# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/228 data_MgAlPO-18 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Apr 20 16:14:42 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'LS refinement (W.Clegg)' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 13.795(3) _cell_length_b 12.830(3) _cell_length_c 18.815(5) _cell_angle_alpha 90 _cell_angle_beta 89.959(7) _cell_angle_gamma 90 _cell_volume 3330(1) _cell_formula_units_Z 24 _cell_measurement_temperature 150 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, +y,1/2-z' ' -x, -y, -z' ' -x, -y, -z' ' +x, -y,1/2+z' ' +x, -y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.035 _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_meas ? _chemical_formula_weight 139.47 _chemical_formula_analytical ? _chemical_formula_sum 'C1.05 Al N0.35 O4 P ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1650.00 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_temperature 150 _diffrn_radiation_wavelength 0.6942 _diffrn_radiation_type 'Monochromated X-ray synchrotron radiation' _diffrn_radiation_source 'synchrotron' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'SMART CCD' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 11252 _reflns_number_total 4501 _reflns_number_observed 2535 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 4.99 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 29.86 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al 0 24 0.064 0.051 'International Tables' P 0 24 0.102 0.094 'International Tables' O 0 96 0.011 0.006 'International Tables' C 0 25 0.003 0.002 'International Tables' N 0 8 0.006 0.003 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom P(1) 0.7722(2) 0.0963(2) 0.0554(1) 0.0171(5) Uij ? ? P(2) 0.1113(1) 0.2324(2) 0.9382(1) 0.0177(5) Uij ? ? P(3) 0.1187(1) 0.9643(2) 0.1667(1) 0.0173(5) Uij ? ? Al(1) 0.8895(2) 0.9596(2) 0.1655(1) 0.0165(6) Uij ? ? Al(2) 0.8828(2) 0.2254(2) 0.9385(1) 0.0179(6) Uij ? ? Al(3) 0.2267(2) 0.0961(2) 0.0495(1) 0.0181(6) Uij ? ? O(1) 0.1803(5) 0.0474(6) 0.1306(4) 0.037(2) Uij ? ? O(2) 0.1405(5) 0.1760(6) 0.0061(4) 0.034(2) Uij ? ? O(3) 0.0053(4) 0.2615(5) 0.9422(4) 0.036(2) Uij ? ? O(4) 0.8466(5) 0.1647(6) 0.0178(4) 0.036(2) Uij ? ? O(5) 0.8168(5) 0.0538(5) 0.1236(3) 0.034(2) Uij ? ? O(6) 0.0124(5) 0.9949(6) 0.1582(4) 0.034(2) Uij ? ? O(7) 0.1377(5) 0.8583(5) 0.1335(4) 0.033(2) Uij ? ? O(8) 0.3319(5) 0.1678(5) 0.0702(4) 0.037(2) Uij ? ? O(9) 0.8529(5) 0.9590(6) 0.2551(3) 0.037(2) Uij ? ? O(10) 0.8163(5) 0.3399(5) 0.9242(4) 0.038(2) Uij ? ? O(11) 0.1300(5) 0.1636(5) 0.8733(4) 0.036(2) Uij ? ? O(12) 0.2600(5) -0.0091(5) 0.9929(4) 0.034(2) Uij ? ? N(1) 0.4871 0.9778 0.3703 0.1900 Uij 0.35 ? N(2) 0.6485 0.8244 0.2436 0.1900 Uij 0.35 ? N(3) 0.3755 0.8121 0.2228 0.1900 Uij 0.35 ? C(1) 0.5055 0.9672 0.4491 0.1900 Uij 0.35 ? C(2) 0.2940 0.7434 0.2477 0.1900 Uij 0.35 ? C(3) 0.5795 0.9698 0.3269 0.1900 Uij 0.35 ? C(4) 0.6241 0.8582 0.3190 0.1900 Uij 0.35 ? C(5) 0.4061 0.9070 0.3455 0.1900 Uij 0.35 ? C(6) 0.3788 0.9136 0.2642 0.1900 Uij 0.35 ? C(7) 0.5634 0.8148 0.1922 0.1900 Uij 0.35 ? C(8) 0.4707 0.7530 0.2171 0.1900 Uij 0.35 ? C(9) 0.7117 0.7295 0.2439 0.1900 Uij 0.35 ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 P(1) 0.020(1) 0.015(1) 0.017(1) 0.0065(9) 0.0041(8) 0.0029(8) P(2) 0.0110(9) 0.0127(10) 0.029(1) -0.0010(8) -0.0025(9) 0.0005(9) P(3) 0.0162(10) 0.024(1) 0.0116(9) -0.0062(9) 0.0037(8) -0.0033(8) Al(1) 0.018(1) 0.020(1) 0.011(1) 0.005(1) -0.0004(9) -0.0006(10) Al(2) 0.012(1) 0.014(1) 0.027(1) 0.0021(10) 0.003(1) -0.0017(10) Al(3) 0.020(1) 0.016(1) 0.018(1) -0.009(1) 0.002(1) 0.0019(10) O(1) 0.041(4) 0.037(4) 0.033(4) -0.023(3) 0.016(3) -0.002(3) O(2) 0.029(4) 0.038(4) 0.036(4) 0.004(3) -0.004(3) 0.014(3) O(3) 0.014(3) 0.031(4) 0.063(5) 0.004(3) -0.003(3) -0.003(3) O(4) 0.030(4) 0.043(4) 0.036(4) -0.007(3) 0.008(3) 0.016(3) O(5) 0.051(4) 0.034(4) 0.017(3) 0.018(3) -0.001(3) 0.005(3) O(6) 0.020(3) 0.047(4) 0.035(4) 0.000(3) 0.006(3) 0.005(3) O(7) 0.038(4) 0.030(4) 0.032(4) 0.000(3) 0.003(3) -0.013(3) O(8) 0.027(4) 0.025(4) 0.059(5) -0.014(3) -0.012(3) 0.007(3) O(9) 0.033(4) 0.067(5) 0.010(3) -0.002(4) -0.003(3) 0.004(3) O(10) 0.032(4) 0.030(4) 0.052(4) 0.019(3) 0.018(3) 0.005(3) O(11) 0.042(4) 0.030(4) 0.037(4) 0.001(3) 0.004(3) -0.005(3) O(12) 0.045(4) 0.028(4) 0.031(4) -0.003(3) 0.000(3) -0.004(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2535 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0837 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1056 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.344 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.22 _refine_diff_density_max 2.06 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P(1) O(4) 1.524(7) ? ? yes P(1) O(5) 1.524(6) ? ? yes P(1) O(10) 1.519(6) ? ? yes P(1) O(12) 1.508(7) ? ? yes P(2) O(2) 1.522(7) ? ? yes P(2) O(3) 1.511(6) ? ? yes P(2) O(8) 1.510(7) ? ? yes P(2) O(11) 1.527(7) ? ? yes P(3) O(1) 1.523(7) ? ? yes P(3) O(6) 1.528(7) ? ? yes P(3) O(7) 1.519(7) ? ? yes P(3) O(9) 1.523(6) ? ? yes Al(1) O(5) 1.758(7) ? ? yes Al(1) O(6) 1.759(7) ? ? yes Al(1) O(9) 1.760(6) ? ? yes Al(1) O(11) 1.763(7) ? ? yes Al(2) O(3) 1.754(7) ? ? yes Al(2) O(4) 1.756(7) ? ? yes Al(2) O(7) 1.751(7) ? ? yes Al(2) O(10) 1.752(7) ? ? yes Al(3) O(1) 1.769(7) ? ? yes Al(3) O(2) 1.771(7) ? ? yes Al(3) O(8) 1.762(7) ? ? yes Al(3) O(12) 1.779(7) ? ? yes #--------------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(4) P(1) O(5) 108.9(4) ? ? ? yes O(4) P(1) O(10) 110.4(4) ? ? ? yes O(4) P(1) O(12) 110.3(4) ? ? ? yes O(5) P(1) O(10) 107.7(4) ? ? ? yes O(5) P(1) O(12) 111.2(4) ? ? ? yes O(10) P(1) O(12) 108.3(4) ? ? ? yes O(2) P(2) O(3) 109.4(4) ? ? ? yes O(2) P(2) O(8) 110.6(4) ? ? ? yes O(2) P(2) O(11) 110.6(4) ? ? ? yes O(3) P(2) O(8) 107.3(4) ? ? ? yes O(3) P(2) O(11) 110.2(4) ? ? ? yes O(8) P(2) O(11) 108.6(4) ? ? ? yes O(1) P(3) O(6) 108.0(4) ? ? ? yes O(1) P(3) O(7) 110.3(4) ? ? ? yes O(1) P(3) O(9) 108.6(4) ? ? ? yes O(6) P(3) O(7) 110.6(4) ? ? ? yes O(6) P(3) O(9) 111.1(4) ? ? ? yes O(7) P(3) O(9) 108.3(4) ? ? ? yes O(5) Al(1) O(6) 109.8(4) ? ? ? yes O(5) Al(1) O(9) 105.6(3) ? ? ? yes O(5) Al(1) O(11) 110.1(4) ? ? ? yes O(6) Al(1) O(9) 110.6(3) ? ? ? yes O(6) Al(1) O(11) 110.2(4) ? ? ? yes O(9) Al(1) O(11) 110.5(4) ? ? ? yes O(3) Al(2) O(4) 110.9(4) ? ? ? yes O(3) Al(2) O(7) 110.4(4) ? ? ? yes O(3) Al(2) O(10) 106.8(4) ? ? ? yes O(4) Al(2) O(7) 109.8(4) ? ? ? yes O(4) Al(2) O(10) 110.7(4) ? ? ? yes O(7) Al(2) O(10) 108.1(4) ? ? ? yes O(1) Al(3) O(2) 111.1(4) ? ? ? yes O(1) Al(3) O(8) 106.9(4) ? ? ? yes O(1) Al(3) O(12) 110.0(3) ? ? ? yes O(2) Al(3) O(8) 110.7(3) ? ? ? yes O(2) Al(3) O(12) 109.6(4) ? ? ? yes O(8) Al(3) O(12) 108.4(4) ? ? ? yes P(3) O(1) Al(3) 146.5(5) ? ? ? yes P(2) O(2) Al(3) 147.2(5) ? ? ? yes P(2) O(3) Al(2) 149.9(5) ? ? ? yes P(1) O(4) Al(2) 147.2(5) ? ? ? yes P(1) O(5) Al(1) 148.7(4) ? ? ? yes P(3) O(6) Al(1) 148.3(5) ? ? ? yes P(3) O(7) Al(2) 147.1(5) ? ? ? yes P(2) O(8) Al(3) 147.9(5) ? ? ? yes P(3) O(9) Al(1) 148.3(5) ? ? ? yes P(1) O(10) Al(2) 146.4(5) ? ? ? yes P(2) O(11) Al(1) 145.4(5) ? ? ? yes P(1) O(12) Al(3) 147.9(5) ? ? ? yes data_eppw3 # CoAlPO-cyclam-1 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C10 H24 N4.Co.Al.P O4.P O3 (OH)' _chemical_formula_structural 'C10 H25 Al Co N4 O8 P2' _chemical_formula_analytical 'C10 H25 Al Co N4 O8 P2' _chemical_formula_sum 'C10 H25 Al Co N4 O8 P2' _chemical_formula_weight 477.19 _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' 'Al' 'Al' 0.0645 0.0514 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9780(8) _cell_length_b 14.7200(8) _cell_length_c 8.4792(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.3230(10) _cell_angle_gamma 90.00 _cell_volume 1849.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max .28 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .25 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method - _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.775120 _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 7991 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2659 _reflns_number_observed 2100 _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 42 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^)+(0.0404P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2617 _refine_ls_number_parameters 259 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_obs 0.0285 _refine_ls_wR_factor_all 0.0818 _refine_ls_wR_factor_obs 0.0643 _refine_ls_goodness_of_fit_all 0.984 _refine_ls_goodness_of_fit_obs 1.042 _refine_ls_restrained_S_all 1.176 _refine_ls_restrained_S_obs 1.041 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.5000 0.5000 0.0000 0.0257(2) Uani 1 d S . N1 N 0.5907(2) 0.4068(2) 0.1259(3) 0.0369(6) Uani 1 d D . H1N H 0.6380(15) 0.4462(17) 0.1797(33) 0.056(10) Uiso 1 d D . C2 C 0.5389(2) 0.3650(2) 0.2419(4) 0.0555(10) Uani 1 d . . H2A H 0.5797(2) 0.3348(2) 0.3248(4) 0.067 Uiso 1 calc R . H2B H 0.4978(2) 0.3199(2) 0.1890(4) 0.067 Uiso 1 calc R . C3 C 0.4861(2) 0.4372(2) 0.3150(4) 0.0554(10) Uani 1 d . . H3A H 0.4517(2) 0.4096(2) 0.3908(4) 0.066 Uiso 1 calc R . H3B H 0.5273(2) 0.4811(2) 0.3714(4) 0.066 Uiso 1 calc R . N4 N 0.4250(2) 0.4829(2) 0.1891(3) 0.0387(6) Uani 1 d D . H4N H 0.3765(16) 0.4396(18) 0.1549(40) 0.071(11) Uiso 1 d D . C5 C 0.3851(2) 0.5683(2) 0.2387(4) 0.0525(10) Uani 1 d . . H5A H 0.4331(2) 0.6099(2) 0.2797(4) 0.063 Uiso 1 calc R . H5B H 0.3502(2) 0.5555(2) 0.3240(4) 0.063 Uiso 1 calc R . C6 C 0.3248(2) 0.6130(3) 0.1021(5) 0.0629(11) Uani 1 d . . H6A H 0.2881(2) 0.6580(3) 0.1463(5) 0.076 Uiso 1 calc R . H6B H 0.2842(2) 0.5672(3) 0.0502(5) 0.076 Uiso 1 calc R . C7 C 0.3709(2) 0.6589(2) -0.0240(5) 0.0546(10) Uani 1 d . . H7A H 0.3275(2) 0.6969(2) -0.0898(5) 0.065 Uiso 1 calc R . H7B H 0.4186(2) 0.6979(2) 0.0275(5) 0.065 Uiso 1 calc R . O1 O 0.56522(11) 0.61272(12) 0.1232(2) 0.0294(5) Uani 1 d . . P1 P 0.66294(4) 0.63284(4) 0.17797(8) 0.0208(2) Uani 1 d . . O2 O 0.71128(12) 0.64824(12) 0.0301(2) 0.0331(5) Uani 1 d . . O3 O 0.71151(12) 0.55526(11) 0.2747(2) 0.0280(4) Uani 1 d . . O4 O 0.67345(11) 0.72135(11) 0.2784(2) 0.0273(4) Uani 1 d . . Al1 Al 0.75679(5) 0.77786(5) 0.40482(9) 0.0187(2) Uani 1 d . . O5 O 0.83194(12) 0.70208(12) 0.5128(2) 0.0272(4) Uani 1 d . . P2 P 0.82969(5) 0.62180(5) 0.62820(8) 0.0226(2) Uani 1 d . . O6 O 0.91204(13) 0.56558(13) 0.6327(2) 0.0383(5) Uani 1 d . . O7 O 0.82170(12) 0.65688(13) 0.7944(2) 0.0349(5) Uani 1 d . . O8 O 0.74191(14) 0.56745(15) 0.5719(2) 0.0420(5) Uani 1 d D . H8O H 0.7255(22) 0.5591(25) 0.4565(10) 0.073(12) Uiso 1 d D . Co2 Co 1.0000 0.5000 0.5000 0.0245(2) Uani 1 d S . N11 N 1.0999(2) 0.5136(2) 0.7018(3) 0.0409(7) Uani 1 d D . H11N H 1.1543(12) 0.4812(17) 0.6823(36) 0.045(9) Uiso 1 d D . C12 C 1.1235(2) 0.6112(2) 0.7035(5) 0.0612(11) Uani 1 d . . H12A H 1.1802(2) 0.6209(2) 0.7726(5) 0.073 Uiso 1 calc R . H12B H 1.0772(2) 0.6460(2) 0.7453(5) 0.073 Uiso 1 calc R . C13 C 1.1316(3) 0.6430(2) 0.5374(5) 0.0640(11) Uani 1 d . . H13A H 1.1467(3) 0.7071(2) 0.5393(5) 0.077 Uiso 1 calc R . H13B H 1.1795(3) 0.6099(2) 0.4971(5) 0.077 Uiso 1 calc R . N14 N 1.0456(2) 0.6279(2) 0.4324(3) 0.0455(7) Uani 1 d D . H14N H 1.0012(17) 0.6734(16) 0.4543(41) 0.069(11) Uiso 1 d D . C15 C 1.0480(3) 0.6363(2) 0.2602(4) 0.0627(11) Uani 1 d . . H15A H 1.0931(3) 0.5949(2) 0.2301(4) 0.075 Uiso 1 calc R . H15B H 1.0660(3) 0.6976(2) 0.2370(4) 0.075 Uiso 1 calc R . C16 C 0.9579(3) 0.6156(3) 0.1611(4) 0.0664(12) Uani 1 d . . H16A H 0.9120(3) 0.6504(3) 0.2040(4) 0.080 Uiso 1 calc R . H16B H 0.9599(3) 0.6374(3) 0.0537(4) 0.080 Uiso 1 calc R . C17 C 0.9283(2) 0.5181(2) 0.1505(4) 0.0548(10) Uani 1 d . . H17A H 0.8786(2) 0.5114(2) 0.0643(4) 0.066 Uiso 1 calc R . H17B H 0.9778(2) 0.4806(2) 0.1259(4) 0.066 Uiso 1 calc R . 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 Co1 0.0283(3) 0.0244(3) 0.0234(3) -0.0010(2) -0.0002(2) -0.0039(2) N1 0.041(2) 0.0233(13) 0.042(2) -0.0048(12) -0.0108(12) -0.0038(12) C2 0.076(3) 0.036(2) 0.047(2) 0.016(2) -0.016(2) -0.015(2) C3 0.082(3) 0.056(2) 0.027(2) 0.003(2) 0.005(2) -0.027(2) N4 0.043(2) 0.042(2) 0.0322(15) -0.0104(13) 0.0087(12) -0.0196(13) C5 0.055(2) 0.053(2) 0.056(2) -0.027(2) 0.028(2) -0.019(2) C6 0.036(2) 0.059(2) 0.093(3) -0.036(2) 0.008(2) 0.003(2) C7 0.040(2) 0.035(2) 0.083(3) -0.013(2) -0.010(2) 0.009(2) O1 0.0256(10) 0.0297(10) 0.0314(11) -0.0031(9) -0.0012(8) -0.0043(8) P1 0.0228(4) 0.0217(4) 0.0173(4) 0.0016(3) 0.0008(3) -0.0045(3) O2 0.0438(12) 0.0316(11) 0.0259(11) 0.0032(9) 0.0117(9) -0.0077(9) O3 0.0344(11) 0.0236(10) 0.0244(10) 0.0019(8) -0.0016(8) -0.0006(9) O4 0.0300(10) 0.0249(10) 0.0252(11) -0.0030(8) -0.0020(8) -0.0017(8) Al1 0.0234(4) 0.0189(4) 0.0143(4) -0.0004(3) 0.0038(3) -0.0005(3) O5 0.0301(11) 0.0246(10) 0.0257(11) 0.0026(9) -0.0002(8) 0.0005(8) P2 0.0274(4) 0.0237(4) 0.0173(4) -0.0007(3) 0.0054(3) 0.0053(3) O6 0.0447(13) 0.0408(12) 0.0309(12) 0.0029(10) 0.0104(10) 0.0246(10) O7 0.0400(12) 0.0434(12) 0.0211(11) -0.0036(9) 0.0035(9) 0.0160(10) O8 0.0460(13) 0.0516(13) 0.0274(13) 0.0052(11) 0.0024(10) -0.0201(11) Co2 0.0292(3) 0.0224(3) 0.0230(3) 0.0007(2) 0.0070(2) 0.0057(2) N11 0.036(2) 0.057(2) 0.0289(15) -0.0069(13) 0.0021(12) 0.0173(13) C12 0.047(2) 0.062(2) 0.072(3) -0.040(2) -0.003(2) -0.003(2) C13 0.066(3) 0.039(2) 0.093(3) -0.017(2) 0.032(2) -0.017(2) N14 0.055(2) 0.0284(14) 0.059(2) 0.0026(14) 0.0257(15) 0.0022(13) C15 0.098(3) 0.034(2) 0.067(3) 0.014(2) 0.050(3) 0.007(2) C16 0.087(3) 0.078(3) 0.038(2) 0.024(2) 0.024(2) 0.043(2) C17 0.061(2) 0.075(3) 0.028(2) 0.000(2) 0.001(2) 0.034(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 Co1 N4 2.102(2) . ? Co1 N4 2.102(2) 3_665 ? Co1 N1 2.109(2) . ? Co1 N1 2.109(2) 3_665 ? Co1 O1 2.122(2) 3_665 ? Co1 O1 2.122(2) . ? N1 C7 1.468(4) 3_665 ? N1 C2 1.473(4) . ? C2 C3 1.509(5) . ? C3 N4 1.466(4) . ? N4 C5 1.479(4) . ? C5 C6 1.512(5) . ? C6 C7 1.513(5) . ? C7 N1 1.468(4) 3_665 ? O1 P1 1.500(2) . ? P1 O3 1.528(2) . ? P1 O4 1.552(2) . ? P1 O2 1.553(2) . ? O2 Al1 1.728(2) 4_575 ? O4 Al1 1.736(2) . ? Al1 O2 1.728(2) 4_576 ? Al1 O7 1.734(2) 4_575 ? Al1 O5 1.747(2) . ? O5 P2 1.538(2) . ? P2 O6 1.481(2) . ? P2 O7 1.522(2) . ? P2 O8 1.554(2) . ? O6 Co2 2.089(2) . ? O7 Al1 1.734(2) 4_576 ? Co2 O6 2.089(2) 3_766 ? Co2 N14 2.109(2) . ? Co2 N14 2.109(2) 3_766 ? Co2 N11 2.113(3) . ? Co2 N11 2.114(3) 3_766 ? N11 C17 1.456(4) 3_766 ? N11 C12 1.478(4) . ? C12 C13 1.506(5) . ? C13 N14 1.473(5) . ? N14 C15 1.472(4) . ? C15 C16 1.513(5) . ? C16 C17 1.501(5) . ? C17 N11 1.456(4) 3_766 ? 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 N4 Co1 N4 180.0 . 3_665 ? N4 Co1 N1 84.98(10) . . ? N4 Co1 N1 95.02(10) 3_665 . ? N4 Co1 N1 95.02(10) . 3_665 ? N4 Co1 N1 84.98(10) 3_665 3_665 ? N1 Co1 N1 180.0 . 3_665 ? N4 Co1 O1 91.32(8) . 3_665 ? N4 Co1 O1 88.67(8) 3_665 3_665 ? N1 Co1 O1 87.56(8) . 3_665 ? N1 Co1 O1 92.44(8) 3_665 3_665 ? N4 Co1 O1 88.68(8) . . ? N4 Co1 O1 91.32(8) 3_665 . ? N1 Co1 O1 92.44(8) . . ? N1 Co1 O1 87.56(8) 3_665 . ? O1 Co1 O1 179.999(1) 3_665 . ? C7 N1 C2 114.0(2) 3_665 . ? C7 N1 Co1 114.2(2) 3_665 . ? C2 N1 Co1 104.2(2) . . ? N1 C2 C3 109.8(3) . . ? N4 C3 C2 109.5(3) . . ? C3 N4 C5 114.8(3) . . ? C3 N4 Co1 105.3(2) . . ? C5 N4 Co1 113.4(2) . . ? N4 C5 C6 111.9(3) . . ? C5 C6 C7 116.9(3) . . ? N1 C7 C6 112.3(3) 3_665 . ? P1 O1 Co1 131.75(11) . . ? O1 P1 O3 112.71(10) . . ? O1 P1 O4 110.64(10) . . ? O3 P1 O4 109.30(10) . . ? O1 P1 O2 109.10(10) . . ? O3 P1 O2 107.54(11) . . ? O4 P1 O2 107.36(10) . . ? P1 O2 Al1 149.30(13) . 4_575 ? P1 O4 Al1 138.42(12) . . ? O2 Al1 O7 106.55(10) 4_576 4_575 ? O2 Al1 O4 111.65(9) 4_576 . ? O7 Al1 O4 109.95(9) 4_575 . ? O2 Al1 O5 111.20(9) 4_576 . ? O7 Al1 O5 105.52(9) 4_575 . ? O4 Al1 O5 111.66(9) . . ? P2 O5 Al1 138.81(12) . . ? O6 P2 O7 110.04(11) . . ? O6 P2 O5 110.54(11) . . ? O7 P2 O5 109.90(10) . . ? O6 P2 O8 112.62(12) . . ? O7 P2 O8 106.43(11) . . ? O5 P2 O8 107.18(10) . . ? P2 O6 Co2 146.32(12) . . ? P2 O7 Al1 144.41(13) . 4_576 ? O6 Co2 O6 180.0 . 3_766 ? O6 Co2 N14 89.32(9) . . ? O6 Co2 N14 90.68(9) 3_766 . ? O6 Co2 N14 90.68(9) . 3_766 ? O6 Co2 N14 89.32(9) 3_766 3_766 ? N14 Co2 N14 180.0 . 3_766 ? O6 Co2 N11 87.03(8) . . ? O6 Co2 N11 92.97(8) 3_766 . ? N14 Co2 N11 85.20(11) . . ? N14 Co2 N11 94.80(11) 3_766 . ? O6 Co2 N11 92.97(8) . 3_766 ? O6 Co2 N11 87.03(8) 3_766 3_766 ? N14 Co2 N11 94.81(11) . 3_766 ? N14 Co2 N11 85.19(11) 3_766 3_766 ? N11 Co2 N11 180.0 . 3_766 ? C17 N11 C12 113.7(3) 3_766 . ? C17 N11 Co2 113.9(2) 3_766 . ? C12 N11 Co2 103.9(2) . . ? N11 C12 C13 110.2(3) . . ? N14 C13 C12 109.6(3) . . ? C15 N14 C13 116.2(3) . . ? C15 N14 Co2 113.6(2) . . ? C13 N14 Co2 105.1(2) . . ? N14 C15 C16 112.7(3) . . ? C17 C16 C15 117.2(3) . . ? N11 C17 C16 112.0(3) 3_766 . ? 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 N4 Co1 N1 C7 140.7(2) . . . 3_665 ? N4 Co1 N1 C7 -39.3(2) 3_665 . . 3_665 ? N1 Co1 N1 C7 75.0(47) 3_665 . . 3_665 ? O1 Co1 N1 C7 49.2(2) 3_665 . . 3_665 ? O1 Co1 N1 C7 -130.8(2) . . . 3_665 ? N4 Co1 N1 C2 15.7(2) . . . . ? N4 Co1 N1 C2 -164.3(2) 3_665 . . . ? N1 Co1 N1 C2 -50.1(47) 3_665 . . . ? O1 Co1 N1 C2 -75.9(2) 3_665 . . . ? O1 Co1 N1 C2 104.1(2) . . . . ? C7 N1 C2 C3 -167.8(3) 3_665 . . . ? Co1 N1 C2 C3 -42.7(3) . . . . ? N1 C2 C3 N4 59.0(4) . . . . ? C2 C3 N4 C5 -166.5(3) . . . . ? C2 C3 N4 Co1 -41.0(3) . . . . ? N4 Co1 N4 C3 148.7(9) 3_665 . . . ? N1 Co1 N4 C3 13.8(2) . . . . ? N1 Co1 N4 C3 -166.2(2) 3_665 . . . ? O1 Co1 N4 C3 101.2(2) 3_665 . . . ? O1 Co1 N4 C3 -78.8(2) . . . . ? N4 Co1 N4 C5 -85.0(8) 3_665 . . . ? N1 Co1 N4 C5 140.1(2) . . . . ? N1 Co1 N4 C5 -39.9(2) 3_665 . . . ? O1 Co1 N4 C5 -132.5(2) 3_665 . . . ? O1 Co1 N4 C5 47.5(2) . . . . ? C3 N4 C5 C6 178.5(3) . . . . ? Co1 N4 C5 C6 57.4(3) . . . . ? N4 C5 C6 C7 -73.5(4) . . . . ? C5 C6 C7 N1 72.4(4) . . . 3_665 ? N4 Co1 O1 P1 123.2(2) . . . . ? N4 Co1 O1 P1 -56.8(2) 3_665 . . . ? N1 Co1 O1 P1 38.3(2) . . . . ? N1 Co1 O1 P1 -141.7(2) 3_665 . . . ? O1 Co1 O1 P1 -39.6(51) 3_665 . . . ? Co1 O1 P1 O3 -51.6(2) . . . . ? Co1 O1 P1 O4 -174.29(12) . . . . ? Co1 O1 P1 O2 67.8(2) . . . . ? O1 P1 O2 Al1 102.8(3) . . . 4_575 ? O3 P1 O2 Al1 -134.6(2) . . . 4_575 ? O4 P1 O2 Al1 -17.1(3) . . . 4_575 ? O1 P1 O4 Al1 166.8(2) . . . . ? O3 P1 O4 Al1 42.1(2) . . . . ? O2 P1 O4 Al1 -74.3(2) . . . . ? P1 O4 Al1 O2 -158.0(2) . . . 4_576 ? P1 O4 Al1 O7 83.9(2) . . . 4_575 ? P1 O4 Al1 O5 -32.8(2) . . . . ? O2 Al1 O5 P2 68.4(2) 4_576 . . . ? O7 Al1 O5 P2 -176.5(2) 4_575 . . . ? O4 Al1 O5 P2 -57.1(2) . . . . ? Al1 O5 P2 O6 159.4(2) . . . . ? Al1 O5 P2 O7 -79.0(2) . . . . ? Al1 O5 P2 O8 36.3(2) . . . . ? O7 P2 O6 Co2 -168.7(2) . . . . ? O5 P2 O6 Co2 -47.1(3) . . . . ? O8 P2 O6 Co2 72.7(3) . . . . ? O6 P2 O7 Al1 179.5(2) . . . 4_576 ? O5 P2 O7 Al1 57.6(3) . . . 4_576 ? O8 P2 O7 Al1 -58.2(3) . . . 4_576 ? P2 O6 Co2 O6 -94.2(87) . . . 3_766 ? P2 O6 Co2 N14 69.5(2) . . . . ? P2 O6 Co2 N14 -110.5(2) . . . 3_766 ? P2 O6 Co2 N11 154.7(2) . . . . ? P2 O6 Co2 N11 -25.3(2) . . . 3_766 ? O6 Co2 N11 C17 50.6(2) . . . 3_766 ? O6 Co2 N11 C17 -129.4(2) 3_766 . . 3_766 ? N14 Co2 N11 C17 140.2(2) . . . 3_766 ? N14 Co2 N11 C17 -39.8(2) 3_766 . . 3_766 ? N11 Co2 N11 C17 -56.0(154) 3_766 . . 3_766 ? O6 Co2 N11 C12 -73.6(2) . . . . ? O6 Co2 N11 C12 106.4(2) 3_766 . . . ? N14 Co2 N11 C12 16.0(2) . . . . ? N14 Co2 N11 C12 -164.0(2) 3_766 . . . ? N11 Co2 N11 C12 179.8(154) 3_766 . . . ? C17 N11 C12 C13 -167.4(3) 3_766 . . . ? Co2 N11 C12 C13 -43.0(3) . . . . ? N11 C12 C13 N14 59.0(4) . . . . ? C12 C13 N14 C15 -166.9(3) . . . . ? C12 C13 N14 Co2 -40.4(3) . . . . ? O6 Co2 N14 C15 -131.6(2) . . . . ? O6 Co2 N14 C15 48.4(2) 3_766 . . . ? N14 Co2 N14 C15 13.7(1000) 3_766 . . . ? N11 Co2 N14 C15 141.3(2) . . . . ? N11 Co2 N14 C15 -38.7(2) 3_766 . . . ? O6 Co2 N14 C13 100.3(2) . . . . ? O6 Co2 N14 C13 -79.7(2) 3_766 . . . ? N14 Co2 N14 C13 -114.4(259) 3_766 . . . ? N11 Co2 N14 C13 13.2(2) . . . . ? N11 Co2 N14 C13 -166.8(2) 3_766 . . . ? C13 N14 C15 C16 177.5(3) . . . . ? Co2 N14 C15 C16 55.4(3) . . . . ? N14 C15 C16 C17 -72.5(4) . . . . ? C15 C16 C17 N11 73.3(4) . . . 3_766 ? _refine_diff_density_max 0.271 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.054 data_A_TEXRAY.INF_file_is_not_p #------------------------------------------------------------------------------ _audit_creation_date 'Wed Apr 27 09:21:29 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'LS (W.Clegg)' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 23.990(8) _cell_length_b 23.990(8) _cell_length_c 23.990(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13806(6) _cell_formula_units_Z 96 _cell_measurement_temperature 150 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'F m -3 c ' _symmetry_Int_Tables_number 226 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x,1/2+y,1/2+z' '1/2+x, +y,1/2+z' '1/2+x,1/2+y, +z' ' +z, +x, +y' ' +z,1/2+x,1/2+y' '1/2+z, +x,1/2+y' '1/2+z,1/2+x, +y' ' +y, +z, +x' ' +y,1/2+z,1/2+x' '1/2+y, +z,1/2+x' '1/2+y,1/2+z, +x' ' +x, -y, -z' ' +x,1/2-y,1/2-z' '1/2+x, -y,1/2-z' '1/2+x,1/2-y, -z' ' +z, -x, -y' ' +z,1/2-x,1/2-y' '1/2+z, -x,1/2-y' '1/2+z,1/2-x, -y' ' +y, -z, -x' ' +y,1/2-z,1/2-x' '1/2+y, -z,1/2-x' '1/2+y,1/2-z, -x' ' -x, +y, -z' ' -x,1/2+y,1/2-z' '1/2-x, +y,1/2-z' '1/2-x,1/2+y, -z' ' -z, +x, -y' ' -z,1/2+x,1/2-y' '1/2-z, +x,1/2-y' '1/2-z,1/2+x, -y' ' -y, +z, -x' ' -y,1/2+z,1/2-x' '1/2-y, +z,1/2-x' '1/2-y,1/2+z, -x' ' -x, -y, +z' ' -x,1/2-y,1/2+z' '1/2-x, -y,1/2+z' '1/2-x,1/2-y, +z' ' -z, -x, +y' ' -z,1/2-x,1/2+y' '1/2-z, -x,1/2+y' '1/2-z,1/2-x, +y' ' -y, -z, +x' ' -y,1/2-z,1/2+x' '1/2-y, -z,1/2+x' '1/2-y,1/2-z, +x' ' +x, +z,1/2+y' ' +x,1/2+z, +y' '1/2+x, +z, +y' '1/2+x,1/2+z,1/2+y' ' +y, +x,1/2+z' ' +y,1/2+x, +z' '1/2+y, +x, +z' '1/2+y,1/2+x,1/2+z' ' +z, +y,1/2+x' ' +z,1/2+y, +x' '1/2+z, +y, +x' '1/2+z,1/2+y,1/2+x' ' +x, -z,1/2-y' ' +x,1/2-z, -y' '1/2+x, -z, -y' '1/2+x,1/2-z,1/2-y' ' +y, -x,1/2-z' ' +y,1/2-x, -z' '1/2+y, -x, -z' '1/2+y,1/2-x,1/2-z' ' +z, -y,1/2-x' ' +z,1/2-y, -x' '1/2+z, -y, -x' '1/2+z,1/2-y,1/2-x' ' -x, +z,1/2-y' ' -x,1/2+z, -y' '1/2-x, +z, -y' '1/2-x,1/2+z,1/2-y' ' -y, +x,1/2-z' ' -y,1/2+x, -z' '1/2-y, +x, -z' '1/2-y,1/2+x,1/2-z' ' -z, +y,1/2-x' ' -z,1/2+y, -x' '1/2-z, +y, -x' '1/2-z,1/2+y,1/2-x' ' -x, -z,1/2+y' ' -x,1/2-z, +y' '1/2-x, -z, +y' '1/2-x,1/2-z,1/2+y' ' -y, -x,1/2+z' ' -y,1/2-x, +z' '1/2-y, -x, +z' '1/2-y,1/2-x,1/2+z' ' -z, -y,1/2+x' ' -z,1/2-y, +x' '1/2-z, -y, +x' '1/2-z,1/2-y,1/2+x' ' -x, -y, -z' ' -x,1/2-y,1/2-z' '1/2-x, -y,1/2-z' '1/2-x,1/2-y, -z' ' -z, -x, -y' ' -z,1/2-x,1/2-y' '1/2-z, -x,1/2-y' '1/2-z,1/2-x, -y' ' -y, -z, -x' ' -y,1/2-z,1/2-x' '1/2-y, -z,1/2-x' '1/2-y,1/2-z, -x' ' -x, +y, +z' ' -x,1/2+y,1/2+z' '1/2-x, +y,1/2+z' '1/2-x,1/2+y, +z' ' -z, +x, +y' ' -z,1/2+x,1/2+y' '1/2-z, +x,1/2+y' '1/2-z,1/2+x, +y' ' -y, +z, +x' ' -y,1/2+z,1/2+x' '1/2-y, +z,1/2+x' '1/2-y,1/2+z, +x' ' +x, -y, +z' ' +x,1/2-y,1/2+z' '1/2+x, -y,1/2+z' '1/2+x,1/2-y, +z' ' +z, -x, +y' ' +z,1/2-x,1/2+y' '1/2+z, -x,1/2+y' '1/2+z,1/2-x, +y' ' +y, -z, +x' ' +y,1/2-z,1/2+x' '1/2+y, -z,1/2+x' '1/2+y,1/2-z, +x' ' +x, +y, -z' ' +x,1/2+y,1/2-z' '1/2+x, +y,1/2-z' '1/2+x,1/2+y, -z' ' +z, +x, -y' ' +z,1/2+x,1/2-y' '1/2+z, +x,1/2-y' '1/2+z,1/2+x, -y' ' +y, +z, -x' ' +y,1/2+z,1/2-x' '1/2+y, +z,1/2-x' '1/2+y,1/2+z, -x' ' -x, -z,1/2-y' ' -x,1/2-z, -y' '1/2-x, -z, -y' '1/2-x,1/2-z,1/2-y' ' -y, -x,1/2-z' ' -y,1/2-x, -z' '1/2-y, -x, -z' '1/2-y,1/2-x,1/2-z' ' -z, -y,1/2-x' ' -z,1/2-y, -x' '1/2-z, -y, -x' '1/2-z,1/2-y,1/2-x' ' -x, +z,1/2+y' ' -x,1/2+z, +y' '1/2-x, +z, +y' '1/2-x,1/2+z,1/2+y' ' -y, +x,1/2+z' ' -y,1/2+x, +z' '1/2-y, +x, +z' '1/2-y,1/2+x,1/2+z' ' -z, +y,1/2+x' ' -z,1/2+y, +x' '1/2-z, +y, +x' '1/2-z,1/2+y,1/2+x' ' +x, -z,1/2+y' ' +x,1/2-z, +y' '1/2+x, -z, +y' '1/2+x,1/2-z,1/2+y' ' +y, -x,1/2+z' ' +y,1/2-x, +z' '1/2+y, -x, +z' '1/2+y,1/2-x,1/2+z' ' +z, -y,1/2+x' ' +z,1/2-y, +x' '1/2+z, -y, +x' '1/2+z,1/2-y,1/2+x' ' +x, +z,1/2-y' ' +x,1/2+z, -y' '1/2+x, +z, -y' '1/2+x,1/2+z,1/2-y' ' +y, +x,1/2-z' ' +y,1/2+x, -z' '1/2+y, +x, -z' '1/2+y,1/2+x,1/2-z' ' +z, +y,1/2-x' ' +z,1/2+y, -x' '1/2+z, +y, -x' '1/2+z,1/2+y,1/2-x' #------------------------------------------------------------------------------ _exptl_crystal_description 'cube' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.020 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_meas ? _chemical_formula_weight 158.03 _chemical_formula_analytical ? _chemical_formula_sum 'C1.50 Al0.80 N0.17 O4.50 P Zn0.20 ' _chemical_formula_moiety 'C1.50 Al0.80 N0.17 O4.50 P Zn0.20 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 7448.64 _exptl_absorpt_coefficient_mu 1.343 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.6942 _diffrn_radiation_type 'Monochromated synchrotron X-rays' _diffrn_radiation_source 'Daresbury Synchrotron' _diffrn_radiation_detector ? _diffrn_measurement_device 'CCD' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 6420 _reflns_number_total 1007 _reflns_number_observed 312 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 8.06 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 29.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al 0 76 0.064 0.051 'International Tables' P 0 96 0.102 0.094 'International Tables' O 0 432 0.011 0.006 'International Tables' N 0 16 0.006 0.003 'International Tables' Zn 0 19 0.284 1.430 'International Tables' C 0 144 0.003 0.002 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Zn(1) 0.0000 0.1839 0.0899 0.0273 Uij ? ? P(1) 0.0000 0.0942(8) 0.1867(7) 0.028(4) Uij ? ? Al(1) 0.0000 0.1839(6) 0.0899(7) 0.027(4) Uij ? ? O(11) 0.0000 0.1086(9) 0.245(2) 0.046(8) Uij ? ? O(12) 0.0000 0.148(2) 0.151(1) 0.036(10) Uij ? ? O(13) 0.0491(10) 0.0597(9) 0.1738(6) 0.047(7) Uij ? ? O(1) 0.2015 0.1583 0.2904 0.1267 Uij 0.083 ? O(2) 0.2425 0.3355 0.3076 0.1267 Uij 0.083 ? O(3) 0.3044 0.1136 0.2310 0.1267 Uij 0.083 ? O(4) 0.3585 0.3041 0.3095 0.1267 Uij 0.083 ? O(5) 0.1467 0.3134 0.1363 0.1267 Uij 0.083 ? O(6) 0.2732 0.3122 0.1350 0.1267 Uij 0.083 ? N(1) 0.1505 0.2667 0.2603 0.1267 Uij 0.083 ? N(2) 0.3435 0.2354 0.2068 0.1267 Uij 0.083 ? C(1) 0.1503 0.2500 0.1503 0.1267 Uij 0.083 ? C(2) 0.3283 0.3283 0.1717 0.1267 Uij 0.083 ? C(3) 0.3636 0.2878 0.1779 0.1267 Uij 0.083 ? C(4) 0.1353 0.2333 0.3118 0.1267 Uij 0.083 ? C(5) 0.1471 0.3288 0.2689 0.1267 Uij 0.083 ? C(6) 0.1855 0.3542 0.3139 0.1267 Uij 0.083 ? C(7) 0.1822 0.1952 0.3339 0.1267 Uij 0.083 ? C(8) 0.2380 0.1144 0.3087 0.1267 Uij 0.083 ? C(9) 0.2835 0.3677 0.3376 0.1267 Uij 0.083 ? C(10) 0.2500 0.0821 0.2500 0.1267 Uij 0.083 ? C(11) 0.3322 0.3310 0.3565 0.1267 Uij 0.083 ? C(12) 0.2879 0.1459 0.1830 0.1267 Uij 0.083 ? C(13) 0.3618 0.2440 0.3120 0.1267 Uij 0.083 ? C(14) 0.3336 0.1881 0.1664 0.1267 Uij 0.083 ? C(15) 0.3802 0.2194 0.2555 0.1267 Uij 0.083 ? C(16) 0.1191 0.2470 0.2095 0.1267 Uij 0.083 ? C(17) 0.1827 0.3291 0.0906 0.1267 Uij 0.083 ? C(18) 0.2371 0.3547 0.1123 0.1267 Uij 0.083 ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn(1) 0.0266 0.0301 0.0252 0.0000 0.0000 0.0115 P(1) 0.033(10) 0.024(8) 0.028(9) 0.0000 0.0000 0.010(8) Al(1) 0.027(8) 0.030(8) 0.025(7) 0.0000 0.0000 0.011(7) O(11) 0.07(2) 0.06(1) 0.01(2) 0.0000 0.0000 0.02(2) O(12) 0.05(1) 0.04(2) 0.02(2) 0.0000 0.0000 0.018(10) O(13) 0.07(2) 0.01(1) 0.06(1) 0.014(9) 0.01(1) 0.015(9) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 312 _refine_ls_number_parameters 33 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.1233 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1329 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 8.098 _refine_ls_shift/esd_max 0.0110 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.88 _refine_diff_density_max 4.49 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn(1) O(11) 1.77(4) ? ? yes Zn(1) O(12) 1.72(5) ? ? yes Zn(1) O(13) 1.75(3) ? ? yes Zn(1) O(13) 1.75(3) ? ? yes P(1) O(11) 1.43(5) ? ? yes P(1) O(12) 1.53(5) ? ? yes P(1) O(13) 1.47(3) ? ? yes P(1) O(13) 1.47(3) ? ? yes Al(1) O(11) 1.77(5) ? ? yes Al(1) O(12) 1.72(5) ? ? yes Al(1) O(13) 1.75(3) ? ? yes Al(1) O(13) 1.75(3) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(11) Zn(1) O(12) 105(1) ? ? ? yes O(11) Zn(1) O(13) 105.9(6) ? ? ? yes O(11) Zn(1) O(13) 105.9(6) ? ? ? yes O(12) Zn(1) O(13) 114.3(6) ? ? ? yes O(12) Zn(1) O(13) 114.3(6) ? ? ? yes O(13) Zn(1) O(13) 109.7(10) ? ? ? yes O(11) P(1) O(12) 109(1) ? ? ? yes O(11) P(1) O(13) 109(1) ? ? ? yes O(11) P(1) O(13) 109(1) ? ? ? yes O(12) P(1) O(13) 110(1) ? ? ? yes O(12) P(1) O(13) 110(1) ? ? ? yes O(13) P(1) O(13) 106(1) ? ? ? yes O(11) Al(1) O(12) 105(1) ? ? ? yes O(11) Al(1) O(13) 105.9(8) ? ? ? yes O(11) Al(1) O(13) 105.9(8) ? ? ? yes O(12) Al(1) O(13) 114.3(8) ? ? ? yes O(12) Al(1) O(13) 114.3(8) ? ? ? yes O(13) Al(1) O(13) 109(1) ? ? ? yes Zn(1) O(11) P(1) 151(1) ? ? ? yes Zn(1) O(12) P(1) 154(1) ? ? ? yes Zn(1) O(13) P(1) 151(1) ? ? ? yes