# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Chad Mirkin' _publ_contact_author_email CHADNANO@NORTHWESTERN.EDU _publ_section_title ; Pseudo-Allosteric Regulation of the Anion Binding Affinity of a Macrocyclic Coordination Complex ; loop_ _publ_author_name 'Chad Mirkin' 'Antonio G. DiPasquale' 'Junpei Kuwabara' 'Arnold Rheingold' 'Hyo Jae Yoon.' # Attachment 'CIF_complex6a.txt' data_complex6a _database_code_depnum_ccdc_archive 'CCDC 719264' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common JunII201 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C147 H92 B2 Cl10 F40 N6 O4 P4 Rh2 S4' _chemical_formula_weight 3600.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 11.7786(7) _cell_length_b 15.5130(9) _cell_length_c 22.6329(15) _cell_angle_alpha 71.650(4) _cell_angle_beta 75.085(3) _cell_angle_gamma 71.629(3) _cell_volume 3667.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9250 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1802 _exptl_absorpt_coefficient_mu 5.397 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.5636 _exptl_absorpt_correction_T_max 0.7378 _exptl_absorpt_process_details SADABS _diffrn_refln_scan_width 0.5 _diffrn_refln_scan_rate 5 _space_group.centring_type primitive _space_group.IT_number 2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 33224 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 68.26 _reflns_number_total 13013 _reflns_number_gt 11335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0530P)^2^+4.4800P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13013 _refine_ls_number_parameters 991 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _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 C1 C 1.0961(3) 0.5593(2) 0.80378(15) 0.0234(6) Uani 1 1 d . . . H1A H 1.0395 0.5190 0.8142 0.028 Uiso 1 1 calc R . . H1B H 1.1796 0.5183 0.8047 0.028 Uiso 1 1 calc R . . C2 C 1.0630(3) 0.6173(2) 0.85195(16) 0.0261(7) Uani 1 1 d . . . H2A H 1.1260 0.6508 0.8452 0.031 Uiso 1 1 calc R . . H2B H 1.0582 0.5755 0.8953 0.031 Uiso 1 1 calc R . . C3 C 0.7840(3) 0.9175(2) 0.61889(15) 0.0227(6) Uani 1 1 d . . . H3A H 0.8247 0.9666 0.6146 0.027 Uiso 1 1 calc R . . H3B H 0.7524 0.9313 0.5795 0.027 Uiso 1 1 calc R . . C4 C 0.6802(3) 0.9179(2) 0.67458(15) 0.0223(6) Uani 1 1 d . . . H4A H 0.6334 0.8739 0.6763 0.027 Uiso 1 1 calc R . . H4B H 0.6247 0.9816 0.6707 0.027 Uiso 1 1 calc R . . C5 C 1.1168(3) 0.5621(2) 0.67348(15) 0.0212(6) Uani 1 1 d . . . C6 C 1.0584(3) 0.4896(2) 0.69165(17) 0.0256(7) Uani 1 1 d . . . H6 H 1.0094 0.4774 0.7323 0.031 Uiso 1 1 calc R . . C7 C 1.0716(3) 0.4356(2) 0.65073(18) 0.0305(7) Uani 1 1 d . . . H7 H 1.0312 0.3867 0.6634 0.037 Uiso 1 1 calc R . . C8 C 1.1432(3) 0.4525(3) 0.59151(18) 0.0320(8) Uani 1 1 d . . . H8 H 1.1513 0.4158 0.5634 0.038 Uiso 1 1 calc R . . C9 C 1.2029(3) 0.5228(3) 0.57335(18) 0.0322(8) Uani 1 1 d . . . H9 H 1.2525 0.5341 0.5328 0.039 Uiso 1 1 calc R . . C10 C 1.1908(3) 0.5773(2) 0.61432(16) 0.0259(7) Uani 1 1 d . . . H10 H 1.2330 0.6250 0.6018 0.031 Uiso 1 1 calc R . . C11 C 1.2221(3) 0.6823(2) 0.70506(14) 0.0199(6) Uani 1 1 d . . . C12 C 1.3374(3) 0.6209(2) 0.70477(17) 0.0273(7) Uani 1 1 d . . . H12 H 1.3464 0.5552 0.7142 0.033 Uiso 1 1 calc R . . C13 C 1.4392(3) 0.6552(3) 0.69079(19) 0.0322(8) Uani 1 1 d . . . H13 H 1.5176 0.6129 0.6917 0.039 Uiso 1 1 calc R . . C14 C 1.4263(3) 0.7512(3) 0.67551(18) 0.0324(8) Uani 1 1 d . . . H14 H 1.4963 0.7747 0.6652 0.039 Uiso 1 1 calc R . . C15 C 1.3121(3) 0.8132(2) 0.67523(18) 0.0307(7) Uani 1 1 d . . . H15 H 1.3038 0.8790 0.6644 0.037 Uiso 1 1 calc R . . C16 C 1.2099(3) 0.7788(2) 0.69079(15) 0.0236(6) Uani 1 1 d . . . H16 H 1.1313 0.8210 0.6917 0.028 Uiso 1 1 calc R . . C17 C 0.8252(3) 0.7318(2) 0.60641(14) 0.0191(6) Uani 1 1 d . . . C18 C 0.8083(3) 0.6469(2) 0.64723(15) 0.0219(6) Uani 1 1 d . . . H18 H 0.8323 0.6265 0.6874 0.026 Uiso 1 1 calc R . . C19 C 0.7566(3) 0.5916(2) 0.62959(17) 0.0272(7) Uani 1 1 d . . . H19 H 0.7463 0.5332 0.6575 0.033 Uiso 1 1 calc R . . C20 C 0.7204(3) 0.6218(3) 0.57123(17) 0.0284(7) Uani 1 1 d . . . H20 H 0.6850 0.5840 0.5592 0.034 Uiso 1 1 calc R . . C21 C 0.7354(3) 0.7067(3) 0.53029(16) 0.0288(7) Uani 1 1 d . . . H21 H 0.7093 0.7276 0.4906 0.035 Uiso 1 1 calc R . . C22 C 0.7890(3) 0.7614(2) 0.54755(16) 0.0256(7) Uani 1 1 d . . . H22 H 0.8009 0.8191 0.5192 0.031 Uiso 1 1 calc R . . C23 C 1.0210(3) 0.8239(2) 0.56889(14) 0.0202(6) Uani 1 1 d . . . C24 C 1.0729(3) 0.7726(2) 0.52322(15) 0.0243(7) Uani 1 1 d . . . H24 H 1.0380 0.7258 0.5222 0.029 Uiso 1 1 calc R . . C25 C 1.1756(3) 0.7900(3) 0.47935(16) 0.0299(7) Uani 1 1 d . . . H25 H 1.2102 0.7552 0.4484 0.036 Uiso 1 1 calc R . . C26 C 1.2273(3) 0.8575(3) 0.48064(16) 0.0308(7) Uani 1 1 d . . . H26 H 1.2977 0.8688 0.4508 0.037 Uiso 1 1 calc R . . C27 C 1.1764(3) 0.9093(3) 0.52563(17) 0.0313(8) Uani 1 1 d . . . H27 H 1.2120 0.9559 0.5265 0.038 Uiso 1 1 calc R . . C28 C 1.0741(3) 0.8927(2) 0.56904(15) 0.0256(7) Uani 1 1 d . . . H28 H 1.0394 0.9285 0.5994 0.031 Uiso 1 1 calc R . . C29 C 0.9295(3) 0.7940(2) 0.86929(14) 0.0203(6) Uani 1 1 d . . . C30 C 1.0256(3) 0.8359(2) 0.84181(15) 0.0227(6) Uani 1 1 d . . . H30 H 1.0854 0.8148 0.8087 0.027 Uiso 1 1 calc R . . C31 C 1.0345(3) 0.9084(2) 0.86256(15) 0.0211(6) Uani 1 1 d . . . H31 H 1.1009 0.9362 0.8442 0.025 Uiso 1 1 calc R . . C32 C 0.9458(3) 0.9401(2) 0.91023(14) 0.0186(6) Uani 1 1 d . . . C33 C 0.8496(3) 0.8978(2) 0.93812(14) 0.0200(6) Uani 1 1 d . . . H33 H 0.7899 0.9188 0.9713 0.024 Uiso 1 1 calc R . . C34 C 0.8413(3) 0.8252(2) 0.91734(15) 0.0219(6) Uani 1 1 d . . . H34 H 0.7755 0.7968 0.9360 0.026 Uiso 1 1 calc R . . C35 C 1.0335(3) 1.0629(2) 0.91642(14) 0.0193(6) Uani 1 1 d . . . C36 C 0.9926(3) 1.1541(2) 0.93538(14) 0.0180(6) Uani 1 1 d . . . C37 C 1.0562(3) 1.2224(2) 0.90498(15) 0.0219(6) Uani 1 1 d . . . H37 H 1.1228 1.2129 0.8715 0.026 Uiso 1 1 calc R . . C38 C 0.6183(3) 0.8558(2) 0.80254(15) 0.0209(6) Uani 1 1 d . . . C39 C 0.5810(3) 0.7758(2) 0.81076(17) 0.0266(7) Uani 1 1 d . . . H39 H 0.6295 0.7301 0.7885 0.032 Uiso 1 1 calc R . . C40 C 0.4744(3) 0.7613(2) 0.85073(17) 0.0276(7) Uani 1 1 d . . . H40 H 0.4493 0.7066 0.8556 0.033 Uiso 1 1 calc R . . C41 C 0.4041(3) 0.8281(2) 0.88381(15) 0.0213(6) Uani 1 1 d . . . C42 C 0.4411(3) 0.9085(2) 0.87618(15) 0.0214(6) Uani 1 1 d . . . H42 H 0.3929 0.9539 0.8987 0.026 Uiso 1 1 calc R . . C43 C 0.5483(3) 0.9223(2) 0.83578(15) 0.0212(6) Uani 1 1 d . . . H43 H 0.5738 0.9769 0.8308 0.025 Uiso 1 1 calc R . . C44 C 0.2495(3) 0.7419(2) 0.94964(17) 0.0275(7) Uani 1 1 d . . . C45 C 0.1387(3) 0.7550(2) 1.00057(15) 0.0215(6) Uani 1 1 d . . . C46 C 0.0778(3) 0.6846(2) 1.02670(17) 0.0260(7) Uani 1 1 d . . . H46 H 0.1029 0.6298 1.0114 0.031 Uiso 1 1 calc R . . C47 C -0.0202(3) 0.6957(2) 1.07546(16) 0.0246(7) Uani 1 1 d . . . H47 H -0.0619 0.6478 1.0951 0.029 Uiso 1 1 calc R . . C48 C 0.5899(3) 0.2946(2) 0.69448(14) 0.0182(6) Uani 1 1 d . . . C49 C 0.5642(3) 0.2258(2) 0.67626(14) 0.0193(6) Uani 1 1 d . . . C50 C 0.5112(3) 0.2426(2) 0.62531(16) 0.0222(6) Uani 1 1 d . . . C51 C 0.4826(3) 0.3325(2) 0.58681(15) 0.0237(6) Uani 1 1 d . . . C52 C 0.5080(3) 0.4031(2) 0.60154(15) 0.0232(6) Uani 1 1 d . . . C53 C 0.5598(3) 0.3826(2) 0.65445(15) 0.0195(6) Uani 1 1 d . . . C54 C 0.6655(3) 0.3540(2) 0.77760(14) 0.0186(6) Uani 1 1 d . . . C55 C 0.7656(3) 0.3708(2) 0.78952(15) 0.0211(6) Uani 1 1 d . . . C56 C 0.7560(3) 0.4394(2) 0.81924(15) 0.0248(7) Uani 1 1 d . . . C57 C 0.6448(4) 0.4930(2) 0.83869(16) 0.0298(7) Uani 1 1 d . . . C58 C 0.5421(3) 0.4807(2) 0.82776(16) 0.0279(7) Uani 1 1 d . . . C59 C 0.5548(3) 0.4118(2) 0.79825(15) 0.0217(6) Uani 1 1 d . . . C60 C 0.6011(3) 0.2020(2) 0.81991(14) 0.0180(6) Uani 1 1 d . . . C61 C 0.6613(3) 0.1659(2) 0.87100(15) 0.0180(6) Uani 1 1 d . . . C62 C 0.6110(3) 0.1263(2) 0.93153(14) 0.0199(6) Uani 1 1 d . . . C63 C 0.4927(3) 0.1220(2) 0.94453(15) 0.0228(6) Uani 1 1 d . . . C64 C 0.4288(3) 0.1548(2) 0.89603(16) 0.0240(7) Uani 1 1 d . . . C65 C 0.4822(3) 0.1944(2) 0.83553(15) 0.0212(6) Uani 1 1 d . . . C66 C 0.8005(3) 0.2083(2) 0.72205(14) 0.0178(6) Uani 1 1 d . . . C67 C 0.8504(3) 0.1124(2) 0.73542(15) 0.0203(6) Uani 1 1 d . . . C68 C 0.9553(3) 0.0694(2) 0.70004(15) 0.0221(6) Uani 1 1 d . . . C69 C 1.0174(3) 0.1223(2) 0.64935(15) 0.0241(7) Uani 1 1 d . . . C70 C 0.9737(3) 0.2188(2) 0.63465(15) 0.0214(6) Uani 1 1 d . . . C71 C 0.8671(3) 0.2586(2) 0.67015(15) 0.0202(6) Uani 1 1 d . . . C72 C 0.3202(5) 0.4283(3) 0.9980(2) 0.0546(12) Uani 1 1 d . . . H72A H 0.3366 0.4898 0.9739 0.066 Uiso 1 1 calc R . . H72B H 0.3155 0.4222 1.0434 0.066 Uiso 1 1 calc R . . C73 C 0.3023(3) 1.0957(3) 0.75660(18) 0.0309(7) Uani 1 1 d . . . H73A H 0.2768 1.0843 0.8030 0.037 Uiso 1 1 calc R . . H73B H 0.3872 1.1012 0.7460 0.037 Uiso 1 1 calc R . . C74 C 0.4998(8) 0.0710(6) 0.4850(4) 0.0442(19) Uani 0.50 1 d P . . H74A H 0.5647 0.0974 0.4869 0.053 Uiso 0.50 1 calc PR . . H74B H 0.4364 0.1229 0.4648 0.053 Uiso 0.50 1 calc PR . . B1 B 0.6650(3) 0.2643(2) 0.75312(16) 0.0162(6) Uani 1 1 d . . . N1 N 0.9459(2) 1.01654(18) 0.93134(12) 0.0178(5) Uani 1 1 d . . . H1 H 0.8805 1.0367 0.9576 0.021 Uiso 1 1 calc R . . N2 N 0.2958(2) 0.81802(18) 0.92615(13) 0.0225(5) Uani 1 1 d . . . H2 H 0.2518 0.8682 0.9393 0.027 Uiso 1 1 calc R . . N3 N 0.1050(2) 0.83478(18) 1.01904(12) 0.0191(5) Uani 1 1 d . . . O1 O 1.1379(2) 1.03546(17) 0.88998(12) 0.0271(5) Uani 1 1 d . . . O2 O 0.2899(3) 0.66808(19) 0.93380(15) 0.0444(7) Uani 1 1 d . . . F1 F 0.59355(17) 0.13471(12) 0.71062(9) 0.0236(4) Uani 1 1 d . . . F2 F 0.48743(18) 0.17166(14) 0.61174(9) 0.0283(4) Uani 1 1 d . . . F3 F 0.43362(19) 0.34976(15) 0.53571(9) 0.0323(4) Uani 1 1 d . . . F4 F 0.48404(19) 0.49140(14) 0.56486(9) 0.0299(4) Uani 1 1 d . . . F5 F 0.58042(16) 0.45754(12) 0.66432(8) 0.0222(4) Uani 1 1 d . . . F6 F 0.87953(16) 0.31964(13) 0.77380(9) 0.0242(4) Uani 1 1 d . . . F7 F 0.85608(19) 0.45179(15) 0.83025(10) 0.0322(4) Uani 1 1 d . . . F8 F 0.6350(2) 0.55817(15) 0.86894(11) 0.0405(5) Uani 1 1 d . . . F9 F 0.4317(2) 0.53283(15) 0.84714(11) 0.0380(5) Uani 1 1 d . . . F10 F 0.45110(16) 0.40114(13) 0.79024(9) 0.0261(4) Uani 1 1 d . . . F11 F 0.77731(15) 0.17151(13) 0.86235(8) 0.0201(4) Uani 1 1 d . . . F12 F 0.67657(16) 0.09236(13) 0.97902(8) 0.0236(4) Uani 1 1 d . . . F13 F 0.43927(17) 0.08781(15) 1.00416(9) 0.0295(4) Uani 1 1 d . . . F14 F 0.31265(17) 0.14990(17) 0.90785(10) 0.0352(5) Uani 1 1 d . . . F15 F 0.40858(16) 0.22816(14) 0.79199(9) 0.0255(4) Uani 1 1 d . . . F16 F 0.79577(16) 0.05400(12) 0.78446(9) 0.0233(4) Uani 1 1 d . . . F17 F 0.99720(18) -0.02496(13) 0.71409(10) 0.0292(4) Uani 1 1 d . . . F18 F 1.11838(18) 0.08158(15) 0.61420(10) 0.0318(4) Uani 1 1 d . . . F19 F 1.03272(18) 0.27259(14) 0.58517(9) 0.0288(4) Uani 1 1 d . . . F20 F 0.82633(16) 0.35315(12) 0.65085(9) 0.0229(4) Uani 1 1 d . . . P1 P 1.08627(7) 0.64022(5) 0.72438(4) 0.01793(15) Uani 1 1 d . . . P2 P 0.89396(7) 0.80092(5) 0.63146(3) 0.01754(15) Uani 1 1 d . . . S1 S 0.91524(7) 0.70221(5) 0.84232(3) 0.02067(15) Uani 1 1 d . . . S2 S 0.74684(6) 0.88122(5) 0.74616(3) 0.01920(15) Uani 1 1 d . . . Rh1 Rh 0.912842(19) 0.753096(15) 0.733692(10) 0.01587(7) Uani 1 1 d . . . Cl1 Cl 0.4399(2) 0.33943(12) 0.97461(8) 0.1146(8) Uani 1 1 d . . . Cl2 Cl 0.17838(18) 0.42586(11) 0.98622(8) 0.0886(6) Uani 1 1 d . . . Cl3 Cl 0.29670(11) 0.99910(8) 0.73296(5) 0.0463(2) Uani 1 1 d . . . Cl4 Cl 0.20853(12) 1.20172(9) 0.71999(7) 0.0611(3) Uani 1 1 d . . . Cl5 Cl 0.4377(2) 0.01660(14) 0.56059(7) 0.0963(6) 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 C1 0.0299(17) 0.0163(14) 0.0222(15) -0.0035(12) -0.0052(12) -0.0044(13) C2 0.0318(18) 0.0228(16) 0.0238(16) -0.0058(13) -0.0104(13) -0.0028(13) C3 0.0264(16) 0.0183(14) 0.0210(15) -0.0034(12) -0.0037(12) -0.0041(12) C4 0.0199(15) 0.0182(14) 0.0241(16) -0.0039(12) -0.0038(12) 0.0001(12) C5 0.0195(15) 0.0176(14) 0.0268(16) -0.0089(13) -0.0048(12) -0.0010(12) C6 0.0231(16) 0.0225(16) 0.0324(17) -0.0107(14) -0.0007(13) -0.0071(13) C7 0.0294(18) 0.0266(17) 0.040(2) -0.0163(15) -0.0037(15) -0.0070(14) C8 0.0322(19) 0.0315(18) 0.039(2) -0.0226(16) -0.0051(15) -0.0047(15) C9 0.0327(19) 0.0371(19) 0.0303(18) -0.0188(16) 0.0009(14) -0.0087(15) C10 0.0270(17) 0.0246(16) 0.0272(17) -0.0099(14) -0.0022(13) -0.0071(13) C11 0.0210(15) 0.0184(14) 0.0210(15) -0.0067(12) -0.0036(11) -0.0043(12) C12 0.0232(16) 0.0192(15) 0.0395(19) -0.0092(14) -0.0059(14) -0.0035(13) C13 0.0197(16) 0.0307(18) 0.050(2) -0.0158(17) -0.0066(15) -0.0049(14) C14 0.0247(17) 0.0356(19) 0.042(2) -0.0119(16) -0.0022(15) -0.0152(15) C15 0.0343(19) 0.0237(16) 0.038(2) -0.0117(15) -0.0026(15) -0.0124(14) C16 0.0250(16) 0.0195(15) 0.0269(16) -0.0103(13) -0.0039(12) -0.0029(12) C17 0.0165(14) 0.0232(15) 0.0198(14) -0.0096(12) -0.0020(11) -0.0049(12) C18 0.0183(15) 0.0216(15) 0.0252(16) -0.0052(13) -0.0046(12) -0.0044(12) C19 0.0268(17) 0.0233(16) 0.0331(18) -0.0073(14) -0.0064(14) -0.0076(13) C20 0.0263(17) 0.0323(18) 0.0337(18) -0.0148(15) -0.0049(14) -0.0110(14) C21 0.0314(18) 0.0368(19) 0.0244(16) -0.0100(15) -0.0071(13) -0.0134(15) C22 0.0294(17) 0.0264(16) 0.0230(16) -0.0058(13) -0.0041(13) -0.0107(14) C23 0.0211(15) 0.0206(15) 0.0163(14) -0.0039(12) -0.0024(11) -0.0032(12) C24 0.0226(16) 0.0280(16) 0.0231(16) -0.0096(13) -0.0030(12) -0.0052(13) C25 0.0301(18) 0.0341(18) 0.0216(16) -0.0103(14) 0.0008(13) -0.0038(15) C26 0.0277(17) 0.0342(19) 0.0252(17) -0.0044(14) 0.0033(13) -0.0104(15) C27 0.0312(18) 0.0307(18) 0.0317(18) -0.0040(15) -0.0004(14) -0.0155(15) C28 0.0306(17) 0.0265(16) 0.0194(15) -0.0052(13) 0.0004(13) -0.0114(14) C29 0.0236(15) 0.0222(15) 0.0167(14) -0.0048(12) -0.0051(11) -0.0069(12) C30 0.0230(16) 0.0255(16) 0.0192(15) -0.0078(13) -0.0016(12) -0.0053(13) C31 0.0181(15) 0.0255(16) 0.0208(15) -0.0075(13) 0.0000(11) -0.0083(12) C32 0.0161(14) 0.0202(14) 0.0202(14) -0.0060(12) -0.0062(11) -0.0024(11) C33 0.0180(14) 0.0215(15) 0.0194(14) -0.0079(12) 0.0006(11) -0.0040(12) C34 0.0209(15) 0.0226(15) 0.0231(15) -0.0050(13) -0.0034(12) -0.0077(12) C35 0.0165(15) 0.0225(15) 0.0184(14) -0.0065(12) -0.0035(11) -0.0028(12) C36 0.0142(14) 0.0204(14) 0.0199(14) -0.0061(12) -0.0043(11) -0.0031(11) C37 0.0190(15) 0.0243(16) 0.0216(15) -0.0032(13) -0.0046(12) -0.0064(12) C38 0.0170(14) 0.0220(15) 0.0238(15) -0.0081(13) -0.0017(12) -0.0045(12) C39 0.0255(16) 0.0195(15) 0.0320(17) -0.0131(14) 0.0042(13) -0.0030(13) C40 0.0251(17) 0.0216(16) 0.0362(18) -0.0146(14) 0.0038(14) -0.0061(13) C41 0.0185(15) 0.0191(14) 0.0229(15) -0.0060(12) -0.0011(12) -0.0016(12) C42 0.0216(15) 0.0212(15) 0.0206(15) -0.0103(12) 0.0001(12) -0.0026(12) C43 0.0217(15) 0.0217(15) 0.0206(15) -0.0084(12) -0.0020(12) -0.0045(12) C44 0.0229(16) 0.0234(16) 0.0338(18) -0.0116(14) 0.0048(14) -0.0064(13) C45 0.0177(15) 0.0193(15) 0.0253(16) -0.0073(13) -0.0001(12) -0.0031(12) C46 0.0228(16) 0.0210(15) 0.0335(18) -0.0085(14) -0.0021(13) -0.0053(13) C47 0.0223(16) 0.0220(15) 0.0291(17) -0.0050(13) -0.0024(13) -0.0085(13) C48 0.0150(14) 0.0203(14) 0.0202(14) -0.0079(12) -0.0020(11) -0.0036(11) C49 0.0182(14) 0.0181(14) 0.0208(15) -0.0054(12) -0.0020(11) -0.0039(11) C50 0.0204(15) 0.0265(16) 0.0273(16) -0.0147(13) -0.0013(12) -0.0106(13) C51 0.0239(16) 0.0305(17) 0.0191(15) -0.0063(13) -0.0083(12) -0.0066(13) C52 0.0243(16) 0.0196(15) 0.0204(15) -0.0008(12) -0.0035(12) -0.0031(12) C53 0.0191(14) 0.0201(15) 0.0219(15) -0.0076(12) -0.0036(11) -0.0061(12) C54 0.0232(15) 0.0155(14) 0.0175(14) -0.0045(12) -0.0038(11) -0.0049(12) C55 0.0220(15) 0.0209(15) 0.0199(15) -0.0041(12) -0.0031(12) -0.0062(12) C56 0.0310(17) 0.0244(16) 0.0239(16) -0.0037(13) -0.0088(13) -0.0131(14) C57 0.048(2) 0.0206(16) 0.0264(17) -0.0114(14) -0.0131(15) -0.0058(15) C58 0.0297(18) 0.0212(16) 0.0284(17) -0.0105(14) -0.0051(14) 0.0035(13) C59 0.0215(15) 0.0209(15) 0.0221(15) -0.0059(13) -0.0047(12) -0.0035(12) C60 0.0164(14) 0.0168(14) 0.0207(15) -0.0062(12) -0.0025(11) -0.0033(11) C61 0.0125(13) 0.0191(14) 0.0232(15) -0.0068(12) -0.0016(11) -0.0048(11) C62 0.0184(15) 0.0219(15) 0.0185(14) -0.0044(12) -0.0049(11) -0.0034(12) C63 0.0181(15) 0.0268(16) 0.0199(15) -0.0043(13) 0.0019(12) -0.0068(13) C64 0.0141(14) 0.0301(17) 0.0278(16) -0.0071(14) -0.0010(12) -0.0079(13) C65 0.0177(15) 0.0241(15) 0.0223(15) -0.0064(13) -0.0065(12) -0.0033(12) C66 0.0148(14) 0.0194(14) 0.0213(14) -0.0082(12) -0.0032(11) -0.0041(11) C67 0.0190(15) 0.0219(15) 0.0214(15) -0.0063(12) -0.0050(12) -0.0050(12) C68 0.0234(16) 0.0175(14) 0.0254(16) -0.0090(13) -0.0052(12) -0.0007(12) C69 0.0189(15) 0.0323(17) 0.0228(16) -0.0154(14) 0.0004(12) -0.0039(13) C70 0.0202(15) 0.0268(16) 0.0197(15) -0.0085(13) 0.0000(12) -0.0095(13) C71 0.0207(15) 0.0187(14) 0.0230(15) -0.0071(12) -0.0051(12) -0.0046(12) C72 0.075(3) 0.047(3) 0.051(3) -0.021(2) -0.021(2) -0.011(2) C73 0.0283(18) 0.0345(19) 0.0338(19) -0.0091(15) -0.0055(14) -0.0132(15) C74 0.036(4) 0.040(4) 0.056(5) -0.017(4) -0.001(4) -0.012(4) B1 0.0141(15) 0.0144(15) 0.0198(16) -0.0056(13) -0.0019(12) -0.0029(12) N1 0.0145(12) 0.0202(12) 0.0181(12) -0.0068(10) -0.0004(9) -0.0036(10) N2 0.0194(13) 0.0172(12) 0.0288(14) -0.0103(11) 0.0031(11) -0.0035(10) N3 0.0171(12) 0.0190(12) 0.0211(13) -0.0063(10) -0.0041(10) -0.0027(10) O1 0.0174(11) 0.0297(12) 0.0363(13) -0.0173(11) 0.0039(9) -0.0071(9) O2 0.0429(16) 0.0275(13) 0.0585(18) -0.0254(13) 0.0239(13) -0.0149(12) F1 0.0266(9) 0.0160(8) 0.0297(10) -0.0056(7) -0.0075(7) -0.0056(7) F2 0.0309(10) 0.0304(10) 0.0334(10) -0.0164(9) -0.0070(8) -0.0118(8) F3 0.0396(12) 0.0387(11) 0.0248(10) -0.0079(9) -0.0158(9) -0.0102(9) F4 0.0383(11) 0.0244(10) 0.0257(10) 0.0019(8) -0.0146(8) -0.0072(8) F5 0.0278(9) 0.0165(8) 0.0250(9) -0.0046(7) -0.0082(7) -0.0071(7) F6 0.0192(9) 0.0280(9) 0.0289(10) -0.0111(8) -0.0032(7) -0.0079(7) F7 0.0385(11) 0.0365(11) 0.0339(11) -0.0115(9) -0.0112(9) -0.0198(9) F8 0.0599(15) 0.0272(10) 0.0438(13) -0.0220(10) -0.0174(11) -0.0045(10) F9 0.0369(12) 0.0320(11) 0.0438(12) -0.0245(10) -0.0084(10) 0.0086(9) F10 0.0181(9) 0.0277(10) 0.0315(10) -0.0104(8) -0.0061(7) -0.0002(7) F11 0.0121(8) 0.0268(9) 0.0209(8) -0.0045(7) -0.0028(6) -0.0060(7) F12 0.0177(8) 0.0339(10) 0.0175(8) -0.0051(8) -0.0036(7) -0.0052(7) F13 0.0225(9) 0.0396(11) 0.0205(9) -0.0021(8) 0.0031(7) -0.0109(8) F14 0.0153(9) 0.0559(14) 0.0323(11) -0.0030(10) -0.0024(8) -0.0158(9) F15 0.0175(9) 0.0347(10) 0.0253(9) -0.0050(8) -0.0084(7) -0.0069(8) F16 0.0249(9) 0.0176(8) 0.0248(9) -0.0037(7) -0.0004(7) -0.0066(7) F17 0.0301(10) 0.0191(9) 0.0332(10) -0.0109(8) -0.0021(8) 0.0023(8) F18 0.0246(10) 0.0377(11) 0.0314(10) -0.0192(9) 0.0055(8) -0.0036(8) F19 0.0297(10) 0.0341(10) 0.0222(9) -0.0087(8) 0.0069(8) -0.0153(8) F20 0.0252(9) 0.0174(8) 0.0252(9) -0.0044(7) -0.0017(7) -0.0074(7) P1 0.0172(4) 0.0157(3) 0.0207(4) -0.0065(3) -0.0022(3) -0.0030(3) P2 0.0197(4) 0.0170(3) 0.0156(3) -0.0052(3) -0.0010(3) -0.0049(3) S1 0.0242(4) 0.0218(3) 0.0177(3) -0.0071(3) -0.0026(3) -0.0070(3) S2 0.0168(3) 0.0187(3) 0.0219(3) -0.0089(3) 0.0003(3) -0.0034(3) Rh1 0.01536(11) 0.01649(11) 0.01628(11) -0.00653(8) -0.00086(8) -0.00395(8) Cl1 0.1487(18) 0.0590(9) 0.0689(10) -0.0049(8) 0.0109(10) 0.0294(10) Cl2 0.1266(14) 0.0708(9) 0.0830(10) 0.0302(8) -0.0662(10) -0.0564(10) Cl3 0.0614(6) 0.0478(5) 0.0418(5) -0.0202(4) -0.0044(4) -0.0255(5) Cl4 0.0602(7) 0.0500(6) 0.0776(8) -0.0163(6) -0.0400(6) 0.0021(5) Cl5 0.1525(17) 0.1074(13) 0.0549(8) -0.0401(9) 0.0291(9) -0.0867(13) _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 C1 C2 1.525(4) . ? C1 P1 1.847(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 S1 1.839(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.514(4) . ? C3 P2 1.849(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 S2 1.832(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.392(5) . ? C5 C6 1.399(4) . ? C5 P1 1.821(3) . ? C6 C7 1.384(5) . ? C6 H6 0.9500 . ? C7 C8 1.383(5) . ? C7 H7 0.9500 . ? C8 C9 1.381(5) . ? C8 H8 0.9500 . ? C9 C10 1.395(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.391(5) . ? C11 C16 1.397(4) . ? C11 P1 1.815(3) . ? C12 C13 1.386(5) . ? C12 H12 0.9500 . ? C13 C14 1.387(5) . ? C13 H13 0.9500 . ? C14 C15 1.385(5) . ? C14 H14 0.9500 . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.390(4) . ? C17 C22 1.397(4) . ? C17 P2 1.815(3) . ? C18 C19 1.392(5) . ? C18 H18 0.9500 . ? C19 C20 1.386(5) . ? C19 H19 0.9500 . ? C20 C21 1.386(5) . ? C20 H20 0.9500 . ? C21 C22 1.394(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.397(5) . ? C23 C24 1.401(4) . ? C23 P2 1.817(3) . ? C24 C25 1.393(5) . ? C24 H24 0.9500 . ? C25 C26 1.377(5) . ? C25 H25 0.9500 . ? C26 C27 1.392(5) . ? C26 H26 0.9500 . ? C27 C28 1.382(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.388(4) . ? C29 C30 1.393(4) . ? C29 S1 1.782(3) . ? C30 C31 1.389(4) . ? C30 H30 0.9500 . ? C31 C32 1.388(4) . ? C31 H31 0.9500 . ? C32 C33 1.397(4) . ? C32 N1 1.412(4) . ? C33 C34 1.389(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 O1 1.226(4) . ? C35 N1 1.353(4) . ? C35 C36 1.505(4) . ? C36 N3 1.339(4) 2_677 ? C36 C37 1.390(4) . ? C37 C47 1.382(5) 2_677 ? C37 H37 0.9500 . ? C38 C39 1.388(5) . ? C38 C43 1.395(4) . ? C38 S2 1.772(3) . ? C39 C40 1.382(5) . ? C39 H39 0.9500 . ? C40 C41 1.395(4) . ? C40 H40 0.9500 . ? C41 C42 1.394(4) . ? C41 N2 1.404(4) . ? C42 C43 1.389(4) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 O2 1.222(4) . ? C44 N2 1.354(4) . ? C44 C45 1.510(4) . ? C45 N3 1.339(4) . ? C45 C46 1.388(4) . ? C46 C47 1.385(5) . ? C46 H46 0.9500 . ? C47 C37 1.382(5) 2_677 ? C47 H47 0.9500 . ? C48 C53 1.375(4) . ? C48 C49 1.395(4) . ? C48 B1 1.647(4) . ? C49 F1 1.363(4) . ? C49 C50 1.366(4) . ? C50 F2 1.355(3) . ? C50 C51 1.382(5) . ? C51 F3 1.339(4) . ? C51 C52 1.373(5) . ? C52 F4 1.344(4) . ? C52 C53 1.386(4) . ? C53 F5 1.353(3) . ? C54 C55 1.389(4) . ? C54 C59 1.392(4) . ? C54 B1 1.654(4) . ? C55 F6 1.349(4) . ? C55 C56 1.391(4) . ? C56 F7 1.347(4) . ? C56 C57 1.359(5) . ? C57 F8 1.351(4) . ? C57 C58 1.375(5) . ? C58 F9 1.344(4) . ? C58 C59 1.380(5) . ? C59 F10 1.347(4) . ? C60 C61 1.385(4) . ? C60 C65 1.387(4) . ? C60 B1 1.655(4) . ? C61 F11 1.356(3) . ? C61 C62 1.374(4) . ? C62 F12 1.358(3) . ? C62 C63 1.367(4) . ? C63 F13 1.349(4) . ? C63 C64 1.364(5) . ? C64 F14 1.347(4) . ? C64 C65 1.385(5) . ? C65 F15 1.351(4) . ? C66 C67 1.381(4) . ? C66 C71 1.392(4) . ? C66 B1 1.653(4) . ? C67 F16 1.354(4) . ? C67 C68 1.386(4) . ? C68 F17 1.348(4) . ? C68 C69 1.371(5) . ? C69 F18 1.343(4) . ? C69 C70 1.379(5) . ? C70 F19 1.345(4) . ? C70 C71 1.382(4) . ? C71 F20 1.355(4) . ? C72 Cl1 1.737(5) . ? C72 Cl2 1.771(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 Cl4 1.755(4) . ? C73 Cl3 1.767(4) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 Cl5 1.735(9) . ? C74 Cl5 1.820(9) 2_656 ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? N1 H1 0.8800 . ? N2 H2 0.8800 . ? N3 C36 1.339(4) 2_677 ? P1 Rh1 2.2449(8) . ? P2 Rh1 2.2437(8) . ? S1 Rh1 2.3385(8) . ? S2 Rh1 2.3394(7) . ? Cl5 C74 1.820(9) 2_656 ? 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 C1 P1 108.7(2) . . ? C2 C1 H1A 109.9 . . ? P1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? P1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C1 C2 S1 108.6(2) . . ? C1 C2 H2A 110.0 . . ? S1 C2 H2A 110.0 . . ? C1 C2 H2B 110.0 . . ? S1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C4 C3 P2 109.3(2) . . ? C4 C3 H3A 109.8 . . ? P2 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? P2 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C3 C4 S2 107.2(2) . . ? C3 C4 H4A 110.3 . . ? S2 C4 H4A 110.3 . . ? C3 C4 H4B 110.3 . . ? S2 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? C10 C5 C6 118.9(3) . . ? C10 C5 P1 121.0(2) . . ? C6 C5 P1 119.9(2) . . ? C7 C6 C5 120.4(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 119.9(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.3(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C5 C10 C9 120.1(3) . . ? C5 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C16 119.3(3) . . ? C12 C11 P1 121.8(2) . . ? C16 C11 P1 118.9(2) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.3(3) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C18 C17 C22 119.4(3) . . ? C18 C17 P2 118.7(2) . . ? C22 C17 P2 122.0(2) . . ? C17 C18 C19 120.4(3) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 119.8(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 119.8(3) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C17 120.2(3) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? C28 C23 C24 118.6(3) . . ? C28 C23 P2 117.8(2) . . ? C24 C23 P2 123.5(2) . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 120.4(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.0(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 119.9(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C23 121.0(3) . . ? C27 C28 H28 119.5 . . ? C23 C28 H28 119.5 . . ? C34 C29 C30 120.0(3) . . ? C34 C29 S1 119.1(2) . . ? C30 C29 S1 120.9(2) . . ? C31 C30 C29 120.3(3) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 C30 119.6(3) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 120.2(3) . . ? C31 C32 N1 122.6(3) . . ? C33 C32 N1 117.2(3) . . ? C34 C33 C32 120.0(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C29 C34 C33 119.9(3) . . ? C29 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? O1 C35 N1 124.9(3) . . ? O1 C35 C36 121.1(3) . . ? N1 C35 C36 114.0(3) . . ? N3 C36 C37 123.3(3) 2_677 . ? N3 C36 C35 117.5(3) 2_677 . ? C37 C36 C35 119.2(3) . . ? C47 C37 C36 118.4(3) 2_677 . ? C47 C37 H37 120.8 2_677 . ? C36 C37 H37 120.8 . . ? C39 C38 C43 119.7(3) . . ? C39 C38 S2 121.9(2) . . ? C43 C38 S2 118.2(2) . . ? C40 C39 C38 121.1(3) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 119.2(3) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C42 C41 C40 120.1(3) . . ? C42 C41 N2 117.0(3) . . ? C40 C41 N2 122.8(3) . . ? C43 C42 C41 120.2(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C38 119.7(3) . . ? C42 C43 H43 120.2 . . ? C38 C43 H43 120.2 . . ? O2 C44 N2 126.3(3) . . ? O2 C44 C45 120.7(3) . . ? N2 C44 C45 113.0(3) . . ? N3 C45 C46 123.1(3) . . ? N3 C45 C44 117.5(3) . . ? C46 C45 C44 119.4(3) . . ? C47 C46 C45 118.7(3) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C37 C47 C46 118.9(3) 2_677 . ? C37 C47 H47 120.5 2_677 . ? C46 C47 H47 120.5 . . ? C53 C48 C49 113.0(3) . . ? C53 C48 B1 126.5(3) . . ? C49 C48 B1 120.0(3) . . ? F1 C49 C50 116.3(3) . . ? F1 C49 C48 119.1(3) . . ? C50 C49 C48 124.6(3) . . ? F2 C50 C49 120.6(3) . . ? F2 C50 C51 119.5(3) . . ? C49 C50 C51 119.8(3) . . ? F3 C51 C52 121.1(3) . . ? F3 C51 C50 120.6(3) . . ? C52 C51 C50 118.4(3) . . ? F4 C52 C51 120.6(3) . . ? F4 C52 C53 119.8(3) . . ? C51 C52 C53 119.5(3) . . ? F5 C53 C48 121.1(3) . . ? F5 C53 C52 114.3(3) . . ? C48 C53 C52 124.6(3) . . ? C55 C54 C59 113.9(3) . . ? C55 C54 B1 126.6(3) . . ? C59 C54 B1 118.7(3) . . ? F6 C55 C54 121.7(3) . . ? F6 C55 C56 115.3(3) . . ? C54 C55 C56 123.0(3) . . ? F7 C56 C57 119.5(3) . . ? F7 C56 C55 120.4(3) . . ? C57 C56 C55 120.0(3) . . ? F8 C57 C56 120.1(3) . . ? F8 C57 C58 120.0(3) . . ? C56 C57 C58 119.9(3) . . ? F9 C58 C57 120.5(3) . . ? F9 C58 C59 120.9(3) . . ? C57 C58 C59 118.6(3) . . ? F10 C59 C58 116.1(3) . . ? F10 C59 C54 119.4(3) . . ? C58 C59 C54 124.5(3) . . ? C61 C60 C65 113.2(3) . . ? C61 C60 B1 118.8(3) . . ? C65 C60 B1 127.0(3) . . ? F11 C61 C62 116.3(3) . . ? F11 C61 C60 119.0(3) . . ? C62 C61 C60 124.7(3) . . ? F12 C62 C63 119.3(3) . . ? F12 C62 C61 120.9(3) . . ? C63 C62 C61 119.7(3) . . ? F13 C63 C64 120.6(3) . . ? F13 C63 C62 120.9(3) . . ? C64 C63 C62 118.5(3) . . ? F14 C64 C63 119.3(3) . . ? F14 C64 C65 120.4(3) . . ? C63 C64 C65 120.3(3) . . ? F15 C65 C64 115.0(3) . . ? F15 C65 C60 121.4(3) . . ? C64 C65 C60 123.5(3) . . ? C67 C66 C71 113.7(3) . . ? C67 C66 B1 127.0(3) . . ? C71 C66 B1 118.6(3) . . ? F16 C67 C66 120.6(3) . . ? F16 C67 C68 115.8(3) . . ? C66 C67 C68 123.6(3) . . ? F17 C68 C69 118.8(3) . . ? F17 C68 C67 120.9(3) . . ? C69 C68 C67 120.3(3) . . ? F18 C69 C68 120.9(3) . . ? F18 C69 C70 120.3(3) . . ? C68 C69 C70 118.8(3) . . ? F19 C70 C69 120.1(3) . . ? F19 C70 C71 120.9(3) . . ? C69 C70 C71 119.0(3) . . ? F20 C71 C70 115.7(3) . . ? F20 C71 C66 119.7(3) . . ? C70 C71 C66 124.6(3) . . ? Cl1 C72 Cl2 113.0(3) . . ? Cl1 C72 H72A 109.0 . . ? Cl2 C72 H72A 109.0 . . ? Cl1 C72 H72B 109.0 . . ? Cl2 C72 H72B 109.0 . . ? H72A C72 H72B 107.8 . . ? Cl4 C73 Cl3 112.4(2) . . ? Cl4 C73 H73A 109.1 . . ? Cl3 C73 H73A 109.1 . . ? Cl4 C73 H73B 109.1 . . ? Cl3 C73 H73B 109.1 . . ? H73A C73 H73B 107.9 . . ? Cl5 C74 Cl5 108.1(5) . 2_656 ? Cl5 C74 H74A 110.1 . . ? Cl5 C74 H74A 110.1 2_656 . ? Cl5 C74 H74B 110.1 . . ? Cl5 C74 H74B 110.1 2_656 . ? H74A C74 H74B 108.4 . . ? C48 B1 C66 101.3(2) . . ? C48 B1 C54 113.9(2) . . ? C66 B1 C54 114.3(2) . . ? C48 B1 C60 113.7(2) . . ? C66 B1 C60 114.8(2) . . ? C54 B1 C60 99.6(2) . . ? C35 N1 C32 128.4(3) . . ? C35 N1 H1 115.8 . . ? C32 N1 H1 115.8 . . ? C44 N2 C41 129.1(3) . . ? C44 N2 H2 115.5 . . ? C41 N2 H2 115.5 . . ? C36 N3 C45 117.4(3) 2_677 . ? C11 P1 C5 104.59(14) . . ? C11 P1 C1 103.09(15) . . ? C5 P1 C1 103.64(14) . . ? C11 P1 Rh1 113.68(10) . . ? C5 P1 Rh1 122.75(10) . . ? C1 P1 Rh1 107.02(11) . . ? C17 P2 C23 105.82(14) . . ? C17 P2 C3 102.58(15) . . ? C23 P2 C3 101.30(14) . . ? C17 P2 Rh1 115.39(10) . . ? C23 P2 Rh1 121.54(10) . . ? C3 P2 Rh1 107.71(10) . . ? C29 S1 C2 100.78(15) . . ? C29 S1 Rh1 109.82(10) . . ? C2 S1 Rh1 106.33(11) . . ? C38 S2 C4 98.38(15) . . ? C38 S2 Rh1 116.38(11) . . ? C4 S2 Rh1 105.72(10) . . ? P2 Rh1 P1 97.34(3) . . ? P2 Rh1 S1 175.06(3) . . ? P1 Rh1 S1 85.78(3) . . ? P2 Rh1 S2 85.34(3) . . ? P1 Rh1 S2 172.63(3) . . ? S1 Rh1 S2 92.02(3) . . ? C74 Cl5 C74 71.9(5) . 2_656 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.156 _refine_diff_density_min -1.464 _refine_diff_density_rms 0.080 # Attachment 'CIF_complex7.txt' data_complex7 _database_code_depnum_ccdc_archive 'CCDC 719265' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H94 Cl10 N6 O4 P4 Rh2 S4' _chemical_formula_weight 2232.23 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' N N 0.0061 0.0033 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 P2(1)/c 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 17.477(5) _cell_length_b 37.810(10) _cell_length_c 15.719(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.518(4) _cell_angle_gamma 90.00 _cell_volume 9729(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7666 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.11 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4560 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7677 _exptl_absorpt_correction_T_max 0.8088 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 70319 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17150 _reflns_number_gt 13331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered CH2CL2, the recrystallization solvent, was rendered using SQUEEZE. FOund 623e/uc. Calc'ed for 16 CH2CL2, 672e/uc. SOlvent is included in the formula and intensive properties. 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^)+(0.1000P)^2^+6.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17150 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.42420(2) 0.922206(9) 0.44610(2) 0.03602(12) Uani 1 1 d . . . Rh2 Rh 0.84554(3) 0.653944(9) 0.67661(2) 0.03731(13) Uani 1 1 d . . . Cl1 Cl 0.34642(12) 0.94055(5) 0.83186(13) 0.0808(5) Uani 1 1 d . . . Cl2 Cl 0.84708(7) 0.85033(3) 0.64257(7) 0.0331(2) Uani 1 1 d . . . S1 S 0.48938(8) 0.95062(3) 0.35602(8) 0.0403(3) Uani 1 1 d . . . S2 S 0.48835(7) 0.95894(3) 0.57205(8) 0.0346(3) Uani 1 1 d . . . S3 S 0.97330(9) 0.66892(3) 0.66648(10) 0.0491(3) Uani 1 1 d . . . S4 S 0.89119(9) 0.67065(3) 0.82973(8) 0.0431(3) Uani 1 1 d . . . P1 P 0.37016(9) 0.88615(3) 0.32694(9) 0.0459(3) Uani 1 1 d . . . P2 P 0.34555(8) 0.90423(3) 0.52376(9) 0.0413(3) Uani 1 1 d . . . P3 P 0.81648(9) 0.63114(3) 0.53692(9) 0.0421(3) Uani 1 1 d . . . P4 P 0.72902(9) 0.63875(3) 0.69739(9) 0.0433(3) Uani 1 1 d . . . O1' O 0.9109(2) 0.98038(9) 0.7482(2) 0.0446(8) Uani 1 1 d . . . O1 O 0.9024(3) 0.96940(12) 0.4659(3) 0.0823(15) Uani 1 1 d . . . O2' O 1.1123(2) 0.82381(10) 0.9343(3) 0.0547(10) Uani 1 1 d . . . O2 O 1.1587(3) 0.83067(14) 0.6800(6) 0.133(3) Uani 1 1 d . . . N1 N 0.8474(2) 0.92176(10) 0.5109(3) 0.0345(9) Uani 1 1 d . . . H1A H 0.8604 0.9018 0.5413 0.041 Uiso 1 1 calc R . . N1' N 0.8450(2) 0.92714(9) 0.7367(2) 0.0319(8) Uani 1 1 d . . . H1'A H 0.8551 0.9045 0.7478 0.038 Uiso 1 1 calc R . . N2' N 0.9803(2) 0.82289(10) 0.8368(3) 0.0398(10) Uani 1 1 d . . . H2'A H 0.9419 0.8364 0.8000 0.048 Uiso 1 1 calc R . . N2 N 1.0208(3) 0.82428(11) 0.6278(3) 0.0473(11) Uani 1 1 d . . . H2A H 0.9753 0.8365 0.6055 0.057 Uiso 1 1 calc R . . N3' N 0.9866(2) 0.89410(10) 0.8183(2) 0.0353(9) Uani 1 1 d . . . N3 N 1.0030(3) 0.89377(11) 0.5834(3) 0.0437(10) Uani 1 1 d . . . C1 C 0.3601(3) 0.93589(13) 0.6174(3) 0.0436(12) Uani 1 1 d . . . H1B H 0.3293 0.9579 0.5937 0.052 Uiso 1 1 calc R . . H1C H 0.3393 0.9256 0.6630 0.052 Uiso 1 1 calc R . . C1' C 0.4390(4) 0.88880(16) 0.2604(4) 0.0603(17) Uani 1 1 d . . . H1D H 0.4915 0.8768 0.2933 0.072 Uiso 1 1 calc R . . H1E H 0.4136 0.8771 0.2007 0.072 Uiso 1 1 calc R . . C2 C 0.4500(3) 0.94414(13) 0.6612(3) 0.0411(11) Uani 1 1 d . . . H2B H 0.4801 0.9228 0.6916 0.049 Uiso 1 1 calc R . . H2C H 0.4582 0.9629 0.7074 0.049 Uiso 1 1 calc R . . C2' C 0.4533(3) 0.92708(16) 0.2478(4) 0.0517(14) Uani 1 1 d . . . H2'B H 0.4017 0.9380 0.2077 0.062 Uiso 1 1 calc R . . H2'C H 0.4942 0.9294 0.2177 0.062 Uiso 1 1 calc R . . C3' C 0.5951(3) 0.94958(12) 0.6246(3) 0.0326(10) Uani 1 1 d . . . C3 C 0.5959(3) 0.94060(12) 0.3964(3) 0.0362(11) Uani 1 1 d . . . C4' C 0.6227(3) 0.91666(11) 0.6610(3) 0.0316(10) Uani 1 1 d . . . H4'A H 0.5850 0.8984 0.6597 0.038 Uiso 1 1 calc R . . C4 C 0.6271(3) 0.91132(12) 0.4526(3) 0.0334(10) Uani 1 1 d . . . H4A H 0.5909 0.8953 0.4657 0.040 Uiso 1 1 calc R . . C5' C 0.7057(3) 0.91058(11) 0.6992(3) 0.0339(10) Uani 1 1 d . . . H5'A H 0.7246 0.8881 0.7253 0.041 Uiso 1 1 calc R . . C5 C 0.7092(3) 0.90585(12) 0.4885(3) 0.0338(10) Uani 1 1 d . . . H5A H 0.7301 0.8859 0.5262 0.041 Uiso 1 1 calc R . . C6' C 0.7621(3) 0.93652(12) 0.7003(3) 0.0314(10) Uani 1 1 d . . . C6 C 0.7627(3) 0.92926(11) 0.4704(3) 0.0349(11) Uani 1 1 d . . . C7' C 0.7347(3) 0.96988(12) 0.6640(3) 0.0368(11) Uani 1 1 d . . . H7'A H 0.7727 0.9879 0.6648 0.044 Uiso 1 1 calc R . . C7 C 0.7321(3) 0.95825(12) 0.4125(3) 0.0405(11) Uani 1 1 d . . . H7A H 0.7682 0.9740 0.3984 0.049 Uiso 1 1 calc R . . C8' C 0.6506(3) 0.97646(12) 0.6265(3) 0.0342(10) Uani 1 1 d . . . H8'A H 0.6314 0.9991 0.6023 0.041 Uiso 1 1 calc R . . C8 C 0.6489(3) 0.96338(12) 0.3767(3) 0.0394(11) Uani 1 1 d . . . H8A H 0.6277 0.9830 0.3378 0.047 Uiso 1 1 calc R . . C9' C 0.9118(3) 0.94836(13) 0.7572(3) 0.0369(11) Uani 1 1 d . . . C9 C 0.9107(3) 0.94214(14) 0.5078(4) 0.0478(13) Uani 1 1 d . . . C10' C 0.9915(3) 0.92851(12) 0.7969(3) 0.0351(10) Uani 1 1 d . . . C10 C 0.9934(3) 0.92822(14) 0.5606(4) 0.0451(12) Uani 1 1 d . . . C11' C 1.0639(3) 0.94554(13) 0.8105(4) 0.0443(12) Uani 1 1 d . . . H11A H 1.0643 0.9697 0.7940 0.053 Uiso 1 1 calc R . . C11 C 1.0589(3) 0.95227(15) 0.5829(4) 0.0484(13) Uani 1 1 d . . . H11B H 1.0505 0.9764 0.5649 0.058 Uiso 1 1 calc R . . C12' C 1.1377(3) 0.92695(15) 0.8491(4) 0.0493(13) Uani 1 1 d . . . H12A H 1.1889 0.9380 0.8586 0.059 Uiso 1 1 calc R . . C12 C 1.1361(3) 0.93953(16) 0.6322(4) 0.0546(14) Uani 1 1 d . . . H12B H 1.1816 0.9551 0.6505 0.065 Uiso 1 1 calc R . . C13' C 1.1328(3) 0.89194(15) 0.8729(4) 0.0489(13) Uani 1 1 d . . . H13A H 1.1812 0.8787 0.9015 0.059 Uiso 1 1 calc R . . C13 C 1.1466(4) 0.90401(16) 0.6545(5) 0.0607(16) Uani 1 1 d . . . H13B H 1.1994 0.8948 0.6866 0.073 Uiso 1 1 calc R . . C14' C 1.0577(3) 0.87661(13) 0.8548(3) 0.0387(11) Uani 1 1 d . . . C14 C 1.0786(3) 0.88217(15) 0.6290(4) 0.0537(14) Uani 1 1 d . . . C15' C 1.0520(3) 0.83850(14) 0.8784(3) 0.0422(12) Uani 1 1 d . . . C15 C 1.0909(4) 0.84307(17) 0.6489(6) 0.071(2) Uani 1 1 d . . . C16 C 1.0114(3) 0.78753(13) 0.6370(4) 0.0449(12) Uani 1 1 d . . . C19' C 0.9130(3) 0.71655(13) 0.8409(3) 0.0432(12) Uani 1 1 d . . . C17 C 1.0766(5) 0.7654(2) 0.6849(7) 0.113(4) Uani 1 1 d . . . H17A H 1.1301 0.7747 0.7129 0.136 Uiso 1 1 calc R . . C18' C 0.8575(3) 0.74186(13) 0.7926(4) 0.0491(13) Uani 1 1 d . . . H18A H 0.8030 0.7351 0.7583 0.059 Uiso 1 1 calc R . . C18 C 1.0612(4) 0.72934(19) 0.6905(7) 0.103(3) Uani 1 1 d . . . H18B H 1.1056 0.7140 0.7205 0.124 Uiso 1 1 calc R . . C19 C 0.9850(3) 0.71560(14) 0.6542(4) 0.0482(13) Uani 1 1 d . . . C17' C 0.8807(3) 0.77701(13) 0.7937(4) 0.0489(13) Uani 1 1 d . . . H19A H 0.8422 0.7939 0.7589 0.059 Uiso 1 1 calc R . . C16' C 0.9582(3) 0.78760(12) 0.8441(3) 0.0386(11) Uani 1 1 d . . . C20 C 0.9220(3) 0.73730(14) 0.6086(4) 0.0522(14) Uani 1 1 d . . . H20A H 0.8683 0.7281 0.5822 0.063 Uiso 1 1 calc R . . C20' C 0.9875(4) 0.72761(15) 0.8959(5) 0.0694(19) Uani 1 1 d . . . H20B H 1.0240 0.7109 0.9344 0.083 Uiso 1 1 calc R . . C21 C 0.9365(3) 0.77311(14) 0.6008(4) 0.0506(14) Uani 1 1 d . . . H21A H 0.8919 0.7880 0.5687 0.061 Uiso 1 1 calc R . . C21' C 1.0122(4) 0.76216(15) 0.8982(5) 0.078(2) Uani 1 1 d . . . H21B H 1.0657 0.7689 0.9361 0.093 Uiso 1 1 calc R . . C22 C 0.9693(4) 0.65328(15) 0.5549(4) 0.0582(16) Uani 1 1 d . . . H22A H 1.0042 0.6686 0.5326 0.070 Uiso 1 1 calc R . . H22B H 0.9914 0.6289 0.5607 0.070 Uiso 1 1 calc R . . C22' C 0.8044(4) 0.66700(15) 0.8683(4) 0.0521(14) Uani 1 1 d . . . H22C H 0.8240 0.6637 0.9349 0.063 Uiso 1 1 calc R . . H22D H 0.7713 0.6889 0.8532 0.063 Uiso 1 1 calc R . . C23 C 0.8839(4) 0.65345(14) 0.4869(4) 0.0527(15) Uani 1 1 d . . . H23A H 0.8823 0.6410 0.4309 0.063 Uiso 1 1 calc R . . H23B H 0.8653 0.6781 0.4707 0.063 Uiso 1 1 calc R . . C23' C 0.7528(4) 0.63533(13) 0.8210(4) 0.0494(13) Uani 1 1 d . . . H23C H 0.7015 0.6348 0.8343 0.059 Uiso 1 1 calc R . . H23D H 0.7831 0.6131 0.8439 0.059 Uiso 1 1 calc R . . C31' C 0.3721(3) 0.86169(14) 0.5818(4) 0.0499(14) Uani 1 1 d . . . C31 C 0.3625(5) 0.83844(16) 0.3410(4) 0.0680(19) Uani 1 1 d . . . C32' C 0.3291(4) 0.84836(17) 0.6340(4) 0.0657(17) Uani 1 1 d . . . H32A H 0.2710 0.8463 0.5947 0.079 Uiso 1 1 calc R . . H32B H 0.3321 0.8659 0.6818 0.079 Uiso 1 1 calc R . . C32 C 0.2902(5) 0.82232(18) 0.3358(5) 0.088(3) Uani 1 1 d . . . H32C H 0.2416 0.8358 0.3227 0.105 Uiso 1 1 calc R . . C33' C 0.3546(5) 0.8150(2) 0.6771(5) 0.082(2) Uani 1 1 d . . . H33A H 0.3264 0.8053 0.7136 0.099 Uiso 1 1 calc R . . C33 C 0.2896(7) 0.7861(2) 0.3500(6) 0.111(4) Uani 1 1 d . . . H33B H 0.2402 0.7749 0.3475 0.133 Uiso 1 1 calc R . . C34' C 0.4176(5) 0.79671(18) 0.6675(5) 0.077(2) Uani 1 1 d . . . H34A H 0.4320 0.7742 0.6955 0.093 Uiso 1 1 calc R . . C34 C 0.3597(9) 0.7660(2) 0.3677(6) 0.124(4) Uani 1 1 d . . . H34B H 0.3577 0.7411 0.3751 0.149 Uiso 1 1 calc R . . C35' C 0.4603(4) 0.81060(15) 0.6176(4) 0.0654(18) Uani 1 1 d . . . H35A H 0.5059 0.7983 0.6125 0.078 Uiso 1 1 calc R . . C35 C 0.4309(8) 0.7816(2) 0.3745(6) 0.125(5) Uani 1 1 d . . . H35B H 0.4794 0.7680 0.3881 0.150 Uiso 1 1 calc R . . C36' C 0.4367(4) 0.84282(14) 0.5743(4) 0.0508(14) Uani 1 1 d . . . H36A H 0.4659 0.8521 0.5385 0.061 Uiso 1 1 calc R . . C36 C 0.4329(5) 0.81756(16) 0.3615(4) 0.082(2) Uani 1 1 d . . . H36B H 0.4833 0.8285 0.3666 0.099 Uiso 1 1 calc R . . C41 C 0.2715(3) 0.89856(14) 0.2432(3) 0.0453(12) Uani 1 1 d . . . C41' C 0.2346(3) 0.90508(16) 0.4684(4) 0.0533(14) Uani 1 1 d . . . C42 C 0.2334(3) 0.87706(14) 0.1675(3) 0.0450(12) Uani 1 1 d . . . H42A H 0.2568 0.8550 0.1605 0.054 Uiso 1 1 calc R . . C42' C 0.1872(4) 0.8744(2) 0.4483(4) 0.0711(19) Uani 1 1 d . . . H42B H 0.2129 0.8521 0.4669 0.085 Uiso 1 1 calc R . . C43 C 0.1611(3) 0.88851(15) 0.1030(4) 0.0496(13) Uani 1 1 d . . . H43A H 0.1358 0.8746 0.0503 0.060 Uiso 1 1 calc R . . C43' C 0.1073(5) 0.8754(3) 0.4040(5) 0.085(2) Uani 1 1 d . . . H43B H 0.0772 0.8539 0.3898 0.102 Uiso 1 1 calc R . . C44 C 0.1249(3) 0.91987(14) 0.1138(4) 0.0510(14) Uani 1 1 d . . . H44A H 0.0751 0.9273 0.0689 0.061 Uiso 1 1 calc R . . C44' C 0.0671(4) 0.9073(3) 0.3782(4) 0.090(3) Uani 1 1 d . . . H44B H 0.0096 0.9078 0.3483 0.108 Uiso 1 1 calc R . . C45 C 0.1611(3) 0.94049(14) 0.1900(4) 0.0488(13) Uani 1 1 d . . . H45A H 0.1355 0.9616 0.1990 0.059 Uiso 1 1 calc R . . C45' C 0.1132(4) 0.9393(2) 0.3968(4) 0.076(2) Uani 1 1 d . . . H45B H 0.0869 0.9615 0.3794 0.091 Uiso 1 1 calc R . . C46 C 0.2354(3) 0.92996(13) 0.2531(3) 0.0451(12) Uani 1 1 d . . . H46A H 0.2618 0.9446 0.3039 0.054 Uiso 1 1 calc R . . C46' C 0.1949(3) 0.93742(19) 0.4399(4) 0.0576(15) Uani 1 1 d . . . H46B H 0.2262 0.9586 0.4511 0.069 Uiso 1 1 calc R . . C51 C 0.7154(4) 0.63240(13) 0.4481(3) 0.0491(14) Uani 1 1 d . . . C51' C 0.6496(3) 0.67148(15) 0.6613(4) 0.0514(14) Uani 1 1 d . . . C52 C 0.6585(4) 0.60612(14) 0.4407(4) 0.0508(14) Uani 1 1 d . . . H52A H 0.6736 0.5860 0.4790 0.061 Uiso 1 1 calc R . . C52' C 0.5917(5) 0.6769(3) 0.7042(6) 0.098(3) Uani 1 1 d . . . H52B H 0.5678 0.6535 0.7084 0.118 Uiso 1 1 calc R . . H52C H 0.6224 0.6845 0.7672 0.118 Uiso 1 1 calc R . . C53 C 0.5797(4) 0.60878(17) 0.3779(4) 0.0594(16) Uani 1 1 d . . . H53A H 0.5417 0.5902 0.3723 0.071 Uiso 1 1 calc R . . C53' C 0.5273(6) 0.7003(3) 0.6690(7) 0.118(4) Uani 1 1 d . . . H53B H 0.4896 0.7038 0.6995 0.142 Uiso 1 1 calc R . . C54 C 0.5566(5) 0.63807(18) 0.3243(4) 0.076(2) Uani 1 1 d . . . H54A H 0.5021 0.6402 0.2828 0.091 Uiso 1 1 calc R . . C54' C 0.5176(4) 0.7182(2) 0.5912(6) 0.080(2) Uani 1 1 d . . . H54B H 0.4729 0.7340 0.5669 0.096 Uiso 1 1 calc R . . C55 C 0.6128(5) 0.66482(18) 0.3305(4) 0.078(2) Uani 1 1 d . . . H55A H 0.5966 0.6850 0.2923 0.094 Uiso 1 1 calc R . . C55' C 0.5721(4) 0.7136(2) 0.5477(6) 0.079(2) Uani 1 1 d . . . H55B H 0.5657 0.7263 0.4934 0.095 Uiso 1 1 calc R . . C56 C 0.6926(4) 0.66250(16) 0.3918(4) 0.0647(17) Uani 1 1 d . . . H56A H 0.7309 0.6808 0.3956 0.078 Uiso 1 1 calc R . . C56' C 0.6370(4) 0.69037(17) 0.5830(5) 0.0653(17) Uani 1 1 d . . . H56B H 0.6742 0.6874 0.5517 0.078 Uiso 1 1 calc R . . C61 C 0.8510(4) 0.58543(13) 0.5366(3) 0.0462(13) Uani 1 1 d . . . C61' C 0.6745(4) 0.59693(16) 0.6596(4) 0.0578(16) Uani 1 1 d . . . C62 C 0.8321(4) 0.56608(14) 0.4572(4) 0.0552(15) Uani 1 1 d . . . H62A H 0.7963 0.5758 0.4018 0.066 Uiso 1 1 calc R . . C62' C 0.5906(4) 0.5955(2) 0.6060(5) 0.073(2) Uani 1 1 d . . . H62B H 0.5604 0.6168 0.5877 0.088 Uiso 1 1 calc R . . C63 C 0.8648(4) 0.53275(15) 0.4577(4) 0.0626(17) Uani 1 1 d . . . H63A H 0.8511 0.5195 0.4030 0.075 Uiso 1 1 calc R . . C63' C 0.5524(5) 0.5633(3) 0.5803(5) 0.085(2) Uani 1 1 d . . . H63B H 0.4966 0.5621 0.5421 0.102 Uiso 1 1 calc R . . C64 C 0.9172(4) 0.51877(14) 0.5378(4) 0.0580(16) Uani 1 1 d . . . H64A H 0.9415 0.4963 0.5376 0.070 Uiso 1 1 calc R . . C64' C 0.5972(7) 0.5328(2) 0.6113(6) 0.094(3) Uani 1 1 d . . . H64B H 0.5705 0.5105 0.5965 0.113 Uiso 1 1 calc R . . C65 C 0.9349(4) 0.53725(14) 0.6186(4) 0.0546(15) Uani 1 1 d . . . H65A H 0.9697 0.5272 0.6741 0.066 Uiso 1 1 calc R . . C65' C 0.6786(6) 0.5334(2) 0.6625(5) 0.080(2) Uani 1 1 d . . . H65B H 0.7079 0.5120 0.6819 0.096 Uiso 1 1 calc R . . C66 C 0.9009(3) 0.57071(13) 0.6175(4) 0.0465(13) Uani 1 1 d . . . H66A H 0.9121 0.5834 0.6726 0.056 Uiso 1 1 calc R . . C66' C 0.7183(5) 0.56606(16) 0.6861(4) 0.0669(18) Uani 1 1 d . . . H66B H 0.7751 0.5669 0.7203 0.080 Uiso 1 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 0.0414(2) 0.0272(2) 0.0325(2) -0.00256(14) 0.00421(16) 0.00095(15) Rh2 0.0564(3) 0.0248(2) 0.0323(2) 0.00525(14) 0.01746(18) 0.00666(16) Cl1 0.0933(13) 0.0761(12) 0.0772(12) 0.0012(9) 0.0349(10) 0.0071(10) Cl2 0.0385(6) 0.0242(5) 0.0328(6) 0.0004(4) 0.0076(5) 0.0034(4) S1 0.0476(7) 0.0366(6) 0.0329(6) 0.0023(5) 0.0095(5) 0.0104(5) S2 0.0392(6) 0.0274(6) 0.0320(6) -0.0010(5) 0.0061(5) 0.0007(5) S3 0.0559(8) 0.0361(7) 0.0563(8) 0.0140(6) 0.0209(7) 0.0120(6) S4 0.0641(8) 0.0281(6) 0.0344(6) 0.0041(5) 0.0138(6) 0.0062(6) P1 0.0529(8) 0.0331(7) 0.0389(7) -0.0076(5) -0.0001(6) 0.0058(6) P2 0.0430(7) 0.0354(7) 0.0378(7) 0.0015(5) 0.0047(6) -0.0059(6) P3 0.0674(9) 0.0280(6) 0.0337(7) 0.0058(5) 0.0210(6) 0.0137(6) P4 0.0650(9) 0.0329(7) 0.0362(7) -0.0009(5) 0.0230(6) -0.0055(6) O1' 0.043(2) 0.0272(19) 0.060(2) -0.0025(15) 0.0128(17) -0.0032(14) O1 0.057(3) 0.065(3) 0.101(4) 0.048(3) -0.001(2) -0.015(2) O2' 0.047(2) 0.042(2) 0.059(2) -0.0026(18) -0.0018(19) 0.0072(17) O2 0.040(3) 0.069(3) 0.281(9) 0.054(5) 0.047(4) 0.004(2) N1 0.043(2) 0.028(2) 0.030(2) 0.0034(15) 0.0087(17) -0.0041(17) N1' 0.037(2) 0.0232(19) 0.035(2) -0.0012(15) 0.0118(17) 0.0000(16) N2' 0.044(2) 0.033(2) 0.032(2) -0.0011(17) 0.0004(18) 0.0101(18) N2 0.042(2) 0.036(2) 0.063(3) 0.005(2) 0.017(2) 0.0009(19) N3' 0.045(2) 0.031(2) 0.029(2) -0.0058(16) 0.0109(17) 0.0003(17) N3 0.048(3) 0.040(2) 0.050(3) 0.0034(19) 0.027(2) -0.0038(19) C1 0.045(3) 0.034(3) 0.044(3) 0.001(2) 0.007(2) 0.000(2) C1' 0.050(3) 0.065(4) 0.052(3) -0.027(3) 0.000(3) 0.014(3) C2 0.047(3) 0.036(3) 0.040(3) -0.006(2) 0.014(2) 0.000(2) C2' 0.046(3) 0.069(4) 0.036(3) -0.009(3) 0.009(2) 0.007(3) C3' 0.040(3) 0.028(2) 0.025(2) -0.0048(18) 0.0060(19) -0.0017(19) C3 0.042(3) 0.028(2) 0.034(2) 0.0004(19) 0.006(2) 0.005(2) C4' 0.041(3) 0.021(2) 0.029(2) -0.0031(18) 0.009(2) -0.0030(19) C4 0.042(3) 0.027(2) 0.027(2) -0.0046(18) 0.007(2) -0.001(2) C5' 0.045(3) 0.019(2) 0.034(2) -0.0015(18) 0.010(2) 0.0008(19) C5 0.044(3) 0.026(2) 0.026(2) -0.0019(18) 0.007(2) -0.001(2) C6' 0.037(3) 0.029(2) 0.026(2) -0.0061(18) 0.0082(19) 0.0006(19) C6 0.052(3) 0.021(2) 0.027(2) -0.0035(18) 0.008(2) -0.003(2) C7' 0.042(3) 0.030(2) 0.034(2) -0.0030(19) 0.009(2) -0.007(2) C7 0.057(3) 0.030(3) 0.035(3) 0.001(2) 0.016(2) -0.007(2) C8' 0.042(3) 0.024(2) 0.033(2) 0.0004(18) 0.010(2) 0.0002(19) C8 0.052(3) 0.028(2) 0.036(3) 0.002(2) 0.012(2) 0.004(2) C9' 0.043(3) 0.033(3) 0.032(2) -0.006(2) 0.010(2) -0.003(2) C9 0.046(3) 0.042(3) 0.048(3) 0.013(2) 0.007(2) -0.014(2) C10' 0.042(3) 0.029(2) 0.033(2) -0.0066(19) 0.011(2) -0.001(2) C10 0.051(3) 0.041(3) 0.045(3) 0.004(2) 0.018(2) -0.012(2) C11' 0.054(3) 0.033(3) 0.050(3) -0.008(2) 0.023(3) -0.009(2) C11 0.054(3) 0.043(3) 0.047(3) 0.005(2) 0.017(3) -0.014(3) C12' 0.034(3) 0.053(3) 0.060(3) -0.011(3) 0.015(3) -0.010(2) C12 0.046(3) 0.059(4) 0.064(4) -0.005(3) 0.025(3) -0.019(3) C13' 0.042(3) 0.052(3) 0.052(3) -0.006(3) 0.016(3) 0.006(2) C13 0.047(3) 0.051(4) 0.091(5) 0.007(3) 0.034(3) -0.006(3) C14' 0.043(3) 0.034(3) 0.034(3) -0.006(2) 0.008(2) 0.002(2) C14 0.035(3) 0.051(3) 0.078(4) 0.009(3) 0.022(3) -0.002(2) C15' 0.047(3) 0.042(3) 0.035(3) -0.006(2) 0.011(2) 0.003(2) C15 0.040(3) 0.053(4) 0.120(6) 0.017(4) 0.029(4) 0.004(3) C16 0.044(3) 0.036(3) 0.058(3) 0.011(2) 0.022(3) 0.008(2) C19' 0.057(3) 0.029(3) 0.037(3) 0.001(2) 0.008(2) 0.006(2) C17 0.051(4) 0.068(5) 0.174(9) 0.038(5) -0.020(5) -0.010(4) C18' 0.053(3) 0.032(3) 0.051(3) 0.004(2) 0.004(3) -0.002(2) C18 0.057(4) 0.054(4) 0.156(8) 0.047(5) -0.016(5) 0.007(3) C19 0.050(3) 0.040(3) 0.052(3) 0.012(2) 0.015(3) 0.004(2) C17' 0.054(3) 0.031(3) 0.049(3) 0.011(2) 0.003(3) 0.007(2) C16' 0.047(3) 0.031(3) 0.032(2) -0.002(2) 0.006(2) 0.008(2) C20 0.048(3) 0.031(3) 0.075(4) -0.002(3) 0.017(3) 0.006(2) C20' 0.068(4) 0.035(3) 0.075(4) 0.005(3) -0.012(3) 0.012(3) C21 0.048(3) 0.033(3) 0.064(4) 0.001(2) 0.010(3) 0.008(2) C21' 0.061(4) 0.034(3) 0.097(5) 0.010(3) -0.024(4) 0.009(3) C22 0.076(4) 0.040(3) 0.074(4) 0.010(3) 0.046(4) 0.016(3) C22' 0.080(4) 0.045(3) 0.035(3) 0.000(2) 0.024(3) 0.008(3) C23 0.088(4) 0.033(3) 0.049(3) 0.012(2) 0.039(3) 0.013(3) C23' 0.077(4) 0.034(3) 0.046(3) 0.003(2) 0.032(3) -0.003(3) C31' 0.056(3) 0.036(3) 0.041(3) 0.005(2) -0.003(3) -0.010(3) C31 0.098(5) 0.041(3) 0.038(3) -0.009(3) -0.010(3) 0.008(3) C32' 0.080(4) 0.063(4) 0.048(3) 0.008(3) 0.015(3) -0.014(3) C32 0.103(6) 0.048(4) 0.079(5) 0.011(3) -0.010(4) -0.025(4) C33' 0.105(6) 0.068(5) 0.071(5) 0.017(4) 0.027(4) -0.022(4) C33 0.156(9) 0.052(5) 0.076(5) 0.007(4) -0.020(5) -0.032(5) C34' 0.107(6) 0.041(4) 0.064(4) 0.009(3) 0.006(4) 0.003(4) C34 0.193(11) 0.043(5) 0.073(5) 0.003(4) -0.032(6) 0.000(6) C35' 0.081(4) 0.038(3) 0.055(4) 0.003(3) -0.004(3) 0.005(3) C35 0.186(11) 0.052(5) 0.074(5) -0.020(4) -0.032(6) 0.039(6) C36' 0.058(4) 0.042(3) 0.038(3) 0.001(2) -0.001(3) -0.005(3) C36 0.115(6) 0.038(3) 0.056(4) -0.008(3) -0.017(4) 0.021(4) C41 0.049(3) 0.040(3) 0.041(3) -0.006(2) 0.008(2) -0.001(2) C41' 0.051(3) 0.064(4) 0.036(3) 0.009(3) 0.004(2) -0.017(3) C42 0.048(3) 0.037(3) 0.043(3) -0.005(2) 0.008(2) -0.008(2) C42' 0.064(4) 0.081(5) 0.057(4) 0.006(3) 0.006(3) -0.035(4) C43 0.054(3) 0.050(3) 0.038(3) -0.012(2) 0.008(3) -0.007(3) C43' 0.059(4) 0.118(7) 0.063(4) 0.002(4) 0.003(4) -0.039(5) C44 0.051(3) 0.048(3) 0.040(3) -0.002(2) -0.002(2) 0.000(3) C44' 0.043(4) 0.184(10) 0.040(4) -0.003(5) 0.009(3) -0.038(5) C45 0.054(3) 0.038(3) 0.047(3) -0.003(2) 0.009(3) 0.002(2) C45' 0.059(4) 0.126(7) 0.043(3) 0.024(4) 0.020(3) 0.023(4) C46 0.053(3) 0.033(3) 0.038(3) -0.006(2) 0.002(2) -0.002(2) C46' 0.047(3) 0.080(4) 0.041(3) 0.009(3) 0.009(3) -0.007(3) C51 0.080(4) 0.034(3) 0.032(3) -0.001(2) 0.018(3) 0.022(3) C51' 0.054(3) 0.055(3) 0.050(3) -0.008(3) 0.024(3) -0.013(3) C52 0.074(4) 0.039(3) 0.043(3) 0.005(2) 0.026(3) 0.010(3) C52' 0.081(5) 0.147(8) 0.085(5) 0.028(5) 0.052(5) 0.022(5) C53 0.073(4) 0.057(4) 0.039(3) -0.006(3) 0.008(3) 0.013(3) C53' 0.094(6) 0.184(10) 0.102(7) 0.028(7) 0.066(6) 0.058(7) C54 0.100(5) 0.055(4) 0.050(4) -0.012(3) -0.002(4) 0.020(4) C54' 0.064(4) 0.085(5) 0.093(6) 0.004(4) 0.030(4) 0.019(4) C55 0.107(6) 0.048(4) 0.051(4) 0.007(3) -0.007(4) 0.016(4) C55' 0.076(5) 0.068(5) 0.097(6) 0.025(4) 0.035(4) 0.017(4) C56 0.092(5) 0.040(3) 0.044(3) 0.004(3) 0.002(3) 0.010(3) C56' 0.077(4) 0.056(4) 0.073(4) 0.016(3) 0.039(4) 0.000(3) C61 0.073(4) 0.029(3) 0.040(3) 0.006(2) 0.024(3) 0.020(2) C61' 0.087(5) 0.052(4) 0.047(3) -0.006(3) 0.041(3) -0.013(3) C62 0.096(5) 0.036(3) 0.042(3) 0.006(2) 0.035(3) 0.014(3) C62' 0.077(5) 0.082(5) 0.076(5) -0.033(4) 0.045(4) -0.032(4) C63 0.106(5) 0.044(3) 0.050(3) 0.003(3) 0.043(3) 0.022(3) C63' 0.083(5) 0.109(7) 0.083(5) -0.038(5) 0.053(4) -0.029(5) C64 0.082(4) 0.030(3) 0.077(4) 0.010(3) 0.047(4) 0.019(3) C64' 0.141(8) 0.071(5) 0.099(6) -0.036(5) 0.077(6) -0.031(6) C65 0.066(4) 0.036(3) 0.062(4) 0.018(3) 0.023(3) 0.017(3) C65' 0.126(7) 0.066(5) 0.067(4) -0.025(4) 0.058(5) -0.039(4) C66 0.062(3) 0.033(3) 0.041(3) 0.006(2) 0.014(3) 0.010(2) C66' 0.114(6) 0.045(3) 0.056(4) -0.004(3) 0.048(4) -0.006(4) _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 P1 2.2404(14) . ? Rh1 P2 2.2402(15) . ? Rh1 S2 2.3558(12) . ? Rh1 S1 2.3636(14) . ? Rh2 P3 2.2453(14) . ? Rh2 P4 2.2474(16) . ? Rh2 S4 2.3414(14) . ? Rh2 S3 2.3624(16) . ? S1 C3 1.784(5) . ? S1 C2' 1.825(5) . ? S2 C3' 1.791(5) . ? S2 C2 1.839(5) . ? S3 C19 1.795(5) . ? S3 C22 1.830(6) . ? S4 C19' 1.772(5) . ? S4 C22' 1.824(6) . ? P1 C41 1.826(5) . ? P1 C31 1.828(6) . ? P1 C1' 1.853(7) . ? P2 C41' 1.826(6) . ? P2 C31' 1.827(5) . ? P2 C1 1.844(5) . ? P3 C51 1.829(6) . ? P3 C61 1.831(5) . ? P3 C23 1.835(6) . ? P4 C51' 1.797(6) . ? P4 C61' 1.834(6) . ? P4 C23' 1.843(5) . ? O1' C9' 1.218(6) . ? O1 C9 1.204(6) . ? O2' C15' 1.242(6) . ? O2 C15 1.207(7) . ? N1 C9 1.363(6) . ? N1 C6 1.419(6) . ? N1' C9' 1.359(6) . ? N1' C6' 1.404(6) . ? N2' C15' 1.331(7) . ? N2' C16' 1.405(6) . ? N2 C15 1.352(7) . ? N2 C16 1.412(6) . ? N3' C14' 1.346(6) . ? N3' C10' 1.354(6) . ? N3 C14 1.338(7) . ? N3 C10 1.345(6) . ? C1 C2 1.511(7) . ? C1' C2' 1.494(9) . ? C3' C4' 1.384(6) . ? C3' C8' 1.398(6) . ? C3 C8 1.377(7) . ? C3 C4 1.402(6) . ? C4' C5' 1.381(7) . ? C4 C5 1.362(7) . ? C5' C6' 1.387(6) . ? C5 C6 1.388(7) . ? C6' C7' 1.398(6) . ? C6 C7 1.405(7) . ? C7' C8' 1.400(7) . ? C7 C8 1.377(7) . ? C9' C10' 1.512(7) . ? C9 C10 1.488(8) . ? C10' C11' 1.368(7) . ? C10 C11 1.407(7) . ? C11' C12' 1.406(8) . ? C11 C12 1.386(8) . ? C12' C13' 1.386(8) . ? C12 C13 1.384(8) . ? C13' C14' 1.370(7) . ? C13 C14 1.386(8) . ? C14' C15' 1.500(7) . ? C14 C15 1.511(8) . ? C16 C21 1.346(7) . ? C16 C17 1.402(9) . ? C19' C20' 1.352(8) . ? C19' C18' 1.385(7) . ? C17 C18 1.398(10) . ? C18' C17' 1.388(7) . ? C18 C19 1.355(9) . ? C19 C20 1.359(7) . ? C17' C16' 1.368(7) . ? C16' C21' 1.406(7) . ? C20 C21 1.391(7) . ? C20' C21' 1.372(9) . ? C22 C23 1.501(9) . ? C22' C23' 1.526(8) . ? C31' C36' 1.375(8) . ? C31' C32' 1.388(9) . ? C31 C32 1.380(11) . ? C31 C36 1.401(10) . ? C32' C33' 1.427(10) . ? C32 C33 1.389(10) . ? C33' C34' 1.352(11) . ? C33 C34 1.386(15) . ? C34' C35' 1.364(11) . ? C34 C35 1.348(16) . ? C35' C36' 1.385(8) . ? C35 C36 1.375(11) . ? C41 C46 1.379(7) . ? C41 C42 1.402(7) . ? C41' C42' 1.398(8) . ? C41' C46' 1.400(9) . ? C42 C43 1.383(7) . ? C42' C43' 1.325(10) . ? C43 C44 1.382(8) . ? C43' C44' 1.382(12) . ? C44 C45 1.382(7) . ? C44' C45' 1.428(12) . ? C45 C46 1.387(7) . ? C45' C46' 1.351(9) . ? C51 C52 1.381(8) . ? C51 C56 1.411(8) . ? C51' C56' 1.373(8) . ? C51' C52' 1.413(9) . ? C52 C53 1.390(8) . ? C52' C53' 1.386(11) . ? C53 C54 1.364(9) . ? C53' C54' 1.356(12) . ? C54 C55 1.390(11) . ? C54' C55' 1.364(10) . ? C55 C56 1.392(9) . ? C55' C56' 1.388(9) . ? C61 C66 1.381(7) . ? C61 C62 1.384(7) . ? C61' C66' 1.377(9) . ? C61' C62' 1.414(9) . ? C62 C63 1.383(8) . ? C62' C63' 1.378(10) . ? C63 C64 1.376(9) . ? C63' C64' 1.385(12) . ? C64 C65 1.387(9) . ? C64' C65' 1.367(12) . ? C65 C66 1.395(7) . ? C65' C66' 1.400(9) . ? 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 P1 Rh1 P2 96.40(6) . . ? P1 Rh1 S2 176.78(5) . . ? P2 Rh1 S2 85.58(5) . . ? P1 Rh1 S1 85.77(6) . . ? P2 Rh1 S1 168.80(5) . . ? S2 Rh1 S1 92.77(5) . . ? P3 Rh2 P4 97.94(5) . . ? P3 Rh2 S4 171.00(5) . . ? P4 Rh2 S4 85.36(5) . . ? P3 Rh2 S3 85.48(5) . . ? P4 Rh2 S3 175.67(5) . . ? S4 Rh2 S3 90.87(5) . . ? C3 S1 C2' 101.8(2) . . ? C3 S1 Rh1 110.63(16) . . ? C2' S1 Rh1 104.8(2) . . ? C3' S2 C2 100.8(2) . . ? C3' S2 Rh1 112.52(15) . . ? C2 S2 Rh1 105.54(16) . . ? C19 S3 C22 100.5(3) . . ? C19 S3 Rh2 112.90(19) . . ? C22 S3 Rh2 105.5(2) . . ? C19' S4 C22' 102.5(3) . . ? C19' S4 Rh2 110.47(17) . . ? C22' S4 Rh2 107.31(19) . . ? C41 P1 C31 104.5(3) . . ? C41 P1 C1' 102.4(3) . . ? C31 P1 C1' 102.2(3) . . ? C41 P1 Rh1 117.45(17) . . ? C31 P1 Rh1 121.80(19) . . ? C1' P1 Rh1 105.77(19) . . ? C41' P2 C31' 107.1(3) . . ? C41' P2 C1 101.3(3) . . ? C31' P2 C1 103.5(2) . . ? C41' P2 Rh1 119.15(18) . . ? C31' P2 Rh1 116.2(2) . . ? C1 P2 Rh1 107.38(18) . . ? C51 P3 C61 104.7(2) . . ? C51 P3 C23 104.7(3) . . ? C61 P3 C23 99.8(3) . . ? C51 P3 Rh2 124.30(17) . . ? C61 P3 Rh2 113.76(17) . . ? C23 P3 Rh2 106.5(2) . . ? C51' P4 C61' 103.6(3) . . ? C51' P4 C23' 104.2(3) . . ? C61' P4 C23' 100.4(2) . . ? C51' P4 Rh2 114.65(18) . . ? C61' P4 Rh2 124.6(2) . . ? C23' P4 Rh2 106.8(2) . . ? C9 N1 C6 127.0(4) . . ? C9' N1' C6' 128.7(4) . . ? C15' N2' C16' 128.3(4) . . ? C15 N2 C16 128.3(5) . . ? C14' N3' C10' 116.6(4) . . ? C14 N3 C10 117.9(4) . . ? C2 C1 P2 109.2(4) . . ? C2' C1' P1 107.4(4) . . ? C1 C2 S2 108.3(3) . . ? C1' C2' S1 111.6(4) . . ? C4' C3' C8' 120.4(4) . . ? C4' C3' S2 121.6(4) . . ? C8' C3' S2 118.0(3) . . ? C8 C3 C4 119.5(4) . . ? C8 C3 S1 119.2(4) . . ? C4 C3 S1 121.2(4) . . ? C5' C4' C3' 119.4(4) . . ? C5 C4 C3 120.1(4) . . ? C4' C5' C6' 121.4(4) . . ? C4 C5 C6 120.4(4) . . ? C5' C6' C7' 119.5(4) . . ? C5' C6' N1' 117.0(4) . . ? C7' C6' N1' 123.5(4) . . ? C5 C6 C7 119.9(5) . . ? C5 C6 N1 116.8(4) . . ? C7 C6 N1 123.2(4) . . ? C6' C7' C8' 119.4(4) . . ? C8 C7 C6 118.9(5) . . ? C3' C8' C7' 119.9(4) . . ? C7 C8 C3 121.2(4) . . ? O1' C9' N1' 125.7(4) . . ? O1' C9' C10' 120.9(4) . . ? N1' C9' C10' 113.3(4) . . ? O1 C9 N1 124.0(5) . . ? O1 C9 C10 121.0(5) . . ? N1 C9 C10 115.0(4) . . ? N3' C10' C11' 123.3(4) . . ? N3' C10' C9' 116.7(4) . . ? C11' C10' C9' 119.9(4) . . ? N3 C10 C11 123.0(5) . . ? N3 C10 C9 119.8(4) . . ? C11 C10 C9 117.2(5) . . ? C10' C11' C12' 119.4(5) . . ? C12 C11 C10 117.6(5) . . ? C13' C12' C11' 117.4(5) . . ? C13 C12 C11 119.7(5) . . ? C14' C13' C12' 119.5(5) . . ? C14 C13 C12 118.7(6) . . ? N3' C14' C13' 123.7(5) . . ? N3' C14' C15' 116.5(4) . . ? C13' C14' C15' 119.8(5) . . ? N3 C14 C13 123.1(5) . . ? N3 C14 C15 118.3(5) . . ? C13 C14 C15 118.6(5) . . ? O2' C15' N2' 124.7(5) . . ? O2' C15' C14' 119.4(5) . . ? N2' C15' C14' 115.9(4) . . ? O2 C15 N2 124.8(6) . . ? O2 C15 C14 120.8(6) . . ? N2 C15 C14 114.4(5) . . ? C21 C16 C17 118.2(5) . . ? C21 C16 N2 119.1(5) . . ? C17 C16 N2 122.7(5) . . ? C20' C19' C18' 118.0(5) . . ? C20' C19' S4 119.5(4) . . ? C18' C19' S4 122.5(4) . . ? C18 C17 C16 118.6(6) . . ? C19' C18' C17' 120.6(5) . . ? C19 C18 C17 122.0(6) . . ? C18 C19 C20 119.1(5) . . ? C18 C19 S3 117.6(4) . . ? C20 C19 S3 123.3(4) . . ? C16' C17' C18' 120.9(5) . . ? C17' C16' N2' 118.4(4) . . ? C17' C16' C21' 118.0(5) . . ? N2' C16' C21' 123.6(5) . . ? C19 C20 C21 119.7(5) . . ? C19' C20' C21' 122.3(5) . . ? C16 C21 C20 122.5(5) . . ? C20' C21' C16' 119.8(6) . . ? C23 C22 S3 112.1(4) . . ? C23' C22' S4 108.4(4) . . ? C22 C23 P3 108.7(4) . . ? C22' C23' P4 109.6(3) . . ? C36' C31' C32' 119.6(5) . . ? C36' C31' P2 119.1(4) . . ? C32' C31' P2 121.3(5) . . ? C32 C31 C36 118.5(7) . . ? C32 C31 P1 122.2(6) . . ? C36 C31 P1 119.3(6) . . ? C31' C32' C33' 117.3(7) . . ? C31 C32 C33 119.0(9) . . ? C34' C33' C32' 122.0(7) . . ? C34 C33 C32 121.1(10) . . ? C33' C34' C35' 119.9(6) . . ? C35 C34 C33 120.2(8) . . ? C34' C35' C36' 119.5(7) . . ? C34 C35 C36 119.5(10) . . ? C31' C36' C35' 121.7(6) . . ? C35 C36 C31 121.7(10) . . ? C46 C41 C42 119.6(5) . . ? C46 C41 P1 119.6(4) . . ? C42 C41 P1 120.7(4) . . ? C42' C41' C46' 117.7(6) . . ? C42' C41' P2 122.7(5) . . ? C46' C41' P2 119.5(4) . . ? C43 C42 C41 118.7(5) . . ? C43' C42' C41' 121.9(8) . . ? C44 C43 C42 121.2(5) . . ? C42' C43' C44' 120.8(8) . . ? C43 C44 C45 119.9(5) . . ? C43' C44' C45' 119.3(6) . . ? C44 C45 C46 119.2(5) . . ? C46' C45' C44' 118.6(8) . . ? C41 C46 C45 121.2(5) . . ? C45' C46' C41' 121.7(7) . . ? C52 C51 C56 119.4(6) . . ? C52 C51 P3 121.3(4) . . ? C56 C51 P3 119.0(5) . . ? C56' C51' C52' 115.9(6) . . ? C56' C51' P4 120.3(5) . . ? C52' C51' P4 123.5(5) . . ? C51 C52 C53 120.9(5) . . ? C53' C52' C51' 121.2(7) . . ? C54 C53 C52 120.1(7) . . ? C54' C53' C52' 120.4(7) . . ? C53 C54 C55 119.9(7) . . ? C53' C54' C55' 120.0(7) . . ? C54 C55 C56 121.0(6) . . ? C54' C55' C56' 119.8(7) . . ? C55 C56 C51 118.6(6) . . ? C51' C56' C55' 122.7(6) . . ? C66 C61 C62 119.4(5) . . ? C66 C61 P3 118.7(4) . . ? C62 C61 P3 121.8(4) . . ? C66' C61' C62' 119.9(6) . . ? C66' C61' P4 117.5(5) . . ? C62' C61' P4 122.6(5) . . ? C63 C62 C61 120.6(5) . . ? C63' C62' C61' 120.2(8) . . ? C64 C63 C62 119.8(5) . . ? C62' C63' C64' 118.4(8) . . ? C63 C64 C65 120.5(5) . . ? C65' C64' C63' 122.4(8) . . ? C64 C65 C66 119.2(5) . . ? C64' C65' C66' 119.3(8) . . ? C61 C66 C65 120.4(5) . . ? C61' C66' C65' 119.7(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.822 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.102