# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_wu22302
_database_code_depnum_ccdc_archive 'CCDC 1413583'
_audit_update_record             
;
2015-07-18 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H24 Al N3'
_chemical_formula_weight         297.37

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.9611(4)
_cell_length_b                   11.2380(3)
_cell_length_c                   8.7019(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.676(2)
_cell_angle_gamma                90.00
_cell_volume                     1624.34(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      28.70

_exptl_crystal_description       lamellar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            18729
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         28.70
_reflns_number_total             4179
_reflns_number_gt                2608
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0502P)²+0.3832P] where P=(Fo²+2Fc²)/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         4179
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1298
_refine_ls_wR_factor_gt          0.1110
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_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 0.29548(4) 0.55149(5) 0.48203(8) 0.02593(17) Uani 1 1 d . . .
C5 C 0.40943(12) 0.39804(18) 0.3917(2) 0.0270(4) Uani 1 1 d . . .
H5A H 0.4221 0.3190 0.3592 0.032 Uiso 1 1 calc R . .
H5B H 0.4433 0.4547 0.3513 0.032 Uiso 1 1 calc R . .
C9 C 0.31387(12) 0.46139(17) 0.1588(2) 0.0272(4) Uani 1 1 d . . .
H9A H 0.3384 0.4008 0.1044 0.033 Uiso 1 1 calc R . .
H9B H 0.3429 0.5352 0.1539 0.033 Uiso 1 1 calc R . .
C8 C 0.22720(12) 0.47805(17) 0.0761(2) 0.0275(5) Uani 1 1 d . . .
H8A H 0.2034 0.5424 0.1255 0.033 Uiso 1 1 calc R . .
H8B H 0.2253 0.4997 -0.0325 0.033 Uiso 1 1 calc R . .
C7 C 0.18701(12) 0.33087(18) 0.2456(2) 0.0281(5) Uani 1 1 d . . .
H7A H 0.1582 0.2564 0.2473 0.034 Uiso 1 1 calc R . .
H7B H 0.1618 0.3899 0.3013 0.034 Uiso 1 1 calc R . .
C10 C 0.10241(12) 0.36601(17) -0.0134(2) 0.0257(4) Uani 1 1 d . . .
C15 C 0.07337(13) 0.45480(18) -0.1218(2) 0.0298(5) Uani 1 1 d . . .
H15 H 0.1048 0.5217 -0.1287 0.036 Uiso 1 1 calc R . .
C6 C 0.27328(12) 0.31444(16) 0.3277(2) 0.0264(4) Uani 1 1 d . . .
H6A H 0.2750 0.2905 0.4354 0.032 Uiso 1 1 calc R . .
H6B H 0.2972 0.2512 0.2766 0.032 Uiso 1 1 calc R . .
C11 C 0.05238(13) 0.26745(18) -0.0054(3) 0.0311(5) Uani 1 1 d . . .
H11 H 0.0698 0.2070 0.0664 0.037 Uiso 1 1 calc R . .
C4 C 0.42530(12) 0.40462(17) 0.5653(2) 0.0263(4) Uani 1 1 d . . .
C14 C -0.00183(13) 0.4447(2) -0.2197(3) 0.0351(5) Uani 1 1 d . . .
H14 H -0.0199 0.5048 -0.2917 0.042 Uiso 1 1 calc R . .
C12 C -0.02242(13) 0.25972(19) -0.1032(3) 0.0349(5) Uani 1 1 d . . .
H12 H -0.0548 0.1941 -0.0956 0.042 Uiso 1 1 calc R . .
C16 C 0.19990(12) 0.51786(19) 0.5703(2) 0.0299(5) Uani 1 1 d . . .
H16A H 0.2017 0.5650 0.6630 0.045 Uiso 1 1 calc R . .
H16B H 0.1991 0.4350 0.5968 0.045 Uiso 1 1 calc R . .
H16C H 0.1522 0.5372 0.4943 0.045 Uiso 1 1 calc R . .
C3 C 0.47619(12) 0.34688(17) 0.6840(3) 0.0299(5) Uani 1 1 d . . .
H3 H 0.5098 0.2833 0.6739 0.036 Uiso 1 1 calc R . .
C2 C 0.46743(13) 0.40342(18) 0.8260(3) 0.0330(5) Uani 1 1 d . . .
H2 H 0.4948 0.3843 0.9267 0.040 Uiso 1 1 calc R . .
C1 C 0.41120(13) 0.49119(19) 0.7860(3) 0.0314(5) Uani 1 1 d . . .
H1 H 0.3935 0.5416 0.8567 0.038 Uiso 1 1 calc R . .
C13 C -0.05030(13) 0.3472(2) -0.2121(3) 0.0348(5) Uani 1 1 d . . .
H13 H -0.1005 0.3405 -0.2786 0.042 Uiso 1 1 calc R . .
C17 C 0.30462(14) 0.71089(17) 0.3945(3) 0.0337(5) Uani 1 1 d . . .
H17A H 0.3494 0.7126 0.3424 0.051 Uiso 1 1 calc R . .
H17B H 0.3129 0.7685 0.4778 0.051 Uiso 1 1 calc R . .
H17C H 0.2560 0.7295 0.3207 0.051 Uiso 1 1 calc R . .
N3 N 0.18094(10) 0.36924(14) 0.08219(19) 0.0249(4) Uani 1 1 d . . .
N2 N 0.32172(10) 0.42576(13) 0.32660(19) 0.0233(4) Uani 1 1 d . . .
N1 N 0.38459(10) 0.49407(14) 0.6257(2) 0.0276(4) Uani 1 1 d . . .


_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 N1 1.8703(18) . ?
Al1 C17 1.965(2) . ?
Al1 C16 1.966(2) . ?
Al1 N2 2.0658(17) . ?
C5 C4 1.481(3) . ?
C5 N2 1.513(2) . ?
C9 N2 1.494(2) . ?
C9 C8 1.512(3) . ?
C8 N3 1.460(2) . ?
C7 N3 1.469(3) . ?
C7 C6 1.504(3) . ?
C10 C15 1.393(3) . ?
C10 C11 1.405(3) . ?
C10 N3 1.421(3) . ?
C15 C14 1.388(3) . ?
C6 N2 1.498(2) . ?
C11 C12 1.380(3) . ?
C4 C3 1.368(3) . ?
C4 N1 1.382(2) . ?
C14 C13 1.380(3) . ?
C12 C13 1.380(3) . ?
C3 C2 1.423(3) . ?
C2 C1 1.367(3) . ?
C1 N1 1.377(3) . ?

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
N1 Al1 C17 117.20(9) . . ?
N1 Al1 C16 106.93(9) . . ?
C17 Al1 C16 117.55(9) . . ?
N1 Al1 N2 87.11(7) . . ?
C17 Al1 N2 109.00(8) . . ?
C16 Al1 N2 115.36(8) . . ?
C4 C5 N2 109.49(16) . . ?
N2 C9 C8 112.61(16) . . ?
N3 C8 C9 110.91(16) . . ?
N3 C7 C6 111.50(16) . . ?
C15 C10 C11 117.63(19) . . ?
C15 C10 N3 122.63(18) . . ?
C11 C10 N3 119.67(18) . . ?
C14 C15 C10 120.8(2) . . ?
N2 C6 C7 112.12(16) . . ?
C12 C11 C10 120.5(2) . . ?
C3 C4 N1 110.21(19) . . ?
C3 C4 C5 134.65(19) . . ?
N1 C4 C5 114.97(18) . . ?
C13 C14 C15 121.2(2) . . ?
C11 C12 C13 121.5(2) . . ?
C4 C3 C2 106.43(19) . . ?
C1 C2 C3 106.9(2) . . ?
C2 C1 N1 110.10(19) . . ?
C14 C13 C12 118.3(2) . . ?
C10 N3 C8 116.57(16) . . ?
C10 N3 C7 115.64(16) . . ?
C8 N3 C7 110.37(16) . . ?
C9 N2 C6 106.84(15) . . ?
C9 N2 C5 107.92(15) . . ?
C6 N2 C5 108.94(14) . . ?
C9 N2 Al1 117.92(12) . . ?
C6 N2 Al1 112.08(12) . . ?
C5 N2 Al1 102.78(12) . . ?
C1 N1 C4 106.34(17) . . ?
C1 N1 Al1 137.73(15) . . ?
C4 N1 Al1 113.29(14) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.055
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_wu22402
_database_code_depnum_ccdc_archive 'CCDC 1413584'
_audit_update_record             
;
2015-07-18 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H39 Al Cl N6'
_chemical_formula_weight         558.11

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)
_symmetry_space_group_name_hall  '-P 2ac 2ab'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.2235(14)
_cell_length_b                   23.797(4)
_cell_length_c                   18.464(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4052.8(11)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1065
_cell_measurement_theta_min      2.468
_cell_measurement_theta_max      17.386

_exptl_crystal_description       columnar
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1782
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9524
_exptl_absorpt_correction_T_max  0.9582
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       /w
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31546
_diffrn_reflns_av_R_equivalents  0.1400
_diffrn_reflns_av_sigmaI/netI    0.1632
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         28.74
_reflns_number_total             10461
_reflns_number_gt                4593
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1000P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.00(16)
_refine_ls_number_reflns         10461
_refine_ls_number_parameters     479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1915
_refine_ls_R_factor_gt           0.0794
_refine_ls_wR_factor_ref         0.2290
_refine_ls_wR_factor_gt          0.1729
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.933
_refine_ls_shift/su_max          0.000
_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 0.80132(16) 0.83931(6) 0.63418(8) 0.0329(3) Uani 1 1 d . . .
C8 C 0.9988(5) 0.6639(2) 0.5974(3) 0.0373(12) Uani 1 1 d . . .
H8A H 0.9678 0.6570 0.5480 0.045 Uiso 1 1 calc R . .
H8B H 1.1014 0.6551 0.6005 0.045 Uiso 1 1 calc R . .
C10 C 0.9419(5) 0.56861(19) 0.6358(3) 0.0320(11) Uani 1 1 d . . .
C19 C 1.1152(5) 0.8512(2) 0.6784(3) 0.0351(12) Uani 1 1 d . . .
C7 C 0.7665(5) 0.64327(19) 0.6561(3) 0.0335(12) Uani 1 1 d . . .
H7A H 0.7251 0.6222 0.6960 0.040 Uiso 1 1 calc R . .
H7B H 0.7121 0.6340 0.6127 0.040 Uiso 1 1 calc R . .
C18 C 1.1968(6) 0.8381(2) 0.7387(3) 0.0413(12) Uani 1 1 d . . .
H18 H 1.2967 0.8419 0.7434 0.050 Uiso 1 1 calc R . .
C2 C 0.8931(5) 0.8440(2) 0.4147(3) 0.0374(12) Uani 1 1 d . . .
H2 H 0.9244 0.8591 0.3710 0.045 Uiso 1 1 calc R . .
C11 C 0.8412(6) 0.5276(2) 0.6565(3) 0.0392(13) Uani 1 1 d . . .
H11 H 0.7525 0.5386 0.6758 0.047 Uiso 1 1 calc R . .
C23 C 1.1547(6) 1.0172(2) 0.5204(3) 0.0398(13) Uani 1 1 d . . .
H23A H 1.1915 1.0301 0.4740 0.048 Uiso 1 1 calc R . .
H23B H 1.0501 1.0213 0.5199 0.048 Uiso 1 1 calc R . .
C16 C 0.9642(6) 0.8184(2) 0.7623(3) 0.0357(12) Uani 1 1 d . . .
H16 H 0.8803 0.8070 0.7861 0.043 Uiso 1 1 calc R . .
C14 C 1.1006(6) 0.4927(2) 0.5975(3) 0.0421(13) Uani 1 1 d . . .
H14 H 1.1877 0.4810 0.5771 0.051 Uiso 1 1 calc R . .
C5 C 0.7506(6) 0.7379(2) 0.5445(3) 0.0342(12) Uani 1 1 d . . .
H5A H 0.7732 0.7018 0.5228 0.041 Uiso 1 1 calc R . .
H5B H 0.6462 0.7411 0.5492 0.041 Uiso 1 1 calc R . .
C25 C 1.1856(5) 1.11073(19) 0.5701(3) 0.0351(11) Uani 1 1 d . . .
C9 C 0.9766(5) 0.72536(19) 0.6151(3) 0.0355(12) Uani 1 1 d . . .
H9A H 1.0203 0.7331 0.6618 0.043 Uiso 1 1 calc R . .
H9B H 1.0271 0.7478 0.5793 0.043 Uiso 1 1 calc R . .
C21 C 1.2143(7) 0.9681(2) 0.6560(3) 0.0454(14) Uani 1 1 d . . .
H21A H 1.3183 0.9633 0.6511 0.054 Uiso 1 1 calc R . .
H21B H 1.1859 0.9546 0.7035 0.054 Uiso 1 1 calc R . .
C13 C 0.9996(7) 0.4530(2) 0.6190(3) 0.0452(14) Uani 1 1 d . . .
H13 H 1.0186 0.4149 0.6134 0.054 Uiso 1 1 calc R . .
C24 C 1.1934(6) 0.9557(2) 0.5304(3) 0.0382(12) Uani 1 1 d . . .
H24A H 1.1515 0.9337 0.4915 0.046 Uiso 1 1 calc R . .
H24B H 1.2979 0.9512 0.5286 0.046 Uiso 1 1 calc R . .
C3 C 0.8464(5) 0.7879(2) 0.4277(3) 0.0365(12) Uani 1 1 d . . .
H3 H 0.8424 0.7589 0.3940 0.044 Uiso 1 1 calc R . .
C26 C 1.1094(6) 1.1424(2) 0.6195(3) 0.0506(15) Uani 1 1 d . . .
H26 H 1.0744 1.1252 0.6613 0.061 Uiso 1 1 calc R . .
C1 C 0.8821(5) 0.8713(2) 0.4807(3) 0.0390(13) Uani 1 1 d . . .
H1 H 0.9071 0.9087 0.4886 0.047 Uiso 1 1 calc R . .
C4 C 0.8089(5) 0.7847(2) 0.4987(3) 0.0324(11) Uani 1 1 d . . .
C15 C 1.0734(6) 0.5496(2) 0.6059(3) 0.0413(13) Uani 1 1 d . . .
H15 H 1.1430 0.5755 0.5916 0.050 Uiso 1 1 calc R . .
C17 C 1.1009(6) 0.8177(2) 0.7918(3) 0.0407(13) Uani 1 1 d . . .
H17 H 1.1254 0.8060 0.8382 0.049 Uiso 1 1 calc R . .
C20 C 1.1676(5) 0.8749(2) 0.6083(3) 0.0361(12) Uani 1 1 d . . .
H20A H 1.2712 0.8684 0.6045 0.043 Uiso 1 1 calc R . .
H20B H 1.1213 0.8548 0.5689 0.043 Uiso 1 1 calc R . .
C29 C 1.2144(7) 1.1956(2) 0.4983(3) 0.0577(17) Uani 1 1 d . . .
H29 H 1.2500 1.2131 0.4570 0.069 Uiso 1 1 calc R . .
C12 C 0.8717(6) 0.4706(2) 0.6486(3) 0.0429(14) Uani 1 1 d . . .
H12 H 0.8040 0.4442 0.6638 0.051 Uiso 1 1 calc R . .
C30 C 1.2393(7) 1.1385(2) 0.5097(3) 0.0488(15) Uani 1 1 d . . .
H30 H 1.2934 1.1185 0.4760 0.059 Uiso 1 1 calc R . .
C27 C 1.0834(7) 1.1991(2) 0.6086(4) 0.0579(17) Uani 1 1 d . . .
H27 H 1.0292 1.2193 0.6422 0.069 Uiso 1 1 calc R . .
C22 C 1.1755(7) 1.0295(2) 0.6486(3) 0.0519(15) Uani 1 1 d . . .
H22A H 1.0718 1.0339 0.6554 0.062 Uiso 1 1 calc R . .
H22B H 1.2241 1.0506 0.6864 0.062 Uiso 1 1 calc R . .
C6 C 0.7521(6) 0.7059(2) 0.6713(3) 0.0354(12) Uani 1 1 d . . .
H6A H 0.6498 0.7152 0.6738 0.043 Uiso 1 1 calc R . .
H6B H 0.7939 0.7136 0.7185 0.043 Uiso 1 1 calc R . .
C28 C 1.1371(8) 1.2256(3) 0.5483(4) 0.0642(19) Uani 1 1 d . . .
H28 H 1.1212 1.2639 0.5415 0.077 Uiso 1 1 calc R . .
C35 C 0.6423(5) 1.0946(2) 0.6822(3) 0.0366(12) Uani 1 1 d . . .
C33 C 0.6757(6) 1.0167(2) 0.5990(3) 0.0418(13) Uani 1 1 d . . .
H33A H 0.7645 1.0314 0.5782 0.050 Uiso 1 1 calc R . .
H33B H 0.5948 1.0312 0.5712 0.050 Uiso 1 1 calc R . .
C40 C 0.7326(6) 1.1279(2) 0.7243(3) 0.0399(13) Uani 1 1 d . . .
H40 H 0.8100 1.1120 0.7493 0.048 Uiso 1 1 calc R . .
C32 C 0.7781(6) 1.0113(2) 0.7184(3) 0.0400(13) Uani 1 1 d . . .
H32A H 0.7631 1.0219 0.7686 0.048 Uiso 1 1 calc R . .
H32B H 0.8704 1.0267 0.7030 0.048 Uiso 1 1 calc R . .
C31 C 0.7834(7) 0.9477(2) 0.7128(3) 0.0441(13) Uani 1 1 d . . .
H31A H 0.8657 0.9339 0.7403 0.053 Uiso 1 1 calc R . .
H31B H 0.6963 0.9321 0.7343 0.053 Uiso 1 1 calc R . .
C34 C 0.6768(6) 0.95267(19) 0.5949(3) 0.0398(13) Uani 1 1 d . . .
H34A H 0.5851 0.9384 0.6129 0.048 Uiso 1 1 calc R . .
H34B H 0.6862 0.9413 0.5447 0.048 Uiso 1 1 calc R . .
C36 C 0.5266(6) 1.1193(2) 0.6466(3) 0.0487(15) Uani 1 1 d . . .
H36 H 0.4638 1.0973 0.6193 0.058 Uiso 1 1 calc R . .
C39 C 0.7058(7) 1.1861(2) 0.7290(3) 0.0450(14) Uani 1 1 d . . .
H39 H 0.7660 1.2086 0.7572 0.054 Uiso 1 1 calc R . .
C38 C 0.5950(7) 1.2095(2) 0.6934(3) 0.0502(15) Uani 1 1 d . . .
H38 H 0.5795 1.2480 0.6969 0.060 Uiso 1 1 calc R . .
C37 C 0.5039(7) 1.1773(2) 0.6517(4) 0.0586(17) Uani 1 1 d . . .
H37 H 0.4273 1.1940 0.6270 0.070 Uiso 1 1 calc R . .
N7 N 1.1391(4) 0.93546(16) 0.5996(2) 0.0331(10) Uani 1 1 d . . .
N3 N 0.9184(4) 0.62658(16) 0.6462(2) 0.0342(10) Uani 1 1 d . . .
N8 N 1.2160(5) 1.05225(16) 0.5786(2) 0.0359(10) Uani 1 1 d . . .
N2 N 0.8222(4) 0.74322(16) 0.6173(2) 0.0319(9) Uani 1 1 d . . .
N5 N 0.7956(5) 0.92759(15) 0.6371(2) 0.0351(9) Uani 1 1 d . . .
H5 H 0.8608 0.9051 0.6207 0.042 Uiso 1 1 calc R . .
N6 N 0.6631(5) 1.03520(16) 0.6744(2) 0.0370(10) Uani 1 1 d . . .
N4 N 0.9698(4) 0.83843(16) 0.6921(2) 0.0309(9) Uani 1 1 d . . .
C41 C 0.6085(6) 0.8281(2) 0.6788(3) 0.0458(14) Uani 1 1 d . . .
H41A H 0.5634 0.8640 0.6867 0.069 Uiso 1 1 calc R . .
H41B H 0.6195 0.8090 0.7242 0.069 Uiso 1 1 calc R . .
H41C H 0.5491 0.8060 0.6471 0.069 Uiso 1 1 calc R . .
C42 C 0.8758(10) 0.1529(5) 0.4147(8) 0.174(7) Uani 1 1 d . . .
H42A H 0.9467 0.1810 0.4285 0.209 Uiso 1 1 calc R . .
H42B H 0.8086 0.1707 0.3814 0.209 Uiso 1 1 calc R . .
Cl1 Cl 0.7851(3) 0.13502(9) 0.48752(15) 0.1216(10) Uani 1 1 d . . .
Cl2 Cl 0.9659(4) 0.10013(18) 0.36777(15) 0.1672(16) Uani 1 1 d . . .
N1 N 0.8289(4) 0.83545(16) 0.5330(2) 0.0317(9) Uani 1 1 d . . .


_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 N4 1.886(4) . ?
Al1 N1 1.888(4) . ?
Al1 C41 1.978(6) . ?
Al1 N5 2.102(4) . ?
Al1 N2 2.316(4) . ?
C8 N3 1.467(6) . ?
C8 C9 1.514(6) . ?
C10 C11 1.401(7) . ?
C10 C15 1.408(7) . ?
C10 N3 1.409(6) . ?
C19 C18 1.380(7) . ?
C19 N4 1.398(6) . ?
C19 C20 1.493(7) . ?
C7 N3 1.468(6) . ?
C7 C6 1.522(6) . ?
C18 C17 1.406(7) . ?
C2 C1 1.385(7) . ?
C2 C3 1.421(7) . ?
C11 C12 1.392(7) . ?
C23 N8 1.474(6) . ?
C23 C24 1.518(7) . ?
C16 C17 1.373(7) . ?
C16 N4 1.383(6) . ?
C14 C13 1.384(8) . ?
C14 C15 1.386(7) . ?
C5 C4 1.498(7) . ?
C5 N2 1.503(6) . ?
C25 C26 1.376(7) . ?
C25 C30 1.386(7) . ?
C25 N8 1.428(6) . ?
C9 N2 1.487(6) . ?
C21 N7 1.472(6) . ?
C21 C22 1.510(7) . ?
C13 C12 1.366(8) . ?
C24 N7 1.453(6) . ?
C3 C4 1.358(7) . ?
C26 C27 1.387(8) . ?
C1 N1 1.379(6) . ?
C4 N1 1.376(6) . ?
C20 N7 1.475(6) . ?
C29 C28 1.368(9) . ?
C29 C30 1.394(8) . ?
C27 C28 1.371(9) . ?
C22 N8 1.450(7) . ?
C6 N2 1.485(6) . ?
C35 C36 1.384(7) . ?
C35 C40 1.388(7) . ?
C35 N6 1.434(6) . ?
C33 N6 1.464(6) . ?
C33 C34 1.525(6) . ?
C40 C39 1.411(7) . ?
C32 N6 1.452(6) . ?
C32 C31 1.519(7) . ?
C31 N5 1.481(6) . ?
C34 N5 1.471(6) . ?
C36 C37 1.400(7) . ?
C39 C38 1.336(8) . ?
C38 C37 1.372(8) . ?
C42 Cl1 1.640(11) . ?
C42 Cl2 1.736(13) . ?

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
N4 Al1 N1 116.69(19) . . ?
N4 Al1 C41 120.2(2) . . ?
N1 Al1 C41 121.8(2) . . ?
N4 Al1 N5 90.99(17) . . ?
N1 Al1 N5 94.43(17) . . ?
C41 Al1 N5 95.8(2) . . ?
N4 Al1 N2 89.84(16) . . ?
N1 Al1 N2 78.89(16) . . ?
C41 Al1 N2 89.88(19) . . ?
N5 Al1 N2 172.88(17) . . ?
N3 C8 C9 112.5(4) . . ?
C11 C10 C15 117.0(4) . . ?
C11 C10 N3 122.9(5) . . ?
C15 C10 N3 120.1(4) . . ?
C18 C19 N4 109.2(4) . . ?
C18 C19 C20 127.5(5) . . ?
N4 C19 C20 123.3(4) . . ?
N3 C7 C6 111.8(4) . . ?
C19 C18 C17 107.3(5) . . ?
C1 C2 C3 105.7(5) . . ?
C12 C11 C10 121.1(5) . . ?
N8 C23 C24 111.5(4) . . ?
C17 C16 N4 110.0(5) . . ?
C13 C14 C15 120.8(5) . . ?
C4 C5 N2 106.5(4) . . ?
C26 C25 C30 117.0(5) . . ?
C26 C25 N8 124.0(5) . . ?
C30 C25 N8 118.9(5) . . ?
N2 C9 C8 114.3(4) . . ?
N7 C21 C22 109.5(5) . . ?
C12 C13 C14 119.2(5) . . ?
N7 C24 C23 110.2(4) . . ?
C4 C3 C2 107.0(4) . . ?
C25 C26 C27 121.6(6) . . ?
N1 C1 C2 110.5(5) . . ?
C3 C4 N1 111.1(4) . . ?
C3 C4 C5 132.7(4) . . ?
N1 C4 C5 116.2(4) . . ?
C14 C15 C10 121.0(5) . . ?
C16 C17 C18 107.4(5) . . ?
N7 C20 C19 113.9(4) . . ?
C28 C29 C30 119.6(6) . . ?
C13 C12 C11 121.0(5) . . ?
C25 C30 C29 121.8(5) . . ?
C28 C27 C26 120.3(6) . . ?
N8 C22 C21 112.4(4) . . ?
N2 C6 C7 115.1(4) . . ?
C29 C28 C27 119.6(6) . . ?
C36 C35 C40 119.1(5) . . ?
C36 C35 N6 118.3(5) . . ?
C40 C35 N6 122.5(5) . . ?
N6 C33 C34 110.4(4) . . ?
C35 C40 C39 119.3(5) . . ?
N6 C32 C31 112.1(4) . . ?
N5 C31 C32 112.9(4) . . ?
N5 C34 C33 112.6(4) . . ?
C35 C36 C37 120.1(5) . . ?
C38 C39 C40 120.9(5) . . ?
C39 C38 C37 120.8(6) . . ?
C38 C37 C36 119.8(6) . . ?
C24 N7 C21 106.6(4) . . ?
C24 N7 C20 111.0(4) . . ?
C21 N7 C20 110.8(4) . . ?
C10 N3 C8 115.5(4) . . ?
C10 N3 C7 115.4(4) . . ?
C8 N3 C7 113.3(4) . . ?
C25 N8 C22 114.4(4) . . ?
C25 N8 C23 113.3(4) . . ?
C22 N8 C23 109.9(4) . . ?
C6 N2 C9 105.3(4) . . ?
C6 N2 C5 111.1(4) . . ?
C9 N2 C5 111.9(4) . . ?
C6 N2 Al1 117.7(3) . . ?
C9 N2 Al1 111.4(3) . . ?
C5 N2 Al1 99.6(3) . . ?
C34 N5 C31 108.2(4) . . ?
C34 N5 Al1 114.3(3) . . ?
C31 N5 Al1 110.4(3) . . ?
C35 N6 C32 115.3(4) . . ?
C35 N6 C33 113.7(4) . . ?
C32 N6 C33 110.9(4) . . ?
C16 N4 C19 106.3(4) . . ?
C16 N4 Al1 120.3(3) . . ?
C19 N4 Al1 133.3(3) . . ?
Cl1 C42 Cl2 117.8(7) . . ?
C4 N1 C1 105.6(4) . . ?
C4 N1 Al1 118.7(3) . . ?
C1 N1 Al1 135.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.74
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.068
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lobo26302
_database_code_depnum_ccdc_archive 'CCDC 1413585'
_audit_update_record             
;
2015-07-18 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H40 Al N3 O2'
_chemical_formula_weight         597.71

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   'P 21/c'
_symmetry_space_group_name_hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.9263(9)
_cell_length_b                   10.5378(12)
_cell_length_c                   33.586(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 85.067(7)
_cell_angle_gamma                90.00
_cell_volume                     3147.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      27.3392

_exptl_crystal_description       columnar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9684
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            45732
_diffrn_reflns_av_R_equivalents  0.1890
_diffrn_reflns_av_sigmaI/netI    0.1424
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         28.80
_reflns_number_total             8155
_reflns_number_gt                3419
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1030P)²+0.0000P] where P=(Fo²+2Fc²)/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       0.0026(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8155
_refine_ls_number_parameters     400
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1964
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.2450
_refine_ls_wR_factor_gt          0.1841
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.011
_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 0.05777(12) 0.11855(11) 0.89521(3) 0.0315(3) Uani 1 1 d . . .
C25 C -0.0662(4) -0.2462(3) 0.92812(10) 0.0300(8) Uani 1 1 d . . .
C21 C -0.2352(4) 0.1529(3) 0.99931(10) 0.0294(8) Uani 1 1 d . . .
C24 C -0.0550(4) -0.1064(4) 0.93238(10) 0.0306(8) Uani 1 1 d . . .
C23 C -0.1362(4) -0.0431(3) 0.96309(10) 0.0318(8) Uani 1 1 d . . .
H23 H -0.1928 -0.0909 0.9822 0.038 Uiso 1 1 calc R . .
C22 C -0.1382(4) 0.0894(3) 0.96707(10) 0.0288(8) Uani 1 1 d . . .
C9 C 0.3720(4) 0.1552(3) 0.78448(10) 0.0347(9) Uani 1 1 d . . .
H9A H 0.3762 0.2293 0.7673 0.042 Uiso 1 1 calc R . .
H9B H 0.4713 0.1420 0.7935 0.042 Uiso 1 1 calc R . .
C8 C 0.2598(4) 0.1780(3) 0.82035(10) 0.0312(8) Uani 1 1 d . . .
H8A H 0.2955 0.2484 0.8356 0.037 Uiso 1 1 calc R . .
H8B H 0.1649 0.2034 0.8108 0.037 Uiso 1 1 calc R . .
C18 C -0.4216(4) 0.2823(4) 1.05648(11) 0.0393(10) Uani 1 1 d . . .
H18 H -0.4842 0.3252 1.0755 0.047 Uiso 1 1 calc R . .
C26 C -0.1861(4) -0.3141(3) 0.94701(11) 0.0356(9) Uani 1 1 d . . .
H26 H -0.2584 -0.2714 0.9635 0.043 Uiso 1 1 calc R . .
C16 C -0.2167(4) 0.2834(4) 1.00550(11) 0.0361(9) Uani 1 1 d . . .
H16 H -0.1414 0.3274 0.9904 0.043 Uiso 1 1 calc R . .
C5 C 0.3661(4) 0.0423(4) 0.86987(11) 0.0350(9) Uani 1 1 d . . .
H5A H 0.3598 -0.0423 0.8813 0.042 Uiso 1 1 calc R . .
H5B H 0.4573 0.0479 0.8520 0.042 Uiso 1 1 calc R . .
C20 C -0.3478(4) 0.0890(4) 1.02231(10) 0.0327(9) Uani 1 1 d . . .
H20 H -0.3613 0.0023 1.0187 0.039 Uiso 1 1 calc R . .
C10 C 0.4056(4) 0.0245(3) 0.72371(10) 0.0325(9) Uani 1 1 d . . .
C4 C 0.3677(4) 0.1393(3) 0.90202(10) 0.0330(9) Uani 1 1 d . . .
C7 C 0.3073(4) -0.0675(3) 0.78756(10) 0.0344(9) Uani 1 1 d . . .
H7A H 0.4023 -0.0915 0.7974 0.041 Uiso 1 1 calc R . .
H7B H 0.2730 -0.1377 0.7720 0.041 Uiso 1 1 calc R . .
C30 C 0.0398(4) -0.3130(4) 0.90352(11) 0.0386(9) Uani 1 1 d . . .
H30 H 0.1203 -0.2699 0.8903 0.046 Uiso 1 1 calc R . .
C11 C 0.3598(5) -0.0726(4) 0.69923(11) 0.0428(10) Uani 1 1 d . . .
H11 H 0.2816 -0.1259 0.7087 0.051 Uiso 1 1 calc R . .
C3 C 0.4780(4) 0.1919(4) 0.92245(11) 0.0398(10) Uani 1 1 d . . .
H3 H 0.5807 0.1767 0.9181 0.048 Uiso 1 1 calc R . .
C15 C 0.5214(4) 0.1020(4) 0.70838(11) 0.0441(10) Uani 1 1 d . . .
H15 H 0.5538 0.1681 0.7239 0.053 Uiso 1 1 calc R . .
C6 C 0.1932(4) -0.0417(3) 0.82250(10) 0.0332(9) Uani 1 1 d . . .
H6A H 0.0963 -0.0259 0.8124 0.040 Uiso 1 1 calc R . .
H6B H 0.1835 -0.1169 0.8392 0.040 Uiso 1 1 calc R . .
C17 C -0.3094(4) 0.3470(4) 1.03386(11) 0.0385(9) Uani 1 1 d . . .
H17 H -0.2963 0.4335 1.0378 0.046 Uiso 1 1 calc R . .
C27 C -0.1997(5) -0.4424(4) 0.94172(12) 0.0460(11) Uani 1 1 d . . .
H27 H -0.2805 -0.4862 0.9546 0.055 Uiso 1 1 calc R . .
C19 C -0.4404(4) 0.1547(4) 1.05072(10) 0.0374(9) Uani 1 1 d . . .
H19 H -0.5159 0.1115 1.0660 0.045 Uiso 1 1 calc R . .
C13 C 0.5448(5) -0.0141(4) 0.64666(12) 0.0465(11) Uani 1 1 d . . .
H13 H 0.5922 -0.0275 0.6213 0.056 Uiso 1 1 calc R . .
C1 C 0.2557(4) 0.2688(4) 0.94657(11) 0.0379(9) Uani 1 1 d . . .
H1 H 0.1820 0.3148 0.9616 0.046 Uiso 1 1 calc R . .
C29 C 0.0269(5) -0.4421(4) 0.89856(13) 0.0482(11) Uani 1 1 d . . .
H29 H 0.0997 -0.4857 0.8825 0.058 Uiso 1 1 calc R . .
C28 C -0.0924(5) -0.5066(4) 0.91716(12) 0.0472(11) Uani 1 1 d . . .
H28 H -0.1014 -0.5936 0.9133 0.057 Uiso 1 1 calc R . .
C2 C 0.4067(4) 0.2737(4) 0.95134(11) 0.0408(10) Uani 1 1 d . . .
H2 H 0.4530 0.3218 0.9700 0.049 Uiso 1 1 calc R . .
C31 C -0.0805(4) 0.1930(4) 0.85871(11) 0.0430(10) Uani 1 1 d . . .
H31A H -0.0701 0.1488 0.8336 0.065 Uiso 1 1 calc R . .
H31B H -0.0565 0.2810 0.8544 0.065 Uiso 1 1 calc R . .
H31C H -0.1822 0.1854 0.8703 0.065 Uiso 1 1 calc R . .
C12 C 0.4287(5) -0.0910(4) 0.66120(12) 0.0454(10) Uani 1 1 d . . .
H12 H 0.3959 -0.1559 0.6453 0.055 Uiso 1 1 calc R . .
C14 C 0.5901(5) 0.0826(4) 0.67008(13) 0.0542(12) Uani 1 1 d . . .
H14 H 0.6676 0.1360 0.6603 0.065 Uiso 1 1 calc R . .
C34 C 0.0643(8) 0.4015(9) 0.7634(2) 0.114(3) Uani 1 1 d . . .
H34 H 0.0151 0.4250 0.7878 0.137 Uiso 1 1 calc R . .
C32 C 0.2387(6) 0.4452(6) 0.70824(18) 0.0721(15) Uani 1 1 d . . .
H32 H 0.3070 0.5061 0.6980 0.086 Uiso 1 1 calc R . .
C37 C 0.2172(7) 0.3356(8) 0.6870(2) 0.095(2) Uani 1 1 d . . .
C38 C 0.2893(8) 0.3106(9) 0.6517(2) 0.141(3) Uani 1 1 d . . .
H38A H 0.2705 0.3771 0.6332 0.211 Uiso 1 1 calc R . .
H38B H 0.2544 0.2313 0.6419 0.211 Uiso 1 1 calc R . .
H38C H 0.3953 0.3052 0.6544 0.211 Uiso 1 1 calc R . .
C36 C 0.1046(6) 0.2432(7) 0.7064(2) 0.092(2) Uani 1 1 d . . .
H36 H 0.0830 0.1660 0.6948 0.111 Uiso 1 1 calc R . .
C35 C 0.0381(7) 0.2808(6) 0.7416(2) 0.0849(18) Uani 1 1 d . . .
H35 H -0.0327 0.2255 0.7539 0.102 Uiso 1 1 calc R . .
C33 C 0.1594(9) 0.4639(10) 0.7443(3) 0.148(4) Uani 1 1 d . . .
H33 H 0.1829 0.5393 0.7568 0.178 Uiso 1 1 calc R . .
N2 N 0.2320(3) 0.0683(3) 0.84762(8) 0.0302(7) Uani 1 1 d . . .
N1 N 0.2292(3) 0.1860(3) 0.91629(8) 0.0317(7) Uani 1 1 d . . .
N3 N 0.3292(3) 0.0446(3) 0.76203(8) 0.0316(7) Uani 1 1 d . . .
O1 O -0.0625(3) 0.1619(2) 0.94270(7) 0.0352(6) Uani 1 1 d . . .
O2 O 0.0329(3) -0.0500(2) 0.90476(7) 0.0330(6) Uani 1 1 d . . .


_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 1.815(3) . ?
Al1 N1 1.880(3) . ?
Al1 O1 1.900(2) . ?
Al1 C31 1.975(4) . ?
Al1 N2 2.197(3) . ?
C25 C30 1.393(5) . ?
C25 C26 1.393(5) . ?
C25 C24 1.484(5) . ?
C21 C20 1.388(5) . ?
C21 C16 1.403(5) . ?
C21 C22 1.486(5) . ?
C24 O2 1.306(4) . ?
C24 C23 1.381(5) . ?
C23 C22 1.402(5) . ?
C22 O1 1.271(4) . ?
C9 N3 1.457(4) . ?
C9 C8 1.518(5) . ?
C8 N2 1.482(4) . ?
C18 C19 1.371(5) . ?
C18 C17 1.384(5) . ?
C26 C27 1.371(5) . ?
C16 C17 1.380(5) . ?
C5 C4 1.488(5) . ?
C5 N2 1.490(5) . ?
C20 C19 1.392(5) . ?
C10 C15 1.382(5) . ?
C10 C11 1.396(5) . ?
C10 N3 1.419(4) . ?
C4 C3 1.366(5) . ?
C4 N1 1.378(4) . ?
C7 N3 1.463(4) . ?
C7 C6 1.511(5) . ?
C30 C29 1.377(5) . ?
C11 C12 1.383(5) . ?
C3 C2 1.408(5) . ?
C15 C14 1.392(5) . ?
C6 N2 1.492(4) . ?
C27 C28 1.386(5) . ?
C13 C14 1.369(6) . ?
C13 C12 1.372(6) . ?
C1 C2 1.372(5) . ?
C1 N1 1.376(4) . ?
C29 C28 1.368(5) . ?
C34 C33 1.212(9) . ?
C34 C35 1.496(10) . ?
C32 C33 1.365(9) . ?
C32 C37 1.381(8) . ?
C37 C38 1.325(8) . ?
C37 C36 1.507(9) . ?
C36 C35 1.336(8) . ?

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 N1 113.24(13) . . ?
O2 Al1 O1 92.02(11) . . ?
N1 Al1 O1 90.71(12) . . ?
O2 Al1 C31 115.14(16) . . ?
N1 Al1 C31 130.99(16) . . ?
O1 Al1 C31 95.00(14) . . ?
O2 Al1 N2 87.77(11) . . ?
N1 Al1 N2 79.44(12) . . ?
O1 Al1 N2 169.16(12) . . ?
C31 Al1 N2 94.90(14) . . ?
C30 C25 C26 117.9(3) . . ?
C30 C25 C24 120.7(3) . . ?
C26 C25 C24 121.4(3) . . ?
C20 C21 C16 118.8(3) . . ?
C20 C21 C22 122.4(3) . . ?
C16 C21 C22 118.7(3) . . ?
O2 C24 C23 123.7(3) . . ?
O2 C24 C25 115.2(3) . . ?
C23 C24 C25 121.1(3) . . ?
C24 C23 C22 123.6(3) . . ?
O1 C22 C23 122.4(3) . . ?
O1 C22 C21 116.3(3) . . ?
C23 C22 C21 121.3(3) . . ?
N3 C9 C8 110.7(3) . . ?
N2 C8 C9 115.5(3) . . ?
C19 C18 C17 119.8(4) . . ?
C27 C26 C25 121.3(4) . . ?
C17 C16 C21 120.5(4) . . ?
C4 C5 N2 107.2(3) . . ?
C21 C20 C19 119.9(4) . . ?
C15 C10 C11 117.5(3) . . ?
C15 C10 N3 122.4(3) . . ?
C11 C10 N3 120.1(3) . . ?
C3 C4 N1 110.1(3) . . ?
C3 C4 C5 134.1(3) . . ?
N1 C4 C5 115.7(3) . . ?
N3 C7 C6 110.9(3) . . ?
C29 C30 C25 120.7(4) . . ?
C12 C11 C10 121.2(4) . . ?
C4 C3 C2 107.0(3) . . ?
C10 C15 C14 120.9(4) . . ?
N2 C6 C7 113.9(3) . . ?
C16 C17 C18 120.1(4) . . ?
C26 C27 C28 119.6(4) . . ?
C18 C19 C20 120.8(4) . . ?
C14 C13 C12 119.1(4) . . ?
C2 C1 N1 110.1(3) . . ?
C28 C29 C30 120.4(4) . . ?
C29 C28 C27 120.0(4) . . ?
C1 C2 C3 106.6(3) . . ?
C13 C12 C11 120.6(4) . . ?
C13 C14 C15 120.8(4) . . ?
C33 C34 C35 109.6(9) . . ?
C33 C32 C37 119.7(7) . . ?
C38 C37 C32 123.4(8) . . ?
C38 C37 C36 120.9(8) . . ?
C32 C37 C36 115.7(6) . . ?
C35 C36 C37 114.9(7) . . ?
C36 C35 C34 127.5(7) . . ?
C34 C33 C32 132.6(11) . . ?
C8 N2 C5 110.8(3) . . ?
C8 N2 C6 106.9(3) . . ?
C5 N2 C6 112.1(3) . . ?
C8 N2 Al1 109.4(2) . . ?
C5 N2 Al1 103.2(2) . . ?
C6 N2 Al1 114.5(2) . . ?
C1 N1 C4 106.1(3) . . ?
C1 N1 Al1 135.7(3) . . ?
C4 N1 Al1 118.0(2) . . ?
C10 N3 C9 117.5(3) . . ?
C10 N3 C7 116.2(3) . . ?
C9 N3 C7 111.7(3) . . ?
C22 O1 Al1 128.8(2) . . ?
C24 O2 Al1 128.9(2) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.80
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.073
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lobo3530201
_database_code_depnum_ccdc_archive 'CCDC 1413586'
_audit_update_record             
;
2015-07-18 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30.50 H38.50 Al N3 O1.50'
_chemical_formula_weight         498.12

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   'C 2/c'
_symmetry_space_group_name_hall  '-C 2yc'

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                   26.8669(10)
_cell_length_b                   12.1406(5)
_cell_length_c                   18.5317(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.230(2)
_cell_angle_gamma                90.00
_cell_volume                     5468.0(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      28.73

_exptl_crystal_description       columnar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2140
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9762
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            39369
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         28.76
_reflns_number_total             7081
_reflns_number_gt                3905
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 The AFIX 66 was applied to C10 to C15 to have contraint on benzene ring.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0869P)²+6.7312P] where P=(Fo²+2Fc²)/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         7081
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0698
_refine_ls_wR_factor_ref         0.2108
_refine_ls_wR_factor_gt          0.1730
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_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 0.74530(3) 0.77383(7) 0.58618(4) 0.0345(2) Uani 1 1 d . . .
C1 C 0.67790(13) 0.9861(3) 0.55425(19) 0.0535(8) Uani 1 1 d . . .
H1 H 0.6521 0.9782 0.5016 0.064 Uiso 1 1 calc R . .
C2 C 0.68265(15) 1.0757(3) 0.6010(2) 0.0628(9) Uani 1 1 d . . .
H2 H 0.6608 1.1385 0.5864 0.075 Uiso 1 1 calc R . .
C3 C 0.72677(15) 1.0555(3) 0.6754(2) 0.0598(9) Uani 1 1 d . . .
H3 H 0.7400 1.1025 0.7192 0.072 Uiso 1 1 calc R . .
C4 C 0.74647(12) 0.9535(3) 0.67093(17) 0.0455(7) Uani 1 1 d . . .
C5 C 0.79192(12) 0.8830(3) 0.72783(16) 0.0512(8) Uani 1 1 d . . .
H5A H 0.7779 0.8337 0.7560 0.061 Uiso 1 1 calc R . .
H5B H 0.8204 0.9286 0.7667 0.061 Uiso 1 1 calc R . .
C6 C 0.85074(12) 0.8920(3) 0.65783(18) 0.0502(7) Uani 1 1 d . . .
H6A H 0.8782 0.9256 0.7058 0.060 Uiso 1 1 calc R . .
H6B H 0.8283 0.9505 0.6239 0.060 Uiso 1 1 calc R . .
C7 C 0.87939(12) 0.8315(3) 0.61469(18) 0.0489(7) Uani 1 1 d . . .
H7A H 0.8521 0.8037 0.5642 0.059 Uiso 1 1 calc R . .
H7B H 0.9031 0.8822 0.6035 0.059 Uiso 1 1 calc R . .
C8 C 0.87832(13) 0.6661(3) 0.6856(2) 0.0570(9) Uani 1 1 d . . .
H8A H 0.9013 0.6079 0.7193 0.068 Uiso 1 1 calc R . .
H8B H 0.8504 0.6323 0.6382 0.068 Uiso 1 1 calc R . .
C9 C 0.85100(12) 0.7275(3) 0.72974(17) 0.0539(8) Uani 1 1 d . . .
H9A H 0.8291 0.6766 0.7445 0.065 Uiso 1 1 calc R . .
H9B H 0.8790 0.7585 0.7783 0.065 Uiso 1 1 calc R . .
C10 C 0.94850(9) 0.6884(2) 0.63393(14) 0.0522(8) Uani 1 1 d G . .
C11 C 0.97459(13) 0.75319(16) 0.5985(2) 0.111(2) Uani 1 1 d G . .
H11 H 0.9669 0.8281 0.5910 0.133 Uiso 1 1 calc R . .
C12 C 1.01213(12) 0.7060(2) 0.5743(2) 0.1080(19) Uani 1 1 d G . .
H12 H 1.0296 0.7493 0.5507 0.130 Uiso 1 1 calc R . .
C13 C 1.02357(10) 0.5940(2) 0.58554(16) 0.0730(11) Uani 1 1 d G . .
H13 H 1.0487 0.5624 0.5694 0.088 Uiso 1 1 calc R . .
C14 C 0.99749(13) 0.5292(2) 0.6209(2) 0.145(3) Uani 1 1 d G . .
H14 H 1.0051 0.4543 0.6284 0.174 Uiso 1 1 calc R . .
C15 C 0.95995(12) 0.5764(2) 0.6451(2) 0.141(3) Uani 1 1 d G . .
H15 H 0.9425 0.5331 0.6688 0.170 Uiso 1 1 calc R . .
C16 C 0.67925(11) 0.6023(2) 0.60891(16) 0.0415(6) Uani 1 1 d . . .
C17 C 0.67456(13) 0.5027(2) 0.56753(17) 0.0462(7) Uani 1 1 d . . .
C18 C 0.62746(15) 0.4406(3) 0.5484(2) 0.0608(9) Uani 1 1 d . . .
H18 H 0.6235 0.3746 0.5210 0.073 Uiso 1 1 calc R . .
C19 C 0.58608(15) 0.4742(3) 0.5690(2) 0.0671(10) Uani 1 1 d . . .
H19 H 0.5544 0.4319 0.5546 0.080 Uiso 1 1 calc R . .
C20 C 0.59194(13) 0.5698(3) 0.6107(2) 0.0608(9) Uani 1 1 d . . .
H20 H 0.5640 0.5918 0.6245 0.073 Uiso 1 1 calc R . .
C21 C 0.63871(12) 0.6351(3) 0.63312(18) 0.0470(7) Uani 1 1 d . . .
C22 C 0.72006(14) 0.4656(3) 0.54594(19) 0.0541(8) Uani 1 1 d . . .
H22 H 0.7318 0.5299 0.5252 0.065 Uiso 1 1 calc R . .
C23 C 0.77000(15) 0.4260(3) 0.6205(2) 0.0730(11) Uani 1 1 d . . .
H23A H 0.7809 0.4824 0.6605 0.110 Uiso 1 1 calc R . .
H23B H 0.7999 0.4103 0.6067 0.110 Uiso 1 1 calc R . .
H23C H 0.7604 0.3605 0.6407 0.110 Uiso 1 1 calc R . .
C24 C 0.70319(19) 0.3759(3) 0.4816(2) 0.0784(12) Uani 1 1 d . . .
H24A H 0.6959 0.3087 0.5025 0.118 Uiso 1 1 calc R . .
H24B H 0.7325 0.3642 0.4658 0.118 Uiso 1 1 calc R . .
H24C H 0.6707 0.3988 0.4362 0.118 Uiso 1 1 calc R . .
C25 C 0.64393(14) 0.7380(3) 0.6816(2) 0.0585(9) Uani 1 1 d . . .
H25 H 0.6807 0.7684 0.6958 0.070 Uiso 1 1 calc R . .
C26 C 0.60247(17) 0.8258(3) 0.6349(3) 0.0929(15) Uani 1 1 d . . .
H26A H 0.6065 0.8427 0.5870 0.139 Uiso 1 1 calc R . .
H26B H 0.6088 0.8910 0.6668 0.139 Uiso 1 1 calc R . .
H26C H 0.5659 0.7991 0.6212 0.139 Uiso 1 1 calc R . .
C27 C 0.63991(17) 0.7097(4) 0.7594(3) 0.0834(13) Uani 1 1 d . . .
H27A H 0.6059 0.6719 0.7475 0.125 Uiso 1 1 calc R . .
H27B H 0.6411 0.7762 0.7881 0.125 Uiso 1 1 calc R . .
H27C H 0.6702 0.6631 0.7914 0.125 Uiso 1 1 calc R . .
C29 C 1.0000 0.2659(5) 0.7500 0.0709(14) Uani 1 2 d S . .
H29 H 1.0000 0.3425 0.7500 0.085 Uiso 1 2 calc SR . .
C30 C 0.97302(15) 0.2110(3) 0.6790(2) 0.0685(10) Uani 1 1 d . . .
C31 C 0.97404(15) 0.0966(4) 0.6797(2) 0.0712(10) Uani 1 1 d . . .
H31 H 0.9569 0.0582 0.6319 0.085 Uiso 1 1 calc R . .
C32 C 1.0000 0.0390(5) 0.7500 0.0752(15) Uani 1 2 d S . .
H32 H 1.0000 -0.0377 0.7500 0.090 Uiso 1 2 calc SR . .
C33 C 0.9408(3) 0.2811(7) 0.6103(4) 0.080(2) Uani 0.50 1 d P . .
H33A H 0.9486 0.3571 0.6251 0.120 Uiso 0.50 1 calc PR . .
H33B H 0.9023 0.2674 0.5939 0.120 Uiso 0.50 1 calc PR . .
H33C H 0.9503 0.2645 0.5671 0.120 Uiso 0.50 1 calc PR . .
N2 N 0.81517(9) 0.8174(2) 0.67998(12) 0.0406(5) Uani 1 1 d . . .
N3 N 0.91209(10) 0.7401(2) 0.66251(14) 0.0512(7) Uani 1 1 d . . .
N1 N 0.71705(9) 0.90905(19) 0.59656(13) 0.0423(5) Uani 1 1 d . . .
O1 O 0.72493(7) 0.66616(16) 0.62762(11) 0.0417(5) Uani 1 1 d . . .
O2 O 0.7500 0.7500 0.5000 0.0415(6) Uani 1 2 d S . .


_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 1.6799(7) . ?
Al1 O1 1.7193(19) . ?
Al1 N1 1.853(2) . ?
Al1 N2 2.011(2) . ?
C1 C2 1.362(5) . ?
C1 N1 1.376(4) . ?
C2 C3 1.405(5) . ?
C3 C4 1.363(4) . ?
C4 N1 1.374(4) . ?
C4 C5 1.496(4) . ?
C5 N2 1.511(3) . ?
C6 N2 1.496(4) . ?
C6 C7 1.515(4) . ?
C7 N3 1.458(4) . ?
C8 N3 1.464(4) . ?
C8 C9 1.509(4) . ?
C9 N2 1.487(4) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C10 N3 1.440(3) . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C16 O1 1.365(3) . ?
C16 C21 1.401(4) . ?
C16 C17 1.409(4) . ?
C17 C18 1.384(5) . ?
C17 C22 1.508(4) . ?
C18 C19 1.383(5) . ?
C19 C20 1.366(5) . ?
C20 C21 1.391(4) . ?
C21 C25 1.510(4) . ?
C22 C24 1.533(5) . ?
C22 C23 1.536(5) . ?
C25 C26 1.518(5) . ?
C25 C27 1.531(5) . ?
C29 C30 1.374(5) 2_756 ?
C29 C30 1.374(5) . ?
C30 C31 1.390(6) . ?
C30 C33 1.467(9) . ?
C31 C32 1.378(5) . ?
C32 C31 1.378(5) 2_756 ?
O2 Al1 1.6799(7) 7_666 ?

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 117.44(8) . . ?
O2 Al1 N1 116.83(8) . . ?
O1 Al1 N1 113.88(10) . . ?
O2 Al1 N2 116.52(7) . . ?
O1 Al1 N2 99.87(10) . . ?
N1 Al1 N2 87.13(10) . . ?
C2 C1 N1 109.8(3) . . ?
C1 C2 C3 107.2(3) . . ?
C4 C3 C2 106.6(3) . . ?
C3 C4 N1 110.3(3) . . ?
C3 C4 C5 134.3(3) . . ?
N1 C4 C5 115.5(2) . . ?
C4 C5 N2 107.8(2) . . ?
N2 C6 C7 112.3(3) . . ?
N3 C7 C6 111.0(2) . . ?
N3 C8 C9 111.1(3) . . ?
N2 C9 C8 111.2(2) . . ?
C11 C10 C15 120.0 . . ?
C11 C10 N3 119.03(19) . . ?
C15 C10 N3 120.88(19) . . ?
C12 C11 C10 120.0 . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C14 120.0 . . ?
C13 C14 C15 120.0 . . ?
C14 C15 C10 120.0 . . ?
O1 C16 C21 119.7(3) . . ?
O1 C16 C17 119.2(2) . . ?
C21 C16 C17 121.1(3) . . ?
C18 C17 C16 117.9(3) . . ?
C18 C17 C22 121.7(3) . . ?
C16 C17 C22 120.4(3) . . ?
C19 C18 C17 121.6(3) . . ?
C20 C19 C18 119.7(3) . . ?
C19 C20 C21 121.6(3) . . ?
C20 C21 C16 118.0(3) . . ?
C20 C21 C25 119.4(3) . . ?
C16 C21 C25 122.5(3) . . ?
C17 C22 C24 114.5(3) . . ?
C17 C22 C23 110.6(2) . . ?
C24 C22 C23 109.4(3) . . ?
C21 C25 C26 112.5(3) . . ?
C21 C25 C27 110.4(3) . . ?
C26 C25 C27 111.5(3) . . ?
C30 C29 C30 122.0(6) 2_756 . ?
C29 C30 C31 118.4(4) . . ?
C29 C30 C33 115.2(5) . . ?
C31 C30 C33 126.1(5) . . ?
C32 C31 C30 121.1(4) . . ?
C31 C32 C31 119.0(6) 2_756 . ?
C9 N2 C6 107.1(2) . . ?
C9 N2 C5 110.1(2) . . ?
C6 N2 C5 108.3(2) . . ?
C9 N2 Al1 117.5(2) . . ?
C6 N2 Al1 113.10(17) . . ?
C5 N2 Al1 100.30(16) . . ?
C10 N3 C7 115.9(2) . . ?
C10 N3 C8 116.3(2) . . ?
C7 N3 C8 110.9(2) . . ?
C4 N1 C1 106.1(2) . . ?
C4 N1 Al1 111.49(19) . . ?
C1 N1 Al1 142.3(2) . . ?
C16 O1 Al1 137.80(17) . . ?
Al1 O2 Al1 179.998(2) 7_666 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.76
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.056

#===END

