#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/27/4062773.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_4062773
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 P4 W, 0.5(C7 H8)'
_chemical_formula_sum            'C66.5 H67 Ge N P4 W'
_chemical_formula_weight         1260.53
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 97.563(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.601(4)
_cell_length_b                   13.466(3)
_cell_length_c                   34.549(5)
_cell_measurement_temperature    180(2)
_cell_volume                     11346(3)
_diffrn_ambient_temperature      180(2)
_exptl_crystal_density_diffrn    1.476
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'C66.50 H67 Ge N P4 W'
_cod_database_code               4062773
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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 0.50828(16) 0.1580(3) 0.42650(13) 0.0217(9) Uani 1 1 d . . .
C5 C 0.50961(17) 0.1882(3) 0.46874(13) 0.0237(10) Uani 1 1 d . . .
C4 C 0.46884(18) 0.1409(3) 0.48418(13) 0.0253(10) Uani 1 1 d . . .
C3 C 0.43964(17) 0.0755(3) 0.45467(13) 0.0263(9) Uani 1 1 d . . .
C2 C 0.46215(16) 0.0830(3) 0.42103(12) 0.0253(9) Uani 1 1 d . . .
C6 C 0.56369(18) 0.1216(3) 0.41601(14) 0.0320(11) Uani 1 1 d . . .
H6C H 0.5592 0.0993 0.3888 0.038 Uiso 1 1 calc R . .
H6B H 0.5769 0.0663 0.4332 0.038 Uiso 1 1 calc R . .
H6A H 0.5903 0.1761 0.4194 0.038 Uiso 1 1 calc R . .
C10 C 0.55296(18) 0.2564(4) 0.48898(14) 0.0340(11) Uani 1 1 d . . .
H10C H 0.5461 0.2674 0.5160 0.041 Uiso 1 1 calc R . .
H10B H 0.5518 0.3200 0.4752 0.041 Uiso 1 1 calc R . .
H10A H 0.5892 0.2260 0.4890 0.041 Uiso 1 1 calc R . .
C9 C 0.4568(2) 0.1482(4) 0.52573(15) 0.0413(13) Uani 1 1 d . . .
H9C H 0.4193 0.1729 0.5260 0.050 Uiso 1 1 calc R . .
H9B H 0.4828 0.1941 0.5403 0.050 Uiso 1 1 calc R . .
H9A H 0.4603 0.0825 0.5379 0.050 Uiso 1 1 calc R . .
C8 C 0.3944(2) 0.0077(4) 0.46243(17) 0.0428(13) Uani 1 1 d . . .
H8C H 0.3834 -0.0336 0.4394 0.051 Uiso 1 1 calc R . .
H8B H 0.3630 0.0470 0.4683 0.051 Uiso 1 1 calc R . .
H8A H 0.4071 -0.0350 0.4848 0.051 Uiso 1 1 calc R . .
C7 C 0.4488(2) 0.0257(4) 0.38365(15) 0.0391(12) Uani 1 1 d . . .
H7A H 0.4811 -0.0122 0.3785 0.047 Uiso 1 1 calc R . .
H7B H 0.4383 0.0720 0.3621 0.047 Uiso 1 1 calc R . .
H7C H 0.4184 -0.0200 0.3860 0.047 Uiso 1 1 calc R . .
C14 C 0.40129(15) 0.3430(3) 0.26360(12) 0.0207(9) Uani 1 1 d . . .
H14A H 0.3712 0.3109 0.2462 0.025 Uiso 1 1 calc R . .
H14B H 0.4113 0.4055 0.2512 0.025 Uiso 1 1 calc R . .
C13 C 0.45089(15) 0.2737(3) 0.27045(13) 0.0203(9) Uani 1 1 d . . .
H13A H 0.4639 0.2580 0.2452 0.024 Uiso 1 1 calc R . .
H13B H 0.4403 0.2108 0.2823 0.024 Uiso 1 1 calc R . .
C12 C 0.50504(14) 0.5746(3) 0.43780(12) 0.0231(9) Uani 1 1 d . . .
H12A H 0.5341 0.5823 0.4603 0.028 Uiso 1 1 calc R . .
H12B H 0.4913 0.6415 0.4297 0.028 Uiso 1 1 calc R . .
C11 C 0.45793(15) 0.5123(3) 0.45015(12) 0.0211(9) Uani 1 1 d . . .
H11A H 0.4393 0.5489 0.4695 0.025 Uiso 1 1 calc R . .
H11B H 0.4720 0.4488 0.4619 0.025 Uiso 1 1 calc R . .
C57 C 0.33889(14) 0.2571(3) 0.32019(12) 0.0176(9) Uani 1 1 d . . .
C62 C 0.34070(16) 0.2171(3) 0.35732(13) 0.0249(10) Uani 1 1 d . . .
H62A H 0.3648 0.2449 0.3783 0.030 Uiso 1 1 calc R . .
C61 C 0.30784(18) 0.1371(4) 0.36427(15) 0.0350(12) Uani 1 1 d . . .
H61A H 0.3093 0.1108 0.3899 0.042 Uiso 1 1 calc R . .
C60 C 0.27300(16) 0.0956(3) 0.33397(15) 0.0343(12) Uani 1 1 d . . .
H60A H 0.2506 0.0406 0.3387 0.041 Uiso 1 1 calc R . .
C59 C 0.27072(16) 0.1341(3) 0.29695(15) 0.0302(11) Uani 1 1 d . . .
H59A H 0.2469 0.1052 0.2761 0.036 Uiso 1 1 calc R . .
C58 C 0.30299(15) 0.2150(3) 0.28981(14) 0.0229(9) Uani 1 1 d . . .
H58A H 0.3007 0.2419 0.2642 0.027 Uiso 1 1 calc R . .
C51 C 0.32262(15) 0.4571(3) 0.29821(12) 0.0198(9) Uani 1 1 d . . .
C56 C 0.27363(16) 0.4492(3) 0.31448(13) 0.0244(10) Uani 1 1 d . . .
H56A H 0.2694 0.3969 0.3323 0.029 Uiso 1 1 calc R . .
C55 C 0.23098(17) 0.5164(3) 0.30507(14) 0.0310(11) Uani 1 1 d . . .
H55A H 0.1982 0.5101 0.3166 0.037 Uiso 1 1 calc R . .
C54 C 0.23632(17) 0.5924(4) 0.27884(14) 0.0350(11) Uani 1 1 d . . .
H54A H 0.2070 0.6375 0.2719 0.042 Uiso 1 1 calc R . .
C53 C 0.28443(18) 0.6022(3) 0.26290(14) 0.0331(11) Uani 1 1 d . . .
H53A H 0.2884 0.6549 0.2452 0.040 Uiso 1 1 calc R . .
C52 C 0.32768(17) 0.5352(3) 0.27252(13) 0.0261(10) Uani 1 1 d . . .
H52A H 0.3607 0.5431 0.2614 0.031 Uiso 1 1 calc R . .
C39 C 0.54329(14) 0.4028(3) 0.26828(11) 0.0170(9) Uani 1 1 d . . .
C40 C 0.55151(17) 0.3597(3) 0.23263(13) 0.0255(10) Uani 1 1 d . . .
H40A H 0.5357 0.2969 0.2253 0.031 Uiso 1 1 calc R . .
C41 C 0.58278(17) 0.4087(3) 0.20798(13) 0.0282(10) Uani 1 1 d . . .
H41A H 0.5870 0.3805 0.1834 0.034 Uiso 1 1 calc R . .
C42 C 0.60774(17) 0.4980(3) 0.21886(14) 0.0291(11) Uani 1 1 d . . .
H42A H 0.6299 0.5305 0.2022 0.035 Uiso 1 1 calc R . .
C43 C 0.60014(16) 0.5399(3) 0.25436(14) 0.0258(10) Uani 1 1 d . . .
H43A H 0.6172 0.6014 0.2620 0.031 Uiso 1 1 calc R . .
C44 C 0.56804(15) 0.4933(3) 0.27891(13) 0.0184(9) Uani 1 1 d . . .
H44A H 0.5629 0.5232 0.3031 0.022 Uiso 1 1 calc R . .
C45 C 0.55597(16) 0.2316(3) 0.31178(12) 0.0186(9) Uani 1 1 d . . .
C50 C 0.61224(17) 0.2525(3) 0.32077(13) 0.0287(11) Uani 1 1 d . . .
H50A H 0.6243 0.3196 0.3228 0.034 Uiso 1 1 calc R . .
C49 C 0.65027(19) 0.1762(4) 0.32663(15) 0.0389(13) Uani 1 1 d . . .
H49A H 0.6881 0.1911 0.3330 0.047 Uiso 1 1 calc R . .
C48 C 0.6332(2) 0.0790(4) 0.32316(15) 0.0436(13) Uani 1 1 d . . .
H48A H 0.6592 0.0268 0.3272 0.052 Uiso 1 1 calc R . .
C47 C 0.5785(2) 0.0573(3) 0.31386(14) 0.0350(12) Uani 1 1 d . . .
H47A H 0.5669 -0.0100 0.3112 0.042 Uiso 1 1 calc R . .
C46 C 0.54042(18) 0.1324(3) 0.30836(13) 0.0270(10) Uani 1 1 d . . .
H46A H 0.5027 0.1162 0.3021 0.032 Uiso 1 1 calc R . .
C33 C 0.56571(15) 0.6242(3) 0.37613(12) 0.0179(9) Uani 1 1 d . . .
C38 C 0.53471(18) 0.7111(3) 0.36822(14) 0.0288(11) Uani 1 1 d . . .
H38A H 0.4978 0.7136 0.3735 0.035 Uiso 1 1 calc R . .
C37 C 0.5581(2) 0.7931(3) 0.35278(16) 0.0391(13) Uani 1 1 d . . .
H37A H 0.5369 0.8517 0.3476 0.047 Uiso 1 1 calc R . .
C36 C 0.6114(2) 0.7914(4) 0.34480(16) 0.0392(13) Uani 1 1 d . . .
H36A H 0.6272 0.8488 0.3347 0.047 Uiso 1 1 calc R . .
C35 C 0.64181(18) 0.7060(3) 0.35154(15) 0.0345(12) Uani 1 1 d . . .
H35A H 0.6784 0.7037 0.3457 0.041 Uiso 1 1 calc R . .
C34 C 0.61894(17) 0.6230(3) 0.36693(13) 0.0258(10) Uani 1 1 d . . .
H34A H 0.6402 0.5642 0.3713 0.031 Uiso 1 1 calc R . .
C27 C 0.59827(15) 0.4592(3) 0.42211(12) 0.0187(9) Uani 1 1 d . . .
C28 C 0.61985(16) 0.3763(3) 0.40606(14) 0.0281(10) Uani 1 1 d . . .
H28A H 0.5994 0.3444 0.3843 0.034 Uiso 1 1 calc R . .
C29 C 0.67096(17) 0.3390(4) 0.42123(16) 0.0394(13) Uani 1 1 d . . .
H29A H 0.6862 0.2845 0.4089 0.047 Uiso 1 1 calc R . .
C30 C 0.69948(18) 0.3814(4) 0.45427(15) 0.0379(13) Uani 1 1 d . . .
H30A H 0.7340 0.3553 0.4651 0.045 Uiso 1 1 calc R . .
C31 C 0.67778(17) 0.4612(4) 0.47137(14) 0.0320(11) Uani 1 1 d . . .
H31A H 0.6969 0.4894 0.4945 0.038 Uiso 1 1 calc R . .
C32 C 0.62810(16) 0.5008(3) 0.45512(13) 0.0247(10) Uani 1 1 d . . .
H32A H 0.6141 0.5577 0.4667 0.030 Uiso 1 1 calc R . .
C15 C 0.35531(14) 0.4182(3) 0.42508(11) 0.0197(8) Uani 1 1 d . . .
C16 C 0.36869(17) 0.3385(3) 0.45043(13) 0.0277(10) Uani 1 1 d . . .
H16A H 0.4060 0.3225 0.4586 0.033 Uiso 1 1 calc R . .
C17 C 0.3278(2) 0.2833(4) 0.46365(15) 0.0386(12) Uani 1 1 d . . .
H17A H 0.3371 0.2299 0.4813 0.046 Uiso 1 1 calc R . .
C18 C 0.2732(2) 0.3049(4) 0.45142(16) 0.0432(14) Uani 1 1 d . . .
H18A H 0.2452 0.2660 0.4604 0.052 Uiso 1 1 calc R . .
C19 C 0.25963(18) 0.3823(4) 0.42640(15) 0.0352(12) Uani 1 1 d . . .
H19A H 0.2221 0.3969 0.4180 0.042 Uiso 1 1 calc R . .
C20 C 0.30019(16) 0.4395(3) 0.41328(13) 0.0247(10) Uani 1 1 d . . .
H20A H 0.2904 0.4937 0.3961 0.030 Uiso 1 1 calc R . .
C21 C 0.37512(15) 0.6108(3) 0.39930(13) 0.0206(10) Uani 1 1 d . . .
C22 C 0.35709(17) 0.6595(3) 0.43116(14) 0.0279(10) Uani 1 1 d . . .
H22A H 0.3634 0.6301 0.4564 0.033 Uiso 1 1 calc R . .
C23 C 0.33034(19) 0.7494(4) 0.42642(16) 0.0369(12) Uani 1 1 d . . .
H23A H 0.3190 0.7823 0.4483 0.044 Uiso 1 1 calc R . .
C24 C 0.31994(19) 0.7920(4) 0.38963(18) 0.0415(13) Uani 1 1 d . . .
H24A H 0.3013 0.8538 0.3864 0.050 Uiso 1 1 calc R . .
C25 C 0.33651(18) 0.7452(4) 0.35775(16) 0.0368(12) Uani 1 1 d . . .
H25A H 0.3289 0.7743 0.3326 0.044 Uiso 1 1 calc R . .
C26 C 0.36446(16) 0.6551(3) 0.36255(14) 0.0265(10) Uani 1 1 d . . .
H26A H 0.3764 0.6235 0.3406 0.032 Uiso 1 1 calc R . .
C63 C 0.45834(14) 0.5448(3) 0.31704(12) 0.0171(9) Uani 1 1 d . . .
C64 C 0.2500 -0.1258(16) 0.5000 0.35(4) Uani 1 2 d SD . .
H64 H 0.2500 -0.1964 0.5000 0.421 Uiso 1 2 calc SR . .
C65 C 0.2746(6) -0.0825(8) 0.5315(5) 0.237(13) Uani 1 1 d D B .
H65 H 0.2913 -0.1207 0.5529 0.285 Uiso 1 1 calc R . .
C66 C 0.2755(4) 0.0160(8) 0.5328(4) 0.149(5) Uani 1 1 d D . .
H66 H 0.2965 0.0343 0.5565 0.179 Uiso 0.50 1 d P A 2
C67 C 0.2500 0.0658(7) 0.5000 0.095(4) Uani 1 2 d SD . .
H67 H 0.2500 0.1363 0.5000 0.115 Uiso 1 2 calc SR . .
C68 C 0.3039(9) 0.0643(18) 0.5670(5) 0.207(17) Uani 0.50 1 d PD B 1
H68A H 0.2992 0.1363 0.5645 0.311 Uiso 0.50 1 calc PR B 1
H68B H 0.3430 0.0479 0.5695 0.311 Uiso 0.50 1 calc PR B 1
H68C H 0.2886 0.0412 0.5903 0.311 Uiso 0.50 1 calc PR B 1
Ge Ge 0.481277(16) 0.27706(3) 0.394625(12) 0.01635(10) Uani 1 1 d . . .
N N 0.45624(14) 0.6094(3) 0.29598(11) 0.0270(9) Uani 1 1 d . . .
P4 P 0.37934(4) 0.36920(8) 0.31165(3) 0.0156(2) Uani 1 1 d . . .
P3 P 0.50641(4) 0.33492(7) 0.30344(3) 0.0145(2) Uani 1 1 d . . .
P2 P 0.53439(4) 0.51408(7) 0.39646(3) 0.0157(2) Uani 1 1 d . . .
P1 P 0.40974(4) 0.48899(8) 0.40528(3) 0.0163(2) Uani 1 1 d . . .
W W 0.462409(6) 0.417626(11) 0.356472(5) 0.01232(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 C5 1.511(6) . ?
C1 C2 1.512(6) . ?
C1 C6 1.536(6) . ?
C1 Ge 2.008(4) . ?
C5 C4 1.355(6) . ?
C5 C10 1.507(6) . ?
C4 C3 1.463(6) . ?
C4 C9 1.507(6) . ?
C3 C2 1.356(6) . ?
C3 C8 1.491(6) . ?
C2 C7 1.503(6) . ?
C6 H6C 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6A 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10A 0.9800 . ?
C9 H9C 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9A 0.9800 . ?
C8 H8C 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8A 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C14 C13 1.530(5) . ?
C14 P4 1.846(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C13 P3 1.853(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C12 C11 1.536(5) . ?
C12 P2 1.870(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C11 P1 1.850(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C57 C62 1.387(6) . ?
C57 C58 1.400(6) . ?
C57 P4 1.853(4) . ?
C62 C61 1.387(6) . ?
C62 H62A 0.9500 . ?
C61 C60 1.381(6) . ?
C61 H61A 0.9500 . ?
C60 C59 1.374(7) . ?
C60 H60A 0.9500 . ?
C59 C58 1.389(6) . ?
C59 H59A 0.9500 . ?
C58 H58A 0.9500 . ?
C51 C52 1.392(6) . ?
C51 C56 1.399(6) . ?
C51 P4 1.842(4) . ?
C56 C55 1.391(6) . ?
C56 H56A 0.9500 . ?
C55 C54 1.385(7) . ?
C55 H55A 0.9500 . ?
C54 C53 1.376(6) . ?
C54 H54A 0.9500 . ?
C53 C52 1.402(6) . ?
C53 H53A 0.9500 . ?
C52 H52A 0.9500 . ?
C39 C44 1.390(5) . ?
C39 C40 1.400(6) . ?
C39 P3 1.850(4) . ?
C40 C41 1.388(6) . ?
C40 H40A 0.9500 . ?
C41 C42 1.380(6) . ?
C41 H41A 0.9500 . ?
C42 C43 1.384(6) . ?
C42 H42A 0.9500 . ?
C43 C44 1.383(6) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C46 1.390(6) . ?
C45 C50 1.407(6) . ?
C45 P3 1.847(4) . ?
C50 C49 1.387(6) . ?
C50 H50A 0.9500 . ?
C49 C48 1.375(7) . ?
C49 H49A 0.9500 . ?
C48 C47 1.372(7) . ?
C48 H48A 0.9500 . ?
C47 C46 1.375(6) . ?
C47 H47A 0.9500 . ?
C46 H46A 0.9500 . ?
C33 C34 1.388(5) . ?
C33 C38 1.403(6) . ?
C33 P2 1.852(4) . ?
C38 C37 1.385(6) . ?
C38 H38A 0.9500 . ?
C37 C36 1.377(7) . ?
C37 H37A 0.9500 . ?
C36 C35 1.375(7) . ?
C36 H36A 0.9500 . ?
C35 C34 1.388(6) . ?
C35 H35A 0.9500 . ?
C34 H34A 0.9500 . ?
C27 C28 1.383(6) . ?
C27 C32 1.390(6) . ?
C27 P2 1.853(4) . ?
C28 C29 1.391(6) . ?
C28 H28A 0.9500 . ?
C29 C30 1.383(7) . ?
C29 H29A 0.9500 . ?
C30 C31 1.367(7) . ?
C30 H30A 0.9500 . ?
C31 C32 1.384(6) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C15 C20 1.394(5) . ?
C15 C16 1.396(6) . ?
C15 P1 1.847(4) . ?
C16 C17 1.376(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.385(7) . ?
C17 H17A 0.9500 . ?
C18 C19 1.367(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.383(6) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
C21 C26 1.396(6) . ?
C21 C22 1.403(6) . ?
C21 P1 1.847(4) . ?
C22 C23 1.377(6) . ?
C22 H22A 0.9500 . ?
C23 C24 1.387(7) . ?
C23 H23A 0.9500 . ?
C24 C25 1.376(7) . ?
C24 H24A 0.9500 . ?
C25 C26 1.394(6) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C63 N 1.130(5) . ?
C63 W 2.183(5) . ?
C64 C65 1.310(16) . ?
C64 C65 1.310(16) 2_556 ?
C64 H64 0.9500 . ?
C65 C66 1.328(13) . ?
C65 H65 0.9500 . ?
C66 C67 1.392(11) . ?
C66 C68 1.447(16) . ?
C66 H66 0.942(15) . ?
C67 C66 1.392(11) 2_556 ?
C67 H67 0.9500 . ?
C68 H66 0.56(2) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
Ge W 2.3184(6) . ?
P4 W 2.4832(11) . ?
P3 W 2.5083(11) . ?
P2 W 2.4672(11) . ?
P1 W 2.4539(11) . ?
