#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:54:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179735 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/31/7003166.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7003166
loop_
_publ_author_name
'Davis, Martin F.'
'Levason, William'
'Reid, Gillian'
'Webster, Michael'
'Zhang, Wenjian'
_publ_section_title
;
 The first examples of germanium tetrafluoride and tin tetrafluoride
 complexes with soft thioether coordination---synthesis, properties and
 crystal structures
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              533
_journal_page_last               538
_journal_paper_doi               10.1039/b713316b
_journal_year                    2008
_chemical_formula_moiety         'C6 H14 F4 Ge S2'
_chemical_formula_sum            'C6 H14 F4 Ge S2'
_chemical_formula_weight         298.88
_chemical_name_common            Tetrafluorido(3,6-dithiaoctane)germanium(IV)
_chemical_name_systematic
;
Tetrafluorido(3,6-dithiaoctane)germanium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-06-23
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.202(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9011(15)
_cell_length_b                   8.5151(15)
_cell_length_c                   11.935(3)
_cell_measurement_reflns_used    2575
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1086.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13998
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.212
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0442P)²+0.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                2103
_reflns_number_total             2474
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b713316b.txt
_cod_data_source_block           07wz094_[C6H14F4GeS2]
_cod_original_cell_volume        1086.7(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7003166
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.73106(2) 0.05433(3) 0.38908(2) 0.01539(11) Uani 1 1 d . . .
F1 F 0.56958(14) 0.03429(18) 0.39027(14) 0.0218(4) Uani 1 1 d . . .
F2 F 0.71717(15) 0.24779(19) 0.33854(15) 0.0261(4) Uani 1 1 d . . .
F3 F 0.71852(15) -0.04027(19) 0.25659(14) 0.0252(4) Uani 1 1 d . . .
F4 F 0.89688(14) 0.05959(17) 0.41078(14) 0.0215(4) Uani 1 1 d . . .
S1 S 0.74011(6) 0.16029(8) 0.58236(6) 0.01689(16) Uani 1 1 d . . .
S2 S 0.76619(6) -0.20839(7) 0.48141(6) 0.01753(16) Uani 1 1 d . . .
C1 C 0.9181(3) 0.3869(4) 0.5845(3) 0.0346(8) Uani 1 1 d . . .
H1A H 1.0036 0.4233 0.6139 0.052 Uiso 1 1 calc R . .
H1B H 0.8585 0.4630 0.6046 0.052 Uiso 1 1 calc R . .
H1C H 0.9049 0.3767 0.5012 0.052 Uiso 1 1 calc R . .
C2 C 0.8985(2) 0.2285(3) 0.6368(2) 0.0213(6) Uani 1 1 d . . .
H2A H 0.9125 0.2382 0.7210 0.026 Uiso 1 1 calc R . .
H2B H 0.9593 0.1516 0.6176 0.026 Uiso 1 1 calc R . .
C3 C 0.7393(3) -0.0180(3) 0.6641(2) 0.0208(6) Uani 1 1 d . . .
H3A H 0.7707 0.0059 0.7458 0.025 Uiso 1 1 calc R . .
H3B H 0.6521 -0.0554 0.6560 0.025 Uiso 1 1 calc R . .
C4 C 0.8188(2) -0.1494(3) 0.6278(2) 0.0189(5) Uani 1 1 d . . .
H4A H 0.8166 -0.2414 0.6781 0.023 Uiso 1 1 calc R . .
H4B H 0.9067 -0.1134 0.6382 0.023 Uiso 1 1 calc R . .
C5 C 0.6131(2) -0.2903(3) 0.4880(2) 0.0206(6) Uani 1 1 d . . .
H5A H 0.6215 -0.3682 0.5506 0.025 Uiso 1 1 calc R . .
H5B H 0.5567 -0.2056 0.5040 0.025 Uiso 1 1 calc R . .
C6 C 0.5580(3) -0.3685(4) 0.3756(3) 0.0298(7) Uani 1 1 d . . .
H6A H 0.4759 -0.4125 0.3796 0.045 Uiso 1 1 calc R . .
H6B H 0.6137 -0.4529 0.3604 0.045 Uiso 1 1 calc R . .
H6C H 0.5488 -0.2908 0.3140 0.045 Uiso 1 1 calc R . .
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'
F F 0.0171 0.0103 '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'
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
F2 Ge1 F3 97.76(8) . . ?
F2 Ge1 F1 94.23(7) . . ?
F3 Ge1 F1 93.40(8) . . ?
F2 Ge1 F4 92.52(7) . . ?
F3 Ge1 F4 92.40(8) . . ?
F1 Ge1 F4 170.42(7) . . ?
F2 Ge1 S1 87.88(6) . . ?
F3 Ge1 S1 173.77(6) . . ?
F1 Ge1 S1 83.49(6) . . ?
F4 Ge1 S1 89.98(6) . . ?
F2 Ge1 S2 173.37(6) . . ?
F3 Ge1 S2 87.98(6) . . ?
F1 Ge1 S2 88.71(5) . . ?
F4 Ge1 S2 83.88(5) . . ?
S1 Ge1 S2 86.55(3) . . ?
C3 S1 C2 100.34(13) . . ?
C3 S1 Ge1 101.24(10) . . ?
C2 S1 Ge1 108.34(9) . . ?
C4 S2 C5 100.74(13) . . ?
C4 S2 Ge1 99.86(9) . . ?
C5 S2 Ge1 107.41(9) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 S1 109.7(2) . . ?
C1 C2 H2A 109.7 . . ?
S1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
S1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 S1 113.57(18) . . ?
C4 C3 H3A 108.9 . . ?
S1 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
S1 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C3 C4 S2 112.81(19) . . ?
C3 C4 H4A 109.0 . . ?
S2 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
S2 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C6 C5 S2 109.78(19) . . ?
C6 C5 H5A 109.7 . . ?
S2 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
S2 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
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 F2 1.7507(16) . ?
Ge1 F3 1.7561(16) . ?
Ge1 F1 1.7714(15) . ?
Ge1 F4 1.7761(15) . ?
Ge1 S1 2.4611(8) . ?
Ge1 S2 2.4903(8) . ?
S1 C3 1.805(3) . ?
S1 C2 1.818(3) . ?
S2 C4 1.802(3) . ?
S2 C5 1.825(3) . ?
C1 C2 1.519(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.529(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.514(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
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
F2 Ge1 S1 C3 174.32(11) . . . . ?
F1 Ge1 S1 C3 79.81(10) . . . . ?
F4 Ge1 S1 C3 -93.15(10) . . . . ?
S2 Ge1 S1 C3 -9.28(9) . . . . ?
F2 Ge1 S1 C2 -80.69(11) . . . . ?
F1 Ge1 S1 C2 -175.20(11) . . . . ?
F4 Ge1 S1 C2 11.83(11) . . . . ?
S2 Ge1 S1 C2 95.71(10) . . . . ?
F3 Ge1 S2 C4 167.63(10) . . . . ?
F1 Ge1 S2 C4 -98.92(10) . . . . ?
F4 Ge1 S2 C4 74.99(10) . . . . ?
S1 Ge1 S2 C4 -15.36(9) . . . . ?
F3 Ge1 S2 C5 -87.73(11) . . . . ?
F1 Ge1 S2 C5 5.73(11) . . . . ?
F4 Ge1 S2 C5 179.64(11) . . . . ?
S1 Ge1 S2 C5 89.29(10) . . . . ?
C3 S1 C2 C1 -176.2(2) . . . . ?
Ge1 S1 C2 C1 78.2(2) . . . . ?
C2 S1 C3 C4 -71.4(2) . . . . ?
Ge1 S1 C3 C4 39.9(2) . . . . ?
S1 C3 C4 S2 -60.9(2) . . . . ?
C5 S2 C4 C3 -65.3(2) . . . . ?
Ge1 S2 C4 C3 44.70(19) . . . . ?
C4 S2 C5 C6 -172.3(2) . . . . ?
Ge1 S2 C5 C6 83.7(2) . . . . ?
