#------------------------------------------------------------------------------
#$Date: 2019-03-16 07:07:26 +0200 (Sat, 16 Mar 2019) $
#$Revision: 214145 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242868.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_2242868
loop_
_publ_author_name
'Vinogradov, Alexander A.'
'Minyaev, Mikhail E.'
'Lyssenko, Konstantin A.'
'Nifant'ev, Ilya E.'
_publ_section_title
;
 Crystal structure of
 bis(μ₂-triphenylacetato-κO:κO')bis(diisobutylaluminium)
;
_journal_coeditor_code           TX2010
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              456
_journal_page_last               459
_journal_paper_doi               10.1107/S2056989019003396
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Al2 (C4 H9)4 (C20 H15 O2)2]'
_chemical_formula_moiety         'C56 H66 Al2 O4'
_chemical_formula_sum            'C56 H66 Al2 O4'
_chemical_formula_weight         857.04
_chemical_name_systematic
;
Bis(μ₂-triphenylacetato-κO:κO')bis(diisobutylaluminium)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2017/1
_cell_angle_alpha                108.7900(10)
_cell_angle_beta                 109.1430(10)
_cell_angle_gamma                91.8660(10)
_cell_formula_units_Z            1
_cell_length_a                   9.2839(3)
_cell_length_b                   12.0281(4)
_cell_length_c                   12.5999(4)
_cell_measurement_reflns_used    4293
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.21
_cell_volume                     1243.25(7)
_computing_cell_refinement
;
APEX2 (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
APEX2 (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al.,
2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_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  0.0163
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16191
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.810
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al.,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         7242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0485P)²+0.4816P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                6063
_reflns_number_total             7242
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            tx2010sup1.cif
_cod_data_source_block           global
_cod_database_code               2242868
_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   0.968
_shelx_estimated_absorpt_t_max   0.982
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 Al 0.36034(4) 0.60789(3) 0.40800(3) 0.01642(8) Uani d 1
O O1 0.46295(9) 0.65487(7) 0.56994(7) 0.02070(16) Uani d 1
O O2 0.59680(10) 0.53977(7) 0.65814(7) 0.02258(17) Uani d 1
C C1 0.55346(11) 0.63769(9) 0.66037(9) 0.01473(18) Uani d 1
C C2 0.60602(11) 0.74392(8) 0.78064(8) 0.01395(17) Uani d 1
C C3 0.70126(11) 0.84711(9) 0.77322(9) 0.01552(18) Uani d 1
C C4 0.72549(13) 0.84652(10) 0.66985(10) 0.0214(2) Uani d 1
H H4 0.679269 0.780431 0.597423 0.026 Uiso calc 1
C C5 0.81694(14) 0.94188(11) 0.67113(11) 0.0264(2) Uani d 1
H H5 0.831675 0.940322 0.599551 0.032 Uiso calc 1
C C6 0.88595(13) 1.03822(10) 0.77555(11) 0.0255(2) Uani d 1
H H6 0.948184 1.102928 0.776255 0.031 Uiso calc 1
C C7 0.86365(14) 1.03974(10) 0.87945(11) 0.0254(2) Uani d 1
H H7 0.910835 1.105845 0.951716 0.030 Uiso calc 1
C C8 0.77282(13) 0.94532(9) 0.87861(10) 0.0213(2) Uani d 1
H H8 0.758995 0.947335 0.950612 0.026 Uiso calc 1
C C9 0.71189(11) 0.70895(9) 0.88401(9) 0.01570(18) Uani d 1
C C10 0.84898(12) 0.66876(9) 0.87587(9) 0.01762(19) Uani d 1
H H10 0.872291 0.660624 0.805990 0.021 Uiso calc 1
C C11 0.95149(13) 0.64058(10) 0.96847(10) 0.0219(2) Uani d 1
H H11 1.043453 0.612413 0.961155 0.026 Uiso calc 1
C C12 0.91965(14) 0.65356(10) 1.07182(10) 0.0245(2) Uani d 1
H H12 0.989225 0.633819 1.135044 0.029 Uiso calc 1
C C13 0.78621(14) 0.69535(11) 1.08199(10) 0.0249(2) Uani d 1
H H13 0.764773 0.705090 1.152906 0.030 Uiso calc 1
C C14 0.68228(13) 0.72347(10) 0.98882(10) 0.0208(2) Uani d 1
H H14 0.591151 0.752588 0.997035 0.025 Uiso calc 1
C C15 0.45248(11) 0.77495(9) 0.79625(9) 0.01574(18) Uani d 1
C C16 0.35242(12) 0.68609(10) 0.79768(10) 0.0204(2) Uani d 1
H H16 0.382480 0.610353 0.792614 0.025 Uiso calc 1
C C17 0.20989(13) 0.70739(11) 0.80642(11) 0.0243(2) Uani d 1
H H17 0.143354 0.646379 0.807484 0.029 Uiso calc 1
C C18 0.16423(13) 0.81765(11) 0.81363(11) 0.0260(2) Uani d 1
H H18 0.066942 0.832509 0.819938 0.031 Uiso calc 1
C C19 0.26197(14) 0.90553(11) 0.81151(12) 0.0276(2) Uani d 1
H H19 0.231175 0.980971 0.816053 0.033 Uiso calc 1
C C20 0.40547(13) 0.88454(10) 0.80277(10) 0.0219(2) Uani d 1
H H20 0.471338 0.945698 0.801290 0.026 Uiso calc 1
C C21 0.46133(13) 0.72019(10) 0.36084(10) 0.0222(2) Uani d 1
H H21A 0.469150 0.800830 0.418442 0.027 Uiso calc 1
H H21C 0.568096 0.703514 0.372745 0.027 Uiso calc 1
C C22 0.39213(13) 0.72538(10) 0.23396(11) 0.0238(2) Uani d 1
H H22 0.281201 0.734727 0.218042 0.029 Uiso calc 1
C C23 0.47318(17) 0.83216(12) 0.22378(13) 0.0320(3) Uani d 1
H H23A 0.460235 0.905703 0.280219 0.048 Uiso calc 1
H H23B 0.427888 0.832215 0.141750 0.048 Uiso calc 1
H H23C 0.583350 0.826987 0.242832 0.048 Uiso calc 1
C C24 0.39865(17) 0.61094(12) 0.13896(12) 0.0333(3) Uani d 1
H H24A 0.357500 0.618086 0.059590 0.050 Uiso calc 1
H H24B 0.336713 0.544191 0.140295 0.050 Uiso calc 1
H H24C 0.505921 0.596939 0.155904 0.050 Uiso calc 1
C C25 0.13991(13) 0.58192(10) 0.38202(10) 0.0220(2) Uani d 1
H H25A 0.081171 0.575283 0.298399 0.026 Uiso calc 1
H H25B 0.116166 0.504248 0.388900 0.026 Uiso calc 1
C C26 0.07847(14) 0.67528(12) 0.46520(11) 0.0279(2) Uani d 1
H H26 0.134767 0.679617 0.549380 0.033 Uiso calc 1
C C27 -0.09381(17) 0.63988(16) 0.43580(15) 0.0430(3) Uani d 1
H H27A -0.128031 0.698006 0.493736 0.064 Uiso calc 1
H H27B -0.111633 0.561008 0.440224 0.064 Uiso calc 1
H H27C -0.152073 0.637961 0.354626 0.064 Uiso calc 1
C C28 0.1090(2) 0.79795(14) 0.45938(16) 0.0440(4) Uani d 1
H H28A 0.068374 0.855379 0.513088 0.066 Uiso calc 1
H H28B 0.057855 0.795392 0.376941 0.066 Uiso calc 1
H H28C 0.220363 0.822015 0.484379 0.066 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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Al O1 2_666 . 106.84(4)
O2 Al C25 2_666 . 104.41(5)
O1 Al C25 . . 106.37(4)
O2 Al C21 2_666 . 108.55(5)
O1 Al C21 . . 103.48(4)
C25 Al C21 . . 125.97(5)
C1 O1 Al . . 151.00(7)
C1 O2 Al . 2_666 156.79(8)
O2 C1 O1 . . 123.64(9)
O2 C1 C2 . . 119.65(9)
O1 C1 C2 . . 116.65(9)
C9 C2 C15 . . 112.68(8)
C9 C2 C3 . . 106.65(8)
C15 C2 C3 . . 113.13(8)
C9 C2 C1 . . 110.97(8)
C15 C2 C1 . . 103.23(8)
C3 C2 C1 . . 110.25(8)
C4 C3 C8 . . 117.96(9)
C4 C3 C2 . . 124.20(9)
C8 C3 C2 . . 117.79(9)
C3 C4 C5 . . 120.85(10)
C3 C4 H4 . . 119.6
C5 C4 H4 . . 119.6
C6 C5 C4 . . 120.45(11)
C6 C5 H5 . . 119.8
C4 C5 H5 . . 119.8
C5 C6 C7 . . 119.35(10)
C5 C6 H6 . . 120.3
C7 C6 H6 . . 120.3
C6 C7 C8 . . 120.41(10)
C6 C7 H7 . . 119.8
C8 C7 H7 . . 119.8
C7 C8 C3 . . 120.97(10)
C7 C8 H8 . . 119.5
C3 C8 H8 . . 119.5
C14 C9 C10 . . 118.49(9)
C14 C9 C2 . . 122.79(9)
C10 C9 C2 . . 118.56(9)
C11 C10 C9 . . 120.97(10)
C11 C10 H10 . . 119.5
C9 C10 H10 . . 119.5
C10 C11 C12 . . 120.06(10)
C10 C11 H11 . . 120.0
C12 C11 H11 . . 120.0
C13 C12 C11 . . 119.55(10)
C13 C12 H12 . . 120.2
C11 C12 H12 . . 120.2
C12 C13 C14 . . 120.62(11)
C12 C13 H13 . . 119.7
C14 C13 H13 . . 119.7
C9 C14 C13 . . 120.28(10)
C9 C14 H14 . . 119.9
C13 C14 H14 . . 119.9
C20 C15 C16 . . 118.53(9)
C20 C15 C2 . . 123.12(9)
C16 C15 C2 . . 118.27(9)
C17 C16 C15 . . 120.81(10)
C17 C16 H16 . . 119.6
C15 C16 H16 . . 119.6
C16 C17 C18 . . 120.23(11)
C16 C17 H17 . . 119.9
C18 C17 H17 . . 119.9
C19 C18 C17 . . 119.28(10)
C19 C18 H18 . . 120.4
C17 C18 H18 . . 120.4
C18 C19 C20 . . 120.70(11)
C18 C19 H19 . . 119.7
C20 C19 H19 . . 119.7
C15 C20 C19 . . 120.45(10)
C15 C20 H20 . . 119.8
C19 C20 H20 . . 119.8
C22 C21 Al . . 120.48(8)
C22 C21 H21A . . 107.2
Al C21 H21A . . 107.2
C22 C21 H21C . . 107.2
Al C21 H21C . . 107.2
H21A C21 H21C . . 106.8
C24 C22 C23 . . 110.11(10)
C24 C22 C21 . . 111.38(10)
C23 C22 C21 . . 111.41(10)
C24 C22 H22 . . 107.9
C23 C22 H22 . . 107.9
C21 C22 H22 . . 107.9
C22 C23 H23A . . 109.5
C22 C23 H23B . . 109.5
H23A C23 H23B . . 109.5
C22 C23 H23C . . 109.5
H23A C23 H23C . . 109.5
H23B C23 H23C . . 109.5
C22 C24 H24A . . 109.5
C22 C24 H24B . . 109.5
H24A C24 H24B . . 109.5
C22 C24 H24C . . 109.5
H24A C24 H24C . . 109.5
H24B C24 H24C . . 109.5
C26 C25 Al . . 117.87(8)
C26 C25 H25A . . 107.8
Al C25 H25A . . 107.8
C26 C25 H25B . . 107.8
Al C25 H25B . . 107.8
H25A C25 H25B . . 107.2
C28 C26 C27 . . 110.38(12)
C28 C26 C25 . . 111.39(11)
C27 C26 C25 . . 111.31(11)
C28 C26 H26 . . 107.9
C27 C26 H26 . . 107.9
C25 C26 H26 . . 107.9
C26 C27 H27A . . 109.5
C26 C27 H27B . . 109.5
H27A C27 H27B . . 109.5
C26 C27 H27C . . 109.5
H27A C27 H27C . . 109.5
H27B C27 H27C . . 109.5
C26 C28 H28A . . 109.5
C26 C28 H28B . . 109.5
H28A C28 H28B . . 109.5
C26 C28 H28C . . 109.5
H28A C28 H28C . . 109.5
H28B C28 H28C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al O1 . 1.8269(8) y
Al O2 2_666 1.8212(8) y
Al C21 . 1.9639(12) y
Al C25 . 1.9611(12) y
O1 C1 . 1.2579(12) y
O2 C1 . 1.2518(12) y
C1 C2 . 1.5473(13) ?
C2 C9 . 1.5425(14) ?
C2 C15 . 1.5431(14) ?
C2 C3 . 1.5455(14) ?
C3 C4 . 1.3905(14) ?
C3 C8 . 1.3999(14) ?
C4 C5 . 1.3973(15) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.3788(17) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.3855(17) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.3875(15) ?
C7 H7 . 0.9500 ?
C8 H8 . 0.9500 ?
C9 C14 . 1.3938(14) ?
C9 C10 . 1.3992(14) ?
C10 C11 . 1.3890(14) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.3900(17) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.3809(17) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.3992(15) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
C15 C20 . 1.3878(14) ?
C15 C16 . 1.4016(14) ?
C16 C17 . 1.3887(15) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.3896(17) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.3831(18) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.3968(16) ?
C19 H19 . 0.9500 ?
C20 H20 . 0.9500 ?
C21 C22 . 1.5381(16) ?
C21 H21A . 0.9900 ?
C21 H21C . 0.9900 ?
C22 C24 . 1.5241(18) ?
C22 C23 . 1.5293(16) ?
C22 H22 . 1.0000 ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
C24 H24A . 0.9800 ?
C24 H24B . 0.9800 ?
C24 H24C . 0.9800 ?
C25 C26 . 1.5363(16) ?
C25 H25A . 0.9900 ?
C25 H25B . 0.9900 ?
C26 C28 . 1.523(2) ?
C26 C27 . 1.5304(19) ?
C26 H26 . 1.0000 ?
C27 H27A . 0.9800 ?
C27 H27B . 0.9800 ?
C27 H27C . 0.9800 ?
C28 H28A . 0.9800 ?
C28 H28B . 0.9800 ?
C28 H28C . 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_site_symmetry_1
_geom_torsion
O2 Al O1 C1 2_666 3.48(16)
C25 Al O1 C1 . 114.58(15)
C21 Al O1 C1 . -111.00(15)
Al O2 C1 O1 2_666 24.1(3)
Al O2 C1 C2 2_666 -158.73(15)
Al O1 C1 O2 . -12.9(2)
Al O1 C1 C2 . 169.90(11)
O2 C1 C2 C9 . 0.80(13)
O1 C1 C2 C9 . 178.13(8)
O2 C1 C2 C15 . -120.15(10)
O1 C1 C2 C15 . 57.18(11)
O2 C1 C2 C3 . 118.74(10)
O1 C1 C2 C3 . -63.94(11)
C9 C2 C3 C4 . 124.93(10)
C15 C2 C3 C4 . -110.63(11)
C1 C2 C3 C4 . 4.38(13)
C9 C2 C3 C8 . -52.35(11)
C15 C2 C3 C8 . 72.08(11)
C1 C2 C3 C8 . -172.91(9)
C8 C3 C4 C5 . -0.80(16)
C2 C3 C4 C5 . -178.08(10)
C3 C4 C5 C6 . 0.48(18)
C4 C5 C6 C7 . -0.07(18)
C5 C6 C7 C8 . 0.01(18)
C6 C7 C8 C3 . -0.36(18)
C4 C3 C8 C7 . 0.74(16)
C2 C3 C8 C7 . 178.19(10)
C15 C2 C9 C14 . -10.07(13)
C3 C2 C9 C14 . 114.64(10)
C1 C2 C9 C14 . -125.27(10)
C15 C2 C9 C10 . 174.54(9)
C3 C2 C9 C10 . -60.76(11)
C1 C2 C9 C10 . 59.34(11)
C14 C9 C10 C11 . 1.83(15)
C2 C9 C10 C11 . 177.43(9)
C9 C10 C11 C12 . -0.82(16)
C10 C11 C12 C13 . -0.44(17)
C11 C12 C13 C14 . 0.67(18)
C10 C9 C14 C13 . -1.60(16)
C2 C9 C14 C13 . -177.00(10)
C12 C13 C14 C9 . 0.37(17)
C9 C2 C15 C20 . 121.13(11)
C3 C2 C15 C20 . 0.05(13)
C1 C2 C15 C20 . -119.09(10)
C9 C2 C15 C16 . -62.24(12)
C3 C2 C15 C16 . 176.68(9)
C1 C2 C15 C16 . 57.54(11)
C20 C15 C16 C17 . -0.52(16)
C2 C15 C16 C17 . -177.30(10)
C15 C16 C17 C18 . 0.15(17)
C16 C17 C18 C19 . 0.25(18)
C17 C18 C19 C20 . -0.28(19)
C16 C15 C20 C19 . 0.49(16)
C2 C15 C20 C19 . 177.11(10)
C18 C19 C20 C15 . -0.10(18)
Al C21 C22 C24 . -66.22(12)
Al C21 C22 C23 . 170.40(8)
Al C25 C26 C28 . 58.20(13)
Al C25 C26 C27 . -178.14(9)
