# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_1H
_database_code_depnum_ccdc_archive 'CCDC 1476165'
_audit_update_record             
;
2016-08-02 deposited with the CCDC.
2016-08-18 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            'C38 H39 N3 O1.50'
_chemical_formula_weight         561.72

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/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   14.5185(6)
_cell_length_b                   9.4875(3)
_cell_length_c                   25.1680(12)
_cell_angle_alpha                90
_cell_angle_beta                 115.815(3)
_cell_angle_gamma                90
_cell_volume                     3120.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3765
_cell_measurement_theta_min      1.558
_cell_measurement_theta_max      25.791

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.073
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12874
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.558
_diffrn_reflns_theta_max         25.791
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5903
_reflns_number_gt                4307
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND & Olex 2.1'
_computing_publication_material  WinGX
_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)+(0.0880P)²+0.9780P] 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         5903
_refine_ls_number_parameters     435
_refine_ls_number_restraints     335
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0610
_refine_ls_wR_factor_ref         0.1796
_refine_ls_wR_factor_gt          0.1577
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.003
_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
C0AA C 0.51844(14) -0.4119(2) -0.07428(8) 0.0376(4) Uani 1 1 d . U . . .
C4AA C 0.58182(15) -0.3026(2) -0.04319(9) 0.0429(5) Uani 1 1 d . U . . .
H4AA H 0.5736 -0.2082 -0.0542 0.052 Uiso 1 1 calc R U . . .
C3 C 0.66042(16) -0.3588(2) 0.00759(9) 0.0426(5) Uani 1 1 d . U . . .
H3 H 0.7137 -0.3087 0.0365 0.051 Uiso 1 1 calc R U . . .
C4 C 0.64452(14) -0.5027(2) 0.00695(8) 0.0366(4) Uani 1 1 d . U . . .
C5 C 0.70500(15) -0.6062(2) 0.04982(8) 0.0379(4) Uani 1 1 d . U . . .
H5 H 0.7612 -0.5752 0.0834 0.045 Uiso 1 1 calc R U . . .
C6 C 0.42816(15) -0.4094(2) -0.12979(9) 0.0385(4) Uani 1 1 d . U . . .
H6 H 0.4064 -0.3238 -0.1492 0.046 Uiso 1 1 calc R U . . .
C5AA C 0.28614(15) -0.5027(2) -0.20988(8) 0.0421(5) Uani 1 1 d . U . . .
H5AA H 0.2816 -0.4034 -0.2215 0.050 Uiso 1 1 calc R U . . .
C8 C 0.19158(16) -0.5388(2) -0.20196(9) 0.0433(5) Uani 1 1 d . U . . .
C6AA C 0.10716(16) -0.4508(3) -0.22438(9) 0.0509(5) Uani 1 1 d . U . . .
H6AA H 0.1085 -0.3703 -0.2451 0.061 Uiso 1 1 calc R U . . .
C10 C 0.02044(18) -0.4811(3) -0.21632(11) 0.0634(7) Uani 1 1 d . U . . .
H10 H -0.0359 -0.4214 -0.2317 0.076 Uiso 1 1 calc R U . . .
C1AA C 0.01828(19) -0.6003(3) -0.18533(11) 0.0644(7) Uani 1 1 d . U . . .
H1AA H -0.0393 -0.6200 -0.1794 0.077 Uiso 1 1 calc R U . . .
C12 C 0.10138(18) -0.6900(3) -0.16323(10) 0.0575(6) Uani 1 1 d . U . . .
H12 H 0.0994 -0.7708 -0.1428 0.069 Uiso 1 1 calc R U . . .
C2AA C 0.18776(17) -0.6602(2) -0.17142(9) 0.0480(5) Uani 1 1 d . U . . .
H2AA H 0.2435 -0.7211 -0.1565 0.058 Uiso 1 1 calc R U . . .
C14 C 0.30009(17) -0.5907(2) -0.25645(9) 0.0469(5) Uani 1 1 d . U . . .
C3AA C 0.22309(19) -0.6732(3) -0.29627(9) 0.0552(6) Uani 1 1 d . U . . .
H3AA H 0.1605 -0.6781 -0.2945 0.066 Uiso 1 1 calc R U . . .
C16 C 0.2377(2) -0.7497(3) -0.33930(11) 0.0708(7) Uani 1 1 d . U . . .
H16 H 0.1853 -0.8063 -0.3655 0.085 Uiso 1 1 calc R U . . .
C17 C 0.3288(3) -0.7417(3) -0.34309(12) 0.0784(8) Uani 1 1 d . U . . .
H17 H 0.3381 -0.7913 -0.3723 0.094 Uiso 1 1 calc R U . . .
C18 C 0.4054(3) -0.6608(4) -0.30391(14) 0.0888(10) Uani 1 1 d . U . . .
H18 H 0.4677 -0.6562 -0.3061 0.107 Uiso 1 1 calc R U . . .
C19 C 0.3921(2) -0.5852(3) -0.26072(12) 0.0726(8) Uani 1 1 d . U . . .
H19 H 0.4453 -0.5301 -0.2343 0.087 Uiso 1 1 calc R U . . .
C20 C 0.75589(15) -0.8260(2) 0.09362(9) 0.0423(5) Uani 1 1 d . U . . .
H20 H 0.8004 -0.7637 0.1256 0.051 Uiso 1 1 calc R U . . .
C21 C 0.69543(18) -0.9171(2) 0.11654(10) 0.0497(5) Uani 1 1 d . U . . .
C22 C 0.60525(19) -0.9829(3) 0.07888(13) 0.0631(6) Uani 1 1 d . U . . .
H22 H 0.5798 -0.9688 0.0384 0.076 Uiso 1 1 calc R U . . .
C23 C 0.5524(3) -1.0692(3) 0.10040(18) 0.0920(11) Uani 1 1 d . U . . .
H23 H 0.4923 -1.1134 0.0747 0.110 Uiso 1 1 calc R U . . .
C24 C 0.5907(3) -1.0890(4) 0.1612(2) 0.1123(14) Uani 1 1 d . U . . .
H24 H 0.5555 -1.1461 0.1762 0.135 Uiso 1 1 calc R U . . .
C25 C 0.6792(4) -1.0250(4) 0.19866(18) 0.1072(13) Uani 1 1 d . U . . .
H25 H 0.7046 -1.0394 0.2391 0.129 Uiso 1 1 calc R U . . .
C26 C 0.7317(2) -0.9386(3) 0.17695(12) 0.0745(8) Uani 1 1 d . U . . .
H26 H 0.7916 -0.8946 0.2030 0.089 Uiso 1 1 calc R U . . .
C27 C 0.82238(16) -0.9150(2) 0.07414(9) 0.0422(5) Uani 1 1 d . U . . .
C28 C 0.78162(18) -0.9996(2) 0.02452(10) 0.0551(6) Uani 1 1 d . U . . .
H28 H 0.7112 -1.0011 0.0016 0.066 Uiso 1 1 calc R U . . .
C29 C 0.8434(2) -1.0815(3) 0.00858(12) 0.0615(6) Uani 1 1 d . U . . .
H29 H 0.8146 -1.1382 -0.0248 0.074 Uiso 1 1 calc R U . . .
C30 C 0.9469(2) -1.0800(3) 0.04160(14) 0.0742(8) Uani 1 1 d . U . . .
H30 H 0.9889 -1.1334 0.0302 0.089 Uiso 1 1 calc R U . . .
C31 C 0.9886(2) -0.9995(4) 0.09165(17) 0.0967(11) Uani 1 1 d . U . . .
H31 H 1.0589 -1.0008 0.1150 0.116 Uiso 1 1 calc R U . . .
C32 C 0.92657(19) -0.9162(3) 0.10759(13) 0.0722(8) Uani 1 1 d . U . . .
H32 H 0.9556 -0.8605 0.1413 0.087 Uiso 1 1 calc R U . . .
C33 C 0.3158(5) -0.2563(7) -0.3897(3) 0.1069(16) Uani 0.75 1 d . U P A 1
H33A H 0.3794 -0.3012 -0.3632 0.128 Uiso 0.75 1 calc R U P A 1
H33B H 0.3124 -0.2544 -0.4290 0.128 Uiso 0.75 1 calc R U P A 1
C34B C 0.2284(4) -0.3321(5) -0.3897(2) 0.0826(12) Uani 0.75 1 d . U P A 1
H34A H 0.1716 -0.3311 -0.4288 0.099 Uiso 0.75 1 calc R U P A 1
H34B H 0.2464 -0.4292 -0.3777 0.099 Uiso 0.75 1 calc R U P A 1
O35B O 0.2019(5) -0.2597(4) -0.3486(3) 0.1468(18) Uani 0.75 1 d . U P A 1
C36B C 0.2300(5) -0.1264(5) -0.3480(3) 0.1054(17) Uani 0.75 1 d . U P A 1
H36A H 0.2566 -0.0897 -0.3080 0.126 Uiso 0.75 1 calc R U P A 1
H36B H 0.1710 -0.0702 -0.3728 0.126 Uiso 0.75 1 calc R U P A 1
C1BB C 0.3100(6) -0.1157(8) -0.3699(4) 0.145(3) Uani 0.75 1 d . U P A 1
H1BA H 0.2901 -0.0488 -0.4021 0.174 Uiso 0.75 1 calc R U P A 1
H1BB H 0.3751 -0.0870 -0.3385 0.174 Uiso 0.75 1 calc R U P A 1
C37B C 0.0760(12) -0.5406(16) 0.0045(8) 0.121(4) Uani 0.5 1 d D U P B -1
H37A H 0.1471 -0.5179 0.0294 0.145 Uiso 0.5 1 calc R U P B -1
H37B H 0.0730 -0.6260 -0.0174 0.145 Uiso 0.5 1 calc R U P B -1
C38B C 0.0182(13) -0.557(2) 0.0400(9) 0.220(11) Uani 0.5 1 d D U P B -1
H38A H -0.0073 -0.6529 0.0367 0.264 Uiso 0.5 1 calc R U P B -1
H38B H 0.0619 -0.5375 0.0812 0.264 Uiso 0.5 1 calc R U P B -1
N1 N 0.55781(12) -0.53300(16) -0.04303(7) 0.0364(4) Uani 1 1 d . U . . .
H1 H 0.5319 -0.6157 -0.0533 0.044 Uiso 1 1 calc R U . . .
N2 N 0.37719(12) -0.51993(17) -0.15310(7) 0.0413(4) Uani 1 1 d . U . . .
N3 N 0.68573(12) -0.73778(17) 0.04424(7) 0.0398(4) Uani 1 1 d . U . . .
O2 O -0.0610(7) -0.3854(8) -0.0309(2) 0.129(2) Uani 0.5 1 d D U P B -1
C38A C 0.0242(9) -0.4232(11) -0.0358(5) 0.109(3) Uani 0.5 1 d D U P B -1
H38C H 0.0702 -0.3432 -0.0265 0.131 Uiso 0.5 1 calc R U P B -1
H38D H 0.0064 -0.4515 -0.0761 0.131 Uiso 0.5 1 calc R U P B -1
C37A C -0.0641(14) -0.4605(19) 0.0175(5) 0.105(4) Uani 0.5 1 d D U P B -1
H37C H -0.0590 -0.3949 0.0482 0.126 Uiso 0.5 1 calc R U P B -1
H37D H -0.1285 -0.5107 0.0044 0.126 Uiso 0.5 1 calc R U P B -1
O1 O 0.3315(10) -0.1861(15) -0.3119(5) 0.128(4) Uani 0.25 1 d . . P C 2
C2 C 0.2441(10) -0.1968(18) -0.3134(6) 0.071(3) Uiso 0.25 1 d . . P C 2
C7AA C 0.182(2) -0.194(3) -0.3818(12) 0.117(8) Uiso 0.2 1 d . . P C 2
C1 C 0.3610(18) -0.203(3) -0.3532(12) 0.133(7) Uiso 0.25 1 d . . P C 2
C8AA C 0.243(3) -0.222(4) -0.4215(15) 0.124(10) Uiso 0.15 1 d . . P C 2
C9AA C 0.311(3) -0.335(4) -0.3546(16) 0.123(10) Uiso 0.15 1 d . . P C 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
C0AA N1 1.369(2) . ?
C0AA C4AA 1.381(3) . ?
C0AA C6 1.441(3) . ?
C4AA C3 1.396(3) . ?
C4AA H4AA 0.9300 . ?
C3 C4 1.383(3) . ?
C3 H3 0.9300 . ?
C4 N1 1.368(2) . ?
C4 C5 1.440(3) . ?
C5 N3 1.274(2) . ?
C5 H5 0.9300 . ?
C6 N2 1.270(2) . ?
C6 H6 0.9300 . ?
C5AA N2 1.474(2) . ?
C5AA C8 1.510(3) . ?
C5AA C14 1.523(3) . ?
C5AA H5AA 0.9800 . ?
C8 C6AA 1.384(3) . ?
C8 C2AA 1.399(3) . ?
C6AA C10 1.390(3) . ?
C6AA H6AA 0.9300 . ?
C10 C1AA 1.382(4) . ?
C10 H10 0.9300 . ?
C1AA C12 1.381(4) . ?
C1AA H1AA 0.9300 . ?
C12 C2AA 1.386(3) . ?
C12 H12 0.9300 . ?
C2AA H2AA 0.9300 . ?
C14 C3AA 1.375(3) . ?
C14 C19 1.387(3) . ?
C3AA C16 1.394(3) . ?
C3AA H3AA 0.9300 . ?
C16 C17 1.370(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.357(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.385(4) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 N3 1.476(2) . ?
C20 C21 1.514(3) . ?
C20 C27 1.516(3) . ?
C20 H20 0.9800 . ?
C21 C22 1.386(3) . ?
C21 C26 1.390(3) . ?
C22 C23 1.383(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.395(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.362(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.383(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C32 1.374(3) . ?
C27 C28 1.382(3) . ?
C28 C29 1.372(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.364(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.368(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.382(4) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C1BB 1.439(8) . ?
C33 C34B 1.458(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34B O35B 1.428(6) . ?
C34B H34A 0.9700 . ?
C34B H34B 0.9700 . ?
O35B C36B 1.327(6) . ?
C36B C1BB 1.491(8) . ?
C36B H36A 0.9700 . ?
C36B H36B 0.9700 . ?
C1BB H1BA 0.9700 . ?
C1BB H1BB 0.9700 . ?
C37B C38A 1.473(13) . ?
C37B C38B 1.476(15) . ?
C37B H37A 0.9700 . ?
C37B H37B 0.9700 . ?
C38B C37A 1.416(14) . ?
C38B H38A 0.9700 . ?
C38B H38B 0.9700 . ?
N1 H1 0.8600 . ?
O2 C38A 1.344(11) . ?
O2 C37A 1.427(11) . ?
C38A H38C 0.9700 . ?
C38A H38D 0.9700 . ?
C37A H37C 0.9700 . ?
C37A H37D 0.9700 . ?
O1 C2 1.258(17) . ?
O1 C1 1.30(3) . ?
O1 C9AA 1.72(4) . ?
C2 C7AA 1.56(3) . ?
C7AA C8AA 1.62(4) . ?
C1 C9AA 1.44(4) . ?
C1 C8AA 1.83(4) . ?
C8AA C9AA 1.87(5) . ?

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
N1 C0AA C4AA 107.21(17) . . ?
N1 C0AA C6 123.18(17) . . ?
C4AA C0AA C6 129.59(18) . . ?
C0AA C4AA C3 108.01(18) . . ?
C0AA C4AA H4AA 126.0 . . ?
C3 C4AA H4AA 126.0 . . ?
C4 C3 C4AA 107.48(18) . . ?
C4 C3 H3 126.3 . . ?
C4AA C3 H3 126.3 . . ?
N1 C4 C3 107.47(17) . . ?
N1 C4 C5 124.24(17) . . ?
C3 C4 C5 128.29(18) . . ?
N3 C5 C4 123.54(18) . . ?
N3 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
N2 C6 C0AA 122.36(18) . . ?
N2 C6 H6 118.8 . . ?
C0AA C6 H6 118.8 . . ?
N2 C5AA C8 109.27(15) . . ?
N2 C5AA C14 108.76(16) . . ?
C8 C5AA C14 114.23(17) . . ?
N2 C5AA H5AA 108.1 . . ?
C8 C5AA H5AA 108.1 . . ?
C14 C5AA H5AA 108.1 . . ?
C6AA C8 C2AA 118.7(2) . . ?
C6AA C8 C5AA 120.3(2) . . ?
C2AA C8 C5AA 121.01(19) . . ?
C8 C6AA C10 120.9(2) . . ?
C8 C6AA H6AA 119.5 . . ?
C10 C6AA H6AA 119.5 . . ?
C1AA C10 C6AA 119.8(2) . . ?
C1AA C10 H10 120.1 . . ?
C6AA C10 H10 120.1 . . ?
C12 C1AA C10 120.1(2) . . ?
C12 C1AA H1AA 120.0 . . ?
C10 C1AA H1AA 120.0 . . ?
C1AA C12 C2AA 120.2(2) . . ?
C1AA C12 H12 119.9 . . ?
C2AA C12 H12 119.9 . . ?
C12 C2AA C8 120.3(2) . . ?
C12 C2AA H2AA 119.8 . . ?
C8 C2AA H2AA 119.8 . . ?
C3AA C14 C19 118.0(2) . . ?
C3AA C14 C5AA 122.3(2) . . ?
C19 C14 C5AA 119.6(2) . . ?
C14 C3AA C16 120.8(2) . . ?
C14 C3AA H3AA 119.6 . . ?
C16 C3AA H3AA 119.6 . . ?
C17 C16 C3AA 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C3AA C16 H16 119.9 . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 120.8(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C14 120.7(3) . . ?
C18 C19 H19 119.7 . . ?
C14 C19 H19 119.7 . . ?
N3 C20 C21 110.03(16) . . ?
N3 C20 C27 110.29(16) . . ?
C21 C20 C27 111.19(16) . . ?
N3 C20 H20 108.4 . . ?
C21 C20 H20 108.4 . . ?
C27 C20 H20 108.4 . . ?
C22 C21 C26 118.5(2) . . ?
C22 C21 C20 121.9(2) . . ?
C26 C21 C20 119.6(2) . . ?
C23 C22 C21 121.2(3) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C22 C23 C24 119.0(4) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
C25 C24 C23 120.3(3) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 120.5(3) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C32 C27 C28 118.2(2) . . ?
C32 C27 C20 119.5(2) . . ?
C28 C27 C20 122.24(19) . . ?
C29 C28 C27 121.1(2) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C30 C29 C28 120.2(2) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C31 119.7(3) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C32 120.2(3) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C27 C32 C31 120.6(3) . . ?
C27 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C1BB C33 C34B 105.9(5) . . ?
C1BB C33 H33A 110.5 . . ?
C34B C33 H33A 110.5 . . ?
C1BB C33 H33B 110.5 . . ?
C34B C33 H33B 110.5 . . ?
H33A C33 H33B 108.7 . . ?
O35B C34B C33 105.7(4) . . ?
O35B C34B H34A 110.6 . . ?
C33 C34B H34A 110.6 . . ?
O35B C34B H34B 110.6 . . ?
C33 C34B H34B 110.6 . . ?
H34A C34B H34B 108.7 . . ?
C36B O35B C34B 106.8(4) . . ?
O35B C36B C1BB 110.2(4) . . ?
O35B C36B H36A 109.6 . . ?
C1BB C36B H36A 109.6 . . ?
O35B C36B H36B 109.6 . . ?
C1BB C36B H36B 109.6 . . ?
H36A C36B H36B 108.1 . . ?
C33 C1BB C36B 103.8(5) . . ?
C33 C1BB H1BA 111.0 . . ?
C36B C1BB H1BA 111.0 . . ?
C33 C1BB H1BB 111.0 . . ?
C36B C1BB H1BB 111.0 . . ?
H1BA C1BB H1BB 109.0 . . ?
C38A C37B C38B 104.1(9) . . ?
C38A C37B H37A 110.9 . . ?
C38B C37B H37A 110.9 . . ?
C38A C37B H37B 110.9 . . ?
C38B C37B H37B 110.9 . . ?
H37A C37B H37B 109.0 . . ?
C37A C38B C37B 107.0(10) . . ?
C37A C38B H38A 110.3 . . ?
C37B C38B H38A 110.3 . . ?
C37A C38B H38B 110.3 . . ?
C37B C38B H38B 110.3 . . ?
H38A C38B H38B 108.6 . . ?
C4 N1 C0AA 109.82(16) . . ?
C4 N1 H1 125.1 . . ?
C0AA N1 H1 125.1 . . ?
C6 N2 C5AA 116.90(17) . . ?
C5 N3 C20 115.14(16) . . ?
C38A O2 C37A 108.5(10) . . ?
O2 C38A C37B 110.7(10) . . ?
O2 C38A H38C 109.5 . . ?
C37B C38A H38C 109.5 . . ?
O2 C38A H38D 109.5 . . ?
C37B C38A H38D 109.5 . . ?
H38C C38A H38D 108.1 . . ?
C38B C37A O2 109.3(11) . . ?
C38B C37A H37C 109.8 . . ?
O2 C37A H37C 109.8 . . ?
C38B C37A H37D 109.8 . . ?
O2 C37A H37D 109.8 . . ?
H37C C37A H37D 108.3 . . ?
C2 O1 C1 130.4(16) . . ?
C2 O1 C9AA 91.0(15) . . ?
C1 O1 C9AA 54.8(17) . . ?
O1 C2 C7AA 96.9(14) . . ?
C2 C7AA C8AA 118(2) . . ?
O1 C1 C9AA 78(2) . . ?
O1 C1 C8AA 105.3(18) . . ?
C9AA C1 C8AA 69(2) . . ?
C7AA C8AA C1 87(2) . . ?
C7AA C8AA C9AA 76(2) . . ?
C1 C8AA C9AA 45.7(16) . . ?
C1 C9AA O1 47.3(15) . . ?
C1 C9AA C8AA 66(2) . . ?
O1 C9AA C8AA 88.3(19) . . ?

_refine_diff_density_max         0.230
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.046



####################################################################### 
# 
# 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_1Na
_database_code_depnum_ccdc_archive 'CCDC 1476166'
_audit_update_record             
;
2016-08-02 deposited with the CCDC.
2016-08-18 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         'C68 H60 N6 Na2 O'
_chemical_formula_sum            'C68 H60 N6 Na2 O'
_chemical_formula_weight         1023.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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                   13.7972(6)
_cell_length_b                   14.1023(8)
_cell_length_c                   17.3629(8)
_cell_angle_alpha                66.499(5)
_cell_angle_beta                 88.058(4)
_cell_angle_gamma                64.994(5)
_cell_volume                     2770.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8548
_cell_measurement_theta_min      3.582
_cell_measurement_theta_max      71.262

_exptl_crystal_description       plates
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_F_000             1080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.706
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18989
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.582
_diffrn_reflns_theta_max         71.262
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10535
_reflns_number_gt                8400
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND & Olex 2.1'
_computing_publication_material  WinGX
_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)+(0.0610P)²+0.7555P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00257(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         10535
_refine_ls_number_parameters     695
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.1411
_refine_ls_wR_factor_gt          0.1310
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.15065(6) 0.62032(6) 0.26096(5) 0.03089(18) Uani 1 1 d . . . . .
Na2 Na 0.28942(6) 0.41673(6) 0.22681(5) 0.03336(18) Uani 1 1 d . . . . .
O1 O 0.14227(13) 0.68899(13) 0.36392(10) 0.0475(4) Uani 1 1 d . . . . .
N1 N 0.23015(12) 0.41727(12) 0.36192(10) 0.0275(3) Uani 1 1 d . . . . .
N2 N -0.00219(12) 0.57868(12) 0.29900(10) 0.0288(3) Uani 1 1 d . . . . .
N3 N 0.45076(12) 0.34456(13) 0.32296(10) 0.0302(3) Uani 1 1 d . . . . .
N4 N 0.16519(12) 0.59681(12) 0.11490(9) 0.0272(3) Uani 1 1 d . . . . .
N5 N 0.21974(13) 0.74359(13) 0.16554(10) 0.0292(3) Uani 1 1 d . . . . .
N6 N 0.17831(13) 0.36674(13) 0.16590(10) 0.0300(3) Uani 1 1 d . . . . .
C1 C 0.32213(15) 0.33487(15) 0.41921(12) 0.0299(4) Uani 1 1 d . . . . .
C2 C 0.29827(16) 0.28466(17) 0.50069(13) 0.0381(5) Uani 1 1 d . . . . .
H2 H 0.3476 0.2275 0.5497 0.046 Uiso 1 1 calc R U . . .
C3 C 0.18652(16) 0.33742(17) 0.49329(13) 0.0362(4) Uani 1 1 d . . . . .
H3 H 0.1456 0.3225 0.5362 0.043 Uiso 1 1 calc R U . . .
C4 C 0.14720(15) 0.41811(15) 0.40777(12) 0.0280(4) Uani 1 1 d . . . . .
C5 C 0.03453(15) 0.49899(15) 0.37482(12) 0.0284(4) Uani 1 1 d . . . . .
H5 H -0.0153 0.4926 0.4116 0.034 Uiso 1 1 calc R U . . .
C6 C 0.43022(15) 0.30293(15) 0.39841(12) 0.0313(4) Uani 1 1 d . . . . .
H6 H 0.4883 0.2490 0.4423 0.038 Uiso 1 1 calc R U . . .
C7 C -0.11873(14) 0.65754(15) 0.28021(12) 0.0294(4) Uani 1 1 d . . . . .
H7 H -0.1465 0.6460 0.3342 0.035 Uiso 1 1 calc R U . . .
C8 C -0.18147(15) 0.63367(15) 0.22573(12) 0.0312(4) Uani 1 1 d . . . . .
C9 C -0.14373(17) 0.61293(17) 0.15601(13) 0.0373(4) Uani 1 1 d . . . . .
H9 H -0.0768 0.6099 0.1432 0.045 Uiso 1 1 calc R U . . .
C10 C -0.2056(2) 0.5968(2) 0.10562(15) 0.0505(6) Uani 1 1 d . . . . .
H10 H -0.1799 0.5832 0.0590 0.061 Uiso 1 1 calc R U . . .
C11 C -0.3049(2) 0.6008(2) 0.12369(17) 0.0585(7) Uani 1 1 d . . . . .
H11 H -0.3465 0.5912 0.0890 0.070 Uiso 1 1 calc R U . . .
C12 C -0.3419(2) 0.6189(2) 0.19333(17) 0.0583(7) Uani 1 1 d . . . . .
H12 H -0.4081 0.6200 0.2066 0.070 Uiso 1 1 calc R U . . .
C13 C -0.28091(17) 0.6357(2) 0.24394(15) 0.0456(5) Uani 1 1 d . . . . .
H13 H -0.3069 0.6485 0.2908 0.055 Uiso 1 1 calc R U . . .
C14 C -0.13520(15) 0.78192(15) 0.23678(12) 0.0307(4) Uani 1 1 d . . . . .
C15 C -0.21510(19) 0.86532(18) 0.25607(15) 0.0478(6) Uani 1 1 d . . . . .
H15 H -0.2564 0.8443 0.2970 0.057 Uiso 1 1 calc R U . . .
C16 C -0.2346(2) 0.98005(19) 0.21514(17) 0.0600(7) Uani 1 1 d . . . . .
H16 H -0.2899 1.0356 0.2278 0.072 Uiso 1 1 calc R U . . .
C17 C -0.1722(2) 1.01247(18) 0.15551(15) 0.0488(6) Uani 1 1 d . . . . .
H17 H -0.1841 1.0891 0.1292 0.059 Uiso 1 1 calc R U . . .
C18 C -0.09223(17) 0.92978(17) 0.13554(14) 0.0395(5) Uani 1 1 d . . . . .
H18 H -0.0499 0.9507 0.0955 0.047 Uiso 1 1 calc R U . . .
C19 C -0.07483(15) 0.81562(16) 0.17499(12) 0.0328(4) Uani 1 1 d . . . . .
H19 H -0.0222 0.7609 0.1600 0.039 Uiso 1 1 calc R U . . .
C20 C 0.56431(15) 0.31143(16) 0.30847(12) 0.0316(4) Uani 1 1 d . . . . .
H20 H 0.5807 0.3734 0.3067 0.038 Uiso 1 1 calc R U . . .
C21 C 0.64805(15) 0.20032(16) 0.37871(13) 0.0322(4) Uani 1 1 d . . . . .
C22 C 0.67765(19) 0.09352(18) 0.37903(15) 0.0473(6) Uani 1 1 d . . . . .
H22 H 0.6470 0.0891 0.3344 0.057 Uiso 1 1 calc R U . . .
C23 C 0.7522(2) -0.0072(2) 0.44452(17) 0.0568(7) Uani 1 1 d . . . . .
H23 H 0.7712 -0.0780 0.4430 0.068 Uiso 1 1 calc R U . . .
C24 C 0.79818(18) -0.00354(19) 0.51184(15) 0.0473(5) Uani 1 1 d . . . . .
H24 H 0.8485 -0.0710 0.5555 0.057 Uiso 1 1 calc R U . . .
C25 C 0.76822(18) 0.1020(2) 0.51308(15) 0.0472(5) Uani 1 1 d . . . . .
H25 H 0.7977 0.1059 0.5585 0.057 Uiso 1 1 calc R U . . .
C26 C 0.69443(17) 0.20255(19) 0.44726(14) 0.0416(5) Uani 1 1 d . . . . .
H26 H 0.6756 0.2731 0.4490 0.050 Uiso 1 1 calc R U . . .
C27 C 0.57203(16) 0.31281(16) 0.22025(12) 0.0325(4) Uani 1 1 d . . . . .
C28 C 0.51196(17) 0.27647(17) 0.18619(13) 0.0365(4) Uani 1 1 d . . . . .
H28 H 0.4662 0.2491 0.2180 0.044 Uiso 1 1 calc R U . . .
C29 C 0.5197(2) 0.28071(19) 0.10465(14) 0.0464(5) Uani 1 1 d . . . . .
H29 H 0.4790 0.2564 0.0824 0.056 Uiso 1 1 calc R U . . .
C30 C 0.5876(2) 0.3208(2) 0.05697(16) 0.0533(6) Uani 1 1 d . . . . .
H30 H 0.5921 0.3243 0.0024 0.064 Uiso 1 1 calc R U . . .
C31 C 0.6485(2) 0.3558(2) 0.09042(16) 0.0520(6) Uani 1 1 d . . . . .
H31 H 0.6945 0.3824 0.0585 0.062 Uiso 1 1 calc R U . . .
C32 C 0.64133(18) 0.35128(18) 0.17174(14) 0.0422(5) Uani 1 1 d . . . . .
H32 H 0.6834 0.3743 0.1940 0.051 Uiso 1 1 calc R U . . .
C33 C 0.12037(14) 0.56509(15) 0.06580(12) 0.0278(4) Uani 1 1 d . . . . .
C34 C 0.07556(16) 0.65374(16) -0.01690(12) 0.0332(4) Uani 1 1 d . . . . .
H34 H 0.0405 0.6522 -0.0609 0.040 Uiso 1 1 calc R U . . .
C35 C 0.09442(16) 0.74374(16) -0.01931(12) 0.0325(4) Uani 1 1 d . . . . .
H35 H 0.0747 0.8148 -0.0655 0.039 Uiso 1 1 calc R U . . .
C36 C 0.14909(14) 0.70667(15) 0.06167(11) 0.0277(4) Uani 1 1 d . . . . .
C37 C 0.18457(15) 0.77359(15) 0.08800(12) 0.0285(4) Uani 1 1 d . . . . .
H37 H 0.1817 0.8419 0.0466 0.034 Uiso 1 1 calc R U . . .
C38 C 0.12632(14) 0.45130(15) 0.09420(12) 0.0284(4) Uani 1 1 d . . . . .
H38 H 0.0900 0.4386 0.0580 0.034 Uiso 1 1 calc R U . . .
C39 C 0.24893(15) 0.82025(15) 0.18723(12) 0.0293(4) Uani 1 1 d . . . . .
H39 H 0.1854 0.8659 0.2060 0.035 Uiso 1 1 calc R U . . .
C40 C 0.34009(15) 0.74990(16) 0.26324(12) 0.0298(4) Uani 1 1 d . . . . .
C41 C 0.40172(16) 0.63143(16) 0.29388(12) 0.0340(4) Uani 1 1 d . . . . .
H41 H 0.3890 0.5913 0.2671 0.041 Uiso 1 1 calc R U . . .
C42 C 0.48283(18) 0.57207(18) 0.36478(13) 0.0405(5) Uani 1 1 d . . . . .
H42 H 0.5228 0.4923 0.3855 0.049 Uiso 1 1 calc R U . . .
C43 C 0.50464(18) 0.62983(18) 0.40463(13) 0.0403(5) Uani 1 1 d . . . . .
H43 H 0.5594 0.5898 0.4514 0.048 Uiso 1 1 calc R U . . .
C44 C 0.44367(19) 0.74821(18) 0.37386(13) 0.0419(5) Uani 1 1 d . . . . .
H44 H 0.4574 0.7882 0.4001 0.050 Uiso 1 1 calc R U . . .
C45 C 0.36249(18) 0.80736(17) 0.30435(13) 0.0372(5) Uani 1 1 d . . . . .
H45 H 0.3220 0.8869 0.2845 0.045 Uiso 1 1 calc R U . . .
C46 C 0.27395(16) 0.90684(16) 0.11397(12) 0.0313(4) Uani 1 1 d . . . . .
C47 C 0.36992(18) 0.87256(19) 0.08245(14) 0.0411(5) Uani 1 1 d . . . . .
H47 H 0.4209 0.7953 0.1067 0.049 Uiso 1 1 calc R U . . .
C48 C 0.3910(2) 0.9526(2) 0.01464(15) 0.0505(6) Uani 1 1 d . . . . .
H48 H 0.4556 0.9287 -0.0066 0.061 Uiso 1 1 calc R U . . .
C49 C 0.3158(2) 1.0679(2) -0.02108(14) 0.0536(7) Uani 1 1 d . . . . .
H49 H 0.3302 1.1217 -0.0658 0.064 Uiso 1 1 calc R U . . .
C50 C 0.2202(2) 1.10244(19) 0.00960(14) 0.0489(6) Uani 1 1 d . . . . .
H50 H 0.1695 1.1798 -0.0146 0.059 Uiso 1 1 calc R U . . .
C51 C 0.19868(18) 1.02244(17) 0.07659(13) 0.0385(5) Uani 1 1 d . . . . .
H51 H 0.1333 1.0465 0.0966 0.046 Uiso 1 1 calc R U . . .
C52 C 0.17980(15) 0.25514(15) 0.18296(12) 0.0306(4) Uani 1 1 d . . . . .
H52 H 0.1684 0.2533 0.1282 0.037 Uiso 1 1 calc R U . . .
C53 C 0.09089(15) 0.23763(15) 0.23233(12) 0.0299(4) Uani 1 1 d . . . . .
C54 C 0.02381(18) 0.31468(18) 0.26318(14) 0.0408(5) Uani 1 1 d . . . . .
H54 H 0.0344 0.3783 0.2563 0.049 Uiso 1 1 calc R U . . .
C55 C -0.0596(2) 0.2977(2) 0.30448(16) 0.0546(6) Uani 1 1 d . . . . .
H55 H -0.1048 0.3504 0.3247 0.066 Uiso 1 1 calc R U . . .
C56 C -0.07584(19) 0.2035(2) 0.31565(16) 0.0531(6) Uani 1 1 d . . . . .
H56 H -0.1316 0.1925 0.3434 0.064 Uiso 1 1 calc R U . . .
C57 C -0.00904(19) 0.1256(2) 0.28560(16) 0.0483(6) Uani 1 1 d . . . . .
H57 H -0.0198 0.0620 0.2929 0.058 Uiso 1 1 calc R U . . .
C58 C 0.07424(17) 0.14223(18) 0.24445(14) 0.0391(5) Uani 1 1 d . . . . .
H58 H 0.1195 0.0890 0.2247 0.047 Uiso 1 1 calc R U . . .
C59 C 0.29190(16) 0.16114(16) 0.22941(13) 0.0352(4) Uani 1 1 d . . . . .
C60 C 0.32472(19) 0.1374(2) 0.31259(15) 0.0490(6) Uani 1 1 d . . . . .
H60 H 0.2768 0.1762 0.3409 0.059 Uiso 1 1 calc R U . . .
C61 C 0.4300(2) 0.0549(2) 0.35342(17) 0.0641(8) Uani 1 1 d . . . . .
H61 H 0.4526 0.0384 0.4091 0.077 Uiso 1 1 calc R U . . .
C62 C 0.5005(2) -0.0022(2) 0.3103(2) 0.0643(8) Uani 1 1 d . . . . .
H62 H 0.5707 -0.0570 0.3375 0.077 Uiso 1 1 calc R U . . .
C63 C 0.4687(2) 0.0208(2) 0.2285(2) 0.0581(7) Uani 1 1 d . . . . .
H63 H 0.5169 -0.0179 0.2003 0.070 Uiso 1 1 calc R U . . .
C64 C 0.36463(18) 0.10183(18) 0.18825(17) 0.0465(6) Uani 1 1 d . . . . .
H64 H 0.3427 0.1171 0.1328 0.056 Uiso 1 1 calc R U . . .
C65 C 0.2217(2) 0.6213(2) 0.43991(14) 0.0462(5) Uani 1 1 d . . . . .
H65A H 0.2765 0.6484 0.4351 0.055 Uiso 1 1 calc R U . . .
H65B H 0.2568 0.5406 0.4500 0.055 Uiso 1 1 calc R U . . .
C66 C 0.1614(2) 0.6358(3) 0.51071(17) 0.0654(8) Uani 1 1 d . . . . .
H66A H 0.2049 0.6370 0.5527 0.078 Uiso 1 1 calc R U . . .
H66B H 0.1407 0.5740 0.5385 0.078 Uiso 1 1 calc R U . . .
C67 C 0.0619(3) 0.7519(3) 0.4665(2) 0.0755(9) Uani 1 1 d . . . . .
H67A H 0.0625 0.8074 0.4858 0.091 Uiso 1 1 calc R U . . .
H67B H -0.0042 0.7437 0.4772 0.091 Uiso 1 1 calc R U . . .
C68 C 0.0713(2) 0.7897(2) 0.3717(2) 0.0725(9) Uani 1 1 d . . . . .
H68A H 0.0009 0.8238 0.3376 0.087 Uiso 1 1 calc R U . . .
H68B H 0.0998 0.8460 0.3531 0.087 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O1 2.3278(17) . ?
Na1 N5 2.3817(16) . ?
Na1 N2 2.4229(17) . ?
Na1 N1 2.4387(16) . ?
Na1 N4 2.6761(17) . ?
Na1 C5 2.9677(19) . ?
Na1 Na2 2.9823(11) . ?
Na1 C4 2.9901(18) . ?
Na1 C19 3.047(2) . ?
Na1 C37 3.0810(19) . ?
Na2 N6 2.3630(18) . ?
Na2 N3 2.3999(17) . ?
Na2 N4 2.4026(16) . ?
Na2 N1 2.4598(17) . ?
Na2 C38 3.022(2) . ?
Na2 C6 3.028(2) . ?
Na2 C1 3.047(2) . ?
Na2 C33 3.047(2) . ?
Na2 C28 3.109(2) . ?
O1 C68 1.401(3) . ?
O1 C65 1.436(3) . ?
N1 C1 1.366(2) . ?
N1 C4 1.370(2) . ?
N2 C5 1.279(2) . ?
N2 C7 1.471(2) . ?
N3 C6 1.282(2) . ?
N3 C20 1.478(2) . ?
N4 C33 1.372(2) . ?
N4 C36 1.373(2) . ?
N5 C37 1.282(2) . ?
N5 C39 1.475(2) . ?
N6 C38 1.281(2) . ?
N6 C52 1.472(2) . ?
C1 C2 1.406(3) . ?
C1 C6 1.443(3) . ?
C2 C3 1.384(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.407(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.444(2) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.521(3) . ?
C7 C14 1.522(2) . ?
C7 H7 0.9800 . ?
C8 C13 1.389(3) . ?
C8 C9 1.390(3) . ?
C9 C10 1.386(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.378(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.372(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.386(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.380(3) . ?
C14 C19 1.392(3) . ?
C15 C16 1.387(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.384(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.381(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(3) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.523(3) . ?
C20 C27 1.525(3) . ?
C20 H20 0.9800 . ?
C21 C22 1.381(3) . ?
C21 C26 1.388(3) . ?
C22 C23 1.387(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.378(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.375(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.385(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.390(3) . ?
C27 C32 1.392(3) . ?
C28 C29 1.395(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.380(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.377(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.390(3) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.408(3) . ?
C33 C38 1.444(2) . ?
C34 C35 1.384(3) . ?
C34 H34 0.9300 . ?
C35 C36 1.404(3) . ?
C35 H35 0.9300 . ?
C36 C37 1.445(3) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C46 1.522(2) . ?
C39 C40 1.524(3) . ?
C39 H39 0.9800 . ?
C40 C41 1.385(3) . ?
C40 C45 1.396(3) . ?
C41 C42 1.396(3) . ?
C41 H41 0.9300 . ?
C42 C43 1.380(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.383(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.380(3) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C46 C47 1.381(3) . ?
C46 C51 1.388(3) . ?
C47 C48 1.393(3) . ?
C47 H47 0.9300 . ?
C48 C49 1.384(4) . ?
C48 H48 0.9300 . ?
C49 C50 1.371(4) . ?
C49 H49 0.9300 . ?
C50 C51 1.388(3) . ?
C50 H50 0.9300 . ?
C51 H51 0.9300 . ?
C52 C59 1.516(3) . ?
C52 C53 1.522(3) . ?
C52 H52 0.9800 . ?
C53 C54 1.380(3) . ?
C53 C58 1.393(3) . ?
C54 C55 1.392(3) . ?
C54 H54 0.9300 . ?
C55 C56 1.376(3) . ?
C55 H55 0.9300 . ?
C56 C57 1.377(3) . ?
C56 H56 0.9300 . ?
C57 C58 1.387(3) . ?
C57 H57 0.9300 . ?
C58 H58 0.9300 . ?
C59 C60 1.390(3) . ?
C59 C64 1.391(3) . ?
C60 C61 1.396(3) . ?
C60 H60 0.9300 . ?
C61 C62 1.387(4) . ?
C61 H61 0.9300 . ?
C62 C63 1.367(4) . ?
C62 H62 0.9300 . ?
C63 C64 1.378(3) . ?
C63 H63 0.9300 . ?
C64 H64 0.9300 . ?
C65 C66 1.494(3) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C66 C67 1.524(4) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C67 C68 1.534(4) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Na1 N5 94.34(6) . . ?
O1 Na1 N2 92.77(6) . . ?
N5 Na1 N2 148.60(6) . . ?
O1 Na1 N1 94.87(6) . . ?
N5 Na1 N1 134.65(6) . . ?
N2 Na1 N1 74.88(5) . . ?
O1 Na1 N4 163.50(6) . . ?
N5 Na1 N4 69.82(5) . . ?
N2 Na1 N4 98.56(6) . . ?
N1 Na1 N4 99.62(5) . . ?
O1 Na1 C5 82.27(6) . . ?
N5 Na1 C5 171.41(6) . . ?
N2 Na1 C5 24.93(5) . . ?
N1 Na1 C5 53.76(5) . . ?
N4 Na1 C5 112.72(5) . . ?
O1 Na1 Na2 139.70(5) . . ?
N5 Na1 Na2 94.64(5) . . ?
N2 Na1 Na2 99.49(5) . . ?
N1 Na1 Na2 52.82(4) . . ?
N4 Na1 Na2 49.89(4) . . ?
C5 Na1 Na2 93.02(4) . . ?
O1 Na1 C4 82.91(6) . . ?
N5 Na1 C4 159.57(6) . . ?
N2 Na1 C4 51.79(5) . . ?
N1 Na1 C4 26.87(5) . . ?
N4 Na1 C4 113.54(5) . . ?
C5 Na1 C4 28.05(5) . . ?
Na2 Na1 C4 75.34(4) . . ?
O1 Na1 C19 88.75(6) . . ?
N5 Na1 C19 86.91(6) . . ?
N2 Na1 C19 62.70(5) . . ?
N1 Na1 C19 137.56(6) . . ?
N4 Na1 C19 85.87(5) . . ?
C5 Na1 C19 85.13(5) . . ?
Na2 Na1 C19 130.91(5) . . ?
C4 Na1 C19 113.17(6) . . ?
O1 Na1 C37 113.17(6) . . ?
N5 Na1 C37 22.88(5) . . ?
N2 Na1 C37 129.86(6) . . ?
N1 Na1 C37 138.74(6) . . ?
N4 Na1 C37 50.35(5) . . ?
C5 Na1 C37 154.31(6) . . ?
Na2 Na1 C37 87.66(4) . . ?
C4 Na1 C37 162.60(6) . . ?
C19 Na1 C37 75.25(5) . . ?
N6 Na2 N3 145.45(6) . . ?
N6 Na2 N4 75.78(6) . . ?
N3 Na2 N4 137.94(6) . . ?
N6 Na2 N1 107.51(6) . . ?
N3 Na2 N1 73.96(6) . . ?
N4 Na2 N1 107.06(6) . . ?
N6 Na2 Na1 109.44(5) . . ?
N3 Na2 Na1 98.53(5) . . ?
N4 Na2 Na1 58.42(4) . . ?
N1 Na2 Na1 52.18(4) . . ?
N6 Na2 C38 23.71(5) . . ?
N3 Na2 C38 163.81(6) . . ?
N4 Na2 C38 52.97(5) . . ?
N1 Na2 C38 117.21(6) . . ?
Na1 Na2 C38 97.65(4) . . ?
N6 Na2 C6 133.46(6) . . ?
N3 Na2 C6 23.92(5) . . ?
N4 Na2 C6 145.37(6) . . ?
N1 Na2 C6 52.55(5) . . ?
Na1 Na2 C6 90.17(4) . . ?
C38 Na2 C6 156.84(6) . . ?
N6 Na2 C1 118.54(6) . . ?
N3 Na2 C1 50.72(5) . . ?
N4 Na2 C1 131.20(6) . . ?
N1 Na2 C1 26.05(5) . . ?
Na1 Na2 C1 73.19(4) . . ?
C38 Na2 C1 136.33(6) . . ?
C6 Na2 C1 27.48(5) . . ?
N6 Na2 C33 51.02(5) . . ?
N3 Na2 C33 159.11(6) . . ?
N4 Na2 C33 25.88(5) . . ?
N1 Na2 C33 118.06(6) . . ?
Na1 Na2 C33 79.09(4) . . ?
C38 Na2 C33 27.53(5) . . ?
C6 Na2 C33 169.17(6) . . ?
C1 Na2 C33 143.92(6) . . ?
N6 Na2 C28 99.72(6) . . ?
N3 Na2 C28 61.34(6) . . ?
N4 Na2 C28 118.19(6) . . ?
N1 Na2 C28 131.57(6) . . ?
Na1 Na2 C28 147.45(5) . . ?
C38 Na2 C28 103.81(6) . . ?
C6 Na2 C28 79.63(6) . . ?
C1 Na2 C28 105.53(6) . . ?
C33 Na2 C28 110.26(6) . . ?
C68 O1 C65 105.63(18) . . ?
C68 O1 Na1 133.95(15) . . ?
C65 O1 Na1 120.42(13) . . ?
C1 N1 C4 104.67(15) . . ?
C1 N1 Na1 139.99(12) . . ?
C4 N1 Na1 99.61(10) . . ?
C1 N1 Na2 101.71(11) . . ?
C4 N1 Na2 143.11(13) . . ?
Na1 N1 Na2 75.01(5) . . ?
C5 N2 C7 116.49(15) . . ?
C5 N2 Na1 102.11(12) . . ?
C7 N2 Na1 129.91(11) . . ?
C6 N3 C20 119.94(16) . . ?
C6 N3 Na2 106.68(13) . . ?
C20 N3 Na2 130.21(12) . . ?
C33 N4 C36 104.34(15) . . ?
C33 N4 Na2 104.30(11) . . ?
C36 N4 Na2 144.40(12) . . ?
C33 N4 Na1 140.84(12) . . ?
C36 N4 Na1 98.08(11) . . ?
Na2 N4 Na1 71.69(5) . . ?
C37 N5 C39 119.67(15) . . ?
C37 N5 Na1 110.89(12) . . ?
C39 N5 Na1 122.88(11) . . ?
C38 N6 C52 117.09(16) . . ?
C38 N6 Na2 108.38(12) . . ?
C52 N6 Na2 132.35(12) . . ?
N1 C1 C2 111.61(17) . . ?
N1 C1 C6 124.11(17) . . ?
C2 C1 C6 124.28(17) . . ?
N1 C1 Na2 52.24(9) . . ?
C2 C1 Na2 152.79(14) . . ?
C6 C1 Na2 75.54(11) . . ?
C3 C2 C1 106.12(17) . . ?
C3 C2 H2 126.9 . . ?
C1 C2 H2 126.9 . . ?
C2 C3 C4 106.19(17) . . ?
C2 C3 H3 126.9 . . ?
C4 C3 H3 126.9 . . ?
N1 C4 C3 111.41(16) . . ?
N1 C4 C5 124.37(16) . . ?
C3 C4 C5 123.97(17) . . ?
N1 C4 Na1 53.53(8) . . ?
C3 C4 Na1 148.12(14) . . ?
C5 C4 Na1 75.11(10) . . ?
N2 C5 C4 125.16(17) . . ?
N2 C5 Na1 52.97(10) . . ?
C4 C5 Na1 76.84(10) . . ?
N2 C5 H5 117.4 . . ?
C4 C5 H5 117.4 . . ?
Na1 C5 H5 154.3 . . ?
N3 C6 C1 123.79(17) . . ?
N3 C6 Na2 49.39(10) . . ?
C1 C6 Na2 76.98(11) . . ?
N3 C6 H6 118.1 . . ?
C1 C6 H6 118.1 . . ?
Na2 C6 H6 158.4 . . ?
N2 C7 C8 111.88(15) . . ?
N2 C7 C14 109.42(15) . . ?
C8 C7 C14 110.77(15) . . ?
N2 C7 H7 108.2 . . ?
C8 C7 H7 108.2 . . ?
C14 C7 H7 108.2 . . ?
C13 C8 C9 118.4(2) . . ?
C13 C8 C7 119.67(19) . . ?
C9 C8 C7 121.90(17) . . ?
C10 C9 C8 120.2(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 120.8(2) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 119.5(2) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 120.2(2) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C8 120.9(2) . . ?
C12 C13 H13 119.5 . . ?
C8 C13 H13 119.5 . . ?
C15 C14 C19 118.49(18) . . ?
C15 C14 C7 119.58(18) . . ?
C19 C14 C7 121.87(16) . . ?
C14 C15 C16 120.8(2) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 119.3(2) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 120.2(2) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C14 120.83(18) . . ?
C18 C19 Na1 121.06(14) . . ?
C14 C19 Na1 99.86(12) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
Na1 C19 H19 45.9 . . ?
N3 C20 C21 115.09(15) . . ?
N3 C20 C27 109.07(15) . . ?
C21 C20 C27 113.49(15) . . ?
N3 C20 H20 106.2 . . ?
C21 C20 H20 106.2 . . ?
C27 C20 H20 106.2 . . ?
C22 C21 C26 117.31(19) . . ?
C22 C21 C20 121.97(18) . . ?
C26 C21 C20 120.67(18) . . ?
C21 C22 C23 121.3(2) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C24 C23 C22 120.7(2) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C25 C24 C23 118.7(2) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C24 C25 C26 120.5(2) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 121.5(2) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?
C28 C27 C32 118.4(2) . . ?
C28 C27 C20 122.12(17) . . ?
C32 C27 C20 119.47(18) . . ?
C27 C28 C29 120.6(2) . . ?
C27 C28 Na2 96.87(12) . . ?
C29 C28 Na2 119.65(15) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
Na2 C28 H28 51.7 . . ?
C30 C29 C28 120.2(2) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 119.8(2) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 120.2(2) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C27 120.8(2) . . ?
C31 C32 H32 119.6 . . ?
C27 C32 H32 119.6 . . ?
N4 C33 C34 111.77(16) . . ?
N4 C33 C38 123.56(16) . . ?
C34 C33 C38 124.51(17) . . ?
N4 C33 Na2 49.83(9) . . ?
C34 C33 Na2 154.53(13) . . ?
C38 C33 Na2 75.27(10) . . ?
C35 C34 C33 105.86(17) . . ?
C35 C34 H34 127.1 . . ?
C33 C34 H34 127.1 . . ?
C34 C35 C36 106.52(16) . . ?
C34 C35 H35 126.7 . . ?
C36 C35 H35 126.7 . . ?
N4 C36 C35 111.51(16) . . ?
N4 C36 C37 122.93(16) . . ?
C35 C36 C37 125.56(16) . . ?
N5 C37 C36 123.37(16) . . ?
N5 C37 Na1 46.24(9) . . ?
C36 C37 Na1 80.29(10) . . ?
N5 C37 H37 118.3 . . ?
C36 C37 H37 118.3 . . ?
Na1 C37 H37 155.1 . . ?
N6 C38 C33 124.32(17) . . ?
N6 C38 Na2 47.91(10) . . ?
C33 C38 Na2 77.21(11) . . ?
N6 C38 H38 117.8 . . ?
C33 C38 H38 117.8 . . ?
Na2 C38 H38 162.7 . . ?
N5 C39 C46 115.54(15) . . ?
N5 C39 C40 110.61(14) . . ?
C46 C39 C40 111.36(15) . . ?
N5 C39 H39 106.2 . . ?
C46 C39 H39 106.2 . . ?
C40 C39 H39 106.2 . . ?
C41 C40 C45 118.27(18) . . ?
C41 C40 C39 123.19(17) . . ?
C45 C40 C39 118.54(17) . . ?
C40 C41 C42 120.17(19) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C43 C42 C41 121.05(19) . . ?
C43 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C42 C43 C44 118.9(2) . . ?
C42 C43 H43 120.6 . . ?
C44 C43 H43 120.6 . . ?
C45 C44 C43 120.4(2) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C40 121.21(19) . . ?
C44 C45 H45 119.4 . . ?
C40 C45 H45 119.4 . . ?
C47 C46 C51 118.80(18) . . ?
C47 C46 C39 121.27(17) . . ?
C51 C46 C39 119.92(19) . . ?
C46 C47 C48 120.6(2) . . ?
C46 C47 H47 119.7 . . ?
C48 C47 H47 119.7 . . ?
C49 C48 C47 119.9(2) . . ?
C49 C48 H48 120.1 . . ?
C47 C48 H48 120.1 . . ?
C50 C49 C48 119.9(2) . . ?
C50 C49 H49 120.1 . . ?
C48 C49 H49 120.1 . . ?
C49 C50 C51 120.2(2) . . ?
C49 C50 H50 119.9 . . ?
C51 C50 H50 119.9 . . ?
C50 C51 C46 120.6(2) . . ?
C50 C51 H51 119.7 . . ?
C46 C51 H51 119.7 . . ?
N6 C52 C59 107.47(15) . . ?
N6 C52 C53 112.36(15) . . ?
C59 C52 C53 112.25(16) . . ?
N6 C52 H52 108.2 . . ?
C59 C52 H52 108.2 . . ?
C53 C52 H52 108.2 . . ?
C54 C53 C58 118.69(19) . . ?
C54 C53 C52 122.51(17) . . ?
C58 C53 C52 118.77(17) . . ?
C53 C54 C55 120.4(2) . . ?
C53 C54 H54 119.8 . . ?
C55 C54 H54 119.8 . . ?
C56 C55 C54 120.5(2) . . ?
C56 C55 H55 119.8 . . ?
C54 C55 H55 119.8 . . ?
C55 C56 C57 119.7(2) . . ?
C55 C56 H56 120.1 . . ?
C57 C56 H56 120.1 . . ?
C56 C57 C58 120.0(2) . . ?
C56 C57 H57 120.0 . . ?
C58 C57 H57 120.0 . . ?
C57 C58 C53 120.8(2) . . ?
C57 C58 H58 119.6 . . ?
C53 C58 H58 119.6 . . ?
C60 C59 C64 119.3(2) . . ?
C60 C59 C52 119.99(19) . . ?
C64 C59 C52 120.6(2) . . ?
C59 C60 C61 119.7(3) . . ?
C59 C60 H60 120.2 . . ?
C61 C60 H60 120.2 . . ?
C62 C61 C60 119.5(3) . . ?
C62 C61 H61 120.3 . . ?
C60 C61 H61 120.3 . . ?
C63 C62 C61 121.1(2) . . ?
C63 C62 H62 119.4 . . ?
C61 C62 H62 119.4 . . ?
C62 C63 C64 119.5(3) . . ?
C62 C63 H63 120.3 . . ?
C64 C63 H63 120.3 . . ?
C63 C64 C59 120.9(3) . . ?
C63 C64 H64 119.5 . . ?
C59 C64 H64 119.5 . . ?
O1 C65 C66 106.1(2) . . ?
O1 C65 H65A 110.5 . . ?
C66 C65 H65A 110.5 . . ?
O1 C65 H65B 110.5 . . ?
C66 C65 H65B 110.5 . . ?
H65A C65 H65B 108.7 . . ?
C65 C66 C67 103.8(2) . . ?
C65 C66 H66A 111.0 . . ?
C67 C66 H66A 111.0 . . ?
C65 C66 H66B 111.0 . . ?
C67 C66 H66B 111.0 . . ?
H66A C66 H66B 109.0 . . ?
C66 C67 C68 104.3(2) . . ?
C66 C67 H67A 110.9 . . ?
C68 C67 H67A 110.9 . . ?
C66 C67 H67B 110.9 . . ?
C68 C67 H67B 110.9 . . ?
H67A C67 H67B 108.9 . . ?
O1 C68 C67 105.7(2) . . ?
O1 C68 H68A 110.6 . . ?
C67 C68 H68A 110.6 . . ?
O1 C68 H68B 110.6 . . ?
C67 C68 H68B 110.6 . . ?
H68A C68 H68B 108.7 . . ?

_refine_diff_density_max         0.394
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.049



####################################################################### 
# 
# 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_1-K
_database_code_depnum_ccdc_archive 'CCDC 1476167'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-08-18 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         'C32 H26 N3, 2(C4 H8 O), K '
_chemical_formula_sum            'C40 H42 K N3 O2'
_chemical_formula_weight         635.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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      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                   13.6800(5)
_cell_length_b                   16.1870(3)
_cell_length_c                   16.4227(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.696(4)
_cell_angle_gamma                90
_cell_volume                     3444.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4406
_cell_measurement_theta_min      4.371
_cell_measurement_theta_max      71.054

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.643
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68215
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7159
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.371
_diffrn_reflns_theta_max         71.054
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3263
_reflns_number_gt                2981
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND & Olex 2.1'
_computing_publication_material  WinGX
_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)+(0.0674P)²+1.1978P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00162(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3263
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1162
_refine_ls_wR_factor_gt          0.1123
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
K1 K 0.5000 0.18334(3) 0.7500 0.04582(18) Uani 1 2 d S T P . .
O1 O 0.35717(11) 0.07256(8) 0.66670(10) 0.0680(4) Uani 1 1 d . . . . .
N1 N 0.5000 0.34628(10) 0.7500 0.0311(3) Uani 1 2 d S T P . .
N2 N 0.51259(9) 0.28204(7) 0.59652(7) 0.0323(3) Uani 1 1 d . . . . .
C1 C 0.50954(9) 0.39650(8) 0.68707(8) 0.0296(3) Uani 1 1 d . . . . .
C2 C 0.50698(10) 0.48050(8) 0.70992(9) 0.0343(3) Uani 1 1 d . . . . .
H2 H 0.5133 0.5264 0.6779 0.041 Uiso 1 1 calc R U . . .
C3 C 0.52254(9) 0.35996(8) 0.61074(8) 0.0306(3) Uani 1 1 d . . . . .
H3 H 0.5385 0.3939 0.5710 0.037 Uiso 1 1 calc R U . . .
C4 C 0.53892(10) 0.24949(9) 0.52264(9) 0.0321(3) Uani 1 1 d . . . . .
H4 H 0.5770 0.2920 0.5028 0.039 Uiso 1 1 calc R U . . .
C5 C 0.61052(11) 0.17617(9) 0.55658(9) 0.0327(3) Uani 1 1 d . . . . .
C6 C 0.71688(12) 0.18827(9) 0.58714(11) 0.0408(4) Uani 1 1 d . . . . .
H6 H 0.7440 0.2401 0.5824 0.049 Uiso 1 1 calc R U . . .
C7 C 0.78288(12) 0.12374(11) 0.62456(11) 0.0476(4) Uani 1 1 d . . . . .
H7 H 0.8537 0.1328 0.6447 0.057 Uiso 1 1 calc R U . . .
C8 C 0.74434(12) 0.04631(10) 0.63221(10) 0.0421(4) Uani 1 1 d . . . . .
H8 H 0.7888 0.0032 0.6573 0.050 Uiso 1 1 calc R U . . .
C9 C 0.63868(12) 0.03364(10) 0.60211(11) 0.0436(4) Uani 1 1 d . . . . .
H9 H 0.6119 -0.0182 0.6071 0.052 Uiso 1 1 calc R U . . .
C10 C 0.57240(11) 0.09813(10) 0.56451(10) 0.0412(4) Uani 1 1 d . . . . .
H10 H 0.5016 0.0889 0.5444 0.049 Uiso 1 1 calc R U . . .
C11 C 0.44357(10) 0.22611(8) 0.44861(9) 0.0317(3) Uani 1 1 d . . . . .
C12 C 0.44846(12) 0.22656(10) 0.36527(10) 0.0402(4) Uani 1 1 d . . . . .
H12 H 0.5098 0.2411 0.3559 0.048 Uiso 1 1 calc R U . . .
C13 C 0.36302(13) 0.20559(11) 0.29602(10) 0.0444(4) Uani 1 1 d . . . . .
H13 H 0.3675 0.2061 0.2407 0.053 Uiso 1 1 calc R U . . .
C14 C 0.27101(12) 0.18388(9) 0.30865(10) 0.0406(4) Uani 1 1 d . . . . .
H14 H 0.2135 0.1705 0.2621 0.049 Uiso 1 1 calc R U . . .
C15 C 0.26571(11) 0.18234(9) 0.39133(10) 0.0386(3) Uani 1 1 d . . . . .
H15 H 0.2044 0.1672 0.4004 0.046 Uiso 1 1 calc R U . . .
C16 C 0.35112(11) 0.20321(9) 0.46095(10) 0.0351(3) Uani 1 1 d . . . . .
H16 H 0.3466 0.2019 0.5162 0.042 Uiso 1 1 calc R U . . .
C021 C 0.26911(15) -0.04814(11) 0.60389(13) 0.0551(4) Uani 1 1 d . . . . .
H02A H 0.2382 -0.0803 0.6391 0.066 Uiso 1 1 calc R U . . .
H02B H 0.2763 -0.0828 0.5580 0.066 Uiso 1 1 calc R U . . .
C022 C 0.37087(14) -0.01378(12) 0.65662(15) 0.0617(5) Uani 1 1 d . . . . .
H02C H 0.3943 -0.0406 0.7123 0.074 Uiso 1 1 calc R U . . .
H02D H 0.4219 -0.0228 0.6280 0.074 Uiso 1 1 calc R U . . .
C023 C 0.20480(15) 0.02813(12) 0.56794(13) 0.0569(5) Uani 1 1 d . . . . .
H02E H 0.2133 0.0455 0.5141 0.068 Uiso 1 1 calc R U . . .
H02F H 0.1322 0.0186 0.5593 0.068 Uiso 1 1 calc R U . . .
C024 C 0.24912(17) 0.08934(13) 0.63712(14) 0.0630(5) Uani 1 1 d . . . . .
H02G H 0.2358 0.1452 0.6150 0.076 Uiso 1 1 calc R U . . .
H02H H 0.2199 0.0826 0.6833 0.076 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
K1 N1 2.6376(16) . ?
K1 O1 2.6816(13) 2_656 ?
K1 O1 2.6816(13) . ?
K1 N2 3.0354(12) . ?
K1 N2 3.0355(12) 2_656 ?
O1 C024 1.426(2) . ?
O1 C022 1.427(2) . ?
N1 C1 1.3536(16) 2_656 ?
N1 C1 1.3536(16) . ?
N2 C3 1.2821(18) . ?
N2 C4 1.4696(17) . ?
C1 C2 1.4141(19) . ?
C1 C3 1.4476(18) . ?
C2 C2 1.389(3) 2_656 ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C11 1.5185(19) . ?
C4 C5 1.5261(19) . ?
C4 H4 0.9800 . ?
C5 C10 1.389(2) . ?
C5 C6 1.393(2) . ?
C6 C7 1.389(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.381(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.385(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.391(2) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.392(2) . ?
C11 C16 1.3936(19) . ?
C12 C13 1.387(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.385(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.383(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.389(2) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C021 C022 1.491(3) . ?
C021 C023 1.521(3) . ?
C021 H02A 0.9700 . ?
C021 H02B 0.9700 . ?
C022 H02C 0.9700 . ?
C022 H02D 0.9700 . ?
C023 C024 1.483(3) . ?
C023 H02E 0.9700 . ?
C023 H02F 0.9700 . ?
C024 H02G 0.9700 . ?
C024 H02H 0.9700 . ?

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
N1 K1 O1 131.96(3) . 2_656 ?
N1 K1 O1 131.97(3) . . ?
O1 K1 O1 96.07(7) 2_656 . ?
N1 K1 N2 58.24(2) . . ?
O1 K1 N2 123.33(4) 2_656 . ?
O1 K1 N2 98.88(4) . . ?
N1 K1 N2 58.24(2) . 2_656 ?
O1 K1 N2 98.88(4) 2_656 2_656 ?
O1 K1 N2 123.34(4) . 2_656 ?
N2 K1 N2 116.48(5) . 2_656 ?
C024 O1 C022 107.90(14) . . ?
C024 O1 K1 123.54(12) . . ?
C022 O1 K1 127.79(12) . . ?
C1 N1 C1 106.19(16) 2_656 . ?
C1 N1 K1 126.91(8) 2_656 . ?
C1 N1 K1 126.90(8) . . ?
C3 N2 C4 117.60(11) . . ?
C3 N2 K1 113.43(8) . . ?
C4 N2 K1 126.23(8) . . ?
N1 C1 C2 110.98(12) . . ?
N1 C1 C3 118.98(12) . . ?
C2 C1 C3 130.02(12) . . ?
C2 C2 C1 105.91(8) 2_656 . ?
C2 C2 H2 127.0 2_656 . ?
C1 C2 H2 127.0 . . ?
N2 C3 C1 121.62(12) . . ?
N2 C3 H3 119.2 . . ?
C1 C3 H3 119.2 . . ?
N2 C4 C11 112.05(11) . . ?
N2 C4 C5 106.00(11) . . ?
C11 C4 C5 112.62(11) . . ?
N2 C4 H4 108.7 . . ?
C11 C4 H4 108.7 . . ?
C5 C4 H4 108.7 . . ?
C10 C5 C6 118.33(13) . . ?
C10 C5 C4 121.70(12) . . ?
C6 C5 C4 119.76(12) . . ?
C7 C6 C5 120.64(14) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C8 C7 C6 120.67(14) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 119.15(14) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C8 C9 C10 120.31(15) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C5 C10 C9 120.89(14) . . ?
C5 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C16 118.44(13) . . ?
C12 C11 C4 119.10(12) . . ?
C16 C11 C4 122.45(12) . . ?
C13 C12 C11 120.79(13) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C12 120.46(14) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 119.19(14) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 120.58(14) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C11 120.54(14) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
C022 C021 C023 103.82(15) . . ?
C022 C021 H02A 111.0 . . ?
C023 C021 H02A 111.0 . . ?
C022 C021 H02B 111.0 . . ?
C023 C021 H02B 111.0 . . ?
H02A C021 H02B 109.0 . . ?
O1 C022 C021 107.44(16) . . ?
O1 C022 H02C 110.2 . . ?
C021 C022 H02C 110.2 . . ?
O1 C022 H02D 110.2 . . ?
C021 C022 H02D 110.2 . . ?
H02C C022 H02D 108.5 . . ?
C024 C023 C021 101.61(16) . . ?
C024 C023 H02E 111.4 . . ?
C021 C023 H02E 111.4 . . ?
C024 C023 H02F 111.4 . . ?
C021 C023 H02F 111.4 . . ?
H02E C023 H02F 109.3 . . ?
O1 C024 C023 104.96(15) . . ?
O1 C024 H02G 110.8 . . ?
C023 C024 H02G 110.8 . . ?
O1 C024 H02H 110.8 . . ?
C023 C024 H02H 110.8 . . ?
H02G C024 H02H 108.8 . . ?

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 N1 C1 C2 0.48(7) 2_656 . . . ?
K1 N1 C1 C2 -179.52(7) . . . . ?
C1 N1 C1 C3 179.21(13) 2_656 . . . ?
K1 N1 C1 C3 -0.79(13) . . . . ?
N1 C1 C2 C2 -1.25(18) . . . 2_656 ?
C3 C1 C2 C2 -179.80(13) . . . 2_656 ?
C4 N2 C3 C1 -173.08(11) . . . . ?
K1 N2 C3 C1 -10.64(15) . . . . ?
N1 C1 C3 N2 8.70(17) . . . . ?
C2 C1 C3 N2 -172.85(13) . . . . ?
C3 N2 C4 C11 -106.33(14) . . . . ?
K1 N2 C4 C11 93.75(12) . . . . ?
C3 N2 C4 C5 130.45(12) . . . . ?
K1 N2 C4 C5 -29.47(13) . . . . ?
N2 C4 C5 C10 83.33(16) . . . . ?
C11 C4 C5 C10 -39.52(18) . . . . ?
N2 C4 C5 C6 -91.34(15) . . . . ?
C11 C4 C5 C6 145.81(13) . . . . ?
C10 C5 C6 C7 0.0(2) . . . . ?
C4 C5 C6 C7 174.85(14) . . . . ?
C5 C6 C7 C8 0.0(3) . . . . ?
C6 C7 C8 C9 -0.1(3) . . . . ?
C7 C8 C9 C10 0.1(2) . . . . ?
C6 C5 C10 C9 0.1(2) . . . . ?
C4 C5 C10 C9 -174.66(14) . . . . ?
C8 C9 C10 C5 -0.2(2) . . . . ?
N2 C4 C11 C12 154.24(13) . . . . ?
C5 C4 C11 C12 -86.36(16) . . . . ?
N2 C4 C11 C16 -26.47(18) . . . . ?
C5 C4 C11 C16 92.93(15) . . . . ?
C16 C11 C12 C13 0.7(2) . . . . ?
C4 C11 C12 C13 -179.99(14) . . . . ?
C11 C12 C13 C14 0.1(3) . . . . ?
C12 C13 C14 C15 -0.8(2) . . . . ?
C13 C14 C15 C16 0.7(2) . . . . ?
C14 C15 C16 C11 0.0(2) . . . . ?
C12 C11 C16 C15 -0.8(2) . . . . ?
C4 C11 C16 C15 179.95(13) . . . . ?
C024 O1 C022 C021 10.9(2) . . . . ?
K1 O1 C022 C021 -178.93(12) . . . . ?
C023 C021 C022 O1 13.0(2) . . . . ?
C022 C021 C023 C024 -30.6(2) . . . . ?
C022 O1 C024 C023 -31.2(2) . . . . ?
K1 O1 C024 C023 158.10(12) . . . . ?
C021 C023 C024 O1 37.96(19) . . . . ?

_refine_diff_density_max         0.206
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.040



####################################################################### 
# 
# 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_1Li
_database_code_depnum_ccdc_archive 'CCDC 1476168'
_audit_update_record             
;
2016-08-02 deposited with the CCDC.
2016-08-18 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            'C72 H68 Li2 N6 O2'
_chemical_formula_weight         1063.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   13.8108(5)
_cell_length_b                   21.2028(8)
_cell_length_c                   21.5594(7)
_cell_angle_alpha                98.470(3)
_cell_angle_beta                 92.153(3)
_cell_angle_gamma                107.438(3)
_cell_volume                     5935.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    17700
_cell_measurement_theta_min      3.282
_cell_measurement_theta_max      70.920

_exptl_crystal_description       plates
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.551
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46701
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.282
_diffrn_reflns_theta_max         70.920
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             22370
_reflns_number_gt                17596
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3 & Olex 2.1'
_computing_publication_material  WinGX
_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)+(0.0910P)²+1.8080P] 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         22370
_refine_ls_number_parameters     1475
_refine_ls_number_restraints     1608
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1796
_refine_ls_wR_factor_gt          0.1638
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 1.2151(2) 0.99741(14) 0.28473(13) 0.0332(6) Uani 1 1 d . U . . .
Li2 Li 1.1493(2) 1.09183(14) 0.31124(13) 0.0321(6) Uani 1 1 d . U . . .
Li3 Li 0.8399(2) 0.41069(14) 0.18440(13) 0.0337(6) Uani 1 1 d . U . . .
Li4 Li 0.7797(2) 0.50810(14) 0.20997(13) 0.0343(6) Uani 1 1 d . U . . .
N1 N 1.28749(10) 1.09638(6) 0.27491(6) 0.0285(3) Uani 1 1 d . U . . .
N2 N 1.34148(10) 1.00112(7) 0.33645(6) 0.0290(3) Uani 1 1 d . U . . .
N3 N 1.11724(10) 1.13453(7) 0.23871(7) 0.0331(3) Uani 1 1 d . U . . .
N4 N 1.07199(10) 0.99257(7) 0.31945(6) 0.0284(3) Uani 1 1 d . U . . .
N5 N 1.13788(10) 1.11552(7) 0.40474(6) 0.0301(3) Uani 1 1 d . U . . .
N6 N 1.13852(10) 0.91925(7) 0.21958(6) 0.0328(3) Uani 1 1 d . U . . .
N7 N 0.70206(10) 0.41044(7) 0.22017(6) 0.0302(3) Uani 1 1 d . U . . .
N8 N 0.86785(11) 0.36900(7) 0.25931(7) 0.0338(3) Uani 1 1 d . U . . .
N9 N 0.65466(10) 0.50799(7) 0.15796(6) 0.0313(3) Uani 1 1 d . U . . .
N10 N 0.92202(10) 0.50887(7) 0.17449(6) 0.0299(3) Uani 1 1 d . U . . .
N11 N 0.86008(11) 0.58670(7) 0.27373(6) 0.0332(3) Uani 1 1 d . U . . .
N12 N 0.85298(10) 0.38382(7) 0.09117(6) 0.0306(3) Uani 1 1 d . U . . .
O2 O 0.61350(12) 0.00554(8) 0.28594(7) 0.0572(4) Uani 1 1 d . U . . .
O3 O 1.37481(11) 0.49026(7) 0.21378(6) 0.0491(3) Uani 1 1 d . U . . .
C1 C 1.38688(12) 1.09922(8) 0.28876(8) 0.0302(3) Uani 1 1 d . U . . .
C2 C 1.45429(13) 1.14948(9) 0.26201(9) 0.0386(4) Uani 1 1 d . U . . .
H2 H 1.5250 1.1612 0.2653 0.046 Uiso 1 1 calc R U . . .
C3 C 1.39447(13) 1.17832(9) 0.22950(9) 0.0380(4) Uani 1 1 d . U . . .
H3 H 1.4172 1.2128 0.2063 0.046 Uiso 1 1 calc R U . . .
C4 C 1.29362(12) 1.14521(8) 0.23861(8) 0.0310(3) Uani 1 1 d . U . . .
C5 C 1.20330(13) 1.15963(8) 0.21723(8) 0.0329(4) Uani 1 1 d . U . . .
H5 H 1.2077 1.1876 0.1873 0.039 Uiso 1 1 calc R U . . .
C6 C 1.41131(12) 1.05176(8) 0.32343(7) 0.0297(3) Uani 1 1 d . U . . .
H6 H 1.4789 1.0580 0.3366 0.036 Uiso 1 1 calc R U . . .
C7 C 1.37203(12) 0.95643(8) 0.37358(8) 0.0306(3) Uani 1 1 d . U . . .
H7 H 1.4460 0.9734 0.3835 0.037 Uiso 1 1 calc R U . . .
C8 C 1.34449(13) 0.88597(8) 0.33516(8) 0.0319(3) Uani 1 1 d . U . . .
C9 C 1.41761(15) 0.86597(11) 0.30340(10) 0.0499(5) Uani 1 1 d . U . . .
H9 H 1.4825 0.8961 0.3040 0.060 Uiso 1 1 calc R U . . .
C10 C 1.39541(19) 0.80152(13) 0.27056(12) 0.0665(7) Uani 1 1 d . U . . .
H10 H 1.4459 0.7885 0.2498 0.080 Uiso 1 1 calc R U . . .
C11 C 1.30010(19) 0.75660(11) 0.26812(11) 0.0590(6) Uani 1 1 d . U . . .
H11 H 1.2857 0.7132 0.2462 0.071 Uiso 1 1 calc R U . . .
C12 C 1.22622(19) 0.77645(11) 0.29838(12) 0.0649(7) Uani 1 1 d . U . . .
H12 H 1.1609 0.7465 0.2965 0.078 Uiso 1 1 calc R U . . .
C13 C 1.24806(17) 0.84072(11) 0.33176(11) 0.0567(6) Uani 1 1 d . U . . .
H13 H 1.1972 0.8536 0.3522 0.068 Uiso 1 1 calc R U . . .
C14 C 1.32115(13) 0.95523(8) 0.43498(8) 0.0317(3) Uani 1 1 d . U . . .
C15 C 1.22832(14) 0.96703(10) 0.44078(8) 0.0402(4) Uani 1 1 d . U . . .
H15 H 1.1968 0.9780 0.4068 0.048 Uiso 1 1 calc R U . . .
C16 C 1.18172(15) 0.96277(10) 0.49648(9) 0.0435(4) Uani 1 1 d . U . . .
H16 H 1.1197 0.9713 0.4996 0.052 Uiso 1 1 calc R U . . .
C17 C 1.22632(16) 0.94597(10) 0.54728(8) 0.0432(4) Uani 1 1 d . U . . .
H17 H 1.1943 0.9423 0.5843 0.052 Uiso 1 1 calc R U . . .
C18 C 1.31911(18) 0.93467(12) 0.54226(9) 0.0533(5) Uani 1 1 d . U . . .
H18 H 1.3503 0.9236 0.5763 0.064 Uiso 1 1 calc R U . . .
C19 C 1.36628(16) 0.93970(11) 0.48665(9) 0.0462(5) Uani 1 1 d . U . . .
H19 H 1.4293 0.9325 0.4841 0.055 Uiso 1 1 calc R U . . .
C20 C 1.02676(13) 1.14684(9) 0.21038(8) 0.0350(4) Uani 1 1 d . U . . .
H20 H 1.0499 1.1861 0.1895 0.042 Uiso 1 1 calc R U . . .
C21 C 0.95884(13) 1.16147(8) 0.26088(8) 0.0350(4) Uani 1 1 d . U . . .
C22 C 0.99864(15) 1.18860(10) 0.32257(9) 0.0424(4) Uani 1 1 d . U . . .
H22 H 1.0679 1.1976 0.3332 0.051 Uiso 1 1 calc R U . . .
C23 C 0.93726(18) 1.20244(11) 0.36843(10) 0.0509(5) Uani 1 1 d . U . . .
H23 H 0.9655 1.2200 0.4095 0.061 Uiso 1 1 calc R U . . .
C24 C 0.83435(17) 1.19052(11) 0.35386(11) 0.0533(5) Uani 1 1 d . U . . .
H24 H 0.7928 1.1993 0.3848 0.064 Uiso 1 1 calc R U . . .
C25 C 0.79457(16) 1.16526(11) 0.29226(12) 0.0577(6) Uani 1 1 d . U . . .
H25 H 0.7257 1.1579 0.2816 0.069 Uiso 1 1 calc R U . . .
C26 C 0.85557(15) 1.15079(11) 0.24622(10) 0.0491(5) Uani 1 1 d . U . . .
H26 H 0.8273 1.1338 0.2051 0.059 Uiso 1 1 calc R U . . .
C27 C 0.97371(13) 1.08623(9) 0.16076(8) 0.0374(4) Uani 1 1 d . U . . .
C28 C 0.96073(19) 1.09306(12) 0.09841(10) 0.0562(5) Uani 1 1 d . U . . .
H28 H 0.9827 1.1354 0.0869 0.067 Uiso 1 1 calc R U . . .
C29 C 0.9151(2) 1.03710(14) 0.05278(11) 0.0726(7) Uani 1 1 d . U . . .
H29 H 0.9062 1.0423 0.0111 0.087 Uiso 1 1 calc R U . . .
C30 C 0.88302(19) 0.97419(13) 0.06873(11) 0.0614(6) Uani 1 1 d . U . . .
H30 H 0.8530 0.9369 0.0380 0.074 Uiso 1 1 calc R U . . .
C31 C 0.89563(16) 0.96666(11) 0.13069(10) 0.0507(5) Uani 1 1 d . U . . .
H31 H 0.8744 0.9242 0.1418 0.061 Uiso 1 1 calc R U . . .
C32 C 0.94011(14) 1.02251(10) 0.17657(9) 0.0432(4) Uani 1 1 d . U . . .
H32 H 0.9475 1.0172 0.2184 0.052 Uiso 1 1 calc R U . . .
C33 C 1.01860(12) 1.00720(8) 0.36913(8) 0.0304(3) Uani 1 1 d . U . . .
C34 C 0.92633(13) 0.95604(9) 0.36870(8) 0.0371(4) Uani 1 1 d . U . . .
H34 H 0.8777 0.9545 0.3976 0.045 Uiso 1 1 calc R U . . .
C35 C 0.92227(13) 0.90811(9) 0.31655(8) 0.0368(4) Uani 1 1 d . U . . .
H35 H 0.8700 0.8682 0.3033 0.044 Uiso 1 1 calc R U . . .
C36 C 1.01229(12) 0.93162(8) 0.28786(8) 0.0306(3) Uani 1 1 d . U . . .
C37 C 1.04768(13) 0.89696(8) 0.23488(8) 0.0329(4) Uani 1 1 d . U . . .
H37 H 1.0035 0.8578 0.2116 0.039 Uiso 1 1 calc R U . . .
C38 C 1.05904(12) 1.06850(8) 0.41396(8) 0.0316(3) Uani 1 1 d . U . . .
H38 H 1.0269 1.0740 0.4506 0.038 Uiso 1 1 calc R U . . .
C39 C 1.17910(12) 1.17201(8) 0.45690(8) 0.0323(3) Uani 1 1 d . U . . .
H39 H 1.1252 1.1742 0.4847 0.039 Uiso 1 1 calc R U . . .
C40 C 1.26584(13) 1.15992(8) 0.49414(8) 0.0339(4) Uani 1 1 d . U . . .
C41 C 1.33701(15) 1.13616(10) 0.46327(9) 0.0471(5) Uani 1 1 d . U . . .
H41 H 1.3298 1.1258 0.4196 0.057 Uiso 1 1 calc R U . . .
C42 C 1.41828(18) 1.12757(12) 0.49597(10) 0.0565(6) Uani 1 1 d . U . . .
H42 H 1.4659 1.1120 0.4744 0.068 Uiso 1 1 calc R U . . .
C43 C 1.4290(2) 1.14208(13) 0.56067(11) 0.0631(6) Uani 1 1 d . U . . .
H43 H 1.4833 1.1356 0.5829 0.076 Uiso 1 1 calc R U . . .
C44 C 1.3606(2) 1.16582(15) 0.59187(10) 0.0697(7) Uani 1 1 d . U . . .
H44 H 1.3688 1.1763 0.6356 0.084 Uiso 1 1 calc R U . . .
C45 C 1.27790(18) 1.17471(12) 0.55919(9) 0.0530(5) Uani 1 1 d . U . . .
H45 H 1.2309 1.1906 0.5811 0.064 Uiso 1 1 calc R U . . .
C46 C 1.21889(13) 1.23873(8) 0.43365(8) 0.0340(4) Uani 1 1 d . U . . .
C47 C 1.19769(15) 1.29457(9) 0.46562(9) 0.0446(4) Uani 1 1 d . U . . .
H47 H 1.1548 1.2896 0.4980 0.054 Uiso 1 1 calc R U . . .
C48 C 1.24014(19) 1.35741(10) 0.44945(11) 0.0576(6) Uani 1 1 d . U . . .
H48 H 1.2262 1.3945 0.4713 0.069 Uiso 1 1 calc R U . . .
C49 C 1.30277(19) 1.36500(10) 0.40127(11) 0.0595(6) Uani 1 1 d . U . . .
H49 H 1.3313 1.4072 0.3905 0.071 Uiso 1 1 calc R U . . .
C50 C 1.32339(18) 1.30995(11) 0.36881(10) 0.0546(5) Uani 1 1 d . U . . .
H50 H 1.3653 1.3151 0.3359 0.065 Uiso 1 1 calc R U . . .
C51 C 1.28198(14) 1.24698(9) 0.38497(9) 0.0414(4) Uani 1 1 d . U . . .
H51 H 1.2966 1.2102 0.3631 0.050 Uiso 1 1 calc R U . . .
C52 C 1.17707(13) 0.88291(9) 0.16759(8) 0.0383(4) Uani 1 1 d . U . . .
H52 H 1.2182 0.8591 0.1866 0.046 Uiso 1 1 calc R U . . .
C53 C 1.09376(13) 0.83037(9) 0.12298(8) 0.0366(4) Uani 1 1 d . U . . .
C54 C 1.07266(15) 0.76271(9) 0.12709(9) 0.0421(4) Uani 1 1 d . U . . .
H54 H 1.1114 0.7497 0.1561 0.051 Uiso 1 1 calc R U . . .
C55 C 0.99437(16) 0.71430(10) 0.08836(9) 0.0465(5) Uani 1 1 d . U . . .
H55 H 0.9812 0.6692 0.0912 0.056 Uiso 1 1 calc R U . . .
C56 C 0.93621(15) 0.73340(10) 0.04566(9) 0.0451(4) Uani 1 1 d . U . . .
H56 H 0.8836 0.7012 0.0198 0.054 Uiso 1 1 calc R U . . .
C57 C 0.95631(15) 0.80064(10) 0.04149(9) 0.0461(5) Uani 1 1 d . U . . .
H57 H 0.9170 0.8136 0.0129 0.055 Uiso 1 1 calc R U . . .
C58 C 1.03508(15) 0.84883(9) 0.07996(9) 0.0420(4) Uani 1 1 d . U . . .
H58 H 1.0484 0.8938 0.0767 0.050 Uiso 1 1 calc R U . . .
C59 C 1.24828(15) 0.93318(11) 0.13292(9) 0.0495(5) Uani 1 1 d . U . . .
C60 C 1.33125(17) 0.91787(15) 0.10753(11) 0.0695(7) Uani 1 1 d . U . . .
H60 H 1.3432 0.8779 0.1123 0.083 Uiso 1 1 calc R U . . .
C61 C 1.3968(2) 0.9630(2) 0.07472(13) 0.0931(11) Uani 1 1 d . U . . .
H61 H 1.4525 0.9530 0.0579 0.112 Uiso 1 1 calc R U . . .
C62 C 1.3792(3) 1.02231(19) 0.06719(13) 0.0983(12) Uani 1 1 d . U . . .
H62 H 1.4227 1.0520 0.0452 0.118 Uiso 1 1 calc R U . . .
C63 C 1.2971(3) 1.03739(14) 0.09221(12) 0.0874(10) Uani 1 1 d . U . . .
H63 H 1.2851 1.0773 0.0870 0.105 Uiso 1 1 calc R U . . .
C64 C 1.2315(2) 0.99307(11) 0.12551(10) 0.0618(6) Uani 1 1 d . U . . .
H64 H 1.1766 1.0038 0.1427 0.074 Uiso 1 1 calc R U . . .
C65 C 0.69237(13) 0.36188(8) 0.25736(8) 0.0325(3) Uani 1 1 d . U . . .
C66 C 0.59015(14) 0.33094(9) 0.26591(9) 0.0398(4) Uani 1 1 d . U . . .
H66 H 0.5650 0.2971 0.2895 0.048 Uiso 1 1 calc R U . . .
C67 C 0.53383(13) 0.36078(9) 0.23215(9) 0.0408(4) Uani 1 1 d . U . . .
H67 H 0.4633 0.3505 0.2282 0.049 Uiso 1 1 calc R U . . .
C68 C 0.60412(12) 0.40951(8) 0.20519(8) 0.0330(4) Uani 1 1 d . U . . .
C69 C 0.58292(12) 0.45783(8) 0.17033(8) 0.0324(3) Uani 1 1 d . U . . .
H69 H 0.5159 0.4525 0.1565 0.039 Uiso 1 1 calc R U . . .
C70 C 0.78023(13) 0.34535(8) 0.27957(8) 0.0343(4) Uani 1 1 d . U . . .
H70 H 0.7732 0.3169 0.3092 0.041 Uiso 1 1 calc R U . . .
C71 C 0.62671(13) 0.55513(8) 0.12263(8) 0.0333(4) Uani 1 1 d . U . . .
H71 H 0.5531 0.5383 0.1112 0.040 Uiso 1 1 calc R U . . .
C72 C 0.65109(13) 0.62324(8) 0.16539(8) 0.0334(4) Uani 1 1 d . U . . .
C73 C 0.59026(14) 0.63015(9) 0.21423(9) 0.0402(4) Uani 1 1 d . U . . .
H73 H 0.5368 0.5934 0.2206 0.048 Uiso 1 1 calc R U . . .
C74 C 0.60823(15) 0.69112(10) 0.25350(9) 0.0464(5) Uani 1 1 d . U . . .
H74 H 0.5668 0.6950 0.2860 0.056 Uiso 1 1 calc R U . . .
C75 C 0.68695(17) 0.74594(10) 0.24475(10) 0.0518(5) Uani 1 1 d . U . . .
H75 H 0.6980 0.7871 0.2705 0.062 Uiso 1 1 calc R U . . .
C76 C 0.7489(2) 0.73932(11) 0.19773(12) 0.0673(7) Uani 1 1 d . U . . .
H76 H 0.8033 0.7759 0.1923 0.081 Uiso 1 1 calc R U . . .
C77 C 0.73131(18) 0.67855(11) 0.15817(11) 0.0580(6) Uani 1 1 d . U . . .
H77 H 0.7739 0.6749 0.1264 0.070 Uiso 1 1 calc R U . . .
C78 C 0.68037(14) 0.55902(9) 0.06242(8) 0.0365(4) Uani 1 1 d . U . . .
C79 C 0.63473(16) 0.57146(11) 0.00896(9) 0.0486(5) Uani 1 1 d . U . . .
H79 H 0.5705 0.5770 0.0099 0.058 Uiso 1 1 calc R U . . .
C80 C 0.68441(18) 0.57574(11) -0.04603(10) 0.0551(5) Uani 1 1 d . U . . .
H80 H 0.6533 0.5845 -0.0814 0.066 Uiso 1 1 calc R U . . .
C81 C 0.77949(17) 0.56711(10) -0.04843(9) 0.0504(5) Uani 1 1 d . U . . .
H81 H 0.8122 0.5693 -0.0853 0.060 Uiso 1 1 calc R U . . .
C82 C 0.82522(16) 0.55518(10) 0.00466(9) 0.0453(4) Uani 1 1 d . U . . .
H82 H 0.8893 0.5494 0.0035 0.054 Uiso 1 1 calc R U . . .
C83 C 0.95537(13) 0.35460(9) 0.28859(8) 0.0363(4) Uani 1 1 d . U . . .
H83 H 0.9296 0.3156 0.3096 0.044 Uiso 1 1 calc R U . . .
C84 C 1.02300(13) 0.33817(8) 0.23868(8) 0.0351(4) Uani 1 1 d . U . . .
C85 C 0.98309(15) 0.31082(9) 0.17705(9) 0.0411(4) Uani 1 1 d . U . . .
H85 H 0.9140 0.3024 0.1663 0.049 Uiso 1 1 calc R U . . .
C86 C 1.04415(17) 0.29596(10) 0.13139(9) 0.0473(5) Uani 1 1 d . U . . .
H86 H 1.0160 0.2785 0.0903 0.057 Uiso 1 1 calc R U . . .
C87 C 1.14655(16) 0.30675(10) 0.14628(10) 0.0489(5) Uani 1 1 d . U . . .
H87 H 1.1878 0.2972 0.1154 0.059 Uiso 1 1 calc R U . . .
C88 C 1.18673(15) 0.33192(10) 0.20782(11) 0.0520(5) Uani 1 1 d . U . . .
H88 H 1.2552 0.3383 0.2187 0.062 Uiso 1 1 calc R U . . .
C89 C 1.12574(14) 0.34768(10) 0.25355(10) 0.0456(4) Uani 1 1 d . U . . .
H89 H 1.1540 0.3648 0.2947 0.055 Uiso 1 1 calc R U . . .
C90 C 1.01068(14) 0.41483(10) 0.33795(8) 0.0390(4) Uani 1 1 d . U . . .
C91 C 1.04783(15) 0.47828(10) 0.32186(9) 0.0445(4) Uani 1 1 d . U . . .
H91 H 1.0404 0.4836 0.2801 0.053 Uiso 1 1 calc R U . . .
C92 C 1.09594(16) 0.53384(11) 0.36720(11) 0.0532(5) Uani 1 1 d . U . . .
H92 H 1.1196 0.5761 0.3558 0.064 Uiso 1 1 calc R U . . .
C93 C 1.10862(19) 0.52624(13) 0.42937(11) 0.0623(6) Uani 1 1 d . U . . .
H93 H 1.1414 0.5632 0.4598 0.075 Uiso 1 1 calc R U . . .
C94 C 1.0724(2) 0.46357(14) 0.44586(11) 0.0676(7) Uani 1 1 d . U . . .
H94 H 1.0809 0.4584 0.4876 0.081 Uiso 1 1 calc R U . . .
C95 C 1.02326(18) 0.40779(12) 0.40057(9) 0.0540(5) Uani 1 1 d . U . . .
H95 H 0.9988 0.3657 0.4123 0.065 Uiso 1 1 calc R U . . .
C96 C 0.97306(12) 0.49274(8) 0.12399(8) 0.0326(3) Uani 1 1 d . U . . .
C97 C 1.06539(13) 0.54337(9) 0.12235(9) 0.0387(4) Uani 1 1 d . U . . .
H97 H 1.1127 0.5438 0.0927 0.046 Uiso 1 1 calc R U . . .
C98 C 1.07163(13) 0.59240(9) 0.17376(9) 0.0383(4) Uani 1 1 d . U . . .
H98 H 1.1244 0.6323 0.1856 0.046 Uiso 1 1 calc R U . . .
C99 C 0.98318(12) 0.57034(8) 0.20435(8) 0.0318(3) Uani 1 1 d . U . . .
C100 C 0.95045(13) 0.60702(8) 0.25718(8) 0.0342(4) Uani 1 1 d . U . . .
H100 H 0.9962 0.6462 0.2795 0.041 Uiso 1 1 calc R U . . .
C101 C 0.93187(12) 0.43019(8) 0.08104(8) 0.0332(4) Uani 1 1 d . U . . .
H101 H 0.9639 0.4233 0.0446 0.040 Uiso 1 1 calc R U . . .
C102 C 0.81544(12) 0.32474(8) 0.04140(8) 0.0321(3) Uani 1 1 d . U . . .
H102 H 0.8736 0.3182 0.0197 0.039 Uiso 1 1 calc R U . . .
C103 C 0.74004(14) 0.33478(10) -0.00660(9) 0.0407(4) Uani 1 1 d . U . . .
C104 C 0.69479(18) 0.38371(11) 0.00393(13) 0.0661(7) Uani 1 1 d . U . . .
H104 H 0.7093 0.4129 0.0422 0.079 Uiso 1 1 calc R U . . .
C105 C 0.6267(2) 0.39045(15) -0.04225(18) 0.0966(11) Uani 1 1 d . U . . .
H105 H 0.5984 0.4253 -0.0352 0.116 Uiso 1 1 calc R U . . .
C106 C 0.6015(3) 0.3473(2) -0.09673(17) 0.1023(12) Uani 1 1 d . U . . .
H106 H 0.5542 0.3512 -0.1266 0.123 Uiso 1 1 calc R U . . .
C107 C 0.6449(3) 0.2984(2) -0.10784(13) 0.1069(12) Uani 1 1 d . U . . .
H107 H 0.6275 0.2684 -0.1456 0.128 Uiso 1 1 calc R U . . .
C108 C 0.7150(2) 0.29234(17) -0.06369(10) 0.0793(9) Uani 1 1 d . U . . .
H108 H 0.7460 0.2591 -0.0726 0.095 Uiso 1 1 calc R U . . .
C109 C 0.76452(13) 0.26179(8) 0.06846(8) 0.0347(4) Uani 1 1 d . U . . .
C110 C 0.69278(14) 0.26176(10) 0.11169(9) 0.0424(4) Uani 1 1 d . U . . .
H110 H 0.6789 0.3013 0.1265 0.051 Uiso 1 1 calc R U . . .
C111 C 0.64147(18) 0.20298(11) 0.13300(10) 0.0584(6) Uani 1 1 d . U . . .
H111 H 0.5939 0.2035 0.1623 0.070 Uiso 1 1 calc R U . . .
C112 C 0.6607(2) 0.14362(12) 0.11093(12) 0.0674(7) Uani 1 1 d . U . . .
H112 H 0.6258 0.1043 0.1250 0.081 Uiso 1 1 calc R U . . .
C113 C 0.7319(2) 0.14331(11) 0.06813(13) 0.0654(7) Uani 1 1 d . U . . .
H113 H 0.7453 0.1036 0.0533 0.078 Uiso 1 1 calc R U . . .
C114 C 0.78414(16) 0.20212(10) 0.04672(10) 0.0500(5) Uani 1 1 d . U . . .
H114 H 0.8323 0.2014 0.0178 0.060 Uiso 1 1 calc R U . . .
C115 C 0.82460(13) 0.62622(9) 0.32489(8) 0.0367(4) Uani 1 1 d . U . . .
H115 H 0.7869 0.6514 0.3048 0.044 Uiso 1 1 calc R U . . .
C116 C 0.90911(13) 0.67757(9) 0.36946(8) 0.0355(4) Uani 1 1 d . U . . .
C117 C 0.93003(14) 0.74555(9) 0.36729(9) 0.0395(4) Uani 1 1 d . U . . .
H117 H 0.8916 0.7593 0.3388 0.047 Uiso 1 1 calc R U . . .
C118 C 1.00752(15) 0.79331(10) 0.40717(9) 0.0445(4) Uani 1 1 d . U . . .
H118 H 1.0201 0.8387 0.4057 0.053 Uiso 1 1 calc R U . . .
C119 C 1.06557(15) 0.77317(10) 0.44885(9) 0.0481(5) Uani 1 1 d . U . . .
H119 H 1.1179 0.8049 0.4754 0.058 Uiso 1 1 calc R U . . .
C120 C 1.04578(15) 0.70539(11) 0.45115(9) 0.0473(5) Uani 1 1 d . U . . .
H120 H 1.0852 0.6918 0.4791 0.057 Uiso 1 1 calc R U . . .
C121 C 0.96749(14) 0.65781(10) 0.41192(9) 0.0409(4) Uani 1 1 d . U . . .
H121 H 0.9542 0.6126 0.4141 0.049 Uiso 1 1 calc R U . . .
C122 C 0.74889(15) 0.57908(11) 0.35986(9) 0.0472(5) Uani 1 1 d . U . . .
C123 C 0.66994(16) 0.59898(15) 0.38588(10) 0.0638(7) Uani 1 1 d . U . . .
H123 H 0.6636 0.6406 0.3817 0.077 Uiso 1 1 calc R U . . .
C124 C 0.59974(19) 0.5559(2) 0.41853(12) 0.0882(10) Uani 1 1 d . U . . .
H124 H 0.5462 0.5689 0.4352 0.106 Uiso 1 1 calc R U . . .
C125 C 0.6099(3) 0.49474(19) 0.42591(13) 0.1000(12) Uani 1 1 d . U . . .
H125 H 0.5638 0.4666 0.4479 0.120 Uiso 1 1 calc R U . . .
C126 C 0.6879(3) 0.47575(14) 0.40087(14) 0.1020(12) Uani 1 1 d . U . . .
H126 H 0.6946 0.4344 0.4059 0.122 Uiso 1 1 calc R U . . .
C127 C 0.7576(2) 0.51711(11) 0.36781(12) 0.0726(8) Uani 1 1 d . U . . .
H127 H 0.8103 0.5032 0.3510 0.087 Uiso 1 1 calc R U . . .
C132 C 0.5808(2) 0.00223(15) 0.22270(11) 0.0732(7) Uani 1 1 d . U . . .
H13A H 0.5992 0.0469 0.2120 0.088 Uiso 1 1 calc R U . . .
H13B H 0.5073 -0.0170 0.2162 0.088 Uiso 1 1 calc R U . . .
C133 C 0.6297(3) -0.03993(19) 0.18189(14) 0.0937(10) Uani 1 1 d . U . . .
H13C H 0.6833 -0.0126 0.1606 0.112 Uiso 1 1 calc R U . . .
H13D H 0.5802 -0.0723 0.1507 0.112 Uiso 1 1 calc R U . . .
C134 C 0.6730(2) -0.07464(14) 0.22782(14) 0.0731(7) Uani 1 1 d . U . . .
H13E H 0.6240 -0.1168 0.2330 0.088 Uiso 1 1 calc R U . . .
H13F H 0.7351 -0.0827 0.2144 0.088 Uiso 1 1 calc R U . . .
C135 C 0.69325(18) -0.02427(13) 0.28666(12) 0.0607(6) Uani 1 1 d . U . . .
H13G H 0.6928 -0.0458 0.3234 0.073 Uiso 1 1 calc R U . . .
H13H H 0.7590 0.0094 0.2874 0.073 Uiso 1 1 calc R U . . .
C136 C 1.39619(17) 0.48928(11) 0.27858(10) 0.0516(5) Uani 1 1 d . U . . .
H13I H 1.4689 0.4993 0.2884 0.062 Uiso 1 1 calc R U . . .
H13J H 1.3619 0.4454 0.2886 0.062 Uiso 1 1 calc R U . . .
C137 C 1.3585(3) 0.54145(18) 0.31587(12) 0.0865(10) Uani 1 1 d . U . . .
H13K H 1.4137 0.5745 0.3430 0.104 Uiso 1 1 calc R U . . .
H13L H 1.3056 0.5210 0.3416 0.104 Uiso 1 1 calc R U . . .
C138 C 1.31681(18) 0.57334(12) 0.26750(12) 0.0606(6) Uani 1 1 d . U . . .
H13M H 1.2550 0.5826 0.2798 0.073 Uiso 1 1 calc R U . . .
H13N H 1.3664 0.6146 0.2609 0.073 Uiso 1 1 calc R U . . .
C139 C 1.29570(17) 0.52040(11) 0.20959(10) 0.0518(5) Uani 1 1 d . U . . .
H13O H 1.2293 0.4875 0.2092 0.062 Uiso 1 1 calc R U . . .
H13P H 1.2979 0.5403 0.1717 0.062 Uiso 1 1 calc R U . . .
C160 C 0.77676(14) 0.55172(9) 0.05985(8) 0.0399(4) Uani 1 1 d . U . . .
H160 H 0.8092 0.5444 0.0955 0.048 Uiso 1 1 calc R U . . .
O0AA O 0.2921(3) 0.2141(3) 0.02439(18) 0.213(2) Uani 1 1 d D U . . .
C4AA C 0.4545(4) 0.2245(4) 0.0129(3) 0.231(4) Uani 1 1 d D U . . .
H4AD H 0.4886 0.2642 -0.0045 0.277 Uiso 0.5 1 calc R U P A 2
H4AC H 0.5043 0.2068 0.0307 0.277 Uiso 0.5 1 calc R U P A 2
H4AB H 0.5109 0.2651 0.0139 0.277 Uiso 0.5 1 calc R U P B 1
H4AA H 0.4812 0.1896 0.0233 0.277 Uiso 0.5 1 calc R U P B 1
C1AA C 0.3804(6) 0.2366(4) 0.0590(3) 0.191(3) Uani 1 1 d D U . . .
H1AA H 0.3801 0.2119 0.0935 0.230 Uiso 1 1 calc R U . . .
H1AB H 0.3964 0.2839 0.0758 0.230 Uiso 1 1 calc R U . . .
C1A C 0.3779(9) 0.1735(6) -0.0331(6) 0.158(5) Uiso 0.5 1 d D . P C 2
H1AC H 0.3395 0.1344 -0.0162 0.189 Uiso 0.5 1 calc R U P C 2
H1AD H 0.4039 0.1608 -0.0727 0.189 Uiso 0.5 1 calc R U P C 2
C1B C 0.2924(9) 0.1944(8) -0.0347(6) 0.187(6) Uiso 0.5 1 d D . P C 1
H1BA H 0.2615 0.2199 -0.0584 0.224 Uiso 0.5 1 calc R U P C 1
H1BB H 0.2527 0.1474 -0.0456 0.224 Uiso 0.5 1 calc R U P C 1
O5AA O 0.7148(3) 0.2822(2) 0.48131(17) 0.1733(16) Uani 1 1 d D U . D 1
C9AA C 0.6771(4) 0.2784(3) 0.5382(2) 0.161(2) Uani 1 1 d D U . D 1
H9AA H 0.7312 0.2968 0.5719 0.193 Uiso 1 1 calc R U . D 1
H9AB H 0.6414 0.2323 0.5418 0.193 Uiso 1 1 calc R U . D 1
C6AA C 0.6372(5) 0.2805(4) 0.4402(3) 0.176(2) Uani 1 1 d D U . D 1
H6AA H 0.6071 0.2352 0.4176 0.211 Uiso 1 1 calc R U . D 1
H6AB H 0.6633 0.3095 0.4098 0.211 Uiso 1 1 calc R U . D 1
C8AA C 0.6066(4) 0.3186(3) 0.5400(3) 0.188(3) Uani 1 1 d D U . D 1
H8AA H 0.6432 0.3661 0.5517 0.226 Uiso 1 1 calc R U . D 1
H8AB H 0.5562 0.3057 0.5698 0.226 Uiso 1 1 calc R U . D 1
C0 C 0.5572(4) 0.3030(3) 0.4738(4) 0.188(3) Uani 1 1 d D U . D 1
H0A H 0.4925 0.2677 0.4691 0.225 Uiso 1 1 calc R U . D 1
H0B H 0.5478 0.3424 0.4598 0.225 Uiso 1 1 calc R U . D 1
C1C C 0.3970(7) 0.2034(6) -0.0511(4) 0.127(3) Uiso 0.5 1 d D . P C 1
H1CA H 0.4184 0.2379 -0.0771 0.153 Uiso 0.5 1 calc R U P C 1
H1CB H 0.4049 0.1619 -0.0726 0.153 Uiso 0.5 1 calc R U P C 1
C1D C 0.3214(7) 0.2301(5) -0.0342(4) 0.108(3) Uiso 0.5 1 d D . P C 2
H1DA H 0.3669 0.2752 -0.0328 0.130 Uiso 0.5 1 calc R U P C 2
H1DB H 0.2657 0.2189 -0.0667 0.130 Uiso 0.5 1 calc R U P C 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
Li1 N6 1.997(3) . ?
Li1 N2 2.011(3) . ?
Li1 N1 2.083(3) . ?
Li1 N4 2.118(3) . ?
Li1 Li2 2.440(4) . ?
Li1 C6 2.654(3) . ?
Li1 C1 2.675(3) . ?
Li1 C37 2.688(3) . ?
Li1 C36 2.737(3) . ?
Li2 N3 2.016(3) . ?
Li2 N5 2.028(3) . ?
Li2 N1 2.072(3) . ?
Li2 N4 2.092(3) . ?
Li2 C38 2.620(3) . ?
Li2 C33 2.631(3) . ?
Li2 C4 2.667(3) . ?
Li3 N8 2.029(3) . ?
Li3 N12 2.037(3) . ?
Li3 N7 2.079(3) . ?
Li3 N10 2.098(3) . ?
Li3 Li4 2.447(4) . ?
Li3 C96 2.653(3) . ?
Li3 C70 2.662(3) . ?
Li3 C65 2.674(3) . ?
Li4 N11 2.000(3) . ?
Li4 N9 2.022(3) . ?
Li4 N7 2.075(3) . ?
Li4 N10 2.132(3) . ?
Li4 C69 2.659(3) . ?
Li4 C68 2.672(3) . ?
Li4 C100 2.688(3) . ?
Li4 C99 2.739(3) . ?
N1 C4 1.372(2) . ?
N1 C1 1.375(2) . ?
N2 C6 1.285(2) . ?
N2 C7 1.468(2) . ?
N3 C5 1.283(2) . ?
N3 C20 1.479(2) . ?
N4 C36 1.369(2) . ?
N4 C33 1.373(2) . ?
N5 C38 1.282(2) . ?
N5 C39 1.473(2) . ?
N6 C37 1.276(2) . ?
N6 C52 1.473(2) . ?
N7 C68 1.372(2) . ?
N7 C65 1.375(2) . ?
N8 C70 1.283(2) . ?
N8 C83 1.474(2) . ?
N9 C69 1.287(2) . ?
N9 C71 1.470(2) . ?
N10 C99 1.371(2) . ?
N10 C96 1.375(2) . ?
N11 C100 1.276(2) . ?
N11 C115 1.474(2) . ?
N12 C101 1.281(2) . ?
N12 C102 1.470(2) . ?
O2 C132 1.405(3) . ?
O2 C135 1.425(3) . ?
O3 C136 1.422(2) . ?
O3 C139 1.428(3) . ?
C1 C2 1.401(2) . ?
C1 C6 1.446(2) . ?
C2 C3 1.390(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.395(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.445(2) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C14 1.522(2) . ?
C7 C8 1.528(2) . ?
C7 H7 0.9800 . ?
C8 C9 1.375(3) . ?
C8 C13 1.380(3) . ?
C9 C10 1.382(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.368(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.367(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.384(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.384(2) . ?
C14 C19 1.385(2) . ?
C15 C16 1.386(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.379(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.378(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.388(3) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C27 1.518(2) . ?
C20 C21 1.521(2) . ?
C20 H20 0.9800 . ?
C21 C22 1.390(3) . ?
C21 C26 1.392(3) . ?
C22 C23 1.382(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.382(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.383(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.385(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.384(3) . ?
C27 C32 1.389(3) . ?
C28 C29 1.391(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.373(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.379(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.390(3) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.403(2) . ?
C33 C38 1.446(2) . ?
C34 C35 1.387(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.398(2) . ?
C35 H35 0.9300 . ?
C36 C37 1.447(2) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C40 1.522(2) . ?
C39 C46 1.523(2) . ?
C39 H39 0.9800 . ?
C40 C41 1.382(3) . ?
C40 C45 1.384(3) . ?
C41 C42 1.375(3) . ?
C41 H41 0.9300 . ?
C42 C43 1.376(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.354(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.394(3) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C46 C51 1.387(3) . ?
C46 C47 1.395(2) . ?
C47 C48 1.387(3) . ?
C47 H47 0.9300 . ?
C48 C49 1.373(4) . ?
C48 H48 0.9300 . ?
C49 C50 1.381(3) . ?
C49 H49 0.9300 . ?
C50 C51 1.388(3) . ?
C50 H50 0.9300 . ?
C51 H51 0.9300 . ?
C52 C53 1.524(2) . ?
C52 C59 1.524(3) . ?
C52 H52 0.9800 . ?
C53 C58 1.382(3) . ?
C53 C54 1.393(3) . ?
C54 C55 1.391(3) . ?
C54 H54 0.9300 . ?
C55 C56 1.381(3) . ?
C55 H55 0.9300 . ?
C56 C57 1.386(3) . ?
C56 H56 0.9300 . ?
C57 C58 1.390(3) . ?
C57 H57 0.9300 . ?
C58 H58 0.9300 . ?
C59 C64 1.387(3) . ?
C59 C60 1.391(3) . ?
C60 C61 1.402(4) . ?
C60 H60 0.9300 . ?
C61 C62 1.381(5) . ?
C61 H61 0.9300 . ?
C62 C63 1.375(5) . ?
C62 H62 0.9300 . ?
C63 C64 1.399(3) . ?
C63 H63 0.9300 . ?
C64 H64 0.9300 . ?
C65 C66 1.399(2) . ?
C65 C70 1.444(2) . ?
C66 C67 1.387(3) . ?
C66 H66 0.9300 . ?
C67 C68 1.402(2) . ?
C67 H67 0.9300 . ?
C68 C69 1.446(2) . ?
C69 H69 0.9300 . ?
C70 H70 0.9300 . ?
C71 C78 1.519(2) . ?
C71 C72 1.530(2) . ?
C71 H71 0.9800 . ?
C72 C77 1.384(3) . ?
C72 C73 1.389(2) . ?
C73 C74 1.385(3) . ?
C73 H73 0.9300 . ?
C74 C75 1.375(3) . ?
C74 H74 0.9300 . ?
C75 C76 1.369(3) . ?
C75 H75 0.9300 . ?
C76 C77 1.385(3) . ?
C76 H76 0.9300 . ?
C77 H77 0.9300 . ?
C78 C160 1.388(3) . ?
C78 C79 1.389(3) . ?
C79 C80 1.393(3) . ?
C79 H79 0.9300 . ?
C80 C81 1.381(3) . ?
C80 H80 0.9300 . ?
C81 C82 1.378(3) . ?
C81 H81 0.9300 . ?
C82 C160 1.387(3) . ?
C82 H82 0.9300 . ?
C83 C90 1.517(3) . ?
C83 C84 1.520(2) . ?
C83 H83 0.9800 . ?
C84 C89 1.390(3) . ?
C84 C85 1.390(2) . ?
C85 C86 1.382(3) . ?
C85 H85 0.9300 . ?
C86 C87 1.381(3) . ?
C86 H86 0.9300 . ?
C87 C88 1.383(3) . ?
C87 H87 0.9300 . ?
C88 C89 1.388(3) . ?
C88 H88 0.9300 . ?
C89 H89 0.9300 . ?
C90 C91 1.389(3) . ?
C90 C95 1.390(3) . ?
C91 C92 1.389(3) . ?
C91 H91 0.9300 . ?
C92 C93 1.384(3) . ?
C92 H92 0.9300 . ?
C93 C94 1.377(4) . ?
C93 H93 0.9300 . ?
C94 C95 1.394(3) . ?
C94 H94 0.9300 . ?
C95 H95 0.9300 . ?
C96 C97 1.405(2) . ?
C96 C101 1.444(2) . ?
C97 C98 1.384(2) . ?
C97 H97 0.9300 . ?
C98 C99 1.398(2) . ?
C98 H98 0.9300 . ?
C99 C100 1.447(2) . ?
C100 H100 0.9300 . ?
C101 H101 0.9300 . ?
C102 C109 1.521(2) . ?
C102 C103 1.522(2) . ?
C102 H102 0.9800 . ?
C103 C104 1.360(3) . ?
C103 C108 1.378(3) . ?
C104 C105 1.396(3) . ?
C104 H104 0.9300 . ?
C105 C106 1.342(5) . ?
C105 H105 0.9300 . ?
C106 C107 1.343(5) . ?
C106 H106 0.9300 . ?
C107 C108 1.379(4) . ?
C107 H107 0.9300 . ?
C108 H108 0.9300 . ?
C109 C110 1.385(3) . ?
C109 C114 1.391(3) . ?
C110 C111 1.389(3) . ?
C110 H110 0.9300 . ?
C111 C112 1.384(4) . ?
C111 H111 0.9300 . ?
C112 C113 1.374(4) . ?
C112 H112 0.9300 . ?
C113 C114 1.394(3) . ?
C113 H113 0.9300 . ?
C114 H114 0.9300 . ?
C115 C122 1.522(3) . ?
C115 C116 1.522(2) . ?
C115 H115 0.9800 . ?
C116 C121 1.387(3) . ?
C116 C117 1.391(3) . ?
C117 C118 1.391(3) . ?
C117 H117 0.9300 . ?
C118 C119 1.377(3) . ?
C118 H118 0.9300 . ?
C119 C120 1.389(3) . ?
C119 H119 0.9300 . ?
C120 C121 1.389(3) . ?
C120 H120 0.9300 . ?
C121 H121 0.9300 . ?
C122 C127 1.389(3) . ?
C122 C123 1.391(3) . ?
C123 C124 1.407(4) . ?
C123 H123 0.9300 . ?
C124 C125 1.377(5) . ?
C124 H124 0.9300 . ?
C125 C126 1.361(5) . ?
C125 H125 0.9300 . ?
C126 C127 1.391(3) . ?
C126 H126 0.9300 . ?
C127 H127 0.9300 . ?
C132 C133 1.485(4) . ?
C132 H13A 0.9700 . ?
C132 H13B 0.9700 . ?
C133 C134 1.521(4) . ?
C133 H13C 0.9700 . ?
C133 H13D 0.9700 . ?
C134 C135 1.491(4) . ?
C134 H13E 0.9700 . ?
C134 H13F 0.9700 . ?
C135 H13G 0.9700 . ?
C135 H13H 0.9700 . ?
C136 C137 1.502(3) . ?
C136 H13I 0.9700 . ?
C136 H13J 0.9700 . ?
C137 C138 1.507(4) . ?
C137 H13K 0.9700 . ?
C137 H13L 0.9700 . ?
C138 C139 1.506(3) . ?
C138 H13M 0.9700 . ?
C138 H13N 0.9700 . ?
C139 H13O 0.9700 . ?
C139 H13P 0.9700 . ?
C160 H160 0.9300 . ?
O0AA C1B 1.281(11) . ?
O0AA C1AA 1.322(6) . ?
O0AA C1D 1.399(8) . ?
C4AA C1C 1.503(9) . ?
C4AA C1A 1.480(10) . ?
C4AA C1AA 1.503(7) . ?
C4AA H4AD 0.9700 . ?
C4AA H4AC 0.9700 . ?
C4AA H4AB 0.9700 . ?
C4AA H4AA 0.9700 . ?
C1AA H1AA 0.9700 . ?
C1AA H1AB 0.9700 . ?
C1A C1D 1.619(11) . ?
C1A H1AC 0.9700 . ?
C1A H1AD 0.9700 . ?
C1B C1C 1.463(11) . ?
C1B H1BA 0.9700 . ?
C1B H1BB 0.9700 . ?
O5AA C9AA 1.353(5) . ?
O5AA C6AA 1.353(5) . ?
C9AA C8AA 1.473(7) . ?
C9AA H9AA 0.9700 . ?
C9AA H9AB 0.9700 . ?
C6AA C0 1.498(6) . ?
C6AA H6AA 0.9700 . ?
C6AA H6AB 0.9700 . ?
C8AA C0 1.506(7) . ?
C8AA H8AA 0.9700 . ?
C8AA H8AB 0.9700 . ?
C0 H0A 0.9700 . ?
C0 H0B 0.9700 . ?
C1C H1CA 0.9700 . ?
C1C H1CB 0.9700 . ?
C1D H1DA 0.9700 . ?
C1D H1DB 0.9700 . ?

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
N6 Li1 N2 123.64(15) . . ?
N6 Li1 N1 129.56(16) . . ?
N2 Li1 N1 87.49(12) . . ?
N6 Li1 N4 86.20(12) . . ?
N2 Li1 N4 125.62(15) . . ?
N1 Li1 N4 107.90(14) . . ?
N6 Li1 Li2 120.16(15) . . ?
N2 Li1 Li2 116.03(14) . . ?
N1 Li1 Li2 53.82(10) . . ?
N4 Li1 Li2 54.09(10) . . ?
N6 Li1 C6 133.03(14) . . ?
N2 Li1 C6 27.85(6) . . ?
N1 Li1 C6 61.10(9) . . ?
N4 Li1 C6 138.52(13) . . ?
Li2 Li1 C6 102.16(12) . . ?
N6 Li1 C1 134.56(14) . . ?
N2 Li1 C1 59.09(9) . . ?
N1 Li1 C1 30.48(6) . . ?
N4 Li1 C1 131.99(13) . . ?
Li2 Li1 C1 80.08(11) . . ?
C6 Li1 C1 31.48(6) . . ?
N6 Li1 C37 26.78(7) . . ?
N2 Li1 C37 133.25(14) . . ?
N1 Li1 C37 138.23(14) . . ?
N4 Li1 C37 59.92(8) . . ?
Li2 Li1 C37 102.88(12) . . ?
C6 Li1 C37 154.94(13) . . ?
C1 Li1 C37 158.59(13) . . ?
N6 Li1 C36 57.63(9) . . ?
N2 Li1 C36 133.46(14) . . ?
N1 Li1 C36 129.85(14) . . ?
N4 Li1 C36 29.37(6) . . ?
Li2 Li1 C36 79.21(11) . . ?
C6 Li1 C36 159.38(13) . . ?
C1 Li1 C36 159.23(13) . . ?
C37 Li1 C36 30.92(6) . . ?
N3 Li2 N5 130.35(15) . . ?
N3 Li2 N1 87.42(12) . . ?
N5 Li2 N1 122.11(15) . . ?
N3 Li2 N4 122.52(15) . . ?
N5 Li2 N4 86.99(12) . . ?
N1 Li2 N4 109.32(14) . . ?
N3 Li2 Li1 116.22(15) . . ?
N5 Li2 Li1 113.43(14) . . ?
N1 Li2 Li1 54.25(10) . . ?
N4 Li2 Li1 55.09(10) . . ?
N3 Li2 C38 131.98(14) . . ?
N5 Li2 C38 28.56(6) . . ?
N1 Li2 C38 139.49(14) . . ?
N4 Li2 C38 61.50(9) . . ?
Li1 Li2 C38 103.68(13) . . ?
N3 Li2 C33 126.98(14) . . ?
N5 Li2 C33 59.98(9) . . ?
N1 Li2 C33 135.45(14) . . ?
N4 Li2 C33 31.23(6) . . ?
Li1 Li2 C33 83.01(11) . . ?
C38 Li2 C33 31.96(6) . . ?
N3 Li2 C4 59.10(9) . . ?
N5 Li2 C4 130.72(14) . . ?
N1 Li2 C4 30.50(6) . . ?
N4 Li2 C4 132.35(13) . . ?
Li1 Li2 C4 80.64(11) . . ?
C38 Li2 C4 158.86(13) . . ?
C33 Li2 C4 163.30(13) . . ?
N8 Li3 N12 130.18(16) . . ?
N8 Li3 N7 87.05(12) . . ?
N12 Li3 N7 122.93(15) . . ?
N8 Li3 N10 122.33(15) . . ?
N12 Li3 N10 87.11(12) . . ?
N7 Li3 N10 109.15(14) . . ?
N8 Li3 Li4 114.93(15) . . ?
N12 Li3 Li4 114.88(15) . . ?
N7 Li3 Li4 53.84(10) . . ?
N10 Li3 Li4 55.32(10) . . ?
N8 Li3 C96 128.09(14) . . ?
N12 Li3 C96 59.61(9) . . ?
N7 Li3 C96 134.48(14) . . ?
N10 Li3 C96 30.94(6) . . ?
Li4 Li3 C96 82.76(12) . . ?
N8 Li3 C70 27.79(7) . . ?
N12 Li3 C70 135.43(14) . . ?
N7 Li3 C70 60.86(9) . . ?
N10 Li3 C70 136.32(14) . . ?
Li4 Li3 C70 101.62(13) . . ?
C96 Li3 C70 154.58(13) . . ?
N8 Li3 C65 58.94(9) . . ?
N12 Li3 C65 130.97(14) . . ?
N7 Li3 C65 30.47(7) . . ?
N10 Li3 C65 132.33(14) . . ?
Li4 Li3 C65 80.13(11) . . ?
C96 Li3 C65 162.73(13) . . ?
C70 Li3 C65 31.40(6) . . ?
N11 Li4 N9 122.74(16) . . ?
N11 Li4 N7 130.62(16) . . ?
N9 Li4 N7 87.76(12) . . ?
N11 Li4 N10 86.16(12) . . ?
N9 Li4 N10 125.29(15) . . ?
N7 Li4 N10 107.97(14) . . ?
N11 Li4 Li3 120.32(15) . . ?
N9 Li4 Li3 116.69(14) . . ?
N7 Li4 Li3 53.99(10) . . ?
N10 Li4 Li3 53.99(10) . . ?
N11 Li4 C69 133.40(14) . . ?
N9 Li4 C69 27.90(7) . . ?
N7 Li4 C69 61.12(9) . . ?
N10 Li4 C69 137.75(14) . . ?
Li3 Li4 C69 102.23(12) . . ?
N11 Li4 C68 135.82(14) . . ?
N9 Li4 C68 59.17(9) . . ?
N7 Li4 C68 30.43(7) . . ?
N10 Li4 C68 131.50(14) . . ?
Li3 Li4 C68 80.04(11) . . ?
C69 Li4 C68 31.47(6) . . ?
N11 Li4 C100 26.80(7) . . ?
N9 Li4 C100 131.75(14) . . ?
N7 Li4 C100 139.58(14) . . ?
N10 Li4 C100 59.93(8) . . ?
Li3 Li4 C100 103.17(13) . . ?
C69 Li4 C100 154.47(13) . . ?
C68 Li4 C100 160.26(13) . . ?
N11 Li4 C99 57.64(9) . . ?
N9 Li4 C99 132.00(14) . . ?
N7 Li4 C99 130.77(14) . . ?
N10 Li4 C99 29.46(6) . . ?
Li3 Li4 C99 79.51(11) . . ?
C69 Li4 C99 157.76(13) . . ?
C68 Li4 C99 159.55(13) . . ?
C100 Li4 C99 30.91(6) . . ?
C4 N1 C1 104.79(13) . . ?
C4 N1 Li2 99.49(13) . . ?
C1 N1 Li2 145.22(13) . . ?
C4 N1 Li1 145.80(13) . . ?
C1 N1 Li1 99.33(13) . . ?
Li2 N1 Li1 71.93(12) . . ?
C6 N2 C7 118.08(14) . . ?
C6 N2 Li1 105.15(13) . . ?
C7 N2 Li1 135.83(13) . . ?
C5 N3 C20 117.83(14) . . ?
C5 N3 Li2 105.13(14) . . ?
C20 N3 Li2 136.85(14) . . ?
C36 N4 C33 104.86(13) . . ?
C36 N4 Li2 145.02(13) . . ?
C33 N4 Li2 96.59(12) . . ?
C36 N4 Li1 101.26(12) . . ?
C33 N4 Li1 148.12(13) . . ?
Li2 N4 Li1 70.82(12) . . ?
C38 N5 C39 117.02(14) . . ?
C38 N5 Li2 102.28(13) . . ?
C39 N5 Li2 139.58(13) . . ?
C37 N6 C52 121.71(14) . . ?
C37 N6 Li1 108.37(14) . . ?
C52 N6 Li1 129.20(14) . . ?
C68 N7 C65 104.85(13) . . ?
C68 N7 Li4 99.60(13) . . ?
C65 N7 Li4 145.44(14) . . ?
C68 N7 Li3 144.74(14) . . ?
C65 N7 Li3 99.45(13) . . ?
Li4 N7 Li3 72.18(12) . . ?
C70 N8 C83 117.98(14) . . ?
C70 N8 Li3 104.72(14) . . ?
C83 N8 Li3 136.91(14) . . ?
C69 N9 C71 118.17(14) . . ?
C69 N9 Li4 104.76(14) . . ?
C71 N9 Li4 135.88(13) . . ?
C99 N10 C96 104.79(13) . . ?
C99 N10 Li3 146.11(14) . . ?
C96 N10 Li3 97.41(13) . . ?
C99 N10 Li4 100.63(13) . . ?
C96 N10 Li4 147.58(13) . . ?
Li3 N10 Li4 70.69(12) . . ?
C100 N11 C115 121.36(14) . . ?
C100 N11 Li4 108.21(14) . . ?
C115 N11 Li4 129.44(14) . . ?
C101 N12 C102 116.68(14) . . ?
C101 N12 Li3 102.51(13) . . ?
C102 N12 Li3 139.07(13) . . ?
C132 O2 C135 107.65(18) . . ?
C136 O3 C139 107.17(15) . . ?
N1 C1 C2 111.07(15) . . ?
N1 C1 C6 121.15(14) . . ?
C2 C1 C6 127.67(15) . . ?
N1 C1 Li1 50.19(10) . . ?
C2 C1 Li1 152.30(14) . . ?
C6 C1 Li1 73.45(11) . . ?
C3 C2 C1 106.35(15) . . ?
C3 C2 H2 126.8 . . ?
C1 C2 H2 126.8 . . ?
C2 C3 C4 106.30(15) . . ?
C2 C3 H3 126.8 . . ?
C4 C3 H3 126.8 . . ?
N1 C4 C3 111.48(15) . . ?
N1 C4 C5 121.00(14) . . ?
C3 C4 C5 127.44(15) . . ?
N1 C4 Li2 50.01(10) . . ?
C3 C4 Li2 151.78(14) . . ?
C5 C4 Li2 73.88(11) . . ?
N3 C5 C4 121.20(15) . . ?
N3 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
N2 C6 C1 121.33(15) . . ?
N2 C6 Li1 46.99(10) . . ?
C1 C6 Li1 75.06(11) . . ?
N2 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
Li1 C6 H6 163.6 . . ?
N2 C7 C14 110.40(13) . . ?
N2 C7 C8 109.76(13) . . ?
C14 C7 C8 110.74(13) . . ?
N2 C7 H7 108.6 . . ?
C14 C7 H7 108.6 . . ?
C8 C7 H7 108.6 . . ?
C9 C8 C13 118.28(17) . . ?
C9 C8 C7 119.65(16) . . ?
C13 C8 C7 122.06(16) . . ?
C8 C9 C10 120.5(2) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 119.0(2) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C11 C12 C13 120.4(2) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C8 C13 C12 120.8(2) . . ?
C8 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C15 C14 C19 117.99(16) . . ?
C15 C14 C7 122.17(15) . . ?
C19 C14 C7 119.80(16) . . ?
C14 C15 C16 120.88(17) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C17 C16 C15 120.69(18) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C18 C17 C16 118.96(18) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 120.28(18) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 121.18(18) . . ?
C14 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
N3 C20 C27 107.31(14) . . ?
N3 C20 C21 110.65(14) . . ?
C27 C20 C21 113.54(14) . . ?
N3 C20 H20 108.4 . . ?
C27 C20 H20 108.4 . . ?
C21 C20 H20 108.4 . . ?
C22 C21 C26 117.82(18) . . ?
C22 C21 C20 121.13(16) . . ?
C26 C21 C20 121.00(16) . . ?
C23 C22 C21 121.25(18) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C22 C23 C24 120.7(2) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C25 118.5(2) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
C24 C25 C26 121.1(2) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C21 120.7(2) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C28 C27 C32 118.57(18) . . ?
C28 C27 C20 120.63(18) . . ?
C32 C27 C20 120.77(16) . . ?
C27 C28 C29 120.4(2) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C30 C29 C28 120.6(2) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C29 C30 C31 119.5(2) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C32 120.0(2) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C27 C32 C31 120.78(19) . . ?
C27 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
N4 C33 C34 111.13(14) . . ?
N4 C33 C38 120.81(14) . . ?
C34 C33 C38 128.05(15) . . ?
N4 C33 Li2 52.18(10) . . ?
C34 C33 Li2 150.70(14) . . ?
C38 C33 Li2 73.58(11) . . ?
C35 C34 C33 106.20(15) . . ?
C35 C34 H34 126.9 . . ?
C33 C34 H34 126.9 . . ?
C34 C35 C36 106.40(15) . . ?
C34 C35 H35 126.8 . . ?
C36 C35 H35 126.8 . . ?
N4 C36 C35 111.40(14) . . ?
N4 C36 C37 120.94(15) . . ?
C35 C36 C37 127.47(15) . . ?
N4 C36 Li1 49.37(10) . . ?
C35 C36 Li1 155.46(13) . . ?
C37 C36 Li1 72.64(11) . . ?
N6 C37 C36 121.10(15) . . ?
N6 C37 Li1 44.85(10) . . ?
C36 C37 Li1 76.44(11) . . ?
N6 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
Li1 C37 H37 163.6 . . ?
N5 C38 C33 121.99(15) . . ?
N5 C38 Li2 49.16(10) . . ?
C33 C38 Li2 74.46(11) . . ?
N5 C38 H38 119.0 . . ?
C33 C38 H38 119.0 . . ?
Li2 C38 H38 161.9 . . ?
N5 C39 C40 108.86(13) . . ?
N5 C39 C46 112.18(13) . . ?
C40 C39 C46 108.95(13) . . ?
N5 C39 H39 108.9 . . ?
C40 C39 H39 108.9 . . ?
C46 C39 H39 108.9 . . ?
C41 C40 C45 118.34(18) . . ?
C41 C40 C39 120.36(15) . . ?
C45 C40 C39 121.26(17) . . ?
C42 C41 C40 121.23(18) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C41 C42 C43 119.8(2) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C44 C43 C42 119.9(2) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 120.7(2) . . ?
C43 C44 H44 119.6 . . ?
C45 C44 H44 119.6 . . ?
C40 C45 C44 120.0(2) . . ?
C40 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C51 C46 C47 118.88(18) . . ?
C51 C46 C39 122.16(16) . . ?
C47 C46 C39 118.76(17) . . ?
C48 C47 C46 120.5(2) . . ?
C48 C47 H47 119.8 . . ?
C46 C47 H47 119.8 . . ?
C49 C48 C47 120.1(2) . . ?
C49 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
C48 C49 C50 119.9(2) . . ?
C48 C49 H49 120.0 . . ?
C50 C49 H49 120.0 . . ?
C49 C50 C51 120.4(2) . . ?
C49 C50 H50 119.8 . . ?
C51 C50 H50 119.8 . . ?
C46 C51 C50 120.22(19) . . ?
C46 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
N6 C52 C53 114.02(14) . . ?
N6 C52 C59 109.36(15) . . ?
C53 C52 C59 112.06(15) . . ?
N6 C52 H52 107.0 . . ?
C53 C52 H52 107.0 . . ?
C59 C52 H52 107.0 . . ?
C58 C53 C54 118.90(16) . . ?
C58 C53 C52 121.06(17) . . ?
C54 C53 C52 119.98(17) . . ?
C55 C54 C53 120.75(19) . . ?
C55 C54 H54 119.6 . . ?
C53 C54 H54 119.6 . . ?
C56 C55 C54 119.78(19) . . ?
C56 C55 H55 120.1 . . ?
C54 C55 H55 120.1 . . ?
C55 C56 C57 119.85(17) . . ?
C55 C56 H56 120.1 . . ?
C57 C56 H56 120.1 . . ?
C56 C57 C58 120.20(19) . . ?
C56 C57 H57 119.9 . . ?
C58 C57 H57 119.9 . . ?
C53 C58 C57 120.52(18) . . ?
C53 C58 H58 119.7 . . ?
C57 C58 H58 119.7 . . ?
C64 C59 C60 119.5(2) . . ?
C64 C59 C52 121.64(19) . . ?
C60 C59 C52 118.8(2) . . ?
C59 C60 C61 119.7(3) . . ?
C59 C60 H60 120.2 . . ?
C61 C60 H60 120.2 . . ?
C62 C61 C60 120.4(3) . . ?
C62 C61 H61 119.8 . . ?
C60 C61 H61 119.8 . . ?
C63 C62 C61 119.9(3) . . ?
C63 C62 H62 120.0 . . ?
C61 C62 H62 120.0 . . ?
C62 C63 C64 120.3(3) . . ?
C62 C63 H63 119.8 . . ?
C64 C63 H63 119.8 . . ?
C59 C64 C63 120.2(3) . . ?
C59 C64 H64 119.9 . . ?
C63 C64 H64 119.9 . . ?
N7 C65 C66 111.31(15) . . ?
N7 C65 C70 121.01(15) . . ?
C66 C65 C70 127.57(16) . . ?
N7 C65 Li3 50.08(10) . . ?
C66 C65 Li3 151.37(14) . . ?
C70 C65 Li3 73.84(11) . . ?
C67 C66 C65 106.25(16) . . ?
C67 C66 H66 126.9 . . ?
C65 C66 H66 126.9 . . ?
C66 C67 C68 106.52(15) . . ?
C66 C67 H67 126.7 . . ?
C68 C67 H67 126.7 . . ?
N7 C68 C67 111.06(15) . . ?
N7 C68 C69 121.50(15) . . ?
C67 C68 C69 127.25(16) . . ?
N7 C68 Li4 49.98(10) . . ?
C67 C68 Li4 151.98(14) . . ?
C69 C68 Li4 73.78(11) . . ?
N9 C69 C68 121.51(15) . . ?
N9 C69 Li4 47.34(11) . . ?
C68 C69 Li4 74.75(11) . . ?
N9 C69 H69 119.2 . . ?
C68 C69 H69 119.2 . . ?
Li4 C69 H69 164.3 . . ?
N8 C70 C65 121.50(16) . . ?
N8 C70 Li3 47.49(11) . . ?
C65 C70 Li3 74.76(11) . . ?
N8 C70 H70 119.2 . . ?
C65 C70 H70 119.2 . . ?
Li3 C70 H70 163.9 . . ?
N9 C71 C78 110.32(14) . . ?
N9 C71 C72 108.84(13) . . ?
C78 C71 C72 112.81(14) . . ?
N9 C71 H71 108.3 . . ?
C78 C71 H71 108.3 . . ?
C72 C71 H71 108.3 . . ?
C77 C72 C73 118.03(17) . . ?
C77 C72 C71 123.30(16) . . ?
C73 C72 C71 118.67(15) . . ?
C74 C73 C72 120.78(18) . . ?
C74 C73 H73 119.6 . . ?
C72 C73 H73 119.6 . . ?
C75 C74 C73 120.37(18) . . ?
C75 C74 H74 119.8 . . ?
C73 C74 H74 119.8 . . ?
C76 C75 C74 119.35(19) . . ?
C76 C75 H75 120.3 . . ?
C74 C75 H75 120.3 . . ?
C75 C76 C77 120.6(2) . . ?
C75 C76 H76 119.7 . . ?
C77 C76 H76 119.7 . . ?
C72 C77 C76 120.82(19) . . ?
C72 C77 H77 119.6 . . ?
C76 C77 H77 119.6 . . ?
C160 C78 C79 118.45(17) . . ?
C160 C78 C71 120.96(16) . . ?
C79 C78 C71 120.57(17) . . ?
C78 C79 C80 120.6(2) . . ?
C78 C79 H79 119.7 . . ?
C80 C79 H79 119.7 . . ?
C81 C80 C79 120.5(2) . . ?
C81 C80 H80 119.7 . . ?
C79 C80 H80 119.7 . . ?
C82 C81 C80 119.05(19) . . ?
C82 C81 H81 120.5 . . ?
C80 C81 H81 120.5 . . ?
C81 C82 C160 120.8(2) . . ?
C81 C82 H82 119.6 . . ?
C160 C82 H82 119.6 . . ?
N8 C83 C90 107.57(14) . . ?
N8 C83 C84 110.32(14) . . ?
C90 C83 C84 113.07(14) . . ?
N8 C83 H83 108.6 . . ?
C90 C83 H83 108.6 . . ?
C84 C83 H83 108.6 . . ?
C89 C84 C85 117.79(17) . . ?
C89 C84 C83 121.25(16) . . ?
C85 C84 C83 120.92(16) . . ?
C86 C85 C84 121.24(18) . . ?
C86 C85 H85 119.4 . . ?
C84 C85 H85 119.4 . . ?
C87 C86 C85 120.57(19) . . ?
C87 C86 H86 119.7 . . ?
C85 C86 H86 119.7 . . ?
C86 C87 C88 118.86(19) . . ?
C86 C87 H87 120.6 . . ?
C88 C87 H87 120.6 . . ?
C87 C88 C89 120.59(19) . . ?
C87 C88 H88 119.7 . . ?
C89 C88 H88 119.7 . . ?
C88 C89 C84 120.88(19) . . ?
C88 C89 H89 119.6 . . ?
C84 C89 H89 119.6 . . ?
C91 C90 C95 118.65(19) . . ?
C91 C90 C83 120.83(16) . . ?
C95 C90 C83 120.50(18) . . ?
C92 C91 C90 121.01(19) . . ?
C92 C91 H91 119.5 . . ?
C90 C91 H91 119.5 . . ?
C93 C92 C91 119.9(2) . . ?
C93 C92 H92 120.1 . . ?
C91 C92 H92 120.1 . . ?
C94 C93 C92 119.6(2) . . ?
C94 C93 H93 120.2 . . ?
C92 C93 H93 120.2 . . ?
C93 C94 C95 120.7(2) . . ?
C93 C94 H94 119.7 . . ?
C95 C94 H94 119.7 . . ?
C90 C95 C94 120.2(2) . . ?
C90 C95 H95 119.9 . . ?
C94 C95 H95 119.9 . . ?
N10 C96 C97 111.17(15) . . ?
N10 C96 C101 121.04(14) . . ?
C97 C96 C101 127.78(15) . . ?
N10 C96 Li3 51.65(10) . . ?
C97 C96 Li3 151.74(14) . . ?
C101 C96 Li3 73.30(11) . . ?
C98 C97 C96 106.08(15) . . ?
C98 C97 H97 127.0 . . ?
C96 C97 H97 127.0 . . ?
C97 C98 C99 106.70(15) . . ?
C97 C98 H98 126.6 . . ?
C99 C98 H98 126.6 . . ?
N10 C99 C98 111.25(15) . . ?
N10 C99 C100 121.19(15) . . ?
C98 C99 C100 127.34(15) . . ?
N10 C99 Li4 49.91(10) . . ?
C98 C99 Li4 154.77(14) . . ?
C100 C99 Li4 72.57(11) . . ?
N11 C100 C99 121.29(15) . . ?
N11 C100 Li4 44.99(10) . . ?
C99 C100 Li4 76.52(11) . . ?
N11 C100 H100 119.4 . . ?
C99 C100 H100 119.4 . . ?
Li4 C100 H100 163.6 . . ?
N12 C101 C96 122.58(15) . . ?
N12 C101 H101 118.7 . . ?
C96 C101 H101 118.7 . . ?
N12 C102 C109 111.48(13) . . ?
N12 C102 C103 111.11(14) . . ?
C109 C102 C103 108.98(13) . . ?
N12 C102 H102 108.4 . . ?
C109 C102 H102 108.4 . . ?
C103 C102 H102 108.4 . . ?
C104 C103 C108 117.5(2) . . ?
C104 C103 C102 123.28(18) . . ?
C108 C103 C102 119.2(2) . . ?
C103 C104 C105 120.4(3) . . ?
C103 C104 H104 119.8 . . ?
C105 C104 H104 119.8 . . ?
C106 C105 C104 120.8(3) . . ?
C106 C105 H105 119.6 . . ?
C104 C105 H105 119.6 . . ?
C107 C106 C105 119.6(3) . . ?
C107 C106 H106 120.2 . . ?
C105 C106 H106 120.2 . . ?
C106 C107 C108 120.4(3) . . ?
C106 C107 H107 119.8 . . ?
C108 C107 H107 119.8 . . ?
C103 C108 C107 121.1(3) . . ?
C103 C108 H108 119.4 . . ?
C107 C108 H108 119.4 . . ?
C110 C109 C114 118.96(18) . . ?
C110 C109 C102 120.67(16) . . ?
C114 C109 C102 120.22(17) . . ?
C109 C110 C111 120.4(2) . . ?
C109 C110 H110 119.8 . . ?
C111 C110 H110 119.8 . . ?
C112 C111 C110 120.4(2) . . ?
C112 C111 H111 119.8 . . ?
C110 C111 H111 119.8 . . ?
C113 C112 C111 119.5(2) . . ?
C113 C112 H112 120.3 . . ?
C111 C112 H112 120.3 . . ?
C112 C113 C114 120.5(2) . . ?
C112 C113 H113 119.7 . . ?
C114 C113 H113 119.7 . . ?
C109 C114 C113 120.2(2) . . ?
C109 C114 H114 119.9 . . ?
C113 C114 H114 119.9 . . ?
N11 C115 C122 109.50(15) . . ?
N11 C115 C116 114.78(14) . . ?
C122 C115 C116 112.02(14) . . ?
N11 C115 H115 106.7 . . ?
C122 C115 H115 106.7 . . ?
C116 C115 H115 106.7 . . ?
C121 C116 C117 118.87(16) . . ?
C121 C116 C115 121.12(16) . . ?
C117 C116 C115 120.00(17) . . ?
C116 C117 C118 120.98(18) . . ?
C116 C117 H117 119.5 . . ?
C118 C117 H117 119.5 . . ?
C119 C118 C117 119.72(19) . . ?
C119 C118 H118 120.1 . . ?
C117 C118 H118 120.1 . . ?
C118 C119 C120 119.80(17) . . ?
C118 C119 H119 120.1 . . ?
C120 C119 H119 120.1 . . ?
C119 C120 C121 120.43(19) . . ?
C119 C120 H120 119.8 . . ?
C121 C120 H120 119.8 . . ?
C116 C121 C120 120.20(18) . . ?
C116 C121 H121 119.9 . . ?
C120 C121 H121 119.9 . . ?
C127 C122 C123 118.8(2) . . ?
C127 C122 C115 121.85(19) . . ?
C123 C122 C115 119.3(2) . . ?
C122 C123 C124 119.8(3) . . ?
C122 C123 H123 120.1 . . ?
C124 C123 H123 120.1 . . ?
C125 C124 C123 120.4(3) . . ?
C125 C124 H124 119.8 . . ?
C123 C124 H124 119.8 . . ?
C126 C125 C124 119.6(3) . . ?
C126 C125 H125 120.2 . . ?
C124 C125 H125 120.2 . . ?
C125 C126 C127 121.1(3) . . ?
C125 C126 H126 119.4 . . ?
C127 C126 H126 119.4 . . ?
C122 C127 C126 120.3(3) . . ?
C122 C127 H127 119.9 . . ?
C126 C127 H127 119.9 . . ?
O2 C132 C133 109.0(2) . . ?
O2 C132 H13A 109.9 . . ?
C133 C132 H13A 109.9 . . ?
O2 C132 H13B 109.9 . . ?
C133 C132 H13B 109.9 . . ?
H13A C132 H13B 108.3 . . ?
C132 C133 C134 103.6(2) . . ?
C132 C133 H13C 111.0 . . ?
C134 C133 H13C 111.0 . . ?
C132 C133 H13D 111.0 . . ?
C134 C133 H13D 111.0 . . ?
H13C C133 H13D 109.0 . . ?
C135 C134 C133 101.5(2) . . ?
C135 C134 H13E 111.5 . . ?
C133 C134 H13E 111.5 . . ?
C135 C134 H13F 111.5 . . ?
C133 C134 H13F 111.5 . . ?
H13E C134 H13F 109.3 . . ?
O2 C135 C134 105.9(2) . . ?
O2 C135 H13G 110.6 . . ?
C134 C135 H13G 110.6 . . ?
O2 C135 H13H 110.6 . . ?
C134 C135 H13H 110.6 . . ?
H13G C135 H13H 108.7 . . ?
O3 C136 C137 107.40(19) . . ?
O3 C136 H13I 110.2 . . ?
C137 C136 H13I 110.2 . . ?
O3 C136 H13J 110.2 . . ?
C137 C136 H13J 110.2 . . ?
H13I C136 H13J 108.5 . . ?
C136 C137 C138 105.2(2) . . ?
C136 C137 H13K 110.7 . . ?
C138 C137 H13K 110.7 . . ?
C136 C137 H13L 110.7 . . ?
C138 C137 H13L 110.7 . . ?
H13K C137 H13L 108.8 . . ?
C139 C138 C137 102.47(19) . . ?
C139 C138 H13M 111.3 . . ?
C137 C138 H13M 111.3 . . ?
C139 C138 H13N 111.3 . . ?
C137 C138 H13N 111.3 . . ?
H13M C138 H13N 109.2 . . ?
O3 C139 C138 104.75(17) . . ?
O3 C139 H13O 110.8 . . ?
C138 C139 H13O 110.8 . . ?
O3 C139 H13P 110.8 . . ?
C138 C139 H13P 110.8 . . ?
H13O C139 H13P 108.9 . . ?
C82 C160 C78 120.65(18) . . ?
C82 C160 H160 119.7 . . ?
C78 C160 H160 119.7 . . ?
C1B O0AA C1AA 118.2(7) . . ?
C1AA O0AA C1D 101.6(6) . . ?
C1C C4AA C1AA 106.9(5) . . ?
C1A C4AA C1AA 96.1(6) . . ?
C1A C4AA H4AD 112.5 . . ?
C1AA C4AA H4AD 112.5 . . ?
C1A C4AA H4AC 112.5 . . ?
C1AA C4AA H4AC 112.5 . . ?
H4AD C4AA H4AC 110.1 . . ?
C1C C4AA H4AB 110.3 . . ?
C1AA C4AA H4AB 110.3 . . ?
C1C C4AA H4AA 110.3 . . ?
C1AA C4AA H4AA 110.3 . . ?
H4AB C4AA H4AA 108.6 . . ?
O0AA C1AA C4AA 102.9(5) . . ?
O0AA C1AA H1AA 111.2 . . ?
C4AA C1AA H1AA 111.2 . . ?
O0AA C1AA H1AB 111.2 . . ?
C4AA C1AA H1AB 111.2 . . ?
H1AA C1AA H1AB 109.1 . . ?
C4AA C1A C1D 85.6(7) . . ?
C4AA C1A H1AC 114.4 . . ?
C1D C1A H1AC 114.4 . . ?
C4AA C1A H1AD 114.4 . . ?
C1D C1A H1AD 114.4 . . ?
H1AC C1A H1AD 111.5 . . ?
O0AA C1B C1C 110.0(9) . . ?
O0AA C1B H1BA 109.7 . . ?
C1C C1B H1BA 109.7 . . ?
O0AA C1B H1BB 109.7 . . ?
C1C C1B H1BB 109.7 . . ?
H1BA C1B H1BB 108.2 . . ?
C9AA O5AA C6AA 106.7(5) . . ?
O5AA C9AA C8AA 104.2(5) . . ?
O5AA C9AA H9AA 110.9 . . ?
C8AA C9AA H9AA 110.9 . . ?
O5AA C9AA H9AB 110.9 . . ?
C8AA C9AA H9AB 110.9 . . ?
H9AA C9AA H9AB 108.9 . . ?
O5AA C6AA C0 111.0(5) . . ?
O5AA C6AA H6AA 109.4 . . ?
C0 C6AA H6AA 109.4 . . ?
O5AA C6AA H6AB 109.4 . . ?
C0 C6AA H6AB 109.4 . . ?
H6AA C6AA H6AB 108.0 . . ?
C9AA C8AA C0 103.9(5) . . ?
C9AA C8AA H8AA 111.0 . . ?
C0 C8AA H8AA 111.0 . . ?
C9AA C8AA H8AB 111.0 . . ?
C0 C8AA H8AB 111.0 . . ?
H8AA C8AA H8AB 109.0 . . ?
C6AA C0 C8AA 99.0(5) . . ?
C6AA C0 H0A 112.0 . . ?
C8AA C0 H0A 112.0 . . ?
C6AA C0 H0B 112.0 . . ?
C8AA C0 H0B 112.0 . . ?
H0A C0 H0B 109.6 . . ?
C1B C1C C4AA 101.1(7) . . ?
C1B C1C H1CA 111.5 . . ?
C4AA C1C H1CA 111.5 . . ?
C1B C1C H1CB 111.5 . . ?
C4AA C1C H1CB 111.5 . . ?
H1CA C1C H1CB 109.4 . . ?
O0AA C1D C1A 83.8(7) . . ?
O0AA C1D H1DA 114.7 . . ?
C1A C1D H1DA 114.7 . . ?
O0AA C1D H1DB 114.7 . . ?
C1A C1D H1DB 114.7 . . ?
H1DA C1D H1DB 111.8 . . ?

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
C4 N1 C1 C2 0.52(18) . . . . ?
Li2 N1 C1 C2 -132.3(2) . . . . ?
Li1 N1 C1 C2 156.07(14) . . . . ?
C4 N1 C1 C6 -175.99(14) . . . . ?
Li2 N1 C1 C6 51.2(3) . . . . ?
Li1 N1 C1 C6 -20.44(18) . . . . ?
C4 N1 C1 Li1 -155.55(16) . . . . ?
Li2 N1 C1 Li1 71.7(2) . . . . ?
N1 C1 C2 C3 -0.9(2) . . . . ?
C6 C1 C2 C3 175.32(16) . . . . ?
Li1 C1 C2 C3 41.2(4) . . . . ?
C1 C2 C3 C4 0.9(2) . . . . ?
C1 N1 C4 C3 0.06(18) . . . . ?
Li2 N1 C4 C3 154.94(14) . . . . ?
Li1 N1 C4 C3 -133.3(2) . . . . ?
C1 N1 C4 C5 -176.96(15) . . . . ?
Li2 N1 C4 C5 -22.08(18) . . . . ?
Li1 N1 C4 C5 49.7(3) . . . . ?
C1 N1 C4 Li2 -154.88(15) . . . . ?
Li1 N1 C4 Li2 71.7(2) . . . . ?
C2 C3 C4 N1 -0.6(2) . . . . ?
C2 C3 C4 C5 176.17(17) . . . . ?
C2 C3 C4 Li2 42.7(3) . . . . ?
C20 N3 C5 C4 -174.70(15) . . . . ?
Li2 N3 C5 C4 9.5(2) . . . . ?
N1 C4 C5 N3 10.3(2) . . . . ?
C3 C4 C5 N3 -166.25(17) . . . . ?
Li2 C4 C5 N3 -7.19(16) . . . . ?
C7 N2 C6 C1 -178.04(14) . . . . ?
Li1 N2 C6 C1 11.31(19) . . . . ?
C7 N2 C6 Li1 170.65(19) . . . . ?
N1 C1 C6 N2 7.7(2) . . . . ?
C2 C1 C6 N2 -168.17(17) . . . . ?
Li1 C1 C6 N2 -8.54(15) . . . . ?
N1 C1 C6 Li1 16.25(14) . . . . ?
C2 C1 C6 Li1 -159.63(19) . . . . ?
C6 N2 C7 C14 119.18(15) . . . . ?
Li1 N2 C7 C14 -73.8(2) . . . . ?
C6 N2 C7 C8 -118.47(15) . . . . ?
Li1 N2 C7 C8 48.5(2) . . . . ?
N2 C7 C8 C9 97.57(19) . . . . ?
C14 C7 C8 C9 -140.28(17) . . . . ?
N2 C7 C8 C13 -83.3(2) . . . . ?
C14 C7 C8 C13 38.8(2) . . . . ?
C13 C8 C9 C10 -1.9(3) . . . . ?
C7 C8 C9 C10 177.3(2) . . . . ?
C8 C9 C10 C11 1.0(4) . . . . ?
C9 C10 C11 C12 0.5(4) . . . . ?
C10 C11 C12 C13 -1.0(4) . . . . ?
C9 C8 C13 C12 1.4(3) . . . . ?
C7 C8 C13 C12 -177.7(2) . . . . ?
C11 C12 C13 C8 0.0(4) . . . . ?
N2 C7 C14 C15 27.8(2) . . . . ?
C8 C7 C14 C15 -93.98(19) . . . . ?
N2 C7 C14 C19 -154.46(16) . . . . ?
C8 C7 C14 C19 83.8(2) . . . . ?
C19 C14 C15 C16 -0.6(3) . . . . ?
C7 C14 C15 C16 177.19(17) . . . . ?
C14 C15 C16 C17 -0.7(3) . . . . ?
C15 C16 C17 C18 1.2(3) . . . . ?
C16 C17 C18 C19 -0.5(3) . . . . ?
C15 C14 C19 C18 1.3(3) . . . . ?
C7 C14 C19 C18 -176.51(19) . . . . ?
C17 C18 C19 C14 -0.8(3) . . . . ?
C5 N3 C20 C27 96.39(18) . . . . ?
Li2 N3 C20 C27 -89.5(2) . . . . ?
C5 N3 C20 C21 -139.25(16) . . . . ?
Li2 N3 C20 C21 34.8(2) . . . . ?
N3 C20 C21 C22 26.3(2) . . . . ?
C27 C20 C21 C22 147.08(17) . . . . ?
N3 C20 C21 C26 -156.43(17) . . . . ?
C27 C20 C21 C26 -35.7(2) . . . . ?
C26 C21 C22 C23 2.2(3) . . . . ?
C20 C21 C22 C23 179.47(17) . . . . ?
C21 C22 C23 C24 -1.0(3) . . . . ?
C22 C23 C24 C25 -0.8(3) . . . . ?
C23 C24 C25 C26 1.3(3) . . . . ?
C24 C25 C26 C21 -0.1(3) . . . . ?
C22 C21 C26 C25 -1.6(3) . . . . ?
C20 C21 C26 C25 -178.94(19) . . . . ?
N3 C20 C27 C28 -119.91(19) . . . . ?
C21 C20 C27 C28 117.5(2) . . . . ?
N3 C20 C27 C32 58.0(2) . . . . ?
C21 C20 C27 C32 -64.6(2) . . . . ?
C32 C27 C28 C29 -0.1(3) . . . . ?
C20 C27 C28 C29 177.9(2) . . . . ?
C27 C28 C29 C30 -0.6(4) . . . . ?
C28 C29 C30 C31 0.5(4) . . . . ?
C29 C30 C31 C32 0.3(4) . . . . ?
C28 C27 C32 C31 0.9(3) . . . . ?
C20 C27 C32 C31 -177.11(17) . . . . ?
C30 C31 C32 C27 -1.0(3) . . . . ?
C36 N4 C33 C34 -0.06(19) . . . . ?
Li2 N4 C33 C34 152.07(15) . . . . ?
Li1 N4 C33 C34 -144.1(2) . . . . ?
C36 N4 C33 C38 179.46(15) . . . . ?
Li2 N4 C33 C38 -28.41(18) . . . . ?
Li1 N4 C33 C38 35.4(3) . . . . ?
C36 N4 C33 Li2 -152.13(15) . . . . ?
Li1 N4 C33 Li2 63.9(2) . . . . ?
N4 C33 C34 C35 -0.3(2) . . . . ?
C38 C33 C34 C35 -179.82(17) . . . . ?
Li2 C33 C34 C35 48.8(3) . . . . ?
C33 C34 C35 C36 0.6(2) . . . . ?
C33 N4 C36 C35 0.45(19) . . . . ?
Li2 N4 C36 C35 -125.4(2) . . . . ?
Li1 N4 C36 C35 162.01(14) . . . . ?
C33 N4 C36 C37 -174.96(15) . . . . ?
Li2 N4 C36 C37 59.1(3) . . . . ?
Li1 N4 C36 C37 -13.41(19) . . . . ?
C33 N4 C36 Li1 -161.56(16) . . . . ?
Li2 N4 C36 Li1 72.5(2) . . . . ?
C34 C35 C36 N4 -0.7(2) . . . . ?
C34 C35 C36 C37 174.37(17) . . . . ?
C34 C35 C36 Li1 33.7(4) . . . . ?
C52 N6 C37 C36 177.17(16) . . . . ?
Li1 N6 C37 C36 6.1(2) . . . . ?
C52 N6 C37 Li1 171.1(2) . . . . ?
N4 C36 C37 N6 6.2(3) . . . . ?
C35 C36 C37 N6 -168.42(17) . . . . ?
Li1 C36 C37 N6 -4.42(16) . . . . ?
N4 C36 C37 Li1 10.62(15) . . . . ?
C35 C36 C37 Li1 -164.00(19) . . . . ?
C39 N5 C38 C33 -172.99(15) . . . . ?
Li2 N5 C38 C33 16.7(2) . . . . ?
C39 N5 C38 Li2 170.27(19) . . . . ?
N4 C33 C38 N5 10.0(3) . . . . ?
C34 C33 C38 N5 -170.57(17) . . . . ?
Li2 C33 C38 N5 -13.07(16) . . . . ?
N4 C33 C38 Li2 23.07(15) . . . . ?
C34 C33 C38 Li2 -157.5(2) . . . . ?
C38 N5 C39 C40 96.26(17) . . . . ?
Li2 N5 C39 C40 -98.5(2) . . . . ?
C38 N5 C39 C46 -143.10(15) . . . . ?
Li2 N5 C39 C46 22.1(3) . . . . ?
N5 C39 C40 C41 42.9(2) . . . . ?
C46 C39 C40 C41 -79.7(2) . . . . ?
N5 C39 C40 C45 -139.63(18) . . . . ?
C46 C39 C40 C45 97.8(2) . . . . ?
C45 C40 C41 C42 -0.3(3) . . . . ?
C39 C40 C41 C42 177.25(19) . . . . ?
C40 C41 C42 C43 0.7(4) . . . . ?
C41 C42 C43 C44 -1.1(4) . . . . ?
C42 C43 C44 C45 1.1(4) . . . . ?
C41 C40 C45 C44 0.3(3) . . . . ?
C39 C40 C45 C44 -177.2(2) . . . . ?
C43 C44 C45 C40 -0.7(4) . . . . ?
N5 C39 C46 C51 -47.3(2) . . . . ?
C40 C39 C46 C51 73.30(19) . . . . ?
N5 C39 C46 C47 137.85(16) . . . . ?
C40 C39 C46 C47 -101.56(18) . . . . ?
C51 C46 C47 C48 -0.8(3) . . . . ?
C39 C46 C47 C48 174.20(17) . . . . ?
C46 C47 C48 C49 0.6(3) . . . . ?
C47 C48 C49 C50 0.1(3) . . . . ?
C48 C49 C50 C51 -0.6(3) . . . . ?
C47 C46 C51 C50 0.3(3) . . . . ?
C39 C46 C51 C50 -174.56(17) . . . . ?
C49 C50 C51 C46 0.4(3) . . . . ?
C37 N6 C52 C53 17.3(2) . . . . ?
Li1 N6 C52 C53 -173.69(16) . . . . ?
C37 N6 C52 C59 143.60(17) . . . . ?
Li1 N6 C52 C59 -47.4(2) . . . . ?
N6 C52 C53 C58 74.5(2) . . . . ?
C59 C52 C53 C58 -50.4(2) . . . . ?
N6 C52 C53 C54 -102.6(2) . . . . ?
C59 C52 C53 C54 132.48(19) . . . . ?
C58 C53 C54 C55 0.4(3) . . . . ?
C52 C53 C54 C55 177.57(17) . . . . ?
C53 C54 C55 C56 -0.6(3) . . . . ?
C54 C55 C56 C57 0.2(3) . . . . ?
C55 C56 C57 C58 0.3(3) . . . . ?
C54 C53 C58 C57 0.0(3) . . . . ?
C52 C53 C58 C57 -177.07(17) . . . . ?
C56 C57 C58 C53 -0.4(3) . . . . ?
N6 C52 C59 C64 -34.7(2) . . . . ?
C53 C52 C59 C64 92.7(2) . . . . ?
N6 C52 C59 C60 146.10(17) . . . . ?
C53 C52 C59 C60 -86.5(2) . . . . ?
C64 C59 C60 C61 -0.1(3) . . . . ?
C52 C59 C60 C61 179.11(19) . . . . ?
C59 C60 C61 C62 -0.4(4) . . . . ?
C60 C61 C62 C63 0.3(4) . . . . ?
C61 C62 C63 C64 0.3(4) . . . . ?
C60 C59 C64 C63 0.6(3) . . . . ?
C52 C59 C64 C63 -178.6(2) . . . . ?
C62 C63 C64 C59 -0.7(4) . . . . ?
C68 N7 C65 C66 -0.20(18) . . . . ?
Li4 N7 C65 C66 133.3(2) . . . . ?
Li3 N7 C65 C66 -154.43(15) . . . . ?
C68 N7 C65 C70 176.35(15) . . . . ?
Li4 N7 C65 C70 -50.1(3) . . . . ?
Li3 N7 C65 C70 22.13(19) . . . . ?
C68 N7 C65 Li3 154.23(16) . . . . ?
Li4 N7 C65 Li3 -72.2(2) . . . . ?
N7 C65 C66 C67 0.7(2) . . . . ?
C70 C65 C66 C67 -175.54(17) . . . . ?
Li3 C65 C66 C67 -43.0(3) . . . . ?
C65 C66 C67 C68 -0.9(2) . . . . ?
C65 N7 C68 C67 -0.41(18) . . . . ?
Li4 N7 C68 C67 -155.77(15) . . . . ?
Li3 N7 C68 C67 131.6(2) . . . . ?
C65 N7 C68 C69 174.90(15) . . . . ?
Li4 N7 C68 C69 19.54(19) . . . . ?
Li3 N7 C68 C69 -53.1(3) . . . . ?
C65 N7 C68 Li4 155.36(16) . . . . ?
Li3 N7 C68 Li4 -72.6(2) . . . . ?
C66 C67 C68 N7 0.9(2) . . . . ?
C66 C67 C68 C69 -174.11(17) . . . . ?
C66 C67 C68 Li4 -41.1(4) . . . . ?
C71 N9 C69 C68 -179.61(14) . . . . ?
Li4 N9 C69 C68 -10.1(2) . . . . ?
C71 N9 C69 Li4 -169.48(19) . . . . ?
N7 C68 C69 N9 -7.8(2) . . . . ?
C67 C68 C69 N9 166.74(17) . . . . ?
Li4 C68 C69 N9 7.71(15) . . . . ?
N7 C68 C69 Li4 -15.47(15) . . . . ?
C67 C68 C69 Li4 159.03(19) . . . . ?
C83 N8 C70 C65 174.55(15) . . . . ?
Li3 N8 C70 C65 -11.4(2) . . . . ?
C83 N8 C70 Li3 -174.0(2) . . . . ?
N7 C65 C70 N8 -8.8(3) . . . . ?
C66 C65 C70 N8 167.16(17) . . . . ?
Li3 C65 C70 N8 8.71(16) . . . . ?
N7 C65 C70 Li3 -17.50(15) . . . . ?
C66 C65 C70 Li3 158.45(19) . . . . ?
C69 N9 C71 C78 -121.71(16) . . . . ?
Li4 N9 C71 C78 73.0(2) . . . . ?
C69 N9 C71 C72 114.02(16) . . . . ?
Li4 N9 C71 C72 -51.3(2) . . . . ?
N9 C71 C72 C77 107.7(2) . . . . ?
C78 C71 C72 C77 -15.1(3) . . . . ?
N9 C71 C72 C73 -71.92(19) . . . . ?
C78 C71 C72 C73 165.29(16) . . . . ?
C77 C72 C73 C74 1.5(3) . . . . ?
C71 C72 C73 C74 -178.87(17) . . . . ?
C72 C73 C74 C75 -0.1(3) . . . . ?
C73 C74 C75 C76 -1.5(3) . . . . ?
C74 C75 C76 C77 1.6(4) . . . . ?
C73 C72 C77 C76 -1.3(3) . . . . ?
C71 C72 C77 C76 179.0(2) . . . . ?
C75 C76 C77 C72 -0.2(4) . . . . ?
N9 C71 C78 C160 -32.8(2) . . . . ?
C72 C71 C78 C160 89.2(2) . . . . ?
N9 C71 C78 C79 148.63(17) . . . . ?
C72 C71 C78 C79 -89.4(2) . . . . ?
C160 C78 C79 C80 0.7(3) . . . . ?
C71 C78 C79 C80 179.32(18) . . . . ?
C78 C79 C80 C81 0.6(3) . . . . ?
C79 C80 C81 C82 -0.9(3) . . . . ?
C80 C81 C82 C160 0.1(3) . . . . ?
C70 N8 C83 C90 -97.51(18) . . . . ?
Li3 N8 C83 C90 91.0(2) . . . . ?
C70 N8 C83 C84 138.74(16) . . . . ?
Li3 N8 C83 C84 -32.8(3) . . . . ?
N8 C83 C84 C89 155.16(16) . . . . ?
C90 C83 C84 C89 34.7(2) . . . . ?
N8 C83 C84 C85 -27.2(2) . . . . ?
C90 C83 C84 C85 -147.69(17) . . . . ?
C89 C84 C85 C86 -2.5(3) . . . . ?
C83 C84 C85 C86 179.79(17) . . . . ?
C84 C85 C86 C87 1.3(3) . . . . ?
C85 C86 C87 C88 0.8(3) . . . . ?
C86 C87 C88 C89 -1.6(3) . . . . ?
C87 C88 C89 C84 0.4(3) . . . . ?
C85 C84 C89 C88 1.6(3) . . . . ?
C83 C84 C89 C88 179.35(18) . . . . ?
N8 C83 C90 C91 -57.4(2) . . . . ?
C84 C83 C90 C91 64.7(2) . . . . ?
N8 C83 C90 C95 121.24(19) . . . . ?
C84 C83 C90 C95 -116.70(19) . . . . ?
C95 C90 C91 C92 -0.5(3) . . . . ?
C83 C90 C91 C92 178.15(17) . . . . ?
C90 C91 C92 C93 0.9(3) . . . . ?
C91 C92 C93 C94 -0.6(3) . . . . ?
C92 C93 C94 C95 0.0(4) . . . . ?
C91 C90 C95 C94 -0.1(3) . . . . ?
C83 C90 C95 C94 -178.8(2) . . . . ?
C93 C94 C95 C90 0.3(4) . . . . ?
C99 N10 C96 C97 0.26(19) . . . . ?
Li3 N10 C96 C97 -153.91(15) . . . . ?
Li4 N10 C96 C97 140.7(2) . . . . ?
C99 N10 C96 C101 179.49(15) . . . . ?
Li3 N10 C96 C101 25.32(19) . . . . ?
Li4 N10 C96 C101 -40.0(3) . . . . ?
C99 N10 C96 Li3 154.17(16) . . . . ?
Li4 N10 C96 Li3 -65.3(2) . . . . ?
N10 C96 C97 C98 0.1(2) . . . . ?
C101 C96 C97 C98 -179.02(17) . . . . ?
Li3 C96 C97 C98 -46.6(4) . . . . ?
C96 C97 C98 C99 -0.5(2) . . . . ?
C96 N10 C99 C98 -0.58(19) . . . . ?
Li3 N10 C99 C98 128.6(2) . . . . ?
Li4 N10 C99 C98 -160.27(15) . . . . ?
C96 N10 C99 C100 174.39(15) . . . . ?
Li3 N10 C99 C100 -56.4(3) . . . . ?
Li4 N10 C99 C100 14.70(19) . . . . ?
C96 N10 C99 Li4 159.69(17) . . . . ?
Li3 N10 C99 Li4 -71.1(2) . . . . ?
C97 C98 C99 N10 0.7(2) . . . . ?
C97 C98 C99 C100 -173.91(17) . . . . ?
C97 C98 C99 Li4 -36.6(4) . . . . ?
C115 N11 C100 C99 -176.01(16) . . . . ?
Li4 N11 C100 C99 -6.4(2) . . . . ?
C115 N11 C100 Li4 -169.6(2) . . . . ?
N10 C99 C100 N11 -7.1(3) . . . . ?
C98 C99 C100 N11 167.01(18) . . . . ?
Li4 C99 C100 N11 4.65(16) . . . . ?
N10 C99 C100 Li4 -11.74(16) . . . . ?
C98 C99 C100 Li4 162.36(19) . . . . ?
C102 N12 C101 C96 175.97(15) . . . . ?
Li3 N12 C101 C96 -16.2(2) . . . . ?
N10 C96 C101 N12 -7.9(3) . . . . ?
C97 C96 C101 N12 171.18(18) . . . . ?
Li3 C96 C101 N12 12.58(16) . . . . ?
C101 N12 C102 C109 149.76(15) . . . . ?
Li3 N12 C102 C109 -12.0(3) . . . . ?
C101 N12 C102 C103 -88.46(18) . . . . ?
Li3 N12 C102 C103 109.8(2) . . . . ?
N12 C102 C103 C104 -15.4(3) . . . . ?
C109 C102 C103 C104 107.8(2) . . . . ?
N12 C102 C103 C108 164.99(19) . . . . ?
C109 C102 C103 C108 -71.8(2) . . . . ?
C108 C103 C104 C105 -0.8(4) . . . . ?
C102 C103 C104 C105 179.6(2) . . . . ?
C103 C104 C105 C106 2.7(5) . . . . ?
C104 C105 C106 C107 -2.2(5) . . . . ?
C105 C106 C107 C108 -0.1(6) . . . . ?
C104 C103 C108 C107 -1.5(4) . . . . ?
C102 C103 C108 C107 178.1(3) . . . . ?
C106 C107 C108 C103 2.0(5) . . . . ?
N12 C102 C109 C110 48.2(2) . . . . ?
C103 C102 C109 C110 -74.8(2) . . . . ?
N12 C102 C109 C114 -136.40(16) . . . . ?
C103 C102 C109 C114 100.59(19) . . . . ?
C114 C109 C110 C111 0.1(3) . . . . ?
C102 C109 C110 C111 175.60(17) . . . . ?
C109 C110 C111 C112 -0.5(3) . . . . ?
C110 C111 C112 C113 0.6(3) . . . . ?
C111 C112 C113 C114 -0.3(3) . . . . ?
C110 C109 C114 C113 0.2(3) . . . . ?
C102 C109 C114 C113 -175.27(17) . . . . ?
C112 C113 C114 C109 -0.1(3) . . . . ?
C100 N11 C115 C122 -146.87(17) . . . . ?
Li4 N11 C115 C122 45.9(2) . . . . ?
C100 N11 C115 C116 -19.9(2) . . . . ?
Li4 N11 C115 C116 172.93(16) . . . . ?
N11 C115 C116 C121 -71.5(2) . . . . ?
C122 C115 C116 C121 54.2(2) . . . . ?
N11 C115 C116 C117 107.43(19) . . . . ?
C122 C115 C116 C117 -126.89(19) . . . . ?
C121 C116 C117 C118 -0.5(3) . . . . ?
C115 C116 C117 C118 -179.40(16) . . . . ?
C116 C117 C118 C119 1.0(3) . . . . ?
C117 C118 C119 C120 -0.5(3) . . . . ?
C118 C119 C120 C121 -0.3(3) . . . . ?
C117 C116 C121 C120 -0.4(3) . . . . ?
C115 C116 C121 C120 178.50(17) . . . . ?
C119 C120 C121 C116 0.8(3) . . . . ?
N11 C115 C122 C127 33.7(2) . . . . ?
C116 C115 C122 C127 -94.8(2) . . . . ?
N11 C115 C122 C123 -147.76(17) . . . . ?
C116 C115 C122 C123 83.7(2) . . . . ?
C127 C122 C123 C124 -1.2(3) . . . . ?
C115 C122 C123 C124 -179.74(18) . . . . ?
C122 C123 C124 C125 1.2(4) . . . . ?
C123 C124 C125 C126 -0.6(5) . . . . ?
C124 C125 C126 C127 -0.1(5) . . . . ?
C123 C122 C127 C126 0.5(4) . . . . ?
C115 C122 C127 C126 179.0(2) . . . . ?
C125 C126 C127 C122 0.1(5) . . . . ?
C135 O2 C132 C133 8.8(3) . . . . ?
O2 C132 C133 C134 13.5(4) . . . . ?
C132 C133 C134 C135 -29.1(3) . . . . ?
C132 O2 C135 C134 -28.2(3) . . . . ?
C133 C134 C135 O2 35.4(3) . . . . ?
C139 O3 C136 C137 -21.0(3) . . . . ?
O3 C136 C137 C138 -1.5(3) . . . . ?
C136 C137 C138 C139 21.8(3) . . . . ?
C136 O3 C139 C138 35.3(2) . . . . ?
C137 C138 C139 O3 -34.9(2) . . . . ?
C81 C82 C160 C78 1.2(3) . . . . ?
C79 C78 C160 C82 -1.5(3) . . . . ?
C71 C78 C160 C82 179.85(16) . . . . ?
C1B O0AA C1AA C4AA -4.8(12) . . . . ?
C1D O0AA C1AA C4AA -33.8(8) . . . . ?
C1C C4AA C1AA O0AA 8.7(9) . . . . ?
C1A C4AA C1AA O0AA -20.1(8) . . . . ?
C1AA C4AA C1A C1D 56.1(8) . . . . ?
C1AA O0AA C1B C1C -1.3(17) . . . . ?
C6AA O5AA C9AA C8AA -37.7(7) . . . . ?
C9AA O5AA C6AA C0 23.0(7) . . . . ?
O5AA C9AA C8AA C0 38.0(6) . . . . ?
O5AA C6AA C0 C8AA 1.2(7) . . . . ?
C9AA C8AA C0 C6AA -22.7(6) . . . . ?
O0AA C1B C1C C4AA 6.7(15) . . . . ?
C1AA C4AA C1C C1B -9.2(12) . . . . ?
C1AA O0AA C1D C1A 67.9(8) . . . . ?
C4AA C1A C1D O0AA -75.1(8) . . . . ?

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
C6 H6 O2 0.93 2.63 3.315(2) 130.9 1_665
C69 H69 O3 0.93 2.60 3.288(2) 130.7 1_455

_refine_diff_density_max         0.491
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.049



####################################################################### 
# 
# 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_2-H
_database_code_depnum_ccdc_archive 'CCDC 1476169'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-08-18 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         'C26 H35 N3'
_chemical_formula_sum            'C26 H35 N3'
_chemical_formula_weight         389.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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      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                   25.4797(19)
_cell_length_b                   6.8484(4)
_cell_length_c                   27.753(2)
_cell_angle_alpha                90
_cell_angle_beta                 112.294(8)
_cell_angle_gamma                90
_cell_volume                     4480.8(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3433
_cell_measurement_theta_min      3.4395
_cell_measurement_theta_max      71.3236

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.514
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8805
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.442
_diffrn_reflns_theta_max         71.464
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4286
_reflns_number_gt                3079
_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)+(0.1686P)²+8.0414P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00066(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4286
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0855
_refine_ls_wR_factor_ref         0.3061
_refine_ls_wR_factor_gt          0.2789
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_restrained_S_all      0.936
_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
N1 N 0.01378(10) 0.0412(4) 0.13979(10) 0.0646(7) Uani 1 1 d . . . . .
H1 H 0.0018 0.1559 0.1282 0.078 Uiso 1 1 calc R U . . .
N2 N -0.07707(11) 0.1564(4) 0.16902(10) 0.0621(7) Uani 1 1 d . . . . .
N3 N 0.07169(11) 0.1881(4) 0.07823(11) 0.0697(8) Uani 1 1 d . . . . .
C1 C 0.05642(13) -0.0559(5) 0.13144(12) 0.0667(8) Uani 1 1 d . . . . .
C2 C 0.06257(15) -0.2326(6) 0.15621(13) 0.0762(10) Uani 1 1 d . . . . .
H2 H 0.0885 -0.3295 0.1571 0.091 Uiso 1 1 calc R U . . .
C3 C 0.02299(15) -0.2414(5) 0.17990(13) 0.0729(9) Uani 1 1 d . . . . .
H3 H 0.0179 -0.3449 0.1994 0.087 Uiso 1 1 calc R U . . .
C4 C -0.00699(13) -0.0700(5) 0.16918(11) 0.0636(8) Uani 1 1 d . . . . .
C5 C -0.05307(12) -0.0059(5) 0.18344(11) 0.0611(8) Uani 1 1 d . . . . .
H5 H -0.0654 -0.0870 0.2039 0.073 Uiso 1 1 calc R U . . .
C6 C 0.08489(13) 0.0242(5) 0.09992(12) 0.0686(9) Uani 1 1 d . . . . .
H6 H 0.1138 -0.0472 0.0955 0.082 Uiso 1 1 calc R U . . .
C7 C -0.12400(12) 0.2171(4) 0.18417(11) 0.0543(7) Uani 1 1 d . . . . .
C8 C -0.13959(15) 0.0751(5) 0.21937(15) 0.0738(9) Uani 1 1 d . . . . .
H8A H -0.1067 0.0523 0.2511 0.089 Uiso 1 1 calc R U . . .
H8B H -0.1512 -0.0489 0.2017 0.089 Uiso 1 1 calc R U . . .
C9 C -0.18894(16) 0.1613(6) 0.23333(17) 0.0832(11) Uani 1 1 d . . . . .
H9 H -0.1986 0.0719 0.2563 0.100 Uiso 1 1 calc R U . . .
C10 C -0.16892(19) 0.3540(7) 0.25999(16) 0.0934(12) Uani 1 1 d . . . . .
H10A H -0.1978 0.4071 0.2711 0.112 Uiso 1 1 calc R U . . .
H10B H -0.1349 0.3333 0.2908 0.112 Uiso 1 1 calc R U . . .
C11 C -0.23912(17) 0.1873(7) 0.18235(18) 0.0945(12) Uani 1 1 d . . . . .
H11A H -0.2490 0.0622 0.1648 0.113 Uiso 1 1 calc R U . . .
H11B H -0.2715 0.2333 0.1894 0.113 Uiso 1 1 calc R U . . .
C12 C -0.15658(18) 0.4978(6) 0.22536(16) 0.0848(11) Uani 1 1 d . . . . .
H12 H -0.1454 0.6237 0.2431 0.102 Uiso 1 1 calc R U . . .
C13 C -0.10746(15) 0.4118(5) 0.21187(16) 0.0789(10) Uani 1 1 d . . . . .
H13A H -0.0977 0.5027 0.1898 0.095 Uiso 1 1 calc R U . . .
H13B H -0.0743 0.3945 0.2436 0.095 Uiso 1 1 calc R U . . .
C14 C -0.22618(15) 0.3291(6) 0.14776(15) 0.0840(11) Uani 1 1 d . . . . .
H14 H -0.2596 0.3480 0.1157 0.101 Uiso 1 1 calc R U . . .
C15 C -0.17600(15) 0.2462(6) 0.13464(14) 0.0793(10) Uani 1 1 d . . . . .
H15A H -0.1870 0.1225 0.1166 0.095 Uiso 1 1 calc R U . . .
H15B H -0.1671 0.3362 0.1118 0.095 Uiso 1 1 calc R U . . .
C16 C 0.09936(12) 0.2653(5) 0.04431(12) 0.0593(8) Uani 1 1 d . . . . .
C17 C 0.05664(19) 0.2566(9) -0.01064(16) 0.1120(18) Uani 1 1 d . . . . .
H17A H 0.0215 0.3172 -0.0126 0.134 Uiso 1 1 calc R U . . .
H17B H 0.0488 0.1216 -0.0215 0.134 Uiso 1 1 calc R U . . .
C18 C 0.1148(2) 0.4734(6) 0.05989(19) 0.0960(13) Uani 1 1 d . . . . .
H18A H 0.1417 0.4784 0.0956 0.115 Uiso 1 1 calc R U . . .
H18B H 0.0811 0.5450 0.0578 0.115 Uiso 1 1 calc R U . . .
C19 C 0.15227(19) 0.1587(8) 0.0458(2) 0.1086(16) Uani 1 1 d . . . . .
H19A H 0.1431 0.0233 0.0360 0.130 Uiso 1 1 calc R U . . .
H19B H 0.1808 0.1617 0.0810 0.130 Uiso 1 1 calc R U . . .
C20 C 0.1761(2) 0.2556(7) 0.0082(2) 0.1068(16) Uani 1 1 d . . . . .
H20 H 0.2099 0.1851 0.0092 0.128 Uiso 1 1 calc R U . . .
C21 C 0.19094(19) 0.4592(9) 0.0244(2) 0.1156(17) Uani 1 1 d . . . . .
H21A H 0.2063 0.5212 0.0012 0.139 Uiso 1 1 calc R U . . .
H21B H 0.2200 0.4616 0.0593 0.139 Uiso 1 1 calc R U . . .
C22 C 0.1321(3) 0.2508(9) -0.0457(2) 0.135(2) Uani 1 1 d . . . . .
H22A H 0.1211 0.1168 -0.0559 0.162 Uiso 1 1 calc R U . . .
H22B H 0.1475 0.3054 -0.0698 0.162 Uiso 1 1 calc R U . . .
C23 C 0.1409(3) 0.5693(7) 0.0238(2) 0.1143(16) Uani 1 1 d . . . . .
H23 H 0.1521 0.7037 0.0352 0.137 Uiso 1 1 calc R U . . .
C24 C 0.0809(2) 0.3676(13) -0.04792(17) 0.131(2) Uani 1 1 d . . . . .
H24 H 0.0525 0.3713 -0.0836 0.158 Uiso 1 1 calc R U . . .
C25 C 0.0976(3) 0.5710(10) -0.0276(3) 0.129(2) Uani 1 1 d . . . . .
H25A H 0.1112 0.6410 -0.0509 0.154 Uiso 1 1 calc R U . . .
H25B H 0.0645 0.6394 -0.0269 0.154 Uiso 1 1 calc R U . . .
C26 C -0.20639(17) 0.5233(6) 0.17462(16) 0.0858(11) Uani 1 1 d . . . . .
H26A H -0.1957 0.6085 0.1519 0.103 Uiso 1 1 calc R U . . .
H26B H -0.2373 0.5849 0.1812 0.103 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
N1 C4 1.361(4) . ?
N1 C1 1.366(4) . ?
N1 H1 0.8600 . ?
N2 C5 1.259(4) . ?
N2 C7 1.470(4) . ?
N3 C6 1.258(4) . ?
N3 C16 1.472(4) . ?
C1 C2 1.371(5) . ?
C1 C6 1.440(5) . ?
C2 C3 1.399(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.370(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.443(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C13 1.516(4) . ?
C7 C15 1.518(4) . ?
C7 C8 1.534(4) . ?
C8 C9 1.565(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.505(6) . ?
C9 C11 1.515(6) . ?
C9 H9 0.9800 . ?
C10 C12 1.491(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C14 1.488(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C26 1.506(5) . ?
C12 C13 1.552(5) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C26 1.515(6) . ?
C14 C15 1.563(5) . ?
C14 H14 0.9800 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C18 1.497(5) . ?
C16 C17 1.502(5) . ?
C16 C19 1.520(4) . ?
C17 C24 1.585(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C23 1.545(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.543(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.471(7) . ?
C20 C22 1.490(8) . ?
C20 H20 0.9800 . ?
C21 C23 1.475(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C24 1.512(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C25 1.435(8) . ?
C23 H23 0.9800 . ?
C24 C25 1.502(9) . ?
C24 H24 0.9800 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?

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
C4 N1 C1 110.1(3) . . ?
C4 N1 H1 124.9 . . ?
C1 N1 H1 124.9 . . ?
C5 N2 C7 120.6(3) . . ?
C6 N3 C16 121.4(3) . . ?
N1 C1 C2 106.9(3) . . ?
N1 C1 C6 122.3(3) . . ?
C2 C1 C6 130.7(3) . . ?
C1 C2 C3 107.9(3) . . ?
C1 C2 H2 126.0 . . ?
C3 C2 H2 126.0 . . ?
C4 C3 C2 107.6(3) . . ?
C4 C3 H3 126.2 . . ?
C2 C3 H3 126.2 . . ?
N1 C4 C3 107.3(3) . . ?
N1 C4 C5 122.4(3) . . ?
C3 C4 C5 130.2(3) . . ?
N2 C5 C4 122.0(3) . . ?
N2 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
N3 C6 C1 121.7(3) . . ?
N3 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
N2 C7 C13 107.1(2) . . ?
N2 C7 C15 107.7(2) . . ?
C13 C7 C15 108.9(3) . . ?
N2 C7 C8 116.0(3) . . ?
C13 C7 C8 108.9(3) . . ?
C15 C7 C8 108.2(3) . . ?
C7 C8 C9 110.2(3) . . ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C11 111.4(3) . . ?
C10 C9 C8 107.3(3) . . ?
C11 C9 C8 106.6(3) . . ?
C10 C9 H9 110.5 . . ?
C11 C9 H9 110.5 . . ?
C8 C9 H9 110.5 . . ?
C12 C10 C9 112.2(3) . . ?
C12 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C12 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C14 C11 C9 111.4(3) . . ?
C14 C11 H11A 109.4 . . ?
C9 C11 H11A 109.4 . . ?
C14 C11 H11B 109.4 . . ?
C9 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C10 C12 C26 111.7(4) . . ?
C10 C12 C13 106.9(3) . . ?
C26 C12 C13 106.8(3) . . ?
C10 C12 H12 110.4 . . ?
C26 C12 H12 110.4 . . ?
C13 C12 H12 110.4 . . ?
C7 C13 C12 111.2(3) . . ?
C7 C13 H13A 109.4 . . ?
C12 C13 H13A 109.4 . . ?
C7 C13 H13B 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C11 C14 C26 111.7(3) . . ?
C11 C14 C15 108.3(3) . . ?
C26 C14 C15 106.5(3) . . ?
C11 C14 H14 110.1 . . ?
C26 C14 H14 110.1 . . ?
C15 C14 H14 110.1 . . ?
C7 C15 C14 110.3(3) . . ?
C7 C15 H15A 109.6 . . ?
C14 C15 H15A 109.6 . . ?
C7 C15 H15B 109.6 . . ?
C14 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
N3 C16 C18 107.1(3) . . ?
N3 C16 C17 107.3(3) . . ?
C18 C16 C17 109.9(4) . . ?
N3 C16 C19 116.4(3) . . ?
C18 C16 C19 108.5(3) . . ?
C17 C16 C19 107.6(3) . . ?
C16 C17 C24 109.4(3) . . ?
C16 C17 H17A 109.8 . . ?
C24 C17 H17A 109.8 . . ?
C16 C17 H17B 109.8 . . ?
C24 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
C16 C18 C23 110.3(3) . . ?
C16 C18 H18A 109.6 . . ?
C23 C18 H18A 109.6 . . ?
C16 C18 H18B 109.6 . . ?
C23 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C16 C19 C20 110.3(4) . . ?
C16 C19 H19A 109.6 . . ?
C20 C19 H19A 109.6 . . ?
C16 C19 H19B 109.6 . . ?
C20 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C21 C20 C22 109.7(5) . . ?
C21 C20 C19 108.7(5) . . ?
C22 C20 C19 109.4(4) . . ?
C21 C20 H20 109.7 . . ?
C22 C20 H20 109.7 . . ?
C19 C20 H20 109.7 . . ?
C20 C21 C23 111.1(4) . . ?
C20 C21 H21A 109.4 . . ?
C23 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
C23 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C20 C22 C24 109.8(4) . . ?
C20 C22 H22A 109.7 . . ?
C24 C22 H22A 109.7 . . ?
C20 C22 H22B 109.7 . . ?
C24 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C25 C23 C21 110.6(4) . . ?
C25 C23 C18 106.8(5) . . ?
C21 C23 C18 111.0(5) . . ?
C25 C23 H23 109.5 . . ?
C21 C23 H23 109.5 . . ?
C18 C23 H23 109.5 . . ?
C25 C24 C22 111.0(4) . . ?
C25 C24 C17 108.9(4) . . ?
C22 C24 C17 105.3(6) . . ?
C25 C24 H24 110.5 . . ?
C22 C24 H24 110.5 . . ?
C17 C24 H24 110.5 . . ?
C23 C25 C24 111.5(5) . . ?
C23 C25 H25A 109.3 . . ?
C24 C25 H25A 109.3 . . ?
C23 C25 H25B 109.3 . . ?
C24 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
C12 C26 C14 111.3(3) . . ?
C12 C26 H26A 109.4 . . ?
C14 C26 H26A 109.4 . . ?
C12 C26 H26B 109.4 . . ?
C14 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?

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
C4 N1 C1 C2 0.0(4) . . . . ?
C4 N1 C1 C6 177.7(3) . . . . ?
N1 C1 C2 C3 -0.1(4) . . . . ?
C6 C1 C2 C3 -177.5(3) . . . . ?
C1 C2 C3 C4 0.2(4) . . . . ?
C1 N1 C4 C3 0.1(4) . . . . ?
C1 N1 C4 C5 -179.0(3) . . . . ?
C2 C3 C4 N1 -0.1(4) . . . . ?
C2 C3 C4 C5 178.8(3) . . . . ?
C7 N2 C5 C4 179.9(3) . . . . ?
N1 C4 C5 N2 0.7(5) . . . . ?
C3 C4 C5 N2 -178.1(3) . . . . ?
C16 N3 C6 C1 -177.4(3) . . . . ?
N1 C1 C6 N3 -0.3(5) . . . . ?
C2 C1 C6 N3 176.8(4) . . . . ?
C5 N2 C7 C13 123.8(3) . . . . ?
C5 N2 C7 C15 -119.3(3) . . . . ?
C5 N2 C7 C8 2.0(4) . . . . ?
N2 C7 C8 C9 178.6(3) . . . . ?
C13 C7 C8 C9 57.8(4) . . . . ?
C15 C7 C8 C9 -60.4(4) . . . . ?
C7 C8 C9 C10 -58.6(4) . . . . ?
C7 C8 C9 C11 60.9(4) . . . . ?
C11 C9 C10 C12 -53.9(5) . . . . ?
C8 C9 C10 C12 62.4(4) . . . . ?
C10 C9 C11 C14 54.4(5) . . . . ?
C8 C9 C11 C14 -62.4(4) . . . . ?
C9 C10 C12 C26 53.9(5) . . . . ?
C9 C10 C12 C13 -62.6(4) . . . . ?
N2 C7 C13 C12 175.1(3) . . . . ?
C15 C7 C13 C12 59.0(4) . . . . ?
C8 C7 C13 C12 -58.8(4) . . . . ?
C10 C12 C13 C7 60.0(4) . . . . ?
C26 C12 C13 C7 -59.7(4) . . . . ?
C9 C11 C14 C26 -55.0(5) . . . . ?
C9 C11 C14 C15 62.0(4) . . . . ?
N2 C7 C15 C14 -174.9(3) . . . . ?
C13 C7 C15 C14 -59.2(4) . . . . ?
C8 C7 C15 C14 59.0(4) . . . . ?
C11 C14 C15 C7 -59.8(4) . . . . ?
C26 C14 C15 C7 60.5(4) . . . . ?
C6 N3 C16 C18 -133.8(4) . . . . ?
C6 N3 C16 C17 108.3(4) . . . . ?
C6 N3 C16 C19 -12.3(5) . . . . ?
N3 C16 C17 C24 171.4(4) . . . . ?
C18 C16 C17 C24 55.3(5) . . . . ?
C19 C16 C17 C24 -62.6(6) . . . . ?
N3 C16 C18 C23 -176.6(4) . . . . ?
C17 C16 C18 C23 -60.4(5) . . . . ?
C19 C16 C18 C23 57.0(5) . . . . ?
N3 C16 C19 C20 179.6(4) . . . . ?
C18 C16 C19 C20 -59.6(5) . . . . ?
C17 C16 C19 C20 59.3(5) . . . . ?
C16 C19 C20 C21 60.6(6) . . . . ?
C16 C19 C20 C22 -59.2(6) . . . . ?
C22 C20 C21 C23 60.0(6) . . . . ?
C19 C20 C21 C23 -59.6(6) . . . . ?
C21 C20 C22 C24 -56.8(6) . . . . ?
C19 C20 C22 C24 62.3(6) . . . . ?
C20 C21 C23 C25 -60.1(6) . . . . ?
C20 C21 C23 C18 58.3(6) . . . . ?
C16 C18 C23 C25 63.7(5) . . . . ?
C16 C18 C23 C21 -57.0(6) . . . . ?
C20 C22 C24 C25 54.1(6) . . . . ?
C20 C22 C24 C17 -63.6(6) . . . . ?
C16 C17 C24 C25 -54.5(6) . . . . ?
C16 C17 C24 C22 64.6(6) . . . . ?
C21 C23 C25 C24 56.7(6) . . . . ?
C18 C23 C25 C24 -64.2(5) . . . . ?
C22 C24 C25 C23 -54.6(6) . . . . ?
C17 C24 C25 C23 60.9(6) . . . . ?
C10 C12 C26 C14 -53.9(5) . . . . ?
C13 C12 C26 C14 62.7(4) . . . . ?
C11 C14 C26 C12 54.8(5) . . . . ?
C15 C14 C26 C12 -63.3(4) . . . . ?

_refine_diff_density_max         0.603
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.050



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

data_3-h
_database_code_depnum_ccdc_archive 'CCDC 1476170'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-08-18 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            'C52 H51 N3 O2'
_chemical_formula_weight         749.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_H-M_alt        'P b c m'
_space_group_name_Hall           '-P 2c 2b'

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

_cell_length_a                   7.3665(4)
_cell_length_b                   17.5179(5)
_cell_length_c                   32.0143(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4131.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10213
_cell_measurement_theta_min      5.049
_cell_measurement_theta_max      69.955

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.565
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10185
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         5.049
_diffrn_reflns_theta_max         69.955
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3932
_reflns_number_gt                3111
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX
_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)+(0.0982P)²+3.4088P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3932
_refine_ls_number_parameters     288
_refine_ls_number_restraints     262
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.2194
_refine_ls_wR_factor_gt          0.2078
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

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
C0AA C 0.4679(4) 0.43125(16) 0.27203(8) 0.0451(7) Uani 1 1 d . U . . .
H0AA H 0.5603 0.4134 0.2892 0.054 Uiso 1 1 calc R U . . .
C1AA C 0.3057(3) 0.46263(15) 0.28491(7) 0.0381(6) Uani 1 1 d . U . . .
C2AA C 0.2307(4) 0.47968(14) 0.32585(8) 0.0394(6) Uani 1 1 d . U . . .
H2AA H 0.2982 0.4713 0.3500 0.047 Uiso 1 1 calc R U . . .
C3AA C -0.0166(3) 0.52649(14) 0.36809(7) 0.0358(6) Uani 1 1 d . U . . .
C4AA C 0.1208(3) 0.54459(14) 0.40297(7) 0.0358(6) Uani 1 1 d . U . . .
C6 C 0.1146(3) 0.50980(15) 0.44206(8) 0.0396(6) Uani 1 1 d . U . . .
H6 H 0.0272 0.4728 0.4475 0.047 Uiso 1 1 calc R U . . .
C7 C 0.2382(4) 0.52988(17) 0.47318(8) 0.0457(7) Uani 1 1 d . U . . .
H7 H 0.2324 0.5061 0.4991 0.055 Uiso 1 1 calc R U . . .
C8 C 0.3684(4) 0.58443(17) 0.46584(9) 0.0476(7) Uani 1 1 d . U . . .
H8 H 0.4495 0.5982 0.4868 0.057 Uiso 1 1 calc R U . . .
C9 C 0.3774(4) 0.61886(15) 0.42670(9) 0.0442(6) Uani 1 1 d . U . . .
H9 H 0.4662 0.6553 0.4213 0.053 Uiso 1 1 calc R U . . .
C10 C 0.2551(3) 0.59925(14) 0.39578(8) 0.0393(6) Uani 1 1 d . U . . .
H10 H 0.2624 0.6228 0.3698 0.047 Uiso 1 1 calc R U . . .
C11 C -0.1410(3) 0.45969(14) 0.38066(8) 0.0364(6) Uani 1 1 d . U . . .
C12 C -0.0959(4) 0.38439(16) 0.37203(10) 0.0489(7) Uani 1 1 d . U . . .
H12 H 0.0088 0.3737 0.3569 0.059 Uiso 1 1 calc R U . . .
C13 C -0.2050(4) 0.32510(17) 0.38570(11) 0.0593(8) Uani 1 1 d . U . . .
H13 H -0.1726 0.2750 0.3796 0.071 Uiso 1 1 calc R U . . .
C14 C -0.3600(4) 0.33911(17) 0.40806(10) 0.0525(7) Uani 1 1 d . U . . .
H14 H -0.4317 0.2989 0.4174 0.063 Uiso 1 1 calc R U . . .
C15 C -0.4085(4) 0.41344(17) 0.41651(9) 0.0467(7) Uani 1 1 d . U . . .
H15 H -0.5145 0.4237 0.4313 0.056 Uiso 1 1 calc R U . . .
C16 C -0.2997(4) 0.47281(15) 0.40306(8) 0.0409(6) Uani 1 1 d . U . . .
H16 H -0.3334 0.5228 0.4091 0.049 Uiso 1 1 calc R U . . .
C17 C -0.1360(3) 0.59669(15) 0.35803(8) 0.0381(6) Uani 1 1 d . U . . .
C18 C -0.1383(4) 0.66283(15) 0.38203(9) 0.0437(6) Uani 1 1 d . U . . .
H18 H -0.0639 0.6663 0.4054 0.052 Uiso 1 1 calc R U . . .
C19 C -0.2495(4) 0.72349(16) 0.37162(10) 0.0525(7) Uani 1 1 d . U . . .
H19 H -0.2472 0.7677 0.3877 0.063 Uiso 1 1 calc R U . . .
C20 C -0.3633(4) 0.71915(18) 0.33776(11) 0.0597(8) Uani 1 1 d . U . . .
H20 H -0.4369 0.7603 0.3307 0.072 Uiso 1 1 calc R U . . .
C21 C -0.3674(4) 0.6526(2) 0.31406(10) 0.0619(9) Uani 1 1 d . U . . .
H21 H -0.4468 0.6484 0.2916 0.074 Uiso 1 1 calc R U . . .
C22 C -0.2538(4) 0.59266(18) 0.32398(9) 0.0503(7) Uani 1 1 d . U . . .
H22 H -0.2557 0.5488 0.3077 0.060 Uiso 1 1 calc R U . . .
N1 N 0.2091(4) 0.48037(17) 0.2500 0.0367(7) Uani 1 2 d S TU P . .
H1 H 0.1021 0.5000 0.2500 0.044 Uiso 1 2 calc R U P . .
N2 N 0.0701(3) 0.50636(12) 0.32780(6) 0.0371(5) Uani 1 1 d . U . . .
O1B O 0.2334(12) 0.6959(4) 0.2436(5) 0.187(5) Uani 0.5 1 d D U P A -1
C2B C 0.1008(13) 0.8140(6) 0.2391(5) 0.129(6) Uani 0.5 1 d D U P A -1
H2BA H 0.1586 0.8555 0.2541 0.154 Uiso 0.5 1 calc R U P A -1
H2BB H 0.0304 0.8350 0.2162 0.154 Uiso 0.5 1 calc R U P A -1
C4B C 0.0835(18) 0.6984(8) 0.2675(6) 0.227(12) Uani 0.5 1 d D U P A -1
H4BA H 0.1167 0.6881 0.2963 0.273 Uiso 0.5 1 calc R U P A -1
H4BB H 0.0003 0.6587 0.2586 0.273 Uiso 0.5 1 calc R U P A -1
C5 C 0.2287(18) 0.7619(7) 0.2246(5) 0.173(7) Uani 0.5 1 d D U P A -1
H5A H 0.2059 0.7529 0.1952 0.207 Uiso 0.5 1 calc R U P A -1
H5B H 0.3478 0.7852 0.2269 0.207 Uiso 0.5 1 calc R U P A -1
C3A C -0.0070(15) 0.7710(6) 0.2653(3) 0.128(4) Uani 0.5 1 d D U P A -1
H3AA H -0.1284 0.7655 0.2540 0.153 Uiso 0.5 1 calc R U P A -1
H3AB H -0.0150 0.7943 0.2928 0.153 Uiso 0.5 1 calc R U P A -1
O2A O 0.6873(9) 0.7500 0.5000 0.079(2) Uani 0.5 2 d S TU P . .
O2B O 1.0187(11) 0.7500 0.5000 0.087(2) Uani 0.5 2 d S TU P . .
C003 C 0.7681(9) 0.6934(3) 0.5143(2) 0.127(2) Uani 1 1 d . U . . .
C004 C 0.9287(10) 0.6911(4) 0.5118(2) 0.133(2) Uani 1 1 d . 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
C0AA C1AA 1.378(4) . ?
C0AA C0AA 1.411(5) 6_556 ?
C0AA H0AA 0.9300 . ?
C1AA N1 1.361(3) . ?
C1AA C2AA 1.453(3) . ?
C2AA N2 1.274(3) . ?
C2AA H2AA 0.9300 . ?
C3AA N2 1.482(3) . ?
C3AA C11 1.540(4) . ?
C3AA C4AA 1.540(3) . ?
C3AA C17 1.546(3) . ?
C4AA C6 1.393(3) . ?
C4AA C10 1.396(4) . ?
C6 C7 1.395(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.374(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.392(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.388(4) . ?
C11 C16 1.391(4) . ?
C12 C13 1.384(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.377(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.382(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.391(4) . ?
C17 C22 1.395(4) . ?
C18 C19 1.383(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.372(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.392(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.379(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N1 C1AA 1.361(3) 6_556 ?
N1 H1 0.8600 . ?
O1B C5 1.307(11) . ?
O1B C4B 1.344(11) . ?
C2B C3A 1.380(11) . ?
C2B C5 1.391(11) . ?
C2B H2BA 0.9700 . ?
C2B H2BB 0.9700 . ?
C4B C3A 1.438(12) . ?
C4B H4BA 0.9700 . ?
C4B H4BB 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
O2A C003 1.244(6) . ?
O2A C003 1.244(6) 3_566 ?
O2B C004 1.283(8) 3_566 ?
O2B C004 1.283(8) . ?
C003 C004 1.187(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
C1AA C0AA C0AA 107.40(15) . 6_556 ?
C1AA C0AA H0AA 126.3 . . ?
C0AA C0AA H0AA 126.3 6_556 . ?
N1 C1AA C0AA 107.4(2) . . ?
N1 C1AA C2AA 119.7(2) . . ?
C0AA C1AA C2AA 132.9(2) . . ?
N2 C2AA C1AA 118.2(2) . . ?
N2 C2AA H2AA 120.9 . . ?
C1AA C2AA H2AA 120.9 . . ?
N2 C3AA C11 107.65(19) . . ?
N2 C3AA C4AA 113.4(2) . . ?
C11 C3AA C4AA 110.99(19) . . ?
N2 C3AA C17 104.67(18) . . ?
C11 C3AA C17 108.7(2) . . ?
C4AA C3AA C17 111.2(2) . . ?
C6 C4AA C10 118.1(2) . . ?
C6 C4AA C3AA 122.7(2) . . ?
C10 C4AA C3AA 119.2(2) . . ?
C4AA C6 C7 120.7(3) . . ?
C4AA C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C8 C7 C6 120.6(3) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 119.2(2) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C4AA 121.0(2) . . ?
C9 C10 H10 119.5 . . ?
C4AA C10 H10 119.5 . . ?
C12 C11 C16 117.4(2) . . ?
C12 C11 C3AA 121.8(2) . . ?
C16 C11 C3AA 120.6(2) . . ?
C13 C12 C11 120.8(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C12 121.0(3) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 119.2(3) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C14 C15 C16 120.0(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C11 121.6(3) . . ?
C15 C16 H16 119.2 . . ?
C11 C16 H16 119.2 . . ?
C18 C17 C22 117.8(2) . . ?
C18 C17 C3AA 123.7(2) . . ?
C22 C17 C3AA 118.5(2) . . ?
C19 C18 C17 120.9(3) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C20 C19 C18 120.6(3) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C19 C20 C21 119.4(3) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C22 C21 C20 119.9(3) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C17 121.3(3) . . ?
C21 C22 H22 119.4 . . ?
C17 C22 H22 119.4 . . ?
C1AA N1 C1AA 110.4(3) 6_556 . ?
C1AA N1 H1 124.8 6_556 . ?
C1AA N1 H1 124.8 . . ?
C2AA N2 C3AA 122.0(2) . . ?
C5 O1B C4B 102.3(8) . . ?
C3A C2B C5 103.6(9) . . ?
C3A C2B H2BA 111.0 . . ?
C5 C2B H2BA 111.1 . . ?
C3A C2B H2BB 111.0 . . ?
C5 C2B H2BB 111.0 . . ?
H2BA C2B H2BB 109.0 . . ?
O1B C4B C3A 112.5(9) . . ?
O1B C4B H4BA 109.1 . . ?
C3A C4B H4BA 109.1 . . ?
O1B C4B H4BB 109.1 . . ?
C3A C4B H4BB 109.1 . . ?
H4BA C4B H4BB 107.8 . . ?
O1B C5 C2B 116.4(8) . . ?
O1B C5 H5A 108.2 . . ?
C2B C5 H5A 108.2 . . ?
O1B C5 H5B 108.2 . . ?
C2B C5 H5B 108.2 . . ?
H5A C5 H5B 107.4 . . ?
C2B C3A C4B 104.2(9) . . ?
C2B C3A H3AA 110.9 . . ?
C4B C3A H3AA 110.9 . . ?
C2B C3A H3AB 110.9 . . ?
C4B C3A H3AB 110.9 . . ?
H3AA C3A H3AB 108.9 . . ?
C003 O2A C003 122.8(8) . 3_566 ?
C004 O2B C004 117.8(9) 3_566 . ?
C004 C003 O2A 118.7(7) . . ?
C003 C004 O2B 120.5(7) . . ?

_refine_diff_density_max         0.552
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.058



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

data_3-Li
_database_code_depnum_ccdc_archive 'CCDC 1476171'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H50 Li N3 O2'
_chemical_formula_sum            'C52 H50 Li N3 O2'
_chemical_formula_weight         755.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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                   9.0800(8)
_cell_length_b                   12.8271(10)
_cell_length_c                   18.6899(14)
_cell_angle_alpha                92.384(6)
_cell_angle_beta                 95.649(7)
_cell_angle_gamma                106.228(7)
_cell_volume                     2074.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5151
_cell_measurement_theta_min      3.598
_cell_measurement_theta_max      71.379

_exptl_crystal_description       plates
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_F_000             804
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.563
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93512
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15211
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.598
_diffrn_reflns_theta_max         71.379
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7804
_reflns_number_gt                6214
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND & Olex 2.1'
_computing_publication_material  WinGX
_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)+(0.0621P)²+0.6395P] 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         7804
_refine_ls_number_parameters     527
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1370
_refine_ls_wR_factor_gt          0.1251
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Li1 Li 0.2321(4) 0.4436(2) 0.21828(16) 0.0337(6) Uani 1 1 d . . . . .
N1 N 0.07065(16) 0.51924(11) 0.22874(7) 0.0288(3) Uani 1 1 d . . . . .
N2 N 0.05911(16) 0.32372(11) 0.14901(7) 0.0287(3) Uani 1 1 d . . . . .
N3 N 0.26323(17) 0.69025(11) 0.33797(8) 0.0300(3) Uani 1 1 d . . . . .
O1 O 0.30018(16) 0.39151(13) 0.30748(7) 0.0461(4) Uani 1 1 d . . . . .
O2 O 0.40252(15) 0.52051(10) 0.16808(7) 0.0395(3) Uani 1 1 d . . . . .
C1 C -0.0584(2) 0.45930(14) 0.18555(9) 0.0300(4) Uani 1 1 d . . . . .
C2 C -0.1812(2) 0.50585(15) 0.18783(10) 0.0367(4) Uani 1 1 d . . . . .
H6 H -0.2803 0.4793 0.1638 0.044 Uiso 1 1 calc R U . . .
C3 C -0.1232(2) 0.59970(15) 0.23354(10) 0.0360(4) Uani 1 1 d . . . . .
H2AA H -0.1756 0.6494 0.2458 0.043 Uiso 1 1 calc R U . . .
C4 C 0.0307(2) 0.60478(13) 0.25774(9) 0.0297(4) Uani 1 1 d . . . . .
C5 C 0.1307(2) 0.69076(14) 0.30775(9) 0.0307(4) Uani 1 1 d . . . . .
H10 H 0.0961 0.7506 0.3187 0.037 Uiso 1 1 calc R U . . .
C6 C -0.0587(2) 0.36196(14) 0.14465(9) 0.0302(4) Uani 1 1 d . . . . .
C7 C 0.3483(2) 0.78263(13) 0.39071(9) 0.0299(4) Uani 1 1 d . . . . .
C8 C 0.5207(2) 0.78882(14) 0.39374(9) 0.0301(4) Uani 1 1 d . . . . .
C9 C 0.5650(2) 0.69466(15) 0.38369(10) 0.0344(4) Uani 1 1 d . . . . .
H28 H 0.4898 0.6287 0.3714 0.041 Uiso 1 1 calc R U . . .
C10 C 0.7194(2) 0.69707(17) 0.39166(10) 0.0403(4) Uani 1 1 d . . . . .
H9EA H 0.7467 0.6331 0.3843 0.048 Uiso 1 1 calc R U . . .
C11 C 0.8328(2) 0.79428(18) 0.41043(11) 0.0440(5) Uani 1 1 d . . . . .
H0FA H 0.9363 0.7958 0.4163 0.053 Uiso 1 1 calc R U . . .
C12 C 0.7913(2) 0.88895(17) 0.42033(11) 0.0424(5) Uani 1 1 d . . . . .
H42 H 0.8671 0.9546 0.4327 0.051 Uiso 1 1 calc R U . . .
C13 C 0.6368(2) 0.88674(15) 0.41184(10) 0.0367(4) Uani 1 1 d . . . . .
H3EA H 0.6101 0.9511 0.4183 0.044 Uiso 1 1 calc R U . . .
C14 C 0.2997(2) 0.75569(13) 0.46666(9) 0.0297(4) Uani 1 1 d . . . . .
C15 C 0.1784(2) 0.66612(15) 0.47750(10) 0.0370(4) Uani 1 1 d . . . . .
H24 H 0.1224 0.6207 0.4381 0.044 Uiso 1 1 calc R U . . .
C16 C 0.1394(2) 0.64344(17) 0.54642(11) 0.0451(5) Uani 1 1 d . . . . .
H5EA H 0.0586 0.5826 0.5525 0.054 Uiso 1 1 calc R U . . .
C17 C 0.2190(2) 0.70992(17) 0.60593(11) 0.0439(5) Uani 1 1 d . . . . .
H1FA H 0.1922 0.6945 0.6519 0.053 Uiso 1 1 calc R U . . .
C18 C 0.3397(2) 0.80024(16) 0.59591(10) 0.0376(4) Uani 1 1 d . . . . .
H1EA H 0.3934 0.8465 0.6354 0.045 Uiso 1 1 calc R U . . .
C19 C 0.3804(2) 0.82169(14) 0.52754(10) 0.0329(4) Uani 1 1 d . . . . .
H9DA H 0.4634 0.8814 0.5219 0.040 Uiso 1 1 calc R U . . .
C20 C 0.3203(2) 0.88968(14) 0.36739(9) 0.0311(4) Uani 1 1 d . . . . .
C21 C 0.2409(2) 0.94781(14) 0.40545(10) 0.0347(4) Uani 1 1 d . . . . .
H6EA H 0.2110 0.9263 0.4500 0.042 Uiso 1 1 calc R U . . .
C22 C 0.2060(2) 1.03836(15) 0.37710(12) 0.0414(4) Uani 1 1 d . . . . .
H2EA H 0.1545 1.0773 0.4034 0.050 Uiso 1 1 calc R U . . .
C23 C 0.2469(2) 1.07048(16) 0.31090(12) 0.0445(5) Uani 1 1 d . . . . .
H33 H 0.2208 1.1296 0.2918 0.053 Uiso 1 1 calc R U . . .
C24 C 0.3276(2) 1.01404(16) 0.27263(11) 0.0437(5) Uani 1 1 d . . . . .
H7EA H 0.3564 1.0357 0.2279 0.052 Uiso 1 1 calc R U . . .
C25 C 0.3651(2) 0.92534(15) 0.30115(10) 0.0378(4) Uani 1 1 d . . . . .
H7DA H 0.4212 0.8890 0.2757 0.045 Uiso 1 1 calc R U . . .
C26 C 0.04350(19) 0.21912(13) 0.10742(9) 0.0287(4) Uani 1 1 d . . . . .
C27 C -0.0495(2) 0.21232(14) 0.03258(9) 0.0296(4) Uani 1 1 d . . . . .
C28 C -0.0026(2) 0.29755(15) -0.01185(10) 0.0373(4) Uani 1 1 d . . . . .
H7BA H 0.0803 0.3572 0.0052 0.045 Uiso 1 1 calc R U . . .
C29 C -0.0761(2) 0.29562(16) -0.08060(10) 0.0419(5) Uani 1 1 d . . . . .
H0BA H -0.0431 0.3534 -0.1092 0.050 Uiso 1 1 calc R U . . .
C30 C -0.1994(2) 0.20653(17) -0.10647(10) 0.0421(5) Uani 1 1 d . . . . .
H6CA H -0.2483 0.2036 -0.1529 0.050 Uiso 1 1 calc R U . . .
C31 C -0.2493(2) 0.12239(16) -0.06308(10) 0.0394(4) Uani 1 1 d . . . . .
H43 H -0.3332 0.0633 -0.0801 0.047 Uiso 1 1 calc R U . . .
C32 C -0.1747(2) 0.12523(14) 0.00628(10) 0.0334(4) Uani 1 1 d . . . . .
H5BA H -0.2095 0.0680 0.0351 0.040 Uiso 1 1 calc R U . . .
C33 C 0.20780(19) 0.21284(13) 0.09798(9) 0.0290(4) Uani 1 1 d . . . . .
C34 C 0.2460(2) 0.17185(14) 0.03450(10) 0.0333(4) Uani 1 1 d . . . . .
H6AA H 0.1722 0.1516 -0.0056 0.040 Uiso 1 1 calc R U . . .
C35 C 0.3928(2) 0.16070(15) 0.03010(11) 0.0391(4) Uani 1 1 d . . . . .
H3BA H 0.4162 0.1327 -0.0127 0.047 Uiso 1 1 calc R U . . .
C36 C 0.5043(2) 0.19090(15) 0.08884(12) 0.0408(4) Uani 1 1 d . . . . .
H54 H 0.6023 0.1832 0.0858 0.049 Uiso 1 1 calc R U . . .
C37 C 0.4690(2) 0.23271(15) 0.15230(11) 0.0388(4) Uani 1 1 d . . . . .
H47 H 0.5439 0.2540 0.1919 0.047 Uiso 1 1 calc R U . . .
C38 C 0.3220(2) 0.24298(14) 0.15691(10) 0.0324(4) Uani 1 1 d . . . . .
H3AA H 0.2991 0.2704 0.2000 0.039 Uiso 1 1 calc R U . . .
C39 C -0.03192(19) 0.12313(13) 0.15235(9) 0.0292(4) Uani 1 1 d . . . . .
C40 C -0.0128(2) 0.02052(14) 0.13766(10) 0.0333(4) Uani 1 1 d . . . . .
H1 H 0.0473 0.0110 0.1018 0.040 Uiso 1 1 calc R U . . .
C41 C -0.0816(2) -0.06754(15) 0.17538(10) 0.0382(4) Uani 1 1 d . . . . .
H8AA H -0.0676 -0.1353 0.1645 0.046 Uiso 1 1 calc R U . . .
C42 C -0.1708(3) -0.05527(16) 0.22907(11) 0.0438(5) Uani 1 1 d . . . . .
H53 H -0.2176 -0.1144 0.2542 0.053 Uiso 1 1 calc R U . . .
C43 C -0.1896(3) 0.04568(17) 0.24488(12) 0.0498(5) Uani 1 1 d . . . . .
H8 H -0.2487 0.0548 0.2813 0.060 Uiso 1 1 calc R U . . .
C44 C -0.1209(2) 0.13454(15) 0.20697(11) 0.0408(4) Uani 1 1 d . . . . .
H4BA H -0.1348 0.2022 0.2184 0.049 Uiso 1 1 calc R U . . .
C45 C 0.1922(3) 0.3765(2) 0.36009(11) 0.0533(6) Uani 1 1 d . . . . .
H3A H 0.1236 0.3029 0.3545 0.064 Uiso 1 1 calc R U . . .
H3B H 0.1306 0.4271 0.3545 0.064 Uiso 1 1 calc R U . . .
C46 C 0.2833(3) 0.3968(4) 0.43040(14) 0.0973(12) Uani 1 1 d . U . . .
H8CA H 0.2354 0.3435 0.4627 0.117 Uiso 1 1 calc R U . . .
H8CB H 0.2895 0.4687 0.4511 0.117 Uiso 1 1 calc R U . . .
C47 C 0.4376(4) 0.3890(3) 0.42079(12) 0.0735(9) Uani 1 1 d . U . . .
H7CA H 0.4541 0.3245 0.4415 0.088 Uiso 1 1 calc R U . . .
H7CB H 0.5157 0.4525 0.4440 0.088 Uiso 1 1 calc R U . . .
C48 C 0.4454(2) 0.38258(17) 0.34048(11) 0.0435(5) Uani 1 1 d . . . . .
H5CA H 0.5298 0.4414 0.3278 0.052 Uiso 1 1 calc R U . . .
H5CB H 0.4612 0.3139 0.3247 0.052 Uiso 1 1 calc R U . . .
C49 C 0.4759(2) 0.63267(16) 0.19301(11) 0.0443(5) Uani 1 1 d . . . . .
H2A H 0.5551 0.6376 0.2328 0.053 Uiso 1 1 calc R U . . .
H2B H 0.4006 0.6665 0.2091 0.053 Uiso 1 1 calc R U . . .
C50 C 0.5467(3) 0.68864(17) 0.12955(12) 0.0498(5) Uani 1 1 d . . . . .
H9AA H 0.5171 0.7548 0.1223 0.060 Uiso 1 1 calc R U . . .
H9AB H 0.6585 0.7068 0.1372 0.060 Uiso 1 1 calc R U . . .
C51 C 0.4842(5) 0.6080(2) 0.06688(14) 0.1003(14) Uani 1 1 d . U . . .
H9A H 0.4319 0.6393 0.0294 0.120 Uiso 1 1 calc R U . . .
H9B H 0.5674 0.5868 0.0472 0.120 Uiso 1 1 calc R U . . .
C52 C 0.3777(3) 0.5151(2) 0.09164(12) 0.0669(8) Uani 1 1 d . U . . .
H4CA H 0.2725 0.5148 0.0761 0.080 Uiso 1 1 calc R U . . .
H4CB H 0.3937 0.4486 0.0716 0.080 Uiso 1 1 calc R U . . .
H0AA H -0.155(2) 0.3266(17) 0.1133(11) 0.040(5) 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
Li1 O1 1.931(3) . ?
Li1 O2 1.938(3) . ?
Li1 N1 1.992(3) . ?
Li1 N2 2.143(3) . ?
Li1 C1 2.714(4) . ?
Li1 C6 2.754(3) . ?
N1 C4 1.357(2) . ?
N1 C1 1.369(2) . ?
N2 C6 1.293(2) . ?
N2 C26 1.487(2) . ?
N3 C5 1.279(2) . ?
N3 C7 1.488(2) . ?
O1 C48 1.436(2) . ?
O1 C45 1.437(3) . ?
O2 C52 1.420(3) . ?
O2 C49 1.441(2) . ?
C1 C2 1.407(2) . ?
C1 C6 1.436(2) . ?
C2 C3 1.388(3) . ?
C2 H6 0.9300 . ?
C3 C4 1.408(2) . ?
C3 H2AA 0.9300 . ?
C4 C5 1.450(2) . ?
C5 H10 0.9300 . ?
C6 H0AA 0.98(2) . ?
C7 C20 1.537(2) . ?
C7 C8 1.541(2) . ?
C7 C14 1.552(2) . ?
C8 C9 1.387(2) . ?
C8 C13 1.399(2) . ?
C9 C10 1.386(3) . ?
C9 H28 0.9300 . ?
C10 C11 1.383(3) . ?
C10 H9EA 0.9300 . ?
C11 C12 1.379(3) . ?
C11 H0FA 0.9300 . ?
C12 C13 1.389(3) . ?
C12 H42 0.9300 . ?
C13 H3EA 0.9300 . ?
C14 C15 1.389(3) . ?
C14 C19 1.399(2) . ?
C15 C16 1.390(3) . ?
C15 H24 0.9300 . ?
C16 C17 1.380(3) . ?
C16 H5EA 0.9300 . ?
C17 C18 1.388(3) . ?
C17 H1FA 0.9300 . ?
C18 C19 1.382(3) . ?
C18 H1EA 0.9300 . ?
C19 H9DA 0.9300 . ?
C20 C21 1.392(3) . ?
C20 C25 1.396(3) . ?
C21 C22 1.398(3) . ?
C21 H6EA 0.9300 . ?
C22 C23 1.373(3) . ?
C22 H2EA 0.9300 . ?
C23 C24 1.389(3) . ?
C23 H33 0.9300 . ?
C24 C25 1.388(3) . ?
C24 H7EA 0.9300 . ?
C25 H7DA 0.9300 . ?
C26 C33 1.543(2) . ?
C26 C27 1.547(2) . ?
C26 C39 1.555(2) . ?
C27 C32 1.384(2) . ?
C27 C28 1.397(3) . ?
C28 C29 1.384(3) . ?
C28 H7BA 0.9300 . ?
C29 C30 1.388(3) . ?
C29 H0BA 0.9300 . ?
C30 C31 1.378(3) . ?
C30 H6CA 0.9300 . ?
C31 C32 1.397(3) . ?
C31 H43 0.9300 . ?
C32 H5BA 0.9300 . ?
C33 C34 1.391(2) . ?
C33 C38 1.398(2) . ?
C34 C35 1.390(3) . ?
C34 H6AA 0.9300 . ?
C35 C36 1.380(3) . ?
C35 H3BA 0.9300 . ?
C36 C37 1.384(3) . ?
C36 H54 0.9300 . ?
C37 C38 1.388(3) . ?
C37 H47 0.9300 . ?
C38 H3AA 0.9300 . ?
C39 C44 1.390(3) . ?
C39 C40 1.395(2) . ?
C40 C41 1.386(3) . ?
C40 H1 0.9300 . ?
C41 C42 1.380(3) . ?
C41 H8AA 0.9300 . ?
C42 C43 1.376(3) . ?
C42 H53 0.9300 . ?
C43 C44 1.395(3) . ?
C43 H8 0.9300 . ?
C44 H4BA 0.9300 . ?
C45 C46 1.454(3) . ?
C45 H3A 0.9700 . ?
C45 H3B 0.9700 . ?
C46 C47 1.460(4) . ?
C46 H8CA 0.9700 . ?
C46 H8CB 0.9700 . ?
C47 C48 1.510(3) . ?
C47 H7CA 0.9700 . ?
C47 H7CB 0.9700 . ?
C48 H5CA 0.9700 . ?
C48 H5CB 0.9700 . ?
C49 C50 1.516(3) . ?
C49 H2A 0.9700 . ?
C49 H2B 0.9700 . ?
C50 C51 1.484(3) . ?
C50 H9AA 0.9700 . ?
C50 H9AB 0.9700 . ?
C51 C52 1.435(3) . ?
C51 H9A 0.9700 . ?
C51 H9B 0.9700 . ?
C52 H4CA 0.9700 . ?
C52 H4CB 0.9700 . ?

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 Li1 O2 112.63(16) . . ?
O1 Li1 N1 113.01(16) . . ?
O2 Li1 N1 115.21(16) . . ?
O1 Li1 N2 114.62(16) . . ?
O2 Li1 N2 112.51(15) . . ?
N1 Li1 N2 86.48(13) . . ?
O1 Li1 C1 123.25(15) . . ?
O2 Li1 C1 121.97(14) . . ?
N1 Li1 C1 28.98(7) . . ?
N2 Li1 C1 57.53(9) . . ?
O1 Li1 C6 124.20(15) . . ?
O2 Li1 C6 119.96(14) . . ?
N1 Li1 C6 59.41(9) . . ?
N2 Li1 C6 27.13(6) . . ?
C1 Li1 C6 30.44(6) . . ?
C4 N1 C1 105.18(14) . . ?
C4 N1 Li1 148.55(15) . . ?
C1 N1 Li1 106.23(14) . . ?
C6 N2 C26 117.81(14) . . ?
C6 N2 Li1 103.78(14) . . ?
C26 N2 Li1 138.38(14) . . ?
C5 N3 C7 118.01(14) . . ?
C48 O1 C45 109.34(15) . . ?
C48 O1 Li1 134.88(16) . . ?
C45 O1 Li1 114.57(15) . . ?
C52 O2 C49 107.68(15) . . ?
C52 O2 Li1 117.42(16) . . ?
C49 O2 Li1 116.24(14) . . ?
N1 C1 C2 111.52(15) . . ?
N1 C1 C6 121.11(15) . . ?
C2 C1 C6 127.37(16) . . ?
N1 C1 Li1 44.80(10) . . ?
C2 C1 Li1 156.31(14) . . ?
C6 C1 Li1 76.31(12) . . ?
C3 C2 C1 105.56(16) . . ?
C3 C2 H6 127.2 . . ?
C1 C2 H6 127.2 . . ?
C2 C3 C4 106.48(16) . . ?
C2 C3 H2AA 126.8 . . ?
C4 C3 H2AA 126.8 . . ?
N1 C4 C3 111.25(15) . . ?
N1 C4 C5 125.34(16) . . ?
C3 C4 C5 123.41(16) . . ?
N3 C5 C4 124.75(16) . . ?
N3 C5 H10 117.6 . . ?
C4 C5 H10 117.6 . . ?
N2 C6 C1 122.21(16) . . ?
N2 C6 Li1 49.09(10) . . ?
C1 C6 Li1 73.25(11) . . ?
N2 C6 H0AA 122.7(12) . . ?
C1 C6 H0AA 115.1(12) . . ?
Li1 C6 H0AA 171.0(12) . . ?
N3 C7 C20 110.78(13) . . ?
N3 C7 C8 106.77(13) . . ?
C20 C7 C8 110.83(14) . . ?
N3 C7 C14 108.92(14) . . ?
C20 C7 C14 112.33(14) . . ?
C8 C7 C14 106.98(13) . . ?
C9 C8 C13 117.96(17) . . ?
C9 C8 C7 120.14(15) . . ?
C13 C8 C7 121.73(16) . . ?
C10 C9 C8 121.18(18) . . ?
C10 C9 H28 119.4 . . ?
C8 C9 H28 119.4 . . ?
C11 C10 C9 120.24(19) . . ?
C11 C10 H9EA 119.9 . . ?
C9 C10 H9EA 119.9 . . ?
C12 C11 C10 119.50(18) . . ?
C12 C11 H0FA 120.2 . . ?
C10 C11 H0FA 120.2 . . ?
C11 C12 C13 120.30(18) . . ?
C11 C12 H42 119.9 . . ?
C13 C12 H42 119.9 . . ?
C12 C13 C8 120.81(18) . . ?
C12 C13 H3EA 119.6 . . ?
C8 C13 H3EA 119.6 . . ?
C15 C14 C19 117.50(17) . . ?
C15 C14 C7 122.44(15) . . ?
C19 C14 C7 120.06(16) . . ?
C14 C15 C16 120.91(17) . . ?
C14 C15 H24 119.5 . . ?
C16 C15 H24 119.5 . . ?
C17 C16 C15 120.97(19) . . ?
C17 C16 H5EA 119.5 . . ?
C15 C16 H5EA 119.5 . . ?
C16 C17 C18 118.79(19) . . ?
C16 C17 H1FA 120.6 . . ?
C18 C17 H1FA 120.6 . . ?
C19 C18 C17 120.28(17) . . ?
C19 C18 H1EA 119.9 . . ?
C17 C18 H1EA 119.9 . . ?
C18 C19 C14 121.53(17) . . ?
C18 C19 H9DA 119.2 . . ?
C14 C19 H9DA 119.2 . . ?
C21 C20 C25 118.15(17) . . ?
C21 C20 C7 123.66(17) . . ?
C25 C20 C7 117.94(16) . . ?
C20 C21 C22 120.37(19) . . ?
C20 C21 H6EA 119.8 . . ?
C22 C21 H6EA 119.8 . . ?
C23 C22 C21 120.76(19) . . ?
C23 C22 H2EA 119.6 . . ?
C21 C22 H2EA 119.6 . . ?
C22 C23 C24 119.53(18) . . ?
C22 C23 H33 120.2 . . ?
C24 C23 H33 120.2 . . ?
C25 C24 C23 119.9(2) . . ?
C25 C24 H7EA 120.0 . . ?
C23 C24 H7EA 120.0 . . ?
C24 C25 C20 121.21(19) . . ?
C24 C25 H7DA 119.4 . . ?
C20 C25 H7DA 119.4 . . ?
N2 C26 C33 107.48(13) . . ?
N2 C26 C27 111.39(13) . . ?
C33 C26 C27 109.66(14) . . ?
N2 C26 C39 109.13(13) . . ?
C33 C26 C39 107.32(13) . . ?
C27 C26 C39 111.69(13) . . ?
C32 C27 C28 117.93(16) . . ?
C32 C27 C26 123.74(16) . . ?
C28 C27 C26 118.32(15) . . ?
C29 C28 C27 121.82(18) . . ?
C29 C28 H7BA 119.1 . . ?
C27 C28 H7BA 119.1 . . ?
C28 C29 C30 119.33(19) . . ?
C28 C29 H0BA 120.3 . . ?
C30 C29 H0BA 120.3 . . ?
C31 C30 C29 119.80(18) . . ?
C31 C30 H6CA 120.1 . . ?
C29 C30 H6CA 120.1 . . ?
C30 C31 C32 120.43(18) . . ?
C30 C31 H43 119.8 . . ?
C32 C31 H43 119.8 . . ?
C27 C32 C31 120.67(18) . . ?
C27 C32 H5BA 119.7 . . ?
C31 C32 H5BA 119.7 . . ?
C34 C33 C38 117.87(16) . . ?
C34 C33 C26 122.97(15) . . ?
C38 C33 C26 119.03(15) . . ?
C35 C34 C33 120.95(17) . . ?
C35 C34 H6AA 119.5 . . ?
C33 C34 H6AA 119.5 . . ?
C36 C35 C34 120.41(18) . . ?
C36 C35 H3BA 119.8 . . ?
C34 C35 H3BA 119.8 . . ?
C35 C36 C37 119.56(18) . . ?
C35 C36 H54 120.2 . . ?
C37 C36 H54 120.2 . . ?
C36 C37 C38 120.05(18) . . ?
C36 C37 H47 120.0 . . ?
C38 C37 H47 120.0 . . ?
C37 C38 C33 121.17(17) . . ?
C37 C38 H3AA 119.4 . . ?
C33 C38 H3AA 119.4 . . ?
C44 C39 C40 117.64(16) . . ?
C44 C39 C26 122.55(15) . . ?
C40 C39 C26 119.81(15) . . ?
C41 C40 C39 121.36(17) . . ?
C41 C40 H1 119.3 . . ?
C39 C40 H1 119.3 . . ?
C42 C41 C40 120.39(18) . . ?
C42 C41 H8AA 119.8 . . ?
C40 C41 H8AA 119.8 . . ?
C43 C42 C41 119.07(18) . . ?
C43 C42 H53 120.5 . . ?
C41 C42 H53 120.5 . . ?
C42 C43 C44 120.78(19) . . ?
C42 C43 H8 119.6 . . ?
C44 C43 H8 119.6 . . ?
C39 C44 C43 120.75(18) . . ?
C39 C44 H4BA 119.6 . . ?
C43 C44 H4BA 119.6 . . ?
O1 C45 C46 106.5(2) . . ?
O1 C45 H3A 110.4 . . ?
C46 C45 H3A 110.4 . . ?
O1 C45 H3B 110.4 . . ?
C46 C45 H3B 110.4 . . ?
H3A C45 H3B 108.6 . . ?
C45 C46 C47 108.1(2) . . ?
C45 C46 H8CA 110.1 . . ?
C47 C46 H8CA 110.1 . . ?
C45 C46 H8CB 110.1 . . ?
C47 C46 H8CB 110.1 . . ?
H8CA C46 H8CB 108.4 . . ?
C46 C47 C48 106.16(19) . . ?
C46 C47 H7CA 110.5 . . ?
C48 C47 H7CA 110.5 . . ?
C46 C47 H7CB 110.5 . . ?
C48 C47 H7CB 110.5 . . ?
H7CA C47 H7CB 108.7 . . ?
O1 C48 C47 106.18(18) . . ?
O1 C48 H5CA 110.5 . . ?
C47 C48 H5CA 110.5 . . ?
O1 C48 H5CB 110.5 . . ?
C47 C48 H5CB 110.5 . . ?
H5CA C48 H5CB 108.7 . . ?
O2 C49 C50 106.53(16) . . ?
O2 C49 H2A 110.4 . . ?
C50 C49 H2A 110.4 . . ?
O2 C49 H2B 110.4 . . ?
C50 C49 H2B 110.4 . . ?
H2A C49 H2B 108.6 . . ?
C51 C50 C49 104.76(18) . . ?
C51 C50 H9AA 110.8 . . ?
C49 C50 H9AA 110.8 . . ?
C51 C50 H9AB 110.8 . . ?
C49 C50 H9AB 110.8 . . ?
H9AA C50 H9AB 108.9 . . ?
C52 C51 C50 107.7(2) . . ?
C52 C51 H9A 110.2 . . ?
C50 C51 H9A 110.2 . . ?
C52 C51 H9B 110.2 . . ?
C50 C51 H9B 110.2 . . ?
H9A C51 H9B 108.5 . . ?
O2 C52 C51 108.57(19) . . ?
O2 C52 H4CA 110.0 . . ?
C51 C52 H4CA 110.0 . . ?
O2 C52 H4CB 110.0 . . ?
C51 C52 H4CB 110.0 . . ?
H4CA C52 H4CB 108.4 . . ?

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
C4 N1 C1 C2 -0.8(2) . . . . ?
Li1 N1 C1 C2 -179.34(16) . . . . ?
C4 N1 C1 C6 179.10(16) . . . . ?
Li1 N1 C1 C6 0.6(2) . . . . ?
C4 N1 C1 Li1 178.53(19) . . . . ?
N1 C1 C2 C3 1.1(2) . . . . ?
C6 C1 C2 C3 -178.79(18) . . . . ?
Li1 C1 C2 C3 0.0(4) . . . . ?
C1 C2 C3 C4 -0.9(2) . . . . ?
C1 N1 C4 C3 0.2(2) . . . . ?
Li1 N1 C4 C3 177.5(2) . . . . ?
C1 N1 C4 C5 179.66(17) . . . . ?
Li1 N1 C4 C5 -3.0(4) . . . . ?
C2 C3 C4 N1 0.5(2) . . . . ?
C2 C3 C4 C5 -178.99(17) . . . . ?
C7 N3 C5 C4 -177.18(16) . . . . ?
N1 C4 C5 N3 -9.1(3) . . . . ?
C3 C4 C5 N3 170.32(18) . . . . ?
C26 N2 C6 C1 176.68(15) . . . . ?
Li1 N2 C6 C1 -4.6(2) . . . . ?
C26 N2 C6 Li1 -178.7(2) . . . . ?
N1 C1 C6 N2 3.2(3) . . . . ?
C2 C1 C6 N2 -176.89(18) . . . . ?
Li1 C1 C6 N2 3.62(17) . . . . ?
N1 C1 C6 Li1 -0.42(16) . . . . ?
C2 C1 C6 Li1 179.5(2) . . . . ?
C5 N3 C7 C20 -35.7(2) . . . . ?
C5 N3 C7 C8 -156.52(15) . . . . ?
C5 N3 C7 C14 88.29(18) . . . . ?
N3 C7 C8 C9 -32.4(2) . . . . ?
C20 C7 C8 C9 -153.12(16) . . . . ?
C14 C7 C8 C9 84.11(18) . . . . ?
N3 C7 C8 C13 152.52(16) . . . . ?
C20 C7 C8 C13 31.8(2) . . . . ?
C14 C7 C8 C13 -90.99(19) . . . . ?
C13 C8 C9 C10 0.3(3) . . . . ?
C7 C8 C9 C10 -174.97(16) . . . . ?
C8 C9 C10 C11 0.5(3) . . . . ?
C9 C10 C11 C12 -0.8(3) . . . . ?
C10 C11 C12 C13 0.3(3) . . . . ?
C11 C12 C13 C8 0.5(3) . . . . ?
C9 C8 C13 C12 -0.8(3) . . . . ?
C7 C8 C13 C12 174.41(17) . . . . ?
N3 C7 C14 C15 -8.9(2) . . . . ?
C20 C7 C14 C15 114.22(18) . . . . ?
C8 C7 C14 C15 -123.95(17) . . . . ?
N3 C7 C14 C19 170.10(15) . . . . ?
C20 C7 C14 C19 -66.8(2) . . . . ?
C8 C7 C14 C19 55.0(2) . . . . ?
C19 C14 C15 C16 0.0(3) . . . . ?
C7 C14 C15 C16 178.97(18) . . . . ?
C14 C15 C16 C17 0.8(3) . . . . ?
C15 C16 C17 C18 -0.2(3) . . . . ?
C16 C17 C18 C19 -1.0(3) . . . . ?
C17 C18 C19 C14 1.8(3) . . . . ?
C15 C14 C19 C18 -1.2(3) . . . . ?
C7 C14 C19 C18 179.74(16) . . . . ?
N3 C7 C20 C21 113.72(18) . . . . ?
C8 C7 C20 C21 -127.94(17) . . . . ?
C14 C7 C20 C21 -8.3(2) . . . . ?
N3 C7 C20 C25 -60.5(2) . . . . ?
C8 C7 C20 C25 57.9(2) . . . . ?
C14 C7 C20 C25 177.49(15) . . . . ?
C25 C20 C21 C22 0.8(3) . . . . ?
C7 C20 C21 C22 -173.34(16) . . . . ?
C20 C21 C22 C23 1.1(3) . . . . ?
C21 C22 C23 C24 -1.8(3) . . . . ?
C22 C23 C24 C25 0.5(3) . . . . ?
C23 C24 C25 C20 1.4(3) . . . . ?
C21 C20 C25 C24 -2.1(3) . . . . ?
C7 C20 C25 C24 172.43(17) . . . . ?
C6 N2 C26 C33 159.22(15) . . . . ?
Li1 N2 C26 C33 -18.9(2) . . . . ?
C6 N2 C26 C27 39.1(2) . . . . ?
Li1 N2 C26 C27 -139.07(18) . . . . ?
C6 N2 C26 C39 -84.71(18) . . . . ?
Li1 N2 C26 C39 97.2(2) . . . . ?
N2 C26 C27 C32 -128.76(17) . . . . ?
C33 C26 C27 C32 112.39(18) . . . . ?
C39 C26 C27 C32 -6.4(2) . . . . ?
N2 C26 C27 C28 52.8(2) . . . . ?
C33 C26 C27 C28 -66.01(19) . . . . ?
C39 C26 C27 C28 175.16(15) . . . . ?
C32 C27 C28 C29 -1.0(3) . . . . ?
C26 C27 C28 C29 177.51(17) . . . . ?
C27 C28 C29 C30 -0.3(3) . . . . ?
C28 C29 C30 C31 1.4(3) . . . . ?
C29 C30 C31 C32 -1.2(3) . . . . ?
C28 C27 C32 C31 1.2(3) . . . . ?
C26 C27 C32 C31 -177.25(16) . . . . ?
C30 C31 C32 C27 -0.1(3) . . . . ?
N2 C26 C33 C34 -140.47(16) . . . . ?
C27 C26 C33 C34 -19.2(2) . . . . ?
C39 C26 C33 C34 102.27(18) . . . . ?
N2 C26 C33 C38 43.75(19) . . . . ?
C27 C26 C33 C38 164.98(14) . . . . ?
C39 C26 C33 C38 -73.51(18) . . . . ?
C38 C33 C34 C35 0.4(3) . . . . ?
C26 C33 C34 C35 -175.45(16) . . . . ?
C33 C34 C35 C36 -0.4(3) . . . . ?
C34 C35 C36 C37 -0.1(3) . . . . ?
C35 C36 C37 C38 0.7(3) . . . . ?
C36 C37 C38 C33 -0.7(3) . . . . ?
C34 C33 C38 C37 0.2(3) . . . . ?
C26 C33 C38 C37 176.19(16) . . . . ?
N2 C26 C39 C44 22.3(2) . . . . ?
C33 C26 C39 C44 138.47(17) . . . . ?
C27 C26 C39 C44 -101.30(19) . . . . ?
N2 C26 C39 C40 -158.55(15) . . . . ?
C33 C26 C39 C40 -42.4(2) . . . . ?
C27 C26 C39 C40 77.86(19) . . . . ?
C44 C39 C40 C41 0.9(3) . . . . ?
C26 C39 C40 C41 -178.33(16) . . . . ?
C39 C40 C41 C42 -0.3(3) . . . . ?
C40 C41 C42 C43 -0.4(3) . . . . ?
C41 C42 C43 C44 0.6(3) . . . . ?
C40 C39 C44 C43 -0.7(3) . . . . ?
C26 C39 C44 C43 178.46(18) . . . . ?
C42 C43 C44 C39 0.0(3) . . . . ?
C48 O1 C45 C46 19.9(3) . . . . ?
Li1 O1 C45 C46 -149.4(2) . . . . ?
O1 C45 C46 C47 -18.1(4) . . . . ?
C45 C46 C47 C48 9.6(4) . . . . ?
C45 O1 C48 C47 -13.8(2) . . . . ?
Li1 O1 C48 C47 152.5(2) . . . . ?
C46 C47 C48 O1 2.4(3) . . . . ?
C52 O2 C49 C50 -20.1(2) . . . . ?
Li1 O2 C49 C50 -154.23(17) . . . . ?
O2 C49 C50 C51 10.1(3) . . . . ?
C49 C50 C51 C52 3.3(4) . . . . ?
C49 O2 C52 C51 22.7(3) . . . . ?
Li1 O2 C52 C51 156.2(3) . . . . ?
C50 C51 C52 O2 -15.9(4) . . . . ?

_refine_diff_density_max         0.323
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.044



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

data_3-Na
_database_code_depnum_ccdc_archive 'CCDC 1476172'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-08-18 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         'C56 H58 N3 Na O3'
_chemical_formula_sum            'C56 H58 N3 Na O3'
_chemical_formula_weight         844.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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                   8.8522(3)
_cell_length_b                   9.4272(3)
_cell_length_c                   29.1528(8)
_cell_angle_alpha                81.636(3)
_cell_angle_beta                 88.161(2)
_cell_angle_gamma                74.457(3)
_cell_volume                     2318.88(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12735
_cell_measurement_theta_min      4.599
_cell_measurement_theta_max      70.703

_exptl_crystal_description       plates
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_F_000             900
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.659
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17860
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         4.599
_diffrn_reflns_theta_max         70.703
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             8688
_reflns_number_gt                8174
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND & Olex 2.1'
_computing_publication_material  WinGX
_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)+(0.0620P)²+1.0980P] 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         8688
_refine_ls_number_parameters     568
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1268
_refine_ls_wR_factor_gt          0.1251
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.53114(7) 0.71682(6) 0.28149(2) 0.02912(15) Uani 1 1 d . . . . .
O1 O 0.29541(17) 0.85523(15) 0.24565(6) 0.0562(4) Uani 1 1 d . . . . .
O2 O 0.72131(14) 0.55594(14) 0.24190(4) 0.0418(3) Uani 1 1 d . . . . .
O3 O 0.40365(15) 0.51887(14) 0.29675(5) 0.0482(3) Uani 1 1 d . . . . .
N1 N 0.66971(14) 0.90839(13) 0.26637(4) 0.0254(3) Uani 1 1 d . . . . .
N2 N 0.61543(14) 0.76398(13) 0.35835(4) 0.0239(2) Uani 1 1 d . . . . .
N3 N 0.70253(14) 1.12261(14) 0.15510(4) 0.0271(3) Uani 1 1 d . . . . .
C1 C 0.71185(16) 1.00805(16) 0.23317(5) 0.0243(3) Uani 1 1 d . . . . .
C2 C 0.79997(17) 1.08989(17) 0.25190(5) 0.0285(3) Uani 1 1 d . . . . .
H14 H 0.8405 1.1643 0.2360 0.034 Uiso 1 1 calc R U . . .
C3 C 0.81409(18) 1.03720(17) 0.29883(5) 0.0294(3) Uani 1 1 d . . . . .
H37 H 0.8665 1.0689 0.3208 0.035 Uiso 1 1 calc R U . . .
C4 C 0.73321(16) 0.92592(16) 0.30661(5) 0.0251(3) Uani 1 1 d . . . . .
C5 C 0.70759(16) 0.84892(16) 0.35150(5) 0.0251(3) Uani 1 1 d . . . . .
H12 H 0.7610 0.8617 0.3769 0.030 Uiso 1 1 calc R U . . .
C6 C 0.66582(16) 1.02450(16) 0.18496(5) 0.0256(3) Uani 1 1 d . . . . .
H32 H 0.6093 0.9632 0.1758 0.031 Uiso 1 1 calc R U . . .
C7 C 0.58434(16) 0.69449(15) 0.40548(5) 0.0220(3) Uani 1 1 d . . . . .
C8 C 0.66762(15) 0.73215(15) 0.44618(5) 0.0216(3) Uani 1 1 d . . . . .
C9 C 0.63231(16) 0.87961(16) 0.45479(5) 0.0251(3) Uani 1 1 d . . . . .
H7 H 0.5643 0.9535 0.4349 0.030 Uiso 1 1 calc R U . . .
C10 C 0.69636(17) 0.91792(17) 0.49226(5) 0.0285(3) Uani 1 1 d . . . . .
H11 H 0.6730 1.0171 0.4968 0.034 Uiso 1 1 calc R U . . .
C11 C 0.79565(17) 0.80898(18) 0.52323(5) 0.0307(3) Uani 1 1 d . . . . .
H34 H 0.8383 0.8346 0.5486 0.037 Uiso 1 1 calc R U . . .
C12 C 0.82983(18) 0.66228(18) 0.51579(5) 0.0311(3) Uani 1 1 d . . . . .
H30 H 0.8947 0.5884 0.5365 0.037 Uiso 1 1 calc R U . . .
C13 C 0.76769(16) 0.62445(16) 0.47741(5) 0.0263(3) Uani 1 1 d . . . . .
H13 H 0.7934 0.5255 0.4725 0.032 Uiso 1 1 calc R U . . .
C14 C 0.63531(16) 0.52538(15) 0.40425(5) 0.0233(3) Uani 1 1 d . . . . .
C15 C 0.78574(18) 0.46264(17) 0.38832(5) 0.0297(3) Uani 1 1 d . . . . .
H8 H 0.8491 0.5240 0.3770 0.036 Uiso 1 1 calc R U . . .
C16 C 0.84156(19) 0.31026(18) 0.38914(5) 0.0342(3) Uani 1 1 d . . . . .
H28 H 0.9422 0.2702 0.3787 0.041 Uiso 1 1 calc R U . . .
C17 C 0.7482(2) 0.21726(17) 0.40543(6) 0.0351(4) Uani 1 1 d . . . . .
H33 H 0.7860 0.1149 0.4062 0.042 Uiso 1 1 calc R U . . .
C18 C 0.59865(19) 0.27807(17) 0.42045(5) 0.0322(3) Uani 1 1 d . . . . .
H26 H 0.5349 0.2164 0.4311 0.039 Uiso 1 1 calc R U . . .
C19 C 0.54254(17) 0.43107(16) 0.41977(5) 0.0267(3) Uani 1 1 d . . . . .
H15 H 0.4413 0.4706 0.4299 0.032 Uiso 1 1 calc R U . . .
C20 C 0.40636(16) 0.74943(15) 0.41370(5) 0.0236(3) Uani 1 1 d . . . . .
C21 C 0.34550(17) 0.72083(16) 0.45769(5) 0.0264(3) Uani 1 1 d . . . . .
H10 H 0.4135 0.6698 0.4819 0.032 Uiso 1 1 calc R U . . .
C22 C 0.18651(18) 0.76646(17) 0.46628(5) 0.0309(3) Uani 1 1 d . . . . .
H18 H 0.1490 0.7472 0.4961 0.037 Uiso 1 1 calc R U . . .
C23 C 0.0838(2) 0.8404(2) 0.43078(7) 0.0485(5) Uani 1 1 d . . . . .
H46 H -0.0235 0.8693 0.4361 0.058 Uiso 1 1 calc R U . . .
C24 C 0.1425(2) 0.8710(3) 0.38718(7) 0.0699(8) Uani 1 1 d . . . . .
H51 H 0.0739 0.9214 0.3631 0.084 Uiso 1 1 calc R U . . .
C25 C 0.3024(2) 0.8277(2) 0.37869(6) 0.0482(5) Uani 1 1 d . . . . .
H43 H 0.3398 0.8516 0.3492 0.058 Uiso 1 1 calc R U . . .
C26 C 0.65299(17) 1.14774(16) 0.10603(5) 0.0261(3) Uani 1 1 d . . . . .
C27 C 0.79076(17) 1.18755(16) 0.07781(5) 0.0263(3) Uani 1 1 d . . . . .
C28 C 0.8768(2) 1.2697(2) 0.09623(6) 0.0372(4) Uani 1 1 d . . . . .
H50 H 0.8512 1.2987 0.1253 0.045 Uiso 1 1 calc R U . . .
C29 C 0.9999(2) 1.3090(2) 0.07204(6) 0.0468(4) Uani 1 1 d . . . . .
H48 H 1.0563 1.3636 0.0850 0.056 Uiso 1 1 calc R U . . .
C30 C 1.0397(2) 1.2674(2) 0.02865(6) 0.0403(4) Uani 1 1 d . . . . .
H42 H 1.1232 1.2930 0.0125 0.048 Uiso 1 1 calc R U . . .
C31 C 0.95398(19) 1.18778(18) 0.00970(5) 0.0345(3) Uani 1 1 d . . . . .
H29 H 0.9794 1.1598 -0.0195 0.041 Uiso 1 1 calc R U . . .
C32 C 0.82964(18) 1.14890(17) 0.03389(5) 0.0301(3) Uani 1 1 d . . . . .
H25 H 0.7718 1.0964 0.0205 0.036 Uiso 1 1 calc R U . . .
C33 C 0.51256(17) 1.28743(17) 0.09889(5) 0.0282(3) Uani 1 1 d . . . . .
C34 C 0.44000(19) 1.35562(19) 0.13592(6) 0.0348(3) Uani 1 1 d . . . . .
H35 H 0.4748 1.3158 0.1660 0.042 Uiso 1 1 calc R U . . .
C35 C 0.3153(2) 1.4833(2) 0.12832(6) 0.0415(4) Uani 1 1 d . . . . .
H41 H 0.2680 1.5282 0.1534 0.050 Uiso 1 1 calc R U . . .
C36 C 0.26113(19) 1.54410(19) 0.08404(7) 0.0402(4) Uani 1 1 d . . . . .
H44 H 0.1777 1.6292 0.0793 0.048 Uiso 1 1 calc R U . . .
C37 C 0.33227(19) 1.47717(19) 0.04680(6) 0.0373(4) Uani 1 1 d . . . . .
H40 H 0.2963 1.5171 0.0168 0.045 Uiso 1 1 calc R U . . .
C38 C 0.45681(18) 1.35083(18) 0.05411(5) 0.0329(3) Uani 1 1 d . . . . .
H36 H 0.5043 1.3073 0.0288 0.039 Uiso 1 1 calc R U . . .
C39 C 0.61548(19) 1.01079(17) 0.09119(5) 0.0291(3) Uani 1 1 d . . . . .
C40 C 0.7374(2) 0.88166(18) 0.09049(5) 0.0341(3) Uani 1 1 d . . . . .
H20 H 0.8387 0.8823 0.0977 0.041 Uiso 1 1 calc R U . . .
C41 C 0.7106(2) 0.7523(2) 0.07922(6) 0.0425(4) Uani 1 1 d . . . . .
H45 H 0.7937 0.6680 0.0784 0.051 Uiso 1 1 calc R U . . .
C42 C 0.5600(3) 0.7491(2) 0.06919(6) 0.0486(5) Uani 1 1 d . . . . .
H38 H 0.5412 0.6626 0.0618 0.058 Uiso 1 1 calc R U . . .
C43 C 0.4382(3) 0.8749(2) 0.07022(6) 0.0483(5) Uani 1 1 d . . . . .
H47 H 0.3368 0.8728 0.0637 0.058 Uiso 1 1 calc R U . . .
C44 C 0.4646(2) 1.0058(2) 0.08097(5) 0.0369(4) Uani 1 1 d . . . . .
H31 H 0.3811 1.0900 0.0813 0.044 Uiso 1 1 calc R U . . .
C45 C 0.2530(2) 1.0131(2) 0.23482(8) 0.0493(5) Uani 1 1 d . . . . .
H49A H 0.3436 1.0510 0.2373 0.059 Uiso 1 1 calc R U . . .
H49B H 0.1732 1.0574 0.2559 0.059 Uiso 1 1 calc R U . . .
C46 C 0.1911(3) 1.0492(2) 0.18591(8) 0.0592(5) Uani 1 1 d . . . . .
H59A H 0.2714 1.0679 0.1643 0.071 Uiso 1 1 calc R U . . .
H59B H 0.1015 1.1359 0.1827 0.071 Uiso 1 1 calc R U . . .
C47 C 0.1439(3) 0.9121(3) 0.17762(8) 0.0612(6) Uani 1 1 d . . . . .
H60A H 0.2054 0.8659 0.1530 0.073 Uiso 1 1 calc R U . . .
H60B H 0.0336 0.9367 0.1695 0.073 Uiso 1 1 calc R U . . .
C48 C 0.1777(3) 0.8097(3) 0.22389(9) 0.0624(6) Uani 1 1 d . . . . .
H58A H 0.0840 0.8211 0.2427 0.075 Uiso 1 1 calc R U . . .
H58B H 0.2153 0.7065 0.2190 0.075 Uiso 1 1 calc R U . . .
C49 C 0.7359(2) 0.5692(3) 0.19277(7) 0.0555(5) Uani 1 1 d . . . . .
H52A H 0.6658 0.6613 0.1782 0.067 Uiso 1 1 calc R U . . .
H52B H 0.7110 0.4866 0.1812 0.067 Uiso 1 1 calc R U . . .
C50 C 0.9044(2) 0.5680(3) 0.18295(7) 0.0644(6) Uani 1 1 d . . . . .
H57A H 0.9402 0.5257 0.1549 0.077 Uiso 1 1 calc R U . . .
H57B H 0.9182 0.6676 0.1799 0.077 Uiso 1 1 calc R U . . .
C51 C 0.9895(2) 0.4721(2) 0.22469(7) 0.0515(5) Uani 1 1 d . . . . .
H56A H 1.0865 0.4965 0.2302 0.062 Uiso 1 1 calc R U . . .
H56B H 1.0124 0.3674 0.2215 0.062 Uiso 1 1 calc R U . . .
C52 C 0.8734(2) 0.5107(3) 0.26265(7) 0.0595(6) Uani 1 1 d . . . . .
H61A H 0.8819 0.4249 0.2862 0.071 Uiso 1 1 calc R U . . .
H61B H 0.8929 0.5906 0.2770 0.071 Uiso 1 1 calc R U . . .
C53 C 0.2695(2) 0.5091(3) 0.32382(7) 0.0506(5) Uani 1 1 d . . . . .
H54A H 0.1748 0.5690 0.3076 0.061 Uiso 1 1 calc R U . . .
H54B H 0.2746 0.5447 0.3532 0.061 Uiso 1 1 calc R U . . .
C54 C 0.2691(3) 0.3462(3) 0.33188(9) 0.0695(7) Uani 1 1 d . . . . .
H53A H 0.2990 0.3020 0.3636 0.083 Uiso 1 1 calc R U . . .
H53B H 0.1665 0.3348 0.3255 0.083 Uiso 1 1 calc R U . . .
C55 C 0.3882(3) 0.2767(3) 0.29841(11) 0.0746(8) Uani 1 1 d . . . . .
H62A H 0.4435 0.1758 0.3112 0.090 Uiso 1 1 calc R U . . .
H62B H 0.3389 0.2748 0.2693 0.090 Uiso 1 1 calc R U . . .
C56 C 0.4954(3) 0.3726(2) 0.29169(9) 0.0556(5) Uani 1 1 d . . . . .
H55A H 0.5791 0.3390 0.3146 0.067 Uiso 1 1 calc R U . . .
H55B H 0.5414 0.3711 0.2611 0.067 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O1 2.3308(14) . ?
Na1 O2 2.3416(13) . ?
Na1 O3 2.4101(14) . ?
Na1 N1 2.4252(13) . ?
Na1 N2 2.5197(13) . ?
O1 C45 1.424(2) . ?
O1 C48 1.426(2) . ?
O2 C49 1.424(2) . ?
O2 C52 1.424(2) . ?
O3 C53 1.421(2) . ?
O3 C56 1.426(2) . ?
N1 C1 1.3633(18) . ?
N1 C4 1.3668(18) . ?
N2 C5 1.2806(19) . ?
N2 C7 1.4845(17) . ?
N3 C6 1.2757(19) . ?
N3 C26 1.4767(17) . ?
C1 C2 1.405(2) . ?
C1 C6 1.4509(19) . ?
C2 C3 1.384(2) . ?
C2 H14 0.9300 . ?
C3 C4 1.410(2) . ?
C3 H37 0.9300 . ?
C4 C5 1.4435(19) . ?
C5 H12 0.9300 . ?
C6 H32 0.9300 . ?
C7 C14 1.5417(18) . ?
C7 C20 1.5434(18) . ?
C7 C8 1.5478(18) . ?
C8 C13 1.3948(19) . ?
C8 C9 1.3989(19) . ?
C9 C10 1.382(2) . ?
C9 H7 0.9300 . ?
C10 C11 1.393(2) . ?
C10 H11 0.9300 . ?
C11 C12 1.382(2) . ?
C11 H34 0.9300 . ?
C12 C13 1.394(2) . ?
C12 H30 0.9300 . ?
C13 H13 0.9300 . ?
C14 C19 1.386(2) . ?
C14 C15 1.399(2) . ?
C15 C16 1.385(2) . ?
C15 H8 0.9300 . ?
C16 C17 1.386(2) . ?
C16 H28 0.9300 . ?
C17 C18 1.379(2) . ?
C17 H33 0.9300 . ?
C18 C19 1.391(2) . ?
C18 H26 0.9300 . ?
C19 H15 0.9300 . ?
C20 C25 1.382(2) . ?
C20 C21 1.393(2) . ?
C21 C22 1.383(2) . ?
C21 H10 0.9300 . ?
C22 C23 1.376(2) . ?
C22 H18 0.9300 . ?
C23 C24 1.378(3) . ?
C23 H46 0.9300 . ?
C24 C25 1.389(3) . ?
C24 H51 0.9300 . ?
C25 H43 0.9300 . ?
C26 C39 1.538(2) . ?
C26 C33 1.544(2) . ?
C26 C27 1.5480(19) . ?
C27 C32 1.390(2) . ?
C27 C28 1.390(2) . ?
C28 C29 1.383(2) . ?
C28 H50 0.9300 . ?
C29 C30 1.385(3) . ?
C29 H48 0.9300 . ?
C30 C31 1.377(3) . ?
C30 H42 0.9300 . ?
C31 C32 1.391(2) . ?
C31 H29 0.9300 . ?
C32 H25 0.9300 . ?
C33 C34 1.388(2) . ?
C33 C38 1.400(2) . ?
C34 C35 1.394(2) . ?
C34 H35 0.9300 . ?
C35 C36 1.379(3) . ?
C35 H41 0.9300 . ?
C36 C37 1.384(3) . ?
C36 H44 0.9300 . ?
C37 C38 1.385(2) . ?
C37 H40 0.9300 . ?
C38 H36 0.9300 . ?
C39 C44 1.392(2) . ?
C39 C40 1.396(2) . ?
C40 C41 1.388(2) . ?
C40 H20 0.9300 . ?
C41 C42 1.383(3) . ?
C41 H45 0.9300 . ?
C42 C43 1.376(3) . ?
C42 H38 0.9300 . ?
C43 C44 1.395(3) . ?
C43 H47 0.9300 . ?
C44 H31 0.9300 . ?
C45 C46 1.503(3) . ?
C45 H49A 0.9700 . ?
C45 H49B 0.9700 . ?
C46 C47 1.513(3) . ?
C46 H59A 0.9700 . ?
C46 H59B 0.9700 . ?
C47 C48 1.528(3) . ?
C47 H60A 0.9700 . ?
C47 H60B 0.9700 . ?
C48 H58A 0.9700 . ?
C48 H58B 0.9700 . ?
C49 C50 1.507(3) . ?
C49 H52A 0.9700 . ?
C49 H52B 0.9700 . ?
C50 C51 1.497(3) . ?
C50 H57A 0.9700 . ?
C50 H57B 0.9700 . ?
C51 C52 1.503(3) . ?
C51 H56A 0.9700 . ?
C51 H56B 0.9700 . ?
C52 H61A 0.9700 . ?
C52 H61B 0.9700 . ?
C53 C54 1.521(3) . ?
C53 H54A 0.9700 . ?
C53 H54B 0.9700 . ?
C54 C55 1.497(4) . ?
C54 H53A 0.9700 . ?
C54 H53B 0.9700 . ?
C55 C56 1.467(3) . ?
C55 H62A 0.9700 . ?
C55 H62B 0.9700 . ?
C56 H55A 0.9700 . ?
C56 H55B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Na1 O2 121.07(6) . . ?
O1 Na1 O3 85.10(5) . . ?
O2 Na1 O3 86.80(5) . . ?
O1 Na1 N1 97.05(5) . . ?
O2 Na1 N1 91.25(5) . . ?
O3 Na1 N1 177.65(5) . . ?
O1 Na1 N2 122.13(5) . . ?
O2 Na1 N2 115.96(5) . . ?
O3 Na1 N2 107.56(5) . . ?
N1 Na1 N2 72.13(4) . . ?
C45 O1 C48 104.81(15) . . ?
C45 O1 Na1 123.66(11) . . ?
C48 O1 Na1 130.88(13) . . ?
C49 O2 C52 109.44(14) . . ?
C49 O2 Na1 124.67(12) . . ?
C52 O2 Na1 114.76(11) . . ?
C53 O3 C56 109.16(15) . . ?
C53 O3 Na1 130.39(12) . . ?
C56 O3 Na1 117.18(11) . . ?
C1 N1 C4 104.88(12) . . ?
C1 N1 Na1 145.13(10) . . ?
C4 N1 Na1 109.98(9) . . ?
C5 N2 C7 122.05(12) . . ?
C5 N2 Na1 109.50(9) . . ?
C7 N2 Na1 128.08(9) . . ?
C6 N3 C26 122.37(12) . . ?
N1 C1 C2 111.74(12) . . ?
N1 C1 C6 122.02(13) . . ?
C2 C1 C6 126.24(13) . . ?
C3 C2 C1 105.94(13) . . ?
C3 C2 H14 127.0 . . ?
C1 C2 H14 127.0 . . ?
C2 C3 C4 106.27(13) . . ?
C2 C3 H37 126.9 . . ?
C4 C3 H37 126.9 . . ?
N1 C4 C3 111.17(12) . . ?
N1 C4 C5 123.58(13) . . ?
C3 C4 C5 125.04(13) . . ?
N2 C5 C4 123.70(13) . . ?
N2 C5 H12 118.2 . . ?
C4 C5 H12 118.2 . . ?
N3 C6 C1 120.34(13) . . ?
N3 C6 H32 119.8 . . ?
C1 C6 H32 119.8 . . ?
N2 C7 C14 105.56(10) . . ?
N2 C7 C20 107.03(11) . . ?
C14 C7 C20 111.25(11) . . ?
N2 C7 C8 116.33(11) . . ?
C14 C7 C8 109.81(11) . . ?
C20 C7 C8 106.88(10) . . ?
C13 C8 C9 117.45(13) . . ?
C13 C8 C7 123.25(12) . . ?
C9 C8 C7 119.09(12) . . ?
C10 C9 C8 121.42(13) . . ?
C10 C9 H7 119.3 . . ?
C8 C9 H7 119.3 . . ?
C9 C10 C11 120.41(14) . . ?
C9 C10 H11 119.8 . . ?
C11 C10 H11 119.8 . . ?
C12 C11 C10 119.06(14) . . ?
C12 C11 H34 120.5 . . ?
C10 C11 H34 120.5 . . ?
C11 C12 C13 120.36(14) . . ?
C11 C12 H30 119.8 . . ?
C13 C12 H30 119.8 . . ?
C12 C13 C8 121.27(13) . . ?
C12 C13 H13 119.4 . . ?
C8 C13 H13 119.4 . . ?
C19 C14 C15 118.08(13) . . ?
C19 C14 C7 123.57(12) . . ?
C15 C14 C7 118.30(12) . . ?
C16 C15 C14 120.87(14) . . ?
C16 C15 H8 119.6 . . ?
C14 C15 H8 119.6 . . ?
C15 C16 C17 120.33(14) . . ?
C15 C16 H28 119.8 . . ?
C17 C16 H28 119.8 . . ?
C18 C17 C16 119.32(14) . . ?
C18 C17 H33 120.3 . . ?
C16 C17 H33 120.3 . . ?
C17 C18 C19 120.44(15) . . ?
C17 C18 H26 119.8 . . ?
C19 C18 H26 119.8 . . ?
C14 C19 C18 120.95(14) . . ?
C14 C19 H15 119.5 . . ?
C18 C19 H15 119.5 . . ?
C25 C20 C21 117.67(14) . . ?
C25 C20 C7 122.37(13) . . ?
C21 C20 C7 119.96(12) . . ?
C22 C21 C20 121.67(14) . . ?
C22 C21 H10 119.2 . . ?
C20 C21 H10 119.2 . . ?
C23 C22 C21 120.03(15) . . ?
C23 C22 H18 120.0 . . ?
C21 C22 H18 120.0 . . ?
C22 C23 C24 118.97(16) . . ?
C22 C23 H46 120.5 . . ?
C24 C23 H46 120.5 . . ?
C23 C24 C25 121.05(17) . . ?
C23 C24 H51 119.5 . . ?
C25 C24 H51 119.5 . . ?
C20 C25 C24 120.57(16) . . ?
C20 C25 H43 119.7 . . ?
C24 C25 H43 119.7 . . ?
N3 C26 C39 112.37(11) . . ?
N3 C26 C33 107.89(11) . . ?
C39 C26 C33 112.50(12) . . ?
N3 C26 C27 105.57(11) . . ?
C39 C26 C27 111.33(12) . . ?
C33 C26 C27 106.77(11) . . ?
C32 C27 C28 118.08(14) . . ?
C32 C27 C26 122.84(13) . . ?
C28 C27 C26 119.05(13) . . ?
C29 C28 C27 121.00(15) . . ?
C29 C28 H50 119.5 . . ?
C27 C28 H50 119.5 . . ?
C28 C29 C30 120.49(16) . . ?
C28 C29 H48 119.8 . . ?
C30 C29 H48 119.8 . . ?
C31 C30 C29 119.11(15) . . ?
C31 C30 H42 120.4 . . ?
C29 C30 H42 120.4 . . ?
C30 C31 C32 120.47(15) . . ?
C30 C31 H29 119.8 . . ?
C32 C31 H29 119.8 . . ?
C27 C32 C31 120.83(15) . . ?
C27 C32 H25 119.6 . . ?
C31 C32 H25 119.6 . . ?
C34 C33 C38 118.06(15) . . ?
C34 C33 C26 121.76(13) . . ?
C38 C33 C26 120.17(13) . . ?
C33 C34 C35 120.47(15) . . ?
C33 C34 H35 119.8 . . ?
C35 C34 H35 119.8 . . ?
C36 C35 C34 120.83(16) . . ?
C36 C35 H41 119.6 . . ?
C34 C35 H41 119.6 . . ?
C35 C36 C37 119.32(16) . . ?
C35 C36 H44 120.3 . . ?
C37 C36 H44 120.3 . . ?
C36 C37 C38 120.11(16) . . ?
C36 C37 H40 119.9 . . ?
C38 C37 H40 119.9 . . ?
C37 C38 C33 121.22(15) . . ?
C37 C38 H36 119.4 . . ?
C33 C38 H36 119.4 . . ?
C44 C39 C40 118.00(15) . . ?
C44 C39 C26 123.45(15) . . ?
C40 C39 C26 118.44(14) . . ?
C41 C40 C39 121.42(16) . . ?
C41 C40 H20 119.3 . . ?
C39 C40 H20 119.3 . . ?
C42 C41 C40 119.88(18) . . ?
C42 C41 H45 120.1 . . ?
C40 C41 H45 120.1 . . ?
C43 C42 C41 119.43(17) . . ?
C43 C42 H38 120.3 . . ?
C41 C42 H38 120.3 . . ?
C42 C43 C44 120.97(18) . . ?
C42 C43 H47 119.5 . . ?
C44 C43 H47 119.5 . . ?
C39 C44 C43 120.29(18) . . ?
C39 C44 H31 119.9 . . ?
C43 C44 H31 119.9 . . ?
O1 C45 C46 106.50(16) . . ?
O1 C45 H49A 110.4 . . ?
C46 C45 H49A 110.4 . . ?
O1 C45 H49B 110.4 . . ?
C46 C45 H49B 110.4 . . ?
H49A C45 H49B 108.6 . . ?
C45 C46 C47 104.40(17) . . ?
C45 C46 H59A 110.9 . . ?
C47 C46 H59A 110.9 . . ?
C45 C46 H59B 110.9 . . ?
C47 C46 H59B 110.9 . . ?
H59A C46 H59B 108.9 . . ?
C46 C47 C48 104.04(17) . . ?
C46 C47 H60A 110.9 . . ?
C48 C47 H60A 110.9 . . ?
C46 C47 H60B 110.9 . . ?
C48 C47 H60B 110.9 . . ?
H60A C47 H60B 109.0 . . ?
O1 C48 C47 105.01(18) . . ?
O1 C48 H58A 110.7 . . ?
C47 C48 H58A 110.7 . . ?
O1 C48 H58B 110.7 . . ?
C47 C48 H58B 110.7 . . ?
H58A C48 H58B 108.8 . . ?
O2 C49 C50 105.62(16) . . ?
O2 C49 H52A 110.6 . . ?
C50 C49 H52A 110.6 . . ?
O2 C49 H52B 110.6 . . ?
C50 C49 H52B 110.6 . . ?
H52A C49 H52B 108.7 . . ?
C51 C50 C49 103.04(17) . . ?
C51 C50 H57A 111.2 . . ?
C49 C50 H57A 111.2 . . ?
C51 C50 H57B 111.2 . . ?
C49 C50 H57B 111.2 . . ?
H57A C50 H57B 109.1 . . ?
C50 C51 C52 102.07(17) . . ?
C50 C51 H56A 111.4 . . ?
C52 C51 H56A 111.4 . . ?
C50 C51 H56B 111.4 . . ?
C52 C51 H56B 111.4 . . ?
H56A C51 H56B 109.2 . . ?
O2 C52 C51 107.12(16) . . ?
O2 C52 H61A 110.3 . . ?
C51 C52 H61A 110.3 . . ?
O2 C52 H61B 110.3 . . ?
C51 C52 H61B 110.3 . . ?
H61A C52 H61B 108.5 . . ?
O3 C53 C54 106.98(18) . . ?
O3 C53 H54A 110.3 . . ?
C54 C53 H54A 110.3 . . ?
O3 C53 H54B 110.3 . . ?
C54 C53 H54B 110.3 . . ?
H54A C53 H54B 108.6 . . ?
C55 C54 C53 103.83(18) . . ?
C55 C54 H53A 111.0 . . ?
C53 C54 H53A 111.0 . . ?
C55 C54 H53B 111.0 . . ?
C53 C54 H53B 111.0 . . ?
H53A C54 H53B 109.0 . . ?
C56 C55 C54 104.3(2) . . ?
C56 C55 H62A 110.9 . . ?
C54 C55 H62A 110.9 . . ?
C56 C55 H62B 110.9 . . ?
C54 C55 H62B 110.9 . . ?
H62A C55 H62B 108.9 . . ?
O3 C56 C55 106.42(18) . . ?
O3 C56 H55A 110.4 . . ?
C55 C56 H55A 110.4 . . ?
O3 C56 H55B 110.4 . . ?
C55 C56 H55B 110.4 . . ?
H55A C56 H55B 108.6 . . ?

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
C4 N1 C1 C2 -0.64(16) . . . . ?
Na1 N1 C1 C2 179.78(12) . . . . ?
C4 N1 C1 C6 -179.74(13) . . . . ?
Na1 N1 C1 C6 0.7(3) . . . . ?
N1 C1 C2 C3 0.57(17) . . . . ?
C6 C1 C2 C3 179.62(14) . . . . ?
C1 C2 C3 C4 -0.25(17) . . . . ?
C1 N1 C4 C3 0.47(16) . . . . ?
Na1 N1 C4 C3 -179.78(10) . . . . ?
C1 N1 C4 C5 175.35(13) . . . . ?
Na1 N1 C4 C5 -4.91(17) . . . . ?
C2 C3 C4 N1 -0.14(17) . . . . ?
C2 C3 C4 C5 -174.92(14) . . . . ?
C7 N2 C5 C4 -175.96(12) . . . . ?
Na1 N2 C5 C4 10.53(17) . . . . ?
N1 C4 C5 N2 -4.5(2) . . . . ?
C3 C4 C5 N2 169.70(14) . . . . ?
C26 N3 C6 C1 -177.48(13) . . . . ?
N1 C1 C6 N3 177.46(13) . . . . ?
C2 C1 C6 N3 -1.5(2) . . . . ?
C5 N2 C7 C14 -121.15(14) . . . . ?
Na1 N2 C7 C14 51.07(14) . . . . ?
C5 N2 C7 C20 120.24(14) . . . . ?
Na1 N2 C7 C20 -67.53(13) . . . . ?
C5 N2 C7 C8 0.88(18) . . . . ?
Na1 N2 C7 C8 173.10(8) . . . . ?
N2 C7 C8 C13 -122.31(14) . . . . ?
C14 C7 C8 C13 -2.55(17) . . . . ?
C20 C7 C8 C13 118.24(14) . . . . ?
N2 C7 C8 C9 63.05(16) . . . . ?
C14 C7 C8 C9 -177.19(12) . . . . ?
C20 C7 C8 C9 -56.40(15) . . . . ?
C13 C8 C9 C10 1.2(2) . . . . ?
C7 C8 C9 C10 176.19(12) . . . . ?
C8 C9 C10 C11 -1.5(2) . . . . ?
C9 C10 C11 C12 0.4(2) . . . . ?
C10 C11 C12 C13 1.0(2) . . . . ?
C11 C12 C13 C8 -1.3(2) . . . . ?
C9 C8 C13 C12 0.2(2) . . . . ?
C7 C8 C13 C12 -174.57(13) . . . . ?
N2 C7 C14 C19 -130.57(13) . . . . ?
C20 C7 C14 C19 -14.81(18) . . . . ?
C8 C7 C14 C19 103.30(15) . . . . ?
N2 C7 C14 C15 52.07(16) . . . . ?
C20 C7 C14 C15 167.82(12) . . . . ?
C8 C7 C14 C15 -74.07(15) . . . . ?
C19 C14 C15 C16 -1.6(2) . . . . ?
C7 C14 C15 C16 175.94(13) . . . . ?
C14 C15 C16 C17 0.6(2) . . . . ?
C15 C16 C17 C18 0.6(2) . . . . ?
C16 C17 C18 C19 -0.7(2) . . . . ?
C15 C14 C19 C18 1.4(2) . . . . ?
C7 C14 C19 C18 -175.98(13) . . . . ?
C17 C18 C19 C14 -0.3(2) . . . . ?
N2 C7 C20 C25 9.6(2) . . . . ?
C14 C7 C20 C25 -105.21(17) . . . . ?
C8 C7 C20 C25 134.92(16) . . . . ?
N2 C7 C20 C21 -170.20(12) . . . . ?
C14 C7 C20 C21 74.96(16) . . . . ?
C8 C7 C20 C21 -44.91(16) . . . . ?
C25 C20 C21 C22 1.1(2) . . . . ?
C7 C20 C21 C22 -179.11(13) . . . . ?
C20 C21 C22 C23 0.9(2) . . . . ?
C21 C22 C23 C24 -1.6(3) . . . . ?
C22 C23 C24 C25 0.4(4) . . . . ?
C21 C20 C25 C24 -2.3(3) . . . . ?
C7 C20 C25 C24 177.9(2) . . . . ?
C23 C24 C25 C20 1.6(4) . . . . ?
C6 N3 C26 C39 -23.09(19) . . . . ?
C6 N3 C26 C33 101.51(15) . . . . ?
C6 N3 C26 C27 -144.62(14) . . . . ?
N3 C26 C27 C32 147.09(14) . . . . ?
C39 C26 C27 C32 24.88(19) . . . . ?
C33 C26 C27 C32 -98.27(16) . . . . ?
N3 C26 C27 C28 -35.09(18) . . . . ?
C39 C26 C27 C28 -157.30(14) . . . . ?
C33 C26 C27 C28 79.55(16) . . . . ?
C32 C27 C28 C29 -1.5(3) . . . . ?
C26 C27 C28 C29 -179.39(16) . . . . ?
C27 C28 C29 C30 0.2(3) . . . . ?
C28 C29 C30 C31 0.7(3) . . . . ?
C29 C30 C31 C32 -0.3(3) . . . . ?
C28 C27 C32 C31 1.8(2) . . . . ?
C26 C27 C32 C31 179.65(14) . . . . ?
C30 C31 C32 C27 -0.9(2) . . . . ?
N3 C26 C33 C34 -8.55(18) . . . . ?
C39 C26 C33 C34 115.97(15) . . . . ?
C27 C26 C33 C34 -121.61(15) . . . . ?
N3 C26 C33 C38 170.13(13) . . . . ?
C39 C26 C33 C38 -65.36(17) . . . . ?
C27 C26 C33 C38 57.06(17) . . . . ?
C38 C33 C34 C35 0.1(2) . . . . ?
C26 C33 C34 C35 178.77(14) . . . . ?
C33 C34 C35 C36 0.3(3) . . . . ?
C34 C35 C36 C37 -0.2(3) . . . . ?
C35 C36 C37 C38 -0.2(2) . . . . ?
C36 C37 C38 C33 0.6(2) . . . . ?
C34 C33 C38 C37 -0.5(2) . . . . ?
C26 C33 C38 C37 -179.20(14) . . . . ?
N3 C26 C39 C44 110.50(16) . . . . ?
C33 C26 C39 C44 -11.51(19) . . . . ?
C27 C26 C39 C44 -131.32(14) . . . . ?
N3 C26 C39 C40 -65.64(17) . . . . ?
C33 C26 C39 C40 172.35(12) . . . . ?
C27 C26 C39 C40 52.54(17) . . . . ?
C44 C39 C40 C41 1.1(2) . . . . ?
C26 C39 C40 C41 177.42(14) . . . . ?
C39 C40 C41 C42 -1.2(2) . . . . ?
C40 C41 C42 C43 0.4(3) . . . . ?
C41 C42 C43 C44 0.4(3) . . . . ?
C40 C39 C44 C43 -0.3(2) . . . . ?
C26 C39 C44 C43 -176.43(14) . . . . ?
C42 C43 C44 C39 -0.4(3) . . . . ?
C48 O1 C45 C46 -37.8(2) . . . . ?
Na1 O1 C45 C46 133.83(15) . . . . ?
O1 C45 C46 C47 21.3(2) . . . . ?
C45 C46 C47 C48 2.1(2) . . . . ?
C45 O1 C48 C47 38.7(2) . . . . ?
Na1 O1 C48 C47 -132.09(17) . . . . ?
C46 C47 C48 O1 -24.6(2) . . . . ?
C52 O2 C49 C50 -14.2(3) . . . . ?
Na1 O2 C49 C50 127.48(17) . . . . ?
O2 C49 C50 C51 31.1(3) . . . . ?
C49 C50 C51 C52 -35.0(3) . . . . ?
C49 O2 C52 C51 -8.5(3) . . . . ?
Na1 O2 C52 C51 -154.31(14) . . . . ?
C50 C51 C52 O2 27.5(2) . . . . ?
C56 O3 C53 C54 -6.2(2) . . . . ?
Na1 O3 C53 C54 -164.73(13) . . . . ?
O3 C53 C54 C55 -12.9(2) . . . . ?
C53 C54 C55 C56 26.5(3) . . . . ?
C53 O3 C56 C55 23.6(2) . . . . ?
Na1 O3 C56 C55 -174.70(16) . . . . ?
C54 C55 C56 O3 -31.1(3) . . . . ?

_refine_diff_density_max         0.870
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.042



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

data_3-k
_database_code_depnum_ccdc_archive 'CCDC 1476173'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-08-18 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            'C56 H58 K N3 O3'
_chemical_formula_weight         860.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   9.7401(3)
_cell_length_b                   17.9994(6)
_cell_length_c                   28.4384(9)
_cell_angle_alpha                97.723(3)
_cell_angle_beta                 95.643(2)
_cell_angle_gamma                104.922(3)
_cell_volume                     4727.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    16421
_cell_measurement_theta_min      3.2381
_cell_measurement_theta_max      70.7245

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_F_000             1832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    1.346
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       w/scan
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36317
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.241
_diffrn_reflns_theta_max         69.995
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             17729
_reflns_number_gt                15459
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX
_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)+(0.1540P)²+3.2980P] 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         17729
_refine_ls_number_parameters     1123
_refine_ls_number_restraints     1132
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0804
_refine_ls_wR_factor_ref         0.2401
_refine_ls_wR_factor_gt          0.2327
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7313(3) 0.25002(14) 0.71808(8) 0.0316(5) Uani 1 1 d . U . . .
C2 C 0.7149(3) 0.32415(16) 0.73381(9) 0.0381(5) Uani 1 1 d . U . . .
H2 H 0.6639 0.3516 0.7169 0.046 Uiso 1 1 calc R U . . .
C3 C 0.7903(3) 0.34802(15) 0.77965(9) 0.0376(5) Uani 1 1 d . U . . .
H3 H 0.7993 0.3945 0.8000 0.045 Uiso 1 1 calc R U . . .
C4 C 0.8508(3) 0.28711(14) 0.78914(8) 0.0313(5) Uani 1 1 d . U . . .
C5 C 0.6692(3) 0.20190(15) 0.67222(8) 0.0329(5) Uani 1 1 d . U . . .
H5 H 0.6282 0.2244 0.6489 0.039 Uiso 1 1 calc R U . . .
C6 C 0.6107(3) 0.08517(15) 0.61281(8) 0.0318(5) Uani 1 1 d . U . . .
C7 C 0.5534(3) 0.13315(15) 0.57891(8) 0.0342(5) Uani 1 1 d . U . . .
C8 C 0.4236(3) 0.15084(18) 0.58532(10) 0.0445(6) Uani 1 1 d . U . . .
H8 H 0.3705 0.1296 0.6081 0.053 Uiso 1 1 calc R U . . .
C9 C 0.3732(3) 0.1993(2) 0.55828(11) 0.0525(7) Uani 1 1 d . U . . .
H9 H 0.2877 0.2110 0.5634 0.063 Uiso 1 1 calc R U . . .
C10 C 0.4494(3) 0.23042(19) 0.52371(11) 0.0508(7) Uani 1 1 d . U . . .
H10 H 0.4152 0.2625 0.5053 0.061 Uiso 1 1 calc R U . . .
C11 C 0.5766(3) 0.21334(18) 0.51674(11) 0.0489(7) Uani 1 1 d . U . . .
H11 H 0.6285 0.2343 0.4936 0.059 Uiso 1 1 calc R U . . .
C12 C 0.6289(3) 0.16478(16) 0.54416(9) 0.0390(6) Uani 1 1 d . U . . .
H12 H 0.7148 0.1537 0.5390 0.047 Uiso 1 1 calc R U . . .
C13 C 0.4907(3) 0.01275(15) 0.61790(9) 0.0351(5) Uani 1 1 d . U . . .
C14 C 0.4808(3) -0.01435(16) 0.66105(9) 0.0389(5) Uani 1 1 d . U . . .
H14 H 0.5456 0.0127 0.6879 0.047 Uiso 1 1 calc R U . . .
C15 C 0.3762(3) -0.08105(17) 0.66506(11) 0.0478(6) Uani 1 1 d . U . . .
H15 H 0.3717 -0.0981 0.6945 0.057 Uiso 1 1 calc R U . . .
C16 C 0.2784(3) -0.12252(17) 0.62566(12) 0.0481(7) Uani 1 1 d . U . . .
H16 H 0.2088 -0.1675 0.6283 0.058 Uiso 1 1 calc R U . . .
C17 C 0.2859(3) -0.09601(18) 0.58260(12) 0.0508(7) Uani 1 1 d . U . . .
H17 H 0.2209 -0.1234 0.5559 0.061 Uiso 1 1 calc R U . . .
C18 C 0.3900(3) -0.02843(18) 0.57854(10) 0.0447(6) Uani 1 1 d . U . . .
H18 H 0.3923 -0.0106 0.5493 0.054 Uiso 1 1 calc R U . . .
C19 C 0.7384(3) 0.05911(15) 0.59451(8) 0.0339(5) Uani 1 1 d . U . . .
C20 C 0.7170(3) -0.00497(17) 0.55835(9) 0.0405(6) Uani 1 1 d . U . . .
H20 H 0.6241 -0.0330 0.5449 0.049 Uiso 1 1 calc R U . . .
C21 C 0.8328(3) -0.0275(2) 0.54206(11) 0.0499(7) Uani 1 1 d . U . . .
H21 H 0.8166 -0.0702 0.5178 0.060 Uiso 1 1 calc R U . . .
C22 C 0.9719(4) 0.0135(2) 0.56174(11) 0.0566(8) Uani 1 1 d . U . . .
H22 H 1.0492 -0.0019 0.5511 0.068 Uiso 1 1 calc R U . . .
C23 C 0.9946(3) 0.0775(2) 0.59739(11) 0.0551(8) Uani 1 1 d . U . . .
H23 H 1.0877 0.1055 0.6107 0.066 Uiso 1 1 calc R U . . .
C24 C 0.8784(3) 0.10011(19) 0.61336(10) 0.0457(6) Uani 1 1 d . U . . .
H24 H 0.8950 0.1435 0.6371 0.055 Uiso 1 1 calc R U . . .
C25 C 0.9397(3) 0.28726(13) 0.83323(8) 0.0311(5) Uani 1 1 d . U . . .
H25 H 0.9586 0.3306 0.8572 0.037 Uiso 1 1 calc R U . . .
C26 C 1.0796(3) 0.23683(13) 0.88835(8) 0.0300(5) Uani 1 1 d . U . . .
C27 C 1.0490(3) 0.29387(14) 0.92856(8) 0.0309(5) Uani 1 1 d . U . . .
C28 C 0.9067(3) 0.28483(15) 0.93773(9) 0.0373(5) Uani 1 1 d . U . . .
H28 H 0.8339 0.2436 0.9200 0.045 Uiso 1 1 calc R U . . .
C29 C 0.8731(3) 0.33612(17) 0.97256(10) 0.0453(6) Uani 1 1 d . U . . .
H29 H 0.7783 0.3292 0.9780 0.054 Uiso 1 1 calc R U . . .
C30 C 0.9797(4) 0.39760(18) 0.99940(10) 0.0501(7) Uani 1 1 d . U . . .
H30 H 0.9569 0.4328 1.0223 0.060 Uiso 1 1 calc R U . . .
C31 C 1.1213(4) 0.40632(18) 0.99180(11) 0.0510(7) Uani 1 1 d . U . . .
H31 H 1.1942 0.4463 1.0105 0.061 Uiso 1 1 calc R U . . .
C32 C 1.1544(3) 0.35536(15) 0.95628(9) 0.0399(6) Uani 1 1 d . U . . .
H32 H 1.2493 0.3627 0.9510 0.048 Uiso 1 1 calc R U . . .
C33 C 1.2399(3) 0.25819(13) 0.88263(9) 0.0323(5) Uani 1 1 d . U . . .
C34 C 1.2910(3) 0.29448(15) 0.84541(9) 0.0375(5) Uani 1 1 d . U . . .
H34 H 1.2278 0.3079 0.8235 0.045 Uiso 1 1 calc R U . . .
C35 C 1.4363(3) 0.31115(17) 0.84042(11) 0.0463(6) Uani 1 1 d . U . . .
H35 H 1.4684 0.3341 0.8147 0.056 Uiso 1 1 calc R U . . .
C36 C 1.5328(3) 0.29413(17) 0.87312(12) 0.0488(7) Uani 1 1 d . U . . .
H36 H 1.6297 0.3059 0.8697 0.059 Uiso 1 1 calc R U . . .
C37 C 1.4841(3) 0.25935(17) 0.91095(12) 0.0478(7) Uani 1 1 d . U . . .
H37 H 1.5486 0.2483 0.9335 0.057 Uiso 1 1 calc R U . . .
C38 C 1.3391(3) 0.24086(16) 0.91540(10) 0.0412(6) Uani 1 1 d . U . . .
H38 H 1.3073 0.2165 0.9407 0.049 Uiso 1 1 calc R U . . .
C39 C 1.0404(3) 0.15261(14) 0.89945(9) 0.0324(5) Uani 1 1 d . U . . .
C40 C 1.0470(3) 0.09290(16) 0.86363(10) 0.0425(6) Uani 1 1 d . U . . .
H40 H 1.0702 0.1044 0.8340 0.051 Uiso 1 1 calc R U . . .
C41 C 1.0193(4) 0.01659(17) 0.87188(12) 0.0509(7) Uani 1 1 d . U . . .
H41 H 1.0248 -0.0227 0.8479 0.061 Uiso 1 1 calc R U . . .
C42 C 0.9834(3) -0.00146(17) 0.91587(12) 0.0506(7) Uani 1 1 d . U . . .
H42 H 0.9641 -0.0527 0.9213 0.061 Uiso 1 1 calc R U . . .
C43 C 0.9767(3) 0.05670(17) 0.95119(11) 0.0470(6) Uani 1 1 d . U . . .
H43 H 0.9524 0.0448 0.9806 0.056 Uiso 1 1 calc R U . . .
C44 C 1.0060(3) 0.13389(16) 0.94329(9) 0.0386(6) Uani 1 1 d . U . . .
H44 H 1.0023 0.1730 0.9677 0.046 Uiso 1 1 calc R U . . .
C45 C 0.8300(5) -0.1002(3) 0.66351(15) 0.0790(11) Uani 1 1 d . U . . .
H45A H 0.9079 -0.1244 0.6669 0.095 Uiso 1 1 calc R U . . .
H45B H 0.8591 -0.0565 0.6467 0.095 Uiso 1 1 calc R U . . .
C46 C 0.6988(6) -0.1572(3) 0.63699(18) 0.0879(13) Uani 1 1 d . U . . .
H46A H 0.6402 -0.1313 0.6193 0.106 Uiso 1 1 calc R U . . .
H46B H 0.7231 -0.1959 0.6146 0.106 Uiso 1 1 calc R U . . .
C47 C 0.6229(7) -0.1937(3) 0.67321(18) 0.0908(14) Uani 1 1 d . U . . .
H47A H 0.6351 -0.2454 0.6738 0.109 Uiso 1 1 calc R U . . .
H47B H 0.5213 -0.1978 0.6671 0.109 Uiso 1 1 calc R U . . .
C48 C 0.6899(7) -0.1408(3) 0.71904(17) 0.0981(16) Uani 1 1 d . U . . .
H48A H 0.6170 -0.1235 0.7348 0.118 Uiso 1 1 calc R U . . .
H48B H 0.7350 -0.1684 0.7402 0.118 Uiso 1 1 calc R U . . .
C49 C 1.1630(5) 0.0196(3) 0.7367(2) 0.1028(17) Uani 1 1 d . U . . .
H49A H 1.1704 -0.0106 0.7066 0.123 Uiso 1 1 calc R U . . .
H49B H 1.1066 -0.0150 0.7554 0.123 Uiso 1 1 calc R U . . .
C50 C 1.3062(5) 0.0592(4) 0.7634(2) 0.1002(16) Uani 1 1 d . U . . .
H50A H 1.3726 0.0279 0.7583 0.120 Uiso 1 1 calc R U . . .
H50B H 1.3022 0.0708 0.7974 0.120 Uiso 1 1 calc R U . . .
C51 C 1.3482(6) 0.1317(4) 0.7426(3) 0.1172(19) Uani 1 1 d . U . . .
H51A H 1.3955 0.1235 0.7147 0.141 Uiso 1 1 calc R U . . .
H51B H 1.4123 0.1736 0.7660 0.141 Uiso 1 1 calc R U . . .
C52 C 1.2066(6) 0.1508(3) 0.7288(2) 0.0978(14) Uani 1 1 d . U . . .
H52A H 1.1944 0.1924 0.7520 0.117 Uiso 1 1 calc R U . . .
H52B H 1.2030 0.1662 0.6974 0.117 Uiso 1 1 calc R U . . .
C53 C 0.6525(4) 0.10476(18) 0.83522(12) 0.0527(7) Uani 1 1 d . U . . .
H53A H 0.5907 0.1327 0.8211 0.063 Uiso 1 1 calc R U . . .
H53B H 0.7497 0.1387 0.8421 0.063 Uiso 1 1 calc R U . . .
C54 C 0.6029(7) 0.0803(2) 0.87939(16) 0.0919(16) Uani 1 1 d . U . . .
H54A H 0.6825 0.0949 0.9052 0.110 Uiso 1 1 calc R U . . .
H54B H 0.5305 0.1054 0.8888 0.110 Uiso 1 1 calc R U . . .
C55 C 0.5431(5) -0.0038(2) 0.86971(14) 0.0715(11) Uani 1 1 d . U . . .
H55A H 0.4396 -0.0178 0.8617 0.086 Uiso 1 1 calc R U . . .
H55B H 0.5673 -0.0270 0.8971 0.086 Uiso 1 1 calc R U . . .
C56 C 0.6117(4) -0.02943(19) 0.82781(13) 0.0607(8) Uani 1 1 d . U . . .
H56A H 0.6972 -0.0440 0.8387 0.073 Uiso 1 1 calc R U . . .
H56B H 0.5456 -0.0740 0.8069 0.073 Uiso 1 1 calc R U . . .
C57 C 0.2419(3) 0.72201(15) 0.72028(8) 0.0329(5) Uani 1 1 d . U . . .
C58 C 0.1917(3) 0.78600(15) 0.73630(9) 0.0351(5) Uani 1 1 d . U . . .
H58 H 0.1238 0.8043 0.7196 0.042 Uiso 1 1 calc R U . . .
C59 C 0.2639(3) 0.81634(15) 0.78210(8) 0.0344(5) Uani 1 1 d . U . . .
H59 H 0.2553 0.8597 0.8022 0.041 Uiso 1 1 calc R U . . .
C60 C 0.3531(3) 0.76820(15) 0.79219(8) 0.0322(5) Uani 1 1 d . U . . .
C61 C 0.2083(3) 0.67071(15) 0.67447(8) 0.0344(5) Uani 1 1 d . U . . .
H61 H 0.2611 0.6350 0.6684 0.041 Uiso 1 1 calc R U . . .
C62 C 0.0825(3) 0.61856(14) 0.59532(8) 0.0327(5) Uani 1 1 d . U . . .
C63 C 0.0364(3) 0.66444(14) 0.55742(8) 0.0331(5) Uani 1 1 d . U . . .
C64 C 0.0685(3) 0.65287(17) 0.51084(9) 0.0400(6) Uani 1 1 d . U . . .
H64 H 0.1163 0.6157 0.5020 0.048 Uiso 1 1 calc R U . . .
C65 C 0.0305(3) 0.6959(2) 0.47743(10) 0.0483(7) Uani 1 1 d . U . . .
H65 H 0.0538 0.6879 0.4466 0.058 Uiso 1 1 calc R U . . .
C66 C -0.0417(3) 0.7505(2) 0.48955(11) 0.0522(7) Uani 1 1 d . U . . .
H66 H -0.0653 0.7802 0.4673 0.063 Uiso 1 1 calc R U . . .
C67 C -0.0786(3) 0.76078(19) 0.53506(12) 0.0513(7) Uani 1 1 d . U . . .
H67 H -0.1293 0.7968 0.5432 0.062 Uiso 1 1 calc R U . . .
C68 C -0.0408(3) 0.71775(16) 0.56896(10) 0.0409(6) Uani 1 1 d . U . . .
H68 H -0.0674 0.7247 0.5994 0.049 Uiso 1 1 calc R U . . .
C69 C -0.0398(3) 0.54621(15) 0.59833(9) 0.0347(5) Uani 1 1 d . U . . .
C70 C -0.0348(3) 0.50771(17) 0.63753(10) 0.0444(6) Uani 1 1 d . U . . .
H70 H 0.0410 0.5274 0.6624 0.053 Uiso 1 1 calc R U . . .
C71 C -0.1403(3) 0.44073(18) 0.64020(11) 0.0494(7) Uani 1 1 d . U . . .
H71 H -0.1347 0.4160 0.6667 0.059 Uiso 1 1 calc R U . . .
C72 C -0.2545(3) 0.41021(17) 0.60355(11) 0.0471(6) Uani 1 1 d . U . . .
H72 H -0.3255 0.3652 0.6053 0.056 Uiso 1 1 calc R U . . .
C73 C -0.2607(3) 0.44798(16) 0.56441(10) 0.0437(6) Uani 1 1 d . U . . .
H73 H -0.3364 0.4280 0.5395 0.052 Uiso 1 1 calc R U . . .
C74 C -0.1560(3) 0.51492(15) 0.56189(9) 0.0373(5) Uani 1 1 d . U . . .
H74 H -0.1627 0.5397 0.5354 0.045 Uiso 1 1 calc R U . . .
C75 C 0.2183(3) 0.59506(15) 0.58282(8) 0.0347(5) Uani 1 1 d . U . . .
C76 C 0.2216(3) 0.51847(17) 0.57148(9) 0.0420(6) Uani 1 1 d . U . . .
H76 H 0.1396 0.4782 0.5714 0.050 Uiso 1 1 calc R U . . .
C77 C 0.3479(4) 0.5012(2) 0.56010(11) 0.0526(7) Uani 1 1 d . U . . .
H77 H 0.3489 0.4494 0.5526 0.063 Uiso 1 1 calc R U . . .
C78 C 0.4697(4) 0.5595(2) 0.55987(11) 0.0551(8) Uani 1 1 d . U . . .
H78 H 0.5532 0.5476 0.5523 0.066 Uiso 1 1 calc R U . . .
C79 C 0.4675(3) 0.6368(2) 0.57105(10) 0.0481(7) Uani 1 1 d . U . . .
H79 H 0.5499 0.6767 0.5710 0.058 Uiso 1 1 calc R U . . .
C80 C 0.3430(3) 0.65436(17) 0.58229(9) 0.0403(6) Uani 1 1 d . U . . .
H80 H 0.3424 0.7062 0.5896 0.048 Uiso 1 1 calc R U . . .
C81 C 0.4403(2) 0.77462(14) 0.83753(8) 0.0315(5) Uani 1 1 d . U . . .
H81 H 0.4503 0.8182 0.8606 0.038 Uiso 1 1 calc R U . . .
C82 C 0.5911(2) 0.73433(14) 0.89557(8) 0.0293(5) Uani 1 1 d . U . . .
C83 C 0.4171(3) 0.78497(16) 0.94371(9) 0.0363(5) Uani 1 1 d . U . . .
H83 H 0.3441 0.7429 0.9271 0.044 Uiso 1 1 calc R U . . .
C84 C 0.3848(3) 0.83857(17) 0.97770(9) 0.0420(6) Uani 1 1 d . U . . .
H84 H 0.2905 0.8320 0.9836 0.050 Uiso 1 1 calc R U . . .
C85 C 0.4917(3) 0.90153(17) 1.00285(9) 0.0435(6) Uani 1 1 d . U . . .
H85 H 0.4697 0.9376 1.0254 0.052 Uiso 1 1 calc R U . . .
C86 C 0.6314(3) 0.91047(16) 0.99430(10) 0.0449(6) Uani 1 1 d . U . . .
H86 H 0.7041 0.9522 1.0115 0.054 Uiso 1 1 calc R U . . .
C87 C 0.6642(3) 0.85722(15) 0.96001(9) 0.0371(5) Uani 1 1 d . U . . .
H87 H 0.7588 0.8644 0.9543 0.044 Uiso 1 1 calc R U . . .
C88 C 0.7509(2) 0.75709(13) 0.88939(8) 0.0290(5) Uani 1 1 d . U . . .
C89 C 0.7989(3) 0.78637(15) 0.84950(9) 0.0348(5) Uani 1 1 d . U . . .
H89 H 0.7335 0.7943 0.8259 0.042 Uiso 1 1 calc R U . . .
C90 C 0.9438(3) 0.80402(16) 0.84446(10) 0.0413(6) Uani 1 1 d . U . . .
H90 H 0.9740 0.8226 0.8172 0.050 Uiso 1 1 calc R U . . .
C91 C 1.0434(3) 0.79422(16) 0.87947(11) 0.0420(6) Uani 1 1 d . U . . .
H91 H 1.1403 0.8068 0.8761 0.050 Uiso 1 1 calc R U . . .
C92 C 0.9968(3) 0.76552(16) 0.91949(10) 0.0419(6) Uani 1 1 d . U . . .
H92 H 1.0628 0.7588 0.9433 0.050 Uiso 1 1 calc R U . . .
C93 C 0.8524(3) 0.74672(15) 0.92433(9) 0.0366(5) Uani 1 1 d . U . . .
H93 H 0.8224 0.7269 0.9513 0.044 Uiso 1 1 calc R U . . .
C94 C 0.5567(3) 0.65086(14) 0.90804(9) 0.0334(5) Uani 1 1 d . U . . .
C95 C 0.4943(3) 0.62860(16) 0.94740(9) 0.0397(6) Uani 1 1 d . U . . .
H95 H 0.4729 0.6656 0.9694 0.048 Uiso 1 1 calc R U . . .
C96 C 0.4631(3) 0.55113(18) 0.95439(11) 0.0504(7) Uani 1 1 d . U . . .
H96 H 0.4192 0.5369 0.9807 0.061 Uiso 1 1 calc R U . . .
C97 C 0.4964(4) 0.49548(18) 0.92301(12) 0.0531(7) Uani 1 1 d . U . . .
H97 H 0.4733 0.4438 0.9277 0.064 Uiso 1 1 calc R U . . .
C98 C 0.5645(4) 0.51691(17) 0.88439(11) 0.0500(7) Uani 1 1 d . U . . .
H98 H 0.5905 0.4801 0.8635 0.060 Uiso 1 1 calc R U . . .
C99 C 0.5934(3) 0.59380(16) 0.87721(10) 0.0429(6) Uani 1 1 d . U . . .
H99 H 0.6385 0.6079 0.8511 0.052 Uiso 1 1 calc R U . . .
C100 C 0.5585(2) 0.79348(14) 0.93415(8) 0.0294(5) Uani 1 1 d . U . . .
C11A C 0.3651(8) 0.3810(5) 0.7140(3) 0.084(2) Uiso 0.6 1 d D . P A 1
H11A H 0.3767 0.3401 0.7318 0.100 Uiso 0.6 1 calc R U P A 1
H11B H 0.4594 0.4149 0.7129 0.100 Uiso 0.6 1 calc R U P A 1
C13A C 0.0978(16) 0.3153(8) 0.6851(5) 0.103(4) Uiso 0.4 1 d D . P B 2
H13A H 0.0040 0.3088 0.6675 0.123 Uiso 0.4 1 calc R U P B 2
H13B H 0.1005 0.2683 0.6980 0.123 Uiso 0.4 1 calc R U P B 2
C11B C 0.3344(16) 0.4131(9) 0.6766(5) 0.116(5) Uiso 0.4 1 d D . P B 2
H11C H 0.4227 0.4013 0.6876 0.139 Uiso 0.4 1 calc R U P B 2
H11D H 0.3522 0.4482 0.6534 0.139 Uiso 0.4 1 calc R U P B 2
C13B C 0.1362(9) 0.3393(5) 0.6684(3) 0.0745(18) Uiso 0.6 1 d D . P A 1
H13C H 0.0810 0.2852 0.6646 0.089 Uiso 0.6 1 calc R U P A 1
H13D H 0.0949 0.3642 0.6446 0.089 Uiso 0.6 1 calc R U P A 1
C1A C 0.2153(17) 0.3403(9) 0.6569(6) 0.105(2) Uiso 0.4 1 d D . P B 2
H1AA H 0.1727 0.3472 0.6260 0.126 Uiso 0.4 1 calc R U P B 2
H1AB H 0.2587 0.2977 0.6509 0.126 Uiso 0.4 1 calc R U P B 2
C104 C 0.1425(5) 0.3835(3) 0.72070(17) 0.0816(12) Uani 1 1 d D . . . .
H10C H 0.1586 0.3678 0.7516 0.098 Uiso 0.4 1 calc R U P B 2
H10D H 0.0644 0.4078 0.7215 0.098 Uiso 0.4 1 calc R U P B 2
H10A H 0.0824 0.4189 0.7204 0.098 Uiso 0.6 1 calc R U P B 1
H10B H 0.1081 0.3464 0.7416 0.098 Uiso 0.6 1 calc R U P B 1
C105 C 0.7654(7) 0.5757(6) 0.7494(3) 0.147(3) Uani 1 1 d D U . . .
H10E H 0.7948 0.5293 0.7392 0.176 Uiso 1 1 calc R U . . .
H10F H 0.7956 0.5934 0.7835 0.176 Uiso 1 1 calc R U . . .
C106 C 0.8206(7) 0.6449(4) 0.7175(2) 0.127(2) Uani 1 1 d D U . . .
H10G H 0.8114 0.6946 0.7328 0.153 Uiso 1 1 calc R U . . .
H10H H 0.9195 0.6505 0.7124 0.153 Uiso 1 1 calc R U . . .
C107 C 0.7228(8) 0.6159(6) 0.6724(3) 0.158(2) Uani 1 1 d D U . . .
H10I H 0.7151 0.6578 0.6550 0.189 Uiso 1 1 calc R U . . .
H10J H 0.7518 0.5767 0.6520 0.189 Uiso 1 1 calc R U . . .
C108 C 0.5948(9) 0.5839(6) 0.6901(3) 0.158(2) Uani 1 1 d D U . . .
H10K H 0.5402 0.5370 0.6684 0.189 Uiso 1 1 calc R U . . .
H10L H 0.5376 0.6208 0.6913 0.189 Uiso 1 1 calc R U . . .
C109 C 0.1413(6) 0.4878(3) 0.84219(19) 0.0901(13) Uani 1 1 d . U . . .
H10M H 0.2347 0.4832 0.8545 0.108 Uiso 1 1 calc R U . . .
H10N H 0.0857 0.4379 0.8237 0.108 Uiso 1 1 calc R U . . .
C110 C 0.0682(8) 0.5113(4) 0.8809(2) 0.1070(18) Uani 1 1 d . U . . .
H11E H -0.0044 0.4669 0.8870 0.128 Uiso 1 1 calc R U . . .
H11F H 0.1357 0.5328 0.9099 0.128 Uiso 1 1 calc R U . . .
C111 C 0.0026(8) 0.5694(4) 0.8664(3) 0.120(2) Uani 1 1 d D U . . .
H11G H -0.0179 0.6022 0.8932 0.143 Uiso 0.5 1 calc R U P C 1
H11H H -0.0826 0.5475 0.8429 0.143 Uiso 0.5 1 calc R U P C 1
H11I H 0.0098 0.6101 0.8933 0.143 Uiso 0.5 1 calc R U P D 2
H11J H -0.0979 0.5460 0.8538 0.143 Uiso 0.5 1 calc R U P D 2
C12A C 0.1336(12) 0.6102(6) 0.8446(4) 0.090(3) Uiso 0.5 1 d D . P B 1
H12A H 0.1133 0.6495 0.8269 0.108 Uiso 0.5 1 calc R U P B 1
H12B H 0.2158 0.6341 0.8690 0.108 Uiso 0.5 1 calc R U P B 1
C12B C 0.0910(11) 0.6046(6) 0.8250(4) 0.083(3) Uiso 0.5 1 d D . P B 2
H12C H 0.0275 0.6098 0.7978 0.099 Uiso 0.5 1 calc R U P B 2
H12D H 0.1604 0.6544 0.8373 0.099 Uiso 0.5 1 calc R U P B 2
N1 N 0.8148(2) 0.22762(11) 0.75170(7) 0.0303(4) Uani 1 1 d . U . . .
N2 N 0.6672(2) 0.13058(12) 0.66177(7) 0.0306(4) Uani 1 1 d . U . . .
N3 N 0.9936(2) 0.23176(11) 0.84130(7) 0.0308(4) Uani 1 1 d . U . . .
N4 N 0.3403(2) 0.71082(13) 0.75406(7) 0.0342(4) Uani 1 1 d . U . . .
N5 N 0.1089(2) 0.67237(12) 0.64186(7) 0.0330(4) Uani 1 1 d . U . . .
N6 N 0.5046(2) 0.72376(12) 0.84780(7) 0.0320(4) Uani 1 1 d . U . . .
O1 O 0.7954(4) -0.07475(15) 0.70928(10) 0.0807(8) Uani 1 1 d . U . . .
O2 O 1.1000(3) 0.07996(19) 0.72856(12) 0.0807(8) Uani 1 1 d . U . . .
O3 O 0.6474(3) 0.03519(13) 0.80315(8) 0.0548(5) Uani 1 1 d . U . . .
O4 O 0.6221(4) 0.5655(2) 0.73683(14) 0.0964(10) Uani 1 1 d D U . . .
O5B O 0.2724(7) 0.4426(4) 0.7146(3) 0.0693(17) Uiso 0.4 1 d D . P B 2
O6 O 0.1557(4) 0.54675(18) 0.81367(14) 0.0932(10) Uani 1 1 d D U . . .
K1 K 0.83481(7) 0.08121(4) 0.74148(2) 0.04672(18) Uani 1 1 d . U . . .
K2 K 0.39674(8) 0.58004(4) 0.77818(2) 0.05306(19) Uani 1 1 d . U . . .
O5A O 0.2808(5) 0.4239(3) 0.73676(18) 0.0693(11) Uiso 0.6 1 d D . P A 1
C1B C 0.2921(10) 0.3463(7) 0.6647(3) 0.105(2) Uiso 0.6 1 d D . P A 1
H1BA H 0.3072 0.2956 0.6549 0.126 Uiso 0.6 1 calc R U P A 1
H1BB H 0.3265 0.3800 0.6420 0.126 Uiso 0.6 1 calc R U P A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.363(3) . ?
C1 C2 1.403(4) . ?
C1 C5 1.445(3) . ?
C2 C3 1.386(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.415(3) . ?
C3 H3 0.9300 . ?
C4 N1 1.353(3) . ?
C4 C25 1.451(3) . ?
C5 N2 1.273(3) . ?
C5 H5 0.9300 . ?
C6 N2 1.490(3) . ?
C6 C7 1.534(3) . ?
C6 C13 1.544(3) . ?
C6 C19 1.550(3) . ?
C7 C12 1.385(4) . ?
C7 C8 1.403(4) . ?
C8 C9 1.386(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.381(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.377(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.402(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.383(4) . ?
C13 C18 1.397(4) . ?
C14 C15 1.386(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.386(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.374(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.395(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C24 1.387(4) . ?
C19 C20 1.395(4) . ?
C20 C21 1.392(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.385(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.384(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.394(4) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 N3 1.278(3) . ?
C25 H25 0.9300 . ?
C26 N3 1.486(3) . ?
C26 C27 1.536(3) . ?
C26 C33 1.540(3) . ?
C26 C39 1.548(3) . ?
C27 C32 1.386(4) . ?
C27 C28 1.408(4) . ?
C28 C29 1.383(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.383(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.389(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.390(4) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.385(3) . ?
C33 C38 1.398(4) . ?
C34 C35 1.395(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.377(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.379(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.388(4) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C44 1.384(4) . ?
C39 C40 1.397(4) . ?
C40 C41 1.387(4) . ?
C40 H40 0.9300 . ?
C41 C42 1.389(4) . ?
C41 H41 0.9300 . ?
C42 C43 1.369(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.398(4) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 O1 1.422(5) . ?
C45 C46 1.477(7) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.456(7) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.487(7) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 O1 1.436(6) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 O2 1.412(6) . ?
C49 C50 1.471(7) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 C51 1.482(9) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.532(8) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 O2 1.421(6) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 O3 1.433(4) . ?
C53 C54 1.471(5) . ?
C53 K1 3.384(3) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.452(5) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.499(5) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 O3 1.423(4) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 N4 1.362(3) . ?
C57 C58 1.402(4) . ?
C57 C61 1.447(3) . ?
C58 C59 1.386(3) . ?
C58 H58 0.9300 . ?
C59 C60 1.412(4) . ?
C59 H59 0.9300 . ?
C60 N4 1.366(3) . ?
C60 C81 1.446(3) . ?
C60 K2 3.496(3) . ?
C61 N5 1.282(3) . ?
C61 H61 0.9300 . ?
C62 N5 1.489(3) . ?
C62 C69 1.541(4) . ?
C62 C63 1.543(3) . ?
C62 C75 1.547(3) . ?
C63 C68 1.389(4) . ?
C63 C64 1.392(4) . ?
C64 C65 1.385(4) . ?
C64 H64 0.9300 . ?
C65 C66 1.374(5) . ?
C65 H65 0.9300 . ?
C66 C67 1.379(5) . ?
C66 H66 0.9300 . ?
C67 C68 1.394(4) . ?
C67 H67 0.9300 . ?
C68 H68 0.9300 . ?
C69 C70 1.393(4) . ?
C69 C74 1.398(4) . ?
C70 C71 1.385(4) . ?
C70 H70 0.9300 . ?
C71 C72 1.389(4) . ?
C71 H71 0.9300 . ?
C72 C73 1.384(4) . ?
C72 H72 0.9300 . ?
C73 C74 1.379(4) . ?
C73 H73 0.9300 . ?
C74 H74 0.9300 . ?
C75 C76 1.382(4) . ?
C75 C80 1.398(4) . ?
C76 C77 1.401(4) . ?
C76 H76 0.9300 . ?
C77 C78 1.368(5) . ?
C77 H77 0.9300 . ?
C78 C79 1.390(5) . ?
C78 H78 0.9300 . ?
C79 C80 1.386(4) . ?
C79 H79 0.9300 . ?
C80 H80 0.9300 . ?
C81 N6 1.283(3) . ?
C81 H81 0.9300 . ?
C82 N6 1.488(3) . ?
C82 C88 1.539(3) . ?
C82 C100 1.539(3) . ?
C82 C94 1.550(3) . ?
C83 C84 1.389(4) . ?
C83 C100 1.403(3) . ?
C83 H83 0.9300 . ?
C84 C85 1.382(4) . ?
C84 H84 0.9300 . ?
C85 C86 1.378(4) . ?
C85 H85 0.9300 . ?
C86 C87 1.393(4) . ?
C86 H86 0.9300 . ?
C87 C100 1.391(3) . ?
C87 H87 0.9300 . ?
C88 C89 1.386(3) . ?
C88 C93 1.396(3) . ?
C89 C90 1.391(4) . ?
C89 H89 0.9300 . ?
C90 C91 1.382(4) . ?
C90 H90 0.9300 . ?
C91 C92 1.381(4) . ?
C91 H91 0.9300 . ?
C92 C93 1.385(4) . ?
C92 H92 0.9300 . ?
C93 H93 0.9300 . ?
C94 C95 1.383(4) . ?
C94 C99 1.400(4) . ?
C95 C96 1.394(4) . ?
C95 H95 0.9300 . ?
C96 C97 1.374(5) . ?
C96 H96 0.9300 . ?
C97 C98 1.386(5) . ?
C97 H97 0.9300 . ?
C98 C99 1.387(4) . ?
C98 H98 0.9300 . ?
C99 K2 3.189(3) . ?
C99 H99 0.9300 . ?
C11A O5A 1.409(8) . ?
C11A C1B 1.484(10) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C13A C104 1.423(11) . ?
C13A C1A 1.474(13) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C11B O5B 1.398(12) . ?
C11B C1A 1.506(13) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C13B C1B 1.507(10) . ?
C13B C104 1.578(8) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C104 O5A 1.355(6) . ?
C104 O5B 1.470(8) . ?
C104 H10C 0.9700 . ?
C104 H10D 0.9700 . ?
C104 H10A 0.9700 . ?
C104 H10B 0.9700 . ?
C105 O4 1.364(7) . ?
C105 C106 1.649(9) . ?
C105 H10E 0.9700 . ?
C105 H10F 0.9700 . ?
C106 C107 1.465(9) . ?
C106 H10G 0.9700 . ?
C106 H10H 0.9700 . ?
C107 C108 1.403(8) . ?
C107 H10I 0.9700 . ?
C107 H10J 0.9700 . ?
C108 O4 1.429(8) . ?
C108 K2 3.306(7) . ?
C108 H10K 0.9700 . ?
C108 H10L 0.9700 . ?
C109 O6 1.407(6) . ?
C109 C110 1.442(7) . ?
C109 K2 3.441(5) . ?
C109 H10M 0.9700 . ?
C109 H10N 0.9700 . ?
C110 C111 1.442(8) . ?
C110 H11E 0.9700 . ?
C110 H11F 0.9700 . ?
C111 C12A 1.532(11) . ?
C111 C12B 1.628(11) . ?
C111 H11G 0.9700 . ?
C111 H11H 0.9700 . ?
C111 H11I 0.9700 . ?
C111 H11J 0.9700 . ?
C12A O6 1.421(10) . ?
C12A K2 3.439(9) . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
C12B O6 1.369(9) . ?
C12B K2 3.484(9) . ?
C12B H12C 0.9700 . ?
C12B H12D 0.9700 . ?
N1 K1 2.672(2) . ?
N2 K1 3.026(2) . ?
N4 K2 2.709(2) . ?
N6 K2 2.921(2) . ?
O1 K1 2.748(3) . ?
O2 K1 2.650(3) . ?
O3 K1 2.708(2) . ?
O4 K2 2.644(4) . ?
O5B K2 2.771(7) . ?
O6 K2 2.606(3) . ?
K2 O5A 2.789(5) . ?
C1B H1BA 0.9700 . ?
C1B H1BB 0.9700 . ?

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
N1 C1 C2 111.6(2) . . ?
N1 C1 C5 122.9(2) . . ?
C2 C1 C5 125.5(2) . . ?
C3 C2 C1 105.9(2) . . ?
C3 C2 H2 127.0 . . ?
C1 C2 H2 127.0 . . ?
C2 C3 C4 105.9(2) . . ?
C2 C3 H3 127.1 . . ?
C4 C3 H3 127.1 . . ?
N1 C4 C3 111.3(2) . . ?
N1 C4 C25 123.7(2) . . ?
C3 C4 C25 125.0(2) . . ?
N2 C5 C1 123.9(2) . . ?
N2 C5 H5 118.0 . . ?
C1 C5 H5 118.0 . . ?
N2 C6 C7 112.5(2) . . ?
N2 C6 C13 107.61(18) . . ?
C7 C6 C13 110.5(2) . . ?
N2 C6 C19 105.46(18) . . ?
C7 C6 C19 111.00(19) . . ?
C13 C6 C19 109.6(2) . . ?
C12 C7 C8 117.9(2) . . ?
C12 C7 C6 123.0(2) . . ?
C8 C7 C6 118.9(2) . . ?
C9 C8 C7 121.2(3) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C10 C9 C8 120.3(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C11 C10 C9 119.3(3) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 120.8(3) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C7 C12 C11 120.5(3) . . ?
C7 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C18 117.9(2) . . ?
C14 C13 C6 121.4(2) . . ?
C18 C13 C6 120.7(2) . . ?
C13 C14 C15 121.3(3) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C16 C15 C14 120.6(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 118.9(3) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C16 C17 C18 120.7(3) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C13 120.7(3) . . ?
C17 C18 H18 119.7 . . ?
C13 C18 H18 119.7 . . ?
C24 C19 C20 118.0(2) . . ?
C24 C19 C6 120.5(2) . . ?
C20 C19 C6 121.5(2) . . ?
C21 C20 C19 120.9(3) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C22 C21 C20 120.3(3) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 119.3(3) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 120.2(3) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C19 C24 C23 121.3(3) . . ?
C19 C24 H24 119.4 . . ?
C23 C24 H24 119.4 . . ?
N3 C25 C4 124.3(2) . . ?
N3 C25 H25 117.8 . . ?
C4 C25 H25 117.8 . . ?
N3 C26 C27 113.41(19) . . ?
N3 C26 C33 109.04(18) . . ?
C27 C26 C33 111.23(19) . . ?
N3 C26 C39 104.94(18) . . ?
C27 C26 C39 111.09(19) . . ?
C33 C26 C39 106.75(19) . . ?
C32 C27 C28 117.4(2) . . ?
C32 C27 C26 123.5(2) . . ?
C28 C27 C26 119.0(2) . . ?
C29 C28 C27 121.2(3) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C30 C29 C28 120.3(3) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C31 119.4(3) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
C30 C31 C32 120.1(3) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C27 C32 C31 121.5(3) . . ?
C27 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C34 C33 C38 117.8(2) . . ?
C34 C33 C26 122.0(2) . . ?
C38 C33 C26 120.3(2) . . ?
C33 C34 C35 120.6(3) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C36 C35 C34 120.9(3) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C35 C36 C37 119.2(3) . . ?
C35 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C36 C37 C38 120.1(3) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C37 C38 C33 121.3(3) . . ?
C37 C38 H38 119.3 . . ?
C33 C38 H38 119.3 . . ?
C44 C39 C40 118.5(2) . . ?
C44 C39 C26 123.8(2) . . ?
C40 C39 C26 117.5(2) . . ?
C41 C40 C39 120.6(3) . . ?
C41 C40 H40 119.7 . . ?
C39 C40 H40 119.7 . . ?
C40 C41 C42 120.3(3) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C43 C42 C41 119.6(3) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C42 C43 C44 120.5(3) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C39 C44 C43 120.6(3) . . ?
C39 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
O1 C45 C46 106.5(4) . . ?
O1 C45 H45A 110.4 . . ?
C46 C45 H45A 110.4 . . ?
O1 C45 H45B 110.4 . . ?
C46 C45 H45B 110.4 . . ?
H45A C45 H45B 108.6 . . ?
C47 C46 C45 105.6(4) . . ?
C47 C46 H46A 110.6 . . ?
C45 C46 H46A 110.6 . . ?
C47 C46 H46B 110.6 . . ?
C45 C46 H46B 110.6 . . ?
H46A C46 H46B 108.7 . . ?
C46 C47 C48 104.4(4) . . ?
C46 C47 H47A 110.9 . . ?
C48 C47 H47A 110.9 . . ?
C46 C47 H47B 110.9 . . ?
C48 C47 H47B 110.9 . . ?
H47A C47 H47B 108.9 . . ?
O1 C48 C47 109.2(4) . . ?
O1 C48 H48A 109.8 . . ?
C47 C48 H48A 109.8 . . ?
O1 C48 H48B 109.8 . . ?
C47 C48 H48B 109.8 . . ?
H48A C48 H48B 108.3 . . ?
O2 C49 C50 105.2(5) . . ?
O2 C49 H49A 110.7 . . ?
C50 C49 H49A 110.7 . . ?
O2 C49 H49B 110.7 . . ?
C50 C49 H49B 110.7 . . ?
H49A C49 H49B 108.8 . . ?
C49 C50 C51 102.8(5) . . ?
C49 C50 H50A 111.2 . . ?
C51 C50 H50A 111.2 . . ?
C49 C50 H50B 111.2 . . ?
C51 C50 H50B 111.2 . . ?
H50A C50 H50B 109.1 . . ?
C50 C51 C52 104.7(5) . . ?
C50 C51 H51A 110.8 . . ?
C52 C51 H51A 110.8 . . ?
C50 C51 H51B 110.8 . . ?
C52 C51 H51B 110.8 . . ?
H51A C51 H51B 108.9 . . ?
O2 C52 C51 104.0(5) . . ?
O2 C52 H52A 111.0 . . ?
C51 C52 H52A 111.0 . . ?
O2 C52 H52B 111.0 . . ?
C51 C52 H52B 111.0 . . ?
H52A C52 H52B 109.0 . . ?
O3 C53 C54 106.9(3) . . ?
O3 C53 K1 50.48(14) . . ?
C54 C53 K1 149.8(3) . . ?
O3 C53 H53A 110.3 . . ?
C54 C53 H53A 110.3 . . ?
K1 C53 H53A 97.6 . . ?
O3 C53 H53B 110.3 . . ?
C54 C53 H53B 110.3 . . ?
K1 C53 H53B 69.1 . . ?
H53A C53 H53B 108.6 . . ?
C55 C54 C53 107.6(3) . . ?
C55 C54 H54A 110.2 . . ?
C53 C54 H54A 110.2 . . ?
C55 C54 H54B 110.2 . . ?
C53 C54 H54B 110.2 . . ?
H54A C54 H54B 108.5 . . ?
C54 C55 C56 103.8(3) . . ?
C54 C55 H55A 111.0 . . ?
C56 C55 H55A 111.0 . . ?
C54 C55 H55B 111.0 . . ?
C56 C55 H55B 111.0 . . ?
H55A C55 H55B 109.0 . . ?
O3 C56 C55 106.4(3) . . ?
O3 C56 H56A 110.4 . . ?
C55 C56 H56A 110.4 . . ?
O3 C56 H56B 110.4 . . ?
C55 C56 H56B 110.4 . . ?
H56A C56 H56B 108.6 . . ?
N4 C57 C58 111.7(2) . . ?
N4 C57 C61 118.2(2) . . ?
C58 C57 C61 130.1(2) . . ?
C59 C58 C57 106.0(2) . . ?
C59 C58 H58 127.0 . . ?
C57 C58 H58 127.0 . . ?
C58 C59 C60 106.2(2) . . ?
C58 C59 H59 126.9 . . ?
C60 C59 H59 126.9 . . ?
N4 C60 C59 110.9(2) . . ?
N4 C60 C81 123.6(2) . . ?
C59 C60 C81 125.4(2) . . ?
N4 C60 K2 45.04(12) . . ?
C59 C60 K2 147.18(17) . . ?
C81 C60 K2 81.41(15) . . ?
N5 C61 C57 122.8(2) . . ?
N5 C61 H61 118.6 . . ?
C57 C61 H61 118.6 . . ?
N5 C62 C69 107.72(19) . . ?
N5 C62 C63 105.30(19) . . ?
C69 C62 C63 110.96(19) . . ?
N5 C62 C75 112.54(19) . . ?
C69 C62 C75 110.9(2) . . ?
C63 C62 C75 109.2(2) . . ?
C68 C63 C64 118.3(2) . . ?
C68 C63 C62 120.4(2) . . ?
C64 C63 C62 121.3(2) . . ?
C65 C64 C63 120.9(3) . . ?
C65 C64 H64 119.5 . . ?
C63 C64 H64 119.5 . . ?
C66 C65 C64 120.5(3) . . ?
C66 C65 H65 119.8 . . ?
C64 C65 H65 119.8 . . ?
C65 C66 C67 119.3(3) . . ?
C65 C66 H66 120.4 . . ?
C67 C66 H66 120.4 . . ?
C66 C67 C68 120.7(3) . . ?
C66 C67 H67 119.7 . . ?
C68 C67 H67 119.7 . . ?
C63 C68 C67 120.2(3) . . ?
C63 C68 H68 119.9 . . ?
C67 C68 H68 119.9 . . ?
C70 C69 C74 117.5(2) . . ?
C70 C69 C62 120.1(2) . . ?
C74 C69 C62 122.4(2) . . ?
C71 C70 C69 121.3(3) . . ?
C71 C70 H70 119.4 . . ?
C69 C70 H70 119.4 . . ?
C70 C71 C72 120.5(3) . . ?
C70 C71 H71 119.8 . . ?
C72 C71 H71 119.8 . . ?
C73 C72 C71 118.8(3) . . ?
C73 C72 H72 120.6 . . ?
C71 C72 H72 120.6 . . ?
C74 C73 C72 120.7(3) . . ?
C74 C73 H73 119.6 . . ?
C72 C73 H73 119.6 . . ?
C73 C74 C69 121.3(3) . . ?
C73 C74 H74 119.4 . . ?
C69 C74 H74 119.4 . . ?
C76 C75 C80 118.5(2) . . ?
C76 C75 C62 123.2(2) . . ?
C80 C75 C62 118.2(2) . . ?
C75 C76 C77 120.4(3) . . ?
C75 C76 H76 119.8 . . ?
C77 C76 H76 119.8 . . ?
C78 C77 C76 120.8(3) . . ?
C78 C77 H77 119.6 . . ?
C76 C77 H77 119.6 . . ?
C77 C78 C79 119.4(3) . . ?
C77 C78 H78 120.3 . . ?
C79 C78 H78 120.3 . . ?
C80 C79 C78 120.2(3) . . ?
C80 C79 H79 119.9 . . ?
C78 C79 H79 119.9 . . ?
C79 C80 C75 120.8(3) . . ?
C79 C80 H80 119.6 . . ?
C75 C80 H80 119.6 . . ?
N6 C81 C60 123.9(2) . . ?
N6 C81 H81 118.1 . . ?
C60 C81 H81 118.1 . . ?
N6 C82 C88 108.39(18) . . ?
N6 C82 C100 114.20(19) . . ?
C88 C82 C100 111.14(18) . . ?
N6 C82 C94 103.44(18) . . ?
C88 C82 C94 106.50(19) . . ?
C100 C82 C94 112.61(19) . . ?
C84 C83 C100 120.9(2) . . ?
C84 C83 H83 119.5 . . ?
C100 C83 H83 119.5 . . ?
C85 C84 C83 120.4(3) . . ?
C85 C84 H84 119.8 . . ?
C83 C84 H84 119.8 . . ?
C86 C85 C84 119.5(3) . . ?
C86 C85 H85 120.3 . . ?
C84 C85 H85 120.3 . . ?
C85 C86 C87 120.3(3) . . ?
C85 C86 H86 119.9 . . ?
C87 C86 H86 119.9 . . ?
C100 C87 C86 121.3(2) . . ?
C100 C87 H87 119.3 . . ?
C86 C87 H87 119.3 . . ?
C89 C88 C93 118.1(2) . . ?
C89 C88 C82 122.3(2) . . ?
C93 C88 C82 119.7(2) . . ?
C88 C89 C90 120.6(2) . . ?
C88 C89 H89 119.7 . . ?
C90 C89 H89 119.7 . . ?
C91 C90 C89 120.8(2) . . ?
C91 C90 H90 119.6 . . ?
C89 C90 H90 119.6 . . ?
C92 C91 C90 119.0(2) . . ?
C92 C91 H91 120.5 . . ?
C90 C91 H91 120.5 . . ?
C91 C92 C93 120.4(2) . . ?
C91 C92 H92 119.8 . . ?
C93 C92 H92 119.8 . . ?
C92 C93 C88 121.1(2) . . ?
C92 C93 H93 119.5 . . ?
C88 C93 H93 119.5 . . ?
C95 C94 C99 117.5(2) . . ?
C95 C94 C82 125.2(2) . . ?
C99 C94 C82 117.2(2) . . ?
C94 C95 C96 120.6(3) . . ?
C94 C95 H95 119.7 . . ?
C96 C95 H95 119.7 . . ?
C97 C96 C95 121.0(3) . . ?
C97 C96 H96 119.5 . . ?
C95 C96 H96 119.5 . . ?
C96 C97 C98 119.5(3) . . ?
C96 C97 H97 120.2 . . ?
C98 C97 H97 120.2 . . ?
C97 C98 C99 119.2(3) . . ?
C97 C98 H98 120.4 . . ?
C99 C98 H98 120.4 . . ?
C98 C99 C94 122.0(3) . . ?
C98 C99 K2 102.41(19) . . ?
C94 C99 K2 103.88(17) . . ?
C98 C99 H99 119.0 . . ?
C94 C99 H99 119.0 . . ?
K2 C99 H99 62.0 . . ?
C87 C100 C83 117.5(2) . . ?
C87 C100 C82 122.5(2) . . ?
C83 C100 C82 120.0(2) . . ?
O5A C11A C1B 108.5(7) . . ?
O5A C11A H11A 110.0 . . ?
C1B C11A H11A 110.0 . . ?
O5A C11A H11B 110.0 . . ?
C1B C11A H11B 110.0 . . ?
H11A C11A H11B 108.4 . . ?
C104 C13A C1A 94.9(10) . . ?
C104 C13A H13A 112.7 . . ?
C1A C13A H13A 112.7 . . ?
C104 C13A H13B 112.7 . . ?
C1A C13A H13B 112.7 . . ?
H13A C13A H13B 110.2 . . ?
O5B C11B C1A 98.9(11) . . ?
O5B C11B H11C 112.0 . . ?
C1A C11B H11C 112.0 . . ?
O5B C11B H11D 112.0 . . ?
C1A C11B H11D 112.0 . . ?
H11C C11B H11D 109.7 . . ?
C1B C13B C104 102.4(6) . . ?
C1B C13B H13C 111.3 . . ?
C104 C13B H13C 111.3 . . ?
C1B C13B H13D 111.3 . . ?
C104 C13B H13D 111.3 . . ?
H13C C13B H13D 109.2 . . ?
C13A C1A C11B 119.2(12) . . ?
C13A C1A H1AA 107.5 . . ?
C11B C1A H1AA 107.5 . . ?
C13A C1A H1AB 107.5 . . ?
C11B C1A H1AB 107.5 . . ?
H1AA C1A H1AB 107.0 . . ?
C13A C104 O5B 116.3(7) . . ?
O5A C104 C13B 108.0(5) . . ?
C13A C104 H10C 108.2 . . ?
O5B C104 H10C 108.2 . . ?
C13A C104 H10D 108.2 . . ?
O5B C104 H10D 108.2 . . ?
H10C C104 H10D 107.4 . . ?
O5A C104 H10A 110.1 . . ?
C13B C104 H10A 110.1 . . ?
O5A C104 H10B 110.1 . . ?
C13B C104 H10B 110.1 . . ?
H10A C104 H10B 108.4 . . ?
O4 C105 C106 96.4(5) . . ?
O4 C105 H10E 112.5 . . ?
C106 C105 H10E 112.5 . . ?
O4 C105 H10F 112.5 . . ?
C106 C105 H10F 112.5 . . ?
H10E C105 H10F 110.0 . . ?
C107 C106 C105 102.2(5) . . ?
C107 C106 H10G 111.3 . . ?
C105 C106 H10G 111.3 . . ?
C107 C106 H10H 111.3 . . ?
C105 C106 H10H 111.3 . . ?
H10G C106 H10H 109.2 . . ?
C108 C107 C106 100.2(6) . . ?
C108 C107 H10I 111.7 . . ?
C106 C107 H10I 111.7 . . ?
C108 C107 H10J 111.7 . . ?
C106 C107 H10J 111.7 . . ?
H10I C107 H10J 109.5 . . ?
C107 C108 O4 111.5(7) . . ?
C107 C108 K2 149.4(7) . . ?
O4 C108 K2 50.7(3) . . ?
C107 C108 H10K 109.3 . . ?
O4 C108 H10K 109.3 . . ?
K2 C108 H10K 100.7 . . ?
C107 C108 H10L 109.3 . . ?
O4 C108 H10L 109.3 . . ?
K2 C108 H10L 64.9 . . ?
H10K C108 H10L 108.0 . . ?
O6 C109 C110 105.6(4) . . ?
O6 C109 K2 43.5(2) . . ?
C110 C109 K2 136.1(4) . . ?
O6 C109 H10M 110.6 . . ?
C110 C109 H10M 110.6 . . ?
K2 C109 H10M 70.2 . . ?
O6 C109 H10N 110.6 . . ?
C110 C109 H10N 110.6 . . ?
K2 C109 H10N 110.1 . . ?
H10M C109 H10N 108.7 . . ?
C111 C110 C109 107.2(5) . . ?
C111 C110 H11E 110.3 . . ?
C109 C110 H11E 110.3 . . ?
C111 C110 H11F 110.3 . . ?
C109 C110 H11F 110.3 . . ?
H11E C110 H11F 108.5 . . ?
C110 C111 C12A 93.3(7) . . ?
C110 C111 C12B 105.6(6) . . ?
C110 C111 H11G 113.1 . . ?
C12A C111 H11G 113.1 . . ?
C110 C111 H11H 113.1 . . ?
C12A C111 H11H 113.1 . . ?
H11G C111 H11H 110.4 . . ?
C110 C111 H11I 110.6 . . ?
C12B C111 H11I 110.6 . . ?
C110 C111 H11J 110.6 . . ?
C12B C111 H11J 110.6 . . ?
H11I C111 H11J 108.7 . . ?
O6 C12A C111 101.4(7) . . ?
O6 C12A K2 43.8(3) . . ?
C111 C12A K2 144.1(6) . . ?
O6 C12A H12A 111.5 . . ?
C111 C12A H12A 111.5 . . ?
K2 C12A H12A 93.4 . . ?
O6 C12A H12B 111.5 . . ?
C111 C12A H12B 111.5 . . ?
K2 C12A H12B 81.9 . . ?
H12A C12A H12B 109.3 . . ?
O6 C12B C111 99.1(6) . . ?
O6 C12B K2 40.8(3) . . ?
C111 C12B K2 134.3(5) . . ?
O6 C12B H12C 112.0 . . ?
C111 C12B H12C 112.0 . . ?
K2 C12B H12C 105.1 . . ?
O6 C12B H12D 112.0 . . ?
C111 C12B H12D 112.0 . . ?
K2 C12B H12D 77.9 . . ?
H12C C12B H12D 109.6 . . ?
C4 N1 C1 105.3(2) . . ?
C4 N1 K1 133.10(15) . . ?
C1 N1 K1 120.41(15) . . ?
C5 N2 C6 121.7(2) . . ?
C5 N2 K1 110.97(15) . . ?
C6 N2 K1 126.49(14) . . ?
C25 N3 C26 119.9(2) . . ?
C57 N4 C60 105.2(2) . . ?
C57 N4 K2 132.16(16) . . ?
C60 N4 K2 114.07(14) . . ?
C61 N5 C62 119.6(2) . . ?
C81 N6 C82 120.5(2) . . ?
C81 N6 K2 110.49(15) . . ?
C82 N6 K2 127.18(15) . . ?
C45 O1 C48 104.5(3) . . ?
C45 O1 K1 120.5(2) . . ?
C48 O1 K1 129.2(3) . . ?
C49 O2 C52 111.1(4) . . ?
C49 O2 K1 125.3(3) . . ?
C52 O2 K1 120.4(3) . . ?
C56 O3 C53 108.7(2) . . ?
C56 O3 K1 135.5(2) . . ?
C53 O3 K1 105.43(17) . . ?
C105 O4 C108 110.5(5) . . ?
C105 O4 K2 138.7(4) . . ?
C108 O4 K2 104.6(4) . . ?
C11B O5B C104 109.4(8) . . ?
C11B O5B K2 125.4(7) . . ?
C104 O5B K2 124.5(4) . . ?
C12B O6 C109 118.0(5) . . ?
C109 O6 C12A 103.2(6) . . ?
C12B O6 K2 119.1(4) . . ?
C109 O6 K2 114.7(3) . . ?
C12A O6 K2 114.0(4) . . ?
O2 K1 N1 109.59(9) . . ?
O2 K1 O3 138.16(10) . . ?
N1 K1 O3 94.94(7) . . ?
O2 K1 O1 79.31(10) . . ?
N1 K1 O1 163.58(9) . . ?
O3 K1 O1 86.30(8) . . ?
O2 K1 N2 115.50(9) . . ?
N1 K1 N2 60.94(6) . . ?
O3 K1 N2 105.93(7) . . ?
O1 K1 N2 102.95(8) . . ?
O2 K1 C53 137.20(10) . . ?
N1 K1 C53 73.25(7) . . ?
O3 K1 C53 24.09(7) . . ?
O1 K1 C53 110.08(9) . . ?
N2 K1 C53 103.21(7) . . ?
O6 K2 O4 161.94(11) . . ?
O6 K2 N4 89.62(9) . . ?
O4 K2 N4 105.79(9) . . ?
O6 K2 O5B 84.35(16) . . ?
O4 K2 O5B 80.36(17) . . ?
N4 K2 O5B 116.66(17) . . ?
O6 K2 O5A 78.90(12) . . ?
O4 K2 O5A 83.84(13) . . ?
N4 K2 O5A 130.71(12) . . ?
O6 K2 N6 90.98(9) . . ?
O4 K2 N6 104.38(10) . . ?
N4 K2 N6 62.34(6) . . ?
O5B K2 N6 175.26(15) . . ?
O5A K2 N6 162.73(12) . . ?
O6 K2 C99 94.85(11) . . ?
O4 K2 C99 86.14(10) . . ?
N4 K2 C99 118.44(7) . . ?
O5B K2 C99 124.89(17) . . ?
O5A K2 C99 110.27(12) . . ?
N6 K2 C99 56.23(6) . . ?
O6 K2 C108 153.93(19) . . ?
O4 K2 C108 24.73(16) . . ?
N4 K2 C108 87.07(17) . . ?
O5B K2 C108 74.2(2) . . ?
O5A K2 C108 83.8(2) . . ?
N6 K2 C108 110.12(19) . . ?
C99 K2 C108 109.43(16) . . ?
O6 K2 C12A 22.17(18) . . ?
O4 K2 C12A 172.8(2) . . ?
N4 K2 C12A 75.1(2) . . ?
O5A K2 C12A 101.1(2) . . ?
N6 K2 C12A 69.51(18) . . ?
C99 K2 C12A 87.2(2) . . ?
C108 K2 C12A 160.1(3) . . ?
O6 K2 C109 21.82(12) . . ?
O4 K2 C109 143.12(12) . . ?
N4 K2 C109 110.84(10) . . ?
O5B K2 C109 79.71(17) . . ?
O5A K2 C109 69.32(13) . . ?
N6 K2 C109 96.24(10) . . ?
C99 K2 C109 80.33(11) . . ?
C108 K2 C109 153.1(2) . . ?
C12A K2 C109 37.6(2) . . ?
O6 K2 C12B 20.08(16) . . ?
O4 K2 C12B 175.61(19) . . ?
N4 K2 C12B 70.67(16) . . ?
O5B K2 C12B 98.8(2) . . ?
N6 K2 C12B 76.49(19) . . ?
C99 K2 C12B 97.8(2) . . ?
C108 K2 C12B 150.9(2) . . ?
C109 K2 C12B 40.19(18) . . ?
O6 K2 C60 83.33(8) . . ?
O4 K2 C60 114.38(9) . . ?
N4 K2 C60 20.89(6) . . ?
O5B K2 C60 135.18(17) . . ?
O5A K2 C60 146.72(11) . . ?
N6 K2 C60 42.96(5) . . ?
C99 K2 C60 99.02(6) . . ?
C108 K2 C60 101.48(18) . . ?
C12A K2 C60 64.02(18) . . ?
C109 K2 C60 101.60(10) . . ?
C12B K2 C60 63.25(16) . . ?
C104 O5A C11A 105.9(5) . . ?
C104 O5A K2 129.8(3) . . ?
C11A O5A K2 121.1(4) . . ?
C11A C1B C13B 103.6(7) . . ?
C11A C1B H1BA 111.0 . . ?
C13B C1B H1BA 111.0 . . ?
C11A C1B H1BB 111.0 . . ?
C13B C1B H1BB 111.0 . . ?
H1BA C1B H1BB 109.0 . . ?

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
N1 C1 C2 C3 -0.9(3) . . . . ?
C5 C1 C2 C3 179.2(2) . . . . ?
C1 C2 C3 C4 0.9(3) . . . . ?
C2 C3 C4 N1 -0.6(3) . . . . ?
C2 C3 C4 C25 179.7(2) . . . . ?
N1 C1 C5 N2 11.4(4) . . . . ?
C2 C1 C5 N2 -168.7(2) . . . . ?
N2 C6 C7 C12 102.9(3) . . . . ?
C13 C6 C7 C12 -136.8(2) . . . . ?
C19 C6 C7 C12 -15.1(3) . . . . ?
N2 C6 C7 C8 -72.5(3) . . . . ?
C13 C6 C7 C8 47.9(3) . . . . ?
C19 C6 C7 C8 169.6(2) . . . . ?
C12 C7 C8 C9 -0.9(4) . . . . ?
C6 C7 C8 C9 174.6(3) . . . . ?
C7 C8 C9 C10 1.0(5) . . . . ?
C8 C9 C10 C11 -0.6(5) . . . . ?
C9 C10 C11 C12 0.2(5) . . . . ?
C8 C7 C12 C11 0.5(4) . . . . ?
C6 C7 C12 C11 -174.9(3) . . . . ?
C10 C11 C12 C7 -0.1(5) . . . . ?
N2 C6 C13 C14 -20.1(3) . . . . ?
C7 C6 C13 C14 -143.3(2) . . . . ?
C19 C6 C13 C14 94.1(3) . . . . ?
N2 C6 C13 C18 161.2(2) . . . . ?
C7 C6 C13 C18 38.0(3) . . . . ?
C19 C6 C13 C18 -84.6(3) . . . . ?
C18 C13 C14 C15 1.2(4) . . . . ?
C6 C13 C14 C15 -177.6(3) . . . . ?
C13 C14 C15 C16 0.1(5) . . . . ?
C14 C15 C16 C17 -0.6(5) . . . . ?
C15 C16 C17 C18 -0.1(5) . . . . ?
C16 C17 C18 C13 1.4(5) . . . . ?
C14 C13 C18 C17 -1.9(4) . . . . ?
C6 C13 C18 C17 176.8(3) . . . . ?
N2 C6 C19 C24 -23.4(3) . . . . ?
C7 C6 C19 C24 98.7(3) . . . . ?
C13 C6 C19 C24 -139.0(2) . . . . ?
N2 C6 C19 C20 157.6(2) . . . . ?
C7 C6 C19 C20 -80.3(3) . . . . ?
C13 C6 C19 C20 42.0(3) . . . . ?
C24 C19 C20 C21 0.6(4) . . . . ?
C6 C19 C20 C21 179.6(2) . . . . ?
C19 C20 C21 C22 0.3(4) . . . . ?
C20 C21 C22 C23 -0.7(5) . . . . ?
C21 C22 C23 C24 0.3(5) . . . . ?
C20 C19 C24 C23 -1.1(4) . . . . ?
C6 C19 C24 C23 179.9(3) . . . . ?
C22 C23 C24 C19 0.6(5) . . . . ?
N1 C4 C25 N3 0.4(4) . . . . ?
C3 C4 C25 N3 180.0(2) . . . . ?
N3 C26 C27 C32 -124.5(2) . . . . ?
C33 C26 C27 C32 -1.1(3) . . . . ?
C39 C26 C27 C32 117.6(3) . . . . ?
N3 C26 C27 C28 54.5(3) . . . . ?
C33 C26 C27 C28 177.8(2) . . . . ?
C39 C26 C27 C28 -63.4(3) . . . . ?
C32 C27 C28 C29 1.0(4) . . . . ?
C26 C27 C28 C29 -178.0(2) . . . . ?
C27 C28 C29 C30 -0.3(4) . . . . ?
C28 C29 C30 C31 -1.5(4) . . . . ?
C29 C30 C31 C32 2.4(5) . . . . ?
C28 C27 C32 C31 0.0(4) . . . . ?
C26 C27 C32 C31 178.9(2) . . . . ?
C30 C31 C32 C27 -1.7(5) . . . . ?
N3 C26 C33 C34 21.9(3) . . . . ?
C27 C26 C33 C34 -103.9(3) . . . . ?
C39 C26 C33 C34 134.8(2) . . . . ?
N3 C26 C33 C38 -157.9(2) . . . . ?
C27 C26 C33 C38 76.3(3) . . . . ?
C39 C26 C33 C38 -45.0(3) . . . . ?
C38 C33 C34 C35 1.6(4) . . . . ?
C26 C33 C34 C35 -178.2(2) . . . . ?
C33 C34 C35 C36 -2.0(4) . . . . ?
C34 C35 C36 C37 0.7(5) . . . . ?
C35 C36 C37 C38 0.9(5) . . . . ?
C36 C37 C38 C33 -1.3(4) . . . . ?
C34 C33 C38 C37 0.0(4) . . . . ?
C26 C33 C38 C37 179.8(2) . . . . ?
N3 C26 C39 C44 -133.1(2) . . . . ?
C27 C26 C39 C44 -10.2(3) . . . . ?
C33 C26 C39 C44 111.2(3) . . . . ?
N3 C26 C39 C40 50.0(3) . . . . ?
C27 C26 C39 C40 172.9(2) . . . . ?
C33 C26 C39 C40 -65.7(3) . . . . ?
C44 C39 C40 C41 0.2(4) . . . . ?
C26 C39 C40 C41 177.2(3) . . . . ?
C39 C40 C41 C42 0.5(5) . . . . ?
C40 C41 C42 C43 -0.5(5) . . . . ?
C41 C42 C43 C44 -0.2(5) . . . . ?
C40 C39 C44 C43 -0.9(4) . . . . ?
C26 C39 C44 C43 -177.7(2) . . . . ?
C42 C43 C44 C39 0.9(4) . . . . ?
O1 C45 C46 C47 -29.9(5) . . . . ?
C45 C46 C47 C48 16.2(6) . . . . ?
C46 C47 C48 O1 2.6(6) . . . . ?
O2 C49 C50 C51 -34.7(6) . . . . ?
C49 C50 C51 C52 31.4(6) . . . . ?
C50 C51 C52 O2 -17.0(6) . . . . ?
O3 C53 C54 C55 -10.8(5) . . . . ?
K1 C53 C54 C55 -47.5(8) . . . . ?
C53 C54 C55 C56 22.3(6) . . . . ?
C54 C55 C56 O3 -26.0(5) . . . . ?
N4 C57 C58 C59 0.6(3) . . . . ?
C61 C57 C58 C59 -177.1(3) . . . . ?
C57 C58 C59 C60 -1.1(3) . . . . ?
C58 C59 C60 N4 1.2(3) . . . . ?
C58 C59 C60 C81 -175.1(2) . . . . ?
C58 C59 C60 K2 -35.3(4) . . . . ?
N4 C57 C61 N5 174.1(2) . . . . ?
C58 C57 C61 N5 -8.3(4) . . . . ?
N5 C62 C63 C68 -32.8(3) . . . . ?
C69 C62 C63 C68 83.5(3) . . . . ?
C75 C62 C63 C68 -153.9(2) . . . . ?
N5 C62 C63 C64 148.3(2) . . . . ?
C69 C62 C63 C64 -95.4(3) . . . . ?
C75 C62 C63 C64 27.2(3) . . . . ?
C68 C63 C64 C65 3.0(4) . . . . ?
C62 C63 C64 C65 -178.1(3) . . . . ?
C63 C64 C65 C66 -0.8(5) . . . . ?
C64 C65 C66 C67 -1.4(5) . . . . ?
C65 C66 C67 C68 1.4(5) . . . . ?
C64 C63 C68 C67 -2.9(4) . . . . ?
C62 C63 C68 C67 178.1(3) . . . . ?
C66 C67 C68 C63 0.8(5) . . . . ?
N5 C62 C69 C70 -49.5(3) . . . . ?
C63 C62 C69 C70 -164.2(2) . . . . ?
C75 C62 C69 C70 74.1(3) . . . . ?
N5 C62 C69 C74 133.0(2) . . . . ?
C63 C62 C69 C74 18.2(3) . . . . ?
C75 C62 C69 C74 -103.4(3) . . . . ?
C74 C69 C70 C71 0.3(4) . . . . ?
C62 C69 C70 C71 -177.4(3) . . . . ?
C69 C70 C71 C72 0.0(5) . . . . ?
C70 C71 C72 C73 0.0(5) . . . . ?
C71 C72 C73 C74 -0.3(4) . . . . ?
C72 C73 C74 C69 0.7(4) . . . . ?
C70 C69 C74 C73 -0.7(4) . . . . ?
C62 C69 C74 C73 176.9(2) . . . . ?
N5 C62 C75 C76 126.6(2) . . . . ?
C69 C62 C75 C76 5.8(3) . . . . ?
C63 C62 C75 C76 -116.9(3) . . . . ?
N5 C62 C75 C80 -54.4(3) . . . . ?
C69 C62 C75 C80 -175.2(2) . . . . ?
C63 C62 C75 C80 62.2(3) . . . . ?
C80 C75 C76 C77 0.5(4) . . . . ?
C62 C75 C76 C77 179.5(2) . . . . ?
C75 C76 C77 C78 -0.2(4) . . . . ?
C76 C77 C78 C79 -0.1(4) . . . . ?
C77 C78 C79 C80 0.0(4) . . . . ?
C78 C79 C80 C75 0.3(4) . . . . ?
C76 C75 C80 C79 -0.5(4) . . . . ?
C62 C75 C80 C79 -179.6(2) . . . . ?
N4 C60 C81 N6 -5.9(4) . . . . ?
C59 C60 C81 N6 170.0(2) . . . . ?
K2 C60 C81 N6 10.7(2) . . . . ?
C100 C83 C84 C85 0.0(4) . . . . ?
C83 C84 C85 C86 -0.6(4) . . . . ?
C84 C85 C86 C87 1.1(4) . . . . ?
C85 C86 C87 C100 -1.0(4) . . . . ?
N6 C82 C88 C89 18.7(3) . . . . ?
C100 C82 C88 C89 -107.6(2) . . . . ?
C94 C82 C88 C89 129.5(2) . . . . ?
N6 C82 C88 C93 -159.9(2) . . . . ?
C100 C82 C88 C93 73.8(3) . . . . ?
C94 C82 C88 C93 -49.1(3) . . . . ?
C93 C88 C89 C90 0.7(4) . . . . ?
C82 C88 C89 C90 -178.0(2) . . . . ?
C88 C89 C90 C91 -1.3(4) . . . . ?
C89 C90 C91 C92 0.9(4) . . . . ?
C90 C91 C92 C93 0.1(4) . . . . ?
C91 C92 C93 C88 -0.8(4) . . . . ?
C89 C88 C93 C92 0.4(4) . . . . ?
C82 C88 C93 C92 179.0(2) . . . . ?
N6 C82 C94 C95 -119.5(3) . . . . ?
C88 C82 C94 C95 126.3(2) . . . . ?
C100 C82 C94 C95 4.2(3) . . . . ?
N6 C82 C94 C99 61.3(3) . . . . ?
C88 C82 C94 C99 -52.9(3) . . . . ?
C100 C82 C94 C99 -174.9(2) . . . . ?
C99 C94 C95 C96 -3.1(4) . . . . ?
C82 C94 C95 C96 177.7(2) . . . . ?
C94 C95 C96 C97 1.4(5) . . . . ?
C95 C96 C97 C98 1.3(5) . . . . ?
C96 C97 C98 C99 -2.2(5) . . . . ?
C97 C98 C99 C94 0.4(5) . . . . ?
C97 C98 C99 K2 -114.8(3) . . . . ?
C95 C94 C99 C98 2.2(4) . . . . ?
C82 C94 C99 C98 -178.5(3) . . . . ?
C95 C94 C99 K2 116.8(2) . . . . ?
C82 C94 C99 K2 -64.0(2) . . . . ?
C86 C87 C100 C83 0.3(4) . . . . ?
C86 C87 C100 C82 179.1(2) . . . . ?
C84 C83 C100 C87 0.2(4) . . . . ?
C84 C83 C100 C82 -178.7(2) . . . . ?
N6 C82 C100 C87 -124.6(2) . . . . ?
C88 C82 C100 C87 -1.6(3) . . . . ?
C94 C82 C100 C87 117.8(2) . . . . ?
N6 C82 C100 C83 54.2(3) . . . . ?
C88 C82 C100 C83 177.2(2) . . . . ?
C94 C82 C100 C83 -63.4(3) . . . . ?
C104 C13A C1A C11B 8(2) . . . . ?
O5B C11B C1A C13A -12(2) . . . . ?
C1A C13A C104 O5B -0.3(14) . . . . ?
C1B C13B C104 O5A 13.4(8) . . . . ?
O4 C105 C106 C107 -42.5(7) . . . . ?
C105 C106 C107 C108 38.5(9) . . . . ?
C106 C107 C108 O4 -22.6(11) . . . . ?
C106 C107 C108 K2 25.2(16) . . . . ?
O6 C109 C110 C111 17.6(7) . . . . ?
K2 C109 C110 C111 54.8(8) . . . . ?
C109 C110 C111 C12A -41.6(7) . . . . ?
C109 C110 C111 C12B -21.7(8) . . . . ?
C110 C111 C12A O6 52.4(8) . . . . ?
C110 C111 C12A K2 40.2(13) . . . . ?
C110 C111 C12B O6 17.3(9) . . . . ?
C110 C111 C12B K2 -6.4(11) . . . . ?
C3 C4 N1 C1 0.1(3) . . . . ?
C25 C4 N1 C1 179.7(2) . . . . ?
C3 C4 N1 K1 -167.01(17) . . . . ?
C25 C4 N1 K1 12.7(4) . . . . ?
C2 C1 N1 C4 0.5(3) . . . . ?
C5 C1 N1 C4 -179.5(2) . . . . ?
C2 C1 N1 K1 169.60(16) . . . . ?
C5 C1 N1 K1 -10.5(3) . . . . ?
C1 C5 N2 C6 -175.7(2) . . . . ?
C1 C5 N2 K1 -5.7(3) . . . . ?
C7 C6 N2 C5 -1.8(3) . . . . ?
C13 C6 N2 C5 -123.8(2) . . . . ?
C19 C6 N2 C5 119.3(2) . . . . ?
C7 C6 N2 K1 -170.21(14) . . . . ?
C13 C6 N2 K1 67.8(2) . . . . ?
C19 C6 N2 K1 -49.1(2) . . . . ?
C4 C25 N3 C26 -178.2(2) . . . . ?
C27 C26 N3 C25 21.3(3) . . . . ?
C33 C26 N3 C25 -103.2(2) . . . . ?
C39 C26 N3 C25 142.8(2) . . . . ?
C58 C57 N4 C60 0.1(3) . . . . ?
C61 C57 N4 C60 178.1(2) . . . . ?
C58 C57 N4 K2 144.78(18) . . . . ?
C61 C57 N4 K2 -37.2(3) . . . . ?
C59 C60 N4 C57 -0.9(3) . . . . ?
C81 C60 N4 C57 175.6(2) . . . . ?
K2 C60 N4 C57 152.0(2) . . . . ?
C59 C60 N4 K2 -152.83(16) . . . . ?
C81 C60 N4 K2 23.6(3) . . . . ?
C57 C61 N5 C62 179.0(2) . . . . ?
C69 C62 N5 C61 95.6(3) . . . . ?
C63 C62 N5 C61 -145.9(2) . . . . ?
C75 C62 N5 C61 -27.0(3) . . . . ?
C60 C81 N6 C82 -179.3(2) . . . . ?
C60 C81 N6 K2 -13.6(3) . . . . ?
C88 C82 N6 C81 -106.6(2) . . . . ?
C100 C82 N6 C81 17.9(3) . . . . ?
C94 C82 N6 C81 140.6(2) . . . . ?
C88 C82 N6 K2 90.2(2) . . . . ?
C100 C82 N6 K2 -145.37(15) . . . . ?
C94 C82 N6 K2 -22.6(2) . . . . ?
C46 C45 O1 C48 31.0(5) . . . . ?
C46 C45 O1 K1 -124.5(3) . . . . ?
C47 C48 O1 C45 -20.9(6) . . . . ?
C47 C48 O1 K1 131.6(4) . . . . ?
C50 C49 O2 C52 25.2(6) . . . . ?
C50 C49 O2 K1 -134.4(4) . . . . ?
C51 C52 O2 C49 -5.0(6) . . . . ?
C51 C52 O2 K1 155.8(4) . . . . ?
C55 C56 O3 C53 20.1(4) . . . . ?
C55 C56 O3 K1 158.2(3) . . . . ?
C54 C53 O3 C56 -6.1(4) . . . . ?
K1 C53 O3 C56 150.9(3) . . . . ?
C54 C53 O3 K1 -157.1(3) . . . . ?
C106 C105 O4 C108 29.1(7) . . . . ?
C106 C105 O4 K2 -117.4(5) . . . . ?
C107 C108 O4 C105 -7.0(11) . . . . ?
K2 C108 O4 C105 -157.9(6) . . . . ?
C107 C108 O4 K2 150.9(7) . . . . ?
C1A C11B O5B C104 9.9(14) . . . . ?
C1A C11B O5B K2 -179.5(9) . . . . ?
C13A C104 O5B C11B -7.0(13) . . . . ?
C13A C104 O5B K2 -177.7(8) . . . . ?
C111 C12B O6 C109 -7.1(9) . . . . ?
K2 C12B O6 C109 146.8(8) . . . . ?
C111 C12B O6 K2 -153.9(4) . . . . ?
C110 C109 O6 C12B -5.8(8) . . . . ?
K2 C109 O6 C12B -148.2(8) . . . . ?
C110 C109 O6 C12A 17.9(7) . . . . ?
K2 C109 O6 C12A -124.6(6) . . . . ?
C110 C109 O6 K2 142.5(4) . . . . ?
C111 C12A O6 C109 -44.7(8) . . . . ?
K2 C12A O6 C109 125.0(5) . . . . ?
C111 C12A O6 K2 -169.7(5) . . . . ?
C13B C104 O5A C11A -29.9(7) . . . . ?
C13B C104 O5A K2 129.7(5) . . . . ?
C1B C11A O5A C104 36.0(8) . . . . ?
C1B C11A O5A K2 -125.8(6) . . . . ?
O5A C11A C1B C13B -26.1(10) . . . . ?
C104 C13B C1B C11A 7.5(9) . . . . ?

_refine_diff_density_max         1.316
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.072



