# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_2a_3tol
_database_code_depnum_ccdc_archive 'CCDC 1897464'
loop_
_audit_author_name
_audit_author_address
'Marta E. G. Mosquera'
;University of Alcala
Spain
;
_audit_update_record             
;
2019-03-24 deposited with the CCDC.	2019-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_2a_3tol             
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Low quality of the crystal
;
_vrf_PLAT020_2a_3tol             
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.199 Report
RESPONSE: Low quality of the crystal
;
_vrf_PLAT201_2a_3tol             
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: Corresponds to a tBu group that is disordered
;
# Added during the CSD deposition process: Sunday 24 March 2019 08:06 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78  H84  Al2  Li2  O2.2C7 H8'
_chemical_formula_sum            'C92 H100 Al2 Li2 O2'
_chemical_formula_weight         1305.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   15.501
_cell_length_b                   10.255
_cell_length_c                   30.557
_cell_angle_alpha                90
_cell_angle_beta                 98.61
_cell_angle_gamma                90
_cell_volume                     4802.9
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    69
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      19.04
_cell_measurement_wavelength     0.71073

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.903
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_absorpt_coefficient_mu    0.069
_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  0.688
_exptl_absorpt_correction_T_max  1.512

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            69473
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_av_R_equivalents  0.1994
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.000
_diffrn_reflns_theta_max         26.891
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             9454
_reflns_number_gt                5688
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-2008 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1161P)²+5.8792P] 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     SHELXL
_refine_ls_extinction_coef       0.0043(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9454
_refine_ls_number_parameters     387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.0993
_refine_ls_wR_factor_ref         0.2873
_refine_ls_wR_factor_gt          0.2540
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# SQUEEZE RESULTS (Version =  40319)
# 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 -0.028 0.250 937 228 ' '
2 -0.000 0.104 0.750 939 228 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;                           
Two molecules of toluene crystallized with every molecule of this 
 compound but presented severe disorder and it was not possible to get a 
 chemical sensible model for them, 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
C1 C 0.3783(3) 0.3930(4) 0.46424(16) 0.0643(11) Uani 1 1 d . . . . .
H1A H 0.4153 0.4698 0.4715 0.096 Uiso 1 1 calc R U . . .
H1B H 0.3528 0.3663 0.4903 0.096 Uiso 1 1 calc R U . . .
H1C H 0.3315 0.4143 0.4400 0.096 Uiso 1 1 calc R U . . .
C2 C 0.5245(2) 0.3104(4) 0.40314(12) 0.0511(9) Uani 1 1 d . . . . .
H2A H 0.5650 0.3767 0.4172 0.077 Uiso 1 1 calc R U . . .
H2B H 0.4880 0.3484 0.3773 0.077 Uiso 1 1 calc R U . . .
H2C H 0.5576 0.2369 0.3937 0.077 Uiso 1 1 calc R U . . .
C3 C 0.5218(2) 0.1648(3) 0.49738(11) 0.0410(8) Uani 1 1 d . . . . .
H3A H 0.5606 0.2299 0.5135 0.061 Uiso 1 1 calc R U . . .
H3B H 0.5568 0.0948 0.4870 0.061 Uiso 1 1 calc R U . . .
H3C H 0.4837 0.1283 0.5171 0.061 Uiso 1 1 calc R U . . .
C4 C 0.1673(2) 0.1263(5) 0.32327(14) 0.0636(12) Uani 1 1 d . . . . .
C5 C 0.1571(2) 0.1397(4) 0.36685(15) 0.0611(11) Uani 1 1 d . . . . .
H5 H 0.1002 0.1544 0.3738 0.073 Uiso 1 1 calc R U . . .
C6 C 0.2268(2) 0.1327(4) 0.40127(12) 0.0468(9) Uani 1 1 d . . . . .
C7 C 0.0888(3) 0.1393(6) 0.28552(19) 0.0873(16) Uani 1 1 d . . . . .
C8 C 0.0223(8) 0.0319(14) 0.2923(4) 0.078(4) Uiso 0.449(9) 1 d . . P A 1
H8A H -0.0244 0.0303 0.2669 0.118 Uiso 0.449(9) 1 calc R U P A 1
H8B H -0.0026 0.0500 0.3193 0.118 Uiso 0.449(9) 1 calc R U P A 1
H8C H 0.0518 -0.0530 0.2951 0.118 Uiso 0.449(9) 1 calc R U P A 1
C9 C 0.1126(8) 0.2547(12) 0.2520(4) 0.088(4) Uiso 0.449(9) 1 d . . P A 1
H9A H 0.0644 0.2644 0.2275 0.133 Uiso 0.449(9) 1 calc R U P A 1
H9B H 0.1660 0.2313 0.2402 0.133 Uiso 0.449(9) 1 calc R U P A 1
H9C H 0.1215 0.3371 0.2682 0.133 Uiso 0.449(9) 1 calc R U P A 1
C10 C 0.0212(9) 0.2532(13) 0.3019(5) 0.089(4) Uiso 0.449(9) 1 d . . P A 1
H10A H -0.0329 0.2563 0.2807 0.134 Uiso 0.449(9) 1 calc R U P A 1
H10B H 0.0498 0.3387 0.3031 0.134 Uiso 0.449(9) 1 calc R U P A 1
H10C H 0.0077 0.2305 0.3312 0.134 Uiso 0.449(9) 1 calc R U P A 1
C8' C 0.0093(13) 0.098(2) 0.3005(7) 0.175(8) Uiso 0.551(9) 1 d . . P A 2
H8'1 H 0.0197 0.0172 0.3174 0.263 Uiso 0.551(9) 1 calc R U P A 2
H8'2 H -0.0359 0.0838 0.2749 0.263 Uiso 0.551(9) 1 calc R U P A 2
H8'3 H -0.0101 0.1662 0.3194 0.263 Uiso 0.551(9) 1 calc R U P A 2
C9' C 0.1069(7) 0.0682(11) 0.2419(4) 0.096(4) Uiso 0.551(9) 1 d . . P A 2
H9'1 H 0.1257 -0.0216 0.2489 0.144 Uiso 0.551(9) 1 calc R U P A 2
H9'2 H 0.1528 0.1148 0.2294 0.144 Uiso 0.551(9) 1 calc R U P A 2
H9'3 H 0.0534 0.0672 0.2203 0.144 Uiso 0.551(9) 1 calc R U P A 2
C10' C 0.0653(9) 0.2691(13) 0.2782(5) 0.118(4) Uiso 0.551(9) 1 d . . P A 2
H10D H 0.0126 0.2742 0.2561 0.178 Uiso 0.551(9) 1 calc R U P A 2
H10E H 0.1129 0.3160 0.2672 0.178 Uiso 0.551(9) 1 calc R U P A 2
H10F H 0.0540 0.3087 0.3059 0.178 Uiso 0.551(9) 1 calc R U P A 2
C11 C 0.4131(2) 0.0551(3) 0.33778(11) 0.0403(8) Uani 1 1 d . . . . .
H11 H 0.4532 0.1261 0.3508 0.048 Uiso 1 1 calc R U . . .
C12 C 0.4205(2) 0.0504(4) 0.28859(11) 0.0467(9) Uani 1 1 d . . . . .
C13 C 0.3967(3) -0.0589(4) 0.26314(13) 0.0682(12) Uani 1 1 d . . . . .
H13 H 0.3752 -0.1337 0.2764 0.082 Uiso 1 1 calc R U . . .
C14 C 0.4039(4) -0.0604(5) 0.21870(14) 0.0855(16) Uani 1 1 d . . . . .
H14 H 0.3874 -0.1365 0.2018 0.103 Uiso 1 1 calc R U . . .
C15 C 0.4340(4) 0.0442(6) 0.19871(15) 0.0885(16) Uani 1 1 d . . . . .
H15 H 0.4396 0.0417 0.1682 0.106 Uiso 1 1 calc R U . . .
C16 C 0.4564(4) 0.1542(5) 0.22345(16) 0.0849(15) Uani 1 1 d . . . . .
H16 H 0.4759 0.2296 0.2098 0.102 Uiso 1 1 calc R U . . .
C17 C 0.4507(3) 0.1558(4) 0.26833(14) 0.0652(11) Uani 1 1 d . . . . .
H17 H 0.4682 0.2316 0.2852 0.078 Uiso 1 1 calc R U . . .
C18 C 0.4463(2) -0.0701(3) 0.36110(10) 0.0411(8) Uani 1 1 d . . . . .
C19 C 0.5353(3) -0.0857(4) 0.37473(12) 0.0531(10) Uani 1 1 d . . . . .
H19 H 0.5743 -0.0168 0.3706 0.064 Uiso 1 1 calc R U . . .
C20 C 0.5678(3) -0.2016(5) 0.39444(13) 0.0685(13) Uani 1 1 d . . . . .
H20 H 0.6288 -0.2121 0.4031 0.082 Uiso 1 1 calc R U . . .
C22 C 0.5124(4) -0.3003(5) 0.40138(13) 0.0708(14) Uani 1 1 d . . . . .
H22 H 0.5349 -0.3787 0.4152 0.085 Uiso 1 1 calc R U . . .
C23 C 0.4243(3) -0.2865(4) 0.38837(13) 0.0642(12) Uani 1 1 d . . . . .
H23 H 0.3857 -0.3554 0.3931 0.077 Uiso 1 1 calc R U . . .
C24 C 0.3917(3) -0.1716(4) 0.36834(12) 0.0523(10) Uani 1 1 d . . . . .
H24 H 0.3306 -0.1626 0.3594 0.063 Uiso 1 1 calc R U . . .
C25 C 0.2152(2) 0.1353(4) 0.44988(13) 0.0509(10) Uani 1 1 d . . . . .
H25 H 0.2618 0.1941 0.4651 0.061 Uiso 1 1 calc R U . . .
C26 C 0.1287(3) 0.1943(5) 0.45737(15) 0.0660(12) Uani 1 1 d . . . . .
C27 C 0.1186(3) 0.3292(6) 0.4566(2) 0.0979(18) Uani 1 1 d . . . . .
H27 H 0.1673 0.3829 0.4538 0.118 Uiso 1 1 calc R U . . .
C28 C 0.0384(4) 0.3872(7) 0.4599(3) 0.126(3) Uani 1 1 d . . . . .
H28 H 0.0325 0.4794 0.4588 0.151 Uiso 1 1 calc R U . . .
C29 C -0.0317(4) 0.3099(8) 0.4648(3) 0.122(2) Uani 1 1 d . . . . .
H29 H -0.0865 0.3484 0.4673 0.147 Uiso 1 1 calc R U . . .
C30 C -0.0226(3) 0.1775(8) 0.4659(2) 0.107(2) Uani 1 1 d . . . . .
H30 H -0.0709 0.1246 0.4703 0.129 Uiso 1 1 calc R U . . .
C31 C 0.0563(3) 0.1189(6) 0.46080(17) 0.0791(14) Uani 1 1 d . . . . .
H31 H 0.0603 0.0265 0.4596 0.095 Uiso 1 1 calc R U . . .
C32 C 0.2313(2) 0.0021(4) 0.47118(13) 0.0507(10) Uani 1 1 d . . . . .
C33 C 0.2241(2) -0.1123(4) 0.44729(14) 0.0586(11) Uani 1 1 d . . . . .
H33 H 0.2096 -0.1087 0.4160 0.070 Uiso 1 1 calc R U . . .
C34 C 0.2375(3) -0.2323(5) 0.46785(19) 0.0776(14) Uani 1 1 d . . . . .
H34 H 0.2323 -0.3104 0.4509 0.093 Uiso 1 1 calc R U . . .
C35 C 0.2589(3) -0.2370(7) 0.5141(2) 0.0886(18) Uani 1 1 d . . . . .
H35 H 0.2686 -0.3183 0.5289 0.106 Uiso 1 1 calc R U . . .
C36 C 0.2656(3) -0.1253(7) 0.53706(17) 0.0817(16) Uani 1 1 d . . . . .
H36 H 0.2802 -0.1290 0.5684 0.098 Uiso 1 1 calc R U . . .
C37 C 0.2523(2) -0.0068(5) 0.51721(14) 0.0684(13) Uani 1 1 d . . . . .
H37 H 0.2573 0.0702 0.5347 0.082 Uiso 1 1 calc R U . . .
C41 C 0.3106(2) 0.1144(3) 0.39051(11) 0.0394(8) Uani 1 1 d . . . . .
C42 C 0.3230(2) 0.0920(3) 0.34685(11) 0.0412(8) Uani 1 1 d . . . . .
C43 C 0.2503(2) 0.0997(4) 0.31350(12) 0.0531(10) Uani 1 1 d . . . . .
H43 H 0.2580 0.0865 0.2836 0.064 Uiso 1 1 calc R U . . .
Al1 Al 0.44955(6) 0.24873(10) 0.44577(3) 0.0369(3) Uani 1 1 d . . . . .
Li1 Li 0.4008(5) -0.0613(7) 0.4443(2) 0.0599(18) Uani 1 1 d . . . . .
O1 O 0.38104(12) 0.1094(2) 0.42407(7) 0.0360(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Al1 1.978(4) . ?
C2 Al1 1.974(4) . ?
C3 Al1 1.989(3) . ?
C3 Li1 2.258(7) 3_656 ?
C4 C5 1.371(6) . ?
C4 C43 1.391(6) . ?
C4 C7 1.552(5) . ?
C5 C6 1.393(5) . ?
C6 C41 1.398(5) . ?
C6 C25 1.523(5) . ?
C7 C10' 1.389(13) . ?
C7 C8' 1.44(2) . ?
C7 C8 1.544(13) . ?
C7 C9' 1.581(11) . ?
C7 C9 1.643(13) . ?
C7 C10 1.693(14) . ?
C11 C42 1.512(5) . ?
C11 C18 1.521(5) . ?
C11 C12 1.525(5) . ?
C12 C17 1.363(5) . ?
C12 C13 1.383(5) . ?
C13 C14 1.379(6) . ?
C14 C15 1.352(7) . ?
C15 C16 1.372(7) . ?
C16 C17 1.387(6) . ?
C18 C24 1.381(5) . ?
C18 C19 1.389(5) . ?
C18 Li1 2.741(8) . ?
C19 C20 1.392(6) . ?
C20 C22 1.364(7) . ?
C22 C23 1.372(7) . ?
C23 C24 1.388(6) . ?
C24 Li1 2.568(8) . ?
C25 C32 1.518(6) . ?
C25 C26 1.519(5) . ?
C26 C31 1.380(6) . ?
C26 C27 1.392(7) . ?
C27 C28 1.394(7) . ?
C28 C29 1.372(9) . ?
C29 C30 1.364(9) . ?
C30 C31 1.393(7) . ?
C32 C33 1.377(6) . ?
C32 C37 1.399(5) . ?
C33 C34 1.384(6) . ?
C34 C35 1.403(8) . ?
C35 C36 1.339(8) . ?
C36 C37 1.360(7) . ?
C41 O1 1.383(4) . ?
C41 C42 1.395(5) . ?
C41 Li1 2.687(7) . ?
C42 C43 1.404(5) . ?
Al1 O1 1.844(2) . ?
Al1 Li1 3.267(7) . ?
Li1 O1 1.867(7) . ?
Li1 C3 2.258(7) 3_656 ?

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
Al1 C3 Li1 177.2(3) . 3_656 ?
C5 C4 C43 118.2(3) . . ?
C5 C4 C7 121.4(4) . . ?
C43 C4 C7 120.3(4) . . ?
C4 C5 C6 122.6(4) . . ?
C5 C6 C41 118.2(4) . . ?
C5 C6 C25 122.9(3) . . ?
C41 C6 C25 118.7(3) . . ?
C10' C7 C8' 96.6(11) . . ?
C10' C7 C4 111.1(7) . . ?
C8' C7 C4 110.6(9) . . ?
C8 C7 C4 107.7(6) . . ?
C10' C7 C9' 112.4(8) . . ?
C8' C7 C9' 113.7(10) . . ?
C4 C7 C9' 111.6(5) . . ?
C8 C7 C9 144.5(7) . . ?
C4 C7 C9 107.5(6) . . ?
C8 C7 C10 89.9(7) . . ?
C4 C7 C10 106.9(6) . . ?
C9 C7 C10 83.9(7) . . ?
C42 C11 C18 112.5(3) . . ?
C42 C11 C12 113.4(3) . . ?
C18 C11 C12 111.4(3) . . ?
C17 C12 C13 118.0(4) . . ?
C17 C12 C11 120.3(3) . . ?
C13 C12 C11 121.8(3) . . ?
C14 C13 C12 120.5(4) . . ?
C15 C14 C13 121.4(5) . . ?
C14 C15 C16 118.6(4) . . ?
C15 C16 C17 120.4(5) . . ?
C12 C17 C16 121.1(4) . . ?
C24 C18 C19 118.1(3) . . ?
C24 C18 C11 122.6(3) . . ?
C19 C18 C11 119.3(3) . . ?
C24 C18 Li1 68.1(2) . . ?
C19 C18 Li1 96.2(3) . . ?
C11 C18 Li1 106.9(3) . . ?
C18 C19 C20 120.4(4) . . ?
C22 C20 C19 120.4(4) . . ?
C20 C22 C23 120.1(4) . . ?
C22 C23 C24 119.8(4) . . ?
C18 C24 C23 121.3(4) . . ?
C18 C24 Li1 82.0(3) . . ?
C23 C24 Li1 90.5(3) . . ?
C32 C25 C26 112.7(3) . . ?
C32 C25 C6 111.5(3) . . ?
C26 C25 C6 112.9(3) . . ?
C31 C26 C27 117.8(4) . . ?
C31 C26 C25 122.3(4) . . ?
C27 C26 C25 119.6(4) . . ?
C26 C27 C28 121.5(6) . . ?
C29 C28 C27 119.3(6) . . ?
C30 C29 C28 119.8(5) . . ?
C29 C30 C31 121.0(5) . . ?
C26 C31 C30 120.3(5) . . ?
C33 C32 C37 117.7(4) . . ?
C33 C32 C25 123.0(3) . . ?
C37 C32 C25 119.3(4) . . ?
C32 C33 C34 121.5(4) . . ?
C33 C34 C35 119.0(5) . . ?
C36 C35 C34 119.1(5) . . ?
C35 C36 C37 122.4(5) . . ?
C36 C37 C32 120.3(5) . . ?
O1 C41 C42 119.7(3) . . ?
O1 C41 C6 119.3(3) . . ?
C42 C41 C6 120.9(3) . . ?
O1 C41 Li1 40.53(19) . . ?
C42 C41 Li1 109.9(3) . . ?
C6 C41 Li1 111.2(3) . . ?
C41 C42 C43 118.3(3) . . ?
C41 C42 C11 118.7(3) . . ?
C43 C42 C11 123.0(3) . . ?
C4 C43 C42 121.6(4) . . ?
O1 Al1 C2 112.04(14) . . ?
O1 Al1 C1 111.48(15) . . ?
C2 Al1 C1 110.93(19) . . ?
O1 Al1 C3 100.10(13) . . ?
C2 Al1 C3 110.17(15) . . ?
C1 Al1 C3 111.70(18) . . ?
O1 Al1 Li1 28.49(12) . . ?
C2 Al1 Li1 117.45(18) . . ?
C1 Al1 Li1 126.4(2) . . ?
C3 Al1 Li1 72.00(14) . . ?
O1 Li1 C3 138.1(3) . 3_656 ?
O1 Li1 C24 97.4(3) . . ?
C3 Li1 C24 117.2(3) 3_656 . ?
O1 Li1 C41 28.78(13) . . ?
C3 Li1 C41 164.7(3) 3_656 . ?
C24 Li1 C41 77.79(19) . . ?
O1 Li1 C18 77.0(2) . . ?
C3 Li1 C18 122.4(3) 3_656 . ?
C24 Li1 C18 29.92(13) . . ?
C41 Li1 C18 68.70(18) . . ?
O1 Li1 Al1 28.11(12) . . ?
C3 Li1 Al1 110.6(2) 3_656 . ?
C24 Li1 Al1 115.0(2) . . ?
C41 Li1 Al1 56.89(14) . . ?
C18 Li1 Al1 87.3(2) . . ?
C41 O1 Al1 125.9(2) . . ?
C41 O1 Li1 110.7(3) . . ?
Al1 O1 Li1 123.4(2) . . ?

_refine_diff_density_max         0.882
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.060

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_3c
_database_code_depnum_ccdc_archive 'CCDC 1897466'
loop_
_audit_author_name
_audit_author_address
'Marta E. G. Mosquera'
;University of Alcala
Spain
;
_audit_update_record             
;
2019-03-22 deposited with the CCDC.	2019-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_3c                  
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Crystal had poor quality and only diffracted up to theta 22.89
;
_vrf_RINTA01_3c                  
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Crystal had poor quality
;
_vrf_PLAT020_3c                  
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.184 Report
RESPONSE: Crystal had poor quality
;
# Added during the CSD deposition process: Friday 22 March 2019 03:05 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H72 Al Na O2.C7 H8'
_chemical_formula_sum            'C81 H80 Al Na O2'
_chemical_formula_weight         1135.42

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   10.356(5)
_cell_length_b                   31.152(15)
_cell_length_c                   21.128(10)
_cell_angle_alpha                90
_cell_angle_beta                 102.94(4)
_cell_angle_gamma                90
_cell_volume                     6643(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      17.82
_cell_measurement_wavelength     0.71073

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_F_000             2424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?


_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_coefficient_mu    0.084
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_T_max  0.993

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'

_diffrn_reflns_number            17638
_diffrn_reflns_av_unetI/netI     0.2766
_diffrn_reflns_av_R_equivalents  0.1841
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.039
_diffrn_reflns_theta_max         22.915
_diffrn_reflns_theta_full        22.915
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             9097
_reflns_number_gt                3609
_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-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0476P)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_number_reflns         9097
_refine_ls_number_parameters     766
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2300
_refine_ls_R_factor_gt           0.0757
_refine_ls_wR_factor_ref         0.1651
_refine_ls_wR_factor_gt          0.1300
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_restrained_S_all      0.925
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.52993(18) 0.14195(6) 0.29487(10) 0.0558(6) Uani 1 1 d . . . . .
Al1 Al 0.72873(15) 0.12054(5) 0.20633(8) 0.0411(5) Uani 1 1 d . . . . .
O1 O 0.7205(3) 0.16249(9) 0.26399(15) 0.0381(9) Uani 1 1 d . . . . .
O2 O 0.5855(3) 0.09329(9) 0.22248(15) 0.0361(9) Uani 1 1 d . . . . .
C1 C 0.6895(5) 0.13559(16) 0.1138(2) 0.0580(16) Uani 1 1 d . . . . .
H1A H 0.765841 0.150462 0.103681 0.087 Uiso 1 1 calc R U . . .
H1B H 0.671337 0.109391 0.087649 0.087 Uiso 1 1 calc R U . . .
H1C H 0.611859 0.154444 0.103861 0.087 Uiso 1 1 calc R U . . .
C2 C 0.8983(5) 0.09172(16) 0.2320(3) 0.0622(18) Uani 1 1 d . . . . .
H2A H 0.967486 0.109682 0.220682 0.093 Uiso 1 1 calc R U . . .
H2B H 0.918772 0.086758 0.279000 0.093 Uiso 1 1 calc R U . . .
H2C H 0.894382 0.064153 0.209308 0.093 Uiso 1 1 calc R U . . .
C3 C 0.5117(5) 0.06361(18) 0.1825(2) 0.0352(13) Uani 1 1 d . . . . .
C4 C 0.5493(5) 0.02028(18) 0.1875(2) 0.0350(13) Uani 1 1 d . . . . .
C5 C 0.4718(6) -0.00904(16) 0.1454(3) 0.0434(15) Uani 1 1 d . . . . .
H5 H 0.496562 -0.038454 0.148795 0.052 Uiso 1 1 calc R U . . .
C6 C 0.3600(5) 0.00272(17) 0.0986(2) 0.0374(14) Uani 1 1 d . . . . .
C7 C 0.3239(5) 0.04573(17) 0.0983(2) 0.0382(14) Uani 1 1 d . . . . .
H7 H 0.245640 0.054521 0.068333 0.046 Uiso 1 1 calc R U . . .
C8 C 0.3945(5) 0.07633(16) 0.1387(3) 0.0343(13) Uani 1 1 d . . . . .
C9 C 0.6712(5) 0.00628(16) 0.2374(2) 0.0411(14) Uani 1 1 d . . . . .
H9 H 0.741102 0.028211 0.236204 0.049 Uiso 1 1 calc R U . . .
C10 C 0.3516(5) 0.12227(15) 0.1382(2) 0.0363(13) Uani 1 1 d . . . . .
H10 H 0.432106 0.139967 0.138028 0.044 Uiso 1 1 calc R U . . .
C11 C 0.8178(5) 0.18953(17) 0.2936(3) 0.0338(13) Uani 1 1 d . . . . .
C12 C 0.8843(5) 0.18208(15) 0.3593(3) 0.0328(13) Uani 1 1 d . . . . .
C13 C 0.9780(5) 0.21168(15) 0.3907(2) 0.0356(14) Uani 1 1 d . . . . .
H13 H 1.021294 0.206267 0.434595 0.043 Uiso 1 1 calc R U . . .
C14 C 1.0109(4) 0.24802(16) 0.3618(3) 0.0302(13) Uani 1 1 d . . . . .
C15 C 0.9466(5) 0.25449(15) 0.2968(3) 0.0378(14) Uani 1 1 d . . . . .
H15 H 0.968951 0.279064 0.274889 0.045 Uiso 1 1 calc R U . . .
C16 C 0.8512(5) 0.22638(17) 0.2631(2) 0.0343(13) Uani 1 1 d . . . . .
C17 C 0.7756(5) 0.23535(15) 0.1940(2) 0.0407(14) Uani 1 1 d . . . . .
H17 H 0.757597 0.206771 0.172303 0.049 Uiso 1 1 calc R U . . .
C18 C 0.8437(5) 0.14302(15) 0.3932(2) 0.0361(13) Uani 1 1 d . . . . .
H18 H 0.830923 0.118897 0.361166 0.043 Uiso 1 1 calc R U . . .
C20 C 0.7098(5) 0.15010(19) 0.4121(2) 0.0379(14) Uani 1 1 d . . . . .
C21 C 0.6373(6) 0.11500(18) 0.4230(2) 0.0515(15) Uani 1 1 d . . . . .
H21 H 0.670714 0.087010 0.418637 0.062 Uiso 1 1 calc R U . . .
C22 C 0.5162(6) 0.1196(2) 0.4402(3) 0.0657(18) Uani 1 1 d . . . . .
H22 H 0.466940 0.095181 0.447768 0.079 Uiso 1 1 calc R U . . .
C23 C 0.4695(6) 0.1601(3) 0.4459(3) 0.0634(18) Uani 1 1 d . . . . .
H23 H 0.386751 0.163539 0.457593 0.076 Uiso 1 1 calc R U . . .
C24 C 0.5379(6) 0.1953(2) 0.4355(3) 0.0635(18) Uani 1 1 d . . . . .
H24 H 0.503804 0.223121 0.440150 0.076 Uiso 1 1 calc R U . . .
C25 C 0.6595(6) 0.19038(19) 0.4176(2) 0.0494(15) Uani 1 1 d . . . . .
H25 H 0.707267 0.215004 0.409402 0.059 Uiso 1 1 calc R U . . .
C26 C 1.1077(5) 0.28071(16) 0.3991(3) 0.0413(14) Uani 1 1 d . . . . .
C27 C 1.0351(6) 0.30796(18) 0.4401(3) 0.083(2) Uani 1 1 d . . . . .
H27A H 0.997281 0.289256 0.468598 0.125 Uiso 1 1 calc R U . . .
H27B H 1.097586 0.328053 0.466612 0.125 Uiso 1 1 calc R U . . .
H27C H 0.963969 0.324083 0.411581 0.125 Uiso 1 1 calc R U . . .
C28 C 1.2228(6) 0.25837(18) 0.4437(3) 0.096(3) Uani 1 1 d . . . . .
H28A H 1.189206 0.238687 0.472385 0.144 Uiso 1 1 calc R U . . .
H28B H 1.273353 0.242147 0.417628 0.144 Uiso 1 1 calc R U . . .
H28C H 1.280532 0.279805 0.469823 0.144 Uiso 1 1 calc R U . . .
C29 C 1.1645(6) 0.31052(19) 0.3561(3) 0.082(2) Uani 1 1 d . . . . .
H29A H 1.225849 0.330686 0.383027 0.123 Uiso 1 1 calc R U . . .
H29B H 1.212119 0.293731 0.329314 0.123 Uiso 1 1 calc R U . . .
H29C H 1.092527 0.326521 0.327848 0.123 Uiso 1 1 calc R U . . .
C30 C 0.9505(5) 0.12905(16) 0.4511(3) 0.0384(14) Uani 1 1 d . . . . .
C31 C 0.9542(6) 0.14086(17) 0.5143(3) 0.0501(15) Uani 1 1 d . . . . .
H31 H 0.885826 0.158636 0.523151 0.060 Uiso 1 1 calc R U . . .
C32 C 1.0543(7) 0.1276(2) 0.5649(3) 0.0660(18) Uani 1 1 d . . . . .
H32 H 1.053054 0.135583 0.608218 0.079 Uiso 1 1 calc R U . . .
C33 C 1.1565(7) 0.1027(2) 0.5529(4) 0.0690(19) Uani 1 1 d . . . . .
H33 H 1.226274 0.093882 0.587719 0.083 Uiso 1 1 calc R U . . .
C34 C 1.1570(6) 0.09089(19) 0.4906(4) 0.0649(18) Uani 1 1 d . . . . .
H34 H 1.227457 0.074088 0.481668 0.078 Uiso 1 1 calc R U . . .
C35 C 1.0537(6) 0.10372(18) 0.4409(3) 0.0580(16) Uani 1 1 d . . . . .
H35 H 1.053384 0.094789 0.397870 0.070 Uiso 1 1 calc R U . . .
C40 C 0.8626(5) 0.2599(2) 0.1568(2) 0.0446(15) Uani 1 1 d . . . . .
C41 C 0.8528(6) 0.3029(2) 0.1455(3) 0.0648(18) Uani 1 1 d . . . . .
H41 H 0.784850 0.318979 0.158192 0.078 Uiso 1 1 calc R U . . .
C42 C 0.9428(7) 0.3236(2) 0.1151(3) 0.082(2) Uani 1 1 d . . . . .
H42 H 0.936320 0.353691 0.107891 0.099 Uiso 1 1 calc R U . . .
C43 C 1.0386(6) 0.3009(3) 0.0962(3) 0.072(2) Uani 1 1 d . . . . .
H43 H 1.099973 0.315320 0.076217 0.086 Uiso 1 1 calc R U . . .
C44 C 1.0482(6) 0.2575(3) 0.1054(3) 0.0659(18) Uani 1 1 d . . . . .
H44 H 1.115138 0.241448 0.091811 0.079 Uiso 1 1 calc R U . . .
C45 C 0.9578(6) 0.23750(19) 0.1351(3) 0.0593(17) Uani 1 1 d . . . . .
H45 H 0.962179 0.207224 0.140602 0.071 Uiso 1 1 calc R U . . .
C50 C 0.6404(5) 0.25596(17) 0.1910(3) 0.0457(15) Uani 1 1 d . . . . .
C51 C 0.6075(6) 0.27416(18) 0.2438(3) 0.0664(19) Uani 1 1 d . . . . .
H51 H 0.670057 0.275312 0.284265 0.080 Uiso 1 1 calc R U . . .
C52 C 0.4803(8) 0.2911(2) 0.2377(4) 0.083(2) Uani 1 1 d . . . . .
H52 H 0.456830 0.303656 0.274579 0.100 Uiso 1 1 calc R U . . .
C53 C 0.3898(7) 0.2901(2) 0.1806(5) 0.091(3) Uani 1 1 d . . . . .
H53 H 0.303876 0.301731 0.177703 0.109 Uiso 1 1 calc R U . . .
C54 C 0.4221(7) 0.2724(2) 0.1270(4) 0.084(2) Uani 1 1 d . . . . .
H54 H 0.359732 0.271842 0.086499 0.101 Uiso 1 1 calc R U . . .
C55 C 0.5471(7) 0.25530(18) 0.1329(3) 0.0618(17) Uani 1 1 d . . . . .
H55 H 0.569734 0.242676 0.095941 0.074 Uiso 1 1 calc R U . . .
C60 C 0.3071(4) 0.13419(18) 0.1997(3) 0.0370(14) Uani 1 1 d . . . . .
C61 C 0.2789(5) 0.10474(18) 0.2428(3) 0.0456(15) Uani 1 1 d . . . . .
H61 H 0.288212 0.075008 0.234904 0.055 Uiso 1 1 calc R U . . .
C62 C 0.2367(5) 0.1176(2) 0.2984(3) 0.0563(17) Uani 1 1 d . . . . .
H62 H 0.217986 0.096753 0.327967 0.068 Uiso 1 1 calc R U . . .
C63 C 0.2225(5) 0.1603(3) 0.3097(3) 0.0665(19) Uani 1 1 d . . . . .
H63 H 0.193936 0.169257 0.347313 0.080 Uiso 1 1 calc R U . . .
C64 C 0.2492(6) 0.1903(2) 0.2672(4) 0.076(2) Uani 1 1 d . . . . .
H64 H 0.237708 0.219992 0.274884 0.091 Uiso 1 1 calc R U . . .
C65 C 0.2934(5) 0.1773(2) 0.2128(3) 0.0578(16) Uani 1 1 d . . . . .
H65 H 0.314441 0.198258 0.184100 0.069 Uiso 1 1 calc R U . . .
C66 C 0.2794(6) -0.02958(17) 0.0522(3) 0.0537(16) Uani 1 1 d . . . . .
C67 C 0.3364(6) -0.07420(16) 0.0589(3) 0.077(2) Uani 1 1 d . . . . .
H67A H 0.345479 -0.084096 0.103744 0.116 Uiso 1 1 calc R U . . .
H67B H 0.277269 -0.093607 0.029329 0.116 Uiso 1 1 calc R U . . .
H67C H 0.423644 -0.073947 0.048146 0.116 Uiso 1 1 calc R U . . .
C68 C 0.2662(7) -0.01496(19) -0.0166(3) 0.095(2) Uani 1 1 d . . . . .
H68A H 0.229075 0.014098 -0.021579 0.143 Uiso 1 1 calc R U . . .
H68B H 0.353626 -0.014887 -0.027156 0.143 Uiso 1 1 calc R U . . .
H68C H 0.207250 -0.034548 -0.045974 0.143 Uiso 1 1 calc R U . . .
C69 C 0.1365(6) -0.03195(19) 0.0655(3) 0.094(2) Uani 1 1 d . . . . .
H69A H 0.142116 -0.041462 0.110273 0.141 Uiso 1 1 calc R U . . .
H69B H 0.095240 -0.003501 0.059265 0.141 Uiso 1 1 calc R U . . .
H69C H 0.082894 -0.052384 0.035375 0.141 Uiso 1 1 calc R U . . .
C70 C 0.2479(5) 0.13584(15) 0.0790(3) 0.0394(14) Uani 1 1 d . . . . .
C71 C 0.2859(5) 0.15479(19) 0.0281(3) 0.0606(17) Uani 1 1 d . . . . .
H71 H 0.377711 0.159084 0.030569 0.073 Uiso 1 1 calc R U . . .
C72 C 0.1957(7) 0.1681(2) -0.0272(3) 0.081(2) Uani 1 1 d . . . . .
H72 H 0.225178 0.180556 -0.062490 0.098 Uiso 1 1 calc R U . . .
C73 C 0.0625(7) 0.1629(2) -0.0300(3) 0.0679(19) Uani 1 1 d . . . . .
H73 H -0.001121 0.172300 -0.067111 0.082 Uiso 1 1 calc R U . . .
C74 C 0.0226(5) 0.14446(18) 0.0203(3) 0.0570(17) Uani 1 1 d . . . . .
H74 H -0.069286 0.140640 0.018089 0.068 Uiso 1 1 calc R U . . .
C75 C 0.1129(5) 0.13120(16) 0.0744(3) 0.0474(15) Uani 1 1 d . . . . .
H75 H 0.082630 0.118605 0.109355 0.057 Uiso 1 1 calc R U . . .
C80 C 0.6507(6) 0.00636(15) 0.3058(3) 0.0414(14) Uani 1 1 d . . . . .
C81 C 0.7594(5) 0.00749(16) 0.3589(3) 0.0508(16) Uani 1 1 d . . . . .
H81 H 0.845547 0.010422 0.350772 0.061 Uiso 1 1 calc R U . . .
C82 C 0.7476(7) 0.00456(17) 0.4223(3) 0.0589(17) Uani 1 1 d . . . . .
H82 H 0.824090 0.005126 0.456905 0.071 Uiso 1 1 calc R U . . .
C83 C 0.6242(7) 0.00082(17) 0.4348(3) 0.0576(16) Uani 1 1 d . . . . .
H83 H 0.614145 -0.000783 0.478375 0.069 Uiso 1 1 calc R U . . .
C84 C 0.5149(6) -0.00059(18) 0.3843(3) 0.0619(17) Uani 1 1 d . . . . .
H84 H 0.429445 -0.003795 0.393140 0.074 Uiso 1 1 calc R U . . .
C85 C 0.5275(6) 0.00257(17) 0.3206(3) 0.0543(16) Uani 1 1 d . . . . .
H85 H 0.450243 0.002145 0.286439 0.065 Uiso 1 1 calc R U . . .
C90 C 0.7265(5) -0.03626(18) 0.2215(3) 0.0450(15) Uani 1 1 d . . . . .
C91 C 0.6957(7) -0.0751(2) 0.2459(3) 0.090(2) Uani 1 1 d . . . . .
H91 H 0.639747 -0.075524 0.275912 0.108 Uiso 1 1 calc R U . . .
C92 C 0.7441(9) -0.1130(2) 0.2278(4) 0.107(3) Uani 1 1 d . . . . .
H92 H 0.722229 -0.139300 0.245630 0.128 Uiso 1 1 calc R U . . .
C93 C 0.8246(8) -0.1132(3) 0.1836(4) 0.102(3) Uani 1 1 d . . . . .
H93 H 0.858719 -0.139400 0.170927 0.122 Uiso 1 1 calc R U . . .
C94 C 0.8537(7) -0.0752(3) 0.1588(3) 0.084(2) Uani 1 1 d . . . . .
H94 H 0.908927 -0.075093 0.128472 0.101 Uiso 1 1 calc R U . . .
C95 C 0.8064(6) -0.0370(2) 0.1760(3) 0.0638(18) Uani 1 1 d . . . . .
H95 H 0.827610 -0.011043 0.157120 0.077 Uiso 1 1 calc R U . . .
C1D C 0.7187(8) 0.1006(2) 0.7442(4) 0.131(3) Uani 1 1 d . . . . .
H1D1 H 0.732966 0.087336 0.787254 0.197 Uiso 1 1 calc R U . . .
H1D2 H 0.765177 0.128236 0.747619 0.197 Uiso 1 1 calc R U . . .
H1D3 H 0.623644 0.105313 0.727214 0.197 Uiso 1 1 calc R U . . .
C2D C 0.7711(7) 0.0716(3) 0.6991(5) 0.080(2) Uani 1 1 d . . . . .
C3D C 0.8250(7) 0.0324(3) 0.7201(4) 0.088(2) Uani 1 1 d . . . . .
H3D H 0.829940 0.023919 0.763745 0.106 Uiso 1 1 calc R U . . .
C4D C 0.8720(7) 0.0052(2) 0.6791(5) 0.089(2) Uani 1 1 d . . . . .
H4D H 0.909333 -0.021709 0.694574 0.107 Uiso 1 1 calc R U . . .
C5D C 0.8648(7) 0.0172(3) 0.6155(5) 0.091(2) Uani 1 1 d . . . . .
H5D H 0.896266 -0.001262 0.586483 0.109 Uiso 1 1 calc R U . . .
C6D C 0.8123(8) 0.0555(3) 0.5957(4) 0.093(2) Uani 1 1 d . . . . .
H6D H 0.808693 0.064134 0.552240 0.111 Uiso 1 1 calc R U . . .
C7D C 0.7643(8) 0.0822(2) 0.6350(5) 0.090(2) Uani 1 1 d . . . . .
H7D H 0.725323 0.108685 0.618424 0.109 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
Na1 O1 2.304(4) . ?
Na1 O2 2.316(4) . ?
Na1 C60 2.711(5) . ?
Na1 C20 2.757(5) . ?
Na1 C21 2.814(6) . ?
Na1 C61 2.834(5) . ?
Na1 C65 2.884(6) . ?
Na1 C25 3.041(6) . ?
Na1 Al1 3.148(3) . ?
Al1 O2 1.806(3) . ?
Al1 O1 1.801(3) . ?
Al1 C2 1.938(5) . ?
Al1 C1 1.962(5) . ?
O1 C11 1.354(5) . ?
O2 C3 1.365(5) . ?
C3 C4 1.402(6) . ?
C3 C8 1.409(6) . ?
C4 C5 1.397(6) . ?
C4 C9 1.516(6) . ?
C5 C6 1.392(6) . ?
C6 C7 1.391(6) . ?
C6 C66 1.518(7) . ?
C7 C8 1.376(6) . ?
C8 C10 1.498(6) . ?
C9 C80 1.508(7) . ?
C9 C90 1.511(7) . ?
C10 C60 1.518(7) . ?
C10 C70 1.515(6) . ?
C11 C16 1.397(6) . ?
C11 C12 1.424(6) . ?
C12 C13 1.394(6) . ?
C12 C18 1.518(6) . ?
C13 C14 1.365(6) . ?
C14 C15 1.400(6) . ?
C14 C26 1.519(6) . ?
C15 C16 1.391(6) . ?
C16 C17 1.520(6) . ?
C17 C40 1.527(7) . ?
C17 C50 1.529(7) . ?
C18 C30 1.517(6) . ?
C18 C20 1.542(6) . ?
C20 C25 1.374(6) . ?
C20 C21 1.375(6) . ?
C21 C22 1.390(7) . ?
C22 C23 1.364(7) . ?
C23 C24 1.350(7) . ?
C24 C25 1.401(7) . ?
C26 C29 1.508(7) . ?
C26 C27 1.526(7) . ?
C26 C28 1.513(7) . ?
C30 C31 1.378(6) . ?
C30 C35 1.384(7) . ?
C31 C32 1.376(7) . ?
C32 C33 1.381(7) . ?
C33 C34 1.368(7) . ?
C34 C35 1.380(7) . ?
C40 C41 1.362(7) . ?
C40 C45 1.368(7) . ?
C41 C42 1.400(7) . ?
C42 C43 1.350(7) . ?
C43 C44 1.368(7) . ?
C44 C45 1.386(7) . ?
C50 C55 1.381(7) . ?
C50 C51 1.362(7) . ?
C51 C52 1.398(8) . ?
C52 C53 1.352(8) . ?
C53 C54 1.367(9) . ?
C54 C55 1.379(8) . ?
C60 C65 1.384(6) . ?
C60 C61 1.371(6) . ?
C61 C62 1.399(7) . ?
C62 C63 1.367(7) . ?
C63 C64 1.365(8) . ?
C64 C65 1.391(7) . ?
C66 C68 1.499(7) . ?
C66 C67 1.504(7) . ?
C66 C69 1.569(7) . ?
C70 C71 1.359(7) . ?
C70 C75 1.388(6) . ?
C71 C72 1.386(7) . ?
C72 C73 1.377(7) . ?
C73 C74 1.352(7) . ?
C74 C75 1.368(7) . ?
C80 C85 1.385(7) . ?
C80 C81 1.401(7) . ?
C81 C82 1.374(7) . ?
C82 C83 1.367(7) . ?
C83 C84 1.371(7) . ?
C84 C85 1.384(7) . ?
C90 C91 1.380(7) . ?
C90 C95 1.401(7) . ?
C91 C92 1.372(8) . ?
C92 C93 1.384(9) . ?
C93 C94 1.356(8) . ?
C94 C95 1.365(7) . ?
C1D C2D 1.501(9) . ?
C2D C7D 1.380(9) . ?
C2D C3D 1.374(8) . ?
C3D C4D 1.375(8) . ?
C4D C5D 1.382(9) . ?
C5D C6D 1.338(9) . ?
C6D C7D 1.347(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Na1 O2 68.85(12) . . ?
O1 Na1 C60 117.08(17) . . ?
O2 Na1 C60 75.39(14) . . ?
O1 Na1 C20 77.25(15) . . ?
O2 Na1 C20 115.82(16) . . ?
C60 Na1 C20 165.09(18) . . ?
O1 Na1 C21 100.15(16) . . ?
O2 Na1 C21 109.68(15) . . ?
C60 Na1 C21 140.76(19) . . ?
C20 Na1 C21 28.55(13) . . ?
O1 Na1 C61 140.67(17) . . ?
O2 Na1 C61 79.53(15) . . ?
C60 Na1 C61 28.52(14) . . ?
C20 Na1 C61 139.71(19) . . ?
C21 Na1 C61 112.44(19) . . ?
O1 Na1 C65 112.95(16) . . ?
O2 Na1 C65 98.97(17) . . ?
C60 Na1 C65 28.43(13) . . ?
C20 Na1 C65 144.80(19) . . ?
C21 Na1 C65 142.35(19) . . ?
C61 Na1 C65 48.76(16) . . ?
O1 Na1 C25 82.04(14) . . ?
O2 Na1 C25 139.53(15) . . ?
C60 Na1 C25 144.76(17) . . ?
C20 Na1 C25 26.85(13) . . ?
C21 Na1 C25 47.45(15) . . ?
C61 Na1 C25 136.47(17) . . ?
C65 Na1 C25 118.47(19) . . ?
O1 Na1 Al1 34.38(9) . . ?
O2 Na1 Al1 34.55(8) . . ?
C60 Na1 Al1 95.82(14) . . ?
C20 Na1 Al1 98.79(13) . . ?
C21 Na1 Al1 109.76(14) . . ?
C61 Na1 Al1 110.38(14) . . ?
C65 Na1 Al1 107.70(15) . . ?
C25 Na1 Al1 112.94(13) . . ?
O2 Al1 O1 92.75(15) . . ?
O2 Al1 C2 117.40(19) . . ?
O1 Al1 C2 108.9(2) . . ?
O2 Al1 C1 107.77(19) . . ?
O1 Al1 C1 118.01(19) . . ?
C2 Al1 C1 111.2(2) . . ?
O2 Al1 Na1 46.63(11) . . ?
O1 Al1 Na1 46.23(11) . . ?
C2 Al1 Na1 127.16(19) . . ?
C1 Al1 Na1 121.64(17) . . ?
C11 O1 Al1 128.4(3) . . ?
C11 O1 Na1 129.6(3) . . ?
Al1 O1 Na1 99.40(15) . . ?
C3 O2 Al1 124.9(3) . . ?
C3 O2 Na1 131.6(3) . . ?
Al1 O2 Na1 98.82(15) . . ?
O2 C3 C4 119.9(5) . . ?
O2 C3 C8 119.8(5) . . ?
C4 C3 C8 120.3(5) . . ?
C3 C4 C5 118.1(5) . . ?
C3 C4 C9 120.2(5) . . ?
C5 C4 C9 121.7(5) . . ?
C6 C5 C4 123.2(5) . . ?
C5 C6 C7 115.9(4) . . ?
C5 C6 C66 122.3(5) . . ?
C7 C6 C66 121.8(5) . . ?
C6 C7 C8 124.0(5) . . ?
C7 C8 C3 118.2(5) . . ?
C7 C8 C10 122.8(5) . . ?
C3 C8 C10 118.9(5) . . ?
C80 C9 C4 113.1(4) . . ?
C80 C9 C90 110.9(4) . . ?
C4 C9 C90 113.3(4) . . ?
C60 C10 C8 111.9(4) . . ?
C60 C10 C70 110.1(4) . . ?
C8 C10 C70 115.3(4) . . ?
O1 C11 C16 122.2(5) . . ?
O1 C11 C12 119.7(5) . . ?
C16 C11 C12 117.9(5) . . ?
C13 C12 C11 119.3(5) . . ?
C13 C12 C18 122.9(5) . . ?
C11 C12 C18 117.8(5) . . ?
C14 C13 C12 123.5(5) . . ?
C15 C14 C13 116.5(4) . . ?
C15 C14 C26 121.7(5) . . ?
C13 C14 C26 121.7(5) . . ?
C14 C15 C16 122.6(5) . . ?
C15 C16 C11 120.1(5) . . ?
C15 C16 C17 122.0(5) . . ?
C11 C16 C17 117.8(5) . . ?
C40 C17 C16 110.5(4) . . ?
C40 C17 C50 114.1(4) . . ?
C16 C17 C50 112.8(4) . . ?
C30 C18 C12 112.4(4) . . ?
C30 C18 C20 111.6(4) . . ?
C12 C18 C20 111.5(4) . . ?
C25 C20 C21 118.7(5) . . ?
C25 C20 C18 122.2(5) . . ?
C21 C20 C18 119.1(5) . . ?
C25 C20 Na1 88.2(3) . . ?
C21 C20 Na1 78.0(3) . . ?
C18 C20 Na1 102.7(3) . . ?
C20 C21 C22 121.4(5) . . ?
C20 C21 Na1 73.4(3) . . ?
C22 C21 Na1 92.0(3) . . ?
C23 C22 C21 118.5(6) . . ?
C22 C23 C24 121.8(6) . . ?
C23 C24 C25 119.4(6) . . ?
C20 C25 C24 120.2(5) . . ?
C20 C25 Na1 65.0(3) . . ?
C24 C25 Na1 91.8(3) . . ?
C29 C26 C14 113.6(5) . . ?
C29 C26 C27 108.0(4) . . ?
C14 C26 C27 108.4(4) . . ?
C29 C26 C28 107.4(5) . . ?
C14 C26 C28 110.5(4) . . ?
C27 C26 C28 108.8(5) . . ?
C31 C30 C35 116.6(5) . . ?
C31 C30 C18 124.2(5) . . ?
C35 C30 C18 119.2(5) . . ?
C30 C31 C32 121.8(5) . . ?
C31 C32 C33 120.0(6) . . ?
C34 C33 C32 119.9(6) . . ?
C33 C34 C35 118.9(6) . . ?
C34 C35 C30 122.8(6) . . ?
C41 C40 C45 118.3(5) . . ?
C41 C40 C17 123.6(5) . . ?
C45 C40 C17 118.0(5) . . ?
C40 C41 C42 120.1(6) . . ?
C43 C42 C41 120.3(6) . . ?
C42 C43 C44 120.6(6) . . ?
C45 C44 C43 118.3(6) . . ?
C44 C45 C40 122.2(6) . . ?
C55 C50 C51 118.7(6) . . ?
C55 C50 C17 118.9(6) . . ?
C51 C50 C17 122.4(5) . . ?
C50 C51 C52 119.0(6) . . ?
C53 C52 C51 121.6(7) . . ?
C52 C53 C54 120.0(7) . . ?
C53 C54 C55 118.7(7) . . ?
C50 C55 C54 122.0(6) . . ?
C65 C60 C61 117.9(5) . . ?
C65 C60 C10 118.2(5) . . ?
C61 C60 C10 123.8(5) . . ?
C65 C60 Na1 82.7(3) . . ?
C61 C60 Na1 80.7(3) . . ?
C10 C60 Na1 106.6(3) . . ?
C60 C61 C62 121.4(5) . . ?
C60 C61 Na1 70.8(3) . . ?
C62 C61 Na1 89.4(3) . . ?
C63 C62 C61 119.4(5) . . ?
C62 C63 C64 120.5(6) . . ?
C65 C64 C63 119.7(6) . . ?
C64 C65 C60 121.2(6) . . ?
C64 C65 Na1 90.4(4) . . ?
C60 C65 Na1 68.8(3) . . ?
C68 C66 C67 108.8(5) . . ?
C68 C66 C6 110.0(5) . . ?
C67 C66 C6 113.8(5) . . ?
C68 C66 C69 107.7(5) . . ?
C67 C66 C69 107.8(5) . . ?
C6 C66 C69 108.6(5) . . ?
C71 C70 C75 117.1(5) . . ?
C71 C70 C10 119.8(5) . . ?
C75 C70 C10 123.1(5) . . ?
C70 C71 C72 122.5(5) . . ?
C73 C72 C71 118.8(6) . . ?
C74 C73 C72 119.7(6) . . ?
C73 C74 C75 120.9(5) . . ?
C74 C75 C70 121.1(5) . . ?
C85 C80 C81 115.9(5) . . ?
C85 C80 C9 123.4(5) . . ?
C81 C80 C9 120.5(5) . . ?
C82 C81 C80 123.2(5) . . ?
C81 C82 C83 119.0(6) . . ?
C82 C83 C84 119.8(6) . . ?
C85 C84 C83 120.9(6) . . ?
C84 C85 C80 121.2(5) . . ?
C91 C90 C95 117.6(5) . . ?
C91 C90 C9 123.6(6) . . ?
C95 C90 C9 118.6(6) . . ?
C90 C91 C92 121.4(6) . . ?
C91 C92 C93 120.4(7) . . ?
C94 C93 C92 118.4(7) . . ?
C95 C94 C93 122.3(6) . . ?
C94 C95 C90 120.0(6) . . ?
C7D C2D C3D 117.2(7) . . ?
C7D C2D C1D 122.2(9) . . ?
C3D C2D C1D 120.6(9) . . ?
C4D C3D C2D 121.3(8) . . ?
C3D C4D C5D 119.7(7) . . ?
C6D C5D C4D 118.3(8) . . ?
C5D C6D C7D 122.6(8) . . ?
C2D C7D C6D 120.8(7) . . ?

_refine_diff_density_max         0.283
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.045

####################################################################### 
# 
# 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_3c_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1897467'
loop_
_audit_author_name
_audit_author_address
'Marta E. G. Mosquera'
;University of Alcala
Spain
;
_audit_update_record             
;
2019-03-24 deposited with the CCDC.	2019-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT201_3c                  
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          1 Report
RESPONSE: Cooresponds to a disordered toluene molecule
;
# Added during the CSD deposition process: Sunday 24 March 2019 08:06 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H72 Al K O2.C7 H8'
_chemical_formula_sum            'C81 H80 Al K O2'
_chemical_formula_weight         1151.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   14.728
_cell_length_b                   24.467
_cell_length_c                   18.957
_cell_angle_alpha                90
_cell_angle_beta                 99.84
_cell_angle_gamma                90
_cell_volume                     6730.9
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    266
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      19.45

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.37
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_F_000             2456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_T_max  0.970

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'

_diffrn_reflns_number            29613
_diffrn_reflns_av_unetI/netI     0.0945
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.150
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             15395
_reflns_number_gt                8426
_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    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1201P)²+1.0062P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15395
_refine_ls_number_parameters     731
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0748
_refine_ls_wR_factor_ref         0.2346
_refine_ls_wR_factor_gt          0.2029
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.18869(5) 0.69105(3) 0.46090(4) 0.0313(2) Uani 1 1 d . . . . .
K1 K 0.32301(6) 0.67213(3) 0.32087(4) 0.0646(3) Uani 1 1 d . . . . .
O2 O 0.14412(11) 0.66745(7) 0.37216(10) 0.0302(4) Uani 1 1 d . . . . .
O1 O 0.30343(11) 0.70616(7) 0.44599(9) 0.0305(4) Uani 1 1 d . . . . .
C42 C -0.08306(17) 0.56224(10) 0.32198(15) 0.0318(6) Uani 1 1 d . . . . .
C1 C 0.1364(2) 0.75944(13) 0.49313(19) 0.0531(8) Uani 1 1 d . . . . .
H1A H 0.165805 0.767636 0.541163 0.080 Uiso 1 1 calc R U . . .
H1B H 0.146790 0.788885 0.461993 0.080 Uiso 1 1 calc R U . . .
H1C H 0.071442 0.754923 0.491866 0.080 Uiso 1 1 calc R U . . .
C2 C 0.1769(2) 0.63092(14) 0.52720(17) 0.0477(8) Uani 1 1 d . . . . .
H2A H 0.200305 0.642362 0.575314 0.072 Uiso 1 1 calc R U . . .
H2B H 0.113204 0.620987 0.523349 0.072 Uiso 1 1 calc R U . . .
H2C H 0.211496 0.599976 0.515380 0.072 Uiso 1 1 calc R U . . .
C41 C 0.00697(17) 0.54341(10) 0.32776(14) 0.0301(6) Uani 1 1 d . . . . .
H41 H 0.016679 0.506353 0.321042 0.036 Uiso 1 1 calc R U . . .
C43 C -0.09409(18) 0.61824(10) 0.33124(15) 0.0337(6) Uani 1 1 d . . . . .
H43 H -0.153497 0.632268 0.326631 0.040 Uiso 1 1 calc R U . . .
C40 C 0.08288(17) 0.57758(10) 0.34314(13) 0.0286(5) Uani 1 1 d . . . . .
C39 C 0.06999(17) 0.63332(10) 0.35543(13) 0.0275(5) Uani 1 1 d . . . . .
C55 C 0.21517(18) 0.57225(10) 0.27320(15) 0.0334(6) Uani 1 1 d . . . . .
C45 C -0.16648(19) 0.52383(11) 0.30868(18) 0.0435(7) Uani 1 1 d . . . . .
C44 C -0.02032(17) 0.65384(10) 0.34703(14) 0.0301(6) Uani 1 1 d . . . . .
C49 C 0.17960(17) 0.55576(10) 0.34187(14) 0.0303(6) Uani 1 1 d . . . . .
H49 H 0.220424 0.573183 0.381795 0.036 Uiso 1 1 calc R U . . .
C53 C 0.2079(2) 0.62567(15) 0.16506(18) 0.0552(9) Uani 1 1 d . . . . .
H53 H 0.175774 0.649726 0.131836 0.066 Uiso 1 1 calc R U . . .
C57 C 0.16373(19) 0.45731(11) 0.29867(18) 0.0429(7) Uani 1 1 d . . . . .
H57 H 0.147323 0.470040 0.252008 0.051 Uiso 1 1 calc R U . . .
C54 C 0.1682(2) 0.60776(13) 0.22277(15) 0.0430(7) Uani 1 1 d . . . . .
H54 H 0.109671 0.619796 0.227438 0.052 Uiso 1 1 calc R U . . .
C50 C 0.3011(2) 0.55358(12) 0.26253(19) 0.0476(8) Uani 1 1 d . . . . .
H50 H 0.332866 0.528544 0.294535 0.057 Uiso 1 1 calc R U . . .
C56 C 0.18693(17) 0.49435(11) 0.35489(16) 0.0355(6) Uani 1 1 d . . . . .
C52 C 0.2945(2) 0.60786(14) 0.15705(19) 0.0559(9) Uani 1 1 d . . . . .
H52 H 0.321465 0.620442 0.119212 0.067 Uiso 1 1 calc R U . . .
C46 C -0.2382(2) 0.54536(15) 0.2490(2) 0.0721(12) Uani 1 1 d . . . . .
H46A H -0.253415 0.582295 0.259449 0.108 Uiso 1 1 calc R U . . .
H46B H -0.214397 0.544490 0.204918 0.108 Uiso 1 1 calc R U . . .
H46C H -0.292441 0.523023 0.244571 0.108 Uiso 1 1 calc R U . . .
C51 C 0.3402(2) 0.57143(14) 0.2054(2) 0.0581(9) Uani 1 1 d . . . . .
H51 H 0.398027 0.558648 0.199783 0.070 Uiso 1 1 calc R U . . .
C61 C 0.2132(2) 0.47401(13) 0.42284(19) 0.0492(8) Uani 1 1 d . . . . .
H61 H 0.230006 0.497973 0.460916 0.059 Uiso 1 1 calc R U . . .
C58 C 0.1651(2) 0.40159(13) 0.3122(2) 0.0563(9) Uani 1 1 d . . . . .
H58 H 0.148478 0.377126 0.274673 0.068 Uiso 1 1 calc R U . . .
C60 C 0.2148(3) 0.41820(15) 0.4353(2) 0.0667(10) Uani 1 1 d . . . . .
H60 H 0.232651 0.404975 0.481585 0.080 Uiso 1 1 calc R U . . .
C47 C -0.2091(3) 0.52233(17) 0.3782(2) 0.0741(12) Uani 1 1 d . . . . .
H47A H -0.164337 0.508671 0.416992 0.111 Uiso 1 1 calc R U . . .
H47B H -0.227283 0.558560 0.389374 0.111 Uiso 1 1 calc R U . . .
H47C H -0.262098 0.498822 0.371194 0.111 Uiso 1 1 calc R U . . .
C59 C 0.1905(3) 0.38258(14) 0.3800(3) 0.0653(11) Uani 1 1 d . . . . .
H59 H 0.191301 0.345171 0.388787 0.078 Uiso 1 1 calc R U . . .
C48 C -0.1404(2) 0.46558(13) 0.2944(3) 0.0708(12) Uani 1 1 d . . . . .
H48A H -0.094661 0.452908 0.333177 0.106 Uiso 1 1 calc R U . . .
H48B H -0.193982 0.442702 0.290243 0.106 Uiso 1 1 calc R U . . .
H48C H -0.115939 0.464169 0.250590 0.106 Uiso 1 1 calc R U . . .
C7D C 0.0033(6) 0.9231(5) 0.4224(6) 0.199(4) Uani 1 1 d D . . . .
H7D H 0.065877 0.916923 0.423710 0.239 Uiso 1 1 calc R U . . .
C63 C -0.12820(18) 0.73090(10) 0.36877(16) 0.0355(6) Uani 1 1 d . . . . .
C62 C -0.03648(18) 0.71526(10) 0.34727(16) 0.0353(6) Uani 1 1 d . . . . .
H62 H 0.011529 0.730226 0.384442 0.042 Uiso 1 1 calc R U . . .
C64 C -0.1953(2) 0.76012(12) 0.32393(17) 0.0431(7) Uani 1 1 d . . . . .
H64 H -0.184973 0.770672 0.278834 0.052 Uiso 1 1 calc R U . . .
C66 C -0.2949(2) 0.75842(14) 0.4118(2) 0.0569(9) Uani 1 1 d . . . . .
H66 H -0.350388 0.767591 0.426007 0.068 Uiso 1 1 calc R U . . .
C68 C -0.1463(2) 0.71619(13) 0.43509(19) 0.0521(8) Uani 1 1 d . . . . .
H68 H -0.101833 0.696951 0.466124 0.063 Uiso 1 1 calc R U . . .
C65 C -0.2777(2) 0.77378(14) 0.3457(2) 0.0540(9) Uani 1 1 d . . . . .
H65 H -0.321891 0.793582 0.315131 0.065 Uiso 1 1 calc R U . . .
C67 C -0.2289(3) 0.72921(14) 0.4570(2) 0.0620(10) Uani 1 1 d . . . . .
H67 H -0.239682 0.718320 0.501876 0.074 Uiso 1 1 calc R U . . .
C69 C -0.0206(2) 0.74069(12) 0.2768(2) 0.0496(8) Uani 1 1 d . . . . .
C70 C -0.0407(3) 0.71345(16) 0.2115(2) 0.0680(11) Uani 1 1 d . . . . .
H70 H -0.063361 0.677935 0.210688 0.082 Uiso 1 1 calc R U . . .
C71 C -0.0282(4) 0.7374(2) 0.1482(3) 0.0896(15) Uani 1 1 d . . . . .
H71 H -0.042723 0.718013 0.105525 0.108 Uiso 1 1 calc R U . . .
C74 C 0.0123(2) 0.79335(14) 0.2756(3) 0.0690(11) Uani 1 1 d . . . . .
H74 H 0.025834 0.813115 0.317998 0.083 Uiso 1 1 calc R U . . .
C73 C 0.0258(3) 0.81763(19) 0.2103(3) 0.0850(16) Uani 1 1 d . . . . .
H73 H 0.048591 0.853035 0.209647 0.102 Uiso 1 1 calc R U . . .
C72 C 0.0045(4) 0.7880(2) 0.1477(4) 0.0978(17) Uani 1 1 d . . . . .
H72 H 0.013189 0.803661 0.104677 0.117 Uiso 1 1 calc R U . . .
C3D C -0.1305(5) 0.9768(3) 0.3972(4) 0.135(2) Uiso 1 1 d D . . . .
H3D H -0.159688 1.009914 0.384165 0.162 Uiso 1 1 calc R U . . .
C2D C -0.0384(6) 0.9730(3) 0.4037(4) 0.142(2) Uiso 1 1 d D . . . .
C4D C -0.1845(6) 0.9296(3) 0.4105(4) 0.158(3) Uiso 1 1 d D . . . .
H4D H -0.248199 0.929950 0.396758 0.189 Uiso 1 1 calc R U . . .
C5D C -0.1421(8) 0.8848(4) 0.4429(5) 0.195(4) Uiso 1 1 d D . . . .
H5D H -0.171508 0.857927 0.465305 0.234 Uiso 1 1 calc R U . . .
C1D C 0.0156(8) 1.0194(4) 0.3852(6) 0.215(4) Uiso 1 1 d . . . . .
H1D1 H 0.079707 1.009747 0.392899 0.322 Uiso 1 1 calc R U . . .
H1D2 H -0.004162 1.028848 0.335836 0.322 Uiso 1 1 calc R U . . .
H1D3 H 0.006670 1.050088 0.414851 0.322 Uiso 1 1 calc R U . . .
C6D C -0.0550(11) 0.8843(6) 0.4387(7) 0.242(6) Uiso 1 1 d D . . . .
H6D H -0.027241 0.850432 0.448842 0.291 Uiso 1 1 calc R U . . .
C4 C 0.38560(18) 0.78954(10) 0.47758(14) 0.0301(6) Uani 1 1 d . . . . .
C5 C 0.45833(18) 0.81601(10) 0.51999(14) 0.0313(6) Uani 1 1 d . . . . .
H5 H 0.465137 0.853413 0.513930 0.038 Uiso 1 1 calc R U . . .
C26 C 0.43190(18) 0.64291(10) 0.53735(15) 0.0312(6) Uani 1 1 d . . . . .
H26 H 0.366127 0.633913 0.527090 0.037 Uiso 1 1 calc R U . . .
C7 C 0.51035(17) 0.73340(10) 0.57742(14) 0.0302(6) Uani 1 1 d . . . . .
H7 H 0.552751 0.714184 0.610216 0.036 Uiso 1 1 calc R U . . .
C8 C 0.43823(17) 0.70499(10) 0.53660(14) 0.0275(5) Uani 1 1 d . . . . .
C9 C 0.59957(18) 0.82188(11) 0.61652(15) 0.0370(6) Uani 1 1 d . . . . .
C3 C 0.37369(17) 0.73318(10) 0.48743(13) 0.0279(5) Uani 1 1 d . . . . .
C20 C 0.33918(19) 0.80035(10) 0.34377(15) 0.0353(6) Uani 1 1 d . . . . .
C33 C 0.46969(18) 0.61735(10) 0.60998(15) 0.0327(6) Uani 1 1 d . . . . .
C6 C 0.52143(18) 0.78926(10) 0.57108(14) 0.0311(6) Uani 1 1 d . . . . .
C13 C 0.32238(19) 0.81873(10) 0.41728(15) 0.0338(6) Uani 1 1 d . . . . .
H13 H 0.259197 0.808042 0.420848 0.041 Uiso 1 1 calc R U . . .
C38 C 0.4079(2) 0.60146(11) 0.65425(16) 0.0382(7) Uani 1 1 d . . . . .
H38 H 0.344968 0.605738 0.638542 0.046 Uiso 1 1 calc R U . . .
C27 C 0.47444(19) 0.61826(11) 0.47712(15) 0.0360(6) Uani 1 1 d . . . . .
C14 C 0.3272(2) 0.88065(11) 0.42491(16) 0.0443(7) Uani 1 1 d . . . . .
C37 C 0.4389(2) 0.57949(13) 0.72103(17) 0.0471(7) Uani 1 1 d . . . . .
H37 H 0.396780 0.568791 0.749726 0.056 Uiso 1 1 calc R U . . .
C34 C 0.5625(2) 0.60968(11) 0.63469(17) 0.0410(7) Uani 1 1 d . . . . .
H34 H 0.604888 0.619030 0.605532 0.049 Uiso 1 1 calc R U . . .
C35 C 0.5936(2) 0.58839(12) 0.70187(18) 0.0478(8) Uani 1 1 d . . . . .
H35 H 0.656486 0.584130 0.718008 0.057 Uiso 1 1 calc R U . . .
C11 C 0.6566(2) 0.85098(15) 0.5677(2) 0.0598(9) Uani 1 1 d . . . . .
H11A H 0.617201 0.874256 0.535006 0.090 Uiso 1 1 calc R U . . .
H11B H 0.703498 0.872619 0.596169 0.090 Uiso 1 1 calc R U . . .
H11C H 0.684880 0.824362 0.541197 0.090 Uiso 1 1 calc R U . . .
C28 C 0.5304(2) 0.64693(13) 0.43882(19) 0.0505(8) Uani 1 1 d . . . . .
H28 H 0.544428 0.683164 0.450894 0.061 Uiso 1 1 calc R U . . .
C32 C 0.4563(2) 0.56384(12) 0.45740(17) 0.0481(8) Uani 1 1 d . . . . .
H32 H 0.418998 0.543062 0.481977 0.058 Uiso 1 1 calc R U . . .
C30 C 0.5470(3) 0.57019(15) 0.3643(2) 0.0612(9) Uani 1 1 d . . . . .
H30 H 0.570258 0.554223 0.326577 0.073 Uiso 1 1 calc R U . . .
C23 C 0.3621(3) 0.76549(14) 0.20753(19) 0.0584(9) Uani 1 1 d . . . . .
H23 H 0.369850 0.753683 0.162296 0.070 Uiso 1 1 calc R U . . .
C25 C 0.4254(2) 0.78650(12) 0.32997(18) 0.0455(7) Uani 1 1 d . . . . .
H25 H 0.476463 0.788595 0.366300 0.055 Uiso 1 1 calc R U . . .
C36 C 0.5311(2) 0.57337(12) 0.74523(18) 0.0495(8) Uani 1 1 d . . . . .
H36 H 0.551825 0.559171 0.790631 0.059 Uiso 1 1 calc R U . . .
C31 C 0.4923(3) 0.54040(14) 0.4025(2) 0.0630(10) Uani 1 1 d . . . . .
H31 H 0.479760 0.503934 0.390946 0.076 Uiso 1 1 calc R U . . .
C12 C 0.6648(3) 0.78598(16) 0.6666(2) 0.0724(12) Uani 1 1 d . . . . .
H12A H 0.692310 0.759584 0.639244 0.109 Uiso 1 1 calc R U . . .
H12B H 0.712203 0.808143 0.693644 0.109 Uiso 1 1 calc R U . . .
H12C H 0.631398 0.767413 0.698698 0.109 Uiso 1 1 calc R U . . .
C24 C 0.4361(3) 0.76933(14) 0.2615(2) 0.0581(9) Uani 1 1 d . . . . .
H24 H 0.494516 0.760415 0.252595 0.070 Uiso 1 1 calc R U . . .
C29 C 0.5667(3) 0.62345(16) 0.3826(2) 0.0651(10) Uani 1 1 d . . . . .
H29 H 0.603998 0.643932 0.357737 0.078 Uiso 1 1 calc R U . . .
C21 C 0.2650(2) 0.79670(14) 0.28793(16) 0.0488(8) Uani 1 1 d . . . . .
H21 H 0.206427 0.806200 0.295739 0.059 Uiso 1 1 calc R U . . .
C15 C 0.3943(3) 0.91149(13) 0.40165(18) 0.0652(11) Uani 1 1 d . . . . .
H15 H 0.435974 0.894749 0.376801 0.078 Uiso 1 1 calc R U . . .
C16 C 0.4007(4) 0.96751(16) 0.4148(2) 0.0919(16) Uani 1 1 d . . . . .
H16 H 0.447282 0.987813 0.399804 0.110 Uiso 1 1 calc R U . . .
C19 C 0.2640(3) 0.90631(15) 0.4600(2) 0.0719(11) Uani 1 1 d . . . . .
H19 H 0.217959 0.886054 0.475814 0.086 Uiso 1 1 calc R U . . .
C10 C 0.5559(3) 0.86369(17) 0.6595(2) 0.0727(12) Uani 1 1 d . . . . .
H10A H 0.514535 0.886409 0.627486 0.109 Uiso 1 1 calc R U . . .
H10B H 0.522397 0.845190 0.691554 0.109 Uiso 1 1 calc R U . . .
H10C H 0.603201 0.885920 0.686499 0.109 Uiso 1 1 calc R U . . .
C22 C 0.2772(3) 0.77903(15) 0.22045(18) 0.0612(10) Uani 1 1 d . . . . .
H22 H 0.226565 0.776473 0.183826 0.073 Uiso 1 1 calc R U . . .
C17 C 0.3396(4) 0.9920(3) 0.4492(3) 0.1001(16) Uiso 1 1 d . . . . .
H17 H 0.344784 1.029391 0.458110 0.120 Uiso 1 1 calc R U . . .
C18 C 0.2695(4) 0.9634(2) 0.4718(3) 0.1091(19) Uani 1 1 d . . . . .
H18 H 0.226584 0.981269 0.494268 0.131 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 1.7934(19) . ?
Al1 O1 1.7988(18) . ?
Al1 C2 1.962(3) . ?
Al1 C1 1.981(3) . ?
Al1 K1 3.6014(11) . ?
K1 O1 2.5761(19) . ?
K1 O2 2.9625(19) . ?
K1 C55 2.970(3) . ?
K1 C50 3.102(3) . ?
K1 C54 3.112(3) . ?
K1 C25 3.170(3) . ?
K1 C20 3.170(3) . ?
K1 C21 3.198(3) . ?
K1 C24 3.216(3) . ?
K1 C22 3.237(4) . ?
K1 C23 3.254(3) . ?
K1 C51 3.334(4) . ?
O2 C39 1.368(3) . ?
O1 C3 1.359(3) . ?
C42 C41 1.390(3) . ?
C42 C43 1.394(4) . ?
C42 C45 1.533(4) . ?
C41 C40 1.387(3) . ?
C43 C44 1.385(4) . ?
C40 C39 1.402(3) . ?
C40 C49 1.525(3) . ?
C39 C44 1.405(3) . ?
C55 C54 1.386(4) . ?
C55 C50 1.393(4) . ?
C55 C49 1.538(4) . ?
C45 C46 1.505(5) . ?
C45 C48 1.513(4) . ?
C45 C47 1.554(5) . ?
C44 C62 1.522(3) . ?
C49 C56 1.524(3) . ?
C53 C52 1.381(5) . ?
C53 C54 1.396(4) . ?
C57 C58 1.387(4) . ?
C57 C56 1.396(4) . ?
C50 C51 1.381(5) . ?
C56 C61 1.373(4) . ?
C52 C51 1.371(5) . ?
C61 C60 1.385(5) . ?
C58 C59 1.359(5) . ?
C60 C59 1.363(6) . ?
C7D C6D 1.351(12) . ?
C7D C2D 1.384(11) . ?
C63 C68 1.377(4) . ?
C63 C64 1.387(4) . ?
C63 C62 1.525(4) . ?
C62 C69 1.527(4) . ?
C64 C65 1.389(4) . ?
C66 C65 1.373(5) . ?
C66 C67 1.381(5) . ?
C68 C67 1.389(5) . ?
C69 C74 1.378(5) . ?
C69 C70 1.392(5) . ?
C70 C71 1.376(6) . ?
C71 C72 1.331(7) . ?
C74 C73 1.417(6) . ?
C73 C72 1.380(7) . ?
C3D C2D 1.345(8) . ?
C3D C4D 1.449(9) . ?
C2D C1D 1.463(11) . ?
C4D C5D 1.354(10) . ?
C5D C6D 1.298(14) . ?
C4 C5 1.385(4) . ?
C4 C3 1.407(3) . ?
C4 C13 1.523(4) . ?
C5 C6 1.386(4) . ?
C26 C27 1.518(4) . ?
C26 C8 1.522(3) . ?
C26 C33 1.528(4) . ?
C7 C6 1.384(3) . ?
C7 C8 1.389(4) . ?
C8 C3 1.395(4) . ?
C9 C12 1.511(5) . ?
C9 C10 1.517(5) . ?
C9 C11 1.528(4) . ?
C9 C6 1.538(4) . ?
C20 C25 1.382(4) . ?
C20 C21 1.388(4) . ?
C20 C13 1.524(4) . ?
C33 C34 1.380(4) . ?
C33 C38 1.394(4) . ?
C13 C14 1.522(4) . ?
C38 C37 1.379(4) . ?
C27 C28 1.380(4) . ?
C27 C32 1.396(4) . ?
C14 C15 1.374(5) . ?
C14 C19 1.384(5) . ?
C37 C36 1.365(4) . ?
C34 C35 1.380(4) . ?
C35 C36 1.385(5) . ?
C28 C29 1.394(5) . ?
C32 C31 1.372(5) . ?
C30 C29 1.367(5) . ?
C30 C31 1.380(5) . ?
C23 C22 1.356(5) . ?
C23 C24 1.365(5) . ?
C25 C24 1.399(5) . ?
C21 C22 1.390(5) . ?
C15 C16 1.394(5) . ?
C16 C17 1.340(7) . ?
C19 C18 1.416(6) . ?
C17 C18 1.374(8) . ?

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 O1 97.00(9) . . ?
O2 Al1 C2 107.53(12) . . ?
O1 Al1 C2 116.30(12) . . ?
O2 Al1 C1 117.52(13) . . ?
O1 Al1 C1 107.44(11) . . ?
C2 Al1 C1 110.74(15) . . ?
O2 Al1 K1 55.00(6) . . ?
O1 Al1 K1 42.39(6) . . ?
C2 Al1 K1 119.71(10) . . ?
C1 Al1 K1 128.84(11) . . ?
O1 K1 O2 57.62(5) . . ?
O1 K1 C55 114.07(7) . . ?
O2 K1 C55 66.97(6) . . ?
O1 K1 C50 127.55(8) . . ?
O2 K1 C50 92.11(6) . . ?
C55 K1 C50 26.41(7) . . ?
O1 K1 C54 121.87(7) . . ?
O2 K1 C54 64.85(7) . . ?
C55 K1 C54 26.21(8) . . ?
C50 K1 C54 44.99(8) . . ?
O1 K1 C25 77.98(7) . . ?
O2 K1 C25 117.25(7) . . ?
C55 K1 C25 165.42(9) . . ?
C50 K1 C25 149.83(8) . . ?
C54 K1 C25 140.57(9) . . ?
O1 K1 C20 64.64(6) . . ?
O2 K1 C20 92.49(6) . . ?
C55 K1 C20 151.60(8) . . ?
C50 K1 C20 167.18(9) . . ?
C54 K1 C20 127.79(8) . . ?
C25 K1 C20 25.19(7) . . ?
O1 K1 C21 78.67(7) . . ?
O2 K1 C21 83.00(7) . . ?
C55 K1 C21 127.86(8) . . ?
C50 K1 C21 144.46(9) . . ?
C54 K1 C21 102.81(8) . . ?
C25 K1 C21 43.77(8) . . ?
C20 K1 C21 25.17(7) . . ?
O1 K1 C24 103.27(8) . . ?
O2 K1 C24 133.36(8) . . ?
C55 K1 C24 141.64(9) . . ?
C50 K1 C24 126.53(9) . . ?
C54 K1 C24 122.37(9) . . ?
C25 K1 C24 25.30(8) . . ?
C20 K1 C24 44.35(8) . . ?
C21 K1 C24 50.49(9) . . ?
O1 K1 C22 103.61(8) . . ?
O2 K1 C22 96.69(8) . . ?
C55 K1 C22 116.04(9) . . ?
C50 K1 C22 123.19(9) . . ?
C54 K1 C22 89.98(9) . . ?
C25 K1 C22 50.82(9) . . ?
C20 K1 C22 44.30(8) . . ?
C21 K1 C22 24.95(8) . . ?
C24 K1 C22 42.70(10) . . ?
O1 K1 C23 116.19(8) . . ?
O2 K1 C23 120.77(9) . . ?
C55 K1 C23 121.50(9) . . ?
C50 K1 C23 116.12(9) . . ?
C54 K1 C23 98.91(9) . . ?
C25 K1 C23 43.94(9) . . ?
C20 K1 C23 51.56(8) . . ?
C21 K1 C23 43.41(9) . . ?
C24 K1 C23 24.34(9) . . ?
C22 K1 C23 24.12(9) . . ?
O1 K1 C51 151.20(8) . . ?
O2 K1 C51 111.02(7) . . ?
C55 K1 C51 44.67(7) . . ?
C50 K1 C51 24.44(8) . . ?
C54 K1 C51 50.50(8) . . ?
C25 K1 C51 126.82(8) . . ?
C20 K1 C51 143.98(8) . . ?
C21 K1 C51 128.61(9) . . ?
C24 K1 C51 102.40(9) . . ?
C22 K1 C51 104.05(9) . . ?
C23 K1 C51 92.49(9) . . ?
C39 O2 Al1 124.31(16) . . ?
C39 O2 K1 131.81(14) . . ?
Al1 O2 K1 95.28(7) . . ?
C3 O1 Al1 130.70(16) . . ?
C3 O1 K1 119.70(14) . . ?
Al1 O1 K1 109.53(8) . . ?
C41 C42 C43 116.5(2) . . ?
C41 C42 C45 122.4(2) . . ?
C43 C42 C45 121.0(2) . . ?
C40 C41 C42 122.7(2) . . ?
C44 C43 C42 122.8(2) . . ?
C41 C40 C39 119.6(2) . . ?
C41 C40 C49 120.5(2) . . ?
C39 C40 C49 119.8(2) . . ?
O2 C39 C40 120.5(2) . . ?
O2 C39 C44 120.7(2) . . ?
C40 C39 C44 118.8(2) . . ?
C54 C55 C50 117.6(3) . . ?
C54 C55 C49 123.1(2) . . ?
C50 C55 C49 119.1(2) . . ?
C54 C55 K1 82.63(17) . . ?
C50 C55 K1 82.07(16) . . ?
C49 C55 K1 101.55(15) . . ?
C46 C45 C48 111.2(3) . . ?
C46 C45 C42 110.4(3) . . ?
C48 C45 C42 112.7(2) . . ?
C46 C45 C47 108.2(3) . . ?
C48 C45 C47 106.4(3) . . ?
C42 C45 C47 107.7(3) . . ?
C43 C44 C39 119.5(2) . . ?
C43 C44 C62 120.3(2) . . ?
C39 C44 C62 119.9(2) . . ?
C56 C49 C40 112.5(2) . . ?
C56 C49 C55 111.8(2) . . ?
C40 C49 C55 112.1(2) . . ?
C52 C53 C54 120.3(3) . . ?
C52 C53 K1 82.3(2) . . ?
C54 C53 K1 68.36(18) . . ?
C58 C57 C56 120.2(3) . . ?
C55 C54 C53 120.8(3) . . ?
C55 C54 K1 71.16(16) . . ?
C53 C54 K1 87.0(2) . . ?
C51 C50 C55 121.4(3) . . ?
C51 C50 K1 87.24(19) . . ?
C55 C50 K1 71.52(16) . . ?
C61 C56 C57 118.3(3) . . ?
C61 C56 C49 120.7(3) . . ?
C57 C56 C49 121.0(3) . . ?
C51 C52 C53 119.3(3) . . ?
C51 C52 K1 73.9(2) . . ?
C53 C52 K1 74.28(19) . . ?
C52 C51 C50 120.5(3) . . ?
C52 C51 K1 82.8(2) . . ?
C50 C51 K1 68.32(18) . . ?
C56 C61 C60 120.7(3) . . ?
C59 C58 C57 120.3(3) . . ?
C59 C60 C61 120.3(4) . . ?
C58 C59 C60 120.2(3) . . ?
C6D C7D C2D 114.0(10) . . ?
C68 C63 C64 117.8(3) . . ?
C68 C63 C62 119.8(3) . . ?
C64 C63 C62 122.4(3) . . ?
C44 C62 C69 110.6(2) . . ?
C44 C62 C63 113.3(2) . . ?
C69 C62 C63 114.0(2) . . ?
C63 C64 C65 120.6(3) . . ?
C65 C66 C67 119.2(3) . . ?
C63 C68 C67 122.0(3) . . ?
C66 C65 C64 120.8(3) . . ?
C66 C67 C68 119.5(3) . . ?
C74 C69 C70 117.0(4) . . ?
C74 C69 C62 120.1(3) . . ?
C70 C69 C62 122.8(3) . . ?
C71 C70 C69 122.2(4) . . ?
C72 C71 C70 120.3(5) . . ?
C69 C74 C73 120.6(5) . . ?
C72 C73 C74 119.1(4) . . ?
C71 C72 C73 120.9(5) . . ?
C2D C3D C4D 120.2(8) . . ?
C3D C2D C7D 118.8(8) . . ?
C3D C2D C1D 120.3(9) . . ?
C7D C2D C1D 120.7(9) . . ?
C5D C4D C3D 120.0(9) . . ?
C6D C5D C4D 111.3(12) . . ?
C5D C6D C7D 132.9(14) . . ?
C5 C4 C3 118.9(2) . . ?
C5 C4 C13 122.0(2) . . ?
C3 C4 C13 119.0(2) . . ?
C4 C5 C6 123.0(2) . . ?
C27 C26 C8 110.8(2) . . ?
C27 C26 C33 112.4(2) . . ?
C8 C26 C33 113.8(2) . . ?
C6 C7 C8 122.4(2) . . ?
C7 C8 C3 119.6(2) . . ?
C7 C8 C26 122.4(2) . . ?
C3 C8 C26 117.6(2) . . ?
C12 C9 C10 109.7(3) . . ?
C12 C9 C11 107.2(3) . . ?
C10 C9 C11 109.8(3) . . ?
C12 C9 C6 112.6(2) . . ?
C10 C9 C6 107.8(2) . . ?
C11 C9 C6 109.8(2) . . ?
O1 C3 C8 120.7(2) . . ?
O1 C3 C4 120.0(2) . . ?
C8 C3 C4 119.2(2) . . ?
O1 C3 K1 40.34(11) . . ?
C8 C3 K1 114.38(16) . . ?
C4 C3 K1 108.34(16) . . ?
C25 C20 C21 117.9(3) . . ?
C25 C20 C13 122.9(3) . . ?
C21 C20 C13 119.1(3) . . ?
C25 C20 K1 77.37(16) . . ?
C21 C20 K1 78.52(18) . . ?
C13 C20 K1 113.39(15) . . ?
C34 C33 C38 117.9(3) . . ?
C34 C33 C26 123.3(2) . . ?
C38 C33 C26 118.8(2) . . ?
C7 C6 C5 116.9(2) . . ?
C7 C6 C9 123.5(2) . . ?
C5 C6 C9 119.6(2) . . ?
C14 C13 C4 112.5(2) . . ?
C14 C13 C20 111.6(2) . . ?
C4 C13 C20 111.9(2) . . ?
C37 C38 C33 120.9(3) . . ?
C28 C27 C32 116.6(3) . . ?
C28 C27 C26 123.7(2) . . ?
C32 C27 C26 119.7(3) . . ?
C15 C14 C19 119.0(3) . . ?
C15 C14 C13 122.7(3) . . ?
C19 C14 C13 118.2(3) . . ?
C36 C37 C38 120.3(3) . . ?
C35 C34 C33 121.2(3) . . ?
C34 C35 C36 119.9(3) . . ?
C27 C28 C29 122.3(3) . . ?
C27 C28 K1 83.78(18) . . ?
C29 C28 K1 89.5(2) . . ?
C31 C32 C27 121.4(3) . . ?
C29 C30 C31 119.1(3) . . ?
C22 C23 C24 119.4(3) . . ?
C22 C23 K1 77.3(2) . . ?
C24 C23 K1 76.3(2) . . ?
C20 C25 C24 120.2(3) . . ?
C20 C25 K1 77.44(16) . . ?
C24 C25 K1 79.19(18) . . ?
C37 C36 C35 119.7(3) . . ?
C32 C31 C30 120.9(3) . . ?
C23 C24 C25 120.9(3) . . ?
C23 C24 K1 79.4(2) . . ?
C25 C24 K1 75.51(17) . . ?
C30 C29 C28 119.7(3) . . ?
C20 C21 C22 120.9(3) . . ?
C20 C21 K1 76.31(17) . . ?
C22 C21 K1 79.1(2) . . ?
C14 C15 C16 120.8(4) . . ?
C17 C16 C15 119.8(5) . . ?
C14 C19 C18 119.9(5) . . ?
C23 C22 C21 120.7(3) . . ?
C23 C22 K1 78.6(2) . . ?
C21 C22 K1 75.9(2) . . ?
C16 C17 C18 121.7(5) . . ?
C17 C18 C19 118.7(5) . . ?

_refine_diff_density_max         0.838
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_2b_2tol
_database_code_depnum_ccdc_archive 'CCDC 1897465'
loop_
_audit_author_name
_audit_author_address
'Angel Gutierrez-Rodriguez'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2019-03-24 deposited with the CCDC.	2019-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_ABSMU01_2b_2tol             
;
PROBLEM: The ratio of given/expected absorption coefficient lies
RESPONSE: Due to the application of the squeeze procedure there is a  discrepancy in the expected contents and the given ones
;
_vrf_RINTA01_2b_2tol             
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Low quality of the crystal
;
_vrf_PLAT020_2b_2tol             
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.203 Report
RESPONSE: Low quality of the crystal
;
# Added during the CSD deposition process: Sunday 24 March 2019 09:35 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78  H84 O2 Na2 Al2.2C7 H8'
_chemical_formula_sum            'C78 H84 Al2 Na2 O2'
_chemical_formula_weight         1153.39

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   15.365(5)
_cell_length_b                   9.989(3)
_cell_length_c                   29.599(11)
_cell_angle_alpha                90
_cell_angle_beta                 103.43(3)
_cell_angle_gamma                90
_cell_volume                     4419(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    54
_cell_measurement_theta_min      3.20
_cell_measurement_theta_max      19.03

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.867
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.49

_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.32
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_T_max  0.975

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            71329
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_av_R_equivalents  0.2034
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.030
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9003
_reflns_number_gt                5441
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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


_computing_data_collection       '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    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0948P)²+3.3177P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9003
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0871
_refine_ls_wR_factor_ref         0.2334
_refine_ls_wR_factor_gt          0.2037
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# SQUEEZE RESULTS (Version =  40319)
# 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 0.250 0.003 0.250 708 192 ' '
2 0.750 -0.040 0.750 708 192 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
Two molecules of toluene 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 0.08345(6) 0.77754(9) 0.56802(3) 0.0384(3) Uani 1 1 d . . . . .
Na1 Na 0.10519(9) 0.44020(14) 0.55970(4) 0.0536(4) Uani 1 1 d . . . . .
O1 O 0.15430(13) 0.63804(19) 0.59311(6) 0.0358(5) Uani 1 1 d . . . . .
C1 C 0.0056(3) 0.8398(4) 0.60849(13) 0.0599(10) Uani 1 1 d . . . . .
H1A H -0.028428 0.763926 0.616411 0.090 Uiso 1 1 calc R U . . .
H1B H -0.035802 0.907918 0.592109 0.090 Uiso 1 1 calc R U . . .
H1C H 0.042648 0.878352 0.636987 0.090 Uiso 1 1 calc R U . . .
C2 C 0.1537(3) 0.9285(3) 0.55089(14) 0.0574(10) Uani 1 1 d . . . . .
H2A H 0.205903 0.945715 0.576349 0.086 Uiso 1 1 calc R U . . .
H2B H 0.116154 1.008850 0.545140 0.086 Uiso 1 1 calc R U . . .
H2C H 0.173629 0.905308 0.522741 0.086 Uiso 1 1 calc R U . . .
C3 C 0.0095(2) 0.6856(3) 0.51212(11) 0.0447(8) Uani 1 1 d . . . . .
H3A H 0.048841 0.645574 0.494099 0.067 Uiso 1 1 calc R U . . .
H3B H -0.030179 0.750887 0.492832 0.067 Uiso 1 1 calc R U . . .
H3C H -0.026549 0.615315 0.522023 0.067 Uiso 1 1 calc R U . . .
C4 C 0.2333(2) 0.6335(3) 0.62545(10) 0.0355(7) Uani 1 1 d . . . . .
C5 C 0.2340(2) 0.6097(3) 0.67207(10) 0.0338(7) Uani 1 1 d . . . . .
C6 C 0.3158(2) 0.6040(3) 0.70409(10) 0.0379(7) Uani 1 1 d . . . . .
H6 H 0.316433 0.589204 0.735872 0.057 Uiso 1 1 calc R U . . .
C7 C 0.3967(2) 0.6192(3) 0.69135(10) 0.0398(8) Uani 1 1 d . . . . .
C8 C 0.3936(2) 0.6363(3) 0.64455(10) 0.0409(8) Uani 1 1 d . . . . .
H8 H 0.448184 0.644162 0.634918 0.061 Uiso 1 1 calc R U . . .
C9 C 0.3134(2) 0.6423(3) 0.61124(10) 0.0366(7) Uani 1 1 d . . . . .
C10 C 0.4878(2) 0.6185(4) 0.72626(12) 0.0531(9) Uani 1 1 d . . . . .
C11 C 0.4773(3) 0.6052(6) 0.77538(14) 0.1000(19) Uani 1 1 d . . . . .
H11A H 0.440999 0.679533 0.782461 0.150 Uiso 1 1 calc R U . . .
H11B H 0.536321 0.607058 0.796869 0.150 Uiso 1 1 calc R U . . .
H11C H 0.447554 0.520168 0.778784 0.150 Uiso 1 1 calc R U . . .
C12 C 0.5353(3) 0.7489(5) 0.7215(2) 0.1034(18) Uani 1 1 d . . . . .
H12A H 0.499800 0.824007 0.728802 0.155 Uiso 1 1 calc R U . . .
H12B H 0.542521 0.758057 0.689649 0.155 Uiso 1 1 calc R U . . .
H12C H 0.594278 0.749103 0.743125 0.155 Uiso 1 1 calc R U . . .
C13 C 0.5433(3) 0.5010(5) 0.71590(16) 0.0848(14) Uani 1 1 d . . . . .
H13A H 0.603148 0.504658 0.736592 0.127 Uiso 1 1 calc R U . . .
H13B H 0.548332 0.505900 0.683540 0.127 Uiso 1 1 calc R U . . .
H13C H 0.514103 0.416887 0.720914 0.127 Uiso 1 1 calc R U . . .
C14 C 0.1010(2) 0.4577(3) 0.66044(10) 0.0391(7) Uani 1 1 d . . . . .
C15 C 0.0080(2) 0.4537(4) 0.64423(11) 0.0524(9) Uani 1 1 d . . . . .
H15 H -0.027127 0.527947 0.649401 0.079 Uiso 1 1 calc R U . . .
C16 C -0.0333(3) 0.3424(4) 0.62070(13) 0.0672(12) Uani 1 1 d . . . . .
H16 H -0.096505 0.341383 0.609472 0.101 Uiso 1 1 calc R U . . .
C17 C 0.0163(3) 0.2338(4) 0.61352(13) 0.0670(12) Uani 1 1 d . . . . .
H17 H -0.012506 0.158075 0.597171 0.100 Uiso 1 1 calc R U . . .
C18 C 0.1081(3) 0.2343(4) 0.63002(12) 0.0591(10) Uani 1 1 d . . . . .
H18 H 0.142788 0.158808 0.625496 0.089 Uiso 1 1 calc R U . . .
C19 C 0.1490(3) 0.3467(3) 0.65332(11) 0.0474(8) Uani 1 1 d . . . . .
H19 H 0.212179 0.346861 0.664674 0.071 Uiso 1 1 calc R U . . .
C21 C 0.2830(2) 0.5188(3) 0.53592(10) 0.0398(7) Uani 1 1 d . . . . .
C22 C 0.2981(2) 0.3972(3) 0.55845(12) 0.0488(9) Uani 1 1 d . . . . .
H22 H 0.329037 0.394729 0.590207 0.073 Uiso 1 1 calc R U . . .
C23 C 0.2688(3) 0.2782(4) 0.53551(14) 0.0596(10) Uani 1 1 d . . . . .
H23 H 0.278816 0.195663 0.551822 0.089 Uiso 1 1 calc R U . . .
C24 C 0.2255(3) 0.2796(4) 0.48940(15) 0.0617(11) Uani 1 1 d . . . . .
H24 H 0.205164 0.198493 0.473735 0.092 Uiso 1 1 calc R U . . .
C25 C 0.2121(3) 0.3987(4) 0.46631(13) 0.0601(10) Uani 1 1 d . . . . .
H25 H 0.183361 0.399708 0.434218 0.090 Uiso 1 1 calc R U . . .
C26 C 0.2397(2) 0.5184(4) 0.48891(11) 0.0493(9) Uani 1 1 d . . . . .
H26 H 0.229095 0.600469 0.472313 0.074 Uiso 1 1 calc R U . . .
C30 C 0.3107(2) 0.6519(3) 0.55972(10) 0.0390(7) Uani 1 1 d . . . . .
H30 H 0.262388 0.717355 0.546269 0.059 Uiso 1 1 calc R U . . .
C31 C 0.3977(2) 0.7084(3) 0.55054(10) 0.0423(8) Uani 1 1 d . . . . .
C32 C 0.4622(3) 0.6313(4) 0.53911(13) 0.0575(10) Uani 1 1 d . . . . .
H32 H 0.453096 0.537551 0.535260 0.086 Uiso 1 1 calc R U . . .
C33 C 0.5419(3) 0.6883(5) 0.53293(15) 0.0755(13) Uani 1 1 d . . . . .
H33 H 0.586502 0.633110 0.525077 0.113 Uiso 1 1 calc R U . . .
C34 C 0.5555(3) 0.8222(5) 0.53815(15) 0.0748(13) Uani 1 1 d . . . . .
H34 H 0.609265 0.861353 0.533775 0.112 Uiso 1 1 calc R U . . .
C35 C 0.4914(3) 0.8995(5) 0.54966(17) 0.0807(14) Uani 1 1 d . . . . .
H35 H 0.500625 0.993288 0.553377 0.121 Uiso 1 1 calc R U . . .
C36 C 0.4127(3) 0.8437(4) 0.55608(14) 0.0657(11) Uani 1 1 d . . . . .
H36 H 0.368697 0.899321 0.564370 0.099 Uiso 1 1 calc R U . . .
C50 C 0.1442(2) 0.5835(3) 0.68454(10) 0.0370(7) Uani 1 1 d . . . . .
H50 H 0.104021 0.659751 0.671474 0.056 Uiso 1 1 calc R U . . .
C51 C 0.1498(2) 0.5815(3) 0.73668(10) 0.0368(7) Uani 1 1 d . . . . .
C52 C 0.1755(3) 0.4699(3) 0.76341(11) 0.0506(9) Uani 1 1 d . . . . .
H52 H 0.191538 0.390833 0.749428 0.076 Uiso 1 1 calc R U . . .
C53 C 0.1785(3) 0.4709(4) 0.81081(12) 0.0607(11) Uani 1 1 d . . . . .
H53 H 0.196053 0.392860 0.828981 0.091 Uiso 1 1 calc R U . . .
C54 C 0.1561(3) 0.5850(4) 0.83107(12) 0.0580(10) Uani 1 1 d . . . . .
H54 H 0.157749 0.586048 0.863343 0.087 Uiso 1 1 calc R U . . .
C55 C 0.1316(3) 0.6969(4) 0.80511(12) 0.0621(11) Uani 1 1 d . . . . .
H55 H 0.116768 0.776408 0.819288 0.093 Uiso 1 1 calc R U . . .
C56 C 0.1282(2) 0.6949(4) 0.75772(11) 0.0498(9) Uani 1 1 d . . . . .
H56 H 0.110767 0.773268 0.739709 0.075 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 O1 1.817(2) . ?
Al1 C1 1.979(4) . ?
Al1 C2 1.987(4) . ?
Al1 C3 2.000(3) . ?
Al1 Na1 3.401(2) . ?
Na1 O1 2.260(2) . ?
Na1 C3 2.731(3) 3_566 ?
Na1 C19 2.853(4) . ?
Na1 C18 2.919(4) . ?
Na1 C14 3.003(3) . ?
Na1 C22 3.004(4) . ?
Na1 C21 3.078(3) . ?
Na1 C4 3.101(3) . ?
Na1 C17 3.109(4) . ?
O1 C4 1.361(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C9 1.393(4) . ?
C4 C5 1.398(4) . ?
C5 C6 1.389(4) . ?
C5 C50 1.531(4) . ?
C6 C7 1.388(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(4) . ?
C7 C10 1.536(5) . ?
C8 C9 1.389(4) . ?
C8 H8 0.9500 . ?
C9 C30 1.519(4) . ?
C10 C11 1.506(6) . ?
C10 C12 1.515(6) . ?
C10 C13 1.523(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C19 1.375(5) . ?
C14 C15 1.399(5) . ?
C14 C50 1.519(4) . ?
C15 C16 1.385(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.371(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C21 C22 1.379(5) . ?
C21 C26 1.396(4) . ?
C21 C30 1.518(4) . ?
C22 C23 1.391(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.372(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.363(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.388(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C30 C31 1.532(4) . ?
C30 H30 1.0000 . ?
C31 C32 1.359(5) . ?
C31 C36 1.374(5) . ?
C32 C33 1.400(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.357(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.355(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C50 C51 1.526(4) . ?
C50 H50 1.0000 . ?
C51 C56 1.370(4) . ?
C51 C52 1.371(4) . ?
C52 C53 1.393(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.369(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.359(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.392(5) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Al1 C1 112.48(14) . . ?
O1 Al1 C2 112.12(14) . . ?
C1 Al1 C2 110.87(17) . . ?
O1 Al1 C3 99.06(12) . . ?
C1 Al1 C3 109.75(17) . . ?
C2 Al1 C3 112.04(16) . . ?
O1 Al1 Na1 37.84(7) . . ?
C1 Al1 Na1 116.01(13) . . ?
C2 Al1 Na1 131.68(12) . . ?
C3 Al1 Na1 62.07(10) . . ?
O1 Na1 C3 146.34(10) . 3_566 ?
O1 Na1 C19 83.21(9) . . ?
C3 Na1 C19 124.71(11) 3_566 . ?
O1 Na1 C18 110.85(10) . . ?
C3 Na1 C18 97.53(12) 3_566 . ?
C19 Na1 C18 27.82(10) . . ?
O1 Na1 C14 66.21(8) . . ?
C3 Na1 C14 129.86(11) 3_566 . ?
C19 Na1 C14 27.01(9) . . ?
C18 Na1 C14 48.18(10) . . ?
O1 Na1 C22 84.26(9) . . ?
C3 Na1 C22 112.62(11) 3_566 . ?
C19 Na1 C22 87.36(11) . . ?
C18 Na1 C22 93.22(12) . . ?
C14 Na1 C22 105.62(10) . . ?
O1 Na1 C21 69.69(9) . . ?
C3 Na1 C21 112.69(11) 3_566 . ?
C19 Na1 C21 106.48(11) . . ?
C18 Na1 C21 118.38(12) . . ?
C14 Na1 C21 115.93(10) . . ?
C22 Na1 C21 26.18(9) . . ?
O1 Na1 C4 23.33(8) . . ?
C3 Na1 C4 167.35(10) 3_566 . ?
C19 Na1 C4 67.79(10) . . ?
C18 Na1 C4 95.10(10) . . ?
C14 Na1 C4 59.83(9) . . ?
C22 Na1 C4 67.17(9) . . ?
C21 Na1 C4 61.08(9) . . ?
O1 Na1 C17 119.84(10) . . ?
C3 Na1 C17 79.22(11) 3_566 . ?
C19 Na1 C17 46.99(11) . . ?
C18 Na1 C17 26.27(11) . . ?
C14 Na1 C17 54.29(10) . . ?
C22 Na1 C17 117.64(13) . . ?
C21 Na1 C17 143.66(12) . . ?
C4 Na1 C17 112.46(10) . . ?
O1 Na1 Al1 29.56(6) . . ?
C3 Na1 Al1 117.12(8) 3_566 . ?
C19 Na1 Al1 105.02(8) . . ?
C18 Na1 Al1 129.20(9) . . ?
C14 Na1 Al1 81.10(7) . . ?
C22 Na1 Al1 104.85(8) . . ?
C21 Na1 Al1 82.59(7) . . ?
C4 Na1 Al1 52.86(6) . . ?
C17 Na1 Al1 123.90(10) . . ?
C4 O1 Al1 131.66(18) . . ?
C4 O1 Na1 115.56(17) . . ?
Al1 O1 Na1 112.59(10) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Al1 C2 H2A 109.5 . . ?
Al1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Al1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Al1 C3 H3A 109.5 . . ?
Al1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Al1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1 C4 C9 119.5(3) . . ?
O1 C4 C5 120.0(3) . . ?
C9 C4 C5 120.3(3) . . ?
O1 C4 Na1 41.10(12) . . ?
C9 C4 Na1 109.07(19) . . ?
C5 C4 Na1 111.8(2) . . ?
C6 C5 C4 118.6(3) . . ?
C6 C5 C50 123.5(3) . . ?
C4 C5 C50 117.9(3) . . ?
C7 C6 C5 122.4(3) . . ?
C7 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C8 C7 C6 117.4(3) . . ?
C8 C7 C10 119.2(3) . . ?
C6 C7 C10 123.4(3) . . ?
C7 C8 C9 122.3(3) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C4 118.9(3) . . ?
C8 C9 C30 121.9(3) . . ?
C4 C9 C30 119.1(3) . . ?
C11 C10 C12 109.1(4) . . ?
C11 C10 C13 108.5(4) . . ?
C12 C10 C13 109.9(4) . . ?
C11 C10 C7 111.3(3) . . ?
C12 C10 C7 108.5(3) . . ?
C13 C10 C7 109.5(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 117.8(3) . . ?
C19 C14 C50 123.2(3) . . ?
C15 C14 C50 119.0(3) . . ?
C19 C14 Na1 70.41(18) . . ?
C15 C14 Na1 85.04(19) . . ?
C50 C14 Na1 114.00(18) . . ?
C16 C15 C14 120.5(4) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 120.4(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 120.1(4) . . ?
C16 C17 Na1 83.2(2) . . ?
C18 C17 Na1 69.2(2) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
Na1 C17 H17 118.4 . . ?
C17 C18 C19 119.0(4) . . ?
C17 C18 Na1 84.5(2) . . ?
C19 C18 Na1 73.4(2) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
Na1 C18 H18 112.0 . . ?
C14 C19 C18 122.0(4) . . ?
C14 C19 Na1 82.58(19) . . ?
C18 C19 Na1 78.8(2) . . ?
C14 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
Na1 C19 H19 109.5 . . ?
C22 C21 C26 117.9(3) . . ?
C22 C21 C30 123.3(3) . . ?
C26 C21 C30 118.8(3) . . ?
C22 C21 Na1 73.9(2) . . ?
C26 C21 Na1 89.1(2) . . ?
C30 C21 Na1 106.58(18) . . ?
C21 C22 C23 121.2(3) . . ?
C21 C22 Na1 79.9(2) . . ?
C23 C22 Na1 85.4(2) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 H22 119.4 . . ?
Na1 C22 H22 105.1 . . ?
C24 C23 C22 120.3(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 119.3(3) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 121.1(4) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C21 120.3(3) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C21 C30 C9 110.5(3) . . ?
C21 C30 C31 113.7(3) . . ?
C9 C30 C31 112.3(2) . . ?
C21 C30 H30 106.6 . . ?
C9 C30 H30 106.6 . . ?
C31 C30 H30 106.6 . . ?
C32 C31 C36 118.4(3) . . ?
C32 C31 C30 123.5(3) . . ?
C36 C31 C30 118.1(3) . . ?
C31 C32 C33 120.8(4) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 120.1(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C35 C34 C33 119.2(4) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C34 C35 C36 120.9(4) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C31 C36 C35 120.5(4) . . ?
C31 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C14 C50 C51 112.3(2) . . ?
C14 C50 C5 110.3(2) . . ?
C51 C50 C5 113.8(2) . . ?
C14 C50 H50 106.6 . . ?
C51 C50 H50 106.6 . . ?
C5 C50 H50 106.6 . . ?
C56 C51 C52 118.5(3) . . ?
C56 C51 C50 119.1(3) . . ?
C52 C51 C50 122.3(3) . . ?
C51 C52 C53 120.8(3) . . ?
C51 C52 H52 119.6 . . ?
C53 C52 H52 119.6 . . ?
C54 C53 C52 119.6(3) . . ?
C54 C53 H53 120.2 . . ?
C52 C53 H53 120.2 . . ?
C55 C54 C53 120.2(3) . . ?
C55 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
C54 C55 C56 119.9(4) . . ?
C54 C55 H55 120.1 . . ?
C56 C55 H55 120.1 . . ?
C51 C56 C55 120.9(3) . . ?
C51 C56 H56 119.5 . . ?
C55 C56 H56 119.5 . . ?

_refine_diff_density_max         0.382
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.055



