#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318096.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_4318096
loop_
_publ_author_name
'Ashley E. Ayers'
'H. V. Rasika Dias'
_publ_section_title
;
 Investigation of Silver Salt Metathesis: Preparation of Cationic
 Germanium(II) and Tin(II) Complexes, and Silver Adducts Containing
 Unsupported Silver-Germanium and Silver-Tin Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3259
_journal_page_last               3268
_journal_paper_doi               10.1021/ic0200747
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C14 H19 F3 Ge N2 O3 S'
_chemical_formula_weight         424.96
_chemical_name_common            '[(n-Pr)2ATI]GeOTf'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.348(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.558(3)
_cell_length_b                   7.3127(5)
_cell_length_c                   11.3595(13)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      4.93
_cell_volume                     877.0(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1681
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.79
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.910
_exptl_absorpt_correction_T_max  0.9742
_exptl_absorpt_correction_T_min  0.7496
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         1191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0363P)²+1.2989P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                1075
_reflns_number_total             1191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0200747_3.cif
_cod_data_source_block           rd258
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318096
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
Ge Ge 0.24536(6) 0.2500 0.65359(5) 0.0272(3) Uani 1 2 d S . .
N1 N 0.3377(5) 0.2500 0.8008(4) 0.0305(12) Uani 1 2 d S . .
N9 N 0.4141(4) 0.2500 0.5921(4) 0.0237(11) Uani 1 2 d S . .
S S 0.21686(14) -0.2500 0.69706(13) 0.0321(4) Uani 1 2 d S . .
O1 O 0.2676(3) -0.0876(5) 0.6432(3) 0.0512(10) Uani 1 1 d . . .
O2 O 0.2084(5) -0.2500 0.8204(4) 0.076(2) Uani 1 2 d S . .
F2 F -0.0086(3) -0.1046(5) 0.6880(3) 0.0698(10) Uani 1 1 d . . .
F1 F 0.0442(5) -0.2500 0.5333(4) 0.100(2) Uani 1 2 d S . .
C C 0.0521(7) -0.2500 0.6483(6) 0.0432(18) Uani 1 2 d S . .
C2 C 0.4655(6) 0.2500 0.7936(5) 0.0265(14) Uani 1 2 d S . .
C3 C 0.5407(6) 0.2500 0.8943(5) 0.0373(17) Uani 1 2 d S . .
H3A H 0.4955 0.2500 0.9653 0.045 Uiso 1 2 calc SR . .
C4 C 0.6718(6) 0.2500 0.9076(6) 0.0466(19) Uani 1 2 d S . .
H4A H 0.7014 0.2500 0.9858 0.056 Uiso 1 2 calc SR . .
C5 C 0.7635(6) 0.2500 0.8238(6) 0.049(2) Uani 1 2 d S . .
H5A H 0.8476 0.2500 0.8515 0.058 Uiso 1 2 calc SR . .
C6 C 0.7478(6) 0.2500 0.7032(6) 0.0415(17) Uani 1 2 d S . .
H6A H 0.8230 0.2500 0.6593 0.050 Uiso 1 2 calc SR . .
C7 C 0.6369(6) 0.2500 0.6376(5) 0.0366(16) Uani 1 2 d S . .
H7A H 0.6489 0.2500 0.5557 0.044 Uiso 1 2 calc SR . .
C8 C 0.5097(5) 0.2500 0.6724(5) 0.0260(14) Uani 1 2 d S . .
C10 C 0.2750(6) 0.2500 0.9143(5) 0.0333(15) Uani 1 2 d S . .
H10A H 0.299(4) 0.364(6) 0.958(4) 0.040 Uiso 1 1 d . . .
C11 C 0.1318(7) 0.2500 0.9052(6) 0.0438(18) Uani 1 2 d S . .
H11B H 0.112(5) 0.361(7) 0.857(4) 0.053 Uiso 1 1 d . . .
C12 C 0.0728(8) 0.2500 1.0270(7) 0.058(2) Uani 1 2 d S . .
H12A H -0.037(9) 0.2500 1.026(7) 0.087 Uiso 1 2 d S . .
H12C H 0.088(6) 0.366(9) 1.056(6) 0.087 Uiso 1 1 d . . .
C13 C 0.4433(6) 0.2500 0.4652(5) 0.0258(14) Uani 1 2 d S . .
H13B H 0.495(4) 0.359(6) 0.448(3) 0.031 Uiso 1 1 d . . .
C14 C 0.3245(6) 0.2500 0.3904(5) 0.0362(16) Uani 1 2 d S . .
H14A H 0.270(4) 0.361(6) 0.408(4) 0.043 Uiso 1 1 d . . .
C15 C 0.3589(8) 0.2500 0.2595(6) 0.048(2) Uani 1 2 d S . .
H15A H 0.286(8) 0.2500 0.206(7) 0.073 Uiso 1 2 d S . .
H15B H 0.409(5) 0.361(8) 0.238(5) 0.073 Uiso 1 1 d . . .
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'
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
N9 Ge N1 81.4(2) . . ?
C2 N1 C10 120.9(5) . . ?
C2 N1 Ge 116.5(4) . . ?
C10 N1 Ge 122.6(4) . . ?
C8 N9 C13 119.9(5) . . ?
C8 N9 Ge 116.4(4) . . ?
C13 N9 Ge 123.8(4) . . ?
O2 S O1 116.72(17) . . ?
O2 S O1 116.72(17) . 4 ?
O1 S O1 111.0(3) . 4 ?
O2 S C 103.7(3) . . ?
O1 S C 103.16(19) . . ?
O1 S C 103.16(19) 4 . ?
F1 C F2 108.2(4) . 4 ?
F1 C F2 108.2(4) . . ?
F2 C F2 107.0(5) 4 . ?
F1 C S 111.0(5) . . ?
F2 C S 111.1(3) 4 . ?
F2 C S 111.1(3) . . ?
N1 C2 C3 121.0(5) . . ?
N1 C2 C8 112.5(5) . . ?
C3 C2 C8 126.5(6) . . ?
C2 C3 C4 130.7(6) . . ?
C5 C4 C3 129.4(6) . . ?
C4 C5 C6 127.8(6) . . ?
C5 C6 C7 129.1(6) . . ?
C6 C7 C8 131.1(6) . . ?
N9 C8 C7 121.4(5) . . ?
N9 C8 C2 113.2(5) . . ?
C7 C8 C2 125.4(5) . . ?
N1 C10 C11 113.5(5) . . ?
C10 C11 C12 110.6(6) . . ?
N9 C13 C14 111.8(5) . . ?
C13 C14 C15 110.2(6) . . ?
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
Ge N9 1.918(5) . ?
Ge N1 1.930(5) . ?
N1 C2 1.353(8) . ?
N1 C10 1.453(7) . ?
N9 C8 1.356(7) . ?
N9 C13 1.476(7) . ?
S O2 1.405(5) . ?
S O1 1.441(3) . ?
S O1 1.441(3) 4 ?
S C 1.822(7) . ?
F2 C 1.322(5) . ?
F1 C 1.309(8) . ?
C F2 1.322(5) 4 ?
C2 C3 1.388(8) . ?
C2 C8 1.456(8) . ?
C3 C4 1.392(9) . ?
C4 C5 1.362(10) . ?
C5 C6 1.379(9) . ?
C6 C7 1.384(9) . ?
C7 C8 1.402(8) . ?
C10 C11 1.514(9) . ?
C11 C12 1.521(9) . ?
C13 C14 1.511(9) . ?
C14 C15 1.533(9) . ?
