#------------------------------------------------------------------------------ #$Date: 2020-08-20 04:49:31 +0300 (Thu, 20 Aug 2020) $ #$Revision: 255468 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705220.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_7705220 loop_ _publ_author_name 'Kataoka, Yusuke' 'Kohara, Yoshihiro' 'Yano, Natsumi' 'Kawamoto, Tatsuya' _publ_section_title ; Unique Vapochromism of a Paddlewheel-type Dirhodium Complex Accompanied by Dynamic Structural and Phase Transitions ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02672G _journal_year 2020 _chemical_formula_sum 'C58 H98 N2 O16 Rh4' _chemical_formula_weight 1491.02 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-07-23 deposited with the CCDC. 2020-08-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 105.984(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 30.1315(6) _cell_length_b 10.23380(18) _cell_length_c 22.3582(4) _cell_measurement_reflns_used 27922 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 31.34 _cell_measurement_theta_min 1.90 _cell_volume 6627.8(2) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT Version 2018/2 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 7.111 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_unetI/netI 0.0289 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 40020 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 24.250 _diffrn_reflns_theta_max 24.250 _diffrn_reflns_theta_min 3.201 _diffrn_source 'Varimax Mo rotating anode' _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 3072 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.191 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 721 _refine_ls_number_reflns 10661 _refine_ls_number_restraints 23 _refine_ls_restrained_S_all 1.162 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0442 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+27.3344P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.1016 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9264 _reflns_number_total 10661 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02672g2.cif _cod_data_source_block shelxl _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7705220 _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_res_file ; shelxl.res created by SHELXL-2014/7 TITL xcalibur CELL 0.71075 30.13150 10.23380 22.35820 90.00000 105.98400 90.00000 ZERR 4 0.00060 0.00018 0.00040 0.00000 0.00200 0.00000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H N O RH UNIT 232 392 8 64 16 SHEL 6.790236 0.865248 L.S. 10 FMAP 2 PLAN 25 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -123.0 SAME 0.06 C39 C40 SAME 0.04 C45 C46 SIMU 0.01 C44 C45 C46 RIGU 0.01 C44 C45 C46 ACTA WGHT 0.029900 27.334400 FVAR 0.21531 RH1 5 0.756392 0.221944 0.465359 11.00000 0.03547 0.01690 = 0.01823 0.00159 0.00574 0.00025 RH2 5 0.768321 0.436865 0.431121 11.00000 0.03204 0.01799 = 0.01968 0.00281 0.00529 -0.00021 RH3 5 0.729111 0.583992 0.289633 11.00000 0.03370 0.01849 = 0.01927 0.00288 0.00481 -0.00200 RH4 5 0.741299 0.797794 0.254423 11.00000 0.03324 0.01743 = 0.01843 0.00224 0.00586 -0.00038 O1 4 0.700549 0.292347 0.489892 11.00000 0.03732 0.02514 = 0.02677 0.00523 0.00985 0.00045 O2 4 0.710217 0.493420 0.453978 11.00000 0.03905 0.02085 = 0.03201 0.00286 0.01273 0.00507 O3 4 0.713145 0.189104 0.378489 11.00000 0.04191 0.02202 = 0.02120 0.00172 0.00417 -0.00402 O4 4 0.727395 0.387556 0.345266 11.00000 0.03782 0.02096 = 0.02113 0.00656 0.00631 -0.00053 O5 4 0.812308 0.163486 0.438327 11.00000 0.04314 0.02273 = 0.03397 0.00430 0.01233 0.00676 O6 4 0.825255 0.368482 0.409423 11.00000 0.03651 0.02959 = 0.03095 0.00797 0.00995 0.00479 O7 4 0.798950 0.269132 0.550278 11.00000 0.04061 0.01858 = 0.02325 0.00234 0.00286 -0.00168 O8 4 0.807764 0.475523 0.519240 11.00000 0.04343 0.02433 = 0.02102 0.00222 0.00201 -0.00497 O9 4 0.672061 0.653542 0.311095 11.00000 0.03559 0.02841 = 0.03237 0.00918 0.01132 -0.00070 O10 4 0.686843 0.857839 0.284680 11.00000 0.03774 0.02784 = 0.02907 0.00465 0.01204 0.00232 O11 4 0.688896 0.544337 0.202135 11.00000 0.04301 0.02388 = 0.02406 -0.00034 0.00320 -0.00883 O12 4 0.696724 0.750336 0.170555 11.00000 0.04026 0.02578 = 0.01967 0.00424 0.00417 0.00000 O13 4 0.786541 0.526065 0.265651 11.00000 0.04237 0.01928 = 0.02808 0.00521 0.01150 0.00400 O14 4 0.795083 0.724424 0.226305 11.00000 0.03697 0.02133 = 0.02427 0.00384 0.01060 0.00066 O15 4 0.770371 0.634745 0.374993 11.00000 0.03809 0.02201 = 0.02072 0.00494 0.00546 -0.00089 O16 4 0.786191 0.829237 0.339794 11.00000 0.04264 0.01914 = 0.02313 -0.00036 0.00372 -0.00351 N1 3 0.746605 0.020872 0.493850 11.00000 0.04233 0.01701 = 0.02478 0.00249 0.00994 -0.00230 N2 3 0.750384 0.997711 0.225095 11.00000 0.03277 0.01941 = 0.02259 -0.00056 0.00926 0.00213 C1 1 0.688783 0.410349 0.477346 11.00000 0.03686 0.03307 = 0.02264 0.00172 0.00857 0.00400 C2 1 0.645854 0.457743 0.492784 11.00000 0.05073 0.05384 = 0.04898 0.01959 0.02645 0.01646 AFIX 23 H2A 2 0.627695 0.380481 0.498556 11.00000 -1.20000 H2B 2 0.655341 0.504448 0.533081 11.00000 -1.20000 AFIX 0 C3 1 0.615434 0.544518 0.446790 11.00000 0.04657 0.07699 = 0.06327 0.02998 0.02162 0.01786 AFIX 23 H3A 2 0.604800 0.496802 0.406874 11.00000 -1.20000 H3B 2 0.633749 0.620428 0.439788 11.00000 -1.20000 AFIX 0 C4 1 0.573100 0.595178 0.464679 11.00000 0.04630 0.09338 = 0.06013 0.02225 0.02364 0.01171 AFIX 23 H4A 2 0.553375 0.519194 0.467258 11.00000 -1.20000 H4B 2 0.583815 0.633064 0.506959 11.00000 -1.20000 AFIX 0 C5 1 0.544661 0.690933 0.424856 11.00000 0.07298 0.07651 = 0.11383 0.01436 0.04925 0.01756 AFIX 23 H5A 2 0.532901 0.653213 0.382671 11.00000 -1.20000 H5B 2 0.564039 0.767316 0.421652 11.00000 -1.20000 AFIX 0 C6 1 0.504372 0.737090 0.446449 11.00000 0.06788 0.07691 = 0.10685 -0.00510 0.04316 0.00808 AFIX 33 H6A 2 0.486766 0.801821 0.417045 11.00000 -1.20000 H6B 2 0.484429 0.662652 0.448679 11.00000 -1.20000 H6C 2 0.515616 0.776934 0.487722 11.00000 -1.20000 AFIX 0 C7 1 0.706050 0.277449 0.337959 11.00000 0.03329 0.02025 = 0.02669 0.00186 0.01026 0.00099 C8 1 0.668339 0.259251 0.279773 11.00000 0.04058 0.02534 = 0.02112 0.00094 0.00382 -0.00497 AFIX 23 H8A 2 0.664006 0.164977 0.269974 11.00000 -1.20000 H8B 2 0.676516 0.303086 0.244783 11.00000 -1.20000 AFIX 0 C9 1 0.623445 0.317581 0.288086 11.00000 0.04391 0.04991 = 0.03912 -0.00417 0.00489 -0.00276 AFIX 23 H9A 2 0.616454 0.275488 0.324316 11.00000 -1.20000 H9B 2 0.628212 0.411951 0.297383 11.00000 -1.20000 AFIX 0 C10 1 0.582347 0.300918 0.231694 11.00000 0.04841 0.05451 = 0.06243 -0.00617 -0.00388 0.00144 AFIX 23 H10A 2 0.576896 0.206356 0.223557 11.00000 -1.20000 H10B 2 0.590006 0.339425 0.195147 11.00000 -1.20000 AFIX 0 C11 1 0.537940 0.363018 0.237875 11.00000 0.04644 0.06787 = 0.08267 -0.00838 0.00395 -0.00539 AFIX 23 H11A 2 0.511972 0.334719 0.202529 11.00000 -1.20000 H11B 2 0.531741 0.331607 0.276677 11.00000 -1.20000 AFIX 0 C12 1 0.540045 0.507277 0.239019 11.00000 0.05589 0.07497 = 0.16344 -0.02737 -0.00546 0.00088 AFIX 33 H12A 2 0.510754 0.542470 0.243040 11.00000 -1.20000 H12B 2 0.565274 0.535963 0.274467 11.00000 -1.20000 H12C 2 0.545502 0.539076 0.200308 11.00000 -1.20000 AFIX 0 C13 1 0.835013 0.248742 0.417871 11.00000 0.03773 0.03595 = 0.02599 0.00133 0.00679 0.00425 C14 1 0.878577 0.201676 0.403535 11.00000 0.05125 0.04585 = 0.04623 0.00636 0.02324 0.01491 AFIX 23 H14A 2 0.888814 0.267735 0.377830 11.00000 -1.20000 H14B 2 0.872047 0.119500 0.379334 11.00000 -1.20000 AFIX 0 C15 1 0.916945 0.178191 0.463137 11.00000 0.05560 0.08802 = 0.10202 0.00392 0.02704 0.01495 AFIX 23 H15A 2 0.905506 0.116945 0.489796 11.00000 -1.20000 H15B 2 0.943194 0.135570 0.452297 11.00000 -1.20000 AFIX 0 C16 1 0.934175 0.300103 0.499941 11.00000 0.06041 0.07909 = 0.07029 0.00556 0.01498 0.01138 AFIX 23 H16A 2 0.945964 0.360876 0.473436 11.00000 -1.20000 H16B 2 0.907839 0.343309 0.510300 11.00000 -1.20000 AFIX 0 C17 1 0.971498 0.277094 0.558953 11.00000 0.07030 0.13621 = 0.09333 0.01716 0.01120 0.00343 AFIX 23 H17A 2 0.959039 0.221795 0.586877 11.00000 -1.20000 H17B 2 0.996938 0.228223 0.549055 11.00000 -1.20000 AFIX 0 C18 1 0.990368 0.398176 0.592233 11.00000 0.08621 0.11854 = 0.09531 0.00500 0.01425 -0.02234 AFIX 33 H18A 2 1.014496 0.376034 0.630193 11.00000 -1.20000 H18B 2 1.003538 0.452654 0.565367 11.00000 -1.20000 H18C 2 0.965597 0.446218 0.603231 11.00000 -1.20000 AFIX 0 C19 1 0.815222 0.384245 0.558651 11.00000 0.03533 0.02188 = 0.02414 0.00146 0.00756 0.00147 C20 1 0.847972 0.411829 0.622544 11.00000 0.04137 0.02740 = 0.02292 -0.00056 0.00363 -0.00509 AFIX 23 H20A 2 0.878550 0.374281 0.624102 11.00000 -1.20000 H20B 2 0.836328 0.366100 0.654208 11.00000 -1.20000 AFIX 0 C21 1 0.854290 0.556300 0.640080 11.00000 0.05103 0.02348 = 0.03550 0.00183 0.00372 -0.00438 AFIX 23 H21A 2 0.859874 0.605694 0.604773 11.00000 -1.20000 H21B 2 0.825450 0.589907 0.647485 11.00000 -1.20000 AFIX 0 C22 1 0.893982 0.580275 0.697570 11.00000 0.04216 0.02923 = 0.03077 -0.00278 0.00574 -0.00977 AFIX 23 H22A 2 0.901221 0.674818 0.700240 11.00000 -1.20000 H22B 2 0.921541 0.533495 0.692722 11.00000 -1.20000 AFIX 0 C23 1 0.884935 0.536953 0.758901 11.00000 0.04230 0.03946 = 0.03302 -0.00359 0.00726 -0.00811 AFIX 23 H23A 2 0.857544 0.583657 0.764366 11.00000 -1.20000 H23B 2 0.878102 0.442177 0.756970 11.00000 -1.20000 AFIX 0 C24 1 0.925671 0.564162 0.813896 11.00000 0.06376 0.05562 = 0.03201 -0.00321 0.00671 -0.01804 AFIX 33 H24A 2 0.918664 0.535323 0.852095 11.00000 -1.20000 H24B 2 0.952712 0.516738 0.809007 11.00000 -1.20000 H24C 2 0.932165 0.658142 0.816399 11.00000 -1.20000 AFIX 0 C25 1 0.764710 -0.018843 0.552375 11.00000 0.06217 0.03137 = 0.02174 -0.00113 0.01212 -0.00935 AFIX 43 H25 2 0.780084 0.043165 0.582639 11.00000 -1.20000 AFIX 0 C26 1 0.761905 -0.145912 0.570346 11.00000 0.07176 0.02949 = 0.02124 0.00451 0.00957 -0.00029 AFIX 43 H26 2 0.775055 -0.171164 0.612395 11.00000 -1.20000 AFIX 0 C27 1 0.740123 -0.235287 0.527380 11.00000 0.05536 0.02341 = 0.03250 0.00726 0.01675 0.00139 AFIX 43 H27 2 0.738140 -0.323996 0.538898 11.00000 -1.20000 AFIX 0 C28 1 0.720968 -0.195817 0.466991 11.00000 0.04400 0.02565 = 0.02862 -0.00445 0.01328 -0.00520 AFIX 43 H28 2 0.705054 -0.256477 0.436399 11.00000 -1.20000 AFIX 0 C29 1 0.725161 -0.067818 0.451580 11.00000 0.04330 0.02514 = 0.02236 0.00111 0.00786 0.00127 AFIX 43 H29 2 0.712490 -0.041014 0.409657 11.00000 -1.20000 AFIX 0 C30 1 0.663067 0.774634 0.303710 11.00000 0.03926 0.03493 = 0.02013 0.00302 0.00818 0.00297 C31 1 0.620044 0.823729 0.317642 11.00000 0.04356 0.04327 = 0.03735 0.00873 0.01791 0.00592 AFIX 23 H31A 2 0.628543 0.872307 0.357470 11.00000 -1.20000 H31B 2 0.600664 0.748444 0.322399 11.00000 -1.20000 AFIX 0 C32 1 0.592197 0.913407 0.265889 11.00000 0.04345 0.04650 = 0.04655 0.00898 0.01665 0.00725 AFIX 23 H32A 2 0.565335 0.948112 0.278219 11.00000 -1.20000 H32B 2 0.611741 0.988499 0.261390 11.00000 -1.20000 AFIX 0 C33 1 0.575062 0.845194 0.203382 11.00000 0.04190 0.05366 = 0.05234 0.00029 0.00083 -0.00218 AFIX 23 H33A 2 0.548551 0.788779 0.204229 11.00000 -1.20000 H33B 2 0.599919 0.787990 0.197180 11.00000 -1.20000 AFIX 0 C34 1 0.560254 0.938271 0.148402 11.00000 0.06250 0.07759 = 0.04945 0.00590 0.00811 0.00917 AFIX 23 H34A 2 0.539633 1.005967 0.157684 11.00000 -1.20000 H34B 2 0.542636 0.889212 0.111280 11.00000 -1.20000 AFIX 0 C35 1 0.601889 1.004616 0.134118 11.00000 0.09091 0.09961 = 0.05216 0.00501 0.03065 0.00101 AFIX 33 H35A 2 0.591083 1.063661 0.098567 11.00000 -1.20000 H35B 2 0.619079 1.054611 0.170523 11.00000 -1.20000 H35C 2 0.622081 0.937923 0.124146 11.00000 -1.20000 AFIX 0 C36 1 0.680209 0.635414 0.162394 11.00000 0.03391 0.02849 = 0.02671 -0.00253 0.00739 -0.00018 C37 1 0.646448 0.606510 0.100716 11.00000 0.04107 0.04913 = 0.02499 0.00180 0.00039 -0.00659 AFIX 23 H37A 2 0.656885 0.652093 0.067949 11.00000 -1.20000 H37B 2 0.616171 0.643990 0.100781 11.00000 -1.20000 AFIX 0 C38 1 0.639625 0.464512 0.083429 11.00000 0.07729 0.07624 = 0.05488 -0.03214 -0.00924 -0.01173 AFIX 23 H38A 2 0.635401 0.416111 0.119808 11.00000 -1.20000 H38B 2 0.668289 0.431610 0.075233 11.00000 -1.20000 AFIX 0 C39 1 0.599180 0.431671 0.027221 11.00000 0.07982 0.14550 = 0.07177 -0.05134 0.01754 -0.01752 AFIX 23 H39A 2 0.590174 0.339466 0.030461 11.00000 -1.20000 H39B 2 0.572502 0.487116 0.028364 11.00000 -1.20000 AFIX 0 C40 1 0.608461 0.449037 -0.028038 11.00000 0.11691 0.13175 = 0.06870 0.00171 0.02234 0.03165 AFIX 23 H40A 2 0.636075 0.397754 -0.029182 11.00000 -1.20000 H40B 2 0.614830 0.542434 -0.033736 11.00000 -1.20000 AFIX 0 C41 1 0.564015 0.401028 -0.083496 11.00000 0.14310 0.15323 = 0.04939 -0.02349 -0.02368 0.02949 AFIX 33 H41A 2 0.570385 0.413211 -0.123816 11.00000 -1.20000 H41B 2 0.558061 0.308385 -0.077733 11.00000 -1.20000 H41C 2 0.536880 0.452631 -0.082274 11.00000 -1.20000 AFIX 0 C42 1 0.806676 0.606163 0.239730 11.00000 0.03648 0.02820 = 0.02144 0.00124 0.00409 -0.00095 C43 1 0.848475 0.557660 0.221376 11.00000 0.04877 0.03808 = 0.04780 0.00845 0.02094 0.00891 AFIX 23 H43A 2 0.837900 0.496026 0.186193 11.00000 -1.20000 H43B 2 0.862918 0.632995 0.206207 11.00000 -1.20000 AFIX 0 C44 1 0.882916 0.494106 0.269335 11.00000 0.07923 0.22550 = 0.13342 0.10638 0.06589 0.08017 AFIX 23 H44A 2 0.868046 0.426271 0.288826 11.00000 -1.20000 H44B 2 0.897288 0.558836 0.301800 11.00000 -1.20000 AFIX 0 C45 1 0.921044 0.429677 0.244835 11.00000 0.08018 0.21695 = 0.15595 0.10458 0.07969 0.07223 AFIX 23 H45A 2 0.908039 0.418552 0.199379 11.00000 -1.20000 H45B 2 0.946404 0.494082 0.250762 11.00000 -1.20000 AFIX 0 C46 1 0.941472 0.309386 0.268247 11.00000 0.12169 0.19566 = 0.17352 0.05950 0.09353 0.03903 AFIX 23 H46A 2 0.916662 0.243215 0.262218 11.00000 -1.20000 H46B 2 0.955308 0.319079 0.313626 11.00000 -1.20000 AFIX 0 C47 1 0.976071 0.259674 0.241853 11.00000 0.09958 0.09265 = 0.09286 -0.01276 0.05261 -0.01574 AFIX 33 H47A 2 0.987638 0.176304 0.261651 11.00000 -1.20000 H47B 2 0.962785 0.246205 0.197086 11.00000 -1.20000 H47C 2 1.001571 0.322342 0.248678 11.00000 -1.20000 AFIX 0 C48 1 0.792409 0.742701 0.381106 11.00000 0.03815 0.02287 = 0.01820 0.00229 0.01055 -0.00082 C49 1 0.829115 0.763263 0.441006 11.00000 0.03872 0.03812 = 0.02351 0.00245 0.00506 -0.00432 AFIX 23 H49A 2 0.819328 0.723552 0.475708 11.00000 -1.20000 H49B 2 0.833765 0.858012 0.449328 11.00000 -1.20000 AFIX 0 C50 1 0.874085 0.701326 0.437055 11.00000 0.05196 0.05939 = 0.04413 0.00366 0.00765 0.00019 AFIX 23 H50A 2 0.886096 0.750669 0.406751 11.00000 -1.20000 H50B 2 0.867911 0.610701 0.421498 11.00000 -1.20000 AFIX 0 C51 1 0.910697 0.699083 0.499570 11.00000 0.05369 0.10044 = 0.05936 0.01225 0.00312 0.00224 AFIX 23 H51A 2 0.898956 0.646487 0.529120 11.00000 -1.20000 H51B 2 0.938527 0.654647 0.494184 11.00000 -1.20000 AFIX 0 C52 1 0.924320 0.829693 0.527362 11.00000 0.08359 0.10400 = 0.08264 -0.01711 -0.00972 -0.02064 AFIX 23 H52A 2 0.896508 0.875179 0.532167 11.00000 -1.20000 H52B 2 0.936899 0.881860 0.498491 11.00000 -1.20000 AFIX 0 C53 1 0.961038 0.823525 0.591963 11.00000 0.07907 0.22332 = 0.07813 -0.01334 -0.01355 -0.03886 AFIX 33 H53A 2 0.968608 0.912362 0.607873 11.00000 -1.20000 H53B 2 0.948575 0.773827 0.621147 11.00000 -1.20000 H53C 2 0.988995 0.780513 0.587447 11.00000 -1.20000 AFIX 0 C54 1 0.771722 1.087330 0.266654 11.00000 0.04036 0.02121 = 0.02364 0.00475 0.01195 0.00347 AFIX 43 H54 2 0.785207 1.060326 0.308365 11.00000 -1.20000 AFIX 0 C55 1 0.775084 1.217433 0.251779 11.00000 0.04482 0.01970 = 0.03013 -0.00488 0.01270 -0.00057 AFIX 43 H55 2 0.790716 1.278475 0.282370 11.00000 -1.20000 AFIX 0 C56 1 0.755036 1.256064 0.191102 11.00000 0.05597 0.01742 = 0.03144 0.00069 0.01772 -0.00084 AFIX 43 H56 2 0.756133 1.344852 0.179191 11.00000 -1.20000 AFIX 0 C57 1 0.733417 1.163376 0.148184 11.00000 0.05772 0.03307 = 0.02015 0.00779 0.01251 0.00141 AFIX 43 H57 2 0.719695 1.187600 0.106127 11.00000 -1.20000 AFIX 0 C58 1 0.731841 1.036633 0.166459 11.00000 0.04508 0.02443 = 0.02135 -0.00195 0.00980 0.00222 AFIX 43 H58 2 0.716998 0.973669 0.136353 11.00000 -1.20000 AFIX 0 HKLF 4 REM xcalibur REM R1 = 0.0442 for 9264 Fo > 4sig(Fo) and 0.0521 for all 10661 data REM 721 parameters refined using 23 restraints END WGHT 0.0300 27.3099 REM Instructions for potential hydrogen bonds HTAB C25 O7 EQIV $1 x, -y+1/2, z+1/2 HTAB C26 O14_$1 EQIV $2 x, y-1, z HTAB C28 O2_$2 HTAB C29 O3 HTAB C54 O16 EQIV $3 x, y+1, z HTAB C55 O13_$3 EQIV $4 x, -y+3/2, z-1/2 HTAB C57 O1_$4 HTAB C58 O12 REM Highest difference peak 1.191, deepest hole -0.759, 1-sigma level 0.093 Q1 1 0.9211 0.3402 0.2390 11.00000 0.05 1.19 Q2 1 0.5923 0.3534 -0.0203 11.00000 0.05 1.14 Q3 1 0.9161 0.2807 0.4345 11.00000 0.05 0.88 Q4 1 0.9317 0.4699 0.2774 11.00000 0.05 0.82 Q5 1 0.5612 0.5292 0.4320 11.00000 0.05 0.71 Q6 1 0.9275 0.2106 0.5237 11.00000 0.05 0.69 Q7 1 0.6026 0.5123 0.0074 11.00000 0.05 0.59 Q8 1 0.7596 0.5994 0.3081 11.00000 0.05 0.57 Q9 1 0.8783 0.4468 0.2568 11.00000 0.05 0.54 Q10 1 0.7706 0.8341 0.2693 11.00000 0.05 0.53 Q11 1 0.8724 0.8288 0.4356 11.00000 0.05 0.52 Q12 1 0.5688 0.4187 -0.0075 11.00000 0.05 0.52 Q13 1 0.5673 0.6959 0.4693 11.00000 0.05 0.51 Q14 1 0.8841 0.5678 0.2675 11.00000 0.05 0.50 Q15 1 0.6095 0.4515 0.4285 11.00000 0.05 0.49 Q16 1 0.7303 0.8591 0.2820 11.00000 0.05 0.49 Q17 1 0.7580 0.2781 0.4982 11.00000 0.05 0.49 Q18 1 0.8005 0.4459 0.4463 11.00000 0.05 0.48 Q19 1 0.9678 0.3585 0.5118 11.00000 0.05 0.48 Q20 1 0.7442 0.6762 0.3371 11.00000 0.05 0.46 Q21 1 0.7890 0.2268 0.4807 11.00000 0.05 0.46 Q22 1 0.7391 0.9125 0.2400 11.00000 0.05 0.45 Q23 1 0.7320 0.6949 0.2839 11.00000 0.05 0.44 Q24 1 0.7219 0.6504 0.3107 11.00000 0.05 0.43 Q25 1 0.7368 0.6516 0.2538 11.00000 0.05 0.41 ; _shelx_res_checksum 99425 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.75639(2) 0.22194(3) 0.46536(2) 0.02386(10) Uani 1 1 d D . . . . Rh2 Rh 0.76832(2) 0.43687(3) 0.43112(2) 0.02360(10) Uani 1 1 d D . . . . Rh3 Rh 0.72911(2) 0.58399(4) 0.28963(2) 0.02431(10) Uani 1 1 d . . . . . Rh4 Rh 0.74130(2) 0.79779(3) 0.25442(2) 0.02328(10) Uani 1 1 d . . . . . O1 O 0.70055(12) 0.2923(3) 0.48989(15) 0.0295(8) Uani 1 1 d . . . . . O2 O 0.71022(12) 0.4934(3) 0.45398(15) 0.0301(8) Uani 1 1 d . . . . . O3 O 0.71315(12) 0.1891(3) 0.37849(14) 0.0293(8) Uani 1 1 d . . . . . O4 O 0.72739(11) 0.3876(3) 0.34527(14) 0.0270(7) Uani 1 1 d . . . . . O5 O 0.81231(12) 0.1635(3) 0.43833(16) 0.0329(8) Uani 1 1 d . . . . . O6 O 0.82526(12) 0.3685(3) 0.40942(15) 0.0322(8) Uani 1 1 d . . . . . O7 O 0.79895(12) 0.2691(3) 0.55028(15) 0.0287(8) Uani 1 1 d . . . . . O8 O 0.80776(12) 0.4755(3) 0.51924(14) 0.0310(8) Uani 1 1 d . . . . . O9 O 0.67206(12) 0.6535(3) 0.31109(15) 0.0317(8) Uani 1 1 d . . . . . O10 O 0.68684(12) 0.8578(3) 0.28468(15) 0.0310(8) Uani 1 1 d . . . . . O11 O 0.68890(12) 0.5443(3) 0.20214(15) 0.0315(8) Uani 1 1 d . . . . . O12 O 0.69672(12) 0.7503(3) 0.17055(14) 0.0294(8) Uani 1 1 d . . . . . O13 O 0.78654(12) 0.5261(3) 0.26565(15) 0.0296(8) Uani 1 1 d . . . . . O14 O 0.79508(11) 0.7244(3) 0.22631(15) 0.0271(7) Uani 1 1 d . . . . . O15 O 0.77037(11) 0.6347(3) 0.37499(14) 0.0275(8) Uani 1 1 d . . . . . O16 O 0.78619(12) 0.8292(3) 0.33979(14) 0.0294(8) Uani 1 1 d . . . . . N1 N 0.74661(15) 0.0209(4) 0.49385(18) 0.0279(9) Uani 1 1 d . . . . . N2 N 0.75038(13) 0.9977(4) 0.22509(17) 0.0246(9) Uani 1 1 d . . . . . C1 C 0.68878(18) 0.4103(5) 0.4773(2) 0.0308(12) Uani 1 1 d . . . . . C2 C 0.6459(2) 0.4577(6) 0.4928(3) 0.0487(16) Uani 1 1 d . . . . . H2A H 0.6277 0.3805 0.4986 0.058 Uiso 1 1 calc R U . . . H2B H 0.6553 0.5044 0.5331 0.058 Uiso 1 1 calc R U . . . C3 C 0.6154(2) 0.5445(7) 0.4468(3) 0.0610(19) Uani 1 1 d . . . . . H3A H 0.6048 0.4968 0.4069 0.073 Uiso 1 1 calc R U . . . H3B H 0.6337 0.6204 0.4398 0.073 Uiso 1 1 calc R U . . . C4 C 0.5731(2) 0.5952(8) 0.4647(3) 0.065(2) Uani 1 1 d . . . . . H4A H 0.5534 0.5192 0.4673 0.078 Uiso 1 1 calc R U . . . H4B H 0.5838 0.6331 0.5070 0.078 Uiso 1 1 calc R U . . . C5 C 0.5447(3) 0.6909(8) 0.4249(4) 0.083(3) Uani 1 1 d . . . . . H5A H 0.5329 0.6532 0.3827 0.100 Uiso 1 1 calc R U . . . H5B H 0.5640 0.7673 0.4217 0.100 Uiso 1 1 calc R U . . . C6 C 0.5044(3) 0.7371(8) 0.4464(4) 0.080(2) Uani 1 1 d . . . . . H6A H 0.4868 0.8018 0.4170 0.096 Uiso 1 1 calc R U . . . H6B H 0.4844 0.6627 0.4487 0.096 Uiso 1 1 calc R U . . . H6C H 0.5156 0.7769 0.4877 0.096 Uiso 1 1 calc R U . . . C7 C 0.70605(17) 0.2774(5) 0.3380(2) 0.0263(11) Uani 1 1 d . . . . . C8 C 0.66834(17) 0.2593(5) 0.2798(2) 0.0299(11) Uani 1 1 d . . . . . H8A H 0.6640 0.1650 0.2700 0.036 Uiso 1 1 calc R U . . . H8B H 0.6765 0.3031 0.2448 0.036 Uiso 1 1 calc R U . . . C9 C 0.6234(2) 0.3176(6) 0.2881(3) 0.0456(14) Uani 1 1 d . . . . . H9A H 0.6165 0.2755 0.3243 0.055 Uiso 1 1 calc R U . . . H9B H 0.6282 0.4120 0.2974 0.055 Uiso 1 1 calc R U . . . C10 C 0.5823(2) 0.3009(7) 0.2317(3) 0.0589(18) Uani 1 1 d . . . . . H10A H 0.5769 0.2064 0.2236 0.071 Uiso 1 1 calc R U . . . H10B H 0.5900 0.3394 0.1951 0.071 Uiso 1 1 calc R U . . . C11 C 0.5379(2) 0.3630(7) 0.2379(4) 0.068(2) Uani 1 1 d . . . . . H11A H 0.5120 0.3347 0.2025 0.082 Uiso 1 1 calc R U . . . H11B H 0.5317 0.3316 0.2767 0.082 Uiso 1 1 calc R U . . . C12 C 0.5400(3) 0.5073(9) 0.2390(5) 0.105(4) Uani 1 1 d . . . . . H12A H 0.5108 0.5425 0.2430 0.126 Uiso 1 1 calc R U . . . H12B H 0.5653 0.5360 0.2745 0.126 Uiso 1 1 calc R U . . . H12C H 0.5455 0.5391 0.2003 0.126 Uiso 1 1 calc R U . . . C13 C 0.83501(18) 0.2487(5) 0.4179(2) 0.0336(12) Uani 1 1 d . . . . . C14 C 0.8786(2) 0.2017(6) 0.4035(3) 0.0458(15) Uani 1 1 d . . . . . H14A H 0.8888 0.2677 0.3778 0.055 Uiso 1 1 calc R U . . . H14B H 0.8720 0.1195 0.3793 0.055 Uiso 1 1 calc R U . . . C15 C 0.9169(3) 0.1782(9) 0.4631(4) 0.081(2) Uani 1 1 d . . . . . H15A H 0.9055 0.1169 0.4898 0.097 Uiso 1 1 calc R U . . . H15B H 0.9432 0.1356 0.4523 0.097 Uiso 1 1 calc R U . . . C16 C 0.9342(3) 0.3001(8) 0.4999(4) 0.071(2) Uani 1 1 d . . . . . H16A H 0.9460 0.3609 0.4734 0.085 Uiso 1 1 calc R U . . . H16B H 0.9078 0.3433 0.5103 0.085 Uiso 1 1 calc R U . . . C17 C 0.9715(3) 0.2771(11) 0.5590(5) 0.102(3) Uani 1 1 d . . . . . H17A H 0.9590 0.2218 0.5869 0.123 Uiso 1 1 calc R U . . . H17B H 0.9969 0.2282 0.5491 0.123 Uiso 1 1 calc R U . . . C18 C 0.9904(3) 0.3982(10) 0.5922(5) 0.102(3) Uani 1 1 d . . . . . H18A H 1.0145 0.3760 0.6302 0.123 Uiso 1 1 calc R U . . . H18B H 1.0035 0.4527 0.5654 0.123 Uiso 1 1 calc R U . . . H18C H 0.9656 0.4462 0.6032 0.123 Uiso 1 1 calc R U . . . C19 C 0.81522(17) 0.3842(5) 0.5587(2) 0.0272(11) Uani 1 1 d . . . . . C20 C 0.84797(18) 0.4118(5) 0.6225(2) 0.0316(12) Uani 1 1 d . . . . . H20A H 0.8786 0.3743 0.6241 0.038 Uiso 1 1 calc R U . . . H20B H 0.8363 0.3661 0.6542 0.038 Uiso 1 1 calc R U . . . C21 C 0.8543(2) 0.5563(5) 0.6401(3) 0.0383(13) Uani 1 1 d . . . . . H21A H 0.8599 0.6057 0.6048 0.046 Uiso 1 1 calc R U . . . H21B H 0.8255 0.5899 0.6475 0.046 Uiso 1 1 calc R U . . . C22 C 0.89398(19) 0.5803(5) 0.6976(2) 0.0349(12) Uani 1 1 d . . . . . H22A H 0.9012 0.6748 0.7002 0.042 Uiso 1 1 calc R U . . . H22B H 0.9215 0.5335 0.6927 0.042 Uiso 1 1 calc R U . . . C23 C 0.88494(19) 0.5370(6) 0.7589(2) 0.0389(13) Uani 1 1 d . . . . . H23A H 0.8575 0.5837 0.7644 0.047 Uiso 1 1 calc R U . . . H23B H 0.8781 0.4422 0.7570 0.047 Uiso 1 1 calc R U . . . C24 C 0.9257(2) 0.5642(6) 0.8139(3) 0.0517(16) Uani 1 1 d . . . . . H24A H 0.9187 0.5353 0.8521 0.062 Uiso 1 1 calc R U . . . H24B H 0.9527 0.5167 0.8090 0.062 Uiso 1 1 calc R U . . . H24C H 0.9322 0.6581 0.8164 0.062 Uiso 1 1 calc R U . . . C25 C 0.7647(2) -0.0188(5) 0.5524(2) 0.0383(13) Uani 1 1 d . . . . . H25 H 0.7801 0.0432 0.5826 0.046 Uiso 1 1 calc R U . . . C26 C 0.7619(2) -0.1459(5) 0.5703(2) 0.0415(14) Uani 1 1 d . . . . . H26 H 0.7751 -0.1712 0.6124 0.050 Uiso 1 1 calc R U . . . C27 C 0.7401(2) -0.2353(5) 0.5274(2) 0.0362(13) Uani 1 1 d . . . . . H27 H 0.7381 -0.3240 0.5389 0.043 Uiso 1 1 calc R U . . . C28 C 0.72097(18) -0.1958(5) 0.4670(2) 0.0321(12) Uani 1 1 d . . . . . H28 H 0.7051 -0.2565 0.4364 0.039 Uiso 1 1 calc R U . . . C29 C 0.72516(18) -0.0678(5) 0.4516(2) 0.0305(12) Uani 1 1 d . . . . . H29 H 0.7125 -0.0410 0.4097 0.037 Uiso 1 1 calc R U . . . C30 C 0.66307(18) 0.7746(5) 0.3037(2) 0.0314(12) Uani 1 1 d . . . . . C31 C 0.62004(19) 0.8237(6) 0.3176(3) 0.0400(13) Uani 1 1 d . . . . . H31A H 0.6285 0.8723 0.3575 0.048 Uiso 1 1 calc R U . . . H31B H 0.6007 0.7484 0.3224 0.048 Uiso 1 1 calc R U . . . C32 C 0.5922(2) 0.9134(6) 0.2659(3) 0.0447(14) Uani 1 1 d . . . . . H32A H 0.5653 0.9481 0.2782 0.054 Uiso 1 1 calc R U . . . H32B H 0.6117 0.9885 0.2614 0.054 Uiso 1 1 calc R U . . . C33 C 0.5751(2) 0.8452(6) 0.2034(3) 0.0517(16) Uani 1 1 d . . . . . H33A H 0.5486 0.7888 0.2042 0.062 Uiso 1 1 calc R U . . . H33B H 0.5999 0.7880 0.1972 0.062 Uiso 1 1 calc R U . . . C34 C 0.5603(2) 0.9383(8) 0.1484(3) 0.0646(19) Uani 1 1 d . . . . . H34A H 0.5396 1.0060 0.1577 0.078 Uiso 1 1 calc R U . . . H34B H 0.5426 0.8892 0.1113 0.078 Uiso 1 1 calc R U . . . C35 C 0.6019(3) 1.0046(9) 0.1341(3) 0.079(2) Uani 1 1 d . . . . . H35A H 0.5911 1.0637 0.0986 0.094 Uiso 1 1 calc R U . . . H35B H 0.6191 1.0546 0.1705 0.094 Uiso 1 1 calc R U . . . H35C H 0.6221 0.9379 0.1241 0.094 Uiso 1 1 calc R U . . . C36 C 0.68021(17) 0.6354(5) 0.1624(2) 0.0299(11) Uani 1 1 d . . . . . C37 C 0.6464(2) 0.6065(6) 0.1007(2) 0.0401(13) Uani 1 1 d . . . . . H37A H 0.6569 0.6521 0.0679 0.048 Uiso 1 1 calc R U . . . H37B H 0.6162 0.6440 0.1008 0.048 Uiso 1 1 calc R U . . . C38 C 0.6396(3) 0.4645(8) 0.0834(3) 0.075(2) Uani 1 1 d . . . . . H38A H 0.6354 0.4161 0.1198 0.090 Uiso 1 1 calc R U . . . H38B H 0.6683 0.4316 0.0752 0.090 Uiso 1 1 calc R U . . . C39 C 0.5992(3) 0.4317(11) 0.0272(4) 0.100(3) Uani 1 1 d D . . . . H39A H 0.5902 0.3395 0.0305 0.120 Uiso 1 1 calc R U . . . H39B H 0.5725 0.4871 0.0284 0.120 Uiso 1 1 calc R U . . . C40 C 0.6085(4) 0.4490(11) -0.0280(4) 0.106(3) Uani 1 1 d D . . . . H40A H 0.6361 0.3978 -0.0292 0.128 Uiso 1 1 calc R U . . . H40B H 0.6148 0.5424 -0.0337 0.128 Uiso 1 1 calc R U . . . C41 C 0.5640(4) 0.4010(12) -0.0835(4) 0.125(4) Uani 1 1 d . . . . . H41A H 0.5704 0.4132 -0.1238 0.150 Uiso 1 1 calc R U . . . H41B H 0.5581 0.3084 -0.0777 0.150 Uiso 1 1 calc R U . . . H41C H 0.5369 0.4526 -0.0823 0.150 Uiso 1 1 calc R U . . . C42 C 0.80668(18) 0.6062(5) 0.2397(2) 0.0295(11) Uani 1 1 d . . . . . C43 C 0.8485(2) 0.5577(6) 0.2214(3) 0.0434(14) Uani 1 1 d . . . . . H43A H 0.8379 0.4960 0.1862 0.052 Uiso 1 1 calc R U . . . H43B H 0.8629 0.6330 0.2062 0.052 Uiso 1 1 calc R U . . . C44 C 0.8829(3) 0.4941(13) 0.2693(5) 0.139(4) Uani 1 1 d . U . . . H44A H 0.8680 0.4263 0.2888 0.167 Uiso 1 1 calc R U . . . H44B H 0.8973 0.5588 0.3018 0.167 Uiso 1 1 calc R U . . . C45 C 0.9210(3) 0.4297(13) 0.2448(6) 0.142(4) Uani 1 1 d D U . . . H45A H 0.9080 0.4186 0.1994 0.170 Uiso 1 1 calc R U . . . H45B H 0.9464 0.4941 0.2508 0.170 Uiso 1 1 calc R U . . . C46 C 0.9415(4) 0.3094(14) 0.2682(6) 0.153(4) Uani 1 1 d D U . . . H46A H 0.9167 0.2432 0.2622 0.184 Uiso 1 1 calc R U . . . H46B H 0.9553 0.3191 0.3136 0.184 Uiso 1 1 calc R U . . . C47 C 0.9761(3) 0.2597(9) 0.2419(4) 0.090(3) Uani 1 1 d . . . . . H47A H 0.9876 0.1763 0.2617 0.108 Uiso 1 1 calc R U . . . H47B H 0.9628 0.2462 0.1971 0.108 Uiso 1 1 calc R U . . . H47C H 1.0016 0.3223 0.2487 0.108 Uiso 1 1 calc R U . . . C48 C 0.79241(17) 0.7427(5) 0.3811(2) 0.0259(11) Uani 1 1 d . . . . . C49 C 0.82911(18) 0.7633(5) 0.4410(2) 0.0341(12) Uani 1 1 d . . . . . H49A H 0.8193 0.7236 0.4757 0.041 Uiso 1 1 calc R U . . . H49B H 0.8338 0.8580 0.4493 0.041 Uiso 1 1 calc R U . . . C50 C 0.8741(2) 0.7013(7) 0.4371(3) 0.0529(16) Uani 1 1 d . . . . . H50A H 0.8861 0.7507 0.4068 0.064 Uiso 1 1 calc R U . . . H50B H 0.8679 0.6107 0.4215 0.064 Uiso 1 1 calc R U . . . C51 C 0.9107(3) 0.6991(9) 0.4996(3) 0.074(2) Uani 1 1 d . . . . . H51A H 0.8990 0.6465 0.5291 0.088 Uiso 1 1 calc R U . . . H51B H 0.9385 0.6546 0.4942 0.088 Uiso 1 1 calc R U . . . C52 C 0.9243(3) 0.8297(10) 0.5274(4) 0.097(3) Uani 1 1 d . . . . . H52A H 0.8965 0.8752 0.5322 0.116 Uiso 1 1 calc R U . . . H52B H 0.9369 0.8819 0.4985 0.116 Uiso 1 1 calc R U . . . C53 C 0.9610(3) 0.8235(13) 0.5920(4) 0.134(5) Uani 1 1 d . . . . . H53A H 0.9686 0.9124 0.6079 0.161 Uiso 1 1 calc R U . . . H53B H 0.9486 0.7738 0.6211 0.161 Uiso 1 1 calc R U . . . H53C H 0.9890 0.7805 0.5874 0.161 Uiso 1 1 calc R U . . . C54 C 0.77172(17) 1.0873(5) 0.2667(2) 0.0278(11) Uani 1 1 d . . . . . H54 H 0.7852 1.0603 0.3084 0.033 Uiso 1 1 calc R U . . . C55 C 0.77508(18) 1.2174(5) 0.2518(2) 0.0311(12) Uani 1 1 d . . . . . H55 H 0.7907 1.2785 0.2824 0.037 Uiso 1 1 calc R U . . . C56 C 0.75504(19) 1.2561(5) 0.1911(2) 0.0338(12) Uani 1 1 d . . . . . H56 H 0.7561 1.3449 0.1792 0.041 Uiso 1 1 calc R U . . . C57 C 0.7334(2) 1.1634(5) 0.1482(2) 0.0366(13) Uani 1 1 d . . . . . H57 H 0.7197 1.1876 0.1061 0.044 Uiso 1 1 calc R U . . . C58 C 0.73184(18) 1.0366(5) 0.1665(2) 0.0302(11) Uani 1 1 d . . . . . H58 H 0.7170 0.9737 0.1364 0.036 Uiso 1 1 calc R U . . . 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 0.0355(2) 0.01690(19) 0.01823(19) 0.00159(14) 0.00574(16) 0.00025(16) Rh2 0.0320(2) 0.0180(2) 0.01968(19) 0.00281(14) 0.00529(16) -0.00021(16) Rh3 0.0337(2) 0.0185(2) 0.01927(19) 0.00288(15) 0.00481(16) -0.00200(16) Rh4 0.0332(2) 0.01743(19) 0.01843(19) 0.00224(14) 0.00586(16) -0.00038(16) O1 0.037(2) 0.0251(19) 0.0268(18) 0.0052(14) 0.0098(16) 0.0004(15) O2 0.039(2) 0.0208(18) 0.0320(19) 0.0029(15) 0.0127(16) 0.0051(15) O3 0.042(2) 0.0220(18) 0.0212(17) 0.0017(14) 0.0042(15) -0.0040(15) O4 0.038(2) 0.0210(18) 0.0211(17) 0.0066(14) 0.0063(15) -0.0005(15) O5 0.043(2) 0.0227(18) 0.034(2) 0.0043(15) 0.0123(17) 0.0068(16) O6 0.037(2) 0.030(2) 0.0310(19) 0.0080(15) 0.0099(16) 0.0048(16) O7 0.041(2) 0.0186(18) 0.0233(18) 0.0023(14) 0.0029(15) -0.0017(15) O8 0.043(2) 0.0243(18) 0.0210(17) 0.0022(15) 0.0020(15) -0.0050(16) O9 0.036(2) 0.028(2) 0.0324(19) 0.0092(15) 0.0113(16) -0.0007(16) O10 0.038(2) 0.0278(19) 0.0291(18) 0.0047(15) 0.0120(16) 0.0023(16) O11 0.043(2) 0.0239(18) 0.0241(18) -0.0003(15) 0.0032(16) -0.0088(16) O12 0.040(2) 0.0258(19) 0.0197(17) 0.0042(14) 0.0042(15) 0.0000(16) O13 0.042(2) 0.0193(17) 0.0281(18) 0.0052(14) 0.0115(16) 0.0040(15) O14 0.037(2) 0.0213(18) 0.0243(18) 0.0038(14) 0.0106(15) 0.0007(15) O15 0.038(2) 0.0220(18) 0.0207(17) 0.0049(14) 0.0055(15) -0.0009(15) O16 0.043(2) 0.0191(17) 0.0231(17) -0.0004(14) 0.0037(15) -0.0035(15) N1 0.042(2) 0.017(2) 0.025(2) 0.0025(17) 0.0099(19) -0.0023(18) N2 0.033(2) 0.019(2) 0.023(2) -0.0006(17) 0.0093(18) 0.0021(17) C1 0.037(3) 0.033(3) 0.023(3) 0.002(2) 0.009(2) 0.004(2) C2 0.051(4) 0.054(4) 0.049(4) 0.020(3) 0.026(3) 0.016(3) C3 0.047(4) 0.077(5) 0.063(4) 0.030(4) 0.022(3) 0.018(4) C4 0.046(4) 0.093(6) 0.060(4) 0.022(4) 0.024(3) 0.012(4) C5 0.073(5) 0.077(6) 0.114(7) 0.014(5) 0.049(5) 0.018(5) C6 0.068(5) 0.077(6) 0.107(7) -0.005(5) 0.043(5) 0.008(4) C7 0.033(3) 0.020(3) 0.027(3) 0.002(2) 0.010(2) 0.001(2) C8 0.041(3) 0.025(3) 0.021(2) 0.001(2) 0.004(2) -0.005(2) C9 0.044(3) 0.050(4) 0.039(3) -0.004(3) 0.005(3) -0.003(3) C10 0.048(4) 0.055(4) 0.062(4) -0.006(3) -0.004(3) 0.001(3) C11 0.046(4) 0.068(5) 0.083(5) -0.008(4) 0.004(4) -0.005(4) C12 0.056(5) 0.075(6) 0.163(10) -0.027(6) -0.005(6) 0.001(4) C13 0.038(3) 0.036(3) 0.026(3) 0.001(2) 0.007(2) 0.004(3) C14 0.051(4) 0.046(4) 0.046(3) 0.006(3) 0.023(3) 0.015(3) C15 0.056(5) 0.088(6) 0.102(7) 0.004(5) 0.027(5) 0.015(4) C16 0.060(5) 0.079(6) 0.070(5) 0.006(4) 0.015(4) 0.011(4) C17 0.070(6) 0.136(9) 0.093(7) 0.017(7) 0.011(5) 0.003(6) C18 0.086(7) 0.119(9) 0.095(7) 0.005(6) 0.014(6) -0.022(6) C19 0.035(3) 0.022(3) 0.024(3) 0.001(2) 0.008(2) 0.001(2) C20 0.041(3) 0.027(3) 0.023(3) -0.001(2) 0.004(2) -0.005(2) C21 0.051(3) 0.023(3) 0.036(3) 0.002(2) 0.004(3) -0.004(2) C22 0.042(3) 0.029(3) 0.031(3) -0.003(2) 0.006(2) -0.010(2) C23 0.042(3) 0.039(3) 0.033(3) -0.004(2) 0.007(3) -0.008(3) C24 0.064(4) 0.056(4) 0.032(3) -0.003(3) 0.007(3) -0.018(3) C25 0.062(4) 0.031(3) 0.022(3) -0.001(2) 0.012(3) -0.009(3) C26 0.072(4) 0.029(3) 0.021(3) 0.005(2) 0.010(3) 0.000(3) C27 0.055(4) 0.023(3) 0.033(3) 0.007(2) 0.017(3) 0.001(2) C28 0.044(3) 0.026(3) 0.029(3) -0.004(2) 0.013(2) -0.005(2) C29 0.043(3) 0.025(3) 0.022(3) 0.001(2) 0.008(2) 0.001(2) C30 0.039(3) 0.035(3) 0.020(3) 0.003(2) 0.008(2) 0.003(2) C31 0.044(3) 0.043(3) 0.037(3) 0.009(3) 0.018(3) 0.006(3) C32 0.043(3) 0.046(4) 0.047(3) 0.009(3) 0.017(3) 0.007(3) C33 0.042(3) 0.054(4) 0.052(4) 0.000(3) 0.001(3) -0.002(3) C34 0.063(4) 0.078(5) 0.049(4) 0.006(4) 0.008(3) 0.009(4) C35 0.091(6) 0.100(7) 0.052(4) 0.005(4) 0.031(4) 0.001(5) C36 0.034(3) 0.028(3) 0.027(3) -0.003(2) 0.007(2) 0.000(2) C37 0.041(3) 0.049(4) 0.025(3) 0.002(2) 0.000(2) -0.007(3) C38 0.077(5) 0.076(5) 0.055(4) -0.032(4) -0.009(4) -0.012(4) C39 0.080(6) 0.145(9) 0.072(6) -0.051(6) 0.018(5) -0.018(6) C40 0.117(8) 0.132(9) 0.069(6) 0.002(6) 0.022(6) 0.032(7) C41 0.143(10) 0.153(10) 0.049(5) -0.023(6) -0.024(6) 0.029(8) C42 0.036(3) 0.028(3) 0.021(2) 0.001(2) 0.004(2) -0.001(2) C43 0.049(4) 0.038(3) 0.048(3) 0.008(3) 0.021(3) 0.009(3) C44 0.079(5) 0.225(10) 0.133(7) 0.106(7) 0.066(5) 0.080(6) C45 0.080(5) 0.217(9) 0.156(7) 0.105(7) 0.080(5) 0.072(6) C46 0.122(7) 0.196(10) 0.174(9) 0.059(8) 0.094(7) 0.039(7) C47 0.100(7) 0.093(7) 0.093(6) -0.013(5) 0.053(6) -0.016(5) C48 0.038(3) 0.023(3) 0.018(2) 0.002(2) 0.011(2) -0.001(2) C49 0.039(3) 0.038(3) 0.024(3) 0.002(2) 0.005(2) -0.004(2) C50 0.052(4) 0.059(4) 0.044(4) 0.004(3) 0.008(3) 0.000(3) C51 0.054(4) 0.100(6) 0.059(5) 0.012(4) 0.003(4) 0.002(4) C52 0.084(6) 0.104(7) 0.083(6) -0.017(6) -0.010(5) -0.021(5) C53 0.079(7) 0.223(14) 0.078(7) -0.013(8) -0.014(5) -0.039(8) C54 0.040(3) 0.021(3) 0.024(3) 0.005(2) 0.012(2) 0.003(2) C55 0.045(3) 0.020(3) 0.030(3) -0.005(2) 0.013(2) -0.001(2) C56 0.056(4) 0.017(3) 0.031(3) 0.001(2) 0.018(3) -0.001(2) C57 0.058(4) 0.033(3) 0.020(3) 0.008(2) 0.013(2) 0.001(3) C58 0.045(3) 0.024(3) 0.021(3) -0.002(2) 0.010(2) 0.002(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Rh1 O7 89.21(14) . . ? O5 Rh1 O1 176.22(13) . . ? O7 Rh1 O1 91.14(14) . . ? O5 Rh1 O3 91.88(14) . . ? O7 Rh1 O3 175.72(13) . . ? O1 Rh1 O3 87.50(13) . . ? O5 Rh1 N1 89.94(14) . . ? O7 Rh1 N1 92.99(14) . . ? O1 Rh1 N1 93.80(14) . . ? O3 Rh1 N1 91.15(14) . . ? O5 Rh1 Rh2 88.02(10) . . ? O7 Rh1 Rh2 88.21(9) . . ? O1 Rh1 Rh2 88.22(9) . . ? O3 Rh1 Rh2 87.69(9) . . ? N1 Rh1 Rh2 177.62(11) . . ? O6 Rh2 O2 176.33(13) . . ? O6 Rh2 O4 91.23(14) . . ? O2 Rh2 O4 88.15(13) . . ? O6 Rh2 O8 89.53(14) . . ? O2 Rh2 O8 90.86(14) . . ? O4 Rh2 O8 176.26(13) . . ? O6 Rh2 Rh1 88.33(10) . . ? O2 Rh2 Rh1 88.03(9) . . ? O4 Rh2 Rh1 88.19(9) . . ? O8 Rh2 Rh1 88.17(9) . . ? O6 Rh2 O15 91.19(12) . . ? O2 Rh2 O15 92.25(12) . . ? O4 Rh2 O15 79.16(12) . . ? O8 Rh2 O15 104.49(12) . . ? Rh1 Rh2 O15 167.33(8) . . ? O13 Rh3 O9 176.24(13) . . ? O13 Rh3 O15 88.70(13) . . ? O9 Rh3 O15 91.55(14) . . ? O13 Rh3 O11 90.75(14) . . ? O9 Rh3 O11 88.77(14) . . ? O15 Rh3 O11 176.33(13) . . ? O13 Rh3 O4 91.96(12) . . ? O9 Rh3 O4 91.77(12) . . ? O15 Rh3 O4 79.67(12) . . ? O11 Rh3 O4 103.98(12) . . ? O13 Rh3 Rh4 87.76(9) . . ? O9 Rh3 Rh4 88.50(9) . . ? O15 Rh3 Rh4 88.03(9) . . ? O11 Rh3 Rh4 88.33(9) . . ? O4 Rh3 Rh4 167.70(8) . . ? O10 Rh4 O14 175.84(13) . . ? O10 Rh4 O16 91.66(14) . . ? O14 Rh4 O16 88.16(13) . . ? O10 Rh4 O12 89.45(14) . . ? O14 Rh4 O12 90.40(13) . . ? O16 Rh4 O12 175.31(13) . . ? O10 Rh4 N2 89.78(14) . . ? O14 Rh4 N2 94.38(13) . . ? O16 Rh4 N2 91.58(13) . . ? O12 Rh4 N2 92.99(14) . . ? O10 Rh4 Rh3 87.47(10) . . ? O14 Rh4 Rh3 88.37(9) . . ? O16 Rh4 Rh3 87.63(9) . . ? O12 Rh4 Rh3 87.87(9) . . ? N2 Rh4 Rh3 177.11(10) . . ? C1 O1 Rh1 118.6(3) . . ? C1 O2 Rh2 119.0(3) . . ? C7 O3 Rh1 120.3(3) . . ? C7 O4 Rh2 119.2(3) . . ? C7 O4 Rh3 139.3(3) . . ? Rh2 O4 Rh3 100.90(13) . . ? C13 O5 Rh1 118.6(3) . . ? C13 O6 Rh2 118.4(3) . . ? C19 O7 Rh1 118.4(3) . . ? C19 O8 Rh2 118.4(3) . . ? C30 O9 Rh3 118.3(3) . . ? C30 O10 Rh4 119.6(3) . . ? C36 O11 Rh3 118.8(3) . . ? C36 O12 Rh4 119.0(3) . . ? C42 O13 Rh3 119.1(3) . . ? C42 O14 Rh4 117.9(3) . . ? C48 O15 Rh3 119.1(3) . . ? C48 O15 Rh2 139.8(3) . . ? Rh3 O15 Rh2 100.27(13) . . ? C48 O16 Rh4 120.2(3) . . ? C25 N1 C29 118.2(4) . . ? C25 N1 Rh1 121.2(3) . . ? C29 N1 Rh1 120.4(3) . . ? C58 N2 C54 117.9(4) . . ? C58 N2 Rh4 121.3(3) . . ? C54 N2 Rh4 120.6(3) . . ? O2 C1 O1 126.0(5) . . ? O2 C1 C2 116.5(5) . . ? O1 C1 C2 117.4(5) . . ? C3 C2 C1 116.3(5) . . ? C3 C2 H2A 108.2 . . ? C1 C2 H2A 108.2 . . ? C3 C2 H2B 108.2 . . ? C1 C2 H2B 108.2 . . ? H2A C2 H2B 107.4 . . ? C2 C3 C4 115.2(5) . . ? C2 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? C2 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C5 C4 C3 117.8(6) . . ? C5 C4 H4A 107.8 . . ? C3 C4 H4A 107.8 . . ? C5 C4 H4B 107.8 . . ? C3 C4 H4B 107.8 . . ? H4A C4 H4B 107.2 . . ? C4 C5 C6 114.3(7) . . ? C4 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 O4 124.0(4) . . ? O3 C7 C8 118.6(4) . . ? O4 C7 C8 117.2(4) . . ? C7 C8 C9 109.4(4) . . ? C7 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 113.6(5) . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C11 114.5(6) . . ? C9 C10 H10A 108.6 . . ? C11 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? C11 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C10 112.6(7) . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O6 C13 O5 126.5(5) . . ? O6 C13 C14 117.2(5) . . ? O5 C13 C14 116.3(5) . . ? C13 C14 C15 111.0(5) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 114.3(7) . . ? C16 C15 H15A 108.7 . . ? C14 C15 H15A 108.7 . . ? C16 C15 H15B 108.7 . . ? C14 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C15 114.4(8) . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C18 C17 C16 113.8(9) . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? C16 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O8 C19 O7 126.6(4) . . ? O8 C19 C20 117.6(4) . . ? O7 C19 C20 115.8(4) . . ? C19 C20 C21 115.0(4) . . ? C19 C20 H20A 108.5 . . ? C21 C20 H20A 108.5 . . ? C19 C20 H20B 108.5 . . ? C21 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C22 C21 C20 112.8(4) . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21B 109.0 . . ? C20 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 114.7(4) . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22B 108.6 . . ? C23 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C24 C23 C22 111.8(5) . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 122.3(5) . . ? N1 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C27 C26 C25 119.3(5) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 119.2(5) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C29 C28 C27 119.0(5) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? N1 C29 C28 122.0(5) . . ? N1 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? O10 C30 O9 125.6(5) . . ? O10 C30 C31 116.6(5) . . ? O9 C30 C31 117.7(5) . . ? C30 C31 C32 111.6(4) . . ? C30 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? C30 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C33 C32 C31 113.3(5) . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32B 108.9 . . ? C31 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C32 C33 C34 113.9(6) . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33B 108.8 . . ? C34 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C33 C34 C35 111.7(6) . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O11 C36 O12 125.8(5) . . ? O11 C36 C37 117.2(5) . . ? O12 C36 C37 117.0(5) . . ? C36 C37 C38 115.9(5) . . ? C36 C37 H37A 108.3 . . ? C38 C37 H37A 108.3 . . ? C36 C37 H37B 108.3 . . ? C38 C37 H37B 108.3 . . ? H37A C37 H37B 107.4 . . ? C37 C38 C39 116.5(7) . . ? C37 C38 H38A 108.2 . . ? C39 C38 H38A 108.2 . . ? C37 C38 H38B 108.2 . . ? C39 C38 H38B 108.2 . . ? H38A C38 H38B 107.3 . . ? C40 C39 C38 113.8(8) . . ? C40 C39 H39A 108.8 . . ? C38 C39 H39A 108.8 . . ? C40 C39 H39B 108.8 . . ? C38 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C39 C40 C41 108.8(9) . . ? C39 C40 H40A 109.9 . . ? C41 C40 H40A 109.9 . . ? C39 C40 H40B 109.9 . . ? C41 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O13 C42 O14 126.5(5) . . ? O13 C42 C43 117.2(5) . . ? O14 C42 C43 116.3(4) . . ? C44 C43 C42 115.7(6) . . ? C44 C43 H43A 108.4 . . ? C42 C43 H43A 108.4 . . ? C44 C43 H43B 108.4 . . ? C42 C43 H43B 108.4 . . ? H43A C43 H43B 107.4 . . ? C43 C44 C45 112.6(8) . . ? C43 C44 H44A 109.1 . . ? C45 C44 H44A 109.1 . . ? C43 C44 H44B 109.1 . . ? C45 C44 H44B 109.1 . . ? H44A C44 H44B 107.8 . . ? C46 C45 C44 122.0(9) . . ? C46 C45 H45A 106.8 . . ? C44 C45 H45A 106.8 . . ? C46 C45 H45B 106.8 . . ? C44 C45 H45B 106.8 . . ? H45A C45 H45B 106.7 . . ? C45 C46 C47 116.9(10) . . ? C45 C46 H46A 108.1 . . ? C47 C46 H46A 108.1 . . ? C45 C46 H46B 108.1 . . ? C47 C46 H46B 108.1 . . ? H46A C46 H46B 107.3 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O16 C48 O15 124.3(4) . . ? O16 C48 C49 118.8(4) . . ? O15 C48 C49 116.8(4) . . ? C48 C49 C50 109.9(4) . . ? C48 C49 H49A 109.7 . . ? C50 C49 H49A 109.7 . . ? C48 C49 H49B 109.7 . . ? C50 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? C49 C50 C51 112.6(5) . . ? C49 C50 H50A 109.1 . . ? C51 C50 H50A 109.1 . . ? C49 C50 H50B 109.1 . . ? C51 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C52 C51 C50 114.7(7) . . ? C52 C51 H51A 108.6 . . ? C50 C51 H51A 108.6 . . ? C52 C51 H51B 108.6 . . ? C50 C51 H51B 108.6 . . ? H51A C51 H51B 107.6 . . ? C51 C52 C53 113.3(9) . . ? C51 C52 H52A 108.9 . . ? C53 C52 H52A 108.9 . . ? C51 C52 H52B 108.9 . . ? C53 C52 H52B 108.9 . . ? H52A C52 H52B 107.7 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N2 C54 C55 123.1(5) . . ? N2 C54 H54 118.4 . . ? C55 C54 H54 118.4 . . ? C56 C55 C54 118.1(5) . . ? C56 C55 H55 121.0 . . ? C54 C55 H55 121.0 . . ? C57 C56 C55 118.8(5) . . ? C57 C56 H56 120.6 . . ? C55 C56 H56 120.6 . . ? C58 C57 C56 119.6(5) . . ? C58 C57 H57 120.2 . . ? C56 C57 H57 120.2 . . ? N2 C58 C57 122.5(5) . . ? N2 C58 H58 118.7 . . ? C57 C58 H58 118.7 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O5 2.030(3) . ? Rh1 O7 2.035(3) . ? Rh1 O1 2.039(3) . ? Rh1 O3 2.047(3) . ? Rh1 N1 2.198(4) . ? Rh1 Rh2 2.3884(5) . ? Rh2 O6 2.031(3) . ? Rh2 O2 2.038(3) . ? Rh2 O4 2.039(3) . ? Rh2 O8 2.040(3) . ? Rh2 O15 2.392(3) . ? Rh3 O13 2.036(3) . ? Rh3 O9 2.036(3) . ? Rh3 O15 2.037(3) . ? Rh3 O11 2.038(3) . ? Rh3 O4 2.372(3) . ? Rh3 Rh4 2.3877(5) . ? Rh4 O10 2.034(3) . ? Rh4 O14 2.036(3) . ? Rh4 O16 2.038(3) . ? Rh4 O12 2.042(3) . ? Rh4 N2 2.188(4) . ? O1 C1 1.268(6) . ? O2 C1 1.264(6) . ? O3 C7 1.256(6) . ? O4 C7 1.285(6) . ? O5 C13 1.269(6) . ? O6 C13 1.262(6) . ? O7 C19 1.270(6) . ? O8 C19 1.261(6) . ? O9 C30 1.270(6) . ? O10 C30 1.260(6) . ? O11 C36 1.264(6) . ? O12 C36 1.270(6) . ? O13 C42 1.253(6) . ? O14 C42 1.272(6) . ? O15 C48 1.277(6) . ? O16 C48 1.256(5) . ? N1 C25 1.335(6) . ? N1 C29 1.341(6) . ? N2 C58 1.336(6) . ? N2 C54 1.338(6) . ? C1 C2 1.508(7) . ? C2 C3 1.472(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.529(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.438(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.501(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.485(7) . ? C8 C9 1.536(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.514(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.522(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.478(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.513(7) . ? C14 C15 1.524(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.506(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.498(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.476(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.522(7) . ? C20 C21 1.528(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.515(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.535(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.505(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.371(7) . ? C25 H25 0.9500 . ? C26 C27 1.358(7) . ? C26 H26 0.9500 . ? C27 C28 1.375(7) . ? C27 H27 0.9500 . ? C28 C29 1.369(7) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.501(7) . ? C31 C32 1.533(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.520(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.522(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.535(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.500(7) . ? C37 C38 1.503(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.528(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.351(11) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.630(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.512(7) . ? C43 C44 1.427(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.550(12) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.411(14) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.426(12) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.498(7) . ? C49 C50 1.520(8) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.524(9) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.483(11) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.560(11) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.383(7) . ? C54 H54 0.9500 . ? C55 C56 1.382(7) . ? C55 H55 0.9500 . ? C56 C57 1.379(7) . ? C56 H56 0.9500 . ? C57 C58 1.365(7) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh2 O2 C1 O1 1.8(7) . . . . ? Rh2 O2 C1 C2 -179.5(4) . . . . ? Rh1 O1 C1 O2 -4.7(7) . . . . ? Rh1 O1 C1 C2 176.7(4) . . . . ? O2 C1 C2 C3 41.5(8) . . . . ? O1 C1 C2 C3 -139.8(6) . . . . ? C1 C2 C3 C4 -177.8(6) . . . . ? C2 C3 C4 C5 173.6(8) . . . . ? C3 C4 C5 C6 -178.9(7) . . . . ? Rh1 O3 C7 O4 6.0(7) . . . . ? Rh1 O3 C7 C8 -169.0(3) . . . . ? Rh2 O4 C7 O3 -9.6(6) . . . . ? Rh3 O4 C7 O3 -179.5(3) . . . . ? Rh2 O4 C7 C8 165.5(3) . . . . ? Rh3 O4 C7 C8 -4.4(7) . . . . ? O3 C7 C8 C9 91.0(6) . . . . ? O4 C7 C8 C9 -84.4(6) . . . . ? C7 C8 C9 C10 -178.5(5) . . . . ? C8 C9 C10 C11 -177.5(6) . . . . ? C9 C10 C11 C12 68.5(9) . . . . ? Rh2 O6 C13 O5 0.9(7) . . . . ? Rh2 O6 C13 C14 -177.8(4) . . . . ? Rh1 O5 C13 O6 -3.7(7) . . . . ? Rh1 O5 C13 C14 175.0(4) . . . . ? O6 C13 C14 C15 104.6(6) . . . . ? O5 C13 C14 C15 -74.2(7) . . . . ? C13 C14 C15 C16 -66.6(8) . . . . ? C14 C15 C16 C17 179.3(7) . . . . ? C15 C16 C17 C18 175.8(8) . . . . ? Rh2 O8 C19 O7 -3.3(7) . . . . ? Rh2 O8 C19 C20 175.0(3) . . . . ? Rh1 O7 C19 O8 0.1(7) . . . . ? Rh1 O7 C19 C20 -178.2(3) . . . . ? O8 C19 C20 C21 21.4(7) . . . . ? O7 C19 C20 C21 -160.1(5) . . . . ? C19 C20 C21 C22 -168.4(4) . . . . ? C20 C21 C22 C23 -72.4(6) . . . . ? C21 C22 C23 C24 -179.8(5) . . . . ? C29 N1 C25 C26 -0.3(8) . . . . ? Rh1 N1 C25 C26 -175.3(4) . . . . ? N1 C25 C26 C27 0.2(9) . . . . ? C25 C26 C27 C28 -0.7(9) . . . . ? C26 C27 C28 C29 1.2(8) . . . . ? C25 N1 C29 C28 0.8(8) . . . . ? Rh1 N1 C29 C28 175.9(4) . . . . ? C27 C28 C29 N1 -1.3(8) . . . . ? Rh4 O10 C30 O9 6.4(7) . . . . ? Rh4 O10 C30 C31 -172.5(3) . . . . ? Rh3 O9 C30 O10 -0.9(7) . . . . ? Rh3 O9 C30 C31 178.0(3) . . . . ? O10 C30 C31 C32 45.7(7) . . . . ? O9 C30 C31 C32 -133.3(5) . . . . ? C30 C31 C32 C33 62.3(7) . . . . ? C31 C32 C33 C34 -162.8(5) . . . . ? C32 C33 C34 C35 72.7(8) . . . . ? Rh3 O11 C36 O12 4.7(7) . . . . ? Rh3 O11 C36 C37 -173.6(4) . . . . ? Rh4 O12 C36 O11 -0.2(7) . . . . ? Rh4 O12 C36 C37 178.1(3) . . . . ? O11 C36 C37 C38 -21.4(8) . . . . ? O12 C36 C37 C38 160.2(6) . . . . ? C36 C37 C38 C39 168.8(6) . . . . ? C37 C38 C39 C40 81.6(11) . . . . ? C38 C39 C40 C41 176.0(8) . . . . ? Rh3 O13 C42 O14 0.3(7) . . . . ? Rh3 O13 C42 C43 -178.5(3) . . . . ? Rh4 O14 C42 O13 4.6(7) . . . . ? Rh4 O14 C42 C43 -176.5(3) . . . . ? O13 C42 C43 C44 -51.5(9) . . . . ? O14 C42 C43 C44 129.5(8) . . . . ? C42 C43 C44 C45 171.7(9) . . . . ? C43 C44 C45 C46 -143.0(14) . . . . ? C44 C45 C46 C47 179.8(12) . . . . ? Rh4 O16 C48 O15 -3.8(7) . . . . ? Rh4 O16 C48 C49 173.8(3) . . . . ? Rh3 O15 C48 O16 9.5(6) . . . . ? Rh2 O15 C48 O16 176.7(3) . . . . ? Rh3 O15 C48 C49 -168.2(3) . . . . ? Rh2 O15 C48 C49 -1.0(7) . . . . ? O16 C48 C49 C50 -92.9(6) . . . . ? O15 C48 C49 C50 84.9(6) . . . . ? C48 C49 C50 C51 -170.7(5) . . . . ? C49 C50 C51 C52 -60.6(9) . . . . ? C50 C51 C52 C53 178.7(7) . . . . ? C58 N2 C54 C55 0.5(7) . . . . ? Rh4 N2 C54 C55 -174.5(4) . . . . ? N2 C54 C55 C56 0.5(8) . . . . ? C54 C55 C56 C57 -1.1(8) . . . . ? C55 C56 C57 C58 0.7(8) . . . . ? C54 N2 C58 C57 -0.9(7) . . . . ? Rh4 N2 C58 C57 174.0(4) . . . . ? C56 C57 C58 N2 0.4(8) . . . . ?