# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_17
_database_code_depnum_ccdc_archive 'CCDC 2151215'
loop_
_audit_author_name
_audit_author_address
'Ana Maria Rodriguez'
;Universidad de Castilla la Mancha
Spain
;
_audit_update_record             
;
2022-06-28 deposited with the CCDC.	2022-06-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H64 Al3 N5 O'
_chemical_formula_weight         663.86

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   20.2041(8)
_cell_length_b                   10.0613(7)
_cell_length_c                   20.8767(11)
_cell_angle_alpha                90
_cell_angle_beta                 115.022(3)
_cell_angle_gamma                90
_cell_volume                     3845.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4308
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      20.58

_exptl_crystal_description       prismatic
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_F_000             1448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.132
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5604
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9512
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.225
_diffrn_reflns_theta_max         20.882
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.582
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.582
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 0.549
_reflns_number_total             3824
_reflns_number_gt                3425
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_max     0.883
_reflns_Friedel_fraction_full    0.517

_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       'Bruker ApexII'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_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)+(0.0538P)²+0.5649P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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_abs_structure_details 
;
 Flack x determined using 1466 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3824
_refine_ls_number_parameters     417
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0972
_refine_ls_wR_factor_gt          0.0932
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Al1 Al 1.00095(10) 0.87333(19) 0.97985(9) 0.0226(5) Uani 1 1 d . . . . .
Al2 Al 0.70630(10) 0.80779(18) 0.84615(9) 0.0214(5) Uani 1 1 d . . . . .
Al3 Al 0.78683(10) 1.10327(18) 0.84743(9) 0.0226(5) Uani 1 1 d . . . . .
C1 C 0.8551(4) 0.8421(6) 0.9083(3) 0.0159(15) Uani 1 1 d . . . . .
C2 C 0.8564(3) 0.7714(6) 0.9642(3) 0.0185(16) Uani 1 1 d . . . . .
C3 C 0.8322(4) 0.4835(7) 0.9963(4) 0.0359(19) Uani 1 1 d . . . . .
H3A H 0.8135 0.5107 1.0296 0.054 Uiso 1 1 calc R U . . .
H3B H 0.8372 0.3885 0.9976 0.054 Uiso 1 1 calc R U . . .
H3C H 0.7990 0.5108 0.9496 0.054 Uiso 1 1 calc R U . . .
C4 C 0.9039(4) 0.5454(6) 1.0149(3) 0.0241(17) Uani 1 1 d . . . . .
C5 C 0.9729(4) 0.4962(7) 1.0488(4) 0.0312(18) Uani 1 1 d . . . . .
H5 H 0.9854 0.4108 1.0669 0.037 Uiso 1 1 calc R U . . .
C6 C 1.0214(4) 0.5974(7) 1.0515(3) 0.0304(18) Uani 1 1 d . . . . .
C7 C 1.1028(4) 0.5933(8) 1.0817(4) 0.049(2) Uani 1 1 d . . . . .
H7A H 1.1183 0.6019 1.0443 0.073 Uiso 1 1 calc R U . . .
H7B H 1.1200 0.5103 1.1057 0.073 Uiso 1 1 calc R U . . .
H7C H 1.1226 0.6653 1.1146 0.073 Uiso 1 1 calc R U . . .
C8 C 0.8846(4) 0.7889(7) 1.1208(3) 0.0332(19) Uani 1 1 d . . . . .
H8A H 0.9074 0.7038 1.1246 0.050 Uiso 1 1 calc R U . . .
H8B H 0.8792 0.8071 1.1635 0.050 Uiso 1 1 calc R U . . .
H8C H 0.9145 0.8564 1.1137 0.050 Uiso 1 1 calc R U . . .
C9 C 0.8122(4) 0.7881(6) 1.0604(3) 0.0235(17) Uani 1 1 d . . . . .
C10 C 0.7430(4) 0.7888(7) 1.0578(4) 0.0309(18) Uani 1 1 d . . . . .
H10 H 0.7316 0.7904 1.0966 0.037 Uiso 1 1 calc R U . . .
C11 C 0.6933(4) 0.7868(6) 0.9877(4) 0.0302(18) Uani 1 1 d . . . . .
C12 C 0.6116(4) 0.7913(8) 0.9565(4) 0.046(2) Uani 1 1 d . . . . .
H12A H 0.5950 0.8761 0.9344 0.070 Uiso 1 1 calc R U . . .
H12B H 0.5954 0.7785 0.9931 0.070 Uiso 1 1 calc R U . . .
H12C H 0.5920 0.7222 0.9218 0.070 Uiso 1 1 calc R U . . .
C13 C 0.9968(4) 1.0132(7) 1.0433(3) 0.0306(18) Uani 1 1 d . . . . .
H13A H 1.0070 1.0980 1.0274 0.037 Uiso 1 1 calc R U . . .
H13B H 0.9476 1.0172 1.0404 0.037 Uiso 1 1 calc R U . . .
C14 C 1.0503(4) 0.9922(8) 1.1201(4) 0.044(2) Uani 1 1 d . . . . .
H14A H 1.0385 0.9113 1.1374 0.066 Uiso 1 1 calc R U . . .
H14B H 1.0472 1.0656 1.1481 0.066 Uiso 1 1 calc R U . . .
H14C H 1.0991 0.9863 1.1234 0.066 Uiso 1 1 calc R U . . .
C15 C 1.0957(4) 0.8637(8) 0.9729(4) 0.040(2) Uani 1 1 d . . . . .
H15A H 1.1063 0.7709 0.9686 0.048 Uiso 1 1 calc R U . . .
H15B H 1.0902 0.9078 0.9296 0.048 Uiso 1 1 calc R U . . .
C16 C 1.1608(4) 0.9233(8) 1.0331(5) 0.058(2) Uani 1 1 d . . . . .
H16A H 1.1510 1.0147 1.0390 0.086 Uiso 1 1 calc R U . . .
H16B H 1.2028 0.9179 1.0229 0.086 Uiso 1 1 calc R U . . .
H16C H 1.1701 0.8753 1.0758 0.086 Uiso 1 1 calc R U . . .
C17 C 0.7059(4) 0.6285(6) 0.8092(4) 0.0272(17) Uani 1 1 d . . . . .
H17A H 0.6925 0.6332 0.7589 0.033 Uiso 1 1 calc R U . . .
H17B H 0.7544 0.5905 0.8321 0.033 Uiso 1 1 calc R U . . .
C18 C 0.6509(4) 0.5385(7) 0.8228(4) 0.0358(19) Uani 1 1 d . . . . .
H18A H 0.6658 0.5296 0.8728 0.054 Uiso 1 1 calc R U . . .
H18B H 0.6497 0.4524 0.8025 0.054 Uiso 1 1 calc R U . . .
H18C H 0.6031 0.5777 0.8015 0.054 Uiso 1 1 calc R U . . .
C19 C 0.6182(4) 0.9132(7) 0.7971(3) 0.0293(18) Uani 1 1 d . . . . .
H19A H 0.6049 0.9533 0.8323 0.035 Uiso 1 1 calc R U . . .
H19B H 0.6297 0.9849 0.7724 0.035 Uiso 1 1 calc R U . . .
C20 C 0.5522(5) 0.8399(8) 0.7444(4) 0.058(3) Uani 1 1 d . . . . .
H20A H 0.5667 0.7843 0.7152 0.087 Uiso 1 1 calc R U . . .
H20B H 0.5165 0.9030 0.7153 0.087 Uiso 1 1 calc R U . . .
H20C H 0.5315 0.7860 0.7693 0.087 Uiso 1 1 calc R U . . .
C21 C 0.7299(4) 1.1741(6) 0.8979(3) 0.0281(18) Uani 1 1 d . . . . .
H21A H 0.7287 1.2703 0.8944 0.034 Uiso 1 1 calc R U . . .
H21B H 0.6800 1.1426 0.8739 0.034 Uiso 1 1 calc R U . . .
C22 C 0.7591(4) 1.1361(7) 0.9755(4) 0.0360(19) Uani 1 1 d . . . . .
H22A H 0.7499 1.0435 0.9795 0.054 Uiso 1 1 calc R U . . .
H22B H 0.7351 1.1883 0.9979 0.054 Uiso 1 1 calc R U . . .
H22C H 0.8107 1.1524 0.9982 0.054 Uiso 1 1 calc R U . . .
C23 C 0.7386(4) 1.1141(7) 0.7423(3) 0.0336(19) Uani 1 1 d . . . . .
H23A H 0.7760 1.1242 0.7250 0.040 Uiso 1 1 calc R U . . .
H23B H 0.7134 1.0311 0.7239 0.040 Uiso 1 1 calc R U . . .
C24 C 0.6837(4) 1.2292(8) 0.7134(4) 0.044(2) Uani 1 1 d . . . . .
H24A H 0.6481 1.2233 0.7324 0.067 Uiso 1 1 calc R U . . .
H24B H 0.6596 1.2236 0.6628 0.067 Uiso 1 1 calc R U . . .
H24C H 0.7091 1.3124 0.7269 0.067 Uiso 1 1 calc R U . . .
C25 C 0.8848(4) 1.1877(6) 0.8888(4) 0.0317(19) Uani 1 1 d . . . . .
H25A H 0.8986 1.2065 0.9384 0.038 Uiso 1 1 calc R U . . .
H25B H 0.9204 1.1266 0.8857 0.038 Uiso 1 1 calc R U . . .
C26 C 0.8856(5) 1.3176(7) 0.8502(5) 0.053(2) Uani 1 1 d . . . . .
H26A H 0.8800 1.2975 0.8033 0.079 Uiso 1 1 calc R U . . .
H26B H 0.9312 1.3627 0.8756 0.079 Uiso 1 1 calc R U . . .
H26C H 0.8461 1.3735 0.8478 0.079 Uiso 1 1 calc R U . . .
C27 C 0.9109(3) 0.8165(6) 0.8233(3) 0.0207(16) Uani 1 1 d . . . . .
C28 C 0.8347(3) 0.7931(7) 0.7655(3) 0.0244(17) Uani 1 1 d . . . . .
H28A H 0.8062 0.8740 0.7578 0.029 Uiso 1 1 calc R U . . .
H28B H 0.8106 0.7243 0.7804 0.029 Uiso 1 1 calc R U . . .
C29 C 0.8378(4) 0.7511(7) 0.6960(3) 0.0315(18) Uani 1 1 d . . . . .
H29 H 0.7879 0.7362 0.6601 0.038 Uiso 1 1 calc R U . . .
C30 C 0.8728(4) 0.8602(8) 0.6713(4) 0.045(2) Uani 1 1 d . . . . .
H30A H 0.8438 0.9407 0.6623 0.054 Uiso 1 1 calc R U . . .
H30B H 0.8754 0.8338 0.6277 0.054 Uiso 1 1 calc R U . . .
C31 C 0.9495(4) 0.8857(8) 0.7286(4) 0.043(2) Uani 1 1 d . . . . .
H31 H 0.9726 0.9567 0.7130 0.051 Uiso 1 1 calc R U . . .
C32 C 0.9943(5) 0.7599(10) 0.7407(4) 0.058(3) Uani 1 1 d . . . . .
H32A H 1.0433 0.7755 0.7769 0.069 Uiso 1 1 calc R U . . .
H32B H 0.9980 0.7349 0.6975 0.069 Uiso 1 1 calc R U . . .
C33 C 0.9582(5) 0.6461(8) 0.7642(4) 0.048(2) Uani 1 1 d . . . . .
H33 H 0.9873 0.5649 0.7720 0.057 Uiso 1 1 calc R U . . .
C34 C 0.9545(4) 0.6878(7) 0.8327(4) 0.036(2) Uani 1 1 d . . . . .
H34A H 1.0037 0.7006 0.8690 0.043 Uiso 1 1 calc R U . . .
H34B H 0.9318 0.6175 0.8482 0.043 Uiso 1 1 calc R U . . .
C35 C 0.8814(4) 0.6221(7) 0.7074(4) 0.043(2) Uani 1 1 d . . . . .
H35A H 0.8580 0.5517 0.7221 0.052 Uiso 1 1 calc R U . . .
H35B H 0.8835 0.5952 0.6637 0.052 Uiso 1 1 calc R U . . .
C36 C 0.9456(4) 0.9275(7) 0.7969(3) 0.0299(18) Uani 1 1 d . . . . .
H36A H 0.9167 1.0079 0.7889 0.036 Uiso 1 1 calc R U . . .
H36B H 0.9943 0.9463 0.8326 0.036 Uiso 1 1 calc R U . . .
N1 N 0.9838(3) 0.7073(5) 1.0219(3) 0.0215(13) Uani 1 1 d . . . . .
N2 N 0.9112(3) 0.6741(5) 0.9989(3) 0.0207(14) Uani 1 1 d . . . . .
N3 N 0.8026(3) 0.7836(5) 0.9918(3) 0.0206(13) Uani 1 1 d . . . . .
N4 N 0.7300(3) 0.7813(5) 0.9464(3) 0.0222(13) Uani 1 1 d . . . . .
N5 N 0.9140(3) 0.8508(5) 0.8945(2) 0.0176(13) Uani 1 1 d . . . . .
O1 O 0.7906(2) 0.9090(4) 0.86773(19) 0.0170(10) 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 N5 1.914(5) . ?
Al1 C13 1.959(7) . ?
Al1 C15 1.983(7) . ?
Al1 N1 1.984(5) . ?
Al2 O1 1.868(4) . ?
Al2 C19 1.950(7) . ?
Al2 N4 1.958(5) . ?
Al2 C17 1.960(7) . ?
Al3 C25 1.984(7) . ?
Al3 C21 1.992(6) . ?
Al3 C23 1.992(7) . ?
Al3 O1 1.995(4) . ?
C1 N5 1.341(8) . ?
C1 C2 1.357(9) . ?
C1 O1 1.391(8) . ?
C2 N2 1.424(8) . ?
C2 N3 1.435(7) . ?
C3 C4 1.471(10) . ?
C4 C5 1.361(9) . ?
C4 N2 1.360(8) . ?
C5 C6 1.397(10) . ?
C6 N1 1.337(8) . ?
C6 C7 1.493(10) . ?
C8 C9 1.473(9) . ?
C9 N3 1.362(8) . ?
C9 C10 1.377(10) . ?
C10 C11 1.380(10) . ?
C11 N4 1.356(8) . ?
C11 C12 1.497(10) . ?
C13 C14 1.523(10) . ?
C15 C16 1.507(11) . ?
C17 C18 1.549(9) . ?
C19 C20 1.514(10) . ?
C21 C22 1.521(9) . ?
C23 C24 1.540(10) . ?
C25 C26 1.538(9) . ?
C27 N5 1.501(8) . ?
C27 C28 1.520(9) . ?
C27 C34 1.532(9) . ?
C27 C36 1.539(9) . ?
C28 C29 1.537(9) . ?
C29 C30 1.510(10) . ?
C29 C35 1.531(10) . ?
C30 C31 1.527(10) . ?
C31 C32 1.514(12) . ?
C31 C36 1.522(9) . ?
C32 C33 1.545(12) . ?
C33 C34 1.520(10) . ?
C33 C35 1.521(11) . ?
N1 N2 1.378(7) . ?
N3 N4 1.368(7) . ?

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
N5 Al1 C13 115.4(3) . . ?
N5 Al1 C15 117.4(3) . . ?
C13 Al1 C15 113.8(3) . . ?
N5 Al1 N1 92.8(2) . . ?
C13 Al1 N1 103.9(3) . . ?
C15 Al1 N1 110.2(3) . . ?
O1 Al2 C19 111.5(2) . . ?
O1 Al2 N4 91.8(2) . . ?
C19 Al2 N4 113.1(3) . . ?
O1 Al2 C17 116.6(2) . . ?
C19 Al2 C17 116.3(3) . . ?
N4 Al2 C17 104.7(3) . . ?
C25 Al3 C21 108.0(3) . . ?
C25 Al3 C23 112.9(3) . . ?
C21 Al3 C23 116.1(3) . . ?
C25 Al3 O1 112.7(2) . . ?
C21 Al3 O1 102.5(2) . . ?
C23 Al3 O1 104.2(3) . . ?
N5 C1 C2 121.5(6) . . ?
N5 C1 O1 121.7(5) . . ?
C2 C1 O1 116.8(5) . . ?
C1 C2 N2 121.8(5) . . ?
C1 C2 N3 123.8(6) . . ?
N2 C2 N3 114.4(5) . . ?
C5 C4 N2 106.3(6) . . ?
C5 C4 C3 131.4(6) . . ?
N2 C4 C3 122.3(6) . . ?
C4 C5 C6 107.6(6) . . ?
N1 C6 C5 109.4(6) . . ?
N1 C6 C7 121.8(7) . . ?
C5 C6 C7 128.8(7) . . ?
N3 C9 C10 105.5(6) . . ?
N3 C9 C8 123.3(6) . . ?
C10 C9 C8 131.2(6) . . ?
C9 C10 C11 108.3(6) . . ?
N4 C11 C10 109.0(6) . . ?
N4 C11 C12 121.5(6) . . ?
C10 C11 C12 129.4(6) . . ?
C14 C13 Al1 113.4(5) . . ?
C16 C15 Al1 116.6(5) . . ?
C18 C17 Al2 110.5(5) . . ?
C20 C19 Al2 116.4(5) . . ?
C22 C21 Al3 115.0(5) . . ?
C24 C23 Al3 114.1(4) . . ?
C26 C25 Al3 111.4(5) . . ?
N5 C27 C28 115.2(5) . . ?
N5 C27 C34 106.7(5) . . ?
C28 C27 C34 107.8(5) . . ?
N5 C27 C36 110.7(5) . . ?
C28 C27 C36 106.8(5) . . ?
C34 C27 C36 109.5(5) . . ?
C27 C28 C29 111.1(5) . . ?
C30 C29 C35 110.3(6) . . ?
C30 C29 C28 109.6(6) . . ?
C35 C29 C28 109.7(5) . . ?
C29 C30 C31 108.8(6) . . ?
C32 C31 C36 109.7(6) . . ?
C32 C31 C30 109.1(7) . . ?
C36 C31 C30 110.0(6) . . ?
C31 C32 C33 110.1(6) . . ?
C34 C33 C35 109.7(7) . . ?
C34 C33 C32 108.1(6) . . ?
C35 C33 C32 109.5(7) . . ?
C33 C34 C27 111.6(6) . . ?
C33 C35 C29 108.4(6) . . ?
C31 C36 C27 110.4(6) . . ?
C6 N1 N2 105.9(5) . . ?
C6 N1 Al1 136.9(5) . . ?
N2 N1 Al1 114.2(4) . . ?
C4 N2 N1 110.8(5) . . ?
C4 N2 C2 129.7(6) . . ?
N1 N2 C2 119.6(5) . . ?
C9 N3 N4 111.3(5) . . ?
C9 N3 C2 129.0(6) . . ?
N4 N3 C2 119.6(5) . . ?
C11 N4 N3 105.9(5) . . ?
C11 N4 Al2 136.2(5) . . ?
N3 N4 Al2 116.3(4) . . ?
C1 N5 C27 121.9(5) . . ?
C1 N5 Al1 110.9(4) . . ?
C27 N5 Al1 125.9(4) . . ?
C1 O1 Al2 114.0(4) . . ?
C1 O1 Al3 123.0(4) . . ?
Al2 O1 Al3 122.3(2) . . ?

_refine_diff_density_max         0.213
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.042

_shelxl_version_number           2014-3


####################################################################### 
# 
# 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_22
_database_code_depnum_ccdc_archive 'CCDC 2151216'
loop_
_audit_author_name
_audit_author_address
'Ana Maria Rodriguez'
;Universidad de Castilla la Mancha
Spain
;
_audit_update_record             
;
2022-06-28 deposited with the CCDC.	2022-06-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H45 Al2 N5 O'
_chemical_formula_sum            'C27 H45 Al2 N5 O'
_chemical_formula_weight         509.64

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'
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           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                   11.7654(13)
_cell_length_b                   19.445(2)
_cell_length_c                   13.2565(15)
_cell_angle_alpha                90
_cell_angle_beta                 97.2330(10)
_cell_angle_gamma                90
_cell_volume                     3008.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    3736
_cell_measurement_theta_min      2.421
_cell_measurement_theta_max      21.313

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_F_000             1104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.260
_exptl_absorpt_coefficient_mu    0.123
_shelx_estimated_absorpt_T_min   0.950
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      290(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector, APEX'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15843
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.727
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_full        22.500
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3933
_reflns_number_gt                2955
_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       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)'
_computing_data_reduction        'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)'
_computing_structure_solution    'SHELXS-2013/4 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013/4 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'WINGX v2014.1 (Farrugia, 2012)'

_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)+(0.0496P)²+1.0634P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         3933
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1073
_refine_ls_wR_factor_gt          0.0950
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
Al1 Al 0.51466(6) 0.12668(4) 0.76529(5) 0.0489(2) Uani 1 1 d . . . . .
Al2 Al 0.06919(7) 0.12558(4) 0.84066(7) 0.0597(3) Uani 1 1 d . . . . .
N1 N 0.51343(16) 0.15997(10) 0.90399(14) 0.0480(5) Uani 1 1 d . . . . .
N2 N 0.42104(16) 0.19004(10) 0.93800(14) 0.0488(5) Uani 1 1 d . . . . .
N3 N 0.44258(17) 0.28835(11) 0.77423(15) 0.0542(5) Uani 1 1 d . . . . .
N4 N 0.35286(16) 0.28304(10) 0.82944(14) 0.0479(5) Uani 1 1 d . . . . .
N5 N 0.35492(15) 0.14636(9) 0.71810(13) 0.0397(5) Uani 1 1 d . . . . .
O1 O 0.17517(13) 0.16514(8) 0.76317(12) 0.0517(4) Uani 1 1 d . . . . .
C1 C 0.5900(2) 0.14995(14) 0.9860(2) 0.0587(7) Uani 1 1 d . . . . .
C2 C 0.5459(3) 0.17442(16) 1.0708(2) 0.0727(8) Uani 1 1 d . . . . .
H2 H 0.582448 0.173652 1.137199 0.087 Uiso 1 1 calc R U . . .
C3 C 0.4399(2) 0.19975(16) 1.03999(19) 0.0659(8) Uani 1 1 d . . . . .
C4 C 0.7032(2) 0.11803(19) 0.9793(2) 0.0895(10) Uani 1 1 d . . . . .
H4A H 0.697694 0.069174 0.987956 0.134 Uiso 1 1 calc R U . . .
H4B H 0.758540 0.136482 1.031725 0.134 Uiso 1 1 calc R U . . .
H4C H 0.726572 0.127751 0.914011 0.134 Uiso 1 1 calc R U . . .
C5 C 0.3538(3) 0.2325(2) 1.0979(2) 0.1160(15) Uani 1 1 d . . . . .
H5A H 0.348905 0.280672 1.082327 0.174 Uiso 1 1 calc R U . . .
H5B H 0.376700 0.226443 1.169446 0.174 Uiso 1 1 calc R U . . .
H5C H 0.280420 0.211391 1.079245 0.174 Uiso 1 1 calc R U . . .
C6 C 0.2885(2) 0.34139(14) 0.8237(2) 0.0596(7) Uani 1 1 d . . . . .
C7 C 0.3413(2) 0.38520(15) 0.7655(2) 0.0676(8) Uani 1 1 d . . . . .
H7 H 0.318580 0.429934 0.748233 0.081 Uiso 1 1 calc R U . . .
C8 C 0.4350(2) 0.35136(14) 0.73646(18) 0.0545(7) Uani 1 1 d . . . . .
C9 C 0.1835(3) 0.34906(16) 0.8746(3) 0.0987(12) Uani 1 1 d . . . . .
H9A H 0.148833 0.392902 0.857340 0.148 Uiso 1 1 calc R U . . .
H9B H 0.203496 0.346159 0.946917 0.148 Uiso 1 1 calc R U . . .
H9C H 0.130320 0.313079 0.852258 0.148 Uiso 1 1 calc R U . . .
C10 C 0.5209(3) 0.37692(16) 0.6719(2) 0.0776(9) Uani 1 1 d . . . . .
H10A H 0.576083 0.341461 0.664824 0.116 Uiso 1 1 calc R U . . .
H10B H 0.559083 0.416533 0.703349 0.116 Uiso 1 1 calc R U . . .
H10C H 0.482851 0.389237 0.606081 0.116 Uiso 1 1 calc R U . . .
C11 C 0.32720(19) 0.21628(12) 0.86841(17) 0.0449(6) Uani 1 1 d . . . . .
H11 H 0.262651 0.222591 0.907555 0.054 Uiso 1 1 calc R U . . .
C12 C 0.28442(19) 0.16968(12) 0.77787(17) 0.0418(6) Uani 1 1 d . . . . .
C13 C 0.30647(19) 0.11981(12) 0.61404(16) 0.0433(6) Uani 1 1 d . . . . .
C14 C 0.4068(2) 0.10864(15) 0.55298(18) 0.0575(7) Uani 1 1 d . . . . .
H14A H 0.459963 0.075839 0.588028 0.069 Uiso 1 1 calc R U . . .
H14B H 0.447182 0.151710 0.547607 0.069 Uiso 1 1 calc R U . . .
C15 C 0.2431(2) 0.05203(12) 0.62127(17) 0.0478(6) Uani 1 1 d . . . . .
H15A H 0.178999 0.058555 0.659639 0.057 Uiso 1 1 calc R U . . .
H15B H 0.294237 0.018180 0.656392 0.057 Uiso 1 1 calc R U . . .
C16 C 0.2278(2) 0.17334(13) 0.55671(18) 0.0586(7) Uani 1 1 d . . . . .
H16A H 0.163352 0.182581 0.593635 0.070 Uiso 1 1 calc R U . . .
H16B H 0.269492 0.215973 0.551431 0.070 Uiso 1 1 calc R U . . .
C17 C 0.1846(3) 0.14651(15) 0.4505(2) 0.0698(8) Uani 1 1 d . . . . .
H17 H 0.132982 0.180521 0.414529 0.084 Uiso 1 1 calc R U . . .
C18 C 0.2852(3) 0.13405(17) 0.3912(2) 0.0820(10) Uani 1 1 d . . . . .
H18A H 0.257646 0.117399 0.323525 0.098 Uiso 1 1 calc R U . . .
H18B H 0.326252 0.176744 0.384482 0.098 Uiso 1 1 calc R U . . .
C19 C 0.3641(2) 0.08176(16) 0.4465(2) 0.0697(8) Uani 1 1 d . . . . .
H19 H 0.429685 0.074160 0.409059 0.084 Uiso 1 1 calc R U . . .
C20 C 0.3009(3) 0.01427(16) 0.4551(2) 0.0720(8) Uani 1 1 d . . . . .
H20A H 0.352253 -0.019554 0.490017 0.086 Uiso 1 1 calc R U . . .
H20B H 0.273865 -0.003181 0.387820 0.086 Uiso 1 1 calc R U . . .
C21 C 0.1998(2) 0.02647(14) 0.51417(18) 0.0604(7) Uani 1 1 d . . . . .
H21 H 0.158085 -0.016780 0.518956 0.072 Uiso 1 1 calc R U . . .
C22 C 0.1198(2) 0.07967(16) 0.4603(2) 0.0711(8) Uani 1 1 d . . . . .
H22A H 0.056006 0.087612 0.498498 0.085 Uiso 1 1 calc R U . . .
H22B H 0.089589 0.062981 0.393273 0.085 Uiso 1 1 calc R U . . .
C23 C 0.5271(3) 0.02702(15) 0.7857(2) 0.0750(9) Uani 1 1 d . . . . .
H23A H 0.474052 0.012541 0.830921 0.112 Uiso 1 1 calc R U . . .
H23B H 0.603680 0.015647 0.814783 0.112 Uiso 1 1 calc R U . . .
H23C H 0.509657 0.004065 0.721554 0.112 Uiso 1 1 calc R U . . .
C24 C 0.6347(2) 0.17440(16) 0.7051(2) 0.0696(8) Uani 1 1 d . . . . .
H24A H 0.675550 0.142159 0.668271 0.104 Uiso 1 1 calc R U . . .
H24B H 0.686697 0.195365 0.757819 0.104 Uiso 1 1 calc R U . . .
H24C H 0.601092 0.209256 0.659435 0.104 Uiso 1 1 calc R U . . .
C25 C 0.1667(3) 0.06428(18) 0.9326(3) 0.0933(10) Uani 1 1 d . . . . .
H25A H 0.214341 0.037427 0.893956 0.140 Uiso 1 1 calc R U . . .
H25B H 0.119297 0.034217 0.966762 0.140 Uiso 1 1 calc R U . . .
H25C H 0.214011 0.091295 0.981903 0.140 Uiso 1 1 calc R U . . .
C26 C -0.0420(3) 0.07946(18) 0.7409(3) 0.0970(11) Uani 1 1 d . . . . .
H26A H -0.070478 0.111491 0.688632 0.145 Uiso 1 1 calc R U . . .
H26B H -0.104511 0.062601 0.773957 0.145 Uiso 1 1 calc R U . . .
H26C H -0.005585 0.041677 0.711146 0.145 Uiso 1 1 calc R U . . .
C27 C 0.0002(2) 0.20293(15) 0.9080(2) 0.0748(9) Uani 1 1 d . . . . .
H27A H 0.056469 0.222778 0.958304 0.112 Uiso 1 1 calc R U . . .
H27B H -0.063319 0.186463 0.940056 0.112 Uiso 1 1 calc R U . . .
H27C H -0.026166 0.237146 0.858257 0.112 Uiso 1 1 calc R U . . .


_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 N5 1.9426(18) . ?
Al1 C24 1.943(3) . ?
Al1 N1 1.951(2) . ?
Al1 C23 1.960(3) . ?
Al2 O1 1.8774(17) . ?
Al2 C26 1.957(3) . ?
Al2 C25 1.967(3) . ?
Al2 C27 1.975(3) . ?
N1 C1 1.336(3) . ?
N1 N2 1.360(3) . ?
N2 C3 1.356(3) . ?
N2 C11 1.440(3) . ?
N3 C8 1.322(3) . ?
N3 N4 1.362(3) . ?
N4 C6 1.361(3) . ?
N4 C11 1.443(3) . ?
N5 C12 1.299(3) . ?
N5 C13 1.515(3) . ?
O1 C12 1.279(3) . ?
C1 C2 1.380(4) . ?
C1 C4 1.481(4) . ?
C2 C3 1.355(4) . ?
C3 C5 1.488(4) . ?
C6 C7 1.352(4) . ?
C6 C9 1.487(4) . ?
C7 C8 1.380(4) . ?
C8 C10 1.489(4) . ?
C11 C12 1.537(3) . ?
C13 C15 1.523(3) . ?
C13 C14 1.528(3) . ?
C13 C16 1.530(3) . ?
C14 C19 1.529(3) . ?
C15 C21 1.530(3) . ?
C16 C17 1.528(4) . ?
C17 C18 1.520(4) . ?
C17 C22 1.521(4) . ?
C18 C19 1.504(4) . ?
C19 C20 1.520(4) . ?
C20 C21 1.523(4) . ?
C21 C22 1.516(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Al1 C24 119.82(11) . . ?
N5 Al1 N1 96.69(8) . . ?
C24 Al1 N1 108.70(11) . . ?
N5 Al1 C23 106.96(11) . . ?
C24 Al1 C23 118.92(13) . . ?
N1 Al1 C23 101.94(11) . . ?
O1 Al2 C26 104.57(12) . . ?
O1 Al2 C25 102.22(12) . . ?
C26 Al2 C25 115.41(16) . . ?
O1 Al2 C27 105.92(10) . . ?
C26 Al2 C27 112.11(14) . . ?
C25 Al2 C27 114.99(15) . . ?
C1 N1 N2 106.16(19) . . ?
C1 N1 Al1 129.35(18) . . ?
N2 N1 Al1 123.78(14) . . ?
C3 N2 N1 110.7(2) . . ?
C3 N2 C11 127.3(2) . . ?
N1 N2 C11 121.34(18) . . ?
C8 N3 N4 104.7(2) . . ?
C6 N4 N3 111.8(2) . . ?
C6 N4 C11 129.0(2) . . ?
N3 N4 C11 118.14(19) . . ?
C12 N5 C13 118.58(18) . . ?
C12 N5 Al1 122.59(15) . . ?
C13 N5 Al1 117.63(14) . . ?
C12 O1 Al2 131.99(15) . . ?
N1 C1 C2 109.1(2) . . ?
N1 C1 C4 122.1(3) . . ?
C2 C1 C4 128.7(3) . . ?
C3 C2 C1 107.8(2) . . ?
C2 C3 N2 106.2(2) . . ?
C2 C3 C5 131.3(3) . . ?
N2 C3 C5 122.5(3) . . ?
C7 C6 N4 105.3(2) . . ?
C7 C6 C9 131.5(3) . . ?
N4 C6 C9 123.1(3) . . ?
C6 C7 C8 107.4(3) . . ?
N3 C8 C7 110.8(2) . . ?
N3 C8 C10 120.5(3) . . ?
C7 C8 C10 128.7(3) . . ?
N2 C11 N4 111.72(19) . . ?
N2 C11 C12 116.14(19) . . ?
N4 C11 C12 108.27(18) . . ?
O1 C12 N5 126.1(2) . . ?
O1 C12 C11 112.57(19) . . ?
N5 C12 C11 120.7(2) . . ?
N5 C13 C15 111.62(18) . . ?
N5 C13 C14 107.67(18) . . ?
C15 C13 C14 109.1(2) . . ?
N5 C13 C16 110.80(18) . . ?
C15 C13 C16 110.49(19) . . ?
C14 C13 C16 107.0(2) . . ?
C13 C14 C19 110.6(2) . . ?
C13 C15 C21 109.34(19) . . ?
C17 C16 C13 109.6(2) . . ?
C18 C17 C22 109.8(3) . . ?
C18 C17 C16 109.9(2) . . ?
C22 C17 C16 109.0(2) . . ?
C19 C18 C17 109.2(2) . . ?
C18 C19 C20 110.0(2) . . ?
C18 C19 C14 109.3(2) . . ?
C20 C19 C14 109.4(2) . . ?
C19 C20 C21 109.0(2) . . ?
C22 C21 C20 110.0(2) . . ?
C22 C21 C15 109.3(2) . . ?
C20 C21 C15 109.7(2) . . ?
C21 C22 C17 109.6(2) . . ?

_refine_diff_density_max         0.156
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.032



# start Validation Reply Form

_vrf_THETM01_17                  
;
PROBLEM:The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The datasets were integrated to a value of 45 for 2theta
due to the low intensity obtained for values higher than it. 
;
_vrf_THETM01_22                  
;
PROBLEM:The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE:
The high angle data above 2theta 45 have been omitted due to 
the low intensity obtained for values higher than it
;
# end Validation Reply Form
