# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1481 data_1.cif _audit_creation_method SHELXL _chemical_name_common ? _chemical_formula_moiety 'C2 H4 Cu1.50 N13' _chemical_formula_structural 'C2 H4 Cu1.50 N13' _chemical_formula_analytical 'C2 H4 Cu1.50 N13' _chemical_formula_sum 'C2 H4 Cu1.50 N13' _chemical_formula_weight 305.49 _chemical_compound_source 'synthesis' 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 8.4444(15) _cell_length_b 11.1376(13) _cell_length_c 9.994(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.48(2) _cell_angle_gamma 90.00 _cell_volume 929.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 4.70 _cell_measurement_theta_max 12.55 _exptl_special_details ; ? ; _exptl_crystal_description 'block ' _exptl_crystal_colour 'brown ' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'none' _exptl_crystal_density_diffrn 2.183 _exptl_crystal_F_000 602 _exptl_absorpt_coefficient_mu 3.464 _exptl_absorpt_correction_type 'empirical \y scan' _exptl_absorpt_correction_T_min 0.1408 _exptl_absorpt_correction_T_max 0.1706 _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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 14.01 _diffrn_reflns_number 1744 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1630 _reflns_number_observed 1311 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.7384P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 1630 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_obs 0.0374 _refine_ls_wR_factor_all 0.0976 _refine_ls_wR_factor_obs 0.0882 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.058 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.61860(6) 1.11885(6) -0.04650(6) 0.0267(2) Uani 1 d . . Cu2 Cu 1.0000 1.0000 0.0000 0.0234(2) Uani 1 d S . N1 N 0.8568(4) 0.9785(3) -0.1756(4) 0.0240(9) Uani 1 d . . N2 N 0.7047(4) 1.0245(4) -0.1906(4) 0.0267(9) Uani 1 d . . N3 N 0.7461(5) 0.9475(4) -0.3805(4) 0.0268(9) Uani 1 d . . N4 N 0.7153(5) 0.9176(4) -0.5189(4) 0.0382(11) Uani 1 d . . H4A H 0.7884(5) 0.8838(4) -0.5572(4) 0.046 Uiso 1 calc R . H4B H 0.6233(5) 0.9332(4) -0.5650(4) 0.046 Uiso 1 calc R . N5 N 0.8462(4) 1.1263(4) 0.0442(4) 0.0258(9) Uani 1 d . . N6 N 0.8989(5) 1.2297(5) 0.0648(4) 0.0387(11) Uani 1 d . . N7 N 0.9461(7) 1.3255(5) 0.0860(6) 0.062(2) Uani 1 d . . N8 N 0.5339(5) 1.2040(5) 0.0983(4) 0.0405(12) Uani 1 d . . N9 N 0.5975(5) 1.1954(4) 0.2118(4) 0.0363(11) Uani 1 d . . N10 N 0.6555(7) 1.1907(5) 0.3245(5) 0.0571(15) Uani 1 d . . N11 N 0.4032(5) 1.0891(5) -0.1473(5) 0.055(2) Uani 1 d . . N12 N 0.2828(5) 1.1276(4) -0.1198(4) 0.0308(10) Uani 1 d . . N13 N 0.1607(6) 1.1628(5) -0.0950(5) 0.0455(12) Uani 1 d . . C1 C 0.8783(6) 0.9317(4) -0.2910(5) 0.0270(11) Uani 1 d . . H1A H 0.9711(6) 0.8934(4) -0.3083(5) 0.032 Uiso 1 calc R . C2 C 0.6395(6) 1.0052(4) -0.3156(5) 0.0291(11) Uani 1 d . . H2A H 0.5365(6) 1.0277(4) -0.3536(5) 0.035 Uiso 1 calc R . 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 0.0163(3) 0.0348(4) 0.0284(3) -0.0071(3) 0.0015(2) 0.0031(3) Cu2 0.0173(4) 0.0306(5) 0.0210(4) -0.0029(3) -0.0013(3) 0.0065(3) N1 0.015(2) 0.029(2) 0.028(2) 0.000(2) 0.001(2) 0.004(2) N2 0.017(2) 0.032(2) 0.029(2) -0.005(2) -0.004(2) 0.003(2) N3 0.027(2) 0.032(2) 0.020(2) -0.003(2) -0.001(2) 0.004(2) N4 0.037(2) 0.055(3) 0.019(2) -0.012(2) -0.007(2) 0.012(2) N5 0.017(2) 0.031(2) 0.028(2) -0.005(2) 0.000(2) 0.002(2) N6 0.025(2) 0.048(3) 0.041(3) -0.007(2) 0.000(2) 0.005(2) N7 0.047(3) 0.039(3) 0.100(5) -0.025(3) 0.009(3) -0.008(3) N8 0.033(2) 0.061(3) 0.026(2) -0.007(2) 0.002(2) 0.013(2) N9 0.038(3) 0.035(3) 0.036(3) -0.006(2) 0.009(2) -0.006(2) N10 0.083(4) 0.055(3) 0.029(3) -0.007(2) -0.006(3) -0.014(3) N11 0.019(2) 0.080(4) 0.065(3) -0.040(3) 0.003(2) 0.006(2) N12 0.025(2) 0.036(2) 0.030(2) -0.002(2) 0.000(2) -0.002(2) N13 0.028(2) 0.051(3) 0.059(3) 0.009(3) 0.011(2) 0.009(2) C1 0.022(2) 0.030(3) 0.027(2) -0.005(2) -0.002(2) 0.006(2) C2 0.020(2) 0.034(3) 0.031(3) -0.008(2) -0.004(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 N8 1.952(4) . ? Cu1 N11 1.973(5) . ? Cu1 N5 2.002(4) . ? Cu1 N2 2.004(4) . ? Cu2 N1 1.993(4) 3_775 ? Cu2 N1 1.993(4) . ? Cu2 N5 2.008(4) 3_775 ? Cu2 N5 2.008(4) . ? N1 C1 1.303(6) . ? N1 N2 1.370(5) . ? N2 C2 1.306(6) . ? N3 C1 1.336(6) . ? N3 C2 1.348(6) . ? N3 N4 1.409(5) . ? N5 N6 1.241(6) . ? N6 N7 1.148(7) . ? N8 N9 1.185(6) . ? N9 N10 1.162(6) . ? N11 N12 1.172(6) . ? N12 N13 1.164(6) . ? 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 N8 Cu1 N11 92.8(2) . . ? N8 Cu1 N5 94.4(2) . . ? N11 Cu1 N5 171.6(2) . . ? N8 Cu1 N2 177.4(2) . . ? N11 Cu1 N2 87.1(2) . . ? N5 Cu1 N2 85.50(15) . . ? N1 Cu2 N1 180.0 3_775 . ? N1 Cu2 N5 87.11(15) 3_775 3_775 ? N1 Cu2 N5 92.89(15) . 3_775 ? N1 Cu2 N5 92.89(15) 3_775 . ? N1 Cu2 N5 87.11(15) . . ? N5 Cu2 N5 180.0 3_775 . ? C1 N1 N2 107.7(4) . . ? C1 N1 Cu2 133.0(3) . . ? N2 N1 Cu2 119.3(3) . . ? C2 N2 N1 107.4(4) . . ? C2 N2 Cu1 128.8(3) . . ? N1 N2 Cu1 123.4(3) . . ? C1 N3 C2 107.0(4) . . ? C1 N3 N4 129.9(4) . . ? C2 N3 N4 123.1(4) . . ? N6 N5 Cu1 114.3(3) . . ? N6 N5 Cu2 117.3(3) . . ? Cu1 N5 Cu2 118.7(2) . . ? N7 N6 N5 178.7(6) . . ? N9 N8 Cu1 120.4(4) . . ? N10 N9 N8 177.1(6) . . ? N12 N11 Cu1 125.8(4) . . ? N13 N12 N11 177.8(5) . . ? N1 C1 N3 109.2(4) . . ? N2 C2 N3 108.8(4) . . ? _refine_diff_density_max 0.492 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.105 ################################################################ data_2.cif _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C8 H16 Cu2 N24 O6' _chemical_formula_structural 'C8 H16 Cu2 N24 O6' _chemical_formula_analytical 'C8 H16 Cu2 N24 O6' _chemical_formula_sum 'C8 H16 Cu2 N24 O6' _chemical_formula_weight 671.53 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.0069(11) _cell_length_b 8.533(2) _cell_length_c 11.013(2) _cell_angle_alpha 70.95(2) _cell_angle_beta 84.824(13) _cell_angle_gamma 74.253(15) _cell_volume 599.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 5.07 _cell_measurement_theta_max 10.11 _exptl_crystal_description 'thin plate' _exptl_crystal_colour 'pale-green ' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_method none _exptl_crystal_F_000 338 _exptl_absorpt_coefficient_mu 1.857 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.2718 _exptl_absorpt_correction_T_max 0.4722 _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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 5.62 _diffrn_reflns_number 2632 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2073 _reflns_number_observed 1944 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+0.8110P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 2072 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_obs 0.0466 _refine_ls_wR_factor_all 0.1352 _refine_ls_wR_factor_obs 0.1312 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.063 _refine_ls_restrained_S_all 1.058 _refine_ls_restrained_S_obs 1.063 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.5000 0.0198(2) Uani 1 d S . Cu2 Cu 0.5000 0.0000 0.5000 0.0201(2) Uani 1 d S . N1 N 0.1565(4) -0.1644(4) 0.6581(3) 0.0234(6) Uani 1 d . . N2 N 0.3458(4) -0.1650(4) 0.6822(3) 0.0278(6) Uani 1 d . . N3 N 0.2382(4) -0.3381(3) 0.8499(3) 0.0236(6) Uani 1 d . . N4 N 0.2348(5) -0.4551(4) 0.9735(3) 0.0314(7) Uani 1 d . . H4B H 0.3360(5) -0.4890(4) 1.0231(3) 0.038 Uiso 1 calc R . H4C H 0.1316(5) -0.4930(4) 0.9997(3) 0.038 Uiso 1 calc R . N5 N 0.2006(4) -0.1027(3) 0.3862(3) 0.0217(6) Uani 1 d . . N6 N 0.4002(4) -0.1123(4) 0.3934(3) 0.0229(6) Uani 1 d . . N7 N 0.3603(4) -0.2184(4) 0.2476(3) 0.0247(6) Uani 1 d . . N8 N 0.4086(6) -0.2885(5) 0.1462(4) 0.0393(9) Uani 1 d . . H8A H 0.5291(6) -0.3110(5) 0.1198(4) 0.047 Uiso 1 calc R . H8B H 0.3175(6) -0.3089(5) 0.1107(4) 0.047 Uiso 1 calc R . N9 N 0.2301(4) 0.1702(4) 0.4835(3) 0.0268(6) Uani 1 d . . N10 N 0.2191(5) 0.3151(4) 0.4227(4) 0.0414(8) Uani 1 d . . N11 N 0.2075(9) 0.4529(6) 0.3575(7) 0.101(2) Uani 1 d . . C1 C 0.0946(5) -0.2693(5) 0.7596(3) 0.0275(7) Uani 1 d . . H1A H -0.0289(5) -0.2929(5) 0.7682(3) 0.033 Uiso 1 calc R . C2 C 0.3897(5) -0.2696(4) 0.7978(3) 0.0278(7) Uani 1 d . . H2A H 0.5095(5) -0.2936(4) 0.8388(3) 0.033 Uiso 1 calc R . C3 C 0.1803(5) -0.1670(4) 0.2976(3) 0.0240(7) Uani 1 d . . H3A H 0.0614(5) -0.1761(4) 0.2729(3) 0.029 Uiso 1 calc R . C4 C 0.4917(5) -0.1824(4) 0.3085(3) 0.0259(7) Uani 1 d . . H4A H 0.6275(5) -0.2042(4) 0.2927(3) 0.031 Uiso 1 calc R . N12 N 0.1783(5) 0.1483(5) 0.9532(3) 0.0413(8) Uani 1 d . . O1 O 0.0878(6) 0.2857(5) 0.8717(4) 0.0513(9) Uani 1 d . . O2 O 0.2206(6) 0.0147(4) 0.9235(4) 0.0640(10) Uani 1 d . . O3 O 0.2228(6) 0.1517(5) 1.0579(3) 0.0602(9) Uani 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 0.0131(3) 0.0247(4) 0.0183(3) -0.0042(2) -0.0004(2) -0.0024(2) Cu2 0.0136(3) 0.0230(4) 0.0257(4) -0.0100(3) -0.0021(2) -0.0044(2) N1 0.0167(13) 0.0274(14) 0.0245(14) -0.0064(12) 0.0000(10) -0.0055(11) N2 0.0181(14) 0.034(2) 0.0275(15) -0.0033(13) -0.0027(11) -0.0066(12) N3 0.0230(14) 0.0238(14) 0.0210(13) -0.0027(11) -0.0035(11) -0.0051(11) N4 0.031(2) 0.036(2) 0.0201(13) 0.0032(12) -0.0054(12) -0.0110(13) N5 0.0142(13) 0.0268(14) 0.0245(14) -0.0083(11) -0.0008(10) -0.0054(11) N6 0.0146(13) 0.0302(15) 0.0276(14) -0.0128(12) 0.0012(11) -0.0077(11) N7 0.0251(14) 0.0257(14) 0.0258(14) -0.0120(12) 0.0006(11) -0.0061(12) N8 0.036(2) 0.054(2) 0.042(2) -0.035(2) 0.004(2) -0.009(2) N9 0.0194(14) 0.024(2) 0.035(2) -0.0074(13) -0.0012(11) -0.0055(11) N10 0.028(2) 0.029(2) 0.062(2) -0.005(2) -0.0073(15) -0.0063(13) N11 0.075(4) 0.032(2) 0.164(6) 0.017(3) -0.014(4) -0.014(2) C1 0.021(2) 0.035(2) 0.024(2) -0.0029(14) -0.0032(13) -0.0109(14) C2 0.020(2) 0.034(2) 0.027(2) -0.0053(15) -0.0033(13) -0.0079(14) C3 0.020(2) 0.027(2) 0.028(2) -0.0104(14) -0.0011(13) -0.0070(13) C4 0.018(2) 0.032(2) 0.029(2) -0.0131(14) 0.0032(13) -0.0064(14) N12 0.037(2) 0.044(2) 0.042(2) -0.013(2) 0.0121(15) -0.014(2) O1 0.051(2) 0.044(2) 0.052(2) -0.006(2) -0.009(2) -0.009(2) O2 0.082(3) 0.045(2) 0.065(2) -0.028(2) 0.006(2) -0.006(2) O3 0.085(3) 0.061(2) 0.034(2) -0.0137(15) 0.001(2) -0.020(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 2.011(3) 2_556 ? Cu1 N5 2.011(3) . ? Cu1 N1 2.029(3) 2_556 ? Cu1 N1 2.029(3) . ? Cu1 N9 2.406(3) . ? Cu1 N9 2.406(3) 2_556 ? Cu2 N6 2.008(3) 2_656 ? Cu2 N6 2.008(3) . ? Cu2 N9 2.029(3) 2_656 ? Cu2 N9 2.029(3) . ? Cu2 N2 2.402(3) 2_656 ? Cu2 N2 2.402(3) . ? N1 C1 1.307(4) . ? N1 N2 1.374(4) . ? N2 C2 1.301(4) . ? N3 C2 1.343(4) . ? N3 C1 1.351(4) . ? N3 N4 1.404(4) . ? N5 C3 1.299(4) . ? N5 N6 1.387(4) . ? N6 C4 1.301(4) . ? N7 C4 1.339(4) . ? N7 C3 1.348(4) . ? N7 N8 1.406(4) . ? N9 N10 1.183(4) . ? N10 N11 1.146(6) . ? N12 O3 1.233(5) . ? N12 O2 1.239(5) . ? N12 O1 1.263(5) . ? 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 N5 180.0 2_556 . ? N5 Cu1 N1 90.49(11) 2_556 2_556 ? N5 Cu1 N1 89.51(11) . 2_556 ? N5 Cu1 N1 89.51(11) 2_556 . ? N5 Cu1 N1 90.49(11) . . ? N1 Cu1 N1 180.0 2_556 . ? N5 Cu1 N9 97.64(10) 2_556 . ? N5 Cu1 N9 82.36(10) . . ? N1 Cu1 N9 94.42(10) 2_556 . ? N1 Cu1 N9 85.58(10) . . ? N5 Cu1 N9 82.36(10) 2_556 2_556 ? N5 Cu1 N9 97.64(10) . 2_556 ? N1 Cu1 N9 85.58(10) 2_556 2_556 ? N1 Cu1 N9 94.42(10) . 2_556 ? N9 Cu1 N9 180.0 . 2_556 ? N6 Cu2 N6 180.0 2_656 . ? N6 Cu2 N9 88.97(11) 2_656 2_656 ? N6 Cu2 N9 91.03(11) . 2_656 ? N6 Cu2 N9 91.03(11) 2_656 . ? N6 Cu2 N9 88.97(11) . . ? N9 Cu2 N9 180.0 2_656 . ? N6 Cu2 N2 87.64(11) 2_656 2_656 ? N6 Cu2 N2 92.36(11) . 2_656 ? N9 Cu2 N2 82.45(11) 2_656 2_656 ? N9 Cu2 N2 97.55(11) . 2_656 ? N6 Cu2 N2 92.36(11) 2_656 . ? N6 Cu2 N2 87.64(11) . . ? N9 Cu2 N2 97.55(11) 2_656 . ? N9 Cu2 N2 82.45(11) . . ? N2 Cu2 N2 180.0 2_656 . ? C1 N1 N2 107.9(3) . . ? C1 N1 Cu1 128.4(2) . . ? N2 N1 Cu1 123.2(2) . . ? C2 N2 N1 106.6(3) . . ? C2 N2 Cu2 139.8(2) . . ? N1 N2 Cu2 113.4(2) . . ? C2 N3 C1 105.6(3) . . ? C2 N3 N4 125.8(3) . . ? C1 N3 N4 128.6(3) . . ? C3 N5 N6 107.7(3) . . ? C3 N5 Cu1 131.3(2) . . ? N6 N5 Cu1 121.0(2) . . ? C4 N6 N5 107.0(3) . . ? C4 N6 Cu2 130.1(2) . . ? N5 N6 Cu2 122.3(2) . . ? C4 N7 C3 107.1(3) . . ? C4 N7 N8 124.2(3) . . ? C3 N7 N8 128.6(3) . . ? N10 N9 Cu2 117.9(2) . . ? N10 N9 Cu1 129.7(2) . . ? Cu2 N9 Cu1 104.05(12) . . ? N11 N10 N9 175.9(6) . . ? N1 C1 N3 109.3(3) . . ? N2 C2 N3 110.7(3) . . ? N5 C3 N7 108.8(3) . . ? N6 C4 N7 109.5(3) . . ? O3 N12 O2 122.5(4) . . ? O3 N12 O1 119.3(4) . . ? O2 N12 O1 118.2(4) . . ? _refine_diff_density_max 0.905 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.117 #######################################################################