# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lang, Jian-Ping' _publ_contact_author_email jplang@suda.edu.cn _publ_section_title ; Cracking the framework of bulk CuCN with flexible bipyrazolyl-based ligands to assemble [CuCN]n-based coordination polymers ; loop_ _publ_author_name L.-L.Li L.-L.Liu A.-X.Zheng Yu.Chang M.Dai Z.-G.Ren H.-X.Li ; J.-P.Lang ; #===END data_[(CuCN)2(dmpzb)]n _database_code_depnum_ccdc_archive 'CCDC 740761' #TrackingRef '- JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H11 Cu N3' _chemical_formula_sum 'C8 H11 Cu N3' _chemical_formula_weight 212.75 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.198(2) _cell_length_b 10.819(2) _cell_length_c 8.9218(18) _cell_angle_alpha 90.00 _cell_angle_beta 109.11(3) _cell_angle_gamma 90.00 _cell_volume 930.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2958 _cell_measurement_theta_min 3.0635 _cell_measurement_theta_max 27.4894 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 2.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5976 _exptl_absorpt_correction_T_max 0.6567 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7217 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2116 _reflns_number_gt 1847 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0482P)^2^+1.8600P] 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_extinction_coef ? _refine_ls_number_reflns 2116 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1261 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.23814(5) 0.34834(5) 0.21983(6) 0.03195(19) Uani 1 1 d . . . N1 N 0.2071(3) 0.6040(3) 0.3394(4) 0.0277(7) Uani 1 1 d . . . N2 N 0.2920(3) 0.5233(3) 0.2977(4) 0.0273(7) Uani 1 1 d . . . N3 N 0.2180(4) 0.2562(4) 0.3981(4) 0.0406(9) Uani 1 1 d . . . C1 C 0.2688(5) 0.7144(4) 0.3848(5) 0.0310(9) Uani 1 1 d . . . C2 C 0.3993(5) 0.7052(4) 0.3716(5) 0.0367(10) Uani 1 1 d . . . H2 H 0.4680 0.7668 0.3950 0.044 Uiso 1 1 calc R . . C3 C 0.4087(4) 0.5857(4) 0.3164(5) 0.0322(9) Uani 1 1 d . . . C4 C 0.1980(5) 0.8181(4) 0.4358(6) 0.0443(12) Uani 1 1 d . . . H4A H 0.1027 0.8234 0.3659 0.066 Uiso 1 1 calc R . . H4B H 0.2458 0.8948 0.4313 0.066 Uiso 1 1 calc R . . H4C H 0.1994 0.8037 0.5437 0.066 Uiso 1 1 calc R . . C5 C 0.5253(5) 0.5273(5) 0.2753(6) 0.0448(12) Uani 1 1 d . . . H5A H 0.4880 0.4722 0.1857 0.067 Uiso 1 1 calc R . . H5B H 0.5834 0.4808 0.3656 0.067 Uiso 1 1 calc R . . H5C H 0.5803 0.5912 0.2478 0.067 Uiso 1 1 calc R . . C6 C 0.0709(4) 0.5631(4) 0.3389(5) 0.0319(9) Uani 1 1 d . . . H6A H 0.0415 0.4924 0.2671 0.038 Uiso 1 1 calc R . . H6B H 0.0038 0.6299 0.2980 0.038 Uiso 1 1 calc R . . C7 C 0.0694(4) 0.5261(4) 0.5032(5) 0.0324(9) Uani 1 1 d . . . H7A H 0.1417 0.4642 0.5483 0.039 Uiso 1 1 calc R . . H7B H 0.0903 0.5986 0.5729 0.039 Uiso 1 1 calc R . . C8 C 0.2221(5) 0.2110(4) 0.5166(5) 0.0318(9) 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 0.0400(4) 0.0321(3) 0.0251(3) -0.0018(2) 0.0126(2) -0.0009(2) N1 0.0312(18) 0.0304(17) 0.0231(17) -0.0013(13) 0.0111(14) 0.0008(14) N2 0.0290(18) 0.0290(17) 0.0268(18) -0.0014(13) 0.0130(15) -0.0010(14) N3 0.053(2) 0.039(2) 0.030(2) -0.0013(16) 0.0135(18) -0.0083(18) C1 0.040(2) 0.026(2) 0.025(2) -0.0017(16) 0.0080(18) -0.0020(18) C2 0.041(3) 0.032(2) 0.034(2) -0.0023(18) 0.008(2) -0.0085(19) C3 0.032(2) 0.036(2) 0.029(2) 0.0010(17) 0.0103(18) -0.0043(18) C4 0.057(3) 0.036(2) 0.039(3) -0.0036(19) 0.013(2) 0.006(2) C5 0.038(3) 0.047(3) 0.054(3) -0.002(2) 0.021(2) -0.001(2) C6 0.026(2) 0.042(2) 0.028(2) -0.0021(18) 0.0103(17) -0.0012(18) C7 0.023(2) 0.045(2) 0.031(2) -0.0023(18) 0.0113(18) 0.0011(18) C8 0.039(2) 0.030(2) 0.025(2) -0.0036(17) 0.0083(18) -0.0032(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 C8 1.880(4) 4_565 ? Cu1 N3 1.944(4) . ? Cu1 N2 2.029(3) . ? N1 C1 1.348(5) . ? N1 N2 1.364(4) . ? N1 C6 1.456(5) . ? N2 C3 1.331(5) . ? N3 C8 1.153(5) . ? C1 C2 1.377(6) . ? C1 C4 1.484(6) . ? C2 C3 1.398(6) . ? C2 H2 0.9400 . ? C3 C5 1.494(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.525(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C7 1.507(8) 3_566 ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 Cu1 1.880(4) 4_566 ? 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 C8 Cu1 N3 127.96(18) 4_565 . ? C8 Cu1 N2 125.27(16) 4_565 . ? N3 Cu1 N2 106.69(15) . . ? C1 N1 N2 111.9(3) . . ? C1 N1 C6 128.3(3) . . ? N2 N1 C6 119.6(3) . . ? C3 N2 N1 105.2(3) . . ? C3 N2 Cu1 130.3(3) . . ? N1 N2 Cu1 124.5(2) . . ? C8 N3 Cu1 170.3(4) . . ? N1 C1 C2 106.2(4) . . ? N1 C1 C4 122.4(4) . . ? C2 C1 C4 131.4(4) . . ? C1 C2 C3 106.1(4) . . ? C1 C2 H2 127.0 . . ? C3 C2 H2 127.0 . . ? N2 C3 C2 110.6(4) . . ? N2 C3 C5 120.4(4) . . ? C2 C3 C5 129.0(4) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 112.8(3) . . ? N1 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? N1 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C7 C7 C6 111.5(4) 3_566 . ? C7 C7 H7A 109.3 3_566 . ? C6 C7 H7A 109.3 . . ? C7 C7 H7B 109.3 3_566 . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N3 C8 Cu1 174.2(4) . 4_566 ? 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 C1 N1 N2 C3 -0.6(4) . . . . ? C6 N1 N2 C3 -177.4(3) . . . . ? C1 N1 N2 Cu1 -179.2(3) . . . . ? C6 N1 N2 Cu1 4.0(5) . . . . ? C8 Cu1 N2 C3 -62.5(4) 4_565 . . . ? N3 Cu1 N2 C3 114.4(4) . . . . ? C8 Cu1 N2 N1 115.7(3) 4_565 . . . ? N3 Cu1 N2 N1 -67.4(3) . . . . ? C8 Cu1 N3 C8 138(2) 4_565 . . . ? N2 Cu1 N3 C8 -39(2) . . . . ? N2 N1 C1 C2 0.2(5) . . . . ? C6 N1 C1 C2 176.7(4) . . . . ? N2 N1 C1 C4 180.0(4) . . . . ? C6 N1 C1 C4 -3.5(6) . . . . ? N1 C1 C2 C3 0.3(5) . . . . ? C4 C1 C2 C3 -179.5(4) . . . . ? N1 N2 C3 C2 0.7(5) . . . . ? Cu1 N2 C3 C2 179.2(3) . . . . ? N1 N2 C3 C5 -177.6(4) . . . . ? Cu1 N2 C3 C5 0.9(6) . . . . ? C1 C2 C3 N2 -0.6(5) . . . . ? C1 C2 C3 C5 177.5(4) . . . . ? C1 N1 C6 C7 -78.4(5) . . . . ? N2 N1 C6 C7 97.9(4) . . . . ? N1 C6 C7 C7 -175.1(4) . . . 3_566 ? Cu1 N3 C8 Cu1 24(6) . . . 4_566 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.443 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.085 #===END data_[(CuCN)2(dmpzp)]n _database_code_depnum_ccdc_archive 'CCDC 740762' #TrackingRef '- JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H24 Cu2 N6' _chemical_formula_sum 'C17 H24 Cu2 N6' _chemical_formula_weight 439.52 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.4333(17) _cell_length_b 9.0155(18) _cell_length_c 25.540(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.81(3) _cell_angle_gamma 90.00 _cell_volume 1939.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5990 _cell_measurement_theta_min 3.1944 _cell_measurement_theta_max 27.4778 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.204 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5576 _exptl_absorpt_correction_T_max 0.7333 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 7735 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4319 _reflns_number_gt 3367 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0359P)^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_extinction_coef ? _refine_ls_number_reflns 4319 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.004 _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 0.33833(4) 0.71104(4) 1.101884(15) 0.03405(12) Uani 1 1 d . . . Cu2 Cu 0.12228(4) 1.20844(4) 1.134227(16) 0.03790(12) Uani 1 1 d . . . N1 N 0.6538(3) 0.7188(3) 1.04864(9) 0.0293(5) Uani 1 1 d . . . N2 N 0.5745(3) 0.6787(2) 1.09179(9) 0.0290(5) Uani 1 1 d . . . N3 N 0.1982(2) 0.9044(2) 0.83468(9) 0.0269(5) Uani 1 1 d . . . N4 N 0.0711(3) 0.8152(2) 0.82198(9) 0.0292(5) Uani 1 1 d . . . N5 N 0.2545(3) 0.5162(3) 1.11632(11) 0.0431(7) Uani 1 1 d . . . N6 N 0.1936(3) 1.0162(3) 1.11024(11) 0.0457(7) Uani 1 1 d . . . C1 C 0.8079(3) 0.6776(3) 1.05365(12) 0.0362(7) Uani 1 1 d . . . C2 C 0.8288(3) 0.6096(3) 1.10164(12) 0.0382(7) Uani 1 1 d . . . H2 H 0.9234 0.5686 1.1163 0.046 Uiso 1 1 calc R . . C3 C 0.6828(3) 0.6134(3) 1.12410(11) 0.0329(7) Uani 1 1 d . . . C4 C 0.9240(4) 0.7108(4) 1.01272(14) 0.0558(10) Uani 1 1 d . . . H4A H 0.8915 0.6604 0.9804 0.084 Uiso 1 1 calc R . . H4B H 1.0287 0.6767 1.0247 0.084 Uiso 1 1 calc R . . H4C H 0.9270 0.8169 1.0066 0.084 Uiso 1 1 calc R . . C5 C 0.6389(4) 0.5572(4) 1.17649(12) 0.0445(8) Uani 1 1 d . . . H5A H 0.6370 0.6392 1.2010 0.067 Uiso 1 1 calc R . . H5B H 0.7165 0.4845 1.1891 0.067 Uiso 1 1 calc R . . H5C H 0.5348 0.5115 1.1734 0.067 Uiso 1 1 calc R . . C6 C 0.5692(3) 0.7934(3) 1.00530(12) 0.0330(7) Uani 1 1 d . . . H6A H 0.6462 0.8475 0.9850 0.040 Uiso 1 1 calc R . . H6B H 0.4968 0.8664 1.0195 0.040 Uiso 1 1 calc R . . C7 C 0.4744(3) 0.6905(3) 0.96858(12) 0.0345(7) Uani 1 1 d . . . H7A H 0.3869 0.6465 0.9872 0.041 Uiso 1 1 calc R . . H7B H 0.5429 0.6098 0.9574 0.041 Uiso 1 1 calc R . . C8 C 0.4077(3) 0.7743(3) 0.92067(12) 0.0349(7) Uani 1 1 d . . . H8A H 0.3878 0.7035 0.8920 0.042 Uiso 1 1 calc R . . H8B H 0.4881 0.8447 0.9096 0.042 Uiso 1 1 calc R . . C9 C 0.2539(3) 0.8594(3) 0.92944(11) 0.0318(6) Uani 1 1 d . . . H9A H 0.1664 0.7884 0.9313 0.038 Uiso 1 1 calc R . . H9B H 0.2646 0.9112 0.9632 0.038 Uiso 1 1 calc R . . C10 C 0.2128(3) 0.9714(3) 0.88660(11) 0.0298(6) Uani 1 1 d . . . H10A H 0.1124 1.0199 0.8940 0.036 Uiso 1 1 calc R . . H10B H 0.2955 1.0479 0.8869 0.036 Uiso 1 1 calc R . . C11 C 0.3005(3) 0.9085(3) 0.79568(12) 0.0356(7) Uani 1 1 d . . . C12 C 0.2362(4) 0.8199(3) 0.75621(12) 0.0386(7) Uani 1 1 d . . . H12 H 0.2793 0.8010 0.7236 0.046 Uiso 1 1 calc R . . C13 C 0.0953(4) 0.7639(3) 0.77404(13) 0.0363(7) Uani 1 1 d . . . C14 C 0.4490(4) 0.9992(4) 0.79862(13) 0.0557(10) Uani 1 1 d . . . H14A H 0.4353 1.0832 0.8217 0.084 Uiso 1 1 calc R . . H14B H 0.4713 1.0345 0.7639 0.084 Uiso 1 1 calc R . . H14C H 0.5367 0.9387 0.8122 0.084 Uiso 1 1 calc R . . C15 C -0.0224(4) 0.6643(4) 0.74569(15) 0.0567(10) Uani 1 1 d . . . H15A H -0.0876 0.6159 0.7709 0.085 Uiso 1 1 calc R . . H15B H 0.0336 0.5899 0.7263 0.085 Uiso 1 1 calc R . . H15C H -0.0894 0.7227 0.7216 0.085 Uiso 1 1 calc R . . C16 C 0.2071(3) 0.3990(3) 1.12423(13) 0.0352(7) Uani 1 1 d . . . C17 C 0.2460(3) 0.9011(3) 1.10332(13) 0.0357(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 Cu1 0.0313(2) 0.0262(2) 0.0446(2) -0.00119(16) 0.00142(16) 0.00173(15) Cu2 0.0336(2) 0.0262(2) 0.0536(3) 0.00251(17) -0.00077(18) -0.00129(16) N1 0.0283(12) 0.0306(13) 0.0288(13) 0.0012(10) -0.0006(10) -0.0016(10) N2 0.0277(12) 0.0266(12) 0.0325(13) 0.0026(10) 0.0004(10) 0.0019(10) N3 0.0283(11) 0.0249(12) 0.0270(13) 0.0020(10) -0.0048(10) -0.0015(10) N4 0.0311(12) 0.0214(12) 0.0347(14) 0.0005(10) -0.0043(10) -0.0030(10) N5 0.0332(13) 0.0348(16) 0.062(2) -0.0015(14) 0.0068(13) -0.0006(12) N6 0.0377(14) 0.0323(15) 0.068(2) -0.0007(14) 0.0081(14) -0.0006(12) C1 0.0253(14) 0.0451(19) 0.0383(18) -0.0066(15) 0.0019(13) 0.0039(13) C2 0.0292(14) 0.0430(19) 0.0420(19) 0.0008(15) -0.0045(13) 0.0113(14) C3 0.0357(15) 0.0301(15) 0.0324(16) 0.0013(13) -0.0037(13) 0.0052(13) C4 0.0392(18) 0.080(3) 0.050(2) -0.001(2) 0.0113(16) 0.0002(18) C5 0.0497(18) 0.0426(19) 0.0409(19) 0.0090(15) -0.0016(15) 0.0050(16) C6 0.0370(15) 0.0282(15) 0.0333(16) 0.0054(13) -0.0041(13) -0.0016(13) C7 0.0386(16) 0.0281(15) 0.0364(17) -0.0009(13) -0.0020(13) 0.0008(13) C8 0.0409(16) 0.0337(16) 0.0300(16) 0.0009(13) -0.0001(13) 0.0090(14) C9 0.0316(14) 0.0371(16) 0.0264(15) 0.0002(13) -0.0020(12) -0.0043(13) C10 0.0269(14) 0.0292(15) 0.0330(16) -0.0038(12) -0.0008(12) 0.0002(12) C11 0.0333(15) 0.0375(17) 0.0358(18) 0.0020(14) -0.0002(13) 0.0001(13) C12 0.0477(18) 0.0390(18) 0.0290(16) -0.0033(14) 0.0002(14) 0.0030(15) C13 0.0420(17) 0.0263(15) 0.0395(18) -0.0061(13) -0.0097(14) 0.0023(13) C14 0.0471(19) 0.075(3) 0.045(2) -0.0101(19) 0.0086(17) -0.0210(19) C15 0.063(2) 0.049(2) 0.056(2) -0.0163(18) -0.0119(18) -0.0090(18) C16 0.0283(14) 0.0253(15) 0.052(2) -0.0039(14) 0.0063(14) -0.0002(12) C17 0.0263(14) 0.0260(15) 0.055(2) 0.0018(14) 0.0010(14) -0.0018(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 Cu1 C17 1.883(3) . ? Cu1 N5 1.936(3) . ? Cu1 N2 2.042(2) . ? Cu2 C16 1.883(3) 1_565 ? Cu2 N6 1.944(3) . ? Cu2 N4 2.034(2) 3_577 ? N1 C1 1.352(4) . ? N1 N2 1.365(3) . ? N1 C6 1.452(3) . ? N2 C3 1.337(3) . ? N3 C11 1.350(3) . ? N3 N4 1.366(3) . ? N3 C10 1.457(3) . ? N4 C13 1.334(4) . ? N4 Cu2 2.034(2) 3_577 ? N5 C16 1.151(4) . ? N6 C17 1.145(4) . ? C1 C2 1.374(4) . ? C1 C4 1.497(4) . ? C2 C3 1.384(4) . ? C2 H2 0.9400 . ? C3 C5 1.494(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.519(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.522(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.533(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.516(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.377(4) . ? C11 C14 1.494(4) . ? C12 C13 1.388(4) . ? C12 H12 0.9400 . ? C13 C15 1.498(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 Cu2 1.883(3) 1_545 ? 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 C17 Cu1 N5 131.82(11) . . ? C17 Cu1 N2 122.63(10) . . ? N5 Cu1 N2 105.19(9) . . ? C16 Cu2 N6 130.22(11) 1_565 . ? C16 Cu2 N4 119.36(10) 1_565 3_577 ? N6 Cu2 N4 110.40(10) . 3_577 ? C1 N1 N2 110.9(2) . . ? C1 N1 C6 129.3(3) . . ? N2 N1 C6 119.8(2) . . ? C3 N2 N1 105.6(2) . . ? C3 N2 Cu1 128.75(19) . . ? N1 N2 Cu1 125.68(18) . . ? C11 N3 N4 111.3(2) . . ? C11 N3 C10 129.2(2) . . ? N4 N3 C10 119.4(2) . . ? C13 N4 N3 105.6(2) . . ? C13 N4 Cu2 129.1(2) . 3_577 ? N3 N4 Cu2 124.90(18) . 3_577 ? C16 N5 Cu1 178.5(3) . . ? C17 N6 Cu2 169.9(3) . . ? N1 C1 C2 106.7(2) . . ? N1 C1 C4 122.5(3) . . ? C2 C1 C4 130.7(3) . . ? C1 C2 C3 106.3(3) . . ? C1 C2 H2 126.8 . . ? C3 C2 H2 126.8 . . ? N2 C3 C2 110.5(3) . . ? N2 C3 C5 120.7(3) . . ? C2 C3 C5 128.8(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 114.3(2) . . ? N1 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? N1 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 C8 110.8(2) . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 114.4(2) . . ? C7 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 113.1(2) . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N3 C10 C9 112.7(2) . . ? N3 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? N3 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N3 C11 C12 106.4(3) . . ? N3 C11 C14 122.8(3) . . ? C12 C11 C14 130.8(3) . . ? C11 C12 C13 106.5(3) . . ? C11 C12 H12 126.8 . . ? C13 C12 H12 126.8 . . ? N4 C13 C12 110.3(3) . . ? N4 C13 C15 121.6(3) . . ? C12 C13 C15 128.1(3) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N5 C16 Cu2 177.1(3) . 1_545 ? N6 C17 Cu1 172.2(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.595 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.067 # Attachment '- JPLangCIF.cif' data_[(CuCN)3(dmpzm)]n _database_code_depnum_ccdc_archive 'CCDC 762447' #TrackingRef '- JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H16 Cu3 N7' _chemical_formula_sum 'C14 H16 Cu3 N7' _chemical_formula_weight 472.99 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 7.4770(15) _cell_length_b 34.389(7) _cell_length_c 7.6782(15) _cell_angle_alpha 90.00 _cell_angle_beta 114.46(3) _cell_angle_gamma 90.00 _cell_volume 1797.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6121 _cell_measurement_theta_min 3.0512 _cell_measurement_theta_max 27.4778 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 3.528 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4848 _exptl_absorpt_correction_T_max 0.7193 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10370 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.1100 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4094 _reflns_number_gt 2259 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1000P)^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_extinction_coef ? _refine_ls_number_reflns 4094 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1612 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2137 _refine_ls_wR_factor_gt 0.1719 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.60072(15) 0.05663(3) 0.39926(16) 0.0427(3) Uani 1 1 d . . . Cu3 Cu 0.34141(16) -0.21096(3) -0.02899(16) 0.0459(3) Uani 1 1 d . . . Cu2 Cu 0.43433(18) -0.07573(3) 0.18184(19) 0.0562(4) Uani 1 1 d . . . N1 N 0.5340(10) 0.14119(18) 0.4023(10) 0.0401(17) Uani 1 1 d . . . N2 N 0.4445(10) 0.10569(19) 0.3634(10) 0.0393(17) Uani 1 1 d . . . N3 N 0.8676(9) 0.12131(18) 0.5902(10) 0.0390(17) Uani 1 1 d . . . N4 N 0.8501(10) 0.0812(2) 0.5820(10) 0.0418(17) Uani 1 1 d . . . N5 N 0.4917(12) -0.0246(2) 0.2481(13) 0.058(2) Uani 1 1 d . . . N6 N 0.3560(11) -0.1580(2) 0.0520(11) 0.054(2) Uani 1 1 d . . . N7 N 0.5314(14) -0.2488(2) 0.1283(13) 0.064(2) Uani 1 1 d . . . C1 C 0.4093(14) 0.1699(2) 0.3941(14) 0.046(2) Uani 1 1 d . . . C2 C 0.2315(15) 0.1527(3) 0.3512(14) 0.051(2) Uani 1 1 d . . . H2 H 0.1136 0.1652 0.3342 0.061 Uiso 1 1 calc R . . C3 C 0.2598(13) 0.1131(3) 0.3374(13) 0.045(2) Uani 1 1 d . . . C4 C 0.4690(17) 0.2118(2) 0.4238(18) 0.065(3) Uani 1 1 d . . . H4A H 0.5860 0.2146 0.5420 0.097 Uiso 1 1 calc R . . H4B H 0.3634 0.2272 0.4310 0.097 Uiso 1 1 calc R . . H4C H 0.4962 0.2208 0.3175 0.097 Uiso 1 1 calc R . . C5 C 0.1185(13) 0.0797(3) 0.2970(15) 0.054(3) Uani 1 1 d . . . H5A H 0.1744 0.0568 0.2653 0.081 Uiso 1 1 calc R . . H5B H -0.0041 0.0863 0.1903 0.081 Uiso 1 1 calc R . . H5C H 0.0939 0.0745 0.4093 0.081 Uiso 1 1 calc R . . C6 C 0.7384(12) 0.1434(2) 0.4265(12) 0.038(2) Uani 1 1 d . . . H6A H 0.7479 0.1334 0.3112 0.046 Uiso 1 1 calc R . . H6B H 0.7805 0.1706 0.4424 0.046 Uiso 1 1 calc R . . C7 C 1.0277(13) 0.1329(2) 0.7433(13) 0.045(2) Uani 1 1 d . . . C8 C 1.1162(12) 0.0999(3) 0.8429(13) 0.045(2) Uani 1 1 d . . . H8 H 1.2302 0.0985 0.9577 0.054 Uiso 1 1 calc R . . C9 C 1.0025(13) 0.0689(3) 0.7390(14) 0.045(2) Uani 1 1 d . . . C10 C 1.0826(14) 0.1746(3) 0.7896(15) 0.060(3) Uani 1 1 d . . . H10A H 1.1148 0.1860 0.6905 0.090 Uiso 1 1 calc R . . H10B H 1.1956 0.1764 0.9117 0.090 Uiso 1 1 calc R . . H10C H 0.9730 0.1886 0.7965 0.090 Uiso 1 1 calc R . . C11 C 1.0298(14) 0.0257(3) 0.7838(15) 0.054(3) Uani 1 1 d . . . H11A H 0.9094 0.0150 0.7828 0.081 Uiso 1 1 calc R . . H11B H 1.1361 0.0220 0.9091 0.081 Uiso 1 1 calc R . . H11C H 1.0613 0.0127 0.6881 0.081 Uiso 1 1 calc R . . C12 C 0.5354(13) 0.0069(3) 0.2980(13) 0.046(2) Uani 1 1 d . . . C13 C 0.3800(13) -0.1259(2) 0.1044(13) 0.041(2) Uani 1 1 d . . . C14 C 0.6468(12) -0.2694(2) 0.2400(11) 0.0356(19) 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 0.0471(6) 0.0326(5) 0.0482(7) -0.0064(5) 0.0197(5) -0.0041(4) Cu3 0.0514(7) 0.0358(6) 0.0479(7) -0.0003(5) 0.0179(5) -0.0033(5) Cu2 0.0651(8) 0.0371(6) 0.0642(8) -0.0151(6) 0.0244(6) -0.0076(5) N1 0.042(4) 0.030(3) 0.047(4) 0.003(3) 0.016(3) 0.002(3) N2 0.036(4) 0.036(4) 0.042(4) -0.002(3) 0.013(3) -0.002(3) N3 0.040(4) 0.029(3) 0.044(4) -0.002(3) 0.013(3) -0.005(3) N4 0.056(4) 0.038(4) 0.039(4) -0.004(3) 0.027(4) -0.004(3) N5 0.062(5) 0.047(5) 0.072(6) -0.011(4) 0.035(4) -0.005(4) N6 0.057(5) 0.052(5) 0.043(5) -0.006(4) 0.011(4) 0.001(4) N7 0.079(6) 0.052(5) 0.062(6) -0.019(4) 0.032(5) -0.022(5) C1 0.060(6) 0.038(4) 0.052(6) -0.002(4) 0.036(5) 0.001(4) C2 0.061(6) 0.050(5) 0.055(6) 0.006(5) 0.038(5) 0.008(5) C3 0.046(5) 0.048(5) 0.043(5) -0.006(4) 0.022(4) -0.001(4) C4 0.092(8) 0.028(4) 0.104(9) 0.004(5) 0.070(7) 0.008(5) C5 0.038(5) 0.063(6) 0.061(6) -0.005(5) 0.020(4) 0.001(5) C6 0.045(5) 0.035(4) 0.035(5) 0.006(4) 0.015(4) 0.009(4) C7 0.048(5) 0.044(5) 0.042(5) -0.009(4) 0.020(4) -0.017(4) C8 0.036(4) 0.060(6) 0.038(5) 0.004(4) 0.013(4) -0.008(4) C9 0.038(4) 0.042(5) 0.054(6) 0.014(4) 0.017(4) 0.005(4) C10 0.054(6) 0.051(5) 0.062(7) -0.006(5) 0.012(5) -0.014(5) C11 0.049(5) 0.055(6) 0.065(7) 0.017(5) 0.030(5) 0.014(5) C12 0.049(5) 0.041(5) 0.050(6) -0.009(4) 0.021(5) 0.001(4) C13 0.054(5) 0.032(4) 0.042(5) -0.007(4) 0.024(4) 0.003(4) C14 0.043(4) 0.029(4) 0.025(4) 0.006(3) 0.003(4) 0.008(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 C12 1.858(9) . ? Cu1 N4 1.998(7) . ? Cu1 N2 2.005(7) . ? Cu3 C14 1.893(7) 4 ? Cu3 N6 1.914(8) . ? Cu3 N7 1.936(10) . ? Cu2 C13 1.814(8) . ? Cu2 N5 1.832(8) . ? N1 C1 1.343(10) . ? N1 N2 1.365(9) . ? N1 C6 1.463(11) . ? N2 C3 1.335(11) . ? N3 C7 1.345(11) . ? N3 N4 1.384(9) . ? N3 C6 1.443(10) . ? N4 C9 1.339(11) . ? N5 C12 1.150(11) . ? N6 C13 1.163(11) . ? N7 C14 1.171(11) . ? C1 C2 1.365(13) . ? C1 C4 1.497(11) . ? C2 C3 1.392(12) . ? C2 H2 0.9400 . ? C3 C5 1.501(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.375(12) . ? C7 C10 1.495(12) . ? C8 C9 1.390(13) . ? C8 H8 0.9400 . ? C9 C11 1.518(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C14 Cu3 1.893(7) 4_656 ? 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 C12 Cu1 N4 133.7(3) . . ? C12 Cu1 N2 132.8(3) . . ? N4 Cu1 N2 93.5(3) . . ? C14 Cu3 N6 124.2(3) 4 . ? C14 Cu3 N7 115.2(3) 4 . ? N6 Cu3 N7 120.6(3) . . ? C13 Cu2 N5 176.8(4) . . ? C1 N1 N2 112.4(7) . . ? C1 N1 C6 129.6(7) . . ? N2 N1 C6 117.7(6) . . ? C3 N2 N1 104.3(7) . . ? C3 N2 Cu1 133.5(6) . . ? N1 N2 Cu1 121.2(5) . . ? C7 N3 N4 111.6(7) . . ? C7 N3 C6 129.7(7) . . ? N4 N3 C6 117.9(6) . . ? C9 N4 N3 104.2(7) . . ? C9 N4 Cu1 134.2(6) . . ? N3 N4 Cu1 119.8(5) . . ? C12 N5 Cu2 176.6(9) . . ? C13 N6 Cu3 174.8(8) . . ? C14 N7 Cu3 172.8(8) . . ? N1 C1 C2 106.3(8) . . ? N1 C1 C4 122.9(8) . . ? C2 C1 C4 130.8(9) . . ? C1 C2 C3 106.3(8) . . ? C1 C2 H2 126.9 . . ? C3 C2 H2 126.9 . . ? N2 C3 C2 110.8(8) . . ? N2 C3 C5 118.8(8) . . ? C2 C3 C5 130.4(8) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N1 111.8(7) . . ? N3 C6 H6A 109.3 . . ? N1 C6 H6A 109.3 . . ? N3 C6 H6B 109.3 . . ? N1 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N3 C7 C8 106.9(7) . . ? N3 C7 C10 123.3(8) . . ? C8 C7 C10 129.7(8) . . ? C7 C8 C9 105.9(8) . . ? C7 C8 H8 127.0 . . ? C9 C8 H8 127.0 . . ? N4 C9 C8 111.4(8) . . ? N4 C9 C11 119.8(8) . . ? C8 C9 C11 128.8(8) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 Cu1 174.4(9) . . ? N6 C13 Cu2 175.5(9) . . ? N7 C14 Cu3 161.8(7) . 4_656 ? 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 C1 N1 N2 C3 -2.3(10) . . . . ? C6 N1 N2 C3 -176.3(7) . . . . ? C1 N1 N2 Cu1 -171.7(6) . . . . ? C6 N1 N2 Cu1 14.3(10) . . . . ? C12 Cu1 N2 C3 35.8(11) . . . . ? N4 Cu1 N2 C3 -144.4(9) . . . . ? C12 Cu1 N2 N1 -158.3(6) . . . . ? N4 Cu1 N2 N1 21.5(7) . . . . ? C7 N3 N4 C9 1.8(10) . . . . ? C6 N3 N4 C9 172.1(8) . . . . ? C7 N3 N4 Cu1 168.4(6) . . . . ? C6 N3 N4 Cu1 -21.4(10) . . . . ? C12 Cu1 N4 C9 -36.5(11) . . . . ? N2 Cu1 N4 C9 143.7(9) . . . . ? C12 Cu1 N4 N3 161.8(6) . . . . ? N2 Cu1 N4 N3 -18.0(6) . . . . ? C13 Cu2 N5 C12 -119(15) . . . . ? C14 Cu3 N6 C13 -134(9) 4 . . . ? N7 Cu3 N6 C13 47(9) . . . . ? C14 Cu3 N7 C14 -147(7) 4 . . . ? N6 Cu3 N7 C14 33(7) . . . . ? N2 N1 C1 C2 1.0(11) . . . . ? C6 N1 C1 C2 174.1(8) . . . . ? N2 N1 C1 C4 -177.6(9) . . . . ? C6 N1 C1 C4 -4.5(15) . . . . ? N1 C1 C2 C3 0.7(11) . . . . ? C4 C1 C2 C3 179.2(11) . . . . ? N1 N2 C3 C2 2.7(10) . . . . ? Cu1 N2 C3 C2 170.2(6) . . . . ? N1 N2 C3 C5 -178.2(8) . . . . ? Cu1 N2 C3 C5 -10.6(14) . . . . ? C1 C2 C3 N2 -2.2(11) . . . . ? C1 C2 C3 C5 178.8(10) . . . . ? C7 N3 C6 N1 -123.5(9) . . . . ? N4 N3 C6 N1 68.3(9) . . . . ? C1 N1 C6 N3 123.3(9) . . . . ? N2 N1 C6 N3 -63.9(9) . . . . ? N4 N3 C7 C8 -1.8(11) . . . . ? C6 N3 C7 C8 -170.6(8) . . . . ? N4 N3 C7 C10 -179.4(8) . . . . ? C6 N3 C7 C10 11.8(15) . . . . ? N3 C7 C8 C9 1.1(11) . . . . ? C10 C7 C8 C9 178.4(10) . . . . ? N3 N4 C9 C8 -1.0(10) . . . . ? Cu1 N4 C9 C8 -164.7(6) . . . . ? N3 N4 C9 C11 178.0(8) . . . . ? Cu1 N4 C9 C11 14.4(14) . . . . ? C7 C8 C9 N4 0.0(11) . . . . ? C7 C8 C9 C11 -179.0(9) . . . . ? Cu2 N5 C12 Cu1 -61(20) . . . . ? N4 Cu1 C12 N5 89(9) . . . . ? N2 Cu1 C12 N5 -91(9) . . . . ? Cu3 N6 C13 Cu2 25(19) . . . . ? N5 Cu2 C13 N6 44(15) . . . . ? Cu3 N7 C14 Cu3 -17(9) . . . 4_656 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.494 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.109 #===END data_[(CuCN)3(dmpze)]n _database_code_depnum_ccdc_archive 'CCDC 762448' #TrackingRef '- JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H18 Cu3 N7' _chemical_formula_sum 'C15 H18 Cu3 N7' _chemical_formula_weight 487.01 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.126(3) _cell_length_b 17.340(4) _cell_length_c 8.1515(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.77(3) _cell_angle_gamma 90.00 _cell_volume 1845.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6667 _cell_measurement_theta_min 3.0552 _cell_measurement_theta_max 27.5049 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 3.437 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4254 _exptl_absorpt_correction_T_max 0.8469 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10551 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4188 _reflns_number_gt 2678 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0756P)^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_extinction_coef ? _refine_ls_number_reflns 4188 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.74460(5) 0.60778(3) 0.46311(9) 0.0360(2) Uani 1 1 d . . . Cu2 Cu 0.75214(6) 0.88720(4) 0.46493(11) 0.0518(3) Uani 1 1 d . . . Cu3 Cu 0.75257(5) 1.16716(4) 0.51877(8) 0.0384(2) Uani 1 1 d . . . N1 N 0.6247(3) 0.4617(2) 0.4126(5) 0.0285(9) Uani 1 1 d . . . N2 N 0.6331(3) 0.5382(2) 0.3742(5) 0.0313(9) Uani 1 1 d . . . N3 N 0.8754(3) 0.4768(2) 0.6001(5) 0.0322(10) Uani 1 1 d . . . N4 N 0.8634(3) 0.5554(2) 0.5865(6) 0.0363(10) Uani 1 1 d . . . N5 N 0.7437(4) 0.7821(3) 0.4470(7) 0.0559(15) Uani 1 1 d . . . N6 N 0.7543(3) 1.0584(3) 0.5012(6) 0.0428(12) Uani 1 1 d . . . N7 N 0.7531(4) 1.2296(3) 0.7148(7) 0.0599(15) Uani 1 1 d . . . C1 C 0.5438(4) 0.4288(3) 0.3274(7) 0.0337(12) Uani 1 1 d . . . C2 C 0.4972(4) 0.4857(3) 0.2267(7) 0.0380(13) Uani 1 1 d . . . H2 H 0.4387 0.4805 0.1509 0.046 Uiso 1 1 calc R . . C3 C 0.5548(4) 0.5520(3) 0.2612(6) 0.0327(11) Uani 1 1 d . . . C4 C 0.5139(4) 0.3460(3) 0.3446(8) 0.0431(14) Uani 1 1 d . . . H4A H 0.5671 0.3130 0.3087 0.065 Uiso 1 1 calc R . . H4B H 0.4501 0.3363 0.2771 0.065 Uiso 1 1 calc R . . H4C H 0.5052 0.3351 0.4591 0.065 Uiso 1 1 calc R . . C5 C 0.5361(5) 0.6308(3) 0.1868(8) 0.0467(15) Uani 1 1 d . . . H5A H 0.5595 0.6698 0.2672 0.070 Uiso 1 1 calc R . . H5B H 0.4635 0.6375 0.1549 0.070 Uiso 1 1 calc R . . H5C H 0.5734 0.6358 0.0904 0.070 Uiso 1 1 calc R . . C6 C 0.6974(4) 0.4266(3) 0.5405(7) 0.0340(12) Uani 1 1 d . . . H6A H 0.6761 0.3734 0.5590 0.041 Uiso 1 1 calc R . . H6B H 0.6945 0.4550 0.6439 0.041 Uiso 1 1 calc R . . C7 C 0.8069(4) 0.4262(3) 0.4966(7) 0.0336(12) Uani 1 1 d . . . H7A H 0.8334 0.3734 0.5063 0.040 Uiso 1 1 calc R . . H7B H 0.8074 0.4422 0.3814 0.040 Uiso 1 1 calc R . . C8 C 0.9540(4) 0.4578(3) 0.7092(7) 0.0354(12) Uani 1 1 d . . . C9 C 0.9965(4) 0.5255(3) 0.7719(7) 0.0426(14) Uani 1 1 d . . . H9 H 1.0530 0.5309 0.8516 0.051 Uiso 1 1 calc R . . C10 C 0.9384(4) 0.5846(3) 0.6925(7) 0.0379(13) Uani 1 1 d . . . C11 C 0.9858(5) 0.3771(3) 0.7523(9) 0.0502(16) Uani 1 1 d . . . H11A H 0.9298 0.3502 0.7966 0.075 Uiso 1 1 calc R . . H11B H 1.0448 0.3779 0.8342 0.075 Uiso 1 1 calc R . . H11C H 1.0036 0.3507 0.6542 0.075 Uiso 1 1 calc R . . C12 C 0.9547(5) 0.6701(3) 0.7119(9) 0.0549(16) Uani 1 1 d . . . H12A H 0.9828 0.6904 0.6151 0.082 Uiso 1 1 calc R . . H12B H 1.0020 0.6800 0.8088 0.082 Uiso 1 1 calc R . . H12C H 0.8898 0.6951 0.7243 0.082 Uiso 1 1 calc R . . C13 C 0.7431(5) 0.7163(3) 0.4458(8) 0.0451(15) Uani 1 1 d . . . C14 C 0.7551(4) 0.9909(3) 0.4884(7) 0.0323(12) Uani 1 1 d . . . C15 C 0.7524(4) 1.2716(3) 0.8243(6) 0.0331(12) 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 0.0337(4) 0.0254(3) 0.0483(5) 0.0000(3) 0.0005(3) -0.0010(3) Cu2 0.0428(5) 0.0244(4) 0.0856(7) -0.0002(4) -0.0070(4) 0.0003(3) Cu3 0.0425(4) 0.0311(4) 0.0410(4) -0.0012(3) 0.0010(3) 0.0004(3) N1 0.026(2) 0.024(2) 0.035(2) -0.0002(17) -0.0017(18) -0.0005(17) N2 0.031(2) 0.027(2) 0.035(2) 0.0060(18) -0.0024(18) 0.0008(18) N3 0.024(2) 0.031(2) 0.040(3) 0.0005(19) -0.0050(19) -0.0001(17) N4 0.034(2) 0.029(2) 0.044(3) 0.001(2) -0.008(2) -0.0031(19) N5 0.054(3) 0.032(3) 0.081(4) 0.000(3) 0.001(3) -0.002(2) N6 0.036(3) 0.045(3) 0.046(3) 0.002(2) -0.005(2) -0.004(2) N7 0.068(4) 0.052(3) 0.058(4) 0.023(3) 0.000(3) -0.008(3) C1 0.029(3) 0.036(3) 0.036(3) -0.004(2) 0.001(2) -0.004(2) C2 0.026(3) 0.043(3) 0.043(3) -0.002(3) -0.006(2) 0.006(2) C3 0.030(3) 0.037(3) 0.031(3) -0.004(2) 0.001(2) 0.007(2) C4 0.037(3) 0.035(3) 0.056(4) -0.006(3) -0.004(3) -0.013(2) C5 0.040(3) 0.049(3) 0.050(4) 0.013(3) -0.005(3) 0.011(3) C6 0.029(3) 0.033(3) 0.038(3) 0.004(2) -0.006(2) -0.002(2) C7 0.031(3) 0.025(2) 0.043(3) -0.003(2) -0.002(2) 0.002(2) C8 0.021(2) 0.045(3) 0.039(3) 0.002(3) -0.003(2) -0.002(2) C9 0.027(3) 0.060(4) 0.039(3) 0.003(3) -0.009(2) -0.010(3) C10 0.025(3) 0.046(3) 0.042(3) -0.012(3) 0.003(2) -0.009(2) C11 0.036(3) 0.050(4) 0.062(4) 0.014(3) -0.005(3) 0.000(3) C12 0.048(4) 0.049(4) 0.066(4) -0.012(3) -0.003(3) -0.010(3) C13 0.042(3) 0.031(3) 0.061(4) 0.006(3) 0.001(3) -0.004(2) C14 0.027(3) 0.020(2) 0.048(3) 0.003(2) -0.004(2) 0.003(2) C15 0.057(4) 0.021(2) 0.021(3) -0.005(2) 0.001(2) -0.005(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 C13 1.887(6) . ? Cu1 N2 1.978(4) . ? Cu1 N4 1.988(4) . ? Cu2 C14 1.809(5) . ? Cu2 N5 1.831(5) . ? Cu3 N6 1.891(5) . ? Cu3 C15 1.908(5) 4_585 ? Cu3 N7 1.929(7) . ? N1 C1 1.336(6) . ? N1 N2 1.370(5) . ? N1 C6 1.472(6) . ? N2 C3 1.331(6) . ? N3 C8 1.334(6) . ? N3 N4 1.376(6) . ? N3 C7 1.460(6) . ? N4 C10 1.342(7) . ? N5 C13 1.141(8) . ? N6 C14 1.175(7) . ? N7 C15 1.153(7) . ? C1 C2 1.386(7) . ? C1 C4 1.499(7) . ? C2 C3 1.389(7) . ? C2 H2 0.9400 . ? C3 C5 1.505(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.517(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.376(8) . ? C8 C11 1.492(8) . ? C9 C10 1.398(8) . ? C9 H9 0.9400 . ? C10 C12 1.503(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C15 Cu3 1.908(5) 4_586 ? 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 C13 Cu1 N2 125.4(2) . . ? C13 Cu1 N4 119.7(2) . . ? N2 Cu1 N4 114.88(17) . . ? C14 Cu2 N5 177.2(2) . . ? N6 Cu3 C15 119.4(2) . 4_585 ? N6 Cu3 N7 128.5(2) . . ? C15 Cu3 N7 112.0(2) 4_585 . ? C1 N1 N2 111.8(4) . . ? C1 N1 C6 128.0(4) . . ? N2 N1 C6 120.1(4) . . ? C3 N2 N1 105.0(4) . . ? C3 N2 Cu1 129.4(3) . . ? N1 N2 Cu1 125.5(3) . . ? C8 N3 N4 111.9(4) . . ? C8 N3 C7 128.8(4) . . ? N4 N3 C7 119.3(4) . . ? C10 N4 N3 104.6(4) . . ? C10 N4 Cu1 129.8(4) . . ? N3 N4 Cu1 124.8(3) . . ? C13 N5 Cu2 175.2(6) . . ? C14 N6 Cu3 179.2(5) . . ? C15 N7 Cu3 174.9(5) . . ? N1 C1 C2 106.6(4) . . ? N1 C1 C4 124.2(5) . . ? C2 C1 C4 129.2(5) . . ? C1 C2 C3 105.6(5) . . ? C1 C2 H2 127.2 . . ? C3 C2 H2 127.2 . . ? N2 C3 C2 111.0(5) . . ? N2 C3 C5 121.7(5) . . ? C2 C3 C5 127.4(5) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 113.4(4) . . ? N1 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? N1 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N3 C7 C6 113.8(4) . . ? N3 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N3 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N3 C8 C9 107.2(5) . . ? N3 C8 C11 124.6(5) . . ? C9 C8 C11 128.2(5) . . ? C8 C9 C10 105.8(5) . . ? C8 C9 H9 127.1 . . ? C10 C9 H9 127.1 . . ? N4 C10 C9 110.6(5) . . ? N4 C10 C12 121.8(5) . . ? C9 C10 C12 127.5(5) . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 Cu1 175.2(6) . . ? N6 C14 Cu2 178.1(5) . . ? N7 C15 Cu3 174.6(5) . 4_586 ? 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 C1 N1 N2 C3 -0.3(5) . . . . ? C6 N1 N2 C3 -177.5(4) . . . . ? C1 N1 N2 Cu1 -177.1(3) . . . . ? C6 N1 N2 Cu1 5.7(6) . . . . ? C13 Cu1 N2 C3 17.3(6) . . . . ? N4 Cu1 N2 C3 -165.0(4) . . . . ? C13 Cu1 N2 N1 -166.7(4) . . . . ? N4 Cu1 N2 N1 10.9(4) . . . . ? C8 N3 N4 C10 0.0(6) . . . . ? C7 N3 N4 C10 -178.3(5) . . . . ? C8 N3 N4 Cu1 -170.8(4) . . . . ? C7 N3 N4 Cu1 10.9(6) . . . . ? C13 Cu1 N4 C10 15.2(6) . . . . ? N2 Cu1 N4 C10 -162.6(5) . . . . ? C13 Cu1 N4 N3 -176.5(4) . . . . ? N2 Cu1 N4 N3 5.7(5) . . . . ? C14 Cu2 N5 C13 -91(8) . . . . ? C15 Cu3 N6 C14 -12(33) 4_585 . . . ? N7 Cu3 N6 C14 169(100) . . . . ? N6 Cu3 N7 C15 -173(6) . . . . ? C15 Cu3 N7 C15 8(6) 4_585 . . . ? N2 N1 C1 C2 0.7(6) . . . . ? C6 N1 C1 C2 177.6(5) . . . . ? N2 N1 C1 C4 -179.1(5) . . . . ? C6 N1 C1 C4 -2.2(8) . . . . ? N1 C1 C2 C3 -0.8(6) . . . . ? C4 C1 C2 C3 179.0(5) . . . . ? N1 N2 C3 C2 -0.2(6) . . . . ? Cu1 N2 C3 C2 176.4(4) . . . . ? N1 N2 C3 C5 179.6(5) . . . . ? Cu1 N2 C3 C5 -3.8(7) . . . . ? C1 C2 C3 N2 0.7(6) . . . . ? C1 C2 C3 C5 -179.1(5) . . . . ? C1 N1 C6 C7 119.3(5) . . . . ? N2 N1 C6 C7 -64.0(6) . . . . ? C8 N3 C7 C6 113.0(6) . . . . ? N4 N3 C7 C6 -69.0(6) . . . . ? N1 C6 C7 N3 112.2(5) . . . . ? N4 N3 C8 C9 0.1(6) . . . . ? C7 N3 C8 C9 178.3(5) . . . . ? N4 N3 C8 C11 179.5(5) . . . . ? C7 N3 C8 C11 -2.4(9) . . . . ? N3 C8 C9 C10 -0.2(6) . . . . ? C11 C8 C9 C10 -179.5(6) . . . . ? N3 N4 C10 C9 -0.2(6) . . . . ? Cu1 N4 C10 C9 170.0(4) . . . . ? N3 N4 C10 C12 178.0(5) . . . . ? Cu1 N4 C10 C12 -11.8(8) . . . . ? C8 C9 C10 N4 0.2(7) . . . . ? C8 C9 C10 C12 -177.8(6) . . . . ? Cu2 N5 C13 Cu1 26(12) . . . . ? N2 Cu1 C13 N5 127(7) . . . . ? N4 Cu1 C13 N5 -51(7) . . . . ? Cu3 N6 C14 Cu2 -55(43) . . . . ? N5 Cu2 C14 N6 -61(18) . . . . ? Cu3 N7 C15 Cu3 178(3) . . . 4_586 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.550 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.122 #===END data_[(CuCN)2(dmpzpr)]n _database_code_depnum_ccdc_archive 'CCDC 762449' #TrackingRef '- JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H20 Cu2 N6' _chemical_formula_sum 'C15 H20 Cu2 N6' _chemical_formula_weight 411.47 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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.520(4) _cell_length_b 8.9518(18) _cell_length_c 22.506(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3529.8(12) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8381 _cell_measurement_theta_min 3.1318 _cell_measurement_theta_max 27.5010 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 2.417 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5309 _exptl_absorpt_correction_T_max 0.8119 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13161 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4006 _reflns_number_gt 2597 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0999P)^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 SHELXL _refine_ls_extinction_coef 0.0057(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4006 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1792 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.19026(3) 0.24833(6) 0.48775(3) 0.0418(2) Uani 1 1 d . . . Cu2 Cu 0.05973(3) 0.28224(7) 0.75246(3) 0.0428(2) Uani 1 1 d . . . N1 N 0.0359(2) 0.3339(4) 0.53330(16) 0.0375(8) Uani 1 1 d . . . N2 N 0.0738(2) 0.2676(4) 0.48744(16) 0.0370(8) Uani 1 1 d . . . N3 N 0.2141(2) 0.3616(4) 0.70283(17) 0.0367(8) Uani 1 1 d . . . N4 N 0.1757(2) 0.2895(4) 0.74740(17) 0.0357(8) Uani 1 1 d . . . N5 N 0.2416(2) 0.4381(5) 0.4900(2) 0.0501(10) Uani 1 1 d . . . N6 N -0.0151(2) -0.0216(5) 0.75686(18) 0.0513(11) Uani 1 1 d . . . C1 C -0.0385(3) 0.2894(5) 0.5352(2) 0.0427(11) Uani 1 1 d . . . C2 C -0.0486(3) 0.1948(6) 0.4880(2) 0.0463(12) Uani 1 1 d . . . H2 H -0.0942 0.1470 0.4770 0.056 Uiso 1 1 calc R . . C3 C 0.0224(3) 0.1827(5) 0.4591(2) 0.0397(10) Uani 1 1 d . . . C4 C -0.0916(3) 0.3413(7) 0.5824(2) 0.0615(15) Uani 1 1 d . . . H4A H -0.0727 0.3094 0.6209 0.092 Uiso 1 1 calc R . . H4B H -0.1418 0.2990 0.5757 0.092 Uiso 1 1 calc R . . H4C H -0.0948 0.4495 0.5815 0.092 Uiso 1 1 calc R . . C5 C 0.0448(3) 0.0960(6) 0.4053(2) 0.0533(13) Uani 1 1 d . . . H5A H 0.0448 0.1614 0.3709 0.080 Uiso 1 1 calc R . . H5B H 0.0086 0.0154 0.3990 0.080 Uiso 1 1 calc R . . H5C H 0.0955 0.0547 0.4109 0.080 Uiso 1 1 calc R . . C6 C 0.0770(3) 0.4294(5) 0.5745(2) 0.0396(10) Uani 1 1 d . . . H6A H 0.0405 0.4909 0.5966 0.047 Uiso 1 1 calc R . . H6B H 0.1106 0.4965 0.5521 0.047 Uiso 1 1 calc R . . C7 C 0.1247(2) 0.3392(5) 0.61825(19) 0.0375(10) Uani 1 1 d . . . H7A H 0.0910 0.2782 0.6431 0.045 Uiso 1 1 calc R . . H7B H 0.1587 0.2719 0.5964 0.045 Uiso 1 1 calc R . . C8 C 0.1719(2) 0.4422(5) 0.6574(2) 0.0387(10) Uani 1 1 d . . . H8A H 0.2080 0.4978 0.6325 0.046 Uiso 1 1 calc R . . H8B H 0.1380 0.5147 0.6766 0.046 Uiso 1 1 calc R . . C9 C 0.2904(3) 0.3353(6) 0.7065(2) 0.0432(11) Uani 1 1 d . . . C10 C 0.3017(3) 0.2474(6) 0.7558(2) 0.0472(13) Uani 1 1 d . . . H10 H 0.3485 0.2130 0.7708 0.057 Uiso 1 1 calc R . . C11 C 0.2292(3) 0.2196(5) 0.7789(2) 0.0392(10) Uani 1 1 d . . . C12 C 0.3462(3) 0.3973(7) 0.6622(3) 0.0643(16) Uani 1 1 d . . . H12A H 0.3430 0.5055 0.6621 0.097 Uiso 1 1 calc R . . H12B H 0.3340 0.3595 0.6229 0.097 Uiso 1 1 calc R . . H12C H 0.3975 0.3669 0.6730 0.097 Uiso 1 1 calc R . . C13 C 0.2074(3) 0.1297(6) 0.8331(2) 0.0583(14) Uani 1 1 d . . . H13A H 0.1553 0.0948 0.8290 0.087 Uiso 1 1 calc R . . H13B H 0.2116 0.1919 0.8682 0.087 Uiso 1 1 calc R . . H13C H 0.2414 0.0446 0.8368 0.087 Uiso 1 1 calc R . . C14 C 0.2695(3) 0.5534(5) 0.4899(2) 0.0397(10) Uani 1 1 d . . . C15 C 0.0132(3) 0.0935(5) 0.7586(2) 0.0433(11) 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 0.0395(4) 0.0400(3) 0.0460(4) -0.0032(3) 0.0011(2) 0.0013(2) Cu2 0.0391(4) 0.0416(4) 0.0477(4) 0.0006(2) 0.0071(3) -0.0016(2) N1 0.037(2) 0.0377(19) 0.038(2) -0.0016(16) -0.0019(16) 0.0082(16) N2 0.036(2) 0.037(2) 0.038(2) -0.0004(16) -0.0070(16) 0.0022(15) N3 0.0341(19) 0.0395(19) 0.0364(19) 0.0010(16) 0.0017(15) -0.0060(16) N4 0.032(2) 0.0382(19) 0.037(2) 0.0011(16) 0.0019(15) 0.0022(15) N5 0.039(2) 0.052(2) 0.059(3) -0.005(2) -0.0018(19) 0.0031(19) N6 0.044(2) 0.046(2) 0.064(3) -0.001(2) 0.011(2) -0.0040(19) C1 0.034(2) 0.047(3) 0.047(3) 0.012(2) -0.002(2) 0.008(2) C2 0.039(3) 0.049(3) 0.052(3) 0.008(2) -0.012(2) -0.009(2) C3 0.045(3) 0.038(2) 0.037(2) 0.0071(19) -0.010(2) -0.005(2) C4 0.042(3) 0.081(4) 0.062(3) 0.007(3) 0.007(2) 0.006(3) C5 0.064(3) 0.050(3) 0.046(3) -0.004(2) -0.009(2) -0.009(2) C6 0.043(3) 0.030(2) 0.046(3) -0.0019(19) 0.000(2) 0.0056(18) C7 0.038(2) 0.035(2) 0.040(2) 0.0006(19) -0.0020(19) -0.0011(18) C8 0.040(2) 0.038(2) 0.038(2) 0.0043(19) 0.0014(19) -0.0058(19) C9 0.032(2) 0.054(3) 0.044(3) -0.012(2) -0.0013(19) -0.002(2) C10 0.045(3) 0.057(3) 0.039(3) -0.014(2) -0.009(2) 0.014(2) C11 0.041(3) 0.041(2) 0.036(2) -0.0044(19) -0.0030(19) 0.009(2) C12 0.037(3) 0.093(4) 0.064(4) 0.005(3) 0.005(2) -0.015(3) C13 0.079(4) 0.050(3) 0.046(3) 0.010(2) -0.004(3) 0.004(3) C14 0.035(3) 0.033(2) 0.052(3) -0.002(2) -0.0031(19) -0.0033(19) C15 0.038(3) 0.040(2) 0.052(3) 0.003(2) 0.007(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 Cu1 C14 1.883(5) 8_655 ? Cu1 N5 1.923(5) . ? Cu1 N2 2.048(4) . ? Cu2 C15 1.881(5) . ? Cu2 N6 1.934(4) 3_556 ? Cu2 N4 2.036(4) . ? N1 N2 1.364(5) . ? N1 C1 1.364(6) . ? N1 C6 1.453(6) . ? N2 C3 1.339(6) . ? N3 C9 1.361(5) . ? N3 N4 1.369(5) . ? N3 C8 1.452(6) . ? N4 C11 1.331(6) . ? N5 C14 1.141(6) . ? N6 C15 1.144(6) . ? N6 Cu2 1.934(4) 3_546 ? C1 C2 1.370(8) . ? C1 C4 1.486(7) . ? C2 C3 1.408(7) . ? C2 H2 0.9400 . ? C3 C5 1.491(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.522(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.520(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.375(8) . ? C9 C12 1.502(7) . ? C10 C11 1.395(7) . ? C10 H10 0.9400 . ? C11 C13 1.510(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 Cu1 1.883(5) 8_665 ? 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 C14 Cu1 N5 130.0(2) 8_655 . ? C14 Cu1 N2 116.80(17) 8_655 . ? N5 Cu1 N2 113.09(16) . . ? C15 Cu2 N6 130.4(2) . 3_556 ? C15 Cu2 N4 117.74(18) . . ? N6 Cu2 N4 111.61(17) 3_556 . ? N2 N1 C1 111.2(4) . . ? N2 N1 C6 119.9(4) . . ? C1 N1 C6 128.8(4) . . ? C3 N2 N1 106.3(4) . . ? C3 N2 Cu1 128.6(3) . . ? N1 N2 Cu1 121.3(3) . . ? C9 N3 N4 110.9(4) . . ? C9 N3 C8 128.9(4) . . ? N4 N3 C8 120.0(3) . . ? C11 N4 N3 105.5(4) . . ? C11 N4 Cu2 131.1(3) . . ? N3 N4 Cu2 123.1(3) . . ? C14 N5 Cu1 177.0(4) . . ? C15 N6 Cu2 175.4(4) . 3_546 ? N1 C1 C2 106.2(4) . . ? N1 C1 C4 121.9(5) . . ? C2 C1 C4 131.9(5) . . ? C1 C2 C3 107.0(4) . . ? C1 C2 H2 126.5 . . ? C3 C2 H2 126.5 . . ? N2 C3 C2 109.3(4) . . ? N2 C3 C5 120.4(4) . . ? C2 C3 C5 130.3(4) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 111.9(3) . . ? N1 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N1 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 110.6(4) . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C7 112.5(4) . . ? N3 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? N3 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N3 C9 C10 106.8(4) . . ? N3 C9 C12 122.4(5) . . ? C10 C9 C12 130.8(5) . . ? C9 C10 C11 105.8(4) . . ? C9 C10 H10 127.1 . . ? C11 C10 H10 127.1 . . ? N4 C11 C10 111.0(4) . . ? N4 C11 C13 120.2(4) . . ? C10 C11 C13 128.8(4) . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 Cu1 176.4(5) . 8_665 ? N6 C15 Cu2 173.9(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 C1 N1 N2 C3 1.4(5) . . . . ? C6 N1 N2 C3 177.4(4) . . . . ? C1 N1 N2 Cu1 -158.3(3) . . . . ? C6 N1 N2 Cu1 17.7(5) . . . . ? C14 Cu1 N2 C3 -38.8(5) 8_655 . . . ? N5 Cu1 N2 C3 144.2(4) . . . . ? C14 Cu1 N2 N1 115.9(3) 8_655 . . . ? N5 Cu1 N2 N1 -61.1(4) . . . . ? C9 N3 N4 C11 0.5(5) . . . . ? C8 N3 N4 C11 176.1(4) . . . . ? C9 N3 N4 Cu2 -173.3(3) . . . . ? C8 N3 N4 Cu2 2.2(5) . . . . ? C15 Cu2 N4 C11 -46.2(5) . . . . ? N6 Cu2 N4 C11 138.8(4) 3_556 . . . ? C15 Cu2 N4 N3 126.0(3) . . . . ? N6 Cu2 N4 N3 -49.1(4) 3_556 . . . ? C14 Cu1 N5 C14 151(9) 8_655 . . . ? N2 Cu1 N5 C14 -32(9) . . . . ? N2 N1 C1 C2 -1.6(5) . . . . ? C6 N1 C1 C2 -177.2(4) . . . . ? N2 N1 C1 C4 177.7(4) . . . . ? C6 N1 C1 C4 2.2(7) . . . . ? N1 C1 C2 C3 1.2(5) . . . . ? C4 C1 C2 C3 -178.1(5) . . . . ? N1 N2 C3 C2 -0.6(5) . . . . ? Cu1 N2 C3 C2 157.1(3) . . . . ? N1 N2 C3 C5 178.7(4) . . . . ? Cu1 N2 C3 C5 -23.6(6) . . . . ? C1 C2 C3 N2 -0.4(5) . . . . ? C1 C2 C3 C5 -179.6(5) . . . . ? N2 N1 C6 C7 -76.0(5) . . . . ? C1 N1 C6 C7 99.2(5) . . . . ? N1 C6 C7 C8 175.4(4) . . . . ? C9 N3 C8 C7 108.2(5) . . . . ? N4 N3 C8 C7 -66.4(5) . . . . ? C6 C7 C8 N3 175.7(4) . . . . ? N4 N3 C9 C10 -1.7(5) . . . . ? C8 N3 C9 C10 -176.8(4) . . . . ? N4 N3 C9 C12 178.3(4) . . . . ? C8 N3 C9 C12 3.3(7) . . . . ? N3 C9 C10 C11 2.1(5) . . . . ? C12 C9 C10 C11 -177.9(5) . . . . ? N3 N4 C11 C10 0.8(5) . . . . ? Cu2 N4 C11 C10 174.0(3) . . . . ? N3 N4 C11 C13 178.9(4) . . . . ? Cu2 N4 C11 C13 -7.9(7) . . . . ? C9 C10 C11 N4 -1.9(6) . . . . ? C9 C10 C11 C13 -179.7(5) . . . . ? Cu1 N5 C14 Cu1 10(16) . . . 8_665 ? Cu2 N6 C15 Cu2 21(10) 3_546 . . . ? N6 Cu2 C15 N6 86(4) 3_556 . . . ? N4 Cu2 C15 N6 -88(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.786 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.151 #===END data_[(CuCN)2(dmpzh)]n _database_code_depnum_ccdc_archive 'CCDC 762450' #TrackingRef '- JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H26 Cu2 N6' _chemical_formula_sum 'C18 H26 Cu2 N6' _chemical_formula_weight 453.55 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6907(17) _cell_length_b 8.8881(18) _cell_length_c 14.374(3) _cell_angle_alpha 90.43(3) _cell_angle_beta 91.41(3) _cell_angle_gamma 109.99(3) _cell_volume 1042.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7286 _cell_measurement_theta_min 3.1505 _cell_measurement_theta_max 27.4739 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 2.052 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5780 _exptl_absorpt_correction_T_max 0.6844 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10071 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4704 _reflns_number_gt 3584 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0701P)^2^+2.9916P] 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_extinction_coef ? _refine_ls_number_reflns 4704 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1754 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 0.42613(8) 0.40228(8) 0.15891(4) 0.0413(2) Uani 1 1 d . . . Cu2 Cu -0.04363(9) 0.08431(8) 0.34093(4) 0.0468(2) Uani 1 1 d . . . N1 N 0.7574(5) 0.4915(4) 0.2653(3) 0.0298(8) Uani 1 1 d . . . N2 N 0.5993(5) 0.4921(4) 0.2630(2) 0.0296(8) Uani 1 1 d . . . N3 N -0.3501(5) -0.0579(5) 0.2231(3) 0.0320(8) Uani 1 1 d . . . N4 N -0.2824(5) 0.0290(5) 0.3005(3) 0.0327(8) Uani 1 1 d . . . N5 N 0.4850(6) 0.4750(6) 0.0369(3) 0.0445(11) Uani 0.50 1 d P . . N6 N 0.1197(7) 0.1990(7) 0.2568(4) 0.0575(13) Uani 1 1 d . . . N7 N -0.0133(8) 0.0212(7) 0.4639(4) 0.0660(18) Uani 0.50 1 d P . . C1 C 0.8423(6) 0.5726(6) 0.3390(3) 0.0392(11) Uani 1 1 d . . . C2 C 0.7402(7) 0.6295(6) 0.3888(3) 0.0411(12) Uani 1 1 d . . . H2 H 0.7654 0.6912 0.4441 0.049 Uiso 1 1 calc R . . C3 C 0.5915(6) 0.5760(6) 0.3394(3) 0.0359(11) Uani 1 1 d . . . C4 C 1.0204(7) 0.5897(9) 0.3581(5) 0.0614(17) Uani 1 1 d . . . H4A H 1.0310 0.4845 0.3581 0.092 Uiso 1 1 calc R . . H4B H 1.0562 0.6417 0.4182 0.092 Uiso 1 1 calc R . . H4C H 1.0876 0.6537 0.3100 0.092 Uiso 1 1 calc R . . C5 C 0.4364(8) 0.6008(8) 0.3635(4) 0.0518(14) Uani 1 1 d . . . H5A H 0.3511 0.5455 0.3180 0.078 Uiso 1 1 calc R . . H5B H 0.4528 0.7143 0.3634 0.078 Uiso 1 1 calc R . . H5C H 0.4041 0.5587 0.4248 0.078 Uiso 1 1 calc R . . C6 C 0.8112(6) 0.4118(5) 0.1903(3) 0.0322(10) Uani 1 1 d . . . H6A H 0.7159 0.3275 0.1626 0.039 Uiso 1 1 calc R . . H6B H 0.8860 0.3607 0.2162 0.039 Uiso 1 1 calc R . . C7 C 0.8970(6) 0.5258(5) 0.1148(3) 0.0305(9) Uani 1 1 d . . . H7A H 0.9887 0.6133 0.1430 0.037 Uiso 1 1 calc R . . H7B H 0.8202 0.5725 0.0865 0.037 Uiso 1 1 calc R . . C8 C 0.9609(6) 0.4444(5) 0.0394(3) 0.0327(10) Uani 1 1 d . . . H8A H 0.8701 0.3531 0.0137 0.039 Uiso 1 1 calc R . . H8B H 1.0420 0.4028 0.0672 0.039 Uiso 1 1 calc R . . C9 C -0.5085(7) -0.0663(7) 0.2093(4) 0.0424(12) Uani 1 1 d . . . C10 C -0.5406(8) 0.0184(7) 0.2829(4) 0.0512(14) Uani 1 1 d . . . H10 H -0.6405 0.0337 0.2939 0.061 Uiso 1 1 calc R . . C11 C -0.3998(8) 0.0758(6) 0.3369(4) 0.0455(13) Uani 1 1 d . . . C12 C -0.6121(8) -0.1577(10) 0.1305(5) 0.0687(19) Uani 1 1 d . . . H12A H -0.6266 -0.2703 0.1365 0.103 Uiso 1 1 calc R . . H12B H -0.5594 -0.1188 0.0725 0.103 Uiso 1 1 calc R . . H12C H -0.7180 -0.1439 0.1310 0.103 Uiso 1 1 calc R . . C13 C -0.3665(10) 0.1725(7) 0.4254(5) 0.068(2) Uani 1 1 d . . . H13A H -0.2981 0.1353 0.4670 0.103 Uiso 1 1 calc R . . H13B H -0.4692 0.1606 0.4547 0.103 Uiso 1 1 calc R . . H13C H -0.3105 0.2844 0.4117 0.103 Uiso 1 1 calc R . . C14 C -0.2533(6) -0.1210(6) 0.1629(3) 0.0325(10) Uani 1 1 d . . . H14A H -0.3251 -0.2207 0.1331 0.039 Uiso 1 1 calc R . . H14B H -0.1706 -0.1464 0.2009 0.039 Uiso 1 1 calc R . . C15 C -0.1685(6) -0.0046(5) 0.0881(3) 0.0318(10) Uani 1 1 d . . . H15A H -0.1099 0.1003 0.1170 0.038 Uiso 1 1 calc R . . H15B H -0.2511 0.0080 0.0442 0.038 Uiso 1 1 calc R . . C16 C -0.0476(6) -0.0610(5) 0.0350(3) 0.0348(10) Uani 1 1 d . . . H16A H 0.0296 -0.0818 0.0796 0.042 Uiso 1 1 calc R . . H16B H -0.1077 -0.1619 0.0022 0.042 Uiso 1 1 calc R . . C17 C 0.2292(6) 0.2731(7) 0.2140(3) 0.0397(11) Uani 1 1 d . . . C18 C -0.0133(8) 0.0212(7) 0.4639(4) 0.0660(18) Uani 0.50 1 d P . . C19 C 0.4850(6) 0.4750(6) 0.0369(3) 0.0445(11) Uani 0.50 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 Cu1 0.0386(4) 0.0502(4) 0.0333(3) 0.0023(3) 0.0020(3) 0.0128(3) Cu2 0.0467(4) 0.0495(4) 0.0333(3) 0.0049(3) -0.0040(3) 0.0029(3) N1 0.027(2) 0.0345(19) 0.0270(18) 0.0009(15) 0.0015(15) 0.0084(16) N2 0.0251(19) 0.035(2) 0.0279(18) 0.0021(15) 0.0038(15) 0.0098(16) N3 0.031(2) 0.037(2) 0.0289(18) 0.0024(16) -0.0005(15) 0.0122(17) N4 0.032(2) 0.035(2) 0.0271(18) 0.0053(15) 0.0107(16) 0.0050(16) N5 0.039(3) 0.057(3) 0.031(2) -0.001(2) 0.0012(19) 0.007(2) N6 0.055(3) 0.070(3) 0.047(3) 0.012(2) -0.008(2) 0.022(3) N7 0.072(4) 0.062(3) 0.033(2) 0.009(2) -0.014(3) -0.015(3) C1 0.034(3) 0.050(3) 0.031(2) -0.001(2) -0.0019(19) 0.011(2) C2 0.047(3) 0.042(3) 0.029(2) -0.006(2) 0.000(2) 0.009(2) C3 0.043(3) 0.036(2) 0.030(2) 0.0004(19) 0.008(2) 0.014(2) C4 0.035(3) 0.093(5) 0.053(3) -0.011(3) -0.011(3) 0.019(3) C5 0.053(4) 0.063(4) 0.049(3) -0.004(3) 0.017(3) 0.030(3) C6 0.031(2) 0.033(2) 0.032(2) 0.0078(18) 0.0126(19) 0.0093(19) C7 0.033(2) 0.029(2) 0.031(2) 0.0061(17) 0.0097(18) 0.0110(19) C8 0.039(3) 0.030(2) 0.033(2) 0.0064(18) 0.009(2) 0.016(2) C9 0.034(3) 0.051(3) 0.046(3) 0.010(2) 0.000(2) 0.019(2) C10 0.045(3) 0.057(3) 0.060(4) 0.013(3) 0.020(3) 0.028(3) C11 0.064(4) 0.033(2) 0.044(3) 0.007(2) 0.020(3) 0.021(3) C12 0.043(4) 0.104(6) 0.061(4) -0.001(4) -0.013(3) 0.029(4) C13 0.099(6) 0.046(3) 0.055(4) -0.005(3) 0.034(4) 0.016(3) C14 0.035(3) 0.036(2) 0.028(2) 0.0025(18) 0.0043(18) 0.014(2) C15 0.038(3) 0.034(2) 0.027(2) 0.0043(18) 0.0074(18) 0.017(2) C16 0.045(3) 0.033(2) 0.031(2) 0.0047(19) 0.011(2) 0.017(2) C17 0.025(2) 0.053(3) 0.036(2) 0.013(2) 0.003(2) 0.006(2) C18 0.072(4) 0.062(3) 0.033(2) 0.009(2) -0.014(3) -0.015(3) C19 0.039(3) 0.057(3) 0.031(2) -0.001(2) 0.0012(19) 0.007(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 N5 1.895(5) . ? Cu1 C17 1.900(5) . ? Cu1 N2 2.047(4) . ? Cu2 N7 1.897(5) . ? Cu2 N6 1.905(6) . ? Cu2 N4 2.031(4) . ? N1 C1 1.332(6) . ? N1 N2 1.375(5) . ? N1 C6 1.457(6) . ? N2 C3 1.338(6) . ? N3 N4 1.351(5) . ? N3 C9 1.362(6) . ? N3 C14 1.457(6) . ? N4 C11 1.343(7) . ? N5 C19 1.154(9) 2_665 ? N5 N5 1.154(9) 2_665 ? N6 C17 1.152(7) . ? N7 C18 1.153(10) 2_556 ? N7 N7 1.153(10) 2_556 ? C1 C2 1.374(7) . ? C1 C4 1.520(8) . ? C2 C3 1.389(7) . ? C2 H2 0.9400 . ? C3 C5 1.487(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.516(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.517(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C8 1.523(8) 2_765 ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.381(8) . ? C9 C12 1.479(9) . ? C10 C11 1.372(9) . ? C10 H10 0.9400 . ? C11 C13 1.495(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.519(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.526(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C16 1.523(9) 2 ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? 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 N5 Cu1 C17 134.6(2) . . ? N5 Cu1 N2 117.00(19) . . ? C17 Cu1 N2 108.10(18) . . ? N7 Cu2 N6 128.0(3) . . ? N7 Cu2 N4 113.8(2) . . ? N6 Cu2 N4 118.12(18) . . ? C1 N1 N2 111.5(4) . . ? C1 N1 C6 129.2(4) . . ? N2 N1 C6 119.3(4) . . ? C3 N2 N1 104.1(4) . . ? C3 N2 Cu1 128.9(3) . . ? N1 N2 Cu1 126.9(3) . . ? N4 N3 C9 111.3(4) . . ? N4 N3 C14 120.9(4) . . ? C9 N3 C14 127.7(4) . . ? C11 N4 N3 106.1(4) . . ? C11 N4 Cu2 129.9(4) . . ? N3 N4 Cu2 123.9(3) . . ? C19 N5 N5 0.0(6) 2_665 2_665 ? C19 N5 Cu1 175.9(7) 2_665 . ? N5 N5 Cu1 175.9(7) 2_665 . ? C17 N6 Cu2 172.9(5) . . ? C18 N7 N7 0.0(6) 2_556 2_556 ? C18 N7 Cu2 175.2(10) 2_556 . ? N7 N7 Cu2 175.2(10) 2_556 . ? N1 C1 C2 107.8(4) . . ? N1 C1 C4 122.1(5) . . ? C2 C1 C4 130.1(5) . . ? C1 C2 C3 104.9(4) . . ? C1 C2 H2 127.6 . . ? C3 C2 H2 127.6 . . ? N2 C3 C2 111.7(4) . . ? N2 C3 C5 120.7(5) . . ? C2 C3 C5 127.5(5) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 112.7(4) . . ? N1 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? N1 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C6 C7 C8 112.6(4) . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C7 C8 C8 113.1(5) . 2_765 ? C7 C8 H8A 109.0 . . ? C8 C8 H8A 109.0 2_765 . ? C7 C8 H8B 109.0 . . ? C8 C8 H8B 109.0 2_765 . ? H8A C8 H8B 107.8 . . ? N3 C9 C10 105.5(5) . . ? N3 C9 C12 122.2(5) . . ? C10 C9 C12 132.3(5) . . ? C11 C10 C9 107.3(5) . . ? C11 C10 H10 126.4 . . ? C9 C10 H10 126.4 . . ? N4 C11 C10 109.9(5) . . ? N4 C11 C13 120.1(6) . . ? C10 C11 C13 130.0(6) . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 112.7(4) . . ? N3 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? N3 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 112.1(4) . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C16 C16 C15 112.5(5) 2 . ? C16 C16 H16A 109.1 2 . ? C15 C16 H16A 109.1 . . ? C16 C16 H16B 109.1 2 . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N6 C17 Cu1 172.2(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.818 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.155 #===END