# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Shengqian Ma' _publ_contact_author_email sqma@usf.edu loop_ _publ_author_name 'Xi-Sen Wang' 'Matthew Chrzanowski' 'Wen-Yang Gao' 'Lukasz Wojtas' 'Yu-Sheng Chen' 'Michael Zaworotko' 'Shengqian Ma' data_MMPF-4 _database_code_depnum_ccdc_archive 'CCDC 862931' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MMPF-4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H60 N12 O50 Zn19' _chemical_formula_weight 4144.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0002 0.0005 '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 0.0004 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0015 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2605 0.5370 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Ia-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z, x, y+1/2' 'z, x+1/2, -y' 'z+1/2, -x, y' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z, x' '-y, z, x+1/2' 'y, z+1/2, -x' _cell_length_a 43.030(2) _cell_length_b 43.030(2) _cell_length_c 43.030(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 79671(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9126 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 10.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 16400 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9880 _exptl_absorpt_correction_T_max 0.9880 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.41328 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'BRUKER SMART APEXII CCD' _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 61875 _diffrn_reflns_av_R_equivalents 0.1131 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 0.78 _diffrn_reflns_theta_max 10.83 _reflns_number_total 5235 _reflns_number_gt 3459 _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. isor 0.01 Zn2 isor 0.01 o15 simu 0.02 o15 Zn5 delu 0.02 o15 Zn5 simu 0.02 o15 c32 delu 0.02 o15 c32 simu 0.02 c25 c32 delu 0.02 c25 c32 simu 0.02 c32 o11 delu 0.02 c32 o11 simu 0.02 o2 c31 o8 delu 0.02 o2 c31 o8 simu 0.02 o9 c29 o1 delu 0.02 o9 c29 o1 simu 0.02 c6 c15 simu 0.02 c6 c4 c7 c12 simu o12 c10 delu o12 c10 simu c1 c2 delu c2 c1 simu c4 c5 delu c4 c5 simu c12 c21 delu c12 c21 simu c16 c23 delu c16 c23 simu c22 c24 delu c22 c24 simu c25 c32 delu c25 c32 isor 0.01 Zn4 simu 0.01 Zn4 O9 o8 o5 delu 0.01 Zn4 O9 o8 o5 simu 0.02 n2 c14 delu 0.02 n2 c14 simu Zn2 N2 simu Zn3 O1 simu O1 C29 simu O9 C29 simu N1 C7 simu N2 C14 simu C1 C5 simu C2 C28 simu C3 C4 simu C4 C6 simu C19 C25 delu Zn2 N2 delu Zn3 O1 delu O1 C29 delu O9 C29 delu N1 C7 delu N2 C14 delu C1 C5 delu C2 C28 delu C3 C4 delu C4 C6 delu C19 C25 dfix 1.5 c28 c29 c1 c10 c25 c32 c31 c27 c4 c6 c15 c22 c4 c6 dfix 1.25 c29 o1 c29 o9 c10 o12 c10 o5 c31 o8 c31 o2 c32 o15 c32 o11 dfix 1.39 c27 c26 c26 c25 c25 c19 c19 c22 c22 c24 c24 c27 dfix 1.39 c1 c2 c2 c28 c28 c3 c3 c4 c4 c5 c5 c1 dfix 1.39 c6 c7 c6 c12 c14 c15 c15 c16 dfix 1.377 0.01 c7 n1 c12 n2 n2 c14 c16 n3 dfix 1.44 c7 c20 c12 c21 c13 c14 eqiv $26 1-x, 0.5-y, z dfix 1.352 c21 c13 c23 c23_$26 c20 c20_$26 dfix 2.383 c1 c28 c5 c3 c2 c4 c19 c26 c22 c27 c25 c27 c22 c27 dfix 2.758 c5 c28 c1 c3 c2 c4 c19 c27 c25 c24 c22 c26 dfix 1.26 c10 o12 c10 o5 c29 o1 c29 o9 c32 o15 c32 o11 c31 o2 c31 o8 dfix 2.505 c32 c26 c19 c32 c26 c31 c31 c24 c5 c10 c2 c10 dfix 2.364 o11 c25 o15 c25 o2 c27 o8 c27 c1 o5 c1 o12 c28 o1 c28 o9 flat c28 c29 o9 o1 flat c1 c10 o5 o12 flat c25 c32 o11 o15 flat c27 c31 o2 o8 flat c22 c19 c25 c26 c27 c24 flat c1 c2 c28 c3 c4 c5 flat n2 c12 c21 c13 c14 flat n1 c7 c20 c20_$26 c7_$26 flat n3 c16 c23 c23_$26 c16_$26 dfix 2.34 0.01 c14 c21 c12 c13 ; _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^)+(0.1000P)^2^+700.0000P] 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 5235 _refine_ls_number_parameters 359 _refine_ls_number_restraints 270 _refine_ls_R_factor_all 0.1429 _refine_ls_R_factor_gt 0.1163 _refine_ls_wR_factor_ref 0.2905 _refine_ls_wR_factor_gt 0.2742 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.158 _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 Zn2 Zn 0.5000 0.2500 0.00881(5) 0.1381(13) Uani 1 2 d SU . . Zn3 Zn 0.32969(4) 0.32743(4) 0.18250(4) 0.1156(8) Uani 1 1 d U . . Zn4 Zn 0.36705(7) 0.12169(7) 0.12703(7) 0.2033(15) Uani 1 1 d U . . Zn5 Zn 0.33307(5) 0.16693(5) -0.16693(5) 0.1680(17) Uani 1 3 d SU . . Zn6 Zn 0.38101(9) 0.11899(9) -0.11899(9) 0.255(3) Uani 1 3 d S . . C1 C 0.3827(3) 0.2204(3) 0.1193(3) 0.111(5) Uani 1 1 d DU . . C2 C 0.3734(3) 0.2487(3) 0.1312(3) 0.100(4) Uani 1 1 d DU . . H2 H 0.3570 0.2487 0.1460 0.120 Uiso 1 1 calc R . . C3 C 0.4086(3) 0.2763(3) 0.1004(3) 0.105(5) Uani 1 1 d DU . . H3 H 0.4170 0.2953 0.0928 0.126 Uiso 1 1 calc R . . C4 C 0.4181(3) 0.2492(4) 0.0899(3) 0.095(4) Uani 1 1 d DU . . C5 C 0.4070(3) 0.2203(3) 0.0983(3) 0.118(5) Uani 1 1 d DU . . H5 H 0.4154 0.2016 0.0901 0.141 Uiso 1 1 calc R . . C6 C 0.4437(3) 0.2490(4) 0.0659(3) 0.132(4) Uani 1 1 d DU . . C7 C 0.4747(3) 0.2459(4) 0.0749(3) 0.125(5) Uani 1 1 d DU . . C10 C 0.3655(3) 0.1911(3) 0.1274(4) 0.148(7) Uani 1 1 d DU . . C12 C 0.4340(3) 0.2461(3) 0.0349(3) 0.098(4) Uani 1 1 d DU . . C13 C 0.4018(3) 0.2474(4) -0.0082(3) 0.127(6) Uani 1 1 d D . . H13 H 0.3844 0.2484 -0.0218 0.153 Uiso 1 1 calc R . . C14 C 0.4347(3) 0.2471(3) -0.0170(3) 0.107(4) Uani 1 1 d DU . . C15 C 0.4444(4) 0.2470(3) -0.0474(3) 0.109(5) Uani 1 1 d D . . C16 C 0.4745(3) 0.2476(4) -0.0565(3) 0.143(6) Uani 1 1 d DU . . C19 C 0.4112(3) 0.2180(3) -0.0829(3) 0.110(5) Uani 1 1 d DU . . H19 H 0.4203 0.1998 -0.0744 0.133 Uiso 1 1 calc R . . C20 C 0.4841(2) 0.2469(3) 0.1078(3) 0.127(6) Uani 1 1 d D . . H20 H 0.4712 0.2440 0.1254 0.152 Uiso 1 1 calc R . . C21 C 0.4010(3) 0.2459(3) 0.0249(3) 0.127(5) Uani 1 1 d DU . . H21 H 0.3832 0.2449 0.0378 0.152 Uiso 1 1 calc R . . C22 C 0.4193(2) 0.2468(4) -0.0713(3) 0.090(4) Uani 1 1 d DU . . C23 C 0.4844(2) 0.2486(4) -0.0922(4) 0.159(7) Uani 1 1 d DU . . H23 H 0.4711 0.2475 -0.1098 0.190 Uiso 1 1 calc R . . C24 C 0.4070(3) 0.2735(3) -0.0838(3) 0.106(4) Uani 1 1 d DU . . H24 H 0.4132 0.2933 -0.0764 0.127 Uiso 1 1 calc R . . C25 C 0.3902(4) 0.2157(3) -0.1065(4) 0.195(7) Uani 1 1 d DU . . C26 C 0.3761(3) 0.2420(3) -0.1188(3) 0.121(6) Uani 1 1 d D . . H26 H 0.3605 0.2403 -0.1343 0.146 Uiso 1 1 calc R . . C27 C 0.3854(4) 0.2709(3) -0.1076(3) 0.133(6) Uani 1 1 d D . . C28 C 0.3855(3) 0.2760(3) 0.1234(3) 0.096(4) Uani 1 1 d DU . . C29 C 0.3755(3) 0.3061(4) 0.1376(3) 0.132(5) Uani 1 1 d DU . . C31 C 0.3730(4) 0.3000(4) -0.1226(4) 0.209(8) Uani 1 1 d DU . . C32 C 0.3820(4) 0.1848(4) -0.1210(4) 0.253(7) Uani 1 1 d DU . . N1 N 0.5000 0.2500 0.0561(3) 0.089(4) Uani 1 2 d SDU . . N2 N 0.4533(2) 0.2469(2) 0.0096(2) 0.090(3) Uani 1 1 d DU . . N3 N 0.5000 0.2500 -0.0379(3) 0.093(5) Uani 1 2 d SD . . O1 O 0.3534(3) 0.3047(3) 0.1574(3) 0.170(4) Uani 1 1 d DU . . O2 O 0.3529(4) 0.2964(4) -0.1425(4) 0.233(6) Uani 1 1 d DU . . O5 O 0.3771(3) 0.1662(3) 0.1182(3) 0.176(5) Uani 1 1 d DU . . O8 O 0.3829(4) 0.3251(3) -0.1138(4) 0.212(6) Uani 1 1 d DU . . O9 O 0.3889(3) 0.3297(3) 0.1285(3) 0.157(4) Uani 1 1 d DU . . O11 O 0.3904(5) 0.1606(3) -0.1078(4) 0.252(7) Uani 1 1 d DU . . O12 O 0.3418(3) 0.1932(3) 0.1444(3) 0.198(6) Uani 1 1 d DU . . O15 O 0.3676(5) 0.1875(5) -0.1465(4) 0.283(7) Uani 1 1 d DU . . O19 O 0.4133(5) 0.0867(5) -0.0867(5) 0.286(16) Uani 1 3 d S . . 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 Zn2 0.0578(15) 0.283(4) 0.0737(17) 0.000 0.000 0.0038(18) Zn3 0.1097(15) 0.1195(15) 0.1177(15) 0.0085(11) 0.0182(11) -0.0279(11) Zn4 0.192(3) 0.208(3) 0.210(3) -0.076(2) 0.042(2) 0.066(2) Zn5 0.1680(17) 0.1680(17) 0.1680(17) 0.0303(15) -0.0303(15) 0.0303(15) Zn6 0.255(3) 0.255(3) 0.255(3) 0.023(3) -0.023(3) 0.023(3) C1 0.092(10) 0.143(12) 0.098(11) -0.015(10) 0.014(7) 0.005(10) C2 0.069(9) 0.135(11) 0.095(10) 0.000(9) -0.003(8) -0.012(8) C3 0.086(10) 0.152(13) 0.079(10) -0.010(9) 0.009(8) -0.010(9) C4 0.082(9) 0.140(10) 0.065(8) 0.009(8) -0.009(6) 0.010(8) C5 0.114(12) 0.144(11) 0.095(11) -0.010(10) 0.018(8) 0.014(10) C6 0.113(10) 0.178(11) 0.105(9) 0.010(9) 0.005(7) 0.001(9) C7 0.100(11) 0.194(13) 0.081(10) -0.001(9) 0.001(7) -0.009(11) C10 0.098(14) 0.156(16) 0.19(2) -0.023(15) 0.014(11) 0.045(14) C12 0.086(8) 0.135(11) 0.071(9) 0.012(8) 0.010(8) -0.004(8) C13 0.090(13) 0.171(16) 0.121(15) -0.001(11) 0.001(10) -0.027(11) C14 0.103(12) 0.144(12) 0.075(10) -0.011(9) -0.013(7) 0.000(9) C15 0.118(14) 0.132(13) 0.078(12) -0.013(9) -0.031(11) 0.005(10) C16 0.097(13) 0.233(19) 0.101(10) 0.037(12) -0.005(11) -0.019(14) C19 0.100(11) 0.115(12) 0.117(12) 0.033(10) -0.015(8) 0.026(10) C20 0.100(11) 0.202(17) 0.078(10) -0.013(11) -0.003(7) 0.019(13) C21 0.112(10) 0.179(15) 0.089(11) 0.002(10) -0.006(9) -0.003(11) C22 0.058(9) 0.121(13) 0.090(11) -0.004(9) 0.004(8) 0.008(8) C23 0.135(15) 0.218(18) 0.122(10) -0.008(13) 0.015(9) -0.023(17) C24 0.094(11) 0.118(12) 0.105(12) -0.019(9) -0.030(9) -0.008(9) C25 0.208(16) 0.219(15) 0.157(15) 0.012(13) -0.067(11) 0.054(15) C26 0.081(11) 0.195(18) 0.088(12) -0.007(12) 0.008(8) -0.035(12) C27 0.123(15) 0.20(2) 0.075(12) -0.005(12) -0.007(10) 0.007(14) C28 0.063(9) 0.132(12) 0.092(10) -0.017(9) 0.010(8) -0.022(8) C29 0.106(12) 0.136(12) 0.155(13) -0.006(11) 0.027(8) 0.006(9) C31 0.181(17) 0.258(18) 0.188(17) 0.043(16) -0.027(12) 0.005(15) C32 0.290(14) 0.234(14) 0.237(14) 0.012(13) -0.034(12) 0.013(14) N1 0.086(11) 0.122(12) 0.059(9) 0.000 0.000 0.021(9) N2 0.077(6) 0.132(9) 0.062(7) -0.012(6) -0.016(5) -0.009(6) N3 0.053(10) 0.142(14) 0.084(11) 0.000 0.000 -0.009(9) O1 0.151(11) 0.159(10) 0.199(12) -0.006(8) 0.048(8) -0.005(8) O2 0.201(15) 0.311(16) 0.188(14) 0.042(12) -0.054(10) 0.033(12) O5 0.133(10) 0.221(10) 0.174(12) -0.030(11) 0.042(9) 0.025(10) O8 0.188(13) 0.235(17) 0.214(14) 0.042(13) -0.030(10) -0.007(12) O9 0.130(9) 0.155(11) 0.185(11) -0.015(9) 0.046(8) 0.006(8) O11 0.324(17) 0.194(14) 0.237(15) 0.039(12) 0.011(13) 0.014(13) O12 0.154(12) 0.213(13) 0.228(15) -0.022(12) 0.042(10) 0.030(11) O15 0.286(11) 0.292(11) 0.273(11) -0.025(9) -0.047(8) -0.026(9) O19 0.286(16) 0.286(16) 0.286(16) -0.027(19) 0.027(19) -0.027(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn2 N3 2.011(15) . ? Zn2 N2 2.013(9) . ? Zn2 N2 2.013(9) 14_554 ? Zn2 N1 2.034(13) . ? Zn3 O1 1.777(11) . ? Zn3 O2 1.858(13) 31_656 ? Zn3 O12 1.879(13) 45 ? Zn4 O8 1.885(14) 23_445 ? Zn4 O9 1.925(11) 41 ? Zn4 O5 2.000(14) . ? Zn5 O15 1.943(16) 12_554 ? Zn5 O15 1.943(16) . ? Zn5 O15 1.943(16) 6 ? Zn6 O11 1.898(15) 12_554 ? Zn6 O11 1.898(15) . ? Zn6 O11 1.898(15) 6 ? Zn6 O19 2.40(4) . ? C1 C2 1.380(12) . ? C1 C5 1.381(13) . ? C1 C10 1.506(13) . ? C2 C28 1.327(12) . ? C2 H2 0.9500 . ? C3 C4 1.314(13) . ? C3 C28 1.403(13) . ? C3 H3 0.9500 . ? C4 C5 1.383(13) . ? C4 C6 1.509(12) . ? C5 H5 0.9500 . ? C6 C7 1.396(14) . ? C6 C12 1.405(14) . ? C7 N1 1.368(9) . ? C7 C20 1.471(14) . ? C10 O5 1.248(11) . ? C10 O12 1.257(11) . ? C12 N2 1.372(9) . ? C12 C21 1.481(13) . ? C13 C21 1.425(13) . ? C13 C14 1.467(13) . ? C13 H13 0.9500 . ? C14 C15 1.374(14) . ? C14 N2 1.395(9) . ? C15 C16 1.352(14) . ? C15 C22 1.494(13) . ? C16 N3 1.361(9) . ? C16 C23 1.60(2) . ? C19 C25 1.363(14) . ? C19 C22 1.381(13) . ? C19 H19 0.9500 . ? C20 C20 1.392(17) 14_554 ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C24 1.374(13) . ? C23 C23 1.346(18) 14_554 ? C23 H23 0.9500 . ? C24 C27 1.385(13) . ? C24 H24 0.9500 . ? C25 C26 1.389(13) . ? C25 C32 1.511(14) . ? C26 C27 1.392(13) . ? C26 H26 0.9500 . ? C27 C31 1.507(14) . ? C28 C29 1.498(14) . ? C29 O9 1.232(11) . ? C29 O1 1.279(12) . ? C31 O8 1.223(12) . ? C31 O2 1.231(12) . ? C32 O11 1.239(13) . ? C32 O15 1.266(13) . ? N1 C7 1.368(9) 14_554 ? N3 C16 1.361(9) 14_554 ? O2 Zn3 1.858(13) 34_565 ? O8 Zn4 1.885(14) 20_544 ? O9 Zn4 1.925(11) 45 ? O12 Zn3 1.879(13) 41 ? 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 N3 Zn2 N2 91.0(3) . . ? N3 Zn2 N2 91.0(3) . 14_554 ? N2 Zn2 N2 178.1(6) . 14_554 ? N3 Zn2 N1 180.000(1) . . ? N2 Zn2 N1 89.0(3) . . ? N2 Zn2 N1 89.0(3) 14_554 . ? O1 Zn3 O2 104.6(7) . 31_656 ? O1 Zn3 O12 108.5(6) . 45 ? O2 Zn3 O12 103.2(7) 31_656 45 ? O8 Zn4 O9 105.8(6) 23_445 41 ? O8 Zn4 O5 109.7(6) 23_445 . ? O9 Zn4 O5 112.9(5) 41 . ? O15 Zn5 O15 102.1(7) 12_554 . ? O15 Zn5 O15 102.1(7) 12_554 6 ? O15 Zn5 O15 102.1(7) . 6 ? O11 Zn6 O11 112.7(5) 12_554 . ? O11 Zn6 O11 112.7(5) 12_554 6 ? O11 Zn6 O11 112.7(5) . 6 ? O11 Zn6 O19 106.0(6) 12_554 . ? O11 Zn6 O19 106.0(6) . . ? O11 Zn6 O19 106.0(6) 6 . ? C2 C1 C5 117.8(10) . . ? C2 C1 C10 120.7(10) . . ? C5 C1 C10 121.3(10) . . ? C28 C2 C1 124.9(10) . . ? C28 C2 H2 117.5 . . ? C1 C2 H2 117.5 . . ? C4 C3 C28 116.9(10) . . ? C4 C3 H3 121.5 . . ? C28 C3 H3 121.5 . . ? C3 C4 C5 127.1(11) . . ? C3 C4 C6 117.8(13) . . ? C5 C4 C6 115.1(13) . . ? C1 C5 C4 115.3(10) . . ? C1 C5 H5 122.4 . . ? C4 C5 H5 122.4 . . ? C7 C6 C12 122.6(12) . . ? C7 C6 C4 120.7(12) . . ? C12 C6 C4 115.6(12) . . ? N1 C7 C6 125.8(11) . . ? N1 C7 C20 110.3(12) . . ? C6 C7 C20 121.7(10) . . ? O5 C10 O12 125.0(14) . . ? O5 C10 C1 116.6(12) . . ? O12 C10 C1 118.2(12) . . ? N2 C12 C6 124.9(11) . . ? N2 C12 C21 110.5(9) . . ? C6 C12 C21 124.2(11) . . ? C21 C13 C14 106.1(8) . . ? C21 C13 H13 126.9 . . ? C14 C13 H13 126.9 . . ? C15 C14 N2 127.2(12) . . ? C15 C14 C13 122.7(11) . . ? N2 C14 C13 110.1(9) . . ? C16 C15 C14 124.6(12) . . ? C16 C15 C22 119.6(12) . . ? C14 C15 C22 115.8(12) . . ? C15 C16 N3 127.1(14) . . ? C15 C16 C23 122.4(10) . . ? N3 C16 C23 110.3(13) . . ? C25 C19 C22 120.0(10) . . ? C25 C19 H19 120.0 . . ? C22 C19 H19 120.0 . . ? C20 C20 C7 106.0(6) 14_554 . ? C20 C20 H20 127.0 14_554 . ? C7 C20 H20 127.0 . . ? C13 C21 C12 105.6(8) . . ? C13 C21 H21 127.2 . . ? C12 C21 H21 127.2 . . ? C24 C22 C19 120.8(10) . . ? C24 C22 C15 123.1(13) . . ? C19 C22 C15 115.7(12) . . ? C23 C23 C16 105.6(6) 14_554 . ? C23 C23 H23 127.2 14_554 . ? C16 C23 H23 127.2 . . ? C22 C24 C27 118.7(11) . . ? C22 C24 H24 120.7 . . ? C27 C24 H24 120.7 . . ? C19 C25 C26 121.0(10) . . ? C19 C25 C32 121.7(11) . . ? C26 C25 C32 117.3(12) . . ? C25 C26 C27 118.0(10) . . ? C25 C26 H26 121.0 . . ? C27 C26 H26 121.0 . . ? C24 C27 C26 121.3(9) . . ? C24 C27 C31 119.0(11) . . ? C26 C27 C31 119.6(10) . . ? C2 C28 C3 117.8(10) . . ? C2 C28 C29 123.4(11) . . ? C3 C28 C29 118.8(11) . . ? O9 C29 O1 126.9(15) . . ? O9 C29 C28 116.7(12) . . ? O1 C29 C28 116.4(12) . . ? O8 C31 O2 125.1(18) . . ? O8 C31 C27 118.6(14) . . ? O2 C31 C27 116.2(14) . . ? O11 C32 O15 128.1(19) . . ? O11 C32 C25 118.9(15) . . ? O15 C32 C25 112.9(14) . . ? C7 N1 C7 107.4(15) . 14_554 ? C7 N1 Zn2 126.3(7) . . ? C7 N1 Zn2 126.3(7) 14_554 . ? C12 N2 C14 107.5(9) . . ? C12 N2 Zn2 128.4(7) . . ? C14 N2 Zn2 124.0(8) . . ? C16 N3 C16 108.2(18) . 14_554 ? C16 N3 Zn2 125.9(9) . . ? C16 N3 Zn2 125.9(9) 14_554 . ? C29 O1 Zn3 143.7(11) . . ? C31 O2 Zn3 143.3(15) . 34_565 ? C10 O5 Zn4 132.3(10) . . ? C31 O8 Zn4 135.2(13) . 20_544 ? C29 O9 Zn4 130.8(11) . 45 ? C32 O11 Zn6 127.9(16) . . ? C10 O12 Zn3 142.0(12) . 41 ? C32 O15 Zn5 136.5(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C28 1.4(16) . . . . ? C10 C1 C2 C28 -174.5(13) . . . . ? C28 C3 C4 C5 2(2) . . . . ? C28 C3 C4 C6 -177.8(11) . . . . ? C2 C1 C5 C4 -3.9(19) . . . . ? C10 C1 C5 C4 172.0(13) . . . . ? C3 C4 C5 C1 2(2) . . . . ? C6 C4 C5 C1 -177.6(12) . . . . ? C3 C4 C6 C7 93.5(19) . . . . ? C5 C4 C6 C7 -87(2) . . . . ? C3 C4 C6 C12 -98.0(18) . . . . ? C5 C4 C6 C12 81.7(18) . . . . ? C12 C6 C7 N1 23(3) . . . . ? C4 C6 C7 N1 -169.7(13) . . . . ? C12 C6 C7 C20 -175.8(13) . . . . ? C4 C6 C7 C20 -8(2) . . . . ? C2 C1 C10 O5 -173.3(13) . . . . ? C5 C1 C10 O5 11(2) . . . . ? C2 C1 C10 O12 2(2) . . . . ? C5 C1 C10 O12 -173.4(15) . . . . ? C7 C6 C12 N2 -15(3) . . . . ? C4 C6 C12 N2 176.8(12) . . . . ? C7 C6 C12 C21 173.1(15) . . . . ? C4 C6 C12 C21 5(2) . . . . ? C21 C13 C14 C15 177.1(14) . . . . ? C21 C13 C14 N2 -2.5(17) . . . . ? N2 C14 C15 C16 -2(3) . . . . ? C13 C14 C15 C16 178.1(17) . . . . ? N2 C14 C15 C22 179.1(13) . . . . ? C13 C14 C15 C22 0(2) . . . . ? C14 C15 C16 N3 -4(3) . . . . ? C22 C15 C16 N3 175.0(14) . . . . ? C14 C15 C16 C23 -177.7(14) . . . . ? C22 C15 C16 C23 1(2) . . . . ? N1 C7 C20 C20 2.4(17) . . . 14_554 ? C6 C7 C20 C20 -161.7(19) . . . 14_554 ? C14 C13 C21 C12 2.4(15) . . . . ? N2 C12 C21 C13 -1.6(13) . . . . ? C6 C12 C21 C13 171.3(15) . . . . ? C25 C19 C22 C24 -1.7(15) . . . . ? C25 C19 C22 C15 -174.9(13) . . . . ? C16 C15 C22 C24 -87.6(19) . . . . ? C14 C15 C22 C24 91.1(17) . . . . ? C16 C15 C22 C19 85.5(18) . . . . ? C14 C15 C22 C19 -95.8(15) . . . . ? C15 C16 C23 C23 175(2) . . . 14_554 ? N3 C16 C23 C23 0.4(18) . . . 14_554 ? C19 C22 C24 C27 3(2) . . . . ? C15 C22 C24 C27 175.2(13) . . . . ? C22 C19 C25 C26 -1.6(18) . . . . ? C22 C19 C25 C32 176.7(16) . . . . ? C19 C25 C26 C27 4(2) . . . . ? C32 C25 C26 C27 -174.5(15) . . . . ? C22 C24 C27 C26 0(2) . . . . ? C22 C24 C27 C31 -176.9(13) . . . . ? C25 C26 C27 C24 -3(2) . . . . ? C25 C26 C27 C31 173.7(14) . . . . ? C1 C2 C28 C3 3.2(15) . . . . ? C1 C2 C28 C29 -177.8(12) . . . . ? C4 C3 C28 C2 -5.0(18) . . . . ? C4 C3 C28 C29 176.0(12) . . . . ? C2 C28 C29 O9 179.5(13) . . . . ? C3 C28 C29 O9 -1.5(19) . . . . ? C2 C28 C29 O1 -2.2(19) . . . . ? C3 C28 C29 O1 176.8(13) . . . . ? C24 C27 C31 O8 2(2) . . . . ? C26 C27 C31 O8 -175.3(18) . . . . ? C24 C27 C31 O2 -176.9(17) . . . . ? C26 C27 C31 O2 6(2) . . . . ? C19 C25 C32 O11 13(3) . . . . ? C26 C25 C32 O11 -169.0(18) . . . . ? C19 C25 C32 O15 -165.7(17) . . . . ? C26 C25 C32 O15 13(2) . . . . ? C6 C7 N1 C7 162(2) . . . 14_554 ? C20 C7 N1 C7 -0.9(6) . . . 14_554 ? C6 C7 N1 Zn2 -18(2) . . . . ? C20 C7 N1 Zn2 179.1(6) . . . . ? N3 Zn2 N1 C7 0(100) . . . . ? N2 Zn2 N1 C7 5.3(9) . . . . ? N2 Zn2 N1 C7 -174.7(9) 14_554 . . . ? N3 Zn2 N1 C7 0(94) . . . 14_554 ? N2 Zn2 N1 C7 -174.7(9) . . . 14_554 ? N2 Zn2 N1 C7 5.3(9) 14_554 . . 14_554 ? C6 C12 N2 C14 -172.9(14) . . . . ? C21 C12 N2 C14 0.1(13) . . . . ? C6 C12 N2 Zn2 3.2(19) . . . . ? C21 C12 N2 Zn2 176.2(9) . . . . ? C15 C14 N2 C12 -178.1(15) . . . . ? C13 C14 N2 C12 1.5(15) . . . . ? C15 C14 N2 Zn2 6(2) . . . . ? C13 C14 N2 Zn2 -174.8(9) . . . . ? N3 Zn2 N2 C12 -178.7(10) . . . . ? N2 Zn2 N2 C12 1.3(10) 14_554 . . . ? N1 Zn2 N2 C12 1.3(10) . . . . ? N3 Zn2 N2 C14 -3.2(10) . . . . ? N2 Zn2 N2 C14 176.8(10) 14_554 . . . ? N1 Zn2 N2 C14 176.8(10) . . . . ? C15 C16 N3 C16 -175(2) . . . 14_554 ? C23 C16 N3 C16 -0.1(6) . . . 14_554 ? C15 C16 N3 Zn2 5(2) . . . . ? C23 C16 N3 Zn2 179.9(6) . . . . ? N2 Zn2 N3 C16 -1.6(10) . . . . ? N2 Zn2 N3 C16 178.4(10) 14_554 . . . ? N1 Zn2 N3 C16 0(100) . . . . ? N2 Zn2 N3 C16 178.4(10) . . . 14_554 ? N2 Zn2 N3 C16 -1.6(10) 14_554 . . 14_554 ? N1 Zn2 N3 C16 0(81) . . . 14_554 ? O9 C29 O1 Zn3 -1(3) . . . . ? C28 C29 O1 Zn3 -179.5(14) . . . . ? O2 Zn3 O1 C29 -48(2) 31_656 . . . ? O12 Zn3 O1 C29 62(2) 45 . . . ? O8 C31 O2 Zn3 2(4) . . . 34_565 ? C27 C31 O2 Zn3 -179.6(17) . . . 34_565 ? O12 C10 O5 Zn4 -4(3) . . . . ? C1 C10 O5 Zn4 170.9(11) . . . . ? O8 Zn4 O5 C10 56.4(17) 23_445 . . . ? O9 Zn4 O5 C10 -61.4(17) 41 . . . ? O2 C31 O8 Zn4 5(3) . . . 20_544 ? C27 C31 O8 Zn4 -173.0(14) . . . 20_544 ? O1 C29 O9 Zn4 -13(3) . . . 45 ? C28 C29 O9 Zn4 164.9(10) . . . 45 ? O15 C32 O11 Zn6 -7(3) . . . . ? C25 C32 O11 Zn6 175.4(14) . . . . ? O11 Zn6 O11 C32 -74.2(18) 12_554 . . . ? O11 Zn6 O11 C32 55(2) 6 . . . ? O19 Zn6 O11 C32 170.3(18) . . . . ? O5 C10 O12 Zn3 21(3) . . . 41 ? C1 C10 O12 Zn3 -154.7(15) . . . 41 ? O11 C32 O15 Zn5 42(4) . . . . ? C25 C32 O15 Zn5 -139.9(19) . . . . ? O15 Zn5 O15 C32 20(2) 12_554 . . . ? O15 Zn5 O15 C32 -85.8(18) 6 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 10.83 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.962 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.081 _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The lack of high angle diffraction data (despite using synchrotron source and trying several crystals) can be attributed to the presence of the ligand / solvent disorder. ; _vrf_PLAT023_I ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 10.83 Deg. RESPONSE:The lack of high angle diffraction data (despite using synchrotron source and trying several crystals) can be attributed to the presence of the ligand / solvent disorder. ; _vrf_PLAT112_I ; PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem... Z RESPONSE: The structure can be solved in Pm-3m space group using smaller unit cell parameters but refinement results in much higher values of anisotropic thermal parameters. The observed pseudosymmetry is most likely due to the merohedral twinning with [0 1 0 1 0 0 0 0 -1] twin low. ; 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 -0.002 -0.013 -0.003 56189 25970 ' ' _platon_squeeze_details ; ; # Attachment '- MMPF-5_revision2.cif' data_MMPF-5 _database_code_depnum_ccdc_archive 'CCDC 862932' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MMPF-5 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H60 Cd11 N12 O51' _chemical_formula_weight 4154.56 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' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pm-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x, -z, y' 'x, -y, -z' 'x, z, -y' 'z, y, -x' '-x, y, -z' '-z, y, x' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' 'y, x, -z' '-y, -x, -z' '-x, z, y' '-x, -z, -y' 'z, -y, x' '-z, -y, -x' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x, z, -y' '-x, y, z' '-x, -z, y' '-z, -y, x' 'x, -y, z' 'z, -y, -x' '-z, -x, -y' '-y, -z, -x' 'y, z, -x' '-z, x, y' 'y, -z, x' 'z, x, -y' 'z, -x, y' '-y, z, x' '-y, -x, z' 'y, x, z' 'x, -z, -y' 'x, z, y' '-z, y, -x' 'z, y, x' _cell_length_a 22.521(15) _cell_length_b 22.521(15) _cell_length_c 22.521(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11423(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 934 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.2 _exptl_crystal_description polyhedron _exptl_crystal_colour black _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 0.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 4.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6746 _exptl_absorpt_correction_T_max 0.6746 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; The crystal has been sealed in the capillary. ; _diffrn_ambient_temperature 293(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 5323 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 33.35 _reflns_number_total 483 _reflns_number_gt 327 _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. All non-H atoms have been found from difference Fourier map. Model was refined using geometry restraints and the validity was confirmed through the inspection of 2Fo-Fc electron density map plotted at 1 sigma level. Restraints list: sadi o3 c10 c10 o2 dfix 1.24 C5 O3 dfix 1.5 c5 c10 sadi c14 c10 c10 c19 c19 c12 eqiv $1 1-x, z, y sadi C10 C10_$1 c19 c19_$1 c14 c19 sadi c14 c12 c10 c19_$1 C19 C10_$1 dfix 1.49 c11 c12 dfix 1.39 c8 c11 dfix 1.436 C8 c9 eqiv $2 1-x, -y, z dfix 1.34 c9 c9_$2 dfix 1.39 c8 n1 dfix 2.4 o2 cd1 dfix 2.4 Cd2 O4 ; _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^)+(0.1761P)^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 483 _refine_ls_number_parameters 38 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2483 _refine_ls_wR_factor_gt 0.2268 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.035 _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 Cd1 Cd 0.28534(10) 0.28534(10) 0.28534(10) 0.187(3) Uani 1 6 d SD . . Cd2 Cd 0.4620(3) 0.0000 0.0000 0.137(3) Uani 0.50 8 d SPD . . N1 N 0.5000 0.0000 0.0957(9) 0.114(8) Uiso 1 4 d SD . . O2 O 0.3446(6) 0.2251(5) 0.2251(5) 0.204(8) Uiso 1 2 d SD . . C8 C 0.5000 0.0509(7) 0.1309(8) 0.139(8) Uiso 1 2 d SD . . C9 C 0.5000 0.0301(4) 0.1927(9) 0.157(10) Uiso 1 2 d SD . . H9A H 0.5000 0.0542 0.2262 0.189 Uiso 1 2 calc SR . . C10 C 0.4470(4) 0.2216(5) 0.2216(5) 0.113(7) Uiso 1 2 d SD . . C11 C 0.5000 0.1091(7) 0.1091(7) 0.136(11) Uiso 1 4 d SD . . C12 C 0.5000 0.1560(6) 0.1560(6) 0.105(10) Uiso 1 4 d SD . . C14 C 0.5000 0.2427(5) 0.2427(5) 0.104(9) Uiso 1 4 d SD . . H14A H 0.5000 0.2719 0.2719 0.125 Uiso 1 4 calc SR . . C19 C 0.4469(4) 0.1777(5) 0.1777(5) 0.123(7) Uiso 1 2 d SD . . H19A H 0.4111 0.1632 0.1632 0.148 Uiso 1 2 calc SR . . O3 O 0.3924(7) 0.2829(5) 0.2829(5) 0.184(7) Uiso 1 2 d SD . . C5 C 0.3894(9) 0.2445(6) 0.2445(6) 0.158(10) Uiso 1 2 d SD . . O4 O 0.3560(9) 0.0000 0.0000 0.24(3) Uiso 0.50 8 d SPD . . 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 Cd1 0.187(3) 0.187(3) 0.187(3) 0.0387(16) 0.0387(16) 0.0387(16) Cd2 0.187(8) 0.112(4) 0.112(4) 0.000 0.000 0.000 _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 Cd1 O2 2.337(13) . ? Cd1 O2 2.337(13) 12 ? Cd1 O2 2.337(13) 11 ? Cd1 O3 2.413(15) . ? Cd1 O3 2.413(15) 12 ? Cd1 O3 2.413(15) 11 ? Cd1 C5 2.681(19) . ? Cd1 C5 2.681(19) 11 ? Cd1 C5 2.681(19) 12 ? Cd2 Cd2 1.710(13) 25_655 ? Cd2 N1 2.32(2) 29_655 ? Cd2 N1 2.32(2) 25_655 ? Cd2 N1 2.32(2) 5 ? Cd2 N1 2.32(2) . ? Cd2 O4 2.39(2) . ? N1 C8 1.393(14) . ? N1 C8 1.393(14) 3_655 ? N1 Cd2 2.32(2) 25_655 ? O2 C5 1.18(2) . ? C8 C11 1.401(15) . ? C8 C9 1.467(15) . ? C9 C9 1.357(18) 3_655 ? C9 H9A 0.9300 . ? C10 C14 1.368(13) . ? C10 C19 1.398(13) . ? C10 C5 1.488(15) . ? C11 C8 1.401(15) 21_655 ? C11 C12 1.493(17) . ? C12 C19 1.382(11) 21_655 ? C12 C19 1.382(11) . ? C14 C10 1.368(13) 21_655 ? C14 H14A 0.9300 . ? C19 H19A 0.9300 . ? O3 C5 1.226(15) . ? 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 O2 Cd1 O2 109.0(4) . 12 ? O2 Cd1 O2 109.0(4) . 11 ? O2 Cd1 O2 109.0(4) 12 11 ? O2 Cd1 O3 53.3(6) . . ? O2 Cd1 O3 125.44(19) 12 . ? O2 Cd1 O3 125.44(19) 11 . ? O2 Cd1 O3 125.44(19) . 12 ? O2 Cd1 O3 53.3(6) 12 12 ? O2 Cd1 O3 125.44(18) 11 12 ? O3 Cd1 O3 92.6(5) . 12 ? O2 Cd1 O3 125.44(19) . 11 ? O2 Cd1 O3 125.44(18) 12 11 ? O2 Cd1 O3 53.3(5) 11 11 ? O3 Cd1 O3 92.6(5) . 11 ? O3 Cd1 O3 92.6(5) 12 11 ? O2 Cd1 C5 26.1(5) . . ? O2 Cd1 C5 120.28(17) 12 . ? O2 Cd1 C5 120.28(17) 11 . ? O3 Cd1 C5 27.2(4) . . ? O3 Cd1 C5 110.8(4) 12 . ? O3 Cd1 C5 110.8(4) 11 . ? O2 Cd1 C5 120.28(17) . 11 ? O2 Cd1 C5 120.28(17) 12 11 ? O2 Cd1 C5 26.1(5) 11 11 ? O3 Cd1 C5 110.8(4) . 11 ? O3 Cd1 C5 110.8(4) 12 11 ? O3 Cd1 C5 27.2(4) 11 11 ? C5 Cd1 C5 118.84(17) . 11 ? O2 Cd1 C5 120.28(17) . 12 ? O2 Cd1 C5 26.1(5) 12 12 ? O2 Cd1 C5 120.28(17) 11 12 ? O3 Cd1 C5 110.8(4) . 12 ? O3 Cd1 C5 27.2(4) 12 12 ? O3 Cd1 C5 110.8(4) 11 12 ? C5 Cd1 C5 118.84(17) . 12 ? C5 Cd1 C5 118.84(17) 11 12 ? Cd2 Cd2 N1 68.4(2) 25_655 29_655 ? Cd2 Cd2 N1 68.4(2) 25_655 25_655 ? N1 Cd2 N1 82.19(16) 29_655 25_655 ? Cd2 Cd2 N1 68.4(2) 25_655 5 ? N1 Cd2 N1 136.7(5) 29_655 5 ? N1 Cd2 N1 82.19(16) 25_655 5 ? Cd2 Cd2 N1 68.4(2) 25_655 . ? N1 Cd2 N1 82.19(16) 29_655 . ? N1 Cd2 N1 136.7(5) 25_655 . ? N1 Cd2 N1 82.19(16) 5 . ? Cd2 Cd2 O4 180.0 25_655 . ? N1 Cd2 O4 111.6(2) 29_655 . ? N1 Cd2 O4 111.6(2) 25_655 . ? N1 Cd2 O4 111.6(2) 5 . ? N1 Cd2 O4 111.6(2) . . ? C8 N1 C8 111(2) . 3_655 ? C8 N1 Cd2 121.9(9) . . ? C8 N1 Cd2 121.9(9) 3_655 . ? C8 N1 Cd2 121.9(9) . 25_655 ? C8 N1 Cd2 121.9(9) 3_655 25_655 ? Cd2 N1 Cd2 43.3(5) . 25_655 ? C5 O2 Cd1 93.4(13) . . ? N1 C8 C11 124.8(19) . . ? N1 C8 C9 106.1(16) . . ? C11 C8 C9 129.1(14) . . ? C9 C9 C8 108.6(8) 3_655 . ? C9 C9 H9A 125.7 3_655 . ? C8 C9 H9A 125.7 . . ? C14 C10 C19 119.5(8) . . ? C14 C10 C5 121.4(12) . . ? C19 C10 C5 119.1(10) . . ? C8 C11 C8 131(2) . 21_655 ? C8 C11 C12 114.5(12) . . ? C8 C11 C12 114.5(12) 21_655 . ? C19 C12 C19 119.8(13) 21_655 . ? C19 C12 C11 120.1(6) 21_655 . ? C19 C12 C11 120.1(6) . . ? C10 C14 C10 121.3(12) . 21_655 ? C10 C14 H14A 119.4 . . ? C10 C14 H14A 119.4 21_655 . ? C12 C19 C10 120.0(9) . . ? C12 C19 H19A 120.0 . . ? C10 C19 H19A 120.0 . . ? C5 O3 Cd1 88.6(13) . . ? O2 C5 O3 125(2) . . ? O2 C5 C10 119.3(16) . . ? O3 C5 C10 116.1(18) . . ? O2 C5 Cd1 60.5(11) . . ? O3 C5 Cd1 64.1(11) . . ? C10 C5 Cd1 179.8(16) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 33.35 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.388 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.059 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 -0.010 -0.007 -0.006 8587 1297 ' ' _platon_squeeze_details ; ; _vrf_THETM01_ma_poccd ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The lack of high angle diffraction data can be attributed to the presence of the disordered solvent. ; _vrf_PLAT023_ma_poccd ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 33.35 Deg. RESPONSE: The lack of high angle diffraction data can be attributed to the presence of the disordered solvent. ; _vrf_PLAT201_ma_poccd ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 11 RESPONSE: Due to the lack of high angle data C,N,O atoms were refined isotropically. ;