data_publication_text _publ_contact_author_name 'Zujin Lin' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China ; _publ_contact_author_email linzujin@fjirsm.ac.cn _publ_contact_author_phone +86-591-83725186 _publ_contact_author_fax +86-591-83796710 loop_ _publ_author_name _publ_author_address 'Lin, Zujin' ; State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China ; data_Cu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H20 Cu4 O24' _chemical_formula_weight 1102.69 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2970(5) _cell_length_b 26.0570(12) _cell_length_c 26.0840(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8357.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9641 _cell_measurement_theta_min 2.7602 _cell_measurement_theta_max 27.4526 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7101 _exptl_absorpt_correction_T_max 0.8335 _exptl_absorpt_process_details ? _exptl_special_details ; The structure contains disordered solvents. Because it was difficult to refine a xonsisten disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. (see more at the bottom of this .cif file) ; _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 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 10359 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59094 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10111 _reflns_number_gt 9654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1809P)^2^+23.8384P] 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 10111 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.2715 _refine_ls_wR_factor_gt 0.2668 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Cu1 Cu 1.14653(7) 0.22428(3) 0.2500 0.0200(2) Uani 1 2 d S . . Cu2 Cu 0.99600(7) 0.29698(3) 0.2500 0.0207(2) Uani 1 2 d S . . Cu3 Cu 0.07413(4) -0.00640(2) 0.03637(2) 0.02050(18) Uani 1 1 d . . . C1 C 0.9668(5) 0.2135(2) 0.1818(2) 0.0316(11) Uani 1 1 d . . . C2 C 0.9054(5) 0.1883(2) 0.1389(2) 0.0319(11) Uani 1 1 d . . . C3 C 0.8142(5) 0.2135(2) 0.1188(2) 0.0359(13) Uani 1 1 d . . . H3 H 0.7914 0.2444 0.1330 0.043 Uiso 1 1 calc R . . C4 C 0.7579(5) 0.1925(2) 0.0779(2) 0.0345(12) Uani 1 1 d . . . C5 C 0.7916(5) 0.1465(2) 0.0565(2) 0.0330(12) Uani 1 1 d . . . H5 H 0.7543 0.1327 0.0287 0.040 Uiso 1 1 calc R . . C6 C 0.8819(4) 0.1209(2) 0.0767(2) 0.0301(11) Uani 1 1 d . . . C7 C 0.9398(4) 0.1418(2) 0.1179(2) 0.0295(11) Uani 1 1 d . . . H7 H 1.0002 0.1249 0.1311 0.035 Uiso 1 1 calc R . . C8 C 0.9223(4) 0.0730(2) 0.0512(2) 0.0279(10) Uani 1 1 d . . . C9 C 0.6152(4) 0.2050(2) 0.0169(2) 0.0321(12) Uani 1 1 d . . . H9A H 0.5707 0.1755 0.0254 0.039 Uiso 1 1 calc R . . H9B H 0.6649 0.1955 -0.0103 0.039 Uiso 1 1 calc R . . C10 C 0.5434(6) 0.2500 0.0000 0.0265(14) Uani 1 2 d S . . C11 C 0.4733(4) 0.2329(2) -0.0452(2) 0.0296(11) Uani 1 1 d . . . H11A H 0.4230 0.2598 -0.0548 0.035 Uiso 1 1 calc R . . H11B H 0.5185 0.2247 -0.0745 0.035 Uiso 1 1 calc R . . C12 C 0.3335(5) 0.1698(2) -0.0582(2) 0.0334(12) Uani 1 1 d . . . C13 C 0.3020(5) 0.1908(2) -0.1050(2) 0.0317(12) Uani 1 1 d . . . H13 H 0.3397 0.2184 -0.1190 0.038 Uiso 1 1 calc R . . C14 C 0.2132(5) 0.1698(2) -0.1305(2) 0.0322(11) Uani 1 1 d . . . C15 C 0.1570(5) 0.1281(2) -0.1106(2) 0.0317(11) Uani 1 1 d . . . H15 H 0.0974 0.1146 -0.1280 0.038 Uiso 1 1 calc R . . C16 C 0.1912(5) 0.1068(2) -0.0643(2) 0.0323(12) Uani 1 1 d . . . C17 C 0.2790(5) 0.1277(2) -0.0382(2) 0.0329(12) Uani 1 1 d . . . H17 H 0.3013 0.1135 -0.0072 0.039 Uiso 1 1 calc R . . C18 C 0.1700(4) 0.1939(2) -0.1791(2) 0.0280(10) Uani 1 1 d . . . C19 C 0.1256(4) 0.0642(2) -0.0405(2) 0.0294(11) Uani 1 1 d . . . O1W O 1.2658(6) 0.1648(3) 0.2500 0.068(3) Uani 1 2 d S . . O2W O 0.8759(7) 0.3577(3) 0.2500 0.079(3) Uani 1 2 d S . . O3 O 1.0524(3) 0.19224(16) 0.19689(15) 0.0307(8) Uani 1 1 d . . . O4 O 0.9287(4) 0.2553(2) 0.1976(2) 0.0583(17) Uani 1 1 d . . . O5 O 1.0022(3) 0.05097(16) 0.07124(17) 0.0341(9) Uani 1 1 d . . . O6 O 0.8753(3) 0.06045(15) 0.01033(16) 0.0328(9) Uani 1 1 d . . . O7 O 0.6745(4) 0.22190(19) 0.0611(2) 0.0479(13) Uani 1 1 d . . . O8 O 0.4151(4) 0.18816(19) -0.02822(18) 0.0428(11) Uani 1 1 d . . . O9 O 0.2147(3) 0.23359(15) -0.19545(15) 0.0289(8) Uani 1 1 d . . . O10 O 0.0864(4) 0.1727(2) -0.1975(2) 0.0559(15) Uani 1 1 d . . . O11 O 0.0380(3) 0.05329(17) -0.06211(17) 0.0364(9) Uani 1 1 d . . . O12 O 0.1631(3) 0.04433(17) -0.00002(16) 0.0350(9) Uani 1 1 d . . . O13W O 0.1877(4) -0.0266(2) 0.0953(2) 0.0546(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0208(4) 0.0230(4) 0.0164(4) 0.000 0.000 0.0040(3) Cu2 0.0217(4) 0.0234(4) 0.0170(4) 0.000 0.000 0.0046(3) Cu3 0.0216(3) 0.0177(3) 0.0222(3) 0.0003(2) -0.0058(2) -0.0007(2) C1 0.031(3) 0.034(3) 0.029(3) -0.005(2) -0.004(2) 0.000(2) C2 0.030(3) 0.031(3) 0.034(3) -0.010(2) -0.006(2) 0.005(2) C3 0.034(3) 0.036(3) 0.038(3) -0.015(2) -0.011(2) 0.009(2) C4 0.033(3) 0.033(3) 0.037(3) -0.011(2) -0.010(2) 0.008(2) C5 0.029(3) 0.032(3) 0.038(3) -0.012(2) -0.012(2) 0.006(2) C6 0.028(2) 0.026(3) 0.037(3) -0.009(2) -0.006(2) 0.002(2) C7 0.026(2) 0.036(3) 0.026(2) -0.006(2) -0.006(2) 0.003(2) C8 0.025(2) 0.027(3) 0.031(3) -0.006(2) -0.002(2) 0.0035(19) C9 0.027(2) 0.034(3) 0.035(3) -0.012(2) -0.009(2) 0.005(2) C10 0.025(3) 0.026(4) 0.029(4) -0.002(3) 0.000 0.000 C11 0.025(2) 0.030(3) 0.034(3) 0.007(2) -0.005(2) -0.007(2) C12 0.030(3) 0.039(3) 0.031(3) 0.010(2) -0.005(2) -0.006(2) C13 0.033(3) 0.033(3) 0.029(3) 0.012(2) -0.005(2) -0.008(2) C14 0.031(3) 0.032(3) 0.033(3) 0.009(2) -0.005(2) -0.005(2) C15 0.030(3) 0.030(3) 0.035(3) 0.007(2) -0.005(2) -0.007(2) C16 0.030(3) 0.034(3) 0.033(3) 0.009(2) -0.006(2) -0.004(2) C17 0.030(3) 0.038(3) 0.031(3) 0.010(2) -0.005(2) -0.005(2) C18 0.029(2) 0.030(3) 0.025(2) 0.002(2) -0.005(2) -0.002(2) C19 0.030(2) 0.027(3) 0.031(3) 0.006(2) -0.002(2) -0.007(2) O1W 0.039(4) 0.049(4) 0.118(8) 0.000 0.000 0.022(3) O2W 0.042(4) 0.039(4) 0.157(10) 0.000 0.000 0.019(3) O3 0.0286(18) 0.034(2) 0.0293(18) -0.0092(16) -0.0065(15) 0.0052(16) O4 0.052(3) 0.056(3) 0.067(3) -0.040(3) -0.036(3) 0.030(2) O5 0.036(2) 0.030(2) 0.036(2) -0.0103(17) -0.0091(17) 0.0078(16) O6 0.0335(19) 0.0283(19) 0.037(2) -0.0117(16) -0.0114(17) 0.0091(16) O7 0.043(2) 0.047(3) 0.054(3) -0.029(2) -0.028(2) 0.023(2) O8 0.041(2) 0.048(3) 0.040(2) 0.022(2) -0.019(2) -0.022(2) O9 0.0271(17) 0.035(2) 0.0243(17) 0.0071(15) -0.0035(14) -0.0038(15) O10 0.060(3) 0.047(3) 0.061(3) 0.029(2) -0.040(3) -0.027(2) O11 0.034(2) 0.038(2) 0.037(2) 0.0129(18) -0.0100(17) -0.0121(18) O12 0.036(2) 0.034(2) 0.035(2) 0.0159(17) -0.0080(17) -0.0126(17) O13W 0.051(3) 0.066(3) 0.046(3) 0.007(2) -0.029(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O9 1.983(4) 8_666 ? Cu1 O9 1.983(4) 3_655 ? Cu1 O3 1.989(4) . ? Cu1 O3 1.989(4) 6_556 ? Cu1 O1W 2.134(7) . ? Cu1 Cu2 2.6485(11) . ? Cu2 O10 1.931(4) 8_666 ? Cu2 O10 1.931(4) 3_655 ? Cu2 O4 1.932(5) . ? Cu2 O4 1.932(5) 6_556 ? Cu2 O2W 2.164(7) . ? Cu3 O11 1.961(4) 5 ? Cu3 O5 1.961(4) 1_455 ? Cu3 O12 1.961(4) . ? Cu3 O6 1.963(4) 5_655 ? Cu3 O13W 2.142(4) . ? Cu3 Cu3 2.6523(11) 5 ? C1 O3 1.252(7) . ? C1 O4 1.257(7) . ? C1 C2 1.500(8) . ? C2 C7 1.397(8) . ? C2 C3 1.401(8) . ? C3 C4 1.384(8) . ? C3 H3 0.9300 . ? C4 O7 1.355(7) . ? C4 C5 1.386(8) . ? C5 C6 1.398(7) . ? C5 H5 0.9300 . ? C6 C7 1.399(7) . ? C6 C8 1.499(7) . ? C7 H7 0.9300 . ? C8 O5 1.252(7) . ? C8 O6 1.255(7) . ? C9 O7 1.431(7) . ? C9 C10 1.532(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.526(7) 3 ? C10 C11 1.526(7) . ? C10 C9 1.532(7) 3 ? C11 O8 1.437(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O8 1.358(7) . ? C12 C17 1.387(8) . ? C12 C13 1.393(7) . ? C13 C14 1.391(8) . ? C13 H13 0.9300 . ? C14 C15 1.387(8) . ? C14 C18 1.513(7) . ? C15 C16 1.395(8) . ? C15 H15 0.9300 . ? C16 C17 1.389(8) . ? C16 C19 1.505(7) . ? C17 H17 0.9300 . ? C18 O9 1.245(7) . ? C18 O10 1.262(7) . ? C19 O11 1.249(7) . ? C19 O12 1.263(7) . ? O5 Cu3 1.961(4) 1_655 ? O6 Cu3 1.963(4) 5_655 ? O9 Cu1 1.983(4) 3_455 ? O10 Cu2 1.931(4) 3_455 ? O11 Cu3 1.961(4) 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 O9 Cu1 O9 91.7(2) 8_666 3_655 ? O9 Cu1 O3 168.01(17) 8_666 . ? O9 Cu1 O3 88.76(17) 3_655 . ? O9 Cu1 O3 88.76(17) 8_666 6_556 ? O9 Cu1 O3 168.01(17) 3_655 6_556 ? O3 Cu1 O3 88.3(3) . 6_556 ? O9 Cu1 O1W 96.4(2) 8_666 . ? O9 Cu1 O1W 96.4(2) 3_655 . ? O3 Cu1 O1W 95.5(2) . . ? O3 Cu1 O1W 95.4(2) 6_556 . ? O9 Cu1 Cu2 84.23(11) 8_666 . ? O9 Cu1 Cu2 84.23(11) 3_655 . ? O3 Cu1 Cu2 83.90(12) . . ? O3 Cu1 Cu2 83.90(12) 6_556 . ? O1W Cu1 Cu2 179.1(2) . . ? O10 Cu2 O10 90.3(4) 8_666 3_655 ? O10 Cu2 O4 167.8(2) 8_666 . ? O10 Cu2 O4 88.6(3) 3_655 . ? O10 Cu2 O4 88.6(3) 8_666 6_556 ? O10 Cu2 O4 167.8(2) 3_655 6_556 ? O4 Cu2 O4 90.0(4) . 6_556 ? O10 Cu2 O2W 95.4(2) 8_666 . ? O10 Cu2 O2W 95.4(2) 3_655 . ? O4 Cu2 O2W 96.8(2) . . ? O4 Cu2 O2W 96.8(2) 6_556 . ? O10 Cu2 Cu1 83.69(14) 8_666 . ? O10 Cu2 Cu1 83.69(14) 3_655 . ? O4 Cu2 Cu1 84.12(13) . . ? O4 Cu2 Cu1 84.12(13) 6_556 . ? O2W Cu2 Cu1 178.7(2) . . ? O11 Cu3 O5 89.9(2) 5 1_455 ? O11 Cu3 O12 168.00(17) 5 . ? O5 Cu3 O12 87.9(2) 1_455 . ? O11 Cu3 O6 89.3(2) 5 5_655 ? O5 Cu3 O6 167.86(16) 1_455 5_655 ? O12 Cu3 O6 90.4(2) . 5_655 ? O11 Cu3 O13W 93.4(2) 5 . ? O5 Cu3 O13W 98.6(2) 1_455 . ? O12 Cu3 O13W 98.6(2) . . ? O6 Cu3 O13W 93.6(2) 5_655 . ? O11 Cu3 Cu3 80.79(12) 5 5 ? O5 Cu3 Cu3 85.74(12) 1_455 5 ? O12 Cu3 Cu3 87.29(12) . 5 ? O6 Cu3 Cu3 82.18(11) 5_655 5 ? O13W Cu3 Cu3 172.83(17) . 5 ? O3 C1 O4 126.4(5) . . ? O3 C1 C2 117.7(5) . . ? O4 C1 C2 115.8(5) . . ? C7 C2 C3 120.1(5) . . ? C7 C2 C1 121.3(5) . . ? C3 C2 C1 118.6(5) . . ? C4 C3 C2 120.3(5) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? O7 C4 C3 113.9(5) . . ? O7 C4 C5 125.8(5) . . ? C3 C4 C5 120.2(5) . . ? C4 C5 C6 119.8(5) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 120.5(5) . . ? C5 C6 C8 119.5(5) . . ? C7 C6 C8 119.8(5) . . ? C2 C7 C6 119.1(5) . . ? C2 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? O5 C8 O6 126.6(5) . . ? O5 C8 C6 117.1(5) . . ? O6 C8 C6 116.2(5) . . ? O7 C9 C10 106.9(4) . . ? O7 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O7 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? C11 C10 C11 111.2(6) 3 . ? C11 C10 C9 108.9(3) 3 3 ? C11 C10 C9 109.1(3) . 3 ? C11 C10 C9 109.1(3) 3 . ? C11 C10 C9 108.9(3) . . ? C9 C10 C9 109.6(6) 3 . ? O8 C11 C10 106.3(4) . . ? O8 C11 H11A 110.5 . . ? C10 C11 H11A 110.5 . . ? O8 C11 H11B 110.5 . . ? C10 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? O8 C12 C17 114.8(5) . . ? O8 C12 C13 124.9(5) . . ? C17 C12 C13 120.4(5) . . ? C14 C13 C12 118.8(5) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 121.5(5) . . ? C15 C14 C18 117.6(5) . . ? C13 C14 C18 120.8(5) . . ? C14 C15 C16 119.0(5) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 120.2(5) . . ? C17 C16 C19 120.2(5) . . ? C15 C16 C19 119.3(5) . . ? C12 C17 C16 120.1(5) . . ? C12 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? O9 C18 O10 126.3(5) . . ? O9 C18 C14 118.5(5) . . ? O10 C18 C14 115.0(5) . . ? O11 C19 O12 126.8(5) . . ? O11 C19 C16 116.3(5) . . ? O12 C19 C16 116.9(5) . . ? C1 O3 Cu1 121.5(4) . . ? C1 O4 Cu2 124.0(4) . . ? C8 O5 Cu3 120.6(4) . 1_655 ? C8 O6 Cu3 124.6(3) . 5_655 ? C4 O7 C9 118.2(4) . . ? C12 O8 C11 118.4(4) . . ? C18 O9 Cu1 121.2(3) . 3_455 ? C18 O10 Cu2 124.0(4) . 3_455 ? C19 O11 Cu3 126.5(4) . 5 ? C19 O12 Cu3 118.5(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.136 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.248 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 -0.125 0.011 0.163 5288.0 3877.8 _platon_squeeze_details ; ; #### data_Zn _publ_contact_author_name 'Zujin Lin' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China ; _publ_contact_author_email linzujin@fjirsm.ac.cn _publ_contact_author_phone 86-591-83725186 _publ_contact_author_fax 86-591-83796710 loop_ _publ_author_name _publ_author_address 'Lin, Zujin' ; State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H20 O24 Zn4' _chemical_formula_weight 1110.01 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4105(5) _cell_length_b 26.2172(12) _cell_length_c 26.2215(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8531.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22415 _cell_measurement_theta_min 3.2031 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 1.156 _exptl_absorpt_correction_type 'Multi-Scan' _exptl_absorpt_correction_T_min 0.6877 _exptl_absorpt_correction_T_max 0.8189 _exptl_absorpt_process_details ? _exptl_special_details ; The structure contains disordered solvents. Because it was difficult to refine a xonsisten disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. (see more at the bottom of this .cif file) ; _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66227 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10222 _reflns_number_gt 9244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1659P)^2^+6.0418P] 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 10222 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.2488 _refine_ls_wR_factor_gt 0.2367 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 1.15408(7) 0.22118(3) 0.2500 0.0389(2) Uani 1 2 d S . . Zn2 Zn 0.98713(7) 0.30297(3) 0.2500 0.0384(2) Uani 1 2 d S . . Zn3 Zn 0.08194(4) -0.00688(2) 0.04080(3) 0.04081(18) Uani 1 1 d . . . C1 C 0.9652(5) 0.2140(3) 0.1801(3) 0.0598(16) Uani 1 1 d . . . C2 C 0.9034(5) 0.1893(3) 0.1379(2) 0.0547(14) Uani 1 1 d . . . C3 C 0.8127(5) 0.2145(3) 0.1190(3) 0.0566(15) Uani 1 1 d . . . H3 H 0.7893 0.2448 0.1337 0.068 Uiso 1 1 calc R . . C4 C 0.7568(5) 0.1928(2) 0.0770(3) 0.0548(14) Uani 1 1 d . . . C5 C 0.7904(5) 0.1466(2) 0.0570(2) 0.0529(14) Uani 1 1 d . . . H5 H 0.7529 0.1317 0.0301 0.063 Uiso 1 1 calc R . . C6 C 0.8809(5) 0.1224(2) 0.0774(3) 0.0508(13) Uani 1 1 d . . . C7 C 0.9364(5) 0.1434(3) 0.1172(3) 0.0576(15) Uani 1 1 d . . . H7 H 0.9965 0.1268 0.1304 0.069 Uiso 1 1 calc R . . C8 C 0.9211(4) 0.0737(2) 0.0518(3) 0.0520(13) Uani 1 1 d . . . C9 C 0.6156(5) 0.2053(2) 0.0164(2) 0.0513(13) Uani 1 1 d . . . H9A H 0.5714 0.1759 0.0247 0.062 Uiso 1 1 calc R . . H9B H 0.6649 0.1959 -0.0107 0.062 Uiso 1 1 calc R . . C10 C 0.5451(5) 0.2500 0.0000 0.0441(16) Uani 1 2 d S . . C11 C 0.4738(4) 0.2325(2) -0.0447(2) 0.0492(12) Uani 1 1 d . . . H11A H 0.4247 0.2596 -0.0546 0.059 Uiso 1 1 calc R . . H11B H 0.5180 0.2237 -0.0739 0.059 Uiso 1 1 calc R . . C12 C 0.3336(5) 0.1709(2) -0.0575(2) 0.0517(13) Uani 1 1 d . . . C13 C 0.3030(5) 0.1916(3) -0.1040(2) 0.0548(14) Uani 1 1 d . . . H13 H 0.3407 0.2188 -0.1181 0.066 Uiso 1 1 calc R . . C14 C 0.2137(5) 0.1705(3) -0.1294(2) 0.0552(14) Uani 1 1 d . . . C15 C 0.1584(5) 0.1294(3) -0.1088(3) 0.0598(15) Uani 1 1 d . . . H15 H 0.0994 0.1157 -0.1259 0.072 Uiso 1 1 calc R . . C16 C 0.1913(5) 0.1085(2) -0.0622(3) 0.0568(14) Uani 1 1 d . . . C17 C 0.2793(5) 0.1289(2) -0.0368(3) 0.0560(14) Uani 1 1 d . . . H17 H 0.3021 0.1149 -0.0061 0.067 Uiso 1 1 calc R . . C18 C 0.1719(5) 0.1945(3) -0.1777(2) 0.0558(14) Uani 1 1 d . . . C19 C 0.1289(5) 0.0656(3) -0.0384(3) 0.0582(15) Uani 1 1 d . . . O1W O 1.2573(7) 0.1634(4) 0.2500 0.119(4) Uani 1 2 d S . . O2W O 0.8812(9) 0.3594(4) 0.2500 0.139(5) Uani 1 2 d S . . O3 O 1.0485(4) 0.1944(2) 0.19612(18) 0.0638(12) Uani 1 1 d . . . O4 O 0.9256(4) 0.2563(2) 0.1966(2) 0.0757(7) Uani 1 1 d . . . O5 O 1.0001(4) 0.0519(2) 0.0729(2) 0.0757(7) Uani 1 1 d . . . O6 O 0.8750(4) 0.06057(19) 0.0119(2) 0.0678(13) Uani 1 1 d . . . O7 O 0.6744(4) 0.22205(19) 0.0606(2) 0.0731(16) Uani 1 1 d . . . O8 O 0.4154(4) 0.1895(2) -0.02777(19) 0.0696(14) Uani 1 1 d . . . O9 O 0.2164(4) 0.23303(19) -0.19426(17) 0.0611(11) Uani 1 1 d . . . O10 O 0.0906(4) 0.1725(2) -0.1973(2) 0.0757(7) Uani 1 1 d . . . O11 O 0.0426(5) 0.0533(2) -0.0602(2) 0.0757(7) Uani 1 1 d . . . O12 O 0.1669(5) 0.0450(2) 0.0016(2) 0.0757(7) Uani 1 1 d . . . O13W O 0.1839(5) -0.0273(2) 0.0947(2) 0.0866(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0348(4) 0.0458(5) 0.0361(4) 0.000 0.000 0.0074(3) Zn2 0.0356(4) 0.0432(5) 0.0363(4) 0.000 0.000 0.0076(3) Zn3 0.0383(3) 0.0374(3) 0.0467(4) 0.0002(2) -0.0119(2) -0.0013(2) C1 0.049(3) 0.071(4) 0.059(4) -0.009(3) -0.011(3) 0.000(3) C2 0.049(3) 0.063(4) 0.052(3) -0.009(3) -0.008(3) 0.002(3) C3 0.051(3) 0.059(3) 0.060(3) -0.017(3) -0.013(3) 0.006(3) C4 0.052(3) 0.052(3) 0.060(3) -0.012(3) -0.016(3) 0.010(3) C5 0.046(3) 0.052(3) 0.060(3) -0.014(3) -0.017(3) 0.011(2) C6 0.045(3) 0.048(3) 0.060(3) -0.014(3) -0.008(2) 0.005(2) C7 0.051(3) 0.068(4) 0.054(3) -0.006(3) -0.013(3) 0.009(3) C8 0.044(3) 0.043(3) 0.069(4) -0.010(3) -0.007(3) 0.007(2) C9 0.045(3) 0.048(3) 0.061(3) -0.013(2) -0.016(2) 0.005(2) C10 0.031(3) 0.051(4) 0.050(4) 0.002(3) 0.000 0.000 C11 0.043(2) 0.053(3) 0.052(3) 0.015(3) -0.008(2) -0.011(2) C12 0.047(3) 0.056(3) 0.052(3) 0.016(3) -0.012(2) -0.015(2) C13 0.048(3) 0.059(3) 0.057(3) 0.020(3) -0.011(3) -0.013(3) C14 0.052(3) 0.066(4) 0.047(3) 0.010(3) -0.009(2) -0.008(3) C15 0.051(3) 0.062(4) 0.067(4) 0.005(3) -0.012(3) -0.015(3) C16 0.060(3) 0.048(3) 0.062(4) 0.005(3) -0.003(3) -0.012(3) C17 0.059(3) 0.050(3) 0.059(3) 0.017(3) -0.012(3) -0.011(3) C18 0.059(3) 0.065(4) 0.043(3) 0.009(3) -0.011(3) 0.001(3) C19 0.054(3) 0.057(3) 0.064(4) -0.005(3) -0.003(3) -0.017(3) O1W 0.063(5) 0.079(6) 0.216(13) 0.000 0.000 0.032(4) O2W 0.085(6) 0.066(6) 0.266(16) 0.000 0.000 0.038(5) O3 0.054(2) 0.085(3) 0.053(2) -0.013(2) -0.013(2) -0.009(2) O4 0.0748(15) 0.0690(16) 0.0833(17) -0.0014(12) -0.0202(13) -0.0046(11) O5 0.0748(15) 0.0690(16) 0.0833(17) -0.0014(12) -0.0202(13) -0.0046(11) O6 0.074(3) 0.057(3) 0.073(3) -0.024(2) -0.014(2) 0.013(2) O7 0.062(3) 0.074(3) 0.084(3) -0.037(3) -0.035(3) 0.032(2) O8 0.068(3) 0.072(3) 0.069(3) 0.031(2) -0.031(2) -0.034(2) O9 0.062(2) 0.076(3) 0.045(2) 0.010(2) -0.007(2) 0.009(2) O10 0.0748(15) 0.0690(16) 0.0833(17) -0.0014(12) -0.0202(13) -0.0046(11) O11 0.0748(15) 0.0690(16) 0.0833(17) -0.0014(12) -0.0202(13) -0.0046(11) O12 0.0748(15) 0.0690(16) 0.0833(17) -0.0014(12) -0.0202(13) -0.0046(11) O13W 0.088(4) 0.090(4) 0.082(4) 0.009(3) -0.046(3) 0.007(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 Zn1 O1W 1.983(8) . ? Zn1 O9 2.043(4) 8_666 ? Zn1 O9 2.043(4) 3_655 ? Zn1 O3 2.051(4) . ? Zn1 O3 2.051(4) 6_556 ? Zn1 Zn2 2.9818(11) . ? Zn2 O2W 1.979(8) . ? Zn2 O10 1.993(5) 8_666 ? Zn2 O10 1.993(5) 3_655 ? Zn2 O4 2.011(6) . ? Zn2 O4 2.011(6) 6_556 ? Zn3 O13W 1.972(5) . ? Zn3 O12 2.005(6) . ? Zn3 O5 2.029(6) 1_455 ? Zn3 O11 2.033(6) 5 ? Zn3 O6 2.043(4) 5_655 ? Zn3 Zn3 2.9741(11) 5 ? C1 O3 1.228(8) . ? C1 O4 1.288(9) . ? C1 C2 1.493(8) . ? C2 C7 1.381(9) . ? C2 C3 1.396(9) . ? C3 C4 1.419(8) . ? C3 H3 0.9300 . ? C4 O7 1.349(7) . ? C4 C5 1.386(8) . ? C5 C6 1.395(8) . ? C5 H5 0.9300 . ? C6 C7 1.367(8) . ? C6 C8 1.527(8) . ? C7 H7 0.9300 . ? C8 O6 1.242(8) . ? C8 O5 1.262(8) . ? C9 O7 1.437(7) . ? C9 C10 1.526(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C9 1.526(7) 3 ? C10 C11 1.539(7) . ? C10 C11 1.539(7) 3 ? C11 O8 1.412(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O8 1.370(7) . ? C12 C13 1.387(8) . ? C12 C17 1.400(8) . ? C13 C14 1.405(8) . ? C13 H13 0.9300 . ? C14 C15 1.388(9) . ? C14 C18 1.506(8) . ? C15 C16 1.399(9) . ? C15 H15 0.9300 . ? C16 C17 1.387(8) . ? C16 C19 1.501(8) . ? C17 H17 0.9300 . ? C18 O9 1.230(8) . ? C18 O10 1.270(8) . ? C19 O11 1.256(8) . ? C19 O12 1.270(9) . ? O5 Zn3 2.029(6) 1_655 ? O6 Zn3 2.043(4) 5_655 ? O9 Zn1 2.043(4) 3_455 ? O10 Zn2 1.993(5) 3_455 ? O11 Zn3 2.033(6) 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 O1W Zn1 O9 101.8(3) . 8_666 ? O1W Zn1 O9 101.8(3) . 3_655 ? O9 Zn1 O9 91.3(3) 8_666 3_655 ? O1W Zn1 O3 98.7(3) . . ? O9 Zn1 O3 159.3(2) 8_666 . ? O9 Zn1 O3 87.2(2) 3_655 . ? O1W Zn1 O3 98.7(3) . 6_556 ? O9 Zn1 O3 87.2(2) 8_666 6_556 ? O9 Zn1 O3 159.3(2) 3_655 6_556 ? O3 Zn1 O3 87.1(3) . 6_556 ? O1W Zn1 Zn2 176.2(3) . . ? O9 Zn1 Zn2 80.81(15) 8_666 . ? O9 Zn1 Zn2 80.81(15) 3_655 . ? O3 Zn1 Zn2 78.60(15) . . ? O3 Zn1 Zn2 78.60(15) 6_556 . ? O2W Zn2 O10 100.8(3) . 8_666 ? O2W Zn2 O10 100.8(3) . 3_655 ? O10 Zn2 O10 87.8(4) 8_666 3_655 ? O2W Zn2 O4 101.7(3) . . ? O10 Zn2 O4 157.5(2) 8_666 . ? O10 Zn2 O4 87.6(2) 3_655 . ? O2W Zn2 O4 101.7(3) . 6_556 ? O10 Zn2 O4 87.6(2) 8_666 6_556 ? O10 Zn2 O4 157.5(2) 3_655 6_556 ? O4 Zn2 O4 88.3(3) . 6_556 ? O2W Zn2 Zn1 177.6(4) . . ? O10 Zn2 Zn1 77.52(17) 8_666 . ? O10 Zn2 Zn1 77.52(17) 3_655 . ? O4 Zn2 Zn1 79.98(16) . . ? O4 Zn2 Zn1 79.98(16) 6_556 . ? O13W Zn3 O12 102.3(2) . . ? O13W Zn3 O5 103.3(2) . 1_455 ? O12 Zn3 O5 87.7(2) . 1_455 ? O13W Zn3 O11 98.4(2) . 5 ? O12 Zn3 O11 159.2(2) . 5 ? O5 Zn3 O11 88.3(2) 1_455 5 ? O13W Zn3 O6 97.5(2) . 5_655 ? O12 Zn3 O6 89.1(2) . 5_655 ? O5 Zn3 O6 159.2(2) 1_455 5_655 ? O11 Zn3 O6 87.4(2) 5 5_655 ? O13W Zn3 Zn3 171.07(19) . 5 ? O12 Zn3 Zn3 84.77(15) . 5 ? O5 Zn3 Zn3 82.20(15) 1_455 5 ? O11 Zn3 Zn3 74.48(16) 5 5 ? O6 Zn3 Zn3 77.05(15) 5_655 5 ? O3 C1 O4 124.5(6) . . ? O3 C1 C2 120.3(6) . . ? O4 C1 C2 115.2(6) . . ? C7 C2 C3 120.8(6) . . ? C7 C2 C1 121.0(6) . . ? C3 C2 C1 118.2(6) . . ? C2 C3 C4 118.7(6) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? O7 C4 C5 127.2(5) . . ? O7 C4 C3 113.0(5) . . ? C5 C4 C3 119.8(5) . . ? C4 C5 C6 119.6(5) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 121.0(6) . . ? C7 C6 C8 120.5(5) . . ? C5 C6 C8 118.4(5) . . ? C6 C7 C2 120.1(6) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? O6 C8 O5 127.1(6) . . ? O6 C8 C6 116.8(5) . . ? O5 C8 C6 116.1(6) . . ? O7 C9 C10 106.4(4) . . ? O7 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 . . ? O7 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? C9 C10 C9 110.0(6) 3 . ? C9 C10 C11 110.1(3) 3 . ? C9 C10 C11 108.4(3) . . ? C9 C10 C11 108.4(3) 3 3 ? C9 C10 C11 110.1(3) . 3 ? C11 C10 C11 109.7(6) . 3 ? O8 C11 C10 107.1(4) . . ? O8 C11 H11A 110.3 . . ? C10 C11 H11A 110.3 . . ? O8 C11 H11B 110.3 . . ? C10 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? O8 C12 C13 124.4(5) . . ? O8 C12 C17 114.5(5) . . ? C13 C12 C17 121.1(5) . . ? C12 C13 C14 118.6(5) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 120.7(6) . . ? C15 C14 C18 118.8(6) . . ? C13 C14 C18 120.4(6) . . ? C14 C15 C16 120.0(6) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 119.8(6) . . ? C17 C16 C19 119.7(6) . . ? C15 C16 C19 120.4(6) . . ? C16 C17 C12 119.8(6) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? O9 C18 O10 125.8(6) . . ? O9 C18 C14 119.0(6) . . ? O10 C18 C14 115.1(6) . . ? O11 C19 O12 125.7(6) . . ? O11 C19 C16 116.2(6) . . ? O12 C19 C16 118.1(6) . . ? C1 O3 Zn1 129.1(5) . . ? C1 O4 Zn2 127.8(4) . . ? C8 O5 Zn3 123.4(5) . 1_655 ? C8 O6 Zn3 129.8(4) . 5_655 ? C4 O7 C9 117.9(5) . . ? C12 O8 C11 119.0(4) . . ? C18 O9 Zn1 124.4(4) . 3_455 ? C18 O10 Zn2 130.3(5) . 3_455 ? C19 O11 Zn3 133.5(5) . 5 ? C19 O12 Zn3 121.1(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.401 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.184 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.451 -0.023 0.003 5443.4 3773.5 _platon_squeeze_details ; ; #### data_Cd _publ_contact_author_name 'Zujin Lin' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China ; _publ_contact_author_email linzujin@fjirsm.ac.cn _publ_contact_author_phone +86-591-83725186 _publ_contact_author_fax +86-591-83796710 loop_ _publ_author_name _publ_author_address 'Lin, Zujin' ; State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H62 Cd4 N6 O26' _chemical_formula_weight 1672.71 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 18.326(4) _cell_length_b 19.033(4) _cell_length_c 12.529(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4370.0(16) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 14107 _cell_measurement_theta_min 2.1348 _cell_measurement_theta_max 27.4855 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7840 _exptl_absorpt_correction_T_max 0.8373 _exptl_absorpt_process_details ? _exptl_special_details ; The structure contains disordered solvents. Because it was difficult to refine a xonsisten disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. (see more at the bottom of this .cif file) ; _diffrn_ambient_temperature 113(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 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 5608 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33111 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9789 _reflns_number_gt 9500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0735P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.24(3) _refine_ls_number_reflns 9789 _refine_ls_number_parameters 463 _refine_ls_number_restraints 1001 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.075 _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 Cd1 Cd 0.728797(14) 0.748422(15) 0.38038(2) 0.01596(8) Uani 1 1 d . . . Cd2 Cd 0.825961(16) 0.663273(15) 0.55800(2) 0.01756(9) Uani 1 1 d U . . O1 O 0.2739(2) 0.36268(17) 1.3303(3) 0.0342(9) Uani 1 1 d . . . O2 O 0.20843(19) 0.42415(17) 1.4495(3) 0.0310(8) Uani 1 1 d . . . O3 O 0.6275(2) 0.7390(2) 0.4786(3) 0.0332(8) Uani 1 1 d . . . O4 O 0.7004(2) 0.6736(2) 0.5805(3) 0.0392(10) Uani 1 1 d . . . O5 O 0.3340(3) 0.73091(17) 1.3709(3) 0.0411(10) Uani 1 1 d . . . O6 O 0.2665(2) 0.67457(18) 1.4952(3) 0.0323(8) Uani 1 1 d . . . O7 O 0.3739(2) 0.7840(2) 0.5931(4) 0.0387(9) Uani 1 1 d . . . O8 O 0.3249(2) 0.7162(2) 0.7161(3) 0.0360(8) Uani 1 1 d . . . O9 O 0.4156(3) 0.5463(2) 1.1249(4) 0.0531(14) Uani 1 1 d . . . O10 O 0.5404(2) 0.5800(3) 0.8660(3) 0.0519(14) Uani 1 1 d . . . C1 C 0.6396(3) 0.7019(3) 0.5596(5) 0.0322(11) Uani 1 1 d . . . C2 C 0.5777(3) 0.6878(3) 0.6337(5) 0.0350(12) Uani 1 1 d . . . C3 C 0.5859(3) 0.6420(4) 0.7193(5) 0.0409(15) Uani 1 1 d . . . H3A H 0.6319 0.6206 0.7320 0.049 Uiso 1 1 calc R . . C4 C 0.5286(3) 0.6274(4) 0.7854(5) 0.0439(17) Uani 1 1 d . . . C5 C 0.4612(3) 0.6612(4) 0.7711(4) 0.0397(14) Uani 1 1 d . . . H5A H 0.4221 0.6529 0.8191 0.048 Uiso 1 1 calc R . . C6 C 0.4524(3) 0.7076(3) 0.6847(4) 0.0324(11) Uani 1 1 d . . . C7 C 0.5109(3) 0.7204(3) 0.6158(4) 0.0310(11) Uani 1 1 d . . . H7A H 0.5050 0.7514 0.5570 0.037 Uiso 1 1 calc R . . C8 C 0.4805(3) 0.5635(3) 0.9330(4) 0.0315(11) Uani 1 1 d . . . H8A H 0.4385 0.5532 0.8900 0.038 Uiso 1 1 d R . . H8B H 0.4690 0.6027 0.9782 0.038 Uiso 1 1 d R . . C9 C 0.3785(3) 0.7391(3) 0.6636(4) 0.0332(12) Uani 1 1 d . . . C10 C 0.2536(3) 0.4189(2) 1.3741(4) 0.0263(10) Uani 1 1 d . . . C11 C 0.2885(3) 0.4853(2) 1.3339(4) 0.0301(11) Uani 1 1 d . . . C12 C 0.2778(3) 0.5483(3) 1.3868(4) 0.0308(11) Uani 1 1 d . . . H12A H 0.2467 0.5501 1.4474 0.037 Uiso 1 1 calc R . . C13 C 0.3124(3) 0.6089(2) 1.3509(5) 0.0328(12) Uani 1 1 d . . . C14 C 0.3567(4) 0.6062(3) 1.2616(4) 0.0355(13) Uani 1 1 d . . . H14A H 0.3801 0.6475 1.2364 0.043 Uiso 1 1 calc R . . C15 C 0.3667(4) 0.5430(3) 1.2096(5) 0.0413(15) Uani 1 1 d . . . C16 C 0.3341(4) 0.4816(2) 1.2441(4) 0.0344(12) Uani 1 1 d . . . H16A H 0.3422 0.4383 1.2082 0.041 Uiso 1 1 calc R . . C17 C 0.3034(3) 0.6773(2) 1.4122(5) 0.0341(13) Uani 1 1 d . . . C18 C 0.4336(3) 0.4820(2) 1.0712(4) 0.0303(11) Uani 1 1 d . . . H18A H 0.3924 0.4659 1.0262 0.036 Uiso 1 1 calc R . . H18B H 0.4456 0.4446 1.1233 0.036 Uiso 1 1 calc R . . C19 C 0.5000 0.5000 1.0025(5) 0.0221(13) Uani 1 2 d S . . O11 O 0.6554(2) 0.7929(3) 0.2517(4) 0.0537(10) Uani 1 1 d DU . . N1 N 0.5403(5) 0.8099(7) 0.1905(8) 0.0643(14) Uani 0.582(9) 1 d PDU A 1 C20 C 0.5883(4) 0.7784(11) 0.2565(10) 0.0597(11) Uani 0.582(9) 1 d PDU A 1 H20A H 0.5714 0.7449 0.3070 0.072 Uiso 0.582(9) 1 calc PR A 1 C21 C 0.4633(5) 0.7975(9) 0.2011(11) 0.0644(15) Uani 0.582(9) 1 d PDU A 1 H21A H 0.4537 0.7732 0.2686 0.097 Uiso 0.582(9) 1 calc PR A 1 H21B H 0.4464 0.7684 0.1415 0.097 Uiso 0.582(9) 1 calc PR A 1 H21C H 0.4374 0.8425 0.2004 0.097 Uiso 0.582(9) 1 calc PR A 1 C22 C 0.5611(7) 0.8223(9) 0.0805(8) 0.0698(15) Uani 0.582(9) 1 d PDU A 1 H22A H 0.6143 0.8270 0.0757 0.105 Uiso 0.582(9) 1 calc PR A 1 H22B H 0.5380 0.8656 0.0550 0.105 Uiso 0.582(9) 1 calc PR A 1 H22C H 0.5451 0.7827 0.0363 0.105 Uiso 0.582(9) 1 calc PR A 1 N1B N 0.5463(6) 0.7707(9) 0.1634(10) 0.0609(15) Uani 0.418(9) 1 d PDU A 2 C20B C 0.5879(5) 0.7826(16) 0.2503(12) 0.0597(11) Uani 0.418(9) 1 d PDU A 2 H20B H 0.5636 0.7833 0.3172 0.072 Uiso 0.418(9) 1 calc PR A 2 C21B C 0.4688(6) 0.7600(12) 0.1764(14) 0.0644(15) Uani 0.418(9) 1 d PDU A 2 H21D H 0.4581 0.7492 0.2513 0.097 Uiso 0.418(9) 1 calc PR A 2 H21E H 0.4529 0.7207 0.1313 0.097 Uiso 0.418(9) 1 calc PR A 2 H21F H 0.4426 0.8027 0.1554 0.097 Uiso 0.418(9) 1 calc PR A 2 C22B C 0.5749(10) 0.7302(11) 0.0756(13) 0.0698(15) Uani 0.418(9) 1 d PDU A 2 H22D H 0.6282 0.7337 0.0749 0.105 Uiso 0.418(9) 1 calc PR A 2 H22E H 0.5553 0.7485 0.0084 0.105 Uiso 0.418(9) 1 calc PR A 2 H22F H 0.5605 0.6809 0.0840 0.105 Uiso 0.418(9) 1 calc PR A 2 O12 O 0.9428(2) 0.6201(3) 0.5712(4) 0.0536(8) Uani 1 1 d DU . . N2 N 1.0449(4) 0.5828(5) 0.4775(6) 0.0609(11) Uani 0.698(9) 1 d PDU B 1 C23 C 0.9766(5) 0.6088(9) 0.4849(7) 0.0609(11) Uani 0.698(9) 1 d PDU B 1 H23A H 0.9520 0.6194 0.4202 0.073 Uiso 0.698(9) 1 calc PR B 1 C24 C 1.0882(5) 0.5711(6) 0.5705(8) 0.0601(14) Uani 0.698(9) 1 d PDU B 1 H24A H 1.0569 0.5722 0.6339 0.090 Uiso 0.698(9) 1 calc PR B 1 H24B H 1.1254 0.6079 0.5761 0.090 Uiso 0.698(9) 1 calc PR B 1 H24C H 1.1120 0.5251 0.5654 0.090 Uiso 0.698(9) 1 calc PR B 1 C25 C 1.0846(6) 0.5808(7) 0.3806(8) 0.0699(15) Uani 0.698(9) 1 d PDU B 1 H25A H 1.0515 0.5895 0.3207 0.105 Uiso 0.698(9) 1 calc PR B 1 H25B H 1.1073 0.5345 0.3722 0.105 Uiso 0.698(9) 1 calc PR B 1 H25C H 1.1226 0.6171 0.3818 0.105 Uiso 0.698(9) 1 calc PR B 1 N2B N 1.0454(8) 0.5751(11) 0.5443(12) 0.0609(11) Uani 0.302(9) 1 d PDU B 2 C23B C 0.9886(10) 0.610(2) 0.5002(11) 0.0609(11) Uani 0.302(9) 1 d PDU B 2 H23B H 0.9845 0.6241 0.4277 0.073 Uiso 0.302(9) 1 calc PR B 2 C24B C 1.0509(12) 0.5678(15) 0.6577(13) 0.0601(14) Uani 0.302(9) 1 d PDU B 2 H24D H 1.0019 0.5681 0.6891 0.090 Uiso 0.302(9) 1 calc PR B 2 H24E H 1.0794 0.6068 0.6868 0.090 Uiso 0.302(9) 1 calc PR B 2 H24F H 1.0751 0.5232 0.6748 0.090 Uiso 0.302(9) 1 calc PR B 2 C25B C 1.1151(8) 0.5756(17) 0.4925(19) 0.0699(15) Uani 0.302(9) 1 d PDU B 2 H25D H 1.1087 0.5870 0.4168 0.105 Uiso 0.302(9) 1 calc PR B 2 H25E H 1.1378 0.5291 0.4993 0.105 Uiso 0.302(9) 1 calc PR B 2 H25F H 1.1465 0.6109 0.5261 0.105 Uiso 0.302(9) 1 calc PR B 2 O13 O 0.8131(3) 0.5967(3) 0.7083(4) 0.0544(9) Uani 1 1 d DU . . N3 N 0.7747(7) 0.5021(6) 0.7957(9) 0.0604(14) Uani 0.524(9) 1 d PDU B 1 C26 C 0.7732(11) 0.5449(8) 0.7117(11) 0.0587(11) Uani 0.524(9) 1 d PDU B 1 H26A H 0.7410 0.5353 0.6540 0.070 Uiso 0.524(9) 1 calc PR B 1 C27 C 0.7303(9) 0.4414(6) 0.8043(13) 0.0647(15) Uani 0.524(9) 1 d PDU B 1 H27A H 0.7009 0.4363 0.7394 0.097 Uiso 0.524(9) 1 calc PR B 1 H27B H 0.6980 0.4460 0.8662 0.097 Uiso 0.524(9) 1 calc PR B 1 H27C H 0.7613 0.3999 0.8131 0.097 Uiso 0.524(9) 1 calc PR B 1 C28 C 0.8266(9) 0.5097(8) 0.8799(11) 0.0689(15) Uani 0.524(9) 1 d PDU B 1 H28A H 0.8613 0.5470 0.8616 0.103 Uiso 0.524(9) 1 calc PR B 1 H28B H 0.8529 0.4654 0.8898 0.103 Uiso 0.524(9) 1 calc PR B 1 H28C H 0.8011 0.5220 0.9461 0.103 Uiso 0.524(9) 1 calc PR B 1 N3B N 0.7466(8) 0.5026(6) 0.7632(9) 0.0595(15) Uani 0.476(9) 1 d PDU B 2 C26B C 0.7731(12) 0.5453(9) 0.6883(10) 0.0587(11) Uani 0.476(9) 1 d PDU B 2 H26B H 0.7611 0.5360 0.6159 0.070 Uiso 0.476(9) 1 calc PR B 2 C27B C 0.7135(10) 0.4370(6) 0.7414(13) 0.0647(15) Uani 0.476(9) 1 d PDU B 2 H27D H 0.7107 0.4300 0.6641 0.097 Uiso 0.476(9) 1 calc PR B 2 H27E H 0.6642 0.4362 0.7717 0.097 Uiso 0.476(9) 1 calc PR B 2 H27F H 0.7427 0.3993 0.7734 0.097 Uiso 0.476(9) 1 calc PR B 2 C28B C 0.7528(11) 0.5182(9) 0.8745(9) 0.0689(15) Uani 0.476(9) 1 d PDU B 2 H28D H 0.7670 0.5675 0.8836 0.103 Uiso 0.476(9) 1 calc PR B 2 H28E H 0.7898 0.4877 0.9067 0.103 Uiso 0.476(9) 1 calc PR B 2 H28F H 0.7057 0.5101 0.9095 0.103 Uiso 0.476(9) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01270(13) 0.01522(14) 0.01995(15) 0.00193(12) -0.00178(10) -0.00225(11) Cd2 0.01485(14) 0.01365(13) 0.02417(16) 0.00177(12) -0.00652(12) -0.00015(11) O1 0.048(2) 0.0158(14) 0.039(2) -0.0003(14) 0.0156(19) -0.0064(16) O2 0.0290(17) 0.0194(14) 0.045(2) 0.0077(16) 0.0202(17) -0.0010(13) O3 0.0281(17) 0.044(2) 0.0273(17) 0.0130(16) 0.0056(14) -0.0011(17) O4 0.0186(16) 0.053(2) 0.046(2) 0.0170(19) 0.0123(15) 0.0072(17) O5 0.065(3) 0.0191(15) 0.039(2) -0.0048(14) 0.030(2) -0.0067(17) O6 0.037(2) 0.0238(16) 0.0361(19) -0.0076(14) 0.0157(17) -0.0033(16) O7 0.0272(18) 0.040(2) 0.049(2) 0.0116(18) -0.0106(16) 0.0103(16) O8 0.0167(15) 0.050(2) 0.041(2) 0.0064(17) -0.0026(16) 0.0122(17) O9 0.090(4) 0.0229(17) 0.046(2) -0.0042(17) 0.054(3) -0.004(2) O10 0.0223(18) 0.092(3) 0.041(2) 0.044(2) 0.0169(17) 0.030(2) C1 0.023(2) 0.046(3) 0.027(2) 0.010(2) 0.009(2) 0.004(2) C2 0.019(2) 0.052(3) 0.034(3) 0.016(2) 0.007(2) 0.003(2) C3 0.017(2) 0.070(4) 0.036(3) 0.022(3) 0.009(2) 0.021(3) C4 0.020(2) 0.076(4) 0.036(3) 0.038(3) 0.009(2) 0.022(3) C5 0.017(2) 0.072(4) 0.030(3) 0.027(3) 0.0039(18) 0.015(3) C6 0.022(2) 0.049(3) 0.027(2) 0.015(2) -0.0003(19) 0.009(2) C7 0.022(2) 0.043(3) 0.028(2) 0.017(2) -0.0017(19) 0.008(2) C8 0.021(2) 0.056(3) 0.017(2) 0.015(2) 0.0094(18) 0.014(2) C9 0.026(2) 0.045(3) 0.029(2) 0.006(2) -0.0052(19) 0.011(2) C10 0.030(2) 0.018(2) 0.030(2) 0.0038(19) 0.010(2) -0.0016(18) C11 0.036(3) 0.017(2) 0.037(3) 0.0031(19) 0.016(2) -0.0070(19) C12 0.041(3) 0.023(2) 0.028(2) -0.0056(19) 0.018(2) 0.001(2) C13 0.041(3) 0.018(2) 0.040(3) -0.0058(19) 0.018(2) -0.001(2) C14 0.057(4) 0.017(2) 0.033(3) 0.0005(19) 0.027(3) -0.008(2) C15 0.066(4) 0.023(2) 0.035(3) -0.008(2) 0.036(3) -0.007(3) C16 0.054(3) 0.019(2) 0.030(3) -0.0011(19) 0.023(3) -0.003(2) C17 0.045(3) 0.016(2) 0.041(3) -0.0074(19) 0.021(2) 0.002(2) C18 0.051(3) 0.024(2) 0.016(2) -0.0027(18) 0.015(2) 0.002(2) C19 0.024(3) 0.028(3) 0.014(3) 0.000 0.000 0.011(3) O11 0.0410(17) 0.070(2) 0.0500(18) 0.0191(17) -0.0077(16) 0.0027(17) N1 0.052(2) 0.074(2) 0.067(2) 0.011(2) -0.007(2) -0.001(2) C20 0.0499(17) 0.0706(19) 0.0588(18) 0.0106(17) -0.0063(16) -0.0031(17) C21 0.055(2) 0.074(2) 0.065(2) 0.007(2) -0.004(2) -0.002(2) C22 0.063(2) 0.079(2) 0.068(2) 0.008(2) -0.003(2) -0.003(2) N1B 0.052(2) 0.070(2) 0.061(2) 0.009(2) -0.005(2) -0.002(2) C20B 0.0499(17) 0.0706(19) 0.0588(18) 0.0106(17) -0.0063(16) -0.0031(17) C21B 0.055(2) 0.074(2) 0.065(2) 0.007(2) -0.004(2) -0.002(2) C22B 0.063(2) 0.079(2) 0.068(2) 0.008(2) -0.003(2) -0.003(2) O12 0.0310(12) 0.0582(16) 0.0716(18) 0.0102(16) -0.0101(15) 0.0170(13) N2 0.0464(17) 0.0637(18) 0.0725(19) 0.0035(17) -0.0032(17) 0.0098(16) C23 0.0464(18) 0.0632(18) 0.0731(19) 0.0043(17) -0.0047(17) 0.0103(17) C24 0.048(2) 0.063(2) 0.069(2) 0.003(2) -0.007(2) 0.008(2) C25 0.058(2) 0.073(2) 0.078(2) 0.001(2) -0.001(2) 0.008(2) N2B 0.0464(17) 0.0637(18) 0.0725(19) 0.0035(17) -0.0032(17) 0.0098(16) C23B 0.0464(18) 0.0632(18) 0.0731(19) 0.0043(17) -0.0047(17) 0.0103(17) C24B 0.048(2) 0.063(2) 0.069(2) 0.003(2) -0.007(2) 0.008(2) C25B 0.058(2) 0.073(2) 0.078(2) 0.001(2) -0.001(2) 0.008(2) O13 0.0534(18) 0.0525(17) 0.0574(18) 0.0218(16) -0.0042(16) 0.0046(16) N3 0.059(2) 0.059(2) 0.064(2) 0.012(2) -0.002(2) 0.003(2) C26 0.0555(17) 0.0569(17) 0.0637(18) 0.0129(16) 0.0011(17) 0.0041(16) C27 0.065(2) 0.062(2) 0.067(2) 0.010(2) 0.002(2) -0.001(2) C28 0.070(2) 0.068(2) 0.069(2) 0.009(2) 0.000(2) 0.000(2) N3B 0.058(2) 0.057(2) 0.063(2) 0.013(2) 0.001(2) 0.002(2) C26B 0.0555(17) 0.0569(17) 0.0637(18) 0.0129(16) 0.0011(17) 0.0041(16) C27B 0.065(2) 0.062(2) 0.067(2) 0.010(2) 0.002(2) -0.001(2) C28B 0.070(2) 0.068(2) 0.069(2) 0.009(2) 0.000(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.206(3) 2_664 ? Cd1 O3 2.234(4) . ? Cd1 O8 2.240(4) 3_566 ? Cd1 O6 2.248(3) 3_567 ? Cd1 O11 2.264(5) . ? Cd1 Cd2 3.2787(6) . ? Cd2 O5 2.207(3) 3_567 ? Cd2 O2 2.239(3) 2_664 ? Cd2 O13 2.282(5) . ? Cd2 O12 2.299(4) . ? Cd2 O7 2.316(4) 3_566 ? Cd2 O4 2.326(4) . ? O1 C10 1.258(6) . ? O1 Cd1 2.206(3) 2_666 ? O2 C10 1.260(6) . ? O2 Cd2 2.239(3) 2_666 ? O3 C1 1.256(7) . ? O4 C1 1.265(6) . ? O5 C17 1.275(6) . ? O5 Cd2 2.207(3) 3_467 ? O6 C17 1.241(6) . ? O6 Cd1 2.248(3) 3_467 ? O7 C9 1.232(7) . ? O7 Cd2 2.316(4) 3_466 ? O8 C9 1.260(7) . ? O8 Cd1 2.240(4) 3_466 ? O9 C15 1.390(6) . ? O9 C18 1.435(6) . ? O10 C4 1.372(6) . ? O10 C8 1.417(6) . ? C1 C2 1.490(7) . ? C2 C7 1.391(7) . ? C2 C3 1.392(8) . ? C3 C4 1.366(7) . ? C4 C5 1.404(7) . ? C5 C6 1.406(7) . ? C6 C7 1.397(7) . ? C6 C9 1.504(7) . ? C8 C19 1.532(6) . ? C10 C11 1.504(6) . ? C11 C12 1.384(7) . ? C11 C16 1.403(7) . ? C12 C13 1.391(7) . ? C13 C14 1.383(7) . ? C13 C17 1.521(6) . ? C14 C15 1.380(7) . ? C15 C16 1.383(7) . ? C18 C19 1.530(6) . ? C19 C18 1.530(6) 2_665 ? C19 C8 1.532(6) 2_665 ? O11 C20B 1.252(8) . ? O11 C20 1.261(8) . ? N1 C20 1.347(10) . ? N1 C21 1.437(8) . ? N1 C22 1.450(8) . ? N1B C20B 1.349(9) . ? N1B C22B 1.441(9) . ? N1B C21B 1.444(8) . ? O12 C23B 1.238(9) . ? O12 C23 1.265(7) . ? N2 C23 1.349(8) . ? N2 C25 1.416(8) . ? N2 C24 1.427(7) . ? N2B C23B 1.352(10) . ? N2B C24B 1.431(9) . ? N2B C25B 1.433(8) . ? O13 C26 1.228(8) . ? O13 C26B 1.247(8) . ? N3 C26 1.332(9) . ? N3 C27 1.416(8) . ? N3 C28 1.428(8) . ? N3B C26B 1.334(9) . ? N3B C27B 1.415(8) . ? N3B C28B 1.430(8) . ? 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 Cd1 O3 93.50(16) 2_664 . ? O1 Cd1 O8 98.76(16) 2_664 3_566 ? O3 Cd1 O8 167.07(15) . 3_566 ? O1 Cd1 O6 145.98(14) 2_664 3_567 ? O3 Cd1 O6 85.75(15) . 3_567 ? O8 Cd1 O6 86.35(15) 3_566 3_567 ? O1 Cd1 O11 98.18(18) 2_664 . ? O3 Cd1 O11 85.90(15) . . ? O8 Cd1 O11 88.31(16) 3_566 . ? O6 Cd1 O11 115.64(18) 3_567 . ? O1 Cd1 Cd2 74.43(10) 2_664 . ? O3 Cd1 Cd2 92.16(10) . . ? O8 Cd1 Cd2 95.04(11) 3_566 . ? O6 Cd1 Cd2 71.62(9) 3_567 . ? O11 Cd1 Cd2 172.25(14) . . ? O5 Cd2 O2 160.38(13) 3_567 2_664 ? O5 Cd2 O13 100.42(18) 3_567 . ? O2 Cd2 O13 93.38(17) 2_664 . ? O5 Cd2 O12 103.59(19) 3_567 . ? O2 Cd2 O12 92.28(16) 2_664 . ? O13 Cd2 O12 80.72(19) . . ? O5 Cd2 O7 84.76(17) 3_567 3_566 ? O2 Cd2 O7 86.15(15) 2_664 3_566 ? O13 Cd2 O7 162.64(17) . 3_566 ? O12 Cd2 O7 81.96(17) . 3_566 ? O5 Cd2 O4 86.56(18) 3_567 . ? O2 Cd2 O4 81.85(16) 2_664 . ? O13 Cd2 O4 81.05(16) . . ? O12 Cd2 O4 160.47(16) . . ? O7 Cd2 O4 115.97(14) 3_566 . ? O5 Cd2 Cd1 81.91(10) 3_567 . ? O2 Cd2 Cd1 78.61(9) 2_664 . ? O13 Cd2 Cd1 141.10(13) . . ? O12 Cd2 Cd1 136.98(13) . . ? O7 Cd2 Cd1 55.75(11) 3_566 . ? O4 Cd2 Cd1 60.22(10) . . ? C10 O1 Cd1 133.2(3) . 2_666 ? C10 O2 Cd2 125.5(3) . 2_666 ? C1 O3 Cd1 110.1(3) . . ? C1 O4 Cd2 151.9(3) . . ? C17 O5 Cd2 122.5(3) . 3_467 ? C17 O6 Cd1 136.2(3) . 3_467 ? C9 O7 Cd2 155.9(4) . 3_466 ? C9 O8 Cd1 103.1(3) . 3_466 ? C15 O9 C18 117.8(4) . . ? C4 O10 C8 117.3(4) . . ? O3 C1 O4 124.2(5) . . ? O3 C1 C2 118.0(5) . . ? O4 C1 C2 117.7(5) . . ? C7 C2 C3 119.9(5) . . ? C7 C2 C1 119.4(5) . . ? C3 C2 C1 120.7(5) . . ? C4 C3 C2 120.8(5) . . ? C3 C4 O10 117.3(4) . . ? C3 C4 C5 120.4(5) . . ? O10 C4 C5 122.3(5) . . ? C4 C5 C6 119.2(5) . . ? C7 C6 C5 119.8(5) . . ? C7 C6 C9 120.8(4) . . ? C5 C6 C9 119.2(5) . . ? C2 C7 C6 119.9(5) . . ? O10 C8 C19 109.3(3) . . ? O7 C9 O8 124.1(5) . . ? O7 C9 C6 117.6(5) . . ? O8 C9 C6 118.2(5) . . ? O1 C10 O2 126.1(4) . . ? O1 C10 C11 116.3(4) . . ? O2 C10 C11 117.6(4) . . ? C12 C11 C16 120.8(4) . . ? C12 C11 C10 120.5(4) . . ? C16 C11 C10 118.7(4) . . ? C11 C12 C13 119.9(4) . . ? C14 C13 C12 119.9(4) . . ? C14 C13 C17 120.3(5) . . ? C12 C13 C17 119.8(4) . . ? C15 C14 C13 119.5(5) . . ? C14 C15 C16 122.1(5) . . ? C14 C15 O9 114.0(5) . . ? C16 C15 O9 123.7(5) . . ? C15 C16 C11 117.7(4) . . ? O6 C17 O5 127.8(4) . . ? O6 C17 C13 116.6(4) . . ? O5 C17 C13 115.6(4) . . ? O9 C18 C19 104.7(4) . . ? C18 C19 C18 111.5(6) 2_665 . ? C18 C19 C8 109.2(3) 2_665 . ? C18 C19 C8 108.1(3) . . ? C18 C19 C8 108.1(3) 2_665 2_665 ? C18 C19 C8 109.2(3) . 2_665 ? C8 C19 C8 110.7(6) . 2_665 ? C20B O11 C20 5.1(17) . . ? C20B O11 Cd1 122.6(11) . . ? C20 O11 Cd1 117.6(6) . . ? C20 N1 C21 120.8(7) . . ? C20 N1 C22 119.0(7) . . ? C21 N1 C22 111.8(8) . . ? O11 C20 N1 120.7(10) . . ? C20B N1B C22B 120.0(8) . . ? C20B N1B C21B 119.3(8) . . ? C22B N1B C21B 111.6(8) . . ? O11 C20B N1B 126.6(12) . . ? C23B O12 C23 13.3(13) . . ? C23B O12 Cd2 129.4(8) . . ? C23 O12 Cd2 117.1(5) . . ? C23 N2 C25 123.0(6) . . ? C23 N2 C24 121.1(6) . . ? C25 N2 C24 114.2(7) . . ? O12 C23 N2 125.1(7) . . ? C23B N2B C24B 120.5(8) . . ? C23B N2B C25B 119.9(9) . . ? C24B N2B C25B 112.8(9) . . ? O12 C23B N2B 107.7(10) . . ? C26 O13 C26B 13.6(9) . . ? C26 O13 Cd2 122.4(6) . . ? C26B O13 Cd2 109.3(6) . . ? C26 N3 C27 123.2(7) . . ? C26 N3 C28 122.4(7) . . ? C27 N3 C28 114.2(7) . . ? O13 C26 N3 120.4(9) . . ? C26B N3B C27B 123.9(7) . . ? C26B N3B C28B 122.1(7) . . ? C27B N3B C28B 113.9(8) . . ? O13 C26B N3B 123.4(9) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.615 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.116 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 -0.125 0.011 0.163 5288.0 3877.8 _platon_squeeze_details ; ;