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#$Date: 2016-03-21 08:19:26 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178602 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/13/4071354.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_4071354
loop_
_publ_author_name
'Canty, Allan J.'
'Watson, Russell P.'
'Karpiniec, Samuel S.'
'Rodemann, Thomas'
'Gardiner, Michael G.'
'Jones, Roderick C.'
_publ_section_title
;
 Synthesis and Reactivity of (η1-Alkynyl)diorganoplatinum(IV) Species,
 Including Structural Studies of PtIMe(p-Tol)(CCSiMe3)(dmpe) [dmpe
 = 1,2-bis(dimethylphosphino)ethane] and the Platinum(II) Reagent
 PtPh2(dmpe)
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3203
_journal_paper_doi               10.1021/om800122k
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C18 H26 P2 Pt'
_chemical_formula_sum            'C18 H26 P2 Pt'
_chemical_formula_weight         499.42
_chemical_name_systematic
; 
{1,2-bis(dimethylphosphino)ethane}diphenylplatinium(II)  
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 106.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.624(9)
_cell_length_b                   10.9514(18)
_cell_length_c                   10.323(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      14.36
_cell_measurement_theta_min      10.01
_cell_volume                     932.4(10)
_computing_cell_refinement       'CAD4 Express (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf-Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
X-SEED (Barbour, 2001) and ORTEPIII (Farrugia, 1997)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta 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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1812
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.688
_exptl_absorpt_correction_T_max  0.9997
_exptl_absorpt_correction_T_min  0.5922
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   4
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.089
_refine_diff_density_min         -2.223
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0275
_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)+(0.0562P)²+0.8078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                1656
_reflns_number_total             1716
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om800122k-file002.cif
_cod_data_source_block           c:113sk1
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               4071354
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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 0.65792(2) 0.7500 0.628369(18) 0.01885(12) Uani 1 2 d S
P1 P 0.5147(2) 0.7500 0.78273(17) 0.0237(4) Uani 1 2 d S
P2 P 0.4098(2) 0.7500 0.47063(17) 0.0250(4) Uani 1 2 d S
C1 C 0.3023(11) 0.7905(8) 0.6927(8) 0.028(2) Uani 0.50 1 d P
H1A H 0.2305 0.7549 0.7421 0.033 Uiso 0.50 1 calc PR
H1B H 0.2905 0.8804 0.6938 0.033 Uiso 0.50 1 calc PR
C2 C 0.2513(9) 0.7500 0.5582(8) 0.068(3) Uani 1 2 d S
H2A H 0.1608 0.8026 0.5067 0.082 Uiso 0.50 1 calc PR
H2B H 0.2085 0.6659 0.5567 0.082 Uiso 0.50 1 calc PR
C3 C 0.7732(9) 0.7500 0.4777(7) 0.0301(16) Uani 1 2 d S
C4 C 0.8076(9) 0.8560(7) 0.4199(9) 0.067(2) Uani 1 1 d .
H4 H 0.7913 0.9318 0.4586 0.081 Uiso 1 1 calc R
C5 C 0.8652(11) 0.8568(12) 0.3079(10) 0.108(5) Uani 1 1 d .
H5 H 0.8849 0.9322 0.2700 0.130 Uiso 1 1 calc R
C6 C 0.8933(13) 0.7500 0.2523(10) 0.099(6) Uani 1 2 d S
H6 H 0.9324 0.7500 0.1753 0.119 Uiso 1 2 calc SR
C7 C 0.8764(7) 0.7500 0.7796(6) 0.0212(12) Uani 1 2 d S
C8 C 0.9514(6) 0.8579(4) 0.8391(5) 0.0310(10) Uani 1 1 d .
H8 H 0.9033 0.9339 0.8053 0.037 Uiso 1 1 calc R
C9 C 1.0949(6) 0.8577(5) 0.9465(5) 0.0396(12) Uani 1 1 d .
H9 H 1.1436 0.9331 0.9819 0.047 Uiso 1 1 calc R
C10 C 1.1665(8) 0.7500 1.0015(7) 0.0343(16) Uani 1 2 d S
H10 H 1.2628 0.7500 1.0756 0.041 Uiso 1 2 calc SR
C11 C 0.5399(12) 0.8781(7) 0.8948(9) 0.084(3) Uani 1 1 d .
H11A H 0.4642 0.8712 0.9491 0.125 Uiso 1 1 calc R
H11B H 0.5180 0.9537 0.8417 0.125 Uiso 1 1 calc R
H11C H 0.6514 0.8796 0.9549 0.125 Uiso 1 1 calc R
C12 C 0.3639(7) 0.8784(6) 0.3550(6) 0.0444(13) Uani 1 1 d .
H12A H 0.4394 0.8792 0.3001 0.067 Uiso 1 1 calc R
H12B H 0.3747 0.9546 0.4067 0.067 Uiso 1 1 calc R
H12C H 0.2526 0.8709 0.2955 0.067 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'
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'
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
C7 Pt1 C3 92.0(3) . .
C7 Pt1 P2 176.83(16) . .
C3 Pt1 P2 91.1(2) . .
C7 Pt1 P1 91.87(18) . .
C3 Pt1 P1 176.1(2) . .
P2 Pt1 P1 84.96(9) . .
C11 P1 C11 103.2(6) . 4_575
C11 P1 C1 115.4(4) . 4_575
C11 P1 C1 93.0(5) 4_575 4_575
C11 P1 C1 93.0(5) . .
C11 P1 C1 115.4(4) 4_575 .
C1 P1 C1 27.8(6) 4_575 .
C11 P1 Pt1 117.5(2) . .
C11 P1 Pt1 117.5(2) 4_575 .
C1 P1 Pt1 107.9(3) 4_575 .
C1 P1 Pt1 107.9(3) . .
C12 P2 C12 101.8(4) 4_575 .
C12 P2 C2 105.8(3) 4_575 .
C12 P2 C2 105.8(3) . .
C12 P2 Pt1 116.72(19) 4_575 .
C12 P2 Pt1 116.7(2) . .
C2 P2 Pt1 109.0(3) . .
C2 C1 P1 113.6(6) . .
C2 C1 H1A 108.8 . .
P1 C1 H1A 108.8 . .
C2 C1 H1B 108.8 . .
P1 C1 H1B 108.8 . .
H1A C1 H1B 107.7 . .
C1 C2 P2 115.0(6) . .
C1 C2 H2A 108.5 . .
P2 C2 H2A 108.5 . .
C1 C2 H2B 108.5 . .
P2 C2 H2B 108.5 . .
H2A C2 H2B 107.5 . .
C4 C3 C4 115.0(8) 4_575 .
C4 C3 Pt1 122.4(4) 4_575 .
C4 C3 Pt1 122.4(4) . .
C3 C4 C5 122.8(8) . .
C3 C4 H4 118.6 . .
C5 C4 H4 118.6 . .
C6 C5 C4 120.0(9) . .
C6 C5 H5 120.0 . .
C4 C5 H5 120.0 . .
C5 C6 C5 119.3(10) . 4_575
C5 C6 H6 120.4 . .
C5 C6 H6 120.4 4_575 .
C8 C7 C8 115.1(6) . 4_575
C8 C7 Pt1 122.3(3) . .
C8 C7 Pt1 122.3(3) 4_575 .
C7 C8 C9 122.3(5) . .
C7 C8 H8 118.8 . .
C9 C8 H8 118.8 . .
C10 C9 C8 121.0(5) . .
C10 C9 H9 119.5 . .
C8 C9 H9 119.5 . .
C9 C10 C9 118.1(6) 4_575 .
C9 C10 H10 120.9 4_575 .
C9 C10 H10 120.9 . .
P1 C11 H11A 109.5 . .
P1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
P1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
P2 C12 H12A 109.5 . .
P2 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
P2 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C7 2.066(6) .
Pt1 C3 2.076(7) .
Pt1 P2 2.279(3) .
Pt1 P1 2.284(2) .
P1 C11 1.791(6) .
P1 C11 1.791(6) 4_575
P1 C1 1.849(9) 4_575
P1 C1 1.849(9) .
P2 C12 1.812(6) 4_575
P2 C12 1.812(6) .
P2 C2 1.846(8) .
C1 C2 1.401(11) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.376(8) 4_575
C3 C4 1.376(8) .
C4 C5 1.386(12) .
C4 H4 0.9500 .
C5 C6 1.355(13) .
C5 H5 0.9500 .
C6 C5 1.355(13) 4_575
C6 H6 0.9500 .
C7 C8 1.400(6) .
C7 C8 1.400(6) 4_575
C8 C9 1.400(7) .
C8 H8 0.9500 .
C9 C10 1.375(7) .
C9 H9 0.9500 .
C10 C9 1.375(7) 4_575
C10 H10 0.9500 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C7 Pt1 P1 C11 62.1(4) . .
C3 Pt1 P1 C11 -117.9(4) . .
P2 Pt1 P1 C11 -117.9(4) . .
C7 Pt1 P1 C11 -62.1(4) . 4_575
C3 Pt1 P1 C11 117.9(4) . 4_575
P2 Pt1 P1 C11 117.9(4) . 4_575
C7 Pt1 P1 C1 -165.4(3) . 4_575
C3 Pt1 P1 C1 14.6(3) . 4_575
P2 Pt1 P1 C1 14.6(3) . 4_575
C7 Pt1 P1 C1 165.4(3) . .
C3 Pt1 P1 C1 -14.6(3) . .
P2 Pt1 P1 C1 -14.6(3) . .
C7 Pt1 P2 C12 -119.7(3) . 4_575
C3 Pt1 P2 C12 60.3(3) . 4_575
P1 Pt1 P2 C12 -119.7(3) . 4_575
C7 Pt1 P2 C12 119.7(3) . .
C3 Pt1 P2 C12 -60.3(3) . .
P1 Pt1 P2 C12 119.7(3) . .
C7 Pt1 P2 C2 0.000(8) . .
C3 Pt1 P2 C2 180.000(1) . .
P1 Pt1 P2 C2 0.0 . .
C11 P1 C1 C2 152.5(6) . .
C11 P1 C1 C2 -101.5(6) 4_575 .
C1 P1 C1 C2 -62.3(6) 4_575 .
Pt1 P1 C1 C2 32.2(6) . .
P1 C1 C2 P2 -33.9(6) . .
C12 P2 C2 C1 146.7(5) 4_575 .
C12 P2 C2 C1 -105.8(5) . .
Pt1 P2 C2 C1 20.5(4) . .
C7 Pt1 C3 C4 93.0(7) . 4_575
P2 Pt1 C3 C4 -87.0(7) . 4_575
P1 Pt1 C3 C4 -87.0(7) . 4_575
C7 Pt1 C3 C4 -93.0(7) . .
P2 Pt1 C3 C4 87.0(7) . .
P1 Pt1 C3 C4 87.0(7) . .
C4 C3 C4 C5 3.0(16) 4_575 .
Pt1 C3 C4 C5 -171.4(8) . .
C3 C4 C5 C6 -1.5(17) . .
C4 C5 C6 C5 0(2) . 4_575
C3 Pt1 C7 C8 93.3(5) . .
P2 Pt1 C7 C8 -86.7(5) . .
P1 Pt1 C7 C8 -86.7(5) . .
C3 Pt1 C7 C8 -93.3(5) . 4_575
P2 Pt1 C7 C8 86.7(5) . 4_575
P1 Pt1 C7 C8 86.7(5) . 4_575
C8 C7 C8 C9 2.6(9) 4_575 .
Pt1 C7 C8 C9 176.5(4) . .
C7 C8 C9 C10 -2.0(9) . .
C8 C9 C10 C9 1.2(10) . 4_575
