#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/45/4064517.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_4064517
loop_
_publ_author_name
'Tanabe, Makoto'
'Jiang, Jian'
'Yamazawa, Hideto'
'Osakada, Kohtaro'
'Ohmura, Toshimichi'
'Suginome, Michinori'
_publ_section_title
;
 Dinuclear Palladium and Platinum Complexes with Bridging Silylene
 Ligands. Preparation Using (Aminosilyl)boronic Ester as the Ligand
 Precursor and Their Reactions with Alkynes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3981
_journal_paper_doi               10.1021/om200156g
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C36 H56 P4 Pd2 Si2 '
_chemical_formula_sum            'C36 H56 P4 Pd2 Si2'
_chemical_formula_weight         881.70
_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                98.7843(13)
_cell_angle_beta                 111.692(4)
_cell_angle_gamma                106.126(7)
_cell_formula_units_Z            1
_cell_length_a                   9.609(4)
_cell_length_b                   10.751(5)
_cell_length_c                   11.421(5)
_cell_measurement_reflns_used    3448
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.7
_cell_volume                     1009.2(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2002
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 29.26
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.030
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8254
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             452.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4427
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0403P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                3408
_reflns_number_total             4427
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            om200156g_si_001.cif
_cod_data_source_block           '___complex2'
_cod_original_formula_sum        'C36 H56 P4 Pd2 Si2 '
_cod_database_code               4064517
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
Pd1 Pd 0.75667(3) 0.44993(2) 0.38113(2) 0.02172(8) Uani 1.00 1 d .
P1 P 0.56987(10) 0.24887(9) 0.21067(9) 0.0305(2) Uani 1.00 1 d .
P2 P 0.60558(10) 0.59490(9) 0.35089(9) 0.0319(2) Uani 1.00 1 d .
Si1 Si 1.02228(10) 0.61860(8) 0.50926(8) 0.01991(17) Uani 1.00 1 d .
C1 C 1.0844(3) 0.6937(3) 0.3876(3) 0.0229(6) Uani 1.00 1 d .
C2 C 1.2260(3) 0.8055(3) 0.4297(3) 0.0292(7) Uani 1.00 1 d .
C3 C 1.2734(4) 0.8572(3) 0.3408(3) 0.0363(8) Uani 1.00 1 d .
C4 C 1.1837(4) 0.7973(3) 0.2078(3) 0.0361(8) Uani 1.00 1 d .
C5 C 1.0451(4) 0.6873(3) 0.1634(3) 0.0384(8) Uani 1.00 1 d .
C6 C 0.9952(3) 0.6370(3) 0.2521(3) 0.0298(7) Uani 1.00 1 d .
C7 C 1.0191(3) 0.7536(2) 0.6339(2) 0.0205(6) Uani 1.00 1 d .
C8 C 1.0051(3) 0.7255(3) 0.7460(3) 0.0239(6) Uani 1.00 1 d .
C9 C 1.0025(3) 0.8196(3) 0.8406(3) 0.0297(7) Uani 1.00 1 d .
C10 C 1.0116(4) 0.9472(3) 0.8261(3) 0.0328(7) Uani 1.00 1 d .
C11 C 1.0243(3) 0.9785(3) 0.7178(3) 0.0289(7) Uani 1.00 1 d .
C12 C 1.0286(3) 0.8832(3) 0.6219(3) 0.0255(6) Uani 1.00 1 d .
C13 C 0.5729(6) 0.2818(4) 0.0607(4) 0.0686(14) Uani 1.00 1 d .
C14 C 0.5827(4) 0.0811(3) 0.1887(3) 0.0402(9) Uani 1.00 1 d .
C15 C 0.3573(5) 0.1921(5) 0.1717(5) 0.0865(19) Uani 1.00 1 d .
C16 C 0.5991(4) 0.6838(3) 0.4979(4) 0.0449(9) Uani 1.00 1 d .
C17 C 0.3925(4) 0.5365(4) 0.2370(4) 0.0565(12) Uani 1.00 1 d .
C18 C 0.6819(4) 0.7352(4) 0.2931(4) 0.0477(10) Uani 1.00 1 d .
H1 H 1.2910 0.8468 0.5212 0.035 Uiso 1.00 1 c R
H2 H 1.3686 0.9345 0.3721 0.044 Uiso 1.00 1 c R
H3 H 1.2178 0.8320 0.1473 0.043 Uiso 1.00 1 c R
H4 H 0.9828 0.6451 0.0716 0.046 Uiso 1.00 1 c R
H5 H 0.8976 0.5618 0.2194 0.036 Uiso 1.00 1 c R
H6 H 0.9970 0.6383 0.7567 0.029 Uiso 1.00 1 c R
H7 H 0.9944 0.7973 0.9157 0.036 Uiso 1.00 1 c R
H8 H 1.0091 1.0122 0.8908 0.039 Uiso 1.00 1 c R
H9 H 1.0306 1.0657 0.7076 0.035 Uiso 1.00 1 c R
H10 H 1.0379 0.9067 0.5476 0.031 Uiso 1.00 1 c R
H11 H 0.4913 0.3207 0.0223 0.082 Uiso 1.00 1 c R
H12 H 0.5488 0.1970 -0.0023 0.082 Uiso 1.00 1 c R
H13 H 0.6791 0.3455 0.0802 0.082 Uiso 1.00 1 c R
H14 H 0.6389 0.0711 0.1335 0.048 Uiso 1.00 1 c R
H15 H 0.4743 0.0121 0.1459 0.048 Uiso 1.00 1 c R
H16 H 0.6423 0.0704 0.2745 0.048 Uiso 1.00 1 c R
H17 H 0.3346 0.1316 0.2237 0.104 Uiso 1.00 1 c R
H18 H 0.2940 0.1435 0.0777 0.104 Uiso 1.00 1 c R
H19 H 0.3280 0.2703 0.1919 0.104 Uiso 1.00 1 c R
H20 H 0.5072 0.6284 0.5085 0.054 Uiso 1.00 1 c R
H21 H 0.5882 0.7702 0.4885 0.054 Uiso 1.00 1 c R
H22 H 0.6988 0.7007 0.5753 0.054 Uiso 1.00 1 c R
H23 H 0.3820 0.5459 0.1505 0.068 Uiso 1.00 1 c R
H24 H 0.3412 0.5908 0.2703 0.068 Uiso 1.00 1 c R
H25 H 0.3402 0.4414 0.2293 0.068 Uiso 1.00 1 c R
H26 H 0.7601 0.8130 0.3685 0.057 Uiso 1.00 1 c R
H27 H 0.5928 0.7592 0.2395 0.057 Uiso 1.00 1 c R
H28 H 0.7345 0.7087 0.2396 0.057 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)
;
Pd Pd -0.999 1.007
;
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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
P1 Pd1 P2 101.26(3) yes . .
P1 Pd1 Si1 152.52(4) yes . .
P1 Pd1 Si1 102.04(3) yes . 2_766
P2 Pd1 Si1 99.00(3) yes . .
P2 Pd1 Si1 156.39(2) yes . 2_766
Si1 Pd1 Si1 60.51(2) yes . 2_766
Pd1 P1 C13 105.29(12) yes . .
Pd1 P1 C14 127.44(10) yes . .
Pd1 P1 C15 121.04(18) yes . .
C13 P1 C14 100.1(2) yes . .
C13 P1 C15 102.9(2) yes . .
C14 P1 C15 96.2(2) yes . .
Pd1 P2 C16 116.56(14) yes . .
Pd1 P2 C17 123.21(14) yes . .
Pd1 P2 C18 114.24(16) yes . .
C16 P2 C17 99.2(2) yes . .
C16 P2 C18 101.1(2) yes . .
C17 P2 C18 98.9(2) yes . .
Pd1 Si1 Pd1 119.49(3) yes . 2_766
Pd1 Si1 Si1 59.77(2) yes . 2_766
Pd1 Si1 C1 106.12(7) yes . .
Pd1 Si1 C7 110.33(9) yes . .
Pd1 Si1 Si1 59.72(3) yes 2_766 2_766
Pd1 Si1 C1 101.51(11) yes 2_766 .
Pd1 Si1 C7 108.39(9) yes 2_766 .
Si1 Si1 C1 118.27(11) yes 2_766 .
Si1 Si1 C7 131.14(11) yes 2_766 .
C1 Si1 C7 110.48(15) yes . .
Si1 C1 C2 121.6(2) yes . .
Si1 C1 C6 121.9(2) yes . .
C2 C1 C6 116.4(3) yes . .
C1 C2 C3 121.4(2) yes . .
C2 C3 C4 120.5(3) yes . .
C3 C4 C5 119.5(4) yes . .
C4 C5 C6 120.2(3) yes . .
C1 C6 C5 121.9(2) yes . .
Si1 C7 C8 119.6(2) yes . .
Si1 C7 C12 123.9(2) yes . .
C8 C7 C12 116.5(3) yes . .
C7 C8 C9 122.4(3) yes . .
C8 C9 C10 120.0(3) yes . .
C9 C10 C11 119.6(3) yes . .
C10 C11 C12 120.5(3) yes . .
C7 C12 C11 121.1(3) yes . .
C1 C2 H1 119.3 no . .
C3 C2 H1 119.3 no . .
C2 C3 H2 119.6 no . .
C4 C3 H2 119.8 no . .
C3 C4 H3 120.2 no . .
C5 C4 H3 120.3 no . .
C4 C5 H4 119.9 no . .
C6 C5 H4 119.8 no . .
C1 C6 H5 119.1 no . .
C5 C6 H5 119.0 no . .
C7 C8 H6 118.7 no . .
C9 C8 H6 118.9 no . .
C8 C9 H7 120.0 no . .
C10 C9 H7 120.1 no . .
C9 C10 H8 120.2 no . .
C11 C10 H8 120.2 no . .
C10 C11 H9 119.7 no . .
C12 C11 H9 119.7 no . .
C7 C12 H10 119.5 no . .
C11 C12 H10 119.4 no . .
P1 C13 H11 109.4 no . .
P1 C13 H12 109.6 no . .
P1 C13 H13 109.6 no . .
H11 C13 H12 109.2 no . .
H11 C13 H13 109.4 no . .
H12 C13 H13 109.6 no . .
P1 C14 H14 109.3 no . .
P1 C14 H15 109.5 no . .
P1 C14 H16 109.5 no . .
H14 C14 H15 109.4 no . .
H14 C14 H16 109.4 no . .
H15 C14 H16 109.7 no . .
P1 C15 H17 109.6 no . .
P1 C15 H18 109.4 no . .
P1 C15 H19 109.6 no . .
H17 C15 H18 109.3 no . .
H17 C15 H19 109.6 no . .
H18 C15 H19 109.3 no . .
P2 C16 H20 109.5 no . .
P2 C16 H21 109.5 no . .
P2 C16 H22 109.4 no . .
H20 C16 H21 109.5 no . .
H20 C16 H22 109.5 no . .
H21 C16 H22 109.4 no . .
P2 C17 H23 109.5 no . .
P2 C17 H24 109.5 no . .
P2 C17 H25 109.4 no . .
H23 C17 H24 109.5 no . .
H23 C17 H25 109.5 no . .
H24 C17 H25 109.4 no . .
P2 C18 H26 109.5 no . .
P2 C18 H27 109.6 no . .
P2 C18 H28 109.4 no . .
H26 C18 H27 109.7 no . .
H26 C18 H28 109.3 no . .
H27 C18 H28 109.3 no . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Pd1 P1 2.3792(7) yes .
Pd1 P2 2.3889(11) yes .
Pd1 Si1 2.4086(7) yes .
Pd1 Si1 2.4098(9) yes 2_766
P1 C13 1.810(5) yes .
P1 C14 1.828(4) yes .
P1 C15 1.815(4) yes .
P2 C16 1.832(4) yes .
P2 C17 1.829(3) yes .
P2 C18 1.816(4) yes .
Si1 Si1 2.4276(12) yes 2_766
Si1 C1 1.905(3) yes .
Si1 C7 1.887(3) yes .
C1 C2 1.399(4) yes .
C1 C6 1.394(4) yes .
C2 C3 1.386(6) yes .
C3 C4 1.374(4) yes .
C4 C5 1.368(4) yes .
C5 C6 1.390(6) yes .
C7 C8 1.404(5) yes .
C7 C12 1.402(4) yes .
C8 C9 1.375(5) yes .
C9 C10 1.389(5) yes .
C10 C11 1.369(5) yes .
C11 C12 1.401(5) yes .
C2 H1 0.949 no .
C3 H2 0.949 no .
C4 H3 0.950 no .
C5 H4 0.950 no .
C6 H5 0.949 no .
C8 H6 0.949 no .
C9 H7 0.949 no .
C10 H8 0.949 no .
C11 H9 0.950 no .
C12 H10 0.950 no .
C13 H11 0.983 no .
C13 H12 0.980 no .
C13 H13 0.978 no .
C14 H14 0.982 no .
C14 H15 0.979 no .
C14 H16 0.978 no .
C15 H17 0.979 no .
C15 H18 0.982 no .
C15 H19 0.979 no .
C16 H20 0.979 no .
C16 H21 0.980 no .
C16 H22 0.980 no .
C17 H23 0.979 no .
C17 H24 0.979 no .
C17 H25 0.980 no .
C18 H26 0.979 no .
C18 H27 0.979 no .
C18 H28 0.982 no .
