#------------------------------------------------------------------------------
#$Date: 2018-08-18 21:37:21 +0300 (Sat, 18 Aug 2018) $
#$Revision: 209913 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/07/49/4074939.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_4074939
loop_
_publ_author_name
'Nilsson, Patrik'
'Puxty, Graeme'
'Wendt, Ola F.'
_publ_section_title
;
 Reaction Mechanism of Transmetalation between Tetraorganostannanes and
 Platinum(II) Aryltriflate Complexes. Mechanistic Model for Stille
 Couplings
;
_journal_coden_ASTM              ORGND7
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1285
_journal_page_last               1292
_journal_paper_doi               10.1021/om051021a
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C46 H58 F6 O8 P4 Pt2 S2'
_chemical_formula_weight         1431.10
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 110.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.078(5)
_cell_length_b                   13.604(3)
_cell_length_c                   18.511(4)
_cell_measurement_reflns_used    4928
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      2.25
_cell_volume                     5930(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond (Brandenburg)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1277
_diffrn_reflns_av_sigmaI/netI    0.1386
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28702
_diffrn_reflns_theta_full        32.01
_diffrn_reflns_theta_max         32.01
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    4.954
_exptl_absorpt_correction_T_max  0.41218
_exptl_absorpt_correction_T_min  0.21269
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'absorption corrections using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.691
_refine_diff_density_min         -1.657
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         8972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1670
_refine_ls_R_factor_gt           0.0589
_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)+(0.0490P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                3974
_reflns_number_total             8972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om051021asi20060106_105841.cif
_cod_data_source_block           compound6
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4074939
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pt1 Pt 0.5000 0.83393(3) 0.7500 0.05021(15) Uani 1 2 d S
Pt2 Pt 0.5000 0.59409(3) 0.7500 0.05558(16) Uani 1 2 d S
P1 P 0.48285(12) 0.48128(16) 0.65520(14) 0.0697(7) Uani 1 1 d .
P2 P 0.46379(10) 0.94706(14) 0.65646(13) 0.0589(6) Uani 1 1 d .
S1 S 0.59276(12) 0.7870(2) 0.57020(16) 0.0845(7) Uani 1 1 d .
F1 F 0.6883(5) 0.7823(9) 0.5449(8) 0.230(6) Uani 1 1 d .
F2 F 0.6982(5) 0.7751(11) 0.6605(8) 0.244(7) Uani 1 1 d .
F3 F 0.6673(4) 0.6521(7) 0.5872(8) 0.209(5) Uani 1 1 d .
O1 O 0.5754(6) 0.7433(10) 0.6249(8) 0.220(7) Uani 1 1 d .
O2 O 0.5677(5) 0.7657(10) 0.4943(6) 0.192(5) Uani 1 1 d .
O3 O 0.5982(5) 0.8925(6) 0.5815(7) 0.189(5) Uani 1 1 d .
O4 O 0.4786(3) 0.7137(3) 0.6722(3) 0.078(2) Uani 1 1 d .
H4 H 0.4687(17) 0.7137(3) 0.636(6) 0.093 Uiso 1 1 calc R
C1 C 0.4520(5) 0.5378(8) 0.5587(5) 0.105(4) Uani 1 1 d .
H1A H 0.4766 0.5891 0.5532 0.158 Uiso 1 1 calc R
H1B H 0.4154 0.5648 0.5528 0.158 Uiso 1 1 calc R
H1C H 0.4480 0.4886 0.5199 0.158 Uiso 1 1 calc R
C2 C 0.4307(5) 0.3867(7) 0.6533(6) 0.095(3) Uani 1 1 d .
H2A H 0.3965 0.4174 0.6546 0.143 Uiso 1 1 calc R
H2B H 0.4458 0.3446 0.6973 0.143 Uiso 1 1 calc R
H2C H 0.4223 0.3486 0.6071 0.143 Uiso 1 1 calc R
C3 C 0.5086(4) 1.0453(6) 0.6428(5) 0.080(3) Uani 1 1 d .
H3A H 0.5418 1.0176 0.6360 0.120 Uiso 1 1 calc R
H3B H 0.5198 1.0874 0.6871 0.120 Uiso 1 1 calc R
H3C H 0.4878 1.0828 0.5980 0.120 Uiso 1 1 calc R
C4 C 0.4366(5) 0.8911(7) 0.5595(5) 0.087(3) Uani 1 1 d .
H4A H 0.4116 0.8376 0.5596 0.131 Uiso 1 1 calc R
H4B H 0.4678 0.8671 0.5458 0.131 Uiso 1 1 calc R
H4C H 0.4161 0.9397 0.5227 0.131 Uiso 1 1 calc R
C5 C 0.6647(8) 0.7502(12) 0.5935(9) 0.135(5) Uani 1 1 d .
C11 C 0.5478(4) 0.4198(6) 0.6531(5) 0.070(2) Uani 1 1 d .
C12 C 0.5969(5) 0.4729(8) 0.6697(7) 0.112(4) Uani 1 1 d .
H12 H 0.5970 0.5392 0.6821 0.134 Uiso 1 1 calc R
C13 C 0.6482(6) 0.4281(10) 0.6681(9) 0.143(6) Uani 1 1 d .
H13 H 0.6813 0.4648 0.6793 0.172 Uiso 1 1 calc R
C14 C 0.6477(8) 0.3271(11) 0.6494(9) 0.133(5) Uani 1 1 d .
H14 H 0.6808 0.2963 0.6492 0.160 Uiso 1 1 calc R
C15 C 0.6002(7) 0.2774(9) 0.6324(9) 0.120(5) Uani 1 1 d .
H15 H 0.6000 0.2114 0.6194 0.144 Uiso 1 1 calc R
C16 C 0.5508(5) 0.3199(7) 0.6333(6) 0.094(3) Uani 1 1 d .
H16 H 0.5181 0.2818 0.6204 0.113 Uiso 1 1 calc R
C21 C 0.4004(3) 1.0047(6) 0.6692(5) 0.064(2) Uani 1 1 d .
C22 C 0.3717(4) 0.9562(7) 0.7102(6) 0.083(3) Uani 1 1 d .
H22 H 0.3843 0.8945 0.7306 0.100 Uiso 1 1 calc R
C23 C 0.3244(4) 0.9966(10) 0.7220(7) 0.117(4) Uani 1 1 d .
H23 H 0.3048 0.9619 0.7484 0.140 Uiso 1 1 calc R
C24 C 0.3074(6) 1.0895(11) 0.6936(9) 0.138(6) Uani 1 1 d .
H24 H 0.2767 1.1186 0.7028 0.166 Uiso 1 1 calc R
C25 C 0.3348(6) 1.1406(10) 0.6516(8) 0.127(5) Uani 1 1 d .
H25 H 0.3217 1.2022 0.6316 0.153 Uiso 1 1 calc R
C26 C 0.3827(5) 1.0990(7) 0.6395(7) 0.098(4) Uani 1 1 d .
H26 H 0.4020 1.1331 0.6125 0.118 Uiso 1 1 calc R
C31 C 0.2833(17) 0.606(3) 0.5209(13) 0.38(3) Uani 1 1 d G
H31 H 0.2853 0.6091 0.4717 0.453 Uiso 1 1 calc R
C32 C 0.3144(10) 0.659(2) 0.573(3) 0.54(5) Uani 1 1 d G
H32 H 0.3398 0.7022 0.5622 0.646 Uiso 1 1 calc R
C33 C 0.3118(14) 0.6557(19) 0.6381(17) 0.30(2) Uani 1 1 d G
H33 H 0.3352 0.6956 0.6769 0.362 Uiso 1 1 calc R
C34 C 0.2780(19) 0.599(3) 0.6520(15) 0.40(3) Uani 1 1 d G
H34 H 0.2760 0.5959 0.7012 0.482 Uiso 1 1 calc R
C35 C 0.2468(12) 0.5456(19) 0.600(3) 0.33(2) Uani 1 1 d G
H35 H 0.2214 0.5028 0.6107 0.395 Uiso 1 1 calc R
C36 C 0.2495(12) 0.5493(18) 0.535(2) 0.249(14) Uani 1 1 d G
H36 H 0.2261 0.5094 0.4959 0.299 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'
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'
P P 0.1023 0.0942 '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'
Pt Pt -1.7033 8.3905 '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
O4 Pt1 O4 79.2(3) . 2_656
O4 Pt1 P2 170.26(17) . 2_656
O4 Pt1 P2 93.64(16) 2_656 2_656
O4 Pt1 P2 93.64(16) . .
O4 Pt1 P2 170.26(17) 2_656 .
P2 Pt1 P2 94.18(12) 2_656 .
O4 Pt2 O4 79.5(3) 2_656 .
O4 Pt2 P1 170.83(16) 2_656 .
O4 Pt2 P1 93.32(16) . .
O4 Pt2 P1 93.32(16) 2_656 2_656
O4 Pt2 P1 170.83(16) . 2_656
P1 Pt2 P1 94.38(12) . 2_656
C2 P1 C11 108.2(5) . .
C2 P1 C1 102.4(5) . .
C11 P1 C1 104.3(5) . .
C2 P1 Pt2 115.9(3) . .
C11 P1 Pt2 113.0(3) . .
C1 P1 Pt2 111.9(3) . .
C3 P2 C4 101.9(4) . .
C3 P2 C21 107.7(4) . .
C4 P2 C21 104.5(4) . .
C3 P2 Pt1 120.2(3) . .
C4 P2 Pt1 112.3(3) . .
C21 P2 Pt1 109.0(3) . .
O2 S1 O1 121.4(10) . .
O2 S1 O3 110.3(8) . .
O1 S1 O3 111.2(8) . .
O2 S1 C5 105.1(8) . .
O1 S1 C5 104.6(7) . .
O3 S1 C5 101.9(8) . .
Pt2 O4 Pt1 100.7(2) . .
Pt2 O4 H4 129.7 . .
Pt1 O4 H4 129.7 . .
P1 C1 H1A 109.5 . .
P1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
P1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
P1 C2 H2A 109.5 . .
P1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
P1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
P2 C3 H3A 109.5 . .
P2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
P2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
P2 C4 H4A 109.5 . .
P2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
P2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
F2 C5 F1 106.0(18) . .
F2 C5 F3 108.2(12) . .
F1 C5 F3 103.0(14) . .
F2 C5 S1 115.7(13) . .
F1 C5 S1 113.6(10) . .
F3 C5 S1 109.5(13) . .
C12 C11 C16 116.2(9) . .
C12 C11 P1 119.3(7) . .
C16 C11 P1 124.5(8) . .
C11 C12 C13 121.1(10) . .
C11 C12 H12 119.5 . .
C13 C12 H12 119.5 . .
C14 C13 C12 119.1(13) . .
C14 C13 H13 120.5 . .
C12 C13 H13 120.5 . .
C15 C14 C13 119.3(14) . .
C15 C14 H14 120.4 . .
C13 C14 H14 120.4 . .
C14 C15 C16 122.1(12) . .
C14 C15 H15 119.0 . .
C16 C15 H15 119.0 . .
C15 C16 C11 122.3(11) . .
C15 C16 H16 118.8 . .
C11 C16 H16 118.8 . .
C22 C21 C26 119.8(8) . .
C22 C21 P2 119.9(6) . .
C26 C21 P2 120.3(7) . .
C21 C22 C23 122.1(9) . .
C21 C22 H22 118.9 . .
C23 C22 H22 118.9 . .
C24 C23 C22 118.1(11) . .
C24 C23 H23 120.9 . .
C22 C23 H23 120.9 . .
C23 C24 C25 121.6(11) . .
C23 C24 H24 119.2 . .
C25 C24 H24 119.2 . .
C24 C25 C26 120.0(11) . .
C24 C25 H25 120.0 . .
C26 C25 H25 120.0 . .
C21 C26 C25 118.3(10) . .
C21 C26 H26 120.8 . .
C25 C26 H26 120.8 . .
C32 C31 C36 120.0 . .
C32 C31 H31 120.0 . .
C36 C31 H31 120.0 . .
C31 C32 C33 120.0 . .
C31 C32 H32 120.0 . .
C33 C32 H32 120.0 . .
C34 C33 C32 120.0 . .
C34 C33 H33 120.0 . .
C32 C33 H33 120.0 . .
C33 C34 C35 120.0 . .
C33 C34 H34 120.0 . .
C35 C34 H34 120.0 . .
C34 C35 C36 120.0 . .
C34 C35 H35 120.0 . .
C36 C35 H35 120.0 . .
C35 C36 C31 120.0 . .
C35 C36 H36 120.0 . .
C31 C36 H36 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 O4 2.122(5) .
Pt1 O4 2.122(5) 2_656
Pt1 P2 2.260(2) 2_656
Pt1 P2 2.260(2) .
Pt2 O4 2.117(5) 2_656
Pt2 O4 2.117(5) .
Pt2 P1 2.258(2) .
Pt2 P1 2.258(2) 2_656
P1 C2 1.826(10) .
P1 C11 1.843(9) .
P1 C1 1.852(10) .
P2 C3 1.819(9) .
P2 C4 1.851(9) .
P2 C21 1.859(8) .
S1 O2 1.358(9) .
S1 O1 1.368(9) .
S1 O3 1.450(9) .
S1 C5 1.777(17) .
F1 C5 1.310(16) .
F2 C5 1.282(18) .
F3 C5 1.343(18) .
O4 H4 0.6238 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C11 C12 1.369(13) .
C11 C16 1.415(11) .
C12 C13 1.432(15) .
C12 H12 0.9300 .
C13 C14 1.417(17) .
C13 H13 0.9300 .
C14 C15 1.310(18) .
C14 H14 0.9300 .
C15 C16 1.374(16) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C21 C22 1.382(11) .
C21 C26 1.406(11) .
C22 C23 1.391(13) .
C22 H22 0.9300 .
C23 C24 1.379(16) .
C23 H23 0.9300 .
C24 C25 1.390(17) .
C24 H24 0.9300 .
C25 C26 1.413(14) .
C25 H25 0.9300 .
C26 H26 0.9300 .
C31 C32 1.239(10) .
C31 C36 1.239(10) .
C31 H31 0.9300 .
C32 C33 1.239(10) .
C32 H32 0.9300 .
C33 C34 1.239(10) .
C33 H33 0.9300 .
C34 C35 1.239(10) .
C34 H34 0.9300 .
C35 C36 1.239(10) .
C35 H35 0.9300 .
C36 H36 0.9300 .
