#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/01/2240183.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2240183
loop_
_publ_author_name
'Abdi, Insaf'
'Al-Sadhan, Khulood'
'Ben Ali, Amor'
_publ_section_title
;
 Crystal structure of bis(propane-1,3-diaminium) hexafluoridoaluminate
 diaquatetrafluoridoaluminate tetrahydrate
;
_journal_coeditor_code           CV5471
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              471
_journal_page_last               473
_journal_paper_doi               10.1107/S1600536814024155
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C3 H12 N2)2 [Al F6] [Al F4 (H2 O)2], 4H2 O'
_chemical_formula_moiety
'2(C3 H12 N2 2+), Al F6 3-, Al F4 H4 O2 -, 4(H2 O)'
_chemical_formula_sum            'C6 H36 Al2 F10 N4 O6'
_chemical_formula_weight         504.35
_chemical_name_systematic
;
Bis(propane-1,3-diaminium) hexafluoridoaluminate
diaquatetrafluoridoaluminate tetrahydrate
;
_space_group_IT_number           65
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2'
_symmetry_space_group_name_H-M   'C m m m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.975(5)
_cell_length_b                   25.115(9)
_cell_length_c                   6.452(9)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2
_cell_volume                     2102(3)
_computing_cell_refinement
;
STADI4  (Stoe & Cie, 2002)
;
_computing_data_collection
;
STADI4 (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXS97 (Sheldrick, 2008) within
WinGX (Farrugia, 2012)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Siemens AED2'
_diffrn_measurement_method       '2θ/ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1371
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelets
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.481
_refine_ls_extinction_coef       0.0022(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
WinGX (Farrugia, 2012)
;
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1371
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0471
_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/[σ²(Fo²)+(0.0452P)²+2.9098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                939
_reflns_number_total             1371
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv5471sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        2103(3)
_cod_original_sg_symbol_Hall     '-C 2 2 '
_cod_database_code               2240183
_cod_database_fobs_code          2240183
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Al Al1 0.0000 0.37606(7) 0.0000 0.0234(4) Uani d S 1 4
Al Al2 0.2500 0.2500 -0.5000 0.0245(4) Uani d S 1 4
F F1 0.0000 0.42435(10) 0.2015(4) 0.0382(6) Uani d S 1 2
F F2 0.13615(17) 0.37342(11) 0.0000 0.0374(6) Uani d S 1 2
F F3 0.2107(2) 0.18091(10) -0.5000 0.0493(8) Uani d S 1 2
F F5 0.15743(14) 0.26362(8) -0.7007(3) 0.0447(5) Uani d . 1 1
N N1 0.3125(2) 0.31814(15) 0.0000 0.0325(8) Uani d S 1 2
H H1A 0.2551 0.3375 0.0000 0.049 Uiso calc SR 1 2
H H1B 0.3141 0.2977 0.1126 0.049 Uiso calc PR 0.50 1
H H1C 0.3141 0.2977 -0.1126 0.049 Uiso calc PR 0.50 1
N N2 0.3447(3) 0.09755(14) -0.5000 0.0331(8) Uani d S 1 2
H H2A 0.3055 0.1266 -0.5000 0.050 Uiso calc SR 1 2
H H2B 0.3843 0.0974 -0.6126 0.050 Uiso calc PR 0.50 1
H H2C 0.3843 0.0974 -0.3874 0.050 Uiso calc PR 0.50 1
C C1 0.4029(3) 0.35390(18) 0.0000 0.0375(11) Uani d S 1 2
H H1D 0.4014 0.3765 0.1219 0.045 Uiso calc PR 0.50 1
H H1E 0.4014 0.3765 -0.1219 0.045 Uiso calc PR 0.50 1
C C2 0.5000 0.3205(2) 0.0000 0.0336(14) Uani d S 1 4
H H2D 0.5000 0.2977 0.1215 0.040 Uiso calc SPR 0.50 2
H H2E 0.5000 0.2977 -0.1215 0.040 Uiso calc SPR 0.50 2
C C3 0.2784(3) 0.04975(18) -0.5000 0.0415(11) Uani d S 1 2
H H3A 0.2346 0.0501 -0.6217 0.050 Uiso calc PR 0.50 1
H H3B 0.2346 0.0501 -0.3783 0.050 Uiso calc PR 0.50 1
C C4 0.3432(5) 0.0000 -0.5000 0.0427(16) Uani d S 1 4
H H4A 0.3872 0.0000 -0.6215 0.051 Uiso calc SPR 0.50 2
H H4B 0.3872 0.0000 -0.3785 0.051 Uiso calc SPR 0.50 2
O OW1 0.0000 0.32173(12) 0.2146(6) 0.0400(8) Uani d SD 1 2
O OW2 0.0000 0.1449(3) -0.5000 0.080(2) Uani d SD 1 4
O OW3 0.3272(7) 0.0000 0.0000 0.104(3) Uani d SD 1 4
O OW4 0.3732(11) 0.5000 0.0000 0.200(6) Uani d SD 1 4
O OW5 0.5000 0.5374(6) 0.342(2) 0.110(4) Uani d SPD 0.50 2
H H1 0.0517(4) 0.3034(11) 0.241(9) 0.165 Uiso d D 1 1
H H2 0.0517(4) 0.1650(8) -0.5000 0.165 Uiso d SD 1 2
H H3 0.3669(15) 0.0267(2) 0.0000 0.165 Uiso d SD 1 2
H H4 0.4125(17) 0.5000 -0.1039(8) 0.165 Uiso d SD 1 2
H H5 0.5516(4) 0.526(5) 0.408(12) 0.165 Uiso d PD 0.50 1
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
F2 Al1 F2 11 . 175.7(2)
F2 Al1 F1 11 . 91.47(7)
F2 Al1 F1 . . 91.47(7)
F2 Al1 F1 11 10 91.47(7)
F2 Al1 F1 . 10 91.47(7)
F1 Al1 F1 . 10 94.0(2)
F2 Al1 OW1 11 . 88.49(7)
F2 Al1 OW1 . . 88.49(7)
F1 Al1 OW1 . . 87.59(16)
F1 Al1 OW1 10 . 178.44(16)
F2 Al1 OW1 11 10 88.49(7)
F2 Al1 OW1 . 10 88.49(7)
F1 Al1 OW1 . 10 178.44(16)
F1 Al1 OW1 10 10 87.60(16)
OW1 Al1 OW1 . 10 90.8(2)
F5 Al2 F5 13_554 . 180.00(14)
F5 Al2 F5 13_554 10_554 87.92(14)
F5 Al2 F5 . 10_554 92.08(14)
F5 Al2 F5 13_554 6 92.08(14)
F5 Al2 F5 . 6 87.92(14)
F5 Al2 F5 10_554 6 180.00(13)
F5 Al2 F3 13_554 . 90.34(9)
F5 Al2 F3 . . 89.66(9)
F5 Al2 F3 10_554 . 89.66(9)
F5 Al2 F3 6 . 90.34(9)
F5 Al2 F3 13_554 13_554 89.66(9)
F5 Al2 F3 . 13_554 90.34(9)
F5 Al2 F3 10_554 13_554 90.34(9)
F5 Al2 F3 6 13_554 89.66(9)
F3 Al2 F3 . 13_554 180.0
C1 N1 H1A . . 109.5
C1 N1 H1B . . 109.5
H1A N1 H1B . . 109.5
C1 N1 H1C . . 109.5
H1A N1 H1C . . 109.5
H1B N1 H1C . . 109.5
C3 N2 H2A . . 109.5
C3 N2 H2B . . 109.5
H2A N2 H2B . . 109.5
C3 N2 H2C . . 109.5
H2A N2 H2C . . 109.5
H2B N2 H2C . . 109.5
N1 C1 C2 . . 108.9(4)
N1 C1 H1D . . 109.9
C2 C1 H1D . . 109.9
N1 C1 H1E . . 109.9
C2 C1 H1E . . 109.9
H1D C1 H1E . . 108.3
C1 C2 C1 11_655 . 112.7(5)
C1 C2 H2D 11_655 . 109.1
C1 C2 H2D . . 109.1
C1 C2 H2E 11_655 . 109.1
C1 C2 H2E . . 109.1
H2D C2 H2E . . 107.8
N2 C3 C4 . . 110.5(4)
N2 C3 H3A . . 109.6
C4 C3 H3A . . 109.6
N2 C3 H3B . . 109.6
C4 C3 H3B . . 109.6
H3A C3 H3B . . 108.1
C3 C4 C3 3_554 . 112.2(5)
C3 C4 H4A 3_554 . 109.2
C3 C4 H4A . . 109.2
C3 C4 H4B 3_554 . 109.2
C3 C4 H4B . . 109.2
H4A C4 H4B . . 107.9
Al1 OW1 H1 . . 122(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Al1 F2 11 1.768(2)
Al1 F2 . 1.768(2)
Al1 F1 . 1.778(3)
Al1 F1 10 1.778(3)
Al1 OW1 . 1.944(4)
Al1 OW1 10 1.944(4)
Al2 F5 13_554 1.799(2)
Al2 F5 . 1.799(2)
Al2 F5 10_554 1.799(2)
Al2 F5 6 1.799(2)
Al2 F3 . 1.809(3)
Al2 F3 13_554 1.809(3)
N1 C1 . 1.476(6)
N1 H1A . 0.8900
N1 H1B . 0.8900
N1 H1C . 0.8900
N2 C3 . 1.477(6)
N2 H2A . 0.8900
N2 H2B . 0.8900
N2 H2C . 0.8900
C1 C2 . 1.514(5)
C1 H1D . 0.9700
C1 H1E . 0.9700
C2 C1 11_655 1.514(5)
C2 H2D . 0.9700
C2 H2E . 0.9700
C3 C4 . 1.505(5)
C3 H3A . 0.9700
C3 H3B . 0.9700
C4 C3 3_554 1.505(5)
C4 H4A . 0.9700
C4 H4B . 0.9700
OW1 H1 . 0.831(10)
OW2 H2 . 0.840(10)
OW3 H3 . 0.846(10)
OW4 H4 . 0.842(10)
OW5 H5 . 0.840(10)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A F2 . 0.89 1.79 2.679(6) 177 yes
N1 H1B F5 6_556 0.89 1.99 2.846(5) 161 yes
N1 H1C F5 13_554 0.89 1.99 2.846(5) 161 yes
N2 H2A F3 . 0.89 1.84 2.722(6) 173 yes
N2 H2B F1 6_554 0.89 2.00 2.841(5) 158 yes
Ow1 H1 F5 1_556 0.83(4) 1.74(4) 2.569(5) 178 yes
Ow2 H2 F3 . 0.84(4) 2.10(4) 2.880(5) 178 yes
Ow4 H4 Ow5 10_555 0.84(4) 2.131 2.910(5) 154 yes
