Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Pilar Amo-Ochoa' ; Departamento de Tecnologia Industrial. Universidad Alfonso X 'El Sabio', E-28691 Villanueva de la Canada, Madrid, Spain ; 'Pablo J. Sanz Miguel' ; Departamento de Quimica Inorganica. Universidad Autonoma de Madrid, E-28049 Madrid, Spain ; 'Oscar Castillo' ; Departamento de Quimica Inorganica. Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; 'Felix Zamora' ; Departamento de Quimica Inorganica. Universidad Autonoma de Madrid, E-28049 Madrid, Spain ; _publ_contact_author ; Felix Zamora, Departamento de Quimica Inorganica. Universidad Autonoma de Madrid, E-28049 Madrid, Spain ; _publ_contact_author_email felix.zamora@uam.es _publ_contact_author_fax '34 91 4974833' _publ_contact_author_phone '34 91 4973962' _publ_section_title ; An unusual triple parallel interpenetrated 2D Cu-polymer, with a 3D triple interpenetration via H-bonding ; _publ_contact_author_name 'Felix Zamora, Departamento de Quimica Inorganica.' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 630735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(\m-cyanido-\kC,N)(\m-isonicotinato-\kN,O) (\m-isonicotinic acid-\kN,O)dicopper(I) ; _chemical_formula_moiety 'C13 H9 Cu2 N3 O4' _chemical_formula_sum 'C13 H9 Cu2 N3 O4' _chemical_formula_iupac 'C13 H9 Cu2 N3 O4' _chemical_formula_weight 398.32 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pc _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 10.864(2) _cell_length_b 5.116(1) _cell_length_c 12.282(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.53(1) _cell_angle_gamma 90.00 _cell_volume 660.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3232 _cell_measurement_theta_min 3.43 _cell_measurement_theta_max 30.30 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 3.240 _exptl_absorpt_correction_type analytical _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 0.307 _exptl_absorpt_correction_T_max 0.623 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 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 6073 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 30.30 _reflns_number_total 3232 _reflns_number_gt 2367 _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^)+(0.0466P)^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 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 0.40(4) _refine_ls_number_reflns 3232 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.962 _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 0.49893(4) 0.4292(2) 0.62014(4) 0.0318(3) Uani 1 1 d . . . Cu2 Cu 0.19115(4) 1.0696(2) 0.42557(4) 0.0311(3) Uani 1 1 d . . . N1 N 0.3805(8) 0.6775(17) 0.5468(7) 0.0320(12) Uani 1 1 d U . . C1 C 0.3076(9) 0.8281(19) 0.5018(8) 0.0257(12) Uani 1 1 d U . . N11 N 0.5592(7) 0.1488(15) 0.7230(6) 0.0228(12) Uani 1 1 d U . . C12 C 0.5094(8) 0.0984(16) 0.8176(7) 0.0272(13) Uani 1 1 d U . . H12 H 0.4430 0.2031 0.8273 0.033 Uiso 1 1 calc R . . C13 C 0.5505(8) -0.0846(16) 0.8915(8) 0.0248(13) Uani 1 1 d U . . H13 H 0.5115 -0.1109 0.9498 0.030 Uiso 1 1 calc R . . C14 C 0.6532(8) -0.2419(16) 0.8833(8) 0.0186(12) Uani 1 1 d U . . C15 C 0.7061(7) -0.1905(15) 0.7890(7) 0.0230(12) Uani 1 1 d U . . H15 H 0.7741 -0.2879 0.7778 0.028 Uiso 1 1 calc R . . C16 C 0.6566(9) -0.006(2) 0.7207(7) 0.0254(13) Uani 1 1 d U . . H16 H 0.6942 0.0224 0.6616 0.031 Uiso 1 1 calc R . . C17 C 0.7092(10) -0.4454(16) 0.9714(7) 0.0195(14) Uani 1 1 d U . . O171 O 0.6645(7) -0.4728(14) 1.0533(6) 0.0298(14) Uani 1 1 d U . . O172 O 0.8027(7) -0.5785(11) 0.9506(6) 0.0299(16) Uani 1 1 d U . . N21 N 0.1288(7) 1.3475(15) 0.3174(6) 0.0232(12) Uani 1 1 d U . . C22 C 0.1785(8) 1.3892(15) 0.2384(7) 0.0291(14) Uani 1 1 d U . . H22 H 0.2488 1.2905 0.2336 0.035 Uiso 1 1 calc R . . C23 C 0.1308(9) 1.5859(17) 0.1533(8) 0.0285(14) Uani 1 1 d U . . H23 H 0.1676 1.6060 0.0931 0.034 Uiso 1 1 calc R . . C24 C 0.0319(8) 1.7413(16) 0.1620(8) 0.0199(12) Uani 1 1 d U . . C25 C -0.0134(7) 1.7107(14) 0.2510(7) 0.0239(13) Uani 1 1 d U . . H25 H -0.0767 1.8228 0.2617 0.029 Uiso 1 1 calc R . . C26 C 0.0338(8) 1.5033(18) 0.3337(7) 0.0230(13) Uani 1 1 d U . . H26 H -0.0004 1.4794 0.3953 0.028 Uiso 1 1 calc R . . C27 C -0.0213(10) 1.9462(16) 0.0734(8) 0.0193(14) Uani 1 1 d U . . O271 O 0.0184(6) 1.9711(13) -0.0094(6) 0.0281(13) Uani 1 1 d U . . O272 O -0.1096(7) 2.0798(11) 0.0917(6) 0.0320(17) Uani 1 1 d U . . H172 H 0.824(5) -0.721(12) 0.995(4) 0.059(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0345(7) 0.0266(7) 0.0319(7) 0.0096(6) 0.0041(6) 0.0119(6) Cu2 0.0343(7) 0.0262(7) 0.0312(7) 0.0099(6) 0.0050(6) 0.0141(6) N1 0.030(2) 0.032(2) 0.036(2) 0.015(2) 0.012(2) 0.002(2) C1 0.021(2) 0.027(2) 0.032(2) 0.012(2) 0.012(2) 0.010(2) N11 0.026(3) 0.025(2) 0.020(2) 0.001(2) 0.011(2) 0.000(2) C12 0.029(2) 0.035(3) 0.025(2) 0.001(2) 0.0211(19) 0.007(2) C13 0.025(3) 0.029(3) 0.027(3) 0.005(2) 0.020(2) 0.009(2) C14 0.022(2) 0.017(2) 0.018(2) -0.0005(19) 0.007(2) 0.001(2) C15 0.026(2) 0.027(2) 0.023(2) 0.0023(19) 0.018(2) 0.005(2) C16 0.028(3) 0.033(3) 0.021(2) 0.006(2) 0.016(2) -0.001(2) C17 0.023(3) 0.019(3) 0.018(3) 0.000(2) 0.007(2) 0.001(2) O171 0.035(3) 0.036(3) 0.023(3) 0.011(2) 0.017(2) 0.006(2) O172 0.031(2) 0.032(2) 0.030(2) 0.0087(15) 0.0134(17) 0.0106(15) N21 0.024(2) 0.019(2) 0.026(3) 0.011(2) 0.004(2) 0.012(2) C22 0.032(3) 0.024(2) 0.032(3) 0.018(2) 0.010(2) 0.022(2) C23 0.033(3) 0.030(3) 0.026(3) 0.014(2) 0.013(2) 0.013(2) C24 0.021(2) 0.017(2) 0.022(2) 0.006(2) 0.005(2) 0.005(2) C25 0.025(2) 0.019(2) 0.026(3) 0.0110(19) 0.004(2) 0.0130(19) C26 0.026(2) 0.021(2) 0.022(2) 0.0082(19) 0.006(2) 0.013(2) C27 0.020(3) 0.016(3) 0.022(3) 0.006(2) 0.005(2) 0.001(2) O271 0.031(3) 0.028(3) 0.029(3) 0.009(2) 0.015(2) 0.010(2) O272 0.036(2) 0.032(2) 0.035(3) 0.0248(18) 0.023(2) 0.0254(18) _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 N1 1.871(9) . ? Cu1 N11 1.915(7) . ? Cu1 O171 2.168(6) 2_554 ? Cu2 C1 1.846(9) . ? Cu2 N21 1.948(6) . ? Cu2 O271 2.226(6) 2_585 ? N1 C1 1.143(13) . ? N11 C16 1.328(11) . ? N11 C12 1.423(9) . ? C12 C13 1.302(11) . ? C12 H12 0.9300 . ? C13 C14 1.399(11) . ? C13 H13 0.9300 . ? C14 C15 1.440(10) . ? C14 C17 1.515(11) . ? C15 C16 1.287(11) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O171 1.229(9) . ? C17 O172 1.300(10) . ? O171 Cu1 2.168(6) 2 ? O172 H172 0.91(6) . ? N21 C22 1.243(9) . ? N21 C26 1.358(10) . ? C22 C23 1.450(10) . ? C22 H22 0.9300 . ? C23 C24 1.362(11) . ? C23 H23 0.9300 . ? C24 C25 1.316(11) . ? C24 C27 1.517(11) . ? C25 C26 1.470(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 O271 1.207(10) . ? C27 O272 1.243(10) . ? O271 Cu2 2.226(6) 2_584 ? 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 Cu1 N11 155.0(3) . . ? N1 Cu1 O171 106.5(3) . 2_554 ? N11 Cu1 O171 98.5(3) . 2_554 ? C1 Cu2 N21 155.7(3) . . ? C1 Cu2 O271 106.7(3) . 2_585 ? N21 Cu2 O271 97.6(3) . 2_585 ? C1 N1 Cu1 179.6(9) . . ? N1 C1 Cu2 178.5(9) . . ? C16 N11 C12 112.2(7) . . ? C16 N11 Cu1 125.1(5) . . ? C12 N11 Cu1 122.5(6) . . ? C13 C12 N11 124.4(8) . . ? C13 C12 H12 117.8 . . ? N11 C12 H12 117.8 . . ? C12 C13 C14 120.3(8) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 116.0(8) . . ? C13 C14 C17 121.9(8) . . ? C15 C14 C17 122.0(7) . . ? C16 C15 C14 118.2(7) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C15 C16 N11 128.9(7) . . ? C15 C16 H16 115.5 . . ? N11 C16 H16 115.5 . . ? O171 C17 O172 126.1(9) . . ? O171 C17 C14 119.5(8) . . ? O172 C17 C14 114.4(7) . . ? C17 O171 Cu1 146.5(7) . 2 ? C17 O172 H172 113(4) . . ? C22 N21 C26 120.7(7) . . ? C22 N21 Cu2 120.9(5) . . ? C26 N21 Cu2 118.4(5) . . ? N21 C22 C23 122.4(8) . . ? N21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C24 C23 C22 119.7(8) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 117.5(8) . . ? C25 C24 C27 121.6(7) . . ? C23 C24 C27 120.9(8) . . ? C24 C25 C26 121.5(7) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? N21 C26 C25 117.9(7) . . ? N21 C26 H26 121.1 . . ? C25 C26 H26 121.1 . . ? O271 C27 O272 123.3(8) . . ? O271 C27 C24 121.7(8) . . ? O272 C27 C24 115.0(7) . . ? C27 O271 Cu2 143.5(7) . 2_584 ? 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 O172 H172 O272 0.91(6) 1.59(5) 2.478(9) 164(6) 1_626 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 30.30 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.475 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.150 _chemical_name_common ; catena-(mu-cyanido-kappaC,N)(mu-isonicotinato-kappaN,O) (mu- isonicotinic acid-kappaN,O)dicopper(i) ;