# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
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#  except for the purpose of generating routine backup copies 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 902920'
#TrackingRef 'web_deposit_cif_file_0_JianZhou_1352237385.1.CIF'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H27 Ge La N6 S4 '
_chemical_formula_sum            'C8 H27 Ge La N6 S4'
_chemical_formula_weight         547.16

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'
S S 0.1246 0.1234 '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'
La La -0.2871 2.4523 '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 2/c'
_symmetry_space_group_name_Hall  '-C 2yc '

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                   27.837(6)
_cell_length_b                   16.993(3)
_cell_length_c                   8.3185(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.96(3)
_cell_angle_gamma                90.00
_cell_volume                     3818.7(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    12654
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      27.65

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2160
_exptl_absorpt_coefficient_mu    4.218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2150
_exptl_absorpt_correction_T_max  0.3894
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_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  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12654
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         27.65
_reflns_number_total             4369
_reflns_number_gt                4056
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
;
In order to prevent C1/C2 and N1/N2 atoms going non-positive-definite
or oblate anisotropic displacement ellipsoids, these atoms were refined by
a soft restraint with a large esd.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0240P)^2^+10.7747P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00157(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4369
_refine_ls_number_parameters     183
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0230
_refine_ls_wR_factor_ref         0.0575
_refine_ls_wR_factor_gt          0.0564
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.094
_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
La1 La 0.368478(5) 0.239397(9) 0.804744(18) 0.02018(6) Uani 1 1 d . . .
Ge1 Ge 0.380492(11) 0.254839(17) 0.37351(4) 0.02468(8) Uani 1 1 d . . .
S1 S 0.32963(3) 0.32460(5) 0.47914(9) 0.03119(16) Uani 1 1 d . . .
S2 S 0.42136(3) 0.17392(5) 0.56057(9) 0.03696(18) Uani 1 1 d . . .
S3 S 0.43957(4) 0.34564(7) 0.33955(12) 0.0562(3) Uani 1 1 d . . .
H3 H 0.4544 0.3284 0.2201 0.084 Uiso 1 1 calc R . .
S4 S 0.34652(3) 0.20122(5) 0.13660(9) 0.03604(18) Uani 1 1 d . . .
N1 N 0.27649(10) 0.29357(17) 0.8012(4) 0.0410(6) Uani 1 1 d U . .
H1C H 0.2560 0.2809 0.7035 0.049 Uiso 1 1 calc R . .
H1D H 0.2656 0.2687 0.8812 0.049 Uiso 1 1 calc R . .
N2 N 0.36270(10) 0.38588(16) 0.9416(4) 0.0390(6) Uani 1 1 d U . .
H2C H 0.3804 0.3821 1.0487 0.047 Uiso 1 1 calc R . .
N3 N 0.44101(10) 0.34601(18) 0.7964(4) 0.0449(7) Uani 1 1 d . . .
H3C H 0.4702 0.3241 0.8469 0.054 Uiso 1 1 calc R . .
H3D H 0.4414 0.3533 0.6896 0.054 Uiso 1 1 calc R . .
N4 N 0.29907(10) 0.14193(17) 0.6227(4) 0.0435(7) Uani 1 1 d . . .
H4C H 0.2692 0.1639 0.6150 0.052 Uiso 1 1 calc R . .
H4D H 0.3039 0.1398 0.5196 0.052 Uiso 1 1 calc R . .
N5 N 0.37820(10) 0.08104(15) 0.8678(3) 0.0351(6) Uani 1 1 d . . .
H5C H 0.3657 0.0736 0.9583 0.042 Uiso 1 1 calc R . .
N6 N 0.45647(10) 0.18898(19) 0.9997(4) 0.0435(7) Uani 1 1 d . . .
H6C H 0.4800 0.1957 0.9434 0.052 Uiso 1 1 calc R . .
H6D H 0.4643 0.2200 1.0899 0.052 Uiso 1 1 calc R . .
C1 C 0.27359(15) 0.3769(3) 0.8254(8) 0.0767(13) Uani 1 1 d U . .
H1A H 0.2738 0.4033 0.7222 0.092 Uiso 1 1 calc R . .
H1B H 0.2422 0.3887 0.8516 0.092 Uiso 1 1 calc R . .
C2 C 0.31173(16) 0.4079(3) 0.9503(7) 0.0725(13) Uani 1 1 d U . .
H2A H 0.3068 0.3907 1.0565 0.087 Uiso 1 1 calc R . .
H2B H 0.3091 0.4648 0.9469 0.087 Uiso 1 1 calc R . .
C3 C 0.38706(17) 0.4470(2) 0.8671(7) 0.0628(11) Uani 1 1 d . . .
H3A H 0.3870 0.4959 0.9270 0.075 Uiso 1 1 calc R . .
H3B H 0.3689 0.4554 0.7533 0.075 Uiso 1 1 calc R . .
C4 C 0.43866(16) 0.4242(2) 0.8710(7) 0.0634(12) Uani 1 1 d . . .
H4A H 0.4531 0.4630 0.8111 0.076 Uiso 1 1 calc R . .
H4B H 0.4580 0.4236 0.9848 0.076 Uiso 1 1 calc R . .
C5 C 0.29722(15) 0.0609(2) 0.6819(6) 0.0610(11) Uani 1 1 d . . .
H5A H 0.2786 0.0281 0.5929 0.073 Uiso 1 1 calc R . .
H5B H 0.2806 0.0599 0.7719 0.073 Uiso 1 1 calc R . .
C6 C 0.34860(16) 0.0297(2) 0.7406(6) 0.0568(10) Uani 1 1 d . . .
H6A H 0.3474 -0.0227 0.7856 0.068 Uiso 1 1 calc R . .
H6B H 0.3640 0.0260 0.6478 0.068 Uiso 1 1 calc R . .
C7 C 0.42991(14) 0.0546(2) 0.9201(5) 0.0494(9) Uani 1 1 d . . .
H7A H 0.4450 0.0563 0.8265 0.059 Uiso 1 1 calc R . .
H7B H 0.4310 0.0007 0.9590 0.059 Uiso 1 1 calc R . .
C8 C 0.45808(14) 0.1064(3) 1.0554(5) 0.0556(10) Uani 1 1 d . . .
H8A H 0.4439 0.1025 1.1508 0.067 Uiso 1 1 calc R . .
H8B H 0.4922 0.0889 1.0885 0.067 Uiso 1 1 calc R . .

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
La1 0.01645(9) 0.02471(9) 0.01972(9) -0.00048(5) 0.00503(6) 0.00091(5)
Ge1 0.02323(15) 0.03328(16) 0.01891(15) 0.00172(10) 0.00774(11) 0.00385(11)
S1 0.0275(3) 0.0402(4) 0.0266(3) 0.0029(3) 0.0081(3) 0.0124(3)
S2 0.0388(4) 0.0465(4) 0.0286(4) 0.0086(3) 0.0141(3) 0.0201(3)
S3 0.0455(5) 0.0759(7) 0.0472(5) 0.0028(5) 0.0112(4) -0.0292(5)
S4 0.0416(4) 0.0463(4) 0.0222(3) -0.0050(3) 0.0117(3) -0.0102(3)
N1 0.0258(13) 0.0450(15) 0.0545(17) -0.0085(13) 0.0140(12) 0.0023(11)
N2 0.0343(14) 0.0352(13) 0.0482(16) -0.0059(12) 0.0113(12) -0.0011(11)
N3 0.0357(15) 0.0534(18) 0.0502(17) -0.0014(14) 0.0195(13) -0.0107(13)
N4 0.0297(14) 0.0429(16) 0.0510(17) -0.0069(13) -0.0038(12) -0.0018(12)
N5 0.0408(15) 0.0320(13) 0.0330(14) 0.0035(10) 0.0098(11) 0.0059(11)
N6 0.0260(13) 0.0635(19) 0.0381(15) -0.0036(13) 0.0020(11) 0.0025(13)
C1 0.039(2) 0.056(2) 0.134(4) -0.024(3) 0.020(2) 0.0064(18)
C2 0.051(2) 0.064(2) 0.098(3) -0.035(2) 0.011(2) 0.0167(19)
C3 0.072(3) 0.0333(19) 0.088(3) 0.001(2) 0.028(3) -0.0055(18)
C4 0.050(2) 0.046(2) 0.096(3) -0.005(2) 0.023(2) -0.0202(18)
C5 0.052(2) 0.045(2) 0.082(3) -0.009(2) 0.007(2) -0.0199(18)
C6 0.073(3) 0.0278(17) 0.066(3) -0.0050(16) 0.011(2) -0.0031(17)
C7 0.055(2) 0.0449(19) 0.052(2) 0.0173(16) 0.0207(18) 0.0237(17)
C8 0.0370(19) 0.082(3) 0.046(2) 0.025(2) 0.0061(16) 0.0246(19)

_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
La1 N4 2.712(3) . ?
La1 N1 2.715(3) . ?
La1 N3 2.726(3) . ?
La1 N6 2.729(3) . ?
La1 N5 2.743(3) . ?
La1 N2 2.758(3) . ?
La1 S2 2.9955(10) . ?
La1 S1 3.0312(10) . ?
La1 S4 3.0381(9) 1_556 ?
Ge1 S4 2.1701(10) . ?
Ge1 S2 2.1799(9) . ?
Ge1 S1 2.1869(8) . ?
Ge1 S3 2.3214(10) . ?
S3 H3 1.2000 . ?
S4 La1 3.0381(9) 1_554 ?
N1 C1 1.436(5) . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N2 C3 1.458(5) . ?
N2 C2 1.486(5) . ?
N2 H2C 0.9100 . ?
N3 C4 1.475(5) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N4 C5 1.467(5) . ?
N4 H4C 0.9000 . ?
N4 H4D 0.9000 . ?
N5 C6 1.463(5) . ?
N5 C7 1.470(4) . ?
N5 H5C 0.9100 . ?
N6 C8 1.476(5) . ?
N6 H6C 0.9000 . ?
N6 H6D 0.9000 . ?
C1 C2 1.397(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.480(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.493(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.493(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 La1 N1 70.01(9) . . ?
N4 La1 N3 145.46(10) . . ?
N1 La1 N3 118.48(9) . . ?
N4 La1 N6 123.80(9) . . ?
N1 La1 N6 145.28(9) . . ?
N3 La1 N6 70.11(10) . . ?
N4 La1 N5 62.08(8) . . ?
N1 La1 N5 112.59(8) . . ?
N3 La1 N5 128.13(9) . . ?
N6 La1 N5 62.95(9) . . ?
N4 La1 N2 132.61(8) . . ?
N1 La1 N2 63.22(8) . . ?
N3 La1 N2 61.84(9) . . ?
N6 La1 N2 99.87(9) . . ?
N5 La1 N2 145.03(8) . . ?
N4 La1 S2 78.17(7) . . ?
N1 La1 S2 137.33(7) . . ?
N3 La1 S2 75.01(7) . . ?
N6 La1 S2 76.63(7) . . ?
N5 La1 S2 73.94(6) . . ?
N2 La1 S2 134.61(6) . . ?
N4 La1 S1 74.95(7) . . ?
N1 La1 S1 72.31(7) . . ?
N3 La1 S1 76.50(7) . . ?
N6 La1 S1 139.16(7) . . ?
N5 La1 S1 129.58(6) . . ?
N2 La1 S1 83.92(7) . . ?
S2 La1 S1 72.50(2) . . ?
N4 La1 S4 95.99(7) . 1_556 ?
N1 La1 S4 71.70(7) . 1_556 ?
N3 La1 S4 118.54(7) . 1_556 ?
N6 La1 S4 75.02(7) . 1_556 ?
N5 La1 S4 69.44(6) . 1_556 ?
N2 La1 S4 76.88(6) . 1_556 ?
S2 La1 S4 140.93(3) . 1_556 ?
S1 La1 S4 143.83(2) . 1_556 ?
S4 Ge1 S2 114.92(4) . . ?
S4 Ge1 S1 114.20(4) . . ?
S2 Ge1 S1 109.39(3) . . ?
S4 Ge1 S3 109.57(4) . . ?
S2 Ge1 S3 104.07(4) . . ?
S1 Ge1 S3 103.59(4) . . ?
Ge1 S1 La1 88.52(3) . . ?
Ge1 S2 La1 89.57(3) . . ?
Ge1 S3 H3 109.5 . . ?
Ge1 S4 La1 126.61(3) . 1_554 ?
C1 N1 La1 114.7(2) . . ?
C1 N1 H1C 108.6 . . ?
La1 N1 H1C 108.6 . . ?
C1 N1 H1D 108.6 . . ?
La1 N1 H1D 108.6 . . ?
H1C N1 H1D 107.6 . . ?
C3 N2 C2 112.9(3) . . ?
C3 N2 La1 112.8(2) . . ?
C2 N2 La1 113.5(2) . . ?
C3 N2 H2C 105.6 . . ?
C2 N2 H2C 105.6 . . ?
La1 N2 H2C 105.6 . . ?
C4 N3 La1 118.7(2) . . ?
C4 N3 H3C 107.6 . . ?
La1 N3 H3C 107.6 . . ?
C4 N3 H3D 107.6 . . ?
La1 N3 H3D 107.6 . . ?
H3C N3 H3D 107.1 . . ?
C5 N4 La1 117.6(2) . . ?
C5 N4 H4C 107.9 . . ?
La1 N4 H4C 107.9 . . ?
C5 N4 H4D 107.9 . . ?
La1 N4 H4D 107.9 . . ?
H4C N4 H4D 107.2 . . ?
C6 N5 C7 111.8(3) . . ?
C6 N5 La1 115.8(2) . . ?
C7 N5 La1 113.6(2) . . ?
C6 N5 H5C 104.8 . . ?
C7 N5 H5C 104.8 . . ?
La1 N5 H5C 104.8 . . ?
C8 N6 La1 116.1(2) . . ?
C8 N6 H6C 108.3 . . ?
La1 N6 H6C 108.3 . . ?
C8 N6 H6D 108.3 . . ?
La1 N6 H6D 108.3 . . ?
H6C N6 H6D 107.4 . . ?
C2 C1 N1 114.6(4) . . ?
C2 C1 H1A 108.6 . . ?
N1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
N1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 N2 115.6(4) . . ?
C1 C2 H2A 108.4 . . ?
N2 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
N2 C2 H2B 108.4 . . ?
H2A C2 H2B 107.4 . . ?
N2 C3 C4 110.7(3) . . ?
N2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N3 C4 C3 111.5(3) . . ?
N3 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N3 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
N4 C5 C6 109.6(3) . . ?
N4 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N4 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
N5 C6 C5 110.6(3) . . ?
N5 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
N5 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
N5 C7 C8 110.0(3) . . ?
N5 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
N5 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
N6 C8 C7 110.7(3) . . ?
N6 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N6 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1D S4 0.90 2.93 3.379(3) 112.4 1_556
N2 H2C S3 0.91 2.65 3.548(3) 168.6 1_556
N3 H3C N6 0.90 2.70 3.133(4) 111.0 .
N3 H3D S3 0.90 2.90 3.791(3) 169.3 .
N4 H4C N1 0.90 2.67 3.113(4) 111.2 .
N4 H4C S1 0.90 2.68 3.523(3) 156.5 7_556
N5 H5C S4 0.91 2.75 3.301(3) 119.9 1_556
N6 H6C S2 0.90 2.78 3.564(3) 146.6 2_656

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.65
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.577
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.088




data_2
_database_code_depnum_ccdc_archive 'CCDC 902921'
#TrackingRef '2.CIF'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H27 Ge N6 Nd S4 '
_chemical_formula_sum            'C8 H27 Ge N6 Nd S4 '
_chemical_formula_weight         552.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'

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

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                   27.694(6)
_cell_length_b                   16.845(4)
_cell_length_c                   8.2868(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.791(2)
_cell_angle_gamma                90.00
_cell_volume                     3754.4(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2184
_exptl_absorpt_coefficient_mu    4.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1231
_exptl_absorpt_correction_T_max  0.2539
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_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  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10255
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3304
_reflns_number_gt                3084
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0144P)^2^+14.6101P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3304
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0470
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.006
_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
Ge2 Ge 0.879969(12) 0.24527(2) 0.37123(4) 0.02184(9) Uani 1 1 d . . .
N1 N 0.95474(11) 0.3064(2) 0.9943(4) 0.0398(8) Uani 1 1 d . . .
H1A H 0.9618 0.2740 1.0833 0.048 Uiso 1 1 calc R . .
H1B H 0.9785 0.2991 0.9381 0.048 Uiso 1 1 calc R . .
N2 N 0.87877(11) 0.41719(17) 0.8685(4) 0.0313(7) Uani 1 1 d . . .
H2 H 0.8662 0.4240 0.9595 0.038 Uiso 1 1 calc R . .
N3 N 0.80045(11) 0.35790(18) 0.6215(4) 0.0366(7) Uani 1 1 d . . .
H3A H 0.8059 0.3609 0.5188 0.044 Uiso 1 1 calc R . .
H3B H 0.7704 0.3354 0.6115 0.044 Uiso 1 1 calc R . .
N4 N 0.77734(11) 0.20976(18) 0.7987(4) 0.0346(7) Uani 1 1 d . . .
H4A H 0.7667 0.2351 0.8794 0.041 Uiso 1 1 calc R . .
H4B H 0.7567 0.2230 0.7010 0.041 Uiso 1 1 calc R . .
N5 N 0.86304(11) 0.11766(17) 0.9411(4) 0.0318(7) Uani 1 1 d . . .
H5 H 0.8811 0.1226 1.0478 0.038 Uiso 1 1 calc R . .
N6 N 0.93884(12) 0.1557(2) 0.7854(4) 0.0403(8) Uani 1 1 d . . .
H6A H 0.9378 0.1472 0.6775 0.048 Uiso 1 1 calc R . .
H6B H 0.9684 0.1784 0.8308 0.048 Uiso 1 1 calc R . .
S1 S 0.82880(3) 0.17618(5) 0.47978(11) 0.02732(19) Uani 1 1 d . . .
S2 S 0.92056(3) 0.32688(6) 0.55938(11) 0.0327(2) Uani 1 1 d . . .
S3 S 0.93962(4) 0.15352(7) 0.33934(14) 0.0504(3) Uani 1 1 d . . .
H3 H 0.9607 0.1775 0.2383 0.076 Uiso 1 1 calc R . .
S4 S 0.84633(3) 0.29818(6) 0.13230(11) 0.0327(2) Uani 1 1 d . . .
Nd1 Nd 0.868050(6) 0.261154(10) 0.79997(2) 0.01783(6) Uani 1 1 d . . .
C1 C 0.77375(16) 0.1247(3) 0.8231(8) 0.0688(17) Uani 1 1 d . . .
H1C H 0.7418 0.1128 0.8467 0.083 Uiso 1 1 calc R . .
H1D H 0.7752 0.0974 0.7213 0.083 Uiso 1 1 calc R . .
C2 C 0.81188(17) 0.0958(3) 0.9537(7) 0.0614(14) Uani 1 1 d . . .
H2A H 0.8095 0.0384 0.9566 0.074 Uiso 1 1 calc R . .
H2B H 0.8067 0.1161 1.0579 0.074 Uiso 1 1 calc R . .
C3 C 0.88701(18) 0.0547(3) 0.8690(7) 0.0574(13) Uani 1 1 d . . .
H3C H 0.8679 0.0436 0.7571 0.069 Uiso 1 1 calc R . .
H3D H 0.8880 0.0067 0.9344 0.069 Uiso 1 1 calc R . .
C4 C 0.93796(16) 0.0779(3) 0.8647(7) 0.0565(13) Uani 1 1 d . . .
H4C H 0.9585 0.0799 0.9773 0.068 Uiso 1 1 calc R . .
H4D H 0.9519 0.0383 0.8040 0.068 Uiso 1 1 calc R . .
C5 C 0.95796(15) 0.3891(3) 1.0545(6) 0.0519(12) Uani 1 1 d . . .
H5A H 0.9926 0.4051 1.0880 0.062 Uiso 1 1 calc R . .
H5B H 0.9438 0.3929 1.1507 0.062 Uiso 1 1 calc R . .
C6 C 0.93072(16) 0.4430(2) 0.9219(6) 0.0455(10) Uani 1 1 d . . .
H6C H 0.9321 0.4970 0.9636 0.055 Uiso 1 1 calc R . .
H6D H 0.9461 0.4420 0.8283 0.055 Uiso 1 1 calc R . .
C7 C 0.84939(18) 0.4709(2) 0.7431(6) 0.0507(11) Uani 1 1 d . . .
H7A H 0.8650 0.4757 0.6504 0.061 Uiso 1 1 calc R . .
H7B H 0.8482 0.5231 0.7910 0.061 Uiso 1 1 calc R . .
C8 C 0.79802(17) 0.4395(3) 0.6831(7) 0.0545(12) Uani 1 1 d . . .
H8A H 0.7811 0.4397 0.7731 0.065 Uiso 1 1 calc R . .
H8B H 0.7794 0.4730 0.5945 0.065 Uiso 1 1 calc R . .

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
Ge2 0.02189(17) 0.03082(19) 0.01423(18) -0.00147(13) 0.00708(14) -0.00363(13)
N1 0.0255(16) 0.062(2) 0.0308(19) 0.0043(16) 0.0041(14) 0.0006(15)
N2 0.0395(17) 0.0308(16) 0.0246(17) -0.0049(12) 0.0098(14) -0.0055(13)
N3 0.0287(16) 0.0370(17) 0.039(2) 0.0053(14) -0.0012(14) 0.0018(13)
N4 0.0248(15) 0.0416(18) 0.0384(19) 0.0065(14) 0.0097(14) -0.0013(13)
N5 0.0324(16) 0.0331(16) 0.0296(18) 0.0031(13) 0.0067(13) 0.0004(13)
N6 0.0358(18) 0.050(2) 0.040(2) 0.0020(15) 0.0171(15) 0.0114(15)
S1 0.0252(4) 0.0366(5) 0.0211(5) -0.0025(3) 0.0075(3) -0.0110(3)
S2 0.0362(5) 0.0413(5) 0.0231(5) -0.0074(4) 0.0123(4) -0.0176(4)
S3 0.0429(6) 0.0716(8) 0.0373(6) 0.0001(5) 0.0111(5) 0.0282(5)
S4 0.0407(5) 0.0428(5) 0.0169(5) 0.0054(4) 0.0114(4) 0.0110(4)
Nd1 0.01577(9) 0.02312(10) 0.01494(10) 0.00068(6) 0.00434(6) -0.00056(6)
C1 0.032(2) 0.046(3) 0.131(5) 0.022(3) 0.024(3) -0.004(2)
C2 0.047(3) 0.055(3) 0.081(4) 0.030(3) 0.013(3) -0.012(2)
C3 0.068(3) 0.032(2) 0.079(4) 0.004(2) 0.031(3) 0.009(2)
C4 0.044(3) 0.041(2) 0.086(4) 0.004(2) 0.018(2) 0.0167(19)
C5 0.031(2) 0.083(3) 0.040(3) -0.023(2) 0.0061(19) -0.021(2)
C6 0.051(2) 0.042(2) 0.045(3) -0.0166(19) 0.015(2) -0.0213(19)
C7 0.069(3) 0.0229(19) 0.057(3) 0.0041(18) 0.008(2) 0.0027(19)
C8 0.051(3) 0.041(2) 0.067(3) 0.006(2) 0.004(2) 0.019(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge2 S4 2.1687(10) . ?
Ge2 S2 2.1791(10) . ?
Ge2 S1 2.1863(9) . ?
Ge2 S3 2.3227(11) . ?
N1 C5 1.476(6) . ?
N1 Nd1 2.664(3) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C6 1.467(5) . ?
N2 C7 1.468(5) . ?
N2 Nd1 2.690(3) . ?
N2 H2 0.9100 . ?
N3 C8 1.474(5) . ?
N3 Nd1 2.651(3) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C1 1.454(5) . ?
N4 Nd1 2.655(3) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C3 1.453(5) . ?
N5 C2 1.491(5) . ?
N5 Nd1 2.703(3) . ?
N5 H5 0.9100 . ?
N6 C4 1.469(5) . ?
N6 Nd1 2.669(3) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
S1 Nd1 2.9825(10) . ?
S2 Nd1 2.9491(10) . ?
S3 H3 1.2000 . ?
S4 Nd1 3.0207(11) 1_554 ?
Nd1 S4 3.0207(11) 1_556 ?
C1 C2 1.406(7) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.473(6) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.485(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.487(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Ge2 S2 115.47(4) . . ?
S4 Ge2 S1 114.52(4) . . ?
S2 Ge2 S1 108.41(4) . . ?
S4 Ge2 S3 109.39(4) . . ?
S2 Ge2 S3 103.98(4) . . ?
S1 Ge2 S3 103.95(5) . . ?
C5 N1 Nd1 116.6(2) . . ?
C5 N1 H1A 108.1 . . ?
Nd1 N1 H1A 108.1 . . ?
C5 N1 H1B 108.1 . . ?
Nd1 N1 H1B 108.1 . . ?
H1A N1 H1B 107.3 . . ?
C6 N2 C7 111.7(3) . . ?
C6 N2 Nd1 113.9(2) . . ?
C7 N2 Nd1 115.9(2) . . ?
C6 N2 H2 104.7 . . ?
C7 N2 H2 104.7 . . ?
Nd1 N2 H2 104.7 . . ?
C8 N3 Nd1 117.7(2) . . ?
C8 N3 H3A 107.9 . . ?
Nd1 N3 H3A 107.9 . . ?
C8 N3 H3B 107.9 . . ?
Nd1 N3 H3B 107.9 . . ?
H3A N3 H3B 107.2 . . ?
C1 N4 Nd1 114.6(2) . . ?
C1 N4 H4A 108.6 . . ?
Nd1 N4 H4A 108.6 . . ?
C1 N4 H4B 108.6 . . ?
Nd1 N4 H4B 108.6 . . ?
H4A N4 H4B 107.6 . . ?
C3 N5 C2 112.5(4) . . ?
C3 N5 Nd1 113.5(2) . . ?
C2 N5 Nd1 113.5(2) . . ?
C3 N5 H5 105.4 . . ?
C2 N5 H5 105.4 . . ?
Nd1 N5 H5 105.4 . . ?
C4 N6 Nd1 118.9(2) . . ?
C4 N6 H6A 107.6 . . ?
Nd1 N6 H6A 107.6 . . ?
C4 N6 H6B 107.6 . . ?
Nd1 N6 H6B 107.6 . . ?
H6A N6 H6B 107.0 . . ?
Ge2 S1 Nd1 88.63(3) . . ?
Ge2 S2 Nd1 89.63(3) . . ?
Ge2 S3 H3 109.5 . . ?
Ge2 S4 Nd1 127.73(4) . 1_554 ?
N3 Nd1 N4 69.91(10) . . ?
N3 Nd1 N1 125.19(10) . . ?
N4 Nd1 N1 144.22(10) . . ?
N3 Nd1 N6 144.34(11) . . ?
N4 Nd1 N6 119.17(10) . . ?
N1 Nd1 N6 69.62(11) . . ?
N3 Nd1 N2 62.93(9) . . ?
N4 Nd1 N2 112.09(9) . . ?
N1 Nd1 N2 63.56(10) . . ?
N6 Nd1 N2 127.90(10) . . ?
N3 Nd1 N5 133.53(9) . . ?
N4 Nd1 N5 64.15(9) . . ?
N1 Nd1 N5 97.24(10) . . ?
N6 Nd1 N5 62.52(10) . . ?
N2 Nd1 N5 142.82(9) . . ?
N3 Nd1 S2 77.79(8) . . ?
N4 Nd1 S2 137.59(7) . . ?
N1 Nd1 S2 77.46(8) . . ?
N6 Nd1 S2 74.54(7) . . ?
N2 Nd1 S2 74.24(7) . . ?
N5 Nd1 S2 135.45(7) . . ?
N3 Nd1 S1 74.91(7) . . ?
N4 Nd1 S1 72.31(7) . . ?
N1 Nd1 S1 139.47(7) . . ?
N6 Nd1 S1 75.90(8) . . ?
N2 Nd1 S1 130.92(7) . . ?
N5 Nd1 S1 84.86(7) . . ?
S2 Nd1 S1 73.30(3) . . ?
N3 Nd1 S4 96.55(8) . 1_556 ?
N4 Nd1 S4 71.16(8) . 1_556 ?
N1 Nd1 S4 74.71(7) . 1_556 ?
N6 Nd1 S4 119.11(8) . 1_556 ?
N2 Nd1 S4 69.02(7) . 1_556 ?
N5 Nd1 S4 75.42(7) . 1_556 ?
S2 Nd1 S4 140.92(3) . 1_556 ?
S1 Nd1 S4 143.19(3) . 1_556 ?
C2 C1 N4 112.6(4) . . ?
C2 C1 H1C 109.1 . . ?
N4 C1 H1C 109.1 . . ?
C2 C1 H1D 109.1 . . ?
N4 C1 H1D 109.1 . . ?
H1C C1 H1D 107.8 . . ?
C1 C2 N5 114.4(4) . . ?
C1 C2 H2A 108.7 . . ?
N5 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
N5 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N5 C3 C4 110.5(4) . . ?
N5 C3 H3C 109.6 . . ?
C4 C3 H3C 109.6 . . ?
N5 C3 H3D 109.6 . . ?
C4 C3 H3D 109.6 . . ?
H3C C3 H3D 108.1 . . ?
N6 C4 C3 111.5(3) . . ?
N6 C4 H4C 109.3 . . ?
C3 C4 H4C 109.3 . . ?
N6 C4 H4D 109.3 . . ?
C3 C4 H4D 109.3 . . ?
H4C C4 H4D 108.0 . . ?
N1 C5 C6 110.4(3) . . ?
N1 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
N1 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N2 C6 C5 109.3(3) . . ?
N2 C6 H6C 109.8 . . ?
C5 C6 H6C 109.8 . . ?
N2 C6 H6D 109.8 . . ?
C5 C6 H6D 109.8 . . ?
H6C C6 H6D 108.3 . . ?
N2 C7 C8 110.0(3) . . ?
N2 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
N2 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
N3 C8 C7 109.1(3) . . ?
N3 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
N3 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.083