#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/11/4071134.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_4071134
loop_
_publ_author_name
'Tanabe, Makoto'
'Ito, Daisuke'
'Osakada, Kohtaro'
_publ_section_title
;
 Ligand Exchange of Diplatinum Complexes with Bridging Silyl Ligands
 Involving Si−H Bond Cleavage and Formation
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2258
_journal_paper_doi               10.1021/om7012869
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C18 H26 P2 Pt Si '
_chemical_formula_sum            'C18 H26 P2 Pt Si'
_chemical_formula_weight         527.53
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                102.781(2)
_cell_angle_beta                 112.877(3)
_cell_angle_gamma                104.3217(5)
_cell_formula_units_Z            2
_cell_length_a                   9.183(2)
_cell_length_b                   11.193(3)
_cell_length_c                   11.320(3)
_cell_measurement_reflns_used    3085
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     970.8(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6669
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    7.419
_exptl_absorpt_correction_T_max  0.051
_exptl_absorpt_correction_T_min  0.030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             512.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.66
_refine_diff_density_min         -1.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3745
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0001Fo² + 1.0000σ(Fo²)]/(4Fo²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                3744
_reflns_number_total             4019
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            om7012869-file001.cif
_cod_data_source_block           '__Complex9'
_cod_original_cell_volume        970.9(5)
_cod_original_formula_sum        'C18 H26 P2 Pt Si '
_cod_database_code               4071134
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -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 0.26024(2) 0.460020(10) 0.376970(10) 0.00942(4) Uani 1.00 1 d .
P1 P 0.02430(12) 0.28165(11) 0.20611(11) 0.0164(2) Uani 1.00 1 d .
P2 P 0.09604(13) 0.58302(11) 0.31573(11) 0.0159(2) Uani 1.00 1 d .
Si1 Si 0.46376(13) 0.37076(11) 0.48576(11) 0.0101(2) Uani 1.00 1 d .
C1 C 0.4023(5) 0.3045(3) 0.6094(4) 0.0125(9) Uani 1.00 1 d .
C2 C 0.4854(5) 0.3760(4) 0.7505(4) 0.0172(10) Uani 1.00 1 d .
C3 C 0.4338(5) 0.3317(4) 0.8397(4) 0.0199(11) Uani 1.00 1 d .
C4 C 0.2991(5) 0.2137(4) 0.7897(4) 0.0198(11) Uani 1.00 1 d .
C5 C 0.2161(5) 0.1389(4) 0.6501(4) 0.0195(11) Uani 1.00 1 d .
C6 C 0.2674(5) 0.1849(4) 0.5629(4) 0.0155(10) Uani 1.00 1 d .
C7 C 0.4602(4) 0.2266(3) 0.3578(3) 0.0120(9) Uani 1.00 1 d .
C8 C 0.4585(5) 0.1043(4) 0.3718(4) 0.0153(10) Uani 1.00 1 d .
C9 C 0.4657(5) 0.0064(4) 0.2759(4) 0.0178(10) Uani 1.00 1 d .
C10 C 0.4717(5) 0.0273(4) 0.1617(4) 0.0214(11) Uani 1.00 1 d .
C11 C 0.4720(5) 0.1463(4) 0.1445(4) 0.0203(11) Uani 1.00 1 d .
C12 C 0.4675(5) 0.2430(4) 0.2411(4) 0.0153(10) Uani 1.00 1 d .
C13 C 0.0178(8) 0.6389(6) 0.4335(6) 0.048(2) Uani 1.00 1 d .
C14 C 0.1678(5) 0.7328(4) 0.2828(4) 0.0261(12) Uani 1.00 1 d .
C15 C -0.0723(5) 0.1214(4) 0.2135(4) 0.0266(12) Uani 1.00 1 d .
C16 C 0.0469(6) 0.2301(5) 0.0515(4) 0.0337(13) Uani 1.00 1 d .
C17 C -0.1568(5) 0.3362(5) 0.1487(5) 0.0325(13) Uani 1.00 1 d .
C18 C -0.0977(5) 0.4782(4) 0.1543(5) 0.0282(12) Uani 1.00 1 d .
H1 H 0.5795 0.4565 0.7868 0.020 Uiso 1.00 1 c R
H2 H 0.4917 0.3833 0.9348 0.025 Uiso 1.00 1 c R
H3 H 0.2636 0.1838 0.8499 0.028 Uiso 1.00 1 c R
H4 H 0.1248 0.0568 0.6145 0.024 Uiso 1.00 1 c R
H5 H 0.2087 0.1334 0.4678 0.019 Uiso 1.00 1 c R
H6 H 0.4518 0.0882 0.4489 0.018 Uiso 1.00 1 c R
H7 H 0.4662 -0.0745 0.2890 0.021 Uiso 1.00 1 c R
H8 H 0.4763 -0.0391 0.0960 0.023 Uiso 1.00 1 c R
H9 H 0.4755 0.1609 0.0659 0.023 Uiso 1.00 1 c R
H10 H 0.4675 0.3237 0.2274 0.018 Uiso 1.00 1 c R
H11 H -0.0895 0.5747 0.4071 0.084 Uiso 1.00 1 c R
H12 H 0.0055 0.7202 0.4309 0.084 Uiso 1.00 1 c R
H13 H 0.0959 0.6507 0.5239 0.084 Uiso 1.00 1 c R
H14 H 0.2221 0.8067 0.3657 0.029 Uiso 1.00 1 c R
H15 H 0.0729 0.7426 0.2173 0.029 Uiso 1.00 1 c R
H16 H 0.2460 0.7274 0.2483 0.029 Uiso 1.00 1 c R
H17 H -0.0224 0.0626 0.1869 0.027 Uiso 1.00 1 c R
H18 H -0.1911 0.0866 0.1528 0.027 Uiso 1.00 1 c R
H19 H -0.0539 0.1319 0.3044 0.027 Uiso 1.00 1 c R
H20 H 0.0029 0.2761 -0.0063 0.035 Uiso 1.00 1 c R
H21 H -0.0143 0.1379 0.0043 0.035 Uiso 1.00 1 c R
H22 H 0.1639 0.2498 0.0762 0.035 Uiso 1.00 1 c R
H23 H -0.2380 0.2798 0.0573 0.035 Uiso 1.00 1 c R
H24 H -0.2075 0.3312 0.2072 0.035 Uiso 1.00 1 c R
H25 H -0.1853 0.5114 0.1471 0.029 Uiso 1.00 1 c R
H26 H -0.0746 0.4796 0.0796 0.029 Uiso 1.00 1 c R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
P P 0.102 0.094
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Pt Pt -1.703 8.390
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.082 0.070
;
International Tables for Crystallography
(1992, 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
P1 Pt1 P2 85.48(3) . .
P1 Pt1 Si1 105.72(3) . .
P1 Pt1 Si1 164.61(5) . 2_666
P2 Pt1 Si1 167.82(3) . .
P2 Pt1 Si1 100.90(4) . 2_666
Si1 Pt1 Si1 69.48(4) . 2_666
Pt1 P1 C15 128.30(14) . .
Pt1 P1 C16 111.49(16) . .
Pt1 P1 C17 108.14(14) . .
C15 P1 C16 100.8(2) . .
C15 P1 C17 102.3(2) . .
C16 P1 C17 102.9(2) . .
Pt1 P2 C13 115.2(2) . .
Pt1 P2 C14 123.45(19) . .
Pt1 P2 C18 108.34(18) . .
C13 P2 C14 100.7(3) . .
C13 P2 C18 104.2(2) . .
C14 P2 C18 102.8(2) . .
Pt1 Si1 Pt1 110.52(4) . 2_666
Pt1 Si1 C1 107.50(15) . .
Pt1 Si1 C7 111.97(13) . .
Pt1 Si1 C1 106.48(9) 2_666 .
Pt1 Si1 C7 112.80(13) 2_666 .
C1 Si1 C7 107.2(2) . .
Si1 C1 C2 121.7(3) . .
Si1 C1 C6 122.0(3) . .
C2 C1 C6 116.3(4) . .
C1 C2 C3 121.8(3) . .
C2 C3 C4 120.2(3) . .
C3 C4 C5 119.4(5) . .
C4 C5 C6 119.7(3) . .
C1 C6 C5 122.7(3) . .
Si1 C7 C8 126.0(3) . .
Si1 C7 C12 118.1(3) . .
C8 C7 C12 115.8(4) . .
C7 C8 C9 122.1(4) . .
C8 C9 C10 119.9(4) . .
C9 C10 C11 119.4(4) . .
C10 C11 C12 120.1(5) . .
C7 C12 C11 122.7(4) . .
P1 C17 C18 110.7(3) . .
P2 C18 C17 110.9(3) . .
C1 C2 H1 119.0 . .
C3 C2 H1 119.2 . .
C2 C3 H2 119.7 . .
C4 C3 H2 120.1 . .
C3 C4 H3 120.3 . .
C5 C4 H3 120.3 . .
C4 C5 H4 120.3 . .
C6 C5 H4 120.0 . .
C1 C6 H5 118.6 . .
C5 C6 H5 118.7 . .
C7 C8 H6 118.7 . .
C9 C8 H6 119.2 . .
C8 C9 H7 120.0 . .
C10 C9 H7 120.1 . .
C9 C10 H8 120.2 . .
C11 C10 H8 120.4 . .
C10 C11 H9 119.7 . .
C12 C11 H9 120.2 . .
C7 C12 H10 118.4 . .
C11 C12 H10 118.8 . .
P2 C13 H11 109.2 . .
P2 C13 H12 109.6 . .
P2 C13 H13 109.6 . .
H11 C13 H12 109.5 . .
H11 C13 H13 109.5 . .
H12 C13 H13 109.5 . .
P2 C14 H14 109.5 . .
P2 C14 H15 109.6 . .
P2 C14 H16 109.4 . .
H14 C14 H15 109.5 . .
H14 C14 H16 109.5 . .
H15 C14 H16 109.5 . .
P1 C15 H17 109.6 . .
P1 C15 H18 109.3 . .
P1 C15 H19 109.6 . .
H17 C15 H18 109.5 . .
H17 C15 H19 109.5 . .
H18 C15 H19 109.5 . .
P1 C16 H20 109.4 . .
P1 C16 H21 109.6 . .
P1 C16 H22 109.5 . .
H20 C16 H21 109.5 . .
H20 C16 H22 109.5 . .
H21 C16 H22 109.5 . .
P1 C17 H23 109.0 . .
P1 C17 H24 109.0 . .
C18 C17 H23 109.7 . .
C18 C17 H24 108.9 . .
H23 C17 H24 109.5 . .
P2 C18 H25 109.2 . .
P2 C18 H26 109.1 . .
C17 C18 H25 109.1 . .
C17 C18 H26 108.9 . .
H25 C18 H26 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 P1 2.3053(8) .
Pt1 P2 2.2992(13) .
Pt1 Si1 2.3846(13) .
Pt1 Si1 2.3847(9) 2_666
P1 C15 1.830(5) .
P1 C16 1.825(6) .
P1 C17 1.844(5) .
P2 C13 1.811(8) .
P2 C14 1.818(5) .
P2 C18 1.836(3) .
Si1 C1 1.922(5) .
Si1 C7 1.899(4) .
C1 C2 1.400(5) .
C1 C6 1.401(5) .
C2 C3 1.402(8) .
C3 C4 1.383(5) .
C4 C5 1.393(5) .
C5 C6 1.389(7) .
C7 C8 1.409(6) .
C7 C12 1.398(7) .
C8 C9 1.396(6) .
C9 C10 1.383(7) .
C10 C11 1.388(7) .
C11 C12 1.380(7) .
C17 C18 1.525(7) .
C2 H1 0.950 .
C3 H2 0.950 .
C4 H3 0.950 .
C5 H4 0.950 .
C6 H5 0.950 .
C8 H6 0.950 .
C9 H7 0.950 .
C10 H8 0.950 .
C11 H9 0.950 .
C12 H10 0.950 .
C13 H11 0.950 .
C13 H12 0.950 .
C13 H13 0.950 .
C14 H14 0.950 .
C14 H15 0.950 .
C14 H16 0.950 .
C15 H17 0.950 .
C15 H18 0.950 .
C15 H19 0.950 .
C16 H20 0.950 .
C16 H21 0.950 .
C16 H22 0.950 .
C17 H23 0.950 .
C17 H24 0.950 .
C18 H25 0.950 .
C18 H26 0.950 .
