# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2251 data_global _publ_title ; Cis-di(\m-trifluoroacetate)dirhodium tetracarbonyl: structure and chemistry ; _publ_author_name ; F. Albert Cotton, Evgeny V. Dikarev and Marina A. Petrukhina ; _publ_author_address ; Department of Chemistry and Laboratory for Molecular Structure and Bonding, P.O. Box 30012, Texas A&M University, College Station, TX 77845 ; #===END data_[Rh2(O2CCF3)2(CO)4]_(2) _audit_creation_method SHELXL _chemical_name_systematic ; Catena-(bis(\m-trifluoroacetato-O,O')-tetracalbonyl-di-rhodium(I)) ; _chemical_formula_moiety 'Rh2 (O2 C C F3)2 (C O)4' _chemical_formula_structural '[Rh2(\m-O2CCF3)2(CO)4] ' _chemical_formula_analytical 'not measured' _chemical_formula_sum 'C8 F6 O8 Rh2' _chemical_formula_weight 543.90 _chemical_melting_point 'not measured' _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 31.137(2) _cell_length_b 11.866(2) _cell_length_c 8.4282(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.90(1) _cell_angle_gamma 90.00 _cell_volume 3091.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 9.05 _cell_measurement_theta_max 20.8 _exptl_crystal_description 'block-shaped' _exptl_crystal_colour 'golden-yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.337 _exptl_crystal_density_method none _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 2.236 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius FAST area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7228 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 22.47 _reflns_number_total 2122 _reflns_number_observed 1786 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MADNES (Enraf-Nonius, 1989)' _computing_cell_refinement 'MADNES (Enraf-Nonius, 1989)' _computing_data_reduction 'PROCOR (Kabsch, 1988)' _computing_structure_solution 'SHELXTL V.5 (Siemens, 1994)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL V.5 (Siemens, 1994)' _computing_publication_material CIFTAB _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+20.9785P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef noref _refine_ls_number_reflns 2122 _refine_ls_number_parameters 265 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_obs 0.0436 _refine_ls_wR_factor_all 0.1227 _refine_ls_wR_factor_obs 0.1139 _refine_ls_goodness_of_fit_all 1.102 _refine_ls_goodness_of_fit_obs 1.133 _refine_ls_restrained_S_all 1.105 _refine_ls_restrained_S_obs 1.132 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 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 Rh1 Rh 0.13351(2) 0.12575(5) 0.52589(6) 0.0500(3) Uani 1 d . . Rh2 Rh 0.13310(2) 0.37386(5) 0.63763(7) 0.0549(3) Uani 1 d . . O1 O 0.0762(2) 0.0949(5) 0.6218(7) 0.0678(14) Uani 1 d . . O2 O 0.1628(2) 0.0935(5) 0.7574(6) 0.0648(14) Uani 1 d . . O3 O 0.2178(2) 0.1599(7) 0.4045(8) 0.094(2) Uani 1 d . . O4 O 0.0881(2) 0.1824(7) 0.2053(8) 0.106(2) Uani 1 d . . O5 O 0.1706(2) 0.4060(5) 0.4529(7) 0.072(2) Uani 1 d . . O6 O 0.0797(2) 0.4063(5) 0.4684(7) 0.073(2) Uani 1 d . . O7 O 0.0789(3) 0.3211(7) 0.8925(9) 0.117(3) Uani 1 d . . O8 O 0.2108(2) 0.3233(7) 0.8631(9) 0.105(2) Uani 1 d . . C1 C 0.0623(3) 0.0000 0.6523(12) 0.061(3) Uani 1 d S . C2 C 0.1684(3) 0.0000 0.8191(11) 0.052(3) Uani 1 d S . C3 C 0.0235(5) 0.0000 0.7548(22) 0.102(5) Uani 1 d SD 1 F1 F -0.0136(9) 0.0000 0.6638(36) 0.089(10) Uiso 0.30 d SPD 1 F2 F 0.0218(8) 0.0945(20) 0.8429(29) 0.105(6) Uiso 0.30 d PD 1 F1X F 0.0040(7) 0.1074(17) 0.7421(29) 0.107(6) Uiso 0.350(9) d P 2 F2X F 0.0364(4) -0.0340(10) 0.8940(15) 0.069(4) Uiso 0.35 d P 2 F3X F -0.0070(6) -0.0589(21) 0.6771(26) 0.097(5) Uiso 0.35 d P 2 C4 C 0.1837(4) 0.0000 1.0001(15) 0.081(4) Uani 1 d SD 3 F4 F 0.2166(12) 0.0000 1.0591(56) 0.083(16) Uiso 0.20 d SPD 3 F5 F 0.1684(8) 0.0799(22) 1.0757(23) 0.049(5) Uiso 0.20 d PD 3 F4X F 0.1621(11) 0.0000 1.0937(36) 0.046(8) Uiso 0.200(12) d SPD 4 F5X F 0.2058(8) 0.0888(20) 1.0429(23) 0.052(5) Uiso 0.20 d PD 4 F4Y F 0.2251(5) 0.0361(14) 1.0243(19) 0.061(5) Uiso 0.300(6) d P 5 F5Y F 0.1848(7) -0.1234(15) 1.0572(19) 0.064(4) Uiso 0.30 d P 5 F6Y F 0.1482(6) 0.0382(15) 1.0715(22) 0.078(6) Uiso 0.30 d P 5 C5 C 0.1854(3) 0.1491(7) 0.4485(9) 0.063(2) Uani 1 d . . C6 C 0.1052(3) 0.1597(8) 0.3258(10) 0.066(2) Uani 1 d . . C7 C 0.1784(4) 0.5000 0.4023(13) 0.060(3) Uani 1 d S . C8 C 0.0670(3) 0.5000 0.4215(12) 0.058(3) Uani 1 d S . C9 C 0.2036(5) 0.5000 0.2522(16) 0.076(3) Uani 1 d S 6 F7 F 0.1738(6) 0.5000 0.1229(21) 0.083(5) Uiso 0.50 d SP 6 F8 F 0.2268(5) 0.4066(12) 0.2422(16) 0.095(3) Uiso 0.50 d P 6 F7X F 0.2026(9) 0.6126(20) 0.1927(30) 0.087(6) Uiso 0.250(7) d P 7 F8X F 0.2408(6) 0.4610(14) 0.2829(20) 0.062(5) Uiso 0.25 d P 7 F9X F 0.1839(8) 0.4453(25) 0.1417(31) 0.087(6) Uiso 0.25 d P 7 C10 C 0.0298(5) 0.5000 0.2840(20) 0.095(4) Uani 1 d SD 8 F10 F 0.0377(11) 0.5000 0.1535(37) 0.085(11) Uiso 0.30 d SPD 8 F11 F 0.0054(8) 0.4120(23) 0.2928(30) 0.093(7) Uiso 0.30 d PD 8 F10X F -0.0066(10) 0.5000 0.3071(43) 0.089(10) Uiso 0.30(2) d SPD 9 F11X F 0.0301(7) 0.4118(19) 0.1840(25) 0.090(6) Uiso 0.30 d PD 9 F10Y F 0.0175(11) 0.6269(27) 0.2490(42) 0.084(9) Uiso 0.200(9) d P 10 F11Y F -0.0041(10) 0.4507(29) 0.3443(38) 0.073(9) Uiso 0.20 d P 10 F12Y F 0.0498(8) 0.4598(22) 0.1545(28) 0.056(7) Uiso 0.20 d P 10 C11 C 0.0994(3) 0.3400(8) 0.7959(11) 0.075(2) Uani 1 d . . C12 C 0.1811(3) 0.3422(7) 0.7780(11) 0.072(2) 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 Rh1 0.0624(4) 0.0472(4) 0.0413(4) -0.0010(2) 0.0105(3) 0.0015(3) Rh2 0.0721(5) 0.0470(4) 0.0481(4) -0.0010(3) 0.0175(3) -0.0001(3) O1 0.066(3) 0.074(4) 0.068(4) 0.001(3) 0.027(3) 0.006(3) O2 0.088(4) 0.061(3) 0.045(3) -0.003(3) 0.004(3) 0.000(3) O3 0.082(4) 0.119(5) 0.089(5) -0.007(4) 0.037(4) -0.017(4) O4 0.123(5) 0.132(6) 0.058(4) 0.029(4) -0.005(4) 0.015(5) O5 0.093(4) 0.063(3) 0.067(4) -0.006(3) 0.035(3) -0.001(3) O6 0.080(4) 0.072(4) 0.065(3) 0.002(3) 0.003(3) -0.008(3) O7 0.143(6) 0.132(6) 0.089(5) 0.028(5) 0.064(5) 0.016(5) O8 0.106(5) 0.105(5) 0.097(5) -0.016(4) -0.024(5) -0.006(4) C1 0.041(6) 0.112(11) 0.033(6) 0.000 0.014(4) 0.000 C2 0.040(5) 0.082(9) 0.033(5) 0.000 0.005(4) 0.000 C3 0.074(9) 0.105(13) 0.122(14) 0.000 -0.004(9) 0.000 C4 0.059(8) 0.138(14) 0.049(7) 0.000 0.016(6) 0.000 C5 0.080(6) 0.058(5) 0.051(5) -0.009(4) 0.012(4) -0.005(4) C6 0.075(5) 0.071(5) 0.055(5) 0.007(4) 0.017(4) 0.009(4) C7 0.059(7) 0.081(9) 0.045(6) 0.000 0.020(5) 0.000 C8 0.054(6) 0.081(9) 0.040(6) 0.000 0.005(5) 0.000 C9 0.090(10) 0.073(9) 0.066(8) 0.000 0.010(7) 0.000 C10 0.091(11) 0.114(14) 0.085(11) 0.000 0.026(9) 0.000 C11 0.092(6) 0.070(6) 0.066(5) 0.012(5) 0.028(5) 0.008(5) C12 0.097(7) 0.057(5) 0.062(5) -0.012(4) 0.013(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C5 1.835(9) . y Rh1 C6 1.851(9) . y Rh1 O1 2.079(5) . y Rh1 O2 2.088(5) . y Rh1 Rh1 2.9844(12) 6 n Rh1 Rh2 3.0915(9) . y Rh2 C12 1.830(11) . y Rh2 C11 1.839(9) . y Rh2 O5 2.090(6) . y Rh2 O6 2.091(6) . y Rh2 Rh2 2.9936(12) 6_565 y O1 C1 1.244(7) . n O2 C2 1.228(7) . n O3 C5 1.122(10) . y O4 C6 1.121(9) . y O5 C7 1.228(7) . n O6 C8 1.230(7) . n O7 C11 1.116(10) . y O8 C12 1.123(10) . y C1 O1 1.244(7) 6 n C1 C3 1.57(2) . n C2 O2 1.228(7) 6 n C2 C4 1.54(2) . n C3 F1 1.31(3) . n C3 F2 1.35(2) 6 n C3 F2 1.35(2) . n C3 F2X 1.26(2) . n C3 F3X 1.29(2) . n C3 F1X 1.41(2) . n C4 F4 1.08(3) . n C4 F5 1.27(2) . n C4 F5 1.27(2) 6 n C4 F4X 1.10(3) . n C4 F5X 1.28(2) . n C4 F4Y 1.35(2) . n C4 F6Y 1.40(2) . n C4 F5Y 1.54(2) . n C7 O5 1.228(7) 6_565 n C7 C9 1.57(2) . n C8 O6 1.230(7) 6_565 n C8 C10 1.54(2) . n C9 F8 1.331(15) . n C9 F8 1.331(15) 6_565 n C9 F7 1.34(2) . n C9 F9X 1.24(2) . n C9 F8X 1.25(2) . n C9 F7X 1.43(2) . n C10 F10 1.16(3) . n C10 F11 1.30(2) . n C10 F11 1.30(2) 6_565 n C10 F10X 1.17(3) . n C10 F11X 1.34(2) . n C10 F11Y 1.36(4) . n C10 F12Y 1.40(3) . n C10 F10Y 1.57(3) . n loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Rh1 C6 89.2(4) . . y C5 Rh1 O1 177.4(3) . . y C6 Rh1 O1 93.2(3) . . y C5 Rh1 O2 93.2(3) . . y C6 Rh1 O2 176.6(3) . . y O1 Rh1 O2 84.5(2) . . y C5 Rh1 Rh1 98.7(3) . 6 y C6 Rh1 Rh1 102.6(3) . 6 y O1 Rh1 Rh1 79.9(2) . 6 y O2 Rh1 Rh1 79.4(2) . 6 y C5 Rh1 Rh2 90.0(2) . . y C6 Rh1 Rh2 93.0(3) . . y O1 Rh1 Rh2 90.8(2) . . y O2 Rh1 Rh2 84.7(2) . . y Rh1 Rh1 Rh2 162.232(14) 6 . y C12 Rh2 C11 88.8(4) . . y C12 Rh2 O5 91.9(3) . . y C11 Rh2 O5 177.6(3) . . y C12 Rh2 O6 177.2(3) . . y C11 Rh2 O6 93.3(3) . . y O5 Rh2 O6 85.8(2) . . y C12 Rh2 Rh2 101.8(3) . 6_565 n C11 Rh2 Rh2 102.6(3) . 6_565 n O5 Rh2 Rh2 79.5(2) . 6_565 n O6 Rh2 Rh2 79.4(2) . 6_565 n C12 Rh2 Rh1 88.2(3) . . n C11 Rh2 Rh1 92.1(3) . . n O5 Rh2 Rh1 85.6(2) . . n O6 Rh2 Rh1 90.0(2) . . n Rh2 Rh2 Rh1 162.231(14) 6_565 . y C1 O1 Rh1 125.1(6) . . n C2 O2 Rh1 125.8(5) . . n C7 O5 Rh2 125.2(6) . . n C8 O6 Rh2 125.8(6) . . n O1 C1 O1 129.7(10) . 6 n O1 C1 C3 115.1(5) . . n O2 C2 O2 129.1(9) 6 . n O2 C2 C4 115.5(5) . . n F1 C3 F2 103.4(16) . . n F2 C3 F2 112.4(27) 6 . n F1 C3 C1 111.2(19) . . n F2 C3 C1 112.8(12) . . n F2X C3 F3X 115.5(15) . . n F2X C3 F1X 116.4(18) . . n F3X C3 F1X 99.5(21) . . n F2X C3 C1 109.6(12) . . n F3X C3 C1 106.9(15) . . n F1X C3 C1 108.2(12) . . n F4 C4 F5 99.3(20) . . n F5 C4 F5 96.8(27) . 6 n F4 C4 C2 128.1(29) . . n F5 C4 C2 114.0(11) . . n F4X C4 F5X 98.7(15) . . n F4X C4 C2 124.6(21) . . n F5X C4 C2 111.6(11) . . n F4Y C4 F6Y 128.4(12) . . n F4Y C4 F5Y 105.6(15) . . n F6Y C4 F5Y 99.4(14) . . n F4Y C4 C2 109.0(11) . . n F6Y C4 C2 105.1(12) . . n F5Y C4 C2 107.5(7) . . n O3 C5 Rh1 177.3(8) . . n O4 C6 Rh1 178.6(9) . . n O5 C7 O5 130.4(10) . 6_565 n O5 C7 C9 114.8(5) . . n O6 C8 O6 129.4(10) 6_565 . n O6 C8 C10 115.3(5) . . n F8 C9 F8 112.7(18) . 6_565 n F8 C9 F7 106.0(10) . . n F8 C9 C7 112.3(8) . . n F7 C9 C7 106.9(12) . . n F9X C9 F8X 109.0(16) . . n F9X C9 F7X 103.8(24) . . n F8X C9 F7X 113.6(18) . . n F9X C9 C7 110.9(15) . . n F8X C9 C7 112.1(12) . . n F7X C9 C7 107.0(11) . . n F10 C10 F11 104.3(18) . . n F11 C10 F11 107.0(30) . 6_565 n F10 C10 C8 119.4(23) . . n F11 C10 C8 110.5(13) . . n F10X C10 F11X 100.6(16) . . n F10X C10 C8 122.0(23) . . n F11X C10 C8 114.3(11) . . n F11Y C10 F12Y 125.6(18) . . n F11Y C10 C8 105.5(16) . . n F12Y C10 C8 102.8(14) . . n F11Y C10 F10Y 107.5(24) . . n F12Y C10 F10Y 107.4(23) . . n C8 C10Y F10Y 106.6(12) . . n O7 C11 Rh2 178.9(9) . . n O8 C12 Rh2 179.3(9) . . n loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Rh1 Rh1 O1 0.0 . . 6 6 n O2 Rh1 Rh1 O2 0.0 . . 6 6 n C5 Rh1 Rh1 C5 0.0 . . 6 6 n C6 Rh1 Rh1 C6 0.0 . . 6 6 n O5 Rh2 Rh2 O5 0.0 . . 1_545 1_545 n O6 Rh2 Rh2 O6 0.0 . . 1_545 1_545 n C11 Rh2 Rh2 C11 0.0 . . 1_545 1_545 n C12 Rh2 Rh2 C12 0.0 . . 1_545 1_545 n O1 Rh1 Rh2 C11 23.9(3) . . . . y O2 Rh1 Rh2 C12 28.3(3) . . . . y C5 Rh1 Rh2 O5 27.2(3) . . . . y C6 Rh1 Rh2 O6 23.8(3) . . . . y _refine_diff_density_max 0.833 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.153 #===END data_[Rh(O2CCF3)(CO)(THF)]4_(3) _audit_creation_method SHELXL _chemical_name_systematic ; Tetrakis((\m-trifluoroacetato-O,O')-(\m-carbonyl)-tetrahydrofuran)- tetra-rhodium(I) ; _chemical_formula_moiety 'Rh4 (O2 C C F3)4 (C O)4 (O C4 H8)4' _chemical_formula_structural '[Rh(\m-O2CCF3)(\m-CO)(THF)]4' _chemical_formula_analytical 'not measured' _chemical_formula_sum 'C28 H32 F12 O16 Rh4' _chemical_formula_weight 1264.18 _chemical_melting_point 'not measured' _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 10.140(1) _cell_length_b 22.979(3) _cell_length_c 8.786(1) _cell_angle_alpha 90.00 _cell_angle_beta 102.636(2) _cell_angle_gamma 90.00 _cell_volume 1997.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3351 _cell_measurement_theta_min 4.48 _cell_measurement_theta_max 54.90 _exptl_crystal_description 'plate-shaped' _exptl_crystal_colour 'pale-green' _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.102 _exptl_crystal_density_method none _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 1.746 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7339 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART CCD' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6257 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2331 _reflns_number_observed 1675 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXTL V.5 (Siemens, 1994)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL V.5 (Siemens, 1994)' _computing_publication_material CIFTAB _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+11.8501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef noref _refine_ls_number_reflns 2331 _refine_ls_number_parameters 175 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_obs 0.0514 _refine_ls_wR_factor_all 0.1462 _refine_ls_wR_factor_obs 0.1259 _refine_ls_goodness_of_fit_all 1.084 _refine_ls_goodness_of_fit_obs 1.116 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.175 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 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 Rh1 Rh 0.09225(5) 0.05710(2) 0.42188(6) 0.0364(2) Uani 1 d . . C1 C 0.2096(10) 0.0000 0.5517(12) 0.043(2) Uani 1 d S . O1 O 0.3044(8) 0.0000 0.6535(9) 0.061(2) Uani 1 d S . C2 C -0.0017(10) 0.0000 0.2713(11) 0.039(2) Uani 1 d S . O2 O -0.0765(8) 0.0000 0.1508(9) 0.058(2) Uani 1 d S . O3 O -0.0192(7) 0.1274(3) 0.2941(8) 0.068(2) Uani 1 d . . O4 O 0.1821(6) 0.1270(3) 0.5746(9) 0.072(2) Uani 1 d . . C3 C -0.1211(8) 0.1474(4) 0.3322(11) 0.057(2) Uani 1 d . . C4 C -0.1746(11) 0.2065(5) 0.2596(16) 0.089(4) Uani 1 d D 1 F1 F -0.3073(20) 0.2144(25) 0.2335(50) 0.134(28) Uiso 0.25 d PD 1 F2 F -0.1483(26) 0.2058(12) 0.1047(22) 0.052(6) Uiso 0.25 d PD 1 F3 F -0.0998(32) 0.2491(13) 0.3232(45) 0.082(10) Uiso 0.25 d PD 1 F1X F -0.3046(17) 0.1999(11) 0.1863(30) 0.062(7) Uiso 0.250(7) d PD 2 F2X F -0.1037(34) 0.2263(18) 0.1670(41) 0.100(19) Uiso 0.25 d PD 2 F3X F -0.1601(33) 0.2499(12) 0.3726(29) 0.086(10) Uiso 0.25 d PD 2 F1Y F -0.2863(21) 0.2238(11) 0.3028(33) 0.062(7) Uiso 0.250(7) d PD 3 F2Y F -0.2071(52) 0.1969(22) 0.1013(30) 0.180(24) Uiso 0.25 d PD 3 F3Y F -0.0812(32) 0.2461(17) 0.2704(57) 0.138(19) Uiso 0.25 d PD 3 F1Z F -0.3055(12) 0.2134(9) 0.2462(28) 0.026(4) Uiso 0.250(7) d PD 4 F2Z F -0.1328(29) 0.2242(12) 0.1442(28) 0.043(6) Uiso 0.25 d PD 4 F3Z F -0.1076(27) 0.2488(10) 0.3786(27) 0.052(6) Uiso 0.25 d PD 4 O5 O 0.2486(6) 0.0741(3) 0.2857(7) 0.0562(15) Uani 1 d D 4 C5 C 0.2118(18) 0.1205(9) 0.1489(23) 0.034(4) Uiso 0.35 d PD 4 C6 C 0.3474(26) 0.1200(13) 0.0953(30) 0.053(7) Uiso 0.35 d PD 4 C7 C 0.4577(19) 0.1117(11) 0.2485(26) 0.037(5) Uiso 0.35 d PD 4 C8 C 0.3791(25) 0.0974(15) 0.3715(28) 0.074(9) Uiso 0.35 d PD 4 C5X C 0.2304(17) 0.0550(8) 0.1293(19) 0.033(4) Uiso 0.350(3) d PD 5 C6X C 0.3624(21) 0.0734(10) 0.0835(23) 0.042(5) Uiso 0.35 d PD 5 C7X C 0.4207(21) 0.1235(9) 0.1989(26) 0.033(4) Uiso 0.35 d PD 5 C8X C 0.3265(21) 0.1273(9) 0.3122(25) 0.045(5) Uiso 0.35 d PD 5 C5Y C 0.1902(52) 0.1027(23) 0.1075(59) 0.099(15) Uiso 0.300(3) d P 6 C6Y C 0.3295(40) 0.1051(19) 0.0590(47) 0.062(10) Uiso 0.30 d P 6 C7Y C 0.4412(28) 0.0974(13) 0.1939(35) 0.040(6) Uiso 0.30 d P 6 C8Y C 0.3766(25) 0.0759(12) 0.3320(31) 0.038(5) Uiso 0.30 d P 6 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 0.0344(3) 0.0416(3) 0.0367(3) -0.0006(3) 0.0152(2) -0.0032(2) C1 0.033(5) 0.055(7) 0.042(6) 0.000 0.012(4) 0.000 O1 0.040(4) 0.095(7) 0.042(4) 0.000 -0.004(4) 0.000 C2 0.035(5) 0.055(6) 0.027(5) 0.000 0.009(4) 0.000 O2 0.054(5) 0.088(6) 0.030(4) 0.000 0.004(3) 0.000 O3 0.072(4) 0.057(4) 0.086(5) 0.033(3) 0.040(4) 0.014(3) O4 0.050(3) 0.074(4) 0.100(5) -0.046(4) 0.033(4) -0.021(3) C3 0.042(4) 0.053(5) 0.076(6) 0.027(4) 0.011(4) -0.001(4) C4 0.058(6) 0.087(8) 0.124(11) 0.043(8) 0.025(7) 0.001(6) O5 0.054(3) 0.063(4) 0.061(4) -0.002(3) 0.033(3) -0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C2 1.956(7) . y Rh1 C1 1.961(8) . y Rh1 O3 2.143(6) . y Rh1 O4 2.163(6) . y Rh1 O5 2.220(5) . y Rh1 Rh1 2.5510(10) 2_556 y Rh1 Rh1 2.6241(12) 6 y C1 O1 1.161(12) . y C1 Rh1 1.961(8) 6 n C2 O2 1.160(12) . y C2 Rh1 1.956(7) 6 n O3 C3 1.242(10) . n O4 C3 1.223(10) 2_556 n C3 O4 1.223(10) 2_556 n C3 C4 1.546(13) . n C4 F3 1.29(2) . n C4 F1 1.33(2) . n C4 F2 1.44(2) . n C4 F2X 1.28(2) . n C4 F1X 1.34(2) . n C4 F3X 1.39(2) . n C4 F3Y 1.30(2) . n C4 F1Y 1.33(2) . n C4 F2Y 1.37(2) . n C4 F2Z 1.25(2) . n C4 F1Z 1.32(2) . n C4 F3Z 1.48(2) . n O5 C8 1.47(2) . n O5 C5 1.59(2) . n C5 C6 1.55(3) . n C6 C7 1.56(3) . n C7 C8 1.51(3) . n O5 C5X 1.42(2) . n O5 C8X 1.45(2) . n C5X C6X 1.54(2) . n C6X C7X 1.56(3) . n C7X C8X 1.53(2) . n O5 C8Y 1.27(3) . n O5 C5Y 1.68(5) . n C5Y C6Y 1.56(6) . n C6Y C7Y 1.46(5) . n C7Y C8Y 1.58(4) . n loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Rh1 C1 95.1(3) . . y C2 Rh1 O3 91.6(3) . . y C1 Rh1 O3 173.0(3) . . y C2 Rh1 O4 174.0(3) . . y C1 Rh1 O4 91.0(3) . . y O3 Rh1 O4 82.4(3) . . y C2 Rh1 O5 93.0(3) . . y C1 Rh1 O5 91.0(3) . . y O3 Rh1 O5 86.7(2) . . y O4 Rh1 O5 87.1(2) . . y C2 Rh1 Rh1 93.3(3) . 2_556 n C1 Rh1 Rh1 96.3(3) . 2_556 n O3 Rh1 Rh1 85.3(2) . 2_556 n O4 Rh1 Rh1 85.7(2) . 2_556 n O5 Rh1 Rh1 169.8(2) . 2_556 n C2 Rh1 Rh1 47.9(2) . 6 n C1 Rh1 Rh1 48.0(2) . 6 n O3 Rh1 Rh1 138.9(2) . 6 n O4 Rh1 Rh1 138.0(2) . 6 n O5 Rh1 Rh1 100.2(2) . 6 n Rh1 Rh1 Rh1 90.0 2_556 6 y O1 C1 Rh1 138.0(2) . 6 n O1 C1 Rh1 138.0(2) . . n Rh1 C1 Rh1 84.0(4) 6 . n O2 C2 Rh1 137.9(2) . 6 n O2 C2 Rh1 137.9(2) . . n Rh1 C2 Rh1 84.2(4) 6 . n C3 O3 Rh1 120.8(5) . . n C3 O4 Rh1 119.6(5) 2_556 . n O4 C3 O3 127.7(8) 2_556 . n O4 C3 C4 115.4(8) 2_556 . n O3 C3 C4 116.8(8) . . n F3 C4 F1 116.6(24) . . n F3 C4 F2 101.8(21) . . n F1 C4 F2 103.2(21) . . n F3 C4 C3 111.6(20) . . n F1 C4 C3 116.3(27) . . n F2 C4 C3 105.1(13) . . n F2X C4 F1X 111.3(21) . . n F2X C4 F3X 102.3(19) . . n F1X C4 F3X 111.2(18) . . n F2X C4 C3 112.3(21) . . n F1X C4 C3 108.6(13) . . n F3X C4 C3 111.2(16) . . n F3Y C4 F1Y 114.8(23) . . n F3Y C4 F2Y 101.3(22) . . n F1Y C4 F2Y 107.8(22) . . n F3Y C4 C3 113.6(22) . . n F1Y C4 C3 112.8(13) . . n F2Y C4 C3 105.3(25) . . n F2Z C4 F1Z 113.7(17) . . n F2Z C4 F3Z 100.1(18) . . n F1Z C4 F3Z 106.4(16) . . n F2Z C4 C3 118.1(15) . . n F1Z C4 C3 113.5(11) . . n F3Z C4 C3 102.7(13) . . n C8 O5 C5 100.3(13) . . n C8 O5 Rh1 117.1(11) . . n C5 O5 Rh1 116.7(7) . . n C6 C5 O5 98.5(14) . . n C5 C6 C7 104.8(16) . . n C8 C7 C6 104.6(15) . . n O5 C8 C7 105.5(16) . . n C5X O5 C8X 111.7(11) . . n C5X O5 Rh1 120.8(7) . . n C8X O5 Rh1 119.4(8) . . n O5 C5X C6X 103.5(12) . . n C5X C6X C7X 105.1(14) . . n C8X C7X C6X 105.3(14) . . n O5 C8X C7X 104.1(13) . . n C8Y O5 C5Y 114.3(21) . . n C8Y O5 Rh1 129.2(12) . . n C5Y O5 Rh1 115.1(18) . . n C6Y C5Y O5 96.4(31) . . n C7Y C6Y C5Y 111.2(32) . . n C6Y C7Y C8Y 106.4(23) . . n O5 C8Y C7Y 109.2(21) . . n _refine_diff_density_max 0.865 _refine_diff_density_min -1.312 _refine_diff_density_rms 0.157 #===END data_Rh2(O2CCF3)2(1,5-cod)2_(4) _audit_creation_method SHELXL _chemical_name_systematic ; Bis(\m-trifluoroacetato-O,O')-bis(\n4-cyclo-octa-1,5-diene)- di-rhodium(I) ; _chemical_formula_moiety 'Rh2 (O2 C C F3)2 (C8 H12)2' _chemical_formula_structural 'Rh2(O2CCF3)2(\n4-1,5-cod)2' _chemical_formula_analytical 'not measured' _chemical_formula_sum 'C20 H24 F6 O4 Rh2' _chemical_formula_weight 648.21 _chemical_melting_point 'not measured' _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.3351(9) _cell_length_b 16.5713(5) _cell_length_c 29.009(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8814.0(8) _cell_formula_units_Z 16 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 249 _cell_measurement_theta_min 9.05 _cell_measurement_theta_max 20.8 _exptl_crystal_description 'block-shaped' _exptl_crystal_colour 'pale-yellow' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.954 _exptl_crystal_density_method none _exptl_crystal_F_000 5120 _exptl_absorpt_coefficient_mu 1.573 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius FAST area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34582 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 22.51 _reflns_number_total 5731 _reflns_number_observed 5225 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MADNES (Enraf-Nonius, 1989)' _computing_cell_refinement 'MADNES (Enraf-Nonius, 1989)' _computing_data_reduction 'PROCOR (Kabsch, 1988)' _computing_structure_solution 'SHELXTL V.5 (Siemens, 1994)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL V.5 (Siemens, 1994)' _computing_publication_material CIFTAB _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+42.8251P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'refined on alkene C atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef noref _refine_ls_number_reflns 5731 _refine_ls_number_parameters 625 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_obs 0.0361 _refine_ls_wR_factor_all 0.0906 _refine_ls_wR_factor_obs 0.0847 _refine_ls_goodness_of_fit_all 1.088 _refine_ls_goodness_of_fit_obs 1.083 _refine_ls_restrained_S_all 1.106 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 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 Rh1 Rh 0.40332(2) 0.11941(3) -0.189687(15) 0.02924(14) Uani 1 d . . Rh2 Rh 0.50750(2) 0.03527(3) -0.278852(14) 0.02909(14) Uani 1 d . . Rh3 Rh 0.15189(2) 0.02659(2) 0.064616(15) 0.02563(13) Uani 1 d . . Rh4 Rh 0.28310(2) -0.08393(3) 0.00635(2) 0.02786(14) Uani 1 d . . O1 O 0.4766(2) 0.0366(2) -0.15958(14) 0.0416(10) Uani 1 d . . O2 O 0.3456(2) 0.0224(3) -0.2190(2) 0.0477(12) Uani 1 d . . O3 O 0.5480(3) -0.0084(3) -0.21645(14) 0.0529(13) Uani 1 d . . O4 O 0.4159(3) -0.0394(3) -0.2707(2) 0.0509(12) Uani 1 d . . O5 O 0.1019(2) -0.0843(2) 0.0492(2) 0.0435(11) Uani 1 d . . O6 O 0.2092(2) -0.0344(3) 0.11601(14) 0.0477(11) Uani 1 d . . O7 O 0.1861(2) -0.1521(2) 0.0097(2) 0.0500(12) Uani 1 d . . O8 O 0.2961(2) -0.1009(3) 0.07825(15) 0.0495(12) Uani 1 d . . C1 C 0.5268(3) -0.0043(3) -0.1765(2) 0.0258(12) Uani 1 d . . C2 C 0.3622(3) -0.0323(3) -0.2454(2) 0.0310(13) Uani 1 d . . C3 C 0.5663(3) -0.0598(4) -0.1431(2) 0.0331(13) Uani 1 d D 1 F1 F 0.5560(5) -0.0377(5) -0.0988(3) 0.043(2) Uiso 0.50 d PD 1 F2 F 0.5447(6) -0.1332(5) -0.1478(3) 0.060(3) Uiso 0.50 d PD 1 F3 F 0.6388(4) -0.0568(5) -0.1500(2) 0.039(2) Uiso 0.50 d PD 1 F1X F 0.5792(6) -0.0267(6) -0.1033(3) 0.061(3) Uiso 0.500(2) d PD 2 F2X F 0.5235(5) -0.1267(5) -0.1349(3) 0.048(2) Uiso 0.50 d PD 2 F3X F 0.6276(4) -0.0923(6) -0.1595(3) 0.056(2) Uiso 0.50 d PD 2 C4 C 0.3081(3) -0.1024(4) -0.2472(2) 0.043(2) Uani 1 d D 1 F4 F 0.2425(6) -0.0793(6) -0.2563(6) 0.057(3) Uiso 0.40 d PD 1 F5 F 0.3277(6) -0.1594(7) -0.2787(4) 0.050(3) Uiso 0.40 d PD 1 F6 F 0.3095(7) -0.1417(7) -0.2067(3) 0.051(3) Uiso 0.40 d PD 1 F4X F 0.2546(6) -0.0863(6) -0.2778(4) 0.040(2) Uiso 0.400(3) d PD 2 F5X F 0.3398(5) -0.1719(6) -0.2607(5) 0.048(3) Uiso 0.40 d PD 2 F6X F 0.2770(8) -0.1154(7) -0.2072(3) 0.054(3) Uiso 0.40 d PD 2 F4Y F 0.2449(10) -0.0855(11) -0.2229(8) 0.045(5) Uiso 0.200(3) d PD 3 F5Y F 0.2833(14) -0.1200(16) -0.2897(6) 0.069(6) Uiso 0.20 d PD 3 F6Y F 0.3333(11) -0.1689(11) -0.2296(10) 0.059(5) Uiso 0.20 d PD 3 C5 C 0.1283(3) -0.1440(3) 0.0309(2) 0.0236(12) Uani 1 d . . C6 C 0.2608(3) -0.0811(3) 0.1127(2) 0.0296(13) Uani 1 d . . C7 C 0.0841(3) -0.2216(3) 0.0356(2) 0.0316(13) Uani 1 d D 1 F7 F 0.0124(4) -0.2026(5) 0.0407(3) 0.031(3) Uiso 0.50 d PD 1 F8 F 0.0914(4) -0.2733(5) 0.0021(3) 0.035(2) Uiso 0.50 d PD 1 F9 F 0.1101(5) -0.2603(6) 0.0738(3) 0.043(3) Uiso 0.50 d PD 1 F7X F 0.0171(4) -0.2132(5) 0.0517(3) 0.035(3) Uiso 0.500(3) d PD 2 F8X F 0.0786(4) -0.2579(5) -0.0079(3) 0.036(2) Uiso 0.50 d PD 2 F9X F 0.1133(5) -0.2743(6) 0.0634(3) 0.047(3) Uiso 0.50 d PD 2 C8 C 0.2820(3) -0.1252(4) 0.1567(2) 0.0386(15) Uani 1 d D 1 F10 F 0.3568(4) -0.1206(5) 0.1622(3) 0.038(2) Uiso 0.50 d PD 1 F11 F 0.2504(5) -0.0994(5) 0.1943(3) 0.042(2) Uiso 0.50 d PD 1 F12 F 0.2659(6) -0.2030(5) 0.1543(3) 0.052(3) Uiso 0.50 d PD 1 F10X F 0.3491(4) -0.1502(6) 0.1590(3) 0.054(3) Uiso 0.500(3) d PD 2 F11X F 0.2683(5) -0.0780(5) 0.1944(3) 0.044(3) Uiso 0.50 d PD 2 F12X F 0.2408(6) -0.1931(5) 0.1604(3) 0.058(3) Uiso 0.50 d PD 2 C1A C 0.4736(3) 0.2155(4) -0.1753(2) 0.0359(14) Uani 1 d . . H1A H 0.5180(37) 0.1907(38) -0.1751(21) 0.043 Uiso 1 d . . C2A C 0.4286(3) 0.2019(4) -0.1371(2) 0.0356(14) Uani 1 d . . H2A H 0.4464(34) 0.1729(38) -0.1144(22) 0.043 Uiso 1 d . . C3A C 0.3651(3) 0.2554(4) -0.1238(2) 0.043(2) Uani 1 d . . H3A1 H 0.3756(3) 0.3110(4) -0.1334(2) 0.052 Uiso 1 calc R . H3A2 H 0.3596(3) 0.2550(4) -0.0902(2) 0.052 Uiso 1 calc R . C4A C 0.2941(3) 0.2281(4) -0.1459(2) 0.047(2) Uani 1 d . . H4A1 H 0.2685(3) 0.1921(4) -0.1245(2) 0.056 Uiso 1 calc R . H4A2 H 0.2631(3) 0.2753(4) -0.1512(2) 0.056 Uiso 1 calc R . C5A C 0.3052(3) 0.1846(4) -0.1910(2) 0.041(2) Uani 1 d . . H5A H 0.2714(37) 0.1471(41) -0.1974(23) 0.050 Uiso 1 d . . C6A C 0.3487(3) 0.2103(4) -0.2278(2) 0.0388(15) Uani 1 d . . H6A H 0.3415(35) 0.1830(39) -0.2540(24) 0.047 Uiso 1 d . . C7A C 0.3884(4) 0.2907(4) -0.2270(2) 0.051(2) Uani 1 d . . H7A1 H 0.3897(4) 0.3128(4) -0.2584(2) 0.061 Uiso 1 calc R . H7A2 H 0.3611(4) 0.3286(4) -0.2077(2) 0.061 Uiso 1 calc R . C8A C 0.4653(4) 0.2836(4) -0.2090(2) 0.049(2) Uani 1 d . . H8A1 H 0.4987(4) 0.2751(4) -0.2349(2) 0.059 Uiso 1 calc R . H8A2 H 0.4790(4) 0.3343(4) -0.1939(2) 0.059 Uiso 1 calc R . C1B C 0.4569(4) 0.1004(4) -0.3311(2) 0.045(2) Uani 1 d . . H1B H 0.4098(40) 0.0967(42) -0.3241(24) 0.054 Uiso 1 d . . C2B C 0.4925(4) 0.0342(4) -0.3505(2) 0.041(2) Uani 1 d . . H2B H 0.4619(38) -0.0072(42) -0.3580(23) 0.050 Uiso 1 d . . C3B C 0.5628(4) 0.0403(5) -0.3773(2) 0.057(2) Uani 1 d . . H3B1 H 0.5648(4) 0.0927(5) -0.3929(2) 0.068 Uiso 1 calc R . H3B2 H 0.5637(4) -0.0018(5) -0.4011(2) 0.068 Uiso 1 calc R . C4B C 0.6294(4) 0.0311(5) -0.3465(2) 0.054(2) Uani 1 d . . H4B1 H 0.6452(4) -0.0254(5) -0.3470(2) 0.065 Uiso 1 calc R . H4B2 H 0.6692(4) 0.0638(5) -0.3592(2) 0.065 Uiso 1 calc R . C5B C 0.6159(3) 0.0564(5) -0.2969(2) 0.045(2) Uani 1 d . . H5B H 0.6442(39) 0.0314(41) -0.2744(25) 0.054 Uiso 1 d . . C6B C 0.5843(4) 0.1292(5) -0.2839(2) 0.050(2) Uani 1 d . . H6B H 0.5924(38) 0.1466(43) -0.2565(27) 0.059 Uiso 1 d . . C7B C 0.5609(5) 0.1946(5) -0.3177(3) 0.063(2) Uani 1 d . . H7B1 H 0.5680(5) 0.2475(5) -0.3034(3) 0.075 Uiso 1 calc R . H7B2 H 0.5921(5) 0.1920(5) -0.3451(3) 0.075 Uiso 1 calc R . C8B C 0.4824(5) 0.1861(5) -0.3322(3) 0.068(2) Uani 1 d . . H8B1 H 0.4517(5) 0.2184(5) -0.3116(3) 0.081 Uiso 1 calc R . H8B2 H 0.4766(5) 0.2074(5) -0.3635(3) 0.081 Uiso 1 calc R . C1C C 0.1131(3) 0.0851(4) 0.0056(2) 0.0398(15) Uani 1 d . . H1C H 0.1082(36) 0.0419(41) -0.0155(23) 0.048 Uiso 1 d . . C2C C 0.0599(3) 0.0864(4) 0.0397(2) 0.0353(14) Uani 1 d . . H2C H 0.0291(37) 0.0512(40) 0.0406(22) 0.042 Uiso 1 d . . C3C C 0.0415(4) 0.1572(4) 0.0696(3) 0.058(2) Uani 1 d . . H3C1 H 0.0201(4) 0.1994(4) 0.0503(3) 0.069 Uiso 1 calc R . H3C2 H 0.0043(4) 0.1404(4) 0.0919(3) 0.069 Uiso 1 calc R . C4C C 0.1044(4) 0.1924(4) 0.0955(3) 0.069(2) Uani 1 d . . H4C1 H 0.0880(4) 0.2074(4) 0.1266(3) 0.082 Uiso 1 calc R . H4C2 H 0.1204(4) 0.2418(4) 0.0799(3) 0.082 Uiso 1 calc R . C5C C 0.1677(4) 0.1358(4) 0.0995(3) 0.050(2) Uani 1 d . . H5C H 0.1776(42) 0.1218(46) 0.1255(27) 0.060 Uiso 1 d . . C6C C 0.2212(4) 0.1269(4) 0.0671(3) 0.045(2) Uani 1 d . . H6C H 0.2637(41) 0.1077(41) 0.0807(24) 0.054 Uiso 1 d . . C7C C 0.2237(5) 0.1696(5) 0.0220(3) 0.072(2) Uani 1 d . . H7C1 H 0.2664(5) 0.1507(5) 0.0048(3) 0.086 Uiso 1 calc R . H7C2 H 0.2302(5) 0.2275(5) 0.0278(3) 0.086 Uiso 1 calc R . C8C C 0.1575(4) 0.1581(5) -0.0070(3) 0.073(3) Uani 1 d . . H8C1 H 0.1726(4) 0.1534(5) -0.0393(3) 0.088 Uiso 1 calc R . H8C2 H 0.1266(4) 0.2061(5) -0.0044(3) 0.088 Uiso 1 calc R . C1D C 0.3647(3) 0.0039(4) -0.0019(2) 0.0327(13) Uani 1 d . . H1D H 0.3618(32) 0.0362(36) 0.0271(22) 0.039 Uiso 1 d . . C2D C 0.3971(3) -0.0702(4) 0.0042(2) 0.0347(14) Uani 1 d . . H2D H 0.4125(33) -0.0833(36) 0.0369(23) 0.042 Uiso 1 d . . C3D C 0.4293(4) -0.1222(4) -0.0319(3) 0.058(2) Uani 1 d . . H3D1 H 0.4414(4) -0.1746(4) -0.0183(3) 0.069 Uiso 1 calc R . H3D2 H 0.4748(4) -0.0976(4) -0.0427(3) 0.069 Uiso 1 calc R . C4D C 0.3786(4) -0.1356(4) -0.0734(2) 0.055(2) Uani 1 d . . H4D1 H 0.3907(4) -0.0964(4) -0.0976(2) 0.066 Uiso 1 calc R . H4D2 H 0.3870(4) -0.1897(4) -0.0859(2) 0.066 Uiso 1 calc R . C5D C 0.2986(4) -0.1269(4) -0.0609(2) 0.041(2) Uani 1 d . . H5D H 0.2720(36) -0.1699(42) -0.0638(22) 0.049 Uiso 1 d . . C6D C 0.2617(4) -0.0529(4) -0.0621(2) 0.0399(15) Uani 1 d . . H6D H 0.2092(38) -0.0572(39) -0.0670(22) 0.048 Uiso 1 d . . C7D C 0.2967(4) 0.0242(4) -0.0764(2) 0.053(2) Uani 1 d . . H7D1 H 0.2607(4) 0.0677(4) -0.0737(2) 0.063 Uiso 1 calc R . H7D2 H 0.3106(4) 0.0202(4) -0.1089(2) 0.063 Uiso 1 calc R . C8D C 0.3626(4) 0.0464(4) -0.0488(2) 0.050(2) Uani 1 d . . H8D1 H 0.3631(4) 0.1049(4) -0.0439(2) 0.060 Uiso 1 calc R . H8D2 H 0.4065(4) 0.0321(4) -0.0663(2) 0.060 Uiso 1 calc R . 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 0.0265(3) 0.0296(3) 0.0317(3) -0.0016(2) -0.0010(2) 0.0020(2) Rh2 0.0251(3) 0.0410(3) 0.0212(2) 0.0055(2) 0.0018(2) -0.0029(2) Rh3 0.0265(3) 0.0218(2) 0.0286(3) -0.0012(2) -0.0035(2) 0.0024(2) Rh4 0.0232(2) 0.0299(3) 0.0304(3) 0.0045(2) 0.0067(2) 0.0006(2) O1 0.050(3) 0.043(2) 0.032(2) 0.005(2) 0.004(2) 0.020(2) O2 0.037(3) 0.044(3) 0.062(3) -0.018(2) 0.013(2) -0.012(2) O3 0.058(3) 0.079(3) 0.022(2) 0.016(2) 0.007(2) 0.026(3) O4 0.048(3) 0.047(3) 0.057(3) -0.008(2) 0.019(2) -0.019(2) O5 0.042(3) 0.024(2) 0.064(3) -0.013(2) 0.017(2) -0.006(2) O6 0.051(3) 0.057(3) 0.035(2) 0.007(2) -0.002(2) 0.022(2) O7 0.034(3) 0.036(2) 0.080(3) -0.007(2) 0.026(2) -0.008(2) O8 0.043(3) 0.074(3) 0.032(2) 0.020(2) 0.009(2) 0.022(2) C1 0.024(3) 0.025(3) 0.028(3) 0.005(2) -0.005(2) 0.000(2) C2 0.026(3) 0.035(3) 0.033(3) 0.001(3) -0.002(3) -0.007(3) C3 0.031(3) 0.041(3) 0.028(3) -0.004(3) -0.001(2) 0.000(3) C4 0.039(4) 0.046(4) 0.044(4) 0.002(3) 0.005(3) -0.007(3) C5 0.027(3) 0.022(3) 0.022(3) 0.002(2) -0.002(2) -0.001(2) C6 0.027(3) 0.036(3) 0.025(3) 0.004(2) -0.003(3) -0.002(3) C7 0.027(3) 0.032(3) 0.036(3) -0.004(3) 0.008(3) -0.001(2) C8 0.031(3) 0.050(4) 0.035(3) 0.001(3) -0.003(3) 0.012(3) C1A 0.028(3) 0.036(3) 0.044(4) -0.011(3) -0.007(3) 0.003(3) C2A 0.043(4) 0.031(3) 0.032(3) -0.005(3) -0.012(3) 0.004(3) C3A 0.053(4) 0.047(4) 0.031(3) -0.004(3) 0.001(3) 0.011(3) C4A 0.039(4) 0.043(4) 0.058(4) -0.002(3) 0.007(3) 0.014(3) C5A 0.027(3) 0.049(4) 0.047(4) 0.001(3) -0.006(3) 0.006(3) C6A 0.024(3) 0.055(4) 0.037(4) 0.001(3) -0.008(3) 0.007(3) C7A 0.047(4) 0.050(4) 0.056(4) 0.017(3) 0.003(3) 0.011(3) C8A 0.056(4) 0.041(4) 0.050(4) 0.004(3) 0.004(3) -0.010(3) C1B 0.051(4) 0.059(4) 0.026(3) 0.003(3) -0.013(3) 0.003(4) C2B 0.042(4) 0.056(4) 0.026(3) -0.002(3) -0.008(3) -0.010(3) C3B 0.065(5) 0.077(5) 0.028(4) -0.009(3) 0.012(3) -0.011(4) C4B 0.042(4) 0.084(5) 0.037(4) -0.001(4) 0.011(3) -0.007(4) C5B 0.029(3) 0.073(5) 0.034(4) -0.004(3) 0.006(3) -0.008(3) C6B 0.040(4) 0.074(5) 0.034(4) -0.010(4) 0.003(3) -0.023(4) C7B 0.084(6) 0.050(4) 0.054(5) 0.005(4) 0.024(4) -0.016(4) C8B 0.106(7) 0.052(5) 0.045(4) 0.011(4) -0.014(4) 0.007(4) C1C 0.036(4) 0.047(4) 0.036(4) 0.006(3) -0.006(3) 0.010(3) C2C 0.026(3) 0.036(4) 0.044(4) 0.007(3) -0.008(3) 0.002(3) C3C 0.051(4) 0.048(4) 0.074(5) -0.002(4) 0.005(4) 0.029(4) C4C 0.066(5) 0.046(4) 0.095(6) -0.038(4) 0.003(4) 0.012(4) C5C 0.053(4) 0.044(4) 0.053(4) -0.025(4) -0.013(4) -0.001(3) C6C 0.037(4) 0.032(4) 0.067(5) -0.012(3) -0.006(4) -0.009(3) C7C 0.076(6) 0.048(5) 0.091(6) 0.002(4) 0.016(5) -0.022(4) C8C 0.044(4) 0.078(6) 0.097(7) 0.052(5) 0.016(4) 0.016(4) C1D 0.022(3) 0.042(4) 0.033(3) -0.002(3) 0.000(2) -0.007(3) C2D 0.020(3) 0.039(4) 0.045(4) 0.010(3) 0.006(3) -0.003(3) C3D 0.034(4) 0.049(4) 0.089(6) -0.012(4) 0.019(4) 0.000(3) C4D 0.068(5) 0.048(4) 0.048(4) -0.001(3) 0.031(4) 0.011(4) C5D 0.049(4) 0.037(4) 0.037(4) -0.009(3) 0.007(3) -0.014(3) C6D 0.037(4) 0.053(4) 0.030(3) 0.004(3) -0.008(3) -0.002(3) C7D 0.081(5) 0.043(4) 0.034(4) 0.013(3) -0.002(3) 0.004(4) C8D 0.047(4) 0.046(4) 0.056(4) 0.014(3) 0.003(3) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1A 2.091(6) . y Rh1 C5A 2.099(6) . y Rh1 C2A 2.100(6) . y Rh1 O2 2.104(4) . y Rh1 O1 2.111(4) . y Rh1 C6A 2.120(6) . y Rh1 Rh2 3.5048(6) . n Rh2 C1B 2.079(6) . y Rh2 C5B 2.085(6) . y Rh2 O3 2.087(4) . y Rh2 C2B 2.096(6) . y Rh2 O4 2.099(4) . y Rh2 C6B 2.104(7) . y Rh3 O6 2.085(4) . y Rh3 C2C 2.086(6) . y Rh3 C1C 2.093(6) . y Rh3 C6C 2.093(6) . y Rh3 C5C 2.094(6) . y Rh3 O5 2.101(4) . y Rh3 Rh4 3.4639(6) . n Rh4 C6D 2.088(6) . y Rh4 C5D 2.096(6) . y Rh4 C1D 2.101(6) . y Rh4 C2D 2.103(5) . y Rh4 O7 2.110(4) . y Rh4 O8 2.118(4) . y O1 C1 1.244(7) . n O2 C2 1.225(7) . n O3 C1 1.223(7) . n O4 C2 1.236(7) . n O5 C5 1.222(6) . n O6 C6 1.226(7) . n O7 C5 1.233(7) . n O8 C6 1.236(7) . n C1 C3 1.521(8) . n C2 C4 1.528(8) . n C3 F2 1.286(10) . n C3 F3 1.346(9) . n C3 F1 1.350(9) . n C3 F1X 1.300(10) . n C3 F3X 1.334(9) . n C3 F2X 1.379(9) . n C4 F4 1.290(11) . n C4 F6 1.343(10) . n C4 F5 1.363(10) . n C4 F6X 1.310(11) . n C4 F5X 1.347(11) . n C4 F4X 1.350(10) . n C4 F6Y 1.30(2) . n C4 F5Y 1.35(2) . n C4 F4Y 1.38(2) . n C5 C7 1.527(8) . n C6 C8 1.521(8) . n C7 F8 1.301(9) . n C7 F7 1.359(9) . n C7 F9 1.366(10) . n C7 F9X 1.304(10) . n C7 F7X 1.321(9) . n C7 F8X 1.400(9) . n C8 F11 1.308(9) . n C8 F12 1.325(10) . n C8 F10 1.383(9) . n C8 F10X 1.299(10) . n C8 F12X 1.360(10) . n C8 F11X 1.367(10) . n C1A C2A 1.402(9) . y C1A C8A 1.500(9) . n C1A H1A 0.91(7) . n C2A C3A 1.512(9) . n C2A H2A 0.88(6) . n C3A C4A 1.520(9) . n C3A H3A1 0.98 . n C3A H3A2 0.98 . n C4A C5A 1.507(9) . n C4A H4A1 0.98 . n C4A H4A2 0.98 . n C5A C6A 1.397(9) . y C5A H5A 0.90(7) . n C6A C7A 1.518(10) . n C6A H6A 0.90(7) . n C7A C8A 1.510(10) . n C7A H7A1 0.98 . n C7A H7A2 0.98 . n C8A H8A1 0.98 . n C8A H8A2 0.98 . n C1B C2B 1.395(10) . y C1B C8B 1.495(10) . n C1B H1B 0.89(7) . n C2B C3B 1.510(9) . n C2B H2B 0.91(7) . n C3B C4B 1.521(10) . n C3B H3B1 0.98 . n C3B H3B2 0.98 . n C4B C5B 1.520(9) . n C4B H4B1 0.98 . n C4B H4B2 0.98 . n C5B C6B 1.390(11) . y C5B H5B 0.93(7) . n C6B C7B 1.522(11) . n C6B H6B 0.86(8) . n C7B C8B 1.507(11) . n C7B H7B1 0.98 . n C7B H7B2 0.98 . n C8B H8B1 0.98 . n C8B H8B2 0.98 . n C1C C2C 1.389(9) . y C1C C8C 1.504(10) . n C1C H1C 0.95(7) . n C2C C3C 1.498(9) . n C2C H2C 0.81(7) . n C3C C4C 1.494(10) . n C3C H3C1 0.98 . n C3C H3C2 0.98 . n C4C C5C 1.496(10) . n C4C H4C1 0.98 . n C4C H4C2 0.98 . n C5C C6C 1.367(10) . y C5C H5C 0.81(7) . n C6C C7C 1.486(11) . n C6C H6C 0.93(7) . n C7C C8C 1.490(12) . n C7C H7C1 0.98 . n C7C H7C2 0.98 . n C8C H8C1 0.98 . n C8C H8C2 0.98 . n C1D C2D 1.374(9) . y C1D C8D 1.531(9) . n C1D H1D 1.00(6) . n C2D C3D 1.478(9) . n C2D H2D 1.01(7) . n C3D C4D 1.538(11) . n C3D H3D1 0.98 . n C3D H3D2 0.98 . n C4D C5D 1.517(10) . n C4D H4D1 0.98 . n C4D H4D2 0.98 . n C5D C6D 1.400(9) . y C5D H5D 0.87(7) . n C6D C7D 1.488(9) . n C6D H6D 0.98(7) . n C7D C8D 1.496(10) . n C7D H7D1 0.98 . n C7D H7D2 0.98 . n C8D H8D1 0.98 . n C8D H8D2 0.98 . n loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A Rh1 C5A 98.0(3) . . y C1A Rh1 C2A 39.1(2) . . y C5A Rh1 C2A 82.4(2) . . y C1A Rh1 O2 166.6(2) . . y C5A Rh1 O2 87.4(2) . . y C2A Rh1 O2 154.4(2) . . y C1A Rh1 O1 91.2(2) . . y C5A Rh1 O1 152.7(2) . . y C2A Rh1 O1 89.0(2) . . y O2 Rh1 O1 89.5(2) . . y C1A Rh1 C6A 81.6(2) . . y C5A Rh1 C6A 38.7(2) . . y C2A Rh1 C6A 91.1(3) . . y O2 Rh1 C6A 95.4(2) . . y O1 Rh1 C6A 168.2(2) . . y C1A Rh1 Rh2 96.6(2) . . y C5A Rh1 Rh2 131.2(2) . . y C2A Rh1 Rh2 132.5(2) . . y O2 Rh1 Rh2 70.87(12) . . y O1 Rh1 Rh2 72.51(11) . . y C6A Rh1 Rh2 99.0(2) . . y C1B Rh2 C5B 98.9(3) . . y C1B Rh2 O3 166.3(2) . . y C5B Rh2 O3 86.4(2) . . y C1B Rh2 C2B 39.0(3) . . y C5B Rh2 C2B 83.0(3) . . y O3 Rh2 C2B 154.7(2) . . y C1B Rh2 O4 91.8(2) . . y C5B Rh2 O4 152.8(2) . . y O3 Rh2 O4 89.0(2) . . y C2B Rh2 O4 90.1(2) . . y C1B Rh2 C6B 82.2(3) . . y C5B Rh2 C6B 38.8(3) . . y O3 Rh2 C6B 94.5(2) . . y C2B Rh2 C6B 91.4(3) . . y O4 Rh2 C6B 168.3(3) . . y C1B Rh2 Rh1 95.1(2) . . y C5B Rh2 Rh1 129.6(2) . . y O3 Rh2 Rh1 72.05(12) . . y C2B Rh2 Rh1 131.6(2) . . y O4 Rh2 Rh1 73.49(12) . . y C6B Rh2 Rh1 97.0(2) . . y O6 Rh3 C2C 152.3(2) . . y O6 Rh3 C1C 168.8(2) . . y C2C Rh3 C1C 38.8(3) . . y O6 Rh3 C6C 93.2(2) . . y C2C Rh3 C6C 97.2(3) . . y C1C Rh3 C6C 82.3(3) . . y O6 Rh3 C5C 90.2(2) . . y C2C Rh3 C5C 82.5(3) . . y C1C Rh3 C5C 92.4(3) . . y C6C Rh3 C5C 38.1(3) . . y O6 Rh3 O5 87.1(2) . . y C2C Rh3 O5 89.3(2) . . y C1C Rh3 O5 94.7(2) . . y C6C Rh3 O5 165.1(2) . . y C5C Rh3 O5 156.8(3) . . y O6 Rh3 Rh4 75.08(12) . . y C2C Rh3 Rh4 130.1(2) . . y C1C Rh3 Rh4 94.7(2) . . y C6C Rh3 Rh4 90.9(2) . . y C5C Rh3 Rh4 126.7(2) . . y O5 Rh3 Rh4 74.73(11) . . y C6D Rh4 C5D 39.1(3) . . y C6D Rh4 C1D 81.6(2) . . y C5D Rh4 C1D 91.9(2) . . y C6D Rh4 C2D 97.5(3) . . y C5D Rh4 C2D 82.8(3) . . y C1D Rh4 C2D 38.2(2) . . y C6D Rh4 O7 91.0(2) . . y C5D Rh4 O7 88.6(2) . . y C1D Rh4 O7 167.6(2) . . y C2D Rh4 O7 153.8(2) . . y C6D Rh4 O8 172.0(2) . . y C5D Rh4 O8 148.9(2) . . y C1D Rh4 O8 97.1(2) . . y C2D Rh4 O8 86.1(2) . . y O7 Rh4 O8 88.8(2) . . y C6D Rh4 Rh3 101.8(2) . . y C5D Rh4 Rh3 136.7(2) . . y C1D Rh4 Rh3 100.6(2) . . y C2D Rh4 Rh3 130.3(2) . . y O7 Rh4 Rh3 71.05(11) . . y O8 Rh4 Rh3 70.59(11) . . y C1 O1 Rh1 131.4(4) . . n C2 O2 Rh1 133.8(4) . . n C1 O3 Rh2 133.5(4) . . n C2 O4 Rh2 130.4(4) . . n C5 O5 Rh3 128.9(4) . . n C6 O6 Rh3 129.7(4) . . n C5 O7 Rh4 133.5(4) . . n C6 O8 Rh4 134.7(4) . . n O3 C1 O1 129.8(5) . . n O3 C1 C3 114.8(5) . . n O1 C1 C3 115.4(5) . . n O2 C2 O4 129.9(5) . . n O2 C2 C4 115.0(5) . . n O4 C2 C4 115.1(5) . . n F2 C3 F3 108.8(7) . . n F2 C3 F1 108.3(7) . . n F3 C3 F1 105.7(7) . . n F2 C3 C1 111.0(6) . . n F3 C3 C1 110.6(5) . . n F1 C3 C1 112.2(6) . . n F1X C3 F3X 109.6(7) . . n F1X C3 F2X 106.9(7) . . n F3X C3 F2X 102.5(7) . . n F1X C3 C1 113.4(6) . . n F3X C3 C1 114.6(6) . . n F2X C3 C1 109.0(5) . . n F4 C4 F6 109.9(9) . . n F4 C4 F5 108.3(9) . . n F6 C4 F5 104.3(9) . . n F4 C4 C2 112.7(7) . . n F6 C4 C2 109.0(6) . . n F5 C4 C2 112.3(6) . . n F6X C4 F5X 107.7(9) . . n F6X C4 F4X 107.2(9) . . n F5X C4 F4X 107.0(8) . . n F6X C4 C2 112.1(7) . . n F5X C4 C2 112.4(6) . . n F4X C4 C2 110.1(6) . . n F6Y C4 F5Y 107.3(14) . . n F6Y C4 F4Y 105.7(13) . . n F5Y C4 F4Y 103.1(13) . . n F6Y C4 C2 113.6(10) . . n F5Y C4 C2 114.5(11) . . n F4Y C4 C2 111.8(9) . . n O5 C5 O7 130.2(5) . . n O5 C5 C7 115.7(5) . . n O7 C5 C7 114.1(5) . . n O6 C6 O8 129.4(5) . . n O6 C6 C8 115.8(5) . . n O8 C6 C8 114.7(5) . . n F8 C7 F7 109.4(6) . . n F8 C7 F9 105.1(7) . . n F7 C7 F9 111.0(7) . . n F8 C7 C5 115.7(5) . . n F7 C7 C5 109.1(6) . . n F9 C7 C5 106.4(6) . . n F9X C7 F7X 103.5(7) . . n F9X C7 F8X 107.4(7) . . n F7X C7 F8X 107.2(6) . . n F9X C7 C5 113.7(6) . . n F7X C7 C5 115.9(6) . . n F8X C7 C5 108.6(5) . . n F11 C8 F12 105.3(8) . . n F11 C8 F10 109.0(7) . . n F12 C8 F10 106.4(7) . . n F11 C8 C6 115.4(6) . . n F12 C8 C6 111.4(6) . . n F10 C8 C6 108.9(6) . . n F10X C8 F12X 104.9(8) . . n F10X C8 F11X 108.4(7) . . n F12X C8 F11X 107.9(7) . . n F10X C8 C6 116.0(6) . . n F12X C8 C6 108.8(6) . . n F11X C8 C6 110.4(6) . . n C2A C1A C8A 125.2(6) . . n C2A C1A Rh1 70.8(3) . . n C8A C1A Rh1 112.4(4) . . n C2A C1A H1A 116.5(40) . . n C8A C1A H1A 115.8(40) . . n Rh1 C1A H1A 102.0(40) . . n C1A C2A C3A 124.1(6) . . n C1A C2A Rh1 70.1(3) . . n C3A C2A Rh1 113.4(4) . . n C1A C2A H2A 117.5(42) . . n C3A C2A H2A 114.6(42) . . n Rh1 C2A H2A 105.6(41) . . n C2A C3A C4A 112.1(5) . . n C2A C3A H3A1 109.2(4) . . n C4A C3A H3A1 109.2(4) . . n C2A C3A H3A2 109.2(3) . . n C4A C3A H3A2 109.2(3) . . n H3A1 C3A H3A2 107.9 . . n C5A C4A C3A 113.1(5) . . n C5A C4A H4A1 109.0(4) . . n C3A C4A H4A1 109.0(4) . . n C5A C4A H4A2 109.0(3) . . n C3A C4A H4A2 109.0(3) . . n H4A1 C4A H4A2 107.8 . . n C6A C5A C4A 126.4(6) . . n C6A C5A Rh1 71.5(4) . . n C4A C5A Rh1 110.2(4) . . n C6A C5A H5A 116.6(44) . . n C4A C5A H5A 114.7(44) . . n Rh1 C5A H5A 103.8(43) . . n C5A C6A C7A 122.0(6) . . n C5A C6A Rh1 69.9(4) . . n C7A C6A Rh1 113.0(4) . . n C5A C6A H6A 114.2(42) . . n C7A C6A H6A 121.7(43) . . n Rh1 C6A H6A 98.8(42) . . n C8A C7A C6A 112.6(5) . . n C8A C7A H7A1 109.1(4) . . n C6A C7A H7A1 109.1(4) . . n C8A C7A H7A2 109.1(4) . . n C6A C7A H7A2 109.1(4) . . n H7A1 C7A H7A2 107.8 . . n C1A C8A C7A 112.3(5) . . n C1A C8A H8A1 109.2(4) . . n C7A C8A H8A1 109.2(4) . . n C1A C8A H8A2 109.2(3) . . n C7A C8A H8A2 109.2(4) . . n H8A1 C8A H8A2 107.9 . . n C2B C1B C8B 126.4(7) . . n C2B C1B Rh2 71.1(4) . . n C8B C1B Rh2 111.7(5) . . n C2B C1B H1B 119.5(47) . . n C8B C1B H1B 111.9(47) . . n Rh2 C1B H1B 103.3(46) . . n C1B C2B C3B 123.7(7) . . n C1B C2B Rh2 69.9(4) . . n C3B C2B Rh2 113.5(4) . . n C1B C2B H2B 113.6(43) . . n C3B C2B H2B 116.9(43) . . n Rh2 C2B H2B 108.9(42) . . n C2B C3B C4B 112.1(5) . . n C2B C3B H3B1 109.2(4) . . n C4B C3B H3B1 109.2(4) . . n C2B C3B H3B2 109.2(4) . . n C4B C3B H3B2 109.2(4) . . n H3B1 C3B H3B2 107.9 . . n C5B C4B C3B 113.4(6) . . n C5B C4B H4B1 108.9(4) . . n C3B C4B H4B1 108.9(4) . . n C5B C4B H4B2 108.9(4) . . n C3B C4B H4B2 108.9(4) . . n H4B1 C4B H4B2 107.7 . . n C6B C5B C4B 124.3(7) . . n C6B C5B Rh2 71.3(4) . . n C4B C5B Rh2 110.3(4) . . n C6B C5B H5B 115.4(43) . . n C4B C5B H5B 116.8(44) . . n Rh2 C5B H5B 106.3(44) . . n C5B C6B C7B 124.1(6) . . n C5B C6B Rh2 69.9(4) . . n C7B C6B Rh2 112.5(5) . . n C5B C6B H6B 118.1(49) . . n C7B C6B H6B 113.9(49) . . n Rh2 C6B H6B 107.5(48) . . n C8B C7B C6B 112.5(6) . . n C8B C7B H7B1 109.1(4) . . n C6B C7B H7B1 109.1(4) . . n C8B C7B H7B2 109.1(4) . . n C6B C7B H7B2 109.1(4) . . n H7B1 C7B H7B2 107.8 . . n C1B C8B C7B 112.4(6) . . n C1B C8B H8B1 109.1(5) . . n C7B C8B H8B1 109.1(4) . . n C1B C8B H8B2 109.1(4) . . n C7B C8B H8B2 109.1(4) . . n H8B1 C8B H8B2 107.9 . . n C2C C1C C8C 122.8(7) . . n C2C C1C Rh3 70.3(3) . . n C8C C1C Rh3 112.8(5) . . n C2C C1C H1C 114.0(41) . . n C8C C1C H1C 120.1(41) . . n Rh3 C1C H1C 102.2(40) . . n C1C C2C C3C 125.6(6) . . n C1C C2C Rh3 70.8(3) . . n C3C C2C Rh3 110.6(4) . . n C1C C2C H2C 120.1(48) . . n C3C C2C H2C 112.8(48) . . n Rh3 C2C H2C 102.0(47) . . n C4C C3C C2C 115.2(6) . . n C4C C3C H3C1 108.5(4) . . n C2C C3C H3C1 108.5(4) . . n C4C C3C H3C2 108.5(5) . . n C2C C3C H3C2 108.5(4) . . n H3C1 C3C H3C2 107.5 . . n C3C C4C C5C 113.0(5) . . n C3C C4C H4C1 109.0(4) . . n C5C C4C H4C1 109.0(5) . . n C3C C4C H4C2 109.0(5) . . n C5C C4C H4C2 109.0(5) . . n H4C1 C4C H4C2 107.8 . . n C6C C5C C4C 124.9(8) . . n C6C C5C Rh3 70.9(4) . . n C4C C5C Rh3 113.4(5) . . n C6C C5C H5C 116.7(57) . . n C4C C5C H5C 115.2(57) . . n Rh3 C5C H5C 103.5(57) . . n C5C C6C C7C 125.2(7) . . n C5C C6C Rh3 71.0(4) . . n C7C C6C Rh3 111.5(5) . . n C5C C6C H6C 110.2(44) . . n C7C C6C H6C 120.7(44) . . n Rh3 C6C H6C 104.5(43) . . n C6C C7C C8C 114.3(6) . . n C6C C7C H7C1 108.7(4) . . n C8C C7C H7C1 108.7(5) . . n C6C C7C H7C2 108.7(4) . . n C8C C7C H7C2 108.7(5) . . n H7C1 C7C H7C2 107.6 . . n C7C C8C C1C 114.0(6) . . n C7C C8C H8C1 108.7(5) . . n C1C C8C H8C1 108.7(5) . . n C7C C8C H8C2 108.7(5) . . n C1C C8C H8C2 108.7(4) . . n H8C1 C8C H8C2 107.6 . . n C2D C1D C8D 122.4(6) . . n C2D C1D Rh4 71.0(3) . . n C8D C1D Rh4 113.7(4) . . n C2D C1D H1D 113.1(34) . . n C8D C1D H1D 120.0(34) . . n Rh4 C1D H1D 103.7(34) . . n C1D C2D C3D 127.0(6) . . n C1D C2D Rh4 70.8(3) . . n C3D C2D Rh4 110.8(4) . . n C1D C2D H2D 115.6(35) . . n C3D C2D H2D 115.2(34) . . n Rh4 C2D H2D 103.1(34) . . n C2D C3D C4D 113.4(6) . . n C2D C3D H3D1 108.9(4) . . n C4D C3D H3D1 108.9(4) . . n C2D C3D H3D2 108.9(3) . . n C4D C3D H3D2 108.9(4) . . n H3D1 C3D H3D2 107.7 . . n C5D C4D C3D 112.5(5) . . n C5D C4D H4D1 109.1(4) . . n C3D C4D H4D1 109.1(4) . . n C5D C4D H4D2 109.1(4) . . n C3D C4D H4D2 109.1(4) . . n H4D1 C4D H4D2 107.8 . . n C6D C5D C4D 122.9(6) . . n C6D C5D Rh4 70.2(3) . . n C4D C5D Rh4 112.7(5) . . n C6D C5D H5D 116.4(45) . . n C4D C5D H5D 116.3(45) . . n Rh4 C5D H5D 107.0(44) . . n C5D C6D C7D 123.5(6) . . n C5D C6D Rh4 70.7(4) . . n C7D C6D Rh4 113.2(4) . . n C5D C6D H6D 114.6(39) . . n C7D C6D H6D 116.5(39) . . n Rh4 C6D H6D 107.7(38) . . n C6D C7D C8D 114.2(5) . . n C6D C7D H7D1 108.7(4) . . n C8D C7D H7D1 108.7(4) . . n C6D C7D H7D2 108.7(4) . . n C8D C7D H7D2 108.7(4) . . n H7D1 C7D H7D2 107.6 . . n C7D C8D C1D 112.5(5) . . n C7D C8D H8D1 109.1(4) . . n C1D C8D H8D1 109.1(4) . . n C7D C8D H8D2 109.1(4) . . n C1D C8D H8D2 109.1(4) . . n H8D1 C8D H8D2 107.8 . . n _refine_diff_density_max 0.765 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.108 #===END