# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Jintha Thomas' ; Departamento de Quimica Inorganica. Facultad de Ciencia y Tecnologia Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; 'Garikoitz Beobide' ; Departamento de Quimica Inorganica. Facultad de Ciencia y Tecnologia Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; 'Oscar Castillo' ; Departamento de Quimica Inorganica. Facultad de Ciencia y Tecnologia Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; 'Javier Cepeda' ; Departamento de Quimica Inorganica. Facultad de Ciencia y Tecnologia Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; 'Antonio Luque' ; Departamento de Quimica Inorganica. Facultad de Ciencia y Tecnologia Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; 'Sonia Perez-Yanez' ; Departamento de Quimica Inorganica. Facultad de Ciencia y Tecnologia Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; ; A.T.Aguayo ; ; Departamento de Ingenieria Quimica. Facultad de Ciencia y Tecnologia Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; 'Pascual Roman' ; Departamento de Quimica Inorganica. Facultad de Ciencia y Tecnologia Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; _publ_contact_author ; Oscar Castillo. Departamento de Quimica Inorganica. Facultad de Ciencia y Tecnologia Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; _publ_contact_author_email oscar.castillo@ehu.es _publ_contact_author_fax '+34-946 013 500' _publ_contact_author_phone '+34-946 015 991' _publ_section_title ; Porous supramolecular compound based on paddle-wheel shaped copper(II)-adenine dinuclear entities ; _publ_contact_author_name 'Oscar Castillo. Departamento de Quimica Inorganica.' data_compound1_293K _database_code_depnum_ccdc_archive 'CCDC 785522' _audit_creation_method SHELXL _chemical_name_systematic ; [Tetrakis(mu-adenine-kN3:kN9)bis(chlorido)dicopper(II)]chloride- methanol (1/2)] ; _chemical_formula_moiety 'C20 H20 Cu2 Cl2 N20, 2 (Cl), 2(C1 H4 O)' _chemical_formula_sum 'C22 H28 Cl4 Cu2 N20 O2' _chemical_formula_iupac '[Cu2(C5H5N5)2Cl]Cl2, 2(C1 H4 O)' _chemical_formula_weight 873.49 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 m' _symmetry_space_group_name_Hall ; -R 3 2" ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'y+1/3, x+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' _cell_length_a 26.820(1) _cell_length_b 26.820(1) _cell_length_c 15.528(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9673.1(8) _cell_formula_units_Z 9 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20165 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.00 _cell_measurement_wavelength 0.71073 _cell_special_details ; ; _exptl_crystal_description conical _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3978 _exptl_absorpt_coefficient_mu 1.284 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'X-RED; Stoe & Cie, 2001' _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 0.904 _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IPDS II' _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 20165 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2029 _reflns_number_gt 1342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe & Cie, 2006)' _computing_cell_refinement IPDS _computing_data_reduction IPDS _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. Positions for some solvate atoms were so severely disordered that no discrete model surfaced in difference Fourier maps. Atoms in the region were removed and the solvent region was refined as a diffuse contribution without specific atom positions using the Platon module SQUEEZE (A.L. Spek (2003) J. Appl. Cryst. 36, 7). An improvement was observed in all refinement parameters and indices. The "squeeze" data are reported here. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.010 1174 181 ' ' 2 0.333 0.667 0.175 1190 182 ' ' 3 0.667 0.333 0.841 1190 182 ' ' _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^)+(0.1794P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 2029 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2601 _refine_ls_wR_factor_gt 0.2501 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.28852(6) 0.14426(3) 0.09429(6) 0.0510(5) Uani 1 2 d S . . Cl1 Cl 0.20825(13) 0.10412(7) -0.00970(16) 0.0695(8) Uani 1 2 d S . . Cl2 Cl 0.28664(16) 0.14332(8) -0.2419(2) 0.0862(12) Uani 1 2 d S . . N1 N 0.3053(3) 0.0455(3) 0.4077(3) 0.0684(19) Uani 1 1 d . . . C2 C 0.3358(3) 0.0965(3) 0.3711(4) 0.061(2) Uani 1 1 d . . . H2 H 0.3666 0.1244 0.4028 0.073 Uiso 1 1 calc R . . N3 N 0.3272(3) 0.1123(2) 0.2935(3) 0.0582(16) Uani 1 1 d . . . C4 C 0.2799(4) 0.0691(3) 0.2510(4) 0.0547(19) Uani 1 1 d . . . C5 C 0.2479(4) 0.0158(3) 0.2822(4) 0.060(2) Uani 1 1 d . . . C6 C 0.2609(4) 0.0022(3) 0.3658(4) 0.063(2) Uani 1 1 d . . . N6 N 0.2311(4) -0.0483(3) 0.4029(4) 0.083(2) Uani 1 1 d . . . H6A H 0.2400 -0.0537 0.4540 0.099 Uiso 1 1 calc R . . H6B H 0.2027 -0.0761 0.3762 0.099 Uiso 1 1 calc R . . N7 N 0.2067(3) -0.0135(3) 0.2219(4) 0.0696(19) Uani 1 1 d . . . H7 H 0.1800 -0.0490 0.2242 0.084 Uiso 1 1 calc R . . C8 C 0.2155(4) 0.0237(3) 0.1582(4) 0.067(2) Uani 1 1 d . . . H8 H 0.1931 0.0139 0.1086 0.081 Uiso 1 1 calc R . . N9 N 0.2583(3) 0.0745(2) 0.1726(3) 0.0525(15) 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 Cu1 0.0944(11) 0.0520(6) 0.0208(6) 0.0052(3) 0.0104(5) 0.0472(5) Cl1 0.093(2) 0.0761(13) 0.0451(13) -0.0007(7) -0.0013(13) 0.0465(11) Cl2 0.137(3) 0.0618(12) 0.085(2) 0.0238(10) 0.0476(19) 0.0686(15) N1 0.114(6) 0.064(4) 0.033(3) 0.016(3) 0.007(3) 0.049(4) C2 0.097(6) 0.057(4) 0.033(3) 0.007(3) 0.007(3) 0.041(4) N3 0.103(5) 0.055(4) 0.027(3) 0.012(2) 0.015(3) 0.047(4) C4 0.101(6) 0.052(4) 0.028(3) 0.011(3) 0.023(4) 0.051(4) C5 0.103(6) 0.057(4) 0.030(3) 0.007(3) 0.012(4) 0.048(4) C6 0.101(6) 0.064(5) 0.034(3) 0.016(3) 0.024(4) 0.048(5) N6 0.130(6) 0.058(4) 0.037(3) 0.021(3) 0.003(4) 0.030(4) N7 0.104(5) 0.054(4) 0.045(3) 0.012(3) 0.009(3) 0.035(4) C8 0.108(7) 0.054(5) 0.036(3) 0.008(3) 0.008(4) 0.038(5) N9 0.085(4) 0.046(3) 0.032(3) 0.007(2) 0.011(3) 0.037(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 Cu1 N3 2.002(6) 11 ? Cu1 N3 2.002(6) 25 ? Cu1 N9 2.031(5) 23 ? Cu1 N9 2.031(5) . ? Cu1 Cl1 2.466(3) . ? N1 C2 1.319(9) . ? N1 C6 1.344(10) . ? C2 N3 1.335(9) . ? C2 H2 0.9300 . ? N3 C4 1.385(9) . ? N3 Cu1 2.002(6) 25 ? C4 C5 1.337(10) . ? C4 N9 1.385(8) . ? C5 N7 1.360(10) . ? C5 C6 1.438(9) . ? C6 N6 1.313(9) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? N7 C8 1.339(9) . ? N7 H7 0.8600 . ? C8 N9 1.287(10) . ? C8 H8 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N3 86.9(3) 11 25 ? N3 Cu1 N9 162.5(3) 11 23 ? N3 Cu1 N9 87.7(2) 25 23 ? N3 Cu1 N9 87.7(2) 11 . ? N3 Cu1 N9 162.5(3) 25 . ? N9 Cu1 N9 92.5(3) 23 . ? N3 Cu1 Cl1 99.79(19) 11 . ? N3 Cu1 Cl1 99.79(19) 25 . ? N9 Cu1 Cl1 97.52(18) 23 . ? N9 Cu1 Cl1 97.52(18) . . ? C2 N1 C6 120.6(6) . . ? N1 C2 N3 127.0(7) . . ? N1 C2 H2 116.5 . . ? N3 C2 H2 116.5 . . ? C2 N3 C4 113.3(6) . . ? C2 N3 Cu1 124.8(6) . 25 ? C4 N3 Cu1 121.8(4) . 25 ? C5 C4 N9 110.6(7) . . ? C5 C4 N3 123.4(6) . . ? N9 C4 N3 126.0(6) . . ? C4 C5 N7 105.6(6) . . ? C4 C5 C6 119.5(8) . . ? N7 C5 C6 134.8(7) . . ? N6 C6 N1 119.9(6) . . ? N6 C6 C5 124.0(8) . . ? N1 C6 C5 116.0(7) . . ? C6 N6 H6A 120.0 . . ? C6 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C8 N7 C5 106.7(7) . . ? C8 N7 H7 126.6 . . ? C5 N7 H7 126.6 . . ? N9 C8 N7 113.0(7) . . ? N9 C8 H8 123.5 . . ? N7 C8 H8 123.5 . . ? C8 N9 C4 104.0(6) . . ? C8 N9 Cu1 127.2(5) . . ? C4 N9 Cu1 128.8(5) . . ? 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 N6 H6A N1 0.86 2.20 3.032(8) 163 4_556 N6 H6B Cl2 0.86 2.69 3.505(8) 158 20 N7 H7 Cl2 0.86 2.23 3.032(7) 156 20 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.995 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.126 _chemical_name_common ;(Tetrakis(mu-adenine- kN3:kN9)bis(chlorido)dicopper(ii))chloride-methanol (1/2)) ; #===END data_compound1_100K _database_code_depnum_ccdc_archive 'CCDC 785523' _audit_creation_method SHELXL _chemical_name_systematic ; [Tetrakis(mu-adenine-kN3:kN9)bis(chlorido)dicopper(II)]chloride- methanol (1/2)] ; _chemical_formula_moiety 'C20 H20 Cu2 Cl2 N20, 2 (Cl), 2(C1 H4 O)' _chemical_formula_sum 'C22 H28 Cl4 Cu2 N20 O2' _chemical_formula_iupac '[Cu2(C5H5N5)2Cl]Cl2, 2(C1 H4 O)' _chemical_formula_weight 873.49 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 m' _symmetry_space_group_name_Hall ; -R 3 2" ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'y+1/3, x+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' _cell_length_a 26.903(2) _cell_length_b 26.903(2) _cell_length_c 15.430(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9671.6(12) _cell_formula_units_Z 9 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11165 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.97 _cell_measurement_wavelength 0.71073 _cell_special_details ; ; _exptl_crystal_description conical _exptl_crystal_colour violet _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3978 _exptl_absorpt_coefficient_mu 1.284 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'X-RED; Stoe & Cie, 2001' _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 0.928 _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IPDS II' _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 11165 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2035 _reflns_number_gt 1629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe & Cie, 2006)' _computing_cell_refinement IPDS _computing_data_reduction IPDS _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. Positions for some solvate atoms were so severely disordered that no discrete model surfaced in difference Fourier maps. Atoms in the region were removed and the solvent region was refined as a diffuse contribution without specific atom positions using the Platon module SQUEEZE (A.L. Spek (2003) J. Appl. Cryst. 36, 7). An improvement was observed in all refinement parameters and indices. The "squeeze" data are reported here. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.012 1160 348 ' ' 2 0.333 0.667 0.175 1176 351 ' ' 3 0.667 0.333 0.842 1176 351 ' ' _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^)+(0.0548P)^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_method none _refine_ls_number_reflns 2035 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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 0.288702(19) 0.144351(9) 0.09322(3) 0.02265(15) Uani 1 2 d S . . Cl1 Cl 0.20992(4) 0.10496(2) -0.01149(6) 0.0309(2) Uani 1 2 d S . . Cl2 Cl 0.28739(4) 0.14369(2) -0.24239(6) 0.0319(2) Uani 1 2 d S . . N1 N 0.30437(11) 0.04413(10) 0.40824(15) 0.0316(5) Uani 1 1 d . . . C2 C 0.33464(12) 0.09544(12) 0.37084(18) 0.0300(6) Uani 1 1 d . . . H2 H 0.3653 0.1232 0.4027 0.036 Uiso 1 1 calc R . . N3 N 0.32612(9) 0.11166(9) 0.29291(14) 0.0256(5) Uani 1 1 d . . . C4 C 0.27993(12) 0.06993(11) 0.25027(17) 0.0257(6) Uani 1 1 d . . . C5 C 0.24696(12) 0.01464(12) 0.28165(18) 0.0282(6) Uani 1 1 d . . . C6 C 0.25931(13) 0.00112(12) 0.36422(18) 0.0300(6) Uani 1 1 d . . . N6 N 0.23019(12) -0.04979(10) 0.40237(16) 0.0373(6) Uani 1 1 d . . . H6A H 0.2399 -0.0549 0.4533 0.045 Uiso 1 1 calc R . . H6B H 0.2016 -0.0777 0.3762 0.045 Uiso 1 1 calc R . . N7 N 0.20494(10) -0.01434(10) 0.22029(15) 0.0305(5) Uani 1 1 d . . . H7 H 0.1782 -0.0497 0.2224 0.037 Uiso 1 1 calc R . . C8 C 0.21376(12) 0.02330(12) 0.15633(18) 0.0301(6) Uani 1 1 d . . . H8 H 0.1911 0.0142 0.1068 0.036 Uiso 1 1 calc R . . N9 N 0.25851(9) 0.07493(9) 0.17201(14) 0.0260(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0259(3) 0.0226(2) 0.0205(2) 0.00114(9) 0.00227(18) 0.01296(13) Cl1 0.0304(5) 0.0331(4) 0.0282(5) -0.0018(2) -0.0035(4) 0.0152(3) Cl2 0.0385(6) 0.0270(3) 0.0339(5) 0.0042(2) 0.0084(4) 0.0193(3) N1 0.0390(14) 0.0267(12) 0.0253(12) 0.0036(10) 0.0015(10) 0.0136(11) C2 0.0334(15) 0.0278(14) 0.0265(14) 0.0015(12) 0.0021(12) 0.0135(12) N3 0.0296(12) 0.0262(12) 0.0219(11) 0.0009(10) 0.0011(9) 0.0147(10) C4 0.0298(14) 0.0269(14) 0.0231(13) 0.0035(11) 0.0059(11) 0.0163(12) C5 0.0324(15) 0.0238(14) 0.0256(14) 0.0029(12) 0.0018(12) 0.0119(12) C6 0.0383(16) 0.0269(14) 0.0240(14) 0.0030(11) 0.0041(12) 0.0157(13) N6 0.0477(15) 0.0261(13) 0.0267(13) 0.0052(10) -0.0011(11) 0.0099(12) N7 0.0324(13) 0.0229(11) 0.0282(13) 0.0023(10) 0.0002(10) 0.0078(10) C8 0.0326(15) 0.0297(15) 0.0272(15) 0.0024(12) 0.0001(12) 0.0150(13) N9 0.0285(12) 0.0246(11) 0.0238(12) 0.0009(9) 0.0010(10) 0.0125(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 Cu1 N3 2.009(2) 11 ? Cu1 N3 2.009(2) 25 ? Cu1 N9 2.027(2) 23 ? Cu1 N9 2.027(2) . ? Cu1 Cl1 2.4454(10) . ? N1 C2 1.333(4) . ? N1 C6 1.367(4) . ? C2 N3 1.337(4) . ? C2 H2 0.9300 . ? N3 C4 1.357(4) . ? N3 Cu1 2.009(2) 25 ? C4 N9 1.373(3) . ? C4 C5 1.384(4) . ? C5 N7 1.379(4) . ? C5 C6 1.409(4) . ? C6 N6 1.328(4) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? N7 C8 1.347(4) . ? N7 H7 0.8600 . ? C8 N9 1.329(4) . ? C8 H8 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N3 87.01(13) 11 25 ? N3 Cu1 N9 161.49(9) 11 23 ? N3 Cu1 N9 87.45(9) 25 23 ? N3 Cu1 N9 87.46(9) 11 . ? N3 Cu1 N9 161.49(9) 25 . ? N9 Cu1 N9 92.27(12) 23 . ? N3 Cu1 Cl1 100.57(7) 11 . ? N3 Cu1 Cl1 100.57(7) 25 . ? N9 Cu1 Cl1 97.80(7) 23 . ? N9 Cu1 Cl1 97.80(7) . . ? C2 N1 C6 119.1(2) . . ? N1 C2 N3 127.7(3) . . ? N1 C2 H2 116.2 . . ? N3 C2 H2 116.2 . . ? C2 N3 C4 113.7(2) . . ? C2 N3 Cu1 123.98(19) . 25 ? C4 N3 Cu1 122.31(18) . 25 ? N3 C4 N9 126.9(2) . . ? N3 C4 C5 123.3(2) . . ? N9 C4 C5 109.8(2) . . ? N7 C5 C4 105.7(2) . . ? N7 C5 C6 135.0(3) . . ? C4 C5 C6 119.1(3) . . ? N6 C6 N1 118.0(3) . . ? N6 C6 C5 125.0(3) . . ? N1 C6 C5 117.0(2) . . ? C6 N6 H6A 120.0 . . ? C6 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C8 N7 C5 107.0(2) . . ? C8 N7 H7 126.5 . . ? C5 N7 H7 126.5 . . ? N9 C8 N7 112.3(2) . . ? N9 C8 H8 123.9 . . ? N7 C8 H8 123.9 . . ? C8 N9 C4 105.2(2) . . ? C8 N9 Cu1 126.18(18) . . ? C4 N9 Cu1 128.55(18) . . ? 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 N6 H6A N1 0.86 2.19 3.015(3) 161 4_556 N6 H6B Cl2 0.86 2.66 3.466(3) 156 20 N7 H7 Cl2 0.86 2.24 3.034(2) 154 20 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.379 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.070 _chemical_name_common ;(Tetrakis(mu-adenine- kN3:kN9)bis(chlorido)dicopper(ii))chloride-methanol (1/2)) ;