# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email wxt@fjirsm.ac.cn _publ_contact_author_name 'Xintao Wu' loop_ _publ_author_name 'Ruibiao Fu' 'Shengmin Hu' 'Xintao Wu' data_f1 _database_code_depnum_ccdc_archive 'CCDC 817237' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H26 N3 O17 P4 Zn3' _chemical_formula_weight 864.40 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.655(3) _cell_length_b 9.344(3) _cell_length_c 30.965(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.859(5) _cell_angle_gamma 90.00 _cell_volume 2787.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6862 _cell_measurement_theta_min 3.0363 _cell_measurement_theta_max 27.4719 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 2.876 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6372 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21087 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6381 _reflns_number_gt 5711 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0604P)^2^+14.0503P] 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 6381 _refine_ls_number_parameters 422 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.009 _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 0.53047(6) 0.28510(6) 0.140955(18) 0.02226(15) Uani 1 1 d . . . Zn2 Zn 0.70144(6) 0.54825(6) 0.038172(18) 0.02255(15) Uani 1 1 d . . . Zn3 Zn 0.44079(6) 0.31141(6) 0.307644(17) 0.01823(14) Uani 1 1 d . . . P1 P 0.46114(12) 0.12142(12) 0.22151(4) 0.0154(2) Uani 1 1 d . . . P2 P 0.74526(12) 0.07250(12) 0.18290(4) 0.0164(2) Uani 1 1 d . . . P3 P 0.41330(12) 0.37673(12) 0.05168(4) 0.0173(2) Uani 1 1 d . . . P4 P 0.51896(12) 0.61306(12) 0.11199(4) 0.0172(2) Uani 1 1 d . . . O1 O 0.4084(4) 0.2157(4) 0.18378(11) 0.0266(8) Uani 1 1 d . . . O2 O 0.4015(3) 0.1691(4) 0.26313(11) 0.0217(7) Uani 1 1 d . . . O3 O 0.4317(3) -0.0384(3) 0.21295(11) 0.0217(7) Uani 1 1 d . . . O4 O 0.6757(4) 0.1436(4) 0.14249(11) 0.0282(8) Uani 1 1 d . . . O5 O 0.7282(4) -0.0899(4) 0.18154(12) 0.0235(7) Uani 1 1 d . . . O6 O 0.8957(3) 0.1149(4) 0.19106(12) 0.0251(8) Uani 1 1 d . . . O7 O 0.6904(4) 0.2878(4) 0.22954(12) 0.0260(8) Uani 1 1 d . . . H7 H 0.6485 0.3304 0.2478 0.039 Uiso 1 1 calc R . . O8 O 0.4133(4) 0.2623(4) 0.08650(11) 0.0228(7) Uani 1 1 d . . . O9 O 0.5565(4) 0.3957(4) 0.03404(11) 0.0225(7) Uani 1 1 d . . . O10 O 0.3021(4) 0.3473(4) 0.01562(11) 0.0226(7) Uani 1 1 d . . . O11 O 0.4672(4) 0.7357(4) 0.13919(10) 0.0220(7) Uani 1 1 d . . . O12 O 0.5719(4) 0.4878(4) 0.13949(12) 0.0262(8) Uani 1 1 d . . . O13 O 0.6258(4) 0.6688(4) 0.08224(11) 0.0265(8) Uani 1 1 d . . . O14 O 0.3258(4) 0.6540(4) 0.04550(11) 0.0261(8) Uani 1 1 d . . . H14 H 0.3618 0.6361 0.0229 0.039 Uiso 1 1 calc R . . O15 O 0.1319(10) 0.3553(10) 0.4068(3) 0.111(3) Uani 1 1 d . . . O16 O 0.8867(10) 0.4768(10) 0.3389(4) 0.159(5) Uani 1 1 d . . . O17 O 0.052(2) 0.359(2) 0.4887(6) 0.272(9) Uani 1 1 d U . . N1 N 1.0367(4) -0.1118(5) 0.29854(15) 0.0287(10) Uani 1 1 d . . . H15 H 1.0695 -0.1973 0.2996 0.034 Uiso 1 1 calc R . . N2 N -0.1194(4) 0.4527(5) 0.05946(14) 0.0262(9) Uani 1 1 d . . . C1 C 0.6518(5) 0.1395(5) 0.22925(14) 0.0168(8) Uani 1 1 d . . . C2 C 0.6936(5) 0.0618(6) 0.27236(15) 0.0221(10) Uani 1 1 d . . . H1 H 0.6537 0.1142 0.2955 0.026 Uiso 1 1 calc R . . H2 H 0.6509 -0.0322 0.2712 0.026 Uiso 1 1 calc R . . C3 C 0.8455(5) 0.0428(5) 0.28431(15) 0.0197(9) Uani 1 1 d . . . C4 C 0.9325(6) 0.1565(6) 0.29615(18) 0.0301(11) Uani 1 1 d . . . H3 H 0.8973 0.2492 0.2956 0.036 Uiso 1 1 calc R . . C5 C 1.0704(6) 0.1339(6) 0.3088(2) 0.0367(13) Uani 1 1 d . . . H4 H 1.1281 0.2104 0.3169 0.044 Uiso 1 1 calc R . . C6 C 1.1207(6) -0.0026(7) 0.3093(2) 0.0355(13) Uani 1 1 d . . . H5 H 1.2140 -0.0195 0.3171 0.043 Uiso 1 1 calc R . . C7 C 0.9031(5) -0.0921(5) 0.28619(16) 0.0247(10) Uani 1 1 d . . . H6 H 0.8478 -0.1710 0.2787 0.030 Uiso 1 1 calc R . . C8 C 0.3676(5) 0.5474(5) 0.07770(15) 0.0204(9) Uani 1 1 d . . . C9 C 0.2450(5) 0.5319(6) 0.10713(15) 0.0224(10) Uani 1 1 d . . . H8 H 0.2808 0.4859 0.1337 0.027 Uiso 1 1 calc R . . H9 H 0.2168 0.6276 0.1148 0.027 Uiso 1 1 calc R . . C10 C 0.1149(5) 0.4516(5) 0.09123(15) 0.0229(10) Uani 1 1 d . . . C11 C 0.0962(6) 0.3095(6) 0.10302(19) 0.0317(12) Uani 1 1 d . . . H10 H 0.1677 0.2609 0.1184 0.038 Uiso 1 1 calc R . . C12 C -0.0273(6) 0.2399(6) 0.0922(2) 0.0360(13) Uani 1 1 d . . . H11 H -0.0390 0.1442 0.0993 0.043 Uiso 1 1 calc R . . C13 C -0.1331(6) 0.3157(6) 0.0705(2) 0.0321(12) Uani 1 1 d . . . H12 H -0.2170 0.2697 0.0634 0.039 Uiso 1 1 calc R . . C14 C 0.0035(5) 0.5184(6) 0.06961(17) 0.0256(10) Uani 1 1 d . . . H13 H 0.0132 0.6136 0.0616 0.031 Uiso 1 1 calc R . . N3 N 0.6950(8) 0.4660(9) 0.3958(3) 0.0244(19) Uani 0.50 1 d P A 1 C15 C 0.7423(16) 0.4759(16) 0.4358(5) 0.057(4) Uani 0.50 1 d PDU A 1 C16 C 0.6385(11) 0.4856(11) 0.4698(4) 0.052(4) Uani 0.50 1 d PGD . 1 C17 C 0.4946(12) 0.4897(14) 0.4584(4) 0.076(8) Uani 0.50 1 d PG . 1 C18 C 0.3995(12) 0.4988(18) 0.4909(5) 0.063(5) Uani 0.50 1 d PG . 1 N4 N 0.4484(14) 0.5038(17) 0.5349(5) 0.081(7) Uani 0.50 1 d PGU . 1 C19 C 0.5923(14) 0.4997(14) 0.5463(4) 0.096(10) Uani 0.50 1 d PG . 1 C20 C 0.6873(11) 0.4906(13) 0.5137(4) 0.063(5) Uani 0.50 1 d PG . 1 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 0.0242(3) 0.0209(3) 0.0217(3) 0.0058(2) 0.0015(2) 0.0031(2) Zn2 0.0183(3) 0.0271(3) 0.0218(3) 0.0024(2) -0.0014(2) -0.0011(2) Zn3 0.0200(3) 0.0159(3) 0.0188(3) 0.00180(19) 0.0020(2) 0.0025(2) P1 0.0145(5) 0.0146(5) 0.0171(5) 0.0018(4) 0.0014(4) 0.0008(4) P2 0.0145(5) 0.0148(5) 0.0199(5) 0.0005(4) 0.0019(4) 0.0001(4) P3 0.0186(6) 0.0173(6) 0.0157(5) 0.0002(4) -0.0002(4) -0.0012(4) P4 0.0171(6) 0.0164(6) 0.0179(5) -0.0009(4) -0.0011(4) -0.0008(4) O1 0.0204(18) 0.033(2) 0.0261(18) 0.0147(15) -0.0014(14) 0.0053(15) O2 0.0179(17) 0.0246(17) 0.0227(16) -0.0042(13) 0.0034(13) 0.0013(13) O3 0.0206(17) 0.0160(16) 0.0289(17) -0.0042(13) 0.0058(13) -0.0016(13) O4 0.033(2) 0.032(2) 0.0196(16) 0.0047(14) 0.0016(14) 0.0108(16) O5 0.0223(18) 0.0128(15) 0.0360(19) -0.0016(14) 0.0070(14) 0.0007(13) O6 0.0147(17) 0.0241(18) 0.037(2) -0.0038(15) 0.0057(14) -0.0024(13) O7 0.0241(19) 0.0163(17) 0.039(2) -0.0059(14) 0.0123(15) -0.0039(13) O8 0.0254(18) 0.0219(17) 0.0207(16) 0.0039(13) -0.0015(13) -0.0023(14) O9 0.0218(18) 0.0215(17) 0.0250(17) -0.0016(13) 0.0058(14) -0.0025(13) O10 0.0237(18) 0.0220(17) 0.0213(16) -0.0003(13) -0.0043(13) -0.0056(14) O11 0.0244(18) 0.0223(17) 0.0190(15) -0.0062(13) -0.0010(13) 0.0011(14) O12 0.0278(19) 0.0195(17) 0.0301(18) 0.0030(14) -0.0077(15) 0.0001(14) O13 0.0266(19) 0.0275(19) 0.0261(17) -0.0035(15) 0.0070(14) -0.0088(15) O14 0.034(2) 0.0241(18) 0.0197(16) 0.0048(14) -0.0017(14) 0.0083(15) O15 0.132(7) 0.107(6) 0.096(6) 0.020(5) 0.021(5) 0.022(5) O16 0.161(8) 0.116(7) 0.217(10) -0.103(7) 0.144(8) -0.102(6) O17 0.299(12) 0.259(12) 0.265(11) -0.007(9) 0.079(9) -0.013(9) N1 0.020(2) 0.025(2) 0.040(3) -0.0012(19) -0.0003(18) 0.0086(17) N2 0.018(2) 0.028(2) 0.032(2) 0.0039(18) 0.0010(17) -0.0017(17) C1 0.014(2) 0.017(2) 0.019(2) -0.0002(16) 0.0005(16) -0.0009(17) C2 0.018(2) 0.028(3) 0.020(2) 0.0008(19) 0.0030(17) 0.0036(19) C3 0.018(2) 0.022(2) 0.019(2) -0.0010(17) 0.0004(17) 0.0012(18) C4 0.030(3) 0.020(2) 0.039(3) -0.004(2) -0.006(2) 0.002(2) C5 0.026(3) 0.031(3) 0.051(4) -0.009(3) -0.012(3) -0.002(2) C6 0.022(3) 0.040(3) 0.043(3) -0.003(3) -0.008(2) 0.005(2) C7 0.022(3) 0.021(2) 0.031(2) -0.0023(19) -0.002(2) 0.0027(19) C8 0.021(2) 0.020(2) 0.020(2) -0.0010(17) -0.0013(17) 0.0013(18) C9 0.021(2) 0.028(3) 0.018(2) -0.0036(18) 0.0004(18) 0.0012(19) C10 0.019(2) 0.027(3) 0.022(2) -0.0016(19) 0.0015(18) 0.0005(19) C11 0.023(3) 0.032(3) 0.039(3) 0.008(2) 0.000(2) 0.000(2) C12 0.028(3) 0.027(3) 0.053(4) 0.009(3) 0.001(3) -0.003(2) C13 0.019(3) 0.027(3) 0.050(3) 0.003(2) 0.002(2) -0.005(2) C14 0.023(3) 0.023(2) 0.031(3) 0.002(2) -0.002(2) -0.002(2) N3 0.016(4) 0.033(5) 0.026(4) -0.019(3) 0.017(3) -0.017(3) C15 0.052(7) 0.046(7) 0.076(8) 0.018(6) 0.021(6) -0.006(6) C16 0.058(10) 0.026(6) 0.072(10) -0.001(6) 0.006(8) 0.007(6) C17 0.102(19) 0.034(9) 0.103(17) 0.001(9) 0.086(15) -0.005(10) C18 0.071(12) 0.066(11) 0.057(10) 0.008(8) 0.030(10) 0.001(10) N4 0.098(10) 0.076(10) 0.070(9) 0.008(7) 0.025(8) -0.008(8) C19 0.13(2) 0.060(12) 0.113(18) 0.032(11) 0.096(18) 0.029(14) C20 0.080(13) 0.045(9) 0.066(11) 0.008(8) 0.019(11) 0.006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.926(4) . ? Zn1 O12 1.937(4) . ? Zn1 O1 1.944(4) . ? Zn1 O8 1.978(3) . ? Zn2 O10 1.929(3) 3_665 ? Zn2 O13 1.949(4) . ? Zn2 O9 1.995(3) . ? Zn2 N2 2.017(4) 1_655 ? Zn3 O5 1.923(3) 2_655 ? Zn3 O2 1.935(3) . ? Zn3 O11 1.950(3) 2_645 ? Zn3 O3 2.000(3) 2_655 ? P1 O2 1.514(3) . ? P1 O1 1.523(3) . ? P1 O3 1.539(3) . ? P1 C1 1.848(5) . ? P2 O6 1.511(4) . ? P2 O5 1.527(3) . ? P2 O4 1.531(4) . ? P2 C1 1.855(5) . ? P3 O8 1.519(3) . ? P3 O10 1.521(3) . ? P3 O9 1.531(4) . ? P3 C8 1.854(5) . ? P4 O12 1.516(4) . ? P4 O13 1.521(4) . ? P4 O11 1.527(3) . ? P4 C8 1.852(5) . ? O3 Zn3 2.000(3) 2_645 ? O5 Zn3 1.923(3) 2_645 ? O7 C1 1.435(5) . ? O7 H7 0.8200 . ? O10 Zn2 1.929(3) 3_665 ? O11 Zn3 1.950(3) 2_655 ? O14 C8 1.447(6) . ? O14 H14 0.8200 . ? N1 C6 1.331(7) . ? N1 C7 1.333(7) . ? N1 H15 0.8600 . ? N2 C13 1.334(7) . ? N2 C14 1.354(7) . ? N2 Zn2 2.017(4) 1_455 ? C1 C2 1.549(6) . ? C2 C3 1.499(7) . ? C2 H1 0.9700 . ? C2 H2 0.9700 . ? C3 C7 1.378(7) . ? C3 C4 1.389(7) . ? C4 C5 1.378(8) . ? C4 H3 0.9300 . ? C5 C6 1.365(8) . ? C5 H4 0.9300 . ? C6 H5 0.9300 . ? C7 H6 0.9300 . ? C8 C9 1.549(7) . ? C9 C10 1.516(7) . ? C9 H8 0.9700 . ? C9 H9 0.9700 . ? C10 C14 1.378(7) . ? C10 C11 1.393(7) . ? C11 C12 1.380(8) . ? C11 H10 0.9300 . ? C12 C13 1.380(8) . ? C12 H11 0.9300 . ? C13 H12 0.9300 . ? C14 H13 0.9300 . ? N3 C15 1.294(19) . ? C15 C16 1.505(14) . ? C16 N4 0.85(2) 3_666 ? C16 C18 1.30(2) 3_666 ? C16 C17 1.411(7) . ? C16 C20 1.411(7) . ? C17 N4 0.58(2) 3_666 ? C17 C19 0.85(3) 3_666 ? C17 C18 1.411(7) . ? C17 C18 1.82(2) 3_666 ? C17 C20 2.02(3) 3_666 ? C18 C20 0.85(3) 3_666 ? C18 C19 1.16(3) 3_666 ? C18 C16 1.30(2) 3_666 ? C18 N4 1.411(7) . ? C18 N4 1.72(2) 3_666 ? C18 C17 1.82(3) 3_666 ? C18 C18 1.983(18) 3_666 ? N4 C17 0.58(3) 3_666 ? N4 C16 0.847(16) 3_666 ? N4 C19 1.411(7) . ? N4 C18 1.719(18) 3_666 ? N4 C20 1.93(3) 3_666 ? C19 C17 0.85(3) 3_666 ? C19 C18 1.16(2) 3_666 ? C19 C20 1.411(7) . ? C20 C18 0.847(18) 3_666 ? C20 N4 1.93(2) 3_666 ? C20 C17 2.02(2) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O12 121.40(17) . . ? O4 Zn1 O1 103.19(15) . . ? O12 Zn1 O1 118.53(16) . . ? O4 Zn1 O8 108.71(15) . . ? O12 Zn1 O8 101.11(14) . . ? O1 Zn1 O8 101.96(15) . . ? O10 Zn2 O13 109.06(16) 3_665 . ? O10 Zn2 O9 109.52(14) 3_665 . ? O13 Zn2 O9 99.40(14) . . ? O10 Zn2 N2 118.11(16) 3_665 1_655 ? O13 Zn2 N2 112.35(17) . 1_655 ? O9 Zn2 N2 106.69(16) . 1_655 ? O5 Zn3 O2 109.00(15) 2_655 . ? O5 Zn3 O11 111.75(15) 2_655 2_645 ? O2 Zn3 O11 114.12(15) . 2_645 ? O5 Zn3 O3 105.48(14) 2_655 2_655 ? O2 Zn3 O3 110.54(14) . 2_655 ? O11 Zn3 O3 105.57(14) 2_645 2_655 ? O2 P1 O1 110.9(2) . . ? O2 P1 O3 110.82(19) . . ? O1 P1 O3 112.4(2) . . ? O2 P1 C1 107.2(2) . . ? O1 P1 C1 109.0(2) . . ? O3 P1 C1 106.4(2) . . ? O6 P2 O5 111.5(2) . . ? O6 P2 O4 112.8(2) . . ? O5 P2 O4 111.6(2) . . ? O6 P2 C1 107.1(2) . . ? O5 P2 C1 107.4(2) . . ? O4 P2 C1 106.0(2) . . ? O8 P3 O10 111.1(2) . . ? O8 P3 O9 112.2(2) . . ? O10 P3 O9 111.6(2) . . ? O8 P3 C8 106.6(2) . . ? O10 P3 C8 107.3(2) . . ? O9 P3 C8 107.6(2) . . ? O12 P4 O13 112.8(2) . . ? O12 P4 O11 112.4(2) . . ? O13 P4 O11 109.8(2) . . ? O12 P4 C8 106.8(2) . . ? O13 P4 C8 107.9(2) . . ? O11 P4 C8 106.8(2) . . ? P1 O1 Zn1 122.0(2) . . ? P1 O2 Zn3 137.8(2) . . ? P1 O3 Zn3 128.7(2) . 2_645 ? P2 O4 Zn1 126.6(2) . . ? P2 O5 Zn3 124.3(2) . 2_645 ? C1 O7 H7 109.5 . . ? P3 O8 Zn1 120.1(2) . . ? P3 O9 Zn2 135.0(2) . . ? P3 O10 Zn2 120.9(2) . 3_665 ? P4 O11 Zn3 126.2(2) . 2_655 ? P4 O12 Zn1 134.9(2) . . ? P4 O13 Zn2 121.9(2) . . ? C8 O14 H14 109.5 . . ? C6 N1 C7 121.9(5) . . ? C6 N1 H15 119.1 . . ? C7 N1 H15 119.1 . . ? C13 N2 C14 118.4(5) . . ? C13 N2 Zn2 114.3(4) . 1_455 ? C14 N2 Zn2 126.4(4) . 1_455 ? O7 C1 C2 113.2(4) . . ? O7 C1 P1 110.2(3) . . ? C2 C1 P1 105.6(3) . . ? O7 C1 P2 101.0(3) . . ? C2 C1 P2 113.3(3) . . ? P1 C1 P2 113.6(2) . . ? C3 C2 C1 117.5(4) . . ? C3 C2 H1 107.9 . . ? C1 C2 H1 107.9 . . ? C3 C2 H2 107.9 . . ? C1 C2 H2 107.9 . . ? H1 C2 H2 107.2 . . ? C7 C3 C4 117.0(5) . . ? C7 C3 C2 120.3(4) . . ? C4 C3 C2 122.7(4) . . ? C5 C4 C3 120.9(5) . . ? C5 C4 H3 119.5 . . ? C3 C4 H3 119.5 . . ? C6 C5 C4 118.9(5) . . ? C6 C5 H4 120.6 . . ? C4 C5 H4 120.6 . . ? N1 C6 C5 120.2(5) . . ? N1 C6 H5 119.9 . . ? C5 C6 H5 119.9 . . ? N1 C7 C3 121.2(5) . . ? N1 C7 H6 119.4 . . ? C3 C7 H6 119.4 . . ? O14 C8 C9 106.3(4) . . ? O14 C8 P4 109.9(3) . . ? C9 C8 P4 107.4(3) . . ? O14 C8 P3 110.9(3) . . ? C9 C8 P3 112.9(3) . . ? P4 C8 P3 109.4(2) . . ? C10 C9 C8 120.3(4) . . ? C10 C9 H8 107.2 . . ? C8 C9 H8 107.2 . . ? C10 C9 H9 107.2 . . ? C8 C9 H9 107.2 . . ? H8 C9 H9 106.9 . . ? C14 C10 C11 116.6(5) . . ? C14 C10 C9 122.4(5) . . ? C11 C10 C9 120.4(5) . . ? C12 C11 C10 120.7(5) . . ? C12 C11 H10 119.6 . . ? C10 C11 H10 119.6 . . ? C13 C12 C11 118.4(5) . . ? C13 C12 H11 120.8 . . ? C11 C12 H11 120.8 . . ? N2 C13 C12 122.3(5) . . ? N2 C13 H12 118.8 . . ? C12 C13 H12 118.8 . . ? N2 C14 C10 123.4(5) . . ? N2 C14 H13 118.3 . . ? C10 C14 H13 118.3 . . ? N3 C15 C16 117.7(13) . . ? N4 C16 C18 79.0(15) 3_666 3_666 ? N4 C16 C17 6.9(15) 3_666 . ? C18 C16 C17 84.0(8) 3_666 . ? N4 C16 C20 115.1(15) 3_666 . ? C18 C16 C20 36.1(8) 3_666 . ? C17 C16 C20 120.0 . . ? N4 C16 C15 126(2) 3_666 . ? C18 C16 C15 154.6(14) 3_666 . ? C17 C16 C15 121.2(11) . . ? C20 C16 C15 118.8(11) . . ? N4 C17 C19 163(4) 3_666 3_666 ? N4 C17 C16 10(2) 3_666 . ? C19 C17 C16 173(2) 3_666 . ? N4 C17 C18 113(2) 3_666 . ? C19 C17 C18 55(2) 3_666 . ? C16 C17 C18 120.0 . . ? N4 C17 C18 38(2) 3_666 3_666 ? C19 C17 C18 129(2) 3_666 3_666 ? C16 C17 C18 45.4(5) . 3_666 ? C18 C17 C18 74.6(5) . 3_666 ? N4 C17 C20 132(3) 3_666 3_666 ? C19 C17 C20 35.1(12) 3_666 3_666 ? C16 C17 C20 140.0(11) . 3_666 ? C18 C17 C20 20.2(11) . 3_666 ? C18 C17 C20 94.6(11) 3_666 3_666 ? C20 C18 C19 88(2) 3_666 3_666 ? C20 C18 C16 79(2) 3_666 3_666 ? C19 C18 C16 166(2) 3_666 3_666 ? C20 C18 N4 115(3) 3_666 . ? C19 C18 N4 156.5(14) 3_666 . ? C16 C18 N4 36.1(8) 3_666 . ? C20 C18 C17 125(3) 3_666 . ? C19 C18 C17 36.9(14) 3_666 . ? C16 C18 C17 155.8(8) 3_666 . ? N4 C18 C17 120.0 . . ? C20 C18 N4 142(3) 3_666 3_666 ? C19 C18 N4 54.6(10) 3_666 3_666 ? C16 C18 N4 137.7(15) 3_666 3_666 ? N4 C18 N4 102.0(8) . 3_666 ? C17 C18 N4 18.1(8) . 3_666 ? C20 C18 C17 129(3) 3_666 3_666 ? C19 C18 C17 141.7(17) 3_666 3_666 ? C16 C18 C17 50.5(8) 3_666 3_666 ? N4 C18 C17 14.8(7) . 3_666 ? C17 C18 C17 105.4(7) . 3_666 ? N4 C18 C17 87.4(11) 3_666 3_666 ? C20 C18 C18 170(3) 3_666 3_666 ? C19 C18 C18 98.6(14) 3_666 3_666 ? C16 C18 C18 93.8(11) 3_666 3_666 ? N4 C18 C18 58.0(6) . 3_666 ? C17 C18 C18 62.1(6) . 3_666 ? N4 C18 C18 44.1(5) 3_666 3_666 ? C17 C18 C18 43.3(6) 3_666 3_666 ? C17 N4 C16 163(4) 3_666 3_666 ? C17 N4 C18 127(2) 3_666 . ? C16 N4 C18 64.9(15) 3_666 . ? C17 N4 C19 10(3) 3_666 . ? C16 N4 C19 173.1(16) 3_666 . ? C18 N4 C19 120.0 . . ? C17 N4 C18 49(2) 3_666 3_666 ? C16 N4 C18 142(2) 3_666 3_666 ? C18 N4 C18 78.0(7) . 3_666 ? C19 N4 C18 42.1(7) . 3_666 ? C17 N4 C20 149(3) 3_666 3_666 ? C16 N4 C20 41.5(11) 3_666 3_666 ? C18 N4 C20 23.4(10) . 3_666 ? C19 N4 C20 143.3(10) . 3_666 ? C18 N4 C20 101.2(14) 3_666 3_666 ? C17 C19 C18 88(2) 3_666 3_666 ? C17 C19 N4 7(2) 3_666 . ? C18 C19 N4 83.3(8) 3_666 . ? C17 C19 C20 124.7(17) 3_666 . ? C18 C19 C20 36.9(8) 3_666 . ? N4 C19 C20 120.0 . . ? C18 C20 C19 55.3(14) 3_666 . ? C18 C20 C16 64.9(14) 3_666 . ? C19 C20 C16 120.0 . . ? C18 C20 N4 41.5(13) 3_666 3_666 ? C19 C20 N4 96.7(6) . 3_666 ? C16 C20 N4 23.4(6) . 3_666 ? C18 C20 C17 35.1(12) 3_666 3_666 ? C19 C20 C17 20.2(8) . 3_666 ? C16 C20 C17 99.9(8) . 3_666 ? N4 C20 C17 76.5(7) 3_666 3_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14 O9 0.82 2.00 2.820(5) 176.1 3_665 N1 H15 O6 0.86 1.81 2.651(6) 166.8 2_745 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.184 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.145 # Attachment '- 4.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 838869' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16.50 H27 N3 O17 P4 Zn3' _chemical_formula_weight 859.40 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.646(3) _cell_length_b 9.410(3) _cell_length_c 30.929(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.338(5) _cell_angle_gamma 90.00 _cell_volume 2802.7(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7155 _cell_measurement_theta_min 3.0257 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 2.860 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7250 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20618 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6373 _reflns_number_gt 5740 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0578P)^2^+39.7608P] 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 6373 _refine_ls_number_parameters 386 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.1864 _refine_ls_wR_factor_gt 0.1820 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.115 _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 0.03557(9) 0.27106(9) 0.14027(3) 0.0248(2) Uani 1 1 d . . . Zn2 Zn 0.21463(9) 0.55604(13) 0.03969(3) 0.0370(3) Uani 1 1 d . . . Zn3 Zn 0.06167(8) -0.19789(8) 0.19345(2) 0.0207(2) Uani 1 1 d . . . P1 P -0.03751(16) 0.11013(17) 0.22080(5) 0.0154(3) Uani 1 1 d . . . P2 P 0.24892(18) 0.06078(17) 0.18270(6) 0.0186(3) Uani 1 1 d . . . P3 P -0.07259(18) 0.37431(19) 0.05042(5) 0.0204(4) Uani 1 1 d . . . P4 P 0.02478(18) 0.59927(18) 0.11450(5) 0.0184(3) Uani 1 1 d . . . O1 O -0.0890(5) 0.1984(6) 0.18205(17) 0.0292(12) Uani 1 1 d . . . O2 O -0.0658(5) -0.0489(5) 0.21381(16) 0.0229(10) Uani 1 1 d . . . O3 O -0.0998(5) 0.1620(5) 0.26185(15) 0.0229(10) Uani 1 1 d . . . O4 O 0.1806(6) 0.1301(6) 0.14180(16) 0.0293(11) Uani 1 1 d . . . O5 O 0.3983(5) 0.1036(6) 0.19050(19) 0.0315(12) Uani 1 1 d . . . O6 O 0.2304(6) -0.1006(5) 0.18157(18) 0.0308(12) Uani 1 1 d . . . O7 O 0.1914(5) 0.2757(5) 0.22864(17) 0.0253(11) Uani 1 1 d . . . H7 H 0.1485 0.3182 0.2468 0.038 Uiso 1 1 calc R . . O8 O -0.0684(6) 0.2543(6) 0.08325(17) 0.0342(13) Uani 1 1 d . . . O9 O 0.0696(5) 0.3996(5) 0.03312(15) 0.0241(10) Uani 1 1 d . . . O10 O -0.1826(5) 0.3433(6) 0.01447(16) 0.0271(11) Uani 1 1 d . . . O11 O -0.0304(6) 0.7159(6) 0.14241(16) 0.0309(12) Uani 1 1 d . . . O12 O 0.1339(6) 0.6591(6) 0.08580(17) 0.0314(12) Uani 1 1 d . . . O13 O 0.0779(5) 0.4724(5) 0.14067(17) 0.0272(11) Uani 1 1 d . . . O14 O -0.1655(6) 0.6453(6) 0.04797(16) 0.0326(12) Uani 1 1 d . . . H14 H -0.1346 0.6272 0.0245 0.049 Uiso 1 1 calc R . . O15 O 0.465(5) 0.864(4) 0.1094(14) 0.24(3) Uani 0.50 1 d P . . O16 O 0.360(2) 0.812(3) 0.0584(14) 0.169(17) Uani 0.50 1 d P . . O17 O 0.798(2) 0.935(2) 0.1096(7) 0.216(10) Uani 1 1 d . . . O18 O 0.6313(15) 0.9758(18) 0.1650(7) 0.178(8) Uani 1 1 d . . . N1 N 0.5330(7) -0.1216(8) 0.2991(2) 0.0353(16) Uani 1 1 d . . . H15 H 0.5654 -0.2067 0.3000 0.042 Uiso 1 1 calc R . . N2 N -0.6082(6) 0.4521(8) 0.0573(2) 0.0345(15) Uani 1 1 d . . . N3 N 0.906(3) 0.986(3) 0.0389(9) 0.208(11) Uiso 1 1 d D . . C1 C 0.1533(6) 0.1284(7) 0.2285(2) 0.0173(12) Uani 1 1 d . . . C2 C 0.1935(7) 0.0544(8) 0.2723(2) 0.0223(14) Uani 1 1 d . . . H2 H 0.1544 0.1098 0.2951 0.027 Uiso 1 1 calc R . . H1 H 0.1485 -0.0378 0.2720 0.027 Uiso 1 1 calc R . . C3 C 0.3443(7) 0.0322(8) 0.2845(2) 0.0231(14) Uani 1 1 d . . . C4 C 0.4327(8) 0.1437(9) 0.2968(3) 0.0335(17) Uani 1 1 d . . . H3 H 0.3985 0.2362 0.2961 0.040 Uiso 1 1 calc R . . C5 C 0.5706(9) 0.1202(10) 0.3100(3) 0.043(2) Uani 1 1 d . . . H4 H 0.6291 0.1954 0.3180 0.052 Uiso 1 1 calc R . . C6 C 0.6179(8) -0.0156(10) 0.3108(3) 0.040(2) Uani 1 1 d . . . H5 H 0.7099 -0.0345 0.3196 0.048 Uiso 1 1 calc R . . C7 C 0.3997(8) -0.1029(8) 0.2861(2) 0.0282(15) Uani 1 1 d . . . H6 H 0.3446 -0.1807 0.2782 0.034 Uiso 1 1 calc R . . C8 C -0.1231(7) 0.5359(8) 0.0788(2) 0.0205(13) Uani 1 1 d . . . C9 C -0.2461(7) 0.5133(10) 0.1080(2) 0.0336(18) Uani 1 1 d . . . H9 H -0.2111 0.4607 0.1333 0.040 Uiso 1 1 calc R . . H8 H -0.2740 0.6061 0.1180 0.040 Uiso 1 1 calc R . . C10 C -0.3765(7) 0.4378(9) 0.0900(3) 0.0314(17) Uani 1 1 d . . . C11 C -0.3953(10) 0.2974(12) 0.0979(5) 0.068(4) Uani 1 1 d . . . H10 H -0.3239 0.2434 0.1111 0.081 Uiso 1 1 calc R . . C12 C -0.5198(11) 0.2370(13) 0.0865(6) 0.086(5) Uani 1 1 d . . . H11 H -0.5346 0.1417 0.0926 0.103 Uiso 1 1 calc R . . C13 C -0.6246(10) 0.3157(12) 0.0658(5) 0.073(4) Uani 1 1 d . . . H12 H -0.7085 0.2719 0.0577 0.087 Uiso 1 1 calc R . . C14 C -0.4875(8) 0.5122(9) 0.0703(2) 0.0289(16) Uani 1 1 d . . . H13 H -0.4770 0.6092 0.0659 0.035 Uiso 1 1 calc R . . C15 C 1.144(3) 1.022(3) 0.0070(9) 0.166(10) Uiso 1 1 d D . . C16 C 1.066(3) 0.968(4) 0.0359(9) 0.190(12) Uiso 1 1 d D . . C17 C 1.119(4) 0.971(8) 0.0818(10) 0.25(3) Uiso 0.50 1 d PD . . 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 0.0277(4) 0.0217(4) 0.0242(4) 0.0079(3) -0.0053(3) -0.0039(3) Zn2 0.0240(4) 0.0669(7) 0.0202(4) 0.0087(4) 0.0014(3) 0.0174(4) Zn3 0.0295(4) 0.0145(4) 0.0184(4) -0.0016(3) 0.0041(3) -0.0007(3) P1 0.0159(7) 0.0131(7) 0.0169(7) 0.0011(6) -0.0013(6) 0.0003(6) P2 0.0206(8) 0.0122(7) 0.0237(8) 0.0007(6) 0.0060(6) 0.0015(6) P3 0.0232(8) 0.0204(8) 0.0168(8) 0.0010(6) -0.0047(6) -0.0034(7) P4 0.0207(8) 0.0184(8) 0.0159(7) -0.0025(6) -0.0015(6) 0.0018(6) O1 0.024(3) 0.033(3) 0.030(3) 0.017(2) -0.003(2) 0.002(2) O2 0.023(2) 0.017(2) 0.029(2) -0.0055(19) 0.0064(19) -0.0026(19) O3 0.023(2) 0.020(2) 0.026(2) -0.0061(19) 0.0043(19) 0.0014(19) O4 0.039(3) 0.027(3) 0.022(2) 0.002(2) 0.006(2) 0.008(2) O5 0.023(3) 0.026(3) 0.047(3) 0.003(2) 0.011(2) 0.001(2) O6 0.040(3) 0.010(2) 0.044(3) 0.000(2) 0.020(2) 0.003(2) O7 0.024(2) 0.013(2) 0.040(3) -0.007(2) 0.012(2) -0.0058(19) O8 0.045(3) 0.031(3) 0.025(3) 0.010(2) -0.015(2) -0.014(2) O9 0.019(2) 0.030(3) 0.024(2) -0.005(2) 0.0006(18) 0.001(2) O10 0.028(3) 0.026(3) 0.026(2) 0.003(2) -0.010(2) -0.012(2) O11 0.038(3) 0.036(3) 0.018(2) -0.010(2) -0.007(2) 0.017(2) O12 0.040(3) 0.029(3) 0.026(3) -0.007(2) 0.010(2) -0.014(2) O13 0.026(3) 0.022(2) 0.032(3) 0.002(2) -0.011(2) 0.003(2) O14 0.042(3) 0.036(3) 0.019(2) 0.003(2) -0.002(2) 0.011(3) O15 0.27(4) 0.17(3) 0.28(4) 0.18(3) 0.24(4) 0.18(3) O16 0.068(14) 0.086(16) 0.36(5) 0.14(2) 0.04(2) 0.017(12) O17 0.190(18) 0.194(19) 0.26(2) 0.010(17) -0.011(17) 0.107(16) O18 0.103(10) 0.146(14) 0.29(2) 0.056(15) 0.059(13) 0.046(10) N1 0.024(3) 0.038(4) 0.044(4) -0.010(3) -0.001(3) 0.015(3) N2 0.016(3) 0.042(4) 0.045(4) 0.012(3) -0.004(3) 0.001(3) C1 0.017(3) 0.014(3) 0.021(3) 0.001(2) 0.000(2) 0.004(2) C2 0.014(3) 0.029(4) 0.024(3) 0.005(3) -0.001(2) 0.006(3) C3 0.018(3) 0.030(4) 0.020(3) 0.002(3) -0.002(2) 0.000(3) C4 0.031(4) 0.027(4) 0.041(4) -0.001(3) -0.008(3) 0.001(3) C5 0.026(4) 0.039(5) 0.063(6) -0.008(4) -0.012(4) -0.004(4) C6 0.022(4) 0.047(5) 0.050(5) -0.011(4) -0.010(3) 0.008(4) C7 0.024(3) 0.030(4) 0.029(4) -0.005(3) -0.006(3) 0.004(3) C8 0.014(3) 0.030(4) 0.016(3) -0.002(3) -0.001(2) 0.002(3) C9 0.020(3) 0.059(5) 0.023(3) -0.001(3) 0.002(3) 0.004(3) C10 0.017(3) 0.046(5) 0.031(4) 0.011(3) 0.003(3) 0.002(3) C11 0.024(4) 0.056(7) 0.121(10) 0.047(7) -0.012(5) 0.000(4) C12 0.033(5) 0.055(7) 0.166(15) 0.051(8) -0.020(7) -0.013(5) C13 0.020(4) 0.045(6) 0.150(13) 0.029(7) -0.016(6) -0.009(4) C14 0.025(4) 0.036(4) 0.025(3) 0.002(3) 0.001(3) 0.003(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 O4 1.926(5) . ? Zn1 O13 1.938(5) . ? Zn1 O1 1.939(5) . ? Zn1 O8 1.984(5) . ? Zn2 O12 1.926(5) . ? Zn2 O10 1.934(5) 3_565 ? Zn2 N2 2.016(6) 1_655 ? Zn2 O9 2.033(5) . ? Zn3 O6 1.922(5) . ? Zn3 O3 1.930(5) 2_545 ? Zn3 O11 1.943(5) 1_545 ? Zn3 O2 1.991(5) . ? P1 O3 1.517(5) . ? P1 O1 1.518(5) . ? P1 O2 1.534(5) . ? P1 C1 1.851(6) . ? P2 O5 1.502(6) . ? P2 O6 1.529(5) . ? P2 O4 1.537(5) . ? P2 C1 1.848(7) . ? P3 O8 1.518(5) . ? P3 O9 1.520(5) . ? P3 O10 1.520(5) . ? P3 C8 1.836(7) . ? P4 O11 1.513(5) . ? P4 O13 1.515(5) . ? P4 O12 1.524(5) . ? P4 C8 1.850(7) . ? O3 Zn3 1.930(5) 2 ? O7 C1 1.434(8) . ? O10 Zn2 1.934(5) 3_565 ? O11 Zn3 1.943(5) 1_565 ? O14 C8 1.447(8) . ? N1 C6 1.327(11) . ? N1 C7 1.336(9) . ? N2 C13 1.322(12) . ? N2 C14 1.335(10) . ? N2 Zn2 2.016(6) 1_455 ? N3 C15 1.48(3) 3_775 ? N3 C16 1.561(18) . ? C1 C2 1.551(9) . ? C2 C3 1.496(9) . ? C3 C7 1.379(10) . ? C3 C4 1.391(10) . ? C4 C5 1.387(11) . ? C5 C6 1.357(13) . ? C8 C9 1.546(9) . ? C9 C10 1.521(11) . ? C10 C11 1.358(13) . ? C10 C14 1.389(10) . ? C11 C12 1.356(14) . ? C12 C13 1.380(15) . ? C15 C16 1.30(3) . ? C15 N3 1.48(3) 3_775 ? C16 C17 1.479(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O13 121.4(2) . . ? O4 Zn1 O1 102.6(2) . . ? O13 Zn1 O1 118.6(2) . . ? O4 Zn1 O8 107.2(2) . . ? O13 Zn1 O8 100.3(2) . . ? O1 Zn1 O8 105.3(2) . . ? O12 Zn2 O10 110.1(2) . 3_565 ? O12 Zn2 N2 114.7(3) . 1_655 ? O10 Zn2 N2 124.2(3) 3_565 1_655 ? O12 Zn2 O9 97.6(2) . . ? O10 Zn2 O9 101.2(2) 3_565 . ? N2 Zn2 O9 104.1(3) 1_655 . ? O6 Zn3 O3 109.5(2) . 2_545 ? O6 Zn3 O11 113.3(2) . 1_545 ? O3 Zn3 O11 110.8(2) 2_545 1_545 ? O6 Zn3 O2 105.7(2) . . ? O3 Zn3 O2 110.5(2) 2_545 . ? O11 Zn3 O2 106.8(2) 1_545 . ? O3 P1 O1 111.0(3) . . ? O3 P1 O2 110.8(3) . . ? O1 P1 O2 112.0(3) . . ? O3 P1 C1 107.5(3) . . ? O1 P1 C1 109.2(3) . . ? O2 P1 C1 106.1(3) . . ? O5 P2 O6 112.3(3) . . ? O5 P2 O4 112.3(3) . . ? O6 P2 O4 111.0(3) . . ? O5 P2 C1 107.5(3) . . ? O6 P2 C1 107.3(3) . . ? O4 P2 C1 106.0(3) . . ? O8 P3 O9 111.3(3) . . ? O8 P3 O10 109.6(3) . . ? O9 P3 O10 112.3(3) . . ? O8 P3 C8 107.1(3) . . ? O9 P3 C8 108.0(3) . . ? O10 P3 C8 108.4(3) . . ? O11 P4 O13 112.7(3) . . ? O11 P4 O12 110.0(3) . . ? O13 P4 O12 112.2(3) . . ? O11 P4 C8 106.8(3) . . ? O13 P4 C8 106.8(3) . . ? O12 P4 C8 107.8(3) . . ? P1 O1 Zn1 122.1(3) . . ? P1 O2 Zn3 128.5(3) . . ? P1 O3 Zn3 138.7(3) . 2 ? P2 O4 Zn1 126.0(3) . . ? P2 O6 Zn3 124.6(3) . . ? P3 O8 Zn1 121.8(3) . . ? P3 O9 Zn2 135.1(3) . . ? P3 O10 Zn2 127.5(3) . 3_565 ? P4 O11 Zn3 127.4(3) . 1_565 ? P4 O12 Zn2 124.6(3) . . ? P4 O13 Zn1 134.6(3) . . ? C6 N1 C7 123.4(7) . . ? C13 N2 C14 117.6(7) . . ? C13 N2 Zn2 114.5(6) . 1_455 ? C14 N2 Zn2 125.9(6) . 1_455 ? C15 N3 C16 102(2) 3_775 . ? O7 C1 C2 112.4(5) . . ? O7 C1 P2 101.3(4) . . ? C2 C1 P2 113.8(4) . . ? O7 C1 P1 110.1(4) . . ? C2 C1 P1 105.5(4) . . ? P2 C1 P1 113.9(3) . . ? C3 C2 C1 118.2(6) . . ? C7 C3 C4 117.1(6) . . ? C7 C3 C2 120.5(7) . . ? C4 C3 C2 122.4(7) . . ? C5 C4 C3 121.5(8) . . ? C6 C5 C4 118.2(8) . . ? N1 C6 C5 120.1(7) . . ? N1 C7 C3 119.8(7) . . ? O14 C8 C9 106.6(6) . . ? O14 C8 P3 110.3(4) . . ? C9 C8 P3 113.5(6) . . ? O14 C8 P4 110.1(5) . . ? C9 C8 P4 106.7(4) . . ? P3 C8 P4 109.6(3) . . ? C10 C9 C8 119.8(6) . . ? C11 C10 C14 117.5(8) . . ? C11 C10 C9 120.3(8) . . ? C14 C10 C9 121.7(8) . . ? C12 C11 C10 119.1(9) . . ? C11 C12 C13 120.6(10) . . ? N2 C13 C12 121.4(9) . . ? N2 C14 C10 123.7(8) . . ? C16 C15 N3 118(3) . 3_775 ? C15 C16 C17 118(2) . . ? C15 C16 N3 128(3) . . ? C17 C16 N3 103.0(16) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.709 _refine_diff_density_min -3.084 _refine_diff_density_rms 0.188