data_adranosite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al2 Cl H18 N4 Na O18 S4' _chemical_formula_weight 602.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/acd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z+1/2' '-x+1/2, y, -z' '-y+1/4, -x+1/4, -z+1/4' 'y+3/4, x+1/4, -z+1/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1, y+1/2, -z+1/2' '-y+3/4, -x+3/4, -z+3/4' 'y+5/4, x+3/4, -z+3/4' 'y+3/4, -x+3/4, z+5/4' '-y+3/4, x+5/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z-1/2' 'x-1/2, -y, z' 'y-1/4, x-1/4, z-1/4' '-y-3/4, -x-1/4, z-1/4' '-y-1/4, x-1/4, -z-3/4' 'y-1/4, -x-3/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' 'y+1/4, x+1/4, z+1/4' '-y-1/4, -x+1/4, z+1/4' '-y+1/4, x+1/4, -z-1/4' 'y+1/4, -x-1/4, -z+1/4' _cell_length_a 18.118(3) _cell_length_b 18.118(3) _cell_length_c 11.320(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3715.5(13) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 741 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 19.58 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.018 _exptl_crystal_size_min 0.012 _exptl_crystal_density_meas 2.15(1) _exptl_crystal_density_diffrn 2.155 _exptl_crystal_density_method flotation _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.843 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Apex II CCD diffractometer' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17231 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 29.31 _reflns_number_total 1248 _reflns_number_gt 596 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1248 _refine_ls_number_parameters 88 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 0.788 _refine_ls_restrained_S_all 0.779 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.011 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na Na 0.5000 0.2500 0.1250 0.0164(3) Uani 1 4 d S . . Al Al 0.30294(2) 0.55294(2) 0.1250 0.01466(15) Uani 1 2 d S . . S S 0.37582(2) 0.39982(2) 0.13783(3) 0.01669(10) Uani 1 1 d . . . Cl Cl 0.5000 0.2500 0.3750 0.0309(2) Uani 1 4 d S . . N N 0.32267(7) 0.23391(6) 0.37653(12) 0.0269(4) Uani 1 1 d D . . O1 O 0.37981(5) 0.48138(5) 0.11043(9) 0.0185(3) Uani 1 1 d . . . O2 O 0.31502(6) 0.36716(6) 0.07200(9) 0.0295(3) Uani 1 1 d . . . O3 O 0.36366(5) 0.39176(5) 0.26733(8) 0.0191(3) Uani 1 1 d . . . O4 O 0.44711(5) 0.36856(6) 0.10786(9) 0.0280(3) Uani 1 1 d . . . O5 O 0.26221(7) 0.5000 0.2500 0.0157(4) Uani 1 2 d SD . . H1 H 0.3013(3) 0.28366(17) 0.3907(5) 0.100(7) Uiso 1 1 d D . . H4 H 0.2835(2) 0.2044(3) 0.3307(4) 0.185(13) Uiso 1 1 d D . . H2 H 0.36767(18) 0.2362(4) 0.3278(4) 0.142(10) Uiso 1 1 d D . . H3 H 0.3311(4) 0.2075(3) 0.4526(3) 0.129(9) Uiso 1 1 d D . . H5 H 0.2127(3) 0.5000 0.2500 0.028(6) Uiso 1 2 d SD . . 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 Na 0.0142(3) 0.0142(3) 0.0209(6) 0.000 0.000 0.000 Al 0.01561(19) 0.01561(19) 0.0127(3) 0.0007(2) -0.0007(2) -0.0004(3) S 0.01877(18) 0.01773(18) 0.01358(17) -0.00127(16) 0.00060(16) 0.00277(16) Cl 0.0320(3) 0.0320(3) 0.0286(4) 0.000 0.000 0.0016(4) N 0.0361(8) 0.0217(7) 0.0229(7) 0.0012(7) 0.0071(8) 0.0079(6) O1 0.0189(5) 0.0150(6) 0.0216(6) 0.0031(4) 0.0040(5) 0.0007(5) O2 0.0332(6) 0.0276(7) 0.0276(6) -0.0077(5) -0.0130(5) -0.0022(6) O3 0.0224(6) 0.0207(5) 0.0143(5) 0.0026(4) 0.0050(4) 0.0039(4) O4 0.0265(6) 0.0276(6) 0.0300(6) 0.0054(6) 0.0124(5) 0.0125(5) O5 0.0143(7) 0.0161(8) 0.0165(7) 0.0046(7) 0.000 0.000 _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 Na O4 2.3599(11) . ? Na O4 2.3599(11) 2_655 ? Na O4 2.3600(11) 32_565 ? Na O4 2.3600(11) 23_656 ? Na Cl 2.8299(7) 19_655 ? Na Cl 2.8299(7) . ? Al O5 1.8618(7) . ? Al O5 1.8619(7) 6_455 ? Al O1 1.9099(10) 6_455 ? Al O1 1.9098(10) . ? Al O3 1.9233(10) 16_544 ? Al O3 1.9233(10) 3_565 ? S O4 1.4506(11) . ? S O2 1.4556(11) . ? S O3 1.4896(10) . ? S O1 1.5115(10) . ? Cl Na 2.8299(7) 19_656 ? N H1 0.994(3) . ? N H4 1.028(4) . ? N H2 0.986(4) . ? N H3 0.996(4) . ? O3 Al 1.9233(10) 3_565 ? O5 Al 1.8618(7) 3_565 ? O5 H5 0.896(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Na O4 170.57(5) . 2_655 ? O4 Na O4 90.389(4) . 32_565 ? O4 Na O4 90.386(4) 2_655 32_565 ? O4 Na O4 90.386(4) . 23_656 ? O4 Na O4 90.389(4) 2_655 23_656 ? O4 Na O4 170.57(5) 32_565 23_656 ? O4 Na Cl 85.28(3) . 19_655 ? O4 Na Cl 85.28(3) 2_655 19_655 ? O4 Na Cl 94.72(3) 32_565 19_655 ? O4 Na Cl 94.72(3) 23_656 19_655 ? O4 Na Cl 94.72(3) . . ? O4 Na Cl 94.72(3) 2_655 . ? O4 Na Cl 85.28(3) 32_565 . ? O4 Na Cl 85.28(3) 23_656 . ? Cl Na Cl 180.0 19_655 . ? O5 Al O5 99.74(6) . 6_455 ? O5 Al O1 92.35(4) . 6_455 ? O5 Al O1 90.28(4) 6_455 6_455 ? O5 Al O1 90.28(4) . . ? O5 Al O1 92.35(4) 6_455 . ? O1 Al O1 175.92(7) 6_455 . ? O5 Al O3 169.31(5) . 16_544 ? O5 Al O3 90.77(4) 6_455 16_544 ? O1 Al O3 89.50(4) 6_455 16_544 ? O1 Al O3 87.35(4) . 16_544 ? O5 Al O3 90.77(4) . 3_565 ? O5 Al O3 169.31(5) 6_455 3_565 ? O1 Al O3 87.35(4) 6_455 3_565 ? O1 Al O3 89.50(4) . 3_565 ? O3 Al O3 78.80(6) 16_544 3_565 ? O4 S O2 113.29(6) . . ? O4 S O3 108.88(6) . . ? O2 S O3 110.61(6) . . ? O4 S O1 106.93(6) . . ? O2 S O1 109.18(6) . . ? O3 S O1 107.75(6) . . ? Na Cl Na 180.0 19_656 . ? H1 N H4 106.6(4) . . ? H1 N H2 112.0(5) . . ? H4 N H2 108.0(4) . . ? H1 N H3 110.7(4) . . ? H4 N H3 107.0(4) . . ? H2 N H3 112.2(5) . . ? S O1 Al 127.66(6) . . ? S O3 Al 131.09(6) . 3_565 ? S O4 Na 134.24(6) . . ? Al O5 Al 133.30(7) . 3_565 ? Al O5 H5 113.35(4) . . ? Al O5 H5 113.35(4) 3_565 . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 29.31 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.333 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.092