# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_31311
_database_code_depnum_ccdc_archive 'CCDC 1561329'
_audit_update_record             
;
2017-07-10 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ge3 Li3 Se6'
_chemical_formula_weight         712.35

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.7728(3)
_cell_length_b                   8.6804(5)
_cell_length_c                   10.6300(5)
_cell_angle_alpha                74.519(4)
_cell_angle_beta                 76.334(4)
_cell_angle_gamma                69.185(4)
_cell_volume                     555.98(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2506
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.183
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             618
_exptl_absorpt_coefficient_mu    27.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4851
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9499
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         27.53
_reflns_number_total             2550
_reflns_number_gt                2124
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0171P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00097(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2550
_refine_ls_number_parameters     113
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0502
_refine_ls_wR_factor_gt          0.0471
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_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
Se1 Se 0.25734(7) 0.85751(6) 0.40466(4) 0.01599(12) Uani 1 1 d . . .
Se2 Se 0.77538(8) 0.52995(6) 0.24387(4) 0.01648(12) Uani 1 1 d . . .
Se3 Se 0.79862(8) 0.78454(6) -0.10436(4) 0.01822(12) Uani 1 1 d . . .
Ge1 Ge 0.56771(8) 0.61650(6) 0.44715(4) 0.01379(12) Uani 1 1 d . . .
Ge2 Ge 0.55315(8) 0.74147(6) 0.09507(4) 0.01361(12) Uani 1 1 d . . .
Se4 Se 0.74589(8) 1.01802(6) 0.24942(5) 0.01903(12) Uani 1 1 d . . .
Ge3 Ge 0.45759(8) 0.97254(6) 0.20559(4) 0.01357(12) Uani 1 1 d . . .
Se5 Se 0.76359(8) 0.66601(6) 0.57205(5) 0.01913(12) Uani 1 1 d . . .
Se6 Se 0.26720(8) 0.66959(6) 0.07830(5) 0.01918(12) Uani 1 1 d . . .
Li1 Li 1.0000 1.0000 0.0000 0.034(3) Uani 1 2 d S . .
Li2 Li 0.0301(16) 0.6879(13) 0.3226(9) 0.037(2) Uani 1 1 d . . .
Li3 Li 0.5000 1.0000 0.5000 0.037(3) Uani 1 2 d S . .
Li4 Li 0.5123(17) 0.3509(12) 0.1913(9) 0.038(2) Uani 1 1 d . . .

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
Se1 0.0150(3) 0.0155(3) 0.0137(2) -0.00082(18) 0.00060(18) -0.00357(19)
Se2 0.0168(3) 0.0151(3) 0.0130(2) -0.00226(19) -0.00146(18) -0.00072(19)
Se3 0.0150(3) 0.0174(3) 0.0147(2) 0.00048(19) 0.00115(18) -0.00096(19)
Ge1 0.0167(3) 0.0124(3) 0.0112(2) 0.00021(19) -0.00168(19) -0.0053(2)
Ge2 0.0158(3) 0.0125(3) 0.0115(2) -0.00150(19) -0.00090(19) -0.0047(2)
Se4 0.0177(3) 0.0200(3) 0.0202(2) -0.0023(2) -0.0038(2) -0.0077(2)
Ge3 0.0160(3) 0.0120(3) 0.0111(2) -0.00109(19) -0.00106(18) -0.0041(2)
Se5 0.0197(3) 0.0213(3) 0.0177(2) -0.0046(2) -0.0047(2) -0.0063(2)
Se6 0.0186(3) 0.0211(3) 0.0195(2) -0.0033(2) -0.0030(2) -0.0088(2)
Li1 0.028(8) 0.041(8) 0.021(6) 0.001(6) 0.004(5) -0.009(6)
Li2 0.030(6) 0.046(7) 0.032(5) -0.004(5) 0.002(4) -0.015(5)
Li3 0.046(9) 0.030(8) 0.029(7) -0.005(6) -0.011(6) -0.004(7)
Li4 0.050(7) 0.028(6) 0.032(5) -0.002(4) -0.007(5) -0.011(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
Se1 Ge3 2.4068(7) . ?
Se1 Ge1 2.4121(7) . ?
Se1 Li3 2.8564(5) . ?
Se1 Li2 2.868(10) . ?
Se2 Ge2 2.3977(6) . ?
Se2 Ge1 2.4272(7) . ?
Se2 Li2 2.921(10) 1_655 ?
Se2 Li4 2.967(11) . ?
Se3 Ge3 2.3845(7) 2_675 ?
Se3 Ge2 2.3982(7) . ?
Se3 Li4 3.151(11) 2_665 ?
Ge1 Se5 2.2912(7) . ?
Ge1 Ge1 2.4109(10) 2_666 ?
Ge2 Se6 2.2920(7) . ?
Ge2 Ge3 2.4080(7) . ?
Se4 Ge3 2.2938(7) . ?
Se4 Li4 2.737(10) 1_565 ?
Se4 Li3 2.7856(5) . ?
Se4 Li1 2.8089(5) . ?
Se4 Li2 2.850(10) 1_655 ?
Ge3 Se3 2.3845(7) 2_675 ?
Se5 Li4 2.760(10) 2_666 ?
Se5 Li3 2.8215(5) . ?
Se5 Li2 2.835(10) 1_655 ?
Se5 Li2 2.915(10) 2_666 ?
Se6 Li2 2.724(10) . ?
Se6 Li4 2.785(9) . ?
Se6 Li1 2.8182(5) 1_455 ?
Se6 Li4 2.922(10) 2_665 ?
Li1 Se4 2.8089(5) 2_775 ?
Li1 Se6 2.8182(5) 2_675 ?
Li1 Se6 2.8182(5) 1_655 ?
Li2 Se5 2.835(10) 1_455 ?
Li2 Se4 2.850(10) 1_455 ?
Li2 Se5 2.915(10) 2_666 ?
Li2 Se2 2.921(10) 1_455 ?
Li3 Se4 2.7856(5) 2_676 ?
Li3 Se5 2.8215(5) 2_676 ?
Li3 Se1 2.8564(5) 2_676 ?
Li4 Se4 2.737(10) 1_545 ?
Li4 Se5 2.760(10) 2_666 ?
Li4 Se6 2.922(10) 2_665 ?
Li4 Se3 3.151(11) 2_665 ?

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
Ge3 Se1 Ge1 90.59(2) . . ?
Ge3 Se1 Li3 76.771(18) . . ?
Ge1 Se1 Li3 79.219(18) . . ?
Ge3 Se1 Li2 105.79(19) . . ?
Ge1 Se1 Li2 96.6(2) . . ?
Li3 Se1 Li2 175.18(19) . . ?
Ge2 Se2 Ge1 97.32(2) . . ?
Ge2 Se2 Li2 107.64(19) . 1_655 ?
Ge1 Se2 Li2 75.7(2) . 1_655 ?
Ge2 Se2 Li4 76.78(18) . . ?
Ge1 Se2 Li4 100.4(2) . . ?
Li2 Se2 Li4 174.3(3) 1_655 . ?
Ge3 Se3 Ge2 93.47(2) 2_675 . ?
Ge3 Se3 Li4 74.17(17) 2_675 2_665 ?
Ge2 Se3 Li4 77.08(19) . 2_665 ?
Se5 Ge1 Ge1 113.59(3) . 2_666 ?
Se5 Ge1 Se1 110.50(3) . . ?
Ge1 Ge1 Se1 105.67(3) 2_666 . ?
Se5 Ge1 Se2 113.48(3) . . ?
Ge1 Ge1 Se2 101.65(3) 2_666 . ?
Se1 Ge1 Se2 111.43(2) . . ?
Se6 Ge2 Se2 112.29(3) . . ?
Se6 Ge2 Se3 116.65(3) . . ?
Se2 Ge2 Se3 103.66(2) . . ?
Se6 Ge2 Ge3 114.01(3) . . ?
Se2 Ge2 Ge3 98.53(2) . . ?
Se3 Ge2 Ge3 109.73(3) . . ?
Ge3 Se4 Li4 84.3(2) . 1_565 ?
Ge3 Se4 Li3 80.015(19) . . ?
Li4 Se4 Li3 88.2(2) 1_565 . ?
Ge3 Se4 Li1 97.70(2) . . ?
Li4 Se4 Li1 97.2(2) 1_565 . ?
Li3 Se4 Li1 173.97(2) . . ?
Ge3 Se4 Li2 103.9(2) . 1_655 ?
Li4 Se4 Li2 171.7(3) 1_565 1_655 ?
Li3 Se4 Li2 91.9(2) . 1_655 ?
Li1 Se4 Li2 83.2(2) . 1_655 ?
Se4 Ge3 Se3 115.75(3) . 2_675 ?
Se4 Ge3 Se1 111.39(2) . . ?
Se3 Ge3 Se1 104.89(2) 2_675 . ?
Se4 Ge3 Ge2 113.70(3) . . ?
Se3 Ge3 Ge2 111.82(2) 2_675 . ?
Se1 Ge3 Ge2 97.37(2) . . ?
Ge1 Se5 Li4 98.0(2) . 2_666 ?
Ge1 Se5 Li3 81.948(18) . . ?
Li4 Se5 Li3 87.0(2) 2_666 . ?
Ge1 Se5 Li2 79.5(2) . 1_655 ?
Li4 Se5 Li2 177.3(3) 2_666 1_655 ?
Li3 Se5 Li2 91.4(2) . 1_655 ?
Ge1 Se5 Li2 95.3(2) . 2_666 ?
Li4 Se5 Li2 83.9(3) 2_666 2_666 ?
Li3 Se5 Li2 170.1(2) . 2_666 ?
Li2 Se5 Li2 97.5(2) 1_655 2_666 ?
Ge2 Se6 Li2 101.4(2) . . ?
Ge2 Se6 Li4 82.3(2) . . ?
Li2 Se6 Li4 87.1(3) . . ?
Ge2 Se6 Li1 96.67(2) . 1_455 ?
Li2 Se6 Li1 85.4(2) . 1_455 ?
Li4 Se6 Li1 172.0(2) . 1_455 ?
Ge2 Se6 Li4 83.6(2) . 2_665 ?
Li2 Se6 Li4 174.8(3) . 2_665 ?
Li4 Se6 Li4 94.8(2) . 2_665 ?
Li1 Se6 Li4 92.87(19) 1_455 2_665 ?
Se4 Li1 Se4 180.0 2_775 . ?
Se4 Li1 Se6 95.085(15) 2_775 2_675 ?
Se4 Li1 Se6 84.915(15) . 2_675 ?
Se4 Li1 Se6 84.915(15) 2_775 1_655 ?
Se4 Li1 Se6 95.085(15) . 1_655 ?
Se6 Li1 Se6 180.000(19) 2_675 1_655 ?
Se6 Li2 Se5 171.1(4) . 1_455 ?
Se6 Li2 Se4 96.3(3) . 1_455 ?
Se5 Li2 Se4 87.5(3) 1_455 1_455 ?
Se6 Li2 Se1 97.0(3) . . ?
Se5 Li2 Se1 91.4(3) 1_455 . ?
Se4 Li2 Se1 84.2(3) 1_455 . ?
Se6 Li2 Se5 92.6(3) . 2_666 ?
Se5 Li2 Se5 82.5(2) 1_455 2_666 ?
Se4 Li2 Se5 167.6(4) 1_455 2_666 ?
Se1 Li2 Se5 103.3(3) . 2_666 ?
Se6 Li2 Se2 85.2(3) . 1_455 ?
Se5 Li2 Se2 86.5(3) 1_455 1_455 ?
Se4 Li2 Se2 93.0(3) 1_455 1_455 ?
Se1 Li2 Se2 176.6(4) . 1_455 ?
Se5 Li2 Se2 79.1(3) 2_666 1_455 ?
Se4 Li3 Se4 180.0 2_676 . ?
Se4 Li3 Se5 89.023(15) 2_676 2_676 ?
Se4 Li3 Se5 90.977(15) . 2_676 ?
Se4 Li3 Se5 90.977(15) 2_676 . ?
Se4 Li3 Se5 89.023(15) . . ?
Se5 Li3 Se5 180.000(1) 2_676 . ?
Se4 Li3 Se1 86.987(14) 2_676 2_676 ?
Se4 Li3 Se1 93.013(14) . 2_676 ?
Se5 Li3 Se1 85.796(14) 2_676 2_676 ?
Se5 Li3 Se1 94.204(14) . 2_676 ?
Se4 Li3 Se1 93.013(14) 2_676 . ?
Se4 Li3 Se1 86.987(14) . . ?
Se5 Li3 Se1 94.204(14) 2_676 . ?
Se5 Li3 Se1 85.796(14) . . ?
Se1 Li3 Se1 180.0 2_676 . ?
Se4 Li4 Se5 93.3(3) 1_545 2_666 ?
Se4 Li4 Se6 166.4(4) 1_545 . ?
Se5 Li4 Se6 94.7(3) 2_666 . ?
Se4 Li4 Se6 84.3(3) 1_545 2_665 ?
Se5 Li4 Se6 165.0(4) 2_666 2_665 ?
Se6 Li4 Se6 85.2(2) . 2_665 ?
Se4 Li4 Se2 104.2(3) 1_545 . ?
Se5 Li4 Se2 100.1(3) 2_666 . ?
Se6 Li4 Se2 85.2(3) . . ?
Se6 Li4 Se2 94.8(3) 2_665 . ?
Se4 Li4 Se3 84.3(3) 1_545 2_665 ?
Se5 Li4 Se3 82.9(3) 2_666 2_665 ?
Se6 Li4 Se3 85.9(3) . 2_665 ?
Se6 Li4 Se3 82.1(3) 2_665 2_665 ?
Se2 Li4 Se3 170.7(3) . 2_665 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.190
