#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:36:07 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178523 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/27/4062772.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_4062772
loop_
_publ_author_name
'Filippou, Alexander C.'
'Philippopoulos, Athanassios I.'
'Portius, Peter'
'Schnakenburg, Gregor'
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om049625m
_journal_year                    2004
_chemical_formula_moiety         'C63 H63 Ge N O1 P4 W, C4 H8 O'
_chemical_formula_sum            'C67 H71 Ge N O2 P4 W'
_chemical_formula_weight         1302.57
_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                 95.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.358(4)
_cell_length_b                   17.610(4)
_cell_length_c                   25.160(8)
_cell_measurement_temperature    180(2)
_cell_volume                     5894(3)
_diffrn_ambient_temperature      180(2)
_exptl_crystal_density_diffrn    1.468
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4062772
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
C1 C 0.0508(4) 0.1671(3) 0.0360(2) 0.0281(13) Uani 1 1 d . . .
C2 C -0.0200(4) 0.2059(3) 0.0699(2) 0.0269(13) Uani 1 1 d . . .
C3 C -0.0365(4) 0.1601(3) 0.1125(2) 0.0299(14) Uani 1 1 d . . .
C4 C 0.0155(4) 0.0899(3) 0.1072(2) 0.0304(13) Uani 1 1 d . . .
C5 C 0.0650(4) 0.0900(3) 0.0623(2) 0.0307(14) Uani 1 1 d . . .
C6 C 0.0321(5) 0.1698(3) -0.0248(2) 0.0425(16) Uani 1 1 d . . .
H6A H 0.0328 0.2227 -0.0369 0.051 Uiso 1 1 calc R . .
H6B H -0.0335 0.1471 -0.0359 0.051 Uiso 1 1 calc R . .
H6C H 0.0849 0.1413 -0.0407 0.051 Uiso 1 1 calc R . .
C7 C -0.0665(5) 0.2820(3) 0.0548(2) 0.0402(15) Uani 1 1 d . . .
H7A H -0.0963 0.2803 0.0178 0.048 Uiso 1 1 calc R . .
H7B H -0.0145 0.3214 0.0584 0.048 Uiso 1 1 calc R . .
H7C H -0.1187 0.2937 0.0785 0.048 Uiso 1 1 calc R . .
C8 C -0.1007(5) 0.1769(3) 0.1578(2) 0.0453(16) Uani 1 1 d . . .
H8A H -0.1408 0.2226 0.1494 0.054 Uiso 1 1 calc R . .
H8B H -0.0572 0.1850 0.1908 0.054 Uiso 1 1 calc R . .
H8C H -0.1455 0.1338 0.1624 0.054 Uiso 1 1 calc R . .
C9 C 0.0146(6) 0.0255(3) 0.1477(3) 0.061(2) Uani 1 1 d . . .
H9A H -0.0550 0.0124 0.1532 0.073 Uiso 1 1 calc R . .
H9B H 0.0497 0.0418 0.1817 0.073 Uiso 1 1 calc R . .
H9C H 0.0485 -0.0190 0.1344 0.073 Uiso 1 1 calc R . .
C10 C 0.1224(5) 0.0265(3) 0.0377(2) 0.0429(16) Uani 1 1 d . . .
H10A H 0.1885 0.0451 0.0298 0.052 Uiso 1 1 calc R . .
H10B H 0.0848 0.0093 0.0047 0.052 Uiso 1 1 calc R . .
H10C H 0.1308 -0.0160 0.0629 0.052 Uiso 1 1 calc R . .
C11 C 0.3442(4) 0.0633(2) 0.12029(19) 0.0189(12) Uani 1 1 d . . .
H11A H 0.3686 0.0216 0.1445 0.023 Uiso 1 1 calc R . .
H11B H 0.2709 0.0567 0.1118 0.023 Uiso 1 1 calc R . .
C12 C 0.3975(4) 0.0591(2) 0.0683(2) 0.0188(12) Uani 1 1 d . . .
H12A H 0.3635 0.0203 0.0446 0.023 Uiso 1 1 calc R . .
H12B H 0.4677 0.0422 0.0772 0.023 Uiso 1 1 calc R . .
C13 C 0.4165(5) 0.4431(2) 0.0633(2) 0.0248(14) Uani 1 1 d . . .
H13A H 0.4848 0.4315 0.0799 0.030 Uiso 1 1 calc R . .
H13B H 0.4205 0.4888 0.0407 0.030 Uiso 1 1 calc R . .
C14 C 0.3443(4) 0.4573(2) 0.10663(19) 0.0237(13) Uani 1 1 d . . .
H14A H 0.2811 0.4794 0.0898 0.028 Uiso 1 1 calc R . .
H14B H 0.3750 0.4947 0.1326 0.028 Uiso 1 1 calc R . .
C15 C 0.2940(4) 0.1414(2) 0.21198(18) 0.0183(11) Uani 1 1 d . . .
C16 C 0.2049(5) 0.1787(3) 0.2158(2) 0.0414(16) Uani 1 1 d . . .
H16A H 0.1812 0.2133 0.1885 0.050 Uiso 1 1 calc R . .
C17 C 0.1474(5) 0.1666(4) 0.2597(2) 0.0563(19) Uani 1 1 d . . .
H17A H 0.0858 0.1931 0.2614 0.068 Uiso 1 1 calc R . .
C18 C 0.1800(5) 0.1168(3) 0.3000(2) 0.0388(15) Uani 1 1 d . . .
H18A H 0.1408 0.1082 0.3291 0.047 Uiso 1 1 calc R . .
C19 C 0.2698(5) 0.0799(3) 0.2975(2) 0.0450(17) Uani 1 1 d . . .
H19A H 0.2930 0.0454 0.3249 0.054 Uiso 1 1 calc R . .
C20 C 0.3274(5) 0.0928(3) 0.2545(2) 0.0386(15) Uani 1 1 d . . .
H20A H 0.3906 0.0683 0.2541 0.046 Uiso 1 1 calc R . .
C21 C 0.4948(4) 0.1431(2) 0.18738(17) 0.0170(11) Uani 1 1 d . . .
C22 C 0.5519(4) 0.0761(2) 0.18603(18) 0.0230(12) Uani 1 1 d . . .
H22A H 0.5256 0.0340 0.1658 0.028 Uiso 1 1 calc R . .
C23 C 0.6460(4) 0.0709(3) 0.2138(2) 0.0309(14) Uani 1 1 d . . .
H23A H 0.6830 0.0248 0.2131 0.037 Uiso 1 1 calc R . .
C24 C 0.6865(4) 0.1323(3) 0.2424(2) 0.0299(13) Uani 1 1 d . . .
H24A H 0.7513 0.1287 0.2612 0.036 Uiso 1 1 calc R . .
C25 C 0.6319(4) 0.1991(3) 0.24376(19) 0.0275(13) Uani 1 1 d . . .
H25A H 0.6597 0.2414 0.2634 0.033 Uiso 1 1 calc R . .
C26 C 0.5375(4) 0.2047(3) 0.21675(19) 0.0263(12) Uani 1 1 d . . .
H26A H 0.5009 0.2508 0.2181 0.032 Uiso 1 1 calc R . .
C27 C 0.3287(4) 0.1311(2) -0.03369(18) 0.0158(11) Uani 1 1 d . . .
C28 C 0.2794(4) 0.1895(3) -0.06213(18) 0.0198(11) Uani 1 1 d . . .
H28A H 0.2807 0.2393 -0.0475 0.024 Uiso 1 1 calc R . .
C29 C 0.2279(4) 0.1760(3) -0.1121(2) 0.0292(13) Uani 1 1 d . . .
H29A H 0.1966 0.2169 -0.1318 0.035 Uiso 1 1 calc R . .
C30 C 0.2223(4) 0.1030(3) -0.1328(2) 0.0323(14) Uani 1 1 d . . .
H30A H 0.1851 0.0935 -0.1661 0.039 Uiso 1 1 calc R . .
C31 C 0.2715(5) 0.0439(3) -0.1046(2) 0.0351(15) Uani 1 1 d . . .
H31A H 0.2678 -0.0063 -0.1185 0.042 Uiso 1 1 calc R . .
C32 C 0.3254(4) 0.0585(3) -0.0567(2) 0.0255(13) Uani 1 1 d . . .
H32A H 0.3616 0.0183 -0.0385 0.031 Uiso 1 1 calc R . .
C33 C 0.5286(4) 0.1503(2) 0.0107(2) 0.0180(11) Uani 1 1 d . . .
C34 C 0.5527(4) 0.1534(2) -0.0417(2) 0.0230(12) Uani 1 1 d . . .
H34A H 0.5000 0.1550 -0.0697 0.028 Uiso 1 1 calc R . .
C35 C 0.6504(5) 0.1541(3) -0.0544(2) 0.0311(15) Uani 1 1 d . . .
H35A H 0.6643 0.1566 -0.0908 0.037 Uiso 1 1 calc R . .
C36 C 0.7291(4) 0.1510(3) -0.0144(2) 0.0328(14) Uani 1 1 d . . .
H36A H 0.7970 0.1505 -0.0230 0.039 Uiso 1 1 calc R . .
C37 C 0.7061(5) 0.1486(3) 0.0387(2) 0.0318(14) Uani 1 1 d . . .
H37A H 0.7591 0.1472 0.0665 0.038 Uiso 1 1 calc R . .
C38 C 0.6077(4) 0.1482(2) 0.0514(2) 0.0235(12) Uani 1 1 d . . .
H38A H 0.5934 0.1465 0.0877 0.028 Uiso 1 1 calc R . .
C39 C 0.4575(4) 0.3543(2) -0.02950(19) 0.0214(12) Uani 1 1 d . . .
C40 C 0.4259(5) 0.3454(2) -0.0838(2) 0.0313(14) Uani 1 1 d . . .
H40A H 0.3560 0.3444 -0.0950 0.038 Uiso 1 1 calc R . .
C41 C 0.4956(5) 0.3379(3) -0.1219(2) 0.0352(15) Uani 1 1 d . . .
H41A H 0.4727 0.3320 -0.1585 0.042 Uiso 1 1 calc R . .
C42 C 0.5968(6) 0.3391(3) -0.1066(2) 0.0422(17) Uani 1 1 d . . .
H42A H 0.6437 0.3339 -0.1326 0.051 Uiso 1 1 calc R . .
C43 C 0.6313(5) 0.3480(3) -0.0525(3) 0.0354(16) Uani 1 1 d . . .
H43A H 0.7013 0.3496 -0.0418 0.042 Uiso 1 1 calc R . .
C44 C 0.5595(5) 0.3546(2) -0.0139(2) 0.0274(14) Uani 1 1 d . . .
H44A H 0.5821 0.3592 0.0229 0.033 Uiso 1 1 calc R . .
C45 C 0.2623(4) 0.4106(2) -0.01482(19) 0.0247(13) Uani 1 1 d . . .
C46 C 0.1651(5) 0.3907(3) -0.0106(2) 0.0454(17) Uani 1 1 d . . .
H46A H 0.1511 0.3475 0.0100 0.055 Uiso 1 1 calc R . .
C47 C 0.0837(6) 0.4330(4) -0.0363(3) 0.062(2) Uani 1 1 d . . .
H47A H 0.0163 0.4172 -0.0334 0.075 Uiso 1 1 calc R . .
C48 C 0.1033(6) 0.4975(3) -0.0656(2) 0.0528(19) Uani 1 1 d . . .
H48A H 0.0495 0.5271 -0.0819 0.063 Uiso 1 1 calc R . .
C49 C 0.2020(6) 0.5182(3) -0.0707(2) 0.0449(18) Uani 1 1 d . . .
H49A H 0.2160 0.5614 -0.0914 0.054 Uiso 1 1 calc R . .
C50 C 0.2809(5) 0.4758(3) -0.0457(2) 0.0331(15) Uani 1 1 d . . .
H50A H 0.3483 0.4908 -0.0495 0.040 Uiso 1 1 calc R . .
C51 C 0.3951(4) 0.3783(2) 0.20535(18) 0.0220(12) Uani 1 1 d . . .
C52 C 0.4920(5) 0.4077(3) 0.2054(2) 0.0304(14) Uani 1 1 d . . .
H52A H 0.5131 0.4298 0.1738 0.036 Uiso 1 1 calc R . .
C53 C 0.5584(5) 0.4047(3) 0.2518(2) 0.0386(15) Uani 1 1 d . . .
H53A H 0.6252 0.4232 0.2515 0.046 Uiso 1 1 calc R . .
C54 C 0.5253(5) 0.3745(3) 0.2982(2) 0.0405(17) Uani 1 1 d . . .
H54A H 0.5696 0.3734 0.3300 0.049 Uiso 1 1 calc R . .
C55 C 0.4318(5) 0.3470(3) 0.2986(2) 0.0358(15) Uani 1 1 d . . .
H55A H 0.4107 0.3265 0.3307 0.043 Uiso 1 1 calc R . .
C56 C 0.3648(4) 0.3479(3) 0.25263(19) 0.0273(13) Uani 1 1 d . . .
H56A H 0.2989 0.3279 0.2535 0.033 Uiso 1 1 calc R . .
C57 C 0.1934(4) 0.3976(3) 0.16676(18) 0.0226(12) Uani 1 1 d . . .
C58 C 0.1063(5) 0.3558(3) 0.1589(2) 0.0324(14) Uani 1 1 d . . .
H58A H 0.1064 0.3093 0.1398 0.039 Uiso 1 1 calc R . .
C59 C 0.0161(5) 0.3813(3) 0.1792(2) 0.0414(16) Uani 1 1 d . . .
H59A H -0.0432 0.3515 0.1736 0.050 Uiso 1 1 calc R . .
C60 C 0.0142(5) 0.4488(3) 0.2068(2) 0.0391(16) Uani 1 1 d . . .
H60A H -0.0461 0.4653 0.2206 0.047 Uiso 1 1 calc R . .
C61 C 0.0988(5) 0.4915(3) 0.2141(2) 0.0420(16) Uani 1 1 d . . .
H61A H 0.0974 0.5382 0.2328 0.050 Uiso 1 1 calc R . .
C62 C 0.1883(5) 0.4675(3) 0.1942(2) 0.0341(14) Uani 1 1 d . . .
H62A H 0.2465 0.4986 0.1992 0.041 Uiso 1 1 calc R . .
C63 C 0.5811(4) 0.3005(3) 0.11516(18) 0.0189(11) Uani 1 1 d . . .
C64 C -0.0611(11) 0.3017(8) 0.3153(6) 0.190(6) Uiso 1 1 d D . .
H64A H -0.0140 0.3342 0.3378 0.228 Uiso 1 1 calc R . .
H64B H -0.0335 0.2978 0.2802 0.228 Uiso 1 1 calc R . .
C65 C -0.0523(11) 0.2144(7) 0.3423(5) 0.162(5) Uiso 1 1 d D . .
H65A H -0.0541 0.1727 0.3159 0.195 Uiso 1 1 calc R . .
H65B H 0.0044 0.2081 0.3701 0.195 Uiso 1 1 calc R . .
C66 C -0.1497(9) 0.2296(6) 0.3635(4) 0.139(4) Uiso 1 1 d D . .
H66A H -0.1911 0.1830 0.3590 0.167 Uiso 1 1 calc R . .
H66B H -0.1372 0.2393 0.4023 0.167 Uiso 1 1 calc R . .
C67 C -0.2029(10) 0.2868(7) 0.3420(5) 0.160(5) Uiso 1 1 d D . .
H67A H -0.2294 0.3152 0.3717 0.192 Uiso 1 1 calc R . .
H67B H -0.2618 0.2645 0.3208 0.192 Uiso 1 1 calc R . .
Ge Ge 0.18414(4) 0.21494(2) 0.06286(2) 0.01875(12) Uani 1 1 d . . .
N N 0.5020(4) 0.28507(18) 0.10582(14) 0.0172(10) Uani 1 1 d . . .
O1 O 0.6691(4) 0.3214(2) 0.12614(17) 0.0532(12) Uani 1 1 d . . .
O2 O -0.1571(13) 0.3457(8) 0.3061(6) 0.316(8) Uiso 1 1 d D . .
P1 P 0.36872(10) 0.15571(6) 0.15423(5) 0.0162(3) Uani 1 1 d . . .
P2 P 0.39861(10) 0.15181(6) 0.03111(5) 0.0141(3) Uani 1 1 d . . .
P3 P 0.36704(11) 0.36139(6) 0.02211(5) 0.0192(3) Uani 1 1 d . . .
P4 P 0.31463(11) 0.36904(6) 0.14296(5) 0.0188(3) Uani 1 1 d . . .
W W 0.345335(15) 0.256025(10) 0.086689(7) 0.01338(5) 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
C1 C2 1.495(7) . ?
C1 C5 1.515(7) . ?
C1 C6 1.528(7) . ?
C1 Ge 2.031(5) . ?
C2 C3 1.375(7) . ?
C2 C7 1.511(7) . ?
C3 C4 1.430(7) . ?
C3 C8 1.516(8) . ?
C4 C5 1.360(8) . ?
C4 C9 1.526(7) . ?
C5 C10 1.518(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.546(7) . ?
C11 P1 1.852(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 P2 1.883(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.540(7) . ?
C13 P3 1.859(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 P4 1.864(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.371(8) . ?
C15 C20 1.411(7) . ?
C15 P1 1.852(5) . ?
C16 C17 1.417(8) . ?
C16 H16A 0.9500 . ?
C17 C18 1.383(8) . ?
C17 H17A 0.9500 . ?
C18 C19 1.371(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.400(8) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
C21 C26 1.404(6) . ?
C21 C22 1.406(6) . ?
C21 P1 1.824(5) . ?
C22 C23 1.385(7) . ?
C22 H22A 0.9500 . ?
C23 C24 1.383(7) . ?
C23 H23A 0.9500 . ?
C24 C25 1.386(7) . ?
C24 H24A 0.9500 . ?
C25 C26 1.382(7) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 C28 1.385(6) . ?
C27 C32 1.401(6) . ?
C27 P2 1.841(5) . ?
C28 C29 1.397(7) . ?
C28 H28A 0.9500 . ?
C29 C30 1.386(7) . ?
C29 H29A 0.9500 . ?
C30 C31 1.391(7) . ?
C30 H30A 0.9500 . ?
C31 C32 1.373(7) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C33 C38 1.403(7) . ?
C33 C34 1.387(7) . ?
C33 P2 1.855(5) . ?
C34 C35 1.371(8) . ?
C34 H34A 0.9500 . ?
C35 C36 1.390(8) . ?
C35 H35A 0.9500 . ?
C36 C37 1.400(8) . ?
C36 H36A 0.9500 . ?
C37 C38 1.381(8) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
C39 C44 1.384(8) . ?
C39 C40 1.402(7) . ?
C39 P3 1.856(5) . ?
C40 C41 1.402(8) . ?
C40 H40A 0.9500 . ?
C41 C42 1.372(9) . ?
C41 H41A 0.9500 . ?
C42 C43 1.406(8) . ?
C42 H42A 0.9500 . ?
C43 C44 1.431(8) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C46 1.357(8) . ?
C45 C50 1.421(6) . ?
C45 P3 1.827(5) . ?
C46 C47 1.424(9) . ?
C46 H46A 0.9500 . ?
C47 C48 1.392(8) . ?
C47 H47A 0.9500 . ?
C48 C49 1.385(9) . ?
C48 H48A 0.9500 . ?
C49 C50 1.394(8) . ?
C49 H49A 0.9500 . ?
C50 H50A 0.9500 . ?
C51 C52 1.394(8) . ?
C51 C56 1.397(7) . ?
C51 P4 1.828(5) . ?
C52 C53 1.402(7) . ?
C52 H52A 0.9500 . ?
C53 C54 1.391(8) . ?
C53 H53A 0.9500 . ?
C54 C55 1.342(8) . ?
C54 H54A 0.9500 . ?
C55 C56 1.398(7) . ?
C55 H55A 0.9500 . ?
C56 H56A 0.9500 . ?
C57 C58 1.375(7) . ?
C57 C62 1.416(6) . ?
C57 P4 1.846(5) . ?
C58 C59 1.422(8) . ?
C58 H58A 0.9500 . ?
C59 C60 1.378(7) . ?
C59 H59A 0.9500 . ?
C60 C61 1.356(8) . ?
C60 H60A 0.9500 . ?
C61 C62 1.402(8) . ?
C61 H61A 0.9500 . ?
C62 H62A 0.9500 . ?
C63 N 1.096(6) . ?
C63 O1 1.238(7) . ?
C64 O2 1.499(14) . ?
C64 C65 1.681(12) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.475(12) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.320(11) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 O2 1.538(13) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
Ge W 2.2991(9) . ?
N W 2.166(5) . ?
P1 W 2.4515(12) . ?
P2 W 2.4514(13) . ?
P3 W 2.5004(13) . ?
P4 W 2.4976(13) . ?
