data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Zhao, Zhifeng' _publ_contact_author_email zhifengzhao1980@yahoo.com _publ_section_title ; Three novel metal-organic frameworks constructed from [Cu(CN)] chains ; loop_ _publ_author_name Z.Su Z.Zhao B.Zhou Yu.Zhang # Attachment '- 1.cif' data_1 #TrackingRef '- 1.cif' _database_code_depnum_ccdc_archive 'CCDC 779821' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H8 Cu3 N5' _chemical_formula_weight 448.88 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 9.6328(8) _cell_length_b 23.4438(19) _cell_length_c 6.8997(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.8260(10) _cell_angle_gamma 90.00 _cell_volume 1539.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3462 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 23.68 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 4.109 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4388 _exptl_absorpt_correction_T_max 0.5593 _exptl_absorpt_process_details SADBAS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13888 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3801 _reflns_number_gt 2687 _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^)+(0.0344P)^2^+1.1027P] 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 3801 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 1.00906(5) 0.29763(2) 0.35600(8) 0.07140(17) Uani 1 1 d . . . Cu2 Cu 1.32845(4) 0.444300(18) 0.65365(6) 0.05001(13) Uani 1 1 d . . . Cu3 Cu 1.15408(6) 0.46562(2) 0.27905(7) 0.06640(16) Uani 1 1 d . . . N1 N 0.8015(3) 0.32425(12) 0.2794(4) 0.0545(7) Uani 1 1 d . . . N2 N 0.9221(3) 0.22040(12) 0.3226(4) 0.0517(7) Uani 1 1 d . . . N3 N 1.2372(3) 0.37806(12) 0.5031(4) 0.0533(7) Uani 1 1 d . . . N4 N 1.2746(3) 0.45087(14) 0.9068(5) 0.0563(9) Uani 0.48(2) 1 d P . . N5 N 1.2336(3) 0.45573(15) 0.0540(5) 0.0588(9) Uani 0.48(2) 1 d P . . N6 N 1.4586(3) 0.48689(13) 0.5335(4) 0.0532(8) Uani 0.52(2) 1 d P . . N7 N 1.0381(4) 0.49187(14) 0.4489(5) 0.0602(9) Uani 0.52(2) 1 d P . . C1 C 0.7416(5) 0.37528(16) 0.2578(5) 0.0640(10) Uani 1 1 d . . . H1 H 0.7995 0.4072 0.2767 0.077 Uiso 1 1 calc R . . C2 C 0.5991(5) 0.38397(17) 0.2091(6) 0.0711(11) Uani 1 1 d . . . H2 H 0.5628 0.4208 0.1955 0.085 Uiso 1 1 calc R . . C3 C 0.5120(4) 0.33792(17) 0.1810(6) 0.0661(10) Uani 1 1 d . . . H3 H 0.4155 0.3430 0.1477 0.079 Uiso 1 1 calc R . . C4 C 0.5692(4) 0.28278(15) 0.2026(5) 0.0525(8) Uani 1 1 d . . . C5 C 0.4877(4) 0.23120(19) 0.1755(6) 0.0655(10) Uani 1 1 d . . . H5 H 0.3906 0.2335 0.1427 0.079 Uiso 1 1 calc R . . C6 C 0.5485(4) 0.18045(17) 0.1964(6) 0.0656(10) Uani 1 1 d . . . H6 H 0.4923 0.1481 0.1782 0.079 Uiso 1 1 calc R . . C7 C 0.6973(4) 0.17341(14) 0.2458(5) 0.0509(8) Uani 1 1 d . . . C8 C 0.7664(4) 0.12091(16) 0.2699(6) 0.0646(10) Uani 1 1 d . . . H8 H 0.7147 0.0873 0.2518 0.077 Uiso 1 1 calc R . . C9 C 0.9073(5) 0.11850(17) 0.3192(6) 0.0678(10) Uani 1 1 d . . . H9 H 0.9531 0.0835 0.3359 0.081 Uiso 1 1 calc R . . C10 C 0.9829(4) 0.16929(17) 0.3446(5) 0.0612(9) Uani 1 1 d . . . H10 H 1.0801 0.1674 0.3783 0.073 Uiso 1 1 calc R . . C11 C 0.7806(3) 0.22272(14) 0.2740(4) 0.0447(7) Uani 1 1 d . . . C12 C 0.7155(3) 0.27799(14) 0.2506(4) 0.0459(7) Uani 1 1 d . . . C13 C 1.1596(4) 0.34458(14) 0.4392(5) 0.0510(8) Uani 1 1 d . . . C14 C 1.4586(3) 0.48689(13) 0.5335(4) 0.0532(8) Uani 0.48(2) 1 d P . . C15 C 1.0381(4) 0.49187(14) 0.4489(5) 0.0602(9) Uani 0.48(2) 1 d P . . C16 C 1.2746(3) 0.45087(14) 0.9068(5) 0.0563(9) Uani 0.52(2) 1 d P . . C17 C 1.2336(3) 0.45573(15) 0.0540(5) 0.0588(9) Uani 0.52(2) 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 0.0575(3) 0.0854(4) 0.0722(3) -0.0167(3) 0.0128(2) -0.0313(2) Cu2 0.0484(2) 0.0496(2) 0.0541(2) 0.00126(18) 0.01440(18) -0.00474(18) Cu3 0.0813(3) 0.0678(3) 0.0557(3) -0.0010(2) 0.0284(2) 0.0094(2) N1 0.0622(18) 0.0442(16) 0.0579(17) -0.0124(13) 0.0122(14) -0.0097(14) N2 0.0456(15) 0.0547(17) 0.0552(17) -0.0103(13) 0.0094(13) -0.0048(13) N3 0.0448(16) 0.0461(17) 0.070(2) 0.0007(14) 0.0116(14) -0.0006(13) N4 0.0541(19) 0.064(2) 0.0514(19) 0.0015(15) 0.0109(15) -0.0047(16) N5 0.059(2) 0.071(2) 0.0484(19) 0.0003(15) 0.0148(15) 0.0032(17) N6 0.065(2) 0.0487(19) 0.0501(18) -0.0135(14) 0.0232(15) -0.0138(15) N7 0.082(3) 0.0470(19) 0.054(2) 0.0091(15) 0.0167(16) 0.0165(17) C1 0.085(3) 0.044(2) 0.063(2) -0.0122(17) 0.013(2) -0.0082(19) C2 0.091(3) 0.051(2) 0.072(3) -0.0099(19) 0.017(2) 0.013(2) C3 0.059(2) 0.068(3) 0.072(3) 0.000(2) 0.0126(19) 0.014(2) C4 0.0509(19) 0.054(2) 0.0532(19) -0.0077(16) 0.0090(15) -0.0006(16) C5 0.045(2) 0.082(3) 0.066(2) 0.003(2) -0.0005(17) -0.0126(19) C6 0.062(2) 0.060(2) 0.071(2) -0.0056(19) 0.0004(19) -0.0224(19) C7 0.058(2) 0.0453(19) 0.0481(18) -0.0068(14) 0.0032(15) -0.0089(16) C8 0.081(3) 0.043(2) 0.066(2) -0.0083(17) 0.001(2) -0.0088(19) C9 0.082(3) 0.051(2) 0.069(2) -0.0097(18) 0.005(2) 0.007(2) C10 0.054(2) 0.068(3) 0.062(2) -0.0079(18) 0.0099(17) 0.0111(19) C11 0.0481(18) 0.0465(18) 0.0401(16) -0.0089(13) 0.0084(13) -0.0072(14) C12 0.0485(18) 0.0485(18) 0.0413(17) -0.0091(13) 0.0089(14) -0.0076(14) C13 0.0453(18) 0.0441(19) 0.063(2) -0.0014(16) 0.0058(16) -0.0001(15) C14 0.065(2) 0.0487(19) 0.0501(18) -0.0135(14) 0.0232(15) -0.0138(15) C15 0.082(3) 0.0470(19) 0.054(2) 0.0091(15) 0.0167(16) 0.0165(17) C16 0.0541(19) 0.064(2) 0.0514(19) 0.0015(15) 0.0109(15) -0.0047(16) C17 0.059(2) 0.071(2) 0.0484(19) 0.0003(15) 0.0148(15) 0.0032(17) _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 1.841(4) . ? Cu1 N2 1.994(3) . ? Cu1 N1 2.084(3) . ? Cu2 N6 1.891(3) . ? Cu2 N4 1.903(3) . ? Cu2 N3 1.996(3) . ? Cu2 Cu3 2.9016(7) . ? Cu3 N7 1.844(3) . ? Cu3 N5 1.848(3) . ? N1 C1 1.326(5) . ? N1 C12 1.360(4) . ? N2 C10 1.332(5) . ? N2 C11 1.354(4) . ? N3 C13 1.126(4) . ? N4 C17 1.150(4) 1_556 ? N4 N5 1.150(4) 1_556 ? N5 C16 1.150(4) 1_554 ? N5 N4 1.150(4) 1_554 ? N6 C14 1.157(5) 3_866 ? N6 N6 1.157(5) 3_866 ? N7 C15 1.158(6) 3_766 ? N7 N7 1.158(6) 3_766 ? C1 C2 1.378(6) . ? C1 H1 0.9300 . ? C2 C3 1.363(6) . ? C2 H2 0.9300 . ? C3 C4 1.404(5) . ? C3 H3 0.9300 . ? C4 C12 1.402(5) . ? C4 C5 1.438(5) . ? C5 C6 1.324(6) . ? C5 H5 0.9300 . ? C6 C7 1.431(5) . ? C6 H6 0.9300 . ? C7 C8 1.397(5) . ? C7 C11 1.403(4) . ? C8 C9 1.349(5) . ? C8 H8 0.9300 . ? C9 C10 1.393(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.438(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 C13 Cu1 N2 151.18(13) . . ? C13 Cu1 N1 125.41(13) . . ? N2 Cu1 N1 82.69(11) . . ? N6 Cu2 N4 130.70(13) . . ? N6 Cu2 N3 116.84(12) . . ? N4 Cu2 N3 112.35(13) . . ? N6 Cu2 Cu3 81.42(10) . . ? N4 Cu2 Cu3 126.97(10) . . ? N3 Cu2 Cu3 61.44(8) . . ? N7 Cu3 N5 160.93(15) . . ? N7 Cu3 Cu2 79.37(11) . . ? N5 Cu3 Cu2 117.96(11) . . ? C1 N1 C12 117.3(3) . . ? C1 N1 Cu1 133.0(3) . . ? C12 N1 Cu1 109.7(2) . . ? C10 N2 C11 118.2(3) . . ? C10 N2 Cu1 129.3(2) . . ? C11 N2 Cu1 112.4(2) . . ? C13 N3 Cu2 163.6(3) . . ? C17 N4 N5 0.0(3) 1_556 1_556 ? C17 N4 Cu2 175.7(3) 1_556 . ? N5 N4 Cu2 175.7(3) 1_556 . ? C16 N5 N4 0.0(4) 1_554 1_554 ? C16 N5 Cu3 175.3(3) 1_554 . ? N4 N5 Cu3 175.3(3) 1_554 . ? C14 N6 N6 0.0(4) 3_866 3_866 ? C14 N6 Cu2 177.5(4) 3_866 . ? N6 N6 Cu2 177.5(4) 3_866 . ? C15 N7 N7 0.0(3) 3_766 3_766 ? C15 N7 Cu3 177.9(5) 3_766 . ? N7 N7 Cu3 177.9(5) 3_766 . ? N1 C1 C2 124.1(4) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C12 C4 C3 117.6(3) . . ? C12 C4 C5 118.2(3) . . ? C3 C4 C5 124.3(3) . . ? C6 C5 C4 121.2(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 122.7(3) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C8 C7 C11 117.2(3) . . ? C8 C7 C6 124.8(3) . . ? C11 C7 C6 117.9(3) . . ? C9 C8 C7 120.6(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118.9(4) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 122.8(3) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C7 122.2(3) . . ? N2 C11 C12 118.0(3) . . ? C7 C11 C12 119.8(3) . . ? N1 C12 C4 122.5(3) . . ? N1 C12 C11 117.2(3) . . ? C4 C12 C11 120.3(3) . . ? N3 C13 Cu1 169.3(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.541 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.063 # Attachment '- 2.cif' data_2 #TrackingRef '- 2.cif' _database_code_depnum_ccdc_archive 'CCDC 779822' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H8 Cu2 N4' _chemical_formula_weight 335.30 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)/n 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 8.5451(3) _cell_length_b 11.6761(4) _cell_length_c 12.5593(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.9110(10) _cell_angle_gamma 90.00 _cell_volume 1230.43(8) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4820 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 27.81 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 3.440 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4923 _exptl_absorpt_correction_T_max 0.6091 _exptl_absorpt_process_details SADBAS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10836 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3035 _reflns_number_gt 2645 _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^)+(0.0441P)^2^+1.1640P] 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 3035 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 1.02888(4) 0.90337(3) 0.54165(2) 0.03402(10) Uani 1 1 d . . . Cu2 Cu 0.64184(4) 0.65350(3) 0.67884(2) 0.03548(10) Uani 1 1 d . . . N1 N 0.5990(3) 0.59695(19) 0.81331(17) 0.0360(5) Uani 1 1 d . . . N2 N 0.7991(3) 0.7368(2) 0.62363(19) 0.0479(6) Uani 1 1 d . . . N3 N 1.2366(2) 0.90226(19) 0.65789(17) 0.0343(4) Uani 1 1 d . . . N4 N 0.4361(2) 0.6322(2) 0.56304(17) 0.0368(5) Uani 1 1 d . . . C1 C 1.0673(3) 0.9207(2) 0.3958(2) 0.0330(5) Uani 1 1 d . . . C2 C 0.8852(3) 0.7960(2) 0.59161(18) 0.0282(5) Uani 1 1 d . . . C3 C 0.2917(3) 0.6180(2) 0.5888(2) 0.0349(5) Uani 1 1 d . . . H3 H 0.2848 0.6141 0.6617 0.042 Uiso 1 1 calc R . . C4 C 0.1536(3) 0.6089(2) 0.5127(2) 0.0347(5) Uani 1 1 d . . . H4 H 0.0561 0.6013 0.5345 0.042 Uiso 1 1 calc R . . C5 C 0.1602(3) 0.6110(2) 0.4021(2) 0.0320(5) Uani 1 1 d . . . C6 C 0.3108(3) 0.6224(3) 0.3759(2) 0.0416(6) Uani 1 1 d . . . H6 H 0.3224 0.6218 0.3037 0.050 Uiso 1 1 calc R . . C7 C 0.4417(3) 0.6345(3) 0.4571(2) 0.0451(7) Uani 1 1 d . . . H7 H 0.5404 0.6449 0.4376 0.054 Uiso 1 1 calc R . . C8 C 0.0141(3) 0.6043(2) 0.3180(2) 0.0324(5) Uani 1 1 d . . . C9 C -0.1276(3) 0.6536(2) 0.3348(2) 0.0362(5) Uani 1 1 d . . . H9 H -0.1321 0.6897 0.4001 0.043 Uiso 1 1 calc R . . C10 C 0.0119(3) 0.5516(3) 0.2189(2) 0.0484(7) Uani 1 1 d . . . H10 H 0.1038 0.5176 0.2038 0.058 Uiso 1 1 calc R . . C11 C 1.2391(3) 0.8515(2) 0.7539(2) 0.0360(5) Uani 1 1 d . . . H11 H 1.1456 0.8179 0.7665 0.043 Uiso 1 1 calc R . . C12 C 1.3723(3) 0.9502(3) 0.6425(2) 0.0503(8) Uani 1 1 d . . . H12 H 1.3730 0.9869 0.5769 0.060 Uiso 1 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 0.03370(17) 0.04306(19) 0.02514(16) 0.00460(12) 0.00517(12) -0.00586(12) Cu2 0.03171(16) 0.0465(2) 0.02941(17) 0.00467(13) 0.00869(12) -0.00693(13) N1 0.0372(11) 0.0429(12) 0.0289(10) 0.0022(9) 0.0091(9) -0.0032(9) N2 0.0481(13) 0.0610(16) 0.0333(12) -0.0042(11) 0.0046(10) -0.0023(12) N3 0.0307(10) 0.0434(12) 0.0277(10) 0.0041(9) 0.0027(8) -0.0017(9) N4 0.0313(10) 0.0483(13) 0.0297(10) 0.0058(9) 0.0031(8) -0.0051(9) C1 0.0290(11) 0.0411(13) 0.0290(12) -0.0002(10) 0.0055(9) -0.0024(10) C2 0.0281(10) 0.0345(12) 0.0244(10) -0.0011(9) 0.0116(8) -0.0096(9) C3 0.0352(12) 0.0422(14) 0.0279(12) 0.0006(10) 0.0075(10) -0.0053(10) C4 0.0302(11) 0.0418(13) 0.0331(13) -0.0006(10) 0.0083(10) -0.0044(10) C5 0.0303(11) 0.0347(12) 0.0294(12) 0.0008(9) 0.0013(9) 0.0016(9) C6 0.0363(13) 0.0631(18) 0.0260(12) 0.0082(12) 0.0074(10) 0.0010(12) C7 0.0298(12) 0.074(2) 0.0316(13) 0.0117(13) 0.0065(10) -0.0027(13) C8 0.0305(11) 0.0352(12) 0.0299(12) 0.0011(10) 0.0018(9) 0.0015(9) C9 0.0343(12) 0.0451(14) 0.0288(12) -0.0075(11) 0.0046(10) 0.0001(11) C10 0.0358(13) 0.068(2) 0.0381(14) -0.0127(14) -0.0004(11) 0.0158(13) C11 0.0308(11) 0.0464(15) 0.0308(12) 0.0061(11) 0.0060(10) -0.0008(10) C12 0.0411(14) 0.072(2) 0.0345(14) 0.0187(14) -0.0011(11) -0.0157(14) _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 C1 1.931(2) . ? Cu1 C2 1.940(2) . ? Cu1 N3 2.074(2) . ? Cu1 C1 2.399(3) 3_776 ? Cu1 Cu1 2.4968(6) 3_776 ? Cu2 N2 1.893(3) . ? Cu2 N1 1.912(2) . ? Cu2 N4 2.074(2) . ? N1 C1 1.139(3) 4_576 ? N2 C2 1.137(3) . ? N3 C12 1.334(3) . ? N3 C11 1.340(3) . ? N4 C7 1.340(3) . ? N4 C3 1.344(3) . ? C1 N1 1.139(3) 4_675 ? C1 Cu1 2.399(3) 3_776 ? C3 C4 1.375(4) . ? C3 H3 0.9300 . ? C4 C5 1.401(3) . ? C4 H4 0.9300 . ? C5 C6 1.393(4) . ? C5 C8 1.477(3) . ? C6 C7 1.372(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C10 1.386(4) . ? C8 C9 1.392(3) . ? C9 C11 1.377(3) 4_475 ? C9 H9 0.9300 . ? C10 C12 1.382(4) 4_475 ? C10 H10 0.9300 . ? C11 C9 1.377(3) 4_776 ? C11 H11 0.9300 . ? C12 C10 1.382(4) 4_776 ? C12 H12 0.9300 . ? 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 C1 Cu1 C2 127.28(10) . . ? C1 Cu1 N3 113.06(9) . . ? C2 Cu1 N3 106.14(9) . . ? C1 Cu1 C1 110.54(8) . 3_776 ? C2 Cu1 C1 99.84(9) . 3_776 ? N3 Cu1 C1 94.33(9) . 3_776 ? C1 Cu1 Cu1 64.12(8) . 3_776 ? C2 Cu1 Cu1 129.25(8) . 3_776 ? N3 Cu1 Cu1 112.06(6) . 3_776 ? C1 Cu1 Cu1 46.41(6) 3_776 3_776 ? N2 Cu2 N1 140.23(10) . . ? N2 Cu2 N4 111.78(9) . . ? N1 Cu2 N4 107.42(9) . . ? C1 N1 Cu2 170.0(2) 4_576 . ? C2 N2 Cu2 173.4(3) . . ? C12 N3 C11 116.8(2) . . ? C12 N3 Cu1 123.15(18) . . ? C11 N3 Cu1 120.09(17) . . ? C7 N4 C3 116.6(2) . . ? C7 N4 Cu2 120.59(17) . . ? C3 N4 Cu2 122.76(17) . . ? N1 C1 Cu1 163.1(2) 4_675 . ? N1 C1 Cu1 127.5(2) 4_675 3_776 ? Cu1 C1 Cu1 69.46(8) . 3_776 ? N2 C2 Cu1 177.0(2) . . ? N4 C3 C4 123.2(2) . . ? N4 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C3 C4 C5 119.9(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 116.7(2) . . ? C6 C5 C8 121.9(2) . . ? C4 C5 C8 121.4(2) . . ? C7 C6 C5 119.6(2) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? N4 C7 C6 124.0(2) . . ? N4 C7 H7 118.0 . . ? C6 C7 H7 118.0 . . ? C10 C8 C9 117.1(2) . . ? C10 C8 C5 122.2(2) . . ? C9 C8 C5 120.8(2) . . ? C11 C9 C8 119.5(2) 4_475 . ? C11 C9 H9 120.2 4_475 . ? C8 C9 H9 120.2 . . ? C12 C10 C8 119.6(3) 4_475 . ? C12 C10 H10 120.2 4_475 . ? C8 C10 H10 120.2 . . ? N3 C11 C9 123.5(2) . 4_776 ? N3 C11 H11 118.2 . . ? C9 C11 H11 118.2 4_776 . ? N3 C12 C10 123.5(3) . 4_776 ? N3 C12 H12 118.2 . . ? C10 C12 H12 118.2 4_776 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.706 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.075 # Attachment '- 3.cif' data_3 #TrackingRef '- 3.cif' _database_code_depnum_ccdc_archive 'CCDC 779823' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 Cu4 N8' _chemical_formula_weight 754.76 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4290(3) _cell_length_b 14.1167(6) _cell_length_c 16.1356(7) _cell_angle_alpha 68.7340(10) _cell_angle_beta 80.8660(10) _cell_angle_gamma 81.6060(10) _cell_volume 1549.76(11) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3889 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.21 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 2.741 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 0.618 _exptl_absorpt_process_details SADBAS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14132 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7269 _reflns_number_gt 4792 _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^)+(0.0450P)^2^+0.3556P] 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 7269 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.17737(6) 0.06101(3) 0.66400(3) 0.06294(12) Uani 1 1 d . . . Cu2 Cu 0.27167(5) 0.39805(3) 0.43640(2) 0.06121(12) Uani 1 1 d . . . Cu3 Cu 0.54303(6) 0.57845(3) 0.13158(2) 0.06469(13) Uani 1 1 d . . . Cu4 Cu 0.69757(6) 0.89988(3) -0.10219(3) 0.06567(13) Uani 1 1 d . . . N1 N 0.2057(4) 0.1906(2) 0.57209(18) 0.0673(7) Uani 1 1 d . . . N2 N 0.3616(4) 0.4610(2) 0.31362(18) 0.0694(7) Uani 1 1 d . . . N3 N 0.5735(4) 0.7119(2) 0.04713(18) 0.0726(7) Uani 1 1 d . . . N4 N 0.8971(4) 0.9493(2) -0.1899(2) 0.0767(8) Uani 1 1 d . . . N5 N 0.4253(4) -0.02928(18) 0.66494(17) 0.0601(6) Uani 1 1 d . . . N6 N 0.2414(3) 0.51597(18) 0.48745(16) 0.0581(6) Uani 1 1 d . . . N7 N 0.7005(3) 0.48717(19) 0.06464(16) 0.0620(6) Uani 1 1 d . . . N8 N 0.4942(3) 1.02180(18) -0.12665(16) 0.0595(6) Uani 1 1 d . . . C1 C 0.2280(4) 0.2699(2) 0.52020(18) 0.0532(7) Uani 1 1 d . . . C2 C 0.4322(4) 0.5056(2) 0.24448(19) 0.0570(7) Uani 1 1 d . . . C3 C 0.6174(4) 0.7844(2) -0.0089(2) 0.0606(8) Uani 1 1 d . . . C4 C 0.0027(4) -0.0104(2) 0.7523(2) 0.0604(8) Uani 1 1 d . . . C5 C 0.4536(5) -0.1205(2) 0.7281(2) 0.0710(9) Uani 1 1 d . . . H5 H 0.3603 -0.1421 0.7744 0.085 Uiso 1 1 calc R . . C6 C 0.6111(5) -0.1844(2) 0.7289(2) 0.0690(9) Uani 1 1 d . . . H6 H 0.6212 -0.2474 0.7747 0.083 Uiso 1 1 calc R . . C7 C 0.7554(4) -0.1561(2) 0.66241(19) 0.0562(7) Uani 1 1 d . . . C8 C 0.7268(5) -0.0617(3) 0.5976(2) 0.0765(10) Uani 1 1 d . . . H8 H 0.8182 -0.0381 0.5507 0.092 Uiso 1 1 calc R . . C9 C 0.5647(5) -0.0021(2) 0.6015(2) 0.0740(10) Uani 1 1 d . . . H9 H 0.5515 0.0615 0.5567 0.089 Uiso 1 1 calc R . . C10 C 0.9280(4) -0.2258(2) 0.6635(2) 0.0664(8) Uani 1 1 d . . . H10A H 0.9015 -0.2840 0.6505 0.080 Uiso 1 1 calc R . . H10B H 0.9634 -0.2514 0.7236 0.080 Uiso 1 1 calc R . . C11 C 1.0908(4) -0.1802(2) 0.5989(2) 0.0659(8) Uani 1 1 d . . . H11A H 1.1189 -0.1219 0.6112 0.079 Uiso 1 1 calc R . . H11B H 1.0581 -0.1558 0.5383 0.079 Uiso 1 1 calc R . . C12 C 0.1919(5) 0.4986(2) 0.5751(2) 0.0684(9) Uani 1 1 d . . . H12 H 0.1528 0.4353 0.6108 0.082 Uiso 1 1 calc R . . C13 C 0.1958(5) 0.5692(3) 0.6144(2) 0.0695(9) Uani 1 1 d . . . H13 H 0.1601 0.5528 0.6755 0.083 Uiso 1 1 calc R . . C14 C 0.2522(4) 0.6645(2) 0.5645(2) 0.0577(7) Uani 1 1 d . . . C15 C 0.2972(5) 0.6837(2) 0.4744(2) 0.0694(9) Uani 1 1 d . . . H15 H 0.3323 0.7474 0.4371 0.083 Uiso 1 1 calc R . . C16 C 0.2910(5) 0.6094(2) 0.4390(2) 0.0682(9) Uani 1 1 d . . . H16 H 0.3230 0.6250 0.3777 0.082 Uiso 1 1 calc R . . C17 C 0.2619(4) 0.7437(3) 0.6051(2) 0.0692(9) Uani 1 1 d . . . H17A H 0.3673 0.7811 0.5752 0.083 Uiso 1 1 calc R . . H17B H 0.2804 0.7096 0.6676 0.083 Uiso 1 1 calc R . . C18 C 0.7335(5) 0.3863(3) 0.1047(2) 0.0795(10) Uani 1 1 d . . . H18 H 0.6975 0.3585 0.1658 0.095 Uiso 1 1 calc R . . C19 C 0.8159(6) 0.3219(3) 0.0620(2) 0.0845(11) Uani 1 1 d . . . H19 H 0.8392 0.2527 0.0943 0.101 Uiso 1 1 calc R . . C20 C 0.8644(4) 0.3582(3) -0.0277(2) 0.0665(8) Uani 1 1 d . . . C21 C 0.8367(4) 0.4624(3) -0.0709(2) 0.0661(8) Uani 1 1 d . . . H21 H 0.8727 0.4912 -0.1319 0.079 Uiso 1 1 calc R . . C22 C 0.7551(4) 0.5237(2) -0.0226(2) 0.0646(8) Uani 1 1 d . . . H22 H 0.7375 0.5937 -0.0526 0.077 Uiso 1 1 calc R . . C23 C 0.9327(5) 0.2817(3) -0.0757(2) 0.0842(11) Uani 1 1 d . . . H23A H 1.0318 0.2364 -0.0454 0.101 Uiso 1 1 calc R . . H23B H 0.8339 0.2405 -0.0687 0.101 Uiso 1 1 calc R . . C24 C 0.9968(6) 0.3238(3) -0.1705(2) 0.0916(12) Uani 1 1 d . . . H24A H 1.1091 0.3549 -0.1779 0.110 Uiso 1 1 calc R . . H24B H 0.9060 0.3767 -0.2004 0.110 Uiso 1 1 calc R . . C25 C 0.3258(5) 1.0080(2) -0.0848(2) 0.0658(8) Uani 1 1 d . . . H25 H 0.3087 0.9490 -0.0353 0.079 Uiso 1 1 calc R . . C26 C 0.1758(5) 1.0761(2) -0.1107(2) 0.0655(8) Uani 1 1 d . . . H26 H 0.0609 1.0622 -0.0792 0.079 Uiso 1 1 calc R . . C27 C 0.1948(4) 1.1652(2) -0.1834(2) 0.0594(8) Uani 1 1 d . . . C28 C 0.3687(5) 1.1807(2) -0.2251(2) 0.0657(8) Uani 1 1 d . . . H28 H 0.3900 1.2403 -0.2734 0.079 Uiso 1 1 calc R . . C29 C 0.5121(5) 1.1089(2) -0.1961(2) 0.0676(9) Uani 1 1 d . . . H29 H 0.6283 1.1215 -0.2265 0.081 Uiso 1 1 calc R . . C30 C 0.0331(5) 1.2399(3) -0.2154(2) 0.0746(9) Uani 1 1 d . . . H30A H -0.0749 1.2034 -0.2020 0.089 Uiso 1 1 calc R . . H30B H 0.0545 1.2728 -0.2799 0.089 Uiso 1 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 0.0712(3) 0.0522(2) 0.0610(2) -0.01708(18) 0.00196(18) -0.00935(18) Cu2 0.0652(3) 0.0552(2) 0.0546(2) -0.01051(17) 0.00009(17) -0.00921(18) Cu3 0.0692(3) 0.0657(2) 0.0495(2) -0.01099(18) 0.00208(17) -0.00987(19) Cu4 0.0660(3) 0.0531(2) 0.0672(3) -0.01027(18) -0.00228(19) -0.00623(18) N1 0.0665(17) 0.0677(17) 0.0625(16) -0.0199(14) 0.0003(13) -0.0064(13) N2 0.0771(19) 0.0638(16) 0.0597(16) -0.0153(13) -0.0051(14) -0.0024(14) N3 0.079(2) 0.0646(17) 0.0654(17) -0.0172(14) 0.0011(14) -0.0051(15) N4 0.0705(19) 0.0620(17) 0.090(2) -0.0210(15) -0.0023(16) -0.0051(14) N5 0.0649(16) 0.0470(13) 0.0617(15) -0.0150(12) 0.0048(12) -0.0080(12) N6 0.0629(16) 0.0530(14) 0.0517(14) -0.0135(11) 0.0056(11) -0.0101(12) N7 0.0673(17) 0.0579(15) 0.0529(14) -0.0149(12) 0.0068(12) -0.0081(12) N8 0.0625(16) 0.0486(13) 0.0567(14) -0.0097(11) 0.0030(12) -0.0054(11) C1 0.0621(18) 0.0485(16) 0.0445(15) -0.0127(13) 0.0006(13) -0.0073(13) C2 0.0630(19) 0.0527(16) 0.0472(16) -0.0125(13) -0.0012(13) 0.0009(14) C3 0.0612(19) 0.0524(17) 0.0579(18) -0.0110(14) 0.0012(14) -0.0036(14) C4 0.0602(19) 0.0486(16) 0.0668(19) -0.0159(14) 0.0032(15) -0.0107(14) C5 0.068(2) 0.0548(18) 0.069(2) -0.0032(15) 0.0113(16) -0.0092(16) C6 0.068(2) 0.0507(17) 0.071(2) -0.0039(15) 0.0011(16) -0.0077(15) C7 0.0601(19) 0.0578(17) 0.0552(17) -0.0249(14) -0.0059(14) -0.0067(14) C8 0.070(2) 0.070(2) 0.062(2) -0.0032(16) 0.0139(16) 0.0011(18) C9 0.078(2) 0.0553(18) 0.066(2) -0.0031(15) 0.0077(17) -0.0015(17) C10 0.067(2) 0.0615(19) 0.068(2) -0.0211(16) -0.0092(16) 0.0020(16) C11 0.062(2) 0.067(2) 0.077(2) -0.0348(17) -0.0053(16) -0.0073(16) C12 0.085(2) 0.0573(18) 0.0521(18) -0.0077(15) 0.0011(16) -0.0129(17) C13 0.080(2) 0.073(2) 0.0510(17) -0.0198(16) -0.0006(16) -0.0054(18) C14 0.0447(17) 0.0643(19) 0.0647(19) -0.0244(15) -0.0076(14) -0.0001(14) C15 0.079(2) 0.0559(18) 0.069(2) -0.0196(16) 0.0079(17) -0.0183(17) C16 0.084(2) 0.0626(19) 0.0514(17) -0.0164(15) 0.0098(15) -0.0141(17) C17 0.060(2) 0.074(2) 0.083(2) -0.0393(19) -0.0072(17) -0.0041(16) C18 0.102(3) 0.061(2) 0.062(2) -0.0110(17) 0.0077(18) -0.0100(19) C19 0.109(3) 0.062(2) 0.067(2) -0.0114(18) -0.006(2) 0.005(2) C20 0.0528(19) 0.067(2) 0.079(2) -0.0277(17) -0.0129(16) 0.0085(15) C21 0.065(2) 0.081(2) 0.0470(16) -0.0190(16) 0.0003(14) -0.0077(17) C22 0.071(2) 0.0577(18) 0.0568(18) -0.0149(15) 0.0041(15) -0.0073(15) C23 0.079(3) 0.074(2) 0.083(3) -0.020(2) 0.0008(19) 0.0139(19) C24 0.090(3) 0.085(3) 0.076(2) -0.012(2) -0.013(2) 0.029(2) C25 0.073(2) 0.0497(17) 0.0601(18) -0.0063(14) 0.0069(16) -0.0091(16) C26 0.0575(19) 0.0630(19) 0.068(2) -0.0181(16) 0.0038(15) -0.0047(15) C27 0.070(2) 0.0535(17) 0.0552(17) -0.0225(14) -0.0089(15) 0.0040(15) C28 0.077(2) 0.0497(17) 0.0539(18) -0.0037(14) 0.0016(16) -0.0015(15) C29 0.066(2) 0.0579(18) 0.0644(19) -0.0091(15) 0.0073(15) -0.0082(16) C30 0.081(2) 0.075(2) 0.069(2) -0.0318(18) -0.0208(18) 0.0199(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 C4 1.867(3) . ? Cu1 N1 1.906(3) . ? Cu1 N5 2.080(3) . ? Cu2 C1 1.861(3) . ? Cu2 N2 1.907(3) . ? Cu2 N6 2.080(2) . ? Cu3 C2 1.862(3) . ? Cu3 N3 1.903(3) . ? Cu3 N7 2.089(3) . ? Cu4 C3 1.870(3) . ? Cu4 N4 1.899(3) . ? Cu4 N8 2.083(2) . ? N1 C1 1.146(4) . ? N2 C2 1.148(4) . ? N3 C3 1.142(4) . ? N4 C4 1.149(4) 1_664 ? N5 C9 1.328(4) . ? N5 C5 1.333(4) . ? N6 C16 1.338(4) . ? N6 C12 1.343(4) . ? N7 C22 1.329(4) . ? N7 C18 1.336(4) . ? N8 C25 1.329(4) . ? N8 C29 1.337(3) . ? C4 N4 1.149(4) 1_446 ? C5 C6 1.368(4) . ? C5 H5 0.9300 . ? C6 C7 1.381(4) . ? C6 H6 0.9300 . ? C7 C8 1.375(4) . ? C7 C10 1.496(4) . ? C8 C9 1.371(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.518(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C17 1.530(4) 1_645 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.368(4) . ? C12 H12 0.9300 . ? C13 C14 1.380(4) . ? C13 H13 0.9300 . ? C14 C15 1.373(4) . ? C14 C17 1.502(4) . ? C15 C16 1.373(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C11 1.530(4) 1_465 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.353(5) . ? C18 H18 0.9300 . ? C19 C20 1.356(5) . ? C19 H19 0.9300 . ? C20 C21 1.381(4) . ? C20 C23 1.530(5) . ? C21 C22 1.381(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.453(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C30 1.571(5) 1_645 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.373(4) . ? C25 H25 0.9300 . ? C26 C27 1.381(4) . ? C26 H26 0.9300 . ? C27 C28 1.367(4) . ? C27 C30 1.501(4) . ? C28 C29 1.371(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C24 1.571(5) 1_465 ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? 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 C4 Cu1 N1 141.05(13) . . ? C4 Cu1 N5 110.56(12) . . ? N1 Cu1 N5 108.39(11) . . ? C1 Cu2 N2 140.54(12) . . ? C1 Cu2 N6 115.37(11) . . ? N2 Cu2 N6 103.75(10) . . ? C2 Cu3 N3 144.09(12) . . ? C2 Cu3 N7 114.22(11) . . ? N3 Cu3 N7 101.69(11) . . ? C3 Cu4 N4 143.58(13) . . ? C3 Cu4 N8 111.71(12) . . ? N4 Cu4 N8 104.63(11) . . ? C1 N1 Cu1 175.9(3) . . ? C2 N2 Cu2 169.8(3) . . ? C3 N3 Cu3 168.6(3) . . ? C4 N4 Cu4 171.4(3) 1_664 . ? C9 N5 C5 115.0(3) . . ? C9 N5 Cu1 122.7(2) . . ? C5 N5 Cu1 122.2(2) . . ? C16 N6 C12 115.5(3) . . ? C16 N6 Cu2 122.9(2) . . ? C12 N6 Cu2 121.0(2) . . ? C22 N7 C18 115.9(3) . . ? C22 N7 Cu3 121.9(2) . . ? C18 N7 Cu3 121.7(2) . . ? C25 N8 C29 115.8(3) . . ? C25 N8 Cu4 120.0(2) . . ? C29 N8 Cu4 122.7(2) . . ? N1 C1 Cu2 178.3(3) . . ? N2 C2 Cu3 179.0(3) . . ? N3 C3 Cu4 177.7(3) . . ? N4 C4 Cu1 175.5(3) 1_446 . ? N5 C5 C6 124.1(3) . . ? N5 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C5 C6 C7 120.6(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 115.2(3) . . ? C8 C7 C10 124.1(3) . . ? C6 C7 C10 120.7(3) . . ? C9 C8 C7 120.6(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? N5 C9 C8 124.3(3) . . ? N5 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? C7 C10 C11 116.5(3) . . ? C7 C10 H10A 108.2 . . ? C11 C10 H10A 108.2 . . ? C7 C10 H10B 108.2 . . ? C11 C10 H10B 108.2 . . ? H10A C10 H10B 107.3 . . ? C10 C11 C17 113.0(3) . 1_645 ? C10 C11 H11A 109.0 . . ? C17 C11 H11A 109.0 1_645 . ? C10 C11 H11B 109.0 . . ? C17 C11 H11B 109.0 1_645 . ? H11A C11 H11B 107.8 . . ? N6 C12 C13 123.4(3) . . ? N6 C12 H12 118.3 . . ? C13 C12 H12 118.3 . . ? C12 C13 C14 120.8(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 116.0(3) . . ? C15 C14 C17 121.4(3) . . ? C13 C14 C17 122.6(3) . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? N6 C16 C15 123.8(3) . . ? N6 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? C14 C17 C11 113.8(3) . 1_465 ? C14 C17 H17A 108.8 . . ? C11 C17 H17A 108.8 1_465 . ? C14 C17 H17B 108.8 . . ? C11 C17 H17B 108.8 1_465 . ? H17A C17 H17B 107.7 . . ? N7 C18 C19 124.3(3) . . ? N7 C18 H18 117.9 . . ? C19 C18 H18 117.9 . . ? C18 C19 C20 120.0(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 117.2(3) . . ? C19 C20 C23 118.6(3) . . ? C21 C20 C23 124.1(3) . . ? C22 C21 C20 119.5(3) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? N7 C22 C21 123.1(3) . . ? N7 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C24 C23 C20 116.9(3) . . ? C24 C23 H23A 108.1 . . ? C20 C23 H23A 108.1 . . ? C24 C23 H23B 108.1 . . ? C20 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? C23 C24 C30 112.0(3) . 1_645 ? C23 C24 H24A 109.2 . . ? C30 C24 H24A 109.2 1_645 . ? C23 C24 H24B 109.2 . . ? C30 C24 H24B 109.2 1_645 . ? H24A C24 H24B 107.9 . . ? N8 C25 C26 123.6(3) . . ? N8 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? C25 C26 C27 120.3(3) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 116.2(3) . . ? C28 C27 C30 122.1(3) . . ? C26 C27 C30 121.8(3) . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? N8 C29 C28 123.7(3) . . ? N8 C29 H29 118.2 . . ? C28 C29 H29 118.2 . . ? C27 C30 C24 112.2(3) . 1_465 ? C27 C30 H30A 109.2 . . ? C24 C30 H30A 109.2 1_465 . ? C27 C30 H30B 109.2 . . ? C24 C30 H30B 109.2 1_465 . ? H30A C30 H30B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.674 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.054