# ic000366c.cif Compound I _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H13 N2 O8 P2 Zn' _chemical_formula_weight 332.46 _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 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 5.2677(5) _cell_length_b 13.3025(13) _cell_length_c 14.7833(14) _cell_angle_alpha 90.00 _cell_angle_beta 96.0490(10) _cell_angle_gamma 90.00 _cell_volume 1030.2(2) _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 2.144 _exptl_crystal_density_method ? _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 2.727 _exptl_absorpt_correction_type none _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4104 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1463 _reflns_number_observed 1291 _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 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^)+(0.0531P)^2^+0.7829P] 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 1463 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_obs 0.0290 _refine_ls_wR_factor_all 0.0916 _refine_ls_wR_factor_obs 0.0783 _refine_ls_goodness_of_fit_all 1.127 _refine_ls_goodness_of_fit_obs 1.033 _refine_ls_restrained_S_all 1.127 _refine_ls_restrained_S_obs 1.033 _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 0.25553(9) 0.98159(4) 0.11203(3) 0.0167(2) Uani 1 d . . P1 P 0.5196(2) 0.93323(8) 0.30328(7) 0.0169(3) Uani 1 d . . P2 P 0.2485(2) 0.89066(8) -0.08934(7) 0.0156(3) Uani 1 d . . O1 O 0.2075(7) 0.8919(2) 0.0105(2) 0.0276(8) Uani 1 d . . O2 O 0.4765(6) 1.0961(2) 0.1066(2) 0.0270(8) Uani 1 d . . O3 O 0.3911(6) 0.8941(2) 0.2127(2) 0.0232(7) Uani 1 d . . O4 O -0.0724(6) 1.0347(2) 0.1439(2) 0.0234(7) Uani 1 d . . O5 O 0.4290(7) 1.0365(2) 0.3272(2) 0.0286(8) Uani 1 d . . O6 O 0.4975(6) 0.8574(2) 0.3787(2) 0.0243(7) Uani 1 d . . O7 O 0.8170(6) 0.9381(3) 0.2944(2) 0.0273(8) Uani 1 d . . H20 H 0.8439(6) 0.9781(3) 0.2543(2) 0.041 Uiso 1 calc R . O8 O 0.1610(6) 0.7842(2) -0.1278(2) 0.0247(8) Uani 1 d . . H30 H 0.2507(6) 0.7405(2) -0.1014(2) 0.037 Uiso 1 calc R . N1 N 0.7463(8) 0.7849(3) 0.7276(3) 0.0285(10) Uani 1 d . . H1 H 0.8185(8) 0.7792(3) 0.7846(3) 0.043 Uiso 1 calc R . H2 H 0.6321(8) 0.7361(3) 0.7160(3) 0.043 Uiso 1 calc R . H3 H 0.6690(8) 0.8443(3) 0.7205(3) 0.043 Uiso 1 calc R . N2 N 0.8019(8) 0.8912(3) 0.5333(3) 0.0286(10) Uani 1 d . . H10 H 0.6874(8) 0.8897(3) 0.4836(3) 0.034 Uiso 1 calc R . H11 H 0.7319(8) 0.9265(3) 0.5763(3) 0.034 Uiso 1 calc R . C3 C 1.0315(9) 0.9456(4) 0.5101(3) 0.0308(12) Uani 1 d . . H9 H 1.0943(9) 0.9146(4) 0.4573(3) 0.037 Uiso 1 calc R . H8 H 1.1647(9) 0.9412(4) 0.5605(3) 0.037 Uiso 1 calc R . C1 C 0.9451(12) 0.7769(5) 0.6641(4) 0.0466(15) Uani 1 d . . H4 H 1.0312(12) 0.7127(5) 0.6737(4) 0.056 Uiso 1 calc R . H5 H 1.0709(12) 0.8293(5) 0.6785(4) 0.056 Uiso 1 calc R . C2 C 0.8450(13) 0.7855(4) 0.5669(4) 0.047(2) Uani 1 d . . H6 H 0.6847(13) 0.7493(4) 0.5573(4) 0.057 Uiso 1 calc R . H7 H 0.9641(13) 0.7530(4) 0.5305(4) 0.057 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 0.0174(3) 0.0182(3) 0.0148(3) -0.0003(2) 0.0027(2) 0.0000(2) P1 0.0223(7) 0.0153(6) 0.0134(6) 0.0004(5) 0.0033(5) 0.0006(5) P2 0.0164(6) 0.0156(6) 0.0152(6) -0.0007(5) 0.0031(5) -0.0008(5) O1 0.046(2) 0.023(2) 0.015(2) -0.0023(13) 0.0070(15) -0.006(2) O2 0.019(2) 0.023(2) 0.040(2) 0.0035(15) 0.0063(15) 0.0007(14) O3 0.031(2) 0.022(2) 0.015(2) 0.0008(13) -0.0030(14) -0.0013(14) O4 0.020(2) 0.028(2) 0.023(2) 0.0064(14) 0.0082(14) 0.0057(14) O5 0.043(2) 0.022(2) 0.022(2) -0.0002(14) 0.010(2) 0.008(2) O6 0.033(2) 0.021(2) 0.019(2) 0.0061(13) 0.0023(14) -0.0043(14) O7 0.025(2) 0.037(2) 0.020(2) 0.0054(15) 0.0048(14) 0.000(2) O8 0.023(2) 0.021(2) 0.029(2) -0.0066(14) 0.0002(14) -0.0009(14) N1 0.039(3) 0.021(2) 0.025(2) 0.003(2) 0.003(2) 0.001(2) N2 0.039(3) 0.034(2) 0.014(2) -0.002(2) 0.005(2) 0.010(2) C3 0.026(3) 0.044(3) 0.022(3) -0.009(2) 0.000(2) 0.007(2) C1 0.056(4) 0.042(4) 0.042(3) 0.006(3) 0.009(3) 0.011(3) C2 0.075(5) 0.031(3) 0.039(3) 0.000(3) 0.014(3) 0.015(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 O1 1.913(3) . ? Zn1 O2 1.924(3) . ? Zn1 O3 1.964(3) . ? Zn1 O4 1.969(3) . ? P1 O5 1.509(3) . ? P1 O6 1.517(3) . ? P1 O3 1.527(3) . ? P1 O7 1.587(3) . ? P2 O2 1.508(3) 3_675 ? P2 O1 1.515(3) . ? P2 O4 1.530(3) 3_575 ? P2 O8 1.577(3) . ? O2 P2 1.508(3) 3_675 ? O4 P2 1.530(3) 3_575 ? O7 H20 0.82 . ? O8 H30 0.82 . ? N1 C1 1.482(7) . ? N1 H1 0.89 . ? N1 H2 0.89 . ? N1 H3 0.89 . ? N2 C3 1.480(6) . ? N2 C2 1.501(7) . ? N2 H10 0.90 . ? N2 H11 0.90 . ? C3 C3 1.508(10) 3_776 ? C3 H9 0.97 . ? C3 H8 0.97 . ? C1 C2 1.483(8) . ? C1 H4 0.97 . ? C1 H5 0.97 . ? C2 H6 0.97 . ? C2 H7 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 O1 Zn1 O2 119.45(14) . . ? O1 Zn1 O3 103.42(13) . . ? O2 Zn1 O3 109.14(13) . . ? O1 Zn1 O4 111.40(14) . . ? O2 Zn1 O4 106.01(13) . . ? O3 Zn1 O4 106.81(12) . . ? O5 P1 O6 112.5(2) . . ? O5 P1 O3 113.2(2) . . ? O6 P1 O3 110.9(2) . . ? O5 P1 O7 108.8(2) . . ? O6 P1 O7 103.9(2) . . ? O3 P1 O7 107.0(2) . . ? O2 P2 O1 113.7(2) 3_675 . ? O2 P2 O4 112.0(2) 3_675 3_575 ? O1 P2 O4 111.5(2) . 3_575 ? O2 P2 O8 107.1(2) 3_675 . ? O1 P2 O8 107.1(2) . . ? O4 P2 O8 104.8(2) 3_575 . ? P2 O1 Zn1 138.6(2) . . ? P2 O2 Zn1 134.1(2) 3_675 . ? P1 O3 Zn1 123.7(2) . . ? P2 O4 Zn1 127.2(2) 3_575 . ? P1 O7 H20 109.47(12) . . ? P2 O8 H30 109.47(12) . . ? C1 N1 H1 109.5(3) . . ? C1 N1 H2 109.5(3) . . ? H1 N1 H2 109.5 . . ? C1 N1 H3 109.5(3) . . ? H1 N1 H3 109.5 . . ? H2 N1 H3 109.5 . . ? C3 N2 C2 115.8(4) . . ? C3 N2 H10 108.3(2) . . ? C2 N2 H10 108.3(3) . . ? C3 N2 H11 108.3(2) . . ? C2 N2 H11 108.3(3) . . ? H10 N2 H11 107.4 . . ? N2 C3 C3 110.3(5) . 3_776 ? N2 C3 H9 109.6(2) . . ? C3 C3 H9 109.6(4) 3_776 . ? N2 C3 H8 109.6(2) . . ? C3 C3 H8 109.6(4) 3_776 . ? H9 C3 H8 108.1 . . ? N1 C1 C2 113.9(5) . . ? N1 C1 H4 108.8(3) . . ? C2 C1 H4 108.8(3) . . ? N1 C1 H5 108.8(3) . . ? C2 C1 H5 108.8(3) . . ? H4 C1 H5 107.7 . . ? C1 C2 N2 114.8(5) . . ? C1 C2 H6 108.6(4) . . ? N2 C2 H6 108.6(3) . . ? C1 C2 H7 108.6(3) . . ? N2 C2 H7 108.6(3) . . ? H6 C2 H7 107.5 . . ? _refine_diff_density_max 0.877 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.153 #===END Compound II _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H14 N2 O12 P3 Zn2' _chemical_formula_weight 493.81 _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 7.5151(6) _cell_length_b 8.2553(7) _cell_length_c 12.9115(11) _cell_angle_alpha 98.6540(10) _cell_angle_beta 101.274(2) _cell_angle_gamma 115.7910(10) _cell_volume 681.69(10) _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 2.406 _exptl_crystal_density_method ? _exptl_crystal_F_000 494 _exptl_absorpt_coefficient_mu 3.938 _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 2853 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.27 _reflns_number_total 1910 _reflns_number_observed 1628 _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 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^)+(0.0619P)^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 1910 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_obs 0.0345 _refine_ls_wR_factor_all 0.1017 _refine_ls_wR_factor_obs 0.0928 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_goodness_of_fit_obs 1.045 _refine_ls_restrained_S_all 1.047 _refine_ls_restrained_S_obs 1.045 _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 0.40696(10) 0.23211(8) -0.00331(5) 0.0153(2) Uani 1 d . . Zn2 Zn 0.16836(9) 0.60046(8) -0.31855(5) 0.0145(2) Uani 1 d . . P1 P 0.4269(2) 0.4326(2) -0.19402(11) 0.0130(3) Uani 1 d . . P2 P 0.8143(2) 0.2023(2) 0.08455(11) 0.0143(4) Uani 1 d . . P3 P 0.2978(2) 0.6376(2) -0.53136(11) 0.0148(4) Uani 1 d . . O1 O 0.1874(6) -0.0212(5) -0.0380(3) 0.0214(9) Uani 1 d . . O2 O 0.6722(6) 0.2435(6) 0.0040(3) 0.0231(9) Uani 1 d . . O3 O 0.3168(6) 0.3391(5) -0.1153(3) 0.0200(9) Uani 1 d . . O4 O 0.4004(6) 0.3688(5) 0.1355(3) 0.0201(9) Uani 1 d . . O5 O 0.2277(7) 0.7928(6) -0.1947(3) 0.0307(11) Uani 1 d . . O6 O 0.2873(6) 0.7239(5) -0.4229(3) 0.0250(10) Uani 1 d . . O7 O 0.2726(6) 0.4266(5) -0.2927(3) 0.0242(10) Uani 1 d . . O8 O -0.1214(6) 0.3932(5) -0.3721(3) 0.0212(9) Uani 1 d . . O9 O 0.5255(6) 0.3132(5) -0.2407(3) 0.0205(9) Uani 1 d . . H40 H 0.6101(6) 0.3126(5) -0.1901(3) 0.031 Uiso 1 calc R . O10 O 1.0369(6) 0.3665(5) 0.0965(4) 0.0317(11) Uani 1 d . . H30 H 1.0432(6) 0.4672(5) 0.1207(4) 0.048 Uiso 1 calc R . O11 O 0.5054(6) 0.7499(6) -0.5501(3) 0.0328(11) Uani 1 d . . O12 O 0.2606(7) 0.4318(6) -0.5342(4) 0.0329(11) Uani 1 d . . H20 H 0.3500(7) 0.4361(6) -0.4842(4) 0.049 Uiso 1 calc R . N2 N 0.8643(7) 0.0209(6) -0.3946(4) 0.0183(11) Uani 1 d . . H9 H 0.7369(7) -0.0513(6) -0.4420(4) 0.022 Uiso 1 calc R . H8 H 0.8926(7) 0.1407(6) -0.3854(4) 0.022 Uiso 1 calc R . N1 N 0.8755(7) 0.2513(7) -0.1710(4) 0.0211(11) Uani 1 d . . H3 H 0.8037(7) 0.2867(7) -0.1346(4) 0.032 Uiso 1 calc R . H2 H 0.8989(7) 0.3111(7) -0.2229(4) 0.032 Uiso 1 calc R . H1 H 0.9955(7) 0.2787(7) -0.1249(4) 0.032 Uiso 1 calc R . C1 C 0.7539(9) 0.0435(8) -0.2232(5) 0.0235(14) Uani 1 d . . H5 H 0.6221(9) 0.0141(8) -0.2723(5) 0.028 Uiso 1 calc R . H4 H 0.7264(9) -0.0209(8) -0.1666(5) 0.028 Uiso 1 calc R . C2 C 0.8673(10) -0.0260(8) -0.2866(5) 0.0225(14) Uani 1 d . . H6 H 1.0098(10) 0.0278(8) -0.2423(5) 0.027 Uiso 1 calc R . H7 H 0.8053(10) -0.1605(8) -0.2994(5) 0.027 Uiso 1 calc R . C3 C 1.0180(9) -0.0079(8) -0.4418(5) 0.0216(13) Uani 1 d . . H10 H 1.0034(9) -0.1302(8) -0.4407(5) 0.026 Uiso 1 calc R . H11 H 1.1571(9) 0.0853(8) -0.3983(5) 0.026 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 0.0149(4) 0.0122(4) 0.0178(4) 0.0013(3) 0.0049(3) 0.0065(3) Zn2 0.0158(4) 0.0135(4) 0.0135(4) 0.0027(3) 0.0044(3) 0.0066(3) P1 0.0135(8) 0.0107(8) 0.0137(8) 0.0003(6) 0.0026(6) 0.0064(6) P2 0.0126(8) 0.0104(8) 0.0163(8) -0.0013(6) 0.0035(6) 0.0041(6) P3 0.0120(8) 0.0150(8) 0.0143(8) 0.0018(6) 0.0034(6) 0.0047(7) O1 0.021(2) 0.011(2) 0.029(2) -0.003(2) 0.008(2) 0.007(2) O2 0.019(2) 0.029(2) 0.025(2) 0.007(2) 0.008(2) 0.014(2) O3 0.019(2) 0.022(2) 0.023(2) 0.008(2) 0.009(2) 0.011(2) O4 0.018(2) 0.015(2) 0.023(2) 0.000(2) 0.008(2) 0.006(2) O5 0.048(3) 0.023(2) 0.023(2) 0.003(2) 0.016(2) 0.017(2) O6 0.036(3) 0.018(2) 0.019(2) 0.003(2) 0.013(2) 0.009(2) O7 0.029(2) 0.022(2) 0.020(2) -0.002(2) -0.002(2) 0.017(2) O8 0.014(2) 0.026(2) 0.020(2) 0.008(2) 0.002(2) 0.008(2) O9 0.020(2) 0.024(2) 0.021(2) 0.001(2) 0.000(2) 0.017(2) O10 0.017(2) 0.008(2) 0.061(3) 0.004(2) 0.007(2) 0.002(2) O11 0.013(2) 0.043(3) 0.021(2) -0.005(2) 0.005(2) -0.001(2) O12 0.031(3) 0.024(3) 0.039(3) 0.002(2) -0.001(2) 0.016(2) N2 0.017(3) 0.015(3) 0.020(3) 0.000(2) 0.004(2) 0.007(2) N1 0.026(3) 0.021(3) 0.019(3) 0.001(2) 0.007(2) 0.014(2) C1 0.028(4) 0.015(3) 0.023(3) 0.003(3) 0.015(3) 0.004(3) C2 0.034(4) 0.017(3) 0.021(3) 0.006(3) 0.011(3) 0.015(3) C3 0.017(3) 0.021(3) 0.022(3) 0.000(3) 0.006(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.929(4) . ? Zn1 O2 1.937(4) . ? Zn1 O3 1.963(4) . ? Zn1 O4 1.991(4) . ? Zn2 O5 1.902(4) . ? Zn2 O6 1.936(4) . ? Zn2 O7 1.951(4) . ? Zn2 O8 1.990(4) . ? P1 O7 1.524(4) . ? P1 O3 1.524(4) . ? P1 O4 1.528(4) 2_665 ? P1 O9 1.586(4) . ? P2 O5 1.514(4) 2_665 ? P2 O1 1.519(4) 2_655 ? P2 O2 1.525(4) . ? P2 O10 1.588(4) . ? P3 O6 1.505(4) . ? P3 O11 1.520(4) . ? P3 O8 1.530(4) 2_564 ? P3 O12 1.591(4) . ? O1 P2 1.519(4) 2_655 ? O4 P1 1.528(4) 2_665 ? O5 P2 1.514(4) 2_665 ? O8 P3 1.530(4) 2_564 ? O9 H40 0.82 . ? O10 H30 0.82 . ? O12 H20 0.82 . ? N2 C3 1.495(7) . ? N2 C2 1.502(7) . ? N2 H9 0.90 . ? N2 H8 0.90 . ? N1 C1 1.510(7) . ? N1 H3 0.89 . ? N1 H2 0.89 . ? N1 H1 0.89 . ? C1 C2 1.511(8) . ? C1 H5 0.97 . ? C1 H4 0.97 . ? C2 H6 0.97 . ? C2 H7 0.97 . ? C3 C3 1.509(11) 2_754 ? C3 H10 0.97 . ? C3 H11 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 O1 Zn1 O2 112.1(2) . . ? O1 Zn1 O3 105.1(2) . . ? O2 Zn1 O3 114.2(2) . . ? O1 Zn1 O4 106.7(2) . . ? O2 Zn1 O4 113.5(2) . . ? O3 Zn1 O4 104.5(2) . . ? O5 Zn2 O6 106.4(2) . . ? O5 Zn2 O7 116.7(2) . . ? O6 Zn2 O7 108.5(2) . . ? O5 Zn2 O8 115.7(2) . . ? O6 Zn2 O8 118.2(2) . . ? O7 Zn2 O8 91.1(2) . . ? O7 P1 O3 110.7(2) . . ? O7 P1 O4 112.2(2) . 2_665 ? O3 P1 O4 111.3(2) . 2_665 ? O7 P1 O9 106.1(2) . . ? O3 P1 O9 107.7(2) . . ? O4 P1 O9 108.7(2) 2_665 . ? O5 P2 O1 111.0(2) 2_665 2_655 ? O5 P2 O2 112.9(2) 2_665 . ? O1 P2 O2 112.7(2) 2_655 . ? O5 P2 O10 110.5(2) 2_665 . ? O1 P2 O10 106.6(2) 2_655 . ? O2 P2 O10 102.6(2) . . ? O6 P3 O11 111.9(2) . . ? O6 P3 O8 112.7(2) . 2_564 ? O11 P3 O8 110.5(2) . 2_564 ? O6 P3 O12 108.8(2) . . ? O11 P3 O12 109.2(3) . . ? O8 P3 O12 103.3(2) 2_564 . ? P2 O1 Zn1 129.1(2) 2_655 . ? P2 O2 Zn1 132.9(3) . . ? P1 O3 Zn1 129.5(2) . . ? P1 O4 Zn1 120.0(2) 2_665 . ? P2 O5 Zn2 134.9(3) 2_665 . ? P3 O6 Zn2 128.4(2) . . ? P1 O7 Zn2 131.5(2) . . ? P3 O8 Zn2 128.6(2) 2_564 . ? P1 O9 H40 109.47(15) . . ? P2 O10 H30 109.5(2) . . ? P3 O12 H20 109.5(2) . . ? C3 N2 C2 111.8(4) . . ? C3 N2 H9 109.3(3) . . ? C2 N2 H9 109.3(3) . . ? C3 N2 H8 109.3(3) . . ? C2 N2 H8 109.3(3) . . ? H9 N2 H8 107.9 . . ? C1 N1 H3 109.5(3) . . ? C1 N1 H2 109.5(3) . . ? H3 N1 H2 109.5 . . ? C1 N1 H1 109.5(3) . . ? H3 N1 H1 109.5 . . ? H2 N1 H1 109.5 . . ? N1 C1 C2 112.2(5) . . ? N1 C1 H5 109.2(3) . . ? C2 C1 H5 109.2(3) . . ? N1 C1 H4 109.2(3) . . ? C2 C1 H4 109.2(3) . . ? H5 C1 H4 107.9 . . ? N2 C2 C1 113.5(5) . . ? N2 C2 H6 108.9(3) . . ? C1 C2 H6 108.9(3) . . ? N2 C2 H7 108.9(3) . . ? C1 C2 H7 108.9(3) . . ? H6 C2 H7 107.7 . . ? N2 C3 C3 109.3(6) . 2_754 ? N2 C3 H10 109.8(3) . . ? C3 C3 H10 109.8(5) 2_754 . ? N2 C3 H11 109.8(3) . . ? C3 C3 H11 109.8(4) 2_754 . ? H10 C3 H11 108.3 . . ? _refine_diff_density_max 0.633 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.168 #===END Compound III _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H11 N2 O8 P2 Zn2' _chemical_formula_weight 395.82 _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 8.0636(9) _cell_length_b 8.4566(10) _cell_length_c 9.0234(11) _cell_angle_alpha 111.941(2) _cell_angle_beta 107.957(2) _cell_angle_gamma 103.649(2) _cell_volume 498.09(10) _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 2.639 _exptl_crystal_density_method ? _exptl_crystal_F_000 394 _exptl_absorpt_coefficient_mu 5.172 _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 2113 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 23.30 _reflns_number_total 1400 _reflns_number_observed 1184 _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 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^)+(0.0653P)^2^+1.1810P] 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 1400 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_obs 0.0437 _refine_ls_wR_factor_all 0.1152 _refine_ls_wR_factor_obs 0.1094 _refine_ls_goodness_of_fit_all 1.059 _refine_ls_goodness_of_fit_obs 1.104 _refine_ls_restrained_S_all 1.059 _refine_ls_restrained_S_obs 1.104 _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 -0.29541(10) -0.02043(10) -1.02795(9) 0.0150(3) Uani 1 d . . Zn2 Zn 0.01991(11) -0.46110(12) -0.72127(11) 0.0227(3) Uani 1 d . . P1 P -0.3158(2) -0.7188(2) -0.6829(2) 0.0158(4) Uani 1 d . . P2 P -0.0178(2) -0.2370(3) -0.9536(2) 0.0199(5) Uani 1 d . . O1 O -0.3266(20) -0.8902(10) -0.8239(14) 0.137(5) Uani 1 d . . O2 O -0.1957(6) 0.1438(7) -1.1121(6) 0.0252(12) Uani 1 d . . O3 O -0.1003(7) -0.0876(7) -0.9110(7) 0.0278(12) Uani 1 d . . O4 O -0.4832(7) -0.2676(10) -1.2675(9) 0.052(2) Uani 1 d . . O5 O 0.2334(8) -0.2861(9) -0.4924(8) 0.049(2) Uani 1 d . . O6 O -0.0601(7) -0.3432(9) -0.8575(9) 0.042(2) Uani 1 d . . O7 O 0.1167(7) -0.6330(7) -0.8438(7) 0.0346(14) Uani 1 d . . O8 O -0.2015(6) -0.5422(7) -0.6781(6) 0.0233(11) Uani 1 d . . N2 N 0.5209(9) 0.4040(8) -0.2154(7) 0.0236(14) Uani 1 d . . H9 H 0.6460(9) 0.4655(8) -0.1770(7) 0.028 Uiso 1 calc R . H8 H 0.4590(9) 0.4643(8) -0.2585(7) 0.028 Uiso 1 calc R . N1 N 0.1978(9) 0.2165(9) -0.5929(8) 0.028(2) Uani 1 d . . H3 H 0.0732(9) 0.1637(9) -0.6621(8) 0.042 Uiso 1 calc R . H2 H 0.2595(9) 0.2035(9) -0.6603(8) 0.042 Uiso 1 calc R . H1 H 0.2319(9) 0.3368(9) -0.5222(8) 0.042 Uiso 1 calc R . C1 C 0.2463(11) 0.1249(10) -0.4820(9) 0.024(2) Uani 1 d . . H5 H 0.2070(11) -0.0065(10) -0.5593(9) 0.029 Uiso 1 calc R . H4 H 0.1772(11) 0.1374(10) -0.4102(9) 0.029 Uiso 1 calc R . C2 C 0.4564(10) 0.2098(10) -0.3622(9) 0.023(2) Uani 1 d . . H7 H 0.4862(10) 0.1324(10) -0.3103(9) 0.028 Uiso 1 calc R . H6 H 0.5256(10) 0.2128(10) -0.4327(9) 0.028 Uiso 1 calc R . C3 C 0.4857(10) 0.4045(10) -0.0632(8) 0.019(2) Uani 1 d . . H10 H 0.5718(10) 0.3630(10) -0.0011(8) 0.023 Uiso 1 calc R . H11 H 0.3567(10) 0.3187(10) -0.1070(8) 0.023 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 0.0107(4) 0.0174(5) 0.0154(5) 0.0090(4) 0.0037(3) 0.0038(3) Zn2 0.0128(5) 0.0276(5) 0.0319(5) 0.0237(4) 0.0051(4) 0.0055(4) P1 0.0167(9) 0.0137(9) 0.0146(9) 0.0063(7) 0.0070(7) 0.0028(7) P2 0.0113(9) 0.0231(10) 0.0269(10) 0.0199(9) 0.0030(8) 0.0033(8) O1 0.327(16) 0.037(5) 0.139(8) 0.047(5) 0.201(10) 0.078(7) O2 0.012(2) 0.036(3) 0.032(3) 0.025(3) 0.006(2) 0.007(2) O3 0.020(3) 0.038(3) 0.038(3) 0.029(3) 0.010(2) 0.016(2) O4 0.012(3) 0.087(5) 0.075(4) 0.067(4) 0.011(3) 0.010(3) O5 0.020(3) 0.066(4) 0.047(4) 0.047(3) -0.006(3) -0.011(3) O6 0.018(3) 0.065(4) 0.077(4) 0.063(4) 0.022(3) 0.018(3) O7 0.031(3) 0.023(3) 0.032(3) 0.010(2) -0.002(2) 0.009(2) O8 0.014(2) 0.025(3) 0.029(3) 0.018(2) 0.006(2) 0.000(2) N2 0.024(3) 0.020(3) 0.022(3) 0.009(3) 0.009(3) 0.003(3) N1 0.033(4) 0.025(4) 0.021(3) 0.009(3) 0.007(3) 0.014(3) C1 0.032(4) 0.017(4) 0.017(4) 0.007(3) 0.008(3) 0.005(3) C2 0.033(4) 0.021(4) 0.013(3) 0.005(3) 0.012(3) 0.009(3) C3 0.026(4) 0.020(4) 0.012(3) 0.007(3) 0.009(3) 0.009(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 O1 1.889(6) 1_565 ? Zn1 O3 1.939(5) . ? Zn1 O2 1.947(5) . ? Zn1 O4 2.109(7) . ? Zn2 O6 1.911(5) . ? Zn2 O5 1.934(5) . ? Zn2 O7 1.952(5) . ? Zn2 O8 1.965(5) . ? P1 O1 1.490(7) . ? P1 O5 1.495(5) 2_544 ? P1 O4 1.505(6) 2_443 ? P1 O8 1.536(5) . ? P2 O6 1.515(6) . ? P2 O2 1.522(5) 2_553 ? P2 O7 1.540(5) 2_543 ? P2 O3 1.542(5) . ? O1 Zn1 1.889(6) 1_545 ? O2 P2 1.522(5) 2_553 ? O4 P1 1.505(6) 2_443 ? O5 P1 1.495(5) 2_544 ? O7 P2 1.540(5) 2_543 ? N2 C3 1.484(9) . ? N2 C2 1.506(9) . ? N2 H9 0.90 . ? N2 H8 0.90 . ? N1 C1 1.494(9) . ? N1 H3 0.89 . ? N1 H2 0.89 . ? N1 H1 0.89 . ? C1 C2 1.507(10) . ? C1 H5 0.97 . ? C1 H4 0.97 . ? C2 H7 0.97 . ? C2 H6 0.97 . ? C3 C3 1.499(13) 2_665 ? C3 H10 0.97 . ? C3 H11 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 O1 Zn1 O3 95.9(4) 1_565 . ? O1 Zn1 O2 111.6(3) 1_565 . ? O3 Zn1 O2 110.7(2) . . ? O1 Zn1 O4 131.0(4) 1_565 . ? O3 Zn1 O4 104.1(2) . . ? O2 Zn1 O4 102.3(2) . . ? O6 Zn2 O5 111.9(3) . . ? O6 Zn2 O7 108.4(3) . . ? O5 Zn2 O7 104.6(3) . . ? O6 Zn2 O8 101.6(2) . . ? O5 Zn2 O8 107.4(2) . . ? O7 Zn2 O8 123.0(2) . . ? O1 P1 O5 108.9(5) . 2_544 ? O1 P1 O4 106.2(6) . 2_443 ? O5 P1 O4 110.8(3) 2_544 2_443 ? O1 P1 O8 112.0(4) . . ? O5 P1 O8 111.5(3) 2_544 . ? O4 P1 O8 107.3(3) 2_443 . ? O6 P2 O2 110.5(3) . 2_553 ? O6 P2 O7 110.5(3) . 2_543 ? O2 P2 O7 110.8(3) 2_553 2_543 ? O6 P2 O3 106.8(3) . . ? O2 P2 O3 109.6(3) 2_553 . ? O7 P2 O3 108.6(3) 2_543 . ? P1 O1 Zn1 153.1(5) . 1_545 ? P2 O2 Zn1 120.1(3) 2_553 . ? P2 O3 Zn1 140.4(3) . . ? P1 O4 Zn1 110.1(4) 2_443 . ? P1 O5 Zn2 135.3(4) 2_544 . ? P2 O6 Zn2 149.3(3) . . ? P2 O7 Zn2 123.2(3) 2_543 . ? P1 O8 Zn2 135.9(3) . . ? C3 N2 C2 112.1(5) . . ? C3 N2 H9 109.2(4) . . ? C2 N2 H9 109.2(4) . . ? C3 N2 H8 109.2(4) . . ? C2 N2 H8 109.2(4) . . ? H9 N2 H8 107.9 . . ? C1 N1 H3 109.5(4) . . ? C1 N1 H2 109.5(4) . . ? H3 N1 H2 109.5 . . ? C1 N1 H1 109.5(4) . . ? H3 N1 H1 109.5 . . ? H2 N1 H1 109.5 . . ? N1 C1 C2 111.4(6) . . ? N1 C1 H5 109.3(4) . . ? C2 C1 H5 109.3(4) . . ? N1 C1 H4 109.3(4) . . ? C2 C1 H4 109.3(4) . . ? H5 C1 H4 108.0 . . ? N2 C2 C1 112.4(6) . . ? N2 C2 H7 109.1(4) . . ? C1 C2 H7 109.1(4) . . ? N2 C2 H6 109.1(4) . . ? C1 C2 H6 109.1(4) . . ? H7 C2 H6 107.9 . . ? N2 C3 C3 110.7(7) . 2_665 ? N2 C3 H10 109.5(4) . . ? C3 C3 H10 109.5(5) 2_665 . ? N2 C3 H11 109.5(4) . . ? C3 C3 H11 109.5(6) 2_665 . ? H10 C3 H11 108.1 . . ? _refine_diff_density_max 1.470 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.188 #===END Compound IV _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H12 N2 O12 P3 Zn3' _chemical_formula_weight 557.17 _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 5.2176(2) _cell_length_b 8.7802(4) _cell_length_c 16.0811(7) _cell_angle_alpha 89.340(2) _cell_angle_beta 83.5370(10) _cell_angle_gamma 74.3370(10) _cell_volume 704.70(5) _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 2.626 _exptl_crystal_density_method ? _exptl_crystal_F_000 550 _exptl_absorpt_coefficient_mu 5.472 _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 2957 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1980 _reflns_number_observed 1728 _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 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^)+(0.0735P)^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 0.0427(30) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1980 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_obs 0.0423 _refine_ls_wR_factor_all 0.1222 _refine_ls_wR_factor_obs 0.1061 _refine_ls_goodness_of_fit_all 1.062 _refine_ls_goodness_of_fit_obs 0.995 _refine_ls_restrained_S_all 1.062 _refine_ls_restrained_S_obs 0.995 _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 0.10879(14) 0.13868(8) 0.05956(5) 0.0143(3) Uani 1 d . . Zn2 Zn -0.23975(14) 0.44126(9) 0.40412(5) 0.0157(3) Uani 1 d . . Zn3 Zn 0.57202(15) -0.55643(9) 0.13268(5) 0.0164(3) Uani 1 d . . P1 P 0.0653(3) 0.3398(2) 0.22842(10) 0.0130(4) Uani 1 d . . P2 P 0.3745(3) -0.2331(2) 0.03101(10) 0.0122(4) Uani 1 d . . P3 P -0.1730(3) 0.3465(2) 0.59170(11) 0.0131(4) Uani 1 d . . O1 O 0.3506(9) 0.2066(6) -0.0221(3) 0.0241(12) Uani 1 d . . O2 O 0.1435(9) 0.1930(5) 0.1735(3) 0.0216(11) Uani 1 d . . O3 O 0.1544(9) -0.0883(5) 0.0692(3) 0.0193(11) Uani 1 d . . O4 O -0.2862(9) 0.2589(5) 0.0567(3) 0.0164(10) Uani 1 d . . O5 O -0.0195(9) 0.3001(5) 0.3173(3) 0.0173(11) Uani 1 d . . O6 O -0.2511(9) 0.3236(5) 0.5054(3) 0.0196(11) Uani 1 d . . O7 O -0.1040(9) 0.6239(5) 0.4104(3) 0.0219(11) Uani 1 d . . O8 O -0.6090(8) 0.5047(5) 0.3672(3) 0.0212(12) Uani 1 d . . O9 O 0.3598(9) -0.3715(5) 0.0872(3) 0.0221(11) Uani 1 d . . O10 O 0.8527(9) -0.5239(5) 0.1938(3) 0.0203(11) Uani 1 d . . O11 O 0.3224(9) -0.5978(6) 0.2313(3) 0.0184(11) Uani 1 d . . O12 O -0.1729(10) 0.2005(6) 0.6434(3) 0.0242(12) Uani 1 d . . H20 H -0.1308(10) 0.2131(6) 0.6900(3) 0.036 Uiso 1 calc R . N2 N 0.4436(11) 0.0619(6) 0.6143(3) 0.0172(13) Uani 1 d . . H8 H 0.3030(11) 0.1460(6) 0.6092(3) 0.021 Uiso 1 calc R . H9 H 0.5891(11) 0.0977(6) 0.6161(3) 0.021 Uiso 1 calc R . N1 N 0.0977(11) 0.2029(7) 0.7875(4) 0.0228(14) Uani 1 d . . H3 H 0.0942(11) 0.2617(7) 0.8325(4) 0.034 Uiso 1 calc R . H2 H -0.0273(11) 0.1509(7) 0.7965(4) 0.034 Uiso 1 calc R . H1 H 0.0657(11) 0.2650(7) 0.7436(4) 0.034 Uiso 1 calc R . C1 C 0.3650(14) 0.0879(9) 0.7706(5) 0.028(2) Uani 1 d . . H5 H 0.3998(14) 0.0227(9) 0.8193(5) 0.034 Uiso 1 calc R . H4 H 0.5000(14) 0.1456(9) 0.7623(5) 0.034 Uiso 1 calc R . C2 C 0.3927(15) -0.0184(9) 0.6951(5) 0.027(2) Uani 1 d . . H6 H 0.5395(15) -0.1123(9) 0.6993(5) 0.032 Uiso 1 calc R . H7 H 0.2300(15) -0.0516(9) 0.6947(5) 0.032 Uiso 1 calc R . C3 C 0.4866(17) -0.0442(9) 0.5395(5) 0.028(2) Uani 1 d . . H11 H 0.3366(17) -0.0897(9) 0.5395(5) 0.033 Uiso 1 calc R . H10 H 0.6475(17) -0.1301(9) 0.5421(5) 0.033 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 0.0149(5) 0.0141(5) 0.0142(5) -0.0006(3) -0.0045(3) -0.0034(3) Zn2 0.0168(5) 0.0180(5) 0.0143(5) -0.0003(3) -0.0047(3) -0.0069(3) Zn3 0.0182(5) 0.0151(5) 0.0162(5) -0.0011(3) -0.0097(3) -0.0017(3) P1 0.0132(9) 0.0161(9) 0.0111(9) -0.0006(7) -0.0055(7) -0.0048(7) P2 0.0123(9) 0.0138(9) 0.0109(9) 0.0003(7) -0.0045(7) -0.0029(7) P3 0.0134(9) 0.0155(9) 0.0125(9) 0.0004(7) -0.0069(7) -0.0055(7) O1 0.019(3) 0.042(3) 0.018(3) 0.005(2) -0.008(2) -0.017(2) O2 0.024(3) 0.023(3) 0.018(3) -0.005(2) -0.009(2) -0.004(2) O3 0.024(3) 0.014(2) 0.018(3) 0.000(2) -0.004(2) -0.001(2) O4 0.017(2) 0.019(2) 0.014(2) -0.003(2) -0.007(2) -0.002(2) O5 0.022(3) 0.016(2) 0.017(3) 0.000(2) -0.003(2) -0.009(2) O6 0.030(3) 0.023(3) 0.013(3) 0.002(2) -0.009(2) -0.016(2) O7 0.013(2) 0.021(3) 0.034(3) -0.002(2) -0.004(2) -0.010(2) O8 0.014(2) 0.028(3) 0.020(3) -0.009(2) -0.006(2) -0.001(2) O9 0.020(3) 0.017(2) 0.026(3) 0.007(2) -0.004(2) -0.001(2) O10 0.018(3) 0.019(3) 0.026(3) 0.001(2) -0.014(2) -0.005(2) O11 0.015(2) 0.030(3) 0.014(2) -0.003(2) -0.005(2) -0.010(2) O12 0.030(3) 0.030(3) 0.019(3) 0.008(2) -0.017(2) -0.015(2) N2 0.016(3) 0.017(3) 0.019(3) 0.000(2) -0.007(2) -0.004(2) N1 0.026(3) 0.025(3) 0.016(3) 0.002(3) -0.003(3) -0.004(3) C1 0.023(4) 0.044(5) 0.017(4) 0.001(4) -0.003(3) -0.007(4) C2 0.024(4) 0.028(4) 0.027(4) 0.008(3) -0.008(3) -0.003(3) C3 0.041(5) 0.019(4) 0.024(4) -0.004(3) -0.007(3) -0.011(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 O1 1.921(5) . ? Zn1 O2 1.939(5) . ? Zn1 O3 1.949(4) . ? Zn1 O4 2.052(4) . ? Zn2 O6 1.922(5) . ? Zn2 O7 1.928(5) . ? Zn2 O5 1.928(5) . ? Zn2 O8 2.012(4) . ? Zn3 O9 1.893(4) . ? Zn3 O10 1.936(4) . ? Zn3 O4 1.965(4) 1_645 ? Zn3 O11 2.030(5) . ? P1 O2 1.506(5) . ? P1 O5 1.513(5) . ? P1 O10 1.542(5) 1_465 ? P1 O11 1.585(5) 1_565 ? P2 O1 1.505(5) 2_655 ? P2 O9 1.519(5) . ? P2 O3 1.544(5) . ? P2 O4 1.569(5) 2 ? P3 O12 1.520(5) . ? P3 O6 1.520(5) . ? P3 O7 1.533(5) 2_566 ? P3 O8 1.577(5) 2_466 ? O1 P2 1.505(5) 2_655 ? O4 P2 1.569(5) 2 ? O4 Zn3 1.966(4) 1_465 ? O7 P3 1.533(5) 2_566 ? O8 P3 1.577(5) 2_466 ? O10 P1 1.542(5) 1_645 ? O11 P1 1.585(5) 1_545 ? O12 H20 0.82 . ? N2 C3 1.490(9) . ? N2 C2 1.501(9) . ? N2 H8 0.90 . ? N2 H9 0.90 . ? N1 C1 1.483(9) . ? N1 H3 0.89 . ? N1 H2 0.89 . ? N1 H1 0.89 . ? C1 C2 1.510(11) . ? C1 H5 0.97 . ? C1 H4 0.97 . ? C2 H6 0.97 . ? C2 H7 0.97 . ? C3 C3 1.49(2) 2_656 ? C3 H11 0.97 . ? C3 H10 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 O1 Zn1 O2 113.1(2) . . ? O1 Zn1 O3 117.3(2) . . ? O2 Zn1 O3 100.4(2) . . ? O1 Zn1 O4 114.0(2) . . ? O2 Zn1 O4 98.3(2) . . ? O3 Zn1 O4 111.4(2) . . ? O6 Zn2 O7 115.6(2) . . ? O6 Zn2 O5 108.1(2) . . ? O7 Zn2 O5 108.5(2) . . ? O6 Zn2 O8 108.6(2) . . ? O7 Zn2 O8 110.2(2) . . ? O5 Zn2 O8 105.4(2) . . ? O9 Zn3 O10 115.0(2) . . ? O9 Zn3 O4 116.6(2) . 1_645 ? O10 Zn3 O4 110.1(2) . 1_645 ? O9 Zn3 O11 102.5(2) . . ? O10 Zn3 O11 98.4(2) . . ? O4 Zn3 O11 112.5(2) 1_645 . ? O2 P1 O5 110.1(3) . . ? O2 P1 O10 112.9(3) . 1_465 ? O5 P1 O10 112.4(3) . 1_465 ? O2 P1 O11 108.2(3) . 1_565 ? O5 P1 O11 106.6(3) . 1_565 ? O10 P1 O11 106.2(3) 1_465 1_565 ? O1 P2 O9 111.7(3) 2_655 . ? O1 P2 O3 112.8(3) 2_655 . ? O9 P2 O3 106.6(3) . . ? O1 P2 O4 111.2(3) 2_655 2 ? O9 P2 O4 110.3(3) . 2 ? O3 P2 O4 104.0(2) . 2 ? O12 P3 O6 109.6(3) . . ? O12 P3 O7 108.0(3) . 2_566 ? O6 P3 O7 113.5(3) . 2_566 ? O12 P3 O8 110.4(3) . 2_466 ? O6 P3 O8 106.4(2) . 2_466 ? O7 P3 O8 108.9(3) 2_566 2_466 ? P2 O1 Zn1 139.8(3) 2_655 . ? P1 O2 Zn1 137.0(3) . . ? P2 O3 Zn1 132.4(3) . . ? P2 O4 Zn3 127.6(3) 2 1_465 ? P2 O4 Zn1 109.6(2) 2 . ? Zn3 O4 Zn1 116.5(2) 1_465 . ? P1 O5 Zn2 127.9(3) . . ? P3 O6 Zn2 132.2(3) . . ? P3 O7 Zn2 136.0(3) 2_566 . ? P3 O8 Zn2 120.4(2) 2_466 . ? P2 O9 Zn3 143.1(3) . . ? P1 O10 Zn3 123.4(3) 1_645 . ? P1 O11 Zn3 127.4(3) 1_545 . ? P3 O12 H20 109.5(2) . . ? C3 N2 C2 113.1(6) . . ? C3 N2 H8 109.0(4) . . ? C2 N2 H8 109.0(4) . . ? C3 N2 H9 109.0(4) . . ? C2 N2 H9 109.0(4) . . ? H8 N2 H9 107.8 . . ? C1 N1 H3 109.5(4) . . ? C1 N1 H2 109.5(4) . . ? H3 N1 H2 109.5 . . ? C1 N1 H1 109.5(4) . . ? H3 N1 H1 109.5 . . ? H2 N1 H1 109.5 . . ? N1 C1 C2 113.8(6) . . ? N1 C1 H5 108.8(4) . . ? C2 C1 H5 108.8(4) . . ? N1 C1 H4 108.8(4) . . ? C2 C1 H4 108.8(4) . . ? H5 C1 H4 107.7 . . ? N2 C2 C1 112.4(6) . . ? N2 C2 H6 109.1(4) . . ? C1 C2 H6 109.1(4) . . ? N2 C2 H7 109.1(4) . . ? C1 C2 H7 109.1(4) . . ? H6 C2 H7 107.9 . . ? N2 C3 C3 111.1(7) . 2_656 ? N2 C3 H11 109.4(4) . . ? C3 C3 H11 109.4(6) 2_656 . ? N2 C3 H10 109.4(4) . . ? C3 C3 H10 109.4(6) 2_656 . ? H11 C3 H10 108.0 . . ? _refine_diff_density_max 0.956 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.252 #===END Compound V _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H10 N2 O12 P3 Zn4' _chemical_formula_weight 620.52 _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 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 9.2187(3) _cell_length_b 15.2389(4) _cell_length_c 10.2265(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.2090(10) _cell_angle_gamma 90.00 _cell_volume 1386.33(7) _cell_formula_units_Z 4 _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 2.973 _exptl_crystal_density_method ? _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 7.254 _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 5660 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 23.22 _reflns_number_total 1972 _reflns_number_observed 1682 _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 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^)+(0.0319P)^2^+6.9206P] 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 0.0033(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1972 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_obs 0.0335 _refine_ls_wR_factor_all 0.0856 _refine_ls_wR_factor_obs 0.0827 _refine_ls_goodness_of_fit_all 1.107 _refine_ls_goodness_of_fit_obs 1.171 _refine_ls_restrained_S_all 1.107 _refine_ls_restrained_S_obs 1.171 _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 0.52452(8) 0.41309(5) 0.12273(7) 0.0132(2) Uani 1 d . . Zn2 Zn 0.45087(8) 0.24333(5) -0.07598(8) 0.0138(2) Uani 1 d . . Zn3 Zn 0.43548(8) 0.06842(5) 0.13158(7) 0.0140(2) Uani 1 d . . Zn4 Zn 0.1060(2) -0.08377(10) -0.3696(2) 0.0156(5) Uani 0.513(3) d P . Zn4A Zn 0.0742(2) -0.07968(10) -0.2271(2) 0.0139(5) Uani 0.487(3) d P . P1 P 0.2709(2) 0.41940(11) -0.1251(2) 0.0116(4) Uani 1 d . . P2 P 0.3088(2) 0.06370(11) -0.1856(2) 0.0123(4) Uani 1 d . . P3 P 0.6544(2) 0.22125(11) 0.2211(2) 0.0124(4) Uani 1 d . . O1 O 0.6664(6) 0.4915(3) 0.0731(5) 0.0254(12) Uani 1 d . . O2 O 0.6687(5) 0.3171(3) 0.1849(5) 0.0197(11) Uani 1 d . . O3 O 0.4470(5) 0.4697(3) 0.2652(4) 0.0164(10) Uani 1 d . . O4 O 0.3644(5) 0.3514(3) -0.0199(4) 0.0145(10) Uani 1 d . . O5 O 0.6053(5) 0.2910(3) -0.1482(5) 0.0219(11) Uani 1 d . . O6 O 0.3091(5) 0.1634(3) -0.1852(5) 0.0206(11) Uani 1 d . . O7 O 0.5346(5) 0.1779(3) 0.0992(4) 0.0163(11) Uani 1 d . . O8 O 0.3258(5) 0.0249(3) -0.0437(4) 0.0189(11) Uani 1 d . . O9 O 0.2936(5) 0.1012(3) 0.2341(4) 0.0194(11) Uani 1 d . . O10 O 0.1065(5) 0.4108(3) -0.1304(5) 0.0243(12) Uani 1 d . . O11 O 0.8042(5) 0.1748(3) 0.2373(5) 0.0254(12) Uani 1 d . . O12 O 0.1640(5) 0.0304(3) -0.2829(5) 0.0218(11) Uani 1 d . . N1 N 0.0782(7) -0.3581(5) -0.0592(6) 0.041(2) Uani 1 d . . C1 C -0.0195(10) -0.2775(8) -0.0890(9) 0.053(3) Uani 1 d . . C2 C 0.0476(11) -0.2019(7) 0.0067(9) 0.053(3) Uani 1 d . . N2 N -0.0012(7) -0.1165(6) -0.0625(6) 0.044(2) Uani 1 d . . C3 C 0.0306(9) -0.0413(7) 0.0375(8) 0.044(2) Uani 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 0.0166(4) 0.0106(5) 0.0121(4) -0.0020(3) 0.0033(3) -0.0008(3) Zn2 0.0174(4) 0.0108(4) 0.0125(4) -0.0013(3) 0.0029(3) -0.0003(3) Zn3 0.0169(4) 0.0138(4) 0.0114(4) 0.0030(3) 0.0039(3) 0.0011(3) Zn4 0.0159(9) 0.0151(9) 0.0147(9) 0.0001(7) 0.0018(7) 0.0007(6) Zn4A 0.0147(9) 0.0132(9) 0.0132(9) -0.0011(7) 0.0027(7) -0.0002(7) P1 0.0120(9) 0.0117(9) 0.0112(9) 0.0020(7) 0.0035(7) 0.0008(7) P2 0.0132(9) 0.0108(9) 0.0121(9) -0.0015(7) 0.0020(7) -0.0011(7) P3 0.0133(9) 0.0120(10) 0.0116(9) 0.0017(7) 0.0025(7) 0.0008(7) O1 0.038(3) 0.013(3) 0.031(3) -0.004(2) 0.021(3) -0.008(2) O2 0.020(3) 0.012(3) 0.025(3) 0.003(2) 0.002(2) 0.001(2) O3 0.020(3) 0.014(3) 0.016(2) -0.005(2) 0.007(2) -0.003(2) O4 0.020(3) 0.012(2) 0.010(2) -0.002(2) 0.000(2) 0.003(2) O5 0.023(3) 0.029(3) 0.015(3) -0.004(2) 0.007(2) -0.002(2) O6 0.024(3) 0.010(3) 0.022(3) -0.001(2) -0.004(2) 0.000(2) O7 0.021(3) 0.015(3) 0.012(2) -0.002(2) 0.003(2) -0.004(2) O8 0.026(3) 0.020(3) 0.011(2) 0.001(2) 0.006(2) -0.007(2) O9 0.020(3) 0.028(3) 0.009(2) 0.001(2) 0.004(2) 0.006(2) O10 0.012(2) 0.037(3) 0.024(3) 0.008(2) 0.005(2) 0.002(2) O11 0.020(3) 0.027(3) 0.032(3) 0.010(2) 0.011(2) 0.010(2) O12 0.018(3) 0.017(3) 0.027(3) -0.005(2) 0.000(2) -0.002(2) N1 0.026(4) 0.076(6) 0.018(4) -0.003(4) 0.003(3) -0.006(4) C1 0.034(5) 0.089(8) 0.028(5) 0.017(5) -0.004(4) -0.016(5) C2 0.062(7) 0.076(8) 0.016(4) 0.007(5) -0.001(4) 0.026(6) N2 0.024(4) 0.093(6) 0.015(4) 0.015(4) 0.004(3) 0.009(4) C3 0.028(5) 0.078(7) 0.025(5) 0.024(5) 0.007(4) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.935(5) . ? Zn1 O2 1.967(5) . ? Zn1 O3 1.981(4) . ? Zn1 O4 2.015(4) . ? Zn2 O5 1.911(5) . ? Zn2 O6 1.916(5) . ? Zn2 O4 1.979(4) . ? Zn2 O7 2.019(4) . ? Zn3 O8 1.930(5) . ? Zn3 O9 1.944(4) . ? Zn3 O7 1.971(4) . ? Zn3 O3 1.988(4) 2_645 ? Zn4 Zn4A 1.562(2) . ? Zn4 O10 1.961(5) 2_544 ? Zn4 O12 1.962(5) . ? Zn4 O11 1.963(5) 3_655 ? Zn4 N1 2.085(7) 4 ? Zn4A O11 1.853(5) 3_655 ? Zn4A O10 1.909(5) 2_544 ? Zn4A O12 2.019(5) . ? Zn4A N2 2.060(7) . ? P1 O10 1.508(5) . ? P1 O1 1.517(5) 3_665 ? P1 O9 1.541(5) 4_565 ? P1 O4 1.577(5) . ? P2 O6 1.520(5) . ? P2 O12 1.527(5) . ? P2 O8 1.537(5) . ? P2 O3 1.573(5) 4_565 ? P3 O2 1.520(5) . ? P3 O11 1.521(5) . ? P3 O5 1.531(5) 4_566 ? P3 O7 1.577(5) . ? O1 P1 1.517(5) 3_665 ? O3 P2 1.573(5) 4_566 ? O3 Zn3 1.988(4) 2_655 ? O5 P3 1.531(5) 4_565 ? O9 P1 1.541(5) 4_566 ? O10 Zn4A 1.909(5) 2_554 ? O10 Zn4 1.961(5) 2_554 ? O11 Zn4A 1.852(5) 3_655 ? O11 Zn4 1.963(5) 3_655 ? N1 C1 1.506(13) . ? N1 Zn4 2.085(7) 4_556 ? C1 C2 1.534(14) . ? C2 N2 1.493(12) . ? N2 C3 1.512(13) . ? C3 C3 1.51(2) 3 ? 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 95.6(2) . . ? O1 Zn1 O3 108.8(2) . . ? O2 Zn1 O3 115.5(2) . . ? O1 Zn1 O4 121.0(2) . . ? O2 Zn1 O4 101.0(2) . . ? O3 Zn1 O4 113.5(2) . . ? O5 Zn2 O6 118.7(2) . . ? O5 Zn2 O4 101.1(2) . . ? O6 Zn2 O4 115.6(2) . . ? O5 Zn2 O7 112.4(2) . . ? O6 Zn2 O7 104.3(2) . . ? O4 Zn2 O7 104.1(2) . . ? O8 Zn3 O9 109.1(2) . . ? O8 Zn3 O7 106.7(2) . . ? O9 Zn3 O7 106.2(2) . . ? O8 Zn3 O3 108.2(2) . 2_645 ? O9 Zn3 O3 105.0(2) . 2_645 ? O7 Zn3 O3 121.2(2) . 2_645 ? Zn4A Zn4 O10 64.5(2) . 2_544 ? Zn4A Zn4 O12 68.8(2) . . ? O10 Zn4 O12 101.0(2) 2_544 . ? Zn4A Zn4 O11 62.2(2) . 3_655 ? O10 Zn4 O11 102.2(2) 2_544 3_655 ? O12 Zn4 O11 107.5(2) . 3_655 ? Zn4A Zn4 N1 151.3(2) . 4 ? O10 Zn4 N1 95.9(2) 2_544 4 ? O12 Zn4 N1 138.5(3) . 4 ? O11 Zn4 N1 105.5(3) 3_655 4 ? Zn4 Zn4A O11 69.6(2) . 3_655 ? Zn4 Zn4A O10 68.0(2) . 2_544 ? O11 Zn4A O10 108.5(2) 3_655 2_544 ? Zn4 Zn4A O12 65.0(2) . . ? O11 Zn4A O12 109.6(2) 3_655 . ? O10 Zn4A O12 100.8(2) 2_544 . ? Zn4 Zn4A N2 159.7(3) . . ? O11 Zn4A N2 99.9(3) 3_655 . ? O10 Zn4A N2 100.9(2) 2_544 . ? O12 Zn4A N2 135.1(3) . . ? O10 P1 O1 112.2(3) . 3_665 ? O10 P1 O9 109.3(3) . 4_565 ? O1 P1 O9 112.2(3) 3_665 4_565 ? O10 P1 O4 109.4(3) . . ? O1 P1 O4 105.0(3) 3_665 . ? O9 P1 O4 108.6(3) 4_565 . ? O6 P2 O12 109.5(3) . . ? O6 P2 O8 112.5(3) . . ? O12 P2 O8 110.0(3) . . ? O6 P2 O3 108.9(3) . 4_565 ? O12 P2 O3 109.1(3) . 4_565 ? O8 P2 O3 106.7(3) . 4_565 ? O2 P3 O11 109.8(3) . . ? O2 P3 O5 113.2(3) . 4_566 ? O11 P3 O5 108.4(3) . 4_566 ? O2 P3 O7 107.3(3) . . ? O11 P3 O7 108.6(3) . . ? O5 P3 O7 109.4(3) 4_566 . ? P1 O1 Zn1 133.0(3) 3_665 . ? P3 O2 Zn1 134.3(3) . . ? P2 O3 Zn1 125.0(3) 4_566 . ? P2 O3 Zn3 116.7(2) 4_566 2_655 ? Zn1 O3 Zn3 118.0(2) . 2_655 ? P1 O4 Zn2 122.6(2) . . ? P1 O4 Zn1 110.7(2) . . ? Zn2 O4 Zn1 108.9(2) . . ? P3 O5 Zn2 135.4(3) 4_565 . ? P2 O6 Zn2 129.6(3) . . ? P3 O7 Zn3 118.8(3) . . ? P3 O7 Zn2 121.3(3) . . ? Zn3 O7 Zn2 118.8(2) . . ? P2 O8 Zn3 130.1(3) . . ? P1 O9 Zn3 136.7(3) 4_566 . ? P1 O10 Zn4A 133.5(3) . 2_554 ? P1 O10 Zn4 172.3(3) . 2_554 ? Zn4A O10 Zn4 47.58(13) 2_554 2_554 ? P3 O11 Zn4A 154.6(4) . 3_655 ? P3 O11 Zn4 127.6(3) . 3_655 ? Zn4A O11 Zn4 48.23(13) 3_655 3_655 ? P2 O12 Zn4 132.6(3) . . ? P2 O12 Zn4A 116.4(3) . . ? Zn4 O12 Zn4A 46.17(12) . . ? C1 N1 Zn4 117.1(5) . 4_556 ? N1 C1 C2 111.3(7) . . ? N2 C2 C1 109.4(7) . . ? C2 N2 C3 111.0(6) . . ? C2 N2 Zn4A 120.0(6) . . ? C3 N2 Zn4A 107.4(5) . . ? C3 C3 N2 108.1(9) 3 . ? _refine_diff_density_max 0.777 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.137 #===END