Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jing-Lin Zuo' _publ_contact_author_address ; Coordination Chemistry Institute Nanjing University Han Kou Road Nanjing Jiangsu 210093 CHINA ; _publ_contact_author_email ZUOJL@NJU.EDU.CN _publ_section_title ; Three-dimensional ferromagnet based on linkages of copper-azido clusters ; loop_ _publ_author_name 'Jing-Lin Zuo' 'Zhi-Guo Gu' 'Xiao-Zeng You' # Attachment 'complex2.cif' data_70112em _database_code_depnum_ccdc_archive 'CCDC 635762' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H21 Cu4.50 N31 O0.50' _chemical_formula_weight 821.47 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' O O 0.0106 0.0060 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.557(3) _cell_length_b 11.849(3) _cell_length_c 12.281(3) _cell_angle_alpha 105.264(4) _cell_angle_beta 101.508(4) _cell_angle_gamma 105.822(5) _cell_volume 1363.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2954 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 24.5 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.001 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 817 _exptl_absorpt_coefficient_mu 3.522 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4180 _exptl_absorpt_correction_T_max 0.4853 _exptl_absorpt_process_details 'SADABS; Bruker(2000)' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6853 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4717 _reflns_number_gt 3487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0663P)^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 4717 _refine_ls_number_parameters 397 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.097 _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 0.16056(9) 1.14660(7) 1.04443(7) 0.0352(3) Uani 1 1 d . . . Cu2 Cu 0.16942(9) 0.87803(7) 0.94806(7) 0.0301(2) Uani 1 1 d . . . Cu3 Cu 0.21818(9) 0.60861(8) 0.90330(8) 0.0353(3) Uani 1 1 d . C . Cu4 Cu 0.49707(9) 0.86163(7) 0.95186(7) 0.0317(2) Uani 1 1 d . . . Cu5 Cu 0.5000 1.0000 0.5000 0.0511(4) Uani 1 2 d SU . . C1 C 0.0198(8) 0.4423(7) 0.6892(7) 0.051(2) Uani 1 1 d . . . H1A H -0.0712 0.3814 0.6549 0.062 Uiso 1 1 d R A 3 C2 C 0.1154(9) 0.3765(7) 0.7190(7) 0.058(2) Uani 1 1 d D C . H2A H 0.1236 0.3239 0.6485 0.069 Uiso 1 1 d R B 4 H2B H 0.0818 0.3255 0.7633 0.069 Uiso 1 1 d R B 4 C3 C 0.130(2) 0.2978(18) 0.6080(12) 0.076(7) Uani 0.445(13) 1 d PDU C 1 H3A H 0.0491 0.2250 0.5701 0.114 Uiso 0.445(13) 1 calc PR C 1 H3B H 0.2091 0.2731 0.6270 0.114 Uiso 0.445(13) 1 calc PR C 1 H3C H 0.1424 0.3450 0.5558 0.114 Uiso 0.445(13) 1 calc PR C 1 C3' C 0.053(2) 0.4971(17) 0.5956(13) 0.080(7) Uani 0.555(13) 1 d P C 2 H3'1 H 0.1461 0.5532 0.6236 0.121 Uiso 0.555(13) 1 calc PR C 2 H3'2 H -0.0082 0.5415 0.5786 0.121 Uiso 0.555(13) 1 calc PR C 2 H3'3 H 0.0407 0.4312 0.5251 0.121 Uiso 0.555(13) 1 calc PR C 2 C4 C 0.4383(10) 0.7399(10) 0.4248(10) 0.0854(15) Uani 1 1 d DU . . H4 H 0.4575 0.7486 0.5086 0.102 Uiso 1 1 d R . . C5 C 0.5852(10) 0.7897(11) 0.4521(12) 0.110(4) Uani 1 1 d D . . H5A H 0.5942 0.7520 0.3750 0.132 Uiso 1 1 d R . . H5B H 0.6353 0.7603 0.5072 0.132 Uiso 1 1 d R . . C6 C 0.3645(12) 0.6031(9) 0.3972(13) 0.120(5) Uani 1 1 d . . . H6A H 0.3045 0.5789 0.3190 0.179 Uiso 1 1 d R . . H6B H 0.3107 0.5880 0.4497 0.179 Uiso 1 1 d R . . H6C H 0.4248 0.5553 0.3968 0.179 Uiso 1 1 d R . . N1 N 0.1810(8) 1.2747(6) 0.9713(6) 0.059(2) Uani 1 1 d . . . N2 N 0.1812(6) 1.3775(6) 1.0056(6) 0.0440(16) Uani 1 1 d . . . N3 N 0.1806(7) 1.4796(6) 1.0317(6) 0.0534(18) Uani 1 1 d . . . N4 N 0.1274(6) 0.9866(5) 1.0817(5) 0.0327(14) Uani 1 1 d . . . N5 N 0.1255(6) 0.9837(6) 1.1774(6) 0.0387(15) Uani 1 1 d . . . N6 N 0.1193(9) 0.9811(8) 1.2678(7) 0.079(3) Uani 1 1 d . . . N7 N 0.2013(7) 1.0360(5) 0.9119(5) 0.0412(16) Uani 1 1 d . . . N8 N 0.2252(6) 1.0595(6) 0.8264(5) 0.0406(15) Uani 1 1 d . . . N9 N 0.2525(10) 1.0863(7) 0.7512(7) 0.079(3) Uani 1 1 d . . . N10 N 0.1681(6) 0.7392(5) 1.0101(5) 0.0357(14) Uani 1 1 d . . . N11 N 0.1635(6) 0.7355(5) 1.1042(6) 0.0366(14) Uani 1 1 d . . . N12 N 0.1571(8) 0.7278(6) 1.1940(6) 0.063(2) Uani 1 1 d . . . N13 N 0.2460(6) 0.7925(5) 0.8280(5) 0.0361(14) Uani 1 1 d . . . N14 N 0.2301(6) 0.7937(6) 0.7294(6) 0.0412(15) Uani 1 1 d . . . N15 N 0.2185(10) 0.7924(9) 0.6377(7) 0.090(3) Uani 1 1 d . . . N16 N 0.4194(6) 0.7062(5) 0.9856(5) 0.0375(14) Uani 1 1 d . . . N17 N 0.4827(6) 0.6694(6) 1.0528(6) 0.0473(16) Uani 1 1 d . . . N18 N 0.5362(9) 0.6366(9) 1.1202(9) 0.100(3) Uani 1 1 d . . . N19 N 0.0220(6) 0.5292(5) 0.8020(5) 0.0392(15) Uani 1 1 d . C . H19A H -0.0300 0.4875 0.8383 0.047 Uiso 1 1 calc R . . H19B H -0.0118 0.5878 0.7883 0.047 Uiso 1 1 calc R . . N20 N 0.2526(7) 0.4717(5) 0.7894(5) 0.0483(17) Uani 1 1 d . . . H20A H 0.2966 0.5018 0.7420 0.058 Uiso 1 1 calc R C . H20B H 0.3047 0.4381 0.8288 0.058 Uiso 1 1 calc R . . N21 N 0.5355(6) 1.0218(5) 0.9137(5) 0.0372(14) Uani 1 1 d . . . N22 N 0.5475(6) 1.0283(5) 0.8203(5) 0.0339(13) Uani 1 1 d . . . N23 N 0.5613(8) 1.0327(7) 0.7333(6) 0.060(2) Uani 1 1 d . . . N24 N 0.5872(7) 0.7922(6) 0.8394(6) 0.0460(16) Uani 1 1 d . . . N25 N 0.5252(8) 0.6963(7) 0.7656(7) 0.059(2) Uani 1 1 d . . . N26 N 0.4669(11) 0.6036(9) 0.6933(9) 0.116(4) Uani 1 1 d . . . N27 N 0.3673(7) 0.8263(6) 0.4517(6) 0.0567(13) Uani 1 1 d U . . H27A H 0.3313 0.8167 0.5106 0.068 Uiso 1 1 calc R . . H27B H 0.2980 0.8117 0.3878 0.068 Uiso 1 1 calc R . . N28 N 0.6456(7) 0.9224(7) 0.4848(6) 0.0607(19) Uani 1 1 d . . . H28A H 0.6836 0.9413 0.4296 0.073 Uiso 1 1 calc R . . H28B H 0.7125 0.9526 0.5539 0.073 Uiso 1 1 calc R . . O1W O 0.915(4) 0.073(3) 0.509(2) 0.30(2) Uani 0.50 1 d P . . H1WA H 0.9591 0.0310 0.5340 0.361 Uiso 0.50 1 d PR . . H1WB H 0.9153 0.0593 0.4375 0.361 Uiso 0.50 1 d PR . . N31 N 0.0800(7) 1.2237(6) 1.1616(6) 0.0423(16) Uani 1 1 d . . . N30 N 0.1279(9) 1.2531(7) 1.2599(7) 0.071(2) Uani 1 1 d . . . N29 N 0.1750(14) 1.2830(12) 1.3595(12) 0.143(5) Uani 1 1 d U . . 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(6) 0.0295(5) 0.0446(5) 0.0209(4) 0.0251(5) 0.0230(4) Cu2 0.0437(5) 0.0277(5) 0.0330(5) 0.0178(4) 0.0201(4) 0.0201(4) Cu3 0.0365(5) 0.0298(5) 0.0457(5) 0.0159(4) 0.0137(4) 0.0165(4) Cu4 0.0408(5) 0.0279(5) 0.0357(5) 0.0163(4) 0.0178(4) 0.0161(4) Cu5 0.0413(9) 0.0740(10) 0.0411(8) 0.0240(7) 0.0165(7) 0.0172(7) C1 0.045(5) 0.046(5) 0.062(5) 0.029(4) 0.009(4) 0.010(4) C2 0.074(7) 0.043(5) 0.057(5) 0.015(4) 0.021(5) 0.021(5) C3 0.076(7) 0.076(7) 0.076(7) 0.025(3) 0.022(2) 0.027(3) C3' 0.135(19) 0.077(13) 0.049(10) 0.032(10) 0.032(11) 0.053(13) C4 0.0860(19) 0.0812(13) 0.0891(19) 0.0270(11) 0.0244(11) 0.0314(11) C5 0.078(9) 0.107(10) 0.158(12) 0.054(10) 0.030(9) 0.047(8) C6 0.094(10) 0.068(8) 0.203(15) 0.050(9) 0.042(10) 0.035(7) N1 0.112(7) 0.039(4) 0.070(5) 0.040(4) 0.060(5) 0.048(4) N2 0.051(4) 0.047(4) 0.057(4) 0.034(3) 0.029(3) 0.025(3) N3 0.071(5) 0.032(4) 0.069(5) 0.024(4) 0.029(4) 0.025(4) N4 0.050(4) 0.033(3) 0.033(3) 0.020(3) 0.023(3) 0.025(3) N5 0.047(4) 0.043(4) 0.037(4) 0.018(3) 0.016(3) 0.024(3) N6 0.121(8) 0.101(7) 0.064(5) 0.051(5) 0.051(5) 0.070(6) N7 0.069(5) 0.035(3) 0.047(4) 0.028(3) 0.038(3) 0.033(3) N8 0.053(4) 0.040(4) 0.045(4) 0.025(3) 0.024(3) 0.025(3) N9 0.133(8) 0.074(6) 0.065(5) 0.045(5) 0.062(6) 0.045(5) N10 0.050(4) 0.035(3) 0.040(3) 0.026(3) 0.021(3) 0.023(3) N11 0.040(4) 0.023(3) 0.050(4) 0.020(3) 0.012(3) 0.009(3) N12 0.098(6) 0.050(4) 0.050(4) 0.031(4) 0.025(4) 0.024(4) N13 0.050(4) 0.035(3) 0.038(4) 0.017(3) 0.025(3) 0.024(3) N14 0.042(4) 0.050(4) 0.033(4) 0.014(3) 0.018(3) 0.014(3) N15 0.107(8) 0.125(8) 0.048(5) 0.030(5) 0.030(5) 0.048(6) N16 0.041(4) 0.030(3) 0.051(4) 0.024(3) 0.014(3) 0.016(3) N17 0.037(4) 0.046(4) 0.066(5) 0.027(4) 0.015(3) 0.016(3) N18 0.070(6) 0.123(8) 0.130(8) 0.101(7) 0.009(6) 0.027(6) N19 0.036(4) 0.034(3) 0.044(4) 0.016(3) 0.003(3) 0.010(3) N20 0.055(4) 0.038(4) 0.052(4) 0.007(3) 0.014(3) 0.023(3) N21 0.053(4) 0.035(3) 0.038(4) 0.020(3) 0.025(3) 0.019(3) N22 0.029(3) 0.034(3) 0.036(4) 0.016(3) 0.008(3) 0.006(3) N23 0.077(6) 0.075(5) 0.043(4) 0.031(4) 0.031(4) 0.029(4) N24 0.049(4) 0.039(4) 0.058(4) 0.012(4) 0.031(4) 0.021(3) N25 0.067(5) 0.050(5) 0.060(5) 0.005(4) 0.037(4) 0.018(4) N26 0.122(9) 0.084(7) 0.099(8) -0.014(6) 0.066(7) -0.008(6) N27 0.052(4) 0.075(2) 0.043(4) 0.028(3) 0.015(3) 0.0140(16) N28 0.058(5) 0.079(6) 0.053(4) 0.027(4) 0.020(4) 0.028(4) O1W 0.46(6) 0.24(3) 0.101(17) 0.07(2) 0.04(3) -0.01(3) N31 0.058(4) 0.048(4) 0.036(4) 0.017(3) 0.021(3) 0.032(3) N30 0.101(7) 0.072(6) 0.052(5) 0.018(5) 0.029(5) 0.046(5) N29 0.143(5) 0.143(5) 0.142(5) 0.0477(18) 0.0412(17) 0.0497(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.943(6) . ? Cu1 N31 1.962(6) . ? Cu1 N7 2.004(6) . ? Cu1 N4 2.021(5) . ? Cu2 N10 1.985(5) . ? Cu2 N7 1.992(5) . ? Cu2 N13 1.998(5) . ? Cu2 N4 2.009(5) . ? Cu3 N19 2.004(6) . ? Cu3 N10 2.012(6) . ? Cu3 N20 2.012(5) . ? Cu3 N16 2.015(6) . ? Cu4 N24 1.960(6) . ? Cu4 N16 1.987(6) . ? Cu4 N21 2.009(6) 2_677 ? Cu4 N21 2.028(6) . ? Cu5 N27 2.001(7) 2_676 ? Cu5 N27 2.001(7) . ? Cu5 N28 2.010(7) . ? Cu5 N28 2.010(7) 2_676 ? C1 C2 1.481(10) . ? C1 N19 1.484(9) . ? C1 C3' 1.514(16) . ? C1 H1A 0.9600 . ? C2 N20 1.488(10) . ? C2 C3 1.5000(11) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C3 H2A 0.5413 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3' H3'1 0.9600 . ? C3' H3'2 0.9600 . ? C3' H3'3 0.9600 . ? C4 C5 1.434(5) . ? C4 N27 1.434(11) . ? C4 C6 1.506(13) . ? C4 H4 0.9799 . ? C5 N28 1.435(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9601 . ? N1 N2 1.179(8) . ? N2 N3 1.169(8) . ? N4 N5 1.190(8) . ? N5 N6 1.132(8) . ? N7 N8 1.210(8) . ? N8 N9 1.117(8) . ? N10 N11 1.178(8) . ? N11 N12 1.144(8) . ? N13 N14 1.193(8) . ? N14 N15 1.105(9) . ? N16 N17 1.203(8) . ? N17 N18 1.122(9) . ? N19 H19A 0.9000 . ? N19 H19B 0.9000 . ? N20 H20A 0.9000 . ? N20 H20B 0.9000 . ? N21 N22 1.198(8) . ? N21 Cu4 2.009(6) 2_677 ? N22 N23 1.119(8) . ? N24 N25 1.165(9) . ? N25 N26 1.128(10) . ? N27 H27A 0.9000 . ? N27 H27B 0.9000 . ? N28 H28A 0.9000 . ? N28 H28B 0.9000 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? N31 N30 1.129(9) . ? N30 N29 1.140(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N31 95.5(3) . . ? N1 Cu1 N7 90.7(2) . . ? N31 Cu1 N7 166.9(3) . . ? N1 Cu1 N4 166.7(3) . . ? N31 Cu1 N4 94.9(2) . . ? N7 Cu1 N4 77.5(2) . . ? N10 Cu2 N7 169.3(3) . . ? N10 Cu2 N13 85.2(2) . . ? N7 Cu2 N13 97.4(2) . . ? N10 Cu2 N4 97.7(2) . . ? N7 Cu2 N4 78.0(2) . . ? N13 Cu2 N4 169.6(2) . . ? N19 Cu3 N10 90.2(2) . . ? N19 Cu3 N20 85.4(3) . . ? N10 Cu3 N20 175.5(3) . . ? N19 Cu3 N16 169.7(2) . . ? N10 Cu3 N16 89.9(2) . . ? N20 Cu3 N16 94.5(3) . . ? N24 Cu4 N16 96.3(2) . . ? N24 Cu4 N21 161.2(3) . 2_677 ? N16 Cu4 N21 97.1(2) . 2_677 ? N24 Cu4 N21 92.0(2) . . ? N16 Cu4 N21 167.8(2) . . ? N21 Cu4 N21 77.1(2) 2_677 . ? N27 Cu5 N27 180.000(1) 2_676 . ? N27 Cu5 N28 93.5(3) 2_676 . ? N27 Cu5 N28 86.5(3) . . ? N27 Cu5 N28 86.5(3) 2_676 2_676 ? N27 Cu5 N28 93.5(3) . 2_676 ? N28 Cu5 N28 180.000(3) . 2_676 ? C2 C1 N19 107.1(6) . . ? C2 C1 C3' 110.2(10) . . ? N19 C1 C3' 117.4(8) . . ? C2 C1 H1A 107.6 . . ? N19 C1 H1A 107.6 . . ? C3' C1 H1A 106.6 . . ? C1 C2 N20 108.1(6) . . ? C1 C2 C3 109.7(10) . . ? N20 C2 C3 108.3(11) . . ? C1 C2 H2A 110.5 . . ? N20 C2 H2A 109.4 . . ? C3 C2 H2A 1.8 . . ? C1 C2 H2B 110.1 . . ? N20 C2 H2B 110.4 . . ? C3 C2 H2B 110.1 . . ? H2A C2 H2B 108.3 . . ? C2 C3 H2A 3.2 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? C1 C3' H3'1 109.5 . . ? C1 C3' H3'2 109.5 . . ? H3'1 C3' H3'2 109.5 . . ? C1 C3' H3'3 109.5 . . ? H3'1 C3' H3'3 109.5 . . ? H3'2 C3' H3'3 109.5 . . ? C5 C4 N27 117.6(9) . . ? C5 C4 C6 121.1(10) . . ? N27 C4 C6 119.7(9) . . ? C5 C4 H4 84.2 . . ? N27 C4 H4 85.4 . . ? C6 C4 H4 87.7 . . ? C4 C5 N28 116.5(9) . . ? C4 C5 H5A 98.8 . . ? N28 C5 H5A 108.1 . . ? C4 C5 H5B 114.9 . . ? N28 C5 H5B 110.0 . . ? H5A C5 H5B 107.5 . . ? C4 C6 H6A 102.5 . . ? C4 C6 H6B 112.2 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 113.4 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 N1 Cu1 130.9(5) . . ? N3 N2 N1 175.2(8) . . ? N5 N4 Cu2 132.8(4) . . ? N5 N4 Cu1 122.0(5) . . ? Cu2 N4 Cu1 101.7(2) . . ? N6 N5 N4 177.6(8) . . ? N8 N7 Cu2 130.3(5) . . ? N8 N7 Cu1 126.4(5) . . ? Cu2 N7 Cu1 102.9(3) . . ? N9 N8 N7 176.6(9) . . ? N11 N10 Cu2 128.4(5) . . ? N11 N10 Cu3 119.5(4) . . ? Cu2 N10 Cu3 111.0(3) . . ? N12 N11 N10 177.8(8) . . ? N14 N13 Cu2 126.4(5) . . ? N15 N14 N13 177.5(8) . . ? N17 N16 Cu4 124.8(5) . . ? N17 N16 Cu3 118.9(5) . . ? Cu4 N16 Cu3 116.3(3) . . ? N18 N17 N16 175.3(9) . . ? C1 N19 Cu3 107.5(5) . . ? C1 N19 H19A 110.2 . . ? Cu3 N19 H19A 110.2 . . ? C1 N19 H19B 110.2 . . ? Cu3 N19 H19B 110.2 . . ? H19A N19 H19B 108.5 . . ? C2 N20 Cu3 106.7(5) . . ? C2 N20 H20A 110.4 . . ? Cu3 N20 H20A 110.4 . . ? C2 N20 H20B 110.4 . . ? Cu3 N20 H20B 110.4 . . ? H20A N20 H20B 108.6 . . ? N22 N21 Cu4 131.9(5) . 2_677 ? N22 N21 Cu4 123.7(5) . . ? Cu4 N21 Cu4 102.9(2) 2_677 . ? N23 N22 N21 178.0(7) . . ? N25 N24 Cu4 118.6(6) . . ? N26 N25 N24 178.8(9) . . ? C4 N27 Cu5 109.1(6) . . ? C4 N27 H27A 109.9 . . ? Cu5 N27 H27A 109.9 . . ? C4 N27 H27B 109.9 . . ? Cu5 N27 H27B 109.9 . . ? H27A N27 H27B 108.3 . . ? C5 N28 Cu5 109.5(6) . . ? C5 N28 H28A 109.8 . . ? Cu5 N28 H28A 109.8 . . ? C5 N28 H28B 109.8 . . ? Cu5 N28 H28B 109.8 . . ? H28A N28 H28B 108.2 . . ? H1WA O1W H1WB 104.5 . . ? N30 N31 Cu1 123.4(6) . . ? N31 N30 N29 179.3(12) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.008 _refine_diff_density_min -1.387 _refine_diff_density_rms 0.118 data_70307am _database_code_depnum_ccdc_archive 'CCDC 641324' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 Cu3 N20' _chemical_formula_weight 530.96 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 P2(1)/c 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 8.6023(10) _cell_length_b 12.4861(14) _cell_length_c 16.2429(19) _cell_angle_alpha 90.00 _cell_angle_beta 99.411(2) _cell_angle_gamma 90.00 _cell_volume 1721.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1253 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 21.7 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 3.715 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4569 _exptl_absorpt_correction_T_max 0.4820 _exptl_absorpt_process_details 'SADABS; Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8993 _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.11 _reflns_number_total 3399 _reflns_number_gt 3090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0598P)^2^+2.7299P] 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 3399 _refine_ls_number_parameters 244 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.104 _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 0.54146(6) 0.87731(4) 0.24323(3) 0.03059(17) Uani 1 1 d . . . Cu2 Cu 0.66347(6) 0.98124(4) 0.08278(3) 0.02818(16) Uani 1 1 d . . . Cu3 Cu 0.73236(6) 1.04070(4) -0.09227(3) 0.02933(17) Uani 1 1 d . . . C1 C 0.5274(8) 1.0155(5) 0.3782(4) 0.0569(15) Uani 1 1 d . . . H1A H 0.4864 1.0312 0.4291 0.068 Uiso 1 1 calc R . . H1B H 0.5382 1.0826 0.3495 0.068 Uiso 1 1 calc R . . C2 C 0.6837(8) 0.9630(5) 0.3991(3) 0.0581(15) Uani 1 1 d . . . H2A H 0.7592 1.0122 0.4296 0.070 Uiso 1 1 calc R . . H2B H 0.6760 0.9006 0.4338 0.070 Uiso 1 1 calc R . . C3 C 0.8708(7) 0.8567(6) 0.3360(4) 0.0662(17) Uani 1 1 d . . . H3A H 0.8941 0.8325 0.2826 0.079 Uiso 1 1 calc R . . H3B H 0.8413 0.7945 0.3657 0.079 Uiso 1 1 calc R . . C4 C 1.0163(8) 0.9047(8) 0.3848(6) 0.102(3) Uani 1 1 d . . . H4A H 1.0315 0.9754 0.3642 0.153 Uiso 1 1 calc R . . H4B H 1.1056 0.8609 0.3789 0.153 Uiso 1 1 calc R . . H4C H 1.0056 0.9087 0.4426 0.153 Uiso 1 1 calc R . . N1 N 0.7354(5) 0.9309(4) 0.3210(3) 0.0410(9) Uani 1 1 d . . . H1 H 0.7686 0.9912 0.2977 0.049 Uiso 1 1 calc R . . N2 N 0.4183(5) 0.9454(3) 0.3251(2) 0.0396(9) Uani 1 1 d . . . H2C H 0.3368 0.9833 0.2979 0.047 Uiso 1 1 calc R . . H2D H 0.3804 0.8948 0.3560 0.047 Uiso 1 1 calc R . . N3 N 0.6684(5) 0.8491(3) 0.1510(2) 0.0389(9) Uani 1 1 d . . . N4 N 0.7151(5) 0.7632(3) 0.1333(3) 0.0411(9) Uani 1 1 d . . . N5 N 0.7598(7) 0.6826(4) 0.1169(5) 0.0781(18) Uani 1 1 d . . . N6 N 0.5181(4) 1.0389(3) 0.1554(2) 0.0300(8) Uani 1 1 d . . . N7 N 0.4897(4) 1.1283(3) 0.1726(2) 0.0307(8) Uani 1 1 d . . . N8 N 0.4523(6) 1.2116(4) 0.1902(4) 0.0607(13) Uani 1 1 d . . . N9 N 0.7767(5) 0.9233(3) -0.0063(2) 0.0357(8) Uani 1 1 d . . . N10 N 0.8996(4) 0.8767(3) 0.0082(2) 0.0340(8) Uani 1 1 d . . . N11 N 1.0147(6) 0.8327(5) 0.0225(4) 0.0681(15) Uani 1 1 d . . . N12 N 0.6261(5) 1.0980(3) -0.0015(2) 0.0329(8) Uani 1 1 d . . . N13 N 0.6205(5) 1.1930(3) 0.0137(2) 0.0354(8) Uani 1 1 d . . . N14 N 0.6127(8) 1.2822(4) 0.0245(3) 0.0664(15) Uani 1 1 d . . . N15 N 0.8415(5) 0.9729(4) -0.1756(3) 0.0469(11) Uani 1 1 d . . . N16 N 0.9788(4) 0.9604(3) -0.1676(2) 0.0358(9) Uani 1 1 d . . . N17 N 1.1095(6) 0.9463(5) -0.1642(4) 0.0737(17) Uani 1 1 d . . . N18 N 0.6600(5) 1.1639(3) -0.1667(2) 0.0394(8) Uani 1 1 d U . . N19 N 0.7458(6) 1.2325(4) -0.1807(3) 0.0568(12) Uani 1 1 d U . . N20 N 0.8234(9) 1.3015(6) -0.1913(6) 0.110(2) Uani 1 1 d U . . 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 0.0300(3) 0.0360(3) 0.0260(3) 0.0024(2) 0.0053(2) 0.0021(2) Cu2 0.0299(3) 0.0300(3) 0.0263(3) 0.00321(19) 0.0096(2) 0.0052(2) Cu3 0.0298(3) 0.0345(3) 0.0243(3) 0.00106(19) 0.0065(2) 0.0018(2) C1 0.069(4) 0.065(4) 0.037(3) -0.012(3) 0.008(3) 0.011(3) C2 0.062(4) 0.076(4) 0.032(3) -0.006(3) -0.006(2) -0.006(3) C3 0.043(3) 0.085(5) 0.066(4) 0.013(3) -0.005(3) 0.011(3) C4 0.046(4) 0.147(8) 0.102(6) 0.027(6) -0.020(4) -0.005(5) N1 0.033(2) 0.053(2) 0.036(2) 0.0049(19) -0.0003(16) -0.0012(18) N2 0.042(2) 0.046(2) 0.031(2) 0.0008(17) 0.0100(17) 0.0050(18) N3 0.046(2) 0.038(2) 0.036(2) 0.0064(17) 0.0146(17) 0.0099(18) N4 0.039(2) 0.036(2) 0.052(3) 0.0036(18) 0.0175(19) 0.0031(18) N5 0.077(4) 0.043(3) 0.122(5) -0.005(3) 0.041(4) 0.010(3) N6 0.0315(19) 0.0271(18) 0.0338(19) 0.0022(14) 0.0122(15) 0.0018(14) N7 0.0284(18) 0.035(2) 0.0286(18) -0.0033(15) 0.0038(14) -0.0029(15) N8 0.063(3) 0.041(3) 0.079(4) -0.025(2) 0.013(3) 0.001(2) N9 0.039(2) 0.040(2) 0.0293(18) 0.0050(16) 0.0102(15) 0.0106(18) N10 0.032(2) 0.039(2) 0.0328(19) 0.0023(16) 0.0098(15) 0.0034(17) N11 0.047(3) 0.086(4) 0.074(4) 0.023(3) 0.017(3) 0.023(3) N12 0.041(2) 0.0302(19) 0.0288(18) 0.0026(15) 0.0091(15) 0.0046(16) N13 0.042(2) 0.037(2) 0.0279(18) -0.0007(15) 0.0089(16) 0.0011(17) N14 0.106(5) 0.040(3) 0.056(3) -0.005(2) 0.022(3) 0.005(3) N15 0.036(2) 0.073(3) 0.032(2) -0.009(2) 0.0075(17) 0.004(2) N16 0.032(2) 0.048(2) 0.0288(19) -0.0085(16) 0.0089(15) -0.0044(17) N17 0.037(3) 0.118(5) 0.065(3) -0.039(3) 0.004(2) 0.000(3) N18 0.0402(19) 0.0414(19) 0.0341(18) 0.0068(16) -0.0012(15) -0.0030(14) N19 0.049(2) 0.054(2) 0.064(3) 0.022(2) 0.000(2) -0.0091(17) N20 0.098(4) 0.100(4) 0.128(4) 0.042(3) 0.007(3) -0.050(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.019(4) . ? Cu1 N3 2.023(4) . ? Cu1 N18 2.027(4) 3_675 ? Cu1 N1 2.034(4) . ? Cu1 N8 2.330(5) 2_645 ? Cu1 N6 2.461(4) . ? Cu2 N3 1.984(4) . ? Cu2 N6 1.988(4) . ? Cu2 N12 1.990(4) . ? Cu2 N9 2.006(4) . ? Cu2 N17 2.353(5) 3_775 ? Cu3 N15 1.961(4) . ? Cu3 N12 1.991(4) . ? Cu3 N18 1.992(4) . ? Cu3 N9 2.018(4) . ? Cu3 N6 2.441(4) 3_675 ? C1 N2 1.458(7) . ? C1 C2 1.484(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N1 1.467(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.477(7) . ? C3 C4 1.494(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? N1 H1 0.9100 . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 N4 1.197(6) . ? N4 N5 1.124(6) . ? N6 N7 1.185(5) . ? N6 Cu3 2.441(4) 3_675 ? N7 N8 1.140(6) . ? N8 Cu1 2.330(4) 2_655 ? N9 N10 1.196(5) . ? N10 N11 1.123(6) . ? N12 N13 1.213(5) . ? N13 N14 1.131(6) . ? N15 N16 1.177(6) . ? N16 N17 1.131(6) . ? N17 Cu2 2.353(5) 3_775 ? N18 N19 1.177(6) . ? N18 Cu1 2.027(4) 3_675 ? N19 N20 1.120(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 N2 Cu1 N3 164.97(17) . . ? N2 Cu1 N18 91.32(17) . 3_675 ? N3 Cu1 N18 90.72(18) . 3_675 ? N2 Cu1 N1 85.27(17) . . ? N3 Cu1 N1 91.72(17) . . ? N18 Cu1 N1 175.20(17) 3_675 . ? N2 Cu1 N8 92.47(19) . 2_645 ? N3 Cu1 N8 102.40(18) . 2_645 ? N18 Cu1 N8 90.66(18) 3_675 2_645 ? N1 Cu1 N8 92.85(18) . 2_645 ? N2 Cu1 N6 92.01(15) . . ? N3 Cu1 N6 73.49(14) . . ? N18 Cu1 N6 82.64(14) 3_675 . ? N1 Cu1 N6 94.09(15) . . ? N8 Cu1 N6 172.03(17) 2_645 . ? N3 Cu2 N6 85.86(15) . . ? N3 Cu2 N12 168.51(17) . . ? N6 Cu2 N12 95.48(15) . . ? N3 Cu2 N9 97.74(16) . . ? N6 Cu2 N9 169.91(15) . . ? N12 Cu2 N9 79.13(15) . . ? N3 Cu2 N17 93.8(2) . 3_775 ? N6 Cu2 N17 94.13(17) . 3_775 ? N12 Cu2 N17 97.5(2) . 3_775 ? N9 Cu2 N17 95.03(17) . 3_775 ? N15 Cu3 N12 174.90(18) . . ? N15 Cu3 N18 93.00(19) . . ? N12 Cu3 N18 92.07(17) . . ? N15 Cu3 N9 96.08(18) . . ? N12 Cu3 N9 78.82(15) . . ? N18 Cu3 N9 170.39(16) . . ? N15 Cu3 N6 91.37(15) . 3_675 ? N12 Cu3 N6 88.66(14) . 3_675 ? N18 Cu3 N6 83.85(14) . 3_675 ? N9 Cu3 N6 92.79(14) . 3_675 ? N2 C1 C2 109.9(5) . . ? N2 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N2 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N1 C2 C1 108.3(4) . . ? N1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? N1 C3 C4 114.0(6) . . ? N1 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 N1 C3 111.8(5) . . ? C2 N1 Cu1 107.1(3) . . ? C3 N1 Cu1 116.1(4) . . ? C2 N1 H1 107.1 . . ? C3 N1 H1 107.1 . . ? Cu1 N1 H1 107.1 . . ? C1 N2 Cu1 106.6(3) . . ? C1 N2 H2C 110.4 . . ? Cu1 N2 H2C 110.4 . . ? C1 N2 H2D 110.4 . . ? Cu1 N2 H2D 110.4 . . ? H2C N2 H2D 108.6 . . ? N4 N3 Cu2 126.0(3) . . ? N4 N3 Cu1 125.2(3) . . ? Cu2 N3 Cu1 107.72(18) . . ? N5 N4 N3 179.6(7) . . ? N7 N6 Cu2 130.9(3) . . ? N7 N6 Cu3 106.3(3) . 3_675 ? Cu2 N6 Cu3 101.60(15) . 3_675 ? N7 N6 Cu1 129.5(3) . . ? Cu2 N6 Cu1 92.71(13) . . ? Cu3 N6 Cu1 83.82(11) 3_675 . ? N8 N7 N6 175.1(5) . . ? N7 N8 Cu1 160.2(4) . 2_655 ? N10 N9 Cu2 123.5(3) . . ? N10 N9 Cu3 123.4(3) . . ? Cu2 N9 Cu3 100.26(17) . . ? N11 N10 N9 179.3(5) . . ? N13 N12 Cu2 125.7(3) . . ? N13 N12 Cu3 122.7(3) . . ? Cu2 N12 Cu3 101.75(16) . . ? N14 N13 N12 177.2(5) . . ? N16 N15 Cu3 124.5(3) . . ? N17 N16 N15 176.3(5) . . ? N16 N17 Cu2 134.0(4) . 3_775 ? N19 N18 Cu3 122.3(4) . . ? N19 N18 Cu1 124.6(4) . 3_675 ? Cu3 N18 Cu1 109.10(19) . 3_675 ? N20 N19 N18 176.1(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.840 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.128