Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_nicoapo-sta-7 _database_code_CSD 158125 _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Cox, P.' 'Garcia, Raquel' 'Philp, Eilidh F.' 'Slawin, A.' 'Wright, P.' _publ_contact_author_name 'Dr P Wright' _publ_contact_author_address ; Dr P Wright School of Chemistry St Andrews University The Purdie Building St Andrews Fife KY16 9ST U.K. ; _publ_contact_author_email 'paw2@st-andrews.ac.uk' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'nicoapo-sta7' _chemical_formula_moiety '[C14 H32 N4 Ni]0.25.[O12 P3 Al2.5 Co0.50][H2 O]0.5.[C3 H9 N1]0.1' _chemical_formula_structural 'C3.80 H9.90 Al2.50 Co0.50 N1.10 Ni0.25 O12.50 P3' _chemical_formula_analytical 'C3.80 H9.90 Al2.50 Co0.50 N1.10 Ni0.25 O12.50 P3' _chemical_formula_sum ; 'C3.80 H9.90 Al2.50 Co0.50 N1.10 Ni0.25 O12.50 P3' ; _chemical_formula_weight 475.53 _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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 '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 18.6842(12) _cell_length_b 18.6842(12) _cell_length_c 9.4080(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3284.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 124 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max .1 _exptl_crystal_size_mid .03 _exptl_crystal_size_min .03 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.923 _exptl_crystal_density_method - _exptl_crystal_F_000 1907 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.765298 _exptl_absorpt_correction_T_max 1.00000 _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 CCD _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 13883 _diffrn_reflns_av_R_equivalents 0.1658 _diffrn_reflns_av_sigmaI/netI 0.1101 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 23.20 _reflns_number_total 2355 _reflns_number_observed 1316 _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 2 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^)+(0.1535P)^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 NONE _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_number_reflns 2353 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1563 _refine_ls_R_factor_obs 0.0781 _refine_ls_wR_factor_all 0.2645 _refine_ls_wR_factor_obs 0.1917 _refine_ls_goodness_of_fit_all 1.079 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.081 _refine_ls_shift/esd_max 0.165 _refine_ls_shift/esd_mean 0.016 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 Ni1 Ni 0.2500 0.2500 0.6431(2) 0.0517(5) Uani 1 d S . N1 N 0.3249(4) 0.1754(4) 0.6432(8) 0.109(2) Uiso 1 d . . C1 C 0.3441(9) 0.1519(9) 0.7846(17) 0.153(6) Uiso 0.75 d P . C2 C 0.3004(10) 0.1021(9) 0.5602(18) 0.185(7) Uiso 0.75 d P . C3 C 0.2900(15) 0.1076(15) 0.6928(28) 0.184(11) Uiso 0.50 d P . C4 C 0.2030(10) 0.1091(10) 0.5519(21) 0.124(7) Uiso 0.50 d P . C5 C 0.2376(17) 0.0946(15) 0.6396(29) 0.193(11) Uiso 0.50 d P . C6 C 0.3432(15) 0.1518(15) 0.4809(32) 0.196(11) Uiso 0.50 d P . P1 P 0.06421(7) -0.05660(7) 0.33485(13) 0.0297(4) Uani 1 d . . O1 O 0.0734(2) -0.0812(2) 0.4871(3) 0.0546(13) Uani 1 d . . O2 O 0.0584(2) -0.1232(2) 0.2423(3) 0.0486(12) Uani 1 d . . O3 O 0.1286(2) -0.0112(2) 0.2933(4) 0.0529(13) Uani 1 d . . O4 O -0.0049(2) -0.0151(2) 0.3217(4) 0.0518(13) Uani 1 d . . Al1 Al 0.16453(6) 0.04424(6) 0.15671(11) 0.0212(5) Uani 0.84 d P . Co1 Co 0.16453(6) 0.04424(6) 0.15671(11) 0.0118(10) Uani 0.16 d P . O5 O 0.1553(2) -0.0007(2) -0.0114(4) 0.0535(13) Uani 1 d . . O6 O 0.2560(2) 0.0629(2) 0.1917(4) 0.0592(13) Uani 1 d . . O7 O 0.1217(2) 0.1267(2) 0.1555(4) 0.0531(13) Uani 1 d . . P3 P 0.05057(7) 0.16669(7) 0.16026(14) 0.0337(4) Uani 1 d . . O8 O 0.0140(2) 0.1578(2) 0.0173(4) 0.0466(12) Uani 1 d . . O9 O 0.0048(2) 0.1362(2) 0.2781(3) 0.0445(12) Uani 1 d . . Al2 Al -0.06542(7) 0.16586(6) -0.08060(12) 0.0327(6) Uani 0.83 d P . Co2 Co -0.06542(7) 0.16586(6) -0.08060(12) 0.0226(11) Uani 0.17 d P . O10 O -0.1376(2) 0.1335(2) 0.0173(4) 0.0521(13) Uani 1 d . . O11 O -0.0806(2) 0.2554(2) -0.1228(4) 0.0564(13) Uani 1 d . . P5 P -0.16652(7) 0.06778(7) 0.09574(13) 0.0290(4) Uani 1 d . . O12 O -0.1297(2) 0.0601(2) 0.2395(4) 0.0492(12) Uani 1 d . . Al3 Al -0.05063(6) 0.06639(7) 0.33547(12) 0.0315(6) Uani 0.83 d P . Co3 Co -0.05063(6) 0.06639(7) 0.33547(12) 0.0217(11) Uani 0.17 d P . O20 O 0.1210(12) -0.2502(13) 0.4968(24) 0.114(8) Uiso 0.25 d P . O30 O 0.2176(19) 0.2715(29) 1.0020(36) 0.134(17) Uiso 0.15 d P . O40 O 0.2393(37) 0.2481(208) 1.2806(31) 0.106(12) Uiso 0.10 d P . C50 C 0.2500 -0.2500 0.5000 0.176(24) Uiso 0.40 d SP . N51 N 0.2500 -0.2500 0.6325(55) 0.124(18) Uiso 0.20 d SP . C52 C 0.1869(27) -0.2487(29) 0.7019(52) 0.133(18) 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 Ni1 0.0510(6) 0.0510(6) 0.0529(9) 0.000 0.000 0.000 P1 0.0415(8) 0.0240(7) 0.0235(6) 0.0014(6) 0.0047(6) 0.0013(6) O1 0.069(3) 0.070(3) 0.025(2) 0.004(2) 0.007(2) 0.018(2) O2 0.073(3) 0.035(2) 0.038(2) -0.017(2) 0.012(2) -0.002(2) O3 0.059(2) 0.043(2) 0.057(2) 0.006(2) 0.010(2) -0.012(2) O4 0.053(2) 0.050(2) 0.052(2) -0.003(2) -0.013(2) 0.016(2) Al1 0.0162(8) 0.0218(8) 0.0256(8) -0.0002(8) 0.0017(8) 0.0010(7) Co1 0.002(2) 0.013(2) 0.020(2) 0.001(2) 0.003(2) 0.001(2) O5 0.055(2) 0.058(2) 0.048(2) -0.017(2) 0.004(2) 0.006(2) O6 0.031(2) 0.066(3) 0.080(3) -0.021(2) -0.007(2) 0.020(2) O7 0.025(2) 0.064(2) 0.070(3) 0.019(2) 0.002(2) 0.008(2) P3 0.0287(7) 0.0284(7) 0.0439(8) 0.0060(7) -0.0009(7) -0.0022(6) O8 0.043(2) 0.051(2) 0.046(2) -0.011(2) -0.015(2) 0.001(2) O9 0.054(2) 0.046(2) 0.033(2) 0.004(2) 0.006(2) -0.005(2) Al2 0.0400(10) 0.0290(10) 0.0290(10) -0.0008(9) -0.0005(9) -0.0037(9) Co2 0.038(2) 0.016(2) 0.015(2) 0.000(2) -0.001(2) -0.009(2) O10 0.050(2) 0.056(2) 0.051(2) 0.004(2) 0.006(2) -0.013(2) O11 0.086(3) 0.031(2) 0.052(2) -0.006(2) -0.003(2) 0.002(2) P5 0.0224(6) 0.0427(8) 0.0218(6) -0.0021(6) 0.0013(6) -0.0038(6) O12 0.047(2) 0.066(3) 0.034(2) 0.002(2) -0.013(2) -0.013(2) Al3 0.0308(10) 0.0380(11) 0.0259(9) 0.0015(9) 0.0001(9) 0.0007(9) Co3 0.020(2) 0.034(2) 0.011(2) 0.006(2) 0.000(2) 0.000(2) _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 Ni1 N1 1.975(7) 3 ? Ni1 N1 1.975(7) 2 ? Ni1 N1 1.975(7) 4 ? Ni1 N1 1.975(7) . ? N1 C1 1.45(2) . ? N1 C3 1.50(3) . ? N1 C4 1.59(2) 3 ? N1 C6 1.63(3) . ? N1 C2 1.64(2) . ? N1 C5 1.90(3) 3 ? C1 C3 1.57(3) . ? C2 C3 1.27(3) . ? C2 C5 1.40(3) . ? C2 C6 1.43(3) . ? C2 C4 1.83(3) . ? C3 C5 1.13(4) . ? C4 C5 1.08(3) . ? C4 C6 1.47(3) 4 ? C4 N1 1.59(2) 4 ? C5 N1 1.90(3) 4 ? C6 C4 1.47(3) 3 ? P1 O4 1.512(4) . ? P1 O1 1.514(4) . ? P1 O3 1.523(4) . ? P1 O2 1.523(4) . ? O1 Co3 1.745(3) 5_556 ? O1 Al3 1.745(3) 5_556 ? O2 Co2 1.722(3) 5 ? O2 Al2 1.722(3) 5 ? O3 Co1 1.782(4) . ? O3 Al1 1.782(4) . ? O4 Co3 1.751(4) . ? O4 Al3 1.751(4) . ? Al1 O7 1.736(4) . ? Al1 O6 1.775(4) . ? Al1 O5 1.799(4) . ? Co1 O7 1.736(4) . ? Co1 O6 1.775(4) . ? Co1 O5 1.799(4) . ? O5 P5 1.498(4) 5 ? O6 P3 1.492(4) 3 ? O7 P3 1.525(4) . ? P3 O6 1.492(4) 4 ? P3 O9 1.512(4) . ? P3 O8 1.518(4) . ? O8 Co2 1.753(4) . ? O8 Al2 1.753(4) . ? O9 Co3 1.751(4) . ? O9 Al3 1.751(4) . ? Al2 O2 1.722(3) 5 ? Al2 O10 1.741(4) . ? Al2 O11 1.743(4) . ? Co2 O2 1.722(3) 5 ? Co2 O10 1.741(4) . ? Co2 O11 1.743(4) . ? O10 P5 1.531(4) . ? O11 P5 1.500(4) 8_565 ? P5 O5 1.498(4) 5 ? P5 O11 1.500(4) 7 ? P5 O12 1.525(4) . ? O12 Co3 1.735(4) . ? O12 Al3 1.735(4) . ? Al3 O1 1.745(3) 5_556 ? Co3 O1 1.745(3) 5_556 ? O30 O30 1.03(6) 4 ? O30 O30 1.03(6) 3 ? O30 O30 1.45(8) 2 ? C50 N51 1.25(5) . ? C50 N51 1.25(5) 7_656 ? N51 C52 1.35(6) 2_545 ? N51 C52 1.35(6) . ? 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 N1 Ni1 N1 90.001(1) 3 2 ? N1 Ni1 N1 179.9(4) 3 4 ? N1 Ni1 N1 89.999(2) 2 4 ? N1 Ni1 N1 89.999(2) 3 . ? N1 Ni1 N1 179.9(4) 2 . ? N1 Ni1 N1 90.0 4 . ? C1 N1 C3 64.2(12) . . ? C1 N1 C4 113.8(11) . 3 ? C3 N1 C4 141.3(14) . 3 ? C1 N1 C6 136.9(13) . . ? C3 N1 C6 98.9(15) . . ? C4 N1 C6 54.3(12) 3 . ? C1 N1 C2 104.7(10) . . ? C3 N1 C2 47.3(12) . . ? C4 N1 C2 103.3(10) 3 . ? C6 N1 C2 52.1(12) . . ? C1 N1 C5 90.4(11) . 3 ? C3 N1 C5 150.1(14) . 3 ? C4 N1 C5 34.7(11) 3 3 ? C6 N1 C5 89.0(13) . 3 ? C2 N1 C5 136.2(12) . 3 ? C1 N1 Ni1 113.0(8) . . ? C3 N1 Ni1 106.7(12) . . ? C4 N1 Ni1 108.7(8) 3 . ? C6 N1 Ni1 109.8(11) . . ? C2 N1 Ni1 113.0(7) . . ? C5 N1 Ni1 97.4(10) 3 . ? N1 C1 C3 59.6(12) . . ? C3 C2 C5 49.6(18) . . ? C3 C2 C6 123.1(22) . . ? C5 C2 C6 144.1(22) . . ? C3 C2 N1 60.5(15) . . ? C5 C2 N1 93.6(15) . . ? C6 C2 N1 63.4(14) . . ? C3 C2 C4 83.3(17) . . ? C5 C2 C4 36.2(14) . . ? C6 C2 C4 119.1(17) . . ? N1 C2 C4 103.8(11) . . ? C5 C3 C2 71.3(22) . . ? C5 C3 N1 114.9(26) . . ? C2 C3 N1 72.2(16) . . ? C5 C3 C1 156.9(30) . . ? C2 C3 C1 119.0(23) . . ? N1 C3 C1 56.2(12) . . ? C5 C4 C6 152.6(26) . 4 ? C5 C4 N1 88.6(20) . 4 ? C6 C4 N1 64.1(14) 4 4 ? C5 C4 C2 49.8(18) . . ? C6 C4 C2 135.4(18) 4 . ? N1 C4 C2 110.9(12) 4 . ? C4 C5 C3 143.5(34) . . ? C4 C5 C2 93.9(23) . . ? C3 C5 C2 59.1(21) . . ? C4 C5 N1 56.7(17) . 4 ? C3 C5 N1 110.7(25) . 4 ? C2 C5 N1 116.4(19) . 4 ? C2 C6 C4 121.6(23) . 3 ? C2 C6 N1 64.5(14) . . ? C4 C6 N1 61.5(14) 3 . ? O4 P1 O1 109.3(2) . . ? O4 P1 O3 111.7(2) . . ? O1 P1 O3 108.8(2) . . ? O4 P1 O2 108.1(2) . . ? O1 P1 O2 107.5(2) . . ? O3 P1 O2 111.4(2) . . ? P1 O1 Co3 146.0(3) . 5_556 ? P1 O1 Al3 146.0(3) . 5_556 ? Co3 O1 Al3 0.00(11) 5_556 5_556 ? P1 O2 Co2 151.4(2) . 5 ? P1 O2 Al2 151.4(2) . 5 ? Co2 O2 Al2 0.00(11) 5 5 ? P1 O3 Co1 143.7(3) . . ? P1 O3 Al1 143.7(3) . . ? Co1 O3 Al1 0.00(10) . . ? P1 O4 Co3 148.9(3) . . ? P1 O4 Al3 148.9(3) . . ? Co3 O4 Al3 0.00(11) . . ? O7 Al1 O6 105.7(2) . . ? O7 Al1 O3 110.3(2) . . ? O6 Al1 O3 110.0(2) . . ? O7 Al1 O5 111.4(2) . . ? O6 Al1 O5 110.3(2) . . ? O3 Al1 O5 109.1(2) . . ? O7 Co1 O6 105.7(2) . . ? O7 Co1 O3 110.3(2) . . ? O6 Co1 O3 110.0(2) . . ? O7 Co1 O5 111.4(2) . . ? O6 Co1 O5 110.3(2) . . ? O3 Co1 O5 109.1(2) . . ? P5 O5 Al1 147.5(3) 5 . ? P5 O5 Co1 147.5(3) 5 . ? Al1 O5 Co1 0.00(9) . . ? P3 O6 Al1 149.9(3) 3 . ? P3 O6 Co1 149.9(3) 3 . ? Al1 O6 Co1 0.00(10) . . ? P3 O7 Al1 146.7(3) . . ? P3 O7 Co1 146.7(3) . . ? Al1 O7 Co1 0.00(10) . . ? O6 P3 O9 107.9(2) 4 . ? O6 P3 O8 110.6(2) 4 . ? O9 P3 O8 110.8(2) . . ? O6 P3 O7 110.2(2) 4 . ? O9 P3 O7 109.2(2) . . ? O8 P3 O7 108.2(2) . . ? P3 O8 Co2 146.9(2) . . ? P3 O8 Al2 146.9(2) . . ? Co2 O8 Al2 0.00(11) . . ? P3 O9 Co3 147.3(2) . . ? P3 O9 Al3 147.3(2) . . ? Co3 O9 Al3 0.00(11) . . ? O2 Al2 O10 111.4(2) 5 . ? O2 Al2 O11 104.8(2) 5 . ? O10 Al2 O11 109.1(2) . . ? O2 Al2 O8 111.1(2) 5 . ? O10 Al2 O8 110.4(2) . . ? O11 Al2 O8 109.9(2) . . ? O2 Co2 O10 111.4(2) 5 . ? O2 Co2 O11 104.8(2) 5 . ? O10 Co2 O11 109.1(2) . . ? O2 Co2 O8 111.1(2) 5 . ? O10 Co2 O8 110.4(2) . . ? O11 Co2 O8 109.9(2) . . ? P5 O10 Al2 143.8(3) . . ? P5 O10 Co2 143.8(3) . . ? Al2 O10 Co2 0.00(11) . . ? P5 O11 Al2 150.3(3) 8_565 . ? P5 O11 Co2 150.3(3) 8_565 . ? Al2 O11 Co2 0.00(11) . . ? O5 P5 O11 111.1(2) 5 7 ? O5 P5 O12 109.1(2) 5 . ? O11 P5 O12 107.7(2) 7 . ? O5 P5 O10 111.5(2) 5 . ? O11 P5 O10 107.3(2) 7 . ? O12 P5 O10 110.1(2) . . ? P5 O12 Co3 147.1(2) . . ? P5 O12 Al3 147.1(2) . . ? Co3 O12 Al3 0.00(11) . . ? O12 Al3 O1 107.5(2) . 5_556 ? O12 Al3 O4 108.5(2) . . ? O1 Al3 O4 109.1(2) 5_556 . ? O12 Al3 O9 113.2(2) . . ? O1 Al3 O9 108.8(2) 5_556 . ? O4 Al3 O9 109.7(2) . . ? O12 Co3 O1 107.5(2) . 5_556 ? O12 Co3 O4 108.5(2) . . ? O1 Co3 O4 109.1(2) 5_556 . ? O12 Co3 O9 113.2(2) . . ? O1 Co3 O9 108.8(2) 5_556 . ? O4 Co3 O9 109.7(2) . . ? O30 O30 O30 90.001(9) 4 3 ? O30 O30 O30 45.000(8) 4 2 ? O30 O30 O30 45.000(13) 3 2 ? 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 N1 Ni1 N1 C1 92.5(8) 3 . . . ? N1 Ni1 N1 C1 2.3(1000) 2 . . . ? N1 Ni1 N1 C1 -87.4(8) 4 . . . ? N1 Ni1 N1 C3 161.0(11) 3 . . . ? N1 Ni1 N1 C3 70.8(1000) 2 . . . ? N1 Ni1 N1 C3 -18.9(12) 4 . . . ? N1 Ni1 N1 C4 -34.9(9) 3 . . 3 ? N1 Ni1 N1 C4 -125.1(1000) 2 . . 3 ? N1 Ni1 N1 C4 145.2(8) 4 . . 3 ? N1 Ni1 N1 C6 -92.7(11) 3 . . . ? N1 Ni1 N1 C6 177.1(1000) 2 . . . ? N1 Ni1 N1 C6 87.4(11) 4 . . . ? N1 Ni1 N1 C2 -148.9(7) 3 . . . ? N1 Ni1 N1 C2 120.9(1000) 2 . . . ? N1 Ni1 N1 C2 31.2(9) 4 . . . ? N1 Ni1 N1 C5 -1.1(10) 3 . . 3 ? N1 Ni1 N1 C5 -91.3(1000) 2 . . 3 ? N1 Ni1 N1 C5 179.0(8) 4 . . 3 ? C3 N1 C1 C3 0.000(2) . . . . ? C4 N1 C1 C3 -137.2(15) 3 . . . ? C6 N1 C1 C3 -74.7(22) . . . . ? C2 N1 C1 C3 -25.2(15) . . . . ? C5 N1 C1 C3 -163.6(16) 3 . . . ? Ni1 N1 C1 C3 98.2(13) . . . . ? C1 N1 C2 C3 31.4(18) . . . . ? C3 N1 C2 C3 0.000(4) . . . . ? C4 N1 C2 C3 150.8(18) 3 . . . ? C6 N1 C2 C3 170.2(23) . . . . ? C5 N1 C2 C3 137.9(21) 3 . . . ? Ni1 N1 C2 C3 -91.9(17) . . . . ? C1 N1 C2 C5 70.1(17) . . . . ? C3 N1 C2 C5 38.6(19) . . . . ? C4 N1 C2 C5 -170.5(16) 3 . . . ? C6 N1 C2 C5 -151.2(22) . . . . ? C5 N1 C2 C5 176.5(21) 3 . . . ? Ni1 N1 C2 C5 -53.3(16) . . . . ? C1 N1 C2 C6 -138.8(16) . . . . ? C3 N1 C2 C6 -170.2(23) . . . . ? C4 N1 C2 C6 -19.4(16) 3 . . . ? C6 N1 C2 C6 0.000(3) . . . . ? C5 N1 C2 C6 -32.4(22) 3 . . . ? Ni1 N1 C2 C6 97.8(14) . . . . ? C1 N1 C2 C4 105.3(12) . . . . ? C3 N1 C2 C4 73.9(18) . . . . ? C4 N1 C2 C4 -135.3(15) 3 . . . ? C6 N1 C2 C4 -115.9(18) . . . . ? C5 N1 C2 C4 -148.3(15) 3 . . . ? Ni1 N1 C2 C4 -18.1(12) . . . . ? C5 C2 C3 C5 0.000(5) . . . . ? C6 C2 C3 C5 135.6(27) . . . . ? N1 C2 C3 C5 125.2(24) . . . . ? C4 C2 C3 C5 15.1(20) . . . . ? C5 C2 C3 N1 -125.2(23) . . . . ? C6 C2 C3 N1 10.4(24) . . . . ? N1 C2 C3 N1 0.000(3) . . . . ? C4 C2 C3 N1 -110.0(12) . . . . ? C5 C2 C3 C1 -157.4(35) . . . . ? C6 C2 C3 C1 -21.7(36) . . . . ? N1 C2 C3 C1 -32.2(17) . . . . ? C4 C2 C3 C1 -142.2(22) . . . . ? C1 N1 C3 C5 155.5(31) . . . . ? C4 N1 C3 C5 -107.9(30) 3 . . . ? C6 N1 C3 C5 -66.4(29) . . . . ? C2 N1 C3 C5 -58.6(25) . . . . ? C5 N1 C3 C5 -170.1(30) 3 . . . ? Ni1 N1 C3 C5 47.5(28) . . . . ? C1 N1 C3 C2 -145.9(19) . . . . ? C4 N1 C3 C2 -49.3(27) 3 . . . ? C6 N1 C3 C2 -7.8(18) . . . . ? C2 N1 C3 C2 0.000(3) . . . . ? C5 N1 C3 C2 -111.5(27) 3 . . . ? Ni1 N1 C3 C2 106.1(14) . . . . ? C1 N1 C3 C1 0.000(2) . . . . ? C4 N1 C3 C1 96.6(20) 3 . . . ? C6 N1 C3 C1 138.1(14) . . . . ? C2 N1 C3 C1 145.9(19) . . . . ? C5 N1 C3 C1 34.4(30) 3 . . . ? Ni1 N1 C3 C1 -108.0(10) . . . . ? N1 C1 C3 C5 -73.9(71) . . . . ? N1 C1 C3 C2 37.6(20) . . . . ? N1 C1 C3 N1 0.000(2) . . . . ? C3 C2 C4 C5 -19.7(26) . . . . ? C5 C2 C4 C5 0.000(7) . . . . ? C6 C2 C4 C5 -144.0(29) . . . . ? N1 C2 C4 C5 -77.0(23) . . . . ? C3 C2 C4 C6 123.3(28) . . . 4 ? C5 C2 C4 C6 143.0(36) . . . 4 ? C6 C2 C4 C6 -1.0(29) . . . 4 ? N1 C2 C4 C6 65.9(27) . . . 4 ? C3 C2 C4 N1 49.4(19) . . . 4 ? C5 C2 C4 N1 69.1(23) . . . 4 ? C6 C2 C4 N1 -74.9(22) . . . 4 ? N1 C2 C4 N1 -7.9(15) . . . 4 ? C6 C4 C5 C3 -74.1(85) 4 . . . ? N1 C4 C5 C3 -79.8(55) 4 . . . ? C2 C4 C5 C3 39.3(48) . . . . ? C6 C4 C5 C2 -113.4(53) 4 . . . ? N1 C4 C5 C2 -119.2(16) 4 . . . ? C2 C4 C5 C2 0.000(4) . . . . ? C6 C4 C5 N1 5.7(50) 4 . . 4 ? N1 C4 C5 N1 0.000(6) 4 . . 4 ? C2 C4 C5 N1 119.2(16) . . . 4 ? C2 C3 C5 C4 -47.5(55) . . . . ? N1 C3 C5 C4 11.6(68) . . . . ? C1 C3 C5 C4 73.3(96) . . . . ? C2 C3 C5 C2 0.000(3) . . . . ? N1 C3 C5 C2 59.1(21) . . . . ? C1 C3 C5 C2 120.8(73) . . . . ? C2 C3 C5 N1 -109.1(21) . . . 4 ? N1 C3 C5 N1 -50.0(30) . . . 4 ? C1 C3 C5 N1 11.7(82) . . . 4 ? C3 C2 C5 C4 154.0(33) . . . . ? C6 C2 C5 C4 61.2(43) . . . . ? N1 C2 C5 C4 108.5(20) . . . . ? C4 C2 C5 C4 0.000(5) . . . . ? C3 C2 C5 C3 0.000(6) . . . . ? C6 C2 C5 C3 -92.8(40) . . . . ? N1 C2 C5 C3 -45.5(21) . . . . ? C4 C2 C5 C3 -154.0(33) . . . . ? C3 C2 C5 N1 99.4(27) . . . 4 ? C6 C2 C5 N1 6.6(46) . . . 4 ? N1 C2 C5 N1 54.0(19) . . . 4 ? C4 C2 C5 N1 -54.5(18) . . . 4 ? C3 C2 C6 C4 14.0(38) . . . 3 ? C5 C2 C6 C4 79.4(43) . . . 3 ? N1 C2 C6 C4 24.2(20) . . . 3 ? C4 C2 C6 C4 115.7(25) . . . 3 ? C3 C2 C6 N1 -10.2(23) . . . . ? C5 C2 C6 N1 55.2(35) . . . . ? N1 C2 C6 N1 0.000(2) . . . . ? C4 C2 C6 N1 91.5(16) . . . . ? C1 N1 C6 C2 68.8(21) . . . . ? C3 N1 C6 C2 7.3(17) . . . . ? C4 N1 C6 C2 156.6(19) 3 . . . ? C2 N1 C6 C2 0.000(2) . . . . ? C5 N1 C6 C2 158.3(15) 3 . . . ? Ni1 N1 C6 C2 -104.2(12) . . . . ? C1 N1 C6 C4 -87.8(20) . . . 3 ? C3 N1 C6 C4 -149.3(16) . . . 3 ? C4 N1 C6 C4 0.000(1) 3 . . 3 ? C2 N1 C6 C4 -156.6(19) . . . 3 ? C5 N1 C6 C4 1.7(15) 3 . . 3 ? Ni1 N1 C6 C4 99.2(12) . . . 3 ? O4 P1 O1 Co3 -23.0(5) . . . 5_556 ? O3 P1 O1 Co3 99.1(5) . . . 5_556 ? O2 P1 O1 Co3 -140.1(4) . . . 5_556 ? O4 P1 O1 Al3 -23.0(5) . . . 5_556 ? O3 P1 O1 Al3 99.1(5) . . . 5_556 ? O2 P1 O1 Al3 -140.1(4) . . . 5_556 ? O4 P1 O2 Co2 84.6(6) . . . 5 ? O1 P1 O2 Co2 -157.5(5) . . . 5 ? O3 P1 O2 Co2 -38.4(6) . . . 5 ? O4 P1 O2 Al2 84.6(6) . . . 5 ? O1 P1 O2 Al2 -157.5(5) . . . 5 ? O3 P1 O2 Al2 -38.4(6) . . . 5 ? O4 P1 O3 Co1 -52.8(5) . . . . ? O1 P1 O3 Co1 -173.4(4) . . . . ? O2 P1 O3 Co1 68.2(5) . . . . ? O4 P1 O3 Al1 -52.8(5) . . . . ? O1 P1 O3 Al1 -173.4(4) . . . . ? O2 P1 O3 Al1 68.2(5) . . . . ? O1 P1 O4 Co3 86.1(5) . . . . ? O3 P1 O4 Co3 -34.3(6) . . . . ? O2 P1 O4 Co3 -157.1(5) . . . . ? O1 P1 O4 Al3 86.1(5) . . . . ? O3 P1 O4 Al3 -34.3(6) . . . . ? O2 P1 O4 Al3 -157.1(5) . . . . ? P1 O3 Al1 O7 74.5(4) . . . . ? Co1 O3 Al1 O7 0.0(1000) . . . . ? P1 O3 Al1 O6 -169.3(4) . . . . ? Co1 O3 Al1 O6 0.0(1000) . . . . ? P1 O3 Al1 O5 -48.2(5) . . . . ? Co1 O3 Al1 O5 0.0(1000) . . . . ? P1 O3 Co1 O7 74.5(4) . . . . ? Al1 O3 Co1 O7 0.0(1000) . . . . ? P1 O3 Co1 O6 -169.3(4) . . . . ? Al1 O3 Co1 O6 0.0(1000) . . . . ? P1 O3 Co1 O5 -48.2(5) . . . . ? Al1 O3 Co1 O5 0.0(1000) . . . . ? O7 Al1 O5 P5 -171.9(4) . . . 5 ? O6 Al1 O5 P5 71.0(5) . . . 5 ? O3 Al1 O5 P5 -49.9(5) . . . 5 ? O7 Al1 O5 Co1 0.0(1000) . . . . ? O6 Al1 O5 Co1 0.0(646) . . . . ? O3 Al1 O5 Co1 0.0(1000) . . . . ? O7 Co1 O5 P5 -171.9(4) . . . 5 ? O6 Co1 O5 P5 71.0(5) . . . 5 ? O3 Co1 O5 P5 -49.9(5) . . . 5 ? O7 Co1 O5 Al1 0.0(1000) . . . . ? O6 Co1 O5 Al1 0.0(646) . . . . ? O3 Co1 O5 Al1 0.0(1000) . . . . ? O7 Al1 O6 P3 -135.9(5) . . . 3 ? O3 Al1 O6 P3 104.9(6) . . . 3 ? O5 Al1 O6 P3 -15.4(6) . . . 3 ? O7 Al1 O6 Co1 0.0(727) . . . . ? O3 Al1 O6 Co1 0.0(1000) . . . . ? O5 Al1 O6 Co1 0.0(1000) . . . . ? O7 Co1 O6 P3 -135.9(5) . . . 3 ? O3 Co1 O6 P3 104.9(6) . . . 3 ? O5 Co1 O6 P3 -15.4(6) . . . 3 ? O7 Co1 O6 Al1 0.0(727) . . . . ? O3 Co1 O6 Al1 0.0(1000) . . . . ? O5 Co1 O6 Al1 0.0(1000) . . . . ? O6 Al1 O7 P3 -165.3(5) . . . . ? O3 Al1 O7 P3 -46.4(5) . . . . ? O5 Al1 O7 P3 74.9(5) . . . . ? O6 Al1 O7 Co1 0.0(573) . . . . ? O3 Al1 O7 Co1 0.0(1000) . . . . ? O5 Al1 O7 Co1 0.0(1000) . . . . ? O6 Co1 O7 P3 -165.3(5) . . . . ? O3 Co1 O7 P3 -46.4(5) . . . . ? O5 Co1 O7 P3 74.9(5) . . . . ? O6 Co1 O7 Al1 0.0(573) . . . . ? O3 Co1 O7 Al1 0.0(1000) . . . . ? O5 Co1 O7 Al1 0.0(1000) . . . . ? Al1 O7 P3 O6 165.2(4) . . . 4 ? Co1 O7 P3 O6 165.2(4) . . . 4 ? Al1 O7 P3 O9 46.8(5) . . . . ? Co1 O7 P3 O9 46.8(5) . . . . ? Al1 O7 P3 O8 -73.8(5) . . . . ? Co1 O7 P3 O8 -73.8(5) . . . . ? O6 P3 O8 Co2 -73.8(5) 4 . . . ? O9 P3 O8 Co2 45.7(5) . . . . ? O7 P3 O8 Co2 165.4(4) . . . . ? O6 P3 O8 Al2 -73.8(5) 4 . . . ? O9 P3 O8 Al2 45.7(5) . . . . ? O7 P3 O8 Al2 165.4(4) . . . . ? O6 P3 O9 Co3 163.4(4) 4 . . . ? O8 P3 O9 Co3 42.3(5) . . . . ? O7 P3 O9 Co3 -76.8(5) . . . . ? O6 P3 O9 Al3 163.4(4) 4 . . . ? O8 P3 O9 Al3 42.3(5) . . . . ? O7 P3 O9 Al3 -76.8(5) . . . . ? P3 O8 Al2 O2 -167.4(4) . . . 5 ? Co2 O8 Al2 O2 0.0(1000) . . . 5 ? P3 O8 Al2 O10 -43.3(5) . . . . ? Co2 O8 Al2 O10 0.0(1000) . . . . ? P3 O8 Al2 O11 77.1(5) . . . . ? Co2 O8 Al2 O11 0.0(1000) . . . . ? P3 O8 Co2 O2 -167.4(4) . . . 5 ? Al2 O8 Co2 O2 0.0(1000) . . . 5 ? P3 O8 Co2 O10 -43.3(5) . . . . ? Al2 O8 Co2 O10 0.0(1000) . . . . ? P3 O8 Co2 O11 77.1(5) . . . . ? Al2 O8 Co2 O11 0.0(1000) . . . . ? O2 Al2 O10 P5 67.2(5) 5 . . . ? O11 Al2 O10 P5 -177.5(4) . . . . ? O8 Al2 O10 P5 -56.7(5) . . . . ? O2 Al2 O10 Co2 0.0(1000) 5 . . . ? O11 Al2 O10 Co2 0.0(1000) . . . . ? O8 Al2 O10 Co2 0.0(1000) . . . . ? O2 Co2 O10 P5 67.2(5) 5 . . . ? O11 Co2 O10 P5 -177.5(4) . . . . ? O8 Co2 O10 P5 -56.7(5) . . . . ? O2 Co2 O10 Al2 0.0(1000) 5 . . . ? O11 Co2 O10 Al2 0.0(1000) . . . . ? O8 Co2 O10 Al2 0.0(1000) . . . . ? O2 Al2 O11 P5 -139.8(5) 5 . . 8_565 ? O10 Al2 O11 P5 100.7(6) . . . 8_565 ? O8 Al2 O11 P5 -20.4(6) . . . 8_565 ? O2 Al2 O11 Co2 0.0(1000) 5 . . . ? O10 Al2 O11 Co2 0.0(1000) . . . . ? O8 Al2 O11 Co2 0.0(908) . . . . ? O2 Co2 O11 P5 -139.8(5) 5 . . 8_565 ? O10 Co2 O11 P5 100.7(6) . . . 8_565 ? O8 Co2 O11 P5 -20.4(6) . . . 8_565 ? O2 Co2 O11 Al2 0.0(1000) 5 . . . ? O10 Co2 O11 Al2 0.0(1000) . . . . ? O8 Co2 O11 Al2 0.0(908) . . . . ? Al2 O10 P5 O5 -44.4(5) . . . 5 ? Co2 O10 P5 O5 -44.4(5) . . . 5 ? Al2 O10 P5 O11 -166.1(4) . . . 7 ? Co2 O10 P5 O11 -166.1(4) . . . 7 ? Al2 O10 P5 O12 76.9(5) . . . . ? Co2 O10 P5 O12 76.9(5) . . . . ? O5 P5 O12 Co3 83.2(5) 5 . . . ? O11 P5 O12 Co3 -156.2(4) 7 . . . ? O10 P5 O12 Co3 -39.5(5) . . . . ? O5 P5 O12 Al3 83.2(5) 5 . . . ? O11 P5 O12 Al3 -156.2(4) 7 . . . ? O10 P5 O12 Al3 -39.5(5) . . . . ? P5 O12 Al3 O1 155.4(5) . . . 5_556 ? Co3 O12 Al3 O1 0.0(1000) . . . 5_556 ? P5 O12 Al3 O4 -86.7(5) . . . . ? Co3 O12 Al3 O4 0.0(1000) . . . . ? P5 O12 Al3 O9 35.2(5) . . . . ? Co3 O12 Al3 O9 0.0(1000) . . . . ? P1 O4 Al3 O12 161.3(5) . . . . ? Co3 O4 Al3 O12 0.0(874) . . . . ? P1 O4 Al3 O1 -81.9(5) . . . 5_556 ? Co3 O4 Al3 O1 0.0(1000) . . . 5_556 ? P1 O4 Al3 O9 37.1(5) . . . . ? Co3 O4 Al3 O9 0.0(1000) . . . . ? P3 O9 Al3 O12 -65.4(5) . . . . ? Co3 O9 Al3 O12 0.0(563) . . . . ? P3 O9 Al3 O1 175.2(4) . . . 5_556 ? Co3 O9 Al3 O1 0.0(1000) . . . 5_556 ? P3 O9 Al3 O4 56.0(5) . . . . ? Co3 O9 Al3 O4 0.0(1000) . . . . ? P5 O12 Co3 O1 155.4(5) . . . 5_556 ? Al3 O12 Co3 O1 0.0(1000) . . . 5_556 ? P5 O12 Co3 O4 -86.7(5) . . . . ? Al3 O12 Co3 O4 0.0(1000) . . . . ? P5 O12 Co3 O9 35.2(5) . . . . ? Al3 O12 Co3 O9 0.0(1000) . . . . ? P1 O4 Co3 O12 161.3(5) . . . . ? Al3 O4 Co3 O12 0.0(874) . . . . ? P1 O4 Co3 O1 -81.9(5) . . . 5_556 ? Al3 O4 Co3 O1 0.0(1000) . . . 5_556 ? P1 O4 Co3 O9 37.1(5) . . . . ? Al3 O4 Co3 O9 0.0(1000) . . . . ? P3 O9 Co3 O12 -65.4(5) . . . . ? Al3 O9 Co3 O12 0.0(563) . . . . ? P3 O9 Co3 O1 175.2(4) . . . 5_556 ? Al3 O9 Co3 O1 0.0(1000) . . . 5_556 ? P3 O9 Co3 O4 56.0(5) . . . . ? Al3 O9 Co3 O4 0.0(1000) . . . . ? _refine_diff_density_max 1.341 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.304