# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email mohamed.eddaoudi@kaust.edu.sa _publ_contact_author_name 'Mohamed Eddaoudi' loop_ _publ_author_name 'Mohamed Eddaoudi' 'Ryan Luebke' 'Jarrod Eubank' 'Amy Cairns' 'Youssef Belmabkhout' 'Lukasz Wojtas' data_me948_0m _database_code_depnum_ccdc_archive 'CCDC 846266' #TrackingRef '- rht-MOF-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H12 Cu3 N6 O15' _chemical_formula_weight 851.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 26.6700(3) _cell_length_b 26.6700(3) _cell_length_c 38.0416(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 27058.6(8) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2921 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 62.0 _exptl_crystal_description octahedron _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6768 _exptl_absorpt_coefficient_mu 1.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8689 _exptl_absorpt_correction_T_max 0.8689 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXII CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44425 _diffrn_reflns_av_R_equivalents 0.1105 _diffrn_reflns_av_sigmaI/netI 0.1097 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 65.45 _reflns_number_total 10968 _reflns_number_gt 6194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'APEX2 (Bruker, 2010)' _publ_section_references ; Bruker AXS. (2010). APEX2 Bruker AXS, Inc. Madison, Wisconsin, USA. Bruker AXS. (2009). SAINT Bruker AXS, Inc. Madison, Wisconsin, USA. Sheldrick, G. M. (2008). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; _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^)+(0.0400P)^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 10968 _refine_ls_number_parameters 466 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.000 _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 0.15909(2) 0.23140(2) 0.197284(13) 0.03186(17) Uani 1 1 d . . . Cu2 Cu 0.11917(2) 0.17426(2) 0.148019(13) 0.03101(17) Uani 1 1 d . . . Cu3 Cu 0.39183(3) 0.06653(3) 0.0000 0.0340(2) Uani 1 2 d S . . Cu4 Cu 0.29457(3) 0.04998(3) 0.0000 0.0311(2) Uani 1 2 d S . . C1 C 0.33235(18) 0.11982(17) 0.04884(10) 0.0353(11) Uani 1 1 d . . . C2 C 0.22156(18) 0.19632(17) 0.14073(10) 0.0396(11) Uani 1 1 d . . . C3 C 0.27729(17) 0.16134(16) 0.09407(10) 0.0389(11) Uani 1 1 d . . . H3 H 0.2485 0.1491 0.0821 0.047 Uiso 1 1 calc R . . C4 C 0.32539(16) 0.15153(17) 0.08111(10) 0.0378(11) Uani 1 1 d . . . C5 C 0.27223(16) 0.18930(17) 0.12486(10) 0.0381(11) Uani 1 1 d . . . C6 C 0.36660(17) 0.17077(19) 0.09814(11) 0.0529(14) Uani 1 1 d . . . H6 H 0.3989 0.1656 0.0883 0.063 Uiso 1 1 calc R . . C7 C 0.36235(17) 0.19765(19) 0.12941(11) 0.0511(14) Uani 1 1 d . . . C8 C 0.31378(17) 0.20734(18) 0.14225(11) 0.0468(13) Uani 1 1 d . . . H8 H 0.3096 0.2265 0.1631 0.056 Uiso 1 1 calc R . . N4 N 0.47757(16) 0.22988(17) 0.17393(10) 0.0647(13) Uani 1 1 d . . . N5 N 0.54881(15) 0.18558(17) 0.15342(11) 0.0667(13) Uani 1 1 d . . . C11 C 0.4511(2) 0.2038(2) 0.15067(12) 0.0724(18) Uani 1 1 d . . . C12 C 0.51915(19) 0.1604(2) 0.13162(12) 0.0549(14) Uani 1 1 d . . . N6 N 0.46925(15) 0.16678(16) 0.12926(10) 0.0559(12) Uani 1 1 d . . . C14 C 0.5261(2) 0.2180(2) 0.17510(12) 0.0645(17) Uani 1 1 d . . . C15 C 0.67378(17) 0.10029(17) 0.11837(10) 0.0398(11) Uani 1 1 d DU . . C16 C 0.63896(17) 0.04820(17) 0.07362(10) 0.0378(11) Uani 1 1 d . . . C17 C 0.64449(19) 0.00877(17) 0.04656(10) 0.0400(12) Uani 1 1 d . . . C18 C 0.68004(16) 0.06519(17) 0.09184(10) 0.0394(11) Uani 1 1 d . . . H18 H 0.7126 0.0530 0.0863 0.047 Uiso 1 1 calc R . . C19 C 0.59250(16) 0.06868(17) 0.08088(10) 0.0425(12) Uani 1 1 d . . . H19 H 0.5642 0.0571 0.0680 0.051 Uiso 1 1 calc R . . C20 C 0.62870(18) 0.1187(2) 0.12554(12) 0.0590(14) Uani 1 1 d DU . . H20 H 0.6254 0.1418 0.1444 0.071 Uiso 1 1 calc R . . C21 C 0.58544(18) 0.1055(2) 0.10619(11) 0.0513(14) Uani 1 1 d . . . C23 C 0.57953(16) 0.31450(16) 0.27688(10) 0.0381(11) Uani 1 1 d . . . C24 C 0.49874(17) 0.26794(18) 0.24515(12) 0.0495(13) Uani 1 1 d . . . H24 H 0.4710 0.2515 0.2346 0.059 Uiso 1 1 calc R . . C25 C 0.54595(18) 0.2661(2) 0.22915(11) 0.0544(14) Uani 1 1 d . . . C26 C 0.58639(17) 0.28836(19) 0.24549(11) 0.0513(14) Uani 1 1 d . . . H26 H 0.6189 0.2859 0.2354 0.062 Uiso 1 1 calc R . . C27 C 0.53362(16) 0.31743(16) 0.29240(10) 0.0358(11) Uani 1 1 d . . . H27 H 0.5291 0.3352 0.3138 0.043 Uiso 1 1 calc R . . C28 C 0.62563(18) 0.33503(16) 0.29524(11) 0.0396(11) Uani 1 1 d . . . C29 C 0.71875(18) 0.11693(17) 0.13929(11) 0.0400(11) Uani 1 1 d . . . C30 C 0.44227(18) 0.29435(18) 0.29379(11) 0.0427(12) Uani 1 1 d U . . C31 C 0.49259(16) 0.29314(17) 0.27572(10) 0.0400(11) Uani 1 1 d . . . N1 N 0.40219(14) 0.21594(18) 0.14954(10) 0.0713(15) Uani 1 1 d . . . H1N H 0.3937 0.2399 0.1642 0.086 Uiso 1 1 calc R . . N2 N 0.53662(14) 0.12411(17) 0.11055(10) 0.0659(14) Uani 1 1 d . . . H2N H 0.5138 0.1096 0.0973 0.079 Uiso 1 1 calc R . . N3 N 0.55701(14) 0.24019(18) 0.19770(11) 0.0761(15) Uani 1 1 d . . . H3N H 0.5890 0.2385 0.1923 0.091 Uiso 1 1 calc R . . O2 O 0.21390(18) 0.0375(2) 0.0000 0.098(2) Uani 1 2 d S . . O3 O 0.47020(19) 0.0830(2) 0.0000 0.0960(19) Uani 1 2 d S . . O4 O 0.60621(11) -0.01369(12) 0.03611(7) 0.0492(8) Uani 1 1 d . . . O5 O 0.37518(11) 0.11415(12) 0.03715(7) 0.0450(8) Uani 1 1 d . . . O6 O 0.29263(11) 0.10120(11) 0.03658(7) 0.0436(8) Uani 1 1 d . . . O7 O 0.61757(11) 0.35554(11) 0.32516(7) 0.0461(8) Uani 1 1 d . . . O8 O 0.66679(11) 0.32960(11) 0.28012(7) 0.0430(8) Uani 1 1 d . . . O9 O 0.40852(11) 0.26721(11) 0.28172(7) 0.0412(8) Uani 1 1 d . . . O10 O 0.43862(10) 0.32246(11) 0.32081(7) 0.0418(8) Uani 1 1 d U . . O11 O 0.76143(11) 0.10114(11) 0.12872(7) 0.0439(8) Uani 1 1 d . . . O12 O 0.71187(11) 0.14261(11) 0.16663(7) 0.0438(8) Uani 1 1 d . . . O13 O 0.07556(17) 0.13566(15) 0.10817(8) 0.0910(14) Uani 1 1 d . . . O14 O 0.20032(15) 0.27185(15) 0.23781(10) 0.0874(13) Uani 1 1 d . . . O15 O 0.68913(11) -0.00009(12) 0.03622(7) 0.0476(8) Uani 1 1 d . . . O16 O 0.21956(10) 0.22026(11) 0.16919(7) 0.0420(8) Uani 1 1 d . . . O17 O 0.18448(11) 0.17781(11) 0.12497(7) 0.0424(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0318(4) 0.0308(4) 0.0331(3) -0.0041(3) -0.0055(3) 0.0026(3) Cu2 0.0301(4) 0.0293(4) 0.0336(3) -0.0034(3) -0.0070(3) 0.0033(3) Cu3 0.0299(5) 0.0424(6) 0.0295(4) 0.000 0.000 -0.0030(5) Cu4 0.0278(5) 0.0390(6) 0.0263(4) 0.000 0.000 -0.0011(4) C1 0.027(3) 0.046(3) 0.033(2) 0.000(2) -0.006(2) -0.001(2) C2 0.041(3) 0.039(3) 0.039(2) 0.003(2) -0.004(2) 0.004(3) C3 0.034(3) 0.047(3) 0.036(2) -0.011(2) -0.009(2) 0.008(2) C4 0.025(3) 0.057(3) 0.032(2) -0.014(2) -0.0001(19) -0.004(2) C5 0.021(3) 0.052(3) 0.041(2) -0.009(2) -0.007(2) 0.012(2) C6 0.026(3) 0.087(4) 0.045(2) -0.020(3) 0.006(2) 0.009(3) C7 0.030(3) 0.073(4) 0.050(3) -0.031(3) -0.005(2) 0.008(3) C8 0.036(3) 0.059(3) 0.046(2) -0.028(2) -0.007(2) 0.000(3) N4 0.039(3) 0.092(4) 0.064(3) -0.038(3) -0.005(2) -0.007(3) N5 0.041(3) 0.089(4) 0.070(3) -0.042(3) -0.008(2) -0.003(3) C11 0.038(3) 0.133(6) 0.046(3) -0.043(3) -0.007(2) -0.006(4) C12 0.033(3) 0.076(4) 0.057(3) -0.026(3) -0.007(2) 0.007(3) N6 0.033(3) 0.077(3) 0.058(2) -0.028(2) -0.008(2) 0.004(2) C14 0.034(3) 0.104(5) 0.055(3) -0.045(3) 0.001(3) -0.003(3) C15 0.035(3) 0.040(3) 0.044(2) -0.007(2) -0.008(2) -0.001(2) C16 0.031(3) 0.050(3) 0.033(2) -0.017(2) 0.002(2) 0.001(2) C17 0.038(3) 0.044(3) 0.038(2) 0.001(2) -0.002(2) -0.003(3) C18 0.029(3) 0.047(3) 0.042(2) -0.009(2) -0.003(2) -0.001(2) C19 0.029(3) 0.056(3) 0.042(2) -0.016(2) -0.002(2) -0.020(3) C20 0.049(3) 0.078(4) 0.050(3) -0.018(3) -0.003(3) -0.011(3) C21 0.030(3) 0.074(4) 0.049(3) -0.025(3) -0.003(2) 0.000(3) C23 0.034(3) 0.041(3) 0.040(2) -0.015(2) -0.011(2) 0.003(2) C24 0.030(3) 0.059(4) 0.060(3) -0.025(3) -0.013(2) 0.000(3) C25 0.033(3) 0.078(4) 0.053(3) -0.038(3) -0.006(2) -0.003(3) C26 0.025(3) 0.073(4) 0.055(3) -0.027(3) -0.003(2) 0.003(3) C27 0.035(3) 0.044(3) 0.0293(19) -0.0121(19) -0.001(2) -0.001(2) C28 0.041(3) 0.030(3) 0.048(3) -0.002(2) -0.004(2) 0.000(2) C29 0.040(3) 0.033(3) 0.047(3) -0.001(2) 0.000(2) 0.000(3) C30 0.040(3) 0.036(3) 0.052(3) 0.005(2) -0.011(2) 0.001(3) C31 0.029(3) 0.049(3) 0.043(2) -0.003(2) 0.003(2) 0.005(2) N1 0.017(2) 0.129(4) 0.068(3) -0.063(3) -0.006(2) 0.004(3) N2 0.025(3) 0.109(4) 0.064(2) -0.059(3) -0.0084(19) 0.005(3) N3 0.018(2) 0.130(4) 0.080(3) -0.067(3) -0.007(2) 0.004(3) O2 0.026(3) 0.087(4) 0.181(6) 0.000 0.000 -0.020(3) O3 0.045(4) 0.145(6) 0.098(4) 0.000 0.000 -0.011(4) O4 0.0261(19) 0.066(2) 0.0556(17) -0.0258(17) -0.0064(15) 0.0020(17) O5 0.0262(19) 0.066(2) 0.0429(15) -0.0149(15) 0.0028(14) -0.0061(17) O6 0.038(2) 0.056(2) 0.0375(14) -0.0155(14) -0.0025(14) -0.0003(17) O7 0.041(2) 0.059(2) 0.0378(15) -0.0179(15) 0.0052(14) -0.0091(17) O8 0.0294(19) 0.059(2) 0.0408(15) -0.0184(15) 0.0044(14) -0.0068(16) O9 0.0309(18) 0.045(2) 0.0482(16) -0.0141(15) -0.0017(14) -0.0022(16) O10 0.0336(19) 0.048(2) 0.0436(15) -0.0155(15) -0.0026(14) -0.0072(16) O11 0.031(2) 0.049(2) 0.0512(17) -0.0215(15) -0.0027(15) -0.0053(16) O12 0.0319(18) 0.048(2) 0.0511(17) -0.0189(15) 0.0009(14) 0.0034(16) O13 0.153(4) 0.081(3) 0.0385(17) -0.0245(18) 0.002(2) -0.069(3) O14 0.087(3) 0.092(3) 0.083(2) -0.038(2) -0.030(2) 0.000(2) O15 0.033(2) 0.062(2) 0.0480(16) -0.0152(16) 0.0038(15) 0.0006(17) O16 0.0346(19) 0.052(2) 0.0392(15) -0.0147(15) -0.0016(13) 0.0056(16) O17 0.0300(18) 0.057(2) 0.0399(15) -0.0109(15) -0.0019(14) -0.0037(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 O8 1.949(3) 16_545 ? Cu1 O16 1.957(3) . ? Cu1 O12 1.960(3) 4_565 ? Cu1 O9 1.972(3) 13 ? Cu1 O14 2.180(3) . ? Cu1 Cu2 2.6397(8) . ? Cu2 O11 1.927(3) 4_565 ? Cu2 O7 1.945(3) 16_545 ? Cu2 O10 1.947(3) 13 ? Cu2 O17 1.952(3) . ? Cu2 O13 2.170(3) . ? Cu3 O5 1.951(3) . ? Cu3 O5 1.951(3) 10 ? Cu3 O4 1.969(3) 2_655 ? Cu3 O4 1.969(3) 9_655 ? Cu3 O3 2.136(5) . ? Cu3 Cu4 2.6312(11) . ? Cu4 O6 1.951(3) . ? Cu4 O6 1.951(3) 10 ? Cu4 O15 1.964(3) 9_655 ? Cu4 O15 1.964(3) 2_655 ? Cu4 O2 2.177(5) . ? C1 O5 1.235(5) . ? C1 O6 1.259(5) . ? C1 C4 1.502(5) . ? C2 O16 1.258(5) . ? C2 O17 1.258(5) . ? C2 C5 1.492(6) . ? C3 C5 1.395(5) . ? C3 C4 1.399(6) . ? C3 H3 0.9500 . ? C4 C6 1.375(6) . ? C5 C8 1.377(6) . ? C6 C7 1.393(6) . ? C6 H6 0.9500 . ? C7 N1 1.398(5) . ? C7 C8 1.408(6) . ? C8 H8 0.9500 . ? N4 C11 1.330(6) . ? N4 C14 1.334(6) . ? N5 C12 1.328(6) . ? N5 C14 1.339(6) . ? C11 N1 1.344(6) . ? C11 N6 1.368(6) . ? C12 N2 1.341(6) . ? C12 N6 1.344(6) . ? C14 N3 1.329(6) . ? C15 C20 1.327(5) . ? C15 C18 1.387(6) . ? C15 C29 1.506(6) . ? C16 C18 1.373(6) . ? C16 C19 1.382(6) . ? C16 C17 1.479(6) . ? C17 O4 1.249(5) . ? C17 O15 1.276(5) . ? C18 H18 0.9500 . ? C19 C21 1.387(6) . ? C19 H19 0.9500 . ? C20 C21 1.414(6) . ? C20 H20 0.9500 . ? C21 N2 1.404(6) . ? C23 C27 1.361(6) . ? C23 C26 1.395(6) . ? C23 C28 1.516(6) . ? C24 C31 1.353(6) . ? C24 C25 1.399(6) . ? C24 H24 0.9500 . ? C25 C26 1.379(6) . ? C25 N3 1.413(5) . ? C26 H26 0.9500 . ? C27 C31 1.421(6) . ? C27 H27 0.9500 . ? C28 O8 1.248(5) . ? C28 O7 1.281(5) . ? C29 O12 1.259(5) . ? C29 O11 1.279(5) . ? C30 O9 1.243(5) . ? C30 O10 1.276(5) . ? C30 C31 1.508(6) . ? N1 H1N 0.8800 . ? N2 H2N 0.8800 . ? N3 H3N 0.8800 . ? O4 Cu3 1.969(3) 9_655 ? O7 Cu2 1.945(3) 15 ? O8 Cu1 1.949(3) 15 ? O9 Cu1 1.972(3) 13 ? O10 Cu2 1.947(3) 13 ? O11 Cu2 1.927(3) 3_655 ? O12 Cu1 1.960(3) 3_655 ? O15 Cu4 1.964(3) 9_655 ? 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 O8 Cu1 O16 88.80(13) 16_545 . ? O8 Cu1 O12 168.37(12) 16_545 4_565 ? O16 Cu1 O12 88.69(12) . 4_565 ? O8 Cu1 O9 88.83(13) 16_545 13 ? O16 Cu1 O9 167.73(12) . 13 ? O12 Cu1 O9 91.22(13) 4_565 13 ? O8 Cu1 O14 92.73(14) 16_545 . ? O16 Cu1 O14 92.62(14) . . ? O12 Cu1 O14 98.73(14) 4_565 . ? O9 Cu1 O14 99.52(14) 13 . ? O8 Cu1 Cu2 82.25(8) 16_545 . ? O16 Cu1 Cu2 81.78(8) . . ? O12 Cu1 Cu2 86.15(8) 4_565 . ? O9 Cu1 Cu2 85.97(9) 13 . ? O14 Cu1 Cu2 172.53(11) . . ? O11 Cu2 O7 168.12(12) 4_565 16_545 ? O11 Cu2 O10 89.69(13) 4_565 13 ? O7 Cu2 O10 89.42(13) 16_545 13 ? O11 Cu2 O17 90.48(13) 4_565 . ? O7 Cu2 O17 87.93(13) 16_545 . ? O10 Cu2 O17 167.90(12) 13 . ? O11 Cu2 O13 91.28(14) 4_565 . ? O7 Cu2 O13 100.58(14) 16_545 . ? O10 Cu2 O13 91.29(13) 13 . ? O17 Cu2 O13 100.80(13) . . ? O11 Cu2 Cu1 81.80(9) 4_565 . ? O7 Cu2 Cu1 86.35(8) 16_545 . ? O10 Cu2 Cu1 82.01(8) 13 . ? O17 Cu2 Cu1 86.04(9) . . ? O13 Cu2 Cu1 170.35(13) . . ? O5 Cu3 O5 92.82(18) . 10 ? O5 Cu3 O4 88.09(13) . 2_655 ? O5 Cu3 O4 167.78(13) 10 2_655 ? O5 Cu3 O4 167.78(13) . 9_655 ? O5 Cu3 O4 88.09(13) 10 9_655 ? O4 Cu3 O4 88.49(19) 2_655 9_655 ? O5 Cu3 O3 95.11(15) . . ? O5 Cu3 O3 95.11(15) 10 . ? O4 Cu3 O3 96.94(16) 2_655 . ? O4 Cu3 O3 96.94(16) 9_655 . ? O5 Cu3 Cu4 83.39(9) . . ? O5 Cu3 Cu4 83.39(9) 10 . ? O4 Cu3 Cu4 84.61(9) 2_655 . ? O4 Cu3 Cu4 84.61(9) 9_655 . ? O3 Cu3 Cu4 177.81(18) . . ? O6 Cu4 O6 91.02(18) . 10 ? O6 Cu4 O15 168.72(13) . 9_655 ? O6 Cu4 O15 88.84(13) 10 9_655 ? O6 Cu4 O15 88.84(13) . 2_655 ? O6 Cu4 O15 168.72(13) 10 2_655 ? O15 Cu4 O15 89.10(18) 9_655 2_655 ? O6 Cu4 O2 94.63(14) . . ? O6 Cu4 O2 94.63(14) 10 . ? O15 Cu4 O2 96.63(15) 9_655 . ? O15 Cu4 O2 96.63(15) 2_655 . ? O6 Cu4 Cu3 84.76(9) . . ? O6 Cu4 Cu3 84.76(9) 10 . ? O15 Cu4 Cu3 84.00(9) 9_655 . ? O15 Cu4 Cu3 84.00(9) 2_655 . ? O2 Cu4 Cu3 179.12(16) . . ? O5 C1 O6 126.6(4) . . ? O5 C1 C4 118.5(4) . . ? O6 C1 C4 114.9(4) . . ? O16 C2 O17 125.2(4) . . ? O16 C2 C5 116.8(4) . . ? O17 C2 C5 118.0(4) . . ? C5 C3 C4 119.0(4) . . ? C5 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C6 C4 C3 119.8(4) . . ? C6 C4 C1 119.8(4) . . ? C3 C4 C1 120.4(4) . . ? C8 C5 C3 120.8(4) . . ? C8 C5 C2 119.4(4) . . ? C3 C5 C2 119.6(4) . . ? C4 C6 C7 121.9(4) . . ? C4 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 N1 125.8(4) . . ? C6 C7 C8 117.7(4) . . ? N1 C7 C8 116.4(4) . . ? C5 C8 C7 120.6(4) . . ? C5 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C11 N4 C14 114.5(4) . . ? C12 N5 C14 116.2(4) . . ? N4 C11 N1 114.2(5) . . ? N4 C11 N6 125.8(5) . . ? N1 C11 N6 120.0(4) . . ? N5 C12 N2 122.1(5) . . ? N5 C12 N6 124.6(4) . . ? N2 C12 N6 113.3(4) . . ? C12 N6 C11 113.7(4) . . ? N3 C14 N4 121.1(4) . . ? N3 C14 N5 114.0(5) . . ? N4 C14 N5 124.8(4) . . ? C20 C15 C18 120.6(4) . . ? C20 C15 C29 120.2(4) . . ? C18 C15 C29 119.2(4) . . ? C18 C16 C19 118.9(4) . . ? C18 C16 C17 120.4(4) . . ? C19 C16 C17 120.6(4) . . ? O4 C17 O15 125.2(4) . . ? O4 C17 C16 118.8(4) . . ? O15 C17 C16 116.1(4) . . ? C16 C18 C15 119.6(4) . . ? C16 C18 H18 120.2 . . ? C15 C18 H18 120.2 . . ? C16 C19 C21 122.7(4) . . ? C16 C19 H19 118.7 . . ? C21 C19 H19 118.7 . . ? C15 C20 C21 122.6(4) . . ? C15 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? C19 C21 N2 117.3(4) . . ? C19 C21 C20 115.3(4) . . ? N2 C21 C20 127.4(4) . . ? C27 C23 C26 121.2(4) . . ? C27 C23 C28 120.6(4) . . ? C26 C23 C28 117.9(4) . . ? C31 C24 C25 120.0(4) . . ? C31 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 119.5(4) . . ? C26 C25 N3 115.4(4) . . ? C24 C25 N3 124.9(4) . . ? C25 C26 C23 119.9(4) . . ? C25 C26 H26 120.1 . . ? C23 C26 H26 120.1 . . ? C23 C27 C31 118.2(4) . . ? C23 C27 H27 120.9 . . ? C31 C27 H27 120.9 . . ? O8 C28 O7 127.4(4) . . ? O8 C28 C23 117.3(4) . . ? O7 C28 C23 115.3(4) . . ? O12 C29 O11 124.7(4) . . ? O12 C29 C15 118.7(4) . . ? O11 C29 C15 116.5(4) . . ? O9 C30 O10 125.8(4) . . ? O9 C30 C31 117.6(4) . . ? O10 C30 C31 116.6(4) . . ? C24 C31 C27 121.1(4) . . ? C24 C31 C30 120.7(4) . . ? C27 C31 C30 118.2(4) . . ? C11 N1 C7 132.1(4) . . ? C11 N1 H1N 114.0 . . ? C7 N1 H1N 114.0 . . ? C12 N2 C21 130.5(4) . . ? C12 N2 H2N 114.8 . . ? C21 N2 H2N 114.8 . . ? C14 N3 C25 129.5(4) . . ? C14 N3 H3N 115.2 . . ? C25 N3 H3N 115.2 . . ? C17 O4 Cu3 122.9(3) . 9_655 ? C1 O5 Cu3 123.4(3) . . ? C1 O6 Cu4 121.2(3) . . ? C28 O7 Cu2 118.9(3) . 15 ? C28 O8 Cu1 123.8(3) . 15 ? C30 O9 Cu1 120.1(3) . 13 ? C30 O10 Cu2 125.3(3) . 13 ? C29 O11 Cu2 126.2(3) . 3_655 ? C29 O12 Cu1 120.1(3) . 3_655 ? C17 O15 Cu4 123.3(3) . 9_655 ? C2 O16 Cu1 125.6(3) . . ? C2 O17 Cu2 120.4(3) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 65.45 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.159 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.069 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.008 -0.016 -0.005 17536 5326 ' ' 2 0.500 0.000 0.036 5 1 ' ' 3 0.500 0.000 0.464 6 1 ' ' 4 0.500 0.000 0.536 5 1 ' ' 5 0.500 0.000 0.964 6 0 ' ' 6 0.000 0.500 0.036 5 1 ' ' 7 0.000 0.500 0.464 6 0 ' ' 8 0.000 0.500 0.536 5 1 ' ' 9 0.000 0.500 0.964 6 1 ' ' _platon_squeeze_details ; ;