# 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_LiSCN-THF
_database_code_depnum_ccdc_archive 'CCDC 2091209'
loop_
_audit_author_name
_audit_author_address
'Sebastian Bette'
;Max Planck Institute for Solid State Research
Germany
;
_audit_update_record             
;
2021-06-21 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_POWD002_LiSCN-THF           
;
PROBLEM: refine_ls_goodness_of_fit_all is missing (this is chi, i.e.
         the square root of 'chi squared'). This should be
         present for a powder diffraction study.
RESPONSE: 
We did not report any GOF, as its definition is not suitable for up-to-date 
detectors. Modern point sensitive Mythen detectors (the devices we used) 
provide large global and local count rates, smooth intensity distribution 
with little statistical fluctuations and a high dynamic range; therefore 
weak reflections can be accurately measure in proximity of strong peaks. 
In addition, these devices are almost noise free. Accordingly, the powder 
pattern is treated by the software like if the scan time was far too long, 
although the applied scan time was moderate (see Table S1 in the supporting 
information). This leads to an artificial high GOF value, even for good 
fits. Hence, we reported Rwp-, are R-F\^A^2^- and R-p-values as well as a figure
(Table S1) showing the fit of the whole powder pattern as the quality of 
the refinement might be better judged be these criteria. This problem is 
well known to powder diffractionists using a synchrotron beam line source 
and a 2D image plate detector or an array of Mythen detectors.
;
_vrf_PLAT043_LiSCN-THF           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by .. 8.07 Check
RESPONSE: 
According to the limits of the XRPD method, we did not do any attempt to 
determine and refine the hydrogen positions. Accordingly, hydrogens related 
to water or THF were not included into the cif 
files. Accordingly, hydrogen atoms that are apparent in the solid phase are 
not included into the cif-file. That is why there is a difference between 
the reported and calculated molar mass (PLAT043 ALERT 1 B).
;

# end Validation Reply Form

_audit_creation_method           TOPAS

_chemical_name_common            'Li(SCN) THF'
_chemical_formula_moiety         '(C4 H8 O), (C N S), Li'
_chemical_formula_sum            'C5 H8 Li N O S'
_chemical_formula_weight         137.13


_cell_length_a                   5.74437(17)
_cell_length_b                   16.4318(4)
_cell_length_c                   8.3018(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.0090(10)
_cell_angle_gamma                90
_cell_volume                     773.94(4)
_symmetry_space_group_name_H-M   P21/c
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14

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

_cell_formula_units_Z            4
_cell_measurement_temperature    295

_exptl_crystal_description       'microcrystalline powder'
_exptl_crystal_colour            white

_exptl_crystal_density_diffrn    1.18

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Li1 Li+1 4 e 1.085(7) 0.989(3) 0.360(6) 1 1.5(3)
C11 C 4 e 0.605(4) 0.9195(8) 0.3712(14) 1 1.5(3)
N11 N 4 e 0.782(3) 0.9536(5) 0.3968(12) 1 1.5(3)
S11 S 4 e 0.352(5) 0.8708(10) 0.3348(19) 1 1.5(3)
O1a O-2 4 e 0.890(2) 0.9247(7) 0.7953(14) 0.53(3) 1.5(3)
C1a C 4 e 1.078(7) 0.867(3) 0.856(5) 0.53(3) 1.5(3)
C2a C 4 e 0.677(6) 0.899(3) 0.857(6) 0.53(3) 1.5(3)
C3a C 4 e 0.752(17) 0.836(4) 0.984(9) 0.53(3) 1.5(3)
C4a C 4 e 0.962(15) 0.796(3) 0.924(11) 0.53(3) 1.5(3)
O1b O-2 4 e 0.890(2) 0.9247(7) 0.7953(14) 0.47(3) 1.5(3)
C1b C 4 e 0.957(15) 0.8399(14) 0.773(7) 0.47(3) 1.5(3)
C2b C 4 e 0.740(7) 0.927(3) 0.922(4) 0.47(3) 1.5(3)
C3b C 4 e 0.760(17) 0.844(4) 1.001(9) 0.47(3) 1.5(3)
C4b C 4 e 0.80(2) 0.789(2) 0.862(13) 0.47(3) 1.5(3)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_multiplicity
Li1 Nii 1.90(3) 4

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_2
_geom_angle_site_symmetry_3
N11 C11 S11 180(0) 1_555 1_555 1_555

# Powder diffraction data for histogram  1
#==============================================================================

# 4. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
;
 ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; 
'Stoe Stadi P, Debye-Scherrer mode, MPI-FKF, Stuttgart, Germany'
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; 
'Standard Reference Materials NIST SRM640c (Silicon powder)'
;

_diffrn_ambient_temperature      295
_diffrn_source                   ?
_diffrn_source_target            ?
_diffrn_source_type              Cu-tube
_diffrn_measurement_device_type  Stoe-Stadi-P
_diffrn_detector                 
; 
 Lynx Eye 1mm  
;
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             step
_pd_meas_special_details         
;  ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     binning

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  'Johannson Ge(111) primary beam monochromator'

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 5. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; 
'0.5 mm glass capillary'
;

_pd_spec_mount_mode              transmission

_pd_spec_shape                   cylinder

_diffrn_radiation_probe          X-ray
_diffrn_radiation_wavelength     1.5406
_diffrn_radiation_type           'Cu K\a'
_refine_ls_number_parameters     50
_pd_proc_ls_prof_R_factor        0.0146
_pd_proc_ls_prof_wR_factor       0.0197
_pd_proc_ls_prof_wR_expected     0.0006
_refine_ls_R_Fsqd_factor         0.0179
_pd_proc_ls_background_function  
;   
'Chebyshev polynomial'
;

_exptl_absorpt_process_details   
;   
 ?
;
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_pd_proc_ls_profile_function     
;
 Fundamental parameters
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_info_datetime           ?
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        5.0
_pd_meas_2theta_range_max        110.0
_pd_meas_2theta_range_inc        0.015
_pd_proc_2theta_range_min        10.0
_pd_proc_2theta_range_max        100.0
_pd_proc_2theta_range_inc        0.015

#====================================================================== 	 
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    
Moisture-sensitive,Hygroscopic,Deliquescent,Heat-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_liscnthf
_database_code_depnum_ccdc_archive 'CCDC 2091745'
loop_
_audit_author_name
_audit_author_address
'Maurice Conrad'
;University of Stuttgart
Germany
;
_audit_update_record             
;
2021-06-23 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT201_liscnthf            
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          5 Report
RESPONSE: We decided to refine any disordered solvent molecules isotropically.
;
# Added during the CSD deposition process: Wednesday 23 June 2021 02:25 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        'lithium thiocyanate ditetrahydrofuranate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H16 Li N O2 S'
_chemical_formula_weight         209.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   11.3273(6)
_cell_length_b                   16.3798(9)
_cell_length_c                   12.6486(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.393(3)
_cell_angle_gamma                90.00
_cell_volume                     2339.9(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    151766
_cell_measurement_theta_min      1.80
_cell_measurement_theta_max      31.35

_exptl_crystal_description       lath-shaped
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.936
_exptl_crystal_size_mid          0.611
_exptl_crystal_size_min          0.492
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  0.885


_exptl_special_details           
; 
 ? 
;

_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'

_diffrn_detector                 Pilatus200K
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_detector_area_resol_mean 5.81

_diffrn_source                   Mo-Genix
_diffrn_source_type              ?
_diffrn_radiation_probe          x-ray
_diffrn_source_target            ?
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'

_diffrn_ambient_temperature      100(2)

_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 4441 frames, detector distance = 60 mm
;

_diffrn_reflns_number            182393
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         31.88
_reflns_number_total             7860
_reflns_number_gt                5631
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_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)+(0.0610P)²+0.2412P] 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         7860
_refine_ls_number_parameters     273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1159
_refine_ls_wR_factor_gt          0.1079
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.42174(17) 0.56407(12) 0.24964(14) 0.0261(4) Uani 1 1 d . . .
Li2 Li 0.90798(17) 0.95266(11) 0.23504(15) 0.0260(4) Uani 1 1 d . . .
S1 S 0.75844(3) 0.179277(19) 0.07862(3) 0.03705(9) Uani 1 1 d . . .
C1 C 0.85265(9) 0.11128(6) 0.12662(8) 0.0221(2) Uani 1 1 d . . .
N1 N 0.91947(9) 0.06172(6) 0.16038(7) 0.02593(19) Uani 1 1 d . . .
S2 S 0.22074(3) 0.36372(2) 0.11979(3) 0.04151(10) Uani 1 1 d . . .
C2 C 0.34175(10) 0.41150(6) 0.16085(8) 0.0237(2) Uani 1 1 d . . .
N2 N 0.42845(9) 0.44603(6) 0.18994(7) 0.0279(2) Uani 1 1 d . . .
O1 O 0.21159(7) 0.07399(5) 0.16768(6) 0.02748(17) Uani 1 1 d . . .
C11 C 0.32383(10) 0.11500(8) 0.18965(9) 0.0313(2) Uani 1 1 d . . .
H111 H 0.3481 0.1129 0.2648 0.045(4) Uiso 1 1 calc R . .
H112 H 0.3180 0.1717 0.1679 0.047(4) Uiso 1 1 calc R . .
C12 C 0.41188(10) 0.06980(8) 0.12638(10) 0.0333(3) Uani 1 1 d . . .
H121 H 0.4500 0.0258 0.1674 0.039(4) Uiso 1 1 calc R . .
H122 H 0.4720 0.1064 0.1030 0.051(5) Uiso 1 1 calc R . .
C13 C 0.33335(11) 0.03711(8) 0.03300(9) 0.0307(2) Uani 1 1 d . . .
H131 H 0.3163 0.0789 -0.0204 0.035(4) Uiso 1 1 calc R . .
H132 H 0.3691 -0.0096 0.0007 0.040(4) Uiso 1 1 calc R . .
C14 C 0.22349(11) 0.01301(7) 0.08596(9) 0.0296(2) Uani 1 1 d . . .
H141 H 0.1547 0.0132 0.0353 0.039(4) Uiso 1 1 calc R . .
H142 H 0.2324 -0.0410 0.1169 0.037(4) Uiso 1 1 calc R . .
O2 O 0.43625(7) 0.64998(5) 0.14896(6) 0.02572(16) Uani 1 1 d . . .
C21 C 0.54114(11) 0.65561(7) 0.09056(9) 0.0306(2) Uani 1 1 d . . .
H211 H 0.5383 0.6159 0.0335 0.038(4) Uiso 1 1 calc R . .
H212 H 0.6120 0.6463 0.1370 0.035(4) Uiso 1 1 calc R . .
C22 C 0.53931(12) 0.74156(8) 0.04710(11) 0.0388(3) Uani 1 1 d . . .
H221 H 0.4890 0.7456 -0.0183 0.053(5) Uiso 1 1 calc R . .
H222 H 0.6184 0.7602 0.0347 0.046(4) Uiso 1 1 calc R . .
C23 C 0.48859(13) 0.78938(8) 0.13569(12) 0.0421(3) Uani 1 1 d . . .
H231 H 0.4518 0.8397 0.1094 0.056(5) Uiso 1 1 calc R . .
H232 H 0.5493 0.8022 0.1915 0.063(5) Uiso 1 1 calc R . .
C24 C 0.39750(12) 0.73086(8) 0.17445(11) 0.0382(3) Uani 1 1 d . . .
H241 H 0.3929 0.7365 0.2504 0.055(5) Uiso 1 1 calc R . .
H242 H 0.3200 0.7419 0.1394 0.062(5) Uiso 1 1 calc R . .
O3 O 0.71652(7) 0.45839(5) 0.17214(6) 0.02860(18) Uani 1 1 d . . .
C31 C 0.83384(10) 0.48458(8) 0.21017(9) 0.0294(2) Uani 1 1 d . . .
H311 H 0.8682 0.4467 0.2628 0.045(4) Uiso 1 1 calc R . .
H312 H 0.8310 0.5383 0.2421 0.035(4) Uiso 1 1 calc R . .
C32 C 0.90606(12) 0.48662(9) 0.11471(10) 0.0376(3) Uani 1 1 d . . .
H321 H 0.9884 0.4734 0.1338 0.078(6) Uiso 1 1 calc R . .
H322 H 0.9013 0.5395 0.0801 0.049(4) Uiso 1 1 calc R . .
C33 C 0.84567(14) 0.42057(9) 0.04510(11) 0.0459(3) Uani 1 1 d . . .
H331 H 0.8590 0.4290 -0.0290 0.073(6) Uiso 1 1 calc R . .
H332 H 0.8738 0.3667 0.0666 0.069(6) Uiso 1 1 calc R . .
C34 C 0.71681(12) 0.43101(8) 0.06385(9) 0.0345(3) Uani 1 1 d . . .
H341 H 0.6799 0.4712 0.0156 0.049(4) Uiso 1 1 calc R . .
H342 H 0.6747 0.3797 0.0540 0.044(4) Uiso 1 1 calc R . .
O4A O 0.87000(17) 0.85763(11) 0.14122(15) 0.0227(5) Uiso 0.653(4) 1 d P A 1
C41A C 0.85493(19) 0.78900(12) 0.2145(2) 0.0288(4) Uiso 0.653(4) 1 d P A 1
H41A H 0.7720 0.7808 0.2256 0.035 Uiso 0.653(4) 1 calc PR A 1
H41B H 0.8983 0.7986 0.2824 0.035 Uiso 0.653(4) 1 calc PR A 1
C42A C 0.90424(19) 0.71697(12) 0.15952(17) 0.0341(5) Uiso 0.653(4) 1 d P A 1
H42A H 0.9363 0.6770 0.2105 0.041 Uiso 0.653(4) 1 calc PR A 1
H42B H 0.8438 0.6912 0.1123 0.041 Uiso 0.653(4) 1 calc PR A 1
C43A C 0.9987(3) 0.75232(16) 0.0992(2) 0.0442(6) Uiso 0.653(4) 1 d P A 1
H43A H 1.0136 0.7186 0.0386 0.053 Uiso 0.653(4) 1 calc PR A 1
H43B H 1.0717 0.7587 0.1438 0.053 Uiso 0.653(4) 1 calc PR A 1
C44A C 0.9483(2) 0.83394(14) 0.06472(19) 0.0305(6) Uiso 0.653(4) 1 d P A 1
H44A H 1.0111 0.8738 0.0611 0.037 Uiso 0.653(4) 1 calc PR A 1
H44B H 0.9060 0.8296 -0.0047 0.037 Uiso 0.653(4) 1 calc PR A 1
O4B O 0.8893(3) 0.8615(2) 0.1527(3) 0.0254(9) Uiso 0.347(4) 1 d P . 2
C41B C 0.8357(4) 0.7829(2) 0.1807(4) 0.0314(9) Uiso 0.347(4) 1 d P . 2
H41C H 0.7870 0.7598 0.1218 0.038 Uiso 0.347(4) 1 calc PR A 2
H41D H 0.7898 0.7877 0.2421 0.038 Uiso 0.347(4) 1 calc PR A 2
C42B C 0.9507(4) 0.7343(2) 0.2053(3) 0.0365(10) Uiso 0.347(4) 1 d P . 2
H42C H 0.9839 0.7451 0.2770 0.044 Uiso 0.347(4) 1 calc PR A 2
H42D H 0.9365 0.6762 0.1975 0.044 Uiso 0.347(4) 1 calc PR A 2
C43B C 0.0314(3) 0.7640(2) 0.1258(3) 0.0237(7) Uiso 0.347(4) 1 d P . 2
H43C H 0.1091 0.7758 0.1601 0.028 Uiso 0.347(4) 1 calc PR A 2
H43D H 0.0400 0.7227 0.0720 0.028 Uiso 0.347(4) 1 calc PR A 2
C44B C 0.9780(4) 0.8394(2) 0.0767(3) 0.0226(9) Uiso 0.347(4) 1 d P . 2
H44C H 1.0368 0.8821 0.0720 0.027 Uiso 0.347(4) 1 calc PR A 2
H44D H 0.9405 0.8286 0.0066 0.027 Uiso 0.347(4) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Li1 0.0260(9) 0.0285(9) 0.0245(9) 0.0022(7) 0.0064(7) 0.0007(7)
Li2 0.0239(9) 0.0276(9) 0.0268(9) 0.0015(7) 0.0052(7) 0.0004(7)
S1 0.04235(18) 0.03323(16) 0.03640(17) 0.00483(12) 0.00835(13) 0.01600(13)
C1 0.0259(5) 0.0237(5) 0.0175(4) -0.0013(4) 0.0067(4) -0.0025(4)
N1 0.0287(5) 0.0282(4) 0.0211(4) 0.0019(3) 0.0035(4) 0.0003(4)
S2 0.03148(17) 0.0500(2) 0.04216(18) 0.00727(14) -0.00278(14) -0.01727(14)
C2 0.0260(5) 0.0246(5) 0.0209(5) 0.0030(4) 0.0053(4) 0.0013(4)
N2 0.0270(5) 0.0310(5) 0.0259(4) -0.0034(4) 0.0044(4) -0.0026(4)
O1 0.0241(4) 0.0326(4) 0.0268(4) -0.0090(3) 0.0093(3) -0.0051(3)
C11 0.0245(5) 0.0418(6) 0.0279(5) -0.0073(5) 0.0043(4) -0.0082(5)
C12 0.0224(5) 0.0455(7) 0.0323(6) 0.0023(5) 0.0047(4) 0.0014(5)
C13 0.0316(6) 0.0359(6) 0.0261(5) -0.0011(4) 0.0114(5) 0.0020(5)
C14 0.0314(6) 0.0319(6) 0.0264(5) -0.0091(4) 0.0090(4) -0.0033(5)
O2 0.0278(4) 0.0269(4) 0.0235(4) 0.0026(3) 0.0087(3) 0.0018(3)
C21 0.0301(6) 0.0349(6) 0.0284(5) 0.0071(4) 0.0131(5) 0.0035(5)
C22 0.0350(7) 0.0405(7) 0.0420(7) 0.0157(6) 0.0111(5) -0.0002(5)
C23 0.0423(7) 0.0287(6) 0.0553(8) 0.0015(6) 0.0041(6) -0.0029(5)
C24 0.0438(7) 0.0292(6) 0.0438(7) 0.0019(5) 0.0181(6) 0.0071(5)
O3 0.0246(4) 0.0405(4) 0.0215(4) -0.0067(3) 0.0070(3) -0.0065(3)
C31 0.0225(5) 0.0379(6) 0.0281(5) -0.0014(5) 0.0045(4) -0.0042(4)
C32 0.0318(6) 0.0453(7) 0.0379(6) -0.0022(5) 0.0159(5) -0.0036(5)
C33 0.0583(9) 0.0430(7) 0.0401(7) -0.0124(6) 0.0284(7) -0.0045(7)
C34 0.0462(7) 0.0383(6) 0.0194(5) -0.0040(4) 0.0054(5) -0.0082(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Li1 O1 1.9087(19) 2 ?
Li1 O2 1.913(2) . ?
Li1 N1 2.054(2) 2_655 ?
Li1 N2 2.079(2) . ?
Li1 Li2 2.652(3) 2_645 ?
Li2 O4B 1.823(4) . ?
Li2 O3 1.9053(19) 2_655 ?
Li2 O4A 1.984(3) . ?
Li2 N2 2.019(2) 2_655 ?
Li2 N1 2.029(2) 1_565 ?
Li2 Li1 2.652(3) 2_655 ?
Li2 C41A 2.755(3) . ?
S1 C1 1.6275(11) . ?
C1 N1 1.1682(14) . ?
N1 Li2 2.029(2) 1_545 ?
N1 Li1 2.054(2) 2_645 ?
S2 C2 1.6286(11) . ?
C2 N2 1.1680(14) . ?
N2 Li2 2.019(2) 2_645 ?
O1 C11 1.4460(13) . ?
O1 C14 1.4510(13) . ?
O1 Li1 1.9087(19) 2_545 ?
C11 C12 1.5184(17) . ?
C12 C13 1.5205(17) . ?
C13 C14 1.5102(16) . ?
O2 C24 1.4400(14) . ?
O2 C21 1.4491(13) . ?
C21 C22 1.5110(17) . ?
C22 C23 1.516(2) . ?
C23 C24 1.5170(18) . ?
O3 C34 1.4415(13) . ?
O3 C31 1.4434(13) . ?
O3 Li2 1.905(2) 2_645 ?
C31 C32 1.5098(16) . ?
C32 C33 1.5235(19) . ?
C33 C34 1.506(2) . ?
O4A C44A 1.416(3) . ?
O4A C41A 1.475(3) . ?
C41A C42A 1.499(3) . ?
C42A C43A 1.479(3) . ?
C43A C44A 1.505(3) . ?
O4B C41B 1.477(5) . ?
O4B C44B 1.488(5) . ?
C41B C42B 1.538(6) . ?
C42B C43B 1.492(5) 1_655 ?
C43B C44B 1.490(5) 1_455 ?
C43B C42B 1.492(5) 1_455 ?
C44B C43B 1.490(5) 1_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 Li1 O2 114.46(10) 2 . ?
O1 Li1 N1 113.21(9) 2 2_655 ?
O2 Li1 N1 105.45(9) . 2_655 ?
O1 Li1 N2 109.31(10) 2 . ?
O2 Li1 N2 115.77(9) . . ?
N1 Li1 N2 97.41(9) 2_655 . ?
O1 Li1 Li2 128.33(10) 2 2_645 ?
O2 Li1 Li2 117.11(9) . 2_645 ?
N1 Li1 Li2 49.11(6) 2_655 2_645 ?
N2 Li1 Li2 48.69(6) . 2_645 ?
O4B Li2 O3 109.47(15) . 2_655 ?
O4B Li2 O4A 6.19(15) . . ?
O3 Li2 O4A 105.69(11) 2_655 . ?
O4B Li2 N2 106.66(15) . 2_655 ?
O3 Li2 N2 114.14(10) 2_655 2_655 ?
O4A Li2 N2 112.83(11) . 2_655 ?
O4B Li2 N1 117.64(15) . 1_565 ?
O3 Li2 N1 108.67(10) 2_655 1_565 ?
O4A Li2 N1 115.52(11) . 1_565 ?
N2 Li2 N1 100.18(9) 2_655 1_565 ?
O4B Li2 Li1 131.10(15) . 2_655 ?
O3 Li2 Li1 119.32(10) 2_655 2_655 ?
O4A Li2 Li1 134.97(11) . 2_655 ?
N2 Li2 Li1 50.68(7) 2_655 2_655 ?
N1 Li2 Li1 49.91(6) 1_565 2_655 ?
O4B Li2 C41A 30.04(13) . . ?
O3 Li2 C41A 86.55(8) 2_655 . ?
O4A Li2 C41A 31.20(8) . . ?
N2 Li2 C41A 100.24(9) 2_655 . ?
N1 Li2 C41A 146.49(11) 1_565 . ?
Li1 Li2 C41A 145.97(10) 2_655 . ?
N1 C1 S1 179.15(10) . . ?
C1 N1 Li2 135.97(10) . 1_545 ?
C1 N1 Li1 134.82(10) . 2_645 ?
Li2 N1 Li1 80.98(8) 1_545 2_645 ?
N2 C2 S2 179.69(11) . . ?
C2 N2 Li2 153.29(11) . 2_645 ?
C2 N2 Li1 120.76(10) . . ?
Li2 N2 Li1 80.62(8) 2_645 . ?
C11 O1 C14 109.17(8) . . ?
C11 O1 Li1 130.93(8) . 2_545 ?
C14 O1 Li1 116.89(9) . 2_545 ?
O1 C11 C12 105.99(9) . . ?
C11 C12 C13 102.26(9) . . ?
C14 C13 C12 101.56(9) . . ?
O1 C14 C13 105.11(9) . . ?
C24 O2 C21 109.35(8) . . ?
C24 O2 Li1 118.97(9) . . ?
C21 O2 Li1 120.11(9) . . ?
O2 C21 C22 104.82(9) . . ?
C21 C22 C23 102.00(10) . . ?
C22 C23 C24 102.60(10) . . ?
O2 C24 C23 106.41(10) . . ?
C34 O3 C31 109.88(9) . . ?
C34 O3 Li2 128.75(9) . 2_645 ?
C31 O3 Li2 121.02(8) . 2_645 ?
O3 C31 C32 106.35(9) . . ?
C31 C32 C33 101.52(10) . . ?
C34 C33 C32 103.06(10) . . ?
O3 C34 C33 104.93(10) . . ?
C44A O4A C41A 109.21(16) . . ?
C44A O4A Li2 120.36(16) . . ?
C41A O4A Li2 104.63(16) . . ?
O4A C41A C42A 104.10(17) . . ?
O4A C41A Li2 44.18(11) . . ?
C42A C41A Li2 136.33(14) . . ?
C43A C42A C41A 103.94(17) . . ?
C42A C43A C44A 102.94(19) . . ?
O4A C44A C43A 106.78(18) . . ?
C41B O4B C44B 104.7(3) . . ?
C41B O4B Li2 127.5(3) . . ?
C44B O4B Li2 120.9(3) . . ?
O4B C41B C42B 98.2(3) . . ?
C43B C42B C41B 104.3(3) 1_655 . ?
C44B C43B C42B 107.5(3) 1_455 1_455 ?
O4B C44B C43B 101.8(3) . 1_655 ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        31.88
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.047
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuran'
_chemical_properties_physical    Moisture-sensitive,Hygroscopic,Heat-sensitive
