# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 1145/271 data_data _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H23 N2 O12 P3 Zn1' _chemical_formula_weight 473.4 _chemical_melting_point ? _chemical_compound_source ? 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6272(2) _cell_length_b 8.8949(2) _cell_length_c 12.6742(2) _cell_angle_alpha 88.9430(10) _cell_angle_beta 75.1700(10) _cell_angle_gamma 63.0650(10) _cell_volume 832.82(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.223 _exptl_crystal_density_method ? _exptl_crystal_F_000 244 _exptl_absorpt_coefficient_mu 6.085 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3555 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 23.24 _reflns_number_total 2369 _reflns_number_observed 2346 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+1.9306P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0592(52) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2368 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_obs 0.0480 _refine_ls_wR_factor_all 0.1313 _refine_ls_wR_factor_obs 0.1307 _refine_ls_goodness_of_fit_all 1.084 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.084 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.25672(6) 0.51918(6) 0.15374(4) 0.0188(3) Uani 1 d . . P1 P -0.14147(14) 0.77138(13) 0.31228(9) 0.0186(3) Uani 1 d . . P2 P 0.64516(15) 0.48170(13) 0.10942(9) 0.0171(3) Uani 1 d . . P3 P 0.38669(15) 0.22294(13) 0.30133(9) 0.0175(3) Uani 1 d . . O1 O 0.0198(4) 0.7054(4) 0.2141(3) 0.0318(8) Uani 1 d . . O2 O 0.2999(5) 0.4569(4) -0.0014(3) 0.0292(8) Uani 1 d . . O3 O 0.4455(4) 0.5760(4) 0.1685(3) 0.0284(8) Uani 1 d . . O4 O 0.2871(4) 0.3046(4) 0.2141(3) 0.0218(7) Uani 1 d . . O5 O 0.2969(4) 0.3315(4) 0.4105(3) 0.0262(7) Uani 1 d . . O6 O 0.5871(4) 0.1784(4) 0.2590(3) 0.0278(8) Uani 1 d . . O7 O 0.3750(4) 0.0500(4) 0.3134(3) 0.0278(8) Uani 1 d . . H20 H 0.4266(4) -0.0007(4) 0.3588(3) 0.042 Uiso 1 calc R . O8 O 0.7076(4) 0.2869(4) 0.0880(3) 0.0239(7) Uani 1 d . . H21 H 0.6787(4) 0.2514(4) 0.1461(3) 0.036 Uiso 1 calc R . O9 O 0.7568(4) 0.4910(4) 0.1869(3) 0.0281(8) Uani 1 d . . H22 H 0.7372(4) 0.5895(4) 0.1978(3) 0.042 Uiso 1 calc R . O10 O -0.0800(5) 0.6667(4) 0.4073(3) 0.0317(8) Uani 1 d . . H23 H -0.1657(5) 0.6997(4) 0.4629(3) 0.048 Uiso 1 calc R . O11 O -0.3060(4) 0.7686(4) 0.2924(3) 0.0270(8) Uani 1 d . . O12 O -0.1919(5) 0.9582(4) 0.3525(3) 0.0302(8) Uani 1 d . . H24 H -0.2153(5) 1.0183(4) 0.3031(3) 0.045 Uiso 1 calc R . N1 N 0.2549(5) 0.6377(5) 0.4968(3) 0.0277(9) Uani 1 d . . H3 H 0.2447(5) 0.5587(5) 0.4585(3) 0.033 Uiso 1 calc R . C1 C 0.4122(8) 0.5456(8) 0.5461(5) 0.0423(13) Uani 1 d . . H2 H 0.3922(8) 0.4640(8) 0.5919(5) 0.051 Uiso 1 calc R . H1 H 0.4208(8) 0.6264(8) 0.5916(5) 0.051 Uiso 1 calc R . C2 C 0.2623(9) 0.7677(8) 0.4236(5) 0.0430(14) Uani 1 d . . H6 H 0.3676(9) 0.7156(8) 0.3618(5) 0.064 Uiso 1 calc R . H5 H 0.2684(9) 0.8548(8) 0.4633(5) 0.064 Uiso 1 calc R . H4 H 0.1557(9) 0.8168(8) 0.3983(5) 0.064 Uiso 1 calc R . C3 C 0.0911(8) 0.7174(7) 0.5938(5) 0.0399(13) Uani 1 d . . H9 H 0.0874(8) 0.6325(7) 0.6407(5) 0.060 Uiso 1 calc R . H8 H -0.0159(8) 0.7665(7) 0.5688(5) 0.060 Uiso 1 calc R . H7 H 0.0969(8) 0.8044(7) 0.6339(5) 0.060 Uiso 1 calc R . N2 N 1.2485(5) 0.0896(5) 0.0736(3) 0.0235(8) Uani 1 d . . H12 H 1.2430(5) 0.1732(5) 0.1171(3) 0.028 Uiso 1 calc R . C4 C 1.4418(6) -0.0394(6) 0.0315(4) 0.0251(10) Uani 1 d . . H11 H 1.4511(6) -0.1285(6) -0.0165(4) 0.030 Uiso 1 calc R . H10 H 1.4871(6) -0.0903(6) 0.0927(4) 0.030 Uiso 1 calc R . C5 C 1.1428(7) 0.0101(7) 0.1433(4) 0.0344(12) Uani 1 d . . H15 H 1.0182(7) 0.0935(7) 0.1704(4) 0.052 Uiso 1 calc R . H14 H 1.1913(7) -0.0319(7) 0.2041(4) 0.052 Uiso 1 calc R . H13 H 1.1514(7) -0.0821(7) 0.0999(4) 0.052 Uiso 1 calc R . C6 C 1.1631(7) 0.1698(7) -0.0162(5) 0.0348(12) Uani 1 d . . H18 H 1.0391(7) 0.2515(7) 0.0158(5) 0.052 Uiso 1 calc R . H17 H 1.1684(7) 0.0836(7) -0.0635(5) 0.052 Uiso 1 calc R . H16 H 1.2275(7) 0.2253(7) -0.0580(5) 0.052 Uiso 1 calc R . 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 0.0189(4) 0.0136(4) 0.0241(4) 0.0075(2) -0.0096(2) -0.0059(3) P1 0.0168(6) 0.0125(6) 0.0261(6) 0.0056(5) -0.0105(5) -0.0043(5) P2 0.0198(6) 0.0142(6) 0.0203(6) 0.0049(5) -0.0096(5) -0.0083(5) P3 0.0203(6) 0.0109(6) 0.0235(6) 0.0085(4) -0.0108(5) -0.0068(5) O1 0.021(2) 0.024(2) 0.037(2) 0.0133(15) -0.0066(14) -0.0006(14) O2 0.041(2) 0.026(2) 0.026(2) 0.0091(14) -0.0133(15) -0.018(2) O3 0.023(2) 0.023(2) 0.039(2) -0.0003(15) -0.0087(14) -0.0108(14) O4 0.029(2) 0.016(2) 0.024(2) 0.0111(13) -0.0161(13) -0.0100(13) O5 0.034(2) 0.023(2) 0.025(2) 0.0068(13) -0.0117(14) -0.0144(15) O6 0.027(2) 0.020(2) 0.038(2) 0.0160(14) -0.0128(14) -0.0105(14) O7 0.028(2) 0.016(2) 0.046(2) 0.0161(14) -0.0176(15) -0.0125(14) O8 0.029(2) 0.016(2) 0.028(2) 0.0048(13) -0.0079(13) -0.0121(14) O9 0.032(2) 0.024(2) 0.035(2) 0.0084(15) -0.0216(15) -0.0125(15) O10 0.032(2) 0.028(2) 0.032(2) 0.016(2) -0.0131(15) -0.010(2) O11 0.022(2) 0.019(2) 0.043(2) 0.0024(14) -0.0142(15) -0.0091(14) O12 0.035(2) 0.014(2) 0.047(2) 0.0054(15) -0.026(2) -0.0078(14) N1 0.028(2) 0.020(2) 0.038(2) -0.001(2) -0.016(2) -0.010(2) C1 0.039(3) 0.045(3) 0.041(3) 0.000(3) -0.014(3) -0.016(3) C2 0.059(4) 0.044(3) 0.034(3) 0.009(3) -0.011(3) -0.033(3) C3 0.047(3) 0.039(3) 0.038(3) 0.004(2) -0.011(2) -0.025(3) N2 0.024(2) 0.021(2) 0.028(2) 0.001(2) -0.011(2) -0.011(2) C4 0.022(2) 0.018(2) 0.033(3) 0.004(2) -0.009(2) -0.007(2) C5 0.029(3) 0.043(3) 0.033(3) 0.009(2) -0.005(2) -0.019(2) C6 0.028(3) 0.034(3) 0.044(3) 0.017(2) -0.020(2) -0.012(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 Zn1 O1 1.920(3) . ? Zn1 O2 1.947(3) . ? Zn1 O3 1.961(3) . ? Zn1 O4 1.973(3) . ? P1 O1 1.494(4) . ? P1 O11 1.515(3) . ? P1 O10 1.561(3) . ? P1 O12 1.573(3) . ? P2 O2 1.507(3) 2_665 ? P2 O3 1.512(3) . ? P2 O9 1.568(3) . ? P2 O8 1.570(3) . ? P3 O5 1.506(3) . ? P3 O6 1.531(3) . ? P3 O4 1.542(3) . ? P3 O7 1.588(3) . ? O2 P2 1.507(3) 2_665 ? O7 H20 0.82 . ? O8 H21 0.82 . ? O9 H22 0.82 . ? O10 H23 0.82 . ? O12 H24 0.82 . ? N1 C2 1.483(7) . ? N1 C3 1.498(7) . ? N1 C1 1.519(7) . ? N1 H3 0.91 . ? C1 C1 1.527(12) 2_666 ? C1 H2 0.97 . ? C1 H1 0.97 . ? C2 H6 0.96 . ? C2 H5 0.96 . ? C2 H4 0.96 . ? C3 H9 0.96 . ? C3 H8 0.96 . ? C3 H7 0.96 . ? N2 C4 1.489(6) . ? N2 C5 1.504(6) . ? N2 C6 1.507(6) . ? N2 H12 0.91 . ? C4 C4 1.531(9) 2_855 ? C4 H11 0.97 . ? C4 H10 0.97 . ? C5 H15 0.96 . ? C5 H14 0.96 . ? C5 H13 0.96 . ? C6 H18 0.96 . ? C6 H17 0.96 . ? C6 H16 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 111.28(15) . . ? O1 Zn1 O3 111.17(14) . . ? O2 Zn1 O3 108.13(14) . . ? O1 Zn1 O4 113.35(13) . . ? O2 Zn1 O4 101.04(13) . . ? O3 Zn1 O4 111.35(13) . . ? O1 P1 O11 114.0(2) . . ? O1 P1 O10 106.8(2) . . ? O11 P1 O10 112.6(2) . . ? O1 P1 O12 109.3(2) . . ? O11 P1 O12 109.1(2) . . ? O10 P1 O12 104.6(2) . . ? O2 P2 O3 114.6(2) 2_665 . ? O2 P2 O9 109.7(2) 2_665 . ? O3 P2 O9 109.3(2) . . ? O2 P2 O8 108.2(2) 2_665 . ? O3 P2 O8 110.5(2) . . ? O9 P2 O8 103.9(2) . . ? O5 P3 O6 112.2(2) . . ? O5 P3 O4 112.2(2) . . ? O6 P3 O4 110.5(2) . . ? O5 P3 O7 109.6(2) . . ? O6 P3 O7 107.6(2) . . ? O4 P3 O7 104.4(2) . . ? P1 O1 Zn1 143.4(2) . . ? P2 O2 Zn1 137.5(2) 2_665 . ? P2 O3 Zn1 126.8(2) . . ? P3 O4 Zn1 126.8(2) . . ? P3 O7 H20 109.47(13) . . ? P2 O8 H21 109.47(12) . . ? P2 O9 H22 109.47(13) . . ? P1 O10 H23 109.47(13) . . ? P1 O12 H24 109.47(13) . . ? C2 N1 C3 110.0(4) . . ? C2 N1 C1 117.4(4) . . ? C3 N1 C1 104.8(4) . . ? C2 N1 H3 108.1(3) . . ? C3 N1 H3 108.1(3) . . ? C1 N1 H3 108.1(3) . . ? N1 C1 C1 109.5(6) . 2_666 ? N1 C1 H2 109.8(3) . . ? C1 C1 H2 109.8(5) 2_666 . ? N1 C1 H1 109.8(3) . . ? C1 C1 H1 109.8(5) 2_666 . ? H2 C1 H1 108.2 . . ? N1 C2 H6 109.5(3) . . ? N1 C2 H5 109.5(3) . . ? H6 C2 H5 109.5 . . ? N1 C2 H4 109.5(3) . . ? H6 C2 H4 109.5 . . ? H5 C2 H4 1 data_test _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H25 N4 O12 P3 Zn' _chemical_formula_weight 503.58 _chemical_melting_point ? _chemical_compound_source ? 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.3253(8) _cell_length_b 14.8374(9) _cell_length_c 19.3273(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3534.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method ? _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.730 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 566(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13962 _diffrn_reflns_av_R_equivalents 0.1110 _diffrn_reflns_av_sigmaI/netI 0.0855 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 23.52 _reflns_number_total 2574 _reflns_number_observed 1696 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0382P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2574 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_obs 0.0413 _refine_ls_wR_factor_all 0.0914 _refine_ls_wR_factor_obs 0.0809 _refine_ls_goodness_of_fit_all 0.944 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 0.944 _refine_ls_restrained_S_obs 1.055 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.05663(5) 0.03522(4) 0.11498(3) 0.0213(2) Uani 1 d . . P1 P 0.19759(10) -0.02838(9) 0.24576(7) 0.0188(3) Uani 1 d . . P2 P -0.05520(11) 0.20638(9) 0.17892(7) 0.0217(3) Uani 1 d . . P3 P 0.16646(11) 0.00127(10) -0.03703(7) 0.0227(4) Uani 1 d . . O1 O 0.0410(2) 0.1573(2) 0.1471(2) 0.0259(9) Uani 1 d . . O2 O 0.1517(3) 0.0314(2) 0.0360(2) 0.0337(10) Uani 1 d . . O3 O 0.1133(3) -0.0401(2) 0.1891(2) 0.0260(9) Uani 1 d . . O4 O -0.0762(2) -0.0259(2) 0.0863(2) 0.0267(9) Uani 1 d . . O5 O 0.2975(2) -0.0853(2) 0.2339(2) 0.0270(9) Uani 1 d . . O6 O 0.1486(2) -0.0468(2) 0.3166(2) 0.0229(8) Uani 1 d . . O7 O 0.2307(3) 0.0755(2) 0.2427(2) 0.0263(9) Uani 1 d . . H30 H 0.2757(3) 0.0862(2) 0.2729(2) 0.039 Uiso 1 calc R . O8 O -0.0527(3) 0.2105(2) 0.2567(2) 0.0310(9) Uani 1 d . . O9 O -0.1640(3) 0.1667(2) 0.1562(2) 0.0335(10) Uani 1 d . . O10 O -0.0402(3) 0.3041(2) 0.1478(2) 0.0407(11) Uani 1 d . . H31 H -0.0895(3) 0.3367(2) 0.1614(2) 0.061 Uiso 1 calc R . O11 O 0.1851(3) -0.1013(2) -0.0382(2) 0.0405(11) Uani 1 d . . H32 H 0.1932(3) -0.1182(2) -0.0782(2) 0.061 Uiso 1 calc R . O12 O 0.2723(3) 0.0501(3) -0.0612(2) 0.0378(11) Uani 1 d . . H34 H 0.2854(3) 0.0365(3) -0.1014(2) 0.057 Uiso 1 calc R . N2 N -0.2500(3) 0.2569(3) 0.3360(2) 0.0271(11) Uani 1 d . . H7 H -0.2817(3) 0.3019(3) 0.3132(2) 0.041 Uiso 1 calc R . H6 H -0.2938(3) 0.2092(3) 0.3362(2) 0.041 Uiso 1 calc R . H5 H -0.1879(3) 0.2426(3) 0.3152(2) 0.041 Uiso 1 calc R . C1 C -0.1742(4) 0.2122(3) 0.4494(3) 0.0265(14) Uani 1 d . . H1 H -0.1680(4) 0.2315(3) 0.4972(3) 0.032 Uiso 1 calc R . H2 H -0.2192(4) 0.1586(3) 0.4483(3) 0.032 Uiso 1 calc R . C2 C -0.2279(4) 0.2853(4) 0.4080(3) 0.0278(14) Uani 1 d . . H3 H -0.2956(4) 0.3020(4) 0.4301(3) 0.033 Uiso 1 calc R . H4 H -0.1814(4) 0.3381(4) 0.4074(3) 0.033 Uiso 1 calc R . N1 N -0.0653(3) 0.1898(3) 0.4227(2) 0.0230(11) Uani 1 d . . C3 C 0.0157(4) 0.2554(4) 0.4479(3) 0.0313(15) Uani 1 d . . H8 H 0.0415(4) 0.2367(4) 0.4931(3) 0.038 Uiso 1 calc R . H9 H -0.0183(4) 0.3140(4) 0.4529(3) 0.038 Uiso 1 calc R . C4 C 0.1111(4) 0.2629(4) 0.3988(3) 0.042(2) Uani 1 d . . H10 H 0.1699(4) 0.2948(4) 0.4215(3) 0.050 Uiso 1 calc R . H11 H 0.1368(4) 0.2031(4) 0.3870(3) 0.050 Uiso 1 calc R . N3 N 0.0805(4) 0.3109(3) 0.3354(2) 0.0445(14) Uani 1 d . . H12 H 0.1376(4) 0.3146(3) 0.3074(2) 0.067 Uiso 1 calc R . H13 H 0.0579(4) 0.3662(3) 0.3461(2) 0.067 Uiso 1 calc R . H14 H 0.0273(4) 0.2812(3) 0.3142(2) 0.067 Uiso 1 calc R . C5 C -0.0348(4) 0.0978(4) 0.4422(3) 0.0311(15) Uani 1 d . . H15 H -0.0544(4) 0.0878(4) 0.4902(3) 0.037 Uiso 1 calc R . H16 H 0.0432(4) 0.0914(4) 0.4383(3) 0.037 Uiso 1 calc R . C6 C -0.0891(4) 0.0270(4) 0.3978(3) 0.0315(15) Uani 1 d . . H17 H -0.0722(4) -0.0325(4) 0.4157(3) 0.038 Uiso 1 calc R . H18 H -0.1672(4) 0.0349(4) 0.3996(3) 0.038 Uiso 1 calc R . N4 N -0.0516(3) 0.0338(3) 0.3251(2) 0.0260(11) Uani 1 d . . H19 H -0.0842(3) -0.0082(3) 0.2997(2) 0.039 Uiso 1 calc R . H20 H 0.0199(3) 0.0258(3) 0.3234(2) 0.039 Uiso 1 calc R . H21 H -0.0680(3) 0.0881(3) 0.3085(2) 0.039 Uiso 1 calc R . 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 0.0199(3) 0.0211(4) 0.0229(4) -0.0011(3) -0.0017(3) 0.0004(3) P1 0.0174(7) 0.0166(8) 0.0225(8) 0.0018(7) -0.0016(6) -0.0005(6) P2 0.0232(8) 0.0170(8) 0.0250(9) -0.0005(6) 0.0022(7) 0.0005(7) P3 0.0189(7) 0.0290(9) 0.0202(8) -0.0021(7) 0.0002(7) -0.0018(7) O1 0.023(2) 0.016(2) 0.039(2) -0.007(2) 0.002(2) 0.001(2) O2 0.029(2) 0.049(3) 0.024(2) -0.010(2) 0.003(2) -0.011(2) O3 0.027(2) 0.023(2) 0.027(2) 0.004(2) -0.007(2) -0.001(2) O4 0.021(2) 0.026(2) 0.033(2) 0.001(2) -0.012(2) -0.005(2) O5 0.021(2) 0.022(2) 0.038(3) 0.001(2) 0.001(2) 0.005(2) O6 0.020(2) 0.027(2) 0.022(2) 0.003(2) 0.000(2) -0.004(2) O7 0.029(2) 0.019(2) 0.031(2) 0.005(2) -0.008(2) -0.002(2) O8 0.031(2) 0.032(2) 0.031(2) -0.003(2) -0.002(2) -0.005(2) O9 0.023(2) 0.038(3) 0.040(2) -0.012(2) -0.001(2) -0.001(2) O10 0.046(3) 0.020(2) 0.056(3) 0.007(2) 0.023(2) 0.010(2) O11 0.064(3) 0.030(3) 0.028(2) -0.003(2) -0.016(2) 0.011(2) O12 0.024(2) 0.066(3) 0.024(2) -0.010(2) 0.004(2) -0.012(2) N2 0.024(3) 0.018(3) 0.039(3) 0.003(2) -0.005(2) 0.000(2) C1 0.027(3) 0.024(4) 0.028(3) 0.004(3) 0.003(3) 0.002(3) C2 0.025(3) 0.026(3) 0.032(3) -0.002(3) 0.007(3) 0.004(3) N1 0.026(2) 0.016(3) 0.027(3) 0.002(2) 0.001(2) -0.002(2) C3 0.035(3) 0.027(4) 0.032(4) 0.001(3) -0.003(3) -0.003(3) C4 0.028(3) 0.038(4) 0.060(5) -0.015(4) -0.004(3) -0.010(3) N3 0.051(3) 0.041(3) 0.042(3) -0.018(3) 0.021(3) -0.024(3) C5 0.029(3) 0.035(4) 0.029(4) 0.003(3) 0.002(3) 0.004(3) C6 0.031(3) 0.024(4) 0.040(4) -0.003(3) 0.005(3) 0.002(3) N4 0.015(2) 0.025(3) 0.038(3) -0.007(2) -0.003(2) 0.004(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 Zn1 O2 1.924(3) . ? Zn1 O1 1.925(3) . ? Zn1 O3 1.946(3) . ? Zn1 O4 1.953(3) . ? P1 O5 1.510(3) . ? P1 O3 1.520(3) . ? P1 O6 1.522(3) . ? P1 O7 1.596(3) . ? P2 O8 1.504(4) . ? P2 O1 1.521(3) . ? P2 O9 1.530(3) . ? P2 O10 1.580(4) . ? P3 O2 1.493(4) . ? P3 O4 1.509(3) 5 ? P3 O11 1.539(4) . ? P3 O12 1.563(3) . ? O4 P3 1.509(3) 5 ? O7 H30 0.82 . ? O10 H31 0.82 . ? O11 H32 0.82 . ? O12 H34 0.82 . ? N2 C2 1.479(6) . ? N2 H7 0.89 . ? N2 H6 0.89 . ? N2 H5 0.89 . ? C1 N1 1.475(6) . ? C1 C2 1.502(6) . ? C1 H1 0.97 . ? C1 H2 0.97 . ? C2 H3 0.97 . ? C2 H4 0.97 . ? N1 C5 1.466(6) . ? N1 C3 1.477(6) . ? C3 C4 1.516(7) . ? C3 H8 0.97 . ? C3 H9 0.97 . ? C4 N3 1.467(7) . ? C4 H10 0.97 . ? C4 H11 0.97 . ? N3 H12 0.89 . ? N3 H13 0.89 . ? N3 H14 0.89 . ? C5 C6 1.513(7) . ? C5 H15 0.97 . ? C5 H16 0.97 . ? C6 N4 1.483(6) . ? C6 H17 0.97 . ? C6 H18 0.97 . ? N4 H19 0.89 . ? N4 H20 0.89 . ? N4 H21 0.89 . ? 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 O2 Zn1 O1 110.16(15) . . ? O2 Zn1 O3 110.37(15) . . ? O1 Zn1 O3 109.80(14) . . ? O2 Zn1 O4 105.76(14) . . ? O1 Zn1 O4 116.43(14) . . ? O3 Zn1 O4 104.07(14) . . ? O5 P1 O3 112.6(2) . . ? O5 P1 O6 111.1(2) . . ? O3 P1 O6 110.9(2) . . ? O5 P1 O7 109.0(2) . . ? O3 P1 O7 105.0(2) . . ? O6 P1 O7 107.9(2) . . ? O8 P2 O1 114.0(2) . . ? O8 P2 O9 108.7(2) . . ? O1 P2 O9 112.5(2) . . ? O8 P2 O10 110.0(2) . . ? O1 P2 O10 101.2(2) . . ? O9 P2 O10 110.3(2) . . ? O2 P3 O4 115.7(2) . 5 ? O2 P3 O11 109.1(2) . . ? O4 P3 O11 109.9(2) 5 . ? O2 P3 O12 104.2(2) . . ? O4 P3 O12 108.3(2) 5 . ? O11 P3 O12 109.3(2) . . ? P2 O1 Zn1 131.2(2) . . ? P3 O2 Zn1 146.4(2) . . ? P1 O3 Zn1 135.3(2) . . ? P3 O4 Zn1 133.2(2) 5 . ? P1 O7 H30 109.47(12) . . ? P2 O10 H31 109.47(13) . . ? P3 O11 H32 109.47(15) . . ? P3 O12 H34 109.47(14) . . ? C2 N2 H7 109.5(3) . . ? C2 N2 H6 109.5(3) . . ? H7 N2 H6 109.5 . . ? C2 N2 H5 109.5(3) . . ? H7 N2 H5 109.5 . . ? H6 N2 H5 109.5 . . ? N1 C1 C2 112.1(4) . . ? N1 C1 H1 109.2(3) . . ? C2 C1 H1 109.2(3) . . ? N1 C1 H2 109.2(3) . . ? C2 C1 H2 109.2(3) . . ? H1 C1 H2 107.9 . . ? N2 C2 C1 112.1(4) . . ? N2 C2 H3 109.2(3) . . ? C1 C2 H3 109.2(3) . . ? N2 C2 H4 109.2(3) . . ? C1 C2 H4 109.2(3) . . ? H3 C2 H4 107.9 . . ? C5 N1 C1 110.6(4) . . ? C5 N1 C3 110.8(4) . . ? C1 N1 C3 110.6(4) . . ? N1 C3 C4 111.5(4) . . ? N1 C3 H8 109.3(3) . . ? C4 C3 H8 109.3(3) . . ? N1 C3 H9 109.3(3) . . ? C4 C3 H9 109.3(3) . . ? H8 C3 H9 108.0 . . ? N3 C4 C3 111.0(5) . . ? N3 C4 H10 109.4(3) . . ? C3 C4 H10 109.4(3) . . ? N3 C4 H11 109.4(3) . . ? C3 C4 H11 109.4(3) . . ? H10 C4 H11 108.0 . . ? C4 N3 H12 109.5(3) . . ? C4 N3 H13 109.5(3) . . ? H12 N3 H13 109.5 . . ? C4 N3 H14 109.5(3) . . ? H12 N3 H14 109.5 . . ? H13 N3 H14 109.5 . . ? N1 C5 C6 112.8(4) . . ? N1 C5 H15 109.0(3) . . ? C6 C5 H15 109.0(3) . . ? N1 C5 H16 109.0(3) . . ? C6 C5 H16 109.0(3) . . ? H15 C5 H16 107.8 . . ? N4 C6 C5 110.6(4) . . ? N4 C6 H17 109.5(3) . . ? C5 C6 H17 109.5(3) . . ? N4 C6 H18 109.5(3) . . ? C5 C6 H18 109.5(3) . . ? H17 C6 H18 108.1 . . ? C6 N4 H19 109.5(3) . . ? C6 N4 H20 109.5(3) . . ? H19 N4 H20 109.5 . . ? C6 N4 H21 109.5(3) . . ? H19 N4 H21 109.5 . . ? H20 N4 H21 109.5 . . ? _refine_diff_density_max 0.495 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.135 09.5 . . ? N1 C3 H9 109.5(3) . . ? N1 C3 H8 109.5(3) . . ? H9 C3 H8 109.5 . . ? N1 C3 H7 109.5(3) . . ? H9 C3 H7 109.5 . . ? H8 C3 H7 109.5 . . ? C4 N2 C5 109.6(4) . . ? C4 N2 C6 113.3(4) . . ? C5 N2 C6 109.9(4) . . ? C4 N2 H12 108.0(2) . . ? C5 N2 H12 108.0(3) . . ? C6 N2 H12 108.0(3) . . ? N2 C4 C4 111.5(5) . 2_855 ? N2 C4 H11 109.3(2) . . ? C4 C4 H11 109.3(4) 2_855 . ? N2 C4 H10 109.3(2) . . ? C4 C4 H10 109.3(4) 2_855 . ? H11 C4 H10 108.0 . . ? N2 C5 H15 109.5(3) . . ? N2 C5 H14 109.5(3) . . ? H15 C5 H14 109.5 . . ? N2 C5 H13 109.5(3) . . ? H15 C5 H13 109.5 . . ? H14 C5 H13 109.5 . . ? N2 C6 H18 109.5(3) . . ? N2 C6 H17 109.5(3) . . ? H18 C6 H17 109.5 . . ? N2 C6 H16 109.5(2) . . ? H18 C6 H16 109.5 . . ? H17 C6 H16 109.5 . . ? _refine_diff_density_max 1.000 _refine_diff_density_min -1.427 _refine_diff_density_rms 0.137 eof ******************************************************************************* COMPOUND II ----------- data_test _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H25 N4 O12 P3 Zn' _chemical_formula_weight 503.58 _chemical_melting_point ? _chemical_compound_source ? 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.3253(8) _cell_length_b 14.8374(9) _cell_length_c 19.3273(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3534.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method ? _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.730 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 566(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13962 _diffrn_reflns_av_R_equivalents 0.1110 _diffrn_reflns_av_sigmaI/netI 0.0855 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 23.52 _reflns_number_total 2574 _reflns_number_observed 1696 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0382P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2574 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_obs 0.0413 _refine_ls_wR_factor_all 0.0914 _refine_ls_wR_factor_obs 0.0809 _refine_ls_goodness_of_fit_all 0.944 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 0.944 _refine_ls_restrained_S_obs 1.055 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.05663(5) 0.03522(4) 0.11498(3) 0.0213(2) Uani 1 d . . P1 P 0.19759(10) -0.02838(9) 0.24576(7) 0.0188(3) Uani 1 d . . P2 P -0.05520(11) 0.20638(9) 0.17892(7) 0.0217(3) Uani 1 d . . P3 P 0.16646(11) 0.00127(10) -0.03703(7) 0.0227(4) Uani 1 d . . O1 O 0.0410(2) 0.1573(2) 0.1471(2) 0.0259(9) Uani 1 d . . O2 O 0.1517(3) 0.0314(2) 0.0360(2) 0.0337(10) Uani 1 d . . O3 O 0.1133(3) -0.0401(2) 0.1891(2) 0.0260(9) Uani 1 d . . O4 O -0.0762(2) -0.0259(2) 0.0863(2) 0.0267(9) Uani 1 d . . O5 O 0.2975(2) -0.0853(2) 0.2339(2) 0.0270(9) Uani 1 d . . O6 O 0.1486(2) -0.0468(2) 0.3166(2) 0.0229(8) Uani 1 d . . O7 O 0.2307(3) 0.0755(2) 0.2427(2) 0.0263(9) Uani 1 d . . H30 H 0.2757(3) 0.0862(2) 0.2729(2) 0.039 Uiso 1 calc R . O8 O -0.0527(3) 0.2105(2) 0.2567(2) 0.0310(9) Uani 1 d . . O9 O -0.1640(3) 0.1667(2) 0.1562(2) 0.0335(10) Uani 1 d . . O10 O -0.0402(3) 0.3041(2) 0.1478(2) 0.0407(11) Uani 1 d . . H31 H -0.0895(3) 0.3367(2) 0.1614(2) 0.061 Uiso 1 calc R . O11 O 0.1851(3) -0.1013(2) -0.0382(2) 0.0405(11) Uani 1 d . . H32 H 0.1932(3) -0.1182(2) -0.0782(2) 0.061 Uiso 1 calc R . O12 O 0.2723(3) 0.0501(3) -0.0612(2) 0.0378(11) Uani 1 d . . H34 H 0.2854(3) 0.0365(3) -0.1014(2) 0.057 Uiso 1 calc R . N2 N -0.2500(3) 0.2569(3) 0.3360(2) 0.0271(11) Uani 1 d . . H7 H -0.2817(3) 0.3019(3) 0.3132(2) 0.041 Uiso 1 calc R . H6 H -0.2938(3) 0.2092(3) 0.3362(2) 0.041 Uiso 1 calc R . H5 H -0.1879(3) 0.2426(3) 0.3152(2) 0.041 Uiso 1 calc R . C1 C -0.1742(4) 0.2122(3) 0.4494(3) 0.0265(14) Uani 1 d . . H1 H -0.1680(4) 0.2315(3) 0.4972(3) 0.032 Uiso 1 calc R . H2 H -0.2192(4) 0.1586(3) 0.4483(3) 0.032 Uiso 1 calc R . C2 C -0.2279(4) 0.2853(4) 0.4080(3) 0.0278(14) Uani 1 d . . H3 H -0.2956(4) 0.3020(4) 0.4301(3) 0.033 Uiso 1 calc R . H4 H -0.1814(4) 0.3381(4) 0.4074(3) 0.033 Uiso 1 calc R . N1 N -0.0653(3) 0.1898(3) 0.4227(2) 0.0230(11) Uani 1 d . . C3 C 0.0157(4) 0.2554(4) 0.4479(3) 0.0313(15) Uani 1 d . . H8 H 0.0415(4) 0.2367(4) 0.4931(3) 0.038 Uiso 1 calc R . H9 H -0.0183(4) 0.3140(4) 0.4529(3) 0.038 Uiso 1 calc R . C4 C 0.1111(4) 0.2629(4) 0.3988(3) 0.042(2) Uani 1 d . . H10 H 0.1699(4) 0.2948(4) 0.4215(3) 0.050 Uiso 1 calc R . H11 H 0.1368(4) 0.2031(4) 0.3870(3) 0.050 Uiso 1 calc R . N3 N 0.0805(4) 0.3109(3) 0.3354(2) 0.0445(14) Uani 1 d . . H12 H 0.1376(4) 0.3146(3) 0.3074(2) 0.067 Uiso 1 calc R . H13 H 0.0579(4) 0.3662(3) 0.3461(2) 0.067 Uiso 1 calc R . H14 H 0.0273(4) 0.2812(3) 0.3142(2) 0.067 Uiso 1 calc R . C5 C -0.0348(4) 0.0978(4) 0.4422(3) 0.0311(15) Uani 1 d . . H15 H -0.0544(4) 0.0878(4) 0.4902(3) 0.037 Uiso 1 calc R . H16 H 0.0432(4) 0.0914(4) 0.4383(3) 0.037 Uiso 1 calc R . C6 C -0.0891(4) 0.0270(4) 0.3978(3) 0.0315(15) Uani 1 d . . H17 H -0.0722(4) -0.0325(4) 0.4157(3) 0.038 Uiso 1 calc R . H18 H -0.1672(4) 0.0349(4) 0.3996(3) 0.038 Uiso 1 calc R . N4 N -0.0516(3) 0.0338(3) 0.3251(2) 0.0260(11) Uani 1 d . . H19 H -0.0842(3) -0.0082(3) 0.2997(2) 0.039 Uiso 1 calc R . H20 H 0.0199(3) 0.0258(3) 0.3234(2) 0.039 Uiso 1 calc R . H21 H -0.0680(3) 0.0881(3) 0.3085(2) 0.039 Uiso 1 calc R . 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 0.0199(3) 0.0211(4) 0.0229(4) -0.0011(3) -0.0017(3) 0.0004(3) P1 0.0174(7) 0.0166(8) 0.0225(8) 0.0018(7) -0.0016(6) -0.0005(6) P2 0.0232(8) 0.0170(8) 0.0250(9) -0.0005(6) 0.0022(7) 0.0005(7) P3 0.0189(7) 0.0290(9) 0.0202(8) -0.0021(7) 0.0002(7) -0.0018(7) O1 0.023(2) 0.016(2) 0.039(2) -0.007(2) 0.002(2) 0.001(2) O2 0.029(2) 0.049(3) 0.024(2) -0.010(2) 0.003(2) -0.011(2) O3 0.027(2) 0.023(2) 0.027(2) 0.004(2) -0.007(2) -0.001(2) O4 0.021(2) 0.026(2) 0.033(2) 0.001(2) -0.012(2) -0.005(2) O5 0.021(2) 0.022(2) 0.038(3) 0.001(2) 0.001(2) 0.005(2) O6 0.020(2) 0.027(2) 0.022(2) 0.003(2) 0.000(2) -0.004(2) O7 0.029(2) 0.019(2) 0.031(2) 0.005(2) -0.008(2) -0.002(2) O8 0.031(2) 0.032(2) 0.031(2) -0.003(2) -0.002(2) -0.005(2) O9 0.023(2) 0.038(3) 0.040(2) -0.012(2) -0.001(2) -0.001(2) O10 0.046(3) 0.020(2) 0.056(3) 0.007(2) 0.023(2) 0.010(2) O11 0.064(3) 0.030(3) 0.028(2) -0.003(2) -0.016(2) 0.011(2) O12 0.024(2) 0.066(3) 0.024(2) -0.010(2) 0.004(2) -0.012(2) N2 0.024(3) 0.018(3) 0.039(3) 0.003(2) -0.005(2) 0.000(2) C1 0.027(3) 0.024(4) 0.028(3) 0.004(3) 0.003(3) 0.002(3) C2 0.025(3) 0.026(3) 0.032(3) -0.002(3) 0.007(3) 0.004(3) N1 0.026(2) 0.016(3) 0.027(3) 0.002(2) 0.001(2) -0.002(2) C3 0.035(3) 0.027(4) 0.032(4) 0.001(3) -0.003(3) -0.003(3) C4 0.028(3) 0.038(4) 0.060(5) -0.015(4) -0.004(3) -0.010(3) N3 0.051(3) 0.041(3) 0.042(3) -0.018(3) 0.021(3) -0.024(3) C5 0.029(3) 0.035(4) 0.029(4) 0.003(3) 0.002(3) 0.004(3) C6 0.031(3) 0.024(4) 0.040(4) -0.003(3) 0.005(3) 0.002(3) N4 0.015(2) 0.025(3) 0.038(3) -0.007(2) -0.003(2) 0.004(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 Zn1 O2 1.924(3) . ? Zn1 O1 1.925(3) . ? Zn1 O3 1.946(3) . ? Zn1 O4 1.953(3) . ? P1 O5 1.510(3) . ? P1 O3 1.520(3) . ? P1 O6 1.522(3) . ? P1 O7 1.596(3) . ? P2 O8 1.504(4) . ? P2 O1 1.521(3) . ? P2 O9 1.530(3) . ? P2 O10 1.580(4) . ? P3 O2 1.493(4) . ? P3 O4 1.509(3) 5 ? P3 O11 1.539(4) . ? P3 O12 1.563(3) . ? O4 P3 1.509(3) 5 ? O7 H30 0.82 . ? O10 H31 0.82 . ? O11 H32 0.82 . ? O12 H34 0.82 . ? N2 C2 1.479(6) . ? N2 H7 0.89 . ? N2 H6 0.89 . ? N2 H5 0.89 . ? C1 N1 1.475(6) . ? C1 C2 1.502(6) . ? C1 H1 0.97 . ? C1 H2 0.97 . ? C2 H3 0.97 . ? C2 H4 0.97 . ? N1 C5 1.466(6) . ? N1 C3 1.477(6) . ? C3 C4 1.516(7) . ? C3 H8 0.97 . ? C3 H9 0.97 . ? C4 N3 1.467(7) . ? C4 H10 0.97 . ? C4 H11 0.97 . ? N3 H12 0.89 . ? N3 H13 0.89 . ? N3 H14 0.89 . ? C5 C6 1.513(7) . ? C5 H15 0.97 . ? C5 H16 0.97 . ? C6 N4 1.483(6) . ? C6 H17 0.97 . ? C6 H18 0.97 . ? N4 H19 0.89 . ? N4 H20 0.89 . ? N4 H21 0.89 . ? 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 O2 Zn1 O1 110.16(15) . . ? O2 Zn1 O3 110.37(15) . . ? O1 Zn1 O3 109.80(14) . . ? O2 Zn1 O4 105.76(14) . . ? O1 Zn1 O4 116.43(14) . . ? O3 Zn1 O4 104.07(14) . . ? O5 P1 O3 112.6(2) . . ? O5 P1 O6 111.1(2) . . ? O3 P1 O6 110.9(2) . . ? O5 P1 O7 109.0(2) . . ? O3 P1 O7 105.0(2) . . ? O6 P1 O7 107.9(2) . . ? O8 P2 O1 114.0(2) . . ? O8 P2 O9 108.7(2) . . ? O1 P2 O9 112.5(2) . . ? O8 P2 O10 110.0(2) . . ? O1 P2 O10 101.2(2) . . ? O9 P2 O10 110.3(2) . . ? O2 P3 O4 115.7(2) . 5 ? O2 P3 O11 109.1(2) . . ? O4 P3 O11 109.9(2) 5 . ? O2 P3 O12 104.2(2) . . ? O4 P3 O12 108.3(2) 5 . ? O11 P3 O12 109.3(2) . . ? P2 O1 Zn1 131.2(2) . . ? P3 O2 Zn1 146.4(2) . . ? P1 O3 Zn1 135.3(2) . . ? P3 O4 Zn1 133.2(2) 5 . ? P1 O7 H30 109.47(12) . . ? P2 O10 H31 109.47(13) . . ? P3 O11 H32 109.47(15) . . ? P3 O12 H34 109.47(14) . . ? C2 N2 H7 109.5(3) . . ? C2 N2 H6 109.5(3) . . ? H7 N2 H6 109.5 . . ? C2 N2 H5 109.5(3) . . ? H7 N2 H5 109.5 . . ? H6 N2 H5 109.5 . . ? N1 C1 C2 112.1(4) . . ? N1 C1 H1 109.2(3) . . ? C2 C1 H1 109.2(3) . . ? N1 C1 H2 109.2(3) . . ? C2 C1 H2 109.2(3) . . ? H1 C1 H2 107.9 . . ? N2 C2 C1 112.1(4) . . ? N2 C2 H3 109.2(3) . . ? C1 C2 H3 109.2(3) . . ? N2 C2 H4 109.2(3) . . ? C1 C2 H4 109.2(3) . . ? H3 C2 H4 107.9 . . ? C5 N1 C1 110.6(4) . . ? C5 N1 C3 110.8(4) . . ? C1 N1 C3 110.6(4) . . ? N1 C3 C4 111.5(4) . . ? N1 C3 H8 109.3(3) . . ? C4 C3 H8 109.3(3) . . ? N1 C3 H9 109.3(3) . . ? C4 C3 H9 109.3(3) . . ? H8 C3 H9 108.0 . . ? N3 C4 C3 111.0(5) . . ? N3 C4 H10 109.4(3) . . ? C3 C4 H10 109.4(3) . . ? N3 C4 H11 109.4(3) . . ? C3 C4 H11 109.4(3) . . ? H10 C4 H11 108.0 . . ? C4 N3 H12 109.5(3) . . ? C4 N3 H13 109.5(3) . . ? H12 N3 H13 109.5 . . ? C4 N3 H14 109.5(3) . . ? H12 N3 H14 109.5 . . ? H13 N3 H14 109.5 . . ? N1 C5 C6 112.8(4) . . ? N1 C5 H15 109.0(3) . . ? C6 C5 H15 109.0(3) . . ? N1 C5 H16 109.0(3) . . ? C6 C5 H16 109.0(3) . . ? H15 C5 H16 107.8 . . ? N4 C6 C5 110.6(4) . . ? N4 C6 H17 109.5(3) . . ? C5 C6 H17 109.5(3) . . ? N4 C6 H18 109.5(3) . . ? C5 C6 H18 109.5(3) . . ? H17 C6 H18 108.1 . . ? C6 N4 H19 109.5(3) . . ? C6 N4 H20 109.5(3) . . ? H19 N4 H20 109.5 . . ? C6 N4 H21 109.5(3) . . ? H19 N4 H21 109.5 . . ? H20 N4 H21 109.5 . . ? _refine_diff_density_max 0.495 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.135 eof ******************************************************************************** COMPOUND III ------------ data_test _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H29 N5 O25 P6 Zn6' _chemical_formula_weight 1149.38 _chemical_melting_point ? _chemical_compound_source ? 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.785(2) _cell_length_b 8.2783(7) _cell_length_c 18.747(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2915.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 571(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.619 _exptl_crystal_density_method ? _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 5.298 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 571(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11429 _diffrn_reflns_av_R_equivalents 0.1251 _diffrn_reflns_av_sigmaI/netI 0.1096 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 23.18 _reflns_number_total 3157 _reflns_number_observed 2376 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 3157 _refine_ls_number_parameters 194 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_obs 0.0669 _refine_ls_wR_factor_all 0.1727 _refine_ls_wR_factor_obs 0.1518 _refine_ls_goodness_of_fit_all 1.010 _refine_ls_goodness_of_fit_obs 1.030 _refine_ls_restrained_S_all 1.010 _refine_ls_restrained_S_obs 1.030 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.59839(12) -0.3520(3) 0.48217(14) 0.0158(6) Uiso 1 d . . Zn2 Zn 0.31821(12) -0.0410(3) 0.48185(14) 0.0154(6) Uiso 1 d . . Zn3 Zn 0.70889(12) 0.1417(3) 0.63826(13) 0.0147(6) Uiso 1 d . . Zn4 Zn 0.67865(12) -0.3582(3) 0.65112(13) 0.0158(6) Uiso 1 d . . Zn5 Zn 0.62271(12) 0.1387(3) 0.46986(13) 0.0161(6) Uiso 1 d . . Zn6 Zn 0.48640(12) -0.9536(3) 0.62808(14) 0.0158(6) Uiso 1 d . . P1 P 0.4832(3) -0.0746(7) 0.4687(3) 0.0163(14) Uiso 1 d . . P2 P 0.7224(3) -0.1421(7) 0.5247(3) 0.0161(14) Uiso 1 d . . P3 P 0.5810(3) -0.6422(7) 0.5934(3) 0.0145(13) Uiso 1 d . . P4 P 0.8184(3) -0.5715(7) 0.6426(3) 0.0147(14) Uiso 1 d . . P5 P 0.1925(3) 0.0720(8) 0.3773(3) 0.0152(14) Uiso 1 d . . P6 P 0.6130(3) -0.0689(7) 0.7343(3) 0.0127(13) Uiso 1 d . . O1 O 0.5606(7) -0.5362(17) 0.5284(8) 0.019(4) Uiso 1 d . . O2 O 0.5276(7) -0.2149(15) 0.4361(7) 0.008(3) Uiso 1 d . . O3 O 0.6543(7) -0.4191(17) 0.3982(7) 0.014(4) Uiso 1 d . . O4 O 0.6646(7) -0.2601(19) 0.5550(8) 0.018(4) Uiso 1 d . . O5 O 0.2832(7) -0.2590(16) 0.4910(8) 0.018(4) Uiso 1 d . . O6 O 0.8245(7) -0.6045(18) 0.5621(8) 0.018(4) Uiso 1 d . . O7 O 0.2672(8) 0.0849(17) 0.4083(8) 0.026(4) Uiso 1 d . . O8 O 0.4108(7) -0.0659(18) 0.4295(8) 0.017(4) Uiso 1 d . . O9 O 0.7809(7) -0.7163(17) 0.6771(8) 0.021(4) Uiso 1 d . . O10 O 0.6634(8) 0.0735(20) 0.7286(9) 0.030(4) Uiso 1 d . . O11 O 0.7514(7) -0.0435(17) 0.5867(7) 0.016(3) Uiso 1 d . . O12 O 0.6383(7) 0.2326(17) 0.5674(7) 0.012(3) Uiso 1 d . . O13 O 0.6152(7) -0.5430(18) 0.6532(8) 0.021(4) Uiso 1 d . . O14 O 0.6557(7) -0.2289(18) 0.7345(8) 0.017(4) Uiso 1 d . . O15 O 0.7801(8) -0.4107(17) 0.6559(9) 0.023(4) Uiso 1 d . . O16 O 0.6874(7) -0.0418(17) 0.4661(8) 0.018(4) Uiso 1 d . . O17 O 0.5231(7) 0.0846(16) 0.4595(8) 0.016(4) Uiso 1 d . . O18 O 0.6472(8) 0.2783(20) 0.3893(8) 0.025(4) Uiso 1 d . . O19 O 0.5150(7) -0.7306(17) 0.6211(8) 0.017(3) Uiso 1 d . . O20 O 0.5568(8) -1.0822(18) 0.6786(8) 0.023(4) Uiso 1 d . . O21 O 0.3928(7) -0.9395(18) 0.6755(8) 0.019(4) Uiso 1 d . . O22 O 0.4686(8) -0.1054(18) 0.5488(9) 0.025(4) Uiso 1 d . . O23 O 0.2011(7) 0.0639(18) 0.2949(8) 0.020(4) Uiso 1 d . . H23 H 0.2243(7) -0.0163(18) 0.2842(8) 0.030 Uiso 1 calc R . O24 O 0.5716(8) -0.0584(17) 0.8075(8) 0.022(4) Uiso 1 d . . H24 H 0.6003(8) -0.0508(17) 0.8403(8) 0.033 Uiso 1 calc R . N1 N 0.0872(10) 0.9251(22) 0.8425(11) 0.027(5) Uiso 1 d . . C1 C 0.1352(11) 1.0706(27) 0.8287(13) 0.025(6) Uiso 1 d . . H1 H 0.1235(11) 1.1174(27) 0.7828(13) 0.029 Uiso 1 calc R . H2 H 0.1267(11) 1.1518(27) 0.8650(13) 0.029 Uiso 1 calc R . C2 C 0.2134(12) 1.0237(29) 0.8296(14) 0.030(6) Uiso 1 d . . H3 H 0.2241(12) 0.9616(29) 0.8721(14) 0.036 Uiso 1 calc R . H4 H 0.2246(12) 0.9581(29) 0.7882(14) 0.036 Uiso 1 calc R . N2 N 0.2561(11) 1.1740(24) 0.8286(12) 0.042(6) Uiso 1 d . . H5 H 0.3022(11) 1.1492(24) 0.8291(12) 0.063 Uiso 1 calc R . H6 H 0.2457(11) 1.2332(24) 0.8668(12) 0.063 Uiso 1 calc R . H7 H 0.2461(11) 1.2300(24) 0.7893(12) 0.063 Uiso 1 calc R . C3 C 0.0095(12) 0.9678(29) 0.8398(14) 0.029(6) Uiso 1 d . . H8 H 0.0041(12) 1.0825(29) 0.8489(14) 0.034 Uiso 1 calc R . H9 H -0.0153(12) 0.9100(29) 0.8774(14) 0.034 Uiso 1 calc R . C4 C -0.0256(12) 0.9259(27) 0.7664(13) 0.024(6) Uiso 1 d . . H10 H -0.0636(12) 1.0018(27) 0.7562(13) 0.029 Uiso 1 calc R . H11 H 0.0095(12) 0.9334(27) 0.7287(13) 0.029 Uiso 1 calc R . N3 N -0.0549(9) 0.7580(23) 0.7697(10) 0.029(5) Uiso 1 d . . H12 H -0.0750(9) 0.7333(23) 0.7281(10) 0.043 Uiso 1 calc R . H13 H -0.0874(9) 0.7520(23) 0.8042(10) 0.043 Uiso 1 calc R . H14 H -0.0198(9) 0.6888(23) 0.7787(10) 0.043 Uiso 1 calc R . C5 C 0.1009(11) 0.8558(28) 0.9168(12) 0.023(6) Uiso 1 d . . H15 H 0.0660(11) 0.7720(28) 0.9260(12) 0.027 Uiso 1 calc R . H16 H 0.1475(11) 0.8051(28) 0.9169(12) 0.027 Uiso 1 calc R . C6 C 0.0982(11) 0.9743(25) 0.9762(13) 0.022(5) Uiso 1 d . . H17 H 0.0539(11) 1.0338(25) 0.9731(13) 0.026 Uiso 1 calc R . H18 H 0.1368(11) 1.0510(25) 0.9702(13) 0.026 Uiso 1 calc R . N4 N 0.1037(10) 0.9010(22) 1.0491(11) 0.031(6) Uiso 1 d . . H19 H 0.1017(10) 0.9788(22) 1.0818(11) 0.047 Uiso 1 calc R . H20 H 0.1448(10) 0.8484(22) 1.0530(11) 0.047 Uiso 1 calc R . H21 H 0.0678(10) 0.8325(22) 1.0557(11) 0.047 Uiso 1 calc R . N5 N 0.3960(8) -0.9253(20) 0.8179(9) 0.015(4) Uiso 1 d . . O100 O 0.1060(7) 1.1809(17) 1.1300(9) 0.029(4) Uiso 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 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.892(15) . ? Zn1 O2 1.950(13) . ? Zn1 O3 1.972(14) . ? Zn1 O4 1.997(15) . ? Zn2 O5 1.928(14) . ? Zn2 O6 1.930(15) 3_445 ? Zn2 O7 1.98(2) . ? Zn2 O8 2.009(14) . ? Zn3 O9 1.934(14) 1_565 ? Zn3 O10 1.98(2) . ? Zn3 O11 1.981(14) . ? Zn3 O12 2.022(14) . ? Zn4 O13 1.940(15) . ? Zn4 O14 1.943(14) . ? Zn4 O15 1.957(15) . ? Zn4 O4 1.995(15) . ? Zn5 O16 1.927(14) . ? Zn5 O17 1.934(13) . ? Zn5 O18 1.96(2) . ? Zn5 O12 2.009(14) . ? Zn6 O19 1.928(14) . ? Zn6 O20 1.943(15) . ? Zn6 O21 1.973(14) . ? Zn6 O22 1.97(2) 1_545 ? P1 O17 1.526(14) . ? P1 O8 1.547(15) . ? P1 O22 1.55(2) . ? P1 O2 1.556(14) . ? P2 O11 1.52(2) . ? P2 O16 1.53(2) . ? P2 O5 1.540(14) 3_545 ? P2 O4 1.57(2) . ? P3 O19 1.530(14) . ? P3 O13 1.53(2) . ? P3 O1 1.55(2) . ? P3 O12 1.572(15) 1_545 ? P4 O21 1.531(14) 3_535 ? P4 O15 1.534(15) . ? P4 O9 1.53(2) . ? P4 O6 1.54(2) . ? P5 O3 1.507(15) 3_445 ? P5 O18 1.52(2) 3_455 ? P5 O7 1.52(2) . ? P5 O23 1.55(2) . ? P6 O20 1.49(2) 1_565 ? P6 O10 1.51(2) . ? P6 O14 1.55(2) . ? P6 O24 1.581(15) . ? O3 P5 1.507(15) 3_545 ? O5 P2 1.540(14) 3_445 ? O6 Zn2 1.930(15) 3_545 ? O9 Zn3 1.934(14) 1_545 ? O12 P3 1.572(15) 1_565 ? O18 P5 1.52(2) 3 ? O20 P6 1.49(2) 1_545 ? O21 P4 1.531(14) 3_435 ? O22 Zn6 1.97(2) 1_565 ? O23 H23 0.82 . ? O24 H24 0.82 . ? N1 C3 1.50(3) . ? N1 C1 1.53(3) . ? N1 C5 1.53(3) . ? C1 C2 1.52(3) . ? C1 H1 0.97 . ? C1 H2 0.97 . ? C2 N2 1.48(3) . ? C2 H3 0.97 . ? C2 H4 0.97 . ? N2 H5 0.89 . ? N2 H6 0.89 . ? N2 H7 0.89 . ? C3 C4 1.57(3) . ? C3 H8 0.97 . ? C3 H9 0.97 . ? C4 N3 1.50(3) . ? C4 H10 0.97 . ? C4 H11 0.97 . ? N3 H12 0.89 . ? N3 H13 0.89 . ? N3 H14 0.89 . ? C5 C6 1.48(3) . ? C5 H15 0.97 . ? C5 H16 0.97 . ? C6 N4 1.50(3) . ? C6 H17 0.97 . ? C6 H18 0.97 . ? N4 H19 0.89 . ? N4 H20 0.89 . ? N4 H21 0.89 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 114.6(6) . . ? O1 Zn1 O3 109.8(6) . . ? O2 Zn1 O3 100.0(6) . . ? O1 Zn1 O4 103.2(6) . . ? O2 Zn1 O4 120.4(6) . . ? O3 Zn1 O4 108.7(6) . . ? O5 Zn2 O6 122.4(6) . 3_445 ? O5 Zn2 O7 113.0(6) . . ? O6 Zn2 O7 104.1(6) 3_445 . ? O5 Zn2 O8 104.1(6) . . ? O6 Zn2 O8 113.1(6) 3_445 . ? O7 Zn2 O8 97.6(6) . . ? O9 Zn3 O10 98.8(7) 1_565 . ? O9 Zn3 O11 111.8(6) 1_565 . ? O10 Zn3 O11 111.7(7) . . ? O9 Zn3 O12 118.7(6) 1_565 . ? O10 Zn3 O12 112.6(6) . . ? O11 Zn3 O12 103.4(6) . . ? O13 Zn4 O14 106.4(6) . . ? O13 Zn4 O15 115.0(6) . . ? O14 Zn4 O15 107.6(6) . . ? O13 Zn4 O4 105.0(6) . . ? O14 Zn4 O4 118.3(6) . . ? O15 Zn4 O4 105.1(6) . . ? O16 Zn5 O17 115.3(6) . . ? O16 Zn5 O18 106.3(6) . . ? O17 Zn5 O18 106.7(6) . . ? O16 Zn5 O12 104.0(6) . . ? O17 Zn5 O12 108.8(6) . . ? O18 Zn5 O12 116.1(6) . . ? O19 Zn6 O20 111.6(6) . . ? O19 Zn6 O21 102.8(6) . . ? O20 Zn6 O21 114.8(6) . . ? O19 Zn6 O22 127.3(7) . 1_545 ? O20 Zn6 O22 97.7(6) . 1_545 ? O21 Zn6 O22 103.0(6) . 1_545 ? O17 P1 O8 109.8(8) . . ? O17 P1 O22 109.8(9) . . ? O8 P1 O22 108.3(8) . . ? O17 P1 O2 109.7(8) . . ? O8 P1 O2 108.6(8) . . ? O22 P1 O2 110.7(8) . . ? O11 P2 O16 114.4(8) . . ? O11 P2 O5 109.5(8) . 3_545 ? O16 P2 O5 108.3(8) . 3_545 ? O11 P2 O4 107.8(8) . . ? O16 P2 O4 107.5(8) . . ? O5 P2 O4 109.3(8) 3_545 . ? O19 P3 O13 110.3(8) . . ? O19 P3 O1 109.7(8) . . ? O13 P3 O1 112.1(9) . . ? O19 P3 O12 110.2(8) . 1_545 ? O13 P3 O12 107.1(8) . 1_545 ? O1 P3 O12 107.4(8) . 1_545 ? O21 P4 O15 108.1(9) 3_535 . ? O21 P4 O9 107.2(9) 3_535 . ? O15 P4 O9 113.2(8) . . ? O21 P4 O6 109.8(8) 3_535 . ? O15 P4 O6 110.4(9) . . ? O9 P4 O6 108.1(9) . . ? O3 P5 O18 112.3(8) 3_445 3_455 ? O3 P5 O7 113.5(9) 3_445 . ? O18 P5 O7 113.7(9) 3_455 . ? O3 P5 O23 105.8(9) 3_445 . ? O18 P5 O23 103.9(9) 3_455 . ? O7 P5 O23 106.7(8) . . ? O20 P6 O10 116.8(9) 1_565 . ? O20 P6 O14 107.8(9) 1_565 . ? O10 P6 O14 110.1(9) . . ? O20 P6 O24 105.3(9) 1_565 . ? O10 P6 O24 109.0(9) . . ? O14 P6 O24 107.4(8) . . ? P3 O1 Zn1 136.3(9) . . ? P1 O2 Zn1 128.8(8) . . ? P5 O3 Zn1 134.3(9) 3_545 . ? P2 O4 Zn4 119.3(8) . . ? P2 O4 Zn1 114.9(9) . . ? Zn4 O4 Zn1 123.0(8) . . ? P2 O5 Zn2 141.9(9) 3_445 . ? P4 O6 Zn2 130.5(9) . 3_545 ? P5 O7 Zn2 132.5(9) . . ? P1 O8 Zn2 122.2(9) . . ? P4 O9 Zn3 129.6(9) . 1_545 ? P6 O10 Zn3 123.5(10) . . ? P2 O11 Zn3 130.1(8) . . ? P3 O12 Zn5 115.9(8) 1_565 . ? P3 O12 Zn3 119.4(8) 1_565 . ? Zn5 O12 Zn3 123.3(7) . . ? P3 O13 Zn4 131.7(10) . . ? P6 O14 Zn4 125.7(9) . . ? P4 O15 Zn4 130.0(9) . . ? P2 O16 Zn5 131.9(10) . . ? P1 O17 Zn5 131.6(8) . . ? P5 O18 Zn5 136.7(10) 3 . ? P3 O19 Zn6 135.0(9) . . ? P6 O20 Zn6 141.6(10) 1_545 . ? P4 O21 Zn6 129.5(9) 3_435 . ? P1 O22 Zn6 126.5(9) . 1_565 ? P5 O23 H23 109.5(6) . . ? P6 O24 H24 109.5(6) . . ? C3 N1 C1 112.5(17) . . ? C3 N1 C5 106.4(17) . . ? C1 N1 C5 110.5(17) . . ? C2 C1 N1 111.6(18) . . ? C2 C1 H1 109.3(13) . . ? N1 C1 H1 109.3(12) . . ? C2 C1 H2 109.3(13) . . ? N1 C1 H2 109.3(12) . . ? H1 C1 H2 108.0 . . ? N2 C2 C1 108.0(19) . . ? N2 C2 H3 110.1(13) . . ? C1 C2 H3 110.1(13) . . ? N2 C2 H4 110.1(13) . . ? C1 C2 H4 110.1(13) . . ? H3 C2 H4 108.4 . . ? C2 N2 H5 109.5(12) . . ? C2 N2 H6 109.5(13) . . ? H5 N2 H6 109.5 . . ? C2 N2 H7 109.5(13) . . ? H5 N2 H7 109.5 . . ? H6 N2 H7 109.5 . . ? N1 C3 C4 112.7(19) . . ? N1 C3 H8 109.1(11) . . ? C4 C3 H8 109.1(12) . . ? N1 C3 H9 109.1(12) . . ? C4 C3 H9 109.1(12) . . ? H8 C3 H9 107.8 . . ? N3 C4 C3 109.0(19) . . ? N3 C4 H10 109.9(11) . . ? C3 C4 H10 109.9(12) . . ? N3 C4 H11 109.9(12) . . ? C3 C4 H11 109.9(13) . . ? H10 C4 H11 108.3 . . ? C4 N3 H12 109.5(11) . . ? C4 N3 H13 109.5(12) . . ? H12 N3 H13 109.5 . . ? C4 N3 H14 109.5(11) . . ? H12 N3 H14 109.5 . . ? H13 N3 H14 109.5 . . ? C6 C5 N1 115.5(19) . . ? C6 C5 H15 108.4(12) . . ? N1 C5 H15 108.4(11) . . ? C6 C5 H16 108.4(12) . . ? N1 C5 H16 108.4(11) . . ? H15 C5 H16 107.5 . . ? C5 C6 N4 114.5(18) . . ? C5 C6 H17 108.6(12) . . ? N4 C6 H17 108.6(11) . . ? C5 C6 H18 108.6(12) . . ? N4 C6 H18 108.6(11) . . ? H17 C6 H18 107.6 . . ? C6 N4 H19 109.5(11) . . ? C6 N4 H20 109.5(11) . . ? H19 N4 H20 109.5 . . ? C6 N4 H21 109.5(11) . . ? H19 N4 H21 109.5 . . ? H20 N4 H21 109.5 . . ? _refine_diff_density_max 1.097 _refine_diff_density_min -1.372 _refine_diff_density_rms 0.226 eof ******************************************************************************** COMPOUND IV ----------- data_amit _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C2 H0 N0.83 O4 P Zn1.17' _chemical_formula_weight 206.93 _chemical_melting_point ? _chemical_compound_source ? 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 ? _symmetry_space_group_name_H-M ? 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 13.6086(4) _cell_length_b 13.6086(4) _cell_length_c 15.2777(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2450.3(2) _cell_formula_units_Z 18 _cell_measurement_temperature 571(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.524 _exptl_crystal_density_method ? _exptl_crystal_F_000 1797 _exptl_absorpt_coefficient_mu 5.448 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 571(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3418 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 23.26 _reflns_number_total 790 _reflns_number_observed 734 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 790 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_obs 0.0433 _refine_ls_wR_factor_all 0.1622 _refine_ls_wR_factor_obs 0.1549 _refine_ls_goodness_of_fit_all 1.449 _refine_ls_goodness_of_fit_obs 1.440 _refine_ls_restrained_S_all 1.449 _refine_ls_restrained_S_obs 1.440 _refine_ls_shift/esd_max 0.942 _refine_ls_shift/esd_mean 0.167 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.0000 0.0179(6) Uani 1 d S . Zn2 Zn -0.02804(6) 0.21547(6) 0.08991(4) 0.0222(5) Uani 1 d . . P1 P -0.22675(14) -0.02013(13) 0.10648(9) 0.0200(6) Uani 1 d . . O1 O -0.0897(6) 0.2947(6) 0.1490(4) 0.060(2) Uani 1 d . . O2 O 0.1178(4) 0.2567(5) 0.1364(4) 0.046(2) Uani 1 d . . O3 O -0.0243(5) 0.2733(5) -0.0281(3) 0.0463(15) Uani 1 d . . O4 O -0.0998(3) 0.0472(3) 0.0790(3) 0.0235(10) Uani 1 d . . N1 N -0.3333 0.3333 -0.0359(18) 0.149(9) Uiso 1 d S . C1 C -0.2075(45) 0.4601(45) 0.0066(41) 0.346(21) Uiso 1 d . . C2 C -0.1415(28) 0.4312(24) -0.0373(19) 0.212(11) Uiso 1 d . . N2 N 0.0000 0.5000 0.0000 0.124(6) Uiso 1 d S . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0128(7) 0.0128(7) 0.0281(10) 0.000 0.000 0.0064(4) Zn2 0.0259(6) 0.0212(6) 0.0248(7) -0.0044(3) -0.0008(3) 0.0158(4) P1 0.0229(10) 0.0240(10) 0.0179(10) -0.0009(6) 0.0039(6) 0.0154(8) O1 0.091(5) 0.080(5) 0.050(3) -0.024(3) -0.008(3) 0.074(4) O2 0.025(3) 0.049(3) 0.066(4) -0.036(3) -0.014(2) 0.021(3) O3 0.087(4) 0.047(3) 0.029(2) 0.001(2) 0.008(3) 0.052(3) O4 0.016(2) 0.020(2) 0.037(3) -0.001(2) 0.002(2) 0.011(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 Zn1 O4 2.141(4) 10 ? Zn1 O4 2.141(4) 2 ? Zn1 O4 2.141(4) 12 ? Zn1 O4 2.141(4) . ? Zn1 O4 2.141(4) 3 ? Zn1 O4 2.141(4) 11 ? Zn2 O1 1.894(5) . ? Zn2 O2 1.909(5) . ? Zn2 O3 1.958(5) . ? Zn2 O4 1.997(4) . ? P1 O1 1.513(5) 13_455 ? P1 O3 1.521(5) 12 ? P1 O2 1.526(5) 2 ? P1 O4 1.555(4) . ? O1 P1 1.513(5) 13_455 ? O2 P1 1.526(5) 3 ? O3 P1 1.521(5) 11 ? N1 C1 1.84(5) 3_455 ? N1 C1 1.84(5) . ? N1 C1 1.84(5) 2_565 ? C1 C2 1.33(5) . ? C2 N2 1.76(3) . ? N2 C2 1.76(3) 10_565 ? 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 O4 88.7(2) 10 2 ? O4 Zn1 O4 91.4(2) 10 12 ? O4 Zn1 O4 88.7(2) 2 12 ? O4 Zn1 O4 180.0 10 . ? O4 Zn1 O4 91.3(2) 2 . ? O4 Zn1 O4 88.6(2) 12 . ? O4 Zn1 O4 88.7(2) 10 3 ? O4 Zn1 O4 91.4(2) 2 3 ? O4 Zn1 O4 180.0 12 3 ? O4 Zn1 O4 91.3(2) . 3 ? O4 Zn1 O4 91.4(2) 10 11 ? O4 Zn1 O4 180.0 2 11 ? O4 Zn1 O4 91.4(2) 12 11 ? O4 Zn1 O4 88.6(2) . 11 ? O4 Zn1 O4 88.6(2) 3 11 ? O1 Zn2 O2 110.3(2) . . ? O1 Zn2 O3 98.0(2) . . ? O2 Zn2 O3 114.2(3) . . ? O1 Zn2 O4 126.2(3) . . ? O2 Zn2 O4 102.0(2) . . ? O3 Zn2 O4 106.5(2) . . ? O1 P1 O3 112.1(3) 13_455 12 ? O1 P1 O2 107.1(3) 13_455 2 ? O3 P1 O2 111.6(4) 12 2 ? O1 P1 O4 108.6(3) 13_455 . ? O3 P1 O4 107.9(3) 12 . ? O2 P1 O4 109.6(3) 2 . ? P1 O1 Zn2 154.6(4) 13_455 . ? P1 O2 Zn2 131.0(3) 3 . ? P1 O3 Zn2 119.1(3) 11 . ? P1 O4 Zn2 114.5(2) . . ? P1 O4 Zn1 131.3(2) . . ? Zn2 O4 Zn1 111.8(2) . . ? C1 N1 C1 108.2(21) 3_455 . ? C1 N1 C1 108.2(21) 3_455 2_565 ? C1 N1 C1 108.2(21) . 2_565 ? C2 C1 N1 89.6(33) . . ? C1 C2 N2 113.5(31) . . ? C2 N2 C2 179.996(2) . 10_565 ? _refine_diff_density_max 1.471 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.362 eof ******************************************************************************** COMPOUND V ---------- data_test _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H5 N2 O4 P Zn' _chemical_formula_weight 229.43 _chemical_melting_point ? _chemical_compound_source ? 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 ? _symmetry_space_group_name_H-M ? 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 5.1971(6) _cell_length_b 7.6972(9) _cell_length_c 17.336(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.618(2) _cell_angle_gamma 90.00 _cell_volume 693.47(14) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.198 _exptl_crystal_density_method ? _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 3.736 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2830 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 23.34 _reflns_number_total 1007 _reflns_number_observed 909 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+6.0376P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1007 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_obs 0.0434 _refine_ls_wR_factor_all 0.1326 _refine_ls_wR_factor_obs 0.1179 _refine_ls_goodness_of_fit_all 1.334 _refine_ls_goodness_of_fit_obs 1.256 _refine_ls_restrained_S_all 1.334 _refine_ls_restrained_S_obs 1.256 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.6866(2) -0.36421(11) 0.41980(5) 0.0174(4) Uani 1 d . . P1 P 1.1828(4) -0.2623(3) 0.50949(12) 0.0164(5) Uani 1 d . . O1 O 0.3303(11) -0.3129(8) 0.4393(3) 0.0290(15) Uani 1 d . . O2 O 0.7918(12) -0.6059(7) 0.4255(3) 0.0247(14) Uani 1 d . . O3 O 0.9032(10) -0.2247(7) 0.4881(3) 0.0235(14) Uani 1 d . . O4 O 1.2935(11) -0.0912(7) 0.5472(4) 0.0302(15) Uani 1 d . . H5 H 1.2842(11) -0.0095(7) 0.5152(4) 0.045 Uiso 1 calc R . N1 N 0.7464(14) -0.3079(9) 0.3096(4) 0.024(2) Uani 1 d . . N2 N 0.9212(16) -0.2197(11) 0.2012(4) 0.035(2) Uani 1 d . . H4 H 1.0282(16) -0.1693(11) 0.1692(4) 0.042 Uiso 1 calc R . C1 C 0.7066(20) -0.3090(14) 0.1818(6) 0.038(2) Uani 1 d . . H1 H 0.6444(20) -0.3301(14) 0.1309(6) 0.045 Uiso 1 calc R . C2 C 0.9415(18) -0.2220(12) 0.2794(5) 0.030(2) Uani 1 d . . H2 H 1.0767(18) -0.1693(12) 0.3084(5) 0.036 Uiso 1 calc R . C3 C 0.5987(19) -0.3616(12) 0.2462(6) 0.034(2) Uani 1 d . . H3 H 0.4436(19) -0.4264(12) 0.2490(6) 0.041 Uiso 1 calc R . 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 0.0193(6) 0.0165(5) 0.0164(5) 0.0014(4) 0.0001(4) 0.0021(4) P1 0.0162(11) 0.0135(11) 0.0196(11) 0.0015(8) -0.0026(8) 0.0020(8) O1 0.020(3) 0.041(4) 0.025(3) -0.006(3) -0.001(3) 0.006(3) O2 0.033(3) 0.017(3) 0.024(3) 0.001(2) -0.001(3) 0.005(3) O3 0.012(3) 0.021(3) 0.038(4) -0.002(3) -0.004(3) 0.002(2) O4 0.032(4) 0.014(3) 0.044(4) 0.000(3) -0.016(3) -0.003(3) N1 0.030(4) 0.023(4) 0.017(4) 0.001(3) 0.000(3) 0.001(3) N2 0.042(5) 0.045(5) 0.018(4) 0.012(4) 0.007(4) -0.006(4) C1 0.043(6) 0.046(6) 0.024(5) 0.002(5) -0.009(4) 0.003(5) C2 0.029(5) 0.034(5) 0.027(5) 0.007(4) 0.003(4) -0.011(4) C3 0.027(5) 0.036(6) 0.040(6) 0.002(4) -0.006(4) -0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.927(6) . ? Zn1 O2 1.941(6) . ? Zn1 O3 1.947(5) . ? Zn1 N1 1.987(7) . ? P1 O1 1.497(6) 1_655 ? P1 O2 1.521(6) 3_746 ? P1 O3 1.524(6) . ? P1 O4 1.576(6) . ? O1 P1 1.497(6) 1_455 ? O2 P1 1.521(6) 3_746 ? O4 H5 0.84 . ? N1 C2 1.323(12) . ? N1 C3 1.396(12) . ? N2 C1 1.350(13) . ? N2 C2 1.359(12) . ? N2 H4 0.88 . ? C1 C3 1.319(14) . ? C1 H1 0.95 . ? C2 H2 0.95 . ? C3 H3 0.95 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 117.3(3) . . ? O1 Zn1 O3 109.3(2) . . ? O2 Zn1 O3 109.7(2) . . ? O1 Zn1 N1 106.5(3) . . ? O2 Zn1 N1 102.2(3) . . ? O3 Zn1 N1 111.6(3) . . ? O1 P1 O2 112.8(4) 1_655 3_746 ? O1 P1 O3 110.3(3) 1_655 . ? O2 P1 O3 112.5(3) 3_746 . ? O1 P1 O4 111.5(4) 1_655 . ? O2 P1 O4 102.8(3) 3_746 . ? O3 P1 O4 106.6(3) . . ? P1 O1 Zn1 134.2(4) 1_455 . ? P1 O2 Zn1 134.4(4) 3_746 . ? P1 O3 Zn1 126.0(3) . . ? P1 O4 H5 109.5(2) . . ? C2 N1 C3 104.7(8) . . ? C2 N1 Zn1 128.1(6) . . ? C3 N1 Zn1 127.0(6) . . ? C1 N2 C2 107.3(8) . . ? C1 N2 H4 126.4(5) . . ? C2 N2 H4 126.4(5) . . ? C3 C1 N2 107.6(8) . . ? C3 C1 H1 126.2(6) . . ? N2 C1 H1 126.2(5) . . ? N1 C2 N2 110.5(8) . . ? N1 C2 H2 124.8(5) . . ? N2 C2 H2 124.8(5) . . ? C1 C3 N1 109.9(9) . . ? C1 C3 H3 125.0(6) . . ? N1 C3 H3 125.0(5) . . ? _refine_diff_density_max 0.640 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.227 eof ******************************************************************************** COMPOUND VI ----------- data_data _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C H N O P Zn' _chemical_formula_weight 139.37 _chemical_melting_point ? _chemical_compound_source ? 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.0755(2) _cell_length_b 14.8887(2) _cell_length_c 11.8358(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.719(2) _cell_angle_gamma 90.00 _cell_volume 2108.66(7) _cell_formula_units_Z 20 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.195 _exptl_crystal_density_method ? _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 6.008 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4339 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 23.30 _reflns_number_total 1525 _reflns_number_observed 1434 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+6.2079P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1522 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_obs 0.0295 _refine_ls_wR_factor_all 0.0799 _refine_ls_wR_factor_obs 0.0768 _refine_ls_goodness_of_fit_all 1.118 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_restrained_S_all 1.121 _refine_ls_restrained_S_obs 1.115 _refine_ls_shift/esd_max 0.027 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.79550(4) 0.38642(3) 0.04387(3) 0.0152(2) Uani 1 d . . Zn2 Zn 0.59593(4) 0.76319(3) -0.08893(3) 0.0146(2) Uani 1 d . . P1 P 0.66986(8) 0.76170(6) -0.34451(8) 0.0125(3) Uani 1 d . . P2 P 0.75213(8) 0.58879(6) -0.03706(8) 0.0140(3) Uani 1 d . . O1 O 0.9550(3) 0.4075(3) 0.1041(3) 0.0356(9) Uani 1 d . . O2 O 0.7345(2) 0.3282(2) 0.1705(2) 0.0208(6) Uani 1 d . . O3 O 0.7380(2) 0.5081(2) 0.0372(2) 0.0243(7) Uani 1 d . . O4 O 0.7571(2) 0.3305(2) -0.1024(2) 0.0201(6) Uani 1 d . . O5 O 0.4393(2) 0.7486(2) -0.0781(2) 0.0269(7) Uani 1 d . . O6 O 0.6518(2) 0.7980(2) -0.2271(2) 0.0216(6) Uani 1 d . . O7 O 0.6601(2) 0.6545(2) -0.0195(2) 0.0270(7) Uani 1 d . . O8 O 0.6342(2) 0.8665(2) 0.0128(2) 0.0249(7) Uani 1 d . . O9 O 0.7389(2) 0.5543(2) -0.1636(2) 0.0265(7) Uani 1 d . . H7 H 0.7462(2) 0.5966(2) -0.2065(2) 0.040 Uiso 1 calc R . O100 O 1.0000 0.5512(3) 0.2500 0.0270(10) Uani 1 d S . N1 N 0.5990(3) 0.6124(3) 0.1987(3) 0.0343(10) Uani 1 d . . H4 H 0.6345(3) 0.6125(3) 0.1365(3) 0.041 Uiso 1 calc R . H3 H 0.6511(3) 0.6112(3) 0.2606(3) 0.041 Uiso 1 calc R . C1 C 0.5285(4) 0.5314(3) 0.1975(4) 0.0368(11) Uani 1 d . . H2 H 0.5742(4) 0.4780(3) 0.1960(4) 0.044 Uiso 1 calc R . H1 H 0.4732(4) 0.5313(3) 0.1300(4) 0.044 Uiso 1 calc R . C2 C 0.5314(4) 0.6952(3) 0.2003(4) 0.0404(12) Uani 1 d . . H5 H 0.4793(4) 0.6990(3) 0.1305(4) 0.048 Uiso 1 calc R . H6 H 0.5800(4) 0.7472(3) 0.2040(4) 0.048 Uiso 1 calc R . H9 H 1.0186(55) 0.3960(42) 0.0614(55) 0.064(19) Uiso 1 d . . H101 H 1.0566(41) 0.5908(38) 0.2511(48) 0.046(16) Uiso 1 d . . H10 H 0.9606(50) 0.4423(40) 0.1270(54) 0.033(21) Uiso 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 0.0231(3) 0.0113(3) 0.0118(3) -0.0003(2) 0.0048(2) -0.0002(2) Zn2 0.0193(3) 0.0135(3) 0.0116(3) 0.0013(2) 0.0039(2) 0.0024(2) P1 0.0171(5) 0.0119(5) 0.0093(5) -0.0007(4) 0.0041(4) 0.0007(4) P2 0.0208(5) 0.0091(5) 0.0125(5) 0.0010(4) 0.0039(4) 0.0002(4) O1 0.025(2) 0.037(2) 0.046(2) -0.026(2) 0.010(2) -0.006(2) O2 0.035(2) 0.0152(13) 0.0138(14) -0.0006(11) 0.0077(12) -0.0052(12) O3 0.043(2) 0.0132(14) 0.0193(14) 0.0047(11) 0.0133(12) 0.0052(12) O4 0.030(2) 0.0173(14) 0.0132(14) -0.0030(11) 0.0025(11) 0.0056(11) O5 0.021(2) 0.037(2) 0.022(2) 0.0064(13) 0.0026(13) -0.0001(13) O6 0.036(2) 0.0176(14) 0.0129(14) -0.0013(11) 0.0107(12) 0.0018(12) O7 0.029(2) 0.024(2) 0.030(2) 0.0134(13) 0.0110(13) 0.0105(13) O8 0.025(2) 0.027(2) 0.024(2) -0.0123(13) 0.0094(12) -0.0034(13) O9 0.047(2) 0.0191(15) 0.0126(15) 0.0006(12) 0.0025(13) -0.0081(13) O100 0.034(3) 0.018(2) 0.030(2) 0.000 0.002(2) 0.000 N1 0.023(2) 0.064(3) 0.018(2) -0.006(2) 0.009(2) -0.007(2) C1 0.028(2) 0.038(3) 0.042(3) -0.016(2) -0.003(2) 0.007(2) C2 0.043(3) 0.040(3) 0.034(3) 0.013(2) -0.008(2) -0.017(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 Zn1 O4 1.921(3) . ? Zn1 O3 1.938(3) . ? Zn1 O2 1.958(3) . ? Zn1 O1 1.987(4) . ? Zn2 O6 1.922(3) . ? Zn2 O5 1.925(3) . ? Zn2 O7 1.929(3) . ? Zn2 O8 1.969(3) . ? P1 O5 1.513(3) 2_654 ? P1 O6 1.534(3) . ? P1 O4 1.540(3) 4_654 ? P1 O2 1.548(3) 6_565 ? P2 O3 1.512(3) . ? P2 O7 1.516(3) . ? P2 O8 1.519(3) 7_665 ? P2 O9 1.571(3) . ? O1 H9 0.99(6) . ? O1 H10 0.58(6) . ? O2 P1 1.548(3) 6_566 ? O4 P1 1.540(3) 4_644 ? O5 P1 1.513(3) 2_654 ? O8 P2 1.519(3) 7_665 ? O9 H7 0.82 . ? O100 H101 0.90(5) . ? N1 C1 1.475(6) . ? N1 C2 1.481(7) . ? N1 H4 0.90 . ? N1 H3 0.90 . ? C1 C1 1.499(10) 2_655 ? C1 H2 0.97 . ? C1 H1 0.97 . ? C2 C2 1.483(10) 2_655 ? C2 H5 0.97 . ? C2 H6 0.97 . ? 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 O3 109.05(12) . . ? O4 Zn1 O2 115.34(12) . . ? O3 Zn1 O2 105.98(11) . . ? O4 Zn1 O1 119.78(14) . . ? O3 Zn1 O1 101.0(2) . . ? O2 Zn1 O1 103.99(15) . . ? O6 Zn2 O5 123.18(12) . . ? O6 Zn2 O7 114.95(12) . . ? O5 Zn2 O7 102.63(12) . . ? O6 Zn2 O8 103.26(11) . . ? O5 Zn2 O8 101.50(12) . . ? O7 Zn2 O8 110.29(13) . . ? O5 P1 O6 112.0(2) 2_654 . ? O5 P1 O4 109.8(2) 2_654 4_654 ? O6 P1 O4 107.13(15) . 4_654 ? O5 P1 O2 110.0(2) 2_654 6_565 ? O6 P1 O2 109.37(15) . 6_565 ? O4 P1 O2 108.3(2) 4_654 6_565 ? O3 P2 O7 106.9(2) . . ? O3 P2 O8 114.1(2) . 7_665 ? O7 P2 O8 110.6(2) . 7_665 ? O3 P2 O9 106.8(2) . . ? O7 P2 O9 111.1(2) . . ? O8 P2 O9 107.3(2) 7_665 . ? Zn1 O1 H9 124.8(38) . . ? Zn1 O1 H10 110.6(61) . . ? H9 O1 H10 110.0(71) . . ? P1 O2 Zn1 122.1(2) 6_566 . ? P2 O3 Zn1 134.3(2) . . ? P1 O4 Zn1 125.0(2) 4_644 . ? P1 O5 Zn2 136.8(2) 2_654 . ? P1 O6 Zn2 141.7(2) . . ? P2 O7 Zn2 137.9(2) . . ? P2 O8 Zn2 126.2(2) 7_665 . ? P2 O9 H7 109.47(11) . . ? C1 N1 C2 111.2(3) . . ? C1 N1 H4 109.4(2) . . ? C2 N1 H4 109.4(2) . . ? C1 N1 H3 109.4(2) . . ? C2 N1 H3 109.4(2) . . ? H4 N1 H3 108.0 . . ? N1 C1 C1 108.7(3) . 2_655 ? N1 C1 H2 109.9(2) . . ? C1 C1 H2 109.9(2) 2_655 . ? N1 C1 H1 109.9(2) . . ? C1 C1 H1 109.9(4) 2_655 . ? H2 C1 H1 108.3 . . ? N1 C2 C2 110.6(3) . 2_655 ? N1 C2 H5 109.5(2) . . ? C2 C2 H5 109.5(4) 2_655 . ? N1 C2 H6 109.5(2) . . ? C2 C2 H6 109.5(2) 2_655 . ? H5 C2 H6 108.1 . . ? _refine_diff_density_max 0.949 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.154 eof *********************************************************************************