#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318098.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_4318098
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            'C13 H19 I N2 Sn'
_chemical_formula_weight         448.89
_chemical_name_common            '[(n-Pr)2ATI]SnI'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.296(6)
_cell_angle_beta                 80.879(8)
_cell_angle_gamma                73.331(11)
_cell_formula_units_Z            4
_cell_length_a                   8.5771(7)
_cell_length_b                   9.9182(9)
_cell_length_c                   18.8976(13)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      5.10
_cell_volume                     1507.6(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens 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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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    0.0315
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4808
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.16
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.725
_exptl_absorpt_correction_T_max  0.9978
_exptl_absorpt_correction_T_min  0.7572
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpipeds
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0308P)²+3.8030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                3518
_reflns_number_total             3853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0200747_5.cif
_cod_data_source_block           rd261a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4318098
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Sn1 Sn -0.07591(6) 0.19455(4) -0.50975(2) 0.03999(14) Uani 1 1 d . . .
Sn2 Sn 0.15900(5) 0.81860(4) 0.03831(2) 0.03206(13) Uani 1 1 d . . .
I1 I -0.37310(6) 0.11625(4) -0.44944(3) 0.04843(15) Uani 1 1 d . . .
I2 I -0.13535(5) 0.78742(5) 0.13476(2) 0.04590(14) Uani 1 1 d . . .
N1 N -0.0378(8) 0.2394(6) -0.4076(3) 0.0562(17) Uani 1 1 d . . .
N9 N -0.1940(6) 0.4169(5) -0.5066(3) 0.0323(11) Uani 1 1 d . . .
N16 N 0.1985(6) 0.6226(5) -0.0046(2) 0.0300(11) Uani 1 1 d . . .
N24 N 0.3153(6) 0.6594(5) 0.1071(2) 0.0294(11) Uani 1 1 d . . .
C2 C -0.0968(7) 0.3703(6) -0.3918(3) 0.0354(14) Uani 1 1 d . . .
C3 C -0.0753(8) 0.4057(7) -0.3254(3) 0.0435(16) Uani 1 1 d . . .
H3A H -0.0149 0.3297 -0.2963 0.052 Uiso 1 1 calc R . .
C4 C -0.1253(9) 0.5295(7) -0.2950(4) 0.0486(17) Uani 1 1 d . . .
H4A H -0.0905 0.5238 -0.2502 0.058 Uiso 1 1 calc R . .
C5 C -0.2188(10) 0.6606(8) -0.3208(4) 0.056(2) Uani 1 1 d . . .
H5A H -0.2416 0.7318 -0.2914 0.067 Uiso 1 1 calc R . .
C6 C -0.2823(9) 0.6967(7) -0.3863(4) 0.0502(18) Uani 1 1 d . . .
H6A H -0.3436 0.7905 -0.3952 0.060 Uiso 1 1 calc R . .
C7 C -0.2691(8) 0.6155(6) -0.4404(3) 0.0394(15) Uani 1 1 d . . .
H7A H -0.3234 0.6647 -0.4797 0.047 Uiso 1 1 calc R . .
C8 C -0.1888(7) 0.4719(6) -0.4478(3) 0.0324(14) Uani 1 1 d . . .
C10 C 0.0341(11) 0.1073(11) -0.3502(5) 0.085(3) Uani 1 1 d . . .
H10A H -0.0130 0.1251 -0.3014 0.102 Uiso 1 1 calc R . .
H10B H 0.0121 0.0218 -0.3598 0.102 Uiso 1 1 calc R . .
C11 C 0.2005(12) 0.0949(11) -0.3596(6) 0.091(3) Uani 1 1 d . . .
H11A H 0.2235 0.1763 -0.3455 0.110 Uiso 1 1 calc R . .
H11B H 0.2462 0.0856 -0.4094 0.110 Uiso 1 1 calc R . .
C12 C 0.2725(11) -0.0485(8) -0.3065(4) 0.073(3) Uani 1 1 d . . .
H12A H 0.3892 -0.0661 -0.3089 0.109 Uiso 1 1 calc R . .
H12B H 0.2476 -0.1271 -0.3214 0.109 Uiso 1 1 calc R . .
H12C H 0.2235 -0.0374 -0.2578 0.109 Uiso 1 1 calc R . .
C13 C -0.2845(8) 0.5028(6) -0.5649(3) 0.0370(14) Uani 1 1 d . . .
H13A H -0.2373 0.5810 -0.5848 0.044 Uiso 1 1 calc R . .
H13B H -0.3972 0.5425 -0.5456 0.044 Uiso 1 1 calc R . .
C14 C -0.2820(9) 0.4182(7) -0.6245(3) 0.0430(16) Uani 1 1 d . . .
H14A H -0.3316 0.3413 -0.6049 0.052 Uiso 1 1 calc R . .
H14B H -0.1693 0.3769 -0.6432 0.052 Uiso 1 1 calc R . .
C15 C -0.3743(11) 0.5105(8) -0.6861(4) 0.063(2) Uani 1 1 d . . .
H15A H -0.3649 0.4548 -0.7243 0.095 Uiso 1 1 calc R . .
H15B H -0.3283 0.5889 -0.7043 0.095 Uiso 1 1 calc R . .
H15C H -0.4878 0.5457 -0.6685 0.095 Uiso 1 1 calc R . .
C17 C 0.2868(7) 0.5040(6) 0.0309(3) 0.0293(13) Uani 1 1 d . . .
C18 C 0.3126(8) 0.3709(6) 0.0068(3) 0.0373(15) Uani 1 1 d . . .
H18A H 0.2622 0.3755 -0.0339 0.045 Uiso 1 1 calc R . .
C19 C 0.3987(8) 0.2352(7) 0.0325(4) 0.0438(16) Uani 1 1 d . . .
H19A H 0.3992 0.1654 0.0051 0.053 Uiso 1 1 calc R . .
C20 C 0.4831(8) 0.1867(6) 0.0912(4) 0.0423(16) Uani 1 1 d . . .
H20A H 0.5346 0.0901 0.0984 0.051 Uiso 1 1 calc R . .
C21 C 0.4991(8) 0.2678(7) 0.1409(4) 0.0427(16) Uani 1 1 d . . .
H21A H 0.5577 0.2179 0.1788 0.051 Uiso 1 1 calc R . .
C22 C 0.4396(7) 0.4142(7) 0.1422(3) 0.0387(15) Uani 1 1 d . . .
H22A H 0.4649 0.4443 0.1819 0.046 Uiso 1 1 calc R . .
C23 C 0.3493(7) 0.5257(6) 0.0959(3) 0.0309(13) Uani 1 1 d . . .
C25 C 0.1314(7) 0.6152(6) -0.0696(3) 0.0322(13) Uani 1 1 d . . .
H25A H 0.0548 0.5571 -0.0573 0.039 Uiso 1 1 calc R . .
H25B H 0.2194 0.5704 -0.1040 0.039 Uiso 1 1 calc R . .
C26 C 0.0435(8) 0.7630(7) -0.1044(3) 0.0395(15) Uani 1 1 d . . .
H26A H 0.1199 0.8212 -0.1172 0.047 Uiso 1 1 calc R . .
H26B H -0.0447 0.8083 -0.0701 0.047 Uiso 1 1 calc R . .
C27 C -0.0263(9) 0.7512(8) -0.1725(3) 0.0500(18) Uani 1 1 d . . .
H27A H -0.0791 0.8444 -0.1944 0.075 Uiso 1 1 calc R . .
H27B H -0.1045 0.6961 -0.1594 0.075 Uiso 1 1 calc R . .
H27C H 0.0611 0.7056 -0.2061 0.075 Uiso 1 1 calc R . .
C28 C 0.3754(8) 0.6966(6) 0.1679(3) 0.0354(14) Uani 1 1 d . . .
H28A H 0.4940 0.6624 0.1634 0.042 Uiso 1 1 calc R . .
H28B H 0.3325 0.6494 0.2128 0.042 Uiso 1 1 calc R . .
C29 C 0.3258(8) 0.8552(7) 0.1709(3) 0.0397(15) Uani 1 1 d . . .
H29A H 0.2074 0.8902 0.1743 0.048 Uiso 1 1 calc R . .
H29B H 0.3714 0.9026 0.1267 0.048 Uiso 1 1 calc R . .
C30 C 0.3858(9) 0.8901(7) 0.2354(4) 0.0487(17) Uani 1 1 d . . .
H30A H 0.3518 0.9909 0.2362 0.073 Uiso 1 1 calc R . .
H30B H 0.5032 0.8577 0.2314 0.073 Uiso 1 1 calc R . .
H30C H 0.3401 0.8437 0.2791 0.073 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'
N N 0.0061 0.0033 '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'
I I -0.4742 1.8119 '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
N1 Sn1 N9 74.19(19) . . ?
N1 Sn1 I1 92.44(19) . . ?
N9 Sn1 I1 92.23(13) . . ?
N16 Sn2 N24 74.23(17) . . ?
N16 Sn2 I2 94.43(13) . . ?
N24 Sn2 I2 91.71(12) . . ?
C2 N1 C10 123.3(6) . . ?
C2 N1 Sn1 118.6(4) . . ?
C10 N1 Sn1 117.3(4) . . ?
C8 N9 C13 120.9(5) . . ?
C8 N9 Sn1 117.8(4) . . ?
C13 N9 Sn1 121.3(4) . . ?
C17 N16 C25 119.7(5) . . ?
C17 N16 Sn2 117.9(4) . . ?
C25 N16 Sn2 122.4(4) . . ?
C23 N24 C28 120.4(5) . . ?
C23 N24 Sn2 118.4(4) . . ?
C28 N24 Sn2 121.2(4) . . ?
N1 C2 C3 121.0(6) . . ?
N1 C2 C8 114.7(5) . . ?
C3 C2 C8 124.4(6) . . ?
C4 C3 C2 133.0(6) . . ?
C3 C4 C5 129.8(7) . . ?
C4 C5 C6 126.2(7) . . ?
C7 C6 C5 130.1(7) . . ?
C6 C7 C8 132.4(6) . . ?
N9 C8 C7 121.1(5) . . ?
N9 C8 C2 114.8(5) . . ?
C7 C8 C2 124.1(6) . . ?
C11 C10 N1 104.0(8) . . ?
C10 C11 C12 103.0(8) . . ?
N9 C13 C14 112.3(5) . . ?
C13 C14 C15 111.7(6) . . ?
N16 C17 C18 120.7(5) . . ?
N16 C17 C23 114.6(5) . . ?
C18 C17 C23 124.8(5) . . ?
C19 C18 C17 132.2(6) . . ?
C20 C19 C18 130.7(7) . . ?
C19 C20 C21 126.1(6) . . ?
C20 C21 C22 129.2(6) . . ?
C21 C22 C23 133.4(6) . . ?
N24 C23 C22 121.8(6) . . ?
N24 C23 C17 114.7(5) . . ?
C22 C23 C17 123.6(5) . . ?
N16 C25 C26 111.5(5) . . ?
C25 C26 C27 110.1(5) . . ?
N24 C28 C29 112.4(5) . . ?
C28 C29 C30 111.2(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
Sn1 N1 2.145(6) . ?
Sn1 N9 2.154(5) . ?
Sn1 I1 2.8837(7) . ?
Sn2 N16 2.148(5) . ?
Sn2 N24 2.151(4) . ?
Sn2 I2 2.9310(7) . ?
N1 C2 1.318(8) . ?
N1 C10 1.595(12) . ?
N9 C8 1.330(8) . ?
N9 C13 1.455(7) . ?
N16 C17 1.338(7) . ?
N16 C25 1.457(7) . ?
N24 C23 1.320(7) . ?
N24 C28 1.470(7) . ?
C2 C3 1.411(9) . ?
C2 C8 1.485(8) . ?
C3 C4 1.370(10) . ?
C4 C5 1.372(10) . ?
C5 C6 1.381(10) . ?
C6 C7 1.377(9) . ?
C7 C8 1.413(8) . ?
C10 C11 1.382(12) . ?
C11 C12 1.619(12) . ?
C13 C14 1.507(9) . ?
C14 C15 1.530(9) . ?
C17 C18 1.414(8) . ?
C17 C23 1.486(8) . ?
C18 C19 1.384(9) . ?
C19 C20 1.363(9) . ?
C20 C21 1.381(10) . ?
C21 C22 1.397(9) . ?
C22 C23 1.409(8) . ?
C25 C26 1.532(8) . ?
C26 C27 1.538(9) . ?
C28 C29 1.515(9) . ?
C29 C30 1.521(9) . ?
