# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 182/1316 data_Ga5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Ga5(OH)2(C10H9N2)(C2O4)(PO4)4].2H2O _chemical_formula_sum 'C12 H15 Ga5 N2 O24 P4' _chemical_formula_weight 1043.74 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 1 _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 18.3430(2) _cell_length_b 15.9372(4) _cell_length_c 9.1019(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.8670(10) _cell_angle_gamma 90.00 _cell_volume 2660.51(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3782 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.135 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.009 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 5.353 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens Smart CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7595 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.95 _reflns_number_total 2902 _reflns_number_gt 2187 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ATOMS _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+12.5437P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00099(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2902 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.17104(3) 0.12924(3) 0.62122(6) 0.01103(16) Uani 1 1 d . . . Ga2 Ga 0.26569(3) -0.11707(3) 0.57565(6) 0.01127(16) Uani 1 1 d . . . Ga3 Ga 0.0000 0.19459(5) 0.7500 0.0157(2) Uani 1 2 d S . . P1 P 0.22301(8) 0.02086(8) 0.34708(15) 0.0112(3) Uani 1 1 d . . . P2 P 0.14607(7) -0.22161(8) 0.42752(15) 0.0115(3) Uani 1 1 d . . . O1 O 0.2752(2) -0.0325(2) 0.4432(4) 0.0164(8) Uani 1 1 d . . . O2 O 0.1670(2) 0.0662(2) 0.4401(4) 0.0170(8) Uani 1 1 d . . . O3 O 0.2727(2) 0.0833(2) 0.2667(4) 0.0159(8) Uani 1 1 d . . . O4 O 0.1821(2) -0.0302(2) 0.2330(4) 0.0179(8) Uani 1 1 d . . . O5 O 0.1783(2) -0.1706(2) 0.5571(4) 0.0176(8) Uani 1 1 d . . . O6 O 0.1565(2) -0.3156(2) 0.4629(4) 0.0168(8) Uani 1 1 d . . . O7 O 0.0654(2) -0.2017(2) 0.4194(4) 0.0171(8) Uani 1 1 d . . . O8 O 0.1861(2) -0.2023(2) 0.2874(4) 0.0191(9) Uani 1 1 d . . . O9 O 0.1564(2) 0.2370(2) 0.4999(4) 0.0159(8) Uani 1 1 d . . . O10 O 0.22269(19) 0.3438(2) 0.4154(4) 0.0150(8) Uani 1 1 d . . . O11 O 0.0655(2) 0.1320(3) 0.6393(4) 0.0183(9) Uani 1 1 d . . . N1 N 0.0000 0.3216(4) 0.7500 0.0228(16) Uani 1 2 d S . . N2 N 0.0000 0.7612(5) 0.7500 0.0335(19) Uani 1 2 d S . . C1 C 0.0484(4) 0.3648(4) 0.6713(8) 0.0316(16) Uani 1 1 d . . . C2 C 0.0508(4) 0.4506(4) 0.6698(8) 0.0295(15) Uani 1 1 d . . . C3 C 0.0000 0.4962(5) 0.7500 0.0216(19) Uani 1 2 d S . . C4 C 0.0000 0.5876(5) 0.7500 0.0232(19) Uani 1 2 d S . . C5 C 0.0648(4) 0.6330(4) 0.7428(7) 0.0280(15) Uani 1 1 d . . . C6 C 0.0634(4) 0.7191(4) 0.7433(7) 0.0335(17) Uani 1 1 d . . . C7 C 0.2147(3) 0.2732(3) 0.4752(6) 0.0137(11) Uani 1 1 d . . . OW1 O 0.0287(8) 0.0714(8) 0.277(3) 0.138(9) Uani 0.50 1 d P . . OW2 O -0.0266(8) 0.0079(13) 0.521(3) 0.140(9) Uani 0.50 1 d P . . HC1 H 0.077(4) 0.339(5) 0.632(9) 0.050 Uiso 1 1 d . . . HC2 H 0.086(4) 0.485(4) 0.617(8) 0.050 Uiso 1 1 d . . . HC5 H 0.107(4) 0.608(5) 0.745(8) 0.050 Uiso 1 1 d . . . HC6 H 0.107(4) 0.751(5) 0.736(8) 0.050 Uiso 1 1 d . . . HO11 H 0.050(4) 0.112(5) 0.571(9) 0.050 Uiso 1 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 Ga1 0.0131(3) 0.0103(3) 0.0097(3) 0.0001(2) 0.0020(2) 0.0011(2) Ga2 0.0151(3) 0.0091(3) 0.0096(3) 0.0004(2) 0.0004(2) 0.0012(2) Ga3 0.0137(5) 0.0161(4) 0.0173(5) 0.000 0.0002(4) 0.000 P1 0.0156(7) 0.0099(6) 0.0082(6) 0.0005(5) 0.0022(5) -0.0001(5) P2 0.0127(7) 0.0099(6) 0.0120(7) 0.0006(5) 0.0005(5) 0.0011(5) O1 0.017(2) 0.0135(19) 0.019(2) 0.0051(16) -0.0015(16) 0.0049(15) O2 0.017(2) 0.020(2) 0.014(2) -0.0013(16) 0.0027(16) 0.0021(16) O3 0.021(2) 0.0152(19) 0.0120(19) 0.0052(16) 0.0006(16) -0.0035(16) O4 0.025(2) 0.0153(19) 0.013(2) -0.0064(16) -0.0005(16) -0.0022(16) O5 0.017(2) 0.021(2) 0.016(2) -0.0053(16) -0.0003(16) -0.0043(16) O6 0.018(2) 0.0104(18) 0.022(2) 0.0048(16) 0.0031(17) 0.0029(15) O7 0.0120(19) 0.024(2) 0.016(2) -0.0021(16) -0.0006(16) 0.0056(16) O8 0.022(2) 0.019(2) 0.017(2) 0.0067(16) 0.0060(17) 0.0042(16) O9 0.0134(19) 0.0111(18) 0.023(2) 0.0062(16) 0.0051(16) 0.0000(15) O10 0.014(2) 0.0137(19) 0.017(2) 0.0000(16) 0.0001(16) -0.0010(15) O11 0.013(2) 0.025(2) 0.017(2) -0.0026(17) 0.0007(17) 0.0017(16) N1 0.021(4) 0.019(4) 0.028(4) 0.000 -0.002(3) 0.000 N2 0.056(6) 0.027(4) 0.017(4) 0.000 0.004(4) 0.000 C1 0.026(4) 0.031(4) 0.038(4) -0.005(3) 0.011(3) 0.010(3) C2 0.029(4) 0.024(3) 0.036(4) 0.006(3) 0.008(3) 0.000(3) C3 0.022(5) 0.015(4) 0.028(5) 0.000 0.003(4) 0.000 C4 0.022(5) 0.029(5) 0.018(4) 0.000 0.004(4) 0.000 C5 0.026(4) 0.031(4) 0.027(4) -0.003(3) 0.001(3) -0.001(3) C6 0.053(5) 0.031(4) 0.016(3) 0.003(3) 0.000(3) -0.017(3) C7 0.019(3) 0.012(3) 0.010(3) -0.002(2) 0.003(2) 0.003(2) OW1 0.088(13) 0.039(7) 0.29(3) 0.005(12) -0.096(15) 0.011(7) OW2 0.063(13) 0.125(14) 0.23(2) -0.107(15) 0.004(16) -0.015(13) _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 Ga1 O4 1.887(4) 6_556 ? Ga1 O8 1.926(4) 6_556 ? Ga1 O2 1.931(4) . ? Ga1 O11 1.945(4) . ? Ga1 O10 2.028(4) 7_556 ? Ga1 O9 2.057(4) . ? Ga2 O1 1.818(4) . ? Ga2 O5 1.821(4) . ? Ga2 O3 1.823(4) 6_556 ? Ga2 O6 1.824(4) 7_546 ? Ga3 O11 1.869(4) 2_556 ? Ga3 O11 1.869(4) . ? Ga3 O7 1.943(4) 5_556 ? Ga3 O7 1.943(4) 6_556 ? Ga3 N1 2.024(7) . ? P1 O4 1.510(4) . ? P1 O2 1.524(4) . ? P1 O3 1.542(4) . ? P1 O1 1.543(4) . ? P2 O8 1.512(4) . ? P2 O7 1.514(4) . ? P2 O5 1.543(4) . ? P2 O6 1.543(4) . ? O3 Ga2 1.823(4) 6 ? O4 Ga1 1.887(4) 6 ? O6 Ga2 1.824(4) 7_546 ? O7 Ga3 1.943(4) 5_556 ? O8 Ga1 1.926(4) 6 ? O9 C7 1.239(6) . ? O10 C7 1.260(6) . ? O10 Ga1 2.028(4) 7_556 ? N1 C1 1.339(7) 2_556 ? N1 C1 1.339(8) . ? N2 C6 1.345(8) 2_556 ? N2 C6 1.345(8) . ? C1 C2 1.368(9) . ? C2 C3 1.396(7) . ? C3 C2 1.396(7) 2_556 ? C3 C4 1.457(11) . ? C4 C5 1.394(8) . ? C4 C5 1.394(8) 2_556 ? C5 C6 1.373(9) . ? C7 C7 1.551(10) 7_556 ? OW1 OW1 1.15(2) 2 ? OW2 OW2 1.08(3) 5_556 ? 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 Ga1 O8 94.00(17) 6_556 6_556 ? O4 Ga1 O2 91.58(16) 6_556 . ? O8 Ga1 O2 171.32(16) 6_556 . ? O4 Ga1 O11 94.12(17) 6_556 . ? O8 Ga1 O11 92.91(16) 6_556 . ? O2 Ga1 O11 93.33(16) . . ? O4 Ga1 O10 99.79(16) 6_556 7_556 ? O8 Ga1 O10 82.80(15) 6_556 7_556 ? O2 Ga1 O10 89.70(15) . 7_556 ? O11 Ga1 O10 165.67(16) . 7_556 ? O4 Ga1 O9 178.66(15) 6_556 . ? O8 Ga1 O9 86.14(16) 6_556 . ? O2 Ga1 O9 88.44(15) . . ? O11 Ga1 O9 84.54(16) . . ? O10 Ga1 O9 81.54(14) 7_556 . ? O1 Ga2 O5 112.30(17) . . ? O1 Ga2 O3 114.04(17) . 6_556 ? O5 Ga2 O3 106.04(17) . 6_556 ? O1 Ga2 O6 103.00(16) . 7_546 ? O5 Ga2 O6 113.37(17) . 7_546 ? O3 Ga2 O6 108.21(17) 6_556 7_546 ? O11 Ga3 O11 115.5(3) 2_556 . ? O11 Ga3 O7 93.69(17) 2_556 5_556 ? O11 Ga3 O7 89.85(16) . 5_556 ? O11 Ga3 O7 89.85(16) 2_556 6_556 ? O11 Ga3 O7 93.69(17) . 6_556 ? O7 Ga3 O7 173.4(2) 5_556 6_556 ? O11 Ga3 N1 122.26(13) 2_556 . ? O11 Ga3 N1 122.26(13) . . ? O7 Ga3 N1 86.68(11) 5_556 . ? O7 Ga3 N1 86.68(11) 6_556 . ? O4 P1 O2 107.7(2) . . ? O4 P1 O3 108.2(2) . . ? O2 P1 O3 111.5(2) . . ? O4 P1 O1 113.0(2) . . ? O2 P1 O1 111.4(2) . . ? O3 P1 O1 105.0(2) . . ? O8 P2 O7 113.7(2) . . ? O8 P2 O5 110.6(2) . . ? O7 P2 O5 106.8(2) . . ? O8 P2 O6 108.2(2) . . ? O7 P2 O6 109.4(2) . . ? O5 P2 O6 107.9(2) . . ? P1 O1 Ga2 136.0(2) . . ? P1 O2 Ga1 134.7(2) . . ? P1 O3 Ga2 127.5(2) . 6 ? P1 O4 Ga1 150.4(3) . 6 ? P2 O5 Ga2 130.1(2) . . ? P2 O6 Ga2 128.7(2) . 7_546 ? P2 O7 Ga3 129.9(2) . 5_556 ? P2 O8 Ga1 136.0(2) . 6 ? C7 O9 Ga1 112.4(3) . . ? C7 O10 Ga1 112.2(3) . 7_556 ? Ga3 O11 Ga1 135.0(2) . . ? C1 N1 C1 118.1(7) 2_556 . ? C1 N1 Ga3 120.9(4) 2_556 . ? C1 N1 Ga3 120.9(4) . . ? C6 N2 C6 120.2(8) 2_556 . ? N1 C1 C2 122.7(6) . . ? C1 C2 C3 119.6(6) . . ? C2 C3 C2 117.2(8) 2_556 . ? C2 C3 C4 121.4(4) 2_556 . ? C2 C3 C4 121.4(4) . . ? C5 C4 C5 117.5(8) . 2_556 ? C5 C4 C3 121.2(4) . . ? C5 C4 C3 121.2(4) 2_556 . ? C6 C5 C4 120.1(7) . . ? N2 C6 C5 121.0(7) . . ? O9 C7 O10 126.9(5) . . ? O9 C7 C7 116.3(6) . 7_556 ? O10 C7 C7 116.8(6) . 7_556 ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.786 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.170