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#$Date: 2016-03-26 01:32:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180107 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/05/7100587.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_7100587
loop_
_publ_author_name
'A. Carty'
'Todd Graham'
'Konstantin A. Udachin'
_publ_section_title
;
Reactivity Patterns of Thermally Stable, Terminal,
Electrophilic Phosphinidene Complexes Towards Diazoalkanes: Oxidation
at the Phosphorus Centre and Formation of P-bound h1-Phosphaimine,
h1-Phosphaalkene and h3-Diazaphosphaallene Complexes.
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b512375e
_journal_year                    2005
_chemical_formula_sum            'C32 H41 Al Cl6 N3 O2 P W'
_chemical_formula_weight         954.18
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 105.265(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.615(3)
_cell_length_b                   14.159(4)
_cell_length_c                   24.833(6)
_cell_measurement_temperature    125(2)
_cell_volume                     3939.9(18)
_diffrn_ambient_temperature      125(2)
_exptl_crystal_density_diffrn    1.609
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7100587
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
W1 W 0.325881(8) -0.322500(6) -0.331490(4) 0.02050(4) Uani 1 1 d . . .
Cl1 Cl 0.80737(7) -0.20526(5) -0.08148(3) 0.04270(17) Uani 1 1 d . . .
Cl2 Cl 0.75055(10) -0.10469(6) 0.03562(3) 0.0553(2) Uani 1 1 d . . .
Cl3 Cl 0.51666(8) -0.16055(7) -0.07936(5) 0.0589(2) Uani 1 1 d . . .
Cl4 Cl 0.67602(9) -0.33959(5) 0.00425(4) 0.04825(19) Uani 1 1 d . . .
P1 P 0.22278(5) -0.14888(4) -0.33362(2) 0.02068(11) Uani 1 1 d . . .
Al1 Al 0.68737(7) -0.20356(6) -0.03023(3) 0.02746(15) Uani 1 1 d . . .
O1 O 0.52880(16) -0.28596(15) -0.22264(8) 0.0329(4) Uani 1 1 d . . .
O2 O 0.48022(18) -0.17422(14) -0.37493(10) 0.0359(5) Uani 1 1 d . . .
N1 N 0.18638(17) -0.30101(14) -0.29507(8) 0.0204(4) Uani 1 1 d . . .
N2 N 0.14988(16) -0.25416(14) -0.34756(8) 0.0205(4) Uani 1 1 d . . .
N3 N 0.19802(17) -0.09933(14) -0.39540(8) 0.0218(4) Uani 1 1 d . . .
C1 C 0.4520(2) -0.29708(17) -0.26199(10) 0.0243(4) Uani 1 1 d . . .
C2 C 0.4218(2) -0.22717(18) -0.35893(11) 0.0260(5) Uani 1 1 d . . .
C3 C 0.2424(2) -0.47478(17) -0.35159(11) 0.0262(5) Uani 1 1 d . . .
C4 C 0.2373(2) -0.43271(17) -0.40378(10) 0.0259(5) Uani 1 1 d . . .
C5 C 0.3564(2) -0.41142(19) -0.40563(11) 0.0302(5) Uani 1 1 d . . .
C6 C 0.4357(2) -0.44249(19) -0.35409(12) 0.0316(5) Uani 1 1 d . . .
C7 C 0.3649(2) -0.48144(18) -0.32032(11) 0.0306(5) Uani 1 1 d . . .
C8 C 0.1364(3) -0.5125(2) -0.33484(13) 0.0371(6) Uani 1 1 d . . .
H8C H 0.1090 -0.5708 -0.3555 0.055(11) Uiso 1 1 d R . .
H8B H 0.1585 -0.5257 -0.2947 0.042(9) Uiso 1 1 d R . .
H8A H 0.0721 -0.4656 -0.3435 0.053(11) Uiso 1 1 d R . .
C9 C 0.1255(3) -0.4199(2) -0.44935(12) 0.0382(6) Uani 1 1 d . . .
H9C H 0.0639 -0.3917 -0.4340 0.068(13) Uiso 1 1 d R . .
H9B H 0.1411 -0.3782 -0.4781 0.088(16) Uiso 1 1 d R . .
H9A H 0.0979 -0.4814 -0.4658 0.058(11) Uiso 1 1 d R . .
C10 C 0.3927(3) -0.3772(3) -0.45576(14) 0.0473(8) Uani 1 1 d . . .
H10C H 0.3349 -0.3303 -0.4756 0.11(2) Uiso 1 1 d R . .
H10B H 0.4720 -0.3482 -0.4439 0.050(10) Uiso 1 1 d R . .
H10A H 0.3949 -0.4305 -0.4806 0.054(11) Uiso 1 1 d R . .
C11 C 0.5690(3) -0.4466(3) -0.34052(18) 0.0513(9) Uani 1 1 d . . .
H11C H 0.5943 -0.5118 -0.3441 0.062(12) Uiso 1 1 d R . .
H11B H 0.5972 -0.4061 -0.3664 0.037(9) Uiso 1 1 d R . .
H11A H 0.6030 -0.4246 -0.3022 0.056(11) Uiso 1 1 d R . .
C12 C 0.4097(3) -0.5337(2) -0.26613(14) 0.0461(8) Uani 1 1 d . . .
H12C H 0.4904 -0.5120 -0.2474 0.075(14) Uiso 1 1 d R . .
H12B H 0.3566 -0.5216 -0.2421 0.103(19) Uiso 1 1 d R . .
H12A H 0.4114 -0.6016 -0.2736 0.053(11) Uiso 1 1 d R . .
C13 C 0.1200(2) -0.31909(15) -0.26186(10) 0.0206(4) Uani 1 1 d . . .
C14 C 0.1803(2) -0.37086(17) -0.21001(10) 0.0234(4) Uani 1 1 d . . .
C15 C 0.1311(2) -0.45310(18) -0.19491(11) 0.0292(5) Uani 1 1 d . . .
H15 H 0.0559 -0.4750 -0.2166 0.032(8) Uiso 1 1 d R . .
C16 C 0.1924(3) -0.5031(2) -0.14810(13) 0.0393(7) Uani 1 1 d . . .
H16 H 0.1595 -0.5599 -0.1382 0.041(9) Uiso 1 1 d R . .
C17 C 0.3012(3) -0.4708(2) -0.11561(12) 0.0414(7) Uani 1 1 d . . .
H17 H 0.3432 -0.5061 -0.0840 0.046(10) Uiso 1 1 d R . .
C18 C 0.3487(3) -0.3875(2) -0.12919(11) 0.0356(6) Uani 1 1 d . . .
H18 H 0.4220 -0.3644 -0.1062 0.046(10) Uiso 1 1 d R . .
C19 C 0.2892(2) -0.33747(18) -0.17648(10) 0.0264(5) Uani 1 1 d . . .
H19 H 0.3223 -0.2805 -0.1860 0.034(8) Uiso 1 1 d R . .
C20 C -0.0068(2) -0.29259(16) -0.27283(10) 0.0218(4) Uani 1 1 d . . .
C21 C -0.0541(2) -0.27895(17) -0.22722(10) 0.0248(5) Uani 1 1 d . . .
H21 H -0.0047 -0.2881 -0.1905 0.032(8) Uiso 1 1 d R . .
C22 C -0.1726(2) -0.25189(19) -0.23496(11) 0.0298(5) Uani 1 1 d . . .
H22 H -0.2038 -0.2419 -0.2037 0.026(7) Uiso 1 1 d R . .
C23 C -0.2445(2) -0.2397(2) -0.28850(12) 0.0309(5) Uani 1 1 d . . .
H23 H -0.3251 -0.2204 -0.2940 0.031(8) Uiso 1 1 d R . .
C24 C -0.1996(2) -0.2557(2) -0.33440(11) 0.0303(5) Uani 1 1 d . . .
H24 H -0.2500 -0.2484 -0.3711 0.027(7) Uiso 1 1 d R . .
C25 C -0.0815(2) -0.28200(18) -0.32683(10) 0.0254(5) Uani 1 1 d . . .
H25 H -0.0513 -0.2930 -0.3583 0.017(6) Uiso 1 1 d R . .
C26 C 0.2036(2) 0.00621(17) -0.39665(10) 0.0247(5) Uani 1 1 d . . .
H26 H 0.1896 0.0254 -0.4366 0.022(7) Uiso 1 1 d R . .
C27 C 0.3260(3) 0.0423(2) -0.36590(15) 0.0471(8) Uani 1 1 d . . .
H27C H 0.3863 0.0142 -0.3821 0.039(9) Uiso 1 1 d R . .
H27B H 0.3280 0.1112 -0.3693 0.035(8) Uiso 1 1 d R . .
H27A H 0.3428 0.0248 -0.3264 0.073(15) Uiso 1 1 d R . .
C28 C 0.1046(3) 0.0502(2) -0.37554(15) 0.0464(8) Uani 1 1 d . . .
H28C H 0.1165 0.0340 -0.3361 0.050(10) Uiso 1 1 d R . .
H28B H 0.1065 0.1190 -0.3796 0.052(11) Uiso 1 1 d R . .
H28A H 0.0272 0.0260 -0.3972 0.11(2) Uiso 1 1 d R . .
C29 C 0.1596(2) -0.15096(19) -0.44907(10) 0.0288(5) Uani 1 1 d . . .
H29 H 0.1788 -0.2191 -0.4408 0.030(8) Uiso 1 1 d R . .
C30 C 0.0259(3) -0.1442(2) -0.47346(14) 0.0458(8) Uani 1 1 d . . .
H30C H 0.0022 -0.0776 -0.4774 0.051(10) Uiso 1 1 d R . .
H30B H 0.0038 -0.1746 -0.5102 0.042(10) Uiso 1 1 d R . .
H30A H -0.0147 -0.1759 -0.4486 0.063(13) Uiso 1 1 d R . .
C31 C 0.2285(3) -0.1193(2) -0.49023(12) 0.0421(7) Uani 1 1 d . . .
H31C H 0.3143 -0.1241 -0.4726 0.053(11) Uiso 1 1 d R . .
H31B H 0.2076 -0.1598 -0.5234 0.069(14) Uiso 1 1 d R . .
H31A H 0.2081 -0.0536 -0.5012 0.051(10) Uiso 1 1 d R . .
Cl1A Cl 0.11112(9) -0.17293(7) -0.09503(3) 0.0516(2) Uani 1 1 d . . .
Cl2A Cl 0.15774(8) -0.08754(6) -0.19413(4) 0.04848(18) Uani 1 1 d . . .
C1A C 0.2028(3) -0.0997(4) -0.12141(15) 0.0629(12) Uani 1 1 d . . .
H1A1 H 0.2850 -0.1252 -0.1105 0.076 Uiso 1 1 calc R . .
H1A2 H 0.2045 -0.0364 -0.1042 0.076 Uiso 1 1 calc R . .
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
W1 C1 1.981(2) . ?
W1 C2 1.981(3) . ?
W1 N1 2.076(2) . ?
W1 N2 2.2011(19) . ?
W1 C6 2.281(3) . ?
W1 C7 2.298(3) . ?
W1 C5 2.333(2) . ?
W1 C3 2.363(2) . ?
W1 C4 2.397(2) . ?
W1 P1 2.7289(9) . ?
Cl1 Al1 2.1206(11) . ?
Cl2 Al1 2.1309(12) . ?
Cl3 Al1 2.1253(13) . ?
Cl4 Al1 2.1259(12) . ?
P1 N3 1.642(2) . ?
P1 N2 1.704(2) . ?
O1 C1 1.147(3) . ?
O2 C2 1.150(3) . ?
N1 C13 1.294(3) . ?
N1 N2 1.424(3) . ?
N3 C29 1.482(3) . ?
N3 C26 1.497(3) . ?
C3 C4 1.414(4) . ?
C3 C7 1.434(4) . ?
C3 C8 1.498(4) . ?
C4 C5 1.429(3) . ?
C4 C9 1.492(4) . ?
C5 C6 1.435(4) . ?
C5 C10 1.496(4) . ?
C6 C7 1.430(4) . ?
C6 C11 1.498(4) . ?
C7 C12 1.503(4) . ?
C13 C20 1.474(3) . ?
C13 C14 1.487(3) . ?
C14 C15 1.391(3) . ?
C14 C19 1.400(4) . ?
C15 C16 1.387(4) . ?
C16 C17 1.386(5) . ?
C17 C18 1.381(5) . ?
C18 C19 1.390(4) . ?
C20 C21 1.396(3) . ?
C20 C25 1.400(3) . ?
C21 C22 1.393(3) . ?
C22 C23 1.382(4) . ?
C23 C24 1.392(4) . ?
C24 C25 1.385(3) . ?
C26 C27 1.514(4) . ?
C26 C28 1.517(4) . ?
C29 C30 1.513(4) . ?
C29 C31 1.523(4) . ?
Cl1A C1A 1.734(4) . ?
Cl2A C1A 1.751(4) . ?
