# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_p-1 _database_code_CSD 173463 _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Liu, Qingliang' 'Du, C.' 'Jiang, H.' 'Xie, Y.' 'Xu, X.' 'Zhu, Y.' _publ_contact_author_name 'Prof Qingliang Liu' _publ_contact_author_address ; Department of Chemistry University of Science and Technology of China Hefei 230026 CHINA ; _publ_contact_author_email 'YSHXIE@USTC.EDU.CN' _publ_section_title ; An unusual alternating ferro- and antiferromagnetic 1D hydrogen-bonded m2-1,3-azide-bridged copper(II) complex: a dominant ferromagnetic coupling ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 Cu N8' _chemical_formula_weight 417.84 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1175(16) _cell_length_b 9.4246(19) _cell_length_c 12.362(3) _cell_angle_alpha 93.23(3) _cell_angle_beta 109.13(3) _cell_angle_gamma 97.09(3) _cell_volume 881.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 414 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Rigaku Raxis-IV' _diffrn_measurement_method 'Oscillation frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3169 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.57 _reflns_number_total 3169 _reflns_number_gt 2404 _reflns_threshold_expression >2sigma(I) _computing_data_collection Raxis _computing_cell_refinement Raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0742P)^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 SHELXL _refine_ls_extinction_coef 0.000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3169 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.613 _refine_ls_shift/su_mean 0.003 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.66882(7) 0.54608(6) 0.93418(5) 0.0407(2) Uani 1 1 d . . . N1 N 0.5255(5) 0.6344(4) 0.7928(3) 0.0427(9) Uani 1 1 d . . . N2 N 0.6756(5) 0.7383(4) 1.0200(3) 0.0428(9) Uani 1 1 d . . . N3 N 0.5792(5) 0.3528(4) 0.8514(4) 0.0540(11) Uani 1 1 d . . . N4 N 0.6562(5) 0.2519(5) 0.8646(4) 0.0495(10) Uani 1 1 d . . . N5 N 0.7222(7) 0.1504(5) 0.8741(5) 0.0757(15) Uani 1 1 d . . . N6 N 0.7914(5) 0.4726(4) 1.0884(4) 0.0518(11) Uani 1 1 d . . . N7 N 0.9319(5) 0.4364(4) 1.0958(3) 0.0465(9) Uani 1 1 d . . . N8 N 1.0678(5) 0.4003(5) 1.1093(4) 0.0593(12) Uani 1 1 d . . . C1 C 0.5536(7) 0.5878(6) 0.6837(4) 0.0566(13) Uani 1 1 d . . . H1A H 0.6747 0.6229 0.6912 0.068 Uiso 1 1 calc R . . H1B H 0.5390 0.4837 0.6747 0.068 Uiso 1 1 calc R . . C2 C 0.4364(7) 0.6357(6) 0.5774(4) 0.0529(13) Uani 1 1 d . . . C3 C 0.2691(8) 0.5580(6) 0.5194(5) 0.0656(15) Uani 1 1 d . . . H3A H 0.2305 0.4769 0.5491 0.079 Uiso 1 1 calc R . . C4 C 0.1603(8) 0.5996(9) 0.4188(6) 0.081(2) Uani 1 1 d . . . H4A H 0.0493 0.5471 0.3808 0.097 Uiso 1 1 calc R . . C5 C 0.2177(10) 0.7195(10) 0.3752(6) 0.087(2) Uani 1 1 d . . . H5A H 0.1453 0.7478 0.3071 0.104 Uiso 1 1 calc R . . C6 C 0.3815(11) 0.7979(8) 0.4314(6) 0.084(2) Uani 1 1 d . . . H6A H 0.4196 0.8790 0.4015 0.101 Uiso 1 1 calc R . . C7 C 0.4879(8) 0.7561(7) 0.5311(5) 0.0639(15) Uani 1 1 d . . . H7A H 0.5981 0.8103 0.5689 0.077 Uiso 1 1 calc R . . C8 C 0.8502(6) 0.8191(6) 1.0810(5) 0.0527(13) Uani 1 1 d . . . H8A H 0.8907 0.8707 1.0264 0.063 Uiso 1 1 calc R . . H8B H 0.9311 0.7518 1.1109 0.063 Uiso 1 1 calc R . . C9 C 0.8581(6) 0.9261(5) 1.1798(4) 0.0461(11) Uani 1 1 d . . . C10 C 0.8103(6) 0.8808(6) 1.2704(5) 0.0564(13) Uani 1 1 d . . . H10A H 0.7707 0.7839 1.2703 0.068 Uiso 1 1 calc R . . C11 C 0.8204(7) 0.9770(8) 1.3616(5) 0.0703(17) Uani 1 1 d . . . H11A H 0.7833 0.9453 1.4209 0.084 Uiso 1 1 calc R . . C12 C 0.8848(8) 1.1190(7) 1.3648(5) 0.0656(15) Uani 1 1 d . . . H12A H 0.8967 1.1836 1.4276 0.079 Uiso 1 1 calc R . . C13 C 0.9310(8) 1.1638(6) 1.2750(5) 0.0699(16) Uani 1 1 d . . . H13A H 0.9725 1.2604 1.2755 0.084 Uiso 1 1 calc R . . C14 C 0.9172(7) 1.0683(6) 1.1830(5) 0.0575(13) Uani 1 1 d . . . H14A H 0.9488 1.1014 1.1220 0.069 Uiso 1 1 calc R . . C15 C 0.5620(6) 0.7926(5) 0.8215(4) 0.0488(12) Uani 1 1 d . . . H15A H 0.4745 0.8379 0.7664 0.059 Uiso 1 1 calc R . . H15B H 0.6775 0.8299 0.8192 0.059 Uiso 1 1 calc R . . C16 C 0.5552(6) 0.8238(5) 0.9401(4) 0.0472(11) Uani 1 1 d . . . H16A H 0.5920 0.9256 0.9653 0.057 Uiso 1 1 calc R . . H16B H 0.4356 0.7980 0.9398 0.057 Uiso 1 1 calc R . . H2B H 0.618(5) 0.710(4) 1.065(4) 0.032(11) Uiso 1 1 d . . . H1B' H 0.423(6) 0.608(5) 0.786(4) 0.051(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 0.0486(3) 0.0381(3) 0.0387(3) 0.0039(2) 0.0169(2) 0.0132(2) N1 0.042(2) 0.048(2) 0.038(2) 0.0009(18) 0.0117(17) 0.0152(17) N2 0.051(2) 0.041(2) 0.038(2) 0.0000(18) 0.0174(18) 0.0078(17) N3 0.062(3) 0.043(2) 0.059(3) 0.002(2) 0.024(2) 0.010(2) N4 0.063(2) 0.046(3) 0.048(3) 0.005(2) 0.031(2) 0.008(2) N5 0.090(3) 0.051(3) 0.100(4) 0.010(3) 0.043(3) 0.027(3) N6 0.048(2) 0.055(3) 0.061(3) 0.016(2) 0.0230(19) 0.0193(19) N7 0.058(3) 0.041(2) 0.041(2) 0.0096(18) 0.0170(18) 0.0063(18) N8 0.055(2) 0.074(3) 0.060(3) 0.025(2) 0.025(2) 0.026(2) C1 0.069(3) 0.066(3) 0.041(3) 0.001(3) 0.020(2) 0.031(3) C2 0.063(3) 0.059(3) 0.040(3) 0.000(2) 0.015(2) 0.027(2) C3 0.082(4) 0.063(4) 0.055(4) -0.012(3) 0.028(3) 0.017(3) C4 0.056(3) 0.125(6) 0.054(4) -0.024(4) 0.009(3) 0.029(4) C5 0.097(5) 0.133(7) 0.042(4) 0.008(4) 0.018(3) 0.071(5) C6 0.125(6) 0.089(5) 0.063(4) 0.027(4) 0.049(4) 0.048(4) C7 0.072(3) 0.069(4) 0.051(3) 0.004(3) 0.020(3) 0.019(3) C8 0.041(2) 0.058(3) 0.058(3) -0.005(3) 0.017(2) 0.007(2) C9 0.043(2) 0.057(3) 0.037(3) -0.003(2) 0.011(2) 0.014(2) C10 0.052(3) 0.060(3) 0.050(3) 0.005(3) 0.010(2) 0.002(2) C11 0.066(3) 0.108(5) 0.039(3) 0.007(3) 0.022(3) 0.009(3) C12 0.074(3) 0.071(4) 0.048(3) -0.011(3) 0.014(3) 0.023(3) C13 0.083(4) 0.055(4) 0.064(4) -0.004(3) 0.017(3) 0.004(3) C14 0.064(3) 0.060(4) 0.049(3) -0.002(3) 0.024(2) 0.001(2) C15 0.057(3) 0.044(3) 0.045(3) 0.002(2) 0.013(2) 0.015(2) C16 0.058(3) 0.038(3) 0.050(3) 0.004(2) 0.021(2) 0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.967(4) . ? Cu1 N2 2.032(4) . ? Cu1 N1 2.043(4) . ? Cu1 N6 2.044(4) . ? Cu1 N8 2.373(4) 2_767 ? N1 C15 1.483(6) . ? N1 C1 1.492(6) . ? N2 C8 1.458(6) . ? N2 C16 1.494(6) . ? N3 N4 1.191(6) . ? N4 N5 1.146(6) . ? N6 N7 1.206(5) . ? N7 N8 1.158(5) . ? N8 Cu1 2.373(4) 2_767 ? C1 C2 1.479(7) . ? C2 C7 1.379(8) . ? C2 C3 1.397(7) . ? C3 C4 1.379(9) . ? C4 C5 1.374(11) . ? C5 C6 1.375(10) . ? C6 C7 1.365(9) . ? C8 C9 1.519(7) . ? C9 C14 1.361(7) . ? C9 C10 1.372(7) . ? C10 C11 1.381(8) . ? C11 C12 1.368(8) . ? C12 C13 1.357(9) . ? C13 C14 1.376(8) . ? C15 C16 1.499(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 160.37(17) . . ? N3 Cu1 N1 90.12(18) . . ? N2 Cu1 N1 84.34(16) . . ? N3 Cu1 N6 94.37(18) . . ? N2 Cu1 N6 89.02(17) . . ? N1 Cu1 N6 171.40(15) . . ? N3 Cu1 N8 100.34(18) . 2_767 ? N2 Cu1 N8 98.68(17) . 2_767 ? N1 Cu1 N8 92.14(16) . 2_767 ? N6 Cu1 N8 94.27(16) . 2_767 ? C15 N1 C1 113.0(4) . . ? C15 N1 Cu1 107.2(3) . . ? C1 N1 Cu1 114.8(3) . . ? C8 N2 C16 113.1(4) . . ? C8 N2 Cu1 116.2(3) . . ? C16 N2 Cu1 108.9(3) . . ? N4 N3 Cu1 126.0(4) . . ? N5 N4 N3 176.4(6) . . ? N7 N6 Cu1 113.5(3) . . ? N8 N7 N6 176.2(5) . . ? N7 N8 Cu1 142.6(4) . 2_767 ? C2 C1 N1 116.1(4) . . ? C7 C2 C3 117.7(5) . . ? C7 C2 C1 121.8(5) . . ? C3 C2 C1 120.5(5) . . ? C4 C3 C2 121.0(6) . . ? C5 C4 C3 119.3(6) . . ? C4 C5 C6 120.5(6) . . ? C7 C6 C5 119.7(7) . . ? C6 C7 C2 121.7(6) . . ? N2 C8 C9 114.5(4) . . ? C14 C9 C10 118.1(5) . . ? C14 C9 C8 121.2(5) . . ? C10 C9 C8 120.6(5) . . ? C9 C10 C11 120.9(5) . . ? C12 C11 C10 120.1(5) . . ? C13 C12 C11 118.8(5) . . ? C12 C13 C14 120.9(6) . . ? C9 C14 C13 121.1(5) . . ? N1 C15 C16 107.7(4) . . ? N2 C16 C15 108.6(4) . . ? _diffrn_measured_fraction_theta_max 0.778 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.778 _refine_diff_density_max 0.652 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.079