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#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/16/4061635.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_4061635
loop_
_publ_author_name
'Vicente, José'
'Abad, José-Antonio'
'López, Joaquín'
'Jones, Peter G.'
'Nájera, Carmen'
'Botella-Segura, Luis'
_publ_section_title
;
 Synthesis and reactivity of ortho-palladated arylureas. Synthesis and
 catalytic activity of a C,N,C pincer complex. Stiochiometric syntheses
 of some N-heterocycles.
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om050451y
_journal_year                    2005
_chemical_formula_sum            'C31 H37 F3 N4 O6 Pd S'
_chemical_formula_weight         757.11
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                96.519(4)
_cell_angle_beta                 94.892(4)
_cell_angle_gamma                105.625(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2565(6)
_cell_length_b                   12.1297(6)
_cell_length_c                   12.7493(6)
_cell_measurement_temperature    133(2)
_cell_volume                     1653.34(14)
_diffrn_ambient_temperature      133(2)
_exptl_crystal_density_diffrn    1.521
_cod_database_code               4061635
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.551216(7) 0.849684(7) 0.682924(6) 0.01650(3) Uani 1 1 d . . .
N1 N 0.63732(11) 1.02400(9) 0.72133(9) 0.0268(2) Uani 1 1 d . . .
N2 N 0.73044(10) 0.83622(9) 0.64951(9) 0.0241(2) Uani 1 1 d . . .
N3 N 0.37172(10) 0.58624(9) 0.75439(8) 0.02180(19) Uani 1 1 d . . .
H03 H 0.3142(16) 0.5380(15) 0.7649(13) 0.030(4) Uiso 1 1 d . . .
N4 N 0.30553(10) 0.53019(9) 0.57673(8) 0.0232(2) Uani 1 1 d . . .
H04 H 0.2431(16) 0.4880(15) 0.5965(13) 0.030(4) Uiso 1 1 d . . .
O1 O 0.48087(8) 0.67722(7) 0.62975(7) 0.02273(17) Uani 1 1 d . . .
O2 O 0.30756(9) 0.98117(9) 0.62632(8) 0.0305(2) Uani 1 1 d . . .
O3 O 0.20457(9) 0.79243(9) 0.61359(7) 0.0292(2) Uani 1 1 d . . .
C1 C 0.59989(17) 1.08360(13) 0.81581(13) 0.0391(3) Uani 1 1 d . . .
H1A H 0.6523 1.1638 0.8313 0.047 Uiso 1 1 calc R . .
H1B H 0.6100 1.0436 0.8772 0.047 Uiso 1 1 calc R . .
H1C H 0.5127 1.0827 0.8014 0.047 Uiso 1 1 calc R . .
C2 C 0.61640(15) 1.08523(12) 0.62954(12) 0.0352(3) Uani 1 1 d . . .
H2A H 0.5284 1.0826 0.6178 0.042 Uiso 1 1 calc R . .
H2B H 0.6397 1.0474 0.5656 0.042 Uiso 1 1 calc R . .
H2C H 0.6673 1.1660 0.6448 0.042 Uiso 1 1 calc R . .
C3 C 0.77228(14) 1.03206(13) 0.74511(14) 0.0393(3) Uani 1 1 d . . .
H3A H 0.7872 1.0071 0.8151 0.047 Uiso 1 1 calc R . .
H3B H 0.8226 1.1134 0.7485 0.047 Uiso 1 1 calc R . .
C4 C 0.81157(13) 0.95660(13) 0.66017(15) 0.0382(3) Uani 1 1 d . . .
H4A H 0.8054 0.9866 0.5915 0.046 Uiso 1 1 calc R . .
H4B H 0.8991 0.9580 0.6794 0.046 Uiso 1 1 calc R . .
C5 C 0.77333(13) 0.77294(14) 0.73091(12) 0.0336(3) Uani 1 1 d . . .
H5A H 0.7191 0.6935 0.7216 0.040 Uiso 1 1 calc R . .
H5B H 0.7705 0.8118 0.8020 0.040 Uiso 1 1 calc R . .
H5C H 0.8588 0.7717 0.7230 0.040 Uiso 1 1 calc R . .
C6 C 0.73071(13) 0.77495(14) 0.54294(12) 0.0336(3) Uani 1 1 d . . .
H6A H 0.7002 0.8153 0.4888 0.040 Uiso 1 1 calc R . .
H6B H 0.6765 0.6957 0.5362 0.040 Uiso 1 1 calc R . .
H6C H 0.8155 0.7731 0.5329 0.040 Uiso 1 1 calc R . .
C11 C 0.45185(10) 0.65442(10) 0.84536(9) 0.0192(2) Uani 1 1 d . . .
C12 C 0.44539(10) 0.76605(10) 0.87977(9) 0.0182(2) Uani 1 1 d . . .
C13 C 0.52197(12) 0.82762(11) 0.97126(10) 0.0246(2) Uani 1 1 d . . .
H13 H 0.5191 0.9037 0.9958 0.029 Uiso 1 1 calc R . .
C14 C 0.60226(13) 0.77976(12) 1.02705(11) 0.0298(3) Uani 1 1 d . . .
H14 H 0.6541 0.8234 1.0889 0.036 Uiso 1 1 calc R . .
C15 C 0.60709(13) 0.66860(12) 0.99287(11) 0.0297(3) Uani 1 1 d . . .
H15 H 0.6615 0.6355 1.0313 0.036 Uiso 1 1 calc R . .
C16 C 0.53160(12) 0.60610(11) 0.90199(10) 0.0255(2) Uani 1 1 d . . .
H16 H 0.5343 0.5298 0.8782 0.031 Uiso 1 1 calc R . .
C17 C 0.35652(10) 0.81603(10) 0.82010(9) 0.0183(2) Uani 1 1 d . . .
C18 C 0.38712(11) 0.85526(10) 0.72867(9) 0.0188(2) Uani 1 1 d . . .
C19 C 0.29779(11) 0.88677(11) 0.65364(9) 0.0213(2) Uani 1 1 d . . .
C20 C 0.10975(14) 0.80789(16) 0.53749(13) 0.0409(4) Uani 1 1 d . . .
H20A H 0.0834 0.8752 0.5648 0.049 Uiso 1 1 calc R . .
H20B H 0.0383 0.7387 0.5261 0.049 Uiso 1 1 calc R . .
H20C H 0.1433 0.8202 0.4699 0.049 Uiso 1 1 calc R . .
C21 C 0.29547(12) 0.54073(10) 0.46669(9) 0.0224(2) Uani 1 1 d . . .
C22 C 0.39727(13) 0.58100(12) 0.41302(10) 0.0281(3) Uani 1 1 d . . .
H22 H 0.4790 0.6039 0.4499 0.034 Uiso 1 1 calc R . .
C23 C 0.37867(14) 0.58760(12) 0.30461(11) 0.0303(3) Uani 1 1 d . . .
H23 H 0.4485 0.6176 0.2689 0.036 Uiso 1 1 calc R . .
C24 C 0.26114(14) 0.55161(12) 0.24742(10) 0.0307(3) Uani 1 1 d . . .
C25 C 0.16063(14) 0.50853(13) 0.30219(11) 0.0317(3) Uani 1 1 d . . .
H25 H 0.0793 0.4819 0.2645 0.038 Uiso 1 1 calc R . .
C26 C 0.17664(12) 0.50372(12) 0.41056(10) 0.0272(2) Uani 1 1 d . . .
H26 H 0.1066 0.4752 0.4465 0.033 Uiso 1 1 calc R . .
C27 C 0.24186(17) 0.56048(16) 0.13029(12) 0.0419(4) Uani 1 1 d . . .
H27A H 0.3213 0.5996 0.1071 0.050 Uiso 1 1 calc R . .
H27B H 0.1823 0.6049 0.1180 0.050 Uiso 1 1 calc R . .
H27C H 0.2095 0.4827 0.0898 0.050 Uiso 1 1 calc R . .
C28 C 0.38920(11) 0.60271(10) 0.65350(9) 0.0195(2) Uani 1 1 d . . .
C31 C 0.23958(11) 0.81499(10) 0.86649(9) 0.0196(2) Uani 1 1 d . . .
C32 C 0.18807(12) 0.90770(11) 0.86388(10) 0.0252(2) Uani 1 1 d . . .
H32 H 0.2279 0.9722 0.8313 0.030 Uiso 1 1 calc R . .
C33 C 0.07915(13) 0.90650(13) 0.90847(11) 0.0315(3) Uani 1 1 d . . .
H33 H 0.0453 0.9701 0.9060 0.038 Uiso 1 1 calc R . .
C34 C 0.01966(13) 0.81314(14) 0.95642(11) 0.0325(3) Uani 1 1 d . . .
H34 H -0.0547 0.8125 0.9867 0.039 Uiso 1 1 calc R . .
C35 C 0.06977(13) 0.72050(13) 0.95972(11) 0.0318(3) Uani 1 1 d . . .
H35 H 0.0293 0.6562 0.9923 0.038 Uiso 1 1 calc R . .
C36 C 0.17869(12) 0.72139(12) 0.91569(10) 0.0264(3) Uani 1 1 d . . .
H36 H 0.2124 0.6578 0.9189 0.032 Uiso 1 1 calc R . .
S S 0.08852(3) 0.33789(3) 0.74764(3) 0.02430(6) Uani 1 1 d . . .
O4 O 0.09794(9) 0.37933(9) 0.64558(8) 0.0340(2) Uani 1 1 d . . .
O5 O -0.03543(9) 0.29163(9) 0.77215(9) 0.0334(2) Uani 1 1 d . . .
O6 O 0.17607(10) 0.41237(9) 0.83333(8) 0.0345(2) Uani 1 1 d . . .
C99 C 0.14620(12) 0.21100(12) 0.72792(10) 0.0266(2) Uani 1 1 d . . .
F1 F 0.08349(8) 0.13722(8) 0.64272(7) 0.03646(19) Uani 1 1 d . . .
F2 F 0.13321(9) 0.15347(8) 0.81170(7) 0.0386(2) Uani 1 1 d . . .
F3 F 0.26609(8) 0.24047(8) 0.71423(7) 0.0384(2) Uani 1 1 d . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd C18 1.9997(11) . ?
Pd O1 2.0388(9) . ?
Pd N1 2.0567(11) . ?
Pd N2 2.1416(10) . ?
N1 C1 1.4847(17) . ?
N1 C2 1.4903(18) . ?
N1 C3 1.4980(19) . ?
N2 C6 1.4734(18) . ?
N2 C5 1.4814(18) . ?
N2 C4 1.4833(17) . ?
N3 C28 1.3466(15) . ?
N3 C11 1.4300(15) . ?
N4 C28 1.3490(15) . ?
N4 C21 1.4209(15) . ?
O1 C28 1.2595(14) . ?
O2 C19 1.2140(15) . ?
O3 C19 1.3418(16) . ?
O3 C20 1.4451(16) . ?
C3 C4 1.510(2) . ?
C11 C16 1.3927(16) . ?
C11 C12 1.3981(16) . ?
C12 C13 1.3948(16) . ?
C12 C17 1.4995(15) . ?
C13 C14 1.3880(18) . ?
C14 C15 1.3860(19) . ?
C15 C16 1.3873(19) . ?
C17 C18 1.3453(15) . ?
C17 C31 1.4860(15) . ?
C18 C19 1.4826(16) . ?
C21 C22 1.3886(18) . ?
C21 C26 1.3940(18) . ?
C22 C23 1.3947(18) . ?
C23 C24 1.387(2) . ?
C24 C25 1.393(2) . ?
C24 C27 1.5108(19) . ?
C25 C26 1.3880(19) . ?
C31 C32 1.3994(16) . ?
C31 C36 1.4028(16) . ?
C32 C33 1.3920(17) . ?
C33 C34 1.387(2) . ?
C34 C35 1.389(2) . ?
C35 C36 1.3893(18) . ?
S O5 1.4323(10) . ?
S O6 1.4469(11) . ?
S O4 1.4493(10) . ?
S C99 1.8255(14) . ?
C99 F3 1.3319(15) . ?
C99 F1 1.3369(16) . ?
C99 F2 1.3379(15) . ?
