77(19) . . . . ? C16 N11 C12 C1 -177.1(2) . . . . ? Cu1 N11 C12 C1 3.2(3) . . . . ? O3 C1 C12 N11 -174.0(2) . . . . ? O2 C1 C12 N11 -49.7(3) . . . . ? C22 C1 C12 N11 66.5(2) . . . . ? O3 C1 C12 C13 9.0(3) . . . . ? O2 C1 C12 C13 133.3(2) . . . . ? C22 C1 C12 C13 -110.5(3) . . . . ? N11 C12 C13 C14 -0.1(4) . . . . ? C1 C12 C13 C14 176.7(2) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? C12 N11 C16 C15 0.5(4) . . . . ? Cu1 N11 C16 C15 -179.8(2) . . . . ? C14 C15 C16 N11 -0.7(4) . . . . ? N11 Cu1 N21 C26 -127.3(2) . . . . ? N41 Cu1 N21 C26 164.8(7) . . . . ? N51 Cu1 N21 C26 47.8(2) . . . . ? O32 Cu1 N21 C26 -29.5(2) . . . . ? O2 Cu1 N21 C26 157.5(2) . . . . ? N11 Cu1 N21 C22 48.27(16) . . . . ? N41 Cu1 N21 C22 -19.6(8) . . . . ? N51 Cu1 N21 C22 -136.69(16) . . . . ? O32 Cu1 N21 C22 146.05(15) . . . . ? O2 Cu1 N21 C22 -26.99(15) . . . . ? C26 N21 C22 C23 0.7(3) . . . . ? Cu1 N21 C22 C23 -175.16(18) . . . . ? C26 N21 C22 C1 178.9(2) . . . . ? Cu1 N21 C22 C1 3.0(2) . . . . ? O3 C1 C22 N21 166.90(19) . . . . ? O2 C1 C22 N21 43.9(2) . . . . ? C12 C1 C22 N21 -70.0(2) . . . . ? O3 C1 C22 C23 -14.9(3) . . . . ? O2 C1 C22 C23 -138.0(2) . . . . ? C12 C1 C22 C23 108.2(2) . . . . ? N21 C22 C23 C24 -1.9(4) . . . . ? C1 C22 C23 C24 -179.9(2) . . . . ? C22 C23 C24 C25 2.0(4) . . . . ? C23 C24 C25 C26 -1.0(4) . . . . ? C22 N21 C26 C25 0.5(4) . . . . ? Cu1 N21 C26 C25 175.9(2) . . . . ? C24 C25 C26 N21 -0.3(4) . . . . ? O33 C31 O32 Cu1 -176.69(18) . . . . ? C42 C31 O32 Cu1 58.45(17) . . . . ? C52 C31 O32 Cu1 -55.84(18) . . . . ? N11 Cu1 O32 C31 -134.65(15) . . . . ? N41 Cu1 O32 C31 -46.65(14) . . . . ? N21 Cu1 O32 C31 134.99(15) . . . . ? N51 Cu1 O32 C31 44.58(15) . . . . ? O2 Cu1 O32 C31 -93.0(4) . . . . ? N11 Cu1 N41 C46 -54.8(2) . . . . ? N21 Cu1 N41 C46 12.9(9) . . . . ? N51 Cu1 N41 C46 130.4(2) . . . . ? O32 Cu1 N41 C46 -153.2(2) . . . . ? O2 Cu1 N41 C46 20.2(2) . . . . ? N11 Cu1 N41 C42 123.81(17) . . . . ? N21 Cu1 N41 C42 -168.5(7) . . . . ? N51 Cu1 N41 C42 -51.00(16) . . . . ? O32 Cu1 N41 C42 25.38(15) . . . . ? O2 Cu1 N41 C42 -161.24(15) . . . . ? C46 N41 C42 C43 -3.1(3) . . . . ? Cu1 N41 C42 C43 178.25(18) . . . . ? C46 N41 C42 C31 179.8(2) . . . . ? Cu1 N41 C42 C31 1.1(2) . . . . ? O33 C31 C42 N41 -170.17(19) . . . . ? O32 C31 C42 N41 -46.5(2) . . . . ? C52 C31 C42 N41 68.8(2) . . . . ? O33 C31 C42 C43 12.7(3) . . . . ? O32 C31 C42 C43 136.4(2) . . . . ? C52 C31 C42 C43 -108.3(2) . . . . ? N41 C42 C43 C44 3.4(4) . . . . ? C31 C42 C43 C44 -179.7(2) . . . . ? C42 C43 C44 C45 -1.6(4) . . . . ? C43 C44 C45 C46 -0.3(4) . . . . ? C42 N41 C46 C45 0.9(4) . . . . ? Cu1 N41 C46 C45 179.5(2) . . . . ? C44 C45 C46 N41 0.7(4) . . . . ? N11 Cu1 N51 C56 164.1(8) . . . . ? N41 Cu1 N51 C56 -128.3(2) . . . . ? N21 Cu1 N51 C56 46.0(2) . . . . ? O32 Cu1 N51 C56 156.3(2) . . . . ? O2 Cu1 N51 C56 -30.2(2) . . . . ? N11 Cu1 N51 C52 -18.2(10) . . . . ? N41 Cu1 N51 C52 49.44(18) . . . . ? N21 Cu1 N51 C52 -136.27(18) . . . . ? O32 Cu1 N51 C52 -25.97(17) . . . . ? O2 Cu1 N51 C52 147.51(16) . . . . ? C56 N51 C52 C53 1.3(4) . . . . ? Cu1 N51 C52 C53 -176.6(2) . . . . ? C56 N51 C52 C31 179.4(2) . . . . ? Cu1 N51 C52 C31 1.6(3) . . . . ? O33 C31 C52 N51 165.6(2) . . . . ? O32 C31 C52 N51 43.0(3) . . . . ? C42 C31 C52 N51 -70.4(3) . . . . ? O33 C31 C52 C53 -16.3(3) . . . . ? O32 C31 C52 C53 -138.9(3) . . . . ? C42 C31 C52 C53 107.8(3) . . . . ? N51 C52 C53 C54 -0.6(4) . . . . ? C31 C52 C53 C54 -178.5(3) . . . . ? C52 C53 C54 C55 0.0(5) . . . . ? C53 C54 C55 C56 -0.1(5) . . . . ? C52 N51 C56 C55 -1.4(4) . . . . ? Cu1 N51 C56 C55 176.2(2) . . . . ? C54 C55 C56 N51 0.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.611 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.047 #===END data_Compound-20 _database_code_CSD 216643 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 20 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Cu N6 O12' _chemical_formula_weight 628.01 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 7.538(2) _cell_length_b 12.048(3) _cell_length_c 14.550(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.479(4) _cell_angle_gamma 90.00 _cell_volume 1318.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 7857 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.29 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.819985 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 16121 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.36 _reflns_number_total 2624 _reflns_number_gt 2219 _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^)+(0.0372P)^2^+1.4121P] 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 2624 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 1.0000 0.5000 0.02128(13) Uani 1 2 d S . . C1 C 0.1014(4) 1.1436(2) 0.35063(17) 0.0254(6) Uani 1 1 d . . . O1 O -0.06383(14) 1.08593(8) 0.34692(7) 0.0277(4) Uani 1 1 d . . . H1A H -0.1477 1.1319 0.3422 0.042 Uiso 1 1 calc R . . O2 O 0.12185(15) 1.21183(10) 0.27460(9) 0.0374(5) Uani 1 1 d R . . H2A H 0.1058 1.1744 0.2261 0.056 Uiso 1 1 calc R . . N11 N 0.21491(14) 0.97725(9) 0.42902(8) 0.0240(5) Uani 1 1 d R . . C12 C 0.24248(14) 1.05217(8) 0.36180(9) 0.0247(6) Uani 1 1 d R . . C13 C 0.38993(14) 1.04688(8) 0.30951(9) 0.0346(7) Uani 1 1 d R . . H13A H 0.4087 1.1010 0.2636 0.042 Uiso 1 1 calc R . . C14 C 0.5098(4) 0.9602(3) 0.3261(2) 0.0401(7) Uani 1 1 d . . . H14A H 0.6111 0.9538 0.2907 0.048 Uiso 1 1 calc R . . C15 C 0.4807(4) 0.8832(2) 0.3943(2) 0.0352(7) Uani 1 1 d . . . H15A H 0.5616 0.8236 0.4062 0.042 Uiso 1 1 calc R . . C16 C 0.3328(4) 0.8942(2) 0.4448(2) 0.0296(6) Uani 1 1 d . . . H16A H 0.3133 0.8419 0.4920 0.035 Uiso 1 1 calc R . . N21 N 0.0712(3) 1.16335(17) 0.51520(14) 0.0224(4) Uani 1 1 d . . . C22 C 0.1139(3) 1.2166(2) 0.43738(17) 0.0237(5) Uani 1 1 d . . . C23 C 0.1648(4) 1.3277(2) 0.4378(2) 0.0317(6) Uani 1 1 d . . . H23A H 0.1942 1.3637 0.3827 0.038 Uiso 1 1 calc R . . C24 C 0.1714(4) 1.3848(2) 0.5214(2) 0.0344(7) Uani 1 1 d . . . H24A H 0.2042 1.4609 0.5236 0.041 Uiso 1 1 calc R . . C25 C 0.1300(4) 1.3302(2) 0.6011(2) 0.0327(6) Uani 1 1 d . . . H25A H 0.1363 1.3681 0.6585 0.039 Uiso 1 1 calc R . . C26 C 0.0790(3) 1.2188(2) 0.59594(18) 0.0262(6) Uani 1 1 d . . . H26A H 0.0491 1.1814 0.6503 0.031 Uiso 1 1 calc R . . N30 N 0.1473(4) 0.1701(2) 0.86008(17) 0.0377(6) Uani 1 1 d . . . O31 O 0.0866(6) 0.0894(3) 0.8184(2) 0.1121(16) Uani 1 1 d . . . O32 O 0.1861(5) 0.1630(2) 0.94323(16) 0.0696(9) Uani 1 1 d . . . O33 O 0.1798(3) 0.25675(19) 0.81655(16) 0.0511(6) Uani 1 1 d . . . O40 O 0.1104(3) 1.08479(19) 0.12147(15) 0.0518(6) Uani 1 1 d . . . H40A H 0.1034 1.1071 0.0658 0.078 Uiso 1 1 d R . . H40B H 0.0616 1.0393 0.1286 0.078 Uiso 1 1 d 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 0.0232(2) 0.0171(2) 0.0240(2) 0.00211(18) 0.00551(15) 0.00002(19) C1 0.0333(15) 0.0209(13) 0.0225(13) 0.0017(10) 0.0054(11) -0.0020(11) O1 0.0285(10) 0.0228(9) 0.0313(10) -0.0011(8) -0.0018(8) 0.0021(8) O2 0.0625(15) 0.0261(10) 0.0241(10) 0.0048(8) 0.0068(9) -0.0034(10) N11 0.0238(11) 0.0195(11) 0.0293(11) -0.0008(8) 0.0056(9) -0.0006(8) C12 0.0281(14) 0.0221(13) 0.0243(13) -0.0027(10) 0.0042(10) -0.0031(11) C13 0.0369(17) 0.0364(15) 0.0320(15) -0.0003(13) 0.0134(12) -0.0054(13) C14 0.0272(16) 0.0469(18) 0.0474(18) -0.0126(15) 0.0133(13) -0.0037(13) C15 0.0235(15) 0.0313(15) 0.0509(18) -0.0103(14) 0.0040(12) 0.0016(12) C16 0.0261(15) 0.0222(13) 0.0402(15) 0.0000(11) 0.0005(12) 0.0010(11) N21 0.0220(11) 0.0206(10) 0.0248(11) -0.0003(8) 0.0037(8) 0.0011(8) C22 0.0232(14) 0.0209(12) 0.0271(13) -0.0001(10) 0.0038(10) 0.0017(10) C23 0.0381(17) 0.0227(13) 0.0345(15) 0.0026(11) 0.0045(12) -0.0025(12) C24 0.0374(17) 0.0213(13) 0.0450(17) -0.0022(12) 0.0053(13) -0.0028(12) C25 0.0307(15) 0.0310(15) 0.0368(15) -0.0116(12) 0.0057(12) -0.0013(12) C26 0.0238(14) 0.0293(14) 0.0257(13) -0.0019(11) 0.0047(10) -0.0001(11) N30 0.0531(17) 0.0272(13) 0.0333(14) -0.0048(11) 0.0065(12) -0.0080(11) O31 0.219(5) 0.070(2) 0.0485(17) -0.0144(15) 0.016(2) -0.092(3) O32 0.131(3) 0.0429(14) 0.0338(13) 0.0020(11) -0.0003(15) -0.0072(15) O33 0.0607(16) 0.0399(13) 0.0504(13) 0.0143(11) -0.0142(11) -0.0221(11) O40 0.0758(18) 0.0444(13) 0.0358(12) -0.0034(10) 0.0098(11) -0.0174(12) _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 N11 1.9923(12) 3_576 ? Cu1 N11 1.9923(13) . ? Cu1 N21 2.048(2) . ? Cu1 N21 2.048(2) 3_576 ? C1 O2 1.394(3) . ? C1 O1 1.425(3) . ? C1 C12 1.533(3) . ? C1 C22 1.536(4) . ? N11 C16 1.348(3) . ? N11 C12 1.3561 . ? C12 C13 1.3860 . ? C13 C14 1.392(3) . ? C14 C15 1.387(5) . ? C15 C16 1.378(4) . ? N21 C26 1.350(3) . ? N21 C22 1.357(3) . ? C22 C23 1.392(4) . ? C23 C24 1.395(4) . ? C24 C25 1.385(4) . ? C25 C26 1.397(4) . ? N30 O31 1.220(3) . ? N30 O32 1.230(3) . ? N30 O33 1.253(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 N11 Cu1 N11 180.0 3_576 . ? N11 Cu1 N21 91.59(7) 3_576 . ? N11 Cu1 N21 88.41(7) . . ? N11 Cu1 N21 88.41(7) 3_576 3_576 ? N11 Cu1 N21 91.59(7) . 3_576 ? N21 Cu1 N21 180.0 . 3_576 ? O2 C1 O1 113.33(19) . . ? O2 C1 C12 113.49(19) . . ? O1 C1 C12 104.65(16) . . ? O2 C1 C22 108.1(2) . . ? O1 C1 C22 108.68(19) . . ? C12 C1 C22 108.45(19) . . ? C16 N11 C12 119.23(14) . . ? C16 N11 Cu1 124.20(14) . . ? C12 N11 Cu1 116.6 . . ? N11 C12 C13 121.9 . . ? N11 C12 C1 114.78(10) . . ? C13 C12 C1 123.31(10) . . ? C12 C13 C14 118.24(14) . . ? C15 C14 C13 119.8(3) . . ? C16 C15 C14 119.0(3) . . ? N11 C16 C15 121.8(3) . . ? C26 N21 C22 119.5(2) . . ? C26 N21 Cu1 124.54(17) . . ? C22 N21 Cu1 115.96(16) . . ? N21 C22 C23 122.0(2) . . ? N21 C22 C1 114.2(2) . . ? C23 C22 C1 123.9(2) . . ? C22 C23 C24 118.3(3) . . ? C25 C24 C23 119.9(3) . . ? C24 C25 C26 119.1(3) . . ? N21 C26 C25 121.3(2) . . ? O31 N30 O32 119.6(3) . . ? O31 N30 O33 119.5(3) . . ? O32 N30 O33 120.8(3) . . ? 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 N11 Cu1 N11 C16 -45(100) 3_576 . . . ? N21 Cu1 N11 C16 131.17(17) . . . . ? N21 Cu1 N11 C16 -48.83(17) 3_576 . . . ? N11 Cu1 N11 C12 136(100) 3_576 . . . ? N21 Cu1 N11 C12 -47.87(6) . . . . ? N21 Cu1 N11 C12 132.13(6) 3_576 . . . ? C16 N11 C12 C13 -0.92(14) . . . . ? Cu1 N11 C12 C13 178.2 . . . . ? C16 N11 C12 C1 -179.3(2) . . . . ? Cu1 N11 C12 C1 -0.24(11) . . . . ? O2 C1 C12 N11 -173.14(13) . . . . ? O1 C1 C12 N11 -49.09(17) . . . . ? C22 C1 C12 N11 66.76(19) . . . . ? O2 C1 C12 C13 8.5(2) . . . . ? O1 C1 C12 C13 132.52(11) . . . . ? C22 C1 C12 C13 -111.62(16) . . . . ? N11 C12 C13 C14 1.43(15) . . . . ? C1 C12 C13 C14 179.7(2) . . . . ? C12 C13 C14 C15 -0.9(3) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C12 N11 C16 C15 -0.1(3) . . . . ? Cu1 N11 C16 C15 -179.13(19) . . . . ? C14 C15 C16 N11 0.6(4) . . . . ? N11 Cu1 N21 C26 48.9(2) 3_576 . . . ? N11 Cu1 N21 C26 -131.1(2) . . . . ? N21 Cu1 N21 C26 164(100) 3_576 . . . ? N11 Cu1 N21 C22 -131.64(18) 3_576 . . . ? N11 Cu1 N21 C22 48.36(18) . . . . ? N21 Cu1 N21 C22 -17(100) 3_576 . . . ? C26 N21 C22 C23 -0.5(4) . . . . ? Cu1 N21 C22 C23 -180.0(2) . . . . ? C26 N21 C22 C1 179.4(2) . . . . ? Cu1 N21 C22 C1 -0.1(3) . . . . ? O2 C1 C22 N21 171.1(2) . . . . ? O1 C1 C22 N21 47.7(3) . . . . ? C12 C1 C22 N21 -65.5(3) . . . . ? O2 C1 C22 C23 -9.0(3) . . . . ? O1 C1 C22 C23 -132.4(3) . . . . ? C12 C1 C22 C23 114.4(3) . . . . ? N21 C22 C23 C24 0.1(4) . . . . ? C1 C22 C23 C24 -179.8(3) . . . . ? C22 C23 C24 C25 0.8(4) . . . . ? C23 C24 C25 C26 -1.2(4) . . . . ? C22 N21 C26 C25 0.1(4) . . . . ? Cu1 N21 C26 C25 179.5(2) . . . . ? C24 C25 C26 N21 0.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.441 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.064 #===END data_Compound-21 _database_code_CSD 216644 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 Cu2 N8 O16' _chemical_formula_weight 839.68 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 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 27.587(16) _cell_length_b 10.068(6) _cell_length_c 14.049(8) _cell_angle_alpha 90.00 _cell_angle_beta 119.649(8) _cell_angle_gamma 90.00 _cell_volume 3391(3) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 2114 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.82 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 1.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7755 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 8673 _diffrn_reflns_av_R_equivalents 0.1156 _diffrn_reflns_av_sigmaI/netI 0.0949 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2207 _reflns_number_gt 1308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0900P)^2^+7.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2207 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1360 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1760 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.014 _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 0.12005(4) 0.59018(11) 0.33205(9) 0.0310(4) Uani 1 1 d . . . C1 C 0.2289(3) 0.7228(8) 0.5049(7) 0.027(2) Uani 1 1 d . . . N11 N 0.1836(3) 0.5080(7) 0.4652(6) 0.0273(17) Uani 1 1 d . . . C12 C 0.2284(3) 0.5818(9) 0.5347(7) 0.027(2) Uani 1 1 d . . . C13 C 0.2714(4) 0.5278(9) 0.6317(8) 0.038(2) Uani 1 1 d . . . H13A H 0.3022 0.5811 0.6805 0.046 Uiso 1 1 calc R . . C14 C 0.2684(4) 0.3957(9) 0.6555(7) 0.036(2) Uani 1 1 d . . . H14A H 0.2975 0.3572 0.7205 0.044 Uiso 1 1 calc R . . C15 C 0.2232(4) 0.3201(10) 0.5849(7) 0.040(3) Uani 1 1 d . . . H15A H 0.2207 0.2295 0.6007 0.048 Uiso 1 1 calc R . . C16 C 0.1811(4) 0.3784(9) 0.4899(7) 0.037(3) Uani 1 1 d . . . H16A H 0.1499 0.3263 0.4411 0.044 Uiso 1 1 calc R . . N21 N 0.1283(3) 0.7497(7) 0.4210(5) 0.0278(17) Uani 1 1 d . . . C22 C 0.1793(3) 0.8024(8) 0.4901(7) 0.024(2) Uani 1 1 d . . . C23 C 0.1858(3) 0.9163(9) 0.5504(7) 0.035(2) Uani 1 1 d . . . H23A H 0.2220 0.9491 0.5998 0.041 Uiso 1 1 calc R . . C24 C 0.1377(4) 0.9833(9) 0.5375(7) 0.038(2) Uani 1 1 d . . . H24A H 0.1408 1.0645 0.5746 0.046 Uiso 1 1 calc R . . C25 C 0.0858(3) 0.9270(10) 0.4693(7) 0.035(2) Uani 1 1 d . . . H25A H 0.0530 0.9668 0.4622 0.042 Uiso 1 1 calc R . . C26 C 0.0825(4) 0.8125(8) 0.4118(7) 0.032(2) Uani 1 1 d . . . H26A H 0.0467 0.7763 0.3640 0.039 Uiso 1 1 calc R . . N10 N 0.0751(3) 0.7595(8) 0.1553(7) 0.0379(19) Uani 1 1 d . . . O11 O 0.0574(2) 0.6781(6) 0.2022(5) 0.0368(16) Uani 1 1 d . . . O12 O 0.1269(3) 0.7677(7) 0.1940(5) 0.054(2) Uani 1 1 d . . . O13 O 0.0419(3) 0.8241(7) 0.0750(6) 0.057(2) Uani 1 1 d . . . N20 N 0.1524(3) 0.4188(9) 0.2150(6) 0.042(2) Uani 1 1 d . . . O21 O 0.1124(2) 0.4381(6) 0.2365(5) 0.0407(17) Uani 1 1 d . . . O22 O 0.1490(3) 0.3279(8) 0.1545(6) 0.067(2) Uani 1 1 d . . . O23 O 0.1922(3) 0.4979(9) 0.2570(6) 0.072(2) Uani 1 1 d . . . O30 O 0.0520(2) 0.4819(6) 0.3474(5) 0.0422(17) Uani 1 1 d . . . H30 H 0.0224 0.5140 0.2958 0.063 Uiso 1 1 d R . . C30 C 0.0463(4) 0.4682(10) 0.4427(7) 0.044(3) Uani 1 1 d . . . H30A H 0.0111 0.4234 0.4230 0.067 Uiso 1 1 calc R . . H30B H 0.0465 0.5563 0.4725 0.067 Uiso 1 1 calc R . . H30C H 0.0775 0.4156 0.4978 0.067 Uiso 1 1 calc R . . O40 O 0.0538(4) 0.2036(9) 0.2788(9) 0.108(4) Uani 1 1 d . . . H40 H 0.0686 0.2768 0.2796 0.162 Uiso 1 1 calc R . . C40 C 0.0640(6) 0.113(2) 0.2152(11) 0.113(7) Uani 1 1 d . . . H40A H 0.1043 0.1032 0.2451 0.170 Uiso 1 1 calc R . . H40B H 0.0469 0.1448 0.1396 0.170 Uiso 1 1 calc R . . H40C H 0.0480 0.0262 0.2165 0.170 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 0.0285(6) 0.0293(7) 0.0280(7) 0.0010(6) 0.0085(5) 0.0008(5) C1 0.023(5) 0.025(5) 0.025(5) -0.001(4) 0.006(4) 0.001(4) N11 0.031(4) 0.015(4) 0.031(4) -0.003(4) 0.011(4) -0.001(3) C12 0.030(5) 0.025(5) 0.032(5) 0.001(5) 0.020(4) -0.002(5) C13 0.032(5) 0.033(6) 0.045(7) -0.006(5) 0.015(5) -0.007(4) C14 0.033(5) 0.032(6) 0.034(6) 0.005(5) 0.009(4) 0.003(5) C15 0.043(6) 0.033(6) 0.040(6) 0.008(5) 0.016(5) 0.004(5) C16 0.028(5) 0.035(7) 0.033(6) 0.002(5) 0.004(4) -0.002(4) N21 0.022(4) 0.034(4) 0.023(4) 0.004(3) 0.007(3) -0.001(3) C22 0.028(5) 0.020(5) 0.028(5) -0.001(4) 0.015(4) -0.003(4) C23 0.024(5) 0.033(6) 0.036(6) 0.002(5) 0.006(4) -0.001(5) C24 0.047(6) 0.028(5) 0.040(6) -0.004(5) 0.022(5) 0.004(5) C25 0.016(4) 0.049(7) 0.039(6) 0.002(5) 0.012(4) 0.006(5) C26 0.032(5) 0.026(6) 0.036(6) -0.004(5) 0.015(5) 0.006(4) N10 0.042(5) 0.039(5) 0.033(5) 0.003(4) 0.019(4) 0.000(4) O11 0.030(3) 0.040(4) 0.030(4) 0.005(3) 0.007(3) -0.006(3) O12 0.041(4) 0.070(5) 0.046(5) 0.003(4) 0.019(4) -0.017(4) O13 0.063(5) 0.045(5) 0.042(5) 0.016(4) 0.011(4) 0.005(4) N20 0.044(5) 0.045(6) 0.026(5) 0.001(5) 0.009(4) 0.012(5) O21 0.032(3) 0.047(5) 0.040(4) -0.016(3) 0.015(3) -0.001(3) O22 0.093(6) 0.059(5) 0.044(5) -0.008(4) 0.032(4) 0.027(4) O23 0.057(5) 0.104(7) 0.065(6) -0.028(5) 0.039(4) -0.026(5) O30 0.031(3) 0.059(5) 0.026(4) 0.011(3) 0.006(3) -0.008(3) C30 0.044(6) 0.053(7) 0.040(6) 0.017(5) 0.023(5) 0.002(5) O40 0.094(7) 0.054(6) 0.102(8) 0.007(6) -0.007(6) -0.027(5) C40 0.082(10) 0.191(19) 0.068(10) -0.027(12) 0.037(8) -0.081(12) _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 N21 1.977(7) . ? Cu1 O21 1.978(6) . ? Cu1 O11 1.995(6) . ? Cu1 N11 2.003(7) . ? Cu1 O30 2.271(6) . ? C1 C1 1.355(16) 7_566 ? C1 C12 1.482(11) . ? C1 C22 1.509(11) . ? N11 C12 1.357(10) . ? N11 C16 1.360(11) . ? C12 C13 1.400(12) . ? C13 C14 1.384(12) . ? C14 C15 1.377(12) . ? C15 C16 1.392(12) . ? N21 C22 1.360(10) . ? N21 C26 1.362(10) . ? C22 C23 1.384(12) . ? C23 C24 1.418(12) . ? C24 C25 1.389(12) . ? C25 C26 1.384(12) . ? N10 O13 1.230(9) . ? N10 O12 1.254(9) . ? N10 O11 1.289(9) . ? N20 O22 1.221(10) . ? N20 O23 1.245(10) . ? N20 O21 1.295(9) . ? O30 C30 1.430(10) . ? O40 C40 1.401(17) . ? 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 N21 Cu1 O21 176.3(3) . . ? N21 Cu1 O11 89.7(3) . . ? O21 Cu1 O11 88.3(3) . . ? N21 Cu1 N11 88.3(3) . . ? O21 Cu1 N11 93.7(3) . . ? O11 Cu1 N11 178.0(3) . . ? N21 Cu1 O30 99.9(3) . . ? O21 Cu1 O30 82.9(2) . . ? O11 Cu1 O30 85.3(2) . . ? N11 Cu1 O30 95.5(3) . . ? C1 C1 C12 123.0(9) 7_566 . ? C1 C1 C22 122.5(10) 7_566 . ? C12 C1 C22 114.4(7) . . ? C12 N11 C16 118.9(7) . . ? C12 N11 Cu1 120.8(6) . . ? C16 N11 Cu1 120.3(6) . . ? N11 C12 C13 121.4(8) . . ? N11 C12 C1 117.0(7) . . ? C13 C12 C1 121.7(8) . . ? C14 C13 C12 119.0(8) . . ? C15 C14 C13 119.9(8) . . ? C14 C15 C16 119.1(9) . . ? N11 C16 C15 121.8(8) . . ? C22 N21 C26 118.0(8) . . ? C22 N21 Cu1 121.5(6) . . ? C26 N21 Cu1 120.4(6) . . ? N21 C22 C23 122.4(7) . . ? N21 C22 C1 116.0(7) . . ? C23 C22 C1 121.4(7) . . ? C22 C23 C24 119.1(8) . . ? C25 C24 C23 118.3(8) . . ? C26 C25 C24 119.4(8) . . ? N21 C26 C25 122.7(8) . . ? O13 N10 O12 122.3(8) . . ? O13 N10 O11 120.4(8) . . ? O12 N10 O11 117.3(7) . . ? N10 O11 Cu1 112.0(5) . . ? O22 N20 O23 123.8(9) . . ? O22 N20 O21 119.6(9) . . ? O23 N20 O21 116.6(8) . . ? N20 O21 Cu1 117.2(6) . . ? C30 O30 Cu1 127.9(5) . . ? 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 N21 Cu1 N11 C12 -39.4(6) . . . . ? O21 Cu1 N11 C12 137.5(6) . . . . ? O11 Cu1 N11 C12 -28(8) . . . . ? O30 Cu1 N11 C12 -139.3(6) . . . . ? N21 Cu1 N11 C16 137.6(7) . . . . ? O21 Cu1 N11 C16 -45.5(7) . . . . ? O11 Cu1 N11 C16 149(8) . . . . ? O30 Cu1 N11 C16 37.8(7) . . . . ? C16 N11 C12 C13 -1.2(12) . . . . ? Cu1 N11 C12 C13 175.9(6) . . . . ? C16 N11 C12 C1 -179.4(7) . . . . ? Cu1 N11 C12 C1 -2.3(10) . . . . ? C1 C1 C12 N11 -124.7(11) 7_566 . . . ? C22 C1 C12 N11 57.3(10) . . . . ? C1 C1 C12 C13 57.2(15) 7_566 . . . ? C22 C1 C12 C13 -120.9(8) . . . . ? N11 C12 C13 C14 1.4(13) . . . . ? C1 C12 C13 C14 179.5(8) . . . . ? C12 C13 C14 C15 -0.9(14) . . . . ? C13 C14 C15 C16 0.3(14) . . . . ? C12 N11 C16 C15 0.5(13) . . . . ? Cu1 N11 C16 C15 -176.6(7) . . . . ? C14 C15 C16 N11 0.0(14) . . . . ? O21 Cu1 N21 C22 -80(4) . . . . ? O11 Cu1 N21 C22 -135.1(6) . . . . ? N11 Cu1 N21 C22 44.5(6) . . . . ? O30 Cu1 N21 C22 139.7(6) . . . . ? O21 Cu1 N21 C26 98(4) . . . . ? O11 Cu1 N21 C26 42.8(6) . . . . ? N11 Cu1 N21 C26 -137.6(7) . . . . ? O30 Cu1 N21 C26 -42.4(7) . . . . ? C26 N21 C22 C23 0.0(12) . . . . ? Cu1 N21 C22 C23 178.0(6) . . . . ? C26 N21 C22 C1 174.8(7) . . . . ? Cu1 N21 C22 C1 -7.2(10) . . . . ? C1 C1 C22 N21 129.9(11) 7_566 . . . ? C12 C1 C22 N21 -52.0(10) . . . . ? C1 C1 C22 C23 -55.2(14) 7_566 . . . ? C12 C1 C22 C23 122.9(9) . . . . ? N21 C22 C23 C24 -2.0(13) . . . . ? C1 C22 C23 C24 -176.5(8) . . . . ? C22 C23 C24 C25 3.7(13) . . . . ? C23 C24 C25 C26 -3.5(13) . . . . ? C22 N21 C26 C25 0.3(12) . . . . ? Cu1 N21 C26 C25 -177.7(7) . . . . ? C24 C25 C26 N21 1.6(13) . . . . ? O13 N10 O11 Cu1 -178.6(6) . . . . ? O12 N10 O11 Cu1 2.4(9) . . . . ? N21 Cu1 O11 N10 81.0(6) . . . . ? O21 Cu1 O11 N10 -96.0(5) . . . . ? N11 Cu1 O11 N10 69(8) . . . . ? O30 Cu1 O11 N10 -179.0(6) . . . . ? O22 N20 O21 Cu1 -178.4(6) . . . . ? O23 N20 O21 Cu1 0.3(10) . . . . ? N21 Cu1 O21 N20 55(4) . . . . ? O11 Cu1 O21 N20 111.0(6) . . . . ? N11 Cu1 O21 N20 -68.5(6) . . . . ? O30 Cu1 O21 N20 -163.5(6) . . . . ? N21 Cu1 O30 C30 -41.0(7) . . . . ? O21 Cu1 O30 C30 141.4(7) . . . . ? O11 Cu1 O30 C30 -129.8(7) . . . . ? N11 Cu1 O30 C30 48.3(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.460 _refine_diff_density_min -1.412 _refine_diff_density_rms 0.121 #===END data_Compound-23 _database_code_CSD 216645 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H40 N4 O14 Pd2' _chemical_formula_weight 893.46 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' Pd Pd -0.9988 1.0072 '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 19.644(8) _cell_length_b 15.938(6) _cell_length_c 14.847(6) _cell_angle_alpha 90.00 _cell_angle_beta 125.925(5) _cell_angle_gamma 90.00 _cell_volume 3764(3) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 4225 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.36 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.752192 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 12495 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3285 _reflns_number_gt 2908 _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^)+(0.0381P)^2^+2.1518P] 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 3285 _refine_ls_number_parameters 244 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 2.231 _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 Pd1 Pd 0.11233(2) 0.35323(2) 0.71486(3) 0.02429(17) Uani 1 1 d . . . C1 C 0.0009(3) 0.4866(3) 0.5434(4) 0.0234(10) Uani 1 1 d . . . N11 N -0.0146(3) 0.3525(2) 0.6063(3) 0.0239(9) Uani 1 1 d . . . C12 C -0.0542(3) 0.4169(3) 0.5335(3) 0.0241(10) Uani 1 1 d . . . C13 C -0.1406(3) 0.4180(3) 0.4552(4) 0.0292(11) Uani 1 1 d . . . H13A H -0.1672 0.4644 0.4062 0.035 Uiso 1 1 calc R . . C14 C -0.1879(3) 0.3506(3) 0.4490(4) 0.0345(12) Uani 1 1 d . . . H14A H -0.2472 0.3498 0.3951 0.041 Uiso 1 1 calc R . . C15 C -0.1473(3) 0.2846(3) 0.5226(4) 0.0315(11) Uani 1 1 d . . . H15A H -0.1783 0.2377 0.5199 0.038 Uiso 1 1 calc R . . C16 C -0.0609(3) 0.2876(3) 0.6003(4) 0.0275(11) Uani 1 1 d . . . H16A H -0.0335 0.2424 0.6511 0.033 Uiso 1 1 calc R . . N21 N 0.1089(2) 0.4766(2) 0.7423(3) 0.0252(9) Uani 1 1 d . . . C22 C 0.0548(3) 0.5277(3) 0.6552(4) 0.0247(10) Uani 1 1 d . . . C23 C 0.0496(3) 0.6127(3) 0.6699(4) 0.0307(11) Uani 1 1 d . . . H23A H 0.0106 0.6471 0.6084 0.037 Uiso 1 1 calc R . . C24 C 0.1020(4) 0.6468(3) 0.7755(5) 0.0393(13) Uani 1 1 d . . . H24A H 0.0995 0.7050 0.7873 0.047 Uiso 1 1 calc R . . C25 C 0.1580(4) 0.5949(4) 0.8632(4) 0.0400(13) Uani 1 1 d . . . H25A H 0.1948 0.6173 0.9361 0.048 Uiso 1 1 calc R . . C26 C 0.1605(3) 0.5104(3) 0.8448(4) 0.0330(11) Uani 1 1 d . . . H26A H 0.1993 0.4753 0.9057 0.040 Uiso 1 1 calc R . . O30 O 0.2384(2) 0.3512(2) 0.8261(3) 0.0357(9) Uani 1 1 d . . . C30 C 0.3751(4) 0.3754(4) 0.8762(6) 0.0603(19) Uani 1 1 d . . . H30A H 0.4026 0.4030 0.8464 0.090 Uiso 1 1 calc R . . H30B H 0.3895 0.3156 0.8875 0.090 Uiso 1 1 calc R . . H30C H 0.3944 0.4011 0.9474 0.090 Uiso 1 1 calc R . . C31 C 0.2806(3) 0.3853(3) 0.7947(5) 0.0380(13) Uani 1 1 d . . . O31 O 0.2488(2) 0.4240(3) 0.7071(3) 0.0516(11) Uani 1 1 d . . . O40 O 0.1181(2) 0.2279(2) 0.6966(3) 0.0339(8) Uani 1 1 d . . . O41 O 0.0841(3) 0.2455(2) 0.5260(3) 0.0543(12) Uani 1 1 d . . . C40 C 0.1210(5) 0.1074(4) 0.6052(6) 0.0615(19) Uani 1 1 d . . . H40A H 0.1111 0.0920 0.5345 0.092 Uiso 1 1 calc R . . H40B H 0.0822 0.0761 0.6139 0.092 Uiso 1 1 calc R . . H40C H 0.1791 0.0936 0.6667 0.092 Uiso 1 1 calc R . . C41 C 0.1064(3) 0.2013(3) 0.6060(4) 0.0373(12) Uani 1 1 d . . . O50 O 0.0765(4) 0.1683(3) 0.3511(5) 0.0687(14) Uani 1 1 d D . . H50A H 0.083(6) 0.188(6) 0.406(5) 0.103 Uiso 1 1 d D . . H50B H 0.029(3) 0.154(6) 0.316(8) 0.103 Uiso 1 1 d D . . O60 O 0.0849(3) 0.1138(3) 0.8132(4) 0.0508(11) Uani 1 1 d D . . H60A H 0.094(5) 0.145(4) 0.777(6) 0.076 Uiso 1 1 d D . . H60B H 0.109(5) 0.068(3) 0.832(6) 0.076 Uiso 1 1 d D . . O70 O 0.3248(3) 0.4691(3) 0.6062(4) 0.0502(11) Uani 1 1 d D . . H70A H 0.306(5) 0.458(5) 0.641(6) 0.075 Uiso 1 1 d D . . H70B H 0.361(4) 0.435(4) 0.633(6) 0.075 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0197(2) 0.0239(2) 0.0245(2) 0.00446(13) 0.01035(18) 0.00091(15) C1 0.019(2) 0.022(2) 0.026(2) 0.0025(18) 0.0118(19) 0.0028(19) N11 0.023(2) 0.025(2) 0.0239(19) 0.0012(15) 0.0137(17) -0.0010(17) C12 0.026(2) 0.026(2) 0.024(2) 0.0009(18) 0.016(2) 0.001(2) C13 0.024(3) 0.033(3) 0.028(2) 0.0055(19) 0.013(2) 0.003(2) C14 0.019(3) 0.043(3) 0.035(3) 0.000(2) 0.012(2) -0.002(2) C15 0.028(3) 0.035(3) 0.034(2) -0.002(2) 0.020(2) -0.007(2) C16 0.031(3) 0.024(3) 0.029(2) 0.0013(19) 0.018(2) -0.002(2) N21 0.022(2) 0.028(2) 0.0233(18) 0.0020(16) 0.0121(17) -0.0029(17) C22 0.022(2) 0.028(3) 0.026(2) 0.0028(18) 0.015(2) -0.001(2) C23 0.032(3) 0.029(3) 0.032(2) 0.003(2) 0.019(2) 0.002(2) C24 0.045(3) 0.032(3) 0.042(3) -0.007(2) 0.027(3) -0.003(2) C25 0.041(3) 0.041(3) 0.032(3) -0.009(2) 0.018(3) -0.007(3) C26 0.030(3) 0.040(3) 0.024(2) 0.002(2) 0.013(2) -0.003(2) O30 0.0241(19) 0.036(2) 0.0367(19) 0.0104(15) 0.0121(17) 0.0022(15) C30 0.027(3) 0.061(4) 0.075(5) 0.026(4) 0.021(3) 0.005(3) C31 0.026(3) 0.030(3) 0.048(3) 0.007(2) 0.016(3) 0.002(2) O31 0.035(2) 0.063(3) 0.057(2) 0.026(2) 0.027(2) 0.010(2) O40 0.033(2) 0.0267(19) 0.0375(19) 0.0047(15) 0.0182(17) 0.0036(15) O41 0.082(3) 0.038(2) 0.047(2) 0.0080(18) 0.040(2) 0.017(2) C40 0.086(5) 0.037(4) 0.062(4) 0.006(3) 0.044(4) 0.016(4) C41 0.033(3) 0.033(3) 0.041(3) 0.003(2) 0.019(2) 0.008(2) O50 0.103(4) 0.053(3) 0.068(3) -0.001(3) 0.060(4) 0.006(3) O60 0.058(3) 0.036(2) 0.069(3) 0.006(2) 0.043(3) 0.007(2) O70 0.046(3) 0.053(3) 0.052(2) 0.006(2) 0.029(2) 0.002(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 Pd1 O30 2.016(4) . ? Pd1 N21 2.017(4) . ? Pd1 N11 2.024(4) . ? Pd1 O40 2.028(4) . ? C1 C1 1.339(9) 5_566 ? C1 C12 1.497(7) . ? C1 C22 1.497(6) . ? N11 C16 1.346(6) . ? N11 C12 1.357(6) . ? C12 C13 1.385(6) . ? C13 C14 1.388(7) . ? C14 C15 1.384(7) . ? C15 C16 1.383(7) . ? N21 C26 1.351(6) . ? N21 C22 1.361(6) . ? C22 C23 1.386(7) . ? C23 C24 1.385(7) . ? C24 C25 1.383(8) . ? C25 C26 1.380(8) . ? O30 C31 1.285(7) . ? C30 C31 1.517(8) . ? C31 O31 1.229(7) . ? O40 C41 1.296(6) . ? O41 C41 1.221(6) . ? C40 C41 1.525(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 O30 Pd1 N21 91.20(15) . . ? O30 Pd1 N11 178.14(14) . . ? N21 Pd1 N11 89.70(15) . . ? O30 Pd1 O40 87.45(14) . . ? N21 Pd1 O40 176.61(13) . . ? N11 Pd1 O40 91.57(14) . . ? C1 C1 C12 122.2(5) 5_566 . ? C1 C1 C22 122.0(5) 5_566 . ? C12 C1 C22 115.7(4) . . ? C16 N11 C12 118.6(4) . . ? C16 N11 Pd1 121.8(3) . . ? C12 N11 Pd1 119.5(3) . . ? N11 C12 C13 121.7(4) . . ? N11 C12 C1 116.1(4) . . ? C13 C12 C1 122.2(4) . . ? C12 C13 C14 119.3(5) . . ? C15 C14 C13 118.9(5) . . ? C16 C15 C14 119.2(5) . . ? N11 C16 C15 122.2(4) . . ? C26 N21 C22 118.9(4) . . ? C26 N21 Pd1 121.7(3) . . ? C22 N21 Pd1 119.4(3) . . ? N21 C22 C23 121.6(4) . . ? N21 C22 C1 116.2(4) . . ? C23 C22 C1 122.2(4) . . ? C24 C23 C22 119.2(5) . . ? C25 C24 C23 118.9(5) . . ? C26 C25 C24 119.9(5) . . ? N21 C26 C25 121.5(5) . . ? C31 O30 Pd1 116.1(3) . . ? O31 C31 O30 124.1(5) . . ? O31 C31 C30 121.4(5) . . ? O30 C31 C30 114.5(5) . . ? C41 O40 Pd1 118.1(3) . . ? O41 C41 O40 124.4(5) . . ? O41 C41 C40 121.4(5) . . ? O40 C41 C40 114.2(5) . . ? 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 O30 Pd1 N11 C16 -23(5) . . . . ? N21 Pd1 N11 C16 -141.3(4) . . . . ? O40 Pd1 N11 C16 35.6(4) . . . . ? O30 Pd1 N11 C12 161(4) . . . . ? N21 Pd1 N11 C12 42.1(3) . . . . ? O40 Pd1 N11 C12 -141.1(3) . . . . ? C16 N11 C12 C13 1.1(7) . . . . ? Pd1 N11 C12 C13 177.8(3) . . . . ? C16 N11 C12 C1 -179.2(4) . . . . ? Pd1 N11 C12 C1 -2.5(5) . . . . ? C1 C1 C12 N11 126.5(6) 5_566 . . . ? C22 C1 C12 N11 -56.7(5) . . . . ? C1 C1 C12 C13 -53.8(8) 5_566 . . . ? C22 C1 C12 C13 123.0(5) . . . . ? N11 C12 C13 C14 -1.5(7) . . . . ? C1 C12 C13 C14 178.8(4) . . . . ? C12 C13 C14 C15 0.9(7) . . . . ? C13 C14 C15 C16 0.1(7) . . . . ? C12 N11 C16 C15 0.0(7) . . . . ? Pd1 N11 C16 C15 -176.7(4) . . . . ? C14 C15 C16 N11 -0.6(7) . . . . ? O30 Pd1 N21 C26 -37.4(4) . . . . ? N11 Pd1 N21 C26 141.0(4) . . . . ? O40 Pd1 N21 C26 29(3) . . . . ? O30 Pd1 N21 C22 141.0(4) . . . . ? N11 Pd1 N21 C22 -40.6(4) . . . . ? O40 Pd1 N21 C22 -153(2) . . . . ? C26 N21 C22 C23 -2.1(7) . . . . ? Pd1 N21 C22 C23 179.5(4) . . . . ? C26 N21 C22 C1 178.6(4) . . . . ? Pd1 N21 C22 C1 0.1(5) . . . . ? C1 C1 C22 N21 -125.0(6) 5_566 . . . ? C12 C1 C22 N21 58.2(6) . . . . ? C1 C1 C22 C23 55.7(8) 5_566 . . . ? C12 C1 C22 C23 -121.1(5) . . . . ? N21 C22 C23 C24 1.4(8) . . . . ? C1 C22 C23 C24 -179.3(5) . . . . ? C22 C23 C24 C25 0.0(8) . . . . ? C23 C24 C25 C26 -0.6(9) . . . . ? C22 N21 C26 C25 1.5(7) . . . . ? Pd1 N21 C26 C25 179.9(4) . . . . ? C24 C25 C26 N21 -0.1(9) . . . . ? N21 Pd1 O30 C31 -74.3(4) . . . . ? N11 Pd1 O30 C31 167(4) . . . . ? O40 Pd1 O30 C31 108.9(4) . . . . ? Pd1 O30 C31 O31 6.3(8) . . . . ? Pd1 O30 C31 C30 -174.5(4) . . . . ? O30 Pd1 O40 C41 -106.5(4) . . . . ? N21 Pd1 O40 C41 -173(2) . . . . ? N11 Pd1 O40 C41 75.1(4) . . . . ? Pd1 O40 C41 O41 -7.4(8) . . . . ? Pd1 O40 C41 C40 173.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.324 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.068 #===END data_Compound-24 _database_code_CSD 216646 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 24 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 N4 O10 Zn2' _chemical_formula_weight 739.34 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' Zn Zn 0.2839 1.4301 '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 8.435(2) _cell_length_b 8.818(2) _cell_length_c 10.670(3) _cell_angle_alpha 78.723(3) _cell_angle_beta 82.103(3) _cell_angle_gamma 88.974(3) _cell_volume 771.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 6765 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.38 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 1.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.835616 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 9413 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.38 _reflns_number_total 3050 _reflns_number_gt 2831 _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^)+(0.0429P)^2^+0.5256P] 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 3050 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.002 _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 -0.18441(3) -0.24715(3) -0.18151(2) 0.01930(9) Uani 1 1 d . . . C1 C -0.0630(2) 0.0013(2) -0.03182(19) 0.0167(4) Uani 1 1 d . . . N11 N -0.2866(2) -0.17724(19) -0.01213(16) 0.0176(3) Uani 1 1 d . . . C12 C -0.2221(2) -0.0640(2) 0.03430(18) 0.0168(4) Uani 1 1 d . . . C13 C -0.3019(2) -0.0028(2) 0.13629(19) 0.0210(4) Uani 1 1 d . . . H13A H -0.2539 0.0776 0.1663 0.025 Uiso 1 1 calc R . . C14 C -0.4517(3) -0.0604(2) 0.1933(2) 0.0233(4) Uani 1 1 d . . . H14A H -0.5094 -0.0187 0.2615 0.028 Uiso 1 1 calc R . . C15 C -0.5158(2) -0.1802(2) 0.1489(2) 0.0237(4) Uani 1 1 d . . . H15A H -0.6165 -0.2246 0.1885 0.028 Uiso 1 1 calc R . . C16 C -0.4311(2) -0.2344(2) 0.0460(2) 0.0219(4) Uani 1 1 d . . . H16A H -0.4769 -0.3153 0.0151 0.026 Uiso 1 1 calc R . . N21 N -0.1133(2) -0.0017(2) -0.24940(16) 0.0203(4) Uani 1 1 d . . . C22 C -0.0597(2) 0.0811(2) -0.16975(19) 0.0170(4) Uani 1 1 d . . . C23 C -0.0128(2) 0.2355(2) -0.2110(2) 0.0211(4) Uani 1 1 d . . . H23A H 0.0223 0.2920 -0.1526 0.025 Uiso 1 1 calc R . . C24 C -0.0182(3) 0.3057(3) -0.3390(2) 0.0253(5) Uani 1 1 d . . . H24A H 0.0130 0.4110 -0.3690 0.030 Uiso 1 1 calc R . . C25 C -0.0698(3) 0.2201(3) -0.4222(2) 0.0275(5) Uani 1 1 d . . . H25A H -0.0727 0.2648 -0.5104 0.033 Uiso 1 1 calc R . . C26 C -0.1169(3) 0.0681(3) -0.3735(2) 0.0252(5) Uani 1 1 d . . . H26A H -0.1536 0.0099 -0.4301 0.030 Uiso 1 1 calc R . . C30 C -0.3480(3) -0.3312(3) -0.3816(2) 0.0261(5) Uani 1 1 d . . . O30 O -0.32586(18) -0.22421(18) -0.31858(15) 0.0269(3) Uani 1 1 d . . . O31 O -0.3185(2) -0.4702(2) -0.34749(18) 0.0379(4) Uani 1 1 d . . . C31 C -0.4139(3) -0.2756(3) -0.5078(2) 0.0398(6) Uani 1 1 d . . . H31A H -0.4263 -0.3636 -0.5493 0.060 Uiso 1 1 calc R . . H31B H -0.3398 -0.1997 -0.5648 0.060 Uiso 1 1 calc R . . H31C H -0.5182 -0.2275 -0.4907 0.060 Uiso 1 1 calc R . . O40 O 0.02278(19) -0.32272(19) -0.25638(15) 0.0294(4) Uani 1 1 d . . . C40 C 0.1209(3) -0.3575(2) -0.1755(2) 0.0221(4) Uani 1 1 d . . . O41 O 0.0919(2) -0.34105(19) -0.06143(15) 0.0311(4) Uani 1 1 d . . . C41 C 0.2798(3) -0.4193(3) -0.2256(3) 0.0356(6) Uani 1 1 d . . . H41A H 0.3463 -0.4423 -0.1559 0.053 Uiso 1 1 calc R . . H41B H 0.3340 -0.3419 -0.2963 0.053 Uiso 1 1 calc R . . H41C H 0.2624 -0.5141 -0.2571 0.053 Uiso 1 1 calc R . . O50 O -0.27559(19) -0.47736(17) -0.10296(15) 0.0267(3) Uani 1 1 d . . . H50A H -0.2750 -0.5035 -0.1814 0.040 Uiso 1 1 d R . . H50B H -0.2137 -0.5421 -0.0614 0.040 Uiso 1 1 d 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 Zn1 0.01912(14) 0.01953(14) 0.02014(14) -0.00548(9) -0.00330(9) -0.00090(9) C1 0.0172(10) 0.0145(9) 0.0180(9) -0.0037(7) -0.0003(7) -0.0011(7) N11 0.0148(8) 0.0174(8) 0.0201(8) -0.0016(6) -0.0030(6) -0.0016(6) C12 0.0161(9) 0.0165(9) 0.0169(9) 0.0009(7) -0.0046(7) 0.0001(7) C13 0.0220(11) 0.0209(10) 0.0205(10) -0.0036(8) -0.0040(8) -0.0007(8) C14 0.0214(10) 0.0255(11) 0.0208(10) -0.0017(8) 0.0007(8) 0.0030(8) C15 0.0153(10) 0.0246(11) 0.0285(11) -0.0001(9) -0.0001(8) -0.0028(8) C16 0.0180(10) 0.0195(10) 0.0276(11) -0.0019(8) -0.0044(8) -0.0035(8) N21 0.0214(9) 0.0213(9) 0.0175(8) -0.0030(7) -0.0016(7) -0.0015(7) C22 0.0124(9) 0.0201(10) 0.0179(10) -0.0033(8) -0.0007(7) 0.0006(7) C23 0.0205(10) 0.0209(10) 0.0213(10) -0.0032(8) -0.0017(8) -0.0012(8) C24 0.0282(12) 0.0207(10) 0.0242(11) 0.0012(8) -0.0015(9) -0.0017(9) C25 0.0332(13) 0.0295(12) 0.0171(10) 0.0017(9) -0.0032(9) -0.0008(9) C26 0.0287(12) 0.0296(12) 0.0178(10) -0.0059(8) -0.0034(8) -0.0025(9) C30 0.0225(11) 0.0321(12) 0.0254(11) -0.0082(9) -0.0053(9) -0.0028(9) O30 0.0279(8) 0.0255(8) 0.0302(8) -0.0066(6) -0.0128(7) 0.0001(6) O31 0.0478(11) 0.0319(10) 0.0407(10) -0.0149(8) -0.0188(8) 0.0069(8) C31 0.0475(16) 0.0464(16) 0.0287(13) -0.0083(11) -0.0149(11) -0.0030(12) O40 0.0254(8) 0.0360(9) 0.0248(8) -0.0023(7) -0.0025(6) 0.0067(7) C40 0.0220(11) 0.0156(10) 0.0270(11) -0.0015(8) -0.0006(8) -0.0036(8) O41 0.0352(9) 0.0322(9) 0.0264(8) -0.0088(7) -0.0022(7) 0.0010(7) C41 0.0264(12) 0.0430(14) 0.0360(13) -0.0066(11) -0.0018(10) 0.0071(10) O50 0.0310(9) 0.0223(8) 0.0267(8) -0.0039(6) -0.0048(6) -0.0006(6) _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 O40 1.9799(16) . ? Zn1 O30 1.9897(15) . ? Zn1 N11 2.0923(17) . ? Zn1 O50 2.1514(16) . ? Zn1 N21 2.2095(18) . ? C1 C1 1.336(4) 2 ? C1 C12 1.496(3) . ? C1 C22 1.499(3) . ? N11 C16 1.348(3) . ? N11 C12 1.351(3) . ? C12 C13 1.394(3) . ? C13 C14 1.385(3) . ? C14 C15 1.385(3) . ? C15 C16 1.387(3) . ? N21 C22 1.349(3) . ? N21 C26 1.351(3) . ? C22 C23 1.393(3) . ? C23 C24 1.391(3) . ? C24 C25 1.389(3) . ? C25 C26 1.384(3) . ? C30 O31 1.239(3) . ? C30 O30 1.291(3) . ? C30 C31 1.516(3) . ? O40 C40 1.268(3) . ? C40 O41 1.244(3) . ? C40 C41 1.507(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 O40 Zn1 O30 106.10(7) . . ? O40 Zn1 N11 139.17(7) . . ? O30 Zn1 N11 114.63(7) . . ? O40 Zn1 O50 92.98(7) . . ? O30 Zn1 O50 90.63(6) . . ? N11 Zn1 O50 89.46(6) . . ? O40 Zn1 N21 93.12(7) . . ? O30 Zn1 N21 88.85(6) . . ? N11 Zn1 N21 85.12(6) . . ? O50 Zn1 N21 173.78(6) . . ? C1 C1 C12 121.6(2) 2 . ? C1 C1 C22 122.8(2) 2 . ? C12 C1 C22 115.39(17) . . ? C16 N11 C12 117.84(17) . . ? C16 N11 Zn1 119.17(14) . . ? C12 N11 Zn1 122.58(13) . . ? N11 C12 C13 122.28(18) . . ? N11 C12 C1 117.75(17) . . ? C13 C12 C1 119.91(17) . . ? C14 C13 C12 119.25(19) . . ? C15 C14 C13 118.6(2) . . ? C14 C15 C16 119.22(19) . . ? N11 C16 C15 122.75(19) . . ? C22 N21 C26 118.06(18) . . ? C22 N21 Zn1 121.17(13) . . ? C26 N21 Zn1 120.73(14) . . ? N21 C22 C23 122.03(18) . . ? N21 C22 C1 116.42(17) . . ? C23 C22 C1 121.44(18) . . ? C24 C23 C22 119.09(19) . . ? C25 C24 C23 119.2(2) . . ? C26 C25 C24 118.3(2) . . ? N21 C26 C25 123.3(2) . . ? O31 C30 O30 125.4(2) . . ? O31 C30 C31 119.7(2) . . ? O30 C30 C31 114.9(2) . . ? C30 O30 Zn1 123.73(15) . . ? C40 O40 Zn1 113.32(14) . . ? O41 C40 O40 123.4(2) . . ? O41 C40 C41 120.6(2) . . ? O40 C40 C41 116.0(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 O40 Zn1 N11 C16 -132.35(15) . . . . ? O30 Zn1 N11 C16 52.04(16) . . . . ? O50 Zn1 N11 C16 -38.41(15) . . . . ? N21 Zn1 N11 C16 138.53(15) . . . . ? O40 Zn1 N11 C12 55.16(19) . . . . ? O30 Zn1 N11 C12 -120.45(15) . . . . ? O50 Zn1 N11 C12 149.10(15) . . . . ? N21 Zn1 N11 C12 -33.96(15) . . . . ? C16 N11 C12 C13 -1.9(3) . . . . ? Zn1 N11 C12 C13 170.68(14) . . . . ? C16 N11 C12 C1 -178.91(17) . . . . ? Zn1 N11 C12 C1 -6.3(2) . . . . ? C1 C1 C12 N11 -122.1(3) 2 . . . ? C22 C1 C12 N11 63.0(2) . . . . ? C1 C1 C12 C13 60.8(3) 2 . . . ? C22 C1 C12 C13 -114.1(2) . . . . ? N11 C12 C13 C14 0.6(3) . . . . ? C1 C12 C13 C14 177.56(18) . . . . ? C12 C13 C14 C15 1.6(3) . . . . ? C13 C14 C15 C16 -2.5(3) . . . . ? C12 N11 C16 C15 1.0(3) . . . . ? Zn1 N11 C16 C15 -171.84(16) . . . . ? C14 C15 C16 N11 1.2(3) . . . . ? O40 Zn1 N21 C22 -98.91(16) . . . . ? O30 Zn1 N21 C22 155.02(16) . . . . ? N11 Zn1 N21 C22 40.18(15) . . . . ? O50 Zn1 N21 C22 69.7(6) . . . . ? O40 Zn1 N21 C26 78.69(17) . . . . ? O30 Zn1 N21 C26 -27.37(16) . . . . ? N11 Zn1 N21 C26 -142.21(17) . . . . ? O50 Zn1 N21 C26 -112.7(5) . . . . ? C26 N21 C22 C23 1.7(3) . . . . ? Zn1 N21 C22 C23 179.36(14) . . . . ? C26 N21 C22 C1 177.91(18) . . . . ? Zn1 N21 C22 C1 -4.4(2) . . . . ? C1 C1 C22 N21 130.4(3) 2 . . . ? C12 C1 C22 N21 -54.8(2) . . . . ? C1 C1 C22 C23 -53.3(3) 2 . . . ? C12 C1 C22 C23 121.5(2) . . . . ? N21 C22 C23 C24 -1.4(3) . . . . ? C1 C22 C23 C24 -177.38(19) . . . . ? C22 C23 C24 C25 -0.1(3) . . . . ? C23 C24 C25 C26 1.2(3) . . . . ? C22 N21 C26 C25 -0.6(3) . . . . ? Zn1 N21 C26 C25 -178.27(17) . . . . ? C24 C25 C26 N21 -0.8(4) . . . . ? O31 C30 O30 Zn1 18.2(3) . . . . ? C31 C30 O30 Zn1 -161.04(16) . . . . ? O40 Zn1 O30 C30 50.45(18) . . . . ? N11 Zn1 O30 C30 -132.53(17) . . . . ? O50 Zn1 O30 C30 -42.84(18) . . . . ? N21 Zn1 O30 C30 143.37(18) . . . . ? O30 Zn1 O40 C40 -173.48(14) . . . . ? N11 Zn1 O40 C40 10.7(2) . . . . ? O50 Zn1 O40 C40 -81.95(15) . . . . ? N21 Zn1 O40 C40 96.82(15) . . . . ? Zn1 O40 C40 O41 -2.2(3) . . . . ? Zn1 O40 C40 C41 178.64(15) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.487 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.071