# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Myoung Soo Lah' _publ_contact_author_address ; Chemistry and Applied Chemistry Hanyang University 1271 Sa-1-dong Ansan Kyunggi-do 426-791 SOUTH KOREA ; _publ_contact_author_email MSLAH@HANYANG.AC.KR _publ_section_title ; An unprecedented twofold interpenetrating (3,4)-connected 3-D metal-organic framework ; loop_ _publ_author_name 'Myoung Soo Lah.' 'Seunghee Hong.' 'Dohyun Moon.' 'Yang Zou.' # Attachment 'mslah_rev.CIF' data_p6_77or _database_code_depnum_ccdc_archive 'CCDC 631720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H72 Cu3 N30 O30' _chemical_formula_weight 2316.46 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 Orthorhombic _symmetry_space_group_name_H-M Pnna _symmetry_space_group_name_Hall -P2a2bc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 56.792(11) _cell_length_b 14.331(3) _cell_length_c 32.170(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26183(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13803 _cell_measurement_theta_min 1.23 _cell_measurement_theta_max 20.61 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4740 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.70000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Fixed gap multiple wiggler beamline' _diffrn_radiation_monochromator 'platinum coated silicon double crystal' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49789 _diffrn_reflns_av_R_equivalents 0.2134 _diffrn_reflns_av_sigmaI/netI 0.2164 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 20.61 _reflns_number_total 13803 _reflns_number_gt 4104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PAL ADSC Quantum-210' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEP3, Diamond 3.1a' _computing_publication_material WinGX _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^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00009(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13803 _refine_ls_number_parameters 660 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1664 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.1930 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 0.688 _refine_ls_restrained_S_all 0.688 _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 0.406143(15) 0.88210(5) 0.48232(4) 0.1543(5) Uani 1 1 d . . . O1N O 0.42279(9) 0.8810(4) 0.5613(3) 0.179(4) Uani 1 1 d . . . O2N O 0.44178(11) 0.8953(4) 0.6206(2) 0.157(2) Uani 1 1 d . . . O3N O 0.43883(9) 1.0146(4) 0.5787(2) 0.190(3) Uani 1 1 d . . . N1N N 0.43381(16) 0.9279(8) 0.5856(4) 0.168(4) Uani 1 1 d . . . Cu2 Cu 0.160322(18) 0.2500 0.7500 0.1172(5) Uani 1 2 d S . . O4N O 0.15970(6) 0.0784(3) 0.72964(15) 0.1449(17) Uani 1 1 d . . . O1A O 0.32916(12) 0.6073(4) 0.6061(3) 0.176(3) Uani 1 1 d . . . O2A O 0.26777(13) 0.4122(5) 0.6757(3) 0.315(5) Uani 1 1 d . . . O3A O 0.30319(9) 0.1535(3) 0.5246(2) 0.186(2) Uani 1 1 d . . . O4A O 0.39051(7) 0.8774(2) 0.4115(2) 0.229(4) Uani 1 1 d . . . N1A N 0.38277(11) 0.7889(3) 0.5051(4) 0.166(4) Uani 1 1 d . . . N2A N 0.18439(13) 0.2801(5) 0.71239(19) 0.133(3) Uani 1 1 d . . . N3A N 0.38476(12) -0.0158(4) 0.4985(3) 0.173(3) Uani 1 1 d . . . N4A N 0.33815(10) 0.5681(4) 0.5410(3) 0.137(2) Uani 1 1 d . . . H4A H 0.3356 0.5218 0.5236 0.165 Uiso 1 1 calc R . . N5A N 0.24391(11) 0.3184(3) 0.6286(2) 0.143(2) Uani 1 1 d . . . H5A H 0.2431 0.2834 0.6062 0.171 Uiso 1 1 calc R . . N6A N 0.34089(11) 0.2049(3) 0.5401(2) 0.165(3) Uani 1 1 d . . . H6A H 0.3489 0.2505 0.5518 0.198 Uiso 1 1 calc R . . C1A C 0.37283(16) 0.7859(7) 0.5450(3) 0.165(5) Uani 1 1 d . . . H1A H 0.3763 0.8341 0.5643 0.199 Uiso 1 1 calc R . . C2A C 0.35779(12) 0.7126(5) 0.5568(3) 0.149(4) Uani 1 1 d . . . H2A H 0.3515 0.7076 0.5841 0.179 Uiso 1 1 calc R . . C3A C 0.35254(13) 0.6452(5) 0.5245(4) 0.146(4) Uani 1 1 d . . . C4A C 0.36114(16) 0.6412(6) 0.4791(4) 0.187(5) Uani 1 1 d . . . H4A1 H 0.3571 0.5975 0.4581 0.225 Uiso 1 1 calc R . . C5A C 0.37726(12) 0.7222(8) 0.4761(3) 0.167(4) Uani 1 1 d . . . H5A1 H 0.3850 0.7290 0.4501 0.200 Uiso 1 1 calc R . . C6A C 0.32843(15) 0.5585(6) 0.5788(4) 0.127(3) Uani 1 1 d . . . C7A C 0.18794(11) 0.2488(6) 0.6780(3) 0.125(3) Uani 1 1 d . . . H7A H 0.1748 0.2130 0.6691 0.150 Uiso 1 1 calc R . . C8A C 0.20719(14) 0.2494(5) 0.6444(2) 0.131(3) Uani 1 1 d . . . H8A H 0.2073 0.2151 0.6192 0.157 Uiso 1 1 calc R . . C9A C 0.22499(14) 0.3126(5) 0.6591(3) 0.121(3) Uani 1 1 d . . . C10A C 0.22248(13) 0.3599(6) 0.6950(3) 0.135(3) Uani 1 1 d . . . H10A H 0.2341 0.4048 0.7023 0.162 Uiso 1 1 calc R . . C11A C 0.20456(15) 0.3464(4) 0.7207(3) 0.159(4) Uani 1 1 d . . . H11A H 0.2044 0.3806 0.7460 0.191 Uiso 1 1 calc R . . C12A C 0.2624(3) 0.3750(9) 0.6335(4) 0.212(5) Uiso 1 1 d . . . C13A C 0.39234(13) 0.0575(6) 0.5269(3) 0.183(4) Uani 1 1 d . . . H13A H 0.4081 0.0547 0.5368 0.219 Uiso 1 1 calc R . . C14A C 0.37870(14) 0.1298(5) 0.5404(3) 0.162(3) Uani 1 1 d . . . H14A H 0.3842 0.1774 0.5584 0.195 Uiso 1 1 calc R . . C15A C 0.35440(15) 0.1261(6) 0.5238(3) 0.147(3) Uani 1 1 d . . . C16A C 0.34517(13) 0.0563(6) 0.4960(3) 0.157(3) Uani 1 1 d . . . H16A H 0.3295 0.0578 0.4859 0.188 Uiso 1 1 calc R . . C17A C 0.36077(17) -0.0120(5) 0.4855(3) 0.166(3) Uani 1 1 d . . . H17A H 0.3552 -0.0610 0.4681 0.199 Uiso 1 1 calc R . . C18A C 0.31751(15) 0.2136(5) 0.5388(3) 0.171(4) Uani 1 1 d . . . C19A C 0.31441(13) 0.4626(5) 0.5791(3) 0.143(3) Uani 1 1 d . . . C20A C 0.29600(13) 0.4619(5) 0.6074(3) 0.163(4) Uani 1 1 d . . . H20A H 0.2926 0.5120 0.6258 0.196 Uiso 1 1 calc R . . C21A C 0.28302(14) 0.3790(6) 0.6059(3) 0.187(4) Uani 1 1 d . . . C22A C 0.28994(14) 0.2971(5) 0.5880(3) 0.156(3) Uani 1 1 d . . . H22A H 0.2824 0.2399 0.5948 0.187 Uiso 1 1 calc R . . C23A C 0.30882(12) 0.2999(5) 0.5590(3) 0.147(3) Uani 1 1 d . . . C24A C 0.32192(11) 0.3851(5) 0.5544(3) 0.146(3) Uani 1 1 d . . . H24A H 0.3349 0.3898 0.5359 0.176 Uiso 1 1 calc R . . O1B O 0.07793(9) 0.4578(4) 0.6183(2) 0.200(3) Uani 1 1 d . . . O2B O 0.00294(8) 0.6216(4) 0.5932(2) 0.184(2) Uani 1 1 d . . . O3B O 0.01226(9) 0.1458(3) 0.5368(2) 0.160(2) Uani 1 1 d . . . N1B N 0.13618(10) 0.2668(5) 0.70681(17) 0.1197(18) Uani 1 1 d . . . N2B N -0.06998(11) 0.7799(5) 0.5234(3) 0.146(3) Uani 1 1 d . . . N3B N -0.06914(12) -0.0222(4) 0.5336(3) 0.135(3) Uani 1 1 d . . . N4B N 0.07633(11) 0.3053(4) 0.6295(2) 0.152(3) Uani 1 1 d . . . H4B H 0.0685 0.2537 0.6241 0.183 Uiso 1 1 calc R . . N5B N -0.02286(11) 0.5569(4) 0.5463(2) 0.160(3) Uani 1 1 d . . . H5B H -0.0253 0.5087 0.5299 0.193 Uiso 1 1 calc R . . N6B N -0.02253(13) 0.2000(4) 0.5608(2) 0.166(3) Uani 1 1 d . . . H6B H -0.0290 0.2484 0.5731 0.200 Uiso 1 1 calc R . . C1B C 0.13318(13) 0.3417(5) 0.6832(3) 0.125(3) Uani 1 1 d . . . H1B H 0.1446 0.3896 0.6860 0.150 Uiso 1 1 calc R . . C2B C 0.11578(13) 0.3579(4) 0.6555(3) 0.119(2) Uani 1 1 d . . . H2B H 0.1159 0.4119 0.6384 0.143 Uiso 1 1 calc R . . C3B C 0.09745(16) 0.2925(5) 0.6528(3) 0.124(2) Uani 1 1 d . . . C4B C 0.09988(13) 0.2143(6) 0.6757(3) 0.137(3) Uani 1 1 d . . . H4B1 H 0.0883 0.1669 0.6723 0.164 Uiso 1 1 calc R . . C5B C 0.11754(13) 0.1977(5) 0.7034(3) 0.135(3) Uani 1 1 d . . . H5B1 H 0.1177 0.1428 0.7199 0.162 Uiso 1 1 calc R . . C6B C 0.06709(12) 0.3785(7) 0.6155(3) 0.147(3) Uani 1 1 d . . . C7B C -0.06786(13) 0.7094(6) 0.5000(3) 0.147(4) Uani 1 1 d . . . H7B H -0.0767 0.7076 0.4750 0.176 Uiso 1 1 calc R . . C8B C -0.05346(14) 0.6360(6) 0.5090(3) 0.143(3) Uani 1 1 d . . . H8B H -0.0536 0.5834 0.4909 0.172 Uiso 1 1 calc R . . C9B C -0.03855(14) 0.6347(6) 0.5436(3) 0.138(3) Uani 1 1 d . . . C10B C -0.03993(13) 0.7117(6) 0.5710(3) 0.173(4) Uani 1 1 d . . . H10B H -0.0304 0.7166 0.5952 0.208 Uiso 1 1 calc R . . C11B C -0.05672(14) 0.7818(5) 0.5594(4) 0.157(4) Uani 1 1 d . . . H11B H -0.0589 0.8330 0.5778 0.188 Uiso 1 1 calc R . . C12B C -0.00448(15) 0.5539(5) 0.5729(3) 0.146(3) Uani 1 1 d . . . C13B C -0.07507(13) 0.0463(7) 0.5585(3) 0.135(3) Uani 1 1 d . . . H13B H -0.0906 0.0458 0.5695 0.162 Uiso 1 1 calc R . . C14B C -0.06069(16) 0.1185(5) 0.5697(3) 0.140(3) Uani 1 1 d . . . H14B H -0.0653 0.1631 0.5900 0.168 Uiso 1 1 calc R . . C15B C -0.03838(18) 0.1232(6) 0.5493(3) 0.164(3) Uani 1 1 d . . . C16B C -0.03100(12) 0.0545(6) 0.5229(3) 0.165(3) Uani 1 1 d . . . H16B H -0.0155 0.0538 0.5117 0.198 Uiso 1 1 calc R . . C17B C -0.04874(18) -0.0197(5) 0.5128(3) 0.169(4) Uani 1 1 d . . . H17B H -0.0455 -0.0645 0.4918 0.203 Uiso 1 1 calc R . . C18B C 0.00092(14) 0.2036(6) 0.5543(3) 0.135(3) Uani 1 1 d . . . C19B C 0.04291(12) 0.3791(6) 0.5974(2) 0.145(3) Uani 1 1 d . . . C20B C 0.03049(15) 0.4616(5) 0.5948(3) 0.157(3) Uani 1 1 d . . . H20B H 0.0368 0.5169 0.6068 0.188 Uiso 1 1 calc R . . C21B C 0.00873(14) 0.4645(5) 0.5744(3) 0.147(3) Uani 1 1 d . . . C22B C -0.00175(11) 0.3793(6) 0.5642(2) 0.159(3) Uani 1 1 d . . . H22B H -0.0178 0.3784 0.5562 0.190 Uiso 1 1 calc R . . C23B C 0.01084(14) 0.2948(5) 0.5654(3) 0.144(3) Uani 1 1 d . . . C24B C 0.03180(16) 0.2917(4) 0.5852(3) 0.162(3) Uani 1 1 d . . . H24B H 0.0392 0.2337 0.5909 0.194 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 0.1037(6) 0.0775(5) 0.2817(13) 0.0023(7) 0.0572(8) 0.0016(5) O1N 0.073(4) 0.068(3) 0.397(12) -0.005(4) 0.008(5) -0.001(3) O2N 0.128(5) 0.116(4) 0.228(7) -0.026(5) 0.054(5) -0.026(4) O3N 0.142(4) 0.088(3) 0.340(8) 0.019(5) 0.012(5) -0.022(3) N1N 0.111(8) 0.166(12) 0.226(13) 0.040(10) 0.051(8) 0.048(7) Cu2 0.0679(7) 0.1103(8) 0.1733(13) 0.0222(9) 0.000 0.000 O4N 0.091(3) 0.125(3) 0.219(5) -0.026(3) -0.027(3) 0.014(2) O1A 0.139(5) 0.113(4) 0.276(9) -0.050(4) 0.074(5) -0.029(4) O2A 0.236(7) 0.220(6) 0.490(13) -0.110(7) 0.240(8) -0.129(5) O3A 0.095(4) 0.115(4) 0.348(8) -0.030(4) 0.038(5) 0.000(3) O4A 0.082(3) 0.073(3) 0.533(11) 0.057(4) 0.080(5) 0.010(2) N1A 0.114(5) 0.047(3) 0.337(13) -0.060(5) -0.042(7) 0.008(3) N2A 0.213(8) 0.145(6) 0.041(4) 0.040(4) 0.014(5) 0.107(6) N3A 0.086(5) 0.086(4) 0.346(10) 0.010(5) 0.015(5) -0.011(4) N4A 0.104(4) 0.085(4) 0.222(8) 0.012(4) 0.051(5) 0.005(4) N5A 0.089(4) 0.090(4) 0.249(8) 0.019(4) 0.037(5) 0.012(3) N6A 0.096(5) 0.093(4) 0.305(8) -0.029(4) 0.052(5) 0.012(4) C1A 0.136(7) 0.185(11) 0.176(9) -0.001(7) 0.081(7) 0.066(7) C2A 0.103(5) 0.075(5) 0.269(11) 0.032(7) 0.064(6) -0.023(4) C3A 0.098(5) 0.050(4) 0.289(13) -0.008(7) -0.043(7) -0.018(4) C4A 0.174(8) 0.138(8) 0.250(11) 0.052(7) 0.145(9) 0.019(6) C5A 0.088(5) 0.193(9) 0.218(10) 0.072(9) 0.043(6) -0.031(6) C6A 0.093(6) 0.116(9) 0.172(12) 0.018(7) 0.063(7) -0.017(6) C7A 0.060(4) 0.174(8) 0.141(8) 0.071(7) -0.013(5) -0.021(5) C8A 0.108(5) 0.116(5) 0.169(7) -0.024(5) 0.008(6) -0.040(5) C9A 0.104(7) 0.085(5) 0.174(9) 0.018(6) 0.066(7) 0.029(5) C10A 0.078(5) 0.143(7) 0.184(9) 0.012(6) 0.102(5) -0.001(5) C11A 0.115(6) 0.077(5) 0.284(13) -0.023(5) -0.014(8) -0.040(4) C13A 0.098(6) 0.079(5) 0.371(13) -0.004(7) 0.026(7) -0.011(5) C14A 0.090(6) 0.094(6) 0.303(11) 0.021(6) 0.042(7) 0.008(5) C15A 0.092(6) 0.107(6) 0.242(9) 0.005(6) 0.056(6) 0.022(6) C16A 0.099(6) 0.087(5) 0.284(11) -0.044(6) 0.031(6) -0.019(5) C17A 0.119(7) 0.120(6) 0.259(10) -0.021(6) 0.036(7) 0.011(6) C18A 0.071(6) 0.086(6) 0.357(13) -0.015(6) 0.081(7) 0.005(5) C19A 0.104(6) 0.071(5) 0.253(9) 0.012(6) 0.061(6) 0.002(4) C20A 0.119(6) 0.091(5) 0.279(10) 0.014(5) 0.119(7) -0.043(5) C21A 0.134(6) 0.112(6) 0.314(11) -0.050(7) 0.152(7) -0.010(6) C22A 0.124(7) 0.118(6) 0.225(9) -0.011(6) 0.067(6) 0.022(5) C23A 0.066(4) 0.092(6) 0.282(10) 0.007(6) 0.047(6) 0.022(5) C24A 0.096(5) 0.075(4) 0.268(9) 0.007(6) 0.043(5) 0.000(5) O1B 0.124(4) 0.120(4) 0.357(8) 0.011(4) -0.124(5) 0.006(3) O2B 0.126(4) 0.104(4) 0.321(7) -0.015(4) -0.103(4) 0.019(3) O3B 0.084(3) 0.090(3) 0.306(7) -0.022(4) -0.034(4) 0.004(3) N1B 0.139(5) 0.115(4) 0.105(5) 0.036(4) 0.014(4) -0.005(4) N2B 0.111(5) 0.094(5) 0.232(8) 0.000(5) -0.085(5) -0.012(4) N3B 0.094(5) 0.070(4) 0.243(8) -0.037(4) -0.016(5) 0.011(4) N4B 0.098(5) 0.083(4) 0.275(8) 0.021(4) -0.088(5) 0.006(3) N5B 0.117(5) 0.077(4) 0.288(8) 0.022(4) -0.119(5) 0.004(4) N6B 0.131(6) 0.077(4) 0.291(8) 0.013(4) -0.074(6) 0.005(4) C1B 0.108(6) 0.118(6) 0.151(7) 0.030(5) -0.051(6) 0.025(5) C2B 0.088(5) 0.090(5) 0.179(8) 0.061(5) -0.011(5) -0.002(4) C3B 0.126(7) 0.075(5) 0.172(8) 0.021(5) -0.016(6) 0.006(5) C4B 0.088(5) 0.153(7) 0.169(8) 0.056(6) -0.051(5) -0.018(5) C5B 0.092(5) 0.119(5) 0.193(9) 0.022(5) -0.032(6) -0.037(5) C6B 0.084(5) 0.094(5) 0.262(9) -0.011(7) -0.084(6) 0.004(5) C7B 0.123(6) 0.050(4) 0.266(11) -0.018(6) -0.025(6) 0.012(5) C8B 0.107(5) 0.120(7) 0.202(9) -0.025(6) -0.059(6) -0.010(5) C9B 0.108(6) 0.075(6) 0.231(10) 0.011(6) -0.062(7) -0.033(5) C10B 0.121(6) 0.067(5) 0.330(12) 0.010(7) -0.056(7) 0.002(5) C11B 0.088(5) 0.084(5) 0.298(13) 0.038(7) 0.008(7) 0.005(5) C12B 0.108(6) 0.073(6) 0.257(10) -0.029(6) -0.039(7) -0.003(5) C13B 0.100(6) 0.127(7) 0.178(8) -0.006(6) -0.017(5) 0.013(6) C14B 0.104(6) 0.068(4) 0.248(9) -0.026(5) 0.007(6) -0.024(5) C15B 0.123(8) 0.073(5) 0.296(11) -0.030(7) -0.030(8) 0.009(6) C16B 0.099(5) 0.080(5) 0.315(11) -0.021(7) -0.047(7) 0.004(5) C17B 0.120(7) 0.077(6) 0.310(12) 0.000(6) -0.037(8) 0.032(6) C18B 0.060(6) 0.122(8) 0.224(9) -0.030(6) -0.049(6) 0.014(5) C19B 0.106(6) 0.125(6) 0.205(8) 0.020(6) -0.087(5) 0.012(6) C20B 0.127(7) 0.088(5) 0.254(10) 0.003(5) -0.080(7) 0.009(5) C21B 0.097(6) 0.080(5) 0.262(9) -0.010(5) -0.074(6) 0.012(5) C22B 0.091(5) 0.096(5) 0.288(10) -0.007(6) -0.077(6) -0.006(5) C23B 0.098(6) 0.076(5) 0.258(9) -0.014(5) -0.110(6) 0.008(5) C24B 0.141(7) 0.068(5) 0.276(10) -0.004(5) -0.072(7) -0.013(5) _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 N3A 1.971(6) 1_565 ? Cu1 N2B 2.005(7) 6_656 ? Cu1 N1A 2.020(8) . ? Cu1 N3B 2.028(6) 6_666 ? Cu1 O4A 2.447(8) . ? Cu1 O1N 2.711(9) . ? O1N N1N 1.206(11) . ? O2N N1N 1.301(9) . ? O3N N1N 1.295(11) . ? Cu2 N2A 1.876(7) 4_556 ? Cu2 N2A 1.876(7) . ? Cu2 N1B 1.967(6) . ? Cu2 N1B 1.967(6) 4_556 ? Cu2 O4N 2.545(4) . ? O1A C6A 1.124(9) . ? O2A C12A 1.490(11) . ? O3A C18A 1.269(8) . ? N1A C5A 1.370(10) . ? N1A C1A 1.404(9) . ? N2A C7A 1.209(8) . ? N2A C11A 1.512(8) . ? N3A C17A 1.426(9) . ? N3A C13A 1.457(9) . ? N3A Cu1 1.971(6) 1_545 ? N4A C6A 1.342(9) . ? N4A C3A 1.473(9) . ? N5A C12A 1.337(13) . ? N5A C9A 1.457(9) . ? N6A C18A 1.334(8) . ? N6A C15A 1.462(8) . ? C1A C2A 1.407(9) . ? C2A C3A 1.450(10) . ? C3A C4A 1.543(11) . ? C4A C5A 1.481(11) . ? C6A C19A 1.589(11) . ? C7A C8A 1.537(10) . ? C8A C9A 1.437(9) . ? C9A C10A 1.347(9) . ? C10A C11A 1.324(9) . ? C12A C21A 1.470(14) . ? C13A C14A 1.365(8) . ? C14A C15A 1.480(10) . ? C15A C16A 1.440(10) . ? C16A C17A 1.364(8) . ? C18A C23A 1.482(9) . ? C19A C20A 1.388(8) . ? C19A C24A 1.430(8) . ? C20A C21A 1.400(8) . ? C21A C22A 1.364(8) . ? C22A C23A 1.422(9) . ? C23A C24A 1.439(8) . ? O1B C6B 1.297(7) . ? O2B C12B 1.244(7) . ? O3B C18B 1.191(8) . ? N1B C1B 1.327(7) . ? N1B C5B 1.453(7) . ? N2B C7B 1.265(8) . ? N2B C11B 1.383(9) . ? N2B Cu1 2.005(7) 6_556 ? N3B C13B 1.311(8) . ? N3B C17B 1.339(9) . ? N3B Cu1 2.028(6) 6_546 ? N4B C6B 1.257(7) . ? N4B C3B 1.425(9) . ? N5B C12B 1.350(9) . ? N5B C9B 1.430(8) . ? N6B C18B 1.349(8) . ? N6B C15B 1.469(9) . ? C1B C2B 1.351(8) . ? C2B C3B 1.403(8) . ? C3B C4B 1.350(8) . ? C4B C5B 1.362(8) . ? C6B C19B 1.490(8) . ? C7B C8B 1.364(8) . ? C8B C9B 1.400(9) . ? C9B C10B 1.414(10) . ? C10B C11B 1.434(8) . ? C12B C21B 1.484(8) . ? C13B C14B 1.367(8) . ? C14B C15B 1.427(10) . ? C15B C16B 1.365(10) . ? C16B C17B 1.500(9) . ? C18B C23B 1.468(9) . ? C19B C20B 1.380(8) . ? C19B C24B 1.457(8) . ? C20B C21B 1.399(8) . ? C21B C22B 1.398(8) . ? C22B C23B 1.406(8) . ? C23B C24B 1.350(8) . ? 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 N3A Cu1 N2B 169.5(4) 1_565 6_656 ? N3A Cu1 N1A 89.5(3) 1_565 . ? N2B Cu1 N1A 89.7(3) 6_656 . ? N3A Cu1 N3B 89.5(2) 1_565 6_666 ? N2B Cu1 N3B 90.2(3) 6_656 6_666 ? N1A Cu1 N3B 173.3(4) . 6_666 ? N3A Cu1 O4A 92.4(3) 1_565 . ? N2B Cu1 O4A 98.1(3) 6_656 . ? N1A Cu1 O4A 94.6(3) . . ? N3B Cu1 O4A 92.0(3) 6_666 . ? N3A Cu1 O1N 88.4(3) 1_565 . ? N2B Cu1 O1N 81.1(3) 6_656 . ? N1A Cu1 O1N 83.4(3) . . ? N3B Cu1 O1N 90.0(3) 6_666 . ? O4A Cu1 O1N 177.90(14) . . ? N1N O1N Cu1 141.7(8) . . ? O1N N1N O3N 122.6(11) . . ? O1N N1N O2N 122.8(13) . . ? O3N N1N O2N 114.6(12) . . ? N2A Cu2 N2A 86.4(4) 4_556 . ? N2A Cu2 N1B 172.7(3) 4_556 . ? N2A Cu2 N1B 91.4(2) . . ? N2A Cu2 N1B 91.4(2) 4_556 4_556 ? N2A Cu2 N1B 172.7(3) . 4_556 ? N1B Cu2 N1B 91.6(3) . 4_556 ? N2A Cu2 O4N 87.4(2) 4_556 . ? N2A Cu2 O4N 93.8(2) . . ? N1B Cu2 O4N 85.8(2) . . ? N1B Cu2 O4N 93.1(2) 4_556 . ? C5A N1A C1A 120.5(8) . . ? C5A N1A Cu1 111.4(8) . . ? C1A N1A Cu1 128.0(7) . . ? C7A N2A C11A 105.5(8) . . ? C7A N2A Cu2 128.8(8) . . ? C11A N2A Cu2 125.6(6) . . ? C17A N3A C13A 116.0(6) . . ? C17A N3A Cu1 122.7(6) . 1_545 ? C13A N3A Cu1 121.2(6) . 1_545 ? C6A N4A C3A 129.0(8) . . ? C12A N5A C9A 122.4(9) . . ? C18A N6A C15A 125.7(7) . . ? N1A C1A C2A 121.0(10) . . ? C1A C2A C3A 115.4(9) . . ? C2A C3A N4A 110.9(10) . . ? C2A C3A C4A 129.7(8) . . ? N4A C3A C4A 119.2(8) . . ? C5A C4A C3A 103.1(9) . . ? N1A C5A C4A 130.1(9) . . ? O1A C6A N4A 129.1(10) . . ? O1A C6A C19A 123.5(10) . . ? N4A C6A C19A 107.5(9) . . ? N2A C7A C8A 139.4(8) . . ? C9A C8A C7A 105.8(7) . . ? C10A C9A C8A 121.6(8) . . ? C10A C9A N5A 128.8(8) . . ? C8A C9A N5A 109.5(9) . . ? C11A C10A C9A 122.8(9) . . ? C10A C11A N2A 124.3(9) . . ? N5A C12A C21A 125.4(12) . . ? N5A C12A O2A 118.9(12) . . ? C21A C12A O2A 112.0(12) . . ? C14A C13A N3A 125.4(7) . . ? C13A C14A C15A 112.8(8) . . ? C16A C15A N6A 124.6(8) . . ? C16A C15A C14A 126.0(7) . . ? N6A C15A C14A 109.4(9) . . ? C17A C16A C15A 114.6(7) . . ? C16A C17A N3A 125.1(8) . . ? O3A C18A N6A 125.9(7) . . ? O3A C18A C23A 120.7(7) . . ? N6A C18A C23A 113.3(8) . . ? C20A C19A C24A 125.8(6) . . ? C20A C19A C6A 112.8(8) . . ? C24A C19A C6A 121.3(8) . . ? C19A C20A C21A 112.3(7) . . ? C22A C21A C20A 126.5(7) . . ? C22A C21A C12A 116.8(9) . . ? C20A C21A C12A 115.4(9) . . ? C21A C22A C23A 118.0(7) . . ? C22A C23A C24A 118.8(7) . . ? C22A C23A C18A 121.1(7) . . ? C24A C23A C18A 119.4(7) . . ? C19A C24A C23A 116.6(6) . . ? C1B N1B C5B 114.5(6) . . ? C1B N1B Cu2 126.4(5) . . ? C5B N1B Cu2 118.6(5) . . ? C7B N2B C11B 117.6(7) . . ? C7B N2B Cu1 126.4(7) . 6_556 ? C11B N2B Cu1 115.5(6) . 6_556 ? C13B N3B C17B 120.5(7) . . ? C13B N3B Cu1 118.9(7) . 6_546 ? C17B N3B Cu1 119.4(7) . 6_546 ? C6B N4B C3B 130.3(6) . . ? C12B N5B C9B 123.1(7) . . ? C18B N6B C15B 126.5(7) . . ? N1B C1B C2B 127.6(7) . . ? C1B C2B C3B 118.0(7) . . ? C4B C3B C2B 116.4(8) . . ? C4B C3B N4B 118.7(8) . . ? C2B C3B N4B 124.8(7) . . ? C3B C4B C5B 125.3(8) . . ? C4B C5B N1B 117.9(6) . . ? N4B C6B O1B 120.6(6) . . ? N4B C6B C19B 122.0(8) . . ? O1B C6B C19B 117.3(8) . . ? N2B C7B C8B 123.2(9) . . ? C7B C8B C9B 122.8(8) . . ? C8B C9B C10B 116.9(8) . . ? C8B C9B N5B 115.8(9) . . ? C10B C9B N5B 127.2(8) . . ? C9B C10B C11B 115.0(8) . . ? N2B C11B C10B 124.4(8) . . ? O2B C12B N5B 124.7(7) . . ? O2B C12B C21B 119.0(8) . . ? N5B C12B C21B 116.1(7) . . ? N3B C13B C14B 125.1(7) . . ? C13B C14B C15B 116.4(8) . . ? C16B C15B C14B 121.6(8) . . ? C16B C15B N6B 120.5(9) . . ? C14B C15B N6B 117.6(9) . . ? C15B C16B C17B 116.1(8) . . ? N3B C17B C16B 119.5(8) . . ? O3B C18B N6B 125.5(8) . . ? O3B C18B C23B 121.8(7) . . ? N6B C18B C23B 112.1(8) . . ? C20B C19B C24B 119.9(6) . . ? C20B C19B C6B 120.1(8) . . ? C24B C19B C6B 119.9(8) . . ? C19B C20B C21B 120.4(6) . . ? C22B C21B C20B 117.4(6) . . ? C22B C21B C12B 122.0(7) . . ? C20B C21B C12B 119.2(7) . . ? C21B C22B C23B 122.0(6) . . ? C24B C23B C22B 119.3(6) . . ? C24B C23B C18B 115.1(7) . . ? C22B C23B C18B 124.4(7) . . ? C23B C24B C19B 118.8(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4B H4B O2N 0.88 2.22 3.066(8) 162.3 2_565 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 20.61 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.212 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.039