# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
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#  except for the purpose of generating routine backup copies 
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data_2
_database_code_depnum_ccdc_archive 'CCDC 874034'
#TrackingRef 'XRAY.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H45 Al N10 O2'
_chemical_formula_weight         700.82
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'
Al Al 0.0645 0.0514 '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'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.3249(13)
_cell_length_b                   12.5257(15)
_cell_length_c                   14.309(2)
_cell_angle_alpha                76.246(4)
_cell_angle_beta                 85.353(5)
_cell_angle_gamma                74.044(4)
_cell_volume                     1895.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    1016
_cell_measurement_theta_min      2.357
_cell_measurement_theta_max      18.596
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6789
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15785
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_sigmaI/netI    0.1476
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6588
_reflns_number_gt                2864
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6588
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1710
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1621
_refine_ls_wR_factor_gt          0.1206
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_restrained_S_all      0.930
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
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 0.21518(10) 0.38590(9) 0.73671(9) 0.0383(3) Uani 1 1 d . . .
O1 O 0.2922(2) 0.24468(19) 0.72390(18) 0.0385(7) Uani 1 1 d . . .
O2 O 0.3191(2) 0.44231(19) 0.78292(18) 0.0387(7) Uani 1 1 d . . .
N1 N 0.2832(3) 0.4435(2) 0.5993(2) 0.0354(8) Uani 1 1 d . . .
N2 N 0.3411(3) 0.5304(2) 0.5771(2) 0.0356(8) Uani 1 1 d . . .
N3 N 0.2069(3) 0.6960(3) 0.6735(3) 0.0532(10) Uani 1 1 d . . .
N4 N 0.3323(3) 0.6703(3) 0.6657(2) 0.0424(9) Uani 1 1 d . . .
N5 N 0.5256(3) 0.4380(3) 0.7782(2) 0.0405(9) Uani 1 1 d . . .
N6 N 0.1804(3) 0.3135(3) 0.8836(3) 0.0430(9) Uani 1 1 d . . .
N7 N 0.1743(3) 0.2023(3) 0.9119(3) 0.0423(9) Uani 1 1 d . . .
N8 N 0.0688(3) 0.1720(3) 0.7868(3) 0.0448(9) Uani 1 1 d . . .
N9 N 0.0831(3) 0.1546(3) 0.6952(3) 0.0517(10) Uani 1 1 d . . .
N10 N 0.3741(3) 0.0494(3) 0.7801(2) 0.0424(9) Uani 1 1 d . . .
C1 C 0.3425(3) 0.5753(3) 0.4811(3) 0.0389(10) Uani 1 1 d . . .
C2 C 0.2844(3) 0.5164(3) 0.4398(3) 0.0434(11) Uani 1 1 d . . .
H2 H 0.2710 0.5276 0.3745 0.052 Uiso 1 1 calc R . .
C3 C 0.2492(3) 0.4362(3) 0.5140(3) 0.0404(10) Uani 1 1 d . . .
C4 C 0.3966(3) 0.6725(3) 0.4400(3) 0.0489(12) Uani 1 1 d . . .
H4A H 0.3460 0.7400 0.4577 0.073 Uiso 1 1 calc R . .
H4B H 0.4010 0.6843 0.3711 0.073 Uiso 1 1 calc R . .
H4C H 0.4776 0.6557 0.4645 0.073 Uiso 1 1 calc R . .
C5 C 0.1824(4) 0.3509(3) 0.5065(3) 0.0553(12) Uani 1 1 d . . .
H5A H 0.2074 0.2843 0.5574 0.083 Uiso 1 1 calc R . .
H5B H 0.2015 0.3302 0.4455 0.083 Uiso 1 1 calc R . .
H5C H 0.0955 0.3835 0.5117 0.083 Uiso 1 1 calc R . .
C6 C 0.3788(4) 0.7529(3) 0.6835(3) 0.0461(11) Uani 1 1 d . . .
C7 C 0.2796(5) 0.8358(4) 0.7020(3) 0.0614(13) Uani 1 1 d . . .
H7 H 0.2804 0.9043 0.7162 0.074 Uiso 1 1 calc R . .
C8 C 0.1765(4) 0.7976(4) 0.6956(3) 0.0604(13) Uani 1 1 d . . .
C9 C 0.5132(4) 0.7416(4) 0.6816(4) 0.0677(14) Uani 1 1 d . . .
H9A H 0.5522 0.6761 0.7295 0.102 Uiso 1 1 calc R . .
H9B H 0.5273 0.8087 0.6949 0.102 Uiso 1 1 calc R . .
H9C H 0.5467 0.7329 0.6193 0.102 Uiso 1 1 calc R . .
C10 C 0.0443(4) 0.8540(4) 0.7098(4) 0.103(2) Uani 1 1 d . . .
H10A H 0.0210 0.9247 0.6630 0.155 Uiso 1 1 calc R . .
H10B H 0.0315 0.8685 0.7733 0.155 Uiso 1 1 calc R . .
H10C H -0.0047 0.8051 0.7024 0.155 Uiso 1 1 calc R . .
C11 C 0.4001(3) 0.5600(3) 0.6495(3) 0.0372(10) Uani 1 1 d . . .
H11 H 0.4815 0.5663 0.6242 0.045 Uiso 1 1 calc R . .
C12 C 0.4186(4) 0.4704(3) 0.7436(3) 0.0380(10) Uani 1 1 d . . .
C13 C 0.5422(3) 0.3589(3) 0.8690(3) 0.0415(11) Uani 1 1 d . . .
C14 C 0.5826(4) 0.3894(4) 0.9442(3) 0.0508(12) Uani 1 1 d . . .
H14 H 0.5970 0.4608 0.9353 0.061 Uiso 1 1 calc R . .
C15 C 0.6019(4) 0.3151(4) 1.0323(4) 0.0649(14) Uani 1 1 d . . .
H15 H 0.6278 0.3371 1.0831 0.078 Uiso 1 1 calc R . .
C16 C 0.5834(4) 0.2094(4) 1.0461(4) 0.0650(14) Uani 1 1 d . . .
H16 H 0.5965 0.1596 1.1062 0.078 Uiso 1 1 calc R . .
C17 C 0.5458(4) 0.1767(4) 0.9723(4) 0.0655(14) Uani 1 1 d . . .
H17 H 0.5336 0.1044 0.9816 0.079 Uiso 1 1 calc R . .
C18 C 0.5254(4) 0.2514(3) 0.8826(3) 0.0532(12) Uani 1 1 d . . .
H18 H 0.5004 0.2288 0.8317 0.064 Uiso 1 1 calc R . .
C19 C 0.1696(4) 0.1683(4) 1.0093(3) 0.0508(12) Uani 1 1 d . . .
C20 C 0.1705(4) 0.2603(4) 1.0443(3) 0.0604(13) Uani 1 1 d . . .
H20 H 0.1671 0.2634 1.1088 0.073 Uiso 1 1 calc R . .
C21 C 0.1774(4) 0.3490(4) 0.9654(4) 0.0532(12) Uani 1 1 d . . .
C22 C 0.1624(4) 0.0515(4) 1.0599(3) 0.0690(14) Uani 1 1 d . . .
H22A H 0.0907 0.0369 1.0396 0.103 Uiso 1 1 calc R . .
H22B H 0.1575 0.0458 1.1281 0.103 Uiso 1 1 calc R . .
H22C H 0.2344 -0.0035 1.0445 0.103 Uiso 1 1 calc R . .
C23 C 0.1836(4) 0.4670(4) 0.9656(3) 0.0766(16) Uani 1 1 d . . .
H23A H 0.2679 0.4679 0.9673 0.115 Uiso 1 1 calc R . .
H23B H 0.1403 0.4898 1.0211 0.115 Uiso 1 1 calc R . .
H23C H 0.1466 0.5189 0.9083 0.115 Uiso 1 1 calc R . .
C24 C -0.0310(4) 0.1794(4) 0.6643(4) 0.0584(14) Uani 1 1 d . . .
C25 C -0.1162(4) 0.2088(4) 0.7353(4) 0.0657(15) Uani 1 1 d . . .
H25 H -0.2013 0.2286 0.7306 0.079 Uiso 1 1 calc R . .
C26 C -0.0515(4) 0.2032(3) 0.8132(4) 0.0516(12) Uani 1 1 d . . .
C27 C -0.0503(4) 0.1733(4) 0.5632(4) 0.0830(17) Uani 1 1 d . . .
H27A H 0.0275 0.1436 0.5341 0.124 Uiso 1 1 calc R . .
H27B H -0.0882 0.2483 0.5265 0.124 Uiso 1 1 calc R . .
H27C H -0.1025 0.1242 0.5644 0.124 Uiso 1 1 calc R . .
C28 C -0.0979(4) 0.2301(4) 0.9076(4) 0.0726(16) Uani 1 1 d . . .
H28A H -0.1860 0.2480 0.9095 0.109 Uiso 1 1 calc R . .
H28B H -0.0722 0.2943 0.9156 0.109 Uiso 1 1 calc R . .
H28C H -0.0655 0.1654 0.9585 0.109 Uiso 1 1 calc R . .
C29 C 0.1804(3) 0.1354(3) 0.8420(3) 0.0407(11) Uani 1 1 d . . .
H29 H 0.1908 0.0557 0.8761 0.049 Uiso 1 1 calc R . .
C30 C 0.2911(4) 0.1424(3) 0.7756(3) 0.0364(10) Uani 1 1 d . . .
C31 C 0.4800(4) 0.0426(3) 0.7201(3) 0.0429(11) Uani 1 1 d . . .
C32 C 0.5923(4) -0.0145(4) 0.7604(4) 0.0656(14) Uani 1 1 d . . .
H32 H 0.5992 -0.0393 0.8269 0.079 Uiso 1 1 calc R . .
C33 C 0.6939(4) -0.0346(5) 0.7020(5) 0.0882(18) Uani 1 1 d . . .
H33 H 0.7694 -0.0734 0.7302 0.106 Uiso 1 1 calc R . .
C34 C 0.6894(5) -0.0005(4) 0.6049(4) 0.0680(15) Uani 1 1 d . . .
H34 H 0.7601 -0.0150 0.5670 0.082 Uiso 1 1 calc R . .
C35 C 0.5784(5) 0.0557(4) 0.5646(4) 0.0659(14) Uani 1 1 d . . .
H35 H 0.5724 0.0791 0.4980 0.079 Uiso 1 1 calc R . .
C36 C 0.4740(4) 0.0784(3) 0.6222(4) 0.0542(12) Uani 1 1 d . . .
H36 H 0.3989 0.1185 0.5937 0.065 Uiso 1 1 calc R . .
C37 C 0.0456(3) 0.4666(3) 0.7026(3) 0.0520(12) Uani 1 1 d . . .
H37A H 0.0478 0.5213 0.6423 0.062 Uiso 1 1 calc R . .
H37B H 0.0069 0.4114 0.6899 0.062 Uiso 1 1 calc R . .
C38 C -0.0387(4) 0.5295(4) 0.7704(4) 0.0949(19) Uani 1 1 d . . .
H38A H -0.0380 0.4794 0.8327 0.142 Uiso 1 1 calc R . .
H38B H -0.1207 0.5555 0.7461 0.142 Uiso 1 1 calc R . .
H38C H -0.0110 0.5937 0.7756 0.142 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Al1 0.0360(7) 0.0338(7) 0.0450(9) -0.0090(6) 0.0015(6) -0.0095(6)
O1 0.0402(15) 0.0285(15) 0.0434(19) -0.0060(13) 0.0046(13) -0.0065(12)
O2 0.0388(16) 0.0385(16) 0.0402(18) -0.0075(13) 0.0028(14) -0.0147(13)
N1 0.0380(19) 0.0321(18) 0.039(2) -0.0074(16) -0.0006(17) -0.0137(15)
N2 0.0395(19) 0.0334(19) 0.037(2) -0.0087(17) -0.0053(17) -0.0128(16)
N3 0.043(2) 0.039(2) 0.074(3) -0.014(2) 0.005(2) -0.0062(17)
N4 0.044(2) 0.030(2) 0.053(3) -0.0101(17) 0.0026(18) -0.0091(17)
N5 0.037(2) 0.038(2) 0.043(2) -0.0014(18) -0.0041(18) -0.0094(16)
N6 0.046(2) 0.041(2) 0.046(3) -0.0121(19) 0.0082(18) -0.0185(17)
N7 0.042(2) 0.041(2) 0.043(3) -0.0057(19) 0.0028(18) -0.0146(17)
N8 0.035(2) 0.046(2) 0.055(3) -0.011(2) -0.003(2) -0.0121(17)
N9 0.052(3) 0.054(2) 0.054(3) -0.015(2) -0.007(2) -0.0182(19)
N10 0.038(2) 0.034(2) 0.050(3) -0.0070(18) 0.0015(18) -0.0042(17)
C1 0.041(2) 0.035(2) 0.034(3) 0.000(2) 0.000(2) -0.006(2)
C2 0.051(3) 0.042(3) 0.035(3) -0.008(2) -0.004(2) -0.008(2)
C3 0.044(3) 0.042(3) 0.036(3) -0.006(2) -0.004(2) -0.013(2)
C4 0.053(3) 0.042(3) 0.047(3) -0.004(2) 0.000(2) -0.009(2)
C5 0.068(3) 0.053(3) 0.050(3) -0.011(2) -0.007(2) -0.024(2)
C6 0.059(3) 0.035(3) 0.046(3) -0.007(2) 0.001(2) -0.018(2)
C7 0.087(4) 0.037(3) 0.061(4) -0.016(2) 0.001(3) -0.014(3)
C8 0.069(3) 0.036(3) 0.070(4) -0.014(3) 0.007(3) -0.004(3)
C9 0.068(3) 0.061(3) 0.086(4) -0.023(3) -0.005(3) -0.029(3)
C10 0.069(4) 0.068(4) 0.164(7) -0.045(4) 0.028(4) 0.003(3)
C11 0.035(2) 0.033(2) 0.044(3) -0.011(2) 0.003(2) -0.0078(19)
C12 0.045(3) 0.030(2) 0.039(3) -0.006(2) 0.001(2) -0.013(2)
C13 0.037(2) 0.041(3) 0.042(3) -0.006(2) -0.001(2) -0.006(2)
C14 0.057(3) 0.047(3) 0.042(3) -0.002(3) -0.007(2) -0.009(2)
C15 0.074(4) 0.066(4) 0.049(4) -0.015(3) -0.006(3) -0.006(3)
C16 0.069(3) 0.058(3) 0.050(4) 0.006(3) 0.000(3) -0.003(3)
C17 0.069(3) 0.046(3) 0.075(4) 0.002(3) -0.006(3) -0.018(3)
C18 0.061(3) 0.043(3) 0.050(3) -0.001(3) -0.011(2) -0.010(2)
C19 0.055(3) 0.059(3) 0.038(3) -0.008(3) 0.003(2) -0.018(2)
C20 0.075(3) 0.077(4) 0.034(3) -0.010(3) 0.002(3) -0.031(3)
C21 0.058(3) 0.063(3) 0.052(3) -0.027(3) 0.014(3) -0.029(2)
C22 0.089(4) 0.060(3) 0.048(3) 0.002(3) 0.008(3) -0.017(3)
C23 0.100(4) 0.082(4) 0.071(4) -0.042(3) 0.032(3) -0.052(3)
C24 0.043(3) 0.060(3) 0.077(4) -0.011(3) -0.013(3) -0.022(2)
C25 0.041(3) 0.072(3) 0.084(4) -0.005(3) -0.009(3) -0.022(3)
C26 0.040(3) 0.048(3) 0.067(4) -0.012(3) 0.008(3) -0.015(2)
C27 0.077(4) 0.101(4) 0.080(5) -0.021(4) -0.025(3) -0.032(3)
C28 0.044(3) 0.078(4) 0.095(5) -0.024(3) 0.015(3) -0.014(3)
C29 0.041(3) 0.034(2) 0.047(3) -0.005(2) -0.001(2) -0.011(2)
C30 0.040(2) 0.039(3) 0.033(3) -0.007(2) -0.004(2) -0.016(2)
C31 0.044(3) 0.035(2) 0.051(3) -0.013(2) 0.005(2) -0.011(2)
C32 0.042(3) 0.093(4) 0.058(4) -0.022(3) -0.010(3) -0.005(3)
C33 0.036(3) 0.137(5) 0.096(5) -0.053(4) 0.001(3) -0.009(3)
C34 0.054(4) 0.077(4) 0.081(5) -0.034(3) 0.017(3) -0.022(3)
C35 0.078(4) 0.051(3) 0.067(4) -0.013(3) 0.014(3) -0.018(3)
C36 0.053(3) 0.047(3) 0.053(4) -0.004(3) 0.006(3) -0.005(2)
C37 0.042(3) 0.048(3) 0.062(3) -0.008(2) 0.000(2) -0.011(2)
C38 0.066(4) 0.107(5) 0.088(5) -0.029(4) 0.015(3) 0.018(3)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O2 1.769(3) . ?
Al1 O1 1.790(3) . ?
Al1 C37 1.949(4) . ?
Al1 N1 2.090(3) . ?
Al1 N6 2.133(4) . ?
O1 C30 1.321(4) . ?
O2 C12 1.315(4) . ?
N1 C3 1.339(5) . ?
N1 N2 1.382(3) . ?
N2 C1 1.355(5) . ?
N2 C11 1.445(4) . ?
N3 C8 1.330(5) . ?
N3 N4 1.368(4) . ?
N4 C6 1.364(4) . ?
N4 C11 1.447(4) . ?
N5 C12 1.269(4) . ?
N5 C13 1.424(5) . ?
N6 C21 1.342(5) . ?
N6 N7 1.374(4) . ?
N7 C19 1.357(5) . ?
N7 C29 1.437(5) . ?
N8 C26 1.358(5) . ?
N8 N9 1.369(4) . ?
N8 C29 1.450(5) . ?
N9 C24 1.330(5) . ?
N10 C30 1.272(4) . ?
N10 C31 1.412(5) . ?
C1 C2 1.366(5) . ?
C1 C4 1.487(5) . ?
C2 C3 1.394(5) . ?
C3 C5 1.496(5) . ?
C6 C7 1.361(5) . ?
C6 C9 1.487(5) . ?
C7 C8 1.396(6) . ?
C8 C10 1.489(6) . ?
C11 C12 1.521(5) . ?
C13 C14 1.372(5) . ?
C13 C18 1.378(5) . ?
C14 C15 1.371(6) . ?
C15 C16 1.364(6) . ?
C16 C17 1.356(6) . ?
C17 C18 1.391(6) . ?
C19 C20 1.365(6) . ?
C19 C22 1.492(5) . ?
C20 C21 1.397(6) . ?
C21 C23 1.500(5) . ?
C24 C25 1.387(6) . ?
C24 C27 1.503(6) . ?
C25 C26 1.361(6) . ?
C26 C28 1.490(6) . ?
C29 C30 1.520(5) . ?
C31 C36 1.368(5) . ?
C31 C32 1.372(5) . ?
C32 C33 1.368(6) . ?
C33 C34 1.353(7) . ?
C34 C35 1.359(6) . ?
C35 C36 1.388(5) . ?
C37 C38 1.508(6) . ?
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
O2 Al1 O1 108.92(13) . . ?
O2 Al1 C37 125.23(16) . . ?
O1 Al1 C37 125.84(16) . . ?
O2 Al1 N1 87.88(12) . . ?
O1 Al1 N1 86.94(12) . . ?
C37 Al1 N1 93.36(16) . . ?
O2 Al1 N6 85.35(12) . . ?
O1 Al1 N6 87.62(13) . . ?
C37 Al1 N6 97.15(16) . . ?
N1 Al1 N6 169.46(13) . . ?
C30 O1 Al1 133.1(3) . . ?
C12 O2 Al1 130.2(3) . . ?
C3 N1 N2 104.4(3) . . ?
C3 N1 Al1 128.9(2) . . ?
N2 N1 Al1 123.4(2) . . ?
C1 N2 N1 111.7(3) . . ?
C1 N2 C11 126.2(3) . . ?
N1 N2 C11 121.9(3) . . ?
C8 N3 N4 103.5(3) . . ?
C6 N4 N3 112.8(3) . . ?
C6 N4 C11 127.5(3) . . ?
N3 N4 C11 119.5(3) . . ?
C12 N5 C13 116.8(3) . . ?
C21 N6 N7 105.4(3) . . ?
C21 N6 Al1 133.2(3) . . ?
N7 N6 Al1 120.8(3) . . ?
C19 N7 N6 111.3(3) . . ?
C19 N7 C29 127.9(3) . . ?
N6 N7 C29 120.6(3) . . ?
C26 N8 N9 111.9(4) . . ?
C26 N8 C29 131.7(4) . . ?
N9 N8 C29 115.3(3) . . ?
C24 N9 N8 104.3(4) . . ?
C30 N10 C31 121.7(3) . . ?
N2 C1 C2 106.2(3) . . ?
N2 C1 C4 121.6(4) . . ?
C2 C1 C4 132.1(4) . . ?
C1 C2 C3 106.9(4) . . ?
N1 C3 C2 110.7(3) . . ?
N1 C3 C5 121.4(3) . . ?
C2 C3 C5 127.9(4) . . ?
C7 C6 N4 105.5(4) . . ?
C7 C6 C9 132.4(4) . . ?
N4 C6 C9 122.0(4) . . ?
C6 C7 C8 106.4(4) . . ?
N3 C8 C7 111.8(4) . . ?
N3 C8 C10 119.0(4) . . ?
C7 C8 C10 129.2(4) . . ?
N2 C11 N4 110.3(3) . . ?
N2 C11 C12 113.3(3) . . ?
N4 C11 C12 110.9(3) . . ?
N5 C12 O2 127.8(4) . . ?
N5 C12 C11 116.4(3) . . ?
O2 C12 C11 115.6(3) . . ?
C14 C13 C18 119.1(4) . . ?
C14 C13 N5 118.4(4) . . ?
C18 C13 N5 122.4(4) . . ?
C15 C14 C13 120.3(4) . . ?
C16 C15 C14 120.6(5) . . ?
C17 C16 C15 120.1(5) . . ?
C16 C17 C18 120.0(4) . . ?
C13 C18 C17 120.0(4) . . ?
N7 C19 C20 106.3(4) . . ?
N7 C19 C22 122.8(4) . . ?
C20 C19 C22 130.9(4) . . ?
C19 C20 C21 107.3(4) . . ?
N6 C21 C20 109.7(4) . . ?
N6 C21 C23 122.1(4) . . ?
C20 C21 C23 128.2(4) . . ?
N9 C24 C25 111.1(5) . . ?
N9 C24 C27 119.0(5) . . ?
C25 C24 C27 129.9(4) . . ?
C26 C25 C24 106.8(4) . . ?
N8 C26 C25 105.8(4) . . ?
N8 C26 C28 125.2(4) . . ?
C25 C26 C28 128.9(4) . . ?
N7 C29 N8 111.6(3) . . ?
N7 C29 C30 109.7(3) . . ?
N8 C29 C30 110.4(3) . . ?
N10 C30 O1 127.9(3) . . ?
N10 C30 C29 115.6(3) . . ?
O1 C30 C29 116.4(3) . . ?
C36 C31 C32 118.4(4) . . ?
C36 C31 N10 122.5(4) . . ?
C32 C31 N10 118.6(4) . . ?
C33 C32 C31 119.4(5) . . ?
C34 C33 C32 122.9(5) . . ?
C33 C34 C35 117.9(5) . . ?
C34 C35 C36 120.4(5) . . ?
C31 C36 C35 120.9(4) . . ?
C38 C37 Al1 120.8(3) . . ?
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.054


data_6
_database_code_depnum_ccdc_archive 'CCDC 907283'
#TrackingRef 'XRAY.CIF'
# start Validation Reply Form
_vrf_PLAT035_6                   
;
PROBLEM: No _chemical_absolute_configuration info given
RESPONSE: The crystal diffracted weakly and the anomalous
dispersion effect is small. Flack's parameter did not
used for absolute structure determination.
;
# end Validation Reply Form
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H53 Al N10 O2'
_chemical_formula_sum            'C42 H53 Al N10 O2'
_chemical_formula_weight         756.92
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'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
_cell_length_a                   12.3440(4)
_cell_length_b                   14.5660(6)
_cell_length_c                   23.8390(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4286.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    647
_cell_measurement_theta_min      2.756
_cell_measurement_theta_max      16.937
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9787
_exptl_absorpt_correction_T_max  0.9833
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      230(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18884
_diffrn_reflns_av_R_equivalents  0.1147
_diffrn_reflns_av_sigmaI/netI    0.1801
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7408
_reflns_number_gt                2921
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0071(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(5)
_refine_ls_number_reflns         7408
_refine_ls_number_parameters     528
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2126
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.2306
_refine_ls_wR_factor_gt          0.1560
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_restrained_S_all      0.940
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
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 0.07478(16) 0.51455(16) 0.34271(9) 0.0553(7) Uani 1 1 d . . .
O1 O 0.1541(3) 0.5801(3) 0.39046(18) 0.0534(13) Uani 1 1 d . A .
O2 O -0.0146(3) 0.4388(3) 0.37918(19) 0.0525(13) Uani 1 1 d . A .
N1 N 0.1917(5) 0.4087(5) 0.3506(3) 0.0581(17) Uani 1 1 d . A .
N2 N 0.2953(5) 0.4218(5) 0.3703(2) 0.0568(17) Uani 1 1 d . . .
N3 N 0.3857(6) 0.5150(6) 0.2878(3) 0.081(2) Uani 1 1 d . A .
N4 N 0.3640(5) 0.5626(5) 0.3353(3) 0.0638(18) Uani 1 1 d . . .
N5 N 0.2565(4) 0.5711(4) 0.4714(3) 0.0501(15) Uani 1 1 d . A .
N6 N -0.0444(4) 0.6176(5) 0.3509(2) 0.0571(17) Uani 1 1 d . A .
N7 N -0.1526(4) 0.6000(4) 0.3579(2) 0.0503(16) Uani 1 1 d . . .
N8 N -0.2098(5) 0.5146(5) 0.2651(3) 0.076(2) Uani 1 1 d . A .
N9 N -0.2079(5) 0.4639(5) 0.3127(3) 0.0575(18) Uani 1 1 d . . .
N10 N -0.1374(4) 0.4375(4) 0.4526(3) 0.0505(16) Uani 1 1 d . A .
C1 C 0.3573(7) 0.3468(7) 0.3626(3) 0.071(2) Uani 1 1 d . A .
C2 C 0.2907(7) 0.2821(6) 0.3406(4) 0.076(3) Uani 1 1 d . . .
H2 H 0.3096 0.2219 0.3321 0.091 Uiso 1 1 calc R A .
C3 C 0.1893(7) 0.3216(6) 0.3329(3) 0.066(2) Uani 1 1 d . A .
C4 C 0.4756(6) 0.3444(6) 0.3754(4) 0.094(3) Uani 1 1 d . . .
H4A H 0.5135 0.3844 0.3502 0.142 Uiso 1 1 calc R A .
H4B H 0.5022 0.2829 0.3711 0.142 Uiso 1 1 calc R . .
H4C H 0.4873 0.3644 0.4133 0.142 Uiso 1 1 calc R . .
C5 C 0.0900(7) 0.2777(6) 0.3111(3) 0.085(3) Uani 1 1 d . . .
H5A H 0.0578 0.2408 0.3400 0.127 Uiso 1 1 calc R A .
H5B H 0.1080 0.2396 0.2796 0.127 Uiso 1 1 calc R . .
H5C H 0.0397 0.3242 0.2995 0.127 Uiso 1 1 calc R . .
C6 C 0.3872(6) 0.6535(7) 0.3304(4) 0.066(2) Uani 1 1 d . A .
C7 C 0.4230(7) 0.6639(8) 0.2767(4) 0.084(3) Uani 1 1 d . . .
H7 H 0.4437 0.7187 0.2597 0.100 Uiso 1 1 calc R A .
C8 C 0.4228(8) 0.5795(9) 0.2527(4) 0.092(3) Uani 1 1 d . A .
C9 C 0.3753(7) 0.7226(6) 0.3752(3) 0.081(3) Uani 1 1 d . . .
H9A H 0.3000 0.7301 0.3840 0.122 Uiso 1 1 calc R A .
H9B H 0.4046 0.7801 0.3627 0.122 Uiso 1 1 calc R . .
H9C H 0.4137 0.7025 0.4080 0.122 Uiso 1 1 calc R . .
C10 C 0.4527(10) 0.5499(9) 0.1957(4) 0.161(5) Uani 1 1 d . . .
H10A H 0.4298 0.4876 0.1899 0.241 Uiso 1 1 calc R A .
H10B H 0.5298 0.5540 0.1912 0.241 Uiso 1 1 calc R . .
H10C H 0.4178 0.5890 0.1687 0.241 Uiso 1 1 calc R . .
C11 C 0.3314(6) 0.5117(6) 0.3854(3) 0.059(2) Uani 1 1 d . A .
H11 H 0.3946 0.5055 0.4100 0.070 Uiso 1 1 calc R . .
C12 C 0.2402(5) 0.5581(5) 0.4188(3) 0.0498(19) Uani 1 1 d . . .
C13 C 0.1631(6) 0.6060(5) 0.5028(3) 0.056(2) Uani 1 1 d . . .
H13 H 0.0965 0.5792 0.4876 0.067 Uiso 1 1 calc R A .
C14 C 0.1752(7) 0.5780(6) 0.5642(3) 0.084(3) Uani 1 1 d . A .
H14A H 0.1846 0.5127 0.5666 0.126 Uiso 1 1 calc R . .
H14B H 0.1114 0.5955 0.5846 0.126 Uiso 1 1 calc R . .
H14C H 0.2372 0.6081 0.5801 0.126 Uiso 1 1 calc R . .
C15 C 0.1571(6) 0.7112(5) 0.4984(3) 0.053(2) Uani 1 1 d . A .
C16 C 0.2454(7) 0.7656(6) 0.5049(3) 0.068(2) Uani 1 1 d . . .
H16 H 0.3124 0.7385 0.5117 0.082 Uiso 1 1 calc R A .
C17 C 0.2388(9) 0.8605(7) 0.5015(3) 0.080(3) Uani 1 1 d . A .
H17 H 0.3008 0.8959 0.5060 0.096 Uiso 1 1 calc R . .
C18 C 0.1415(10) 0.9021(7) 0.4918(4) 0.095(3) Uani 1 1 d . . .
H18 H 0.1362 0.9657 0.4903 0.114 Uiso 1 1 calc R A .
C19 C 0.0532(9) 0.8490(8) 0.4842(4) 0.105(3) Uani 1 1 d . A .
H19 H -0.0130 0.8765 0.4763 0.126 Uiso 1 1 calc R . .
C20 C 0.0591(7) 0.7532(6) 0.4881(3) 0.070(2) Uani 1 1 d . . .
H20 H -0.0031 0.7179 0.4837 0.084 Uiso 1 1 calc R A .
C21 C -0.2147(6) 0.6767(6) 0.3504(3) 0.058(2) Uani 1 1 d . A .
C22 C -0.1434(7) 0.7464(6) 0.3410(3) 0.064(2) Uani 1 1 d . . .
H22 H -0.1607 0.8079 0.3353 0.076 Uiso 1 1 calc R A .
C23 C -0.0391(6) 0.7081(7) 0.3417(3) 0.067(2) Uani 1 1 d . A .
C24 C -0.3350(6) 0.6743(6) 0.3516(3) 0.075(2) Uani 1 1 d . . .
H24A H -0.3606 0.6301 0.3248 0.112 Uiso 1 1 calc R A .
H24B H -0.3629 0.7339 0.3422 0.112 Uiso 1 1 calc R . .
H24C H -0.3592 0.6573 0.3884 0.112 Uiso 1 1 calc R . .
C25 C 0.0654(7) 0.7572(6) 0.3324(4) 0.097(3) Uani 1 1 d . . .
H25A H 0.0929 0.7790 0.3676 0.145 Uiso 1 1 calc R A .
H25B H 0.0538 0.8083 0.3076 0.145 Uiso 1 1 calc R . .
H25C H 0.1170 0.7159 0.3158 0.145 Uiso 1 1 calc R . .
C26 C -0.2314(6) 0.3737(6) 0.3024(4) 0.061(2) Uani 1 1 d . A .
C27 C -0.2499(7) 0.3687(7) 0.2466(4) 0.080(3) Uani 1 1 d . . .
H27 H -0.2698 0.3165 0.2266 0.095 Uiso 1 1 calc R A .
C28 C -0.2334(8) 0.4565(8) 0.2248(4) 0.087(3) Uani 1 1 d . A .
C29 C -0.2350(6) 0.3010(6) 0.3464(4) 0.082(3) Uani 1 1 d . . .
H29A H -0.2756 0.2494 0.3327 0.123 Uiso 1 1 calc R A .
H29B H -0.2693 0.3249 0.3795 0.123 Uiso 1 1 calc R . .
H29C H -0.1626 0.2819 0.3553 0.123 Uiso 1 1 calc R . .
C30 C -0.2366(9) 0.4903(7) 0.1660(3) 0.134(4) Uani 1 1 d . . .
H30A H -0.2566 0.5539 0.1657 0.200 Uiso 1 1 calc R A .
H30B H -0.2888 0.4555 0.1451 0.200 Uiso 1 1 calc R . .
H30C H -0.1664 0.4832 0.1492 0.200 Uiso 1 1 calc R . .
C31 C -0.1904(6) 0.5063(5) 0.3664(3) 0.056(2) Uani 1 1 d . A .
H31 H -0.2597 0.5085 0.3864 0.067 Uiso 1 1 calc R . .
C32 C -0.1091(5) 0.4571(5) 0.4030(3) 0.0486(19) Uani 1 1 d . . .
C33 C -0.0554(6) 0.3930(5) 0.4897(3) 0.058(2) Uani 1 1 d . . .
H33 H 0.0167 0.4153 0.4792 0.069 Uiso 1 1 calc R A .
C34 C -0.0776(8) 0.4206(6) 0.5497(3) 0.090(3) Uani 1 1 d . A .
H34A H -0.1446 0.3937 0.5619 0.136 Uiso 1 1 calc R . .
H34B H -0.0825 0.4862 0.5521 0.136 Uiso 1 1 calc R . .
H34C H -0.0197 0.3994 0.5733 0.136 Uiso 1 1 calc R . .
C35 C -0.0594(7) 0.2917(6) 0.4803(3) 0.058(2) Uani 1 1 d . A .
C36 C 0.0292(8) 0.2438(6) 0.4619(4) 0.082(3) Uani 1 1 d . . .
H36 H 0.0941 0.2747 0.4560 0.099 Uiso 1 1 calc R A .
C37 C 0.0240(11) 0.1500(9) 0.4518(5) 0.120(4) Uani 1 1 d . A .
H37 H 0.0838 0.1186 0.4379 0.144 Uiso 1 1 calc R . .
C38 C -0.0704(13) 0.1050(7) 0.4628(5) 0.116(4) Uani 1 1 d . . .
H38 H -0.0740 0.0420 0.4566 0.139 Uiso 1 1 calc R A .
C39 C -0.1597(10) 0.1495(8) 0.4825(4) 0.102(3) Uani 1 1 d . A .
H39 H -0.2232 0.1177 0.4905 0.122 Uiso 1 1 calc R . .
C40 C -0.1531(8) 0.2426(7) 0.4902(3) 0.076(3) Uani 1 1 d . . .
H40 H -0.2142 0.2739 0.5027 0.091 Uiso 1 1 calc R A .
C41 C 0.072(2) 0.499(2) 0.2631(13) 0.070(8) Uani 0.50 1 d P A 1
H41A H 0.1299 0.4571 0.2537 0.084 Uiso 0.50 1 calc PR A 1
H41B H 0.0045 0.4674 0.2544 0.084 Uiso 0.50 1 calc PR A 1
C42 C 0.080(3) 0.578(2) 0.2237(11) 0.082(18) Uani 0.50 1 d P A 1
H42A H 0.0222 0.6203 0.2311 0.123 Uiso 0.50 1 calc PR A 1
H42B H 0.0741 0.5558 0.1858 0.123 Uiso 0.50 1 calc PR A 1
H42C H 0.1483 0.6078 0.2287 0.123 Uiso 0.50 1 calc PR A 1
C41A C 0.097(2) 0.544(2) 0.2615(13) 0.072(10) Uani 0.50 1 d P A 2
H41C H 0.0276 0.5656 0.2481 0.086 Uiso 0.50 1 calc PR A 2
H41D H 0.1448 0.5972 0.2612 0.086 Uiso 0.50 1 calc PR A 2
C42A C 0.135(2) 0.4891(16) 0.2214(8) 0.076(8) Uani 0.50 1 d P A 2
H42D H 0.2020 0.4624 0.2332 0.114 Uiso 0.50 1 calc PR A 2
H42E H 0.1461 0.5240 0.1877 0.114 Uiso 0.50 1 calc PR A 2
H42F H 0.0830 0.4413 0.2143 0.114 Uiso 0.50 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Al1 0.0478(12) 0.0736(17) 0.0444(13) -0.0001(13) 0.0011(11) 0.0045(13)
O1 0.046(3) 0.060(4) 0.055(3) -0.003(3) -0.005(2) 0.006(3)
O2 0.045(3) 0.057(3) 0.055(3) -0.003(3) 0.005(2) 0.003(3)
N1 0.051(4) 0.069(5) 0.055(4) -0.010(4) 0.011(3) 0.004(3)
N2 0.051(4) 0.054(5) 0.065(4) -0.009(4) 0.006(3) -0.003(4)
N3 0.091(5) 0.101(7) 0.050(5) -0.013(5) 0.016(4) 0.013(5)
N4 0.056(4) 0.074(6) 0.061(5) 0.004(4) 0.003(3) 0.001(4)
N5 0.049(3) 0.046(4) 0.055(4) 0.004(3) -0.004(3) 0.001(3)
N6 0.046(4) 0.067(5) 0.058(4) 0.021(4) -0.008(3) -0.003(3)
N7 0.040(3) 0.059(5) 0.052(4) 0.002(3) -0.001(3) -0.004(3)
N8 0.081(5) 0.079(6) 0.068(5) -0.010(5) -0.014(4) 0.020(4)
N9 0.058(4) 0.062(5) 0.052(5) -0.018(4) -0.011(3) 0.012(4)
N10 0.057(4) 0.037(4) 0.058(4) -0.003(3) 0.003(3) -0.006(3)
C1 0.068(6) 0.066(6) 0.078(6) -0.004(5) 0.005(5) 0.019(5)
C2 0.087(6) 0.053(6) 0.088(6) -0.013(5) 0.017(6) 0.018(5)
C3 0.075(6) 0.067(7) 0.055(5) -0.014(5) 0.022(4) 0.006(5)
C4 0.065(6) 0.094(7) 0.125(8) -0.012(6) 0.003(5) 0.033(5)
C5 0.090(6) 0.084(7) 0.081(6) -0.034(5) 0.007(5) -0.002(6)
C6 0.047(4) 0.080(8) 0.071(7) -0.011(6) -0.005(4) -0.001(5)
C7 0.075(6) 0.116(10) 0.060(6) 0.017(6) 0.008(5) -0.001(7)
C8 0.106(7) 0.125(10) 0.045(6) -0.007(7) 0.017(5) 0.002(8)
C9 0.078(6) 0.083(7) 0.083(6) 0.015(6) -0.005(5) -0.017(5)
C10 0.230(14) 0.176(12) 0.076(8) -0.011(8) 0.062(9) -0.024(11)
C11 0.044(4) 0.081(7) 0.051(5) -0.011(5) -0.007(4) 0.010(5)
C12 0.042(4) 0.054(5) 0.053(5) 0.006(4) -0.007(4) 0.002(4)
C13 0.058(5) 0.050(6) 0.059(5) -0.008(4) 0.014(4) -0.001(4)
C14 0.120(7) 0.073(7) 0.060(6) 0.001(5) 0.017(5) 0.006(6)
C15 0.055(5) 0.049(6) 0.056(5) -0.003(4) 0.005(4) 0.008(4)
C16 0.061(5) 0.059(6) 0.084(6) -0.009(5) -0.001(5) -0.006(5)
C17 0.111(8) 0.062(7) 0.067(6) -0.013(5) 0.013(6) -0.023(6)
C18 0.126(9) 0.069(8) 0.090(8) -0.003(6) -0.016(7) 0.011(8)
C19 0.101(8) 0.069(8) 0.145(10) -0.014(7) -0.034(7) 0.023(7)
C20 0.067(5) 0.067(6) 0.077(6) -0.002(5) -0.012(5) -0.003(5)
C21 0.065(5) 0.061(6) 0.048(5) -0.007(4) -0.004(4) 0.014(5)
C22 0.081(6) 0.051(5) 0.059(5) 0.007(5) -0.011(5) 0.011(5)
C23 0.065(6) 0.080(7) 0.057(5) 0.020(5) -0.007(4) -0.002(5)
C24 0.064(5) 0.078(6) 0.083(6) -0.007(5) -0.016(5) 0.025(5)
C25 0.081(6) 0.084(7) 0.125(8) 0.027(6) -0.006(6) -0.016(6)
C26 0.054(5) 0.061(7) 0.068(6) -0.011(5) -0.001(4) 0.000(5)
C27 0.080(6) 0.083(8) 0.075(7) -0.028(6) -0.025(5) 0.015(6)
C28 0.104(7) 0.094(9) 0.062(6) -0.023(7) -0.017(5) 0.037(7)
C29 0.075(6) 0.075(7) 0.097(7) -0.018(6) -0.002(6) -0.021(5)
C30 0.225(12) 0.122(9) 0.054(6) -0.024(7) -0.040(7) 0.052(9)
C31 0.047(4) 0.055(6) 0.065(5) 0.009(5) 0.004(4) -0.002(4)
C32 0.048(4) 0.046(5) 0.052(5) -0.005(4) 0.006(4) 0.006(4)
C33 0.069(5) 0.045(5) 0.059(5) 0.001(4) -0.013(4) -0.005(4)
C34 0.138(8) 0.092(7) 0.041(5) 0.003(5) -0.007(5) 0.004(7)
C35 0.071(5) 0.055(6) 0.049(5) 0.014(4) 0.002(4) -0.003(5)
C36 0.090(7) 0.052(6) 0.104(7) 0.013(5) 0.018(6) 0.012(5)
C37 0.144(11) 0.072(9) 0.144(11) 0.025(8) 0.028(9) 0.039(8)
C38 0.172(12) 0.051(7) 0.124(10) -0.003(7) -0.003(9) 0.002(9)
C39 0.123(9) 0.058(8) 0.124(9) 0.019(7) 0.007(8) -0.009(7)
C40 0.076(6) 0.061(7) 0.091(7) 0.005(5) 0.007(5) 0.002(5)
C41 0.078(17) 0.071(3) 0.062(15) 0.015(17) 0.025(12) -0.020(14)
C42 0.098(5) 0.086(3) 0.062(17) 0.049(18) 0.03(2) 0.03(3)
C41A 0.069(15) 0.097(3) 0.050(14) 0.03(2) 0.018(11) -0.024(16)
C42A 0.095(2) 0.097(19) 0.036(11) 0.016(12) 0.002(13) 0.030(18)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.779(5) . ?
Al1 O2 1.786(5) . ?
Al1 C41 1.91(3) . ?
Al1 C41A 2.00(3) . ?
Al1 N6 2.110(6) . ?
Al1 N1 2.120(7) . ?
O1 C12 1.300(7) . ?
O2 C32 1.324(8) . ?
N1 C3 1.337(9) . ?
N1 N2 1.376(7) . ?
N2 C1 1.347(9) . ?
N2 C11 1.429(9) . ?
N3 C8 1.340(11) . ?
N3 N4 1.354(8) . ?
N4 C6 1.359(10) . ?
N4 C11 1.463(9) . ?
N5 C12 1.284(8) . ?
N5 C13 1.466(8) . ?
N6 C23 1.338(9) . ?
N6 N7 1.371(7) . ?
N7 C21 1.366(8) . ?
N7 C31 1.456(9) . ?
N8 C28 1.314(11) . ?
N8 N9 1.353(8) . ?
N9 C26 1.368(9) . ?
N9 C31 1.438(9) . ?
N10 C32 1.265(8) . ?
N10 C33 1.493(8) . ?
C1 C2 1.355(11) . ?
C1 C4 1.493(11) . ?
C2 C3 1.389(11) . ?
C3 C5 1.477(10) . ?
C6 C7 1.362(11) . ?
C6 C9 1.475(11) . ?
C7 C8 1.357(12) . ?
C8 C10 1.472(12) . ?
C11 C12 1.535(9) . ?
C13 C14 1.526(9) . ?
C13 C15 1.538(10) . ?
C15 C16 1.357(10) . ?
C15 C20 1.378(10) . ?
C16 C17 1.386(11) . ?
C17 C18 1.365(12) . ?
C18 C19 1.348(13) . ?
C19 C20 1.400(12) . ?
C21 C22 1.363(10) . ?
C21 C24 1.486(10) . ?
C22 C23 1.404(10) . ?
C23 C25 1.493(10) . ?
C26 C27 1.350(10) . ?
C26 C29 1.492(10) . ?
C27 C28 1.396(12) . ?
C28 C30 1.485(12) . ?
C31 C32 1.510(9) . ?
C33 C35 1.492(10) . ?
C33 C34 1.511(9) . ?
C35 C36 1.369(11) . ?
C35 C40 1.381(11) . ?
C36 C37 1.388(13) . ?
C37 C38 1.363(14) . ?
C38 C39 1.363(14) . ?
C39 C40 1.371(13) . ?
C41 C42 1.49(3) . ?
C41A C42A 1.33(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 111.1(2) . . ?
O1 Al1 C41 135.3(7) . . ?
O2 Al1 C41 113.4(7) . . ?
O1 Al1 C41A 115.3(8) . . ?
O2 Al1 C41A 133.6(8) . . ?
C41 Al1 C41A 21.4(10) . . ?
O1 Al1 N6 86.7(2) . . ?
O2 Al1 N6 87.9(2) . . ?
C41 Al1 N6 99.3(11) . . ?
C41A Al1 N6 91.9(11) . . ?
O1 Al1 N1 87.6(2) . . ?
O2 Al1 N1 85.9(2) . . ?
C41 Al1 N1 90.9(11) . . ?
C41A Al1 N1 98.4(11) . . ?
N6 Al1 N1 169.6(2) . . ?
C12 O1 Al1 130.6(5) . . ?
C32 O2 Al1 129.0(5) . . ?
C3 N1 N2 105.1(6) . . ?
C3 N1 Al1 130.3(6) . . ?
N2 N1 Al1 124.2(5) . . ?
C1 N2 N1 111.7(7) . . ?
C1 N2 C11 127.0(7) . . ?
N1 N2 C11 120.2(6) . . ?
C8 N3 N4 103.3(8) . . ?
N3 N4 C6 112.7(7) . . ?
N3 N4 C11 118.5(7) . . ?
C6 N4 C11 128.4(8) . . ?
C12 N5 C13 115.3(6) . . ?
C23 N6 N7 104.6(6) . . ?
C23 N6 Al1 130.7(5) . . ?
N7 N6 Al1 123.9(5) . . ?
C21 N7 N6 112.2(6) . . ?
C21 N7 C31 127.2(6) . . ?
N6 N7 C31 120.3(6) . . ?
C28 N8 N9 105.5(8) . . ?
N8 N9 C26 111.7(7) . . ?
N8 N9 C31 121.0(7) . . ?
C26 N9 C31 127.2(8) . . ?
C32 N10 C33 117.6(6) . . ?
N2 C1 C2 105.8(7) . . ?
N2 C1 C4 123.1(9) . . ?
C2 C1 C4 131.1(9) . . ?
C1 C2 C3 108.1(8) . . ?
N1 C3 C2 109.3(8) . . ?
N1 C3 C5 122.7(8) . . ?
C2 C3 C5 128.0(9) . . ?
N4 C6 C7 104.9(8) . . ?
N4 C6 C9 125.5(8) . . ?
C7 C6 C9 129.5(10) . . ?
C8 C7 C6 107.2(9) . . ?
N3 C8 C7 111.8(8) . . ?
N3 C8 C10 117.3(11) . . ?
C7 C8 C10 130.9(11) . . ?
N2 C11 N4 110.1(6) . . ?
N2 C11 C12 107.8(6) . . ?
N4 C11 C12 113.7(7) . . ?
N5 C12 O1 126.9(7) . . ?
N5 C12 C11 117.1(6) . . ?
O1 C12 C11 116.0(6) . . ?
N5 C13 C14 108.7(6) . . ?
N5 C13 C15 110.4(6) . . ?
C14 C13 C15 109.7(6) . . ?
C16 C15 C20 117.8(7) . . ?
C16 C15 C13 122.4(8) . . ?
C20 C15 C13 119.8(8) . . ?
C15 C16 C17 121.9(9) . . ?
C18 C17 C16 120.3(9) . . ?
C19 C18 C17 118.7(10) . . ?
C18 C19 C20 121.4(9) . . ?
C15 C20 C19 120.0(8) . . ?
C22 C21 N7 105.7(6) . . ?
C22 C21 C24 131.7(8) . . ?
N7 C21 C24 122.6(8) . . ?
C21 C22 C23 107.0(7) . . ?
N6 C23 C22 110.5(7) . . ?
N6 C23 C25 122.6(8) . . ?
C22 C23 C25 126.9(8) . . ?
C27 C26 N9 105.4(8) . . ?
C27 C26 C29 130.4(9) . . ?
N9 C26 C29 124.2(8) . . ?
C26 C27 C28 107.0(8) . . ?
N8 C28 C27 110.4(8) . . ?
N8 C28 C30 118.9(11) . . ?
C27 C28 C30 130.7(10) . . ?
N9 C31 N7 109.0(6) . . ?
N9 C31 C32 114.3(6) . . ?
N7 C31 C32 108.2(6) . . ?
N10 C32 O2 126.8(7) . . ?
N10 C32 C31 117.6(6) . . ?
O2 C32 C31 115.6(6) . . ?
C35 C33 N10 108.5(6) . . ?
C35 C33 C34 113.6(6) . . ?
N10 C33 C34 108.8(6) . . ?
C36 C35 C40 117.4(8) . . ?
C36 C35 C33 121.7(8) . . ?
C40 C35 C33 120.9(8) . . ?
C35 C36 C37 121.3(10) . . ?
C38 C37 C36 118.7(11) . . ?
C37 C38 C39 121.9(11) . . ?
C38 C39 C40 118.0(11) . . ?
C39 C40 C35 122.6(10) . . ?
C42 C41 Al1 122(2) . . ?
C42A C41A Al1 128(3) . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.105


data_7
_database_code_depnum_ccdc_archive 'CCDC 907284'
#TrackingRef 'XRAY.CIF'
# start Validation Reply Form
_vrf_THETM01_7                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Crystals were weakly diffracting and no significant data could be
obtained beyond theta = 22.5. This was the limit of observed reflections.
This resolution has been considered as sufficient to resolve the structure
from experimental data.
;
_vrf_PLAT023_7                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.49 Deg.
RESPONSE: Crystals were weakly diffracting and no significant data could be
obtained beyond theta = 22.5. This was the limit of observed reflections.
This resolution has been considered as sufficient to resolve the structure
from experimental data.
;
_vrf_RINTA01_7                   
;
PROBLEM: The value of Rint is greater than 0.18 Rint given 0.216
RESPONSE:
Quality of the data was poor due to the crystal quality and also
the crystal is very weakly diffracting, so that a large proportion
of essentially "unobserved" reflections were used in the refinement.
;
# end Validation Reply Form
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H57 Al N10 O3'
_chemical_formula_sum            'C40 H57 Al N10 O3'
_chemical_formula_weight         752.94
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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   18.826(3)
_cell_length_b                   14.547(4)
_cell_length_c                   16.447(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.58(2)
_cell_angle_gamma                90.00
_cell_volume                     4158.9(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    175
_cell_measurement_theta_min      2.343
_cell_measurement_theta_max      11.797
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9726
_exptl_absorpt_correction_T_max  0.9941
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      230(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8930
_diffrn_reflns_av_R_equivalents  0.2158
_diffrn_reflns_av_sigmaI/netI    0.2810
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         22.49
_reflns_number_total             2705
_reflns_number_gt                827
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2705
_refine_ls_number_parameters     247
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2310
_refine_ls_R_factor_gt           0.0690
_refine_ls_wR_factor_ref         0.2233
_refine_ls_wR_factor_gt          0.1382
_refine_ls_goodness_of_fit_ref   0.794
_refine_ls_restrained_S_all      0.794
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
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 0.0000 0.35809(19) 0.2500 0.0640(10) Uani 1 2 d S . .
N1 N 0.1002(4) 0.3543(4) 0.3607(4) 0.0649(16) Uani 1 1 d . . .
N2 N 0.1066(3) 0.3168(4) 0.4394(4) 0.0652(16) Uani 1 1 d . . .
N3 N 0.0837(3) 0.1473(4) 0.3408(3) 0.0603(16) Uani 1 1 d . . .
N4 N 0.0767(3) 0.1584(4) 0.4206(3) 0.0587(15) Uani 1 1 d . . .
N5 N -0.0776(4) 0.2430(4) 0.4240(3) 0.0734(17) Uani 1 1 d . B .
O1 O -0.0490(2) 0.3096(3) 0.3123(3) 0.0619(13) Uani 1 1 d . . .
O2 O 0.0000 0.4752(5) 0.2500 0.089(2) Uani 1 2 d S . .
C1 C 0.1739(4) 0.3394(6) 0.5066(5) 0.079(2) Uani 1 1 d . . .
C2 C 0.2092(5) 0.3949(6) 0.4684(6) 0.090(3) Uani 1 1 d . . .
H2 H 0.2566 0.4230 0.4977 0.108 Uiso 1 1 calc R . .
C3 C 0.1653(5) 0.4044(5) 0.3796(6) 0.075(2) Uani 1 1 d . . .
C4 C 0.1971(4) 0.3068(5) 0.5976(4) 0.104(3) Uani 1 1 d . . .
H4A H 0.2112 0.2431 0.6006 0.155 Uiso 1 1 calc R . .
H4B H 0.1550 0.3140 0.6163 0.155 Uiso 1 1 calc R . .
H4C H 0.2403 0.3420 0.6353 0.155 Uiso 1 1 calc R . .
C5 C 0.1798(5) 0.4565(5) 0.3083(5) 0.105(3) Uani 1 1 d . . .
H5A H 0.2340 0.4675 0.3263 0.158 Uiso 1 1 calc R . .
H5B H 0.1530 0.5141 0.2982 0.158 Uiso 1 1 calc R . .
H5C H 0.1618 0.4210 0.2550 0.158 Uiso 1 1 calc R . .
C6 C 0.0837(4) 0.0764(6) 0.4645(4) 0.069(2) Uani 1 1 d . . .
C7 C 0.0962(4) 0.0124(5) 0.4104(5) 0.074(2) Uani 1 1 d . . .
H7 H 0.1036 -0.0503 0.4216 0.089 Uiso 1 1 calc R . .
C8 C 0.0958(4) 0.0583(6) 0.3350(5) 0.071(2) Uani 1 1 d . . .
C9 C 0.0784(4) 0.0681(5) 0.5522(4) 0.090(2) Uani 1 1 d . . .
H9A H 0.0854 0.0050 0.5707 0.135 Uiso 1 1 calc R . .
H9B H 0.0287 0.0888 0.5481 0.135 Uiso 1 1 calc R . .
H9C H 0.1176 0.1051 0.5943 0.135 Uiso 1 1 calc R . .
C10 C 0.1090(4) 0.0231(5) 0.2579(4) 0.093(3) Uani 1 1 d . . .
H10A H 0.0836 -0.0351 0.2406 0.139 Uiso 1 1 calc R . .
H10B H 0.1632 0.0154 0.2729 0.139 Uiso 1 1 calc R . .
H10C H 0.0888 0.0659 0.2101 0.139 Uiso 1 1 calc R . .
C12 C 0.0515(4) 0.2472(5) 0.4435(4) 0.066(2) Uani 1 1 d . . .
H12 H 0.0563 0.2432 0.5048 0.079 Uiso 1 1 calc R . .
C13 C -0.0321(4) 0.2673(5) 0.3877(5) 0.0578(19) Uani 1 1 d . . .
C14 C -0.1580(5) 0.2613(5) 0.3768(5) 0.083(2) Uani 1 1 d . . .
H14 H -0.1746 0.2702 0.3131 0.099 Uiso 1 1 calc R A 1
C15 C -0.1753(15) 0.3415(15) 0.4286(14) 0.123(10) Uiso 0.50 1 d P B 1
H15A H -0.1518 0.3968 0.4191 0.185 Uiso 0.50 1 calc PR B 1
H15B H -0.1550 0.3271 0.4903 0.185 Uiso 0.50 1 calc PR B 1
H15C H -0.2299 0.3502 0.4085 0.185 Uiso 0.50 1 calc PR B 1
C16 C -0.2021(12) 0.1927(14) 0.4054(15) 0.102(8) Uiso 0.50 1 d P B 1
H16A H -0.1901 0.1985 0.4680 0.123 Uiso 0.50 1 calc PR B 1
H16B H -0.1893 0.1308 0.3936 0.123 Uiso 0.50 1 calc PR B 1
C17 C -0.2959(9) 0.2142(11) 0.3477(10) 0.120(6) Uiso 0.50 1 d P B 1
H17A H -0.3265 0.1724 0.3657 0.180 Uiso 0.50 1 calc PR B 1
H17B H -0.3072 0.2064 0.2860 0.180 Uiso 0.50 1 calc PR B 1
H17C H -0.3074 0.2762 0.3586 0.180 Uiso 0.50 1 calc PR B 1
C15A C -0.1777(11) 0.3573(13) 0.3970(13) 0.082(6) Uiso 0.50 1 d P B 2
H15D H -0.1543 0.3695 0.4597 0.099 Uiso 0.50 1 calc PR B 2
H15E H -0.1598 0.4029 0.3662 0.099 Uiso 0.50 1 calc PR B 2
C16A C -0.2086(14) 0.1738(14) 0.3732(14) 0.122(10) Uiso 0.50 1 d P B 2
H16C H -0.2002 0.1283 0.3356 0.182 Uiso 0.50 1 calc PR B 2
H16D H -0.2620 0.1908 0.3503 0.182 Uiso 0.50 1 calc PR B 2
H16E H -0.1946 0.1490 0.4314 0.182 Uiso 0.50 1 calc PR B 2
C17A C -0.2627(14) 0.3592(14) 0.3659(14) 0.194(9) Uiso 0.50 1 d P B 2
H17D H -0.2778 0.4042 0.3989 0.291 Uiso 0.50 1 calc PR B 2
H17E H -0.2810 0.2997 0.3742 0.291 Uiso 0.50 1 calc PR B 2
H17F H -0.2843 0.3749 0.3045 0.291 Uiso 0.50 1 calc PR B 2
C18 C 0.0000 0.5691(8) 0.2500 0.076(3) Uani 1 2 d S . .
C19 C 0.0009(4) 0.6143(5) 0.3243(5) 0.070(2) Uani 1 1 d . . .
C20 C 0.0018(4) 0.7076(6) 0.3225(5) 0.092(3) Uani 1 1 d . . .
H20 H 0.0037 0.7388 0.3726 0.111 Uiso 1 1 calc R . .
C21 C 0.0000 0.7602(9) 0.2500 0.114(4) Uani 1 2 d S . .
H21 H 0.0000 0.8241 0.2500 0.137 Uiso 1 2 calc SR . .
C22 C -0.0016(5) 0.5594(5) 0.4017(4) 0.108(3) Uani 1 1 d . . .
H22A H -0.0033 0.4949 0.3885 0.161 Uiso 1 1 calc R . .
H22B H -0.0465 0.5761 0.4124 0.161 Uiso 1 1 calc R . .
H22C H 0.0436 0.5724 0.4531 0.161 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Al1 0.064(2) 0.061(2) 0.073(2) 0.000 0.0318(18) 0.000
N1 0.067(5) 0.059(4) 0.064(4) -0.006(3) 0.019(4) -0.015(4)
N2 0.044(4) 0.085(5) 0.056(4) 0.002(3) 0.006(4) 0.007(4)
N3 0.061(4) 0.065(4) 0.057(4) -0.007(3) 0.026(3) -0.010(3)
N4 0.067(4) 0.063(4) 0.051(4) 0.002(3) 0.028(3) -0.004(3)
N5 0.048(5) 0.103(5) 0.072(4) 0.013(3) 0.026(4) 0.010(4)
O1 0.054(3) 0.068(3) 0.061(3) 0.010(2) 0.018(3) 0.002(2)
O2 0.105(6) 0.073(6) 0.086(5) 0.000 0.034(4) 0.000
C1 0.023(5) 0.124(7) 0.073(7) -0.023(5) 0.000(5) -0.007(5)
C2 0.046(6) 0.110(7) 0.096(8) -0.052(5) 0.009(6) -0.025(5)
C3 0.053(6) 0.076(6) 0.094(7) -0.017(5) 0.025(6) -0.007(5)
C4 0.052(6) 0.156(8) 0.063(6) -0.015(5) -0.022(4) -0.014(5)
C5 0.105(7) 0.089(6) 0.140(7) -0.013(5) 0.066(6) -0.031(5)
C6 0.068(6) 0.068(6) 0.060(5) -0.002(4) 0.013(4) -0.018(4)
C7 0.075(6) 0.071(5) 0.068(5) 0.007(5) 0.016(5) 0.005(4)
C8 0.057(5) 0.077(6) 0.079(6) -0.016(5) 0.025(5) -0.007(5)
C9 0.108(7) 0.120(6) 0.044(5) 0.013(4) 0.030(5) 0.000(5)
C10 0.100(7) 0.103(6) 0.082(5) -0.030(4) 0.044(5) -0.004(5)
C12 0.058(6) 0.078(6) 0.061(5) -0.015(4) 0.022(4) -0.013(5)
C13 0.028(5) 0.077(5) 0.061(5) -0.002(4) 0.010(5) 0.002(4)
C14 0.059(6) 0.103(7) 0.085(5) 0.014(5) 0.026(5) -0.013(5)
C18 0.051(7) 0.070(9) 0.098(10) 0.000 0.019(7) 0.000
C19 0.068(6) 0.069(6) 0.076(6) -0.014(5) 0.031(4) -0.003(5)
C20 0.087(7) 0.082(7) 0.122(8) -0.026(6) 0.057(6) -0.005(6)
C21 0.123(12) 0.072(10) 0.175(14) 0.000 0.088(11) 0.000
C22 0.147(9) 0.132(7) 0.059(5) -0.006(5) 0.057(5) 0.019(6)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O2 1.704(8) . ?
Al1 O1 1.768(4) 2 ?
Al1 O1 1.768(4) . ?
Al1 N1 2.058(6) . ?
Al1 N1 2.058(6) 2 ?
N1 C3 1.356(8) . ?
N1 N2 1.368(6) . ?
N2 C1 1.363(8) . ?
N2 C12 1.470(8) . ?
N3 C8 1.325(8) . ?
N3 N4 1.377(6) . ?
N4 C6 1.374(8) . ?
N4 C12 1.475(7) . ?
N5 C13 1.268(7) . ?
N5 C14 1.436(8) . ?
O1 C13 1.309(7) . ?
O2 C18 1.366(11) . ?
C1 C2 1.346(9) . ?
C1 C4 1.467(9) . ?
C2 C3 1.381(8) . ?
C3 C5 1.506(9) . ?
C6 C7 1.369(8) . ?
C6 C9 1.488(7) . ?
C7 C8 1.407(8) . ?
C8 C10 1.474(8) . ?
C12 C13 1.515(8) . ?
C14 C16 1.49(2) . ?
C14 C15A 1.514(19) . ?
C14 C15 1.55(2) . ?
C14 C16A 1.58(2) . ?
C16 C17 1.68(3) . ?
C15A C17A 1.48(3) . ?
C18 C19 1.382(8) . ?
C18 C19 1.382(8) 2 ?
C19 C20 1.357(9) . ?
C19 C22 1.519(8) . ?
C20 C21 1.406(9) . ?
C21 C20 1.406(9) 2 ?
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
O2 Al1 O1 113.51(15) . 2 ?
O2 Al1 O1 113.51(15) . . ?
O1 Al1 O1 133.0(3) 2 . ?
O2 Al1 N1 91.52(17) . . ?
O1 Al1 N1 89.8(2) 2 . ?
O1 Al1 N1 89.0(2) . . ?
O2 Al1 N1 91.52(17) . 2 ?
O1 Al1 N1 89.0(2) 2 2 ?
O1 Al1 N1 89.8(2) . 2 ?
N1 Al1 N1 177.0(3) . 2 ?
C3 N1 N2 104.7(6) . . ?
C3 N1 Al1 129.0(6) . . ?
N2 N1 Al1 124.5(5) . . ?
C1 N2 N1 112.9(7) . . ?
C1 N2 C12 125.6(7) . . ?
N1 N2 C12 120.7(6) . . ?
C8 N3 N4 105.4(5) . . ?
N3 N4 C6 112.0(6) . . ?
N3 N4 C12 120.2(5) . . ?
C6 N4 C12 127.0(6) . . ?
C13 N5 C14 117.1(6) . . ?
C13 O1 Al1 138.2(5) . . ?
C18 O2 Al1 180.000(2) . . ?
C2 C1 N2 103.7(8) . . ?
C2 C1 C4 131.6(8) . . ?
N2 C1 C4 124.7(8) . . ?
C1 C2 C3 110.6(7) . . ?
N1 C3 C2 108.1(7) . . ?
N1 C3 C5 120.6(8) . . ?
C2 C3 C5 131.3(8) . . ?
N4 C6 C7 104.7(6) . . ?
N4 C6 C9 123.5(7) . . ?
C7 C6 C9 131.8(7) . . ?
C6 C7 C8 107.8(7) . . ?
N3 C8 C7 110.0(6) . . ?
N3 C8 C10 119.5(7) . . ?
C7 C8 C10 130.4(8) . . ?
N2 C12 N4 106.9(5) . . ?
N2 C12 C13 115.3(6) . . ?
N4 C12 C13 112.1(5) . . ?
N5 C13 O1 128.0(6) . . ?
N5 C13 C12 113.1(7) . . ?
O1 C13 C12 118.8(7) . . ?
N5 C14 C16 107.8(10) . . ?
N5 C14 C15A 110.4(9) . . ?
C16 C14 C15A 109.7(13) . . ?
N5 C14 C15 104.0(11) . . ?
C16 C14 C15 94.0(12) . . ?
C15A C14 C15 20.8(12) . . ?
N5 C14 C16A 111.6(10) . . ?
C16 C14 C16A 21.1(13) . . ?
C15A C14 C16A 123.8(14) . . ?
C15 C14 C16A 112.1(13) . . ?
C14 C16 C17 106.8(13) . . ?
C17A C15A C14 105.4(15) . . ?
O2 C18 C19 118.4(5) . . ?
O2 C18 C19 118.4(5) . 2 ?
C19 C18 C19 123.1(11) . 2 ?
C20 C19 C18 116.9(8) . . ?
C20 C19 C22 123.3(7) . . ?
C18 C19 C22 119.8(7) . . ?
C19 C20 C21 124.5(9) . . ?
C20 C21 C20 114.0(11) 2 . ?
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        22.49
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.039