Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Oscar Castillo' _publ_contact_author_address ; Quimica Inorganica Universidad del Pais Vasco Apdo. 644, 48080 Bilbao 48080 SPAIN ; _publ_contact_author_email OSCAR.CASTILLO@EHU.ES _publ_section_title ; Supramolecular architectures assembled by the interaction of purine nucleobases with metal-oxalato frameworks. Non-covalent stabilization of the 7H-adenine tautomer in the solid-state ; loop_ _publ_author_name 'Oscar Castillo' 'Garikoitz Beobide' 'Urko Garcia-Couceiro' 'Juan P. Garcia-Teran' ; A.Luque ; 'P. Roman' # Attachment 'CASTILLO.CIF' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 278470' _audit_creation_method SHELXL _chemical_name_systematic ; catena-[aqua(mu-oxalato)(purine)manganese(II)] ; _chemical_formula_moiety 'C7 H6 Mn1 N4 O5' _chemical_formula_structural 'C7 H6 Mn1 N4 O5' _chemical_formula_sum 'C7 H6 Mn N4 O5' _chemical_formula_weight 281.10 _chemical_compound_source 'synthesis as described' 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 6.913(1) _cell_length_b 16.283(3) _cell_length_c 8.594(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.09(2) _cell_angle_gamma 90.00 _cell_volume 934.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7058 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 28.09 _exptl_crystal_description polyhedric _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_meas 1.99(1) _exptl_crystal_density_method flotation _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 1.433 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.921 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Xcalibur _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7058 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 28.09 _reflns_number_total 2272 _reflns_number_gt 1409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2003)' _computing_structure_solution 'Sir92 (Altamore et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2272 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Mn Mn 0.66882(5) 0.08130(2) 0.79099(4) 0.0235(1) Uani 1 1 d . . . C9 C 0.6039(3) 0.0000(1) 0.4805(3) 0.0208(5) Uani 1 1 d . . . O1 O 0.7497(2) 0.0281(1) 0.58475(17) 0.0255(4) Uani 1 1 d . . . O2 O 0.3907(2) 0.0277(1) 0.65550(18) 0.0232(4) Uani 1 1 d . . . C10 C 0.9346(4) -0.0385(1) 1.0036(3) 0.0222(5) Uani 1 1 d . . . O3 O 0.7515(2) -0.0322(1) 0.93567(18) 0.0271(4) Uani 1 1 d . . . O4 O 0.9797(2) 0.0999(1) 0.92348(18) 0.0281(4) Uani 1 1 d . . . O5w O 0.5382(3) 0.1283(1) 0.9776(2) 0.0289(4) Uani 1 1 d . . . N1 N 0.3034(3) 0.2954(1) 0.2354(2) 0.0291(5) Uani 1 1 d . . . C2 C 0.3180(4) 0.2149(2) 0.2625(3) 0.0289(6) Uani 1 1 d . . . N3 N 0.4153(3) 0.1749(1) 0.3952(2) 0.0240(5) Uani 1 1 d . . . C4 C 0.5094(3) 0.2260(1) 0.5135(3) 0.0196(5) Uani 1 1 d . . . C5 C 0.5065(3) 0.3109(1) 0.4962(3) 0.0220(5) Uani 1 1 d . . . C6 C 0.3998(4) 0.3453(2) 0.3535(3) 0.0296(6) Uani 1 1 d . . . N7 N 0.6187(3) 0.3404(1) 0.6402(3) 0.0283(6) Uani 1 1 d . . . C8 C 0.6815(4) 0.2755(2) 0.7354(3) 0.0259(6) Uani 1 1 d . . . N9 N 0.6191(3) 0.2042(1) 0.6667(2) 0.0219(5) Uani 1 1 d . . . H51w H 0.614(4) 0.150(2) 1.052(3) 0.033 Uiso 1 1 d . . . H52w H 0.467(4) 0.103(2) 1.013(3) 0.033 Uiso 1 1 d . . . H2 H 0.256(3) 0.182(1) 0.182(3) 0.026 Uiso 1 1 d . . . H6 H 0.386(3) 0.402(1) 0.337(3) 0.026 Uiso 1 1 d . . . H7 H 0.658(4) 0.381(2) 0.663(3) 0.026 Uiso 1 1 d . . . H8 H 0.769(3) 0.281(1) 0.838(3) 0.026 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.0247(2) 0.0231(2) 0.01967(19) 0.00001(18) 0.00061(15) 0.00121(18) C9 0.0244(14) 0.0122(12) 0.0252(14) 0.0030(10) 0.0051(11) 0.0024(10) O1 0.0207(9) 0.0313(10) 0.0225(9) -0.0051(7) 0.0022(8) -0.0029(7) O2 0.0244(9) 0.0252(9) 0.0197(9) -0.0042(7) 0.0053(7) 0.0011(7) C10 0.0294(14) 0.0207(14) 0.0165(12) -0.0010(11) 0.0059(11) -0.0025(11) O3 0.0192(9) 0.0267(10) 0.0310(10) 0.0050(8) -0.0015(8) -0.0043(7) O4 0.0280(9) 0.0214(10) 0.0301(10) 0.0075(8) -0.0010(8) -0.0022(7) O5w 0.0309(11) 0.0339(12) 0.0214(10) -0.0041(8) 0.0061(8) -0.0081(8) N1 0.0297(13) 0.0315(13) 0.0265(12) 0.0062(10) 0.0080(10) 0.0056(10) C2 0.0215(14) 0.0384(17) 0.0264(15) -0.0089(13) 0.0056(12) -0.0019(12) N3 0.0249(12) 0.0248(12) 0.0218(11) -0.0020(9) 0.0050(9) -0.0008(9) C4 0.0183(13) 0.0202(13) 0.0217(13) 0.0009(10) 0.0075(11) 0.0004(10) C5 0.0205(13) 0.0219(13) 0.0260(13) -0.0009(11) 0.0104(11) -0.0009(10) C6 0.0334(16) 0.0232(14) 0.0361(16) 0.0069(13) 0.0163(13) 0.0094(12) N7 0.0352(14) 0.0174(12) 0.0330(13) -0.0061(10) 0.0101(11) -0.0065(10) C8 0.0250(15) 0.0303(16) 0.0220(14) 0.0003(12) 0.0054(12) -0.0018(12) N9 0.0221(11) 0.0219(11) 0.0208(11) 0.0007(9) 0.0041(9) -0.0007(9) _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 Mn O1 2.173(2) . ? Mn O2 2.156(2) . ? Mn O3 2.217(2) . ? Mn O4 2.175(2) . ? Mn O5W 2.174(2) . ? Mn N9 2.253(2) . ? Mn Mn 5.603(1) 3_656 ? Mn Mn 5.685(1) 3_757 ? C9 O1 1.248(3) . ? C9 O2 1.263(3) 3_656 ? C9 C9 1.558(4) 3_656 ? O2 C9 1.263(3) 3_656 ? C10 O4 1.245(3) 3_757 ? C10 O3 1.252(3) . ? C10 C10 1.557(4) 3_757 ? O4 C10 1.245(3) 3_757 ? O5w H51w 0.80(2) . ? O5w H52w 0.77(2) . ? N1 C2 1.330(3) . ? N1 C6 1.335(3) . ? C2 N3 1.334(3) . ? C2 H2 0.89(2) . ? N3 C4 1.343(3) . ? C4 N9 1.383(3) . ? C4 C5 1.390(3) . ? C5 N7 1.365(3) . ? C5 C6 1.375(3) . ? C6 H6 0.94(2) . ? N7 C8 1.338(3) . ? N7 H7 0.72(2) . ? C8 N9 1.323(3) . ? C8 H8 0.94(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn O1 77.34(6) . . ? O2 Mn O5W 93.29(6) . . ? O1 Mn O5W 170.61(6) . . ? O2 Mn O4 163.67(6) . . ? O1 Mn O4 93.07(6) . . ? O5w Mn O4 96.21(7) . . ? O2 Mn O3 91.67(6) . . ? O1 Mn O3 92.39(6) . . ? O5w Mn O3 88.59(6) . . ? O4 Mn O3 75.36(5) . . ? O2 Mn N9 95.67(6) . . ? O1 Mn N9 90.42(6) . . ? O5w Mn N9 89.76(7) . . ? O4 Mn N9 97.61(6) . . ? O3 Mn N9 172.55(6) . . ? O1 C9 O2 125.6(2) . 3_656 ? O1 C9 C9 117.6(3) . 3_656 ? O2 C9 C9 116.8(2) 3_656 3_656 ? C9 O1 Mn 113.6(1) . . ? C9 O2 Mn 114.0(1) 3_656 . ? O4 C10 O3 126.3(2) 3_757 . ? O4 C10 C10 117.5(3) 3_757 3_757 ? O3 C10 C10 116.2(2) . 3_757 ? C10 O3 Mn 114.3(1) . . ? C10 O4 Mn 115.3(2) 3_757 . ? Mn O5w H51w 116(2) . . ? Mn O5w H52w 122(2) . . ? H51w O5w H52w 106(3) . . ? C2 N1 C6 117.8(2) . . ? N1 C2 N3 129.0(2) . . ? N1 C2 H2 118(1) . . ? N3 C2 H2 114(1) . . ? C2 N3 C4 112.5(2) . . ? N3 C4 N9 126.8(2) . . ? N3 C4 C5 123.0(2) . . ? N9 C4 C5 110.2(2) . . ? N7 C5 C6 135.3(2) . . ? N7 C5 C4 105.4(2) . . ? C6 C5 C4 119.3(2) . . ? N1 C6 C5 118.4(2) . . ? N1 C6 H6 118(1) . . ? C5 C6 H6 123(1) . . ? C8 N7 C5 107.1(2) . . ? C8 N7 H7 121(2) . . ? C5 N7 H7 131(2) . . ? N9 C8 N7 113.8(2) . . ? N9 C8 H8 124(1) . . ? N7 C8 H8 122(1) . . ? C8 N9 C4 103.6(2) . . ? C8 N9 Mn 125.2(2) . . ? C4 N9 Mn 131.1(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5w H51w N1 0.80(2) 1.98(2) 2.775(3) 179(3) 4_666 O5w H52w O3 0.77(2) 2.03(2) 2.792(2) 169(3) 3_657 N7 H7 O2 0.72(2) 2.20(2) 2.834(3) 147(3) 4_665 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.421 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.067 _chemical_name_common catena-(aqua(mu-oxalato)(purine)manganese(ii)) #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 278471' _audit_creation_method SHELXL _chemical_name_systematic ; catena-[diaqua(mu-oxalato)manganese(II)-adenine-water (1/1/1)] ; _chemical_formula_moiety 'C2 H4 Mn1 O6, C5 H5 N5, H2 O' _chemical_formula_structural 'C2 H4 Mn1 O6, C5 H5 N5, H2 O' _chemical_formula_sum 'C7 H11 Mn N5 O7' _chemical_formula_weight 332.15 _chemical_compound_source 'synthesis as described' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.340(1) _cell_length_b 9.513(2) _cell_length_c 9.741(2) _cell_angle_alpha 75.47(2) _cell_angle_beta 80.60(2) _cell_angle_gamma 75.17(2) _cell_volume 632.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5463 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 28.06 _exptl_crystal_description polyhedric _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_meas 1.74(1) _exptl_crystal_density_method flotation _exptl_crystal_F_000 338 _exptl_absorpt_coefficient_mu 1.085 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_absorpt_correction_T_min 0.859 _exptl_absorpt_correction_T_max 0.945 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Xcalibur _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5463 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.1037 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 28.06 _reflns_number_total 3036 _reflns_number_gt 1673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2003)' _computing_structure_solution 'Sir92 (Altamore et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0172P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3036 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Mn Mn 0.19328(5) 0.19469(4) 0.56830(4) 0.03165(13) Uani 1 1 d . . . O1 O 0.0939(2) 0.3763(2) 0.3870(2) 0.0357(4) Uani 1 1 d . . . O2 O 0.0631(2) 0.3862(2) 0.6637(2) 0.0343(4) Uani 1 1 d . . . C9 C 0.0079(3) 0.4969(3) 0.4206(2) 0.0275(6) Uani 1 1 d . . . O3 O -0.0784(2) 0.1216(2) 0.6165(2) 0.0373(4) Uani 1 1 d . . . O4 O 0.2305(2) 0.0241(2) 0.4460(2) 0.0371(4) Uani 1 1 d . . . C10 C -0.0885(3) 0.0284(3) 0.5489(2) 0.0296(6) Uani 1 1 d . . . O5w O 0.2855(3) 0.0506(2) 0.7592(2) 0.0481(6) Uani 1 1 d . . . O6w O 0.4708(2) 0.2323(2) 0.5026(2) 0.0411(5) Uani 1 1 d . . . N1 N 0.4287(3) 0.3350(2) -0.1110(2) 0.0362(5) Uani 1 1 d . . . C2 C 0.4678(4) 0.4369(3) -0.2287(3) 0.0416(7) Uani 1 1 d . . . N3 N 0.4089(3) 0.5830(2) -0.2544(2) 0.0393(6) Uani 1 1 d . . . C4 C 0.2921(3) 0.6308(3) -0.1452(3) 0.0331(6) Uani 1 1 d . . . C5 C 0.2401(3) 0.5357(2) -0.0197(2) 0.0272(6) Uani 1 1 d . . . C6 C 0.3129(3) 0.3822(3) -0.0014(3) 0.0297(6) Uani 1 1 d . . . N6 N 0.2738(3) 0.2819(2) 0.1147(2) 0.0386(6) Uani 1 1 d . . . N7 N 0.1196(3) 0.6269(2) 0.0622(2) 0.0343(5) Uani 1 1 d . . . C8 C 0.1068(4) 0.7667(3) -0.0140(3) 0.0426(7) Uani 1 1 d . . . N9 N 0.2073(3) 0.7763(2) -0.1408(2) 0.0405(6) Uani 1 1 d . . . O7w O 0.6290(3) 0.0500(2) 0.8551(2) 0.0497(6) Uani 1 1 d . . . H51w H 0.272(4) -0.053(3) 0.790(3) 0.074 Uiso 1 1 d . . . H52w H 0.386(4) 0.053(3) 0.790(3) 0.074 Uiso 1 1 d . . . H61w H 0.542(4) 0.164(3) 0.507(3) 0.074 Uiso 1 1 d . . . H62w H 0.513(4) 0.291(3) 0.419(3) 0.074 Uiso 1 1 d . . . H2 H 0.555(3) 0.399(3) -0.307(3) 0.060 Uiso 1 1 d . . . H61 H 0.322(3) 0.196(3) 0.109(3) 0.060 Uiso 1 1 d . . . H62 H 0.207(4) 0.320(3) 0.184(3) 0.060 Uiso 1 1 d . . . H7 H 0.062(3) 0.602(3) 0.146(3) 0.060 Uiso 1 1 d . . . H8 H 0.027(3) 0.844(3) 0.029(3) 0.060 Uiso 1 1 d . . . H71w H 0.716(4) 0.063(3) 0.785(3) 0.074 Uiso 1 1 d . . . H72w H 0.582(4) 0.122(3) 0.882(3) 0.074 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.0323(2) 0.0243(2) 0.0342(2) -0.00376(18) -0.00011(18) -0.00366(16) O1 0.0446(11) 0.0242(9) 0.0308(10) -0.0071(8) -0.0035(8) 0.0062(8) O2 0.0453(11) 0.0234(9) 0.0252(9) 0.0001(8) -0.0035(8) 0.0029(8) C9 0.0244(14) 0.0273(14) 0.0293(14) -0.0071(12) 0.0012(12) -0.0047(11) O3 0.0294(10) 0.0405(11) 0.0458(11) -0.0222(9) 0.0049(8) -0.0080(8) O4 0.0259(10) 0.0367(10) 0.0491(11) -0.0164(9) 0.0066(8) -0.0076(8) C10 0.0247(15) 0.0270(14) 0.0309(15) -0.0030(12) -0.0008(11) 0.0006(11) O5w 0.0585(14) 0.0318(11) 0.0537(13) 0.0120(10) -0.0242(10) -0.0190(10) O6w 0.0307(12) 0.0356(12) 0.0453(12) 0.0042(10) 0.0032(10) -0.0040(8) N1 0.0418(13) 0.0309(12) 0.0357(13) -0.0103(11) 0.0023(11) -0.0089(10) C2 0.0456(18) 0.0446(18) 0.0355(17) -0.0118(15) 0.0039(14) -0.0139(14) N3 0.0459(14) 0.0371(14) 0.0321(13) -0.0033(11) 0.0065(11) -0.0153(11) C4 0.0357(15) 0.0296(15) 0.0343(16) -0.0020(13) -0.0044(13) -0.0123(12) C5 0.0290(14) 0.0256(14) 0.0270(14) -0.0046(12) -0.0015(11) -0.0081(11) C6 0.0335(15) 0.0304(15) 0.0276(14) -0.0040(12) -0.0059(12) -0.0121(12) N6 0.0506(16) 0.0251(12) 0.0345(14) -0.0037(11) 0.0017(11) -0.0050(11) N7 0.0396(14) 0.0293(12) 0.0318(13) -0.0054(11) 0.0013(11) -0.0079(10) C8 0.0463(18) 0.0289(16) 0.049(2) -0.0067(14) -0.0013(15) -0.0065(13) N9 0.0479(14) 0.0264(12) 0.0424(14) 0.0003(10) 0.0014(12) -0.0112(10) O7w 0.0642(15) 0.0357(12) 0.0446(14) -0.0139(10) 0.0179(10) -0.0132(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn O1 2.209(2) . ? Mn O2 2.183(2) . ? Mn O3 2.218(2) . ? Mn O4 2.182(2) . ? Mn O5w 2.110(2) . ? Mn O6w 2.126(2) . ? Mn Mn 5.699(1) 2_566 ? Mn Mn 5.712(1) 2_556 ? O1 C9 1.254(2) . ? O2 C9 1.252(2) 2_566 ? C9 O2 1.252(2) 2_566 ? C9 C9 1.547(4) 2_566 ? O3 C10 1.252(3) . ? O4 C10 1.256(3) 2_556 ? C10 O4 1.256(3) 2_556 ? C10 C10 1.543(4) 2_556 ? O5w H51w 0.98(3) . ? O5w H52w 0.85(3) . ? O6w H61w 0.72(3) . ? O6w H62w 0.92(3) . ? N1 C6 1.346(3) . ? N1 C2 1.347(3) . ? C2 N3 1.318(3) . ? C2 H2 0.99(2) . ? N3 C4 1.349(3) . ? C4 N9 1.373(3) . ? C4 C5 1.389(3) . ? C5 N7 1.377(3) . ? C5 C6 1.396(3) . ? C6 N6 1.328(3) . ? N6 H61 0.82(2) . ? N6 H62 0.86(2) . ? N7 C8 1.339(3) . ? N7 H7 0.86(2) . ? C8 N9 1.326(3) . ? C8 H8 0.95(2) . ? O7w H71w 0.86(3) . ? O7w H72w 0.77(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 O5w Mn O6w 90.24(8) . . ? O5w Mn O4 97.21(7) . . ? O6w Mn O4 94.35(7) . . ? O5w Mn O2 95.28(7) . . ? O6w Mn O2 100.28(7) . . ? O4 Mn O2 160.68(6) . . ? O5w Mn O1 170.27(7) . . ? O6w Mn O1 88.18(7) . . ? O4 Mn O1 92.49(6) . . ? O2 Mn O1 75.57(6) . . ? O5w Mn O3 89.82(7) . . ? O6w Mn O3 169.58(7) . . ? O4 Mn O3 75.30(6) . . ? O2 Mn O3 90.10(6) . . ? O1 Mn O3 93.46(7) . . ? C9 O1 Mn 114.5(2) . . ? C9 O2 Mn 115.6(1) 2_566 . ? O2 C9 O1 125.7(2) 2_566 . ? O2 C9 C9 117.1(2) 2_566 2_566 ? O1 C9 C9 117.3(3) . 2_566 ? C10 O3 Mn 114.2(1) . . ? C10 O4 Mn 115.9(2) 2_556 . ? O3 C10 O4 125.7(2) . 2_556 ? O3 C10 C10 117.7(3) . 2_556 ? O4 C10 C10 116.6(3) 2_556 2_556 ? Mn O5w H51w 124(2) . . ? Mn O5w H52w 121(2) . . ? H51w O5w H52w 106(2) . . ? Mn O6w H61w 112(3) . . ? Mn O6w H62w 128(2) . . ? H61w O6w H62w 102(3) . . ? C6 N1 C2 118.7(2) . . ? N3 C2 N1 128.9(2) . . ? N3 C2 H2 114(1) . . ? N1 C2 H2 117(1) . . ? C2 N3 C4 112.6(2) . . ? N3 C4 N9 126.2(2) . . ? N3 C4 C5 123.4(2) . . ? N9 C4 C5 110.5(2) . . ? N7 C5 C4 105.3(2) . . ? N7 C5 C6 134.9(2) . . ? C4 C5 C6 119.7(2) . . ? N6 C6 N1 118.8(2) . . ? N6 C6 C5 124.5(2) . . ? N1 C6 C5 116.6(2) . . ? C6 N6 H61 114(2) . . ? C6 N6 H62 114(2) . . ? H61 N6 H62 132(3) . . ? C8 N7 C5 106.5(2) . . ? C8 N7 H7 125(2) . . ? C5 N7 H7 129(2) . . ? N9 C8 N7 113.9(2) . . ? N9 C8 H8 130(2) . . ? N7 C8 H8 117(2) . . ? C8 N9 C4 103.9(2) . . ? H71w O7w H72w 113(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5w H51w N9 0.98(3) 1.75(3) 2.719(3) 169(2) 1_546 O5w H52w O7w 0.85(3) 1.98(3) 2.826(3) 177(3) . O6w H61w O4 0.72(3) 2.12(3) 2.831(2) 168(3) 2_656 O6w H62w N3 0.92(3) 1.85(3) 2.771(3) 178(2) 2_665 N6 H61 O7w 0.82(2) 2.22(3) 3.003(3) 161(2) 2_656 N6 H62 O1 0.86(2) 2.16(2) 3.005(3) 166(2) . N7 H7 O2 0.86(2) 1.94(3) 2.773(3) 161(2) 2_566 O7w H71w O3 0.86(3) 2.11(3) 2.967(2) 173(3) 1_655 O7w H72w N1 0.77(3) 2.06(3) 2.806(3) 162(3) 1_556 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.481 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.058 _chemical_name_common 'catena-(diaqua(mu-oxalato)manganese(ii)-adenine-water (1/1/1))' #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 278472' _audit_creation_method SHELXL97 _chemical_name_systematic ; adenine(aqua)oxalatocopper(II)-water (1/1.66) ; _chemical_formula_moiety 'C14 H14 Cu2 N10 O10, 3.33(H2 O)' _chemical_formula_structural '2(C7 H7 Cu N5 O5), 3.33(H2 O)' _chemical_formula_sum 'C14 H20.66 Cu2 N10 O13.33' _chemical_formula_weight 669.24 _chemical_compound_source 'synthesis as described' 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 3.587(1) _cell_length_b 17.965(2) _cell_length_c 18.010(2) _cell_angle_alpha 97.70(1) _cell_angle_beta 92.42(1) _cell_angle_gamma 91.87(1) _cell_volume 1148.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9791 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 28.06 _exptl_crystal_description prismatic _exptl_crystal_colour blue _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 1.93(1) _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method flotation _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.944 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.921 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Xcalibur _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9791 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.2041 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 28.06 _reflns_number_total 5540 _reflns_number_gt 2579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2003)' _computing_structure_solution 'Sir92 (Altamore et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_coef none _refine_ls_number_reflns 5540 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.117 _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 Cu1A Cu 0.2658(3) 0.19096(6) 0.18889(6) 0.0234(3) Uani 1 1 d . . . Cu1B Cu 0.5614(3) 0.68828(7) 0.30773(7) 0.0254(3) Uani 1 1 d . . . N1A N 0.8966(19) 0.2743(4) 0.4804(4) 0.0219(15) Uani 1 1 d U . . C2A C 0.721(3) 0.2136(5) 0.4409(5) 0.027(2) Uani 1 1 d U . . H2A H 0.6814 0.1739 0.4683 0.032 Uiso 1 1 calc R . . N3A N 0.5949(19) 0.2000(3) 0.3715(3) 0.0194(15) Uani 1 1 d U . . C4A C 0.667(2) 0.2584(5) 0.3344(5) 0.0131(12) Uani 1 1 d U . . C5A C 0.842(2) 0.3254(4) 0.3677(5) 0.0156(16) Uani 1 1 d U . . C6A C 0.963(2) 0.3347(4) 0.4419(4) 0.0131(14) Uani 1 1 d U . . N6A N 1.1299(18) 0.3972(4) 0.4781(4) 0.0266(17) Uani 1 1 d U . . H61A H 1.1987 0.3994 0.5247 0.032 Uiso 1 1 calc R . . H62A H 1.1691 0.4354 0.4549 0.032 Uiso 1 1 calc R . . N7A N 0.857(2) 0.3704(4) 0.3104(4) 0.0232(16) Uani 1 1 d U . . H7A H 0.9557 0.4151 0.3144 0.028 Uiso 1 1 calc R . . C8A C 0.691(2) 0.3319(5) 0.2475(5) 0.0198(18) Uani 1 1 d U . . H8A H 0.6609 0.3504 0.2019 0.024 Uiso 1 1 calc R . . N9A N 0.5752(18) 0.2628(4) 0.2600(4) 0.0187(14) Uani 1 1 d U . . N1B N 0.8929(19) 0.9793(4) 0.2413(4) 0.0224(15) Uani 1 1 d U . . C2B C 0.934(3) 0.9434(5) 0.3005(5) 0.027(2) Uani 1 1 d U . . H2B H 1.0397 0.9727 0.3432 0.033 Uiso 1 1 calc R . . N3B N 0.8481(18) 0.8714(4) 0.3092(4) 0.0210(12) Uani 1 1 d U . . C4B C 0.674(2) 0.8336(5) 0.2448(5) 0.0168(12) Uani 1 1 d U . . C5B C 0.606(2) 0.8639(5) 0.1806(5) 0.0153(15) Uani 1 1 d U . . C6B C 0.721(2) 0.9425(4) 0.1774(4) 0.0179(15) Uani 1 1 d U . . N6B N 0.661(2) 0.9746(4) 0.1178(4) 0.0293(18) Uani 1 1 d U . . H61B H 0.7302 1.0209 0.1178 0.035 Uiso 1 1 calc R . . H62B H 0.5509 0.9497 0.0784 0.035 Uiso 1 1 calc R . . N7B N 0.4399(19) 0.8079(4) 0.1303(4) 0.0203(15) Uani 1 1 d U . . H7B H 0.3668 0.8113 0.0848 0.024 Uiso 1 1 calc R . . C8B C 0.412(2) 0.7471(5) 0.1646(5) 0.0189(18) Uani 1 1 d U . . H8B H 0.3093 0.7008 0.1425 0.023 Uiso 1 1 calc R . . N9B N 0.552(2) 0.7617(4) 0.2358(4) 0.0222(17) Uani 1 1 d U . . C9A C -0.130(2) 0.1563(5) 0.0586(4) 0.025(2) Uani 1 1 d U . . C10A C 0.069(2) 0.2342(5) 0.0558(5) 0.0190(17) Uani 1 1 d U . . O1A O -0.0880(16) 0.1315(3) 0.1198(3) 0.0302(15) Uani 1 1 d U . . O2A O 0.2616(18) 0.2575(3) 0.1151(4) 0.0268(15) Uani 1 1 d U . . O3A O 0.0261(17) 0.2633(4) -0.0008(3) 0.0347(17) Uani 1 1 d U . . O4A O -0.3179(19) 0.1261(3) 0.0030(3) 0.0400(19) Uani 1 1 d U . . C9B C 0.162(2) 0.5564(5) 0.2694(5) 0.0205(17) Uani 1 1 d U . . C10B C 0.370(2) 0.5530(5) 0.3466(5) 0.0218(17) Uani 1 1 d U . . O1B O 0.2060(16) 0.6208(3) 0.2460(3) 0.0276(15) Uani 1 1 d U . . O2B O 0.5712(16) 0.6112(3) 0.3719(3) 0.0221(14) Uani 1 1 d U . . O3B O 0.3273(17) 0.4968(3) 0.3765(3) 0.0297(14) Uani 1 1 d U . . O4B O -0.0230(18) 0.5037(3) 0.2393(4) 0.0368(17) Uani 1 1 d U . . O5wA O 0.2553(19) 0.1162(4) 0.2554(4) 0.0309(18) Uani 1 1 d U . . H51wA H 0.1795 0.0701 0.2462 0.046 Uiso 1 1 d . . . H52wA H 0.3101 0.1233 0.3041 0.046 Uiso 1 1 d . . . O5wB O 0.9485(16) 0.7460(3) 0.3736(3) 0.0279(15) Uani 1 1 d U . . H51wB H 1.0213 0.7421 0.4191 0.042 Uiso 1 1 d . . . H52wB H 1.0074 0.7927 0.3683 0.042 Uiso 1 1 d . . . O6w O 0.500(4) 0.3947(8) -0.0175(8) 0.050 Uiso 0.50 1 d P . . O7w O 0.177(4) 0.4170(7) 0.0173(7) 0.050 Uiso 0.50 1 d P . . O8w O 0.007(4) 0.4990(7) 0.0826(7) 0.050 Uiso 0.50 1 d P . . O9w O -0.351(4) 0.5224(7) 0.0926(8) 0.050 Uiso 0.50 1 d P . . O10w O 0.664(6) 0.9359(11) 0.4916(11) 0.050 Uiso 0.33 1 d P . . O11w O 0.859(5) 0.9951(13) 0.4929(12) 0.050 Uiso 0.33 1 d P . . O12w O 0.950(6) 1.0648(11) 0.5231(11) 0.050 Uiso 0.33 1 d P . . O13w O 0.614(6) 1.0102(14) 0.4973(15) 0.050 Uiso 0.33 1 d P . . 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 Cu1A 0.0283(7) 0.0226(7) 0.0182(7) 0.0027(4) -0.0067(6) -0.0061(6) Cu1B 0.0346(8) 0.0201(7) 0.0212(7) 0.0069(5) -0.0083(6) -0.0074(6) N1A 0.027(4) 0.024(3) 0.013(3) -0.001(2) -0.005(3) -0.009(3) C2A 0.049(6) 0.016(3) 0.013(3) 0.001(2) -0.010(4) -0.006(4) N3A 0.031(4) 0.017(3) 0.009(2) 0.0008(19) -0.001(3) -0.010(3) C4A 0.013(2) 0.0125(17) 0.0137(17) 0.0018(12) -0.0018(17) -0.0016(16) C5A 0.016(5) 0.011(3) 0.018(2) -0.001(2) -0.003(3) 0.000(3) C6A 0.005(4) 0.015(3) 0.017(2) -0.0043(19) 0.000(3) 0.003(3) N6A 0.035(5) 0.018(3) 0.025(3) 0.001(2) -0.015(3) -0.004(3) N7A 0.039(5) 0.005(3) 0.025(3) 0.001(2) -0.004(3) 0.002(3) C8A 0.027(5) 0.014(4) 0.019(3) 0.006(2) 0.000(4) -0.001(4) N9A 0.027(4) 0.015(3) 0.012(2) 0.0026(18) -0.002(3) -0.006(3) N1B 0.027(4) 0.013(3) 0.027(3) 0.0017(19) -0.005(3) 0.002(3) C2B 0.044(6) 0.014(3) 0.022(3) -0.001(2) -0.006(4) -0.001(4) N3B 0.024(2) 0.0191(18) 0.0192(16) 0.0024(13) -0.0021(16) -0.0035(16) C4B 0.017(2) 0.0165(17) 0.0170(16) 0.0016(12) 0.0006(16) -0.0008(17) C5B 0.013(4) 0.015(2) 0.018(3) 0.0019(19) 0.002(3) 0.002(3) C6B 0.020(5) 0.016(2) 0.018(3) 0.001(2) 0.007(3) 0.000(3) N6B 0.042(5) 0.015(3) 0.030(3) 0.006(3) -0.012(4) -0.005(3) N7B 0.022(4) 0.017(3) 0.022(2) 0.003(2) -0.008(3) 0.001(3) C8B 0.027(5) 0.015(3) 0.013(3) -0.002(2) 0.006(3) -0.001(3) N9B 0.024(5) 0.019(3) 0.024(3) 0.007(2) -0.010(3) -0.006(3) C9A 0.038(5) 0.025(4) 0.010(3) 0.000(3) -0.007(3) -0.012(3) C10A 0.017(5) 0.022(4) 0.018(3) 0.003(3) -0.004(3) -0.002(3) O1A 0.043(4) 0.029(3) 0.017(3) 0.007(2) -0.013(3) -0.015(3) O2A 0.036(4) 0.019(3) 0.024(3) 0.003(3) -0.012(3) -0.010(3) O3A 0.037(4) 0.040(4) 0.029(3) 0.018(3) -0.011(3) -0.013(3) O4A 0.055(5) 0.037(4) 0.025(3) 0.010(3) -0.026(3) -0.023(3) C9B 0.016(5) 0.023(3) 0.022(4) 0.002(3) 0.002(3) -0.003(3) C10B 0.025(5) 0.014(3) 0.026(4) 0.006(3) -0.002(3) 0.000(3) O1B 0.033(4) 0.028(3) 0.021(3) 0.007(2) -0.016(3) -0.011(3) O2B 0.033(4) 0.020(3) 0.013(3) 0.005(2) 0.001(2) -0.006(2) O3B 0.042(4) 0.017(3) 0.032(3) 0.008(2) 0.001(3) -0.002(3) O4B 0.046(4) 0.030(3) 0.032(4) 0.001(3) -0.007(3) -0.016(3) O5wA 0.042(3) 0.025(3) 0.024(3) 0.001(2) -0.009(3) -0.006(3) O5wB 0.042(3) 0.020(3) 0.020(3) 0.002(2) -0.008(2) -0.009(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 Cu1A O2A 1.903(6) . ? Cu1A O5wA 1.916(6) . ? Cu1A O1A 1.929(5) . ? Cu1A N9A 1.971(5) . ? Cu1A O1A 2.848(6) 1_655 ? Cu1B O2B 1.919(5) . ? Cu1B O1B 1.936(6) . ? Cu1B O5wB 1.961(6) . ? Cu1B N9B 1.969(6) . ? Cu1B O5wB 2.712(6) 1_455 ? Cu1B O1B 2.844(7) 1_655 ? N1A C2A 1.342(10) . ? N1A C6A 1.385(9) . ? C2A N3A 1.299(9) . ? C2A H2A 0.93 . ? N3A C4A 1.341(10) . ? C4A N9A 1.378(10) . ? C4A C5A 1.389(10) . ? C5A C6A 1.373(10) . ? C5A N7A 1.396(8) . ? C6A N6A 1.332(9) . ? N6A H61A 0.86 . ? N6A H62A 0.86 . ? N7A C8A 1.350(10) . ? N7A H7A 0.86 . ? C8A N9A 1.346(10) . ? C8A H8A 0.93 . ? N1B C2B 1.324(10) . ? N1B C6B 1.361(10) . ? C2B N3B 1.352(10) . ? C2B H2B 0.93 . ? N3B C4B 1.378(10) . ? C4B N9B 1.337(10) . ? C4B C5B 1.357(11) . ? C5B N7B 1.364(8) . ? C5B C6B 1.466(11) . ? C6B N6B 1.299(10) . ? N6B H61B 0.86 . ? N6B H62B 0.86 . ? N7B C8B 1.328(10) . ? N7B H7B 0.86 . ? C8B N9B 1.346(11) . ? C8B H8B 0.93 . ? C9A O4A 1.235(9) . ? C9A O1A 1.249(9) . ? C9A C10A 1.557(11) . ? C10A O3A 1.211(9) . ? C10A O2A 1.263(9) . ? C9B O4B 1.191(9) . ? C9B O1B 1.290(10) . ? C9B C10B 1.561(11) . ? C10B O3B 1.214(9) . ? C10B O2B 1.271(9) . ? O5wA H51wA 0.86 . ? O5wA H52wA 0.88 . ? O5wB H51wB 0.86 . ? O5wB H52wB 0.88 . ? 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 O2A Cu1A O5wA 174.3(2) . . ? O2A Cu1A O1A 84.0(3) . . ? O5wA Cu1A O1A 90.8(3) . . ? O2A Cu1A N9A 92.0(3) . . ? O5wA Cu1A N9A 93.4(3) . . ? O1A Cu1A N9A 171.9(3) . . ? O2A Cu1A O1A 85.9(3) . 1_655 ? O5wA Cu1A O1A 92.2(3) . 1_655 ? O1A Cu1A O1A 95.4(2) . 1_655 ? N9A Cu1A O1A 91.3(2) . 1_655 ? O2B Cu1B O1B 84.8(3) . . ? O2B Cu1B O5wB 89.5(2) . . ? O1B Cu1B O5wB 173.3(2) . . ? O2B Cu1B N9B 176.0(3) . . ? O1B Cu1B N9B 92.2(3) . . ? O5wB Cu1B N9B 93.3(3) . . ? O2B Cu1B O5wB 90.8(2) . 1_455 ? O1B Cu1B O5wB 84.6(2) . 1_455 ? O5wB Cu1B O5wB 99.0(2) . 1_455 ? N9B Cu1B O5wB 91.6(3) . 1_455 ? O2B Cu1B O1B 85.3(2) . 1_655 ? O1B Cu1B O1B 95.4(2) . 1_655 ? O5wB Cu1B O1B 80.6(2) . 1_655 ? N9B Cu1B O1B 92.3(3) . 1_655 ? O5wB Cu1B O1B 176.1(2) 1_455 1_655 ? C2A N1A C6A 116.1(7) . . ? N3A C2A N1A 132.0(8) . . ? N3A C2A H2A 114.0 . . ? N1A C2A H2A 114.0 . . ? C2A N3A C4A 111.4(7) . . ? N3A C4A N9A 126.7(7) . . ? N3A C4A C5A 123.4(8) . . ? N9A C4A C5A 109.8(7) . . ? C6A C5A C4A 120.9(7) . . ? C6A C5A N7A 134.2(8) . . ? C4A C5A N7A 104.9(8) . . ? N6A C6A C5A 124.6(7) . . ? N6A C6A N1A 119.2(7) . . ? C5A C6A N1A 116.2(7) . . ? C6A N6A H62A 120.0 . . ? C6A N6A H61A 120.0 . . ? H62A N6A H61A 120.0 . . ? C8A N7A C5A 108.5(8) . . ? C8A N7A H7A 125.8 . . ? C5A N7A H7A 125.8 . . ? N9A C8A N7A 110.5(7) . . ? N9A C8A H8A 124.8 . . ? N7A C8A H8A 124.8 . . ? C8A N9A C4A 106.4(5) . . ? C8A N9A Cu1A 125.1(6) . . ? C4A N9A Cu1A 127.9(6) . . ? C2B N1B C6B 118.9(7) . . ? N1B C2B N3B 130.7(8) . . ? N1B C2B H2B 114.6 . . ? N3B C2B H2B 114.6 . . ? C2B N3B C4B 110.7(7) . . ? N9B C4B C5B 110.1(8) . . ? N9B C4B N3B 125.1(8) . . ? C5B C4B N3B 124.8(8) . . ? C4B C5B N7B 106.3(8) . . ? C4B C5B C6B 119.5(8) . . ? N7B C5B C6B 134.2(9) . . ? N6B C6B N1B 122.4(7) . . ? N6B C6B C5B 122.2(7) . . ? N1B C6B C5B 115.4(7) . . ? C6B N6B H61B 120.0 . . ? C6B N6B H62B 120.0 . . ? H61B N6B H62B 120.0 . . ? C8B N7B C5B 107.2(8) . . ? C8B N7B H7B 126.4 . . ? C5B N7B H7B 126.4 . . ? N7B C8B N9B 110.7(8) . . ? N7B C8B H8B 124.7 . . ? N9B C8B H8B 124.7 . . ? C4B N9B C8B 105.7(6) . . ? C4B N9B Cu1B 129.8(6) . . ? C8B N9B Cu1B 124.5(6) . . ? O4A C9A O1A 126.3(8) . . ? O4A C9A C10A 119.0(7) . . ? O1A C9A C10A 114.7(7) . . ? O3A C10A O2A 129.1(8) . . ? O3A C10A C9A 118.3(7) . . ? O2A C10A C9A 112.6(7) . . ? C9A O1A Cu1A 113.2(5) . . ? C10A O2A Cu1A 115.0(5) . . ? O4B C9B O1B 126.8(8) . . ? O4B C9B C10B 120.4(8) . . ? O1B C9B C10B 112.7(7) . . ? O3B C10B O2B 126.5(8) . . ? O3B C10B C9B 118.5(8) . . ? O2B C10B C9B 115.0(7) . . ? C9B O1B Cu1B 113.5(5) . . ? C10B O2B Cu1B 113.6(5) . . ? Cu1A O5wA H51wA 128.8 . . ? Cu1A O5wA H52wA 126.7 . . ? H52wA O5wA H51wA 104.3 . . ? Cu1B O5wB H51wB 130.3 . . ? Cu1B O5wB H52wB 120.7 . . ? H51wB O5wB H52wB 104.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6A H61A O2B 0.86 2.04 2.888(9) 169 2_766 N6A H62A O3B 0.86 2.00 2.821(9) 161 1_655 N7A H7A O3B 0.86 2.12 2.877(9) 147 1_655 N6B H61B O1A 0.86 2.07 2.926(9) 178 1_665 N6B H62B O4A 0.86 2.00 2.845(9) 169 2_565 N7B H7B O4A 0.86 2.07 2.841(9) 150 2_565 O5wA H51wA N1B 0.86 1.89 2.720(9) 163 1_445 O5wA H52wA N3A 0.88 1.94 2.636(9) 134 . O5wB H51wB N1A 0.86 1.89 2.739(9) 171 2_766 O5wB H52wB N3B 0.88 1.96 2.695(9) 140 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.725 _refine_diff_density_min -1.350 _refine_diff_density_rms 0.127 #===END _chemical_name_common 'adenine(aqua)oxalatocopper(ii)-water (1/1.66)'