#------------------------------------------------------------------------------
#$Date: 2025-02-13 17:45:00 +0200 (Thu, 13 Feb 2025) $
#$Revision: 297721 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/07/4060773.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_4060773
loop_
_publ_author_name
'Cera, Martin'
'Cerrada, Elena'
'Laguna, Mariano'
'Mata, José A.'
'Teruel, Helena'
_publ_section_title
;
Ortho-Metalated Benzenethiolate Bridging Dinuclear Palladium(II) Complexes. 
X-ray Structures of [Sn₂(μ-C₆H₄S)₂(tBu)₄] and 
[Pd₂(μ-C₆H₄S)(μ-dppm)₂Cl₂]
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              121
_journal_page_last               126
_journal_paper_doi               10.1021/om010538t
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C28 H44 S2 Sn2'
_chemical_formula_structural     '[Sn (C6 H4 S)2 (C4 H9)2]2'
_chemical_formula_sum            'C28 H44 S2 Sn2'
_chemical_formula_weight         682.13
_chemical_name_systematic
;
Ditertbuthyl-bis(mu!2$-bis(1-benzenethiolate)tin(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.902(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5408(9)
_cell_length_b                   14.7314(12)
_cell_length_c                   19.6027(16)
_cell_measurement_reflns_used    4830
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.25
_cell_measurement_theta_min      4.47
_cell_volume                     3040.0(4)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SHELXTL'
_computing_molecular_graphics    'XP, SHEXTL v. 4.2 (Siemens)'
_computing_publication_material  'CIBTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  '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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19828
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         57.38
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         7211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0391
_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)+(0.0243P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                5374
_reflns_number_total             7211
_reflns_threshold_expression     >2sigma(I)
_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 3105 2015-03-04 15:46:00Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4060773
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 1.09206(2) 0.670037(17) 0.301153(13) 0.03341(8) Uani 1 d . . .
Sn2 Sn 0.78483(2) 0.588378(16) 0.150508(12) 0.02860(7) Uani 1 d . . .
S1 S 1.11331(9) 0.58367(6) 0.19686(5) 0.0364(2) Uani 1 d . . .
S2 S 0.87315(10) 0.72064(7) 0.29617(5) 0.0425(3) Uani 1 d . . .
C1 C 1.0615(3) 0.6670(2) 0.13508(17) 0.0309(8) Uani 1 d . . .
C2 C 0.9328(3) 0.6766(2) 0.11556(17) 0.0313(8) Uani 1 d . . .
C3 C 0.9018(4) 0.7415(2) 0.06573(18) 0.0378(9) Uani 1 d . . .
H3 H 0.8169 0.7503 0.0522 0.045 Uiso 1 calc R . .
C4 C 0.9926(4) 0.7928(3) 0.0359(2) 0.0467(11) Uani 1 d . . .
H4 H 0.9688 0.8350 0.0023 0.056 Uiso 1 calc R . .
C5 C 1.1185(4) 0.7818(3) 0.0556(2) 0.0466(11) Uani 1 d . . .
H5 H 1.1803 0.8168 0.0358 0.056 Uiso 1 calc R . .
C6 C 1.1524(4) 0.7185(3) 0.10475(19) 0.0404(9) Uani 1 d . . .
H6 H 1.2377 0.7102 0.1177 0.048 Uiso 1 calc R . .
C7 C 0.7952(4) 0.6152(3) 0.30957(19) 0.0380(9) Uani 1 d . . .
C8 C 0.7752(3) 0.5527(2) 0.25707(17) 0.0324(8) Uani 1 d . . .
C9 C 0.7193(4) 0.4710(3) 0.2731(2) 0.0429(10) Uani 1 d . . .
H9 H 0.7100 0.4268 0.2393 0.051 Uiso 1 calc R . .
C10 C 0.6768(4) 0.4525(3) 0.3367(2) 0.0588(13) Uani 1 d . . .
H10 H 0.6388 0.3971 0.3456 0.071 Uiso 1 calc R . .
C11 C 0.6916(4) 0.5174(4) 0.3869(2) 0.0677(15) Uani 1 d . . .
H11 H 0.6609 0.5067 0.4298 0.081 Uiso 1 calc R . .
C12 C 0.7509(4) 0.5973(3) 0.3741(2) 0.0572(12) Uani 1 d . . .
H12 H 0.7620 0.6403 0.4086 0.069 Uiso 1 calc R . .
C13 C 1.1957(4) 0.7980(2) 0.30405(19) 0.0383(9) Uani 1 d . . .
C14 C 1.1250(4) 0.8667(3) 0.2585(2) 0.0510(11) Uani 1 d . . .
H14A H 1.1677 0.9242 0.2619 0.077 Uiso 1 calc R . .
H14B H 1.0398 0.8732 0.2728 0.077 Uiso 1 calc R . .
H14C H 1.1230 0.8460 0.2120 0.077 Uiso 1 calc R . .
C15 C 1.3290(4) 0.7845(3) 0.2797(2) 0.0568(12) Uani 1 d . . .
H15A H 1.3749 0.8408 0.2834 0.085 Uiso 1 calc R . .
H15B H 1.3241 0.7652 0.2328 0.085 Uiso 1 calc R . .
H15C H 1.3723 0.7392 0.3073 0.085 Uiso 1 calc R . .
C16 C 1.2028(5) 0.8329(3) 0.3771(2) 0.0575(12) Uani 1 d . . .
H16A H 1.2495 0.7906 0.4059 0.086 Uiso 1 calc R . .
H16B H 1.1185 0.8396 0.3927 0.086 Uiso 1 calc R . .
H16C H 1.2450 0.8907 0.3787 0.086 Uiso 1 calc R . .
C17 C 1.1403(4) 0.5706(3) 0.3808(2) 0.0472(11) Uani 1 d . . .
C18 C 1.0773(5) 0.4798(3) 0.3633(2) 0.0601(13) Uani 1 d . . .
H18A H 1.0997 0.4611 0.3185 0.090 Uiso 1 calc R . .
H18B H 0.9867 0.4861 0.3640 0.090 Uiso 1 calc R . .
H18C H 1.1057 0.4350 0.3962 0.090 Uiso 1 calc R . .
C19 C 1.2845(5) 0.5598(3) 0.3838(2) 0.0689(15) Uani 1 d . . .
H19A H 1.3092 0.5144 0.4170 0.103 Uiso 1 calc R . .
H19B H 1.3237 0.6166 0.3966 0.103 Uiso 1 calc R . .
H19C H 1.3114 0.5418 0.3398 0.103 Uiso 1 calc R . .
C20 C 1.0956(5) 0.6046(3) 0.4497(2) 0.0696(15) Uani 1 d . . .
H20A H 1.1187 0.5613 0.4847 0.104 Uiso 1 calc R . .
H20B H 1.0050 0.6121 0.4468 0.104 Uiso 1 calc R . .
H20C H 1.1352 0.6619 0.4606 0.104 Uiso 1 calc R . .
C21 C 0.5990(3) 0.6549(2) 0.1342(2) 0.0370(9) Uani 1 d . . .
C22 C 0.5020(4) 0.5993(3) 0.1714(2) 0.0544(12) Uani 1 d . . .
H22A H 0.4207 0.6286 0.1671 0.082 Uiso 1 calc R . .
H22B H 0.5286 0.5944 0.2188 0.082 Uiso 1 calc R . .
H22C H 0.4957 0.5397 0.1516 0.082 Uiso 1 calc R . .
C23 C 0.6044(4) 0.7503(3) 0.1648(2) 0.0570(12) Uani 1 d . . .
H23A H 0.5212 0.7769 0.1615 0.085 Uiso 1 calc R . .
H23B H 0.6620 0.7870 0.1403 0.085 Uiso 1 calc R . .
H23C H 0.6336 0.7468 0.2120 0.085 Uiso 1 calc R . .
C24 C 0.5563(4) 0.6615(3) 0.0589(2) 0.0576(13) Uani 1 d . . .
H24A H 0.5450 0.6015 0.0403 0.086 Uiso 1 calc R . .
H24B H 0.6197 0.6930 0.0345 0.086 Uiso 1 calc R . .
H24C H 0.4775 0.6940 0.0543 0.086 Uiso 1 calc R . .
C25 C 0.7961(4) 0.4670(2) 0.08584(19) 0.0390(9) Uani 1 d . . .
C26 C 0.9038(4) 0.4065(3) 0.1121(2) 0.0645(14) Uani 1 d . . .
H26A H 0.9100 0.3549 0.0825 0.097 Uiso 1 calc R . .
H26B H 0.8878 0.3862 0.1574 0.097 Uiso 1 calc R . .
H26C H 0.9821 0.4399 0.1131 0.097 Uiso 1 calc R . .
C27 C 0.6724(4) 0.4137(3) 0.0820(2) 0.0541(12) Uani 1 d . . .
H27A H 0.6056 0.4512 0.0622 0.081 Uiso 1 calc R . .
H27B H 0.6515 0.3957 0.1271 0.081 Uiso 1 calc R . .
H27C H 0.6819 0.3608 0.0541 0.081 Uiso 1 calc R . .
C28 C 0.8226(5) 0.5013(3) 0.0141(2) 0.0647(14) Uani 1 d . . .
H28A H 0.8991 0.5368 0.0162 0.097 Uiso 1 calc R . .
H28B H 0.7528 0.5381 -0.0029 0.097 Uiso 1 calc R . .
H28C H 0.8325 0.4505 -0.0158 0.097 Uiso 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'
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
C13 Sn1 C17 117.63(14) . . ?
C13 Sn1 S2 102.15(11) . . ?
C17 Sn1 S2 114.98(13) . . ?
C13 Sn1 S1 114.07(11) . . ?
C17 Sn1 S1 102.88(11) . . ?
S2 Sn1 S1 104.81(3) . . ?
C8 Sn2 C2 121.40(13) . . ?
C8 Sn2 C25 111.47(14) . . ?
C2 Sn2 C25 104.17(14) . . ?
C8 Sn2 C21 99.44(14) . . ?
C2 Sn2 C21 109.66(13) . . ?
C25 Sn2 C21 110.64(14) . . ?
C1 S1 Sn1 99.92(11) . . ?
C7 S2 Sn1 99.85(13) . . ?
C6 C1 C2 120.8(3) . . ?
C6 C1 S1 118.2(3) . . ?
C2 C1 S1 120.9(3) . . ?
C3 C2 C1 116.8(3) . . ?
C3 C2 Sn2 119.1(3) . . ?
C1 C2 Sn2 123.8(3) . . ?
C4 C3 C2 122.2(4) . . ?
C5 C4 C3 120.0(4) . . ?
C4 C5 C6 119.3(4) . . ?
C5 C6 C1 120.9(4) . . ?
C8 C7 C12 120.1(4) . . ?
C8 C7 S2 121.5(3) . . ?
C12 C7 S2 118.4(3) . . ?
C9 C8 C7 117.3(3) . . ?
C9 C8 Sn2 118.2(3) . . ?
C7 C8 Sn2 122.9(3) . . ?
C10 C9 C8 122.7(4) . . ?
C9 C10 C11 118.8(4) . . ?
C12 C11 C10 120.3(4) . . ?
C11 C12 C7 120.5(4) . . ?
C16 C13 C15 109.8(3) . . ?
C16 C13 C14 109.1(3) . . ?
C15 C13 C14 109.6(4) . . ?
C16 C13 Sn1 108.6(3) . . ?
C15 C13 Sn1 110.5(3) . . ?
C14 C13 Sn1 109.3(2) . . ?
C18 C17 C19 109.8(4) . . ?
C18 C17 C20 109.6(4) . . ?
C19 C17 C20 110.4(3) . . ?
C18 C17 Sn1 110.1(3) . . ?
C19 C17 Sn1 107.0(3) . . ?
C20 C17 Sn1 109.8(3) . . ?
C24 C21 C22 109.0(3) . . ?
C24 C21 C23 109.0(3) . . ?
C22 C21 C23 108.6(3) . . ?
C24 C21 Sn2 112.7(3) . . ?
C22 C21 Sn2 107.7(2) . . ?
C23 C21 Sn2 109.7(2) . . ?
C26 C25 C27 109.9(3) . . ?
C26 C25 C28 109.8(4) . . ?
C27 C25 C28 108.7(3) . . ?
C26 C25 Sn2 110.2(2) . . ?
C27 C25 Sn2 112.1(3) . . ?
C28 C25 Sn2 106.1(2) . . ?
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 C13 2.178(4) . ?
Sn1 C17 2.182(4) . ?
Sn1 S2 2.4221(11) . ?
Sn1 S1 2.4279(10) . ?
Sn2 C8 2.161(3) . ?
Sn2 C2 2.168(4) . ?
Sn2 C25 2.199(4) . ?
Sn2 C21 2.199(3) . ?
S1 C1 1.790(4) . ?
S2 C7 1.783(4) . ?
C1 C6 1.380(5) . ?
C1 C2 1.398(5) . ?
C2 C3 1.393(5) . ?
C3 C4 1.373(5) . ?
C4 C5 1.373(5) . ?
C5 C6 1.376(5) . ?
C7 C8 1.388(5) . ?
C7 C12 1.396(5) . ?
C8 C9 1.383(5) . ?
C9 C10 1.373(5) . ?
C10 C11 1.376(6) . ?
C11 C12 1.362(6) . ?
C13 C16 1.519(5) . ?
C13 C15 1.520(6) . ?
C13 C14 1.520(5) . ?
C17 C18 1.526(5) . ?
C17 C19 1.527(6) . ?
C17 C20 1.536(6) . ?
C21 C24 1.524(5) . ?
C21 C22 1.525(5) . ?
C21 C23 1.528(5) . ?
C25 C26 1.513(5) . ?
C25 C27 1.521(5) . ?
C25 C28 1.533(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30659596
