#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:20:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179785 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/81/7008136.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_7008136
loop_
_publ_author_name
'Gonsior, Marcin'
'Krossing, Ingo'
_publ_section_title
;
 Preparation of stable AsBr4+ and I2As-PI3+ salts. Why didn't we
 succeed to prepare AsI4+ and As2X5+? A combined experimental and
 theoretical study.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1203
_journal_page_last               1213
_journal_paper_doi               10.1039/b417629d
_journal_year                    2005
_chemical_formula_sum            'C24 H16 Al2 F38 O6'
_chemical_formula_weight         1176.33
_chemical_name_systematic
;
[(RO)2AlF(THF)]2 (R = C(CF3)3)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.34(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6522(19)
_cell_length_b                   12.727(3)
_cell_length_c                   15.596(3)
_cell_measurement_reflns_used    3207
_cell_measurement_temperature    100(2)
_cell_volume                     1904.2(7)
_computing_cell_refinement       'CELL (STOE)'
_computing_data_collection       'XPOSE (STOE)'
_computing_data_reduction        'XRED (STOE)'
_computing_molecular_graphics    RESVIEW
_computing_publication_material  RESVIEW
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'IPDS II (STOE)'
_diffrn_measurement_method       'Image Plate Technique'
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7799
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0004(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         3426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0446P)²+0.1223P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                2749
_reflns_number_total             3426
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b417629d.txt
_cod_data_source_block           p21n
_cod_original_cell_volume        1904.1(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7008136
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.05607(6) 0.40927(4) 0.95793(3) 0.01510(14) Uani 1 1 d . . .
F10 F -0.25227(13) 0.39318(9) 0.82413(7) 0.0288(3) Uani 1 1 d . . .
F01 F 0.06189(11) 0.47282(8) 1.06075(6) 0.0184(2) Uani 1 1 d . . .
F15 F -0.30769(14) 0.10270(10) 0.92823(8) 0.0326(3) Uani 1 1 d . . .
F4 F -0.04253(12) 0.52624(10) 0.75603(7) 0.0302(3) Uani 1 1 d . . .
F13 F -0.23926(13) 0.20204(9) 1.03630(7) 0.0296(3) Uani 1 1 d . . .
F1 F 0.30328(15) 0.33474(9) 0.76555(8) 0.0356(3) Uani 1 1 d . . .
O2 O -0.07592(13) 0.31711(10) 0.95176(7) 0.0188(3) Uani 1 1 d . . .
F11 F -0.37874(12) 0.32151(10) 0.91257(7) 0.0288(3) Uani 1 1 d . . .
F16 F -0.06235(13) 0.26036(10) 0.76869(7) 0.0306(3) Uani 1 1 d . . .
F17 F 0.05693(12) 0.17211(10) 0.86852(7) 0.0318(3) Uani 1 1 d . . .
F7 F 0.30121(14) 0.58256(10) 0.92971(7) 0.0314(3) Uani 1 1 d . . .
F14 F -0.09547(14) 0.09441(10) 0.98846(8) 0.0344(3) Uani 1 1 d . . .
F2 F 0.32093(14) 0.47099(10) 0.68581(7) 0.0317(3) Uani 1 1 d . . .
F5 F 0.07290(13) 0.65121(9) 0.82375(7) 0.0277(3) Uani 1 1 d . . .
F6 F 0.11286(13) 0.61025(10) 0.69425(7) 0.0300(3) Uani 1 1 d . . .
F12 F -0.35089(13) 0.24467(10) 0.79283(7) 0.0298(3) Uani 1 1 d . . .
O3 O 0.19914(14) 0.32059(10) 1.00992(7) 0.0192(3) Uani 1 1 d . . .
F18 F -0.13123(14) 0.10650(10) 0.80221(8) 0.0350(3) Uani 1 1 d . . .
F8 F 0.43581(13) 0.49006(10) 0.85983(8) 0.0330(3) Uani 1 1 d . . .
O1 O 0.14237(14) 0.42742(10) 0.86800(8) 0.0197(3) Uani 1 1 d . . .
F3 F 0.12513(15) 0.38894(11) 0.68303(7) 0.0376(3) Uani 1 1 d . . .
F9 F 0.35305(13) 0.63531(9) 0.80609(7) 0.0290(3) Uani 1 1 d . . .
C6 C -0.2862(2) 0.30251(16) 0.85717(11) 0.0220(4) Uani 1 1 d . . .
C5 C -0.1556(2) 0.24677(14) 0.90323(11) 0.0187(4) Uani 1 1 d . . .
C7 C -0.2010(2) 0.16008(16) 0.96468(12) 0.0249(4) Uani 1 1 d . . .
C8 C -0.0721(2) 0.19457(16) 0.83459(12) 0.0245(4) Uani 1 1 d . . .
C2 C 0.2381(2) 0.42001(16) 0.73493(12) 0.0272(5) Uani 1 1 d . . .
C03 C 0.2679(2) 0.16272(18) 1.07872(14) 0.0282(5) Uani 1 1 d . . .
C3 C 0.0821(2) 0.57019(16) 0.76974(12) 0.0235(4) Uani 1 1 d . . .
C04 C 0.1820(2) 0.25922(17) 1.08829(12) 0.0248(4) Uani 1 1 d . . .
C02 C 0.3921(2) 0.20600(19) 1.03846(14) 0.0304(5) Uani 1 1 d . . .
C1 C 0.1930(2) 0.49051(15) 0.80829(10) 0.0181(4) Uani 1 1 d . . .
C4 C 0.3226(2) 0.55104(16) 0.85087(12) 0.0249(4) Uani 1 1 d . . .
C01 C 0.3281(2) 0.28700(19) 0.97494(13) 0.0279(5) Uani 1 1 d . . .
H7 H 0.086(3) 0.2466(18) 1.0885(13) 0.026(6) Uiso 1 1 d . . .
H1 H 0.383(3) 0.346(2) 0.9694(14) 0.029(6) Uiso 1 1 d . . .
H2 H 0.298(3) 0.257(2) 0.9188(16) 0.034(6) Uiso 1 1 d . . .
H8 H 0.223(3) 0.3011(19) 1.1376(15) 0.033(6) Uiso 1 1 d . . .
H3 H 0.440(3) 0.155(2) 1.0082(14) 0.033(6) Uiso 1 1 d . . .
H5 H 0.294(3) 0.127(2) 1.1324(17) 0.041(7) Uiso 1 1 d . . .
H6 H 0.217(3) 0.117(2) 1.0439(17) 0.040(7) Uiso 1 1 d . . .
H4 H 0.461(3) 0.244(2) 1.0856(16) 0.044(7) Uiso 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'
O O 0.0106 0.0060 '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'
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
_geom_angle_publ_flag
O1 Al1 O2 117.75(7) . . ?
O1 Al1 F01 134.23(7) . . ?
O2 Al1 F01 107.85(6) . . ?
O1 Al1 F01 96.05(6) . 3_567 ?
O2 Al1 F01 95.90(6) . 3_567 ?
F01 Al1 F01 74.80(6) . 3_567 ?
O1 Al1 O3 91.90(6) . . ?
O2 Al1 O3 96.76(7) . . ?
F01 Al1 O3 86.36(6) . . ?
F01 Al1 O3 159.82(6) 3_567 . ?
O1 Al1 Al1 119.71(5) . 3_567 ?
O2 Al1 Al1 104.73(5) . 3_567 ?
F01 Al1 Al1 38.54(4) . 3_567 ?
F01 Al1 Al1 36.27(3) 3_567 3_567 ?
O3 Al1 Al1 124.55(5) . 3_567 ?
Al1 F01 Al1 105.20(6) . 3_567 ?
C5 O2 Al1 148.15(11) . . ?
C04 O3 C01 109.20(14) . . ?
C04 O3 Al1 121.80(11) . . ?
C01 O3 Al1 128.22(11) . . ?
C1 O1 Al1 151.43(12) . . ?
F10 C6 F11 107.92(16) . . ?
F10 C6 F12 107.62(14) . . ?
F11 C6 F12 107.14(16) . . ?
F10 C6 C5 110.89(16) . . ?
F11 C6 C5 110.58(15) . . ?
F12 C6 C5 112.49(15) . . ?
O2 C5 C6 109.78(15) . . ?
O2 C5 C7 107.78(14) . . ?
C6 C5 C7 109.85(15) . . ?
O2 C5 C8 111.14(15) . . ?
C6 C5 C8 109.41(15) . . ?
C7 C5 C8 108.86(16) . . ?
F13 C7 F15 107.75(15) . . ?
F13 C7 F14 106.99(16) . . ?
F15 C7 F14 107.68(17) . . ?
F13 C7 C5 110.91(16) . . ?
F15 C7 C5 112.43(16) . . ?
F14 C7 C5 110.85(15) . . ?
F17 C8 F18 108.27(17) . . ?
F17 C8 F16 107.37(15) . . ?
F18 C8 F16 107.41(15) . . ?
F17 C8 C5 110.56(15) . . ?
F18 C8 C5 112.75(16) . . ?
F16 C8 C5 110.29(16) . . ?
F1 C2 F2 108.42(17) . . ?
F1 C2 F3 107.42(17) . . ?
F2 C2 F3 107.16(16) . . ?
F1 C2 C1 111.72(15) . . ?
F2 C2 C1 112.09(17) . . ?
F3 C2 C1 109.83(17) . . ?
C04 C03 C02 102.40(18) . . ?
F4 C3 F5 107.73(15) . . ?
F4 C3 F6 107.66(16) . . ?
F5 C3 F6 107.14(16) . . ?
F4 C3 C1 111.33(16) . . ?
F5 C3 C1 110.54(15) . . ?
F6 C3 C1 112.23(14) . . ?
O3 C04 C03 103.75(15) . . ?
C01 C02 C03 103.51(18) . . ?
O1 C1 C3 111.54(15) . . ?
O1 C1 C2 108.32(15) . . ?
C3 C1 C2 109.28(15) . . ?
O1 C1 C4 109.46(15) . . ?
C3 C1 C4 109.32(16) . . ?
C2 C1 C4 108.87(15) . . ?
F9 C4 F7 107.93(16) . . ?
F9 C4 F8 107.35(15) . . ?
F7 C4 F8 106.69(16) . . ?
F9 C4 C1 112.90(16) . . ?
F7 C4 C1 110.14(15) . . ?
F8 C4 C1 111.55(17) . . ?
O3 C01 C02 104.80(15) . . ?
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 O1 1.7239(13) . ?
Al1 O2 1.7266(14) . ?
Al1 F01 1.7914(11) . ?
Al1 F01 1.8868(12) 3_567 ?
Al1 O3 1.8950(15) . ?
Al1 Al1 2.9225(11) 3_567 ?
F10 C6 1.320(2) . ?
F01 Al1 1.8868(12) 3_567 ?
F15 C7 1.337(3) . ?
F4 C3 1.323(2) . ?
F13 C7 1.327(2) . ?
F1 C2 1.317(3) . ?
O2 C5 1.355(2) . ?
F11 C6 1.332(2) . ?
F16 C8 1.337(2) . ?
F17 C8 1.329(2) . ?
F7 C4 1.331(2) . ?
F14 C7 1.338(3) . ?
F2 C2 1.335(2) . ?
F5 C3 1.341(2) . ?
F6 C3 1.346(2) . ?
F12 C6 1.342(2) . ?
O3 C04 1.475(2) . ?
O3 C01 1.476(2) . ?
F18 C8 1.332(2) . ?
F8 C4 1.335(3) . ?
O1 C1 1.361(2) . ?
F3 C2 1.344(3) . ?
F9 C4 1.330(2) . ?
C6 C5 1.552(3) . ?
C5 C7 1.556(3) . ?
C5 C8 1.558(2) . ?
C2 C1 1.553(3) . ?
C03 C04 1.498(3) . ?
C03 C02 1.517(3) . ?
C3 C1 1.547(3) . ?
C02 C01 1.514(3) . ?
C1 C4 1.554(3) . ?
