#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:08:33 +0100 (lun 21 de mar de 2016) $
#$Revision: 178596 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/07/4070726.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_4070726
loop_
_publ_author_name
'Yang, Ying'
'Schulz, Thomas'
'John, Michael'
'Yang, Zhi'
'Jiménez-Pérez, Victor Manuel'
'Roesky, Herbert W.'
'Gurubasavaraj, Prabhuodeyara M.'
'Stalke, Dietmar'
'Ye, Hongqi'
_publ_contact_author
'Prof. Dr. Dietmar Stalke, Prof. Dr. H. W. Roesky'
_publ_section_title
;
 Organoaluminum Hydroxides Supported by β-Diketiminato Ligands:
 Synthesis, Structural Characterization, and Reactions
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              769
_journal_paper_doi               10.1021/om700969g
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C32 H38 Al N2 O'
_chemical_formula_weight         493.62
_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                93.6510(10)
_cell_angle_beta                 106.2490(10)
_cell_angle_gamma                114.6840(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4187(11)
_cell_length_b                   11.5317(11)
_cell_length_c                   12.1602(11)
_cell_measurement_reflns_used    8831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.302
_cell_measurement_theta_min      2.2395
_cell_volume                     1366.6(2)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.1.0'
_computing_data_reduction        'SAINT V7.23A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.12'
_computing_publication_material  'XP in SHELXTL ver. 6.12'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.12'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.12'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker TXS-Mo rotating anode with APEX II detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25588
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.786432
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5606
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0392
_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)+(0.0428P)²+0.7135P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                4370
_reflns_number_total             5606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700969g-file002.cif
_cod_data_source_block           L1AlPh(OH)
_cod_original_cell_volume        1366.5(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070726
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
Al1 Al 0.56565(5) 0.92300(4) 0.46171(4) 0.02065(12) Uani 1 1 d .
O1 O 0.40129(12) 0.93667(11) 0.42935(10) 0.0237(2) Uani 1 1 d D
H100 H 0.3298(16) 0.8910(17) 0.3772(15) 0.028 Uiso 1 1 d D
N1 N 0.71555(14) 0.89887(12) 0.57238(11) 0.0218(3) Uani 1 1 d .
N2 N 0.45955(14) 0.73228(12) 0.40475(11) 0.0220(3) Uani 1 1 d .
C1 C 0.43616(18) 0.51735(16) 0.32831(15) 0.0289(4) Uani 1 1 d .
H1A H 0.3726 0.4668 0.3670 0.043 Uiso 1 1 calc R
H1B H 0.4972 0.4787 0.3248 0.043 Uiso 1 1 calc R
H1C H 0.3843 0.5164 0.2487 0.043 Uiso 1 1 calc R
C2 C 0.52004(17) 0.65622(15) 0.39675(14) 0.0236(3) Uani 1 1 d .
C3 C 0.65921(17) 0.69564(15) 0.45481(14) 0.0242(3) Uani 1 1 d .
H3 H 0.6977 0.6448 0.4292 0.029 Uiso 1 1 calc R
C4 C 0.74648(17) 0.80277(15) 0.54677(14) 0.0229(3) Uani 1 1 d .
C5 C 0.87752(17) 0.80412(17) 0.62108(15) 0.0278(4) Uani 1 1 d .
H5A H 0.9547 0.8895 0.6312 0.042 Uiso 1 1 calc R
H5B H 0.8915 0.7361 0.5825 0.042 Uiso 1 1 calc R
H5C H 0.8715 0.7876 0.6979 0.042 Uiso 1 1 calc R
C6 C 0.80281(17) 0.98693(15) 0.68415(14) 0.0228(3) Uani 1 1 d .
C7 C 0.77876(17) 0.94969(16) 0.78649(14) 0.0240(3) Uani 1 1 d .
C8 C 0.86359(18) 1.03428(16) 0.89367(15) 0.0268(4) Uani 1 1 d .
H8 H 0.8472 1.0090 0.9629 0.032 Uiso 1 1 calc R
C9 C 0.97127(18) 1.15417(17) 0.90302(15) 0.0281(4) Uani 1 1 d .
C10 C 0.99393(17) 1.18820(16) 0.80071(15) 0.0278(4) Uani 1 1 d .
H10 H 1.0680 1.2696 0.8056 0.033 Uiso 1 1 calc R
C11 C 0.91170(17) 1.10705(16) 0.69119(15) 0.0249(4) Uani 1 1 d .
C12 C 0.66658(18) 0.81847(16) 0.78251(15) 0.0277(4) Uani 1 1 d .
H12A H 0.6998 0.7527 0.7812 0.042 Uiso 1 1 calc R
H12B H 0.5873 0.7948 0.7118 0.042 Uiso 1 1 calc R
H12C H 0.6397 0.8225 0.8519 0.042 Uiso 1 1 calc R
C13 C 0.94365(19) 1.14791(17) 0.58370(16) 0.0313(4) Uani 1 1 d .
H13A H 1.0253 1.2326 0.6065 0.047 Uiso 1 1 calc R
H13B H 0.8659 1.1550 0.5304 0.047 Uiso 1 1 calc R
H13C H 0.9606 1.0827 0.5442 0.047 Uiso 1 1 calc R
C14 C 1.0599(2) 1.24557(18) 1.02032(16) 0.0380(5) Uani 1 1 d .
H14A H 1.0192 1.3014 1.0375 0.057 Uiso 1 1 calc R
H14B H 1.1517 1.3000 1.0183 0.057 Uiso 1 1 calc R
H14C H 1.0663 1.1947 1.0813 0.057 Uiso 1 1 calc R
C15 C 0.31161(17) 0.66694(15) 0.35103(14) 0.0240(3) Uani 1 1 d .
C16 C 0.25014(18) 0.65401(16) 0.23070(15) 0.0275(4) Uani 1 1 d .
C17 C 0.10856(19) 0.58063(17) 0.18184(16) 0.0315(4) Uani 1 1 d .
H17 H 0.0661 0.5715 0.1004 0.038 Uiso 1 1 calc R
C18 C 0.02719(18) 0.52057(17) 0.24674(17) 0.0333(4) Uani 1 1 d .
C19 C 0.09121(18) 0.53840(17) 0.36643(16) 0.0316(4) Uani 1 1 d .
H19 H 0.0370 0.4993 0.4130 0.038 Uiso 1 1 calc R
C20 C 0.23154(17) 0.61138(16) 0.41994(15) 0.0263(4) Uani 1 1 d .
C21 C 0.29614(19) 0.62910(18) 0.54979(16) 0.0322(4) Uani 1 1 d .
H21A H 0.3233 0.7181 0.5882 0.048 Uiso 1 1 calc R
H21B H 0.3771 0.6141 0.5656 0.048 Uiso 1 1 calc R
H21C H 0.2301 0.5666 0.5802 0.048 Uiso 1 1 calc R
C22 C 0.3311(2) 0.71233(19) 0.15272(16) 0.0355(4) Uani 1 1 d .
H22A H 0.3080 0.6441 0.0867 0.053 Uiso 1 1 calc R
H22B H 0.4291 0.7505 0.1974 0.053 Uiso 1 1 calc R
H22C H 0.3088 0.7803 0.1231 0.053 Uiso 1 1 calc R
C23 C -0.1252(2) 0.4387(2) 0.1904(2) 0.0487(5) Uani 1 1 d .
H23A H -0.1720 0.4616 0.2378 0.073 Uiso 1 1 calc R
H23B H -0.1477 0.3462 0.1850 0.073 Uiso 1 1 calc R
H23C H -0.1549 0.4550 0.1117 0.073 Uiso 1 1 calc R
C24 C 0.63183(17) 0.98344(15) 0.33051(14) 0.0242(3) Uani 1 1 d .
C25 C 0.72868(17) 0.95822(16) 0.29726(15) 0.0260(4) Uani 1 1 d .
H25 H 0.7737 0.9165 0.3446 0.031 Uiso 1 1 calc R
C26 C 0.76150(18) 0.99163(17) 0.19817(15) 0.0297(4) Uani 1 1 d .
H26 H 0.8272 0.9720 0.1789 0.036 Uiso 1 1 calc R
C27 C 0.69873(19) 1.05339(17) 0.12743(16) 0.0323(4) Uani 1 1 d .
H27 H 0.7211 1.0767 0.0598 0.039 Uiso 1 1 calc R
C28 C 0.60268(19) 1.08060(18) 0.15692(16) 0.0322(4) Uani 1 1 d .
H28 H 0.5590 1.1232 0.1096 0.039 Uiso 1 1 calc R
C29 C 0.57051(18) 1.04556(16) 0.25540(15) 0.0279(4) Uani 1 1 d .
H29 H 0.5036 1.0644 0.2732 0.034 Uiso 1 1 calc R
C30 C 0.5409(2) 0.4391(2) 0.0855(2) 0.0468(5) Uani 1 1 d .
H30 H 0.5696 0.3975 0.1450 0.056 Uiso 1 1 calc R
C31 C 0.5917(2) 0.5729(2) 0.1080(2) 0.0492(5) Uani 1 1 d .
H31 H 0.6552 0.6231 0.1829 0.059 Uiso 1 1 calc R
C32 C 0.5506(2) 0.6341(2) 0.0222(2) 0.0466(5) Uani 1 1 d .
H32 H 0.5856 0.7263 0.0376 0.056 Uiso 1 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'
N N 0.0061 0.0033 '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
O1 Al1 O1 72.82(6) 2_676
O1 Al1 N2 144.59(6) 2_676
O1 Al1 N2 89.84(6) .
O1 Al1 N1 90.40(6) 2_676
O1 Al1 N1 149.75(6) .
N2 Al1 N1 89.98(6) .
O1 Al1 C24 110.98(6) 2_676
O1 Al1 C24 103.95(6) .
N2 Al1 C24 102.97(6) .
N1 Al1 C24 105.56(7) .
Al1 O1 Al1 107.18(6) 2_676
C4 N1 C6 114.94(13) .
C4 N1 Al1 122.44(11) .
C6 N1 Al1 122.58(10) .
C2 N2 C15 114.50(13) .
C2 N2 Al1 122.00(11) .
C15 N2 Al1 122.77(10) .
N2 C2 C3 123.40(15) .
N2 C2 C1 120.14(15) .
C3 C2 C1 116.36(14) .
C4 C3 C2 125.91(15) .
N1 C4 C3 122.64(15) .
N1 C4 C5 120.47(15) .
C3 C4 C5 116.85(14) .
C11 C6 C7 119.99(15) .
C11 C6 N1 120.78(14) .
C7 C6 N1 119.22(14) .
C8 C7 C6 118.95(16) .
C8 C7 C12 119.70(15) .
C6 C7 C12 121.31(15) .
C9 C8 C7 122.24(16) .
C8 C9 C10 117.74(16) .
C8 C9 C14 121.16(17) .
C10 C9 C14 121.09(17) .
C9 C10 C11 122.23(16) .
C10 C11 C6 118.85(15) .
C10 C11 C13 119.73(15) .
C6 C11 C13 121.40(15) .
C20 C15 C16 120.49(15) .
C20 C15 N2 118.96(14) .
C16 C15 N2 120.47(15) .
C17 C16 C15 118.06(16) .
C17 C16 C22 119.18(16) .
C15 C16 C22 122.72(16) .
C18 C17 C16 122.81(17) .
C17 C18 C19 117.55(17) .
C17 C18 C23 121.40(18) .
C19 C18 C23 121.05(18) .
C20 C19 C18 122.11(17) .
C19 C20 C15 118.90(16) .
C19 C20 C21 120.27(16) .
C15 C20 C21 120.83(15) .
C25 C24 C29 114.62(15) .
C25 C24 Al1 125.19(12) .
C29 C24 Al1 119.88(13) .
C26 C25 C24 122.87(16) .
C27 C26 C25 120.24(17) .
C26 C27 C28 118.95(16) .
C29 C28 C27 119.94(16) .
C28 C29 C24 123.36(16) .
C32 C30 C31 120.3(2) 2_665
C30 C31 C32 120.3(2) .
C30 C32 C31 119.4(2) 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O1 1.8583(12) 2_676
Al1 O1 1.8825(12) .
Al1 N2 1.9736(14) .
Al1 N1 1.9937(14) .
Al1 C24 1.9946(18) .
O1 Al1 1.8583(12) 2_676
N1 C4 1.339(2) .
N1 C6 1.447(2) .
N2 C2 1.337(2) .
N2 C15 1.451(2) .
C1 C2 1.509(2) .
C2 C3 1.399(2) .
C3 C4 1.394(2) .
C4 C5 1.509(2) .
C6 C11 1.400(2) .
C6 C7 1.403(2) .
C7 C8 1.390(2) .
C7 C12 1.507(2) .
C8 C9 1.385(3) .
C9 C10 1.388(2) .
C9 C14 1.510(2) .
C10 C11 1.392(2) .
C11 C13 1.505(2) .
C15 C20 1.399(2) .
C15 C16 1.402(2) .
C16 C17 1.392(2) .
C16 C22 1.503(3) .
C17 C18 1.381(3) .
C18 C19 1.391(3) .
C18 C23 1.505(3) .
C19 C20 1.385(2) .
C20 C21 1.503(2) .
C24 C25 1.405(2) .
C24 C29 1.408(2) .
C25 C26 1.390(2) .
C26 C27 1.386(3) .
C27 C28 1.387(3) .
C28 C29 1.384(2) .
C30 C32 1.370(3) 2_665
C30 C31 1.379(3) .
C31 C32 1.381(3) .
C32 C30 1.370(3) 2_665
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
_geom_torsion_site_symmetry_4
O1 Al1 O1 Al1 0.0 2_676 2_676
N2 Al1 O1 Al1 148.65(7) . 2_676
N1 Al1 O1 Al1 58.97(13) . 2_676
C24 Al1 O1 Al1 -108.02(7) . 2_676
O1 Al1 N1 C4 178.19(13) 2_676 .
O1 Al1 N1 C4 123.24(14) . .
N2 Al1 N1 C4 33.59(13) . .
C24 Al1 N1 C4 -69.88(14) . .
O1 Al1 N1 C6 -4.51(12) 2_676 .
O1 Al1 N1 C6 -59.46(18) . .
N2 Al1 N1 C6 -149.11(12) . .
C24 Al1 N1 C6 107.42(13) . .
O1 Al1 N2 C2 -125.24(13) 2_676 .
O1 Al1 N2 C2 175.69(13) . .
N1 Al1 N2 C2 -34.57(13) . .
C24 Al1 N2 C2 71.41(13) . .
O1 Al1 N2 C15 65.07(16) 2_676 .
O1 Al1 N2 C15 5.99(13) . .
N1 Al1 N2 C15 155.74(12) . .
C24 Al1 N2 C15 -98.29(13) . .
C15 N2 C2 C3 -171.92(15) . .
Al1 N2 C2 C3 17.6(2) . .
C15 N2 C2 C1 4.3(2) . .
Al1 N2 C2 C1 -166.20(12) . .
N2 C2 C3 C4 15.2(3) . .
C1 C2 C3 C4 -161.10(16) . .
C6 N1 C4 C3 167.42(15) . .
Al1 N1 C4 C3 -15.1(2) . .
C6 N1 C4 C5 -10.1(2) . .
Al1 N1 C4 C5 167.36(12) . .
C2 C3 C4 N1 -16.4(3) . .
C2 C3 C4 C5 161.19(16) . .
C4 N1 C6 C11 98.41(18) . .
Al1 N1 C6 C11 -79.08(17) . .
C4 N1 C6 C7 -80.45(18) . .
Al1 N1 C6 C7 102.07(15) . .
C11 C6 C7 C8 0.6(2) . .
N1 C6 C7 C8 179.51(14) . .
C11 C6 C7 C12 -177.11(15) . .
N1 C6 C7 C12 1.8(2) . .
C6 C7 C8 C9 -0.1(2) . .
C12 C7 C8 C9 177.72(15) . .
C7 C8 C9 C10 -0.6(2) . .
C7 C8 C9 C14 178.57(16) . .
C8 C9 C10 C11 0.8(2) . .
C14 C9 C10 C11 -178.43(16) . .
C9 C10 C11 C6 -0.2(2) . .
C9 C10 C11 C13 -178.45(15) . .
C7 C6 C11 C10 -0.5(2) . .
N1 C6 C11 C10 -179.35(14) . .
C7 C6 C11 C13 177.70(15) . .
N1 C6 C11 C13 -1.1(2) . .
C2 N2 C15 C20 92.68(18) . .
Al1 N2 C15 C20 -96.92(16) . .
C2 N2 C15 C16 -84.16(18) . .
Al1 N2 C15 C16 86.24(17) . .
C20 C15 C16 C17 -2.3(2) . .
N2 C15 C16 C17 174.47(14) . .
C20 C15 C16 C22 179.63(16) . .
N2 C15 C16 C22 -3.6(2) . .
C15 C16 C17 C18 -0.1(3) . .
C22 C16 C17 C18 178.05(17) . .
C16 C17 C18 C19 1.8(3) . .
C16 C17 C18 C23 -178.21(18) . .
C17 C18 C19 C20 -1.1(3) . .
C23 C18 C19 C20 178.84(18) . .
C18 C19 C20 C15 -1.2(3) . .
C18 C19 C20 C21 179.41(16) . .
C16 C15 C20 C19 2.9(2) . .
N2 C15 C20 C19 -173.92(14) . .
C16 C15 C20 C21 -177.65(15) . .
N2 C15 C20 C21 5.5(2) . .
O1 Al1 C24 C25 121.89(14) 2_676 .
O1 Al1 C24 C25 -161.46(14) . .
N2 Al1 C24 C25 -68.35(15) . .
N1 Al1 C24 C25 25.31(16) . .
O1 Al1 C24 C29 -64.80(15) 2_676 .
O1 Al1 C24 C29 11.85(15) . .
N2 Al1 C24 C29 104.96(13) . .
N1 Al1 C24 C29 -161.38(13) . .
C29 C24 C25 C26 -0.1(2) . .
Al1 C24 C25 C26 173.55(13) . .
C24 C25 C26 C27 0.5(3) . .
C25 C26 C27 C28 -0.3(3) . .
C26 C27 C28 C29 -0.3(3) . .
C27 C28 C29 C24 0.7(3) . .
C25 C24 C29 C28 -0.5(3) . .
Al1 C24 C29 C28 -174.49(14) . .
C32 C30 C31 C32 0.0(4) 2_665 .
C30 C31 C32 C30 0.0(4) . 2_665
