#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:37:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178818 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/72/4107290.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_4107290
loop_
_publ_author_name
'Anette Yahav-Levi'
'Israel Goldberg'
'Arkadi Vigalok'
'Andrei N. Vedernikov'
_publ_section_title
;
 Competitive Aryl-Iodide vs Aryl-Aryl Reductive Elimination Reactions in
 Pt(IV) Complexes: Experimental and Theoretical Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              724
_journal_page_last               731
_journal_paper_doi               10.1021/ja077258a
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C22 H24 F2 I2 P2 Pt, C H2 Cl2, 0.5(C6 H6)'
_chemical_formula_sum            'C26 H29 Cl2 F2 I2 P2 Pt'
_chemical_formula_weight         961.22
_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                97.5703(12)
_cell_angle_beta                 98.9282(12)
_cell_angle_gamma                92.0227(17)
_cell_formula_units_Z            2
_cell_length_a                   9.2719(3)
_cell_length_b                   12.7773(4)
_cell_length_c                   12.8114(4)
_cell_measurement_reflns_used    4908
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.12
_cell_volume                     1483.90(8)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF-96
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. φ ans 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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13895
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.124
_exptl_absorpt_correction_T_max  0.7171
_exptl_absorpt_correction_T_min  0.2690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.151
_exptl_crystal_description       plates
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.968
_refine_diff_density_min         -2.769
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0490
_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)+(0.0744P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                4680
_reflns_number_total             6907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077258asi20070919_042735.cif
_cod_data_source_block           ar29
_cod_database_code               4107290
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
Pt1 Pt 0.83189(3) 0.20266(2) 0.18340(2) 0.01837(11) Uani 1 1 d .
I2 I 1.12064(6) 0.18829(4) 0.19731(5) 0.02538(15) Uani 1 1 d .
I3 I 0.53833(5) 0.20378(4) 0.16001(4) 0.02129(14) Uani 1 1 d .
P4 P 0.8005(2) 0.19093(16) -0.00687(18) 0.0220(5) Uani 1 1 d .
P5 P 0.8352(2) 0.38629(16) 0.17338(18) 0.0210(5) Uani 1 1 d .
C6 C 0.7269(9) 0.3161(6) -0.0385(7) 0.0228(18) Uani 1 1 d .
C7 C 0.6627(9) 0.3301(7) -0.1415(7) 0.0278(19) Uani 1 1 d .
H7 H 0.6489 0.2710 -0.1961 0.033 Uiso 1 1 calc R
C8 C 0.6191(10) 0.4262(8) -0.1660(8) 0.034(2) Uani 1 1 d .
H8 H 0.5744 0.4330 -0.2366 0.041 Uiso 1 1 calc R
C9 C 0.6404(10) 0.5145(8) -0.0872(8) 0.032(2) Uani 1 1 d .
H9 H 0.6116 0.5819 -0.1036 0.039 Uiso 1 1 calc R
C10 C 0.7035(10) 0.5021(6) 0.0141(7) 0.0256(19) Uani 1 1 d .
H10 H 0.7189 0.5618 0.0680 0.031 Uiso 1 1 calc R
C11 C 0.7456(8) 0.4034(6) 0.0401(7) 0.0219(18) Uani 1 1 d .
C12 C 0.9635(10) 0.1883(8) -0.0716(8) 0.036(2) Uani 1 1 d .
H12A H 1.0130 0.1230 -0.0616 0.053 Uiso 1 1 calc R
H12B H 1.0300 0.2494 -0.0398 0.053 Uiso 1 1 calc R
H12C H 0.9346 0.1912 -0.1480 0.053 Uiso 1 1 calc R
C13 C 0.6844(10) 0.0875(7) -0.0943(7) 0.032(2) Uani 1 1 d .
H13A H 0.6741 0.1029 -0.1679 0.048 Uiso 1 1 calc R
H13B H 0.5878 0.0844 -0.0723 0.048 Uiso 1 1 calc R
H13C H 0.7285 0.0194 -0.0897 0.048 Uiso 1 1 calc R
C14 C 1.0093(10) 0.4600(7) 0.1861(7) 0.031(2) Uani 1 1 d .
H14A H 1.0622 0.4307 0.1294 0.046 Uiso 1 1 calc R
H14B H 1.0675 0.4549 0.2557 0.046 Uiso 1 1 calc R
H14C H 0.9924 0.5344 0.1800 0.046 Uiso 1 1 calc R
C15 C 0.7378(9) 0.4644(6) 0.2659(7) 0.0261(19) Uani 1 1 d .
H15A H 0.7850 0.4611 0.3393 0.039 Uiso 1 1 calc R
H15B H 0.6362 0.4363 0.2562 0.039 Uiso 1 1 calc R
H15C H 0.7397 0.5381 0.2522 0.039 Uiso 1 1 calc R
C16 C 0.8185(9) 0.0368(6) 0.2003(6) 0.0201(17) Uani 1 1 d .
C17 C 0.9051(9) 0.0033(7) 0.2867(7) 0.0262(19) Uani 1 1 d .
H17 H 0.9725 0.0519 0.3343 0.031 Uiso 1 1 calc R
C18 C 0.8926(10) -0.1035(7) 0.3036(7) 0.031(2) Uani 1 1 d .
H18 H 0.9486 -0.1280 0.3632 0.037 Uiso 1 1 calc R
C19 C 0.7948(10) -0.1715(6) 0.2293(8) 0.028(2) Uani 1 1 d .
C20 C 0.7095(10) -0.1387(7) 0.1460(8) 0.031(2) Uani 1 1 d .
H20 H 0.6420 -0.1869 0.0979 0.037 Uiso 1 1 calc R
C21 C 0.7225(9) -0.0325(6) 0.1319(7) 0.0243(18) Uani 1 1 d .
H21 H 0.6632 -0.0084 0.0735 0.029 Uiso 1 1 calc R
F22 F 0.7859(6) -0.2764(4) 0.2436(4) 0.0390(14) Uani 1 1 d .
C23 C 0.8527(9) 0.2367(6) 0.3509(7) 0.0237(18) Uani 1 1 d .
C24 C 0.7504(9) 0.1951(6) 0.4050(7) 0.0237(18) Uani 1 1 d .
H24 H 0.6732 0.1484 0.3655 0.028 Uiso 1 1 calc R
C25 C 0.7565(10) 0.2189(7) 0.5145(7) 0.029(2) Uani 1 1 d .
H25 H 0.6866 0.1880 0.5500 0.035 Uiso 1 1 calc R
C26 C 0.8677(11) 0.2894(7) 0.5706(7) 0.030(2) Uani 1 1 d .
C27 C 0.9732(10) 0.3316(7) 0.5228(8) 0.032(2) Uani 1 1 d .
H27 H 1.0511 0.3771 0.5632 0.038 Uiso 1 1 calc R
C28 C 0.9629(10) 0.3054(7) 0.4125(7) 0.028(2) Uani 1 1 d .
H28 H 1.0342 0.3359 0.3779 0.034 Uiso 1 1 calc R
F29 F 0.8725(6) 0.3132(4) 0.6779(4) 0.0416(14) Uani 1 1 d .
C30 C 0.4096(12) 0.3419(9) 0.4425(9) 0.052(3) Uani 1 1 d .
H30A H 0.5152 0.3478 0.4380 0.062 Uiso 1 1 calc R
H30B H 0.3646 0.2806 0.3908 0.062 Uiso 1 1 calc R
Cl31 Cl 0.3874(3) 0.3210(2) 0.5719(2) 0.0449(6) Uani 1 1 d .
Cl32 Cl 0.3283(3) 0.4574(3) 0.4092(3) 0.0734(11) Uani 1 1 d .
C33 C 0.4144(11) 0.0176(7) 0.4040(9) 0.038(2) Uani 1 1 d .
H33 H 0.3557 0.0290 0.3393 0.046 Uiso 1 1 calc R
C34 C 0.3719(13) 0.0521(8) 0.5023(9) 0.048(3) Uani 1 1 d .
H34 H 0.2847 0.0886 0.5048 0.058 Uiso 1 1 calc R
C35 C 0.4583(13) 0.0326(7) 0.5974(9) 0.044(3) Uani 1 1 d .
H35 H 0.4275 0.0549 0.6637 0.053 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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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'
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
C23 Pt1 C16 88.0(3) .
C23 Pt1 P5 89.2(2) .
C16 Pt1 P5 176.1(2) .
C23 Pt1 P4 171.5(2) .
C16 Pt1 P4 100.1(2) .
P5 Pt1 P4 82.56(7) .
C23 Pt1 I2 90.8(2) .
C16 Pt1 I2 87.4(2) .
P5 Pt1 I2 95.44(5) .
P4 Pt1 I2 91.86(5) .
C23 Pt1 I3 91.9(2) .
C16 Pt1 I3 89.6(2) .
P5 Pt1 I3 87.71(5) .
P4 Pt1 I3 85.90(5) .
I2 Pt1 I3 175.88(2) .
C13 P4 C6 106.0(4) .
C13 P4 C12 100.6(5) .
C6 P4 C12 101.3(4) .
C13 P4 Pt1 122.2(3) .
C6 P4 Pt1 105.7(3) .
C12 P4 Pt1 118.6(3) .
C14 P5 C15 103.9(4) .
C14 P5 C11 103.0(4) .
C15 P5 C11 106.0(4) .
C14 P5 Pt1 119.3(3) .
C15 P5 Pt1 115.7(3) .
C11 P5 Pt1 107.5(3) .
C11 C6 C7 118.0(8) .
C11 C6 P4 119.2(6) .
C7 C6 P4 122.5(7) .
C8 C7 C6 122.0(9) .
C8 C7 H7 119.0 .
C6 C7 H7 119.0 .
C7 C8 C9 119.9(9) .
C7 C8 H8 120.0 .
C9 C8 H8 120.0 .
C10 C9 C8 118.7(8) .
C10 C9 H9 120.6 .
C8 C9 H9 120.6 .
C9 C10 C11 121.6(8) .
C9 C10 H10 119.2 .
C11 C10 H10 119.2 .
C6 C11 C10 119.7(8) .
C6 C11 P5 118.1(6) .
C10 C11 P5 122.1(6) .
P4 C12 H12A 109.5 .
P4 C12 H12B 109.5 .
H12A C12 H12B 109.5 .
P4 C12 H12C 109.5 .
H12A C12 H12C 109.5 .
H12B C12 H12C 109.5 .
P4 C13 H13A 109.5 .
P4 C13 H13B 109.5 .
H13A C13 H13B 109.5 .
P4 C13 H13C 109.5 .
H13A C13 H13C 109.5 .
H13B C13 H13C 109.5 .
P5 C14 H14A 109.5 .
P5 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
P5 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
P5 C15 H15A 109.5 .
P5 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
P5 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
C21 C16 C17 120.4(7) .
C21 C16 Pt1 121.3(6) .
C17 C16 Pt1 118.3(6) .
C16 C17 C18 119.7(8) .
C16 C17 H17 120.2 .
C18 C17 H17 120.2 .
C19 C18 C17 117.4(8) .
C19 C18 H18 121.3 .
C17 C18 H18 121.3 .
C20 C19 F22 119.6(8) .
C20 C19 C18 122.9(8) .
F22 C19 C18 117.5(8) .
C19 C20 C21 118.6(8) .
C19 C20 H20 120.7 .
C21 C20 H20 120.7 .
C16 C21 C20 121.1(8) .
C16 C21 H21 119.5 .
C20 C21 H21 119.5 .
C24 C23 C28 116.4(8) .
C24 C23 Pt1 120.7(6) .
C28 C23 Pt1 122.8(6) .
C25 C24 C23 122.6(8) .
C25 C24 H24 118.7 .
C23 C24 H24 118.7 .
C24 C25 C26 117.9(8) .
C24 C25 H25 121.0 .
C26 C25 H25 121.0 .
F29 C26 C27 119.8(8) .
F29 C26 C25 117.7(8) .
C27 C26 C25 122.4(8) .
C26 C27 C28 117.7(8) .
C26 C27 H27 121.2 .
C28 C27 H27 121.2 .
C23 C28 C27 122.9(8) .
C23 C28 H28 118.5 .
C27 C28 H28 118.5 .
Cl32 C30 Cl31 110.9(7) .
Cl32 C30 H30A 109.5 .
Cl31 C30 H30A 109.5 .
Cl32 C30 H30B 109.5 .
Cl31 C30 H30B 109.5 .
H30A C30 H30B 108.0 .
C35 C33 C34 118.9(10) 2_656
C35 C33 H33 120.6 2_656
C34 C33 H33 120.6 .
C33 C34 C35 119.9(11) .
C33 C34 H34 120.0 .
C35 C34 H34 120.0 .
C33 C35 C34 121.2(10) 2_656
C33 C35 H35 119.4 2_656
C34 C35 H35 119.4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C23 2.110(9) .
Pt1 C16 2.160(7) .
Pt1 P5 2.366(2) .
Pt1 P4 2.394(2) .
Pt1 I2 2.6698(6) .
Pt1 I3 2.6924(6) .
P4 C13 1.815(8) .
P4 C6 1.830(8) .
P4 C12 1.832(9) .
P5 C14 1.814(9) .
P5 C15 1.817(9) .
P5 C11 1.823(9) .
C6 C11 1.387(11) .
C6 C7 1.398(12) .
C7 C8 1.366(12) .
C7 H7 0.9500 .
C8 C9 1.398(13) .
C8 H8 0.9500 .
C9 C10 1.371(12) .
C9 H9 0.9500 .
C10 C11 1.399(11) .
C10 H10 0.9500 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C21 1.357(11) .
C16 C17 1.388(11) .
C17 C18 1.414(12) .
C17 H17 0.9500 .
C18 C19 1.393(12) .
C18 H18 0.9500 .
C19 C20 1.350(13) .
C19 F22 1.378(9) .
C20 C21 1.396(11) .
C20 H20 0.9500 .
C21 H21 0.9500 .
C23 C24 1.389(11) .
C23 C28 1.394(11) .
C24 C25 1.388(12) .
C24 H24 0.9500 .
C25 C26 1.387(12) .
C25 H25 0.9500 .
C26 F29 1.361(9) .
C26 C27 1.363(13) .
C27 C28 1.396(13) .
C27 H27 0.9500 .
C28 H28 0.9500 .
C30 Cl32 1.753(12) .
C30 Cl31 1.755(11) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C33 C35 1.365(15) 2_656
C33 C34 1.398(14) .
C33 H33 0.9500 .
C34 C35 1.407(15) .
C34 H34 0.9500 .
C35 C33 1.365(15) 2_656
C35 H35 0.9500 .
