1,4,8,11-Tetraazacyclodecane-1,4,8,11-tetraium bis(aquapentafluoroaluminate) dihydrate
Goreshnik, E.; Leblanc, M.; Maisonneuve, V.; Acta Crystallographica, Section E: Structure Reports Online 59 (2003) 1059–1061; doi:10.1107/S1600536803023699

data_3500078
_publ_section_title
;
 1,4,8,11-Tetraazacyclodecane-1,4,8,11-tetraium
 bis(aquapentafluoroaluminate) dihydrate
;
_journal_coden_ASTM              ACSEBH
_journal_issue                   11
_journal_name_full
;
 Acta Crystallographica, Section E: Structure Reports Online
;
_journal_page_first              1059
_journal_page_last               1061
_journal_paper_doi               10.1107/S1600536803023699
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C10 H28 N4) [Al F5 (H2 O)]2, 2H2 O'
_chemical_formula_moiety         'C10 H28 N4 1+, 2Al F5 H2 O 2-, 2H2 O'
_chemical_formula_sum            'C10 H36 Al2 F10 N4 O4'
_chemical_formula_weight         520.3675
_chemical_name_systematic
;
1,4,8,11-Tetraazacyclodecane-1,4,8,11-tetraium
bis(aquapentafluoroaluminate) dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.141(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4930(8)
_cell_length_b                   8.9320(10)
_cell_length_c                   13.434(2)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      2.5
_cell_volume                     1011.2(2)
_computing_cell_refinement       'STADI4 (Stoe & Cie, 1998)'
_computing_data_collection       'STADI4 (Stoe & Cie, 1998)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1998)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2001), ORTEPIII (Burnett & Johnson, 1996)
and ORTEP-3 Farrugia, 1997)
;
_computing_publication_material  'enCIFer (CCDC, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens AED2'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0919
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2955
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        15
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_special_details
;
?
;
_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.
;
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.468
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2955
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1639
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.517P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1508
_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.
;
_reflns_number_gt                1591
_reflns_number_total             2955
_reflns_threshold_expression     I>2\s(I)
_cod_duplicate_entry             1100118
_cod_data_source_file            1100118.cif
_cod_data_source_block           1100118
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               3500078