# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/195 data_shelxl _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H16 Ga3 N2 O15 P3' _chemical_formula_weight 622.25 _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' 'Ga' 'Ga' 0.2307 1.6083 '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' 'O' 'O' 0.0106 0.0060 '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' _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+1/2, -y+1/2, z' '-x, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y, -z-1/2' '-x-1/2, y-1/2, -z' 'x, y-1/2, -z-1/2' _cell_length_a 10.043(3) _cell_length_b 15.989(4) _cell_length_c 18.308(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2939.9(15) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.812 _exptl_crystal_density_method ? _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 5.878 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _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 4266 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1273 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 29.89 _reflns_number_total 4266 _reflns_number_observed 2269 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. 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^)+(0.0775P)^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 0.00050(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4266 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1277 _refine_ls_R_factor_obs 0.0436 _refine_ls_wR_factor_all 0.1351 _refine_ls_wR_factor_obs 0.1164 _refine_ls_goodness_of_fit_all 0.992 _refine_ls_goodness_of_fit_obs 1.197 _refine_ls_restrained_S_all 0.992 _refine_ls_restrained_S_obs 1.197 _refine_ls_shift/esd_max 0.007 _refine_ls_shift/esd_mean 0.001 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 Ga1 Ga 0.34755(6) 0.99491(4) 0.40569(3) 0.00769(15) Uani 1 d . . Ga2 Ga 0.31552(7) 0.96521(4) 0.21765(4) 0.00779(16) Uani 1 d . . Ga3 Ga 0.16442(7) 1.14742(4) 0.17452(3) 0.00806(16) Uani 1 d . . P1 P 0.11577(15) 1.06658(10) 0.31906(8) 0.0071(3) Uani 1 d . . P2 P 0.33959(15) 0.81904(10) 0.33169(8) 0.0072(3) Uani 1 d . . P3 P 0.63779(15) 1.01525(10) 0.42420(8) 0.0076(3) Uani 1 d . . O1 O 0.1470(4) 0.9912(3) 0.2710(2) 0.0104(8) Uani 1 d . . O2 O -0.0300(4) 1.0635(3) 0.3434(2) 0.0124(9) Uani 1 d . . O3 O 0.2032(4) 1.0681(3) 0.3885(2) 0.0115(9) Uani 1 d . . O4 O 0.1417(5) 1.1490(3) 0.2770(2) 0.0138(9) Uani 1 d . . O5 O 0.3025(4) 0.8490(3) 0.2552(2) 0.0099(9) Uani 1 d . . O6 O 0.2567(5) 0.7421(3) 0.3526(2) 0.0114(9) Uani 1 d . . O7 O 0.4884(4) 0.7958(3) 0.3361(2) 0.0126(9) Uani 1 d . . O8 O 0.3034(4) 0.8834(3) 0.3918(2) 0.0108(9) Uani 1 d . . O9 O 0.7190(4) 1.0198(3) 0.4948(2) 0.0093(9) Uani 1 d . . O10 O 0.7075(4) 1.0668(3) 0.3642(2) 0.0087(9) Uani 1 d . . O11 O 0.6168(5) 0.9232(3) 0.4016(2) 0.0131(9) Uani 1 d . . O12 O 0.4985(4) 1.0538(3) 0.4366(2) 0.0098(9) Uani 1 d . . O13 O 0.3293(4) 1.0819(3) 0.1839(2) 0.0119(9) Uani 1 d . . O14 O 0.4115(4) 0.9972(3) 0.3047(2) 0.0108(9) Uani 1 d . . OW O 0.5101(7) 0.6780(4) 0.2177(4) 0.0470(17) Uiso 1 d . . N1 N 0.3321(9) 0.7555(6) 0.1208(5) 0.049(2) Uiso 1 d . . C2 C 0.4953(11) 0.7722(6) 0.0223(5) 0.042(2) Uiso 1 d . . C1 C 0.3526(12) 0.7510(8) 0.0417(6) 0.052(3) Uiso 1 d . . C3 C 0.5147(14) 0.8464(9) -0.0253(8) 0.072(4) Uiso 1 d . . N21 N 0.4714(11) 0.8563(7) -0.0872(6) 0.014(2) Uiso 0.50 d P . N22 N 0.4965(15) 0.9333(9) -0.0197(8) 0.031(3) Uiso 0.50 d P . 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 0.0049(3) 0.0096(3) 0.0085(3) -0.0004(2) -0.0009(2) -0.0001(3) Ga2 0.0058(3) 0.0093(3) 0.0083(3) 0.0000(2) -0.0008(2) 0.0009(3) Ga3 0.0065(3) 0.0084(3) 0.0093(3) 0.0009(2) -0.0002(2) -0.0010(3) P1 0.0033(6) 0.0095(7) 0.0086(7) 0.0001(6) -0.0002(5) -0.0002(6) P2 0.0052(6) 0.0077(7) 0.0087(7) 0.0002(5) 0.0012(6) 0.0000(6) P3 0.0045(6) 0.0107(7) 0.0076(7) -0.0006(5) 0.0015(5) -0.0012(5) O1 0.007(2) 0.012(2) 0.0123(19) -0.0025(16) 0.0005(16) 0.0012(17) O2 0.006(2) 0.016(2) 0.015(2) -0.0015(18) -0.0032(17) -0.0005(18) O3 0.012(2) 0.013(2) 0.010(2) -0.0009(17) -0.0031(16) 0.0081(18) O4 0.017(2) 0.014(2) 0.011(2) 0.0059(18) 0.0020(18) 0.001(2) O5 0.011(2) 0.006(2) 0.013(2) 0.0004(17) -0.0002(17) 0.0033(17) O6 0.011(2) 0.007(2) 0.017(2) 0.0002(17) -0.0018(18) -0.0052(18) O7 0.006(2) 0.013(2) 0.019(2) 0.0006(17) 0.0018(17) -0.0043(18) O8 0.013(2) 0.011(2) 0.009(2) -0.0034(17) 0.0022(17) -0.0024(18) O9 0.0035(19) 0.019(2) 0.0056(18) 0.0011(17) -0.0010(15) -0.0006(17) O10 0.0040(19) 0.012(2) 0.0097(19) -0.0017(17) 0.0003(15) -0.0031(17) O11 0.016(2) 0.010(2) 0.013(2) -0.0013(17) 0.0044(18) -0.0033(19) O12 0.0034(19) 0.016(2) 0.010(2) -0.0041(17) -0.0018(16) 0.0013(16) O13 0.011(2) 0.007(2) 0.018(2) -0.0005(17) -0.0022(18) -0.0005(18) O14 0.008(2) 0.018(2) 0.0070(19) -0.0012(17) -0.0035(15) -0.0052(19) _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 O8 1.854(5) . ? Ga1 O12 1.872(4) . ? Ga1 O3 1.889(4) . ? Ga1 O9 1.955(4) 5_676 ? Ga1 O14 1.958(4) . ? Ga2 O10 1.920(4) 6_576 ? Ga2 O14 1.931(4) . ? Ga2 O2 1.967(4) 6_676 ? Ga2 O13 1.970(4) . ? Ga2 O5 1.986(4) . ? Ga2 O1 1.997(4) . ? Ga3 O6 1.843(4) 8_566 ? Ga3 O11 1.857(5) 6_576 ? Ga3 O4 1.890(4) . ? Ga3 O13 1.967(5) . ? Ga3 O7 1.996(4) 6_576 ? P1 O1 1.526(5) . ? P1 O2 1.531(5) . ? P1 O3 1.545(4) . ? P1 O4 1.548(5) . ? P2 O5 1.526(5) . ? P2 O6 1.534(5) . ? P2 O7 1.542(5) . ? P2 O8 1.551(4) . ? P3 O9 1.530(4) . ? P3 O10 1.541(4) . ? P3 O11 1.543(5) . ? P3 O12 1.545(4) . ? O2 Ga2 1.967(4) 6_576 ? O6 Ga3 1.843(4) 8_556 ? O7 Ga3 1.996(4) 6_676 ? O9 Ga1 1.955(4) 5_676 ? O10 Ga2 1.920(4) 6_676 ? O11 Ga3 1.857(4) 6_676 ? N1 C1 1.465(14) . ? C2 C3 1.485(17) . ? C2 C1 1.515(15) . ? C3 N21 1.225(16) . ? C3 N22 1.405(19) . ? N21 N22 1.763(19) . ? 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 O8 Ga1 O12 135.9(2) . . ? O8 Ga1 O3 112.9(2) . . ? O12 Ga1 O3 111.1(2) . . ? O8 Ga1 O9 85.98(18) . 5_676 ? O12 Ga1 O9 93.18(18) . 5_676 ? O3 Ga1 O9 88.15(18) . 5_676 ? O8 Ga1 O14 88.10(19) . . ? O12 Ga1 O14 90.63(18) . . ? O3 Ga1 O14 94.75(19) . . ? O9 Ga1 O14 174.05(19) 5_676 . ? O10 Ga2 O14 175.44(19) 6_576 . ? O10 Ga2 O2 86.56(18) 6_576 6_676 ? O14 Ga2 O2 97.86(19) . 6_676 ? O10 Ga2 O13 92.76(18) 6_576 . ? O14 Ga2 O13 88.43(19) . . ? O2 Ga2 O13 89.26(19) 6_676 . ? O10 Ga2 O5 89.05(19) 6_576 . ? O14 Ga2 O5 89.70(19) . . ? O2 Ga2 O5 91.76(19) 6_676 . ? O13 Ga2 O5 177.98(18) . . ? O10 Ga2 O1 87.60(18) 6_576 . ? O14 Ga2 O1 87.98(19) . . ? O2 Ga2 O1 174.16(18) 6_676 . ? O13 Ga2 O1 90.92(19) . . ? O5 Ga2 O1 88.24(18) . . ? O6 Ga3 O11 115.3(2) 8_566 6_576 ? O6 Ga3 O4 108.5(2) 8_566 . ? O11 Ga3 O4 136.2(2) 6_576 . ? O6 Ga3 O13 92.1(2) 8_566 . ? O11 Ga3 O13 87.64(19) 6_576 . ? O4 Ga3 O13 91.24(19) . . ? O6 Ga3 O7 92.6(2) 8_566 6_576 ? O11 Ga3 O7 88.57(19) 6_576 6_576 ? O4 Ga3 O7 89.1(2) . 6_576 ? O13 Ga3 O7 174.85(19) . 6_576 ? O1 P1 O2 109.8(3) . . ? O1 P1 O3 111.7(2) . . ? O2 P1 O3 107.7(2) . . ? O1 P1 O4 110.5(3) . . ? O2 P1 O4 109.5(3) . . ? O3 P1 O4 107.5(3) . . ? O5 P2 O6 110.3(3) . . ? O5 P2 O7 111.1(3) . . ? O6 P2 O7 108.7(3) . . ? O5 P2 O8 112.7(3) . . ? O6 P2 O8 103.2(2) . . ? O7 P2 O8 110.5(3) . . ? O9 P3 O10 109.5(2) . . ? O9 P3 O11 110.2(3) . . ? O10 P3 O11 112.4(2) . . ? O9 P3 O12 109.8(2) . . ? O10 P3 O12 107.6(3) . . ? O11 P3 O12 107.2(3) . . ? P1 O1 Ga2 128.4(3) . . ? P1 O2 Ga2 126.6(3) . 6_576 ? P1 O3 Ga1 124.3(3) . . ? P1 O4 Ga3 120.2(3) . . ? P2 O5 Ga2 126.5(3) . . ? P2 O6 Ga3 149.9(3) . 8_556 ? P2 O7 Ga3 138.0(3) . 6_676 ? P2 O8 Ga1 132.8(3) . . ? P3 O9 Ga1 126.8(3) . 5_676 ? P3 O10 Ga2 132.1(3) . 6_676 ? P3 O11 Ga3 138.2(3) . 6_676 ? P3 O12 Ga1 119.2(3) . . ? Ga3 O13 Ga2 118.2(2) . . ? Ga2 O14 Ga1 127.6(2) . . ? C3 C2 C1 116.1(10) . . ? N1 C1 C2 110.7(9) . . ? N21 C3 N22 83.9(12) . . ? N21 C3 C2 126.9(13) . . ? N22 C3 C2 137.0(13) . . ? C3 N21 N22 52.4(9) . . ? C3 N22 N21 43.7(8) . . ? _refine_diff_density_max 1.836 _refine_diff_density_min -1.853 _refine_diff_density_rms 0.304