# 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 2023

####################################################################### 
# 
# 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_ES0114h_k2
_database_code_depnum_ccdc_archive 'CCDC 2257494'
loop_
_audit_author_name
_audit_author_address
'Uwe Boehme'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2023-04-19 deposited with the CCDC.	2023-08-09 downloaded from the CCDC.
;





_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          470
_chemical_formula_moiety         'C51 H93 Al3 N9 O13, 11(C H Cl3), Cl'
_chemical_formula_sum            'C62 H104 Al3 Cl34 N9 O13'
_chemical_formula_weight         2469.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.2329(3)
_cell_length_b                   15.2329(3)
_cell_length_c                   27.0649(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5438.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    31630
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      27.30


_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_F_000             2520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_exptl_absorpt_coefficient_mu    0.924
_shelx_estimated_absorpt_T_min   0.681
_shelx_estimated_absorpt_T_max   0.738
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.7510
_exptl_absorpt_correction_T_max  0.8573
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
30 7 0 0.1200
3 30 -5 0.1297
9 2 30 0.1680
15 -13 2 0.2277
17 -13 -30 0.2347
10 3 -30 0.1931
-1 5 10 0.2031
-10 -3 0 0.1222
-6 -30 -1 0.1302
-2 -1 -6 0.1588
-10 7 -30 0.2070
-5 4 0 0.2318
-8 6 15 0.2562
-7 -14 30 0.1658


_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_absorpt_special_details   ?
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_voltage           50
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_ambient_temperature      153
_diffrn_measurement_method       'rotation method'
_diffrn_measurement_details      
; 343 frames, detector distance = 119 mm
;


_diffrn_reflns_number            65373
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.674
_diffrn_reflns_theta_max         27.271
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7788
_reflns_number_gt                7178
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2015b)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 There is a disorder at the aluminium bound piperidine ring. 
 This was resolved at the carbon atoms C3 to C7. 
 The localisation of the nitrogen bound hydrogen atom (N1-H1) 
 within the disordered piperidine ring caused serious problems. 
 It was possible to assign at least one position for H1. Bond 
 length and angles including H1 should not be overemphasized! 
;

_vrf_PLAT303_ES0114h_k2          
;
PROBLEM: Full Occupancy Atom H1        with # Connections       1.24 Check 
RESPONSE: Hydrogen Atom H1 lies within the disordered piperidine ring. 
 It was difficult to assign a position at all for this atom. 
 Bond length and angles including H1 should not be overemphasized! 
;



_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0223P)²+2.0308P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin. 
 Flack test results are ambiguous with a Flack parameter 
 of 0.46(5). Therefore, the absolute structure parameter
 was removed from the CIF.
;

_vrf_PLAT034_ES0114h_k2          
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do !  
RESPONSE: The structure was refined as an inversion twin. 
 Flack test results are ambiguous with a Flack parameter 
 of 0.46(5). Therefore, the absolute structure parameter
 was removed from the CIF.
;




_chemical_absolute_configuration ?
_refine_ls_number_reflns         7788
_refine_ls_number_parameters     452
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0637
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.101
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 1.000000 1.000000 0.33515(5) 0.0334(2) Uani 1 3 d S T P . .
Al1 Al 0.76331(5) 0.46608(5) 0.57587(3) 0.02100(14) Uani 1 1 d . . . . .
O1 O 0.82498(14) 0.45447(13) 0.63491(7) 0.0247(4) Uani 1 1 d . . . . .
O2 O 0.82069(13) 0.30831(13) 0.61644(7) 0.0249(4) Uani 1 1 d . . . . .
O3 O 0.71542(13) 0.49684(13) 0.51777(7) 0.0258(4) Uani 1 1 d . . . . .
O4 O 0.54829(13) 0.40608(13) 0.53487(7) 0.0243(4) Uani 1 1 d . . . . .
O5 O 0.666667 0.333333 0.57542(11) 0.0213(6) Uani 1 3 d S T P . .
N2 N 0.9040(2) 0.39705(19) 0.68407(9) 0.0343(6) Uani 1 1 d . . . . .
N3 N 0.60245(18) 0.48946(19) 0.46224(9) 0.0314(5) Uani 1 1 d . . . . .
C1 C 0.84678(19) 0.3854(2) 0.64395(10) 0.0235(5) Uani 1 1 d . . . . .
C2 C 0.6224(2) 0.46259(19) 0.50644(10) 0.0241(5) Uani 1 1 d . . . . .
N1 N 0.87570(16) 0.61992(16) 0.58205(12) 0.0328(5) Uani 1 1 d D . . . .
H1 H 0.869(3) 0.632(3) 0.6190(16) 0.049 Uiso 1 1 d . U . . .
C3A C 0.8627(7) 0.6999(6) 0.5587(5) 0.035(2) Uani 0.761(10) 1 d D . P A 1
H3A H 0.791233 0.682748 0.562499 0.042 Uiso 0.761(10) 1 calc R U P A 1
H3B H 0.876778 0.701432 0.522919 0.042 Uiso 0.761(10) 1 calc R U P A 1
C4A C 0.9308(4) 0.8045(4) 0.5801(3) 0.0433(14) Uani 0.761(10) 1 d D . P A 1
H4A H 0.907751 0.807226 0.613959 0.052 Uiso 0.761(10) 1 calc R U P A 1
H4B H 0.924678 0.855237 0.559812 0.052 Uiso 0.761(10) 1 calc R U P A 1
C5A C 1.0420(4) 0.8322(3) 0.5819(2) 0.0405(12) Uani 0.761(10) 1 d D . P A 1
H5A H 1.069247 0.842347 0.547869 0.049 Uiso 0.761(10) 1 calc R U P A 1
H5B H 1.081723 0.896559 0.600212 0.049 Uiso 0.761(10) 1 calc R U P A 1
C6A C 1.0532(7) 0.7491(7) 0.6070(5) 0.0387(18) Uani 0.761(10) 1 d D . P A 1
H6A H 1.037710 0.747416 0.642628 0.046 Uiso 0.761(10) 1 calc R U P A 1
H6B H 1.124088 0.764053 0.603777 0.046 Uiso 0.761(10) 1 calc R U P A 1
C7A C 0.9821(3) 0.6464(3) 0.5840(2) 0.0309(11) Uani 0.761(10) 1 d D . P A 1
H7A H 1.005476 0.645492 0.549978 0.037 Uiso 0.761(10) 1 calc R U P A 1
H7B H 0.987028 0.593556 0.603122 0.037 Uiso 0.761(10) 1 calc R U P A 1
C3B C 0.8429(19) 0.6925(15) 0.5648(15) 0.031(7) Uani 0.239(10) 1 d D U P A 2
H3C H 0.797204 0.695169 0.589974 0.037 Uiso 0.239(10) 1 calc R U P A 2
H3D H 0.803217 0.665520 0.533996 0.037 Uiso 0.239(10) 1 calc R U P A 2
C4B C 0.9291(13) 0.8010(12) 0.5549(7) 0.039(4) Uani 0.239(10) 1 d D . P A 2
H4C H 0.963663 0.802672 0.523620 0.047 Uiso 0.239(10) 1 calc R U P A 2
H4D H 0.900727 0.846612 0.551258 0.047 Uiso 0.239(10) 1 calc R U P A 2
C5B C 1.0046(16) 0.8378(12) 0.5965(7) 0.049(5) Uani 0.239(10) 1 d D . P A 2
H5C H 0.971600 0.839747 0.627690 0.059 Uiso 0.239(10) 1 calc R U P A 2
H5D H 1.060952 0.906945 0.589387 0.059 Uiso 0.239(10) 1 calc R U P A 2
C6B C 1.044(2) 0.7645(17) 0.6013(19) 0.052(10) Uani 0.239(10) 1 d D . P A 2
H6C H 1.094759 0.786774 0.628375 0.063 Uiso 0.239(10) 1 calc R U P A 2
H6D H 1.078722 0.764245 0.570223 0.063 Uiso 0.239(10) 1 calc R U P A 2
C7B C 0.9576(10) 0.6580(9) 0.6119(6) 0.032(4) Uani 0.239(10) 1 d D . P A 2
H7C H 0.985016 0.611270 0.610956 0.039 Uiso 0.239(10) 1 calc R U P A 2
H7D H 0.934215 0.657224 0.646161 0.039 Uiso 0.239(10) 1 calc R U P A 2
C8 C 0.9245(2) 0.4744(2) 0.72127(11) 0.0344(6) Uani 1 1 d . . . . .
H8A H 0.910050 0.525967 0.707410 0.041 Uiso 1 1 calc R U . . .
H8B H 0.996978 0.508652 0.730752 0.041 Uiso 1 1 calc R U . . .
C9 C 0.8591(3) 0.4262(3) 0.76644(13) 0.0447(8) Uani 1 1 d . . . . .
H9A H 0.786976 0.399414 0.757746 0.054 Uiso 1 1 calc R U . . .
H9B H 0.877394 0.478126 0.792504 0.054 Uiso 1 1 calc R U . . .
C10 C 0.8734(3) 0.3400(3) 0.78610(13) 0.0518(9) Uani 1 1 d . . . . .
H10A H 0.942842 0.368457 0.799568 0.062 Uiso 1 1 calc R U . . .
H10B H 0.824881 0.305029 0.813336 0.062 Uiso 1 1 calc R U . . .
C11 C 0.8571(3) 0.2638(2) 0.74580(14) 0.0439(8) Uani 1 1 d . . . . .
H11A H 0.874052 0.213299 0.758658 0.053 Uiso 1 1 calc R U . . .
H11B H 0.784823 0.227499 0.735873 0.053 Uiso 1 1 calc R U . . .
C12 C 0.9225(2) 0.3166(2) 0.70134(12) 0.0359(7) Uani 1 1 d . . . . .
H12A H 0.994812 0.345977 0.710255 0.043 Uiso 1 1 calc R U . . .
H12B H 0.906915 0.266754 0.674497 0.043 Uiso 1 1 calc R U . . .
C13 C 0.4997(2) 0.4563(3) 0.44514(11) 0.0361(7) Uani 1 1 d . . . . .
H13A H 0.488425 0.514904 0.444414 0.043 Uiso 1 1 calc R U . . .
H13B H 0.450258 0.405533 0.468438 0.043 Uiso 1 1 calc R U . . .
C14 C 0.4826(2) 0.4100(3) 0.39381(13) 0.0460(8) Uani 1 1 d . . . . .
H14A H 0.415137 0.394625 0.381583 0.055 Uiso 1 1 calc R U . . .
H14B H 0.483592 0.345619 0.395555 0.055 Uiso 1 1 calc R U . . .
C15 C 0.5639(3) 0.4817(4) 0.35787(14) 0.0626(12) Uani 1 1 d . . . . .
H15A H 0.558006 0.543009 0.352995 0.075 Uiso 1 1 calc R U . . .
H15B H 0.554228 0.447948 0.325459 0.075 Uiso 1 1 calc R U . . .
C16 C 0.6685(3) 0.5119(4) 0.37818(13) 0.0556(10) Uani 1 1 d . . . . .
H16A H 0.676392 0.451328 0.380241 0.067 Uiso 1 1 calc R U . . .
H16B H 0.721214 0.561120 0.355514 0.067 Uiso 1 1 calc R U . . .
C17 C 0.6826(2) 0.5586(3) 0.42861(12) 0.0396(7) Uani 1 1 d . . . . .
H17A H 0.749413 0.574512 0.442015 0.048 Uiso 1 1 calc R U . . .
H17B H 0.681289 0.622783 0.426010 0.048 Uiso 1 1 calc R U . . .
C18 C 0.333333 0.666667 0.7134(4) 0.074(2) Uani 1 3 d S T P . .
H18 H 0.333332 0.666666 0.676452 0.088 Uiso 1 3 calc R U P . .
Cl2 Cl 0.45828(12) 0.74258(14) 0.73377(7) 0.1109(6) Uani 1 1 d . . . . .
C19 C 0.333333 0.666667 0.4279(3) 0.0587(17) Uani 1 3 d S T P . .
H19 H 0.333334 0.666668 0.464868 0.070 Uiso 1 3 calc R U P B 3
Cl3A Cl 0.2506(8) 0.5416(5) 0.4090(3) 0.084(3) Uani 0.72(8) 1 d . . P C 3
Cl3B Cl 0.273(6) 0.548(3) 0.4046(14) 0.128(8) Uani 0.28(8) 1 d . . P C 4
C20 C 0.5108(3) 0.6056(3) 0.56209(16) 0.0523(9) Uani 1 1 d . . . . .
H20A H 0.522045 0.546353 0.563097 0.063 Uiso 0.59(4) 1 calc R U P D 5
H20B H 0.530544 0.552117 0.562210 0.063 Uiso 0.41(4) 1 calc R U P D 6
Cl4A Cl 0.5121(8) 0.6486(8) 0.6246(4) 0.0713(16) Uani 0.59(4) 1 d . . P D 5
Cl5A Cl 0.3886(5) 0.5657(5) 0.5384(3) 0.0585(14) Uani 0.59(4) 1 d . . P D 5
Cl6A Cl 0.6061(7) 0.7026(5) 0.5236(3) 0.0499(14) Uani 0.59(4) 1 d . . P D 5
Cl4B Cl 0.5258(17) 0.6497(10) 0.6188(8) 0.086(4) Uani 0.41(4) 1 d . . P D 6
Cl5B Cl 0.3878(9) 0.5502(17) 0.5376(4) 0.079(2) Uani 0.41(4) 1 d . . P D 6
Cl6B Cl 0.5942(13) 0.6999(9) 0.5259(5) 0.080(4) Uani 0.41(4) 1 d . . P D 6
C21 C 0.1077(2) 0.2053(2) 0.40806(13) 0.0385(7) Uani 1 1 d . . . . .
H21 H 0.104892 0.146790 0.389881 0.046 Uiso 1 1 calc R U . . .
Cl7 Cl 0.22612(7) 0.27283(9) 0.43746(4) 0.0645(3) Uani 1 1 d . . . . .
Cl8 Cl 0.00999(7) 0.15813(7) 0.45202(4) 0.0558(2) Uani 1 1 d . . . . .
Cl9 Cl 0.09266(8) 0.28364(7) 0.36528(4) 0.0537(2) Uani 1 1 d . . . . .
C22 C 0.9136(3) 0.1264(3) 0.26818(13) 0.0423(7) Uani 1 1 d . . . . .
H22 H 0.965997 0.118840 0.286905 0.051 Uiso 1 1 calc R U . . .
Cl10 Cl 0.80661(7) 0.08742(7) 0.30658(4) 0.0555(2) Uani 1 1 d . . . . .
Cl11 Cl 0.96460(8) 0.25541(7) 0.25238(4) 0.0637(3) Uani 1 1 d . . . . .
Cl12 Cl 0.88056(8) 0.05007(9) 0.21515(4) 0.0607(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 O5 1.8110(7) . ?
Al1 O3 1.8885(19) . ?
Al1 O1 1.906(2) . ?
Al1 O2 1.9138(19) 2_655 ?
Al1 O4 1.9146(19) 3_665 ?
Al1 N1 2.107(2) . ?
O1 C1 1.275(3) . ?
O2 C1 1.275(3) . ?
O3 C2 1.278(3) . ?
O4 C2 1.279(3) . ?
N2 C1 1.348(3) . ?
N2 C8 1.460(4) . ?
N2 C12 1.464(4) . ?
N3 C2 1.348(3) . ?
N3 C13 1.459(4) . ?
N3 C17 1.464(4) . ?
N1 C7B 1.350(11) . ?
N1 C7A 1.463(4) . ?
N1 C3A 1.471(7) . ?
N1 C3B 1.497(18) . ?
N1 H1 1.03(4) . ?
C3A C4A 1.515(10) . ?
C3A H3A 0.9900 . ?
C3A H3B 0.9900 . ?
C4A C5A 1.528(8) . ?
C4A H4A 0.9900 . ?
C4A H4B 0.9900 . ?
C5A C6A 1.519(10) . ?
C5A H5A 0.9900 . ?
C5A H5B 0.9900 . ?
C6A C7A 1.522(9) . ?
C6A H6A 0.9900 . ?
C6A H6B 0.9900 . ?
C7A H7A 0.9900 . ?
C7A H7B 0.9900 . ?
C3B C4B 1.54(2) . ?
C3B H3C 0.9900 . ?
C3B H3D 0.9900 . ?
C4B C5B 1.503(19) . ?
C4B H4C 0.9900 . ?
C4B H4D 0.9900 . ?
C5B C6B 1.52(2) . ?
C5B H5C 0.9900 . ?
C5B H5D 0.9900 . ?
C6B C7B 1.52(2) . ?
C6B H6C 0.9900 . ?
C6B H6D 0.9900 . ?
C7B H1 1.22(4) . ?
C7B H7C 0.9900 . ?
C7B H7D 0.9900 . ?
C8 C9 1.515(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.531(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.519(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.512(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.520(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.523(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.524(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.504(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 Cl2 1.750(4) 2_665 ?
C18 Cl2 1.750(4) 3_565 ?
C18 Cl2 1.750(4) . ?
C18 H18 1.0000 . ?
C19 Cl3B 1.69(3) 3_565 ?
C19 Cl3B 1.69(3) 2_665 ?
C19 Cl3B 1.69(3) . ?
C19 Cl3A 1.755(8) 3_565 ?
C19 Cl3A 1.755(8) 2_665 ?
C19 Cl3A 1.755(8) . ?
C19 H19 1.0000 . ?
C20 Cl4B 1.65(2) . ?
C20 Cl6B 1.677(15) . ?
C20 Cl5B 1.755(13) . ?
C20 Cl5A 1.765(8) . ?
C20 Cl6A 1.798(9) . ?
C20 Cl4A 1.812(12) . ?
C20 H20A 1.0000 . ?
C20 H20B 1.0000 . ?
C21 Cl8 1.755(3) . ?
C21 Cl7 1.757(3) . ?
C21 Cl9 1.758(4) . ?
C21 H21 1.0000 . ?
C22 Cl12 1.755(4) . ?
C22 Cl10 1.766(4) . ?
C22 Cl11 1.766(3) . ?
C22 H22 1.0000 . ?

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


O5 Al1 O3 94.14(10) . . ?
O5 Al1 O1 93.74(10) . . ?
O3 Al1 O1 172.11(9) . . ?
O5 Al1 O2 96.92(8) . 2_655 ?
O3 Al1 O2 91.39(9) . 2_655 ?
O1 Al1 O2 87.22(8) . 2_655 ?
O5 Al1 O4 96.10(8) . 3_665 ?
O3 Al1 O4 87.22(9) . 3_665 ?
O1 Al1 O4 92.39(8) . 3_665 ?
O2 Al1 O4 166.97(8) 2_655 3_665 ?
O5 Al1 N1 175.83(14) . . ?
O3 Al1 N1 89.43(10) . . ?
O1 Al1 N1 82.68(10) . . ?
O2 Al1 N1 80.82(9) 2_655 . ?
O4 Al1 N1 86.21(9) 3_665 . ?
C1 O1 Al1 125.53(17) . . ?
C1 O2 Al1 129.18(16) . 3_665 ?
C2 O3 Al1 125.82(17) . . ?
C2 O4 Al1 127.69(16) . 2_655 ?
Al1 O5 Al1 119.997(3) 2_655 . ?
Al1 O5 Al1 119.995(3) 2_655 3_665 ?
Al1 O5 Al1 119.995(3) . 3_665 ?
C1 N2 C8 121.7(2) . . ?
C1 N2 C12 122.0(2) . . ?
C8 N2 C12 113.7(2) . . ?
C2 N3 C13 122.9(2) . . ?
C2 N3 C17 122.5(2) . . ?
C13 N3 C17 114.6(2) . . ?
O2 C1 O1 123.9(2) . . ?
O2 C1 N2 118.3(2) . . ?
O1 C1 N2 117.7(2) . . ?
O3 C2 O4 123.8(2) . . ?
O3 C2 N3 117.5(2) . . ?
O4 C2 N3 118.7(2) . . ?
C7A N1 C3A 112.1(5) . . ?
C7B N1 C3B 116.6(12) . . ?
C7B N1 Al1 126.0(5) . . ?
C7A N1 Al1 118.79(19) . . ?
C3A N1 Al1 121.1(4) . . ?
C3B N1 Al1 114.3(9) . . ?
C7B N1 H1 60(2) . . ?
C7A N1 H1 97(2) . . ?
C3A N1 H1 101(2) . . ?
C3B N1 H1 94(3) . . ?
Al1 N1 H1 100(2) . . ?
N1 C3A C4A 113.7(6) . . ?
N1 C3A H3A 108.8 . . ?
C4A C3A H3A 108.8 . . ?
N1 C3A H3B 108.8 . . ?
C4A C3A H3B 108.8 . . ?
H3A C3A H3B 107.7 . . ?
C3A C4A C5A 112.6(6) . . ?
C3A C4A H4A 109.1 . . ?
C5A C4A H4A 109.1 . . ?
C3A C4A H4B 109.1 . . ?
C5A C4A H4B 109.1 . . ?
H4A C4A H4B 107.8 . . ?
C6A C5A C4A 110.8(6) . . ?
C6A C5A H5A 109.5 . . ?
C4A C5A H5A 109.5 . . ?
C6A C5A H5B 109.5 . . ?
C4A C5A H5B 109.5 . . ?
H5A C5A H5B 108.1 . . ?
C5A C6A C7A 110.8(7) . . ?
C5A C6A H6A 109.5 . . ?
C7A C6A H6A 109.5 . . ?
C5A C6A H6B 109.5 . . ?
C7A C6A H6B 109.5 . . ?
H6A C6A H6B 108.1 . . ?
N1 C7A C6A 114.7(5) . . ?
N1 C7A H7A 108.6 . . ?
C6A C7A H7A 108.6 . . ?
N1 C7A H7B 108.6 . . ?
C6A C7A H7B 108.6 . . ?
H7A C7A H7B 107.6 . . ?
N1 C3B C4B 115.3(16) . . ?
N1 C3B H3C 108.4 . . ?
C4B C3B H3C 108.4 . . ?
N1 C3B H3D 108.4 . . ?
C4B C3B H3D 108.4 . . ?
H3C C3B H3D 107.5 . . ?
C5B C4B C3B 110.7(18) . . ?
C5B C4B H4C 109.5 . . ?
C3B C4B H4C 109.5 . . ?
C5B C4B H4D 109.5 . . ?
C3B C4B H4D 109.5 . . ?
H4C C4B H4D 108.1 . . ?
C4B C5B C6B 108(2) . . ?
C4B C5B H5C 110.2 . . ?
C6B C5B H5C 110.2 . . ?
C4B C5B H5D 110.2 . . ?
C6B C5B H5D 110.2 . . ?
H5C C5B H5D 108.5 . . ?
C5B C6B C7B 110.1(19) . . ?
C5B C6B H6C 109.6 . . ?
C7B C6B H6C 109.6 . . ?
C5B C6B H6D 109.6 . . ?
C7B C6B H6D 109.6 . . ?
H6C C6B H6D 108.1 . . ?
N1 C7B C6B 117.9(17) . . ?
N1 C7B H1 47(2) . . ?
C6B C7B H1 127(2) . . ?
N1 C7B H7C 107.8 . . ?
C6B C7B H7C 107.8 . . ?
H1 C7B H7C 124.8 . . ?
N1 C7B H7D 107.8 . . ?
C6B C7B H7D 107.8 . . ?
H1 C7B H7D 61.1 . . ?
H7C C7B H7D 107.2 . . ?
N2 C8 C9 110.0(3) . . ?
N2 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
N2 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 C10 110.7(3) . . ?
C8 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C9 111.5(3) . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 110.7(3) . . ?
C12 C11 H11A 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
N2 C12 C11 110.3(3) . . ?
N2 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
N2 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N3 C13 C14 110.8(3) . . ?
N3 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 C15 111.2(3) . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 109.8(3) . . ?
C14 C15 H15A 109.7 . . ?
C16 C15 H15A 109.7 . . ?
C14 C15 H15B 109.7 . . ?
C16 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C17 C16 C15 110.5(3) . . ?
C17 C16 H16A 109.6 . . ?
C15 C16 H16A 109.6 . . ?
C17 C16 H16B 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N3 C17 C16 110.7(3) . . ?
N3 C17 H17A 109.5 . . ?
C16 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
Cl2 C18 Cl2 110.6(3) 2_665 3_565 ?
Cl2 C18 Cl2 110.6(3) 2_665 . ?
Cl2 C18 Cl2 110.6(3) 3_565 . ?
Cl2 C18 H18 108.4 2_665 . ?
Cl2 C18 H18 108.4 3_565 . ?
Cl2 C18 H18 108.4 . . ?
Cl3B C19 Cl3B 106.9(16) 3_565 2_665 ?
Cl3B C19 Cl3B 106.9(17) 3_565 . ?
Cl3B C19 Cl3B 106.9(16) 2_665 . ?
Cl3A C19 Cl3A 111.9(3) 3_565 2_665 ?
Cl3A C19 Cl3A 111.9(3) 3_565 . ?
Cl3A C19 Cl3A 111.9(3) 2_665 . ?
Cl3A C19 H19 107.0 3_565 . ?
Cl3A C19 H19 107.0 2_665 . ?
Cl3A C19 H19 107.0 . . ?
Cl4B C20 Cl6B 107.7(8) . . ?
Cl4B C20 Cl5B 116.5(11) . . ?
Cl6B C20 Cl5B 111.2(6) . . ?
Cl5A C20 Cl6A 110.6(4) . . ?
Cl5A C20 Cl4A 106.5(5) . . ?
Cl6A C20 Cl4A 112.7(5) . . ?
Cl5A C20 H20A 109.0 . . ?
Cl6A C20 H20A 109.0 . . ?
Cl4A C20 H20A 109.0 . . ?
Cl4B C20 H20B 107.0 . . ?
Cl6B C20 H20B 107.0 . . ?
Cl5B C20 H20B 107.0 . . ?
Cl8 C21 Cl7 110.18(19) . . ?
Cl8 C21 Cl9 110.64(18) . . ?
Cl7 C21 Cl9 110.18(18) . . ?
Cl8 C21 H21 108.6 . . ?
Cl7 C21 H21 108.6 . . ?
Cl9 C21 H21 108.6 . . ?
Cl12 C22 Cl10 110.34(19) . . ?
Cl12 C22 Cl11 111.10(19) . . ?
Cl10 C22 Cl11 109.6(2) . . ?
Cl12 C22 H22 108.6 . . ?
Cl10 C22 H22 108.6 . . ?
Cl11 C22 H22 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Al1 O3 C2 40.4(2) . . . . ?
O2 Al1 O3 C2 -56.6(2) 2_655 . . . ?
O4 Al1 O3 C2 136.3(2) 3_665 . . . ?
N1 Al1 O3 C2 -137.4(2) . . . . ?
O3 Al1 O5 Al1 -57.32(19) . . . 2_655 ?
O1 Al1 O5 Al1 122.23(18) . . . 2_655 ?
O2 Al1 O5 Al1 34.6(2) 2_655 . . 2_655 ?
O4 Al1 O5 Al1 -144.97(17) 3_665 . . 2_655 ?
O3 Al1 O5 Al1 124.01(18) . . . 3_665 ?
O1 Al1 O5 Al1 -56.44(19) . . . 3_665 ?
O2 Al1 O5 Al1 -144.08(17) 2_655 . . 3_665 ?
O4 Al1 O5 Al1 36.4(2) 3_665 . . 3_665 ?
Al1 O2 C1 O1 -31.3(4) 3_665 . . . ?
Al1 O2 C1 N2 151.3(2) 3_665 . . . ?
Al1 O1 C1 O2 -7.4(4) . . . . ?
Al1 O1 C1 N2 170.03(19) . . . . ?
C8 N2 C1 O2 -170.8(3) . . . . ?
C12 N2 C1 O2 -10.4(4) . . . . ?
C8 N2 C1 O1 11.6(4) . . . . ?
C12 N2 C1 O1 172.0(3) . . . . ?
Al1 O3 C2 O4 4.0(4) . . . . ?
Al1 O3 C2 N3 -177.13(18) . . . . ?
Al1 O4 C2 O3 -40.3(4) 2_655 . . . ?
Al1 O4 C2 N3 140.9(2) 2_655 . . . ?
C13 N3 C2 O3 -179.4(3) . . . . ?
C17 N3 C2 O3 -2.6(4) . . . . ?
C13 N3 C2 O4 -0.5(4) . . . . ?
C17 N3 C2 O4 176.3(3) . . . . ?
C7A N1 C3A C4A -50.7(11) . . . . ?
Al1 N1 C3A C4A 160.8(6) . . . . ?
N1 C3A C4A C5A 51.3(12) . . . . ?
C3A C4A C5A C6A -51.4(11) . . . . ?
C4A C5A C6A C7A 51.5(11) . . . . ?
C3A N1 C7A C6A 52.4(9) . . . . ?
Al1 N1 C7A C6A -158.4(6) . . . . ?
C5A C6A C7A N1 -53.4(10) . . . . ?
C7B N1 C3B C4B 35(4) . . . . ?
Al1 N1 C3B C4B -163(2) . . . . ?
N1 C3B C4B C5B -46(4) . . . . ?
C3B C4B C5B C6B 58(3) . . . . ?
C4B C5B C6B C7B -60(4) . . . . ?
C3B N1 C7B C6B -38(3) . . . . ?
Al1 N1 C7B C6B 163.3(19) . . . . ?
C5B C6B C7B N1 51(4) . . . . ?
C1 N2 C8 C9 103.1(3) . . . . ?
C12 N2 C8 C9 -58.8(3) . . . . ?
N2 C8 C9 C10 54.6(4) . . . . ?
C8 C9 C10 C11 -53.1(4) . . . . ?
C9 C10 C11 C12 53.1(4) . . . . ?
C1 N2 C12 C11 -102.8(3) . . . . ?
C8 N2 C12 C11 59.0(3) . . . . ?
C10 C11 C12 N2 -54.8(3) . . . . ?
C2 N3 C13 C14 -128.6(3) . . . . ?
C17 N3 C13 C14 54.4(4) . . . . ?
N3 C13 C14 C15 -53.3(4) . . . . ?
C13 C14 C15 C16 55.0(5) . . . . ?
C14 C15 C16 C17 -56.5(5) . . . . ?
C2 N3 C17 C16 126.8(3) . . . . ?
C13 N3 C17 C16 -56.2(4) . . . . ?
C15 C16 C17 N3 56.2(4) . . . . ?

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
_geom_hbond_publ_flag
C3A^a H3A^a O2 0.99 2.69 3.154(10) 109.0 2_655 yes
C6A^a H6A^a Cl11 0.99 2.97 3.942(13) 167.2 4_765 yes
C7A^a H7B^a O1 0.99 2.47 3.029(4) 115.5 . yes
C3B^b H3D^b O3 0.99 2.27 2.91(3) 121.7 . yes
C4B^b H4D^b Cl8 0.99 2.85 3.339(18) 111.6 2_665 yes
C4B^b H4C^b Cl7 0.99 2.79 3.77(2) 170.8 3_665 yes
C14 H14A Cl7 0.99 2.95 3.587(4) 123.4 . yes
C20 H20A^e O4 1.00 2.48 3.442(4) 160.5 . yes
C21 H21 Cl1 1.00 2.48 3.352(3) 144.8 1_445 yes
C22 H22 Cl1 1.00 2.49 3.356(3) 145.0 1_545 yes

_refine_diff_density_max         0.290
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.040

####################################################################### 
# 
# 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_es0113p_n9
_database_code_depnum_ccdc_archive 'CCDC 2257495'
loop_
_audit_author_name
_audit_author_address
'Uwe Boehme'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-08-09 downloaded from the CCDC.
;





_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          496
_chemical_formula_moiety         'C42 H74 Al3 N9 O13, 5(C6 H6), Cl'
_chemical_formula_sum            'C72 H104 Al3 Cl N9 O13'
_chemical_formula_weight         1420.03


# start Validation Reply Form
_vrf_PLAT910_es0113p_n9          
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         20 Note  
RESPONSE: The crystals are weakly diffracting. Therefore, 
data collection had to be performed with long exposure 
times of 5 minutes per frame. However, several reflections 
are still missing in the data.
;
# end Validation Reply Form



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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   25.0203(9)
_cell_length_b                   22.6402(6)
_cell_length_c                   27.6410(11)
_cell_angle_alpha                90
_cell_angle_beta                 105.685(3)
_cell_angle_gamma                90
_cell_volume                     15074.6(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    58503
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      27.28



_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_F_000             6072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.152
_shelx_estimated_absorpt_T_min   0.935
_shelx_estimated_absorpt_T_max   0.970

_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.9478
_exptl_absorpt_correction_T_max  0.9816
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 2 30 0.0523
-30 0 7 0.3256
-29 30 6 0.1993
0 -1 0 0.1971
-1 1 -30 0.0573


_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_absorpt_special_details   ?

_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_voltage           50
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_ambient_temperature      153
_diffrn_measurement_method       'rotation method'
_diffrn_measurement_details      
; 203 frames, detector distance = 119 mm
;


_diffrn_reflns_number            63158
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.805
_diffrn_reflns_theta_max         27.279
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             16731
_reflns_number_gt                12445
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2015b)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0646P)²+29.1802P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16731
_refine_ls_number_parameters     983
_refine_ls_number_restraints     1015
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_ref         0.1582
_refine_ls_wR_factor_gt          0.1373
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.042
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.22494(3) 0.50041(3) 0.16941(2) 0.03909(14) Uani 1 1 d . . . . .
Al1 Al -0.01444(3) 0.01922(3) 0.19283(2) 0.02610(14) Uani 1 1 d . . . . .
Al2 Al -0.04889(3) 0.06277(3) 0.28933(2) 0.02424(14) Uani 1 1 d . . . . .
Al3 Al 0.07864(3) 0.06168(3) 0.28863(2) 0.02495(14) Uani 1 1 d . . . . .
O1 O -0.06469(7) -0.03952(8) 0.20281(6) 0.0383(4) Uani 1 1 d . . . . .
O2 O -0.08853(9) -0.00766(8) 0.27059(8) 0.0530(6) Uani 1 1 d . . . . .
O3 O -0.07213(8) 0.07345(9) 0.16612(6) 0.0467(5) Uani 1 1 d . . . . .
O4 O -0.09601(7) 0.10432(9) 0.23442(6) 0.0389(4) Uani 1 1 d . . . . .
O5 O -0.01056(9) 0.02392(10) 0.34918(7) 0.0585(6) Uani 1 1 d . . . . .
O6 O 0.07654(8) 0.01742(10) 0.34499(7) 0.0558(6) Uani 1 1 d . . . . .
O7 O -0.02162(7) 0.13687(8) 0.31739(7) 0.0413(4) Uani 1 1 d . . . . .
O8 O 0.06789(7) 0.13489(7) 0.31879(7) 0.0365(4) Uani 1 1 d . . . . .
O9 O 0.10741(8) -0.00762(8) 0.26604(9) 0.0544(6) Uani 1 1 d . . . . .
O10 O 0.04002(7) -0.04114(8) 0.20119(6) 0.0380(4) Uani 1 1 d . . . . .
O11 O 0.09380(7) 0.10408(8) 0.23475(6) 0.0362(4) Uani 1 1 d . . . . .
O12 O 0.03209(8) 0.06882(9) 0.16589(6) 0.0450(5) Uani 1 1 d . . . . .
O13 O 0.00495(6) 0.04862(6) 0.25642(5) 0.0244(3) Uani 1 1 d . . . . .
N1 N -0.03970(9) -0.01904(13) 0.11861(8) 0.0492(6) Uani 1 1 d . . . . .
N2 N -0.11093(8) 0.08004(9) 0.32666(7) 0.0278(4) Uani 1 1 d . . . . .
H2 H -0.1340(12) 0.0497(13) 0.3198(11) 0.042 Uiso 1 1 d . U . . .
N3 N 0.16204(8) 0.07842(9) 0.32830(7) 0.0297(4) Uani 1 1 d . . . . .
H3 H 0.1810(13) 0.0498(14) 0.3218(11) 0.044 Uiso 1 1 d . U . . .
N4 N -0.12082(9) -0.09358(9) 0.23596(8) 0.0359(4) Uani 1 1 d . . . . .
N5 N -0.13177(9) 0.14781(11) 0.16025(8) 0.0421(5) Uani 1 1 d . . . . .
N6 N 0.04978(8) -0.03445(9) 0.40229(7) 0.0306(4) Uani 1 1 d . . . . .
N7 N 0.03616(8) 0.20523(8) 0.36052(7) 0.0303(4) Uani 1 1 d . . . . .
N8 N 0.11748(8) -0.09366(9) 0.23056(8) 0.0353(4) Uani 1 1 d . . . . .
N9 N 0.09851(9) 0.13047(10) 0.15810(8) 0.0389(5) Uani 1 1 d . . . . .
C1 C -0.09009(9) -0.04502(10) 0.23642(8) 0.0287(4) Uani 1 1 d . . . . .
C2 C -0.09835(9) 0.10679(11) 0.18834(8) 0.0311(5) Uani 1 1 d . . . . .
C3 C 0.03763(10) 0.00394(9) 0.36374(8) 0.0292(5) Uani 1 1 d . . . . .
C4 C 0.02694(9) 0.15661(9) 0.33074(7) 0.0235(4) Uani 1 1 d . . . . .
C5 C 0.08722(9) -0.04554(10) 0.23302(9) 0.0297(4) Uani 1 1 d . . . . .
C6 C 0.07353(10) 0.09972(10) 0.18774(9) 0.0308(5) Uani 1 1 d . . . . .
C7A C -0.0147(6) -0.0062(8) 0.0797(4) 0.065(3) Uani 0.60(3) 1 d . U P A 1
H7A H 0.025291 -0.016155 0.090204 0.078 Uiso 0.60(3) 1 calc R U P A 1
H7B H -0.018721 0.036236 0.070897 0.078 Uiso 0.60(3) 1 calc R U P A 1
C7B C -0.0065(6) -0.0304(11) 0.0879(7) 0.057(4) Uani 0.40(3) 1 d . . P A 2
H7C H 0.017933 -0.064504 0.100818 0.068 Uiso 0.40(3) 1 calc R U P A 2
H7D H 0.017082 0.004345 0.086555 0.068 Uiso 0.40(3) 1 calc R U P A 2
C8 C -0.04514(15) -0.0444(2) 0.03417(12) 0.0692(10) Uani 1 1 d . . . . .
H8A H -0.043465 -0.026172 0.002056 0.083 Uiso 1 1 calc R U . A 1
H8B H -0.029491 -0.084790 0.036445 0.083 Uiso 1 1 calc R U . A 1
C9 C -0.10281(14) -0.04482(18) 0.03929(11) 0.0606(9) Uani 1 1 d . . . . .
H9A H -0.119270 -0.084739 0.032480 0.073 Uiso 1 1 calc R U . . .
H9B H -0.126390 -0.016546 0.015513 0.073 Uiso 1 1 calc R U . . .
C10 C -0.09799(13) -0.0269(2) 0.09268(12) 0.0741(12) Uani 1 1 d . . . . .
H10A H -0.118385 0.010484 0.093236 0.089 Uiso 1 1 calc R U . . .
H10B H -0.114354 -0.057731 0.109668 0.089 Uiso 1 1 calc R U . . .
C11 C -0.14638(10) 0.13328(11) 0.31050(9) 0.0323(5) Uani 1 1 d . . . . .
H11A H -0.174892 0.125441 0.278538 0.039 Uiso 1 1 calc R U . . .
H11B H -0.123487 0.167216 0.305525 0.039 Uiso 1 1 calc R U . . .
C12 C -0.17379(11) 0.14648(12) 0.35238(10) 0.0407(6) Uani 1 1 d . . . . .
H12A H -0.179240 0.189496 0.355371 0.049 Uiso 1 1 calc R U . . .
H12B H -0.210213 0.126465 0.346011 0.049 Uiso 1 1 calc R U . . .
C13 C -0.13340(12) 0.12244(17) 0.39946(11) 0.0565(8) Uani 1 1 d . . . . .
H13A H -0.113914 0.155258 0.420718 0.068 Uiso 1 1 calc R U . . .
H13B H -0.153410 0.098896 0.419192 0.068 Uiso 1 1 calc R U . . .
C14 C -0.09230(11) 0.08405(12) 0.38262(8) 0.0374(5) Uani 1 1 d . . . . .
H14A H -0.054720 0.101626 0.393515 0.045 Uiso 1 1 calc R U . . .
H14B H -0.090938 0.044189 0.397626 0.045 Uiso 1 1 calc R U . . .
C15 C 0.17439(11) 0.08009(13) 0.38434(9) 0.0403(6) Uani 1 1 d . . . . .
H15A H 0.179696 0.039526 0.398197 0.048 Uiso 1 1 calc R U . . .
H15B H 0.143243 0.098632 0.394477 0.048 Uiso 1 1 calc R U . . .
C16 C 0.22690(12) 0.11587(17) 0.40387(11) 0.0572(8) Uani 1 1 d . . . . .
H16A H 0.223805 0.141645 0.431925 0.069 Uiso 1 1 calc R U . . .
H16B H 0.259322 0.089496 0.416009 0.069 Uiso 1 1 calc R U . . .
C17 C 0.23301(16) 0.15203(16) 0.36066(15) 0.0760(12) Uani 1 1 d . . . . .
H17A H 0.270178 0.145753 0.355363 0.091 Uiso 1 1 calc R U . . .
H17B H 0.228931 0.194494 0.367433 0.091 Uiso 1 1 calc R U . . .
C18 C 0.18839(10) 0.13313(11) 0.31456(10) 0.0368(5) Uani 1 1 d . . . . .
H18A H 0.160329 0.164763 0.304031 0.044 Uiso 1 1 calc R U . . .
H18B H 0.204810 0.124854 0.286454 0.044 Uiso 1 1 calc R U . . .
C19 C -0.12816(14) -0.13983(14) 0.19817(12) 0.0556(8) Uani 1 1 d . . . . .
H19A H -0.092197 -0.151125 0.192318 0.067 Uiso 1 1 calc R U . B 3
H19B H -0.153825 -0.126987 0.165972 0.067 Uiso 1 1 calc R U . B 3
C20A C -0.1529(5) -0.1911(3) 0.2212(4) 0.066(2) Uani 0.76(2) 1 d . . P C 3
H20A H -0.179501 -0.213933 0.194842 0.079 Uiso 0.76(2) 1 calc R U P C 3
H20B H -0.123369 -0.217906 0.240139 0.079 Uiso 0.76(2) 1 calc R U P C 3
C20B C -0.1777(13) -0.1735(14) 0.2072(9) 0.064(5) Uani 0.24(2) 1 d . U P C 4
H20C H -0.212312 -0.161071 0.182303 0.076 Uiso 0.24(2) 1 calc R U P C 4
H20D H -0.172764 -0.216462 0.203145 0.076 Uiso 0.24(2) 1 calc R U P C 4
C21 C -0.18131(18) -0.16177(16) 0.25511(17) 0.0771(12) Uani 1 1 d . . . . .
H21A H -0.182808 -0.188465 0.283082 0.093 Uiso 1 1 calc R U . C 3
H21B H -0.219727 -0.150996 0.236542 0.093 Uiso 1 1 calc R U . C 3
C22 C -0.14827(12) -0.10729(12) 0.27501(11) 0.0441(6) Uani 1 1 d . . . . .
H22A H -0.172801 -0.074547 0.279341 0.053 Uiso 1 1 calc R U . . .
H22B H -0.120807 -0.115250 0.307569 0.053 Uiso 1 1 calc R U . . .
C23 C -0.13570(16) 0.15799(18) 0.10724(11) 0.0671(10) Uani 1 1 d . . . . .
H23A H -0.144006 0.120741 0.087908 0.081 Uiso 1 1 calc R U . D 5
H23B H -0.100567 0.174520 0.103107 0.081 Uiso 1 1 calc R U . D 5
C24A C -0.1817(6) 0.2008(7) 0.0902(4) 0.080(3) Uani 0.55(2) 1 d . U P E 5
H24A H -0.218520 0.181502 0.083464 0.096 Uiso 0.55(2) 1 calc R U P E 5
H24B H -0.179018 0.222997 0.060139 0.096 Uiso 0.55(2) 1 calc R U P E 5
C25A C -0.1690(8) 0.2428(6) 0.1403(4) 0.078(3) Uani 0.55(2) 1 d . U P E 5
H25A H -0.134685 0.266251 0.144640 0.094 Uiso 0.55(2) 1 calc R U P E 5
H25B H -0.200521 0.269279 0.140238 0.094 Uiso 0.55(2) 1 calc R U P E 5
C24B C -0.1618(7) 0.2234(7) 0.1011(6) 0.074(4) Uani 0.45(2) 1 d . U P E 6
H24C H -0.132204 0.253754 0.109753 0.089 Uiso 0.45(2) 1 calc R U P E 6
H24D H -0.184713 0.230245 0.066311 0.089 Uiso 0.45(2) 1 calc R U P E 6
C25B C -0.1959(8) 0.2246(7) 0.1367(4) 0.073(3) Uani 0.45(2) 1 d . U P E 6
H25C H -0.231954 0.204652 0.122412 0.087 Uiso 0.45(2) 1 calc R U P E 6
H25D H -0.202785 0.265621 0.145713 0.087 Uiso 0.45(2) 1 calc R U P E 6
C26 C -0.16200(16) 0.19201(17) 0.18086(13) 0.0667(10) Uani 1 1 d . . . . .
H26A H -0.140263 0.205572 0.214471 0.080 Uiso 1 1 calc R U . E 5
H26B H -0.198386 0.176822 0.183034 0.080 Uiso 1 1 calc R U . E 5
C27 C 0.01130(12) -0.05263(16) 0.43032(10) 0.0511(8) Uani 1 1 d . . . . .
H27A H -0.018649 -0.077675 0.409546 0.061 Uiso 1 1 calc R U . . .
H27B H -0.005461 -0.018004 0.442499 0.061 Uiso 1 1 calc R U . . .
C28 C 0.04810(13) -0.08777(17) 0.47425(12) 0.0612(9) Uani 1 1 d . . . . .
H28A H 0.063167 -0.061902 0.503657 0.073 Uiso 1 1 calc R U . . .
H28B H 0.026993 -0.120378 0.484284 0.073 Uiso 1 1 calc R U . . .
C29 C 0.09411(12) -0.11151(13) 0.45389(11) 0.0490(7) Uani 1 1 d . . . . .
H29A H 0.127994 -0.119305 0.481425 0.059 Uiso 1 1 calc R U . . .
H29B H 0.082565 -0.148476 0.434796 0.059 Uiso 1 1 calc R U . . .
C30 C 0.10399(10) -0.06303(13) 0.41999(10) 0.0415(6) Uani 1 1 d . . . . .
H30A H 0.132347 -0.034853 0.438748 0.050 Uiso 1 1 calc R U . . .
H30B H 0.116248 -0.079436 0.391556 0.050 Uiso 1 1 calc R U . . .
C31 C -0.00720(12) 0.23645(12) 0.37626(11) 0.0464(7) Uani 1 1 d D . . . .
H31A H -0.015279 0.217965 0.405972 0.056 Uiso 1 1 calc R U . F 7
H31B H -0.041843 0.240030 0.348739 0.056 Uiso 1 1 calc R U . F 7
C32A C 0.0245(2) 0.2988(2) 0.3896(2) 0.0430(15) Uani 0.626(10) 1 d D . P G 7
H32A H 0.021017 0.322658 0.358875 0.052 Uiso 0.626(10) 1 calc R U P G 7
H32B H 0.009341 0.321715 0.413406 0.052 Uiso 0.626(10) 1 calc R U P G 7
C33A C 0.0850(2) 0.2819(2) 0.4136(2) 0.0411(13) Uani 0.626(10) 1 d D . P G 7
H33A H 0.110734 0.315264 0.414079 0.049 Uiso 0.626(10) 1 calc R U P G 7
H33B H 0.090801 0.265965 0.447971 0.049 Uiso 0.626(10) 1 calc R U P G 7
C32B C 0.0172(3) 0.2823(3) 0.4127(3) 0.0370(19) Uani 0.374(10) 1 d D . P G 8
H32C H 0.033284 0.266391 0.446922 0.044 Uiso 0.374(10) 1 calc R U P G 8
H32D H -0.009189 0.314602 0.413672 0.044 Uiso 0.374(10) 1 calc R U P G 8
C33B C 0.0616(4) 0.3005(3) 0.3866(4) 0.041(2) Uani 0.374(10) 1 d D . P G 8
H33C H 0.089859 0.326512 0.408460 0.049 Uiso 0.374(10) 1 calc R U P G 8
H33D H 0.044789 0.321113 0.354513 0.049 Uiso 0.374(10) 1 calc R U P G 8
C34 C 0.08988(13) 0.23484(14) 0.37653(13) 0.0560(8) Uani 1 1 d D . . . .
H34A H 0.099431 0.252787 0.347284 0.067 Uiso 1 1 calc R U . G 7
H34B H 0.119276 0.206221 0.392486 0.067 Uiso 1 1 calc R U . G 7
C35 C 0.17011(12) -0.10844(12) 0.26719(13) 0.0535(8) Uani 1 1 d . . . . .
H35A H 0.163833 -0.124823 0.298411 0.064 Uiso 1 1 calc R U . . .
H35B H 0.194592 -0.073445 0.275622 0.064 Uiso 1 1 calc R U . . .
C36 C 0.19436(13) -0.15452(15) 0.23942(16) 0.0693(11) Uani 1 1 d . . . . .
H36A H 0.217031 -0.135688 0.219388 0.083 Uiso 1 1 calc R U . . .
H36B H 0.217867 -0.182791 0.263255 0.083 Uiso 1 1 calc R U . . .
C37 C 0.14492(14) -0.18508(14) 0.20593(14) 0.0598(8) Uani 1 1 d . . . . .
H37A H 0.131207 -0.216521 0.224402 0.072 Uiso 1 1 calc R U . . .
H37B H 0.154233 -0.202791 0.176480 0.072 Uiso 1 1 calc R U . . .
C38 C 0.10202(12) -0.13654(13) 0.18977(11) 0.0471(7) Uani 1 1 d . . . . .
H38A H 0.103802 -0.118783 0.157509 0.057 Uiso 1 1 calc R U . . .
H38B H 0.064075 -0.151873 0.186106 0.057 Uiso 1 1 calc R U . . .
C39 C 0.14747(14) 0.16742(16) 0.17778(12) 0.0596(9) Uani 1 1 d . . . . .
H39A H 0.180793 0.143137 0.192550 0.072 Uiso 1 1 calc R U . H 9
H39B H 0.141727 0.195383 0.203455 0.072 Uiso 1 1 calc R U . H 9
C40A C 0.1526(7) 0.2003(7) 0.1303(5) 0.068(3) Uani 0.46(2) 1 d . U P I 9
H40A H 0.131606 0.237819 0.126066 0.081 Uiso 0.46(2) 1 calc R U P I 9
H40B H 0.192009 0.209194 0.132765 0.081 Uiso 0.46(2) 1 calc R U P I 9
C41A C 0.1297(7) 0.1610(9) 0.0881(6) 0.064(3) Uani 0.46(2) 1 d . . P I 9
H41A H 0.157920 0.132221 0.083853 0.077 Uiso 0.46(2) 1 calc R U P I 9
H41B H 0.115870 0.183570 0.056540 0.077 Uiso 0.46(2) 1 calc R U P I 9
C40B C 0.1692(6) 0.1766(8) 0.1325(4) 0.072(3) Uani 0.54(2) 1 d . U P I 10
H40C H 0.192893 0.143372 0.127698 0.086 Uiso 0.54(2) 1 calc R U P I 10
H40D H 0.190056 0.214105 0.134716 0.086 Uiso 0.54(2) 1 calc R U P I 10
C41B C 0.1117(7) 0.1788(7) 0.0891(5) 0.065(3) Uani 0.54(2) 1 d . . P I 10
H41C H 0.092228 0.216790 0.089342 0.078 Uiso 0.54(2) 1 calc R U P I 10
H41D H 0.117774 0.172636 0.055498 0.078 Uiso 0.54(2) 1 calc R U P I 10
C42 C 0.08051(13) 0.12879(14) 0.10328(10) 0.0497(7) Uani 1 1 d . . . . .
H42A H 0.045039 0.150198 0.090145 0.060 Uiso 1 1 calc R U . I 9
H42B H 0.076081 0.087632 0.090727 0.060 Uiso 1 1 calc R U . I 9
C43 C 0.09957(17) 0.41842(16) -0.01142(13) 0.0637(9) Uani 1 1 d G . . . .
H43 H 0.096589 0.441823 -0.040560 0.076 Uiso 1 1 calc R U . . .
C44 C 0.07904(16) 0.36201(17) -0.01595(13) 0.0672(9) Uani 1 1 d . . . . .
H44 H 0.060937 0.346178 -0.048028 0.081 Uiso 1 1 calc R U . . .
C45 C 0.08518(18) 0.32848(16) 0.02712(15) 0.0748(11) Uani 1 1 d . . . . .
H45 H 0.071480 0.289153 0.024878 0.090 Uiso 1 1 calc R U . . .
C46 C 0.11134(16) 0.35258(17) 0.07330(12) 0.0636(9) Uani 1 1 d . . . . .
H46 H 0.116422 0.329410 0.102853 0.076 Uiso 1 1 calc R U . . .
C47 C 0.12952(12) 0.40818(16) 0.07671(12) 0.0555(8) Uani 1 1 d . . . . .
H47 H 0.146262 0.424709 0.108829 0.067 Uiso 1 1 calc R U . . .
C48 C 0.12447(15) 0.44109(15) 0.03535(14) 0.0624(8) Uani 1 1 d . . . . .
H48 H 0.138227 0.480407 0.038429 0.075 Uiso 1 1 calc R U . . .
C49 C 0.60031(19) 0.1233(2) 0.03733(19) 0.1090(17) Uani 1 1 d DG . . . .
H49 H 0.598094 0.082551 0.044829 0.131 Uiso 1 1 calc R U . . .
C50 C 0.5587(2) 0.1491(2) -0.00028(19) 0.1126(18) Uani 1 1 d D . . . .
H50 H 0.529009 0.125517 -0.019238 0.135 Uiso 1 1 calc R U . . .
C51 C 0.5599(2) 0.2090(2) -0.01062(18) 0.1088(17) Uani 1 1 d D . . . .
H51 H 0.530110 0.227513 -0.034501 0.131 Uiso 1 1 calc R U . . .
C52 C 0.6063(2) 0.24089(19) 0.01517(17) 0.1162(19) Uani 1 1 d D U . . .
H52 H 0.608557 0.281557 0.007489 0.139 Uiso 1 1 calc R U . . .
C53 C 0.6496(2) 0.21560(16) 0.05178(18) 0.1063(16) Uani 1 1 d D . . . .
H53 H 0.681422 0.238109 0.068018 0.128 Uiso 1 1 calc R U . . .
C54 C 0.64516(19) 0.15658(16) 0.06411(17) 0.0900(13) Uani 1 1 d D . . . .
H54 H 0.672781 0.139093 0.090784 0.108 Uiso 1 1 calc R U . . .
C55 C 0.250000 0.5380(2) 0.000000 0.0507(10) Uani 1 2 d S T P . .
H55 H 0.250002 0.496087 -0.000001 0.061 Uiso 1 2 calc R U P . .
C56 C 0.24894(11) 0.56817(15) 0.04311(11) 0.0498(7) Uani 1 1 d . . . . .
H56 H 0.248051 0.547145 0.072624 0.060 Uiso 1 1 calc R U . . .
C57 C 0.24917(11) 0.62930(15) 0.04298(11) 0.0497(7) Uani 1 1 d . . . . .
H57 H 0.248752 0.650270 0.072647 0.060 Uiso 1 1 calc R U . . .
C58 C 0.250000 0.66006(19) 0.000000 0.0493(9) Uani 1 2 d S T P . .
H58 H 0.250000 0.702018 0.000001 0.059 Uiso 1 2 calc R U P . .
C59 C 0.49566(17) 0.26007(17) 0.33632(14) 0.0680(9) Uani 1 1 d G . . . .
H59 H 0.490370 0.290852 0.357918 0.082 Uiso 1 1 calc R U . . .
C60 C 0.49305(17) 0.20208(18) 0.35054(14) 0.0722(10) Uani 1 1 d . . . . .
H60 H 0.485480 0.193199 0.381628 0.087 Uiso 1 1 calc R U . . .
C61 C 0.50128(15) 0.15711(15) 0.32020(13) 0.0614(8) Uani 1 1 d . . . . .
H61 H 0.499763 0.117165 0.330280 0.074 Uiso 1 1 calc R U . . .
C62 C 0.51169(15) 0.17011(15) 0.27526(13) 0.0617(9) Uani 1 1 d . . . . .
H62 H 0.517302 0.139327 0.253797 0.074 Uiso 1 1 calc R U . . .
C63 C 0.51396(15) 0.22891(16) 0.26136(13) 0.0636(9) Uani 1 1 d . . . . .
H63 H 0.521353 0.238103 0.230254 0.076 Uiso 1 1 calc R U . . .
C64 C 0.50572(13) 0.27371(14) 0.29176(13) 0.0553(7) Uani 1 1 d . . . . .
H64 H 0.507024 0.313748 0.281857 0.066 Uiso 1 1 calc R U . . .
C65 C 0.31386(16) 0.50138(19) 0.39624(12) 0.0849(12) Uani 1 1 d DG . . . .
H65 H 0.341735 0.497345 0.427150 0.102 Uiso 1 1 calc R U . . .
C66 C 0.32785(15) 0.49482(17) 0.35130(12) 0.0739(10) Uani 1 1 d D . . . .
H66 H 0.365350 0.487701 0.351581 0.089 Uiso 1 1 calc R U . . .
C67 C 0.28743(14) 0.49860(15) 0.30614(12) 0.0711(10) Uani 1 1 d D . . . .
H67 H 0.296809 0.493654 0.275302 0.085 Uiso 1 1 calc R U . . .
C68 C 0.23324(14) 0.50966(17) 0.30632(13) 0.0808(12) Uani 1 1 d D . . . .
H68 H 0.205149 0.511359 0.275363 0.097 Uiso 1 1 calc R U . . .
C69 C 0.21921(15) 0.51830(19) 0.35094(14) 0.0936(15) Uani 1 1 d D . . . .
H69 H 0.181959 0.527335 0.350349 0.112 Uiso 1 1 calc R U . . .
C70 C 0.25953(16) 0.51379(19) 0.39662(14) 0.0956(15) Uani 1 1 d D . . . .
H70 H 0.250161 0.519066 0.427438 0.115 Uiso 1 1 calc R U . . .
C71 C 0.750000 0.7684(3) 0.000000 0.138(3) Uani 1 2 d DGS TU P . .
H71 H 0.749999 0.726409 0.000000 0.166 Uiso 1 2 calc R U P . .
C72 C 0.7575(3) 0.79937(18) 0.04481(17) 0.1202(19) Uani 1 1 d D U . . .
H72 H 0.761652 0.778437 0.075395 0.144 Uiso 1 1 calc R U . . .
C73 C 0.75885(19) 0.86072(18) 0.04513(14) 0.0910(13) Uani 1 1 d D . . . .
H73 H 0.765795 0.881770 0.075936 0.109 Uiso 1 1 calc R U . . .
C74 C 0.750000 0.8909(3) 0.000000 0.0796(15) Uani 1 2 d DS T P . .
H74 H 0.749997 0.932873 0.000000 0.096 Uiso 1 2 calc R U P . .


_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 O13 1.8186(15) . ?
Al1 O3 1.8867(19) . ?
Al1 O10 1.8994(18) . ?
Al1 O1 1.9007(18) . ?
Al1 O12 1.9079(18) . ?
Al1 N1 2.158(2) . ?
Al2 O13 1.8458(16) . ?
Al2 O2 1.8753(19) . ?
Al2 O5 1.8900(18) . ?
Al2 O7 1.8961(18) . ?
Al2 O4 1.9002(17) . ?
Al2 N2 2.1197(19) . ?
Al3 O13 1.8416(16) . ?
Al3 O6 1.8651(19) . ?
Al3 O11 1.8944(17) . ?
Al3 O9 1.9007(19) . ?
Al3 O8 1.9068(17) . ?
Al3 N3 2.113(2) . ?
O1 C1 1.266(3) . ?
O2 C1 1.260(3) . ?
O3 C2 1.263(3) . ?
O4 C2 1.260(3) . ?
O5 C3 1.248(3) . ?
O6 C3 1.258(3) . ?
O7 C4 1.253(3) . ?
O8 C4 1.258(3) . ?
O9 C5 1.255(3) . ?
O10 C5 1.271(3) . ?
O11 C6 1.265(3) . ?
O12 C6 1.261(3) . ?
N1 C7B 1.362(16) . ?
N1 C7A 1.413(9) . ?
N1 C10 1.452(4) . ?
N2 C11 1.492(3) . ?
N2 C14 1.493(3) . ?
N2 H2 0.88(3) . ?
N3 C15 1.496(3) . ?
N3 C18 1.500(3) . ?
N3 H3 0.85(3) . ?
N4 C1 1.340(3) . ?
N4 C19 1.455(3) . ?
N4 C22 1.461(3) . ?
N5 C2 1.347(3) . ?
N5 C23 1.460(3) . ?
N5 C26 1.460(4) . ?
N6 C3 1.345(3) . ?
N6 C27 1.449(3) . ?
N6 C30 1.463(3) . ?
N7 C4 1.356(3) . ?
N7 C31 1.456(3) . ?
N7 C34 1.459(3) . ?
N8 C5 1.339(3) . ?
N8 C38 1.459(3) . ?
N8 C35 1.466(3) . ?
N9 C6 1.350(3) . ?
N9 C42 1.460(3) . ?
N9 C39 1.462(4) . ?
C7A C8 1.546(11) . ?
C7A H7A 0.9900 . ?
C7A H7B 0.9900 . ?
C7B C8 1.571(15) . ?
C7B H7C 0.9900 . ?
C7B H7D 0.9900 . ?
C8 C9 1.487(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.504(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.526(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.516(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.513(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.513(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.490(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.511(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20A 1.531(6) . ?
C19 C20B 1.532(19) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20A C21 1.478(7) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
C20B C21 1.38(2) . ?
C20B H20C 0.9900 . ?
C20B H20D 0.9900 . ?
C21 C22 1.504(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24A 1.481(10) . ?
C23 C24B 1.609(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24A C25A 1.64(2) . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
C25A C26 1.582(11) . ?
C25A H25A 0.9900 . ?
C25A H25B 0.9900 . ?
C24B C25B 1.47(2) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
C25B C26 1.481(10) . ?
C25B H25C 0.9900 . ?
C25B H25D 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.533(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.510(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.506(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32B 1.460(7) . ?
C31 C32A 1.614(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32A C33A 1.528(7) . ?
C32A H32A 0.9900 . ?
C32A H32B 0.9900 . ?
C33A C34 1.505(5) . ?
C33A H33A 0.9900 . ?
C33A H33B 0.9900 . ?
C32B C33B 1.537(10) . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
C33B C34 1.701(8) . ?
C33B H33C 0.9900 . ?
C33B H33D 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.516(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.499(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.517(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40B 1.506(11) . ?
C39 C40A 1.544(12) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40A C41A 1.45(2) . ?
C40A H40A 0.9900 . ?
C40A H40B 0.9900 . ?
C41A C42 1.582(14) . ?
C41A H41A 0.9900 . ?
C41A H41B 0.9900 . ?
C40B C41B 1.60(3) . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
C41B C42 1.487(13) . ?
C41B H41C 0.9900 . ?
C41B H41D 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.370(5) . ?
C43 C48 1.374(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.385(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.380(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.333(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.342(5) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C50 1.386(2) . ?
C49 C54 1.388(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.387(2) . ?
C50 H50 0.9500 . ?
C51 C52 1.389(2) . ?
C51 H51 0.9500 . ?
C52 C53 1.390(2) . ?
C52 H52 0.9500 . ?
C53 C54 1.391(2) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.379(4) 2 ?
C55 C56 1.379(4) . ?
C55 H55 0.9500 . ?
C56 C57 1.384(5) . ?
C56 H56 0.9500 . ?
C57 C58 1.382(4) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C59 C64 1.358(5) . ?
C59 C60 1.377(5) . ?
C59 H59 0.9500 . ?
C60 C61 1.370(5) . ?
C60 H60 0.9500 . ?
C61 C62 1.368(5) . ?
C61 H61 0.9500 . ?
C62 C63 1.391(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.368(5) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
C65 C66 1.3866(19) . ?
C65 C70 1.391(2) . ?
C65 H65 0.9500 . ?
C66 C67 1.3803(19) . ?
C66 H66 0.9500 . ?
C67 C68 1.3800(19) . ?
C67 H67 0.9500 . ?
C68 C69 1.385(2) . ?
C68 H68 0.9500 . ?
C69 C70 1.391(2) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
C71 C72 1.392(2) . ?
C71 C72 1.392(2) 2_655 ?
C71 H71 0.9500 . ?
C72 C73 1.390(2) . ?
C72 H72 0.9500 . ?
C73 C74 1.3866(19) . ?
C73 H73 0.9500 . ?
C74 H74 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
O13 Al1 O3 96.66(8) . . ?
O13 Al1 O10 98.66(7) . . ?
O3 Al1 O10 164.50(8) . . ?
O13 Al1 O1 97.46(7) . . ?
O3 Al1 O1 92.63(10) . . ?
O10 Al1 O1 87.70(9) . . ?
O13 Al1 O12 97.49(7) . . ?
O3 Al1 O12 86.98(10) . . ?
O10 Al1 O12 88.71(9) . . ?
O1 Al1 O12 164.98(8) . . ?
O13 Al1 N1 177.19(9) . . ?
O3 Al1 N1 83.85(9) . . ?
O10 Al1 N1 80.97(9) . . ?
O1 Al1 N1 79.75(9) . . ?
O12 Al1 N1 85.29(9) . . ?
O13 Al2 O2 96.79(8) . . ?
O13 Al2 O5 94.90(8) . . ?
O2 Al2 O5 87.21(12) . . ?
O13 Al2 O7 97.20(7) . . ?
O2 Al2 O7 165.99(8) . . ?
O5 Al2 O7 90.71(10) . . ?
O13 Al2 O4 94.02(7) . . ?
O2 Al2 O4 91.87(10) . . ?
O5 Al2 O4 171.08(8) . . ?
O7 Al2 O4 88.04(9) . . ?
O13 Al2 N2 179.29(8) . . ?
O2 Al2 N2 83.64(8) . . ?
O5 Al2 N2 85.69(8) . . ?
O7 Al2 N2 82.39(8) . . ?
O4 Al2 N2 85.39(7) . . ?
O13 Al3 O6 93.84(8) . . ?
O13 Al3 O11 95.08(7) . . ?
O6 Al3 O11 170.33(9) . . ?
O13 Al3 O9 97.31(8) . . ?
O6 Al3 O9 85.96(11) . . ?
O11 Al3 O9 89.19(10) . . ?
O13 Al3 O8 96.31(7) . . ?
O6 Al3 O8 93.59(10) . . ?
O11 Al3 O8 89.15(8) . . ?
O9 Al3 O8 166.38(8) . . ?
O13 Al3 N3 177.40(8) . . ?
O6 Al3 N3 84.82(8) . . ?
O11 Al3 N3 86.42(8) . . ?
O9 Al3 N3 84.83(8) . . ?
O8 Al3 N3 81.57(8) . . ?
C1 O1 Al1 131.19(15) . . ?
C1 O2 Al2 133.20(16) . . ?
C2 O3 Al1 129.92(15) . . ?
C2 O4 Al2 132.73(16) . . ?
C3 O5 Al2 131.93(16) . . ?
C3 O6 Al3 132.39(17) . . ?
C4 O7 Al2 130.48(15) . . ?
C4 O8 Al3 132.49(15) . . ?
C5 O9 Al3 133.60(16) . . ?
C5 O10 Al1 129.95(15) . . ?
C6 O11 Al3 131.18(16) . . ?
C6 O12 Al1 130.47(15) . . ?
Al1 O13 Al3 119.78(8) . . ?
Al1 O13 Al2 120.02(8) . . ?
Al3 O13 Al2 120.17(8) . . ?
C7B N1 C10 111.7(7) . . ?
C7A N1 C10 103.9(6) . . ?
C7B N1 Al1 126.6(7) . . ?
C7A N1 Al1 124.5(4) . . ?
C10 N1 Al1 121.02(18) . . ?
C11 N2 C14 104.77(17) . . ?
C11 N2 Al2 117.24(14) . . ?
C14 N2 Al2 116.82(14) . . ?
C11 N2 H2 105.2(19) . . ?
C14 N2 H2 105.8(19) . . ?
Al2 N2 H2 105.9(19) . . ?
C15 N3 C18 105.04(18) . . ?
C15 N3 Al3 116.14(15) . . ?
C18 N3 Al3 117.19(15) . . ?
C15 N3 H3 105(2) . . ?
C18 N3 H3 106(2) . . ?
Al3 N3 H3 106(2) . . ?
C1 N4 C19 123.9(2) . . ?
C1 N4 C22 123.4(2) . . ?
C19 N4 C22 112.6(2) . . ?
C2 N5 C23 123.4(2) . . ?
C2 N5 C26 123.6(2) . . ?
C23 N5 C26 112.4(2) . . ?
C3 N6 C27 124.5(2) . . ?
C3 N6 C30 122.8(2) . . ?
C27 N6 C30 112.68(19) . . ?
C4 N7 C31 123.8(2) . . ?
C4 N7 C34 123.3(2) . . ?
C31 N7 C34 112.7(2) . . ?
C5 N8 C38 123.0(2) . . ?
C5 N8 C35 124.4(2) . . ?
C38 N8 C35 112.5(2) . . ?
C6 N9 C42 123.6(2) . . ?
C6 N9 C39 123.2(2) . . ?
C42 N9 C39 113.2(2) . . ?
O2 C1 O1 124.3(2) . . ?
O2 C1 N4 117.3(2) . . ?
O1 C1 N4 118.3(2) . . ?
O4 C2 O3 125.2(2) . . ?
O4 C2 N5 117.7(2) . . ?
O3 C2 N5 117.1(2) . . ?
O5 C3 O6 124.5(2) . . ?
O5 C3 N6 118.8(2) . . ?
O6 C3 N6 116.7(2) . . ?
O7 C4 O8 125.2(2) . . ?
O7 C4 N7 117.42(19) . . ?
O8 C4 N7 117.35(19) . . ?
O9 C5 O10 124.4(2) . . ?
O9 C5 N8 118.1(2) . . ?
O10 C5 N8 117.4(2) . . ?
O12 C6 O11 125.8(2) . . ?
O12 C6 N9 116.8(2) . . ?
O11 C6 N9 117.4(2) . . ?
N1 C7A C8 106.5(6) . . ?
N1 C7A H7A 110.4 . . ?
C8 C7A H7A 110.4 . . ?
N1 C7A H7B 110.4 . . ?
C8 C7A H7B 110.4 . . ?
H7A C7A H7B 108.6 . . ?
N1 C7B C8 107.7(10) . . ?
N1 C7B H7C 110.2 . . ?
C8 C7B H7C 110.2 . . ?
N1 C7B H7D 110.2 . . ?
C8 C7B H7D 110.2 . . ?
H7C C7B H7D 108.5 . . ?
C9 C8 C7A 101.7(6) . . ?
C9 C8 C7B 106.0(6) . . ?
C9 C8 H8A 111.4 . . ?
C7A C8 H8A 111.4 . . ?
C9 C8 H8B 111.4 . . ?
C7A C8 H8B 111.4 . . ?
H8A C8 H8B 109.3 . . ?
C8 C9 C10 105.6(2) . . ?
C8 C9 H9A 110.6 . . ?
C10 C9 H9A 110.6 . . ?
C8 C9 H9B 110.6 . . ?
C10 C9 H9B 110.6 . . ?
H9A C9 H9B 108.7 . . ?
N1 C10 C9 108.7(3) . . ?
N1 C10 H10A 109.9 . . ?
C9 C10 H10A 109.9 . . ?
N1 C10 H10B 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
N2 C11 C12 106.49(18) . . ?
N2 C11 H11A 110.4 . . ?
C12 C11 H11A 110.4 . . ?
N2 C11 H11B 110.4 . . ?
C12 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
C13 C12 C11 104.4(2) . . ?
C13 C12 H12A 110.9 . . ?
C11 C12 H12A 110.9 . . ?
C13 C12 H12B 110.9 . . ?
C11 C12 H12B 110.9 . . ?
H12A C12 H12B 108.9 . . ?
C14 C13 C12 107.0(2) . . ?
C14 C13 H13A 110.3 . . ?
C12 C13 H13A 110.3 . . ?
C14 C13 H13B 110.3 . . ?
C12 C13 H13B 110.3 . . ?
H13A C13 H13B 108.6 . . ?
N2 C14 C13 107.8(2) . . ?
N2 C14 H14A 110.1 . . ?
C13 C14 H14A 110.1 . . ?
N2 C14 H14B 110.1 . . ?
C13 C14 H14B 110.1 . . ?
H14A C14 H14B 108.5 . . ?
N3 C15 C16 107.4(2) . . ?
N3 C15 H15A 110.2 . . ?
C16 C15 H15A 110.2 . . ?
N3 C15 H15B 110.2 . . ?
C16 C15 H15B 110.2 . . ?
H15A C15 H15B 108.5 . . ?
C17 C16 C15 106.0(2) . . ?
C17 C16 H16A 110.5 . . ?
C15 C16 H16A 110.5 . . ?
C17 C16 H16B 110.5 . . ?
C15 C16 H16B 110.5 . . ?
H16A C16 H16B 108.7 . . ?
C16 C17 C18 107.9(2) . . ?
C16 C17 H17A 110.1 . . ?
C18 C17 H17A 110.1 . . ?
C16 C17 H17B 110.1 . . ?
C18 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
N3 C18 C17 107.2(2) . . ?
N3 C18 H18A 110.3 . . ?
C17 C18 H18A 110.3 . . ?
N3 C18 H18B 110.3 . . ?
C17 C18 H18B 110.3 . . ?
H18A C18 H18B 108.5 . . ?
N4 C19 C20A 103.5(3) . . ?
N4 C19 C20B 101.1(9) . . ?
N4 C19 H19A 111.1 . . ?
C20A C19 H19A 111.1 . . ?
N4 C19 H19B 111.1 . . ?
C20A C19 H19B 111.1 . . ?
H19A C19 H19B 109.0 . . ?
C21 C20A C19 104.0(4) . . ?
C21 C20A H20A 111.0 . . ?
C19 C20A H20A 111.0 . . ?
C21 C20A H20B 111.0 . . ?
C19 C20A H20B 111.0 . . ?
H20A C20A H20B 109.0 . . ?
C21 C20B C19 109.0(12) . . ?
C21 C20B H20C 109.9 . . ?
C19 C20B H20C 109.9 . . ?
C21 C20B H20D 109.9 . . ?
C19 C20B H20D 109.9 . . ?
H20C C20B H20D 108.3 . . ?
C20B C21 C22 109.7(8) . . ?
C20A C21 C22 106.8(3) . . ?
C20A C21 H21A 110.4 . . ?
C22 C21 H21A 110.4 . . ?
C20A C21 H21B 110.4 . . ?
C22 C21 H21B 110.4 . . ?
H21A C21 H21B 108.6 . . ?
N4 C22 C21 103.0(2) . . ?
N4 C22 H22A 111.2 . . ?
C21 C22 H22A 111.2 . . ?
N4 C22 H22B 111.2 . . ?
C21 C22 H22B 111.2 . . ?
H22A C22 H22B 109.1 . . ?
N5 C23 C24A 104.9(5) . . ?
N5 C23 C24B 99.6(6) . . ?
N5 C23 H23A 110.8 . . ?
C24A C23 H23A 110.8 . . ?
N5 C23 H23B 110.8 . . ?
C24A C23 H23B 110.8 . . ?
H23A C23 H23B 108.8 . . ?
C23 C24A C25A 98.9(9) . . ?
C23 C24A H24A 112.0 . . ?
C25A C24A H24A 112.0 . . ?
C23 C24A H24B 112.0 . . ?
C25A C24A H24B 112.0 . . ?
H24A C24A H24B 109.7 . . ?
C26 C25A C24A 97.8(10) . . ?
C26 C25A H25A 112.2 . . ?
C24A C25A H25A 112.2 . . ?
C26 C25A H25B 112.2 . . ?
C24A C25A H25B 112.2 . . ?
H25A C25A H25B 109.8 . . ?
C25B C24B C23 103.8(10) . . ?
C25B C24B H24C 111.0 . . ?
C23 C24B H24C 111.0 . . ?
C25B C24B H24D 111.0 . . ?
C23 C24B H24D 111.0 . . ?
H24C C24B H24D 109.0 . . ?
C24B C25B C26 103.7(11) . . ?
C24B C25B H25C 111.0 . . ?
C26 C25B H25C 111.0 . . ?
C24B C25B H25D 111.0 . . ?
C26 C25B H25D 111.0 . . ?
H25C C25B H25D 109.0 . . ?
N5 C26 C25B 105.1(5) . . ?
N5 C26 C25A 101.0(4) . . ?
N5 C26 H26A 111.6 . . ?
C25A C26 H26A 111.6 . . ?
N5 C26 H26B 111.6 . . ?
C25A C26 H26B 111.6 . . ?
H26A C26 H26B 109.4 . . ?
N6 C27 C28 103.1(2) . . ?
N6 C27 H27A 111.1 . . ?
C28 C27 H27A 111.1 . . ?
N6 C27 H27B 111.1 . . ?
C28 C27 H27B 111.1 . . ?
H27A C27 H27B 109.1 . . ?
C29 C28 C27 104.2(2) . . ?
C29 C28 H28A 110.9 . . ?
C27 C28 H28A 110.9 . . ?
C29 C28 H28B 110.9 . . ?
C27 C28 H28B 110.9 . . ?
H28A C28 H28B 108.9 . . ?
C30 C29 C28 104.0(2) . . ?
C30 C29 H29A 111.0 . . ?
C28 C29 H29A 111.0 . . ?
C30 C29 H29B 111.0 . . ?
C28 C29 H29B 111.0 . . ?
H29A C29 H29B 109.0 . . ?
N6 C30 C29 103.7(2) . . ?
N6 C30 H30A 111.0 . . ?
C29 C30 H30A 111.0 . . ?
N6 C30 H30B 111.0 . . ?
C29 C30 H30B 111.0 . . ?
H30A C30 H30B 109.0 . . ?
N7 C31 C32B 110.2(4) . . ?
N7 C31 C32A 97.6(3) . . ?
N7 C31 H31A 112.2 . . ?
C32A C31 H31A 112.2 . . ?
N7 C31 H31B 112.2 . . ?
C32A C31 H31B 112.2 . . ?
H31A C31 H31B 109.8 . . ?
C33A C32A C31 104.3(3) . . ?
C33A C32A H32A 110.9 . . ?
C31 C32A H32A 110.9 . . ?
C33A C32A H32B 110.9 . . ?
C31 C32A H32B 110.9 . . ?
H32A C32A H32B 108.9 . . ?
C34 C33A C32A 97.8(4) . . ?
C34 C33A H33A 112.2 . . ?
C32A C33A H33A 112.2 . . ?
C34 C33A H33B 112.2 . . ?
C32A C33A H33B 112.2 . . ?
H33A C33A H33B 109.8 . . ?
C31 C32B C33B 95.0(6) . . ?
C31 C32B H32C 112.7 . . ?
C33B C32B H32C 112.7 . . ?
C31 C32B H32D 112.7 . . ?
C33B C32B H32D 112.7 . . ?
H32C C32B H32D 110.2 . . ?
C32B C33B C34 103.2(5) . . ?
C32B C33B H33C 111.1 . . ?
C34 C33B H33C 111.1 . . ?
C32B C33B H33D 111.1 . . ?
C34 C33B H33D 111.1 . . ?
H33C C33B H33D 109.1 . . ?
N7 C34 C33A 107.1(3) . . ?
N7 C34 C33B 93.5(3) . . ?
N7 C34 H34A 110.3 . . ?
C33A C34 H34A 110.3 . . ?
N7 C34 H34B 110.3 . . ?
C33A C34 H34B 110.3 . . ?
H34A C34 H34B 108.5 . . ?
N8 C35 C36 102.4(2) . . ?
N8 C35 H35A 111.3 . . ?
C36 C35 H35A 111.3 . . ?
N8 C35 H35B 111.3 . . ?
C36 C35 H35B 111.3 . . ?
H35A C35 H35B 109.2 . . ?
C37 C36 C35 104.7(3) . . ?
C37 C36 H36A 110.8 . . ?
C35 C36 H36A 110.8 . . ?
C37 C36 H36B 110.8 . . ?
C35 C36 H36B 110.8 . . ?
H36A C36 H36B 108.9 . . ?
C36 C37 C38 104.3(2) . . ?
C36 C37 H37A 110.9 . . ?
C38 C37 H37A 110.9 . . ?
C36 C37 H37B 110.9 . . ?
C38 C37 H37B 110.9 . . ?
H37A C37 H37B 108.9 . . ?
N8 C38 C37 103.6(2) . . ?
N8 C38 H38A 111.0 . . ?
C37 C38 H38A 111.0 . . ?
N8 C38 H38B 111.0 . . ?
C37 C38 H38B 111.0 . . ?
H38A C38 H38B 109.0 . . ?
N9 C39 C40B 102.9(4) . . ?
N9 C39 C40A 102.3(5) . . ?
N9 C39 H39A 111.3 . . ?
C40A C39 H39A 111.3 . . ?
N9 C39 H39B 111.3 . . ?
C40A C39 H39B 111.3 . . ?
H39A C39 H39B 109.2 . . ?
C41A C40A C39 106.4(11) . . ?
C41A C40A H40A 110.5 . . ?
C39 C40A H40A 110.5 . . ?
C41A C40A H40B 110.5 . . ?
C39 C40A H40B 110.5 . . ?
H40A C40A H40B 108.6 . . ?
C40A C41A C42 103.6(12) . . ?
C40A C41A H41A 111.0 . . ?
C42 C41A H41A 111.0 . . ?
C40A C41A H41B 111.0 . . ?
C42 C41A H41B 111.0 . . ?
H41A C41A H41B 109.0 . . ?
C39 C40B C41B 100.1(10) . . ?
C39 C40B H40C 111.8 . . ?
C41B C40B H40C 111.8 . . ?
C39 C40B H40D 111.8 . . ?
C41B C40B H40D 111.8 . . ?
H40C C40B H40D 109.5 . . ?
C42 C41B C40B 102.0(11) . . ?
C42 C41B H41C 111.4 . . ?
C40B C41B H41C 111.4 . . ?
C42 C41B H41D 111.4 . . ?
C40B C41B H41D 111.4 . . ?
H41C C41B H41D 109.2 . . ?
N9 C42 C41B 102.6(6) . . ?
N9 C42 C41A 102.7(6) . . ?
N9 C42 H42A 111.2 . . ?
C41A C42 H42A 111.2 . . ?
N9 C42 H42B 111.2 . . ?
C41A C42 H42B 111.2 . . ?
H42A C42 H42B 109.1 . . ?
C44 C43 C48 119.9(3) . . ?
C44 C43 H43 120.1 . . ?
C48 C43 H43 120.1 . . ?
C43 C44 C45 118.7(3) . . ?
C43 C44 H44 120.6 . . ?
C45 C44 H44 120.6 . . ?
C46 C45 C44 119.5(3) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C47 C46 C45 120.4(3) . . ?
C47 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C46 C47 C48 120.8(3) . . ?
C46 C47 H47 119.6 . . ?
C48 C47 H47 119.6 . . ?
C47 C48 C43 120.6(3) . . ?
C47 C48 H48 119.7 . . ?
C43 C48 H48 119.7 . . ?
C50 C49 C54 120.4(4) . . ?
C50 C49 H49 119.8 . . ?
C54 C49 H49 119.8 . . ?
C49 C50 C51 120.9(5) . . ?
C49 C50 H50 119.6 . . ?
C51 C50 H50 119.6 . . ?
C50 C51 C52 117.7(4) . . ?
C50 C51 H51 121.2 . . ?
C52 C51 H51 121.2 . . ?
C51 C52 C53 122.5(4) . . ?
C51 C52 H52 118.7 . . ?
C53 C52 H52 118.7 . . ?
C52 C53 C54 118.4(4) . . ?
C52 C53 H53 120.8 . . ?
C54 C53 H53 120.8 . . ?
C49 C54 C53 119.8(4) . . ?
C49 C54 H54 120.1 . . ?
C53 C54 H54 120.1 . . ?
C56 C55 C56 120.7(4) 2 . ?
C56 C55 H55 119.6 2 . ?
C56 C55 H55 119.6 . . ?
C55 C56 C57 119.4(3) . . ?
C55 C56 H56 120.3 . . ?
C57 C56 H56 120.3 . . ?
C58 C57 C56 120.5(3) . . ?
C58 C57 H57 119.8 . . ?
C56 C57 H57 119.8 . . ?
C57 C58 C57 119.5(4) . 2 ?
C57 C58 H58 120.3 . . ?
C57 C58 H58 120.3 2 . ?
C64 C59 C60 120.7(3) . . ?
C64 C59 H59 119.6 . . ?
C60 C59 H59 119.6 . . ?
C61 C60 C59 120.5(3) . . ?
C61 C60 H60 119.8 . . ?
C59 C60 H60 119.8 . . ?
C62 C61 C60 119.5(3) . . ?
C62 C61 H61 120.2 . . ?
C60 C61 H61 120.2 . . ?
C61 C62 C63 119.3(3) . . ?
C61 C62 H62 120.4 . . ?
C63 C62 H62 120.4 . . ?
C64 C63 C62 121.0(3) . . ?
C64 C63 H63 119.5 . . ?
C62 C63 H63 119.5 . . ?
C59 C64 C63 119.0(3) . . ?
C59 C64 H64 120.5 . . ?
C63 C64 H64 120.5 . . ?
C66 C65 C70 120.8(3) . . ?
C66 C65 H65 119.6 . . ?
C70 C65 H65 119.6 . . ?
C67 C66 C65 120.2(3) . . ?
C67 C66 H66 119.9 . . ?
C65 C66 H66 119.9 . . ?
C68 C67 C66 119.2(3) . . ?
C68 C67 H67 120.4 . . ?
C66 C67 H67 120.4 . . ?
C67 C68 C69 121.0(3) . . ?
C67 C68 H68 119.5 . . ?
C69 C68 H68 119.5 . . ?
C68 C69 C70 120.1(3) . . ?
C68 C69 H69 119.9 . . ?
C70 C69 H69 119.9 . . ?
C69 C70 C65 118.6(3) . . ?
C69 C70 H70 120.7 . . ?
C65 C70 H70 120.7 . . ?
C72 C71 C72 119.4(7) . 2_655 ?
C72 C71 H71 120.3 . . ?
C72 C71 H71 120.3 2_655 . ?
C73 C72 C71 120.5(6) . . ?
C73 C72 H72 119.8 . . ?
C71 C72 H72 119.8 . . ?
C74 C73 C72 119.3(5) . . ?
C74 C73 H73 120.3 . . ?
C72 C73 H73 120.3 . . ?
C73 C74 C73 120.9(6) . 2_655 ?
C73 C74 H74 119.5 . . ?
C73 C74 H74 119.5 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O13 Al2 O2 C1 -18.2(3) . . . . ?
O5 Al2 O2 C1 -112.8(3) . . . . ?
O7 Al2 O2 C1 165.5(3) . . . . ?
O4 Al2 O2 C1 76.1(3) . . . . ?
N2 Al2 O2 C1 161.2(3) . . . . ?
O13 Al1 O3 C2 -17.8(3) . . . . ?
O10 Al1 O3 C2 170.9(3) . . . . ?
O1 Al1 O3 C2 80.0(2) . . . . ?
O12 Al1 O3 C2 -115.0(2) . . . . ?
N1 Al1 O3 C2 159.4(3) . . . . ?
O13 Al2 O5 C3 9.5(3) . . . . ?
O2 Al2 O5 C3 106.1(3) . . . . ?
O7 Al2 O5 C3 -87.8(3) . . . . ?
N2 Al2 O5 C3 -170.1(3) . . . . ?
O13 Al3 O6 C3 -24.6(3) . . . . ?
O9 Al3 O6 C3 -121.7(3) . . . . ?
O8 Al3 O6 C3 72.0(3) . . . . ?
N3 Al3 O6 C3 153.2(3) . . . . ?
O13 Al2 O7 C4 -30.1(2) . . . . ?
O2 Al2 O7 C4 146.2(4) . . . . ?
O5 Al2 O7 C4 65.0(2) . . . . ?
O4 Al2 O7 C4 -123.9(2) . . . . ?
N2 Al2 O7 C4 150.5(2) . . . . ?
O13 Al1 O10 C5 -24.1(2) . . . . ?
O3 Al1 O10 C5 147.2(3) . . . . ?
O1 Al1 O10 C5 -121.3(2) . . . . ?
O12 Al1 O10 C5 73.3(2) . . . . ?
N1 Al1 O10 C5 158.8(2) . . . . ?
O13 Al3 O11 C6 -31.6(2) . . . . ?
O9 Al3 O11 C6 65.6(2) . . . . ?
O8 Al3 O11 C6 -127.9(2) . . . . ?
N3 Al3 O11 C6 150.5(2) . . . . ?
O3 Al1 O13 Al3 -132.92(10) . . . . ?
O10 Al1 O13 Al3 44.73(11) . . . . ?
O1 Al1 O13 Al3 133.53(10) . . . . ?
O12 Al1 O13 Al3 -45.10(11) . . . . ?
O3 Al1 O13 Al2 49.26(11) . . . . ?
O10 Al1 O13 Al2 -133.09(10) . . . . ?
O1 Al1 O13 Al2 -44.29(11) . . . . ?
O12 Al1 O13 Al2 137.08(10) . . . . ?
O6 Al3 O13 Al1 -126.66(11) . . . . ?
O11 Al3 O13 Al1 49.58(11) . . . . ?
O9 Al3 O13 Al1 -40.25(12) . . . . ?
O8 Al3 O13 Al1 139.29(10) . . . . ?
O6 Al3 O13 Al2 51.15(12) . . . . ?
O11 Al3 O13 Al2 -132.60(10) . . . . ?
O9 Al3 O13 Al2 137.56(11) . . . . ?
O8 Al3 O13 Al2 -42.90(11) . . . . ?
O2 Al2 O13 Al1 43.82(12) . . . . ?
O5 Al2 O13 Al1 131.59(12) . . . . ?
O7 Al2 O13 Al1 -137.08(10) . . . . ?
O4 Al2 O13 Al1 -48.55(11) . . . . ?
O2 Al2 O13 Al3 -133.99(11) . . . . ?
O5 Al2 O13 Al3 -46.22(12) . . . . ?
O7 Al2 O13 Al3 45.11(11) . . . . ?
O4 Al2 O13 Al3 133.64(10) . . . . ?
Al2 O2 C1 O1 -4.8(4) . . . . ?
Al2 O2 C1 N4 175.2(2) . . . . ?
Al1 O1 C1 O2 4.2(4) . . . . ?
Al1 O1 C1 N4 -175.89(17) . . . . ?
C19 N4 C1 O2 178.1(3) . . . . ?
C22 N4 C1 O2 -5.3(4) . . . . ?
C19 N4 C1 O1 -1.9(4) . . . . ?
C22 N4 C1 O1 174.8(2) . . . . ?
Al2 O4 C2 O3 10.5(4) . . . . ?
Al2 O4 C2 N5 -170.15(18) . . . . ?
Al1 O3 C2 O4 -10.7(4) . . . . ?
Al1 O3 C2 N5 169.95(19) . . . . ?
C23 N5 C2 O4 176.0(3) . . . . ?
C26 N5 C2 O4 4.7(4) . . . . ?
C23 N5 C2 O3 -4.6(4) . . . . ?
C26 N5 C2 O3 -175.9(3) . . . . ?
Al2 O5 C3 O6 16.9(4) . . . . ?
Al2 O5 C3 N6 -163.5(2) . . . . ?
Al3 O6 C3 O5 -7.3(4) . . . . ?
Al3 O6 C3 N6 173.12(19) . . . . ?
C27 N6 C3 O5 -3.1(4) . . . . ?
C30 N6 C3 O5 176.1(2) . . . . ?
C27 N6 C3 O6 176.5(3) . . . . ?
C30 N6 C3 O6 -4.3(3) . . . . ?
Al2 O7 C4 O8 15.4(4) . . . . ?
Al2 O7 C4 N7 -164.51(16) . . . . ?
Al3 O8 C4 O7 -12.4(4) . . . . ?
Al3 O8 C4 N7 167.53(16) . . . . ?
C31 N7 C4 O7 -2.1(3) . . . . ?
C34 N7 C4 O7 -176.4(3) . . . . ?
C31 N7 C4 O8 178.0(2) . . . . ?
C34 N7 C4 O8 3.6(3) . . . . ?
Al3 O9 C5 O10 8.5(4) . . . . ?
Al3 O9 C5 N8 -172.3(2) . . . . ?
Al1 O10 C5 O9 -1.2(4) . . . . ?
Al1 O10 C5 N8 179.61(17) . . . . ?
C38 N8 C5 O9 -171.2(3) . . . . ?
C35 N8 C5 O9 6.9(4) . . . . ?
C38 N8 C5 O10 8.0(4) . . . . ?
C35 N8 C5 O10 -173.8(3) . . . . ?
Al1 O12 C6 O11 0.2(4) . . . . ?
Al1 O12 C6 N9 179.78(18) . . . . ?
Al3 O11 C6 O12 9.0(4) . . . . ?
Al3 O11 C6 N9 -170.51(17) . . . . ?
C42 N9 C6 O12 -0.9(4) . . . . ?
C39 N9 C6 O12 -178.9(3) . . . . ?
C42 N9 C6 O11 178.7(3) . . . . ?
C39 N9 C6 O11 0.7(4) . . . . ?
C10 N1 C7A C8 -36.7(13) . . . . ?
Al1 N1 C7A C8 178.8(5) . . . . ?
C10 N1 C7B C8 3.2(18) . . . . ?
Al1 N1 C7B C8 -167.4(6) . . . . ?
N1 C7A C8 C9 34.8(13) . . . . ?
N1 C7B C8 C9 -4.8(17) . . . . ?
C7A C8 C9 C10 -18.3(8) . . . . ?
C7B C8 C9 C10 4.4(10) . . . . ?
C7B N1 C10 C9 -0.5(12) . . . . ?
C7A N1 C10 C9 24.7(9) . . . . ?
Al1 N1 C10 C9 170.8(3) . . . . ?
C8 C9 C10 N1 -2.7(5) . . . . ?
C14 N2 C11 C12 -31.3(3) . . . . ?
Al2 N2 C11 C12 -162.67(16) . . . . ?
N2 C11 C12 C13 27.7(3) . . . . ?
C11 C12 C13 C14 -13.4(3) . . . . ?
C11 N2 C14 C13 22.8(3) . . . . ?
Al2 N2 C14 C13 154.3(2) . . . . ?
C12 C13 C14 N2 -5.6(3) . . . . ?
C18 N3 C15 C16 -26.0(3) . . . . ?
Al3 N3 C15 C16 -157.2(2) . . . . ?
N3 C15 C16 C17 20.0(4) . . . . ?
C15 C16 C17 C18 -6.1(4) . . . . ?
C15 N3 C18 C17 22.0(3) . . . . ?
Al3 N3 C18 C17 152.6(2) . . . . ?
C16 C17 C18 N3 -9.9(4) . . . . ?
C1 N4 C19 C20A 165.9(6) . . . . ?
C22 N4 C19 C20A -11.1(6) . . . . ?
C1 N4 C19 C20B -165.2(16) . . . . ?
C22 N4 C19 C20B 17.9(16) . . . . ?
N4 C19 C20A C21 26.4(9) . . . . ?
N4 C19 C20B C21 -21(3) . . . . ?
C19 C20B C21 C22 18(3) . . . . ?
C19 C20A C21 C22 -32.6(9) . . . . ?
C1 N4 C22 C21 174.6(3) . . . . ?
C19 N4 C22 C21 -8.4(4) . . . . ?
C20B C21 C22 N4 -6.2(19) . . . . ?
C20A C21 C22 N4 25.5(7) . . . . ?
C2 N5 C23 C24A 173.1(8) . . . . ?
C26 N5 C23 C24A -14.8(9) . . . . ?
C2 N5 C23 C24B -160.2(8) . . . . ?
C26 N5 C23 C24B 11.9(8) . . . . ?
N5 C23 C24A C25A 39.0(14) . . . . ?
C23 C24A C25A C26 -48.4(15) . . . . ?
N5 C23 C24B C25B -31.5(17) . . . . ?
C23 C24B C25B C26 40(2) . . . . ?
C2 N5 C26 C25B -176.2(9) . . . . ?
C23 N5 C26 C25B 11.6(10) . . . . ?
C2 N5 C26 C25A 154.3(8) . . . . ?
C23 N5 C26 C25A -17.8(8) . . . . ?
C24B C25B C26 N5 -32.3(19) . . . . ?
C24A C25A C26 N5 39.4(13) . . . . ?
C3 N6 C27 C28 -171.2(3) . . . . ?
C30 N6 C27 C28 9.5(3) . . . . ?
N6 C27 C28 C29 -27.5(4) . . . . ?
C27 C28 C29 C30 35.5(3) . . . . ?
C3 N6 C30 C29 -166.9(2) . . . . ?
C27 N6 C30 C29 12.4(3) . . . . ?
C28 C29 C30 N6 -29.3(3) . . . . ?
C4 N7 C31 C32B 173.3(4) . . . . ?
C34 N7 C31 C32B -11.8(5) . . . . ?
C4 N7 C31 C32A -158.8(3) . . . . ?
C34 N7 C31 C32A 16.1(4) . . . . ?
N7 C31 C32A C33A -38.1(5) . . . . ?
C31 C32A C33A C34 44.6(5) . . . . ?
N7 C31 C32B C33B 38.4(7) . . . . ?
C31 C32B C33B C34 -48.8(7) . . . . ?
C4 N7 C34 C33A -173.5(3) . . . . ?
C31 N7 C34 C33A 11.5(4) . . . . ?
C4 N7 C34 C33B 156.4(4) . . . . ?
C31 N7 C34 C33B -18.6(4) . . . . ?
C32A C33A C34 N7 -34.7(5) . . . . ?
C32B C33B C34 N7 42.3(6) . . . . ?
C5 N8 C35 C36 -163.7(3) . . . . ?
C38 N8 C35 C36 14.6(4) . . . . ?
N8 C35 C36 C37 -30.6(4) . . . . ?
C35 C36 C37 C38 35.7(4) . . . . ?
C5 N8 C38 C37 -174.6(3) . . . . ?
C35 N8 C38 C37 7.0(3) . . . . ?
C36 C37 C38 N8 -26.1(4) . . . . ?
C6 N9 C39 C40B 163.6(9) . . . . ?
C42 N9 C39 C40B -14.6(9) . . . . ?
C6 N9 C39 C40A -170.5(8) . . . . ?
C42 N9 C39 C40A 11.3(9) . . . . ?
N9 C39 C40A C41A -29.4(18) . . . . ?
C39 C40A C41A C42 35(2) . . . . ?
N9 C39 C40B C41B 34.5(14) . . . . ?
C39 C40B C41B C42 -44.0(17) . . . . ?
C6 N9 C42 C41B 167.7(8) . . . . ?
C39 N9 C42 C41B -14.1(8) . . . . ?
C6 N9 C42 C41A -169.1(8) . . . . ?
C39 N9 C42 C41A 9.1(8) . . . . ?
C40B C41B C42 N9 34.9(14) . . . . ?
C40A C41A C42 N9 -27.2(17) . . . . ?
C48 C43 C44 C45 -1.5(6) . . . . ?
C43 C44 C45 C46 0.4(6) . . . . ?
C44 C45 C46 C47 1.5(6) . . . . ?
C45 C46 C47 C48 -2.3(6) . . . . ?
C46 C47 C48 C43 1.1(5) . . . . ?
C44 C43 C48 C47 0.8(6) . . . . ?
C54 C49 C50 C51 -2.5(10) . . . . ?
C49 C50 C51 C52 5.1(9) . . . . ?
C50 C51 C52 C53 -2.7(9) . . . . ?
C51 C52 C53 C54 -2.2(9) . . . . ?
C50 C49 C54 C53 -2.6(9) . . . . ?
C52 C53 C54 C49 4.9(8) . . . . ?
C56 C55 C56 C57 -0.26(19) 2 . . . ?
C55 C56 C57 C58 0.5(4) . . . . ?
C56 C57 C58 C57 -0.26(19) . . . 2 ?
C64 C59 C60 C61 0.8(6) . . . . ?
C59 C60 C61 C62 -0.6(6) . . . . ?
C60 C61 C62 C63 0.3(6) . . . . ?
C61 C62 C63 C64 -0.3(6) . . . . ?
C60 C59 C64 C63 -0.8(6) . . . . ?
C62 C63 C64 C59 0.6(5) . . . . ?
C70 C65 C66 C67 -2.2(7) . . . . ?
C65 C66 C67 C68 0.8(6) . . . . ?
C66 C67 C68 C69 1.5(6) . . . . ?
C67 C68 C69 C70 -2.4(6) . . . . ?
C68 C69 C70 C65 0.9(7) . . . . ?
C66 C65 C70 C69 1.3(7) . . . . ?
C72 C71 C72 C73 -1.6(4) 2_655 . . . ?
C71 C72 C73 C74 3.1(8) . . . . ?
C72 C73 C74 C73 -1.6(4) . . . 2_655 ?

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
_geom_hbond_publ_flag
N2 H2 Cl1 0.88(3) 2.62(3) 3.401(2) 147(2) 4_445 yes
N3 H3 Cl1 0.85(3) 2.57(3) 3.330(2) 150(3) 7 yes
C7B^b H7D^b O12 0.99 2.58 3.081(17) 111.6 . yes
C10 H10A O3 0.99 2.48 2.998(4) 112.0 . yes
C11 H11B O7 0.99 2.57 3.077(3) 111.4 . yes
C12 H12B Cl1 0.99 2.89 3.538(3) 123.5 4_445 yes
C14 H14A O7 0.99 2.59 3.087(3) 111.3 . yes
C15 H15B O8 0.99 2.54 3.052(3) 111.7 . yes
C18 H18A O8 0.99 2.55 3.049(3) 111.3 . yes
C22 H22A Cl1 0.99 2.75 3.685(3) 156.7 4_445 yes
C35 H35B Cl1 0.99 2.73 3.669(3) 158.9 7 yes

_refine_diff_density_max         0.639
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.058

####################################################################### 
# 
# 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_es1432_sq2
_database_code_depnum_ccdc_archive 'CCDC 2257496'
loop_
_audit_author_name
_audit_author_address
'Uwe Boehme'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2023-04-19 deposited with the CCDC.	2023-08-09 downloaded from the CCDC.
;





_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          455
_chemical_formula_moiety         'C45 H63 Al3 N9 O13, 4(C H Cl3), Cl'
_chemical_formula_sum            'C49 H67 Al3 Cl13 N9 O13'
_chemical_formula_weight         1531.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   12.8674(2)
_cell_length_b                   25.1293(4)
_cell_length_c                   22.9381(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.8100(10)
_cell_angle_gamma                90
_cell_volume                     7413.31(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    165289
_cell_measurement_theta_min      1.58
_cell_measurement_theta_max      28.09


_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_F_000             3152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    0.578
_shelx_estimated_absorpt_T_min   0.781
_shelx_estimated_absorpt_T_max   0.802

_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.8536
_exptl_absorpt_correction_T_max  0.9608
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
30 -1 -5 0.1362
8 -30 9 0.0629
4 -15 -5 0.0763
22 1 -30 0.1391
0 1 0 0.0612
-1 -3 30 0.1771
-1 -5 0 0.0909
-5 30 -9 0.0625
-8 30 3 0.0548
-9 0 10 0.1105
0 -1 -30 0.1707

_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_absorpt_special_details   ?


_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_voltage           50
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_ambient_temperature      183
_diffrn_measurement_method       'rotation method'
_diffrn_measurement_details      
; 394 frames, detector distance = 114 mm
;

_diffrn_reflns_number            130269
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.779
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             16985
_reflns_number_gt                14773
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2015b)'


_refine_special_details          
; 
 There is a disordered toluene molecule in the crystal structure. 
 Refinement of this molecule leads to unsatisfactory results. 
 Therefore, the toluene molecule has been removed with the SQUEEZE 
 procedure from PLATON. 
 Four molecules chloroform are as well in the structure. These 
 were refined properly. Two of the chloroform molecules are 
 disordered and were treated with a split atom model. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0482P)²+5.4400P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16985
_refine_ls_number_parameters     868
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1159
_refine_ls_wR_factor_gt          0.1082
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.74842(4) 0.42351(2) 0.18138(2) 0.04432(12) Uani 1 1 d . . . . .
Al1 Al 0.53385(4) 0.73700(2) 0.54594(2) 0.02086(10) Uani 1 1 d . . . . .
Al2 Al 0.77276(4) 0.73870(2) 0.57896(2) 0.02025(10) Uani 1 1 d . . . . .
Al3 Al 0.69753(3) 0.73505(2) 0.44687(2) 0.02034(10) Uani 1 1 d . . . . .
O1 O 0.54984(9) 0.69123(5) 0.61060(5) 0.0295(3) Uani 1 1 d . . . . .
O2 O 0.72243(9) 0.68259(5) 0.62558(5) 0.0289(3) Uani 1 1 d . . . . .
O3 O 0.54472(9) 0.79745(5) 0.59509(6) 0.0327(3) Uani 1 1 d . . . . .
O4 O 0.71072(9) 0.78993(5) 0.62763(5) 0.0302(3) Uani 1 1 d . . . . .
O5 O 0.86064(9) 0.68817(5) 0.54456(5) 0.0299(3) Uani 1 1 d . . . . .
O6 O 0.79168(10) 0.67733(5) 0.45366(5) 0.0291(3) Uani 1 1 d . . . . .
O7 O 0.84834(10) 0.79477(5) 0.54643(5) 0.0308(3) Uani 1 1 d . . . . .
O8 O 0.80809(9) 0.78397(5) 0.45109(5) 0.0289(3) Uani 1 1 d . . . . .
O9 O 0.59407(9) 0.68561(5) 0.42261(5) 0.0312(3) Uani 1 1 d . . . . .
O10 O 0.49171(9) 0.67756(5) 0.50015(5) 0.0290(2) Uani 1 1 d . . . . .
O11 O 0.60837(9) 0.79097(5) 0.42288(5) 0.0309(3) Uani 1 1 d . . . . .
O12 O 0.48160(9) 0.78377(5) 0.48793(5) 0.0313(3) Uani 1 1 d . . . . .
O13 O 0.66803(8) 0.73660(4) 0.52402(5) 0.0208(2) Uani 1 1 d . . . . .
N1 N 0.37729(11) 0.73659(6) 0.57173(6) 0.0253(3) Uani 1 1 d . . . . .
N2 N 0.89181(11) 0.74208(6) 0.64552(6) 0.0247(3) Uani 1 1 d . . . . .
N3 N 0.73857(10) 0.73417(6) 0.35775(6) 0.0233(3) Uani 1 1 d . . . . .
N4 N 0.61213(11) 0.63991(7) 0.68259(6) 0.0317(3) Uani 1 1 d . . . . .
N5 N 0.61603(12) 0.86052(6) 0.65169(7) 0.0342(3) Uani 1 1 d . . . . .
N6 N 0.92688(12) 0.62816(7) 0.48415(6) 0.0315(3) Uani 1 1 d . . . . .
N7 N 0.93001(11) 0.84210(6) 0.47957(6) 0.0272(3) Uani 1 1 d . . . . .
N8 N 0.45344(12) 0.63413(7) 0.41712(7) 0.0343(3) Uani 1 1 d . . . . .
N9 N 0.47039(12) 0.84485(6) 0.41788(6) 0.0307(3) Uani 1 1 d . . . . .
C1 C 0.62888(12) 0.67279(6) 0.63788(7) 0.0228(3) Uani 1 1 d . . . . .
C2 C 0.62453(13) 0.81422(7) 0.62347(7) 0.0247(3) Uani 1 1 d . . . . .
C3 C 0.85702(12) 0.66615(7) 0.49462(7) 0.0234(3) Uani 1 1 d . . . . .
C4 C 0.85904(12) 0.80559(6) 0.49276(7) 0.0223(3) Uani 1 1 d . . . . .
C5 C 0.51547(12) 0.66729(6) 0.44786(7) 0.0242(3) Uani 1 1 d . . . . .
C6 C 0.52263(12) 0.80504(7) 0.44420(7) 0.0244(3) Uani 1 1 d . . . . .
C7 C 0.32898(13) 0.69096(8) 0.58514(8) 0.0299(3) Uani 1 1 d . . . . .
H7 H 0.366773 0.658561 0.583318 0.036 Uiso 1 1 calc R U . . .
C8 C 0.22665(14) 0.68930(9) 0.60146(9) 0.0378(4) Uani 1 1 d . . . . .
H8 H 0.195082 0.656416 0.611095 0.045 Uiso 1 1 calc R U . . .
C9 C 0.17110(15) 0.73605(10) 0.60354(9) 0.0415(5) Uani 1 1 d . . . . .
H9 H 0.100096 0.735857 0.613711 0.050 Uiso 1 1 calc R U . . .
C10 C 0.22006(14) 0.78295(9) 0.59068(8) 0.0369(4) Uani 1 1 d . . . . .
H10 H 0.183695 0.815773 0.592580 0.044 Uiso 1 1 calc R U . . .
C11 C 0.32270(13) 0.78190(8) 0.57496(7) 0.0298(3) Uani 1 1 d . . . . .
H11 H 0.355958 0.814527 0.566077 0.036 Uiso 1 1 calc R U . . .
C12 C 0.92531(13) 0.78940(8) 0.66617(7) 0.0297(3) Uani 1 1 d . . . . .
H12 H 0.900570 0.820952 0.647616 0.036 Uiso 1 1 calc R U . . .
C13 C 0.99440(15) 0.79386(9) 0.71339(8) 0.0367(4) Uani 1 1 d . . . . .
H13 H 1.016846 0.827858 0.726822 0.044 Uiso 1 1 calc R U . . .
C14 C 1.03019(15) 0.74810(10) 0.74068(8) 0.0408(5) Uani 1 1 d . . . . .
H14 H 1.075384 0.750153 0.774162 0.049 Uiso 1 1 calc R U . . .
C15 C 0.99937(15) 0.69952(9) 0.71861(8) 0.0378(4) Uani 1 1 d . . . . .
H15 H 1.025529 0.667507 0.735512 0.045 Uiso 1 1 calc R U . . .
C16 C 0.92946(13) 0.69791(8) 0.67126(7) 0.0296(3) Uani 1 1 d . . . . .
H16 H 0.907506 0.664263 0.656559 0.036 Uiso 1 1 calc R U . . .
C17 C 0.75912(13) 0.78026(7) 0.33056(7) 0.0271(3) Uani 1 1 d . . . . .
H17 H 0.748747 0.812684 0.350860 0.033 Uiso 1 1 calc R U . . .
C18 C 0.79472(15) 0.78247(9) 0.27428(8) 0.0355(4) Uani 1 1 d . . . . .
H18 H 0.808248 0.815740 0.256384 0.043 Uiso 1 1 calc R U . . .
C19 C 0.81023(17) 0.73540(9) 0.24459(8) 0.0417(5) Uani 1 1 d . . . . .
H19 H 0.836121 0.735728 0.206265 0.050 Uiso 1 1 calc R U . . .
C20 C 0.78742(17) 0.68785(9) 0.27165(8) 0.0391(4) Uani 1 1 d . . . . .
H20 H 0.795930 0.654991 0.251889 0.047 Uiso 1 1 calc R U . . .
C21 C 0.75188(14) 0.68885(7) 0.32816(7) 0.0298(4) Uani 1 1 d . . . . .
H21 H 0.736365 0.656068 0.346592 0.036 Uiso 1 1 calc R U . . .
C22 C 0.50860(15) 0.62763(10) 0.70336(9) 0.0431(5) Uani 1 1 d . . . . .
H22A H 0.472829 0.601100 0.677911 0.052 Uiso 1 1 calc R U . . .
H22B H 0.465186 0.660072 0.705231 0.052 Uiso 1 1 calc R U . . .
C23 C 0.5315(2) 0.60524(14) 0.76348(12) 0.0694(9) Uani 1 1 d . . . . .
H23A H 0.531109 0.633780 0.793231 0.083 Uiso 1 1 calc R U . . .
H23B H 0.479446 0.578002 0.773461 0.083 Uiso 1 1 calc R U . . .
C24 C 0.6357(2) 0.58139(13) 0.76026(12) 0.0656(8) Uani 1 1 d . . . . .
H24A H 0.631054 0.544681 0.744746 0.079 Uiso 1 1 calc R U . . .
H24B H 0.670559 0.580343 0.799355 0.079 Uiso 1 1 calc R U . . .
C25 C 0.69496(16) 0.61679(9) 0.71957(9) 0.0408(5) Uani 1 1 d . . . . .
H25A H 0.734084 0.644688 0.741414 0.049 Uiso 1 1 calc R U . . .
H25B H 0.743864 0.595854 0.696253 0.049 Uiso 1 1 calc R U . . .
C26 C 0.52261(17) 0.89369(8) 0.64860(11) 0.0444(5) Uani 1 1 d . . . . .
H26A H 0.469680 0.880751 0.675613 0.053 Uiso 1 1 calc R U . . .
H26B H 0.491944 0.894751 0.608491 0.053 Uiso 1 1 calc R U . . .
C27 C 0.5642(2) 0.94779(10) 0.66712(14) 0.0663(8) Uani 1 1 d . . . . .
H27A H 0.589160 0.967882 0.633171 0.080 Uiso 1 1 calc R U . . .
H27B H 0.509999 0.968925 0.686214 0.080 Uiso 1 1 calc R U . . .
C28 C 0.6523(2) 0.93516(11) 0.70924(16) 0.0735(9) Uani 1 1 d . . . . .
H28A H 0.626346 0.927128 0.748445 0.088 Uiso 1 1 calc R U . . .
H28B H 0.701971 0.965198 0.712369 0.088 Uiso 1 1 calc R U . . .
C29 C 0.70322(18) 0.88635(9) 0.68287(12) 0.0514(6) Uani 1 1 d . . . . .
H29A H 0.758229 0.896660 0.655849 0.062 Uiso 1 1 calc R U . . .
H29B H 0.733564 0.862843 0.713585 0.062 Uiso 1 1 calc R U . . .
C30 C 1.00784(15) 0.61123(9) 0.52624(9) 0.0411(5) Uani 1 1 d . . . . .
H30A H 0.979213 0.587503 0.556224 0.049 Uiso 1 1 calc R U . . .
H30B H 1.041462 0.642207 0.545696 0.049 Uiso 1 1 calc R U . . .
C31 C 1.08391(17) 0.58163(10) 0.48850(11) 0.0499(6) Uani 1 1 d . . . . .
H31A H 1.136215 0.606222 0.472791 0.060 Uiso 1 1 calc R U . . .
H31B H 1.120171 0.553136 0.510932 0.060 Uiso 1 1 calc R U . . .
C32 C 1.01526(18) 0.55852(10) 0.43996(11) 0.0491(5) Uani 1 1 d . . . . .
H32A H 0.981609 0.525231 0.452652 0.059 Uiso 1 1 calc R U . . .
H32B H 1.055920 0.551038 0.404960 0.059 Uiso 1 1 calc R U . . .
C33 C 0.93475(15) 0.60187(8) 0.42755(8) 0.0351(4) Uani 1 1 d . . . . .
H33A H 0.958611 0.626973 0.397520 0.042 Uiso 1 1 calc R U . . .
H33B H 0.867191 0.586418 0.414463 0.042 Uiso 1 1 calc R U . . .
C34 C 1.00294(16) 0.86480(8) 0.52290(8) 0.0385(4) Uani 1 1 d . . . . .
H34A H 1.019083 0.839267 0.554789 0.046 Uiso 0.647(13) 1 calc R U P A 1
H34B H 0.975540 0.898084 0.539651 0.046 Uiso 0.647(13) 1 calc R U P A 1
H34C H 1.047617 0.836881 0.541011 0.046 Uiso 0.353(13) 1 calc R U P A 2
H34D H 0.965767 0.883729 0.553840 0.046 Uiso 0.353(13) 1 calc R U P A 2
C35A C 1.1007(4) 0.8758(3) 0.48550(17) 0.0422(12) Uani 0.647(13) 1 d . . P A 1
H35A H 1.145406 0.903979 0.502999 0.051 Uiso 0.647(13) 1 calc R U P A 1
H35B H 1.142347 0.843149 0.480051 0.051 Uiso 0.647(13) 1 calc R U P A 1
C36A C 1.0467(10) 0.8944(5) 0.4275(6) 0.055(3) Uani 0.647(13) 1 d . . P A 1
H36A H 1.022819 0.931718 0.430359 0.066 Uiso 0.647(13) 1 calc R U P A 1
H36B H 1.094361 0.891328 0.394574 0.066 Uiso 0.647(13) 1 calc R U P A 1
C35B C 1.0648(9) 0.9022(5) 0.4882(3) 0.047(3) Uani 0.353(13) 1 d . . P A 2
H35C H 1.136837 0.904734 0.504345 0.057 Uiso 0.353(13) 1 calc R U P A 2
H35D H 1.033158 0.938105 0.488059 0.057 Uiso 0.353(13) 1 calc R U P A 2
C36B C 1.0636(16) 0.8797(7) 0.4283(11) 0.040(3) Uani 0.353(13) 1 d . . P A 2
H36C H 1.117162 0.851634 0.424957 0.048 Uiso 0.353(13) 1 calc R U P A 2
H36D H 1.076331 0.907751 0.399133 0.048 Uiso 0.353(13) 1 calc R U P A 2
C37 C 0.95496(15) 0.85648(8) 0.41974(8) 0.0340(4) Uani 1 1 d . . . . .
H37A H 0.895292 0.874273 0.399624 0.041 Uiso 0.647(13) 1 calc R U P A 1
H37B H 0.974402 0.824646 0.397113 0.041 Uiso 0.647(13) 1 calc R U P A 1
H37C H 0.905572 0.883177 0.403367 0.041 Uiso 0.353(13) 1 calc R U P A 2
H37D H 0.955071 0.824864 0.393991 0.041 Uiso 0.353(13) 1 calc R U P A 2
C38 C 0.47224(18) 0.62034(10) 0.35653(9) 0.0478(6) Uani 1 1 d . . . . .
H38A H 0.541702 0.604001 0.352710 0.057 Uiso 1 1 calc R U . . .
H38B H 0.467067 0.652114 0.331080 0.057 Uiso 1 1 calc R U . . .
C39 C 0.38618(18) 0.58060(10) 0.34143(10) 0.0489(5) Uani 1 1 d . . . . .
H39A H 0.363363 0.583724 0.299947 0.059 Uiso 1 1 calc R U . . .
H39B H 0.409702 0.543681 0.349117 0.059 Uiso 1 1 calc R U . . .
C40 C 0.29927(17) 0.59597(10) 0.38135(10) 0.0469(5) Uani 1 1 d . . . . .
H40A H 0.252416 0.565449 0.387909 0.056 Uiso 1 1 calc R U . . .
H40B H 0.258010 0.625924 0.364789 0.056 Uiso 1 1 calc R U . . .
C41 C 0.35606(15) 0.61229(9) 0.43768(9) 0.0403(5) Uani 1 1 d . . . . .
H41A H 0.316301 0.639454 0.458895 0.048 Uiso 1 1 calc R U . . .
H41B H 0.368806 0.581245 0.463496 0.048 Uiso 1 1 calc R U . . .
C42 C 0.50337(17) 0.87065(9) 0.36445(8) 0.0403(4) Uani 1 1 d . . . . .
H42A H 0.521687 0.844063 0.334626 0.048 Uiso 1 1 calc R U . . .
H42B H 0.563710 0.894327 0.372247 0.048 Uiso 1 1 calc R U . . .
C43 C 0.4089(2) 0.90185(11) 0.34559(11) 0.0563(6) Uani 1 1 d . . . . .
H43A H 0.429132 0.934827 0.325254 0.068 Uiso 1 1 calc R U . . .
H43B H 0.363665 0.880484 0.318854 0.068 Uiso 1 1 calc R U . . .
C44 C 0.3542(2) 0.91471(12) 0.39940(11) 0.0611(7) Uani 1 1 d . . . . .
H44A H 0.278508 0.918332 0.391137 0.073 Uiso 1 1 calc R U . . .
H44B H 0.380644 0.948430 0.416531 0.073 Uiso 1 1 calc R U . . .
C45 C 0.37613(15) 0.86850(8) 0.44066(9) 0.0354(4) Uani 1 1 d . . . . .
H45A H 0.388043 0.881137 0.481201 0.043 Uiso 1 1 calc R U . . .
H45B H 0.317961 0.842697 0.439640 0.043 Uiso 1 1 calc R U . . .
C46A C 0.8807(9) 0.4792(4) 0.2990(5) 0.048(2) Uani 0.50(2) 1 d D . P B 3
H46A H 0.846607 0.463172 0.263335 0.058 Uiso 0.50(2) 1 calc R U P B 3
Cl2A Cl 1.0066(4) 0.45228(17) 0.30820(18) 0.0664(12) Uani 0.50(2) 1 d D . P B 3
Cl3A Cl 0.8880(4) 0.54844(18) 0.28943(14) 0.0529(10) Uani 0.50(2) 1 d D . P B 3
Cl4A Cl 0.8035(4) 0.46538(19) 0.35960(18) 0.0710(13) Uani 0.50(2) 1 d D . P B 3
C46B C 0.8520(13) 0.4735(5) 0.2981(6) 0.068(4) Uani 0.50(2) 1 d D . P B 4
H46B H 0.822122 0.458231 0.260933 0.082 Uiso 0.50(2) 1 calc R U P B 4
Cl2B Cl 0.9719(14) 0.4441(4) 0.3138(4) 0.122(3) Uani 0.50(2) 1 d D . P B 4
Cl3B Cl 0.8656(9) 0.5416(3) 0.2903(2) 0.0961(18) Uani 0.50(2) 1 d D . P B 4
Cl4B Cl 0.7694(14) 0.4588(3) 0.3551(3) 0.127(2) Uani 0.50(2) 1 d D . P B 4
C47 C 0.6049(2) 0.53311(10) 0.17902(11) 0.0563(6) Uani 1 1 d . . . . .
H47 H 0.634890 0.496853 0.173213 0.068 Uiso 1 1 calc R U . C 5
Cl5A Cl 0.6912(7) 0.5795(3) 0.1458(3) 0.0905(16) Uani 0.59(3) 1 d . . P D 5
Cl6A Cl 0.5973(7) 0.5425(5) 0.2545(3) 0.099(2) Uani 0.59(3) 1 d . . P D 5
Cl7A Cl 0.4734(5) 0.53206(16) 0.1464(3) 0.0801(11) Uani 0.59(3) 1 d . . P D 5
Cl5B Cl 0.6722(9) 0.5861(4) 0.1542(5) 0.0750(19) Uani 0.41(3) 1 d . . P D 6
Cl6B Cl 0.5822(14) 0.5483(8) 0.2505(6) 0.110(3) Uani 0.41(3) 1 d . . P D 6
Cl7B Cl 0.5000(16) 0.5316(3) 0.1392(6) 0.115(3) Uani 0.41(3) 1 d . . P D 6
C48 C 0.7094(2) 0.95331(10) 0.46439(11) 0.0529(6) Uani 1 1 d . . . . .
H48 H 0.724060 0.937124 0.425688 0.063 Uiso 1 1 calc R U . . .
Cl8 Cl 0.82371(8) 0.98000(4) 0.49357(7) 0.1150(4) Uani 1 1 d . . . . .
Cl9 Cl 0.61769(8) 1.00394(4) 0.45379(4) 0.0884(3) Uani 1 1 d . . . . .
Cl10 Cl 0.66285(9) 0.90380(3) 0.50978(4) 0.0869(3) Uani 1 1 d . . . . .
C49 C 0.6606(2) 0.57114(9) 0.53252(12) 0.0549(6) Uani 1 1 d . . . . .
H49 H 0.661549 0.610903 0.531024 0.066 Uiso 1 1 calc R U . . .
Cl11 Cl 0.67052(8) 0.54658(3) 0.46171(4) 0.0807(2) Uani 1 1 d . . . . .
Cl12 Cl 0.54391(6) 0.55069(3) 0.56172(4) 0.06755(18) Uani 1 1 d . . . . .
Cl13 Cl 0.76624(6) 0.54951(3) 0.57632(4) 0.0806(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 O13 1.8135(12) . ?
Al1 O1 1.8831(12) . ?
Al1 O12 1.8835(13) . ?
Al1 O3 1.8940(13) . ?
Al1 O10 1.8954(13) . ?
Al1 N1 2.1175(14) . ?
Al2 O13 1.8165(12) . ?
Al2 O7 1.8798(13) . ?
Al2 O5 1.8895(13) . ?
Al2 O2 1.8960(13) . ?
Al2 O4 1.8965(13) . ?
Al2 N2 2.1301(14) . ?
Al3 O13 1.8220(11) . ?
Al3 O8 1.8802(13) . ?
Al3 O11 1.8851(13) . ?
Al3 O9 1.8919(13) . ?
Al3 O6 1.8932(13) . ?
Al3 N3 2.1275(14) . ?
O1 C1 1.265(2) . ?
O2 C1 1.2692(19) . ?
O3 C2 1.270(2) . ?
O4 C2 1.267(2) . ?
O5 C3 1.272(2) . ?
O6 C3 1.272(2) . ?
O7 C4 1.2726(19) . ?
O8 C4 1.2645(19) . ?
O9 C5 1.268(2) . ?
O10 C5 1.273(2) . ?
O11 C6 1.271(2) . ?
O12 C6 1.266(2) . ?
N1 C11 1.341(2) . ?
N1 C7 1.344(2) . ?
N2 C16 1.340(2) . ?
N2 C12 1.346(2) . ?
N3 C21 1.340(2) . ?
N3 C17 1.346(2) . ?
N4 C1 1.340(2) . ?
N4 C25 1.461(2) . ?
N4 C22 1.462(2) . ?
N5 C2 1.338(2) . ?
N5 C26 1.463(2) . ?
N5 C29 1.463(3) . ?
N6 C3 1.338(2) . ?
N6 C30 1.461(2) . ?
N6 C33 1.463(2) . ?
N7 C4 1.336(2) . ?
N7 C34 1.461(2) . ?
N7 C37 1.464(2) . ?
N8 C5 1.339(2) . ?
N8 C41 1.460(2) . ?
N8 C38 1.460(2) . ?
N9 C6 1.338(2) . ?
N9 C42 1.461(2) . ?
N9 C45 1.462(2) . ?
C7 C8 1.381(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.373(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(2) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.384(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.375(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.384(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.382(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.382(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.388(2) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.510(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.472(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.513(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.517(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.500(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.525(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.521(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.515(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.524(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35B 1.480(7) . ?
C34 C35A 1.569(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 H34C 0.9900 . ?
C34 H34D 0.9900 . ?
C35A C36A 1.554(13) . ?
C35A H35A 0.9900 . ?
C35A H35B 0.9900 . ?
C36A C37 1.523(13) . ?
C36A H36A 0.9900 . ?
C36A H36B 0.9900 . ?
C35B C36B 1.48(3) . ?
C35B H35C 0.9900 . ?
C35B H35D 0.9900 . ?
C36B C37 1.52(2) . ?
C36B H36C 0.9900 . ?
C36B H36D 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 H37C 0.9900 . ?
C37 H37D 0.9900 . ?
C38 C39 1.523(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.518(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.521(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.499(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.476(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.519(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46A Cl3A 1.756(9) . ?
C46A Cl2A 1.763(10) . ?
C46A Cl4A 1.769(9) . ?
C46A H46A 1.0000 . ?
C46B Cl3B 1.729(10) . ?
C46B Cl2B 1.738(11) . ?
C46B Cl4B 1.752(11) . ?
C46B H46B 1.0000 . ?
C47 Cl7B 1.606(13) . ?
C47 Cl5B 1.696(8) . ?
C47 Cl6B 1.716(13) . ?
C47 Cl6A 1.754(8) . ?
C47 Cl5A 1.796(6) . ?
C47 Cl7A 1.828(7) . ?
C47 H47 1.0000 . ?
C48 Cl8 1.732(3) . ?
C48 Cl10 1.741(3) . ?
C48 Cl9 1.747(3) . ?
C48 H48 1.0000 . ?
C49 Cl12 1.741(3) . ?
C49 Cl11 1.746(3) . ?
C49 Cl13 1.751(3) . ?
C49 H49 1.0000 . ?

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
O13 Al1 O1 97.69(5) . . ?
O13 Al1 O12 97.43(5) . . ?
O1 Al1 O12 164.87(6) . . ?
O13 Al1 O3 96.69(5) . . ?
O1 Al1 O3 90.97(6) . . ?
O12 Al1 O3 86.46(6) . . ?
O13 Al1 O10 95.75(5) . . ?
O1 Al1 O10 88.70(6) . . ?
O12 Al1 O10 90.61(6) . . ?
O3 Al1 O10 167.49(6) . . ?
O13 Al1 N1 179.39(6) . . ?
O1 Al1 N1 81.85(5) . . ?
O12 Al1 N1 83.05(5) . . ?
O3 Al1 N1 83.72(6) . . ?
O10 Al1 N1 83.85(6) . . ?
O13 Al2 O7 97.37(5) . . ?
O13 Al2 O5 97.55(5) . . ?
O7 Al2 O5 90.80(6) . . ?
O13 Al2 O2 96.35(5) . . ?
O7 Al2 O2 166.29(6) . . ?
O5 Al2 O2 87.44(6) . . ?
O13 Al2 O4 96.39(5) . . ?
O7 Al2 O4 87.57(6) . . ?
O5 Al2 O4 166.06(6) . . ?
O2 Al2 O4 90.87(6) . . ?
O13 Al2 N2 178.03(6) . . ?
O7 Al2 N2 83.41(6) . . ?
O5 Al2 N2 84.24(5) . . ?
O2 Al2 N2 82.88(5) . . ?
O4 Al2 N2 81.81(5) . . ?
O13 Al3 O8 96.69(5) . . ?
O13 Al3 O11 97.13(5) . . ?
O8 Al3 O11 88.87(6) . . ?
O13 Al3 O9 97.67(5) . . ?
O8 Al3 O9 165.64(6) . . ?
O11 Al3 O9 89.29(6) . . ?
O13 Al3 O6 95.10(5) . . ?
O8 Al3 O6 90.89(6) . . ?
O11 Al3 O6 167.72(6) . . ?
O9 Al3 O6 87.90(6) . . ?
O13 Al3 N3 177.58(6) . . ?
O8 Al3 N3 81.14(5) . . ?
O11 Al3 N3 83.95(5) . . ?
O9 Al3 N3 84.51(5) . . ?
O6 Al3 N3 83.89(5) . . ?
C1 O1 Al1 132.80(11) . . ?
C1 O2 Al2 127.81(11) . . ?
C2 O3 Al1 127.90(11) . . ?
C2 O4 Al2 131.79(11) . . ?
C3 O5 Al2 131.55(11) . . ?
C3 O6 Al3 129.51(11) . . ?
C4 O7 Al2 128.12(11) . . ?
C4 O8 Al3 133.89(11) . . ?
C5 O9 Al3 131.93(11) . . ?
C5 O10 Al1 127.49(11) . . ?
C6 O11 Al3 128.52(11) . . ?
C6 O12 Al1 132.42(11) . . ?
Al1 O13 Al2 119.95(6) . . ?
Al1 O13 Al3 119.93(6) . . ?
Al2 O13 Al3 120.11(6) . . ?
C11 N1 C7 117.68(15) . . ?
C11 N1 Al1 121.05(12) . . ?
C7 N1 Al1 121.26(12) . . ?
C16 N2 C12 117.99(15) . . ?
C16 N2 Al2 121.63(12) . . ?
C12 N2 Al2 120.16(12) . . ?
C21 N3 C17 117.83(14) . . ?
C21 N3 Al3 122.36(12) . . ?
C17 N3 Al3 119.65(11) . . ?
C1 N4 C25 123.88(15) . . ?
C1 N4 C22 123.36(15) . . ?
C25 N4 C22 112.47(14) . . ?
C2 N5 C26 123.51(16) . . ?
C2 N5 C29 123.31(16) . . ?
C26 N5 C29 112.77(16) . . ?
C3 N6 C30 123.92(15) . . ?
C3 N6 C33 123.16(14) . . ?
C30 N6 C33 112.77(14) . . ?
C4 N7 C34 122.89(14) . . ?
C4 N7 C37 123.59(14) . . ?
C34 N7 C37 112.71(14) . . ?
C5 N8 C41 124.55(15) . . ?
C5 N8 C38 122.35(15) . . ?
C41 N8 C38 112.84(15) . . ?
C6 N9 C42 123.70(15) . . ?
C6 N9 C45 123.59(14) . . ?
C42 N9 C45 112.68(14) . . ?
O1 C1 O2 124.90(14) . . ?
O1 C1 N4 117.28(14) . . ?
O2 C1 N4 117.81(14) . . ?
O4 C2 O3 124.77(15) . . ?
O4 C2 N5 117.87(15) . . ?
O3 C2 N5 117.35(15) . . ?
O5 C3 O6 125.01(15) . . ?
O5 C3 N6 117.80(14) . . ?
O6 C3 N6 117.19(14) . . ?
O8 C4 O7 124.76(15) . . ?
O8 C4 N7 117.76(14) . . ?
O7 C4 N7 117.48(14) . . ?
O9 C5 O10 125.13(15) . . ?
O9 C5 N8 117.14(15) . . ?
O10 C5 N8 117.73(15) . . ?
O12 C6 O11 125.16(15) . . ?
O12 C6 N9 117.18(15) . . ?
O11 C6 N9 117.65(15) . . ?
N1 C7 C8 122.65(18) . . ?
N1 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C9 C8 C7 118.96(19) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C10 C9 C8 118.86(17) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C9 C10 C11 119.28(19) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
N1 C11 C10 122.54(18) . . ?
N1 C11 H11 118.7 . . ?
C10 C11 H11 118.7 . . ?
N2 C12 C13 122.53(18) . . ?
N2 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
C14 C13 C12 118.94(19) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C15 C14 C13 118.95(17) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 119.07(19) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
N2 C16 C15 122.45(18) . . ?
N2 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
N3 C17 C18 122.84(17) . . ?
N3 C17 H17 118.6 . . ?
C18 C17 H17 118.6 . . ?
C19 C18 C17 118.83(18) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C20 C19 C18 118.84(17) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C19 C20 C21 118.98(18) . . ?
C19 C20 H20 120.5 . . ?
C21 C20 H20 120.5 . . ?
N3 C21 C20 122.66(18) . . ?
N3 C21 H21 118.7 . . ?
C20 C21 H21 118.7 . . ?
N4 C22 C23 102.85(17) . . ?
N4 C22 H22A 111.2 . . ?
C23 C22 H22A 111.2 . . ?
N4 C22 H22B 111.2 . . ?
C23 C22 H22B 111.2 . . ?
H22A C22 H22B 109.1 . . ?
C24 C23 C22 104.9(2) . . ?
C24 C23 H23A 110.8 . . ?
C22 C23 H23A 110.8 . . ?
C24 C23 H23B 110.8 . . ?
C22 C23 H23B 110.8 . . ?
H23A C23 H23B 108.8 . . ?
C23 C24 C25 105.6(2) . . ?
C23 C24 H24A 110.6 . . ?
C25 C24 H24A 110.6 . . ?
C23 C24 H24B 110.6 . . ?
C25 C24 H24B 110.6 . . ?
H24A C24 H24B 108.8 . . ?
N4 C25 C24 102.69(16) . . ?
N4 C25 H25A 111.2 . . ?
C24 C25 H25A 111.2 . . ?
N4 C25 H25B 111.2 . . ?
C24 C25 H25B 111.2 . . ?
H25A C25 H25B 109.1 . . ?
N5 C26 C27 102.41(19) . . ?
N5 C26 H26A 111.3 . . ?
C27 C26 H26A 111.3 . . ?
N5 C26 H26B 111.3 . . ?
C27 C26 H26B 111.3 . . ?
H26A C26 H26B 109.2 . . ?
C28 C27 C26 104.1(2) . . ?
C28 C27 H27A 110.9 . . ?
C26 C27 H27A 110.9 . . ?
C28 C27 H27B 110.9 . . ?
C26 C27 H27B 110.9 . . ?
H27A C27 H27B 109.0 . . ?
C27 C28 C29 103.9(2) . . ?
C27 C28 H28A 111.0 . . ?
C29 C28 H28A 111.0 . . ?
C27 C28 H28B 111.0 . . ?
C29 C28 H28B 111.0 . . ?
H28A C28 H28B 109.0 . . ?
N5 C29 C28 102.62(19) . . ?
N5 C29 H29A 111.2 . . ?
C28 C29 H29A 111.2 . . ?
N5 C29 H29B 111.2 . . ?
C28 C29 H29B 111.2 . . ?
H29A C29 H29B 109.2 . . ?
N6 C30 C31 102.97(16) . . ?
N6 C30 H30A 111.2 . . ?
C31 C30 H30A 111.2 . . ?
N6 C30 H30B 111.2 . . ?
C31 C30 H30B 111.2 . . ?
H30A C30 H30B 109.1 . . ?
C32 C31 C30 103.59(17) . . ?
C32 C31 H31A 111.0 . . ?
C30 C31 H31A 111.0 . . ?
C32 C31 H31B 111.0 . . ?
C30 C31 H31B 111.0 . . ?
H31A C31 H31B 109.0 . . ?
C31 C32 C33 103.91(17) . . ?
C31 C32 H32A 111.0 . . ?
C33 C32 H32A 111.0 . . ?
C31 C32 H32B 111.0 . . ?
C33 C32 H32B 111.0 . . ?
H32A C32 H32B 109.0 . . ?
N6 C33 C32 102.87(15) . . ?
N6 C33 H33A 111.2 . . ?
C32 C33 H33A 111.2 . . ?
N6 C33 H33B 111.2 . . ?
C32 C33 H33B 111.2 . . ?
H33A C33 H33B 109.1 . . ?
N7 C34 C35B 103.1(3) . . ?
N7 C34 C35A 101.85(19) . . ?
N7 C34 H34A 111.4 . . ?
C35A C34 H34A 111.4 . . ?
N7 C34 H34B 111.4 . . ?
C35A C34 H34B 111.4 . . ?
H34A C34 H34B 109.3 . . ?
N7 C34 H34C 111.1 . . ?
C35B C34 H34C 111.1 . . ?
N7 C34 H34D 111.1 . . ?
C35B C34 H34D 111.1 . . ?
H34C C34 H34D 109.1 . . ?
C36A C35A C34 100.2(6) . . ?
C36A C35A H35A 111.7 . . ?
C34 C35A H35A 111.7 . . ?
C36A C35A H35B 111.7 . . ?
C34 C35A H35B 111.7 . . ?
H35A C35A H35B 109.5 . . ?
C37 C36A C35A 103.6(7) . . ?
C37 C36A H36A 111.0 . . ?
C35A C36A H36A 111.0 . . ?
C37 C36A H36B 111.0 . . ?
C35A C36A H36B 111.0 . . ?
H36A C36A H36B 109.0 . . ?
C34 C35B C36B 105.4(10) . . ?
C34 C35B H35C 110.7 . . ?
C36B C35B H35C 110.7 . . ?
C34 C35B H35D 110.7 . . ?
C36B C35B H35D 110.7 . . ?
H35C C35B H35D 108.8 . . ?
C35B C36B C37 104.3(14) . . ?
C35B C36B H36C 110.9 . . ?
C37 C36B H36C 110.9 . . ?
C35B C36B H36D 110.9 . . ?
C37 C36B H36D 110.9 . . ?
H36C C36B H36D 108.9 . . ?
N7 C37 C36B 101.6(10) . . ?
N7 C37 C36A 103.7(5) . . ?
N7 C37 H37A 111.0 . . ?
C36A C37 H37A 111.0 . . ?
N7 C37 H37B 111.0 . . ?
C36A C37 H37B 111.0 . . ?
H37A C37 H37B 109.0 . . ?
N7 C37 H37C 111.5 . . ?
C36B C37 H37C 111.5 . . ?
N7 C37 H37D 111.5 . . ?
C36B C37 H37D 111.5 . . ?
H37C C37 H37D 109.3 . . ?
N8 C38 C39 103.35(16) . . ?
N8 C38 H38A 111.1 . . ?
C39 C38 H38A 111.1 . . ?
N8 C38 H38B 111.1 . . ?
C39 C38 H38B 111.1 . . ?
H38A C38 H38B 109.1 . . ?
C40 C39 C38 103.90(17) . . ?
C40 C39 H39A 111.0 . . ?
C38 C39 H39A 111.0 . . ?
C40 C39 H39B 111.0 . . ?
C38 C39 H39B 111.0 . . ?
H39A C39 H39B 109.0 . . ?
C39 C40 C41 103.77(17) . . ?
C39 C40 H40A 111.0 . . ?
C41 C40 H40A 111.0 . . ?
C39 C40 H40B 111.0 . . ?
C41 C40 H40B 111.0 . . ?
H40A C40 H40B 109.0 . . ?
N8 C41 C40 102.78(16) . . ?
N8 C41 H41A 111.2 . . ?
C40 C41 H41A 111.2 . . ?
N8 C41 H41B 111.2 . . ?
C40 C41 H41B 111.2 . . ?
H41A C41 H41B 109.1 . . ?
N9 C42 C43 102.69(17) . . ?
N9 C42 H42A 111.2 . . ?
C43 C42 H42A 111.2 . . ?
N9 C42 H42B 111.2 . . ?
C43 C42 H42B 111.2 . . ?
H42A C42 H42B 109.1 . . ?
C44 C43 C42 106.09(19) . . ?
C44 C43 H43A 110.5 . . ?
C42 C43 H43A 110.5 . . ?
C44 C43 H43B 110.5 . . ?
C42 C43 H43B 110.5 . . ?
H43A C43 H43B 108.7 . . ?
C43 C44 C45 105.63(19) . . ?
C43 C44 H44A 110.6 . . ?
C45 C44 H44A 110.6 . . ?
C43 C44 H44B 110.6 . . ?
C45 C44 H44B 110.6 . . ?
H44A C44 H44B 108.7 . . ?
N9 C45 C44 103.20(16) . . ?
N9 C45 H45A 111.1 . . ?
C44 C45 H45A 111.1 . . ?
N9 C45 H45B 111.1 . . ?
C44 C45 H45B 111.1 . . ?
H45A C45 H45B 109.1 . . ?
Cl3A C46A Cl2A 110.0(6) . . ?
Cl3A C46A Cl4A 109.0(6) . . ?
Cl2A C46A Cl4A 111.5(6) . . ?
Cl3A C46A H46A 108.7 . . ?
Cl2A C46A H46A 108.7 . . ?
Cl4A C46A H46A 108.7 . . ?
Cl3B C46B Cl2B 110.5(7) . . ?
Cl3B C46B Cl4B 110.6(7) . . ?
Cl2B C46B Cl4B 108.1(7) . . ?
Cl3B C46B H46B 109.2 . . ?
Cl2B C46B H46B 109.2 . . ?
Cl4B C46B H46B 109.2 . . ?
Cl7B C47 Cl5B 104.8(5) . . ?
Cl7B C47 Cl6B 112.5(6) . . ?
Cl5B C47 Cl6B 104.5(8) . . ?
Cl6A C47 Cl5A 112.7(5) . . ?
Cl6A C47 Cl7A 109.1(4) . . ?
Cl5A C47 Cl7A 114.3(4) . . ?
Cl6A C47 H47 106.8 . . ?
Cl5A C47 H47 106.8 . . ?
Cl7A C47 H47 106.8 . . ?
Cl8 C48 Cl10 110.47(15) . . ?
Cl8 C48 Cl9 109.48(14) . . ?
Cl10 C48 Cl9 111.12(15) . . ?
Cl8 C48 H48 108.6 . . ?
Cl10 C48 H48 108.6 . . ?
Cl9 C48 H48 108.6 . . ?
Cl12 C49 Cl11 110.06(15) . . ?
Cl12 C49 Cl13 110.55(15) . . ?
Cl11 C49 Cl13 110.23(15) . . ?
Cl12 C49 H49 108.7 . . ?
Cl11 C49 H49 108.7 . . ?
Cl13 C49 H49 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O13 Al1 O1 C1 11.21(17) . . . . ?
O12 Al1 O1 C1 -165.6(2) . . . . ?
O3 Al1 O1 C1 -85.68(16) . . . . ?
O10 Al1 O1 C1 106.83(16) . . . . ?
N1 Al1 O1 C1 -169.20(17) . . . . ?
O13 Al2 O2 C1 -39.36(15) . . . . ?
O7 Al2 O2 C1 140.5(2) . . . . ?
O5 Al2 O2 C1 -136.67(14) . . . . ?
O4 Al2 O2 C1 57.17(14) . . . . ?
N2 Al2 O2 C1 138.81(15) . . . . ?
O13 Al1 O3 C2 -28.47(16) . . . . ?
O1 Al1 O3 C2 69.38(15) . . . . ?
O12 Al1 O3 C2 -125.54(15) . . . . ?
O10 Al1 O3 C2 157.8(2) . . . . ?
N1 Al1 O3 C2 151.07(15) . . . . ?
O13 Al2 O4 C2 0.56(16) . . . . ?
O7 Al2 O4 C2 97.70(16) . . . . ?
O5 Al2 O4 C2 -178.8(2) . . . . ?
O2 Al2 O4 C2 -95.93(16) . . . . ?
N2 Al2 O4 C2 -178.61(16) . . . . ?
O13 Al2 O5 C3 10.28(16) . . . . ?
O7 Al2 O5 C3 -87.26(16) . . . . ?
O2 Al2 O5 C3 106.35(16) . . . . ?
O4 Al2 O5 C3 -170.4(2) . . . . ?
N2 Al2 O5 C3 -170.55(16) . . . . ?
O13 Al3 O6 C3 -36.73(15) . . . . ?
O8 Al3 O6 C3 60.07(15) . . . . ?
O11 Al3 O6 C3 148.9(3) . . . . ?
O9 Al3 O6 C3 -134.24(15) . . . . ?
N3 Al3 O6 C3 141.06(15) . . . . ?
O13 Al2 O7 C4 -34.41(15) . . . . ?
O5 Al2 O7 C4 63.30(15) . . . . ?
O2 Al2 O7 C4 145.8(2) . . . . ?
O4 Al2 O7 C4 -130.55(15) . . . . ?
N2 Al2 O7 C4 147.41(15) . . . . ?
O13 Al3 O8 C4 9.90(17) . . . . ?
O11 Al3 O8 C4 106.95(16) . . . . ?
O9 Al3 O8 C4 -170.3(2) . . . . ?
O6 Al3 O8 C4 -85.33(16) . . . . ?
N3 Al3 O8 C4 -169.00(17) . . . . ?
O13 Al3 O9 C5 12.86(17) . . . . ?
O8 Al3 O9 C5 -166.9(2) . . . . ?
O11 Al3 O9 C5 -84.24(16) . . . . ?
O6 Al3 O9 C5 107.72(16) . . . . ?
N3 Al3 O9 C5 -168.22(17) . . . . ?
O13 Al1 O10 C5 -42.48(15) . . . . ?
O1 Al1 O10 C5 -140.07(14) . . . . ?
O12 Al1 O10 C5 55.05(15) . . . . ?
O3 Al1 O10 C5 131.3(3) . . . . ?
N1 Al1 O10 C5 137.99(15) . . . . ?
O13 Al3 O11 C6 -30.79(16) . . . . ?
O8 Al3 O11 C6 -127.40(15) . . . . ?
O9 Al3 O11 C6 66.85(15) . . . . ?
O6 Al3 O11 C6 143.6(3) . . . . ?
N3 Al3 O11 C6 151.40(15) . . . . ?
O13 Al1 O12 C6 5.43(17) . . . . ?
O1 Al1 O12 C6 -177.7(2) . . . . ?
O3 Al1 O12 C6 101.73(17) . . . . ?
O10 Al1 O12 C6 -90.44(17) . . . . ?
N1 Al1 O12 C6 -174.17(17) . . . . ?
O1 Al1 O13 Al2 -40.22(8) . . . . ?
O12 Al1 O13 Al2 138.95(7) . . . . ?
O3 Al1 O13 Al2 51.67(8) . . . . ?
O10 Al1 O13 Al2 -129.68(7) . . . . ?
O1 Al1 O13 Al3 140.67(7) . . . . ?
O12 Al1 O13 Al3 -40.16(8) . . . . ?
O3 Al1 O13 Al3 -127.44(7) . . . . ?
O10 Al1 O13 Al3 51.21(8) . . . . ?
O7 Al2 O13 Al1 -129.88(7) . . . . ?
O5 Al2 O13 Al1 138.33(7) . . . . ?
O2 Al2 O13 Al1 50.08(8) . . . . ?
O4 Al2 O13 Al1 -41.51(8) . . . . ?
O7 Al2 O13 Al3 49.24(8) . . . . ?
O5 Al2 O13 Al3 -42.56(8) . . . . ?
O2 Al2 O13 Al3 -130.81(7) . . . . ?
O4 Al2 O13 Al3 137.60(7) . . . . ?
O8 Al3 O13 Al1 138.97(7) . . . . ?
O11 Al3 O13 Al1 49.27(8) . . . . ?
O9 Al3 O13 Al1 -40.97(8) . . . . ?
O6 Al3 O13 Al1 -129.53(7) . . . . ?
O8 Al3 O13 Al2 -40.14(8) . . . . ?
O11 Al3 O13 Al2 -129.84(7) . . . . ?
O9 Al3 O13 Al2 139.92(7) . . . . ?
O6 Al3 O13 Al2 51.36(8) . . . . ?
Al1 O1 C1 O2 -0.1(3) . . . . ?
Al1 O1 C1 N4 -179.15(13) . . . . ?
Al2 O2 C1 O1 17.3(2) . . . . ?
Al2 O2 C1 N4 -163.62(13) . . . . ?
C25 N4 C1 O1 -177.86(18) . . . . ?
C22 N4 C1 O1 -4.4(3) . . . . ?
C25 N4 C1 O2 3.0(3) . . . . ?
C22 N4 C1 O2 176.50(18) . . . . ?
Al2 O4 C2 O3 24.2(3) . . . . ?
Al2 O4 C2 N5 -156.87(13) . . . . ?
Al1 O3 C2 O4 -6.5(3) . . . . ?
Al1 O3 C2 N5 174.58(13) . . . . ?
C26 N5 C2 O4 177.33(18) . . . . ?
C29 N5 C2 O4 5.2(3) . . . . ?
C26 N5 C2 O3 -3.7(3) . . . . ?
C29 N5 C2 O3 -175.85(19) . . . . ?
Al2 O5 C3 O6 5.0(3) . . . . ?
Al2 O5 C3 N6 -174.82(13) . . . . ?
Al3 O6 C3 O5 11.6(3) . . . . ?
Al3 O6 C3 N6 -168.65(12) . . . . ?
C30 N6 C3 O5 -1.1(3) . . . . ?
C33 N6 C3 O5 -176.47(17) . . . . ?
C30 N6 C3 O6 179.12(18) . . . . ?
C33 N6 C3 O6 3.7(3) . . . . ?
Al3 O8 C4 O7 5.1(3) . . . . ?
Al3 O8 C4 N7 -175.63(12) . . . . ?
Al2 O7 C4 O8 10.1(3) . . . . ?
Al2 O7 C4 N7 -169.26(12) . . . . ?
C34 N7 C4 O8 -171.80(17) . . . . ?
C37 N7 C4 O8 -2.9(3) . . . . ?
C34 N7 C4 O7 7.6(3) . . . . ?
C37 N7 C4 O7 176.49(16) . . . . ?
Al3 O9 C5 O10 -4.0(3) . . . . ?
Al3 O9 C5 N8 176.73(13) . . . . ?
Al1 O10 C5 O9 22.0(3) . . . . ?
Al1 O10 C5 N8 -158.71(13) . . . . ?
C41 N8 C5 O9 -175.51(18) . . . . ?
C38 N8 C5 O9 -1.8(3) . . . . ?
C41 N8 C5 O10 5.2(3) . . . . ?
C38 N8 C5 O10 178.88(19) . . . . ?
Al1 O12 C6 O11 14.2(3) . . . . ?
Al1 O12 C6 N9 -167.00(13) . . . . ?
Al3 O11 C6 O12 1.7(3) . . . . ?
Al3 O11 C6 N9 -177.04(12) . . . . ?
C42 N9 C6 O12 -175.15(18) . . . . ?
C45 N9 C6 O12 7.1(3) . . . . ?
C42 N9 C6 O11 3.7(3) . . . . ?
C45 N9 C6 O11 -174.02(17) . . . . ?
C11 N1 C7 C8 0.4(3) . . . . ?
Al1 N1 C7 C8 -179.25(14) . . . . ?
N1 C7 C8 C9 0.7(3) . . . . ?
C7 C8 C9 C10 -1.6(3) . . . . ?
C8 C9 C10 C11 1.2(3) . . . . ?
C7 N1 C11 C10 -0.8(3) . . . . ?
Al1 N1 C11 C10 178.92(14) . . . . ?
C9 C10 C11 N1 -0.1(3) . . . . ?
C16 N2 C12 C13 -1.6(3) . . . . ?
Al2 N2 C12 C13 173.10(14) . . . . ?
N2 C12 C13 C14 -0.3(3) . . . . ?
C12 C13 C14 C15 2.6(3) . . . . ?
C13 C14 C15 C16 -3.0(3) . . . . ?
C12 N2 C16 C15 1.3(3) . . . . ?
Al2 N2 C16 C15 -173.38(14) . . . . ?
C14 C15 C16 N2 1.0(3) . . . . ?
C21 N3 C17 C18 -1.1(2) . . . . ?
Al3 N3 C17 C18 174.41(13) . . . . ?
N3 C17 C18 C19 -0.2(3) . . . . ?
C17 C18 C19 C20 1.4(3) . . . . ?
C18 C19 C20 C21 -1.4(3) . . . . ?
C17 N3 C21 C20 1.2(3) . . . . ?
Al3 N3 C21 C20 -174.22(14) . . . . ?
C19 C20 C21 N3 0.1(3) . . . . ?
C1 N4 C22 C23 -162.2(2) . . . . ?
C25 N4 C22 C23 12.0(3) . . . . ?
N4 C22 C23 C24 -28.4(3) . . . . ?
C22 C23 C24 C25 34.8(3) . . . . ?
C1 N4 C25 C24 -177.2(2) . . . . ?
C22 N4 C25 C24 8.7(3) . . . . ?
C23 C24 C25 N4 -26.6(3) . . . . ?
C2 N5 C26 C27 -159.5(2) . . . . ?
C29 N5 C26 C27 13.4(3) . . . . ?
N5 C26 C27 C28 -31.5(3) . . . . ?
C26 C27 C28 C29 38.3(3) . . . . ?
C2 N5 C29 C28 -177.3(2) . . . . ?
C26 N5 C29 C28 9.8(3) . . . . ?
C27 C28 C29 N5 -29.4(3) . . . . ?
C3 N6 C30 C31 -163.08(19) . . . . ?
C33 N6 C30 C31 12.7(2) . . . . ?
N6 C30 C31 C32 -30.8(3) . . . . ?
C30 C31 C32 C33 37.8(3) . . . . ?
C3 N6 C33 C32 -173.72(18) . . . . ?
C30 N6 C33 C32 10.4(2) . . . . ?
C31 C32 C33 N6 -29.5(2) . . . . ?
C4 N7 C34 C35B 179.7(6) . . . . ?
C37 N7 C34 C35B 9.7(7) . . . . ?
C4 N7 C34 C35A 148.2(3) . . . . ?
C37 N7 C34 C35A -21.8(3) . . . . ?
N7 C34 C35A C36A 37.7(7) . . . . ?
C34 C35A C36A C37 -41.2(9) . . . . ?
N7 C34 C35B C36B -28.5(12) . . . . ?
C34 C35B C36B C37 36.9(14) . . . . ?
C4 N7 C37 C36B -157.6(6) . . . . ?
C34 N7 C37 C36B 12.3(6) . . . . ?
C4 N7 C37 C36A -174.1(5) . . . . ?
C34 N7 C37 C36A -4.1(5) . . . . ?
C35B C36B C37 N7 -29.5(12) . . . . ?
C35A C36A C37 N7 28.8(8) . . . . ?
C5 N8 C38 C39 177.65(19) . . . . ?
C41 N8 C38 C39 -8.0(3) . . . . ?
N8 C38 C39 C40 27.5(3) . . . . ?
C38 C39 C40 C41 -36.9(3) . . . . ?
C5 N8 C41 C40 159.50(19) . . . . ?
C38 N8 C41 C40 -14.7(3) . . . . ?
C39 C40 C41 N8 31.4(2) . . . . ?
C6 N9 C42 C43 166.9(2) . . . . ?
C45 N9 C42 C43 -15.2(2) . . . . ?
N9 C42 C43 C44 28.5(3) . . . . ?
C42 C43 C44 C45 -31.7(3) . . . . ?
C6 N9 C45 C44 174.3(2) . . . . ?
C42 N9 C45 C44 -3.6(2) . . . . ?
C43 C44 C45 N9 21.5(3) . . . . ?

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
_geom_hbond_publ_flag
C10 H10 Cl5A^e 0.95 2.90 3.703(7) 142.8 4_576 yes
C10 H10 Cl5B^f 0.95 2.85 3.660(8) 143.9 4_576 yes
C17 H17 Cl1 0.95 2.88 3.6114(19) 134.4 2_655 yes
C27 H27B Cl3A^c 0.99 2.91 3.664(5) 133.2 4_576 yes
C30 H30A Cl13 0.99 2.95 3.690(2) 132.1 . yes
C33 H33B Cl11 0.99 2.96 3.778(2) 140.8 . yes
C35A^a H35A^a Cl8 0.99 2.94 3.779(6) 142.8 3_776 yes
C35B^b H35D^b Cl8 0.99 2.90 3.672(15) 135.5 . yes
C35B^b H35D^b Cl8 0.99 2.78 3.311(9) 113.8 3_776 yes
C37 H37A^a Cl1 0.99 2.86 3.832(2) 166.9 2_655 yes
C38 H38A Cl6A^e 0.99 2.84 3.482(10) 123.1 . yes
C38 H38A Cl6B^f 0.99 2.79 3.379(15) 118.4 . yes
C42 H42B Cl1 0.99 2.84 3.644(2) 138.6 2_655 yes
C46A^c H46A^c Cl1 1.00 2.44 3.441(13) 174.6 . yes
C46B^d H46B^d Cl1 1.00 2.21 3.208(16) 177.0 . yes
C47 H47^e Cl1 1.00 2.36 3.315(3) 160.6 . yes
C48 H48 Cl1 1.00 2.52 3.486(3) 163.4 2_655 yes

_refine_diff_density_max         0.696
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.049



