#------------------------------------------------------------------------------ #$Date: 2016-02-04 23:53:04 +0200 (Thu, 04 Feb 2016) $ #$Revision: 175914 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/05/1540583.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1540583 loop_ _publ_author_name 'Boerth, Jeffrey A.' 'Ellman, Jonathan A.' _publ_section_title ; Rh(iii)-catalyzed diastereoselective C--H bond addition/cyclization cascade of enone tethered aldehydes ; _journal_issue 2 _journal_name_full 'Chem. Sci.' _journal_page_first 1474 _journal_paper_doi 10.1039/C5SC04138D _journal_volume 7 _journal_year 2016 _chemical_formula_moiety 'C24 B F20, C30 H31 N O Rh' _chemical_formula_sum 'C54 H31 B F20 N O Rh' _chemical_formula_weight 1203.52 _chemical_melting_point 377 _chemical_name_systematic 'Cp*Rhodium(III) Enolate of 1-phenyl-3-(2-(pyridin-2-yl)phenyl)propan-1-one' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2015-10-16 deposited with the CCDC. 2015-11-23 downloaded from the CCDC. ; _cell_angle_alpha 79.702(2) _cell_angle_beta 80.128(2) _cell_angle_gamma 73.163(2) _cell_formula_units_Z 2 _cell_length_a 11.8540(8) _cell_length_b 13.0781(9) _cell_length_c 16.1540(11) _cell_measurement_reflns_used -403 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 68.3 _cell_measurement_theta_min 2.8 _cell_volume 2339.2(3) _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_data_collection 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_molecular_graphics ; Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., OLEX2: A complete structure solution, refinement and analysis program (2009). J. Appl. Cryst., 42, 339-341. ; _computing_publication_material 'SHELXL-2013/2 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT-2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 93(2) _diffrn_detector_area_resol_mean 22.2 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Rigaku Saturn 944+ CCD' _diffrn_measurement_method \w _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_unetI/netI 0.0278 _diffrn_reflns_laue_measured_fraction_full 0.977 _diffrn_reflns_laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 75602 _diffrn_reflns_point_group_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.095 _diffrn_reflns_theta_min 2.803 _diffrn_source 'Sealed Tube' _exptl_absorpt_coefficient_mu 4.074 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_crystal_colour Orange _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1200 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Chloroform' _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.401 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 712 _refine_ls_number_reflns 8279 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.126 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_gt 0.0250 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.6328P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.0731 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7906 _reflns_number_total 8279 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc04138d2.cif _cod_data_source_block 007-15127 _cod_depositor_comments 'Adding full bibliography for 1540582--1540583.cif.' _cod_database_code 1540583 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.736 _shelx_estimated_absorpt_t_max 0.854 _shelx_res_file ; 007-15127.res created by SHELXL-2014/7 TITL JAB-I-658 007-15127 CELL 1.54178 11.854 13.0781 16.154 79.702 80.128 73.163 ZERR 2 0.0008 0.0009 0.0011 0.002 0.002 0.002 LATT 1 SFAC C H B F N O Rh UNIT 108 62 2 40 2 2 2 L.S. 10 SIZE 0.08 0.08 0.04 TEMP -180 BOND $H MORE -1 CONF ACTA WGHT 0.041000 0.632800 FVAR 0.34554 RH1 7 0.057288 0.805248 0.216133 11.00000 0.01958 0.02014 = 0.01599 -0.00202 -0.00295 -0.00796 O1 6 0.099854 0.654104 0.298973 11.00000 0.02181 0.02072 = 0.02461 -0.00060 -0.00430 -0.00633 N1 5 0.217269 0.819063 0.251140 11.00000 0.02261 0.02024 = 0.01874 0.00113 -0.00219 -0.00872 C1 1 -0.009537 0.700569 0.326328 11.00000 0.02309 0.02124 = 0.01579 0.00214 -0.00450 -0.00785 C2 1 -0.033720 0.809564 0.343934 11.00000 0.02088 0.02106 = 0.01786 -0.00158 -0.00102 -0.00956 H2 2 -0.121472 0.852540 0.347596 11.00000 0.01308 C3 1 0.034965 0.843090 0.400653 11.00000 0.02294 0.02302 = 0.01647 -0.00107 -0.00239 -0.01054 AFIX 23 H3A 2 -0.003170 0.834967 0.460093 11.00000 -1.20000 H3B 2 0.117129 0.795702 0.398102 11.00000 -1.20000 AFIX 0 C4 1 0.037970 0.959099 0.372598 11.00000 0.02204 0.02320 = 0.01860 -0.00337 -0.00576 -0.01017 C5 1 -0.052573 1.042250 0.404746 11.00000 0.02246 0.02776 = 0.02363 -0.00565 -0.00486 -0.00963 AFIX 43 H5 2 -0.114807 1.024959 0.445300 11.00000 -1.20000 AFIX 0 C6 1 -0.054277 1.150010 0.379018 11.00000 0.02715 0.02486 = 0.03142 -0.00805 -0.00717 -0.00636 AFIX 43 H6 2 -0.118358 1.205289 0.400610 11.00000 -1.20000 AFIX 0 C7 1 0.037483 1.176517 0.321953 11.00000 0.03210 0.02103 = 0.03530 -0.00348 -0.00712 -0.01027 AFIX 43 H7 2 0.037431 1.249913 0.304884 11.00000 -1.20000 AFIX 0 C8 1 0.129273 1.095387 0.289947 11.00000 0.02691 0.02678 = 0.02957 -0.00113 -0.00240 -0.01482 AFIX 43 H8 2 0.192830 1.113503 0.251317 11.00000 -1.20000 AFIX 0 C9 1 0.129883 0.986901 0.313664 11.00000 0.02151 0.02302 = 0.02233 -0.00322 -0.00565 -0.00974 C10 1 0.233604 0.903803 0.280878 11.00000 0.02391 0.02300 = 0.01958 0.00098 -0.00251 -0.01272 C11 1 0.347487 0.912483 0.282161 11.00000 0.02598 0.02937 = 0.03355 -0.00394 -0.00192 -0.01485 AFIX 43 H11 2 0.357607 0.972155 0.303233 11.00000 -1.20000 AFIX 0 C12 1 0.445538 0.835343 0.253158 11.00000 0.02110 0.03651 = 0.04144 -0.00115 -0.00200 -0.01355 AFIX 43 H12 2 0.523350 0.842127 0.252505 11.00000 -1.20000 AFIX 0 C13 1 0.428643 0.747783 0.224989 11.00000 0.02243 0.02849 = 0.03387 -0.00054 0.00041 -0.00707 AFIX 43 H13 2 0.494650 0.692690 0.205302 11.00000 -1.20000 AFIX 0 C14 1 0.313747 0.741886 0.226005 11.00000 0.02411 0.02200 = 0.02634 0.00033 -0.00133 -0.00878 AFIX 43 H14 2 0.302461 0.680561 0.208144 11.00000 -1.20000 AFIX 0 C15 1 -0.102108 0.643874 0.328278 11.00000 0.02524 0.02005 = 0.02176 0.00017 -0.00627 -0.00894 C16 1 -0.219422 0.685056 0.362704 11.00000 0.02486 0.02100 = 0.03364 0.00161 -0.00636 -0.00963 AFIX 43 H16 2 -0.241962 0.751674 0.384867 11.00000 -1.20000 AFIX 0 C17 1 -0.303763 0.629249 0.364831 11.00000 0.02570 0.03051 = 0.04457 0.00533 -0.00743 -0.01296 AFIX 43 H17 2 -0.384010 0.658499 0.387196 11.00000 -1.20000 AFIX 0 C18 1 -0.270362 0.530604 0.334161 11.00000 0.03731 0.03069 = 0.04895 0.00347 -0.01622 -0.02142 AFIX 43 H18 2 -0.327950 0.492707 0.334961 11.00000 -1.20000 AFIX 0 C19 1 -0.153337 0.487704 0.302509 11.00000 0.04299 0.02365 = 0.03958 -0.00053 -0.01667 -0.01559 AFIX 43 H19 2 -0.130518 0.419373 0.283001 11.00000 -1.20000 AFIX 0 C20 1 -0.068939 0.543272 0.298918 11.00000 0.03024 0.02190 = 0.02605 -0.00188 -0.00749 -0.00737 AFIX 43 H20 2 0.011186 0.513370 0.276642 11.00000 -1.20000 AFIX 0 C21 1 -0.004260 0.772020 0.105231 11.00000 0.04422 0.03352 = 0.01728 0.00067 -0.01216 -0.01752 C22 1 -0.091843 0.858252 0.143039 11.00000 0.02804 0.04162 = 0.01711 0.00056 -0.01014 -0.01236 C23 1 -0.038087 0.944421 0.139181 11.00000 0.02668 0.02915 = 0.01866 -0.00156 -0.00729 -0.00417 C24 1 0.080960 0.911144 0.097660 11.00000 0.03063 0.02665 = 0.01438 0.00208 -0.00359 -0.00885 C25 1 0.102721 0.804726 0.077208 11.00000 0.03553 0.02819 = 0.01589 -0.00129 -0.00352 -0.00825 C26 1 -0.021073 0.666893 0.092888 11.00000 0.07073 0.04321 = 0.02967 -0.00339 -0.01664 -0.03014 AFIX 137 H26A 2 0.050478 0.608885 0.104401 11.00000 -1.50000 H26B 2 -0.035316 0.670614 0.034293 11.00000 -1.50000 H26C 2 -0.089390 0.652347 0.131890 11.00000 -1.50000 AFIX 0 C27 1 -0.218615 0.862047 0.175293 11.00000 0.02782 0.06887 = 0.02844 0.00335 -0.01036 -0.01758 AFIX 137 H27A 2 -0.228211 0.788685 0.186215 11.00000 -1.50000 H27B 2 -0.269343 0.905614 0.132812 11.00000 -1.50000 H27C 2 -0.241492 0.894334 0.228022 11.00000 -1.50000 AFIX 0 C28 1 -0.098869 1.052129 0.166916 11.00000 0.04336 0.03107 = 0.03216 -0.00509 -0.01222 0.00510 AFIX 137 H28A 2 -0.161098 1.044567 0.214250 11.00000 -1.50000 H28B 2 -0.134589 1.101678 0.119513 11.00000 -1.50000 H28C 2 -0.040799 1.080810 0.185183 11.00000 -1.50000 AFIX 0 C29 1 0.166196 0.979613 0.077101 11.00000 0.04029 0.03390 = 0.02921 0.00654 -0.00526 -0.01759 AFIX 137 H29A 2 0.146122 1.032200 0.117183 11.00000 -1.50000 H29B 2 0.161132 1.017709 0.019257 11.00000 -1.50000 H29C 2 0.247198 0.933807 0.081388 11.00000 -1.50000 AFIX 0 C30 1 0.216717 0.740824 0.032628 11.00000 0.05133 0.03569 = 0.02466 -0.00455 0.00307 -0.00177 AFIX 137 H30A 2 0.282885 0.767347 0.040605 11.00000 -1.50000 H30B 2 0.210612 0.749089 -0.028076 11.00000 -1.50000 H30C 2 0.230797 0.664473 0.056358 11.00000 -1.50000 AFIX 0 F1 4 0.285077 0.227829 0.355719 11.00000 0.02471 0.02006 = 0.02829 -0.00091 -0.00084 -0.01203 F2 4 0.112489 0.328898 0.464850 11.00000 0.02471 0.03722 = 0.03305 -0.00480 0.00701 -0.01554 F3 4 0.110585 0.528143 0.498736 11.00000 0.02710 0.03688 = 0.03171 -0.01217 0.00691 -0.00478 F4 4 0.289603 0.617467 0.424124 11.00000 0.03342 0.02096 = 0.03384 -0.00871 -0.00299 -0.00627 F5 4 0.459100 0.520344 0.312763 11.00000 0.02497 0.02045 = 0.02945 -0.00283 0.00164 -0.01179 F6 4 0.607065 0.325719 0.390287 11.00000 0.03066 0.01827 = 0.02726 -0.00063 -0.00817 -0.01156 F7 4 0.691960 0.179935 0.517670 11.00000 0.03823 0.03699 = 0.02495 0.00295 -0.01179 -0.01446 F8 4 0.686390 -0.028966 0.528207 11.00000 0.03763 0.02838 = 0.03712 0.01474 -0.00867 -0.00709 F9 4 0.592373 -0.087376 0.406249 11.00000 0.03509 0.01476 = 0.04731 0.00133 0.00244 -0.00910 F10 4 0.506733 0.054764 0.280406 11.00000 0.03226 0.02186 = 0.03669 -0.00513 -0.00529 -0.01552 F11 4 0.622113 0.156568 0.143181 11.00000 0.02293 0.03202 = 0.03562 -0.01181 0.00341 -0.01129 F12 4 0.553764 0.088661 0.018915 11.00000 0.04863 0.05395 = 0.03930 -0.02808 0.01128 -0.02423 F13 4 0.320541 0.152281 -0.008358 11.00000 0.06175 0.06661 = 0.03147 -0.01380 -0.01006 -0.03859 F14 4 0.159523 0.286305 0.092464 11.00000 0.03342 0.05241 = 0.03213 0.00591 -0.01394 -0.02353 F15 4 0.225402 0.363035 0.210591 11.00000 0.02177 0.03509 = 0.02854 -0.00226 -0.00556 -0.00580 F16 4 0.754736 0.259338 0.239608 11.00000 0.01913 0.02623 = 0.02813 0.00025 -0.00197 -0.00672 F17 4 0.879337 0.372611 0.129043 11.00000 0.02184 0.04751 = 0.03418 -0.00278 0.00375 -0.01662 F18 4 0.770083 0.550297 0.027424 11.00000 0.04092 0.04912 = 0.03709 0.01230 0.00363 -0.02849 F19 4 0.527584 0.609809 0.037555 11.00000 0.04235 0.03277 = 0.03438 0.01468 -0.00655 -0.01449 F20 4 0.399546 0.496181 0.147288 11.00000 0.02292 0.02569 = 0.03117 0.00470 -0.00448 -0.00661 C31 1 0.377893 0.370712 0.324909 11.00000 0.01847 0.01965 = 0.01781 0.00139 -0.00411 -0.00622 C32 1 0.287781 0.326619 0.369194 11.00000 0.02073 0.01900 = 0.02198 -0.00066 -0.00518 -0.00626 C33 1 0.197986 0.376722 0.426730 11.00000 0.01946 0.02807 = 0.02318 0.00106 -0.00036 -0.00994 C34 1 0.197290 0.476086 0.444569 11.00000 0.01979 0.02799 = 0.01975 -0.00383 0.00068 -0.00123 C35 1 0.287418 0.521480 0.405676 11.00000 0.02464 0.01855 = 0.02327 -0.00256 -0.00597 -0.00367 C36 1 0.374082 0.469204 0.347421 11.00000 0.01964 0.02069 = 0.02041 0.00154 -0.00322 -0.00765 C37 1 0.551238 0.200311 0.327061 11.00000 0.01630 0.01881 = 0.02121 -0.00163 0.00220 -0.00778 C38 1 0.601161 0.223587 0.391464 11.00000 0.01860 0.01723 = 0.02525 -0.00125 0.00030 -0.00764 C39 1 0.645638 0.150349 0.458018 11.00000 0.02151 0.02677 = 0.02425 0.00093 -0.00398 -0.00917 C40 1 0.643366 0.044237 0.463653 11.00000 0.02043 0.02316 = 0.02971 0.00877 -0.00069 -0.00456 C41 1 0.596552 0.015664 0.402216 11.00000 0.02117 0.01525 = 0.03482 0.00065 0.00476 -0.00682 C42 1 0.552597 0.092613 0.336249 11.00000 0.01687 0.02047 = 0.02682 -0.00313 0.00078 -0.00795 C43 1 0.427849 0.259814 0.187430 11.00000 0.02278 0.02060 = 0.01965 0.00080 -0.00142 -0.01216 C44 1 0.504737 0.191722 0.132969 11.00000 0.02592 0.02660 = 0.02576 -0.00369 0.00020 -0.01459 C45 1 0.472118 0.154804 0.068487 11.00000 0.03866 0.03458 = 0.02488 -0.00916 0.00560 -0.02030 C46 1 0.355498 0.186261 0.054501 11.00000 0.04592 0.04200 = 0.02136 -0.00273 -0.00481 -0.02986 C47 1 0.274616 0.254512 0.104906 11.00000 0.02889 0.03695 = 0.02344 0.00666 -0.00849 -0.02046 C48 1 0.311808 0.291397 0.168128 11.00000 0.02679 0.02583 = 0.01947 0.00178 -0.00105 -0.01328 C49 1 0.569131 0.371680 0.200880 11.00000 0.02228 0.01944 = 0.01871 -0.00480 -0.00066 -0.00932 C50 1 0.691953 0.346407 0.192358 11.00000 0.02490 0.02051 = 0.01884 -0.00308 -0.00252 -0.00900 C51 1 0.759699 0.404471 0.135402 11.00000 0.02007 0.03360 = 0.02509 -0.00747 0.00234 -0.01425 C52 1 0.705170 0.493955 0.083388 11.00000 0.03633 0.03363 = 0.02060 0.00115 0.00356 -0.02286 C53 1 0.582996 0.523122 0.088723 11.00000 0.03377 0.02485 = 0.02095 0.00337 -0.00392 -0.01177 C54 1 0.519407 0.462454 0.145940 11.00000 0.02237 0.02393 = 0.02184 -0.00240 -0.00066 -0.00927 B1 3 0.482186 0.300742 0.259942 11.00000 0.01834 0.01728 = 0.02315 -0.00126 -0.00262 -0.00778 HKLF 4 REM JAB-I-658 007-15127 REM R1 = 0.0250 for 7906 Fo > 4sig(Fo) and 0.0260 for all 8279 data REM 712 parameters refined using 0 restraints END WGHT 0.0410 0.6329 REM Highest difference peak 0.401, deepest hole -0.735, 1-sigma level 0.061 Q1 1 0.0015 0.8868 0.2311 11.00000 0.05 0.40 Q2 1 0.0380 0.9019 0.1597 11.00000 0.05 0.36 Q3 1 0.1024 0.8033 0.2696 11.00000 0.05 0.35 Q4 1 -0.0173 0.7602 0.2196 11.00000 0.05 0.33 Q5 1 0.5266 0.3445 0.2350 11.00000 0.05 0.31 Q6 1 0.7242 0.3578 0.1493 11.00000 0.05 0.30 Q7 1 0.0141 0.8141 0.1570 11.00000 0.05 0.30 Q8 1 0.3967 0.3856 0.3504 11.00000 0.05 0.29 Q9 1 0.0786 0.7078 0.2617 11.00000 0.05 0.29 Q10 1 -0.0215 0.8214 0.2940 11.00000 0.05 0.29 Q11 1 0.1807 0.7426 0.2212 11.00000 0.05 0.29 Q12 1 0.3621 0.4248 0.3255 11.00000 0.05 0.28 Q13 1 -0.0419 0.7567 0.3548 11.00000 0.05 0.28 Q14 1 0.0016 0.8302 0.3665 11.00000 0.05 0.28 Q15 1 -0.0782 0.9127 0.1278 11.00000 0.05 0.27 Q16 1 -0.0726 0.9998 0.1491 11.00000 0.05 0.26 Q17 1 0.2602 0.3424 0.4075 11.00000 0.05 0.26 Q18 1 0.0438 0.9030 0.3906 11.00000 0.05 0.25 Q19 1 0.1397 0.8367 0.1964 11.00000 0.05 0.25 Q20 1 0.2998 0.5693 0.4131 11.00000 0.05 0.25 ; _shelx_res_checksum 86799 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Rh1 Rh 0.05729(2) 0.80525(2) 0.21613(2) 0.01797(6) Uani 1 1 d . . O1 O 0.09985(12) 0.65410(11) 0.29897(8) 0.0224(3) Uani 1 1 d . . N1 N 0.21727(15) 0.81906(13) 0.25114(10) 0.0204(3) Uani 1 1 d . . C1 C -0.00954(18) 0.70057(15) 0.32633(12) 0.0200(4) Uani 1 1 d . . C2 C -0.03372(18) 0.80956(15) 0.34393(12) 0.0194(4) Uani 1 1 d . . H2 H -0.121(2) 0.8525(16) 0.3476(12) 0.013(5) Uiso 1 1 d . . C3 C 0.03496(18) 0.84309(15) 0.40065(12) 0.0201(4) Uani 1 1 d . . H3A H -0.0032 0.8350 0.4601 0.024 Uiso 1 1 calc R U H3B H 0.1171 0.7957 0.3981 0.024 Uiso 1 1 calc R U C4 C 0.03797(18) 0.95910(15) 0.37260(12) 0.0199(4) Uani 1 1 d . . C5 C -0.05257(18) 1.04225(16) 0.40475(13) 0.0235(4) Uani 1 1 d . . H5 H -0.1148 1.0250 0.4453 0.028 Uiso 1 1 calc R U C6 C -0.0543(2) 1.15001(17) 0.37902(14) 0.0270(4) Uani 1 1 d . . H6 H -0.1184 1.2053 0.4006 0.032 Uiso 1 1 calc R U C7 C 0.0375(2) 1.17652(17) 0.32195(14) 0.0285(5) Uani 1 1 d . . H7 H 0.0374 1.2499 0.3049 0.034 Uiso 1 1 calc R U C8 C 0.12927(19) 1.09539(17) 0.28995(13) 0.0266(4) Uani 1 1 d . . H8 H 0.1928 1.1135 0.2513 0.032 Uiso 1 1 calc R U C9 C 0.12988(18) 0.98690(16) 0.31366(12) 0.0211(4) Uani 1 1 d . . C10 C 0.23360(18) 0.90380(16) 0.28088(12) 0.0213(4) Uani 1 1 d . . C11 C 0.34749(19) 0.91248(17) 0.28216(14) 0.0283(5) Uani 1 1 d . . H11 H 0.3576 0.9722 0.3032 0.034 Uiso 1 1 calc R U C12 C 0.4455(2) 0.83534(19) 0.25316(15) 0.0325(5) Uani 1 1 d . . H12 H 0.5234 0.8421 0.2525 0.039 Uiso 1 1 calc R U C13 C 0.42864(19) 0.74778(18) 0.22499(14) 0.0292(5) Uani 1 1 d . . H13 H 0.4946 0.6927 0.2053 0.035 Uiso 1 1 calc R U C14 C 0.31375(18) 0.74189(16) 0.22600(13) 0.0243(4) Uani 1 1 d . . H14 H 0.3025 0.6806 0.2081 0.029 Uiso 1 1 calc R U C15 C -0.10211(18) 0.64387(15) 0.32828(12) 0.0217(4) Uani 1 1 d . . C16 C -0.21942(19) 0.68506(16) 0.36270(14) 0.0261(4) Uani 1 1 d . . H16 H -0.2420 0.7517 0.3849 0.031 Uiso 1 1 calc R U C17 C -0.3038(2) 0.62925(18) 0.36483(15) 0.0334(5) Uani 1 1 d . . H17 H -0.3840 0.6585 0.3872 0.040 Uiso 1 1 calc R U C18 C -0.2704(2) 0.53060(18) 0.33416(16) 0.0362(5) Uani 1 1 d . . H18 H -0.3280 0.4927 0.3350 0.043 Uiso 1 1 calc R U C19 C -0.1533(2) 0.48770(18) 0.30251(15) 0.0330(5) Uani 1 1 d . . H19 H -0.1305 0.4194 0.2830 0.040 Uiso 1 1 calc R U C20 C -0.0689(2) 0.54327(16) 0.29892(13) 0.0257(4) Uani 1 1 d . . H20 H 0.0112 0.5134 0.2766 0.031 Uiso 1 1 calc R U C21 C -0.0043(2) 0.77202(18) 0.10523(13) 0.0297(5) Uani 1 1 d . . C22 C -0.09184(19) 0.85825(18) 0.14304(12) 0.0280(5) Uani 1 1 d . . C23 C -0.03809(19) 0.94442(17) 0.13918(12) 0.0252(4) Uani 1 1 d . . C24 C 0.08096(19) 0.91114(16) 0.09766(12) 0.0242(4) Uani 1 1 d . . C25 C 0.1027(2) 0.80473(17) 0.07721(12) 0.0268(4) Uani 1 1 d . . C26 C -0.0211(3) 0.6669(2) 0.09289(15) 0.0436(6) Uani 1 1 d . . H26A H 0.0505 0.6089 0.1044 0.065 Uiso 1 1 calc R U H26B H -0.0353 0.6706 0.0343 0.065 Uiso 1 1 calc R U H26C H -0.0894 0.6523 0.1319 0.065 Uiso 1 1 calc R U C27 C -0.2186(2) 0.8620(2) 0.17529(15) 0.0412(6) Uani 1 1 d . . H27A H -0.2282 0.7887 0.1862 0.062 Uiso 1 1 calc R U H27B H -0.2693 0.9056 0.1328 0.062 Uiso 1 1 calc R U H27C H -0.2415 0.8943 0.2280 0.062 Uiso 1 1 calc R U C28 C -0.0989(2) 1.05213(18) 0.16692(15) 0.0377(6) Uani 1 1 d . . H28A H -0.1611 1.0446 0.2142 0.057 Uiso 1 1 calc R U H28B H -0.1346 1.1017 0.1195 0.057 Uiso 1 1 calc R U H28C H -0.0408 1.0808 0.1852 0.057 Uiso 1 1 calc R U C29 C 0.1662(2) 0.97961(19) 0.07710(14) 0.0341(5) Uani 1 1 d . . H29A H 0.1461 1.0322 0.1172 0.051 Uiso 1 1 calc R U H29B H 0.1611 1.0177 0.0193 0.051 Uiso 1 1 calc R U H29C H 0.2472 0.9338 0.0814 0.051 Uiso 1 1 calc R U C30 C 0.2167(2) 0.7408(2) 0.03263(15) 0.0403(6) Uani 1 1 d . . H30A H 0.2829 0.7673 0.0406 0.060 Uiso 1 1 calc R U H30B H 0.2106 0.7491 -0.0281 0.060 Uiso 1 1 calc R U H30C H 0.2308 0.6645 0.0564 0.060 Uiso 1 1 calc R U F1 F 0.28508(10) 0.22783(9) 0.35572(7) 0.0237(2) Uani 1 1 d . . F2 F 0.11249(11) 0.32890(10) 0.46485(8) 0.0314(3) Uani 1 1 d . . F3 F 0.11059(11) 0.52814(10) 0.49874(8) 0.0331(3) Uani 1 1 d . . F4 F 0.28960(11) 0.61747(9) 0.42412(8) 0.0291(3) Uani 1 1 d . . F5 F 0.45910(10) 0.52034(9) 0.31276(7) 0.0244(2) Uani 1 1 d . . F6 F 0.60707(10) 0.32572(9) 0.39029(7) 0.0241(2) Uani 1 1 d . . F7 F 0.69196(12) 0.17993(10) 0.51767(7) 0.0324(3) Uani 1 1 d . . F8 F 0.68639(12) -0.02897(10) 0.52821(8) 0.0367(3) Uani 1 1 d . . F9 F 0.59237(11) -0.08738(9) 0.40625(8) 0.0335(3) Uani 1 1 d . . F10 F 0.50673(11) 0.05476(9) 0.28041(8) 0.0282(3) Uani 1 1 d . . F11 F 0.62211(10) 0.15657(10) 0.14318(8) 0.0293(3) Uani 1 1 d . . F12 F 0.55376(13) 0.08866(12) 0.01892(9) 0.0443(4) Uani 1 1 d . . F13 F 0.32054(14) 0.15228(13) -0.00836(9) 0.0473(4) Uani 1 1 d . . F14 F 0.15952(12) 0.28630(11) 0.09246(8) 0.0370(3) Uani 1 1 d . . F15 F 0.22540(10) 0.36303(10) 0.21059(7) 0.0288(3) Uani 1 1 d . . F16 F 0.75474(10) 0.25934(9) 0.23961(7) 0.0250(2) Uani 1 1 d . . F17 F 0.87934(11) 0.37261(11) 0.12904(8) 0.0342(3) Uani 1 1 d . . F18 F 0.77008(13) 0.55030(12) 0.02742(9) 0.0422(3) Uani 1 1 d . . F19 F 0.52758(12) 0.60981(10) 0.03755(8) 0.0378(3) Uani 1 1 d . . F20 F 0.39955(10) 0.49618(9) 0.14729(7) 0.0275(3) Uani 1 1 d . . C31 C 0.37789(17) 0.37071(15) 0.32491(12) 0.0187(4) Uani 1 1 d . . C32 C 0.28778(18) 0.32662(15) 0.36919(12) 0.0203(4) Uani 1 1 d . . C33 C 0.19799(18) 0.37672(16) 0.42673(12) 0.0237(4) Uani 1 1 d . . C34 C 0.19729(18) 0.47609(17) 0.44457(12) 0.0239(4) Uani 1 1 d . . C35 C 0.28742(18) 0.52148(15) 0.40568(12) 0.0223(4) Uani 1 1 d . . C36 C 0.37408(17) 0.46920(15) 0.34742(12) 0.0202(4) Uani 1 1 d . . C37 C 0.55124(17) 0.20031(15) 0.32706(12) 0.0188(4) Uani 1 1 d . . C38 C 0.60116(17) 0.22359(15) 0.39146(12) 0.0203(4) Uani 1 1 d . . C39 C 0.64564(18) 0.15035(17) 0.45802(13) 0.0240(4) Uani 1 1 d . . C40 C 0.64337(19) 0.04424(16) 0.46365(13) 0.0266(4) Uani 1 1 d . . C41 C 0.59655(18) 0.01566(16) 0.40222(14) 0.0249(4) Uani 1 1 d . . C42 C 0.55260(17) 0.09261(16) 0.33625(13) 0.0212(4) Uani 1 1 d . . C43 C 0.42785(18) 0.25981(15) 0.18743(12) 0.0203(4) Uani 1 1 d . . C44 C 0.50474(19) 0.19172(16) 0.13297(13) 0.0249(4) Uani 1 1 d . . C45 C 0.4721(2) 0.15480(18) 0.06849(13) 0.0310(5) Uani 1 1 d . . C46 C 0.3555(2) 0.18626(19) 0.05450(13) 0.0327(5) Uani 1 1 d . . C47 C 0.27462(19) 0.25451(18) 0.10491(13) 0.0280(5) Uani 1 1 d . . C48 C 0.31181(19) 0.29140(16) 0.16813(12) 0.0236(4) Uani 1 1 d . . C49 C 0.56913(17) 0.37168(15) 0.20088(12) 0.0193(4) Uani 1 1 d . . C50 C 0.69195(18) 0.34641(15) 0.19236(12) 0.0208(4) Uani 1 1 d . . C51 C 0.75970(18) 0.40447(17) 0.13540(13) 0.0249(4) Uani 1 1 d . . C52 C 0.7052(2) 0.49396(18) 0.08339(13) 0.0288(5) Uani 1 1 d . . C53 C 0.5830(2) 0.52312(17) 0.08872(13) 0.0265(4) Uani 1 1 d . . C54 C 0.51941(18) 0.46245(16) 0.14594(12) 0.0224(4) Uani 1 1 d . . B1 B 0.4822(2) 0.30074(17) 0.25994(14) 0.0191(4) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01958(9) 0.02014(9) 0.01599(8) -0.00202(6) -0.00295(6) -0.00796(6) O1 0.0218(8) 0.0207(7) 0.0246(7) -0.0006(5) -0.0043(6) -0.0063(6) N1 0.0226(9) 0.0202(8) 0.0187(8) 0.0011(6) -0.0022(7) -0.0087(7) C1 0.0231(11) 0.0212(9) 0.0158(9) 0.0021(7) -0.0045(8) -0.0078(8) C2 0.0209(11) 0.0211(9) 0.0179(9) -0.0016(7) -0.0010(7) -0.0096(8) C3 0.0229(10) 0.0230(10) 0.0165(9) -0.0011(7) -0.0024(7) -0.0105(8) C4 0.0220(10) 0.0232(10) 0.0186(9) -0.0034(7) -0.0058(8) -0.0102(8) C5 0.0225(11) 0.0278(10) 0.0236(10) -0.0056(8) -0.0049(8) -0.0096(9) C6 0.0272(12) 0.0249(10) 0.0314(11) -0.0081(8) -0.0072(9) -0.0064(9) C7 0.0321(12) 0.0210(10) 0.0353(12) -0.0035(8) -0.0071(9) -0.0103(9) C8 0.0269(12) 0.0268(11) 0.0296(11) -0.0011(8) -0.0024(9) -0.0148(9) C9 0.0215(10) 0.0230(10) 0.0223(10) -0.0032(8) -0.0057(8) -0.0097(8) C10 0.0239(11) 0.0230(10) 0.0196(9) 0.0010(7) -0.0025(8) -0.0127(8) C11 0.0260(12) 0.0294(11) 0.0335(12) -0.0039(9) -0.0019(9) -0.0148(10) C12 0.0211(12) 0.0365(12) 0.0414(13) -0.0012(10) -0.0020(9) -0.0136(10) C13 0.0224(11) 0.0285(11) 0.0339(12) -0.0005(9) 0.0004(9) -0.0071(9) C14 0.0241(11) 0.0220(10) 0.0263(10) 0.0003(8) -0.0013(8) -0.0088(9) C15 0.0252(11) 0.0201(9) 0.0218(10) 0.0002(8) -0.0063(8) -0.0089(8) C16 0.0249(11) 0.0210(10) 0.0336(11) 0.0016(8) -0.0064(9) -0.0096(9) C17 0.0257(12) 0.0305(11) 0.0446(13) 0.0053(10) -0.0074(10) -0.0130(10) C18 0.0373(14) 0.0307(12) 0.0490(14) 0.0035(10) -0.0162(11) -0.0214(11) C19 0.0430(14) 0.0236(10) 0.0396(13) -0.0005(9) -0.0167(11) -0.0156(10) C20 0.0302(12) 0.0219(10) 0.0261(10) -0.0019(8) -0.0075(9) -0.0074(9) C21 0.0442(14) 0.0335(11) 0.0173(10) 0.0007(8) -0.0122(9) -0.0175(10) C22 0.0280(12) 0.0416(12) 0.0171(10) 0.0006(8) -0.0101(8) -0.0124(10) C23 0.0267(11) 0.0292(11) 0.0187(9) -0.0016(8) -0.0073(8) -0.0042(9) C24 0.0306(12) 0.0267(10) 0.0144(9) 0.0021(7) -0.0036(8) -0.0089(9) C25 0.0355(12) 0.0282(11) 0.0159(9) -0.0013(8) -0.0035(8) -0.0082(9) C26 0.0707(19) 0.0432(14) 0.0297(12) -0.0034(10) -0.0166(12) -0.0301(14) C27 0.0278(13) 0.0689(17) 0.0284(12) 0.0033(11) -0.0104(10) -0.0176(12) C28 0.0434(15) 0.0311(12) 0.0322(12) -0.0051(9) -0.0122(10) 0.0051(11) C29 0.0403(14) 0.0339(12) 0.0292(11) 0.0065(9) -0.0053(10) -0.0176(11) C30 0.0513(16) 0.0357(12) 0.0247(11) -0.0046(9) 0.0031(10) -0.0018(12) F1 0.0247(6) 0.0201(5) 0.0283(6) -0.0009(4) -0.0008(5) -0.0120(5) F2 0.0247(7) 0.0372(7) 0.0331(7) -0.0048(5) 0.0070(5) -0.0155(6) F3 0.0271(7) 0.0369(7) 0.0317(7) -0.0122(5) 0.0069(5) -0.0048(6) F4 0.0334(7) 0.0210(6) 0.0338(6) -0.0087(5) -0.0030(5) -0.0063(5) F5 0.0250(6) 0.0204(6) 0.0295(6) -0.0028(5) 0.0016(5) -0.0118(5) F6 0.0307(7) 0.0183(5) 0.0273(6) -0.0006(4) -0.0082(5) -0.0116(5) F7 0.0382(7) 0.0370(7) 0.0250(6) 0.0029(5) -0.0118(5) -0.0145(6) F8 0.0376(8) 0.0284(6) 0.0371(7) 0.0147(5) -0.0087(6) -0.0071(6) F9 0.0351(7) 0.0148(5) 0.0473(8) 0.0013(5) 0.0024(6) -0.0091(5) F10 0.0323(7) 0.0219(6) 0.0367(7) -0.0051(5) -0.0053(5) -0.0155(5) F11 0.0229(6) 0.0320(6) 0.0356(7) -0.0118(5) 0.0034(5) -0.0113(5) F12 0.0486(9) 0.0540(9) 0.0393(8) -0.0281(7) 0.0113(6) -0.0242(7) F13 0.0618(10) 0.0666(10) 0.0315(7) -0.0138(7) -0.0101(7) -0.0386(8) F14 0.0334(7) 0.0524(8) 0.0321(7) 0.0059(6) -0.0139(6) -0.0235(6) F15 0.0218(6) 0.0351(7) 0.0285(6) -0.0023(5) -0.0056(5) -0.0058(5) F16 0.0191(6) 0.0262(6) 0.0281(6) 0.0003(5) -0.0020(5) -0.0067(5) F17 0.0218(7) 0.0475(8) 0.0342(7) -0.0028(6) 0.0037(5) -0.0166(6) F18 0.0409(8) 0.0491(8) 0.0371(7) 0.0123(6) 0.0036(6) -0.0285(7) F19 0.0423(8) 0.0328(7) 0.0344(7) 0.0147(5) -0.0065(6) -0.0145(6) F20 0.0229(6) 0.0257(6) 0.0312(6) 0.0047(5) -0.0045(5) -0.0066(5) C31 0.0185(10) 0.0196(9) 0.0178(9) 0.0014(7) -0.0041(7) -0.0062(8) C32 0.0207(10) 0.0190(9) 0.0220(10) -0.0007(7) -0.0052(8) -0.0063(8) C33 0.0195(10) 0.0281(10) 0.0232(10) 0.0011(8) -0.0004(8) -0.0099(9) C34 0.0198(10) 0.0280(10) 0.0197(10) -0.0038(8) 0.0007(8) -0.0012(9) C35 0.0246(11) 0.0186(9) 0.0233(10) -0.0026(7) -0.0060(8) -0.0037(8) C36 0.0196(10) 0.0207(9) 0.0204(9) 0.0015(7) -0.0032(8) -0.0077(8) C37 0.0163(10) 0.0188(9) 0.0212(9) -0.0016(7) 0.0022(7) -0.0078(8) C38 0.0186(10) 0.0172(9) 0.0253(10) -0.0012(7) 0.0003(8) -0.0076(8) C39 0.0215(11) 0.0268(10) 0.0243(10) 0.0009(8) -0.0040(8) -0.0092(9) C40 0.0204(11) 0.0232(10) 0.0297(11) 0.0088(8) -0.0007(8) -0.0046(9) C41 0.0212(11) 0.0153(9) 0.0348(11) 0.0007(8) 0.0048(9) -0.0068(8) C42 0.0169(10) 0.0205(9) 0.0268(10) -0.0031(8) 0.0008(8) -0.0080(8) C43 0.0228(10) 0.0206(9) 0.0196(9) 0.0008(7) -0.0014(8) -0.0122(8) C44 0.0259(11) 0.0266(10) 0.0258(10) -0.0037(8) 0.0002(8) -0.0146(9) C45 0.0387(13) 0.0346(12) 0.0249(11) -0.0092(9) 0.0056(9) -0.0203(10) C46 0.0459(14) 0.0420(13) 0.0214(10) -0.0027(9) -0.0048(9) -0.0299(11) C47 0.0289(12) 0.0370(12) 0.0234(10) 0.0067(9) -0.0085(9) -0.0205(10) C48 0.0268(11) 0.0258(10) 0.0195(9) 0.0018(8) -0.0010(8) -0.0133(9) C49 0.0223(10) 0.0194(9) 0.0187(9) -0.0048(7) -0.0007(8) -0.0093(8) C50 0.0249(11) 0.0205(9) 0.0188(9) -0.0031(7) -0.0025(8) -0.0090(8) C51 0.0201(11) 0.0336(11) 0.0251(10) -0.0075(8) 0.0023(8) -0.0143(9) C52 0.0363(13) 0.0336(11) 0.0206(10) 0.0011(8) 0.0036(9) -0.0229(10) C53 0.0338(12) 0.0248(10) 0.0209(10) 0.0034(8) -0.0039(9) -0.0118(9) C54 0.0224(11) 0.0239(10) 0.0218(10) -0.0024(8) -0.0007(8) -0.0093(9) B1 0.0183(11) 0.0173(10) 0.0231(11) -0.0013(8) -0.0026(9) -0.0078(9) 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' F F 0.0727 0.0534 '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' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 Rh1 C23 115.14(7) N1 Rh1 O1 82.21(6) C23 Rh1 O1 161.95(7) N1 Rh1 C2 93.17(7) C23 Rh1 C2 106.80(8) O1 Rh1 C2 65.33(6) N1 Rh1 C22 153.09(7) C23 Rh1 C22 38.78(8) O1 Rh1 C22 124.48(7) C2 Rh1 C22 101.06(8) N1 Rh1 C24 90.51(7) C23 Rh1 C24 38.67(8) O1 Rh1 C24 153.41(7) C2 Rh1 C24 140.94(8) C22 Rh1 C24 64.14(8) N1 Rh1 C21 138.34(8) C23 Rh1 C21 64.50(8) O1 Rh1 C21 106.46(7) C2 Rh1 C21 127.84(8) C22 Rh1 C21 38.46(9) C24 Rh1 C21 63.34(8) N1 Rh1 C25 101.90(7) C23 Rh1 C25 64.56(8) O1 Rh1 C25 118.81(7) C2 Rh1 C25 164.74(8) C22 Rh1 C25 64.14(8) C24 Rh1 C25 37.90(8) C21 Rh1 C25 37.77(8) N1 Rh1 C1 103.60(6) C23 Rh1 C1 130.00(8) O1 Rh1 C1 34.46(6) C2 Rh1 C1 38.33(7) C22 Rh1 C1 101.69(7) C24 Rh1 C1 165.81(8) C21 Rh1 C1 105.49(7) C25 Rh1 C1 137.05(7) C1 O1 Rh1 75.49(10) C14 N1 C10 118.38(17) C14 N1 Rh1 113.10(13) C10 N1 Rh1 127.43(14) O1 C1 C2 116.53(17) O1 C1 C15 118.68(17) C2 C1 C15 124.43(18) O1 C1 Rh1 70.05(10) C2 C1 Rh1 68.51(10) C15 C1 Rh1 126.47(13) C1 C2 C3 123.38(18) C1 C2 Rh1 73.17(11) C3 C2 Rh1 111.55(13) C1 C2 H2 115.2(11) C3 C2 H2 112.8(11) Rh1 C2 H2 114.3(11) C4 C3 C2 110.31(15) C4 C3 H3A 109.6 C2 C3 H3A 109.6 C4 C3 H3B 109.6 C2 C3 H3B 109.6 H3A C3 H3B 108.1 C5 C4 C9 117.95(18) C5 C4 C3 120.06(17) C9 C4 C3 121.99(17) C6 C5 C4 121.72(19) C6 C5 H5 119.1 C4 C5 H5 119.1 C7 C6 C5 119.9(2) C7 C6 H6 120.1 C5 C6 H6 120.1 C8 C7 C6 119.50(19) C8 C7 H7 120.3 C6 C7 H7 120.3 C7 C8 C9 120.93(19) C7 C8 H8 119.5 C9 C8 H8 119.5 C8 C9 C4 119.96(18) C8 C9 C10 118.30(18) C4 C9 C10 121.54(17) N1 C10 C11 120.65(19) N1 C10 C9 119.97(17) C11 C10 C9 119.38(17) C12 C11 C10 120.50(19) C12 C11 H11 119.7 C10 C11 H11 119.7 C11 C12 C13 118.7(2) C11 C12 H12 120.7 C13 C12 H12 120.7 C12 C13 C14 118.7(2) C12 C13 H13 120.6 C14 C13 H13 120.6 N1 C14 C13 122.98(19) N1 C14 H14 118.5 C13 C14 H14 118.5 C16 C15 C20 119.19(18) C16 C15 C1 121.75(18) C20 C15 C1 118.97(19) C17 C16 C15 120.4(2) C17 C16 H16 119.8 C15 C16 H16 119.8 C18 C17 C16 119.9(2) C18 C17 H17 120.1 C16 C17 H17 120.1 C19 C18 C17 119.9(2) C19 C18 H18 120.0 C17 C18 H18 120.0 C18 C19 C20 120.7(2) C18 C19 H19 119.6 C20 C19 H19 119.7 C19 C20 C15 119.8(2) C19 C20 H20 120.1 C15 C20 H20 120.1 C25 C21 C22 108.59(18) C25 C21 C26 124.5(2) C22 C21 C26 126.9(2) C25 C21 Rh1 71.76(11) C22 C21 Rh1 69.67(11) C26 C21 Rh1 126.48(15) C23 C22 C21 107.73(18) C23 C22 C27 125.3(2) C21 C22 C27 126.8(2) C23 C22 Rh1 69.77(11) C21 C22 Rh1 71.87(12) C27 C22 Rh1 126.96(15) C24 C23 C22 107.33(18) C24 C23 C28 126.6(2) C22 C23 C28 125.9(2) C24 C23 Rh1 71.85(11) C22 C23 Rh1 71.45(12) C28 C23 Rh1 125.85(14) C25 C24 C23 109.19(18) C25 C24 C29 126.1(2) C23 C24 C29 124.68(19) C25 C24 Rh1 72.46(11) C23 C24 Rh1 69.48(11) C29 C24 Rh1 125.68(14) C24 C25 C21 107.16(19) C24 C25 C30 125.9(2) C21 C25 C30 126.9(2) C24 C25 Rh1 69.65(11) C21 C25 Rh1 70.48(11) C30 C25 Rh1 126.06(16) C21 C26 H26A 109.5 C21 C26 H26B 109.5 H26A C26 H26B 109.5 C21 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C22 C27 H27A 109.5 C22 C27 H27B 109.5 H27A C27 H27B 109.5 C22 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C23 C28 H28A 109.5 C23 C28 H28B 109.5 H28A C28 H28B 109.5 C23 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C24 C29 H29A 109.5 C24 C29 H29B 109.5 H29A C29 H29B 109.5 C24 C29 H29C 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C25 C30 H30A 109.5 C25 C30 H30B 109.5 H30A C30 H30B 109.5 C25 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C36 C31 C32 113.56(17) C36 C31 B1 126.55(17) C32 C31 B1 119.65(16) F1 C32 C33 116.25(16) F1 C32 C31 119.22(17) C33 C32 C31 124.53(18) F2 C33 C34 120.69(18) F2 C33 C32 120.28(18) C34 C33 C32 119.02(18) F3 C34 C35 120.12(18) F3 C34 C33 120.82(18) C35 C34 C33 119.06(18) F4 C35 C34 119.75(18) F4 C35 C36 120.46(17) C34 C35 C36 119.78(18) F5 C36 C35 115.30(16) F5 C36 C31 120.75(17) C35 C36 C31 123.94(18) C42 C37 C38 112.49(18) C42 C37 B1 127.60(17) C38 C37 B1 119.23(16) F6 C38 C39 115.73(17) F6 C38 C37 119.12(17) C39 C38 C37 125.15(17) F7 C39 C38 121.22(17) F7 C39 C40 119.46(18) C38 C39 C40 119.32(19) F8 C40 C41 120.99(18) F8 C40 C39 120.43(19) C41 C40 C39 118.58(19) F9 C41 C40 119.99(19) F9 C41 C42 120.05(19) C40 C41 C42 119.96(18) F10 C42 C37 121.16(18) F10 C42 C41 114.33(17) C37 C42 C41 124.49(19) C48 C43 C44 112.52(18) C48 C43 B1 127.99(18) C44 C43 B1 119.31(17) F11 C44 C45 115.91(18) F11 C44 C43 118.86(17) C45 C44 C43 125.2(2) F12 C45 C46 119.94(19) F12 C45 C44 120.7(2) C46 C45 C44 119.3(2) F13 C46 C47 120.2(2) F13 C46 C45 120.9(2) C47 C46 C45 118.85(19) F14 C47 C46 119.90(19) F14 C47 C48 120.2(2) C46 C47 C48 119.9(2) F15 C48 C47 114.57(18) F15 C48 C43 121.32(17) C47 C48 C43 124.1(2) C50 C49 C54 113.06(17) C50 C49 B1 127.36(17) C54 C49 B1 119.27(17) F16 C50 C49 120.85(17) F16 C50 C51 115.03(18) C49 C50 C51 124.11(19) F17 C51 C52 119.44(18) F17 C51 C50 120.53(19) C52 C51 C50 120.02(19) F18 C52 C51 120.5(2) F18 C52 C53 120.9(2) C51 C52 C53 118.62(18) F19 C53 C54 121.0(2) F19 C53 C52 119.70(18) C54 C53 C52 119.28(19) F20 C54 C53 115.77(18) F20 C54 C49 119.32(17) C53 C54 C49 124.90(19) C31 B1 C49 113.38(15) C31 B1 C37 101.43(15) C49 B1 C37 114.14(16) C31 B1 C43 112.85(16) C49 B1 C43 102.21(15) C37 B1 C43 113.33(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Rh1 N1 2.1334(16) Rh1 C23 2.149(2) Rh1 O1 2.1588(13) Rh1 C2 2.1614(19) Rh1 C22 2.171(2) Rh1 C24 2.1801(19) Rh1 C21 2.200(2) Rh1 C25 2.217(2) Rh1 C1 2.2235(18) O1 C1 1.300(2) N1 C14 1.345(3) N1 C10 1.358(2) C1 C2 1.441(3) C1 C15 1.485(3) C2 C3 1.517(3) C2 H2 1.03(2) C3 C4 1.513(3) C3 H3A 0.9900 C3 H3B 0.9900 C4 C5 1.392(3) C4 C9 1.406(3) C5 C6 1.391(3) C5 H5 0.9500 C6 C7 1.383(3) C6 H6 0.9500 C7 C8 1.383(3) C7 H7 0.9500 C8 C9 1.400(3) C8 H8 0.9500 C9 C10 1.477(3) C10 C11 1.391(3) C11 C12 1.375(3) C11 H11 0.9500 C12 C13 1.382(3) C12 H12 0.9500 C13 C14 1.383(3) C13 H13 0.9500 C14 H14 0.9500 C15 C16 1.393(3) C15 C20 1.404(3) C16 C17 1.391(3) C16 H16 0.9500 C17 C18 1.390(3) C17 H17 0.9500 C18 C19 1.382(4) C18 H18 0.9500 C19 C20 1.385(3) C19 H19 0.9500 C20 H20 0.9500 C21 C25 1.430(3) C21 C22 1.440(3) C21 C26 1.497(3) C22 C23 1.434(3) C22 C27 1.493(3) C23 C24 1.433(3) C23 C28 1.494(3) C24 C25 1.428(3) C24 C29 1.495(3) C25 C30 1.507(3) C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 F1 C32 1.358(2) F2 C33 1.346(2) F3 C34 1.336(2) F4 C35 1.349(2) F5 C36 1.356(2) F6 C38 1.354(2) F7 C39 1.348(2) F8 C40 1.344(2) F9 C41 1.352(2) F10 C42 1.356(2) F11 C44 1.362(2) F12 C45 1.350(3) F13 C46 1.346(2) F14 C47 1.345(3) F15 C48 1.353(2) F16 C50 1.351(2) F17 C51 1.349(2) F18 C52 1.343(2) F19 C53 1.349(2) F20 C54 1.358(2) C31 C36 1.386(3) C31 C32 1.390(3) C31 B1 1.646(3) C32 C33 1.379(3) C33 C34 1.378(3) C34 C35 1.376(3) C35 C36 1.378(3) C37 C42 1.385(3) C37 C38 1.398(3) C37 B1 1.656(3) C38 C39 1.373(3) C39 C40 1.382(3) C40 C41 1.369(3) C41 C42 1.387(3) C43 C48 1.390(3) C43 C44 1.390(3) C43 B1 1.660(3) C44 C45 1.376(3) C45 C46 1.370(3) C46 C47 1.369(3) C47 C48 1.387(3) C49 C50 1.384(3) C49 C54 1.393(3) C49 B1 1.653(3) C50 C51 1.385(3) C51 C52 1.375(3) C52 C53 1.378(3) C53 C54 1.377(3) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion Rh1 O1 C1 C2 -51.91(15) Rh1 O1 C1 C15 121.47(16) O1 C1 C2 C3 -52.4(3) C15 C1 C2 C3 134.6(2) Rh1 C1 C2 C3 -105.08(18) O1 C1 C2 Rh1 52.66(15) C15 C1 C2 Rh1 -120.30(18) C1 C2 C3 C4 150.26(18) Rh1 C2 C3 C4 66.72(18) C2 C3 C4 C5 88.5(2) C2 C3 C4 C9 -91.0(2) C9 C4 C5 C6 1.0(3) C3 C4 C5 C6 -178.53(18) C4 C5 C6 C7 -1.9(3) C5 C6 C7 C8 1.0(3) C6 C7 C8 C9 0.8(3) C7 C8 C9 C4 -1.8(3) C7 C8 C9 C10 -176.75(19) C5 C4 C9 C8 0.9(3) C3 C4 C9 C8 -179.64(18) C5 C4 C9 C10 175.69(17) C3 C4 C9 C10 -4.8(3) C14 N1 C10 C11 2.5(3) Rh1 N1 C10 C11 -164.71(15) C14 N1 C10 C9 -176.48(17) Rh1 N1 C10 C9 16.4(2) C8 C9 C10 N1 -136.21(19) C4 C9 C10 N1 48.9(3) C8 C9 C10 C11 44.8(3) C4 C9 C10 C11 -130.0(2) N1 C10 C11 C12 0.1(3) C9 C10 C11 C12 179.0(2) C10 C11 C12 C13 -1.8(3) C11 C12 C13 C14 0.9(3) C10 N1 C14 C13 -3.4(3) Rh1 N1 C14 C13 165.50(16) C12 C13 C14 N1 1.8(3) O1 C1 C15 C16 175.08(18) C2 C1 C15 C16 -12.1(3) Rh1 C1 C15 C16 -99.5(2) O1 C1 C15 C20 -1.3(3) C2 C1 C15 C20 171.49(18) Rh1 C1 C15 C20 84.1(2) C20 C15 C16 C17 -2.6(3) C1 C15 C16 C17 -178.99(19) C15 C16 C17 C18 1.4(3) C16 C17 C18 C19 0.7(4) C17 C18 C19 C20 -1.7(4) C18 C19 C20 C15 0.5(3) C16 C15 C20 C19 1.6(3) C1 C15 C20 C19 178.13(18) C25 C21 C22 C23 -0.6(2) C26 C21 C22 C23 -178.1(2) Rh1 C21 C22 C23 60.88(13) C25 C21 C22 C27 175.4(2) C26 C21 C22 C27 -2.1(3) Rh1 C21 C22 C27 -123.0(2) C25 C21 C22 Rh1 -61.52(14) C26 C21 C22 Rh1 121.0(2) C21 C22 C23 C24 1.1(2) C27 C22 C23 C24 -175.06(19) Rh1 C22 C23 C24 63.32(14) C21 C22 C23 C28 176.46(19) C27 C22 C23 C28 0.3(3) Rh1 C22 C23 C28 -121.3(2) C21 C22 C23 Rh1 -62.23(14) C27 C22 C23 Rh1 121.6(2) C22 C23 C24 C25 -1.2(2) C28 C23 C24 C25 -176.48(19) Rh1 C23 C24 C25 61.90(14) C22 C23 C24 C29 177.05(19) C28 C23 C24 C29 1.7(3) Rh1 C23 C24 C29 -119.9(2) C22 C23 C24 Rh1 -63.06(13) C28 C23 C24 Rh1 121.6(2) C23 C24 C25 C21 0.8(2) C29 C24 C25 C21 -177.41(19) Rh1 C24 C25 C21 60.82(14) C23 C24 C25 C30 179.5(2) C29 C24 C25 C30 1.3(3) Rh1 C24 C25 C30 -120.4(2) C23 C24 C25 Rh1 -60.05(14) C29 C24 C25 Rh1 121.8(2) C22 C21 C25 C24 -0.1(2) C26 C21 C25 C24 177.5(2) Rh1 C21 C25 C24 -60.29(14) C22 C21 C25 C30 -178.8(2) C26 C21 C25 C30 -1.2(3) Rh1 C21 C25 C30 121.0(2) C22 C21 C25 Rh1 60.21(14) C26 C21 C25 Rh1 -122.2(2) C36 C31 C32 F1 -176.97(16) B1 C31 C32 F1 -2.3(3) C36 C31 C32 C33 3.6(3) B1 C31 C32 C33 178.22(18) F1 C32 C33 F2 -1.3(3) C31 C32 C33 F2 178.12(18) F1 C32 C33 C34 178.58(18) C31 C32 C33 C34 -2.0(3) F2 C33 C34 F3 -1.4(3) C32 C33 C34 F3 178.73(18) F2 C33 C34 C35 178.70(18) C32 C33 C34 C35 -1.2(3) F3 C34 C35 F4 1.7(3) C33 C34 C35 F4 -178.32(18) F3 C34 C35 C36 -177.52(18) C33 C34 C35 C36 2.4(3) F4 C35 C36 F5 0.9(3) C34 C35 C36 F5 -179.87(17) F4 C35 C36 C31 -179.84(18) C34 C35 C36 C31 -0.6(3) C32 C31 C36 F5 176.96(16) B1 C31 C36 F5 2.8(3) C32 C31 C36 C35 -2.3(3) B1 C31 C36 C35 -176.48(18) C42 C37 C38 F6 179.32(16) B1 C37 C38 F6 -9.4(3) C42 C37 C38 C39 -1.0(3) B1 C37 C38 C39 170.28(19) F6 C38 C39 F7 -0.1(3) C37 C38 C39 F7 -179.77(18) F6 C38 C39 C40 -179.74(17) C37 C38 C39 C40 0.6(3) F7 C39 C40 F8 0.3(3) C38 C39 C40 F8 179.99(18) F7 C39 C40 C41 -179.65(18) C38 C39 C40 C41 0.0(3) F8 C40 C41 F9 0.5(3) C39 C40 C41 F9 -179.58(18) F8 C40 C41 C42 179.95(18) C39 C40 C41 C42 -0.1(3) C38 C37 C42 F10 179.23(17) B1 C37 C42 F10 8.9(3) C38 C37 C42 C41 0.9(3) B1 C37 C42 C41 -169.45(19) F9 C41 C42 F10 0.6(3) C40 C41 C42 F10 -178.86(18) F9 C41 C42 C37 179.06(18) C40 C41 C42 C37 -0.4(3) C48 C43 C44 F11 178.37(16) B1 C43 C44 F11 2.9(3) C48 C43 C44 C45 -2.3(3) B1 C43 C44 C45 -177.74(19) F11 C44 C45 F12 -0.6(3) C43 C44 C45 F12 -179.98(19) F11 C44 C45 C46 179.73(18) C43 C44 C45 C46 0.4(3) F12 C45 C46 F13 -0.1(3) C44 C45 C46 F13 179.57(19) F12 C45 C46 C47 -179.15(19) C44 C45 C46 C47 0.5(3) F13 C46 C47 F14 1.1(3) C45 C46 C47 F14 -179.85(19) F13 C46 C47 C48 -178.34(18) C45 C46 C47 C48 0.7(3) F14 C47 C48 F15 -3.0(3) C46 C47 C48 F15 176.43(18) F14 C47 C48 C43 177.58(18) C46 C47 C48 C43 -3.0(3) C44 C43 C48 F15 -175.81(17) B1 C43 C48 F15 -0.8(3) C44 C43 C48 C47 3.6(3) B1 C43 C48 C47 178.55(18) C54 C49 C50 F16 -178.62(16) B1 C49 C50 F16 -5.1(3) C54 C49 C50 C51 0.0(3) B1 C49 C50 C51 173.49(18) F16 C50 C51 F17 0.8(3) C49 C50 C51 F17 -177.87(17) F16 C50 C51 C52 179.28(17) C49 C50 C51 C52 0.6(3) F17 C51 C52 F18 -0.9(3) C50 C51 C52 F18 -179.43(18) F17 C51 C52 C53 177.77(18) C50 C51 C52 C53 -0.7(3) F18 C52 C53 F19 -0.5(3) C51 C52 C53 F19 -179.14(18) F18 C52 C53 C54 178.98(19) C51 C52 C53 C54 0.3(3) F19 C53 C54 F20 -0.4(3) C52 C53 C54 F20 -179.87(18) F19 C53 C54 C49 179.75(18) C52 C53 C54 C49 0.3(3) C50 C49 C54 F20 179.75(16) B1 C49 C54 F20 5.6(3) C50 C49 C54 C53 -0.4(3) B1 C49 C54 C53 -174.54(18) C36 C31 B1 C49 -15.6(3) C32 C31 B1 C49 170.49(17) C36 C31 B1 C37 107.2(2) C32 C31 B1 C37 -66.7(2) C36 C31 B1 C43 -131.24(19) C32 C31 B1 C43 54.9(2) C50 C49 B1 C31 126.4(2) C54 C49 B1 C31 -60.4(2) C50 C49 B1 C37 10.9(3) C54 C49 B1 C37 -175.90(16) C50 C49 B1 C43 -111.8(2) C54 C49 B1 C43 61.4(2) C42 C37 B1 C31 111.1(2) C38 C37 B1 C31 -58.7(2) C42 C37 B1 C49 -126.6(2) C38 C37 B1 C49 63.6(2) C42 C37 B1 C43 -10.2(3) C38 C37 B1 C43 -179.95(17) C48 C43 B1 C31 11.0(3) C44 C43 B1 C31 -174.28(17) C48 C43 B1 C49 -111.1(2) C44 C43 B1 C49 63.6(2) C48 C43 B1 C37 125.6(2) C44 C43 B1 C37 -59.7(2)