# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_added_by_encifer _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ; A highly porous metal organic framework, constructed from a cuboctahedral super-molecular building block, with exceptionally high methane uptake ; _publ_section_abstract ; A highly porous metal-organic framework Cu2(BBCDC) (DUT-49) shows a specific surface area of 5476 m2/g, a pore volume of 2.68 cm3/g, a H2 excess uptake of 80 mg g-1 at 77K , a CO2 excess uptake of 2.01 g g-1 at 298K, and an exceptionally high excess methane storage capacity of 308 mg g-1 at 298K. ; _publ_contact_author_name 'Stefan Kaskel' _publ_contact_author_address ;Department of Inorganic Chemistry Dresden University of Technology Bergstr. 66, 01069 Dresden (Germany) ; _publ_contact_author_email stefan.kaskel@chemie.tu-dresden.de _publ_contact_author_phone (+49)351-463-34885 _publ_contact_author_fax '(+49)351-463-37287 ' loop_ _publ_author_name _publ_author_address 'Ulrich Stoeck' ;Department of Inorganic Chemistry Dresden University of Technology Bergstr. 66, 01069 Dresden (Germany) ; 'Simon Krause' ;Department of Inorganic Chemistry Dresden University of Technology Bergstr. 66, 01069 Dresden (Germany) ; 'Volodymyr Bon' ;Department of Inorganic Chemistry Dresden University of Technology Bergstr. 66, 01069 Dresden (Germany) ; 'Irena Senkovska' ;Department of Inorganic Chemistry Dresden University of Technology Bergstr. 66, 01069 Dresden (Germany) ; 'Stefan Kaskel' ;Department of Inorganic Chemistry Dresden University of Technology Bergstr. 66, 01069 Dresden (Germany) ; data_DUT-49(Co) _database_code_depnum_ccdc_archive 'CCDC 890364' #TrackingRef '- DUT-49(Co)_revised_CCDC890364.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H20 Co2 N2 O10' _chemical_formula_weight 806.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0060 0.0030 '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 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3090 1.4430 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Fm-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y, x+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'y, -x+1/2, z+1/2' '-y, x+1/2, z+1/2' 'x, z+1/2, -y+1/2' '-x, z+1/2, y+1/2' '-x, -z+1/2, -y+1/2' 'x, -z+1/2, y+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' '-z, y+1/2, x+1/2' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1/2, x, -z+1/2' '-y+1/2, -x, -z+1/2' 'y+1/2, -x, z+1/2' '-y+1/2, x, z+1/2' 'x+1/2, z, -y+1/2' '-x+1/2, z, y+1/2' '-x+1/2, -z, -y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' '-z+1/2, y, x+1/2' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, -z' '-y+1/2, -x+1/2, -z' 'y+1/2, -x+1/2, z' '-y+1/2, x+1/2, z' 'x+1/2, z+1/2, -y' '-x+1/2, z+1/2, y' '-x+1/2, -z+1/2, -y' 'x+1/2, -z+1/2, y' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' '-z+1/2, y+1/2, x' '-z+1/2, -y+1/2, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' '-x, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' '-z, -x+1/2, -y+1/2' '-z, x+1/2, y+1/2' 'z, x+1/2, -y+1/2' 'z, -x+1/2, y+1/2' '-y, -z+1/2, -x+1/2' 'y, -z+1/2, x+1/2' '-y, z+1/2, x+1/2' 'y, z+1/2, -x+1/2' '-y, -x+1/2, z+1/2' 'y, x+1/2, z+1/2' '-y, x+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' '-x, -z+1/2, y+1/2' 'x, -z+1/2, -y+1/2' 'x, z+1/2, y+1/2' '-x, z+1/2, -y+1/2' '-z, -y+1/2, x+1/2' '-z, y+1/2, -x+1/2' 'z, -y+1/2, -x+1/2' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' '-z+1/2, -x, -y+1/2' '-z+1/2, x, y+1/2' 'z+1/2, x, -y+1/2' 'z+1/2, -x, y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/2, -z, x+1/2' '-y+1/2, z, x+1/2' 'y+1/2, z, -x+1/2' '-y+1/2, -x, z+1/2' 'y+1/2, x, z+1/2' '-y+1/2, x, -z+1/2' 'y+1/2, -x, -z+1/2' '-x+1/2, -z, y+1/2' 'x+1/2, -z, -y+1/2' 'x+1/2, z, y+1/2' '-x+1/2, z, -y+1/2' '-z+1/2, -y, x+1/2' '-z+1/2, y, -x+1/2' 'z+1/2, -y, -x+1/2' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-z+1/2, -x+1/2, -y' '-z+1/2, x+1/2, y' 'z+1/2, x+1/2, -y' 'z+1/2, -x+1/2, y' '-y+1/2, -z+1/2, -x' 'y+1/2, -z+1/2, x' '-y+1/2, z+1/2, x' 'y+1/2, z+1/2, -x' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' '-y+1/2, x+1/2, -z' 'y+1/2, -x+1/2, -z' '-x+1/2, -z+1/2, y' 'x+1/2, -z+1/2, -y' 'x+1/2, z+1/2, y' '-x+1/2, z+1/2, -y' '-z+1/2, -y+1/2, x' '-z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, -x' 'z+1/2, y+1/2, x' _cell_length_a 46.730(10) _cell_length_b 46.730(10) _cell_length_c 46.730(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 102044(38) _cell_formula_units_Z 24 _cell_measurement_temperature 263(2) _cell_measurement_reflns_used 735 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.36 _exptl_crystal_description cubic _exptl_crystal_colour purple _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9792 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9705 _exptl_absorpt_correction_T_max 0.9705 _exptl_absorpt_process_details Scala _exptl_special_details ; The meaurement was performed at Helmholz cetntre Berlin for materials and energy, beamline MX BL-14.2, equipped with 1-axis goniometer allowing only phi rotation of the crystal. Unfortunately, the beamline is not equipped with tools, allowing to provide numerical absorption correction of measured crystal. On this ground, Scala program was used for scaling reflection intensities. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_reflns_number 9373 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 2 _diffrn_reflns_limit_k_max 59 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 34.14 _reflns_number_total 5183 _reflns_number_gt 1909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement Mosflm _computing_data_reduction Scala _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material enCIFer _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^)+(0.1000P)^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 0.00013(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5183 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0798 _refine_ls_wR_factor_ref 0.2487 _refine_ls_wR_factor_gt 0.2324 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _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 Co1 Co 0.0000 1.0000 0.35220(2) 0.1086(4) Uani 1 8 d S . . Co2 Co 0.0000 1.0000 0.29162(2) 0.1227(5) Uani 1 8 d S . . O1 O 0.0000 0.95713(7) 0.34656(8) 0.1482(11) Uani 1 2 d S . . O2 O 0.0000 0.95753(7) 0.29798(8) 0.1658(12) Uani 1 2 d S . . O3 O 0.0000 1.0000 0.24778(14) 0.245(4) Uani 1 8 d S . . O4 O 0.0000 1.0000 0.39600(13) 0.199(3) Uani 1 8 d S . . N1 N 0.0000 0.82507(8) 0.32507(8) 0.207(3) Uani 1 4 d S . . C1 C 0.0000 0.94606(11) 0.32219(14) 0.1423(15) Uani 1 2 d S . . C2 C 0.0000 0.91334(11) 0.32207(12) 0.1561(16) Uani 1 2 d S . . C3 C 0.0000 0.89819(10) 0.34723(10) 0.1462(15) Uani 1 2 d S . . H3A H 0.0000 0.9078 0.3647 0.175 Uiso 1 2 calc SR . . C4 C 0.0000 0.86865(10) 0.34656(8) 0.1616(18) Uani 1 2 d S . . C5 C 0.0000 0.85444(11) 0.31983(11) 0.190(3) Uani 1 2 d S . . C6 C 0.0000 0.86862(12) 0.29441(12) 0.201(3) Uani 1 2 d S . . H6 H 0.0000 0.8588 0.2771 0.241 Uiso 1 2 calc SR . . C7 C 0.0000 0.89785(13) 0.29544(10) 0.188(2) Uani 1 2 d S . . H7 H 0.0000 0.9081 0.2784 0.225 Uiso 1 2 calc SR . . C8 C 0.0000 0.80311(11) 0.30311(11) 0.201(5) Uani 1 4 d S . . C9 C 0.0204(2) 0.80252(19) 0.28440(17) 0.250(7) Uani 0.50 1 d P A -1 H9A H 0.0348 0.8163 0.2850 0.300 Uiso 0.50 1 calc PR A -1 C10 C 0.02101(19) 0.78080(15) 0.26278(16) 0.229(5) Uani 0.50 1 d P A -1 H10A H 0.0360 0.7803 0.2498 0.275 Uiso 0.50 1 calc PR A -1 C11 C 0.0000 0.76111(10) 0.26111(10) 0.202(4) Uani 1 4 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 Co1 0.1205(6) 0.1205(6) 0.0846(7) 0.000 0.000 0.000 Co2 0.1426(7) 0.1426(7) 0.0830(7) 0.000 0.000 0.000 O1 0.169(3) 0.131(2) 0.145(3) -0.0229(19) 0.000 0.000 O2 0.206(3) 0.149(3) 0.142(3) 0.004(2) 0.000 0.000 O3 0.316(6) 0.316(6) 0.103(5) 0.000 0.000 0.000 O4 0.247(5) 0.247(5) 0.102(4) 0.000 0.000 0.000 N1 0.395(11) 0.113(3) 0.113(3) -0.031(3) 0.000 0.000 C1 0.149(4) 0.126(4) 0.151(5) -0.002(4) 0.000 0.000 C2 0.198(5) 0.135(4) 0.135(4) -0.017(3) 0.000 0.000 C3 0.211(5) 0.113(3) 0.115(3) -0.019(3) 0.000 0.000 C4 0.269(6) 0.116(3) 0.099(3) -0.017(2) 0.000 0.000 C5 0.347(8) 0.113(4) 0.108(4) -0.021(3) 0.000 0.000 C6 0.356(8) 0.122(4) 0.124(4) -0.025(3) 0.000 0.000 C7 0.303(7) 0.154(5) 0.107(4) -0.010(3) 0.000 0.000 C8 0.371(16) 0.115(4) 0.115(4) -0.039(5) 0.000 0.000 C9 0.372(13) 0.191(9) 0.188(11) -0.095(9) 0.067(7) -0.070(7) C10 0.362(12) 0.159(8) 0.166(7) -0.072(7) 0.060(6) -0.050(6) C11 0.371(14) 0.118(3) 0.118(3) -0.036(4) 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 Co1 O1 2.021(3) . ? Co1 O1 2.021(3) 110_465 ? Co1 O1 2.021(3) 109_665 ? Co1 O1 2.021(3) 2_575 ? Co1 O4 2.047(6) . ? Co2 O2 2.007(4) 109_665 ? Co2 O2 2.007(4) 2_575 ? Co2 O2 2.007(4) 110_465 ? Co2 O2 2.007(4) . ? Co2 O3 2.048(7) . ? O1 C1 1.251(5) . ? O2 C1 1.252(5) . ? N1 C5 1.394(5) 42_554 ? N1 C5 1.394(5) . ? N1 C8 1.451(9) . ? C1 C2 1.529(6) . ? C2 C3 1.372(6) . ? C2 C7 1.440(6) . ? C3 C4 1.381(5) . ? C3 H3A 0.9300 . ? C4 C5 1.414(5) . ? C4 C4 1.460(9) 42_554 ? C5 C6 1.360(6) . ? C6 C7 1.367(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.294(8) 42_554 ? C8 C9 1.294(8) 100 ? C8 C9 1.294(8) 139_554 ? C8 C9 1.294(8) . ? C9 C10 1.432(8) . ? C9 H9A 0.9300 . ? C10 C11 1.348(7) . ? C10 H10A 0.9300 . ? C11 C10 1.348(7) 139_554 ? C11 C10 1.348(7) 100 ? C11 C10 1.348(7) 42_554 ? C11 C11 1.469(14) 121_565 ? 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 O1 Co1 O1 89.03(3) . 110_465 ? O1 Co1 O1 89.03(3) . 109_665 ? O1 Co1 O1 165.0(2) 110_465 109_665 ? O1 Co1 O1 165.0(2) . 2_575 ? O1 Co1 O1 89.03(3) 110_465 2_575 ? O1 Co1 O1 89.03(3) 109_665 2_575 ? O1 Co1 O4 97.49(10) . . ? O1 Co1 O4 97.49(10) 110_465 . ? O1 Co1 O4 97.49(10) 109_665 . ? O1 Co1 O4 97.49(10) 2_575 . ? O2 Co2 O2 88.74(3) 109_665 2_575 ? O2 Co2 O2 163.0(2) 109_665 110_465 ? O2 Co2 O2 88.74(3) 2_575 110_465 ? O2 Co2 O2 88.74(3) 109_665 . ? O2 Co2 O2 163.0(2) 2_575 . ? O2 Co2 O2 88.74(3) 110_465 . ? O2 Co2 O3 98.52(11) 109_665 . ? O2 Co2 O3 98.52(11) 2_575 . ? O2 Co2 O3 98.52(11) 110_465 . ? O2 Co2 O3 98.52(11) . . ? C1 O1 Co1 121.9(3) . . ? C1 O2 Co2 123.9(4) . . ? C5 N1 C5 110.2(5) 42_554 . ? C5 N1 C8 124.9(3) 42_554 . ? C5 N1 C8 124.9(3) . . ? O1 C1 O2 130.2(5) . . ? O1 C1 C2 114.6(5) . . ? O2 C1 C2 115.1(5) . . ? C3 C2 C7 118.7(5) . . ? C3 C2 C1 120.9(5) . . ? C7 C2 C1 120.4(5) . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 C4 133.7(2) . 42_554 ? C5 C4 C4 107.0(3) . 42_554 ? C6 C5 N1 129.3(4) . . ? C6 C5 C4 122.9(5) . . ? N1 C5 C4 107.9(5) . . ? C5 C6 C7 117.1(5) . . ? C5 C6 H6 121.4 . . ? C7 C6 H6 121.4 . . ? C6 C7 C2 122.2(5) . . ? C6 C7 H7 118.9 . . ? C2 C7 H7 118.9 . . ? C9 C8 C9 55.1(9) 42_554 100 ? C9 C8 C9 95.0(9) 42_554 139_554 ? C9 C8 C9 121.0(10) 100 139_554 ? C9 C8 C9 121.0(10) 42_554 . ? C9 C8 C9 95.0(9) 100 . ? C9 C8 C9 55.1(9) 139_554 . ? C9 C8 N1 119.5(5) 42_554 . ? C9 C8 N1 119.5(5) 100 . ? C9 C8 N1 119.5(5) 139_554 . ? C9 C8 N1 119.5(5) . . ? C8 C9 C10 120.4(9) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 120.7(8) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C10 52.4(7) 139_554 . ? C10 C11 C10 116.8(8) 139_554 100 ? C10 C11 C10 93.5(8) . 100 ? C10 C11 C10 93.5(8) 139_554 42_554 ? C10 C11 C10 116.8(8) . 42_554 ? C10 C11 C10 52.4(7) 100 42_554 ? C10 C11 C11 121.6(4) 139_554 121_565 ? C10 C11 C11 121.6(4) . 121_565 ? C10 C11 C11 121.6(4) 100 121_565 ? C10 C11 C11 121.6(4) 42_554 121_565 ? 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 O1 Co1 O1 C1 82.58(10) 110_465 . . . ? O1 Co1 O1 C1 -82.58(10) 109_665 . . . ? O1 Co1 O1 C1 0.000(3) 2_575 . . . ? O4 Co1 O1 C1 180.000(2) . . . . ? O2 Co2 O2 C1 81.57(11) 109_665 . . . ? O2 Co2 O2 C1 0.000(3) 2_575 . . . ? O2 Co2 O2 C1 -81.57(11) 110_465 . . . ? O3 Co2 O2 C1 180.000(2) . . . . ? Co1 O1 C1 O2 0.000(3) . . . . ? Co1 O1 C1 C2 180.000(2) . . . . ? Co2 O2 C1 O1 0.000(3) . . . . ? Co2 O2 C1 C2 180.000(1) . . . . ? O1 C1 C2 C3 0.000(3) . . . . ? O2 C1 C2 C3 180.000(2) . . . . ? O1 C1 C2 C7 180.000(2) . . . . ? O2 C1 C2 C7 0.000(3) . . . . ? C7 C2 C3 C4 0.000(2) . . . . ? C1 C2 C3 C4 180.000(2) . . . . ? C2 C3 C4 C5 0.000(2) . . . . ? C2 C3 C4 C4 180.000(2) . . . 42_554 ? C5 N1 C5 C6 180.000(2) 42_554 . . . ? C8 N1 C5 C6 0.000(2) . . . . ? C5 N1 C5 C4 0.000(2) 42_554 . . . ? C8 N1 C5 C4 180.000(2) . . . . ? C3 C4 C5 C6 0.000(2) . . . . ? C4 C4 C5 C6 180.000(2) 42_554 . . . ? C3 C4 C5 N1 180.000(1) . . . . ? C4 C4 C5 N1 0.000(1) 42_554 . . . ? N1 C5 C6 C7 180.000(2) . . . . ? C4 C5 C6 C7 0.000(2) . . . . ? C5 C6 C7 C2 0.000(3) . . . . ? C3 C2 C7 C6 0.000(2) . . . . ? C1 C2 C7 C6 180.000(2) . . . . ? C5 N1 C8 C9 57.9(5) 42_554 . . 42_554 ? C5 N1 C8 C9 -122.1(5) . . . 42_554 ? C5 N1 C8 C9 122.1(5) 42_554 . . 100 ? C5 N1 C8 C9 -57.9(5) . . . 100 ? C5 N1 C8 C9 -57.9(5) 42_554 . . 139_554 ? C5 N1 C8 C9 122.1(5) . . . 139_554 ? C5 N1 C8 C9 -122.1(5) 42_554 . . . ? C5 N1 C8 C9 57.9(5) . . . . ? C9 C8 C9 C10 -0.8(7) 42_554 . . . ? C9 C8 C9 C10 -52.7(12) 100 . . . ? C9 C8 C9 C10 72.0(10) 139_554 . . . ? N1 C8 C9 C10 179.2(7) . . . . ? C8 C9 C10 C11 1.7(14) . . . . ? C9 C10 C11 C10 -73.2(9) . . . 139_554 ? C9 C10 C11 C10 48.4(11) . . . 100 ? C9 C10 C11 C10 -0.8(6) . . . 42_554 ? C9 C10 C11 C11 179.2(6) . . . 121_565 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 34.14 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.466 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.030 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.004 -0.002 85584 5992 ' ' _platon_squeeze_details ; The SQUEEZE procedure (PLATON) was used to correct intensities corresponding to disordered solvent molecules, located in pores. The resulted hkl file was used at the final refinement stage. Crystal data from original dataset: Overall formula: C40H20Co2N2O10x4.6C5H9NO(NMP) Formula weight: 1261.84 Calculated density: 0.493 F(OOO): 15756 _exptl_absorpt_coefficient_mu 0.397 _refine_ls_R_factor_all 0.2161 _refine_ls_R_factor_gt 0.1390 _refine_ls_wR_factor_ref 0.4030 _refine_ls_wR_factor_gt 0.3726 _refine_ls_goodness_of_fit_ref 1.963 _refine_ls_restrained_S_all 1.963 _refine_diff_density_max 0.432 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.075 ; # Attachment '- DUT-49(Zn)_revised_CCDC890363.cif' data_DUT-49(Zn) _database_code_depnum_ccdc_archive 'CCDC 890363' #TrackingRef '- DUT-49(Zn)_revised_CCDC890363.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H20 N2 O10 Zn2' _chemical_formula_weight 819.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0060 0.0030 '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 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.0350 2.0980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Fm-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x, -y, -z' 'y, x, -z' '-x, y, -z' '-y, -x, -z' 'z, x, y' '-x, z, y' '-z, -x, y' 'x, -z, y' 'z, -x, -y' 'x, z, -y' '-z, x, -y' '-x, -z, -y' 'y, z, x' '-z, -y, -x' '-z, y, x' 'z, y, -x' 'z, -y, x' 'y, -z, -x' '-y, -z, x' '-y, z, -x' 'x, y+1/2, z+1/2' '-y, x+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'y, -x+1/2, z+1/2' 'x, -y+1/2, -z+1/2' 'y, x+1/2, -z+1/2' '-x, y+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'z, x+1/2, y+1/2' '-x, z+1/2, y+1/2' '-z, -x+1/2, y+1/2' 'x, -z+1/2, y+1/2' 'z, -x+1/2, -y+1/2' 'x, z+1/2, -y+1/2' '-z, x+1/2, -y+1/2' '-x, -z+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-z, -y+1/2, -x+1/2' '-z, y+1/2, x+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-y+1/2, x, z+1/2' '-x+1/2, -y, z+1/2' 'y+1/2, -x, z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x, -z+1/2' '-x+1/2, y, -z+1/2' '-y+1/2, -x, -z+1/2' 'z+1/2, x, y+1/2' '-x+1/2, z, y+1/2' '-z+1/2, -x, y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, -x, -y+1/2' 'x+1/2, z, -y+1/2' '-z+1/2, x, -y+1/2' '-x+1/2, -z, -y+1/2' 'y+1/2, z, x+1/2' '-z+1/2, -y, -x+1/2' '-z+1/2, y, x+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' '-y+1/2, z, -x+1/2' 'x+1/2, y+1/2, z' '-y+1/2, x+1/2, z' '-x+1/2, -y+1/2, z' 'y+1/2, -x+1/2, z' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z' '-x+1/2, y+1/2, -z' '-y+1/2, -x+1/2, -z' 'z+1/2, x+1/2, y' '-x+1/2, z+1/2, y' '-z+1/2, -x+1/2, y' 'x+1/2, -z+1/2, y' 'z+1/2, -x+1/2, -y' 'x+1/2, z+1/2, -y' '-z+1/2, x+1/2, -y' '-x+1/2, -z+1/2, -y' 'y+1/2, z+1/2, x' '-z+1/2, -y+1/2, -x' '-z+1/2, y+1/2, x' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' '-y+1/2, z+1/2, -x' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x, y, z' '-y, -x, z' 'x, -y, z' 'y, x, z' '-z, -x, -y' 'x, -z, -y' 'z, x, -y' '-x, z, -y' '-z, x, y' '-x, -z, y' 'z, -x, y' 'x, z, y' '-y, -z, -x' 'z, y, x' 'z, -y, -x' '-z, -y, x' '-z, y, -x' '-y, z, x' 'y, z, -x' 'y, -z, x' '-x, -y+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' 'x, y+1/2, -z+1/2' '-y, x+1/2, -z+1/2' '-x, y+1/2, z+1/2' '-y, -x+1/2, z+1/2' 'x, -y+1/2, z+1/2' 'y, x+1/2, z+1/2' '-z, -x+1/2, -y+1/2' 'x, -z+1/2, -y+1/2' 'z, x+1/2, -y+1/2' '-x, z+1/2, -y+1/2' '-z, x+1/2, y+1/2' '-x, -z+1/2, y+1/2' 'z, -x+1/2, y+1/2' 'x, z+1/2, y+1/2' '-y, -z+1/2, -x+1/2' 'z, y+1/2, x+1/2' 'z, -y+1/2, -x+1/2' '-z, -y+1/2, x+1/2' '-z, y+1/2, -x+1/2' '-y, z+1/2, x+1/2' 'y, z+1/2, -x+1/2' 'y, -z+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'y+1/2, -x, -z+1/2' 'x+1/2, y, -z+1/2' '-y+1/2, x, -z+1/2' '-x+1/2, y, z+1/2' '-y+1/2, -x, z+1/2' 'x+1/2, -y, z+1/2' 'y+1/2, x, z+1/2' '-z+1/2, -x, -y+1/2' 'x+1/2, -z, -y+1/2' 'z+1/2, x, -y+1/2' '-x+1/2, z, -y+1/2' '-z+1/2, x, y+1/2' '-x+1/2, -z, y+1/2' 'z+1/2, -x, y+1/2' 'x+1/2, z, y+1/2' '-y+1/2, -z, -x+1/2' 'z+1/2, y, x+1/2' 'z+1/2, -y, -x+1/2' '-z+1/2, -y, x+1/2' '-z+1/2, y, -x+1/2' '-y+1/2, z, x+1/2' 'y+1/2, z, -x+1/2' 'y+1/2, -z, x+1/2' '-x+1/2, -y+1/2, -z' 'y+1/2, -x+1/2, -z' 'x+1/2, y+1/2, -z' '-y+1/2, x+1/2, -z' '-x+1/2, y+1/2, z' '-y+1/2, -x+1/2, z' 'x+1/2, -y+1/2, z' 'y+1/2, x+1/2, z' '-z+1/2, -x+1/2, -y' 'x+1/2, -z+1/2, -y' 'z+1/2, x+1/2, -y' '-x+1/2, z+1/2, -y' '-z+1/2, x+1/2, y' '-x+1/2, -z+1/2, y' 'z+1/2, -x+1/2, y' 'x+1/2, z+1/2, y' '-y+1/2, -z+1/2, -x' 'z+1/2, y+1/2, x' 'z+1/2, -y+1/2, -x' '-z+1/2, -y+1/2, x' '-z+1/2, y+1/2, -x' '-y+1/2, z+1/2, x' 'y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, x' _cell_length_a 46.806(5) _cell_length_b 46.806(5) _cell_length_c 46.806(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 102541(20) _cell_formula_units_Z 24 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 735 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.36 _exptl_crystal_description cubic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9936 _exptl_absorpt_coefficient_mu 0.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9843 _exptl_absorpt_correction_T_max 0.9843 _exptl_absorpt_process_details Scala _exptl_special_details ; The meaurement was performed at Helmholz cetntre Berlin for materials and energy, beamline MX BL-14.2, equipped with 1-axis goniometer allowing only phi rotation of the crystal. Unfortunately, the beamline is not equipped with tools, allowing to provide numerical absorption correction of measured crystal. On this ground, Scala program was used for scaling reflection intensities. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_reflns_number 9434 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 2 _diffrn_reflns_limit_k_max 59 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 34.12 _reflns_number_total 5206 _reflns_number_gt 2841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement Mosflm _computing_data_reduction Scala _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material enCIFer _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^)+(0.1343P)^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 5206 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1968 _refine_ls_wR_factor_gt 0.1822 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _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 Zn1 Zn 0.0000 1.0000 0.353658(11) 0.0836(2) Uani 1 8 d S . . Zn2 Zn 0.0000 1.0000 0.290296(12) 0.0955(3) Uani 1 8 d S . . O1 O 0.0000 0.95731(5) 0.34603(5) 0.1142(7) Uani 1 2 d S . . O2 O 0.0000 0.95752(5) 0.29821(6) 0.1303(8) Uani 1 2 d S . . O3 O 0.0000 1.0000 0.24784(10) 0.161(2) Uani 1 8 d S . . O4 O 0.0000 1.0000 0.39627(10) 0.176(2) Uani 1 8 d S . . N1 N 0.0000 0.82515(5) 0.32515(5) 0.163(2) Uani 1 4 d S . . C1 C 0.0000 0.94534(7) 0.32188(8) 0.1130(10) Uani 1 2 d S . . C2 C 0.0000 0.91311(7) 0.32183(7) 0.1195(10) Uani 1 2 d S . . C3 C 0.0000 0.89805(7) 0.34755(7) 0.1121(10) Uani 1 2 d S . . H3A H 0.0000 0.9077 0.3649 0.134 Uiso 1 2 calc SR . . C4 C 0.0000 0.86872(7) 0.34663(6) 0.1200(11) Uani 1 2 d S . . C5 C 0.0000 0.85434(8) 0.31987(8) 0.1419(15) Uani 1 2 d S . . C6 C 0.0000 0.86920(9) 0.29429(8) 0.1537(17) Uani 1 2 d S . . H6 H 0.0000 0.8597 0.2768 0.184 Uiso 1 2 calc SR . . C7 C 0.0000 0.89821(9) 0.29579(8) 0.1441(15) Uani 1 2 d S . . H7 H 0.0000 0.9086 0.2789 0.173 Uiso 1 2 calc SR . . C8 C 0.0000 0.80299(8) 0.30299(8) 0.155(2) Uani 1 4 d S . . C9 C 0.02187(16) 0.80217(13) 0.28431(12) 0.198(4) Uani 0.50 1 d P A -1 H9A H 0.0369 0.8151 0.2852 0.237 Uiso 0.50 1 calc PR A -1 C10 C 0.02050(16) 0.78008(12) 0.26294(13) 0.192(4) Uani 0.50 1 d P A -1 H10A H 0.0352 0.7793 0.2496 0.230 Uiso 0.50 1 calc PR A -1 C11 C 0.0000 0.76095(7) 0.26095(7) 0.153(2) Uani 1 4 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 Zn1 0.0962(3) 0.0962(3) 0.0583(3) 0.000 0.000 0.000 Zn2 0.1142(4) 0.1142(4) 0.0583(3) 0.000 0.000 0.000 O1 0.1359(17) 0.0929(14) 0.1139(16) -0.0088(12) 0.000 0.000 O2 0.170(2) 0.1117(16) 0.1096(16) 0.0088(13) 0.000 0.000 O3 0.201(3) 0.201(3) 0.080(3) 0.000 0.000 0.000 O4 0.225(4) 0.225(4) 0.078(3) 0.000 0.000 0.000 N1 0.312(8) 0.0881(17) 0.0881(17) -0.026(2) 0.000 0.000 C1 0.127(3) 0.106(2) 0.107(2) -0.002(2) 0.000 0.000 C2 0.162(3) 0.094(2) 0.103(2) -0.0086(18) 0.000 0.000 C3 0.154(3) 0.0880(19) 0.095(2) -0.0122(16) 0.000 0.000 C4 0.177(3) 0.097(2) 0.0854(18) -0.0136(15) 0.000 0.000 C5 0.234(5) 0.099(2) 0.093(2) -0.0199(18) 0.000 0.000 C6 0.257(5) 0.114(3) 0.090(2) -0.019(2) 0.000 0.000 C7 0.226(5) 0.113(3) 0.094(2) -0.0062(19) 0.000 0.000 C8 0.265(8) 0.100(2) 0.100(2) -0.021(3) 0.000 0.000 C9 0.306(9) 0.150(6) 0.138(5) -0.065(5) 0.064(5) -0.046(5) C10 0.288(8) 0.146(6) 0.141(5) -0.066(5) 0.057(5) -0.042(5) C11 0.241(8) 0.108(2) 0.108(2) -0.038(3) 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 Zn1 O4 1.994(5) . ? Zn1 O1 2.030(2) 4_465 ? Zn1 O1 2.030(2) 2_665 ? Zn1 O1 2.030(2) 3_575 ? Zn1 O1 2.030(2) . ? Zn2 O3 1.987(5) . ? Zn2 O2 2.023(2) 3_575 ? Zn2 O2 2.023(2) 2_665 ? Zn2 O2 2.023(2) 4_465 ? Zn2 O2 2.023(2) . ? O1 C1 1.261(4) . ? O2 C1 1.246(4) . ? N1 C5 1.388(4) 34_554 ? N1 C5 1.389(4) . ? N1 C8 1.466(6) . ? C1 C2 1.508(5) . ? C2 C3 1.395(4) . ? C2 C7 1.404(4) . ? C3 C4 1.374(4) . ? C3 H3A 0.9300 . ? C4 C5 1.422(4) . ? C4 C4 1.462(6) 34_554 ? C5 C6 1.385(5) . ? C6 C7 1.359(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.347(6) 34_554 ? C8 C9 1.347(6) 101 ? C8 C9 1.347(6) 136_554 ? C8 C9 1.347(6) . ? C9 C10 1.440(6) . ? C9 H9A 0.9300 . ? C10 C11 1.316(6) . ? C10 H10A 0.9300 . ? C11 C10 1.316(6) 136_554 ? C11 C10 1.316(6) 34_554 ? C11 C10 1.316(6) 101 ? C11 C11 1.449(10) 121_565 ? 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 O4 Zn1 O1 100.14(7) . 4_465 ? O4 Zn1 O1 100.14(7) . 2_665 ? O1 Zn1 O1 159.72(14) 4_465 2_665 ? O4 Zn1 O1 100.14(7) . 3_575 ? O1 Zn1 O1 88.22(2) 4_465 3_575 ? O1 Zn1 O1 88.22(2) 2_665 3_575 ? O4 Zn1 O1 100.14(7) . . ? O1 Zn1 O1 88.22(3) 4_465 . ? O1 Zn1 O1 88.22(2) 2_665 . ? O1 Zn1 O1 159.73(14) 3_575 . ? O3 Zn2 O2 100.56(8) . 3_575 ? O3 Zn2 O2 100.56(8) . 2_665 ? O2 Zn2 O2 88.07(3) 3_575 2_665 ? O3 Zn2 O2 100.56(8) . 4_465 ? O2 Zn2 O2 88.07(3) 3_575 4_465 ? O2 Zn2 O2 158.87(15) 2_665 4_465 ? O3 Zn2 O2 100.56(8) . . ? O2 Zn2 O2 158.88(15) 3_575 . ? O2 Zn2 O2 88.07(3) 2_665 . ? O2 Zn2 O2 88.07(3) 4_465 . ? C1 O1 Zn1 126.5(2) . . ? C1 O2 Zn2 127.8(2) . . ? C5 N1 C5 110.5(4) 34_554 . ? C5 N1 C8 124.75(19) 34_554 . ? C5 N1 C8 124.75(19) . . ? O2 C1 O1 126.4(3) . . ? O2 C1 C2 117.1(3) . . ? O1 C1 C2 116.5(3) . . ? C3 C2 C7 119.9(3) . . ? C3 C2 C1 120.3(3) . . ? C7 C2 C1 119.9(3) . . ? C4 C3 C2 118.6(3) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 C4 133.20(19) . 34_554 ? C5 C4 C4 106.8(2) . 34_554 ? C6 C5 N1 130.4(3) . . ? C6 C5 C4 121.6(3) . . ? N1 C5 C4 108.0(3) . . ? C7 C6 C5 117.2(3) . . ? C7 C6 H6 121.4 . . ? C5 C6 H6 121.4 . . ? C6 C7 C2 122.8(4) . . ? C6 C7 H7 118.6 . . ? C2 C7 H7 118.6 . . ? C9 C8 C9 52.1(6) 34_554 101 ? C9 C8 C9 98.9(7) 34_554 136_554 ? C9 C8 C9 122.7(7) 101 136_554 ? C9 C8 C9 122.7(7) 34_554 . ? C9 C8 C9 98.9(7) 101 . ? C9 C8 C9 52.1(6) 136_554 . ? C9 C8 N1 118.6(4) 34_554 . ? C9 C8 N1 118.6(4) 101 . ? C9 C8 N1 118.6(4) 136_554 . ? C9 C8 N1 118.6(4) . . ? C8 C9 C10 116.0(6) . . ? C8 C9 H9A 122.0 . . ? C10 C9 H9A 122.0 . . ? C11 C10 C9 124.8(6) . . ? C11 C10 H10A 117.6 . . ? C9 C10 H10A 117.6 . . ? C10 C11 C10 51.1(6) . 136_554 ? C10 C11 C10 115.8(7) . 34_554 ? C10 C11 C10 93.6(6) 136_554 34_554 ? C10 C11 C10 93.6(6) . 101 ? C10 C11 C10 115.8(7) 136_554 101 ? C10 C11 C10 51.1(6) 34_554 101 ? C10 C11 C11 122.1(3) . 121_565 ? C10 C11 C11 122.1(3) 136_554 121_565 ? C10 C11 C11 122.1(3) 34_554 121_565 ? C10 C11 C11 122.1(3) 101 121_565 ? 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 O4 Zn1 O1 C1 180.000(1) . . . . ? O1 Zn1 O1 C1 80.02(7) 4_465 . . . ? O1 Zn1 O1 C1 -80.02(7) 2_665 . . . ? O1 Zn1 O1 C1 0.000(2) 3_575 . . . ? O3 Zn2 O2 C1 180.000(1) . . . . ? O2 Zn2 O2 C1 0.000(2) 3_575 . . . ? O2 Zn2 O2 C1 79.61(7) 2_665 . . . ? O2 Zn2 O2 C1 -79.61(7) 4_465 . . . ? Zn2 O2 C1 O1 0.000(2) . . . . ? Zn2 O2 C1 C2 180.000(1) . . . . ? Zn1 O1 C1 O2 0.000(2) . . . . ? Zn1 O1 C1 C2 180.000(1) . . . . ? O2 C1 C2 C3 180.000(2) . . . . ? O1 C1 C2 C3 0.000(2) . . . . ? O2 C1 C2 C7 0.000(2) . . . . ? O1 C1 C2 C7 180.000(2) . . . . ? C7 C2 C3 C4 0.000(1) . . . . ? C1 C2 C3 C4 180.000(1) . . . . ? C2 C3 C4 C5 0.000(2) . . . . ? C2 C3 C4 C4 180.000(1) . . . 34_554 ? C5 N1 C5 C6 180.000(1) 34_554 . . . ? C8 N1 C5 C6 0.000(2) . . . . ? C5 N1 C5 C4 0.000(1) 34_554 . . . ? C8 N1 C5 C4 180.000(1) . . . . ? C3 C4 C5 C6 0.000(2) . . . . ? C4 C4 C5 C6 180.000(1) 34_554 . . . ? C3 C4 C5 N1 180.000(1) . . . . ? C4 C4 C5 N1 0.0 34_554 . . . ? N1 C5 C6 C7 180.000(1) . . . . ? C4 C5 C6 C7 0.000(2) . . . . ? C5 C6 C7 C2 0.000(2) . . . . ? C3 C2 C7 C6 0.000(2) . . . . ? C1 C2 C7 C6 180.000(1) . . . . ? C5 N1 C8 C9 60.0(4) 34_554 . . 34_554 ? C5 N1 C8 C9 -120.0(4) . . . 34_554 ? C5 N1 C8 C9 120.0(4) 34_554 . . 101 ? C5 N1 C8 C9 -60.0(4) . . . 101 ? C5 N1 C8 C9 -60.0(4) 34_554 . . 136_554 ? C5 N1 C8 C9 120.0(4) . . . 136_554 ? C5 N1 C8 C9 -120.0(4) 34_554 . . . ? C5 N1 C8 C9 60.0(4) . . . . ? C9 C8 C9 C10 0.5(4) 34_554 . . . ? C9 C8 C9 C10 -49.8(8) 101 . . . ? C9 C8 C9 C10 75.0(6) 136_554 . . . ? N1 C8 C9 C10 -179.5(4) . . . . ? C8 C9 C10 C11 -1.1(10) . . . . ? C9 C10 C11 C10 -72.0(7) . . . 136_554 ? C9 C10 C11 C10 0.6(5) . . . 34_554 ? C9 C10 C11 C10 48.6(9) . . . 101 ? C9 C10 C11 C11 -179.4(5) . . . 121_565 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 34.12 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.263 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.031 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.001 -0.003 -0.002 85919 6866 ' ' _platon_squeeze_details ; The SQUEEZE procedure (PLATON) was used to correct intensities corresponding to disordered solvent molecules, located in pores. The resulted hkl file was used at the final refinement stage. Crystal data from original dataset: Overall formula: C40H20N2O10Zn2x5.3C5H9NO(NMP) Formula weight: 1344.72 Calculated density: 0.523 F(OOO): 16805 _exptl_absorpt_coefficient_mu 0.553 _refine_ls_R_factor_all 0.1454 _refine_ls_R_factor_gt 0.1047 _refine_ls_wR_factor_ref 0.3419 _refine_ls_wR_factor_gt 0.3231 _refine_ls_goodness_of_fit_ref 2.005 _refine_ls_restrained_S_all 2.005 _refine_diff_density_max 0.561 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.083 ; # Attachment '- DUT49(Cu)_revised_CCDC889572.cif' data_DUT-49(Cu) _database_code_depnum_ccdc_archive 'CCDC 889572' #TrackingRef '- DUT49(Cu)_revised_CCDC889572.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H20 Cu2 N2 O10' _chemical_formula_weight 815.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0060 0.0030 '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' Cu Cu 0.1640 1.8640 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Fm-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x, -y, -z' 'y, x, -z' '-x, y, -z' '-y, -x, -z' 'z, x, y' '-x, z, y' '-z, -x, y' 'x, -z, y' 'z, -x, -y' 'x, z, -y' '-z, x, -y' '-x, -z, -y' 'y, z, x' '-z, -y, -x' '-z, y, x' 'z, y, -x' 'z, -y, x' 'y, -z, -x' '-y, -z, x' '-y, z, -x' 'x, y+1/2, z+1/2' '-y, x+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'y, -x+1/2, z+1/2' 'x, -y+1/2, -z+1/2' 'y, x+1/2, -z+1/2' '-x, y+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'z, x+1/2, y+1/2' '-x, z+1/2, y+1/2' '-z, -x+1/2, y+1/2' 'x, -z+1/2, y+1/2' 'z, -x+1/2, -y+1/2' 'x, z+1/2, -y+1/2' '-z, x+1/2, -y+1/2' '-x, -z+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-z, -y+1/2, -x+1/2' '-z, y+1/2, x+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-y+1/2, x, z+1/2' '-x+1/2, -y, z+1/2' 'y+1/2, -x, z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x, -z+1/2' '-x+1/2, y, -z+1/2' '-y+1/2, -x, -z+1/2' 'z+1/2, x, y+1/2' '-x+1/2, z, y+1/2' '-z+1/2, -x, y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, -x, -y+1/2' 'x+1/2, z, -y+1/2' '-z+1/2, x, -y+1/2' '-x+1/2, -z, -y+1/2' 'y+1/2, z, x+1/2' '-z+1/2, -y, -x+1/2' '-z+1/2, y, x+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' '-y+1/2, z, -x+1/2' 'x+1/2, y+1/2, z' '-y+1/2, x+1/2, z' '-x+1/2, -y+1/2, z' 'y+1/2, -x+1/2, z' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z' '-x+1/2, y+1/2, -z' '-y+1/2, -x+1/2, -z' 'z+1/2, x+1/2, y' '-x+1/2, z+1/2, y' '-z+1/2, -x+1/2, y' 'x+1/2, -z+1/2, y' 'z+1/2, -x+1/2, -y' 'x+1/2, z+1/2, -y' '-z+1/2, x+1/2, -y' '-x+1/2, -z+1/2, -y' 'y+1/2, z+1/2, x' '-z+1/2, -y+1/2, -x' '-z+1/2, y+1/2, x' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' '-y+1/2, z+1/2, -x' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x, y, z' '-y, -x, z' 'x, -y, z' 'y, x, z' '-z, -x, -y' 'x, -z, -y' 'z, x, -y' '-x, z, -y' '-z, x, y' '-x, -z, y' 'z, -x, y' 'x, z, y' '-y, -z, -x' 'z, y, x' 'z, -y, -x' '-z, -y, x' '-z, y, -x' '-y, z, x' 'y, z, -x' 'y, -z, x' '-x, -y+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' 'x, y+1/2, -z+1/2' '-y, x+1/2, -z+1/2' '-x, y+1/2, z+1/2' '-y, -x+1/2, z+1/2' 'x, -y+1/2, z+1/2' 'y, x+1/2, z+1/2' '-z, -x+1/2, -y+1/2' 'x, -z+1/2, -y+1/2' 'z, x+1/2, -y+1/2' '-x, z+1/2, -y+1/2' '-z, x+1/2, y+1/2' '-x, -z+1/2, y+1/2' 'z, -x+1/2, y+1/2' 'x, z+1/2, y+1/2' '-y, -z+1/2, -x+1/2' 'z, y+1/2, x+1/2' 'z, -y+1/2, -x+1/2' '-z, -y+1/2, x+1/2' '-z, y+1/2, -x+1/2' '-y, z+1/2, x+1/2' 'y, z+1/2, -x+1/2' 'y, -z+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'y+1/2, -x, -z+1/2' 'x+1/2, y, -z+1/2' '-y+1/2, x, -z+1/2' '-x+1/2, y, z+1/2' '-y+1/2, -x, z+1/2' 'x+1/2, -y, z+1/2' 'y+1/2, x, z+1/2' '-z+1/2, -x, -y+1/2' 'x+1/2, -z, -y+1/2' 'z+1/2, x, -y+1/2' '-x+1/2, z, -y+1/2' '-z+1/2, x, y+1/2' '-x+1/2, -z, y+1/2' 'z+1/2, -x, y+1/2' 'x+1/2, z, y+1/2' '-y+1/2, -z, -x+1/2' 'z+1/2, y, x+1/2' 'z+1/2, -y, -x+1/2' '-z+1/2, -y, x+1/2' '-z+1/2, y, -x+1/2' '-y+1/2, z, x+1/2' 'y+1/2, z, -x+1/2' 'y+1/2, -z, x+1/2' '-x+1/2, -y+1/2, -z' 'y+1/2, -x+1/2, -z' 'x+1/2, y+1/2, -z' '-y+1/2, x+1/2, -z' '-x+1/2, y+1/2, z' '-y+1/2, -x+1/2, z' 'x+1/2, -y+1/2, z' 'y+1/2, x+1/2, z' '-z+1/2, -x+1/2, -y' 'x+1/2, -z+1/2, -y' 'z+1/2, x+1/2, -y' '-x+1/2, z+1/2, -y' '-z+1/2, x+1/2, y' '-x+1/2, -z+1/2, y' 'z+1/2, -x+1/2, y' 'x+1/2, z+1/2, y' '-y+1/2, -z+1/2, -x' 'z+1/2, y+1/2, x' 'z+1/2, -y+1/2, -x' '-z+1/2, -y+1/2, x' '-z+1/2, y+1/2, -x' '-y+1/2, z+1/2, x' 'y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, x' _cell_length_a 46.588(5) _cell_length_b 46.588(5) _cell_length_c 46.588(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 101117(19) _cell_formula_units_Z 24 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 342 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.45 _exptl_crystal_description cubic _exptl_crystal_colour green _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9888 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9857 _exptl_absorpt_correction_T_max 0.9857 _exptl_absorpt_process_details Scala _exptl_special_details ; The meaurement was performed at Helmholz cetntre Berlin for materials and energy, beamline MX BL-14.2, equipped with 1-axis goniometer allowing only phi rotation of the crystal. Unfortunately, the beamline is not equipped with tools, allowing to provide numerical absorption correction of measured crystal. On this ground, Scala program was used for scaling reflection intensities. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_reflns_number 9285 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min 2 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 34.15 _reflns_number_total 5122 _reflns_number_gt 2402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement Mosflm _computing_data_reduction Scala _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material enCIFer _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^)+(0.1034P)^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 5122 _refine_ls_number_parameters 97 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _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 0.0000 1.0000 0.350490(14) 0.0670(3) Uani 1 8 d S . . Cu2 Cu 0.0000 1.0000 0.293952(15) 0.0788(3) Uani 1 8 d S . . O1 O 0.0000 0.95789(5) 0.34618(4) 0.0871(7) Uani 1 2 d S . . O2 O 0.0000 0.95805(5) 0.29804(5) 0.1024(8) Uani 1 2 d S . . O3 O 0.0000 1.0000 0.24645(10) 0.152(2) Uani 1 8 d S . . O4 O 0.0000 1.0000 0.39758(9) 0.1274(19) Uani 1 8 d S . . N1 N 0.0000 0.82547(6) 0.32547(6) 0.144(2) Uani 1 4 d S . . C1 C 0.0000 0.94612(8) 0.32245(8) 0.0853(9) Uani 1 2 d S . . C2 C 0.0000 0.91407(8) 0.32184(8) 0.0998(11) Uani 1 2 d S . . C3 C 0.0000 0.89829(7) 0.34735(7) 0.0911(10) Uani 1 2 d S . . H3A H 0.0000 0.9080 0.3648 0.109 Uiso 1 2 calc SR . . C4 C 0.0000 0.86921(7) 0.34718(7) 0.1013(12) Uani 1 2 d S . . C5 C 0.0000 0.85474(8) 0.32020(8) 0.1273(17) Uani 1 2 d S . . C6 C 0.0000 0.87040(10) 0.29449(9) 0.1386(18) Uani 1 2 d S . . H6 H 0.0000 0.8610 0.2769 0.166 Uiso 1 2 calc SR . . C7 C 0.0000 0.89895(9) 0.29562(8) 0.1222(15) Uani 1 2 d S . . H7 H 0.0000 0.9093 0.2785 0.147 Uiso 1 2 calc SR . . C8 C 0.0000 0.80321(9) 0.30321(9) 0.147(3) Uani 1 4 d S . . C9 C 0.02349(17) 0.80150(15) 0.28532(14) 0.190(5) Uani 0.50 1 d PD A -1 H9A H 0.0392 0.8136 0.2874 0.228 Uiso 0.50 1 calc PR A -1 C10 C 0.02236(16) 0.78012(13) 0.26347(13) 0.175(4) Uani 0.50 1 d PD A -1 H10A H 0.0373 0.7788 0.2502 0.210 Uiso 0.50 1 calc PR A -1 C11 C 0.0000 0.76161(8) 0.26161(8) 0.150(3) Uani 1 4 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 Cu1 0.0785(4) 0.0785(4) 0.0441(4) 0.000 0.000 0.000 Cu2 0.0963(4) 0.0963(4) 0.0438(4) 0.000 0.000 0.000 O1 0.1219(18) 0.0798(15) 0.0597(14) -0.0078(11) 0.000 0.000 O2 0.155(2) 0.0929(17) 0.0596(14) -0.0044(12) 0.000 0.000 O3 0.206(4) 0.206(4) 0.045(3) 0.000 0.000 0.000 O4 0.165(3) 0.165(3) 0.053(3) 0.000 0.000 0.000 N1 0.285(7) 0.0739(19) 0.0739(19) -0.035(2) 0.000 0.000 C1 0.098(3) 0.086(2) 0.072(2) -0.0033(19) 0.000 0.000 C2 0.135(3) 0.086(3) 0.078(2) -0.009(2) 0.000 0.000 C3 0.135(3) 0.076(2) 0.063(2) -0.0132(16) 0.000 0.000 C4 0.170(4) 0.069(2) 0.065(2) -0.0159(15) 0.000 0.000 C5 0.236(5) 0.079(3) 0.067(2) -0.022(2) 0.000 0.000 C6 0.241(6) 0.105(3) 0.069(3) -0.024(2) 0.000 0.000 C7 0.202(5) 0.092(3) 0.073(2) -0.020(2) 0.000 0.000 C8 0.285(10) 0.078(3) 0.078(3) -0.032(3) 0.000 0.000 C9 0.307(10) 0.127(7) 0.136(8) -0.072(6) 0.058(5) -0.057(5) C10 0.279(8) 0.123(6) 0.123(6) -0.069(6) 0.059(5) -0.056(5) C11 0.275(10) 0.087(3) 0.087(3) -0.034(3) 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 Cu1 O1 1.972(2) . ? Cu1 O1 1.972(2) 4_465 ? Cu1 O1 1.972(2) 3_575 ? Cu1 O1 1.972(2) 2_665 ? Cu1 O4 2.194(4) . ? Cu2 O2 1.963(2) 3_575 ? Cu2 O2 1.963(2) 2_665 ? Cu2 O2 1.963(2) 4_465 ? Cu2 O2 1.963(2) . ? Cu2 O3 2.213(5) . ? O1 C1 1.234(4) . ? O2 C1 1.266(4) . ? N1 C5 1.386(4) 34_554 ? N1 C5 1.386(4) . ? N1 C8 1.466(7) . ? C1 C2 1.493(5) . ? C2 C3 1.397(4) . ? C2 C7 1.410(4) . ? C3 C4 1.355(4) . ? C3 H3A 0.9300 . ? C4 C5 1.427(4) . ? C4 C4 1.451(7) 34_554 ? C5 C6 1.402(5) . ? C6 C7 1.331(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.378(7) 34_554 ? C8 C9 1.378(7) 101 ? C8 C9 1.378(7) 136_554 ? C8 C9 1.378(7) . ? C9 C10 1.426(6) . ? C9 H9A 0.9300 . ? C10 C11 1.355(6) . ? C10 H10A 0.9300 . ? C11 C10 1.355(6) 136_554 ? C11 C10 1.355(6) 101 ? C11 C10 1.355(6) 34_554 ? C11 C11 1.529(11) 121_565 ? 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 O1 Cu1 O1 89.407(13) . 4_465 ? O1 Cu1 O1 168.32(13) . 3_575 ? O1 Cu1 O1 89.407(13) 4_465 3_575 ? O1 Cu1 O1 89.407(13) . 2_665 ? O1 Cu1 O1 168.32(13) 4_465 2_665 ? O1 Cu1 O1 89.407(13) 3_575 2_665 ? O1 Cu1 O4 95.84(6) . . ? O1 Cu1 O4 95.84(6) 4_465 . ? O1 Cu1 O4 95.84(6) 3_575 . ? O1 Cu1 O4 95.84(6) 2_665 . ? O2 Cu2 O2 89.460(14) 3_575 2_665 ? O2 Cu2 O2 89.460(14) 3_575 4_465 ? O2 Cu2 O2 168.86(13) 2_665 4_465 ? O2 Cu2 O2 168.86(13) 3_575 . ? O2 Cu2 O2 89.460(13) 2_665 . ? O2 Cu2 O2 89.460(13) 4_465 . ? O2 Cu2 O3 95.57(7) 3_575 . ? O2 Cu2 O3 95.57(7) 2_665 . ? O2 Cu2 O3 95.57(7) 4_465 . ? O2 Cu2 O3 95.57(7) . . ? C1 O1 Cu1 122.2(2) . . ? C1 O2 Cu2 121.6(2) . . ? C5 N1 C5 110.4(4) 34_554 . ? C5 N1 C8 124.8(2) 34_554 . ? C5 N1 C8 124.8(2) . . ? O1 C1 O2 127.5(3) . . ? O1 C1 C2 117.5(3) . . ? O2 C1 C2 115.0(3) . . ? C3 C2 C7 118.3(4) . . ? C3 C2 C1 120.6(3) . . ? C7 C2 C1 121.1(3) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 118.5(3) . . ? C3 C4 C4 134.68(19) . 34_554 ? C5 C4 C4 106.8(2) . 34_554 ? N1 C5 C6 131.5(3) . . ? N1 C5 C4 108.0(3) . . ? C6 C5 C4 120.5(4) . . ? C7 C6 C5 119.1(4) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C2 122.2(4) . . ? C6 C7 H7 118.9 . . ? C2 C7 H7 118.9 . . ? C9 C8 C9 45.5(7) 34_554 101 ? C9 C8 C9 105.2(7) 34_554 136_554 ? C9 C8 C9 124.1(7) 101 136_554 ? C9 C8 C9 124.1(7) 34_554 . ? C9 C8 C9 105.2(7) 101 . ? C9 C8 C9 45.5(7) 136_554 . ? C9 C8 N1 117.9(3) 34_554 . ? C9 C8 N1 117.9(3) 101 . ? C9 C8 N1 117.9(3) 136_554 . ? C9 C8 N1 117.9(3) . . ? C8 C9 C10 116.3(6) . . ? C8 C9 H9A 121.8 . . ? C10 C9 H9A 121.8 . . ? C11 C10 C9 121.2(6) . . ? C11 C10 H10A 119.4 . . ? C9 C10 H10A 119.4 . . ? C10 C11 C10 47.8(6) 136_554 . ? C10 C11 C10 120.6(7) 136_554 101 ? C10 C11 C10 100.5(7) . 101 ? C10 C11 C10 100.5(7) 136_554 34_554 ? C10 C11 C10 120.6(7) . 34_554 ? C10 C11 C10 47.8(6) 101 34_554 ? C10 C11 C11 119.7(3) 136_554 121_565 ? C10 C11 C11 119.7(3) . 121_565 ? C10 C11 C11 119.7(3) 101 121_565 ? C10 C11 C11 119.7(3) 34_554 121_565 ? 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 O1 Cu1 O1 C1 84.19(6) 4_465 . . . ? O1 Cu1 O1 C1 0.000(2) 3_575 . . . ? O1 Cu1 O1 C1 -84.19(6) 2_665 . . . ? O4 Cu1 O1 C1 180.000(1) . . . . ? O2 Cu2 O2 C1 0.000(3) 3_575 . . . ? O2 Cu2 O2 C1 84.46(7) 2_665 . . . ? O2 Cu2 O2 C1 -84.46(7) 4_465 . . . ? O3 Cu2 O2 C1 180.000(1) . . . . ? Cu1 O1 C1 O2 0.000(2) . . . . ? Cu1 O1 C1 C2 180.000(1) . . . . ? Cu2 O2 C1 O1 0.000(2) . . . . ? Cu2 O2 C1 C2 180.000(1) . . . . ? O1 C1 C2 C3 0.000(2) . . . . ? O2 C1 C2 C3 180.000(2) . . . . ? O1 C1 C2 C7 180.000(2) . . . . ? O2 C1 C2 C7 0.000(2) . . . . ? C7 C2 C3 C4 0.000(2) . . . . ? C1 C2 C3 C4 180.000(1) . . . . ? C2 C3 C4 C5 0.000(2) . . . . ? C2 C3 C4 C4 180.000(2) . . . 34_554 ? C5 N1 C5 C6 180.000(2) 34_554 . . . ? C8 N1 C5 C6 0.000(2) . . . . ? C5 N1 C5 C4 0.000(1) 34_554 . . . ? C8 N1 C5 C4 180.000(1) . . . . ? C3 C4 C5 N1 180.0 . . . . ? C4 C4 C5 N1 0.0 34_554 . . . ? C3 C4 C5 C6 0.000(2) . . . . ? C4 C4 C5 C6 180.000(1) 34_554 . . . ? N1 C5 C6 C7 180.000(2) . . . . ? C4 C5 C6 C7 0.000(2) . . . . ? C5 C6 C7 C2 0.000(2) . . . . ? C3 C2 C7 C6 0.000(2) . . . . ? C1 C2 C7 C6 180.000(2) . . . . ? C5 N1 C8 C9 64.0(4) 34_554 . . 34_554 ? C5 N1 C8 C9 -116.0(4) . . . 34_554 ? C5 N1 C8 C9 116.0(4) 34_554 . . 101 ? C5 N1 C8 C9 -64.0(4) . . . 101 ? C5 N1 C8 C9 -64.0(4) 34_554 . . 136_554 ? C5 N1 C8 C9 116.0(4) . . . 136_554 ? C5 N1 C8 C9 -116.0(4) 34_554 . . . ? C5 N1 C8 C9 64.0(4) . . . . ? C9 C8 C9 C10 1.7(5) 34_554 . . . ? C9 C8 C9 C10 -44.5(10) 101 . . . ? C9 C8 C9 C10 78.8(7) 136_554 . . . ? N1 C8 C9 C10 -178.3(5) . . . . ? C8 C9 C10 C11 -3.5(11) . . . . ? C9 C10 C11 C10 -73.6(8) . . . 136_554 ? C9 C10 C11 C10 48.6(9) . . . 101 ? C9 C10 C11 C10 1.8(6) . . . 34_554 ? C9 C10 C11 C11 -178.2(6) . . . 121_565 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 34.15 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.364 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.031 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.003 -0.002 84702 6728 ' ' _platon_squeeze_details ; The SQUEEZE procedure (PLATON) was used to correct intensities corresponding to disordered solvent molecules, located in pores. The resulted hkl file was used at the final refinement stage. Crystal data from original dataset: Overall formula: C40H20Cu2N2O10x5.2C5H9NO (NMP) Formula weight: 1331.15 Calculated density: 0.525 F(OOO): 16627 _exptl_absorpt_coefficient_mu 0.504 _refine_ls_R_factor_all 0.1785 _refine_ls_R_factor_gt 0.1080 _refine_ls_wR_factor_ref 0.3473 _refine_ls_wR_factor_gt 0.3265 _refine_ls_goodness_of_fit_ref 1.723 _refine_ls_restrained_S_all 1.723 _refine_diff_density_max 0.414 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.071 ;