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