#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:25:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179411 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/08/4330852.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4330852
loop_
_publ_author_name
'Anton Dimitrov'
'Detlef Heidemann'
'Khalaf I. Khallow'
'Erhard Kemnitz'
_publ_contact_author
;
      Prof. Dr. Erhard Kemnitz
      Institut für Chemie
      Humboldt-Universität zu Berlin
      Brook-Taylor Str.2
      12489 Berlin, 
      Germany
;
_publ_contact_author_email       erhard.kemnitz@chemie.hu-berlin.de
_publ_contact_author_fax         '+49 30 20937277'
_publ_contact_author_phone       '+49 30 20937555'
_publ_section_title
;
 Syntheses and Characterization of Salts with the [Al(D)4F2]+ Cation (D =
 Pyridine or Water)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11612
_journal_page_last               11622
_journal_paper_doi               10.1021/ic301502u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'Al F2 H8 O4, 2(C5 H6 N), 3(Cl)'
_chemical_formula_sum            'C10 H20 Al Cl3 F2 N2 O4'
_chemical_formula_weight         403.61
_chemical_name_systematic
; 
 trans-Difluoro-tetrakis(aqua)-aluminium bis(pyridinium) trichloride 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 103.089(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.0967(3)
_cell_length_b                   19.7672(11)
_cell_length_c                   9.0423(7)
_cell_measurement_reflns_used    2543
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.53
_cell_measurement_theta_min      2.29
_cell_volume                     887.32(10)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'PLATON, 1990'
_computing_publication_material  'PLATON, 1990'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       'ω-rotation,ω-incr.=1°,319 exposures'
_diffrn_radiation_collimation    '0.5 mm diameter monocapillary'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'long fine focus sealed x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18004
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.9480
_exptl_absorpt_correction_T_min  0.8894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON, 1990'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       plate
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2105
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0388
_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)+(0.0359P)²+0.2339P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                1799
_reflns_number_total             2105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301502u_si_001_1.cif
_cod_data_source_block           V4
_cod_database_code               4330852
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
Al1 Al 0.08721(14) 0.2500 0.83678(8) 0.01292(16) Uani 1 2 d S . .
F1 F -0.2190(3) 0.2500 0.70246(16) 0.0174(3) Uani 1 2 d S . .
F2 F 0.3956(3) 0.2500 0.96983(16) 0.0189(3) Uani 1 2 d S . .
O1 O 0.2749(3) 0.2500 0.6783(2) 0.0215(4) Uani 1 2 d S . .
H1A H 0.4505 0.2500 0.6780 0.047(12) Uiso 1 2 d SR . .
H1B H 0.2026 0.2500 0.5743 0.051(12) Uiso 1 2 d SR . .
O2 O 0.0889(3) 0.15307(7) 0.84237(17) 0.0265(3) Uani 1 1 d . . .
H2A H -0.0410 0.1311 0.8236 0.058(10) Uiso 1 1 d R . .
H2B H 0.2195 0.1327 0.8333 0.038(8) Uiso 1 1 d R . .
O3 O -0.0997(3) 0.2500 0.9944(2) 0.0221(4) Uani 1 2 d S . .
H3A H -0.2609 0.2500 0.9783 0.036(10) Uiso 1 2 d SR . .
H3B H -0.0401 0.2500 1.0823 0.050(13) Uiso 1 2 d SR . .
Cl1 Cl 0.17325(12) 0.2500 0.32838(6) 0.01828(15) Uani 1 2 d S . .
Cl2 Cl 0.56480(9) 0.07266(3) 0.78437(6) 0.02659(14) Uani 1 1 d . . .
N1A N 0.7367(17) 0.0926(4) 0.1533(7) 0.0163(16) Uani 0.390(13) 1 d PDU A 1
H1A1 H 0.6743 0.0931 0.0542 0.020 Uiso 0.390(13) 1 calc PR A 1
C2A C 0.6016(13) 0.1273(5) 0.2389(15) 0.0220(19) Uani 0.390(13) 1 d PDU A 1
H2A1 H 0.4427 0.1514 0.1933 0.026 Uiso 0.390(13) 1 calc PR A 1
C3A C 0.695(2) 0.1275(5) 0.3926(13) 0.021(2) Uani 0.390(13) 1 d PDU A 1
H3A1 H 0.6016 0.1514 0.4561 0.025 Uiso 0.390(13) 1 calc PR A 1
C4A C 0.927(4) 0.0925(15) 0.454(2) 0.025(3) Uani 0.390(13) 1 d PDU A 1
H4A H 0.9952 0.0925 0.5605 0.030 Uiso 0.390(13) 1 calc PR A 1
C5A C 1.062(3) 0.0573(10) 0.3630(14) 0.019(2) Uani 0.390(13) 1 d PDU A 1
H5A H 1.2236 0.0336 0.4061 0.023 Uiso 0.390(13) 1 calc PR A 1
C6A C 0.9601(19) 0.0571(5) 0.2085(13) 0.0184(17) Uani 0.390(13) 1 d PDU A 1
H6A H 1.0463 0.0323 0.1429 0.022 Uiso 0.390(13) 1 calc PR A 1
N1B N 0.6158(7) 0.1458(3) 0.3032(8) 0.0212(11) Uani 0.610(13) 1 d PDU A 2
H1B1 H 0.4823 0.1746 0.2985 0.025 Uiso 0.610(13) 1 calc PR A 2
C2B C 0.6466(15) 0.1173(4) 0.1755(7) 0.0258(14) Uani 0.610(13) 1 d PDU A 2
H2B1 H 0.5271 0.1282 0.0818 0.031 Uiso 0.610(13) 1 calc PR A 2
C3B C 0.8517(19) 0.0720(3) 0.1793(6) 0.0281(16) Uani 0.610(13) 1 d PDU A 2
H3B1 H 0.8744 0.0507 0.0888 0.034 Uiso 0.610(13) 1 calc PR A 2
C4B C 1.025(2) 0.0579(6) 0.3168(10) 0.027(2) Uani 0.610(13) 1 d PDU A 2
H4B H 1.1696 0.0272 0.3213 0.033 Uiso 0.610(13) 1 calc PR A 2
C5B C 0.987(3) 0.0886(9) 0.4491(15) 0.0231(19) Uani 0.610(13) 1 d PU A 2
H5B H 1.1036 0.0789 0.5444 0.028 Uiso 0.610(13) 1 calc PR A 2
C6B C 0.7771(15) 0.1331(4) 0.4386(7) 0.0220(13) Uani 0.610(13) 1 d PDU A 2
H6B H 0.7469 0.1548 0.5270 0.026 Uiso 0.610(13) 1 calc PR A 2
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'
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'
F F 0.0171 0.0103 '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'
H H 0.0000 0.0000 '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_site_symmetry_1
_geom_angle_site_symmetry_3
F1 Al1 F2 179.43(7) . .
F1 Al1 O3 90.04(8) . .
F2 Al1 O3 90.53(8) . .
F1 Al1 O1 89.93(8) . .
F2 Al1 O1 89.50(8) . .
O3 Al1 O1 179.97(9) . .
F1 Al1 O2 90.94(5) . 4_565
F2 Al1 O2 89.07(5) . 4_565
O3 Al1 O2 88.86(5) . 4_565
O1 Al1 O2 91.14(5) . 4_565
F1 Al1 O2 90.94(5) . .
F2 Al1 O2 89.07(5) . .
O3 Al1 O2 88.86(5) . .
O1 Al1 O2 91.14(5) . .
O2 Al1 O2 177.05(10) 4_565 .
Al1 O1 H1A 132.7 . .
Al1 O1 H1B 127.8 . .
H1A O1 H1B 99.4 . .
Al1 O2 H2A 123.7 . .
Al1 O2 H2B 120.1 . .
H2A O2 H2B 112.5 . .
Al1 O3 H3A 122.3 . .
Al1 O3 H3B 128.3 . .
H3A O3 H3B 109.4 . .
C6A N1A C2A 124.1(9) . .
C6A N1A H1A1 117.9 . .
C2A N1A H1A1 117.9 . .
N1A C2A C3A 119.1(7) . .
N1A C2A H2A1 120.5 . .
C3A C2A H2A1 120.5 . .
C2A C3A C4A 118.5(11) . .
C2A C3A H3A1 120.7 . .
C4A C3A H3A1 120.7 . .
C5A C4A C3A 121.2(16) . .
C5A C4A H4A 119.4 . .
C3A C4A H4A 119.4 . .
C4A C5A C6A 118.8(14) . .
C4A C5A H5A 120.6 . .
C6A C5A H5A 120.6 . .
N1A C6A C5A 118.2(11) . .
N1A C6A H6A 120.9 . .
C5A C6A H6A 120.9 . .
C2B N1B C6B 123.3(5) . .
C2B N1B H1B1 118.4 . .
C6B N1B H1B1 118.4 . .
N1B C2B C3B 119.8(5) . .
N1B C2B H2B1 120.1 . .
C3B C2B H2B1 120.1 . .
C2B C3B C4B 118.8(6) . .
C2B C3B H3B1 120.6 . .
C4B C3B H3B1 120.6 . .
C3B C4B C5B 120.1(8) . .
C3B C4B H4B 120.0 . .
C5B C4B H4B 120.0 . .
C6B C5B C4B 118.5(11) . .
C6B C5B H5B 120.7 . .
C4B C5B H5B 120.7 . .
N1B C6B C5B 119.5(8) . .
N1B C6B H6B 120.2 . .
C5B C6B H6B 120.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 F1 1.7472(16) .
Al1 F2 1.7496(16) .
Al1 O3 1.8855(17) .
Al1 O1 1.8944(17) .
Al1 O2 1.9165(15) 4_565
Al1 O2 1.9166(15) .
O1 H1A 0.8957 .
O1 H1B 0.9294 .
O2 H2A 0.7781 .
O2 H2B 0.7983 .
O3 H3A 0.8009 .
O3 H3B 0.7834 .
N1A C6A 1.334(8) .
N1A C2A 1.336(8) .
N1A H1A1 0.8800 .
C2A C3A 1.363(9) .
C2A H2A1 0.9500 .
C3A C4A 1.374(12) .
C3A H3A1 0.9500 .
C4A C5A 1.373(13) .
C4A H4A 0.9500 .
C5A C6A 1.376(9) .
C5A H5A 0.9500 .
C6A H6A 0.9500 .
N1B C2B 1.326(6) .
N1B C6B 1.335(6) .
N1B H1B1 0.8800 .
C2B C3B 1.371(7) .
C2B H2B1 0.9500 .
C3B C4B 1.380(8) .
C3B H3B1 0.9500 .
C4B C5B 1.393(12) .
C4B H4B 0.9500 .
C5B C6B 1.370(10) .
C5B H5B 0.9500 .
C6B H6B 0.9500 .
