#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008173.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_2008173 _journal_name_full 'Acta Crystallographica' _journal_year 1999 _journal_volume C55 _publ_section_title ; Tricarbonyl{1,1,1-tris(dimethylphosphinomethyl)ethane}chromium(0), -molybdenum(0) and -tungsten(0) ; loop_ _publ_author_name 'Suzuki, Takayoshi' 'Imamura, Takeshi' 'Kaizaki, Sumio' 'Tricarbonyl[1,1,1-tris(dimethylphosphinomethyl)ethane]chromium(0)' _chemical_formula_moiety 'C14 H27 Cr O3 P3' _chemical_formula_sum 'C14 H27 Cr O3 P3' _chemical_formula_iupac '[Cr (C11 H27 P3) (C O)3]' _chemical_formula_weight 388.28 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' _cell_length_a 15.684(3) _cell_length_b 16.170(3) _cell_length_c 17.222(3) _cell_angle_alpha 90 _cell_angle_beta 116.750(10) _cell_angle_gamma 90 _cell_volume 3900.0(10) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _exptl_crystal_density_diffrn 1.322 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cr1 0.22975(4) 0.21310(4) 0.01139(4) 0.0390(2) Uani . 1.00 . . Cr Cr2 0.29065(4) 0.70429(4) -0.00300(4) 0.0407(2) Uani . 1.00 . . Cr P11 0.30323(9) 0.11831(7) -0.04135(7) 0.0533(3) Uani . 1.00 . . P P12 0.13001(8) 0.74172(7) -0.07834(9) 0.0549(4) Uani . 1.00 . . P P21 0.22365(7) 0.10587(7) 0.09892(7) 0.0447(3) Uani . 1.00 . . P P22 0.23570(8) 0.60028(7) 0.05727(7) 0.0481(3) Uani . 1.00 . . P P31 0.38471(7) 0.23529(6) 0.12211(7) 0.0418(3) Uani . 1.00 . . P P32 0.25682(7) 0.61087(7) -0.11649(7) 0.0454(3) Uani . 1.00 . . P O11 0.1484(3) 0.3397(2) 0.0856(3) 0.097(2) Uani . 1.00 . . O O12 0.4916(2) 0.6431(2) 0.0947(2) 0.0860(10) Uani . 1.00 . . O O21 0.2465(4) 0.3439(2) -0.1030(3) 0.117(2) Uani . 1.00 . . O O22 0.3509(3) 0.8377(2) -0.0885(3) 0.0920(10) Uani . 1.00 . . O O31 0.0333(3) 0.1752(3) -0.1261(2) 0.118(2) Uani . 1.00 . . O O32 0.3279(3) 0.8215(3) 0.1432(3) 0.106(2) Uani . 1.00 . . O C11 0.4911(3) -0.0074(3) 0.1840(4) 0.077(2) Uani . 1.00 . . C C12 -0.0080(3) 0.5123(3) -0.1559(3) 0.0660(10) Uani . 1.00 . . C C21 0.4149(3) 0.0580(2) 0.1327(3) 0.0480(10) Uani . 1.00 . . C C22 0.0792(3) 0.5695(3) -0.1112(2) 0.0440(10) Uani . 1.00 . . C C31 0.3814(3) 0.0412(3) 0.0371(3) 0.071(2) Uani . 1.00 . . C C32 0.0463(3) 0.6584(3) -0.1410(3) 0.0540(10) Uani . 1.00 . . C C41 0.3346(3) 0.0483(3) 0.1596(3) 0.073(2) Uani . 1.00 . . C C42 0.1145(3) 0.5604(3) -0.0126(3) 0.0500(10) Uani . 1.00 . . C C51 0.4617(3) 0.1433(3) 0.1597(3) 0.0550(10) Uani . 1.00 . . C C52 0.1546(3) 0.5410(3) -0.1397(3) 0.0520(10) Uani . 1.00 . . C C61 0.3850(6) 0.1600(4) -0.0807(5) 0.127(3) Uani . 1.00 . . C C62 0.0958(4) 0.8240(3) -0.1594(4) 0.102(2) Uani . 1.00 . . C C71 0.2304(5) 0.0528(4) -0.1323(4) 0.121(2) Uani . 1.00 . . C C72 0.0755(4) 0.7814(3) -0.0111(4) 0.087(2) Uani . 1.00 . . C C81 0.1387(4) 0.0232(4) 0.0452(4) 0.109(2) Uani . 1.00 . . C C82 0.2302(4) 0.6209(4) 0.1596(3) 0.089(2) Uani . 1.00 . . C C91 0.1906(5) 0.1299(4) 0.1851(4) 0.107(3) Uani . 1.00 . . C C92 0.3042(4) 0.5041(3) 0.0867(3) 0.082(2) Uani . 1.00 . . C C101 0.3952(4) 0.2770(3) 0.2246(3) 0.076(2) Uani . 1.00 . . C C102 0.3499(3) 0.5377(3) -0.1074(3) 0.071(2) Uani . 1.00 . . C C111 0.4635(4) 0.3082(3) 0.1054(4) 0.089(2) Uani . 1.00 . . C C112 0.2269(4) 0.6538(4) -0.2235(3) 0.080(2) Uani . 1.00 . . C C211 0.1803(3) 0.2892(3) 0.0580(3) 0.0570(10) Uani . 1.00 . . C C212 0.4139(3) 0.6661(3) 0.0560(3) 0.0530(10) Uani . 1.00 . . C C221 0.2413(4) 0.2927(3) -0.0579(3) 0.068(2) Uani . 1.00 . . C C222 0.3272(3) 0.7853(3) -0.0563(3) 0.0580(10) Uani . 1.00 . . C C231 0.1099(3) 0.1888(3) -0.0731(3) 0.069(2) Uani . 1.00 . . C C232 0.3114(3) 0.7759(3) 0.0857(3) 0.066(2) Uani . 1.00 . . C H1 0.4633 -0.0629 0.1713 0.0942 Uiso . 1.00 . . H H2 0.5149 -0.0003 0.2464 0.0942 Uiso . 1.00 . . H H3 0.5438 -0.0069 0.1715 0.0942 Uiso . 1.00 . . H H4 0.4375 0.0359 0.0279 0.0916 Uiso . 1.00 . . H H5 0.3488 -0.0102 0.0238 0.0916 Uiso . 1.00 . . H H6 0.3188 -0.0079 0.1593 0.0924 Uiso . 1.00 . . H H7 0.3594 0.0675 0.2208 0.0924 Uiso . 1.00 . . H H8 0.5107 0.1477 0.1405 0.0663 Uiso . 1.00 . . H H9 0.4947 0.1446 0.2230 0.0663 Uiso . 1.00 . . H H10 0.3559 0.1949 -0.1282 0.1406 Uiso . 1.00 . . H H11 0.4192 0.1168 -0.0929 0.1406 Uiso . 1.00 . . H H12 0.4361 0.1931 -0.0332 0.1406 Uiso . 1.00 . . H H13 0.1885 0.0199 -0.1185 0.1403 Uiso . 1.00 . . H H14 0.1911 0.0866 -0.1822 0.1403 Uiso . 1.00 . . H H15 0.2686 0.0181 -0.1478 0.1403 Uiso . 1.00 . . H H16 0.1417 -0.0180 0.0862 0.1263 Uiso . 1.00 . . H H17 0.0760 0.0432 0.0150 0.1263 Uiso . 1.00 . . H H18 0.1552 -0.0045 0.0033 0.1263 Uiso . 1.00 . . H H19 0.2061 0.1849 0.2045 0.1226 Uiso . 1.00 . . H H20 0.1213 0.1235 0.1629 0.1226 Uiso . 1.00 . . H H21 0.2199 0.0927 0.2325 0.1226 Uiso . 1.00 . . H H22 0.3638 0.2413 0.2486 0.0929 Uiso . 1.00 . . H H23 0.3645 0.3304 0.2155 0.0929 Uiso . 1.00 . . H H24 0.4598 0.2831 0.2662 0.0929 Uiso . 1.00 . . H H25 0.5233 0.3121 0.1563 0.1076 Uiso . 1.00 . . H H26 0.4350 0.3636 0.0953 0.1076 Uiso . 1.00 . . H H27 0.4731 0.2940 0.0573 0.1076 Uiso . 1.00 . . H H28 -0.0640 0.5353 -0.1436 0.0740 Uiso . 1.00 . . H H29 0.0018 0.4566 -0.1515 0.0740 Uiso . 1.00 . . H H30 -0.0318 0.5141 -0.2205 0.0740 Uiso . 1.00 . . H H31 0.0282 0.6711 -0.2093 0.0740 Uiso . 1.00 . . H H32 -0.0210 0.6733 -0.1479 0.0740 Uiso . 1.00 . . H H33 0.0582 0.5839 0.0059 0.0740 Uiso . 1.00 . . H H34 0.1059 0.4935 -0.0130 0.0740 Uiso . 1.00 . . H H35 0.1224 0.5364 -0.2037 0.0740 Uiso . 1.00 . . H H36 0.1659 0.4797 -0.1245 0.0740 Uiso . 1.00 . . H H37 0.0301 0.8357 -0.1832 0.1154 Uiso . 1.00 . . H H38 0.1307 0.8745 -0.1323 0.1154 Uiso . 1.00 . . H H39 0.1125 0.8099 -0.2046 0.1154 Uiso . 1.00 . . H H40 0.0184 0.8106 -0.0427 0.1033 Uiso . 1.00 . . H H41 0.1199 0.8203 0.0339 0.1033 Uiso . 1.00 . . H H42 0.0643 0.7381 0.0219 0.1033 Uiso . 1.00 . . H H43 0.1823 0.6631 0.1457 0.0740 Uiso . 1.00 . . H H44 0.1909 0.5683 0.1696 0.0740 Uiso . 1.00 . . H H45 0.2940 0.6210 0.2098 0.0740 Uiso . 1.00 . . H H46 0.2857 0.4695 0.1220 0.0995 Uiso . 1.00 . . H H47 0.3710 0.5139 0.1175 0.0995 Uiso . 1.00 . . H H48 0.2928 0.4723 0.0350 0.0995 Uiso . 1.00 . . H H49 0.3575 0.4952 -0.0656 0.0844 Uiso . 1.00 . . H H50 0.4100 0.5650 -0.0887 0.0844 Uiso . 1.00 . . H H51 0.3340 0.5115 -0.1619 0.0844 Uiso . 1.00 . . H H52 0.2101 0.6107 -0.2661 0.0950 Uiso . 1.00 . . H H53 0.1694 0.6887 -0.2422 0.0950 Uiso . 1.00 . . H H54 0.2757 0.6862 -0.2239 0.0950 Uiso . 1.00 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr1 0.0422(3) 0.0379(3) 0.0362(3) 0.0072(3) 0.0170(3) 0.0077(3) Cr2 0.0412(3) 0.0370(3) 0.0511(4) -0.0074(3) 0.0272(3) -0.0075(3) P11 0.0738(8) 0.0515(7) 0.0383(6) 0.0050(6) 0.0285(6) -0.0049(5) P12 0.0488(7) 0.0407(6) 0.0839(9) 0.0054(5) 0.0376(6) 0.0080(6) P21 0.0391(6) 0.0466(6) 0.0499(6) -0.0017(5) 0.0213(5) 0.0106(5) P22 0.0521(6) 0.0520(7) 0.0356(5) -0.0156(5) 0.0156(5) -0.0014(5) P31 0.0413(6) 0.0350(5) 0.0513(6) -0.0029(4) 0.0229(5) -0.0052(5) P32 0.0441(6) 0.0517(7) 0.0470(6) -0.0041(5) 0.0264(5) -0.0089(5) O11 0.102(3) 0.060(2) 0.169(4) 0.006(2) 0.097(3) -0.014(3) O12 0.045(2) 0.109(3) 0.084(3) 0.002(2) 0.012(2) -0.005(2) O21 0.193(5) 0.072(3) 0.112(3) 0.024(3) 0.091(3) 0.048(3) O22 0.094(3) 0.069(2) 0.143(4) -0.009(2) 0.079(3) 0.026(2) O31 0.057(2) 0.183(5) 0.071(3) 0.000(3) -0.010(2) -0.009(3) O32 0.123(3) 0.102(3) 0.126(3) -0.052(3) 0.086(3) -0.075(3) C11 0.062(3) 0.056(3) 0.090(4) 0.023(2) 0.016(3) 0.011(3) C12 0.048(3) 0.076(3) 0.064(3) -0.023(2) 0.016(2) -0.016(3) C21 0.037(2) 0.042(2) 0.057(3) 0.007(2) 0.014(2) 0.005(2) C22 0.040(2) 0.050(2) 0.040(2) -0.010(2) 0.017(2) -0.004(2) C31 0.073(3) 0.066(3) 0.062(3) 0.024(3) 0.019(3) -0.014(3) C32 0.037(2) 0.065(3) 0.055(3) 0.003(2) 0.017(2) 0.010(2) C41 0.059(3) 0.067(3) 0.090(4) 0.014(3) 0.031(3) 0.045(3) C42 0.046(2) 0.052(2) 0.049(2) -0.020(2) 0.020(2) 0.000(2) C51 0.043(2) 0.053(3) 0.058(3) 0.003(2) 0.013(2) -0.004(2) C52 0.050(2) 0.055(3) 0.048(2) -0.014(2) 0.019(2) -0.016(2) C61 0.199(8) 0.105(5) 0.166(7) 0.005(5) 0.159(6) -0.003(5) C62 0.084(4) 0.066(4) 0.155(6) 0.024(3) 0.054(4) 0.052(4) C71 0.133(6) 0.117(5) 0.065(4) 0.007(5) 0.003(4) -0.050(4) C72 0.068(3) 0.070(4) 0.144(5) 0.003(3) 0.066(4) -0.024(4) C81 0.086(4) 0.081(4) 0.118(5) -0.045(3) 0.010(4) 0.019(4) C82 0.092(4) 0.131(5) 0.046(3) -0.041(4) 0.035(3) -0.012(3) C91 0.153(6) 0.115(5) 0.105(5) 0.019(4) 0.105(5) 0.035(4) C92 0.073(3) 0.065(3) 0.076(4) -0.001(3) 0.004(3) 0.023(3) C101 0.077(3) 0.081(4) 0.058(3) 0.001(3) 0.019(3) -0.030(3) C102 0.059(3) 0.070(3) 0.097(4) -0.001(3) 0.046(3) -0.032(3) C111 0.070(3) 0.077(4) 0.128(5) -0.018(3) 0.053(4) 0.012(4) C112 0.086(4) 0.116(5) 0.051(3) -0.016(3) 0.042(3) 0.002(3) C211 0.056(3) 0.042(2) 0.083(3) 0.005(2) 0.041(3) 0.003(2) C212 0.046(2) 0.058(3) 0.054(3) -0.012(2) 0.022(2) -0.013(2) C221 0.098(4) 0.050(3) 0.065(3) 0.019(3) 0.045(3) 0.022(2) C222 0.055(3) 0.051(3) 0.086(3) -0.001(2) 0.047(3) 0.000(2) C231 0.056(3) 0.084(4) 0.053(3) 0.010(3) 0.012(2) 0.009(3) C232 0.069(3) 0.061(3) 0.086(4) -0.023(2) 0.052(3) -0.026(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cr1 P11 . . 2.3330(10) yes Cr1 P21 . . 2.3280(10) yes Cr1 P31 . . 2.3450(10) yes Cr1 C211 . . 1.821(4) yes Cr1 C221 . . 1.818(5) yes Cr1 C231 . . 1.829(5) yes Cr2 P12 . . 2.3360(10) yes Cr2 P22 . . 2.3350(10) yes Cr2 P32 . . 2.3350(10) yes Cr2 C212 . . 1.839(5) yes Cr2 C222 . . 1.833(4) yes Cr2 C232 . . 1.825(5) yes P11 C31 . . 1.842(5) no P11 C61 . . 1.827(6) no P11 C71 . . 1.808(5) no P12 C32 . . 1.852(4) no P12 C62 . . 1.825(5) no P12 C72 . . 1.837(5) no P21 C41 . . 1.830(4) no P21 C81 . . 1.819(5) no P21 C91 . . 1.821(5) no P22 C42 . . 1.849(4) no P22 C82 . . 1.833(5) no P22 C92 . . 1.827(5) no P31 C51 . . 1.840(4) no P31 C101 . . 1.827(5) no P31 C111 . . 1.822(5) no P32 C52 . . 1.852(4) no P32 C102 . . 1.831(4) no P32 C112 . . 1.822(5) no O11 C211 . . 1.166(5) yes O12 C212 . . 1.156(5) yes O21 C221 . . 1.165(5) yes O22 C222 . . 1.162(5) yes O31 C231 . . 1.157(5) yes O32 C232 . . 1.168(5) yes C11 C21 . . 1.541(6) no C12 C22 . . 1.539(5) no C21 C31 . . 1.510(6) no C21 C41 . . 1.534(6) no C21 C51 . . 1.533(6) no C22 C32 . . 1.536(6) no C22 C42 . . 1.538(5) no C22 C52 . . 1.541(5) no C11 H1 . . 0.979 no C11 H2 . . 0.972 no C11 H3 . . 0.942 no C12 H28 . . 1.058 no C12 H29 . . 0.912 no C12 H30 . . 1.002 no C31 H4 . . 0.966 no C31 H5 . . 0.949 no C32 H31 . . 1.098 no C32 H32 . . 1.037 no C41 H6 . . 0.941 no C41 H7 . . 0.995 no C42 H33 . . 1.130 no C42 H34 . . 1.090 no C51 H8 . . 0.966 no C51 H9 . . 0.975 no C52 H35 . . 0.987 no C52 H36 . . 1.019 no C61 H10 . . 0.927 no C61 H11 . . 0.961 no C61 H12 . . 1.004 no C62 H37 . . 0.941 no C62 H38 . . 0.978 no C62 H39 . . 0.954 no C71 H13 . . 0.956 no C71 H14 . . 0.968 no C71 H15 . . 0.943 no C72 H40 . . 0.939 no C72 H41 . . 0.997 no C72 H42 . . 0.967 no C81 H16 . . 0.957 no C81 H17 . . 0.939 no C81 H18 . . 0.978 no C82 H43 . . 0.962 no C82 H44 . . 1.109 no C82 H45 . . 0.986 no C91 H19 . . 0.942 no C91 H20 . . 0.982 no C91 H21 . . 0.949 no C92 H46 . . 0.962 no C92 H47 . . 0.951 no C92 H48 . . 0.972 no C101 H22 . . 0.965 no C101 H23 . . 0.966 no C101 H24 . . 0.947 no C102 H49 . . 0.964 no C102 H50 . . 0.956 no C102 H51 . . 0.954 no C111 H25 . . 0.956 no C111 H26 . . 0.981 no C111 H27 . . 0.935 no C112 H52 . . 0.960 no C112 H53 . . 0.987 no C112 H54 . . 0.930 no