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

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1470028'
_audit_update_record             
;
2016-03-22 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H33 Al1 K1 O1'
_chemical_formula_sum            'C34 H26 Al D6 K O'
_chemical_formula_weight         528.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 '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                   9.3304(19)
_cell_length_b                   22.004(7)
_cell_length_c                   14.487(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.699(19)
_cell_angle_gamma                90
_cell_volume                     2971.0(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    31
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      14.87
_cell_measurement_wavelength     0.71073

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_F_000             1104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    0.232


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

_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_T_max  0.983

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            19633
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_av_R_equivalents  0.1341
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.114
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5217
_reflns_number_gt                2803
_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       '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-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0603P)²+1.1878P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5217
_refine_ls_number_parameters     350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_ref         0.1648
_refine_ls_wR_factor_gt          0.1425
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.17
_refine_diff_density_rms         0.045

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
O1 O 1.4027(3) 0.23381(13) 0.59640(16) 0.0564(7) Uani 1 1 d . . . . .
Al1 Al 1.21872(12) 0.24304(5) 0.61168(7) 0.0459(3) Uani 1 1 d . . . . .
K1 K 0.96653(9) 0.23777(5) 0.38389(6) 0.0642(3) Uani 1 1 d . . . . .
C1 C 1.0131(4) 0.2745(2) 0.1585(3) 0.0567(11) Uani 1 1 d . . . . .
C1D C 0.1068(6) 0.0282(2) 0.7386(4) 0.0791(15) Uani 1 1 d . . . . .
D1D D 0.0865 0.0350 0.6760 0.095 Uiso 1 1 calc R U . . .
C2 C 1.0443(6) 0.3286(3) 0.1932(4) 0.0764(15) Uani 1 1 d . . . . .
C2D C 0.0335(5) 0.0589(2) 0.8024(4) 0.0701(13) Uani 1 1 d . . . . .
D2D D -0.0367 0.0868 0.7835 0.084 Uiso 1 1 calc R U . . .
C3 C 0.9662(6) 0.3859(2) 0.1690(4) 0.1033(19) Uani 1 1 d . . . . .
H3A H 1.0091 0.4191 0.2033 0.155 Uiso 1 1 calc R U . . .
H3B H 0.9716 0.3937 0.1040 0.155 Uiso 1 1 calc R U . . .
H3C H 0.8675 0.3820 0.1840 0.155 Uiso 1 1 calc R U . . .
C3D C 0.0632(5) 0.0487(2) 0.8950(4) 0.0725(13) Uani 1 1 d . . . . .
D3D D 0.0140 0.0701 0.9390 0.087 Uiso 1 1 calc R U . . .
C4 C 1.3303(6) 0.0533(3) 0.2548(4) 0.112(2) Uani 1 1 d . . . . .
H4A H 1.4137 0.0635 0.2930 0.167 Uiso 1 1 calc R U . . .
H4B H 1.2708 0.0259 0.2876 0.167 Uiso 1 1 calc R U . . .
H4C H 1.3595 0.0341 0.1992 0.167 Uiso 1 1 calc R U . . .
C4D C 0.1650(5) 0.0072(2) 0.9220(3) 0.0691(13) Uani 1 1 d . . . . .
D4D D 0.1843 0.0002 0.9846 0.083 Uiso 1 1 calc R U . . .
C5 C 1.0477(5) 0.1626(2) 0.1541(3) 0.0619(12) Uani 1 1 d . . . . .
H5 H 0.9632 0.1601 0.1175 0.074 Uiso 1 1 calc R U . . .
C5D C 0.2385(5) -0.0239(2) 0.8590(4) 0.0699(13) Uani 1 1 d . . . . .
D5D D 0.3071 -0.0525 0.8784 0.084 Uiso 1 1 calc R U . . .
C6 C 1.1223(5) 0.1097(2) 0.1762(3) 0.0711(13) Uani 1 1 d . . . . .
H6 H 1.0871 0.0727 0.1539 0.085 Uiso 1 1 calc R U . . .
C6D C 0.2112(6) -0.0132(2) 0.7661(3) 0.0775(14) Uani 1 1 d . . . . .
D6D D 0.2627 -0.0337 0.7223 0.093 Uiso 1 1 calc R U . . .
C7 C 1.2465(5) 0.1107(3) 0.2303(3) 0.0755(14) Uani 1 1 d . . . . .
C8 C 1.2931(5) 0.1670(3) 0.2629(3) 0.0755(15) Uani 1 1 d . . . . .
H8 H 1.3752 0.1689 0.3017 0.091 Uiso 1 1 calc R U . . .
C9 C 1.2223(5) 0.2199(3) 0.2397(3) 0.0640(13) Uani 1 1 d . . . . .
C10 C 1.0952(4) 0.2189(2) 0.1846(2) 0.0516(11) Uani 1 1 d . . . . .
C11 C 0.6872(4) 0.1820(2) 0.2793(3) 0.0522(11) Uani 1 1 d . . . . .
H11 H 0.7046 0.1500 0.2394 0.063 Uiso 1 1 calc R U . . .
C12 C 0.6639(4) 0.1688(2) 0.3704(3) 0.0640(12) Uani 1 1 d . . . . .
H12 H 0.6663 0.1286 0.3904 0.077 Uiso 1 1 calc R U . . .
C13 C 0.6375(5) 0.2142(3) 0.4313(3) 0.0788(16) Uani 1 1 d . . . . .
H13 H 0.6214 0.2053 0.4927 0.095 Uiso 1 1 calc R U . . .
C14 C 0.6350(6) 0.2728(3) 0.4006(3) 0.0797(17) Uani 1 1 d . . . . .
C15 C 0.6590(4) 0.2855(2) 0.3085(3) 0.0634(12) Uani 1 1 d . . . . .
H15 H 0.6568 0.3258 0.2892 0.076 Uiso 1 1 calc R U . . .
C16 C 0.6859(3) 0.24076(19) 0.2444(2) 0.0443(10) Uani 1 1 d . . . . .
C21 C 1.1492(4) 0.31363(17) 0.5353(2) 0.0453(10) Uani 1 1 d . . . . .
C22 C 1.0127(5) 0.3364(2) 0.5467(3) 0.0521(11) Uani 1 1 d . . . . .
C23 C 0.9541(5) 0.3838(2) 0.4954(3) 0.0686(13) Uani 1 1 d . . . . .
H23 H 0.8622 0.3976 0.5062 0.082 Uiso 1 1 calc R U . . .
C24 C 1.0321(5) 0.4103(2) 0.4283(3) 0.0717(13) Uani 1 1 d . . . . .
H24 H 0.9935 0.4422 0.3932 0.086 Uiso 1 1 calc R U . . .
C25 C 1.1665(5) 0.3894(2) 0.4135(3) 0.0663(12) Uani 1 1 d . . . . .
H25 H 1.2199 0.4072 0.3681 0.080 Uiso 1 1 calc R U . . .
C26 C 1.2242(4) 0.34172(19) 0.4655(2) 0.0508(10) Uani 1 1 d . . . . .
H26 H 1.3157 0.3279 0.4537 0.061 Uiso 1 1 calc R U . . .
C31 C 1.1051(4) 0.17216(17) 0.5642(2) 0.0470(10) Uani 1 1 d . . . . .
C32 C 1.1475(5) 0.1331(2) 0.4952(3) 0.0628(12) Uani 1 1 d . . . . .
H32 H 1.2386 0.1379 0.4729 0.075 Uiso 1 1 calc R U . . .
C33 C 1.0614(6) 0.0877(2) 0.4586(3) 0.0752(14) Uani 1 1 d . . . . .
H33 H 1.0942 0.0635 0.4114 0.090 Uiso 1 1 calc R U . . .
C34 C 0.9292(6) 0.0779(2) 0.4902(3) 0.0742(14) Uani 1 1 d . . . . .
H34 H 0.8717 0.0468 0.4655 0.089 Uiso 1 1 calc R U . . .
C35 C 0.8806(5) 0.1145(2) 0.5598(3) 0.0655(12) Uani 1 1 d . . . . .
H35 H 0.7904 0.1082 0.5828 0.079 Uiso 1 1 calc R U . . .
C36 C 0.9676(5) 0.16024(19) 0.5945(3) 0.0592(11) Uani 1 1 d . . . . .
H36 H 0.9332 0.1847 0.6408 0.071 Uiso 1 1 calc R U . . .
H2 H 1.132(6) 0.327(2) 0.228(4) 0.12(2) Uiso 1 1 d . . . . .
H22 H 0.956(4) 0.3214(15) 0.590(2) 0.038(10) Uiso 1 1 d . . . . .
H9 H 1.252(4) 0.2587(17) 0.254(2) 0.044(11) Uiso 1 1 d . . . . .
H10 H 0.622(5) 0.304(2) 0.436(3) 0.080(16) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.347(4) 4_666 ?
O1 Al1 1.753(3) . ?
Al1 C31 1.990(4) . ?
Al1 C21 1.998(4) . ?
Al1 C16 1.994(4) 4_666 ?
Al1 K1 3.9635(16) . ?
K1 C21 3.186(4) . ?
K1 C11 3.197(4) . ?
K1 C12 3.204(4) . ?
K1 C15 3.200(4) . ?
K1 C31 3.203(4) . ?
K1 C10 3.206(4) . ?
K1 C14 3.208(5) . ?
K1 C13 3.220(5) . ?
K1 C22 3.220(4) . ?
K1 C16 3.232(3) . ?
K1 C32 3.241(4) . ?
K1 C9 3.268(5) . ?
C1 C2 1.319(6) . ?
C1 O1 1.347(4) 4_565 ?
C1 C10 1.483(6) . ?
C1D C2D 1.356(6) . ?
C1D C6D 1.378(6) . ?
C2 C3 1.491(7) . ?
C2D C3D 1.376(6) . ?
C3D C4D 1.362(6) . ?
C4 C7 1.519(7) . ?
C4D C5D 1.353(6) . ?
C5 C10 1.381(6) . ?
C5 C6 1.387(6) . ?
C5D C6D 1.380(6) . ?
C6 C7 1.368(6) . ?
C7 C8 1.389(7) . ?
C8 C9 1.373(7) . ?
C9 C10 1.399(6) . ?
C11 C12 1.378(5) . ?
C11 C16 1.389(5) . ?
C12 C13 1.363(6) . ?
C13 C14 1.365(7) . ?
C14 C15 1.391(6) . ?
C15 C16 1.385(5) . ?
C16 Al1 1.994(4) 4_565 ?
C21 C22 1.386(5) . ?
C21 C26 1.399(5) . ?
C22 C23 1.377(6) . ?
C23 C24 1.372(6) . ?
C24 C25 1.362(6) . ?
C25 C26 1.385(5) . ?
C31 C32 1.390(5) . ?
C31 C36 1.400(6) . ?
C32 C33 1.373(6) . ?
C33 C34 1.354(6) . ?
C34 C35 1.383(6) . ?
C35 C36 1.374(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 Al1 130.8(2) 4_666 . ?
O1 Al1 C31 112.00(16) . . ?
O1 Al1 C21 108.31(15) . . ?
C31 Al1 C21 105.31(15) . . ?
O1 Al1 C16 109.77(13) . 4_666 ?
C31 Al1 C16 111.71(16) . 4_666 ?
C21 Al1 C16 109.57(17) . 4_666 ?
O1 Al1 K1 115.97(9) . . ?
C31 Al1 K1 53.39(11) . . ?
C21 Al1 K1 52.91(11) . . ?
C16 Al1 K1 134.13(11) 4_666 . ?
C21 K1 C11 157.68(11) . . ?
C21 K1 C12 137.04(11) . . ?
C11 K1 C12 24.86(10) . . ?
C21 K1 C15 120.34(11) . . ?
C11 K1 C15 42.80(11) . . ?
C12 K1 C15 50.29(12) . . ?
C21 K1 C31 59.50(10) . . ?
C11 K1 C31 120.13(11) . . ?
C12 K1 C31 99.02(11) . . ?
C15 K1 C31 138.36(11) . . ?
C21 K1 C10 118.49(10) . . ?
C11 K1 C10 81.67(10) . . ?
C12 K1 C10 104.47(11) . . ?
C15 K1 C10 95.91(11) . . ?
C31 K1 C10 121.49(11) . . ?
C21 K1 C14 107.99(13) . . ?
C11 K1 C14 50.24(14) . . ?
C12 K1 C14 42.97(15) . . ?
C15 K1 C14 25.07(12) . . ?
C31 K1 C14 113.60(13) . . ?
C10 K1 C14 120.15(11) . . ?
C21 K1 C13 114.98(12) . . ?
C11 K1 C13 43.52(11) . . ?
C12 K1 C13 24.50(12) . . ?
C15 K1 C13 43.68(13) . . ?
C31 K1 C13 96.06(12) . . ?
C10 K1 C13 124.93(11) . . ?
C14 K1 C13 24.52(13) . . ?
C21 K1 C22 24.99(10) . . ?
C11 K1 C22 133.15(11) . . ?
C12 K1 C22 116.84(13) . . ?
C15 K1 C22 96.64(11) . . ?
C31 K1 C22 70.82(10) . . ?
C10 K1 C22 134.77(12) . . ?
C14 K1 C22 83.06(14) . . ?
C13 K1 C22 92.79(13) . . ?
C21 K1 C16 144.21(10) . . ?
C11 K1 C16 24.94(9) . . ?
C12 K1 C16 44.42(10) . . ?
C15 K1 C16 24.86(10) . . ?
C31 K1 C16 143.42(11) . . ?
C10 K1 C16 76.48(10) . . ?
C14 K1 C16 44.48(11) . . ?
C13 K1 C16 51.98(10) . . ?
C22 K1 C16 121.39(10) . . ?
C21 K1 C32 77.31(11) . . ?
C11 K1 C32 110.92(11) . . ?
C12 K1 C32 97.51(12) . . ?
C15 K1 C32 147.28(13) . . ?
C31 K1 C32 24.90(10) . . ?
C10 K1 C32 98.50(11) . . ?
C14 K1 C32 127.96(15) . . ?
C13 K1 C32 105.01(14) . . ?
C22 K1 C32 93.78(11) . . ?
C16 K1 C32 135.53(11) . . ?
C21 K1 C9 96.87(11) . . ?
C11 K1 C9 104.76(11) . . ?
C12 K1 C9 124.90(13) . . ?
C15 K1 C9 119.44(11) . . ?
C31 K1 C9 100.85(12) . . ?
C10 K1 C9 24.93(10) . . ?
C14 K1 C9 144.36(12) . . ?
C13 K1 C9 148.14(13) . . ?
C22 K1 C9 118.19(12) . . ?
C16 K1 C9 101.38(10) . . ?
C32 K1 C9 81.59(13) . . ?
C2 C1 O1 121.7(5) . 4_565 ?
C2 C1 C10 123.0(4) . . ?
O1 C1 C10 115.3(4) 4_565 . ?
C2 C1 K1 83.4(3) . . ?
O1 C1 K1 118.6(2) 4_565 . ?
C10 C1 K1 69.4(2) . . ?
C2D C1D C6D 120.3(5) . . ?
C1 C2 C3 125.2(5) . . ?
C1 C2 K1 74.7(3) . . ?
C3 C2 K1 123.4(4) . . ?
C1D C2D C3D 120.0(5) . . ?
C4D C3D C2D 119.6(5) . . ?
C5D C4D C3D 121.1(5) . . ?
C10 C5 C6 121.9(4) . . ?
C4D C5D C6D 119.6(5) . . ?
C7 C6 C5 121.4(5) . . ?
C1D C6D C5D 119.4(5) . . ?
C6 C7 C8 116.9(5) . . ?
C6 C7 C4 122.2(5) . . ?
C8 C7 C4 120.9(5) . . ?
C9 C8 C7 122.3(4) . . ?
C8 C9 C10 120.7(5) . . ?
C8 C9 K1 107.7(3) . . ?
C10 C9 K1 75.0(2) . . ?
C5 C10 C9 116.6(5) . . ?
C5 C10 C1 120.3(4) . . ?
C9 C10 C1 123.1(4) . . ?
C5 C10 K1 106.0(3) . . ?
C9 C10 K1 80.0(2) . . ?
C1 C10 K1 84.9(2) . . ?
C12 C11 C16 123.1(4) . . ?
C12 C11 K1 77.8(2) . . ?
C16 C11 K1 78.9(2) . . ?
C13 C12 C11 120.4(5) . . ?
C13 C12 K1 78.4(3) . . ?
C11 C12 K1 77.3(2) . . ?
C14 C13 C12 118.8(4) . . ?
C14 C13 K1 77.3(3) . . ?
C12 C13 K1 77.1(3) . . ?
C13 C14 C15 120.1(5) . . ?
C13 C14 K1 78.2(3) . . ?
C15 C14 K1 77.1(3) . . ?
C16 C15 C14 122.8(5) . . ?
C16 C15 K1 78.9(2) . . ?
C14 C15 K1 77.8(3) . . ?
C11 C16 C15 114.6(4) . . ?
C11 C16 Al1 121.3(3) . 4_565 ?
C15 C16 Al1 124.1(3) . 4_565 ?
C11 C16 K1 76.1(2) . . ?
C15 C16 K1 76.3(2) . . ?
Al1 C16 K1 116.75(14) 4_565 . ?
C22 C21 C26 114.8(4) . . ?
C22 C21 Al1 119.4(3) . . ?
C26 C21 Al1 125.7(3) . . ?
C22 C21 K1 78.9(2) . . ?
C26 C21 K1 90.2(2) . . ?
Al1 C21 K1 97.08(14) . . ?
C23 C22 C21 123.6(4) . . ?
C23 C22 K1 94.5(3) . . ?
C21 C22 K1 76.1(2) . . ?
C24 C23 C22 119.6(4) . . ?
C25 C24 C23 119.4(4) . . ?
C24 C25 C26 120.5(4) . . ?
C25 C26 C21 122.2(4) . . ?
C25 C26 K1 93.9(2) . . ?
C21 C26 K1 66.1(2) . . ?
C32 C31 C36 113.9(4) . . ?
C32 C31 Al1 124.6(3) . . ?
C36 C31 Al1 121.3(3) . . ?
C32 C31 K1 79.0(2) . . ?
C36 C31 K1 90.0(2) . . ?
Al1 C31 K1 96.70(14) . . ?
C33 C32 C31 123.1(4) . . ?
C33 C32 K1 92.4(3) . . ?
C31 C32 K1 76.0(2) . . ?
C34 C33 C32 120.8(5) . . ?
C33 C34 C35 119.2(5) . . ?
C36 C35 C34 119.0(5) . . ?
C35 C36 C31 123.9(4) . . ?
C35 C36 K1 93.5(3) . . ?
C31 C36 K1 66.4(2) . . ?



####################################################################### 
# 
# 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_1R4S_1a
_database_code_depnum_ccdc_archive 'CCDC 1470029'
_audit_update_record             
;
2016-03-22 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H77 Al2 K2 N4 O2.C6 D6'
_chemical_formula_sum            'C58 H77 Al2 D6 K2 N4 O2'
_chemical_formula_weight         1006.48

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

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

_cell_length_a                   32.214(11)
_cell_length_b                   11.964(8)
_cell_length_c                   15.575(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6003(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    22
_cell_measurement_theta_max      16.076
_cell_measurement_theta_min      2.986

_diffrn_ambient_temperature      200
_diffrn_radiation_probe          x-ray
_exptl_crystal_description       prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.114
_exptl_crystal_F_000             2156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_absorpt_coefficient_mu    0.228
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

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

_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_T_max  1.093






_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_number            92427
_diffrn_reflns_av_unetI/netI     0.1432
_diffrn_reflns_av_R_equivalents  0.1692
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.049
_diffrn_reflns_theta_max         19.997
_diffrn_reflns_theta_full        19.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5580
_reflns_number_gt                3230
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

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

_computing_data_collection       '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-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


_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)+(0.1452P)²] 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 872 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(5)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         5580
_refine_ls_number_parameters     549
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1572
_refine_ls_R_factor_gt           0.0998
_refine_ls_wR_factor_ref         0.2563
_refine_ls_wR_factor_gt          0.2245
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# 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 -0.033 0.362 437 45 ' '
2 0.500 -0.086 0.638 437 45 ' '
3 0.676 0.057 0.735 12 1 ' '
4 0.179 0.083 0.750 7 0 ' '
5 0.176 0.443 0.265 12 1 ' '
6 0.679 0.417 0.250 7 0 ' '
7 0.824 0.557 0.265 12 0 ' '
8 0.321 0.583 0.250 7 0 ' '
9 0.324 0.943 0.735 12 0 ' '
10 0.821 0.917 0.750 7 0 ' '
_platon_squeeze_details          
;
 A molecule of deuterated benzene 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 
 their contribution to the structure factors.
;






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 0.08557(19) 0.4146(5) 0.7856(4) 0.0687(19) Uani 1 1 d . . . . .
Al2 Al 0.20976(17) 0.7764(5) 0.7782(3) 0.0579(17) Uani 1 1 d . . . . .
K1 K 0.19605(13) 0.4749(3) 0.7997(2) 0.0632(13) Uani 1 1 d . . . . .
K2 K 0.10080(14) 0.7123(4) 0.7623(3) 0.0830(16) Uani 1 1 d . . . . .
N11 N 0.2444(5) 0.5883(11) 0.4654(8) 0.044(4) Uani 1 1 d . . . . .
H11 H 0.2400 0.5951 0.4099 0.053 Uiso 1 1 calc R U . . .
N21 N 0.1186(5) 0.439(2) 1.1292(11) 0.079(5) Uani 1 1 d . . . . .
H21 H 0.1054 0.4685 1.1731 0.095 Uiso 1 1 calc R U . . .
N1 N 0.1942(4) 0.6100(12) 0.6589(10) 0.050(4) Uani 1 1 d . . . . .
N2 N 0.1349(4) 0.5017(13) 0.9202(11) 0.058(4) Uani 1 1 d . . . . .
O1 O 0.1756(3) 0.6907(10) 0.7120(6) 0.057(3) Uani 1 1 d . . . . .
O2 O 0.1111(4) 0.5258(10) 0.8433(7) 0.062(4) Uani 1 1 d . . . . .
C1 C 0.0734(7) 0.4894(19) 0.6731(14) 0.094(7) Uani 1 1 d . . . . .
C3 C 0.0376(7) 0.346(2) 0.8517(14) 0.124(10) Uani 1 1 d . . . . .
H3A H 0.0250 0.2863 0.8173 0.187 Uiso 1 1 calc R U . . .
H3B H 0.0479 0.3147 0.9058 0.187 Uiso 1 1 calc R U . . .
H3C H 0.0168 0.4035 0.8638 0.187 Uiso 1 1 calc R U . . .
C2 C 0.1276(6) 0.2951(17) 0.7653(14) 0.087(7) Uani 1 1 d . . . . .
C4 C 0.2344(7) 0.8973(18) 0.7066(14) 0.110(8) Uani 1 1 d . . . . .
H4A H 0.2527 0.9435 0.7420 0.164 Uiso 1 1 calc R U . . .
H4B H 0.2504 0.8641 0.6595 0.164 Uiso 1 1 calc R U . . .
H4C H 0.2121 0.9440 0.6829 0.164 Uiso 1 1 calc R U . . .
C5 C 0.1709(6) 0.8350(17) 0.8679(11) 0.075(6) Uani 1 1 d . . . . .
C6 C 0.2540(6) 0.6798(16) 0.8307(11) 0.070(6) Uani 1 1 d . . . . .
C10 C 0.1945(5) 0.6324(13) 0.5786(11) 0.037(4) Uani 1 1 d . . . . .
C18 C 0.1752(5) 0.7294(15) 0.5319(9) 0.048(5) Uani 1 1 d . . . . .
H18A H 0.1634 0.7816 0.5747 0.058 Uiso 1 1 calc R U . . .
H18B H 0.1973 0.7697 0.5004 0.058 Uiso 1 1 calc R U . . .
C12 C 0.1420(5) 0.6979(15) 0.4700(11) 0.047(5) Uiso 1 1 d . . . . .
H12 H 0.1191 0.6630 0.5042 0.056 Uiso 1 1 calc R U . . .
C13 C 0.1239(7) 0.791(2) 0.4234(12) 0.072(6) Uani 1 1 d . . . . .
C14 C 0.1371(8) 0.890(2) 0.4243(14) 0.095(8) Uani 1 1 d . . . . .
H14A H 0.1608 0.9091 0.4576 0.114 Uiso 1 1 calc R U . . .
H14B H 0.1233 0.9461 0.3916 0.114 Uiso 1 1 calc R U . . .
C15 C 0.0835(7) 0.7662(19) 0.3734(12) 0.095(8) Uani 1 1 d . . . . .
H15A H 0.0768 0.6866 0.3778 0.143 Uiso 1 1 calc R U . . .
H15B H 0.0607 0.8105 0.3977 0.143 Uiso 1 1 calc R U . . .
H15C H 0.0873 0.7863 0.3129 0.143 Uiso 1 1 calc R U . . .
C16 C 0.1573(6) 0.6097(17) 0.4078(11) 0.065(6) Uani 1 1 d . . . . .
H16A H 0.1340 0.5846 0.3713 0.078 Uiso 1 1 calc R U . . .
H16B H 0.1787 0.6427 0.3699 0.078 Uiso 1 1 calc R U . . .
C17 C 0.1758(5) 0.5086(16) 0.4549(11) 0.063(6) Uani 1 1 d . . . . .
H17A H 0.1866 0.4546 0.4121 0.075 Uiso 1 1 calc R U . . .
H17B H 0.1536 0.4710 0.4880 0.075 Uiso 1 1 calc R U . . .
C11 C 0.2120(5) 0.5429(13) 0.5178(10) 0.038(5) Uani 1 1 d . . . . .
C30 C 0.2270(5) 0.4378(14) 0.5674(11) 0.055(5) Uani 1 1 d . . . . .
H30A H 0.2042 0.4086 0.6026 0.082 Uiso 1 1 calc R U . . .
H30B H 0.2359 0.3804 0.5264 0.082 Uiso 1 1 calc R U . . .
H30C H 0.2504 0.4579 0.6046 0.082 Uiso 1 1 calc R U . . .
C26 C 0.2812(6) 0.6210(16) 0.4972(14) 0.053(6) Uani 1 1 d . . . . .
C20 C 0.2886(7) 0.6487(17) 0.5852(14) 0.064(6) Uani 1 1 d . . . . .
H20 H 0.2668 0.6395 0.6258 0.077 Uiso 1 1 calc R U . . .
C22 C 0.3254(9) 0.687(2) 0.6119(14) 0.089(8) Uani 1 1 d . . . . .
H22 H 0.3295 0.7028 0.6711 0.107 Uiso 1 1 calc R U . . .
C23 C 0.3572(7) 0.7041(17) 0.5554(17) 0.077(7) Uani 1 1 d . . . . .
H23 H 0.3828 0.7334 0.5756 0.092 Uiso 1 1 calc R U . . .
C24 C 0.3525(7) 0.6789(18) 0.4677(14) 0.074(7) Uani 1 1 d . . . . .
H24 H 0.3749 0.6861 0.4283 0.089 Uiso 1 1 calc R U . . .
C25 C 0.3128(8) 0.6423(15) 0.4413(14) 0.069(7) Uani 1 1 d . . . . .
H25 H 0.3078 0.6320 0.3817 0.083 Uiso 1 1 calc R U . . .
C39 C 0.1172(6) 0.5270(16) 0.9912(12) 0.042(5) Uani 1 1 d . . . . .
C31 C 0.0780(7) 0.5757(16) 0.9998(11) 0.060(6) Uani 1 1 d . . . . .
H31A H 0.0598 0.5236 1.0318 0.072 Uiso 1 1 calc R U . . .
H31B H 0.0659 0.5861 0.9420 0.072 Uiso 1 1 calc R U . . .
C32 C 0.0782(7) 0.690(2) 1.0468(13) 0.082(7) Uani 1 1 d . . . . .
H32 H 0.0950 0.7429 1.0114 0.099 Uiso 1 1 calc R U . . .
C33 C 0.0364(10) 0.741(2) 1.060(2) 0.097(9) Uani 1 1 d . . . . .
C34 C 0.0312(10) 0.839(4) 1.016(2) 0.169(15) Uani 1 1 d . . . . .
H34A H 0.0568 0.8578 0.9850 0.253 Uiso 1 1 calc R U . . .
H34B H 0.0083 0.8315 0.9747 0.253 Uiso 1 1 calc R U . . .
H34C H 0.0247 0.8994 1.0566 0.253 Uiso 1 1 calc R U . . .
C35 C 0.0043(7) 0.699(2) 1.1074(15) 0.118(10) Uani 1 1 d . . . . .
H35A H -0.0213 0.7383 1.1102 0.141 Uiso 1 1 calc R U . . .
H35B H 0.0077 0.6310 1.1379 0.141 Uiso 1 1 calc R U . . .
C36 C 0.0999(7) 0.6760(19) 1.1310(12) 0.078(7) Uani 1 1 d . . . . .
H36A H 0.1040 0.7500 1.1580 0.094 Uiso 1 1 calc R U . . .
H36B H 0.0826 0.6300 1.1700 0.094 Uiso 1 1 calc R U . . .
C37 C 0.1419(8) 0.619(2) 1.1169(12) 0.094(8) Uani 1 1 d . . . . .
H37A H 0.1547 0.6059 1.1737 0.113 Uiso 1 1 calc R U . . .
H37B H 0.1601 0.6716 1.0852 0.113 Uiso 1 1 calc R U . . .
C21 C 0.1410(7) 0.5115(19) 1.0694(12) 0.066(6) Uani 1 1 d . . . . .
C40 C 0.1867(6) 0.4702(18) 1.0541(12) 0.081(7) Uani 1 1 d . . . . .
H40A H 0.2007 0.5208 1.0139 0.122 Uiso 1 1 calc R U . . .
H40B H 0.2018 0.4695 1.1088 0.122 Uiso 1 1 calc R U . . .
H40C H 0.1862 0.3945 1.0300 0.122 Uiso 1 1 calc R U . . .
C46 C 0.1178(6) 0.321(3) 1.1175(16) 0.089(9) Uani 1 1 d . . . . .
C41 C 0.1126(7) 0.275(2) 1.040(2) 0.137(13) Uani 1 1 d . . . . .
H41 H 0.1131 0.3227 0.9909 0.164 Uiso 1 1 calc R U . . .
C42 C 0.1068(7) 0.166(4) 1.0293(18) 0.137(12) Uani 1 1 d . . . . .
H42 H 0.1019 0.1386 0.9730 0.165 Uiso 1 1 calc R U . . .
C43 C 0.1077(8) 0.087(2) 1.101(2) 0.117(9) Uani 1 1 d . . . . .
H43 H 0.1067 0.0076 1.0960 0.140 Uiso 1 1 calc R U . . .
C44 C 0.1100(9) 0.141(3) 1.169(2) 0.143(12) Uiso 1 1 d . . . . .
H44 H 0.1083 0.0948 1.2185 0.172 Uiso 1 1 calc R U . . .
C45 C 0.1143(7) 0.249(2) 1.1877(14) 0.091(8) Uani 1 1 d . . . . .
H45 H 0.1149 0.2759 1.2451 0.109 Uiso 1 1 calc R U . . .
C60 C -0.0103(10) 0.788(3) 0.6349(19) 0.161(12) Uani 1 1 d . . . . .
H60A H -0.0292 0.7810 0.6839 0.241 Uiso 1 1 calc R U . . .
H60B H -0.0244 0.8277 0.5881 0.241 Uiso 1 1 calc R U . . .
H60C H -0.0019 0.7140 0.6153 0.241 Uiso 1 1 calc R U . . .
C61 C 0.0298(9) 0.858(2) 0.663(2) 0.089(8) Uani 1 1 d . . . . .
C62 C 0.0620(11) 0.883(3) 0.6107(17) 0.106(10) Uani 1 1 d . . . . .
H62 H 0.0626 0.8541 0.5538 0.127 Uiso 1 1 calc R U . . .
C63 C 0.0926(11) 0.947(3) 0.639(3) 0.138(14) Uani 1 1 d . . . . .
H63 H 0.1147 0.9673 0.6018 0.165 Uiso 1 1 calc R U . . .
C64 C 0.0920(12) 0.981(3) 0.718(3) 0.125(12) Uani 1 1 d . . . . .
H64 H 0.1139 1.0290 0.7359 0.150 Uiso 1 1 calc R U . . .
C65 C 0.0633(13) 0.955(2) 0.774(2) 0.105(9) Uani 1 1 d . . . . .
H65 H 0.0649 0.9805 0.8320 0.126 Uiso 1 1 calc R U . . .
C66 C 0.0301(9) 0.887(3) 0.746(2) 0.103(8) Uani 1 1 d . . . . .
H66 H 0.0089 0.8634 0.7843 0.123 Uiso 1 1 calc R U . . .
C70 C 0.2154(11) 0.138(3) 0.917(2) 0.187(17) Uani 1 1 d . . . . .
H70A H 0.2060 0.0862 0.8722 0.281 Uiso 1 1 calc R U . . .
H70B H 0.2315 0.0962 0.9600 0.281 Uiso 1 1 calc R U . . .
H70C H 0.1913 0.1723 0.9447 0.281 Uiso 1 1 calc R U . . .
C71 C 0.2414(9) 0.224(2) 0.8790(19) 0.096(9) Uani 1 1 d . . . . .
C72 C 0.2498(10) 0.221(2) 0.791(3) 0.124(11) Uani 1 1 d . . . . .
H72 H 0.2365 0.1659 0.7572 0.149 Uiso 1 1 calc R U . . .
C73 C 0.2777(12) 0.299(3) 0.7491(17) 0.117(12) Uani 1 1 d . . . . .
H73 H 0.2835 0.2938 0.6894 0.141 Uiso 1 1 calc R U . . .
C74 C 0.2940(10) 0.373(3) 0.797(3) 0.127(12) Uani 1 1 d . . . . .
H74 H 0.3129 0.4248 0.7713 0.153 Uiso 1 1 calc R U . . .
C75 C 0.2856(10) 0.383(3) 0.883(3) 0.117(10) Uani 1 1 d . . . . .
H75 H 0.2980 0.4408 0.9152 0.140 Uiso 1 1 calc R U . . .
C76 C 0.2603(8) 0.311(2) 0.9200(16) 0.081(7) Uani 1 1 d . . . . .
H76 H 0.2550 0.3200 0.9796 0.098 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 O2 1.804(13) . ?
Al1 C1 2.01(2) . ?
Al1 C2 1.99(2) . ?
Al1 C3 2.03(2) . ?
Al1 K2 3.613(8) . ?
Al1 K1 3.638(8) . ?
Al2 O1 1.824(12) . ?
Al2 C6 2.01(2) . ?
Al2 C5 2.002(19) . ?
Al2 C4 1.99(2) . ?
Al2 K2 3.602(7) . ?
Al2 K1 3.650(8) . ?
K1 N1 2.724(14) . ?
K1 N2 2.739(17) . ?
K1 O2 2.884(13) . ?
K1 O1 2.994(12) . ?
K1 C6 3.118(19) . ?
K1 C2 3.13(2) . ?
K1 C75 3.35(2) . ?
K1 C76 3.41(2) . ?
K1 C74 3.38(3) . ?
K1 C72 3.50(2) . ?
K1 C73 3.46(2) . ?
K2 O1 2.546(12) . ?
K2 O2 2.584(13) . ?
K2 C66 3.10(2) . ?
K2 C1 3.13(2) . ?
K2 C5 3.16(2) . ?
K2 C65 3.15(2) . ?
K2 C61 3.26(2) . ?
K2 C64 3.30(3) . ?
K2 C62 3.36(3) . ?
K2 C63 3.41(3) . ?
N11 C26 1.34(2) . ?
N11 C11 1.431(19) . ?
N21 C46 1.42(3) . ?
N21 C21 1.47(2) . ?
N1 C10 1.279(18) . ?
N1 O1 1.406(16) . ?
N2 C39 1.281(19) . ?
N2 O2 1.451(17) . ?
C10 C18 1.50(2) . ?
C10 C11 1.54(2) . ?
C18 C12 1.49(2) . ?
C12 C13 1.45(2) . ?
C12 C16 1.52(2) . ?
C13 C14 1.27(3) . ?
C13 C15 1.55(3) . ?
C16 C17 1.53(2) . ?
C17 C11 1.58(2) . ?
C11 C30 1.55(2) . ?
C26 C25 1.36(2) . ?
C26 C20 1.43(2) . ?
C20 C22 1.34(2) . ?
C22 C23 1.36(3) . ?
C23 C24 1.41(2) . ?
C24 C25 1.41(3) . ?
C39 C31 1.40(2) . ?
C39 C21 1.45(2) . ?
C31 C32 1.55(3) . ?
C32 C36 1.50(2) . ?
C32 C33 1.49(3) . ?
C33 C35 1.37(3) . ?
C33 C34 1.37(4) . ?
C36 C37 1.53(3) . ?
C37 C21 1.49(3) . ?
C21 C40 1.57(3) . ?
C46 C41 1.33(3) . ?
C46 C45 1.39(3) . ?
C41 C42 1.33(4) . ?
C42 C43 1.46(4) . ?
C43 C44 1.24(3) . ?
C44 C45 1.34(4) . ?
C60 C61 1.60(3) . ?
C61 C62 1.36(3) . ?
C61 C66 1.33(3) . ?
C62 C63 1.33(4) . ?
C63 C64 1.29(4) . ?
C64 C65 1.32(4) . ?
C65 C66 1.41(3) . ?
C70 C71 1.46(3) . ?
C71 C76 1.36(3) . ?
C71 C72 1.40(4) . ?
C72 C73 1.44(4) . ?
C73 C74 1.27(4) . ?
C74 C75 1.37(4) . ?
C75 C76 1.32(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Al1 C1 101.3(8) . . ?
O2 Al1 C2 107.3(8) . . ?
C1 Al1 C2 108.3(9) . . ?
O2 Al1 C3 113.2(8) . . ?
C1 Al1 C3 118.3(10) . . ?
C2 Al1 C3 107.8(10) . . ?
O2 Al1 K2 42.4(4) . . ?
C1 Al1 K2 60.0(7) . . ?
C2 Al1 K2 126.8(6) . . ?
C3 Al1 K2 123.6(9) . . ?
O2 Al1 K1 51.5(4) . . ?
C1 Al1 K1 99.0(7) . . ?
C2 Al1 K1 59.2(6) . . ?
C3 Al1 K1 142.6(7) . . ?
K2 Al1 K1 71.21(15) . . ?
O1 Al2 C6 109.5(7) . . ?
O1 Al2 C5 102.4(7) . . ?
C6 Al2 C5 111.1(8) . . ?
O1 Al2 C4 109.4(7) . . ?
C6 Al2 C4 111.4(9) . . ?
C5 Al2 C4 112.7(9) . . ?
O1 Al2 K2 41.7(4) . . ?
C6 Al2 K2 126.6(6) . . ?
C5 Al2 K2 60.9(6) . . ?
C4 Al2 K2 120.3(7) . . ?
O1 Al2 K1 54.7(4) . . ?
C6 Al2 K1 58.6(6) . . ?
C5 Al2 K1 101.9(6) . . ?
C4 Al2 K1 144.8(7) . . ?
K2 Al2 K1 71.20(14) . . ?
N1 K1 N2 117.8(5) . . ?
N1 K1 O2 92.5(4) . . ?
N2 K1 O2 29.8(3) . . ?
N1 K1 O1 28.0(3) . . ?
N2 K1 O1 93.1(4) . . ?
O2 K1 O1 73.5(3) . . ?
N1 K1 C6 70.8(5) . . ?
N2 K1 C6 103.4(5) . . ?
O2 K1 C6 111.4(5) . . ?
O1 K1 C6 61.6(4) . . ?
N1 K1 C2 104.8(5) . . ?
N2 K1 C2 72.0(5) . . ?
O2 K1 C2 61.1(4) . . ?
O1 K1 C2 111.1(5) . . ?
C6 K1 C2 171.6(5) . . ?
N1 K1 C75 121.6(9) . . ?
N2 K1 C75 113.2(8) . . ?
O2 K1 C75 142.8(8) . . ?
O1 K1 C75 130.5(8) . . ?
C6 K1 C75 71.6(7) . . ?
C2 K1 C75 116.6(8) . . ?
N1 K1 C76 142.7(6) . . ?
N2 K1 C76 97.3(6) . . ?
O2 K1 C76 124.6(5) . . ?
O1 K1 C76 151.6(6) . . ?
C6 K1 C76 90.2(6) . . ?
C2 K1 C76 97.3(7) . . ?
C75 K1 C76 22.5(6) . . ?
N1 K1 C74 102.8(7) . . ?
N2 K1 C74 136.3(8) . . ?
O2 K1 C74 164.7(7) . . ?
O1 K1 C74 120.6(5) . . ?
C6 K1 C74 74.1(7) . . ?
C2 K1 C74 114.1(8) . . ?
C75 K1 C74 23.5(6) . . ?
C76 K1 C74 40.1(6) . . ?
N1 K1 C72 119.7(9) . . ?
N2 K1 C72 118.9(9) . . ?
O2 K1 C72 131.5(8) . . ?
O1 K1 C72 147.1(8) . . ?
C6 K1 C72 113.1(7) . . ?
C2 K1 C72 75.3(7) . . ?
C75 K1 C72 45.7(7) . . ?
C76 K1 C72 38.9(6) . . ?
C74 K1 C72 39.2(7) . . ?
N1 K1 C73 101.2(7) . . ?
N2 K1 C73 140.6(7) . . ?
O2 K1 C73 154.5(9) . . ?
O1 K1 C73 126.1(7) . . ?
C6 K1 C73 93.4(9) . . ?
C2 K1 C73 94.5(9) . . ?
C75 K1 C73 39.8(7) . . ?
C76 K1 C73 46.6(6) . . ?
C74 K1 C73 21.4(7) . . ?
C72 K1 C73 24.0(6) . . ?
N1 K1 Al1 92.8(3) . . ?
N2 K1 Al1 50.3(3) . . ?
O2 K1 Al1 29.3(3) . . ?
O1 K1 Al1 85.9(3) . . ?
C6 K1 Al1 138.6(4) . . ?
C2 K1 Al1 33.2(4) . . ?
C75 K1 Al1 143.2(8) . . ?
C76 K1 Al1 120.8(6) . . ?
C74 K1 Al1 147.2(7) . . ?
C72 K1 Al1 108.1(6) . . ?
C73 K1 Al1 127.5(8) . . ?
O1 K2 O2 86.6(4) . . ?
O1 K2 C66 137.5(6) . . ?
O2 K2 C66 135.8(6) . . ?
O1 K2 C1 92.5(5) . . ?
O2 K2 C1 61.2(5) . . ?
C66 K2 C1 109.3(9) . . ?
O1 K2 C5 62.0(4) . . ?
O2 K2 C5 93.1(5) . . ?
C66 K2 C5 104.7(9) . . ?
C1 K2 C5 146.0(6) . . ?
O1 K2 C65 118.3(9) . . ?
O2 K2 C65 144.7(7) . . ?
C66 K2 C65 26.1(6) . . ?
C1 K2 C65 134.6(8) . . ?
C5 K2 C65 79.3(8) . . ?
O1 K2 C61 125.0(7) . . ?
O2 K2 C61 141.4(6) . . ?
C66 K2 C61 24.1(6) . . ?
C1 K2 C61 92.7(7) . . ?
C5 K2 C61 120.0(7) . . ?
C65 K2 C61 42.9(7) . . ?
O1 K2 C64 96.6(8) . . ?
O2 K2 C64 162.6(9) . . ?
C66 K2 C64 42.5(8) . . ?
C1 K2 C64 135.3(8) . . ?
C5 K2 C64 73.6(8) . . ?
C65 K2 C64 23.4(6) . . ?
C61 K2 C64 47.3(8) . . ?
O1 K2 C62 101.4(6) . . ?
O2 K2 C62 156.1(7) . . ?
C66 K2 C62 42.3(6) . . ?
C1 K2 C62 95.7(8) . . ?
C5 K2 C62 110.5(8) . . ?
C65 K2 C62 48.7(7) . . ?
C61 K2 C62 23.6(6) . . ?
C64 K2 C62 39.6(9) . . ?
O1 K2 C63 89.1(7) . . ?
O2 K2 C63 174.3(9) . . ?
C66 K2 C63 48.9(7) . . ?
C1 K2 C63 115.4(10) . . ?
C5 K2 C63 88.1(10) . . ?
C65 K2 C63 41.0(8) . . ?
C61 K2 C63 40.6(7) . . ?
C64 K2 C63 22.1(7) . . ?
C62 K2 C63 22.6(7) . . ?
O1 K2 Al2 28.4(3) . . ?
O2 K2 Al2 91.4(3) . . ?
C66 K2 Al2 125.3(7) . . ?
C1 K2 Al2 119.1(5) . . ?
C5 K2 Al2 33.7(3) . . ?
C65 K2 Al2 100.0(8) . . ?
C61 K2 Al2 127.1(6) . . ?
C64 K2 Al2 83.7(7) . . ?
C62 K2 Al2 106.4(7) . . ?
C63 K2 Al2 86.5(7) . . ?
O1 K2 Al1 93.4(3) . . ?
O2 K2 Al1 28.1(3) . . ?
C66 K2 Al1 125.0(7) . . ?
C1 K2 Al1 33.7(4) . . ?
C5 K2 Al1 120.2(4) . . ?
C65 K2 Al1 148.3(9) . . ?
C61 K2 Al1 118.5(5) . . ?
C64 K2 Al1 165.8(7) . . ?
C62 K2 Al1 128.2(7) . . ?
C63 K2 Al1 149.0(10) . . ?
Al2 K2 Al1 109.60(18) . . ?
C26 N11 C11 123.0(14) . . ?
C46 N21 C21 121.0(18) . . ?
C10 N1 O1 115.7(13) . . ?
C10 N1 K1 155.6(12) . . ?
O1 N1 K1 86.7(8) . . ?
C39 N2 O2 115.5(14) . . ?
C39 N2 K1 160.0(12) . . ?
O2 N2 K1 80.6(8) . . ?
N1 O1 Al2 117.4(9) . . ?
N1 O1 K2 130.9(9) . . ?
Al2 O1 K2 109.9(5) . . ?
N1 O1 K1 65.3(7) . . ?
Al2 O1 K1 95.4(5) . . ?
K2 O1 K1 99.0(4) . . ?
N2 O2 Al1 120.4(10) . . ?
N2 O2 K2 130.0(9) . . ?
Al1 O2 K2 109.5(6) . . ?
N2 O2 K1 69.6(8) . . ?
Al1 O2 K1 99.2(5) . . ?
K2 O2 K1 100.9(4) . . ?
Al1 C1 K2 86.4(7) . . ?
Al1 C2 K1 87.6(7) . . ?
Al2 C5 K2 85.5(6) . . ?
Al2 C6 K1 88.0(6) . . ?
N1 C10 C18 129.2(14) . . ?
N1 C10 C11 117.3(15) . . ?
C18 C10 C11 113.0(13) . . ?
C12 C18 C10 114.5(15) . . ?
C13 C12 C18 114.8(16) . . ?
C13 C12 C16 110.1(15) . . ?
C18 C12 C16 110.8(15) . . ?
C14 C13 C12 126(2) . . ?
C14 C13 C15 118(2) . . ?
C12 C13 C15 117(2) . . ?
C17 C16 C12 111.7(14) . . ?
C16 C17 C11 112.2(15) . . ?
N11 C11 C10 110.8(13) . . ?
N11 C11 C17 106.5(12) . . ?
C10 C11 C17 107.0(13) . . ?
N11 C11 C30 111.3(13) . . ?
C10 C11 C30 111.8(13) . . ?
C17 C11 C30 109.2(14) . . ?
N11 C26 C25 118(2) . . ?
N11 C26 C20 124.6(18) . . ?
C25 C26 C20 116.5(19) . . ?
C22 C20 C26 121.6(19) . . ?
C23 C22 C20 121(2) . . ?
C24 C23 C22 121.0(19) . . ?
C23 C24 C25 116.4(18) . . ?
C26 C25 C24 123.2(19) . . ?
N2 C39 C31 125.7(17) . . ?
N2 C39 C21 117.3(18) . . ?
C31 C39 C21 116.8(18) . . ?
C39 C31 C32 114.2(17) . . ?
C36 C32 C31 108.5(19) . . ?
C36 C32 C33 110(2) . . ?
C31 C32 C33 114.9(19) . . ?
C35 C33 C34 119(3) . . ?
C35 C33 C32 127(2) . . ?
C34 C33 C32 113(3) . . ?
C37 C36 C32 109.6(17) . . ?
C36 C37 C21 116.2(17) . . ?
N21 C21 C39 110.4(18) . . ?
N21 C21 C37 102.0(17) . . ?
C39 C21 C37 108.4(18) . . ?
N21 C21 C40 111.9(17) . . ?
C39 C21 C40 114.1(16) . . ?
C37 C21 C40 109(2) . . ?
N21 C46 C41 121(3) . . ?
N21 C46 C45 121(2) . . ?
C41 C46 C45 117(3) . . ?
C42 C41 C46 122(3) . . ?
C41 C42 C43 123(3) . . ?
C44 C43 C42 108(3) . . ?
C43 C44 C45 134(4) . . ?
C46 C45 C44 116(3) . . ?
C62 C61 C66 121(3) . . ?
C62 C61 C60 124(3) . . ?
C66 C61 C60 114(3) . . ?
C62 C61 K2 82.3(15) . . ?
C66 C61 K2 71.3(15) . . ?
C60 C61 K2 115.0(16) . . ?
C61 C62 C63 120(3) . . ?
C61 C62 K2 74.1(14) . . ?
C63 C62 K2 81(2) . . ?
C64 C63 C62 119(4) . . ?
C64 C63 K2 74(2) . . ?
C62 C63 K2 76.5(18) . . ?
C63 C64 C65 125(4) . . ?
C63 C64 K2 84(2) . . ?
C65 C64 K2 71.7(17) . . ?
C64 C65 C66 117(3) . . ?
C64 C65 K2 84.9(17) . . ?
C66 C65 K2 75.0(13) . . ?
C61 C66 C65 117(3) . . ?
C61 C66 K2 84.6(16) . . ?
C65 C66 K2 78.8(14) . . ?
C76 C71 C70 127(3) . . ?
C76 C71 C72 113(3) . . ?
C70 C71 C72 120(3) . . ?
C73 C72 C71 123(3) . . ?
C73 C72 K1 76.7(13) . . ?
C71 C72 K1 81.1(14) . . ?
C74 C73 C72 116(3) . . ?
C74 C73 K1 75.8(16) . . ?
C72 C73 K1 79.3(15) . . ?
C73 C74 C75 123(3) . . ?
C73 C74 K1 82.8(19) . . ?
C75 C74 K1 76.9(14) . . ?
C76 C75 C74 120(3) . . ?
C76 C75 K1 81.6(15) . . ?
C74 C75 K1 79.7(16) . . ?
C75 C76 C71 124(3) . . ?
C75 C76 K1 75.9(16) . . ?
C71 C76 K1 84.7(13) . . ?

_refine_diff_density_max         0.323
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_1S4R_1a
_database_code_depnum_ccdc_archive 'CCDC 1470030'
_audit_update_record             
;
2016-03-22 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H77 Al2 K2 N4 O2.C6 D6'
_chemical_formula_sum            'C58 H77 Al2 D6 K2 N4 O2'
_chemical_formula_weight         1006.48

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

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

_cell_length_a                   11.9997(17)
_cell_length_b                   32.297(9)
_cell_length_c                   15.606(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6048(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    47
_cell_measurement_theta_max      14.65
_cell_measurement_theta_min      3.142



_exptl_crystal_description       prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.32

_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_F_000             2156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_absorpt_coefficient_mu    0.226
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;

_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_T_max  1.716



_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a


_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'

_diffrn_reflns_number            55741
_diffrn_reflns_av_unetI/netI     0.0945
_diffrn_reflns_av_R_equivalents  0.1287
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.114
_diffrn_reflns_theta_max         23.520
_diffrn_reflns_theta_full        23.520
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             8910
_reflns_number_gt                6360
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    0.987

_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       '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-86 (Sheldrick, 1986)'

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'



_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)+(0.1456P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2077 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(4)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         8910
_refine_ls_number_parameters     567
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0790
_refine_ls_wR_factor_ref         0.2251
_refine_ls_wR_factor_gt          0.2060
_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



# 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 -0.030 0.000 0.133 378 45 ' '
2 0.029 0.500 0.867 378 45 ' '
_platon_squeeze_details          
;
 A molecule of deuterated benzene 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 
 their contribution to the structure factors.
;



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 0.22365(19) 0.21006(7) 0.72157(14) 0.0553(6) Uani 1 1 d . . . . .
Al2 Al 0.5857(2) 0.08568(8) 0.71421(16) 0.0650(7) Uani 1 1 d . . . . .
K1 K 0.52411(14) 0.19575(5) 0.70044(11) 0.0589(5) Uani 1 1 d . . . . .
K2 K 0.28801(16) 0.10056(6) 0.73843(14) 0.0731(6) Uani 1 1 d . . . . .
N1 N 0.4977(5) 0.13421(19) 0.5815(4) 0.0569(16) Uani 1 1 d . . . . .
N2 N 0.3910(5) 0.19430(18) 0.8426(4) 0.0511(14) Uani 1 1 d . . . . .
N11 N 0.5660(9) 0.1187(2) 0.3719(6) 0.081(2) Uani 1 1 d . . . . .
N21 N 0.4092(6) 0.24471(18) 1.0354(4) 0.0546(15) Uani 1 1 d . . . . .
O1 O 0.4724(4) 0.11141(16) 0.6559(3) 0.0569(13) Uani 1 1 d . . . . .
O2 O 0.3079(4) 0.17603(14) 0.7892(3) 0.0562(12) Uani 1 1 d . . . . .
C1 C 0.1692(8) 0.1705(3) 0.6316(5) 0.074(2) Uani 1 1 d . . . . .
C2 C 0.3197(7) 0.2543(3) 0.6701(6) 0.071(2) Uani 1 1 d . . . . .
C3 C 0.1030(7) 0.2336(3) 0.7943(6) 0.079(3) Uani 1 1 d . . . . .
H3A H 0.0563 0.2520 0.7596 0.118 Uiso 1 1 calc R U . . .
H3B H 0.0572 0.2110 0.8173 0.118 Uiso 1 1 calc R U . . .
H3C H 0.1360 0.2492 0.8417 0.118 Uiso 1 1 calc R U . . .
C4 C 0.6438(12) 0.0381(4) 0.6474(7) 0.108(4) Uani 1 1 d . . . . .
H4A H 0.7042 0.0248 0.6795 0.162 Uiso 1 1 calc R U . . .
H4B H 0.5837 0.0181 0.6377 0.162 Uiso 1 1 calc R U . . .
H4C H 0.6723 0.0480 0.5922 0.162 Uiso 1 1 calc R U . . .
C5 C 0.5101(10) 0.0703(4) 0.8238(7) 0.098(3) Uani 1 1 d . . . . .
C6 C 0.7047(8) 0.1282(3) 0.7336(8) 0.095(3) Uani 1 1 d . . . . .
C10 C 0.4713(7) 0.1166(2) 0.5112(5) 0.057(2) Uani 1 1 d . . . . .
C11 C 0.4894(8) 0.1413(3) 0.4299(5) 0.071(2) Uani 1 1 d . . . . .
C12 C 0.3770(10) 0.1428(3) 0.3835(6) 0.089(3) Uani 1 1 d . . . . .
H12A H 0.3255 0.1605 0.4169 0.107 Uiso 1 1 calc R U . . .
H12B H 0.3878 0.1560 0.3269 0.107 Uiso 1 1 calc R U . . .
C13 C 0.3233(9) 0.1014(3) 0.3702(6) 0.084(3) Uani 1 1 d . . . . .
H13A H 0.3704 0.0845 0.3318 0.100 Uiso 1 1 calc R U . . .
H13B H 0.2500 0.1053 0.3422 0.100 Uiso 1 1 calc R U . . .
C14 C 0.3073(8) 0.0786(3) 0.4553(6) 0.073(2) Uani 1 1 d . . . . .
H14 H 0.2592 0.0964 0.4925 0.088 Uiso 1 1 calc R U . . .
C15 C 0.4221(7) 0.0749(2) 0.4998(5) 0.061(2) Uani 1 1 d . . . . .
H15A H 0.4131 0.0614 0.5563 0.074 Uiso 1 1 calc R U . . .
H15B H 0.4724 0.0576 0.4646 0.074 Uiso 1 1 calc R U . . .
C16 C 0.2500(10) 0.0374(3) 0.4468(7) 0.090(3) Uani 1 1 d . . . . .
C17 C 0.3070(11) 0.0045(3) 0.3966(8) 0.110(4) Uani 1 1 d . . . . .
H17A H 0.2735 -0.0220 0.3907 0.132 Uiso 1 1 calc R U . . .
H17B H 0.3768 0.0100 0.3703 0.132 Uiso 1 1 calc R U . . .
C18 C 0.1474(13) 0.0302(4) 0.4861(9) 0.121(4) Uani 1 1 d . . . . .
H18A H 0.1233 0.0553 0.5161 0.181 Uiso 1 1 calc R U . . .
H18B H 0.0921 0.0228 0.4425 0.181 Uiso 1 1 calc R U . . .
H18C H 0.1548 0.0075 0.5273 0.181 Uiso 1 1 calc R U . . .
C20 C 0.3693(6) 0.1938(2) 0.9228(5) 0.0458(16) Uani 1 1 d . . . . .
C21 C 0.4592(6) 0.2115(2) 0.9814(5) 0.0503(17) Uani 1 1 d . . . . .
C22 C 0.4912(6) 0.1765(2) 1.0443(5) 0.0546(18) Uani 1 1 d . . . . .
H22A H 0.5293 0.1542 1.0120 0.066 Uiso 1 1 calc R U . . .
H22B H 0.5446 0.1875 1.0869 0.066 Uiso 1 1 calc R U . . .
C23 C 0.3924(7) 0.1582(2) 1.0910(5) 0.0559(19) Uani 1 1 d . . . . .
H23A H 0.3593 0.1797 1.1284 0.067 Uiso 1 1 calc R U . . .
H23B H 0.4186 0.1353 1.1282 0.067 Uiso 1 1 calc R U . . .
C24 C 0.3020(6) 0.1416(2) 1.0301(5) 0.0507(18) Uani 1 1 d . . . . .
H24 H 0.3377 0.1191 0.9957 0.061 Uiso 1 1 calc R U . . .
C25 C 0.2692(6) 0.1759(2) 0.9661(4) 0.0456(16) Uani 1 1 d . . . . .
H25A H 0.2183 0.1643 0.9223 0.055 Uiso 1 1 calc R U . . .
H25B H 0.2290 0.1981 0.9969 0.055 Uiso 1 1 calc R U . . .
C26 C 0.2093(8) 0.1224(2) 1.0764(5) 0.063(2) Uani 1 1 d . . . . .
C27 C 0.2332(10) 0.0840(3) 1.1276(7) 0.096(3) Uani 1 1 d . . . . .
H27A H 0.3115 0.0762 1.1201 0.143 Uiso 1 1 calc R U . . .
H27B H 0.2185 0.0894 1.1883 0.143 Uiso 1 1 calc R U . . .
H27C H 0.1853 0.0615 1.1076 0.143 Uiso 1 1 calc R U . . .
C28 C 0.1072(10) 0.1381(3) 1.0781(6) 0.083(3) Uani 1 1 d . . . . .
H28A H 0.0911 0.1630 1.0482 0.099 Uiso 1 1 calc R U . . .
H28B H 0.0500 0.1243 1.1093 0.099 Uiso 1 1 calc R U . . .
C30 C 0.5326(11) 0.1858(3) 0.4445(6) 0.087(3) Uani 1 1 d . . . . .
H30A H 0.4815 0.2005 0.4829 0.131 Uiso 1 1 calc R U . . .
H30B H 0.6069 0.1847 0.4705 0.131 Uiso 1 1 calc R U . . .
H30C H 0.5367 0.2003 0.3895 0.131 Uiso 1 1 calc R U . . .
C31 C 0.6830(10) 0.1173(2) 0.3861(6) 0.077(3) Uani 1 1 d . . . . .
C32 C 0.7496(13) 0.1142(3) 0.3160(9) 0.105(4) Uani 1 1 d . . . . .
H32 H 0.7173 0.1147 0.2604 0.126 Uiso 1 1 calc R U . . .
C33 C 0.864(2) 0.1105(5) 0.3247(13) 0.156(8) Uani 1 1 d . . . . .
H33 H 0.9093 0.1103 0.2749 0.187 Uiso 1 1 calc R U . . .
C34 C 0.9109(12) 0.1072(4) 0.4025(13) 0.125(5) Uani 1 1 d . . . . .
H34 H 0.9892 0.1038 0.4080 0.150 Uiso 1 1 calc R U . . .
C35 C 0.8463(12) 0.1088(4) 0.4716(10) 0.121(4) Uani 1 1 d . . . . .
H35 H 0.8788 0.1064 0.5269 0.145 Uiso 1 1 calc R U . . .
C36 C 0.7326(11) 0.1140(4) 0.4640(8) 0.112(4) Uani 1 1 d . . . . .
H36 H 0.6881 0.1153 0.5142 0.134 Uiso 1 1 calc R U . . .
C40 C 0.5618(7) 0.2262(3) 0.9335(6) 0.066(2) Uani 1 1 d . . . . .
H40A H 0.5916 0.2034 0.8990 0.099 Uiso 1 1 calc R U . . .
H40B H 0.5416 0.2493 0.8959 0.099 Uiso 1 1 calc R U . . .
H40C H 0.6183 0.2354 0.9746 0.099 Uiso 1 1 calc R U . . .
C41 C 0.3741(6) 0.2828(2) 1.0029(5) 0.0516(18) Uani 1 1 d . . . . .
C42 C 0.3485(7) 0.2899(2) 0.9170(6) 0.062(2) Uani 1 1 d . . . . .
H42 H 0.3604 0.2687 0.8758 0.075 Uiso 1 1 calc R U . . .
C43 C 0.3059(8) 0.3277(3) 0.8916(6) 0.073(2) Uani 1 1 d . . . . .
H43 H 0.2867 0.3318 0.8332 0.087 Uiso 1 1 calc R U . . .
C44 C 0.2907(8) 0.3593(3) 0.9482(7) 0.081(3) Uani 1 1 d . . . . .
H44 H 0.2640 0.3855 0.9292 0.097 Uiso 1 1 calc R U . . .
C45 C 0.3148(8) 0.3528(2) 1.0345(7) 0.069(2) Uani 1 1 d . . . . .
H45 H 0.3030 0.3744 1.0749 0.083 Uiso 1 1 calc R U . . .
C46 C 0.3560(7) 0.3150(2) 1.0616(5) 0.060(2) Uani 1 1 d . . . . .
H46 H 0.3721 0.3108 1.1205 0.072 Uiso 1 1 calc R U . . .
C60 C 0.1435(9) 0.0296(3) 0.8327(8) 0.086(3) Uani 1 1 d . . . . .
C61 C 0.1047(9) 0.0314(3) 0.7489(8) 0.089(3) Uani 1 1 d . . . . .
H61 H 0.1225 0.0103 0.7088 0.107 Uiso 1 1 calc R U . . .
C62 C 0.0400(9) 0.0646(4) 0.7257(8) 0.092(3) Uani 1 1 d . . . . .
H62 H 0.0108 0.0665 0.6692 0.110 Uiso 1 1 calc R U . . .
C63 C 0.0177(9) 0.0951(3) 0.7843(9) 0.093(3) Uani 1 1 d . . . . .
H63 H -0.0275 0.1181 0.7687 0.111 Uiso 1 1 calc R U . . .
C64 C 0.0590(10) 0.0927(4) 0.8622(9) 0.097(3) Uani 1 1 d . . . . .
H64 H 0.0442 0.1145 0.9014 0.117 Uiso 1 1 calc R U . . .
C65 C 0.1197(10) 0.0613(3) 0.8879(8) 0.086(3) Uani 1 1 d . . . . .
H65 H 0.1473 0.0606 0.9449 0.104 Uiso 1 1 calc R U . . .
C66 C 0.2117(16) -0.0072(4) 0.8646(10) 0.146(6) Uani 1 1 d . . . . .
H66A H 0.2215 -0.0272 0.8178 0.219 Uiso 1 1 calc R U . . .
H66B H 0.2848 0.0024 0.8841 0.219 Uiso 1 1 calc R U . . .
H66C H 0.1726 -0.0206 0.9122 0.219 Uiso 1 1 calc R U . . .
C70 C 0.7703(8) 0.2414(3) 0.6268(6) 0.076(3) Uani 1 1 d . . . . .
C71 C 0.6902(9) 0.2613(3) 0.5791(6) 0.074(2) Uani 1 1 d . . . . .
H71 H 0.6856 0.2569 0.5190 0.089 Uiso 1 1 calc R U . . .
C72 C 0.6189(10) 0.2869(3) 0.6180(9) 0.092(3) Uani 1 1 d . . . . .
H72 H 0.5630 0.2998 0.5842 0.110 Uiso 1 1 calc R U . . .
C73 C 0.6217(13) 0.2952(4) 0.7005(12) 0.117(4) Uani 1 1 d . . . . .
H73 H 0.5697 0.3144 0.7235 0.140 Uiso 1 1 calc R U . . .
C74 C 0.6937(15) 0.2778(5) 0.7516(10) 0.117(5) Uani 1 1 d . . . . .
H74 H 0.6940 0.2836 0.8113 0.141 Uiso 1 1 calc R U . . .
C75 C 0.7720(11) 0.2497(4) 0.7150(8) 0.110(5) Uani 1 1 d . . . . .
H75 H 0.8257 0.2365 0.7506 0.132 Uiso 1 1 calc R U . . .
C76 C 0.8547(13) 0.2145(4) 0.5863(11) 0.135(5) Uani 1 1 d . . . . .
H76A H 0.9041 0.2031 0.6304 0.202 Uiso 1 1 calc R U . . .
H76B H 0.8173 0.1917 0.5562 0.202 Uiso 1 1 calc R U . . .
H76C H 0.8985 0.2307 0.5453 0.202 Uiso 1 1 calc R U . . .
H1 H 0.465(7) 0.258(2) 1.076(5) 0.06(2) Uiso 1 1 d . . . . .
H2 H 0.533(7) 0.123(2) 0.321(6) 0.06(2) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 O2 1.828(6) . ?
Al1 C3 1.990(9) . ?
Al1 C2 2.003(9) . ?
Al1 C1 2.007(9) . ?
Al1 K2 3.629(3) . ?
Al1 K1 3.650(3) . ?
Al2 O1 1.835(6) . ?
Al2 C5 1.999(11) . ?
Al2 C4 1.983(10) . ?
Al2 C6 2.005(11) . ?
Al2 K2 3.624(3) . ?
Al2 K1 3.637(3) . ?
K1 N2 2.734(6) . ?
K1 N1 2.738(6) . ?
K1 O1 2.879(5) . ?
K1 O2 3.009(5) . ?
K1 C6 3.117(10) . ?
K1 C2 3.132(9) . ?
K1 C72 3.408(10) . ?
K1 C73 3.418(11) . ?
K1 C74 3.435(12) . ?
K1 C75 3.455(10) . ?
K1 C71 3.470(9) . ?
K1 C70 3.496(9) . ?
K2 O2 2.574(5) . ?
K2 O1 2.583(5) . ?
K2 C5 3.135(12) . ?
K2 C61 3.138(9) . ?
K2 C1 3.150(9) . ?
K2 C62 3.200(10) . ?
K2 C60 3.229(10) . ?
K2 C65 3.336(11) . ?
K2 C63 3.326(11) . ?
K2 C64 3.369(11) . ?
N1 C10 1.277(9) . ?
N1 O1 1.408(8) . ?
N2 C20 1.279(9) . ?
N2 O2 1.427(8) . ?
N11 C31 1.422(15) . ?
N11 C11 1.482(12) . ?
N21 C41 1.396(9) . ?
N21 C21 1.489(9) . ?
C10 C15 1.481(12) . ?
C10 C11 1.514(12) . ?
C11 C12 1.532(15) . ?
C11 C30 1.545(13) . ?
C12 C13 1.497(15) . ?
C13 C14 1.531(14) . ?
C14 C16 1.504(14) . ?
C14 C15 1.547(13) . ?
C16 C18 1.395(18) . ?
C16 C17 1.485(15) . ?
C20 C25 1.493(10) . ?
C20 C21 1.526(10) . ?
C21 C40 1.517(11) . ?
C21 C22 1.546(10) . ?
C22 C23 1.512(11) . ?
C23 C24 1.539(11) . ?
C24 C26 1.463(11) . ?
C24 C25 1.543(10) . ?
C26 C28 1.326(14) . ?
C26 C27 1.502(13) . ?
C31 C36 1.357(16) . ?
C31 C32 1.358(15) . ?
C32 C33 1.38(3) . ?
C33 C34 1.35(2) . ?
C34 C35 1.33(2) . ?
C35 C36 1.380(18) . ?
C41 C42 1.394(11) . ?
C41 C46 1.403(11) . ?
C42 C43 1.381(11) . ?
C43 C44 1.363(13) . ?
C44 C45 1.393(14) . ?
C45 C46 1.382(11) . ?
C60 C65 1.368(14) . ?
C60 C61 1.389(16) . ?
C60 C66 1.528(17) . ?
C61 C62 1.373(15) . ?
C62 C63 1.371(16) . ?
C63 C64 1.314(16) . ?
C64 C65 1.312(16) . ?
C70 C71 1.377(14) . ?
C70 C75 1.402(16) . ?
C70 C76 1.476(17) . ?
C71 C72 1.335(15) . ?
C72 C73 1.316(18) . ?
C73 C74 1.30(2) . ?
C74 C75 1.43(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Al1 C3 107.6(3) . . ?
O2 Al1 C2 110.0(3) . . ?
C3 Al1 C2 112.1(4) . . ?
O2 Al1 C1 101.6(3) . . ?
C3 Al1 C1 113.9(4) . . ?
C2 Al1 C1 111.1(4) . . ?
O2 Al1 K2 41.83(15) . . ?
C3 Al1 K2 119.0(3) . . ?
C2 Al1 K2 126.9(3) . . ?
C1 Al1 K2 60.0(3) . . ?
O2 Al1 K1 55.24(17) . . ?
C3 Al1 K1 144.9(3) . . ?
C2 Al1 K1 59.0(3) . . ?
C1 Al1 K1 100.2(3) . . ?
K2 Al1 K1 70.91(6) . . ?
O1 Al2 C5 101.5(4) . . ?
O1 Al2 C4 110.6(4) . . ?
C5 Al2 C4 114.7(5) . . ?
O1 Al2 C6 107.0(4) . . ?
C5 Al2 C6 111.3(5) . . ?
C4 Al2 C6 111.1(6) . . ?
O1 Al2 K2 42.36(17) . . ?
C5 Al2 K2 59.7(3) . . ?
C4 Al2 K2 120.3(4) . . ?
C6 Al2 K2 126.5(3) . . ?
O1 Al2 K1 51.50(17) . . ?
C5 Al2 K1 101.6(4) . . ?
C4 Al2 K1 142.9(4) . . ?
C6 Al2 K1 58.9(3) . . ?
K2 Al2 K1 71.11(6) . . ?
N2 K1 N1 118.0(2) . . ?
N2 K1 O1 93.07(17) . . ?
N1 K1 O1 28.90(17) . . ?
N2 K1 O2 28.25(15) . . ?
N1 K1 O2 93.35(17) . . ?
O1 K1 O2 74.03(14) . . ?
N2 K1 C6 105.0(3) . . ?
N1 K1 C6 71.7(2) . . ?
O1 K1 C6 61.8(2) . . ?
O2 K1 C6 112.0(2) . . ?
N2 K1 C2 71.0(2) . . ?
N1 K1 C2 104.2(2) . . ?
O1 K1 C2 111.4(2) . . ?
O2 K1 C2 61.44(19) . . ?
C6 K1 C2 172.5(3) . . ?
N2 K1 C72 121.1(3) . . ?
N1 K1 C72 114.2(3) . . ?
O1 K1 C72 143.0(3) . . ?
O2 K1 C72 130.1(2) . . ?
C6 K1 C72 115.8(3) . . ?
C2 K1 C72 71.5(3) . . ?
N2 K1 C73 102.5(3) . . ?
N1 K1 C73 136.2(3) . . ?
O1 K1 C73 164.3(3) . . ?
O2 K1 C73 119.6(3) . . ?
C6 K1 C73 114.8(4) . . ?
C2 K1 C73 72.6(4) . . ?
C72 K1 C73 22.2(3) . . ?
N2 K1 C74 99.8(3) . . ?
N1 K1 C74 141.8(3) . . ?
O1 K1 C74 156.0(4) . . ?
O2 K1 C74 124.5(3) . . ?
C6 K1 C74 95.1(4) . . ?
C2 K1 C74 91.9(4) . . ?
C72 K1 C74 39.1(4) . . ?
C73 K1 C74 21.9(3) . . ?
N2 K1 C75 117.3(3) . . ?
N1 K1 C75 120.7(3) . . ?
O1 K1 C75 132.7(3) . . ?
O2 K1 C75 145.0(3) . . ?
C6 K1 C75 75.1(3) . . ?
C2 K1 C75 112.3(3) . . ?
C72 K1 C75 45.7(3) . . ?
C73 K1 C75 39.8(4) . . ?
C74 K1 C75 23.9(3) . . ?
N2 K1 C71 142.1(2) . . ?
N1 K1 C71 98.0(2) . . ?
O1 K1 C71 124.7(2) . . ?
O2 K1 C71 151.1(2) . . ?
C6 K1 C71 96.8(3) . . ?
C2 K1 C71 89.9(2) . . ?
C72 K1 C71 22.4(3) . . ?
C73 K1 C71 39.7(3) . . ?
C74 K1 C71 46.8(3) . . ?
C75 K1 C71 40.0(2) . . ?
N2 K1 C70 140.2(2) . . ?
N1 K1 C70 100.4(2) . . ?
O1 K1 C70 120.1(2) . . ?
O2 K1 C70 165.7(2) . . ?
C6 K1 C70 76.2(3) . . ?
C2 K1 C70 111.0(2) . . ?
C72 K1 C70 39.6(3) . . ?
C73 K1 C70 46.7(3) . . ?
C74 K1 C70 41.5(3) . . ?
C75 K1 C70 23.3(3) . . ?
C71 K1 C70 22.8(2) . . ?
O2 K2 O1 86.87(17) . . ?
O2 K2 C5 94.9(3) . . ?
O1 K2 C5 61.7(2) . . ?
O2 K2 C61 136.3(2) . . ?
O1 K2 C61 136.3(2) . . ?
C5 K2 C61 110.6(3) . . ?
O2 K2 C1 61.7(2) . . ?
O1 K2 C1 91.5(2) . . ?
C5 K2 C1 146.4(3) . . ?
C61 K2 C1 102.8(3) . . ?
O2 K2 C62 116.6(3) . . ?
O1 K2 C62 144.5(3) . . ?
C5 K2 C62 134.8(3) . . ?
C61 K2 C62 25.0(3) . . ?
C1 K2 C62 78.8(3) . . ?
O2 K2 C60 125.6(2) . . ?
O1 K2 C60 141.6(2) . . ?
C5 K2 C60 92.4(3) . . ?
C61 K2 C60 25.2(3) . . ?
C1 K2 C60 120.5(3) . . ?
C62 K2 C60 43.2(3) . . ?
O2 K2 C65 101.6(2) . . ?
O1 K2 C65 156.7(3) . . ?
C5 K2 C65 95.7(3) . . ?
C61 K2 C65 43.0(3) . . ?
C1 K2 C65 111.7(3) . . ?
C62 K2 C65 48.9(3) . . ?
C60 K2 C65 24.0(3) . . ?
O2 K2 C63 94.2(2) . . ?
O1 K2 C63 161.7(3) . . ?
C5 K2 C63 136.1(3) . . ?
C61 K2 C63 43.0(3) . . ?
C1 K2 C63 73.2(3) . . ?
C62 K2 C63 24.2(3) . . ?
C60 K2 C63 48.8(3) . . ?
C65 K2 C63 40.5(3) . . ?
O2 K2 C64 88.3(2) . . ?
O1 K2 C64 174.0(3) . . ?
C5 K2 C64 115.2(3) . . ?
C61 K2 C64 49.1(3) . . ?
C1 K2 C64 89.3(3) . . ?
C62 K2 C64 41.4(3) . . ?
C60 K2 C64 41.1(3) . . ?
C65 K2 C64 22.6(3) . . ?
C63 K2 C64 22.6(3) . . ?
O2 K2 Al2 93.80(14) . . ?
O1 K2 Al2 28.60(12) . . ?
C5 K2 Al2 33.4(2) . . ?
C61 K2 Al2 127.0(2) . . ?
C1 K2 Al2 119.1(2) . . ?
C62 K2 Al2 149.6(2) . . ?
C60 K2 Al2 118.9(2) . . ?
C65 K2 Al2 128.3(2) . . ?
C63 K2 Al2 167.6(2) . . ?
C64 K2 Al2 148.6(3) . . ?
O2 K2 Al1 28.27(12) . . ?
O1 K2 Al1 90.79(12) . . ?
C5 K2 Al1 121.0(3) . . ?
C61 K2 Al1 123.2(2) . . ?
C1 K2 Al1 33.50(16) . . ?
C62 K2 Al1 98.7(2) . . ?
C60 K2 Al1 127.6(2) . . ?
C65 K2 Al1 106.99(19) . . ?
C63 K2 Al1 81.9(2) . . ?
C64 K2 Al1 86.6(2) . . ?
Al2 K2 Al1 109.35(7) . . ?
C10 N1 O1 115.0(6) . . ?
C10 N1 K1 159.3(5) . . ?
O1 N1 K1 81.1(3) . . ?
C20 N2 O2 115.1(6) . . ?
C20 N2 K1 156.0(5) . . ?
O2 N2 K1 86.7(3) . . ?
C31 N11 C11 122.2(8) . . ?
C41 N21 C21 123.5(6) . . ?
N1 O1 Al2 119.0(4) . . ?
N1 O1 K2 131.8(4) . . ?
Al2 O1 K2 109.0(2) . . ?
N1 O1 K1 70.0(3) . . ?
Al2 O1 K1 98.6(2) . . ?
K2 O1 K1 101.12(17) . . ?
N2 O2 Al1 118.3(4) . . ?
N2 O2 K2 129.5(4) . . ?
Al1 O2 K2 109.9(2) . . ?
N2 O2 K1 65.1(3) . . ?
Al1 O2 K1 94.8(2) . . ?
K2 O2 K1 97.97(16) . . ?
Al1 C1 K2 86.5(3) . . ?
Al1 C2 K1 87.7(3) . . ?
Al2 C5 K2 86.9(4) . . ?
Al2 C6 K1 87.7(3) . . ?
N1 C10 C15 127.4(7) . . ?
N1 C10 C11 116.8(7) . . ?
C15 C10 C11 115.8(7) . . ?
N11 C11 C12 105.9(7) . . ?
N11 C11 C10 109.9(6) . . ?
C12 C11 C10 106.6(8) . . ?
N11 C11 C30 109.9(9) . . ?
C12 C11 C30 109.6(8) . . ?
C10 C11 C30 114.4(7) . . ?
C13 C12 C11 114.6(7) . . ?
C12 C13 C14 111.3(8) . . ?
C16 C14 C13 114.0(8) . . ?
C16 C14 C15 112.2(7) . . ?
C13 C14 C15 108.3(8) . . ?
C10 C15 C14 109.8(6) . . ?
C18 C16 C17 121.3(11) . . ?
C18 C16 C14 120.8(10) . . ?
C17 C16 C14 118.0(10) . . ?
N2 C20 C25 127.7(6) . . ?
N2 C20 C21 116.0(6) . . ?
C25 C20 C21 116.2(6) . . ?
N21 C21 C40 112.4(6) . . ?
N21 C21 C20 109.0(6) . . ?
C40 C21 C20 113.3(6) . . ?
N21 C21 C22 105.6(6) . . ?
C40 C21 C22 109.9(6) . . ?
C20 C21 C22 106.3(6) . . ?
C23 C22 C21 113.4(6) . . ?
C22 C23 C24 113.0(6) . . ?
C26 C24 C23 112.2(6) . . ?
C26 C24 C25 115.4(6) . . ?
C23 C24 C25 109.2(6) . . ?
C20 C25 C24 111.4(6) . . ?
C28 C26 C24 123.5(8) . . ?
C28 C26 C27 118.7(9) . . ?
C24 C26 C27 117.8(8) . . ?
C36 C31 C32 117.3(12) . . ?
C36 C31 N11 125.0(10) . . ?
C32 C31 N11 117.3(10) . . ?
C31 C32 C33 120.7(15) . . ?
C34 C33 C32 120.9(15) . . ?
C35 C34 C33 118.9(15) . . ?
C34 C35 C36 120.8(15) . . ?
C31 C36 C35 121.3(13) . . ?
C42 C41 N21 124.1(7) . . ?
C42 C41 C46 118.1(7) . . ?
N21 C41 C46 117.6(7) . . ?
C43 C42 C41 120.2(8) . . ?
C44 C43 C42 121.7(9) . . ?
C43 C44 C45 119.0(8) . . ?
C46 C45 C44 120.3(8) . . ?
C45 C46 C41 120.7(8) . . ?
C65 C60 C61 119.5(10) . . ?
C65 C60 C66 119.3(12) . . ?
C61 C60 C66 121.3(11) . . ?
C65 C60 K2 82.4(6) . . ?
C61 C60 K2 73.8(6) . . ?
C66 C60 K2 114.4(8) . . ?
C62 C61 C60 118.1(10) . . ?
C62 C61 K2 80.0(5) . . ?
C60 C61 K2 81.1(6) . . ?
C63 C62 C61 119.7(12) . . ?
C63 C62 K2 83.1(6) . . ?
C61 C62 K2 75.0(6) . . ?
C64 C63 C62 120.0(11) . . ?
C64 C63 K2 80.5(7) . . ?
C62 C63 K2 72.8(6) . . ?
C63 C64 C65 122.6(11) . . ?
C63 C64 K2 76.9(7) . . ?
C65 C64 K2 77.3(7) . . ?
C64 C65 C60 120.1(12) . . ?
C64 C65 K2 80.1(7) . . ?
C60 C65 K2 73.6(6) . . ?
C71 C70 C75 116.9(11) . . ?
C71 C70 C76 121.5(11) . . ?
C75 C70 C76 121.5(12) . . ?
C71 C70 K1 77.6(5) . . ?
C75 C70 K1 76.7(6) . . ?
C76 C70 K1 118.2(7) . . ?
C72 C71 C70 119.4(10) . . ?
C72 C71 K1 76.2(6) . . ?
C70 C71 K1 79.7(5) . . ?
C73 C72 C71 123.7(14) . . ?
C73 C72 K1 79.3(7) . . ?
C71 C72 K1 81.4(6) . . ?
C72 C73 C74 121.9(15) . . ?
C72 C73 K1 78.5(7) . . ?
C74 C73 K1 79.8(8) . . ?
C73 C74 C75 117.8(13) . . ?
C73 C74 K1 78.3(7) . . ?
C75 C74 K1 78.8(6) . . ?
C70 C75 C74 120.4(11) . . ?
C70 C75 K1 80.0(6) . . ?
C74 C75 K1 77.3(6) . . ?

_refine_diff_density_max         0.318
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.068

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

data_1S4R_1c
_database_code_depnum_ccdc_archive 'CCDC 1470031'
_audit_update_record             
;
2016-03-22 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H60 Al2 D12 K2 N4 O2.0.5C6 D6.0.5C7 H8'
_chemical_formula_sum            'C56.50 H64 Al2 D15 K2 N4 O2'
_chemical_formula_weight         993.48

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

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

_cell_length_a                   31.579(5)
_cell_length_b                   11.8642(11)
_cell_length_c                   15.4746(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5797.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    189
_cell_measurement_theta_max      19.35
_cell_measurement_theta_min      3.07

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.42
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_F_000             2104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_absorpt_coefficient_mu    0.235
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

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

_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_T_max  1.719


_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'

_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            66701
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.099
_diffrn_reflns_theta_max         26.899
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             12414
_reflns_number_gt                9185
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_max     0.983
_reflns_Friedel_fraction_full    0.986

_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       '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-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


_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)+(0.0819P)²+0.5374P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2934 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         12414
_refine_ls_number_parameters     624
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.1540
_refine_ls_wR_factor_gt          0.1398
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



# 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 0.596 193 21 ' '
2 0.500 0.500 0.404 193 21 ' '
_platon_squeeze_details          
;
 A molecule of toluene crystallized with every two molecules 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 
 their contribution to the structure factors.
;

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 0.21175(5) 0.27365(10) 0.21884(8) 0.0471(3) Uani 1 1 d . . . . .
Al2 Al 0.08423(5) -0.09793(12) 0.20337(9) 0.0519(3) Uani 1 1 d . . . . .
K1 K 0.19568(3) -0.03357(7) 0.19665(6) 0.0451(2) Uani 1 1 d . . . . .
K2 K 0.09865(4) 0.20240(9) 0.23583(9) 0.0703(4) Uani 1 1 d . . . . .
N1 N 0.13454(11) -0.0044(3) 0.0750(2) 0.0410(8) Uani 1 1 d . . . . .
N2 N 0.19419(12) 0.1040(3) 0.3383(2) 0.0463(8) Uani 1 1 d . . . . .
N11 N 0.11806(13) -0.0738(4) -0.1334(3) 0.0568(10) Uani 1 1 d . . . . .
N21 N 0.24312(11) 0.0753(3) 0.5342(2) 0.0446(8) Uani 1 1 d . . . . .
O1 O 0.11150(9) 0.0197(2) 0.15097(17) 0.0442(6) Uani 1 1 d . . . . .
O2 O 0.17597(10) 0.1887(2) 0.28553(18) 0.0499(7) Uani 1 1 d . . . . .
C1 C 0.1718(3) 0.3462(7) 0.1373(5) 0.0767(18) Uani 1 1 d . . . . .
C2 C 0.2526(2) 0.1755(5) 0.1590(4) 0.0596(13) Uani 1 1 d . . . . .
C3 C 0.2395(2) 0.3838(4) 0.2950(3) 0.0732(16) Uani 1 1 d . . . . .
H3A H 0.2589 0.4306 0.2610 0.110 Uiso 1 1 calc R U . . .
H3B H 0.2179 0.4317 0.3220 0.110 Uiso 1 1 calc R U . . .
H3C H 0.2554 0.3439 0.3399 0.110 Uiso 1 1 calc R U . . .
C4 C 0.0360(2) -0.1463(7) 0.1317(4) 0.093(2) Uani 1 1 d . . . . .
H4A H 0.0214 -0.2093 0.1599 0.139 Uiso 1 1 calc R U . . .
H4B H 0.0162 -0.0833 0.1246 0.139 Uiso 1 1 calc R U . . .
H4C H 0.0463 -0.1704 0.0749 0.139 Uiso 1 1 calc R U . . .
C5 C 0.0683(3) -0.0300(7) 0.3158(4) 0.0851(19) Uani 1 1 d . . . . .
C6 C 0.1253(2) -0.2223(5) 0.2209(5) 0.0788(18) Uani 1 1 d . . . . .
C10 C 0.11695(12) 0.0255(3) 0.0039(2) 0.0382(9) Uani 1 1 d . . . . .
C11 C 0.14192(13) 0.0043(4) -0.0788(3) 0.0442(10) Uani 1 1 d . . . . .
C12 C 0.14389(15) 0.1179(5) -0.1268(3) 0.0572(12) Uani 1 1 d . . . . .
H12A H 0.1629 0.1693 -0.0945 0.069 Uiso 1 1 calc R U . . .
H12B H 0.1566 0.1053 -0.1845 0.069 Uiso 1 1 calc R U . . .
C13 C 0.10130(15) 0.1757(4) -0.1387(3) 0.0556(12) Uani 1 1 d . . . . .
H13A H 0.0828 0.1280 -0.1752 0.067 Uiso 1 1 calc R U . . .
H13B H 0.1054 0.2486 -0.1686 0.067 Uiso 1 1 calc R U . . .
C14 C 0.08011(15) 0.1956(4) -0.0517(3) 0.0495(10) Uani 1 1 d . . . . .
H14 H 0.0997 0.2428 -0.0160 0.059 Uiso 1 1 calc R U . . .
C15 C 0.07483(13) 0.0811(3) -0.0056(3) 0.0423(9) Uani 1 1 d . . . . .
H15A H 0.0620 0.0927 0.0520 0.051 Uiso 1 1 calc R U . . .
H15B H 0.0557 0.0321 -0.0397 0.051 Uiso 1 1 calc R U . . .
C16 C 0.03793(16) 0.2581(4) -0.0581(3) 0.0591(12) Uani 1 1 d . . . . .
C17 C 0.00347(18) 0.2062(6) -0.1090(4) 0.0823(18) Uani 1 1 d . . . . .
H17A H 0.0131 0.1338 -0.1324 0.123 Uiso 1 1 calc R U . . .
H17B H -0.0212 0.1938 -0.0717 0.123 Uiso 1 1 calc R U . . .
H17C H -0.0044 0.2564 -0.1567 0.123 Uiso 1 1 calc R U . . .
C18 C 0.0331(2) 0.3559(5) -0.0197(5) 0.0896(19) Uani 1 1 d . . . . .
H18A H 0.0070 0.3951 -0.0242 0.108 Uiso 1 1 calc R U . . .
H18B H 0.0558 0.3874 0.0127 0.108 Uiso 1 1 calc R U . . .
C20 C 0.19271(13) 0.1221(3) 0.4189(2) 0.0392(9) Uani 1 1 d . . . . .
C21 C 0.20983(14) 0.0289(3) 0.4774(3) 0.0430(9) Uani 1 1 d . . . . .
C22 C 0.17263(15) -0.0046(4) 0.5371(3) 0.0486(10) Uani 1 1 d . . . . .
H22A H 0.1503 -0.0406 0.5017 0.058 Uiso 1 1 calc R U . . .
H22B H 0.1828 -0.0612 0.5792 0.058 Uiso 1 1 calc R U . . .
C23 C 0.15344(14) 0.0922(4) 0.5857(3) 0.0469(10) Uani 1 1 d . . . . .
H23A H 0.1747 0.1232 0.6263 0.056 Uiso 1 1 calc R U . . .
H23B H 0.1292 0.0644 0.6202 0.056 Uiso 1 1 calc R U . . .
C24 C 0.13808(14) 0.1871(3) 0.5250(3) 0.0423(9) Uani 1 1 d . . . . .
H24 H 0.1152 0.1545 0.4878 0.051 Uiso 1 1 calc R U . . .
C25 C 0.17435(14) 0.2217(3) 0.4651(3) 0.0413(9) Uani 1 1 d . . . . .
H25A H 0.1637 0.2767 0.4221 0.050 Uiso 1 1 calc R U . . .
H25B H 0.1968 0.2589 0.4994 0.050 Uiso 1 1 calc R U . . .
C26 C 0.11864(15) 0.2819(4) 0.5758(3) 0.0506(10) Uani 1 1 d . . . . .
C27 C 0.07747(19) 0.2562(5) 0.6209(4) 0.0744(15) Uani 1 1 d . . . . .
H27A H 0.0697 0.1774 0.6106 0.112 Uiso 1 1 calc R U . . .
H27B H 0.0808 0.2688 0.6832 0.112 Uiso 1 1 calc R U . . .
H27C H 0.0552 0.3056 0.5984 0.112 Uiso 1 1 calc R U . . .
C28 C 0.13556(18) 0.3841(4) 0.5806(3) 0.0625(13) Uani 1 1 d . . . . .
H28A H 0.1612 0.4002 0.5511 0.075 Uiso 1 1 calc R U . . .
H28B H 0.1220 0.4412 0.6136 0.075 Uiso 1 1 calc R U . . .
C30 C 0.18718(14) -0.0363(5) -0.0627(3) 0.0573(12) Uani 1 1 d . . . . .
H30A H 0.2020 0.0182 -0.0260 0.086 Uiso 1 1 calc R U . . .
H30B H 0.1865 -0.1098 -0.0339 0.086 Uiso 1 1 calc R U . . .
H30C H 0.2021 -0.0432 -0.1180 0.086 Uiso 1 1 calc R U . . .
C31 C 0.11718(13) -0.1902(4) -0.1213(3) 0.0521(11) Uani 1 1 d . . . . .
C32 C 0.11319(15) -0.2593(5) -0.1926(4) 0.0667(14) Uani 1 1 d . . . . .
H32 H 0.1119 -0.2272 -0.2488 0.080 Uiso 1 1 calc R U . . .
C33 C 0.1111(2) -0.3753(6) -0.1824(5) 0.087(2) Uani 1 1 d . . . . .
H33 H 0.1091 -0.4215 -0.2324 0.104 Uiso 1 1 calc R U . . .
C34 C 0.1117(2) -0.4243(5) -0.1043(5) 0.087(2) Uani 1 1 d . . . . .
H34 H 0.1095 -0.5038 -0.0989 0.105 Uiso 1 1 calc R U . . .
C35 C 0.1157(2) -0.3576(5) -0.0326(5) 0.0868(19) Uani 1 1 d . . . . .
H35 H 0.1165 -0.3913 0.0231 0.104 Uiso 1 1 calc R U . . .
C36 C 0.1185(2) -0.2404(4) -0.0404(4) 0.0722(15) Uani 1 1 d . . . . .
H36 H 0.1213 -0.1951 0.0098 0.087 Uiso 1 1 calc R U . . .
C40 C 0.22492(18) -0.0754(4) 0.4285(3) 0.0589(12) Uani 1 1 d . . . . .
H40A H 0.2020 -0.1035 0.3916 0.088 Uiso 1 1 calc R U . . .
H40B H 0.2494 -0.0557 0.3925 0.088 Uiso 1 1 calc R U . . .
H40C H 0.2331 -0.1341 0.4699 0.088 Uiso 1 1 calc R U . . .
C41 C 0.28256(14) 0.1115(3) 0.5062(3) 0.0425(9) Uani 1 1 d . . . . .
C42 C 0.29142(15) 0.1406(4) 0.4207(3) 0.0508(11) Uani 1 1 d . . . . .
H42 H 0.2702 0.1317 0.3778 0.061 Uiso 1 1 calc R U . . .
C43 C 0.33030(17) 0.1819(4) 0.3980(4) 0.0629(13) Uani 1 1 d . . . . .
H43 H 0.3355 0.2012 0.3394 0.075 Uiso 1 1 calc R U . . .
C44 C 0.36183(18) 0.1959(4) 0.4576(4) 0.0708(16) Uani 1 1 d . . . . .
H44 H 0.3887 0.2245 0.4408 0.085 Uiso 1 1 calc R U . . .
C45 C 0.35384(16) 0.1676(4) 0.5434(4) 0.0620(13) Uani 1 1 d . . . . .
H45 H 0.3752 0.1772 0.5860 0.074 Uiso 1 1 calc R U . . .
C46 C 0.31472(14) 0.1255(4) 0.5662(3) 0.0520(11) Uani 1 1 d . . . . .
H46 H 0.3097 0.1055 0.6247 0.062 Uiso 1 1 calc R U . . .
C60 C 0.0413(4) 0.3428(9) 0.3750(6) 0.127(4) Uani 1 1 d . . . . .
D60 D 0.0337 0.3045 0.4266 0.152 Uiso 1 1 calc R U . . .
C61 C 0.0163(2) 0.3304(7) 0.2987(6) 0.100(2) Uani 1 1 d . . . . .
D61 D -0.0081 0.2836 0.2981 0.121 Uiso 1 1 calc R U . . .
C62 C 0.0282(2) 0.3864(6) 0.2288(5) 0.0817(18) Uani 1 1 d . . . . .
D62 D 0.0120 0.3791 0.1774 0.098 Uiso 1 1 calc R U . . .
C63 C 0.0625(2) 0.4529(5) 0.2282(5) 0.0884(19) Uani 1 1 d . . . . .
D63 D 0.0702 0.4922 0.1770 0.106 Uiso 1 1 calc R U . . .
C64 C 0.0862(2) 0.4641(5) 0.3006(6) 0.091(2) Uani 1 1 d . . . . .
D64 D 0.1104 0.5115 0.2996 0.109 Uiso 1 1 calc R U . . .
C65 C 0.0763(3) 0.4105(8) 0.3728(6) 0.109(3) Uani 1 1 d . . . . .
D65 D 0.0935 0.4190 0.4228 0.130 Uiso 1 1 calc R U . . .
C70 C 0.2900(2) -0.1270(5) 0.1309(6) 0.090(2) Uani 1 1 d . . . . .
D70 D 0.3075 -0.0674 0.1108 0.108 Uiso 1 1 calc R U . . .
C71 C 0.2643(2) -0.1849(6) 0.0758(4) 0.0746(16) Uani 1 1 d . . . . .
D71 D 0.2637 -0.1656 0.0163 0.089 Uiso 1 1 calc R U . . .
C72 C 0.2404(2) -0.2675(6) 0.1048(5) 0.0792(17) Uani 1 1 d . . . . .
D72 D 0.2228 -0.3070 0.0653 0.095 Uiso 1 1 calc R U . . .
C73 C 0.2401(2) -0.2974(5) 0.1872(5) 0.0861(19) Uani 1 1 d . . . . .
D73 D 0.2224 -0.3575 0.2055 0.103 Uiso 1 1 calc R U . . .
C74 C 0.2638(3) -0.2457(7) 0.2438(4) 0.087(2) Uani 1 1 d . . . . .
D74 D 0.2630 -0.2686 0.3025 0.104 Uiso 1 1 calc R U . . .
C75 C 0.2897(2) -0.1590(8) 0.2198(6) 0.101(3) Uani 1 1 d . . . . .
D75 D 0.3070 -0.1212 0.2609 0.121 Uiso 1 1 calc R U . . .
H11 H 0.1197(16) -0.050(4) -0.184(4) 0.057(15) Uiso 1 1 d . . . . .
H21 H 0.2448(12) 0.044(3) 0.587(3) 0.034(10) Uiso 1 1 d . . . . .
H2A H 0.2396(15) 0.129(4) 0.112(3) 0.058(13) Uiso 1 1 d . . . . .
H6A H 0.144(2) -0.204(5) 0.274(4) 0.086(19) Uiso 1 1 d . . . . .
H2B H 0.277(2) 0.210(6) 0.136(5) 0.11(2) Uiso 1 1 d . . . . .
H1A H 0.150(2) 0.370(6) 0.169(4) 0.08(2) Uiso 1 1 d . . . . .
H1B H 0.159(2) 0.291(7) 0.103(5) 0.10(3) Uiso 1 1 d . . . . .
H5A H 0.0601(17) -0.102(5) 0.354(4) 0.077(16) Uiso 1 1 d . . . . .
H1C H 0.1846(19) 0.394(6) 0.104(4) 0.080(19) Uiso 1 1 d . . . . .
H2C H 0.2653(17) 0.129(5) 0.192(4) 0.063(16) Uiso 1 1 d . . . . .
H5B H 0.091(2) -0.003(5) 0.342(4) 0.07(2) Uiso 1 1 d . . . . .
H6B H 0.107(3) -0.273(8) 0.246(6) 0.15(3) Uiso 1 1 d . . . . .
H5C H 0.045(3) 0.017(8) 0.315(5) 0.13(3) Uiso 1 1 d . . . . .
H6C H 0.143(3) -0.231(7) 0.167(6) 0.13(3) Uiso 1 1 d . . . . .
C81 C 0.0134(2) 0.5418(7) 0.7218(5) 0.103(2) Uani 1 1 d . . . . .
D81 D 0.0231 0.5721 0.7751 0.124 Uiso 1 1 calc R U . . .
C82 C 0.0273(3) 0.5848(7) 0.6483(7) 0.113(3) Uani 1 1 d . . . . .
D82 D 0.0467 0.6460 0.6493 0.135 Uiso 1 1 calc R U . . .
C83 C 0.0141(2) 0.5427(9) 0.5721(6) 0.127(4) Uani 1 1 d . . . . .
D83 D 0.0246 0.5725 0.5192 0.153 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 O2 1.833(3) . ?
Al1 C3 1.965(5) . ?
Al1 C2 1.969(6) . ?
Al1 C1 1.981(6) . ?
Al1 K2 3.680(2) . ?
Al1 K1 3.6961(15) . ?
Al2 O1 1.829(3) . ?
Al2 C4 1.970(6) . ?
Al2 C5 1.983(7) . ?
Al2 C6 1.983(7) . ?
Al2 K1 3.6027(18) . ?
Al2 K2 3.6270(18) . ?
K1 N1 2.719(3) . ?
K1 N2 2.733(3) . ?
K1 O1 2.822(3) . ?
K1 O2 3.039(3) . ?
K1 C2 3.118(6) . ?
K1 C6 3.178(7) . ?
K1 C75 3.341(6) . ?
K1 C70 3.337(6) . ?
K1 C71 3.380(5) . ?
K1 C74 3.390(6) . ?
K1 C72 3.424(6) . ?
K1 C73 3.433(6) . ?
K2 O2 2.565(3) . ?
K2 O1 2.567(3) . ?
K2 C62 3.118(6) . ?
K2 C5 3.171(8) . ?
K2 C61 3.165(6) . ?
K2 C63 3.186(6) . ?
K2 C1 3.251(9) . ?
K2 C60 3.270(7) . ?
K2 C64 3.286(6) . ?
K2 C65 3.330(7) . ?
N1 C10 1.283(5) . ?
N1 O1 1.412(4) . ?
N2 C20 1.266(5) . ?
N2 O2 1.417(4) . ?
N11 C31 1.395(7) . ?
N11 C11 1.463(6) . ?
N21 C41 1.387(6) . ?
N21 C21 1.477(5) . ?
C10 C15 1.492(6) . ?
C10 C11 1.523(6) . ?
C11 C30 1.529(6) . ?
C11 C12 1.541(6) . ?
C12 C13 1.521(7) . ?
C13 C14 1.523(7) . ?
C14 C16 1.527(7) . ?
C14 C15 1.544(6) . ?
C16 C18 1.313(8) . ?
C16 C17 1.478(8) . ?
C20 C25 1.497(5) . ?
C20 C21 1.528(5) . ?
C21 C40 1.527(6) . ?
C21 C22 1.547(6) . ?
C22 C23 1.500(6) . ?
C23 C24 1.545(6) . ?
C24 C26 1.503(6) . ?
C24 C25 1.530(6) . ?
C26 C28 1.327(7) . ?
C26 C27 1.507(7) . ?
C31 C32 1.379(7) . ?
C31 C36 1.387(7) . ?
C32 C33 1.387(9) . ?
C33 C34 1.341(10) . ?
C34 C35 1.369(9) . ?
C35 C36 1.398(8) . ?
C41 C46 1.386(6) . ?
C41 C42 1.396(6) . ?
C42 C43 1.368(7) . ?
C43 C44 1.367(8) . ?
C44 C45 1.393(8) . ?
C45 C46 1.378(7) . ?
C60 C65 1.368(14) . ?
C60 C61 1.428(13) . ?
C61 C62 1.324(10) . ?
C62 C63 1.341(9) . ?
C63 C64 1.353(10) . ?
C64 C65 1.322(12) . ?
C70 C71 1.362(10) . ?
C70 C75 1.427(11) . ?
C71 C72 1.316(9) . ?
C72 C73 1.324(9) . ?
C73 C74 1.303(11) . ?
C74 C75 1.366(11) . ?
C81 C81 1.305(15) 2_565 ?
C81 C82 1.320(11) . ?
C82 C83 1.347(12) . ?
C83 C83 1.35(2) 2_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Al1 C3 107.6(2) . . ?
O2 Al1 C2 110.1(2) . . ?
C3 Al1 C2 112.6(3) . . ?
O2 Al1 C1 101.8(3) . . ?
C3 Al1 C1 112.1(3) . . ?
C2 Al1 C1 112.0(3) . . ?
O2 Al1 K2 40.07(9) . . ?
C3 Al1 K2 122.8(2) . . ?
C2 Al1 K2 122.25(18) . . ?
C1 Al1 K2 61.8(3) . . ?
O2 Al1 K1 54.92(10) . . ?
C3 Al1 K1 140.59(17) . . ?
C2 Al1 K1 57.53(17) . . ?
C1 Al1 K1 106.4(3) . . ?
K2 Al1 K1 69.31(3) . . ?
O1 Al2 C4 109.7(2) . . ?
O1 Al2 C5 101.5(3) . . ?
C4 Al2 C5 114.6(4) . . ?
O1 Al2 C6 108.7(2) . . ?
C4 Al2 C6 111.5(3) . . ?
C5 Al2 C6 110.4(4) . . ?
O1 Al2 K1 50.63(10) . . ?
C4 Al2 K1 143.2(2) . . ?
C5 Al2 K1 100.8(3) . . ?
C6 Al2 K1 61.5(2) . . ?
O1 Al2 K2 41.67(9) . . ?
C4 Al2 K2 117.5(2) . . ?
C5 Al2 K2 60.7(2) . . ?
C6 Al2 K2 129.1(2) . . ?
K1 Al2 K2 70.92(3) . . ?
N1 K1 N2 117.85(11) . . ?
N1 K1 O1 29.45(9) . . ?
N2 K1 O1 92.93(10) . . ?
N1 K1 O2 93.30(9) . . ?
N2 K1 O2 27.79(9) . . ?
O1 K1 O2 74.11(8) . . ?
N1 K1 C2 100.30(15) . . ?
N2 K1 C2 71.63(13) . . ?
O1 K1 C2 108.56(14) . . ?
O2 K1 C2 60.81(12) . . ?
N1 K1 C6 71.02(15) . . ?
N2 K1 C6 108.30(17) . . ?
O1 K1 C6 61.86(14) . . ?
O2 K1 C6 114.50(15) . . ?
C2 K1 C6 170.38(18) . . ?
N1 K1 C75 139.65(14) . . ?
N2 K1 C75 101.26(14) . . ?
O1 K1 C75 164.53(13) . . ?
O2 K1 C75 121.34(13) . . ?
C2 K1 C75 82.1(2) . . ?
C6 K1 C75 107.2(2) . . ?
N1 K1 C70 117.70(18) . . ?
N2 K1 C70 117.28(18) . . ?
O1 K1 C70 147.00(18) . . ?
O2 K1 C70 127.53(15) . . ?
C2 K1 C70 72.11(16) . . ?
C6 K1 C70 115.23(17) . . ?
C75 K1 C70 24.68(19) . . ?
N1 K1 C71 98.05(13) . . ?
N2 K1 C71 140.53(15) . . ?
O1 K1 C71 125.78(13) . . ?
O2 K1 C71 147.46(15) . . ?
C2 K1 C71 87.10(17) . . ?
C6 K1 C71 98.03(19) . . ?
C75 K1 C71 41.61(16) . . ?
C70 K1 C71 23.38(17) . . ?
N1 K1 C74 133.95(17) . . ?
N2 K1 C74 106.36(15) . . ?
O1 K1 C74 144.86(18) . . ?
O2 K1 C74 132.60(16) . . ?
C2 K1 C74 105.4(2) . . ?
C6 K1 C74 84.0(2) . . ?
C75 K1 C74 23.40(19) . . ?
C70 K1 C74 41.63(17) . . ?
C71 K1 C74 46.95(14) . . ?
N1 K1 C72 96.24(14) . . ?
N2 K1 C72 145.51(14) . . ?
O1 K1 C72 117.78(13) . . ?
O2 K1 C72 167.45(13) . . ?
C2 K1 C72 109.24(16) . . ?
C6 K1 C72 76.49(18) . . ?
C75 K1 C72 46.90(16) . . ?
C70 K1 C72 40.16(17) . . ?
C71 K1 C72 22.30(16) . . ?
C74 K1 C72 39.25(17) . . ?
N1 K1 C73 112.15(16) . . ?
N2 K1 C73 125.82(16) . . ?
O1 K1 C73 125.35(15) . . ?
O2 K1 C73 153.39(16) . . ?
C2 K1 C73 118.78(17) . . ?
C6 K1 C73 69.44(18) . . ?
C75 K1 C73 40.10(19) . . ?
C70 K1 C73 47.09(16) . . ?
C71 K1 C73 39.63(16) . . ?
C74 K1 C73 22.01(18) . . ?
C72 K1 C73 22.27(16) . . ?
O2 K2 O1 87.10(9) . . ?
O2 K2 C62 137.20(15) . . ?
O1 K2 C62 133.32(14) . . ?
O2 K2 C5 96.7(2) . . ?
O1 K2 C5 60.86(14) . . ?
C62 K2 C5 114.0(2) . . ?
O2 K2 C61 136.09(18) . . ?
O1 K2 C61 133.82(17) . . ?
C62 K2 C61 24.32(19) . . ?
C5 K2 C61 92.8(2) . . ?
O2 K2 C63 114.27(16) . . ?
O1 K2 C63 145.64(16) . . ?
C62 K2 C63 24.53(17) . . ?
C5 K2 C63 135.9(2) . . ?
C61 K2 C63 43.1(2) . . ?
O2 K2 C1 59.83(13) . . ?
O1 K2 C1 95.23(17) . . ?
C62 K2 C1 97.1(2) . . ?
C5 K2 C1 148.7(2) . . ?
C61 K2 C1 118.4(2) . . ?
C63 K2 C1 75.4(2) . . ?
O2 K2 C60 111.2(3) . . ?
O1 K2 C60 148.7(3) . . ?
C62 K2 C60 43.2(2) . . ?
C5 K2 C60 91.0(2) . . ?
C61 K2 C60 25.6(2) . . ?
C63 K2 C60 49.5(2) . . ?
C1 K2 C60 115.8(3) . . ?
O2 K2 C64 94.73(14) . . ?
O1 K2 C64 166.64(19) . . ?
C62 K2 C64 42.59(17) . . ?
C5 K2 C64 131.8(2) . . ?
C61 K2 C64 49.8(2) . . ?
C63 K2 C64 24.08(17) . . ?
C1 K2 C64 74.5(2) . . ?
C60 K2 C64 41.5(2) . . ?
O2 K2 C65 93.31(17) . . ?
O1 K2 C65 170.2(2) . . ?
C62 K2 C65 49.62(18) . . ?
C5 K2 C65 109.4(3) . . ?
C61 K2 C65 43.5(2) . . ?
C63 K2 C65 41.9(2) . . ?
C1 K2 C65 93.4(3) . . ?
C60 K2 C65 23.9(2) . . ?
C64 K2 C65 23.0(2) . . ?
O2 K2 Al2 95.67(8) . . ?
O1 K2 Al2 28.27(7) . . ?
C62 K2 Al2 126.39(14) . . ?
C5 K2 Al2 33.06(12) . . ?
C61 K2 Al2 114.26(16) . . ?
C63 K2 Al2 150.05(14) . . ?
C1 K2 Al2 122.67(15) . . ?
C60 K2 Al2 121.5(2) . . ?
C64 K2 Al2 162.80(17) . . ?
C65 K2 Al2 142.2(2) . . ?
O2 K2 Al1 27.38(7) . . ?
O1 K2 Al1 90.23(7) . . ?
C62 K2 Al1 121.93(15) . . ?
C5 K2 Al1 121.42(19) . . ?
C61 K2 Al1 135.18(15) . . ?
C63 K2 Al1 97.49(14) . . ?
C1 K2 Al1 32.47(11) . . ?
C60 K2 Al1 117.9(3) . . ?
C64 K2 Al1 85.48(14) . . ?
C65 K2 Al1 94.6(2) . . ?
Al2 K2 Al1 109.73(4) . . ?
C10 N1 O1 115.8(3) . . ?
C10 N1 K1 159.5(3) . . ?
O1 N1 K1 79.35(18) . . ?
C20 N2 O2 115.6(3) . . ?
C20 N2 K1 153.1(3) . . ?
O2 N2 K1 88.19(19) . . ?
C31 N11 C11 124.1(4) . . ?
C41 N21 C21 124.6(4) . . ?
N1 O1 Al2 117.2(2) . . ?
N1 O1 K2 132.7(2) . . ?
Al2 O1 K2 110.06(13) . . ?
N1 O1 K1 71.20(18) . . ?
Al2 O1 K1 99.31(12) . . ?
K2 O1 K1 102.11(10) . . ?
N2 O2 Al1 117.7(2) . . ?
N2 O2 K2 127.2(2) . . ?
Al1 O2 K2 112.54(13) . . ?
N2 O2 K1 64.02(17) . . ?
Al1 O2 K1 95.51(12) . . ?
K2 O2 K1 96.56(9) . . ?
Al1 C1 K2 85.8(3) . . ?
Al1 C2 K1 90.3(2) . . ?
Al2 C5 K2 86.2(2) . . ?
Al2 C6 K1 85.2(2) . . ?
N1 C10 C15 126.4(4) . . ?
N1 C10 C11 116.7(4) . . ?
C15 C10 C11 116.8(3) . . ?
N11 C11 C10 108.9(3) . . ?
N11 C11 C30 112.1(4) . . ?
C10 C11 C30 113.6(3) . . ?
N11 C11 C12 107.2(4) . . ?
C10 C11 C12 106.4(4) . . ?
C30 C11 C12 108.4(4) . . ?
C13 C12 C11 114.6(4) . . ?
C12 C13 C14 110.6(4) . . ?
C16 C14 C13 113.7(4) . . ?
C16 C14 C15 111.3(4) . . ?
C13 C14 C15 108.6(4) . . ?
C10 C15 C14 109.8(3) . . ?
C18 C16 C17 121.7(6) . . ?
C18 C16 C14 120.0(5) . . ?
C17 C16 C14 118.3(5) . . ?
N2 C20 C25 128.2(4) . . ?
N2 C20 C21 116.5(3) . . ?
C25 C20 C21 115.2(3) . . ?
N21 C21 C40 112.0(4) . . ?
N21 C21 C20 109.5(3) . . ?
C40 C21 C20 113.8(3) . . ?
N21 C21 C22 106.3(3) . . ?
C40 C21 C22 109.0(4) . . ?
C20 C21 C22 105.7(3) . . ?
C23 C22 C21 114.2(3) . . ?
C22 C23 C24 112.3(4) . . ?
C26 C24 C25 114.9(3) . . ?
C26 C24 C23 110.8(3) . . ?
C25 C24 C23 109.2(3) . . ?
C20 C25 C24 111.6(3) . . ?
C28 C26 C24 123.3(4) . . ?
C28 C26 C27 120.4(5) . . ?
C24 C26 C27 116.3(4) . . ?
C32 C31 C36 118.0(5) . . ?
C32 C31 N11 118.9(5) . . ?
C36 C31 N11 123.1(4) . . ?
C31 C32 C33 120.2(6) . . ?
C34 C33 C32 122.1(6) . . ?
C33 C34 C35 118.8(6) . . ?
C34 C35 C36 120.6(7) . . ?
C31 C36 C35 120.3(5) . . ?
N21 C41 C46 119.1(4) . . ?
N21 C41 C42 123.6(4) . . ?
C46 C41 C42 117.3(4) . . ?
C43 C42 C41 120.8(5) . . ?
C44 C43 C42 121.6(5) . . ?
C43 C44 C45 118.8(5) . . ?
C46 C45 C44 119.6(5) . . ?
C45 C46 C41 121.9(5) . . ?
C65 C60 C61 119.1(8) . . ?
C65 C60 K2 80.5(5) . . ?
C61 C60 K2 73.1(4) . . ?
C62 C61 C60 117.8(8) . . ?
C62 C61 K2 75.8(4) . . ?
C60 C61 K2 81.3(4) . . ?
C61 C62 C63 122.1(7) . . ?
C61 C62 K2 79.8(4) . . ?
C63 C62 K2 80.6(4) . . ?
C62 C63 C64 119.8(7) . . ?
C62 C63 K2 74.9(3) . . ?
C64 C63 K2 82.1(4) . . ?
C65 C64 C63 121.6(8) . . ?
C65 C64 K2 80.3(4) . . ?
C63 C64 K2 73.8(3) . . ?
C64 C65 C60 119.6(8) . . ?
C64 C65 K2 76.6(4) . . ?
C60 C65 K2 75.6(4) . . ?
C71 C70 C75 117.7(6) . . ?
C71 C70 K1 80.1(3) . . ?
C75 C70 K1 77.8(3) . . ?
C72 C71 C70 120.3(6) . . ?
C72 C71 K1 80.7(3) . . ?
C70 C71 K1 76.6(3) . . ?
C73 C72 C71 122.0(7) . . ?
C73 C72 K1 79.3(3) . . ?
C71 C72 K1 77.0(3) . . ?
C74 C73 C72 121.1(7) . . ?
C74 C73 K1 77.1(4) . . ?
C72 C73 K1 78.5(4) . . ?
C73 C74 C75 121.0(7) . . ?
C73 C74 K1 80.9(4) . . ?
C75 C74 K1 76.3(3) . . ?
C74 C75 C70 117.7(6) . . ?
C74 C75 K1 80.3(3) . . ?
C70 C75 K1 77.5(3) . . ?
C81 C81 C82 120.6(5) 2_565 . ?
C81 C82 C83 120.6(8) . . ?
C83 C83 C82 118.8(5) 2_565 . ?

_refine_diff_density_max         0.298
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.050

