Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email MARINA@ALBANY.EDU _publ_contact_author_name 'Prof Marina A Petrukhina' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry University at Albany SUNY Albany New York 12222 UNITED STATES OF AMERICA ; _publ_section_title ; Direct Gas-Phase Interaction of Aryldiazoacetates and Dirhodium Catalysts ; loop_ _publ_author_name 'Marina A. Petrukhina' 'Kristian W. Andreini' 'Huw M. L. Davies' 'Abbas M. Walji' data_(1) _database_code_CSD 217509 _chemical_name_common ; Catena-(mu2-O,O'-a,a'-azinobis(4-methoxy-phenyl acetic acid) dimethyl ester)) -tetrakis(mu2-trimethylacetate-O,O') di-rhodium(II,II)) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Catena-(mu2-O,O'-a,a'-azinobis(4-methoxy-phenyl acetic acid) dimethyl ester)) -tetrakis(mu2-trimethylacetate-O,O') di-rhodium(II,II)) ; _chemical_melting_point 'not measured' _chemical_formula_moiety '[Rh2 (O2 C C (CH3)3)4 (C20 H20 O6 N2)]' _chemical_formula_sum 'C40 H56 N2 O14 Rh2' _chemical_formula_weight 994.69 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4127(9) _cell_length_b 11.7589(11) _cell_length_c 12.0273(11) _cell_angle_alpha 61.582(2) _cell_angle_beta 76.869(2) _cell_angle_gamma 71.626(2) _cell_volume 1106.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 6718 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.183 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method none _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_absorpt_correction_T_min 0.8745 _exptl_absorpt_correction_T_max 0.9606 _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 6994 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.25 _reflns_number_total 4925 _reflns_number_gt 4436 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-93 (Sheldrick, 1993)' _computing_publication_material 'SHELXCIF-93 (Sheldrick, 1993)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.6947P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef noref _refine_ls_number_reflns 4925 _refine_ls_number_parameters 296 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_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 0.085707(19) 0.014416(17) -0.091942(16) 0.02120(7) Uani 1 1 d . . . O1 O -0.05206(19) -0.03778(18) -0.15729(16) 0.0286(4) Uani 1 1 d . A . O2 O -0.03239(19) 0.20785(16) -0.17294(16) 0.0284(4) Uani 1 1 d . B . O3 O 0.21601(19) 0.06469(18) -0.01651(16) 0.0290(4) Uani 1 1 d . . . O4 O 0.1941(2) -0.17981(17) -0.00222(16) 0.0301(4) Uani 1 1 d . . . C1 C -0.1744(3) -0.0634(2) -0.0914(2) 0.0260(5) Uani 1 1 d . . . C2 C -0.1462(3) 0.2486(2) -0.1102(2) 0.0258(5) Uani 1 1 d . . . C3 C -0.2803(3) -0.0889(3) -0.1510(3) 0.0343(6) Uani 1 1 d D A 1 C15 C -0.3890(12) 0.0533(8) -0.2171(11) 0.0282(18) Uiso 0.33 1 d PD A 1 H15A H -0.4617 0.0473 -0.2585 0.042 Uiso 0.33 1 calc PR A 1 H15B H -0.3307 0.1153 -0.2796 0.042 Uiso 0.33 1 calc PR A 1 H15C H -0.4411 0.0844 -0.1536 0.042 Uiso 0.33 1 calc PR A 1 C17 C -0.1967(10) -0.1400(13) -0.2491(10) 0.0230(19) Uiso 0.33 1 d PD A 1 H17A H -0.2678 -0.1550 -0.2848 0.034 Uiso 0.33 1 calc PR A 1 H17B H -0.1235 -0.2230 -0.2086 0.034 Uiso 0.33 1 calc PR A 1 H17C H -0.1457 -0.0745 -0.3162 0.034 Uiso 0.33 1 calc PR A 1 C19 C -0.3731(12) -0.1837(10) -0.0521(7) 0.0198(16) Uiso 0.33 1 d PD A 1 H19A H -0.4389 -0.1972 -0.0939 0.030 Uiso 0.33 1 calc PR A 1 H19B H -0.4331 -0.1460 0.0049 0.030 Uiso 0.33 1 calc PR A 1 H19C H -0.3067 -0.2684 -0.0041 0.030 Uiso 0.33 1 calc PR A 1 C15X C -0.3568(15) 0.0484(10) -0.2515(12) 0.062(4) Uiso 0.33 1 d PD A 2 H15D H -0.4257 0.0369 -0.2921 0.092 Uiso 0.33 1 calc PR A 2 H15E H -0.2808 0.0890 -0.3148 0.092 Uiso 0.33 1 calc PR A 2 H15F H -0.4118 0.1055 -0.2106 0.092 Uiso 0.33 1 calc PR A 2 C17X C -0.1913(15) -0.1776(13) -0.2165(13) 0.061(4) Uiso 0.33 1 d PD A 2 H17D H -0.2598 -0.1931 -0.2543 0.092 Uiso 0.33 1 calc PR A 2 H17E H -0.1387 -0.2621 -0.1545 0.092 Uiso 0.33 1 calc PR A 2 H17F H -0.1190 -0.1339 -0.2822 0.092 Uiso 0.33 1 calc PR A 2 C19X C -0.4076(12) -0.1460(13) -0.0589(10) 0.050(3) Uiso 0.33 1 d PD A 2 H19D H -0.4704 -0.1595 -0.1032 0.074 Uiso 0.33 1 calc PR A 2 H19E H -0.4676 -0.0844 -0.0242 0.074 Uiso 0.33 1 calc PR A 2 H19F H -0.3661 -0.2306 0.0095 0.074 Uiso 0.33 1 calc PR A 2 C15Y C -0.4174(14) 0.0270(13) -0.1811(15) 0.075(5) Uiso 0.33 1 d PD A 3 H15G H -0.4866 0.0132 -0.2195 0.113 Uiso 0.33 1 calc PR A 3 H15H H -0.3870 0.1089 -0.2396 0.113 Uiso 0.33 1 calc PR A 3 H15I H -0.4665 0.0334 -0.1034 0.113 Uiso 0.33 1 calc PR A 3 C17Y C -0.2091(11) -0.0988(11) -0.2736(9) 0.037(3) Uiso 0.33 1 d PD A 3 H17G H -0.2803 -0.1149 -0.3084 0.056 Uiso 0.33 1 calc PR A 3 H17H H -0.1198 -0.1718 -0.2567 0.056 Uiso 0.33 1 calc PR A 3 H17I H -0.1818 -0.0161 -0.3343 0.056 Uiso 0.33 1 calc PR A 3 C19Y C -0.3222(16) -0.2201(11) -0.0518(11) 0.063(4) Uiso 0.33 1 d PD A 3 H19G H -0.3900 -0.2403 -0.0860 0.094 Uiso 0.33 1 calc PR A 3 H19H H -0.3711 -0.2106 0.0246 0.094 Uiso 0.33 1 calc PR A 3 H19I H -0.2318 -0.2918 -0.0316 0.094 Uiso 0.33 1 calc PR A 3 C4 C -0.2322(3) 0.3942(3) -0.1755(3) 0.0357(6) Uani 1 1 d D B 1 C16 C -0.1675(12) 0.4696(9) -0.1289(11) 0.0308(18) Uiso 0.33 1 d PD B 1 H16A H -0.1856 0.4343 -0.0372 0.046 Uiso 0.33 1 calc PR B 1 H16B H -0.2166 0.5638 -0.1672 0.046 Uiso 0.33 1 calc PR B 1 H16C H -0.0602 0.4575 -0.1533 0.046 Uiso 0.33 1 calc PR B 1 C18 C -0.2038(11) 0.4500(9) -0.3188(6) 0.0248(16) Uiso 0.33 1 d PD B 1 H18A H -0.2598 0.5422 -0.3570 0.037 Uiso 0.33 1 calc PR B 1 H18B H -0.2362 0.3985 -0.3475 0.037 Uiso 0.33 1 calc PR B 1 H18C H -0.0973 0.4449 -0.3436 0.037 Uiso 0.33 1 calc PR B 1 C20 C -0.4009(7) 0.4104(8) -0.1296(9) 0.0200(14) Uiso 0.33 1 d PD B 1 H20A H -0.4135 0.3730 -0.0376 0.030 Uiso 0.33 1 calc PR B 1 H20B H -0.4438 0.3640 -0.1571 0.030 Uiso 0.33 1 calc PR B 1 H20C H -0.4518 0.5042 -0.1650 0.030 Uiso 0.33 1 calc PR B 1 C16X C -0.1445(16) 0.4876(15) -0.1846(16) 0.084(5) Uiso 0.33 1 d PD B 2 H16D H -0.2012 0.5791 -0.2263 0.127 Uiso 0.33 1 calc PR B 2 H16E H -0.0483 0.4750 -0.2333 0.127 Uiso 0.33 1 calc PR B 2 H16F H -0.1279 0.4682 -0.0999 0.127 Uiso 0.33 1 calc PR B 2 C18X C -0.2499(16) 0.4255(14) -0.3131(10) 0.069(4) Uiso 0.33 1 d PD B 2 H18D H -0.3041 0.5176 -0.3567 0.103 Uiso 0.33 1 calc PR B 2 H18E H -0.3054 0.3673 -0.3107 0.103 Uiso 0.33 1 calc PR B 2 H18F H -0.1513 0.4111 -0.3579 0.103 Uiso 0.33 1 calc PR B 2 C20X C -0.3828(12) 0.4287(13) -0.1055(12) 0.060(4) Uiso 0.33 1 d PD B 2 H20D H -0.4305 0.5223 -0.1519 0.090 Uiso 0.33 1 calc PR B 2 H20E H -0.3674 0.4114 -0.0212 0.090 Uiso 0.33 1 calc PR B 2 H20F H -0.4466 0.3746 -0.0985 0.090 Uiso 0.33 1 calc PR B 2 C16Y C -0.2096(19) 0.4653(17) -0.1008(15) 0.083(6) Uiso 0.33 1 d PD B 3 H16G H -0.2620 0.5587 -0.1390 0.124 Uiso 0.33 1 calc PR B 3 H16H H -0.1032 0.4578 -0.1043 0.124 Uiso 0.33 1 calc PR B 3 H16I H -0.2496 0.4234 -0.0130 0.124 Uiso 0.33 1 calc PR B 3 C18Y C -0.1618(14) 0.4673(12) -0.3095(10) 0.058(3) Uiso 0.33 1 d PD B 3 H18G H -0.2195 0.5590 -0.3472 0.086 Uiso 0.33 1 calc PR B 3 H18H H -0.1618 0.4239 -0.3607 0.086 Uiso 0.33 1 calc PR B 3 H18I H -0.0592 0.4655 -0.3057 0.086 Uiso 0.33 1 calc PR B 3 C20Y C -0.3938(12) 0.3999(15) -0.1686(15) 0.072(4) Uiso 0.33 1 d PD B 3 H20G H -0.4490 0.4921 -0.2099 0.107 Uiso 0.33 1 calc PR B 3 H20H H -0.4334 0.3604 -0.0804 0.107 Uiso 0.33 1 calc PR B 3 H20I H -0.4044 0.3510 -0.2110 0.107 Uiso 0.33 1 calc PR B 3 O5 O 0.2574(2) 0.02735(18) -0.27862(16) 0.0298(4) Uani 1 1 d . . . O6 O 0.1601(2) 0.0900(2) -0.46031(18) 0.0401(5) Uani 1 1 d . . . O7 O 0.2128(3) -0.5684(2) -0.2476(2) 0.0497(5) Uani 1 1 d . . . N1 N 0.4934(3) -0.0651(2) -0.4812(2) 0.0324(5) Uani 1 1 d . . . C5 C 0.2577(3) 0.0171(2) -0.3743(2) 0.0270(5) Uani 1 1 d . . . C6 C 0.3701(3) -0.0866(3) -0.4116(2) 0.0284(5) Uani 1 1 d . . . C7 C 0.3308(3) -0.2134(3) -0.3689(2) 0.0295(5) Uani 1 1 d . . . C8 C 0.3929(3) -0.2896(3) -0.4353(3) 0.0375(6) Uani 1 1 d . . . C9 C 0.3551(3) -0.4078(3) -0.3992(3) 0.0397(6) Uani 1 1 d . . . C10 C 0.2549(3) -0.4524(3) -0.2938(3) 0.0355(6) Uani 1 1 d . . . C11 C 0.1910(4) -0.3764(3) -0.2273(3) 0.0456(7) Uani 1 1 d . . . C12 C 0.2265(4) -0.2580(3) -0.2650(3) 0.0419(7) Uani 1 1 d . . . C13 C 0.2811(4) -0.6552(3) -0.3056(3) 0.0531(8) Uani 1 1 d . . . H13A H 0.2596 -0.6102 -0.3937 0.080 Uiso 1 1 calc R . . H13B H 0.2416 -0.7342 -0.2615 0.080 Uiso 1 1 calc R . . H13C H 0.3890 -0.6808 -0.3013 0.080 Uiso 1 1 calc R . . C14 C 0.0428(4) 0.1962(3) -0.4431(3) 0.0482(8) Uani 1 1 d . . . H14A H -0.0226 0.1585 -0.3672 0.072 Uiso 1 1 calc R . . H14B H -0.0154 0.2462 -0.5161 0.072 Uiso 1 1 calc R . . H14C H 0.0877 0.2550 -0.4345 0.072 Uiso 1 1 calc R . . H8 H 0.182(4) -0.209(3) -0.220(3) 0.049(9) Uiso 1 1 d . . . H9 H 0.461(4) -0.260(3) -0.511(3) 0.054(10) Uiso 1 1 d . . . H10 H 0.394(4) -0.451(3) -0.451(3) 0.050(9) Uiso 1 1 d . . . H11 H 0.125(4) -0.404(3) -0.156(3) 0.054(10) Uiso 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 0.02223(10) 0.02478(10) 0.01767(10) -0.01089(7) 0.00229(6) -0.00736(7) O1 0.0294(9) 0.0389(10) 0.0246(8) -0.0186(7) 0.0025(7) -0.0135(8) O2 0.0310(9) 0.0256(8) 0.0233(8) -0.0098(7) 0.0019(7) -0.0047(7) O3 0.0276(9) 0.0410(10) 0.0251(9) -0.0180(7) 0.0034(7) -0.0151(8) O4 0.0311(9) 0.0260(8) 0.0261(9) -0.0101(7) 0.0034(7) -0.0041(7) C1 0.0281(12) 0.0261(11) 0.0243(11) -0.0114(9) -0.0015(9) -0.0072(9) C2 0.0277(12) 0.0259(11) 0.0270(12) -0.0134(9) -0.0018(9) -0.0080(9) C3 0.0341(13) 0.0461(15) 0.0318(13) -0.0208(12) 0.0000(11) -0.0171(12) C4 0.0322(13) 0.0267(12) 0.0371(14) -0.0092(11) -0.0014(11) -0.0018(10) O5 0.0299(9) 0.0393(10) 0.0252(9) -0.0189(7) 0.0042(7) -0.0119(8) O6 0.0388(11) 0.0488(12) 0.0312(10) -0.0228(9) -0.0042(8) 0.0005(9) O7 0.0529(13) 0.0417(11) 0.0604(14) -0.0283(10) 0.0145(11) -0.0231(10) N1 0.0325(11) 0.0348(11) 0.0312(11) -0.0187(9) 0.0090(9) -0.0113(9) C5 0.0247(11) 0.0303(12) 0.0268(12) -0.0140(10) 0.0074(9) -0.0119(10) C6 0.0301(12) 0.0334(12) 0.0244(11) -0.0163(10) 0.0024(9) -0.0086(10) C7 0.0274(12) 0.0345(13) 0.0263(12) -0.0147(10) 0.0028(9) -0.0083(10) C8 0.0380(15) 0.0386(14) 0.0344(14) -0.0188(12) 0.0096(11) -0.0119(12) C9 0.0457(16) 0.0372(14) 0.0384(15) -0.0235(12) 0.0077(12) -0.0097(12) C10 0.0315(13) 0.0343(13) 0.0406(15) -0.0167(11) -0.0027(11) -0.0076(11) C11 0.0461(17) 0.0496(18) 0.0453(17) -0.0260(14) 0.0193(14) -0.0249(14) C12 0.0447(16) 0.0478(17) 0.0410(16) -0.0292(14) 0.0180(13) -0.0207(14) C13 0.065(2) 0.0395(16) 0.060(2) -0.0277(15) 0.0073(17) -0.0196(16) C14 0.0444(17) 0.0460(17) 0.0419(17) -0.0197(14) -0.0036(13) 0.0053(14) _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 O1 2.0249(17) . y Rh1 O4 2.0265(17) . y Rh1 O2 2.0365(17) . y Rh1 O3 2.0372(17) . y Rh1 Rh1 2.3705(4) 2 y Rh1 O5 2.4201(17) . y O1 C1 1.273(3) . n O2 C2 1.265(3) . n O3 C1 1.262(3) 2 n O4 C2 1.264(3) 2 n C1 O3 1.262(3) 2 n C1 C3 1.522(3) . n C2 O4 1.264(3) 2 n C2 C4 1.530(3) . n C3 C19 1.517(7) . n C3 C17 1.525(7) . n C3 C15 1.580(8) . n C15 H15A 0.9700 . n C15 H15B 0.9700 . n C15 H15C 0.9700 . n C17 H17A 0.9700 . n C17 H17B 0.9700 . n C17 H17C 0.9700 . n C19 H19A 0.9700 . n C19 H19B 0.9700 . n C19 H19C 0.9700 . n C15X H15D 0.9700 . n C15X H15E 0.9700 . n C15X H15F 0.9700 . n C17X H17D 0.9700 . n C17X H17E 0.9700 . n C17X H17F 0.9700 . n C19X H19D 0.9700 . n C19X H19E 0.9700 . n C19X H19F 0.9700 . n C15Y H15G 0.9700 . n C15Y H15H 0.9700 . n C15Y H15I 0.9700 . n C17Y H17G 0.9700 . n C17Y H17H 0.9700 . n C17Y H17I 0.9700 . n C19Y H19G 0.9700 . n C19Y H19H 0.9700 . n C19Y H19I 0.9700 . n C4 C18 1.515(7) . n C4 C20 1.541(7) . n C4 C16 1.561(8) . n C16 H16A 0.9700 . n C16 H16B 0.9700 . n C16 H16C 0.9700 . n C18 H18A 0.9700 . n C18 H18B 0.9700 . n C18 H18C 0.9700 . n C20 H20A 0.9700 . n C20 H20B 0.9700 . n C20 H20C 0.9700 . n C16X H16D 0.9700 . n C16X H16E 0.9700 . n C16X H16F 0.9700 . n C18X H18D 0.9700 . n C18X H18E 0.9700 . n C18X H18F 0.9700 . n C20X H20D 0.9700 . n C20X H20E 0.9700 . n C20X H20F 0.9700 . n C16Y H16G 0.9700 . n C16Y H16H 0.9700 . n C16Y H16I 0.9700 . n C18Y H18G 0.9700 . n C18Y H18H 0.9700 . n C18Y H18I 0.9700 . n C20Y H20G 0.9700 . n C20Y H20H 0.9700 . n C20Y H20I 0.9700 . n O5 C5 1.213(3) . y O6 C5 1.319(3) . y O6 C14 1.447(3) . n O7 C10 1.359(3) . n O7 C13 1.415(4) . n N1 C6 1.286(3) . y N1 N1 1.413(4) 2_654 y C5 C6 1.516(3) . y C6 C7 1.468(4) . y C7 C8 1.386(4) . y C7 C12 1.394(4) . y C8 C9 1.383(4) . y C8 H9 0.97(4) . n C9 C10 1.382(4) . y C9 H10 0.93(3) . n C10 C11 1.386(4) . y C11 C12 1.371(4) . y C11 H11 0.92(4) . n C12 H8 0.91(4) . n C13 H13A 0.9700 . n C13 H13B 0.9700 . n C13 H13C 0.9700 . n C14 H14A 0.9700 . n C14 H14B 0.9700 . n C14 H14C 0.9700 . 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 O1 Rh1 O4 89.91(7) . . y O1 Rh1 O2 89.78(7) . . y O4 Rh1 O2 176.59(6) . . y O1 Rh1 O3 176.60(6) . . y O4 Rh1 O3 89.79(7) . . y O2 Rh1 O3 90.31(7) . . y O1 Rh1 Rh1 88.45(5) . 2 y O4 Rh1 Rh1 88.73(5) . 2 y O2 Rh1 Rh1 87.87(5) . 2 y O3 Rh1 Rh1 88.16(5) . 2 y O1 Rh1 O5 87.98(6) . . n O4 Rh1 O5 88.15(6) . . n O2 Rh1 O5 95.23(6) . . n O3 Rh1 O5 95.39(6) . . n Rh1 Rh1 O5 175.26(4) 2 . y C1 O1 Rh1 119.12(15) . . n C2 O2 Rh1 119.05(15) . . n C1 O3 Rh1 119.07(15) 2 . n C2 O4 Rh1 118.68(15) 2 . n O3 C1 O1 125.1(2) 2 . n O3 C1 C3 118.1(2) 2 . n O1 C1 C3 116.7(2) . . n O4 C2 O2 125.7(2) 2 . n O4 C2 C4 117.2(2) 2 . n O2 C2 C4 117.1(2) . . n C19 C3 C1 112.1(4) . . n C19 C3 C17 110.2(6) . . n C1 C3 C17 112.0(4) . . n C19 C3 C15 108.7(7) . . n C1 C3 C15 103.2(4) . . n C17 C3 C15 110.5(7) . . n C3 C15 H15A 109.5 . . n C3 C15 H15B 109.5 . . n H15A C15 H15B 109.5 . . n C3 C15 H15C 109.5 . . n H15A C15 H15C 109.5 . . n H15B C15 H15C 109.5 . . n C3 C17 H17A 109.5 . . n C3 C17 H17B 109.5 . . n H17A C17 H17B 109.5 . . n C3 C17 H17C 109.5 . . n H17A C17 H17C 109.5 . . n H17B C17 H17C 109.5 . . n C3 C19 H19A 109.5 . . n C3 C19 H19B 109.5 . . n H19A C19 H19B 109.5 . . n C3 C19 H19C 109.5 . . n H19A C19 H19C 109.5 . . n H19B C19 H19C 109.5 . . n H15D C15X H15E 109.5 . . n H15D C15X H15F 109.5 . . n H15E C15X H15F 109.5 . . n H17D C17X H17E 109.5 . . n H17D C17X H17F 109.5 . . n H17E C17X H17F 109.5 . . n H19D C19X H19E 109.5 . . n H19D C19X H19F 109.5 . . n H19E C19X H19F 109.5 . . n H15G C15Y H15H 109.5 . . n H15G C15Y H15I 109.5 . . n H15H C15Y H15I 109.5 . . n H17G C17Y H17H 109.5 . . n H17G C17Y H17I 109.5 . . n H17H C17Y H17I 109.5 . . n H19G C19Y H19H 109.5 . . n H19G C19Y H19I 109.5 . . n H19H C19Y H19I 109.5 . . n C18 C4 C2 111.7(4) . . n C18 C4 C20 112.5(6) . . n C2 C4 C20 110.7(3) . . n C18 C4 C16 109.2(6) . . n C2 C4 C16 104.6(4) . . n C20 C4 C16 107.9(6) . . n C4 C16 H16A 109.5 . . n C4 C16 H16B 109.5 . . n H16A C16 H16B 109.5 . . n C4 C16 H16C 109.5 . . n H16A C16 H16C 109.5 . . n H16B C16 H16C 109.5 . . n C4 C18 H18A 109.5 . . n C4 C18 H18B 109.5 . . n H18A C18 H18B 109.5 . . n C4 C18 H18C 109.5 . . n H18A C18 H18C 109.5 . . n H18B C18 H18C 109.5 . . n C4 C20 H20A 109.5 . . n C4 C20 H20B 109.5 . . n H20A C20 H20B 109.5 . . n C4 C20 H20C 109.5 . . n H20A C20 H20C 109.5 . . n H20B C20 H20C 109.5 . . n H16D C16X H16E 109.5 . . n H16D C16X H16F 109.5 . . n H16E C16X H16F 109.5 . . n H18D C18X H18E 109.5 . . n H18D C18X H18F 109.5 . . n H18E C18X H18F 109.5 . . n H20D C20X H20E 109.5 . . n H20D C20X H20F 109.5 . . n H20E C20X H20F 109.5 . . n H16G C16Y H16H 109.5 . . n H16G C16Y H16I 109.5 . . n H16H C16Y H16I 109.5 . . n H18G C18Y H18H 109.5 . . n H18G C18Y H18I 109.5 . . n H18H C18Y H18I 109.5 . . n H20G C20Y H20H 109.5 . . n H20G C20Y H20I 109.5 . . n H20H C20Y H20I 109.5 . . n C5 O5 Rh1 136.57(16) . . y C5 O6 C14 118.0(2) . . n C10 O7 C13 118.9(2) . . n C6 N1 N1 111.7(3) . 2_654 y O5 C5 O6 126.4(2) . . y O5 C5 C6 124.5(2) . . y O6 C5 C6 109.0(2) . . y N1 C6 C7 120.2(2) . . y N1 C6 C5 122.4(2) . . y C7 C6 C5 117.3(2) . . y C8 C7 C12 118.1(2) . . y C8 C7 C6 120.2(2) . . n C12 C7 C6 121.7(2) . . n C9 C8 C7 121.5(3) . . n C9 C8 H9 118(2) . . n C7 C8 H9 121(2) . . n C10 C9 C8 119.6(3) . . n C10 C9 H10 123(2) . . n C8 C9 H10 118(2) . . n O7 C10 C9 124.7(3) . . n O7 C10 C11 115.9(3) . . n C9 C10 C11 119.4(3) . . n C12 C11 C10 120.7(3) . . n C12 C11 H11 118(2) . . n C10 C11 H11 122(2) . . n C11 C12 C7 120.7(3) . . n C11 C12 H8 119(2) . . n C7 C12 H8 120(2) . . n O7 C13 H13A 109.5 . . n O7 C13 H13B 109.5 . . n H13A C13 H13B 109.5 . . n O7 C13 H13C 109.5 . . n H13A C13 H13C 109.5 . . n H13B C13 H13C 109.5 . . n O6 C14 H14A 109.5 . . n O6 C14 H14B 109.5 . . n H14A C14 H14B 109.5 . . n O6 C14 H14C 109.5 . . n H14A C14 H14C 109.5 . . n H14B C14 H14C 109.5 . . n _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 0.698 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.077 #===END data_(2) _database_code_CSD 217510 _chemical_name_common ; Catena-(mu2-(2,3-bis(4-methoxy-phenyl)-2-Butendioic acid-O,O'- dimethyl ester)-tetrakis(mu2-trifluoroacetato-O,O')- di-rhodium (II,II)) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Catena-(mu2-(2,3-bis(4-methoxy-phenyl)-2-Butendioic acid-O,O'-dimethyl ester)- tetrakis(mu2-trifluoroacetato-O,O')- di-rhodium (II,II)) ; _chemical_melting_point 'not measured' _chemical_formula_moiety '[Rh2 (O2 C CF3)4 (OC(OCH3)CC6H4(OCH3))2]' _chemical_formula_sum 'C28 H20 F12 O14 Rh2' _chemical_formula_weight 1014.26 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 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.064(3) _cell_length_b 20.754(6) _cell_length_c 8.544(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.010(4) _cell_angle_gamma 90.00 _cell_volume 1706.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5107 _cell_measurement_theta_min 2.3325 _cell_measurement_theta_max 27.7435 _exptl_crystal_description plate _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method none _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.100 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_absorpt_correction_T_min 0.7481 _exptl_absorpt_correction_T_max 0.9573 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exprosures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 10438 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2990 _reflns_number_gt 2431 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-93 (Sheldrick, 1993)' _computing_publication_material 'SHELXCIF-93 (Sheldrick, 1993)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+6.5551P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef noref _refine_ls_number_reflns 2990 _refine_ls_number_parameters 280 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.285 _refine_ls_restrained_S_all 1.311 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_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 0.37989(5) 0.48524(2) 0.44854(5) 0.02600(15) Uani 1 1 d . . . O1 O 0.3420(4) 0.5732(2) 0.3399(5) 0.0310(9) Uani 1 1 d . . . O2 O 0.3514(4) 0.52623(19) 0.6532(5) 0.0301(9) Uani 1 1 d . A . O3 O 0.4325(4) 0.3990(2) 0.5636(5) 0.0314(9) Uani 1 1 d . . . O4 O 0.4220(4) 0.4456(2) 0.2518(5) 0.0306(10) Uani 1 1 d . . . C1 C 0.4429(7) 0.6105(3) 0.3640(7) 0.0300(14) Uani 1 1 d . . . C2 C 0.4557(6) 0.5514(3) 0.7524(7) 0.0295(14) Uani 1 1 d . . . C3 C 0.4063(7) 0.6800(3) 0.3024(8) 0.0410(16) Uani 1 1 d . . . C4 C 0.4251(7) 0.5855(4) 0.8971(8) 0.0396(16) Uani 1 1 d . A 1 F4 F 0.3269(13) 0.6343(6) 0.8370(12) 0.027(2) Uiso 0.50 1 d P A 1 F5 F 0.3644(11) 0.5356(4) 0.9789(11) 0.030(2) Uiso 0.50 1 d P A 1 F6 F 0.5361(8) 0.6086(5) 1.0028(10) 0.0252(18) Uiso 0.50 1 d P A 1 F4X F 0.317(2) 0.6178(10) 0.864(3) 0.039(6) Uiso 0.25 1 d P A 2 F5X F 0.4045(19) 0.5559(10) 1.000(2) 0.034(4) Uiso 0.25 1 d P A 2 F6X F 0.5277(17) 0.6336(9) 0.960(2) 0.044(5) Uiso 0.25 1 d P A 2 F4Y F 0.374(3) 0.6393(13) 0.857(3) 0.064(8) Uiso 0.25 1 d P A 3 F5Y F 0.346(2) 0.5567(10) 0.960(2) 0.031(5) Uiso 0.25 1 d P A 3 F6Y F 0.5372(16) 0.5835(9) 1.0320(19) 0.035(5) Uiso 0.25 1 d P A 3 O5 O 0.1598(4) 0.4553(2) 0.3194(5) 0.0326(10) Uani 1 1 d . . . O6 O -0.0641(4) 0.4539(2) 0.1840(5) 0.0369(10) Uani 1 1 d . . . O7 O -0.0996(6) 0.7743(2) 0.2674(8) 0.0696(18) Uani 1 1 d . . . C5 C 0.0419(6) 0.4696(3) 0.3093(7) 0.0288(13) Uani 1 1 d . . . C6 C 0.0012(6) 0.5120(4) 0.4306(8) 0.0393(15) Uani 1 1 d . . . C7 C -0.0277(6) 0.5821(3) 0.3855(8) 0.0335(14) Uani 1 1 d . . . C8 C 0.0574(7) 0.6303(3) 0.4722(9) 0.0408(17) Uani 1 1 d . . . C9 C 0.0327(8) 0.6938(4) 0.4272(10) 0.051(2) Uani 1 1 d . . . C10 C -0.0791(7) 0.7104(3) 0.2968(9) 0.0410(16) Uani 1 1 d . . . C11 C -0.1641(7) 0.6625(3) 0.2110(8) 0.0364(15) Uani 1 1 d . . . C12 C -0.1383(6) 0.5994(3) 0.2550(8) 0.0352(15) Uani 1 1 d . . . C13 C -0.2221(8) 0.7938(4) 0.1445(13) 0.074(3) Uani 1 1 d . . . H13A H -0.2200 0.7770 0.0381 0.111 Uiso 1 1 calc R . . H13B H -0.2267 0.8410 0.1399 0.111 Uiso 1 1 calc R . . H13C H -0.3040 0.7770 0.1708 0.111 Uiso 1 1 calc R . . C14 C -0.0339(7) 0.4173(3) 0.0535(7) 0.0410(16) Uani 1 1 d . . . H14A H 0.0439 0.4373 0.0245 0.062 Uiso 1 1 calc R . . H14B H -0.1161 0.4168 -0.0425 0.062 Uiso 1 1 calc R . . H14C H -0.0091 0.3730 0.0906 0.062 Uiso 1 1 calc R . . F1 F 0.3834(6) 0.7142(2) 0.4221(6) 0.0700(14) Uani 1 1 d . . . F2 F 0.2951(5) 0.6828(2) 0.1769(5) 0.0669(13) Uani 1 1 d . . . F3 F 0.5088(5) 0.7080(2) 0.2621(7) 0.0695(14) Uani 1 1 d . . . H8 H 0.130(7) 0.620(3) 0.551(8) 0.037(18) Uiso 1 1 d . . . H9 H 0.086(8) 0.724(4) 0.478(10) 0.06(3) Uiso 1 1 d . . . H11 H -0.248(7) 0.672(3) 0.119(8) 0.041(18) Uiso 1 1 d . . . H12 H -0.195(6) 0.568(3) 0.198(7) 0.025(15) Uiso 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 0.0266(2) 0.0296(3) 0.0227(2) -0.0042(2) 0.00875(17) -0.0027(2) O1 0.029(2) 0.033(3) 0.030(2) -0.0060(18) 0.0081(17) -0.0014(19) O2 0.030(2) 0.036(3) 0.027(2) -0.0061(18) 0.0134(17) -0.0027(18) O3 0.032(2) 0.033(2) 0.030(2) 0.0010(18) 0.0094(18) -0.0033(19) O4 0.033(2) 0.034(3) 0.026(2) -0.0062(18) 0.0104(17) -0.0023(18) C1 0.040(4) 0.031(4) 0.022(3) -0.002(3) 0.013(3) 0.003(3) C2 0.031(3) 0.033(4) 0.026(3) -0.001(3) 0.009(3) -0.002(3) C3 0.050(4) 0.035(4) 0.040(4) 0.001(3) 0.017(3) 0.000(3) C4 0.031(4) 0.052(5) 0.033(4) -0.010(3) 0.005(3) 0.000(3) O5 0.025(2) 0.038(3) 0.034(2) -0.0124(19) 0.0084(17) -0.0013(19) O6 0.031(2) 0.049(3) 0.030(2) -0.012(2) 0.0089(19) 0.002(2) O7 0.052(3) 0.025(3) 0.112(5) 0.018(3) -0.006(3) -0.001(2) C5 0.039(4) 0.022(3) 0.029(3) 0.000(2) 0.015(3) -0.001(3) C6 0.033(3) 0.046(4) 0.039(3) -0.004(3) 0.011(3) 0.000(3) C7 0.032(3) 0.029(4) 0.044(4) 0.002(3) 0.019(3) 0.000(3) C8 0.033(4) 0.039(4) 0.043(4) 0.006(3) 0.001(3) 0.010(3) C9 0.048(4) 0.030(4) 0.063(5) -0.006(4) 0.000(4) -0.003(4) C10 0.035(4) 0.027(4) 0.058(4) 0.009(3) 0.009(3) 0.002(3) C11 0.034(4) 0.039(4) 0.034(4) 0.006(3) 0.006(3) 0.001(3) C12 0.029(3) 0.034(4) 0.040(4) -0.006(3) 0.006(3) -0.007(3) C13 0.048(5) 0.038(5) 0.123(8) 0.036(5) 0.004(5) 0.007(4) C14 0.045(4) 0.054(5) 0.024(3) -0.018(3) 0.010(3) -0.003(3) F1 0.118(4) 0.039(3) 0.060(3) -0.007(2) 0.038(3) 0.017(3) F2 0.073(3) 0.046(3) 0.060(3) 0.013(2) -0.014(2) 0.003(2) F3 0.070(3) 0.047(3) 0.102(4) 0.027(3) 0.041(3) 0.001(2) _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 O4 2.024(4) . y Rh1 O1 2.032(4) . y Rh1 O3 2.036(4) . y Rh1 O2 2.039(4) . y Rh1 O5 2.254(4) . y Rh1 Rh1 2.3980(11) 3_666 y O1 C1 1.246(7) . n O2 C2 1.254(7) . n O3 C1 1.241(7) 3_666 n O4 C2 1.243(7) 3_666 n C1 O3 1.241(7) 3_666 n C1 C3 1.542(9) . n C2 O4 1.243(7) 3_666 n C2 C4 1.532(8) . n C3 F2 1.306(8) . n C3 F3 1.315(8) . n C3 F1 1.320(8) . n C4 F6 1.305(10) . n C4 F4 1.403(13) . n C4 F5 1.478(11) . n O5 C5 1.201(7) . y O6 C5 1.312(7) . y O6 C14 1.453(7) . n O7 C10 1.355(8) . n O7 C13 1.425(9) . n C5 C6 1.505(9) . y C6 C6 1.292(13) 3_566 y C6 C7 1.511(9) . y C7 C12 1.373(9) . y C7 C8 1.383(9) . y C8 C9 1.375(10) . y C8 H8 0.86(7) . n C9 C10 1.375(10) . y C9 H9 0.85(8) . n C10 C11 1.374(9) . y C11 C12 1.365(9) . y C11 H11 0.99(7) . n C12 H12 0.91(6) . n C13 H13A 0.9800 . n C13 H13B 0.9800 . n C13 H13C 0.9800 . n C14 H14A 0.9800 . n C14 H14B 0.9800 . n C14 H14C 0.9800 . 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 O4 Rh1 O1 92.45(16) . . y O4 Rh1 O3 87.45(16) . . y O1 Rh1 O3 175.87(16) . . y O4 Rh1 O2 176.14(16) . . y O1 Rh1 O2 87.84(16) . . y O3 Rh1 O2 91.99(16) . . y O4 Rh1 O5 84.03(15) . . y O1 Rh1 O5 89.86(16) . . y O3 Rh1 O5 94.24(16) . . y O2 Rh1 O5 99.82(15) . . y O4 Rh1 Rh1 88.55(12) . 3_666 n O1 Rh1 Rh1 88.42(11) . 3_666 n O3 Rh1 Rh1 87.46(12) . 3_666 n O2 Rh1 Rh1 87.61(11) . 3_666 n O5 Rh1 Rh1 172.30(10) . 3_666 y C1 O1 Rh1 116.6(4) . . n C2 O2 Rh1 117.0(4) . . n C1 O3 Rh1 117.6(4) 3_666 . n C2 O4 Rh1 117.0(4) 3_666 . n O3 C1 O1 129.8(6) 3_666 . n O3 C1 C3 115.1(6) 3_666 . n O1 C1 C3 115.0(6) . . n O4 C2 O2 129.9(5) 3_666 . n O4 C2 C4 115.8(5) 3_666 . n O2 C2 C4 114.3(5) . . n F2 C3 F3 108.3(6) . . n F2 C3 F1 108.1(6) . . n F3 C3 F1 107.0(6) . . n F2 C3 C1 112.6(6) . . n F3 C3 C1 112.0(6) . . n F1 C3 C1 108.5(5) . . n F6 C4 F4 110.9(9) . . n F6 C4 F5 108.6(8) . . n F4 C4 F5 109.6(8) . . n F6 C4 C2 113.2(6) . . n F4 C4 C2 108.9(6) . . n F5 C4 C2 105.5(6) . . n C5 O5 Rh1 140.9(4) . . y C5 O6 C14 116.9(5) . . n C10 O7 C13 117.8(6) . . n O5 C5 O6 123.2(5) . . y O5 C5 C6 123.8(6) . . y O6 C5 C6 112.8(5) . . n C6 C6 C5 119.3(9) 3_566 . y C6 C6 C7 123.4(8) 3_566 . n C5 C6 C7 117.3(5) . . n C12 C7 C8 118.2(6) . . n C12 C7 C6 120.6(6) . . n C8 C7 C6 121.1(6) . . n C9 C8 C7 120.7(7) . . n C9 C8 H8 119(4) . . n C7 C8 H8 120(4) . . n C8 C9 C10 120.3(7) . . n C8 C9 H9 122(6) . . n C10 C9 H9 118(6) . . n O7 C10 C11 124.9(6) . . n O7 C10 C9 116.0(6) . . n C11 C10 C9 119.0(6) . . n C12 C11 C10 120.5(6) . . n C12 C11 H11 117(4) . . n C10 C11 H11 123(4) . . n C11 C12 C7 121.2(6) . . n C11 C12 H12 120(4) . . n C7 C12 H12 119(4) . . n O7 C13 H13A 109.5 . . n O7 C13 H13B 109.5 . . n H13A C13 H13B 109.5 . . n O7 C13 H13C 109.5 . . n H13A C13 H13C 109.5 . . n H13B C13 H13C 109.5 . . n O6 C14 H14A 109.5 . . n O6 C14 H14B 109.5 . . n H14A C14 H14B 109.5 . . n O6 C14 H14C 109.5 . . n H14A C14 H14C 109.5 . . n H14B C14 H14C 109.5 . . n _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.971 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.109 #===END