# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 #TrackingRef '- MOF1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Zn11(C9H3O6)6(NO3)4(C7H15NO)8 _chemical_formula_sum 'C110 H138 N12 O56 Zn11' _chemical_formula_weight 3243.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P m -3 m' 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, -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' _cell_length_a 20.6155(7) _cell_length_b 20.6155(7) _cell_length_c 20.6155(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8761.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2586 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8432 _exptl_absorpt_correction_T_max 0.8481 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 44794 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1591 _reflns_number_gt 1119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _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^)+(0.1830P)^2^+0.1741P] 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 1591 _refine_ls_number_parameters 67 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.2702 _refine_ls_wR_factor_gt 0.2512 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.42776(8) 0.0000 0.0794(7) Uani 1 8 d S . . Zn2 Zn 0.23888(4) 0.23888(4) 0.23888(4) 0.0693(6) Uani 1 6 d S . . Zn3 Zn 0.33549(5) 0.33549(5) 0.33549(5) 0.0977(8) Uani 1 6 d S . . O1 O 0.0689(2) 0.4458(3) 0.0689(2) 0.0987(19) Uani 1 2 d S . . O2 O 0.2157(2) 0.3279(3) 0.2157(2) 0.100(2) Uani 1 2 d S . . O3 O 0.2832(3) 0.3868(4) 0.2832(3) 0.144(3) Uani 1 2 d S . . O4 O 0.0000 0.3329(5) 0.0000 0.105(4) Uani 1 8 d S . . O5? O 0.3884(5) 0.3884(5) 0.3884(5) 0.333(19) Uani 1 6 d S . . O6? O 0.1772(4) 0.1772(4) 0.1772(4) 0.144(5) Uani 1 6 d S . . C1 C 0.0894(5) 0.5000 0.0894(5) 0.090(3) Uani 1 4 d S . . C2 C 0.1400(4) 0.5000 0.1400(4) 0.074(3) Uani 1 4 d S . . C3 C 0.1638(3) 0.4415(4) 0.1638(3) 0.078(2) Uani 1 2 d S . . H3 H 0.1481 0.4022 0.1481 0.093 Uiso 1 2 calc SR . . C4 C 0.2103(3) 0.4427(4) 0.2103(3) 0.082(2) Uani 1 2 d S . . C5 C 0.2339(4) 0.5000 0.2339(4) 0.081(3) Uani 1 4 d S . . H5 H 0.2658 0.5000 0.2658 0.097 Uiso 1 4 calc SR . . C6 C 0.2394(4) 0.3801(5) 0.2394(4) 0.095(3) Uani 1 2 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 0.0986(10) 0.0410(9) 0.0986(10) 0.000 0.000 0.000 Zn2 0.0693(6) 0.0693(6) 0.0693(6) -0.0018(4) -0.0018(4) -0.0018(4) Zn3 0.0977(8) 0.0977(8) 0.0977(8) -0.0132(5) -0.0132(5) -0.0132(5) O1 0.110(3) 0.077(4) 0.110(3) -0.006(2) -0.018(4) -0.006(2) O2 0.119(3) 0.064(3) 0.119(3) 0.003(2) -0.007(4) 0.003(2) O3 0.167(5) 0.098(5) 0.167(5) 0.013(3) -0.068(7) 0.013(3) O4 0.131(7) 0.052(6) 0.131(7) 0.000 0.000 0.000 O5? 0.333(19) 0.333(19) 0.333(19) -0.128(12) -0.128(12) -0.128(12) O6? 0.144(5) 0.144(5) 0.144(5) -0.026(5) -0.026(5) -0.026(5) C1 0.098(6) 0.073(8) 0.098(6) 0.000 0.006(7) 0.000 C2 0.083(5) 0.058(6) 0.083(5) 0.000 0.009(6) 0.000 C3 0.086(3) 0.062(5) 0.086(3) -0.007(3) 0.011(4) -0.007(3) C4 0.093(3) 0.061(5) 0.093(3) 0.009(3) 0.001(5) 0.009(3) C5 0.094(5) 0.055(6) 0.094(5) 0.000 0.001(7) 0.000 C6 0.104(4) 0.077(6) 0.104(4) 0.007(4) 0.018(6) 0.007(4) _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 1.956(11) . ? Zn1 O1 2.042(6) . ? Zn1 O1 2.042(6) 3 ? Zn1 O1 2.042(6) 28 ? Zn1 O1 2.042(6) 26 ? Zn1 Zn1 2.979(3) 25_565 ? Zn2 O2 1.956(6) 5 ? Zn2 O2 1.956(6) . ? Zn2 O2 1.956(6) 9 ? Zn2 O6? 2.201(14) . ? Zn3 O3 1.856(7) 5 ? Zn3 O3 1.856(7) . ? Zn3 O3 1.856(7) 9 ? Zn3 O5? 1.889(18) . ? O1 C1 1.268(8) . ? O2 C6 1.280(12) . ? O3 C6 1.285(12) . ? C1 O1 1.268(8) 27_565 ? C1 C2 1.477(18) . ? C2 C3 1.392(11) 27_565 ? C2 C3 1.392(11) . ? C3 C4 1.356(12) . ? C3 H3 0.9300 . ? C4 C5 1.367(11) . ? C4 C6 1.544(12) . ? C5 C4 1.367(11) 27_565 ? C5 H5 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O1 100.47(18) . . ? O4 Zn1 O1 100.47(18) . 3 ? O1 Zn1 O1 159.1(4) . 3 ? O4 Zn1 O1 100.47(18) . 28 ? O1 Zn1 O1 88.11(6) . 28 ? O1 Zn1 O1 88.11(6) 3 28 ? O4 Zn1 O1 100.47(18) . 26 ? O1 Zn1 O1 88.11(6) . 26 ? O1 Zn1 O1 88.11(6) 3 26 ? O1 Zn1 O1 159.1(4) 28 26 ? O4 Zn1 Zn1 180.0 . 25_565 ? O1 Zn1 Zn1 79.53(18) . 25_565 ? O1 Zn1 Zn1 79.53(18) 3 25_565 ? O1 Zn1 Zn1 79.53(18) 28 25_565 ? O1 Zn1 Zn1 79.53(18) 26 25_565 ? O2 Zn2 O2 113.53(17) 5 . ? O2 Zn2 O2 113.53(17) 5 9 ? O2 Zn2 O2 113.53(17) . 9 ? O2 Zn2 O6? 105.0(2) 5 . ? O2 Zn2 O6? 105.0(2) . . ? O2 Zn2 O6? 105.0(2) 9 . ? O3 Zn3 O3 109.0(3) 5 . ? O3 Zn3 O3 109.0(3) 5 9 ? O3 Zn3 O3 109.0(3) . 9 ? O3 Zn3 O5? 109.9(3) 5 . ? O3 Zn3 O5? 109.9(3) . . ? O3 Zn3 O5? 109.9(3) 9 . ? C1 O1 Zn1 128.6(7) . . ? C6 O2 Zn2 127.0(7) . . ? C6 O3 Zn3 139.0(7) . . ? O1 C1 O1 123.8(13) . 27_565 ? O1 C1 C2 118.1(6) . . ? O1 C1 C2 118.1(6) 27_565 . ? C3 C2 C3 120.3(11) 27_565 . ? C3 C2 C1 119.8(6) 27_565 . ? C3 C2 C1 119.8(6) . . ? C4 C3 C2 118.7(8) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 121.3(8) . . ? C3 C4 C6 122.2(8) . . ? C5 C4 C6 116.4(9) . . ? C4 C5 C4 119.5(12) . 27_565 ? C4 C5 H5 120.2 . . ? C4 C5 H5 120.2 27_565 . ? O2 C6 O3 128.9(9) . . ? O2 C6 C4 113.9(9) . . ? O3 C6 C4 117.2(9) . . ? 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 180.0 . . . . ? O1 Zn1 O1 C1 0.000(1) 3 . . . ? O1 Zn1 O1 C1 -79.70(17) 28 . . . ? O1 Zn1 O1 C1 79.70(17) 26 . . . ? Zn1 Zn1 O1 C1 0.0 25_565 . . . ? O2 Zn2 O2 C6 65.8(3) 5 . . . ? O2 Zn2 O2 C6 -65.8(3) 9 . . . ? O6? Zn2 O2 C6 180.000(1) . . . . ? O3 Zn3 O3 C6 -59.4(3) 5 . . . ? O3 Zn3 O3 C6 59.4(3) 9 . . . ? O5? Zn3 O3 C6 180.000(2) . . . . ? Zn1 O1 C1 O1 0.000(2) . . . 27_565 ? Zn1 O1 C1 C2 180.000(1) . . . . ? O1 C1 C2 C3 180.000(2) . . . 27_565 ? O1 C1 C2 C3 0.000(2) 27_565 . . 27_565 ? O1 C1 C2 C3 0.000(2) . . . . ? O1 C1 C2 C3 180.000(2) 27_565 . . . ? C3 C2 C3 C4 0.000(2) 27_565 . . . ? C1 C2 C3 C4 180.000(2) . . . . ? C2 C3 C4 C5 0.000(2) . . . . ? C2 C3 C4 C6 180.000(1) . . . . ? C3 C4 C5 C4 0.000(2) . . . 27_565 ? C6 C4 C5 C4 180.0 . . . 27_565 ? Zn2 O2 C6 O3 0.000(2) . . . . ? Zn2 O2 C6 C4 180.000(1) . . . . ? Zn3 O3 C6 O2 0.000(3) . . . . ? Zn3 O3 C6 C4 180.000(1) . . . . ? C3 C4 C6 O2 0.000(2) . . . . ? C5 C4 C6 O2 180.000(2) . . . . ? C3 C4 C6 O3 180.000(2) . . . . ? C5 C4 C6 O3 0.000(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.286 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.104 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 -0.019 -0.011 -0.010 6012 1573 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 838771' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 N6 O17 Zn4' _chemical_formula_weight 1098.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P213 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' '-z, x+1/2, -y+1/2' 'y, z, x' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' '-y+1/2, -z, x+1/2' _cell_length_a 14.2941(8) _cell_length_b 14.2941(8) _cell_length_c 14.2941(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2920.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour reddish-brown _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 1.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6413 _exptl_absorpt_correction_T_max 0.6984 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14025 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1718 _reflns_number_gt 1516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1907P)^2^+0.1677P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 1718 _refine_ls_number_parameters 102 _refine_ls_number_restraints 89 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.2523 _refine_ls_wR_factor_gt 0.2344 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.265 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3486(3) 0.8944(3) 0.5165(3) 0.0622(10) Uani 1 1 d DU . . C2 C 0.4255(3) 0.8328(3) 0.5317(3) 0.0656(10) Uani 1 1 d DU . . H2 H 0.4359 0.7826 0.4917 0.079 Uiso 1 1 calc R . . C3 C 0.2792(4) 0.8764(3) 0.4391(3) 0.0760(11) Uani 1 1 d U . . C4 C 0.1254(6) 0.9532(9) 0.7918(7) 0.1837(18) Uani 1 1 d DU . . H4A H 0.0943 0.9379 0.8493 0.276 Uiso 1 1 calc R . . H4B H 0.1664 1.0054 0.8018 0.276 Uiso 1 1 calc R . . H4C H 0.1611 0.9003 0.7709 0.276 Uiso 1 1 calc R . . C5 C 0.0725(8) 1.0671(7) 0.6870(8) 0.1797(18) Uani 1 1 d DU . . H5A H 0.0177 1.1042 0.6981 0.270 Uiso 1 1 calc R . . H5B H 0.0836 1.0627 0.6209 0.270 Uiso 1 1 calc R . . H5C H 0.1255 1.0958 0.7167 0.270 Uiso 1 1 calc R . . C6 C 0.0841(9) 0.9294(9) 0.6448(5) 0.1764(17) Uani 1 1 d DU . . H6 H 0.1098 0.8736 0.6664 0.212 Uiso 1 1 calc R . . N1 N 0.0590(6) 0.9765(7) 0.7241(5) 0.1775(17) Uani 1 1 d DU . . O1 O 0.2990(2) 0.8071(2) 0.3855(2) 0.0789(10) Uani 1 1 d . . . O2 O 0.3003(5) 0.6997(5) 0.1997(5) 0.183(5) Uani 1 3 d S . . O3 O 0.2178(3) 0.9326(2) 0.4254(3) 0.0845(10) Uani 1 1 d . . . O4 O 0.0893(10) 0.9244(11) 0.5665(6) 0.1526(16) Uani 0.50 1 d PDU . . Zn1 Zn 0.22027(3) 0.77973(3) 0.27973(3) 0.06126(18) Uani 1 3 d S . . Zn2 Zn 0.07348(4) 0.92652(4) 0.42652(4) 0.0818(3) 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 C1 0.0674(19) 0.0546(18) 0.065(2) 0.0035(16) -0.0078(17) 0.0001(16) C2 0.076(2) 0.063(2) 0.0579(18) 0.0017(17) 0.0067(19) 0.0017(19) C3 0.092(2) 0.0699(19) 0.066(2) 0.0044(18) 0.001(2) -0.003(2) C4 0.183(3) 0.230(3) 0.138(3) -0.011(3) 0.002(3) -0.037(3) C5 0.175(3) 0.225(3) 0.139(3) -0.012(3) 0.005(3) -0.031(3) C6 0.172(3) 0.226(3) 0.132(3) -0.013(3) 0.011(3) -0.036(3) N1 0.176(3) 0.228(3) 0.129(3) -0.014(3) 0.008(3) -0.037(3) O1 0.084(2) 0.0756(19) 0.0772(19) -0.0038(16) -0.0163(16) -0.0003(16) O2 0.183(5) 0.183(5) 0.183(5) -0.040(4) 0.040(4) 0.040(4) O3 0.0698(16) 0.0773(18) 0.106(2) 0.0032(19) -0.0261(18) -0.0008(16) O4 0.157(3) 0.199(3) 0.102(3) -0.020(3) 0.008(3) -0.032(3) Zn1 0.06126(18) 0.06126(18) 0.06126(18) -0.0005(2) 0.0005(2) 0.0005(2) Zn2 0.0818(3) 0.0818(3) 0.0818(3) -0.0126(3) 0.0126(3) 0.0126(3) _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 C1 C2 1.362(6) 10_466 ? C1 C2 1.424(6) . ? C1 C3 1.509(7) . ? C2 C1 1.362(6) 8_656 ? C2 H2 0.9300 . ? C3 O3 1.205(7) . ? C3 O1 1.285(6) . ? C4 N1 1.395(11) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 N1 1.413(12) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 O4 1.124(10) . ? C6 N1 1.367(11) . ? C6 H6 0.9300 . ? O1 Zn1 1.925(3) . ? O2 Zn1 1.981(12) . ? O3 Zn2 2.065(4) . ? O4 Zn2 2.013(9) . ? Zn1 O1 1.925(3) 6_564 ? Zn1 O1 1.925(3) 11_655 ? Zn2 O4 2.013(9) 6_564 ? Zn2 O4 2.013(9) 11_655 ? Zn2 O3 2.065(4) 6_564 ? Zn2 O3 2.065(4) 11_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C2 120.9(4) 10_466 . ? C2 C1 C3 118.0(4) 10_466 . ? C2 C1 C3 120.9(4) . . ? C1 C2 C1 119.1(4) 8_656 . ? C1 C2 H2 120.5 8_656 . ? C1 C2 H2 120.5 . . ? O3 C3 O1 125.3(5) . . ? O3 C3 C1 119.0(4) . . ? O1 C3 C1 115.1(5) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 N1 151.0(15) . . ? O4 C6 H6 104.5 . . ? N1 C6 H6 104.5 . . ? C6 N1 C4 106.2(9) . . ? C6 N1 C5 95.9(8) . . ? C4 N1 C5 112.7(9) . . ? C3 O1 Zn1 119.7(3) . . ? C3 O3 Zn2 134.3(3) . . ? C6 O4 Zn2 168.9(14) . . ? O1 Zn1 O1 114.74(8) 6_564 . ? O1 Zn1 O1 114.74(8) 6_564 11_655 ? O1 Zn1 O1 114.74(8) . 11_655 ? O1 Zn1 O2 103.48(10) 6_564 . ? O1 Zn1 O2 103.48(10) . . ? O1 Zn1 O2 103.48(10) 11_655 . ? O4 Zn2 O4 97.2(6) . 6_564 ? O4 Zn2 O4 97.2(6) . 11_655 ? O4 Zn2 O4 97.2(6) 6_564 11_655 ? O4 Zn2 O3 86.7(5) . 6_564 ? O4 Zn2 O3 84.1(4) 6_564 6_564 ? O4 Zn2 O3 175.7(4) 11_655 6_564 ? O4 Zn2 O3 84.1(4) . . ? O4 Zn2 O3 175.7(4) 6_564 . ? O4 Zn2 O3 86.7(5) 11_655 . ? O3 Zn2 O3 91.97(15) 6_564 . ? O4 Zn2 O3 175.7(4) . 11_655 ? O4 Zn2 O3 86.7(5) 6_564 11_655 ? O4 Zn2 O3 84.1(4) 11_655 11_655 ? O3 Zn2 O3 91.97(15) 6_564 11_655 ? O3 Zn2 O3 91.97(14) . 11_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.989 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.175 _database_code_depnum_ccdc_archive 'CCDC 963915' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_11p _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H36 N8 O94 Zn22' _chemical_formula_weight 4388.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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, -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, -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' _cell_length_a 20.4666(8) _cell_length_b 20.4666(8) _cell_length_c 20.4666(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8573.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2151 _exptl_absorpt_coefficient_mu 1.556 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.721 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90052 _diffrn_reflns_av_R_equivalents 0.0871 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.30 _reflns_number_total 1778 _reflns_number_gt 1471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1745P)^2^+7.6599P] 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 1778 _refine_ls_number_parameters 73 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.2818 _refine_ls_wR_factor_gt 0.2615 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.112 _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 C1 C 0.3773(7) 0.7615(4) 0.7615(4) 0.113(3) Uani 1 2 d S . . C2 C 0.5000 0.9117(4) 0.9117(4) 0.082(3) Uani 1 4 d S . . C3 C 0.5000 0.8608(3) 0.8608(3) 0.076(2) Uani 1 4 d S . . C4 C 0.4407(4) 0.8356(3) 0.8356(3) 0.084(2) Uani 1 2 d S . . H4 H 0.4001 0.8515 0.8515 0.101 Uiso 1 2 calc SR . . C5 C 0.4418(4) 0.7878(3) 0.7878(3) 0.090(2) Uani 1 2 d S . . C6 C 0.5000 0.7651(4) 0.7651(4) 0.099(4) Uani 1 4 d S . . H6 H 0.5000 0.7323 0.7323 0.118 Uiso 1 4 calc SR . . O1 O 0.3275(4) 0.7826(3) 0.7826(3) 0.112(2) Uani 1 2 d S . . O2 O 0.3859(6) 0.7179(3) 0.7179(3) 0.228(7) Uani 1 2 d S . . O3 O 0.3283(5) 1.0000 1.0000 0.088(3) Uani 1 8 d S . . O4 O 0.4445(3) 0.93163(17) 0.93163(17) 0.0925(17) Uani 1 2 d S . . O5 O 0.3917(5) 0.6083(5) 0.6083(5) 0.225(10) Uani 1 6 d S . . N1 N 0.1782(6) 0.8218(6) 0.8218(6) 0.159(8) Uani 1 6 d S . . Zn1 Zn 0.33696(3) 0.66304(3) 0.66304(3) 0.0716(6) Uani 1 6 d SU . . Zn2 Zn 0.42623(7) 1.0000 1.0000 0.0604(5) Uani 1 8 d S . . Zn3 Zn 0.23581(5) 0.76419(5) 0.76419(5) 0.0946(7) Uani 1 6 d S . . O6 O 0.2116(15) 0.7884(15) 0.866(2) 0.218(12) Uani 0.33 2 d SPU . . 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 C1 0.133(9) 0.104(5) 0.104(5) -0.027(6) -0.014(4) -0.014(4) C2 0.112(9) 0.067(4) 0.067(4) 0.000(5) 0.000 0.000 C3 0.076(6) 0.076(4) 0.076(4) -0.020(5) 0.000 0.000 C4 0.089(5) 0.082(3) 0.082(3) -0.008(4) 0.009(3) 0.009(3) C5 0.087(5) 0.091(3) 0.091(3) -0.025(5) -0.005(3) -0.005(3) C6 0.121(10) 0.088(5) 0.088(5) -0.041(6) 0.000 0.000 O1 0.104(5) 0.116(3) 0.116(3) -0.014(4) -0.007(3) -0.007(3) O2 0.155(9) 0.265(10) 0.265(10) -0.173(12) -0.036(4) -0.036(4) O3 0.067(6) 0.099(5) 0.099(5) 0.000 0.000 0.000 O4 0.111(4) 0.083(2) 0.083(2) -0.025(3) 0.006(2) 0.006(2) O5 0.225(10) 0.225(10) 0.225(10) -0.068(8) 0.068(8) 0.068(8) N1 0.159(8) 0.159(8) 0.159(8) -0.024(8) 0.024(8) 0.024(8) Zn1 0.0716(6) 0.0716(6) 0.0716(6) -0.0123(3) 0.0123(3) 0.0123(3) Zn2 0.0602(9) 0.0605(6) 0.0605(6) 0.000 0.000 0.000 Zn3 0.0946(7) 0.0946(7) 0.0946(7) -0.0164(5) 0.0164(5) 0.0164(5) O6 0.223(12) 0.223(12) 0.207(16) -0.004(7) 0.004(7) 0.003(10) _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 C1 O1 1.190(14) . ? C1 O2 1.274(14) . ? C1 C5 1.524(14) . ? C2 O4 1.274(7) . ? C2 O4 1.274(7) 29_655 ? C2 C3 1.474(15) . ? C3 C4 1.416(10) . ? C3 C4 1.416(10) 29_655 ? C4 C5 1.382(11) . ? C4 H4 0.9500 . ? C5 C6 1.360(10) . ? C6 C5 1.360(10) 29_655 ? C6 H6 0.9500 . ? O1 Zn3 1.951(8) . ? O2 Zn1 1.877(8) . ? O3 Zn2 2.003(10) . ? O4 Zn2 2.014(5) . ? O5 Zn1 1.940(16) . ? N1 O6 1.32(4) . ? N1 O6 1.32(4) 11_665 ? N1 O6 1.32(4) 40 ? N1 Zn3 2.04(2) . ? Zn1 O2 1.877(8) 45_656 ? Zn1 O2 1.877(8) 30_665 ? Zn2 O4 2.014(5) 5_577 ? Zn2 O4 2.014(5) 31_575 ? Zn2 O4 2.014(5) 27_557 ? Zn2 Zn2 3.020(3) 25_677 ? Zn3 O1 1.951(8) 45_656 ? Zn3 O1 1.951(8) 30_665 ? Zn3 O6 2.19(5) 40 ? Zn3 O6 2.19(5) 11_665 ? Zn3 O6 2.19(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 128.9(11) . . ? O1 C1 C5 119.0(9) . . ? O2 C1 C5 112.1(11) . . ? O4 C2 O4 126.1(11) . 29_655 ? O4 C2 C3 116.9(5) . . ? O4 C2 C3 116.9(5) 29_655 . ? C4 C3 C4 118.0(9) . 29_655 ? C4 C3 C2 121.0(5) . . ? C4 C3 C2 121.0(5) 29_655 . ? C5 C4 C3 120.1(8) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 119.8(8) . . ? C6 C5 C1 121.1(8) . . ? C4 C5 C1 119.1(9) . . ? C5 C6 C5 122.3(10) 29_655 . ? C5 C6 H6 118.9 29_655 . ? C5 C6 H6 118.9 . . ? C1 O1 Zn3 133.1(7) . . ? C1 O2 Zn1 139.9(10) . . ? C2 O4 Zn2 127.7(6) . . ? O6 N1 O6 116.0(15) . 11_665 ? O6 N1 O6 116.0(15) . 40 ? O6 N1 O6 116.0(15) 11_665 40 ? O6 N1 Zn3 78(2) . . ? O6 N1 Zn3 78(2) 11_665 . ? O6 N1 Zn3 78(2) 40 . ? O2 Zn1 O2 106.3(4) . 45_656 ? O2 Zn1 O2 106.3(4) . 30_665 ? O2 Zn1 O2 106.3(4) 45_656 30_665 ? O2 Zn1 O5 112.5(4) . . ? O2 Zn1 O5 112.5(4) 45_656 . ? O2 Zn1 O5 112.5(4) 30_665 . ? O3 Zn2 O4 100.71(19) . 5_577 ? O3 Zn2 O4 100.71(19) . . ? O4 Zn2 O4 158.6(4) 5_577 . ? O3 Zn2 O4 100.71(19) . 31_575 ? O4 Zn2 O4 88.02(7) 5_577 31_575 ? O4 Zn2 O4 88.02(7) . 31_575 ? O3 Zn2 O4 100.71(19) . 27_557 ? O4 Zn2 O4 88.02(7) 5_577 27_557 ? O4 Zn2 O4 88.02(7) . 27_557 ? O4 Zn2 O4 158.6(4) 31_575 27_557 ? O3 Zn2 Zn2 180.000(1) . 25_677 ? O4 Zn2 Zn2 79.29(19) 5_577 25_677 ? O4 Zn2 Zn2 79.29(19) . 25_677 ? O4 Zn2 Zn2 79.29(19) 31_575 25_677 ? O4 Zn2 Zn2 79.29(19) 27_557 25_677 ? O1 Zn3 O1 109.6(2) . 45_656 ? O1 Zn3 O1 109.6(2) . 30_665 ? O1 Zn3 O1 109.6(2) 45_656 30_665 ? O1 Zn3 N1 109.4(2) . . ? O1 Zn3 N1 109.4(2) 45_656 . ? O1 Zn3 N1 109.4(2) 30_665 . ? O1 Zn3 O6 89.4(7) . 40 ? O1 Zn3 O6 89.4(7) 45_656 40 ? O1 Zn3 O6 145.5(11) 30_665 40 ? N1 Zn3 O6 36.1(11) . 40 ? O1 Zn3 O6 145.5(11) . 11_665 ? O1 Zn3 O6 89.4(7) 45_656 11_665 ? O1 Zn3 O6 89.4(7) 30_665 11_665 ? N1 Zn3 O6 36.1(11) . 11_665 ? O6 Zn3 O6 61.4(18) 40 11_665 ? O1 Zn3 O6 89.4(7) . . ? O1 Zn3 O6 145.5(11) 45_656 . ? O1 Zn3 O6 89.4(7) 30_665 . ? N1 Zn3 O6 36.1(11) . . ? O6 Zn3 O6 61.4(18) 40 . ? O6 Zn3 O6 61.4(18) 11_665 . ? N1 O6 Zn3 66(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.830 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.101 _database_code_depnum_ccdc_archive 'CCDC 963916'