# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1a_tol
_database_code_depnum_ccdc_archive 'CCDC 1825590'
_audit_update_record             
;
2018-04-05 deposited with the CCDC.
2018-04-06 downloaded from the CCDC.
;

_audit_creation_date             2018-01-12T15:35:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C6  H12  Li1  N1  O1  Al1'
_chemical_formula_sum            'C46 H54 Al2 Li2 N2 O2'
_chemical_formula_weight         734.75

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.1067(12)
_cell_length_b                   8.8238(11)
_cell_length_c                   22.6234(19)
_cell_angle_alpha                90
_cell_angle_beta                 94.210(7)
_cell_angle_gamma                90
_cell_volume                     2211.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    62
_cell_measurement_theta_min      3.013
_cell_measurement_theta_max      19.23
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.3
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -2 10 0.296
-3 2 -9 0.298
2 -1 -4 0.195
-2 1 5 0.214
10 9 4 0.148
-5 -4 -2 0.133


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#


_exptl_absorpt_coefficient_mu    0.102
_shelx_estimated_absorpt_T_min   0.952
_shelx_estimated_absorpt_T_max   0.97

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;

_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_T_max  1.143


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_number            9774
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.047
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             5085
_reflns_number_gt                2888
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     'direct - structure invariant direct methods'
_atom_sites_solution_secondary   'direct - structure invariant direct methods'
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0896P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5085
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1609
_refine_ls_wR_factor_gt          0.1401
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_restrained_S_all      0.976
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.4
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.046

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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 0.006 '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'

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
C1 C 0.7467(2) 0.1430(3) 0.01358(11) 0.0548(6) Uani 1 1 d . . . . .
H1A H 0.7368 0.0532 0.0383 0.082 Uiso 1 1 calc R U . . .
H1B H 0.6683 0.1929 0.0056 0.082 Uiso 1 1 calc R U . . .
H1C H 0.7782 0.1124 -0.024 0.082 Uiso 1 1 calc R U . . .
C1D C 1.0116(4) 0.5602(6) 0.61087(18) 0.1366(18) Uani 1 1 d . . . . .
H1D1 H 0.9641 0.4928 0.5837 0.205 Uiso 1 1 calc R U . . .
H1D2 H 1.0316 0.6529 0.5898 0.205 Uiso 1 1 calc R U . . .
H1D3 H 1.0861 0.5088 0.6255 0.205 Uiso 1 1 calc R U . . .
C2 C 0.8109(2) 0.3621(3) 0.13136(9) 0.0537(6) Uani 1 1 d . . . . .
H2A H 0.8029 0.2775 0.1588 0.08 Uiso 1 1 calc R U . . .
H2B H 0.872 0.4332 0.1482 0.08 Uiso 1 1 calc R U . . .
H2C H 0.7332 0.4144 0.1249 0.08 Uiso 1 1 calc R U . . .
C2D C 0.9392(3) 0.6002(4) 0.66235(14) 0.0861(10) Uani 1 1 d . . . . .
C3 C 1.0306(2) 0.2115(3) 0.05809(12) 0.0506(6) Uani 1 1 d . . . . .
C3D C 0.9890(3) 0.6944(4) 0.70611(18) 0.0904(10) Uani 1 1 d . . . . .
H3D H 1.068 0.7335 0.7032 0.108 Uiso 1 1 calc R U . . .
C4 C 0.83217(18) 0.3848(2) -0.12306(8) 0.0393(5) Uani 1 1 d . . . . .
H4 H 0.803 0.3622 -0.1626 0.047 Uiso 1 1 calc R U . . .
C4D C 0.9268(3) 0.7321(4) 0.75328(17) 0.0882(10) Uani 1 1 d . . . . .
H4D H 0.9621 0.7988 0.7826 0.106 Uiso 1 1 calc R U . . .
C5 C 0.77171(16) 0.5027(2) -0.02693(8) 0.0349(5) Uani 1 1 d . . . . .
C5D C 0.8147(3) 0.6756(4) 0.75911(14) 0.0767(8) Uani 1 1 d . . . . .
H5D H 0.7721 0.7019 0.7926 0.092 Uiso 1 1 calc R U . . .
C6 C 0.68970(19) 0.5892(3) 0.00119(10) 0.0492(6) Uani 1 1 d . . . . .
H6 H 0.7054 0.6137 0.0419 0.059 Uiso 1 1 calc R U . . .
C6D C 0.7637(3) 0.5820(4) 0.71718(16) 0.0781(9) Uani 1 1 d . . . . .
H6D H 0.6853 0.5422 0.7214 0.094 Uiso 1 1 calc R U . . .
C7 C 0.5853(2) 0.6408(3) -0.02902(11) 0.0613(7) Uani 1 1 d . . . . .
H7 H 0.5301 0.7014 -0.0092 0.074 Uiso 1 1 calc R U . . .
C7D C 0.8247(3) 0.5433(4) 0.66780(14) 0.0795(9) Uani 1 1 d . . . . .
H7D H 0.7881 0.4784 0.6382 0.095 Uiso 1 1 calc R U . . .
C8 C 0.5610(2) 0.6046(3) -0.08771(11) 0.0618(7) Uani 1 1 d . . . . .
H8 H 0.4884 0.6384 -0.1084 0.074 Uiso 1 1 calc R U . . .
C9 C 0.6417(2) 0.5197(3) -0.11621(10) 0.0512(6) Uani 1 1 d . . . . .
H9 H 0.624 0.4951 -0.1568 0.061 Uiso 1 1 calc R U . . .
C10 C 0.75022(17) 0.4679(2) -0.08719(8) 0.0368(5) Uani 1 1 d . . . . .
C11 C 1.00613(18) 0.2666(2) -0.15030(8) 0.0364(5) Uani 1 1 d . . . . .
C12 C 1.0807(2) 0.1484(3) -0.13189(9) 0.0478(6) Uani 1 1 d . . . . .
H12 H 1.0853 0.1178 -0.0915 0.057 Uiso 1 1 calc R U . . .
C13 C 1.1484(2) 0.0743(3) -0.17117(11) 0.0621(7) Uani 1 1 d . . . . .
H13 H 1.1982 -0.0085 -0.1581 0.075 Uiso 1 1 calc R U . . .
C14 C 1.1444(3) 0.1200(3) -0.22958(11) 0.0642(7) Uani 1 1 d . . . . .
H14 H 1.1905 0.0682 -0.257 0.077 Uiso 1 1 calc R U . . .
C15 C 1.0739(2) 0.2396(3) -0.24773(10) 0.0591(7) Uani 1 1 d . . . . .
H15 H 1.0724 0.2723 -0.2878 0.071 Uiso 1 1 calc R U . . .
C16 C 1.0046(2) 0.3143(3) -0.20866(9) 0.0488(6) Uani 1 1 d . . . . .
H16 H 0.956 0.3981 -0.2218 0.059 Uiso 1 1 calc R U . . .
Li1 Li 1.0188(3) 0.3760(4) -0.02711(13) 0.0390(8) Uani 1 1 d . . . . .
N1 N 0.93810(14) 0.33960(19) -0.10713(6) 0.0354(4) Uani 1 1 d . . . . .
O1 O 0.87404(11) 0.45339(15) 0.00494(5) 0.0342(3) Uani 1 1 d . . . . .
Al1 Al 0.86043(5) 0.28449(7) 0.05541(2) 0.0388(2) Uani 1 1 d . . . . .
H2 H 1.028(2) 0.128(3) 0.0856(12) 0.068(7) Uiso 1 1 d . . . . .
H1 H 1.091(2) 0.283(3) 0.0763(11) 0.069(8) Uiso 1 1 d . . . . .
H3 H 1.055(3) 0.175(4) 0.0190(16) 0.114(12) Uiso 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 Al1 1.969(2) . ?
C1D C2D 1.505(5) . ?
C2 Al1 1.965(2) . ?
C2D C3D 1.377(5) . ?
C2D C7D 1.381(5) . ?
C3 Al1 1.993(2) . ?
C3 Li1 2.409(4) . ?
C3D C4D 1.355(5) . ?
C4 N1 1.269(2) . ?
C4 C10 1.460(3) . ?
C4D C5D 1.357(5) . ?
C5 O1 1.371(2) . ?
C5 C6 1.379(3) . ?
C5 C10 1.401(3) . ?
C5 Li1 2.764(4) 3_765 ?
C5D C6D 1.351(4) . ?
C6 C7 1.380(3) . ?
C6D C7D 1.391(4) . ?
C7 C8 1.373(4) . ?
C8 C9 1.365(3) . ?
C9 C10 1.406(3) . ?
C11 C12 1.377(3) . ?
C11 C16 1.385(3) . ?
C11 N1 1.431(2) . ?
C12 C13 1.372(3) . ?
C13 C14 1.379(3) . ?
C14 C15 1.359(4) . ?
C15 C16 1.382(3) . ?
Li1 O1 1.936(3) . ?
Li1 O1 1.961(4) 3_765 ?
Li1 N1 1.986(3) . ?
Li1 Li1 2.558(7) 3_765 ?
Li1 C5 2.764(4) 3_765 ?
Li1 Al1 2.777(3) . ?
O1 Al1 1.8903(14) . ?
O1 Li1 1.961(4) 3_765 ?

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
C3D C2D C7D 118.6(3) . . ?
C3D C2D C1D 119.2(4) . . ?
C7D C2D C1D 122.1(4) . . ?
Al1 C3 Li1 77.59(11) . . ?
C4D C3D C2D 120.9(3) . . ?
N1 C4 C10 127.06(17) . . ?
C3D C4D C5D 120.8(4) . . ?
O1 C5 C6 118.88(17) . . ?
O1 C5 C10 121.17(17) . . ?
C6 C5 C10 119.94(18) . . ?
O1 C5 Li1 41.56(11) . 3_765 ?
C6 C5 Li1 98.31(16) . 3_765 ?
C10 C5 Li1 126.39(14) . 3_765 ?
C6D C5D C4D 119.8(3) . . ?
C7 C6 C5 120.9(2) . . ?
C5D C6D C7D 120.7(3) . . ?
C6 C7 C8 120.1(2) . . ?
C2D C7D C6D 119.2(3) . . ?
C9 C8 C7 119.7(2) . . ?
C8 C9 C10 121.9(2) . . ?
C9 C10 C5 117.51(19) . . ?
C9 C10 C4 116.86(18) . . ?
C5 C10 C4 125.62(17) . . ?
C12 C11 C16 118.94(19) . . ?
C12 C11 N1 118.08(17) . . ?
C16 C11 N1 122.91(19) . . ?
C13 C12 C11 120.8(2) . . ?
C12 C13 C14 120.0(2) . . ?
C15 C14 C13 119.6(2) . . ?
C14 C15 C16 120.8(2) . . ?
C15 C16 C11 119.8(2) . . ?
O1 Li1 O1 97.97(16) . 3_765 ?
O1 Li1 N1 93.84(14) . . ?
O1 Li1 N1 125.59(18) 3_765 . ?
O1 Li1 C3 84.88(13) . . ?
O1 Li1 C3 105.17(15) 3_765 . ?
N1 Li1 C3 128.77(19) . . ?
O1 Li1 Li1 49.42(11) . 3_765 ?
O1 Li1 Li1 48.55(12) 3_765 3_765 ?
N1 Li1 Li1 119.8(2) . 3_765 ?
C3 Li1 Li1 97.65(17) . 3_765 ?
O1 Li1 C5 113.15(15) . 3_765 ?
O1 Li1 C5 27.63(7) 3_765 3_765 ?
N1 Li1 C5 140.78(16) . 3_765 ?
C3 Li1 C5 83.39(12) . 3_765 ?
Li1 Li1 C5 67.55(14) 3_765 3_765 ?
O1 Li1 Al1 42.82(7) . . ?
O1 Li1 Al1 116.98(14) 3_765 . ?
N1 Li1 Al1 107.47(14) . . ?
C3 Li1 Al1 44.50(8) . . ?
Li1 Li1 Al1 78.04(14) 3_765 . ?
C5 Li1 Al1 111.68(11) 3_765 . ?
C4 N1 C11 118.21(16) . . ?
C4 N1 Li1 123.68(16) . . ?
C11 N1 Li1 117.99(15) . . ?
C5 O1 Al1 117.88(11) . . ?
C5 O1 Li1 126.44(14) . . ?
Al1 O1 Li1 93.07(12) . . ?
C5 O1 Li1 110.80(15) . 3_765 ?
Al1 O1 Li1 121.64(11) . 3_765 ?
Li1 O1 Li1 82.03(16) . 3_765 ?
O1 Al1 C1 106.65(8) . . ?
O1 Al1 C2 107.04(9) . . ?
C1 Al1 C2 115.51(11) . . ?
O1 Al1 C3 98.95(9) . . ?
C1 Al1 C3 112.52(12) . . ?
C2 Al1 C3 114.31(11) . . ?
O1 Al1 Li1 44.11(8) . . ?
C1 Al1 Li1 106.08(10) . . ?
C2 Al1 Li1 135.89(11) . . ?
C3 Al1 Li1 57.91(10) . . ?


# END of CIF
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_4bC6H6
_database_code_depnum_ccdc_archive 'CCDC 1825591'
_audit_update_record             
;
2018-04-05 deposited with the CCDC.
2018-04-06 downloaded from the CCDC.
;

_audit_creation_date             2018-04-04T18:37:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C52  H62  O2  K1  Al1  N2'
_chemical_formula_sum            'C52 H62 Al K N2 O2'
_chemical_formula_weight         813.11

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.053(3)
_cell_length_b                   11.5534(14)
_cell_length_c                   20.4001(16)
_cell_angle_alpha                90
_cell_angle_beta                 90.391(10)
_cell_angle_gamma                90
_cell_volume                     4726.1(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    209
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      19.56
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.42
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_T_max  1.331

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_number            33758
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.048
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_reflns_Friedel_coverage         0
_reflns_number_total             10658
_reflns_number_gt                6703
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELX (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0760P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10658
_refine_ls_number_parameters     529
_refine_ls_number_restraints     468
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.154
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.051

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

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
K1 K 0.24920(4) 0.51177(6) 0.31475(2) 0.03977(16) Uani 1 1 d . U . . .
Al1 Al 0.24965(6) 0.49745(8) 0.48692(3) 0.03087(17) Uani 1 1 d . U . . .
N1 N 0.12809(12) 0.61466(18) 0.34591(11) 0.0309(5) Uani 1 1 d . U . . .
N2 N 0.37041(12) 0.40398(19) 0.34219(12) 0.0361(5) Uani 1 1 d . U . . .
O1 O 0.19418(9) 0.43777(15) 0.42536(9) 0.0314(4) Uani 1 1 d . U . . .
O2 O 0.30393(10) 0.56648(16) 0.42963(9) 0.0332(4) Uani 1 1 d . U . . .
C1 C 0.19518(17) 0.5996(3) 0.54190(16) 0.0473(8) Uani 1 1 d . U . . .
H1A H 0.2233 0.6341 0.5762 0.071 Uiso 1 1 calc R U . . .
H1B H 0.1757 0.661 0.5147 0.071 Uiso 1 1 calc R U . . .
H1C H 0.1594 0.5545 0.5622 0.071 Uiso 1 1 calc R U . . .
C2 C 0.30419(17) 0.3880(3) 0.53786(17) 0.0523(9) Uani 1 1 d . U . . .
H2A H 0.3319 0.4308 0.5693 0.078 Uiso 1 1 calc R U . . .
H2B H 0.275 0.3346 0.5615 0.078 Uiso 1 1 calc R U . . .
H2C H 0.3329 0.3441 0.5082 0.078 Uiso 1 1 calc R U . . .
C10 C 0.07862(15) 0.5737(2) 0.37596(14) 0.0311(6) Uani 1 1 d . U . . .
H10 H 0.0387 0.6179 0.3741 0.037 Uiso 1 1 calc R U . . .
C11 C 0.07577(13) 0.4655(2) 0.41348(13) 0.0278(6) Uani 1 1 d . U . . .
C12 C 0.13137(14) 0.4024(2) 0.43612(12) 0.0270(5) Uani 1 1 d . U . . .
C13 C 0.12052(16) 0.2987(2) 0.46897(14) 0.0355(6) Uani 1 1 d . U . . .
H13 H 0.1577 0.2552 0.4842 0.043 Uiso 1 1 calc R U . . .
C14 C 0.05652(16) 0.2576(3) 0.47994(15) 0.0402(7) Uani 1 1 d . U . . .
H14 H 0.0503 0.1857 0.5016 0.048 Uiso 1 1 calc R U . . .
C15 C 0.00216(16) 0.3210(2) 0.45948(15) 0.0379(7) Uani 1 1 d . U . . .
H15 H -0.0417 0.2937 0.4676 0.046 Uiso 1 1 calc R U . . .
C16 C 0.01153(15) 0.4241(2) 0.42721(15) 0.0345(6) Uani 1 1 d . U . . .
H16 H -0.0262 0.4682 0.4139 0.041 Uiso 1 1 calc R U . . .
C17 C 0.13055(17) 0.8365(2) 0.41624(16) 0.0421(7) Uani 1 1 d . U . . .
H17 H 0.1142 0.7623 0.4357 0.05 Uiso 1 1 calc R U . . .
C18 C 0.0906(3) 0.9339(4) 0.4468(2) 0.0791(13) Uani 1 1 d . U . . .
H18A H 0.0435 0.9252 0.4349 0.119 Uiso 1 1 calc R U . . .
H18B H 0.0955 0.931 0.4946 0.119 Uiso 1 1 calc R U . . .
H18C H 0.1071 1.0084 0.4306 0.119 Uiso 1 1 calc R U . . .
C19 C 0.2035(2) 0.8474(4) 0.4337(2) 0.0755(12) Uani 1 1 d . U . . .
H19A H 0.2284 0.7837 0.4135 0.113 Uiso 1 1 calc R U . . .
H19B H 0.2206 0.9214 0.4174 0.113 Uiso 1 1 calc R U . . .
H19C H 0.2091 0.844 0.4814 0.113 Uiso 1 1 calc R U . . .
C20 C 0.42028(15) 0.4411(2) 0.37482(14) 0.0329(6) Uani 1 1 d . U . . .
H20 H 0.4603 0.3975 0.3718 0.04 Uiso 1 1 calc R U . . .
C21 C 0.42241(14) 0.5439(2) 0.41652(13) 0.0300(6) Uani 1 1 d . U . . .
C22 C 0.36648(14) 0.6030(2) 0.44144(13) 0.0304(6) Uani 1 1 d . U . . .
C23 C 0.37709(17) 0.7021(2) 0.47905(15) 0.0397(7) Uani 1 1 d . U . . .
H23 H 0.3398 0.7415 0.4969 0.048 Uiso 1 1 calc R U . . .
C24 C 0.44059(17) 0.7448(3) 0.49109(16) 0.0449(7) Uani 1 1 d . U . . .
H24 H 0.4463 0.8142 0.5155 0.054 Uiso 1 1 calc R U . . .
C25 C 0.49544(17) 0.6866(3) 0.46759(16) 0.0416(7) Uani 1 1 d . U . . .
H25 H 0.5392 0.7146 0.4761 0.05 Uiso 1 1 calc R U . . .
C26 C 0.48569(15) 0.5873(2) 0.43162(15) 0.0361(7) Uani 1 1 d . U . . .
H26 H 0.5236 0.5465 0.4164 0.043 Uiso 1 1 calc R U . . .
C27 C 0.36647(18) 0.1748(3) 0.40409(17) 0.0453(7) Uani 1 1 d . U . . .
H27 H 0.3813 0.2467 0.4272 0.054 Uiso 1 1 calc R U . . .
C28 C 0.2925(2) 0.1598(4) 0.4164(2) 0.0739(12) Uani 1 1 d . U . . .
H28A H 0.285 0.1487 0.4634 0.111 Uiso 1 1 calc R U . . .
H28B H 0.2686 0.229 0.4014 0.111 Uiso 1 1 calc R U . . .
H28C H 0.2762 0.092 0.3923 0.111 Uiso 1 1 calc R U . . .
C29 C 0.4054(2) 0.0731(4) 0.4331(2) 0.0772(12) Uani 1 1 d . U . . .
H29A H 0.3958 0.0667 0.48 0.116 Uiso 1 1 calc R U . . .
H29B H 0.3921 0.0015 0.4109 0.116 Uiso 1 1 calc R U . . .
H29C H 0.4533 0.0859 0.4271 0.116 Uiso 1 1 calc R U . . .
C30 C 0.11959(14) 0.7198(2) 0.30973(14) 0.0316(6) Uani 1 1 d . U . . .
C31 C 0.11456(15) 0.7138(2) 0.24173(14) 0.0351(6) Uani 1 1 d . U . . .
C32 C 0.11055(17) 0.8161(3) 0.20599(16) 0.0433(7) Uani 1 1 d . U . . .
H32 H 0.1068 0.8132 0.1596 0.052 Uiso 1 1 calc R U . . .
C33 C 0.11204(17) 0.9223(3) 0.23766(17) 0.0494(8) Uani 1 1 d . U . . .
H33 H 0.109 0.9917 0.2129 0.059 Uiso 1 1 calc R U . . .
C34 C 0.11790(17) 0.9276(2) 0.30416(17) 0.0453(7) Uani 1 1 d . U . . .
H34 H 0.1197 1.0011 0.3249 0.054 Uiso 1 1 calc R U . . .
C35 C 0.12137(15) 0.8277(2) 0.34269(14) 0.0351(6) Uani 1 1 d . U . . .
C36 C 0.11226(16) 0.5982(3) 0.20592(15) 0.0395(7) Uani 1 1 d . U . . .
H36 H 0.1241 0.5362 0.2381 0.047 Uiso 1 1 calc R U . . .
C37 C 0.0424(2) 0.5742(3) 0.1807(2) 0.0685(11) Uani 1 1 d . U . . .
H37A H 0.0417 0.4996 0.1578 0.103 Uiso 1 1 calc R U . . .
H37B H 0.0115 0.5717 0.2177 0.103 Uiso 1 1 calc R U . . .
H37C H 0.0288 0.6357 0.1504 0.103 Uiso 1 1 calc R U . . .
C38 C 0.1616(2) 0.5922(4) 0.1502(2) 0.0723(12) Uani 1 1 d . U . . .
H38A H 0.1582 0.5166 0.1288 0.108 Uiso 1 1 calc R U . . .
H38B H 0.1515 0.6534 0.1183 0.108 Uiso 1 1 calc R U . . .
H38C H 0.2069 0.6029 0.1675 0.108 Uiso 1 1 calc R U . . .
C40 C 0.37968(14) 0.3021(2) 0.30265(15) 0.0355(6) Uani 1 1 d . U . . .
C41 C 0.38489(15) 0.3165(2) 0.23465(15) 0.0373(6) Uani 1 1 d . U . . .
C42 C 0.39089(17) 0.2176(3) 0.19536(17) 0.0475(8) Uani 1 1 d . U . . .
H42 H 0.3951 0.2256 0.1492 0.057 Uiso 1 1 calc R U . . .
C43 C 0.39078(18) 0.1086(3) 0.22333(17) 0.0525(8) Uani 1 1 d . U . . .
H43 H 0.3957 0.042 0.1964 0.063 Uiso 1 1 calc R U . . .
C44 C 0.38361(17) 0.0963(3) 0.28984(18) 0.0483(8) Uani 1 1 d . U . . .
H44 H 0.3824 0.0207 0.3081 0.058 Uiso 1 1 calc R U . . .
C45 C 0.37803(16) 0.1920(2) 0.33135(15) 0.0384(6) Uani 1 1 d . U . . .
C46 C 0.38595(17) 0.4352(3) 0.20185(15) 0.0438(7) Uani 1 1 d . U . . .
H46 H 0.3753 0.4945 0.2359 0.053 Uiso 1 1 calc R U . . .
C47 C 0.4541(2) 0.4622(4) 0.1751(3) 0.0836(14) Uani 1 1 d . U . . .
H47A H 0.4873 0.456 0.2103 0.125 Uiso 1 1 calc R U . . .
H47B H 0.4648 0.4071 0.1402 0.125 Uiso 1 1 calc R U . . .
H47C H 0.4543 0.541 0.1573 0.125 Uiso 1 1 calc R U . . .
C48 C 0.3336(3) 0.4444(4) 0.1475(2) 0.0815(13) Uani 1 1 d . U . . .
H48A H 0.2896 0.4268 0.1654 0.122 Uiso 1 1 calc R U . . .
H48B H 0.3336 0.5232 0.1297 0.122 Uiso 1 1 calc R U . . .
H48C H 0.3441 0.3893 0.1126 0.122 Uiso 1 1 calc R U . . .
C50 C 0.1592(3) 0.2517(4) 0.2847(3) 0.0744(11) Uani 1 1 d . U . . .
H50 H 0.178(3) 0.255(6) 0.335(3) 0.17(3) Uiso 1 1 d . . . . .
C51 C 0.0975(2) 0.2756(3) 0.2720(3) 0.0727(11) Uani 1 1 d . U . . .
H51 H 0.0694 0.2971 0.3073 0.087 Uiso 1 1 calc R U . . .
C52 C 0.0727(2) 0.2715(3) 0.2144(3) 0.0773(11) Uani 1 1 d . U . . .
H52 H 0.0268 0.2892 0.2087 0.093 Uiso 1 1 calc R U . . .
C53 C 0.1076(3) 0.2440(4) 0.1625(2) 0.0934(13) Uani 1 1 d . U . . .
H53 H 0.088 0.2449 0.12 0.112 Uiso 1 1 calc R U . . .
C54 C 0.1750(3) 0.2132(4) 0.1716(3) 0.1048(16) Uani 1 1 d . U . . .
H54 H 0.202 0.1889 0.1361 0.126 Uiso 1 1 calc R U . . .
C55 C 0.2012(2) 0.2204(4) 0.2385(3) 0.0898(13) Uani 1 1 d . U . . .
H55 H 0.2466 0.2033 0.2483 0.108 Uiso 1 1 calc R U . . .
C60 C 0.3391(2) 0.7722(4) 0.2991(2) 0.0730(11) Uani 1 1 d . U . . .
H60 H 0.3239 0.7634 0.3428 0.73(18) Uiso 1 1 calc R . . . .
C61 C 0.2971(2) 0.8038(4) 0.2539(3) 0.0832(12) Uani 1 1 d . U . . .
H61 H 0.2525 0.8208 0.2661 0.1 Uiso 1 1 calc R U . . .
C62 C 0.3137(3) 0.8136(4) 0.1909(3) 0.0987(14) Uani 1 1 d . U . . .
H62 H 0.2822 0.8359 0.1583 0.118 Uiso 1 1 calc R U . . .
C63 C 0.3840(3) 0.7877(4) 0.1745(2) 0.0947(14) Uani 1 1 d . U . . .
H63 H 0.3996 0.7911 0.1306 0.114 Uiso 1 1 calc R U . . .
C64 C 0.4260(2) 0.7582(3) 0.2263(3) 0.0791(11) Uani 1 1 d . U . . .
H64 H 0.4718 0.7426 0.2186 0.095 Uiso 1 1 calc R U . . .
C65 C 0.4021(2) 0.7519(3) 0.2862(2) 0.0706(10) Uani 1 1 d . U . . .
H65 H 0.4314 0.7321 0.3213 0.085 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
K1 O2 2.657(2) . ?
K1 O1 2.660(2) . ?
K1 N1 2.781(2) . ?
K1 N2 2.784(3) . ?
K1 Al1 3.5162(8) . ?
K1 C50 3.556(4) . ?
Al1 O1 1.809(2) . ?
Al1 O2 1.790(2) . ?
Al1 C1 1.965(3) . ?
Al1 C2 1.964(3) . ?
N1 C10 1.262(4) . ?
N1 C30 1.431(3) . ?
N2 C20 1.272(4) . ?
N2 C40 1.439(3) . ?
O1 C12 1.344(3) . ?
O2 C22 1.343(3) . ?
C10 C11 1.466(4) . ?
C11 C16 1.404(4) . ?
C11 C12 1.408(4) . ?
C12 C13 1.390(4) . ?
C13 C14 1.388(4) . ?
C14 C15 1.376(5) . ?
C15 C16 1.374(4) . ?
C17 C18 1.518(5) . ?
C17 C19 1.509(6) . ?
C17 C35 1.514(4) . ?
C20 C21 1.461(4) . ?
C21 C26 1.397(4) . ?
C21 C22 1.411(4) . ?
C22 C23 1.394(4) . ?
C23 C24 1.386(5) . ?
C24 C25 1.378(5) . ?
C25 C26 1.375(4) . ?
C27 C45 1.516(5) . ?
C27 C28 1.515(5) . ?
C27 C29 1.528(5) . ?
C30 C35 1.417(4) . ?
C30 C31 1.392(4) . ?
C31 C32 1.390(4) . ?
C31 C36 1.523(4) . ?
C32 C33 1.387(4) . ?
C33 C34 1.362(5) . ?
C34 C35 1.397(4) . ?
C36 C37 1.514(5) . ?
C36 C38 1.513(5) . ?
C40 C41 1.402(4) . ?
C40 C45 1.402(4) . ?
C41 C42 1.401(4) . ?
C41 C46 1.526(4) . ?
C42 C43 1.384(5) . ?
C43 C44 1.373(5) . ?
C44 C45 1.398(4) . ?
C46 C48 1.524(5) . ?
C46 C47 1.507(5) . ?
C50 C51 1.292(6) . ?
C50 C55 1.318(7) . ?
C51 C52 1.274(7) . ?
C52 C53 1.313(7) . ?
C53 C54 1.408(8) . ?
C54 C55 1.462(8) . ?
C60 C61 1.298(7) . ?
C60 C65 1.311(6) . ?
C61 C62 1.334(7) . ?
C62 C63 1.481(8) . ?
C63 C64 1.389(8) . ?
C64 C65 1.318(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
O2 K1 O1 59.96(5) . . ?
O2 K1 N1 93.02(7) . . ?
O1 K1 N1 64.89(6) . . ?
O2 K1 N2 64.81(7) . . ?
O1 K1 N2 92.99(7) . . ?
N1 K1 N2 155.16(6) . . ?
O2 K1 Al1 29.77(5) . . ?
O1 K1 Al1 30.19(4) . . ?
N1 K1 Al1 77.77(5) . . ?
N2 K1 Al1 77.40(5) . . ?
O2 K1 C50 124.00(9) . . ?
O1 K1 C50 70.23(10) . . ?
N1 K1 C50 87.57(10) . . ?
N2 K1 C50 95.63(10) . . ?
Al1 K1 C50 97.49(9) . . ?
O1 Al1 O2 95.18(7) . . ?
O1 Al1 C1 106.48(13) . . ?
O2 Al1 C1 116.62(13) . . ?
O1 Al1 C2 117.36(14) . . ?
O2 Al1 C2 107.06(13) . . ?
C1 Al1 C2 113.22(12) . . ?
O1 Al1 K1 47.69(6) . . ?
O2 Al1 K1 47.48(6) . . ?
C1 Al1 K1 122.98(11) . . ?
C2 Al1 K1 123.80(11) . . ?
C10 N1 C30 118.5(2) . . ?
C10 N1 K1 129.88(17) . . ?
C30 N1 K1 110.24(16) . . ?
C20 N2 C40 117.7(2) . . ?
C20 N2 K1 129.54(18) . . ?
C40 N2 K1 111.64(18) . . ?
C12 O1 Al1 125.12(17) . . ?
C12 O1 K1 129.14(16) . . ?
Al1 O1 K1 102.11(8) . . ?
C22 O2 Al1 126.42(18) . . ?
C22 O2 K1 127.76(17) . . ?
Al1 O2 K1 102.75(9) . . ?
N1 C10 C11 127.4(3) . . ?
C16 C11 C12 118.9(2) . . ?
C16 C11 C10 115.7(2) . . ?
C12 C11 C10 125.4(2) . . ?
O1 C12 C13 119.4(2) . . ?
O1 C12 C11 122.0(2) . . ?
C13 C12 C11 118.6(3) . . ?
C14 C13 C12 121.4(3) . . ?
C13 C14 C15 120.0(3) . . ?
C16 C15 C14 119.7(3) . . ?
C15 C16 C11 121.3(3) . . ?
C18 C17 C19 110.8(3) . . ?
C18 C17 C35 113.3(3) . . ?
C19 C17 C35 110.5(3) . . ?
N2 C20 C21 126.8(3) . . ?
C26 C21 C22 118.0(3) . . ?
C26 C21 C20 116.3(2) . . ?
C22 C21 C20 125.6(3) . . ?
O2 C22 C23 119.7(3) . . ?
O2 C22 C21 121.8(2) . . ?
C23 C22 C21 118.5(3) . . ?
C24 C23 C22 121.8(3) . . ?
C25 C24 C23 119.9(3) . . ?
C24 C25 C26 118.8(3) . . ?
C25 C26 C21 122.9(3) . . ?
C45 C27 C28 109.5(3) . . ?
C45 C27 C29 113.5(3) . . ?
C28 C27 C29 110.2(3) . . ?
C35 C30 C31 121.2(2) . . ?
C35 C30 N1 120.0(3) . . ?
C31 C30 N1 118.7(2) . . ?
C30 C31 C32 118.9(3) . . ?
C30 C31 C36 121.6(2) . . ?
C32 C31 C36 119.5(3) . . ?
C33 C32 C31 120.4(3) . . ?
C34 C33 C32 120.3(3) . . ?
C33 C34 C35 121.8(3) . . ?
C30 C35 C34 117.3(3) . . ?
C30 C35 C17 122.1(2) . . ?
C34 C35 C17 120.5(3) . . ?
C31 C36 C37 110.4(3) . . ?
C31 C36 C38 112.5(3) . . ?
C37 C36 C38 110.2(3) . . ?
C41 C40 C45 121.6(2) . . ?
C41 C40 N2 117.9(2) . . ?
C45 C40 N2 120.3(3) . . ?
C42 C41 C40 118.5(3) . . ?
C42 C41 C46 118.7(3) . . ?
C40 C41 C46 122.8(2) . . ?
C43 C42 C41 120.4(3) . . ?
C42 C43 C44 120.2(3) . . ?
C45 C44 C43 121.8(3) . . ?
C44 C45 C40 117.6(3) . . ?
C44 C45 C27 120.2(3) . . ?
C40 C45 C27 122.1(2) . . ?
C48 C46 C47 110.1(3) . . ?
C48 C46 C41 111.7(3) . . ?
C47 C46 C41 111.1(3) . . ?
C51 C50 C55 122.1(5) . . ?
C51 C50 K1 109.8(3) . . ?
C55 C50 K1 91.6(3) . . ?
C52 C51 C50 122.9(5) . . ?
C51 C52 C53 123.1(5) . . ?
C52 C53 C54 118.1(5) . . ?
C53 C54 C55 116.6(4) . . ?
C50 C55 C54 117.0(5) . . ?
C61 C60 C65 122.0(5) . . ?
C60 C61 C62 122.8(5) . . ?
C61 C62 C63 116.5(5) . . ?
C64 C63 C62 116.7(4) . . ?
C65 C64 C63 119.8(5) . . ?
C60 C65 C64 122.1(5) . . ?


# END of CIF
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_5b
_database_code_depnum_ccdc_archive 'CCDC 1825592'
_audit_update_record             
;
2018-04-05 deposited with the CCDC.
2018-04-06 downloaded from the CCDC.
;

_audit_creation_date             2018-04-04T12:37:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C58  H69  N3  O3  Al1  K1'
_chemical_formula_sum            'C64 H83 Al K N3 O3'
_chemical_formula_weight         1008.41

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_Int_Tables_number      148
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   13.4310(11)
_cell_length_b                   13.4310(11)
_cell_length_c                   57.550(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     8990.6(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    223
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      19.02
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.43
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3264
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 7 0.295
-1 1 -7 0.263
3 4 5 0.277
-5 -1 6 0.278
-3 2 8 0.229
5 -4 -16 0.283
1 -3 -3 0.335


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.146


_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;

_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_T_max  1.008

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_number            13711
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_theta_min         3.033
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             4615
_reflns_number_gt                3239
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-2008 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1143P)²+13.4951P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4615
_refine_ls_number_parameters     198
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1995
_refine_ls_wR_factor_gt          0.1805
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.065

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 573 71 ' '
2 0.333 0.667 0.667 573 71 ' '
3 0.667 0.333 0.333 573 71 ' '
_platon_squeeze_details          
;                           
A molecules of hexene crystallized with every molecule of this 
 compound but presented severe disorder and it was not possible to get a 
 chemical sensible model for it, so Squeeze procedure was used to remove 
 its contribution to the structure factors.
;

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Al2 Al 0.333333 0.666667 0.01739(2) 0.0272(3) Uani 1 3 d S T P . .
K1 K 0.333333 0.666667 0.07254(2) 0.0326(2) Uani 1 3 d S T P . .
N1 N 0.58236(16) 0.77206(16) 0.07449(3) 0.0317(4) Uani 1 1 d . . . . .
O1 O 0.30000(15) 0.53820(13) 0.03194(3) 0.0345(4) Uani 1 1 d . . . . .
C1 C 0.333333 0.666667 -0.01637(7) 0.0430(10) Uani 1 3 d S T P . .
H1A H 0.353195 0.743205 -0.02205 0.064 Uiso 0.3333 1 calc R U P . .
H1B H 0.39001 0.646806 -0.02205 0.064 Uiso 0.3333 1 calc R U P . .
H1C H 0.256795 0.60999 -0.02205 0.064 Uiso 0.3333 1 calc R U P . .
C2 C 0.30048(18) 0.44236(18) 0.02623(4) 0.0280(4) Uani 1 1 d . . . . .
C3 C 0.35544(18) 0.4355(2) 0.00609(4) 0.0328(5) Uani 1 1 d . . . . .
H3 H 0.395946 0.501736 -0.003411 0.039 Uiso 1 1 calc R U . . .
C4 C 0.3521(2) 0.3352(2) -0.00023(4) 0.0384(5) Uani 1 1 d . . . . .
H4 H 0.390994 0.333337 -0.013867 0.046 Uiso 1 1 calc R U . . .
C5 C 0.2927(2) 0.2369(2) 0.01311(5) 0.0463(6) Uani 1 1 d . . . . .
H5 H 0.288796 0.167056 0.008587 0.056 Uiso 1 1 calc R U . . .
C6 C 0.2394(2) 0.2426(2) 0.03301(5) 0.0436(6) Uani 1 1 d . . . . .
H6 H 0.198893 0.17529 0.042233 0.052 Uiso 1 1 calc R U . . .
C7 C 0.24259(19) 0.34373(19) 0.04026(4) 0.0316(5) Uani 1 1 d . . . . .
C8 C 0.6642(2) 0.8481(2) 0.06218(4) 0.0340(5) Uani 1 1 d . . . . .
C9 C 0.61944(19) 0.74041(19) 0.09519(4) 0.0317(5) Uani 1 1 d . . . . .
C10 C 0.6534(2) 0.6573(2) 0.09399(4) 0.0400(5) Uani 1 1 d . . . . .
C11 C 0.6889(3) 0.6293(3) 0.11447(5) 0.0472(6) Uani 1 1 d . . . . .
H11 H 0.7111 0.572364 0.11414 0.057 Uiso 1 1 calc R U . . .
C12 C 0.6927(2) 0.6824(3) 0.13518(5) 0.0464(6) Uani 1 1 d . . . . .
H12 H 0.718916 0.663157 0.148871 0.056 Uiso 1 1 calc R U . . .
C13 C 0.6585(2) 0.7633(2) 0.13605(4) 0.0422(6) Uani 1 1 d . . . . .
H13 H 0.661167 0.799404 0.150417 0.051 Uiso 1 1 calc R U . . .
C14 C 0.6202(2) 0.7931(2) 0.11623(4) 0.0355(5) Uani 1 1 d . . . . .
C15 C 0.5820(3) 0.8821(2) 0.11749(5) 0.0460(6) Uani 1 1 d . . . . .
H15 H 0.542976 0.879062 0.102485 0.055 Uiso 1 1 calc R U . . .
C16 C 0.6824(4) 1.0018(3) 0.12009(11) 0.0913(14) Uani 1 1 d . . . . .
H16A H 0.7375 1.017434 0.107509 0.137 Uiso 1 1 calc R U . . .
H16B H 0.655391 1.057328 0.119382 0.137 Uiso 1 1 calc R U . . .
H16C H 0.71995 1.008726 0.135089 0.137 Uiso 1 1 calc R U . . .
C17 C 0.4964(4) 0.8569(4) 0.13679(8) 0.0791(11) Uani 1 1 d . . . . .
H17A H 0.431186 0.778799 0.134964 0.119 Uiso 1 1 calc R U . . .
H17B H 0.53349 0.863544 0.151825 0.119 Uiso 1 1 calc R U . . .
H17C H 0.468932 0.912146 0.136117 0.119 Uiso 1 1 calc R U . . .
C20 C 0.7412(11) 0.6293(12) 0.0602(2) 0.072(4) Uiso 0.302(9) 1 d . . P A 1
H20A H 0.806751 0.683859 0.069629 0.108 Uiso 0.302(9) 1 calc R U P A 1
H20B H 0.748683 0.561812 0.05681 0.108 Uiso 0.302(9) 1 calc R U P A 1
H20C H 0.73976 0.666158 0.045621 0.108 Uiso 0.302(9) 1 calc R U P A 1
C18 C 0.650189 0.598776 0.071126 0.040(17) Uiso 0.302(9) 1 d . . P A 1
H18 H 0.656316 0.536333 0.079292 0.061 Uiso 0.302(9) 1 calc R U P A 1
C19 C 0.5338(5) 0.5184(6) 0.06316(12) 0.0166(17) Uiso 0.302(9) 1 d . . P A 1
H19A H 0.478424 0.50999 0.075184 0.025 Uiso 0.302(9) 1 calc R U P A 1
H19B H 0.517907 0.547739 0.04888 0.025 Uiso 0.302(9) 1 calc R U P A 1
H19C H 0.52683 0.443393 0.060068 0.025 Uiso 0.302(9) 1 calc R U P A 1
C20' C 0.7345(4) 0.5501(4) 0.07093(9) 0.0608(15) Uiso 0.698(9) 1 d . . P A 2
H20D H 0.813572 0.613078 0.073158 0.091 Uiso 0.698(9) 1 calc R U P A 2
H20E H 0.713965 0.494145 0.083535 0.091 Uiso 0.698(9) 1 calc R U P A 2
H20F H 0.728645 0.512429 0.056004 0.091 Uiso 0.698(9) 1 calc R U P A 2
C18' C 0.6503(4) 0.5995(4) 0.07107(8) 0.054(10) Uiso 0.698(9) 1 d . . P A 2
H18' H 0.668054 0.654214 0.057864 0.081 Uiso 0.698(9) 1 calc R U P A 2
C19' C 0.5375(10) 0.4954(11) 0.0676(2) 0.142(4) Uiso 0.698(9) 1 d . . P A 2
H19D H 0.537404 0.459534 0.052745 0.213 Uiso 0.698(9) 1 calc R U P A 2
H19E H 0.522866 0.441072 0.080273 0.213 Uiso 0.698(9) 1 calc R U P A 2
H19F H 0.477303 0.516297 0.067416 0.213 Uiso 0.698(9) 1 calc R U P A 2
H8 H 0.746(3) 0.877(3) 0.0673(5) 0.052(8) Uiso 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Al2 O1 1.7625(16) . ?
Al2 O1 1.7625(16) 2_665 ?
Al2 O1 1.7625(16) 3_565 ?
Al2 C1 1.943(4) . ?
Al2 K1 3.1740(13) . ?
K1 O1 2.8045(17) 2_665 ?
K1 O1 2.8046(16) 3_565 ?
K1 O1 2.8046(16) . ?
K1 N1 2.9101(19) 2_665 ?
K1 N1 2.9102(19) 3_565 ?
K1 N1 2.9102(19) . ?
N1 C8 1.277(3) . ?
N1 C9 1.435(3) . ?
O1 C2 1.332(3) . ?
C2 C3 1.401(3) . ?
C2 C7 1.408(3) . ?
C3 C4 1.374(3) . ?
C4 C5 1.384(4) . ?
C5 C6 1.372(4) . ?
C6 C7 1.402(3) . ?
C7 C8 1.462(3) 3_565 ?
C9 C14 1.400(3) . ?
C9 C10 1.403(3) . ?
C10 C11 1.392(4) . ?
C10 C18' 1.521(5) . ?
C10 C18 1.522(2) . ?
C11 C12 1.377(4) . ?
C12 C13 1.376(4) . ?
C13 C14 1.390(3) . ?
C14 C15 1.521(3) . ?
C15 C16 1.503(5) . ?
C15 C17 1.510(5) . ?
C20 C18 1.248(13) . ?
C18 C19 1.461(6) . ?
C20' C18' 1.572(7) . ?
C18' C19' 1.473(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Al2 O1 99.29(7) . 2_665 ?
O1 Al2 O1 99.29(7) . 3_565 ?
O1 Al2 O1 99.29(7) 2_665 3_565 ?
O1 Al2 C1 118.36(6) . . ?
O1 Al2 C1 118.37(6) 2_665 . ?
O1 Al2 C1 118.36(6) 3_565 . ?
O1 Al2 K1 61.64(6) . . ?
O1 Al2 K1 61.63(6) 2_665 . ?
O1 Al2 K1 61.64(6) 3_565 . ?
C1 Al2 K1 180 . . ?
O1 K1 O1 57.23(5) 2_665 3_565 ?
O1 K1 O1 57.23(5) 2_665 . ?
O1 K1 O1 57.23(5) 3_565 . ?
O1 K1 N1 97.03(5) 2_665 2_665 ?
O1 K1 N1 60.98(5) 3_565 2_665 ?
O1 K1 N1 117.33(5) . 2_665 ?
O1 K1 N1 117.33(5) 2_665 3_565 ?
O1 K1 N1 97.04(5) 3_565 3_565 ?
O1 K1 N1 60.98(5) . 3_565 ?
N1 K1 N1 119.854(5) 2_665 3_565 ?
O1 K1 N1 60.98(5) 2_665 . ?
O1 K1 N1 117.33(5) 3_565 . ?
O1 K1 N1 97.04(5) . . ?
N1 K1 N1 119.852(5) 2_665 . ?
N1 K1 N1 119.851(5) 3_565 . ?
O1 K1 Al2 33.57(3) 2_665 . ?
O1 K1 Al2 33.57(3) 3_565 . ?
O1 K1 Al2 33.57(3) . . ?
N1 K1 Al2 92.21(4) 2_665 . ?
N1 K1 Al2 92.21(4) 3_565 . ?
N1 K1 Al2 92.21(4) . . ?
C8 N1 C9 114.24(19) . . ?
C8 N1 K1 133.43(15) . . ?
C9 N1 K1 111.88(13) . . ?
C2 O1 Al2 135.03(14) . . ?
C2 O1 K1 136.38(13) . . ?
Al2 O1 K1 84.79(6) . . ?
O1 C2 C3 121.7(2) . . ?
O1 C2 C7 120.04(19) . . ?
C3 C2 C7 118.3(2) . . ?
C4 C3 C2 121.6(2) . . ?
C3 C4 C5 120.6(2) . . ?
C6 C5 C4 118.6(2) . . ?
C5 C6 C7 122.5(2) . . ?
C6 C7 C2 118.4(2) . . ?
C6 C7 C8 115.6(2) . 3_565 ?
C2 C7 C8 126.0(2) . 3_565 ?
N1 C8 C7 128.1(2) . 2_665 ?
C14 C9 C10 121.4(2) . . ?
C14 C9 N1 119.0(2) . . ?
C10 C9 N1 119.6(2) . . ?
C11 C10 C9 117.7(2) . . ?
C11 C10 C18' 121.5(3) . . ?
C9 C10 C18' 120.8(3) . . ?
C11 C10 C18 121.2(2) . . ?
C9 C10 C18 121.13(19) . . ?
C12 C11 C10 121.5(2) . . ?
C13 C12 C11 120.0(2) . . ?
C12 C13 C14 121.0(2) . . ?
C13 C14 C9 118.3(2) . . ?
C13 C14 C15 120.4(2) . . ?
C9 C14 C15 121.2(2) . . ?
C16 C15 C17 110.0(3) . . ?
C16 C15 C14 111.7(3) . . ?
C17 C15 C14 112.2(3) . . ?
C19 C18 C20 126.6(7) . . ?
C19 C18 C10 113.4(3) . . ?
C20 C18 C10 119.7(6) . . ?
C19' C18' C10 110.8(6) . . ?
C19' C18' C20' 102.4(6) . . ?
C10 C18' C20' 112.2(4) . . ?



# END of CIF
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_refine_special_details          SQUEEZE
