#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:20:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179785 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/81/7008140.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_7008140
loop_
_publ_author_name
'Shukla, Piyush'
'Cowley, Alan H.'
'Jones, Jamie N.'
'Gordon, John C.'
'Scott, Brian L.'
_publ_section_title
;
 Fluoroaryl-substituted aminoalane dimers: syntheses and structures.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1019
_journal_page_last               1022
_journal_paper_doi               10.1039/b417652a
_journal_year                    2005
_chemical_formula_sum            'C16 H16 Al2 F8 N2'
_chemical_formula_weight         442.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.044(7)
_cell_angle_beta                 92.103(8)
_cell_angle_gamma                94.798(9)
_cell_formula_units_Z            2
_cell_length_a                   7.712(3)
_cell_length_b                   9.689(4)
_cell_length_c                   17.153(8)
_cell_measurement_reflns_used    825
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      54.5
_cell_measurement_theta_min      4.8
_cell_volume                     1276.1(9)
_computing_cell_refinement       'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_data_collection       'Siemens SMART (v. 4.202, Siemens 1996)'
_computing_data_reduction        'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_molecular_graphics    'Bruker AXS SHEXTL (v. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker P4 with SMART 1k CCD'
_diffrn_measurement_method       'φ scans'
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6287
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9795
_exptl_absorpt_correction_T_min  0.9532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.537
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.537
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0822
_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)+(0.0849P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2025
_refine_ls_wR_factor_ref         0.2091
_reflns_number_gt                2331
_reflns_number_total             3101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b417652a.txt
_cod_data_source_block           ccd518s
_cod_original_cell_volume        1276.1(10)
_cod_database_code               7008140
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.4319(2) 0.39297(17) 0.14146(10) 0.0324(5) Uani 1 1 d . . .
Al2 Al 0.4638(2) 0.55509(17) 0.28576(10) 0.0313(5) Uani 1 1 d . . .
F1 F 0.0874(4) 0.5375(3) 0.19850(19) 0.0419(9) Uani 1 1 d . . .
F2 F -0.1574(5) 0.6954(4) 0.1412(2) 0.0552(11) Uani 1 1 d . . .
F3 F 0.2732(5) 0.9756(3) 0.0174(2) 0.0531(11) Uani 1 1 d . . .
F4 F 0.5206(5) 0.8211(3) 0.0771(2) 0.0464(10) Uani 1 1 d . . .
F5 F 0.4874(5) 0.3631(3) 0.41376(19) 0.0510(11) Uani 1 1 d . . .
F6 F 0.6169(6) 0.1451(4) 0.4841(2) 0.0632(12) Uani 1 1 d . . .
F7 F 0.5643(5) -0.1062(3) 0.2462(2) 0.0561(11) Uani 1 1 d . . .
F8 F 0.4297(5) 0.1082(3) 0.17626(18) 0.0450(10) Uani 1 1 d . . .
N1 N 0.4400(7) 0.5950(5) 0.1710(3) 0.0305(12) Uani 1 1 d . . .
H1 H 0.538(11) 0.631(8) 0.157(4) 0.080 Uiso 1 1 d . . .
H2 H 0.259(10) 0.316(7) 0.259(4) 0.080 Uiso 1 1 d . . .
N2 N 0.3907(7) 0.3592(4) 0.2541(3) 0.0302(12) Uani 1 1 d . . .
C1 C 0.6657(9) 0.3591(7) 0.1145(4) 0.0493(18) Uani 1 1 d . . .
H1A H 0.7459 0.3932 0.1559 0.074 Uiso 1 1 calc R . .
H1B H 0.6943 0.4059 0.0673 0.074 Uiso 1 1 calc R . .
H1C H 0.6730 0.2614 0.1070 0.074 Uiso 1 1 calc R . .
C2 C 0.2328(9) 0.3361(7) 0.0715(4) 0.0511(19) Uani 1 1 d . . .
H2A H 0.1280 0.3609 0.0946 0.077 Uiso 1 1 calc R . .
H2B H 0.2263 0.2376 0.0629 0.077 Uiso 1 1 calc R . .
H2C H 0.2463 0.3817 0.0226 0.077 Uiso 1 1 calc R . .
C3 C 0.7121(8) 0.5814(6) 0.3136(4) 0.0423(16) Uani 1 1 d . . .
H3A H 0.7757 0.5319 0.2767 0.063 Uiso 1 1 calc R . .
H3B H 0.7328 0.5468 0.3649 0.063 Uiso 1 1 calc R . .
H3C H 0.7501 0.6782 0.3129 0.063 Uiso 1 1 calc R . .
C4 C 0.2946(10) 0.6451(6) 0.3488(4) 0.0516(19) Uani 1 1 d . . .
H4A H 0.1792 0.6221 0.3269 0.077 Uiso 1 1 calc R . .
H4B H 0.3207 0.7437 0.3487 0.077 Uiso 1 1 calc R . .
H4C H 0.3016 0.6132 0.4014 0.077 Uiso 1 1 calc R . .
C5 C 0.3116(8) 0.6767(5) 0.1411(3) 0.0278(14) Uani 1 1 d . . .
C6 C 0.1366(8) 0.6489(6) 0.1547(3) 0.0325(15) Uani 1 1 d . . .
C7 C 0.0102(8) 0.7280(6) 0.1247(3) 0.0351(15) Uani 1 1 d . . .
C8 C 0.0519(8) 0.8401(6) 0.0792(3) 0.0373(16) Uani 1 1 d . . .
H8 H -0.0329 0.8943 0.0596 0.045 Uiso 1 1 calc R . .
C9 C 0.2241(9) 0.8685(6) 0.0642(3) 0.0389(17) Uani 1 1 d . . .
C10 C 0.3543(7) 0.7902(5) 0.0943(3) 0.0269(14) Uani 1 1 d . . .
C11 C 0.4622(8) 0.2442(5) 0.2918(3) 0.0298(14) Uani 1 1 d . . .
C12 C 0.5085(8) 0.2485(6) 0.3713(3) 0.0345(15) Uani 1 1 d . . .
C13 C 0.5728(8) 0.1354(6) 0.4070(3) 0.0375(16) Uani 1 1 d . . .
C14 C 0.5943(8) 0.0147(6) 0.3665(3) 0.0386(16) Uani 1 1 d . . .
H14 H 0.6386 -0.0607 0.3907 0.046 Uiso 1 1 calc R . .
C15 C 0.5474(8) 0.0112(6) 0.2893(4) 0.0390(16) Uani 1 1 d . . .
C16 C 0.4821(8) 0.1206(6) 0.2522(3) 0.0284(14) 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'
N N 0.0061 0.0033 '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'
Al Al 0.0645 0.0514 '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
_geom_angle_publ_flag
C1 Al1 C2 121.2(3) . . ?
C1 Al1 N2 111.9(3) . . ?
C2 Al1 N2 114.3(3) . . ?
C1 Al1 N1 106.0(3) . . ?
C2 Al1 N1 111.7(3) . . ?
N2 Al1 N1 85.61(19) . . ?
C1 Al1 Al2 106.4(2) . . ?
C2 Al1 Al2 132.1(2) . . ?
N2 Al1 Al2 43.37(13) . . ?
N1 Al1 Al2 44.10(14) . . ?
C3 Al2 C4 120.2(3) . . ?
C3 Al2 N2 111.7(3) . . ?
C4 Al2 N2 114.5(3) . . ?
C3 Al2 N1 106.3(2) . . ?
C4 Al2 N1 113.1(3) . . ?
N2 Al2 N1 85.45(19) . . ?
C3 Al2 Al1 106.4(2) . . ?
C4 Al2 Al1 133.2(2) . . ?
N2 Al2 Al1 43.48(13) . . ?
N1 Al2 Al1 43.82(14) . . ?
C6 F1 N2 115.4(3) . . ?
C10 F4 N1 61.4(3) . . ?
C5 N1 Al1 120.1(3) . . ?
C5 N1 Al2 121.8(4) . . ?
Al1 N1 Al2 92.1(2) . . ?
C5 N1 F4 57.9(3) . . ?
Al1 N1 F4 127.8(2) . . ?
Al2 N1 F4 136.0(2) . . ?
C11 N2 Al2 122.1(4) . . ?
C11 N2 Al1 120.0(4) . . ?
Al2 N2 Al1 93.16(19) . . ?
C11 N2 F1 154.6(4) . . ?
Al2 N2 F1 73.24(16) . . ?
Al1 N2 F1 75.34(16) . . ?
C6 C5 C10 116.0(5) . . ?
C6 C5 N1 122.6(5) . . ?
C10 C5 N1 121.4(5) . . ?
F1 C6 C7 118.9(5) . . ?
F1 C6 C5 118.4(5) . . ?
C7 C6 C5 122.7(5) . . ?
F2 C7 C8 119.3(6) . . ?
F2 C7 C6 119.3(5) . . ?
C8 C7 C6 121.4(6) . . ?
C9 C8 C7 116.9(6) . . ?
F3 C9 C8 119.7(6) . . ?
F3 C9 C10 117.7(5) . . ?
C8 C9 C10 122.6(5) . . ?
F4 C10 C5 119.3(5) . . ?
F4 C10 C9 120.3(5) . . ?
C5 C10 C9 120.4(5) . . ?
C16 C11 C12 116.1(5) . . ?
C16 C11 N2 122.1(5) . . ?
C12 C11 N2 121.7(5) . . ?
F5 C12 C13 119.7(5) . . ?
F5 C12 C11 119.4(5) . . ?
C13 C12 C11 120.9(5) . . ?
F6 C13 C14 119.3(5) . . ?
F6 C13 C12 118.6(5) . . ?
C14 C13 C12 122.1(5) . . ?
C15 C14 C13 116.5(6) . . ?
F7 C15 C14 119.2(6) . . ?
F7 C15 C16 117.9(5) . . ?
C14 C15 C16 122.9(6) . . ?
F8 C16 C15 120.0(5) . . ?
F8 C16 C11 118.5(5) . . ?
C15 C16 C11 121.4(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 C1 1.931(7) . ?
Al1 C2 1.949(6) . ?
Al1 N2 1.998(5) . ?
Al1 N1 2.008(5) . ?
Al1 Al2 2.899(2) . ?
Al2 C3 1.952(6) . ?
Al2 C4 1.972(6) . ?
Al2 N2 1.994(5) . ?
Al2 N1 2.019(5) . ?
F1 C6 1.362(6) . ?
F1 N2 3.152(6) . ?
F2 C7 1.346(7) . ?
F3 C9 1.359(6) . ?
F4 C10 1.338(6) . ?
F4 N1 2.784(6) . ?
F5 C12 1.342(6) . ?
F6 C13 1.354(7) . ?
F7 C15 1.363(7) . ?
F8 C16 1.350(6) . ?
N1 C5 1.406(7) . ?
N2 C11 1.438(7) . ?
C5 C6 1.383(8) . ?
C5 C10 1.397(7) . ?
C6 C7 1.380(8) . ?
C7 C8 1.373(8) . ?
C8 C9 1.369(9) . ?
C9 C10 1.398(8) . ?
C11 C16 1.388(8) . ?
C11 C12 1.396(8) . ?
C12 C13 1.383(8) . ?
C13 C14 1.374(8) . ?
C14 C15 1.360(8) . ?
C15 C16 1.368(8) . ?
