# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Qingxia Yao' 'Jie Su' 'Ocean Cheung' 'Niklas Hedin' 'Xiaodong Zou' _publ_contact_author_name 'Xiaodong Zou' _publ_contact_author_email xzou@mmk.su.se data_SUMOF-2 _database_code_depnum_ccdc_archive 'CCDC 853630' #TrackingRef '- SUMOF-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H12.25 O14 Zn4.13' _chemical_formula_weight 794.24 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' 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 trigonal _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 18.4010(10) _cell_length_b 18.4010(10) _cell_length_c 44.057(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12918.9(14) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5477 _cell_measurement_theta_min 4.1178 _cell_measurement_theta_max 32.3903 _exptl_crystal_description cubic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 2.314 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96827 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 16.5467 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29350 _diffrn_reflns_av_R_equivalents 0.1114 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3211 _reflns_number_gt 2450 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0784P)^2^+273.2506P] 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 3211 _refine_ls_number_parameters 175 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2308 _refine_ls_wR_factor_gt 0.2153 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.099 _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 0.38975(4) 0.61025(4) -0.00048(2) 0.0308(3) Uani 1 2 d S . . Zn2 Zn 0.3333 0.6667 0.06086(4) 0.0374(5) Uani 1 6 d S . . Zn3 Zn 0.60881(5) 0.39119(5) 0.19597(3) 0.0484(4) Uani 1 2 d S . . Zn4 Zn 0.6667 0.3333 0.13789(4) 0.0316(5) Uani 1 6 d S . . Zn5 Zn 0.3333 0.6667 0.1667 0.067(2) Uani 0.50 12 d SPD . . O1 O 0.3333 0.6667 0.0149(2) 0.028(2) Uani 1 6 d S . . O2 O 0.6667 0.3333 0.1813(3) 0.039(3) Uani 1 6 d S . . O3 O 0.6108(2) 0.3892(2) 0.11996(17) 0.054(2) Uani 1 2 d S . . O4 O 0.3171(4) 0.5140(4) -0.02657(14) 0.0579(16) Uani 1 1 d . . . O5 O 0.6802(6) 0.4874(5) 0.2188(2) 0.105(3) Uani 1 1 d . . . O6 O 0.5705(3) 0.4295(3) 0.16141(19) 0.070(3) Uani 1 2 d S . . O7 O 0.4358(3) 0.5642(3) 0.02825(18) 0.056(2) Uani 1 2 d S . . O8 O 0.4254(12) 0.6337(11) 0.0667(3) 0.113(10) Uani 0.50 1 d P . . C4 C 0.5768(4) 0.4232(4) 0.1334(2) 0.041(2) Uani 1 2 d SD . . C5 C 0.2414(4) 0.4829(7) -0.0336(2) 0.048(3) Uani 1 2 d S . . C6 C 0.2522(7) 0.3709(8) -0.0615(3) 0.099(5) Uani 1 1 d . . . H6 H 0.3087 0.3957 -0.0564 0.119 Uiso 1 1 calc R . . C7 C 0.7512(7) 0.6301(8) 0.2549(3) 0.103(5) Uani 1 1 d . . . H7 H 0.6948 0.6040 0.2495 0.124 Uiso 1 1 calc R . . C9 C 0.2034(4) 0.4067(9) -0.0524(3) 0.065(4) Uani 1 2 d S . . C10 C 0.4472(8) 0.5884(8) 0.0556(3) 0.043(5) Uani 0.50 1 d PD . . C13 C 0.7574(6) 0.5148(13) 0.2271(5) 0.115(8) Uani 1 2 d S . . C14 C 0.7973(5) 0.5946(11) 0.2461(4) 0.093(6) Uani 1 2 d S . . C15 C 0.4826(8) 0.5455(8) 0.07553(19) 0.055(6) Uani 0.50 1 d PGD . . C20 C 0.4956(9) 0.5669(7) 0.1061(2) 0.073(7) Uani 0.50 1 d PGD . . H20 H 0.4824 0.6059 0.1139 0.087 Uiso 0.50 1 calc PR . . C16 C 0.5284(10) 0.5300(10) 0.12509(18) 0.081(10) Uani 0.50 1 d PGD . . H16 H 0.5371 0.5443 0.1455 0.097 Uiso 0.50 1 calc PR . . C8 C 0.5481(15) 0.4717(15) 0.11350(17) 0.035(5) Uani 0.50 1 d PGD . . C3 C 0.535(2) 0.4503(19) 0.08293(19) 0.053(6) Uani 0.50 1 d PGD . . H3 H 0.5463 0.4103 0.0748 0.063 Uiso 0.50 1 calc PR . . C2 C 0.5023(16) 0.4945(15) 0.06389(14) 0.064(4) Uani 1 2 d SGD . . H2 H 0.4962 0.4846 0.0431 0.076 Uiso 0.50 1 calc PR . . O9 O 0.3333 0.6667 0.1100(8) 0.077(10) Uani 0.50 6 d SP . . H9 H 0.3091 0.6909 0.1162 0.092 Uiso 0.17 2 calc SPR . . O10 O 0.2674(7) 0.5348(14) 0.1477(8) 0.168(14) Uiso 0.50 2 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 Zn1 0.0317(5) 0.0317(5) 0.0292(6) -0.0003(2) 0.0003(2) 0.0159(5) Zn2 0.0427(8) 0.0427(8) 0.0268(10) 0.000 0.000 0.0213(4) Zn3 0.0559(7) 0.0559(7) 0.0364(7) 0.0026(3) -0.0026(3) 0.0302(7) Zn4 0.0337(7) 0.0337(7) 0.0275(10) 0.000 0.000 0.0168(3) Zn5 0.066(3) 0.066(3) 0.071(5) 0.000 0.000 0.0328(16) O1 0.033(4) 0.033(4) 0.018(5) 0.000 0.000 0.0163(18) O2 0.045(4) 0.045(4) 0.026(6) 0.000 0.000 0.022(2) O3 0.072(5) 0.072(5) 0.043(4) 0.0030(18) -0.0030(18) 0.055(5) O4 0.051(3) 0.056(4) 0.067(4) -0.035(3) -0.012(3) 0.027(3) O5 0.103(7) 0.081(6) 0.128(7) -0.059(5) -0.041(6) 0.043(5) O6 0.100(6) 0.100(6) 0.049(5) 0.005(2) -0.005(2) 0.078(7) O7 0.072(4) 0.072(4) 0.041(4) 0.0080(19) -0.0080(19) 0.049(5) O8 0.19(3) 0.14(2) 0.079(9) -0.067(11) -0.074(12) 0.14(2) C4 0.050(5) 0.050(5) 0.029(5) 0.003(2) -0.003(2) 0.029(6) C5 0.057(6) 0.043(7) 0.039(6) -0.007(5) -0.003(2) 0.021(3) C6 0.069(7) 0.095(9) 0.148(11) -0.082(8) -0.035(7) 0.052(7) C7 0.066(7) 0.086(9) 0.145(11) -0.076(8) -0.044(8) 0.028(7) C9 0.057(6) 0.065(9) 0.075(9) -0.038(7) -0.019(4) 0.033(4) C10 0.036(11) 0.041(12) 0.055(8) -0.013(7) -0.020(6) 0.021(11) C13 0.083(8) 0.119(16) 0.155(18) -0.110(15) -0.055(7) 0.059(8) C14 0.082(8) 0.079(11) 0.116(14) -0.070(11) -0.035(5) 0.040(6) C15 0.075(17) 0.071(16) 0.031(6) 0.002(8) 0.003(8) 0.045(16) C20 0.106(17) 0.094(16) 0.061(10) -0.026(10) -0.024(10) 0.081(15) C16 0.14(3) 0.12(2) 0.043(8) -0.025(10) -0.032(10) 0.11(2) C8 0.033(13) 0.030(13) 0.044(6) 0.010(7) 0.008(7) 0.016(12) C3 0.076(16) 0.072(18) 0.040(6) -0.020(13) -0.019(13) 0.059(13) C2 0.085(8) 0.085(8) 0.039(6) 0.003(3) -0.003(3) 0.056(9) O9 0.083(15) 0.083(15) 0.06(2) 0.000 0.000 0.042(8) _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 O1 1.921(4) . ? Zn1 O7 1.937(7) . ? Zn1 O4 1.969(5) . ? Zn1 O4 1.969(5) 22_665 ? Zn1 Zn1 3.114(2) 2_665 ? Zn1 Zn1 3.114(2) 3_565 ? Zn2 O1 2.025(10) . ? Zn2 O8 2.080(15) 2_665 ? Zn2 O8 2.080(15) 23 ? Zn2 O8 2.080(15) 24_565 ? Zn2 O8 2.080(15) 3_565 ? Zn2 O8 2.080(15) . ? Zn2 O8 2.080(15) 22_665 ? Zn2 O9 2.16(3) . ? Zn3 O5 1.883(7) . ? Zn3 O5 1.883(7) 22_665 ? Zn3 O6 1.953(8) . ? Zn3 O2 1.955(4) . ? Zn3 Zn4 3.154(2) . ? Zn4 O2 1.911(12) . ? Zn4 O3 1.948(8) 2_655 ? Zn4 O3 1.948(8) 3_665 ? Zn4 O3 1.948(8) . ? Zn4 Zn3 3.154(2) 3_665 ? Zn4 Zn3 3.154(2) 2_655 ? Zn5 O10 2.262(18) 27 ? Zn5 O10 2.262(18) 3_565 ? Zn5 O10 2.262(18) . ? Zn5 O10 2.262(19) 2_665 ? Zn5 O10 2.262(18) 25_565 ? Zn5 O10 2.262(18) 26_455 ? O1 Zn1 1.921(4) 3_565 ? O1 Zn1 1.921(4) 2_665 ? O2 Zn3 1.955(4) 3_665 ? O2 Zn3 1.955(4) 2_655 ? O3 C4 1.237(13) . ? O4 C5 1.251(7) . ? O5 C13 1.300(10) . ? O6 C4 1.249(13) . ? O7 C10 1.266(16) . ? O7 C10 1.266(16) 22_665 ? O8 C10 1.195(19) . ? C4 C8 1.522(12) 22_665 ? C4 C8 1.522(12) . ? C5 O4 1.251(7) 23 ? C5 C9 1.470(16) . ? C6 C7 1.398(14) 35_544 ? C6 C9 1.413(12) . ? C7 C14 1.361(14) . ? C7 C6 1.398(14) 29 ? C9 C6 1.413(12) 23 ? C10 C15 1.528(15) . ? C13 O5 1.300(10) 23_655 ? C13 C14 1.521(19) . ? C14 C7 1.361(14) 23_655 ? C15 C2 1.259(10) 22_665 ? C15 C20 1.3900 . ? C15 C2 1.2705 . ? C20 C16 1.3900 . ? C16 C8 1.3900 . ? C8 C3 1.3900 . ? C3 C2 1.4896 . ? 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 Zn1 O7 118.5(4) . . ? O1 Zn1 O4 112.6(2) . . ? O7 Zn1 O4 103.7(2) . . ? O1 Zn1 O4 112.6(2) . 22_665 ? O7 Zn1 O4 103.7(2) . 22_665 ? O4 Zn1 O4 104.2(4) . 22_665 ? O1 Zn1 Zn1 35.86(15) . 2_665 ? O7 Zn1 Zn1 130.96(19) . 2_665 ? O4 Zn1 Zn1 124.04(19) . 2_665 ? O4 Zn1 Zn1 76.74(17) 22_665 2_665 ? O1 Zn1 Zn1 35.86(15) . 3_565 ? O7 Zn1 Zn1 130.96(19) . 3_565 ? O4 Zn1 Zn1 76.74(17) . 3_565 ? O4 Zn1 Zn1 124.04(19) 22_665 3_565 ? Zn1 Zn1 Zn1 60.0 2_665 3_565 ? O1 Zn2 O8 97.1(4) . 2_665 ? O1 Zn2 O8 97.1(4) . 23 ? O8 Zn2 O8 88.6(10) 2_665 23 ? O1 Zn2 O8 97.1(4) . 24_565 ? O8 Zn2 O8 30.3(11) 2_665 24_565 ? O8 Zn2 O8 118.51(16) 23 24_565 ? O1 Zn2 O8 97.1(4) . 3_565 ? O8 Zn2 O8 118.51(16) 2_665 3_565 ? O8 Zn2 O8 30.3(11) 23 3_565 ? O8 Zn2 O8 147.4(11) 24_565 3_565 ? O1 Zn2 O8 97.1(4) . . ? O8 Zn2 O8 118.51(16) 2_665 . ? O8 Zn2 O8 147.4(11) 23 . ? O8 Zn2 O8 88.6(10) 24_565 . ? O8 Zn2 O8 118.51(16) 3_565 . ? O1 Zn2 O8 97.1(4) . 22_665 ? O8 Zn2 O8 147.4(11) 2_665 22_665 ? O8 Zn2 O8 118.51(16) 23 22_665 ? O8 Zn2 O8 118.51(17) 24_565 22_665 ? O8 Zn2 O8 88.6(10) 3_565 22_665 ? O8 Zn2 O8 30.3(11) . 22_665 ? O1 Zn2 O9 180.000(3) . . ? O8 Zn2 O9 82.9(4) 2_665 . ? O8 Zn2 O9 82.9(4) 23 . ? O8 Zn2 O9 82.9(4) 24_565 . ? O8 Zn2 O9 82.9(4) 3_565 . ? O8 Zn2 O9 82.9(4) . . ? O8 Zn2 O9 82.9(4) 22_665 . ? O5 Zn3 O5 109.8(6) . 22_665 ? O5 Zn3 O6 106.6(3) . . ? O5 Zn3 O6 106.6(3) 22_665 . ? O5 Zn3 O2 112.1(3) . . ? O5 Zn3 O2 112.1(3) 22_665 . ? O6 Zn3 O2 109.4(4) . . ? O5 Zn3 Zn4 123.8(3) . . ? O5 Zn3 Zn4 123.8(3) 22_665 . ? O6 Zn3 Zn4 74.5(3) . . ? O2 Zn3 Zn4 34.9(3) . . ? O2 Zn4 O3 113.9(2) . 2_655 ? O2 Zn4 O3 113.9(2) . 3_665 ? O3 Zn4 O3 104.7(3) 2_655 3_665 ? O2 Zn4 O3 113.9(2) . . ? O3 Zn4 O3 104.7(3) 2_655 . ? O3 Zn4 O3 104.7(3) 3_665 . ? O2 Zn4 Zn3 35.78(3) . 3_665 ? O3 Zn4 Zn3 126.61(18) 2_655 3_665 ? O3 Zn4 Zn3 78.2(2) 3_665 3_665 ? O3 Zn4 Zn3 126.60(18) . 3_665 ? O2 Zn4 Zn3 35.78(3) . 2_655 ? O3 Zn4 Zn3 78.2(2) 2_655 2_655 ? O3 Zn4 Zn3 126.61(18) 3_665 2_655 ? O3 Zn4 Zn3 126.60(18) . 2_655 ? Zn3 Zn4 Zn3 60.84(5) 3_665 2_655 ? O2 Zn4 Zn3 35.78(3) . . ? O3 Zn4 Zn3 126.61(18) 2_655 . ? O3 Zn4 Zn3 126.61(18) 3_665 . ? O3 Zn4 Zn3 78.2(2) . . ? Zn3 Zn4 Zn3 60.84(5) 3_665 . ? Zn3 Zn4 Zn3 60.84(5) 2_655 . ? O10 Zn5 O10 179.997(3) 27 3_565 ? O10 Zn5 O10 72.9(11) 27 . ? O10 Zn5 O10 107.1(11) 3_565 . ? O10 Zn5 O10 72.9(11) 27 2_665 ? O10 Zn5 O10 107.1(11) 3_565 2_665 ? O10 Zn5 O10 107.1(11) . 2_665 ? O10 Zn5 O10 107.1(11) 27 25_565 ? O10 Zn5 O10 72.9(11) 3_565 25_565 ? O10 Zn5 O10 180.0(8) . 25_565 ? O10 Zn5 O10 72.9(11) 2_665 25_565 ? O10 Zn5 O10 107.1(11) 27 26_455 ? O10 Zn5 O10 72.9(11) 3_565 26_455 ? O10 Zn5 O10 72.9(11) . 26_455 ? O10 Zn5 O10 179.997(2) 2_665 26_455 ? O10 Zn5 O10 107.1(11) 25_565 26_455 ? Zn1 O1 Zn1 108.3(3) 3_565 2_665 ? Zn1 O1 Zn1 108.3(3) 3_565 . ? Zn1 O1 Zn1 108.3(3) 2_665 . ? Zn1 O1 Zn2 110.6(3) 3_565 . ? Zn1 O1 Zn2 110.6(3) 2_665 . ? Zn1 O1 Zn2 110.6(3) . . ? Zn4 O2 Zn3 109.4(3) . 3_665 ? Zn4 O2 Zn3 109.4(3) . 2_655 ? Zn3 O2 Zn3 109.6(3) 3_665 2_655 ? Zn4 O2 Zn3 109.4(3) . . ? Zn3 O2 Zn3 109.6(3) 3_665 . ? Zn3 O2 Zn3 109.6(3) 2_655 . ? C4 O3 Zn4 127.4(7) . . ? C5 O4 Zn1 131.0(6) . . ? C13 O5 Zn3 128.9(8) . . ? C4 O6 Zn3 132.0(8) . . ? C10 O7 C10 30.0(12) . 22_665 ? C10 O7 Zn1 120.1(8) . . ? C10 O7 Zn1 120.1(8) 22_665 . ? C10 O8 Zn2 139.4(12) . . ? O3 C4 O6 127.9(10) . . ? O3 C4 C8 115.6(9) . 22_665 ? O6 C4 C8 116.1(10) . 22_665 ? O3 C4 C8 115.6(8) . . ? O6 C4 C8 116.1(10) . . ? C8 C4 C8 14(2) 22_665 . ? O4 C5 O4 124.2(10) 23 . ? O4 C5 C9 117.8(5) 23 . ? O4 C5 C9 117.8(5) . . ? C7 C6 C9 117.4(10) 35_544 . ? C14 C7 C6 122.4(11) . 29 ? C6 C9 C6 120.8(12) 23 . ? C6 C9 C5 119.6(6) 23 . ? C6 C9 C5 119.6(6) . . ? O8 C10 O7 125.3(14) . . ? O8 C10 C15 120.4(14) . . ? O7 C10 C15 113.8(12) . . ? O5 C13 O5 128.0(13) 23_655 . ? O5 C13 C14 115.8(7) 23_655 . ? O5 C13 C14 115.8(7) . . ? C7 C14 C7 119.4(13) . 23_655 ? C7 C14 C13 120.3(6) . . ? C7 C14 C13 120.3(6) 23_655 . ? C2 C15 C20 121.5(4) 22_665 . ? C2 C15 C2 3(3) 22_665 . ? C20 C15 C2 121.9 . . ? C2 C15 C10 120.4(9) 22_665 . ? C20 C15 C10 117.9(8) . . ? C2 C15 C10 120.2(8) . . ? C16 C20 C15 120.0 . . ? C20 C16 C8 120.0 . . ? C16 C8 C3 120.0 . . ? C16 C8 C4 122.8(7) . . ? C3 C8 C4 117.0(7) . . ? C2 C3 C8 116.8 . . ? C3 C2 C15 121.2 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.362 _refine_diff_density_min -2.194 _refine_diff_density_rms 0.133 # 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 -0.049 -0.034 0.000 5352 585 ' ' _platon_squeeze_details ; ; # Attachment '- SUMOF-3.cif' data_SUMOF-3 _database_code_depnum_ccdc_archive 'CCDC 853631' #TrackingRef '- SUMOF-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H50 N O31.70 Zn8' _chemical_formula_weight 1995.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.6086(8) _cell_length_b 20.2422(7) _cell_length_c 20.8135(7) _cell_angle_alpha 70.421(3) _cell_angle_beta 68.955(3) _cell_angle_gamma 68.031(4) _cell_volume 6600.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11718 _cell_measurement_theta_min 4.1312 _cell_measurement_theta_max 32.2935 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2001 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92284 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 16.5467 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45520 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0900 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 26.37 _reflns_number_total 26227 _reflns_number_gt 15115 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0722P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26227 _refine_ls_number_parameters 1015 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1616 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Zn1 Zn 0.63553(3) 0.78775(3) 0.47691(2) 0.02789(13) Uani 1 1 d . . . Zn2 Zn 0.61532(3) 0.64152(3) 0.47331(3) 0.02931(13) Uani 1 1 d . . . Zn3 Zn 0.78068(3) 0.64767(3) 0.47471(2) 0.02844(13) Uani 1 1 d . . . Zn4 Zn 0.63571(3) 0.65894(3) 0.61730(3) 0.03334(14) Uani 1 1 d . . . Zn5 Zn 0.19902(3) 0.20825(3) 0.90605(2) 0.02949(13) Uani 1 1 d . . . Zn6 Zn 0.19587(3) 1.07844(3) 1.04017(3) 0.03294(14) Uani 1 1 d . . . Zn7 Zn 1.05113(3) 1.22246(3) 0.04027(2) 0.02935(13) Uani 1 1 d . . . Zn8 Zn 0.22546(3) 0.22332(3) 1.04454(3) 0.03545(14) Uani 1 1 d . . . O1 O 0.66564(17) 0.68268(15) 0.51020(14) 0.0253(6) Uani 1 1 d . . . O2 O 1.16572(18) 1.18387(15) 0.00863(14) 0.0289(7) Uani 1 1 d . . . O3 O 0.9938(2) 1.1486(2) 0.09644(19) 0.0564(10) Uani 1 1 d . . . O4 O 0.8436(2) 0.5753(2) 0.53720(18) 0.0552(10) Uani 1 1 d . . . O5 O 0.5697(2) 0.85211(18) 0.54086(17) 0.0507(10) Uani 1 1 d . . . O6 O 0.8086(2) 0.5956(2) 0.4001(2) 0.0573(11) Uani 1 1 d . . . O7 O 0.7258(2) 0.82588(18) 0.41564(18) 0.0489(9) Uani 1 1 d . . . O8 O 1.0973(3) 1.0473(2) 0.0929(2) 0.0627(11) Uani 1 1 d . . . O9 O 0.6922(2) 0.5859(2) 0.4027(2) 0.0588(11) Uani 1 1 d . . . O10 O 0.5609(3) 0.5716(2) 0.54023(18) 0.0568(11) Uani 1 1 d . . . O11 O 1.0142(2) 1.2888(2) 0.1020(2) 0.0586(11) Uani 1 1 d . . . O12 O 0.2679(3) 0.2710(2) 0.8597(2) 0.0646(12) Uani 1 1 d . . . O13 O 0.5371(2) 0.71676(19) 0.42335(19) 0.0516(10) Uani 1 1 d . . . O14 O 0.2470(3) 1.0287(2) 0.96243(19) 0.0676(12) Uani 1 1 d . . . O15 O 0.9999(2) 0.2781(2) 0.96268(17) 0.0574(11) Uani 1 1 d . . . O16 O 0.2560(3) 1.0319(2) 0.1088(2) 0.0781(14) Uani 1 1 d . . . O17 O 0.5534(2) 0.6041(2) 0.63433(18) 0.0542(10) Uani 1 1 d . . . O18 O 1.1044(2) 0.2590(2) 0.86834(18) 0.0598(11) Uani 1 1 d . . . O19 O 0.2501(2) 1.1223(2) 0.86604(18) 0.0540(10) Uani 1 1 d . . . O20 O 0.5678(3) 0.8174(2) 0.4114(2) 0.0603(11) Uani 1 1 d . . . O21 O 0.8325(2) 0.72570(19) 0.42078(18) 0.0501(9) Uani 1 1 d . . . O22 O 0.1330(2) 0.2932(2) 1.10112(19) 0.0517(10) Uani 1 1 d . . . O23 O 0.7336(2) 0.5603(2) 0.62413(18) 0.0551(10) Uani 1 1 d . . . O24 O 0.5445(2) 0.7582(2) 0.62950(19) 0.0622(12) Uani 1 1 d . . . O25 O 0.6120(3) 0.6353(3) 0.7276(2) 0.0730(13) Uani 1 1 d D . . H25A H 0.626(3) 0.5831(12) 0.748(3) 0.088 Uiso 1 1 d D . . H25B H 0.5565(15) 0.652(3) 0.751(3) 0.088 Uiso 1 1 d D . . O26 O 0.2434(3) 0.3097(2) 0.9548(2) 0.0877(16) Uani 1 1 d . . . O27 O 0.23759(18) 1.13670(16) 0.13382(14) 0.0904(17) Uani 1 1 d . . . O28 O 0.72777(18) 0.71491(16) 0.60895(14) 0.1115(19) Uani 1 1 d RD . . H28A H 0.7444 0.7304 0.6363 0.134 Uiso 1 1 d RD . . H28B H 0.7417 0.6656 0.6179 0.134 Uiso 1 1 d RD . . O29 O 0.33452(18) 0.15516(16) 0.98327(14) 0.1080(18) Uani 1 1 d RD . . H29A H 0.3889 0.1465 0.9730 0.130 Uiso 1 1 d RD . . H29B H 0.3216 0.1149 0.9874 0.130 Uiso 1 1 d RD . . O30 O 0.3054(3) 0.2519(3) 1.0751(3) 0.1008(17) Uani 1 1 d . . . C1 C 0.5396(3) 0.5674(3) 0.6053(3) 0.0399(12) Uani 1 1 d . . . C2 C 0.0599(4) 0.3107(3) 1.1193(3) 0.0445(13) Uani 1 1 d . . . C3 C 1.0249(3) 1.0809(3) 0.1144(3) 0.0462(13) Uani 1 1 d . . . C4 C 0.7997(3) 0.7924(3) 0.3974(2) 0.0382(12) Uani 1 1 d . . . C5 C 0.8219(3) 0.9097(3) 0.3171(3) 0.0556(16) Uani 1 1 d . . . H5 H 0.7667 0.9311 0.3313 0.067 Uiso 1 1 calc R . . C6 C 0.4908(3) 0.4599(3) 0.6230(3) 0.0500(14) Uani 1 1 d . . . H6 H 0.5159 0.4601 0.5754 0.060 Uiso 1 1 calc R . . C7 C 0.4940(3) 0.5123(3) 0.6522(3) 0.0454(13) Uani 1 1 d . . . C8 C 1.0032(3) 0.9649(3) 0.1972(3) 0.0605(17) Uani 1 1 d . . . H8 H 1.0586 0.9441 0.1841 0.073 Uiso 1 1 calc R . . C9 C 0.3655(3) 0.3597(3) 0.7784(3) 0.0509(14) Uani 1 1 d . . . H9 H 0.3635 0.3253 0.7591 0.061 Uiso 1 1 calc R . . C10 C 0.4571(3) 0.5122(3) 0.7217(3) 0.0521(15) Uani 1 1 d . . . H10 H 0.4606 0.5459 0.7408 0.063 Uiso 1 1 calc R . . C11 C 1.0151(3) 0.3631(3) 0.1680(3) 0.0463(13) Uani 1 1 d . . . C12 C 0.8705(3) 0.9532(3) 0.2662(3) 0.0525(15) Uani 1 1 d . . . C13 C 0.4107(3) 0.4097(3) 0.7358(3) 0.0489(14) Uani 1 1 d . . . C14 C 0.8531(3) 0.8370(3) 0.3463(3) 0.0494(14) Uani 1 1 d . . . C15 C 0.4513(3) 0.4092(3) 0.6639(3) 0.0478(14) Uani 1 1 d . . . H15 H 0.4509 0.3741 0.6446 0.057 Uiso 1 1 calc R . . C16 C 0.9544(3) 0.9211(3) 0.2476(3) 0.0561(16) Uani 1 1 d . . . C17 C 1.0569(4) 0.3957(4) 0.1854(4) 0.075(2) Uani 1 1 d . . . H17 H 1.1126 0.3841 0.1678 0.090 Uiso 1 1 calc R . . C18 C 0.9711(3) 1.0368(3) 0.1673(3) 0.0495(14) Uani 1 1 d . . . C19 C 0.9585(3) 0.3909(3) 0.7323(2) 0.0416(12) Uani 1 1 d . . . C20 C 1.0079(3) 0.3445(3) 0.7777(3) 0.0442(13) Uani 1 1 d . . . H20 H 1.0616 0.3215 0.7582 0.053 Uiso 1 1 calc R . . C21 C 0.8917(3) 0.5073(3) 0.3036(3) 0.0565(16) Uani 1 1 d . . . H21 H 0.9201 0.5284 0.3157 0.068 Uiso 1 1 calc R . . C22 C 0.4111(3) 1.0028(3) 0.6591(3) 0.0472(14) Uani 1 1 d . . . H22 H 0.3969 1.0525 0.6380 0.057 Uiso 1 1 calc R . . C23 C 0.4586(3) 0.9531(3) 0.6183(3) 0.0513(15) Uani 1 1 d . . . H23 H 0.4758 0.9699 0.5695 0.062 Uiso 1 1 calc R . . C24 C 0.4818(3) 0.8780(3) 0.6480(3) 0.0432(13) Uani 1 1 d . . . C25 C 0.3839(3) 0.9786(3) 0.7329(2) 0.0405(12) Uani 1 1 d . . . C26 C 0.8599(3) 0.4912(3) 0.6453(3) 0.0439(13) Uani 1 1 d . . . C27 C 0.9332(3) 0.4607(3) 0.2568(3) 0.0534(15) Uani 1 1 d . . . C28 C 0.9400(3) 0.4571(3) 0.6154(3) 0.0517(15) Uani 1 1 d . . . H28 H 0.9612 0.4686 0.5666 0.062 Uiso 1 1 calc R . . C29 C 0.5359(3) 0.8251(3) 0.6025(3) 0.0464(13) Uani 1 1 d . . . C30 C 0.8884(4) 1.0675(3) 0.1872(4) 0.076(2) Uani 1 1 d . . . H30 H 0.8664 1.1163 0.1668 0.091 Uiso 1 1 calc R . . C31 C 0.9884(3) 0.4064(3) 0.6575(3) 0.0496(14) Uani 1 1 d . . . H31 H 1.0410 0.3822 0.6367 0.060 Uiso 1 1 calc R . . C32 C 0.3365(4) 0.9262(3) 0.8805(3) 0.075(2) Uani 1 1 d . . . H32 H 0.3217 0.9096 0.9294 0.090 Uiso 1 1 calc R . . C33 C 0.3247(4) 0.3614(3) 0.8477(3) 0.0685(19) Uani 1 1 d . . . C34 C 0.3795(5) 0.8780(3) 0.8400(3) 0.081(2) Uani 1 1 d . . . H34 H 0.3920 0.8282 0.8610 0.097 Uiso 1 1 calc R . . C35 C 0.7674(3) 0.5717(3) 0.3823(3) 0.0426(13) Uani 1 1 d . . . C36 C 0.9780(3) 0.3328(3) 0.8497(3) 0.0450(13) Uani 1 1 d . . . C37 C 0.2763(4) 0.3094(3) 0.8921(3) 0.0641(18) Uani 1 1 d . . . C38 C 0.8070(4) 0.5465(3) 0.5998(3) 0.0513(14) Uani 1 1 d . . . C39 C 0.3376(3) 1.0269(3) 0.7777(3) 0.0448(13) Uani 1 1 d . . . H39 H 0.3229 1.0770 0.7582 0.054 Uiso 1 1 calc R . . C40 C 0.3136(3) 1.0015(3) 0.8499(3) 0.0484(14) Uani 1 1 d . . . C41 C 0.8381(4) 1.0280(3) 0.2358(4) 0.081(2) Uani 1 1 d . . . H41 H 0.7830 1.0502 0.2488 0.097 Uiso 1 1 calc R . . C42 C 0.8099(3) 0.5224(3) 0.3320(3) 0.0472(13) Uani 1 1 d . . . C43 C 0.4067(4) 0.9022(3) 0.7640(3) 0.0562(16) Uani 1 1 d . . . C44 C 0.2655(3) 1.0553(3) 0.8964(3) 0.0486(14) Uani 1 1 d . . . C45 C 0.4559(4) 0.8530(3) 0.7196(3) 0.0533(15) Uani 1 1 d . . . H45 H 0.4708 0.8030 0.7395 0.064 Uiso 1 1 calc R . . C46 C 1.0325(3) 0.2866(3) 0.8968(3) 0.0447(13) Uani 1 1 d . . . C47 C 0.8962(3) 0.3684(4) 0.8788(3) 0.069(2) Uani 1 1 d . . . H47 H 0.8759 0.3606 0.9277 0.083 Uiso 1 1 calc R . . C48 C 0.9325(3) 0.3795(3) 0.1947(3) 0.0575(16) Uani 1 1 d . . . H48 H 0.9045 0.3578 0.1827 0.069 Uiso 1 1 calc R . . C49 C 0.8478(4) 0.4122(4) 0.8382(3) 0.070(2) Uani 1 1 d . . . H49 H 0.7944 0.4342 0.8592 0.084 Uiso 1 1 calc R . . C50 C 0.8903(3) 0.4276(3) 0.2391(3) 0.0535(15) Uani 1 1 d . . . C51 C 0.8765(3) 0.4265(3) 0.7621(3) 0.0467(14) Uani 1 1 d . . . C52 C 0.4138(4) 0.4620(3) 0.7650(3) 0.0567(16) Uani 1 1 d . . . C53 C 0.8279(3) 0.4755(3) 0.7175(3) 0.0517(15) Uani 1 1 d . . . H53 H 0.7739 0.4973 0.7369 0.062 Uiso 1 1 calc R . . C54 C 0.8067(4) 0.4448(4) 0.2682(4) 0.083(2) Uani 1 1 d . . . H54 H 0.7774 0.4241 0.2566 0.100 Uiso 1 1 calc R . . C55 C 1.0184(4) 0.4445(5) 0.2276(4) 0.096(3) Uani 1 1 d . . . H55 H 1.0474 0.4671 0.2373 0.115 Uiso 1 1 calc R . . C56 C 0.7671(3) 0.4911(4) 0.3130(4) 0.071(2) Uani 1 1 d . . . H56 H 0.7115 0.5019 0.3310 0.085 Uiso 1 1 calc R . . C57 C 0.9851(4) 0.8485(4) 0.2786(4) 0.094(3) Uani 1 1 d . . . H57 H 1.0405 0.8274 0.2667 0.113 Uiso 1 1 calc R . . C58 C 0.3286(5) 0.4149(4) 0.8766(3) 0.090(3) Uani 1 1 d . . . H58 H 0.3005 0.4173 0.9233 0.108 Uiso 1 1 calc R . . C59 C 0.4083(6) 1.0204(4) 0.2552(4) 0.108(3) Uani 1 1 d . . . H59 H 0.4404 1.0417 0.2624 0.129 Uiso 1 1 calc R . . C60 C 0.4107(4) 0.9467(3) 0.2873(3) 0.0673(19) Uani 1 1 d . . . C61 C 0.5303(3) 0.7848(3) 0.4008(3) 0.0458(13) Uani 1 1 d . . . C62 C 0.9375(4) 0.8065(3) 0.3260(4) 0.085(2) Uani 1 1 d . . . H62 H 0.9607 0.7575 0.3451 0.102 Uiso 1 1 calc R . . C63 C 0.4722(4) 0.8285(3) 0.3570(3) 0.0548(15) Uani 1 1 d . . . C64 C 0.2618(4) 1.0709(4) 0.1431(3) 0.0662(18) Uani 1 1 d . . . C65 C 0.4626(4) 0.9020(3) 0.3309(3) 0.070(2) Uani 1 1 d . . . H65 H 0.4913 0.9235 0.3423 0.084 Uiso 1 1 calc R . . C66 C 0.3126(4) 1.0269(4) 0.1952(3) 0.0679(18) Uani 1 1 d . . . C67 C 0.3731(5) 0.4622(4) 0.8365(3) 0.089(3) Uani 1 1 d . . . H67 H 0.3765 0.4951 0.8567 0.107 Uiso 1 1 calc R . . C68 C 0.4263(4) 0.7963(3) 0.3423(4) 0.075(2) Uani 1 1 d . . . H68 H 0.4314 0.7466 0.3604 0.090 Uiso 1 1 calc R . . C69 C 0.3186(4) 0.9555(4) 0.2247(3) 0.0701(19) Uani 1 1 d . . . H69 H 0.2900 0.9334 0.2137 0.084 Uiso 1 1 calc R . . C70 C 0.3666(4) 0.9131(3) 0.2716(3) 0.0682(18) Uani 1 1 d . . . C71 C 0.3557(6) 1.0610(4) 0.2118(4) 0.105(3) Uani 1 1 d . . . H71 H 0.3491 1.1110 0.1938 0.126 Uiso 1 1 calc R . . C72 C 0.3738(5) 0.8385(4) 0.3009(4) 0.093(3) Uani 1 1 d . . . H72 H 0.3428 0.8169 0.2925 0.112 Uiso 1 1 calc R . . C81 C 0.2909(7) 0.3160(6) 1.0763(5) 0.124(3) Uiso 1 1 d . . . H81 H 0.2462 0.3502 1.0622 0.149 Uiso 1 1 calc R . . N1 N 0.3388(9) 0.3402(8) 1.0980(6) 0.202(5) Uiso 1 1 d . . . C82 C 0.3229(13) 0.4129(12) 1.1046(11) 0.321(11) Uiso 1 1 d . . . H82A H 0.3675 0.4315 1.0749 0.385 Uiso 1 1 calc R . . H82B H 0.3155 0.4119 1.1529 0.385 Uiso 1 1 calc R . . H82C H 0.2751 0.4439 1.0903 0.385 Uiso 1 1 calc R . . C83 C 0.4128(12) 0.2882(11) 1.1098(10) 0.282(9) Uiso 1 1 d . . . H83A H 0.4017 0.2476 1.1479 0.338 Uiso 1 1 calc R . . H83B H 0.4416 0.3111 1.1217 0.338 Uiso 1 1 calc R . . H83C H 0.4449 0.2710 1.0675 0.338 Uiso 1 1 calc R . . OW1 O 0.4545(5) 0.6708(4) 0.8152(4) 0.143(3) Uiso 0.85 1 d P . . OW2 O 0.6242(5) 0.4870(4) 0.8054(4) 0.145(3) Uiso 0.85 1 d P . . 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 0.0292(3) 0.0245(3) 0.0251(3) -0.0054(2) -0.0017(2) -0.0081(2) Zn2 0.0303(3) 0.0279(3) 0.0269(3) -0.0075(2) -0.0030(2) -0.0087(2) Zn3 0.0276(3) 0.0266(3) 0.0247(3) -0.0031(2) -0.0027(2) -0.0076(2) Zn4 0.0395(3) 0.0347(3) 0.0237(3) -0.0054(2) -0.0026(2) -0.0152(3) Zn5 0.0331(3) 0.0271(3) 0.0231(3) -0.0049(2) -0.0016(2) -0.0096(2) Zn6 0.0390(3) 0.0307(3) 0.0246(3) -0.0060(2) -0.0015(2) -0.0122(3) Zn7 0.0311(3) 0.0288(3) 0.0224(3) -0.0044(2) -0.0020(2) -0.0087(2) Zn8 0.0388(3) 0.0339(3) 0.0323(3) -0.0110(2) -0.0056(3) -0.0099(3) O1 0.0253(16) 0.0247(16) 0.0221(14) -0.0050(12) -0.0018(12) -0.0077(13) O2 0.0333(17) 0.0235(16) 0.0235(15) -0.0021(12) -0.0040(13) -0.0077(14) O3 0.050(2) 0.039(2) 0.063(2) 0.0079(18) -0.0033(19) -0.0247(19) O4 0.044(2) 0.059(2) 0.039(2) 0.0097(18) -0.0139(17) -0.006(2) O5 0.064(2) 0.039(2) 0.0344(19) -0.0191(16) 0.0087(18) -0.0106(19) O6 0.042(2) 0.077(3) 0.060(2) -0.049(2) 0.0041(19) -0.013(2) O7 0.038(2) 0.037(2) 0.050(2) 0.0013(16) 0.0069(17) -0.0157(18) O8 0.058(3) 0.044(2) 0.074(3) 0.001(2) -0.001(2) -0.030(2) O9 0.044(2) 0.075(3) 0.070(3) -0.050(2) -0.003(2) -0.013(2) O10 0.083(3) 0.060(3) 0.035(2) -0.0005(17) -0.008(2) -0.046(2) O11 0.047(2) 0.070(3) 0.065(3) -0.046(2) 0.002(2) -0.012(2) O12 0.082(3) 0.062(3) 0.051(2) -0.009(2) 0.007(2) -0.051(2) O13 0.064(3) 0.037(2) 0.061(2) -0.0074(18) -0.035(2) -0.0080(19) O14 0.096(3) 0.049(2) 0.041(2) -0.0193(18) 0.013(2) -0.025(2) O15 0.047(2) 0.074(3) 0.0290(19) -0.0011(18) -0.0099(17) -0.003(2) O16 0.099(4) 0.068(3) 0.069(3) 0.004(2) -0.046(3) -0.021(3) O17 0.063(3) 0.062(3) 0.044(2) -0.0176(18) 0.0076(19) -0.041(2) O18 0.046(2) 0.078(3) 0.034(2) -0.0033(19) -0.0142(18) 0.000(2) O19 0.073(3) 0.041(2) 0.038(2) -0.0205(17) -0.0050(19) -0.005(2) O20 0.085(3) 0.041(2) 0.071(3) 0.0049(19) -0.056(2) -0.018(2) O21 0.046(2) 0.035(2) 0.053(2) -0.0027(17) 0.0049(18) -0.0187(18) O22 0.042(2) 0.056(2) 0.052(2) -0.0312(19) 0.0049(18) -0.0092(19) O23 0.044(2) 0.059(3) 0.048(2) 0.0179(18) -0.0187(19) -0.018(2) O24 0.077(3) 0.042(2) 0.046(2) -0.0219(18) 0.023(2) -0.020(2) O25 0.091(3) 0.088(3) 0.039(2) -0.008(2) -0.013(2) -0.035(3) O26 0.122(4) 0.074(3) 0.059(3) -0.028(2) 0.035(3) -0.064(3) O27 0.122(4) 0.070(3) 0.059(3) -0.020(2) -0.047(3) 0.021(3) O28 0.083(4) 0.090(4) 0.145(5) -0.018(3) 0.005(3) -0.049(3) O29 0.121(4) 0.091(4) 0.096(4) -0.060(3) 0.009(3) -0.014(3) O30 0.096(4) 0.095(4) 0.134(5) -0.054(3) -0.041(4) -0.018(3) C1 0.038(3) 0.035(3) 0.045(3) -0.004(2) -0.007(2) -0.018(2) C2 0.053(4) 0.036(3) 0.039(3) -0.017(2) -0.005(3) -0.007(3) C3 0.046(3) 0.049(4) 0.040(3) -0.001(3) -0.002(3) -0.028(3) C4 0.037(3) 0.036(3) 0.039(3) -0.004(2) 0.000(2) -0.021(2) C5 0.033(3) 0.036(3) 0.071(4) 0.002(3) 0.009(3) -0.015(3) C6 0.055(4) 0.061(4) 0.037(3) -0.008(3) -0.001(3) -0.034(3) C7 0.048(3) 0.046(3) 0.042(3) -0.006(2) -0.004(3) -0.025(3) C8 0.039(3) 0.051(4) 0.071(4) 0.006(3) -0.002(3) -0.022(3) C9 0.066(4) 0.052(3) 0.040(3) -0.011(3) 0.002(3) -0.038(3) C10 0.066(4) 0.055(4) 0.043(3) -0.014(3) 0.002(3) -0.040(3) C11 0.047(3) 0.047(3) 0.044(3) -0.024(3) 0.004(3) -0.016(3) C12 0.042(3) 0.037(3) 0.064(4) 0.003(3) -0.002(3) -0.021(3) C13 0.054(4) 0.053(3) 0.041(3) -0.004(3) -0.004(3) -0.031(3) C14 0.035(3) 0.041(3) 0.054(3) 0.002(3) 0.001(3) -0.015(3) C15 0.062(4) 0.057(4) 0.039(3) -0.011(3) -0.006(3) -0.041(3) C16 0.038(3) 0.038(3) 0.072(4) 0.007(3) -0.003(3) -0.018(3) C17 0.042(4) 0.102(6) 0.100(5) -0.069(5) 0.005(3) -0.023(4) C18 0.041(3) 0.041(3) 0.054(3) 0.002(3) -0.002(3) -0.020(3) C19 0.038(3) 0.044(3) 0.033(3) -0.005(2) -0.010(2) -0.004(2) C20 0.041(3) 0.046(3) 0.039(3) -0.007(2) -0.015(2) -0.003(3) C21 0.043(3) 0.059(4) 0.069(4) -0.044(3) 0.005(3) -0.010(3) C22 0.056(3) 0.031(3) 0.042(3) -0.011(2) -0.007(3) -0.003(3) C23 0.064(4) 0.046(3) 0.031(3) -0.012(2) 0.001(3) -0.013(3) C24 0.049(3) 0.030(3) 0.039(3) -0.011(2) 0.002(2) -0.009(2) C25 0.046(3) 0.032(3) 0.036(3) -0.016(2) 0.000(2) -0.006(2) C26 0.034(3) 0.050(3) 0.039(3) 0.006(2) -0.016(2) -0.011(3) C27 0.048(3) 0.055(4) 0.060(4) -0.042(3) 0.005(3) -0.010(3) C28 0.045(3) 0.059(4) 0.033(3) -0.001(2) -0.012(3) -0.004(3) C29 0.050(3) 0.043(3) 0.039(3) -0.021(2) 0.006(3) -0.012(3) C30 0.054(4) 0.040(4) 0.099(5) 0.019(3) -0.007(4) -0.019(3) C31 0.035(3) 0.060(4) 0.038(3) -0.008(3) -0.008(2) -0.002(3) C32 0.124(6) 0.038(3) 0.030(3) -0.015(2) 0.020(3) -0.019(4) C33 0.085(5) 0.069(4) 0.054(4) -0.016(3) 0.017(3) -0.057(4) C34 0.132(6) 0.035(3) 0.033(3) -0.006(3) 0.015(4) -0.016(4) C35 0.041(3) 0.043(3) 0.034(3) -0.017(2) -0.001(2) -0.004(3) C36 0.036(3) 0.054(3) 0.036(3) -0.002(2) -0.014(2) -0.007(3) C37 0.079(5) 0.058(4) 0.052(4) -0.018(3) 0.018(3) -0.045(4) C38 0.054(4) 0.044(3) 0.045(3) -0.001(3) -0.020(3) -0.005(3) C39 0.051(3) 0.031(3) 0.043(3) -0.014(2) -0.005(3) -0.004(3) C40 0.063(4) 0.037(3) 0.036(3) -0.019(2) 0.005(3) -0.012(3) C41 0.040(3) 0.041(4) 0.116(6) 0.023(4) -0.002(4) -0.016(3) C42 0.041(3) 0.054(3) 0.050(3) -0.028(3) -0.007(3) -0.009(3) C43 0.078(4) 0.029(3) 0.035(3) -0.013(2) 0.008(3) -0.003(3) C44 0.058(4) 0.044(3) 0.039(3) -0.024(3) 0.009(3) -0.017(3) C45 0.074(4) 0.026(3) 0.042(3) -0.016(2) 0.006(3) -0.008(3) C46 0.052(3) 0.036(3) 0.039(3) 0.000(2) -0.017(3) -0.008(3) C47 0.048(4) 0.094(5) 0.028(3) -0.004(3) -0.003(3) 0.004(3) C48 0.041(3) 0.066(4) 0.073(4) -0.044(3) -0.008(3) -0.006(3) C49 0.045(3) 0.082(5) 0.038(3) 0.003(3) -0.007(3) 0.010(3) C50 0.037(3) 0.064(4) 0.057(4) -0.037(3) 0.001(3) -0.005(3) C51 0.037(3) 0.047(3) 0.040(3) 0.000(2) -0.012(2) -0.002(3) C52 0.081(4) 0.061(4) 0.037(3) -0.018(3) 0.009(3) -0.048(3) C53 0.041(3) 0.050(3) 0.042(3) -0.002(3) -0.011(3) 0.003(3) C54 0.048(4) 0.114(6) 0.121(6) -0.091(5) -0.005(4) -0.019(4) C55 0.050(4) 0.152(8) 0.115(6) -0.108(6) 0.012(4) -0.026(5) C56 0.027(3) 0.094(5) 0.100(5) -0.067(4) -0.003(3) 0.000(3) C57 0.039(4) 0.052(4) 0.133(6) 0.025(4) 0.008(4) -0.021(3) C58 0.139(7) 0.102(6) 0.048(4) -0.034(4) 0.027(4) -0.088(6) C59 0.184(9) 0.045(4) 0.128(7) -0.001(4) -0.123(7) -0.007(5) C60 0.086(5) 0.044(4) 0.073(4) -0.006(3) -0.052(4) 0.003(3) C61 0.050(3) 0.036(3) 0.046(3) -0.003(2) -0.024(3) -0.001(3) C62 0.048(4) 0.046(4) 0.102(5) 0.019(4) 0.013(4) -0.013(3) C63 0.059(4) 0.050(4) 0.058(4) 0.003(3) -0.034(3) -0.014(3) C64 0.087(5) 0.055(4) 0.041(3) -0.007(3) -0.021(3) -0.003(4) C65 0.096(5) 0.045(4) 0.093(5) -0.006(3) -0.070(4) -0.012(4) C66 0.078(5) 0.065(4) 0.066(4) -0.008(3) -0.044(4) -0.011(4) C67 0.141(7) 0.100(6) 0.049(4) -0.037(4) 0.025(4) -0.089(6) C68 0.086(5) 0.050(4) 0.098(5) 0.006(4) -0.059(4) -0.017(4) C69 0.074(4) 0.067(5) 0.064(4) 0.010(3) -0.044(4) -0.014(4) C70 0.076(5) 0.053(4) 0.075(4) 0.003(3) -0.049(4) -0.006(4) C71 0.163(9) 0.041(4) 0.109(6) 0.004(4) -0.086(6) 0.001(5) C72 0.105(6) 0.080(5) 0.124(6) 0.020(5) -0.087(6) -0.044(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.928(3) . ? Zn1 O5 1.941(3) . ? Zn1 O7 1.953(3) . ? Zn1 O20 1.982(3) . ? Zn1 Zn3 3.0993(7) . ? Zn1 Zn2 3.1482(7) . ? Zn2 O1 1.921(3) . ? Zn2 O10 1.925(3) . ? Zn2 O9 1.967(4) . ? Zn2 O13 1.972(3) . ? Zn2 Zn3 3.1366(8) . ? Zn3 O1 1.926(3) . ? Zn3 O4 1.935(3) . ? Zn3 O21 1.964(3) . ? Zn3 O6 1.975(3) . ? Zn4 O1 2.025(3) . ? Zn4 O17 2.079(4) . ? Zn4 O25 2.094(4) . ? Zn4 O24 2.113(4) . ? Zn4 O23 2.144(4) . ? Zn4 O28 2.314(3) . ? Zn5 O12 1.921(4) . ? Zn5 O2 1.939(3) 1_446 ? Zn5 O19 1.947(3) 1_545 ? Zn5 O18 1.967(4) 1_455 ? Zn5 Zn6 3.1277(7) 1_545 ? Zn5 Zn7 3.1440(7) 1_446 ? Zn6 O16 1.908(4) 1_556 ? Zn6 O2 1.931(3) 1_456 ? Zn6 O14 1.950(4) . ? Zn6 O8 1.980(4) 1_456 ? Zn6 Zn5 3.1277(7) 1_565 ? Zn6 Zn7 3.1430(8) 1_456 ? Zn7 O2 1.918(3) . ? Zn7 O11 1.938(4) . ? Zn7 O3 1.967(3) . ? Zn7 O15 1.967(3) 1_564 ? Zn7 Zn6 3.1430(8) 1_654 ? Zn7 Zn5 3.1440(7) 1_664 ? Zn8 O2 2.023(3) 1_446 ? Zn8 O22 2.047(3) . ? Zn8 O27 2.098(3) 1_546 ? Zn8 O26 2.111(4) . ? Zn8 O30 2.128(5) . ? Zn8 O29 2.208(3) . ? O2 Zn6 1.931(3) 1_654 ? O2 Zn5 1.939(3) 1_664 ? O2 Zn8 2.023(3) 1_664 ? O3 C3 1.254(6) . ? O4 C38 1.285(6) . ? O5 C29 1.244(6) . ? O6 C35 1.250(6) . ? O7 C4 1.263(6) . ? O8 C3 1.251(6) . ? O8 Zn6 1.980(4) 1_654 ? O9 C35 1.254(6) . ? O10 C1 1.250(6) . ? O11 C2 1.288(6) 1_664 ? O12 C37 1.266(7) . ? O13 C61 1.271(6) . ? O14 C44 1.266(6) . ? O15 C46 1.265(6) . ? O15 Zn7 1.967(3) 1_546 ? O16 C64 1.279(7) . ? O16 Zn6 1.908(4) 1_554 ? O17 C1 1.240(6) . ? O18 C46 1.244(6) . ? O18 Zn5 1.967(4) 1_655 ? O19 C44 1.259(6) . ? O19 Zn5 1.947(3) 1_565 ? O20 C61 1.232(6) . ? O21 C4 1.260(6) . ? O22 C2 1.215(6) . ? O23 C38 1.230(6) . ? O24 C29 1.252(6) . ? O26 C37 1.226(6) . ? O27 C64 1.207(7) . ? O27 Zn8 2.098(3) 1_564 ? O30 C81 1.228(10) . ? C1 C7 1.516(7) . ? C2 O11 1.288(6) 1_446 ? C2 C11 1.517(7) 1_456 ? C3 C18 1.492(7) . ? C4 C14 1.484(6) . ? C5 C14 1.373(7) . ? C5 C12 1.414(7) . ? C6 C15 1.359(7) . ? C6 C7 1.416(7) . ? C7 C10 1.360(7) . ? C8 C18 1.369(7) . ? C8 C16 1.414(7) . ? C9 C33 1.373(7) . ? C9 C13 1.420(7) . ? C10 C52 1.405(7) . ? C11 C48 1.383(7) . ? C11 C17 1.385(7) . ? C11 C2 1.517(7) 1_654 ? C12 C16 1.409(8) . ? C12 C41 1.416(7) . ? C13 C52 1.412(8) . ? C13 C15 1.414(7) . ? C14 C62 1.415(8) . ? C16 C57 1.381(8) . ? C17 C55 1.364(8) . ? C18 C30 1.388(8) . ? C19 C20 1.415(6) . ? C19 C31 1.419(6) . ? C19 C51 1.424(7) . ? C20 C36 1.370(6) . ? C21 C42 1.373(7) . ? C21 C27 1.401(7) . ? C22 C23 1.372(7) . ? C22 C25 1.406(6) . ? C23 C24 1.396(7) . ? C24 C45 1.369(7) . ? C24 C29 1.498(7) . ? C25 C39 1.405(6) . ? C25 C43 1.422(7) . ? C26 C53 1.375(7) . ? C26 C28 1.393(7) . ? C26 C38 1.502(7) . ? C27 C50 1.414(8) . ? C27 C55 1.430(8) . ? C28 C31 1.379(6) . ? C30 C41 1.370(7) . ? C32 C34 1.336(7) . ? C32 C40 1.404(7) . ? C33 C58 1.439(8) . ? C33 C37 1.495(7) . ? C34 C43 1.445(7) . ? C35 C42 1.493(7) . ? C36 C47 1.419(7) . ? C36 C46 1.501(7) . ? C39 C40 1.377(7) . ? C40 C44 1.509(7) . ? C42 C56 1.401(8) . ? C43 C45 1.418(7) . ? C47 C49 1.325(7) . ? C48 C50 1.389(7) . ? C49 C51 1.442(7) . ? C50 C54 1.402(8) . ? C51 C53 1.407(6) . ? C52 C67 1.407(7) . ? C54 C56 1.367(8) . ? C57 C62 1.360(7) . ? C58 C67 1.363(8) . ? C59 C60 1.406(9) . ? C59 C71 1.408(9) . ? C60 C65 1.413(7) . ? C60 C70 1.415(9) . ? C61 C63 1.496(7) . ? C63 C65 1.367(7) . ? C63 C68 1.409(8) . ? C64 C66 1.524(8) . ? C66 C69 1.347(8) . ? C66 C71 1.419(10) . ? C68 C72 1.382(8) . ? C69 C70 1.407(7) . ? C70 C72 1.402(9) . ? C81 N1 1.416(13) . ? N1 C83 1.431(17) . ? N1 C82 1.43(2) . ? 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 Zn1 O5 121.78(13) . . ? O1 Zn1 O7 113.63(13) . . ? O5 Zn1 O7 107.40(16) . . ? O1 Zn1 O20 109.47(14) . . ? O5 Zn1 O20 100.61(17) . . ? O7 Zn1 O20 101.29(17) . . ? O1 Zn1 Zn3 36.46(8) . . ? O5 Zn1 Zn3 137.32(11) . . ? O7 Zn1 Zn3 77.21(10) . . ? O20 Zn1 Zn3 120.47(12) . . ? O1 Zn1 Zn2 35.04(8) . . ? O5 Zn1 Zn2 128.71(11) . . ? O7 Zn1 Zn2 123.76(11) . . ? O20 Zn1 Zn2 74.48(11) . . ? Zn3 Zn1 Zn2 60.265(17) . . ? O1 Zn2 O10 116.58(13) . . ? O1 Zn2 O9 112.96(14) . . ? O10 Zn2 O9 102.43(17) . . ? O1 Zn2 O13 112.72(13) . . ? O10 Zn2 O13 106.55(17) . . ? O9 Zn2 O13 104.40(16) . . ? O1 Zn2 Zn3 35.44(8) . . ? O10 Zn2 Zn3 123.75(12) . . ? O9 Zn2 Zn3 77.73(11) . . ? O13 Zn2 Zn3 128.24(11) . . ? O1 Zn2 Zn1 35.19(8) . . ? O10 Zn2 Zn1 134.90(11) . . ? O9 Zn2 Zn1 120.28(12) . . ? O13 Zn2 Zn1 77.80(11) . . ? Zn3 Zn2 Zn1 59.094(17) . . ? O1 Zn3 O4 119.66(13) . . ? O1 Zn3 O21 114.02(13) . . ? O4 Zn3 O21 109.40(16) . . ? O1 Zn3 O6 110.32(14) . . ? O4 Zn3 O6 100.93(17) . . ? O21 Zn3 O6 99.88(16) . . ? O1 Zn3 Zn1 36.50(8) . . ? O4 Zn3 Zn1 139.56(12) . . ? O21 Zn3 Zn1 77.55(11) . . ? O6 Zn3 Zn1 117.44(12) . . ? O1 Zn3 Zn2 35.32(8) . . ? O4 Zn3 Zn2 123.15(12) . . ? O21 Zn3 Zn2 127.28(11) . . ? O6 Zn3 Zn2 75.47(11) . . ? Zn1 Zn3 Zn2 60.641(16) . . ? O1 Zn4 O17 96.82(13) . . ? O1 Zn4 O25 176.16(16) . . ? O17 Zn4 O25 86.77(16) . . ? O1 Zn4 O24 96.48(13) . . ? O17 Zn4 O24 92.60(16) . . ? O25 Zn4 O24 84.70(17) . . ? O1 Zn4 O23 93.51(13) . . ? O17 Zn4 O23 93.52(15) . . ? O25 Zn4 O23 84.86(17) . . ? O24 Zn4 O23 167.58(16) . . ? O1 Zn4 O28 88.17(11) . . ? O17 Zn4 O28 174.76(12) . . ? O25 Zn4 O28 88.21(14) . . ? O24 Zn4 O28 88.40(14) . . ? O23 Zn4 O28 84.55(13) . . ? O12 Zn5 O2 117.95(15) . 1_446 ? O12 Zn5 O19 106.69(17) . 1_545 ? O2 Zn5 O19 112.98(14) 1_446 1_545 ? O12 Zn5 O18 104.63(18) . 1_455 ? O2 Zn5 O18 110.18(14) 1_446 1_455 ? O19 Zn5 O18 103.09(17) 1_545 1_455 ? O12 Zn5 Zn6 132.36(13) . 1_545 ? O2 Zn5 Zn6 36.00(8) 1_446 1_545 ? O19 Zn5 Zn6 76.98(10) 1_545 1_545 ? O18 Zn5 Zn6 121.08(12) 1_455 1_545 ? O12 Zn5 Zn7 127.65(13) . 1_446 ? O2 Zn5 Zn7 35.19(9) 1_446 1_446 ? O19 Zn5 Zn7 124.67(12) 1_545 1_446 ? O18 Zn5 Zn7 75.04(11) 1_455 1_446 ? Zn6 Zn5 Zn7 60.151(17) 1_545 1_446 ? O16 Zn6 O2 119.36(17) 1_556 1_456 ? O16 Zn6 O14 108.6(2) 1_556 . ? O2 Zn6 O14 113.17(14) 1_456 . ? O16 Zn6 O8 100.02(19) 1_556 1_456 ? O2 Zn6 O8 108.82(15) 1_456 1_456 ? O14 Zn6 O8 105.13(18) . 1_456 ? O16 Zn6 Zn5 135.70(15) 1_556 1_565 ? O2 Zn6 Zn5 36.16(8) 1_456 1_565 ? O14 Zn6 Zn5 77.02(11) . 1_565 ? O8 Zn6 Zn5 121.39(12) 1_456 1_565 ? O16 Zn6 Zn7 126.57(16) 1_556 1_456 ? O2 Zn6 Zn7 35.14(9) 1_456 1_456 ? O14 Zn6 Zn7 124.40(13) . 1_456 ? O8 Zn6 Zn7 73.69(12) 1_456 1_456 ? Zn5 Zn6 Zn7 60.182(16) 1_565 1_456 ? O2 Zn7 O11 115.04(15) . . ? O2 Zn7 O3 114.86(14) . . ? O11 Zn7 O3 102.46(17) . . ? O2 Zn7 O15 113.58(13) . 1_564 ? O11 Zn7 O15 104.59(17) . 1_564 ? O3 Zn7 O15 105.00(17) . 1_564 ? O2 Zn7 Zn6 35.41(8) . 1_654 ? O11 Zn7 Zn6 127.12(12) . 1_654 ? O3 Zn7 Zn6 79.46(11) . 1_654 ? O15 Zn7 Zn6 126.27(11) 1_564 1_654 ? O2 Zn7 Zn5 35.61(8) . 1_664 ? O11 Zn7 Zn5 128.95(12) . 1_664 ? O3 Zn7 Zn5 126.57(12) . 1_664 ? O15 Zn7 Zn5 77.99(11) 1_564 1_664 ? Zn6 Zn7 Zn5 59.667(16) 1_654 1_664 ? O2 Zn8 O22 101.80(14) 1_446 . ? O2 Zn8 O27 95.93(11) 1_446 1_546 ? O22 Zn8 O27 93.95(13) . 1_546 ? O2 Zn8 O26 96.42(16) 1_446 . ? O22 Zn8 O26 92.01(16) . . ? O27 Zn8 O26 164.90(18) 1_546 . ? O2 Zn8 O30 170.59(17) 1_446 . ? O22 Zn8 O30 87.54(18) . . ? O27 Zn8 O30 82.18(18) 1_546 . ? O26 Zn8 O30 84.2(2) . . ? O2 Zn8 O29 84.64(12) 1_446 . ? O22 Zn8 O29 173.19(14) . . ? O27 Zn8 O29 87.52(11) 1_546 . ? O26 Zn8 O29 85.01(15) . . ? O30 Zn8 O29 86.06(17) . . ? Zn2 O1 Zn3 109.24(13) . . ? Zn2 O1 Zn1 109.77(13) . . ? Zn3 O1 Zn1 107.05(13) . . ? Zn2 O1 Zn4 113.36(13) . . ? Zn3 O1 Zn4 109.23(13) . . ? Zn1 O1 Zn4 108.00(13) . . ? Zn7 O2 Zn6 109.46(14) . 1_654 ? Zn7 O2 Zn5 109.20(14) . 1_664 ? Zn6 O2 Zn5 107.84(14) 1_654 1_664 ? Zn7 O2 Zn8 112.80(14) . 1_664 ? Zn6 O2 Zn8 108.75(13) 1_654 1_664 ? Zn5 O2 Zn8 108.67(13) 1_664 1_664 ? C3 O3 Zn7 126.5(4) . . ? C38 O4 Zn3 118.9(3) . . ? C29 O5 Zn1 118.8(3) . . ? C35 O6 Zn3 131.6(3) . . ? C4 O7 Zn1 129.6(3) . . ? C3 O8 Zn6 133.8(4) . 1_654 ? C35 O9 Zn2 129.0(4) . . ? C1 O10 Zn2 122.1(3) . . ? C2 O11 Zn7 125.4(3) 1_664 . ? C37 O12 Zn5 121.6(4) . . ? C61 O13 Zn2 127.4(3) . . ? C44 O14 Zn6 129.7(4) . . ? C46 O15 Zn7 128.0(3) . 1_546 ? C64 O16 Zn6 119.0(4) . 1_554 ? C1 O17 Zn4 139.9(4) . . ? C46 O18 Zn5 132.2(3) . 1_655 ? C44 O19 Zn5 130.1(3) . 1_565 ? C61 O20 Zn1 132.1(3) . . ? C4 O21 Zn3 128.1(3) . . ? C2 O22 Zn8 138.1(4) . . ? C38 O23 Zn4 133.8(4) . . ? C29 O24 Zn4 137.0(4) . . ? C37 O26 Zn8 131.1(4) . . ? C64 O27 Zn8 134.1(3) . 1_564 ? C81 O30 Zn8 118.8(7) . . ? O17 C1 O10 125.2(5) . . ? O17 C1 C7 117.8(5) . . ? O10 C1 C7 117.0(5) . . ? O22 C2 O11 126.7(5) . 1_446 ? O22 C2 C11 118.9(5) . 1_456 ? O11 C2 C11 114.4(5) 1_446 1_456 ? O8 C3 O3 125.7(5) . . ? O8 C3 C18 117.2(5) . . ? O3 C3 C18 117.1(5) . . ? O21 C4 O7 126.2(4) . . ? O21 C4 C14 117.2(5) . . ? O7 C4 C14 116.5(4) . . ? C14 C5 C12 122.5(5) . . ? C15 C6 C7 120.5(5) . . ? C10 C7 C6 119.8(5) . . ? C10 C7 C1 121.0(5) . . ? C6 C7 C1 119.2(5) . . ? C18 C8 C16 121.9(5) . . ? C33 C9 C13 121.0(5) . . ? C7 C10 C52 121.2(5) . . ? C48 C11 C17 119.4(5) . . ? C48 C11 C2 120.6(5) . 1_654 ? C17 C11 C2 120.0(5) . 1_654 ? C16 C12 C5 118.2(5) . . ? C16 C12 C41 119.3(5) . . ? C5 C12 C41 122.4(5) . . ? C52 C13 C15 119.3(5) . . ? C52 C13 C9 119.6(5) . . ? C15 C13 C9 121.1(5) . . ? C5 C14 C62 117.6(5) . . ? C5 C14 C4 120.9(5) . . ? C62 C14 C4 121.5(5) . . ? C6 C15 C13 120.3(5) . . ? C57 C16 C12 118.6(5) . . ? C57 C16 C8 123.2(5) . . ? C12 C16 C8 118.3(5) . . ? C55 C17 C11 121.6(6) . . ? C8 C18 C30 118.8(5) . . ? C8 C18 C3 120.0(5) . . ? C30 C18 C3 121.2(5) . . ? C20 C19 C31 122.4(5) . . ? C20 C19 C51 119.4(4) . . ? C31 C19 C51 118.1(4) . . ? C36 C20 C19 121.0(5) . . ? C42 C21 C27 121.5(5) . . ? C23 C22 C25 120.1(5) . . ? C22 C23 C24 121.8(5) . . ? C45 C24 C23 119.3(5) . . ? C45 C24 C29 119.9(5) . . ? C23 C24 C29 120.8(5) . . ? C39 C25 C22 122.7(5) . . ? C39 C25 C43 118.4(4) . . ? C22 C25 C43 118.9(4) . . ? C53 C26 C28 120.4(4) . . ? C53 C26 C38 118.7(5) . . ? C28 C26 C38 120.9(5) . . ? C21 C27 C50 119.4(5) . . ? C21 C27 C55 121.6(6) . . ? C50 C27 C55 119.0(5) . . ? C31 C28 C26 120.7(5) . . ? O5 C29 O24 125.6(5) . . ? O5 C29 C24 116.3(5) . . ? O24 C29 C24 118.1(4) . . ? C41 C30 C18 122.0(5) . . ? C28 C31 C19 120.5(5) . . ? C34 C32 C40 120.6(5) . . ? C9 C33 C58 118.7(5) . . ? C9 C33 C37 120.9(5) . . ? C58 C33 C37 120.4(5) . . ? C32 C34 C43 121.0(5) . . ? O6 C35 O9 125.5(5) . . ? O6 C35 C42 118.3(5) . . ? O9 C35 C42 116.2(5) . . ? C20 C36 C47 119.0(5) . . ? C20 C36 C46 120.2(5) . . ? C47 C36 C46 120.7(5) . . ? O26 C37 O12 124.3(5) . . ? O26 C37 C33 119.7(6) . . ? O12 C37 C33 115.7(5) . . ? O23 C38 O4 125.4(5) . . ? O23 C38 C26 118.7(5) . . ? O4 C38 C26 115.9(5) . . ? C40 C39 C25 121.2(5) . . ? C39 C40 C32 120.3(5) . . ? C39 C40 C44 119.6(5) . . ? C32 C40 C44 120.0(5) . . ? C30 C41 C12 119.7(5) . . ? C21 C42 C56 119.1(5) . . ? C21 C42 C35 120.3(5) . . ? C56 C42 C35 120.6(5) . . ? C45 C43 C25 119.0(5) . . ? C45 C43 C34 122.6(5) . . ? C25 C43 C34 118.5(5) . . ? O19 C44 O14 126.1(5) . . ? O19 C44 C40 117.1(5) . . ? O14 C44 C40 116.7(5) . . ? C24 C45 C43 121.0(5) . . ? O18 C46 O15 125.8(5) . . ? O18 C46 C36 118.0(5) . . ? O15 C46 C36 116.1(5) . . ? C49 C47 C36 121.9(5) . . ? C11 C48 C50 121.5(5) . . ? C47 C49 C51 121.2(5) . . ? C48 C50 C54 123.2(6) . . ? C48 C50 C27 119.0(5) . . ? C54 C50 C27 117.8(5) . . ? C53 C51 C19 119.9(5) . . ? C53 C51 C49 122.6(5) . . ? C19 C51 C49 117.5(4) . . ? C10 C52 C67 122.2(5) . . ? C10 C52 C13 118.8(5) . . ? C67 C52 C13 118.9(5) . . ? C26 C53 C51 120.3(5) . . ? C56 C54 C50 121.9(6) . . ? C17 C55 C27 119.6(6) . . ? C54 C56 C42 120.2(5) . . ? C62 C57 C16 122.7(6) . . ? C67 C58 C33 120.8(6) . . ? C60 C59 C71 118.0(7) . . ? C59 C60 C65 121.5(6) . . ? C59 C60 C70 120.6(6) . . ? C65 C60 C70 117.7(6) . . ? O20 C61 O13 125.8(5) . . ? O20 C61 C63 117.8(5) . . ? O13 C61 C63 116.5(5) . . ? C57 C62 C14 120.3(6) . . ? C65 C63 C68 118.9(5) . . ? C65 C63 C61 119.2(5) . . ? C68 C63 C61 121.9(5) . . ? O27 C64 O16 127.1(6) . . ? O27 C64 C66 119.2(6) . . ? O16 C64 C66 113.4(6) . . ? C63 C65 C60 122.6(6) . . ? C69 C66 C71 119.4(6) . . ? C69 C66 C64 120.8(6) . . ? C71 C66 C64 119.8(6) . . ? C58 C67 C52 121.0(6) . . ? C72 C68 C63 120.1(6) . . ? C66 C69 C70 122.0(7) . . ? C72 C70 C69 121.7(6) . . ? C72 C70 C60 119.5(5) . . ? C69 C70 C60 118.7(6) . . ? C59 C71 C66 121.0(7) . . ? C68 C72 C70 121.0(6) . . ? O30 C81 N1 123.2(11) . . ? C81 N1 C83 116.6(14) . . ? C81 N1 C82 126.2(16) . . ? C83 N1 C82 117.1(17) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.487 _refine_diff_density_min -1.384 _refine_diff_density_rms 0.098 # 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 -0.006 0.005 -0.003 3408 379 ' ' _platon_squeeze_details ; ; # Attachment '- SUMOF-4.cif' data_SUMOF-4 _database_code_depnum_ccdc_archive 'CCDC 853632' #TrackingRef '- SUMOF-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H24 N O15 Zn4' _chemical_formula_weight 936.01 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 18.3770(6) _cell_length_b 17.3043(4) _cell_length_c 17.9565(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5710.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5610 _cell_measurement_theta_min 4.1876 _cell_measurement_theta_max 32.1671 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85492 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 16.5467 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19462 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5966 _reflns_number_gt 4341 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1180P)^2^+0.0194P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5966 _refine_ls_number_parameters 270 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1937 _refine_ls_wR_factor_gt 0.1828 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.087 _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 0.39337(4) 0.32393(4) 0.0000 0.0317(2) Uani 1 2 d S . . Zn2 Zn 0.21553(4) 0.32091(4) 0.0000 0.0390(2) Uani 1 2 d S . . Zn3 Zn 0.31234(3) 0.19160(3) 0.08628(3) 0.03256(19) Uani 1 1 d . . . O1 O 0.30912(19) 0.2580(2) 0.0000 0.0297(9) Uani 1 2 d S . . O2 O 0.4561(2) 0.3038(2) 0.0862(2) 0.0641(11) Uani 1 1 d . . . O3 O 0.3798(3) 0.4347(3) 0.0000 0.0607(14) Uani 1 2 d S . . O4 O 0.2042(2) 0.3181(2) 0.1195(3) 0.0719(13) Uani 1 1 d . . . O5 O 0.4072(2) 0.1992(2) 0.1386(2) 0.0607(10) Uani 1 1 d . . . O6 O 0.2595(3) 0.4306(3) 0.0000 0.0643(15) Uani 1 2 d S . . O7 O 0.2400(2) 0.2046(2) 0.1632(2) 0.0602(10) Uani 1 1 d . . . O8 O 0.3076(2) 0.08125(19) 0.0614(2) 0.0567(10) Uani 1 1 d . . . O9 O 0.1149(4) 0.3766(4) 0.0000 0.096(2) Uani 1 2 d SD . . H9A H 0.127(8) 0.408(4) 0.0422(6) 0.115 Uiso 0.50 1 d PD . . O10 O 0.1635(4) 0.2108(4) 0.0000 0.0841(19) Uani 1 2 d S . . C2 C 0.3176(4) 0.5522(4) 0.0000 0.0445(16) Uani 1 2 d S . . C4 C 0.3065(3) 0.0476(4) 0.0000 0.0430(16) Uani 1 2 d S . . C6 C 0.3189(4) 0.4651(3) 0.0000 0.0422(16) Uani 1 2 d S . . C7 C 0.1987(3) 0.2620(3) 0.1630(3) 0.0552(14) Uani 1 1 d . . . C9 C 0.3731(5) 0.6742(5) -0.0174(7) 0.050(5) Uani 0.50 1 d P . . H9 H 0.4146 0.7017 -0.0308 0.059 Uiso 0.50 1 calc PR . . C10 C 0.3753(5) 0.5940(5) 0.0153(13) 0.052(7) Uani 0.50 1 d P . . H10 H 0.4191 0.5691 0.0249 0.063 Uiso 0.50 1 calc PR . . C11 C 0.3098(4) 0.7138(4) 0.0000 0.0459(17) Uani 1 2 d S . . C12 C 0.1377(3) 0.2611(3) 0.2179(3) 0.0575(14) Uani 1 1 d . . . C13 C 0.5195(3) 0.2443(3) 0.1844(3) 0.0515(12) Uani 1 1 d . . . C15 C 0.4557(3) 0.2496(3) 0.1320(3) 0.0483(12) Uani 1 1 d . . . C16 C 0.5303(4) 0.1813(3) 0.2287(4) 0.0718(19) Uani 1 1 d . . . H16 H 0.4977 0.1402 0.2268 0.086 Uiso 1 1 calc R . . C17 C 0.5700(4) 0.3036(4) 0.1860(4) 0.091(3) Uani 1 1 d . . . H17 H 0.5651 0.3453 0.1537 0.109 Uiso 1 1 calc R . . C19 C 0.1278(4) 0.1988(4) 0.2647(4) 0.086(2) Uani 1 1 d . . . H19 H 0.1605 0.1578 0.2631 0.103 Uiso 1 1 calc R . . C20 C 0.5894(4) 0.1779(3) 0.2767(4) 0.080(2) Uani 1 1 d . . . H20 H 0.5966 0.1340 0.3056 0.096 Uiso 1 1 calc R . . C5 C 0.3073(3) -0.03905(19) 0.0000 0.0456(16) Uani 1 2 d SG . . C23B C 0.2878(5) -0.0799(3) -0.0636(2) 0.073(5) Uani 0.50 1 d PG . . H23B H 0.2745 -0.0535 -0.1066 0.088 Uiso 0.50 1 calc PR . . C22B C 0.2883(5) -0.1602(3) -0.0629(5) 0.068(4) Uani 0.50 1 d PG . . H22B H 0.2750 -0.1874 -0.1055 0.081 Uiso 0.50 1 calc PR . . C8 C 0.3082(3) -0.19970(19) 0.0002(6) 0.0519(19) Uani 1 2 d SG . . C23A C 0.3276(5) -0.1588(3) 0.0650(5) 0.068(4) Uani 0.50 1 d PG . . H23A H 0.3407 -0.1854 0.1080 0.081 Uiso 0.50 1 calc PR . . C22A C 0.3272(5) -0.0785(3) 0.0643(2) 0.073(5) Uani 0.50 1 d PG . . H22A H 0.3402 -0.0512 0.1069 0.088 Uiso 0.50 1 calc PR . . C25 C 0.2531(6) 0.5898(5) 0.0208(6) 0.058(4) Uani 0.50 1 d P . . H25 H 0.2123 0.5614 0.0345 0.070 Uiso 0.50 1 calc PR . . C26 C 0.2507(7) 0.6722(5) -0.0208(7) 0.068(6) Uani 0.50 1 d P . . H26 H 0.2083 0.6975 -0.0351 0.081 Uiso 0.50 1 calc PR . . N1 N 0.0659(10) 0.1305(10) 0.0000 0.176(6) Uiso 1 2 d SD . . C30 C 0.1069(10) 0.2005(12) 0.0000 0.153(6) Uiso 1 2 d S . . H30 H 0.0786 0.2451 0.0000 0.184 Uiso 1 2 calc SR . . C31 C 0.1077(13) 0.0671(15) 0.0346(13) 0.189(12) Uiso 0.50 1 d P . . H31A H 0.1583 0.0806 0.0360 0.227 Uiso 0.50 1 calc PR . . H31B H 0.1015 0.0207 0.0059 0.227 Uiso 0.50 1 calc PR . . H31C H 0.0904 0.0586 0.0844 0.227 Uiso 0.50 1 calc PR . . C32 C -0.0183(14) 0.123(2) 0.0000 0.37(2) Uiso 1 2 d SD . . H32A H -0.0389 0.1597 0.0337 0.443 Uiso 0.50 1 calc PR . . H32B H -0.0315 0.0714 0.0156 0.443 Uiso 0.50 1 calc PR . . H32C H -0.0365 0.1318 -0.0493 0.443 Uiso 0.50 1 calc PR . . 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 0.0302(4) 0.0264(3) 0.0386(4) 0.000 0.000 -0.0016(3) Zn2 0.0337(4) 0.0306(4) 0.0527(5) 0.000 0.000 0.0025(3) Zn3 0.0342(3) 0.0275(3) 0.0359(3) 0.00130(18) 0.0026(2) -0.00071(18) O1 0.030(2) 0.0249(19) 0.034(2) 0.000 0.000 0.0053(15) O2 0.057(3) 0.062(2) 0.073(3) 0.0194(19) -0.031(2) -0.0137(19) O3 0.054(3) 0.028(2) 0.100(4) 0.000 0.000 0.001(2) O4 0.090(3) 0.057(2) 0.070(3) 0.005(2) 0.045(2) 0.004(2) O5 0.051(2) 0.065(2) 0.067(2) 0.0144(18) -0.0241(18) -0.0097(18) O6 0.059(4) 0.025(2) 0.109(4) 0.000 0.000 -0.003(2) O7 0.056(2) 0.068(2) 0.057(2) 0.0066(18) 0.0229(18) 0.011(2) O8 0.083(3) 0.0270(16) 0.060(2) -0.0021(16) 0.0004(18) 0.0033(16) O9 0.049(4) 0.096(5) 0.143(6) 0.000 0.000 0.024(4) O10 0.052(4) 0.075(4) 0.125(6) 0.000 0.000 -0.026(3) C2 0.059(5) 0.024(3) 0.050(4) 0.000 0.000 0.001(3) C4 0.039(4) 0.031(3) 0.059(4) 0.000 0.000 -0.003(3) C6 0.057(5) 0.023(3) 0.047(4) 0.000 0.000 -0.001(3) C7 0.060(3) 0.052(3) 0.054(3) 0.002(3) 0.021(2) 0.001(3) C9 0.048(5) 0.026(4) 0.074(15) 0.009(4) 0.005(5) -0.005(3) C10 0.040(5) 0.030(4) 0.09(2) -0.002(5) -0.019(7) 0.002(3) C11 0.057(5) 0.024(3) 0.057(4) 0.000 0.000 -0.005(3) C12 0.062(4) 0.056(3) 0.054(3) 0.006(2) 0.021(3) 0.006(3) C13 0.048(3) 0.051(3) 0.055(3) 0.003(2) -0.021(2) -0.003(2) C15 0.049(3) 0.048(3) 0.048(3) 0.003(2) -0.013(2) -0.002(2) C16 0.067(4) 0.072(4) 0.076(4) 0.022(3) -0.036(3) -0.027(3) C17 0.100(6) 0.066(4) 0.105(5) 0.034(4) -0.071(5) -0.034(4) C19 0.090(5) 0.067(4) 0.101(5) 0.028(3) 0.051(4) 0.032(4) C20 0.095(5) 0.064(4) 0.082(4) 0.025(3) -0.045(4) -0.024(3) C5 0.049(4) 0.025(3) 0.062(4) 0.000 0.000 0.000(3) C23B 0.121(15) 0.029(3) 0.069(4) 0.006(5) -0.026(5) -0.005(5) C22B 0.105(13) 0.032(3) 0.066(4) -0.004(5) -0.029(5) -0.009(5) C8 0.061(5) 0.024(3) 0.071(5) 0.000 0.000 0.002(3) C23A 0.105(13) 0.032(3) 0.066(4) -0.004(5) -0.029(5) -0.009(5) C22A 0.121(15) 0.029(3) 0.069(4) 0.006(5) -0.026(5) -0.005(5) C25 0.064(6) 0.034(4) 0.077(12) -0.001(4) 0.026(5) 0.000(4) C26 0.068(7) 0.033(4) 0.102(17) -0.011(5) -0.035(7) 0.010(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 O1 1.923(4) . ? Zn1 O3 1.934(5) . ? Zn1 O2 1.961(3) . ? Zn1 O2 1.961(3) 6 ? Zn1 Zn3 3.1403(7) 6 ? Zn1 Zn3 3.1403(7) . ? Zn2 O1 2.035(4) . ? Zn2 O6 2.063(5) . ? Zn2 O9 2.084(6) . ? Zn2 O10 2.132(6) . ? Zn2 O4 2.156(4) . ? Zn2 O4 2.156(4) 6 ? Zn3 O1 1.930(2) . ? Zn3 O7 1.930(3) . ? Zn3 O8 1.963(3) . ? Zn3 O5 1.984(3) . ? Zn3 Zn3 3.0987(10) 6 ? O1 Zn3 1.930(2) 6 ? O2 C15 1.247(6) . ? O3 C6 1.237(8) . ? O4 C7 1.249(6) . ? O5 C15 1.253(6) . ? O6 C6 1.243(8) . ? O7 C7 1.250(6) . ? O8 C4 1.248(5) . ? O10 C30 1.056(17) . ? C2 C10 1.312(12) . ? C2 C10 1.312(12) 6 ? C2 C25 1.403(12) 6 ? C2 C25 1.403(12) . ? C2 C6 1.508(8) . ? C4 O8 1.248(5) 6 ? C4 C5 1.499(7) . ? C7 C12 1.493(7) . ? C9 C11 1.384(11) . ? C9 C10 1.390(11) 6 ? C10 C9 1.390(11) 6 ? C11 C26 1.356(12) . ? C11 C26 1.356(12) 6 ? C11 C9 1.384(11) 6 ? C11 C8 1.498(7) 1_565 ? C12 C19 1.379(7) . ? C12 C20 1.382(8) 4_455 ? C13 C16 1.365(7) . ? C13 C17 1.384(7) . ? C13 C15 1.507(6) . ? C16 C20 1.387(8) . ? C17 C19 1.383(8) 4 ? C19 C17 1.383(8) 4_455 ? C20 C12 1.382(8) 4 ? C5 C23B 1.390(6) 6 ? C5 C23B 1.3896 . ? C5 C22A 1.3904 . ? C5 C22A 1.390(7) 6 ? C23B C22B 1.3900 . ? C22B C8 1.3725 . ? C8 C22B 1.367(14) 6 ? C8 C23A 1.4074 . ? C8 C23A 1.413(15) 6 ? C8 C11 1.498(7) 1_545 ? C23A C22A 1.3900 . ? C25 C26 1.425(12) 6 ? C26 C25 1.425(12) 6 ? N1 C30 1.43(2) . ? N1 C31 1.48(2) 6 ? N1 C31 1.48(2) . ? N1 C32 1.554(18) . ? 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 Zn1 O3 118.99(19) . . ? O1 Zn1 O2 111.56(12) . . ? O3 Zn1 O2 104.59(15) . . ? O1 Zn1 O2 111.56(12) . 6 ? O3 Zn1 O2 104.59(15) . 6 ? O2 Zn1 O2 104.3(3) . 6 ? Zn3 Zn1 Zn3 59.12(2) 6 . ? O1 Zn2 O6 99.27(18) . . ? O1 Zn2 O9 175.2(2) . . ? O6 Zn2 O9 85.5(3) . . ? O1 Zn2 O10 84.3(2) . . ? O6 Zn2 O10 176.4(3) . . ? O9 Zn2 O10 90.9(3) . . ? O1 Zn2 O4 93.97(12) . . ? O6 Zn2 O4 93.37(11) . . ? O9 Zn2 O4 85.70(12) . . ? O10 Zn2 O4 86.35(11) . . ? O1 Zn2 O4 93.97(12) . 6 ? O6 Zn2 O4 93.37(11) . 6 ? O9 Zn2 O4 85.70(12) . 6 ? O10 Zn2 O4 86.35(11) . 6 ? O4 Zn2 O4 168.6(3) . 6 ? O1 Zn3 O7 118.93(15) . . ? O1 Zn3 O8 113.30(15) . . ? O7 Zn3 O8 104.23(16) . . ? O1 Zn3 O5 111.56(15) . . ? O7 Zn3 O5 104.97(17) . . ? O8 Zn3 O5 102.18(16) . . ? Zn1 O1 Zn3 109.18(12) . . ? Zn1 O1 Zn3 109.18(12) . 6 ? Zn3 O1 Zn3 106.80(18) . 6 ? Zn1 O1 Zn2 111.29(18) . . ? Zn3 O1 Zn2 110.15(12) . . ? Zn3 O1 Zn2 110.15(12) 6 . ? C15 O2 Zn1 130.6(3) . . ? C6 O3 Zn1 122.5(4) . . ? C7 O4 Zn2 130.4(4) . . ? C15 O5 Zn3 128.8(3) . . ? C6 O6 Zn2 141.7(4) . . ? C7 O7 Zn3 120.6(3) . . ? C4 O8 Zn3 131.0(4) . . ? C30 O10 Zn2 126.3(13) . . ? C10 C2 C25 118.9(7) . 6 ? C10 C2 C25 111.8(8) 6 6 ? C10 C2 C25 111.8(8) . . ? C10 C2 C25 118.9(7) 6 . ? C10 C2 C6 122.5(7) . . ? C10 C2 C6 122.5(7) 6 . ? C25 C2 C6 118.5(6) 6 . ? C25 C2 C6 118.5(6) . . ? O8 C4 O8 124.3(6) . 6 ? O8 C4 C5 117.8(3) . . ? O8 C4 C5 117.8(3) 6 . ? O3 C6 O6 126.2(6) . . ? O3 C6 C2 116.0(6) . . ? O6 C6 C2 117.8(6) . . ? O4 C7 O7 124.7(5) . . ? O4 C7 C12 118.9(5) . . ? O7 C7 C12 116.4(5) . . ? C11 C9 C10 120.8(9) . 6 ? C2 C10 C9 122.2(9) . 6 ? C26 C11 C9 118.2(7) . 6 ? C26 C11 C9 110.4(7) 6 6 ? C26 C11 C9 110.4(7) . . ? C26 C11 C9 118.2(7) 6 . ? C26 C11 C8 121(2) . 1_565 ? C26 C11 C8 121(2) 6 1_565 ? C9 C11 C8 121(2) 6 1_565 ? C9 C11 C8 121(2) . 1_565 ? C19 C12 C20 118.0(5) . 4_455 ? C19 C12 C7 120.7(5) . . ? C20 C12 C7 121.3(5) 4_455 . ? C16 C13 C17 119.0(5) . . ? C16 C13 C15 121.6(5) . . ? C17 C13 C15 119.3(5) . . ? O2 C15 O5 126.1(5) . . ? O2 C15 C13 116.9(4) . . ? O5 C15 C13 117.0(4) . . ? C13 C16 C20 120.5(5) . . ? C19 C17 C13 120.3(5) 4 . ? C12 C19 C17 121.0(5) . 4_455 ? C12 C20 C16 121.0(5) 4 . ? C23B C5 C23B 110.49(17) 6 . ? C23B C5 C22A 120.0 . . ? C23B C5 C22A 120.00(19) 6 6 ? C22A C5 C22A 112.28(18) . 6 ? C23B C5 C4 120.4(2) 6 . ? C23B C5 C4 120.4(3) . . ? C22A C5 C4 119.6(3) . . ? C22A C5 C4 119.6(2) 6 . ? C22B C23B C5 120.0 . . ? C8 C22B C23B 120.4 . . ? C22B C8 C22B 111.1(4) 6 . ? C22B C8 C23A 120.0 . . ? C22B C8 C23A 119.99(19) 6 6 ? C23A C8 C23A 111.6(4) . 6 ? C22B C8 C11 120.5(10) 6 1_545 ? C22B C8 C11 120.1(7) . 1_545 ? C23A C8 C11 119.9(7) . 1_545 ? C23A C8 C11 119.6(10) 6 1_545 ? C8 C23A C22A 119.6 . . ? C23A C22A C5 120.0 . . ? C2 C25 C26 119.3(9) . 6 ? C11 C26 C25 120.4(9) . 6 ? C30 N1 C31 111.0(17) . 6 ? C30 N1 C31 111.0(17) . . ? C30 N1 C32 127(2) . . ? C31 N1 C32 117(2) 6 . ? C31 N1 C32 117(2) . . ? O10 C30 N1 132(2) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.649 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.110 # 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 0.492 -0.003 -0.003 2502 232 ' ' _platon_squeeze_details ; ;