# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Gillian Reid'
_publ_contact_author_email       G.REID@SOTON.AC.UK

_publ_section_title              
;
Coordination networks derived from germanium(II)
thioether macrocyclic complexes - the first authenticated
chalcogenoether complexes of Ge(II)
;
loop_
_publ_author_name
'Gillian Reid'
'Fei Cheng.'
'Andrew Hector'
'W Levason'
'Michael Webster'
'Wenjian Zhang.'

# Attachment 'Ge_all4_4.cif'

# Manuscript ref.: B809444F
# Title: Coordination networks derived from germanium(II) thioether
# macrocyclic complexes -- the first authenticated chalcogenoether
# complexes of Ge(II)
# Authors: F. Cheng, A.L. Hector, W. Levason, G. Reid, M. Webster, W. Zhang
# Journal: Chem. Comm.
# CCDC ref. no(s).: 690317-690320
# DOI:
#
##############################################################################
### CIF submission form for molecular structure report ###
### Version: 2.0.2 (6 July 1998). (Updated 20-Apr-2005) ###
##############################################################################

# This is an electronic "form" for submitting structural details as a
# Crystallographic Information File (CIF).
# Full details of the format of such files are given in the paper "The
# Crystallographic Information File (CIF): a New Standard Archive File for
# Crystallography" by S. R. Hall, F. H. Allen and I. D. Brown [Acta Cryst.
# (1991), A47, 655-685].
#
# The current version of the core CIF dictionary is obtainable from
# www.iucr.org as a pdf file. The current version number is 2.3.
#
# CIFs can be checked for legal syntax and possible errors (ALERTS) by
# using checkcif software.
# See the web (http://journals.iucr.org/services/cif/checkcif.html).
# The website http://checkcif.iucr.org produces o/p in pdf format.
#
#==============================================================================

data_07wz018_[C6H12Cl2GeS3]
_database_code_depnum_ccdc_archive 'CCDC 690317'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2007-11-05
_audit_author_name               'Webster, M.'
_audit_update_record             
; 2008-07-27 changed _refine_ls_hydrogen_treatment to constr
;

_chemical_name_systematic        
;
catena-dichlorido(mu-1,4,7-trithiacyclononane)germanium(II)
;

# sulphur ligand C6H12S3 = [9]aneS3

_chemical_name_common            
catena-dichlorido(mu-1,4,7-trithiacyclononane)germanium(ii)
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H12 Cl2 Ge S3'
_chemical_formula_sum            'C6 H12 Cl2 Ge S3'
_chemical_formula_weight         323.83

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c a 21'
_symmetry_Int_Tables_number      29 # Superceded **
_symmetry_space_group_name_Hall  'P 2c -2ac' # Superceded **

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

_cell_length_a                   15.025(3)
_cell_length_b                   14.182(3)
_cell_length_c                   16.401(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3494.7(11)
_cell_formula_units_Z            12
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    26978
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1944
_exptl_absorpt_coefficient_mu    3.574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6428 # 0.4136
_exptl_absorpt_correction_T_max  0.7456 # 0.4686
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            30595
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         27.63
_reflns_number_total             7868
_reflns_number_gt                6190
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 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     
'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+11.1883P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(2)
_chemical_absolute_configuration unk

_refine_ls_number_reflns         7868
_refine_ls_number_parameters     326
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.0966
_refine_ls_wR_factor_gt          0.0870
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
Ge1 Ge 0.26524(5) 1.05969(8) 0.38866(5) 0.0163(2) Uani 1 1 d . . .
Ge2 Ge 0.24644(5) 0.72466(6) 0.41360(6) 0.01601(17) Uani 1 1 d . . .
Ge3 Ge 0.23403(5) 0.39190(7) 0.40690(5) 0.0201(2) Uani 1 1 d . . .
Cl1 Cl 0.35718(13) 1.18116(18) 0.34779(14) 0.0226(5) Uani 1 1 d . . .
Cl2 Cl 0.14852(13) 1.1454(2) 0.44074(15) 0.0269(5) Uani 1 1 d . . .
Cl3 Cl 0.36108(13) 0.81365(19) 0.36407(14) 0.0264(5) Uani 1 1 d . . .
Cl4 Cl 0.15154(12) 0.84388(17) 0.45519(13) 0.0191(4) Uani 1 1 d . . .
Cl5 Cl 0.12881(14) 0.4970(2) 0.45058(16) 0.0367(6) Uani 1 1 d . . .
Cl6 Cl 0.33749(14) 0.4973(2) 0.35713(14) 0.0276(5) Uani 1 1 d . . .
S1 S 0.34154(15) 1.08361(17) 0.53770(14) 0.0172(5) Uani 1 1 d . . .
S2 S 0.32322(14) 1.08552(17) 0.74424(14) 0.0166(5) Uani 1 1 d . . .
S3 S 0.52819(13) 1.08795(18) 0.65586(15) 0.0165(4) Uani 1 1 d . . .
S4 S 0.33034(13) 0.74777(16) 0.55928(13) 0.0132(5) Uani 1 1 d . . .
S5 S 0.33338(13) 0.74849(17) 0.76452(13) 0.0151(5) Uani 1 1 d . . .
S6 S 0.52983(11) 0.75474(17) 0.65848(14) 0.0148(4) Uani 1 1 d . . .
S7 S 0.32632(14) 0.41752(17) 0.55228(15) 0.0171(5) Uani 1 1 d . . .
S8 S 0.33921(15) 0.41205(18) 0.75778(15) 0.0204(5) Uani 1 1 d . . .
S9 S 0.52987(14) 0.42216(19) 0.64669(14) 0.0176(5) Uani 1 1 d . . .
C1 C 0.2840(5) 0.9942(6) 0.5938(5) 0.0171(16) Uani 1 1 d . . .
H1A H 0.2361 0.9678 0.5593 0.020 Uiso 1 1 calc R . .
H1B H 0.3261 0.9425 0.6066 0.020 Uiso 1 1 calc R . .
C2 C 0.2426(5) 1.0314(6) 0.6750(5) 0.0175(16) Uani 1 1 d . . .
H2A H 0.2133 0.9782 0.7034 0.021 Uiso 1 1 calc R . .
H2B H 0.1961 1.0784 0.6617 0.021 Uiso 1 1 calc R . .
C3 C 0.4042(4) 0.9937(5) 0.7590(4) 0.0143(14) Uani 1 1 d . . .
H3A H 0.3964 0.9662 0.8140 0.017 Uiso 1 1 calc R . .
H3B H 0.3937 0.9431 0.7186 0.017 Uiso 1 1 calc R . .
C4 C 0.5005(5) 1.0295(8) 0.7502(6) 0.023(2) Uani 1 1 d . . .
H4A H 0.5411 0.9751 0.7570 0.027 Uiso 1 1 calc R . .
H4B H 0.5125 1.0738 0.7956 0.027 Uiso 1 1 calc R . .
C5 C 0.5047(6) 0.9977(8) 0.5821(6) 0.027(2) Uani 1 1 d . . .
H5A H 0.5619 0.9733 0.5608 0.032 Uiso 1 1 calc R . .
H5B H 0.4743 0.9449 0.6101 0.032 Uiso 1 1 calc R . .
C6 C 0.4465(5) 1.0292(6) 0.5090(4) 0.0188(17) Uani 1 1 d . . .
H6A H 0.4338 0.9735 0.4745 0.023 Uiso 1 1 calc R . .
H6B H 0.4809 1.0745 0.4756 0.023 Uiso 1 1 calc R . .
C7 C 0.2487(6) 0.6889(8) 0.6234(7) 0.023(2) Uani 1 1 d . . .
H7A H 0.1984 0.7328 0.6322 0.027 Uiso 1 1 calc R . .
H7B H 0.2253 0.6339 0.5931 0.027 Uiso 1 1 calc R . .
C8 C 0.2801(5) 0.6559(7) 0.7041(5) 0.0189(19) Uani 1 1 d . . .
H8A H 0.3230 0.6037 0.6960 0.023 Uiso 1 1 calc R . .
H8B H 0.2288 0.6306 0.7350 0.023 Uiso 1 1 calc R . .
C9 C 0.4366(5) 0.6949(8) 0.7963(6) 0.021(2) Uani 1 1 d . . .
H9A H 0.4687 0.7411 0.8307 0.025 Uiso 1 1 calc R . .
H9B H 0.4219 0.6403 0.8313 0.025 Uiso 1 1 calc R . .
C10 C 0.5006(4) 0.6611(6) 0.7307(5) 0.0095(18) Uani 1 1 d . . .
H10A H 0.4731 0.6081 0.7006 0.011 Uiso 1 1 calc R . .
H10B H 0.5556 0.6373 0.7569 0.011 Uiso 1 1 calc R . .
C11 C 0.5098(5) 0.6981(8) 0.5600(5) 0.020(2) Uani 1 1 d . . .
H11A H 0.5216 0.7450 0.5166 0.024 Uiso 1 1 calc R . .
H11B H 0.5538 0.6467 0.5534 0.024 Uiso 1 1 calc R . .
C12 C 0.4168(5) 0.6569(7) 0.5458(5) 0.0162(18) Uani 1 1 d . . .
H12A H 0.4063 0.6047 0.5847 0.019 Uiso 1 1 calc R . .
H12B H 0.4132 0.6309 0.4899 0.019 Uiso 1 1 calc R . .
C13 C 0.2802(6) 0.3215(7) 0.6106(5) 0.0259(19) Uani 1 1 d . . .
H13A H 0.2278 0.2955 0.5818 0.031 Uiso 1 1 calc R . .
H13B H 0.3250 0.2706 0.6156 0.031 Uiso 1 1 calc R . .
C14 C 0.2526(6) 0.3546(7) 0.6957(5) 0.0229(19) Uani 1 1 d . . .
H14A H 0.2302 0.2993 0.7263 0.027 Uiso 1 1 calc R . .
H14B H 0.2024 0.3992 0.6896 0.027 Uiso 1 1 calc R . .
C15 C 0.4270(6) 0.3243(7) 0.7629(6) 0.031(2) Uani 1 1 d . . .
H15A H 0.4297 0.2996 0.8193 0.038 Uiso 1 1 calc R . .
H15B H 0.4108 0.2711 0.7268 0.038 Uiso 1 1 calc R . .
C16 C 0.5146(6) 0.3569(9) 0.7404(6) 0.033(3) Uani 1 1 d . . .
H16A H 0.5540 0.3010 0.7379 0.039 Uiso 1 1 calc R . .
H16B H 0.5366 0.3970 0.7855 0.039 Uiso 1 1 calc R . .
C17 C 0.4965(6) 0.3380(8) 0.5693(7) 0.040(3) Uani 1 1 d . . .
H17A H 0.5504 0.3195 0.5386 0.048 Uiso 1 1 calc R . .
H17B H 0.4745 0.2808 0.5975 0.048 Uiso 1 1 calc R . .
C18 C 0.4296(5) 0.3661(7) 0.5109(5) 0.0266(19) Uani 1 1 d . . .
H18A H 0.4134 0.3102 0.4780 0.032 Uiso 1 1 calc R . .
H18B H 0.4567 0.4127 0.4734 0.032 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
Ge1 0.0141(4) 0.0172(5) 0.0175(4) -0.0013(4) 0.0003(3) 0.0016(3)
Ge2 0.0199(3) 0.0139(4) 0.0142(3) -0.0004(4) -0.0043(3) -0.0004(3)
Ge3 0.0208(4) 0.0132(4) 0.0263(4) 0.0038(4) -0.0043(4) -0.0007(3)
Cl1 0.0170(9) 0.0300(12) 0.0207(10) -0.0007(9) 0.0039(7) -0.0090(8)
Cl2 0.0213(9) 0.0332(12) 0.0261(11) 0.0075(9) 0.0120(8) 0.0083(9)
Cl3 0.0209(9) 0.0313(12) 0.0271(11) -0.0009(9) 0.0079(8) -0.0005(8)
Cl4 0.0171(8) 0.0239(11) 0.0163(10) -0.0040(8) -0.0014(7) -0.0036(8)
Cl5 0.0260(10) 0.0515(15) 0.0327(11) 0.0150(11) 0.0125(9) 0.0095(10)
Cl6 0.0217(8) 0.0404(13) 0.0207(10) -0.0056(9) 0.0043(7) -0.0068(9)
S1 0.0168(10) 0.0168(12) 0.0181(11) -0.0035(9) -0.0024(8) 0.0019(8)
S2 0.0126(9) 0.0190(13) 0.0181(11) -0.0026(9) 0.0033(8) -0.0018(8)
S3 0.0113(8) 0.0175(12) 0.0207(10) 0.0023(10) -0.0012(8) -0.0013(8)
S4 0.0144(9) 0.0134(12) 0.0118(9) 0.0009(8) -0.0012(7) -0.0011(7)
S5 0.0139(9) 0.0185(12) 0.0128(10) -0.0019(8) 0.0035(7) -0.0016(7)
S6 0.0127(7) 0.0169(11) 0.0150(10) 0.0005(9) 0.0008(8) -0.0023(7)
S7 0.0156(9) 0.0141(12) 0.0215(10) 0.0030(8) -0.0022(8) -0.0023(8)
S8 0.0174(10) 0.0211(13) 0.0227(11) 0.0054(9) 0.0055(8) 0.0006(8)
S9 0.0146(10) 0.0180(14) 0.0200(13) -0.0022(9) -0.0009(7) -0.0006(9)
C1 0.023(4) 0.013(4) 0.015(3) -0.007(3) -0.005(3) -0.001(3)
C2 0.010(3) 0.027(4) 0.016(4) -0.004(3) -0.003(3) -0.001(3)
C3 0.018(3) 0.014(4) 0.012(3) 0.006(3) -0.002(2) -0.001(3)
C4 0.010(3) 0.033(6) 0.025(4) 0.019(4) -0.005(3) 0.002(3)
C5 0.021(4) 0.030(6) 0.028(5) -0.008(4) -0.001(3) 0.012(4)
C6 0.021(4) 0.024(5) 0.011(3) 0.004(3) 0.005(3) 0.000(3)
C7 0.007(3) 0.030(5) 0.032(5) 0.005(4) -0.004(3) -0.001(4)
C8 0.008(3) 0.035(6) 0.013(4) -0.004(4) 0.000(3) -0.006(4)
C9 0.013(3) 0.031(6) 0.019(4) 0.006(4) -0.004(3) -0.006(3)
C10 0.007(4) 0.013(5) 0.008(3) 0.008(3) 0.000(2) 0.001(3)
C11 0.015(4) 0.028(5) 0.018(4) 0.007(4) 0.006(3) -0.003(4)
C12 0.012(3) 0.028(5) 0.009(4) 0.002(3) -0.003(3) 0.001(3)
C13 0.023(4) 0.031(5) 0.024(4) 0.002(4) -0.003(3) -0.011(4)
C14 0.021(4) 0.028(5) 0.020(4) -0.001(3) 0.008(3) -0.016(3)
C15 0.036(4) 0.025(5) 0.034(5) 0.015(4) 0.001(4) 0.010(4)
C16 0.024(4) 0.049(7) 0.025(5) 0.018(5) 0.004(4) 0.013(4)
C17 0.024(5) 0.049(8) 0.046(6) -0.015(5) 0.006(4) -0.002(5)
C18 0.025(4) 0.033(5) 0.022(4) -0.011(4) 0.000(3) 0.000(4)

_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
Ge1 Cl2 2.299(2) . ?
Ge1 Cl1 2.308(2) . ?
Ge1 S1 2.721(3) . ?
Ge1 S2 2.741(3) 4_554 ?
Ge2 Cl3 2.285(2) . ?
Ge2 Cl4 2.315(2) . ?
Ge2 S4 2.721(2) . ?
Ge2 S5 2.744(3) 4_554 ?
Ge3 Cl5 2.288(3) . ?
Ge3 Cl6 2.305(3) . ?
Ge3 S8 2.697(3) 4_554 ?
Ge3 S7 2.782(3) . ?
S1 C1 1.789(9) . ?
S1 C6 1.818(8) . ?
S2 C3 1.799(7) . ?
S2 C2 1.829(8) . ?
S2 Ge1 2.741(3) 4 ?
S3 C5 1.796(11) . ?
S3 C4 1.804(9) . ?
S4 C7 1.819(10) . ?
S4 C12 1.844(9) . ?
S5 C9 1.804(9) . ?
S5 C8 1.830(9) . ?
S5 Ge2 2.744(3) 4 ?
S6 C11 1.829(10) . ?
S6 C10 1.833(8) . ?
S7 C13 1.803(9) . ?
S7 C18 1.843(8) . ?
S8 C15 1.816(9) . ?
S8 C14 1.842(9) . ?
S8 Ge3 2.697(3) 4 ?
S9 C16 1.809(11) . ?
S9 C17 1.813(12) . ?
C1 C2 1.561(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.540(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.550(12) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.480(13) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.520(12) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.532(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.529(12) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.442(13) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.445(14) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Ge1 Cl1 99.77(10) . . ?
Cl2 Ge1 S1 85.51(9) . . ?
Cl1 Ge1 S1 85.16(8) . . ?
Cl2 Ge1 S2 83.13(8) . 4_554 ?
Cl1 Ge1 S2 86.53(8) . 4_554 ?
S1 Ge1 S2 164.58(8) . 4_554 ?
Cl3 Ge2 Cl4 99.54(9) . . ?
Cl3 Ge2 S4 84.06(8) . . ?
Cl4 Ge2 S4 86.48(8) . . ?
Cl3 Ge2 S5 86.83(9) . 4_554 ?
Cl4 Ge2 S5 84.45(8) . 4_554 ?
S4 Ge2 S5 165.91(7) . 4_554 ?
Cl5 Ge3 Cl6 98.88(10) . . ?
Cl5 Ge3 S8 86.15(9) . 4_554 ?
Cl6 Ge3 S8 83.42(8) . 4_554 ?
Cl5 Ge3 S7 89.48(9) . . ?
Cl6 Ge3 S7 83.27(8) . . ?
S8 Ge3 S7 165.17(8) 4_554 . ?
C1 S1 C6 104.5(4) . . ?
C1 S1 Ge1 99.8(3) . . ?
C6 S1 Ge1 94.6(3) . . ?
C3 S2 C2 103.2(4) . . ?
C3 S2 Ge1 96.6(2) . 4 ?
C2 S2 Ge1 99.2(2) . 4 ?
C5 S3 C4 101.8(5) . . ?
C7 S4 C12 103.0(4) . . ?
C7 S4 Ge2 98.1(3) . . ?
C12 S4 Ge2 97.9(3) . . ?
C9 S5 C8 103.3(5) . . ?
C9 S5 Ge2 93.8(3) . 4 ?
C8 S5 Ge2 101.7(3) . 4 ?
C11 S6 C10 102.3(4) . . ?
C13 S7 C18 102.7(4) . . ?
C13 S7 Ge3 99.5(3) . . ?
C18 S7 Ge3 93.0(3) . . ?
C15 S8 C14 103.6(5) . . ?
C15 S8 Ge3 100.5(3) . 4 ?
C14 S8 Ge3 99.6(3) . 4 ?
C16 S9 C17 102.9(6) . . ?
C2 C1 S1 113.1(6) . . ?
C2 C1 H1A 109.0 . . ?
S1 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
S1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 S2 114.0(5) . . ?
C1 C2 H2A 108.8 . . ?
S2 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
S2 C2 H2B 108.8 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 S2 112.6(6) . . ?
C4 C3 H3A 109.1 . . ?
S2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
S2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 S3 116.6(5) . . ?
C3 C4 H4A 108.1 . . ?
S3 C4 H4A 108.1 . . ?
C3 C4 H4B 108.1 . . ?
S3 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C6 C5 S3 115.2(7) . . ?
C6 C5 H5A 108.5 . . ?
S3 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
S3 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
C5 C6 S1 114.3(6) . . ?
C5 C6 H6A 108.7 . . ?
S1 C6 H6A 108.7 . . ?
C5 C6 H6B 108.7 . . ?
S1 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
C8 C7 S4 116.6(6) . . ?
C8 C7 H7A 108.2 . . ?
S4 C7 H7A 108.2 . . ?
C8 C7 H7B 108.2 . . ?
S4 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 S5 113.3(7) . . ?
C7 C8 H8A 108.9 . . ?
S5 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
S5 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 S5 118.2(6) . . ?
C10 C9 H9A 107.8 . . ?
S5 C9 H9A 107.8 . . ?
C10 C9 H9B 107.8 . . ?
S5 C9 H9B 107.8 . . ?
H9A C9 H9B 107.1 . . ?
C9 C10 S6 112.3(6) . . ?
C9 C10 H10A 109.1 . . ?
S6 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
S6 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
C12 C11 S6 116.8(6) . . ?
C12 C11 H11A 108.1 . . ?
S6 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
S6 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 S4 111.0(7) . . ?
C11 C12 H12A 109.4 . . ?
S4 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
S4 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C14 C13 S7 110.9(6) . . ?
C14 C13 H13A 109.5 . . ?
S7 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
S7 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 S8 116.6(6) . . ?
C13 C14 H14A 108.1 . . ?
S8 C14 H14A 108.1 . . ?
C13 C14 H14B 108.1 . . ?
S8 C14 H14B 108.1 . . ?
H14A C14 H14B 107.3 . . ?
C16 C15 S8 115.5(7) . . ?
C16 C15 H15A 108.4 . . ?
S8 C15 H15A 108.4 . . ?
C16 C15 H15B 108.4 . . ?
S8 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
C15 C16 S9 119.8(7) . . ?
C15 C16 H16A 107.4 . . ?
S9 C16 H16A 107.4 . . ?
C15 C16 H16B 107.4 . . ?
S9 C16 H16B 107.4 . . ?
H16A C16 H16B 106.9 . . ?
C18 C17 S9 118.3(8) . . ?
C18 C17 H17A 107.7 . . ?
S9 C17 H17A 107.7 . . ?
C18 C17 H17B 107.7 . . ?
S9 C17 H17B 107.7 . . ?
H17A C17 H17B 107.1 . . ?
C17 C18 S7 116.8(7) . . ?
C17 C18 H18A 108.1 . . ?
S7 C18 H18A 108.1 . . ?
C17 C18 H18B 108.1 . . ?
S7 C18 H18B 108.1 . . ?
H18A C18 H18B 107.3 . . ?

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
Cl2 Ge1 S1 C1 79.9(3) . . . . ?
Cl1 Ge1 S1 C1 -179.8(3) . . . . ?
S2 Ge1 S1 C1 122.5(4) 4_554 . . . ?
Cl2 Ge1 S1 C6 -174.4(3) . . . . ?
Cl1 Ge1 S1 C6 -74.2(3) . . . . ?
S2 Ge1 S1 C6 -131.8(4) 4_554 . . . ?
Cl3 Ge2 S4 C7 175.8(4) . . . . ?
Cl4 Ge2 S4 C7 75.8(4) . . . . ?
S5 Ge2 S4 C7 125.8(5) 4_554 . . . ?
Cl3 Ge2 S4 C12 -79.8(3) . . . . ?
Cl4 Ge2 S4 C12 -179.8(3) . . . . ?
S5 Ge2 S4 C12 -129.8(4) 4_554 . . . ?
Cl5 Ge3 S7 C13 93.6(3) . . . . ?
Cl6 Ge3 S7 C13 -167.4(3) . . . . ?
S8 Ge3 S7 C13 166.4(4) 4_554 . . . ?
Cl5 Ge3 S7 C18 -163.0(3) . . . . ?
Cl6 Ge3 S7 C18 -64.0(3) . . . . ?
S8 Ge3 S7 C18 -90.2(4) 4_554 . . . ?
C6 S1 C1 C2 133.4(6) . . . . ?
Ge1 S1 C1 C2 -129.2(5) . . . . ?
S1 C1 C2 S2 -57.0(7) . . . . ?
C3 S2 C2 C1 -56.4(7) . . . . ?
Ge1 S2 C2 C1 -155.5(6) 4 . . . ?
C2 S2 C3 C4 133.2(6) . . . . ?
Ge1 S2 C3 C4 -125.8(5) 4 . . . ?
S2 C3 C4 S3 -55.8(9) . . . . ?
C5 S3 C4 C3 -59.1(9) . . . . ?
C4 S3 C5 C6 130.8(7) . . . . ?
S3 C5 C6 S1 -54.2(9) . . . . ?
C1 S1 C6 C5 -60.6(7) . . . . ?
Ge1 S1 C6 C5 -162.0(7) . . . . ?
C12 S4 C7 C8 59.8(9) . . . . ?
Ge2 S4 C7 C8 159.8(8) . . . . ?
S4 C7 C8 S5 53.5(9) . . . . ?
C9 S5 C8 C7 -130.0(7) . . . . ?
Ge2 S5 C8 C7 133.2(6) 4 . . . ?
C8 S5 C9 C10 59.0(8) . . . . ?
Ge2 S5 C9 C10 162.0(7) 4 . . . ?
S5 C9 C10 S6 55.2(8) . . . . ?
C11 S6 C10 C9 -129.8(6) . . . . ?
C10 S6 C11 C12 55.6(8) . . . . ?
S6 C11 C12 S4 56.6(8) . . . . ?
C7 S4 C12 C11 -133.1(6) . . . . ?
Ge2 S4 C12 C11 126.7(5) . . . . ?
C18 S7 C13 C14 131.8(6) . . . . ?
Ge3 S7 C13 C14 -132.9(6) . . . . ?
S7 C13 C14 S8 -55.6(9) . . . . ?
C15 S8 C14 C13 -57.2(8) . . . . ?
Ge3 S8 C14 C13 -160.5(7) 4 . . . ?
C14 S8 C15 C16 128.3(8) . . . . ?
Ge3 S8 C15 C16 -129.1(7) 4 . . . ?
S8 C15 C16 S9 -49.2(11) . . . . ?
C17 S9 C16 C15 -62.1(10) . . . . ?
C16 S9 C17 C18 126.5(9) . . . . ?
S9 C17 C18 S7 -50.6(11) . . . . ?
C13 S7 C18 C17 -63.2(8) . . . . ?
Ge3 S7 C18 C17 -163.6(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.63
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.110
_refine_diff_density_min         -1.432
_refine_diff_density_rms         0.134

#===END OF CIF ==============================================================
# 08wz403

data_08wz403_[C10H20Cl4Ge2S4]
_database_code_depnum_ccdc_archive 'CCDC 690318'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2008-04-18
_audit_author_name               'Webster, M.'
_audit_update_record             
; 2008-05-16 revised systematic name.
2008-07-27 added CH2Cl2 to systematic name.
2008-07-27 added treatment of CH2Cl2 to _refine_special_details
;

_chemical_name_systematic        
;
(1,4,8,11-tetrathiacyclotetradecane)bis(dichlorogermanium(II))
dichloromethane solvate
;

# 1,4,8,11-tetrathiacyclotetradecane = [14]aneS4
# tetrachloro(1,4,8,11-tetrathiacyclotetradecane)digermanium(II)

_chemical_name_common            
;
(1,4,8,11-
tetrathiacyclotetradecane)bis(dichlorogermanium(ii)) dichloromethane
solvate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H20 Cl4 Ge2 S4, 0.705(C H2 Cl2)'
_chemical_formula_sum            'C10.70 H21.41 Cl5.41 Ge2 S4'
_chemical_formula_weight         615.14

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c m'
_symmetry_Int_Tables_number      57 # Superceded **
_symmetry_space_group_name_Hall  '-P 2c 2b' # Superceded **

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

_cell_length_a                   4.9051(10)
_cell_length_b                   22.596(3)
_cell_length_c                   20.973(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2324.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2895
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       rhombus
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1222
_exptl_absorpt_coefficient_mu    3.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7878 # 0.5362
_exptl_absorpt_correction_T_max  1.0000 # 0.9007
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12862
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2721
_reflns_number_gt                2131
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 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.

The disordered CH2Cl2 solvate was modelled with C6 and Cl4 lying on a
mirror plane (x,y,1/4) and with the second Cl (Cl5) bonded to C6
occupying a disordered general position. All the atoms were given a
common refined sof. The largest residual peak (2.02 e A^-3^) was
1.98 A from Cl4 and 2.02 A from Cl5, but attempts to fit this to a
solvate model were not successful.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+25.7997P] 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         2721
_refine_ls_number_parameters     118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1572
_refine_ls_wR_factor_gt          0.1405
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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
Ge1 Ge 0.2146(2) 0.45260(5) 0.2500 0.0338(3) Uani 1 2 d S . .
Ge2 Ge 0.11639(19) 0.2500 0.5000 0.0223(2) Uani 1 2 d S . .
Cl1 Cl 0.4886(7) 0.37156(12) 0.2500 0.0421(6) Uani 1 2 d S . .
Cl2 Cl 0.5516(6) 0.52200(12) 0.2500 0.0411(6) Uani 1 2 d S . .
Cl3 Cl 0.4195(3) 0.25558(7) 0.41749(7) 0.0280(4) Uani 1 1 d . . .
S1 S 0.2411(3) 0.45255(7) 0.38146(7) 0.0245(3) Uani 1 1 d . . .
S2 S 0.1345(3) 0.37197(6) 0.51344(7) 0.0220(3) Uani 1 1 d . . .
C1 C -0.0074(15) 0.3939(3) 0.3886(3) 0.0299(14) Uani 1 1 d . . .
H1A H -0.1572 0.4015 0.3580 0.036 Uiso 1 1 calc R . .
H1B H 0.0800 0.3561 0.3761 0.036 Uiso 1 1 calc R . .
C2 C -0.1293(13) 0.3866(3) 0.4549(3) 0.0247(13) Uani 1 1 d . . .
H2A H -0.2614 0.3535 0.4546 0.030 Uiso 1 1 calc R . .
H2B H -0.2287 0.4231 0.4667 0.030 Uiso 1 1 calc R . .
C3 C -0.0611(16) 0.3711(3) 0.5871(3) 0.0330(16) Uani 1 1 d . . .
H3A H -0.1937 0.3382 0.5850 0.040 Uiso 1 1 calc R . .
H3B H 0.0647 0.3629 0.6229 0.040 Uiso 1 1 calc R . .
C4 C -0.2159(15) 0.4282(3) 0.6016(3) 0.0320(15) Uani 1 1 d . . .
H4A H -0.3555 0.4346 0.5682 0.038 Uiso 1 1 calc R . .
H4B H -0.3119 0.4237 0.6429 0.038 Uiso 1 1 calc R . .
C5 C -0.0338(13) 0.4819(3) 0.6049(3) 0.0252(13) Uani 1 1 d . . .
H5A H 0.0683 0.4862 0.5644 0.030 Uiso 1 1 calc R . .
H5B H 0.0995 0.4773 0.6400 0.030 Uiso 1 1 calc R . .
Cl4 Cl 0.2745(17) 0.1571(2) 0.2500 0.081(3) Uani 0.701(12) 2 d SP . .
Cl5 Cl -0.0934(19) 0.2509(5) 0.2171(6) 0.110(4) Uani 0.350(6) 1 d P . .
C6 C 0.216(6) 0.2293(8) 0.2500 0.068(7) Uani 0.701(12) 2 d SP . .
H6A H 0.3643 0.2491 0.2262 0.082 Uiso 0.350(6) 1 calc PR . .
H6B H 0.2233 0.2437 0.2946 0.082 Uiso 0.350(6) 1 calc PR . .

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
Ge1 0.0299(6) 0.0532(7) 0.0184(5) 0.000 0.000 0.0136(5)
Ge2 0.0218(5) 0.0198(4) 0.0251(5) -0.0015(3) 0.000 0.000
Cl1 0.0585(17) 0.0429(14) 0.0248(11) 0.000 0.000 0.0149(13)
Cl2 0.0506(16) 0.0488(14) 0.0238(11) 0.000 0.000 0.0075(12)
Cl3 0.0350(8) 0.0260(7) 0.0230(7) -0.0017(6) 0.0047(6) -0.0007(6)
S1 0.0253(8) 0.0283(8) 0.0199(7) 0.0002(6) 0.0011(6) 0.0060(6)
S2 0.0235(7) 0.0223(7) 0.0201(7) -0.0024(6) 0.0005(6) 0.0000(6)
C1 0.036(4) 0.026(3) 0.027(3) -0.001(3) -0.007(3) 0.003(3)
C2 0.020(3) 0.028(3) 0.026(3) 0.003(2) -0.005(3) 0.000(2)
C3 0.046(4) 0.028(3) 0.025(3) -0.002(3) 0.014(3) -0.013(3)
C4 0.034(4) 0.030(3) 0.031(3) -0.011(3) 0.012(3) -0.005(3)
C5 0.024(3) 0.024(3) 0.027(3) -0.009(2) -0.002(3) 0.004(2)
Cl4 0.155(7) 0.052(3) 0.035(2) 0.000 0.000 0.017(3)
Cl5 0.066(6) 0.095(6) 0.168(11) 0.020(6) 0.027(6) 0.022(5)
C6 0.14(2) 0.040(9) 0.026(8) 0.000 0.000 0.004(12)

_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
Ge1 Cl1 2.272(3) . ?
Ge1 Cl2 2.278(3) . ?
Ge1 S1 2.7602(15) . ?
Ge2 Cl3 2.2850(17) 4_556 ?
Ge2 Cl3 2.2850(17) . ?
Ge2 S2 2.7719(15) . ?
S1 C1 1.808(7) . ?
S1 C5 1.819(6) 5_566 ?
S2 C2 1.815(6) . ?
S2 C3 1.818(6) . ?
C1 C2 1.523(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.528(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.509(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 S1 1.819(6) 5_566 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
Cl4 C6 1.656(18) . ?
Cl5 Cl5 1.38(3) 6_556 ?
Cl5 C6 1.74(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Ge1 Cl2 97.22(12) . . ?
Cl1 Ge1 S1 88.38(4) . . ?
Cl2 Ge1 S1 88.06(4) . . ?
Cl3 Ge2 Cl3 98.81(9) 4_556 . ?
Cl3 Ge2 S2 87.53(5) 4_556 . ?
Cl3 Ge2 S2 90.07(5) . . ?
C1 S1 C5 102.0(3) . 5_566 ?
C1 S1 Ge1 92.9(2) . . ?
C5 S1 Ge1 97.5(2) 5_566 . ?
C2 S2 C3 101.6(3) . . ?
C2 S2 Ge2 95.1(2) . . ?
C3 S2 Ge2 93.4(2) . . ?
C2 C1 S1 114.8(4) . . ?
C2 C1 H1A 108.6 . . ?
S1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
S1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.5 . . ?
C1 C2 S2 111.0(5) . . ?
C1 C2 H2A 109.4 . . ?
S2 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
S2 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C4 C3 S2 115.0(5) . . ?
C4 C3 H3A 108.5 . . ?
S2 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
S2 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C5 C4 C3 113.2(6) . . ?
C5 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 S1 109.3(5) . 5_566 ?
C4 C5 H5A 109.8 . . ?
S1 C5 H5A 109.8 5_566 . ?
C4 C5 H5B 109.8 . . ?
S1 C5 H5B 109.8 5_566 . ?
H5A C5 H5B 108.3 . . ?
Cl5 Cl5 C6 66.6(5) 6_556 . ?
Cl4 C6 Cl5 115.4(14) . . ?
Cl4 C6 H6A 108.4 . . ?
Cl5 C6 H6A 108.4 . . ?
Cl4 C6 H6B 108.4 . . ?
Cl5 C6 H6B 108.4 . . ?
H6A C6 H6B 107.5 . . ?

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
Cl1 Ge1 S1 C1 -79.0(2) . . . . ?
Cl2 Ge1 S1 C1 -176.2(2) . . . . ?
Cl1 Ge1 S1 C5 178.6(2) . . . 5_566 ?
Cl2 Ge1 S1 C5 81.3(2) . . . 5_566 ?
Cl3 Ge2 S2 C2 -174.6(2) 4_556 . . . ?
Cl3 Ge2 S2 C2 86.6(2) . . . . ?
Cl3 Ge2 S2 C3 -72.6(3) 4_556 . . . ?
Cl3 Ge2 S2 C3 -171.4(3) . . . . ?
C5 S1 C1 C2 -65.9(5) 5_566 . . . ?
Ge1 S1 C1 C2 -164.2(5) . . . . ?
S1 C1 C2 S2 -58.6(6) . . . . ?
C3 S2 C2 C1 175.8(5) . . . . ?
Ge2 S2 C2 C1 -89.7(4) . . . . ?
C2 S2 C3 C4 -58.9(6) . . . . ?
Ge2 S2 C3 C4 -154.9(5) . . . . ?
S2 C3 C4 C5 -57.3(7) . . . . ?
C3 C4 C5 S1 177.3(5) . . . 5_566 ?
# Cl5 Cl5 C6 Cl4 101.9(9) 6_556 . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         2.016
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.172

#===END OF CIF ==============================================================
# 08wz012

data_08wz012_[C10H20Br2GeS4]
_database_code_depnum_ccdc_archive 'CCDC 690319'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2008-05-07
_audit_author_name               'Webster, M.'

_chemical_name_systematic        
;
catena(dibromo-(1,4,8,11-tetrathiacyclotetradecane)germanium(II))
;

# S ligand = [14]aneS~4~

_chemical_name_common            
;catena(dibromo-(1,4,8,11-
tetrathiacyclotetradecane)germanium(ii))
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H20 Br2 Ge S4'
_chemical_formula_sum            'C10 H20 Br2 Ge S4'
_chemical_formula_weight         500.91

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'
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'
Br Br -0.2901 2.4595 '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 2/n'
_symmetry_Int_Tables_number      13 # Superceded **
_symmetry_space_group_name_Hall  '-P 2yac' # Superceded **

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

_cell_length_a                   10.241(2)
_cell_length_b                   4.8585(10)
_cell_length_c                   17.778(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.475(10)
_cell_angle_gamma                90.00
_cell_volume                     863.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5514
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             492
_exptl_absorpt_coefficient_mu    6.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7422 # 0.3883
_exptl_absorpt_correction_T_max  1.0000 # 0.5469
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9076
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.67
_diffrn_reflns_theta_max         28.42
_reflns_number_total             1958
_reflns_number_gt                1738
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 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     
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.7323P] 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         1958
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0605
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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
Ge1 Ge 0.7500 0.18302(8) 0.2500 0.01562(11) Uani 1 2 d S . .
Br1 Br 0.59546(3) 0.50894(6) 0.169580(15) 0.02004(10) Uani 1 1 d . . .
S1 S 0.58846(6) 0.23575(14) 0.35423(4) 0.01654(15) Uani 1 1 d . . .
S2 S 0.28674(7) 0.19955(14) 0.39330(4) 0.01832(16) Uani 1 1 d . . .
C1 C 0.4548(3) 0.0147(6) 0.30330(17) 0.0192(6) Uani 1 1 d . . .
H1A H 0.4024 0.1173 0.2588 0.023 Uiso 1 1 calc R . .
H1B H 0.4952 -0.1464 0.2829 0.023 Uiso 1 1 calc R . .
C2 C 0.3600(3) -0.0877(6) 0.35214(16) 0.0177(5) Uani 1 1 d . . .
H2A H 0.4095 -0.2065 0.3940 0.021 Uiso 1 1 calc R . .
H2B H 0.2883 -0.1993 0.3199 0.021 Uiso 1 1 calc R . .
C3 C 0.1689(3) 0.0210(6) 0.43939(17) 0.0219(6) Uani 1 1 d . . .
H3A H 0.1130 0.1593 0.4586 0.026 Uiso 1 1 calc R . .
H3B H 0.1090 -0.0926 0.4003 0.026 Uiso 1 1 calc R . .
C4 C 0.2351(3) -0.1660(6) 0.50705(15) 0.0210(6) Uani 1 1 d . . .
H4A H 0.1647 -0.2586 0.5281 0.025 Uiso 1 1 calc R . .
H4B H 0.2881 -0.3099 0.4879 0.025 Uiso 1 1 calc R . .
C5 C 0.3253(3) -0.0055(6) 0.57064(16) 0.0217(6) Uani 1 1 d . . .
H5A H 0.2713 0.1283 0.5930 0.026 Uiso 1 1 calc R . .
H5B H 0.3918 0.0987 0.5490 0.026 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
Ge1 0.0158(2) 0.0122(2) 0.0196(2) 0.000 0.00565(17) 0.000
Br1 0.01841(15) 0.02201(16) 0.01912(16) 0.00026(10) 0.00280(12) 0.00408(10)
S1 0.0170(3) 0.0157(3) 0.0173(3) 0.0010(2) 0.0046(3) -0.0008(2)
S2 0.0214(3) 0.0158(3) 0.0189(3) 0.0006(3) 0.0071(3) -0.0023(3)
C1 0.0201(14) 0.0204(14) 0.0175(14) -0.0041(11) 0.0048(12) -0.0032(11)
C2 0.0209(13) 0.0130(13) 0.0188(13) 0.0002(11) 0.0033(11) -0.0015(11)
C3 0.0159(13) 0.0304(17) 0.0195(15) 0.0044(12) 0.0039(12) -0.0074(11)
C4 0.0220(14) 0.0237(15) 0.0173(14) 0.0004(11) 0.0043(12) -0.0054(11)
C5 0.0265(15) 0.0195(15) 0.0170(14) -0.0002(11) 0.0001(12) 0.0026(11)

_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
Ge1 Br1 2.4656(5) 2_655 ?
Ge1 Br1 2.4656(5) . ?
Ge1 S1 2.7498(8) . ?
Ge1 S1 2.7498(8) 2_655 ?
S1 C5 1.818(3) 3_656 ?
S1 C1 1.820(3) . ?
S2 C2 1.812(3) . ?
S2 C3 1.819(3) . ?
C1 C2 1.519(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.542(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.513(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 S1 1.818(3) 3_656 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Ge1 Br1 100.08(2) 2_655 . ?
Br1 Ge1 S1 87.34(2) 2_655 . ?
Br1 Ge1 S1 85.79(2) . . ?
Br1 Ge1 S1 85.79(2) 2_655 2_655 ?
Br1 Ge1 S1 87.34(2) . 2_655 ?
S1 Ge1 S1 169.31(3) . 2_655 ?
C5 S1 C1 101.31(14) 3_656 . ?
C5 S1 Ge1 99.80(10) 3_656 . ?
C1 S1 Ge1 96.15(9) . . ?
C2 S2 C3 100.81(13) . . ?
C2 C1 S1 114.4(2) . . ?
C2 C1 H1A 108.7 . . ?
S1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
S1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 S2 110.49(19) . . ?
C1 C2 H2A 109.6 . . ?
S2 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
S2 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 S2 114.19(19) . . ?
C4 C3 H3A 108.7 . . ?
S2 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
S2 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C5 C4 C3 111.9(2) . . ?
C5 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 S1 110.67(19) . 3_656 ?
C4 C5 H5A 109.5 . . ?
S1 C5 H5A 109.5 3_656 . ?
C4 C5 H5B 109.5 . . ?
S1 C5 H5B 109.5 3_656 . ?
H5A C5 H5B 108.1 . . ?

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
Br1 Ge1 S1 C5 -79.94(10) 2_655 . . 3_656 ?
Br1 Ge1 S1 C5 179.74(10) . . . 3_656 ?
S1 Ge1 S1 C5 -130.04(10) 2_655 . . 3_656 ?
Br1 Ge1 S1 C1 177.43(10) 2_655 . . . ?
Br1 Ge1 S1 C1 77.11(10) . . . . ?
S1 Ge1 S1 C1 127.32(10) 2_655 . . . ?
C5 S1 C1 C2 60.9(2) 3_656 . . . ?
Ge1 S1 C1 C2 162.25(19) . . . . ?
S1 C1 C2 S2 56.8(2) . . . . ?
C3 S2 C2 C1 174.7(2) . . . . ?
C2 S2 C3 C4 65.9(2) . . . . ?
S2 C3 C4 C5 60.2(3) . . . . ?
C3 C4 C5 S1 -175.53(19) . . . 3_656 ?

_diffrn_measured_fraction_theta_max 0.897
_diffrn_reflns_theta_full        28.42
_diffrn_measured_fraction_theta_full 0.897
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.120

#===END OF CIF ==============================================================
# 08wz405

data_08wz405_[C12H24Br2GeS4]
_database_code_depnum_ccdc_archive 'CCDC 690320'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2008-05-18
_audit_author_name               'Webster, M.'

_chemical_name_systematic        
;
catena-dibromo(\m~2~-1,5,9,13-tetrathiacyclohexadecane)germaniun(II)
;

# 1,5,9,13-tetrathiacyclohexadecane = [16]aneS4

_chemical_name_common            
;catena-dibromo(mu!2$-1,5,9,13-
tetrathiacyclohexadecane)germaniun(ii)
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 Br2 Ge S4'
_chemical_formula_sum            'C12 H24 Br2 Ge S4'
_chemical_formula_weight         528.96

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'
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'
Br Br -0.2901 2.4595 '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 2/c'
_symmetry_Int_Tables_number      13 # Superceded **
_symmetry_space_group_name_Hall  '-P 2yc' # Superceded **

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

_cell_length_a                   13.0690(15)
_cell_length_b                   4.9527(5)
_cell_length_c                   15.898(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.114(10)
_cell_angle_gamma                90.00
_cell_volume                     953.35(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2369
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             524
_exptl_absorpt_coefficient_mu    6.222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7884 #
_exptl_absorpt_correction_T_max  1.0000 #
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10369
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         27.52
_reflns_number_total             2194
_reflns_number_gt                1996
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 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     
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.8730P] 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         2194
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0458
_refine_ls_wR_factor_gt          0.0431
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.002
_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
Ge1 Ge 0.0000 0.12686(6) 0.7500 0.01677(8) Uani 1 2 d S . .
Br1 Br -0.058701(17) 0.43989(5) 0.621228(14) 0.02200(7) Uani 1 1 d . . .
S1 S 0.20773(4) 0.16705(11) 0.74842(3) 0.01791(12) Uani 1 1 d . . .
S2 S 0.39673(4) -0.10283(11) 0.59965(4) 0.02178(13) Uani 1 1 d . . .
C1 C 0.17991(17) -0.0483(5) 0.64929(15) 0.0210(5) Uani 1 1 d . . .
H1A H 0.2319 -0.2026 0.6654 0.025 Uiso 1 1 calc R . .
H1B H 0.1039 -0.1208 0.6297 0.025 Uiso 1 1 calc R . .
C2 C 0.19253(17) 0.1100(5) 0.57185(14) 0.0208(5) Uani 1 1 d . . .
H2A H 0.1462 0.2743 0.5610 0.025 Uiso 1 1 calc R . .
H2B H 0.1641 -0.0013 0.5161 0.025 Uiso 1 1 calc R . .
C3 C 0.31105(17) 0.1943(5) 0.58826(15) 0.0203(4) Uani 1 1 d . . .
H3A H 0.3410 0.3044 0.6442 0.024 Uiso 1 1 calc R . .
H3B H 0.3118 0.3057 0.5368 0.024 Uiso 1 1 calc R . .
C4 C 0.53116(17) 0.0522(5) 0.62737(15) 0.0211(5) Uani 1 1 d . . .
H4A H 0.5312 0.1662 0.5762 0.025 Uiso 1 1 calc R . .
H4B H 0.5487 0.1680 0.6818 0.025 Uiso 1 1 calc R . .
C5 C 0.61699(17) -0.1708(5) 0.64563(16) 0.0236(5) Uani 1 1 d . . .
H5A H 0.5923 -0.2999 0.5943 0.028 Uiso 1 1 calc R . .
H5B H 0.6216 -0.2699 0.7010 0.028 Uiso 1 1 calc R . .
C6 C 0.73185(17) -0.0670(5) 0.65806(15) 0.0237(5) Uani 1 1 d . . .
H6A H 0.7275 0.0233 0.6012 0.028 Uiso 1 1 calc R . .
H6B H 0.7820 -0.2237 0.6675 0.028 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
Ge1 0.01502(15) 0.01754(17) 0.01834(16) 0.000 0.00696(13) 0.000
Br1 0.02175(12) 0.02448(13) 0.01946(12) 0.00318(9) 0.00741(9) 0.00127(9)
S1 0.0161(2) 0.0205(3) 0.0178(3) 0.0002(2) 0.0071(2) 0.0005(2)
S2 0.0176(3) 0.0201(3) 0.0290(3) -0.0026(2) 0.0103(2) -0.0029(2)
C1 0.0176(10) 0.0223(12) 0.0246(11) -0.0048(9) 0.0095(9) -0.0039(9)
C2 0.0199(11) 0.0242(12) 0.0180(10) 0.0000(9) 0.0068(9) 0.0007(9)
C3 0.0224(11) 0.0205(11) 0.0213(11) 0.0002(9) 0.0121(9) -0.0003(9)
C4 0.0174(10) 0.0223(12) 0.0251(11) -0.0012(9) 0.0096(9) -0.0043(9)
C5 0.0194(11) 0.0245(12) 0.0264(12) -0.0049(10) 0.0082(9) -0.0019(9)
C6 0.0178(10) 0.0321(14) 0.0220(11) -0.0068(10) 0.0083(9) -0.0014(9)

_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
Ge1 Br1 2.4497(4) 2_556 ?
Ge1 Br1 2.4497(4) . ?
Ge1 S1 2.7316(6) . ?
Ge1 S1 2.7316(6) 2_556 ?
S1 C6 1.815(2) 2_656 ?
S1 C1 1.823(2) . ?
S2 C4 1.813(2) . ?
S2 C3 1.817(2) . ?
C1 C2 1.520(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.529(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.522(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.528(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 S1 1.815(2) 2_656 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Ge1 Br1 101.473(18) 2_556 . ?
Br1 Ge1 S1 87.817(15) 2_556 . ?
Br1 Ge1 S1 86.896(15) . . ?
Br1 Ge1 S1 86.896(15) 2_556 2_556 ?
Br1 Ge1 S1 87.817(15) . 2_556 ?
S1 Ge1 S1 171.64(3) . 2_556 ?
C6 S1 C1 102.61(11) 2_656 . ?
C6 S1 Ge1 94.21(7) 2_656 . ?
C1 S1 Ge1 95.16(7) . . ?
C4 S2 C3 100.71(10) . . ?
C2 C1 S1 110.58(15) . . ?
C2 C1 H1A 109.5 . . ?
S1 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
S1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 114.49(18) . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 S2 110.04(15) . . ?
C2 C3 H3A 109.7 . . ?
S2 C3 H3A 109.7 . . ?
C2 C3 H3B 109.7 . . ?
S2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C5 C4 S2 108.43(15) . . ?
C5 C4 H4A 110.0 . . ?
S2 C4 H4A 110.0 . . ?
C5 C4 H4B 110.0 . . ?
S2 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
C4 C5 C6 113.47(19) . . ?
C4 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 S1 115.11(15) . 2_656 ?
C5 C6 H6A 108.5 . . ?
S1 C6 H6A 108.5 2_656 . ?
C5 C6 H6B 108.5 . . ?
S1 C6 H6B 108.5 2_656 . ?
H6A C6 H6B 107.5 . . ?

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
# S1 Ge1 S1 C6 130.35(8) 2_556 . . 2_656 ?
# S1 Ge1 S1 C1 -126.56(7) 2_556 . . . ?
Br1 Ge1 S1 C6 79.57(8) 2_556 . . 2_656 ?
Br1 Ge1 S1 C6 -178.81(8) . . . 2_656 ?
Br1 Ge1 S1 C1 -177.34(7) 2_556 . . . ?
Br1 Ge1 S1 C1 -75.72(8) . . . . ?
C6 S1 C1 C2 -147.41(15) 2_656 . . . ?
Ge1 S1 C1 C2 117.09(14) . . . . ?
S1 C1 C2 C3 68.5(2) . . . . ?
C1 C2 C3 S2 62.9(2) . . . . ?
C4 S2 C3 C2 -175.49(14) . . . . ?
C3 S2 C4 C5 176.47(15) . . . . ?
S2 C4 C5 C6 172.70(15) . . . . ?
C4 C5 C6 S1 60.1(2) . . . 2_656 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.083

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