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

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

data_0425
_database_code_depnum_ccdc_archive 'CCDC 1446110'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H37 Al N2 O7'
_chemical_formula_weight         612.63

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5013(5)
_cell_length_b                   11.9173(5)
_cell_length_c                   13.3035(6)
_cell_angle_alpha                102.745(2)
_cell_angle_beta                 106.178(2)
_cell_angle_gamma                112.038(2)
_cell_volume                     1511.12(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9909
_cell_measurement_theta_min      2.780
_cell_measurement_theta_max      29.329

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_F_000             648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.120
_shelx_estimated_absorpt_T_min   0.968
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6321
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;    
 SADABS-2014/4 - Bruker AXS area detector scaling and absorption correction 
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59195
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.712
_diffrn_reflns_theta_max         30.619
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9242
_reflns_number_gt                5781
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9242
_refine_ls_number_parameters     417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1942
_refine_ls_wR_factor_gt          0.1634
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.164
_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
Al01 Al 0.84787(5) 0.35445(6) 0.31564(5) 0.01703(15) Uani 1 1 d . . . . .
O002 O 0.82888(14) 0.47737(15) 0.42277(13) 0.0202(3) Uani 1 1 d . . . . .
H36 H 0.829(4) 0.466(4) 0.476(4) 0.090(15) Uiso 1 1 d . . . . .
O003 O 0.92067(13) 0.29419(14) 0.42029(12) 0.0224(3) Uani 1 1 d . . . . .
O004 O 1.02465(13) 0.47754(14) 0.35118(12) 0.0211(3) Uani 1 1 d . . . . .
O8 O 1.28989(13) 0.59688(15) 0.42975(12) 0.0250(3) Uani 1 1 d . . . . .
O006 O 0.86679(16) 0.22532(15) 0.20463(13) 0.0261(4) Uani 1 1 d . . . . .
H35 H 0.938(4) 0.227(4) 0.234(3) 0.083(13) Uiso 1 1 d . . . . .
O007 O 1.09141(14) 0.26643(15) 0.57371(13) 0.0268(3) Uani 1 1 d . . . . .
N008 N 0.77700(15) 0.40999(16) 0.19364(14) 0.0185(3) Uani 1 1 d . . . . .
N009 N 0.66088(15) 0.22357(16) 0.28340(14) 0.0178(3) Uani 1 1 d . . . . .
O00A O 1.07433(18) 0.1988(2) 0.33101(16) 0.0492(5) Uani 1 1 d . . . . .
H34 H 1.0490 0.2291 0.3791 0.074 Uiso 1 1 calc R U . . .
C00B C 1.07876(18) 0.54274(19) 0.29339(16) 0.0180(4) Uani 1 1 d . . . . .
C00C C 0.62594(18) 0.13635(19) 0.33399(17) 0.0193(4) Uani 1 1 d . . . . .
C00D C 0.64020(19) 0.3713(2) 0.12864(17) 0.0199(4) Uani 1 1 d . . . . .
C00E C 1.00157(19) 0.55277(19) 0.19601(17) 0.0199(4) Uani 1 1 d . . . . .
C00F C 0.85238(19) 0.4919(2) 0.15341(17) 0.0200(4) Uani 1 1 d . . . . .
C00G C 0.86507(19) 0.20291(19) 0.45947(17) 0.0186(4) Uani 1 1 d . . . . .
C00H C 0.72332(19) 0.12330(19) 0.42126(17) 0.0205(4) Uani 1 1 d . . . . .
C00I C 0.10578(19) 0.1380(2) -0.06571(18) 0.0220(4) Uani 1 1 d . . . . .
C00J C 1.22378(19) 0.6101(2) 0.33313(17) 0.0201(4) Uani 1 1 d . . . . .
C00K C 0.38644(18) 0.2397(2) 0.05948(17) 0.0209(4) Uani 1 1 d . . . . .
C00L C 0.53885(18) 0.20534(19) 0.20639(17) 0.0189(4) Uani 1 1 d . . . . .
C00M C 0.17073(19) 0.2373(2) 0.03928(18) 0.0225(4) Uani 1 1 d . . . . .
H24 H 0.1185 0.2696 0.0689 0.027 Uiso 1 1 calc R U . . .
C00N C 0.52942(18) 0.2760(2) 0.13574(17) 0.0198(4) Uani 1 1 d . . . . .
C00O C 0.32561(19) 0.1467(2) -0.04927(18) 0.0226(4) Uani 1 1 d . . . . .
C00P C 0.42697(19) 0.1036(2) 0.21041(18) 0.0235(4) Uani 1 1 d . . . . .
H32 H 0.3327 0.0721 0.1667 0.028 Uiso 1 1 calc R U . . .
C00Q C 0.48029(19) 0.0599(2) 0.28873(18) 0.0230(4) Uani 1 1 d . . . . .
H33 H 0.4303 -0.0084 0.3094 0.028 Uiso 1 1 calc R U . . .
C00R C 0.95504(19) 0.1846(2) 0.54386(18) 0.0232(4) Uani 1 1 d . . . . .
C00S C 0.7656(2) 0.5090(2) 0.06444(19) 0.0260(5) Uani 1 1 d . . . . .
H1 H 0.7936 0.5616 0.0229 0.031 Uiso 1 1 calc R U . . .
C00T C 0.31111(19) 0.2906(2) 0.10213(18) 0.0218(4) Uani 1 1 d . . . . .
C00U C 0.1856(2) 0.0990(2) -0.11104(18) 0.0240(4) Uani 1 1 d . . . . .
H25 H 0.1441 0.0383 -0.1860 0.029 Uiso 1 1 calc R U . . .
C00V C 1.2885(2) 0.6795(2) 0.27692(19) 0.0248(5) Uani 1 1 d . . . . .
H2 H 1.3855 0.7235 0.3051 0.030 Uiso 1 1 calc R U . . .
C00W C 0.6338(2) 0.4344(2) 0.05075(18) 0.0250(5) Uani 1 1 d . . . . .
H3 H 0.5532 0.4267 -0.0016 0.030 Uiso 1 1 calc R U . . .
C19 C 1.43515(19) 0.6652(2) 0.47898(19) 0.0291(5) Uani 1 1 d . . . . .
H6 H 1.4710 0.6316 0.4275 0.044 Uiso 1 1 calc R U . . .
H7 H 1.4690 0.6530 0.5499 0.044 Uiso 1 1 calc R U . . .
H8 H 1.4657 0.7580 0.4936 0.044 Uiso 1 1 calc R U . . .
C00Y C -0.0476(2) 0.0737(2) -0.1289(2) 0.0312(5) Uani 1 1 d . . . . .
H12 H -0.0743 0.0083 -0.2017 0.047 Uiso 1 1 calc R U . . .
H13 H -0.0756 0.1395 -0.1411 0.047 Uiso 1 1 calc R U . . .
H14 H -0.0923 0.0317 -0.0850 0.047 Uiso 1 1 calc R U . . .
C00Z C 1.0699(2) 0.6228(2) 0.13930(19) 0.0263(5) Uani 1 1 d . . . . .
H4 H 1.0177 0.6275 0.0725 0.032 Uiso 1 1 calc R U . . .
C010 C 0.6768(2) 0.0318(2) 0.4711(2) 0.0310(5) Uani 1 1 d . . . . .
H26 H 0.5812 -0.0205 0.4473 0.037 Uiso 1 1 calc R U . . .
C011 C 1.2099(2) 0.6841(2) 0.17869(19) 0.0278(5) Uani 1 1 d . . . . .
H5 H 1.2534 0.7300 0.1388 0.033 Uiso 1 1 calc R U . . .
C012 C 0.4060(2) 0.0956(2) -0.1001(2) 0.0332(6) Uani 1 1 d . . . . .
H15 H 0.3451 0.0300 -0.1756 0.050 Uiso 1 1 calc R U . . .
H16 H 0.4461 0.0562 -0.0527 0.050 Uiso 1 1 calc R U . . .
H17 H 0.4793 0.1674 -0.1051 0.050 Uiso 1 1 calc R U . . .
C013 C 0.9075(2) 0.0928(2) 0.5895(2) 0.0337(6) Uani 1 1 d . . . . .
H27 H 0.9697 0.0812 0.6451 0.040 Uiso 1 1 calc R U . . .
C014 C 1.1899(2) 0.2586(3) 0.6612(2) 0.0343(6) Uani 1 1 d . . . . .
H28 H 1.1693 0.2704 0.7283 0.051 Uiso 1 1 calc R U . . .
H29 H 1.2815 0.3268 0.6791 0.051 Uiso 1 1 calc R U . . .
H30 H 1.1864 0.1732 0.6362 0.051 Uiso 1 1 calc R U . . .
C015 C 0.3809(2) 0.4056(2) 0.2119(2) 0.0348(6) Uani 1 1 d . . . . .
H18 H 0.4475 0.4809 0.2050 0.052 Uiso 1 1 calc R U . . .
H19 H 0.4280 0.3839 0.2723 0.052 Uiso 1 1 calc R U . . .
H20 H 0.3122 0.4263 0.2293 0.052 Uiso 1 1 calc R U . . .
C016 C 0.8264(3) 0.1947(3) 0.0851(2) 0.0346(6) Uani 1 1 d . . . . .
H21 H 0.7309 0.1766 0.0506 0.052 Uiso 1 1 calc R U . . .
H22 H 0.8356 0.1180 0.0521 0.052 Uiso 1 1 calc R U . . .
H23 H 0.8852 0.2686 0.0714 0.052 Uiso 1 1 calc R U . . .
C017 C 0.7659(2) 0.0168(3) 0.5526(2) 0.0401(6) Uani 1 1 d . . . . .
H31 H 0.7317 -0.0456 0.5846 0.048 Uiso 1 1 calc R U . . .
C018 C 1.2149(3) 0.2665(3) 0.3692(3) 0.0535(8) Uani 1 1 d . . . . .
H9 H 1.2434 0.3596 0.3885 0.080 Uiso 1 1 calc R U . . .
H10 H 1.2437 0.2367 0.3103 0.080 Uiso 1 1 calc R U . . .
H11 H 1.2575 0.2511 0.4361 0.080 Uiso 1 1 calc R U . . .
H37 H 0.888(3) 0.550(3) 0.433(2) 0.048(9) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al01 O003 1.8433(16) . ?
Al01 O004 1.8519(14) . ?
Al01 O002 1.9279(16) . ?
Al01 N008 1.9693(18) . ?
Al01 N009 1.9787(16) . ?
Al01 O006 2.0061(16) . ?
O002 H36 0.75(4) . ?
O002 H37 0.83(3) . ?
O003 C00G 1.333(2) . ?
O004 C00B 1.323(2) . ?
O8 C00J 1.375(3) . ?
O8 C19 1.420(2) . ?
O006 C016 1.443(3) . ?
O006 H35 0.79(4) . ?
O007 C00R 1.380(2) . ?
O007 C014 1.428(3) . ?
N008 C00F 1.359(2) . ?
N008 C00D 1.399(2) . ?
N009 C00C 1.357(3) . ?
N009 C00L 1.392(2) . ?
O00A C018 1.380(3) . ?
O00A H34 0.8400 . ?
C00B C00E 1.410(3) . ?
C00B C00J 1.422(2) . ?
C00C C00Q 1.432(2) . ?
C00C C00H 1.453(3) . ?
C00D C00N 1.396(3) . ?
C00D C00W 1.410(3) . ?
C00E C00Z 1.414(3) . ?
C00E C00F 1.461(3) . ?
C00F C00S 1.428(3) . ?
C00G C00H 1.408(3) . ?
C00G C00R 1.418(3) . ?
C00H C010 1.412(3) . ?
C00I C00U 1.389(3) . ?
C00I C00M 1.391(3) . ?
C00I C00Y 1.510(3) . ?
C00J C00V 1.385(3) . ?
C00K C00O 1.399(3) . ?
C00K C00T 1.399(3) . ?
C00K C00N 1.504(3) . ?
C00L C00N 1.402(3) . ?
C00L C00P 1.423(3) . ?
C00M C00T 1.398(3) . ?
C00M H24 0.9500 . ?
C00O C00U 1.400(3) . ?
C00O C012 1.508(3) . ?
C00P C00Q 1.363(3) . ?
C00P H32 0.9500 . ?
C00Q H33 0.9500 . ?
C00R C013 1.375(3) . ?
C00S C00W 1.373(3) . ?
C00S H1 0.9500 . ?
C00T C015 1.514(3) . ?
C00U H25 0.9500 . ?
C00V C011 1.393(3) . ?
C00V H2 0.9500 . ?
C00W H3 0.9500 . ?
C19 H6 0.9800 . ?
C19 H7 0.9800 . ?
C19 H8 0.9800 . ?
C00Y H12 0.9800 . ?
C00Y H13 0.9800 . ?
C00Y H14 0.9800 . ?
C00Z C011 1.370(3) . ?
C00Z H4 0.9500 . ?
C010 C017 1.364(3) . ?
C010 H26 0.9500 . ?
C011 H5 0.9500 . ?
C012 H15 0.9800 . ?
C012 H16 0.9800 . ?
C012 H17 0.9800 . ?
C013 C017 1.403(3) . ?
C013 H27 0.9500 . ?
C014 H28 0.9800 . ?
C014 H29 0.9800 . ?
C014 H30 0.9800 . ?
C015 H18 0.9800 . ?
C015 H19 0.9800 . ?
C015 H20 0.9800 . ?
C016 H21 0.9800 . ?
C016 H22 0.9800 . ?
C016 H23 0.9800 . ?
C017 H31 0.9500 . ?
C018 H9 0.9800 . ?
C018 H10 0.9800 . ?
C018 H11 0.9800 . ?

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
O003 Al01 O004 87.99(6) . . ?
O003 Al01 O002 93.90(7) . . ?
O004 Al01 O002 90.19(7) . . ?
O003 Al01 N008 174.05(7) . . ?
O004 Al01 N008 90.42(7) . . ?
O002 Al01 N008 91.84(7) . . ?
O003 Al01 N009 90.34(7) . . ?
O004 Al01 N009 177.95(7) . . ?
O002 Al01 N009 88.73(7) . . ?
N008 Al01 N009 91.35(7) . . ?
O003 Al01 O006 85.77(7) . . ?
O004 Al01 O006 90.19(7) . . ?
O002 Al01 O006 179.50(8) . . ?
N008 Al01 O006 88.49(7) . . ?
N009 Al01 O006 90.89(7) . . ?
Al01 O002 H36 117(3) . . ?
Al01 O002 H37 106(2) . . ?
H36 O002 H37 114(4) . . ?
C00G O003 Al01 133.25(12) . . ?
C00B O004 Al01 131.64(13) . . ?
C00J O8 C19 117.63(16) . . ?
C016 O006 Al01 128.88(15) . . ?
C016 O006 H35 113(3) . . ?
Al01 O006 H35 108(3) . . ?
C00R O007 C014 117.58(17) . . ?
C00F N008 C00D 105.86(17) . . ?
C00F N008 Al01 126.47(13) . . ?
C00D N008 Al01 127.66(13) . . ?
C00C N009 C00L 106.42(15) . . ?
C00C N009 Al01 126.89(13) . . ?
C00L N009 Al01 126.67(14) . . ?
C018 O00A H34 109.5 . . ?
O004 C00B C00E 124.05(16) . . ?
O004 C00B C00J 118.34(18) . . ?
C00E C00B C00J 117.59(17) . . ?
N009 C00C C00Q 110.14(18) . . ?
N009 C00C C00H 124.45(16) . . ?
C00Q C00C C00H 125.41(18) . . ?
C00N C00D N008 123.69(19) . . ?
C00N C00D C00W 126.51(19) . . ?
N008 C00D C00W 109.59(17) . . ?
C00B C00E C00Z 119.38(17) . . ?
C00B C00E C00F 120.79(17) . . ?
C00Z C00E C00F 119.83(19) . . ?
N008 C00F C00S 110.60(17) . . ?
N008 C00F C00E 124.01(18) . . ?
C00S C00F C00E 125.39(18) . . ?
O003 C00G C00H 124.01(18) . . ?
O003 C00G C00R 117.59(16) . . ?
C00H C00G C00R 118.39(18) . . ?
C00G C00H C010 118.68(19) . . ?
C00G C00H C00C 121.00(18) . . ?
C010 C00H C00C 120.31(18) . . ?
C00U C00I C00M 118.28(18) . . ?
C00U C00I C00Y 120.67(19) . . ?
C00M C00I C00Y 121.05(19) . . ?
O8 C00J C00V 124.79(17) . . ?
O8 C00J C00B 113.26(17) . . ?
C00V C00J C00B 121.94(19) . . ?
C00O C00K C00T 120.53(18) . . ?
C00O C00K C00N 120.05(18) . . ?
C00T C00K C00N 119.15(18) . . ?
N009 C00L C00N 124.79(17) . . ?
N009 C00L C00P 109.27(18) . . ?
C00N C00L C00P 125.94(18) . . ?
C00I C00M C00T 121.45(19) . . ?
C00I C00M H24 119.3 . . ?
C00T C00M H24 119.3 . . ?
C00D C00N C00L 125.40(18) . . ?
C00D C00N C00K 119.10(19) . . ?
C00L C00N C00K 115.46(17) . . ?
C00K C00O C00U 118.51(19) . . ?
C00K C00O C012 121.82(18) . . ?
C00U C00O C012 119.67(19) . . ?
C00Q C00P C00L 107.25(17) . . ?
C00Q C00P H32 126.4 . . ?
C00L C00P H32 126.4 . . ?
C00P C00Q C00C 106.91(17) . . ?
C00P C00Q H33 126.5 . . ?
C00C C00Q H33 126.5 . . ?
C013 C00R O007 124.65(19) . . ?
C013 C00R C00G 121.91(18) . . ?
O007 C00R C00G 113.44(18) . . ?
C00W C00S C00F 106.47(19) . . ?
C00W C00S H1 126.8 . . ?
C00F C00S H1 126.8 . . ?
C00M C00T C00K 118.89(19) . . ?
C00M C00T C015 120.20(19) . . ?
C00K C00T C015 120.85(18) . . ?
C00I C00U C00O 121.8(2) . . ?
C00I C00U H25 119.1 . . ?
C00O C00U H25 119.1 . . ?
C00J C00V C011 119.34(18) . . ?
C00J C00V H2 120.3 . . ?
C011 C00V H2 120.3 . . ?
C00S C00W C00D 107.44(18) . . ?
C00S C00W H3 126.3 . . ?
C00D C00W H3 126.3 . . ?
O8 C19 H6 109.5 . . ?
O8 C19 H7 109.5 . . ?
H6 C19 H7 109.5 . . ?
O8 C19 H8 109.5 . . ?
H6 C19 H8 109.5 . . ?
H7 C19 H8 109.5 . . ?
C00I C00Y H12 109.5 . . ?
C00I C00Y H13 109.5 . . ?
H12 C00Y H13 109.5 . . ?
C00I C00Y H14 109.5 . . ?
H12 C00Y H14 109.5 . . ?
H13 C00Y H14 109.5 . . ?
C011 C00Z C00E 121.4(2) . . ?
C011 C00Z H4 119.3 . . ?
C00E C00Z H4 119.3 . . ?
C017 C010 C00H 121.6(2) . . ?
C017 C010 H26 119.2 . . ?
C00H C010 H26 119.2 . . ?
C00Z C011 C00V 120.31(19) . . ?
C00Z C011 H5 119.8 . . ?
C00V C011 H5 119.8 . . ?
C00O C012 H15 109.5 . . ?
C00O C012 H16 109.5 . . ?
H15 C012 H16 109.5 . . ?
C00O C012 H17 109.5 . . ?
H15 C012 H17 109.5 . . ?
H16 C012 H17 109.5 . . ?
C00R C013 C017 118.9(2) . . ?
C00R C013 H27 120.5 . . ?
C017 C013 H27 120.5 . . ?
O007 C014 H28 109.5 . . ?
O007 C014 H29 109.5 . . ?
H28 C014 H29 109.5 . . ?
O007 C014 H30 109.5 . . ?
H28 C014 H30 109.5 . . ?
H29 C014 H30 109.5 . . ?
C00T C015 H18 109.5 . . ?
C00T C015 H19 109.5 . . ?
H18 C015 H19 109.5 . . ?
C00T C015 H20 109.5 . . ?
H18 C015 H20 109.5 . . ?
H19 C015 H20 109.5 . . ?
O006 C016 H21 109.5 . . ?
O006 C016 H22 109.5 . . ?
H21 C016 H22 109.5 . . ?
O006 C016 H23 109.5 . . ?
H21 C016 H23 109.5 . . ?
H22 C016 H23 109.5 . . ?
C010 C017 C013 120.4(2) . . ?
C010 C017 H31 119.8 . . ?
C013 C017 H31 119.8 . . ?
O00A C018 H9 109.5 . . ?
O00A C018 H10 109.5 . . ?
H9 C018 H10 109.5 . . ?
O00A C018 H11 109.5 . . ?
H9 C018 H11 109.5 . . ?
H10 C018 H11 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O004 Al01 O003 C00G 176.04(19) . . . . ?
O002 Al01 O003 C00G 85.99(19) . . . . ?
N009 Al01 O003 C00G -2.76(19) . . . . ?
O006 Al01 O003 C00G -93.62(19) . . . . ?
O003 Al01 O004 C00B 155.97(18) . . . . ?
O002 Al01 O004 C00B -110.14(18) . . . . ?
N008 Al01 O004 C00B -18.29(19) . . . . ?
O006 Al01 O004 C00B 70.20(18) . . . . ?
Al01 O004 C00B C00E 15.4(3) . . . . ?
Al01 O004 C00B C00J -166.41(14) . . . . ?
C00L N009 C00C C00Q 0.6(2) . . . . ?
Al01 N009 C00C C00Q 179.01(13) . . . . ?
C00L N009 C00C C00H -179.45(19) . . . . ?
Al01 N009 C00C C00H -1.1(3) . . . . ?
C00F N008 C00D C00N 173.08(19) . . . . ?
Al01 N008 C00D C00N -5.3(3) . . . . ?
C00F N008 C00D C00W -2.0(2) . . . . ?
Al01 N008 C00D C00W 179.69(15) . . . . ?
O004 C00B C00E C00Z -178.7(2) . . . . ?
C00J C00B C00E C00Z 3.1(3) . . . . ?
O004 C00B C00E C00F 1.4(3) . . . . ?
C00J C00B C00E C00F -176.81(18) . . . . ?
C00D N008 C00F C00S 1.3(2) . . . . ?
Al01 N008 C00F C00S 179.70(14) . . . . ?
C00D N008 C00F C00E -178.39(19) . . . . ?
Al01 N008 C00F C00E 0.0(3) . . . . ?
C00B C00E C00F N008 -8.4(3) . . . . ?
C00Z C00E C00F N008 171.7(2) . . . . ?
C00B C00E C00F C00S 171.9(2) . . . . ?
C00Z C00E C00F C00S -8.0(3) . . . . ?
Al01 O003 C00G C00H 2.2(3) . . . . ?
Al01 O003 C00G C00R -178.55(15) . . . . ?
O003 C00G C00H C010 -178.7(2) . . . . ?
C00R C00G C00H C010 2.1(3) . . . . ?
O003 C00G C00H C00C 0.0(3) . . . . ?
C00R C00G C00H C00C -179.28(19) . . . . ?
N009 C00C C00H C00G -0.4(3) . . . . ?
C00Q C00C C00H C00G 179.51(19) . . . . ?
N009 C00C C00H C010 178.3(2) . . . . ?
C00Q C00C C00H C010 -1.8(3) . . . . ?
C19 O8 C00J C00V 3.6(3) . . . . ?
C19 O8 C00J C00B -177.34(18) . . . . ?
O004 C00B C00J O8 0.3(3) . . . . ?
C00E C00B C00J O8 178.58(18) . . . . ?
O004 C00B C00J C00V 179.32(19) . . . . ?
C00E C00B C00J C00V -2.4(3) . . . . ?
C00C N009 C00L C00N -179.64(19) . . . . ?
Al01 N009 C00L C00N 2.0(3) . . . . ?
C00C N009 C00L C00P -0.2(2) . . . . ?
Al01 N009 C00L C00P -178.59(14) . . . . ?
C00U C00I C00M C00T -4.7(3) . . . . ?
C00Y C00I C00M C00T 175.1(2) . . . . ?
N008 C00D C00N C00L -1.0(3) . . . . ?
C00W C00D C00N C00L 173.2(2) . . . . ?
N008 C00D C00N C00K -178.43(18) . . . . ?
C00W C00D C00N C00K -4.2(3) . . . . ?
N009 C00L C00N C00D 2.7(3) . . . . ?
C00P C00L C00N C00D -176.7(2) . . . . ?
N009 C00L C00N C00K -179.81(18) . . . . ?
C00P C00L C00N C00K 0.9(3) . . . . ?
C00O C00K C00N C00D 85.1(3) . . . . ?
C00T C00K C00N C00D -100.8(2) . . . . ?
C00O C00K C00N C00L -92.6(2) . . . . ?
C00T C00K C00N C00L 81.5(3) . . . . ?
C00T C00K C00O C00U -4.6(3) . . . . ?
C00N C00K C00O C00U 169.3(2) . . . . ?
C00T C00K C00O C012 176.4(2) . . . . ?
C00N C00K C00O C012 -9.6(3) . . . . ?
N009 C00L C00P C00Q -0.3(2) . . . . ?
C00N C00L C00P C00Q 179.1(2) . . . . ?
C00L C00P C00Q C00C 0.7(2) . . . . ?
N009 C00C C00Q C00P -0.8(2) . . . . ?
C00H C00C C00Q C00P 179.26(19) . . . . ?
C014 O007 C00R C013 -2.5(3) . . . . ?
C014 O007 C00R C00G 177.74(19) . . . . ?
O003 C00G C00R C013 -180.0(2) . . . . ?
C00H C00G C00R C013 -0.7(3) . . . . ?
O003 C00G C00R O007 -0.2(3) . . . . ?
C00H C00G C00R O007 179.13(18) . . . . ?
N008 C00F C00S C00W -0.2(3) . . . . ?
C00E C00F C00S C00W 179.5(2) . . . . ?
C00I C00M C00T C00K -2.0(3) . . . . ?
C00I C00M C00T C015 175.2(2) . . . . ?
C00O C00K C00T C00M 6.8(3) . . . . ?
C00N C00K C00T C00M -167.22(19) . . . . ?
C00O C00K C00T C015 -170.4(2) . . . . ?
C00N C00K C00T C015 15.6(3) . . . . ?
C00M C00I C00U C00O 7.0(3) . . . . ?
C00Y C00I C00U C00O -172.8(2) . . . . ?
C00K C00O C00U C00I -2.4(3) . . . . ?
C012 C00O C00U C00I 176.6(2) . . . . ?
O8 C00J C00V C011 179.1(2) . . . . ?
C00B C00J C00V C011 0.2(3) . . . . ?
C00F C00S C00W C00D -1.0(2) . . . . ?
C00N C00D C00W C00S -173.0(2) . . . . ?
N008 C00D C00W C00S 1.9(2) . . . . ?
C00B C00E C00Z C011 -1.7(3) . . . . ?
C00F C00E C00Z C011 178.2(2) . . . . ?
C00G C00H C010 C017 -1.8(4) . . . . ?
C00C C00H C010 C017 179.5(2) . . . . ?
C00E C00Z C011 C00V -0.5(4) . . . . ?
C00J C00V C011 C00Z 1.3(3) . . . . ?
O007 C00R C013 C017 179.2(2) . . . . ?
C00G C00R C013 C017 -1.1(4) . . . . ?
C00H C010 C017 C013 0.1(4) . . . . ?
C00R C013 C017 C010 1.4(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C018 H9 O8 0.98 2.57 3.544(4) 173.7 .
C018 H9 O8 0.98 2.57 3.544(4) 173.7 .
C018 H9 O8 0.98 2.57 3.544(4) 173.7 .
C018 H9 O8 0.98 2.57 3.544(4) 173.7 .
C018 H9 O8 0.98 2.57 3.544(4) 173.7 .
C018 H9 O8 0.98 2.57 3.544(4) 173.7 .
C018 H9 O8 0.98 2.57 3.544(4) 173.7 .
O00A H34 O003 0.84 2.05 2.812(2) 150.6 .
O00A H34 O007 0.84 2.40 3.081(2) 138.5 .
C018 H9 O8 0.98 2.57 3.544(4) 173.7 .
O00A H34 O003 0.84 2.05 2.812(2) 150.6 .
O00A H34 O007 0.84 2.40 3.081(2) 138.5 .
O002 H36 O004 0.75(4) 2.21(4) 2.820(2) 139(4) 2_766
O002 H36 O8 0.75(4) 2.15(4) 2.802(2) 147(4) 2_766
O006 H35 O00A 0.79(4) 1.93(4) 2.681(2) 160(4) .
O00A H34 O003 0.84 2.05 2.812(2) 150.6 .
O00A H34 O007 0.84 2.40 3.081(2) 138.5 .
C018 H9 O8 0.98 2.57 3.544(4) 173.7 .
O002 H37 O003 0.83(3) 2.25(3) 2.885(2) 134(3) 2_766
O002 H37 O007 0.83(3) 2.13(3) 2.824(2) 141(3) 2_766
O002 H36 O004 0.75(4) 2.21(4) 2.820(2) 139(4) 2_766
O002 H36 O8 0.75(4) 2.15(4) 2.802(2) 147(4) 2_766
O006 H35 O00A 0.79(4) 1.93(4) 2.681(2) 160(4) .
O002 H37 O003 0.83(3) 2.25(3) 2.885(2) 134(3) 2_766
O002 H37 O007 0.83(3) 2.13(3) 2.824(2) 141(3) 2_766

_refine_diff_density_max         0.929
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.070



####################################################################### 
# 
# 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_171aa
_database_code_depnum_ccdc_archive 'CCDC 1446111'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H27 B N2 O4'
_chemical_formula_weight         514.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   17.1558(6)
_cell_length_b                   11.8814(4)
_cell_length_c                   24.8691(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5069.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    8947
_cell_measurement_theta_min      2.375
_cell_measurement_theta_max      29.937

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_F_000             2160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.088
_shelx_estimated_absorpt_T_min   0.983
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;    
 SADABS-2014/4 - Bruker AXS area detector scaling and absorption correction 
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42692
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.638
_diffrn_reflns_theta_max         30.518
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7727
_reflns_number_gt                5373
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1000P)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         7727
_refine_ls_number_parameters     357
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1700
_refine_ls_wR_factor_gt          0.1454
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.010
_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
O1 O -0.12560(7) 0.75144(9) 0.14410(4) 0.0234(3) Uani 1 1 d . . . . .
O2 O 0.01790(6) 0.86259(8) 0.13417(4) 0.0164(2) Uani 1 1 d . . . . .
O3 O 0.01766(6) 1.06268(8) 0.13368(4) 0.0158(2) Uani 1 1 d . . . . .
O4 O -0.11325(7) 1.17789(9) 0.14123(4) 0.0226(3) Uani 1 1 d . . . . .
N1 N 0.11321(8) 0.95175(9) 0.07808(5) 0.0141(3) Uani 1 1 d . . . . .
N2 N 0.12889(7) 0.97308(10) 0.17385(5) 0.0149(3) Uani 1 1 d . . . . .
C1 C -0.12906(12) 0.83677(16) 0.18500(7) 0.0327(4) Uani 1 1 d . . . . .
H28 H -0.0793 0.8394 0.2043 0.049 Uiso 1 1 calc R U . . .
H3 H -0.1711 0.8191 0.2103 0.049 Uiso 1 1 calc R U . . .
H1 H -0.1391 0.9100 0.1683 0.049 Uiso 1 1 calc R U . . .
C2 C -0.09576(9) 0.78280(12) 0.09483(6) 0.0190(3) Uani 1 1 d . . . . .
C3 C -0.02467(9) 0.83909(11) 0.08920(6) 0.0159(3) Uani 1 1 d . . . . .
C4 C 0.00294(9) 0.86423(11) 0.03670(6) 0.0163(3) Uani 1 1 d . . . . .
C5 C 0.08030(9) 0.91265(11) 0.03248(5) 0.0151(3) Uani 1 1 d . . . . .
C6 C 0.19339(9) 0.96013(11) 0.07106(6) 0.0158(3) Uani 1 1 d . . . . .
C7 C 0.24289(9) 0.96543(11) 0.11583(6) 0.0158(3) Uani 1 1 d . . . . .
C8 C 0.32894(9) 0.96472(11) 0.10850(6) 0.0167(3) Uani 1 1 d . . . . .
C9 C 0.36545(10) 1.05303(12) 0.08022(6) 0.0191(3) Uani 1 1 d . . . . .
C10 C 0.44538(10) 1.04814(12) 0.07071(6) 0.0205(3) Uani 1 1 d . . . . .
H18 H 0.4698 1.1075 0.0515 0.025 Uiso 1 1 calc R U . . .
C11 C 0.49033(10) 0.95807(13) 0.08878(6) 0.0211(3) Uani 1 1 d . . . . .
C12 C 0.57644(11) 0.95343(15) 0.07703(8) 0.0314(4) Uani 1 1 d . . . . .
H2 H 0.5889 1.0063 0.0481 0.047 Uiso 1 1 calc R U . . .
H19 H 0.5907 0.8770 0.0660 0.047 Uiso 1 1 calc R U . . .
H20 H 0.6057 0.9739 0.1094 0.047 Uiso 1 1 calc R U . . .
C13 C -0.00822(9) 1.08852(11) 0.18396(6) 0.0161(3) Uani 1 1 d . . . . .
C14 C -0.07718(9) 1.15128(12) 0.18884(6) 0.0183(3) Uani 1 1 d . . . . .
C15 C -0.18567(11) 1.23606(16) 0.14511(8) 0.0314(4) Uani 1 1 d . . . . .
H5 H -0.2237 1.1885 0.1637 0.047 Uiso 1 1 calc R U . . .
H4 H -0.2048 1.2537 0.1089 0.047 Uiso 1 1 calc R U . . .
H6 H -0.1783 1.3060 0.1653 0.047 Uiso 1 1 calc R U . . .
C16 C -0.10404(10) 1.18230(14) 0.23948(6) 0.0236(3) Uani 1 1 d . . . . .
H7 H -0.1508 1.2245 0.2427 0.028 Uiso 1 1 calc R U . . .
C17 C -0.06292(11) 1.15207(14) 0.28562(6) 0.0257(4) Uani 1 1 d . . . . .
H8 H -0.0821 1.1733 0.3200 0.031 Uiso 1 1 calc R U . . .
C18 C 0.00521(10) 1.09168(14) 0.28165(6) 0.0235(3) Uani 1 1 d . . . . .
H9 H 0.0330 1.0714 0.3132 0.028 Uiso 1 1 calc R U . . .
C19 C 0.03391(10) 1.05981(12) 0.23081(6) 0.0175(3) Uani 1 1 d . . . . .
C20 C 0.11127(9) 1.01386(12) 0.22318(6) 0.0171(3) Uani 1 1 d . . . . .
C21 C 0.20945(9) 0.97074(11) 0.16771(6) 0.0164(3) Uani 1 1 d . . . . .
C22 C -0.03926(9) 0.82881(12) -0.00850(6) 0.0190(3) Uani 1 1 d . . . . .
H12 H -0.0199 0.8437 -0.0436 0.023 Uiso 1 1 calc R U . . .
C23 C -0.10892(10) 0.77230(13) -0.00194(6) 0.0231(3) Uani 1 1 d . . . . .
H10 H -0.1375 0.7480 -0.0325 0.028 Uiso 1 1 calc R U . . .
C24 C -0.13718(10) 0.75099(13) 0.04952(6) 0.0227(3) Uani 1 1 d . . . . .
H11 H -0.1859 0.7139 0.0536 0.027 Uiso 1 1 calc R U . . .
C25 C 0.13820(10) 0.90923(12) -0.00843(6) 0.0185(3) Uani 1 1 d . . . . .
H14 H 0.1304 0.8911 -0.0452 0.022 Uiso 1 1 calc R U . . .
C26 C 0.20784(9) 0.93728(11) 0.01576(6) 0.0181(3) Uani 1 1 d . . . . .
H13 H 0.2571 0.9408 -0.0016 0.022 Uiso 1 1 calc R U . . .
C27 C 0.37406(10) 0.87418(12) 0.12796(6) 0.0177(3) Uani 1 1 d . . . . .
C28 C 0.45375(10) 0.87312(12) 0.11779(6) 0.0212(3) Uani 1 1 d . . . . .
H21 H 0.4842 0.8124 0.1311 0.025 Uiso 1 1 calc R U . . .
C29 C 0.32189(11) 1.15691(13) 0.06158(7) 0.0263(4) Uani 1 1 d . . . . .
H15 H 0.3521 1.2243 0.0707 0.039 Uiso 1 1 calc R U . . .
H16 H 0.2710 1.1602 0.0794 0.039 Uiso 1 1 calc R U . . .
H17 H 0.3144 1.1534 0.0225 0.039 Uiso 1 1 calc R U . . .
C30 C 0.33939(11) 0.77428(13) 0.15726(7) 0.0240(3) Uani 1 1 d . . . . .
H22 H 0.3559 0.7045 0.1396 0.036 Uiso 1 1 calc R U . . .
H23 H 0.2824 0.7794 0.1565 0.036 Uiso 1 1 calc R U . . .
H24 H 0.3574 0.7742 0.1947 0.036 Uiso 1 1 calc R U . . .
C31 C 0.24211(10) 1.00007(12) 0.21805(6) 0.0200(3) Uani 1 1 d . . . . .
H25 H 0.2961 1.0017 0.2266 0.024 Uiso 1 1 calc R U . . .
C32 C 0.18151(10) 1.02595(12) 0.25262(6) 0.0204(3) Uani 1 1 d . . . . .
H26 H 0.1861 1.0477 0.2892 0.024 Uiso 1 1 calc R U . . .
B1 B 0.06784(11) 0.96225(13) 0.13014(6) 0.0150(3) 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
O1 C2 1.3793(18) . ?
O1 C1 1.4373(19) . ?
O2 C3 1.3646(17) . ?
O2 B1 1.4651(18) . ?
O3 C13 1.3619(17) . ?
O3 B1 1.4740(19) . ?
O4 C14 1.3728(18) . ?
O4 C15 1.425(2) . ?
N1 C5 1.3492(18) . ?
N1 C6 1.390(2) . ?
N1 B1 1.516(2) . ?
N2 C20 1.3531(18) . ?
N2 C21 1.391(2) . ?
N2 B1 1.515(2) . ?
C1 H28 0.9800 . ?
C1 H3 0.9800 . ?
C1 H1 0.9800 . ?
C2 C24 1.385(2) . ?
C2 C3 1.398(2) . ?
C3 C4 1.420(2) . ?
C4 C22 1.402(2) . ?
C4 C5 1.450(2) . ?
C5 C25 1.422(2) . ?
C6 C7 1.402(2) . ?
C6 C26 1.424(2) . ?
C7 C21 1.413(2) . ?
C7 C8 1.487(2) . ?
C8 C9 1.410(2) . ?
C8 C27 1.411(2) . ?
C9 C10 1.393(2) . ?
C9 C29 1.515(2) . ?
C10 C11 1.394(2) . ?
C10 H18 0.9500 . ?
C11 C28 1.390(2) . ?
C11 C12 1.507(2) . ?
C12 H2 0.9800 . ?
C12 H19 0.9800 . ?
C12 H20 0.9800 . ?
C13 C14 1.404(2) . ?
C13 C19 1.413(2) . ?
C14 C16 1.391(2) . ?
C15 H5 0.9800 . ?
C15 H4 0.9800 . ?
C15 H6 0.9800 . ?
C16 C17 1.394(2) . ?
C16 H7 0.9500 . ?
C17 C18 1.375(3) . ?
C17 H8 0.9500 . ?
C18 C19 1.409(2) . ?
C18 H9 0.9500 . ?
C19 C20 1.448(2) . ?
C20 C32 1.417(2) . ?
C21 C31 1.415(2) . ?
C22 C23 1.381(2) . ?
C22 H12 0.9500 . ?
C23 C24 1.392(2) . ?
C23 H10 0.9500 . ?
C24 H11 0.9500 . ?
C25 C26 1.378(2) . ?
C25 H14 0.9500 . ?
C26 H13 0.9500 . ?
C27 C28 1.390(2) . ?
C27 C30 1.515(2) . ?
C28 H21 0.9500 . ?
C29 H15 0.9800 . ?
C29 H16 0.9800 . ?
C29 H17 0.9800 . ?
C30 H22 0.9800 . ?
C30 H23 0.9800 . ?
C30 H24 0.9800 . ?
C31 C32 1.384(2) . ?
C31 H25 0.9500 . ?
C32 H26 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
C2 O1 C1 116.97(12) . . ?
C3 O2 B1 114.99(11) . . ?
C13 O3 B1 115.33(11) . . ?
C14 O4 C15 116.52(13) . . ?
C5 N1 C6 109.47(12) . . ?
C5 N1 B1 122.09(13) . . ?
C6 N1 B1 127.55(12) . . ?
C20 N2 C21 109.19(12) . . ?
C20 N2 B1 121.77(13) . . ?
C21 N2 B1 127.34(12) . . ?
O1 C1 H28 109.5 . . ?
O1 C1 H3 109.5 . . ?
H28 C1 H3 109.5 . . ?
O1 C1 H1 109.5 . . ?
H28 C1 H1 109.5 . . ?
H3 C1 H1 109.5 . . ?
O1 C2 C24 117.30(14) . . ?
O1 C2 C3 122.83(13) . . ?
C24 C2 C3 119.79(14) . . ?
O2 C3 C2 118.86(13) . . ?
O2 C3 C4 122.12(14) . . ?
C2 C3 C4 118.93(13) . . ?
C22 C4 C3 120.11(14) . . ?
C22 C4 C5 122.25(13) . . ?
C3 C4 C5 117.08(13) . . ?
N1 C5 C25 108.59(14) . . ?
N1 C5 C4 117.30(13) . . ?
C25 C5 C4 132.80(13) . . ?
N1 C6 C7 120.20(13) . . ?
N1 C6 C26 106.25(13) . . ?
C7 C6 C26 132.10(15) . . ?
C6 C7 C21 118.76(14) . . ?
C6 C7 C8 120.25(13) . . ?
C21 C7 C8 120.99(13) . . ?
C9 C8 C27 119.65(14) . . ?
C9 C8 C7 119.85(13) . . ?
C27 C8 C7 120.46(13) . . ?
C10 C9 C8 119.41(14) . . ?
C10 C9 C29 117.87(13) . . ?
C8 C9 C29 122.66(15) . . ?
C9 C10 C11 121.48(14) . . ?
C9 C10 H18 119.3 . . ?
C11 C10 H18 119.3 . . ?
C28 C11 C10 118.36(15) . . ?
C28 C11 C12 121.10(15) . . ?
C10 C11 C12 120.54(15) . . ?
C11 C12 H2 109.5 . . ?
C11 C12 H19 109.5 . . ?
H2 C12 H19 109.5 . . ?
C11 C12 H20 109.5 . . ?
H2 C12 H20 109.5 . . ?
H19 C12 H20 109.5 . . ?
O3 C13 C14 118.28(13) . . ?
O3 C13 C19 122.41(14) . . ?
C14 C13 C19 119.22(13) . . ?
O4 C14 C16 124.79(15) . . ?
O4 C14 C13 115.33(13) . . ?
C16 C14 C13 119.88(14) . . ?
O4 C15 H5 109.5 . . ?
O4 C15 H4 109.5 . . ?
H5 C15 H4 109.5 . . ?
O4 C15 H6 109.5 . . ?
H5 C15 H6 109.5 . . ?
H4 C15 H6 109.5 . . ?
C14 C16 C17 120.63(16) . . ?
C14 C16 H7 119.7 . . ?
C17 C16 H7 119.7 . . ?
C18 C17 C16 120.36(14) . . ?
C18 C17 H8 119.8 . . ?
C16 C17 H8 119.8 . . ?
C17 C18 C19 120.13(15) . . ?
C17 C18 H9 119.9 . . ?
C19 C18 H9 119.9 . . ?
C18 C19 C13 119.76(15) . . ?
C18 C19 C20 122.65(14) . . ?
C13 C19 C20 116.87(13) . . ?
N2 C20 C32 108.34(14) . . ?
N2 C20 C19 117.30(13) . . ?
C32 C20 C19 132.34(14) . . ?
N2 C21 C7 120.30(13) . . ?
N2 C21 C31 106.94(13) . . ?
C7 C21 C31 131.13(15) . . ?
C23 C22 C4 119.88(14) . . ?
C23 C22 H12 120.1 . . ?
C4 C22 H12 120.1 . . ?
C22 C23 C24 119.92(14) . . ?
C22 C23 H10 120.0 . . ?
C24 C23 H10 120.0 . . ?
C2 C24 C23 121.32(15) . . ?
C2 C24 H11 119.3 . . ?
C23 C24 H11 119.3 . . ?
C26 C25 C5 106.63(13) . . ?
C26 C25 H14 126.7 . . ?
C5 C25 H14 126.7 . . ?
C25 C26 C6 108.46(14) . . ?
C25 C26 H13 125.8 . . ?
C6 C26 H13 125.8 . . ?
C28 C27 C8 118.96(14) . . ?
C28 C27 C30 117.81(13) . . ?
C8 C27 C30 123.16(15) . . ?
C11 C28 C27 122.11(14) . . ?
C11 C28 H21 118.9 . . ?
C27 C28 H21 118.9 . . ?
C9 C29 H15 109.5 . . ?
C9 C29 H16 109.5 . . ?
H15 C29 H16 109.5 . . ?
C9 C29 H17 109.5 . . ?
H15 C29 H17 109.5 . . ?
H16 C29 H17 109.5 . . ?
C27 C30 H22 109.5 . . ?
C27 C30 H23 109.5 . . ?
H22 C30 H23 109.5 . . ?
C27 C30 H24 109.5 . . ?
H22 C30 H24 109.5 . . ?
H23 C30 H24 109.5 . . ?
C32 C31 C21 107.87(14) . . ?
C32 C31 H25 126.1 . . ?
C21 C31 H25 126.1 . . ?
C31 C32 C20 107.18(14) . . ?
C31 C32 H26 126.4 . . ?
C20 C32 H26 126.4 . . ?
O2 B1 O3 107.98(13) . . ?
O2 B1 N2 115.08(12) . . ?
O3 B1 N2 106.98(11) . . ?
O2 B1 N1 106.99(11) . . ?
O3 B1 N1 114.68(11) . . ?
N2 B1 N1 105.36(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 O1 C2 C24 -132.91(16) . . . . ?
C1 O1 C2 C3 50.5(2) . . . . ?
B1 O2 C3 C2 -151.84(13) . . . . ?
B1 O2 C3 C4 31.81(19) . . . . ?
O1 C2 C3 O2 1.1(2) . . . . ?
C24 C2 C3 O2 -175.39(13) . . . . ?
O1 C2 C3 C4 177.59(13) . . . . ?
C24 C2 C3 C4 1.1(2) . . . . ?
O2 C3 C4 C22 173.80(13) . . . . ?
C2 C3 C4 C22 -2.6(2) . . . . ?
O2 C3 C4 C5 2.2(2) . . . . ?
C2 C3 C4 C5 -174.11(13) . . . . ?
C6 N1 C5 C25 -8.03(15) . . . . ?
B1 N1 C5 C25 -177.97(12) . . . . ?
C6 N1 C5 C4 160.58(12) . . . . ?
B1 N1 C5 C4 -9.36(19) . . . . ?
C22 C4 C5 N1 175.07(13) . . . . ?
C3 C4 C5 N1 -13.57(19) . . . . ?
C22 C4 C5 C25 -19.7(2) . . . . ?
C3 C4 C5 C25 151.64(15) . . . . ?
C5 N1 C6 C7 -160.67(12) . . . . ?
B1 N1 C6 C7 8.6(2) . . . . ?
C5 N1 C6 C26 7.21(15) . . . . ?
B1 N1 C6 C26 176.45(12) . . . . ?
N1 C6 C7 C21 -4.75(19) . . . . ?
C26 C6 C7 C21 -168.99(14) . . . . ?
N1 C6 C7 C8 174.86(12) . . . . ?
C26 C6 C7 C8 10.6(2) . . . . ?
C6 C7 C8 C9 62.64(18) . . . . ?
C21 C7 C8 C9 -117.76(15) . . . . ?
C6 C7 C8 C27 -115.03(15) . . . . ?
C21 C7 C8 C27 64.57(18) . . . . ?
C27 C8 C9 C10 1.6(2) . . . . ?
C7 C8 C9 C10 -176.08(13) . . . . ?
C27 C8 C9 C29 -175.55(14) . . . . ?
C7 C8 C9 C29 6.8(2) . . . . ?
C8 C9 C10 C11 -0.3(2) . . . . ?
C29 C9 C10 C11 176.97(15) . . . . ?
C9 C10 C11 C28 -1.3(2) . . . . ?
C9 C10 C11 C12 178.73(15) . . . . ?
B1 O3 C13 C14 -155.57(13) . . . . ?
B1 O3 C13 C19 27.94(19) . . . . ?
C15 O4 C14 C16 -3.7(2) . . . . ?
C15 O4 C14 C13 176.57(13) . . . . ?
O3 C13 C14 O4 1.8(2) . . . . ?
C19 C13 C14 O4 178.38(12) . . . . ?
O3 C13 C14 C16 -177.95(13) . . . . ?
C19 C13 C14 C16 -1.4(2) . . . . ?
O4 C14 C16 C17 -179.44(14) . . . . ?
C13 C14 C16 C17 0.3(2) . . . . ?
C14 C16 C17 C18 0.5(2) . . . . ?
C16 C17 C18 C19 -0.1(2) . . . . ?
C17 C18 C19 C13 -1.0(2) . . . . ?
C17 C18 C19 C20 168.96(14) . . . . ?
O3 C13 C19 C18 178.19(13) . . . . ?
C14 C13 C19 C18 1.7(2) . . . . ?
O3 C13 C19 C20 7.6(2) . . . . ?
C14 C13 C19 C20 -168.83(13) . . . . ?
C21 N2 C20 C32 -7.09(16) . . . . ?
B1 N2 C20 C32 -173.23(12) . . . . ?
C21 N2 C20 C19 158.77(12) . . . . ?
B1 N2 C20 C19 -7.36(19) . . . . ?
C18 C19 C20 N2 171.81(13) . . . . ?
C13 C19 C20 N2 -17.93(19) . . . . ?
C18 C19 C20 C32 -26.5(2) . . . . ?
C13 C19 C20 C32 143.80(16) . . . . ?
C20 N2 C21 C7 -160.43(12) . . . . ?
B1 N2 C21 C7 4.7(2) . . . . ?
C20 N2 C21 C31 6.57(15) . . . . ?
B1 N2 C21 C31 171.73(13) . . . . ?
C6 C7 C21 N2 -1.38(19) . . . . ?
C8 C7 C21 N2 179.01(12) . . . . ?
C6 C7 C21 C31 -164.78(14) . . . . ?
C8 C7 C21 C31 15.6(2) . . . . ?
C3 C4 C22 C23 1.9(2) . . . . ?
C5 C4 C22 C23 173.01(13) . . . . ?
C4 C22 C23 C24 0.2(2) . . . . ?
O1 C2 C24 C23 -175.66(14) . . . . ?
C3 C2 C24 C23 1.0(2) . . . . ?
C22 C23 C24 C2 -1.7(2) . . . . ?
N1 C5 C25 C26 5.59(15) . . . . ?
C4 C5 C25 C26 -160.56(15) . . . . ?
C5 C25 C26 C6 -1.09(15) . . . . ?
N1 C6 C26 C25 -3.61(15) . . . . ?
C7 C6 C26 C25 162.24(14) . . . . ?
C9 C8 C27 C28 -1.2(2) . . . . ?
C7 C8 C27 C28 176.43(13) . . . . ?
C9 C8 C27 C30 -178.13(14) . . . . ?
C7 C8 C27 C30 -0.5(2) . . . . ?
C10 C11 C28 C27 1.7(2) . . . . ?
C12 C11 C28 C27 -178.35(15) . . . . ?
C8 C27 C28 C11 -0.4(2) . . . . ?
C30 C27 C28 C11 176.64(14) . . . . ?
N2 C21 C31 C32 -3.47(16) . . . . ?
C7 C21 C31 C32 161.59(15) . . . . ?
C21 C31 C32 C20 -0.74(16) . . . . ?
N2 C20 C32 C31 4.83(16) . . . . ?
C19 C20 C32 C31 -158.11(15) . . . . ?
C3 O2 B1 O3 74.64(14) . . . . ?
C3 O2 B1 N2 -165.95(12) . . . . ?
C3 O2 B1 N1 -49.29(16) . . . . ?
C13 O3 B1 O2 76.33(15) . . . . ?
C13 O3 B1 N2 -48.08(16) . . . . ?
C13 O3 B1 N1 -164.52(12) . . . . ?
C20 N2 B1 O2 -80.56(17) . . . . ?
C21 N2 B1 O2 115.98(15) . . . . ?
C20 N2 B1 O3 39.39(17) . . . . ?
C21 N2 B1 O3 -124.07(14) . . . . ?
C20 N2 B1 N1 161.86(12) . . . . ?
C21 N2 B1 N1 -1.61(18) . . . . ?
C5 N1 B1 O2 39.98(17) . . . . ?
C6 N1 B1 O2 -128.03(13) . . . . ?
C5 N1 B1 O3 -79.72(16) . . . . ?
C6 N1 B1 O3 112.27(15) . . . . ?
C5 N1 B1 N2 162.91(11) . . . . ?
C6 N1 B1 N2 -5.10(17) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C25 H14 O4 0.95 2.54 3.4875(18) 174.1 5_575
C25 H14 O4 0.95 2.54 3.4875(18) 174.1 5_575
C25 H14 O4 0.95 2.54 3.4875(18) 174.1 5_575
C25 H14 O4 0.95 2.54 3.4875(18) 174.1 5_575
C25 H14 O4 0.95 2.54 3.4875(18) 174.1 5_575

_refine_diff_density_max         0.377
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.059



####################################################################### 
# 
# 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_l8al_0ma
_database_code_depnum_ccdc_archive 'CCDC 1446112'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H59 Al2 N4 Na O11'
_chemical_formula_weight         1137.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   24.6207(14)
_cell_length_b                   7.271(3)
_cell_length_c                   35.445(6)
_cell_angle_alpha                90
_cell_angle_beta                 111.987(3)
_cell_angle_gamma                90
_cell_volume                     5884(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_F_000             2384
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.121
_shelx_estimated_absorpt_T_min   0.976
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15115
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.750
_diffrn_reflns_theta_max         27.604
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             6541
_reflns_number_gt                3452
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.2000P)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         6541
_refine_ls_number_parameters     381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1919
_refine_ls_R_factor_gt           0.1208
_refine_ls_wR_factor_ref         0.3923
_refine_ls_wR_factor_gt          0.3497
_refine_ls_goodness_of_fit_ref   1.314
_refine_ls_restrained_S_all      1.314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
# start Validation Reply Form
_vrf_EXPT005_l8al_0ma            
;
PROBLEM: _exptl_crystal_description is missing
RESPONSE: It cannot be reported due to the failure to take experimetal notes.
;
_vrf_DIFMX01_l8al_0ma            
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*2.00
RESPONSE: Disordered solvent molecules were not able to be fully located.
;
_vrf_PLAT097_l8al_0ma            
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       3.62 eA-3
RESPONSE: Disordered solvent molecules were not able to be fully located.
;
_vrf_PLAT183_l8al_0ma            
;
PROBLEM: Missing _cell_measurement_reflns_used value ....     Please Do !
RESPONSE: The data could not be found due to the loss of the original files
on the determination of the cell.
;
_vrf_PLAT184_l8al_0ma            
;
PROBLEM: Missing _cell_measurement_theta_min value ......     Please Do !
RESPONSE: The data could not be found due to the loss of the original files
on the determination of the cell.
;
_vrf_PLAT185_l8al_0ma            
;
PROBLEM: Missing _cell_measurement_theta_max value ......     Please Do !
RESPONSE: The data could not be found due to the loss of the original files
on the determination of the cell.
;
# end Validation Reply Form
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 0.05772(7) 0.2942(3) 0.17112(4) 0.0396(6) Uani 1 1 d . . . . .
C1 C 0.0504(2) 0.3022(8) 0.08428(13) 0.0315(13) Uani 1 1 d . . . . .
C2 C -0.0730(2) 0.4404(8) 0.10907(14) 0.0351(13) Uani 1 1 d . . . . .
C3 C 0.1555(2) 0.0622(8) -0.00566(14) 0.0335(13) Uani 1 1 d . . . . .
C4 C -0.0285(2) 0.4105(8) 0.09211(14) 0.0316(12) Uani 1 1 d . . . . .
C5 C 0.1008(2) 0.0033(9) 0.03776(15) 0.0392(14) Uani 1 1 d . . . . .
C6 C 0.1759(2) 0.2200(9) 0.01539(14) 0.0382(14) Uani 1 1 d . . . . .
H1 H 0.2021 0.2940 0.0080 0.046 Uiso 1 1 calc R U . . .
C7 C 0.1915(3) 0.1242(11) 0.32301(15) 0.0496(17) Uani 1 1 d . . . . .
H2 H 0.1958 0.1274 0.3508 0.059 Uiso 1 1 calc R U . . .
C8 C 0.1735(2) 0.1095(9) 0.19874(14) 0.0366(14) Uani 1 1 d . . . . .
C9 C 0.1036(2) 0.2125(8) 0.09328(14) 0.0307(12) Uani 1 1 d . . . . .
C10 C -0.0340(2) 0.4504(8) 0.05108(14) 0.0363(14) Uani 1 1 d . . . . .
H3 H -0.0654 0.5135 0.0310 0.044 Uiso 1 1 calc R U . . .
C11 C 0.0146(2) 0.3795(9) 0.04674(14) 0.0349(13) Uani 1 1 d . . . . .
H4 H 0.0229 0.3819 0.0226 0.042 Uiso 1 1 calc R U . . .
C12 C 0.2139(3) 0.0280(10) 0.18381(15) 0.0465(17) Uani 1 1 d . . . . .
H5 H 0.2490 -0.0349 0.1993 0.056 Uiso 1 1 calc R U . . .
C13 C 0.1453(2) 0.2067(9) 0.29390(13) 0.0352(14) Uani 1 1 d . . . . .
C14 C 0.1597(2) 0.2797(8) 0.04789(13) 0.0328(13) Uani 1 1 d . . . . .
C15 C 0.1219(2) 0.1641(8) 0.05852(13) 0.0312(13) Uani 1 1 d . . . . .
C16 C 0.1177(3) -0.0486(9) 0.00557(15) 0.0405(15) Uani 1 1 d . . . . .
H6 H 0.1033 -0.1600 -0.0087 0.049 Uiso 1 1 calc R U . . .
C17 C -0.1117(2) 0.3753(10) 0.16066(14) 0.0430(16) Uani 1 1 d . . . . .
C18 C 0.1790(2) 0.1139(9) 0.24114(14) 0.0392(15) Uani 1 1 d . . . . .
C19 C 0.1396(2) 0.1544(9) 0.13221(14) 0.0364(14) Uani 1 1 d . . . . .
C20 C 0.1923(2) 0.0581(9) 0.14260(15) 0.0433(16) Uani 1 1 d . . . . .
H7 H 0.2101 0.0200 0.1243 0.052 Uiso 1 1 calc R U . . .
C21 C 0.1828(3) 0.4553(10) 0.06935(17) 0.0467(16) Uani 1 1 d . . . . .
H13 H 0.1572 0.5568 0.0550 0.070 Uiso 1 1 calc R U . . .
H14 H 0.2224 0.4765 0.0699 0.070 Uiso 1 1 calc R U . . .
H15 H 0.1841 0.4483 0.0973 0.070 Uiso 1 1 calc R U . . .
C22 C -0.1256(3) 0.5232(11) 0.08627(17) 0.056(2) Uani 1 1 d . . . . .
H8 H -0.1311 0.5701 0.0601 0.068 Uiso 1 1 calc R U . . .
C23 C 0.1737(3) 0.0009(11) -0.03984(18) 0.0548(19) Uani 1 1 d . . . . .
H16 H 0.1824 0.1090 -0.0531 0.082 Uiso 1 1 calc R U . . .
H17 H 0.1418 -0.0693 -0.0597 0.082 Uiso 1 1 calc R U . . .
H18 H 0.2086 -0.0768 -0.0289 0.082 Uiso 1 1 calc R U . . .
C24 C -0.1631(3) 0.4650(12) 0.13839(18) 0.063(2) Uani 1 1 d . . . . .
H9 H -0.1933 0.4755 0.1489 0.075 Uiso 1 1 calc R U . . .
C25 C 0.0591(3) -0.1218(10) 0.04872(17) 0.0514(17) Uani 1 1 d . . . . .
H19 H 0.0718 -0.1296 0.0784 0.077 Uiso 1 1 calc R U . . .
H20 H 0.0595 -0.2449 0.0375 0.077 Uiso 1 1 calc R U . . .
H21 H 0.0194 -0.0713 0.0373 0.077 Uiso 1 1 calc R U . . .
C26 C 0.2273(3) 0.0342(12) 0.27091(17) 0.065(2) Uani 1 1 d . . . . .
H10 H 0.2570 -0.0210 0.2637 0.079 Uiso 1 1 calc R U . . .
C27 C -0.1709(3) 0.5398(14) 0.1007(2) 0.084(3) Uani 1 1 d . . . . .
H11 H -0.2062 0.6010 0.0850 0.101 Uiso 1 1 calc R U . . .
C28 C 0.2324(3) 0.0350(13) 0.31112(17) 0.072(3) Uani 1 1 d . . . . .
H12 H 0.2644 -0.0267 0.3310 0.087 Uiso 1 1 calc R U . . .
O1 O -0.01344(15) 0.3077(6) 0.17411(9) 0.0344(10) Uani 1 1 d . . . . .
O2 O 0.08501(14) 0.2556(5) 0.22571(9) 0.0312(9) Uani 1 1 d . . . . .
N1 N 0.12821(19) 0.1880(7) 0.16773(11) 0.0354(12) Uani 1 1 d . . . . .
O3 O 0.10071(16) 0.2957(7) 0.30152(10) 0.0459(12) Uani 1 1 d . . . . .
N2 N 0.02328(18) 0.3247(6) 0.11211(10) 0.0281(10) Uani 1 1 d . . . . .
C29 C -0.0639(2) 0.3741(8) 0.14842(13) 0.0312(12) Uani 1 1 d . . . . .
C30 C 0.1356(2) 0.1971(8) 0.25206(13) 0.0321(13) Uani 1 1 d . . . . .
Na1 Na 0.0000 0.2623(6) 0.2500 0.0529(11) Uani 1 2 d S T P . .
O4 O 0.0785(2) 0.5450(6) 0.17792(12) 0.0511(12) Uani 1 1 d . . . . .
O5 O 0.0351(3) 0.0128(12) 0.16458(18) 0.109(2) Uani 1 1 d . . . . .
C31 C 0.1060(5) 0.6483(13) 0.1561(4) 0.102(4) Uani 1 1 d . . . . .
H41 H 0.1385 0.5769 0.1539 0.153 Uiso 1 1 calc R U . . .
H42 H 0.1212 0.7635 0.1706 0.153 Uiso 1 1 calc R U . . .
H43 H 0.0775 0.6758 0.1288 0.153 Uiso 1 1 calc R U . . .
C32 C -0.0273 -0.0783 0.1393 0.094(5) Uani 0.7 1 d . . P A 1
H34 H -0.0215 -0.1917 0.1263 0.140 Uiso 0.7 1 calc R U P A 1
H35 H -0.0510 0.0080 0.1184 0.140 Uiso 0.7 1 calc R U P A 1
H36 H -0.0474 -0.1069 0.1577 0.140 Uiso 0.7 1 calc R U P A 1
O6 O 0.0000 -0.0792(14) 0.2500 0.193(8) Uani 1 2 d S T P . .
H40 H 0.0323 -0.1177 0.2666 0.290 Uiso 0.5 1 calc R U P . .
C34 C -0.0030 -0.1920 0.1735 0.038(4) Uani 0.3 1 d . . P A 2
H37 H -0.0375 -0.1530 0.1789 0.057 Uiso 0.3 1 calc R U P A 2
H38 H 0.0236 -0.2605 0.1970 0.057 Uiso 0.3 1 calc R U P A 2
H39 H -0.0154 -0.2710 0.1494 0.057 Uiso 0.3 1 calc R U P A 2


_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 1.797(4) . ?
Al1 O2 1.817(3) . ?
Al1 O4 1.885(5) . ?
Al1 N1 1.944(4) . ?
Al1 N2 1.953(4) . ?
Al1 O5 2.111(9) . ?
Al1 Na1 3.5870(15) . ?
C1 C9 1.390(7) . ?
C1 N2 1.392(6) . ?
C1 C11 1.409(7) . ?
C2 C22 1.382(8) . ?
C2 C29 1.412(6) . ?
C2 C4 1.451(6) . ?
C3 C6 1.358(8) . ?
C3 C16 1.397(8) . ?
C3 C23 1.507(7) . ?
C4 N2 1.356(6) . ?
C4 C10 1.438(6) . ?
C5 C15 1.376(8) . ?
C5 C16 1.405(7) . ?
C5 C25 1.526(8) . ?
C6 C14 1.420(6) . ?
C7 C13 1.357(8) . ?
C7 C28 1.388(9) . ?
C8 N1 1.364(6) . ?
C8 C12 1.420(7) . ?
C8 C18 1.458(6) . ?
C9 C19 1.397(7) . ?
C9 C15 1.504(6) . ?
C10 C11 1.365(7) . ?
C12 C20 1.372(7) . ?
C13 O3 1.386(6) . ?
C13 C30 1.412(6) . ?
C14 C15 1.405(7) . ?
C14 C21 1.486(8) . ?
C17 C24 1.380(8) . ?
C17 O3 1.391(6) 2 ?
C17 C29 1.398(7) . ?
C18 C26 1.386(8) . ?
C18 C30 1.404(7) . ?
C19 C20 1.396(7) . ?
C19 N1 1.410(6) . ?
C22 C27 1.393(8) . ?
C24 C27 1.389(8) . ?
C26 C28 1.383(7) . ?
O1 C29 1.327(6) . ?
O1 Na1 2.605(3) . ?
O2 C30 1.316(6) . ?
O2 Na1 2.544(3) . ?
O3 C17 1.391(6) 2 ?
O3 Na1 2.480(4) . ?
Na1 O3 2.480(4) 2 ?
Na1 O6 2.483(11) . ?
Na1 O2 2.544(3) 2 ?
Na1 O1 2.605(3) 2 ?
Na1 Al1 3.5871(15) 2 ?
O4 C31 1.419(9) . ?
O5 C32 1.603(7) . ?
O5 C34 1.850(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
O1 Al1 O2 85.73(15) . . ?
O1 Al1 O4 99.4(2) . . ?
O2 Al1 O4 92.24(19) . . ?
O1 Al1 N1 159.7(2) . . ?
O2 Al1 N1 91.23(17) . . ?
O4 Al1 N1 100.7(2) . . ?
O1 Al1 N2 90.87(17) . . ?
O2 Al1 N2 175.7(2) . . ?
O4 Al1 N2 90.9(2) . . ?
N1 Al1 N2 91.07(17) . . ?
O1 Al1 O5 80.6(2) . . ?
O2 Al1 O5 86.8(2) . . ?
O4 Al1 O5 179.0(2) . . ?
N1 Al1 O5 79.2(2) . . ?
N2 Al1 O5 90.1(2) . . ?
O1 Al1 Na1 43.78(10) . . ?
O2 Al1 Na1 41.95(11) . . ?
O4 Al1 Na1 97.51(15) . . ?
N1 Al1 Na1 130.23(14) . . ?
N2 Al1 Na1 134.61(13) . . ?
O5 Al1 Na1 81.83(18) . . ?
C9 C1 N2 123.6(4) . . ?
C9 C1 C11 127.3(4) . . ?
N2 C1 C11 109.1(4) . . ?
C22 C2 C29 119.6(5) . . ?
C22 C2 C4 120.8(4) . . ?
C29 C2 C4 119.5(5) . . ?
C6 C3 C16 118.6(5) . . ?
C6 C3 C23 122.1(5) . . ?
C16 C3 C23 119.3(5) . . ?
N2 C4 C10 109.6(4) . . ?
N2 C4 C2 124.1(4) . . ?
C10 C4 C2 126.0(5) . . ?
C15 C5 C16 119.7(5) . . ?
C15 C5 C25 121.8(5) . . ?
C16 C5 C25 118.6(6) . . ?
C3 C6 C14 123.1(5) . . ?
C13 C7 C28 118.2(5) . . ?
N1 C8 C12 110.5(4) . . ?
N1 C8 C18 123.7(4) . . ?
C12 C8 C18 125.8(5) . . ?
C1 C9 C19 124.3(4) . . ?
C1 C9 C15 117.9(4) . . ?
C19 C9 C15 117.7(4) . . ?
C11 C10 C4 106.4(4) . . ?
C10 C11 C1 108.0(4) . . ?
C20 C12 C8 106.4(5) . . ?
C7 C13 O3 123.9(4) . . ?
C7 C13 C30 122.8(5) . . ?
O3 C13 C30 113.1(4) . . ?
C15 C14 C6 116.7(5) . . ?
C15 C14 C21 122.8(4) . . ?
C6 C14 C21 120.5(5) . . ?
C5 C15 C14 121.4(4) . . ?
C5 C15 C9 117.9(4) . . ?
C14 C15 C9 120.7(5) . . ?
C3 C16 C5 120.6(6) . . ?
C24 C17 O3 123.6(5) . 2 ?
C24 C17 C29 121.6(5) . . ?
O3 C17 C29 114.5(5) 2 . ?
C26 C18 C30 119.6(5) . . ?
C26 C18 C8 119.9(5) . . ?
C30 C18 C8 120.5(5) . . ?
C20 C19 C9 126.5(4) . . ?
C20 C19 N1 109.1(4) . . ?
C9 C19 N1 124.4(5) . . ?
C12 C20 C19 108.2(4) . . ?
C2 C22 C27 121.8(5) . . ?
C17 C24 C27 120.1(5) . . ?
C28 C26 C18 120.2(6) . . ?
C24 C27 C22 118.6(6) . . ?
C26 C28 C7 121.2(6) . . ?
C29 O1 Al1 131.5(3) . . ?
C29 O1 Na1 118.6(3) . . ?
Al1 O1 Na1 107.72(15) . . ?
C30 O2 Al1 132.8(3) . . ?
C30 O2 Na1 116.5(3) . . ?
Al1 O2 Na1 109.53(16) . . ?
C8 N1 C19 105.7(4) . . ?
C8 N1 Al1 126.6(3) . . ?
C19 N1 Al1 127.2(3) . . ?
C13 O3 C17 120.0(4) . 2 ?
C13 O3 Na1 117.2(3) . . ?
C17 O3 Na1 122.0(3) 2 . ?
C4 N2 C1 106.8(4) . . ?
C4 N2 Al1 123.9(3) . . ?
C1 N2 Al1 127.9(3) . . ?
O1 C29 C17 118.1(4) . . ?
O1 C29 C2 124.3(4) . . ?
C17 C29 C2 117.6(5) . . ?
O2 C30 C18 124.0(4) . . ?
O2 C30 C13 118.2(4) . . ?
C18 C30 C13 117.6(5) . . ?
O3 Na1 O3 168.8(3) 2 . ?
O3 Na1 O6 95.61(15) 2 . ?
O3 Na1 O6 95.61(15) . . ?
O3 Na1 O2 118.36(10) 2 . ?
O3 Na1 O2 61.88(10) . . ?
O6 Na1 O2 88.89(13) . . ?
O3 Na1 O2 61.88(10) 2 2 ?
O3 Na1 O2 118.37(10) . 2 ?
O6 Na1 O2 88.89(13) . 2 ?
O2 Na1 O2 177.8(3) . 2 ?
O3 Na1 O1 61.44(11) 2 . ?
O3 Na1 O1 116.96(12) . . ?
O6 Na1 O1 97.27(13) . . ?
O2 Na1 O1 57.02(10) . . ?
O2 Na1 O1 123.31(10) 2 . ?
O3 Na1 O1 116.96(12) 2 2 ?
O3 Na1 O1 61.44(11) . 2 ?
O6 Na1 O1 97.27(13) . 2 ?
O2 Na1 O1 123.31(10) . 2 ?
O2 Na1 O1 57.03(10) 2 2 ?
O1 Na1 O1 165.5(3) . 2 ?
O3 Na1 Al1 89.90(8) 2 . ?
O3 Na1 Al1 89.37(8) . . ?
O6 Na1 Al1 93.71(8) . . ?
O2 Na1 Al1 28.52(8) . . ?
O2 Na1 Al1 151.78(8) 2 . ?
O1 Na1 Al1 28.51(8) . . ?
O1 Na1 Al1 149.59(10) 2 . ?
O3 Na1 Al1 89.37(8) 2 2 ?
O3 Na1 Al1 89.91(8) . 2 ?
O6 Na1 Al1 93.71(8) . 2 ?
O2 Na1 Al1 151.78(8) . 2 ?
O2 Na1 Al1 28.52(8) 2 2 ?
O1 Na1 Al1 149.59(10) . 2 ?
O1 Na1 Al1 28.50(8) 2 2 ?
Al1 Na1 Al1 172.59(15) . 2 ?
C31 O4 Al1 127.2(5) . . ?
C32 O5 Al1 128.3(4) . . ?
C34 O5 Al1 153.1(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C22 C2 C4 N2 -177.7(6) . . . . ?
C29 C2 C4 N2 -1.5(9) . . . . ?
C22 C2 C4 C10 -3.8(10) . . . . ?
C29 C2 C4 C10 172.4(6) . . . . ?
C16 C3 C6 C14 -1.1(8) . . . . ?
C23 C3 C6 C14 -179.5(6) . . . . ?
N2 C1 C9 C19 -8.1(9) . . . . ?
C11 C1 C9 C19 173.6(6) . . . . ?
N2 C1 C9 C15 167.8(5) . . . . ?
C11 C1 C9 C15 -10.5(9) . . . . ?
N2 C4 C10 C11 2.4(7) . . . . ?
C2 C4 C10 C11 -172.2(6) . . . . ?
C4 C10 C11 C1 -1.6(7) . . . . ?
C9 C1 C11 C10 178.8(6) . . . . ?
N2 C1 C11 C10 0.3(7) . . . . ?
N1 C8 C12 C20 -0.1(8) . . . . ?
C18 C8 C12 C20 -179.0(6) . . . . ?
C28 C7 C13 O3 178.1(7) . . . . ?
C28 C7 C13 C30 3.4(11) . . . . ?
C3 C6 C14 C15 1.6(8) . . . . ?
C3 C6 C14 C21 -179.1(5) . . . . ?
C16 C5 C15 C14 0.8(8) . . . . ?
C25 C5 C15 C14 -179.2(6) . . . . ?
C16 C5 C15 C9 -178.8(5) . . . . ?
C25 C5 C15 C9 1.1(8) . . . . ?
C6 C14 C15 C5 -1.4(8) . . . . ?
C21 C14 C15 C5 179.3(5) . . . . ?
C6 C14 C15 C9 178.3(5) . . . . ?
C21 C14 C15 C9 -1.0(8) . . . . ?
C1 C9 C15 C5 -84.2(7) . . . . ?
C19 C9 C15 C5 92.0(6) . . . . ?
C1 C9 C15 C14 96.1(6) . . . . ?
C19 C9 C15 C14 -87.7(7) . . . . ?
C6 C3 C16 C5 0.5(8) . . . . ?
C23 C3 C16 C5 178.9(6) . . . . ?
C15 C5 C16 C3 -0.4(9) . . . . ?
C25 C5 C16 C3 179.7(6) . . . . ?
N1 C8 C18 C26 -178.4(7) . . . . ?
C12 C8 C18 C26 0.3(11) . . . . ?
N1 C8 C18 C30 2.0(10) . . . . ?
C12 C8 C18 C30 -179.3(6) . . . . ?
C1 C9 C19 C20 177.5(6) . . . . ?
C15 C9 C19 C20 1.5(9) . . . . ?
C1 C9 C19 N1 -3.7(10) . . . . ?
C15 C9 C19 N1 -179.6(5) . . . . ?
C8 C12 C20 C19 -0.4(8) . . . . ?
C9 C19 C20 C12 179.8(6) . . . . ?
N1 C19 C20 C12 0.8(7) . . . . ?
C29 C2 C22 C27 -1.5(12) . . . . ?
C4 C2 C22 C27 174.7(7) . . . . ?
O3 C17 C24 C27 -179.5(8) 2 . . . ?
C29 C17 C24 C27 7.0(12) . . . . ?
C30 C18 C26 C28 0.7(12) . . . . ?
C8 C18 C26 C28 -178.8(7) . . . . ?
C17 C24 C27 C22 -0.5(14) . . . . ?
C2 C22 C27 C24 -2.2(14) . . . . ?
C18 C26 C28 C7 -3.9(14) . . . . ?
C13 C7 C28 C26 1.9(13) . . . . ?
O2 Al1 O1 C29 163.1(5) . . . . ?
O4 Al1 O1 C29 71.6(5) . . . . ?
N1 Al1 O1 C29 -114.9(6) . . . . ?
N2 Al1 O1 C29 -19.5(5) . . . . ?
O5 Al1 O1 C29 -109.4(5) . . . . ?
Na1 Al1 O1 C29 162.6(6) . . . . ?
O2 Al1 O1 Na1 0.5(2) . . . . ?
O4 Al1 O1 Na1 -91.0(2) . . . . ?
N1 Al1 O1 Na1 82.5(5) . . . . ?
N2 Al1 O1 Na1 177.9(2) . . . . ?
O5 Al1 O1 Na1 88.0(2) . . . . ?
O1 Al1 O2 C30 166.4(5) . . . . ?
O4 Al1 O2 C30 -94.3(5) . . . . ?
N1 Al1 O2 C30 6.5(5) . . . . ?
O5 Al1 O2 C30 85.6(5) . . . . ?
Na1 Al1 O2 C30 166.9(6) . . . . ?
O1 Al1 O2 Na1 -0.5(2) . . . . ?
O4 Al1 O2 Na1 98.8(2) . . . . ?
N1 Al1 O2 Na1 -160.5(2) . . . . ?
O5 Al1 O2 Na1 -81.3(3) . . . . ?
C12 C8 N1 C19 0.6(7) . . . . ?
C18 C8 N1 C19 179.5(6) . . . . ?
C12 C8 N1 Al1 173.1(4) . . . . ?
C18 C8 N1 Al1 -8.0(9) . . . . ?
C20 C19 N1 C8 -0.9(7) . . . . ?
C9 C19 N1 C8 -179.9(6) . . . . ?
C20 C19 N1 Al1 -173.4(5) . . . . ?
C9 C19 N1 Al1 7.6(9) . . . . ?
C7 C13 O3 C17 28.1(9) . . . 2 ?
C30 C13 O3 C17 -156.7(5) . . . 2 ?
C7 C13 O3 Na1 -142.3(5) . . . . ?
C30 C13 O3 Na1 32.8(6) . . . . ?
C10 C4 N2 C1 -2.2(6) . . . . ?
C2 C4 N2 C1 172.6(5) . . . . ?
C10 C4 N2 Al1 165.6(4) . . . . ?
C2 C4 N2 Al1 -19.7(8) . . . . ?
C9 C1 N2 C4 -177.4(5) . . . . ?
C11 C1 N2 C4 1.2(6) . . . . ?
C9 C1 N2 Al1 15.5(8) . . . . ?
C11 C1 N2 Al1 -165.9(4) . . . . ?
Al1 O1 C29 C17 -176.0(4) . . . . ?
Na1 O1 C29 C17 -14.9(7) . . . . ?
Al1 O1 C29 C2 5.4(9) . . . . ?
Na1 O1 C29 C2 166.4(5) . . . . ?
C24 C17 C29 O1 170.7(7) . . . . ?
O3 C17 C29 O1 -3.3(8) 2 . . . ?
C24 C17 C29 C2 -10.5(10) . . . . ?
O3 C17 C29 C2 175.5(5) 2 . . . ?
C22 C2 C29 O1 -173.7(6) . . . . ?
C4 C2 C29 O1 10.1(9) . . . . ?
C22 C2 C29 C17 7.7(9) . . . . ?
C4 C2 C29 C17 -168.5(6) . . . . ?
Al1 O2 C30 C18 -13.3(9) . . . . ?
Na1 O2 C30 C18 152.9(5) . . . . ?
Al1 O2 C30 C13 171.4(4) . . . . ?
Na1 O2 C30 C13 -22.4(7) . . . . ?
C26 C18 C30 O2 -171.1(6) . . . . ?
C8 C18 C30 O2 8.4(10) . . . . ?
C26 C18 C30 C13 4.2(10) . . . . ?
C8 C18 C30 C13 -176.2(5) . . . . ?
C7 C13 C30 O2 169.2(6) . . . . ?
O3 C13 C30 O2 -6.0(8) . . . . ?
C7 C13 C30 C18 -6.4(9) . . . . ?
O3 C13 C30 C18 178.3(5) . . . . ?
O1 Al1 O4 C31 -137.5(7) . . . . ?
O2 Al1 O4 C31 136.4(7) . . . . ?
N1 Al1 O4 C31 44.7(8) . . . . ?
N2 Al1 O4 C31 -46.5(7) . . . . ?
Na1 Al1 O4 C31 178.2(7) . . . . ?

_refine_diff_density_max         3.615
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.157



####################################################################### 
# 
# 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_cycn2o6_0m_a_sqd
_database_code_depnum_ccdc_archive 'CCDC 1446113'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H100 N8 O12'
_chemical_formula_weight         1846.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   23.498(4)
_cell_length_b                   38.393(7)
_cell_length_c                   23.360(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.080(3)
_cell_angle_gamma                90
_cell_volume                     21071(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9398
_cell_measurement_theta_min      2.199
_cell_measurement_theta_max      24.277

_exptl_crystal_description       purple
_exptl_crystal_colour            block
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_F_000             7776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.076
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6541
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   
;    
 SADABS-2014/4 - Bruker AXS area detector scaling and absorption correction 
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50237
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.016
_diffrn_reflns_theta_max         24.850
_diffrn_reflns_theta_full        24.850
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             18144
_reflns_number_gt                11457
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1000P)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         18144
_refine_ls_number_parameters     1296
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1857
_refine_ls_wR_factor_gt          0.1701
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_DIFMX01_cycn2o6_0m_a_sqd    
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*2.00
RESPONSE: Solvent accessible voids of 2831 cubic angstroms were found,
where solvent molecules (chloroform and hexane) were heavily disordered.
The electron densities in the voids were treated by the SQUEEZE program.
Residual electron densities around the water molecules in the macrocycles
due to the disordred solvent molecules were not fully determined.
;
_vrf_PLAT097_cycn2o6_0m_a_sqd    
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       1.61 eA-3  
RESPONSE: Solvent accessible voids of 2831 cubic angstroms were found,
where solvent molecules (chloroform and hexane) were heavily disordered.
The electron densities in the voids were treated by the SQUEEZE program.
Residual electron densities around the water molecules in the macrocycles
due to the disordred solvent molecules were not fully determined.
;
# end Validation Reply Form

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.42095(8) 0.80021(4) 0.04026(7) 0.0315(4) Uani 1 1 d . . . . .
H112 H 0.4172 0.7794 0.0505 0.047 Uiso 1 1 calc R U . . .
O2 O 0.70462(8) 0.79971(4) 0.17326(7) 0.0325(5) Uani 1 1 d . . . . .
H106 H 0.6962 0.7789 0.1660 0.049 Uiso 1 1 calc R U . . .
O3 O 0.65441(9) 0.70721(4) 0.06157(8) 0.0392(5) Uani 1 1 d . . . . .
H107 H 0.6563 0.7162 0.0943 0.059 Uiso 1 1 calc R U . . .
O4 O 0.33635(9) 0.77370(4) 0.10597(9) 0.0417(5) Uani 1 1 d . . . . .
O5 O 0.31303(9) 0.70622(5) 0.09374(9) 0.0384(5) Uani 1 1 d . . . . .
H113 H 0.3446 0.7165 0.0944 0.058 Uiso 1 1 calc R U . . .
O6 O 0.63663(9) 0.77411(5) 0.08735(8) 0.0423(5) Uani 1 1 d . . . . .
O7 O 0.39888(9) 0.65864(5) 0.01910(9) 0.0454(5) Uani 1 1 d . . . . .
H114 H 0.3691 0.6485 0.0293 0.068 Uiso 1 1 calc R U . . .
O8 O 0.50887(10) 0.75623(5) -0.00792(9) 0.0482(6) Uani 1 1 d . . . . .
H115 H 0.5130 0.7767 -0.0196 0.072 Uiso 1 1 calc R U . . .
N1 N 0.47495(9) 0.85676(5) -0.00209(8) 0.0258(5) Uani 1 1 d . . . . .
H116 H 0.4750 0.8340 -0.0067 0.031 Uiso 1 1 calc R U . . .
N2 N 0.74879(9) 0.85528(5) 0.22933(8) 0.0274(5) Uani 1 1 d . . . . .
H108 H 0.7542 0.8326 0.2280 0.033 Uiso 1 1 calc R U . . .
O9 O 0.75808(10) 0.75500(5) 0.25876(9) 0.0529(6) Uani 1 1 d . . . . .
H109 H 0.7692 0.7755 0.2647 0.079 Uiso 1 1 calc R U . . .
O10 O 0.73314(11) 0.65844(5) 0.14651(8) 0.0511(6) Uani 1 1 d . . . . .
H110 H 0.7271 0.6473 0.1160 0.077 Uiso 1 1 calc R U . . .
N3 N 0.23883(10) 0.65468(5) 0.06526(8) 0.0295(5) Uani 1 1 d . . . . .
H117 H 0.2761 0.6570 0.0661 0.035 Uiso 1 1 calc R U . . .
N4 N 0.53128(9) 0.80677(5) -0.08041(9) 0.0292(5) Uani 1 1 d . . . . .
N5 N 0.69272(10) 0.60772(5) 0.08071(9) 0.0301(5) Uani 1 1 d . . . . .
N6 N 0.68638(10) 0.65787(5) -0.01366(9) 0.0303(5) Uani 1 1 d . . . . .
H111 H 0.6844 0.6595 0.0238 0.036 Uiso 1 1 calc R U . . .
N7 N 0.33581(10) 0.60654(5) 0.05778(9) 0.0308(5) Uani 1 1 d . . . . .
N8 N 0.83019(10) 0.80539(5) 0.28276(9) 0.0315(5) Uani 1 1 d . . . . .
O11 O 0.50089(10) 0.69019(5) 0.01637(11) 0.0622(7) Uani 1 1 d . . . . .
O12 O 0.73298(12) 0.68971(5) 0.24956(10) 0.0658(8) Uani 1 1 d . . . . .
C1 C 0.44586(12) 0.87396(7) 0.03931(11) 0.0284(6) Uani 1 1 d . . . . .
C2 C 0.70552(12) 0.87266(7) 0.20164(10) 0.0290(6) Uani 1 1 d . . . . .
C3 C 0.78284(12) 0.87846(7) 0.25976(10) 0.0292(6) Uani 1 1 d . . . . .
C4 C 0.55154(12) 0.78188(7) -0.11421(12) 0.0315(6) Uani 1 1 d . . . . .
C5 C 0.54843(12) 0.83860(7) -0.10481(11) 0.0291(6) Uani 1 1 d . . . . .
C6 C 0.45669(12) 0.90925(7) 0.03254(11) 0.0319(7) Uani 1 1 d . . . . .
H23 H 0.4421 0.9276 0.0554 0.038 Uiso 1 1 calc R U . . .
C7 C 0.50424(11) 0.87996(6) -0.03570(11) 0.0272(6) Uani 1 1 d . . . . .
C8 C 0.71108(13) 0.90760(7) 0.21548(11) 0.0316(6) Uani 1 1 d . . . . .
H13 H 0.6866 0.9259 0.2029 0.038 Uiso 1 1 calc R U . . .
C9 C 0.38525(13) 0.58874(7) 0.06052(11) 0.0322(7) Uani 1 1 d . . . . .
C10 C 0.29220(13) 0.58194(7) 0.06176(11) 0.0318(7) Uani 1 1 d . . . . .
C11 C 0.53808(12) 0.87129(7) -0.08380(11) 0.0290(6) Uani 1 1 d . . . . .
C12 C 0.68911(12) 0.62660(7) -0.04438(11) 0.0302(6) Uani 1 1 d . . . . .
C13 C 0.40716(12) 0.85712(6) 0.07966(11) 0.0295(6) Uani 1 1 d . . . . .
C14 C 0.39311(12) 0.82147(7) 0.07743(11) 0.0294(6) Uani 1 1 d . . . . .
C15 C 0.68860(12) 0.58938(7) 0.12917(12) 0.0326(7) Uani 1 1 d . . . . .
C16 C 0.66648(12) 0.82111(7) 0.14691(11) 0.0310(6) Uani 1 1 d . . . . .
C17 C 0.85474(12) 0.83693(7) 0.30112(11) 0.0327(7) Uani 1 1 d . . . . .
C18 C 0.68779(12) 0.58392(7) 0.03592(11) 0.0311(6) Uani 1 1 d . . . . .
C19 C 0.27035(13) 0.72993(7) 0.08375(11) 0.0301(7) Uani 1 1 d . . . . .
C20 C 0.68718(12) 0.68530(6) -0.05004(11) 0.0285(6) Uani 1 1 d . . . . .
C21 C 0.20114(12) 0.68136(7) 0.06602(10) 0.0297(6) Uani 1 1 d . . . . .
C22 C 0.20989(13) 0.62301(7) 0.06297(11) 0.0321(7) Uani 1 1 d . . . . .
C23 C 0.21585(13) 0.71805(7) 0.06927(10) 0.0296(6) Uani 1 1 d . . . . .
C24 C 0.66500(12) 0.73214(7) 0.02124(11) 0.0312(7) Uani 1 1 d . . . . .
C25 C 0.83280(12) 0.86953(7) 0.29181(11) 0.0311(6) Uani 1 1 d . . . . .
C26 C 0.65742(13) 0.76738(7) 0.03257(12) 0.0337(7) Uani 1 1 d . . . . .
C27 C 0.28053(13) 0.76570(7) 0.08848(11) 0.0326(7) Uani 1 1 d . . . . .
C28 C 0.75877(13) 0.91119(7) 0.25111(11) 0.0330(7) Uani 1 1 d . . . . .
H14 H 0.7726 0.9324 0.2669 0.040 Uiso 1 1 calc R U . . .
C29 C 0.86367(13) 0.89988(7) 0.31921(11) 0.0342(7) Uani 1 1 d . . . . .
C30 C 0.66416(12) 0.85625(7) 0.16266(11) 0.0303(6) Uani 1 1 d . . . . .
C31 C 0.68232(12) 0.72171(7) -0.03341(11) 0.0306(6) Uani 1 1 d . . . . .
C32 C 0.49275(12) 0.91305(7) -0.01357(11) 0.0326(7) Uani 1 1 d . . . . .
H24 H 0.5071 0.9345 -0.0277 0.039 Uiso 1 1 calc R U . . .
C33 C 0.23442(13) 0.58960(7) 0.06307(11) 0.0331(7) Uani 1 1 d . . . . .
C34 C 0.69482(12) 0.74771(7) -0.07345(12) 0.0354(7) Uani 1 1 d . . . . .
H1 H 0.7068 0.7412 -0.1106 0.042 Uiso 1 1 calc R U . . .
C35 C 0.69160(14) 0.60615(7) 0.18524(11) 0.0373(7) Uani 1 1 d . . . . .
C36 C 0.69223(13) 0.63639(7) -0.10242(11) 0.0340(7) Uani 1 1 d . . . . .
H2 H 0.6946 0.6209 -0.1339 0.041 Uiso 1 1 calc R U . . .
C37 C 0.69129(13) 0.67207(7) -0.10588(12) 0.0347(7) Uani 1 1 d . . . . .
H3 H 0.6931 0.6855 -0.1400 0.042 Uiso 1 1 calc R U . . .
C38 C 0.68134(13) 0.54968(7) 0.05910(12) 0.0367(7) Uani 1 1 d . . . . .
H4 H 0.6778 0.5286 0.0381 0.044 Uiso 1 1 calc R U . . .
C39 C 0.68750(12) 0.59302(7) -0.02174(11) 0.0323(7) Uani 1 1 d . . . . .
C40 C 0.38040(13) 0.87757(7) 0.12060(12) 0.0367(7) Uani 1 1 d . . . . .
H25 H 0.3895 0.9016 0.1229 0.044 Uiso 1 1 calc R U . . .
C41 C 0.56593(13) 0.90165(7) -0.11254(11) 0.0347(7) Uani 1 1 d . . . . .
C42 C 0.54582(12) 0.74492(7) -0.10199(12) 0.0332(7) Uani 1 1 d . . . . .
C43 C 0.86555(13) 0.78034(7) 0.30166(11) 0.0352(7) Uani 1 1 d . . . . .
C44 C 0.57961(13) 0.83115(7) -0.15617(12) 0.0374(7) Uani 1 1 d . . . . .
H26 H 0.5959 0.8478 -0.1811 0.045 Uiso 1 1 calc R U . . .
C45 C 0.85309(14) 0.74336(7) 0.29426(11) 0.0372(7) Uani 1 1 d . . . . .
C46 C 0.68123(13) 0.55314(7) 0.11711(12) 0.0364(7) Uani 1 1 d . . . . .
H5 H 0.6771 0.5350 0.1443 0.044 Uiso 1 1 calc R U . . .
C47 C 0.31714(14) 0.54801(7) 0.06629(12) 0.0367(7) Uani 1 1 d . . . . .
H60 H 0.2972 0.5266 0.0688 0.044 Uiso 1 1 calc R U . . .
C48 C 0.44021(13) 0.60569(7) 0.05673(12) 0.0376(7) Uani 1 1 d . . . . .
C49 C 0.14626(13) 0.66699(7) 0.06406(11) 0.0351(7) Uani 1 1 d . . . . .
H37 H 0.1116 0.6797 0.0640 0.042 Uiso 1 1 calc R U . . .
C50 C 0.23866(14) 0.78950(7) 0.07527(12) 0.0382(8) Uani 1 1 d . . . . .
H38 H 0.2467 0.8137 0.0768 0.046 Uiso 1 1 calc R U . . .
C51 C 0.52546(12) 0.73368(7) -0.04895(13) 0.0363(7) Uani 1 1 d . . . . .
C52 C 0.35071(14) 0.80870(7) 0.11240(12) 0.0381(7) Uani 1 1 d . . . . .
C53 C 0.37443(14) 0.55205(7) 0.06631(12) 0.0373(7) Uani 1 1 d . . . . .
H61 H 0.4021 0.5341 0.0695 0.045 Uiso 1 1 calc R U . . .
C54 C 0.63013(14) 0.80889(7) 0.10333(12) 0.0398(7) Uani 1 1 d . . . . .
C55 C 0.17327(14) 0.74301(7) 0.05758(11) 0.0351(7) Uani 1 1 d . . . . .
H39 H 0.1358 0.7355 0.0480 0.042 Uiso 1 1 calc R U . . .
C56 C 0.69009(13) 0.78225(7) -0.05987(13) 0.0378(7) Uani 1 1 d . . . . .
H6 H 0.6999 0.7994 -0.0873 0.045 Uiso 1 1 calc R U . . .
C57 C 0.18511(15) 0.77804(7) 0.05986(12) 0.0394(7) Uani 1 1 d . . . . .
H40 H 0.1561 0.7945 0.0507 0.047 Uiso 1 1 calc R U . . .
C58 C 0.58131(13) 0.79639(7) -0.16218(12) 0.0390(7) Uani 1 1 d . . . . .
H27 H 0.5987 0.7838 -0.1922 0.047 Uiso 1 1 calc R U . . .
C59 C 0.68447(14) 0.56474(7) -0.06675(12) 0.0380(7) Uani 1 1 d . . . . .
C60 C 0.44473(14) 0.64000(7) 0.03642(13) 0.0422(8) Uani 1 1 d . . . . .
C61 C 0.15128(13) 0.63129(7) 0.06219(12) 0.0371(7) Uani 1 1 d . . . . .
H41 H 0.1207 0.6151 0.0607 0.045 Uiso 1 1 calc R U . . .
C62 C 0.56159(13) 0.71964(7) -0.14247(14) 0.0409(7) Uani 1 1 d . . . . .
H28 H 0.5760 0.7267 -0.1783 0.049 Uiso 1 1 calc R U . . .
C63 C 0.90748(14) 0.82937(8) 0.33112(12) 0.0412(7) Uani 1 1 d . . . . .
H15 H 0.9327 0.8460 0.3479 0.049 Uiso 1 1 calc R U . . .
C64 C 0.90439(13) 0.91822(7) 0.28882(13) 0.0385(7) Uani 1 1 d . . . . .
C65 C 0.67127(13) 0.79249(7) -0.00701(13) 0.0397(7) Uani 1 1 d . . . . .
H7 H 0.6679 0.8165 0.0021 0.048 Uiso 1 1 calc R U . . .
C66 C 0.53551(15) 0.92193(7) -0.15228(12) 0.0417(8) Uani 1 1 d . . . . .
C67 C 0.62186(13) 0.87709(7) 0.13661(12) 0.0395(7) Uani 1 1 d . . . . .
H16 H 0.6194 0.9010 0.1470 0.047 Uiso 1 1 calc R U . . .
C68 C 0.91455(13) 0.79490(8) 0.33107(12) 0.0412(7) Uani 1 1 d . . . . .
H17 H 0.9458 0.7824 0.3473 0.049 Uiso 1 1 calc R U . . .
C69 C 0.71366(15) 0.63977(7) 0.19142(12) 0.0428(8) Uani 1 1 d . . . . .
C70 C 0.79995(15) 0.73243(7) 0.27402(11) 0.0388(8) Uani 1 1 d . . . . .
C71 C 0.19185(14) 0.56007(7) 0.06605(14) 0.0436(8) Uani 1 1 d . . . . .
C72 C 0.55621(14) 0.68473(8) -0.13035(15) 0.0467(8) Uani 1 1 d . . . . .
H29 H 0.5663 0.6679 -0.1582 0.056 Uiso 1 1 calc R U . . .
C73 C 0.89412(15) 0.71791(8) 0.30933(13) 0.0457(8) Uani 1 1 d . . . . .
H18 H 0.9304 0.7249 0.3238 0.055 Uiso 1 1 calc R U . . .
C74 C 0.73474(16) 0.55081(7) -0.08796(14) 0.0474(9) Uani 1 1 d . . . . .
C75 C 0.49068(14) 0.58864(8) 0.07374(14) 0.0471(8) Uani 1 1 d . . . . .
H62 H 0.4886 0.5653 0.0871 0.057 Uiso 1 1 calc R U . . .
C76 C 0.78795(16) 0.69710(7) 0.26931(12) 0.0468(9) Uani 1 1 d . . . . .
C77 C 0.63175(16) 0.55499(7) -0.09038(13) 0.0462(8) Uani 1 1 d . . . . .
C78 C 0.34142(15) 0.86403(7) 0.15766(13) 0.0475(9) Uani 1 1 d . . . . .
H30 H 0.3254 0.8784 0.1862 0.057 Uiso 1 1 calc R U . . .
C79 C 0.85060(14) 0.90924(8) 0.37528(13) 0.0465(8) Uani 1 1 d . . . . .
C80 C 0.52105(13) 0.69800(7) -0.03798(15) 0.0442(8) Uani 1 1 d . . . . .
C81 C 0.53598(13) 0.67382(7) -0.07731(15) 0.0455(8) Uani 1 1 d . . . . .
H31 H 0.5327 0.6497 -0.0689 0.055 Uiso 1 1 calc R U . . .
C82 C 0.67141(15) 0.58932(8) 0.23405(13) 0.0476(9) Uani 1 1 d . . . . .
H8 H 0.6565 0.5664 0.2305 0.057 Uiso 1 1 calc R U . . .
C83 C 0.62240(14) 0.90968(8) -0.09775(13) 0.0447(8) Uani 1 1 d . . . . .
C84 C 0.49836(15) 0.65529(7) 0.03373(15) 0.0508(9) Uani 1 1 d . . . . .
C85 C 0.82885(18) 0.67244(8) 0.28316(12) 0.0510(10) Uani 1 1 d . . . . .
H19 H 0.8206 0.6483 0.2790 0.061 Uiso 1 1 calc R U . . .
C86 C 0.58391(15) 0.86399(8) 0.09660(14) 0.0497(9) Uani 1 1 d . . . . .
H20 H 0.5547 0.8784 0.0808 0.060 Uiso 1 1 calc R U . . .
C87 C 0.58877(15) 0.82947(8) 0.07955(14) 0.0531(9) Uani 1 1 d . . . . .
H21 H 0.5633 0.8202 0.0514 0.064 Uiso 1 1 calc R U . . .
C88 C 0.88181(17) 0.68308(8) 0.30314(13) 0.0518(9) Uani 1 1 d . . . . .
H22 H 0.9099 0.6662 0.3127 0.062 Uiso 1 1 calc R U . . .
C89 C 0.16703(14) 0.55139(8) 0.11792(16) 0.0505(9) Uani 1 1 d . . . . .
C90 C 0.32550(15) 0.82946(8) 0.15340(14) 0.0500(9) Uani 1 1 d . . . . .
H32 H 0.2978 0.8201 0.1781 0.060 Uiso 1 1 calc R U . . .
C91 C 0.92186(15) 0.90588(8) 0.23024(13) 0.0492(8) Uani 1 1 d . . . . .
H42 H 0.9507 0.9217 0.2151 0.074 Uiso 1 1 calc R U . . .
H43 H 0.9377 0.8823 0.2333 0.074 Uiso 1 1 calc R U . . .
H44 H 0.8885 0.9056 0.2044 0.074 Uiso 1 1 calc R U . . .
C92 C 0.91748(15) 0.95752(8) 0.36993(17) 0.0551(10) Uani 1 1 d . . . . .
C93 C 0.71518(17) 0.65510(7) 0.24536(13) 0.0546(10) Uani 1 1 d . . . . .
C94 C 0.56264(19) 0.95085(8) -0.17601(13) 0.0564(10) Uani 1 1 d . . . . .
H35 H 0.5424 0.9647 -0.2033 0.068 Uiso 1 1 calc R U . . .
C95 C 0.7301(2) 0.52776(8) -0.13522(15) 0.0606(11) Uani 1 1 d . . . . .
H9 H 0.7639 0.5183 -0.1507 0.073 Uiso 1 1 calc R U . . .
C96 C 0.64782(17) 0.93894(9) -0.12254(15) 0.0595(10) Uani 1 1 d . . . . .
H36 H 0.6862 0.9445 -0.1127 0.071 Uiso 1 1 calc R U . . .
C97 C 0.17438(17) 0.54236(8) 0.01663(16) 0.0583(10) Uani 1 1 d . . . . .
C98 C 0.87771(16) 0.93825(9) 0.39961(15) 0.0570(10) Uani 1 1 d . . . . .
H33 H 0.8687 0.9450 0.4375 0.068 Uiso 1 1 calc R U . . .
C99 C 0.47647(16) 0.91157(9) -0.17175(15) 0.0612(10) Uani 1 1 d . . . . .
H94 H 0.4778 0.8888 -0.1905 0.092 Uiso 1 1 calc R U . . .
H95 H 0.4615 0.9289 -0.1989 0.092 Uiso 1 1 calc R U . . .
H96 H 0.4516 0.9103 -0.1386 0.092 Uiso 1 1 calc R U . . .
C100 C 0.67254(18) 0.60505(8) 0.28713(13) 0.0568(10) Uani 1 1 d . . . . .
H10 H 0.6587 0.5931 0.3196 0.068 Uiso 1 1 calc R U . . .
C101 C 0.79093(16) 0.56062(8) -0.06352(17) 0.0612(10) Uani 1 1 d . . . . .
H76 H 0.7959 0.5859 -0.0663 0.092 Uiso 1 1 calc R U . . .
H77 H 0.8209 0.5489 -0.0848 0.092 Uiso 1 1 calc R U . . .
H78 H 0.7932 0.5536 -0.0232 0.092 Uiso 1 1 calc R U . . .
C102 C 0.54272(15) 0.60452(8) 0.07171(17) 0.0581(10) Uani 1 1 d . . . . .
H63 H 0.5761 0.5923 0.0836 0.070 Uiso 1 1 calc R U . . .
C103 C 0.6183(2) 0.95991(9) -0.16089(15) 0.0613(11) Uani 1 1 d . . . . .
C104 C 0.6300(2) 0.53193(8) -0.13589(14) 0.0617(11) Uani 1 1 d . . . . .
H11 H 0.5940 0.5251 -0.1514 0.074 Uiso 1 1 calc R U . . .
C105 C 0.57702(16) 0.56959(9) -0.06776(16) 0.0644(10) Uani 1 1 d . . . . .
H79 H 0.5460 0.5652 -0.0954 0.097 Uiso 1 1 calc R U . . .
H80 H 0.5811 0.5947 -0.0618 0.097 Uiso 1 1 calc R U . . .
H81 H 0.5684 0.5583 -0.0313 0.097 Uiso 1 1 calc R U . . .
C106 C 0.65564(15) 0.88695(9) -0.05649(16) 0.0614(10) Uani 1 1 d . . . . .
H97 H 0.6928 0.8976 -0.0483 0.092 Uiso 1 1 calc R U . . .
H98 H 0.6610 0.8639 -0.0735 0.092 Uiso 1 1 calc R U . . .
H99 H 0.6347 0.8846 -0.0208 0.092 Uiso 1 1 calc R U . . .
C107 C 0.6784(2) 0.51867(8) -0.15936(15) 0.0694(13) Uani 1 1 d . . . . .
C108 C 0.54658(16) 0.63850(9) 0.05225(17) 0.0639(11) Uani 1 1 d . . . . .
H64 H 0.5824 0.6500 0.0518 0.077 Uiso 1 1 calc R U . . .
C109 C 0.69391(19) 0.63820(8) 0.29269(14) 0.0629(11) Uani 1 1 d . . . . .
H12 H 0.6941 0.6495 0.3289 0.075 Uiso 1 1 calc R U . . .
C110 C 0.18406(16) 0.56967(9) 0.17284(15) 0.0621(10) Uani 1 1 d . . . . .
H100 H 0.1677 0.5931 0.1730 0.093 Uiso 1 1 calc R U . . .
H101 H 0.2256 0.5712 0.1756 0.093 Uiso 1 1 calc R U . . .
H102 H 0.1699 0.5565 0.2055 0.093 Uiso 1 1 calc R U . . .
C111 C 0.13109(19) 0.51663(9) 0.0212(2) 0.0794(15) Uani 1 1 d . . . . .
H68 H 0.1188 0.5044 -0.0122 0.095 Uiso 1 1 calc R U . . .
C112 C 0.80914(18) 0.88780(10) 0.40930(14) 0.0706(12) Uani 1 1 d . . . . .
H51 H 0.8051 0.8981 0.4474 0.106 Uiso 1 1 calc R U . . .
H52 H 0.7720 0.8875 0.3894 0.106 Uiso 1 1 calc R U . . .
H53 H 0.8235 0.8639 0.4131 0.106 Uiso 1 1 calc R U . . .
C113 C 0.12531(17) 0.52632(9) 0.1199(2) 0.0728(12) Uani 1 1 d . . . . .
H69 H 0.1091 0.5209 0.1558 0.087 Uiso 1 1 calc R U . . .
C114 C 0.2009(2) 0.55078(10) -0.04023(18) 0.0848(14) Uani 1 1 d . . . . .
H85 H 0.1962 0.5757 -0.0484 0.127 Uiso 1 1 calc R U . . .
H86 H 0.1821 0.5371 -0.0706 0.127 Uiso 1 1 calc R U . . .
H87 H 0.2415 0.5450 -0.0386 0.127 Uiso 1 1 calc R U . . .
C115 C 0.1065(2) 0.50909(10) 0.0731(3) 0.0869(15) Uani 1 1 d . . . . .
C116 C 0.94564(18) 0.98868(9) 0.3980(2) 0.0841(14) Uani 1 1 d . . . . .
H54 H 0.9308 0.9917 0.4366 0.126 Uiso 1 1 calc R U . . .
H55 H 0.9869 0.9849 0.4004 0.126 Uiso 1 1 calc R U . . .
H56 H 0.9375 1.0096 0.3751 0.126 Uiso 1 1 calc R U . . .
C117 C 0.6757(3) 0.49439(9) -0.21059(17) 0.110(2) Uani 1 1 d . . . . .
H91 H 0.6576 0.4724 -0.1996 0.165 Uiso 1 1 calc R U . . .
H92 H 0.7143 0.4897 -0.2237 0.165 Uiso 1 1 calc R U . . .
H93 H 0.6534 0.5053 -0.2416 0.165 Uiso 1 1 calc R U . . .
C118 C 0.6464(2) 0.99164(10) -0.18707(17) 0.0992(18) Uani 1 1 d . . . . .
H103 H 0.6864 0.9926 -0.1746 0.149 Uiso 1 1 calc R U . . .
H104 H 0.6268 1.0128 -0.1746 0.149 Uiso 1 1 calc R U . . .
H105 H 0.6442 0.9900 -0.2289 0.149 Uiso 1 1 calc R U . . .
C119 C 0.0585(2) 0.48162(12) 0.0738(3) 0.141(3) Uani 1 1 d . . . . .
H88 H 0.0597 0.4692 0.1105 0.211 Uiso 1 1 calc R U . . .
H89 H 0.0638 0.4650 0.0426 0.211 Uiso 1 1 calc R U . . .
H90 H 0.0216 0.4932 0.0689 0.211 Uiso 1 1 calc R U . . .
C120 C 0.93028(14) 0.94704(8) 0.31510(16) 0.0512(9) Uani 1 1 d . . . . .
H34 H 0.9577 0.9599 0.2945 0.061 Uiso 1 1 calc R U . . .
O14 O 0.67188(13) 0.73038(5) 0.17346(10) 0.0688(8) Uani 1 1 d . . . . .
O13 O 0.42328(11) 0.73087(5) 0.07431(13) 0.0711(8) 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
O1 C14 1.367(3) . ?
O2 C16 1.355(3) . ?
O3 C24 1.369(3) . ?
O4 C52 1.393(3) . ?
O4 C27 1.401(4) . ?
O5 C19 1.371(3) . ?
O6 C54 1.395(3) . ?
O6 C26 1.402(3) . ?
O7 C60 1.349(4) . ?
O8 C51 1.354(3) . ?
N1 C1 1.365(3) . ?
N1 C7 1.380(3) . ?
N2 C2 1.368(3) . ?
N2 C3 1.384(3) . ?
O9 C70 1.354(4) . ?
O10 C69 1.357(3) . ?
N3 C21 1.355(3) . ?
N3 C22 1.394(3) . ?
N4 C4 1.333(3) . ?
N4 C5 1.411(3) . ?
N5 C15 1.338(3) . ?
N5 C18 1.392(3) . ?
N6 C20 1.353(3) . ?
N6 C12 1.401(3) . ?
N7 C9 1.348(4) . ?
N7 C10 1.398(3) . ?
N8 C43 1.340(4) . ?
N8 C17 1.405(3) . ?
O11 C80 1.396(4) . ?
O11 C84 1.402(3) . ?
O12 C76 1.392(4) . ?
O12 C93 1.396(3) . ?
C1 C6 1.388(4) . ?
C1 C13 1.472(4) . ?
C2 C8 1.385(4) . ?
C2 C30 1.462(4) . ?
C3 C28 1.391(4) . ?
C3 C25 1.422(4) . ?
C4 C58 1.444(4) . ?
C4 C42 1.454(4) . ?
C5 C11 1.371(4) . ?
C5 C44 1.446(4) . ?
C6 C32 1.391(4) . ?
C7 C32 1.400(4) . ?
C7 C11 1.428(4) . ?
C8 C28 1.390(4) . ?
C9 C53 1.438(4) . ?
C9 C48 1.450(4) . ?
C10 C33 1.390(4) . ?
C10 C47 1.431(4) . ?
C11 C41 1.502(4) . ?
C12 C39 1.394(4) . ?
C12 C36 1.410(4) . ?
C13 C40 1.396(4) . ?
C13 C14 1.409(4) . ?
C14 C52 1.389(4) . ?
C15 C46 1.430(4) . ?
C15 C35 1.460(4) . ?
C16 C54 1.398(4) . ?
C16 C30 1.400(4) . ?
C17 C25 1.369(4) . ?
C17 C63 1.442(4) . ?
C18 C39 1.391(4) . ?
C18 C38 1.431(4) . ?
C19 C23 1.395(4) . ?
C19 C27 1.398(4) . ?
C20 C37 1.405(4) . ?
C20 C31 1.456(4) . ?
C21 C49 1.402(4) . ?
C21 C23 1.452(4) . ?
C22 C33 1.406(4) . ?
C22 C61 1.413(4) . ?
C23 C55 1.408(4) . ?
C24 C26 1.391(4) . ?
C24 C31 1.406(4) . ?
C25 C29 1.509(4) . ?
C26 C65 1.379(4) . ?
C27 C50 1.373(4) . ?
C29 C64 1.393(4) . ?
C29 C79 1.398(4) . ?
C30 C67 1.405(4) . ?
C31 C34 1.403(4) . ?
C33 C71 1.514(4) . ?
C34 C56 1.369(4) . ?
C35 C69 1.397(4) . ?
C35 C82 1.401(4) . ?
C36 C37 1.372(4) . ?
C38 C46 1.362(4) . ?
C39 C59 1.512(4) . ?
C40 C78 1.374(4) . ?
C41 C66 1.398(4) . ?
C41 C83 1.399(4) . ?
C42 C51 1.405(4) . ?
C42 C62 1.409(4) . ?
C43 C68 1.442(4) . ?
C43 C45 1.459(4) . ?
C44 C58 1.343(4) . ?
C45 C70 1.391(4) . ?
C45 C73 1.412(4) . ?
C47 C53 1.355(4) . ?
C48 C60 1.405(4) . ?
C48 C75 1.405(4) . ?
C49 C61 1.376(4) . ?
C50 C57 1.375(4) . ?
C51 C80 1.398(4) . ?
C52 C90 1.387(4) . ?
C54 C87 1.363(4) . ?
C55 C57 1.374(4) . ?
C56 C65 1.377(4) . ?
C59 C74 1.396(4) . ?
C59 C77 1.398(5) . ?
C60 C84 1.393(4) . ?
C62 C72 1.376(4) . ?
C63 C68 1.334(4) . ?
C64 C120 1.399(4) . ?
C64 C91 1.512(4) . ?
C66 C94 1.400(4) . ?
C66 C99 1.505(5) . ?
C67 C86 1.375(4) . ?
C69 C93 1.391(4) . ?
C70 C76 1.390(4) . ?
C71 C97 1.395(4) . ?
C71 C89 1.395(5) . ?
C72 C81 1.400(4) . ?
C73 C88 1.375(4) . ?
C74 C95 1.418(5) . ?
C74 C101 1.478(5) . ?
C75 C102 1.368(5) . ?
C76 C85 1.383(5) . ?
C77 C104 1.384(4) . ?
C77 C105 1.508(5) . ?
C78 C90 1.382(4) . ?
C79 C98 1.399(4) . ?
C79 C112 1.512(5) . ?
C80 C81 1.357(4) . ?
C82 C100 1.379(4) . ?
C83 C96 1.403(4) . ?
C83 C106 1.507(5) . ?
C84 C108 1.367(5) . ?
C85 C88 1.383(5) . ?
C86 C87 1.389(4) . ?
C89 C113 1.375(5) . ?
C89 C110 1.510(5) . ?
C92 C120 1.381(5) . ?
C92 C98 1.388(5) . ?
C92 C116 1.511(5) . ?
C93 C109 1.383(5) . ?
C94 C103 1.394(5) . ?
C95 C107 1.376(6) . ?
C96 C103 1.381(5) . ?
C97 C111 1.423(6) . ?
C97 C114 1.513(6) . ?
C100 C109 1.373(4) . ?
C102 C108 1.385(4) . ?
C103 C118 1.519(4) . ?
C104 C107 1.370(6) . ?
C107 C117 1.517(5) . ?
C111 C115 1.384(7) . ?
C113 C115 1.347(6) . ?
C115 C119 1.544(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C52 O4 C27 117.8(2) . . ?
C54 O6 C26 117.5(2) . . ?
C1 N1 C7 110.6(2) . . ?
C2 N2 C3 110.3(2) . . ?
C21 N3 C22 110.0(2) . . ?
C4 N4 C5 105.9(2) . . ?
C15 N5 C18 106.5(2) . . ?
C20 N6 C12 110.1(2) . . ?
C9 N7 C10 106.6(2) . . ?
C43 N8 C17 105.6(2) . . ?
C80 O11 C84 119.0(2) . . ?
C76 O12 C93 119.5(3) . . ?
N1 C1 C6 107.2(2) . . ?
N1 C1 C13 124.4(2) . . ?
C6 C1 C13 128.2(2) . . ?
N2 C2 C8 107.2(2) . . ?
N2 C2 C30 124.3(2) . . ?
C8 C2 C30 128.4(3) . . ?
N2 C3 C28 106.1(2) . . ?
N2 C3 C25 125.4(2) . . ?
C28 C3 C25 128.6(3) . . ?
N4 C4 C58 111.5(2) . . ?
N4 C4 C42 123.2(2) . . ?
C58 C4 C42 125.2(2) . . ?
C11 C5 N4 126.5(2) . . ?
C11 C5 C44 125.0(2) . . ?
N4 C5 C44 108.5(2) . . ?
C1 C6 C32 107.8(2) . . ?
N1 C7 C32 105.9(2) . . ?
N1 C7 C11 126.0(2) . . ?
C32 C7 C11 128.0(2) . . ?
C2 C8 C28 107.9(3) . . ?
N7 C9 C53 110.3(3) . . ?
N7 C9 C48 122.5(2) . . ?
C53 C9 C48 127.2(3) . . ?
C33 C10 N7 125.2(2) . . ?
C33 C10 C47 126.1(3) . . ?
N7 C10 C47 108.7(3) . . ?
C5 C11 C7 126.9(2) . . ?
C5 C11 C41 118.0(2) . . ?
C7 C11 C41 115.1(2) . . ?
C39 C12 N6 126.6(2) . . ?
C39 C12 C36 127.8(2) . . ?
N6 C12 C36 105.5(2) . . ?
C40 C13 C14 117.6(2) . . ?
C40 C13 C1 118.9(2) . . ?
C14 C13 C1 123.4(2) . . ?
O1 C14 C52 121.3(2) . . ?
O1 C14 C13 119.3(2) . . ?
C52 C14 C13 119.4(2) . . ?
N5 C15 C46 110.8(2) . . ?
N5 C15 C35 121.6(2) . . ?
C46 C15 C35 127.6(2) . . ?
O2 C16 C54 121.1(2) . . ?
O2 C16 C30 119.6(2) . . ?
C54 C16 C30 119.3(3) . . ?
C25 C17 N8 126.0(3) . . ?
C25 C17 C63 125.4(3) . . ?
N8 C17 C63 108.6(2) . . ?
C39 C18 N5 124.2(2) . . ?
C39 C18 C38 126.8(2) . . ?
N5 C18 C38 109.1(2) . . ?
O5 C19 C23 119.3(2) . . ?
O5 C19 C27 121.0(3) . . ?
C23 C19 C27 119.7(3) . . ?
N6 C20 C37 107.7(2) . . ?
N6 C20 C31 125.3(2) . . ?
C37 C20 C31 127.0(2) . . ?
N3 C21 C49 107.6(2) . . ?
N3 C21 C23 125.4(3) . . ?
C49 C21 C23 127.0(3) . . ?
N3 C22 C33 126.6(3) . . ?
N3 C22 C61 106.2(2) . . ?
C33 C22 C61 127.2(3) . . ?
C19 C23 C55 118.0(2) . . ?
C19 C23 C21 123.1(3) . . ?
C55 C23 C21 118.8(3) . . ?
O3 C24 C26 121.6(2) . . ?
O3 C24 C31 119.0(2) . . ?
C26 C24 C31 119.4(2) . . ?
C17 C25 C3 127.5(3) . . ?
C17 C25 C29 117.5(3) . . ?
C3 C25 C29 115.0(2) . . ?
C65 C26 C24 121.3(3) . . ?
C65 C26 O6 125.0(2) . . ?
C24 C26 O6 113.6(2) . . ?
C50 C27 C19 121.0(3) . . ?
C50 C27 O4 125.6(2) . . ?
C19 C27 O4 113.3(3) . . ?
C8 C28 C3 108.6(2) . . ?
C64 C29 C79 120.8(3) . . ?
C64 C29 C25 120.2(2) . . ?
C79 C29 C25 118.9(3) . . ?
C16 C30 C67 117.7(3) . . ?
C16 C30 C2 123.4(3) . . ?
C67 C30 C2 118.7(2) . . ?
C34 C31 C24 118.1(2) . . ?
C34 C31 C20 119.1(2) . . ?
C24 C31 C20 122.8(2) . . ?
C6 C32 C7 108.4(2) . . ?
C10 C33 C22 126.4(3) . . ?
C10 C33 C71 119.3(2) . . ?
C22 C33 C71 114.3(3) . . ?
C56 C34 C31 121.1(3) . . ?
C69 C35 C82 118.2(3) . . ?
C69 C35 C15 120.8(2) . . ?
C82 C35 C15 121.0(3) . . ?
C37 C36 C12 108.8(2) . . ?
C36 C37 C20 107.9(2) . . ?
C46 C38 C18 106.8(2) . . ?
C18 C39 C12 126.8(2) . . ?
C18 C39 C59 119.5(2) . . ?
C12 C39 C59 113.7(2) . . ?
C78 C40 C13 122.2(3) . . ?
C66 C41 C83 120.8(3) . . ?
C66 C41 C11 120.5(3) . . ?
C83 C41 C11 118.7(3) . . ?
C51 C42 C62 118.6(3) . . ?
C51 C42 C4 120.5(2) . . ?
C62 C42 C4 120.9(3) . . ?
N8 C43 C68 111.3(2) . . ?
N8 C43 C45 122.5(3) . . ?
C68 C43 C45 126.2(3) . . ?
C58 C44 C5 107.4(2) . . ?
C70 C45 C73 118.7(3) . . ?
C70 C45 C43 120.7(3) . . ?
C73 C45 C43 120.6(3) . . ?
C38 C46 C15 106.8(2) . . ?
C53 C47 C10 107.5(3) . . ?
C60 C48 C75 117.6(3) . . ?
C60 C48 C9 120.9(3) . . ?
C75 C48 C9 121.4(2) . . ?
C61 C49 C21 108.3(3) . . ?
C27 C50 C57 119.6(3) . . ?
O8 C51 C80 118.3(3) . . ?
O8 C51 C42 122.4(2) . . ?
C80 C51 C42 119.4(3) . . ?
C90 C52 C14 121.6(3) . . ?
C90 C52 O4 121.5(2) . . ?
C14 C52 O4 116.9(2) . . ?
C47 C53 C9 106.8(3) . . ?
C87 C54 O6 121.8(3) . . ?
C87 C54 C16 121.6(3) . . ?
O6 C54 C16 116.6(3) . . ?
C57 C55 C23 121.1(3) . . ?
C34 C56 C65 120.9(3) . . ?
C55 C57 C50 120.5(3) . . ?
C44 C58 C4 106.7(2) . . ?
C74 C59 C77 120.4(3) . . ?
C74 C59 C39 119.5(3) . . ?
C77 C59 C39 119.8(3) . . ?
O7 C60 C84 118.8(3) . . ?
O7 C60 C48 122.3(3) . . ?
C84 C60 C48 119.0(3) . . ?
C49 C61 C22 107.9(3) . . ?
C72 C62 C42 120.4(3) . . ?
C68 C63 C17 107.8(3) . . ?
C29 C64 C120 118.2(3) . . ?
C29 C64 C91 120.2(3) . . ?
C120 C64 C91 121.4(3) . . ?
C56 C65 C26 119.1(3) . . ?
C41 C66 C94 118.3(3) . . ?
C41 C66 C99 120.7(3) . . ?
C94 C66 C99 120.9(3) . . ?
C86 C67 C30 122.0(3) . . ?
C63 C68 C43 106.7(3) . . ?
O10 C69 C93 118.3(3) . . ?
O10 C69 C35 122.5(3) . . ?
C93 C69 C35 119.2(3) . . ?
O9 C70 C76 117.3(3) . . ?
O9 C70 C45 122.7(2) . . ?
C76 C70 C45 120.0(3) . . ?
C97 C71 C89 118.8(3) . . ?
C97 C71 C33 120.7(3) . . ?
C89 C71 C33 120.4(3) . . ?
C62 C72 C81 120.5(3) . . ?
C88 C73 C45 120.3(3) . . ?
C59 C74 C95 117.6(4) . . ?
C59 C74 C101 121.4(3) . . ?
C95 C74 C101 121.0(3) . . ?
C102 C75 C48 122.2(3) . . ?
C85 C76 C70 120.7(3) . . ?
C85 C76 O12 125.0(3) . . ?
C70 C76 O12 114.3(3) . . ?
C104 C77 C59 119.3(3) . . ?
C104 C77 C105 119.6(3) . . ?
C59 C77 C105 121.2(3) . . ?
C40 C78 C90 120.0(3) . . ?
C29 C79 C98 118.6(3) . . ?
C29 C79 C112 120.5(3) . . ?
C98 C79 C112 120.9(3) . . ?
C81 C80 O11 124.4(3) . . ?
C81 C80 C51 121.7(3) . . ?
O11 C80 C51 113.9(3) . . ?
C80 C81 C72 119.4(3) . . ?
C100 C82 C35 121.9(3) . . ?
C41 C83 C96 118.9(3) . . ?
C41 C83 C106 120.5(3) . . ?
C96 C83 C106 120.5(3) . . ?
C108 C84 C60 122.2(3) . . ?
C108 C84 O11 120.2(3) . . ?
C60 C84 O11 117.3(3) . . ?
C88 C85 C76 119.6(3) . . ?
C67 C86 C87 119.2(3) . . ?
C54 C87 C86 119.9(3) . . ?
C73 C88 C85 120.6(3) . . ?
C113 C89 C71 120.5(4) . . ?
C113 C89 C110 118.3(3) . . ?
C71 C89 C110 121.2(3) . . ?
C78 C90 C52 118.9(3) . . ?
C120 C92 C98 117.9(3) . . ?
C120 C92 C116 122.1(4) . . ?
C98 C92 C116 120.0(3) . . ?
C109 C93 C69 121.5(3) . . ?
C109 C93 O12 120.2(3) . . ?
C69 C93 O12 118.0(3) . . ?
C103 C94 C66 122.0(3) . . ?
C107 C95 C74 122.1(4) . . ?
C103 C96 C83 121.5(4) . . ?
C71 C97 C111 118.4(4) . . ?
C71 C97 C114 120.2(3) . . ?
C111 C97 C114 121.3(4) . . ?
C92 C98 C79 121.8(3) . . ?
C109 C100 C82 119.5(3) . . ?
C75 C102 C108 119.7(3) . . ?
C96 C103 C94 118.4(3) . . ?
C96 C103 C118 120.8(4) . . ?
C94 C103 C118 120.7(4) . . ?
C107 C104 C77 122.1(4) . . ?
C104 C107 C95 118.4(3) . . ?
C104 C107 C117 121.4(5) . . ?
C95 C107 C117 120.2(5) . . ?
C84 C108 C102 119.3(3) . . ?
C100 C109 C93 119.7(3) . . ?
C115 C111 C97 121.4(4) . . ?
C115 C113 C89 122.6(5) . . ?
C113 C115 C111 118.3(4) . . ?
C113 C115 C119 123.7(6) . . ?
C111 C115 C119 118.1(5) . . ?
C92 C120 C64 122.5(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N1 C1 C6 -0.2(3) . . . . ?
C7 N1 C1 C13 175.5(2) . . . . ?
C3 N2 C2 C8 -1.3(3) . . . . ?
C3 N2 C2 C30 175.7(2) . . . . ?
C2 N2 C3 C28 1.1(3) . . . . ?
C2 N2 C3 C25 -177.6(2) . . . . ?
C5 N4 C4 C58 -1.3(3) . . . . ?
C5 N4 C4 C42 176.4(3) . . . . ?
C4 N4 C5 C11 -178.6(3) . . . . ?
C4 N4 C5 C44 0.9(3) . . . . ?
N1 C1 C6 C32 0.0(3) . . . . ?
C13 C1 C6 C32 -175.5(3) . . . . ?
C1 N1 C7 C32 0.3(3) . . . . ?
C1 N1 C7 C11 -178.5(3) . . . . ?
N2 C2 C8 C28 1.0(3) . . . . ?
C30 C2 C8 C28 -175.9(3) . . . . ?
C10 N7 C9 C53 0.1(3) . . . . ?
C10 N7 C9 C48 178.9(2) . . . . ?
C9 N7 C10 C33 177.2(2) . . . . ?
C9 N7 C10 C47 -0.8(3) . . . . ?
N4 C5 C11 C7 -5.3(5) . . . . ?
C44 C5 C11 C7 175.3(3) . . . . ?
N4 C5 C11 C41 173.0(3) . . . . ?
C44 C5 C11 C41 -6.5(4) . . . . ?
N1 C7 C11 C5 -1.1(4) . . . . ?
C32 C7 C11 C5 -179.6(3) . . . . ?
N1 C7 C11 C41 -179.4(3) . . . . ?
C32 C7 C11 C41 2.1(4) . . . . ?
C20 N6 C12 C39 -177.9(3) . . . . ?
C20 N6 C12 C36 0.6(3) . . . . ?
N1 C1 C13 C40 179.2(3) . . . . ?
C6 C1 C13 C40 -6.1(4) . . . . ?
N1 C1 C13 C14 -4.2(4) . . . . ?
C6 C1 C13 C14 170.5(3) . . . . ?
C40 C13 C14 O1 -176.1(3) . . . . ?
C1 C13 C14 O1 7.3(4) . . . . ?
C40 C13 C14 C52 4.8(4) . . . . ?
C1 C13 C14 C52 -171.7(3) . . . . ?
C18 N5 C15 C46 0.4(3) . . . . ?
C18 N5 C15 C35 -179.6(3) . . . . ?
C43 N8 C17 C25 -179.4(3) . . . . ?
C43 N8 C17 C63 1.2(3) . . . . ?
C15 N5 C18 C39 177.1(3) . . . . ?
C15 N5 C18 C38 -1.0(3) . . . . ?
C12 N6 C20 C37 -0.8(3) . . . . ?
C12 N6 C20 C31 177.0(3) . . . . ?
C22 N3 C21 C49 -0.1(3) . . . . ?
C22 N3 C21 C23 178.9(2) . . . . ?
C21 N3 C22 C33 -178.3(2) . . . . ?
C21 N3 C22 C61 0.1(3) . . . . ?
O5 C19 C23 C55 -178.1(2) . . . . ?
C27 C19 C23 C55 2.6(4) . . . . ?
O5 C19 C23 C21 2.2(4) . . . . ?
C27 C19 C23 C21 -177.1(2) . . . . ?
N3 C21 C23 C19 -13.6(4) . . . . ?
C49 C21 C23 C19 165.3(3) . . . . ?
N3 C21 C23 C55 166.7(2) . . . . ?
C49 C21 C23 C55 -14.4(4) . . . . ?
N8 C17 C25 C3 -3.3(4) . . . . ?
C63 C17 C25 C3 176.0(3) . . . . ?
N8 C17 C25 C29 175.3(2) . . . . ?
C63 C17 C25 C29 -5.3(4) . . . . ?
N2 C3 C25 C17 -3.7(4) . . . . ?
C28 C3 C25 C17 177.9(3) . . . . ?
N2 C3 C25 C29 177.6(2) . . . . ?
C28 C3 C25 C29 -0.8(4) . . . . ?
O3 C24 C26 C65 176.2(3) . . . . ?
C31 C24 C26 C65 -5.7(4) . . . . ?
O3 C24 C26 O6 -1.9(4) . . . . ?
C31 C24 C26 O6 176.1(2) . . . . ?
C54 O6 C26 C65 -0.8(4) . . . . ?
C54 O6 C26 C24 177.2(3) . . . . ?
O5 C19 C27 C50 176.2(2) . . . . ?
C23 C19 C27 C50 -4.5(4) . . . . ?
O5 C19 C27 O4 -2.2(3) . . . . ?
C23 C19 C27 O4 177.0(2) . . . . ?
C52 O4 C27 C50 2.1(4) . . . . ?
C52 O4 C27 C19 -179.5(2) . . . . ?
C2 C8 C28 C3 -0.3(3) . . . . ?
N2 C3 C28 C8 -0.5(3) . . . . ?
C25 C3 C28 C8 178.2(3) . . . . ?
C17 C25 C29 C64 93.8(3) . . . . ?
C3 C25 C29 C64 -87.4(3) . . . . ?
C17 C25 C29 C79 -86.4(3) . . . . ?
C3 C25 C29 C79 92.4(3) . . . . ?
O2 C16 C30 C67 -176.5(2) . . . . ?
C54 C16 C30 C67 4.9(4) . . . . ?
O2 C16 C30 C2 7.7(4) . . . . ?
C54 C16 C30 C2 -171.0(3) . . . . ?
N2 C2 C30 C16 -3.8(4) . . . . ?
C8 C2 C30 C16 172.5(3) . . . . ?
N2 C2 C30 C67 -179.6(2) . . . . ?
C8 C2 C30 C67 -3.3(4) . . . . ?
O3 C24 C31 C34 -177.9(3) . . . . ?
C26 C24 C31 C34 4.0(4) . . . . ?
O3 C24 C31 C20 2.8(4) . . . . ?
C26 C24 C31 C20 -175.4(3) . . . . ?
N6 C20 C31 C34 167.6(3) . . . . ?
C37 C20 C31 C34 -15.0(4) . . . . ?
N6 C20 C31 C24 -13.0(4) . . . . ?
C37 C20 C31 C24 164.4(3) . . . . ?
C1 C6 C32 C7 0.2(3) . . . . ?
N1 C7 C32 C6 -0.3(3) . . . . ?
C11 C7 C32 C6 178.4(3) . . . . ?
N7 C10 C33 C22 -2.7(4) . . . . ?
C47 C10 C33 C22 174.9(3) . . . . ?
N7 C10 C33 C71 178.5(2) . . . . ?
C47 C10 C33 C71 -3.8(4) . . . . ?
N3 C22 C33 C10 -4.4(4) . . . . ?
C61 C22 C33 C10 177.5(3) . . . . ?
N3 C22 C33 C71 174.3(2) . . . . ?
C61 C22 C33 C71 -3.7(4) . . . . ?
C24 C31 C34 C56 -0.3(4) . . . . ?
C20 C31 C34 C56 179.1(3) . . . . ?
N5 C15 C35 C69 -17.2(5) . . . . ?
C46 C15 C35 C69 162.9(3) . . . . ?
N5 C15 C35 C82 161.5(3) . . . . ?
C46 C15 C35 C82 -18.5(5) . . . . ?
C39 C12 C36 C37 178.4(3) . . . . ?
N6 C12 C36 C37 -0.1(3) . . . . ?
C12 C36 C37 C20 -0.4(3) . . . . ?
N6 C20 C37 C36 0.7(3) . . . . ?
C31 C20 C37 C36 -177.0(3) . . . . ?
C39 C18 C38 C46 -176.8(3) . . . . ?
N5 C18 C38 C46 1.2(3) . . . . ?
N5 C18 C39 C12 -3.4(5) . . . . ?
C38 C18 C39 C12 174.4(3) . . . . ?
N5 C18 C39 C59 177.4(3) . . . . ?
C38 C18 C39 C59 -4.9(5) . . . . ?
N6 C12 C39 C18 -6.0(5) . . . . ?
C36 C12 C39 C18 175.9(3) . . . . ?
N6 C12 C39 C59 173.3(3) . . . . ?
C36 C12 C39 C59 -4.8(4) . . . . ?
C14 C13 C40 C78 -0.3(5) . . . . ?
C1 C13 C40 C78 176.4(3) . . . . ?
C5 C11 C41 C66 99.5(3) . . . . ?
C7 C11 C41 C66 -82.0(3) . . . . ?
C5 C11 C41 C83 -81.9(3) . . . . ?
C7 C11 C41 C83 96.5(3) . . . . ?
N4 C4 C42 C51 -9.3(4) . . . . ?
C58 C4 C42 C51 168.0(3) . . . . ?
N4 C4 C42 C62 172.0(3) . . . . ?
C58 C4 C42 C62 -10.7(4) . . . . ?
C17 N8 C43 C68 -1.8(3) . . . . ?
C17 N8 C43 C45 176.1(2) . . . . ?
C11 C5 C44 C58 179.3(3) . . . . ?
N4 C5 C44 C58 -0.2(3) . . . . ?
N8 C43 C45 C70 -8.9(4) . . . . ?
C68 C43 C45 C70 168.6(3) . . . . ?
N8 C43 C45 C73 173.2(2) . . . . ?
C68 C43 C45 C73 -9.2(4) . . . . ?
C18 C38 C46 C15 -1.0(3) . . . . ?
N5 C15 C46 C38 0.4(3) . . . . ?
C35 C15 C46 C38 -179.6(3) . . . . ?
C33 C10 C47 C53 -176.7(3) . . . . ?
N7 C10 C47 C53 1.3(3) . . . . ?
N7 C9 C48 C60 -15.5(4) . . . . ?
C53 C9 C48 C60 163.2(3) . . . . ?
N7 C9 C48 C75 163.8(3) . . . . ?
C53 C9 C48 C75 -17.6(4) . . . . ?
N3 C21 C49 C61 0.1(3) . . . . ?
C23 C21 C49 C61 -178.9(2) . . . . ?
C19 C27 C50 C57 3.2(4) . . . . ?
O4 C27 C50 C57 -178.5(2) . . . . ?
C62 C42 C51 O8 -179.3(3) . . . . ?
C4 C42 C51 O8 1.9(4) . . . . ?
C62 C42 C51 C80 -0.4(4) . . . . ?
C4 C42 C51 C80 -179.2(3) . . . . ?
O1 C14 C52 C90 174.8(3) . . . . ?
C13 C14 C52 C90 -6.2(5) . . . . ?
O1 C14 C52 O4 -2.7(4) . . . . ?
C13 C14 C52 O4 176.4(3) . . . . ?
C27 O4 C52 C90 64.3(4) . . . . ?
C27 O4 C52 C14 -118.2(3) . . . . ?
C10 C47 C53 C9 -1.2(3) . . . . ?
N7 C9 C53 C47 0.7(3) . . . . ?
C48 C9 C53 C47 -178.0(3) . . . . ?
C26 O6 C54 C87 70.6(4) . . . . ?
C26 O6 C54 C16 -112.3(3) . . . . ?
O2 C16 C54 C87 175.0(3) . . . . ?
C30 C16 C54 C87 -6.4(5) . . . . ?
O2 C16 C54 O6 -2.1(4) . . . . ?
C30 C16 C54 O6 176.5(2) . . . . ?
C19 C23 C55 C57 0.5(4) . . . . ?
C21 C23 C55 C57 -179.7(2) . . . . ?
C31 C34 C56 C65 -2.0(4) . . . . ?
C23 C55 C57 C50 -1.9(4) . . . . ?
C27 C50 C57 C55 0.0(4) . . . . ?
C5 C44 C58 C4 -0.5(3) . . . . ?
N4 C4 C58 C44 1.1(3) . . . . ?
C42 C4 C58 C44 -176.4(3) . . . . ?
C18 C39 C59 C74 -91.2(3) . . . . ?
C12 C39 C59 C74 89.5(3) . . . . ?
C18 C39 C59 C77 94.5(3) . . . . ?
C12 C39 C59 C77 -84.9(3) . . . . ?
C75 C48 C60 O7 -179.9(3) . . . . ?
C9 C48 C60 O7 -0.6(4) . . . . ?
C75 C48 C60 C84 0.4(4) . . . . ?
C9 C48 C60 C84 179.8(3) . . . . ?
C21 C49 C61 C22 0.0(3) . . . . ?
N3 C22 C61 C49 -0.1(3) . . . . ?
C33 C22 C61 C49 178.3(3) . . . . ?
C51 C42 C62 C72 1.0(4) . . . . ?
C4 C42 C62 C72 179.7(3) . . . . ?
C25 C17 C63 C68 -179.6(3) . . . . ?
N8 C17 C63 C68 -0.1(3) . . . . ?
C79 C29 C64 C120 -2.4(4) . . . . ?
C25 C29 C64 C120 177.5(3) . . . . ?
C79 C29 C64 C91 174.6(3) . . . . ?
C25 C29 C64 C91 -5.6(4) . . . . ?
C34 C56 C65 C26 0.4(4) . . . . ?
C24 C26 C65 C56 3.5(4) . . . . ?
O6 C26 C65 C56 -178.6(3) . . . . ?
C83 C41 C66 C94 -1.2(4) . . . . ?
C11 C41 C66 C94 177.3(3) . . . . ?
C83 C41 C66 C99 174.9(3) . . . . ?
C11 C41 C66 C99 -6.6(4) . . . . ?
C16 C30 C67 C86 -0.5(4) . . . . ?
C2 C30 C67 C86 175.6(3) . . . . ?
C17 C63 C68 C43 -0.9(3) . . . . ?
N8 C43 C68 C63 1.7(3) . . . . ?
C45 C43 C68 C63 -176.0(3) . . . . ?
C82 C35 C69 O10 -178.6(3) . . . . ?
C15 C35 C69 O10 0.1(5) . . . . ?
C82 C35 C69 C93 0.5(5) . . . . ?
C15 C35 C69 C93 179.2(3) . . . . ?
C73 C45 C70 O9 179.8(2) . . . . ?
C43 C45 C70 O9 1.9(4) . . . . ?
C73 C45 C70 C76 0.4(4) . . . . ?
C43 C45 C70 C76 -177.5(3) . . . . ?
C10 C33 C71 C97 -82.4(4) . . . . ?
C22 C33 C71 C97 98.7(3) . . . . ?
C10 C33 C71 C89 101.2(3) . . . . ?
C22 C33 C71 C89 -77.7(3) . . . . ?
C42 C62 C72 C81 -1.1(5) . . . . ?
C70 C45 C73 C88 1.0(4) . . . . ?
C43 C45 C73 C88 178.9(3) . . . . ?
C77 C59 C74 C95 2.4(4) . . . . ?
C39 C59 C74 C95 -171.9(2) . . . . ?
C77 C59 C74 C101 -179.8(3) . . . . ?
C39 C59 C74 C101 6.0(4) . . . . ?
C60 C48 C75 C102 0.9(5) . . . . ?
C9 C48 C75 C102 -178.4(3) . . . . ?
O9 C70 C76 C85 178.9(3) . . . . ?
C45 C70 C76 C85 -1.7(4) . . . . ?
O9 C70 C76 O12 -0.6(4) . . . . ?
C45 C70 C76 O12 178.8(3) . . . . ?
C93 O12 C76 C85 3.2(5) . . . . ?
C93 O12 C76 C70 -177.3(3) . . . . ?
C74 C59 C77 C104 -1.4(4) . . . . ?
C39 C59 C77 C104 172.9(3) . . . . ?
C74 C59 C77 C105 179.6(3) . . . . ?
C39 C59 C77 C105 -6.1(4) . . . . ?
C13 C40 C78 C90 -3.1(5) . . . . ?
C64 C29 C79 C98 2.4(5) . . . . ?
C25 C29 C79 C98 -177.5(3) . . . . ?
C64 C29 C79 C112 -176.1(3) . . . . ?
C25 C29 C79 C112 4.1(5) . . . . ?
C84 O11 C80 C81 3.6(5) . . . . ?
C84 O11 C80 C51 -175.7(3) . . . . ?
O8 C51 C80 C81 179.0(3) . . . . ?
C42 C51 C80 C81 0.0(5) . . . . ?
O8 C51 C80 O11 -1.7(4) . . . . ?
C42 C51 C80 O11 179.3(3) . . . . ?
O11 C80 C81 C72 -179.4(3) . . . . ?
C51 C80 C81 C72 -0.2(5) . . . . ?
C62 C72 C81 C80 0.7(5) . . . . ?
C69 C35 C82 C100 0.4(5) . . . . ?
C15 C35 C82 C100 -178.3(3) . . . . ?
C66 C41 C83 C96 1.4(4) . . . . ?
C11 C41 C83 C96 -177.2(3) . . . . ?
C66 C41 C83 C106 -177.8(3) . . . . ?
C11 C41 C83 C106 3.7(4) . . . . ?
O7 C60 C84 C108 177.8(3) . . . . ?
C48 C60 C84 C108 -2.6(5) . . . . ?
O7 C60 C84 O11 3.9(4) . . . . ?
C48 C60 C84 O11 -176.4(3) . . . . ?
C80 O11 C84 C108 78.7(4) . . . . ?
C80 O11 C84 C60 -107.3(3) . . . . ?
C70 C76 C85 C88 1.5(4) . . . . ?
O12 C76 C85 C88 -179.1(3) . . . . ?
C30 C67 C86 C87 -2.6(5) . . . . ?
O6 C54 C87 C86 -179.8(3) . . . . ?
C16 C54 C87 C86 3.2(5) . . . . ?
C67 C86 C87 C54 1.3(5) . . . . ?
C45 C73 C88 C85 -1.2(4) . . . . ?
C76 C85 C88 C73 0.0(4) . . . . ?
C97 C71 C89 C113 -1.3(5) . . . . ?
C33 C71 C89 C113 175.2(3) . . . . ?
C97 C71 C89 C110 -179.9(3) . . . . ?
C33 C71 C89 C110 -3.4(5) . . . . ?
C40 C78 C90 C52 1.8(5) . . . . ?
C14 C52 C90 C78 2.8(5) . . . . ?
O4 C52 C90 C78 -179.9(3) . . . . ?
O10 C69 C93 C109 177.3(3) . . . . ?
C35 C69 C93 C109 -1.8(5) . . . . ?
O10 C69 C93 O12 4.4(5) . . . . ?
C35 C69 C93 O12 -174.8(3) . . . . ?
C76 O12 C93 C109 84.7(4) . . . . ?
C76 O12 C93 C69 -102.3(4) . . . . ?
C41 C66 C94 C103 -0.4(5) . . . . ?
C99 C66 C94 C103 -176.6(3) . . . . ?
C59 C74 C95 C107 -1.0(4) . . . . ?
C101 C74 C95 C107 -178.9(3) . . . . ?
C41 C83 C96 C103 0.2(5) . . . . ?
C106 C83 C96 C103 179.3(3) . . . . ?
C89 C71 C97 C111 1.2(5) . . . . ?
C33 C71 C97 C111 -175.2(3) . . . . ?
C89 C71 C97 C114 -179.3(3) . . . . ?
C33 C71 C97 C114 4.3(5) . . . . ?
C120 C92 C98 C79 -0.6(5) . . . . ?
C116 C92 C98 C79 180.0(3) . . . . ?
C29 C79 C98 C92 -0.9(5) . . . . ?
C112 C79 C98 C92 177.6(3) . . . . ?
C35 C82 C100 C109 0.1(6) . . . . ?
C48 C75 C102 C108 -0.1(5) . . . . ?
C83 C96 C103 C94 -1.8(5) . . . . ?
C83 C96 C103 C118 179.6(3) . . . . ?
C66 C94 C103 C96 1.9(5) . . . . ?
C66 C94 C103 C118 -179.5(3) . . . . ?
C59 C77 C104 C107 -1.1(5) . . . . ?
C105 C77 C104 C107 177.9(3) . . . . ?
C77 C104 C107 C95 2.4(5) . . . . ?
C77 C104 C107 C117 -177.8(3) . . . . ?
C74 C95 C107 C104 -1.3(5) . . . . ?
C74 C95 C107 C117 178.9(3) . . . . ?
C60 C84 C108 C102 3.3(6) . . . . ?
O11 C84 C108 C102 177.0(3) . . . . ?
C75 C102 C108 C84 -2.0(6) . . . . ?
C82 C100 C109 C93 -1.4(6) . . . . ?
C69 C93 C109 C100 2.3(6) . . . . ?
O12 C93 C109 C100 175.1(4) . . . . ?
C71 C97 C111 C115 0.0(5) . . . . ?
C114 C97 C111 C115 -179.5(4) . . . . ?
C71 C89 C113 C115 0.1(6) . . . . ?
C110 C89 C113 C115 178.7(4) . . . . ?
C89 C113 C115 C111 1.2(6) . . . . ?
C89 C113 C115 C119 -178.1(4) . . . . ?
C97 C111 C115 C113 -1.3(6) . . . . ?
C97 C111 C115 C119 178.2(4) . . . . ?
C98 C92 C120 C64 0.6(5) . . . . ?
C116 C92 C120 C64 -180.0(3) . . . . ?
C29 C64 C120 C92 0.9(5) . . . . ?
C91 C64 C120 C92 -176.0(3) . . . . ?

_refine_diff_density_max         1.610
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.051



# SQUEEZE RESULTS (Version = 301115)
# 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 0.250 0.250 660 167 ' '
2 0.500 0.750 0.250 660 167 ' '
3 0.727 0.476 0.142 12 0 ' '
4 0.227 0.976 0.142 12 0 ' '
5 0.500 0.250 0.250 13 0 ' '
6 1.000 0.750 0.250 13 0 ' '
7 0.500 0.327 0.250 9 0 ' '
8 0.000 0.827 0.250 9 0 ' '
9 0.273 0.476 0.357 12 0 ' '
10 0.773 0.976 0.357 12 0 ' '
11 0.500 0.250 0.750 660 167 ' '
12 0.000 0.750 0.750 660 167 ' '
13 0.227 0.024 0.642 12 0 ' '
14 0.727 0.524 0.642 12 0 ' '
15 0.000 0.250 0.750 13 0 ' '
16 0.500 0.750 0.750 13 0 ' '
17 0.000 0.173 0.750 9 0 ' '
18 0.500 0.673 0.750 9 0 ' '
19 0.773 0.024 0.857 12 0 ' '
20 0.273 0.524 0.857 12 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

####################################################################### 
# 
# 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_1112
_database_code_depnum_ccdc_archive 'CCDC 1446114'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H60 N4 O8'
_chemical_formula_weight         1013.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   13.3625(9)
_cell_length_b                   13.7619(9)
_cell_length_c                   28.7802(18)
_cell_angle_alpha                90
_cell_angle_beta                 90.967(3)
_cell_angle_gamma                90
_cell_volume                     5291.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9866
_cell_measurement_theta_min      2.248
_cell_measurement_theta_max      30.430

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_F_000             2144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    0.084
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2338
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;    
 SADABS-2014/4 - Bruker AXS area detector scaling and absorption correction 
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            66238
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.415
_diffrn_reflns_theta_max         30.544
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16105
_reflns_number_gt                10738
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16105
_refine_ls_number_parameters     701
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1468
_refine_ls_R_factor_gt           0.0969
_refine_ls_wR_factor_ref         0.2529
_refine_ls_wR_factor_gt          0.2289
_refine_ls_goodness_of_fit_ref   1.428
_refine_ls_restrained_S_all      1.428
_refine_ls_shift/su_max          0.004
_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
O1 O 0.89839(13) 0.82077(12) 0.20918(6) 0.0317(4) Uani 1 1 d . . . . .
O2 O 0.87960(13) 0.45703(13) 0.13961(6) 0.0311(4) Uani 1 1 d . . . . .
O3 O 0.99176(12) 0.47645(13) 0.21633(6) 0.0289(4) Uani 1 1 d . . . . .
H60 H 0.9339 0.4928 0.2106 0.043 Uiso 1 1 calc R U . . .
O4 O 1.02058(12) 0.69398(11) 0.24770(5) 0.0221(3) Uani 1 1 d . . . . .
O5 O 1.17607(13) 0.63032(13) 0.17934(6) 0.0337(4) Uani 1 1 d . . . . .
O6 O 0.89337(13) 0.53006(12) 0.30009(5) 0.0288(4) Uani 1 1 d . . . . .
O7 O 0.99008(13) 0.67500(13) 0.15228(5) 0.0297(4) Uani 1 1 d . . . . .
H59 H 1.0173 0.6746 0.1780 0.044 Uiso 1 1 calc R U . . .
O8 O 0.82045(12) 0.57925(11) 0.21718(5) 0.0236(3) Uani 1 1 d . . . . .
N1 N 1.11949(14) 0.62535(12) 0.31981(6) 0.0186(4) Uani 1 1 d . . . . .
N2 N 1.16000(15) 0.44943(13) 0.26274(6) 0.0208(4) Uani 1 1 d . . . . .
H56 H 1.098(3) 0.488(3) 0.2616(15) 0.102(15) Uiso 1 1 d . . . . .
N3 N 0.84420(14) 0.67265(14) 0.08915(6) 0.0233(4) Uani 1 1 d . . . . .
N4 N 0.70045(14) 0.68589(13) 0.16505(6) 0.0223(4) Uani 1 1 d . . . . .
H62 H 0.7598 0.6625 0.1626 0.027 Uiso 1 1 calc R U . . .
C1 C 0.8337(2) 0.88921(19) 0.18694(10) 0.0375(6) Uani 1 1 d . . . . .
H22 H 0.7704 0.8898 0.2022 0.056 Uiso 1 1 calc R U . . .
H21 H 0.8240 0.8713 0.1549 0.056 Uiso 1 1 calc R U . . .
H1 H 0.8632 0.9527 0.1887 0.056 Uiso 1 1 calc R U . . .
C2 C 0.92101(18) 0.83583(17) 0.25507(9) 0.0267(5) Uani 1 1 d . . . . .
C3 C 0.98543(16) 0.76660(15) 0.27503(8) 0.0203(4) Uani 1 1 d . . . . .
C4 C 1.01344(17) 0.77248(16) 0.32187(8) 0.0230(5) Uani 1 1 d . . . . .
C5 C 1.08042(17) 0.70106(16) 0.34336(7) 0.0213(5) Uani 1 1 d . . . . .
C6 C 1.18443(17) 0.57567(15) 0.34962(7) 0.0210(4) Uani 1 1 d . . . . .
C7 C 1.24157(17) 0.49414(16) 0.33805(8) 0.0221(4) Uani 1 1 d . . . . .
C8 C 1.23317(17) 0.43894(16) 0.29752(8) 0.0224(5) Uani 1 1 d . . . . .
C9 C 1.17922(17) 0.38487(16) 0.22870(8) 0.0225(5) Uani 1 1 d . . . . .
C10 C 1.11860(18) 0.37504(15) 0.18642(8) 0.0227(5) Uani 1 1 d . . . . .
C11 C 1.02615(17) 0.42083(15) 0.18105(7) 0.0212(4) Uani 1 1 d . . . . .
C12 C 0.96883(18) 0.40813(16) 0.14039(8) 0.0225(5) Uani 1 1 d . . . . .
C13 C 0.8138(2) 0.44113(19) 0.10111(9) 0.0358(6) Uani 1 1 d . . . . .
H28 H 0.8467 0.4588 0.0729 0.054 Uiso 1 1 calc R U . . .
H3 H 0.7548 0.4801 0.1045 0.054 Uiso 1 1 calc R U . . .
H2 H 0.7954 0.3737 0.0998 0.054 Uiso 1 1 calc R U . . .
C14 C 1.1530(2) 0.31678(19) 0.14966(8) 0.0336(6) Uani 1 1 d . . . . .
H5 H 1.2151 0.2866 0.1523 0.040 Uiso 1 1 calc R U . . .
C15 C 1.0961(2) 0.3042(2) 0.11014(9) 0.0392(7) Uani 1 1 d . . . . .
H6 H 1.1196 0.2650 0.0863 0.047 Uiso 1 1 calc R U . . .
C16 C 1.0035(2) 0.34951(18) 0.10527(8) 0.0319(6) Uani 1 1 d . . . . .
H7 H 0.9650 0.3403 0.0784 0.038 Uiso 1 1 calc R U . . .
C17 C 1.29851(18) 0.36318(17) 0.28361(9) 0.0290(5) Uani 1 1 d . . . . .
H9 H 1.3537 0.3401 0.3003 0.035 Uiso 1 1 calc R U . . .
C18 C 1.26554(19) 0.33042(18) 0.24131(9) 0.0292(5) Uani 1 1 d . . . . .
H8 H 1.2945 0.2813 0.2239 0.035 Uiso 1 1 calc R U . . .
C19 C 1.32285(18) 0.46556(16) 0.37184(8) 0.0255(5) Uani 1 1 d . . . . .
C20 C 1.4173(2) 0.50795(19) 0.36736(10) 0.0348(6) Uani 1 1 d . . . . .
C21 C 1.4911(2) 0.4845(2) 0.40038(11) 0.0452(7) Uani 1 1 d . . . . .
H17 H 1.5537 0.5135 0.3983 0.054 Uiso 1 1 calc R U . . .
C22 C 1.4745(2) 0.4200(2) 0.43596(11) 0.0480(8) Uani 1 1 d . . . . .
C23 C 1.3820(2) 0.3763(2) 0.43842(10) 0.0434(7) Uani 1 1 d . . . . .
H10 H 1.3707 0.3311 0.4618 0.052 Uiso 1 1 calc R U . . .
C24 C 1.3047(2) 0.39802(18) 0.40676(9) 0.0327(6) Uani 1 1 d . . . . .
C25 C 1.2040(2) 0.3491(2) 0.41013(11) 0.0485(8) Uani 1 1 d . . . . .
H11 H 1.1547 0.3959 0.4191 0.073 Uiso 1 1 calc R U . . .
H12 H 1.2077 0.2982 0.4329 0.073 Uiso 1 1 calc R U . . .
H13 H 1.1855 0.3219 0.3805 0.073 Uiso 1 1 calc R U . . .
C26 C 1.5565(3) 0.3956(3) 0.47104(14) 0.0735(13) Uani 1 1 d . . . . .
H14 H 1.5287 0.3594 0.4962 0.110 Uiso 1 1 calc R U . . .
H16 H 1.5858 0.4545 0.4828 0.110 Uiso 1 1 calc R U . . .
H15 H 1.6070 0.3573 0.4563 0.110 Uiso 1 1 calc R U . . .
C27 C 1.4402(2) 0.5735(2) 0.32722(12) 0.0511(8) Uani 1 1 d . . . . .
H20 H 1.5025 0.6064 0.3332 0.077 Uiso 1 1 calc R U . . .
H19 H 1.3876 0.6205 0.3234 0.077 Uiso 1 1 calc R U . . .
H18 H 1.4452 0.5355 0.2994 0.077 Uiso 1 1 calc R U . . .
C28 C 0.8864(2) 0.91231(19) 0.28159(10) 0.0385(6) Uani 1 1 d . . . . .
H25 H 0.8438 0.9586 0.2684 0.046 Uiso 1 1 calc R U . . .
C29 C 0.9155(2) 0.9194(2) 0.32785(10) 0.0429(7) Uani 1 1 d . . . . .
H24 H 0.8930 0.9713 0.3455 0.052 Uiso 1 1 calc R U . . .
C30 C 0.9771(2) 0.85135(19) 0.34800(10) 0.0354(6) Uani 1 1 d . . . . .
H23 H 0.9951 0.8571 0.3792 0.042 Uiso 1 1 calc R U . . .
C31 C 1.11857(19) 0.70024(17) 0.38988(8) 0.0267(5) Uani 1 1 d . . . . .
H27 H 1.1023 0.7436 0.4134 0.032 Uiso 1 1 calc R U . . .
C32 C 1.18373(19) 0.62365(17) 0.39355(8) 0.0268(5) Uani 1 1 d . . . . .
H26 H 1.2208 0.6061 0.4199 0.032 Uiso 1 1 calc R U . . .
C33 C 1.27615(19) 0.6110(2) 0.19449(11) 0.0397(7) Uani 1 1 d . . . . .
H55 H 1.2920 0.5442 0.1886 0.060 Uiso 1 1 calc R U . . .
H29 H 1.2825 0.6238 0.2272 0.060 Uiso 1 1 calc R U . . .
H31 H 1.3213 0.6521 0.1779 0.060 Uiso 1 1 calc R U . . .
C34 C 1.15279(18) 0.61591(17) 0.13351(9) 0.0272(5) Uani 1 1 d . . . . .
C35 C 1.05410(17) 0.63899(16) 0.12038(8) 0.0237(5) Uani 1 1 d . . . . .
C36 C 1.02023(18) 0.62640(16) 0.07470(8) 0.0245(5) Uani 1 1 d . . . . .
C37 C 0.91772(18) 0.64590(16) 0.05984(8) 0.0250(5) Uani 1 1 d . . . . .
C38 C 0.75593(18) 0.68297(17) 0.06360(8) 0.0257(5) Uani 1 1 d . . . . .
C39 C 0.66150(18) 0.70603(16) 0.08137(8) 0.0248(5) Uani 1 1 d . . . . .
C40 C 0.63744(17) 0.71147(17) 0.12851(8) 0.0253(5) Uani 1 1 d . . . . .
C41 C 0.65324(17) 0.70377(16) 0.20508(8) 0.0235(5) Uani 1 1 d . . . . .
C42 C 0.69679(17) 0.68162(16) 0.25044(7) 0.0214(4) Uani 1 1 d . . . . .
C43 C 0.77834(16) 0.61937(16) 0.25537(7) 0.0202(4) Uani 1 1 d . . . . .
C44 C 0.81494(17) 0.59309(16) 0.29970(8) 0.0232(5) Uani 1 1 d . . . . .
C45 C 0.9282(2) 0.4961(2) 0.34414(8) 0.0341(6) Uani 1 1 d . . . . .
H33 H 0.9477 0.5504 0.3631 0.051 Uiso 1 1 calc R U . . .
H32 H 0.9847 0.4540 0.3400 0.051 Uiso 1 1 calc R U . . .
H30 H 0.8757 0.4608 0.3590 0.051 Uiso 1 1 calc R U . . .
C46 C 0.77001(19) 0.63100(19) 0.33846(8) 0.0304(6) Uani 1 1 d . . . . .
H36 H 0.7932 0.6132 0.3679 0.036 Uiso 1 1 calc R U . . .
C47 C 0.6908(2) 0.6953(2) 0.33402(9) 0.0342(6) Uani 1 1 d . . . . .
H34 H 0.6624 0.7216 0.3605 0.041 Uiso 1 1 calc R U . . .
C48 C 0.65388(19) 0.72072(18) 0.29083(8) 0.0296(5) Uani 1 1 d . . . . .
H35 H 0.6004 0.7638 0.2882 0.036 Uiso 1 1 calc R U . . .
C49 C 0.55612(19) 0.74180(19) 0.19471(9) 0.0314(6) Uani 1 1 d . . . . .
H38 H 0.5084 0.7604 0.2161 0.038 Uiso 1 1 calc R U . . .
C50 C 0.54652(19) 0.74572(19) 0.14745(9) 0.0315(5) Uani 1 1 d . . . . .
H37 H 0.4906 0.7670 0.1307 0.038 Uiso 1 1 calc R U . . .
C51 C 0.57890(19) 0.72588(18) 0.04725(8) 0.0273(5) Uani 1 1 d . . . . .
C52 C 0.57248(19) 0.81615(18) 0.02462(8) 0.0286(5) Uani 1 1 d . . . . .
C53 C 0.4917(2) 0.83365(19) -0.00559(8) 0.0321(6) Uani 1 1 d . . . . .
H39 H 0.4869 0.8937 -0.0203 0.038 Uiso 1 1 calc R U . . .
C54 C 0.4187(2) 0.7646(2) -0.01434(8) 0.0347(6) Uani 1 1 d . . . . .
C55 C 0.4281(2) 0.6750(2) 0.00723(9) 0.0354(6) Uani 1 1 d . . . . .
H40 H 0.3808 0.6271 0.0007 0.042 Uiso 1 1 calc R U . . .
C56 C 0.50625(19) 0.65414(18) 0.03847(9) 0.0305(5) Uani 1 1 d . . . . .
C57 C 0.5108(2) 0.5562(2) 0.06190(11) 0.0433(7) Uani 1 1 d . . . . .
H41 H 0.4963 0.5636 0.0943 0.065 Uiso 1 1 calc R U . . .
H42 H 0.5765 0.5292 0.0587 0.065 Uiso 1 1 calc R U . . .
H43 H 0.4624 0.5136 0.0476 0.065 Uiso 1 1 calc R U . . .
C58 C 0.3309(3) 0.7853(3) -0.04646(10) 0.0537(8) Uani 1 1 d . . . . .
H46 H 0.3177 0.8538 -0.0468 0.081 Uiso 1 1 calc R U . . .
H45 H 0.2730 0.7513 -0.0357 0.081 Uiso 1 1 calc R U . . .
H44 H 0.3461 0.7638 -0.0773 0.081 Uiso 1 1 calc R U . . .
C59 C 0.6501(2) 0.8938(2) 0.03222(10) 0.0409(7) Uani 1 1 d . . . . .
H47 H 0.7109 0.8753 0.0173 0.061 Uiso 1 1 calc R U . . .
H48 H 0.6627 0.9018 0.0649 0.061 Uiso 1 1 calc R U . . .
H49 H 0.6262 0.9540 0.0193 0.061 Uiso 1 1 calc R U . . .
C60 C 0.7771(2) 0.66289(18) 0.01619(8) 0.0313(6) Uani 1 1 d . . . . .
H51 H 0.7318 0.6652 -0.0087 0.038 Uiso 1 1 calc R U . . .
C61 C 0.8766(2) 0.63951(19) 0.01403(8) 0.0325(6) Uani 1 1 d . . . . .
H50 H 0.9110 0.6225 -0.0126 0.039 Uiso 1 1 calc R U . . .
C62 C 1.0887(2) 0.58911(19) 0.04206(9) 0.0347(6) Uani 1 1 d . . . . .
H52 H 1.0680 0.5798 0.0114 0.042 Uiso 1 1 calc R U . . .
C63 C 1.1843(2) 0.5668(2) 0.05518(10) 0.0414(7) Uani 1 1 d . . . . .
H53 H 1.2280 0.5422 0.0333 0.050 Uiso 1 1 calc R U . . .
C64 C 1.2179(2) 0.58012(19) 0.10087(10) 0.0376(6) Uani 1 1 d . . . . .
H54 H 1.2836 0.5651 0.1093 0.045 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
O1 C2 1.365(3) . ?
O1 C1 1.423(3) . ?
O2 C12 1.369(3) . ?
O2 C13 1.420(3) . ?
O3 C11 1.358(3) . ?
O3 H60 0.8200 . ?
O4 C3 1.360(2) . ?
O5 C34 1.365(3) . ?
O5 C33 1.424(3) . ?
O6 C44 1.360(3) . ?
O6 C45 1.422(3) . ?
O7 C35 1.359(3) . ?
O7 H59 0.8200 . ?
O8 C43 1.360(2) . ?
N1 C5 1.352(3) . ?
N1 C6 1.390(3) . ?
N2 C9 1.350(3) . ?
N2 C8 1.395(3) . ?
N2 H56 0.98(5) . ?
N3 C37 1.357(3) . ?
N3 C38 1.387(3) . ?
N4 C41 1.345(3) . ?
N4 C40 1.382(3) . ?
N4 H62 0.8600 . ?
C1 H22 0.9600 . ?
C1 H21 0.9600 . ?
C1 H1 0.9600 . ?
C2 C28 1.385(3) . ?
C2 C3 1.401(3) . ?
C3 C4 1.395(3) . ?
C4 C30 1.411(3) . ?
C4 C5 1.460(3) . ?
C5 C31 1.425(3) . ?
C6 C7 1.400(3) . ?
C6 C32 1.426(3) . ?
C7 C8 1.395(3) . ?
C7 C19 1.498(3) . ?
C8 C17 1.422(3) . ?
C9 C18 1.417(3) . ?
C9 C10 1.457(3) . ?
C10 C11 1.393(3) . ?
C10 C14 1.411(3) . ?
C11 C12 1.399(3) . ?
C12 C16 1.379(3) . ?
C13 H28 0.9600 . ?
C13 H3 0.9600 . ?
C13 H2 0.9600 . ?
C14 C15 1.369(4) . ?
C14 H5 0.9300 . ?
C15 C16 1.391(4) . ?
C15 H6 0.9300 . ?
C16 H7 0.9300 . ?
C17 C18 1.365(3) . ?
C17 H9 0.9300 . ?
C18 H8 0.9300 . ?
C19 C24 1.393(3) . ?
C19 C20 1.398(4) . ?
C20 C21 1.396(4) . ?
C20 C27 1.502(4) . ?
C21 C22 1.376(5) . ?
C21 H17 0.9300 . ?
C22 C23 1.377(5) . ?
C22 C26 1.515(4) . ?
C23 C24 1.399(4) . ?
C23 H10 0.9300 . ?
C24 C25 1.509(4) . ?
C25 H11 0.9600 . ?
C25 H12 0.9600 . ?
C25 H13 0.9600 . ?
C26 H14 0.9600 . ?
C26 H16 0.9600 . ?
C26 H15 0.9600 . ?
C27 H20 0.9600 . ?
C27 H19 0.9600 . ?
C27 H18 0.9600 . ?
C28 C29 1.384(4) . ?
C28 H25 0.9300 . ?
C29 C30 1.369(4) . ?
C29 H24 0.9300 . ?
C30 H23 0.9300 . ?
C31 C32 1.370(3) . ?
C31 H27 0.9300 . ?
C32 H26 0.9300 . ?
C33 H55 0.9600 . ?
C33 H29 0.9600 . ?
C33 H31 0.9600 . ?
C34 C64 1.382(4) . ?
C34 C35 1.402(3) . ?
C35 C36 1.394(3) . ?
C36 C62 1.418(3) . ?
C36 C37 1.453(3) . ?
C37 C61 1.422(3) . ?
C38 C39 1.406(3) . ?
C38 C60 1.425(3) . ?
C39 C40 1.402(3) . ?
C39 C51 1.490(3) . ?
C40 C50 1.420(3) . ?
C41 C49 1.426(3) . ?
C41 C42 1.453(3) . ?
C42 C43 1.392(3) . ?
C42 C48 1.411(3) . ?
C43 C44 1.406(3) . ?
C44 C46 1.378(3) . ?
C45 H33 0.9600 . ?
C45 H32 0.9600 . ?
C45 H30 0.9600 . ?
C46 C47 1.384(4) . ?
C46 H36 0.9300 . ?
C47 C48 1.375(4) . ?
C47 H34 0.9300 . ?
C48 H35 0.9300 . ?
C49 C50 1.365(4) . ?
C49 H38 0.9300 . ?
C50 H37 0.9300 . ?
C51 C52 1.404(3) . ?
C51 C56 1.405(4) . ?
C52 C53 1.395(3) . ?
C52 C59 1.503(4) . ?
C53 C54 1.382(4) . ?
C53 H39 0.9300 . ?
C54 C55 1.386(4) . ?
C54 C58 1.509(4) . ?
C55 C56 1.396(3) . ?
C55 H40 0.9300 . ?
C56 C57 1.507(4) . ?
C57 H41 0.9600 . ?
C57 H42 0.9600 . ?
C57 H43 0.9600 . ?
C58 H46 0.9600 . ?
C58 H45 0.9600 . ?
C58 H44 0.9600 . ?
C59 H47 0.9600 . ?
C59 H48 0.9600 . ?
C59 H49 0.9600 . ?
C60 C61 1.370(4) . ?
C60 H51 0.9300 . ?
C61 H50 0.9300 . ?
C62 C63 1.362(4) . ?
C62 H52 0.9300 . ?
C63 C64 1.394(4) . ?
C63 H53 0.9300 . ?
C64 H54 0.9300 . ?

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
C2 O1 C1 117.22(19) . . ?
C12 O2 C13 117.69(19) . . ?
C11 O3 H60 109.5 . . ?
C34 O5 C33 117.8(2) . . ?
C44 O6 C45 117.21(19) . . ?
C35 O7 H59 109.5 . . ?
C5 N1 C6 108.18(18) . . ?
C9 N2 C8 108.23(19) . . ?
C9 N2 H56 120(3) . . ?
C8 N2 H56 131(3) . . ?
C37 N3 C38 108.45(19) . . ?
C41 N4 C40 108.46(19) . . ?
C41 N4 H62 125.8 . . ?
C40 N4 H62 125.8 . . ?
O1 C1 H22 109.5 . . ?
O1 C1 H21 109.5 . . ?
H22 C1 H21 109.5 . . ?
O1 C1 H1 109.5 . . ?
H22 C1 H1 109.5 . . ?
H21 C1 H1 109.5 . . ?
O1 C2 C28 125.3(2) . . ?
O1 C2 C3 114.70(19) . . ?
C28 C2 C3 120.0(2) . . ?
O4 C3 C4 120.77(19) . . ?
O4 C3 C2 118.6(2) . . ?
C4 C3 C2 120.65(19) . . ?
C3 C4 C30 118.0(2) . . ?
C3 C4 C5 121.52(19) . . ?
C30 C4 C5 120.4(2) . . ?
N1 C5 C31 109.3(2) . . ?
N1 C5 C4 123.05(19) . . ?
C31 C5 C4 127.6(2) . . ?
N1 C6 C7 125.8(2) . . ?
N1 C6 C32 107.81(19) . . ?
C7 C6 C32 126.4(2) . . ?
C8 C7 C6 126.8(2) . . ?
C8 C7 C19 116.6(2) . . ?
C6 C7 C19 116.6(2) . . ?
N2 C8 C7 126.1(2) . . ?
N2 C8 C17 107.5(2) . . ?
C7 C8 C17 126.4(2) . . ?
N2 C9 C18 109.0(2) . . ?
N2 C9 C10 123.9(2) . . ?
C18 C9 C10 127.1(2) . . ?
C11 C10 C14 118.3(2) . . ?
C11 C10 C9 122.03(19) . . ?
C14 C10 C9 119.7(2) . . ?
O3 C11 C10 118.9(2) . . ?
O3 C11 C12 120.6(2) . . ?
C10 C11 C12 120.6(2) . . ?
O2 C12 C16 125.3(2) . . ?
O2 C12 C11 114.64(19) . . ?
C16 C12 C11 120.0(2) . . ?
O2 C13 H28 109.5 . . ?
O2 C13 H3 109.5 . . ?
H28 C13 H3 109.5 . . ?
O2 C13 H2 109.5 . . ?
H28 C13 H2 109.5 . . ?
H3 C13 H2 109.5 . . ?
C15 C14 C10 120.8(2) . . ?
C15 C14 H5 119.6 . . ?
C10 C14 H5 119.6 . . ?
C14 C15 C16 120.5(2) . . ?
C14 C15 H6 119.7 . . ?
C16 C15 H6 119.7 . . ?
C12 C16 C15 119.8(2) . . ?
C12 C16 H7 120.1 . . ?
C15 C16 H7 120.1 . . ?
C18 C17 C8 107.6(2) . . ?
C18 C17 H9 126.2 . . ?
C8 C17 H9 126.2 . . ?
C17 C18 C9 107.6(2) . . ?
C17 C18 H8 126.2 . . ?
C9 C18 H8 126.2 . . ?
C24 C19 C20 120.9(2) . . ?
C24 C19 C7 120.7(2) . . ?
C20 C19 C7 118.4(2) . . ?
C21 C20 C19 118.0(3) . . ?
C21 C20 C27 120.8(3) . . ?
C19 C20 C27 121.2(2) . . ?
C22 C21 C20 122.4(3) . . ?
C22 C21 H17 118.8 . . ?
C20 C21 H17 118.8 . . ?
C21 C22 C23 118.4(3) . . ?
C21 C22 C26 121.0(3) . . ?
C23 C22 C26 120.6(3) . . ?
C22 C23 C24 121.8(3) . . ?
C22 C23 H10 119.1 . . ?
C24 C23 H10 119.1 . . ?
C19 C24 C23 118.5(3) . . ?
C19 C24 C25 120.7(2) . . ?
C23 C24 C25 120.8(3) . . ?
C24 C25 H11 109.5 . . ?
C24 C25 H12 109.5 . . ?
H11 C25 H12 109.5 . . ?
C24 C25 H13 109.5 . . ?
H11 C25 H13 109.5 . . ?
H12 C25 H13 109.5 . . ?
C22 C26 H14 109.5 . . ?
C22 C26 H16 109.5 . . ?
H14 C26 H16 109.5 . . ?
C22 C26 H15 109.5 . . ?
H14 C26 H15 109.5 . . ?
H16 C26 H15 109.5 . . ?
C20 C27 H20 109.5 . . ?
C20 C27 H19 109.5 . . ?
H20 C27 H19 109.5 . . ?
C20 C27 H18 109.5 . . ?
H20 C27 H18 109.5 . . ?
H19 C27 H18 109.5 . . ?
C29 C28 C2 119.5(2) . . ?
C29 C28 H25 120.2 . . ?
C2 C28 H25 120.2 . . ?
C30 C29 C28 121.1(2) . . ?
C30 C29 H24 119.4 . . ?
C28 C29 H24 119.4 . . ?
C29 C30 C4 120.7(2) . . ?
C29 C30 H23 119.7 . . ?
C4 C30 H23 119.7 . . ?
C32 C31 C5 107.2(2) . . ?
C32 C31 H27 126.4 . . ?
C5 C31 H27 126.4 . . ?
C31 C32 C6 107.6(2) . . ?
C31 C32 H26 126.2 . . ?
C6 C32 H26 126.2 . . ?
O5 C33 H55 109.5 . . ?
O5 C33 H29 109.5 . . ?
H55 C33 H29 109.5 . . ?
O5 C33 H31 109.5 . . ?
H55 C33 H31 109.5 . . ?
H29 C33 H31 109.5 . . ?
O5 C34 C64 125.0(2) . . ?
O5 C34 C35 115.2(2) . . ?
C64 C34 C35 119.8(2) . . ?
O7 C35 C36 119.0(2) . . ?
O7 C35 C34 120.0(2) . . ?
C36 C35 C34 121.0(2) . . ?
C35 C36 C62 117.8(2) . . ?
C35 C36 C37 123.0(2) . . ?
C62 C36 C37 119.1(2) . . ?
N3 C37 C61 108.7(2) . . ?
N3 C37 C36 123.8(2) . . ?
C61 C37 C36 127.5(2) . . ?
N3 C38 C39 126.2(2) . . ?
N3 C38 C60 107.9(2) . . ?
C39 C38 C60 125.9(2) . . ?
C40 C39 C38 125.9(2) . . ?
C40 C39 C51 116.7(2) . . ?
C38 C39 C51 117.4(2) . . ?
N4 C40 C39 125.2(2) . . ?
N4 C40 C50 107.9(2) . . ?
C39 C40 C50 126.9(2) . . ?
N4 C41 C49 109.0(2) . . ?
N4 C41 C42 123.0(2) . . ?
C49 C41 C42 127.9(2) . . ?
C43 C42 C48 118.6(2) . . ?
C43 C42 C41 121.46(19) . . ?
C48 C42 C41 119.9(2) . . ?
O8 C43 C42 120.1(2) . . ?
O8 C43 C44 119.1(2) . . ?
C42 C43 C44 120.7(2) . . ?
O6 C44 C46 125.5(2) . . ?
O6 C44 C43 115.31(19) . . ?
C46 C44 C43 119.2(2) . . ?
O6 C45 H33 109.5 . . ?
O6 C45 H32 109.5 . . ?
H33 C45 H32 109.5 . . ?
O6 C45 H30 109.5 . . ?
H33 C45 H30 109.5 . . ?
H32 C45 H30 109.5 . . ?
C44 C46 C47 120.7(2) . . ?
C44 C46 H36 119.7 . . ?
C47 C46 H36 119.7 . . ?
C48 C47 C46 120.6(2) . . ?
C48 C47 H34 119.7 . . ?
C46 C47 H34 119.7 . . ?
C47 C48 C42 120.2(2) . . ?
C47 C48 H35 119.9 . . ?
C42 C48 H35 119.9 . . ?
C50 C49 C41 107.0(2) . . ?
C50 C49 H38 126.5 . . ?
C41 C49 H38 126.5 . . ?
C49 C50 C40 107.6(2) . . ?
C49 C50 H37 126.2 . . ?
C40 C50 H37 126.2 . . ?
C52 C51 C56 120.1(2) . . ?
C52 C51 C39 120.4(2) . . ?
C56 C51 C39 119.4(2) . . ?
C53 C52 C51 118.8(2) . . ?
C53 C52 C59 119.5(2) . . ?
C51 C52 C59 121.7(2) . . ?
C54 C53 C52 122.1(2) . . ?
C54 C53 H39 119.0 . . ?
C52 C53 H39 119.0 . . ?
C53 C54 C55 118.2(2) . . ?
C53 C54 C58 121.4(3) . . ?
C55 C54 C58 120.4(3) . . ?
C54 C55 C56 122.2(3) . . ?
C54 C55 H40 118.9 . . ?
C56 C55 H40 118.9 . . ?
C55 C56 C51 118.6(2) . . ?
C55 C56 C57 119.7(2) . . ?
C51 C56 C57 121.7(2) . . ?
C56 C57 H41 109.5 . . ?
C56 C57 H42 109.5 . . ?
H41 C57 H42 109.5 . . ?
C56 C57 H43 109.5 . . ?
H41 C57 H43 109.5 . . ?
H42 C57 H43 109.5 . . ?
C54 C58 H46 109.5 . . ?
C54 C58 H45 109.5 . . ?
H46 C58 H45 109.5 . . ?
C54 C58 H44 109.5 . . ?
H46 C58 H44 109.5 . . ?
H45 C58 H44 109.5 . . ?
C52 C59 H47 109.5 . . ?
C52 C59 H48 109.5 . . ?
H47 C59 H48 109.5 . . ?
C52 C59 H49 109.5 . . ?
H47 C59 H49 109.5 . . ?
H48 C59 H49 109.5 . . ?
C61 C60 C38 107.3(2) . . ?
C61 C60 H51 126.4 . . ?
C38 C60 H51 126.4 . . ?
C60 C61 C37 107.7(2) . . ?
C60 C61 H50 126.2 . . ?
C37 C61 H50 126.2 . . ?
C63 C62 C36 120.7(3) . . ?
C63 C62 H52 119.6 . . ?
C36 C62 H52 119.6 . . ?
C62 C63 C64 121.1(2) . . ?
C62 C63 H53 119.4 . . ?
C64 C63 H53 119.4 . . ?
C34 C64 C63 119.5(2) . . ?
C34 C64 H54 120.3 . . ?
C63 C64 H54 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 O1 C2 C28 -0.2(4) . . . . ?
C1 O1 C2 C3 -179.6(2) . . . . ?
O1 C2 C3 O4 1.4(3) . . . . ?
C28 C2 C3 O4 -178.0(2) . . . . ?
O1 C2 C3 C4 -179.0(2) . . . . ?
C28 C2 C3 C4 1.5(3) . . . . ?
O4 C3 C4 C30 177.9(2) . . . . ?
C2 C3 C4 C30 -1.6(3) . . . . ?
O4 C3 C4 C5 -0.5(3) . . . . ?
C2 C3 C4 C5 180.0(2) . . . . ?
C6 N1 C5 C31 -1.2(2) . . . . ?
C6 N1 C5 C4 176.3(2) . . . . ?
C3 C4 C5 N1 0.0(3) . . . . ?
C30 C4 C5 N1 -178.4(2) . . . . ?
C3 C4 C5 C31 177.1(2) . . . . ?
C30 C4 C5 C31 -1.3(4) . . . . ?
C5 N1 C6 C7 -178.4(2) . . . . ?
C5 N1 C6 C32 0.5(2) . . . . ?
N1 C6 C7 C8 -10.6(4) . . . . ?
C32 C6 C7 C8 170.7(2) . . . . ?
N1 C6 C7 C19 166.8(2) . . . . ?
C32 C6 C7 C19 -11.9(3) . . . . ?
C9 N2 C8 C7 178.1(2) . . . . ?
C9 N2 C8 C17 -0.8(2) . . . . ?
C6 C7 C8 N2 -6.2(4) . . . . ?
C19 C7 C8 N2 176.4(2) . . . . ?
C6 C7 C8 C17 172.4(2) . . . . ?
C19 C7 C8 C17 -5.0(3) . . . . ?
C8 N2 C9 C18 0.6(2) . . . . ?
C8 N2 C9 C10 -179.7(2) . . . . ?
N2 C9 C10 C11 -10.7(3) . . . . ?
C18 C9 C10 C11 169.0(2) . . . . ?
N2 C9 C10 C14 170.0(2) . . . . ?
C18 C9 C10 C14 -10.3(4) . . . . ?
C14 C10 C11 O3 179.4(2) . . . . ?
C9 C10 C11 O3 0.1(3) . . . . ?
C14 C10 C11 C12 0.7(3) . . . . ?
C9 C10 C11 C12 -178.6(2) . . . . ?
C13 O2 C12 C16 4.7(3) . . . . ?
C13 O2 C12 C11 -174.9(2) . . . . ?
O3 C11 C12 O2 1.2(3) . . . . ?
C10 C11 C12 O2 179.9(2) . . . . ?
O3 C11 C12 C16 -178.4(2) . . . . ?
C10 C11 C12 C16 0.3(3) . . . . ?
C11 C10 C14 C15 -1.2(4) . . . . ?
C9 C10 C14 C15 178.1(2) . . . . ?
C10 C14 C15 C16 0.7(4) . . . . ?
O2 C12 C16 C15 179.5(2) . . . . ?
C11 C12 C16 C15 -0.9(4) . . . . ?
C14 C15 C16 C12 0.4(4) . . . . ?
N2 C8 C17 C18 0.8(3) . . . . ?
C7 C8 C17 C18 -178.1(2) . . . . ?
C8 C17 C18 C9 -0.4(3) . . . . ?
N2 C9 C18 C17 -0.1(3) . . . . ?
C10 C9 C18 C17 -179.8(2) . . . . ?
C8 C7 C19 C24 -90.0(3) . . . . ?
C6 C7 C19 C24 92.4(3) . . . . ?
C8 C7 C19 C20 89.8(3) . . . . ?
C6 C7 C19 C20 -87.9(3) . . . . ?
C24 C19 C20 C21 -3.4(4) . . . . ?
C7 C19 C20 C21 176.9(2) . . . . ?
C24 C19 C20 C27 174.2(3) . . . . ?
C7 C19 C20 C27 -5.6(4) . . . . ?
C19 C20 C21 C22 1.7(4) . . . . ?
C27 C20 C21 C22 -175.9(3) . . . . ?
C20 C21 C22 C23 0.9(4) . . . . ?
C20 C21 C22 C26 179.6(3) . . . . ?
C21 C22 C23 C24 -1.9(4) . . . . ?
C26 C22 C23 C24 179.4(3) . . . . ?
C20 C19 C24 C23 2.4(4) . . . . ?
C7 C19 C24 C23 -177.8(2) . . . . ?
C20 C19 C24 C25 -177.2(3) . . . . ?
C7 C19 C24 C25 2.5(4) . . . . ?
C22 C23 C24 C19 0.3(4) . . . . ?
C22 C23 C24 C25 179.9(3) . . . . ?
O1 C2 C28 C29 -179.6(3) . . . . ?
C3 C2 C28 C29 -0.3(4) . . . . ?
C2 C28 C29 C30 -0.9(5) . . . . ?
C28 C29 C30 C4 0.7(5) . . . . ?
C3 C4 C30 C29 0.5(4) . . . . ?
C5 C4 C30 C29 179.0(3) . . . . ?
N1 C5 C31 C32 1.6(3) . . . . ?
C4 C5 C31 C32 -175.8(2) . . . . ?
C5 C31 C32 C6 -1.2(3) . . . . ?
N1 C6 C32 C31 0.5(3) . . . . ?
C7 C6 C32 C31 179.4(2) . . . . ?
C33 O5 C34 C64 2.8(4) . . . . ?
C33 O5 C34 C35 -178.1(2) . . . . ?
O5 C34 C35 O7 1.4(3) . . . . ?
C64 C34 C35 O7 -179.4(2) . . . . ?
O5 C34 C35 C36 -179.1(2) . . . . ?
C64 C34 C35 C36 0.0(3) . . . . ?
O7 C35 C36 C62 179.7(2) . . . . ?
C34 C35 C36 C62 0.3(3) . . . . ?
O7 C35 C36 C37 -2.9(3) . . . . ?
C34 C35 C36 C37 177.7(2) . . . . ?
C38 N3 C37 C61 0.5(3) . . . . ?
C38 N3 C37 C36 -178.6(2) . . . . ?
C35 C36 C37 N3 -3.9(4) . . . . ?
C62 C36 C37 N3 173.5(2) . . . . ?
C35 C36 C37 C61 177.1(2) . . . . ?
C62 C36 C37 C61 -5.5(4) . . . . ?
C37 N3 C38 C39 177.2(2) . . . . ?
C37 N3 C38 C60 -0.9(3) . . . . ?
N3 C38 C39 C40 -8.0(4) . . . . ?
C60 C38 C39 C40 169.8(2) . . . . ?
N3 C38 C39 C51 172.5(2) . . . . ?
C60 C38 C39 C51 -9.7(4) . . . . ?
C41 N4 C40 C39 178.0(2) . . . . ?
C41 N4 C40 C50 -0.7(3) . . . . ?
C38 C39 C40 N4 -6.6(4) . . . . ?
C51 C39 C40 N4 172.9(2) . . . . ?
C38 C39 C40 C50 171.9(2) . . . . ?
C51 C39 C40 C50 -8.6(4) . . . . ?
C40 N4 C41 C49 0.3(3) . . . . ?
C40 N4 C41 C42 177.6(2) . . . . ?
N4 C41 C42 C43 -16.1(3) . . . . ?
C49 C41 C42 C43 160.6(2) . . . . ?
N4 C41 C42 C48 166.3(2) . . . . ?
C49 C41 C42 C48 -17.0(4) . . . . ?
C48 C42 C43 O8 179.0(2) . . . . ?
C41 C42 C43 O8 1.3(3) . . . . ?
C48 C42 C43 C44 2.3(3) . . . . ?
C41 C42 C43 C44 -175.3(2) . . . . ?
C45 O6 C44 C46 3.9(3) . . . . ?
C45 O6 C44 C43 -175.6(2) . . . . ?
O8 C43 C44 O6 1.8(3) . . . . ?
C42 C43 C44 O6 178.50(19) . . . . ?
O8 C43 C44 C46 -177.7(2) . . . . ?
C42 C43 C44 C46 -1.0(3) . . . . ?
O6 C44 C46 C47 179.6(2) . . . . ?
C43 C44 C46 C47 -1.0(3) . . . . ?
C44 C46 C47 C48 1.6(4) . . . . ?
C46 C47 C48 C42 -0.3(4) . . . . ?
C43 C42 C48 C47 -1.7(3) . . . . ?
C41 C42 C48 C47 176.0(2) . . . . ?
N4 C41 C49 C50 0.2(3) . . . . ?
C42 C41 C49 C50 -176.8(2) . . . . ?
C41 C49 C50 C40 -0.7(3) . . . . ?
N4 C40 C50 C49 0.9(3) . . . . ?
C39 C40 C50 C49 -177.8(2) . . . . ?
C40 C39 C51 C52 102.1(3) . . . . ?
C38 C39 C51 C52 -78.4(3) . . . . ?
C40 C39 C51 C56 -76.8(3) . . . . ?
C38 C39 C51 C56 102.8(3) . . . . ?
C56 C51 C52 C53 1.6(4) . . . . ?
C39 C51 C52 C53 -177.3(2) . . . . ?
C56 C51 C52 C59 -178.5(2) . . . . ?
C39 C51 C52 C59 2.7(4) . . . . ?
C51 C52 C53 C54 -0.8(4) . . . . ?
C59 C52 C53 C54 179.3(2) . . . . ?
C52 C53 C54 C55 -1.2(4) . . . . ?
C52 C53 C54 C58 178.9(2) . . . . ?
C53 C54 C55 C56 2.4(4) . . . . ?
C58 C54 C55 C56 -177.6(3) . . . . ?
C54 C55 C56 C51 -1.7(4) . . . . ?
C54 C55 C56 C57 178.2(3) . . . . ?
C52 C51 C56 C55 -0.4(4) . . . . ?
C39 C51 C56 C55 178.5(2) . . . . ?
C52 C51 C56 C57 179.7(2) . . . . ?
C39 C51 C56 C57 -1.4(4) . . . . ?
N3 C38 C60 C61 0.9(3) . . . . ?
C39 C38 C60 C61 -177.2(2) . . . . ?
C38 C60 C61 C37 -0.6(3) . . . . ?
N3 C37 C61 C60 0.0(3) . . . . ?
C36 C37 C61 C60 179.2(2) . . . . ?
C35 C36 C62 C63 -0.2(4) . . . . ?
C37 C36 C62 C63 -177.7(2) . . . . ?
C36 C62 C63 C64 -0.2(4) . . . . ?
O5 C34 C64 C63 178.7(2) . . . . ?
C35 C34 C64 C63 -0.4(4) . . . . ?
C62 C63 C64 C34 0.5(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H60 O2 0.82 2.21 2.661(2) 114.8 .
O3 H60 O8 0.82 1.94 2.691(2) 152.3 .
O7 H59 O4 0.82 2.02 2.782(2) 153.8 .
O7 H59 O5 0.82 2.21 2.664(2) 115.4 .
N2 H56 O3 0.98(5) 1.92(4) 2.622(3) 126(4) .
N4 H62 O8 0.86 2.10 2.626(2) 119.3 .
N4 H62 N3 0.86 2.42 2.939(3) 119.6 .
O3 H60 O2 0.82 2.21 2.661(2) 114.8 .
O3 H60 O8 0.82 1.94 2.691(2) 152.3 .
O7 H59 O4 0.82 2.02 2.782(2) 153.8 .
O7 H59 O5 0.82 2.21 2.664(2) 115.4 .
N2 H56 O3 0.98(5) 1.92(4) 2.622(3) 126(4) .
N4 H62 O8 0.86 2.10 2.626(2) 119.3 .
N4 H62 N3 0.86 2.42 2.939(3) 119.6 .
O3 H60 O2 0.82 2.21 2.661(2) 114.8 .
O3 H60 O8 0.82 1.94 2.691(2) 152.3 .
O3 H60 O2 0.82 2.21 2.661(2) 114.8 .
O3 H60 O8 0.82 1.94 2.691(2) 152.3 .
O7 H59 O4 0.82 2.02 2.782(2) 153.8 .
O7 H59 O5 0.82 2.21 2.664(2) 115.4 .
N2 H56 O3 0.98(5) 1.92(4) 2.622(3) 126(4) .
N4 H62 O8 0.86 2.10 2.626(2) 119.3 .
N4 H62 N3 0.86 2.42 2.939(3) 119.6 .
O3 H60 O2 0.82 2.21 2.661(2) 114.8 .
O3 H60 O8 0.82 1.94 2.691(2) 152.3 .
O7 H59 O4 0.82 2.02 2.782(2) 153.8 .
O7 H59 O5 0.82 2.21 2.664(2) 115.4 .
N2 H56 O3 0.98(5) 1.92(4) 2.622(3) 126(4) .
N4 H62 O8 0.86 2.10 2.626(2) 119.3 .
N4 H62 N3 0.86 2.42 2.939(3) 119.6 .

_refine_diff_density_max         0.613
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.081



