# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2293 data_sad1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C1.50 H6 N O10 P2 Zn3' _chemical_formula_weight 456.12 _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 5.00300(10) _cell_length_b 8.5434(3) _cell_length_c 12.4336(5) _cell_angle_alpha 92.99 _cell_angle_beta 97.138(2) _cell_angle_gamma 91.465(2) _cell_volume 526.33(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 23.25 _exptl_crystal_description rectangular plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.878 _exptl_crystal_density_method ? _exptl_crystal_F_000 444 _exptl_absorpt_coefficient_mu 7.131 _exptl_absorpt_correction_type empirical(SADABS) _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 smart-CCD diffractometer _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2197 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 23.25 _reflns_number_total 1476 _reflns_number_observed 1185 _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 ? _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^)+(0.0919P)^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 1476 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_obs 0.0534 _refine_ls_wR_factor_all 0.1417 _refine_ls_wR_factor_obs 0.1288 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.071 _refine_ls_restrained_S_all 1.040 _refine_ls_restrained_S_obs 1.071 _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 C1 C 0.4234(54) 0.5907(35) 0.4191(19) 0.038(7) Uani 0.50 d P . C1A C 0.6232(52) 0.5298(29) 0.4136(18) 0.028(6) Uani 0.50 d P . C2 C 0.5000 0.5000 0.5000 0.084(10) Uani 1 d S . C10 C 0.0405(22) 1.0850(14) -0.4827(8) 0.022(3) Uani 1 d . . Zn1 Zn 0.3937(2) 0.86326(13) 0.05955(9) 0.0133(4) Uani 1 d . . Zn2 Zn -0.1138(2) 0.63724(13) -0.13950(9) 0.0132(4) Uani 1 d . . Zn3 Zn -0.1447(2) 0.96820(13) -0.29767(9) 0.0136(4) Uani 1 d . . P1 P 0.3822(5) 0.8239(3) -0.2003(2) 0.0128(6) Uani 1 d . . P2 P -0.0418(5) 0.7121(3) 0.1231(2) 0.0112(6) Uani 1 d . . O1 O 0.6609(14) 0.7250(8) 0.1233(6) 0.019(2) Uani 1 d . . O2 O 0.4549(14) 0.9144(8) -0.0903(5) 0.018(2) Uani 1 d . . O3 O 0.1187(14) 0.8633(8) 0.1713(5) 0.015(2) Uani 1 d . . O4 O 0.0452(14) 0.6949(8) 0.0070(5) 0.016(2) Uani 1 d . . O5 O -0.0519(14) 0.4262(8) -0.1901(5) 0.016(2) Uani 1 d . . O6 O -0.4901(14) 0.6636(8) -0.1918(6) 0.017(2) Uani 1 d . . O7 O 0.0716(13) 0.7987(8) -0.2215(5) 0.013(2) Uani 1 d . . O8 O -0.5276(14) 0.9198(8) -0.2897(5) 0.017(2) Uani 1 d . . O9 O -0.0101(17) 1.1368(8) -0.3901(6) 0.026(2) Uani 1 d . . O10 O -0.1430(17) 0.8365(8) -0.4507(6) 0.028(2) Uani 1 d . . N1 N 0.5574(25) 0.6287(13) 0.3297(8) 0.045(3) 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 C1 0.028(16) 0.070(20) 0.016(15) -0.012(14) 0.001(11) 0.009(14) C1A 0.031(16) 0.041(15) 0.016(14) 0.004(12) 0.011(11) 0.002(12) C2 0.145(27) 0.080(18) 0.019(12) 0.039(12) -0.027(14) -0.065(17) C10 0.021(6) 0.040(7) 0.006(6) 0.009(5) -0.005(5) 0.005(5) Zn1 0.0143(7) 0.0147(7) 0.0113(7) 0.0029(5) 0.0017(5) 0.0024(5) Zn2 0.0140(7) 0.0129(7) 0.0120(7) -0.0001(5) -0.0009(5) 0.0035(5) Zn3 0.0152(7) 0.0151(7) 0.0107(7) 0.0008(5) 0.0017(5) 0.0027(5) P1 0.0118(15) 0.0159(14) 0.0102(14) -0.0001(11) -0.0009(11) 0.0039(11) P2 0.0143(14) 0.0121(14) 0.0070(14) 0.0011(11) 0.0000(11) 0.0038(11) O1 0.017(4) 0.026(4) 0.017(4) 0.011(3) 0.002(3) 0.006(3) O2 0.026(4) 0.021(4) 0.006(4) -0.002(3) 0.000(3) 0.003(3) O3 0.019(4) 0.023(4) 0.004(4) -0.001(3) 0.001(3) 0.004(3) O4 0.015(4) 0.022(4) 0.012(4) -0.002(3) 0.002(3) -0.003(3) O5 0.026(4) 0.012(4) 0.009(4) 0.000(3) -0.001(3) 0.006(3) O6 0.011(4) 0.013(4) 0.026(4) -0.004(3) 0.000(3) 0.004(3) O7 0.008(4) 0.016(4) 0.015(4) 0.006(3) 0.000(3) 0.005(3) O8 0.016(4) 0.029(4) 0.006(4) 0.001(3) 0.001(3) -0.002(3) O9 0.051(6) 0.017(4) 0.010(4) 0.002(3) 0.007(4) 0.004(4) O10 0.054(6) 0.015(4) 0.017(4) -0.005(3) 0.016(4) -0.007(4) N1 0.069(9) 0.050(7) 0.016(6) 0.012(5) 0.001(6) -0.030(6) _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 C1 C1A 1.15(3) . ? C1 C2 1.33(3) . ? C1 N1 1.41(3) . ? C1A C2 1.33(2) . ? C1A N1 1.39(3) . ? C2 C1 1.33(3) 2_666 ? C2 C1A 1.33(2) 2_666 ? C10 O10 1.243(14) 2_574 ? C10 O9 1.269(13) . ? C10 C10 1.52(2) 2_574 ? Zn1 O1 1.930(7) . ? Zn1 O2 1.994(7) . ? Zn1 O2 2.027(7) 2_675 ? Zn1 O3 2.073(7) . ? Zn1 O4 2.242(7) . ? Zn1 P2 2.726(3) . ? Zn1 Zn1 3.067(2) 2_675 ? Zn2 O5 1.924(6) . ? Zn2 O4 1.928(7) . ? Zn2 O6 1.937(7) . ? Zn2 O7 2.030(7) . ? Zn3 O8 1.965(7) . ? Zn3 O7 2.033(6) . ? Zn3 O9 2.040(7) . ? Zn3 O3 2.064(6) 2_575 ? Zn3 O10 2.160(7) . ? P1 O8 1.520(8) 1_655 ? P1 O6 1.529(7) 1_655 ? P1 O2 1.534(7) . ? P1 O7 1.551(7) . ? P2 O1 1.495(8) 1_455 ? P2 O5 1.531(7) 2_565 ? P2 O3 1.556(7) . ? P2 O4 1.559(7) . ? O1 P2 1.495(8) 1_655 ? O2 Zn1 2.027(7) 2_675 ? O3 Zn3 2.064(6) 2_575 ? O5 P2 1.531(7) 2_565 ? O6 P1 1.529(7) 1_455 ? O8 P1 1.520(8) 1_455 ? O10 C10 1.243(14) 2_574 ? 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 C1A C1 C2 64.8(18) . . ? C1A C1 N1 64.8(19) . . ? C2 C1 N1 129.6(21) . . ? C1 C1A C2 64.1(18) . . ? C1 C1A N1 67.0(20) . . ? C2 C1A N1 131.1(20) . . ? C1 C2 C1 179.999(12) . 2_666 ? C1 C2 C1A 129.0(15) . 2_666 ? C1 C2 C1A 51.0(15) 2_666 2_666 ? C1 C2 C1A 51.0(15) . . ? C1 C2 C1A 129.0(15) 2_666 . ? C1A C2 C1A 179.998(9) 2_666 . ? O10 C10 O9 125.2(11) 2_574 . ? O10 C10 C10 117.0(12) 2_574 2_574 ? O9 C10 C10 117.7(13) . 2_574 ? O1 Zn1 O2 112.0(3) . . ? O1 Zn1 O2 107.3(3) . 2_675 ? O2 Zn1 O2 80.6(3) . 2_675 ? O1 Zn1 O3 101.4(3) . . ? O2 Zn1 O3 145.3(3) . . ? O2 Zn1 O3 98.9(3) 2_675 . ? O1 Zn1 O4 101.4(3) . . ? O2 Zn1 O4 95.3(3) . . ? O2 Zn1 O4 150.4(3) 2_675 . ? O3 Zn1 O4 68.1(3) . . ? O1 Zn1 P2 96.5(2) . . ? O2 Zn1 P2 128.0(2) . . ? O2 Zn1 P2 132.0(2) 2_675 . ? O3 Zn1 P2 34.6(2) . . ? O4 Zn1 P2 34.9(2) . . ? O1 Zn1 Zn1 116.1(2) . 2_675 ? O2 Zn1 Zn1 40.7(2) . 2_675 ? O2 Zn1 Zn1 39.9(2) 2_675 2_675 ? O3 Zn1 Zn1 129.5(2) . 2_675 ? O4 Zn1 Zn1 129.5(2) . 2_675 ? P2 Zn1 Zn1 147.37(8) . 2_675 ? O5 Zn2 O4 115.1(3) . . ? O5 Zn2 O6 103.1(3) . . ? O4 Zn2 O6 123.6(3) . . ? O5 Zn2 O7 112.1(3) . . ? O4 Zn2 O7 100.2(3) . . ? O6 Zn2 O7 102.0(3) . . ? O8 Zn3 O7 107.5(3) . . ? O8 Zn3 O9 123.9(3) . . ? O7 Zn3 O9 127.8(3) . . ? O8 Zn3 O3 93.1(3) . 2_575 ? O7 Zn3 O3 99.2(3) . 2_575 ? O9 Zn3 O3 87.5(3) . 2_575 ? O8 Zn3 O10 93.8(3) . . ? O7 Zn3 O10 89.6(3) . . ? O9 Zn3 O10 79.2(3) . . ? O3 Zn3 O10 166.7(3) 2_575 . ? O8 P1 O6 114.2(4) 1_655 1_655 ? O8 P1 O2 109.5(4) 1_655 . ? O6 P1 O2 107.4(4) 1_655 . ? O8 P1 O7 108.6(4) 1_655 . ? O6 P1 O7 108.5(4) 1_655 . ? O2 P1 O7 108.6(4) . . ? O1 P2 O5 108.4(4) 1_455 2_565 ? O1 P2 O3 112.7(4) 1_455 . ? O5 P2 O3 109.1(4) 2_565 . ? O1 P2 O4 113.6(4) 1_455 . ? O5 P2 O4 111.0(4) 2_565 . ? O3 P2 O4 102.0(4) . . ? O1 P2 Zn1 141.8(3) 1_455 . ? O5 P2 Zn1 109.5(3) 2_565 . ? O3 P2 Zn1 49.1(3) . . ? O4 P2 Zn1 55.3(3) . . ? P2 O1 Zn1 134.6(5) 1_655 . ? P1 O2 Zn1 131.7(5) . . ? P1 O2 Zn1 128.5(4) . 2_675 ? Zn1 O2 Zn1 99.4(3) . 2_675 ? P2 O3 Zn3 142.7(4) . 2_575 ? P2 O3 Zn1 96.3(3) . . ? Zn3 O3 Zn1 120.9(3) 2_575 . ? P2 O4 Zn2 138.8(4) . . ? P2 O4 Zn1 89.8(3) . . ? Zn2 O4 Zn1 127.3(3) . . ? P2 O5 Zn2 128.3(4) 2_565 . ? P1 O6 Zn2 123.2(4) 1_455 . ? P1 O7 Zn2 119.9(4) . . ? P1 O7 Zn3 117.6(4) . . ? Zn2 O7 Zn3 120.3(3) . . ? P1 O8 Zn3 121.7(4) 1_455 . ? C10 O9 Zn3 113.9(7) . . ? C10 O10 Zn3 111.5(7) 2_574 . ? C1A N1 C1 48.2(14) . . ? _refine_diff_density_max 1.187 _refine_diff_density_min -1.197 _refine_diff_density_rms 0.262