#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/97/2019729.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_2019729
loop_
_publ_author_name
'Tillmann, Jan'
'Lerner, Hans-Wolfram'
'Bolte, Michael'
_publ_section_title
;
 Two ammonium tetrachloridoaluminate salts: how a twinned orthorhombic
 structure emulates a trigonal crystal system
;
_journal_coeditor_code           SK3567
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229614022621
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C8 H20 N) [Al Cl4]'
_chemical_formula_moiety         'C8 H20 N +, Al Cl4 -'
_chemical_formula_sum            'C8 H20 Al Cl4 N'
_chemical_formula_weight         299.03
_chemical_name_systematic
;
Tetraethylammonium tetrachloridoaluminate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0348(10)
_cell_length_b                   8.1362(7)
_cell_length_c                   12.8892(12)
_cell_measurement_reflns_used    13398
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      3.21
_cell_volume                     1471.8(2)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2001)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2001)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2001)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al., 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010), SHELXL97 (Sheldrick, 2008) and PLATON
(Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97(Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Stoe IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6472
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.843
_diffrn_reflns_theta_min         4.034
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
X-AREA (Stoe & Cie, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.146
_refine_ls_abs_structure_details
;
Flack x determined using 1046 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2522
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0263P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0518
_reflns_number_gt                2423
_reflns_number_total             2522
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sk3567sup1.cif
_cod_data_source_block           II
_cod_database_code               2019729
_cod_database_fobs_code          2019729
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.921
_shelxl_version_number           2014/6
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
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_occupancy
Al Al1 0.24065(8) 0.72153(13) 0.52107(7) 0.0232(2) Uani d 1
Cl Cl1 0.10146(7) 0.69274(11) 0.45644(7) 0.0306(2) Uani d 1
Cl Cl2 0.23073(8) 0.72358(13) 0.68639(6) 0.0335(2) Uani d 1
Cl Cl3 0.32847(7) 0.52335(10) 0.47060(7) 0.0309(2) Uani d 1
Cl Cl4 0.30042(7) 0.95065(10) 0.47242(7) 0.0334(2) Uani d 1
N N1 0.0859(2) 0.2192(4) 0.2809(2) 0.0203(6) Uani d 1
C C1 0.0915(3) 0.0357(4) 0.2601(3) 0.0253(8) Uani d 1
H H1A 0.1239 0.0186 0.1927 0.030 Uiso calc 1
H H1B 0.1315 -0.0154 0.3145 0.030 Uiso calc 1
C C2 -0.0035(3) -0.0524(5) 0.2574(3) 0.0315(9) Uani d 1
H H2A 0.0069 -0.1695 0.2435 0.047 Uiso calc 1
H H2B -0.0356 -0.0394 0.3244 0.047 Uiso calc 1
H H2C -0.0433 -0.0053 0.2024 0.047 Uiso calc 1
C C3 0.1843(3) 0.2859(5) 0.2990(3) 0.0262(8) Uani d 1
H H3A 0.2099 0.2359 0.3632 0.031 Uiso calc 1
H H3B 0.1793 0.4057 0.3110 0.031 Uiso calc 1
C C4 0.2555(4) 0.2571(5) 0.2122(4) 0.0392(10) Uani d 1
H H4A 0.3171 0.3049 0.2314 0.059 Uiso calc 1
H H4B 0.2630 0.1387 0.2007 0.059 Uiso calc 1
H H4C 0.2323 0.3091 0.1484 0.059 Uiso calc 1
C C5 0.0245(3) 0.2566(4) 0.3755(3) 0.0253(8) Uani d 1
H H5A 0.0255 0.3767 0.3878 0.030 Uiso calc 1
H H5B -0.0421 0.2254 0.3596 0.030 Uiso calc 1
C C6 0.0545(3) 0.1703(5) 0.4745(3) 0.0353(9) Uani d 1
H H6A 0.0113 0.2014 0.5309 0.053 Uiso calc 1
H H6B 0.0519 0.0511 0.4641 0.053 Uiso calc 1
H H6C 0.1197 0.2028 0.4924 0.053 Uiso calc 1
C C7 0.0390(3) 0.2995(4) 0.1872(3) 0.0247(8) Uani d 1
H H7A 0.0794 0.2792 0.1255 0.030 Uiso calc 1
H H7B -0.0232 0.2453 0.1748 0.030 Uiso calc 1
C C8 0.0225(3) 0.4827(5) 0.1968(3) 0.0318(9) Uani d 1
H H8A -0.0078 0.5237 0.1333 0.048 Uiso calc 1
H H8B -0.0191 0.5045 0.2563 0.048 Uiso calc 1
H H8C 0.0837 0.5385 0.2069 0.048 Uiso calc 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'
Al Al 0.0645 0.0514 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cl3 Al1 Cl2 110.38(6) y
Cl3 Al1 Cl1 109.08(6) y
Cl2 Al1 Cl1 109.29(7) y
Cl3 Al1 Cl4 110.07(6) y
Cl2 Al1 Cl4 108.14(6) y
Cl1 Al1 Cl4 109.87(6) y
C3 N1 C1 109.5(3) y
C3 N1 C5 108.9(3) y
C1 N1 C5 111.6(3) y
C3 N1 C7 111.4(3) y
C1 N1 C7 107.7(3) y
C5 N1 C7 107.7(3) y
C2 C1 N1 115.1(3) ?
C2 C1 H1A 108.5 ?
N1 C1 H1A 108.5 ?
C2 C1 H1B 108.5 ?
N1 C1 H1B 108.5 ?
H1A C1 H1B 107.5 ?
C1 C2 H2A 109.5 ?
C1 C2 H2B 109.5 ?
H2A C2 H2B 109.5 ?
C1 C2 H2C 109.5 ?
H2A C2 H2C 109.5 ?
H2B C2 H2C 109.5 ?
N1 C3 C4 115.8(3) ?
N1 C3 H3A 108.3 ?
C4 C3 H3A 108.3 ?
N1 C3 H3B 108.3 ?
C4 C3 H3B 108.3 ?
H3A C3 H3B 107.4 ?
C3 C4 H4A 109.5 ?
C3 C4 H4B 109.5 ?
H4A C4 H4B 109.5 ?
C3 C4 H4C 109.5 ?
H4A C4 H4C 109.5 ?
H4B C4 H4C 109.5 ?
C6 C5 N1 115.0(3) ?
C6 C5 H5A 108.5 ?
N1 C5 H5A 108.5 ?
C6 C5 H5B 108.5 ?
N1 C5 H5B 108.5 ?
H5A C5 H5B 107.5 ?
C5 C6 H6A 109.5 ?
C5 C6 H6B 109.5 ?
H6A C6 H6B 109.5 ?
C5 C6 H6C 109.5 ?
H6A C6 H6C 109.5 ?
H6B C6 H6C 109.5 ?
C8 C7 N1 115.1(3) ?
C8 C7 H7A 108.5 ?
N1 C7 H7A 108.5 ?
C8 C7 H7B 108.5 ?
N1 C7 H7B 108.5 ?
H7A C7 H7B 107.5 ?
C7 C8 H8A 109.5 ?
C7 C8 H8B 109.5 ?
H8A C8 H8B 109.5 ?
C7 C8 H8C 109.5 ?
H8A C8 H8C 109.5 ?
H8B C8 H8C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 Cl3 2.1313(14) y
Al1 Cl2 2.1354(11) y
Al1 Cl1 2.1365(14) y
Al1 Cl4 2.1383(14) y
N1 C3 1.503(5) y
N1 C1 1.519(4) y
N1 C5 1.523(4) y
N1 C7 1.524(4) y
C1 C2 1.514(5) y
C1 H1A 0.9900 ?
C1 H1B 0.9900 ?
C2 H2A 0.9800 ?
C2 H2B 0.9800 ?
C2 H2C 0.9800 ?
C3 C4 1.518(6) ?
C3 H3A 0.9900 ?
C3 H3B 0.9900 ?
C4 H4A 0.9800 ?
C4 H4B 0.9800 ?
C4 H4C 0.9800 ?
C5 C6 1.516(5) ?
C5 H5A 0.9900 ?
C5 H5B 0.9900 ?
C6 H6A 0.9800 ?
C6 H6B 0.9800 ?
C6 H6C 0.9800 ?
C7 C8 1.513(5) ?
C7 H7A 0.9900 ?
C7 H7B 0.9900 ?
C8 H8A 0.9800 ?
C8 H8B 0.9800 ?
C8 H8C 0.9800 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C3 N1 C1 C2 170.8(3)
C5 N1 C1 C2 50.1(4)
C7 N1 C1 C2 -67.9(4)
C1 N1 C3 C4 57.0(4)
C5 N1 C3 C4 179.3(3)
C7 N1 C3 C4 -62.0(4)
C3 N1 C5 C6 -65.5(4)
C1 N1 C5 C6 55.6(4)
C7 N1 C5 C6 173.6(3)
C3 N1 C7 C8 -63.0(4)
C1 N1 C7 C8 176.8(3)
C5 N1 C7 C8 56.4(4)
