# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/241 data_sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C2 H10 N O6 P1.50 Zn' _chemical_formula_weight 255.93 _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 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 17.3514(6) _cell_length_b 9.5075(3) _cell_length_c 9.8065(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.682(2) _cell_angle_gamma 90.00 _cell_volume 1578.29(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.154 _exptl_crystal_density_method ? _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 3.406 _exptl_absorpt_correction_type emperical(SADABS) _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 3170 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 23.23 _reflns_number_total 1124 _reflns_number_observed 977 _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^)+(0.0390P)^2^+0.1707P] 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 0.0018(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1124 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_obs 0.0266 _refine_ls_wR_factor_all 0.0737 _refine_ls_wR_factor_obs 0.0706 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.087 _refine_ls_restrained_S_all 1.051 _refine_ls_restrained_S_obs 1.087 _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 0.17892(2) 0.07950(4) 0.37523(4) 0.0165(2) Uani 1 d . . P1 P 0.18957(6) 0.17787(10) 0.68124(10) 0.0171(3) Uani 1 d . . P2 P 0.0000 0.04456(15) 0.2500 0.0176(4) Uani 1 d S . O1 O 0.2506(2) 0.2087(3) 0.3193(3) 0.0321(8) Uani 1 d . . O2 O 0.1869(2) 0.0619(3) 0.5735(3) 0.0250(7) Uani 1 d . . O3 O 0.2030(2) -0.1142(3) 0.3282(3) 0.0235(7) Uani 1 d . . O4 O 0.07412(15) 0.1351(3) 0.2653(3) 0.0225(6) Uani 1 d . . O5 O 0.1064(2) 0.2549(3) 0.6501(3) 0.0306(7) Uani 1 d . . H20 H 0.0713(2) 0.1969(3) 0.6492(3) 0.046 Uiso 1 calc R . O6 O -0.0089(2) -0.0543(3) 0.1204(3) 0.0224(7) Uani 1 d . . H10 H 0.0307(2) -0.1032(3) 0.1283(3) 0.034 Uiso 1 calc R . N1 N 0.1363(2) 0.2669(4) 1.0383(4) 0.0327(9) Uani 1 d . . H1 H 0.1196(2) 0.2160(4) 1.1022(4) 0.049 Uiso 1 calc R . H2 H 0.1868(2) 0.2898(4) 1.0702(4) 0.049 Uiso 1 calc R . H3 H 0.1315(2) 0.2169(4) 0.9601(4) 0.049 Uiso 1 calc R . C1 C 0.0887(3) 0.3953(5) 1.0089(7) 0.059(2) Uani 1 d . . H4 H 0.0338(3) 0.3685(5) 0.9771(7) 0.071 Uiso 1 calc R . H5 H 0.0933(3) 0.4470(5) 1.0956(7) 0.071 Uiso 1 calc R . C2 C 0.1097(3) 0.4885(5) 0.9059(5) 0.0480(14) Uani 1 d . . H6 H 0.0756(3) 0.5692(5) 0.8936(5) 0.072 Uiso 1 calc R . H7 H 0.1039(3) 0.4397(5) 0.8185(5) 0.072 Uiso 1 calc R . H8 H 0.1636(3) 0.5184(5) 0.9373(5) 0.072 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 0.0141(3) 0.0193(3) 0.0162(3) -0.0003(2) 0.0036(2) -0.0028(2) P1 0.0160(6) 0.0208(6) 0.0152(6) 0.0006(4) 0.0047(4) -0.0046(4) P2 0.0090(7) 0.0210(7) 0.0224(9) 0.000 0.0024(6) 0.000 O1 0.030(2) 0.035(2) 0.032(2) 0.0027(14) 0.0074(14) -0.0165(14) O2 0.031(2) 0.0276(15) 0.018(2) -0.0016(12) 0.0080(13) -0.0024(12) O3 0.034(2) 0.0222(14) 0.015(2) -0.0003(12) 0.0063(13) 0.0053(13) O4 0.0122(15) 0.0269(14) 0.027(2) 0.0041(13) 0.0022(12) -0.0022(12) O5 0.021(2) 0.025(2) 0.043(2) 0.0003(13) 0.0014(14) 0.0002(13) O6 0.018(2) 0.0289(15) 0.020(2) -0.0039(12) 0.0025(12) 0.0049(12) N1 0.029(2) 0.042(2) 0.025(2) 0.001(2) 0.001(2) -0.001(2) C1 0.046(4) 0.047(3) 0.093(5) 0.010(3) 0.036(3) 0.009(3) C2 0.062(4) 0.040(3) 0.042(3) -0.002(2) 0.011(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 1.912(3) . ? Zn1 O2 1.926(3) . ? Zn1 O3 1.966(3) . ? Zn1 O4 1.972(3) . ? P1 O1 1.498(3) 7_556 ? P1 O2 1.521(3) . ? P1 O3 1.533(3) 6_556 ? P1 O5 1.586(3) . ? P2 O4 1.527(3) 2 ? P2 O4 1.528(3) . ? P2 O6 1.561(3) . ? P2 O6 1.561(3) 2 ? O1 P1 1.498(3) 7_556 ? O3 P1 1.533(3) 6 ? O5 H20 0.82 . ? O6 H10 0.82 . ? N1 C1 1.467(6) . ? N1 H1 0.89 . ? N1 H2 0.89 . ? N1 H3 0.89 . ? C1 C2 1.450(7) . ? C1 H4 0.97 . ? C1 H5 0.97 . ? C2 H6 0.96 . ? C2 H7 0.96 . ? C2 H8 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 115.99(12) . . ? O1 Zn1 O3 110.43(12) . . ? O2 Zn1 O3 100.60(11) . . ? O1 Zn1 O4 104.53(12) . . ? O2 Zn1 O4 115.36(12) . . ? O3 Zn1 O4 109.95(12) . . ? O1 P1 O2 115.8(2) 7_556 . ? O1 P1 O3 109.0(2) 7_556 6_556 ? O2 P1 O3 110.0(2) . 6_556 ? O1 P1 O5 105.6(2) 7_556 . ? O2 P1 O5 108.2(2) . . ? O3 P1 O5 107.9(2) 6_556 . ? O4 P2 O4 111.4(2) 2 . ? O4 P2 O6 109.17(14) 2 . ? O4 P2 O6 110.54(13) . . ? O4 P2 O6 110.54(13) 2 2 ? O4 P2 O6 109.17(14) . 2 ? O6 P2 O6 105.9(2) . 2 ? P1 O1 Zn1 163.5(2) 7_556 . ? P1 O2 Zn1 128.6(2) . . ? P1 O3 Zn1 126.5(2) 6 . ? P2 O4 Zn1 123.9(2) . . ? P1 O5 H20 109.47(10) . . ? P2 O6 H10 109.47(10) . . ? C1 N1 H1 109.5(2) . . ? 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 . . ? C2 C1 N1 115.4(4) . . ? C2 C1 H4 108.4(3) . . ? N1 C1 H4 108.4(3) . . ? C2 C1 H5 108.4(3) . . ? N1 C1 H5 108.4(3) . . ? H4 C1 H5 107.5 . . ? C1 C2 H6 109.5(3) . . ? C1 C2 H7 109.5(3) . . ? H6 C2 H7 109.5 . . ? C1 C2 H8 109.5(3) . . ? H6 C2 H8 109.5 . . ? H7 C2 H8 109.5 . . ? _refine_diff_density_max 0.554 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.171