Hemi(piperazinediium) hexaaquaaluminium(III) bis(sulfate) tetrahydrate: a new double aluminium sulfate salt
Bataille, Thierry; Acta Crystallographica Section C 59 (2003) m459–m461; doi:10.1107/S0108270103021243

data_2013564
_publ_section_title
;
 Hemi(piperazinediium) hexaaquaaluminium(III) bis(sulfate)
 tetrahydrate: a new double aluminium sulfate salt
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m459
_journal_page_last               m461
_journal_paper_doi               10.1107/S0108270103021243
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Al (H2 O)6]2 (C4 H12 N2) (S O4)4, 8H2 O'
_chemical_formula_moiety         '2(H12 Al O6), C4 H12 N2, 4(O4 S), 8(H2 O)'
_chemical_formula_sum            'C4 H32 Al2 N2 O36 S4'
_chemical_formula_weight         886.64
_chemical_name_common            'aluminium piperazinium sulfate decahydrate'
_chemical_name_systematic
;
Hexaaquaaluminium hemi(piperidin-1,4-diium) bis(sulfate) tetrahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0815(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.57370(10)
_cell_length_b                   12.0671(2)
_cell_length_c                   21.5206(5)
_cell_measurement_reflns_used    11232
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1707.13(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) and Scalepack'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19066
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.9668
_exptl_absorpt_correction_T_min  0.7966
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.470
_refine_ls_extinction_coef       0.0181(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3911
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.047P)^2^+0.84P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                2991
_reflns_number_total             3911
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn1030.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_moiety     'H12 Al O6, 0.5(C4 H12 N2), 2(O4 S), 4(H2 O)'
_cod_original_formula_iupac      '[Al (H2 O)6] (C4 H12 N2)0.5 (S O4)2, 4H2 O'
_cod_original_formula_sum        'C2 H26 Al N O18 S2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     443.32
_cod_database_code               2013564
_cod_database_fobs_code          2013564