# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1897 data_mgapo-sta-7 _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_name_common Mg-STA-7 _chemical_formula_moiety 'C3.38 H8.62 Al3 N1.12 O12.38 P3' _chemical_formula_structural 'C3.38 H8.62 Al3 N1.12 O12.38 P3' _chemical_formula_analytical 'C3.38 H8.62 Al3 N1.12 O12.38 P3' _chemical_formula_sum 'C3.38 H8.62 Al3 N1.12 O12.38 P3' _chemical_formula_weight 436.84 _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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 18.7732(8) _cell_length_b 18.7732(8) _cell_length_c 9.4537(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3331.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 57 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method - _exptl_crystal_F_000 1758 _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.844449 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 14250 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2403 _reflns_number_observed 1629 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 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^)+(0.1393P)^2^+6.1083P] 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(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2353 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_obs 0.0539 _refine_ls_wR_factor_all 0.2303 _refine_ls_wR_factor_obs 0.1422 _refine_ls_goodness_of_fit_all 0.806 _refine_ls_goodness_of_fit_obs 0.828 _refine_ls_restrained_S_all 1.113 _refine_ls_restrained_S_obs 0.828 _refine_ls_shift/esd_max -0.054 _refine_ls_shift/esd_mean 0.005 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 P1 P 0.06413(8) 0.55768(8) 0.3363(2) 0.0268(5) Uani 1 d . . O1 O 0.0574(3) 0.6243(2) 0.2463(5) 0.0479(12) Uani 1 d . . O2 O 0.0754(3) 0.5807(3) 0.4878(4) 0.0473(13) Uani 1 d . . O3 O 0.1273(2) 0.5128(2) 0.2903(5) 0.0465(12) Uani 1 d . . O4 O -0.0050(2) 0.5162(2) 0.3239(5) 0.0477(12) Uani 1 d . . Al1 Al 0.06412(9) 0.66568(9) 0.0809(2) 0.0258(5) Uani 1 d . . P2 P -0.05021(8) 0.66685(8) -0.1622(2) 0.0268(5) Uani 1 d . . O5 O -0.0151(2) 0.6567(2) -0.0189(5) 0.0452(12) Uani 1 d . . O6 O -0.0026(2) 0.6359(2) -0.2775(5) 0.0461(12) Uani 1 d . . O7 O -0.1221(2) 0.6292(2) -0.1598(5) 0.0499(13) Uani 1 d . . O8 O -0.0624(3) 0.7442(2) -0.1932(6) 0.0524(14) Uani 1 d . . Al2 Al -0.04423(9) 0.83599(9) -0.1578(2) 0.0270(5) Uani 1 d . . P3 P 0.06624(9) 0.83420(8) 0.0942(2) 0.0272(4) Uani 1 d . . O9 O -0.0021(3) 0.8449(3) 0.0127(5) 0.0492(13) Uani 1 d . . O10 O 0.1297(2) 0.8630(2) 0.0146(5) 0.0458(12) Uani 1 d . . O11 O 0.0599(3) 0.8703(2) 0.2363(4) 0.0524(14) Uani 1 d . . O12 O 0.0795(3) 0.7556(2) 0.1207(5) 0.0503(13) Uani 1 d . . Al3 Al -0.05070(9) 0.43481(9) 0.3358(2) 0.0252(5) Uani 1 d . . N1 N -0.1485(5) 0.7867(5) 0.3433(10) 0.103(3) Uiso 1 d . . C1 C -0.1274(10) 0.7369(11) 0.2487(21) 0.177(6) Uiso 1 d . . C2 C -0.1513(9) 0.6575(8) 0.2573(18) 0.143(5) Uiso 1 d . . C3 C -0.0891(12) 0.8019(12) 0.4511(23) 0.204(8) Uiso 1 d . . O20 O -0.2500 0.7500 -0.0803(25) 0.164(8) Uiso 1 d S . O30 O -0.2500 0.7500 -0.3900(61) 0.211(21) Uiso 0.50 d SP . C4 C 0.2500 0.7500 0.3428(48) 0.108(13) Uiso 0.40 d SP . C5 C 0.1764(27) 0.7449(26) 0.4623(55) 0.083(14) Uiso 0.20 d P . C6 C 0.0924(19) 0.7466(19) 0.4881(35) 0.046(9) Uiso 0.20 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 P1 0.0387(10) 0.0228(8) 0.0188(8) 0.0005(6) 0.0042(7) -0.0030(7) O1 0.072(3) 0.033(3) 0.039(3) 0.010(2) 0.012(2) 0.002(2) O2 0.060(3) 0.055(3) 0.026(3) -0.009(2) 0.003(2) -0.014(2) O3 0.049(3) 0.043(3) 0.047(3) -0.002(2) 0.006(2) 0.007(2) O4 0.048(3) 0.046(3) 0.049(3) 0.004(2) -0.001(2) -0.016(2) Al1 0.0330(10) 0.0210(9) 0.0235(10) 0.0004(7) 0.0015(8) 0.0034(7) P2 0.0229(9) 0.0222(8) 0.0352(10) -0.0058(7) -0.0014(7) 0.0009(6) O5 0.044(3) 0.050(3) 0.041(3) 0.001(2) -0.010(2) 0.001(2) O6 0.051(3) 0.044(3) 0.043(3) -0.005(2) 0.005(2) 0.014(2) O7 0.025(2) 0.047(3) 0.077(4) -0.013(3) -0.005(2) -0.009(2) O8 0.060(3) 0.030(3) 0.068(3) -0.005(2) -0.014(3) 0.014(2) Al2 0.0283(10) 0.0211(10) 0.0317(10) 0.0024(8) 0.0009(8) 0.0017(7) P3 0.0406(10) 0.0195(8) 0.0216(8) 0.0008(6) -0.0013(7) -0.0055(7) O9 0.057(3) 0.053(3) 0.038(3) -0.006(2) -0.008(2) 0.006(2) O10 0.048(3) 0.044(3) 0.046(3) 0.011(2) 0.009(2) -0.006(2) O11 0.086(4) 0.046(3) 0.026(3) -0.010(2) 0.002(2) -0.013(3) O12 0.071(3) 0.029(3) 0.051(3) 0.008(2) -0.012(3) -0.006(2) Al3 0.0259(10) 0.0321(10) 0.0177(9) -0.0032(7) -0.0022(7) 0.0016(7) _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 P1 O3 1.520(5) . ? P1 O2 1.511(4) . ? P1 O1 1.518(4) . ? P1 O4 1.517(5) . ? O1 Al1 1.750(5) . ? O2 Al3 1.755(4) 5_566 ? O3 Al2 1.785(5) 8_665 ? O4 Al3 1.757(5) . ? Al1 O10 1.772(5) 8_665 ? Al1 O12 1.753(5) . ? Al1 O5 1.769(5) . ? P2 O8 1.500(4) . ? P2 O6 1.525(4) . ? P2 O5 1.519(5) . ? P2 O7 1.523(4) . ? O6 Al3 1.751(4) 5_565 ? O7 Al2 1.779(5) 4_455 ? O8 Al2 1.787(5) . ? Al2 O7 1.779(5) 3_565 ? Al2 O3 1.785(5) 7_565 ? Al2 O9 1.802(5) . ? P3 O12 1.518(4) . ? P3 O11 1.509(4) . ? P3 O10 1.510(5) . ? P3 O9 1.511(5) . ? O10 Al1 1.772(5) 7_565 ? O11 Al3 1.759(4) 3_565 ? Al3 O11 1.759(4) 4_455 ? Al3 O6 1.751(4) 5_565 ? Al3 O2 1.755(4) 5_566 ? 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 O3 P1 O2 108.7(3) . . ? O3 P1 O1 111.2(3) . . ? O2 P1 O1 108.0(3) . . ? O3 P1 O4 111.2(3) . . ? O2 P1 O4 109.9(3) . . ? O1 P1 O4 107.9(3) . . ? P1 O1 Al1 149.4(3) . . ? P1 O2 Al3 144.7(3) . 5_566 ? P1 O3 Al2 146.6(3) . 8_665 ? P1 O4 Al3 149.2(3) . . ? O1 Al1 O10 110.0(2) . 8_665 ? O1 Al1 O12 104.3(2) . . ? O10 Al1 O12 110.4(2) 8_665 . ? O1 Al1 O5 111.9(2) . . ? O10 Al1 O5 109.9(2) 8_665 . ? O12 Al1 O5 110.2(2) . . ? O8 P2 O6 108.6(3) . . ? O8 P2 O5 111.2(3) . . ? O6 P2 O5 109.5(3) . . ? O8 P2 O7 108.5(3) . . ? O6 P2 O7 110.7(3) . . ? O5 P2 O7 108.2(3) . . ? P2 O5 Al1 146.0(3) . . ? P2 O6 Al3 148.1(3) . 5_565 ? P2 O7 Al2 143.9(3) . 4_455 ? P2 O8 Al2 150.2(3) . . ? O7 Al2 O8 104.7(2) 3_565 . ? O7 Al2 O3 111.0(2) 3_565 7_565 ? O8 Al2 O3 110.7(2) . 7_565 ? O7 Al2 O9 111.2(2) 3_565 . ? O8 Al2 O9 109.9(2) . . ? O3 Al2 O9 109.2(2) 7_565 . ? O12 P3 O11 107.6(3) . . ? O12 P3 O10 107.5(3) . . ? O11 P3 O10 110.2(3) . . ? O12 P3 O9 110.7(3) . . ? O11 P3 O9 109.1(3) . . ? O10 P3 O9 111.6(3) . . ? P3 O9 Al2 144.7(3) . . ? P3 O10 Al1 146.2(3) . 7_565 ? P3 O11 Al3 148.2(3) . 3_565 ? P3 O12 Al1 150.8(3) . . ? O11 Al3 O4 109.2(2) 4_455 . ? O11 Al3 O6 110.8(2) 4_455 5_565 ? O4 Al3 O6 111.1(2) . 5_565 ? O11 Al3 O2 107.1(2) 4_455 5_566 ? O4 Al3 O2 109.5(2) . 5_566 ? O6 Al3 O2 109.0(2) 5_565 5_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 Al1 37.4(7) . . . . ? O2 P1 O1 Al1 156.5(6) . . . . ? O4 P1 O1 Al1 -84.8(7) . . . . ? O3 P1 O2 Al3 -103.3(6) . . . 5_566 ? O1 P1 O2 Al3 136.0(5) . . . 5_566 ? O4 P1 O2 Al3 18.6(7) . . . 5_566 ? O2 P1 O3 Al2 170.6(5) . . . 8_665 ? O1 P1 O3 Al2 -70.7(6) . . . 8_665 ? O4 P1 O3 Al2 49.5(6) . . . 8_665 ? O3 P1 O4 Al3 34.6(7) . . . . ? O2 P1 O4 Al3 -85.8(7) . . . . ? O1 P1 O4 Al3 156.8(6) . . . . ? P1 O1 Al1 O10 -36.1(7) . . . 8_665 ? P1 O1 Al1 O12 -154.5(6) . . . . ? P1 O1 Al1 O5 86.3(7) . . . . ? O8 P2 O5 Al1 -72.1(6) . . . . ? O6 P2 O5 Al1 48.0(6) . . . . ? O7 P2 O5 Al1 168.8(5) . . . . ? O1 Al1 O5 P2 -170.3(5) . . . . ? O10 Al1 O5 P2 -47.8(6) 8_665 . . . ? O12 Al1 O5 P2 74.1(6) . . . . ? O8 P2 O6 Al3 167.6(6) . . . 5_565 ? O5 P2 O6 Al3 45.9(7) . . . 5_565 ? O7 P2 O6 Al3 -73.4(6) . . . 5_565 ? O8 P2 O7 Al2 168.3(5) . . . 4_455 ? O6 P2 O7 Al2 49.2(6) . . . 4_455 ? O5 P2 O7 Al2 -70.9(6) . . . 4_455 ? O6 P2 O8 Al2 -103.8(7) . . . . ? O5 P2 O8 Al2 16.8(8) . . . . ? O7 P2 O8 Al2 135.8(7) . . . . ? P2 O8 Al2 O7 -136.3(7) . . . 3_565 ? P2 O8 Al2 O3 104.0(7) . . . 7_565 ? P2 O8 Al2 O9 -16.8(8) . . . . ? O12 P3 O9 Al2 -73.0(6) . . . . ? O11 P3 O9 Al2 168.8(5) . . . . ? O10 P3 O9 Al2 46.8(6) . . . . ? O7 Al2 O9 P3 -170.3(5) 3_565 . . . ? O8 Al2 O9 P3 74.2(6) . . . . ? O3 Al2 O9 P3 -47.5(6) 7_565 . . . ? O12 P3 O10 Al1 169.7(5) . . . 7_565 ? O11 P3 O10 Al1 -73.3(6) . . . 7_565 ? O9 P3 O10 Al1 48.1(6) . . . 7_565 ? O12 P3 O11 Al3 157.8(6) . . . 3_565 ? O10 P3 O11 Al3 40.9(7) . . . 3_565 ? O9 P3 O11 Al3 -82.0(7) . . . 3_565 ? O11 P3 O12 Al1 138.2(7) . . . . ? O10 P3 O12 Al1 -103.1(7) . . . . ? O9 P3 O12 Al1 19.1(8) . . . . ? O1 Al1 O12 P3 -138.1(7) . . . . ? O10 Al1 O12 P3 103.8(7) 8_665 . . . ? O5 Al1 O12 P3 -17.8(8) . . . . ? P1 O4 Al3 O11 -158.9(6) . . . 4_455 ? P1 O4 Al3 O6 -36.3(7) . . . 5_565 ? P1 O4 Al3 O2 84.1(7) . . . 5_566 ? #===END data_Co-STA-7 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C1.75 H5.50 Al2.10 Co0.90 N0.50 O12.75 P3' _chemical_formula_structural 'C1.75 H5.50 Al2.10 Co0.90 N0.50 O12.75 P3' _chemical_formula_analytical 'C1.75 H5.50 Al2.10 Co0.90 N0.50 O12.75 P3' _chemical_formula_sum 'C1.75 H5.50 Al2.10 Co0.90 N0.50 O12.75 P3' _chemical_formula_weight 440.17 _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' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 18.740(5) _cell_length_b 18.740 _cell_length_c 9.439(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3314.9(25) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.61 _cell_measurement_theta_max 12.18 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method - _exptl_crystal_F_000 1745 _exptl_absorpt_coefficient_mu 11.749 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.6209 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device AFC7S _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time - _diffrn_standards_decay_% 1.3 _diffrn_reflns_number 2642 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 60.14 _reflns_number_total 2472 _reflns_number_observed 1311 _reflns_observed_criterion >2sigma(I) _computing_data_collection teXsan _computing_cell_refinement teXsan _computing_data_reduction teXsan _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 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^)+(0.2179P)^2^+36.8230P] 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-SWAT _refine_ls_extinction_coef - _refine_ls_number_reflns 2422 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2029 _refine_ls_R_factor_obs 0.1169 _refine_ls_wR_factor_all 0.4409 _refine_ls_wR_factor_obs 0.3134 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.203 _refine_ls_restrained_S_all 1.277 _refine_ls_restrained_S_obs 1.203 _refine_ls_shift/esd_max -1.068 _refine_ls_shift/esd_mean 0.059 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 Al1 Al 0.0661(2) 0.55131(15) 0.3350(3) 0.107(3) Uani 0.70 d P . Co1 Co 0.0661(2) 0.55131(15) 0.3350(3) 0.0181(13) Uani 0.30 d P . O1 O 0.0602(5) 0.6278(4) 0.2396(8) 0.064(2) Uani 1 d . . O2 O 0.0803(5) 0.5745(5) 0.5058(9) 0.071(3) Uani 1 d . . O3 O 0.1370(5) 0.5002(5) 0.2824(9) 0.069(3) Uani 1 d . . O4 O -0.0129(5) 0.5051(5) 0.3198(9) 0.073(3) Uani 1 d . . P1 P 0.0675(2) 0.6661(2) 0.0924(3) 0.0467(7) Uani 1 d . . Al2 Al -0.04526(14) 0.66417(13) -0.1571(3) 0.053(2) Uani 0.70 d P . Co2 Co -0.04526(14) 0.66417(13) -0.1571(3) 0.043(2) Uani 0.30 d P . O5 O -0.0008(5) 0.6544(5) 0.0060(10) 0.080(3) Uani 1 d . . O6 O 0.0097(5) 0.6306(5) -0.2909(9) 0.074(3) Uani 1 d . . O7 O -0.1265(5) 0.6214(4) -0.1555(10) 0.072(3) Uani 1 d . . O8 O -0.0639(5) 0.7524(4) -0.1914(9) 0.067(3) Uani 1 d . . P2 P -0.0490(2) 0.83370(15) -0.1596(3) 0.0452(7) Uani 1 d . . Al3 Al 0.0660(2) 0.83436(15) 0.0833(3) 0.057(2) Uani 0.70 d P . Co3 Co 0.0660(2) 0.83436(15) 0.0833(3) 0.057(2) Uani 0.30 d P . O9 O -0.0127(5) 0.8440(6) -0.0114(11) 0.086(3) Uani 1 d . . O10 O 0.1365(5) 0.8668(4) -0.0096(11) 0.068(3) Uani 1 d . . O11 O 0.0599(5) 0.8766(4) 0.2431(9) 0.067(3) Uani 1 d . . O12 O 0.0800(5) 0.7470(5) 0.1255(10) 0.075(3) Uani 1 d . . P3 P -0.05544(15) 0.4349(2) 0.3361(3) 0.0451(8) Uani 1 d . . O20 O 0.2500 0.2500 0.1929 0.204 Uiso 1 d S . O30 O 0.2500 0.7500 0.5000 0.207 Uiso 1 d S . O40 O 0.2500 0.2500 -0.0188 0.200 Uiso 1 d S . N1 N 0.3948 0.2638 0.6431 0.050 Uiso 0.13 d P . C1 C 0.4601 0.2412 0.5655 0.050 Uiso 0.13 d P . N2 N 0.0717 0.2598 0.6719 0.050 Uiso 0.13 d P . C2 C 0.0052 0.2818 0.5974 0.050 Uiso 0.13 d P . N3 N 0.2803 0.4072 0.6005 0.050 Uiso 0.13 d P . C3 C 0.2906 0.3986 0.7556 0.050 Uiso 0.13 d P . N4 N 0.2251 0.1373 0.6606 0.050 Uiso 0.13 d P . C4 C 0.2270 0.0861 0.5396 0.050 Uiso 0.13 d P . C5 C 0.1258 0.3187 0.6827 0.050 Uiso 0.13 d P . C6 C 0.1551 0.3497 0.5420 0.050 Uiso 0.13 d P . C7 C 0.2040 0.4157 0.5565 0.050 Uiso 0.13 d P . C8 C 0.3248 0.3598 0.5071 0.050 Uiso 0.13 d P . C9 C 0.3329 0.2800 0.5470 0.050 Uiso 0.13 d P . C10 C 0.3766 0.2174 0.7670 0.050 Uiso 0.13 d P . C11 C 0.3562 0.1382 0.7411 0.050 Uiso 0.13 d P . C12 C 0.2777 0.1183 0.7735 0.050 Uiso 0.13 d P . C13 C 0.1512 0.1486 0.7171 0.050 Uiso 0.13 d P . C14 C 0.1005 0.1904 0.6164 0.050 Uiso 0.13 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 Al1 0.165(8) 0.081(5) 0.076(5) -0.030(4) -0.002(5) -0.019(5) Co1 0.009(2) 0.035(3) 0.011(2) 0.016(2) 0.007(2) 0.010(2) O1 0.089(6) 0.061(5) 0.042(4) 0.017(4) 0.005(4) 0.020(4) O2 0.080(6) 0.091(6) 0.043(5) -0.016(4) 0.021(4) -0.029(5) O3 0.081(6) 0.076(6) 0.051(5) -0.005(5) 0.010(5) 0.004(5) O4 0.073(6) 0.075(6) 0.070(6) 0.013(5) -0.015(5) -0.002(5) P1 0.059(2) 0.0454(15) 0.0360(14) 0.0003(13) -0.0002(14) 0.0001(13) Al2 0.036(2) 0.068(3) 0.055(3) -0.008(3) 0.008(3) 0.028(2) Co2 0.077(4) 0.021(3) 0.032(4) 0.001(3) -0.011(4) -0.036(3) O5 0.091(7) 0.092(7) 0.058(6) 0.000(5) 0.000(5) 0.001(6) O6 0.086(6) 0.082(6) 0.054(5) -0.004(5) -0.006(5) 0.003(5) O7 0.078(6) 0.053(5) 0.086(6) 0.005(5) 0.010(5) -0.015(5) O8 0.086(6) 0.047(5) 0.066(6) 0.006(4) -0.009(5) 0.002(4) P2 0.0472(15) 0.0419(14) 0.047(2) 0.0049(14) -0.0024(14) 0.0040(12) Al3 0.102(4) 0.030(2) 0.040(3) -0.013(2) 0.014(3) -0.037(2) Co3 0.036(3) 0.093(5) 0.041(4) 0.008(4) -0.006(4) 0.043(3) O9 0.083(6) 0.101(8) 0.073(7) 0.000(6) 0.004(5) 0.010(6) O10 0.068(5) 0.054(5) 0.082(6) 0.001(5) -0.007(5) -0.010(4) O11 0.106(7) 0.052(5) 0.043(5) -0.013(4) 0.008(5) -0.010(5) O12 0.096(6) 0.055(5) 0.075(6) 0.003(4) -0.018(5) -0.001(5) P3 0.0451(15) 0.056(2) 0.0344(14) -0.0050(13) 0.0009(13) -0.0016(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 Al1 O2 1.691(9) . ? Al1 O1 1.697(8) . ? Al1 O3 1.710(9) . ? Al1 O4 1.722(10) . ? Co1 O2 1.691(9) . ? Co1 O1 1.697(8) . ? Co1 O3 1.710(9) . ? Co1 O4 1.722(10) . ? O1 P1 1.570(8) . ? O2 P3 1.573(8) 5_566 ? O3 P2 1.580(9) 8_665 ? O4 P3 1.546(10) . ? P1 O5 1.534(10) . ? P1 O10 1.560(9) 8_665 ? P1 O12 1.565(9) . ? Al2 O8 1.721(8) . ? Al2 O7 1.721(9) . ? Al2 O6 1.747(10) . ? Al2 O5 1.760(10) . ? Co2 O8 1.721(8) . ? Co2 O7 1.721(9) . ? Co2 O6 1.747(10) . ? Co2 O5 1.760(10) . ? O6 P3 1.557(10) 5_565 ? O7 P2 1.548(9) 4_455 ? O8 P2 1.578(8) . ? P2 O7 1.548(9) 3_565 ? P2 O9 1.568(11) . ? P2 O3 1.580(9) 7_565 ? Al3 O10 1.698(9) . ? Al3 O12 1.705(9) . ? Al3 O11 1.707(8) . ? Al3 O9 1.735(11) . ? Co3 O10 1.698(9) . ? Co3 O12 1.705(9) . ? Co3 O11 1.707(8) . ? Co3 O9 1.735(11) . ? O10 P1 1.560(9) 7_565 ? O11 P3 1.550(8) 3_565 ? P3 O11 1.550(8) 4_455 ? P3 O6 1.557(10) 5_565 ? P3 O2 1.573(8) 5_566 ? 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 O2 Al1 O1 107.4(4) . . ? O2 Al1 O3 107.4(5) . . ? O1 Al1 O3 111.7(4) . . ? O2 Al1 O4 110.1(4) . . ? O1 Al1 O4 108.9(4) . . ? O3 Al1 O4 111.2(5) . . ? O2 Co1 O1 107.4(4) . . ? O2 Co1 O3 107.4(5) . . ? O1 Co1 O3 111.7(4) . . ? O2 Co1 O4 110.1(4) . . ? O1 Co1 O4 108.9(4) . . ? O3 Co1 O4 111.2(5) . . ? P1 O1 Al1 148.2(6) . . ? P1 O1 Co1 148.2(6) . . ? Al1 O1 Co1 0.0(3) . . ? P3 O2 Al1 146.1(6) 5_566 . ? P3 O2 Co1 146.1(6) 5_566 . ? Al1 O2 Co1 0.0(3) . . ? P2 O3 Al1 144.1(6) 8_665 . ? P2 O3 Co1 144.1(6) 8_665 . ? Al1 O3 Co1 0.0(3) . . ? P3 O4 Al1 149.7(6) . . ? P3 O4 Co1 149.7(6) . . ? Al1 O4 Co1 0.0(3) . . ? O5 P1 O10 110.0(5) . 8_665 ? O5 P1 O12 111.7(5) . . ? O10 P1 O12 109.1(5) 8_665 . ? O5 P1 O1 109.4(5) . . ? O10 P1 O1 110.5(5) 8_665 . ? O12 P1 O1 106.2(5) . . ? O8 Al2 O7 105.6(4) . . ? O8 Al2 O6 109.3(5) . . ? O7 Al2 O6 111.1(5) . . ? O8 Al2 O5 111.1(5) . . ? O7 Al2 O5 111.3(5) . . ? O6 Al2 O5 108.4(5) . . ? O8 Co2 O7 105.6(4) . . ? O8 Co2 O6 109.3(5) . . ? O7 Co2 O6 111.1(5) . . ? O8 Co2 O5 111.1(5) . . ? O7 Co2 O5 111.3(5) . . ? O6 Co2 O5 108.4(5) . . ? P1 O5 Co2 147.7(7) . . ? P1 O5 Al2 147.7(7) . . ? Co2 O5 Al2 0.0(2) . . ? P3 O6 Al2 143.8(6) 5_565 . ? P3 O6 Co2 143.8(6) 5_565 . ? Al2 O6 Co2 0.0(2) . . ? P2 O7 Al2 146.5(6) 4_455 . ? P2 O7 Co2 146.5(6) 4_455 . ? Al2 O7 Co2 0.0(2) . . ? P2 O8 Al2 148.9(6) . . ? P2 O8 Co2 148.9(6) . . ? Al2 O8 Co2 0.0(2) . . ? O7 P2 O9 107.3(5) 3_565 . ? O7 P2 O8 108.3(5) 3_565 . ? O9 P2 O8 111.5(5) . . ? O7 P2 O3 111.3(5) 3_565 7_565 ? O9 P2 O3 111.0(5) . 7_565 ? O8 P2 O3 107.4(5) . 7_565 ? O10 Al3 O12 110.1(5) . . ? O10 Al3 O11 110.0(5) . . ? O12 Al3 O11 104.4(4) . . ? O10 Al3 O9 111.0(5) . . ? O12 Al3 O9 110.6(5) . . ? O11 Al3 O9 110.5(5) . . ? O10 Co3 O12 110.1(5) . . ? O10 Co3 O11 110.0(5) . . ? O12 Co3 O11 104.4(4) . . ? O10 Co3 O9 111.0(5) . . ? O12 Co3 O9 110.6(5) . . ? O11 Co3 O9 110.5(5) . . ? P2 O9 Co3 144.7(7) . . ? P2 O9 Al3 144.7(7) . . ? Co3 O9 Al3 0.0(3) . . ? P1 O10 Al3 144.9(6) 7_565 . ? P1 O10 Co3 144.9(6) 7_565 . ? Al3 O10 Co3 0.0(3) . . ? P3 O11 Al3 151.3(6) 3_565 . ? P3 O11 Co3 151.3(6) 3_565 . ? Al3 O11 Co3 0.0(3) . . ? P1 O12 Co3 149.3(7) . . ? P1 O12 Al3 149.3(7) . . ? Co3 O12 Al3 0.0(3) . . ? O4 P3 O11 108.3(5) . 4_455 ? O4 P3 O6 111.0(5) . 5_565 ? O11 P3 O6 110.3(5) 4_455 5_565 ? O4 P3 O2 110.0(5) . 5_566 ? O11 P3 O2 107.5(5) 4_455 5_566 ? O6 P3 O2 109.5(5) 5_565 5_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Al1 O1 P1 155.8(11) . . . . ? O3 Al1 O1 P1 38.2(13) . . . . ? O4 Al1 O1 P1 -85.0(12) . . . . ? O2 Al1 O1 Co1 0.0(1000) . . . . ? O3 Al1 O1 Co1 0.0(1000) . . . . ? O4 Al1 O1 Co1 0.0(1000) . . . . ? O2 Co1 O1 P1 155.8(11) . . . . ? O3 Co1 O1 P1 38.2(13) . . . . ? O4 Co1 O1 P1 -85.0(12) . . . . ? O2 Co1 O1 Al1 0.0(1000) . . . . ? O3 Co1 O1 Al1 0.0(1000) . . . . ? O4 Co1 O1 Al1 0.0(1000) . . . . ? O1 Al1 O2 P3 128.3(11) . . . 5_566 ? O3 Al1 O2 P3 -111.3(11) . . . 5_566 ? O4 Al1 O2 P3 9.9(13) . . . 5_566 ? O1 Al1 O2 Co1 0.0(1000) . . . . ? O3 Al1 O2 Co1 0.0(1000) . . . . ? O4 Al1 O2 Co1 0.0(1000) . . . . ? O1 Co1 O2 P3 128.3(11) . . . 5_566 ? O3 Co1 O2 P3 -111.3(11) . . . 5_566 ? O4 Co1 O2 P3 9.9(13) . . . 5_566 ? O1 Co1 O2 Al1 0.0(1000) . . . . ? O3 Co1 O2 Al1 0.0(1000) . . . . ? O4 Co1 O2 Al1 0.0(1000) . . . . ? O2 Al1 O3 P2 170.9(9) . . . 8_665 ? O1 Al1 O3 P2 -71.6(11) . . . 8_665 ? O4 Al1 O3 P2 50.3(11) . . . 8_665 ? O2 Al1 O3 Co1 0.0(1000) . . . . ? O1 Al1 O3 Co1 0.0(1000) . . . . ? O4 Al1 O3 Co1 0.0(1000) . . . . ? O2 Co1 O3 P2 170.9(9) . . . 8_665 ? O1 Co1 O3 P2 -71.6(11) . . . 8_665 ? O4 Co1 O3 P2 50.3(11) . . . 8_665 ? O2 Co1 O3 Al1 0.0(1000) . . . . ? O1 Co1 O3 Al1 0.0(1000) . . . . ? O4 Co1 O3 Al1 0.0(1000) . . . . ? O2 Al1 O4 P3 -78.8(13) . . . . ? O1 Al1 O4 P3 163.7(11) . . . . ? O3 Al1 O4 P3 40.1(13) . . . . ? O2 Al1 O4 Co1 0.0(1000) . . . . ? O1 Al1 O4 Co1 0.0(1000) . . . . ? O3 Al1 O4 Co1 0.0(1000) . . . . ? O2 Co1 O4 P3 -78.8(13) . . . . ? O1 Co1 O4 P3 163.7(11) . . . . ? O3 Co1 O4 P3 40.1(13) . . . . ? O2 Co1 O4 Al1 0.0(1000) . . . . ? O1 Co1 O4 Al1 0.0(1000) . . . . ? O3 Co1 O4 Al1 0.0(1000) . . . . ? Al1 O1 P1 O5 82.4(12) . . . . ? Co1 O1 P1 O5 82.4(12) . . . . ? Al1 O1 P1 O10 -38.7(13) . . . 8_665 ? Co1 O1 P1 O10 -38.7(13) . . . 8_665 ? Al1 O1 P1 O12 -156.9(11) . . . . ? Co1 O1 P1 O12 -156.9(11) . . . . ? O10 P1 O5 Co2 -50.9(14) 8_665 . . . ? O12 P1 O5 Co2 70.3(13) . . . . ? O1 P1 O5 Co2 -172.4(11) . . . . ? O10 P1 O5 Al2 -50.9(14) 8_665 . . . ? O12 P1 O5 Al2 70.3(13) . . . . ? O1 P1 O5 Al2 -172.4(11) . . . . ? O8 Co2 O5 P1 -69.8(13) . . . . ? O7 Co2 O5 P1 172.9(12) . . . . ? O6 Co2 O5 P1 50.4(14) . . . . ? O8 Co2 O5 Al2 0.0(1000) . . . . ? O7 Co2 O5 Al2 0.0(1000) . . . . ? O6 Co2 O5 Al2 0.0(1000) . . . . ? O8 Al2 O5 P1 -69.8(13) . . . . ? O7 Al2 O5 P1 172.9(12) . . . . ? O6 Al2 O5 P1 50.4(14) . . . . ? O8 Al2 O5 Co2 0.0(1000) . . . . ? O7 Al2 O5 Co2 0.0(1000) . . . . ? O6 Al2 O5 Co2 0.0(1000) . . . . ? O8 Al2 O6 P3 171.5(10) . . . 5_565 ? O7 Al2 O6 P3 -72.3(11) . . . 5_565 ? O5 Al2 O6 P3 50.3(12) . . . 5_565 ? O8 Al2 O6 Co2 0.0(1000) . . . . ? O7 Al2 O6 Co2 0.0(1000) . . . . ? O5 Al2 O6 Co2 0.0(1000) . . . . ? O8 Co2 O6 P3 171.5(10) . . . 5_565 ? O7 Co2 O6 P3 -72.3(11) . . . 5_565 ? O5 Co2 O6 P3 50.3(12) . . . 5_565 ? O8 Co2 O6 Al2 0.0(1000) . . . . ? O7 Co2 O6 Al2 0.0(1000) . . . . ? O5 Co2 O6 Al2 0.0(1000) . . . . ? O8 Al2 O7 P2 165.5(11) . . . 4_455 ? O6 Al2 O7 P2 47.1(13) . . . 4_455 ? O5 Al2 O7 P2 -73.8(13) . . . 4_455 ? O8 Al2 O7 Co2 0.0(1000) . . . . ? O6 Al2 O7 Co2 0.0(1000) . . . . ? O5 Al2 O7 Co2 0.0(1000) . . . . ? O8 Co2 O7 P2 165.5(11) . . . 4_455 ? O6 Co2 O7 P2 47.1(13) . . . 4_455 ? O5 Co2 O7 P2 -73.8(13) . . . 4_455 ? O8 Co2 O7 Al2 0.0(1000) . . . . ? O6 Co2 O7 Al2 0.0(1000) . . . . ? O5 Co2 O7 Al2 0.0(1000) . . . . ? O7 Al2 O8 P2 138.8(12) . . . . ? O6 Al2 O8 P2 -101.6(12) . . . . ? O5 Al2 O8 P2 18.0(14) . . . . ? O7 Al2 O8 Co2 0.0(1000) . . . . ? O6 Al2 O8 Co2 0.0(1000) . . . . ? O5 Al2 O8 Co2 0.0(1000) . . . . ? O7 Co2 O8 P2 138.8(12) . . . . ? O6 Co2 O8 P2 -101.6(12) . . . . ? O5 Co2 O8 P2 18.0(14) . . . . ? O7 Co2 O8 Al2 0.0(1000) . . . . ? O6 Co2 O8 Al2 0.0(1000) . . . . ? O5 Co2 O8 Al2 0.0(1000) . . . . ? Al2 O8 P2 O7 -138.4(11) . . . 3_565 ? Co2 O8 P2 O7 -138.4(11) . . . 3_565 ? Al2 O8 P2 O9 -20.5(14) . . . . ? Co2 O8 P2 O9 -20.5(14) . . . . ? Al2 O8 P2 O3 101.3(12) . . . 7_565 ? Co2 O8 P2 O3 101.3(12) . . . 7_565 ? O7 P2 O9 Co3 -167.8(11) 3_565 . . . ? O8 P2 O9 Co3 73.7(13) . . . . ? O3 P2 O9 Co3 -46.0(13) 7_565 . . . ? O7 P2 O9 Al3 -167.8(11) 3_565 . . . ? O8 P2 O9 Al3 73.7(13) . . . . ? O3 P2 O9 Al3 -46.0(13) 7_565 . . . ? O10 Co3 O9 P2 46.5(13) . . . . ? O12 Co3 O9 P2 -76.0(13) . . . . ? O11 Co3 O9 P2 168.8(11) . . . . ? O10 Co3 O9 Al3 0.0(1000) . . . . ? O12 Co3 O9 Al3 0.0(1000) . . . . ? O11 Co3 O9 Al3 0.0(1000) . . . . ? O10 Al3 O9 P2 46.5(13) . . . . ? O12 Al3 O9 P2 -76.0(13) . . . . ? O11 Al3 O9 P2 168.8(11) . . . . ? O10 Al3 O9 Co3 0.0(1000) . . . . ? O12 Al3 O9 Co3 0.0(1000) . . . . ? O11 Al3 O9 Co3 0.0(1000) . . . . ? O12 Al3 O10 P1 174.8(10) . . . 7_565 ? O11 Al3 O10 P1 -70.6(12) . . . 7_565 ? O9 Al3 O10 P1 52.0(12) . . . 7_565 ? O12 Al3 O10 Co3 0.0(1000) . . . . ? O11 Al3 O10 Co3 0.0(1000) . . . . ? O9 Al3 O10 Co3 0.0(1000) . . . . ? O12 Co3 O10 P1 174.8(10) . . . 7_565 ? O11 Co3 O10 P1 -70.6(12) . . . 7_565 ? O9 Co3 O10 P1 52.0(12) . . . 7_565 ? O12 Co3 O10 Al3 0.0(1000) . . . . ? O11 Co3 O10 Al3 0.0(1000) . . . . ? O9 Co3 O10 Al3 0.0(1000) . . . . ? O10 Al3 O11 P3 38.9(15) . . . 3_565 ? O12 Al3 O11 P3 157.1(13) . . . 3_565 ? O9 Al3 O11 P3 -84.0(14) . . . 3_565 ? O10 Al3 O11 Co3 0.0(1000) . . . . ? O12 Al3 O11 Co3 0.0(1000) . . . . ? O9 Al3 O11 Co3 0.0(1000) . . . . ? O10 Co3 O11 P3 38.9(15) . . . 3_565 ? O12 Co3 O11 P3 157.1(13) . . . 3_565 ? O9 Co3 O11 P3 -84.0(14) . . . 3_565 ? O10 Co3 O11 Al3 0.0(1000) . . . . ? O12 Co3 O11 Al3 0.0(1000) . . . . ? O9 Co3 O11 Al3 0.0(1000) . . . . ? O5 P1 O12 Co3 -23.9(15) . . . . ? O10 P1 O12 Co3 97.8(14) 8_665 . . . ? O1 P1 O12 Co3 -143.1(13) . . . . ? O5 P1 O12 Al3 -23.9(15) . . . . ? O10 P1 O12 Al3 97.8(14) 8_665 . . . ? O1 P1 O12 Al3 -143.1(13) . . . . ? O10 Co3 O12 P1 -97.6(14) . . . . ? O11 Co3 O12 P1 144.2(13) . . . . ? O9 Co3 O12 P1 25.4(15) . . . . ? O10 Co3 O12 Al3 0.0(1000) . . . . ? O11 Co3 O12 Al3 0.0(1000) . . . . ? O9 Co3 O12 Al3 0.0(1000) . . . . ? O10 Al3 O12 P1 -97.6(14) . . . . ? O11 Al3 O12 P1 144.2(13) . . . . ? O9 Al3 O12 P1 25.4(15) . . . . ? O10 Al3 O12 Co3 0.0(1000) . . . . ? O11 Al3 O12 Co3 0.0(1000) . . . . ? O9 Al3 O12 Co3 0.0(1000) . . . . ? Al1 O4 P3 O11 -160.5(11) . . . 4_455 ? Co1 O4 P3 O11 -160.5(11) . . . 4_455 ? Al1 O4 P3 O6 -39.2(14) . . . 5_565 ? Co1 O4 P3 O6 -39.2(14) . . . 5_565 ? Al1 O4 P3 O2 82.3(13) . . . 5_566 ? Co1 O4 P3 O2 82.3(13) . . . 5_566 ? _refine_diff_density_max 2.925 _refine_diff_density_min -1.979 _refine_diff_density_rms 0.208 #===END data_Zn-STA-7 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C1.75 H5 Al2.40 N0.50 O12.50 P3 Zn0.60' _chemical_formula_structural 'C1.75 H5 Al2.40 N0.50 O12.50 P3 Zn0.60' _chemical_formula_analytical 'C1.75 H5 Al2.40 N0.50 O12.50 P3 Zn0.60' _chemical_formula_sum 'C1.75 H5 Al2.40 N0.50 O12.50 P3 Zn0.60' _chemical_formula_weight 429.95 _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' 'Al' 'Al' 0.0645 0.0514 '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 Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 18.691(2) _cell_length_b 18.691(2) _cell_length_c 9.4230(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3292.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 83 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _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 1.735 _exptl_crystal_density_method - _exptl_crystal_F_000 1706 _exptl_absorpt_coefficient_mu 1.394 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68840 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time ? _diffrn_standards_decay_% - _diffrn_reflns_number 23263 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 29.46 _reflns_number_total 4743 _reflns_number_observed 3851 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 53 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^)+(0.0901P)^2^+15.7264P] 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 4690 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_obs 0.0912 _refine_ls_wR_factor_all 0.2595 _refine_ls_wR_factor_obs 0.2203 _refine_ls_goodness_of_fit_all 1.234 _refine_ls_goodness_of_fit_obs 1.311 _refine_ls_restrained_S_all 1.407 _refine_ls_restrained_S_obs 1.311 _refine_ls_shift/esd_max -8.433 _refine_ls_shift/esd_mean 0.247 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 P1 P 0.06489(3) 0.55720(2) 0.33558(5) 0.02538(11) Uani 1 d . . O1 O 0.05926(11) 0.62405(8) 0.2451(2) 0.0505(5) Uani 1 d . . O2 O 0.07494(11) 0.58091(10) 0.4891(2) 0.0495(5) Uani 1 d . . O3 O 0.12878(10) 0.51258(9) 0.2938(2) 0.0484(5) Uani 1 d . . O4 O -0.00461(9) 0.51641(9) 0.3214(2) 0.0479(5) Uani 1 d . . Al1 Al 0.06521(4) 0.66548(3) 0.08049(7) 0.02227(15) Uani 0.80 d P . Zn1 Zn 0.06403(6) 0.66497(6) 0.08047(12) 0.0283(3) Uani 0.20 d P . P2 P -0.05034(2) 0.66641(2) -0.16022(5) 0.02634(11) Uani 1 d . . O5 O -0.01476(9) 0.65644(10) -0.0164(2) 0.0476(5) Uani 1 d . . O6 O -0.00287(9) 0.63711(9) -0.2784(2) 0.0460(5) Uani 1 d . . O7 O -0.12185(9) 0.62916(10) -0.1574(2) 0.0538(5) Uani 1 d . . O8 O -0.06258(11) 0.74461(8) -0.1912(2) 0.0544(5) Uani 1 d . . Al2 Al -0.04419(4) 0.83607(3) -0.15605(7) 0.0221(2) Uani 0.80 d P . Zn2 Zn -0.04401(5) 0.83608(5) -0.15620(11) 0.0168(2) Uani 0.20 d P . P3 P 0.06733(3) 0.83418(2) 0.09549(5) 0.02615(11) Uani 1 d . . O9 O -0.00005(10) 0.84590(10) 0.0114(2) 0.0527(5) Uani 1 d . . O10 O 0.13261(10) 0.86198(10) 0.0170(2) 0.0493(5) Uani 1 d . . O11 O 0.06064(11) 0.86991(9) 0.2391(2) 0.0506(5) Uani 1 d . . O12 O 0.08017(11) 0.75543(8) 0.1223(2) 0.0540(5) Uani 1 d . . Al3 Al -0.05065(4) 0.43423(4) 0.33459(7) 0.0262(2) Uani 0.80 d P . Zn3 Zn -0.05024(5) 0.43416(6) 0.33524(11) 0.0208(2) Uani 0.20 d P . O20 O 0.2500 0.2500 0.6892(19) 0.272(7) Uiso 1 d S . O30 O 0.2500 0.2500 1.2550(21) 0.288(8) Uiso 1 d S . N1 N 0.3948 0.2638 0.6431 0.050 Uiso 0.13 d P . C1 C 0.4601 0.2412 0.5655 0.050 Uiso 0.13 d P . N2 N 0.0717 0.2598 0.6719 0.050 Uiso 0.13 d P . C2 C 0.0052 0.2818 0.5974 0.050 Uiso 0.13 d P . N3 N 0.2803 0.4072 0.6005 0.050 Uiso 0.13 d P . C3 C 0.2906 0.3986 0.7556 0.050 Uiso 0.13 d P . N4 N 0.2251 0.1373 0.6606 0.050 Uiso 0.13 d P . C4 C 0.2270 0.0861 0.5396 0.050 Uiso 0.13 d P . C5 C 0.1258 0.3187 0.6827 0.050 Uiso 0.13 d P . C6 C 0.1551 0.3497 0.5420 0.050 Uiso 0.13 d P . C7 C 0.2040 0.4157 0.5565 0.050 Uiso 0.13 d P . C8 C 0.3248 0.3598 0.5071 0.050 Uiso 0.13 d P . C9 C 0.3329 0.2800 0.5470 0.050 Uiso 0.13 d P . C10 C 0.3766 0.2174 0.7670 0.050 Uiso 0.13 d P . C11 C 0.3562 0.1382 0.7411 0.050 Uiso 0.13 d P . C12 C 0.2777 0.1183 0.7735 0.050 Uiso 0.13 d P . C13 C 0.1512 0.1486 0.7171 0.050 Uiso 0.13 d P . C14 C 0.1005 0.1904 0.6164 0.050 Uiso 0.13 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 P1 0.0349(2) 0.0223(2) 0.0190(2) 0.0010(2) 0.0033(2) -0.0019(2) O1 0.0846(12) 0.0291(7) 0.0378(7) 0.0129(6) 0.0152(8) 0.0038(8) O2 0.0699(10) 0.0551(9) 0.0236(6) -0.0064(7) 0.0025(7) -0.0147(8) O3 0.0512(9) 0.0437(8) 0.0503(9) -0.0027(7) 0.0064(8) 0.0114(7) O4 0.0475(8) 0.0449(8) 0.0513(9) 0.0023(7) -0.0083(7) -0.0130(7) Al1 0.0358(3) 0.0148(2) 0.0162(2) 0.0019(2) 0.0002(2) -0.0086(2) Zn1 0.0297(5) 0.0287(5) 0.0265(5) -0.0025(4) -0.0020(4) 0.0214(4) P2 0.0224(2) 0.0200(2) 0.0366(2) -0.0042(2) -0.0033(2) 0.0002(2) O5 0.0463(8) 0.0528(9) 0.0436(8) 0.0038(7) -0.0107(7) -0.0039(7) O6 0.0461(8) 0.0432(8) 0.0486(9) -0.0093(7) 0.0040(7) 0.0093(7) O7 0.0308(7) 0.0450(8) 0.0855(13) -0.0097(9) 0.0005(8) -0.0107(7) O8 0.0668(11) 0.0264(7) 0.0698(11) -0.0046(7) -0.0098(9) 0.0118(7) Al2 0.0222(3) 0.0197(3) 0.0244(3) 0.0008(2) -0.0009(2) 0.0008(2) Zn2 0.0171(4) 0.0130(4) 0.0205(4) 0.0014(3) -0.0014(4) 0.0014(3) P3 0.0399(2) 0.0181(2) 0.0204(2) 0.0000(2) -0.0024(2) -0.0035(2) O9 0.0560(9) 0.0568(10) 0.0453(9) -0.0034(8) -0.0187(8) 0.0062(8) O10 0.0499(9) 0.0487(9) 0.0492(9) 0.0060(8) 0.0087(8) -0.0076(8) O11 0.0807(12) 0.0435(8) 0.0277(7) -0.0126(6) 0.0056(8) -0.0088(8) O12 0.0768(12) 0.0251(7) 0.0602(10) 0.0034(7) -0.0126(9) -0.0015(8) Al3 0.0286(3) 0.0343(3) 0.0156(3) -0.0030(2) 0.0046(2) 0.0081(3) Zn3 0.0165(4) 0.0242(4) 0.0218(4) -0.0011(4) -0.0097(3) -0.0092(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 P1 O3 1.509(2) . ? P1 O4 1.512(2) . ? P1 O1 1.516(2) . ? P1 O2 1.525(2) . ? O1 Zn1 1.732(2) . ? O1 Al1 1.737(2) . ? O2 Zn3 1.741(2) 5_566 ? O2 Al3 1.745(2) 5_566 ? O3 Zn2 1.797(2) 8_665 ? O3 Al2 1.800(2) 8_665 ? O4 Zn3 1.763(2) . ? O4 Al3 1.765(2) . ? Al1 O12 1.749(2) . ? Al1 O10 1.753(2) 8_665 ? Al1 O5 1.760(2) . ? Zn1 O5 1.740(2) . ? Zn1 O12 1.762(2) . ? Zn1 O10 1.767(2) 8_665 ? P2 O7 1.507(2) . ? P2 O8 1.508(2) . ? P2 O5 1.521(2) . ? P2 O6 1.525(2) . ? O6 Zn3 1.746(2) 5_565 ? O6 Al3 1.749(2) 5_565 ? O7 Al2 1.772(2) 4_455 ? O7 Zn2 1.775(2) 4_455 ? O8 Al2 1.775(2) . ? O8 Zn2 1.775(2) . ? Al2 O7 1.772(2) 3_565 ? Al2 O9 1.790(2) . ? Al2 O3 1.800(2) 7_565 ? Zn2 O7 1.775(2) 3_565 ? Zn2 O9 1.790(2) . ? Zn2 O3 1.797(2) 7_565 ? P3 O9 1.504(2) . ? P3 O12 1.513(2) . ? P3 O11 1.514(2) . ? P3 O10 1.518(2) . ? O10 Al1 1.753(2) 7_565 ? O10 Zn1 1.767(2) 7_565 ? O11 Al3 1.739(2) 3_565 ? O11 Zn3 1.749(2) 3_565 ? Al3 O11 1.739(2) 4_455 ? Al3 O2 1.745(2) 5_566 ? Al3 O6 1.749(2) 5_565 ? Zn3 O2 1.741(2) 5_566 ? Zn3 O6 1.745(2) 5_565 ? Zn3 O11 1.749(2) 4_455 ? 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 O3 P1 O4 112.22(10) . . ? O3 P1 O1 111.32(10) . . ? O4 P1 O1 107.82(10) . . ? O3 P1 O2 108.12(11) . . ? O4 P1 O2 109.66(10) . . ? O1 P1 O2 107.60(10) . . ? P1 O1 Zn1 149.76(12) . . ? P1 O1 Al1 149.86(11) . . ? Zn1 O1 Al1 0.77(4) . . ? P1 O2 Zn3 145.31(13) . 5_566 ? P1 O2 Al3 145.49(13) . 5_566 ? Zn3 O2 Al3 0.30(4) 5_566 5_566 ? P1 O3 Zn2 143.40(13) . 8_665 ? P1 O3 Al2 143.39(12) . 8_665 ? Zn2 O3 Al2 0.06(4) 8_665 8_665 ? P1 O4 Zn3 148.06(12) . . ? P1 O4 Al3 148.35(12) . . ? Zn3 O4 Al3 0.32(4) . . ? O1 Al1 O12 103.75(9) . . ? O1 Al1 O10 111.20(9) . 8_665 ? O12 Al1 O10 109.31(10) . 8_665 ? O1 Al1 O5 111.47(9) . . ? O12 Al1 O5 110.17(10) . . ? O10 Al1 O5 110.72(9) 8_665 . ? O1 Zn1 O5 112.70(11) . . ? O1 Zn1 O12 103.43(10) . . ? O5 Zn1 O12 110.50(11) . . ? O1 Zn1 O10 110.78(10) . 8_665 ? O5 Zn1 O10 111.00(10) . 8_665 ? O12 Zn1 O10 108.10(11) . 8_665 ? O7 P2 O8 108.45(11) . . ? O7 P2 O5 108.38(11) . . ? O8 P2 O5 110.95(11) . . ? O7 P2 O6 111.28(10) . . ? O8 P2 O6 107.16(11) . . ? O5 P2 O6 110.62(10) . . ? P2 O5 Zn1 145.71(13) . . ? P2 O5 Al1 145.28(12) . . ? Zn1 O5 Al1 0.45(4) . . ? P2 O6 Zn3 145.97(12) . 5_565 ? P2 O6 Al3 145.83(12) . 5_565 ? Zn3 O6 Al3 0.31(4) 5_565 5_565 ? P2 O7 Al2 143.86(12) . 4_455 ? P2 O7 Zn2 143.80(12) . 4_455 ? Al2 O7 Zn2 0.07(3) 4_455 4_455 ? P2 O8 Al2 150.23(14) . . ? P2 O8 Zn2 150.20(14) . . ? Al2 O8 Zn2 0.11(3) . . ? O7 Al2 O8 104.63(9) 3_565 . ? O7 Al2 O9 111.94(10) 3_565 . ? O8 Al2 O9 110.65(10) . . ? O7 Al2 O3 111.16(9) 3_565 7_565 ? O8 Al2 O3 109.35(10) . 7_565 ? O9 Al2 O3 109.04(9) . 7_565 ? O8 Zn2 O7 104.49(10) . 3_565 ? O8 Zn2 O9 110.63(10) . . ? O7 Zn2 O9 111.82(11) 3_565 . ? O8 Zn2 O3 109.45(10) . 7_565 ? O7 Zn2 O3 111.17(10) 3_565 7_565 ? O9 Zn2 O3 109.18(10) . 7_565 ? O9 P3 O12 111.26(11) . . ? O9 P3 O11 109.73(11) . . ? O12 P3 O11 107.04(10) . . ? O9 P3 O10 111.50(10) . . ? O12 P3 O10 106.66(11) . . ? O11 P3 O10 110.52(11) . . ? P3 O9 Zn2 146.56(13) . . ? P3 O9 Al2 146.66(13) . . ? Zn2 O9 Al2 0.11(4) . . ? P3 O10 Al1 143.36(12) . 7_565 ? P3 O10 Zn1 142.75(13) . 7_565 ? Al1 O10 Zn1 0.64(4) 7_565 7_565 ? P3 O11 Al3 146.56(12) . 3_565 ? P3 O11 Zn3 146.59(12) . 3_565 ? Al3 O11 Zn3 0.05(4) 3_565 3_565 ? P3 O12 Al1 150.73(14) . . ? P3 O12 Zn1 150.37(14) . . ? Al1 O12 Zn1 0.66(4) . . ? O11 Al3 O2 106.22(9) 4_455 5_566 ? O11 Al3 O6 111.94(9) 4_455 5_565 ? O2 Al3 O6 108.26(9) 5_566 5_565 ? O11 Al3 O4 109.38(10) 4_455 . ? O2 Al3 O4 109.58(9) 5_566 . ? O6 Al3 O4 111.30(9) 5_565 . ? O2 Zn3 O6 108.61(10) 5_566 5_565 ? O2 Zn3 O11 105.97(10) 5_566 4_455 ? O6 Zn3 O11 111.64(10) 5_565 4_455 ? O2 Zn3 O4 109.87(10) 5_566 . ? O6 Zn3 O4 111.57(10) 5_565 . ? O11 Zn3 O4 109.02(10) 4_455 . ?