#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4061835.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_4061835 _journal_name_full 'Organometallics' _journal_year 2003 _chemical_formula_sum 'C42 H49 Cl O5 P Rh' _chemical_formula_weight 803.14 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 10.831(2) _cell_length_b 10.831(2) _cell_length_c 31.904(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3742.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _exptl_crystal_density_diffrn 1.425 _diffrn_ambient_temperature 200(2) _refine_ls_R_factor_obs 0.0286 _refine_ls_wR_factor_obs 0.0628 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1019(5) 0.2482(5) 0.5042(2) 0.0253(14) Uani 1 d . . H1 H 0.0903(5) 0.1963(5) 0.4806(2) 0.030 Uiso 1 calc R . C2 C 0.1634(5) 0.1966(5) 0.5382(2) 0.0294(14) Uani 1 d . . H2 H 0.1943(5) 0.1151(5) 0.5350(2) 0.035 Uiso 1 calc R . C3 C 0.1857(5) 0.2597(6) 0.5804(2) 0.037(2) Uani 1 d . . H3A H 0.1857(5) 0.1964(6) 0.6028(2) 0.044 Uiso 1 calc R . H3B H 0.1168(5) 0.3174(6) 0.5861(2) 0.044 Uiso 1 calc R . C4 C 0.3080(6) 0.3313(6) 0.5821(2) 0.038(2) Uani 1 d . . H4A H 0.3016(6) 0.3958(6) 0.6040(2) 0.046 Uiso 1 calc R . H4B H 0.3746(6) 0.2739(6) 0.5905(2) 0.046 Uiso 1 calc R . C5 C 0.3432(6) 0.3912(5) 0.5417(2) 0.0325(15) Uani 1 d . . H5 H 0.4277(6) 0.3861(5) 0.5339(2) 0.039 Uiso 1 calc R . C6 C 0.2673(5) 0.4522(5) 0.5149(2) 0.0303(15) Uani 1 d . . H6 H 0.3029(5) 0.4822(5) 0.4897(2) 0.036 Uiso 1 calc R . C7 C 0.1313(5) 0.4767(5) 0.5215(2) 0.034(2) Uani 1 d . . H7A H 0.1105(5) 0.5589(5) 0.5099(2) 0.041 Uiso 1 calc R . H7B H 0.1136(5) 0.4783(5) 0.5519(2) 0.041 Uiso 1 calc R . C8 C 0.0508(5) 0.3798(5) 0.5008(2) 0.033(2) Uani 1 d . . H8A H 0.0412(5) 0.4009(5) 0.4708(2) 0.039 Uiso 1 calc R . H8B H -0.0322(5) 0.3822(5) 0.5138(2) 0.039 Uiso 1 calc R . C9 C 0.4871(4) -0.1004(4) 0.4651(2) 0.0183(12) Uani 1 d . . C10 C 0.5256(4) -0.1067(4) 0.4234(2) 0.0162(12) Uani 1 d . . C11 C 0.5911(5) -0.2116(5) 0.4115(2) 0.0219(13) Uani 1 d . . H11 H 0.6148(5) -0.2211(5) 0.3830(2) 0.026 Uiso 1 calc R . C12 C 0.6228(5) -0.3023(5) 0.4401(2) 0.0240(13) Uani 1 d . . C13 C 0.5861(4) -0.2894(4) 0.4816(2) 0.0195(13) Uani 1 d . . H13 H 0.6094(4) -0.3513(4) 0.5012(2) 0.023 Uiso 1 calc R . C14 C 0.5167(4) -0.1896(4) 0.4957(2) 0.0186(12) Uani 1 d . . C15 C 0.4844(5) -0.1759(5) 0.5423(2) 0.0257(13) Uani 1 d . . C16 C 0.5445(6) -0.0588(5) 0.5598(2) 0.038(2) Uani 1 d . . H16A H 0.5154(6) 0.0131(5) 0.5440(2) 0.057 Uiso 1 calc R . H16B H 0.6344(6) -0.0653(5) 0.5573(2) 0.057 Uiso 1 calc R . H16C H 0.5221(6) -0.0493(5) 0.5894(2) 0.057 Uiso 1 calc R . C17 C 0.4122(4) 0.0710(4) 0.38649(15) 0.0164(12) Uani 1 d . . C18 C 0.4031(5) 0.1605(4) 0.3545(2) 0.0227(13) Uani 1 d . . C19 C 0.5082(5) 0.1744(5) 0.3299(2) 0.0258(13) Uani 1 d . . H19 H 0.5075(5) 0.2343(5) 0.3081(2) 0.031 Uiso 1 calc R . C20 C 0.6140(5) 0.1045(5) 0.3359(2) 0.0247(13) Uani 1 d . . C21 C 0.6183(5) 0.0181(5) 0.3670(2) 0.0242(13) Uani 1 d . . H21 H 0.6915(5) -0.0285(5) 0.3713(2) 0.029 Uiso 1 calc R . C22 C 0.5146(4) -0.0023(4) 0.3927(2) 0.0189(12) Uani 1 d . . C23 C 0.7479(5) -0.4779(5) 0.4548(2) 0.041(2) Uani 1 d . . H23A H 0.7963(5) -0.5408(5) 0.4400(2) 0.061 Uiso 1 calc R . H23B H 0.6826(5) -0.5181(5) 0.4711(2) 0.061 Uiso 1 calc R . H23C H 0.8019(5) -0.4313(5) 0.4736(2) 0.061 Uiso 1 calc R . C24 C 0.1399(5) -0.1260(4) 0.4499(2) 0.0205(13) Uani 1 d . . C25 C 0.2130(5) -0.2297(5) 0.4459(2) 0.0251(13) Uani 1 d . . H25 H 0.2966(5) -0.2275(5) 0.4549(2) 0.030 Uiso 1 calc R . C26 C 0.1645(6) -0.3372(5) 0.4288(2) 0.034(2) Uani 1 d . . H26 H 0.2144(6) -0.4087(5) 0.4256(2) 0.040 Uiso 1 calc R . C27 C 0.0426(5) -0.3378(5) 0.4166(2) 0.036(2) Uani 1 d . . H27 H 0.0080(5) -0.4108(5) 0.4050(2) 0.043 Uiso 1 calc R . C28 C -0.0312(6) -0.2322(5) 0.4210(2) 0.036(2) Uani 1 d . . H28 H -0.1152(6) -0.2349(5) 0.4125(2) 0.043 Uiso 1 calc R . C29 C 0.0166(5) -0.1240(5) 0.4376(2) 0.0286(14) Uani 1 d . . C30 C -0.0640(5) -0.0120(5) 0.4397(2) 0.0242(13) Uani 1 d . . C31 C -0.1740(5) -0.0138(5) 0.4617(2) 0.0303(14) Uani 1 d . . H31 H -0.1973(5) -0.0858(5) 0.4768(2) 0.036 Uiso 1 calc R . C32 C -0.2505(5) 0.0887(6) 0.4620(2) 0.039(2) Uani 1 d . . H32 H -0.3241(5) 0.0880(6) 0.4782(2) 0.047 Uiso 1 calc R . C33 C -0.2202(5) 0.1911(6) 0.4390(2) 0.039(2) Uani 1 d . . H33 H -0.2746(5) 0.2598(6) 0.4383(2) 0.047 Uiso 1 calc R . C34 C -0.1115(6) 0.1945(6) 0.4170(2) 0.039(2) Uani 1 d . . H34 H -0.0894(6) 0.2667(6) 0.4018(2) 0.047 Uiso 1 calc R . C35 C -0.0330(5) 0.0915(5) 0.4169(2) 0.0329(15) Uani 1 d . . H35 H 0.0415(5) 0.0932(5) 0.4012(2) 0.039 Uiso 1 calc R . C36 C 0.8120(6) 0.0441(6) 0.3088(2) 0.050(2) Uani 1 d . . H36A H 0.8733(6) 0.0702(6) 0.2881(2) 0.075 Uiso 1 calc R . H36B H 0.7830(6) -0.0393(6) 0.3020(2) 0.075 Uiso 1 calc R . H36C H 0.8496(6) 0.0440(6) 0.3368(2) 0.075 Uiso 1 calc R . C37 C 0.2846(5) 0.2331(5) 0.3446(2) 0.0255(13) Uani 1 d . . C38 C 0.3055(6) 0.3271(6) 0.3083(2) 0.043(2) Uani 1 d . . H38A H 0.3348(6) 0.2831(6) 0.2833(2) 0.065 Uiso 1 calc R . H38B H 0.3673(6) 0.3882(6) 0.3168(2) 0.065 Uiso 1 calc R . H38C H 0.2276(6) 0.3691(6) 0.3018(2) 0.065 Uiso 1 calc R . C39 C 0.2393(5) 0.3098(5) 0.3819(2) 0.0344(15) Uani 1 d . . H39A H 0.3052(5) 0.3657(5) 0.3910(2) 0.052 Uiso 1 calc R . H39B H 0.2168(5) 0.2547(5) 0.4050(2) 0.052 Uiso 1 calc R . H39C H 0.1670(5) 0.3583(5) 0.3735(2) 0.052 Uiso 1 calc R . C40 C 0.1837(5) 0.1443(5) 0.3293(2) 0.0321(14) Uani 1 d . . H40A H 0.2148(5) 0.0964(5) 0.3055(2) 0.048 Uiso 1 calc R . H40B H 0.1110(5) 0.1917(5) 0.3206(2) 0.048 Uiso 1 calc R . H40C H 0.1609(5) 0.0881(5) 0.3521(2) 0.048 Uiso 1 calc R . C41 C 0.5327(6) -0.2847(6) 0.5680(2) 0.040(2) Uani 1 d . . H41A H 0.4959(6) -0.3614(6) 0.5576(2) 0.060 Uiso 1 calc R . H41B H 0.5104(6) -0.2731(6) 0.5975(2) 0.060 Uiso 1 calc R . H41C H 0.6227(6) -0.2892(6) 0.5654(2) 0.060 Uiso 1 calc R . C42 C 0.3445(5) -0.1716(6) 0.5491(2) 0.039(2) Uani 1 d . . H42A H 0.3093(5) -0.1028(6) 0.5332(2) 0.058 Uiso 1 calc R . H42B H 0.3271(5) -0.1600(6) 0.5790(2) 0.058 Uiso 1 calc R . H42C H 0.3076(5) -0.2493(6) 0.5396(2) 0.058 Uiso 1 calc R . O1 O 0.4233(3) 0.0052(3) 0.47886(10) 0.0194(8) Uani 1 d . . O2 O 0.3059(3) 0.0456(3) 0.41123(10) 0.0193(8) Uani 1 d . . O3 O 0.6938(3) -0.3960(3) 0.42505(11) 0.0294(9) Uani 1 d . . O4 O 0.1854(3) -0.0182(3) 0.47059(10) 0.0215(8) Uani 1 d . . O5 O 0.7090(3) 0.1284(4) 0.30831(12) 0.0370(10) Uani 1 d . . P1 P 0.30082(12) 0.06983(12) 0.46093(4) 0.0185(3) Uani 1 d . . Cl1 Cl 0.47966(12) 0.30770(14) 0.45762(5) 0.0349(4) Uani 1 d . . Rh1 Rh 0.29397(4) 0.25396(4) 0.491619(11) 0.02050(12) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(3) 0.026(3) 0.025(4) -0.007(2) 0.005(3) 0.010(2) C2 0.025(3) 0.036(3) 0.028(4) -0.004(3) 0.001(3) 0.005(3) C3 0.041(4) 0.044(4) 0.026(4) 0.002(3) 0.003(3) 0.012(3) C4 0.045(4) 0.046(4) 0.024(4) -0.010(3) -0.006(3) 0.011(3) C5 0.034(3) 0.032(3) 0.031(4) 0.000(3) 0.000(3) 0.008(3) C6 0.030(3) 0.032(3) 0.029(3) -0.008(3) 0.002(3) 0.000(3) C7 0.033(4) 0.022(3) 0.047(4) -0.001(3) 0.002(3) 0.012(3) C8 0.017(3) 0.044(4) 0.038(4) -0.002(3) 0.005(3) 0.016(3) C9 0.014(3) 0.016(3) 0.025(4) -0.005(3) 0.001(2) 0.000(2) C10 0.008(3) 0.014(3) 0.026(3) 0.003(2) -0.003(2) 0.000(2) C11 0.024(3) 0.025(3) 0.017(3) -0.002(3) -0.008(2) 0.002(3) C12 0.020(3) 0.022(3) 0.030(4) -0.002(3) -0.002(3) 0.000(3) C13 0.021(3) 0.016(3) 0.021(4) 0.004(2) -0.006(2) 0.008(2) C14 0.018(3) 0.022(3) 0.016(3) 0.003(3) -0.006(3) -0.007(2) C15 0.024(3) 0.027(3) 0.027(3) 0.004(3) 0.000(3) 0.004(3) C16 0.049(4) 0.041(4) 0.025(4) -0.008(3) -0.001(3) -0.002(3) C17 0.019(3) 0.016(3) 0.015(3) -0.003(2) 0.001(2) -0.003(2) C18 0.024(3) 0.020(3) 0.024(3) -0.004(3) -0.001(3) -0.003(3) C19 0.031(4) 0.020(3) 0.026(3) 0.000(3) -0.002(3) -0.001(3) C20 0.032(4) 0.024(3) 0.018(3) -0.005(3) 0.003(3) -0.010(3) C21 0.021(3) 0.026(3) 0.026(3) -0.006(3) -0.003(3) -0.002(3) C22 0.020(3) 0.020(3) 0.017(3) -0.007(2) 0.002(3) -0.002(3) C23 0.039(4) 0.026(3) 0.057(5) 0.012(3) 0.007(3) 0.010(3) C24 0.024(3) 0.020(3) 0.017(3) 0.000(2) -0.004(2) -0.010(3) C25 0.024(3) 0.027(3) 0.024(3) 0.007(3) 0.005(2) 0.001(3) C26 0.051(4) 0.023(4) 0.028(3) 0.000(3) -0.002(3) -0.006(3) C27 0.041(4) 0.029(4) 0.039(4) -0.007(3) -0.004(3) -0.013(3) C28 0.033(3) 0.041(4) 0.035(4) -0.005(3) -0.007(3) -0.006(3) C29 0.032(4) 0.029(3) 0.024(3) 0.002(3) 0.003(3) -0.007(3) C30 0.018(3) 0.033(4) 0.021(3) -0.005(3) -0.003(3) -0.004(3) C31 0.024(3) 0.033(4) 0.034(4) -0.005(3) -0.004(3) -0.006(3) C32 0.023(3) 0.051(4) 0.043(4) -0.012(4) -0.001(3) -0.009(3) C33 0.026(4) 0.034(4) 0.057(4) -0.017(3) -0.008(3) -0.001(3) C34 0.039(4) 0.029(4) 0.049(4) 0.005(3) -0.001(3) 0.000(3) C35 0.019(3) 0.048(4) 0.031(4) 0.002(3) 0.001(3) 0.001(3) C36 0.042(4) 0.055(5) 0.052(5) 0.010(4) 0.020(3) -0.001(4) C37 0.032(3) 0.020(3) 0.024(3) 0.002(3) -0.007(3) 0.004(3) C38 0.043(4) 0.033(4) 0.053(5) 0.029(3) 0.002(3) 0.006(3) C39 0.036(4) 0.022(3) 0.046(4) -0.003(3) -0.005(3) 0.013(3) C40 0.029(3) 0.037(4) 0.030(4) 0.003(3) 0.002(3) 0.013(3) C41 0.048(4) 0.049(4) 0.022(3) 0.008(3) -0.001(3) 0.007(3) C42 0.038(4) 0.054(4) 0.024(4) 0.007(3) 0.007(3) 0.001(3) O1 0.022(2) 0.018(2) 0.018(2) 0.0016(15) -0.0042(14) 0.011(2) O2 0.018(2) 0.022(2) 0.017(2) 0.002(2) 0.002(2) 0.003(2) O3 0.035(2) 0.023(2) 0.030(2) 0.001(2) 0.001(2) 0.015(2) O4 0.021(2) 0.020(2) 0.024(2) -0.004(2) 0.002(2) -0.001(2) O5 0.030(2) 0.042(2) 0.039(3) 0.015(2) 0.010(2) -0.002(2) P1 0.0150(7) 0.0198(8) 0.0206(9) 0.0004(6) -0.0006(6) 0.0015(6) Cl1 0.0242(8) 0.0395(9) 0.0409(10) -0.0053(7) 0.0063(7) -0.0052(7) Rh1 0.0178(2) 0.0200(2) 0.0237(2) -0.0043(2) 0.0007(2) 0.0019(2) 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 1.390(7) . ? C1 C8 1.533(7) . ? C1 Rh1 2.120(5) . ? C2 C3 1.528(8) . ? C2 Rh1 2.144(5) . ? C3 C4 1.536(8) . ? C4 C5 1.492(8) . ? C5 C6 1.358(8) . ? C5 Rh1 2.247(6) . ? C6 C7 1.511(8) . ? C6 Rh1 2.291(5) . ? C7 C8 1.516(8) . ? C9 C10 1.397(7) . ? C9 O1 1.406(5) . ? C9 C14 1.410(7) . ? C10 C11 1.392(7) . ? C10 C22 1.500(7) . ? C11 C12 1.382(7) . ? C12 O3 1.361(6) . ? C12 C13 1.392(7) . ? C13 C14 1.391(7) . ? C14 C15 1.533(8) . ? C15 C41 1.528(8) . ? C15 C16 1.531(8) . ? C15 C42 1.531(8) . ? C17 C22 1.379(7) . ? C17 C18 1.411(7) . ? C17 O2 1.422(6) . ? C18 C19 1.391(8) . ? C18 C37 1.538(7) . ? C19 C20 1.387(8) . ? C20 C21 1.366(8) . ? C20 O5 1.377(6) . ? C21 C22 1.408(7) . ? C23 O3 1.424(7) . ? C24 C25 1.380(7) . ? C24 C29 1.393(7) . ? C24 O4 1.428(6) . ? C25 C26 1.389(8) . ? C26 C27 1.377(8) . ? C27 C28 1.402(8) . ? C28 C29 1.386(8) . ? C29 C30 1.496(8) . ? C30 C35 1.377(8) . ? C30 C31 1.384(8) . ? C31 C32 1.385(8) . ? C32 C33 1.369(8) . ? C33 C34 1.371(8) . ? C34 C35 1.403(8) . ? C36 O5 1.442(7) . ? C37 C39 1.532(8) . ? C37 C40 1.535(8) . ? C37 C38 1.559(8) . ? O1 P1 1.605(3) . ? O2 P1 1.608(4) . ? O4 P1 1.602(4) . ? P1 Rh1 2.2229(14) . ? Cl1 Rh1 2.3581(14) . ?