# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

####################################################################### 
# 
# 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_Al2
_database_code_depnum_ccdc_archive 'CCDC 1037364'
_audit_update_record             
;
2014-12-03 deposited with the CCDC.
2015-01-06 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 H18 Al N O2'
_chemical_formula_weight         295.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P21/c

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                   11.55200(10)
_cell_length_b                   12.36600(10)
_cell_length_c                   22.1490(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.83
_cell_angle_gamma                90.00
_cell_volume                     3134.55(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    57236
_cell_measurement_theta_min      3.51
_cell_measurement_theta_max      25.03

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9366
_exptl_absorpt_correction_T_max  0.9488
_exptl_absorpt_process_details   'Sortav, Blessing 1995'

_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  'nonius kappa ccd'
_diffrn_measurement_method       ccd
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            60619
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.56
_diffrn_reflns_theta_max         27.49
_reflns_number_total             7141
_reflns_number_gt                5980
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_structure_solution    
;
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
 (1999) J. Appl. Cryst. 32, 115-119.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0532P)²+1.1433P] 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         7141
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.1063
_refine_ls_wR_factor_gt          0.0982
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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 0.33784(4) 0.25439(4) 0.72817(2) 0.03404(12) Uani 1 1 d . . .
O1 O 0.30332(8) 0.17519(7) 0.65865(4) 0.0296(2) Uani 1 1 d . . .
N1 N 0.11938(10) 0.28281(9) 0.59362(5) 0.0283(2) Uani 1 1 d . . .
C1 C 0.41070(17) 0.16923(17) 0.79669(9) 0.0548(5) Uani 1 1 d . . .
H1A H 0.3646 0.1037 0.8005 0.082 Uiso 1 1 calc R . .
H1B H 0.4143 0.2120 0.8342 0.082 Uiso 1 1 calc R . .
H1C H 0.4900 0.1491 0.7899 0.082 Uiso 1 1 calc R . .
Al2 Al 0.13152(3) 0.15714(3) 0.654002(17) 0.02325(10) Uani 1 1 d . . .
O2 O -0.02264(8) 0.16757(7) 0.66040(4) 0.02546(19) Uani 1 1 d . . .
N2 N 0.14748(10) 0.03683(9) 0.71521(5) 0.0251(2) Uani 1 1 d . . .
C2 C 0.40103(18) 0.39802(15) 0.71530(10) 0.0582(5) Uani 1 1 d . . .
H2A H 0.4378 0.3978 0.6780 0.087 Uiso 1 1 calc R . .
H2B H 0.4593 0.4170 0.7501 0.087 Uiso 1 1 calc R . .
H2C H 0.3376 0.4513 0.7114 0.087 Uiso 1 1 calc R . .
O3 O 0.17781(8) 0.25070(7) 0.72388(4) 0.0284(2) Uani 1 1 d . . .
C3 C 0.35748(12) 0.17386(11) 0.60687(7) 0.0314(3) Uani 1 1 d . . .
O4 O 0.13157(8) 0.06171(7) 0.59258(4) 0.02462(19) Uani 1 1 d . . .
C4 C 0.45073(13) 0.10466(13) 0.60283(8) 0.0384(3) Uani 1 1 d . . .
H4 H 0.4781 0.0578 0.6357 0.046 Uiso 1 1 calc R . .
C5 C 0.50346(14) 0.10496(14) 0.54999(9) 0.0463(4) Uani 1 1 d . . .
H5 H 0.5693 0.0601 0.5473 0.056 Uiso 1 1 calc R . .
C6 C 0.46076(15) 0.17011(15) 0.50130(9) 0.0483(4) Uani 1 1 d . . .
H6 H 0.4960 0.1685 0.4650 0.058 Uiso 1 1 calc R . .
C7 C 0.36673(15) 0.23755(14) 0.50553(8) 0.0438(4) Uani 1 1 d . . .
H7 H 0.3371 0.2816 0.4718 0.053 Uiso 1 1 calc R . .
C8 C 0.31485(13) 0.24161(12) 0.55894(7) 0.0355(3) Uani 1 1 d . . .
C9 C 0.22213(14) 0.32397(13) 0.56680(8) 0.0413(4) Uani 1 1 d . . .
H9A H 0.2585 0.3829 0.5931 0.050 Uiso 1 1 calc R . .
H9B H 0.1940 0.3557 0.5264 0.050 Uiso 1 1 calc R . .
C10 C 0.02474(12) 0.33668(11) 0.57787(6) 0.0293(3) Uani 1 1 d . . .
H10 H 0.0285 0.3925 0.5487 0.035 Uiso 1 1 calc R . .
C11 C -0.08601(12) 0.32180(10) 0.59951(6) 0.0263(3) Uani 1 1 d . . .
C12 C -0.10457(11) 0.23793(10) 0.64023(6) 0.0242(3) Uani 1 1 d . . .
C13 C -0.21682(12) 0.22841(11) 0.65887(6) 0.0279(3) Uani 1 1 d . . .
C14 C -0.30380(12) 0.30018(11) 0.63630(6) 0.0313(3) Uani 1 1 d . . .
H14 H -0.3786 0.2925 0.6490 0.038 Uiso 1 1 calc R . .
C15 C -0.28724(13) 0.38386(11) 0.59550(6) 0.0319(3) Uani 1 1 d . . .
C16 C -0.17790(13) 0.39328(11) 0.57794(6) 0.0302(3) Uani 1 1 d . . .
H16 H -0.1638 0.4494 0.5506 0.036 Uiso 1 1 calc R . .
C17 C -0.23915(13) 0.13832(13) 0.70146(7) 0.0372(3) Uani 1 1 d . . .
H17A H -0.3169 0.1472 0.7138 0.056 Uiso 1 1 calc R . .
H17B H -0.1800 0.1404 0.7376 0.056 Uiso 1 1 calc R . .
H17C H -0.2351 0.0687 0.6807 0.056 Uiso 1 1 calc R . .
C18 C -0.38695(14) 0.45818(14) 0.57161(8) 0.0431(4) Uani 1 1 d . . .
H18A H -0.3606 0.5095 0.5426 0.065 Uiso 1 1 calc R . .
H18B H -0.4128 0.4980 0.6056 0.065 Uiso 1 1 calc R . .
H18C H -0.4521 0.4153 0.5511 0.065 Uiso 1 1 calc R . .
C19 C 0.12522(12) 0.25019(11) 0.77641(6) 0.0285(3) Uani 1 1 d . . .
C20 C 0.11095(13) 0.34892(12) 0.80450(7) 0.0365(3) Uani 1 1 d . . .
H20 H 0.1350 0.4138 0.7869 0.044 Uiso 1 1 calc R . .
C21 C 0.06174(14) 0.35295(14) 0.85818(7) 0.0431(4) Uani 1 1 d . . .
H21 H 0.0522 0.4204 0.8774 0.052 Uiso 1 1 calc R . .
C22 C 0.02665(15) 0.25851(14) 0.88361(7) 0.0429(4) Uani 1 1 d . . .
H22 H -0.0067 0.2607 0.9205 0.052 Uiso 1 1 calc R . .
C23 C 0.04038(13) 0.16049(13) 0.85510(6) 0.0365(3) Uani 1 1 d . . .
H23 H 0.0152 0.0960 0.8726 0.044 Uiso 1 1 calc R . .
C24 C 0.09055(12) 0.15431(11) 0.80100(6) 0.0294(3) Uani 1 1 d . . .
C25 C 0.10272(15) 0.04331(12) 0.77452(6) 0.0366(3) Uani 1 1 d . . .
H25A H 0.1553 0.0004 0.8044 0.044 Uiso 1 1 calc R . .
H25B H 0.0251 0.0081 0.7700 0.044 Uiso 1 1 calc R . .
C26 C 0.19411(12) -0.05518(10) 0.70454(6) 0.0266(3) Uani 1 1 d . . .
H26 H 0.2107 -0.1035 0.7379 0.032 Uiso 1 1 calc R . .
C27 C 0.22306(11) -0.09068(10) 0.64651(6) 0.0251(3) Uani 1 1 d . . .
C28 C 0.27305(12) -0.19436(11) 0.64348(6) 0.0293(3) Uani 1 1 d . . .
H28 H 0.2975 -0.2326 0.6802 0.035 Uiso 1 1 calc R . .
C29 C 0.28734(12) -0.24147(11) 0.58875(6) 0.0298(3) Uani 1 1 d . . .
C30 C 0.25194(11) -0.18111(11) 0.53554(6) 0.0279(3) Uani 1 1 d . . .
H30 H 0.2626 -0.2118 0.4974 0.034 Uiso 1 1 calc R . .
C31 C 0.20253(11) -0.07957(11) 0.53603(6) 0.0249(3) Uani 1 1 d . . .
C32 C 0.18547(11) -0.03275(10) 0.59244(6) 0.0230(2) Uani 1 1 d . . .
C33 C 0.33456(16) -0.35463(13) 0.58461(7) 0.0422(4) Uani 1 1 d . . .
H33A H 0.3510 -0.3857 0.6256 0.063 Uiso 1 1 calc R . .
H33B H 0.4067 -0.3523 0.5660 0.063 Uiso 1 1 calc R . .
H33C H 0.2766 -0.3994 0.5596 0.063 Uiso 1 1 calc R . .
C34 C 0.16453(12) -0.01823(12) 0.47808(6) 0.0307(3) Uani 1 1 d . . .
H34A H 0.1907 -0.0567 0.4437 0.046 Uiso 1 1 calc R . .
H34B H 0.1990 0.0543 0.4812 0.046 Uiso 1 1 calc R . .
H34C H 0.0791 -0.0123 0.4716 0.046 Uiso 1 1 calc R . .


_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 1.8227(10) . ?
Al1 O3 1.8387(10) . ?
Al1 C1 1.9423(19) . ?
Al1 C2 1.9559(18) . ?
Al1 Al2 2.9596(6) . ?
O1 C3 1.3793(16) . ?
O1 Al2 1.9858(10) . ?
N1 C10 1.2872(18) . ?
N1 C9 1.4877(18) . ?
N1 Al2 2.0426(12) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Al2 O4 1.8010(9) . ?
Al2 O2 1.8102(10) . ?
Al2 O3 1.9480(10) . ?
Al2 N2 2.0043(11) . ?
O2 C12 1.3180(15) . ?
N2 C26 1.2943(17) . ?
N2 C25 1.4781(16) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C19 1.3838(16) . ?
C3 C4 1.388(2) . ?
C3 C8 1.389(2) . ?
O4 C32 1.3239(15) . ?
C4 C5 1.391(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.398(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.505(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.4378(19) . ?
C10 H10 0.9500 . ?
C11 C12 1.4098(18) . ?
C11 C16 1.4136(18) . ?
C12 C13 1.4183(18) . ?
C13 C14 1.3822(19) . ?
C13 C17 1.505(2) . ?
C14 C15 1.404(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(2) . ?
C15 C18 1.5117(19) . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C24 1.386(2) . ?
C19 C20 1.3903(19) . ?
C20 C21 1.387(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.381(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.4023(19) . ?
C23 H23 0.9500 . ?
C24 C25 1.5068(19) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.4400(17) . ?
C26 H26 0.9500 . ?
C27 C28 1.4114(18) . ?
C27 C32 1.4123(17) . ?
C28 C29 1.3751(19) . ?
C28 H28 0.9500 . ?
C29 C30 1.4079(19) . ?
C29 C33 1.5092(19) . ?
C30 C31 1.3800(18) . ?
C30 H30 0.9500 . ?
C31 C32 1.4148(17) . ?
C31 C34 1.5040(18) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

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 O3 80.81(4) . . ?
O1 Al1 C1 112.98(7) . . ?
O3 Al1 C1 110.64(7) . . ?
O1 Al1 C2 114.07(7) . . ?
O3 Al1 C2 114.05(7) . . ?
C1 Al1 C2 118.39(10) . . ?
O1 Al1 Al2 41.04(3) . . ?
O3 Al1 Al2 39.94(3) . . ?
C1 Al1 Al2 116.35(7) . . ?
C2 Al1 Al2 125.20(7) . . ?
C3 O1 Al1 129.57(8) . . ?
C3 O1 Al2 121.26(8) . . ?
Al1 O1 Al2 101.90(5) . . ?
C10 N1 C9 114.15(12) . . ?
C10 N1 Al2 123.45(9) . . ?
C9 N1 Al2 122.30(9) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O4 Al2 O2 101.97(4) . . ?
O4 Al2 O3 163.96(5) . . ?
O2 Al2 O3 93.56(4) . . ?
O4 Al2 O1 90.55(4) . . ?
O2 Al2 O1 167.12(4) . . ?
O3 Al2 O1 74.21(4) . . ?
O4 Al2 N2 90.87(4) . . ?
O2 Al2 N2 90.05(4) . . ?
O3 Al2 N2 85.03(4) . . ?
O1 Al2 N2 92.82(4) . . ?
O4 Al2 N1 90.63(4) . . ?
O2 Al2 N1 90.94(4) . . ?
O3 Al2 N1 93.17(5) . . ?
O1 Al2 N1 85.84(4) . . ?
N2 Al2 N1 178.00(5) . . ?
O4 Al2 Al1 127.04(3) . . ?
O2 Al2 Al1 130.85(3) . . ?
O3 Al2 Al1 37.29(3) . . ?
O1 Al2 Al1 37.06(3) . . ?
N2 Al2 Al1 86.17(3) . . ?
N1 Al2 Al1 91.87(4) . . ?
C12 O2 Al2 133.57(9) . . ?
C26 N2 C25 114.50(11) . . ?
C26 N2 Al2 122.09(9) . . ?
C25 N2 Al2 123.35(9) . . ?
Al1 C2 H2A 109.5 . . ?
Al1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Al1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C19 O3 Al1 120.67(8) . . ?
C19 O3 Al2 124.11(8) . . ?
Al1 O3 Al2 102.77(5) . . ?
O1 C3 C4 120.31(14) . . ?
O1 C3 C8 118.33(12) . . ?
C4 C3 C8 121.34(14) . . ?
C32 O4 Al2 128.94(8) . . ?
C3 C4 C5 119.02(16) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 120.49(15) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 119.92(15) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C8 120.69(17) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C3 C8 C7 118.48(14) . . ?
C3 C8 C9 120.24(14) . . ?
C7 C8 C9 121.06(15) . . ?
N1 C9 C8 115.70(12) . . ?
N1 C9 H9A 108.4 . . ?
C8 C9 H9A 108.4 . . ?
N1 C9 H9B 108.4 . . ?
C8 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
N1 C10 C11 127.22(12) . . ?
N1 C10 H10 116.4 . . ?
C11 C10 H10 116.4 . . ?
C12 C11 C16 120.24(12) . . ?
C12 C11 C10 121.81(12) . . ?
C16 C11 C10 117.94(12) . . ?
O2 C12 C11 122.52(12) . . ?
O2 C12 C13 119.30(12) . . ?
C11 C12 C13 118.17(12) . . ?
C14 C13 C12 119.33(13) . . ?
C14 C13 C17 121.60(13) . . ?
C12 C13 C17 119.05(12) . . ?
C13 C14 C15 123.37(13) . . ?
C13 C14 H14 118.3 . . ?
C15 C14 H14 118.3 . . ?
C16 C15 C14 117.06(13) . . ?
C16 C15 C18 122.31(14) . . ?
C14 C15 C18 120.62(14) . . ?
C15 C16 C11 121.83(13) . . ?
C15 C16 H16 119.1 . . ?
C11 C16 H16 119.1 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O3 C19 C24 121.17(11) . . ?
O3 C19 C20 117.69(13) . . ?
C24 C19 C20 121.12(13) . . ?
C21 C20 C19 120.18(15) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 119.78(14) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 119.70(14) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C22 C23 C24 121.55(15) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C19 C24 C23 117.66(13) . . ?
C19 C24 C25 125.37(12) . . ?
C23 C24 C25 116.97(13) . . ?
N2 C25 C24 117.25(12) . . ?
N2 C25 H25A 108.0 . . ?
C24 C25 H25A 108.0 . . ?
N2 C25 H25B 108.0 . . ?
C24 C25 H25B 108.0 . . ?
H25A C25 H25B 107.2 . . ?
N2 C26 C27 125.73(12) . . ?
N2 C26 H26 117.1 . . ?
C27 C26 H26 117.1 . . ?
C28 C27 C32 120.07(11) . . ?
C28 C27 C26 117.75(12) . . ?
C32 C27 C26 121.35(11) . . ?
C29 C28 C27 121.72(12) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C28 C29 C30 117.21(12) . . ?
C28 C29 C33 122.29(13) . . ?
C30 C29 C33 120.46(12) . . ?
C31 C30 C29 123.31(12) . . ?
C31 C30 H30 118.3 . . ?
C29 C30 H30 118.3 . . ?
C30 C31 C32 119.13(12) . . ?
C30 C31 C34 121.67(12) . . ?
C32 C31 C34 119.18(11) . . ?
O4 C32 C27 122.41(11) . . ?
O4 C32 C31 119.03(11) . . ?
C27 C32 C31 118.52(11) . . ?
C29 C33 H33A 109.5 . . ?
C29 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C29 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.060
####################################################################### 
# 
# 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_Al4
_database_code_depnum_ccdc_archive 'CCDC 1037365'
_audit_update_record             
;
2014-12-03 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C102 H95 Al4 Cl8 N4 O8'
_chemical_formula_weight         1896.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
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   Pbn21

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'

_cell_length_a                   12.0601(2)
_cell_length_b                   22.5938(3)
_cell_length_c                   35.5013(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9673.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    103792
_cell_measurement_theta_min      3.51
_cell_measurement_theta_max      25.03

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3948
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'nonius kappa ccd'
_diffrn_measurement_method       ccd
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            77915
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         25.02
_reflns_number_total             16713
_reflns_number_gt                11894
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_structure_solution    
;
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
 (1999) J. Appl. Cryst. 32, 115-119.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0838P)²+14.2157P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.25(7)
_refine_ls_number_reflns         16713
_refine_ls_number_parameters     1014
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0756
_refine_ls_wR_factor_ref         0.1950
_refine_ls_wR_factor_gt          0.1719
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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
Cl1 Cl -0.51474(13) 0.95692(7) 0.85588(5) 0.0522(4) Uani 1 1 d . . .
Al1 Al -0.16921(14) 0.89288(7) 0.89207(5) 0.0354(4) Uani 1 1 d . . .
O1 O -0.3107(3) 0.91632(16) 0.89030(11) 0.0341(9) Uani 1 1 d . . .
N1 N -0.1935(4) 0.8611(2) 0.94404(15) 0.0444(13) Uani 1 1 d . . .
C1 C -0.1250(6) 0.8158(3) 0.8703(2) 0.0518(17) Uani 1 1 d . . .
H1A H -0.1875 0.7989 0.8563 0.078 Uiso 1 1 calc R . .
H1B H -0.1036 0.7887 0.8906 0.078 Uiso 1 1 calc R . .
H1C H -0.0621 0.8216 0.8532 0.078 Uiso 1 1 calc R . .
Cl2 Cl -0.71105(19) 0.84868(14) 0.97328(8) 0.1084(9) Uani 1 1 d . . .
Al2 Al -0.01428(14) 0.99007(7) 0.86898(5) 0.0351(4) Uani 1 1 d . . .
O2 O -0.0699(3) 0.94577(16) 0.91321(11) 0.0361(9) Uani 1 1 d . . .
N2 N 0.0062(4) 1.02440(19) 0.81808(13) 0.0334(11) Uani 1 1 d . . .
C2 C 0.1381(5) 0.9624(3) 0.87540(19) 0.0475(16) Uani 1 1 d . . .
H2A H 0.1872 0.9846 0.8585 0.071 Uiso 1 1 calc R . .
H2B H 0.1422 0.9202 0.8693 0.071 Uiso 1 1 calc R . .
H2C H 0.1613 0.9686 0.9016 0.071 Uiso 1 1 calc R . .
Cl3 Cl -0.1397(2) 1.14984(8) 0.93855(5) 0.0747(6) Uani 1 1 d . . .
Al3 Al 0.19407(14) 0.87472(8) 0.64748(5) 0.0390(4) Uani 1 1 d . . .
O3 O -0.0630(3) 1.05942(15) 0.88590(11) 0.0380(9) Uani 1 1 d . . .
N3 N 0.0164(4) 0.7452(2) 0.72354(14) 0.0374(11) Uani 1 1 d . . .
C3 C -0.1136(5) 0.8031(3) 0.66547(19) 0.0494(17) Uani 1 1 d . . .
H3A H -0.1624 0.7694 0.6706 0.074 Uiso 1 1 calc R . .
H3B H -0.1246 0.8165 0.6395 0.074 Uiso 1 1 calc R . .
H3C H -0.1311 0.8355 0.6828 0.074 Uiso 1 1 calc R . .
Cl4 Cl -0.02149(16) 1.30323(7) 0.83060(7) 0.0661(5) Uani 1 1 d . . .
Al4 Al 0.04152(15) 0.77898(8) 0.67245(5) 0.0379(4) Uani 1 1 d . . .
O4 O -0.1215(3) 0.94018(16) 0.84905(11) 0.0380(9) Uani 1 1 d . . .
N4 N 0.2253(4) 0.9002(2) 0.59484(15) 0.0448(13) Uani 1 1 d . . .
C4 C 0.1438(6) 0.9521(3) 0.6658(2) 0.0598(19) Uani 1 1 d . . .
H4A H 0.1621 0.9561 0.6926 0.090 Uiso 1 1 calc R . .
H4B H 0.0634 0.9554 0.6624 0.090 Uiso 1 1 calc R . .
H4C H 0.1809 0.9836 0.6515 0.090 Uiso 1 1 calc R . .
Cl5 Cl 0.53481(14) 0.81124(8) 0.69028(6) 0.0602(5) Uani 1 1 d . . .
O5 O 0.0975(4) 0.71045(18) 0.65721(12) 0.0463(11) Uani 1 1 d . . .
C5 C -0.5046(5) 0.9160(3) 0.89708(19) 0.0450(16) Uani 1 1 d . . .
Cl6 Cl 0.74428(17) 0.88629(13) 0.56541(8) 0.0965(8) Uani 1 1 d . . .
O6 O 0.1441(3) 0.83089(17) 0.69199(11) 0.0389(9) Uani 1 1 d . . .
C6 C -0.5985(5) 0.9008(3) 0.9160(2) 0.0547(18) Uani 1 1 d . . .
H6 H -0.6692 0.9126 0.9069 0.066 Uiso 1 1 calc R . .
Cl7 Cl 0.1901(2) 0.62077(11) 0.60784(7) 0.0940(8) Uani 1 1 d . . .
O7 O 0.3327(3) 0.85049(17) 0.65165(12) 0.0396(10) Uani 1 1 d . . .
C7 C -0.5896(6) 0.8678(4) 0.9488(2) 0.065(2) Uani 1 1 d . . .
Cl8 Cl -0.00217(17) 0.46685(8) 0.70366(8) 0.0836(7) Uani 1 1 d . . .
O8 O 0.0962(3) 0.82031(19) 0.62774(11) 0.0417(10) Uani 1 1 d . . .
C8 C -0.4891(6) 0.8501(4) 0.9624(2) 0.062(2) Uani 1 1 d . . .
H8 H -0.4849 0.8268 0.9846 0.074 Uiso 1 1 calc R . .
C9 C -0.3913(5) 0.8668(3) 0.94321(19) 0.0451(15) Uani 1 1 d . . .
C10 C -0.3987(5) 0.9016(3) 0.90946(18) 0.0387(14) Uani 1 1 d . . .
C11 C -0.2881(5) 0.8499(3) 0.95909(19) 0.0452(16) Uani 1 1 d . . .
H11 H -0.2889 0.8291 0.9823 0.054 Uiso 1 1 calc R . .
C12 C -0.0904(6) 0.8462(3) 0.9644(2) 0.0542(18) Uani 1 1 d . . .
H12A H -0.0422 0.8212 0.9484 0.065 Uiso 1 1 calc R . .
H12B H -0.1080 0.8241 0.9877 0.065 Uiso 1 1 calc R . .
C13 C -0.0320(5) 0.9031(3) 0.97397(19) 0.0482(16) Uani 1 1 d . . .
C14 C 0.0161(6) 0.9096(4) 1.0100(2) 0.0586(19) Uani 1 1 d . . .
H14 H 0.0104 0.8782 1.0277 0.070 Uiso 1 1 calc R . .
C15 C 0.0713(6) 0.9608(4) 1.0202(2) 0.061(2) Uani 1 1 d . . .
H15 H 0.1059 0.9640 1.0441 0.074 Uiso 1 1 calc R . .
C16 C 0.0753(6) 1.0066(3) 0.99516(19) 0.0527(17) Uani 1 1 d . . .
H16 H 0.1118 1.0422 1.0023 0.063 Uiso 1 1 calc R . .
C18 C -0.0272(5) 0.9504(3) 0.94915(17) 0.0423(15) Uani 1 1 d . . .
C19 C -0.0536(5) 1.1143(2) 0.87223(17) 0.0364(13) Uani 1 1 d . . .
C20 C -0.0869(5) 1.1628(3) 0.89412(18) 0.0457(15) Uani 1 1 d . . .
C21 C -0.0770(5) 1.2198(3) 0.8817(2) 0.0487(17) Uani 1 1 d . . .
H21 H -0.0991 1.2517 0.8975 0.058 Uiso 1 1 calc R . .
C22 C -0.0348(5) 1.2309(3) 0.84625(19) 0.0441(16) Uani 1 1 d . . .
C23 C -0.0058(5) 1.1850(3) 0.82318(19) 0.0438(15) Uani 1 1 d . . .
H23 H 0.0211 1.1927 0.7985 0.053 Uiso 1 1 calc R . .
C24 C -0.0156(4) 1.1258(2) 0.83595(17) 0.0353(13) Uani 1 1 d . . .
C25 C 0.0094(5) 1.0798(2) 0.80963(17) 0.0363(13) Uani 1 1 d . . .
H25 H 0.0293 1.0906 0.7847 0.044 Uiso 1 1 calc R . .
C26 C 0.0207(5) 0.9795(3) 0.78826(19) 0.0427(15) Uani 1 1 d . . .
H26A H 0.0770 0.9500 0.7961 0.051 Uiso 1 1 calc R . .
H26B H 0.0465 0.9986 0.7647 0.051 Uiso 1 1 calc R . .
C27 C -0.0886(5) 0.9495(2) 0.78170(17) 0.0383(14) Uani 1 1 d . . .
C28 C -0.1561(5) 0.9317(3) 0.81177(16) 0.0391(14) Uani 1 1 d . . .
C29 C -0.2565(5) 0.9050(3) 0.80490(17) 0.0443(15) Uani 1 1 d . . .
H29 H -0.3017 0.8929 0.8254 0.053 Uiso 1 1 calc R . .
C30 C -0.2924(6) 0.8956(3) 0.7684(2) 0.0510(17) Uani 1 1 d . . .
H30 H -0.3626 0.8777 0.7641 0.061 Uiso 1 1 calc R . .
C31 C -0.2270(6) 0.9119(3) 0.7385(2) 0.0502(17) Uani 1 1 d . . .
H31 H -0.2507 0.9044 0.7135 0.060 Uiso 1 1 calc R . .
C32 C -0.1271(6) 0.9392(3) 0.74509(19) 0.0475(16) Uani 1 1 d . . .
H32 H -0.0832 0.9515 0.7243 0.057 Uiso 1 1 calc R . .
C33 C 0.0772(5) 0.6556(3) 0.66934(19) 0.0451(15) Uani 1 1 d . . .
C34 C 0.1108(6) 0.6072(3) 0.6477(2) 0.0595(19) Uani 1 1 d . . .
C35 C 0.0860(6) 0.5489(3) 0.6577(2) 0.060(2) Uani 1 1 d . . .
H35 H 0.1075 0.5166 0.6422 0.072 Uiso 1 1 calc R . .
C36 C 0.0292(5) 0.5398(3) 0.6908(2) 0.0533(18) Uani 1 1 d . . .
C37 C 0.0001(5) 0.5845(3) 0.7142(2) 0.0486(17) Uani 1 1 d . . .
H37 H -0.0367 0.5762 0.7372 0.058 Uiso 1 1 calc R . .
C38 C 0.0246(5) 0.6438(2) 0.70417(18) 0.0388(14) Uani 1 1 d . . .
C39 C 0.0027(5) 0.6898(3) 0.73096(18) 0.0401(14) Uani 1 1 d . . .
H39 H -0.0230 0.6790 0.7553 0.048 Uiso 1 1 calc R . .
C40 C 0.0021(5) 0.7893(3) 0.75305(18) 0.0421(15) Uani 1 1 d . . .
H40A H -0.0215 0.7698 0.7767 0.051 Uiso 1 1 calc R . .
H40B H -0.0559 0.8180 0.7456 0.051 Uiso 1 1 calc R . .
C41 C 0.1116(5) 0.8211(3) 0.75906(18) 0.0408(14) Uani 1 1 d . . .
C42 C 0.1484(6) 0.8310(3) 0.79518(18) 0.0458(16) Uani 1 1 d . . .
H42 H 0.1042 0.8181 0.8158 0.055 Uiso 1 1 calc R . .
C43 C 0.2487(6) 0.8592(3) 0.80237(19) 0.0537(18) Uani 1 1 d . . .
H43 H 0.2727 0.8656 0.8275 0.064 Uiso 1 1 calc R . .
C44 C 0.3126(6) 0.8778(3) 0.77250(19) 0.0531(18) Uani 1 1 d . . .
H44 H 0.3812 0.8972 0.7770 0.064 Uiso 1 1 calc R . .
C45 C 0.2766(6) 0.8683(3) 0.7357(2) 0.0498(17) Uani 1 1 d . . .
H45 H 0.3207 0.8813 0.7152 0.060 Uiso 1 1 calc R . .
C46 C 0.1771(5) 0.8400(3) 0.72898(17) 0.0384(14) Uani 1 1 d . . .
C47 C 0.4230(5) 0.8606(3) 0.63162(17) 0.0387(14) Uani 1 1 d . . .
C48 C 0.5287(5) 0.8432(3) 0.6459(2) 0.0483(16) Uani 1 1 d . . .
C49 C 0.6241(5) 0.8529(3) 0.6260(2) 0.0538(18) Uani 1 1 d . . .
H49 H 0.6936 0.8421 0.6366 0.065 Uiso 1 1 calc R . .
C50 C 0.6201(6) 0.8780(3) 0.5910(2) 0.062(2) Uani 1 1 d . . .
C51 C 0.5214(6) 0.8949(3) 0.5752(2) 0.0604(19) Uani 1 1 d . . .
H51 H 0.5194 0.9119 0.5507 0.072 Uiso 1 1 calc R . .
C52 C 0.4222(5) 0.8866(3) 0.5960(2) 0.0468(16) Uani 1 1 d . . .
C53 C 0.3188(5) 0.9033(3) 0.5785(2) 0.0471(16) Uani 1 1 d . . .
H53 H 0.3208 0.9174 0.5533 0.056 Uiso 1 1 calc R . .
C54 C 0.1234(5) 0.9138(3) 0.57326(19) 0.0515(17) Uani 1 1 d . . .
H54A H 0.1428 0.9343 0.5495 0.062 Uiso 1 1 calc R . .
H54B H 0.0747 0.9401 0.5882 0.062 Uiso 1 1 calc R . .
C55 C 0.0640(5) 0.8569(3) 0.56463(17) 0.0429(15) Uani 1 1 d . . .
C56 C 0.0540(5) 0.8123(3) 0.59142(18) 0.0438(15) Uani 1 1 d . . .
C57 C 0.0016(5) 0.7598(3) 0.5829(2) 0.0525(17) Uani 1 1 d . . .
H57 H -0.0042 0.7293 0.6013 0.063 Uiso 1 1 calc R . .
C58 C -0.0425(6) 0.7519(4) 0.5474(2) 0.0593(19) Uani 1 1 d . . .
H58 H -0.0790 0.7159 0.5412 0.071 Uiso 1 1 calc R . .
C59 C -0.0337(6) 0.7966(4) 0.5205(2) 0.064(2) Uani 1 1 d . . .
H59 H -0.0651 0.7914 0.4961 0.076 Uiso 1 1 calc R . .
C60 C 0.0196(6) 0.8473(4) 0.5291(2) 0.060(2) Uani 1 1 d . . .
H60 H 0.0270 0.8772 0.5104 0.072 Uiso 1 1 calc R . .
C61 C 0.0278(5) 1.0028(3) 0.95970(19) 0.0458(16) Uani 1 1 d . . .
C100 C 0.595(2) 0.7925(10) 0.4957(8) 0.37(2) Uani 1 1 d . . .
H10A H 0.6035 0.7687 0.4728 0.552 Uiso 1 1 calc R . .
H10B H 0.6519 0.7808 0.5140 0.552 Uiso 1 1 calc R . .
H10C H 0.6042 0.8345 0.4895 0.552 Uiso 1 1 calc R . .
C101 C 0.5028(6) 0.7844(3) 0.5092(3) 0.108(4) Uani 1 1 d G . .
C102 C 0.5157(6) 0.7521(3) 0.5422(3) 0.098(4) Uani 1 1 d G . .
H102 H 0.5876 0.7403 0.5501 0.117 Uiso 1 1 calc R . .
C103 C 0.4234(10) 0.7371(3) 0.5636(2) 0.141(6) Uani 1 1 d G . .
H103 H 0.4322 0.7150 0.5862 0.169 Uiso 1 1 calc R . .
C104 C 0.3182(7) 0.7544(3) 0.5520(2) 0.118(4) Uani 1 1 d G . .
H104 H 0.2551 0.7441 0.5666 0.142 Uiso 1 1 calc R . .
C105 C 0.3053(6) 0.7867(3) 0.5189(2) 0.092(3) Uani 1 1 d G . .
H105 H 0.2334 0.7985 0.5110 0.111 Uiso 1 1 calc R . .
C106 C 0.3976(8) 0.8017(3) 0.49753(18) 0.100(3) Uani 1 1 d G . .
H106 H 0.3888 0.8237 0.4750 0.120 Uiso 1 1 calc R . .
C210 C 0.8266(9) 0.5818(7) 0.8319(5) 0.180(8) Uani 1 1 d . . .
H21A H 0.7822 0.5884 0.8547 0.269 Uiso 1 1 calc R . .
H21B H 0.9043 0.5914 0.8371 0.269 Uiso 1 1 calc R . .
H21C H 0.8207 0.5402 0.8243 0.269 Uiso 1 1 calc R . .
C211 C 0.7837(5) 0.6798(3) 0.8057(2) 0.069(2) Uani 1 1 d G . .
H211 H 0.8087 0.6983 0.8282 0.082 Uiso 1 1 calc R . .
C212 C 0.7442(6) 0.7139(3) 0.7760(3) 0.126(5) Uani 1 1 d G . .
H212 H 0.7421 0.7558 0.7782 0.151 Uiso 1 1 calc R . .
C213 C 0.7077(6) 0.6867(6) 0.7432(2) 0.148(7) Uani 1 1 d G . .
H213 H 0.6807 0.7100 0.7229 0.178 Uiso 1 1 calc R . .
C214 C 0.7107(6) 0.6254(7) 0.7400(2) 0.170(9) Uani 1 1 d G . .
H214 H 0.6857 0.6068 0.7175 0.204 Uiso 1 1 calc R . .
C215 C 0.7502(6) 0.5913(3) 0.7697(3) 0.131(6) Uani 1 1 d G . .
H215 H 0.7523 0.5494 0.7675 0.157 Uiso 1 1 calc R . .
C216 C 0.7867(5) 0.6185(3) 0.8025(2) 0.107(4) Uani 1 1 d G . .
C300 C -0.330(5) 0.724(2) 0.397(2) 0.35(4) Uiso 0.52(2) 1 d PD A 1
H30A H -0.3953 0.7196 0.3804 0.527 Uiso 0.52(2) 1 calc PR A 1
H30B H -0.3476 0.7110 0.4221 0.527 Uiso 0.52(2) 1 calc PR A 1
H30C H -0.2692 0.6997 0.3865 0.527 Uiso 0.52(2) 1 calc PR A 1
C301 C -0.2920(10) 0.7926(5) 0.3973(3) 0.053(5) Uiso 0.52(2) 1 d PG A 1
C302 C -0.2056(10) 0.8058(5) 0.4218(4) 0.110(8) Uiso 0.52(2) 1 d PGD A 1
H302 H -0.1530 0.7762 0.4282 0.132 Uiso 0.52(2) 1 calc PR A 1
C303 C -0.1961(10) 0.8623(6) 0.4369(4) 0.099(7) Uiso 0.52(2) 1 d PG A 1
H303 H -0.1370 0.8713 0.4537 0.119 Uiso 0.52(2) 1 calc PR A 1
C304 C -0.2731(14) 0.9057(5) 0.4275(5) 0.105(7) Uiso 0.52(2) 1 d PG A 1
H304 H -0.2666 0.9443 0.4379 0.126 Uiso 0.52(2) 1 calc PR A 1
C305 C -0.3595(14) 0.8925(6) 0.4030(5) 0.130(11) Uiso 0.52(2) 1 d PG A 1
H305 H -0.4121 0.9221 0.3966 0.156 Uiso 0.52(2) 1 calc PR A 1
C306 C -0.3690(11) 0.8360(7) 0.3879(4) 0.129(9) Uiso 0.52(2) 1 d PG A 1
H306 H -0.4281 0.8270 0.3712 0.155 Uiso 0.52(2) 1 calc PR A 1
C310 C -0.277(3) 0.7278(9) 0.3862(9) 0.124(10) Uiso 0.48(2) 1 d PD A 2
H31A H -0.3454 0.7069 0.3798 0.186 Uiso 0.48(2) 1 calc PR A 2
H31B H -0.2386 0.7067 0.4066 0.186 Uiso 0.48(2) 1 calc PR A 2
H31C H -0.2285 0.7296 0.3641 0.186 Uiso 0.48(2) 1 calc PR A 2
C311 C -0.3038(17) 0.7890(7) 0.3989(7) 0.27(3) Uiso 0.48(2) 1 d PGD A 2
C312 C -0.2209(13) 0.8279(8) 0.4102(7) 0.120(9) Uiso 0.48(2) 1 d PGD A 2
H312 H -0.1492 0.8133 0.4162 0.144 Uiso 0.48(2) 1 calc PR A 2
C313 C -0.2430(15) 0.8881(8) 0.4128(6) 0.137(11) Uiso 0.48(2) 1 d PG A 2
H313 H -0.1864 0.9147 0.4205 0.164 Uiso 0.48(2) 1 calc PR A 2
C314 C -0.3480(18) 0.9095(7) 0.4040(7) 0.124(12) Uiso 0.48(2) 1 d PG A 2
H314 H -0.3631 0.9507 0.4058 0.149 Uiso 0.48(2) 1 calc PR A 2
C315 C -0.4309(14) 0.8706(10) 0.3927(7) 0.160(13) Uiso 0.48(2) 1 d PG A 2
H315 H -0.5026 0.8852 0.3867 0.192 Uiso 0.48(2) 1 calc PR A 2
C316 C -0.4088(15) 0.8104(9) 0.3901(7) 0.129(10) Uiso 0.48(2) 1 d PG A 2
H316 H -0.4654 0.7838 0.3824 0.155 Uiso 0.48(2) 1 calc PR A 2
C400 C 0.7206(17) 0.4973(10) 0.6387(6) 0.201(8) Uiso 1 1 d . . .
H40C H 0.7310 0.4904 0.6658 0.302 Uiso 1 1 calc R . .
H40D H 0.7888 0.4870 0.6252 0.302 Uiso 1 1 calc R . .
H40E H 0.6595 0.4726 0.6295 0.302 Uiso 1 1 calc R . .
C401 C 0.6967(15) 0.5545(5) 0.6329(3) 0.146(6) Uani 1 1 d G . .
C402 C 0.5912(11) 0.5770(7) 0.6395(3) 0.160(7) Uani 1 1 d G . .
H402 H 0.5315 0.5509 0.6448 0.192 Uiso 1 1 calc R . .
C403 C 0.5731(11) 0.6377(7) 0.6383(3) 0.222(11) Uani 1 1 d G . .
H403 H 0.5010 0.6531 0.6428 0.267 Uiso 1 1 calc R . .
C404 C 0.6604(17) 0.6759(4) 0.6304(4) 0.189(10) Uani 1 1 d G . .
H404 H 0.6480 0.7174 0.6296 0.226 Uiso 1 1 calc R . .
C405 C 0.7659(13) 0.6534(8) 0.6238(4) 0.48(5) Uani 1 1 d G . .
H405 H 0.8256 0.6795 0.6184 0.575 Uiso 1 1 calc R . .
C406 C 0.7840(9) 0.5927(8) 0.6250(4) 0.34(2) Uani 1 1 d G . .
H406 H 0.8561 0.5773 0.6205 0.413 Uiso 1 1 calc R . .
C500 C 0.5684(18) 1.0408(8) 0.5372(7) 0.160(12) Uani 0.607(16) 1 d PD B 1
H50A H 0.5647 1.0835 0.5419 0.241 Uiso 0.607(16) 1 calc PR B 1
H50B H 0.6343 1.0318 0.5221 0.241 Uiso 0.607(16) 1 calc PR B 1
H50C H 0.5726 1.0197 0.5613 0.241 Uiso 0.607(16) 1 calc PR B 1
C501 C 0.4673(12) 1.0217(6) 0.5165(4) 0.103(6) Uiso 0.607(16) 1 d PG B 1
C502 C 0.3580(15) 1.0356(6) 0.5251(3) 0.104(6) Uiso 0.607(16) 1 d PGD B 1
H502 H 0.3417 1.0590 0.5467 0.125 Uiso 0.607(16) 1 calc PR B 1
C503 C 0.2725(9) 1.0153(6) 0.5023(4) 0.095(6) Uiso 0.607(16) 1 d PG B 1
H503 H 0.1978 1.0248 0.5082 0.114 Uiso 0.607(16) 1 calc PR B 1
C504 C 0.2963(8) 0.9812(5) 0.4707(4) 0.064(4) Uiso 0.607(16) 1 d PG B 1
H504 H 0.2379 0.9673 0.4551 0.077 Uiso 0.607(16) 1 calc PR B 1
C505 C 0.4057(11) 0.9673(5) 0.4621(3) 0.098(6) Uiso 0.607(16) 1 d PG B 1
H505 H 0.4220 0.9439 0.4405 0.117 Uiso 0.607(16) 1 calc PR B 1
C506 C 0.4912(6) 0.9875(6) 0.4849(4) 0.063(4) Uiso 0.607(16) 1 d PG B 1
H506 H 0.5659 0.9780 0.4790 0.076 Uiso 0.607(16) 1 calc PR B 1
C510 C 0.615(2) 1.0038(18) 0.5058(12) 0.160(16) Uiso 0.393(16) 1 d PD B 2
H51A H 0.6334 0.9745 0.5251 0.239 Uiso 0.393(16) 1 calc PR B 2
H51B H 0.6514 1.0414 0.5117 0.239 Uiso 0.393(16) 1 calc PR B 2
H51C H 0.6394 0.9897 0.4811 0.239 Uiso 0.393(16) 1 calc PR B 2
C511 C 0.5016(7) 1.0122(9) 0.5052(6) 0.078(7) Uiso 0.393(16) 1 d PG B 2
C512 C 0.4229(13) 1.0384(6) 0.5285(4) 0.054(5) Uiso 0.393(16) 1 d PGD B 2
H512 H 0.4457 1.0605 0.5498 0.065 Uiso 0.393(16) 1 calc PR B 2
C513 C 0.3107(10) 1.0321(6) 0.5204(4) 0.046(5) Uiso 0.393(16) 1 d PG B 2
H513 H 0.2569 1.0500 0.5363 0.056 Uiso 0.393(16) 1 calc PR B 2
C514 C 0.2773(11) 0.9997(7) 0.4891(5) 0.048(5) Uiso 0.393(16) 1 d PG B 2
H514 H 0.2006 0.9954 0.4836 0.058 Uiso 0.393(16) 1 calc PR B 2
C515 C 0.356(2) 0.9735(8) 0.4659(4) 0.094(8) Uiso 0.393(16) 1 d PG B 2
H515 H 0.3332 0.9514 0.4445 0.113 Uiso 0.393(16) 1 calc PR B 2
C516 C 0.4682(17) 0.9798(9) 0.4740(6) 0.121(12) Uiso 0.393(16) 1 d PG B 2
H516 H 0.5220 0.9619 0.4581 0.146 Uiso 0.393(16) 1 calc PR B 2
C600 C 0.189(2) 0.5523(9) 0.7955(6) 0.124(8) Uiso 0.553(14) 1 d PD C 1
H60A H 0.2050 0.5601 0.8221 0.185 Uiso 0.553(14) 1 calc PR C 1
H60B H 0.2249 0.5153 0.7879 0.185 Uiso 0.553(14) 1 calc PR C 1
H60C H 0.1087 0.5489 0.7919 0.185 Uiso 0.553(14) 1 calc PR C 1
C601 C 0.2295(9) 0.5988(4) 0.7736(3) 0.082(5) Uiso 0.553(14) 1 d PGD C 1
C602 C 0.2414(8) 0.6589(4) 0.7808(3) 0.038(3) Uiso 0.553(14) 1 d PG C 1
H602 H 0.2154 0.6750 0.8039 0.046 Uiso 0.553(14) 1 calc PR C 1
C603 C 0.2912(10) 0.6955(4) 0.7543(3) 0.072(5) Uiso 0.553(14) 1 d PG C 1
H603 H 0.2993 0.7366 0.7592 0.087 Uiso 0.553(14) 1 calc PR C 1
C604 C 0.3292(11) 0.6720(5) 0.7205(3) 0.115(7) Uiso 0.553(14) 1 d PG C 1
H604 H 0.3632 0.6970 0.7023 0.138 Uiso 0.553(14) 1 calc PR C 1
C605 C 0.3173(11) 0.6118(6) 0.7132(3) 0.087(6) Uiso 0.553(14) 1 d PG C 1
H605 H 0.3432 0.5957 0.6901 0.104 Uiso 0.553(14) 1 calc PR C 1
C606 C 0.2674(11) 0.5753(4) 0.7398(4) 0.078(6) Uiso 0.553(14) 1 d PG C 1
H606 H 0.2593 0.5342 0.7348 0.094 Uiso 0.553(14) 1 calc PR C 1
C610 C 0.351(2) 0.6838(12) 0.7067(7) 0.122(10) Uiso 0.447(14) 1 d PD C 2
H61A H 0.4317 0.6781 0.7083 0.182 Uiso 0.447(14) 1 calc PR C 2
H61B H 0.3340 0.7260 0.7092 0.182 Uiso 0.447(14) 1 calc PR C 2
H61C H 0.3244 0.6693 0.6824 0.182 Uiso 0.447(14) 1 calc PR C 2
C611 C 0.2964(10) 0.6504(4) 0.7376(3) 0.057(5) Uiso 0.447(14) 1 d PGD C 2
C612 C 0.2849(9) 0.5898(4) 0.7320(3) 0.028(4) Uiso 0.447(14) 1 d PG C 2
H612 H 0.3095 0.5723 0.7092 0.034 Uiso 0.447(14) 1 calc PR C 2
C613 C 0.2375(11) 0.5548(4) 0.7599(3) 0.057(5) Uiso 0.447(14) 1 d PG C 2
H613 H 0.2297 0.5134 0.7561 0.069 Uiso 0.447(14) 1 calc PR C 2
C614 C 0.2016(12) 0.5804(6) 0.7934(3) 0.101(8) Uiso 0.447(14) 1 d PG C 2
H614 H 0.1692 0.5565 0.8124 0.121 Uiso 0.447(14) 1 calc PR C 2
C615 C 0.2131(12) 0.6410(6) 0.7989(3) 0.080(6) Uiso 0.447(14) 1 d PG C 2
H615 H 0.1885 0.6585 0.8218 0.096 Uiso 0.447(14) 1 calc PR C 2
C616 C 0.2605(11) 0.6760(4) 0.7710(4) 0.059(5) Uiso 0.447(14) 1 d PG C 2
H616 H 0.2683 0.7174 0.7748 0.071 Uiso 0.447(14) 1 calc PR C 2


_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
Cl1 C5 1.734(7) . ?
Al1 O1 1.787(4) . ?
Al1 O2 1.851(4) . ?
Al1 O4 1.951(4) . ?
Al1 C1 1.978(6) . ?
Al1 N1 2.002(6) . ?
Al1 Al2 2.998(2) . ?
O1 C10 1.303(7) . ?
N1 C11 1.284(8) . ?
N1 C12 1.477(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Cl2 C7 1.756(7) . ?
Al2 O3 1.778(4) . ?
Al2 O4 1.856(4) . ?
Al2 C2 1.954(6) . ?
Al2 O2 1.979(4) . ?
Al2 N2 1.982(5) . ?
O2 C18 1.380(7) . ?
N2 C25 1.287(7) . ?
N2 C26 1.477(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
Cl3 C20 1.726(7) . ?
Al3 O7 1.765(4) . ?
Al3 O8 1.843(4) . ?
Al3 O6 1.960(4) . ?
Al3 C4 1.962(7) . ?
Al3 N4 1.992(6) . ?
Al3 Al4 2.975(3) . ?
O3 C19 1.337(7) . ?
N3 C39 1.290(8) . ?
N3 C40 1.455(8) . ?
N3 Al4 1.991(5) . ?
C3 Al4 1.964(7) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
Cl4 C22 1.733(6) . ?
Al4 O5 1.774(4) . ?
Al4 O6 1.841(4) . ?
Al4 O8 1.956(4) . ?
O4 C28 1.401(7) . ?
N4 C53 1.269(8) . ?
N4 C54 1.481(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
Cl5 C48 1.735(7) . ?
O5 C33 1.334(7) . ?
C5 C6 1.362(9) . ?
C5 C10 1.390(8) . ?
Cl6 C50 1.762(7) . ?
O6 C46 1.388(7) . ?
C6 C7 1.387(11) . ?
C6 H6 0.9500 . ?
Cl7 C34 1.735(8) . ?
O7 C47 1.321(7) . ?
C7 C8 1.364(11) . ?
Cl8 C36 1.753(7) . ?
O8 C56 1.397(7) . ?
C8 C9 1.413(9) . ?
C8 H8 0.9500 . ?
C9 C11 1.418(9) . ?
C9 C10 1.437(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.505(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.386(9) . ?
C13 C14 1.413(10) . ?
C14 C15 1.381(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.365(10) . ?
C15 H15 0.9500 . ?
C16 C61 1.386(9) . ?
C16 H16 0.9500 . ?
C18 C61 1.408(9) . ?
C19 C24 1.391(8) . ?
C19 C20 1.402(8) . ?
C20 C21 1.367(9) . ?
C21 C22 1.381(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.368(9) . ?
C23 C24 1.417(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.430(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.501(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C32 1.399(9) . ?
C27 C28 1.401(8) . ?
C28 C29 1.375(8) . ?
C29 C30 1.381(9) . ?
C29 H29 0.9500 . ?
C30 C31 1.374(10) . ?
C30 H30 0.9500 . ?
C31 C32 1.374(9) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.397(9) . ?
C33 C38 1.415(9) . ?
C34 C35 1.397(10) . ?
C35 C36 1.376(11) . ?
C35 H35 0.9500 . ?
C36 C37 1.353(10) . ?
C37 C38 1.417(8) . ?
C37 H37 0.9500 . ?
C38 C39 1.433(9) . ?
C39 H39 0.9500 . ?
C40 C41 1.518(8) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.376(9) . ?
C41 C46 1.396(9) . ?
C42 C43 1.391(10) . ?
C42 H42 0.9500 . ?
C43 C44 1.376(10) . ?
C43 H43 0.9500 . ?
C44 C45 1.393(9) . ?
C44 H44 0.9500 . ?
C45 C46 1.380(9) . ?
C45 H45 0.9500 . ?
C47 C52 1.393(9) . ?
C47 C48 1.427(8) . ?
C48 C49 1.368(10) . ?
C49 C50 1.368(10) . ?
C49 H49 0.9500 . ?
C50 C51 1.370(11) . ?
C51 C52 1.419(10) . ?
C51 H51 0.9500 . ?
C52 C53 1.445(9) . ?
C53 H53 0.9500 . ?
C54 C55 1.503(9) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C60 1.387(9) . ?
C55 C56 1.391(9) . ?
C56 C57 1.379(9) . ?
C57 C58 1.380(10) . ?
C57 H57 0.9500 . ?
C58 C59 1.394(11) . ?
C58 H58 0.9500 . ?
C59 C60 1.350(11) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C100 C101 1.227(19) . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
C101 C102 1.3900 . ?
C101 C106 1.3900 . ?
C102 C103 1.3900 . ?
C102 H102 0.9500 . ?
C103 C104 1.3900 . ?
C103 H103 0.9500 . ?
C104 C105 1.3900 . ?
C104 H104 0.9500 . ?
C105 C106 1.3900 . ?
C105 H105 0.9500 . ?
C106 H106 0.9500 . ?
C210 C216 1.417(14) . ?
C210 H21A 0.9800 . ?
C210 H21B 0.9800 . ?
C210 H21C 0.9800 . ?
C211 C212 1.3900 . ?
C211 C216 1.3900 . ?
C211 H211 0.9500 . ?
C212 C213 1.3900 . ?
C212 H212 0.9500 . ?
C213 C214 1.3900 . ?
C213 H213 0.9500 . ?
C214 C215 1.3900 . ?
C214 H214 0.9500 . ?
C215 C216 1.3900 . ?
C215 H215 0.9500 . ?
C300 C301 1.62(4) . ?
C300 H30A 0.9800 . ?
C300 H30B 0.9800 . ?
C300 H30C 0.9800 . ?
C301 C302 1.3900 . ?
C301 C306 1.3900 . ?
C302 C303 1.3900 . ?
C302 H302 0.9500 . ?
C303 C304 1.3900 . ?
C303 H303 0.9500 . ?
C304 C305 1.3900 . ?
C304 H304 0.9500 . ?
C305 C306 1.3900 . ?
C305 H305 0.9500 . ?
C306 H306 0.9500 . ?
C310 C311 1.489(16) . ?
C310 H31A 0.9800 . ?
C310 H31B 0.9800 . ?
C310 H31C 0.9800 . ?
C311 C312 1.3900 . ?
C311 C316 1.3900 . ?
C312 C313 1.3900 . ?
C312 H312 0.9500 . ?
C313 C314 1.3900 . ?
C313 H313 0.9500 . ?
C314 C315 1.3900 . ?
C314 H314 0.9500 . ?
C315 C316 1.3900 . ?
C315 H315 0.9500 . ?
C316 H316 0.9500 . ?
C400 C401 1.34(2) . ?
C400 H40C 0.9800 . ?
C400 H40D 0.9800 . ?
C400 H40E 0.9800 . ?
C401 C402 1.3900 . ?
C401 C406 1.3900 . ?
C402 C403 1.3900 . ?
C402 H402 0.9500 . ?
C403 C404 1.3900 . ?
C403 H403 0.9500 . ?
C404 C405 1.3900 . ?
C404 H404 0.9500 . ?
C405 C406 1.3900 . ?
C405 H405 0.9500 . ?
C406 H406 0.9500 . ?
C500 C501 1.488(16) . ?
C500 H50A 0.9800 . ?
C500 H50B 0.9800 . ?
C500 H50C 0.9800 . ?
C501 C502 1.3900 . ?
C501 C506 1.3900 . ?
C502 C503 1.3900 . ?
C502 H502 0.9500 . ?
C503 C504 1.3900 . ?
C503 H503 0.9500 . ?
C504 C505 1.3900 . ?
C504 H504 0.9500 . ?
C505 C506 1.3900 . ?
C505 H505 0.9500 . ?
C506 H506 0.9500 . ?
C510 C511 1.38(2) . ?
C510 H51A 0.9800 . ?
C510 H51B 0.9800 . ?
C510 H51C 0.9800 . ?
C511 C512 1.3900 . ?
C511 C516 1.3900 . ?
C512 C513 1.3900 . ?
C512 H512 0.9500 . ?
C513 C514 1.3900 . ?
C513 H513 0.9500 . ?
C514 C515 1.3900 . ?
C514 H514 0.9500 . ?
C515 C516 1.3900 . ?
C515 H515 0.9500 . ?
C516 H516 0.9500 . ?
C600 C601 1.395(16) . ?
C600 H60A 0.9800 . ?
C600 H60B 0.9800 . ?
C600 H60C 0.9800 . ?
C601 C602 1.3900 . ?
C601 C606 1.3900 . ?
C602 C603 1.3900 . ?
C602 H602 0.9500 . ?
C603 C604 1.3900 . ?
C603 H603 0.9500 . ?
C604 C605 1.3900 . ?
C604 H604 0.9500 . ?
C605 C606 1.3900 . ?
C605 H605 0.9500 . ?
C606 H606 0.9500 . ?
C610 C611 1.486(18) . ?
C610 H61A 0.9800 . ?
C610 H61B 0.9800 . ?
C610 H61C 0.9800 . ?
C611 C612 1.3900 . ?
C611 C616 1.3900 . ?
C612 C613 1.3900 . ?
C612 H612 0.9500 . ?
C613 C614 1.3900 . ?
C613 H613 0.9500 . ?
C614 C615 1.3900 . ?
C614 H614 0.9500 . ?
C615 C616 1.3900 . ?
C615 H615 0.9500 . ?
C616 H616 0.9500 . ?

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 116.13(19) . . ?
O1 Al1 O4 95.25(18) . . ?
O2 Al1 O4 76.89(18) . . ?
O1 Al1 C1 120.3(3) . . ?
O2 Al1 C1 123.5(3) . . ?
O4 Al1 C1 95.6(3) . . ?
O1 Al1 N1 89.9(2) . . ?
O2 Al1 N1 87.3(2) . . ?
O4 Al1 N1 164.1(2) . . ?
C1 Al1 N1 94.8(3) . . ?
O1 Al1 Al2 111.61(14) . . ?
O2 Al1 Al2 40.06(13) . . ?
O4 Al1 Al2 36.95(12) . . ?
C1 Al1 Al2 111.7(2) . . ?
N1 Al1 Al2 127.33(17) . . ?
C10 O1 Al1 133.1(4) . . ?
C11 N1 C12 120.0(6) . . ?
C11 N1 Al1 125.7(4) . . ?
C12 N1 Al1 114.2(4) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 Al2 O4 115.7(2) . . ?
O3 Al2 C2 123.6(3) . . ?
O4 Al2 C2 120.4(2) . . ?
O3 Al2 O2 93.76(18) . . ?
O4 Al2 O2 76.06(17) . . ?
C2 Al2 O2 93.7(2) . . ?
O3 Al2 N2 90.26(19) . . ?
O4 Al2 N2 88.68(19) . . ?
C2 Al2 N2 96.5(3) . . ?
O2 Al2 N2 164.47(19) . . ?
O3 Al2 Al1 110.31(15) . . ?
O4 Al2 Al1 39.18(13) . . ?
C2 Al2 Al1 108.7(2) . . ?
O2 Al2 Al1 36.99(12) . . ?
N2 Al2 Al1 127.86(15) . . ?
C18 O2 Al1 131.7(4) . . ?
C18 O2 Al2 124.7(4) . . ?
Al1 O2 Al2 102.9(2) . . ?
C25 N2 C26 119.8(5) . . ?
C25 N2 Al2 126.6(4) . . ?
C26 N2 Al2 113.5(4) . . ?
Al2 C2 H2A 109.5 . . ?
Al2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Al2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O7 Al3 O8 115.6(2) . . ?
O7 Al3 O6 93.83(18) . . ?
O8 Al3 O6 76.87(18) . . ?
O7 Al3 C4 122.8(3) . . ?
O8 Al3 C4 121.5(3) . . ?
O6 Al3 C4 95.1(3) . . ?
O7 Al3 N4 89.4(2) . . ?
O8 Al3 N4 87.5(2) . . ?
O6 Al3 N4 163.9(2) . . ?
C4 Al3 N4 96.4(3) . . ?
O7 Al3 Al4 109.59(15) . . ?
O8 Al3 Al4 39.84(13) . . ?
O6 Al3 Al4 37.08(12) . . ?
C4 Al3 Al4 111.0(2) . . ?
N4 Al3 Al4 127.37(17) . . ?
C19 O3 Al2 131.8(4) . . ?
C39 N3 C40 120.1(5) . . ?
C39 N3 Al4 125.3(4) . . ?
C40 N3 Al4 114.3(4) . . ?
Al4 C3 H3A 109.5 . . ?
Al4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Al4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O5 Al4 O6 114.5(2) . . ?
O5 Al4 O8 92.3(2) . . ?
O6 Al4 O8 77.00(18) . . ?
O5 Al4 C3 124.5(3) . . ?
O6 Al4 C3 120.7(2) . . ?
O8 Al4 C3 94.9(2) . . ?
O5 Al4 N3 90.1(2) . . ?
O6 Al4 N3 90.2(2) . . ?
O8 Al4 N3 166.8(2) . . ?
C3 Al4 N3 94.4(3) . . ?
O5 Al4 Al3 107.97(16) . . ?
O6 Al4 Al3 39.93(14) . . ?
O8 Al4 Al3 37.12(13) . . ?
C3 Al4 Al3 110.5(2) . . ?
N3 Al4 Al3 130.11(16) . . ?
C28 O4 Al2 130.6(4) . . ?
C28 O4 Al1 125.3(3) . . ?
Al2 O4 Al1 103.9(2) . . ?
C53 N4 C54 119.3(6) . . ?
C53 N4 Al3 127.8(5) . . ?
C54 N4 Al3 112.8(4) . . ?
Al3 C4 H4A 109.5 . . ?
Al3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Al3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C33 O5 Al4 130.0(4) . . ?
C6 C5 C10 123.3(6) . . ?
C6 C5 Cl1 119.6(5) . . ?
C10 C5 Cl1 117.1(5) . . ?
C46 O6 Al4 130.1(4) . . ?
C46 O6 Al3 126.9(4) . . ?
Al4 O6 Al3 103.0(2) . . ?
C5 C6 C7 119.1(6) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C47 O7 Al3 133.0(4) . . ?
C8 C7 C6 121.5(7) . . ?
C8 C7 Cl2 119.7(6) . . ?
C6 C7 Cl2 118.8(6) . . ?
C56 O8 Al3 132.1(4) . . ?
C56 O8 Al4 124.4(4) . . ?
Al3 O8 Al4 103.0(2) . . ?
C7 C8 C9 119.6(7) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C8 C9 C11 118.0(6) . . ?
C8 C9 C10 119.8(6) . . ?
C11 C9 C10 122.2(6) . . ?
O1 C10 C5 121.6(6) . . ?
O1 C10 C9 121.6(5) . . ?
C5 C10 C9 116.7(5) . . ?
N1 C11 C9 124.2(6) . . ?
N1 C11 H11 117.9 . . ?
C9 C11 H11 117.9 . . ?
N1 C12 C13 108.1(5) . . ?
N1 C12 H12A 110.1 . . ?
C13 C12 H12A 110.1 . . ?
N1 C12 H12B 110.1 . . ?
C13 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
C18 C13 C14 118.6(6) . . ?
C18 C13 C12 122.3(6) . . ?
C14 C13 C12 119.1(6) . . ?
C15 C14 C13 121.4(7) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C16 C15 C14 118.8(7) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C15 C16 C61 121.9(7) . . ?
C15 C16 H16 119.0 . . ?
C61 C16 H16 119.0 . . ?
O2 C18 C13 120.9(6) . . ?
O2 C18 C61 119.0(6) . . ?
C13 C18 C61 119.9(6) . . ?
O3 C19 C24 122.5(5) . . ?
O3 C19 C20 120.0(5) . . ?
C24 C19 C20 117.5(5) . . ?
C21 C20 C19 122.3(6) . . ?
C21 C20 Cl3 119.1(5) . . ?
C19 C20 Cl3 118.7(5) . . ?
C20 C21 C22 119.7(6) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 120.2(6) . . ?
C23 C22 Cl4 120.0(5) . . ?
C21 C22 Cl4 119.8(5) . . ?
C22 C23 C24 120.2(6) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C19 C24 C23 120.0(5) . . ?
C19 C24 C25 122.6(5) . . ?
C23 C24 C25 117.3(6) . . ?
N2 C25 C24 123.2(6) . . ?
N2 C25 H25 118.4 . . ?
C24 C25 H25 118.4 . . ?
N2 C26 C27 108.6(5) . . ?
N2 C26 H26A 110.0 . . ?
C27 C26 H26A 110.0 . . ?
N2 C26 H26B 110.0 . . ?
C27 C26 H26B 110.0 . . ?
H26A C26 H26B 108.4 . . ?
C32 C27 C28 117.9(6) . . ?
C32 C27 C26 120.7(6) . . ?
C28 C27 C26 121.4(5) . . ?
C29 C28 O4 119.3(5) . . ?
C29 C28 C27 120.1(5) . . ?
O4 C28 C27 120.5(5) . . ?
C28 C29 C30 120.7(6) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C31 C30 C29 120.2(6) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C32 C31 C30 119.6(6) . . ?
C32 C31 H31 120.2 . . ?
C30 C31 H31 120.2 . . ?
C31 C32 C27 121.5(6) . . ?
C31 C32 H32 119.2 . . ?
C27 C32 H32 119.2 . . ?
O5 C33 C34 119.7(6) . . ?
O5 C33 C38 122.6(5) . . ?
C34 C33 C38 117.6(6) . . ?
C35 C34 C33 122.4(7) . . ?
C35 C34 Cl7 119.5(5) . . ?
C33 C34 Cl7 118.0(5) . . ?
C36 C35 C34 117.6(6) . . ?
C36 C35 H35 121.2 . . ?
C34 C35 H35 121.2 . . ?
C37 C36 C35 122.8(6) . . ?
C37 C36 Cl8 119.1(6) . . ?
C35 C36 Cl8 118.0(6) . . ?
C36 C37 C38 119.9(7) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C33 C38 C37 119.3(6) . . ?
C33 C38 C39 121.7(5) . . ?
C37 C38 C39 118.8(6) . . ?
N3 C39 C38 123.0(6) . . ?
N3 C39 H39 118.5 . . ?
C38 C39 H39 118.5 . . ?
N3 C40 C41 108.8(5) . . ?
N3 C40 H40A 109.9 . . ?
C41 C40 H40A 109.9 . . ?
N3 C40 H40B 109.9 . . ?
C41 C40 H40B 109.9 . . ?
H40A C40 H40B 108.3 . . ?
C42 C41 C46 118.7(6) . . ?
C42 C41 C40 119.3(6) . . ?
C46 C41 C40 122.0(6) . . ?
C41 C42 C43 121.8(6) . . ?
C41 C42 H42 119.1 . . ?
C43 C42 H42 119.1 . . ?
C44 C43 C42 119.0(6) . . ?
C44 C43 H43 120.5 . . ?
C42 C43 H43 120.5 . . ?
C43 C44 C45 120.0(7) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C46 C45 C44 120.4(7) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 O6 118.8(6) . . ?
C45 C46 C41 120.1(6) . . ?
O6 C46 C41 121.1(5) . . ?
O7 C47 C52 123.7(5) . . ?
O7 C47 C48 119.9(6) . . ?
C52 C47 C48 116.4(6) . . ?
C49 C48 C47 121.6(6) . . ?
C49 C48 Cl5 120.0(5) . . ?
C47 C48 Cl5 118.4(5) . . ?
C50 C49 C48 120.4(6) . . ?
C50 C49 H49 119.8 . . ?
C48 C49 H49 119.8 . . ?
C49 C50 C51 121.3(7) . . ?
C49 C50 Cl6 118.8(6) . . ?
C51 C50 Cl6 119.9(6) . . ?
C50 C51 C52 118.8(7) . . ?
C50 C51 H51 120.6 . . ?
C52 C51 H51 120.6 . . ?
C47 C52 C51 121.5(6) . . ?
C47 C52 C53 120.5(6) . . ?
C51 C52 C53 117.9(6) . . ?
N4 C53 C52 123.7(6) . . ?
N4 C53 H53 118.2 . . ?
C52 C53 H53 118.2 . . ?
N4 C54 C55 108.9(5) . . ?
N4 C54 H54A 109.9 . . ?
C55 C54 H54A 109.9 . . ?
N4 C54 H54B 109.9 . . ?
C55 C54 H54B 109.9 . . ?
H54A C54 H54B 108.3 . . ?
C60 C55 C56 118.4(6) . . ?
C60 C55 C54 120.2(6) . . ?
C56 C55 C54 121.4(5) . . ?
C57 C56 C55 120.9(6) . . ?
C57 C56 O8 118.7(6) . . ?
C55 C56 O8 120.4(6) . . ?
C56 C57 C58 119.2(7) . . ?
C56 C57 H57 120.4 . . ?
C58 C57 H57 120.4 . . ?
C57 C58 C59 120.2(7) . . ?
C57 C58 H58 119.9 . . ?
C59 C58 H58 119.9 . . ?
C60 C59 C58 119.7(7) . . ?
C60 C59 H59 120.2 . . ?
C58 C59 H59 120.2 . . ?
C59 C60 C55 121.6(7) . . ?
C59 C60 H60 119.2 . . ?
C55 C60 H60 119.2 . . ?
C16 C61 C18 119.3(6) . . ?
C101 C100 H10A 109.5 . . ?
C101 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
C101 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C100 C101 C102 107.9(19) . . ?
C100 C101 C106 132.1(19) . . ?
C102 C101 C106 120.0 . . ?
C101 C102 C103 120.0 . . ?
C101 C102 H102 120.0 . . ?
C103 C102 H102 120.0 . . ?
C104 C103 C102 120.0 . . ?
C104 C103 H103 120.0 . . ?
C102 C103 H103 120.0 . . ?
C103 C104 C105 120.0 . . ?
C103 C104 H104 120.0 . . ?
C105 C104 H104 120.0 . . ?
C106 C105 C104 120.0 . . ?
C106 C105 H105 120.0 . . ?
C104 C105 H105 120.0 . . ?
C105 C106 C101 120.0 . . ?
C105 C106 H106 120.0 . . ?
C101 C106 H106 120.0 . . ?
C216 C210 H21A 109.5 . . ?
C216 C210 H21B 109.5 . . ?
H21A C210 H21B 109.5 . . ?
C216 C210 H21C 109.5 . . ?
H21A C210 H21C 109.5 . . ?
H21B C210 H21C 109.5 . . ?
C212 C211 C216 120.0 . . ?
C212 C211 H211 120.0 . . ?
C216 C211 H211 120.0 . . ?
C211 C212 C213 120.0 . . ?
C211 C212 H212 120.0 . . ?
C213 C212 H212 120.0 . . ?
C212 C213 C214 120.0 . . ?
C212 C213 H213 120.0 . . ?
C214 C213 H213 120.0 . . ?
C213 C214 C215 120.0 . . ?
C213 C214 H214 120.0 . . ?
C215 C214 H214 120.0 . . ?
C216 C215 C214 120.0 . . ?
C216 C215 H215 120.0 . . ?
C214 C215 H215 120.0 . . ?
C215 C216 C211 120.0 . . ?
C215 C216 C210 117.8(11) . . ?
C211 C216 C210 122.2(11) . . ?
C301 C300 H30A 109.5 . . ?
C301 C300 H30B 109.5 . . ?
H30A C300 H30B 109.5 . . ?
C301 C300 H30C 109.5 . . ?
H30A C300 H30C 109.5 . . ?
H30B C300 H30C 109.5 . . ?
C302 C301 C306 120.0 . . ?
C302 C301 C300 115(2) . . ?
C306 C301 C300 119(2) . . ?
C303 C302 C301 120.0 . . ?
C303 C302 H302 120.0 . . ?
C301 C302 H302 120.0 . . ?
C302 C303 C304 120.0 . . ?
C302 C303 H303 120.0 . . ?
C304 C303 H303 120.0 . . ?
C305 C304 C303 120.0 . . ?
C305 C304 H304 120.0 . . ?
C303 C304 H304 120.0 . . ?
C306 C305 C304 120.0 . . ?
C306 C305 H305 120.0 . . ?
C304 C305 H305 120.0 . . ?
C305 C306 C301 120.0 . . ?
C305 C306 H306 120.0 . . ?
C301 C306 H306 120.0 . . ?
C311 C310 H31A 109.5 . . ?
C311 C310 H31B 109.5 . . ?
H31A C310 H31B 109.5 . . ?
C311 C310 H31C 109.5 . . ?
H31A C310 H31C 109.5 . . ?
H31B C310 H31C 109.5 . . ?
C312 C311 C316 120.0 . . ?
C312 C311 C310 121.1(15) . . ?
C316 C311 C310 117.0(15) . . ?
C313 C312 C311 120.0 . . ?
C313 C312 H312 120.0 . . ?
C311 C312 H312 120.0 . . ?
C312 C313 C314 120.0 . . ?
C312 C313 H313 120.0 . . ?
C314 C313 H313 120.0 . . ?
C315 C314 C313 120.0 . . ?
C315 C314 H314 120.0 . . ?
C313 C314 H314 120.0 . . ?
C314 C315 C316 120.0 . . ?
C314 C315 H315 120.0 . . ?
C316 C315 H315 120.0 . . ?
C315 C316 C311 120.0 . . ?
C315 C316 H316 120.0 . . ?
C311 C316 H316 120.0 . . ?
C401 C400 H40C 109.5 . . ?
C401 C400 H40D 109.5 . . ?
H40C C400 H40D 109.5 . . ?
C401 C400 H40E 109.5 . . ?
H40C C400 H40E 109.5 . . ?
H40D C400 H40E 109.5 . . ?
C400 C401 C402 121.6(16) . . ?
C400 C401 C406 117.8(16) . . ?
C402 C401 C406 120.0 . . ?
C403 C402 C401 120.0 . . ?
C403 C402 H402 120.0 . . ?
C401 C402 H402 120.0 . . ?
C402 C403 C404 120.0 . . ?
C402 C403 H403 120.0 . . ?
C404 C403 H403 120.0 . . ?
C405 C404 C403 120.0 . . ?
C405 C404 H404 120.0 . . ?
C403 C404 H404 120.0 . . ?
C406 C405 C404 120.0 . . ?
C406 C405 H405 120.0 . . ?
C404 C405 H405 120.0 . . ?
C405 C406 C401 120.0 . . ?
C405 C406 H406 120.0 . . ?
C401 C406 H406 120.0 . . ?
C501 C500 H50A 109.5 . . ?
C501 C500 H50B 109.5 . . ?
H50A C500 H50B 109.5 . . ?
C501 C500 H50C 109.5 . . ?
H50A C500 H50C 109.5 . . ?
H50B C500 H50C 109.5 . . ?
C502 C501 C506 120.0 . . ?
C502 C501 C500 127.0(13) . . ?
C506 C501 C500 113.0(13) . . ?
C501 C502 C503 120.0 . . ?
C501 C502 H502 120.0 . . ?
C503 C502 H502 120.0 . . ?
C504 C503 C502 120.0 . . ?
C504 C503 H503 120.0 . . ?
C502 C503 H503 120.0 . . ?
C503 C504 C505 120.0 . . ?
C503 C504 H504 120.0 . . ?
C505 C504 H504 120.0 . . ?
C504 C505 C506 120.0 . . ?
C504 C505 H505 120.0 . . ?
C506 C505 H505 120.0 . . ?
C505 C506 C501 120.0 . . ?
C505 C506 H506 120.0 . . ?
C501 C506 H506 120.0 . . ?
C511 C510 H51A 109.5 . . ?
C511 C510 H51B 109.5 . . ?
H51A C510 H51B 109.5 . . ?
C511 C510 H51C 109.5 . . ?
H51A C510 H51C 109.5 . . ?
H51B C510 H51C 109.5 . . ?
C510 C511 C512 137(2) . . ?
C510 C511 C516 103(2) . . ?
C512 C511 C516 120.0 . . ?
C513 C512 C511 120.0 . . ?
C513 C512 H512 120.0 . . ?
C511 C512 H512 120.0 . . ?
C512 C513 C514 120.0 . . ?
C512 C513 H513 120.0 . . ?
C514 C513 H513 120.0 . . ?
C515 C514 C513 120.0 . . ?
C515 C514 H514 120.0 . . ?
C513 C514 H514 120.0 . . ?
C514 C515 C516 120.0 . . ?
C514 C515 H515 120.0 . . ?
C516 C515 H515 120.0 . . ?
C515 C516 C511 120.0 . . ?
C515 C516 H516 120.0 . . ?
C511 C516 H516 120.0 . . ?
C601 C600 H60A 109.5 . . ?
C601 C600 H60B 109.5 . . ?
H60A C600 H60B 109.5 . . ?
C601 C600 H60C 109.5 . . ?
H60A C600 H60C 109.5 . . ?
H60B C600 H60C 109.5 . . ?
C602 C601 C606 120.0 . . ?
C602 C601 C600 131.9(12) . . ?
C606 C601 C600 108.0(12) . . ?
C601 C602 C603 120.0 . . ?
C601 C602 H602 120.0 . . ?
C603 C602 H602 120.0 . . ?
C604 C603 C602 120.0 . . ?
C604 C603 H603 120.0 . . ?
C602 C603 H603 120.0 . . ?
C603 C604 C605 120.0 . . ?
C603 C604 H604 120.0 . . ?
C605 C604 H604 120.0 . . ?
C606 C605 C604 120.0 . . ?
C606 C605 H605 120.0 . . ?
C604 C605 H605 120.0 . . ?
C605 C606 C601 120.0 . . ?
C605 C606 H606 120.0 . . ?
C601 C606 H606 120.0 . . ?
C611 C610 H61A 109.5 . . ?
C611 C610 H61B 109.5 . . ?
H61A C610 H61B 109.5 . . ?
C611 C610 H61C 109.5 . . ?
H61A C610 H61C 109.5 . . ?
H61B C610 H61C 109.5 . . ?
C612 C611 C616 120.0 . . ?
C612 C611 C610 116.1(14) . . ?
C616 C611 C610 123.9(14) . . ?
C613 C612 C611 120.0 . . ?
C613 C612 H612 120.0 . . ?
C611 C612 H612 120.0 . . ?
C612 C613 C614 120.0 . . ?
C612 C613 H613 120.0 . . ?
C614 C613 H613 120.0 . . ?
C615 C614 C613 120.0 . . ?
C615 C614 H614 120.0 . . ?
C613 C614 H614 120.0 . . ?
C616 C615 C614 120.0 . . ?
C616 C615 H615 120.0 . . ?
C614 C615 H615 120.0 . . ?
C615 C616 C611 120.0 . . ?
C615 C616 H616 120.0 . . ?
C611 C616 H616 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.069
####################################################################### 
# 
# 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_Al5
_database_code_depnum_ccdc_archive 'CCDC 1037366'
_audit_update_record             
;
2014-12-03 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C69 H100 Al2 N2 O4'
_chemical_formula_weight         1075.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P21/n

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

_cell_length_a                   13.632(3)
_cell_length_b                   19.1280(17)
_cell_length_c                   25.491(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.037(7)
_cell_angle_gamma                90.00
_cell_volume                     6564.3(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    44097
_cell_measurement_theta_min      3.51
_cell_measurement_theta_max      25.03

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2344
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'nonius kappa ccd'
_diffrn_measurement_method       ccd
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            73557
_diffrn_reflns_av_R_equivalents  0.1273
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         25.03
_reflns_number_total             11493
_reflns_number_gt                7575
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_structure_solution    
;
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
 (1999) J. Appl. Cryst. 32, 115-119.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0590P)²+8.4688P] 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         11493
_refine_ls_number_parameters     746
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0638
_refine_ls_wR_factor_ref         0.1716
_refine_ls_wR_factor_gt          0.1417
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.051
_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 0.47694(7) 0.21807(5) 0.42461(4) 0.0309(2) Uani 1 1 d . . .
O1 O 0.61133(15) 0.23560(10) 0.43318(8) 0.0251(5) Uani 1 1 d . . .
N1 N 0.63848(18) 0.29237(12) 0.33805(10) 0.0244(5) Uani 1 1 d . . .
C1 C 0.4242(3) 0.1494(2) 0.47028(15) 0.0487(10) Uani 1 1 d . . .
H1A H 0.3970 0.1093 0.4488 0.073 Uiso 1 1 calc R . .
H1B H 0.3716 0.1711 0.4869 0.073 Uiso 1 1 calc R . .
H1C H 0.4778 0.1335 0.4979 0.073 Uiso 1 1 calc R . .
Al2 Al 0.65240(7) 0.19554(4) 0.36868(3) 0.0226(2) Uani 1 1 d . . .
O2 O 0.65760(15) 0.15959(10) 0.30322(8) 0.0256(5) Uani 1 1 d . . .
N2 N 0.67114(18) 0.09834(12) 0.39804(9) 0.0231(5) Uani 1 1 d . . .
C2 C 0.4026(3) 0.3060(2) 0.42438(18) 0.0542(11) Uani 1 1 d . . .
H2A H 0.4370 0.3374 0.4516 0.081 Uiso 1 1 calc R . .
H2B H 0.3357 0.2963 0.4320 0.081 Uiso 1 1 calc R . .
H2C H 0.3981 0.3282 0.3894 0.081 Uiso 1 1 calc R . .
O3 O 0.50420(15) 0.17824(10) 0.36268(8) 0.0251(5) Uani 1 1 d . . .
C3 C 0.6596(2) 0.29453(15) 0.45788(12) 0.0251(7) Uani 1 1 d . . .
O4 O 0.78275(15) 0.21431(10) 0.39233(8) 0.0257(5) Uani 1 1 d . . .
C4 C 0.6604(2) 0.35369(16) 0.42597(12) 0.0276(7) Uani 1 1 d . . .
C5 C 0.7040(2) 0.41523(16) 0.44702(13) 0.0315(7) Uani 1 1 d . . .
H5 H 0.7049 0.4549 0.4247 0.038 Uiso 1 1 calc R . .
C6 C 0.7461(3) 0.41966(17) 0.50004(12) 0.0326(8) Uani 1 1 d . A .
C7 C 0.7449(3) 0.35962(17) 0.53032(13) 0.0335(8) Uani 1 1 d . . .
H7 H 0.7732 0.3622 0.5668 0.040 Uiso 1 1 calc R . .
C8 C 0.7049(2) 0.29535(16) 0.51111(12) 0.0288(7) Uani 1 1 d . . .
C9 C 0.7894(2) 0.48814(15) 0.52536(11) 0.0415(9) Uani 1 1 d D . .
C10 C 0.8933(3) 0.4723(3) 0.5575(2) 0.0582(15) Uani 0.75 1 d PD A 1
H10A H 0.9350 0.4503 0.5342 0.087 Uiso 0.75 1 calc PR A 1
H10B H 0.8862 0.4406 0.5869 0.087 Uiso 0.75 1 calc PR A 1
H10C H 0.9242 0.5160 0.5717 0.087 Uiso 0.75 1 calc PR A 1
C11 C 0.7263(4) 0.5146(3) 0.5659(2) 0.0534(14) Uani 0.75 1 d PD A 1
H11A H 0.7572 0.5565 0.5835 0.080 Uiso 0.75 1 calc PR A 1
H11B H 0.7218 0.4782 0.5924 0.080 Uiso 0.75 1 calc PR A 1
H11C H 0.6595 0.5262 0.5477 0.080 Uiso 0.75 1 calc PR A 1
C12 C 0.8122(6) 0.5422(3) 0.48459(17) 0.073(2) Uani 0.75 1 d PD A 1
H12A H 0.8486 0.5815 0.5031 0.110 Uiso 0.75 1 calc PR A 1
H12B H 0.7499 0.5592 0.4641 0.110 Uiso 0.75 1 calc PR A 1
H12C H 0.8527 0.5205 0.4605 0.110 Uiso 0.75 1 calc PR A 1
C13 C 0.7111(3) 0.23356(17) 0.55037(13) 0.0340(8) Uani 1 1 d . . .
C14 C 0.7097(4) 0.16155(18) 0.52390(15) 0.0559(12) Uani 1 1 d . . .
H14A H 0.6456 0.1545 0.5011 0.084 Uiso 1 1 calc R . .
H14B H 0.7196 0.1252 0.5513 0.084 Uiso 1 1 calc R . .
H14C H 0.7631 0.1590 0.5023 0.084 Uiso 1 1 calc R . .
C15 C 0.6231(3) 0.2397(2) 0.58077(17) 0.0583(12) Uani 1 1 d . . .
H15A H 0.6275 0.2839 0.6004 0.087 Uiso 1 1 calc R . .
H15B H 0.6245 0.2006 0.6058 0.087 Uiso 1 1 calc R . .
H15C H 0.5608 0.2384 0.5556 0.087 Uiso 1 1 calc R . .
C16 C 0.8078(3) 0.2359(2) 0.58999(15) 0.0501(10) Uani 1 1 d . . .
H16A H 0.8644 0.2365 0.5706 0.075 Uiso 1 1 calc R . .
H16B H 0.8119 0.1946 0.6129 0.075 Uiso 1 1 calc R . .
H16C H 0.8088 0.2782 0.6118 0.075 Uiso 1 1 calc R . .
C17 C 0.6090(2) 0.35204(16) 0.36921(12) 0.0291(7) Uani 1 1 d . . .
H17A H 0.5364 0.3500 0.3689 0.035 Uiso 1 1 calc R . .
H17B H 0.6237 0.3961 0.3516 0.035 Uiso 1 1 calc R . .
C18 C 0.6602(2) 0.30773(16) 0.29207(12) 0.0272(7) Uani 1 1 d . . .
H18 H 0.6611 0.3560 0.2835 0.033 Uiso 1 1 calc R . .
C19 C 0.6833(2) 0.25993(15) 0.25207(12) 0.0269(7) Uani 1 1 d . . .
C20 C 0.6791(2) 0.18634(16) 0.25856(12) 0.0250(7) Uani 1 1 d . . .
C21 C 0.6952(2) 0.14354(16) 0.21489(12) 0.0253(7) Uani 1 1 d . . .
C22 C 0.7129(2) 0.17644(17) 0.16882(12) 0.0303(7) Uani 1 1 d . . .
H22 H 0.7236 0.1475 0.1400 0.036 Uiso 1 1 calc R . .
C23 C 0.7161(2) 0.24905(17) 0.16134(13) 0.0320(7) Uani 1 1 d . B .
C24 C 0.7018(2) 0.28962(17) 0.20421(12) 0.0316(7) Uani 1 1 d . . .
H24 H 0.7047 0.3391 0.2013 0.038 Uiso 1 1 calc R . .
C25 C 0.6864(2) 0.06329(16) 0.21727(12) 0.0293(7) Uani 1 1 d . . .
C26 C 0.5769(3) 0.04474(18) 0.21887(15) 0.0408(9) Uani 1 1 d . . .
H26A H 0.5559 0.0662 0.2502 0.061 Uiso 1 1 calc R . .
H26B H 0.5698 -0.0062 0.2207 0.061 Uiso 1 1 calc R . .
H26C H 0.5354 0.0624 0.1867 0.061 Uiso 1 1 calc R . .
C27 C 0.7514(3) 0.03276(18) 0.26645(14) 0.0424(9) Uani 1 1 d . . .
H27A H 0.8211 0.0448 0.2658 0.064 Uiso 1 1 calc R . .
H27B H 0.7441 -0.0182 0.2664 0.064 Uiso 1 1 calc R . .
H27C H 0.7306 0.0521 0.2986 0.064 Uiso 1 1 calc R . .
C28 C 0.7169(3) 0.02736(18) 0.16859(14) 0.0408(9) Uani 1 1 d . . .
H28A H 0.6736 0.0432 0.1364 0.061 Uiso 1 1 calc R . .
H28B H 0.7108 -0.0234 0.1721 0.061 Uiso 1 1 calc R . .
H28C H 0.7860 0.0393 0.1661 0.061 Uiso 1 1 calc R . .
C29 C 0.7283(3) 0.28286(18) 0.10822(13) 0.0402(9) Uani 1 1 d D . .
C30 C 0.6296(4) 0.3228(3) 0.0874(2) 0.0579(16) Uani 0.75 1 d P B 1
H30A H 0.5737 0.2901 0.0840 0.087 Uiso 0.75 1 calc PR B 1
H30B H 0.6339 0.3434 0.0526 0.087 Uiso 0.75 1 calc PR B 1
H30C H 0.6196 0.3600 0.1125 0.087 Uiso 0.75 1 calc PR B 1
C31 C 0.7449(5) 0.2296(3) 0.06597(18) 0.0465(13) Uani 0.75 1 d P B 1
H31A H 0.8038 0.2015 0.0789 0.070 Uiso 0.75 1 calc PR B 1
H31B H 0.7547 0.2541 0.0334 0.070 Uiso 0.75 1 calc PR B 1
H31C H 0.6867 0.1990 0.0584 0.070 Uiso 0.75 1 calc PR B 1
C32 C 0.8137(5) 0.3351(3) 0.1159(2) 0.0538(15) Uani 0.75 1 d P B 1
H32A H 0.8031 0.3693 0.1431 0.081 Uiso 0.75 1 calc PR B 1
H32B H 0.8166 0.3594 0.0824 0.081 Uiso 0.75 1 calc PR B 1
H32C H 0.8764 0.3103 0.1273 0.081 Uiso 0.75 1 calc PR B 1
C33 C 0.4633(2) 0.11623(15) 0.33857(12) 0.0233(6) Uani 1 1 d . . .
C34 C 0.3871(2) 0.11648(16) 0.29480(12) 0.0257(7) Uani 1 1 d . . .
C35 C 0.3553(2) 0.05095(16) 0.27437(12) 0.0278(7) Uani 1 1 d . . .
H35 H 0.3022 0.0497 0.2454 0.033 Uiso 1 1 calc R . .
C36 C 0.3961(2) -0.01243(16) 0.29363(12) 0.0267(7) Uani 1 1 d . . .
C37 C 0.4710(2) -0.00964(16) 0.33714(12) 0.0266(7) Uani 1 1 d . . .
H37 H 0.5000 -0.0519 0.3518 0.032 Uiso 1 1 calc R . .
C38 C 0.5046(2) 0.05381(15) 0.35980(12) 0.0248(7) Uani 1 1 d . . .
C39 C 0.3392(2) 0.18330(17) 0.26835(12) 0.0298(7) Uani 1 1 d . . .
C40 C 0.2644(3) 0.1673(2) 0.21835(15) 0.0466(10) Uani 1 1 d . . .
H40A H 0.2984 0.1436 0.1922 0.070 Uiso 1 1 calc R . .
H40B H 0.2353 0.2111 0.2032 0.070 Uiso 1 1 calc R . .
H40C H 0.2118 0.1370 0.2277 0.070 Uiso 1 1 calc R . .
C41 C 0.2815(3) 0.2210(2) 0.30659(15) 0.0481(10) Uani 1 1 d . . .
H41A H 0.2542 0.2647 0.2904 0.072 Uiso 1 1 calc R . .
H41B H 0.3260 0.2313 0.3397 0.072 Uiso 1 1 calc R . .
H41C H 0.2270 0.1910 0.3142 0.072 Uiso 1 1 calc R . .
C42 C 0.4190(3) 0.23061(19) 0.25138(16) 0.0442(9) Uani 1 1 d . . .
H42A H 0.4582 0.2040 0.2291 0.066 Uiso 1 1 calc R . .
H42B H 0.4627 0.2478 0.2830 0.066 Uiso 1 1 calc R . .
H42C H 0.3873 0.2703 0.2312 0.066 Uiso 1 1 calc R . .
C43 C 0.3563(2) -0.08162(16) 0.26821(13) 0.0304(7) Uani 1 1 d . . .
C44 C 0.2636(3) -0.10103(19) 0.29183(16) 0.0448(9) Uani 1 1 d . . .
H44A H 0.2811 -0.1063 0.3304 0.067 Uiso 1 1 calc R . .
H44B H 0.2365 -0.1452 0.2763 0.067 Uiso 1 1 calc R . .
H44C H 0.2137 -0.0640 0.2839 0.067 Uiso 1 1 calc R . .
C45 C 0.3290(3) -0.07410(19) 0.20776(14) 0.0447(9) Uani 1 1 d . . .
H45A H 0.3079 -0.1196 0.1922 0.067 Uiso 1 1 calc R . .
H45B H 0.3869 -0.0576 0.1930 0.067 Uiso 1 1 calc R . .
H45C H 0.2746 -0.0404 0.1995 0.067 Uiso 1 1 calc R . .
C46 C 0.4328(3) -0.14039(18) 0.27937(15) 0.0435(9) Uani 1 1 d . . .
H46A H 0.4483 -0.1483 0.3178 0.065 Uiso 1 1 calc R . .
H46B H 0.4935 -0.1272 0.2657 0.065 Uiso 1 1 calc R . .
H46C H 0.4056 -0.1833 0.2618 0.065 Uiso 1 1 calc R . .
C47 C 0.5858(2) 0.05504(16) 0.40715(12) 0.0261(7) Uani 1 1 d . . .
H47A H 0.5588 0.0735 0.4382 0.031 Uiso 1 1 calc R . .
H47B H 0.6089 0.0067 0.4155 0.031 Uiso 1 1 calc R . .
C48 C 0.7563(2) 0.06795(15) 0.40388(11) 0.0251(7) Uani 1 1 d . . .
H48 H 0.7569 0.0191 0.4108 0.030 Uiso 1 1 calc R . .
C49 C 0.8506(2) 0.09994(16) 0.40101(12) 0.0268(7) Uani 1 1 d . . .
C50 C 0.9343(2) 0.05527(16) 0.40537(12) 0.0288(7) Uani 1 1 d . . .
H50 H 0.9248 0.0062 0.4073 0.035 Uiso 1 1 calc R . .
C51 C 1.0285(2) 0.08078(16) 0.40682(12) 0.0291(7) Uani 1 1 d . . .
C52 C 1.0381(2) 0.15406(16) 0.40629(12) 0.0287(7) Uani 1 1 d . . .
H52 H 1.1033 0.1727 0.4092 0.034 Uiso 1 1 calc R . .
C53 C 0.9600(2) 0.20098(16) 0.40185(12) 0.0275(7) Uani 1 1 d . . .
C54 C 0.8620(2) 0.17321(15) 0.39765(12) 0.0254(7) Uani 1 1 d . . .
C55 C 1.1201(2) 0.03310(17) 0.41218(13) 0.0329(8) Uani 1 1 d . . .
C56 C 1.1715(3) 0.0343(2) 0.47039(15) 0.0474(10) Uani 1 1 d . . .
H56A H 1.1903 0.0825 0.4807 0.071 Uiso 1 1 calc R . .
H56B H 1.2312 0.0050 0.4743 0.071 Uiso 1 1 calc R . .
H56C H 1.1259 0.0163 0.4933 0.071 Uiso 1 1 calc R . .
C57 C 1.0900(3) -0.04229(19) 0.39564(19) 0.0543(11) Uani 1 1 d . . .
H57A H 1.1498 -0.0702 0.3941 0.082 Uiso 1 1 calc R . .
H57B H 1.0484 -0.0419 0.3606 0.082 Uiso 1 1 calc R . .
H57C H 1.0527 -0.0628 0.4217 0.082 Uiso 1 1 calc R . .
C58 C 1.1941(3) 0.05810(19) 0.37700(14) 0.0396(8) Uani 1 1 d . . .
H58A H 1.2185 0.1047 0.3885 0.059 Uiso 1 1 calc R . .
H58B H 1.1612 0.0602 0.3400 0.059 Uiso 1 1 calc R . .
H58C H 1.2501 0.0254 0.3799 0.059 Uiso 1 1 calc R . .
C59 C 0.9786(2) 0.28067(16) 0.40250(13) 0.0318(7) Uani 1 1 d . . .
C60 C 1.0889(3) 0.29826(18) 0.40491(16) 0.0419(9) Uani 1 1 d . . .
H60A H 1.1267 0.2787 0.4375 0.063 Uiso 1 1 calc R . .
H60B H 1.0974 0.3491 0.4048 0.063 Uiso 1 1 calc R . .
H60C H 1.1130 0.2782 0.3739 0.063 Uiso 1 1 calc R . .
C61 C 0.9221(3) 0.31514(18) 0.35212(15) 0.0414(9) Uani 1 1 d . . .
H61A H 0.9362 0.3654 0.3529 0.062 Uiso 1 1 calc R . .
H61B H 0.8506 0.3077 0.3507 0.062 Uiso 1 1 calc R . .
H61C H 0.9436 0.2942 0.3207 0.062 Uiso 1 1 calc R . .
C62 C 0.9438(3) 0.31195(19) 0.45161(15) 0.0427(9) Uani 1 1 d . . .
H62A H 0.9814 0.2910 0.4837 0.064 Uiso 1 1 calc R . .
H62B H 0.8729 0.3024 0.4504 0.064 Uiso 1 1 calc R . .
H62C H 0.9548 0.3626 0.4522 0.064 Uiso 1 1 calc R . .
C63 C 0.9680(4) 0.1678(3) 0.2561(2) 0.0741(14) Uani 1 1 d . . .
H63A H 1.0292 0.1930 0.2699 0.111 Uiso 1 1 calc R . .
H63B H 0.9419 0.1452 0.2856 0.111 Uiso 1 1 calc R . .
H63C H 0.9186 0.2007 0.2383 0.111 Uiso 1 1 calc R . .
C64 C 0.9898(3) 0.1130(2) 0.21710(17) 0.0552(11) Uani 1 1 d . . .
C65 C 0.9848(4) 0.1308(3) 0.16391(19) 0.0664(13) Uani 1 1 d . . .
H65 H 0.9672 0.1769 0.1521 0.080 Uiso 1 1 calc R . .
C66 C 1.0060(4) 0.0802(3) 0.1282(2) 0.0869(18) Uani 1 1 d . . .
H66 H 1.0033 0.0921 0.0918 0.104 Uiso 1 1 calc R . .
C67 C 1.0309(4) 0.0127(3) 0.1449(3) 0.0879(19) Uani 1 1 d . . .
H67 H 1.0453 -0.0212 0.1199 0.105 Uiso 1 1 calc R . .
C68 C 1.0349(4) -0.0047(3) 0.1952(3) 0.0885(19) Uani 1 1 d . . .
H68 H 1.0452 -0.0524 0.2050 0.106 Uiso 1 1 calc R . .
C69 C 1.0253(2) 0.0399(2) 0.23147(18) 0.0863(19) Uani 1 1 d . . .
H69 H 1.0408 0.0268 0.2678 0.104 Uiso 1 1 calc R . .
C11' C 0.7074(2) 0.5425(2) 0.50381(18) 0.093(7) Uiso 0.25 1 d PRD A 2
H11D H 0.7112 0.5825 0.5280 0.140 Uiso 0.25 1 calc PR C 2
H11E H 0.6418 0.5206 0.5013 0.140 Uiso 0.25 1 calc PR D 2
H11F H 0.7176 0.5585 0.4685 0.140 Uiso 0.25 1 calc PR E 2
C12' C 0.8861(2) 0.4916(2) 0.50190(18) 0.107(8) Uiso 0.25 1 d PRD A 2
H12D H 0.9316 0.5249 0.5223 0.160 Uiso 0.25 1 calc PR F 2
H12E H 0.8715 0.5069 0.4648 0.160 Uiso 0.25 1 calc PR G 2
H12F H 0.9169 0.4452 0.5036 0.160 Uiso 0.25 1 calc PR H 2
C10' C 0.7930(18) 0.4914(12) 0.58592(19) 0.077(6) Uiso 0.25 1 d PD A 2
H10D H 0.8552 0.4706 0.6036 0.115 Uiso 0.25 1 calc PR A 2
H10E H 0.7367 0.4654 0.5958 0.115 Uiso 0.25 1 calc PR A 2
H10F H 0.7894 0.5403 0.5970 0.115 Uiso 0.25 1 calc PR A 2
C30' C 0.6404(14) 0.2622(15) 0.0655(8) 0.111(9) Uiso 0.25 1 d PD B 2
H30D H 0.6316 0.2113 0.0657 0.166 Uiso 0.25 1 calc PR B 2
H30E H 0.6538 0.2770 0.0305 0.166 Uiso 0.25 1 calc PR B 2
H30F H 0.5798 0.2850 0.0731 0.166 Uiso 0.25 1 calc PR B 2
C32' C 0.7516(18) 0.3616(3) 0.1127(9) 0.077(6) Uiso 0.25 1 d PD B 2
H32D H 0.6909 0.3875 0.1163 0.116 Uiso 0.25 1 calc PR B 2
H32E H 0.7767 0.3773 0.0807 0.116 Uiso 0.25 1 calc PR B 2
H32F H 0.8020 0.3702 0.1439 0.116 Uiso 0.25 1 calc PR B 2
C31' C 0.8171(15) 0.2459(14) 0.0896(11) 0.107(8) Uiso 0.25 1 d PD B 2
H31D H 0.8790 0.2688 0.1055 0.161 Uiso 0.25 1 calc PR B 2
H31E H 0.8104 0.2487 0.0508 0.161 Uiso 0.25 1 calc PR B 2
H31F H 0.8185 0.1967 0.1005 0.161 Uiso 0.25 1 calc PR B 2


_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 1.841(2) . ?
Al1 O3 1.843(2) . ?
Al1 C2 1.962(4) . ?
Al1 C1 1.965(4) . ?
O1 C3 1.404(3) . ?
O1 Al2 1.973(2) . ?
N1 C18 1.287(4) . ?
N1 C17 1.481(4) . ?
N1 Al2 2.008(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Al2 O2 1.817(2) . ?
Al2 O4 1.820(2) . ?
Al2 N2 2.005(3) . ?
Al2 O3 2.029(2) . ?
O2 C20 1.322(3) . ?
N2 C48 1.286(4) . ?
N2 C47 1.475(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C33 1.410(3) . ?
C3 C4 1.395(4) . ?
C3 C8 1.400(4) . ?
O4 C54 1.326(4) . ?
C4 C5 1.388(4) . ?
C4 C17 1.506(4) . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(4) . ?
C6 C9 1.537(4) . ?
C7 C8 1.402(4) . ?
C7 H7 0.9500 . ?
C8 C13 1.542(4) . ?
C9 C11 1.531(2) . ?
C9 C12' 1.532(2) . ?
C9 C12 1.532(2) . ?
C9 C10' 1.538(2) . ?
C9 C10 1.550(2) . ?
C9 C11' 1.562(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C16 1.530(5) . ?
C13 C14 1.533(5) . ?
C13 C15 1.532(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.440(4) . ?
C18 H18 0.9500 . ?
C19 C24 1.404(4) . ?
C19 C20 1.420(4) . ?
C20 C21 1.426(4) . ?
C21 C22 1.386(4) . ?
C21 C25 1.542(4) . ?
C22 C23 1.403(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(5) . ?
C23 C29 1.533(4) . ?
C24 H24 0.9500 . ?
C25 C28 1.532(4) . ?
C25 C27 1.532(5) . ?
C25 C26 1.541(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C32 1.524(6) . ?
C29 C31 1.524(6) . ?
C29 C30' 1.539(2) . ?
C29 C32' 1.540(2) . ?
C29 C31' 1.541(2) . ?
C29 C30 1.566(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C38 1.393(4) . ?
C33 C34 1.399(4) . ?
C34 C35 1.400(4) . ?
C34 C39 1.542(4) . ?
C35 C36 1.391(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.386(4) . ?
C36 C43 1.535(4) . ?
C37 C38 1.390(4) . ?
C37 H37 0.9500 . ?
C38 C47 1.505(4) . ?
C39 C41 1.527(5) . ?
C39 C42 1.529(5) . ?
C39 C40 1.533(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.529(5) . ?
C43 C46 1.529(5) . ?
C43 C45 1.534(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.436(4) . ?
C48 H48 0.9500 . ?
C49 C54 1.414(4) . ?
C49 C50 1.415(4) . ?
C50 C51 1.369(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.408(4) . ?
C51 C55 1.535(4) . ?
C52 C53 1.384(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.425(4) . ?
C53 C59 1.545(4) . ?
C55 C58 1.528(5) . ?
C55 C56 1.539(5) . ?
C55 C57 1.540(5) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C62 1.529(5) . ?
C59 C60 1.533(5) . ?
C59 C61 1.538(5) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C64 1.506(6) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 C65 1.389(6) . ?
C64 C69 1.505(6) . ?
C65 C66 1.391(7) . ?
C65 H65 0.9500 . ?
C66 C67 1.385(8) . ?
C66 H66 0.9500 . ?
C67 C68 1.319(8) . ?
C67 H67 0.9500 . ?
C68 C69 1.280(7) . ?
C68 H68 0.9500 . ?
C69 H69 0.9500 . ?
C11' H11D 0.9800 . ?
C11' H11E 0.9800 . ?
C11' H11F 0.9800 . ?
C12' H12D 0.9800 . ?
C12' H12E 0.9800 . ?
C12' H12F 0.9800 . ?
C10' H10D 0.9800 . ?
C10' H10E 0.9800 . ?
C10' H10F 0.9800 . ?
C30' H30D 0.9800 . ?
C30' H30E 0.9800 . ?
C30' H30F 0.9800 . ?
C32' H32D 0.9800 . ?
C32' H32E 0.9800 . ?
C32' H32F 0.9800 . ?
C31' H31D 0.9800 . ?
C31' H31E 0.9800 . ?
C31' H31F 0.9800 . ?

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 O3 81.14(9) . . ?
O1 Al1 C2 110.36(14) . . ?
O3 Al1 C2 121.67(16) . . ?
O1 Al1 C1 120.07(15) . . ?
O3 Al1 C1 111.90(14) . . ?
C2 Al1 C1 109.76(18) . . ?
C3 O1 Al1 125.96(18) . . ?
C3 O1 Al2 120.75(17) . . ?
Al1 O1 Al2 103.75(10) . . ?
C18 N1 C17 115.7(2) . . ?
C18 N1 Al2 122.9(2) . . ?
C17 N1 Al2 121.28(19) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Al2 O4 101.65(10) . . ?
O2 Al2 O1 165.85(10) . . ?
O4 Al2 O1 92.15(10) . . ?
O2 Al2 N2 88.32(10) . . ?
O4 Al2 N2 89.93(10) . . ?
O1 Al2 N2 94.90(10) . . ?
O2 Al2 N1 90.39(10) . . ?
O4 Al2 N1 88.54(10) . . ?
O1 Al2 N1 86.79(10) . . ?
N2 Al2 N1 177.77(11) . . ?
O2 Al2 O3 92.92(9) . . ?
O4 Al2 O3 164.97(10) . . ?
O1 Al2 O3 73.55(9) . . ?
N2 Al2 O3 86.79(9) . . ?
N1 Al2 O3 95.10(10) . . ?
C20 O2 Al2 133.66(19) . . ?
C48 N2 C47 116.6(2) . . ?
C48 N2 Al2 121.5(2) . . ?
C47 N2 Al2 121.46(19) . . ?
Al1 C2 H2A 109.5 . . ?
Al1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Al1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C33 O3 Al1 127.01(18) . . ?
C33 O3 Al2 119.42(17) . . ?
Al1 O3 Al2 101.56(10) . . ?
C4 C3 C8 120.9(3) . . ?
C4 C3 O1 115.8(3) . . ?
C8 C3 O1 123.2(3) . . ?
C54 O4 Al2 130.89(19) . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 C17 119.7(3) . . ?
C3 C4 C17 119.9(3) . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C7 C6 C5 117.0(3) . . ?
C7 C6 C9 120.7(3) . . ?
C5 C6 C9 122.3(3) . . ?
C6 C7 C8 124.8(3) . . ?
C6 C7 H7 117.6 . . ?
C8 C7 H7 117.6 . . ?
C3 C8 C7 115.9(3) . . ?
C3 C8 C13 126.2(3) . . ?
C7 C8 C13 117.8(3) . . ?
C11 C9 C12' 149.1(4) . . ?
C11 C9 C12 115.4(4) . . ?
C12' C9 C12 55.1(3) . . ?
C11 C9 C6 110.3(3) . . ?
C12' C9 C6 99.8(3) . . ?
C12 C9 C6 113.3(3) . . ?
C11 C9 C10' 40.7(9) . . ?
C12' C9 C10' 119.8(9) . . ?
C12 C9 C10' 132.5(9) . . ?
C6 C9 C10' 113.9(9) . . ?
C11 C9 C10 105.8(4) . . ?
C12' C9 C10 56.2(3) . . ?
C12 C9 C10 103.0(4) . . ?
C6 C9 C10 108.3(3) . . ?
C10' C9 C10 66.1(9) . . ?
C11 C9 C11' 64.5(3) . . ?
C12' C9 C11' 116.51(16) . . ?
C12 C9 C11' 61.5(3) . . ?
C6 C9 C11' 102.3(3) . . ?
C10' C9 C11' 103.6(9) . . ?
C10 C9 C11' 149.3(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
C16 C13 C14 105.5(3) . . ?
C16 C13 C15 109.0(3) . . ?
C14 C13 C15 109.6(3) . . ?
C16 C13 C8 111.1(3) . . ?
C14 C13 C8 114.0(3) . . ?
C15 C13 C8 107.6(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C17 C4 114.0(2) . . ?
N1 C17 H17A 108.7 . . ?
C4 C17 H17A 108.7 . . ?
N1 C17 H17B 108.7 . . ?
C4 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
N1 C18 C19 127.4(3) . . ?
N1 C18 H18 116.3 . . ?
C19 C18 H18 116.3 . . ?
C24 C19 C20 121.2(3) . . ?
C24 C19 C18 116.6(3) . . ?
C20 C19 C18 122.0(3) . . ?
O2 C20 C19 120.2(3) . . ?
O2 C20 C21 122.1(3) . . ?
C19 C20 C21 117.7(3) . . ?
C22 C21 C20 118.0(3) . . ?
C22 C21 C25 120.7(3) . . ?
C20 C21 C25 121.2(3) . . ?
C21 C22 C23 125.3(3) . . ?
C21 C22 H22 117.4 . . ?
C23 C22 H22 117.4 . . ?
C24 C23 C22 116.0(3) . . ?
C24 C23 C29 120.7(3) . . ?
C22 C23 C29 123.2(3) . . ?
C23 C24 C19 121.9(3) . . ?
C23 C24 H24 119.1 . . ?
C19 C24 H24 119.1 . . ?
C28 C25 C27 107.2(3) . . ?
C28 C25 C21 112.5(3) . . ?
C27 C25 C21 111.9(3) . . ?
C28 C25 C26 107.8(3) . . ?
C27 C25 C26 109.2(3) . . ?
C21 C25 C26 108.2(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32 C29 C31 109.6(4) . . ?
C32 C29 C23 110.5(3) . . ?
C31 C29 C23 113.0(3) . . ?
C32 C29 C30' 139.0(11) . . ?
C31 C29 C30' 60.9(11) . . ?
C23 C29 C30' 109.6(11) . . ?
C32 C29 C32' 37.3(9) . . ?
C31 C29 C32' 130.8(9) . . ?
C23 C29 C32' 113.4(9) . . ?
C30' C29 C32' 115.6(15) . . ?
C32 C29 C31' 73.7(12) . . ?
C31 C29 C31' 42.7(11) . . ?
C23 C29 C31' 106.2(11) . . ?
C30' C29 C31' 103.1(16) . . ?
C32' C29 C31' 108.0(15) . . ?
C32 C29 C30 108.8(4) . . ?
C31 C29 C30 107.5(4) . . ?
C23 C29 C30 107.4(3) . . ?
C30' C29 C30 49.7(11) . . ?
C32' C29 C30 72.7(10) . . ?
C31' C29 C30 142.6(11) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
C38 C33 C34 121.1(3) . . ?
C38 C33 O3 116.3(3) . . ?
C34 C33 O3 122.5(3) . . ?
C33 C34 C35 116.2(3) . . ?
C33 C34 C39 124.2(3) . . ?
C35 C34 C39 119.6(3) . . ?
C36 C35 C34 124.5(3) . . ?
C36 C35 H35 117.8 . . ?
C34 C35 H35 117.8 . . ?
C37 C36 C35 116.9(3) . . ?
C37 C36 C43 122.6(3) . . ?
C35 C36 C43 120.5(3) . . ?
C36 C37 C38 121.3(3) . . ?
C36 C37 H37 119.4 . . ?
C38 C37 H37 119.4 . . ?
C37 C38 C33 120.0(3) . . ?
C37 C38 C47 120.0(3) . . ?
C33 C38 C47 120.0(3) . . ?
C41 C39 C42 111.3(3) . . ?
C41 C39 C40 106.4(3) . . ?
C42 C39 C40 107.0(3) . . ?
C41 C39 C34 109.7(3) . . ?
C42 C39 C34 110.1(3) . . ?
C40 C39 C34 112.3(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C46 109.3(3) . . ?
C44 C43 C36 107.6(3) . . ?
C46 C43 C36 111.7(3) . . ?
C44 C43 C45 109.4(3) . . ?
C46 C43 C45 107.9(3) . . ?
C36 C43 C45 110.9(3) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N2 C47 C38 112.4(2) . . ?
N2 C47 H47A 109.1 . . ?
C38 C47 H47A 109.1 . . ?
N2 C47 H47B 109.1 . . ?
C38 C47 H47B 109.1 . . ?
H47A C47 H47B 107.9 . . ?
N2 C48 C49 126.9(3) . . ?
N2 C48 H48 116.5 . . ?
C49 C48 H48 116.5 . . ?
C54 C49 C50 120.6(3) . . ?
C54 C49 C48 122.2(3) . . ?
C50 C49 C48 117.1(3) . . ?
C51 C50 C49 121.9(3) . . ?
C51 C50 H50 119.1 . . ?
C49 C50 H50 119.1 . . ?
C50 C51 C52 116.3(3) . . ?
C50 C51 C55 122.5(3) . . ?
C52 C51 C55 121.1(3) . . ?
C53 C52 C51 125.1(3) . . ?
C53 C52 H52 117.4 . . ?
C51 C52 H52 117.4 . . ?
C52 C53 C54 117.7(3) . . ?
C52 C53 C59 121.1(3) . . ?
C54 C53 C59 121.2(3) . . ?
O4 C54 C49 119.9(3) . . ?
O4 C54 C53 121.7(3) . . ?
C49 C54 C53 118.4(3) . . ?
C58 C55 C51 111.4(3) . . ?
C58 C55 C56 108.6(3) . . ?
C51 C55 C56 108.5(3) . . ?
C58 C55 C57 107.7(3) . . ?
C51 C55 C57 110.7(3) . . ?
C56 C55 C57 109.9(3) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C62 C59 C60 108.0(3) . . ?
C62 C59 C61 109.7(3) . . ?
C60 C59 C61 107.4(3) . . ?
C62 C59 C53 108.9(3) . . ?
C60 C59 C53 112.0(3) . . ?
C61 C59 C53 110.8(3) . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C64 C63 H63A 109.5 . . ?
C64 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C64 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C65 C64 C63 119.3(5) . . ?
C65 C64 C69 115.4(4) . . ?
C63 C64 C69 125.1(4) . . ?
C64 C65 C66 119.1(5) . . ?
C64 C65 H65 120.5 . . ?
C66 C65 H65 120.5 . . ?
C67 C66 C65 120.9(6) . . ?
C67 C66 H66 119.6 . . ?
C65 C66 H66 119.6 . . ?
C68 C67 C66 120.4(6) . . ?
C68 C67 H67 119.8 . . ?
C66 C67 H67 119.8 . . ?
C69 C68 C67 122.7(6) . . ?
C69 C68 H68 118.6 . . ?
C67 C68 H68 118.6 . . ?
C68 C69 C64 120.6(5) . . ?
C68 C69 H69 119.7 . . ?
C64 C69 H69 119.7 . . ?
C9 C11' H11D 109.5 . . ?
C9 C11' H11E 109.5 . . ?
H11D C11' H11E 109.5 . . ?
C9 C11' H11F 109.5 . . ?
H11D C11' H11F 109.5 . . ?
H11E C11' H11F 109.5 . . ?
C9 C12' H12D 109.5 . . ?
C9 C12' H12E 109.5 . . ?
H12D C12' H12E 109.5 . . ?
C9 C12' H12F 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 109.5 . . ?
C9 C10' H10D 109.5 . . ?
C9 C10' H10E 109.5 . . ?
H10D C10' H10E 109.5 . . ?
C9 C10' H10F 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?
C29 C30' H30D 109.5 . . ?
C29 C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C29 C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
C29 C32' H32D 109.5 . . ?
C29 C32' H32E 109.5 . . ?
H32D C32' H32E 109.5 . . ?
C29 C32' H32F 109.5 . . ?
H32D C32' H32F 109.5 . . ?
H32E C32' H32F 109.5 . . ?
C29 C31' H31D 109.5 . . ?
C29 C31' H31E 109.5 . . ?
H31D C31' H31E 109.5 . . ?
C29 C31' H31F 109.5 . . ?
H31D C31' H31F 109.5 . . ?
H31E C31' H31F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.057
####################################################################### 
# 
# 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_1H2
_database_code_depnum_ccdc_archive 'CCDC 1037367'
_audit_update_record             
;
2014-12-03 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H13 N O2'
_chemical_formula_weight         227.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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                   22.3830(16)
_cell_length_b                   5.7810(5)
_cell_length_c                   17.8440(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.915(4)
_cell_angle_gamma                90.00
_cell_volume                     2274.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7670
_cell_measurement_theta_min      3.51
_cell_measurement_theta_max      25.03

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'nonius kappa ccd'
_diffrn_measurement_method       ccd
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11736
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.64
_diffrn_reflns_theta_max         25.03
_reflns_number_total             2008
_reflns_number_gt                1657
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_structure_solution    
;
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
 (1999) J. Appl. Cryst. 32, 115-119.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0425P)²+1.1002P] 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_number_reflns         2008
_refine_ls_number_parameters     166
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
O1 O 0.71060(4) -0.10129(16) 0.59858(5) 0.0322(3) Uani 1 1 d . . .
N1 N 0.78687(5) 0.2365(2) 0.60631(6) 0.0271(3) Uani 1 1 d . . .
C1 C 0.68246(6) 0.0126(2) 0.64483(7) 0.0267(3) Uani 1 1 d . . .
O2 O 0.81908(4) -0.05007(17) 0.48999(5) 0.0323(3) Uani 1 1 d . . .
C2 C 0.62910(6) -0.0728(3) 0.66787(8) 0.0320(3) Uani 1 1 d . . .
H2 H 0.6130 -0.2175 0.6489 0.038 Uiso 1 1 calc R . .
C3 C 0.60028(6) 0.0494(3) 0.71696(8) 0.0348(4) Uani 1 1 d . . .
H3 H 0.5642 -0.0116 0.7305 0.042 Uiso 1 1 calc R . .
C4 C 0.62251(7) 0.2618(3) 0.74776(8) 0.0354(4) Uani 1 1 d . . .
H4 H 0.6025 0.3424 0.7827 0.043 Uiso 1 1 calc R . .
C5 C 0.67384(6) 0.3508(2) 0.72627(8) 0.0316(3) Uani 1 1 d . . .
H5 H 0.6891 0.4954 0.7464 0.038 Uiso 1 1 calc R . .
C6 C 0.70437(6) 0.2324(2) 0.67504(7) 0.0263(3) Uani 1 1 d . . .
C7 C 0.75615(6) 0.3363(2) 0.65215(8) 0.0274(3) Uani 1 1 d . . .
C8 C 0.83871(6) 0.3395(2) 0.57778(8) 0.0298(3) Uani 1 1 d . . .
H8A H 0.8548 0.4713 0.6106 0.036 Uiso 1 1 calc R . .
H8B H 0.8252 0.3991 0.5256 0.036 Uiso 1 1 calc R . .
C9 C 0.88816(6) 0.1628(2) 0.57708(7) 0.0277(3) Uani 1 1 d . . .
C10 C 0.94534(6) 0.1871(3) 0.62111(8) 0.0336(3) Uani 1 1 d . . .
H10 H 0.9542 0.3206 0.6520 0.040 Uiso 1 1 calc R . .
C11 C 0.98972(6) 0.0203(3) 0.62076(9) 0.0383(4) Uani 1 1 d . . .
H11 H 1.0285 0.0387 0.6516 0.046 Uiso 1 1 calc R . .
C12 C 0.97709(6) -0.1733(3) 0.57517(9) 0.0372(4) Uani 1 1 d . . .
H12 H 1.0074 -0.2882 0.5747 0.045 Uiso 1 1 calc R . .
C13 C 0.92044(6) -0.2006(2) 0.53006(8) 0.0316(3) Uani 1 1 d . . .
H13 H 0.9122 -0.3332 0.4985 0.038 Uiso 1 1 calc R . .
C14 C 0.87592(6) -0.0343(2) 0.53112(7) 0.0275(3) Uani 1 1 d . . .
H7 H 0.7694(6) 0.490(3) 0.6713(8) 0.030(4) Uiso 1 1 d . . .
H1' H 0.7719(8) 0.090(3) 0.5872(10) 0.050(5) Uiso 1 1 d . . .
H2' H 0.8142(8) -0.183(3) 0.4581(11) 0.057(5) Uiso 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
O1 C1 1.3001(16) . ?
N1 C7 1.2915(18) . ?
N1 C8 1.4710(16) . ?
N1 H1' 0.955(19) . ?
C1 C2 1.4172(19) . ?
C1 C6 1.4334(19) . ?
O2 C14 1.3580(16) . ?
O2 H2' 0.95(2) . ?
C2 C3 1.370(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.401(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.4091(19) . ?
C5 H5 0.9500 . ?
C6 C7 1.4262(19) . ?
C7 H7 0.978(15) . ?
C8 C9 1.5082(19) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.3888(19) . ?
C9 C14 1.4028(19) . ?
C10 C11 1.385(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.3873(19) . ?
C13 H13 0.9500 . ?

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
C7 N1 C8 125.18(12) . . ?
C7 N1 H1' 115.6(10) . . ?
C8 N1 H1' 119.0(10) . . ?
O1 C1 C2 122.17(12) . . ?
O1 C1 C6 121.06(12) . . ?
C2 C1 C6 116.77(12) . . ?
C14 O2 H2' 112.2(11) . . ?
C3 C2 C1 121.26(13) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 121.88(13) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C5 C4 C3 118.47(13) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 121.47(13) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C7 119.34(12) . . ?
C5 C6 C1 120.12(12) . . ?
C7 C6 C1 120.52(12) . . ?
N1 C7 C6 122.74(13) . . ?
N1 C7 H7 117.7(8) . . ?
C6 C7 H7 119.6(8) . . ?
N1 C8 C9 110.63(11) . . ?
N1 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C14 118.77(13) . . ?
C10 C9 C8 122.20(13) . . ?
C14 C9 C8 119.03(12) . . ?
C11 C10 C9 121.25(14) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C12 C11 C10 119.44(13) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 120.42(14) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 119.96(14) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
O2 C14 C13 123.67(12) . . ?
O2 C14 C9 116.17(12) . . ?
C13 C14 C9 120.15(12) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2' O1 0.95(2) 1.64(2) 2.5768(13) 167.1(17) 7_646
N1 H1' O1 0.955(19) 1.800(18) 2.5818(14) 137.0(15) .
N1 H1' O2 0.955(19) 2.324(17) 2.8439(15) 113.6(13) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.044
####################################################################### 
# 
# 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_2H2
_database_code_depnum_ccdc_archive 'CCDC 1037368'
_audit_update_record             
;
2014-12-03 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H17 N O2'
_chemical_formula_weight         255.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

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

_cell_length_a                   9.5050(2)
_cell_length_b                   11.2580(2)
_cell_length_c                   13.5330(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.0580(10)
_cell_angle_gamma                90.00
_cell_volume                     1368.76(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    15282
_cell_measurement_theta_min      3.51
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             544
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'nonius kappa ccd'
_diffrn_measurement_method       ccd
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25556
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.62
_diffrn_reflns_theta_max         27.49
_reflns_number_total             3133
_reflns_number_gt                2338
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_structure_solution    
;
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
 (1999) J. Appl. Cryst. 32, 115-119.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0561P)²+0.3301P] 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_number_reflns         3133
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1182
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
O1 O 0.66391(12) 0.08667(9) 1.08373(8) 0.0311(3) Uani 1 1 d . . .
N1 N 0.65220(13) 0.19971(11) 0.88248(9) 0.0246(3) Uani 1 1 d . . .
C1 C 0.64634(15) 0.20150(12) 1.10818(11) 0.0245(3) Uani 1 1 d . . .
O2 O 0.40886(11) 0.07924(9) 0.80723(7) 0.0263(2) Uani 1 1 d . . .
C2 C 0.57865(16) 0.23411(14) 1.18135(11) 0.0271(3) Uani 1 1 d . . .
H2 H 0.5437 0.1750 1.2177 0.033 Uiso 1 1 calc R . .
C3 C 0.56269(17) 0.35334(14) 1.20060(12) 0.0324(4) Uani 1 1 d . . .
H3 H 0.5167 0.3756 1.2505 0.039 Uiso 1 1 calc R . .
C4 C 0.61294(18) 0.44058(14) 1.14814(12) 0.0357(4) Uani 1 1 d . . .
H4 H 0.6020 0.5221 1.1622 0.043 Uiso 1 1 calc R . .
C5 C 0.67952(17) 0.40783(13) 1.07466(12) 0.0307(3) Uani 1 1 d . . .
H5 H 0.7133 0.4675 1.0381 0.037 Uiso 1 1 calc R . .
C6 C 0.69708(15) 0.28906(13) 1.05429(10) 0.0239(3) Uani 1 1 d . . .
C7 C 0.76629(16) 0.25046(13) 0.97388(10) 0.0256(3) Uani 1 1 d . . .
H7A H 0.8135 0.3195 0.9520 0.031 Uiso 1 1 calc R . .
H7B H 0.8444 0.1905 1.0048 0.031 Uiso 1 1 calc R . .
C8 C 0.64550(16) 0.21676(13) 0.78609(11) 0.0258(3) Uani 1 1 d . . .
H8 H 0.7201 0.2644 0.7732 0.031 Uiso 1 1 calc R . .
C9 C 0.53253(16) 0.16795(13) 0.69886(11) 0.0249(3) Uani 1 1 d . . .
C10 C 0.53891(17) 0.18878(13) 0.59705(11) 0.0276(3) Uani 1 1 d . . .
H10 H 0.6193 0.2335 0.5892 0.033 Uiso 1 1 calc R . .
C11 C 0.43189(17) 0.14589(13) 0.50979(11) 0.0279(3) Uani 1 1 d . . .
C12 C 0.31345(16) 0.08105(12) 0.52520(11) 0.0279(3) Uani 1 1 d . . .
H12 H 0.2376 0.0521 0.4652 0.033 Uiso 1 1 calc R . .
C13 C 0.30147(16) 0.05727(12) 0.62207(11) 0.0260(3) Uani 1 1 d . . .
C14 C 0.41442(15) 0.09942(12) 0.71375(11) 0.0229(3) Uani 1 1 d . . .
C15 C 0.43933(19) 0.16476(15) 0.40123(11) 0.0334(4) Uani 1 1 d . . .
H15A H 0.5305 0.2082 0.4056 0.050 Uiso 1 1 calc R . .
H15B H 0.3526 0.2107 0.3598 0.050 Uiso 1 1 calc R . .
H15C H 0.4398 0.0876 0.3678 0.050 Uiso 1 1 calc R . .
C16 C 0.17343(17) -0.01257(15) 0.63470(13) 0.0355(4) Uani 1 1 d . . .
H16A H 0.1104 0.0400 0.6600 0.053 Uiso 1 1 calc R . .
H16B H 0.2119 -0.0768 0.6852 0.053 Uiso 1 1 calc R . .
H16C H 0.1146 -0.0464 0.5671 0.053 Uiso 1 1 calc R . .
H1B H 0.575(2) 0.1505(17) 0.8905(14) 0.045(5) Uiso 1 1 d . . .
H1A H 0.640(2) 0.036(2) 1.1297(16) 0.059(6) Uiso 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
O1 C1 1.3582(17) . ?
O1 H1A 0.93(2) . ?
N1 C8 1.2994(18) . ?
N1 C7 1.4685(18) . ?
N1 H1B 0.95(2) . ?
C1 C2 1.395(2) . ?
C1 C6 1.402(2) . ?
O2 C14 1.3033(16) . ?
C2 C3 1.385(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.5078(19) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.422(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.4182(19) . ?
C9 C14 1.430(2) . ?
C10 C11 1.370(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.413(2) . ?
C11 C15 1.509(2) . ?
C12 C13 1.379(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.431(2) . ?
C13 C16 1.505(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

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
C1 O1 H1A 110.2(13) . . ?
C8 N1 C7 124.66(12) . . ?
C8 N1 H1B 114.4(11) . . ?
C7 N1 H1B 121.0(11) . . ?
O1 C1 C2 123.05(13) . . ?
O1 C1 C6 116.87(12) . . ?
C2 C1 C6 120.06(13) . . ?
C3 C2 C1 119.53(14) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 120.89(14) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 119.47(15) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 120.67(14) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C1 119.37(13) . . ?
C5 C6 C7 122.06(13) . . ?
C1 C6 C7 118.56(13) . . ?
N1 C7 C6 110.11(11) . . ?
N1 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 . . ?
N1 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
N1 C8 C9 123.55(13) . . ?
N1 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C10 C9 C8 118.85(13) . . ?
C10 C9 C14 120.72(13) . . ?
C8 C9 C14 120.43(12) . . ?
C11 C10 C9 121.59(14) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C12 117.24(13) . . ?
C10 C11 C15 122.14(14) . . ?
C12 C11 C15 120.62(13) . . ?
C13 C12 C11 123.90(13) . . ?
C13 C12 H12 118.1 . . ?
C11 C12 H12 118.1 . . ?
C12 C13 C14 119.25(13) . . ?
C12 C13 C16 122.03(13) . . ?
C14 C13 C16 118.72(13) . . ?
O2 C14 C9 120.90(12) . . ?
O2 C14 C13 121.81(12) . . ?
C9 C14 C13 117.27(12) . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.046
####################################################################### 
# 
# 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_4H2
_database_code_depnum_ccdc_archive 'CCDC 1037369'
_audit_update_record             
;
2014-12-03 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H11 Cl2 N O2'
_chemical_formula_weight         296.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   8.0410(5)
_cell_length_b                   8.6470(6)
_cell_length_c                   18.7420(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.121(4)
_cell_angle_gamma                90.00
_cell_volume                     1297.94(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    16496
_cell_measurement_theta_min      3.51
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'nonius kappa ccd'
_diffrn_measurement_method       ccd
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21524
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.57
_diffrn_reflns_theta_max         27.44
_reflns_number_total             2946
_reflns_number_gt                2442
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_structure_solution    
;
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
 (1999) J. Appl. Cryst. 32, 115-119.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0497P)²+0.5404P] 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_number_reflns         2946
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0857
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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
Cl1 Cl 0.16672(6) -0.40680(5) 0.54231(2) 0.03194(13) Uani 1 1 d . . .
O1 O 0.38722(16) 0.57636(14) 0.39623(7) 0.0306(3) Uani 1 1 d . . .
N1 N 0.22036(18) 0.26343(16) 0.40929(8) 0.0264(3) Uani 1 1 d . . .
C1 C 0.4372(2) 0.50592(19) 0.33739(9) 0.0251(4) Uani 1 1 d . . .
Cl2 Cl 0.52948(5) 0.06325(5) 0.66369(2) 0.02845(13) Uani 1 1 d . . .
O2 O 0.38488(15) 0.24076(13) 0.53656(6) 0.0283(3) Uani 1 1 d . . .
C2 C 0.5848(2) 0.5432(2) 0.30730(10) 0.0316(4) Uani 1 1 d . . .
H2 H 0.6541 0.6244 0.3270 0.038 Uiso 1 1 calc R . .
C3 C 0.6293(3) 0.4609(3) 0.24847(10) 0.0393(5) Uani 1 1 d . . .
H3 H 0.7302 0.4856 0.2282 0.047 Uiso 1 1 calc R . .
C4 C 0.5287(3) 0.3429(3) 0.21869(10) 0.0407(5) Uani 1 1 d . . .
H4 H 0.5608 0.2866 0.1786 0.049 Uiso 1 1 calc R . .
C5 C 0.3811(2) 0.3080(2) 0.24790(9) 0.0336(4) Uani 1 1 d . . .
H5 H 0.3114 0.2281 0.2273 0.040 Uiso 1 1 calc R . .
C6 C 0.3333(2) 0.38862(19) 0.30723(9) 0.0260(4) Uani 1 1 d . . .
C7 C 0.1775(2) 0.3488(2) 0.34211(9) 0.0299(4) Uani 1 1 d . . .
H7A H 0.1169 0.4448 0.3524 0.036 Uiso 1 1 calc R . .
H7B H 0.1033 0.2847 0.3091 0.036 Uiso 1 1 calc R . .
C8 C 0.1795(2) 0.1206(2) 0.41869(9) 0.0255(4) Uani 1 1 d . . .
C9 C 0.2312(2) 0.03205(19) 0.48067(8) 0.0230(3) Uani 1 1 d . . .
C10 C 0.3395(2) 0.09941(18) 0.53768(9) 0.0225(3) Uani 1 1 d . . .
C11 C 0.3906(2) -0.00587(19) 0.59464(9) 0.0228(3) Uani 1 1 d . . .
C12 C 0.3375(2) -0.15628(19) 0.59645(8) 0.0237(3) Uani 1 1 d . . .
H12 H 0.3731 -0.2206 0.6360 0.028 Uiso 1 1 calc R . .
C13 C 0.2302(2) -0.21494(19) 0.53976(9) 0.0243(3) Uani 1 1 d . . .
C14 C 0.1793(2) -0.12383(19) 0.48262(9) 0.0250(3) Uani 1 1 d . . .
H14 H 0.1086 -0.1653 0.4440 0.030 Uiso 1 1 calc R . .
H8 H 0.1066 0.0805 0.3787 0.039(6) Uiso 1 1 d R . .
H1A H 0.2768 0.3150 0.4461 0.046(6) Uiso 1 1 d R . .
H1B H 0.4623 0.6546 0.4137 0.064(8) Uiso 1 1 d R . .


_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
Cl1 C13 1.7376(17) . ?
O1 C1 1.352(2) . ?
O1 H1B 0.9458 . ?
N1 C8 1.294(2) . ?
N1 C7 1.473(2) . ?
N1 H1A 0.9085 . ?
C1 C6 1.401(2) . ?
C1 C2 1.396(2) . ?
Cl2 C11 1.7379(16) . ?
O2 C10 1.276(2) . ?
C2 C3 1.386(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.395(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.504(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.422(2) . ?
C8 H8 0.9738 . ?
C9 C14 1.413(2) . ?
C9 C10 1.440(2) . ?
C10 C11 1.435(2) . ?
C11 C12 1.370(2) . ?
C12 C13 1.402(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.363(2) . ?
C14 H14 0.9500 . ?

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
C1 O1 H1B 112.2 . . ?
C8 N1 C7 123.46(14) . . ?
C8 N1 H1A 118.8 . . ?
C7 N1 H1A 117.8 . . ?
O1 C1 C6 116.44(15) . . ?
O1 C1 C2 123.41(16) . . ?
C6 C1 C2 120.14(16) . . ?
C3 C2 C1 119.46(18) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.96(18) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 119.41(18) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.90(18) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.11(17) . . ?
C5 C6 C7 122.11(16) . . ?
C1 C6 C7 118.72(15) . . ?
N1 C7 C6 110.23(14) . . ?
N1 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 . . ?
N1 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
N1 C8 C9 124.45(15) . . ?
N1 C8 H8 112.2 . . ?
C9 C8 H8 123.3 . . ?
C14 C9 C8 117.99(15) . . ?
C14 C9 C10 121.83(15) . . ?
C8 C9 C10 120.11(15) . . ?
O2 C10 C11 123.81(15) . . ?
O2 C10 C9 122.01(15) . . ?
C11 C10 C9 114.18(14) . . ?
C12 C11 C10 123.45(15) . . ?
C12 C11 Cl2 119.27(12) . . ?
C10 C11 Cl2 117.27(12) . . ?
C11 C12 C13 119.78(15) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 120.51(15) . . ?
C14 C13 Cl1 120.35(13) . . ?
C12 C13 Cl1 119.13(13) . . ?
C13 C14 C9 120.21(15) . . ?
C13 C14 H14 119.9 . . ?
C9 C14 H14 119.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1B O2 0.95 1.73 2.6520(16) 164.0 3_666
O1 H1B Cl2 0.95 2.84 3.3993(13) 118.7 3_666
N1 H1A O2 0.91 1.94 2.6297(18) 130.9 .

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.070
####################################################################### 
# 
# 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_5H2
_database_code_depnum_ccdc_archive 'CCDC 1037370'
_audit_update_record             
;
2014-12-03 deposited with the CCDC.
2015-01-06 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 H45 N O2'
_chemical_formula_weight         451.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   9.96000(10)
_cell_length_b                   24.2760(3)
_cell_length_c                   12.2260(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.9810(10)
_cell_angle_gamma                90.00
_cell_volume                     2855.64(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'nonius kappa ccd'
_diffrn_measurement_method       ccd
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38743
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.55
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6517
_reflns_number_gt                5218
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_structure_solution    
;
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
 (1999) J. Appl. Cryst. 32, 115-119.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0690P)²+0.9460P] 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_number_reflns         6517
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1392
_refine_ls_wR_factor_gt          0.1286
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
O1 O 0.21416(12) 0.59253(5) 0.62954(10) 0.0405(3) Uani 1 1 d . . .
N1 N 0.48865(12) 0.56860(4) 0.57843(9) 0.0233(2) Uani 1 1 d . . .
C1 C 0.29754(14) 0.62996(5) 0.70111(11) 0.0253(3) Uani 1 1 d . . .
O2 O 0.35754(9) 0.57858(4) 0.36333(8) 0.0260(2) Uani 1 1 d . . .
C2 C 0.23681(14) 0.67639(5) 0.73710(11) 0.0270(3) Uani 1 1 d . . .
C3 C 0.32658(14) 0.71258(5) 0.80982(11) 0.0260(3) Uani 1 1 d . . .
H3 H 0.2874 0.7439 0.8363 0.031 Uiso 1 1 calc R . .
C4 C 0.46997(14) 0.70550(5) 0.84585(10) 0.0236(3) Uani 1 1 d . . .
C5 C 0.52497(13) 0.65904(5) 0.80605(10) 0.0235(3) Uani 1 1 d . . .
H5 H 0.6227 0.6535 0.8271 0.028 Uiso 1 1 calc R . .
C6 C 0.44037(14) 0.62073(5) 0.73642(10) 0.0226(3) Uani 1 1 d . . .
C7 C 0.08050(16) 0.68815(7) 0.69597(14) 0.0419(4) Uani 1 1 d . . .
C8 C 0.0446(2) 0.69804(11) 0.56671(17) 0.0730(7) Uani 1 1 d . . .
H8A H 0.0716 0.6657 0.5293 0.109 Uiso 1 1 calc R . .
H8B H 0.0951 0.7304 0.5507 0.109 Uiso 1 1 calc R . .
H8C H -0.0556 0.7042 0.5381 0.109 Uiso 1 1 calc R . .
C9 C -0.00415(19) 0.64045(9) 0.7239(2) 0.0728(7) Uani 1 1 d . . .
H9A H 0.0154 0.6070 0.6858 0.109 Uiso 1 1 calc R . .
H9B H -0.1034 0.6492 0.6980 0.109 Uiso 1 1 calc R . .
H9C H 0.0210 0.6344 0.8059 0.109 Uiso 1 1 calc R . .
C10 C 0.03952(18) 0.74005(8) 0.75058(17) 0.0535(5) Uani 1 1 d . . .
H10A H -0.0607 0.7462 0.7222 0.080 Uiso 1 1 calc R . .
H10B H 0.0899 0.7718 0.7316 0.080 Uiso 1 1 calc R . .
H10C H 0.0631 0.7354 0.8330 0.080 Uiso 1 1 calc R . .
C11 C 0.56540(15) 0.74691(5) 0.92391(12) 0.0299(3) Uani 1 1 d . . .
C12 C 0.48351(18) 0.78782(7) 0.97736(14) 0.0437(4) Uani 1 1 d . . .
H12A H 0.4272 0.7675 1.0188 0.066 Uiso 1 1 calc R . .
H12B H 0.4226 0.8100 0.9177 0.066 Uiso 1 1 calc R . .
H12C H 0.5484 0.8121 1.0297 0.066 Uiso 1 1 calc R . .
C13 C 0.64671(17) 0.77944(7) 0.85428(14) 0.0413(4) Uani 1 1 d . . .
H13A H 0.7067 0.8065 0.9031 0.062 Uiso 1 1 calc R . .
H13B H 0.5814 0.7985 0.7921 0.062 Uiso 1 1 calc R . .
H13C H 0.7039 0.7540 0.8233 0.062 Uiso 1 1 calc R . .
C14 C 0.66777(18) 0.71670(7) 1.02073(13) 0.0416(4) Uani 1 1 d . . .
H14A H 0.6159 0.6952 1.0641 0.062 Uiso 1 1 calc R . .
H14B H 0.7268 0.7436 1.0706 0.062 Uiso 1 1 calc R . .
H14C H 0.7260 0.6919 0.9893 0.062 Uiso 1 1 calc R . .
C15 C 0.50181(15) 0.56893(5) 0.70103(11) 0.0262(3) Uani 1 1 d . . .
H15A H 0.6012 0.5664 0.7422 0.031 Uiso 1 1 calc R . .
H15B H 0.4535 0.5364 0.7215 0.031 Uiso 1 1 calc R . .
C16 C 0.59987(13) 0.56333(5) 0.54588(10) 0.0223(3) Uani 1 1 d . . .
H16 H 0.6848 0.5580 0.6019 0.027 Uiso 1 1 calc R . .
C17 C 0.60381(13) 0.56510(5) 0.42742(10) 0.0203(3) Uani 1 1 d . . .
C18 C 0.73306(13) 0.55924(5) 0.40269(10) 0.0213(3) Uani 1 1 d . . .
H18 H 0.8138 0.5530 0.4627 0.026 Uiso 1 1 calc R . .
C19 C 0.74533(13) 0.56233(5) 0.29286(10) 0.0207(3) Uani 1 1 d . . .
C20 C 0.62232(13) 0.57154(5) 0.20730(10) 0.0213(3) Uani 1 1 d . . .
H20 H 0.6296 0.5742 0.1315 0.026 Uiso 1 1 calc R . .
C21 C 0.49088(13) 0.57698(5) 0.22583(10) 0.0199(2) Uani 1 1 d . . .
C22 C 0.48282(12) 0.57364(5) 0.33929(10) 0.0198(2) Uani 1 1 d . . .
C23 C 0.88539(13) 0.55817(6) 0.26281(11) 0.0247(3) Uani 1 1 d . . .
C24 C 0.92483(18) 0.61519(7) 0.22924(17) 0.0484(4) Uani 1 1 d . . .
H24A H 0.8544 0.6279 0.1623 0.073 Uiso 1 1 calc R . .
H24B H 1.0154 0.6134 0.2119 0.073 Uiso 1 1 calc R . .
H24C H 0.9300 0.6409 0.2920 0.073 Uiso 1 1 calc R . .
C25 C 1.00121(14) 0.53754(7) 0.36297(13) 0.0359(3) Uani 1 1 d . . .
H25A H 1.0161 0.5643 0.4250 0.054 Uiso 1 1 calc R . .
H25B H 1.0873 0.5331 0.3391 0.054 Uiso 1 1 calc R . .
H25C H 0.9743 0.5020 0.3888 0.054 Uiso 1 1 calc R . .
C26 C 0.87364(16) 0.51692(8) 0.16580(14) 0.0450(4) Uani 1 1 d . . .
H26A H 0.8454 0.4809 0.1885 0.067 Uiso 1 1 calc R . .
H26B H 0.9639 0.5135 0.1483 0.067 Uiso 1 1 calc R . .
H26C H 0.8041 0.5300 0.0986 0.067 Uiso 1 1 calc R . .
C27 C 0.36057(13) 0.58648(5) 0.12780(11) 0.0236(3) Uani 1 1 d . . .
C28 C 0.39462(14) 0.58624(6) 0.01220(11) 0.0297(3) Uani 1 1 d . . .
H28A H 0.3094 0.5927 -0.0478 0.045 Uiso 1 1 calc R . .
H28B H 0.4341 0.5505 0.0002 0.045 Uiso 1 1 calc R . .
H28C H 0.4620 0.6154 0.0104 0.045 Uiso 1 1 calc R . .
C29 C 0.25428(14) 0.54014(6) 0.12512(11) 0.0300(3) Uani 1 1 d . . .
H29A H 0.2300 0.5389 0.1978 0.045 Uiso 1 1 calc R . .
H29B H 0.2947 0.5048 0.1117 0.045 Uiso 1 1 calc R . .
H29C H 0.1705 0.5473 0.0642 0.045 Uiso 1 1 calc R . .
C30 C 0.29546(15) 0.64262(6) 0.14214(13) 0.0342(3) Uani 1 1 d . . .
H30A H 0.2696 0.6433 0.2142 0.051 Uiso 1 1 calc R . .
H30B H 0.2124 0.6484 0.0797 0.051 Uiso 1 1 calc R . .
H30C H 0.3629 0.6720 0.1416 0.051 Uiso 1 1 calc R . .
H1 H 0.283(3) 0.5676(10) 0.604(2) 0.084(8) Uiso 1 1 d . . .
H2 H 0.374(2) 0.5771(8) 0.4415(17) 0.047(5) Uiso 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
O1 C1 1.3803(16) . ?
O1 H1 1.02(3) . ?
N1 C16 1.2765(17) . ?
N1 C15 1.4705(15) . ?
C1 C6 1.3939(19) . ?
C1 C2 1.4026(18) . ?
O2 C22 1.3592(15) . ?
O2 H2 0.93(2) . ?
C2 C3 1.3968(18) . ?
C2 C7 1.5341(19) . ?
C3 C4 1.3921(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.3953(18) . ?
C4 C11 1.5348(18) . ?
C5 C6 1.3888(18) . ?
C5 H5 0.9500 . ?
C6 C15 1.5098(17) . ?
C7 C9 1.522(3) . ?
C7 C10 1.530(2) . ?
C7 C8 1.546(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.534(2) . ?
C11 C14 1.535(2) . ?
C11 C13 1.536(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.4595(17) . ?
C16 H16 0.9500 . ?
C17 C18 1.4036(17) . ?
C17 C22 1.4089(17) . ?
C18 C19 1.3816(17) . ?
C18 H18 0.9500 . ?
C19 C20 1.4081(17) . ?
C19 C23 1.5350(17) . ?
C20 C21 1.3913(17) . ?
C20 H20 0.9500 . ?
C21 C22 1.4123(17) . ?
C21 C27 1.5395(17) . ?
C23 C24 1.524(2) . ?
C23 C25 1.5333(19) . ?
C23 C26 1.533(2) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.5363(18) . ?
C27 C30 1.5387(19) . ?
C27 C29 1.5393(18) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

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
C1 O1 H1 104.0(14) . . ?
C16 N1 C15 117.54(11) . . ?
O1 C1 C6 119.28(12) . . ?
O1 C1 C2 119.36(12) . . ?
C6 C1 C2 121.36(12) . . ?
C22 O2 H2 106.7(12) . . ?
C3 C2 C1 116.62(12) . . ?
C3 C2 C7 121.33(12) . . ?
C1 C2 C7 122.02(12) . . ?
C4 C3 C2 124.01(12) . . ?
C4 C3 H3 118.0 . . ?
C2 C3 H3 118.0 . . ?
C3 C4 C5 116.91(12) . . ?
C3 C4 C11 122.39(12) . . ?
C5 C4 C11 120.69(12) . . ?
C6 C5 C4 121.63(12) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C1 119.41(11) . . ?
C5 C6 C15 120.45(12) . . ?
C1 C6 C15 120.13(12) . . ?
C9 C7 C10 107.63(15) . . ?
C9 C7 C2 111.03(14) . . ?
C10 C7 C2 111.90(13) . . ?
C9 C7 C8 110.63(18) . . ?
C10 C7 C8 107.51(15) . . ?
C2 C7 C8 108.10(14) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C14 107.52(13) . . ?
C12 C11 C4 112.14(12) . . ?
C14 C11 C4 110.35(11) . . ?
C12 C11 C13 108.52(13) . . ?
C14 C11 C13 109.44(13) . . ?
C4 C11 C13 108.82(11) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 C6 111.15(10) . . ?
N1 C15 H15A 109.4 . . ?
C6 C15 H15A 109.4 . . ?
N1 C15 H15B 109.4 . . ?
C6 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
N1 C16 C17 123.68(12) . . ?
N1 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C18 C17 C22 120.06(11) . . ?
C18 C17 C16 118.18(11) . . ?
C22 C17 C16 121.74(11) . . ?
C19 C18 C17 121.36(11) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 116.88(11) . . ?
C18 C19 C23 122.91(11) . . ?
C20 C19 C23 120.18(11) . . ?
C21 C20 C19 124.66(11) . . ?
C21 C20 H20 117.7 . . ?
C19 C20 H20 117.7 . . ?
C20 C21 C22 116.70(11) . . ?
C20 C21 C27 121.79(11) . . ?
C22 C21 C27 121.52(11) . . ?
O2 C22 C17 119.94(11) . . ?
O2 C22 C21 119.72(11) . . ?
C17 C22 C21 120.33(11) . . ?
C24 C23 C25 108.58(12) . . ?
C24 C23 C26 111.00(13) . . ?
C25 C23 C26 107.20(12) . . ?
C24 C23 C19 108.55(11) . . ?
C25 C23 C19 111.90(11) . . ?
C26 C23 C19 109.61(11) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C30 107.94(11) . . ?
C28 C27 C29 106.96(11) . . ?
C30 C27 C29 110.00(11) . . ?
C28 C27 C21 111.93(10) . . ?
C30 C27 C21 109.84(10) . . ?
C29 C27 C21 110.11(10) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.053

