# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_wo6ck
_database_code_depnum_ccdc_archive 'CCDC 2089028'
loop_
_audit_author_name
_audit_author_address
'Christian Kleeberg'
;Technische Universitaet Braunschweig, Institut fuer Anorganische und Analytische Chemie
Germany
;
_audit_update_record             
;
2021-06-09 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H66 B4 Li2 N6 O6'
_chemical_formula_sum            'C38 H66 B4 Li2 N6 O6'
_chemical_formula_weight         760.08

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'
B B 0.0090 0.0039 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   12.5438(4)
_cell_length_b                   19.8952(6)
_cell_length_c                   17.7349(6)
_cell_angle_alpha                90
_cell_angle_beta                 106.128(3)
_cell_angle_gamma                90
_cell_volume                     4251.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16107
_cell_measurement_theta_min      3.39
_cell_measurement_theta_max      75.90


_exptl_crystal_recrystallization_method 
;
 From a solution in TMEDA/THF layered with n-pentane at -40deg C.
;

_exptl_special_details           
;
 The crystal was mounted at rt with perfluoroether oil on top of a human hair
 and placed in a cold nitrogen gas stream on the diffractometer.

 The collected data cover more than a hemisphere of the reciprocal space.
 A combination of 32 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 1.2 deg in ω.
 Each frame was exposured for 3 s (low 2θ angles) or 15 s (high 2θ angles).
 Nominal crystal to detector distance 53 mm.
;

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7337
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;




_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            68449
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.415
_diffrn_reflns_theta_max         76.098
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8841
_reflns_number_gt                6865
_reflns_threshold_expression     'I > 2σ(I)'


_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;



_computing_data_collection       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution    
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_molecular_graphics    
;
 K. Brandenburg, 2016, Diamond 4.2.2, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;



_refine_special_details          
;
 NH hydrogen atoms were refined freely. All other H atoms were placed in 
 idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond but not tip.


 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;



_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0657P)²+1.1748P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8841
_refine_ls_number_parameters     525
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1366
_refine_ls_wR_factor_gt          0.1255
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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 0.54390(14) 0.54605(8) 0.77395(9) 0.0271(3) Uani 1 1 d . . . . .
C2 C 0.65940(14) 0.54255(9) 0.79330(9) 0.0309(3) Uani 1 1 d . . . . .
H2 H 0.7029 0.5824 0.8003 0.037 Uiso 1 1 calc R U . . .
C3 C 0.71008(15) 0.47919(10) 0.80219(10) 0.0337(4) Uani 1 1 d . . . . .
H3 H 0.7886 0.4763 0.8142 0.040 Uiso 1 1 calc R U . . .
C4 C 0.64776(16) 0.42035(10) 0.79386(11) 0.0366(4) Uani 1 1 d . . . . .
H4 H 0.6843 0.3780 0.8000 0.044 Uiso 1 1 calc R U . . .
C5 C 0.53247(16) 0.42274(9) 0.77660(10) 0.0346(4) Uani 1 1 d . . . . .
H5 H 0.4898 0.3827 0.7717 0.042 Uiso 1 1 calc R U . . .
C6 C 0.48170(14) 0.48576(9) 0.76673(9) 0.0294(3) Uani 1 1 d . . . . .
C7 C 0.09246(14) 0.63707(10) 0.60491(10) 0.0329(4) Uani 1 1 d . . . . .
C8 C 0.06263(14) 0.58455(9) 0.66135(10) 0.0329(4) Uani 1 1 d . . . . .
C9 C 0.06879(16) 0.61316(11) 0.51995(11) 0.0431(5) Uani 1 1 d . . . . .
H9A H 0.0912 0.6481 0.4885 0.065 Uiso 1 1 calc R U . . .
H9B H -0.0107 0.6041 0.4988 0.065 Uiso 1 1 calc R U . . .
H9C H 0.1108 0.5719 0.5182 0.065 Uiso 1 1 calc R U . . .
C10 C 0.03540(15) 0.70482(10) 0.60537(11) 0.0368(4) Uani 1 1 d . . . . .
H10A H 0.0493 0.7207 0.6596 0.055 Uiso 1 1 calc R U . . .
H10B H -0.0447 0.6998 0.5818 0.055 Uiso 1 1 calc R U . . .
H10C H 0.0649 0.7375 0.5750 0.055 Uiso 1 1 calc R U . . .
C11 C 0.08574(16) 0.51231(10) 0.64117(12) 0.0406(4) Uani 1 1 d . . . . .
H11A H 0.1610 0.5093 0.6353 0.061 Uiso 1 1 calc R U . . .
H11B H 0.0319 0.4991 0.5919 0.061 Uiso 1 1 calc R U . . .
H11C H 0.0791 0.4822 0.6834 0.061 Uiso 1 1 calc R U . . .
C12 C -0.05659(14) 0.59011(10) 0.66629(12) 0.0403(4) Uani 1 1 d . . . . .
H12A H -0.0708 0.5545 0.7005 0.060 Uiso 1 1 calc R U . . .
H12B H -0.1079 0.5852 0.6137 0.060 Uiso 1 1 calc R U . . .
H12C H -0.0676 0.6341 0.6879 0.060 Uiso 1 1 calc R U . . .
C13 C 0.21873(13) 0.73687(8) 0.80943(9) 0.0265(3) Uani 1 1 d . . . . .
C14 C 0.11051(14) 0.73542(9) 0.81679(10) 0.0302(3) Uani 1 1 d . . . . .
H14 H 0.0607 0.7007 0.7924 0.036 Uiso 1 1 calc R U . . .
C15 C 0.07639(14) 0.78536(9) 0.86021(11) 0.0339(4) Uani 1 1 d . . . . .
H15 H 0.0035 0.7837 0.8663 0.041 Uiso 1 1 calc R U . . .
C16 C 0.14686(16) 0.83759(10) 0.89485(12) 0.0384(4) Uani 1 1 d . . . . .
H16 H 0.1214 0.8713 0.9236 0.046 Uiso 1 1 calc R U . . .
C17 C 0.25457(15) 0.84060(9) 0.88757(11) 0.0350(4) Uani 1 1 d . . . . .
H17 H 0.3028 0.8764 0.9107 0.042 Uiso 1 1 calc R U . . .
C18 C 0.28993(13) 0.79032(8) 0.84593(10) 0.0279(3) Uani 1 1 d . . . . .
C19 C 0.57349(14) 0.71558(9) 0.65347(10) 0.0309(4) Uani 1 1 d . . . . .
C20 C 0.64244(14) 0.73970(9) 0.73591(11) 0.0319(4) Uani 1 1 d . . . . .
C21 C 0.55434(17) 0.76925(11) 0.58945(12) 0.0415(4) Uani 1 1 d . . . . .
H21A H 0.5107 0.7501 0.5395 0.062 Uiso 1 1 calc R U . . .
H21B H 0.6260 0.7849 0.5842 0.062 Uiso 1 1 calc R U . . .
H21C H 0.5140 0.8072 0.6036 0.062 Uiso 1 1 calc R U . . .
C22 C 0.62319(15) 0.65351(9) 0.62494(10) 0.0347(4) Uani 1 1 d . . . . .
H22A H 0.6395 0.6192 0.6663 0.052 Uiso 1 1 calc R U . . .
H22B H 0.6919 0.6661 0.6124 0.052 Uiso 1 1 calc R U . . .
H22C H 0.5700 0.6355 0.5779 0.052 Uiso 1 1 calc R U . . .
C23 C 0.76805(14) 0.73342(10) 0.75010(12) 0.0382(4) Uani 1 1 d . . . . .
H23A H 0.8060 0.7535 0.8009 0.057 Uiso 1 1 calc R U . . .
H23B H 0.7903 0.7570 0.7083 0.057 Uiso 1 1 calc R U . . .
H23C H 0.7883 0.6858 0.7501 0.057 Uiso 1 1 calc R U . . .
C24 C 0.61283(15) 0.81220(10) 0.75289(12) 0.0386(4) Uani 1 1 d . . . . .
H24A H 0.5320 0.8171 0.7391 0.058 Uiso 1 1 calc R U . . .
H24B H 0.6432 0.8436 0.7216 0.058 Uiso 1 1 calc R U . . .
H24C H 0.6445 0.8221 0.8088 0.058 Uiso 1 1 calc R U . . .
C25 C 0.3456(2) 0.61089(11) 0.43604(11) 0.0471(5) Uani 1 1 d . . . . .
H25A H 0.4214 0.6121 0.4294 0.057 Uiso 1 1 calc R U . . .
H25B H 0.3033 0.6499 0.4084 0.057 Uiso 1 1 calc R U . . .
C26 C 0.2879(3) 0.54562(12) 0.40439(12) 0.0593(7) Uani 1 1 d . . . . .
H26A H 0.3209 0.5256 0.3649 0.071 Uiso 1 1 calc R U . . .
H26B H 0.2077 0.5530 0.3800 0.071 Uiso 1 1 calc R U . . .
C27 C 0.3067(2) 0.50065(11) 0.47610(12) 0.0461(5) Uani 1 1 d . . . . .
H27A H 0.2350 0.4858 0.4837 0.055 Uiso 1 1 calc R U . . .
H27B H 0.3505 0.4605 0.4706 0.055 Uiso 1 1 calc R U . . .
C28 C 0.36957(18) 0.54360(10) 0.54378(11) 0.0410(4) Uani 1 1 d . . . . .
H28A H 0.3424 0.5358 0.5904 0.049 Uiso 1 1 calc R U . . .
H28B H 0.4499 0.5332 0.5577 0.049 Uiso 1 1 calc R U . . .
C29 C 0.23220(19) 0.79551(11) 0.47341(11) 0.0446(5) Uani 1 1 d . . . . .
H29A H 0.1622 0.7739 0.4433 0.054 Uiso 1 1 calc R U . . .
H29B H 0.2877 0.7908 0.4435 0.054 Uiso 1 1 calc R U . . .
C30 C 0.21292(18) 0.86920(11) 0.48805(13) 0.0444(5) Uani 1 1 d . . . . .
H30A H 0.1498 0.8877 0.4465 0.053 Uiso 1 1 calc R U . . .
H30B H 0.2800 0.8964 0.4910 0.053 Uiso 1 1 calc R U . . .
C31 C 0.18684(17) 0.86680(10) 0.56723(12) 0.0415(4) Uani 1 1 d . . . . .
H31A H 0.2013 0.9106 0.5946 0.050 Uiso 1 1 calc R U . . .
H31B H 0.1089 0.8534 0.5612 0.050 Uiso 1 1 calc R U . . .
C32 C 0.26717(16) 0.81352(10) 0.60994(11) 0.0376(4) Uani 1 1 d . . . . .
H32A H 0.3412 0.8332 0.6343 0.045 Uiso 1 1 calc R U . . .
H32B H 0.2399 0.7920 0.6514 0.045 Uiso 1 1 calc R U . . .
C33 C 0.14543(18) 0.56713(11) 0.98589(12) 0.0449(5) Uani 1 1 d . . . . .
H33A H 0.1163 0.5323 1.0148 0.054 Uiso 1 1 calc R U . . .
H33B H 0.1392 0.6112 1.0103 0.054 Uiso 1 1 calc R U . . .
C34 C 0.26610(17) 0.55273(10) 0.99311(11) 0.0415(4) Uani 1 1 d . . . . .
H34A H 0.3090 0.5544 1.0491 0.050 Uiso 1 1 calc R U . . .
H34B H 0.2732 0.5069 0.9734 0.050 Uiso 1 1 calc R U . . .
C35 C -0.03004(18) 0.60023(12) 0.89683(15) 0.0506(5) Uani 1 1 d . . . . .
H35A H -0.0738 0.6012 0.8417 0.076 Uiso 1 1 calc R U . . .
H35B H -0.0180 0.6463 0.9170 0.076 Uiso 1 1 calc R U . . .
H35C H -0.0701 0.5746 0.9275 0.076 Uiso 1 1 calc R U . . .
C36 C 0.05961(17) 0.49961(11) 0.87125(13) 0.0445(5) Uani 1 1 d . . . . .
H36A H 0.0252 0.4722 0.9040 0.067 Uiso 1 1 calc R U . . .
H36B H 0.1310 0.4798 0.8709 0.067 Uiso 1 1 calc R U . . .
H36C H 0.0106 0.5012 0.8176 0.067 Uiso 1 1 calc R U . . .
C37 C 0.33290(17) 0.66667(10) 0.98968(11) 0.0413(4) Uani 1 1 d . . . . .
H37A H 0.2619 0.6868 0.9904 0.062 Uiso 1 1 calc R U . . .
H37B H 0.3716 0.6968 0.9624 0.062 Uiso 1 1 calc R U . . .
H37C H 0.3787 0.6597 1.0437 0.062 Uiso 1 1 calc R U . . .
C38 C 0.41901(16) 0.57524(11) 0.94125(11) 0.0424(4) Uani 1 1 d . . . . .
H38A H 0.4689 0.5669 0.9937 0.064 Uiso 1 1 calc R U . . .
H38B H 0.4529 0.6082 0.9138 0.064 Uiso 1 1 calc R U . . .
H38C H 0.4061 0.5331 0.9114 0.064 Uiso 1 1 calc R U . . .
Li1 Li 0.3285(2) 0.67862(16) 0.59468(17) 0.0332(6) Uani 1 1 d . . . . .
Li2 Li 0.1835(3) 0.61394(17) 0.84543(18) 0.0370(7) Uani 1 1 d . . . . .
B1 B 0.35931(15) 0.57563(10) 0.74444(10) 0.0268(4) Uani 1 1 d . . . . .
B2 B 0.24385(15) 0.62801(10) 0.72296(11) 0.0267(4) Uani 1 1 d . . . . .
B3 B 0.39149(15) 0.71729(10) 0.78970(10) 0.0264(4) Uani 1 1 d . . . . .
B4 B 0.49122(15) 0.67760(10) 0.75441(10) 0.0266(4) Uani 1 1 d . . . . .
N1 N 0.47148(11) 0.60073(7) 0.76055(8) 0.0262(3) Uani 1 1 d . . . . .
N2 N 0.36995(12) 0.50305(8) 0.74887(8) 0.0296(3) Uani 1 1 d . . . . .
N3 N 0.27832(11) 0.69212(7) 0.77571(8) 0.0257(3) Uani 1 1 d . . . . .
N4 N 0.39274(12) 0.77917(7) 0.83311(8) 0.0294(3) Uani 1 1 d . . . . .
N5 N 0.07761(13) 0.56806(9) 0.90318(10) 0.0396(4) Uani 1 1 d . . . . .
N6 N 0.31253(13) 0.60161(8) 0.94847(8) 0.0341(3) Uani 1 1 d . . . . .
O1 O 0.20998(9) 0.64435(6) 0.63670(6) 0.0290(3) Uani 1 1 d . . . . .
O2 O 0.13811(9) 0.60102(6) 0.73597(7) 0.0288(2) Uani 1 1 d . . . . .
O3 O 0.46987(9) 0.69814(6) 0.66757(7) 0.0283(2) Uani 1 1 d . . . . .
O4 O 0.60959(9) 0.69532(6) 0.78821(7) 0.0289(3) Uani 1 1 d . . . . .
O5 O 0.34968(11) 0.61193(7) 0.51729(7) 0.0362(3) Uani 1 1 d . . . . .
O6 O 0.27225(11) 0.76538(7) 0.54989(7) 0.0374(3) Uani 1 1 d . . . . .
H2N H 0.323(2) 0.4725(13) 0.7404(14) 0.046(7) Uiso 1 1 d . . . . .
H4N H 0.4496(19) 0.8022(12) 0.8520(14) 0.041(6) 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
C1 C2 1.395(2) . ?
C1 N1 1.395(2) . ?
C1 C6 1.417(2) . ?
C2 C3 1.401(2) . ?
C3 C4 1.393(3) . ?
C4 C5 1.393(3) . ?
C5 C6 1.395(2) . ?
C6 N2 1.392(2) . ?
C7 O1 1.432(2) . ?
C7 C10 1.527(3) . ?
C7 C9 1.528(2) . ?
C7 C8 1.563(3) . ?
C8 O2 1.4350(19) . ?
C8 C12 1.526(2) . ?
C8 C11 1.528(2) . ?
C13 N3 1.399(2) . ?
C13 C14 1.400(2) . ?
C13 C18 1.424(2) . ?
C13 Li2 2.596(4) . ?
C14 C15 1.395(2) . ?
C14 Li2 2.584(4) . ?
C15 C16 1.392(3) . ?
C16 C17 1.394(3) . ?
C17 C18 1.387(2) . ?
C18 N4 1.388(2) . ?
C19 O3 1.433(2) . ?
C19 C21 1.528(2) . ?
C19 C22 1.531(2) . ?
C19 C20 1.554(2) . ?
C20 O4 1.422(2) . ?
C20 C23 1.530(2) . ?
C20 C24 1.540(2) . ?
C25 O5 1.428(2) . ?
C25 C26 1.516(3) . ?
C26 C27 1.519(3) . ?
C27 C28 1.506(3) . ?
C28 O5 1.437(2) . ?
C29 O6 1.440(2) . ?
C29 C30 1.520(3) . ?
C30 C31 1.528(3) . ?
C31 C32 1.513(3) . ?
C32 O6 1.447(2) . ?
C33 N5 1.477(3) . ?
C33 C34 1.511(3) . ?
C34 N6 1.472(2) . ?
C35 N5 1.470(3) . ?
C36 N5 1.468(3) . ?
C37 N6 1.473(2) . ?
C38 N6 1.473(3) . ?
Li1 O3 1.921(3) . ?
Li1 O6 1.949(3) . ?
Li1 O1 1.961(3) . ?
Li1 O5 1.979(3) . ?
Li2 O2 1.883(3) . ?
Li2 N6 2.092(3) . ?
Li2 N5 2.098(4) . ?
Li2 N3 2.486(4) . ?
Li2 B2 2.506(4) . ?
B1 N1 1.445(2) . ?
B1 N2 1.450(2) . ?
B1 B2 1.738(3) . ?
B2 O1 1.505(2) . ?
B2 O2 1.507(2) . ?
B2 N3 1.570(2) . ?
B3 N4 1.450(2) . ?
B3 N3 1.460(2) . ?
B3 B4 1.737(3) . ?
B4 O4 1.481(2) . ?
B4 O3 1.543(2) . ?
B4 N1 1.558(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 131.58(16) . . ?
C2 C1 C6 119.22(16) . . ?
N1 C1 C6 109.18(14) . . ?
C1 C2 C3 118.72(17) . . ?
C4 C3 C2 121.38(16) . . ?
C3 C4 C5 120.83(17) . . ?
C4 C5 C6 117.91(17) . . ?
N2 C6 C5 130.28(17) . . ?
N2 C6 C1 107.81(15) . . ?
C5 C6 C1 121.91(16) . . ?
O1 C7 C10 109.97(14) . . ?
O1 C7 C9 108.45(14) . . ?
C10 C7 C9 108.48(15) . . ?
O1 C7 C8 102.64(13) . . ?
C10 C7 C8 113.01(15) . . ?
C9 C7 C8 114.06(16) . . ?
O2 C8 C12 109.66(15) . . ?
O2 C8 C11 108.13(14) . . ?
C12 C8 C11 109.52(15) . . ?
O2 C8 C7 102.95(13) . . ?
C12 C8 C7 113.65(15) . . ?
C11 C8 C7 112.60(16) . . ?
N3 C13 C14 132.38(15) . . ?
N3 C13 C18 109.12(14) . . ?
C14 C13 C18 118.37(15) . . ?
N3 C13 Li2 69.71(11) . . ?
C14 C13 Li2 73.87(12) . . ?
C18 C13 Li2 136.05(13) . . ?
C15 C14 C13 119.41(16) . . ?
C15 C14 Li2 134.73(15) . . ?
C13 C14 Li2 74.79(12) . . ?
C16 C15 C14 121.38(17) . . ?
C15 C16 C17 120.30(17) . . ?
C18 C17 C16 118.66(16) . . ?
C17 C18 N4 130.64(16) . . ?
C17 C18 C13 121.86(16) . . ?
N4 C18 C13 107.47(14) . . ?
O3 C19 C21 109.63(14) . . ?
O3 C19 C22 109.55(14) . . ?
C21 C19 C22 108.21(15) . . ?
O3 C19 C20 101.85(13) . . ?
C21 C19 C20 114.51(16) . . ?
C22 C19 C20 112.87(14) . . ?
O4 C20 C23 108.28(14) . . ?
O4 C20 C24 108.95(15) . . ?
C23 C20 C24 109.73(15) . . ?
O4 C20 C19 103.63(13) . . ?
C23 C20 C19 114.09(15) . . ?
C24 C20 C19 111.84(15) . . ?
O5 C25 C26 105.40(17) . . ?
C25 C26 C27 104.33(17) . . ?
C28 C27 C26 104.97(17) . . ?
O5 C28 C27 105.73(15) . . ?
O6 C29 C30 105.72(16) . . ?
C29 C30 C31 102.23(16) . . ?
C32 C31 C30 101.48(16) . . ?
O6 C32 C31 104.75(15) . . ?
N5 C33 C34 111.94(16) . . ?
N6 C34 C33 111.46(16) . . ?
O3 Li1 O6 104.91(15) . . ?
O3 Li1 O1 118.03(16) . . ?
O6 Li1 O1 103.64(15) . . ?
O3 Li1 O5 109.00(16) . . ?
O6 Li1 O5 114.47(15) . . ?
O1 Li1 O5 106.99(15) . . ?
O2 Li2 N6 145.47(19) . . ?
O2 Li2 N5 113.12(16) . . ?
N6 Li2 N5 87.91(14) . . ?
O2 Li2 N3 67.80(11) . . ?
N6 Li2 N3 98.46(13) . . ?
N5 Li2 N3 165.97(18) . . ?
O2 Li2 B2 36.82(8) . . ?
N6 Li2 B2 115.07(15) . . ?
N5 Li2 B2 148.88(17) . . ?
N3 Li2 B2 36.65(7) . . ?
O2 Li2 C14 86.32(13) . . ?
N6 Li2 C14 115.29(15) . . ?
N5 Li2 C14 105.36(14) . . ?
N3 Li2 C14 60.62(9) . . ?
B2 Li2 C14 84.32(11) . . ?
O2 Li2 C13 84.17(13) . . ?
N6 Li2 C13 100.49(13) . . ?
N5 Li2 C13 134.73(16) . . ?
N3 Li2 C13 31.86(6) . . ?
B2 Li2 C13 64.45(10) . . ?
C14 Li2 C13 31.35(7) . . ?
N1 B1 N2 105.28(14) . . ?
N1 B1 B2 122.85(15) . . ?
N2 B1 B2 131.86(15) . . ?
O1 B2 O2 102.75(12) . . ?
O1 B2 N3 112.55(14) . . ?
O2 B2 N3 107.86(13) . . ?
O1 B2 B1 109.56(13) . . ?
O2 B2 B1 117.90(14) . . ?
N3 B2 B1 106.36(12) . . ?
O1 B2 Li2 146.83(14) . . ?
O2 B2 Li2 48.48(10) . . ?
N3 B2 Li2 70.96(11) . . ?
B1 B2 Li2 100.19(12) . . ?
N4 B3 N3 104.37(14) . . ?
N4 B3 B4 132.45(15) . . ?
N3 B3 B4 123.13(14) . . ?
O4 B4 O3 102.56(13) . . ?
O4 B4 N1 111.49(14) . . ?
O3 B4 N1 110.05(13) . . ?
O4 B4 B3 119.17(14) . . ?
O3 B4 B3 107.25(13) . . ?
N1 B4 B3 106.07(13) . . ?
C1 N1 B1 108.45(14) . . ?
C1 N1 B4 131.99(14) . . ?
B1 N1 B4 119.37(14) . . ?
C6 N2 B1 109.28(14) . . ?
C13 N3 B3 108.59(13) . . ?
C13 N3 B2 132.87(14) . . ?
B3 N3 B2 118.28(13) . . ?
C13 N3 Li2 78.43(12) . . ?
B3 N3 Li2 134.98(13) . . ?
B2 N3 Li2 72.38(11) . . ?
C18 N4 B3 110.43(14) . . ?
C36 N5 C35 109.55(17) . . ?
C36 N5 C33 110.84(16) . . ?
C35 N5 C33 110.18(17) . . ?
C36 N5 Li2 105.40(16) . . ?
C35 N5 Li2 117.77(16) . . ?
C33 N5 Li2 102.83(15) . . ?
C34 N6 C38 108.37(16) . . ?
C34 N6 C37 110.70(15) . . ?
C38 N6 C37 108.63(15) . . ?
C34 N6 Li2 102.81(15) . . ?
C38 N6 Li2 117.76(14) . . ?
C37 N6 Li2 108.41(15) . . ?
C7 O1 B2 110.33(13) . . ?
C7 O1 Li1 133.77(13) . . ?
B2 O1 Li1 115.56(13) . . ?
C8 O2 B2 108.87(13) . . ?
C8 O2 Li2 156.25(15) . . ?
B2 O2 Li2 94.71(13) . . ?
C19 O3 B4 108.91(12) . . ?
C19 O3 Li1 130.07(14) . . ?
B4 O3 Li1 119.33(13) . . ?
C20 O4 B4 108.86(12) . . ?
C25 O5 C28 105.70(14) . . ?
C25 O5 Li1 137.35(15) . . ?
C28 O5 Li1 116.86(14) . . ?
C29 O6 C32 110.05(14) . . ?
C29 O6 Li1 138.15(15) . . ?
C32 O6 Li1 111.79(14) . . ?

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 -179.09(16) . . . . ?
C6 C1 C2 C3 2.3(2) . . . . ?
C1 C2 C3 C4 -1.5(3) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C3 C4 C5 C6 1.0(3) . . . . ?
C4 C5 C6 N2 179.44(17) . . . . ?
C4 C5 C6 C1 -0.1(3) . . . . ?
C2 C1 C6 N2 178.79(14) . . . . ?
N1 C1 C6 N2 -0.10(18) . . . . ?
C2 C1 C6 C5 -1.6(2) . . . . ?
N1 C1 C6 C5 179.55(15) . . . . ?
O1 C7 C8 O2 35.04(16) . . . . ?
C10 C7 C8 O2 -83.35(16) . . . . ?
C9 C7 C8 O2 152.12(14) . . . . ?
O1 C7 C8 C12 153.56(14) . . . . ?
C10 C7 C8 C12 35.2(2) . . . . ?
C9 C7 C8 C12 -89.35(19) . . . . ?
O1 C7 C8 C11 -81.16(16) . . . . ?
C10 C7 C8 C11 160.45(14) . . . . ?
C9 C7 C8 C11 35.9(2) . . . . ?
N3 C13 C14 C15 174.33(17) . . . . ?
C18 C13 C14 C15 -0.9(2) . . . . ?
Li2 C13 C14 C15 133.15(18) . . . . ?
N3 C13 C14 Li2 41.19(19) . . . . ?
C18 C13 C14 Li2 -134.07(16) . . . . ?
C13 C14 C15 C16 1.6(3) . . . . ?
Li2 C14 C15 C16 99.3(2) . . . . ?
C14 C15 C16 C17 -0.8(3) . . . . ?
C15 C16 C17 C18 -0.6(3) . . . . ?
C16 C17 C18 N4 -176.34(18) . . . . ?
C16 C17 C18 C13 1.3(3) . . . . ?
N3 C13 C18 C17 -176.78(16) . . . . ?
C14 C13 C18 C17 -0.5(3) . . . . ?
Li2 C13 C18 C17 -96.5(2) . . . . ?
N3 C13 C18 N4 1.30(18) . . . . ?
C14 C13 C18 N4 177.59(15) . . . . ?
Li2 C13 C18 N4 81.6(2) . . . . ?
O3 C19 C20 O4 37.57(16) . . . . ?
C21 C19 C20 O4 155.79(14) . . . . ?
C22 C19 C20 O4 -79.80(17) . . . . ?
O3 C19 C20 C23 155.09(15) . . . . ?
C21 C19 C20 C23 -86.69(19) . . . . ?
C22 C19 C20 C23 37.7(2) . . . . ?
O3 C19 C20 C24 -79.64(17) . . . . ?
C21 C19 C20 C24 38.6(2) . . . . ?
C22 C19 C20 C24 163.00(15) . . . . ?
O5 C25 C26 C27 -23.6(3) . . . . ?
C25 C26 C27 C28 2.0(3) . . . . ?
C26 C27 C28 O5 20.1(2) . . . . ?
O6 C29 C30 C31 -28.3(2) . . . . ?
C29 C30 C31 C32 38.7(2) . . . . ?
C30 C31 C32 O6 -35.6(2) . . . . ?
N5 C33 C34 N6 56.7(2) . . . . ?
N1 B1 B2 O1 84.86(18) . . . . ?
N2 B1 B2 O1 -93.5(2) . . . . ?
N1 B1 B2 O2 -158.19(14) . . . . ?
N2 B1 B2 O2 23.5(3) . . . . ?
N1 B1 B2 N3 -37.0(2) . . . . ?
N2 B1 B2 N3 144.63(17) . . . . ?
N1 B1 B2 Li2 -110.03(16) . . . . ?
N2 B1 B2 Li2 71.6(2) . . . . ?
N4 B3 B4 O4 19.4(3) . . . . ?
N3 B3 B4 O4 -163.76(14) . . . . ?
N4 B3 B4 O3 -96.4(2) . . . . ?
N3 B3 B4 O3 80.51(18) . . . . ?
N4 B3 B4 N1 146.05(17) . . . . ?
N3 B3 B4 N1 -37.1(2) . . . . ?
C2 C1 N1 B1 -178.52(17) . . . . ?
C6 C1 N1 B1 0.19(17) . . . . ?
C2 C1 N1 B4 6.7(3) . . . . ?
C6 C1 N1 B4 -174.64(15) . . . . ?
N2 B1 N1 C1 -0.20(17) . . . . ?
B2 B1 N1 C1 -178.90(14) . . . . ?
N2 B1 N1 B4 175.39(13) . . . . ?
B2 B1 N1 B4 -3.3(2) . . . . ?
O4 B4 N1 C1 -17.2(2) . . . . ?
O3 B4 N1 C1 95.88(18) . . . . ?
B3 B4 N1 C1 -148.41(15) . . . . ?
O4 B4 N1 B1 168.41(13) . . . . ?
O3 B4 N1 B1 -78.48(18) . . . . ?
B3 B4 N1 B1 37.22(18) . . . . ?
C5 C6 N2 B1 -179.64(18) . . . . ?
C1 C6 N2 B1 -0.02(18) . . . . ?
N1 B1 N2 C6 0.14(18) . . . . ?
B2 B1 N2 C6 178.68(16) . . . . ?
C14 C13 N3 B3 -176.23(17) . . . . ?
C18 C13 N3 B3 -0.65(18) . . . . ?
Li2 C13 N3 B3 -133.82(14) . . . . ?
C14 C13 N3 B2 9.9(3) . . . . ?
C18 C13 N3 B2 -174.53(16) . . . . ?
Li2 C13 N3 B2 52.29(17) . . . . ?
C14 C13 N3 Li2 -42.41(19) . . . . ?
C18 C13 N3 Li2 133.18(14) . . . . ?
N4 B3 N3 C13 -0.23(17) . . . . ?
B4 B3 N3 C13 -177.84(14) . . . . ?
N4 B3 N3 B2 174.69(13) . . . . ?
B4 B3 N3 B2 -2.9(2) . . . . ?
N4 B3 N3 Li2 -92.3(2) . . . . ?
B4 B3 N3 Li2 90.0(2) . . . . ?
O1 B2 N3 C13 90.2(2) . . . . ?
O2 B2 N3 C13 -22.4(2) . . . . ?
B1 B2 N3 C13 -149.79(16) . . . . ?
Li2 B2 N3 C13 -54.41(18) . . . . ?
O1 B2 N3 B3 -83.19(17) . . . . ?
O2 B2 N3 B3 164.18(13) . . . . ?
B1 B2 N3 B3 36.80(18) . . . . ?
Li2 B2 N3 B3 132.17(15) . . . . ?
O1 B2 N3 Li2 144.64(15) . . . . ?
O2 B2 N3 Li2 32.00(13) . . . . ?
B1 B2 N3 Li2 -95.38(14) . . . . ?
C17 C18 N4 B3 176.39(19) . . . . ?
C13 C18 N4 B3 -1.46(19) . . . . ?
N3 B3 N4 C18 1.05(18) . . . . ?
B4 B3 N4 C18 178.35(16) . . . . ?
C34 C33 N5 C36 74.4(2) . . . . ?
C34 C33 N5 C35 -164.17(17) . . . . ?
C34 C33 N5 Li2 -37.8(2) . . . . ?
C33 C34 N6 C38 -165.76(16) . . . . ?
C33 C34 N6 C37 75.2(2) . . . . ?
C33 C34 N6 Li2 -40.4(2) . . . . ?
C10 C7 O1 B2 94.35(17) . . . . ?
C9 C7 O1 B2 -147.18(15) . . . . ?
C8 C7 O1 B2 -26.16(17) . . . . ?
C10 C7 O1 Li1 -78.5(2) . . . . ?
C9 C7 O1 Li1 40.0(3) . . . . ?
C8 C7 O1 Li1 160.98(17) . . . . ?
O2 B2 O1 C7 7.83(17) . . . . ?
N3 B2 O1 C7 -107.92(15) . . . . ?
B1 B2 O1 C7 133.95(14) . . . . ?
Li2 B2 O1 C7 -18.5(3) . . . . ?
O2 B2 O1 Li1 -177.88(13) . . . . ?
N3 B2 O1 Li1 66.37(18) . . . . ?
B1 B2 O1 Li1 -51.75(18) . . . . ?
Li2 B2 O1 Li1 155.8(2) . . . . ?
C12 C8 O2 B2 -152.77(15) . . . . ?
C11 C8 O2 B2 87.86(17) . . . . ?
C7 C8 O2 B2 -31.49(17) . . . . ?
C12 C8 O2 Li2 20.0(4) . . . . ?
C11 C8 O2 Li2 -99.4(4) . . . . ?
C7 C8 O2 Li2 141.3(3) . . . . ?
O1 B2 O2 C8 16.01(17) . . . . ?
N3 B2 O2 C8 135.09(13) . . . . ?
B1 B2 O2 C8 -104.54(15) . . . . ?
Li2 B2 O2 C8 177.09(17) . . . . ?
O1 B2 O2 Li2 -161.08(14) . . . . ?
N3 B2 O2 Li2 -42.00(16) . . . . ?
B1 B2 O2 Li2 78.37(17) . . . . ?
N6 Li2 O2 C8 140.8(3) . . . . ?
N5 Li2 O2 C8 17.4(5) . . . . ?
N3 Li2 O2 C8 -147.4(3) . . . . ?
B2 Li2 O2 C8 -173.2(4) . . . . ?
C14 Li2 O2 C8 -87.7(4) . . . . ?
C13 Li2 O2 C8 -119.1(3) . . . . ?
N6 Li2 O2 B2 -46.0(3) . . . . ?
N5 Li2 O2 B2 -169.43(16) . . . . ?
N3 Li2 O2 B2 25.75(10) . . . . ?
C14 Li2 O2 B2 85.44(12) . . . . ?
C13 Li2 O2 B2 54.05(12) . . . . ?
C21 C19 O3 B4 -149.21(15) . . . . ?
C22 C19 O3 B4 92.18(16) . . . . ?
C20 C19 O3 B4 -27.55(16) . . . . ?
C21 C19 O3 Li1 46.1(2) . . . . ?
C22 C19 O3 Li1 -72.5(2) . . . . ?
C20 C19 O3 Li1 167.72(16) . . . . ?
O4 B4 O3 C19 8.43(17) . . . . ?
N1 B4 O3 C19 -110.30(14) . . . . ?
B3 B4 O3 C19 134.74(14) . . . . ?
O4 B4 O3 Li1 175.06(14) . . . . ?
N1 B4 O3 Li1 56.32(19) . . . . ?
B3 B4 O3 Li1 -58.63(18) . . . . ?
C23 C20 O4 B4 -155.32(14) . . . . ?
C24 C20 O4 B4 85.39(16) . . . . ?
C19 C20 O4 B4 -33.82(17) . . . . ?
O3 B4 O4 C20 16.78(16) . . . . ?
N1 B4 O4 C20 134.51(14) . . . . ?
B3 B4 O4 C20 -101.41(16) . . . . ?
C26 C25 O5 C28 37.2(2) . . . . ?
C26 C25 O5 Li1 -139.1(2) . . . . ?
C27 C28 O5 C25 -36.0(2) . . . . ?
C27 C28 O5 Li1 141.21(17) . . . . ?
C30 C29 O6 C32 6.3(2) . . . . ?
C30 C29 O6 Li1 -174.92(19) . . . . ?
C31 C32 O6 C29 18.7(2) . . . . ?
C31 C32 O6 Li1 -160.37(16) . . . . ?

_refine_diff_density_max         0.343
_refine_diff_density_min         -0.291
_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_wo2ck
_database_code_depnum_ccdc_archive 'CCDC 2089029'
loop_
_audit_author_name
_audit_author_address
'Christian Kleeberg'
;Technische Universitaet Braunschweig, Institut fuer Anorganische und Analytische Chemie
Germany
;
_audit_update_record             
;
2021-06-09 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66.91 H105.82 B8 N8 Na4 O12.73'
_chemical_formula_sum            'C66.91 H105.82 B8 N8 Na4 O12.73'
_chemical_formula_weight         1404.41

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'
B B 0.0090 0.0039 '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'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_H-M_alt        'P 32 2 1'
_space_group_name_Hall           'P 32 2"'

_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'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'

_cell_length_a                   16.6556(2)
_cell_length_b                   16.6556(2)
_cell_length_c                   27.4355(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6591.19(17)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    28056
_cell_measurement_theta_min      4.42
_cell_measurement_theta_max      75.75

_exptl_crystal_description       'fragment of prism'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_F_000             2247.4
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.242
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7937
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_crystal_recrystallization_method 
;
 From a solution in THF layered with n-pentane at -40deg C.
;

_exptl_special_details           
;
 The crystal was mounted at rt with perfluoroether oil on top of a human hair
 and placed in a cold nitrogen gas stream on the diffractometer.

 The collected data cover more than a hemisphere of the reciprocal space.
 A combination of 18 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 1.0 deg in ω.
 Each frame was exposured for 2 s (low 2θ angles) or 6 s (high 2θ angles).
 Nominal crystal to detector distance 53 mm.
;



_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            59566
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.462
_diffrn_reflns_theta_max         76.061
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9108
_reflns_number_gt                8695
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.999

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



_computing_data_collection       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution    
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_molecular_graphics    
;
 K. Brandenburg, 2016, Diamond 4.2.2, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;




_refine_special_details          
;
 The crystal was refined a 2-component inversion twin.

 No appropriate model could be established for cocrystallised solvent 
 molecules; the data were processed using the SQUEEZE/PLATON program 
 (A. L. Spek, Acta Cryst., 2015, C71, 9-18.).

 Two disordered THF moieties (one including the coordinated Na atom) were 
 refined using split atom model (0.51(2) and 0.769(7) SOF of main components).
 One of these moieties was refined applying similarity restraints (SAME) and
 restraining the ADP to approximate isotropic behaviour.

 N-H hydrogen atoms were identified clearly in the difference fourier map and 
 were refined restraining the NHC distance to 0.87 Ang (DFIX),
 all other H atoms were placed in idealised positions and refined using a 
 riding model, with a common U restrained to be 1.2 (1.5 for methyl groups) 
 times the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond but not tip.


 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;




_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0766P)²+2.7526P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9108
_refine_ls_number_parameters     535
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1469
_refine_ls_wR_factor_gt          0.1453
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.069
_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
C1 C 0.6084(2) 0.1059(2) 0.78532(11) 0.0325(6) Uani 1 1 d . . . . .
C2 C 0.6248(2) 0.0794(2) 0.83043(11) 0.0370(7) Uani 1 1 d . . . . .
H2 H 0.5840 0.0687 0.8570 0.044 Uiso 1 1 calc R U . . .
C3 C 0.7022(3) 0.0686(2) 0.83630(11) 0.0411(7) Uani 1 1 d . . . . .
H3 H 0.7146 0.0514 0.8672 0.049 Uiso 1 1 calc R U . . .
C4 C 0.7612(3) 0.0829(3) 0.79728(12) 0.0426(7) Uani 1 1 d . . . . .
H4 H 0.8127 0.0739 0.8016 0.051 Uiso 1 1 calc R U . . .
C5 C 0.7455(2) 0.1106(2) 0.75172(11) 0.0383(7) Uani 1 1 d . . . . .
H5 H 0.7862 0.1204 0.7253 0.046 Uiso 1 1 calc R U . . .
C6 C 0.6700(2) 0.1235(2) 0.74550(10) 0.0323(6) Uani 1 1 d . . . . .
C7 C 0.4666(3) 0.3098(3) 0.69193(13) 0.0485(9) Uani 1 1 d . . . . .
C8 C 0.3843(3) 0.2217(3) 0.71341(12) 0.0488(9) Uani 1 1 d . . . . .
C9 C 0.5049(4) 0.3947(3) 0.72524(16) 0.0658(13) Uani 1 1 d . . . . .
H9A H 0.5300 0.3828 0.7549 0.099 Uiso 1 1 calc R U . . .
H9B H 0.4550 0.4070 0.7339 0.099 Uiso 1 1 calc R U . . .
H9C H 0.5542 0.4486 0.7082 0.099 Uiso 1 1 calc R U . . .
C10 C 0.4469(4) 0.3374(3) 0.64179(14) 0.0594(11) Uani 1 1 d . . . . .
H10A H 0.5049 0.3863 0.6276 0.089 Uiso 1 1 calc R U . . .
H10B H 0.4033 0.3603 0.6455 0.089 Uiso 1 1 calc R U . . .
H10C H 0.4199 0.2832 0.6202 0.089 Uiso 1 1 calc R U . . .
C11 C 0.3932(3) 0.2129(3) 0.76847(12) 0.0561(10) Uani 1 1 d . . . . .
H11A H 0.3483 0.1498 0.7790 0.084 Uiso 1 1 calc R U . . .
H11B H 0.3810 0.2573 0.7856 0.084 Uiso 1 1 calc R U . . .
H11C H 0.4561 0.2260 0.7761 0.084 Uiso 1 1 calc R U . . .
C12 C 0.2892(4) 0.2110(4) 0.70297(15) 0.0675(13) Uani 1 1 d . . . . .
H12A H 0.2821 0.2155 0.6678 0.101 Uiso 1 1 calc R U . . .
H12B H 0.2841 0.2602 0.7197 0.101 Uiso 1 1 calc R U . . .
H12C H 0.2406 0.1505 0.7147 0.101 Uiso 1 1 calc R U . . .
C13 C 0.4405(2) 0.1223(2) 0.58757(10) 0.0340(6) Uani 1 1 d . . . . .
C14 C 0.3519(3) 0.1113(3) 0.58087(12) 0.0419(7) Uani 1 1 d . . . . .
H14 H 0.3226 0.1254 0.6065 0.050 Uiso 1 1 calc R U . A 3
C15 C 0.3076(3) 0.0792(3) 0.53602(12) 0.0462(8) Uani 1 1 d . . . . .
H15 H 0.2477 0.0717 0.5314 0.055 Uiso 1 1 calc R U . . .
C16 C 0.3490(3) 0.0582(3) 0.49808(12) 0.0433(8) Uani 1 1 d . . . . .
H16 H 0.3169 0.0360 0.4681 0.052 Uiso 1 1 calc R U . . .
C17 C 0.4370(2) 0.0694(2) 0.50352(11) 0.0379(7) Uani 1 1 d . . . . .
H17 H 0.4660 0.0563 0.4773 0.045 Uiso 1 1 calc R U . . .
C18 C 0.4816(2) 0.1002(2) 0.54825(11) 0.0343(6) Uani 1 1 d . . . . .
C19 C 0.8189(2) 0.2042(3) 0.61634(11) 0.0442(8) Uani 1 1 d . . . . .
C20 C 0.8372(2) 0.2977(3) 0.63795(13) 0.0468(8) Uani 1 1 d . . . . .
C21 C 0.8953(3) 0.1803(4) 0.62529(14) 0.0574(11) Uani 1 1 d . . . . .
H21A H 0.9039 0.1773 0.6604 0.086 Uiso 1 1 calc R U . . .
H21B H 0.9534 0.2281 0.6107 0.086 Uiso 1 1 calc R U . . .
H21C H 0.8774 0.1201 0.6105 0.086 Uiso 1 1 calc R U . . .
C22 C 0.7980(3) 0.1963(3) 0.56136(12) 0.0490(9) Uani 1 1 d . . . . .
H22A H 0.7753 0.1323 0.5507 0.073 Uiso 1 1 calc R U . . .
H22B H 0.8547 0.2380 0.5435 0.073 Uiso 1 1 calc R U . . .
H22C H 0.7506 0.2134 0.5549 0.073 Uiso 1 1 calc R U . . .
C23 C 0.8944(3) 0.3246(3) 0.68490(14) 0.0558(10) Uani 1 1 d . . . . .
H23A H 0.8950 0.3786 0.6995 0.084 Uiso 1 1 calc R U . . .
H23B H 0.9580 0.3398 0.6774 0.084 Uiso 1 1 calc R U . . .
H23C H 0.8667 0.2726 0.7079 0.084 Uiso 1 1 calc R U . . .
C24 C 0.8826(3) 0.3792(3) 0.60223(15) 0.0629(12) Uani 1 1 d . . . . .
H24A H 0.8436 0.3650 0.5732 0.094 Uiso 1 1 calc R U . . .
H24B H 0.9438 0.3895 0.5928 0.094 Uiso 1 1 calc R U . . .
H24C H 0.8893 0.4351 0.6179 0.094 Uiso 1 1 calc R U . . .
C25 C 0.8082(4) 0.3594(4) 0.80500(17) 0.0713(14) Uani 1 1 d . . . . .
H25A H 0.8664 0.4157 0.7953 0.086 Uiso 1 1 calc R U . . .
H25B H 0.8099 0.3043 0.7929 0.086 Uiso 1 1 calc R U . . .
B1 B 0.5502(3) 0.1444(2) 0.71852(12) 0.0332(7) Uani 1 1 d . . . . .
B2 B 0.4908(3) 0.1803(3) 0.67992(12) 0.0346(7) Uani 1 1 d . . . . .
B3 B 0.5832(3) 0.1481(2) 0.61360(12) 0.0332(7) Uani 1 1 d . . . . .
B4 B 0.6786(2) 0.1794(2) 0.65174(11) 0.0317(7) Uani 1 1 d . . . . .
N1 N 0.63554(18) 0.14720(17) 0.70465(8) 0.0310(5) Uani 1 1 d . . . . .
N2 N 0.5375(2) 0.11886(19) 0.76964(9) 0.0344(5) Uani 1 1 d D . . . .
N3 N 0.50006(19) 0.15008(18) 0.62762(9) 0.0326(5) Uani 1 1 d . . . . .
N4 N 0.56727(19) 0.11633(18) 0.56341(9) 0.0343(5) Uani 1 1 d D . . . .
O1 O 0.53653(18) 0.28453(16) 0.68592(8) 0.0409(5) Uani 1 1 d . . . . .
O2 O 0.39065(17) 0.14883(17) 0.68984(8) 0.0400(5) Uani 1 1 d . . . . .
O3 O 0.73753(16) 0.13779(15) 0.64166(7) 0.0357(5) Uani 1 1 d . . . . .
O4 O 0.74572(17) 0.28165(16) 0.64940(8) 0.0402(5) Uani 1 1 d . . . . .
Na1 Na 0.68781(11) 0.34226(10) 0.70377(5) 0.0515(4) Uani 1 1 d . . . . .
Na2 Na 0.62863(12) 0.0000 0.6667 0.0426(4) Uani 1 2 d S T P . .
Na3 Na 0.2931(2) 0.0000 0.6667 0.0443(8) Uani 0.728(8) 2 d S T P B 3
O7 O 0.1470(3) 0.0000 0.6667 0.0705(19) Uani 0.728(8) 2 d S T P B 3
C33 C 0.0839(6) -0.0274(8) 0.7082(3) 0.098(3) Uani 0.728(8) 1 d . . P B 3
H33A H 0.1177 -0.0035 0.7394 0.117 Uiso 0.728(8) 1 calc R U P B 3
H33B H 0.0436 -0.0955 0.7103 0.117 Uiso 0.728(8) 1 calc R U P B 3
C34 C 0.027(2) 0.022(3) 0.6940(9) 0.111(12) Uani 0.364(4) 1 d . . P B 3
H34A H -0.0386 -0.0174 0.7039 0.134 Uiso 0.364(4) 1 calc R U P B 3
H34B H 0.0525 0.0818 0.7116 0.134 Uiso 0.364(4) 1 calc R U P B 3
C35 C 0.031(2) 0.037(3) 0.6472(13) 0.117(12) Uani 0.364(4) 1 d . . P B 3
H35A H 0.0418 0.1001 0.6409 0.140 Uiso 0.364(4) 1 calc R U P B 3
H35B H -0.0281 -0.0082 0.6318 0.140 Uiso 0.364(4) 1 calc R U P B 3
Na3' Na 0.3512(8) 0.0000 0.6667 0.051(3) Uani 0.272(8) 2 d S T P B 4
H2N H 0.487(3) 0.108(3) 0.7908(15) 0.044(10) Uiso 1 1 d D . . . .
H4N H 0.619(5) 0.117(5) 0.543(3) 0.12(2) Uiso 1 1 d D . . . .
O5 O 0.7291(2) 0.3617(2) 0.78543(10) 0.0583(7) Uani 1 1 d . . . . .
C26 C 0.7973(6) 0.3552(7) 0.8587(2) 0.105(3) Uani 1 1 d . . . . .
H26A H 0.7759 0.2915 0.8706 0.126 Uiso 1 1 calc R U . . .
H26B H 0.8570 0.3980 0.8746 0.126 Uiso 1 1 calc R U . . .
C27 C 0.7280(5) 0.3827(5) 0.86967(17) 0.0850(18) Uani 1 1 d . . . . .
H27A H 0.7578 0.4504 0.8751 0.102 Uiso 1 1 calc R U . . .
H27B H 0.6911 0.3499 0.8988 0.102 Uiso 1 1 calc R U . . .
C28 C 0.6688(4) 0.3542(4) 0.82486(15) 0.0660(12) Uani 1 1 d . . . . .
H28A H 0.6170 0.2896 0.8280 0.079 Uiso 1 1 calc R U . . .
H28B H 0.6429 0.3955 0.8193 0.079 Uiso 1 1 calc R U . . .
O6 O 0.7831(9) 0.4990(5) 0.6865(3) 0.080(3) Uani 0.543(15) 1 d D . P C 1
C29 C 0.8157(10) 0.5714(7) 0.7192(4) 0.082(3) Uani 0.543(15) 1 d D U P C 1
H29A H 0.8723 0.5793 0.7354 0.099 Uiso 0.543(15) 1 calc R U P C 1
H29B H 0.7684 0.5583 0.7445 0.099 Uiso 0.543(15) 1 calc R U P C 1
C30 C 0.8361(9) 0.6530(7) 0.6936(5) 0.075(4) Uani 0.543(15) 1 d D U P C 1
H30A H 0.9020 0.7009 0.6978 0.091 Uiso 0.543(15) 1 calc R U P C 1
H30B H 0.7968 0.6782 0.7054 0.091 Uiso 0.543(15) 1 calc R U P C 1
C31 C 0.8154(14) 0.6240(12) 0.6418(5) 0.139(7) Uani 0.543(15) 1 d D U P C 1
H31A H 0.7591 0.6247 0.6310 0.167 Uiso 0.543(15) 1 calc R U P C 1
H31B H 0.8679 0.6664 0.6207 0.167 Uiso 0.543(15) 1 calc R U P C 1
C32 C 0.8030(14) 0.5426(11) 0.6395(5) 0.110(5) Uani 0.543(15) 1 d D U P C 1
H32A H 0.8593 0.5450 0.6260 0.132 Uiso 0.543(15) 1 calc R U P C 1
H32B H 0.7508 0.5050 0.6171 0.132 Uiso 0.543(15) 1 calc R U P C 1
O6' O 0.7381(9) 0.4953(6) 0.6905(3) 0.061(2) Uani 0.457(15) 1 d D . P C 2
C29' C 0.7674(11) 0.5756(6) 0.7183(3) 0.065(4) Uani 0.457(15) 1 d D U P C 2
H29C H 0.8151 0.5827 0.7422 0.078 Uiso 0.457(15) 1 calc R U P C 2
H29D H 0.7146 0.5733 0.7361 0.078 Uiso 0.457(15) 1 calc R U P C 2
C30' C 0.8045(16) 0.6489(9) 0.6847(6) 0.106(7) Uani 0.457(15) 1 d D U P C 2
H30C H 0.8730 0.6836 0.6866 0.128 Uiso 0.457(15) 1 calc R U P C 2
H30D H 0.7813 0.6921 0.6913 0.128 Uiso 0.457(15) 1 calc R U P C 2
C31' C 0.7737(19) 0.6057(14) 0.6359(6) 0.133(8) Uani 0.457(15) 1 d D U P C 2
H31C H 0.7299 0.6230 0.6215 0.160 Uiso 0.457(15) 1 calc R U P C 2
H31D H 0.8276 0.6273 0.6138 0.160 Uiso 0.457(15) 1 calc R U P C 2
C32' C 0.7347(10) 0.5196(10) 0.6413(3) 0.075(4) Uani 0.457(15) 1 d D U P C 2
H32C H 0.7655 0.4947 0.6203 0.090 Uiso 0.457(15) 1 calc R U P C 2
H32D H 0.6692 0.4910 0.6308 0.090 Uiso 0.457(15) 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
C1 N2 1.372(4) . ?
C1 C2 1.386(4) . ?
C1 C6 1.425(4) . ?
C2 C3 1.396(5) . ?
C3 C4 1.391(5) . ?
C4 C5 1.401(4) . ?
C5 C6 1.388(5) . ?
C5 Na2 3.007(3) . ?
C6 N1 1.404(4) . ?
C6 Na2 2.822(3) . ?
C7 O1 1.432(5) . ?
C7 C9 1.529(5) . ?
C7 C10 1.537(5) . ?
C7 C8 1.539(6) . ?
C8 O2 1.425(4) . ?
C8 C12 1.529(6) . ?
C8 C11 1.532(4) . ?
C13 N3 1.396(4) . ?
C13 C14 1.404(5) . ?
C13 C18 1.421(4) . ?
C13 Na3' 2.835(4) . ?
C14 C15 1.396(5) . ?
C14 Na3 2.849(3) . ?
C14 Na3' 2.992(5) . ?
C15 C16 1.386(5) . ?
C16 C17 1.390(5) . ?
C17 C18 1.393(4) . ?
C18 N4 1.378(4) . ?
C19 O3 1.430(4) . ?
C19 C21 1.532(6) . ?
C19 C22 1.539(4) . ?
C19 C20 1.546(6) . ?
C20 O4 1.444(5) . ?
C20 C23 1.529(5) . ?
C20 C24 1.532(5) . ?
C25 O5 1.440(6) . ?
C25 C26 1.481(7) . ?
B1 N1 1.449(5) . ?
B1 N2 1.450(4) . ?
B1 B2 1.748(5) . ?
B1 Na1 2.954(4) . ?
B2 O2 1.502(5) . ?
B2 O1 1.516(4) . ?
B2 N3 1.554(4) . ?
B2 Na3' 2.752(6) . ?
B2 Na1 3.102(4) . ?
B2 Na3 3.179(4) . ?
B3 N4 1.451(4) . ?
B3 N3 1.454(5) . ?
B3 B4 1.750(5) . ?
B4 O3 1.484(4) . ?
B4 O4 1.500(4) . ?
B4 N1 1.589(4) . ?
B4 Na2 2.703(3) . ?
B4 Na1 3.000(4) . ?
N1 Na2 2.613(3) . ?
N1 Na1 2.913(3) . ?
N3 Na3' 2.710(7) . ?
O1 Na1 2.256(3) . ?
O2 Na3 2.272(3) . ?
O2 Na3' 2.314(4) . ?
O3 Na2 2.206(2) . ?
O4 Na1 2.269(3) . ?
Na1 O6' 2.279(8) . ?
Na1 O5 2.318(3) . ?
Na1 O6 2.327(7) . ?
Na2 O3 2.206(2) 5_556 ?
Na2 N1 2.613(3) 5_556 ?
Na2 B4 2.703(4) 5_556 ?
Na2 C6 2.822(3) 5_556 ?
Na2 C5 3.007(3) 5_556 ?
Na3 O2 2.272(3) 5_556 ?
Na3 O7 2.433(7) . ?
Na3 C14 2.849(3) 5_556 ?
Na3 B2 3.179(4) 5_556 ?
O7 C33 1.461(8) . ?
O7 C33 1.461(8) 5_556 ?
C33 C34 1.58(3) . ?
C34 C35 1.30(2) . ?
C35 C33 1.54(3) 5_556 ?
Na3' O2 2.314(4) 5_556 ?
Na3' N3 2.710(6) 5_556 ?
Na3' B2 2.752(5) 5_556 ?
Na3' C13 2.835(4) 5_556 ?
Na3' C14 2.992(5) 5_556 ?
O5 C28 1.438(5) . ?
C26 C27 1.471(8) . ?
C27 C28 1.497(6) . ?
O6 C29 1.379(10) . ?
O6 C32 1.435(11) . ?
C29 C30 1.412(12) . ?
C30 C31 1.486(15) . ?
C31 C32 1.266(17) . ?
O6' C29' 1.399(9) . ?
O6' C32' 1.418(10) . ?
C29' C30' 1.403(13) . ?
C30' C31' 1.484(16) . ?
C31' C32' 1.254(17) . ?

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
N2 C1 C2 130.7(3) . . ?
N2 C1 C6 108.4(3) . . ?
C2 C1 C6 120.9(3) . . ?
C1 C2 C3 119.0(3) . . ?
C4 C3 C2 120.5(3) . . ?
C3 C4 C5 120.7(3) . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 Na2 68.91(18) . . ?
C4 C5 Na2 131.4(2) . . ?
C5 C6 N1 132.2(3) . . ?
C5 C6 C1 119.3(3) . . ?
N1 C6 C1 108.4(3) . . ?
C5 C6 Na2 83.8(2) . . ?
N1 C6 Na2 66.92(15) . . ?
C1 C6 Na2 123.3(2) . . ?
O1 C7 C9 108.4(3) . . ?
O1 C7 C10 108.2(3) . . ?
C9 C7 C10 108.2(3) . . ?
O1 C7 C8 103.4(3) . . ?
C9 C7 C8 114.4(4) . . ?
C10 C7 C8 113.9(4) . . ?
O2 C8 C12 109.2(3) . . ?
O2 C8 C11 108.3(3) . . ?
C12 C8 C11 108.5(3) . . ?
O2 C8 C7 103.2(3) . . ?
C12 C8 C7 114.6(4) . . ?
C11 C8 C7 112.7(3) . . ?
N3 C13 C14 132.3(3) . . ?
N3 C13 C18 109.2(3) . . ?
C14 C13 C18 118.5(3) . . ?
N3 C13 Na3' 70.5(2) . . ?
C14 C13 Na3' 82.4(3) . . ?
C18 C13 Na3' 122.9(3) . . ?
C15 C14 C13 119.0(3) . . ?
C15 C14 Na3 122.4(3) . . ?
C13 C14 Na3 88.5(2) . . ?
C15 C14 Na3' 128.2(3) . . ?
C13 C14 Na3' 69.9(3) . . ?
C16 C15 C14 121.6(3) . . ?
C15 C16 C17 120.6(3) . . ?
C16 C17 C18 118.5(3) . . ?
N4 C18 C17 130.4(3) . . ?
N4 C18 C13 107.8(3) . . ?
C17 C18 C13 121.8(3) . . ?
O3 C19 C21 108.1(3) . . ?
O3 C19 C22 108.9(3) . . ?
C21 C19 C22 108.5(3) . . ?
O3 C19 C20 103.1(3) . . ?
C21 C19 C20 115.4(3) . . ?
C22 C19 C20 112.6(3) . . ?
O4 C20 C23 108.4(3) . . ?
O4 C20 C24 108.0(3) . . ?
C23 C20 C24 108.7(3) . . ?
O4 C20 C19 103.8(3) . . ?
C23 C20 C19 113.5(4) . . ?
C24 C20 C19 114.1(3) . . ?
O5 C25 C26 106.2(4) . . ?
N1 B1 N2 105.1(3) . . ?
N1 B1 B2 123.0(3) . . ?
N2 B1 B2 131.4(3) . . ?
N1 B1 Na1 74.14(17) . . ?
N2 B1 Na1 112.2(2) . . ?
B2 B1 Na1 77.93(17) . . ?
O2 B2 O1 102.4(3) . . ?
O2 B2 N3 109.1(3) . . ?
O1 B2 N3 113.4(3) . . ?
O2 B2 B1 119.4(3) . . ?
O1 B2 B1 106.3(3) . . ?
N3 B2 B1 106.4(3) . . ?
O2 B2 Na3' 57.2(3) . . ?
O1 B2 Na3' 158.6(4) . . ?
N3 B2 Na3' 71.98(19) . . ?
B1 B2 Na3' 91.1(3) . . ?
O2 B2 Na1 140.6(2) . . ?
O1 B2 Na1 43.43(15) . . ?
N3 B2 Na1 104.1(2) . . ?
B1 B2 Na1 68.64(17) . . ?
Na3' B2 Na1 157.8(3) . . ?
O2 B2 Na3 41.06(15) . . ?
O1 B2 Na3 141.7(2) . . ?
N3 B2 Na3 79.16(18) . . ?
B1 B2 Na3 104.01(19) . . ?
Na1 B2 Na3 172.48(14) . . ?
N4 B3 N3 104.9(3) . . ?
N4 B3 B4 130.5(3) . . ?
N3 B3 B4 124.6(3) . . ?
O3 B4 O4 103.4(3) . . ?
O3 B4 N1 107.7(2) . . ?
O4 B4 N1 112.2(2) . . ?
O3 B4 B3 117.6(2) . . ?
O4 B4 B3 111.3(2) . . ?
N1 B4 B3 104.9(2) . . ?
O3 B4 Na2 54.64(14) . . ?
O4 B4 Na2 154.7(2) . . ?
N1 B4 Na2 69.54(15) . . ?
B3 B4 Na2 91.67(18) . . ?
O3 B4 Na1 139.9(2) . . ?
O4 B4 Na1 47.31(14) . . ?
N1 B4 Na1 71.41(15) . . ?
B3 B4 Na1 100.52(19) . . ?
Na2 B4 Na1 140.88(12) . . ?
C6 N1 B1 108.3(2) . . ?
C6 N1 B4 130.2(3) . . ?
B1 N1 B4 121.4(2) . . ?
C6 N1 Na2 83.47(17) . . ?
B1 N1 Na2 119.5(2) . . ?
B4 N1 Na2 75.73(16) . . ?
C6 N1 Na1 112.62(18) . . ?
B1 N1 Na1 77.28(17) . . ?
B4 N1 Na1 77.46(16) . . ?
Na2 N1 Na1 153.07(10) . . ?
C1 N2 B1 109.7(3) . . ?
C13 N3 B3 108.2(2) . . ?
C13 N3 B2 131.7(3) . . ?
B3 N3 B2 120.1(3) . . ?
C13 N3 Na3' 80.5(2) . . ?
B3 N3 Na3' 121.7(3) . . ?
B2 N3 Na3' 74.98(17) . . ?
C18 N4 B3 109.9(3) . . ?
C7 O1 B2 109.4(3) . . ?
C7 O1 Na1 138.5(2) . . ?
B2 O1 Na1 109.1(2) . . ?
C8 O2 B2 109.1(3) . . ?
C8 O2 Na3 137.7(2) . . ?
B2 O2 Na3 113.2(2) . . ?
C8 O2 Na3' 159.2(3) . . ?
B2 O2 Na3' 89.7(4) . . ?
C19 O3 B4 108.7(3) . . ?
C19 O3 Na2 157.6(2) . . ?
B4 O3 Na2 92.09(18) . . ?
C20 O4 B4 109.7(3) . . ?
C20 O4 Na1 134.8(2) . . ?
B4 O4 Na1 103.62(18) . . ?
O1 Na1 O4 107.47(10) . . ?
O1 Na1 O6' 98.6(3) . . ?
O4 Na1 O6' 113.1(3) . . ?
O1 Na1 O5 117.34(12) . . ?
O4 Na1 O5 122.35(12) . . ?
O6' Na1 O5 94.7(2) . . ?
O1 Na1 O6 115.1(4) . . ?
O4 Na1 O6 99.3(3) . . ?
O5 Na1 O6 93.0(2) . . ?
O1 Na1 N1 83.06(9) . . ?
O4 Na1 N1 57.70(8) . . ?
O6' Na1 N1 170.5(3) . . ?
O5 Na1 N1 92.86(11) . . ?
O6 Na1 N1 155.3(3) . . ?
O1 Na1 B1 58.41(10) . . ?
O4 Na1 B1 81.88(10) . . ?
O6' Na1 B1 156.3(3) . . ?
O5 Na1 B1 91.93(12) . . ?
O6 Na1 B1 173.2(3) . . ?
N1 Na1 B1 28.59(9) . . ?
O1 Na1 B4 88.29(10) . . ?
O4 Na1 B4 29.06(9) . . ?
O6' Na1 B4 139.4(3) . . ?
O5 Na1 B4 117.61(12) . . ?
O6 Na1 B4 128.0(3) . . ?
N1 Na1 B4 31.13(7) . . ?
B1 Na1 B4 52.85(9) . . ?
O1 Na1 B2 27.50(9) . . ?
O4 Na1 B2 88.55(10) . . ?
O6' Na1 B2 125.2(3) . . ?
O5 Na1 B2 115.86(12) . . ?
O6 Na1 B2 139.8(3) . . ?
N1 Na1 B2 55.65(9) . . ?
B1 Na1 B2 33.43(10) . . ?
B4 Na1 B2 63.90(10) . . ?
O3 Na2 O3 144.84(16) . 5_556 ?
O3 Na2 N1 61.33(8) . . ?
O3 Na2 N1 137.44(8) 5_556 . ?
O3 Na2 N1 137.44(8) . 5_556 ?
O3 Na2 N1 61.33(8) 5_556 5_556 ?
N1 Na2 N1 129.69(14) . 5_556 ?
O3 Na2 B4 33.27(9) . . ?
O3 Na2 B4 169.75(9) 5_556 . ?
N1 Na2 B4 34.73(8) . . ?
N1 Na2 B4 127.85(11) 5_556 . ?
O3 Na2 B4 169.75(9) . 5_556 ?
O3 Na2 B4 33.27(9) 5_556 5_556 ?
N1 Na2 B4 127.85(11) . 5_556 ?
N1 Na2 B4 34.73(8) 5_556 5_556 ?
B4 Na2 B4 151.65(17) . 5_556 ?
O3 Na2 C6 111.50(8) . 5_556 ?
O3 Na2 C6 72.91(8) 5_556 5_556 ?
N1 Na2 C6 140.12(11) . 5_556 ?
N1 Na2 C6 29.61(8) 5_556 5_556 ?
B4 Na2 C6 117.31(10) . 5_556 ?
B4 Na2 C6 58.83(9) 5_556 5_556 ?
O3 Na2 C6 72.91(8) . . ?
O3 Na2 C6 111.50(8) 5_556 . ?
N1 Na2 C6 29.61(8) . . ?
N1 Na2 C6 140.12(11) 5_556 . ?
B4 Na2 C6 58.83(9) . . ?
B4 Na2 C6 117.31(10) 5_556 . ?
C6 Na2 C6 166.22(16) 5_556 . ?
O3 Na2 C5 70.15(9) . . ?
O3 Na2 C5 97.67(9) 5_556 . ?
N1 Na2 C5 53.46(9) . . ?
N1 Na2 C5 152.31(8) 5_556 . ?
B4 Na2 C5 72.14(10) . . ?
B4 Na2 C5 118.29(9) 5_556 . ?
C6 Na2 C5 166.03(12) 5_556 . ?
C6 Na2 C5 27.31(9) . . ?
O3 Na2 C5 97.67(9) . 5_556 ?
O3 Na2 C5 70.15(9) 5_556 5_556 ?
N1 Na2 C5 152.31(8) . 5_556 ?
N1 Na2 C5 53.46(9) 5_556 5_556 ?
B4 Na2 C5 118.29(9) . 5_556 ?
B4 Na2 C5 72.14(10) 5_556 5_556 ?
C6 Na2 C5 27.31(9) 5_556 5_556 ?
C6 Na2 C5 166.03(12) . 5_556 ?
C5 Na2 C5 140.10(15) . 5_556 ?
O2 Na3 O2 160.5(2) . 5_556 ?
O2 Na3 O7 99.77(11) . . ?
O2 Na3 O7 99.77(11) 5_556 . ?
O2 Na3 C14 107.33(10) . 5_556 ?
O2 Na3 C14 72.28(9) 5_556 5_556 ?
O7 Na3 C14 91.08(10) . 5_556 ?
O2 Na3 C14 72.29(9) . . ?
O2 Na3 C14 107.33(9) 5_556 . ?
O7 Na3 C14 91.08(10) . . ?
C14 Na3 C14 177.8(2) 5_556 . ?
O2 Na3 B2 135.21(17) . 5_556 ?
O2 Na3 B2 25.73(9) 5_556 5_556 ?
O7 Na3 B2 124.28(9) . 5_556 ?
C14 Na3 B2 67.85(10) 5_556 5_556 ?
C14 Na3 B2 110.84(11) . 5_556 ?
O2 Na3 B2 25.73(9) . . ?
O2 Na3 B2 135.21(17) 5_556 . ?
O7 Na3 B2 124.28(9) . . ?
C14 Na3 B2 110.85(11) 5_556 . ?
C14 Na3 B2 67.85(10) . . ?
B2 Na3 B2 111.43(17) 5_556 . ?
C33 O7 C33 111.3(8) . 5_556 ?
C33 O7 Na3 124.3(4) . . ?
C33 O7 Na3 124.3(4) 5_556 . ?
O7 C33 C34 99.8(12) . . ?
C35 C34 C33 111(3) . . ?
C34 C35 C33 110(3) . 5_556 ?
O2 Na3' O2 150.8(6) . 5_556 ?
O2 Na3' N3 58.78(10) . . ?
O2 Na3' N3 138.32(18) 5_556 . ?
O2 Na3' N3 138.32(18) . 5_556 ?
O2 Na3' N3 58.78(10) 5_556 5_556 ?
N3 Na3' N3 126.1(5) . 5_556 ?
O2 Na3' B2 171.3(2) . 5_556 ?
O2 Na3' B2 33.07(11) 5_556 5_556 ?
N3 Na3' B2 124.6(4) . 5_556 ?
N3 Na3' B2 33.04(10) 5_556 5_556 ?
O2 Na3' B2 33.07(11) . . ?
O2 Na3' B2 171.3(2) 5_556 . ?
N3 Na3' B2 33.04(10) . . ?
N3 Na3' B2 124.6(4) 5_556 . ?
B2 Na3' B2 145.2(5) 5_556 . ?
O2 Na3' C13 114.11(9) . 5_556 ?
O2 Na3' C13 71.02(8) 5_556 5_556 ?
N3 Na3' C13 136.4(4) . 5_556 ?
N3 Na3' C13 29.04(9) 5_556 5_556 ?
B2 Na3' C13 57.58(11) 5_556 5_556 ?
B2 Na3' C13 115.9(2) . 5_556 ?
O2 Na3' C13 71.02(8) . . ?
O2 Na3' C13 114.11(9) 5_556 . ?
N3 Na3' C13 29.04(9) . . ?
N3 Na3' C13 136.4(4) 5_556 . ?
B2 Na3' C13 115.9(2) 5_556 . ?
B2 Na3' C13 57.58(11) . . ?
C13 Na3' C13 161.0(5) 5_556 . ?
O2 Na3' C14 101.8(2) . 5_556 ?
O2 Na3' C14 68.99(14) 5_556 5_556 ?
N3 Na3' C14 151.41(17) . 5_556 ?
N3 Na3' C14 53.07(9) 5_556 5_556 ?
B2 Na3' C14 71.84(10) 5_556 5_556 ?
B2 Na3' C14 119.63(10) . 5_556 ?
C13 Na3' C14 27.71(10) 5_556 5_556 ?
C13 Na3' C14 170.5(4) . 5_556 ?
O2 Na3' C14 68.99(14) . . ?
O2 Na3' C14 101.8(2) 5_556 . ?
N3 Na3' C14 53.07(9) . . ?
N3 Na3' C14 151.41(17) 5_556 . ?
B2 Na3' C14 119.63(10) 5_556 . ?
B2 Na3' C14 71.84(10) . . ?
C13 Na3' C14 170.5(4) 5_556 . ?
C13 Na3' C14 27.71(10) . . ?
C14 Na3' C14 144.4(5) 5_556 . ?
C28 O5 C25 109.0(3) . . ?
C28 O5 Na1 124.7(3) . . ?
C25 O5 Na1 124.6(2) . . ?
C27 C26 C25 106.6(5) . . ?
C26 C27 C28 103.1(4) . . ?
O5 C28 C27 105.7(4) . . ?
C29 O6 C32 104.7(8) . . ?
C29 O6 Na1 126.7(7) . . ?
C32 O6 Na1 127.3(8) . . ?
O6 C29 C30 108.5(9) . . ?
C29 C30 C31 104.9(9) . . ?
C32 C31 C30 106.5(11) . . ?
C31 C32 O6 111.6(12) . . ?
C29' O6' C32' 106.9(8) . . ?
C29' O6' Na1 137.6(7) . . ?
C32' O6' Na1 115.3(7) . . ?
O6' C29' C30' 105.3(8) . . ?
C29' C30' C31' 106.1(11) . . ?
C32' C31' C30' 107.6(12) . . ?
C31' C32' O6' 111.6(11) . . ?

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
N2 C1 C2 C3 178.1(3) . . . . ?
C6 C1 C2 C3 -1.0(5) . . . . ?
C1 C2 C3 C4 -0.9(5) . . . . ?
C2 C3 C4 C5 1.6(5) . . . . ?
C3 C4 C5 C6 -0.2(5) . . . . ?
C3 C4 C5 Na2 -87.2(4) . . . . ?
C4 C5 C6 N1 -177.4(3) . . . . ?
Na2 C5 C6 N1 -50.9(3) . . . . ?
C4 C5 C6 C1 -1.7(5) . . . . ?
Na2 C5 C6 C1 124.9(3) . . . . ?
C4 C5 C6 Na2 -126.6(3) . . . . ?
N2 C1 C6 C5 -177.0(3) . . . . ?
C2 C1 C6 C5 2.3(5) . . . . ?
N2 C1 C6 N1 -0.3(3) . . . . ?
C2 C1 C6 N1 179.0(3) . . . . ?
N2 C1 C6 Na2 -74.3(3) . . . . ?
C2 C1 C6 Na2 105.0(3) . . . . ?
O1 C7 C8 O2 -35.3(3) . . . . ?
C9 C7 C8 O2 -153.0(3) . . . . ?
C10 C7 C8 O2 81.8(4) . . . . ?
O1 C7 C8 C12 -153.9(3) . . . . ?
C9 C7 C8 C12 88.4(4) . . . . ?
C10 C7 C8 C12 -36.8(4) . . . . ?
O1 C7 C8 C11 81.3(3) . . . . ?
C9 C7 C8 C11 -36.4(4) . . . . ?
C10 C7 C8 C11 -161.6(3) . . . . ?
N3 C13 C14 C15 -178.2(3) . . . . ?
C18 C13 C14 C15 0.0(5) . . . . ?
Na3' C13 C14 C15 -123.4(3) . . . . ?
N3 C13 C14 Na3 -51.5(4) . . . . ?
C18 C13 C14 Na3 126.7(3) . . . . ?
N3 C13 C14 Na3' -54.8(3) . . . . ?
C18 C13 C14 Na3' 123.4(3) . . . . ?
C13 C14 C15 C16 -0.1(6) . . . . ?
Na3 C14 C15 C16 -108.5(4) . . . . ?
Na3' C14 C15 C16 -86.5(5) . . . . ?
C14 C15 C16 C17 -0.6(6) . . . . ?
C15 C16 C17 C18 1.4(5) . . . . ?
C16 C17 C18 N4 179.5(3) . . . . ?
C16 C17 C18 C13 -1.5(5) . . . . ?
N3 C13 C18 N4 -1.4(3) . . . . ?
C14 C13 C18 N4 -179.9(3) . . . . ?
Na3' C13 C18 N4 -80.1(4) . . . . ?
N3 C13 C18 C17 179.4(3) . . . . ?
C14 C13 C18 C17 0.8(5) . . . . ?
Na3' C13 C18 C17 100.7(4) . . . . ?
O3 C19 C20 O4 -31.5(3) . . . . ?
C21 C19 C20 O4 -149.0(3) . . . . ?
C22 C19 C20 O4 85.7(3) . . . . ?
O3 C19 C20 C23 86.0(3) . . . . ?
C21 C19 C20 C23 -31.6(4) . . . . ?
C22 C19 C20 C23 -156.9(3) . . . . ?
O3 C19 C20 C24 -148.8(3) . . . . ?
C21 C19 C20 C24 93.7(4) . . . . ?
C22 C19 C20 C24 -31.6(4) . . . . ?
N1 B1 B2 O2 161.1(3) . . . . ?
N2 B1 B2 O2 -28.0(5) . . . . ?
Na1 B1 B2 O2 -137.1(3) . . . . ?
N1 B1 B2 O1 -84.0(3) . . . . ?
N2 B1 B2 O1 86.9(4) . . . . ?
Na1 B1 B2 O1 -22.1(2) . . . . ?
N1 B1 B2 N3 37.2(4) . . . . ?
N2 B1 B2 N3 -151.9(3) . . . . ?
Na1 B1 B2 N3 99.0(2) . . . . ?
N1 B1 B2 Na3' 108.7(3) . . . . ?
N2 B1 B2 Na3' -80.4(4) . . . . ?
Na1 B1 B2 Na3' 170.6(2) . . . . ?
N1 B1 B2 Na1 -61.8(3) . . . . ?
N2 B1 B2 Na1 109.1(3) . . . . ?
N1 B1 B2 Na3 119.8(3) . . . . ?
N2 B1 B2 Na3 -69.3(4) . . . . ?
Na1 B1 B2 Na3 -178.36(13) . . . . ?
N4 B3 B4 O3 -26.2(5) . . . . ?
N3 B3 B4 O3 154.3(3) . . . . ?
N4 B3 B4 O4 92.8(4) . . . . ?
N3 B3 B4 O4 -86.8(4) . . . . ?
N4 B3 B4 N1 -145.8(3) . . . . ?
N3 B3 B4 N1 34.7(4) . . . . ?
N4 B3 B4 Na2 -76.5(3) . . . . ?
N3 B3 B4 Na2 104.0(3) . . . . ?
N4 B3 B4 Na1 140.9(3) . . . . ?
N3 B3 B4 Na1 -38.7(3) . . . . ?
C5 C6 N1 B1 175.9(3) . . . . ?
C1 C6 N1 B1 -0.2(3) . . . . ?
Na2 C6 N1 B1 118.9(2) . . . . ?
C5 C6 N1 B4 -8.1(5) . . . . ?
C1 C6 N1 B4 175.8(3) . . . . ?
Na2 C6 N1 B4 -65.1(3) . . . . ?
C5 C6 N1 Na2 56.9(4) . . . . ?
C1 C6 N1 Na2 -119.2(2) . . . . ?
C5 C6 N1 Na1 -100.7(4) . . . . ?
C1 C6 N1 Na1 83.2(3) . . . . ?
Na2 C6 N1 Na1 -157.59(15) . . . . ?
N2 B1 N1 C6 0.7(3) . . . . ?
B2 B1 N1 C6 173.6(3) . . . . ?
Na1 B1 N1 C6 109.9(2) . . . . ?
N2 B1 N1 B4 -175.8(2) . . . . ?
B2 B1 N1 B4 -2.8(4) . . . . ?
Na1 B1 N1 B4 -66.5(2) . . . . ?
N2 B1 N1 Na2 93.5(2) . . . . ?
B2 B1 N1 Na2 -93.6(3) . . . . ?
Na1 B1 N1 Na2 -157.26(15) . . . . ?
N2 B1 N1 Na1 -109.3(2) . . . . ?
B2 B1 N1 Na1 63.7(3) . . . . ?
O3 B4 N1 C6 28.5(4) . . . . ?
O4 B4 N1 C6 -84.6(4) . . . . ?
B3 B4 N1 C6 154.5(3) . . . . ?
Na2 B4 N1 C6 68.4(3) . . . . ?
Na1 B4 N1 C6 -109.1(3) . . . . ?
O3 B4 N1 B1 -155.9(3) . . . . ?
O4 B4 N1 B1 91.0(3) . . . . ?
B3 B4 N1 B1 -29.9(4) . . . . ?
Na2 B4 N1 B1 -116.1(3) . . . . ?
Na1 B4 N1 B1 66.4(2) . . . . ?
O3 B4 N1 Na2 -39.8(2) . . . . ?
O4 B4 N1 Na2 -152.9(3) . . . . ?
B3 B4 N1 Na2 86.2(2) . . . . ?
Na1 B4 N1 Na2 -177.51(11) . . . . ?
O3 B4 N1 Na1 137.7(2) . . . . ?
O4 B4 N1 Na1 24.6(2) . . . . ?
B3 B4 N1 Na1 -96.3(2) . . . . ?
Na2 B4 N1 Na1 177.51(11) . . . . ?
C2 C1 N2 B1 -178.5(3) . . . . ?
C6 C1 N2 B1 0.7(3) . . . . ?
N1 B1 N2 C1 -0.8(3) . . . . ?
B2 B1 N2 C1 -173.0(3) . . . . ?
Na1 B1 N2 C1 -79.6(3) . . . . ?
C14 C13 N3 B3 179.6(4) . . . . ?
C18 C13 N3 B3 1.3(3) . . . . ?
Na3' C13 N3 B3 120.4(3) . . . . ?
C14 C13 N3 B2 -0.7(6) . . . . ?
C18 C13 N3 B2 -179.0(3) . . . . ?
Na3' C13 N3 B2 -59.9(4) . . . . ?
C14 C13 N3 Na3' 59.2(4) . . . . ?
C18 C13 N3 Na3' -119.1(3) . . . . ?
N4 B3 N3 C13 -0.8(3) . . . . ?
B4 B3 N3 C13 178.9(3) . . . . ?
N4 B3 N3 B2 179.5(3) . . . . ?
B4 B3 N3 B2 -0.8(4) . . . . ?
N4 B3 N3 Na3' 89.1(3) . . . . ?
B4 B3 N3 Na3' -91.2(3) . . . . ?
O2 B2 N3 C13 17.7(4) . . . . ?
O1 B2 N3 C13 -95.7(4) . . . . ?
B1 B2 N3 C13 147.8(3) . . . . ?
Na3' B2 N3 C13 62.0(4) . . . . ?
Na1 B2 N3 C13 -140.7(3) . . . . ?
Na3 B2 N3 C13 46.2(3) . . . . ?
O2 B2 N3 B3 -162.6(3) . . . . ?
O1 B2 N3 B3 83.9(4) . . . . ?
B1 B2 N3 B3 -32.6(4) . . . . ?
Na3' B2 N3 B3 -118.3(4) . . . . ?
Na1 B2 N3 B3 38.9(3) . . . . ?
Na3 B2 N3 B3 -134.1(3) . . . . ?
O2 B2 N3 Na3' -44.3(3) . . . . ?
O1 B2 N3 Na3' -157.8(4) . . . . ?
B1 B2 N3 Na3' 85.7(3) . . . . ?
Na1 B2 N3 Na3' 157.2(3) . . . . ?
C17 C18 N4 B3 -179.9(3) . . . . ?
C13 C18 N4 B3 0.9(3) . . . . ?
N3 B3 N4 C18 -0.1(3) . . . . ?
B4 B3 N4 C18 -179.7(3) . . . . ?
C9 C7 O1 B2 147.7(3) . . . . ?
C10 C7 O1 B2 -95.2(4) . . . . ?
C8 C7 O1 B2 25.9(3) . . . . ?
C9 C7 O1 Na1 -9.2(5) . . . . ?
C10 C7 O1 Na1 107.9(3) . . . . ?
C8 C7 O1 Na1 -131.0(3) . . . . ?
O2 B2 O1 C7 -7.3(3) . . . . ?
N3 B2 O1 C7 110.1(3) . . . . ?
B1 B2 O1 C7 -133.3(3) . . . . ?
Na3' B2 O1 C7 9.7(7) . . . . ?
Na1 B2 O1 C7 -164.0(3) . . . . ?
Na3 B2 O1 C7 7.5(4) . . . . ?
O2 B2 O1 Na1 156.69(17) . . . . ?
N3 B2 O1 Na1 -85.9(3) . . . . ?
B1 B2 O1 Na1 30.7(3) . . . . ?
Na3' B2 O1 Na1 173.7(5) . . . . ?
Na3 B2 O1 Na1 171.6(2) . . . . ?
C12 C8 O2 B2 154.2(3) . . . . ?
C11 C8 O2 B2 -87.8(4) . . . . ?
C7 C8 O2 B2 31.9(3) . . . . ?
C12 C8 O2 Na3 -28.9(4) . . . . ?
C11 C8 O2 Na3 89.1(4) . . . . ?
C7 C8 O2 Na3 -151.2(2) . . . . ?
C12 C8 O2 Na3' -51.8(9) . . . . ?
C11 C8 O2 Na3' 66.2(9) . . . . ?
C7 C8 O2 Na3' -174.1(7) . . . . ?
O1 B2 O2 C8 -16.3(3) . . . . ?
N3 B2 O2 C8 -136.7(3) . . . . ?
B1 B2 O2 C8 100.7(3) . . . . ?
Na3' B2 O2 C8 171.1(2) . . . . ?
Na1 B2 O2 C8 9.1(4) . . . . ?
Na3 B2 O2 C8 177.8(3) . . . . ?
O1 B2 O2 Na3 165.98(16) . . . . ?
N3 B2 O2 Na3 45.5(3) . . . . ?
B1 B2 O2 Na3 -77.1(3) . . . . ?
Na1 B2 O2 Na3 -168.6(2) . . . . ?
O1 B2 O2 Na3' 172.7(2) . . . . ?
N3 B2 O2 Na3' 52.2(2) . . . . ?
B1 B2 O2 Na3' -70.4(3) . . . . ?
Na1 B2 O2 Na3' -161.9(3) . . . . ?
C21 C19 O3 B4 155.9(3) . . . . ?
C22 C19 O3 B4 -86.5(3) . . . . ?
C20 C19 O3 B4 33.3(3) . . . . ?
C21 C19 O3 Na2 -46.5(6) . . . . ?
C22 C19 O3 Na2 71.1(6) . . . . ?
C20 C19 O3 Na2 -169.1(4) . . . . ?
O4 B4 O3 C19 -22.1(3) . . . . ?
N1 B4 O3 C19 -141.0(2) . . . . ?
B3 B4 O3 C19 101.0(3) . . . . ?
Na2 B4 O3 C19 171.6(2) . . . . ?
Na1 B4 O3 C19 -59.0(4) . . . . ?
O4 B4 O3 Na2 166.27(18) . . . . ?
N1 B4 O3 Na2 47.4(2) . . . . ?
B3 B4 O3 Na2 -70.7(2) . . . . ?
Na1 B4 O3 Na2 129.4(3) . . . . ?
C23 C20 O4 B4 -102.4(3) . . . . ?
C24 C20 O4 B4 140.0(3) . . . . ?
C19 C20 O4 B4 18.6(3) . . . . ?
C23 C20 O4 Na1 32.8(4) . . . . ?
C24 C20 O4 Na1 -84.8(4) . . . . ?
C19 C20 O4 Na1 153.7(2) . . . . ?
O3 B4 O4 C20 0.8(3) . . . . ?
N1 B4 O4 C20 116.6(3) . . . . ?
B3 B4 O4 C20 -126.3(3) . . . . ?
Na2 B4 O4 C20 27.8(6) . . . . ?
Na1 B4 O4 C20 149.0(3) . . . . ?
O3 B4 O4 Na1 -148.22(17) . . . . ?
N1 B4 O4 Na1 -32.5(3) . . . . ?
B3 B4 O4 Na1 84.7(2) . . . . ?
Na2 B4 O4 Na1 -121.2(4) . . . . ?
C33 O7 C33 C34 -20.5(13) 5_556 . . . ?
Na3 O7 C33 C34 159.5(13) . . . . ?
O7 C33 C34 C35 23(4) . . . . ?
C33 C34 C35 C33 -16(5) . . . 5_556 ?
C26 C25 O5 C28 -2.9(6) . . . . ?
C26 C25 O5 Na1 -168.6(4) . . . . ?
O5 C25 C26 C27 -16.4(8) . . . . ?
C25 C26 C27 C28 28.4(8) . . . . ?
C25 O5 C28 C27 20.8(6) . . . . ?
Na1 O5 C28 C27 -173.6(4) . . . . ?
C26 C27 C28 O5 -30.1(7) . . . . ?
C32 O6 C29 C30 12.0(14) . . . . ?
Na1 O6 C29 C30 -155.6(10) . . . . ?
O6 C29 C30 C31 -1.7(15) . . . . ?
C29 C30 C31 C32 -11(2) . . . . ?
C30 C31 C32 O6 19(2) . . . . ?
C29 O6 C32 C31 -20(2) . . . . ?
Na1 O6 C32 C31 147.3(15) . . . . ?
C32' O6' C29' C30' -15.7(17) . . . . ?
Na1 O6' C29' C30' 169.3(11) . . . . ?
O6' C29' C30' C31' 14(2) . . . . ?
C29' C30' C31' C32' -7(2) . . . . ?
C30' C31' C32' O6' -3(2) . . . . ?
C29' O6' C32' C31' 12(2) . . . . ?
Na1 O6' C32' C31' -171.9(14) . . . . ?

_refine_diff_density_max         0.293
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.053



####################################################################### 
# 
# 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_wo4ck
_database_code_depnum_ccdc_archive 'CCDC 2089033'
loop_
_audit_author_name
_audit_author_address
'Christian Kleeberg'
;Technische Universitaet Braunschweig, Institut fuer Anorganische und Analytische Chemie
Germany
;
_audit_update_record             
;
2021-06-09 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H146 B8 Li6 N8 O18'
_chemical_formula_sum            'C88 H146 B8 Li6 N8 O18'
_chemical_formula_weight         1732.24

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'
B B 0.0090 0.0039 '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      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                   27.2197(8)
_cell_length_b                   12.9528(5)
_cell_length_c                   33.2002(12)
_cell_angle_alpha                90
_cell_angle_beta                 103.948(3)
_cell_angle_gamma                90
_cell_volume                     11360.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12720
_cell_measurement_theta_min      3.79
_cell_measurement_theta_max      73.90

_exptl_crystal_description       'fragment of prism'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.013
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_recrystallization_method 
;
 From a solution in THF layered with n-pentane at -40 deg C.
;

_exptl_special_details           
;
 The crystal was mounted at rt with perfluoroether oil on top of a human hair
 and placed in a cold nitrogen gas stream on the diffractometer.

 The collected data cover more than a hemisphere of the reciprocal space.
 A combination of 21 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 1.5 deg in ω.
 Each frame was exposured for 5 s (low 2θ angles) or 20 s (high 2θ angles).
 Nominal crystal to detector distance 53 mm.
;




_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            52148
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.346
_diffrn_reflns_theta_max         66.997
_diffrn_reflns_theta_full        66.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10115
_reflns_number_gt                8512
_reflns_threshold_expression     'I > 2σ(I)'




_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
;


_computing_data_collection       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution    
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_molecular_graphics    
;
 K. Brandenburg, 2016, Diamond 4.2.2, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;



_refine_special_details          
;
 No appropriate model could be established for cocrystallised solvent molecules;
 the data were processed using the SQUEEZE/PLATON program (A. L. Spek, J. Appl.
 Crystallogr. 2003, 36, 7-13.).

 Two disordered THF moieties were refined using  split atom model (0.43(2)
 and 0.745(8) SOF  of main component).

 The N-H hydrogen atom was refined freely.
 All other H atoms were placed in idealised positions and refined using a 
 riding model, with a common U restrained to be 1.2 (1.5 for methyl groups) 
 times the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond but not tip.


 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;




_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0814P)²+8.1037P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10115
_refine_ls_number_parameters     654
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1602
_refine_ls_wR_factor_gt          0.1520
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
H2N H 0.5603(9) 0.517(2) 0.5650(8) 0.046(6) Uiso 1 1 d . . . . .
C1 C 0.47120(7) 0.40790(16) 0.59033(6) 0.0367(4) Uani 1 1 d . . . . .
C2 C 0.41901(7) 0.39888(18) 0.58517(7) 0.0424(5) Uani 1 1 d . . . . .
H2 H 0.4055 0.3543 0.6026 0.051 Uiso 1 1 calc R U . . .
C3 C 0.38686(8) 0.4562(2) 0.55412(7) 0.0516(6) Uani 1 1 d . . . . .
H3 H 0.3513 0.4507 0.5507 0.062 Uiso 1 1 calc R U . . .
C4 C 0.40552(9) 0.52104(19) 0.52818(7) 0.0504(5) Uani 1 1 d . . . . .
H4 H 0.3826 0.5583 0.5071 0.060 Uiso 1 1 calc R U . . .
C5 C 0.45741(8) 0.53224(17) 0.53267(6) 0.0439(5) Uani 1 1 d . . . . .
H5 H 0.4703 0.5766 0.5149 0.053 Uiso 1 1 calc R U . . .
C6 C 0.48982(7) 0.47651(16) 0.56399(6) 0.0378(4) Uani 1 1 d . . . . .
C7 C 0.69718(7) 0.41708(16) 0.63069(6) 0.0378(4) Uani 1 1 d . . . . .
C8 C 0.69344(7) 0.30304(16) 0.64398(6) 0.0375(4) Uani 1 1 d . . . . .
C9 C 0.68460(9) 0.42952(19) 0.58348(7) 0.0465(5) Uani 1 1 d . . . . .
H9A H 0.6519 0.3970 0.5713 0.070 Uiso 1 1 calc R U . . .
H9B H 0.7110 0.3964 0.5725 0.070 Uiso 1 1 calc R U . . .
H9C H 0.6829 0.5031 0.5764 0.070 Uiso 1 1 calc R U . . .
C10 C 0.74811(8) 0.46765(18) 0.64938(7) 0.0451(5) Uani 1 1 d . . . . .
H10A H 0.7479 0.5387 0.6391 0.068 Uiso 1 1 calc R U . . .
H10B H 0.7750 0.4285 0.6413 0.068 Uiso 1 1 calc R U . . .
H10C H 0.7542 0.4683 0.6797 0.068 Uiso 1 1 calc R U . . .
C11 C 0.71337(8) 0.22479(18) 0.61729(7) 0.0456(5) Uani 1 1 d . . . . .
H11A H 0.7108 0.1550 0.6280 0.068 Uiso 1 1 calc R U . . .
H11B H 0.7489 0.2401 0.6182 0.068 Uiso 1 1 calc R U . . .
H11C H 0.6933 0.2291 0.5886 0.068 Uiso 1 1 calc R U . . .
C12 C 0.72001(7) 0.28402(17) 0.68962(6) 0.0402(4) Uani 1 1 d . . . . .
H12A H 0.7087 0.3355 0.7070 0.060 Uiso 1 1 calc R U . . .
H12B H 0.7567 0.2897 0.6932 0.060 Uiso 1 1 calc R U . . .
H12C H 0.7116 0.2147 0.6977 0.060 Uiso 1 1 calc R U . . .
C13 C 0.62728(7) 0.43211(15) 0.72862(6) 0.0337(4) Uani 1 1 d . . . . .
C14 C 0.67028(7) 0.49380(17) 0.74132(6) 0.0399(4) Uani 1 1 d . . . . .
H14 H 0.6909 0.5085 0.7226 0.048 Uiso 1 1 calc R U . . .
C15 C 0.68295(8) 0.53388(18) 0.78151(7) 0.0445(5) Uani 1 1 d . . . . .
H15 H 0.7120 0.5767 0.7899 0.053 Uiso 1 1 calc R U . . .
C16 C 0.65356(8) 0.51185(18) 0.80947(7) 0.0444(5) Uani 1 1 d . . . . .
H16 H 0.6628 0.5394 0.8368 0.053 Uiso 1 1 calc R U . . .
C17 C 0.61073(8) 0.44968(17) 0.79765(6) 0.0407(4) Uani 1 1 d . . . . .
H17 H 0.5910 0.4346 0.8169 0.049 Uiso 1 1 calc R U . . .
C18 C 0.59670(7) 0.40930(15) 0.75730(6) 0.0343(4) Uani 1 1 d . . . . .
C19 C 0.48718(7) 0.11427(16) 0.62868(6) 0.0382(4) Uani 1 1 d . . . . .
C20 C 0.45219(8) 0.15336(17) 0.65658(6) 0.0397(4) Uani 1 1 d . . . . .
C21 C 0.46331(8) 0.12965(18) 0.58244(6) 0.0444(5) Uani 1 1 d . . . . .
H21A H 0.4524 0.2016 0.5774 0.067 Uiso 1 1 calc R U . . .
H21B H 0.4340 0.0839 0.5738 0.067 Uiso 1 1 calc R U . . .
H21C H 0.4883 0.1133 0.5665 0.067 Uiso 1 1 calc R U . . .
C22 C 0.50359(9) 0.00230(18) 0.63594(7) 0.0491(5) Uani 1 1 d . . . . .
H22A H 0.5241 -0.0171 0.6166 0.074 Uiso 1 1 calc R U . . .
H22B H 0.4736 -0.0421 0.6314 0.074 Uiso 1 1 calc R U . . .
H22C H 0.5236 -0.0061 0.6645 0.074 Uiso 1 1 calc R U . . .
C23 C 0.39549(8) 0.1405(2) 0.63756(7) 0.0494(5) Uani 1 1 d . . . . .
H23A H 0.3764 0.1695 0.6564 0.074 Uiso 1 1 calc R U . . .
H23B H 0.3875 0.0670 0.6332 0.074 Uiso 1 1 calc R U . . .
H23C H 0.3863 0.1768 0.6109 0.074 Uiso 1 1 calc R U . . .
C24 C 0.46506(9) 0.10342(19) 0.69958(7) 0.0475(5) Uani 1 1 d . . . . .
H24A H 0.5015 0.1093 0.7118 0.071 Uiso 1 1 calc R U . . .
H24B H 0.4554 0.0304 0.6971 0.071 Uiso 1 1 calc R U . . .
H24C H 0.4465 0.1386 0.7175 0.071 Uiso 1 1 calc R U . . .
C29 C 0.73779(8) 0.7181(2) 0.69711(7) 0.0490(5) Uani 1 1 d . . . . .
H29A H 0.7435 0.6493 0.7104 0.059 Uiso 1 1 calc R U . . .
H29B H 0.7270 0.7663 0.7165 0.059 Uiso 1 1 calc R U . . .
C30 C 0.78452(11) 0.7557(3) 0.68691(9) 0.0777(9) Uani 1 1 d . . . . .
H30A H 0.8019 0.8062 0.7079 0.093 Uiso 1 1 calc R U . . .
H30B H 0.8079 0.6975 0.6861 0.093 Uiso 1 1 calc R U . . .
C31 C 0.76889(11) 0.8045(3) 0.64605(9) 0.0812(10) Uani 1 1 d . . . . .
H31A H 0.7929 0.7870 0.6289 0.097 Uiso 1 1 calc R U . . .
H31B H 0.7679 0.8805 0.6489 0.097 Uiso 1 1 calc R U . . .
C32 C 0.71792(9) 0.7643(2) 0.62667(8) 0.0531(6) Uani 1 1 d . . . . .
H32A H 0.6950 0.8217 0.6148 0.064 Uiso 1 1 calc R U . . .
H32B H 0.7196 0.7156 0.6040 0.064 Uiso 1 1 calc R U . . .
C33 C 0.54022(9) 0.6141(2) 0.66988(10) 0.0633(7) Uani 1 1 d . . . . .
H33A H 0.5154 0.6527 0.6485 0.076 Uiso 0.437(18) 1 calc R U P A 1
H33B H 0.5385 0.5402 0.6620 0.076 Uiso 0.437(18) 1 calc R U P A 1
H33C H 0.5415 0.5396 0.6768 0.076 Uiso 0.563(18) 1 calc R U P A 2
H33D H 0.5193 0.6234 0.6413 0.076 Uiso 0.563(18) 1 calc R U P A 2
C34 C 0.5295(4) 0.6268(9) 0.7097(4) 0.073(3) Uani 0.437(18) 1 d . . P A 1
H34A H 0.5463 0.5730 0.7295 0.087 Uiso 0.437(18) 1 calc R U P A 1
H34B H 0.4927 0.6256 0.7077 0.087 Uiso 0.437(18) 1 calc R U P A 1
C35 C 0.5534(5) 0.7397(11) 0.7227(5) 0.073(3) Uani 0.437(18) 1 d . . P A 1
H35A H 0.5322 0.7959 0.7073 0.088 Uiso 0.437(18) 1 calc R U P A 1
H35B H 0.5598 0.7523 0.7529 0.088 Uiso 0.437(18) 1 calc R U P A 1
C34A C 0.5186(3) 0.6738(11) 0.6998(4) 0.083(3) Uani 0.563(18) 1 d . . P A 2
H34C H 0.4953 0.6312 0.7116 0.099 Uiso 0.563(18) 1 calc R U P A 2
H34D H 0.5007 0.7364 0.6869 0.099 Uiso 0.563(18) 1 calc R U P A 2
C35A C 0.5671(3) 0.7009(8) 0.7327(3) 0.0618(19) Uani 0.563(18) 1 d . . P A 2
H35C H 0.5617 0.7616 0.7493 0.074 Uiso 0.563(18) 1 calc R U P A 2
H35D H 0.5786 0.6419 0.7516 0.074 Uiso 0.563(18) 1 calc R U P A 2
C36 C 0.60300(10) 0.7236(2) 0.70824(9) 0.0608(6) Uani 1 1 d . . . . .
H36A H 0.6154 0.7902 0.6999 0.073 Uiso 0.437(18) 1 calc R U P A 1
H36B H 0.6296 0.6935 0.7309 0.073 Uiso 0.437(18) 1 calc R U P A 1
H36C H 0.5997 0.7962 0.6987 0.073 Uiso 0.563(18) 1 calc R U P A 2
H36D H 0.6381 0.7120 0.7247 0.073 Uiso 0.563(18) 1 calc R U P A 2
C37 C 0.57662(10) 0.2087(2) 0.54500(7) 0.0547(6) Uani 1 1 d . . . . .
H37A H 0.5894 0.2754 0.5580 0.066 Uiso 1 1 calc R U . . .
H37B H 0.5393 0.2125 0.5355 0.066 Uiso 1 1 calc R U . . .
C38 C 0.59929(15) 0.1859(3) 0.50967(10) 0.0833(9) Uani 1 1 d . . . . .
H38A H 0.6345 0.2116 0.5149 0.100 Uiso 1 1 calc R U . . .
H38B H 0.5790 0.2161 0.4835 0.100 Uiso 1 1 calc R U . . .
C39 C 0.5975(2) 0.0711(3) 0.50863(11) 0.1153(16) Uani 1 1 d . . . . .
H39A H 0.6236 0.0427 0.4955 0.138 Uiso 1 1 calc R U . . .
H39B H 0.5638 0.0463 0.4932 0.138 Uiso 1 1 calc R U . . .
C40 C 0.60790(17) 0.0406(2) 0.55373(11) 0.0858(10) Uani 1 1 d . . . . .
H40A H 0.5890 -0.0227 0.5571 0.103 Uiso 1 1 calc R U . . .
H40B H 0.6445 0.0278 0.5650 0.103 Uiso 1 1 calc R U . . .
C41 C 0.66474(8) -0.01313(18) 0.68504(7) 0.0456(5) Uani 1 1 d . . . . .
H41A H 0.6947 0.0021 0.6740 0.055 Uiso 1 1 calc R U . . .
H41B H 0.6474 -0.0747 0.6706 0.055 Uiso 1 1 calc R U . . .
C42 C 0.68058(9) -0.0317(2) 0.73153(7) 0.0527(6) Uani 1 1 d . . . . .
H42A H 0.6845 -0.1064 0.7379 0.063 Uiso 1 1 calc R U . . .
H42B H 0.7128 0.0040 0.7441 0.063 Uiso 1 1 calc R U . . .
C43 C 0.63702(9) 0.0136(2) 0.74680(7) 0.0517(5) Uani 1 1 d . . . . .
H43A H 0.6086 -0.0358 0.7434 0.062 Uiso 1 1 calc R U . . .
H43B H 0.6479 0.0345 0.7763 0.062 Uiso 1 1 calc R U . . .
C44 C 0.62298(9) 0.10503(19) 0.71898(7) 0.0491(5) Uani 1 1 d . . . . .
H44A H 0.5871 0.1240 0.7162 0.059 Uiso 1 1 calc R U . . .
H44B H 0.6445 0.1651 0.7300 0.059 Uiso 1 1 calc R U . . .
Li1 Li 0.64035(13) 0.6119(3) 0.64242(11) 0.0432(8) Uani 1 1 d . . . . .
Li2 Li 0.59852(13) 0.1677(3) 0.63363(10) 0.0405(7) Uani 1 1 d . . . . .
Li3 Li 0.47917(12) 0.3294(3) 0.71491(10) 0.0390(7) Uani 1 1 d . . . . .
B1 B 0.55801(8) 0.40915(18) 0.61245(7) 0.0350(4) Uani 1 1 d . . . . .
B2 B 0.61665(8) 0.38979(18) 0.64746(7) 0.0338(4) Uani 1 1 d . . . . .
B3 B 0.55914(8) 0.33607(17) 0.69664(7) 0.0323(4) Uani 1 1 d . . . . .
B4 B 0.51513(8) 0.28377(18) 0.65428(6) 0.0338(4) Uani 1 1 d . . . . .
N1 N 0.51172(6) 0.36448(13) 0.61856(5) 0.0344(3) Uani 1 1 d . . . . .
N2 N 0.54233(6) 0.47545(14) 0.57666(5) 0.0382(4) Uani 1 1 d . . . . .
N3 N 0.60486(5) 0.38712(12) 0.69096(5) 0.0325(3) Uani 1 1 d . . . . .
N4 N 0.55489(6) 0.34986(12) 0.73894(5) 0.0329(3) Uani 1 1 d . . . . .
O1 O 0.65812(5) 0.46734(10) 0.64581(4) 0.0349(3) Uani 1 1 d . . . . .
O2 O 0.64012(5) 0.28930(11) 0.63798(4) 0.0354(3) Uani 1 1 d . . . . .
O3 O 0.53065(5) 0.17898(11) 0.64134(4) 0.0348(3) Uani 1 1 d . . . . .
O4 O 0.46340(5) 0.26131(11) 0.66148(4) 0.0355(3) Uani 1 1 d . . . . .
O5 O 0.60676(19) 0.6872(4) 0.58915(16) 0.0415(9) Uani 0.745(8) 1 d . . P B 3
C25 C 0.57744(14) 0.7767(3) 0.59227(12) 0.0508(10) Uani 0.745(8) 1 d . . P B 3
H25A H 0.5987 0.8395 0.5959 0.061 Uiso 0.745(8) 1 calc R U P B 3
H25B H 0.5614 0.7707 0.6160 0.061 Uiso 0.745(8) 1 calc R U P B 3
C26 C 0.53751(13) 0.7800(3) 0.55129(12) 0.0514(10) Uani 0.745(8) 1 d . . P B 3
H26A H 0.5247 0.8510 0.5446 0.062 Uiso 0.745(8) 1 calc R U P B 3
H26B H 0.5088 0.7336 0.5518 0.062 Uiso 0.745(8) 1 calc R U P B 3
C27 C 0.5674(6) 0.7418(10) 0.5204(5) 0.053(2) Uani 0.745(8) 1 d . . P B 3
H27A H 0.5468 0.6934 0.5001 0.063 Uiso 0.745(8) 1 calc R U P B 3
H27B H 0.5779 0.8004 0.5053 0.063 Uiso 0.745(8) 1 calc R U P B 3
C28 C 0.61276(15) 0.6878(4) 0.54724(16) 0.0467(10) Uani 0.745(8) 1 d . . P B 3
H28A H 0.6149 0.6162 0.5374 0.056 Uiso 0.745(8) 1 calc R U P B 3
H28B H 0.6442 0.7246 0.5460 0.056 Uiso 0.745(8) 1 calc R U P B 3
O5A O 0.6161(7) 0.6697(15) 0.5785(5) 0.057(3) Uani 0.255(8) 1 d . . P B 4
C25A C 0.5705(6) 0.7334(11) 0.5714(5) 0.093(6) Uani 0.255(8) 1 d . . P B 4
H25C H 0.5762 0.7954 0.5893 0.111 Uiso 0.255(8) 1 calc R U P B 4
H25D H 0.5416 0.6939 0.5768 0.111 Uiso 0.255(8) 1 calc R U P B 4
C26A C 0.5611(18) 0.763(3) 0.5263(13) 0.076(13) Uani 0.255(8) 1 d . . P B 4
H26C H 0.5462 0.8327 0.5214 0.091 Uiso 0.255(8) 1 calc R U P B 4
H26D H 0.5382 0.7128 0.5085 0.091 Uiso 0.255(8) 1 calc R U P B 4
C27A C 0.6148(7) 0.7599(11) 0.5177(4) 0.095(6) Uani 0.255(8) 1 d . . P B 4
H27C H 0.6132 0.7498 0.4879 0.114 Uiso 0.255(8) 1 calc R U P B 4
H27D H 0.6343 0.8233 0.5276 0.114 Uiso 0.255(8) 1 calc R U P B 4
C28A C 0.6363(10) 0.6691(12) 0.5425(5) 0.077(5) Uani 0.255(8) 1 d . . P B 4
H28C H 0.6265 0.6049 0.5263 0.092 Uiso 0.255(8) 1 calc R U P B 4
H28D H 0.6737 0.6734 0.5506 0.092 Uiso 0.255(8) 1 calc R U P B 4
O6 O 0.69943(5) 0.71201(12) 0.65844(5) 0.0447(3) Uani 1 1 d . . . . .
O7 O 0.59096(6) 0.65405(13) 0.67338(5) 0.0517(4) Uani 1 1 d . . . . .
O8 O 0.59158(6) 0.12462(13) 0.57425(5) 0.0521(4) Uani 1 1 d . . . . .
O9 O 0.63132(6) 0.07291(12) 0.67925(5) 0.0478(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.383(2) . ?
C1 C2 1.394(3) . ?
C1 C6 1.423(3) . ?
C2 C3 1.395(3) . ?
C3 C4 1.384(4) . ?
C4 C5 1.392(3) . ?
C5 C6 1.392(3) . ?
C6 N2 1.389(3) . ?
C7 O1 1.437(2) . ?
C7 C10 1.524(3) . ?
C7 C9 1.530(3) . ?
C7 C8 1.552(3) . ?
C8 O2 1.428(2) . ?
C8 C11 1.529(3) . ?
C8 C12 1.534(3) . ?
C13 N3 1.381(2) . ?
C13 C14 1.396(3) . ?
C13 C18 1.438(3) . ?
C14 C15 1.395(3) . ?
C15 C16 1.393(3) . ?
C16 C17 1.393(3) . ?
C17 C18 1.403(3) . ?
C18 N4 1.387(2) . ?
C18 Li3 2.666(4) 2_656 ?
C19 O3 1.428(2) . ?
C19 C22 1.520(3) . ?
C19 C21 1.529(3) . ?
C19 C20 1.564(3) . ?
C20 O4 1.432(3) . ?
C20 C23 1.529(3) . ?
C20 C24 1.529(3) . ?
C29 O6 1.449(3) . ?
C29 C30 1.475(4) . ?
C30 C31 1.464(4) . ?
C31 C32 1.477(4) . ?
C32 O6 1.442(3) . ?
C33 C34 1.429(11) . ?
C33 O7 1.453(3) . ?
C33 C34A 1.488(8) . ?
C34 C35 1.617(18) . ?
C35 C36 1.553(12) . ?
C34A C35A 1.537(14) . ?
C35A C36 1.444(9) . ?
C36 O7 1.440(3) . ?
C37 O8 1.451(3) . ?
C37 C38 1.481(4) . ?
C38 C39 1.488(6) . ?
C39 C40 1.508(5) . ?
C40 O8 1.411(3) . ?
C41 O9 1.422(3) . ?
C41 C42 1.518(3) . ?
C42 C43 1.516(3) . ?
C43 C44 1.494(3) . ?
C44 O9 1.452(3) . ?
Li1 O1 1.930(4) . ?
Li1 O7 1.957(4) . ?
Li1 O5 2.034(7) . ?
Li1 O6 2.034(4) . ?
Li1 O5A 2.198(18) . ?
Li2 O2 1.925(4) . ?
Li2 O3 1.931(4) . ?
Li2 O9 1.986(4) . ?
Li2 O8 2.013(4) . ?
Li3 O4 1.934(3) . ?
Li3 N4 1.991(4) 2_656 ?
Li3 N4 2.040(3) . ?
Li3 Li3 2.333(6) 2_656 ?
Li3 B3 2.398(4) . ?
Li3 B4 2.512(4) . ?
Li3 C18 2.666(4) 2_656 ?
B1 N1 1.445(3) . ?
B1 N2 1.445(3) . ?
B1 B2 1.751(3) . ?
B2 O2 1.516(3) . ?
B2 O1 1.522(2) . ?
B2 N3 1.554(3) . ?
B3 N4 1.448(3) . ?
B3 N3 1.461(3) . ?
B3 B4 1.749(3) . ?
B4 O4 1.512(2) . ?
B4 O3 1.514(3) . ?
B4 N1 1.567(3) . ?
N4 Li3 1.991(4) 2_656 ?
O5 C25 1.425(6) . ?
O5 C28 1.439(5) . ?
C25 C26 1.523(5) . ?
C26 C27 1.535(12) . ?
C27 C28 1.510(16) . ?
O5A C28A 1.430(16) . ?
O5A C25A 1.46(2) . ?
C25A C26A 1.51(4) . ?
C26A C27A 1.56(5) . ?
C27A C28A 1.47(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 132.18(19) . . ?
N1 C1 C6 109.06(17) . . ?
C2 C1 C6 118.70(18) . . ?
C1 C2 C3 119.0(2) . . ?
C4 C3 C2 121.6(2) . . ?
C3 C4 C5 120.8(2) . . ?
C4 C5 C6 118.0(2) . . ?
N2 C6 C5 130.67(19) . . ?
N2 C6 C1 107.50(17) . . ?
C5 C6 C1 121.82(19) . . ?
O1 C7 C10 109.90(17) . . ?
O1 C7 C9 107.97(16) . . ?
C10 C7 C9 109.20(17) . . ?
O1 C7 C8 103.13(14) . . ?
C10 C7 C8 114.15(17) . . ?
C9 C7 C8 112.18(18) . . ?
O2 C8 C11 109.10(16) . . ?
O2 C8 C12 109.83(15) . . ?
C11 C8 C12 108.50(17) . . ?
O2 C8 C7 102.31(15) . . ?
C11 C8 C7 114.18(17) . . ?
C12 C8 C7 112.71(17) . . ?
N3 C13 C14 132.10(18) . . ?
N3 C13 C18 108.21(16) . . ?
C14 C13 C18 119.64(18) . . ?
C15 C14 C13 119.85(19) . . ?
C16 C15 C14 120.79(19) . . ?
C15 C16 C17 120.44(19) . . ?
C16 C17 C18 120.08(19) . . ?
N4 C18 C17 129.21(18) . . ?
N4 C18 C13 111.56(16) . . ?
C17 C18 C13 119.20(18) . . ?
N4 C18 Li3 46.74(11) . 2_656 ?
C17 C18 Li3 82.51(14) . 2_656 ?
C13 C18 Li3 158.30(16) . 2_656 ?
O3 C19 C22 108.80(17) . . ?
O3 C19 C21 109.90(16) . . ?
C22 C19 C21 108.73(18) . . ?
O3 C19 C20 102.43(15) . . ?
C22 C19 C20 114.38(17) . . ?
C21 C19 C20 112.36(17) . . ?
O4 C20 C23 108.65(18) . . ?
O4 C20 C24 108.19(16) . . ?
C23 C20 C24 108.71(18) . . ?
O4 C20 C19 103.88(15) . . ?
C23 C20 C19 114.72(17) . . ?
C24 C20 C19 112.38(18) . . ?
O6 C29 C30 106.95(19) . . ?
C31 C30 C29 106.3(2) . . ?
C30 C31 C32 106.5(2) . . ?
O6 C32 C31 107.7(2) . . ?
C34 C33 O7 106.7(5) . . ?
O7 C33 C34A 106.4(4) . . ?
C33 C34 C35 101.1(8) . . ?
C36 C35 C34 96.8(9) . . ?
C33 C34A C35A 100.6(7) . . ?
C36 C35A C34A 103.2(7) . . ?
O7 C36 C35A 105.7(4) . . ?
O7 C36 C35 106.6(5) . . ?
O8 C37 C38 106.1(2) . . ?
C37 C38 C39 101.5(3) . . ?
C38 C39 C40 103.9(3) . . ?
O8 C40 C39 105.8(3) . . ?
O9 C41 C42 106.11(17) . . ?
C43 C42 C41 103.01(18) . . ?
C44 C43 C42 101.8(2) . . ?
O9 C44 C43 105.17(18) . . ?
O1 Li1 O7 115.73(19) . . ?
O1 Li1 O5 124.7(2) . . ?
O7 Li1 O5 95.81(19) . . ?
O1 Li1 O6 115.60(18) . . ?
O7 Li1 O6 106.53(19) . . ?
O5 Li1 O6 94.8(2) . . ?
O1 Li1 O5A 113.6(5) . . ?
O7 Li1 O5A 109.2(5) . . ?
O6 Li1 O5A 94.0(5) . . ?
O2 Li2 O3 119.48(19) . . ?
O2 Li2 O9 107.47(17) . . ?
O3 Li2 O9 102.39(17) . . ?
O2 Li2 O8 102.39(17) . . ?
O3 Li2 O8 106.49(17) . . ?
O9 Li2 O8 119.64(19) . . ?
O4 Li3 N4 136.48(18) . 2_656 ?
O4 Li3 N4 113.45(17) . . ?
N4 Li3 N4 107.19(16) 2_656 . ?
O4 Li3 Li3 149.66(15) . 2_656 ?
N4 Li3 Li3 55.64(14) 2_656 2_656 ?
N4 Li3 Li3 53.65(13) . 2_656 ?
O4 Li3 B3 78.39(13) . . ?
N4 Li3 B3 144.04(17) 2_656 . ?
N4 Li3 B3 36.98(8) . . ?
Li3 Li3 B3 90.01(18) 2_656 . ?
O4 Li3 B4 36.97(8) . . ?
N4 Li3 B4 172.75(19) 2_656 . ?
N4 Li3 B4 77.99(12) . . ?
Li3 Li3 B4 127.7(2) 2_656 . ?
B3 Li3 B4 41.66(9) . . ?
O4 Li3 C18 118.38(15) . 2_656 ?
N4 Li3 C18 30.50(8) 2_656 2_656 ?
N4 Li3 C18 127.44(16) . 2_656 ?
Li3 Li3 C18 83.39(16) 2_656 2_656 ?
B3 Li3 C18 154.11(17) . 2_656 ?
B4 Li3 C18 148.52(15) . 2_656 ?
N1 B1 N2 105.00(16) . . ?
N1 B1 B2 122.38(17) . . ?
N2 B1 B2 132.25(18) . . ?
O2 B2 O1 101.88(14) . . ?
O2 B2 N3 111.45(16) . . ?
O1 B2 N3 111.68(16) . . ?
O2 B2 B1 110.32(16) . . ?
O1 B2 B1 116.54(16) . . ?
N3 B2 B1 105.12(15) . . ?
N4 B3 N3 109.81(16) . . ?
N4 B3 B4 128.93(17) . . ?
N3 B3 B4 120.74(16) . . ?
N4 B3 Li3 57.96(12) . . ?
N3 B3 Li3 154.48(17) . . ?
B4 B3 Li3 72.65(13) . . ?
O4 B4 O3 101.92(15) . . ?
O4 B4 N1 111.14(15) . . ?
O3 B4 N1 110.68(15) . . ?
O4 B4 B3 115.51(15) . . ?
O3 B4 B3 113.04(15) . . ?
N1 B4 B3 104.73(15) . . ?
O4 B4 Li3 50.27(11) . . ?
O3 B4 Li3 128.86(16) . . ?
N1 B4 Li3 119.09(16) . . ?
B3 B4 Li3 65.69(12) . . ?
C1 N1 B1 108.78(16) . . ?
C1 N1 B4 132.56(16) . . ?
B1 N1 B4 118.63(15) . . ?
C6 N2 B1 109.47(17) . . ?
C13 N3 B3 106.18(15) . . ?
C13 N3 B2 133.39(16) . . ?
B3 N3 B2 120.21(15) . . ?
C18 N4 B3 104.23(15) . . ?
C18 N4 Li3 102.75(15) . 2_656 ?
B3 N4 Li3 153.02(17) . 2_656 ?
C18 N4 Li3 152.67(17) . . ?
B3 N4 Li3 85.06(14) . . ?
Li3 N4 Li3 70.72(16) 2_656 . ?
C7 O1 B2 109.35(15) . . ?
C7 O1 Li1 127.97(16) . . ?
B2 O1 Li1 117.70(15) . . ?
C8 O2 B2 109.21(15) . . ?
C8 O2 Li2 132.24(16) . . ?
B2 O2 Li2 116.65(15) . . ?
C19 O3 B4 109.97(14) . . ?
C19 O3 Li2 131.90(16) . . ?
B4 O3 Li2 116.55(16) . . ?
C20 O4 B4 110.55(15) . . ?
C20 O4 Li3 122.92(16) . . ?
B4 O4 Li3 92.76(14) . . ?
C25 O5 C28 105.2(4) . . ?
C25 O5 Li1 118.0(3) . . ?
C28 O5 Li1 135.3(3) . . ?
O5 C25 C26 104.4(4) . . ?
C25 C26 C27 102.0(7) . . ?
C28 C27 C26 104.2(9) . . ?
O5 C28 C27 107.8(6) . . ?
C28A O5A C25A 110.5(15) . . ?
C28A O5A Li1 135.9(12) . . ?
C25A O5A Li1 113.2(10) . . ?
O5A C25A C26A 104(2) . . ?
C25A C26A C27A 104(3) . . ?
C28A C27A C26A 100(2) . . ?
O5A C28A C27A 106.4(16) . . ?
C32 O6 C29 108.58(17) . . ?
C32 O6 Li1 120.07(17) . . ?
C29 O6 Li1 128.46(17) . . ?
C36 O7 C33 108.35(19) . . ?
C36 O7 Li1 122.98(18) . . ?
C33 O7 Li1 128.22(19) . . ?
C40 O8 C37 109.0(2) . . ?
C40 O8 Li2 136.1(2) . . ?
C37 O8 Li2 113.11(17) . . ?
C41 O9 C44 109.68(16) . . ?
C41 O9 Li2 137.95(17) . . ?
C44 O9 Li2 112.07(16) . . ?

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 177.7(2) . . . . ?
C6 C1 C2 C3 0.8(3) . . . . ?
C1 C2 C3 C4 0.5(4) . . . . ?
C2 C3 C4 C5 -0.9(4) . . . . ?
C3 C4 C5 C6 -0.1(4) . . . . ?
C4 C5 C6 N2 -177.1(2) . . . . ?
C4 C5 C6 C1 1.4(3) . . . . ?
N1 C1 C6 N2 -0.6(2) . . . . ?
C2 C1 C6 N2 176.99(18) . . . . ?
N1 C1 C6 C5 -179.37(19) . . . . ?
C2 C1 C6 C5 -1.8(3) . . . . ?
O1 C7 C8 O2 37.35(18) . . . . ?
C10 C7 C8 O2 156.54(16) . . . . ?
C9 C7 C8 O2 -78.58(18) . . . . ?
O1 C7 C8 C11 155.07(16) . . . . ?
C10 C7 C8 C11 -85.7(2) . . . . ?
C9 C7 C8 C11 39.1(2) . . . . ?
O1 C7 C8 C12 -80.54(18) . . . . ?
C10 C7 C8 C12 38.6(2) . . . . ?
C9 C7 C8 C12 163.54(16) . . . . ?
N3 C13 C14 C15 176.6(2) . . . . ?
C18 C13 C14 C15 -0.8(3) . . . . ?
C13 C14 C15 C16 1.0(3) . . . . ?
C14 C15 C16 C17 -0.3(3) . . . . ?
C15 C16 C17 C18 -0.4(3) . . . . ?
C16 C17 C18 N4 -177.2(2) . . . . ?
C16 C17 C18 C13 0.6(3) . . . . ?
C16 C17 C18 Li3 -179.2(2) . . . 2_656 ?
N3 C13 C18 N4 0.3(2) . . . . ?
C14 C13 C18 N4 178.17(17) . . . . ?
N3 C13 C18 C17 -177.90(17) . . . . ?
C14 C13 C18 C17 0.0(3) . . . . ?
N3 C13 C18 Li3 1.5(5) . . . 2_656 ?
C14 C13 C18 Li3 179.5(3) . . . 2_656 ?
O3 C19 C20 O4 32.80(19) . . . . ?
C22 C19 C20 O4 150.33(17) . . . . ?
C21 C19 C20 O4 -85.09(19) . . . . ?
O3 C19 C20 C23 151.24(18) . . . . ?
C22 C19 C20 C23 -91.2(2) . . . . ?
C21 C19 C20 C23 33.4(3) . . . . ?
O3 C19 C20 C24 -83.92(19) . . . . ?
C22 C19 C20 C24 33.6(2) . . . . ?
C21 C19 C20 C24 158.20(18) . . . . ?
O6 C29 C30 C31 19.3(4) . . . . ?
C29 C30 C31 C32 -19.4(4) . . . . ?
C30 C31 C32 O6 12.4(4) . . . . ?
O7 C33 C34 C35 40.8(12) . . . . ?
C33 C34 C35 C36 -43.2(14) . . . . ?
O7 C33 C34A C35A -28.8(12) . . . . ?
C33 C34A C35A C36 39.1(14) . . . . ?
C34A C35A C36 O7 -35.2(11) . . . . ?
C34 C35 C36 O7 31.2(12) . . . . ?
O8 C37 C38 C39 33.2(4) . . . . ?
C37 C38 C39 C40 -36.1(4) . . . . ?
C38 C39 C40 O8 26.6(5) . . . . ?
O9 C41 C42 C43 25.2(3) . . . . ?
C41 C42 C43 C44 -36.4(2) . . . . ?
C42 C43 C44 O9 35.0(2) . . . . ?
N1 B1 B2 O2 84.6(2) . . . . ?
N2 B1 B2 O2 -103.5(2) . . . . ?
N1 B1 B2 O1 -159.95(18) . . . . ?
N2 B1 B2 O1 12.0(3) . . . . ?
N1 B1 B2 N3 -35.7(3) . . . . ?
N2 B1 B2 N3 136.2(2) . . . . ?
N4 B3 B4 O4 7.9(3) . . . . ?
N3 B3 B4 O4 -163.02(17) . . . . ?
Li3 B3 B4 O4 -6.93(17) . . . . ?
N4 B3 B4 O3 -109.0(2) . . . . ?
N3 B3 B4 O3 80.1(2) . . . . ?
Li3 B3 B4 O3 -123.77(17) . . . . ?
N4 B3 B4 N1 130.5(2) . . . . ?
N3 B3 B4 N1 -40.4(2) . . . . ?
Li3 B3 B4 N1 115.65(16) . . . . ?
N4 B3 B4 Li3 14.8(2) . . . . ?
N3 B3 B4 Li3 -156.1(2) . . . . ?
C2 C1 N1 B1 -173.9(2) . . . . ?
C6 C1 N1 B1 3.2(2) . . . . ?
C2 C1 N1 B4 3.8(4) . . . . ?
C6 C1 N1 B4 -179.05(19) . . . . ?
N2 B1 N1 C1 -4.4(2) . . . . ?
B2 B1 N1 C1 169.41(18) . . . . ?
N2 B1 N1 B4 177.44(16) . . . . ?
B2 B1 N1 B4 -8.7(3) . . . . ?
O4 B4 N1 C1 -8.7(3) . . . . ?
O3 B4 N1 C1 103.8(2) . . . . ?
B3 B4 N1 C1 -134.0(2) . . . . ?
Li3 B4 N1 C1 -64.0(3) . . . . ?
O4 B4 N1 B1 168.92(16) . . . . ?
O3 B4 N1 B1 -78.6(2) . . . . ?
B3 B4 N1 B1 43.5(2) . . . . ?
Li3 B4 N1 B1 113.61(19) . . . . ?
C5 C6 N2 B1 176.4(2) . . . . ?
C1 C6 N2 B1 -2.3(2) . . . . ?
N1 B1 N2 C6 4.1(2) . . . . ?
B2 B1 N2 C6 -168.8(2) . . . . ?
C14 C13 N3 B3 -177.1(2) . . . . ?
C18 C13 N3 B3 0.4(2) . . . . ?
C14 C13 N3 B2 -2.8(4) . . . . ?
C18 C13 N3 B2 174.78(18) . . . . ?
N4 B3 N3 C13 -0.9(2) . . . . ?
B4 B3 N3 C13 171.53(17) . . . . ?
Li3 B3 N3 C13 55.4(4) . . . . ?
N4 B3 N3 B2 -176.20(16) . . . . ?
B4 B3 N3 B2 -3.7(3) . . . . ?
Li3 B3 N3 B2 -119.8(4) . . . . ?
O2 B2 N3 C13 105.7(2) . . . . ?
O1 B2 N3 C13 -7.6(3) . . . . ?
B1 B2 N3 C13 -134.8(2) . . . . ?
O2 B2 N3 B3 -80.6(2) . . . . ?
O1 B2 N3 B3 166.17(16) . . . . ?
B1 B2 N3 B3 38.9(2) . . . . ?
C17 C18 N4 B3 177.1(2) . . . . ?
C13 C18 N4 B3 -0.8(2) . . . . ?
Li3 C18 N4 B3 179.8(2) 2_656 . . . ?
C17 C18 N4 Li3 -2.7(3) . . . 2_656 ?
C13 C18 N4 Li3 179.34(16) . . . 2_656 ?
C17 C18 N4 Li3 69.8(4) . . . . ?
C13 C18 N4 Li3 -108.1(3) . . . . ?
Li3 C18 N4 Li3 72.6(3) 2_656 . . . ?
N3 B3 N4 C18 1.1(2) . . . . ?
B4 B3 N4 C18 -170.61(19) . . . . ?
Li3 B3 N4 C18 -153.89(18) . . . . ?
N3 B3 N4 Li3 -179.3(3) . . . 2_656 ?
B4 B3 N4 Li3 9.1(5) . . . 2_656 ?
Li3 B3 N4 Li3 25.8(3) . . . 2_656 ?
N3 B3 N4 Li3 154.97(18) . . . . ?
B4 B3 N4 Li3 -16.7(2) . . . . ?
C10 C7 O1 B2 -149.75(16) . . . . ?
C9 C7 O1 B2 91.23(18) . . . . ?
C8 C7 O1 B2 -27.66(18) . . . . ?
C10 C7 O1 Li1 56.2(2) . . . . ?
C9 C7 O1 Li1 -62.8(2) . . . . ?
C8 C7 O1 Li1 178.31(17) . . . . ?
O2 B2 O1 C7 8.01(18) . . . . ?
N3 B2 O1 C7 127.07(16) . . . . ?
B1 B2 O1 C7 -112.11(18) . . . . ?
O2 B2 O1 Li1 165.05(16) . . . . ?
N3 B2 O1 Li1 -75.9(2) . . . . ?
B1 B2 O1 Li1 44.9(2) . . . . ?
C11 C8 O2 B2 -154.87(16) . . . . ?
C12 C8 O2 B2 86.33(19) . . . . ?
C7 C8 O2 B2 -33.59(18) . . . . ?
C11 C8 O2 Li2 41.8(3) . . . . ?
C12 C8 O2 Li2 -77.0(2) . . . . ?
C7 C8 O2 Li2 163.08(18) . . . . ?
O1 B2 O2 C8 17.16(18) . . . . ?
N3 B2 O2 C8 -102.06(17) . . . . ?
B1 B2 O2 C8 141.55(15) . . . . ?
O1 B2 O2 Li2 -176.58(15) . . . . ?
N3 B2 O2 Li2 64.2(2) . . . . ?
B1 B2 O2 Li2 -52.2(2) . . . . ?
C22 C19 O3 B4 -152.89(16) . . . . ?
C21 C19 O3 B4 88.17(19) . . . . ?
C20 C19 O3 B4 -31.45(19) . . . . ?
C22 C19 O3 Li2 42.3(3) . . . . ?
C21 C19 O3 Li2 -76.6(2) . . . . ?
C20 C19 O3 Li2 163.77(18) . . . . ?
O4 B4 O3 C19 18.15(18) . . . . ?
N1 B4 O3 C19 -100.12(17) . . . . ?
B3 B4 O3 C19 142.76(16) . . . . ?
Li3 B4 O3 C19 66.2(2) . . . . ?
O4 B4 O3 Li2 -174.47(15) . . . . ?
N1 B4 O3 Li2 67.3(2) . . . . ?
B3 B4 O3 Li2 -49.9(2) . . . . ?
Li3 B4 O3 Li2 -126.45(19) . . . . ?
C23 C20 O4 B4 -145.24(16) . . . . ?
C24 C20 O4 B4 96.90(18) . . . . ?
C19 C20 O4 B4 -22.70(19) . . . . ?
C23 C20 O4 Li3 107.1(2) . . . . ?
C24 C20 O4 Li3 -10.8(2) . . . . ?
C19 C20 O4 Li3 -130.39(17) . . . . ?
O3 B4 O4 C20 4.37(18) . . . . ?
N1 B4 O4 C20 122.31(17) . . . . ?
B3 B4 O4 C20 -118.59(18) . . . . ?
Li3 B4 O4 C20 -126.81(18) . . . . ?
O3 B4 O4 Li3 131.17(16) . . . . ?
N1 B4 O4 Li3 -110.89(18) . . . . ?
B3 B4 O4 Li3 8.2(2) . . . . ?
C28 O5 C25 C26 40.9(5) . . . . ?
Li1 O5 C25 C26 -150.9(3) . . . . ?
O5 C25 C26 C27 -36.8(7) . . . . ?
C25 C26 C27 C28 18.9(9) . . . . ?
C25 O5 C28 C27 -28.6(8) . . . . ?
Li1 O5 C28 C27 166.4(7) . . . . ?
C26 C27 C28 O5 4.8(10) . . . . ?
C28A O5A C25A C26A 6(3) . . . . ?
Li1 O5A C25A C26A -180(2) . . . . ?
O5A C25A C26A C27A -27(3) . . . . ?
C25A C26A C27A C28A 38(3) . . . . ?
C25A O5A C28A C27A 20(2) . . . . ?
Li1 O5A C28A C27A -153.2(15) . . . . ?
C26A C27A C28A O5A -35(2) . . . . ?
C31 C32 O6 C29 -0.4(3) . . . . ?
C31 C32 O6 Li1 -162.7(2) . . . . ?
C30 C29 O6 C32 -11.7(3) . . . . ?
C30 C29 O6 Li1 148.7(2) . . . . ?
C35A C36 O7 C33 17.3(5) . . . . ?
C35 C36 O7 C33 -9.1(8) . . . . ?
C35A C36 O7 Li1 -155.6(5) . . . . ?
C35 C36 O7 Li1 178.0(7) . . . . ?
C34 C33 O7 C36 -21.3(6) . . . . ?
C34A C33 O7 C36 8.5(7) . . . . ?
C34 C33 O7 Li1 151.2(5) . . . . ?
C34A C33 O7 Li1 -179.1(7) . . . . ?
C39 C40 O8 C37 -5.8(4) . . . . ?
C39 C40 O8 Li2 -168.8(3) . . . . ?
C38 C37 O8 C40 -17.5(3) . . . . ?
C38 C37 O8 Li2 149.8(2) . . . . ?
C42 C41 O9 C44 -3.4(2) . . . . ?
C42 C41 O9 Li2 169.4(2) . . . . ?
C43 C44 O9 C41 -20.2(2) . . . . ?
C43 C44 O9 Li2 164.98(18) . . . . ?

_refine_diff_density_max         0.377
_refine_diff_density_min         -0.415
_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_wo3wo
_database_code_depnum_ccdc_archive 'CCDC 2089032'
loop_
_audit_author_name
_audit_author_address
'Christian Kleeberg'
;Technische Universitaet Braunschweig, Institut fuer Anorganische und Analytische Chemie
Germany
;
_audit_update_record             
;
2021-06-09 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            WO_155
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H100 B4 Li6 N6 O8'
_chemical_formula_sum            'C58 H100 B4 Li6 N6 O8'
_chemical_formula_weight         1094.31

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'
B B 0.0090 0.0039 '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      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                   19.3963(12)
_cell_length_b                   16.7860(8)
_cell_length_c                   22.9634(14)
_cell_angle_alpha                90
_cell_angle_beta                 101.073(6)
_cell_angle_gamma                90
_cell_volume                     7337.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.3(2)
_cell_measurement_reflns_used    10910
_cell_measurement_theta_min      3.4720
_cell_measurement_theta_max      75.9570

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.991
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_min  0.87740
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_recrystallization_method 
;
 From a solution in THF/Et2O solution at room temperature.
;

_exptl_special_details           
;
 The crystal was mounted at rt with perfluoroether oil on top of a human hair
 and placed in a cold nitrogen gas stream on the diffractometer.

 The collected data cover more than a hemisphere of the reciprocal space.
 A combination of 30 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 1.5 deg in ω.
 Each frame was exposured for 3 s (low 2θ angles) or 9 s (high 2θ angles).
 Nominal crystal to detector distance 53 mm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            61863
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.511
_diffrn_reflns_theta_max         76.211
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7623
_reflns_number_gt                5796
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000


_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 Structure factors included contributions from the .fab file.

;

_computing_data_collection       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution    
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_molecular_graphics    
;
 K. Brandenburg, 2016, Diamond 4.2.2, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;



_refine_special_details          
;
 
 No appropriate model could be established for two sites of cocrystallised 
 THF/Et2O molecules; the data were processed using the SQUEEZE/PLATON 
 program (A. L. Spek, J. Appl. Crystallogr. 2003, 36, 7-13.).

 A disordered TMP moiety was refined using a split atom model (0.873(2) SOF
 of main component), applying similarity restraints on the C-CH3 distances 
 (SADI). A common ADP was refined for each disordered atom pair (EADP).

 All H atoms were placed in idealised positions and refined using a 
 riding model, with a common U restrained to be 1.2 (1.5 for methyl groups) 
 times the equivalent isotropic displacement parameter of the parent atom.
 Non-disorderd methyl groups were treated as a rigid bodies and allowed to 
 rotate about the E-CH3 bond but not tip.


 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0777P)²+1.8885P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7623
_refine_ls_number_parameters     402
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1497
_refine_ls_wR_factor_gt          0.1360
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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 0.36609(7) 0.79211(9) 0.31016(7) 0.0255(3) Uani 1 1 d . . . . .
C2 C 0.64408(7) 0.82492(8) 0.24838(7) 0.0229(3) Uani 1 1 d . . . . .
C3 C 0.70851(8) 0.81774(9) 0.28717(8) 0.0274(3) Uani 1 1 d . . . . .
H3 H 0.7147 0.8378 0.3265 0.033 Uiso 1 1 calc R U . . .
C4 C 0.76402(8) 0.78034(10) 0.26689(9) 0.0333(4) Uani 1 1 d . . . . .
H4 H 0.8085 0.7758 0.2926 0.040 Uiso 1 1 calc R U . . .
C5 C 0.75506(8) 0.74976(11) 0.20972(9) 0.0366(4) Uani 1 1 d . . . . .
H5 H 0.7935 0.7249 0.1968 0.044 Uiso 1 1 calc R U . . .
C6 C 0.30986(8) 0.75504(10) 0.32917(8) 0.0329(4) Uani 1 1 d . . . . .
H6 H 0.3156 0.7336 0.3681 0.039 Uiso 1 1 calc R U . . .
C7 C 0.61053(8) 0.95460(9) 0.39990(7) 0.0267(3) Uani 1 1 d . . . . .
C8 C 0.60174(8) 1.01788(9) 0.34966(7) 0.0264(3) Uani 1 1 d . . . . .
C9 C 0.68363(9) 0.95214(11) 0.43883(8) 0.0355(4) Uani 1 1 d . . . . .
H9A H 0.6850 0.9110 0.4693 0.053 Uiso 1 1 calc R U . . .
H9B H 0.6945 1.0041 0.4579 0.053 Uiso 1 1 calc R U . . .
H9C H 0.7184 0.9397 0.4143 0.053 Uiso 1 1 calc R U . . .
C10 C 0.55581(10) 0.96388(11) 0.43930(8) 0.0355(4) Uani 1 1 d . . . . .
H10A H 0.5087 0.9655 0.4145 0.053 Uiso 1 1 calc R U . . .
H10B H 0.5645 1.0135 0.4620 0.053 Uiso 1 1 calc R U . . .
H10C H 0.5591 0.9186 0.4667 0.053 Uiso 1 1 calc R U . . .
C11 C 0.66779(8) 1.02760(10) 0.32327(8) 0.0312(3) Uani 1 1 d . . . . .
H11A H 0.6837 0.9752 0.3125 0.047 Uiso 1 1 calc R U . . .
H11B H 0.7048 1.0527 0.3526 0.047 Uiso 1 1 calc R U . . .
H11C H 0.6572 1.0612 0.2878 0.047 Uiso 1 1 calc R U . . .
C12 C 0.57833(9) 1.09959(10) 0.36694(9) 0.0356(4) Uani 1 1 d . . . . .
H12A H 0.5729 1.1353 0.3326 0.053 Uiso 1 1 calc R U . . .
H12B H 0.6137 1.1213 0.3993 0.053 Uiso 1 1 calc R U . . .
H12C H 0.5333 1.0947 0.3800 0.053 Uiso 1 1 calc R U . . .
C13 C 0.52779(9) 0.70339(9) 0.50262(7) 0.0294(3) Uani 1 1 d D . . . .
C14 C 0.59650(12) 0.72720(14) 0.54668(9) 0.0370(5) Uani 0.873(2) 1 d . . P A 1
H14A H 0.6076 0.7837 0.5402 0.044 Uiso 0.873(2) 1 calc R U P A 1
H14B H 0.5890 0.7217 0.5879 0.044 Uiso 0.873(2) 1 calc R U P A 1
C15 C 0.65863(11) 0.67488(15) 0.53829(10) 0.0433(5) Uani 0.873(2) 1 d . . P A 1
H15A H 0.7021 0.6940 0.5645 0.052 Uiso 0.873(2) 1 calc R U P A 1
H15B H 0.6503 0.6192 0.5494 0.052 Uiso 0.873(2) 1 calc R U P A 1
C16 C 0.66756(11) 0.67783(16) 0.47405(12) 0.0364(5) Uani 0.873(2) 1 d . . P A 1
H16A H 0.7053 0.6405 0.4686 0.044 Uiso 0.873(2) 1 calc R U P A 1
H16B H 0.6821 0.7322 0.4648 0.044 Uiso 0.873(2) 1 calc R U P A 1
C18 C 0.49795(13) 0.62751(13) 0.52545(10) 0.0391(5) Uani 0.873(2) 1 d D . P A 1
H18A H 0.4928 0.6354 0.5667 0.059 Uiso 0.873(2) 1 calc R U P A 1
H18B H 0.4520 0.6157 0.5009 0.059 Uiso 0.873(2) 1 calc R U P A 1
H18C H 0.5300 0.5829 0.5234 0.059 Uiso 0.873(2) 1 calc R U P A 1
C19 C 0.47395(11) 0.76959(12) 0.50706(10) 0.0365(4) Uani 0.873(2) 1 d D . P A 1
H19A H 0.4652 0.7718 0.5477 0.055 Uiso 0.873(2) 1 calc R U P A 1
H19B H 0.4925 0.8209 0.4968 0.055 Uiso 0.873(2) 1 calc R U P A 1
H19C H 0.4299 0.7581 0.4795 0.055 Uiso 0.873(2) 1 calc R U P A 1
C20 C 0.58997(13) 0.56310(12) 0.43321(12) 0.0368(5) Uani 0.873(2) 1 d D . P A 1
H20A H 0.6325 0.5364 0.4260 0.055 Uiso 0.873(2) 1 calc R U P A 1
H20B H 0.5812 0.5478 0.4723 0.055 Uiso 0.873(2) 1 calc R U P A 1
H20C H 0.5498 0.5473 0.4026 0.055 Uiso 0.873(2) 1 calc R U P A 1
C21 C 0.6083(8) 0.6728(10) 0.3674(2) 0.0354(9) Uani 0.873(2) 1 d D . P A 1
H21A H 0.6485 0.6430 0.3587 0.053 Uiso 0.873(2) 1 calc R U P A 1
H21B H 0.5655 0.6564 0.3400 0.053 Uiso 0.873(2) 1 calc R U P A 1
H21C H 0.6160 0.7300 0.3627 0.053 Uiso 0.873(2) 1 calc R U P A 1
C14' C 0.5323(9) 0.6067(10) 0.5215(7) 0.0370(5) Uani 0.127(2) 1 d . . P A 2
H14C H 0.5248 0.6004 0.5627 0.044 Uiso 0.127(2) 1 calc R U P A 2
H14D H 0.4952 0.5765 0.4948 0.044 Uiso 0.127(2) 1 calc R U P A 2
C15' C 0.6037(8) 0.5748(10) 0.5165(7) 0.0433(5) Uani 0.127(2) 1 d . . P A 2
H15C H 0.6405 0.6047 0.5436 0.052 Uiso 0.127(2) 1 calc R U P A 2
H15D H 0.6071 0.5181 0.5285 0.052 Uiso 0.127(2) 1 calc R U P A 2
C16' C 0.6155(8) 0.5823(10) 0.4547(8) 0.0364(5) Uani 0.127(2) 1 d . . P A 2
H16C H 0.6653 0.5700 0.4542 0.044 Uiso 0.127(2) 1 calc R U P A 2
H16D H 0.5862 0.5425 0.4295 0.044 Uiso 0.127(2) 1 calc R U P A 2
C18' C 0.5686(9) 0.7529(9) 0.5531(5) 0.0391(5) Uani 0.127(2) 1 d D . P A 2
H18D H 0.5505 0.7424 0.5894 0.059 Uiso 0.127(2) 1 calc R U P A 2
H18E H 0.6184 0.7386 0.5594 0.059 Uiso 0.127(2) 1 calc R U P A 2
H18F H 0.5630 0.8096 0.5431 0.059 Uiso 0.127(2) 1 calc R U P A 2
C19' C 0.4477(3) 0.7183(9) 0.4900(6) 0.0365(4) Uani 0.127(2) 1 d D . P A 2
H19D H 0.4309 0.7207 0.5276 0.055 Uiso 0.127(2) 1 calc R U P A 2
H19E H 0.4375 0.7688 0.4687 0.055 Uiso 0.127(2) 1 calc R U P A 2
H19F H 0.4239 0.6748 0.4657 0.055 Uiso 0.127(2) 1 calc R U P A 2
C20' C 0.6669(6) 0.7086(9) 0.4554(8) 0.053(6) Uani 0.127(2) 1 d D . P A 2
H20D H 0.6591 0.7629 0.4398 0.079 Uiso 0.127(2) 1 calc R U P A 2
H20E H 0.6750 0.7099 0.4988 0.079 Uiso 0.127(2) 1 calc R U P A 2
H20F H 0.7080 0.6857 0.4426 0.079 Uiso 0.127(2) 1 calc R U P A 2
C21' C 0.604(6) 0.670(7) 0.3661(15) 0.0354(9) Uani 0.127(2) 1 d D . P A 2
H21D H 0.5917 0.7258 0.3557 0.053 Uiso 0.127(2) 1 calc R U P A 2
H21E H 0.6519 0.6597 0.3602 0.053 Uiso 0.127(2) 1 calc R U P A 2
H21F H 0.5712 0.6347 0.3408 0.053 Uiso 0.127(2) 1 calc R U P A 2
C17 C 0.60019(8) 0.65590(10) 0.43112(7) 0.0293(3) Uani 1 1 d D . . . .
C22 C 0.38108(12) 0.53683(13) 0.37169(11) 0.0525(6) Uani 1 1 d . . . . .
H22A H 0.3401 0.5575 0.3869 0.063 Uiso 1 1 calc R U . . .
H22B H 0.4155 0.5149 0.4053 0.063 Uiso 1 1 calc R U . . .
C23 C 0.35867(14) 0.47439(13) 0.32559(12) 0.0607(6) Uani 1 1 d . . . . .
H23A H 0.3182 0.4435 0.3338 0.073 Uiso 1 1 calc R U . . .
H23B H 0.3977 0.4375 0.3226 0.073 Uiso 1 1 calc R U . . .
C24 C 0.33867(12) 0.52412(14) 0.27048(10) 0.0537(5) Uani 1 1 d . . . . .
H24A H 0.2909 0.5466 0.2674 0.064 Uiso 1 1 calc R U . . .
H24B H 0.3403 0.4923 0.2345 0.064 Uiso 1 1 calc R U . . .
C25 C 0.39399(11) 0.58997(13) 0.27871(9) 0.0471(5) Uani 1 1 d . . . . .
H25A H 0.4352 0.5740 0.2619 0.056 Uiso 1 1 calc R U . . .
H25B H 0.3744 0.6399 0.2594 0.056 Uiso 1 1 calc R U . . .
C26 C 0.33411(10) 0.97741(11) 0.34839(9) 0.0382(4) Uani 1 1 d . . . . .
H26A H 0.3574 0.9324 0.3723 0.046 Uiso 1 1 calc R U . . .
H26B H 0.3008 0.9558 0.3138 0.046 Uiso 1 1 calc R U . . .
C27 C 0.29621(12) 1.03058(14) 0.38559(10) 0.0489(5) Uani 1 1 d . . . . .
H27A H 0.2464 1.0148 0.3817 0.059 Uiso 1 1 calc R U . . .
H27B H 0.3191 1.0288 0.4280 0.059 Uiso 1 1 calc R U . . .
C28 C 0.30267(9) 1.11244(12) 0.35942(10) 0.0438(5) Uani 1 1 d . . . . .
H28A H 0.2665 1.1208 0.3232 0.053 Uiso 1 1 calc R U . . .
H28B H 0.2985 1.1549 0.3885 0.053 Uiso 1 1 calc R U . . .
C29 C 0.37549(11) 1.11035(12) 0.34525(11) 0.0481(5) Uani 1 1 d . . . . .
H29A H 0.3788 1.1468 0.3120 0.058 Uiso 1 1 calc R U . . .
H29B H 0.4111 1.1262 0.3803 0.058 Uiso 1 1 calc R U . . .
Li1 Li 0.53084(14) 0.80530(16) 0.39722(13) 0.0286(5) Uani 1 1 d . . . . .
Li2 Li 0.44541(14) 0.98852(16) 0.27958(13) 0.0288(5) Uani 1 1 d . . . . .
Li3 Li 0.45431(15) 0.69448(16) 0.37935(13) 0.0323(6) Uani 1 1 d . . . . .
B1 B 0.46790(8) 0.84847(9) 0.30106(8) 0.0223(3) Uani 1 1 d . . . . .
B2 B 0.55200(8) 0.89074(9) 0.30976(8) 0.0216(3) Uani 1 1 d . . . . .
N1 N 0.43475(6) 0.80378(7) 0.34154(6) 0.0252(3) Uani 1 1 d . . . . .
N2 N 0.58157(6) 0.86156(7) 0.25518(6) 0.0222(3) Uani 1 1 d . . . . .
N3 N 0.53899(6) 0.70237(7) 0.44145(6) 0.0247(3) Uani 1 1 d . . . . .
O1 O 0.59863(5) 0.87981(6) 0.36866(5) 0.0240(2) Uani 1 1 d . . . . .
O2 O 0.54673(5) 0.98397(6) 0.30536(5) 0.0236(2) Uani 1 1 d . . . . .
O3 O 0.41287(7) 0.59973(7) 0.34203(6) 0.0405(3) Uani 1 1 d . . . . .
O4 O 0.38585(6) 1.02884(7) 0.32907(6) 0.0341(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.397(2) . ?
C1 N1 1.4009(19) . ?
C1 C2 1.431(2) 2_655 ?
C1 Li3 2.663(3) . ?
C2 C3 1.394(2) . ?
C2 N2 1.3948(18) . ?
C2 C1 1.431(2) 2_655 ?
C3 C4 1.401(2) . ?
C4 C5 1.389(3) . ?
C5 C6 1.400(2) 2_655 ?
C6 C5 1.400(2) 2_655 ?
C7 O1 1.4423(18) . ?
C7 C9 1.525(2) . ?
C7 C10 1.529(2) . ?
C7 C8 1.553(2) . ?
C8 O2 1.4423(18) . ?
C8 C12 1.521(2) . ?
C8 C11 1.528(2) . ?
C13 N3 1.462(2) . ?
C13 C18' 1.519(5) . ?
C13 C18 1.532(2) . ?
C13 C19 1.542(2) . ?
C13 C19' 1.545(5) . ?
C13 C14 1.563(3) . ?
C13 C14' 1.677(16) . ?
C14 C15 1.533(3) . ?
C15 C16 1.519(4) . ?
C16 C17 1.523(3) . ?
C20 C17 1.572(2) . ?
C21 C17 1.528(3) . ?
C14' C15' 1.51(2) . ?
C15' C16' 1.48(2) . ?
C16' C17 1.359(16) . ?
C20' C17 1.578(6) . ?
C21' C17 1.528(5) . ?
C17 N3 1.4772(19) . ?
C22 O3 1.456(2) . ?
C22 C23 1.494(3) . ?
C23 C24 1.503(3) . ?
C24 C25 1.527(3) . ?
C25 O3 1.439(2) . ?
C26 O4 1.456(2) . ?
C26 C27 1.519(2) . ?
C27 C28 1.515(3) . ?
C28 C29 1.510(3) . ?
C29 O4 1.442(2) . ?
Li1 N3 1.995(3) . ?
Li1 O1 2.014(3) . ?
Li1 N1 2.048(3) . ?
Li1 Li3 2.366(4) . ?
Li1 B1 2.420(3) . ?
Li1 B2 2.564(3) . ?
Li2 O4 1.894(3) . ?
Li2 O2 1.942(3) . ?
Li2 O2 1.987(3) 2_655 ?
Li2 N2 2.300(3) 2_655 ?
Li2 B1 2.424(3) . ?
Li2 B2 2.626(3) . ?
Li2 B2 2.635(3) 2_655 ?
Li2 Li2 2.727(5) 2_655 ?
Li3 O3 1.909(3) . ?
Li3 N3 1.962(3) . ?
Li3 N1 2.034(3) . ?
B1 N1 1.439(2) . ?
B1 N2 1.470(2) 2_655 ?
B1 B2 1.755(2) . ?
B2 O1 1.4870(19) . ?
B2 N2 1.554(2) . ?
B2 O2 1.5703(18) . ?
B2 Li2 2.635(3) 2_655 ?
N2 B1 1.470(2) 2_655 ?
N2 Li2 2.300(3) 2_655 ?
O2 Li2 1.987(3) 2_655 ?

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
C6 C1 N1 128.60(15) . . ?
C6 C1 C2 119.35(14) . 2_655 ?
N1 C1 C2 112.04(13) . 2_655 ?
C6 C1 Li3 89.44(12) . . ?
N1 C1 Li3 48.77(9) . . ?
C2 C1 Li3 138.96(12) 2_655 . ?
C3 C2 N2 131.20(15) . . ?
C3 C2 C1 120.81(14) . 2_655 ?
N2 C2 C1 107.99(13) . 2_655 ?
C2 C3 C4 118.57(15) . . ?
C5 C4 C3 121.01(15) . . ?
C4 C5 C6 120.89(15) . 2_655 ?
C1 C6 C5 119.32(16) . 2_655 ?
O1 C7 C9 108.06(13) . . ?
O1 C7 C10 108.67(12) . . ?
C9 C7 C10 109.20(14) . . ?
O1 C7 C8 103.98(12) . . ?
C9 C7 C8 114.28(13) . . ?
C10 C7 C8 112.34(13) . . ?
O2 C8 C12 108.80(13) . . ?
O2 C8 C11 108.99(13) . . ?
C12 C8 C11 108.80(13) . . ?
O2 C8 C7 102.41(11) . . ?
C12 C8 C7 114.74(14) . . ?
C11 C8 C7 112.76(13) . . ?
N3 C13 C18' 126.0(6) . . ?
N3 C13 C18 117.04(15) . . ?
N3 C13 C19 107.43(14) . . ?
C18 C13 C19 105.75(16) . . ?
N3 C13 C19' 98.7(6) . . ?
C18' C13 C19' 114.3(9) . . ?
N3 C13 C14 111.05(14) . . ?
C18 C13 C14 108.80(16) . . ?
C19 C13 C14 106.09(16) . . ?
N3 C13 C14' 103.1(6) . . ?
C18' C13 C14' 109.8(8) . . ?
C19' C13 C14' 101.8(8) . . ?
C15 C14 C13 111.43(17) . . ?
C16 C15 C14 110.03(18) . . ?
C15 C16 C17 112.15(18) . . ?
C15' C14' C13 109.0(12) . . ?
C16' C15' C14' 110.8(12) . . ?
C17 C16' C15' 113.4(13) . . ?
C16' C17 N3 122.5(7) . . ?
N3 C17 C16 112.61(16) . . ?
N3 C17 C21 106.8(6) . . ?
C16 C17 C21 110.0(6) . . ?
C16' C17 C21' 119(4) . . ?
N3 C17 C21' 105(4) . . ?
N3 C17 C20 114.10(14) . . ?
C16 C17 C20 108.49(17) . . ?
C21 C17 C20 104.5(6) . . ?
C16' C17 C20' 105.5(9) . . ?
N3 C17 C20' 106.1(6) . . ?
C21' C17 C20' 94(4) . . ?
O3 C22 C23 105.6(2) . . ?
C22 C23 C24 101.53(18) . . ?
C23 C24 C25 103.66(17) . . ?
O3 C25 C24 104.12(17) . . ?
O4 C26 C27 105.03(15) . . ?
C28 C27 C26 102.95(16) . . ?
C29 C28 C27 102.51(16) . . ?
O4 C29 C28 105.07(16) . . ?
N3 Li1 O1 135.30(15) . . ?
N3 Li1 N1 106.30(13) . . ?
O1 Li1 N1 112.16(13) . . ?
N3 Li1 Li3 52.64(10) . . ?
O1 Li1 Li3 149.21(17) . . ?
N1 Li1 Li3 54.30(10) . . ?
N3 Li1 B1 134.48(14) . . ?
O1 Li1 B1 76.31(10) . . ?
N1 Li1 B1 36.37(7) . . ?
Li3 Li1 B1 83.54(12) . . ?
N3 Li1 B2 150.94(15) . . ?
O1 Li1 B2 35.39(6) . . ?
N1 Li1 B2 77.37(10) . . ?
Li3 Li1 B2 119.56(14) . . ?
B1 Li1 B2 41.10(7) . . ?
O4 Li2 O2 121.95(15) . . ?
O4 Li2 O2 140.65(16) . 2_655 ?
O2 Li2 O2 91.94(12) . 2_655 ?
O4 Li2 N2 114.51(14) . 2_655 ?
O2 Li2 N2 102.64(12) . 2_655 ?
O2 Li2 N2 71.29(10) 2_655 2_655 ?
O4 Li2 B1 109.33(13) . . ?
O2 Li2 B1 76.58(10) . . ?
O2 Li2 B1 96.77(11) 2_655 . ?
N2 Li2 B1 36.13(6) 2_655 . ?
O4 Li2 B2 127.21(14) . . ?
O2 Li2 B2 36.47(6) . . ?
O2 Li2 B2 91.73(11) 2_655 . ?
N2 Li2 B2 68.14(8) 2_655 . ?
B1 Li2 B2 40.41(6) . . ?
O4 Li2 B2 142.61(14) . 2_655 ?
O2 Li2 B2 92.49(11) . 2_655 ?
O2 Li2 B2 36.42(6) 2_655 2_655 ?
N2 Li2 B2 35.91(6) 2_655 2_655 ?
B1 Li2 B2 61.63(8) . 2_655 ?
B2 Li2 B2 71.61(9) . 2_655 ?
O4 Li2 Li2 156.98(12) . 2_655 ?
O2 Li2 Li2 46.73(9) . 2_655 ?
O2 Li2 Li2 45.38(9) 2_655 2_655 ?
N2 Li2 Li2 88.50(9) 2_655 2_655 ?
B1 Li2 Li2 88.55(8) . 2_655 ?
B2 Li2 Li2 58.95(9) . 2_655 ?
B2 Li2 Li2 58.63(9) 2_655 2_655 ?
O3 Li3 N3 127.15(16) . . ?
O3 Li3 N1 122.13(16) . . ?
N3 Li3 N1 108.11(13) . . ?
O3 Li3 Li1 158.24(19) . . ?
N3 Li3 Li1 53.92(10) . . ?
N1 Li3 Li1 54.85(10) . . ?
O3 Li3 C1 94.47(12) . . ?
N3 Li3 C1 138.10(14) . . ?
N1 Li3 C1 31.19(6) . . ?
Li1 Li3 C1 85.96(11) . . ?
N1 B1 N2 110.38(12) . 2_655 ?
N1 B1 B2 131.17(13) . . ?
N2 B1 B2 118.38(12) 2_655 . ?
N1 B1 Li1 57.59(10) . . ?
N2 B1 Li1 167.48(13) 2_655 . ?
B2 B1 Li1 73.87(10) . . ?
N1 B1 Li2 123.50(12) . . ?
N2 B1 Li2 67.34(10) 2_655 . ?
B2 B1 Li2 76.00(10) . . ?
Li1 B1 Li2 121.04(11) . . ?
O1 B2 N2 116.13(12) . . ?
O1 B2 O2 101.67(11) . . ?
N2 B2 O2 106.96(11) . . ?
O1 B2 B1 116.32(12) . . ?
N2 B2 B1 105.05(11) . . ?
O2 B2 B1 110.37(11) . . ?
O1 B2 Li1 51.65(9) . . ?
N2 B2 Li1 126.49(11) . . ?
O2 B2 Li1 126.13(12) . . ?
B1 B2 Li1 65.03(9) . . ?
O1 B2 Li2 128.88(12) . . ?
N2 B2 Li2 112.19(11) . . ?
O2 B2 Li2 47.31(8) . . ?
B1 B2 Li2 63.59(9) . . ?
Li1 B2 Li2 108.66(10) . . ?
O1 B2 Li2 133.29(11) . 2_655 ?
N2 B2 Li2 60.22(9) . 2_655 ?
O2 B2 Li2 48.69(9) . 2_655 ?
B1 B2 Li2 108.63(11) . 2_655 ?
Li1 B2 Li2 171.08(11) . 2_655 ?
Li2 B2 Li2 62.42(12) . 2_655 ?
C1 N1 B1 103.84(12) . . ?
C1 N1 Li3 100.04(12) . . ?
B1 N1 Li3 132.56(13) . . ?
C1 N1 Li1 169.79(13) . . ?
B1 N1 Li1 86.04(12) . . ?
Li3 N1 Li1 70.85(11) . . ?
C2 N2 B1 105.69(12) . 2_655 ?
C2 N2 B2 133.83(13) . . ?
B1 N2 B2 118.42(11) 2_655 . ?
C2 N2 Li2 120.95(11) . 2_655 ?
B1 N2 Li2 76.53(11) 2_655 2_655 ?
B2 N2 Li2 83.87(10) . 2_655 ?
C13 N3 C17 115.64(12) . . ?
C13 N3 Li3 116.15(13) . . ?
C17 N3 Li3 115.72(13) . . ?
C13 N3 Li1 117.85(13) . . ?
C17 N3 Li1 111.30(13) . . ?
Li3 N3 Li1 73.44(12) . . ?
C7 O1 B2 110.87(11) . . ?
C7 O1 Li1 115.51(12) . . ?
B2 O1 Li1 92.97(11) . . ?
C8 O2 B2 108.52(11) . . ?
C8 O2 Li2 140.15(12) . . ?
B2 O2 Li2 96.22(11) . . ?
C8 O2 Li2 119.44(12) . 2_655 ?
B2 O2 Li2 94.88(11) . 2_655 ?
Li2 O2 Li2 87.89(12) . 2_655 ?
C25 O3 C22 109.98(15) . . ?
C25 O3 Li3 123.50(15) . . ?
C22 O3 Li3 125.01(16) . . ?
C29 O4 C26 110.23(13) . . ?
C29 O4 Li2 128.67(15) . . ?
C26 O4 Li2 120.42(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C2 C3 C4 -176.89(15) . . . . ?
C1 C2 C3 C4 2.4(2) 2_655 . . . ?
C2 C3 C4 C5 -1.1(3) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . 2_655 ?
N1 C1 C6 C5 179.94(16) . . . 2_655 ?
C2 C1 C6 C5 0.9(2) 2_655 . . 2_655 ?
Li3 C1 C6 C5 -148.41(17) . . . 2_655 ?
O1 C7 C8 O2 35.44(14) . . . . ?
C9 C7 C8 O2 153.00(13) . . . . ?
C10 C7 C8 O2 -81.88(15) . . . . ?
O1 C7 C8 C12 153.13(13) . . . . ?
C9 C7 C8 C12 -89.31(17) . . . . ?
C10 C7 C8 C12 35.81(18) . . . . ?
O1 C7 C8 C11 -81.54(14) . . . . ?
C9 C7 C8 C11 36.02(18) . . . . ?
C10 C7 C8 C11 161.14(13) . . . . ?
N3 C13 C14 C15 -52.9(2) . . . . ?
C18 C13 C14 C15 77.3(2) . . . . ?
C19 C13 C14 C15 -169.31(17) . . . . ?
C13 C14 C15 C16 54.9(2) . . . . ?
C14 C15 C16 C17 -54.4(3) . . . . ?
N3 C13 C14' C15' 60.1(10) . . . . ?
C18' C13 C14' C15' -76.4(13) . . . . ?
C19' C13 C14' C15' 162.1(11) . . . . ?
C13 C14' C15' C16' -60.5(16) . . . . ?
C14' C15' C16' C17 48.7(18) . . . . ?
C15' C16' C17 N3 -39.5(16) . . . . ?
C15' C16' C17 C21' -175(5) . . . . ?
C15' C16' C17 C20' 81.6(14) . . . . ?
C15 C16 C17 N3 51.8(2) . . . . ?
C15 C16 C17 C21 170.8(7) . . . . ?
C15 C16 C17 C20 -75.5(2) . . . . ?
O3 C22 C23 C24 -33.6(2) . . . . ?
C22 C23 C24 C25 38.5(3) . . . . ?
C23 C24 C25 O3 -29.6(2) . . . . ?
O4 C26 C27 C28 28.0(2) . . . . ?
C26 C27 C28 C29 -37.3(2) . . . . ?
C27 C28 C29 O4 33.2(2) . . . . ?
N1 B1 B2 O1 -0.1(2) . . . . ?
N2 B1 B2 O1 176.55(12) 2_655 . . . ?
Li1 B1 B2 O1 -6.28(12) . . . . ?
Li2 B1 B2 O1 122.42(13) . . . . ?
N1 B1 B2 N2 129.83(16) . . . . ?
N2 B1 B2 N2 -53.52(14) 2_655 . . . ?
Li1 B1 B2 N2 123.65(12) . . . . ?
Li2 B1 B2 N2 -107.65(12) . . . . ?
N1 B1 B2 O2 -115.21(17) . . . . ?
N2 B1 B2 O2 61.44(17) 2_655 . . . ?
Li1 B1 B2 O2 -121.39(13) . . . . ?
Li2 B1 B2 O2 7.31(12) . . . . ?
N1 B1 B2 Li1 6.18(16) . . . . ?
N2 B1 B2 Li1 -177.17(15) 2_655 . . . ?
Li2 B1 B2 Li1 128.70(11) . . . . ?
N1 B1 B2 Li2 -122.52(18) . . . . ?
N2 B1 B2 Li2 54.13(13) 2_655 . . . ?
Li1 B1 B2 Li2 -128.70(11) . . . . ?
N1 B1 B2 Li2 -167.05(15) . . . 2_655 ?
N2 B1 B2 Li2 9.60(16) 2_655 . . 2_655 ?
Li1 B1 B2 Li2 -173.23(12) . . . 2_655 ?
Li2 B1 B2 Li2 -44.53(13) . . . 2_655 ?
C6 C1 N1 B1 -177.07(16) . . . . ?
C2 C1 N1 B1 2.04(17) 2_655 . . . ?
Li3 C1 N1 B1 138.69(16) . . . . ?
C6 C1 N1 Li3 44.2(2) . . . . ?
C2 C1 N1 Li3 -136.65(14) 2_655 . . . ?
C6 C1 N1 Li1 17.9(9) . . . . ?
C2 C1 N1 Li1 -163.0(7) 2_655 . . . ?
Li3 C1 N1 Li1 -26.4(8) . . . . ?
N2 B1 N1 C1 -1.26(16) 2_655 . . . ?
B2 B1 N1 C1 175.59(14) . . . . ?
Li1 B1 N1 C1 -177.37(14) . . . . ?
Li2 B1 N1 C1 74.44(16) . . . . ?
N2 B1 N1 Li3 116.77(17) 2_655 . . . ?
B2 B1 N1 Li3 -66.4(2) . . . . ?
Li1 B1 N1 Li3 -59.33(17) . . . . ?
Li2 B1 N1 Li3 -167.52(15) . . . . ?
N2 B1 N1 Li1 176.11(13) 2_655 . . . ?
B2 B1 N1 Li1 -7.04(18) . . . . ?
Li2 B1 N1 Li1 -108.19(15) . . . . ?
C3 C2 N2 B1 -179.46(16) . . . 2_655 ?
C1 C2 N2 B1 1.18(15) 2_655 . . 2_655 ?
C3 C2 N2 B2 -16.7(3) . . . . ?
C1 C2 N2 B2 163.93(14) 2_655 . . . ?
C3 C2 N2 Li2 97.1(2) . . . 2_655 ?
C1 C2 N2 Li2 -82.30(15) 2_655 . . 2_655 ?
O1 B2 N2 C2 1.1(2) . . . . ?
O2 B2 N2 C2 113.71(16) . . . . ?
B1 B2 N2 C2 -128.98(15) . . . . ?
Li1 B2 N2 C2 -59.2(2) . . . . ?
Li2 B2 N2 C2 163.84(14) . . . . ?
Li2 B2 N2 C2 127.88(17) 2_655 . . . ?
O1 B2 N2 B1 162.11(12) . . . 2_655 ?
O2 B2 N2 B1 -85.23(14) . . . 2_655 ?
B1 B2 N2 B1 32.07(14) . . . 2_655 ?
Li1 B2 N2 B1 101.90(15) . . . 2_655 ?
Li2 B2 N2 B1 -35.11(16) . . . 2_655 ?
Li2 B2 N2 B1 -71.06(13) 2_655 . . 2_655 ?
O1 B2 N2 Li2 -126.82(13) . . . 2_655 ?
O2 B2 N2 Li2 -14.17(11) . . . 2_655 ?
B1 B2 N2 Li2 103.14(11) . . . 2_655 ?
Li1 B2 N2 Li2 172.97(14) . . . 2_655 ?
Li2 B2 N2 Li2 35.96(13) . . . 2_655 ?
C18' C13 N3 C17 77.4(9) . . . . ?
C18 C13 N3 C17 -74.63(19) . . . . ?
C19 C13 N3 C17 166.71(14) . . . . ?
C19' C13 N3 C17 -153.9(6) . . . . ?
C14 C13 N3 C17 51.12(19) . . . . ?
C14' C13 N3 C17 -49.4(6) . . . . ?
C18' C13 N3 Li3 -142.1(9) . . . . ?
C18 C13 N3 Li3 65.9(2) . . . . ?
C19 C13 N3 Li3 -52.74(18) . . . . ?
C19' C13 N3 Li3 -13.3(6) . . . . ?
C14 C13 N3 Li3 -168.34(15) . . . . ?
C14' C13 N3 Li3 91.1(6) . . . . ?
C18' C13 N3 Li1 -57.8(9) . . . . ?
C18 C13 N3 Li1 150.20(16) . . . . ?
C19 C13 N3 Li1 31.54(19) . . . . ?
C19' C13 N3 Li1 71.0(6) . . . . ?
C14 C13 N3 Li1 -84.06(17) . . . . ?
C14' C13 N3 Li1 175.4(6) . . . . ?
C16' C17 N3 C13 44.4(9) . . . . ?
C16 C17 N3 C13 -51.0(2) . . . . ?
C21 C17 N3 C13 -171.8(6) . . . . ?
C21' C17 N3 C13 -175(4) . . . . ?
C20 C17 N3 C13 73.22(19) . . . . ?
C20' C17 N3 C13 -76.5(7) . . . . ?
C16' C17 N3 Li3 -96.4(9) . . . . ?
C16 C17 N3 Li3 168.27(16) . . . . ?
C21 C17 N3 Li3 47.4(6) . . . . ?
C21' C17 N3 Li3 44(4) . . . . ?
C20 C17 N3 Li3 -67.5(2) . . . . ?
C20' C17 N3 Li3 142.8(7) . . . . ?
C16' C17 N3 Li1 -177.6(9) . . . . ?
C16 C17 N3 Li1 86.99(19) . . . . ?
C21 C17 N3 Li1 -33.8(6) . . . . ?
C21' C17 N3 Li1 -37(4) . . . . ?
C20 C17 N3 Li1 -148.77(16) . . . . ?
C20' C17 N3 Li1 61.5(7) . . . . ?
C9 C7 O1 B2 -148.94(13) . . . . ?
C10 C7 O1 B2 92.69(15) . . . . ?
C8 C7 O1 B2 -27.15(15) . . . . ?
C9 C7 O1 Li1 106.98(15) . . . . ?
C10 C7 O1 Li1 -11.39(17) . . . . ?
C8 C7 O1 Li1 -131.23(13) . . . . ?
N2 B2 O1 C7 124.07(13) . . . . ?
O2 B2 O1 C7 8.41(14) . . . . ?
B1 B2 O1 C7 -111.51(13) . . . . ?
Li1 B2 O1 C7 -118.77(13) . . . . ?
Li2 B2 O1 C7 -35.31(18) . . . . ?
Li2 B2 O1 C7 51.40(19) 2_655 . . . ?
N2 B2 O1 Li1 -117.16(13) . . . . ?
O2 B2 O1 Li1 127.18(12) . . . . ?
B1 B2 O1 Li1 7.27(14) . . . . ?
Li2 B2 O1 Li1 83.46(15) . . . . ?
Li2 B2 O1 Li1 170.17(15) 2_655 . . . ?
C12 C8 O2 B2 -152.80(13) . . . . ?
C11 C8 O2 B2 88.69(14) . . . . ?
C7 C8 O2 B2 -30.97(14) . . . . ?
C12 C8 O2 Li2 -27.4(2) . . . . ?
C11 C8 O2 Li2 -145.89(17) . . . . ?
C7 C8 O2 Li2 94.5(2) . . . . ?
C12 C8 O2 Li2 100.21(16) . . . 2_655 ?
C11 C8 O2 Li2 -18.30(18) . . . 2_655 ?
C7 C8 O2 Li2 -137.95(13) . . . 2_655 ?
O1 B2 O2 C8 15.36(14) . . . . ?
N2 B2 O2 C8 -106.86(12) . . . . ?
B1 B2 O2 C8 139.39(12) . . . . ?
Li1 B2 O2 C8 66.04(15) . . . . ?
Li2 B2 O2 C8 148.31(14) . . . . ?
Li2 B2 O2 C8 -123.29(13) 2_655 . . . ?
O1 B2 O2 Li2 -132.95(12) . . . . ?
N2 B2 O2 Li2 104.83(13) . . . . ?
B1 B2 O2 Li2 -8.92(14) . . . . ?
Li1 B2 O2 Li2 -82.27(15) . . . . ?
Li2 B2 O2 Li2 88.40(12) 2_655 . . . ?
O1 B2 O2 Li2 138.65(12) . . . 2_655 ?
N2 B2 O2 Li2 16.43(13) . . . 2_655 ?
B1 B2 O2 Li2 -97.32(13) . . . 2_655 ?
Li1 B2 O2 Li2 -170.67(13) . . . 2_655 ?
Li2 B2 O2 Li2 -88.40(12) . . . 2_655 ?
C24 C25 O3 C22 8.6(2) . . . . ?
C24 C25 O3 Li3 -157.89(17) . . . . ?
C23 C22 O3 C25 15.8(2) . . . . ?
C23 C22 O3 Li3 -177.88(18) . . . . ?
C28 C29 O4 C26 -16.2(2) . . . . ?
C28 C29 O4 Li2 154.21(17) . . . . ?
C27 C26 O4 C29 -7.5(2) . . . . ?
C27 C26 O4 Li2 -178.87(15) . . . . ?
O2 Li2 O4 C29 73.4(2) . . . . ?
O2 Li2 O4 C29 -72.0(3) 2_655 . . . ?
N2 Li2 O4 C29 -161.98(16) 2_655 . . . ?
B1 Li2 O4 C29 159.35(16) . . . . ?
B2 Li2 O4 C29 117.7(2) . . . . ?
B2 Li2 O4 C29 -132.4(2) 2_655 . . . ?
Li2 Li2 O4 C29 20.1(6) 2_655 . . . ?
O2 Li2 O4 C26 -117.00(18) . . . . ?
O2 Li2 O4 C26 97.6(3) 2_655 . . . ?
N2 Li2 O4 C26 7.6(2) 2_655 . . . ?
B1 Li2 O4 C26 -31.1(2) . . . . ?
B2 Li2 O4 C26 -72.8(2) . . . . ?
B2 Li2 O4 C26 37.2(3) 2_655 . . . ?
Li2 Li2 O4 C26 -170.3(4) 2_655 . . . ?

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
C21 H21C O1 0.98 2.54 3.480(16) 159.6 .
C21 H21C O1 0.98 2.54 3.480(16) 159.6 .

_refine_diff_density_max         0.548
_refine_diff_density_min         -0.289
_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_wo1wo
_database_code_depnum_ccdc_archive 'CCDC 2089027'
loop_
_audit_author_name
_audit_author_address
'Christian Kleeberg'
;Technische Universitaet Braunschweig, Institut fuer Anorganische und Analytische Chemie
Germany
;
_audit_update_record             
;
2021-08-24 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C16 H27 B2 N2 O3, 0.5 (C4 H8 O K), 0.5 (C8 H16 O2 K)'
_chemical_formula_sum            'C22 H39 B2 K N2 O4.50'
_chemical_formula_weight         464.27

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'
B B 0.0090 0.0039 '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      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

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

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

_cell_length_a                   11.5005(6)
_cell_length_b                   21.0732(9)
_cell_length_c                   11.8580(6)
_cell_angle_alpha                90
_cell_angle_beta                 114.857(6)
_cell_angle_gamma                90
_cell_volume                     2607.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15591
_cell_measurement_theta_min      4.102
_cell_measurement_theta_max      75.709

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.138
_exptl_absorpt_coefficient_mu    2.025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_recrystallization_method 
;
 From a solution in THF layered with n-pentane at -40 deg C.
;

_exptl_special_details           
;
 The crystal was mounted at rt with perfluoroether oil on top of a human hair
 and placed in a cold nitrogen gas stream on the diffractometer.

 The collected data cover more than a hemisphere of the reciprocal space.
 A combination of 48 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 1.5 deg in ω.
 Each frame was exposured for 3 s (low 2θ angles) or 9 s (high 2θ angles).
 Nominal crystal to detector distance 53 mm.
;


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            34751
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.109
_diffrn_reflns_theta_max         76.598
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             5235
_reflns_number_gt                5013
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_max     0.910
_reflns_Friedel_fraction_full    0.924

_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 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution    
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_molecular_graphics    
;
 K. Brandenburg, 2016, Diamond 4.2.2, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 Olex2 (Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)
;


_refine_special_details          
;
 NH hydrogen atoms were refined freely.
 
 Refinement as a inversion twin resulted in a BASF differing less than 
 2 sigma from 0.
 
 A THF moiety located on a C2 axis was described using a split atom model;
 geometrical restraints were applied.


 All other H atoms were placed in idealised positions and refined using a
 riding model, with a common U restrained to be 1.2 (1.5 for methyl groups) 
 times the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond but not tip.


 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;



_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+1.0410P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2182 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(5)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5235
_refine_ls_number_parameters     323
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0860
_refine_ls_wR_factor_gt          0.0835
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.061
_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
C1 C 0.6120(3) 0.68028(15) 0.1869(3) 0.0341(6) Uani 1 1 d . . . . .
K1 K 0.500000 0.42149(4) 0.000000 0.03537(19) Uani 1 2 d S T P . .
B1 B 0.7118(3) 0.58055(16) 0.2145(3) 0.0282(6) Uani 1 1 d . . . . .
O1 O 0.59751(16) 0.47168(10) 0.21926(16) 0.0283(4) Uani 1 1 d . . . . .
N1 N 0.5926(2) 0.61500(12) 0.1753(2) 0.0327(5) Uani 1 1 d . . . . .
H1 H 0.519(4) 0.6024(19) 0.154(4) 0.043(10) Uiso 1 1 d . . . . .
N2 N 0.8057(2) 0.63188(11) 0.2514(2) 0.0284(4) Uani 1 1 d . . . . .
H2 H 0.890(4) 0.6326(19) 0.270(3) 0.041(9) Uiso 1 1 d . . . . .
B2 B 0.7199(3) 0.49817(15) 0.2203(3) 0.0259(6) Uani 1 1 d . . . . .
K2 K 1.000000 0.54874(4) 0.500000 0.02913(17) Uani 1 2 d S T P . .
C2 C 0.5282(3) 0.73053(17) 0.1653(3) 0.0459(7) Uani 1 1 d . . . . .
H2A H 0.438404 0.723534 0.132942 0.055 Uiso 1 1 calc R U . . .
O2 O 0.82017(16) 0.47579(9) 0.34403(16) 0.0277(4) Uani 1 1 d . . . . .
C3 C 0.5784(4) 0.79170(17) 0.1921(4) 0.0508(8) Uani 1 1 d . . . . .
H3 H 0.522068 0.826683 0.178883 0.061 Uiso 1 1 calc R U . . .
O3 O 0.72690(17) 0.46509(9) 0.11287(16) 0.0277(4) Uani 1 1 d . . . . .
C4 C 0.7096(3) 0.80237(16) 0.2378(3) 0.0432(7) Uani 1 1 d . . . . .
H4 H 0.741572 0.844528 0.254544 0.052 Uiso 1 1 calc R U . . .
O4 O 0.89147(18) 0.62883(10) 0.62361(18) 0.0357(4) Uani 1 1 d . . . . .
C5 C 0.7947(3) 0.75194(14) 0.2594(3) 0.0366(6) Uani 1 1 d . . . . .
H5 H 0.884384 0.759162 0.290619 0.044 Uiso 1 1 calc R U . . .
C6 C 0.7450(3) 0.69071(14) 0.2339(2) 0.0299(5) Uani 1 1 d . . . . .
C7 C 0.6232(3) 0.44732(15) 0.3392(2) 0.0332(6) Uani 1 1 d . . . . .
C8 C 0.7661(2) 0.42582(15) 0.3881(2) 0.0325(5) Uani 1 1 d . . . . .
C9 C 0.5304(3) 0.39336(18) 0.3273(3) 0.0443(7) Uani 1 1 d . . . . .
H9A H 0.443475 0.410434 0.299825 0.066 Uiso 1 1 calc R U . . .
H9B H 0.555833 0.372535 0.408092 0.066 Uiso 1 1 calc R U . . .
H9C H 0.532111 0.362431 0.266301 0.066 Uiso 1 1 calc R U . . .
C10 C 0.6050(3) 0.50032(18) 0.4173(3) 0.0417(7) Uani 1 1 d . . . . .
H10A H 0.670965 0.532814 0.432714 0.063 Uiso 1 1 calc R U . . .
H10B H 0.612388 0.483006 0.496706 0.063 Uiso 1 1 calc R U . . .
H10C H 0.520056 0.519319 0.372766 0.063 Uiso 1 1 calc R U . . .
C11 C 0.7806(3) 0.36270(15) 0.3321(3) 0.0406(7) Uani 1 1 d . . . . .
H11A H 0.730300 0.363749 0.241808 0.061 Uiso 1 1 calc R U . . .
H11B H 0.749645 0.328178 0.367711 0.061 Uiso 1 1 calc R U . . .
H11C H 0.871067 0.355653 0.350787 0.061 Uiso 1 1 calc R U . . .
C12 C 0.8356(3) 0.42231(19) 0.5292(3) 0.0426(7) Uani 1 1 d . . . . .
H12A H 0.830320 0.463525 0.565041 0.064 Uiso 1 1 calc R U . . .
H12B H 0.925772 0.411389 0.553226 0.064 Uiso 1 1 calc R U . . .
H12C H 0.795583 0.389744 0.560221 0.064 Uiso 1 1 calc R U . . .
C13 C 0.8060(2) 0.48286(13) 0.0527(2) 0.0273(5) Uani 1 1 d . . . . .
C14 C 0.7441(3) 0.53744(14) -0.0379(2) 0.0330(6) Uani 1 1 d . . . . .
H14A H 0.735377 0.574415 0.008139 0.050 Uiso 1 1 calc R U . . .
H14B H 0.659221 0.524348 -0.099103 0.050 Uiso 1 1 calc R U . . .
H14C H 0.798007 0.548530 -0.080608 0.050 Uiso 1 1 calc R U . . .
C15 C 0.8122(2) 0.42467(16) -0.0207(2) 0.0332(5) Uani 1 1 d . . . . .
H15A H 0.849496 0.389081 0.036343 0.050 Uiso 1 1 calc R U . . .
H15B H 0.865490 0.434068 -0.064952 0.050 Uiso 1 1 calc R U . . .
H15C H 0.725522 0.413417 -0.080839 0.050 Uiso 1 1 calc R U . . .
C16 C 0.9405(3) 0.50060(16) 0.1463(3) 0.0337(6) Uani 1 1 d . . . . .
H16A H 0.936405 0.538662 0.191975 0.051 Uiso 1 1 calc R U . . .
H16B H 0.994475 0.509063 0.102355 0.051 Uiso 1 1 calc R U . . .
H16C H 0.977194 0.465487 0.204788 0.051 Uiso 1 1 calc R U . . .
C17 C 0.8429(3) 0.68784(16) 0.5589(3) 0.0411(7) Uani 1 1 d . . . . .
H17A H 0.865597 0.692438 0.487501 0.049 Uiso 1 1 calc R U . . .
H17B H 0.877771 0.724505 0.615327 0.049 Uiso 1 1 calc R U . . .
C18 C 0.6992(3) 0.68321(17) 0.5152(3) 0.0449(7) Uani 1 1 d . . . . .
H18A H 0.659632 0.657233 0.438813 0.054 Uiso 1 1 calc R U . . .
H18B H 0.658782 0.725706 0.499585 0.054 Uiso 1 1 calc R U . . .
C19 C 0.6889(3) 0.6509(2) 0.6252(3) 0.0531(9) Uani 1 1 d . . . . .
H19A H 0.686702 0.682633 0.685813 0.064 Uiso 1 1 calc R U . . .
H19B H 0.610701 0.624432 0.597530 0.064 Uiso 1 1 calc R U . . .
C20 C 0.8086(3) 0.61008(16) 0.6820(3) 0.0383(6) Uani 1 1 d . . . . .
H20A H 0.852051 0.616997 0.772900 0.046 Uiso 1 1 calc R U . . .
H20B H 0.786046 0.564596 0.666374 0.046 Uiso 1 1 calc R U . . .
O5 O 0.5075(16) 0.3004(3) 0.0217(11) 0.075(4) Uani 0.5 1 d D . P A -1
C21 C 0.3916(10) 0.2596(6) -0.0182(10) 0.051(3) Uani 0.5 1 d D . P A -1
H21A H 0.341773 0.268570 0.030734 0.061 Uiso 0.5 1 calc R U P A -1
H21B H 0.335636 0.265061 -0.107676 0.061 Uiso 0.5 1 calc R U P A -1
C22 C 0.448(3) 0.1959(7) 0.008(3) 0.105(9) Uani 0.5 1 d D . P A -1
H22A H 0.384742 0.163124 -0.039467 0.126 Uiso 0.5 1 calc R U P A -1
H22B H 0.482347 0.185906 0.097843 0.126 Uiso 0.5 1 calc R U P A -1
C23 C 0.554(3) 0.2010(8) -0.035(3) 0.115(10) Uani 0.5 1 d D . P A -1
H23A H 0.624475 0.171132 0.012074 0.137 Uiso 0.5 1 calc R U P A -1
H23B H 0.521566 0.191203 -0.124433 0.137 Uiso 0.5 1 calc R U P A -1
C24 C 0.599(2) 0.2664(10) -0.011(2) 0.137(10) Uani 0.5 1 d D . P A -1
H24A H 0.685935 0.268197 0.058875 0.164 Uiso 0.5 1 calc R U P A -1
H24B H 0.603471 0.285244 -0.085286 0.164 Uiso 0.5 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 C2 1.381(4) . ?
C1 N1 1.391(4) . ?
C1 C6 1.407(4) . ?
K1 O3 2.5512(18) 2_655 ?
K1 O3 2.5512(18) . ?
K1 O5 2.561(7) . ?
K1 O1 2.5856(18) . ?
K1 O1 2.5856(18) 2_655 ?
B1 N1 1.444(4) . ?
B1 N2 1.460(4) . ?
B1 B2 1.738(5) . ?
O1 C7 1.421(3) . ?
O1 B2 1.509(3) . ?
N1 H1 0.82(4) . ?
N2 C6 1.395(4) . ?
N2 H2 0.90(4) . ?
B2 O3 1.484(3) . ?
B2 O2 1.511(4) . ?
K2 O2 2.6163(19) 2_756 ?
K2 O2 2.6164(19) . ?
K2 O4 2.845(2) 2_756 ?
K2 O4 2.845(2) . ?
C2 C3 1.393(5) . ?
C2 H2A 0.9500 . ?
O2 C8 1.429(3) . ?
C3 C4 1.390(5) . ?
C3 H3 0.9500 . ?
O3 C13 1.422(3) . ?
C4 C5 1.394(5) . ?
C4 H4 0.9500 . ?
O4 C17 1.445(4) . ?
O4 C20 1.449(3) . ?
C5 C6 1.392(4) . ?
C5 H5 0.9500 . ?
C7 C10 1.520(4) . ?
C7 C9 1.525(4) . ?
C7 C8 1.562(4) . ?
C8 C12 1.523(4) . ?
C8 C11 1.527(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C15 1.523(4) . ?
C13 C16 1.523(4) . ?
C13 C14 1.530(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.512(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.520(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.519(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
O5 C24 1.456(14) . ?
O5 C21 1.487(12) . ?
C21 C22 1.466(15) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.510(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.458(15) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 132.0(3) . . ?
C2 C1 C6 120.7(3) . . ?
N1 C1 C6 107.2(2) . . ?
O3 K1 O3 137.78(10) 2_655 . ?
O3 K1 O5 113.3(4) 2_655 . ?
O3 K1 O5 108.8(4) . . ?
O3 K1 O1 107.21(6) 2_655 . ?
O3 K1 O1 53.81(5) . . ?
O5 K1 O1 108.9(3) . . ?
O3 K1 O1 53.81(5) 2_655 2_655 ?
O3 K1 O1 107.21(6) . 2_655 ?
O5 K1 O1 119.4(3) . 2_655 ?
O1 K1 O1 131.70(10) . 2_655 ?
O3 K1 B2 26.93(6) 2_655 2_655 ?
O3 K1 B2 121.90(7) . 2_655 ?
O5 K1 B2 124.4(3) . 2_655 ?
O1 K1 B2 118.25(7) . 2_655 ?
O1 K1 B2 27.65(6) 2_655 2_655 ?
O3 K1 B2 121.90(7) 2_655 . ?
O3 K1 B2 26.93(6) . . ?
O5 K1 B2 116.0(3) . . ?
O1 K1 B2 27.65(6) . . ?
O1 K1 B2 118.25(7) 2_655 . ?
B2 K1 B2 119.46(11) 2_655 . ?
O3 K1 C24 126.7(4) 2_655 . ?
O3 K1 C24 94.5(4) . . ?
O5 K1 C24 21.8(4) . . ?
O1 K1 C24 114.2(4) . . ?
O1 K1 C24 111.0(4) 2_655 . ?
B2 K1 C24 127.0(4) 2_655 . ?
B2 K1 C24 110.1(4) . . ?
N1 B1 N2 101.9(2) . . ?
N1 B1 B2 122.9(2) . . ?
N2 B1 B2 135.0(2) . . ?
C7 O1 B2 108.91(19) . . ?
C7 O1 K1 132.72(17) . . ?
B2 O1 K1 99.70(13) . . ?
C1 N1 B1 112.0(2) . . ?
C1 N1 H1 117(3) . . ?
B1 N1 H1 131(3) . . ?
C6 N2 B1 110.7(2) . . ?
C6 N2 H2 116(3) . . ?
B1 N2 H2 132(3) . . ?
O3 B2 O1 101.9(2) . . ?
O3 B2 O2 113.1(2) . . ?
O1 B2 O2 102.78(19) . . ?
O3 B2 B1 117.2(2) . . ?
O1 B2 B1 109.6(2) . . ?
O2 B2 B1 110.9(2) . . ?
O3 B2 K1 51.12(11) . . ?
O1 B2 K1 52.65(11) . . ?
O2 B2 K1 130.74(17) . . ?
B1 B2 K1 117.41(17) . . ?
O2 K2 O2 108.03(9) 2_756 . ?
O2 K2 O4 108.97(6) 2_756 2_756 ?
O2 K2 O4 111.84(5) . 2_756 ?
O2 K2 O4 111.84(5) 2_756 . ?
O2 K2 O4 108.97(6) . . ?
O4 K2 O4 107.22(9) 2_756 . ?
O2 K2 N2 69.42(6) 2_756 2_756 ?
O2 K2 N2 165.10(5) . 2_756 ?
O4 K2 N2 82.42(6) 2_756 2_756 ?
O4 K2 N2 60.73(6) . 2_756 ?
O2 K2 C12 45.32(6) 2_756 2_756 ?
O2 K2 C12 76.91(7) . 2_756 ?
O4 K2 C12 91.69(8) 2_756 2_756 ?
O4 K2 C12 155.39(7) . 2_756 ?
N2 K2 C12 107.98(6) 2_756 2_756 ?
O2 K2 H2 151.9(7) 2_756 . ?
O2 K2 H2 78.5(7) . . ?
O4 K2 H2 45.7(7) 2_756 . ?
O4 K2 H2 90.5(7) . . ?
N2 K2 H2 110.9(7) 2_756 . ?
C12 K2 H2 114.1(7) 2_756 . ?
C1 C2 C3 118.5(3) . . ?
C1 C2 H2A 120.8 . . ?
C3 C2 H2A 120.8 . . ?
C8 O2 B2 108.25(19) . . ?
C8 O2 K2 120.72(14) . . ?
B2 O2 K2 123.84(15) . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C13 O3 B2 125.7(2) . . ?
C13 O3 K1 124.11(14) . . ?
B2 O3 K1 101.95(13) . . ?
C3 C4 C5 120.8(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C17 O4 C20 107.7(2) . . ?
C17 O4 K2 113.11(16) . . ?
C20 O4 K2 127.14(18) . . ?
C6 C5 C4 118.3(3) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
C5 C6 N2 131.1(3) . . ?
C5 C6 C1 120.7(3) . . ?
N2 C6 C1 108.2(2) . . ?
O1 C7 C10 108.7(2) . . ?
O1 C7 C9 109.5(2) . . ?
C10 C7 C9 109.5(2) . . ?
O1 C7 C8 102.72(19) . . ?
C10 C7 C8 112.3(2) . . ?
C9 C7 C8 113.8(3) . . ?
O2 C8 C12 109.2(2) . . ?
O2 C8 C11 109.8(2) . . ?
C12 C8 C11 109.4(3) . . ?
O2 C8 C7 101.7(2) . . ?
C12 C8 C7 114.0(2) . . ?
C11 C8 C7 112.4(2) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 C13 C15 105.6(2) . . ?
O3 C13 C16 111.5(2) . . ?
C15 C13 C16 109.7(2) . . ?
O3 C13 C14 110.0(2) . . ?
C15 C13 C14 108.9(2) . . ?
C16 C13 C14 110.9(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 C18 104.4(3) . . ?
O4 C17 H17A 110.9 . . ?
C18 C17 H17A 110.9 . . ?
O4 C17 H17B 110.9 . . ?
C18 C17 H17B 110.9 . . ?
H17A C17 H17B 108.9 . . ?
C17 C18 C19 101.7(2) . . ?
C17 C18 H18A 111.4 . . ?
C19 C18 H18A 111.4 . . ?
C17 C18 H18B 111.4 . . ?
C19 C18 H18B 111.4 . . ?
H18A C18 H18B 109.3 . . ?
C20 C19 C18 104.6(2) . . ?
C20 C19 H19A 110.8 . . ?
C18 C19 H19A 110.8 . . ?
C20 C19 H19B 110.8 . . ?
C18 C19 H19B 110.8 . . ?
H19A C19 H19B 108.9 . . ?
O4 C20 C19 106.8(3) . . ?
O4 C20 H20A 110.4 . . ?
C19 C20 H20A 110.4 . . ?
O4 C20 H20B 110.4 . . ?
C19 C20 H20B 110.4 . . ?
H20A C20 H20B 108.6 . . ?
C24 O5 C21 106.5(9) . . ?
C24 O5 K1 117.5(11) . . ?
C21 O5 K1 123.9(9) . . ?
C22 C21 O5 101.8(10) . . ?
C22 C21 H21A 111.4 . . ?
O5 C21 H21A 111.4 . . ?
C22 C21 H21B 111.4 . . ?
O5 C21 H21B 111.4 . . ?
H21A C21 H21B 109.3 . . ?
C21 C22 C23 102.2(13) . . ?
C21 C22 H22A 111.3 . . ?
C23 C22 H22A 111.3 . . ?
C21 C22 H22B 111.3 . . ?
C23 C22 H22B 111.3 . . ?
H22A C22 H22B 109.2 . . ?
C24 C23 C22 105.9(13) . . ?
C24 C23 H23A 110.6 . . ?
C22 C23 H23A 110.6 . . ?
C24 C23 H23B 110.6 . . ?
C22 C23 H23B 110.6 . . ?
H23A C23 H23B 108.7 . . ?
O5 C24 C23 106.2(12) . . ?
C23 C24 K1 143.0(13) . . ?
O5 C24 H24A 110.5 . . ?
C23 C24 H24A 110.5 . . ?
K1 C24 H24A 99.5 . . ?
O5 C24 H24B 110.5 . . ?
C23 C24 H24B 110.5 . . ?
K1 C24 H24B 78.2 . . ?
H24A C24 H24B 108.7 . . ?

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
C2 C1 N1 B1 -177.3(3) . . . . ?
C6 C1 N1 B1 0.1(3) . . . . ?
N2 B1 N1 C1 0.1(3) . . . . ?
B2 B1 N1 C1 175.8(2) . . . . ?
N1 B1 N2 C6 -0.4(3) . . . . ?
B2 B1 N2 C6 -175.3(3) . . . . ?
C7 O1 B2 O3 127.2(2) . . . . ?
K1 O1 B2 O3 -14.7(2) . . . . ?
C7 O1 B2 O2 9.9(3) . . . . ?
K1 O1 B2 O2 -131.97(16) . . . . ?
C7 O1 B2 B1 -108.1(2) . . . . ?
K1 O1 B2 B1 110.09(18) . . . . ?
C7 O1 B2 K1 141.8(2) . . . . ?
N1 B1 B2 O3 97.6(3) . . . . ?
N2 B1 B2 O3 -88.4(4) . . . . ?
N1 B1 B2 O1 -17.8(3) . . . . ?
N2 B1 B2 O1 156.3(3) . . . . ?
N1 B1 B2 O2 -130.5(2) . . . . ?
N2 B1 B2 O2 43.5(4) . . . . ?
N1 B1 B2 K1 39.5(3) . . . . ?
N2 B1 B2 K1 -146.5(2) . . . . ?
N1 C1 C2 C3 176.6(3) . . . . ?
C6 C1 C2 C3 -0.5(5) . . . . ?
O3 B2 O2 C8 -92.2(2) . . . . ?
O1 B2 O2 C8 16.8(3) . . . . ?
B1 B2 O2 C8 133.8(2) . . . . ?
K1 B2 O2 C8 -34.4(3) . . . . ?
O3 B2 O2 K2 117.48(19) . . . . ?
O1 B2 O2 K2 -133.48(15) . . . . ?
B1 B2 O2 K2 -16.5(3) . . . . ?
K1 B2 O2 K2 175.25(9) . . . . ?
C1 C2 C3 C4 0.9(6) . . . . ?
O1 B2 O3 C13 164.1(2) . . . . ?
O2 B2 O3 C13 -86.3(3) . . . . ?
B1 B2 O3 C13 44.6(3) . . . . ?
K1 B2 O3 C13 149.1(3) . . . . ?
O1 B2 O3 K1 15.0(2) . . . . ?
O2 B2 O3 K1 124.58(17) . . . . ?
B1 B2 O3 K1 -104.5(2) . . . . ?
C2 C3 C4 C5 -0.7(5) . . . . ?
C3 C4 C5 C6 0.0(5) . . . . ?
C4 C5 C6 N2 -176.5(3) . . . . ?
C4 C5 C6 C1 0.4(4) . . . . ?
B1 N2 C6 C5 177.7(3) . . . . ?
B1 N2 C6 C1 0.5(3) . . . . ?
C2 C1 C6 C5 -0.2(4) . . . . ?
N1 C1 C6 C5 -177.9(2) . . . . ?
C2 C1 C6 N2 177.4(3) . . . . ?
N1 C1 C6 N2 -0.4(3) . . . . ?
B2 O1 C7 C10 89.1(2) . . . . ?
K1 O1 C7 C10 -146.93(18) . . . . ?
B2 O1 C7 C9 -151.3(2) . . . . ?
K1 O1 C7 C9 -27.4(3) . . . . ?
B2 O1 C7 C8 -30.0(3) . . . . ?
K1 O1 C7 C8 93.9(2) . . . . ?
B2 O2 C8 C12 -155.0(2) . . . . ?
K2 O2 C8 C12 -3.6(3) . . . . ?
B2 O2 C8 C11 85.0(3) . . . . ?
K2 O2 C8 C11 -123.62(19) . . . . ?
B2 O2 C8 C7 -34.2(3) . . . . ?
K2 O2 C8 C7 117.15(17) . . . . ?
O1 C7 C8 O2 39.5(3) . . . . ?
C10 C7 C8 O2 -77.1(3) . . . . ?
C9 C7 C8 O2 157.8(2) . . . . ?
O1 C7 C8 C12 156.9(3) . . . . ?
C10 C7 C8 C12 40.3(4) . . . . ?
C9 C7 C8 C12 -84.9(3) . . . . ?
O1 C7 C8 C11 -77.8(3) . . . . ?
C10 C7 C8 C11 165.6(2) . . . . ?
C9 C7 C8 C11 40.4(3) . . . . ?
B2 O3 C13 C15 162.3(2) . . . . ?
K1 O3 C13 C15 -55.0(2) . . . . ?
B2 O3 C13 C16 43.2(3) . . . . ?
K1 O3 C13 C16 -174.12(17) . . . . ?
B2 O3 C13 C14 -80.4(3) . . . . ?
K1 O3 C13 C14 62.3(3) . . . . ?
C20 O4 C17 C18 -33.1(3) . . . . ?
K2 O4 C17 C18 112.4(2) . . . . ?
O4 C17 C18 C19 38.7(3) . . . . ?
C17 C18 C19 C20 -29.9(4) . . . . ?
C17 O4 C20 C19 13.6(3) . . . . ?
K2 O4 C20 C19 -125.7(2) . . . . ?
C18 C19 C20 O4 11.0(4) . . . . ?
C24 O5 C21 C22 36.0(19) . . . . ?
K1 O5 C21 C22 177.1(14) . . . . ?
O5 C21 C22 C23 -41.1(14) . . . . ?
C21 C22 C23 C24 32.6(19) . . . . ?
C21 O5 C24 C23 -16(2) . . . . ?
K1 O5 C24 C23 -159.6(19) . . . . ?
C21 O5 C24 K1 144.0(15) . . . . ?
C22 C23 C24 O5 -10(2) . . . . ?
C22 C23 C24 K1 -33(4) . . . . ?

_refine_diff_density_max         0.187
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.041

####################################################################### 
# 
# 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_wo3ck
_database_code_depnum_ccdc_archive 'CCDC 2089031'
loop_
_audit_author_name
_audit_author_address
'Christian Kleeberg'
;Technische Universitaet Braunschweig, Institut fuer Anorganische und Analytische Chemie
Germany
;
_audit_update_record             
;
2021-06-09 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H74 B4 Li2 N4 O9'
_chemical_formula_sum            'C44 H74 B4 Li2 N4 O9'
_chemical_formula_weight         860.19

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'
B B 0.0090 0.0039 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.5646(5)
_cell_length_b                   23.7208(10)
_cell_length_c                   18.0699(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.697(4)
_cell_angle_gamma                90
_cell_volume                     4886.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9614
_cell_measurement_theta_min      4.22
_cell_measurement_theta_max      75.66

_exptl_crystal_description       'fragment of prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_crystal_recrystallization_method 
;
 From a solution in THF layered with n-pentane at -40 deg C.
;

_exptl_special_details           
;
 The crystal was mounted at rt with perfluoroether oil on top of a human hair
 and placed in a cold nitrogen gas stream on the diffractometer.

 The collected data cover more than a hemisphere of the reciprocal space.
 A combination of 13 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 1.5 deg in ω.
 Each frame was exposured for 2.8 s (low 2θ angles) or 6 s (high 2θ angles).
 Nominal crystal to detector distance 53 mm.
;


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            34055
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.727
_diffrn_reflns_theta_max         69.990
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             9161
_reflns_number_gt                7136
_reflns_threshold_expression     'I > 2σ(I)'



_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;


_computing_data_collection       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution    
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_molecular_graphics    
;
 K. Brandenburg, 1999, Diamond 3.2i, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;




_refine_special_details          
;
 N-H hydrogen atoms were refined freely.

 All other H atoms were placed in idealised positions and refined using a 
 riding model, with a common U restrained to be 1.2 (1.5 for methyl groups) 
 times the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond but not tip.


 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;



_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0558P)²+0.5743P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9161
_refine_ls_number_parameters     584
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1135
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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 0.31130(13) 0.41544(7) 0.82961(9) 0.0239(3) Uani 1 1 d . . . . .
C2 C 0.29733(13) 0.47376(7) 0.82338(9) 0.0264(3) Uani 1 1 d . . . . .
H2 H 0.3321 0.4942 0.7876 0.032 Uiso 1 1 calc R U . . .
C3 C 0.23176(14) 0.50195(7) 0.87018(10) 0.0304(4) Uani 1 1 d . . . . .
H3 H 0.2219 0.5416 0.8655 0.036 Uiso 1 1 calc R U . . .
C4 C 0.18073(14) 0.47322(7) 0.92346(10) 0.0308(4) Uani 1 1 d . . . . .
H4 H 0.1372 0.4933 0.9550 0.037 Uiso 1 1 calc R U . . .
C5 C 0.19345(14) 0.41489(7) 0.93068(10) 0.0293(4) Uani 1 1 d . . . . .
H5 H 0.1590 0.3949 0.9670 0.035 Uiso 1 1 calc R U . . .
C6 C 0.25712(13) 0.38658(7) 0.88398(9) 0.0251(3) Uani 1 1 d . . . . .
C7 C 0.34849(13) 0.16962(7) 0.81730(10) 0.0257(3) Uani 1 1 d . . . . .
C8 C 0.34165(13) 0.17737(7) 0.73123(10) 0.0262(3) Uani 1 1 d . . . . .
C9 C 0.23037(14) 0.18208(7) 0.84210(11) 0.0317(4) Uani 1 1 d . . . . .
H9A H 0.2414 0.1840 0.8970 0.048 Uiso 1 1 calc R U . . .
H9B H 0.1745 0.1520 0.8242 0.048 Uiso 1 1 calc R U . . .
H9C H 0.1998 0.2182 0.8208 0.048 Uiso 1 1 calc R U . . .
C10 C 0.39176(15) 0.11179(7) 0.84700(11) 0.0319(4) Uani 1 1 d . . . . .
H10A H 0.4718 0.1058 0.8376 0.048 Uiso 1 1 calc R U . . .
H10B H 0.3401 0.0825 0.8214 0.048 Uiso 1 1 calc R U . . .
H10C H 0.3911 0.1100 0.9011 0.048 Uiso 1 1 calc R U . . .
C11 C 0.22605(14) 0.15744(7) 0.68487(11) 0.0324(4) Uani 1 1 d . . . . .
H11A H 0.1612 0.1798 0.6980 0.049 Uiso 1 1 calc R U . . .
H11B H 0.2138 0.1176 0.6955 0.049 Uiso 1 1 calc R U . . .
H11C H 0.2290 0.1621 0.6313 0.049 Uiso 1 1 calc R U . . .
C12 C 0.44341(14) 0.14871(7) 0.70133(10) 0.0295(4) Uani 1 1 d . . . . .
H12A H 0.4430 0.1603 0.6492 0.044 Uiso 1 1 calc R U . . .
H12B H 0.4344 0.1077 0.7034 0.044 Uiso 1 1 calc R U . . .
H12C H 0.5179 0.1598 0.7322 0.044 Uiso 1 1 calc R U . . .
C13 C 0.65622(13) 0.25241(7) 0.79767(9) 0.0234(3) Uani 1 1 d . . . . .
C14 C 0.69178(14) 0.20144(7) 0.83284(9) 0.0261(3) Uani 1 1 d . . . . .
H14 H 0.6368 0.1779 0.8515 0.031 Uiso 1 1 calc R U . . .
C15 C 0.80974(14) 0.18548(7) 0.84020(9) 0.0278(3) Uani 1 1 d . . . . .
H15 H 0.8341 0.1505 0.8632 0.033 Uiso 1 1 calc R U . . .
C16 C 0.89211(13) 0.21995(7) 0.81452(9) 0.0281(4) Uani 1 1 d . . . . .
H16 H 0.9718 0.2084 0.8206 0.034 Uiso 1 1 calc R U . . .
C17 C 0.85834(13) 0.27125(7) 0.77994(9) 0.0272(3) Uani 1 1 d . . . . .
H17 H 0.9144 0.2950 0.7626 0.033 Uiso 1 1 calc R U . . .
C18 C 0.74090(13) 0.28713(7) 0.77125(9) 0.0244(3) Uani 1 1 d . . . . .
C19 C 0.34365(13) 0.41582(7) 0.60983(9) 0.0258(3) Uani 1 1 d . . . . .
C20 C 0.44668(14) 0.45702(7) 0.63813(9) 0.0264(3) Uani 1 1 d . . . . .
C21 C 0.22533(14) 0.43744(8) 0.62576(10) 0.0311(4) Uani 1 1 d . . . . .
H21A H 0.1660 0.4078 0.6139 0.047 Uiso 1 1 calc R U . . .
H21B H 0.2017 0.4707 0.5947 0.047 Uiso 1 1 calc R U . . .
H21C H 0.2327 0.4476 0.6789 0.047 Uiso 1 1 calc R U . . .
C22 C 0.33121(15) 0.40115(8) 0.52666(10) 0.0333(4) Uani 1 1 d . . . . .
H22A H 0.4019 0.3815 0.5174 0.050 Uiso 1 1 calc R U . . .
H22B H 0.3209 0.4358 0.4968 0.050 Uiso 1 1 calc R U . . .
H22C H 0.2628 0.3767 0.5123 0.050 Uiso 1 1 calc R U . . .
C23 C 0.41369(15) 0.51922(7) 0.63077(10) 0.0326(4) Uani 1 1 d . . . . .
H23A H 0.3558 0.5277 0.6630 0.049 Uiso 1 1 calc R U . . .
H23B H 0.3802 0.5276 0.5784 0.049 Uiso 1 1 calc R U . . .
H23C H 0.4839 0.5423 0.6461 0.049 Uiso 1 1 calc R U . . .
C24 C 0.55195(14) 0.44662(8) 0.59854(10) 0.0325(4) Uani 1 1 d . . . . .
H24A H 0.6171 0.4711 0.6205 0.049 Uiso 1 1 calc R U . . .
H24B H 0.5299 0.4551 0.5449 0.049 Uiso 1 1 calc R U . . .
H24C H 0.5762 0.4071 0.6049 0.049 Uiso 1 1 calc R U . . .
C25 C 0.07450(15) 0.29550(8) 0.64642(10) 0.0326(4) Uani 1 1 d . . . . .
H25A H 0.0978 0.3294 0.6773 0.039 Uiso 1 1 calc R U . . .
H25B H 0.0735 0.2627 0.6802 0.039 Uiso 1 1 calc R U . . .
C26 C -0.04554(16) 0.30391(10) 0.59816(11) 0.0431(5) Uani 1 1 d . . . . .
H26A H -0.0605 0.3442 0.5858 0.052 Uiso 1 1 calc R U . . .
H26B H -0.1089 0.2892 0.6235 0.052 Uiso 1 1 calc R U . . .
C27 C -0.03509(15) 0.26960(9) 0.52826(10) 0.0387(4) Uani 1 1 d . . . . .
H27A H -0.0459 0.2288 0.5365 0.046 Uiso 1 1 calc R U . . .
H27B H -0.0923 0.2822 0.4843 0.046 Uiso 1 1 calc R U . . .
C28 C 0.08900(14) 0.28283(8) 0.51887(10) 0.0317(4) Uani 1 1 d . . . . .
H28A H 0.1206 0.2528 0.4898 0.038 Uiso 1 1 calc R U . . .
H28B H 0.0925 0.3192 0.4924 0.038 Uiso 1 1 calc R U . . .
C29 C 0.37819(14) 0.21954(7) 0.50182(10) 0.0304(4) Uani 1 1 d . . . . .
H29A H 0.3344 0.2381 0.4566 0.036 Uiso 1 1 calc R U . . .
H29B H 0.3276 0.1902 0.5186 0.036 Uiso 1 1 calc R U . . .
C30 C 0.49117(16) 0.19372(8) 0.48488(11) 0.0364(4) Uani 1 1 d . . . . .
H30A H 0.5132 0.1597 0.5157 0.044 Uiso 1 1 calc R U . . .
H30B H 0.4842 0.1838 0.4311 0.044 Uiso 1 1 calc R U . . .
C31 C 0.57896(15) 0.24099(9) 0.50600(11) 0.0379(4) Uani 1 1 d . . . . .
H31A H 0.6600 0.2263 0.5184 0.045 Uiso 1 1 calc R U . . .
H31B H 0.5751 0.2690 0.4651 0.045 Uiso 1 1 calc R U . . .
C32 C 0.53848(14) 0.26612(8) 0.57444(11) 0.0338(4) Uani 1 1 d . . . . .
H32A H 0.5733 0.2455 0.6205 0.041 Uiso 1 1 calc R U . . .
H32B H 0.5611 0.3063 0.5803 0.041 Uiso 1 1 calc R U . . .
C33 C 0.89203(14) 0.43392(8) 0.79858(10) 0.0317(4) Uani 1 1 d . . . . .
H33A H 0.8728 0.3967 0.8181 0.038 Uiso 1 1 calc R U . . .
H33B H 0.9141 0.4600 0.8414 0.038 Uiso 1 1 calc R U . . .
C34 C 0.99006(14) 0.42874(8) 0.75349(11) 0.0351(4) Uani 1 1 d . . . . .
H34A H 0.9818 0.3943 0.7221 0.042 Uiso 1 1 calc R U . . .
H34B H 1.0679 0.4287 0.7862 0.042 Uiso 1 1 calc R U . . .
C35 C 0.97126(15) 0.48179(8) 0.70594(12) 0.0399(4) Uani 1 1 d . . . . .
H35A H 1.0089 0.4787 0.6608 0.048 Uiso 1 1 calc R U . . .
H35B H 1.0020 0.5155 0.7351 0.048 Uiso 1 1 calc R U . . .
C36 C 0.83848(15) 0.48374(9) 0.68510(11) 0.0381(4) Uani 1 1 d . . . . .
H36A H 0.8107 0.5232 0.6797 0.046 Uiso 1 1 calc R U . . .
H36B H 0.8123 0.4638 0.6371 0.046 Uiso 1 1 calc R U . . .
C37 C 0.70008(15) 0.39120(7) 0.92238(10) 0.0321(4) Uani 1 1 d . . . . .
H37A H 0.7708 0.4003 0.9595 0.039 Uiso 1 1 calc R U . . .
H37B H 0.7198 0.3611 0.8887 0.039 Uiso 1 1 calc R U . . .
C38 C 0.59951(15) 0.37331(8) 0.96127(10) 0.0338(4) Uani 1 1 d . . . . .
H38A H 0.6281 0.3510 1.0070 0.041 Uiso 1 1 calc R U . . .
H38B H 0.5409 0.3509 0.9273 0.041 Uiso 1 1 calc R U . . .
C39 C 0.54826(15) 0.42950(8) 0.98085(10) 0.0354(4) Uani 1 1 d . . . . .
H39A H 0.5790 0.4402 1.0335 0.042 Uiso 1 1 calc R U . . .
H39B H 0.4616 0.4276 0.9740 0.042 Uiso 1 1 calc R U . . .
C40 C 0.58800(15) 0.47157(8) 0.92604(10) 0.0330(4) Uani 1 1 d . . . . .
H40A H 0.5192 0.4889 0.8942 0.040 Uiso 1 1 calc R U . . .
H40B H 0.6358 0.5018 0.9538 0.040 Uiso 1 1 calc R U . . .
C41 C 0.76059(15) 0.57196(8) 0.83167(12) 0.0398(4) Uani 1 1 d . . . . .
H41A H 0.8212 0.5703 0.7991 0.048 Uiso 1 1 calc R U . . .
H41B H 0.7877 0.5495 0.8775 0.048 Uiso 1 1 calc R U . . .
C42 C 0.73843(15) 0.63250(7) 0.85208(10) 0.0330(4) Uani 1 1 d . . . . .
H42A H 0.7524 0.6588 0.8119 0.040 Uiso 1 1 calc R U . . .
H42B H 0.7887 0.6435 0.8998 0.040 Uiso 1 1 calc R U . . .
C43 C 0.60951(16) 0.63151(8) 0.86005(11) 0.0366(4) Uani 1 1 d . . . . .
H43A H 0.5990 0.6175 0.9101 0.044 Uiso 1 1 calc R U . . .
H43B H 0.5736 0.6694 0.8518 0.044 Uiso 1 1 calc R U . . .
C44 C 0.55826(14) 0.59096(7) 0.79852(11) 0.0330(4) Uani 1 1 d . . . . .
H44A H 0.4884 0.5718 0.8116 0.040 Uiso 1 1 calc R U . . .
H44B H 0.5349 0.6113 0.7505 0.040 Uiso 1 1 calc R U . . .
Li1 Li 0.3256(2) 0.28806(12) 0.63814(16) 0.0290(6) Uani 1 1 d . . . . .
Li2 Li 0.6318(2) 0.46664(12) 0.77559(17) 0.0294(6) Uani 1 1 d . . . . .
B1 B 0.35694(14) 0.32102(8) 0.82313(10) 0.0241(4) Uani 1 1 d . . . . .
B2 B 0.42328(15) 0.26050(8) 0.79744(10) 0.0234(4) Uani 1 1 d . . . . .
B3 B 0.56177(15) 0.33367(8) 0.75039(10) 0.0235(4) Uani 1 1 d . . . . .
B4 B 0.44780(15) 0.38213(8) 0.72884(10) 0.0230(4) Uani 1 1 d . . . . .
N1 N 0.37209(11) 0.37680(5) 0.79267(7) 0.0229(3) Uani 1 1 d . . . . .
N2 N 0.28271(11) 0.32979(6) 0.87907(8) 0.0257(3) Uani 1 1 d . . . . .
N3 N 0.54799(11) 0.27961(6) 0.78483(7) 0.0230(3) Uani 1 1 d . . . . .
N4 N 0.68410(11) 0.33564(6) 0.74095(8) 0.0250(3) Uani 1 1 d . . . . .
O1 O 0.43176(9) 0.21089(4) 0.84831(6) 0.0242(2) Uani 1 1 d . . . . .
O2 O 0.35147(9) 0.23725(4) 0.72424(6) 0.0252(2) Uani 1 1 d . . . . .
O3 O 0.37656(9) 0.36615(5) 0.65340(6) 0.0250(2) Uani 1 1 d . . . . .
O4 O 0.48092(9) 0.44297(4) 0.71639(6) 0.0241(2) Uani 1 1 d . . . . .
O5 O 0.15478(10) 0.28588(5) 0.59436(7) 0.0317(3) Uani 1 1 d . . . . .
O6 O 0.41261(10) 0.26018(5) 0.56050(7) 0.0318(3) Uani 1 1 d . . . . .
O7 O 0.79316(9) 0.45600(5) 0.74602(7) 0.0311(3) Uani 1 1 d . . . . .
O8 O 0.64980(9) 0.55033(5) 0.79225(7) 0.0314(3) Uani 1 1 d . . . . .
O9 O 0.65685(10) 0.44039(5) 0.88029(7) 0.0309(3) Uani 1 1 d . . . . .
H4N H 0.7239(17) 0.3627(8) 0.7243(11) 0.031(5) Uiso 1 1 d . . . . .
H2N H 0.2598(17) 0.3048(8) 0.9106(12) 0.033(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
C1 N1 1.392(2) . ?
C1 C2 1.395(2) . ?
C1 C6 1.426(2) . ?
C2 C3 1.398(2) . ?
C3 C4 1.390(2) . ?
C4 C5 1.395(2) . ?
C5 C6 1.384(2) . ?
C6 N2 1.385(2) . ?
C7 O1 1.4205(18) . ?
C7 C10 1.526(2) . ?
C7 C9 1.536(2) . ?
C7 C8 1.555(2) . ?
C8 O2 1.4322(19) . ?
C8 C11 1.528(2) . ?
C8 C12 1.534(2) . ?
C13 N3 1.3924(19) . ?
C13 C14 1.395(2) . ?
C13 C18 1.422(2) . ?
C14 C15 1.400(2) . ?
C15 C16 1.393(2) . ?
C16 C17 1.393(2) . ?
C17 C18 1.393(2) . ?
C18 N4 1.391(2) . ?
C19 O3 1.4324(19) . ?
C19 C22 1.526(2) . ?
C19 C21 1.533(2) . ?
C19 C20 1.559(2) . ?
C20 O4 1.442(2) . ?
C20 C23 1.524(2) . ?
C20 C24 1.532(2) . ?
C25 O5 1.447(2) . ?
C25 C26 1.523(2) . ?
C26 C27 1.524(3) . ?
C27 C28 1.506(2) . ?
C28 O5 1.447(2) . ?
C29 O6 1.439(2) . ?
C29 C30 1.520(2) . ?
C30 C31 1.518(3) . ?
C31 C32 1.516(3) . ?
C32 O6 1.442(2) . ?
C33 O7 1.455(2) . ?
C33 C34 1.508(2) . ?
C34 C35 1.519(3) . ?
C35 C36 1.519(2) . ?
C36 O7 1.454(2) . ?
C37 O9 1.436(2) . ?
C37 C38 1.517(2) . ?
C38 C39 1.524(3) . ?
C39 C40 1.530(3) . ?
C40 O9 1.444(2) . ?
C41 O8 1.451(2) . ?
C41 C42 1.515(3) . ?
C42 C43 1.522(2) . ?
C43 C44 1.513(3) . ?
C44 O8 1.4502(19) . ?
Li1 O3 1.950(3) . ?
Li1 O2 1.951(3) . ?
Li1 O6 1.973(3) . ?
Li1 O5 2.001(3) . ?
Li2 O9 1.966(3) . ?
Li2 O4 1.969(3) . ?
Li2 O8 2.013(3) . ?
Li2 O7 2.041(3) . ?
B1 N2 1.447(2) . ?
B1 N1 1.455(2) . ?
B1 B2 1.728(3) . ?
B2 O1 1.486(2) . ?
B2 O2 1.541(2) . ?
B2 N3 1.565(2) . ?
B3 N3 1.446(2) . ?
B3 N4 1.454(2) . ?
B3 B4 1.743(2) . ?
B4 O3 1.517(2) . ?
B4 O4 1.519(2) . ?
B4 N1 1.566(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 132.47(15) . . ?
N1 C1 C6 109.29(14) . . ?
C2 C1 C6 118.23(14) . . ?
C1 C2 C3 119.53(15) . . ?
C4 C3 C2 121.45(16) . . ?
C3 C4 C5 120.05(16) . . ?
C6 C5 C4 118.87(16) . . ?
C5 C6 N2 130.72(15) . . ?
C5 C6 C1 121.86(15) . . ?
N2 C6 C1 107.41(14) . . ?
O1 C7 C10 108.68(13) . . ?
O1 C7 C9 109.23(13) . . ?
C10 C7 C9 108.98(14) . . ?
O1 C7 C8 103.30(12) . . ?
C10 C7 C8 114.61(14) . . ?
C9 C7 C8 111.78(13) . . ?
O2 C8 C11 109.48(13) . . ?
O2 C8 C12 109.36(13) . . ?
C11 C8 C12 108.78(14) . . ?
O2 C8 C7 102.37(12) . . ?
C11 C8 C7 113.84(14) . . ?
C12 C8 C7 112.77(13) . . ?
N3 C13 C14 131.69(15) . . ?
N3 C13 C18 109.04(14) . . ?
C14 C13 C18 119.20(14) . . ?
C13 C14 C15 119.03(15) . . ?
C16 C15 C14 121.31(15) . . ?
C15 C16 C17 120.42(14) . . ?
C18 C17 C16 118.75(15) . . ?
N4 C18 C17 130.93(15) . . ?
N4 C18 C13 107.76(13) . . ?
C17 C18 C13 121.28(15) . . ?
O3 C19 C22 109.03(13) . . ?
O3 C19 C21 109.56(13) . . ?
C22 C19 C21 108.80(14) . . ?
O3 C19 C20 102.56(12) . . ?
C22 C19 C20 113.96(14) . . ?
C21 C19 C20 112.69(14) . . ?
O4 C20 C23 109.43(13) . . ?
O4 C20 C24 108.19(13) . . ?
C23 C20 C24 108.78(14) . . ?
O4 C20 C19 104.20(12) . . ?
C23 C20 C19 114.32(13) . . ?
C24 C20 C19 111.68(14) . . ?
O5 C25 C26 105.73(14) . . ?
C25 C26 C27 102.29(15) . . ?
C28 C27 C26 101.07(15) . . ?
O5 C28 C27 105.29(14) . . ?
O6 C29 C30 106.13(13) . . ?
C31 C30 C29 102.29(14) . . ?
C32 C31 C30 102.13(14) . . ?
O6 C32 C31 105.09(14) . . ?
O7 C33 C34 104.85(14) . . ?
C33 C34 C35 100.90(14) . . ?
C34 C35 C36 102.00(15) . . ?
O7 C36 C35 106.07(15) . . ?
O9 C37 C38 104.30(13) . . ?
C37 C38 C39 102.78(14) . . ?
C38 C39 C40 104.43(14) . . ?
O9 C40 C39 106.93(14) . . ?
O8 C41 C42 106.45(14) . . ?
C41 C42 C43 102.53(14) . . ?
C44 C43 C42 102.06(14) . . ?
O8 C44 C43 106.21(14) . . ?
O3 Li1 O2 118.17(15) . . ?
O3 Li1 O6 103.93(14) . . ?
O2 Li1 O6 109.37(14) . . ?
O3 Li1 O5 109.60(14) . . ?
O2 Li1 O5 107.94(14) . . ?
O6 Li1 O5 107.34(14) . . ?
O9 Li2 O4 113.94(14) . . ?
O9 Li2 O8 99.99(14) . . ?
O4 Li2 O8 114.98(14) . . ?
O9 Li2 O7 102.69(13) . . ?
O4 Li2 O7 126.03(16) . . ?
O8 Li2 O7 94.88(12) . . ?
N2 B1 N1 104.89(14) . . ?
N2 B1 B2 130.50(15) . . ?
N1 B1 B2 124.54(14) . . ?
O1 B2 O2 102.57(12) . . ?
O1 B2 N3 110.68(12) . . ?
O2 B2 N3 110.81(13) . . ?
O1 B2 B1 118.55(14) . . ?
O2 B2 B1 109.18(12) . . ?
N3 B2 B1 105.08(12) . . ?
N3 B3 N4 105.01(14) . . ?
N3 B3 B4 123.18(13) . . ?
N4 B3 B4 131.81(15) . . ?
O3 B4 O4 102.50(12) . . ?
O3 B4 N1 110.80(12) . . ?
O4 B4 N1 111.83(13) . . ?
O3 B4 B3 108.16(13) . . ?
O4 B4 B3 117.36(12) . . ?
N1 B4 B3 106.12(13) . . ?
C1 N1 B1 108.34(13) . . ?
C1 N1 B4 133.63(13) . . ?
B1 N1 B4 118.02(13) . . ?
C6 N2 B1 110.04(14) . . ?
C13 N3 B3 108.76(13) . . ?
C13 N3 B2 131.77(13) . . ?
B3 N3 B2 119.39(13) . . ?
C18 N4 B3 109.36(14) . . ?
C7 O1 B2 109.39(12) . . ?
C8 O2 B2 108.57(12) . . ?
C8 O2 Li1 132.79(13) . . ?
B2 O2 Li1 116.86(12) . . ?
C19 O3 B4 110.01(12) . . ?
C19 O3 Li1 131.13(13) . . ?
B4 O3 Li1 118.03(13) . . ?
C20 O4 B4 109.29(12) . . ?
C20 O4 Li2 122.60(12) . . ?
B4 O4 Li2 114.39(12) . . ?
C25 O5 C28 109.13(12) . . ?
C25 O5 Li1 115.96(13) . . ?
C28 O5 Li1 134.50(13) . . ?
C29 O6 C32 109.89(12) . . ?
C29 O6 Li1 129.61(13) . . ?
C32 O6 Li1 117.64(13) . . ?
C36 O7 C33 108.25(12) . . ?
C36 O7 Li2 127.17(13) . . ?
C33 O7 Li2 121.75(13) . . ?
C44 O8 C41 108.81(13) . . ?
C44 O8 Li2 127.50(12) . . ?
C41 O8 Li2 118.86(13) . . ?
C37 O9 C40 106.81(13) . . ?
C37 O9 Li2 138.48(14) . . ?
C40 O9 Li2 112.49(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -178.58(16) . . . . ?
C6 C1 C2 C3 0.2(2) . . . . ?
C1 C2 C3 C4 0.6(2) . . . . ?
C2 C3 C4 C5 -0.6(3) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
C4 C5 C6 N2 -179.78(16) . . . . ?
C4 C5 C6 C1 0.9(2) . . . . ?
N1 C1 C6 C5 178.10(14) . . . . ?
C2 C1 C6 C5 -0.9(2) . . . . ?
N1 C1 C6 N2 -1.35(17) . . . . ?
C2 C1 C6 N2 179.61(13) . . . . ?
O1 C7 C8 O2 -37.27(14) . . . . ?
C10 C7 C8 O2 -155.33(12) . . . . ?
C9 C7 C8 O2 80.04(15) . . . . ?
O1 C7 C8 C11 -155.31(13) . . . . ?
C10 C7 C8 C11 86.63(17) . . . . ?
C9 C7 C8 C11 -38.00(19) . . . . ?
O1 C7 C8 C12 80.12(15) . . . . ?
C10 C7 C8 C12 -37.93(18) . . . . ?
C9 C7 C8 C12 -162.57(13) . . . . ?
N3 C13 C14 C15 -177.53(16) . . . . ?
C18 C13 C14 C15 -0.9(2) . . . . ?
C13 C14 C15 C16 1.3(2) . . . . ?
C14 C15 C16 C17 -0.7(3) . . . . ?
C15 C16 C17 C18 -0.4(2) . . . . ?
C16 C17 C18 N4 178.34(16) . . . . ?
C16 C17 C18 C13 0.7(2) . . . . ?
N3 C13 C18 N4 -0.87(18) . . . . ?
C14 C13 C18 N4 -178.19(14) . . . . ?
N3 C13 C18 C17 177.23(14) . . . . ?
C14 C13 C18 C17 -0.1(2) . . . . ?
O3 C19 C20 O4 -33.81(15) . . . . ?
C22 C19 C20 O4 -151.50(13) . . . . ?
C21 C19 C20 O4 83.89(15) . . . . ?
O3 C19 C20 C23 -153.21(14) . . . . ?
C22 C19 C20 C23 89.10(17) . . . . ?
C21 C19 C20 C23 -35.51(19) . . . . ?
O3 C19 C20 C24 82.74(15) . . . . ?
C22 C19 C20 C24 -34.94(19) . . . . ?
C21 C19 C20 C24 -159.55(14) . . . . ?
O5 C25 C26 C27 28.1(2) . . . . ?
C25 C26 C27 C28 -39.2(2) . . . . ?
C26 C27 C28 O5 37.03(19) . . . . ?
O6 C29 C30 C31 -27.85(18) . . . . ?
C29 C30 C31 C32 37.16(18) . . . . ?
C30 C31 C32 O6 -33.86(18) . . . . ?
O7 C33 C34 C35 38.98(17) . . . . ?
C33 C34 C35 C36 -40.69(19) . . . . ?
C34 C35 C36 O7 28.6(2) . . . . ?
O9 C37 C38 C39 -36.82(17) . . . . ?
C37 C38 C39 C40 22.18(17) . . . . ?
C38 C39 C40 O9 -0.42(18) . . . . ?
O8 C41 C42 C43 29.0(2) . . . . ?
C41 C42 C43 C44 -36.73(18) . . . . ?
C42 C43 C44 O8 32.16(18) . . . . ?
N2 B1 B2 O1 -15.6(2) . . . . ?
N1 B1 B2 O1 160.82(14) . . . . ?
N2 B1 B2 O2 101.28(19) . . . . ?
N1 B1 B2 O2 -82.34(18) . . . . ?
N2 B1 B2 N3 -139.81(16) . . . . ?
N1 B1 B2 N3 36.6(2) . . . . ?
N3 B3 B4 O3 -83.65(18) . . . . ?
N4 B3 B4 O3 97.03(19) . . . . ?
N3 B3 B4 O4 161.13(14) . . . . ?
N4 B3 B4 O4 -18.2(3) . . . . ?
N3 B3 B4 N1 35.3(2) . . . . ?
N4 B3 B4 N1 -144.03(17) . . . . ?
C2 C1 N1 B1 179.24(16) . . . . ?
C6 C1 N1 B1 0.39(17) . . . . ?
C2 C1 N1 B4 -1.0(3) . . . . ?
C6 C1 N1 B4 -179.85(15) . . . . ?
N2 B1 N1 C1 0.68(16) . . . . ?
B2 B1 N1 C1 -176.47(14) . . . . ?
N2 B1 N1 B4 -179.13(12) . . . . ?
B2 B1 N1 B4 3.7(2) . . . . ?
O3 B4 N1 C1 -99.23(18) . . . . ?
O4 B4 N1 C1 14.4(2) . . . . ?
B3 B4 N1 C1 143.58(16) . . . . ?
O3 B4 N1 B1 80.52(16) . . . . ?
O4 B4 N1 B1 -165.81(12) . . . . ?
B3 B4 N1 B1 -36.67(17) . . . . ?
C5 C6 N2 B1 -177.59(17) . . . . ?
C1 C6 N2 B1 1.79(17) . . . . ?
N1 B1 N2 C6 -1.54(17) . . . . ?
B2 B1 N2 C6 175.38(15) . . . . ?
C14 C13 N3 B3 175.96(17) . . . . ?
C18 C13 N3 B3 -0.91(18) . . . . ?
C14 C13 N3 B2 -7.4(3) . . . . ?
C18 C13 N3 B2 175.77(15) . . . . ?
N4 B3 N3 C13 2.24(17) . . . . ?
B4 B3 N3 C13 -177.24(14) . . . . ?
N4 B3 N3 B2 -174.93(13) . . . . ?
B4 B3 N3 B2 5.6(2) . . . . ?
O1 B2 N3 C13 16.5(2) . . . . ?
O2 B2 N3 C13 -96.58(19) . . . . ?
B1 B2 N3 C13 145.61(16) . . . . ?
O1 B2 N3 B3 -167.09(13) . . . . ?
O2 B2 N3 B3 79.82(17) . . . . ?
B1 B2 N3 B3 -37.99(18) . . . . ?
C17 C18 N4 B3 -175.54(17) . . . . ?
C13 C18 N4 B3 2.31(18) . . . . ?
N3 B3 N4 C18 -2.80(17) . . . . ?
B4 B3 N4 C18 176.62(16) . . . . ?
C10 C7 O1 B2 154.47(13) . . . . ?
C9 C7 O1 B2 -86.74(16) . . . . ?
C8 C7 O1 B2 32.35(15) . . . . ?
O2 B2 O1 C7 -15.05(15) . . . . ?
N3 B2 O1 C7 -133.30(13) . . . . ?
B1 B2 O1 C7 105.24(15) . . . . ?
C11 C8 O2 B2 149.56(14) . . . . ?
C12 C8 O2 B2 -91.34(15) . . . . ?
C7 C8 O2 B2 28.47(14) . . . . ?
C11 C8 O2 Li1 -46.6(2) . . . . ?
C12 C8 O2 Li1 72.48(19) . . . . ?
C7 C8 O2 Li1 -167.71(14) . . . . ?
O1 B2 O2 C8 -10.01(15) . . . . ?
N3 B2 O2 C8 108.14(14) . . . . ?
B1 B2 O2 C8 -136.59(13) . . . . ?
O1 B2 O2 Li1 -176.76(12) . . . . ?
N3 B2 O2 Li1 -58.61(17) . . . . ?
B1 B2 O2 Li1 56.66(17) . . . . ?
C22 C19 O3 B4 151.05(13) . . . . ?
C21 C19 O3 B4 -89.99(15) . . . . ?
C20 C19 O3 B4 29.91(15) . . . . ?
C22 C19 O3 Li1 -39.9(2) . . . . ?
C21 C19 O3 Li1 79.1(2) . . . . ?
C20 C19 O3 Li1 -160.99(15) . . . . ?
O4 B4 O3 C19 -14.95(15) . . . . ?
N1 B4 O3 C19 104.50(14) . . . . ?
B3 B4 O3 C19 -139.57(12) . . . . ?
O4 B4 O3 Li1 174.33(12) . . . . ?
N1 B4 O3 Li1 -66.22(17) . . . . ?
B3 B4 O3 Li1 49.71(17) . . . . ?
C23 C20 O4 B4 148.23(13) . . . . ?
C24 C20 O4 B4 -93.39(14) . . . . ?
C19 C20 O4 B4 25.57(15) . . . . ?
C23 C20 O4 Li2 -73.78(17) . . . . ?
C24 C20 O4 Li2 44.60(19) . . . . ?
C19 C20 O4 Li2 163.56(13) . . . . ?
O3 B4 O4 C20 -7.91(15) . . . . ?
N1 B4 O4 C20 -126.64(13) . . . . ?
B3 B4 O4 C20 110.40(15) . . . . ?
O3 B4 O4 Li2 -149.66(12) . . . . ?
N1 B4 O4 Li2 91.61(15) . . . . ?
B3 B4 O4 Li2 -31.36(19) . . . . ?
C26 C25 O5 C28 -5.2(2) . . . . ?
C26 C25 O5 Li1 168.54(15) . . . . ?
C27 C28 O5 C25 -20.32(19) . . . . ?
C27 C28 O5 Li1 167.58(17) . . . . ?
C30 C29 O6 C32 6.95(19) . . . . ?
C30 C29 O6 Li1 -153.04(16) . . . . ?
C31 C32 O6 C29 17.05(19) . . . . ?
C31 C32 O6 Li1 179.74(15) . . . . ?
C35 C36 O7 C33 -4.5(2) . . . . ?
C35 C36 O7 Li2 156.49(16) . . . . ?
C34 C33 O7 C36 -21.86(18) . . . . ?
C34 C33 O7 Li2 175.94(14) . . . . ?
C43 C44 O8 C41 -14.60(19) . . . . ?
C43 C44 O8 Li2 140.09(16) . . . . ?
C42 C41 O8 C44 -9.3(2) . . . . ?
C42 C41 O8 Li2 -166.51(15) . . . . ?
C38 C37 O9 C40 37.82(17) . . . . ?
C38 C37 O9 Li2 -122.93(19) . . . . ?
C39 C40 O9 C37 -23.27(17) . . . . ?
C39 C40 O9 Li2 143.04(14) . . . . ?

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
C2 H2 O4 0.95 2.61 3.188(2) 119.2 .
C14 H14 O1 0.95 2.49 3.0747(19) 120.0 .
C27 H27B O1 0.99 2.53 3.243(2) 129.2 4_565
N4 H4N O7 0.87(2) 2.36(2) 3.1162(18) 144.6(17) .

_refine_diff_density_max         0.261
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.043

####################################################################### 
# 
# 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_wo8ck2
_database_code_depnum_ccdc_archive 'CCDC 2089030'
loop_
_audit_author_name
_audit_author_address
'Christian Kleeberg'
;Technische Universitaet Braunschweig, Institut fuer Anorganische und Analytische Chemie
Germany
;
_audit_update_record             
;
2021-06-09 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H98 B4 Li6 N4 O10, 1.810 (C4 H8 O)'
_chemical_formula_sum            'C63.24 H112.48 B4 Li6 N4 O11.81'
_chemical_formula_weight         1202.73

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'
B B 0.0090 0.0039 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

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

_cell_length_a                   22.5108(4)
_cell_length_b                   12.8635(2)
_cell_length_c                   27.2387(5)
_cell_angle_alpha                90
_cell_angle_beta                 111.665(2)
_cell_angle_gamma                90
_cell_volume                     7330.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    35773
_cell_measurement_theta_min      3.83
_cell_measurement_theta_max      75.43

_exptl_crystal_description       'irregular block'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_F_000             2610
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.363
_exptl_crystal_size_min          0.243
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
 Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model.
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_crystal_recrystallization_method 
;
 From a solution in THF layered with n-pentane at -40deg C.
;

_exptl_special_details           
;
 The crystal was mounted at rt with perfluoroether oil on top of a human hair
 and placed in a cold nitrogen gas stream on the diffractometer.

 The collected data cover more than a hemisphere of the reciprocal space.
 A combination of 41 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 1.5 deg in ω.
 Each frame was exposured for 8 s (low 2θ angles) or 30 s (high 2θ angles).
 Nominal crystal to detector distance 53 mm.
;





_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            84735
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.492
_diffrn_reflns_theta_max         76.075
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7627
_reflns_number_gt                6880
_reflns_threshold_expression     'I > 2σ(I)'


_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;


_computing_data_collection       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement       
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution    
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_molecular_graphics    
;
 K. Brandenburg, 2016, Diamond 4.2.2, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 Olex2 (Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)
;



_refine_special_details          
;
 Three disordered THF molecules were refined using split atom models.
 The SOF refined to 0.802(4) (O4), 0.78(1) (O5) and, only partly occupied,
 0.137(3) (O6) and  0.768(4) (O6'). Similarity restraints (SAME) were
 employed for the fragments containing O4/O4' and O6/O6'. Common ADPs
 were refined for the thf molecules containing O6/O6' (EADP).


 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond but not tip.


 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1025P)²+3.9317P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7627
_refine_ls_number_parameters     486
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1655
_refine_ls_wR_factor_gt          0.1607
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.024
_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
C1 C 0.57187(6) 0.68267(10) 0.23965(5) 0.0317(3) Uani 1 1 d . . . . .
C2 C 0.50821(6) 0.65576(11) 0.21082(6) 0.0364(3) Uani 1 1 d . . . . .
H2 H 0.479877 0.641997 0.228644 0.044 Uiso 1 1 calc R U . . .
C3 C 0.48640(6) 0.64917(11) 0.15584(6) 0.0399(3) Uani 1 1 d . . . . .
H3 H 0.443127 0.631309 0.136268 0.048 Uiso 1 1 calc R U . . .
C4 C 0.52789(7) 0.66871(11) 0.12959(6) 0.0389(3) Uani 1 1 d . . . . .
H4 H 0.512378 0.664829 0.092125 0.047 Uiso 1 1 calc R U . . .
C5 C 0.59232(6) 0.69406(11) 0.15761(5) 0.0346(3) Uani 1 1 d . . . . .
H5 H 0.620217 0.706219 0.139213 0.041 Uiso 1 1 calc R U . . .
C6 C 0.61518(6) 0.70131(10) 0.21277(5) 0.0302(3) Uani 1 1 d . . . . .
C7 C 0.69771(6) 0.93386(11) 0.37941(5) 0.0354(3) Uani 1 1 d . . . . .
C8 C 0.76631(6) 0.93572(11) 0.37720(5) 0.0348(3) Uani 1 1 d . . . . .
C9 C 0.64600(6) 0.96390(12) 0.32649(6) 0.0391(3) Uani 1 1 d . . . . .
H9A H 0.650558 0.921201 0.298289 0.059 Uiso 1 1 calc R U . . .
H9B H 0.650626 1.037459 0.319226 0.059 Uiso 1 1 calc R U . . .
H9C H 0.603720 0.952287 0.328069 0.059 Uiso 1 1 calc R U . . .
C10 C 0.69011(7) 1.00253(12) 0.42241(6) 0.0445(3) Uani 1 1 d . . . . .
H10A H 0.645889 0.998737 0.420653 0.067 Uiso 1 1 calc R U . . .
H10B H 0.700484 1.074612 0.417070 0.067 Uiso 1 1 calc R U . . .
H10C H 0.719074 0.978348 0.457111 0.067 Uiso 1 1 calc R U . . .
C11 C 0.77590(7) 1.01714(12) 0.34013(6) 0.0428(3) Uani 1 1 d . . . . .
H11A H 0.819446 1.011822 0.340382 0.064 Uiso 1 1 calc R U . . .
H11B H 0.769334 1.086641 0.351963 0.064 Uiso 1 1 calc R U . . .
H11C H 0.745103 1.005278 0.304208 0.064 Uiso 1 1 calc R U . . .
C12 C 0.81864(7) 0.95027(12) 0.43180(6) 0.0421(3) Uani 1 1 d . . . . .
H12A H 0.810604 0.903645 0.457128 0.063 Uiso 1 1 calc R U . . .
H12B H 0.818512 1.022475 0.443239 0.063 Uiso 1 1 calc R U . . .
H12C H 0.860327 0.934010 0.430016 0.063 Uiso 1 1 calc R U . . .
C13 C 0.75849(7) 0.65985(11) 0.40211(6) 0.0371(3) Uani 1 1 d . . . . .
C14 C 0.79147(8) 0.59069(13) 0.37388(6) 0.0457(3) Uani 1 1 d . . . . .
H14A H 0.824843 0.630643 0.367280 0.069 Uiso 1 1 calc R U . . .
H14B H 0.759890 0.566757 0.340192 0.069 Uiso 1 1 calc R U . . .
H14C H 0.810737 0.530526 0.396127 0.069 Uiso 1 1 calc R U . . .
C15 C 0.70845(7) 0.59392(13) 0.41381(6) 0.0448(3) Uani 1 1 d . . . . .
H15A H 0.729872 0.537696 0.438195 0.067 Uiso 1 1 calc R U . . .
H15B H 0.678548 0.564208 0.380808 0.067 Uiso 1 1 calc R U . . .
H15C H 0.684963 0.637756 0.429894 0.067 Uiso 1 1 calc R U . . .
C16 C 0.80903(7) 0.69271(13) 0.45514(6) 0.0437(3) Uani 1 1 d . . . . .
H16A H 0.789355 0.737870 0.473865 0.066 Uiso 1 1 calc R U . . .
H16B H 0.843422 0.730463 0.448946 0.066 Uiso 1 1 calc R U . . .
H16C H 0.826635 0.630807 0.476546 0.066 Uiso 1 1 calc R U . . .
C17 C 0.48526(7) 0.86486(15) 0.35956(8) 0.0546(4) Uani 1 1 d . . . . .
H17A H 0.455582 0.816285 0.333919 0.065 Uiso 1 1 calc R U . . .
H17B H 0.489578 0.928194 0.340491 0.065 Uiso 1 1 calc R U . . .
C18 C 0.46096(9) 0.89206(18) 0.40253(10) 0.0704(6) Uani 1 1 d . . . . .
H18A H 0.433922 0.835724 0.407765 0.084 Uiso 1 1 calc R U . . .
H18B H 0.436047 0.957490 0.394357 0.084 Uiso 1 1 calc R U . . .
C19 C 0.52185(11) 0.90451(18) 0.45058(9) 0.0663(5) Uani 1 1 d . . . . .
H19A H 0.541030 0.974100 0.451532 0.080 Uiso 1 1 calc R U . . .
H19B H 0.514165 0.893217 0.483696 0.080 Uiso 1 1 calc R U . . .
C20 C 0.56347(8) 0.82006(14) 0.44187(6) 0.0495(4) Uani 1 1 d . . . . .
H20A H 0.609300 0.837104 0.460000 0.059 Uiso 1 1 calc R U . . .
H20B H 0.554716 0.752461 0.455222 0.059 Uiso 1 1 calc R U . . .
O4 O 0.52433(14) 0.5047(3) 0.33907(16) 0.0469(5) Uani 0.802(4) 1 d D . P A 1
C21 C 0.47274(15) 0.43521(19) 0.30953(14) 0.0378(8) Uani 0.802(4) 1 d D . P A 1
H21A H 0.481190 0.363803 0.324009 0.045 Uiso 0.802(4) 1 calc R U P A 1
H21B H 0.467546 0.433343 0.271826 0.045 Uiso 0.802(4) 1 calc R U P A 1
C22 C 0.41379(17) 0.4797(3) 0.31579(16) 0.0474(8) Uani 0.802(4) 1 d D . P A 1
H22A H 0.379820 0.426723 0.309236 0.057 Uiso 0.802(4) 1 calc R U P A 1
H22B H 0.396723 0.540077 0.292251 0.057 Uiso 0.802(4) 1 calc R U P A 1
C23 C 0.44169(11) 0.5117(2) 0.37335(10) 0.0609(7) Uani 0.802(4) 1 d D . P A 1
H23A H 0.414622 0.564482 0.381410 0.073 Uiso 0.802(4) 1 calc R U P A 1
H23B H 0.446612 0.451021 0.396920 0.073 Uiso 0.802(4) 1 calc R U P A 1
C24 C 0.50589(12) 0.5563(2) 0.37883(10) 0.0608(7) Uani 0.802(4) 1 d D . P A 1
H24A H 0.502634 0.632342 0.372764 0.073 Uiso 0.802(4) 1 calc R U P A 1
H24B H 0.537797 0.542780 0.414631 0.073 Uiso 0.802(4) 1 calc R U P A 1
O4' O 0.5090(4) 0.5198(9) 0.3284(6) 0.062(5) Uani 0.198(4) 1 d D . P A 2
C21' C 0.4659(6) 0.4343(8) 0.3046(7) 0.086(9) Uani 0.198(4) 1 d D . P A 2
H21C H 0.486963 0.366721 0.317536 0.103 Uiso 0.198(4) 1 calc R U P A 2
H21D H 0.452113 0.436199 0.265661 0.103 Uiso 0.198(4) 1 calc R U P A 2
C22' C 0.4096(5) 0.4499(6) 0.3214(6) 0.044(4) Uani 0.198(4) 1 d D . P A 2
H22C H 0.419194 0.426516 0.358144 0.053 Uiso 0.198(4) 1 calc R U P A 2
H22D H 0.370916 0.413691 0.297449 0.053 Uiso 0.198(4) 1 calc R U P A 2
C23' C 0.4027(3) 0.5669(6) 0.3163(4) 0.061(3) Uani 0.198(4) 1 d D . P A 2
H23C H 0.380825 0.587991 0.278940 0.074 Uiso 0.198(4) 1 calc R U P A 2
H23D H 0.378560 0.594409 0.337374 0.074 Uiso 0.198(4) 1 calc R U P A 2
C24' C 0.4712(4) 0.6038(6) 0.3378(4) 0.063(3) Uani 0.198(4) 1 d D . P A 2
H24C H 0.475933 0.667885 0.319484 0.075 Uiso 0.198(4) 1 calc R U P A 2
H24D H 0.485088 0.618629 0.376106 0.075 Uiso 0.198(4) 1 calc R U P A 2
C25 C 0.65449(8) 0.44276(12) 0.25646(7) 0.0458(3) Uani 1 1 d . . . . .
H25A H 0.677559 0.509914 0.262341 0.055 Uiso 1 1 calc R U . . .
H25B H 0.626437 0.437660 0.218726 0.055 Uiso 1 1 calc R U . . .
C26 C 0.70096(14) 0.35344(17) 0.27199(14) 0.0906(9) Uani 1 1 d . . . . .
H26A H 0.708972 0.325763 0.241083 0.109 Uiso 0.780(11) 1 calc R U P B 3
H26B H 0.742122 0.374664 0.299418 0.109 Uiso 0.780(11) 1 calc R U P B 3
H26C H 0.744726 0.376685 0.276943 0.109 Uiso 0.220(11) 1 calc R U P B 4
H26D H 0.687971 0.297598 0.245090 0.109 Uiso 0.220(11) 1 calc R U P B 4
C27 C 0.6671(2) 0.2747(3) 0.2932(2) 0.0775(14) Uani 0.780(11) 1 d . . P B 3
H27A H 0.635938 0.233950 0.264270 0.093 Uiso 0.780(11) 1 calc R U P B 3
H27B H 0.697908 0.226509 0.318245 0.093 Uiso 0.780(11) 1 calc R U P B 3
C27' C 0.6972(8) 0.3170(13) 0.3237(11) 0.114(8) Uani 0.220(11) 1 d . . P B 4
H27C H 0.705284 0.241341 0.328329 0.137 Uiso 0.220(11) 1 calc R U P B 4
H27D H 0.729143 0.353785 0.353883 0.137 Uiso 0.220(11) 1 calc R U P B 4
C28 C 0.63432(10) 0.34066(14) 0.32052(9) 0.0622(5) Uani 1 1 d . . . . .
H28A H 0.595665 0.305390 0.321454 0.075 Uiso 0.780(11) 1 calc R U P B 3
H28B H 0.663257 0.356001 0.357179 0.075 Uiso 0.780(11) 1 calc R U P B 3
H28C H 0.633319 0.351684 0.356175 0.075 Uiso 0.220(11) 1 calc R U P B 4
H28D H 0.604495 0.283650 0.302967 0.075 Uiso 0.220(11) 1 calc R U P B 4
O6 O 0.3889(8) 0.7993(9) 0.5005(8) 0.206(3) Uani 0.137(3) 1 d D . P C 5
C29 C 0.4191(6) 0.7081(11) 0.4888(7) 0.1029(15) Uani 0.137(3) 1 d D . P C 5
H29A H 0.419307 0.714489 0.452613 0.123 Uiso 0.137(3) 1 calc R U P C 5
H29B H 0.464071 0.704799 0.513694 0.123 Uiso 0.137(3) 1 calc R U P C 5
C30 C 0.3869(8) 0.6130(9) 0.4925(8) 0.1172(17) Uani 0.137(3) 1 d D . P C 5
H30A H 0.413753 0.570439 0.522908 0.141 Uiso 0.137(3) 1 calc R U P C 5
H30B H 0.375842 0.571353 0.459810 0.141 Uiso 0.137(3) 1 calc R U P C 5
C31 C 0.3277(7) 0.6504(12) 0.5003(7) 0.0995(13) Uani 0.137(3) 1 d D . P C 5
H31A H 0.290826 0.605535 0.480564 0.119 Uiso 0.137(3) 1 calc R U P C 5
H31B H 0.333906 0.647982 0.538240 0.119 Uiso 0.137(3) 1 calc R U P C 5
C32 C 0.3164(6) 0.7515(12) 0.4818(9) 0.131(2) Uani 0.137(3) 1 d D . P C 5
H32A H 0.290199 0.789726 0.498098 0.157 Uiso 0.137(3) 1 calc R U P C 5
H32B H 0.294776 0.753257 0.442908 0.157 Uiso 0.137(3) 1 calc R U P C 5
O6' O 0.3301(3) 0.7196(5) 0.45103(18) 0.206(3) Uani 0.768(4) 1 d D . P D 6
C29' C 0.3902(3) 0.6792(3) 0.45115(16) 0.1029(15) Uani 0.768(4) 1 d D . P D 6
H29C H 0.381573 0.629269 0.421678 0.123 Uiso 0.768(4) 1 calc R U P D 6
H29D H 0.415635 0.737182 0.445091 0.123 Uiso 0.768(4) 1 calc R U P D 6
C30' C 0.4271(3) 0.6280(4) 0.50018(19) 0.1172(17) Uani 0.768(4) 1 d D . P D 6
H30C H 0.470722 0.657583 0.515662 0.141 Uiso 0.768(4) 1 calc R U P D 6
H30D H 0.430327 0.552384 0.494790 0.141 Uiso 0.768(4) 1 calc R U P D 6
C31' C 0.3897(2) 0.6492(4) 0.53483(15) 0.0995(13) Uani 0.768(4) 1 d D . P D 6
H31C H 0.362263 0.588902 0.534546 0.119 Uiso 0.768(4) 1 calc R U P D 6
H31D H 0.419131 0.661701 0.571662 0.119 Uiso 0.768(4) 1 calc R U P D 6
C32' C 0.3525(3) 0.7363(5) 0.5150(2) 0.131(2) Uani 0.768(4) 1 d D . P D 6
H32C H 0.377744 0.800977 0.526530 0.157 Uiso 0.768(4) 1 calc R U P D 6
H32D H 0.315316 0.738641 0.526060 0.157 Uiso 0.768(4) 1 calc R U P D 6
Li1 Li 0.60663(12) 0.7725(2) 0.35526(10) 0.0423(5) Uani 1 1 d . . . . .
Li2 Li 0.57983(13) 0.5540(2) 0.30700(12) 0.0478(6) Uani 1 1 d . . . . .
Li3 Li 0.73871(11) 0.7029(2) 0.21220(9) 0.0368(5) Uani 1 1 d . . . . .
N1 N 0.60291(5) 0.69352(9) 0.29373(5) 0.0331(2) Uani 1 1 d . . . . .
N2 N 0.67601(5) 0.72519(8) 0.24878(4) 0.0299(2) Uani 1 1 d . . . . .
O1 O 0.77226(4) 0.83545(7) 0.35704(4) 0.0327(2) Uani 1 1 d . . . . .
O2 O 0.68985(4) 0.82751(7) 0.39118(4) 0.0349(2) Uani 1 1 d . . . . .
O3 O 0.54658(5) 0.81671(8) 0.38561(4) 0.0406(2) Uani 1 1 d . . . . .
O5 O 0.61745(5) 0.43451(8) 0.28977(5) 0.0473(3) Uani 1 1 d . . . . .
B1 B 0.66879(7) 0.72111(11) 0.30039(6) 0.0313(3) Uani 1 1 d . . . . .
B2 B 0.72375(7) 0.75861(12) 0.36334(6) 0.0321(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3849(18) . ?
C1 C2 1.3998(18) . ?
C1 C6 1.4394(17) . ?
C1 Li2 2.428(3) . ?
C2 C3 1.396(2) . ?
C3 C4 1.393(2) . ?
C4 C5 1.4054(18) . ?
C5 C6 1.3999(19) . ?
C6 N2 1.3928(16) . ?
C6 Li3 2.787(2) . ?
C7 O2 1.4310(17) . ?
C7 C10 1.5263(19) . ?
C7 C9 1.5307(19) . ?
C7 C8 1.5675(18) . ?
C8 O1 1.4274(16) . ?
C8 C11 1.525(2) . ?
C8 C12 1.5301(19) . ?
C13 C16 1.532(2) . ?
C13 C15 1.534(2) . ?
C13 C14 1.535(2) . ?
C13 B2 1.653(2) . ?
C17 O3 1.4385(18) . ?
C17 C18 1.505(3) . ?
C18 C19 1.514(3) . ?
C19 C20 1.509(3) . ?
C20 O3 1.4371(19) . ?
O4 C21 1.451(3) . ?
O4 C24 1.455(3) . ?
O4 Li2 1.879(4) . ?
C21 C22 1.511(3) . ?
C22 C23 1.515(4) . ?
C23 C24 1.510(3) . ?
O4' C21' 1.451(3) . ?
O4' C24' 1.455(3) . ?
O4' Li2 1.940(10) . ?
C21' C22' 1.511(3) . ?
C22' C23' 1.515(4) . ?
C23' C24' 1.510(3) . ?
C25 O5 1.4452(19) . ?
C25 C26 1.505(3) . ?
C26 C27 1.505(4) . ?
C26 C27' 1.52(2) . ?
C27 C28 1.492(4) . ?
C27' C28 1.418(13) . ?
C28 O5 1.438(2) . ?
O6 C29 1.449(7) . ?
O6 C32 1.640(6) . ?
C29 C30 1.446(6) . ?
C30 C31 1.504(6) . ?
C31 C32 1.384(7) . ?
O6' C29' 1.449(7) . ?
O6' C32' 1.640(6) . ?
C29' C30' 1.445(6) . ?
C30' C31' 1.504(6) . ?
C31' C32' 1.384(7) . ?
Li1 O2 1.901(3) . ?
Li1 O3 1.913(3) . ?
Li1 N1 1.935(3) . ?
Li1 B1 2.485(3) . ?
Li1 B2 2.570(3) . ?
Li1 Li2 3.067(4) . ?
Li2 O5 1.895(3) . ?
Li2 N1 1.940(3) . ?
Li3 O1 1.875(2) 7_665 ?
Li3 N2 2.026(2) . ?
Li3 N2 2.041(2) 7_665 ?
Li3 Li3 2.280(5) 7_665 ?
Li3 B1 2.436(3) 7_665 ?
Li3 B2 2.545(3) 7_665 ?
N1 B1 1.4697(17) . ?
N2 B1 1.4745(18) . ?
O1 B2 1.5288(16) . ?
O2 B2 1.5396(16) . ?
B1 B2 1.771(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 129.18(12) . . ?
N1 C1 C6 110.73(11) . . ?
C2 C1 C6 120.08(12) . . ?
N1 C1 Li2 52.95(9) . . ?
C2 C1 Li2 91.72(11) . . ?
C6 C1 Li2 128.54(11) . . ?
C3 C2 C1 119.92(12) . . ?
C4 C3 C2 120.21(12) . . ?
C3 C4 C5 121.07(13) . . ?
C6 C5 C4 119.69(12) . . ?
N2 C6 C5 130.31(11) . . ?
N2 C6 C1 110.67(11) . . ?
C5 C6 C1 119.02(11) . . ?
N2 C6 Li3 43.84(7) . . ?
C5 C6 Li3 88.10(9) . . ?
C1 C6 Li3 150.33(10) . . ?
O2 C7 C10 108.85(11) . . ?
O2 C7 C9 109.79(11) . . ?
C10 C7 C9 108.35(12) . . ?
O2 C7 C8 103.19(10) . . ?
C10 C7 C8 114.31(11) . . ?
C9 C7 C8 112.18(11) . . ?
O1 C8 C11 108.03(11) . . ?
O1 C8 C12 109.67(11) . . ?
C11 C8 C12 108.26(12) . . ?
O1 C8 C7 103.57(10) . . ?
C11 C8 C7 114.73(12) . . ?
C12 C8 C7 112.36(11) . . ?
C16 C13 C15 107.66(12) . . ?
C16 C13 C14 107.71(12) . . ?
C15 C13 C14 108.16(13) . . ?
C16 C13 B2 113.71(12) . . ?
C15 C13 B2 110.31(11) . . ?
C14 C13 B2 109.12(11) . . ?
O3 C17 C18 105.95(15) . . ?
C17 C18 C19 102.93(14) . . ?
C20 C19 C18 101.80(16) . . ?
O3 C20 C19 104.71(14) . . ?
C21 O4 C24 107.69(18) . . ?
C21 O4 Li2 118.9(2) . . ?
C24 O4 Li2 127.8(2) . . ?
O4 C21 C22 105.10(19) . . ?
C21 C22 C23 100.0(2) . . ?
C24 C23 C22 102.8(2) . . ?
O4 C24 C23 106.17(18) . . ?
C21' O4' C24' 107.7(2) . . ?
C21' O4' Li2 121.7(7) . . ?
C24' O4' Li2 118.9(7) . . ?
O4' C21' C22' 105.1(2) . . ?
C21' C22' C23' 100.0(3) . . ?
C24' C23' C22' 102.8(2) . . ?
O4' C24' C23' 106.1(2) . . ?
O5 C25 C26 105.64(15) . . ?
C27 C26 C25 102.96(19) . . ?
C25 C26 C27' 103.0(5) . . ?
C28 C27 C26 102.8(2) . . ?
C28 C27' C26 105.9(12) . . ?
C27' C28 O5 105.0(6) . . ?
O5 C28 C27 105.07(18) . . ?
C29 O6 C32 97.0(4) . . ?
C30 C29 O6 112.4(4) . . ?
C29 C30 C31 103.5(4) . . ?
C32 C31 C30 107.6(4) . . ?
C31 C32 O6 102.3(4) . . ?
C29' O6' C32' 97.1(4) . . ?
C30' C29' O6' 112.6(4) . . ?
C29' C30' C31' 103.5(4) . . ?
C32' C31' C30' 107.5(4) . . ?
C31' C32' O6' 102.3(4) . . ?
O2 Li1 O3 112.73(13) . . ?
O2 Li1 N1 111.14(12) . . ?
O3 Li1 N1 135.95(14) . . ?
O2 Li1 B1 75.04(9) . . ?
O3 Li1 B1 169.69(15) . . ?
N1 Li1 B1 36.22(6) . . ?
O2 Li1 B2 36.57(6) . . ?
O3 Li1 B2 148.23(14) . . ?
N1 Li1 B2 75.68(9) . . ?
B1 Li1 B2 40.98(6) . . ?
O2 Li1 Li2 124.21(12) . . ?
O3 Li1 Li2 113.51(12) . . ?
N1 Li1 Li2 37.71(8) . . ?
B1 Li1 Li2 64.13(8) . . ?
B2 Li1 Li2 90.35(9) . . ?
O4 Li2 O5 106.04(16) . . ?
O4 Li2 N1 131.95(18) . . ?
O5 Li2 N1 121.96(14) . . ?
O5 Li2 O4' 112.5(3) . . ?
N1 Li2 O4' 124.9(3) . . ?
O4 Li2 C1 134.82(19) . . ?
O5 Li2 C1 106.30(13) . . ?
N1 Li2 C1 34.74(7) . . ?
O4' Li2 C1 122.8(5) . . ?
O4 Li2 Li1 99.74(14) . . ?
O5 Li2 Li1 144.48(14) . . ?
N1 Li2 Li1 37.60(8) . . ?
O4' Li2 Li1 97.6(3) . . ?
C1 Li2 Li1 69.32(9) . . ?
O1 Li3 N2 132.43(13) 7_665 . ?
O1 Li3 N2 113.10(11) 7_665 7_665 ?
N2 Li3 N2 111.81(11) . 7_665 ?
O1 Li3 Li3 162.0(2) 7_665 7_665 ?
N2 Li3 Li3 56.21(10) . 7_665 ?
N2 Li3 Li3 55.61(10) 7_665 7_665 ?
O1 Li3 B1 76.48(9) 7_665 7_665 ?
N2 Li3 B1 143.02(12) . 7_665 ?
N2 Li3 B1 37.15(6) 7_665 7_665 ?
Li3 Li3 B1 89.80(13) 7_665 7_665 ?
O1 Li3 B2 36.67(6) 7_665 7_665 ?
N2 Li3 B2 150.39(13) . 7_665 ?
N2 Li3 B2 78.67(8) 7_665 7_665 ?
Li3 Li3 B2 126.65(16) 7_665 7_665 ?
B1 Li3 B2 41.58(6) 7_665 7_665 ?
O1 Li3 C6 104.03(10) 7_665 . ?
N2 Li3 C6 28.43(5) . . ?
N2 Li3 C6 138.51(11) 7_665 . ?
Li3 Li3 C6 83.62(12) 7_665 . ?
B1 Li3 C6 155.51(12) 7_665 . ?
B2 Li3 C6 129.48(10) 7_665 . ?
C1 N1 B1 104.20(10) . . ?
C1 N1 Li1 144.86(12) . . ?
B1 N1 Li1 92.71(11) . . ?
C1 N1 Li2 92.31(12) . . ?
B1 N1 Li2 121.87(12) . . ?
Li1 N1 Li2 104.69(13) . . ?
C6 N2 B1 103.76(10) . . ?
C6 N2 Li3 107.73(10) . . ?
B1 N2 Li3 143.69(11) . . ?
C6 N2 Li3 163.34(12) . 7_665 ?
B1 N2 Li3 86.16(10) . 7_665 ?
Li3 N2 Li3 68.19(11) . 7_665 ?
C8 O1 B2 111.64(9) . . ?
C8 O1 Li3 128.91(11) . 7_665 ?
B2 O1 Li3 96.23(10) . 7_665 ?
C7 O2 B2 108.37(10) . . ?
C7 O2 Li1 114.85(11) . . ?
B2 O2 Li1 96.07(10) . . ?
C20 O3 C17 109.94(12) . . ?
C20 O3 Li1 121.26(12) . . ?
C17 O3 Li1 128.13(13) . . ?
C28 O5 C25 109.74(13) . . ?
C28 O5 Li2 125.61(14) . . ?
C25 O5 Li2 120.68(12) . . ?
N1 B1 N2 110.64(11) . . ?
N1 B1 B2 119.83(11) . . ?
N2 B1 B2 129.04(11) . . ?
N1 B1 Li3 162.84(12) . 7_665 ?
N2 B1 Li3 56.69(8) . 7_665 ?
B2 B1 Li3 72.49(8) . 7_665 ?
N1 B1 Li1 51.07(9) . . ?
N2 B1 Li1 148.08(11) . . ?
B2 B1 Li1 72.08(9) . . ?
Li3 B1 Li1 132.69(10) 7_665 . ?
O1 B2 O2 100.81(10) . . ?
O1 B2 C13 112.31(10) . . ?
O2 B2 C13 109.35(10) . . ?
O1 B2 B1 109.88(10) . . ?
O2 B2 B1 109.73(10) . . ?
C13 B2 B1 113.95(11) . . ?
O1 B2 Li3 47.10(7) . 7_665 ?
O2 B2 Li3 131.22(11) . 7_665 ?
C13 B2 Li3 116.51(10) . 7_665 ?
B1 B2 Li3 65.93(8) . 7_665 ?
O1 B2 Li1 134.28(11) . . ?
O2 B2 Li1 47.36(8) . . ?
C13 B2 Li1 109.68(10) . . ?
B1 B2 Li1 66.94(8) . . ?
Li3 B2 Li1 123.62(10) 7_665 . ?

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 179.95(13) . . . . ?
C6 C1 C2 C3 -1.4(2) . . . . ?
Li2 C1 C2 C3 -138.91(14) . . . . ?
C1 C2 C3 C4 0.4(2) . . . . ?
C2 C3 C4 C5 0.8(2) . . . . ?
C3 C4 C5 C6 -0.9(2) . . . . ?
C4 C5 C6 N2 -179.79(13) . . . . ?
C4 C5 C6 C1 -0.10(19) . . . . ?
C4 C5 C6 Li3 167.26(13) . . . . ?
N1 C1 C6 N2 -0.12(15) . . . . ?
C2 C1 C6 N2 -179.03(11) . . . . ?
Li2 C1 C6 N2 -58.64(17) . . . . ?
N1 C1 C6 C5 -179.87(11) . . . . ?
C2 C1 C6 C5 1.22(19) . . . . ?
Li2 C1 C6 C5 121.61(15) . . . . ?
N1 C1 C6 Li3 26.4(2) . . . . ?
C2 C1 C6 Li3 -152.56(17) . . . . ?
Li2 C1 C6 Li3 -32.2(3) . . . . ?
O2 C7 C8 O1 32.94(12) . . . . ?
C10 C7 C8 O1 150.98(12) . . . . ?
C9 C7 C8 O1 -85.16(13) . . . . ?
O2 C7 C8 C11 150.44(11) . . . . ?
C10 C7 C8 C11 -91.52(15) . . . . ?
C9 C7 C8 C11 32.34(16) . . . . ?
O2 C7 C8 C12 -85.34(13) . . . . ?
C10 C7 C8 C12 32.70(17) . . . . ?
C9 C7 C8 C12 156.56(12) . . . . ?
O3 C17 C18 C19 26.3(2) . . . . ?
C17 C18 C19 C20 -37.2(2) . . . . ?
C18 C19 C20 O3 35.00(19) . . . . ?
C24 O4 C21 C22 24.1(4) . . . . ?
Li2 O4 C21 C22 -131.6(3) . . . . ?
O4 C21 C22 C23 -40.1(4) . . . . ?
C21 C22 C23 C24 40.4(3) . . . . ?
C21 O4 C24 C23 2.1(4) . . . . ?
Li2 O4 C24 C23 155.0(3) . . . . ?
C22 C23 C24 O4 -27.3(4) . . . . ?
C24' O4' C21' C22' -23.8(8) . . . . ?
Li2 O4' C21' C22' -166.3(11) . . . . ?
O4' C21' C22' C23' 40.0(6) . . . . ?
C21' C22' C23' C24' -40.6(5) . . . . ?
C21' O4' C24' C23' -2.5(9) . . . . ?
Li2 O4' C24' C23' 141.2(9) . . . . ?
C22' C23' C24' O4' 27.6(7) . . . . ?
O5 C25 C26 C27 26.2(3) . . . . ?
O5 C25 C26 C27' -14.1(10) . . . . ?
C25 C26 C27 C28 -36.4(4) . . . . ?
C25 C26 C27' C28 29.4(15) . . . . ?
C26 C27' C28 O5 -33.2(15) . . . . ?
C26 C27 C28 O5 33.6(4) . . . . ?
C32 O6 C29 C30 -28.0(8) . . . . ?
O6 C29 C30 C31 7.6(10) . . . . ?
C29 C30 C31 C32 21.5(9) . . . . ?
C30 C31 C32 O6 -38.1(7) . . . . ?
C29 O6 C32 C31 39.9(6) . . . . ?
C32' O6' C29' C30' 27.1(6) . . . . ?
O6' C29' C30' C31' -6.5(6) . . . . ?
C29' C30' C31' C32' -22.2(5) . . . . ?
C30' C31' C32' O6' 38.4(5) . . . . ?
C29' O6' C32' C31' -39.6(5) . . . . ?
C21 O4 Li2 O5 -59.2(3) . . . . ?
C24 O4 Li2 O5 150.6(3) . . . . ?
C21 O4 Li2 N1 123.4(3) . . . . ?
C24 O4 Li2 N1 -26.9(5) . . . . ?
C21 O4 Li2 C1 75.0(3) . . . . ?
C24 O4 Li2 C1 -75.2(4) . . . . ?
C21 O4 Li2 Li1 145.5(3) . . . . ?
C24 O4 Li2 Li1 -4.8(4) . . . . ?
C2 C1 N1 B1 179.21(13) . . . . ?
C6 C1 N1 B1 0.43(14) . . . . ?
Li2 C1 N1 B1 123.73(13) . . . . ?
C2 C1 N1 Li1 -64.4(3) . . . . ?
C6 C1 N1 Li1 116.81(19) . . . . ?
Li2 C1 N1 Li1 -119.9(2) . . . . ?
C2 C1 N1 Li2 55.48(16) . . . . ?
C6 C1 N1 Li2 -123.30(12) . . . . ?
C5 C6 N2 B1 179.47(13) . . . . ?
C1 C6 N2 B1 -0.25(14) . . . . ?
Li3 C6 N2 B1 -161.67(14) . . . . ?
C5 C6 N2 Li3 -18.86(18) . . . . ?
C1 C6 N2 Li3 161.42(11) . . . . ?
C5 C6 N2 Li3 54.2(4) . . . 7_665 ?
C1 C6 N2 Li3 -125.6(4) . . . 7_665 ?
Li3 C6 N2 Li3 73.0(4) . . . 7_665 ?
C11 C8 O1 B2 -140.91(11) . . . . ?
C12 C8 O1 B2 101.30(12) . . . . ?
C7 C8 O1 B2 -18.83(13) . . . . ?
C11 C8 O1 Li3 -22.86(17) . . . 7_665 ?
C12 C8 O1 Li3 -140.65(13) . . . 7_665 ?
C7 C8 O1 Li3 99.22(14) . . . 7_665 ?
C10 C7 O2 B2 -156.84(11) . . . . ?
C9 C7 O2 B2 84.71(12) . . . . ?
C8 C7 O2 B2 -35.05(13) . . . . ?
C10 C7 O2 Li1 97.10(13) . . . . ?
C9 C7 O2 Li1 -21.35(15) . . . . ?
C8 C7 O2 Li1 -141.10(11) . . . . ?
C19 C20 O3 C17 -19.47(19) . . . . ?
C19 C20 O3 Li1 151.80(15) . . . . ?
C18 C17 O3 C20 -4.46(19) . . . . ?
C18 C17 O3 Li1 -174.97(16) . . . . ?
C27' C28 O5 C25 24.5(12) . . . . ?
C27 C28 O5 C25 -17.7(3) . . . . ?
C27' C28 O5 Li2 -132.9(12) . . . . ?
C27 C28 O5 Li2 -175.2(3) . . . . ?
C26 C25 O5 C28 -5.6(2) . . . . ?
C26 C25 O5 Li2 153.19(19) . . . . ?
O4 Li2 O5 C28 -35.4(3) . . . . ?
N1 Li2 O5 C28 142.33(19) . . . . ?
O4' Li2 O5 C28 -46.3(5) . . . . ?
C1 Li2 O5 C28 176.57(14) . . . . ?
Li1 Li2 O5 C28 99.5(3) . . . . ?
O4 Li2 O5 C25 169.36(17) . . . . ?
N1 Li2 O5 C25 -12.9(3) . . . . ?
O4' Li2 O5 C25 158.5(5) . . . . ?
C1 Li2 O5 C25 21.34(19) . . . . ?
Li1 Li2 O5 C25 -55.7(3) . . . . ?
C1 N1 B1 N2 -0.59(14) . . . . ?
Li1 N1 B1 N2 -149.51(12) . . . . ?
Li2 N1 B1 N2 101.31(16) . . . . ?
C1 N1 B1 B2 172.11(11) . . . . ?
Li1 N1 B1 B2 23.19(15) . . . . ?
Li2 N1 B1 B2 -85.98(17) . . . . ?
C1 N1 B1 Li3 39.1(4) . . . 7_665 ?
Li1 N1 B1 Li3 -109.8(4) . . . 7_665 ?
Li2 N1 B1 Li3 141.0(4) . . . 7_665 ?
C1 N1 B1 Li1 148.93(14) . . . . ?
Li2 N1 B1 Li1 -109.17(17) . . . . ?
C6 N2 B1 N1 0.52(14) . . . . ?
Li3 N2 B1 N1 -149.10(16) . . . . ?
Li3 N2 B1 N1 166.96(12) 7_665 . . . ?
C6 N2 B1 B2 -171.33(12) . . . . ?
Li3 N2 B1 B2 39.1(3) . . . . ?
Li3 N2 B1 B2 -4.89(15) 7_665 . . . ?
C6 N2 B1 Li3 -166.44(12) . . . 7_665 ?
Li3 N2 B1 Li3 43.9(2) . . . 7_665 ?
C6 N2 B1 Li1 -47.8(2) . . . . ?
Li3 N2 B1 Li1 162.61(19) . . . . ?
Li3 N2 B1 Li1 118.7(2) 7_665 . . . ?
C8 O1 B2 O2 -1.30(13) . . . . ?
Li3 O1 B2 O2 -137.60(11) 7_665 . . . ?
C8 O1 B2 C13 -117.59(12) . . . . ?
Li3 O1 B2 C13 106.11(12) 7_665 . . . ?
C8 O1 B2 B1 114.46(11) . . . . ?
Li3 O1 B2 B1 -21.85(13) 7_665 . . . ?
C8 O1 B2 Li3 136.30(13) . . . 7_665 ?
C8 O1 B2 Li1 37.71(18) . . . . ?
Li3 O1 B2 Li1 -98.59(15) 7_665 . . . ?
C7 O2 B2 O1 23.50(12) . . . . ?
Li1 O2 B2 O1 142.23(11) . . . . ?
C7 O2 B2 C13 141.96(11) . . . . ?
Li1 O2 B2 C13 -99.31(13) . . . . ?
C7 O2 B2 B1 -92.37(12) . . . . ?
Li1 O2 B2 B1 26.36(13) . . . . ?
C7 O2 B2 Li3 -17.55(16) . . . 7_665 ?
Li1 O2 B2 Li3 101.18(15) . . . 7_665 ?
C7 O2 B2 Li1 -118.73(13) . . . . ?
C16 C13 B2 O1 50.58(15) . . . . ?
C15 C13 B2 O1 171.63(11) . . . . ?
C14 C13 B2 O1 -69.68(14) . . . . ?
C16 C13 B2 O2 -60.45(14) . . . . ?
C15 C13 B2 O2 60.60(14) . . . . ?
C14 C13 B2 O2 179.29(11) . . . . ?
C16 C13 B2 B1 176.34(11) . . . . ?
C15 C13 B2 B1 -62.61(14) . . . . ?
C14 C13 B2 B1 56.09(14) . . . . ?
C16 C13 B2 Li3 102.44(13) . . . 7_665 ?
C15 C13 B2 Li3 -136.51(12) . . . 7_665 ?
C14 C13 B2 Li3 -17.82(15) . . . 7_665 ?
C16 C13 B2 Li1 -110.90(12) . . . . ?
C15 C13 B2 Li1 10.15(15) . . . . ?
C14 C13 B2 Li1 128.84(12) . . . . ?
N1 B1 B2 O1 -149.54(11) . . . . ?
N2 B1 B2 O1 21.65(18) . . . . ?
Li3 B1 B2 O1 17.37(10) 7_665 . . . ?
Li1 B1 B2 O1 -130.76(12) . . . . ?
N1 B1 B2 O2 -39.57(16) . . . . ?
N2 B1 B2 O2 131.62(13) . . . . ?
Li3 B1 B2 O2 127.34(11) 7_665 . . . ?
Li1 B1 B2 O2 -20.80(10) . . . . ?
N1 B1 B2 C13 83.42(14) . . . . ?
N2 B1 B2 C13 -105.38(15) . . . . ?
Li3 B1 B2 C13 -109.67(11) 7_665 . . . ?
Li1 B1 B2 C13 102.20(12) . . . . ?
N1 B1 B2 Li3 -166.91(14) . . . 7_665 ?
N2 B1 B2 Li3 4.28(13) . . . 7_665 ?
Li1 B1 B2 Li3 -148.13(10) . . . 7_665 ?
N1 B1 B2 Li1 -18.78(12) . . . . ?
N2 B1 B2 Li1 152.42(15) . . . . ?
Li3 B1 B2 Li1 148.13(10) 7_665 . . . ?

_refine_diff_density_max         0.450
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.046

