#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4060627.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_4060627 _journal_name_full 'Organometallics' _journal_year 2006 _chemical_formula_sum 'C57 H44 F3 N4 O2 Rh' _chemical_formula_weight 976.87 _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.6870(18) _cell_length_b 13.3266(7) _cell_length_c 22.7762(11) _cell_angle_alpha 90.00 _cell_angle_beta 116.9640(10) _cell_angle_gamma 90.00 _cell_volume 9384.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.383 _diffrn_ambient_temperature 293(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 Rh1 Rh 0.347310(14) 0.46053(4) 0.74551(2) 0.05078(18) Uani 1 1 d . . . O1 O 0.34756(18) 0.4900(4) 0.6240(3) 0.0894(16) Uani 1 1 d . . . O2 O 0.3347(2) 0.5084(5) 0.8398(3) 0.111(2) Uani 1 1 d . . . H2 H 0.3403 0.4794 0.8129 0.167 Uiso 1 1 calc R . . N1 N 0.37401(15) 0.5990(4) 0.7519(2) 0.0581(13) Uani 1 1 d . . . N2 N 0.40653(15) 0.4081(4) 0.8099(2) 0.0553(13) Uani 1 1 d . . . N3 N 0.32096(15) 0.3250(4) 0.7467(2) 0.0543(12) Uani 1 1 d . . . N4 N 0.28756(15) 0.5163(4) 0.6863(2) 0.0562(13) Uani 1 1 d . . . C1 C 0.3517(2) 0.6833(5) 0.7183(3) 0.0623(17) Uani 1 1 d . . . C2 C 0.3828(2) 0.7637(5) 0.7330(4) 0.082(2) Uani 1 1 d . . . H2A H 0.3768 0.8283 0.7157 0.099 Uiso 1 1 calc R . . C3 C 0.4215(2) 0.7294(5) 0.7756(3) 0.076(2) Uani 1 1 d . . . H3A H 0.4470 0.7665 0.7946 0.091 Uiso 1 1 calc R . . C4 C 0.41699(19) 0.6243(5) 0.7874(3) 0.0593(16) Uani 1 1 d . . . C5 C 0.44972(19) 0.5623(5) 0.8278(3) 0.0585(17) Uani 1 1 d . . . C6 C 0.44479(19) 0.4607(5) 0.8380(3) 0.0607(16) Uani 1 1 d . . . C7 C 0.4787(2) 0.3960(6) 0.8793(3) 0.079(2) Uani 1 1 d . . . H7A H 0.5076 0.4138 0.9031 0.095 Uiso 1 1 calc R . . C8 C 0.4620(2) 0.3045(6) 0.8784(3) 0.082(2) Uani 1 1 d . . . H8A H 0.4768 0.2479 0.9014 0.099 Uiso 1 1 calc R . . C9 C 0.41620(19) 0.3122(5) 0.8341(3) 0.0618(17) Uani 1 1 d . . . C10 C 0.3869(2) 0.2321(5) 0.8211(3) 0.0614(17) Uani 1 1 d . . . C11 C 0.3421(2) 0.2405(5) 0.7799(3) 0.0600(16) Uani 1 1 d . . . C12 C 0.3118(2) 0.1590(5) 0.7637(3) 0.0687(19) Uani 1 1 d . . . H12A H 0.3179 0.0939 0.7799 0.082 Uiso 1 1 calc R . . C13 C 0.2733(2) 0.1941(5) 0.7212(3) 0.0670(18) Uani 1 1 d . . . H13A H 0.2477 0.1574 0.7021 0.080 Uiso 1 1 calc R . . C14 C 0.27785(18) 0.2972(5) 0.7099(3) 0.0527(15) Uani 1 1 d . . . C15 C 0.24494(18) 0.3595(5) 0.6670(3) 0.0534(15) Uani 1 1 d . . . C16 C 0.24921(18) 0.4610(5) 0.6576(3) 0.0553(15) Uani 1 1 d . . . C17 C 0.2151(2) 0.5275(5) 0.6159(3) 0.0653(18) Uani 1 1 d . . . H17A H 0.1862 0.5104 0.5911 0.078 Uiso 1 1 calc R . . C18 C 0.2323(2) 0.6181(5) 0.6188(3) 0.0649(17) Uani 1 1 d . . . H18A H 0.2174 0.6753 0.5968 0.078 Uiso 1 1 calc R . . C19 C 0.2779(2) 0.6116(5) 0.6621(3) 0.0580(16) Uani 1 1 d . . . C20 C 0.3073(2) 0.6896(5) 0.6745(3) 0.0644(17) Uani 1 1 d . . . C21 C 0.49491(19) 0.6036(5) 0.8645(3) 0.0637(17) Uani 1 1 d . . . C22 C 0.5119(3) 0.6281(8) 0.9274(5) 0.127(4) Uani 1 1 d . . . H22A H 0.4949 0.6226 0.9493 0.152 Uiso 1 1 calc R . . C23 C 0.5550(3) 0.6625(9) 0.9628(5) 0.141(4) Uani 1 1 d . . . H23A H 0.5662 0.6766 1.0075 0.169 Uiso 1 1 calc R . . C24 C 0.5799(3) 0.6750(8) 0.9319(5) 0.108(3) Uani 1 1 d . . . C25 C 0.5650(3) 0.6381(11) 0.8725(5) 0.157(5) Uani 1 1 d . . . H25A H 0.5831 0.6345 0.8525 0.189 Uiso 1 1 calc R . . C26 C 0.5227(3) 0.6039(12) 0.8388(5) 0.180(6) Uani 1 1 d . . . H26A H 0.5132 0.5801 0.7961 0.216 Uiso 1 1 calc R . . C27 C 0.6264(3) 0.7131(10) 0.9685(6) 0.163(5) Uani 1 1 d . . . H27A H 0.6387 0.7177 0.9384 0.245 Uiso 1 1 calc R . . H27B H 0.6431 0.6674 1.0034 0.245 Uiso 1 1 calc R . . H27C H 0.6265 0.7782 0.9866 0.245 Uiso 1 1 calc R . . C31 C 0.4047(2) 0.1342(5) 0.8526(4) 0.071(2) Uani 1 1 d . . . C32 C 0.3981(3) 0.1018(7) 0.9051(4) 0.100(3) Uani 1 1 d . . . H32A H 0.3804 0.1377 0.9185 0.120 Uiso 1 1 calc R . . C33 C 0.4190(4) 0.0118(9) 0.9379(5) 0.132(4) Uani 1 1 d . . . H33A H 0.4148 -0.0115 0.9730 0.158 Uiso 1 1 calc R . . C34 C 0.4454(3) -0.0412(8) 0.9183(7) 0.128(5) Uani 1 1 d . . . C35 C 0.4498(3) -0.0083(8) 0.8670(6) 0.126(4) Uani 1 1 d . . . H35A H 0.4672 -0.0447 0.8534 0.151 Uiso 1 1 calc R . . C36 C 0.4301(3) 0.0761(7) 0.8329(5) 0.106(3) Uani 1 1 d . . . H36A H 0.4336 0.0950 0.7963 0.127 Uiso 1 1 calc R . . C37 C 0.4690(4) -0.1348(7) 0.9603(6) 0.218(8) Uani 1 1 d . . . H37A H 0.4865 -0.1651 0.9424 0.326 Uiso 1 1 calc R . . H37B H 0.4480 -0.1824 0.9595 0.326 Uiso 1 1 calc R . . H37C H 0.4871 -0.1144 1.0049 0.326 Uiso 1 1 calc R . . C41 C 0.20161(18) 0.3117(5) 0.6258(3) 0.0550(15) Uani 1 1 d . . . C42 C 0.1730(2) 0.2910(6) 0.6491(3) 0.081(2) Uani 1 1 d . . . H42A H 0.1791 0.3116 0.6914 0.098 Uiso 1 1 calc R . . C43 C 0.1344(2) 0.2393(6) 0.6111(4) 0.088(2) Uani 1 1 d . . . H43A H 0.1150 0.2276 0.6280 0.106 Uiso 1 1 calc R . . C44 C 0.1253(2) 0.2063(6) 0.5497(4) 0.073(2) Uani 1 1 d . . . C45 C 0.1528(2) 0.2304(6) 0.5252(4) 0.088(2) Uani 1 1 d . . . H45A H 0.1461 0.2124 0.4822 0.106 Uiso 1 1 calc R . . C46 C 0.1913(2) 0.2817(6) 0.5628(3) 0.083(2) Uani 1 1 d . . . H46A H 0.2101 0.2958 0.5450 0.100 Uiso 1 1 calc R . . C47 C 0.0847(2) 0.1457(7) 0.5074(4) 0.115(3) Uani 1 1 d . . . H47A H 0.0845 0.1295 0.4662 0.173 Uiso 1 1 calc R . . H47B H 0.0595 0.1847 0.4994 0.173 Uiso 1 1 calc R . . H47C H 0.0846 0.0850 0.5300 0.173 Uiso 1 1 calc R . . C51 C 0.2912(2) 0.7873(5) 0.6392(4) 0.0699(19) Uani 1 1 d . . . C52 C 0.2755(6) 0.8602(8) 0.6612(5) 0.221(9) Uani 1 1 d . . . H52A H 0.2733 0.8528 0.7002 0.265 Uiso 1 1 calc R . . C53 C 0.2618(6) 0.9511(8) 0.6238(6) 0.240(10) Uani 1 1 d . . . H53A H 0.2527 1.0036 0.6413 0.288 Uiso 1 1 calc R . . C54 C 0.2613(3) 0.9653(7) 0.5670(5) 0.101(3) Uani 1 1 d . . . C55 C 0.2730(5) 0.8917(10) 0.5461(7) 0.209(8) Uani 1 1 d . . . H55A H 0.2714 0.8965 0.5043 0.251 Uiso 1 1 calc R . . C56 C 0.2885(5) 0.8013(8) 0.5806(6) 0.183(7) Uani 1 1 d . . . H56A H 0.2971 0.7502 0.5613 0.220 Uiso 1 1 calc R . . C57 C 0.2442(4) 1.0624(6) 0.5268(5) 0.148(5) Uani 1 1 d . . . H57A H 0.2465 1.0574 0.4865 0.222 Uiso 1 1 calc R . . H57B H 0.2609 1.1185 0.5519 0.222 Uiso 1 1 calc R . . H57C H 0.2144 1.0718 0.5169 0.222 Uiso 1 1 calc R . . C61 C 0.3746(2) 0.3306(5) 0.6648(3) 0.0660(18) Uani 1 1 d . . . C62 C 0.4181(3) 0.3222(7) 0.6794(4) 0.096(3) Uani 1 1 d . . . H62A H 0.4362 0.3778 0.6938 0.115 Uiso 1 1 calc R . . C63 C 0.4342(3) 0.2295(10) 0.6721(5) 0.118(3) Uani 1 1 d . . . H63A H 0.4632 0.2243 0.6816 0.142 Uiso 1 1 calc R . . C64 C 0.4085(4) 0.1466(8) 0.6513(5) 0.106(3) Uani 1 1 d . . . C65 C 0.3658(3) 0.1545(7) 0.6368(4) 0.103(3) Uani 1 1 d . . . H65A H 0.3479 0.0986 0.6219 0.124 Uiso 1 1 calc R . . C66 C 0.3492(3) 0.2443(6) 0.6442(4) 0.081(2) Uani 1 1 d . . . H66A H 0.3203 0.2477 0.6352 0.097 Uiso 1 1 calc R . . C67 C 0.4259(7) 0.0485(15) 0.6475(11) 0.176(7) Uani 1 1 d . . . C68 C 0.35582(19) 0.4314(5) 0.6687(3) 0.0628(18) Uani 1 1 d . . . C71 C 0.3426(8) 0.4469(11) 0.8907(8) 0.306(14) Uani 1 1 d . . . H71A H 0.3355 0.4805 0.9219 0.459 Uiso 1 1 calc R . . H71B H 0.3726 0.4288 0.9117 0.459 Uiso 1 1 calc R . . H71C H 0.3253 0.3875 0.8750 0.459 Uiso 1 1 calc R . . F1 F 0.4314(8) -0.0117(9) 0.6850(9) 0.343(12) Uani 1 1 d . . . F2 F 0.4606(5) 0.0552(9) 0.6417(16) 0.381(13) Uani 1 1 d . . . F3 F 0.4072(6) 0.0083(11) 0.5950(8) 0.343(11) Uani 1 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 Rh1 0.0405(3) 0.0527(3) 0.0464(3) 0.0007(2) 0.00853(18) -0.0050(2) O1 0.102(4) 0.096(4) 0.068(3) 0.018(3) 0.036(3) 0.008(3) O2 0.143(6) 0.112(5) 0.094(4) -0.022(4) 0.067(4) -0.022(4) N1 0.041(3) 0.062(3) 0.059(3) 0.004(3) 0.011(2) -0.001(2) N2 0.046(3) 0.058(3) 0.048(3) 0.003(2) 0.009(2) -0.008(2) N3 0.048(3) 0.058(3) 0.044(3) 0.002(2) 0.010(2) -0.005(2) N4 0.046(3) 0.055(3) 0.057(3) 0.002(2) 0.015(2) -0.001(2) C1 0.064(4) 0.048(4) 0.066(4) 0.008(3) 0.021(3) -0.005(3) C2 0.076(5) 0.055(4) 0.098(6) 0.006(4) 0.022(4) -0.017(4) C3 0.059(4) 0.071(5) 0.076(5) -0.001(4) 0.011(4) -0.019(4) C4 0.049(4) 0.059(4) 0.056(4) -0.001(3) 0.012(3) -0.013(3) C5 0.049(4) 0.064(5) 0.044(3) 0.000(3) 0.006(3) -0.012(3) C6 0.044(3) 0.067(4) 0.057(4) 0.008(3) 0.011(3) -0.001(3) C7 0.040(4) 0.085(5) 0.086(5) 0.016(4) 0.006(3) -0.005(4) C8 0.052(4) 0.075(5) 0.084(5) 0.017(4) 0.000(4) -0.007(4) C9 0.050(4) 0.068(5) 0.048(4) 0.007(3) 0.006(3) -0.001(3) C10 0.055(4) 0.063(4) 0.049(4) 0.004(3) 0.009(3) -0.003(3) C11 0.055(4) 0.061(4) 0.049(4) 0.003(3) 0.010(3) -0.008(3) C12 0.064(4) 0.058(4) 0.064(4) 0.008(3) 0.011(3) -0.008(3) C13 0.059(4) 0.064(4) 0.061(4) 0.003(3) 0.013(3) -0.020(3) C14 0.046(3) 0.057(4) 0.047(3) -0.002(3) 0.014(3) -0.012(3) C15 0.042(3) 0.060(4) 0.053(4) -0.001(3) 0.017(3) -0.007(3) C16 0.039(3) 0.069(4) 0.048(3) -0.004(3) 0.010(3) 0.000(3) C17 0.042(3) 0.075(5) 0.068(4) 0.001(4) 0.016(3) -0.002(3) C18 0.048(4) 0.060(4) 0.076(4) 0.008(4) 0.019(3) 0.006(3) C19 0.054(4) 0.052(4) 0.061(4) -0.002(3) 0.020(3) 0.001(3) C20 0.058(4) 0.055(4) 0.068(4) 0.005(3) 0.017(3) 0.007(3) C21 0.046(4) 0.080(5) 0.054(4) -0.001(4) 0.013(3) -0.016(3) C22 0.063(5) 0.208(11) 0.115(7) -0.077(7) 0.046(5) -0.049(6) C23 0.074(6) 0.217(13) 0.122(8) -0.084(8) 0.036(6) -0.052(7) C24 0.062(5) 0.145(9) 0.109(7) -0.022(6) 0.031(5) -0.049(5) C25 0.081(7) 0.285(17) 0.105(8) -0.011(9) 0.041(6) -0.055(9) C26 0.090(7) 0.37(2) 0.074(6) -0.032(9) 0.037(6) -0.090(10) C27 0.063(6) 0.212(13) 0.193(11) -0.024(9) 0.039(7) -0.057(7) C31 0.048(4) 0.059(4) 0.077(5) 0.020(4) 0.004(3) -0.006(3) C32 0.081(6) 0.105(7) 0.086(6) 0.031(5) 0.015(4) -0.003(5) C33 0.108(8) 0.129(9) 0.107(8) 0.068(7) 0.003(6) -0.033(7) C34 0.075(6) 0.071(6) 0.156(11) 0.026(7) -0.018(7) -0.009(5) C35 0.105(8) 0.077(7) 0.159(11) 0.009(7) 0.027(8) 0.018(6) C36 0.100(7) 0.086(6) 0.121(7) 0.021(6) 0.041(6) 0.015(5) C37 0.133(9) 0.090(7) 0.264(15) 0.094(9) -0.056(9) -0.007(7) C41 0.038(3) 0.064(4) 0.053(4) 0.000(3) 0.012(3) -0.001(3) C42 0.061(4) 0.119(6) 0.060(4) -0.015(4) 0.023(4) -0.027(4) C43 0.058(5) 0.125(7) 0.083(6) -0.006(5) 0.033(4) -0.027(5) C44 0.045(4) 0.082(5) 0.072(5) -0.003(4) 0.008(3) -0.013(3) C45 0.070(5) 0.115(7) 0.066(5) -0.024(4) 0.018(4) -0.020(5) C46 0.062(4) 0.124(7) 0.058(4) -0.017(4) 0.021(4) -0.035(4) C47 0.062(5) 0.119(7) 0.135(8) -0.030(6) 0.019(5) -0.035(5) C51 0.064(4) 0.055(4) 0.072(5) -0.001(4) 0.014(4) 0.008(3) C52 0.43(2) 0.098(8) 0.067(6) 0.009(6) 0.048(10) 0.117(11) C53 0.46(3) 0.085(8) 0.090(8) 0.001(7) 0.053(12) 0.128(12) C54 0.096(6) 0.065(5) 0.088(6) 0.016(5) -0.005(5) -0.008(5) C55 0.38(2) 0.142(11) 0.223(14) 0.112(11) 0.236(16) 0.133(13) C56 0.335(19) 0.126(9) 0.201(12) 0.100(9) 0.219(14) 0.136(11) C57 0.158(10) 0.071(6) 0.143(9) 0.042(6) 0.006(8) 0.017(6) C61 0.062(4) 0.082(5) 0.050(4) -0.006(3) 0.022(3) 0.000(4) C62 0.059(5) 0.128(8) 0.097(6) -0.025(5) 0.032(4) -0.003(5) C63 0.081(7) 0.152(10) 0.112(7) -0.012(7) 0.035(6) 0.039(7) C64 0.114(8) 0.096(7) 0.108(7) -0.009(6) 0.050(6) 0.028(6) C65 0.112(8) 0.091(7) 0.112(7) -0.018(5) 0.054(6) 0.003(6) C66 0.078(5) 0.077(5) 0.085(5) -0.016(4) 0.036(4) -0.010(4) C67 0.217(18) 0.175(16) 0.166(15) -0.009(12) 0.114(14) 0.083(14) C68 0.045(4) 0.072(5) 0.059(4) 0.005(3) 0.012(3) -0.007(3) C71 0.65(4) 0.170(15) 0.246(18) 0.017(13) 0.33(3) -0.019(19) F1 0.61(3) 0.172(10) 0.352(18) 0.101(11) 0.32(2) 0.216(15) F2 0.265(15) 0.200(11) 0.80(4) -0.109(18) 0.35(2) 0.025(10) F3 0.45(3) 0.259(14) 0.254(14) -0.100(11) 0.100(14) 0.169(15) 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 Rh1 C68 1.941(7) . ? Rh1 N3 2.030(5) . ? Rh1 N2 2.032(5) . ? Rh1 N4 2.033(5) . ? Rh1 N1 2.040(5) . ? O1 C68 1.209(7) . ? O2 C71 1.342(13) . ? N1 C4 1.377(7) . ? N1 C1 1.383(8) . ? N2 C9 1.372(8) . ? N2 C6 1.375(7) . ? N3 C11 1.369(7) . ? N3 C14 1.392(7) . ? N4 C19 1.365(8) . ? N4 C16 1.397(7) . ? C1 C20 1.408(8) . ? C1 C2 1.449(9) . ? C2 C3 1.330(9) . ? C3 C4 1.448(9) . ? C4 C5 1.368(8) . ? C5 C6 1.397(9) . ? C5 C21 1.507(8) . ? C6 C7 1.416(9) . ? C7 C8 1.346(9) . ? C8 C9 1.448(8) . ? C9 C10 1.408(8) . ? C10 C11 1.409(8) . ? C10 C31 1.482(9) . ? C11 C12 1.440(8) . ? C12 C13 1.328(8) . ? C13 C14 1.421(8) . ? C14 C15 1.392(8) . ? C15 C16 1.386(8) . ? C15 C41 1.506(8) . ? C16 C17 1.439(8) . ? C17 C18 1.335(8) . ? C18 C19 1.437(8) . ? C19 C20 1.391(8) . ? C20 C51 1.499(9) . ? C21 C22 1.319(9) . ? C21 C26 1.337(11) . ? C22 C23 1.414(11) . ? C23 C24 1.353(12) . ? C24 C25 1.304(12) . ? C24 C27 1.527(11) . ? C25 C26 1.389(12) . ? C31 C32 1.385(10) . ? C31 C36 1.390(11) . ? C32 C33 1.425(13) . ? C33 C34 1.382(17) . ? C34 C35 1.321(16) . ? C34 C37 1.559(13) . ? C35 C36 1.363(12) . ? C41 C42 1.347(8) . ? C41 C46 1.371(8) . ? C42 C43 1.402(9) . ? C43 C44 1.358(9) . ? C44 C45 1.345(9) . ? C44 C47 1.527(9) . ? C45 C46 1.394(9) . ? C51 C56 1.309(11) . ? C51 C52 1.319(12) . ? C52 C53 1.432(13) . ? C53 C54 1.299(15) . ? C54 C55 1.236(13) . ? C54 C57 1.541(11) . ? C55 C56 1.405(13) . ? C61 C66 1.394(9) . ? C61 C62 1.397(10) . ? C61 C68 1.512(9) . ? C62 C63 1.396(12) . ? C63 C64 1.364(13) . ? C64 C65 1.367(12) . ? C64 C67 1.458(17) . ? C65 C66 1.371(10) . ? C67 F1 1.124(18) . ? C67 F3 1.20(2) . ? C67 F2 1.27(2) . ? F2 F3 1.778(19) . ?