#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:44:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178791 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/45/4104599.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_4104599
loop_
_publ_author_name
'Nandita M. Weliange'
'Endre Szuromi'
'Paul R. Sharp'
_publ_section_title
;
 Proton-Catalyzed Oxo-Alkene Coupling: 2-Platinaoxetane Formation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8736
_journal_page_last               8737
_journal_paper_doi               10.1021/ja902180k
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C36 H52 F12 O16 Pt4 S4'
_chemical_formula_weight         1877.38
_chemical_name_systematic
; 
 ? 
;
_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                 133.29
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.560(3)
_cell_length_b                   10.5832(10)
_cell_length_c                   21.554(2)
_cell_measurement_reflns_used    6390
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.60
_cell_volume                     4908.1(8)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
   L. J. Barbour, X-Seed - Graphical Interface to
   SHELX-97 and POV-Ray, 1999
   ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997)
;
_computing_structure_refinement
;
   SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to
   SHELX-97 and POV-Ray, 1999
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16923
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    11.648
_exptl_absorpt_correction_T_max  0.3888
_exptl_absorpt_correction_T_min  0.2740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
   Data were corrected for decay and absorption using the program SADABS
   based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.541
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.746
_refine_diff_density_min         -3.474
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5412
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0489P)²+463.1043P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                4180
_reflns_number_total             5412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902180k_si_002.cif
_cod_data_source_block           '[Pt(COD)(m-OH)]4(OTf)4_(5-OTf,n=4)'
_cod_original_cell_volume        4907.9(8)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4104599
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.57827(3) 0.46696(6) 0.37518(4) 0.03313(18) Uani 1 1 d . . .
Pt2 Pt 0.55432(3) 0.26212(5) 0.22165(4) 0.02473(16) Uani 1 1 d . . .
O1 O 0.5732(6) 0.2916(10) 0.3308(7) 0.042(3) Uani 1 1 d . . .
H1O H 0.6138 0.2505 0.3769 0.050 Uiso 1 1 d R . .
O2 O 0.5120(7) 0.4365(12) 0.1862(9) 0.052(4) Uani 1 1 d . . .
H2O H 0.5174 0.4746 0.1496 0.063 Uiso 1 1 d R . .
C2 C 0.6802(8) 0.4660(15) 0.4705(12) 0.037(4) Uani 1 1 d . . .
H2 H 0.6987 0.3818 0.4778 0.045 Uiso 1 1 calc R . .
C10 C 0.5754(9) 0.0652(14) 0.2517(13) 0.041(4) Uani 1 1 d . . .
H10 H 0.5810 0.0365 0.3008 0.049 Uiso 1 1 calc R . .
C1 C 0.6561(9) 0.5327(16) 0.3943(13) 0.044(4) Uani 1 1 d . . .
H1 H 0.6621 0.4884 0.3593 0.053 Uiso 1 1 calc R . .
C14 C 0.5552(8) 0.2744(16) 0.1235(11) 0.037(4) Uani 1 1 d . . .
H14 H 0.5418 0.3580 0.0939 0.044 Uiso 1 1 calc R . .
C13 C 0.5063(10) 0.195(2) 0.0957(11) 0.054(5) Uani 1 1 d . . .
H13 H 0.4642 0.2332 0.0504 0.064 Uiso 1 1 calc R . .
C9 C 0.6271(9) 0.1275(18) 0.2747(14) 0.048(5) Uani 1 1 d . . .
H9 H 0.6632 0.1359 0.3376 0.058 Uiso 1 1 calc R . .
C3 C 0.7034(10) 0.5199(19) 0.5475(13) 0.053(5) Uani 1 1 d . . .
H3A H 0.7449 0.5562 0.5773 0.064 Uiso 1 1 calc R . .
H3B H 0.7097 0.4510 0.5837 0.064 Uiso 1 1 calc R . .
C6 C 0.5674(11) 0.6661(18) 0.3855(16) 0.059(6) Uani 1 1 d . . .
H6 H 0.5233 0.6914 0.3522 0.070 Uiso 1 1 calc R . .
C15 C 0.6179(10) 0.229(2) 0.1590(15) 0.058(6) Uani 1 1 d . . .
H15A H 0.6475 0.3006 0.1874 0.070 Uiso 1 1 calc R . .
H15B H 0.6134 0.2005 0.1113 0.070 Uiso 1 1 calc R . .
C8 C 0.6569(10) 0.6762(17) 0.3914(16) 0.055(5) Uani 1 1 d . . .
H8A H 0.6634 0.7020 0.3538 0.066 Uiso 1 1 calc R . .
H8B H 0.6924 0.7084 0.4494 0.066 Uiso 1 1 calc R . .
C5 C 0.5952(10) 0.607(2) 0.4614(14) 0.056(6) Uani 1 1 d . . .
H5 H 0.5681 0.5992 0.4733 0.068 Uiso 1 1 calc R . .
C7 C 0.5971(12) 0.7367(18) 0.359(2) 0.078(8) Uani 1 1 d . . .
H7A H 0.6063 0.8243 0.3810 0.093 Uiso 1 1 calc R . .
H7B H 0.5667 0.7410 0.2962 0.093 Uiso 1 1 calc R . .
C12 C 0.5064(13) 0.052(2) 0.0913(16) 0.082(9) Uani 1 1 d . . .
H12A H 0.4639 0.0221 0.0417 0.099 Uiso 1 1 calc R . .
H12B H 0.5340 0.0256 0.0830 0.099 Uiso 1 1 calc R . .
C4 C 0.6651(11) 0.620(2) 0.5418(16) 0.075(8) Uani 1 1 d . . .
H4A H 0.6797 0.7042 0.5413 0.090 Uiso 1 1 calc R . .
H4B H 0.6711 0.6158 0.5929 0.090 Uiso 1 1 calc R . .
C16 C 0.6448(12) 0.120(2) 0.2233(16) 0.071(7) Uiso 1 1 d . . .
H16A H 0.6298 0.0389 0.1920 0.086 Uiso 1 1 calc R . .
H16B H 0.6906 0.1213 0.2628 0.086 Uiso 1 1 calc R . .
C11 C 0.5280(14) -0.008(2) 0.1708(18) 0.087(10) Uani 1 1 d . . .
H11A H 0.5458 -0.0920 0.1775 0.105 Uiso 1 1 calc R . .
H11B H 0.4914 -0.0224 0.1632 0.105 Uiso 1 1 calc R . .
S1 S 0.5810(3) 0.6531(7) 0.1248(4) 0.0814(19) Uiso 1 1 d G A 1
O3 O 0.5705(6) 0.6036(13) 0.1768(7) 0.093(6) Uiso 1 1 d G A 1
O4 O 0.5708(6) 0.5608(12) 0.0665(8) 0.104(6) Uiso 1 1 d G A 1
O5 O 0.5503(6) 0.7729(9) 0.0847(9) 0.199(15) Uiso 1 1 d G A 1
F1 F 0.6775(7) 0.734(2) 0.1575(14) 0.51(5) Uiso 1 1 d G A 1
F2 F 0.6773(7) 0.7720(19) 0.2551(9) 0.182(11) Uiso 1 1 d G A 1
F3 F 0.6954(4) 0.584(2) 0.2390(11) 0.48(4) Uiso 1 1 d G A 1
C1T C 0.6621(3) 0.6877(16) 0.1980(8) 0.22(3) Uiso 1 1 d G A 1
S2 S 0.6951(4) 0.0903(7) 0.5211(5) 0.033(2) Uani 0.516(12) 1 d PG B 1
O6 O 0.6985(7) 0.0060(12) 0.4714(8) 0.043(6) Uani 0.516(12) 1 d PG B 1
O7 O 0.7491(5) 0.1713(12) 0.5782(9) 0.064(9) Uani 0.516(12) 1 d PG B 1
O8 O 0.6366(5) 0.1577(12) 0.4705(8) 0.044(6) Uani 0.516(12) 1 d PG B 1
F4 F 0.6941(11) 0.0565(19) 0.6381(11) 0.16(3) Uani 0.516(12) 1 d PG B 1
F5 F 0.6493(9) -0.0898(13) 0.5436(15) 0.113(14) Uani 0.516(12) 1 d PG B 1
F6 F 0.7488(9) -0.0778(16) 0.6389(10) 0.125(15) Uani 0.516(12) 1 d PG B 1
C2T C 0.6969(8) -0.0106(12) 0.5891(9) 0.077(17) Uani 0.516(12) 1 d PGU B 1
S2' S 0.6705(4) 0.0468(7) 0.4892(5) 0.036(3) Uani 0.484(12) 1 d PG B 2
O6' O 0.7102(6) -0.0634(9) 0.5220(8) 0.031(5) Uani 0.484(12) 1 d PG B 2
O7' O 0.6810(7) 0.1386(11) 0.4503(8) 0.035(6) Uani 0.484(12) 1 d PG B 2
O8' O 0.6054(4) 0.0162(15) 0.4371(9) 0.094(15) Uani 0.484(12) 1 d PG B 2
F4' F 0.6604(10) 0.2275(12) 0.5588(12) 0.086(11) Uani 0.484(12) 1 d PG B 2
F5' F 0.6863(11) 0.0488(16) 0.6223(11) 0.13(2) Uani 0.484(12) 1 d PG B 2
F6' F 0.7532(8) 0.1571(15) 0.6339(7) 0.093(12) Uani 0.484(12) 1 d PG B 2
C2T' C 0.6938(8) 0.1242(10) 0.5809(7) 0.11(3) Uani 0.484(12) 1 d PG B 2
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'
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
O2 Pt1 O1 84.8(5) 2_655
O2 Pt1 C5 95.5(6) 2_655
O1 Pt1 C5 158.2(7) .
O2 Pt1 C1 158.2(6) 2_655
O1 Pt1 C1 96.2(6) .
C5 Pt1 C1 91.5(7) .
O2 Pt1 C6 90.0(7) 2_655
O1 Pt1 C6 164.2(7) .
C5 Pt1 C6 37.2(8) .
C1 Pt1 C6 83.2(7) .
O2 Pt1 C2 162.9(6) 2_655
O1 Pt1 C2 92.7(6) .
C5 Pt1 C2 80.7(8) .
C1 Pt1 C2 38.9(7) .
C6 Pt1 C2 96.5(8) .
O1 Pt2 O2 84.7(5) .
O1 Pt2 C14 162.7(5) .
O2 Pt2 C14 89.7(6) .
O1 Pt2 C9 96.1(7) .
O2 Pt2 C9 157.7(6) .
C14 Pt2 C9 83.1(7) .
O1 Pt2 C10 90.4(6) .
O2 Pt2 C10 163.7(6) .
C14 Pt2 C10 99.2(7) .
C9 Pt2 C10 38.3(7) .
O1 Pt2 C13 158.8(6) .
O2 Pt2 C13 97.0(8) .
C14 Pt2 C13 38.3(6) .
C9 Pt2 C13 90.3(9) .
C10 Pt2 C13 82.1(8) .
Pt2 O1 Pt1 123.7(5) .
Pt1 O2 Pt2 125.1(7) 2_655
C3 C2 C1 127.0(16) .
C3 C2 Pt1 110.3(13) .
C1 C2 Pt1 69.1(10) .
C9 C10 C11 125.1(18) .
C9 C10 Pt2 70.8(9) .
C11 C10 Pt2 107.8(16) .
C2 C1 C8 121.6(18) .
C2 C1 Pt1 72.0(9) .
C8 C1 Pt1 111.0(12) .
C13 C14 C15 124.7(18) .
C13 C14 Pt2 71.2(10) .
C15 C14 Pt2 108.7(12) .
C14 C13 C12 125(2) .
C14 C13 Pt2 70.5(10) .
C12 C13 Pt2 112.5(15) .
C10 C9 C16 124(2) .
C10 C9 Pt2 70.9(9) .
C16 C9 Pt2 111.5(14) .
C2 C3 C4 117.4(19) .
C5 C6 C7 129(2) .
C5 C6 Pt1 70.8(12) .
C7 C6 Pt1 105.9(12) .
C14 C15 C16 113.0(16) .
C1 C8 C7 113.0(15) .
C6 C5 C4 122.9(19) .
C6 C5 Pt1 72.0(10) .
C4 C5 Pt1 111.8(14) .
C6 C7 C8 114.0(18) .
C11 C12 C13 111.7(16) .
C3 C4 C5 112.6(17) .
C9 C16 C15 113.3(19) .
C12 C11 C10 115.8(17) .
O4 S1 O5 113.5 .
O4 S1 O3 113.4 .
O5 S1 O3 113.4 .
O4 S1 C1T 105.1 .
O5 S1 C1T 105.1 .
O3 S1 C1T 105.1 .
F2 C1T F1 108.2 .
F2 C1T F3 108.2 .
F1 C1T F3 108.2 .
F2 C1T S1 110.7 .
F1 C1T S1 110.7 .
F3 C1T S1 110.7 .
O6 S2 O8 113.5 .
O6 S2 O7 113.5 .
O8 S2 O7 113.4 .
O6 S2 C2T 105.1 .
O8 S2 C2T 105.1 .
O7 S2 C2T 105.1 .
F4 C2T F5 108.3 .
F4 C2T F6 108.2 .
F5 C2T F6 108.2 .
F4 C2T S2 110.7 .
F5 C2T S2 110.7 .
F6 C2T S2 110.7 .
O8' S2' O6' 113.5 .
O8' S2' O7' 113.5 .
O6' S2' O7' 113.4 .
O8' S2' C2T' 105.1 .
O6' S2' C2T' 105.1 .
O7' S2' C2T' 105.1 .
F4' C2T' F6' 108.2 .
F4' C2T' F5' 108.2 .
F6' C2T' F5' 108.2 .
F4' C2T' S2' 110.7 .
F6' C2T' S2' 110.7 .
F5' C2T' S2' 110.7 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 O2 2.034(13) 2_655
Pt1 O1 2.046(10) .
Pt1 C5 2.151(17) .
Pt1 C1 2.156(17) .
Pt1 C6 2.166(18) .
Pt1 C2 2.194(17) .
Pt2 O1 2.034(11) .
Pt2 O2 2.060(12) .
Pt2 C14 2.137(17) .
Pt2 C9 2.143(16) .
Pt2 C10 2.144(15) .
Pt2 C13 2.147(17) .
O2 Pt1 2.034(13) 2_655
C2 C3 1.41(3) .
C2 C1 1.45(2) .
C10 C9 1.41(2) .
C10 C11 1.50(3) .
C1 C8 1.52(2) .
C14 C13 1.40(2) .
C14 C15 1.52(3) .
C13 C12 1.51(3) .
C9 C16 1.52(3) .
C3 C4 1.50(3) .
C6 C5 1.38(3) .
C6 C7 1.53(3) .
C15 C16 1.54(3) .
C8 C7 1.53(3) .
C5 C4 1.54(3) .
C12 C11 1.50(4) .
S1 O4 1.4494 .
S1 O5 1.4504 .
S1 O3 1.4511 .
S1 C1T 1.7835 .
F1 C1T 1.3240 .
F2 C1T 1.3239 .
F3 C1T 1.3244 .
S2 O6 1.4494 .
S2 O8 1.4500 .
S2 O7 1.4500 .
S2 C2T 1.7841 .
F4 C2T 1.3233 .
F5 C2T 1.3235 .
F6 C2T 1.3248 .
S2' O8' 1.4498 .
S2' O6' 1.4498 .
S2' O7' 1.4500 .
S2' C2T' 1.7836 .
F4' C2T' 1.3241 .
F5' C2T' 1.3244 .
F6' C2T' 1.3243 .
