#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:25:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179411 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/08/4330854.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_4330854
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         'C20 H20 Al F2 N4, I'
_chemical_formula_sum            'C20 H20 Al F2 I N4'
_chemical_formula_weight         508.28
_chemical_name_common
; 
  trans-Difluoro-tetrakis(pyridine)-aluminium iodide 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 119.816(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1899(16)
_cell_length_b                   12.2837(14)
_cell_length_c                   13.0435(14)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     2111.6(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        XPREP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12316
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.37
_diffrn_source
'sealed x-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           45
_diffrn_source_power             2.25
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_T_max  0.7631
_exptl_absorpt_correction_T_min  0.61542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   PLATON
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.055
_refine_diff_density_min         -2.116
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0549
_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)+(0.0437P)²+13.4383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                2554
_reflns_number_total             2825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301502u_si_001_3.cif
_cod_data_source_block           2vc
_cod_database_code               4330854
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
C1 C 0.3967(3) 0.6342(4) 0.1027(4) 0.0198(8) Uani 1 1 d .
H1 H 0.3751 0.5646 0.1134 0.024 Uiso 1 1 calc R
C2 C 0.3619(4) 0.7264(4) 0.1335(4) 0.0227(9) Uani 1 1 d .
H2 H 0.3169 0.7196 0.1640 0.027 Uiso 1 1 calc R
C3 C 0.3935(4) 0.8279(4) 0.1192(4) 0.0212(9) Uani 1 1 d .
H3 H 0.3703 0.8920 0.1391 0.025 Uiso 1 1 calc R
C4 C 0.4598(4) 0.8342(4) 0.0752(4) 0.0212(9) Uani 1 1 d .
H4 H 0.4837 0.9029 0.0659 0.025 Uiso 1 1 calc R
C5 C 0.4909(3) 0.7393(3) 0.0448(4) 0.0182(8) Uani 1 1 d .
H5 H 0.5353 0.7446 0.0134 0.022 Uiso 1 1 calc R
C6 C 0.6197(3) 0.3892(4) 0.2345(4) 0.0189(8) Uani 1 1 d .
H6 H 0.5590 0.3480 0.2059 0.023 Uiso 1 1 calc R
C7 C 0.7013(4) 0.3637(4) 0.3450(4) 0.0210(9) Uani 1 1 d .
H7 H 0.6962 0.3055 0.3898 0.025 Uiso 1 1 calc R
C8 C 0.7898(4) 0.4236(4) 0.3892(4) 0.0231(9) Uani 1 1 d .
H8 H 0.8458 0.4090 0.4654 0.028 Uiso 1 1 calc R
C9 C 0.7943(4) 0.5060(4) 0.3184(4) 0.0230(9) Uani 1 1 d .
H9 H 0.8542 0.5483 0.3455 0.028 Uiso 1 1 calc R
C10 C 0.7110(3) 0.5259(4) 0.2083(4) 0.0197(8) Uani 1 1 d .
H10 H 0.7157 0.5811 0.1603 0.024 Uiso 1 1 calc R
Al1 Al 0.5000 0.5000 0.0000 0.0147(3) Uani 1 2 d S
F1 F 0.4232(2) 0.4225(2) 0.0337(2) 0.0170(5) Uani 1 1 d .
I1 I 0.5000 0.11771(3) 0.2500 0.01743(12) Uani 1 2 d S
N1 N 0.4603(3) 0.6398(3) 0.0581(3) 0.0160(7) Uani 1 1 d .
N2 N 0.6228(3) 0.4695(3) 0.1664(3) 0.0167(7) Uani 1 1 d .
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'
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'
I I -0.4742 1.8119 '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'
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
N1 C1 C2 122.5(4) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C3 C2 C1 119.2(4) . .
C3 C2 H2 120.4 . .
C1 C2 H2 120.4 . .
C2 C3 C4 118.6(4) . .
C2 C3 H3 120.7 . .
C4 C3 H3 120.7 . .
C3 C4 C5 119.5(4) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
N1 C5 C4 122.4(4) . .
N1 C5 H5 118.8 . .
C4 C5 H5 118.8 . .
N2 C6 C7 123.0(4) . .
N2 C6 H6 118.5 . .
C7 C6 H6 118.5 . .
C8 C7 C6 119.5(4) . .
C8 C7 H7 120.2 . .
C6 C7 H7 120.2 . .
C7 C8 C9 117.9(4) . .
C7 C8 H8 121.0 . .
C9 C8 H8 121.0 . .
C10 C9 C8 119.6(4) . .
C10 C9 H9 120.2 . .
C8 C9 H9 120.2 . .
N2 C10 C9 122.6(4) . .
N2 C10 H10 118.7 . .
C9 C10 H10 118.7 . .
F1 Al1 F1 179.998(1) . 5_665
F1 Al1 N2 90.22(13) . .
F1 Al1 N2 89.78(13) 5_665 .
F1 Al1 N2 89.78(13) . 5_665
F1 Al1 N2 90.22(13) 5_665 5_665
N2 Al1 N2 180.0 . 5_665
F1 Al1 N1 89.56(13) . 5_665
F1 Al1 N1 90.44(13) 5_665 5_665
N2 Al1 N1 87.69(14) . 5_665
N2 Al1 N1 92.31(14) 5_665 5_665
F1 Al1 N1 90.44(13) . .
F1 Al1 N1 89.56(13) 5_665 .
N2 Al1 N1 92.31(14) . .
N2 Al1 N1 87.69(14) 5_665 .
N1 Al1 N1 180.0 5_665 .
C5 N1 C1 117.8(4) . .
C5 N1 Al1 121.3(3) . .
C1 N1 Al1 120.7(3) . .
C6 N2 C10 117.4(4) . .
C6 N2 Al1 121.0(3) . .
C10 N2 Al1 121.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.355(5) .
C1 C2 1.391(6) .
C1 H1 0.9500 .
C2 C3 1.382(6) .
C2 H2 0.9500 .
C3 C4 1.387(7) .
C3 H3 0.9500 .
C4 C5 1.388(6) .
C4 H4 0.9500 .
C5 N1 1.348(5) .
C5 H5 0.9500 .
C6 N2 1.344(5) .
C6 C7 1.391(6) .
C6 H6 0.9500 .
C7 C8 1.382(7) .
C7 H7 0.9500 .
C8 C9 1.395(7) .
C8 H8 0.9500 .
C9 C10 1.384(7) .
C9 H9 0.9500 .
C10 N2 1.358(6) .
C10 H10 0.9500 .
Al1 F1 1.724(2) .
Al1 F1 1.724(2) 5_665
Al1 N2 2.075(4) .
Al1 N2 2.075(4) 5_665
Al1 N1 2.084(3) 5_665
Al1 N1 2.084(3) .
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
_geom_torsion_site_symmetry_1
N1 C1 C2 C3 -0.5(7) .
C1 C2 C3 C4 -0.5(7) .
C2 C3 C4 C5 1.2(7) .
C3 C4 C5 N1 -1.1(7) .
N2 C6 C7 C8 1.0(7) .
C6 C7 C8 C9 -1.9(7) .
C7 C8 C9 C10 0.7(7) .
C8 C9 C10 N2 1.5(7) .
C4 C5 N1 C1 0.2(6) .
C4 C5 N1 Al1 175.4(3) .
C2 C1 N1 C5 0.6(7) .
C2 C1 N1 Al1 -174.7(3) .
F1 Al1 N1 C5 -173.8(3) .
F1 Al1 N1 C5 6.2(3) 5_665
N2 Al1 N1 C5 96.0(3) .
N2 Al1 N1 C5 -84.0(3) 5_665
F1 Al1 N1 C1 1.4(3) .
F1 Al1 N1 C1 -178.6(3) 5_665
N2 Al1 N1 C1 -88.9(3) .
N2 Al1 N1 C1 91.1(3) 5_665
C7 C6 N2 C10 1.2(6) .
C7 C6 N2 Al1 177.9(3) .
C9 C10 N2 C6 -2.4(6) .
C9 C10 N2 Al1 -179.1(3) .
F1 Al1 N2 C6 15.3(3) .
F1 Al1 N2 C6 -164.7(3) 5_665
N1 Al1 N2 C6 -74.2(3) 5_665
N1 Al1 N2 C6 105.8(3) .
F1 Al1 N2 C10 -168.1(3) .
F1 Al1 N2 C10 11.9(3) 5_665
N1 Al1 N2 C10 102.4(3) 5_665
N1 Al1 N2 C10 -77.6(3) .
