#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:38:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179981 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/75/7027569.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7027569
loop_
_publ_author_name
'Lewiński, Janusz'
'Justyniak, Iwona'
'Ochal, Zbigniew'
'Zachara, Janusz'
_publ_section_title
;
 Dramatic structural changes of donor-functionalized alkoxides of
 aluminium upon replacement of the ester functionality by ketone
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2909
_journal_paper_doi               10.1039/a904176a
_journal_year                    1999
_chemical_formula_moiety         'C16 H34 Al2 O4'
_chemical_formula_structural     '[Al(C2H5)2(C4H7O2)]2'
_chemical_formula_sum            'C16 H34 Al2 O4'
_chemical_formula_weight         344.39
_chemical_name_systematic
; 
 bis[μ-(acetoinato)]tetraethyldialuminum  
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                84.371(16)
_cell_angle_beta                 86.844(18)
_cell_angle_gamma                78.253(17)
_cell_formula_units_Z            2
_cell_length_a                   7.3548(18)
_cell_length_b                   8.8850(17)
_cell_length_c                   16.790(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.80
_cell_measurement_theta_min      7.68
_cell_volume                     1068.3(4)
_computing_cell_refinement       'Siemens P3 software'
_computing_data_collection       'Siemens P3 software'
_computing_data_reduction        'XDISK, Siemens P3 software'
_computing_molecular_graphics    'ORTEP III (Burnett, Johnson, 1996)'
_computing_publication_material
;
SHELXL-93 (Sheldrick, 1993) & PARST 96 (Nardelli, 1996)'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P3 four-circle diffractometer'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7403
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        8.6
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3785
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1032P)²+0.2931P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                2947
_reflns_number_total             3785
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904176asup1.cif
_cod_data_source_block           acet
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+0.2931P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+0.2931P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7027569
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.60574(12) -0.11100(9) 0.06150(5) 0.0536(3) Uani 1 d . . .
Al2 Al 0.12490(12) 0.40689(9) 0.44233(4) 0.0547(3) Uani 1 d . . .
O1 O 0.5416(2) 0.09788(19) 0.03169(10) 0.0518(5) Uani 1 d . . .
O2 O 0.7324(3) -0.0094(2) 0.15077(12) 0.0722(6) Uani 1 d . . .
O3 O 0.0791(2) 0.4190(2) 0.55073(10) 0.0527(5) Uani 1 d . . .
O4 O 0.3278(3) 0.2180(3) 0.49488(13) 0.0773(6) Uani 1 d . . .
C1 C 0.4710(6) 0.3425(4) 0.0896(3) 0.1012(14) Uani 1 d . . .
H1A H 0.4016 0.3895 0.0437 0.126(9) Uiso 1 calc R . .
H1B H 0.5293 0.4171 0.1103 0.126(9) Uiso 1 calc R . .
H1C H 0.3888 0.3064 0.1301 0.126(9) Uiso 1 calc R . .
C2 C 0.6173(4) 0.2089(3) 0.06558(18) 0.0620(7) Uani 1 d . . .
H2 H 0.7027 0.2483 0.0258 0.071(9) Uiso 1 calc R . .
C3 C 0.7272(4) 0.1279(4) 0.13551(17) 0.0636(7) Uani 1 d . . .
C4 C 0.8293(6) 0.2146(5) 0.1837(2) 0.0900(11) Uani 1 d . . .
H4A H 0.9241 0.1432 0.2127 0.155(12) Uiso 1 calc R . .
H4B H 0.7439 0.2707 0.2208 0.155(12) Uiso 1 calc R . .
H4C H 0.8855 0.2855 0.1486 0.155(12) Uiso 1 calc R . .
C5 C 0.4510(5) -0.2053(4) 0.14355(19) 0.0763(9) Uani 1 d . . .
H5A H 0.4080 -0.2878 0.1212 0.097(8) Uiso 1 calc R . .
H5B H 0.5276 -0.2510 0.1883 0.097(8) Uiso 1 calc R . .
C6 C 0.2852(6) -0.0947(6) 0.1743(3) 0.1069(14) Uani 1 d . . .
H6A H 0.2227 -0.1468 0.2168 0.135(10) Uiso 1 calc R . .
H6B H 0.2015 -0.0571 0.1316 0.135(10) Uiso 1 calc R . .
H6C H 0.3254 -0.0095 0.1940 0.135(10) Uiso 1 calc R . .
C7 C 0.8578(5) -0.2190(4) 0.0276(2) 0.0753(9) Uani 1 d . . .
H7A H 0.8499 -0.2577 -0.0239 0.097(9) Uiso 1 calc R . .
H7B H 0.9382 -0.1443 0.0202 0.097(9) Uiso 1 calc R . .
C8 C 0.9468(6) -0.3509(5) 0.0845(3) 0.1117(15) Uani 1 d . . .
H8A H 1.0665 -0.3969 0.0629 0.144(11) Uiso 1 calc R . .
H8B H 0.8697 -0.4266 0.0920 0.144(11) Uiso 1 calc R . .
H8C H 0.9612 -0.3136 0.1351 0.144(11) Uiso 1 calc R . .
C11 C 0.0914(7) 0.2539(7) 0.6740(3) 0.107(3) Uani 0.853(11) d PDU A 1
H11A H 0.0049 0.3310 0.7004 0.129(12) Uiso 0.853(11) calc PR A 1
H11B H 0.1774 0.1954 0.7120 0.129(12) Uiso 0.853(11) calc PR A 1
H11C H 0.0251 0.1861 0.6519 0.129(12) Uiso 0.853(11) calc PR A 1
C12 C 0.1942(5) 0.3294(4) 0.60910(17) 0.0679(8) Uani 0.853(11) d PD A 1
H12 H 0.2609 0.3976 0.6331 0.064(10) Uiso 0.853(11) calc PR A 1
C11A C 0.200(5) 0.377(4) 0.6894(11) 0.112(14) Uani 0.147(11) d PDU A 2
H11D H 0.0906 0.4530 0.7000 0.167 Uiso 0.147(11) calc PR A 2
H11E H 0.3083 0.4197 0.6933 0.167 Uiso 0.147(11) calc PR A 2
H11F H 0.2041 0.2888 0.7278 0.167 Uiso 0.147(11) calc PR A 2
C12A C 0.1942(5) 0.3294(4) 0.60910(17) 0.0679(8) Uani 0.147(11) d PD A 2
H12A H 0.1096 0.2585 0.6244 0.081 Uiso 0.147(11) calc PR A 2
C13 C 0.3346(4) 0.2139(3) 0.56698(19) 0.0659(8) Uani 1 d . . .
C14 C 0.4801(6) 0.1031(4) 0.6134(3) 0.0982(13) Uani 1 d . . .
H14A H 0.5887 0.0750 0.5794 0.170(13) Uiso 1 calc R . .
H14B H 0.4333 0.0124 0.6324 0.170(13) Uiso 1 calc R . .
H14C H 0.5119 0.1509 0.6582 0.170(13) Uiso 1 calc R . .
C15 C 0.0098(6) 0.2697(5) 0.3858(2) 0.0907(11) Uani 1 d . . .
H15A H -0.0456 0.3275 0.3381 0.121(11) Uiso 1 calc R . .
H15B H 0.1068 0.1868 0.3685 0.121(11) Uiso 1 calc R . .
C16 C -0.1342(9) 0.2009(6) 0.4324(4) 0.147(2) Uani 1 d . . .
H16A H -0.1857 0.1392 0.3992 0.25(2) Uiso 1 calc R . .
H16B H -0.2309 0.2815 0.4504 0.25(2) Uiso 1 calc R . .
H16C H -0.0795 0.1371 0.4779 0.25(2) Uiso 1 calc R . .
C17 C 0.3298(5) 0.4993(4) 0.3898(2) 0.0772(9) Uani 1 d . . .
H17A H 0.2838 0.6089 0.3772 0.110(10) Uiso 1 calc R . .
H17B H 0.4281 0.4879 0.4275 0.110(10) Uiso 1 calc R . .
C18 C 0.4110(7) 0.4296(6) 0.3142(3) 0.1233(18) Uani 1 d . . .
H18A H 0.4978 0.4883 0.2889 0.164(13) Uiso 1 calc R . .
H18B H 0.3131 0.4312 0.2784 0.164(13) Uiso 1 calc R . .
H18C H 0.4738 0.3249 0.3271 0.164(13) Uiso 1 calc R . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Al1 O1 75.88(8) . 2_655
O1 Al1 C5 119.11(12) . .
O1 Al1 C5 100.62(13) 2_655 .
O1 Al1 C7 117.12(13) . .
O1 Al1 C7 104.49(12) 2_655 .
C5 Al1 C7 122.26(15) . .
O1 Al1 O2 76.75(8) . .
O1 Al1 O2 152.63(9) 2_655 .
C5 Al1 O2 91.93(13) . .
C7 Al1 O2 88.68(13) . .
O1 Al1 Al1 38.98(6) . 2_655
O1 Al1 Al1 36.91(5) 2_655 2_655
C5 Al1 Al1 114.88(12) . 2_655
C7 Al1 Al1 116.39(11) . 2_655
O2 Al1 Al1 115.73(7) . 2_655
O3 Al2 O3 75.85(9) . 2_566
O3 Al2 C15 119.96(15) . .
O3 Al2 C15 100.75(14) 2_566 .
O3 Al2 C17 118.49(13) . .
O3 Al2 C17 103.76(13) 2_566 .
C15 Al2 C17 120.33(17) . .
O3 Al2 O4 76.72(8) . .
O3 Al2 O4 152.56(9) 2_566 .
C15 Al2 O4 92.78(14) . .
C17 Al2 O4 89.40(13) . .
O3 Al2 Al2 38.98(6) . 2_566
O3 Al2 Al2 36.87(5) 2_566 2_566
C15 Al2 Al2 115.47(14) . 2_566
C17 Al2 Al2 116.71(12) . 2_566
O4 Al2 Al2 115.69(7) . 2_566
C2 O1 Al1 123.32(17) . .
C2 O1 Al1 131.76(17) . 2_655
Al1 O1 Al1 104.12(8) . 2_655
C3 O2 Al1 113.44(19) . .
C12 O3 Al2 123.28(17) . .
C12 O3 Al2 131.94(16) . 2_566
Al2 O3 Al2 104.15(9) . 2_566
C13 O4 Al2 114.3(2) . .
O1 C2 C3 107.2(2) . .
O1 C2 C1 112.4(3) . .
C3 C2 C1 111.9(3) . .
O2 C3 C4 121.5(3) . .
O2 C3 C2 118.1(3) . .
C4 C3 C2 120.4(3) . .
C6 C5 Al1 114.3(2) . .
C8 C7 Al1 115.4(3) . .
O3 C12 C11 113.5(3) . .
O3 C12 C13 107.5(2) . .
C11 C12 C13 111.7(3) . .
O4 C13 C14 122.4(3) . .
O4 C13 C12 117.5(3) . .
C14 C13 C12 120.1(3) . .
C16 C15 Al2 115.6(3) . .
C18 C17 Al2 114.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O1 1.8452(18) .
Al1 O1 1.9328(19) 2_655
Al1 C5 1.971(3) .
Al1 C7 1.987(3) .
Al1 O2 2.166(2) .
Al1 Al1 2.9799(17) 2_655
Al2 O3 1.8423(18) .
Al2 O3 1.9311(19) 2_566
Al2 C15 1.959(4) .
Al2 C17 1.984(3) .
Al2 O4 2.158(2) .
Al2 Al2 2.9770(17) 2_566
O1 C2 1.406(3) .
O1 Al1 1.9328(19) 2_655
O2 C3 1.215(4) .
O3 C12 1.405(3) .
O3 Al2 1.9311(19) 2_566
O4 C13 1.211(4) .
C1 C2 1.502(4) .
C2 C3 1.501(4) .
C3 C4 1.495(4) .
C5 C6 1.504(5) .
C7 C8 1.501(5) .
C11 C12 1.477(5) .
C12 C13 1.500(4) .
C13 C14 1.495(5) .
C15 C16 1.479(7) .
C17 C18 1.508(5) .
