#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:37:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179386 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/83/4328328.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_4328328
loop_
_publ_author_name
'Ying Yang'
'Haipu Li'
'Chen Wang'
'Herbert W. Roesky'
_publ_contact_author
;
Herbert W. ROESKY
;
_publ_contact_author_address
;
Institut fuer Anorganische Chemie
Universitaet Goettingen
Tammannstrasse 4, 37077 Goettingen (Germany)
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_section_title
;
 Studies of the Ligand Effect on the Synthesis of Dialuminoxanes by
 Various β-Diketiminato Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2204
_journal_page_last               2211
_journal_paper_doi               10.1021/ic2021879
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C132 H183 Al4 N4 O8'
_chemical_formula_weight         2061.74
_chemical_name_common            iPr_LAl(OH)(mu-O)Al(OAr*)2
_chemical_name_systematic
; 
 ? 
;
_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                 100.695(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6794(3)
_cell_length_b                   20.4959(5)
_cell_length_c                   21.2644(4)
_cell_measurement_reflns_used    12789
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0819
_cell_measurement_theta_min      2.7786
_cell_volume                     6286.6(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47010
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_correction_T_min  0.9470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       block
_exptl_crystal_F_000             2238
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         11048
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0616
_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)+(0.0659P)²+4.0439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                8542
_reflns_number_total             11048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2021879_si_002_01.cif
_cod_data_source_block           compound3'
_cod_database_code               4328328
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 0.02522(5) 0.23226(3) 0.08614(3) 0.02304(17) Uani 1 1 d U . .
Al2 Al 0.11057(5) 0.21751(3) 0.23944(3) 0.02138(17) Uani 1 1 d . . .
N1 N 0.10132(13) 0.24676(9) 0.02402(9) 0.0233(4) Uani 1 1 d . . .
N2 N -0.06254(13) 0.29839(10) 0.05708(9) 0.0238(4) Uani 1 1 d . . .
O1 O -0.0236(2) 0.15739(14) 0.06717(14) 0.0897(9) Uani 1 1 d U . .
H1 H -0.0584 0.1479 0.0930 0.134 Uiso 1 1 calc R . .
O2 O 0.07659(11) 0.24251(8) 0.16444(7) 0.0273(4) Uani 1 1 d . . .
O3 O 0.21827(10) 0.22675(8) 0.28346(7) 0.0268(4) Uani 1 1 d . . .
O4 O 0.04746(11) 0.17578(8) 0.28437(8) 0.0293(4) Uani 1 1 d . . .
C1 C 0.11801(18) 0.26925(14) -0.08713(12) 0.0364(6) Uani 1 1 d . . .
H1A H 0.1778 0.2910 -0.0731 0.055 Uiso 1 1 calc R . .
H1B H 0.0831 0.2922 -0.1244 0.055 Uiso 1 1 calc R . .
H1C H 0.1285 0.2240 -0.0988 0.055 Uiso 1 1 calc R . .
C2 C 0.06377(17) 0.27021(12) -0.03365(11) 0.0264(5) Uani 1 1 d . . .
C3 C -0.02519(17) 0.29778(13) -0.04758(11) 0.0292(6) Uani 1 1 d . . .
H3 H -0.0494 0.3056 -0.0915 0.035 Uiso 1 1 calc R . .
C4 C -0.08198(16) 0.31500(12) -0.00499(11) 0.0276(5) Uani 1 1 d . . .
C5 C -0.16633(19) 0.35542(15) -0.02999(12) 0.0400(7) Uani 1 1 d . . .
H5A H -0.2197 0.3377 -0.0140 0.060 Uiso 1 1 calc R . .
H5B H -0.1788 0.3543 -0.0769 0.060 Uiso 1 1 calc R . .
H5C H -0.1554 0.4006 -0.0154 0.060 Uiso 1 1 calc R . .
C6 C 0.19626(16) 0.22378(12) 0.03266(10) 0.0251(5) Uani 1 1 d . . .
C7 C 0.26756(17) 0.26658(13) 0.06027(11) 0.0293(6) Uani 1 1 d . B .
C8 C 0.35824(18) 0.24456(14) 0.06675(13) 0.0379(7) Uani 1 1 d . . .
H8 H 0.4075 0.2726 0.0852 0.045 Uiso 1 1 calc R . .
C9 C 0.37870(19) 0.18316(15) 0.04718(13) 0.0423(7) Uani 1 1 d . . .
H9 H 0.4414 0.1693 0.0519 0.051 Uiso 1 1 calc R . .
C10 C 0.30794(19) 0.14187(14) 0.02075(13) 0.0381(7) Uani 1 1 d . . .
H10 H 0.3226 0.0994 0.0077 0.046 Uiso 1 1 calc R . .
C11 C 0.21519(17) 0.16090(12) 0.01264(11) 0.0292(6) Uani 1 1 d . . .
C12 C 0.14042(19) 0.11334(13) -0.01727(12) 0.0352(6) Uani 1 1 d . . .
H12 H 0.0801 0.1374 -0.0256 0.042 Uiso 1 1 calc R . .
C13 C 0.1311(2) 0.05673(15) 0.02774(15) 0.0498(8) Uani 1 1 d . . .
H13A H 0.1908 0.0343 0.0393 0.075 Uiso 1 1 calc R . .
H13B H 0.0843 0.0260 0.0063 0.075 Uiso 1 1 calc R . .
H13C H 0.1122 0.0735 0.0665 0.075 Uiso 1 1 calc R . .
C14 C 0.1578(2) 0.08653(16) -0.08143(14) 0.0546(8) Uani 1 1 d . . .
H14A H 0.1653 0.1229 -0.1099 0.082 Uiso 1 1 calc R . .
H14B H 0.1049 0.0597 -0.1012 0.082 Uiso 1 1 calc R . .
H14C H 0.2142 0.0599 -0.0741 0.082 Uiso 1 1 calc R . .
C15 C 0.24701(19) 0.33436(13) 0.08176(13) 0.0381(6) Uani 1 1 d D . .
H15 H 0.1801 0.3423 0.0829 0.046 Uiso 1 1 calc R A 1
C16 C 0.2295(6) 0.3843(2) 0.0291(2) 0.0610(17) Uani 0.745(10) 1 d PD B 2
H16A H 0.2833 0.3865 0.0080 0.091 Uiso 0.745(10) 1 calc PR B 2
H16B H 0.2192 0.4270 0.0472 0.091 Uiso 0.745(10) 1 calc PR B 2
H16C H 0.1745 0.3718 -0.0022 0.091 Uiso 0.745(10) 1 calc PR B 2
C6' C 0.2906(16) 0.3841(8) 0.0325(7) 0.0610(17) Uani 0.255(10) 1 d PD B 1
H6'1 H 0.2675 0.4285 0.0365 0.091 Uiso 0.255(10) 1 calc PR B 1
H6'2 H 0.2715 0.3691 -0.0117 0.091 Uiso 0.255(10) 1 calc PR B 1
H6'3 H 0.3585 0.3840 0.0439 0.091 Uiso 0.255(10) 1 calc PR B 1
C17 C 0.3121(3) 0.35694(16) 0.14038(15) 0.0588(9) Uani 1 1 d . B .
H17A H 0.3733 0.3652 0.1298 0.088 Uiso 1 1 calc R . .
H17B H 0.3173 0.3232 0.1735 0.088 Uiso 1 1 calc R . .
H17C H 0.2883 0.3972 0.1562 0.088 Uiso 1 1 calc R . .
C18 C -0.11702(16) 0.32918(12) 0.09947(11) 0.0276(6) Uani 1 1 d . . .
C19 C -0.19240(17) 0.29581(14) 0.11610(12) 0.0328(6) Uani 1 1 d . . .
C20 C -0.2401(2) 0.32643(16) 0.15865(14) 0.0451(7) Uani 1 1 d . . .
H20 H -0.2905 0.3044 0.1716 0.054 Uiso 1 1 calc R . .
C21 C -0.2163(2) 0.38737(16) 0.18226(15) 0.0524(9) Uani 1 1 d . . .
H21 H -0.2501 0.4071 0.2112 0.063 Uiso 1 1 calc R . .
C22 C -0.1436(2) 0.42028(15) 0.16428(14) 0.0453(7) Uani 1 1 d . . .
H22 H -0.1280 0.4627 0.1807 0.054 Uiso 1 1 calc R . .
C23 C -0.09254(18) 0.39214(13) 0.12222(12) 0.0327(6) Uani 1 1 d . . .
C24 C -0.01146(19) 0.42929(13) 0.10370(13) 0.0363(6) Uani 1 1 d . . .
H24 H 0.0056 0.4068 0.0658 0.044 Uiso 1 1 calc R . .
C25 C -0.0351(2) 0.49977(15) 0.08467(16) 0.0557(8) Uani 1 1 d . . .
H25A H -0.0909 0.5009 0.0513 0.083 Uiso 1 1 calc R . .
H25B H 0.0167 0.5196 0.0684 0.083 Uiso 1 1 calc R . .
H25C H -0.0463 0.5242 0.1221 0.083 Uiso 1 1 calc R . .
C26 C 0.0723(2) 0.42579(16) 0.15802(15) 0.0495(8) Uani 1 1 d . . .
H26A H 0.0574 0.4471 0.1961 0.074 Uiso 1 1 calc R . .
H26B H 0.1250 0.4480 0.1451 0.074 Uiso 1 1 calc R . .
H26C H 0.0883 0.3800 0.1677 0.074 Uiso 1 1 calc R . .
C27 C -0.22475(18) 0.22981(14) 0.08852(12) 0.0378(6) Uani 1 1 d . . .
H27 H -0.1860 0.2180 0.0562 0.045 Uiso 1 1 calc R . .
C28 C -0.3262(2) 0.2321(2) 0.05409(16) 0.0615(9) Uani 1 1 d . . .
H28A H -0.3659 0.2432 0.0849 0.092 Uiso 1 1 calc R . .
H28B H -0.3442 0.1894 0.0351 0.092 Uiso 1 1 calc R . .
H28C H -0.3334 0.2652 0.0203 0.092 Uiso 1 1 calc R . .
C29 C -0.2108(2) 0.17742(16) 0.13965(15) 0.0550(8) Uani 1 1 d . . .
H29A H -0.1456 0.1765 0.1609 0.083 Uiso 1 1 calc R . .
H29B H -0.2281 0.1349 0.1199 0.083 Uiso 1 1 calc R . .
H29C H -0.2498 0.1869 0.1713 0.083 Uiso 1 1 calc R . .
C30 C 0.30850(15) 0.24071(12) 0.28093(10) 0.0241(5) Uani 1 1 d . . .
C31 C 0.34877(16) 0.29867(12) 0.30911(11) 0.0249(5) Uani 1 1 d . . .
C32 C 0.43741(16) 0.31422(12) 0.29939(11) 0.0277(5) Uani 1 1 d . . .
H32 H 0.4654 0.3533 0.3176 0.033 Uiso 1 1 calc R . .
C33 C 0.48653(16) 0.27523(13) 0.26438(11) 0.0299(6) Uani 1 1 d . . .
C34 C 0.44886(17) 0.21573(13) 0.24355(12) 0.0304(6) Uani 1 1 d . . .
H34 H 0.4839 0.1873 0.2220 0.037 Uiso 1 1 calc R . .
C35 C 0.36178(17) 0.19544(12) 0.25264(11) 0.0268(5) Uani 1 1 d . . .
C36 C 0.32963(17) 0.12519(12) 0.23614(11) 0.0303(6) Uani 1 1 d . . .
C37 C 0.2407(2) 0.12202(15) 0.18560(15) 0.0521(8) Uani 1 1 d . . .
H37A H 0.2348 0.0786 0.1660 0.078 Uiso 1 1 calc R . .
H37B H 0.2432 0.1550 0.1526 0.078 Uiso 1 1 calc R . .
H37C H 0.1871 0.1305 0.2059 0.078 Uiso 1 1 calc R . .
C38 C 0.3145(2) 0.09089(13) 0.29731(13) 0.0389(7) Uani 1 1 d . . .
H38A H 0.2687 0.1151 0.3162 0.058 Uiso 1 1 calc R . .
H38B H 0.3733 0.0891 0.3279 0.058 Uiso 1 1 calc R . .
H38C H 0.2920 0.0465 0.2870 0.058 Uiso 1 1 calc R . .
C39 C 0.4028(2) 0.08528(15) 0.20981(15) 0.0484(8) Uani 1 1 d . . .
H39A H 0.3813 0.0401 0.2026 0.073 Uiso 1 1 calc R . .
H39B H 0.4613 0.0859 0.2407 0.073 Uiso 1 1 calc R . .
H39C H 0.4124 0.1043 0.1693 0.073 Uiso 1 1 calc R . .
C40 C 0.29796(17) 0.34550(12) 0.34763(12) 0.0296(6) Uani 1 1 d . . .
C41 C 0.25618(18) 0.30882(13) 0.39822(12) 0.0346(6) Uani 1 1 d . . .
H41A H 0.2213 0.3394 0.4201 0.052 Uiso 1 1 calc R . .
H41B H 0.3060 0.2890 0.4294 0.052 Uiso 1 1 calc R . .
H41C H 0.2145 0.2746 0.3775 0.052 Uiso 1 1 calc R . .
C42 C 0.22298(19) 0.38229(14) 0.30158(14) 0.0428(7) Uani 1 1 d . . .
H42A H 0.1832 0.3510 0.2745 0.064 Uiso 1 1 calc R . .
H42B H 0.2522 0.4114 0.2747 0.064 Uiso 1 1 calc R . .
H42C H 0.1854 0.4080 0.3261 0.064 Uiso 1 1 calc R . .
C43 C 0.3640(2) 0.39625(15) 0.38474(15) 0.0484(8) Uani 1 1 d . . .
H43A H 0.3902 0.4233 0.3545 0.073 Uiso 1 1 calc R . .
H43B H 0.4142 0.3739 0.4135 0.073 Uiso 1 1 calc R . .
H43C H 0.3298 0.4239 0.4099 0.073 Uiso 1 1 calc R . .
C44 C 0.57849(18) 0.29634(14) 0.24957(14) 0.0404(7) Uani 1 1 d . . .
H44A H 0.6170 0.2578 0.2465 0.061 Uiso 1 1 calc R . .
H44B H 0.6099 0.3250 0.2837 0.061 Uiso 1 1 calc R . .
H44C H 0.5684 0.3199 0.2088 0.061 Uiso 1 1 calc R . .
C45 C -0.04023(16) 0.15862(12) 0.29190(11) 0.0252(5) Uani 1 1 d . . .
C46 C -0.09759(16) 0.20553(11) 0.31341(11) 0.0238(5) Uani 1 1 d . . .
C47 C -0.18797(17) 0.18711(12) 0.31634(12) 0.0287(6) Uani 1 1 d . . .
H47 H -0.2282 0.2185 0.3295 0.034 Uiso 1 1 calc R . .
C48 C -0.22148(17) 0.12499(12) 0.30083(13) 0.0328(6) Uani 1 1 d . . .
C49 C -0.16106(18) 0.07922(12) 0.28491(13) 0.0336(6) Uani 1 1 d . . .
H49 H -0.1826 0.0358 0.2765 0.040 Uiso 1 1 calc R . .
C50 C -0.06968(18) 0.09368(12) 0.28064(12) 0.0309(6) Uani 1 1 d . . .
C51 C -0.0058(2) 0.03972(13) 0.26379(16) 0.0481(8) Uani 1 1 d . . .
C52 C -0.0508(3) -0.02851(14) 0.26325(19) 0.0641(11) Uani 1 1 d . . .
H52A H -0.0069 -0.0617 0.2542 0.096 Uiso 1 1 calc R . .
H52B H -0.1069 -0.0299 0.2301 0.096 Uiso 1 1 calc R . .
H52C H -0.0671 -0.0372 0.3051 0.096 Uiso 1 1 calc R . .
C53 C 0.0831(2) 0.03650(16) 0.3132(2) 0.0713(12) Uani 1 1 d . . .
H53A H 0.1139 0.0791 0.3162 0.107 Uiso 1 1 calc R . .
H53B H 0.1243 0.0034 0.3004 0.107 Uiso 1 1 calc R . .
H53C H 0.0685 0.0248 0.3549 0.107 Uiso 1 1 calc R . .
C54 C 0.0112(3) 0.05180(16) 0.19530(19) 0.0710(12) Uani 1 1 d . . .
H54A H 0.0367 0.0957 0.1926 0.106 Uiso 1 1 calc R . .
H54B H -0.0475 0.0480 0.1649 0.106 Uiso 1 1 calc R . .
H54C H 0.0552 0.0194 0.1849 0.106 Uiso 1 1 calc R . .
C55 C -0.06162(17) 0.27315(12) 0.33748(12) 0.0290(6) Uani 1 1 d . . .
C56 C 0.0084(2) 0.26395(15) 0.40013(13) 0.0428(7) Uani 1 1 d . . .
H56A H 0.0363 0.3061 0.4143 0.064 Uiso 1 1 calc R . .
H56B H 0.0570 0.2335 0.3930 0.064 Uiso 1 1 calc R . .
H56C H -0.0235 0.2463 0.4330 0.064 Uiso 1 1 calc R . .
C57 C -0.13964(19) 0.31703(13) 0.35243(14) 0.0403(7) Uani 1 1 d . . .
H57A H -0.1870 0.3225 0.3137 0.060 Uiso 1 1 calc R . .
H57B H -0.1142 0.3598 0.3670 0.060 Uiso 1 1 calc R . .
H57C H -0.1676 0.2968 0.3861 0.060 Uiso 1 1 calc R . .
C58 C -0.01509(19) 0.31010(13) 0.28886(13) 0.0369(6) Uani 1 1 d . . .
H58A H -0.0445 0.2976 0.2453 0.055 Uiso 1 1 calc R . .
H58B H 0.0510 0.2990 0.2959 0.055 Uiso 1 1 calc R . .
H58C H -0.0221 0.3572 0.2944 0.055 Uiso 1 1 calc R . .
C59 C -0.3209(2) 0.10699(15) 0.30196(17) 0.0514(8) Uani 1 1 d . . .
H59A H -0.3405 0.0719 0.2711 0.077 Uiso 1 1 calc R . .
H59B H -0.3606 0.1452 0.2905 0.077 Uiso 1 1 calc R . .
H59C H -0.3261 0.0922 0.3450 0.077 Uiso 1 1 calc R . .
C60 C 0.6140(11) 0.4675(14) 1.0497(8) 0.191(6) Uani 0.50 1 d PU . .
C61 C 0.5640(11) 0.4110(6) 1.0051(7) 0.238(6) Uani 1 1 d U . .
C62 C 0.4694(17) 0.4251(10) 0.9606(9) 0.175(5) Uani 0.50 1 d PU . .
C63 C 0.4398(6) 0.4817(5) 0.9605(3) 0.129(2) Uani 1 1 d U . .
C64 C 0.4807(11) 0.5328(6) 1.0022(6) 0.108(3) Uani 0.50 1 d PU . .
C65 C 0.5840(9) 0.0338(5) 0.0108(7) 0.206(4) Uani 1 1 d U . .
H65 H 0.6410 0.0568 0.0159 0.247 Uiso 1 1 calc R . .
C66 C 0.5523(11) 0.0125(5) 0.0647(7) 0.201(4) Uani 1 1 d U . .
C67 C 0.4662(10) -0.0220(4) 0.0514(6) 0.195(3) Uani 1 1 d U . .
H67 H 0.4413 -0.0380 0.0866 0.234 Uiso 1 1 calc R . .
C68 C 0.6008(15) 0.0205(8) 0.1277(10) 0.216(7) Uani 0.50 1 d PU . .
H68A H 0.6639 0.0034 0.1310 0.323 Uiso 0.50 1 calc PR . .
H68B H 0.5688 -0.0034 0.1571 0.323 Uiso 0.50 1 calc PR . .
H68C H 0.6035 0.0669 0.1388 0.323 Uiso 0.50 1 calc PR . .
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
_geom_angle_site_symmetry_3
O2 Al1 O1 115.47(12) . .
O2 Al1 N2 112.38(9) . .
O1 Al1 N2 109.62(12) . .
O2 Al1 N1 116.55(9) . .
O1 Al1 N1 104.49(11) . .
N2 Al1 N1 96.50(8) . .
O2 Al2 O4 127.09(9) . .
O2 Al2 O3 125.44(9) . .
O4 Al2 O3 107.41(9) . .
C2 N1 C6 117.11(18) . .
C2 N1 Al1 119.81(16) . .
C6 N1 Al1 122.35(14) . .
C4 N2 C18 117.27(19) . .
C4 N2 Al1 120.70(16) . .
C18 N2 Al1 121.83(14) . .
Al1 O1 H1 109.5 . .
Al2 O2 Al1 153.80(11) . .
C30 O3 Al2 144.59(15) . .
C45 O4 Al2 145.48(16) . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 C3 123.2(2) . .
N1 C2 C1 120.2(2) . .
C3 C2 C1 116.6(2) . .
C4 C3 C2 127.9(2) . .
C4 C3 H3 116.1 . .
C2 C3 H3 116.1 . .
N2 C4 C3 122.3(2) . .
N2 C4 C5 119.9(2) . .
C3 C4 C5 117.7(2) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C11 C6 C7 121.7(2) . .
C11 C6 N1 120.0(2) . .
C7 C6 N1 118.2(2) . .
C8 C7 C6 117.6(2) . .
C8 C7 C15 120.7(2) . .
C6 C7 C15 121.6(2) . .
C9 C8 C7 121.8(3) . .
C9 C8 H8 119.1 . .
C7 C8 H8 119.1 . .
C8 C9 C10 119.7(3) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C9 C10 C11 121.6(3) . .
C9 C10 H10 119.2 . .
C11 C10 H10 119.2 . .
C10 C11 C6 117.6(2) . .
C10 C11 C12 119.1(2) . .
C6 C11 C12 123.3(2) . .
C11 C12 C13 111.6(2) . .
C11 C12 C14 112.1(2) . .
C13 C12 C14 109.5(2) . .
C11 C12 H12 107.8 . .
C13 C12 H12 107.8 . .
C14 C12 H12 107.8 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C17 C15 C16 113.9(3) . .
C17 C15 C7 113.8(2) . .
C16 C15 C7 114.6(3) . .
C17 C15 C6' 94.2(7) . .
C16 C15 C6' 31.9(6) . .
C7 C15 C6' 104.5(6) . .
C17 C15 H15 114.1 . .
C16 C15 H15 82.8 . .
C7 C15 H15 114.1 . .
C6' C15 H15 114.1 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C6' H6'1 109.5 . .
C15 C6' H6'2 109.5 . .
C15 C6' H6'3 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C19 C18 C23 121.8(2) . .
C19 C18 N2 119.7(2) . .
C23 C18 N2 118.6(2) . .
C20 C19 C18 117.4(3) . .
C20 C19 C27 119.7(2) . .
C18 C19 C27 122.9(2) . .
C21 C20 C19 121.7(3) . .
C21 C20 H20 119.1 . .
C19 C20 H20 119.1 . .
C20 C21 C22 120.3(3) . .
C20 C21 H21 119.8 . .
C22 C21 H21 119.8 . .
C21 C22 C23 120.9(3) . .
C21 C22 H22 119.6 . .
C23 C22 H22 119.6 . .
C22 C23 C18 117.9(3) . .
C22 C23 C24 119.8(3) . .
C18 C23 C24 122.2(2) . .
C25 C24 C26 111.0(3) . .
C25 C24 C23 113.1(2) . .
C26 C24 C23 109.8(2) . .
C25 C24 H24 107.6 . .
C26 C24 H24 107.6 . .
C23 C24 H24 107.6 . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C24 C26 H26A 109.5 . .
C24 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C24 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C29 C27 C19 111.4(2) . .
C29 C27 C28 110.7(3) . .
C19 C27 C28 111.4(3) . .
C29 C27 H27 107.7 . .
C19 C27 H27 107.7 . .
C28 C27 H27 107.7 . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C27 C29 H29A 109.5 . .
C27 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C27 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
O3 C30 C31 119.5(2) . .
O3 C30 C35 119.7(2) . .
C31 C30 C35 120.7(2) . .
C32 C31 C30 117.4(2) . .
C32 C31 C40 119.6(2) . .
C30 C31 C40 123.0(2) . .
C33 C32 C31 122.9(2) . .
C33 C32 H32 118.6 . .
C31 C32 H32 118.6 . .
C34 C33 C32 117.8(2) . .
C34 C33 C44 120.6(2) . .
C32 C33 C44 121.6(2) . .
C33 C34 C35 123.0(2) . .
C33 C34 H34 118.5 . .
C35 C34 H34 118.5 . .
C34 C35 C30 117.2(2) . .
C34 C35 C36 120.0(2) . .
C30 C35 C36 122.7(2) . .
C38 C36 C37 109.8(2) . .
C38 C36 C35 108.9(2) . .
C37 C36 C35 112.7(2) . .
C38 C36 C39 106.6(2) . .
C37 C36 C39 106.5(2) . .
C35 C36 C39 112.1(2) . .
C36 C37 H37A 109.5 . .
C36 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
C36 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
C36 C38 H38A 109.5 . .
C36 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
C36 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
C36 C39 H39A 109.5 . .
C36 C39 H39B 109.5 . .
H39A C39 H39B 109.5 . .
C36 C39 H39C 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
C42 C40 C41 111.0(2) . .
C42 C40 C43 107.8(2) . .
C41 C40 C43 105.6(2) . .
C42 C40 C31 109.2(2) . .
C41 C40 C31 111.4(2) . .
C43 C40 C31 111.9(2) . .
C40 C41 H41A 109.5 . .
C40 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C40 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C40 C42 H42A 109.5 . .
C40 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C40 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C40 C43 H43A 109.5 . .
C40 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
C40 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C33 C44 H44A 109.5 . .
C33 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C33 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
O4 C45 C50 119.2(2) . .
O4 C45 C46 119.5(2) . .
C50 C45 C46 121.2(2) . .
C47 C46 C45 117.5(2) . .
C47 C46 C55 120.1(2) . .
C45 C46 C55 122.3(2) . .
C48 C47 C46 122.6(2) . .
C48 C47 H47 118.7 . .
C46 C47 H47 118.7 . .
C49 C48 C47 118.0(2) . .
C49 C48 C59 120.4(2) . .
C47 C48 C59 121.6(2) . .
C48 C49 C50 122.9(2) . .
C48 C49 H49 118.5 . .
C50 C49 H49 118.5 . .
C49 C50 C45 117.4(2) . .
C49 C50 C51 120.0(2) . .
C45 C50 C51 122.7(2) . .
C53 C51 C50 110.7(3) . .
C53 C51 C54 113.1(3) . .
C50 C51 C54 108.5(2) . .
C53 C51 C52 106.1(3) . .
C50 C51 C52 112.0(2) . .
C54 C51 C52 106.4(3) . .
C51 C52 H52A 109.5 . .
C51 C52 H52B 109.5 . .
H52A C52 H52B 109.5 . .
C51 C52 H52C 109.5 . .
H52A C52 H52C 109.5 . .
H52B C52 H52C 109.5 . .
C51 C53 H53A 109.5 . .
C51 C53 H53B 109.5 . .
H53A C53 H53B 109.5 . .
C51 C53 H53C 109.5 . .
H53A C53 H53C 109.5 . .
H53B C53 H53C 109.5 . .
C51 C54 H54A 109.5 . .
C51 C54 H54B 109.5 . .
H54A C54 H54B 109.5 . .
C51 C54 H54C 109.5 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
C57 C55 C56 107.3(2) . .
C57 C55 C46 112.0(2) . .
C56 C55 C46 108.1(2) . .
C57 C55 C58 107.0(2) . .
C56 C55 C58 109.5(2) . .
C46 C55 C58 112.8(2) . .
C55 C56 H56A 109.5 . .
C55 C56 H56B 109.5 . .
H56A C56 H56B 109.5 . .
C55 C56 H56C 109.5 . .
H56A C56 H56C 109.5 . .
H56B C56 H56C 109.5 . .
C55 C57 H57A 109.5 . .
C55 C57 H57B 109.5 . .
H57A C57 H57B 109.5 . .
C55 C57 H57C 109.5 . .
H57A C57 H57C 109.5 . .
H57B C57 H57C 109.5 . .
C55 C58 H58A 109.5 . .
C55 C58 H58B 109.5 . .
H58A C58 H58B 109.5 . .
C55 C58 H58C 109.5 . .
H58A C58 H58C 109.5 . .
H58B C58 H58C 109.5 . .
C48 C59 H59A 109.5 . .
C48 C59 H59B 109.5 . .
H59A C59 H59B 109.5 . .
C48 C59 H59C 109.5 . .
H59A C59 H59C 109.5 . .
H59B C59 H59C 109.5 . .
C63 C60 C61 106.6(12) 3_667 .
C63 C60 C64 57.8(7) 3_667 3_667
C61 C60 C64 48.9(8) . 3_667
C64 C61 C62 53.0(9) 3_667 .
C64 C61 C60 66.3(11) 3_667 .
C62 C61 C60 119.3(10) . .
C63 C62 C64 62.5(10) . 3_667
C63 C62 C61 116.6(15) . .
C64 C62 C61 54.2(11) 3_667 .
C62 C63 C60 162.2(17) . 3_667
C62 C63 C64 61.2(12) . 3_667
C60 C63 C64 136.2(15) 3_667 3_667
C62 C63 C64 125.3(15) . .
C60 C63 C64 71.8(13) 3_667 .
C64 C63 C64 64.4(9) 3_667 .
C62 C64 C63 56.4(15) 3_667 3_667
C62 C64 C61 72.8(12) 3_667 3_667
C63 C64 C61 129.2(17) 3_667 3_667
C62 C64 C63 170.7(16) 3_667 .
C63 C64 C63 115.6(9) 3_667 .
C61 C64 C63 115.1(16) 3_667 .
C62 C64 C64 118(2) 3_667 3_667
C63 C64 C64 61.5(10) 3_667 3_667
C61 C64 C64 169(2) 3_667 3_667
C63 C64 C64 54.1(10) . 3_667
C62 C64 C60 137.5(16) 3_667 3_667
C63 C64 C60 166.0(15) 3_667 3_667
C61 C64 C60 64.8(11) 3_667 3_667
C63 C64 C60 50.4(12) . 3_667
C64 C64 C60 104(2) 3_667 3_667
C66 C65 C67 121.7(15) . 3_655
C66 C65 H65 119.1 . .
C67 C65 H65 119.1 3_655 .
C65 C66 C68 124(2) . .
C65 C66 C67 114.3(15) . .
C68 C66 C67 121.3(19) . .
C65 C67 C66 124.0(15) 3_655 .
C65 C67 H67 118.0 3_655 .
C66 C67 H67 118.0 . .
C66 C68 H68A 109.5 . .
C66 C68 H68B 109.5 . .
H68A C68 H68B 109.5 . .
C66 C68 H68C 109.5 . .
H68A C68 H68C 109.5 . .
H68B C68 H68C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O2 1.7085(17) .
Al1 O1 1.710(3) .
Al1 N2 1.893(2) .
Al1 N1 1.9048(19) .
Al2 O2 1.6614(17) .
Al2 O4 1.6826(16) .
Al2 O3 1.6918(17) .
N1 C2 1.337(3) .
N1 C6 1.450(3) .
N2 C4 1.342(3) .
N2 C18 1.455(3) .
O1 H1 0.8400 .
O3 C30 1.366(3) .
O4 C45 1.372(3) .
C1 C2 1.504(3) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.403(3) .
C3 C4 1.386(3) .
C3 H3 0.9500 .
C4 C5 1.502(3) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C11 1.401(3) .
C6 C7 1.408(3) .
C7 C8 1.388(4) .
C7 C15 1.510(4) .
C8 C9 1.376(4) .
C8 H8 0.9500 .
C9 C10 1.376(4) .
C9 H9 0.9500 .
C10 C11 1.396(4) .
C10 H10 0.9500 .
C11 C12 1.517(4) .
C12 C13 1.526(4) .
C12 C14 1.535(4) .
C12 H12 1.0000 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C17 1.496(4) .
C15 C16 1.503(5) .
C15 C6' 1.672(15) .
C15 H15 1.0000 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C6' H6'1 0.9800 .
C6' H6'2 0.9800 .
C6' H6'3 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 C19 1.401(4) .
C18 C23 1.401(4) .
C19 C20 1.392(4) .
C19 C27 1.515(4) .
C20 C21 1.367(4) .
C20 H20 0.9500 .
C21 C22 1.375(4) .
C21 H21 0.9500 .
C22 C23 1.394(4) .
C22 H22 0.9500 .
C23 C24 1.525(4) .
C24 C25 1.523(4) .
C24 C26 1.524(4) .
C24 H24 1.0000 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 C29 1.515(4) .
C27 C28 1.534(4) .
C27 H27 1.0000 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C30 C31 1.410(3) .
C30 C35 1.417(3) .
C31 C32 1.392(3) .
C31 C40 1.541(3) .
C32 C33 1.383(3) .
C32 H32 0.9500 .
C33 C34 1.378(4) .
C33 C44 1.505(3) .
C34 C35 1.391(3) .
C34 H34 0.9500 .
C35 C36 1.535(4) .
C36 C38 1.531(4) .
C36 C37 1.531(4) .
C36 C39 1.536(4) .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
C38 H38A 0.9800 .
C38 H38B 0.9800 .
C38 H38C 0.9800 .
C39 H39A 0.9800 .
C39 H39B 0.9800 .
C39 H39C 0.9800 .
C40 C42 1.529(4) .
C40 C41 1.531(3) .
C40 C43 1.537(4) .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
C44 H44A 0.9800 .
C44 H44B 0.9800 .
C44 H44C 0.9800 .
C45 C50 1.406(3) .
C45 C46 1.409(3) .
C46 C47 1.392(3) .
C46 C55 1.537(3) .
C47 C48 1.382(3) .
C47 H47 0.9500 .
C48 C49 1.376(4) .
C48 C59 1.510(4) .
C49 C50 1.393(3) .
C49 H49 0.9500 .
C50 C51 1.535(4) .
C51 C53 1.517(5) .
C51 C54 1.543(5) .
C51 C52 1.546(4) .
C52 H52A 0.9800 .
C52 H52B 0.9800 .
C52 H52C 0.9800 .
C53 H53A 0.9800 .
C53 H53B 0.9800 .
C53 H53C 0.9800 .
C54 H54A 0.9800 .
C54 H54B 0.9800 .
C54 H54C 0.9800 .
C55 C57 1.535(4) .
C55 C56 1.536(4) .
C55 C58 1.540(3) .
C56 H56A 0.9800 .
C56 H56B 0.9800 .
C56 H56C 0.9800 .
C57 H57A 0.9800 .
C57 H57B 0.9800 .
C57 H57C 0.9800 .
C58 H58A 0.9800 .
C58 H58B 0.9800 .
C58 H58C 0.9800 .
C59 H59A 0.9800 .
C59 H59B 0.9800 .
C59 H59C 0.9800 .
C60 C63 1.302(19) 3_667
C60 C61 1.59(2) .
C60 C64 1.61(2) 3_667
C61 C64 1.321(12) 3_667
C61 C62 1.56(2) .
C62 C63 1.24(2) .
C62 C64 1.30(2) 3_667
C63 C60 1.302(19) 3_667
C63 C64 1.318(16) 3_667
C63 C64 1.431(16) .
C64 C62 1.30(2) 3_667
C64 C63 1.318(15) 3_667
C64 C61 1.321(12) 3_667
C64 C64 1.47(2) 3_667
C64 C60 1.61(2) 3_667
C65 C66 1.384(16) .
C65 C67 1.410(13) 3_655
C65 H65 0.9500 .
C66 C68 1.40(2) .
C66 C67 1.430(15) .
C67 C65 1.410(13) 3_655
C67 H67 0.9500 .
C68 H68A 0.9800 .
C68 H68B 0.9800 .
C68 H68C 0.9800 .
