# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_fjl151d #TrackingRef '19531_web_deposit_cif_file_0_RamonMacias_1366120078.compound_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H32.50 B9 N2 P Rh S' _chemical_formula_sum 'C23 H32.50 B9 N2 P Rh S' _chemical_formula_weight 600.24 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 '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' S S 0.1246 0.1234 '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 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.565(5) _cell_length_b 18.761(7) _cell_length_c 13.508(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.7160(10) _cell_angle_gamma 90.00 _cell_volume 2818.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3698 _cell_measurement_theta_min 2.762 _cell_measurement_theta_max 25.515 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.236 _exptl_crystal_size_mid 0.185 _exptl_crystal_size_min 0.124 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1222 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8259 _exptl_absorpt_correction_T_max 0.9711 _exptl_absorpt_process_details ; Multi-scan correction included in APEX2 package (Bruker AXS, 2008) ; _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 'Bruker APEX system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 29436 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6787 _reflns_number_gt 4524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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. The structure was solved by Patterson method and anisotropic refinement of all non hydrogen atoms was applied. Hydrogen atoms were included in all cases in calculated positions and refined with a riding model. The asymmetric unit contains a rhodathiaborane molecule. A static disorder has been observed in the borane and one phosphines group. It has been modeled with two sets of positions with equal complementary occupancy factors. Residual electron density peaks are observed around the metal atom and they have no chemical sense. ; _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^)+(0.0270P)^2^+3.7004P] 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 ? _refine_ls_number_reflns 6787 _refine_ls_number_parameters 460 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl151d_0m in P2(1)/c CELL 0.71073 12.5649 18.7607 13.5078 90.000 117.716 90.000 ZERR 4.00 0.0047 0.0070 0.0050 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B N P RH S UNIT 92 130 36 8 4 4 4 MERG 2 OMIT -5 20 6 OMIT -15 2 10 OMIT -14 9 13 OMIT -13 11 12 OMIT -12 4 10 OMIT -10 12 14 OMIT -3 6 8 OMIT 8 16 0 OMIT 11 14 1 OMIT -11 4 11 OMIT 1 17 2 OMIT -13 5 10 OMIT -14 6 7 OMIT -11 15 1 OMIT -10 4 9 OMIT 10 2 4 SHEL 1000 0.7569 FREE B1 S7B FREE H B9B FREE H H10B SIMU C1 C2 C2 C3 SIMU C6 C5 C5 C4 DFIX 1.800 0.020 B10 B11 FMAP 2 PLAN 30 ACTA L.S. 6 TEMP -173.00 WGHT 0.027000 3.700400 FVAR 0.10060 MOLE 1 PART 4 RH8 6 0.102749 0.119025 0.257064 11.00000 0.03946 0.03093 = 0.02596 -0.00729 -0.00426 0.00841 N1 4 0.140104 0.063946 0.485694 11.00000 0.05493 0.05154 = 0.05183 0.00379 0.02086 -0.02310 N2 4 0.148307 -0.020044 0.380880 11.00000 0.03302 0.03359 = 0.06727 0.00328 -0.00315 -0.00798 S7 7 0.083302 0.205196 0.106119 10.50000 0.02900 0.02790 = 0.03054 0.00528 0.01117 0.00148 B1 3 -0.133092 0.102875 -0.002364 10.50000 0.02532 0.03149 = 0.02988 0.00043 0.00486 0.00323 AFIX 153 H101 2 -0.179707 0.063711 -0.071953 10.50000 -1.20000 AFIX 0 B2 3 -0.063145 0.176770 -0.029894 10.50000 0.02526 0.03830 = 0.03278 0.00278 0.00476 0.00106 AFIX 153 H102 2 -0.066319 0.185216 -0.113307 10.50000 -1.20000 AFIX 0 B3 3 0.022258 0.103182 0.067419 10.50000 0.03158 0.02775 = 0.02839 0.00337 0.00749 -0.00187 AFIX 153 H103 2 0.077104 0.065796 0.044897 10.50000 -1.20000 AFIX 0 B4 3 -0.063426 0.072838 0.139416 10.50000 0.02691 0.01770 = 0.02442 -0.00554 0.00830 -0.00142 AFIX 153 H104 2 -0.065318 0.015109 0.159664 10.50000 -1.20000 AFIX 0 B5 3 -0.193254 0.125644 0.088550 10.50000 0.03027 0.04987 = 0.04167 -0.01284 0.01283 0.00705 AFIX 153 H105 2 -0.280999 0.102637 0.075750 10.50000 -1.20000 AFIX 0 B6 3 -0.187971 0.191758 -0.003297 10.50000 0.03309 0.04466 = 0.03814 0.01022 0.00928 0.01370 AFIX 153 H106 2 -0.271644 0.213871 -0.073909 10.50000 -1.20000 AFIX 0 B9 3 -0.076285 0.138794 0.226484 10.50000 0.03329 AFIX 153 H109 2 -0.067215 0.145837 0.312405 10.50000 -1.20000 AFIX 0 B10 3 -0.155555 0.213909 0.132758 10.50000 0.04016 0.03979 = 0.03874 -0.01344 0.02221 0.01631 AFIX 153 H110 2 -0.180597 0.255977 0.177023 10.50000 -1.20000 AFIX 0 B11 3 -0.068713 0.249194 0.066750 10.50000 0.02661 0.03434 = 0.04874 -0.01990 -0.00681 0.00199 PART 3 S7B 7 0.043124 0.185340 0.101205 10.50000 0.03251 0.03545 = 0.02532 0.00823 0.01176 0.01132 B1B 3 -0.175710 0.087179 0.035794 10.50000 0.03445 0.03625 = 0.03861 -0.00937 -0.00209 0.00313 AFIX 153 H1B 2 -0.232038 0.045151 -0.024853 10.50000 -1.20000 AFIX 0 B2B 3 -0.116921 0.153970 -0.015989 10.50000 0.03620 0.04728 = 0.01765 -0.00165 -0.00361 0.02050 AFIX 153 H2B 2 -0.135058 0.154314 -0.105394 10.50000 -1.20000 AFIX 0 B4B 3 -0.087549 0.064866 0.179755 10.50000 0.02988 0.03407 = 0.02865 -0.00448 0.00165 0.00021 AFIX 153 H4B 2 -0.050193 0.016160 0.232692 10.50000 -1.20000 AFIX 0 B3B 3 -0.022233 0.083388 0.088111 10.50000 0.03167 0.02325 = 0.02630 -0.01025 -0.00218 0.01209 AFIX 153 H3B 2 0.050089 0.043699 0.102387 10.50000 -1.20000 AFIX 0 B5B 3 -0.210908 0.122892 0.138848 10.50000 0.03187 0.04338 = 0.04617 -0.01597 0.00986 0.00012 AFIX 153 H5B 2 -0.293830 0.106159 0.143865 10.50000 -1.20000 AFIX 0 B6B 3 -0.222757 0.178133 0.028808 10.50000 0.03010 0.03326 = 0.03266 0.00020 0.00322 0.01968 AFIX 153 H6B 2 -0.313235 0.197970 -0.034098 10.50000 -1.20000 AFIX 0 B9B 3 -0.073110 0.138876 0.263921 10.50000 0.03972 0.04909 = 0.03072 -0.01843 0.00299 -0.00385 B11B 3 -0.106460 0.233974 0.059112 10.50000 0.02529 0.03123 = 0.04760 -0.01435 -0.01077 0.00924 AFIX 153 H111 2 -0.093400 0.292191 0.049882 10.50000 -1.20000 AFIX 0 B10B 3 -0.161638 0.213447 0.167878 10.50000 0.03640 0.04034 = 0.03912 -0.02484 0.01669 -0.00128 PART 0 P1 5 0.297356 0.169244 0.350940 11.00000 0.04455 0.02910 = 0.02324 0.00498 0.01369 0.00299 C22 1 0.152201 -0.058953 0.289619 11.00000 0.05226 0.03947 = 0.07988 -0.01154 -0.01206 0.01159 AFIX 33 H22A 2 0.090989 -0.096521 0.263749 11.00000 -1.50000 H22B 2 0.231860 -0.080440 0.315709 11.00000 -1.50000 H22C 2 0.136380 -0.026144 0.227844 11.00000 -1.50000 AFIX 0 C23 1 0.138375 0.133809 0.531080 11.00000 0.09336 0.06379 = 0.06327 -0.01172 0.04785 -0.03005 AFIX 33 H23A 2 0.220939 0.151184 0.574469 11.00000 -1.50000 H23B 2 0.100120 0.130443 0.579717 11.00000 -1.50000 H23C 2 0.092898 0.166973 0.469697 11.00000 -1.50000 AFIX 0 C20 1 0.165877 -0.050351 0.481536 11.00000 0.05339 0.05102 = 0.09462 0.02711 0.00915 -0.02325 AFIX 43 H20 2 0.178816 -0.099454 0.500612 11.00000 -1.20000 AFIX 0 C21 1 0.161270 0.001938 0.546262 11.00000 0.08125 0.06591 = 0.08296 0.02537 0.03231 -0.03044 AFIX 43 H21 2 0.170770 -0.002733 0.619964 11.00000 -1.20000 AFIX 0 C1 1 0.289970 0.266554 0.346314 11.00000 0.06353 0.03091 = 0.02855 0.00422 0.02482 -0.00123 C2 1 0.368419 0.309508 0.326663 11.00000 0.10283 0.03872 = 0.06486 0.00724 0.06438 -0.00049 AFIX 43 H2 2 0.429272 0.288577 0.313113 11.00000 -1.20000 AFIX 0 C3 1 0.357314 0.383244 0.326952 11.00000 0.13673 0.04017 = 0.07709 -0.00089 0.08356 -0.01874 AFIX 43 H3 2 0.410626 0.412663 0.313280 11.00000 -1.20000 AFIX 0 C4 1 0.269717 0.413851 0.346889 11.00000 0.12598 0.02984 = 0.04988 -0.00674 0.05982 -0.01033 AFIX 43 H4 2 0.262481 0.464264 0.346622 11.00000 -1.20000 AFIX 0 C5 1 0.192270 0.371485 0.367292 11.00000 0.07959 0.03225 = 0.05100 -0.00410 0.03822 -0.00079 AFIX 43 H5 2 0.132376 0.392632 0.382014 11.00000 -1.20000 AFIX 0 C6 1 0.202244 0.297903 0.366213 11.00000 0.05613 0.02908 = 0.04835 0.00070 0.02736 -0.00267 AFIX 43 H6 2 0.148213 0.268762 0.379288 11.00000 -1.20000 AFIX 0 C7 1 0.399453 0.148628 0.496701 11.00000 0.02803 0.03563 = 0.02505 0.00158 0.00954 -0.00831 C8 1 0.464905 0.200320 0.574516 11.00000 0.03104 0.04060 = 0.03927 -0.00401 0.01359 -0.01049 AFIX 43 H8 2 0.453111 0.249341 0.554702 11.00000 -1.20000 AFIX 0 C9 1 0.547829 0.179901 0.681633 11.00000 0.02675 0.06691 = 0.04079 -0.01873 0.00446 -0.00371 AFIX 43 H9 2 0.593585 0.215119 0.735104 11.00000 -1.20000 AFIX 0 C10 1 0.564248 0.109223 0.710917 11.00000 0.03460 0.08190 = 0.02881 -0.00218 -0.00254 0.01264 AFIX 43 H10 2 0.621189 0.095838 0.784562 11.00000 -1.20000 AFIX 0 C11 1 0.498413 0.057252 0.633896 11.00000 0.03425 0.05092 = 0.03122 0.00911 0.00722 0.00073 AFIX 43 H11 2 0.508916 0.008380 0.654687 11.00000 -1.20000 AFIX 0 C12 1 0.417751 0.077096 0.527102 11.00000 0.02838 0.03893 = 0.02476 0.00350 0.00371 -0.00893 AFIX 43 H12 2 0.373956 0.041553 0.473387 11.00000 -1.20000 AFIX 0 C19 1 0.132486 0.051166 0.382890 11.00000 0.02775 0.03090 = 0.05249 -0.00217 0.00140 -0.00895 PART 1 AFIX 66 C18A 1 0.363534 0.110908 0.194193 10.50000 0.02781 0.04820 = 0.01724 0.00748 0.00381 0.01711 AFIX 43 H18A 2 0.280736 0.098750 0.154849 10.50000 -1.20000 AFIX 65 C13A 1 0.407652 0.147274 0.295244 10.50000 0.03119 0.02435 = 0.02781 0.00162 0.00966 -0.01213 C14A 1 0.528799 0.165061 0.352809 10.50000 0.03702 0.03530 = 0.03249 0.00305 0.01659 -0.00441 AFIX 43 H14A 2 0.558951 0.189916 0.421873 10.50000 -1.20000 AFIX 65 C15A 1 0.605828 0.146483 0.309324 10.50000 0.03500 0.06385 = 0.04848 0.02621 0.00781 0.00041 AFIX 43 H15A 2 0.688627 0.158640 0.348668 10.50000 -1.20000 AFIX 65 C16A 1 0.561712 0.110117 0.208274 10.50000 0.04681 0.07684 = 0.05289 0.03965 0.03684 0.02168 AFIX 43 H16A 2 0.614358 0.097419 0.178554 10.50000 -1.20000 AFIX 65 C17A 1 0.440565 0.092329 0.150707 10.50000 0.04190 0.07913 = 0.02446 0.01986 0.01153 0.04061 AFIX 43 H17A 2 0.410413 0.067474 0.081644 10.50000 -1.20000 PART 2 AFIX 66 C13B 1 0.370614 0.133362 0.272743 10.50000 0.02614 0.03268 = 0.02690 0.01261 0.00722 -0.00322 C18B 1 0.311290 0.089391 0.180198 10.50000 0.02903 0.03677 = 0.02911 0.01117 0.00639 0.00309 AFIX 43 H18B 2 0.228834 0.078191 0.154220 10.50000 -1.20000 AFIX 65 C17B 1 0.372610 0.061807 0.125661 10.50000 0.03569 0.03827 = 0.03037 0.00440 0.01091 -0.00130 AFIX 43 H17B 2 0.332064 0.031755 0.062410 10.50000 -1.20000 AFIX 65 C16B 1 0.493254 0.078194 0.163669 10.50000 0.03405 0.03114 = 0.03865 0.01073 0.02267 0.00614 AFIX 43 H16B 2 0.535163 0.059342 0.126395 10.50000 -1.20000 AFIX 65 C15B 1 0.552580 0.122165 0.256214 10.50000 0.04274 0.04543 = 0.03129 0.01674 0.01749 0.00422 AFIX 43 H15B 2 0.635035 0.133365 0.282191 10.50000 -1.20000 AFIX 65 C14B 1 0.491261 0.149750 0.310752 10.50000 0.05537 0.02951 = 0.02605 -0.00408 0.01385 -0.02088 AFIX 43 H14B 2 0.531808 0.179802 0.374003 10.50000 -1.20000 AFIX 0 PART 4 H 2 -0.054156 0.208982 0.227623 11.00000 10.03812 PART 3 H9B 2 -0.087149 0.134235 0.332984 10.50000 0.04054 H10B 2 -0.225322 0.250000 0.167950 10.50000 0.02608 HKLF 4 REM fjl151d_0m in P2(1)/c REM R1 = 0.0488 for 4524 Fo > 4sig(Fo) and 0.0888 for all 6787 data REM 460 parameters refined using 25 restraints END ; 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 Rh8 Rh 0.10275(3) 0.119025(16) 0.25706(2) 0.03982(10) Uani 1 1 d . A 4 N1 N 0.1401(3) 0.06395(19) 0.4857(3) 0.0543(10) Uani 1 1 d . A 4 N2 N 0.1483(3) -0.02004(18) 0.3809(3) 0.0551(10) Uani 1 1 d . A 4 S7 S 0.0833(3) 0.20520(15) 0.1061(3) 0.0302(6) Uani 0.50 1 d P A 4 B1 B -0.1331(8) 0.1029(5) -0.0024(8) 0.032(2) Uani 0.50 1 d P A 4 H101 H -0.1797 0.0637 -0.0720 0.038 Uiso 0.50 1 calc PR A 4 B2 B -0.0631(9) 0.1768(5) -0.0299(8) 0.036(2) Uani 0.50 1 d P A 4 H102 H -0.0663 0.1852 -0.1133 0.043 Uiso 0.50 1 calc PR A 4 B3 B 0.0223(9) 0.1032(5) 0.0674(8) 0.032(2) Uani 0.50 1 d P A 4 H103 H 0.0771 0.0658 0.0449 0.038 Uiso 0.50 1 calc PR A 4 B4 B -0.0634(9) 0.0728(5) 0.1394(9) 0.024(2) Uani 0.50 1 d P A 4 H104 H -0.0653 0.0151 0.1597 0.029 Uiso 0.50 1 calc PR A 4 B5 B -0.1933(9) 0.1256(6) 0.0885(10) 0.042(3) Uani 0.50 1 d P A 4 H105 H -0.2810 0.1026 0.0758 0.051 Uiso 0.50 1 calc PR A 4 B6 B -0.1880(11) 0.1918(6) -0.0033(10) 0.042(3) Uani 0.50 1 d P A 4 H106 H -0.2716 0.2139 -0.0739 0.050 Uiso 0.50 1 calc PR A 4 B9 B -0.0763(12) 0.1388(7) 0.2265(10) 0.033(3) Uiso 0.50 1 d P A 4 H109 H -0.0672 0.1458 0.3124 0.040 Uiso 0.50 1 calc PR A 4 B10 B -0.156(2) 0.2139(12) 0.1328(14) 0.038(4) Uani 0.50 1 d PD A 4 H110 H -0.1806 0.2560 0.1770 0.046 Uiso 0.50 1 calc PR A 4 B11 B -0.0687(15) 0.2492(11) 0.0668(19) 0.046(4) Uani 0.50 1 d PD A 4 S7B S 0.0431(3) 0.18534(16) 0.1012(3) 0.0318(6) Uani 0.50 1 d P B 3 B1B B -0.1757(9) 0.0872(5) 0.0358(9) 0.044(2) Uani 0.50 1 d P B 3 H1B H -0.2320 0.0452 -0.0249 0.053 Uiso 0.50 1 calc PR B 3 B2B B -0.1169(10) 0.1540(6) -0.0160(7) 0.040(2) Uani 0.50 1 d P B 3 H2B H -0.1351 0.1543 -0.1054 0.048 Uiso 0.50 1 calc PR B 3 B4B B -0.0875(10) 0.0649(6) 0.1798(9) 0.036(2) Uani 0.50 1 d P B 3 H4B H -0.0502 0.0162 0.2327 0.043 Uiso 0.50 1 calc PR B 3 B3B B -0.0222(9) 0.0834(5) 0.0881(8) 0.033(2) Uani 0.50 1 d P B 3 H3B H 0.0501 0.0437 0.1024 0.040 Uiso 0.50 1 calc PR B 3 B5B B -0.2109(9) 0.1229(6) 0.1388(10) 0.044(2) Uani 0.50 1 d P B 3 H5B H -0.2938 0.1062 0.1439 0.053 Uiso 0.50 1 calc PR B 3 B6B B -0.2228(10) 0.1781(6) 0.0288(9) 0.037(2) Uani 0.50 1 d P B 3 H6B H -0.3132 0.1980 -0.0341 0.044 Uiso 0.50 1 calc PR B 3 B9B B -0.0731(11) 0.1389(7) 0.2639(11) 0.045(3) Uani 0.50 1 d P B 3 B11B B -0.1065(14) 0.2340(11) 0.0591(18) 0.046(4) Uani 0.50 1 d P B 3 H111 H -0.0934 0.2922 0.0499 0.055 Uiso 0.50 1 calc PR B 3 B10B B -0.162(2) 0.2134(12) 0.1679(15) 0.039(4) Uani 0.50 1 d P B 3 P1 P 0.29736(9) 0.16924(5) 0.35094(7) 0.0331(2) Uani 1 1 d . . . C22 C 0.1522(4) -0.0590(2) 0.2896(4) 0.0741(17) Uani 1 1 d . . . H22A H 0.0910 -0.0965 0.2637 0.111 Uiso 1 1 calc R A 4 H22B H 0.2319 -0.0804 0.3157 0.111 Uiso 1 1 calc R A 4 H22C H 0.1364 -0.0261 0.2278 0.111 Uiso 1 1 calc R A 4 C23 C 0.1384(5) 0.1338(2) 0.5311(4) 0.0690(15) Uani 1 1 d . . . H23A H 0.2209 0.1512 0.5745 0.103 Uiso 1 1 calc R A 4 H23B H 0.1001 0.1304 0.5797 0.103 Uiso 1 1 calc R A 4 H23C H 0.0929 0.1670 0.4697 0.103 Uiso 1 1 calc R A 4 C20 C 0.1659(4) -0.0504(3) 0.4815(5) 0.0763(17) Uani 1 1 d . . . H20 H 0.1788 -0.0995 0.5006 0.092 Uiso 1 1 calc R A 4 C21 C 0.1613(5) 0.0019(3) 0.5463(5) 0.0790(17) Uani 1 1 d . A . H21 H 0.1708 -0.0027 0.6200 0.095 Uiso 1 1 calc R C 4 C1 C 0.2900(4) 0.26655(19) 0.3463(3) 0.0396(9) Uani 1 1 d U A . C2 C 0.3684(5) 0.3095(2) 0.3267(4) 0.0588(13) Uani 1 1 d U . . H2 H 0.4293 0.2886 0.3131 0.071 Uiso 1 1 calc R A . C3 C 0.3573(5) 0.3832(2) 0.3270(4) 0.0713(16) Uani 1 1 d U A . H3 H 0.4106 0.4127 0.3133 0.086 Uiso 1 1 calc R . . C4 C 0.2697(5) 0.4139(2) 0.3469(4) 0.0611(14) Uani 1 1 d U . . H4 H 0.2625 0.4643 0.3466 0.073 Uiso 1 1 calc R A . C5 C 0.1923(4) 0.3715(2) 0.3673(3) 0.0512(11) Uani 1 1 d U A . H5 H 0.1324 0.3926 0.3820 0.061 Uiso 1 1 calc R . . C6 C 0.2022(4) 0.29790(19) 0.3662(3) 0.0433(10) Uani 1 1 d U . . H6 H 0.1482 0.2688 0.3793 0.052 Uiso 1 1 calc R A . C7 C 0.3995(3) 0.14863(19) 0.4967(3) 0.0307(8) Uani 1 1 d . A . C8 C 0.4649(3) 0.2003(2) 0.5745(3) 0.0381(9) Uani 1 1 d . . . H8 H 0.4531 0.2493 0.5547 0.046 Uiso 1 1 calc R A . C9 C 0.5478(3) 0.1799(2) 0.6816(3) 0.0493(11) Uani 1 1 d . A . H9 H 0.5936 0.2151 0.7351 0.059 Uiso 1 1 calc R . . C10 C 0.5642(4) 0.1092(3) 0.7109(3) 0.0553(12) Uani 1 1 d . . . H10 H 0.6212 0.0958 0.7846 0.066 Uiso 1 1 calc R A . C11 C 0.4984(3) 0.0573(2) 0.6339(3) 0.0420(9) Uani 1 1 d . A . H11 H 0.5089 0.0084 0.6547 0.050 Uiso 1 1 calc R . . C12 C 0.4178(3) 0.07710(19) 0.5271(3) 0.0341(8) Uani 1 1 d . . . H12 H 0.3740 0.0416 0.4734 0.041 Uiso 1 1 calc R A . C19 C 0.1325(3) 0.0512(2) 0.3829(3) 0.0439(10) Uani 1 1 d . . . C18A C 0.3635(4) 0.1109(3) 0.1942(5) 0.034(2) Uani 0.50 1 d PG A 1 H18A H 0.2807 0.0988 0.1548 0.040 Uiso 0.50 1 calc PR A 1 C13A C 0.4077(5) 0.1473(4) 0.2952(5) 0.029(2) Uani 0.50 1 d PG A 1 C14A C 0.5288(6) 0.1651(4) 0.3528(5) 0.035(2) Uani 0.50 1 d PG A 1 H14A H 0.5590 0.1899 0.4219 0.042 Uiso 0.50 1 calc PR A 1 C15A C 0.6058(4) 0.1465(4) 0.3093(5) 0.054(3) Uani 0.50 1 d PG A 1 H15A H 0.6886 0.1586 0.3487 0.064 Uiso 0.50 1 calc PR A 1 C16A C 0.5617(5) 0.1101(4) 0.2083(5) 0.053(3) Uani 0.50 1 d PG A 1 H16A H 0.6144 0.0974 0.1786 0.064 Uiso 0.50 1 calc PR A 1 C17A C 0.4406(6) 0.0923(4) 0.1507(4) 0.050(3) Uani 0.50 1 d PG A 1 H17A H 0.4104 0.0675 0.0816 0.060 Uiso 0.50 1 calc PR A 1 C13B C 0.3706(6) 0.1334(4) 0.2727(5) 0.031(3) Uani 0.50 1 d PG A 2 C18B C 0.3113(4) 0.0894(3) 0.1802(5) 0.034(2) Uani 0.50 1 d PG A 2 H18B H 0.2288 0.0782 0.1542 0.041 Uiso 0.50 1 calc PR A 2 C17B C 0.3726(5) 0.0618(3) 0.1257(4) 0.0365(19) Uani 0.50 1 d PG A 2 H17B H 0.3321 0.0318 0.0624 0.044 Uiso 0.50 1 calc PR A 2 C16B C 0.4933(5) 0.0782(3) 0.1637(5) 0.032(2) Uani 0.50 1 d PG A 2 H16B H 0.5352 0.0593 0.1264 0.039 Uiso 0.50 1 calc PR A 2 C15B C 0.5526(4) 0.1222(3) 0.2562(5) 0.040(2) Uani 0.50 1 d PG A 2 H15B H 0.6350 0.1334 0.2822 0.048 Uiso 0.50 1 calc PR A 2 C14B C 0.4913(6) 0.1497(3) 0.3108(5) 0.039(2) Uani 0.50 1 d PG A 2 H14B H 0.5318 0.1798 0.3740 0.047 Uiso 0.50 1 calc PR A 2 H H -0.054(3) 0.2090(18) 0.228(3) 0.038 Uiso 1 1 d . D 4 H9B H -0.087(6) 0.134(4) 0.333(6) 0.04(2) Uiso 0.50 1 d P E 3 H10B H -0.225(6) 0.250(3) 0.168(5) 0.026(18) Uiso 0.50 1 d P F 3 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 Rh8 0.03946(17) 0.03093(15) 0.02596(15) -0.00729(13) -0.00426(11) 0.00841(14) N1 0.055(2) 0.052(2) 0.052(2) 0.0038(19) 0.0209(18) -0.0231(18) N2 0.0330(19) 0.0336(19) 0.067(3) 0.0033(18) -0.0031(17) -0.0080(15) S7 0.0290(16) 0.0279(14) 0.0305(11) 0.0053(10) 0.0112(12) 0.0015(10) B1 0.025(5) 0.031(6) 0.030(5) 0.000(4) 0.005(4) 0.003(4) B2 0.025(5) 0.038(5) 0.033(5) 0.003(4) 0.005(4) 0.001(4) B3 0.032(6) 0.028(5) 0.028(5) 0.003(4) 0.007(4) -0.002(4) B4 0.027(5) 0.018(4) 0.024(6) -0.006(4) 0.008(4) -0.001(3) B5 0.030(5) 0.050(6) 0.042(7) -0.013(6) 0.013(5) 0.007(5) B6 0.033(7) 0.045(6) 0.038(6) 0.010(5) 0.009(5) 0.014(5) B10 0.040(6) 0.040(6) 0.039(10) -0.013(7) 0.022(7) 0.016(5) B11 0.027(10) 0.034(9) 0.049(7) -0.020(6) -0.007(7) 0.002(6) S7B 0.0325(17) 0.0355(17) 0.0253(11) 0.0082(11) 0.0118(12) 0.0113(11) B1B 0.034(6) 0.036(5) 0.039(6) -0.009(5) -0.002(4) 0.003(4) B2B 0.036(6) 0.047(8) 0.018(4) -0.002(4) -0.004(4) 0.021(6) B4B 0.030(6) 0.034(5) 0.029(6) -0.004(4) 0.002(4) 0.000(4) B3B 0.032(6) 0.023(5) 0.026(5) -0.010(4) -0.002(4) 0.012(4) B5B 0.032(5) 0.043(6) 0.046(7) -0.016(6) 0.010(5) 0.000(4) B6B 0.030(6) 0.033(6) 0.033(6) 0.000(4) 0.003(4) 0.020(4) B9B 0.040(6) 0.049(7) 0.031(7) -0.018(5) 0.003(5) -0.004(4) B11B 0.025(10) 0.031(9) 0.048(7) -0.014(6) -0.011(7) 0.009(6) B10B 0.036(7) 0.040(6) 0.039(10) -0.025(7) 0.017(7) -0.001(5) P1 0.0445(6) 0.0291(5) 0.0232(5) 0.0050(4) 0.0137(4) 0.0030(4) C22 0.052(3) 0.039(3) 0.080(4) -0.012(2) -0.012(2) 0.012(2) C23 0.093(4) 0.064(3) 0.063(3) -0.012(3) 0.048(3) -0.030(3) C20 0.053(3) 0.051(3) 0.095(4) 0.027(3) 0.009(3) -0.023(2) C21 0.081(4) 0.066(4) 0.083(4) 0.025(3) 0.032(3) -0.030(3) C1 0.064(3) 0.0309(19) 0.0286(19) 0.0042(16) 0.0248(19) -0.0012(18) C2 0.103(4) 0.039(2) 0.065(3) 0.007(2) 0.064(3) 0.000(2) C3 0.137(5) 0.040(2) 0.077(3) -0.001(2) 0.084(4) -0.019(3) C4 0.126(5) 0.030(2) 0.050(3) -0.0067(19) 0.060(3) -0.010(3) C5 0.080(3) 0.032(2) 0.051(3) -0.0041(19) 0.038(2) -0.001(2) C6 0.056(3) 0.0291(19) 0.048(2) 0.0007(18) 0.027(2) -0.0027(18) C7 0.0280(19) 0.0356(19) 0.0250(18) 0.0016(15) 0.0095(15) -0.0083(15) C8 0.031(2) 0.041(2) 0.039(2) -0.0040(17) 0.0136(17) -0.0105(17) C9 0.027(2) 0.067(3) 0.041(2) -0.019(2) 0.0045(17) -0.004(2) C10 0.035(2) 0.082(4) 0.029(2) -0.002(2) -0.0025(17) 0.013(2) C11 0.034(2) 0.051(2) 0.031(2) 0.0091(18) 0.0072(16) 0.0007(18) C12 0.0284(19) 0.039(2) 0.0248(18) 0.0035(15) 0.0037(15) -0.0089(16) C19 0.028(2) 0.031(2) 0.052(3) -0.0022(18) 0.0014(18) -0.0090(16) C18A 0.028(5) 0.048(5) 0.017(4) 0.007(4) 0.004(4) 0.017(4) C13A 0.031(6) 0.024(4) 0.028(4) 0.002(3) 0.010(5) -0.012(4) C14A 0.037(5) 0.035(5) 0.032(5) 0.003(4) 0.017(4) -0.004(4) C15A 0.035(5) 0.064(6) 0.048(6) 0.026(5) 0.008(4) 0.000(4) C16A 0.047(6) 0.077(8) 0.053(7) 0.040(6) 0.037(5) 0.022(5) C17A 0.042(7) 0.079(8) 0.024(4) 0.020(4) 0.012(4) 0.041(6) C13B 0.026(5) 0.033(5) 0.027(5) 0.013(4) 0.007(4) -0.003(4) C18B 0.029(5) 0.037(5) 0.029(4) 0.011(3) 0.006(4) 0.003(4) C17B 0.036(5) 0.038(4) 0.030(4) 0.004(3) 0.011(4) -0.001(4) C16B 0.034(6) 0.031(5) 0.039(5) 0.011(4) 0.023(4) 0.006(4) C15B 0.043(6) 0.045(5) 0.031(5) 0.017(4) 0.017(4) 0.004(4) C14B 0.055(7) 0.030(4) 0.026(5) -0.004(4) 0.014(5) -0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh8 C19 2.015(4) . ? Rh8 B9 2.122(13) . ? Rh8 B4 2.133(9) . ? Rh8 B3 2.294(10) . ? Rh8 P1 2.3644(13) . ? Rh8 S7 2.523(3) . ? N1 C19 1.368(5) . ? N1 C21 1.375(6) . ? N1 C23 1.451(6) . ? N2 C19 1.353(5) . ? N2 C20 1.393(6) . ? N2 C22 1.453(6) . ? S7 B11 1.92(2) . ? S7 B2 1.975(10) . ? S7 B3 2.038(10) . ? B1 B3 1.728(14) . ? B1 B5 1.768(15) . ? B1 B2 1.771(14) . ? B1 B4 1.787(15) . ? B1 B6 1.802(15) . ? B2 B6 1.787(15) . ? B2 B3 1.864(14) . ? B2 B11 1.91(2) . ? B3 B4 1.845(14) . ? B4 B5 1.753(14) . ? B4 B9 1.766(16) . ? B5 B10 1.75(2) . ? B5 B9 1.773(16) . ? B5 B6 1.777(17) . ? B6 B11 1.727(17) . ? B6 B10 1.738(19) . ? B9 B10 1.85(3) . ? B10 B11 1.825(18) . ? S7B B11B 1.92(2) . ? S7B B2B 1.984(11) . ? S7B B3B 2.056(11) . ? B1B B3B 1.719(15) . ? B1B B2B 1.757(17) . ? B1B B5B 1.776(16) . ? B1B B4B 1.783(15) . ? B1B B6B 1.794(14) . ? B2B B6B 1.757(16) . ? B2B B11B 1.78(2) . ? B2B B3B 1.895(13) . ? B4B B9B 1.750(16) . ? B4B B5B 1.760(16) . ? B4B B3B 1.809(16) . ? B5B B6B 1.761(17) . ? B5B B10B 1.79(2) . ? B5B B9B 1.795(15) . ? B6B B11B 1.686(19) . ? B6B B10B 1.793(18) . ? B9B B10B 1.88(3) . ? B11B B10B 1.93(3) . ? P1 C13B 1.822(4) . ? P1 C7 1.823(3) . ? P1 C1 1.828(4) . ? P1 C13A 1.904(4) . ? C20 C21 1.333(8) . ? C1 C6 1.382(5) . ? C1 C2 1.391(5) . ? C2 C3 1.391(6) . ? C3 C4 1.375(7) . ? C4 C5 1.380(6) . ? C5 C6 1.387(5) . ? C7 C8 1.385(5) . ? C7 C12 1.391(5) . ? C8 C9 1.387(5) . ? C9 C10 1.372(6) . ? C10 C11 1.384(6) . ? C11 C12 1.374(5) . ? C18A C13A 1.3900 . ? C18A C17A 1.3900 . ? C13A C14A 1.3900 . ? C14A C15A 1.3900 . ? C15A C16A 1.3900 . ? C16A C17A 1.3900 . ? C13B C18B 1.3900 . ? C13B C14B 1.3900 . ? C18B C17B 1.3900 . ? C17B C16B 1.3900 . ? C16B C15B 1.3900 . ? C15B C14B 1.3900 . ? 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 C19 Rh8 B9 92.2(4) . . ? C19 Rh8 B4 96.0(3) . . ? B9 Rh8 B4 49.0(4) . . ? C19 Rh8 B3 132.3(3) . . ? B9 Rh8 B3 85.9(4) . . ? B4 Rh8 B3 49.1(4) . . ? C19 Rh8 P1 93.42(10) . . ? B9 Rh8 P1 140.6(3) . . ? B4 Rh8 P1 166.2(3) . . ? B3 Rh8 P1 117.3(3) . . ? C19 Rh8 S7 175.46(12) . . ? B9 Rh8 S7 92.0(3) . . ? B4 Rh8 S7 88.0(3) . . ? B3 Rh8 S7 49.8(2) . . ? P1 Rh8 S7 82.27(7) . . ? C19 N1 C21 111.0(4) . . ? C19 N1 C23 125.4(4) . . ? C21 N1 C23 123.3(4) . . ? C19 N2 C20 110.0(4) . . ? C19 N2 C22 125.2(4) . . ? C20 N2 C22 124.8(4) . . ? B11 S7 B2 58.7(7) . . ? B11 S7 B3 97.2(6) . . ? B2 S7 B3 55.3(4) . . ? B11 S7 Rh8 102.1(7) . . ? B2 S7 Rh8 106.1(3) . . ? B3 S7 Rh8 59.3(3) . . ? B3 B1 B5 111.1(7) . . ? B3 B1 B2 64.3(6) . . ? B5 B1 B2 111.8(7) . . ? B3 B1 B4 63.3(5) . . ? B5 B1 B4 59.1(6) . . ? B2 B1 B4 115.4(7) . . ? B3 B1 B6 109.4(7) . . ? B5 B1 B6 59.7(6) . . ? B2 B1 B6 60.0(6) . . ? B4 B1 B6 107.1(7) . . ? B1 B2 B6 60.9(6) . . ? B1 B2 B3 56.7(5) . . ? B6 B2 B3 104.2(8) . . ? B1 B2 B11 103.5(8) . . ? B6 B2 B11 55.6(6) . . ? B3 B2 B11 103.7(9) . . ? B1 B2 S7 110.8(6) . . ? B6 B2 S7 107.2(6) . . ? B3 B2 S7 64.0(4) . . ? B11 B2 S7 59.1(6) . . ? B1 B3 B4 59.9(6) . . ? B1 B3 B2 58.9(5) . . ? B4 B3 B2 108.3(7) . . ? B1 B3 S7 109.8(6) . . ? B4 B3 S7 113.4(6) . . ? B2 B3 S7 60.6(4) . . ? B1 B3 Rh8 114.1(7) . . ? B4 B3 Rh8 60.9(4) . . ? B2 B3 Rh8 120.1(6) . . ? S7 B3 Rh8 71.0(3) . . ? B5 B4 B9 60.5(6) . . ? B5 B4 B1 59.9(6) . . ? B9 B4 B1 110.0(7) . . ? B5 B4 B3 106.5(8) . . ? B9 B4 B3 113.1(7) . . ? B1 B4 B3 56.8(6) . . ? B5 B4 Rh8 118.2(6) . . ? B9 B4 Rh8 65.2(5) . . ? B1 B4 Rh8 119.5(7) . . ? B3 B4 Rh8 70.0(5) . . ? B10 B5 B4 110.3(10) . . ? B10 B5 B1 109.3(9) . . ? B4 B5 B1 61.0(6) . . ? B10 B5 B9 63.2(9) . . ? B4 B5 B9 60.1(6) . . ? B1 B5 B9 110.5(8) . . ? B10 B5 B6 59.0(8) . . ? B4 B5 B6 109.8(8) . . ? B1 B5 B6 61.1(6) . . ? B9 B5 B6 110.8(8) . . ? B11 B6 B10 63.5(9) . . ? B11 B6 B5 111.0(10) . . ? B10 B6 B5 59.7(9) . . ? B11 B6 B2 65.7(10) . . ? B10 B6 B2 117.0(10) . . ? B5 B6 B2 110.6(8) . . ? B11 B6 B1 110.0(10) . . ? B10 B6 B1 108.2(10) . . ? B5 B6 B1 59.2(6) . . ? B2 B6 B1 59.1(6) . . ? B4 B9 B5 59.4(6) . . ? B4 B9 B10 105.4(8) . . ? B5 B9 B10 57.8(8) . . ? B4 B9 Rh8 65.8(5) . . ? B5 B9 Rh8 117.8(7) . . ? B10 B9 Rh8 116.9(8) . . ? B6 B10 B5 61.3(8) . . ? B6 B10 B11 57.9(7) . . ? B5 B10 B11 107.8(10) . . ? B6 B10 B9 109.2(11) . . ? B5 B10 B9 59.0(9) . . ? B11 B10 B9 111.0(13) . . ? B6 B11 B10 58.5(8) . . ? B6 B11 B2 58.6(8) . . ? B10 B11 B2 107.3(10) . . ? B6 B11 S7 112.5(12) . . ? B10 B11 S7 117.0(14) . . ? B2 B11 S7 62.2(8) . . ? B11B S7B B2B 54.3(6) . . ? B11B S7B B3B 96.9(6) . . ? B2B S7B B3B 55.9(4) . . ? B3B B1B B2B 66.1(7) . . ? B3B B1B B5B 109.5(7) . . ? B2B B1B B5B 110.3(7) . . ? B3B B1B B4B 62.2(6) . . ? B2B B1B B4B 116.0(7) . . ? B5B B1B B4B 59.3(7) . . ? B3B B1B B6B 109.9(8) . . ? B2B B1B B6B 59.3(6) . . ? B5B B1B B6B 59.1(6) . . ? B4B B1B B6B 107.6(7) . . ? B1B B2B B6B 61.4(7) . . ? B1B B2B B11B 107.9(10) . . ? B6B B2B B11B 56.9(7) . . ? B1B B2B B3B 56.0(6) . . ? B6B B2B B3B 103.8(8) . . ? B11B B2B B3B 108.2(9) . . ? B1B B2B S7B 110.6(6) . . ? B6B B2B S7B 107.3(6) . . ? B11B B2B S7B 61.1(6) . . ? B3B B2B S7B 64.0(4) . . ? B9B B4B B5B 61.5(6) . . ? B9B B4B B1B 110.3(8) . . ? B5B B4B B1B 60.2(6) . . ? B9B B4B B3B 110.4(8) . . ? B5B B4B B3B 106.3(8) . . ? B1B B4B B3B 57.2(6) . . ? B1B B3B B4B 60.7(7) . . ? B1B B3B B2B 57.9(6) . . ? B4B B3B B2B 108.3(7) . . ? B1B B3B S7B 108.9(6) . . ? B4B B3B S7B 114.2(6) . . ? B2B B3B S7B 60.1(5) . . ? B4B B5B B6B 110.2(8) . . ? B4B B5B B1B 60.6(6) . . ? B6B B5B B1B 61.0(6) . . ? B4B B5B B10B 110.8(10) . . ? B6B B5B B10B 60.7(8) . . ? B1B B5B B10B 110.1(9) . . ? B4B B5B B9B 59.0(6) . . ? B6B B5B B9B 111.2(9) . . ? B1B B5B B9B 108.5(8) . . ? B10B B5B B9B 63.3(9) . . ? B11B B6B B2B 62.3(10) . . ? B11B B6B B5B 115.9(10) . . ? B2B B6B B5B 111.0(7) . . ? B11B B6B B10B 67.4(10) . . ? B2B B6B B10B 115.6(10) . . ? B5B B6B B10B 60.4(9) . . ? B11B B6B B1B 110.5(10) . . ? B2B B6B B1B 59.3(6) . . ? B5B B6B B1B 60.0(6) . . ? B10B B6B B1B 109.0(10) . . ? B4B B9B B5B 59.5(6) . . ? B4B B9B B10B 107.0(9) . . ? B5B B9B B10B 58.2(8) . . ? B6B B11B B2B 60.8(8) . . ? B6B B11B S7B 113.2(12) . . ? B2B B11B S7B 64.6(8) . . ? B6B B11B B10B 58.9(8) . . ? B2B B11B B10B 107.9(11) . . ? S7B B11B B10B 109.1(13) . . ? B5B B10B B6B 58.9(8) . . ? B5B B10B B9B 58.5(9) . . ? B6B B10B B9B 106.0(11) . . ? B5B B10B B11B 103.5(10) . . ? B6B B10B B11B 53.7(7) . . ? B9B B10B B11B 111.5(13) . . ? C13B P1 C7 104.8(3) . . ? C13B P1 C1 112.4(3) . . ? C7 P1 C1 104.35(17) . . ? C7 P1 C13A 96.0(2) . . ? C1 P1 C13A 103.7(3) . . ? C13B P1 Rh8 102.5(2) . . ? C7 P1 Rh8 121.84(11) . . ? C1 P1 Rh8 110.87(14) . . ? C13A P1 Rh8 117.58(19) . . ? C21 C20 N2 107.7(4) . . ? C20 C21 N1 106.7(5) . . ? C6 C1 C2 119.4(4) . . ? C6 C1 P1 116.8(3) . . ? C2 C1 P1 123.8(3) . . ? C3 C2 C1 119.7(4) . . ? C4 C3 C2 120.4(4) . . ? C3 C4 C5 120.1(4) . . ? C4 C5 C6 119.7(4) . . ? C1 C6 C5 120.7(4) . . ? C8 C7 C12 119.6(3) . . ? C8 C7 P1 122.9(3) . . ? C12 C7 P1 117.4(3) . . ? C7 C8 C9 119.4(4) . . ? C10 C9 C8 120.5(4) . . ? C9 C10 C11 120.5(4) . . ? C12 C11 C10 119.3(4) . . ? C11 C12 C7 120.8(3) . . ? N2 C19 N1 104.6(4) . . ? N2 C19 Rh8 125.3(3) . . ? N1 C19 Rh8 130.1(3) . . ? C13A C18A C17A 120.0 . . ? C18A C13A C14A 120.0 . . ? C18A C13A P1 117.6(3) . . ? C14A C13A P1 122.4(3) . . ? C15A C14A C13A 120.0 . . ? C16A C15A C14A 120.0 . . ? C17A C16A C15A 120.0 . . ? C16A C17A C18A 120.0 . . ? C18B C13B C14B 120.0 . . ? C18B C13B P1 122.4(3) . . ? C14B C13B P1 117.5(4) . . ? C13B C18B C17B 120.0 . . ? C16B C17B C18B 120.0 . . ? C15B C16B C17B 120.0 . . ? C16B C15B C14B 120.0 . . ? C15B C14B C13B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.695 _refine_diff_density_min -1.409 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 934329' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_fjl2161a #TrackingRef '19532_web_deposit_cif_file_0_RamonMacias_1366120253.compound_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H36 B9 N3 P Rh S, C H2 Cl2' _chemical_formula_sum 'C29 H38 B9 Cl2 N3 P Rh S' _chemical_formula_weight 762.75 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' B B 0.0013 0.0007 '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' 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' Rh Rh -1.1178 0.9187 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.478(3) _cell_length_b 18.762(5) _cell_length_c 15.649(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.586(4) _cell_angle_gamma 90.00 _cell_volume 3332.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7351 _cell_measurement_theta_min 2.3295 _cell_measurement_theta_max 27.896 _exptl_crystal_description Cube _exptl_crystal_colour Red _exptl_crystal_size_max 0.181 _exptl_crystal_size_mid 0.137 _exptl_crystal_size_min 0.118 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8670 _exptl_absorpt_correction_T_max 0.9103 _exptl_absorpt_process_details ; Multi-scan correction included in APEX2 package (Bruker AXS, 2008) ; _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 'Bruker APEX system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 39222 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.48 _reflns_number_total 7940 _reflns_number_gt 6260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v. 2009.7 (Bruker AXS, 2008)' _computing_cell_refinement 'APEX2 v. 2009.7 (Bruker AXS, 2008)' _computing_data_reduction 'APEX2 v. 2009.7 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The structure was solved by Patterson method and anisotropic refinement of all non hydrogen atoms was applied. All Hydrogen atoms were included in calculated positions and refined with a riding model. Hydrogen atoms of the borane fragment were observed in Fourier difference maps and freely refined, The asymmetric unit contains a rhodathiaborane molecule and a dichloromethane molecule. A static disorder has been observed in the dichloromethane molecule. It has been modeled with two sets of positions with equal complementary occupancy factors. A geometrical restrain in Cl-Cl distance has been used in the refinement. Residual electron density peaks are observed around the metal atom and they have no chemical sense. ; _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^)+(0.0767P)^2^+3.9757P] 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 ? _refine_ls_number_reflns 7940 _refine_ls_number_parameters 477 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1458 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl216a_0m in P2(1)/n CELL 0.71073 11.4784 18.7624 15.6492 90.000 98.586 90.000 ZERR 4.00 0.0033 0.0054 0.0046 0.000 0.004 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H B N P S RH CL UNIT 116 152 36 12 4 4 4 8 MERG 2 DFIX 21.0 0.020 C50A Cl1A C50A Cl2A C50B Cl1B C50B Cl2B DFIX 21.63 0.020 Cl1A Cl2A Cl1B Cl2B OMIT 0 17 2 OMIT 0 15 3 OMIT -5 4 20 OMIT -14 5 5 OMIT -9 15 11 OMIT 0 10 10 OMIT -7 21 6 OMIT 9 1 12 FMAP 2 PLAN 10 ACTA 55 WPDB -2 BOND $H SIZE 0.181 0.137 0.118 L.S. 6 TEMP -173.00 WGHT 0.076700 3.975700 FVAR 0.09414 1.75320 PART 1 10.5 C50A 1 0.862921 0.438663 0.362703 10.50000 0.03334 0.02976 = 0.06350 -0.00936 0.00792 0.00226 AFIX 23 H50A 2 0.801677 0.427075 0.398845 10.50000 -1.20000 H50B 2 0.940059 0.440337 0.400615 10.50000 -1.20000 AFIX 0 CL1A 8 0.865558 0.372910 0.283676 10.50000 0.04580 0.04550 = 0.06177 -0.01897 -0.00092 0.00767 CL2A 8 0.832989 0.520826 0.313660 10.50000 0.05275 0.03365 = 0.04441 -0.00358 0.00278 0.00345 PART 2 10.5 C50B 1 0.842847 0.477363 0.319828 10.50000 0.04564 0.01245 = 0.08141 0.01386 0.02193 0.00571 AFIX 23 H50C 2 0.757799 0.488991 0.312264 10.50000 -1.20000 H50D 2 0.883040 0.514448 0.289946 10.50000 -1.20000 AFIX 0 CL1B 8 0.862340 0.394655 0.273606 10.50000 0.03490 0.05688 = 0.05701 0.00455 0.01023 0.00553 CL2B 8 0.899849 0.477624 0.430550 10.50000 0.07613 0.03481 = 0.06455 0.00045 0.02919 0.01119 PART 0 RH1 7 0.218321 0.159778 0.227205 11.00000 0.01814 0.01707 = 0.02201 0.00021 0.00339 -0.00067 S2 6 0.233743 0.127864 0.081510 11.00000 0.02664 0.02438 = 0.02441 -0.00205 0.00508 -0.00261 P1 5 0.071838 0.101903 0.282729 11.00000 0.01954 0.01680 = 0.02161 -0.00033 0.00387 -0.00029 N1 4 0.203893 0.302220 0.345688 11.00000 0.02511 0.01605 = 0.02856 0.00131 0.00572 -0.00003 N2 4 0.378107 0.032329 0.281739 11.00000 0.02266 0.01969 = 0.03744 0.00200 0.00560 0.00253 N3 4 0.397743 0.111879 0.379083 11.00000 0.02115 0.02148 = 0.02851 0.00196 0.00245 -0.00104 B3 3 0.223574 0.265840 0.261097 11.00000 0.02266 0.02070 = 0.02647 0.00298 0.00494 -0.00090 B4 3 0.363687 0.184872 0.140851 11.00000 0.02378 0.02369 = 0.02885 -0.00294 0.00610 -0.00256 B5 3 0.129302 0.206997 0.079391 11.00000 0.01986 0.02753 = 0.02724 0.00001 0.00197 -0.00013 B6 3 0.126855 0.270108 0.167765 11.00000 0.02533 0.01978 = 0.02924 -0.00070 0.00706 -0.00322 B7 3 0.356100 0.249625 0.226640 11.00000 0.02185 0.02057 = 0.02783 -0.00005 0.00520 -0.00317 B8 3 0.275108 0.221814 0.038811 11.00000 0.02897 0.02671 = 0.02641 0.00144 0.00656 -0.00358 B9 3 0.262008 0.319887 0.181213 11.00000 0.02588 0.02074 = 0.03066 0.00356 0.00404 -0.00328 B10 3 0.353481 0.276025 0.116871 11.00000 0.02399 0.02858 = 0.03217 0.00159 0.00887 -0.00438 B11 3 0.198992 0.291689 0.077699 11.00000 0.02795 0.02218 = 0.02836 0.00531 0.00630 -0.00054 C1 1 0.287505 0.341355 0.392250 11.00000 0.02958 0.02167 = 0.03769 -0.00162 -0.00019 -0.00015 AFIX 43 H1 2 0.359536 0.349324 0.370731 11.00000 -1.20000 AFIX 0 C2 1 0.272431 0.370218 0.469844 11.00000 0.04813 0.02629 = 0.03855 -0.00995 -0.00089 -0.00109 AFIX 43 H2 2 0.333588 0.397592 0.501854 11.00000 -1.20000 AFIX 0 C3 1 0.168963 0.359591 0.501352 11.00000 0.05759 0.03342 = 0.03096 -0.00564 0.00965 0.00845 AFIX 43 H3 2 0.157611 0.379045 0.555547 11.00000 -1.20000 AFIX 0 C4 1 0.081213 0.320106 0.453090 11.00000 0.04658 0.03175 = 0.03869 -0.00088 0.01653 0.00103 AFIX 43 H4 2 0.008206 0.312291 0.473271 11.00000 -1.20000 AFIX 0 C5 1 0.101089 0.292608 0.376205 11.00000 0.03029 0.02079 = 0.03480 -0.00352 0.00948 -0.00147 AFIX 43 H5 2 0.040539 0.265703 0.342812 11.00000 -1.20000 AFIX 0 C6 1 -0.073437 0.142570 0.279763 11.00000 0.02009 0.02009 = 0.03256 -0.00484 0.00472 -0.00345 C7 1 -0.147096 0.128651 0.340576 11.00000 0.02818 0.03174 = 0.03048 -0.00045 0.00657 0.00159 AFIX 43 H7 2 -0.120062 0.099475 0.389113 11.00000 -1.20000 AFIX 0 C8 1 -0.259029 0.156851 0.330995 11.00000 0.02414 0.04304 = 0.04268 -0.00185 0.01368 0.00346 AFIX 43 H8 2 -0.307974 0.147901 0.373698 11.00000 -1.20000 AFIX 0 C9 1 -0.300759 0.198035 0.259846 11.00000 0.02035 0.03440 = 0.05071 -0.00982 0.00210 0.00449 AFIX 43 H9 2 -0.378208 0.217160 0.253436 11.00000 -1.20000 AFIX 0 C10 1 -0.229711 0.211169 0.198473 11.00000 0.02820 0.02694 = 0.04134 -0.00168 -0.00233 0.00471 AFIX 43 H10 2 -0.258156 0.239276 0.149271 11.00000 -1.20000 AFIX 0 C11 1 -0.116809 0.183594 0.208059 11.00000 0.02352 0.02611 = 0.03230 0.00081 0.00351 0.00009 AFIX 43 H11 2 -0.068302 0.192790 0.165143 11.00000 -1.20000 AFIX 0 C12 1 0.116015 0.076556 0.395214 11.00000 0.02024 0.02237 = 0.02355 0.00096 0.00361 -0.00410 C13 1 0.181393 0.014491 0.415480 11.00000 0.01885 0.02584 = 0.02978 0.00035 0.00644 -0.00153 AFIX 43 H13 2 0.194839 -0.017109 0.370533 11.00000 -1.20000 AFIX 0 C14 1 0.226471 -0.001447 0.499473 11.00000 0.02190 0.03417 = 0.03434 0.00742 0.00509 0.00151 AFIX 43 H14 2 0.269704 -0.044269 0.512344 11.00000 -1.20000 AFIX 0 C15 1 0.209366 0.044237 0.565031 11.00000 0.02811 0.04039 = 0.02574 0.00736 0.00211 -0.00673 AFIX 43 H15 2 0.241760 0.033403 0.623026 11.00000 -1.20000 AFIX 0 C16 1 0.145446 0.105514 0.546626 11.00000 0.03644 0.03311 = 0.02484 -0.00362 0.00586 -0.00607 AFIX 43 H16 2 0.133163 0.137017 0.591963 11.00000 -1.20000 AFIX 0 C17 1 0.099039 0.121457 0.462540 11.00000 0.03366 0.01924 = 0.02538 -0.00125 0.00778 -0.00295 AFIX 43 H17 2 0.054635 0.163957 0.450488 11.00000 -1.20000 AFIX 0 C18 1 0.019452 0.018093 0.229891 11.00000 0.01588 0.02155 = 0.02533 -0.00244 0.00426 0.00019 C19 1 0.004144 0.016403 0.141040 11.00000 0.02798 0.02537 = 0.02765 0.00018 0.00706 -0.00748 AFIX 43 H19 2 0.028143 0.056093 0.110234 11.00000 -1.20000 AFIX 0 C20 1 -0.045593 -0.042110 0.095855 11.00000 0.03561 0.03454 = 0.02517 -0.00173 0.00573 -0.00787 AFIX 43 H20 2 -0.057921 -0.041745 0.034462 11.00000 -1.20000 AFIX 0 C21 1 -0.077480 -0.101275 0.139980 11.00000 0.02849 0.02362 = 0.03147 -0.00751 0.00667 -0.00324 AFIX 43 H21 2 -0.109886 -0.142041 0.109156 11.00000 -1.20000 AFIX 0 C22 1 -0.061861 -0.100453 0.228418 11.00000 0.02331 0.01927 = 0.03433 0.00311 0.00582 -0.00191 AFIX 43 H22 2 -0.082741 -0.141083 0.259039 11.00000 -1.20000 AFIX 0 C23 1 -0.015655 -0.040592 0.273793 11.00000 0.02490 0.02254 = 0.02410 0.00141 0.00742 -0.00147 AFIX 43 H23 2 -0.008074 -0.039838 0.335073 11.00000 -1.20000 AFIX 0 C24 1 0.336593 0.097723 0.301219 11.00000 0.02015 0.02042 = 0.03030 0.00131 0.00832 -0.00080 C25 1 0.462477 0.007997 0.347323 11.00000 0.02544 0.02953 = 0.04416 0.01018 0.00816 0.01030 AFIX 43 H25 2 0.504183 -0.035815 0.348560 11.00000 -1.20000 AFIX 0 C26 1 0.474038 0.057588 0.408235 11.00000 0.02402 0.03132 = 0.03655 0.00769 0.00037 0.00362 AFIX 43 H26 2 0.525237 0.055982 0.461828 11.00000 -1.20000 AFIX 0 C27 1 0.341669 -0.007519 0.202771 11.00000 0.03003 0.02099 = 0.04337 -0.00337 0.00874 0.00386 AFIX 137 H27A 2 0.255521 -0.007009 0.189148 11.00000 -1.50000 H27B 2 0.369275 -0.056847 0.210600 11.00000 -1.50000 H27C 2 0.375609 0.014394 0.155249 11.00000 -1.50000 AFIX 0 C28 1 0.384402 0.174892 0.431287 11.00000 0.03242 0.02791 = 0.02480 -0.00127 -0.00198 0.00198 AFIX 137 H28A 2 0.428580 0.214617 0.411094 11.00000 -1.50000 H28B 2 0.414823 0.164752 0.491952 11.00000 -1.50000 H28C 2 0.300837 0.187657 0.425904 11.00000 -1.50000 AFIX 0 H4B 2 0.443974 0.155518 0.136118 11.00000 0.01856 H5B 2 0.043527 0.192562 0.036528 11.00000 0.00967 H6B 2 0.047125 0.290019 0.166101 11.00000 0.00878 H7B 2 0.439455 0.252606 0.270344 11.00000 0.01248 H8B 2 0.292264 0.224333 -0.025895 11.00000 0.01887 H9B 2 0.271442 0.375860 0.196343 11.00000 0.01905 H10B 2 0.426087 0.303321 0.093672 11.00000 0.03656 H11B 2 0.163890 0.332130 0.034914 11.00000 0.02224 HKLF 4 REM fjl216a_0m in P2(1)/n REM R1 = 0.0548 for 6260 Fo > 4sig(Fo) and 0.0737 for all 7940 data REM 477 parameters refined using 6 restraints END ; 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 C50A C 0.8629(9) 0.4387(5) 0.3627(7) 0.042(2) Uani 0.50 1 d PD A 1 H50A H 0.8017 0.4271 0.3988 0.051 Uiso 0.50 1 calc PR A 1 H50B H 0.9401 0.4403 0.4006 0.051 Uiso 0.50 1 calc PR A 1 Cl1A Cl 0.8656(9) 0.3729(3) 0.2837(5) 0.0519(17) Uani 0.50 1 d PD A 1 Cl2A Cl 0.8330(2) 0.52083(15) 0.31366(16) 0.0441(5) Uani 0.50 1 d PD A 1 C50B C 0.8428(9) 0.4774(5) 0.3198(7) 0.045(3) Uani 0.50 1 d PD B 2 H50C H 0.7578 0.4890 0.3123 0.054 Uiso 0.50 1 calc PR B 2 H50D H 0.8830 0.5144 0.2899 0.054 Uiso 0.50 1 calc PR B 2 Cl1B Cl 0.8623(8) 0.3947(3) 0.2736(6) 0.0493(14) Uani 0.50 1 d PD B 2 Cl2B Cl 0.8998(3) 0.47762(14) 0.43055(19) 0.0566(7) Uani 0.50 1 d PD B 2 Rh1 Rh 0.21832(2) 0.159778(15) 0.227205(18) 0.01903(10) Uani 1 1 d . . . S2 S 0.23374(9) 0.12786(5) 0.08151(6) 0.0250(2) Uani 1 1 d . . . P1 P 0.07184(8) 0.10190(5) 0.28273(6) 0.0192(2) Uani 1 1 d . . . N1 N 0.2039(3) 0.30222(16) 0.3457(2) 0.0231(6) Uani 1 1 d . . . N2 N 0.3781(3) 0.03233(17) 0.2817(2) 0.0265(7) Uani 1 1 d . . . N3 N 0.3977(3) 0.11188(17) 0.3791(2) 0.0238(7) Uani 1 1 d . . . B3 B 0.2236(4) 0.2658(2) 0.2611(3) 0.0231(8) Uani 1 1 d . . . B4 B 0.3637(4) 0.1849(2) 0.1409(3) 0.0252(9) Uani 1 1 d . . . B5 B 0.1293(4) 0.2070(2) 0.0794(3) 0.0250(9) Uani 1 1 d . . . B6 B 0.1269(4) 0.2701(2) 0.1678(3) 0.0245(9) Uani 1 1 d . . . B7 B 0.3561(4) 0.2496(2) 0.2266(3) 0.0233(8) Uani 1 1 d . . . B8 B 0.2751(4) 0.2218(2) 0.0388(3) 0.0271(9) Uani 1 1 d . . . B9 B 0.2620(4) 0.3199(2) 0.1812(3) 0.0258(9) Uani 1 1 d . . . B10 B 0.3535(4) 0.2760(3) 0.1169(3) 0.0278(9) Uani 1 1 d . . . B11 B 0.1990(4) 0.2917(2) 0.0777(3) 0.0259(9) Uani 1 1 d . . . C1 C 0.2875(4) 0.3414(2) 0.3922(3) 0.0302(9) Uani 1 1 d . . . H1 H 0.3595 0.3493 0.3707 0.036 Uiso 1 1 calc R . . C2 C 0.2724(4) 0.3702(2) 0.4698(3) 0.0384(10) Uani 1 1 d . . . H2 H 0.3336 0.3976 0.5019 0.046 Uiso 1 1 calc R . . C3 C 0.1690(5) 0.3596(3) 0.5014(3) 0.0403(11) Uani 1 1 d . . . H3 H 0.1576 0.3790 0.5555 0.048 Uiso 1 1 calc R . . C4 C 0.0812(5) 0.3201(2) 0.4531(3) 0.0380(10) Uani 1 1 d . . . H4 H 0.0082 0.3123 0.4733 0.046 Uiso 1 1 calc R . . C5 C 0.1011(4) 0.2926(2) 0.3762(3) 0.0282(8) Uani 1 1 d . . . H5 H 0.0405 0.2657 0.3428 0.034 Uiso 1 1 calc R . . C6 C -0.0734(3) 0.1426(2) 0.2798(3) 0.0242(8) Uani 1 1 d . . . C7 C -0.1471(4) 0.1287(2) 0.3406(3) 0.0299(9) Uani 1 1 d . . . H7 H -0.1201 0.0995 0.3891 0.036 Uiso 1 1 calc R . . C8 C -0.2590(4) 0.1569(2) 0.3310(3) 0.0357(10) Uani 1 1 d . . . H8 H -0.3080 0.1479 0.3737 0.043 Uiso 1 1 calc R . . C9 C -0.3008(4) 0.1980(2) 0.2598(3) 0.0355(10) Uani 1 1 d . . . H9 H -0.3782 0.2172 0.2534 0.043 Uiso 1 1 calc R . . C10 C -0.2297(4) 0.2112(2) 0.1985(3) 0.0329(9) Uani 1 1 d . . . H10 H -0.2582 0.2393 0.1493 0.040 Uiso 1 1 calc R . . C11 C -0.1168(4) 0.1836(2) 0.2081(3) 0.0274(8) Uani 1 1 d . . . H11 H -0.0683 0.1928 0.1651 0.033 Uiso 1 1 calc R . . C12 C 0.1160(3) 0.0766(2) 0.3952(2) 0.0220(7) Uani 1 1 d . . . C13 C 0.1814(3) 0.0145(2) 0.4155(3) 0.0245(8) Uani 1 1 d . . . H13 H 0.1948 -0.0171 0.3705 0.029 Uiso 1 1 calc R . . C14 C 0.2265(4) -0.0014(2) 0.4995(3) 0.0300(9) Uani 1 1 d . . . H14 H 0.2697 -0.0443 0.5123 0.036 Uiso 1 1 calc R . . C15 C 0.2094(4) 0.0442(2) 0.5650(3) 0.0316(9) Uani 1 1 d . . . H15 H 0.2418 0.0334 0.6230 0.038 Uiso 1 1 calc R . . C16 C 0.1454(4) 0.1055(2) 0.5466(3) 0.0313(9) Uani 1 1 d . . . H16 H 0.1332 0.1370 0.5920 0.038 Uiso 1 1 calc R . . C17 C 0.0990(4) 0.1215(2) 0.4625(2) 0.0258(8) Uani 1 1 d . . . H17 H 0.0546 0.1640 0.4505 0.031 Uiso 1 1 calc R . . C18 C 0.0195(3) 0.01809(19) 0.2299(2) 0.0208(7) Uani 1 1 d . . . C19 C 0.0041(4) 0.0164(2) 0.1410(3) 0.0267(8) Uani 1 1 d . . . H19 H 0.0281 0.0561 0.1102 0.032 Uiso 1 1 calc R . . C20 C -0.0456(4) -0.0421(2) 0.0959(3) 0.0317(9) Uani 1 1 d . . . H20 H -0.0579 -0.0417 0.0345 0.038 Uiso 1 1 calc R . . C21 C -0.0775(4) -0.1013(2) 0.1400(3) 0.0276(8) Uani 1 1 d . . . H21 H -0.1099 -0.1420 0.1092 0.033 Uiso 1 1 calc R . . C22 C -0.0619(3) -0.1005(2) 0.2284(3) 0.0255(8) Uani 1 1 d . . . H22 H -0.0827 -0.1411 0.2590 0.031 Uiso 1 1 calc R . . C23 C -0.0157(3) -0.0406(2) 0.2738(2) 0.0235(8) Uani 1 1 d . . . H23 H -0.0081 -0.0398 0.3351 0.028 Uiso 1 1 calc R . . C24 C 0.3366(3) 0.0977(2) 0.3012(2) 0.0232(8) Uani 1 1 d . . . C25 C 0.4625(4) 0.0080(2) 0.3473(3) 0.0327(9) Uani 1 1 d . . . H25 H 0.5042 -0.0358 0.3486 0.039 Uiso 1 1 calc R . . C26 C 0.4740(4) 0.0576(2) 0.4082(3) 0.0311(9) Uani 1 1 d . . . H26 H 0.5252 0.0560 0.4618 0.037 Uiso 1 1 calc R . . C27 C 0.3417(4) -0.0075(2) 0.2028(3) 0.0311(9) Uani 1 1 d . . . H27A H 0.2555 -0.0070 0.1891 0.047 Uiso 1 1 calc R . . H27B H 0.3693 -0.0568 0.2106 0.047 Uiso 1 1 calc R . . H27C H 0.3756 0.0144 0.1552 0.047 Uiso 1 1 calc R . . C28 C 0.3844(4) 0.1749(2) 0.4313(3) 0.0290(9) Uani 1 1 d . . . H28A H 0.4286 0.2146 0.4111 0.044 Uiso 1 1 calc R . . H28B H 0.4148 0.1648 0.4920 0.044 Uiso 1 1 calc R . . H28C H 0.3008 0.1877 0.4259 0.044 Uiso 1 1 calc R . . H4B H 0.444(4) 0.156(2) 0.136(3) 0.019(10) Uiso 1 1 d . . . H5B H 0.044(3) 0.193(2) 0.037(2) 0.010(9) Uiso 1 1 d . . . H6B H 0.047(3) 0.2900(19) 0.166(2) 0.009(9) Uiso 1 1 d . . . H7B H 0.439(3) 0.253(2) 0.270(2) 0.012(9) Uiso 1 1 d . . . H8B H 0.292(3) 0.224(2) -0.026(3) 0.019(10) Uiso 1 1 d . . . H9B H 0.271(4) 0.376(2) 0.196(2) 0.019(10) Uiso 1 1 d . . . H10B H 0.426(4) 0.303(3) 0.094(3) 0.037(13) Uiso 1 1 d . . . H11B H 0.164(4) 0.332(2) 0.035(3) 0.022(11) 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 C50A 0.033(5) 0.030(5) 0.063(7) -0.009(5) 0.008(4) 0.002(4) Cl1A 0.046(2) 0.045(3) 0.062(4) -0.019(3) -0.001(2) 0.008(3) Cl2A 0.0528(15) 0.0336(14) 0.0444(13) -0.0036(11) 0.0028(11) 0.0034(11) C50B 0.046(6) 0.012(4) 0.081(8) 0.014(5) 0.022(5) 0.006(4) Cl1B 0.0349(18) 0.057(4) 0.057(2) 0.005(3) 0.0102(14) 0.006(3) Cl2B 0.076(2) 0.0348(13) 0.0645(17) 0.0005(12) 0.0292(15) 0.0112(13) Rh1 0.01814(16) 0.01707(16) 0.02201(16) 0.00021(10) 0.00339(11) -0.00067(10) S2 0.0266(5) 0.0244(5) 0.0244(5) -0.0020(4) 0.0051(4) -0.0026(4) P1 0.0195(4) 0.0168(4) 0.0216(5) -0.0003(3) 0.0039(4) -0.0003(3) N1 0.0251(16) 0.0160(15) 0.0286(17) 0.0013(12) 0.0057(13) 0.0000(12) N2 0.0227(16) 0.0197(16) 0.0374(19) 0.0020(14) 0.0056(14) 0.0025(13) N3 0.0212(16) 0.0215(16) 0.0285(17) 0.0020(13) 0.0025(13) -0.0010(12) B3 0.023(2) 0.021(2) 0.026(2) 0.0030(16) 0.0049(16) -0.0009(16) B4 0.024(2) 0.024(2) 0.029(2) -0.0029(17) 0.0061(17) -0.0026(17) B5 0.020(2) 0.028(2) 0.027(2) 0.0000(17) 0.0020(17) -0.0001(17) B6 0.025(2) 0.020(2) 0.029(2) -0.0007(16) 0.0071(18) -0.0032(16) B7 0.022(2) 0.021(2) 0.028(2) -0.0001(16) 0.0052(17) -0.0032(16) B8 0.029(2) 0.027(2) 0.026(2) 0.0014(17) 0.0066(18) -0.0036(18) B9 0.026(2) 0.021(2) 0.031(2) 0.0036(17) 0.0040(18) -0.0033(17) B10 0.024(2) 0.029(2) 0.032(2) 0.0016(18) 0.0089(18) -0.0044(18) B11 0.028(2) 0.022(2) 0.028(2) 0.0053(17) 0.0063(18) -0.0005(17) C1 0.030(2) 0.022(2) 0.038(2) -0.0016(16) -0.0002(17) -0.0001(15) C2 0.048(3) 0.026(2) 0.039(3) -0.0100(18) -0.001(2) -0.0011(19) C3 0.058(3) 0.033(2) 0.031(2) -0.0056(18) 0.010(2) 0.008(2) C4 0.047(3) 0.032(2) 0.039(2) -0.0009(19) 0.017(2) 0.001(2) C5 0.030(2) 0.0208(19) 0.035(2) -0.0035(16) 0.0095(17) -0.0015(15) C6 0.0201(18) 0.0201(18) 0.033(2) -0.0048(15) 0.0047(15) -0.0035(14) C7 0.028(2) 0.032(2) 0.030(2) -0.0005(17) 0.0066(17) 0.0016(17) C8 0.024(2) 0.043(3) 0.043(3) -0.002(2) 0.0137(19) 0.0035(18) C9 0.0204(19) 0.034(2) 0.051(3) -0.010(2) 0.0021(18) 0.0045(17) C10 0.028(2) 0.027(2) 0.041(2) -0.0017(18) -0.0023(18) 0.0047(17) C11 0.0235(19) 0.026(2) 0.032(2) 0.0008(16) 0.0035(16) 0.0001(16) C12 0.0202(17) 0.0224(18) 0.0236(18) 0.0010(14) 0.0036(14) -0.0041(14) C13 0.0188(18) 0.0258(19) 0.030(2) 0.0004(15) 0.0064(15) -0.0015(15) C14 0.0219(19) 0.034(2) 0.034(2) 0.0074(17) 0.0051(16) 0.0015(16) C15 0.028(2) 0.040(2) 0.026(2) 0.0074(17) 0.0021(16) -0.0067(18) C16 0.036(2) 0.033(2) 0.025(2) -0.0036(16) 0.0059(17) -0.0061(18) C17 0.034(2) 0.0192(18) 0.0254(19) -0.0012(14) 0.0078(16) -0.0029(15) C18 0.0159(16) 0.0216(18) 0.0253(18) -0.0024(14) 0.0043(14) 0.0002(13) C19 0.028(2) 0.025(2) 0.028(2) 0.0002(15) 0.0071(16) -0.0075(16) C20 0.036(2) 0.035(2) 0.025(2) -0.0017(17) 0.0057(17) -0.0079(18) C21 0.028(2) 0.024(2) 0.031(2) -0.0075(16) 0.0067(16) -0.0032(15) C22 0.0233(19) 0.0193(18) 0.034(2) 0.0031(15) 0.0058(16) -0.0019(14) C23 0.0249(19) 0.0225(19) 0.0241(19) 0.0014(14) 0.0074(15) -0.0015(15) C24 0.0201(18) 0.0204(18) 0.030(2) 0.0013(15) 0.0083(15) -0.0008(14) C25 0.025(2) 0.030(2) 0.044(2) 0.0102(18) 0.0082(18) 0.0103(16) C26 0.024(2) 0.031(2) 0.037(2) 0.0077(18) 0.0004(17) 0.0036(17) C27 0.030(2) 0.0210(19) 0.043(2) -0.0034(17) 0.0087(18) 0.0039(16) C28 0.032(2) 0.028(2) 0.025(2) -0.0013(16) -0.0020(16) 0.0020(16) _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 C50A Cl2A 1.733(10) . ? C50A Cl1A 1.750(11) . ? C50A H50A 0.9900 . ? C50A H50B 0.9900 . ? C50B Cl1B 1.741(11) . ? C50B Cl2B 1.758(11) . ? C50B H50C 0.9900 . ? C50B H50D 0.9900 . ? Rh1 C24 2.018(4) . ? Rh1 B3 2.058(4) . ? Rh1 P1 2.2798(11) . ? Rh1 B7 2.312(4) . ? Rh1 B4 2.346(5) . ? Rh1 S2 2.3893(12) . ? Rh1 B6 2.442(5) . ? Rh1 B5 2.544(5) . ? S2 B5 1.905(5) . ? S2 B4 1.954(5) . ? S2 B8 1.968(5) . ? P1 C12 1.821(4) . ? P1 C6 1.828(4) . ? P1 C18 1.836(4) . ? N1 C1 1.335(5) . ? N1 C5 1.350(5) . ? N1 B3 1.536(5) . ? N2 C24 1.367(5) . ? N2 C25 1.379(5) . ? N2 C27 1.451(5) . ? N3 C24 1.339(5) . ? N3 C26 1.376(5) . ? N3 C28 1.458(5) . ? B3 B6 1.699(6) . ? B3 B7 1.715(6) . ? B3 B9 1.718(6) . ? B4 B10 1.751(7) . ? B4 B7 1.822(6) . ? B4 B8 1.892(7) . ? B4 H4B 1.09(4) . ? B5 B11 1.781(6) . ? B5 B6 1.824(6) . ? B5 B8 1.897(7) . ? B5 H5B 1.14(4) . ? B6 B11 1.785(6) . ? B6 B9 1.796(6) . ? B6 H6B 0.99(4) . ? B7 B9 1.783(6) . ? B7 B10 1.784(6) . ? B7 H7B 1.09(4) . ? B8 B10 1.734(7) . ? B8 B11 1.735(7) . ? B8 H8B 1.06(4) . ? B9 B11 1.754(7) . ? B9 B10 1.763(7) . ? B9 H9B 1.08(4) . ? B10 B11 1.812(7) . ? B10 H10B 1.09(5) . ? B11 H11B 1.05(4) . ? C1 C2 1.364(6) . ? C1 H1 0.9500 . ? C2 C3 1.367(7) . ? C2 H2 0.9500 . ? C3 C4 1.381(7) . ? C3 H3 0.9500 . ? C4 C5 1.359(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.389(6) . ? C6 C11 1.390(6) . ? C7 C8 1.377(6) . ? C7 H7 0.9500 . ? C8 C9 1.381(7) . ? C8 H8 0.9500 . ? C9 C10 1.372(7) . ? C9 H9 0.9500 . ? C10 C11 1.383(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.385(5) . ? C12 C13 1.396(5) . ? C13 C14 1.372(6) . ? C13 H13 0.9500 . ? C14 C15 1.373(6) . ? C14 H14 0.9500 . ? C15 C16 1.371(6) . ? C15 H15 0.9500 . ? C16 C17 1.377(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.376(5) . ? C18 C23 1.389(5) . ? C19 C20 1.382(6) . ? C19 H19 0.9500 . ? C20 C21 1.385(6) . ? C20 H20 0.9500 . ? C21 C22 1.369(6) . ? C21 H21 0.9500 . ? C22 C23 1.391(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C25 C26 1.324(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 Cl2A C50A Cl1A 109.7(6) . . ? Cl2A C50A H50A 109.7 . . ? Cl1A C50A H50A 109.7 . . ? Cl2A C50A H50B 109.7 . . ? Cl1A C50A H50B 109.7 . . ? H50A C50A H50B 108.2 . . ? Cl1B C50B Cl2B 111.1(6) . . ? Cl1B C50B H50C 109.4 . . ? Cl2B C50B H50C 109.4 . . ? Cl1B C50B H50D 109.4 . . ? Cl2B C50B H50D 109.4 . . ? H50C C50B H50D 108.0 . . ? C24 Rh1 B3 114.75(16) . . ? C24 Rh1 P1 88.72(11) . . ? B3 Rh1 P1 110.93(12) . . ? C24 Rh1 B7 91.20(15) . . ? B3 Rh1 B7 45.76(16) . . ? P1 Rh1 B7 153.18(11) . . ? C24 Rh1 B4 88.34(16) . . ? B3 Rh1 B4 87.62(16) . . ? P1 Rh1 B4 160.64(11) . . ? B7 Rh1 B4 46.05(15) . . ? C24 Rh1 S2 105.30(11) . . ? B3 Rh1 S2 119.00(12) . . ? P1 Rh1 S2 114.10(4) . . ? B7 Rh1 S2 91.77(11) . . ? B4 Rh1 S2 48.72(11) . . ? C24 Rh1 B6 157.25(15) . . ? B3 Rh1 B6 43.34(16) . . ? P1 Rh1 B6 104.44(11) . . ? B7 Rh1 B6 68.65(15) . . ? B4 Rh1 B6 85.00(16) . . ? S2 Rh1 B6 86.44(11) . . ? C24 Rh1 B5 150.15(15) . . ? B3 Rh1 B5 83.68(16) . . ? P1 Rh1 B5 107.06(10) . . ? B7 Rh1 B5 85.68(15) . . ? B4 Rh1 B5 68.29(15) . . ? S2 Rh1 B5 45.30(11) . . ? B6 Rh1 B5 42.86(15) . . ? B5 S2 B4 90.9(2) . . ? B5 S2 B8 58.6(2) . . ? B4 S2 B8 57.7(2) . . ? B5 S2 Rh1 71.66(14) . . ? B4 S2 Rh1 64.49(14) . . ? B8 S2 Rh1 98.95(14) . . ? C12 P1 C6 104.77(18) . . ? C12 P1 C18 103.71(17) . . ? C6 P1 C18 96.31(17) . . ? C12 P1 Rh1 112.21(12) . . ? C6 P1 Rh1 120.89(13) . . ? C18 P1 Rh1 116.55(12) . . ? C1 N1 C5 118.4(4) . . ? C1 N1 B3 121.9(3) . . ? C5 N1 B3 119.6(3) . . ? C24 N2 C25 111.1(3) . . ? C24 N2 C27 125.9(3) . . ? C25 N2 C27 123.0(3) . . ? C24 N3 C26 112.1(3) . . ? C24 N3 C28 125.9(3) . . ? C26 N3 C28 122.0(3) . . ? N1 B3 B6 124.0(3) . . ? N1 B3 B7 127.0(3) . . ? B6 B3 B7 103.6(3) . . ? N1 B3 B9 116.9(3) . . ? B6 B3 B9 63.4(3) . . ? B7 B3 B9 62.6(3) . . ? N1 B3 Rh1 130.5(3) . . ? B6 B3 Rh1 80.4(2) . . ? B7 B3 Rh1 75.0(2) . . ? B9 B3 Rh1 112.6(3) . . ? B10 B4 B7 59.8(3) . . ? B10 B4 B8 56.7(3) . . ? B7 B4 B8 107.4(3) . . ? B10 B4 S2 114.3(3) . . ? B7 B4 S2 126.7(3) . . ? B8 B4 S2 61.5(2) . . ? B10 B4 Rh1 106.8(3) . . ? B7 B4 Rh1 65.99(19) . . ? B8 B4 Rh1 102.8(2) . . ? S2 B4 Rh1 66.79(14) . . ? B10 B4 H4B 121(2) . . ? B7 B4 H4B 122(2) . . ? B8 B4 H4B 119(2) . . ? S2 B4 H4B 107(2) . . ? Rh1 B4 H4B 128(2) . . ? B11 B5 B6 59.3(2) . . ? B11 B5 B8 56.2(2) . . ? B6 B5 B8 105.8(3) . . ? B11 B5 S2 114.4(3) . . ? B6 B5 S2 125.0(3) . . ? B8 B5 S2 62.3(2) . . ? B11 B5 Rh1 101.8(2) . . ? B6 B5 Rh1 65.6(2) . . ? B8 B5 Rh1 95.8(2) . . ? S2 B5 Rh1 63.04(13) . . ? B11 B5 H5B 123.7(19) . . ? B6 B5 H5B 119.4(19) . . ? B8 B5 H5B 124.5(18) . . ? S2 B5 H5B 108.1(19) . . ? Rh1 B5 H5B 130.4(19) . . ? B3 B6 B11 111.6(3) . . ? B3 B6 B9 58.8(3) . . ? B11 B6 B9 58.7(3) . . ? B3 B6 B5 122.6(3) . . ? B11 B6 B5 59.1(2) . . ? B9 B6 B5 108.4(3) . . ? B3 B6 Rh1 56.22(19) . . ? B11 B6 Rh1 105.6(3) . . ? B9 B6 Rh1 94.7(2) . . ? B5 B6 Rh1 71.6(2) . . ? B3 B6 H6B 122(2) . . ? B11 B6 H6B 116(2) . . ? B9 B6 H6B 126(2) . . ? B5 B6 H6B 110(2) . . ? Rh1 B6 H6B 133(2) . . ? B3 B7 B9 58.8(2) . . ? B3 B7 B10 111.4(3) . . ? B9 B7 B10 59.2(3) . . ? B3 B7 B4 119.5(3) . . ? B9 B7 B4 107.0(3) . . ? B10 B7 B4 58.1(3) . . ? B3 B7 Rh1 59.27(19) . . ? B9 B7 Rh1 99.6(2) . . ? B10 B7 Rh1 107.0(3) . . ? B4 B7 Rh1 68.0(2) . . ? B3 B7 H7B 122.0(19) . . ? B9 B7 H7B 129(2) . . ? B10 B7 H7B 118.5(19) . . ? B4 B7 H7B 111(2) . . ? Rh1 B7 H7B 125(2) . . ? B10 B8 B11 63.0(3) . . ? B10 B8 B4 57.6(3) . . ? B11 B8 B4 102.5(3) . . ? B10 B8 B5 103.9(3) . . ? B11 B8 B5 58.5(3) . . ? B4 B8 B5 93.1(3) . . ? B10 B8 S2 114.3(3) . . ? B11 B8 S2 113.5(3) . . ? B4 B8 S2 60.8(2) . . ? B5 B8 S2 59.04(19) . . ? B10 B8 H8B 120(2) . . ? B11 B8 H8B 118(2) . . ? B4 B8 H8B 132(2) . . ? B5 B8 H8B 129(2) . . ? S2 B8 H8B 117(2) . . ? B3 B9 B11 112.3(3) . . ? B3 B9 B10 112.3(3) . . ? B11 B9 B10 62.0(3) . . ? B3 B9 B7 58.6(2) . . ? B11 B9 B7 106.7(3) . . ? B10 B9 B7 60.4(3) . . ? B3 B9 B6 57.8(2) . . ? B11 B9 B6 60.3(3) . . ? B10 B9 B6 105.5(3) . . ? B7 B9 B6 97.1(3) . . ? B3 B9 H9B 116(2) . . ? B11 B9 H9B 121(2) . . ? B10 B9 H9B 122(2) . . ? B7 B9 H9B 127(2) . . ? B6 B9 H9B 126(2) . . ? B8 B10 B4 65.7(3) . . ? B8 B10 B9 112.7(3) . . ? B4 B10 B9 111.1(3) . . ? B8 B10 B7 116.6(3) . . ? B4 B10 B7 62.1(3) . . ? B9 B10 B7 60.4(3) . . ? B8 B10 B11 58.5(3) . . ? B4 B10 B11 105.2(3) . . ? B9 B10 B11 58.8(3) . . ? B7 B10 B11 104.2(3) . . ? B8 B10 H10B 113(2) . . ? B4 B10 H10B 120(3) . . ? B9 B10 H10B 122(3) . . ? B7 B10 H10B 123(2) . . ? B11 B10 H10B 125(3) . . ? B8 B11 B9 113.1(3) . . ? B8 B11 B5 65.3(3) . . ? B9 B11 B5 112.3(3) . . ? B8 B11 B6 115.0(3) . . ? B9 B11 B6 61.0(3) . . ? B5 B11 B6 61.5(2) . . ? B8 B11 B10 58.5(3) . . ? B9 B11 B10 59.2(3) . . ? B5 B11 B10 105.6(3) . . ? B6 B11 B10 104.0(3) . . ? B8 B11 H11B 119(2) . . ? B9 B11 H11B 116(2) . . ? B5 B11 H11B 122(2) . . ? B6 B11 H11B 119(2) . . ? B10 B11 H11B 127(2) . . ? N1 C1 C2 121.9(4) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 119.7(4) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 118.9(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 122.3(4) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C7 C6 C11 118.4(4) . . ? C7 C6 P1 123.4(3) . . ? C11 C6 P1 117.8(3) . . ? C8 C7 C6 120.4(4) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.6(4) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 119.6(4) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.2(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.8(4) . . ? C10 C11 H11 119.6 . . ? C6 C11 H11 119.6 . . ? C17 C12 C13 117.8(4) . . ? C17 C12 P1 121.7(3) . . ? C13 C12 P1 120.0(3) . . ? C14 C13 C12 120.8(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.3(4) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 119.9(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.1(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 121.1(4) . . ? C16 C17 H17 119.5 . . ? C12 C17 H17 119.5 . . ? C19 C18 C23 118.6(3) . . ? C19 C18 P1 117.3(3) . . ? C23 C18 P1 123.8(3) . . ? C18 C19 C20 121.1(4) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 120.1(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 119.4(4) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 120.5(4) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 120.3(4) . . ? C18 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? N3 C24 N2 103.2(3) . . ? N3 C24 Rh1 128.6(3) . . ? N2 C24 Rh1 128.1(3) . . ? C26 C25 N2 106.7(4) . . ? C26 C25 H25 126.7 . . ? N2 C25 H25 126.7 . . ? C25 C26 N3 106.9(4) . . ? C25 C26 H26 126.5 . . ? N3 C26 H26 126.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 H28A 109.5 . . ? N3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.531 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 934330'