#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318097.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_4318097
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 N2 O3 S Sn'
_chemical_formula_weight         471.06
_chemical_name_common            '[(n-Pr)2ATI]SnOTf'
_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                 90.513(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5691(15)
_cell_length_b                   7.3568(17)
_cell_length_c                   11.5109(17)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      5.23
_cell_volume                     895.0(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      208(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1707
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.77
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_T_max  0.8939
_exptl_absorpt_correction_T_min  0.7834
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         1223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0321
_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)+(0.0500P)²+1.0941P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                1135
_reflns_number_total             1223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0200747_4.cif
_cod_data_source_block           rd279
_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               4318097
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
Sn Sn 0.76815(4) 0.2500 0.85062(4) 0.0295(2) Uani 1 2 d S . .
S S 0.78922(15) -0.2500 0.80021(14) 0.0314(4) Uani 1 2 d S . .
O1 O 0.7385(3) -0.0889(5) 0.8522(3) 0.0551(11) Uani 1 1 d . . .
O2 O 0.7983(5) -0.2500 0.6787(4) 0.085(3) Uani 1 2 d S . .
N1 N 0.6566(5) 0.2500 0.6955(4) 0.0301(13) Uani 1 2 d S . .
N9 N 0.5776(5) 0.2500 0.9080(4) 0.0249(12) Uani 1 2 d S . .
C C 0.9531(7) -0.2500 0.8498(6) 0.045(2) Uani 1 2 d S . .
C2 C 0.5304(6) 0.2500 0.7058(5) 0.0288(15) Uani 1 2 d S . .
C3 C 0.4497(7) 0.2500 0.6085(6) 0.0391(18) Uani 1 2 d S . .
H3A H 0.4937 0.2500 0.5379 0.047 Uiso 1 2 calc SR . .
C4 C 0.3199(7) 0.2500 0.5933(6) 0.049(2) Uani 1 2 d S . .
H4A H 0.2910 0.2500 0.5158 0.059 Uiso 1 2 calc SR . .
C5 C 0.2273(7) 0.2500 0.6767(7) 0.053(2) Uani 1 2 d S . .
H5A H 0.1430 0.2500 0.6501 0.063 Uiso 1 2 calc SR . .
C6 C 0.2465(7) 0.2500 0.7955(6) 0.045(2) Uani 1 2 d S . .
H6A H 0.1723 0.2500 0.8400 0.054 Uiso 1 2 calc SR . .
C7 C 0.3571(6) 0.2500 0.8585(6) 0.0349(17) Uani 1 2 d S . .
H7A H 0.3445 0.2500 0.9392 0.042 Uiso 1 2 calc SR . .
C8 C 0.4846(6) 0.2500 0.8278(5) 0.0269(15) Uani 1 2 d S . .
C10 C 0.7140(7) 0.2500 0.5798(6) 0.0359(17) Uani 1 2 d S . .
C11 C 0.8566(8) 0.2500 0.5866(7) 0.046(2) Uani 1 2 d S . .
C12 C 0.9147(10) 0.2500 0.4653(8) 0.066(3) Uani 1 2 d S . .
C13 C 0.5448(6) 0.2500 1.0316(5) 0.0273(15) Uani 1 2 d S . .
C14 C 0.6605(8) 0.2500 1.1101(6) 0.0386(18) Uani 1 2 d S . .
C15 C 0.6234(10) 0.2500 1.2385(7) 0.051(2) Uani 1 2 d S . .
F1 F 0.9596(5) -0.2500 0.9624(4) 0.120(3) Uani 1 2 d S . .
F2 F 1.0133(3) -0.1062(5) 0.8109(4) 0.0751(11) Uani 1 1 d . . .
H10A H 0.678(5) 0.150(7) 0.536(4) 0.046(15) Uiso 1 1 d . . .
H15B H 0.581(6) 0.145(9) 1.256(5) 0.056(17) Uiso 1 1 d . . .
H14A H 0.713(4) 0.155(7) 1.095(4) 0.024(12) Uiso 1 1 d . . .
H15A H 0.691(10) 0.2500 1.292(9) 0.09(3) Uiso 1 2 d S . .
H12B H 0.883(6) 0.146(9) 0.431(5) 0.06(2) Uiso 1 1 d . . .
H11A H 0.879(5) 0.139(8) 0.620(4) 0.042(15) Uiso 1 1 d . . .
H12A H 1.002(8) 0.2500 0.467(6) 0.05(2) Uiso 1 2 d S . .
H13A H 0.505(6) 0.141(9) 1.043(5) 0.069 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'
Sn Sn -0.6537 1.4246 '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 Sn N1 75.03(19) . . ?
N9 Sn O1 83.06(8) . . ?
N1 Sn O1 86.45(10) . . ?
N9 Sn O1 83.06(8) . 4_565 ?
N1 Sn O1 86.45(10) . 4_565 ?
O1 Sn O1 165.64(16) . 4_565 ?
O2 S O1 116.4(2) . . ?
O2 S O1 116.4(2) . 4 ?
O1 S O1 111.5(3) . 4 ?
O2 S C 103.9(3) . . ?
O1 S C 103.2(2) . . ?
O1 S C 103.2(2) 4 . ?
S O1 Sn 140.3(2) . . ?
C2 N1 C10 120.0(5) . . ?
C2 N1 Sn 118.0(4) . . ?
C10 N1 Sn 122.0(4) . . ?
C8 N9 C13 119.3(5) . . ?
C8 N9 Sn 118.4(4) . . ?
C13 N9 Sn 122.3(4) . . ?
F1 C F2 108.6(4) . 4 ?
F1 C F2 108.6(4) . . ?
F2 C F2 107.1(6) 4 . ?
F1 C S 110.8(5) . . ?
F2 C S 110.8(4) 4 . ?
F2 C S 110.8(4) . . ?
N1 C2 C3 121.9(6) . . ?
N1 C2 C8 114.5(5) . . ?
C3 C2 C8 123.6(6) . . ?
C4 C3 C2 134.3(7) . . ?
C5 C4 C3 128.5(7) . . ?
C4 C5 C6 126.3(7) . . ?
C7 C6 C5 129.8(7) . . ?
C6 C7 C8 133.4(6) . . ?
N9 C8 C7 121.9(5) . . ?
N9 C8 C2 114.0(5) . . ?
C7 C8 C2 124.1(6) . . ?
N1 C10 C11 112.0(6) . . ?
C10 C11 C12 111.2(7) . . ?
N9 C13 C14 112.5(5) . . ?
C13 C14 C15 111.3(7) . . ?
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
Sn N9 2.125(5) . ?
Sn N1 2.131(5) . ?
Sn O1 2.513(4) . ?
Sn O1 2.513(4) 4_565 ?
S O2 1.403(5) . ?
S O1 1.434(4) . ?
S O1 1.434(4) 4 ?
S C 1.819(8) . ?
N1 C2 1.341(9) . ?
N1 C10 1.468(8) . ?
N9 C8 1.342(8) . ?
N9 C13 1.468(8) . ?
C F1 1.298(9) . ?
C F2 1.315(5) 4 ?
C F2 1.315(5) . ?
C2 C3 1.401(9) . ?
C2 C8 1.490(9) . ?
C3 C4 1.381(10) . ?
C4 C5 1.377(10) . ?
C5 C6 1.381(10) . ?
C6 C7 1.370(10) . ?
C7 C8 1.396(9) . ?
C10 C11 1.509(11) . ?
C11 C12 1.530(11) . ?
C13 C14 1.514(10) . ?
C14 C15 1.533(11) . ?
