# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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 
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data_3THF
_database_code_depnum_ccdc_archive 'CCDC 1535025'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.	2020-01-07 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_KDP021              
;
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: A partial occupancy lattice solvent THF is
present in the asymmetric unit. The corresponding H-atoms
could not be satisfactorily introduced into ideal
positions and were therefore omitted from the model. They
have been included in the formula for the calculation
of intensive properties.
;
_vrf_PLAT041_KDP021              
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ 
RESPONSE: A partial occupancy lattice solvent THF is
present in the asymmetric unit. The corresponding H-atoms
could not be satisfactorily introduced into ideal
positions and were therefore omitted from the model. They
have been included in the formula for the calculation
of intensive properties.
;
_vrf_PLAT043_KDP021              
;
PROBLEM: Check Reported Molecular Weight 
RESPONSE: A partial occupancy lattice solvent THF is
present in the asymmetric unit. The corresponding H-atoms
could not be satisfactorily introduced into ideal
positions and were therefore omitted from the model. They
have been included in the formula for the calculation
of intensive properties.
;
_vrf_PLAT068_KDP021              
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)
RESPONSE: A partial occupancy lattice solvent THF is
present in the asymmetric unit. The corresponding H-atoms
could not be satisfactorily introduced into ideal
positions and were therefore omitted from the model. They
have been included in the formula for the calculation
of intensive properties.
;
_vrf_PLAT230_KDP021              
;
PROBLEM: Hirshfeld Test Diff for    C18    --  C19
RESPONSE: C18 and C19 are adjacent pyridine ring atoms. The
pyridine ring is part of the main ligand, and is coordinated
to the sodium ion. This test result does not indicate that
a wrong atom-type has been assigned.
;
_vrf_PLAT241_KDP021              
;
PROBLEM: Check High Ueq as Compared to Neighbors for C34 
RESPONSE: C34 is part of a coordinated THF molecule. This 
test result does not indicate that a wrong atom-type 
has been assigned. There was no strong evidence to indicate
that a significant disorder component was present.
;
_vrf_FORMU01_KDP021              
;
PROBLEM: There is a discrepancy between the atom counts in the
RESPONSE: A partial occupancy lattice solvent THF is
present in the asymmetric unit. The corresponding H-atoms
could not be satisfactorily introduced into ideal
positions and were therefore omitted from the model. They
have been included in the formula for the calculation
of intensive properties.
;
_vrf_CELLZ01_KDP021              
;
PROBLEM: Difference between formula and atom_site contents detected
RESPONSE: A partial occupancy lattice solvent THF is
present in the asymmetric unit. The corresponding H-atoms
could not be satisfactorily introduced into ideal
positions and were therefore omitted from the model. They
have been included in the formula for the calculation
of intensive properties.
;
_vrf_PLAT002_KDP021              
;
PROBLEM:  Number of Distance or Angle Restraints on AtSite
RESPONSE: A distance restraint was applied to the O2-H2
bond. Please see _refine_special_details for full information.
;
_vrf_PLAT003_KDP021              
;
PROBLEM:  Number of Uiso or Uij Restrained Atom Sites
RESPONSE: A partial occupancy disordered lattice THF
molecule is present in the asymmetric unit. Similarity 
restraints were applied to the atoms in this molecule.
 Please see _refine_special_details for full information.
;
_vrf_PLAT042_KDP021              
;
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ 
RESPONSE: A partial occupancy lattice solvent THF is
present in the asymmetric unit. The corresponding H-atoms
could not be satisfactorily introduced into ideal
positions and were therefore omitted from the model. They
have been included in the formula for the calculation
of intensive properties.
;
_vrf_PLAT860_KDP021              
;
PROBLEM:  Note: Number of Least-Squares Restraints
RESPONSE: Please see _refine_special_details for full information.
;
_vrf_PLAT045_KDP021              
;
PROBLEM:  Calculated and Reported Z Differ
RESPONSE: The reported formula unit (reflected by the value of Z)
is based on the main fragment, and not the partial occupancy lattice
solvent THF molecule.
;
_vrf_PLAT244_KDP021              
;
PROBLEM:  Low   'Solvent' Ueq as Compared to Neighbors of
RESPONSE: C37 is part of a partial occupancy disordered THF
group. Great care was taken in assigning atoms in this group (that
is, in determining the location of the oxygen.) Consideration
was given to exchanging the atom identities of C37 and O7, however,
this lead to an NDP atom upon anisotropic refinement.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C30 H39 N2 O4), Na, 1.5(C4 H8 O)'
_chemical_formula_sum            'C36 H51 N2 Na O5.50'
_chemical_formula_weight         622.80

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

loop_
_symmetry_equiv_pos_as_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                   22.745(7)
_cell_length_b                   16.871(5)
_cell_length_c                   18.568(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.513(4)
_cell_angle_gamma                90.00
_cell_volume                     6898(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    14413
_cell_measurement_theta_min      1.6
_cell_measurement_theta_max      29.7

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2688
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            21786
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         26.50
_reflns_number_total             7065
_reflns_number_gt                5898
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.2008, A64, 112-122)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'

_refine_special_details          
; 
 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. 

 All non-hydrogen atoms were refined anisotropically, while all H-atoms
 except H2 were introduced in calculated positions and refined on a
 riding model. H2 was introduced in its difference map position and
 refined with Uiso = 1.5 Ueq of O2. A distance restraint was applied to the
 O2-H2 bond. One half-occupancy, disordered THF molecule is present about
 a two-fold screw axis (the symmetry operation must be applied to generate
 the full molecule.) Similarity restraints were applied to atoms in that
 molecule. H-atoms for the disordered THF could not be located from
 difference maps, and could not be satisfactorily introduced by
 calculation, and were therefore omitted from the model. They have been
 included in the formula for the calculation of intensive properties.

 Please see _iucr_refine_instructions_details for more information.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1147P)²+8.4711P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7065
_refine_ls_number_parameters     426
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.2275
_refine_ls_wR_factor_gt          0.2156
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.103
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.32935(4) 0.18244(6) 0.08161(5) 0.0359(3) Uani 1 1 d . . .
O1 O 0.24962(7) 0.22594(10) 0.12944(9) 0.0344(4) Uani 1 1 d . . .
O2 O 0.33424(8) 0.20529(11) -0.04160(9) 0.0359(4) Uani 1 1 d D . .
H2 H 0.3061(12) 0.2345(17) -0.0696(16) 0.054 Uiso 1 1 d D . .
O3 O 0.32696(10) 0.39511(13) 0.39183(11) 0.0517(5) Uani 1 1 d . . .
O4 O 0.55403(10) 0.34996(15) -0.03363(14) 0.0621(6) Uani 1 1 d . . .
O5 O 0.32280(10) 0.03961(12) 0.08302(11) 0.0516(5) Uani 1 1 d . . .
O6 O 0.4479(3) 0.5076(3) 0.2580(3) 0.0828(14) Uani 0.50 1 d PU . .
N1 N 0.35610(9) 0.32627(12) 0.09483(11) 0.0320(4) Uani 1 1 d . . .
N2 N 0.43984(10) 0.19524(14) 0.13958(13) 0.0438(5) Uani 1 1 d . . .
C1 C 0.26987(11) 0.26656(14) 0.19410(13) 0.0329(5) Uani 1 1 d . . .
C2 C 0.26097(11) 0.23738(15) 0.26273(14) 0.0357(5) Uani 1 1 d . . .
C3 C 0.28119(12) 0.28411(17) 0.32578(14) 0.0402(6) Uani 1 1 d . . .
H3 H 0.2751 0.2656 0.3717 0.048 Uiso 1 1 calc R . .
C4 C 0.30967(12) 0.35620(16) 0.32452(14) 0.0390(6) Uani 1 1 d . . .
C5 C 0.31945(11) 0.38403(15) 0.25819(14) 0.0363(5) Uani 1 1 d . . .
H5 H 0.3394 0.4333 0.2568 0.044 Uiso 1 1 calc R . .
C6 C 0.29971(11) 0.33915(14) 0.19356(13) 0.0326(5) Uani 1 1 d . . .
C7 C 0.30942(11) 0.37020(14) 0.12143(13) 0.0334(5) Uani 1 1 d . . .
H7A H 0.2705 0.3675 0.0829 0.040 Uiso 1 1 calc R . .
H7B H 0.3215 0.4266 0.1280 0.040 Uiso 1 1 calc R . .
C8 C 0.35682(11) 0.35773(15) 0.02053(13) 0.0346(5) Uani 1 1 d . . .
H8A H 0.3670 0.4149 0.0251 0.042 Uiso 1 1 calc R . .
H8B H 0.3157 0.3524 -0.0132 0.042 Uiso 1 1 calc R . .
C9 C 0.40188(11) 0.31556(15) -0.01328(13) 0.0353(5) Uani 1 1 d . . .
C10 C 0.45646(12) 0.35137(17) -0.01295(14) 0.0407(6) Uani 1 1 d . . .
H10 H 0.4643 0.4040 0.0052 0.049 Uiso 1 1 calc R . .
C11 C 0.49979(13) 0.31104(19) -0.03893(15) 0.0457(6) Uani 1 1 d . . .
C12 C 0.48738(12) 0.23571(18) -0.06760(15) 0.0443(6) Uani 1 1 d . . .
H12 H 0.5175 0.2085 -0.0854 0.053 Uiso 1 1 calc R . .
C13 C 0.43171(12) 0.19814(16) -0.07130(14) 0.0386(6) Uani 1 1 d . . .
C14 C 0.38861(11) 0.23900(15) -0.04299(13) 0.0348(5) Uani 1 1 d . . .
C15 C 0.41579(11) 0.33513(16) 0.14749(14) 0.0363(5) Uani 1 1 d . . .
H15A H 0.4097 0.3390 0.1983 0.044 Uiso 1 1 calc R . .
H15B H 0.4338 0.3858 0.1367 0.044 Uiso 1 1 calc R . .
C16 C 0.46069(11) 0.26977(16) 0.14675(13) 0.0365(5) Uani 1 1 d . . .
C17 C 0.52224(12) 0.28710(18) 0.15946(15) 0.0442(6) Uani 1 1 d . . .
H17 H 0.5356 0.3407 0.1635 0.053 Uiso 1 1 calc R . .
C18 C 0.56364(13) 0.22674(19) 0.16615(16) 0.0491(7) Uani 1 1 d . . .
H18 H 0.6058 0.2379 0.1755 0.059 Uiso 1 1 calc R . .
C19 C 0.54312(14) 0.1504(2) 0.15917(17) 0.0549(8) Uani 1 1 d . . .
H19 H 0.5707 0.1073 0.1639 0.066 Uiso 1 1 calc R . .
C20 C 0.48116(14) 0.13743(19) 0.14509(19) 0.0546(8) Uani 1 1 d . . .
H20 H 0.4671 0.0842 0.1389 0.066 Uiso 1 1 calc R . .
C21 C 0.23116(12) 0.15666(17) 0.26765(14) 0.0416(6) Uani 1 1 d . . .
C22 C 0.26632(14) 0.09122(17) 0.23983(18) 0.0495(7) Uani 1 1 d . . .
H22A H 0.3087 0.0916 0.2691 0.059 Uiso 1 1 calc R . .
H22B H 0.2649 0.1004 0.1873 0.059 Uiso 1 1 calc R . .
H22C H 0.2480 0.0397 0.2453 0.059 Uiso 1 1 calc R . .
C23 C 0.16494(13) 0.15782(19) 0.22197(17) 0.0491(7) Uani 1 1 d . . .
H23A H 0.1455 0.1073 0.2283 0.059 Uiso 1 1 calc R . .
H23B H 0.1637 0.1655 0.1693 0.059 Uiso 1 1 calc R . .
H23C H 0.1433 0.2013 0.2391 0.059 Uiso 1 1 calc R . .
C24 C 0.23068(16) 0.1354(2) 0.34795(17) 0.0584(8) Uani 1 1 d . . .
H24A H 0.2071 0.1751 0.3673 0.070 Uiso 1 1 calc R . .
H24B H 0.2724 0.1345 0.3790 0.070 Uiso 1 1 calc R . .
H24C H 0.2122 0.0831 0.3488 0.070 Uiso 1 1 calc R . .
C25 C 0.36653(15) 0.46062(18) 0.39669(16) 0.0505(7) Uani 1 1 d . . .
H25A H 0.4008 0.4459 0.3764 0.061 Uiso 1 1 calc R . .
H25B H 0.3816 0.4763 0.4489 0.061 Uiso 1 1 calc R . .
H25C H 0.3445 0.5051 0.3682 0.061 Uiso 1 1 calc R . .
C26 C 0.60387(15) 0.3035(3) -0.0418(3) 0.0789(13) Uani 1 1 d . . .
H26A H 0.6101 0.2594 -0.0065 0.095 Uiso 1 1 calc R . .
H26B H 0.6405 0.3364 -0.0321 0.095 Uiso 1 1 calc R . .
H26C H 0.5955 0.2827 -0.0927 0.095 Uiso 1 1 calc R . .
C27 C 0.42017(13) 0.11429(17) -0.10466(16) 0.0436(6) Uani 1 1 d . . .
C28 C 0.47102(16) 0.0859(2) -0.1387(2) 0.0621(9) Uani 1 1 d . . .
H28A H 0.5092 0.0833 -0.0999 0.075 Uiso 1 1 calc R . .
H28B H 0.4755 0.1230 -0.1776 0.075 Uiso 1 1 calc R . .
H28C H 0.4610 0.0331 -0.1604 0.075 Uiso 1 1 calc R . .
C29 C 0.36171(16) 0.1112(2) -0.16594(19) 0.0605(9) Uani 1 1 d . . .
H29A H 0.3568 0.0582 -0.1882 0.073 Uiso 1 1 calc R . .
H29B H 0.3634 0.1506 -0.2042 0.073 Uiso 1 1 calc R . .
H29C H 0.3272 0.1228 -0.1449 0.073 Uiso 1 1 calc R . .
C30 C 0.41652(16) 0.05565(18) -0.04294(19) 0.0564(8) Uani 1 1 d . . .
H30A H 0.4067 0.0028 -0.0644 0.068 Uiso 1 1 calc R . .
H30B H 0.3849 0.0727 -0.0190 0.068 Uiso 1 1 calc R . .
H30C H 0.4557 0.0539 -0.0059 0.068 Uiso 1 1 calc R . .
C31 C 0.28371(15) -0.00948(19) 0.02895(19) 0.0548(7) Uani 1 1 d . . .
H31A H 0.2851 0.0066 -0.0219 0.066 Uiso 1 1 calc R . .
H31B H 0.2413 -0.0051 0.0332 0.066 Uiso 1 1 calc R . .
C32 C 0.30646(19) -0.0930(2) 0.04458(19) 0.0680(10) Uani 1 1 d . . .
H32A H 0.3353 -0.1073 0.0146 0.082 Uiso 1 1 calc R . .
H32B H 0.2725 -0.1315 0.0344 0.082 Uiso 1 1 calc R . .
C33 C 0.3378(2) -0.0901(2) 0.1266(2) 0.0732(11) Uani 1 1 d . . .
H33A H 0.3090 -0.1017 0.1572 0.088 Uiso 1 1 calc R . .
H33B H 0.3718 -0.1286 0.1391 0.088 Uiso 1 1 calc R . .
C34 C 0.3599(2) -0.0097(2) 0.1378(2) 0.0788(12) Uani 1 1 d . . .
H34A H 0.3588 0.0086 0.1881 0.095 Uiso 1 1 calc R . .
H34B H 0.4025 -0.0073 0.1339 0.095 Uiso 1 1 calc R . .
C35 C 0.4549(3) 0.5581(5) 0.1997(5) 0.0683(16) Uani 0.50 1 d PU . .
C36 C 0.5122(6) 0.6129(7) 0.2865(6) 0.105(2) Uani 0.50 1 d PU . .
C37 C 0.4873(4) 0.5472(5) 0.3160(5) 0.0769(17) Uani 0.50 1 d PU . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O1 2.329(2) . ?
Na1 O2 2.350(2) . ?
Na1 O5 2.415(2) . ?
Na1 N2 2.483(3) . ?
Na1 N1 2.499(2) . ?
Na1 C1 3.102(3) . ?
Na1 C14 3.105(3) . ?
O1 C1 1.359(3) . ?
O2 C14 1.367(3) . ?
O2 H2 0.871(18) . ?
O3 C4 1.379(3) . ?
O3 C25 1.414(4) . ?
O4 C11 1.379(3) . ?
O4 C26 1.417(4) . ?
O5 C34 1.418(4) . ?
O5 C31 1.427(4) . ?
O6 C37 1.386(10) . ?
O6 C35 1.418(9) . ?
N1 C15 1.468(3) . ?
N1 C7 1.478(3) . ?
N1 C8 1.482(3) . ?
N2 C16 1.339(4) . ?
N2 C20 1.340(4) . ?
C1 C6 1.401(3) . ?
C1 C2 1.427(3) . ?
C2 C3 1.391(4) . ?
C2 C21 1.534(4) . ?
C3 C4 1.381(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(4) . ?
C5 C6 1.395(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.505(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.508(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.379(4) . ?
C9 C14 1.407(4) . ?
C10 C11 1.380(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.379(4) . ?
C12 C13 1.402(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.404(3) . ?
C13 C27 1.540(4) . ?
C15 C16 1.505(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.391(4) . ?
C17 C18 1.371(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.365(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.527(4) . ?
C21 C23 1.532(4) . ?
C21 C24 1.536(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.519(4) . ?
C27 C28 1.527(4) . ?
C27 C30 1.532(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.505(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.511(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.443(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C37 1.429(10) 2_655 ?
C36 C36 1.33(2) 2_655 ?
C36 C37 1.416(13) . ?
C37 C35 1.429(10) 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
O1 Na1 O2 123.43(7) . . ?
O1 Na1 O5 104.73(7) . . ?
O2 Na1 O5 101.09(7) . . ?
O1 Na1 N2 127.41(8) . . ?
O2 Na1 N2 96.78(8) . . ?
O5 Na1 N2 98.07(8) . . ?
O1 Na1 N1 81.39(7) . . ?
O2 Na1 N1 82.33(7) . . ?
O5 Na1 N1 169.15(8) . . ?
N2 Na1 N1 71.21(8) . . ?
O1 Na1 C1 23.99(6) . . ?
O2 Na1 C1 135.68(7) . . ?
O5 Na1 C1 114.25(7) . . ?
N2 Na1 C1 103.48(8) . . ?
N1 Na1 C1 68.05(7) . . ?
O1 Na1 C14 135.41(7) . . ?
O2 Na1 C14 24.36(6) . . ?
O5 Na1 C14 110.74(7) . . ?
N2 Na1 C14 73.45(8) . . ?
N1 Na1 C14 68.55(7) . . ?
C1 Na1 C14 134.83(7) . . ?
C1 O1 Na1 111.84(14) . . ?
C14 O2 Na1 110.51(14) . . ?
C14 O2 H2 107(2) . . ?
Na1 O2 H2 118(2) . . ?
C4 O3 C25 117.5(2) . . ?
C11 O4 C26 117.0(3) . . ?
C34 O5 C31 108.5(2) . . ?
C34 O5 Na1 124.5(2) . . ?
C31 O5 Na1 126.91(18) . . ?
C37 O6 C35 97.5(6) . . ?
C15 N1 C7 110.38(19) . . ?
C15 N1 C8 111.06(19) . . ?
C7 N1 C8 107.93(18) . . ?
C15 N1 Na1 109.03(15) . . ?
C7 N1 Na1 110.02(14) . . ?
C8 N1 Na1 108.39(14) . . ?
C16 N2 C20 116.9(2) . . ?
C16 N2 Na1 114.81(16) . . ?
C20 N2 Na1 125.7(2) . . ?
O1 C1 C6 119.5(2) . . ?
O1 C1 C2 121.5(2) . . ?
C6 C1 C2 119.0(2) . . ?
C6 C1 Na1 95.81(14) . . ?
C2 C1 Na1 128.82(17) . . ?
C3 C2 C1 117.7(2) . . ?
C3 C2 C21 120.7(2) . . ?
C1 C2 C21 121.5(2) . . ?
C4 C3 C2 122.9(2) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
O3 C4 C3 115.6(2) . . ?
O3 C4 C5 124.8(2) . . ?
C3 C4 C5 119.6(2) . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 121.4(2) . . ?
C5 C6 C7 119.3(2) . . ?
C1 C6 C7 119.3(2) . . ?
N1 C7 C6 113.63(19) . . ?
N1 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
N1 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N1 C8 C9 112.7(2) . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C14 120.5(2) . . ?
C10 C9 C8 119.8(2) . . ?
C14 C9 C8 119.7(2) . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
O4 C11 C12 124.0(3) . . ?
O4 C11 C10 116.4(3) . . ?
C12 C11 C10 119.6(3) . . ?
C11 C12 C13 122.0(2) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
C12 C13 C14 117.8(2) . . ?
C12 C13 C27 119.7(2) . . ?
C14 C13 C27 122.5(2) . . ?
O2 C14 C13 121.5(2) . . ?
O2 C14 C9 118.7(2) . . ?
C13 C14 C9 119.7(2) . . ?
O2 C14 Na1 45.14(10) . . ?
C13 C14 Na1 127.03(17) . . ?
C9 C14 Na1 94.62(14) . . ?
N1 C15 C16 115.8(2) . . ?
N1 C15 H15A 108.3 . . ?
C16 C15 H15A 108.3 . . ?
N1 C15 H15B 108.3 . . ?
C16 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
N2 C16 C17 122.0(2) . . ?
N2 C16 C15 117.7(2) . . ?
C17 C16 C15 120.0(2) . . ?
C18 C17 C16 119.9(3) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C19 C18 C17 118.8(3) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C20 118.4(3) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
N2 C20 C19 124.1(3) . . ?
N2 C20 H20 118.0 . . ?
C19 C20 H20 118.0 . . ?
C22 C21 C23 110.3(2) . . ?
C22 C21 C2 110.2(2) . . ?
C23 C21 C2 110.1(2) . . ?
C22 C21 C24 106.9(2) . . ?
C23 C21 C24 107.2(2) . . ?
C2 C21 C24 112.1(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O3 C25 H25A 109.5 . . ?
O3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O4 C26 H26A 109.5 . . ?
O4 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O4 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29 C27 C28 106.9(3) . . ?
C29 C27 C30 109.7(3) . . ?
C28 C27 C30 107.2(3) . . ?
C29 C27 C13 111.2(2) . . ?
C28 C27 C13 112.6(2) . . ?
C30 C27 C13 109.1(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O5 C31 C32 106.5(3) . . ?
O5 C31 H31A 110.4 . . ?
C32 C31 H31A 110.4 . . ?
O5 C31 H31B 110.4 . . ?
C32 C31 H31B 110.4 . . ?
H31A C31 H31B 108.6 . . ?
C31 C32 C33 102.5(3) . . ?
C31 C32 H32A 111.3 . . ?
C33 C32 H32A 111.3 . . ?
C31 C32 H32B 111.3 . . ?
C33 C32 H32B 111.3 . . ?
H32A C32 H32B 109.2 . . ?
C34 C33 C32 103.6(3) . . ?
C34 C33 H33A 111.0 . . ?
C32 C33 H33A 111.0 . . ?
C34 C33 H33B 111.0 . . ?
C32 C33 H33B 111.0 . . ?
H33A C33 H33B 109.0 . . ?
O5 C34 C33 108.9(3) . . ?
O5 C34 H34A 109.9 . . ?
C33 C34 H34A 109.9 . . ?
O5 C34 H34B 109.9 . . ?
C33 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
C36 C35 O6 119.4(9) 2_655 . ?
C36 C35 C37 65.0(7) 2_655 2_655 ?
O6 C35 C37 111.3(7) . 2_655 ?
O6 C35 C36 80.7(6) . . ?
C37 C35 C36 77.2(7) 2_655 . ?
C35 C36 C36 107.7(9) 2_655 2_655 ?
C35 C36 C37 66.2(8) 2_655 . ?
C36 C36 C37 106.8(9) 2_655 . ?
C35 C36 C35 93.6(9) 2_655 . ?
C37 C36 C35 73.2(6) . . ?
O6 C37 C36 108.7(8) . . ?
O6 C37 C35 110.7(7) . 2_655 ?
C36 C37 C35 48.9(6) . 2_655 ?

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
O2 Na1 O1 C1 -128.70(15) . . . . ?
O5 Na1 O1 C1 116.98(15) . . . . ?
N2 Na1 O1 C1 4.39(19) . . . . ?
N1 Na1 O1 C1 -53.87(15) . . . . ?
C14 Na1 O1 C1 -100.98(17) . . . . ?
O1 Na1 O2 C14 127.66(15) . . . . ?
O5 Na1 O2 C14 -116.24(16) . . . . ?
N2 Na1 O2 C14 -16.60(16) . . . . ?
N1 Na1 O2 C14 53.32(16) . . . . ?
C1 Na1 O2 C14 100.64(17) . . . . ?
O1 Na1 O5 C34 -100.7(3) . . . . ?
O2 Na1 O5 C34 130.1(3) . . . . ?
N2 Na1 O5 C34 31.5(3) . . . . ?
N1 Na1 O5 C34 22.6(6) . . . . ?
C1 Na1 O5 C34 -77.3(3) . . . . ?
C14 Na1 O5 C34 106.8(3) . . . . ?
O1 Na1 O5 C31 81.9(2) . . . . ?
O2 Na1 O5 C31 -47.3(2) . . . . ?
N2 Na1 O5 C31 -145.9(2) . . . . ?
N1 Na1 O5 C31 -154.8(4) . . . . ?
C1 Na1 O5 C31 105.3(2) . . . . ?
C14 Na1 O5 C31 -70.6(2) . . . . ?
O1 Na1 N1 C15 118.17(15) . . . . ?
O2 Na1 N1 C15 -116.19(15) . . . . ?
O5 Na1 N1 C15 -7.0(5) . . . . ?
N2 Na1 N1 C15 -16.31(14) . . . . ?
C1 Na1 N1 C15 97.43(15) . . . . ?
C14 Na1 N1 C15 -95.38(15) . . . . ?
O1 Na1 N1 C7 -3.01(14) . . . . ?
O2 Na1 N1 C7 122.63(15) . . . . ?
O5 Na1 N1 C7 -128.2(4) . . . . ?
N2 Na1 N1 C7 -137.49(16) . . . . ?
C1 Na1 N1 C7 -23.75(14) . . . . ?
C14 Na1 N1 C7 143.44(16) . . . . ?
O1 Na1 N1 C8 -120.82(15) . . . . ?
O2 Na1 N1 C8 4.82(14) . . . . ?
O5 Na1 N1 C8 114.0(4) . . . . ?
N2 Na1 N1 C8 104.70(15) . . . . ?
C1 Na1 N1 C8 -141.55(16) . . . . ?
C14 Na1 N1 C8 25.63(14) . . . . ?
O1 Na1 N2 C16 -65.5(2) . . . . ?
O2 Na1 N2 C16 76.60(19) . . . . ?
O5 Na1 N2 C16 178.87(18) . . . . ?
N1 Na1 N2 C16 -2.89(17) . . . . ?
C1 Na1 N2 C16 -63.71(19) . . . . ?
C14 Na1 N2 C16 69.54(18) . . . . ?
O1 Na1 N2 C20 133.5(2) . . . . ?
O2 Na1 N2 C20 -84.4(3) . . . . ?
O5 Na1 N2 C20 17.9(3) . . . . ?
N1 Na1 N2 C20 -163.9(3) . . . . ?
C1 Na1 N2 C20 135.3(3) . . . . ?
C14 Na1 N2 C20 -91.5(3) . . . . ?
Na1 O1 C1 C6 65.5(2) . . . . ?
Na1 O1 C1 C2 -115.1(2) . . . . ?
O2 Na1 C1 O1 68.80(18) . . . . ?
O5 Na1 C1 O1 -70.96(16) . . . . ?
N2 Na1 C1 O1 -176.41(15) . . . . ?
N1 Na1 C1 O1 120.57(16) . . . . ?
C14 Na1 C1 O1 103.65(16) . . . . ?
O1 Na1 C1 C6 -127.2(2) . . . . ?
O2 Na1 C1 C6 -58.42(18) . . . . ?
O5 Na1 C1 C6 161.82(14) . . . . ?
N2 Na1 C1 C6 56.37(16) . . . . ?
N1 Na1 C1 C6 -6.65(14) . . . . ?
C14 Na1 C1 C6 -23.57(19) . . . . ?
O1 Na1 C1 C2 97.7(3) . . . . ?
O2 Na1 C1 C2 166.52(19) . . . . ?
O5 Na1 C1 C2 26.8(2) . . . . ?
N2 Na1 C1 C2 -78.7(2) . . . . ?
N1 Na1 C1 C2 -141.7(2) . . . . ?
C14 Na1 C1 C2 -158.62(19) . . . . ?
O1 C1 C2 C3 -177.7(2) . . . . ?
C6 C1 C2 C3 1.7(4) . . . . ?
Na1 C1 C2 C3 128.2(2) . . . . ?
O1 C1 C2 C21 3.3(4) . . . . ?
C6 C1 C2 C21 -177.3(2) . . . . ?
Na1 C1 C2 C21 -50.8(3) . . . . ?
C1 C2 C3 C4 -0.7(4) . . . . ?
C21 C2 C3 C4 178.3(2) . . . . ?
C25 O3 C4 C3 167.7(3) . . . . ?
C25 O3 C4 C5 -11.6(4) . . . . ?
C2 C3 C4 O3 -180.0(2) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
O3 C4 C5 C6 -179.9(2) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C4 C5 C6 C1 0.3(4) . . . . ?
C4 C5 C6 C7 178.9(2) . . . . ?
O1 C1 C6 C5 177.9(2) . . . . ?
C2 C1 C6 C5 -1.6(4) . . . . ?
Na1 C1 C6 C5 -142.5(2) . . . . ?
O1 C1 C6 C7 -0.8(3) . . . . ?
C2 C1 C6 C7 179.8(2) . . . . ?
Na1 C1 C6 C7 38.8(2) . . . . ?
C15 N1 C7 C6 -63.8(3) . . . . ?
C8 N1 C7 C6 174.7(2) . . . . ?
Na1 N1 C7 C6 56.6(2) . . . . ?
C5 C6 C7 N1 109.0(3) . . . . ?
C1 C6 C7 N1 -72.3(3) . . . . ?
C15 N1 C8 C9 60.4(3) . . . . ?
C7 N1 C8 C9 -178.5(2) . . . . ?
Na1 N1 C8 C9 -59.3(2) . . . . ?
N1 C8 C9 C10 -103.1(3) . . . . ?
N1 C8 C9 C14 75.1(3) . . . . ?
C14 C9 C10 C11 -2.8(4) . . . . ?
C8 C9 C10 C11 175.4(2) . . . . ?
C26 O4 C11 C12 -15.1(5) . . . . ?
C26 O4 C11 C10 164.4(3) . . . . ?
C9 C10 C11 O4 -177.3(2) . . . . ?
C9 C10 C11 C12 2.2(4) . . . . ?
O4 C11 C12 C13 179.4(3) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
C11 C12 C13 C14 -1.5(4) . . . . ?
C11 C12 C13 C27 179.4(3) . . . . ?
Na1 O2 C14 C13 112.7(2) . . . . ?
Na1 O2 C14 C9 -65.4(2) . . . . ?
C12 C13 C14 O2 -177.2(2) . . . . ?
C27 C13 C14 O2 1.9(4) . . . . ?
C12 C13 C14 C9 0.9(4) . . . . ?
C27 C13 C14 C9 -179.9(2) . . . . ?
C12 C13 C14 Na1 -122.2(2) . . . . ?
C27 C13 C14 Na1 56.9(3) . . . . ?
C10 C9 C14 O2 179.4(2) . . . . ?
C8 C9 C14 O2 1.2(3) . . . . ?
C10 C9 C14 C13 1.2(4) . . . . ?
C8 C9 C14 C13 -177.0(2) . . . . ?
C10 C9 C14 Na1 139.1(2) . . . . ?
C8 C9 C14 Na1 -39.1(2) . . . . ?
O1 Na1 C14 O2 -70.25(18) . . . . ?
O5 Na1 C14 O2 70.25(17) . . . . ?
N2 Na1 C14 O2 162.78(17) . . . . ?
N1 Na1 C14 O2 -121.36(16) . . . . ?
C1 Na1 C14 O2 -104.50(17) . . . . ?
O1 Na1 C14 C13 -170.2(2) . . . . ?
O2 Na1 C14 C13 -99.9(3) . . . . ?
O5 Na1 C14 C13 -29.7(2) . . . . ?
N2 Na1 C14 C13 62.8(2) . . . . ?
N1 Na1 C14 C13 138.7(2) . . . . ?
C1 Na1 C14 C13 155.6(2) . . . . ?
O1 Na1 C14 C9 56.62(18) . . . . ?
O2 Na1 C14 C9 126.9(2) . . . . ?
O5 Na1 C14 C9 -162.88(15) . . . . ?
N2 Na1 C14 C9 -70.35(15) . . . . ?
N1 Na1 C14 C9 5.51(14) . . . . ?
C1 Na1 C14 C9 22.36(19) . . . . ?
C7 N1 C15 C16 155.0(2) . . . . ?
C8 N1 C15 C16 -85.3(3) . . . . ?
Na1 N1 C15 C16 34.0(2) . . . . ?
C20 N2 C16 C17 -0.1(4) . . . . ?
Na1 N2 C16 C17 -162.9(2) . . . . ?
C20 N2 C16 C15 -174.7(2) . . . . ?
Na1 N2 C16 C15 22.5(3) . . . . ?
N1 C15 C16 N2 -40.1(3) . . . . ?
N1 C15 C16 C17 145.2(2) . . . . ?
N2 C16 C17 C18 -1.0(4) . . . . ?
C15 C16 C17 C18 173.5(2) . . . . ?
C16 C17 C18 C19 0.8(4) . . . . ?
C17 C18 C19 C20 0.5(5) . . . . ?
C16 N2 C20 C19 1.5(5) . . . . ?
Na1 N2 C20 C19 162.1(2) . . . . ?
C18 C19 C20 N2 -1.7(5) . . . . ?
C3 C2 C21 C22 -122.0(3) . . . . ?
C1 C2 C21 C22 56.9(3) . . . . ?
C3 C2 C21 C23 116.1(3) . . . . ?
C1 C2 C21 C23 -65.0(3) . . . . ?
C3 C2 C21 C24 -3.1(4) . . . . ?
C1 C2 C21 C24 175.9(3) . . . . ?
C12 C13 C27 C29 -126.6(3) . . . . ?
C14 C13 C27 C29 54.3(3) . . . . ?
C12 C13 C27 C28 -6.7(4) . . . . ?
C14 C13 C27 C28 174.2(3) . . . . ?
C12 C13 C27 C30 112.2(3) . . . . ?
C14 C13 C27 C30 -66.9(3) . . . . ?
C34 O5 C31 C32 -10.7(4) . . . . ?
Na1 O5 C31 C32 167.0(2) . . . . ?
O5 C31 C32 C33 25.8(4) . . . . ?
C31 C32 C33 C34 -31.0(4) . . . . ?
C31 O5 C34 C33 -9.9(5) . . . . ?
Na1 O5 C34 C33 172.3(3) . . . . ?
C32 C33 C34 O5 26.0(5) . . . . ?
C37 O6 C35 C36 0.1(10) . . . 2_655 ?
C37 O6 C35 C37 72.6(7) . . . 2_655 ?
C37 O6 C35 C36 0.3(6) . . . . ?
C36 C35 C36 C35 -116.9(18) 2_655 . . 2_655 ?
O6 C35 C36 C35 63.4(6) . . . 2_655 ?
C37 C35 C36 C35 -51.1(8) 2_655 . . 2_655 ?
O6 C35 C36 C36 -179.7(13) . . . 2_655 ?
C37 C35 C36 C36 65.8(12) 2_655 . . 2_655 ?
C36 C35 C36 C37 179.3(16) 2_655 . . . ?
O6 C35 C36 C37 -0.3(6) . . . . ?
C37 C35 C36 C37 -114.8(8) 2_655 . . . ?
C35 O6 C37 C36 -0.5(8) . . . . ?
C35 O6 C37 C35 -52.6(8) . . . 2_655 ?
C35 C36 C37 O6 -101.5(8) 2_655 . . . ?
C36 C36 C37 O6 0.8(13) 2_655 . . . ?
C35 C36 C37 O6 0.4(6) . . . . ?
C36 C36 C37 C35 102.3(12) 2_655 . . 2_655 ?
C35 C36 C37 C35 101.9(7) . . . 2_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2 H2 O1 . . 7_555 2.467(2) 0.871(18) 1.61(3) 170(3) no

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.061

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene, THF'
_chemical_properties_physical    ', Moisture-sensitive'
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1535026'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.	2020-01-07 downloaded from the CCDC.
;
# start Validation Reply Form

_vrf_THETM01_KDP044              
;
PROBLEM: The value of sine(theta_max)/wavelength
RESPONSE: 2theta was cut-off at 47 degrees. These crystals
diffracted very weakly and no significant diffraction was
observed above this level.
;

_vrf_PLAT029_KDP044              
;
PROBLEM: _diffrn_measured_fraction_theta_full Low
RESPONSE: 2theta was cut-off at 47 degrees. These crystals
diffracted very weakly and no significant diffraction was
observed above this level. Completeness is still significantly above
90%, problems due to truncation of the Fourier map were not observed.
;

_vrf_PLAT340_KDP044              
;
PROBLEM: Low Bond Precision on  C-C Bonds
RESPONSE: The large associated su's on the C-C bonds,
and many of the light atom angles, is the
expected result of the weakly diffracting data-set.
;

_vrf_REFLT03_KDP044              
;
PROBLEM: Reflection count < 95% complete
RESPONSE: 2theta was cut-off at 47 degrees. These crystals
diffracted very weakly and no significant diffraction was
observed above this level. Completeness is still significantly above
90%, problems due to truncation of the Fourier map were not observed.
;

_vrf_RFACG01_KDP044              
;
PROBLEM: The value of the R factor is > 0.10
RESPONSE: The crystal under consideration diffracted weakly
and therefore the high weighted R factor does not indicate 
an incorrect model.
;

_vrf_PLAT082_KDP044              
;
PROBLEM: The value of the R factor is > 0.10
RESPONSE: The crystal under consideration diffracted weakly
and therefore the high weighted R factor does not indicate 
an incorrect model.
;

_vrf_PLAT234_KDP044              
;
PROBLEM: Hirshfeld Test Diff
RESPONSE: Due to weak diffraction some of the light atoms show
some discontinuities in anisotropic displacement. 
The atoms identified by the Hirshfeld Rigid Bond Test were carefully
examined to ensure that they are not the result of an incorrect 
atom-type assignment.
;

_vrf_PLAT241_KDP044              
;
PROBLEM: 
RESPONSE: Due to weak diffraction some of the light atoms show
some discontinuities in anisotropic displacement. 
The atoms identified by the Hirshfeld Rigid Bond Test were carefully
examined to ensure that they are not the result of an incorrect 
atom-type assignment.
;

_vrf_PLAT243_KDP044              
;
PROBLEM: 
RESPONSE: Due to weak diffraction some of the light atoms show
some discontinuities in anisotropic displacement. 
The atoms identified by the Hirshfeld Rigid Bond Test were carefully
examined to ensure that they are not the result of an incorrect 
atom-type assignment.
;

_vrf_PLAT244_KDP044              
;
PROBLEM: 
RESPONSE: Due to weak diffraction some of the light atoms show
some discontinuities in anisotropic displacement. 
The atoms identified by the Hirshfeld Rigid Bond Test were carefully
examined to ensure that they are not the result of an incorrect 
atom-type assignment.
;

_vrf_PLAT355_KDP044              
;
PROBLEM: Long O-H Bond (0.82A)   O2 - H2
RESPONSE: This hydrogen was found in the difference map and
refined freely. (please see iucr_refine_instructions_details for more
information.)
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H39 Li N2 O4, C7 H8'
_chemical_formula_sum            'C37 H47 Li N2 O4'
_chemical_formula_weight         590.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   17.399(7)
_cell_length_b                   12.202(5)
_cell_length_c                   19.503(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 127.700(9)
_cell_angle_gamma                90.00
_cell_volume                     3276(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2358
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.7

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   FS-PROCESS

_exptl_special_details           
; 
 While these were regular crystals in appearance, they
diffracted weakly. 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            8557
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_sigmaI/netI    0.1426
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         23.49
_reflns_number_total             4562
_reflns_number_gt                2424
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_structure_solution    'SHELXS-97 (Acta Cryst.2008, A64, 112-122)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.2008, A64, 112-122)'
_computing_molecular_graphics    'Olex2 v1.2-alpha ()'
_computing_publication_material  'Olex2 v1.2-alpha ()'

_refine_special_details          
; 
 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.

 All hydrogens except H2 were instroduced in calculated positions and
 refined on a riding model. H2 was introduced from its difference map
 position and allowed to refine isotropically and for position. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0359P)²+10.3170P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4562
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2006
_refine_ls_R_factor_gt           0.1163
_refine_ls_wR_factor_ref         0.2396
_refine_ls_wR_factor_gt          0.1988
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.9058(3) 0.6368(3) -0.9763(3) 0.0399(11) Uani 1 1 d . . .
O3 O -0.5644(3) 0.7761(4) -0.9139(3) 0.0459(12) Uani 1 1 d . . .
O2 O -0.9488(3) 0.4138(4) -0.8794(3) 0.0397(12) Uani 1 1 d . . .
O4 O -0.7032(3) 0.0731(4) -0.6713(3) 0.0570(14) Uani 1 1 d . . .
N1 N -0.7828(4) 0.4364(4) -0.8908(3) 0.0338(13) Uani 1 1 d . . .
C20 C -0.8234(4) 0.2841(5) -0.8361(4) 0.0368(17) Uani 1 1 d . . .
C19 C -0.8203(5) 0.3247(5) -0.9069(4) 0.0374(17) Uani 1 1 d . . .
H19A H -0.7793 0.2765 -0.9116 0.045 Uiso 1 1 calc R . .
H19B H -0.8852 0.3225 -0.9616 0.045 Uiso 1 1 calc R . .
C22 C -0.7672(5) 0.1586(5) -0.7213(4) 0.0402(17) Uani 1 1 d . . .
N2 N -0.7659(4) 0.5708(5) -0.7686(3) 0.0439(15) Uani 1 1 d . . .
C14 C -0.6872(5) 0.5098(5) -0.7398(4) 0.0354(16) Uani 1 1 d . . .
C4 C -0.7962(4) 0.7850(5) -0.9500(4) 0.0321(15) Uani 1 1 d . . .
C24 C -0.8896(5) 0.2912(5) -0.7562(4) 0.0382(17) Uani 1 1 d . . .
C3 C -0.8217(5) 0.6709(6) -0.9609(4) 0.0371(17) Uani 1 1 d . . .
C13 C -0.6853(4) 0.4489(6) -0.8059(4) 0.0418(18) Uani 1 1 d . . .
H13A H -0.6433 0.4876 -0.8146 0.050 Uiso 1 1 calc R . .
H13B H -0.6577 0.3767 -0.7833 0.050 Uiso 1 1 calc R . .
C5 C -0.7091(5) 0.8103(5) -0.9359(4) 0.0401(17) Uani 1 1 d . . .
H5 H -0.6913 0.8836 -0.9295 0.048 Uiso 1 1 calc R . .
C1 C -0.7843(5) 0.4739(5) -0.9640(4) 0.0399(17) Uani 1 1 d . . .
H1A H -0.8484 0.4617 -1.0181 0.048 Uiso 1 1 calc R . .
H1B H -0.7382 0.4312 -0.9653 0.048 Uiso 1 1 calc R . .
C7 C -0.6720(4) 0.6251(6) -0.9399(4) 0.0360(16) Uani 1 1 d . . .
H7 H -0.6307 0.5724 -0.9356 0.043 Uiso 1 1 calc R . .
C21 C -0.7635(4) 0.1991(5) -0.7843(4) 0.0390(17) Uani 1 1 d . . .
H21 H -0.7203 0.1693 -0.7923 0.047 Uiso 1 1 calc R . .
C2 C -0.7588(5) 0.5943(5) -0.9555(4) 0.0344(16) Uani 1 1 d . . .
C27 C -0.9563(5) 0.3404(6) -0.7377(4) 0.0419(18) Uani 1 1 d . . .
C28 C -1.0626(5) 0.3141(6) -0.8129(4) 0.054(2) Uani 1 1 d . . .
H28A H -1.0815 0.3537 -0.8636 0.080 Uiso 1 1 calc R . .
H28B H -1.1033 0.3352 -0.7975 0.080 Uiso 1 1 calc R . .
H28C H -1.0693 0.2369 -0.8247 0.080 Uiso 1 1 calc R . .
C23 C -0.8275(5) 0.2045(5) -0.7071(4) 0.0421(18) Uani 1 1 d . . .
H23 H -0.8273 0.1767 -0.6625 0.050 Uiso 1 1 calc R . .
C6 C -0.6489(5) 0.7335(6) -0.9310(4) 0.0408(17) Uani 1 1 d . . .
C12 C -0.4959(5) 0.6992(6) -0.9010(5) 0.053(2) Uani 1 1 d . . .
H12A H -0.4774 0.6508 -0.8543 0.079 Uiso 1 1 calc R . .
H12B H -0.4395 0.7371 -0.8869 0.079 Uiso 1 1 calc R . .
H12C H -0.5242 0.6573 -0.9530 0.079 Uiso 1 1 calc R . .
C25 C -0.8887(4) 0.3312(5) -0.8238(4) 0.0373(17) Uani 1 1 d . . .
C18 C -0.7647(5) 0.6316(6) -0.7111(5) 0.0494(19) Uani 1 1 d . . .
H18 H -0.8187 0.6748 -0.7310 0.059 Uiso 1 1 calc R . .
C10 C -0.9588(5) 0.8739(5) -1.0385(4) 0.053(2) Uani 1 1 d . . .
H10A H -0.9528 0.8860 -1.0837 0.079 Uiso 1 1 calc R . .
H10B H -0.9974 0.9313 -1.0397 0.079 Uiso 1 1 calc R . .
H10C H -0.9897 0.8045 -1.0474 0.079 Uiso 1 1 calc R . .
C9 C -0.8652(5) 0.8516(6) -0.8782(5) 0.058(2) Uani 1 1 d . . .
H9A H -0.8939 0.7808 -0.8863 0.087 Uiso 1 1 calc R . .
H9B H -0.9047 0.9068 -0.8784 0.087 Uiso 1 1 calc R . .
H9C H -0.8012 0.8531 -0.8237 0.087 Uiso 1 1 calc R . .
C8 C -0.8588(5) 0.8738(5) -0.9514(4) 0.0436(18) Uani 1 1 d . . .
C15 C -0.6073(5) 0.5097(6) -0.6523(5) 0.058(2) Uani 1 1 d . . .
H15 H -0.5529 0.4675 -0.6328 0.070 Uiso 1 1 calc R . .
C11 C -0.8161(5) 0.9876(5) -0.9382(5) 0.061(2) Uani 1 1 d . . .
H11A H -0.7522 0.9903 -0.8837 0.091 Uiso 1 1 calc R . .
H11B H -0.8569 1.0408 -0.9385 0.091 Uiso 1 1 calc R . .
H11C H -0.8122 1.0035 -0.9843 0.091 Uiso 1 1 calc R . .
C16 C -0.6098(6) 0.5730(7) -0.5947(5) 0.075(3) Uani 1 1 d . . .
H16 H -0.5574 0.5734 -0.5360 0.090 Uiso 1 1 calc R . .
C30 C -0.9359(5) 0.2910(7) -0.6558(5) 0.061(2) Uani 1 1 d . . .
H30A H -0.9474 0.2134 -0.6634 0.092 Uiso 1 1 calc R . .
H30B H -0.9781 0.3241 -0.6455 0.092 Uiso 1 1 calc R . .
H30C H -0.8695 0.3045 -0.6071 0.092 Uiso 1 1 calc R . .
C29 C -0.9417(6) 0.4630(6) -0.7234(5) 0.063(2) Uani 1 1 d . . .
H29A H -0.8756 0.4780 -0.6748 0.095 Uiso 1 1 calc R . .
H29B H -0.9844 0.4915 -0.7120 0.095 Uiso 1 1 calc R . .
H29C H -0.9560 0.4974 -0.7743 0.095 Uiso 1 1 calc R . .
C17 C -0.6890(6) 0.6340(6) -0.6250(5) 0.060(2) Uani 1 1 d . . .
H17 H -0.6920 0.6773 -0.5874 0.072 Uiso 1 1 calc R . .
C26 C -0.7278(6) 0.0020(7) -0.6319(6) 0.076(3) Uani 1 1 d . . .
H26A H -0.7162 0.0370 -0.5823 0.114 Uiso 1 1 calc R . .
H26B H -0.6889 -0.0632 -0.6139 0.114 Uiso 1 1 calc R . .
H26C H -0.7953 -0.0171 -0.6724 0.114 Uiso 1 1 calc R . .
Li1 Li -0.8788(7) 0.5318(9) -0.8899(7) 0.040(3) Uani 1 1 d . . .
C37 C -0.4761(6) 0.7158(8) -0.6833(6) 0.072(3) Uani 1 1 d . . .
H37 H -0.5081 0.7146 -0.7427 0.087 Uiso 1 1 calc R . .
C33 C -0.4404(7) 0.8011(9) -0.5586(6) 0.077(3) Uani 1 1 d . . .
H33 H -0.4466 0.8591 -0.5314 0.093 Uiso 1 1 calc R . .
C32 C -0.4940(6) 0.8009(7) -0.6501(6) 0.072(3) Uani 1 1 d . . .
C35 C -0.3641(6) 0.6334(10) -0.5467(7) 0.088(3) Uani 1 1 d . . .
H35 H -0.3200 0.5780 -0.5124 0.106 Uiso 1 1 calc R . .
C34 C -0.3802(7) 0.7165(11) -0.5111(7) 0.100(4) Uani 1 1 d . . .
H34 H -0.3487 0.7155 -0.4517 0.120 Uiso 1 1 calc R . .
C36 C -0.4150(7) 0.6331(9) -0.6355(7) 0.091(3) Uani 1 1 d . . .
H36 H -0.4069 0.5759 -0.6621 0.110 Uiso 1 1 calc R . .
C31 C -0.5591(7) 0.8893(9) -0.7007(7) 0.116(4) Uani 1 1 d . . .
H31A H -0.5274 0.9408 -0.7131 0.173 Uiso 1 1 calc R . .
H31B H -0.5775 0.9253 -0.6689 0.173 Uiso 1 1 calc R . .
H31C H -0.6161 0.8611 -0.7540 0.173 Uiso 1 1 calc R . .
H2 H -1.010(6) 0.387(7) -0.937(6) 0.10(3) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C3 1.365(7) . ?
O1 Li1 1.932(11) . ?
O3 C6 1.394(7) . ?
O3 C12 1.414(7) . ?
O2 C25 1.377(7) . ?
O2 Li1 1.976(12) . ?
O4 C26 1.388(8) . ?
O4 C22 1.397(7) . ?
N1 C19 1.459(7) . ?
N1 C1 1.484(7) . ?
N1 C13 1.486(7) . ?
N1 Li1 2.044(12) . ?
C20 C21 1.377(9) . ?
C20 C25 1.418(8) . ?
C20 C19 1.500(8) . ?
C22 C23 1.359(9) . ?
C22 C21 1.362(9) . ?
N2 C18 1.334(8) . ?
N2 C14 1.343(8) . ?
N2 Li1 2.000(12) . ?
C14 C15 1.394(9) . ?
C14 C13 1.506(9) . ?
C4 C5 1.400(8) . ?
C4 C3 1.437(9) . ?
C4 C8 1.524(8) . ?
C24 C23 1.392(9) . ?
C24 C25 1.414(9) . ?
C24 C27 1.533(9) . ?
C3 C2 1.393(8) . ?
C5 C6 1.365(9) . ?
C1 C2 1.515(9) . ?
C7 C6 1.363(9) . ?
C7 C2 1.398(8) . ?
C27 C29 1.515(9) . ?
C27 C30 1.532(9) . ?
C27 C28 1.536(9) . ?
C18 C17 1.361(9) . ?
C10 C8 1.517(9) . ?
C9 C8 1.523(9) . ?
C8 C11 1.520(9) . ?
C15 C16 1.385(10) . ?
C16 C17 1.344(10) . ?
C37 C36 1.344(11) . ?
C37 C32 1.357(11) . ?
C33 C34 1.354(13) . ?
C33 C32 1.420(11) . ?
C32 C31 1.433(11) . ?
C35 C34 1.352(13) . ?
C35 C36 1.380(12) . ?

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
C3 O1 Li1 110.7(5) . . ?
C6 O3 C12 116.5(5) . . ?
C25 O2 Li1 113.3(5) . . ?
C26 O4 C22 118.0(5) . . ?
C19 N1 C1 109.7(5) . . ?
C19 N1 C13 113.0(5) . . ?
C1 N1 C13 112.1(5) . . ?
C19 N1 Li1 105.9(5) . . ?
C1 N1 Li1 107.4(5) . . ?
C13 N1 Li1 108.3(5) . . ?
C21 C20 C25 120.5(6) . . ?
C21 C20 C19 119.1(6) . . ?
C25 C20 C19 120.4(6) . . ?
N1 C19 C20 111.9(5) . . ?
C23 C22 C21 120.3(6) . . ?
C23 C22 O4 123.3(6) . . ?
C21 C22 O4 116.4(6) . . ?
C18 N2 C14 118.0(6) . . ?
C18 N2 Li1 128.7(6) . . ?
C14 N2 Li1 112.0(5) . . ?
N2 C14 C15 120.7(6) . . ?
N2 C14 C13 117.8(6) . . ?
C15 C14 C13 121.3(6) . . ?
C5 C4 C3 116.2(6) . . ?
C5 C4 C8 121.5(6) . . ?
C3 C4 C8 122.3(6) . . ?
C23 C24 C25 117.3(6) . . ?
C23 C24 C27 121.0(6) . . ?
C25 C24 C27 121.7(6) . . ?
O1 C3 C2 119.9(6) . . ?
O1 C3 C4 121.4(6) . . ?
C2 C3 C4 118.8(6) . . ?
N1 C13 C14 113.4(5) . . ?
C6 C5 C4 123.7(6) . . ?
N1 C1 C2 111.2(5) . . ?
C6 C7 C2 119.0(6) . . ?
C22 C21 C20 120.1(6) . . ?
C3 C2 C7 122.0(6) . . ?
C3 C2 C1 118.6(6) . . ?
C7 C2 C1 119.3(6) . . ?
C29 C27 C30 106.9(6) . . ?
C29 C27 C24 111.4(6) . . ?
C30 C27 C24 111.5(6) . . ?
C29 C27 C28 110.5(6) . . ?
C30 C27 C28 106.8(6) . . ?
C24 C27 C28 109.7(5) . . ?
C22 C23 C24 122.9(6) . . ?
C7 C6 C5 120.2(6) . . ?
C7 C6 O3 125.4(6) . . ?
C5 C6 O3 114.4(6) . . ?
O2 C25 C24 123.4(6) . . ?
O2 C25 C20 117.7(6) . . ?
C24 C25 C20 118.9(6) . . ?
N2 C18 C17 123.7(7) . . ?
C10 C8 C11 107.2(6) . . ?
C10 C8 C9 111.0(6) . . ?
C11 C8 C9 108.2(6) . . ?
C10 C8 C4 109.8(5) . . ?
C11 C8 C4 112.1(6) . . ?
C9 C8 C4 108.5(5) . . ?
C16 C15 C14 119.3(7) . . ?
C17 C16 C15 119.0(8) . . ?
C16 C17 C18 119.3(7) . . ?
O1 Li1 O2 137.5(6) . . ?
O1 Li1 N2 114.4(6) . . ?
O2 Li1 N2 105.8(5) . . ?
O1 Li1 N1 97.7(5) . . ?
O2 Li1 N1 98.3(5) . . ?
N2 Li1 N1 85.9(4) . . ?
C36 C37 C32 124.0(9) . . ?
C34 C33 C32 119.8(10) . . ?
C37 C32 C33 115.8(9) . . ?
C37 C32 C31 124.2(9) . . ?
C33 C32 C31 120.0(9) . . ?
C34 C35 C36 118.1(10) . . ?
C35 C34 C33 122.5(10) . . ?
C37 C36 C35 119.8(10) . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        23.49
_diffrn_measured_fraction_theta_full 0.943
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.059


#===END



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene, pentane'
_chemical_properties_physical    ', Moisture-sensitive'
