# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chang Seop Hong' _publ_contact_author_email cshong@korea.ac.kr loop_ _publ_author_name 'Chang Seop Hong' 'Woo Ram Lee' 'Dae Won Ryu' 'Won Ju Phang' 'Ji Hye Park' # Attachment '- cif-complex1-revise2.cif' data_cutpo2 _database_code_depnum_ccdc_archive 'CCDC 859100' #TrackingRef '- cif-complex1-revise2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.88 H26 Cu N O11 P' _chemical_formula_weight 597.47 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' P P 0.1023 0.0942 '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' 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 Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.0811(4) _cell_length_b 24.0918(6) _cell_length_c 14.2992(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5539.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 8338 _cell_measurement_theta_min 2.548 _cell_measurement_theta_max 28.119 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2466 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7315 _exptl_absorpt_correction_T_max 0.7905 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83887 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6858 _reflns_number_gt 5413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'bruker smart apexii' _computing_cell_refinement 'bruker smart apexii' _computing_data_reduction 'bruker saint' _computing_structure_solution shelxtl _computing_structure_refinement 'shelxl-97 (sheldrick, 1997)' _computing_molecular_graphics wingx _computing_publication_material wingx _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^)+(0.0839P)^2^+1.0527P] 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 6858 _refine_ls_number_parameters 272 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.112 _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 Cu1 Cu 0.439732(16) 0.647317(10) 0.811672(18) 0.02007(10) Uani 1 1 d . . . O1 O 0.33839(10) 0.64613(6) 0.90240(11) 0.0266(4) Uani 1 1 d . . . O2 O 0.04119(19) 0.47765(16) 0.6016(2) 0.0937(10) Uani 1 1 d . . . O3 O 0.0520(2) 0.56142(19) 0.5366(2) 0.1138(14) Uani 1 1 d U . . H21 H 0.0100 0.5525 0.5052 0.171 Uiso 1 1 calc R . . O4 O 0.11259(10) 0.80333(7) 1.21961(11) 0.0287(4) Uani 1 1 d . . . O5 O 0.40110(10) 0.41774(6) 1.23962(10) 0.0252(3) Uani 1 1 d . . . O6 O 0.48386(9) 0.40017(6) 1.11631(10) 0.0242(3) Uani 1 1 d . . . O7 O -0.00415(10) 0.78739(6) 1.13560(12) 0.0289(4) Uani 1 1 d . . . P1 P 0.26673(4) 0.61111(2) 0.93235(4) 0.02192(14) Uani 1 1 d . . . C1 C 0.20525(15) 0.58670(11) 0.83593(16) 0.0303(5) Uani 1 1 d . . . C2 C 0.16329(18) 0.53591(14) 0.8382(2) 0.0454(7) Uani 1 1 d . . . H2 H 0.1662 0.5134 0.8927 0.055 Uiso 1 1 calc R . . C3 C 0.11764(19) 0.51799(17) 0.7620(2) 0.0583(9) Uani 1 1 d . . . H3 H 0.0901 0.4831 0.7643 0.070 Uiso 1 1 calc R . . C4 C 0.1119(2) 0.54969(18) 0.6845(3) 0.0610(10) Uani 1 1 d . . . C5 C 0.1513(3) 0.60032(19) 0.6803(2) 0.0718(12) Uani 1 1 d . . . H5 H 0.1453 0.6227 0.6260 0.086 Uiso 1 1 calc R . . C6 C 0.2006(2) 0.61954(13) 0.7560(2) 0.0504(8) Uani 1 1 d . . . H6 H 0.2296 0.6538 0.7521 0.060 Uiso 1 1 calc R . . C7 C 0.0636(2) 0.5268(2) 0.5987(3) 0.0664(10) Uani 1 1 d . . . C8 C 0.20144(15) 0.65309(9) 1.00549(15) 0.0244(5) Uani 1 1 d . . . C9 C 0.11737(16) 0.66080(11) 0.9893(2) 0.0380(6) Uani 1 1 d . . . H9 H 0.0892 0.6389 0.9440 0.046 Uiso 1 1 calc R . . C10 C 0.24129(17) 0.68393(12) 1.07426(19) 0.0405(6) Uani 1 1 d . . . H10 H 0.2986 0.6777 1.0867 0.049 Uiso 1 1 calc R . . C11 C 0.30171(13) 0.55160(9) 0.99746(15) 0.0220(4) Uani 1 1 d . . . C12 C 0.36260(14) 0.51868(10) 0.95587(15) 0.0262(5) Uani 1 1 d . . . H12 H 0.3781 0.5250 0.8926 0.031 Uiso 1 1 calc R . . C13 C 0.19841(16) 0.72345(11) 1.12450(19) 0.0386(6) Uani 1 1 d . . . H13 H 0.2260 0.7443 1.1716 0.046 Uiso 1 1 calc R . . C14 C 0.11491(14) 0.73264(9) 1.10620(16) 0.0263(5) Uani 1 1 d . . . C15 C 0.07424(16) 0.70114(12) 1.0401(2) 0.0404(7) Uani 1 1 d . . . H15 H 0.0166 0.7069 1.0289 0.048 Uiso 1 1 calc R . . C16 C 0.07074(14) 0.77801(10) 1.15794(17) 0.0266(5) Uani 1 1 d . . . C17 C 0.27693(15) 0.54098(10) 1.08920(16) 0.0291(5) Uani 1 1 d . . . H17 H 0.2339 0.5624 1.1169 0.035 Uiso 1 1 calc R . . C18 C 0.31540(15) 0.49883(10) 1.14009(16) 0.0298(5) Uani 1 1 d . . . H18 H 0.2986 0.4915 1.2026 0.036 Uiso 1 1 calc R . . C19 C 0.37842(14) 0.46742(9) 1.09936(15) 0.0237(4) Uani 1 1 d . . . C20 C 0.40062(14) 0.47672(9) 1.00655(15) 0.0264(5) Uani 1 1 d . . . H20 H 0.4419 0.4543 0.9779 0.032 Uiso 1 1 calc R . . C21 C 0.42439(13) 0.42516(9) 1.15632(15) 0.0222(4) 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 0.02024(16) 0.01668(15) 0.02328(16) -0.00010(9) -0.00086(10) -0.00036(9) O1 0.0287(8) 0.0205(8) 0.0307(8) -0.0010(6) 0.0060(7) 0.0016(6) O2 0.080(2) 0.111(3) 0.090(2) -0.044(2) -0.0264(17) -0.0082(19) O3 0.093(2) 0.184(4) 0.065(2) -0.030(2) -0.0367(17) 0.029(2) O4 0.0287(8) 0.0261(8) 0.0313(8) -0.0092(7) 0.0027(7) -0.0009(7) O5 0.0292(8) 0.0234(8) 0.0229(7) 0.0029(6) 0.0009(6) 0.0044(7) O6 0.0244(8) 0.0238(7) 0.0245(7) 0.0004(6) 0.0010(6) 0.0042(6) O7 0.0234(8) 0.0237(8) 0.0397(9) -0.0071(7) 0.0031(7) 0.0018(7) P1 0.0232(3) 0.0204(3) 0.0221(3) -0.0017(2) 0.0009(2) 0.0044(2) C1 0.0260(12) 0.0374(13) 0.0275(11) -0.0093(10) -0.0041(9) 0.0098(10) C2 0.0352(15) 0.0577(18) 0.0433(15) -0.0160(14) 0.0004(12) -0.0068(13) C3 0.0366(16) 0.085(3) 0.0536(19) -0.0282(18) -0.0052(14) -0.0062(16) C4 0.0381(17) 0.085(3) 0.060(2) -0.0335(19) -0.0109(15) 0.0105(17) C5 0.090(3) 0.093(3) 0.0326(16) -0.0018(17) -0.0190(17) 0.039(3) C6 0.062(2) 0.0510(17) 0.0382(15) 0.0008(13) -0.0113(14) 0.0124(15) C7 0.054(2) 0.078(3) 0.068(2) 0.001(2) -0.0065(18) 0.019(2) C8 0.0284(11) 0.0198(10) 0.0249(10) -0.0012(8) 0.0038(9) 0.0043(9) C9 0.0273(12) 0.0355(13) 0.0511(16) -0.0206(12) -0.0015(11) 0.0028(11) C10 0.0309(13) 0.0475(16) 0.0432(14) -0.0208(12) -0.0059(11) 0.0123(12) C11 0.0241(10) 0.0199(10) 0.0221(10) 0.0005(8) -0.0013(8) -0.0003(8) C12 0.0288(12) 0.0279(11) 0.0218(10) 0.0000(9) 0.0033(9) 0.0046(9) C13 0.0308(13) 0.0424(15) 0.0426(14) -0.0200(12) -0.0067(11) 0.0091(11) C14 0.0259(11) 0.0252(11) 0.0278(11) -0.0032(9) 0.0019(9) 0.0043(9) C15 0.0247(12) 0.0430(15) 0.0534(16) -0.0230(13) 0.0011(11) 0.0036(11) C16 0.0280(12) 0.0219(11) 0.0299(11) -0.0024(9) 0.0031(9) -0.0010(9) C17 0.0289(12) 0.0288(12) 0.0296(11) 0.0024(9) 0.0081(9) 0.0091(10) C18 0.0326(12) 0.0319(12) 0.0249(11) 0.0036(9) 0.0063(9) 0.0076(10) C19 0.0257(11) 0.0205(10) 0.0249(10) -0.0013(8) -0.0012(8) 0.0019(9) C20 0.0262(11) 0.0268(11) 0.0262(11) -0.0002(9) 0.0028(9) 0.0054(9) C21 0.0237(11) 0.0202(10) 0.0228(10) 0.0001(8) -0.0007(8) 0.0002(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 Cu1 O4 1.9634(15) 2_564 ? Cu1 O7 1.9640(15) 4_567 ? Cu1 O6 1.9696(15) 5_667 ? Cu1 O5 1.9759(15) 7_565 ? Cu1 O1 2.0832(16) . ? Cu1 Cu1 2.6207(5) 3_656 ? O1 P1 1.4910(17) . ? O2 C7 1.238(5) . ? O3 C7 1.233(5) . ? O3 H21 0.8400 . ? O4 C16 1.266(3) . ? O4 Cu1 1.9634(15) 2_565 ? O5 C21 1.261(3) . ? O5 Cu1 1.9759(15) 7_566 ? O6 C21 1.267(3) . ? O6 Cu1 1.9696(15) 5_667 ? O7 C16 1.266(3) . ? O7 Cu1 1.9640(15) 4_467 ? P1 C8 1.794(2) . ? P1 C1 1.796(2) . ? P1 C11 1.800(2) . ? C1 C6 1.393(4) . ? C1 C2 1.398(4) . ? C2 C3 1.382(4) . ? C2 H2 0.9500 . ? C3 C4 1.349(5) . ? C3 H3 0.9500 . ? C4 C5 1.375(6) . ? C4 C7 1.553(5) . ? C5 C6 1.420(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.384(3) . ? C8 C10 1.389(3) . ? C9 C15 1.398(3) . ? C9 H9 0.9500 . ? C10 C13 1.378(3) . ? C10 H10 0.9500 . ? C11 C12 1.393(3) . ? C11 C17 1.395(3) . ? C12 C20 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.386(3) . ? C13 H13 0.9500 . ? C14 C15 1.378(3) . ? C14 C16 1.499(3) . ? C15 H15 0.9500 . ? C17 C18 1.394(3) . ? C17 H17 0.9500 . ? C18 C19 1.393(3) . ? C18 H18 0.9500 . ? C19 C20 1.392(3) . ? C19 C21 1.499(3) . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cu1 O7 88.24(7) 2_564 4_567 ? O4 Cu1 O6 165.87(7) 2_564 5_667 ? O7 Cu1 O6 88.73(6) 4_567 5_667 ? O4 Cu1 O5 89.77(7) 2_564 7_565 ? O7 Cu1 O5 168.52(7) 4_567 7_565 ? O6 Cu1 O5 90.46(6) 5_667 7_565 ? O4 Cu1 O1 95.20(7) 2_564 . ? O7 Cu1 O1 97.55(6) 4_567 . ? O6 Cu1 O1 98.88(6) 5_667 . ? O5 Cu1 O1 93.89(6) 7_565 . ? O4 Cu1 Cu1 82.28(5) 2_564 3_656 ? O7 Cu1 Cu1 85.33(5) 4_567 3_656 ? O6 Cu1 Cu1 83.71(4) 5_667 3_656 ? O5 Cu1 Cu1 83.20(5) 7_565 3_656 ? O1 Cu1 Cu1 176.14(5) . 3_656 ? P1 O1 Cu1 142.31(9) . . ? C7 O3 H21 109.5 . . ? C16 O4 Cu1 122.08(15) . 2_565 ? C21 O5 Cu1 120.76(14) . 7_566 ? C21 O6 Cu1 120.73(14) . 5_667 ? C16 O7 Cu1 118.88(15) . 4_467 ? O1 P1 C8 107.50(10) . . ? O1 P1 C1 112.97(11) . . ? C8 P1 C1 108.06(11) . . ? O1 P1 C11 110.97(10) . . ? C8 P1 C11 109.29(10) . . ? C1 P1 C11 107.97(11) . . ? C6 C1 C2 119.4(3) . . ? C6 C1 P1 118.3(2) . . ? C2 C1 P1 122.3(2) . . ? C3 C2 C1 120.8(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 C7 118.8(4) . . ? C5 C4 C7 120.7(4) . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 118.1(3) . . ? C1 C6 H6 121.0 . . ? C5 C6 H6 121.0 . . ? O3 C7 O2 128.8(4) . . ? O3 C7 C4 113.9(4) . . ? O2 C7 C4 117.3(4) . . ? C9 C8 C10 119.8(2) . . ? C9 C8 P1 123.33(18) . . ? C10 C8 P1 116.37(18) . . ? C8 C9 C15 119.4(2) . . ? C8 C9 H9 120.3 . . ? C15 C9 H9 120.3 . . ? C13 C10 C8 120.5(2) . . ? C13 C10 H10 119.7 . . ? C8 C10 H10 119.7 . . ? C12 C11 C17 119.9(2) . . ? C12 C11 P1 116.88(16) . . ? C17 C11 P1 122.92(17) . . ? C20 C12 C11 120.1(2) . . ? C20 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C10 C13 C14 119.8(2) . . ? C10 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.1(2) . . ? C15 C14 C16 121.0(2) . . ? C13 C14 C16 118.8(2) . . ? C14 C15 C9 120.3(2) . . ? C14 C15 H15 119.9 . . ? C9 C15 H15 119.9 . . ? O4 C16 O7 126.5(2) . . ? O4 C16 C14 116.3(2) . . ? O7 C16 C14 117.1(2) . . ? C18 C17 C11 119.9(2) . . ? C18 C17 H17 120.1 . . ? C11 C17 H17 120.1 . . ? C19 C18 C17 120.0(2) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 119.8(2) . . ? C20 C19 C21 120.06(19) . . ? C18 C19 C21 120.1(2) . . ? C12 C20 C19 120.2(2) . . ? C12 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? O5 C21 O6 125.7(2) . . ? O5 C21 C19 117.58(19) . . ? O6 C21 C19 116.73(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.242 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.086 # 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 0.121 0.250 0.012 1165.5 273.9 2 0.143 0.750 -0.085 1165.5 273.7 _platon_squeeze_details ; The contributions of some 548 electrons were removed from the unit-cell contents, and as Z = 8 in this case, this could/might correspond with the removal of solvent such as 1(DMF) and 3(H2O) [some 69 electrons] per asymmetric unit. ; # Attachment '- cif-complex2-revise2.cif' data_squeezed _database_code_depnum_ccdc_archive 'CCDC 859101' #TrackingRef '- cif-complex2-revise2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C258 H384 N13.33 O129 P8 Zn15' _chemical_formula_weight 6964.76 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' P P 0.1023 0.0942 '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 Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, 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' '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' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -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' '-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' _cell_length_a 34.340(3) _cell_length_b 34.340(3) _cell_length_c 19.451(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19865(4) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2455 _cell_measurement_theta_min 3.7745 _cell_measurement_theta_max 20.2715 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10882 _exptl_absorpt_coefficient_mu 1.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7426 _exptl_absorpt_correction_T_max 0.8687 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27880 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.1439 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.30 _reflns_number_total 10904 _reflns_number_gt 4379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEXll' _computing_cell_refinement 'Bruker SMART APEXll' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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.The water and carboxylate oxygens were disordered over two sites (0.61:0.39 for O8A and O8B; 0.5:0.5 for O3A and O3B), respectively. ; _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^)+(0.1166P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10904 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.2382 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _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 Zn1 Zn 0.72831(2) 0.12767(2) 0.66024(3) 0.0576(2) Uani 1 1 d . . . Zn2 Zn 0.82213(2) 0.15235(2) 0.74203(4) 0.0629(3) Uani 1 1 d . . . Zn3 Zn 0.94357(4) -0.04899(4) 0.96208(6) 0.0471(3) Uani 0.50 1 d P . . P1 P 0.77896(5) 0.03685(5) 0.74416(7) 0.0478(4) Uani 1 1 d . . . P2 P 0.6667 0.3333 0.54562(16) 0.0671(8) Uani 1 3 d S . . O1 O 0.79911(13) 0.08558(12) 0.72716(19) 0.0588(10) Uani 1 1 d . A . O2 O 0.9027(2) -0.0334(2) 0.9168(3) 0.125(2) Uani 1 1 d . . . O4 O 1.0000 0.0000 1.0000 0.0412(19) Uani 1 6 d S . . O5 O 0.5682(3) -0.0422(3) 0.8553(4) 0.141(3) Uani 1 1 d . . . O6 O 0.70060(15) -0.10807(16) 0.4785(2) 0.0730(12) Uani 1 1 d . . . O7 O 0.73952(15) -0.04312(15) 0.4237(2) 0.0693(12) Uani 1 1 d . . . O8A O 0.8636(3) 0.1663(3) 0.8228(4) 0.095(4) Uiso 0.612(14) 1 d P A 1 O8B O 0.8613(5) 0.2012(5) 0.8007(7) 0.107(7) Uiso 0.388(14) 1 d P A 2 O9 O 0.5981(2) -0.0387(2) 0.9515(3) 0.131(3) Uani 1 1 d . . . O10 O 0.70923(15) 0.16911(15) 0.6273(2) 0.0716(12) Uani 1 1 d . . . O11 O 0.76614(16) 0.22583(15) 0.6871(2) 0.0803(13) Uani 1 1 d . . . O12 O 0.6667 0.3333 0.4648(4) 0.076(2) Uani 1 3 d S . . O14 O 0.79419(12) 0.16592(13) 0.66208(18) 0.0559(10) Uani 1 1 d . . . H14 H 0.7985 0.1962 0.6739 0.067 Uiso 1 1 calc R . . C1 C 0.81787(19) 0.0269(2) 0.7909(3) 0.0549(14) Uani 1 1 d . A . C2 C 0.8556(3) 0.0630(3) 0.8226(4) 0.103(3) Uani 1 1 d . . . H2 H 0.8611 0.0928 0.8171 0.123 Uiso 1 1 calc R A . C3 C 0.8839(3) 0.0554(3) 0.8607(5) 0.125(4) Uani 1 1 d . A . H3 H 0.9084 0.0799 0.8834 0.150 Uiso 1 1 calc R . . C4 C 0.8779(3) 0.0134(3) 0.8673(4) 0.093(3) Uani 1 1 d . . . C5 C 0.8434(3) -0.0214(3) 0.8355(4) 0.081(2) Uani 1 1 d . A . H5 H 0.8407 -0.0502 0.8385 0.097 Uiso 1 1 calc R . . C6 C 0.8111(3) -0.0168(2) 0.7981(4) 0.084(2) Uani 1 1 d . . . H6 H 0.7858 -0.0421 0.7785 0.100 Uiso 1 1 calc R A . C7 C 0.9131(4) 0.0098(4) 0.9070(6) 0.125(3) Uiso 1 1 d . A . O3A O 0.9540(2) 0.0486(2) 0.9161(3) 0.0500(18) Uiso 0.50 1 d P . . O3B O 0.9221(3) 0.0239(3) 0.9683(5) 0.077(2) Uiso 0.50 1 d P A . C8 C 0.72834(19) 0.01471(19) 0.7941(3) 0.0536(14) Uani 1 1 d . A . C9 C 0.6910(3) 0.0126(3) 0.7633(5) 0.111(3) Uani 1 1 d . . . H9 H 0.6941 0.0234 0.7175 0.133 Uiso 1 1 calc R A . C10 C 0.6519(3) -0.0032(3) 0.7927(6) 0.116(3) Uani 1 1 d . A . H10 H 0.6270 -0.0061 0.7674 0.139 Uiso 1 1 calc R . . C11 C 0.6473(2) -0.0151(2) 0.8574(5) 0.075(2) Uani 1 1 d . . . C12 C 0.6830(3) -0.0146(3) 0.8945(4) 0.111(3) Uani 1 1 d . A . H12 H 0.6793 -0.0244 0.9410 0.133 Uiso 1 1 calc R . . C13 C 0.7250(2) 0.0014(3) 0.8593(3) 0.098(3) Uani 1 1 d . . . H13 H 0.7500 0.0024 0.8820 0.117 Uiso 1 1 calc R A . C14 C 0.6017(3) -0.0337(3) 0.8950(7) 0.105(3) Uani 1 1 d . A . C15 C 0.76379(18) 0.0040(2) 0.6660(3) 0.0499(14) Uani 1 1 d . A . C16 C 0.7847(2) 0.0267(2) 0.6062(3) 0.0707(18) Uani 1 1 d . . . H16 H 0.8069 0.0577 0.6074 0.085 Uiso 1 1 calc R A . C17 C 0.7320(2) -0.0415(2) 0.6643(3) 0.0630(16) Uani 1 1 d . . . H17 H 0.7186 -0.0568 0.7059 0.076 Uiso 1 1 calc R A . C18 C 0.7726(2) 0.0032(2) 0.5443(3) 0.081(2) Uani 1 1 d . A . H18 H 0.7866 0.0181 0.5027 0.097 Uiso 1 1 calc R . . C19 C 0.7399(2) -0.0420(2) 0.5434(3) 0.0590(15) Uani 1 1 d . . . C20 C 0.7198(2) -0.0648(2) 0.6029(3) 0.0634(16) Uani 1 1 d . A . H20 H 0.6979 -0.0959 0.6018 0.076 Uiso 1 1 calc R . . C21 C 0.7252(2) -0.0671(3) 0.4758(3) 0.0617(16) Uani 1 1 d . A . C22 C 0.6866(2) 0.2985(2) 0.5801(3) 0.0668(17) Uani 1 1 d . . . C23 C 0.6675(3) 0.2544(2) 0.5540(4) 0.088(2) Uani 1 1 d . . . H23 H 0.6452 0.2446 0.5191 0.106 Uiso 1 1 calc R . . C24 C 0.6811(2) 0.2252(2) 0.5787(4) 0.083(2) Uani 1 1 d . . . H24 H 0.6671 0.1950 0.5627 0.099 Uiso 1 1 calc R . . C25 C 0.7154(2) 0.2405(2) 0.6270(3) 0.0620(16) Uani 1 1 d . . . C26 C 0.7335(2) 0.2825(2) 0.6537(3) 0.0709(18) Uani 1 1 d . . . H26 H 0.7558 0.2922 0.6885 0.085 Uiso 1 1 calc R . . C27 C 0.7188(2) 0.3114(2) 0.6294(4) 0.077(2) Uani 1 1 d . . . H27 H 0.7318 0.3409 0.6478 0.093 Uiso 1 1 calc R . . C28 C 0.7315(2) 0.2100(2) 0.6495(3) 0.0658(17) 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 0.0524(4) 0.0549(4) 0.0531(4) -0.0048(3) 0.0064(3) 0.0176(4) Zn2 0.0592(5) 0.0634(5) 0.0655(5) -0.0023(4) 0.0186(3) 0.0303(4) Zn3 0.0404(7) 0.0407(7) 0.0603(8) 0.0001(6) 0.0038(6) 0.0203(6) P1 0.0498(9) 0.0516(9) 0.0449(8) -0.0023(6) -0.0049(6) 0.0275(7) P2 0.0633(12) 0.0633(12) 0.075(2) 0.000 0.000 0.0317(6) O1 0.068(3) 0.045(2) 0.061(2) -0.0029(18) -0.006(2) 0.027(2) O2 0.172(6) 0.178(6) 0.104(4) -0.059(4) -0.069(4) 0.145(6) O4 0.036(3) 0.036(3) 0.051(5) 0.000 0.000 0.0182(14) O5 0.103(5) 0.194(8) 0.144(6) 0.023(5) 0.031(5) 0.088(5) O6 0.068(3) 0.070(3) 0.063(3) -0.024(2) -0.022(2) 0.021(3) O7 0.090(3) 0.068(3) 0.053(3) -0.022(2) -0.022(2) 0.042(3) O9 0.119(5) 0.098(4) 0.088(4) -0.025(3) 0.057(4) -0.011(3) O10 0.069(3) 0.067(3) 0.079(3) -0.020(2) -0.009(2) 0.035(3) O11 0.083(3) 0.072(3) 0.101(3) -0.023(3) -0.029(3) 0.050(3) O12 0.066(3) 0.066(3) 0.097(6) 0.000 0.000 0.0328(15) O14 0.046(2) 0.059(2) 0.063(2) -0.0090(19) 0.0067(18) 0.026(2) C1 0.052(4) 0.066(4) 0.049(3) -0.017(3) -0.005(3) 0.031(3) C2 0.092(6) 0.120(7) 0.118(6) -0.036(5) -0.048(5) 0.068(6) C3 0.113(7) 0.131(8) 0.171(9) -0.079(7) -0.093(7) 0.090(7) C4 0.112(6) 0.138(7) 0.091(5) -0.055(5) -0.052(5) 0.110(6) C5 0.092(5) 0.082(5) 0.089(5) -0.018(4) -0.019(4) 0.057(5) C6 0.104(6) 0.072(5) 0.090(5) -0.016(4) -0.039(4) 0.055(5) C8 0.048(3) 0.050(3) 0.065(4) -0.014(3) -0.001(3) 0.026(3) C9 0.062(5) 0.115(7) 0.175(9) 0.049(6) 0.013(5) 0.059(5) C10 0.076(6) 0.136(8) 0.167(10) 0.015(7) 0.033(6) 0.076(6) C11 0.047(4) 0.075(5) 0.105(6) -0.044(4) 0.009(4) 0.031(4) C12 0.115(7) 0.129(8) 0.048(4) -0.020(4) 0.018(4) 0.029(6) C13 0.061(4) 0.163(8) 0.050(4) -0.012(4) 0.009(3) 0.041(5) C14 0.055(5) 0.081(6) 0.146(9) -0.019(6) 0.006(6) 0.009(5) C15 0.046(3) 0.062(4) 0.046(3) -0.008(3) -0.009(2) 0.031(3) C16 0.072(4) 0.059(4) 0.053(4) -0.013(3) 0.007(3) 0.012(3) C17 0.071(4) 0.057(4) 0.051(3) 0.003(3) 0.000(3) 0.025(4) C18 0.075(5) 0.081(5) 0.042(3) -0.007(3) -0.007(3) 0.006(4) C19 0.053(4) 0.068(4) 0.057(4) -0.015(3) -0.017(3) 0.032(3) C20 0.065(4) 0.054(4) 0.063(4) -0.002(3) -0.007(3) 0.023(3) C21 0.065(4) 0.073(5) 0.062(4) -0.017(4) -0.019(3) 0.046(4) C22 0.047(4) 0.060(4) 0.082(4) -0.017(3) -0.008(3) 0.018(3) C23 0.089(6) 0.068(5) 0.114(6) -0.025(4) -0.034(5) 0.044(4) C24 0.088(5) 0.054(4) 0.106(6) -0.023(4) -0.031(4) 0.036(4) C25 0.065(4) 0.057(4) 0.064(4) -0.013(3) -0.012(3) 0.030(3) C26 0.079(5) 0.077(5) 0.060(4) -0.021(3) -0.020(3) 0.042(4) C27 0.078(5) 0.066(5) 0.086(5) -0.028(4) -0.007(4) 0.035(4) C28 0.070(5) 0.071(5) 0.068(4) -0.012(3) -0.007(3) 0.043(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 O9 1.940(6) 9_654 ? Zn1 O10 1.949(4) . ? Zn1 O7 1.963(4) 5_545 ? Zn1 O14 1.968(4) . ? Zn2 O8B 1.917(15) . ? Zn2 O14 2.001(4) . ? Zn2 O6 2.010(4) 5_545 ? Zn2 O8A 2.012(8) . ? Zn2 O1 2.038(4) . ? Zn2 O14 2.063(3) 13_656 ? Zn2 Zn2 3.0655(14) 13_656 ? Zn3 O3B 1.924(9) 12_547 ? Zn3 O3A 1.934(7) 2_645 ? Zn3 O2 1.945(5) . ? Zn3 O4 1.9670(12) . ? Zn3 Zn3 2.3455(19) 11_667 ? Zn3 Zn3 2.3455(19) 12_547 ? Zn3 Zn3 3.158(2) 3_765 ? Zn3 Zn3 3.158(2) 2_645 ? P1 O1 1.494(4) . ? P1 C1 1.785(6) . ? P1 C8 1.795(6) . ? P1 C15 1.808(5) . ? P2 O12 1.572(8) . ? P2 C22 1.780(7) . ? P2 C22 1.780(7) 2_655 ? P2 C22 1.780(7) 3_665 ? O2 C7 1.352(11) . ? O4 Zn3 1.9670(12) 12_547 ? O4 Zn3 1.9670(12) 11_667 ? O4 Zn3 1.9670(12) 10_757 ? O4 Zn3 1.9670(12) 3_765 ? O4 Zn3 1.9670(12) 2_645 ? O5 C14 1.291(11) . ? O6 C21 1.227(7) . ? O6 Zn2 2.010(4) 9_654 ? O7 C21 1.243(8) . ? O7 Zn1 1.963(4) 9_654 ? O9 C14 1.110(11) . ? O9 Zn1 1.940(6) 5_545 ? O10 C28 1.293(7) . ? O11 C28 1.264(7) . ? O14 Zn2 2.063(3) 13_656 ? O14 H14 1.0000 . ? C1 C6 1.405(8) . ? C1 C2 1.412(9) . ? C2 C3 1.345(10) . ? C2 H2 0.9500 . ? C3 C4 1.357(11) . ? C3 H3 0.9500 . ? C4 C5 1.342(10) . ? C4 C7 1.493(12) . ? C5 C6 1.397(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O3B 1.266(12) . ? C7 O3A 1.382(12) . ? O3A O3B 1.422(11) . ? O3A Zn3 1.934(7) 3_765 ? O3B Zn3 1.924(9) 11_667 ? C8 C13 1.333(8) . ? C8 C9 1.382(9) . ? C9 C10 1.303(10) . ? C9 H9 0.9500 . ? C10 C11 1.308(11) . ? C10 H10 0.9500 . ? C11 C12 1.414(11) . ? C11 C14 1.549(11) . ? C12 C13 1.434(10) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C15 C16 1.385(8) . ? C15 C17 1.387(8) . ? C16 C18 1.392(8) . ? C16 H16 0.9500 . ? C17 C20 1.381(8) . ? C17 H17 0.9500 . ? C18 C19 1.390(9) . ? C18 H18 0.9500 . ? C19 C20 1.374(8) . ? C19 C21 1.513(8) . ? C20 H20 0.9500 . ? C22 C27 1.361(9) . ? C22 C23 1.410(9) . ? C23 C24 1.388(9) . ? C23 H23 0.9500 . ? C24 C25 1.388(9) . ? C24 H24 0.9500 . ? C25 C26 1.356(8) . ? C25 C28 1.473(8) . ? C26 C27 1.399(9) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? 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 Zn1 O10 114.0(2) 9_654 . ? O9 Zn1 O7 103.6(3) 9_654 5_545 ? O10 Zn1 O7 105.78(19) . 5_545 ? O9 Zn1 O14 124.3(3) 9_654 . ? O10 Zn1 O14 102.27(17) . . ? O7 Zn1 O14 105.43(17) 5_545 . ? O8B Zn2 O14 117.9(5) . . ? O8B Zn2 O6 84.5(4) . 5_545 ? O14 Zn2 O6 97.24(17) . 5_545 ? O8B Zn2 O8A 39.0(5) . . ? O14 Zn2 O8A 156.5(3) . . ? O6 Zn2 O8A 85.9(3) 5_545 . ? O8B Zn2 O1 141.0(5) . . ? O14 Zn2 O1 100.97(16) . . ? O6 Zn2 O1 94.17(18) 5_545 . ? O8A Zn2 O1 102.0(3) . . ? O8B Zn2 O14 92.5(4) . 13_656 ? O14 Zn2 O14 82.08(16) . 13_656 ? O6 Zn2 O14 176.27(18) 5_545 13_656 ? O8A Zn2 O14 93.2(3) . 13_656 ? O1 Zn2 O14 89.56(16) . 13_656 ? O8B Zn2 Zn2 109.6(5) . 13_656 ? O14 Zn2 Zn2 41.81(10) . 13_656 ? O6 Zn2 Zn2 138.93(14) 5_545 13_656 ? O8A Zn2 Zn2 129.5(2) . 13_656 ? O1 Zn2 Zn2 96.84(11) . 13_656 ? O14 Zn2 Zn2 40.27(10) 13_656 13_656 ? O3B Zn3 O3A 108.2(3) 12_547 2_645 ? O3B Zn3 O2 87.2(3) 12_547 . ? O3A Zn3 O2 115.1(3) 2_645 . ? O3B Zn3 O4 112.0(3) 12_547 . ? O3A Zn3 O4 112.9(2) 2_645 . ? O2 Zn3 O4 118.2(2) . . ? O3B Zn3 Zn3 73.1(3) 12_547 11_667 ? O3A Zn3 Zn3 163.2(2) 2_645 11_667 ? O2 Zn3 Zn3 81.55(16) . 11_667 ? O4 Zn3 Zn3 53.40(2) . 11_667 ? O3B Zn3 Zn3 86.6(3) 12_547 12_547 ? O3A Zn3 Zn3 78.8(2) 2_645 12_547 ? O2 Zn3 Zn3 166.01(17) . 12_547 ? O4 Zn3 Zn3 53.40(2) . 12_547 ? Zn3 Zn3 Zn3 84.64(7) 11_667 12_547 ? O3B Zn3 Zn3 120.7(3) 12_547 3_765 ? O3A Zn3 Zn3 129.0(2) 2_645 3_765 ? O2 Zn3 Zn3 82.4(2) . 3_765 ? O4 Zn3 Zn3 36.60(2) . 3_765 ? Zn3 Zn3 Zn3 47.68(4) 11_667 3_765 ? Zn3 Zn3 Zn3 90.0 12_547 3_765 ? O3B Zn3 Zn3 133.1(3) 12_547 2_645 ? O3A Zn3 Zn3 76.9(2) 2_645 2_645 ? O2 Zn3 Zn3 134.2(2) . 2_645 ? O4 Zn3 Zn3 36.60(2) . 2_645 ? Zn3 Zn3 Zn3 90.0 11_667 2_645 ? Zn3 Zn3 Zn3 47.68(4) 12_547 2_645 ? Zn3 Zn3 Zn3 60.0 3_765 2_645 ? O1 P1 C1 110.9(3) . . ? O1 P1 C8 113.7(2) . . ? C1 P1 C8 107.6(3) . . ? O1 P1 C15 109.9(2) . . ? C1 P1 C15 108.5(2) . . ? C8 P1 C15 105.9(3) . . ? O12 P2 C22 112.2(2) . . ? O12 P2 C22 112.2(2) . 2_655 ? C22 P2 C22 106.7(3) . 2_655 ? O12 P2 C22 112.2(2) . 3_665 ? C22 P2 C22 106.7(3) . 3_665 ? C22 P2 C22 106.7(3) 2_655 3_665 ? P1 O1 Zn2 158.6(3) . . ? C7 O2 Zn3 122.3(7) . . ? Zn3 O4 Zn3 106.80(4) 12_547 11_667 ? Zn3 O4 Zn3 73.20(4) 12_547 . ? Zn3 O4 Zn3 73.20(4) 11_667 . ? Zn3 O4 Zn3 106.80(4) 12_547 10_757 ? Zn3 O4 Zn3 106.80(4) 11_667 10_757 ? Zn3 O4 Zn3 180.00(7) . 10_757 ? Zn3 O4 Zn3 180.00(3) 12_547 3_765 ? Zn3 O4 Zn3 73.20(4) 11_667 3_765 ? Zn3 O4 Zn3 106.80(4) . 3_765 ? Zn3 O4 Zn3 73.20(4) 10_757 3_765 ? Zn3 O4 Zn3 73.20(4) 12_547 2_645 ? Zn3 O4 Zn3 180.00(7) 11_667 2_645 ? Zn3 O4 Zn3 106.80(4) . 2_645 ? Zn3 O4 Zn3 73.20(4) 10_757 2_645 ? Zn3 O4 Zn3 106.80(4) 3_765 2_645 ? C21 O6 Zn2 133.9(4) . 9_654 ? C21 O7 Zn1 128.6(4) . 9_654 ? C14 O9 Zn1 120.0(7) . 5_545 ? C28 O10 Zn1 116.8(4) . . ? Zn1 O14 Zn2 112.56(18) . . ? Zn1 O14 Zn2 134.01(19) . 13_656 ? Zn2 O14 Zn2 97.92(16) . 13_656 ? Zn1 O14 H14 102.9 . . ? Zn2 O14 H14 102.9 . . ? Zn2 O14 H14 102.9 13_656 . ? C6 C1 C2 118.9(6) . . ? C6 C1 P1 121.1(5) . . ? C2 C1 P1 120.0(5) . . ? C3 C2 C1 120.4(8) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 121.1(8) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 120.0(6) . . ? C5 C4 C7 123.7(8) . . ? C3 C4 C7 116.1(8) . . ? C4 C5 C6 122.4(7) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 117.1(7) . . ? C5 C6 H6 121.4 . . ? C1 C6 H6 121.4 . . ? O3B C7 O2 99.8(9) . . ? O3B C7 O3A 64.8(7) . . ? O2 C7 O3A 128.5(10) . . ? O3B C7 C4 120.5(10) . . ? O2 C7 C4 112.6(9) . . ? O3A C7 C4 117.4(10) . . ? C7 O3A O3B 53.6(6) . . ? C7 O3A Zn3 129.0(7) . 3_765 ? O3B O3A Zn3 98.5(5) . 3_765 ? C7 O3B O3A 61.6(7) . . ? C7 O3B Zn3 127.7(8) . 11_667 ? O3A O3B Zn3 108.7(6) . 11_667 ? C13 C8 C9 118.3(7) . . ? C13 C8 P1 124.0(5) . . ? C9 C8 P1 117.6(6) . . ? C10 C9 C8 124.5(9) . . ? C10 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? C9 C10 C11 119.5(9) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C10 C11 C12 121.2(7) . . ? C10 C11 C14 121.5(8) . . ? C12 C11 C14 117.2(9) . . ? C11 C12 C13 117.3(7) . . ? C11 C12 H12 121.3 . . ? C13 C12 H12 121.3 . . ? C8 C13 C12 119.0(7) . . ? C8 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? O9 C14 O5 122.8(10) . . ? O9 C14 C11 122.8(10) . . ? O5 C14 C11 114.4(10) . . ? C16 C15 C17 120.5(5) . . ? C16 C15 P1 116.6(4) . . ? C17 C15 P1 122.8(4) . . ? C15 C16 C18 118.6(6) . . ? C15 C16 H16 120.7 . . ? C18 C16 H16 120.7 . . ? C20 C17 C15 120.9(6) . . ? C20 C17 H17 119.5 . . ? C15 C17 H17 119.5 . . ? C19 C18 C16 120.0(6) . . ? C19 C18 H18 120.0 . . ? C16 C18 H18 120.0 . . ? C20 C19 C18 121.3(5) . . ? C20 C19 C21 118.6(6) . . ? C18 C19 C21 120.1(6) . . ? C19 C20 C17 118.5(6) . . ? C19 C20 H20 120.7 . . ? C17 C20 H20 120.7 . . ? O6 C21 O7 127.7(6) . . ? O6 C21 C19 117.3(6) . . ? O7 C21 C19 115.0(6) . . ? C27 C22 C23 117.9(6) . . ? C27 C22 P2 124.8(5) . . ? C23 C22 P2 117.3(5) . . ? C24 C23 C22 120.6(6) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.2(6) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C26 C25 C24 120.9(6) . . ? C26 C25 C28 120.5(6) . . ? C24 C25 C28 118.7(6) . . ? C25 C26 C27 119.3(6) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C22 C27 C26 122.0(6) . . ? C22 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? O11 C28 O10 125.3(6) . . ? O11 C28 C25 118.3(6) . . ? O10 C28 C25 116.4(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.350 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.098 # 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 -0.009 -0.005 0.421 8902.1 1258.6 _platon_squeeze_details ; The contributions of some 1259 electrons were removed from the unit-cell contents. The oxygen (O4) atom is at a site with -3 symmetry and there are six Zn(II)2.5 formula units in the unit cell. Therefore, this could/might correspond with the removal of solvent such as 5(DMF) and 1(H2O) [some 210 electrons] from the Zn(II)2.5 formula unit. ; # Attachment '- cif-complex3-revise2.cif' data_cutb _database_code_depnum_ccdc_archive 'CCDC 859102' #TrackingRef '- cif-complex3-revise2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H44.50 N2 O21 P2 Tb2' _chemical_formula_weight 1377.15 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 '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 monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 14.4794(6) _cell_length_b 10.5573(5) _cell_length_c 23.3160(11) _cell_angle_alpha 90.00 _cell_angle_beta 107.316(3) _cell_angle_gamma 90.00 _cell_volume 3402.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4542 _cell_measurement_theta_min 2.4345 _cell_measurement_theta_max 25.013 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1361 _exptl_absorpt_coefficient_mu 2.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7466 _exptl_absorpt_correction_T_max 0.8472 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28623 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.34 _reflns_number_total 8407 _reflns_number_gt 6104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'bruker smart apexii' _computing_cell_refinement 'bruker smart apexii' _computing_data_reduction 'bruker saint' _computing_structure_solution shelxtl _computing_structure_refinement 'shelxl-97 (sheldrick, 1997)' _computing_molecular_graphics wingx _computing_publication_material wingx _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^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8407 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _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 Tb1 Tb 0.574091(15) 0.95195(2) 0.230027(10) 0.02528(8) Uani 1 1 d . . . O1 O 0.4861(2) 1.0752(3) 0.14949(15) 0.0298(7) Uani 1 1 d . . . O2 O 0.4700(2) 0.7973(3) 0.15866(16) 0.0421(9) Uani 1 1 d . . . O3 O 0.5806(2) 0.7247(3) 0.23828(16) 0.0437(9) Uani 1 1 d . . . O4 O 0.4496(3) 0.9007(4) 0.27801(18) 0.0477(10) Uani 1 1 d . . . O5 O 0.4937(2) 1.0983(3) 0.27938(16) 0.0405(9) Uani 1 1 d . . . O6 O 0.6779(2) 0.9010(4) 0.17739(16) 0.0503(10) Uani 1 1 d . . . O7 O 0.6730(2) 0.9108(4) 0.32713(15) 0.0436(9) Uani 1 1 d . . . O8 O 0.6733(2) 1.1328(3) 0.24817(19) 0.0499(10) Uani 1 1 d . . . O9 O 0.7500 0.6351(15) 0.2500 0.223(6) Uani 1 2 d S . . P1 P 0.40153(8) 1.16027(11) 0.12202(5) 0.0259(3) Uani 1 1 d . . . C1 C 0.2999(3) 1.1216(4) 0.1479(2) 0.0265(10) Uani 1 1 d . . . C2 C 0.2385(4) 1.2116(5) 0.1590(2) 0.0383(12) Uani 1 1 d . . . H2 H 0.2500 1.2968 0.1538 0.046 Uiso 1 1 calc R . . C3 C 0.4321(3) 1.3220(4) 0.1384(2) 0.0304(11) Uani 1 1 d . . . C4 C 0.5049(5) 1.3501(6) 0.1907(3) 0.072(2) Uani 1 1 d . . . H4 H 0.5373 1.2844 0.2151 0.087 Uiso 1 1 calc R . . C5 C 0.3603(3) 1.1445(4) 0.0418(2) 0.0287(10) Uani 1 1 d . . . C6 C 0.2631(4) 1.1360(6) 0.0112(3) 0.0540(17) Uani 1 1 d . . . H6 H 0.2178 1.1393 0.0322 0.065 Uiso 1 1 calc R . . C7 C 0.2326(4) 1.1228(6) -0.0502(2) 0.0546(17) Uani 1 1 d . . . H7 H 0.1667 1.1180 -0.0702 0.066 Uiso 1 1 calc R . . C8 C 0.4261(4) 1.1415(6) 0.0097(2) 0.0509(16) Uani 1 1 d . . . H8 H 0.4919 1.1495 0.0295 0.061 Uiso 1 1 calc R . . C9 C 0.5298(5) 0.4729(5) 0.2071(3) 0.084(3) Uani 1 1 d . . . H9 H 0.5783 0.4895 0.2427 0.100 Uiso 1 1 calc R . . C10 C 0.4833(4) 0.5739(4) 0.1709(3) 0.0387(13) Uani 1 1 d . . . C11 C 0.4114(4) 0.5466(5) 0.1187(3) 0.0562(17) Uani 1 1 d . . . H11 H 0.3795 0.6122 0.0941 0.067 Uiso 1 1 calc R . . C12 C 0.3858(4) 0.4219(5) 0.1023(3) 0.0585(18) Uani 1 1 d . . . H12 H 0.3372 0.4050 0.0669 0.070 Uiso 1 1 calc R . . C13 C 0.5133(4) 0.7066(5) 0.1909(3) 0.0393(13) Uani 1 1 d . . . C14 C 0.2199(3) 0.9952(5) 0.3444(2) 0.0357(12) Uani 1 1 d . . . H14 H 0.1794 0.9330 0.3518 0.043 Uiso 1 1 calc R . . C15 C 0.2972(3) 0.9604(5) 0.3263(2) 0.0394(13) Uani 1 1 d . . . H15 H 0.3099 0.8751 0.3224 0.047 Uiso 1 1 calc R . . C16 C 0.3569(3) 1.0512(5) 0.3137(2) 0.0323(11) Uani 1 1 d . . . C17 C 0.3401(4) 1.1774(5) 0.3221(2) 0.0409(13) Uani 1 1 d . . . H17 H 0.3812 1.2392 0.3151 0.049 Uiso 1 1 calc R . . C18 C 0.4395(3) 1.0153(5) 0.2899(2) 0.0354(12) Uani 1 1 d . . . C19 C 0.6052(3) 0.8732(6) 0.0522(2) 0.0506(16) Uani 1 1 d . . . H19 H 0.5603 0.8761 0.0735 0.061 Uiso 1 1 calc R . . C20 C 0.7025(3) 0.8835(5) 0.0825(2) 0.0306(11) Uani 1 1 d . . . C21 C 0.7381(3) 0.9004(4) 0.1495(2) 0.0275(10) Uani 1 1 d . . . C22 C 0.7500 1.1798(7) 0.2500 0.063(3) Uani 1 2 d S . . H22 H 0.7500 1.2679 0.2500 0.076 Uiso 1 2 calc SR . . 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 Tb1 0.02495(12) 0.02862(13) 0.02085(13) -0.00032(11) 0.00465(9) 0.00045(10) O1 0.0312(17) 0.0257(17) 0.031(2) 0.0058(15) 0.0068(15) 0.0016(13) O2 0.046(2) 0.0300(19) 0.041(2) -0.0025(18) -0.0011(18) 0.0016(16) O3 0.049(2) 0.035(2) 0.036(2) -0.0070(18) -0.0043(19) -0.0023(16) O4 0.047(2) 0.044(2) 0.058(3) -0.009(2) 0.025(2) -0.0030(17) O5 0.0394(19) 0.043(2) 0.047(2) -0.0044(19) 0.0249(18) -0.0016(16) O6 0.037(2) 0.085(3) 0.032(2) -0.017(2) 0.0149(17) 0.0017(19) O7 0.038(2) 0.064(2) 0.023(2) 0.0035(18) 0.0008(16) 0.0032(17) O8 0.0345(19) 0.040(2) 0.073(3) 0.000(2) 0.0140(19) -0.0048(17) O9 0.114(8) 0.290(17) 0.253(16) 0.000 0.034(9) 0.000 P1 0.0278(6) 0.0282(6) 0.0203(7) 0.0016(5) 0.0050(5) -0.0022(5) C1 0.026(2) 0.035(3) 0.016(2) -0.002(2) 0.0017(19) -0.0040(19) C2 0.049(3) 0.029(3) 0.042(3) 0.000(2) 0.021(3) 0.001(2) C3 0.035(2) 0.027(3) 0.028(3) 0.004(2) 0.007(2) 0.000(2) C4 0.089(5) 0.032(3) 0.059(5) -0.003(3) -0.035(4) 0.002(3) C5 0.028(2) 0.033(3) 0.022(3) -0.003(2) 0.003(2) 0.003(2) C6 0.028(3) 0.104(5) 0.034(3) -0.002(4) 0.014(2) -0.006(3) C7 0.025(3) 0.113(5) 0.022(3) -0.016(3) 0.003(2) -0.009(3) C8 0.026(3) 0.094(5) 0.030(3) -0.010(3) 0.006(2) -0.005(3) C9 0.102(5) 0.033(4) 0.068(5) 0.001(3) -0.048(4) -0.006(3) C10 0.043(3) 0.024(3) 0.046(4) -0.003(2) 0.009(3) -0.004(2) C11 0.074(4) 0.028(3) 0.051(4) -0.001(3) -0.004(3) -0.003(3) C12 0.059(4) 0.047(4) 0.048(4) 0.001(3) -0.017(3) -0.008(3) C13 0.042(3) 0.023(3) 0.057(4) 0.005(3) 0.022(3) 0.005(2) C14 0.030(3) 0.036(3) 0.042(3) 0.008(3) 0.014(2) -0.001(2) C15 0.032(3) 0.044(3) 0.042(3) -0.002(3) 0.010(2) 0.004(2) C16 0.029(2) 0.045(3) 0.023(3) -0.002(2) 0.009(2) 0.003(2) C17 0.037(3) 0.043(3) 0.050(4) 0.002(3) 0.023(3) -0.003(2) C18 0.035(3) 0.045(3) 0.024(3) -0.004(2) 0.005(2) 0.005(2) C19 0.027(3) 0.094(5) 0.034(3) -0.004(3) 0.014(2) -0.004(3) C20 0.032(2) 0.040(3) 0.018(3) 0.000(2) 0.004(2) 0.000(2) C21 0.030(2) 0.029(2) 0.024(3) -0.001(2) 0.008(2) 0.0028(19) C22 0.031(4) 0.030(4) 0.124(9) 0.000 0.016(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O6 2.271(3) . ? Tb1 O1 2.328(3) . ? Tb1 O7 2.331(3) . ? Tb1 O8 2.351(3) . ? Tb1 O3 2.407(4) . ? Tb1 O5 2.422(3) . ? Tb1 O4 2.448(3) . ? Tb1 O2 2.492(3) . ? Tb1 C18 2.796(5) . ? Tb1 C13 2.800(5) . ? O1 P1 1.500(3) . ? O2 C13 1.263(6) . ? O3 C13 1.251(6) . ? O4 C18 1.259(6) . ? O5 C18 1.249(6) . ? O6 C21 1.232(5) . ? O7 C21 1.245(5) 2_655 ? O8 C22 1.205(4) . ? P1 C3 1.777(5) . ? P1 C5 1.793(5) . ? P1 C1 1.795(4) . ? C1 C2 1.379(6) . ? C1 C14 1.387(7) 2 ? C2 C17 1.384(6) 2 ? C3 C4 1.386(7) . ? C3 C12 1.389(7) 1_565 ? C4 C9 1.370(7) 1_565 ? C5 C6 1.378(6) . ? C5 C8 1.378(6) . ? C6 C7 1.373(7) . ? C7 C20 1.368(6) 3_675 ? C8 C19 1.386(7) 3_675 ? C9 C4 1.370(7) 1_545 ? C9 C10 1.401(8) . ? C10 C11 1.378(8) . ? C10 C13 1.499(7) . ? C11 C12 1.390(7) . ? C12 C3 1.389(7) 1_545 ? C14 C15 1.360(6) . ? C14 C1 1.387(7) 2 ? C15 C16 1.379(6) . ? C16 C17 1.379(7) . ? C16 C18 1.508(6) . ? C17 C2 1.384(6) 2 ? C19 C20 1.379(6) . ? C19 C8 1.386(7) 3_675 ? C20 C7 1.368(6) 3_675 ? C20 C21 1.504(6) . ? C21 O7 1.245(5) 2_655 ? C22 O8 1.205(4) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Tb1 O1 89.32(13) . . ? O6 Tb1 O7 99.60(13) . . ? O1 Tb1 O7 156.65(12) . . ? O6 Tb1 O8 79.76(14) . . ? O1 Tb1 O8 81.37(12) . . ? O7 Tb1 O8 79.09(13) . . ? O6 Tb1 O3 77.89(14) . . ? O1 Tb1 O3 128.37(11) . . ? O7 Tb1 O3 74.84(13) . . ? O8 Tb1 O3 141.98(12) . . ? O6 Tb1 O5 153.83(14) . . ? O1 Tb1 O5 78.56(12) . . ? O7 Tb1 O5 84.28(13) . . ? O8 Tb1 O5 75.57(12) . . ? O3 Tb1 O5 127.67(12) . . ? O6 Tb1 O4 152.97(15) . . ? O1 Tb1 O4 101.03(12) . . ? O7 Tb1 O4 80.67(13) . . ? O8 Tb1 O4 126.21(13) . . ? O3 Tb1 O4 76.12(12) . . ? O5 Tb1 O4 53.15(12) . . ? O6 Tb1 O2 81.36(13) . . ? O1 Tb1 O2 75.54(11) . . ? O7 Tb1 O2 126.94(12) . . ? O8 Tb1 O2 150.19(13) . . ? O3 Tb1 O2 53.27(11) . . ? O5 Tb1 O2 117.04(11) . . ? O4 Tb1 O2 77.27(12) . . ? O6 Tb1 C18 177.40(14) . . ? O1 Tb1 C18 88.48(13) . . ? O7 Tb1 C18 82.95(14) . . ? O8 Tb1 C18 101.27(14) . . ? O3 Tb1 C18 102.43(15) . . ? O5 Tb1 C18 26.47(13) . . ? O4 Tb1 C18 26.74(14) . . ? O2 Tb1 C18 96.74(14) . . ? O6 Tb1 C13 78.41(15) . . ? O1 Tb1 C13 102.17(14) . . ? O7 Tb1 C13 100.76(16) . . ? O8 Tb1 C13 157.82(13) . . ? O3 Tb1 C13 26.45(13) . . ? O5 Tb1 C13 126.60(13) . . ? O4 Tb1 C13 75.04(14) . . ? O2 Tb1 C13 26.82(13) . . ? C18 Tb1 C13 100.71(15) . . ? P1 O1 Tb1 149.40(19) . . ? C13 O2 Tb1 90.3(3) . . ? C13 O3 Tb1 94.6(3) . . ? C18 O4 Tb1 92.2(3) . . ? C18 O5 Tb1 93.7(3) . . ? C21 O6 Tb1 166.4(4) . . ? C21 O7 Tb1 134.2(3) 2_655 . ? C22 O8 Tb1 148.0(4) . . ? O1 P1 C3 111.4(2) . . ? O1 P1 C5 111.5(2) . . ? C3 P1 C5 107.3(2) . . ? O1 P1 C1 111.5(2) . . ? C3 P1 C1 108.9(2) . . ? C5 P1 C1 106.1(2) . . ? C2 C1 C14 117.9(4) . 2 ? C2 C1 P1 123.1(4) . . ? C14 C1 P1 118.9(3) 2 . ? C1 C2 C17 121.2(5) . 2 ? C4 C3 C12 118.3(5) . 1_565 ? C4 C3 P1 118.0(4) . . ? C12 C3 P1 123.7(4) 1_565 . ? C9 C4 C3 121.1(5) 1_565 . ? C6 C5 C8 118.7(5) . . ? C6 C5 P1 121.3(4) . . ? C8 C5 P1 120.0(4) . . ? C7 C6 C5 120.6(5) . . ? C20 C7 C6 121.1(5) 3_675 . ? C5 C8 C19 120.2(4) . 3_675 ? C4 C9 C10 120.8(6) 1_545 . ? C11 C10 C9 118.3(5) . . ? C11 C10 C13 122.9(5) . . ? C9 C10 C13 118.8(5) . . ? C10 C11 C12 120.7(5) . . ? C3 C12 C11 120.8(5) 1_545 . ? O3 C13 O2 121.9(5) . . ? O3 C13 C10 119.6(5) . . ? O2 C13 C10 118.5(5) . . ? O3 C13 Tb1 59.0(3) . . ? O2 C13 Tb1 62.9(3) . . ? C10 C13 Tb1 178.5(4) . . ? C15 C14 C1 121.4(5) . 2 ? C14 C15 C16 120.3(5) . . ? C17 C16 C15 119.5(4) . . ? C17 C16 C18 119.2(4) . . ? C15 C16 C18 121.3(5) . . ? C16 C17 C2 119.6(4) . 2 ? O5 C18 O4 120.6(4) . . ? O5 C18 C16 120.6(5) . . ? O4 C18 C16 118.7(5) . . ? O5 C18 Tb1 59.8(2) . . ? O4 C18 Tb1 61.0(2) . . ? C16 C18 Tb1 172.0(4) . . ? C20 C19 C8 120.7(4) . 3_675 ? C7 C20 C19 118.6(5) 3_675 . ? C7 C20 C21 119.9(4) 3_675 . ? C19 C20 C21 121.5(4) . . ? O6 C21 O7 124.8(5) . 2_655 ? O6 C21 C20 118.1(4) . . ? O7 C21 C20 117.0(4) 2_655 . ? O8 C22 O8 131.4(8) 2_655 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.737 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.126 # 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 0.019 -0.041 0.019 1685.2 199.3 _platon_squeeze_details ; The contributions of some 199 electrons were removed from the unit-cell contents, and as Z = 2 in this case, this could/might correspond with the removal of solvent such as 2(DMF) and 2(H2O) [some 100 electrons] from the Tb(III)2 formula unit. ;