#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/72/4307277.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_4307277
loop_
_publ_author_name
'Teresita Munguia'
'Marcela López-Cardoso'
'Francisco Cervantes-Lee'
'Keith H. Pannell'
_publ_section_title
;
Intramolecular Chalcogen-Tin Interactions in (o-MeE-C6H4)CH2SnPh3-nCln (E
= S, O; n= 0, 1, 2), Characterized by X-ray Diffraction and 119Sn Solution
and Solid-State NMR
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1305
_journal_page_last               1314
_journal_paper_doi               10.1021/ic061811s
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C20 H19 Cl S Sn'
_chemical_formula_weight         445.55
_chemical_name_systematic
; 
 (2-thiomethylbenzyl)triphenyltin 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.8220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8031(6)
_cell_length_b                   27.5903(18)
_cell_length_c                   8.5728(6)
_cell_measurement_reflns_used    4520
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.272
_cell_measurement_theta_min      2.529
_cell_volume                     1904.8(2)
_computing_cell_refinement       'Bruker SMART V5.625, 2001'
_computing_data_collection       'Bruker SMART V5.625, 2001'
_computing_data_reduction        'Bruker SAINT V5.622, 2001'
_computing_molecular_graphics    'Bruker SHELXTL V6.10, 2000'
_computing_publication_material  'Bruker SHELXTL V6.10, 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11995
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_T_max  0.9107
_exptl_absorpt_correction_T_min  0.7852
_exptl_absorpt_correction_type   'Bruker SADABS V2.05'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.425
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.425
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          1.285
_refine_ls_shift/su_mean         0.110
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1093P)²+13.0580P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                3610
_reflns_number_total             4411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061811ssi20060922_123928_4.cif
_cod_data_source_block           tm853
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4307277
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
Sn1 Sn 0.28621(3) 0.398108(8) 0.80451(3) 0.04732(9) Uani 1 1 d . . .
Cl1 Cl 0.52915(13) 0.41485(4) 1.06098(13) 0.0765(3) Uani 1 1 d . . .
S2 S -0.03223(11) 0.39928(3) 0.47736(12) 0.0574(2) Uani 1 1 d . . .
C1 C 0.1916(4) 0.47009(12) 0.7263(5) 0.0614(9) Uani 1 1 d . . .
H1A H 0.2554 0.4931 0.8136 0.074 Uiso 1 1 calc R . .
H1B H 0.2037 0.4785 0.6220 0.074 Uiso 1 1 calc R . .
C2 C 0.0137(5) 0.47315(12) 0.6974(4) 0.0581(8) Uani 1 1 d . . .
C3 C -0.1054(4) 0.44022(12) 0.5895(4) 0.0537(7) Uani 1 1 d . . .
C4 C -0.2679(5) 0.44136(16) 0.5720(5) 0.0708(10) Uani 1 1 d . . .
H4 H -0.3447 0.4196 0.4993 0.085 Uiso 1 1 calc R . .
C5 C -0.3162(6) 0.4745(2) 0.6618(6) 0.0849(13) Uani 1 1 d . . .
H5 H -0.4251 0.4747 0.6527 0.102 Uiso 1 1 calc R . .
C6 C -0.2029(6) 0.50791(19) 0.7661(6) 0.0837(13) Uani 1 1 d . . .
H6 H -0.2367 0.5308 0.8251 0.100 Uiso 1 1 calc R . .
C7 C -0.0399(6) 0.50739(14) 0.7830(5) 0.0696(10) Uani 1 1 d . . .
H7 H 0.0346 0.5302 0.8523 0.084 Uiso 1 1 calc R . .
C8 C -0.1574(5) 0.34646(15) 0.4530(6) 0.0780(11) Uani 1 1 d . . .
H8A H -0.1577 0.3377 0.5613 0.117 Uiso 1 1 calc R . .
H8B H -0.1128 0.3202 0.4111 0.117 Uiso 1 1 calc R . .
H8C H -0.2690 0.3531 0.3735 0.117 Uiso 1 1 calc R . .
C9 C 0.1522(4) 0.35319(11) 0.9083(4) 0.0474(7) Uani 1 1 d . . .
C10 C 0.1838(5) 0.30388(12) 0.9250(5) 0.0579(8) Uani 1 1 d . . .
H10 H 0.2588 0.2907 0.8853 0.070 Uiso 1 1 calc R . .
C11 C 0.1062(6) 0.27372(14) 0.9995(6) 0.0714(10) Uani 1 1 d . . .
H11 H 0.1291 0.2407 1.0101 0.086 Uiso 1 1 calc R . .
C12 C -0.0051(6) 0.29326(16) 1.0576(5) 0.0750(11) Uani 1 1 d . . .
H12 H -0.0571 0.2733 1.1086 0.090 Uiso 1 1 calc R . .
C13 C -0.0401(5) 0.34176(16) 1.0411(5) 0.0717(10) Uani 1 1 d . . .
H13 H -0.1164 0.3546 1.0797 0.086 Uiso 1 1 calc R . .
C14 C 0.0384(5) 0.37184(13) 0.9667(5) 0.0596(8) Uani 1 1 d . . .
H14 H 0.0143 0.4048 0.9558 0.072 Uiso 1 1 calc R . .
C15 C 0.3958(4) 0.35652(13) 0.6674(4) 0.0539(7) Uani 1 1 d . . .
C16 C 0.5163(6) 0.32262(16) 0.7519(6) 0.0746(11) Uani 1 1 d . . .
H16 H 0.5576 0.3207 0.8702 0.090 Uiso 1 1 calc R . .
C17 C 0.5768(7) 0.29153(18) 0.6649(8) 0.0958(16) Uani 1 1 d . . .
H17 H 0.6574 0.2688 0.7248 0.115 Uiso 1 1 calc R . .
C18 C 0.5192(8) 0.2938(2) 0.4911(9) 0.0968(17) Uani 1 1 d . . .
H18 H 0.5583 0.2724 0.4320 0.116 Uiso 1 1 calc R . .
C19 C 0.4024(7) 0.3283(3) 0.4049(7) 0.1017(19) Uani 1 1 d . . .
H19 H 0.3650 0.3308 0.2871 0.122 Uiso 1 1 calc R . .
C20 C 0.3406(5) 0.3591(2) 0.4911(5) 0.0797(12) Uani 1 1 d . . .
H20 H 0.2608 0.3819 0.4307 0.096 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'
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'
Cl Cl 0.1484 0.1585 '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
C15 Sn1 C9 111.49(13) . . ?
C15 Sn1 C1 121.93(15) . . ?
C9 Sn1 C1 117.08(13) . . ?
C15 Sn1 Cl1 100.00(10) . . ?
C9 Sn1 Cl1 99.60(9) . . ?
C1 Sn1 Cl1 101.32(10) . . ?
C3 S2 C8 104.0(2) . . ?
C2 C1 Sn1 110.7(2) . . ?
C7 C2 C3 117.5(4) . . ?
C7 C2 C1 120.7(4) . . ?
C3 C2 C1 121.7(3) . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 S2 123.1(3) . . ?
C2 C3 S2 115.5(3) . . ?
C5 C4 C3 119.9(4) . . ?
C4 C5 C6 120.1(4) . . ?
C7 C6 C5 120.4(4) . . ?
C6 C7 C2 120.7(4) . . ?
C10 C9 C14 118.1(3) . . ?
C10 C9 Sn1 119.4(2) . . ?
C14 C9 Sn1 122.4(2) . . ?
C11 C10 C9 121.5(4) . . ?
C10 C11 C12 119.2(4) . . ?
C13 C12 C11 120.6(4) . . ?
C14 C13 C12 120.0(4) . . ?
C13 C14 C9 120.7(3) . . ?
C20 C15 C16 117.6(4) . . ?
C20 C15 Sn1 122.3(3) . . ?
C16 C15 Sn1 119.9(3) . . ?
C17 C16 C15 121.4(4) . . ?
C18 C17 C16 120.5(5) . . ?
C17 C18 C19 119.0(5) . . ?
C18 C19 C20 120.7(5) . . ?
C15 C20 C19 120.8(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 C15 2.132(3) . ?
Sn1 C9 2.137(3) . ?
Sn1 C1 2.153(3) . ?
Sn1 Cl1 2.4130(9) . ?
S2 C3 1.765(4) . ?
S2 C8 1.788(4) . ?
C1 C2 1.486(5) . ?
C2 C7 1.390(5) . ?
C2 C3 1.413(5) . ?
C3 C4 1.377(5) . ?
C4 C5 1.370(6) . ?
C5 C6 1.386(7) . ?
C6 C7 1.382(6) . ?
C9 C10 1.385(4) . ?
C9 C14 1.387(5) . ?
C10 C11 1.385(5) . ?
C11 C12 1.376(6) . ?
C12 C13 1.368(6) . ?
C13 C14 1.389(5) . ?
C15 C20 1.390(5) . ?
C15 C16 1.380(6) . ?
C16 C17 1.377(6) . ?
C17 C18 1.368(8) . ?
C18 C19 1.376(9) . ?
C19 C20 1.374(7) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660839
