#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/7/7051276.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_7051276 _journal_name_full 'New Journal of Chemistry' _journal_year 2000 _publ_section_title ; Oxidative Addition of Iodine, Iodomethane and Iodobenzene to the Rhodium Phosphino Enolate Complex (Rh(Ph2PCH...C(...O)Ph)(CO)(PPh3)) and Carbon Monoxide Insertion into the resulting Rh-Carbon Bond of (Rh(Ph2PCH...C(...O)Ph)Me(I)(CO)(PPh3)). ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _publ_author_name 'Braunstein Pierre' 'Fischer Jean' 'Chauvin Yves' 'Olivier Helene' 'Strohmann Carsten' 'Toronto Dawn V.' _chemical_formula_moiety 'C40 H34 I O2 P2 Rh' _chemical_formula_sum 'C40 H34 I O2 P2 Rh' _chemical_formula_weight 838.47 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.054(3) _cell_length_b 24.130(3) _cell_length_c 12.213(3) _cell_angle_alpha 90 _cell_angle_beta 92.25(2) _cell_angle_gamma 90 _cell_volume 3549(2) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _exptl_crystal_density_diffrn 1.57 _diffrn_ambient_temperature 294 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_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RH 0.06662(3) 0.10259(2) 0.26465(3) 0.0355(2) Uani ? ? Rh O1 0.0651(3) 0.1176(2) 0.4322(2) 0.045(2) Uani ? ? O C1 -0.0298(4) 0.1314(2) 0.4742(4) 0.044(3) Uani ? ? C C2 -0.1278(4) 0.1339(3) 0.4141(4) 0.049(3) Uani ? ? C C3 -0.0237(4) 0.1433(2) 0.5940(4) 0.046(3) Uani ? ? C C4 0.0513(5) 0.1154(2) 0.6622(4) 0.053(3) Uani ? ? C C5 0.0547(6) 0.1255(3) 0.7737(5) 0.066(4) Uani ? ? C C6 -0.0150(6) 0.1649(3) 0.8194(5) 0.070(4) Uani ? ? C C7 -0.0877(5) 0.1928(3) 0.7505(4) 0.066(4) Uani ? ? C C8 -0.0935(5) 0.1827(3) 0.6392(4) 0.059(3) Uani ? ? C P1 -0.1229(1) 0.11630(6) 0.2761(1) 0.0426(7) Uani ? ? P C9 -0.1940(4) 0.1682(2) 0.1917(4) 0.045(3) Uani ? ? C C10 -0.2604(6) 0.2074(3) 0.2382(5) 0.077(4) Uani ? ? C C11 -0.3238(7) 0.2427(3) 0.1736(6) 0.103(5) Uani ? ? C C12 -0.3173(5) 0.2424(3) 0.0616(5) 0.063(3) Uani ? ? C C13 -0.2483(5) 0.2054(3) 0.0149(5) 0.063(3) Uani ? ? C C14 -0.1865(5) 0.1691(3) 0.0797(5) 0.064(3) Uani ? ? C C15 -0.2126(4) 0.0560(2) 0.2495(4) 0.043(2) Uani ? ? C C16 -0.2250(6) 0.0314(3) 0.1473(5) 0.071(4) Uani ? ? C C17 -0.2964(6) -0.0127(3) 0.1295(5) 0.079(4) Uani ? ? C C18 -0.3595(5) -0.0314(3) 0.2122(6) 0.073(4) Uani ? ? C C19 -0.3485(6) -0.0077(3) 0.3121(5) 0.088(4) Uani ? ? C C20 -0.2763(5) 0.0361(3) 0.3337(5) 0.070(4) Uani ? ? C C21 0.0378(5) 0.0203(2) 0.3128(5) 0.055(3) Uani ? ? C C22 0.0560(4) 0.0825(2) 0.1206(4) 0.047(3) Uani ? ? C O2 0.0474(4) 0.0672(2) 0.0339(3) 0.070(3) Uani ? ? O P2 0.2655(1) 0.08963(5) 0.2643(1) 0.0393(6) Uani ? ? P C23 0.3364(4) 0.1103(2) 0.1409(4) 0.045(3) Uani ? ? C C24 0.2906(5) 0.1476(3) 0.0655(5) 0.062(3) Uani ? ? C C25 0.3518(6) 0.1658(3) -0.0213(5) 0.074(4) Uani ? ? C C26 0.4546(6) 0.1473(3) -0.0350(5) 0.081(4) Uani ? ? C C27 0.4995(5) 0.1082(4) 0.0356(6) 0.081(4) Uani ? ? C C28 0.4423(5) 0.0901(3) 0.1233(6) 0.073(4) Uani ? ? C C29 0.3047(4) 0.0166(2) 0.2762(4) 0.041(2) Uani ? ? C C30 0.3559(5) -0.0064(2) 0.3684(5) 0.056(3) Uani ? ? C C31 0.3760(5) -0.0625(2) 0.3767(5) 0.061(3) Uani ? ? C C32 0.3450(5) -0.0967(3) 0.2911(6) 0.069(4) Uani ? ? C C33 0.2931(6) -0.0753(3) 0.1998(5) 0.067(4) Uani ? ? C C34 0.2728(5) -0.0191(2) 0.1895(5) 0.059(3) Uani ? ? C C35 0.3414(4) 0.1249(2) 0.3759(5) 0.051(3) Uani ? ? C C36 0.4277(6) 0.1605(3) 0.3591(6) 0.078(4) Uani ? ? C C37 0.4810(7) 0.1874(3) 0.4459(7) 0.108(5) Uani ? ? C C38 0.4460(7) 0.1802(3) 0.5490(6) 0.102(4) Uani ? ? C C39 0.3593(6) 0.1452(3) 0.5701(5) 0.097(4) Uani ? ? C C40 0.3069(5) 0.1172(3) 0.4802(5) 0.067(3) Uani ? ? C I 0.09763(3) 0.21656(1) 0.24651(3) 0.0514(2) Uani ? ? I H1 -0.1951 0.1447 0.4460 0.0667 Uiso calc C2 H H2 0.1007 0.0892 0.6324 0.0704 Uiso calc C4 H H3 0.1052 0.1054 0.8202 0.0887 Uiso calc C5 H H4 -0.0120 0.1721 0.8959 0.0942 Uiso calc C6 H H5 -0.1354 0.2198 0.7799 0.0873 Uiso calc C7 H H6 -0.1451 0.2025 0.5932 0.0766 Uiso calc C8 H H7 -0.2623 0.2102 0.3157 0.1009 Uiso calc C10 H H8 -0.3731 0.2677 0.2069 0.1351 Uiso calc C11 H H9 -0.3601 0.2675 0.0176 0.0828 Uiso calc C12 H H10 -0.2427 0.2046 -0.0624 0.0842 Uiso calc C13 H H11 -0.1373 0.1441 0.0461 0.0825 Uiso calc C14 H H12 -0.1835 0.0450 0.0885 0.0927 Uiso calc C16 H H13 -0.3018 -0.0299 0.0596 0.1049 Uiso calc C17 H H14 -0.4106 -0.0609 0.1995 0.0959 Uiso calc C18 H H15 -0.3916 -0.0214 0.3696 0.1166 Uiso calc C19 H H16 -0.2705 0.0523 0.4047 0.0924 Uiso calc C20 H H17 0.1061 0.0006 0.3167 0.0733 Uiso calc C21 H H18 0.0058 0.0201 0.3826 0.0733 Uiso calc C21 H H19 -0.0115 0.0030 0.2607 0.0733 Uiso calc C21 H H20 0.2170 0.1607 0.0733 0.0805 Uiso calc C24 H H21 0.3200 0.1918 -0.0718 0.0981 Uiso calc C25 H H22 0.4967 0.1611 -0.0932 0.1053 Uiso calc C26 H H23 0.5711 0.0936 0.0233 0.1113 Uiso calc C27 H H24 0.4750 0.0636 0.1723 0.1010 Uiso calc C28 H H25 0.3780 0.0170 0.4279 0.0725 Uiso calc C30 H H26 0.4110 -0.0775 0.4412 0.0806 Uiso calc C31 H H27 0.3597 -0.1353 0.2956 0.0939 Uiso calc C32 H H28 0.2703 -0.0994 0.1418 0.0929 Uiso calc C33 H H29 0.2377 -0.0047 0.1246 0.0774 Uiso calc C34 H H30 0.4511 0.1668 0.2867 0.1047 Uiso calc C36 H H31 0.5423 0.2111 0.4334 0.1557 Uiso calc C37 H H32 0.4820 0.1997 0.6079 0.1416 Uiso calc C38 H H33 0.3353 0.1399 0.6426 0.1304 Uiso calc C39 H H34 0.2469 0.0927 0.4924 0.0878 Uiso calc C40 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 _atom_site_aniso_type_symbol RH 0.0339(2) 0.0347(2) 0.0382(2) 0.0015(2) 0.0016(1) 0.0017(2) Rh O1 0.044(2) 0.055(2) 0.038(2) 0.002(2) 0.002(1) -0.001(2) O C1 0.055(3) 0.046(3) 0.033(2) -0.001(2) 0.001(2) 0.001(2) C C2 0.043(3) 0.073(4) 0.039(2) -0.001(3) 0.008(2) -0.005(2) C C3 0.053(3) 0.045(3) 0.041(2) -0.010(2) 0.004(2) -0.002(2) C C4 0.068(3) 0.046(3) 0.048(3) -0.000(3) 0.002(3) 0.005(2) C C5 0.090(4) 0.061(3) 0.053(3) -0.016(3) -0.002(3) 0.013(3) C C6 0.093(4) 0.080(4) 0.046(3) -0.022(4) 0.017(3) -0.013(3) C C7 0.079(4) 0.071(4) 0.052(3) -0.006(3) 0.017(3) -0.013(3) C C8 0.059(3) 0.065(4) 0.054(3) -0.006(3) 0.012(3) -0.007(3) C P1 0.0371(6) 0.0497(7) 0.0418(6) 0.0005(6) 0.0034(5) -0.0025(6) P C9 0.032(2) 0.052(3) 0.054(3) 0.001(2) -0.001(2) -0.001(2) C C10 0.092(4) 0.079(4) 0.063(3) 0.043(3) 0.014(3) -0.007(3) C C11 0.123(5) 0.107(5) 0.082(4) 0.069(4) 0.010(4) -0.012(4) C C12 0.061(3) 0.065(4) 0.063(3) 0.015(3) -0.011(3) 0.006(3) C C13 0.075(4) 0.071(4) 0.048(3) 0.011(3) -0.006(3) 0.016(3) C C14 0.059(3) 0.073(4) 0.059(3) 0.022(3) 0.016(3) 0.003(3) C C15 0.035(2) 0.049(3) 0.047(2) -0.000(2) 0.002(2) 0.003(2) C C16 0.081(4) 0.076(4) 0.058(3) -0.025(3) 0.012(3) -0.002(3) C C17 0.103(5) 0.072(4) 0.068(4) -0.031(4) 0.007(4) -0.018(3) C C18 0.062(3) 0.073(4) 0.085(4) -0.031(3) -0.005(3) -0.002(3) C C19 0.081(4) 0.117(5) 0.072(4) -0.058(3) 0.012(3) 0.001(4) C C20 0.062(3) 0.094(5) 0.057(3) -0.020(3) 0.008(3) 0.003(3) C C21 0.057(3) 0.041(3) 0.071(3) 0.002(3) 0.002(3) 0.006(3) C C22 0.042(3) 0.057(3) 0.044(2) 0.002(2) 0.005(2) -0.000(2) C O2 0.080(3) 0.100(3) 0.043(2) 0.006(3) 0.004(2) -0.014(2) O P2 0.0364(6) 0.0380(7) 0.0437(6) 0.0017(5) -0.0005(5) 0.0022(5) P C23 0.040(3) 0.045(3) 0.051(3) -0.005(2) 0.005(2) 0.001(2) C C24 0.063(3) 0.065(4) 0.058(3) 0.009(3) 0.012(3) 0.016(3) C C25 0.095(5) 0.074(4) 0.058(3) -0.002(4) 0.014(3) 0.012(3) C C26 0.074(4) 0.100(5) 0.071(4) -0.029(4) 0.028(3) 0.002(4) C C27 0.052(3) 0.119(6) 0.088(4) -0.007(4) 0.026(3) 0.014(4) C C28 0.042(3) 0.087(5) 0.105(5) 0.004(3) 0.015(3) 0.023(4) C C29 0.034(2) 0.038(2) 0.053(3) 0.001(2) 0.009(2) 0.003(2) C C30 0.053(3) 0.056(3) 0.058(3) 0.012(3) 0.004(2) 0.002(3) C C31 0.069(4) 0.045(3) 0.073(3) 0.015(3) 0.009(3) 0.009(3) C C32 0.070(4) 0.044(3) 0.104(4) 0.013(3) 0.027(3) 0.010(3) C C33 0.079(4) 0.041(3) 0.094(4) 0.002(3) 0.006(4) -0.020(3) C C34 0.067(3) 0.048(3) 0.064(3) 0.007(3) 0.001(3) -0.006(3) C C35 0.049(3) 0.042(3) 0.064(3) 0.011(2) -0.017(2) -0.004(3) C C36 0.094(5) 0.061(4) 0.084(4) -0.020(3) -0.031(4) 0.011(3) C C37 0.128(5) 0.059(4) 0.165(6) -0.023(4) -0.085(4) 0.012(5) C C38 0.136(5) 0.066(4) 0.118(4) 0.021(4) -0.083(3) -0.037(3) C C39 0.112(5) 0.106(5) 0.078(3) 0.054(4) -0.055(3) -0.045(3) C C40 0.057(3) 0.077(4) 0.067(3) 0.021(3) -0.018(3) -0.022(3) C I 0.0524(2) 0.0376(2) 0.0690(2) 0.0017(2) -0.0036(2) 0.0037(2) I loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RH O1 2.079(3) . . ? RH P1 2.318(1) . . ? RH C21 2.104(6) . . ? RH C22 1.824(5) . . ? RH P2 2.418(1) . . ? RH I 2.7854(5) . . ? O1 C1 1.314(6) . . ? C1 C2 1.368(7) . . ? C1 C3 1.490(7) . . ? C2 P1 1.741(5) . . ? C3 C4 1.381(8) . . ? C3 C8 1.397(8) . . ? C4 C5 1.383(8) . . ? C5 C6 1.40(1) . . ? C6 C7 1.37(1) . . ? C7 C8 1.380(8) . . ? P1 C9 1.816(6) . . ? P1 C15 1.834(6) . . ? C9 C10 1.376(8) . . ? C9 C14 1.375(8) . . ? C10 C11 1.37(1) . . ? C11 C12 1.373(9) . . ? C12 C13 1.360(9) . . ? C13 C14 1.379(8) . . ? C15 C16 1.386(8) . . ? C15 C20 1.393(8) . . ? C16 C17 1.379(9) . . ? C17 C18 1.364(9) . . ? C18 C19 1.35(1) . . ? C19 C20 1.388(9) . . ? C22 O2 1.123(6) . . ? P2 C23 1.830(5) . . ? P2 C29 1.829(5) . . ? P2 C35 1.822(6) . . ? C23 C24 1.387(8) . . ? C23 C28 1.392(8) . . ? C24 C25 1.386(9) . . ? C25 C26 1.33(1) . . ? C26 C27 1.37(1) . . ? C27 C28 1.368(9) . . ? C29 C30 1.380(7) . . ? C29 C34 1.406(8) . . ? C30 C31 1.379(8) . . ? C31 C32 1.37(1) . . ? C32 C33 1.36(1) . . ? C33 C34 1.383(9) . . ? C35 C36 1.371(9) . . ? C35 C40 1.368(9) . . ? C36 C37 1.38(1) . . ? C37 C38 1.35(1) . . ? C38 C39 1.38(1) . . ? C39 C40 1.416(9) . . ? _cod_database_code 7051276