#------------------------------------------------------------------------------ #$Date: 2019-11-17 09:21:22 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229072 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229961.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_7229961 loop_ _publ_author_name 'Aghabali, Amineh' 'Jun, Sharon' 'Olmstead, Marilyn M.' 'Balch, Alan L.' _publ_section_title ; The directional character of the piperazine double addition product, e{N(CH2CH2)2N}2C60, as a building block for forming crystalline fullerene polymers ; _journal_issue 7 _journal_name_full CrystEngComm _journal_page_first 924 _journal_paper_doi 10.1039/C7CE02117H _journal_volume 20 _journal_year 2018 _chemical_formula_moiety 'C80 H34 N4 O12 Rh3, 0.5(C S2)' _chemical_formula_sum 'C80.5 H34 N4 O12 Rh3 S' _chemical_formula_weight 1589.91 _chemical_name_common '{(e(N2C4H8)2C60)(Rh2(O2CCH3)4)2}n 0.5CS2' _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_Hall '-I 2y' _space_group_name_H-M_alt 'I 1 2/m 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2017-11-03 deposited with the CCDC. 2018-01-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.063(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.8849(8) _cell_length_b 18.9471(10) _cell_length_c 19.6812(18) _cell_measurement_reflns_used 9829 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 71.32 _cell_measurement_theta_min 3.58 _cell_volume 5923.5(7) _computing_cell_refinement 'SAINT (Bruker, 2013)' _computing_data_collection 'Apex2 (Bruker, 2014)' _computing_data_reduction 'SAINT (Bruker, 2013)' _computing_publication_material 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT (Sheldrick, 2014)' _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_unetI/netI 0.0300 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 33873 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 63.722 _diffrn_reflns_theta_max 63.722 _diffrn_reflns_theta_min 3.238 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 7.662 _exptl_absorpt_correction_T_max 0.7537 _exptl_absorpt_correction_T_min 0.5158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS-2014/3 _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.783 _exptl_crystal_description block _exptl_crystal_F_000 3168 _exptl_crystal_size_max 0.105 _exptl_crystal_size_mid 0.103 _exptl_crystal_size_min 0.079 _refine_diff_density_max 1.759 _refine_diff_density_min -1.903 _refine_diff_density_rms 0.198 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 500 _refine_ls_number_reflns 4926 _refine_ls_number_restraints 473 _refine_ls_restrained_S_all 1.163 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0762 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+137.7951P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2016 _refine_ls_wR_factor_ref 0.2055 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4699 _reflns_number_total 4926 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce02117h1.cif _cod_data_source_block aa97 _cod_depositor_comments ; Updating space group information. Antanas Vaitkus, 2018-07-22 Adding full bibliography for 7229960--7229961.cif. ; _cod_original_sg_symbol_H-M 'I 2/m' _cod_original_formula_sum 'C80.50 H34 N4 O12 Rh3 S' _cod_database_code 7229961 _shelx_shelxl_version_number 2017/1 _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 0.514 _shelx_estimated_absorpt_t_max 0.595 _shelx_res_file ; TITL aa97 {(e(N2C4H8)2C60)(Rh2(O2CCH3)4)2}n 0.5CS2 aa97.res created by SHELXL-2017/1 at 13:46:28 on 18-Oct-2017 CELL 1.54178 15.8849 18.9471 19.6812 90 90.063 90 ZERR 4 0.0008 0.001 0.0018 0 0.002 0 LATT 2 SYMM -X,+Y,-Z SFAC C H N O Rh S UNIT 322 136 16 48 12 4 L.S. 12 omit 0 1 1 omit 1 1 0 omit -1 0 1 TEMP -183 BOND $H MORE -1 DFIX 1.56 .01 C39 c40 c41 c42 c45 c46 C47 c48 CONF acta simu 0.008 WGHT 0.095000 137.795105 BASF 0.47546 FVAR 3.36677 RH1 5 0.721517 0.308740 0.748596 11.00000 0.01591 0.00860 = 0.07463 0.00051 0.01627 0.00170 RH2 5 0.073417 0.500000 0.985006 10.50000 0.03653 0.03430 = 0.08011 0.00000 0.03313 0.00000 PART 1 O1 4 0.614264 0.268656 0.789556 10.50000 0.03117 0.02748 = 0.04687 0.00647 0.00484 0.00594 O2 4 0.662589 0.158615 0.779476 10.50000 0.03097 0.02120 = 0.04690 0.00158 -0.00180 0.00173 O3 4 0.769339 0.314202 0.845170 10.50000 0.04430 0.03545 = 0.04501 0.00006 -0.00341 0.00421 O4 4 0.818990 0.199791 0.842191 10.50000 0.04147 0.03395 = 0.04227 0.00071 0.00190 0.00525 PART 2 O5 4 0.702676 0.303429 0.850567 10.50000 0.03555 0.02883 = 0.04368 0.00129 0.00433 0.00761 O6 4 0.760475 0.195717 0.857070 10.50000 0.03704 0.02928 = 0.04079 -0.00103 -0.00143 0.00489 O7 4 0.605474 0.260544 0.731972 10.50000 0.02339 0.01613 = 0.04267 0.00273 0.00130 0.00581 O8 4 0.663367 0.152093 0.737804 10.50000 0.02615 0.01843 = 0.03530 0.00409 -0.00262 0.00321 PART 0 O9 4 0.034293 0.500000 0.886009 10.50000 0.05764 0.08819 = 0.08513 0.00000 0.02166 0.00000 O10 4 -0.101894 0.500000 0.913837 10.50000 0.06625 0.10827 = 0.07759 0.00000 0.02663 0.00000 O12 4 0.069795 0.396212 0.986351 11.00000 0.07552 0.05803 = 0.10173 0.01180 0.03392 0.00073 N1 3 0.673723 0.430946 0.742259 11.00000 0.01447 0.01155 = 0.06588 0.00170 0.01275 -0.00173 N2 3 0.228379 0.500000 0.963076 10.50000 0.04178 0.09559 = 0.07936 0.00000 0.03002 0.00000 N3 3 0.390334 0.500000 0.976962 10.50000 0.04490 0.11020 = 0.08627 0.00000 0.02632 0.00000 C1 1 0.369652 0.500000 0.902144 10.50000 0.03307 0.07568 = 0.08012 0.00000 0.03137 0.00000 C2 1 0.267559 0.500000 0.896014 10.50000 0.02947 0.06762 = 0.07901 0.00000 0.03141 0.00000 C3 1 0.232961 0.438140 0.852678 11.00000 0.02057 0.03710 = 0.08490 0.00798 0.02939 -0.00340 C4 1 0.168557 0.462526 0.806675 11.00000 0.02019 0.02876 = 0.09069 -0.00078 0.02300 -0.00508 C5 1 0.148707 0.424695 0.747764 11.00000 0.01955 0.03204 = 0.10170 -0.00760 0.01796 -0.00598 C6 1 0.130228 0.463607 0.685372 11.00000 0.02496 0.04606 = 0.09979 -0.01144 0.01700 -0.00653 C7 1 0.165369 0.426851 0.630144 11.00000 0.03509 0.06138 = 0.10627 -0.01570 0.01144 -0.00572 C8 1 0.199116 0.462592 0.574631 11.00000 0.04035 0.08535 = 0.10149 -0.02059 0.01112 -0.00092 C9 1 0.277425 0.438189 0.545879 11.00000 0.04284 0.08838 = 0.09541 -0.02185 0.01314 -0.00016 C10 1 0.324521 0.500000 0.530513 10.50000 0.03962 0.08747 = 0.09041 0.00000 0.01368 0.00000 C11 1 0.414845 0.500000 0.541078 10.50000 0.03510 0.07973 = 0.08780 0.00000 0.01576 0.00000 C12 1 0.455870 0.438104 0.569923 11.00000 0.03334 0.06584 = 0.08203 -0.01436 0.01479 0.00175 C13 1 0.525447 0.462103 0.611547 11.00000 0.02488 0.04748 = 0.07781 -0.01068 0.01956 -0.00204 C14 1 0.545761 0.424664 0.670598 11.00000 0.02138 0.02295 = 0.08207 -0.01160 0.01607 0.00088 C15 1 0.584328 0.457002 0.733719 11.00000 0.01791 0.01016 = 0.07394 -0.00434 0.01494 0.00159 C16 1 0.528341 0.424357 0.788767 11.00000 0.02116 0.01131 = 0.08091 -0.00198 0.01680 -0.00411 C17 1 0.491667 0.460453 0.841025 11.00000 0.02184 0.03098 = 0.07948 0.00368 0.01892 -0.00590 C18 1 0.413692 0.439244 0.868943 11.00000 0.02669 0.04615 = 0.08102 0.01221 0.02436 -0.00524 C19 1 0.372835 0.380450 0.845014 11.00000 0.02594 0.03102 = 0.09685 0.01547 0.02563 0.00043 C20 1 0.278852 0.379797 0.833573 11.00000 0.02151 0.03061 = 0.09940 0.01827 0.02237 -0.00386 C21 1 0.260803 0.341027 0.773699 11.00000 0.02393 0.01805 = 0.10800 0.00543 0.01624 -0.01009 C22 1 0.197766 0.363241 0.731656 11.00000 0.02250 0.02472 = 0.10882 -0.00927 0.01722 -0.00934 C23 1 0.205434 0.362102 0.657213 11.00000 0.03009 0.04278 = 0.11165 -0.01891 0.01289 -0.00917 C24 1 0.282170 0.341417 0.628251 11.00000 0.03596 0.04601 = 0.10850 -0.02832 0.01489 -0.01085 C25 1 0.316158 0.379093 0.574078 11.00000 0.03848 0.07057 = 0.09777 -0.03699 0.01041 -0.00849 C26 1 0.410529 0.380705 0.583907 11.00000 0.03424 0.06282 = 0.09637 -0.03270 0.01171 -0.00208 C27 1 0.429117 0.340341 0.644864 11.00000 0.03301 0.03427 = 0.10593 -0.02610 0.01589 -0.00387 C28 1 0.495452 0.364790 0.689886 11.00000 0.02367 0.01771 = 0.09412 -0.01817 0.01663 0.00447 C29 1 0.486268 0.365234 0.761995 11.00000 0.02183 0.00820 = 0.09308 -0.00380 0.01681 -0.00029 C30 1 0.409358 0.342612 0.788606 11.00000 0.02465 0.01809 = 0.10558 0.00297 0.02202 -0.00336 C31 1 0.340934 0.318424 0.744600 11.00000 0.02859 0.01500 = 0.11053 -0.00395 0.01644 -0.00449 C32 1 0.350450 0.317085 0.676200 11.00000 0.03381 0.02326 = 0.11269 -0.02318 0.01470 -0.00824 C33 1 0.352242 0.435547 1.008065 11.00000 0.04950 0.12242 = 0.08764 0.01494 0.02982 0.00741 AFIX 23 H33A 2 0.368160 0.432922 1.056647 11.00000 -1.20000 H33B 2 0.374452 0.392988 0.985056 11.00000 -1.20000 AFIX 0 C34 1 0.258372 0.437047 1.001832 11.00000 0.04586 0.11739 = 0.08988 0.01232 0.03045 0.01068 AFIX 23 H34A 2 0.239142 0.393623 0.978538 11.00000 -1.20000 H34B 2 0.233175 0.437614 1.047814 11.00000 -1.20000 AFIX 0 C35 1 0.710673 0.459527 0.809828 11.00000 0.01929 0.01747 = 0.06040 0.00479 0.01179 0.00079 AFIX 23 H35A 2 0.676657 0.442029 0.848434 11.00000 -1.20000 H35B 2 0.768968 0.442033 0.815615 11.00000 -1.20000 AFIX 0 C36 1 0.724308 0.459932 0.687171 11.00000 0.02787 0.01522 = 0.05692 -0.00181 0.01487 -0.00520 AFIX 23 H36A 2 0.701930 0.442764 0.643209 11.00000 -1.20000 H36B 2 0.782912 0.442765 0.691684 11.00000 -1.20000 AFIX 0 PART 1 C37 1 0.607080 0.208758 0.799998 10.50000 0.03517 C38 1 0.518661 0.176021 0.817920 10.50000 0.07896 AFIX 137 H38A 2 0.517570 0.126256 0.804376 10.50000 -1.50000 H38B 2 0.474432 0.201761 0.793569 10.50000 -1.50000 H38C 2 0.508989 0.179686 0.866963 10.50000 -1.50000 AFIX 0 C39 1 0.809425 0.256691 0.874802 10.50000 0.04183 C40 1 0.865556 0.269034 0.938829 10.50000 0.08584 AFIX 33 H40A 2 0.851741 0.314832 0.959094 10.50000 -1.50000 H40B 2 0.855176 0.231494 0.972034 10.50000 -1.50000 H40C 2 0.925000 0.268526 0.925568 10.50000 -1.50000 AFIX 0 PART 2 C41 1 0.724459 0.250810 0.881529 10.50000 0.03562 C42 1 0.710328 0.251991 0.959655 10.50000 0.03747 AFIX 137 H42A 2 0.692906 0.205016 0.975020 10.50000 -1.50000 H42B 2 0.666335 0.286368 0.970727 10.50000 -1.50000 H42C 2 0.762831 0.265334 0.982475 10.50000 -1.50000 AFIX 0 C43 1 0.598408 0.194573 0.728448 10.50000 0.02989 C44 1 0.517005 0.164236 0.717133 10.50000 0.04947 AFIX 137 H44A 2 0.521945 0.124695 0.685287 10.50000 -1.50000 H44B 2 0.479281 0.200050 0.698030 10.50000 -1.50000 H44C 2 0.494091 0.147207 0.760341 10.50000 -1.50000 AFIX 0 PART 0 C45 1 -0.040369 0.500000 0.877591 10.50000 0.08496 C46 1 -0.067645 0.500000 0.801329 10.50000 0.13880 AFIX 1 H46A 2 -0.016620 0.500000 0.770170 10.50000 -1.50000 H46B 2 -0.098970 0.458630 0.788560 11.00000 -1.50000 AFIX 0 C47 1 0.000000 0.362675 1.000000 10.50000 0.08755 C48 1 0.000000 0.280036 1.000000 10.50000 0.16356 AFIX 33 H48A 2 0.056515 0.262796 0.988948 10.50000 -1.50000 H48B 2 -0.016345 0.262796 1.045040 10.50000 -1.50000 H48C 2 -0.040171 0.262795 0.966013 10.50000 -1.50000 AFIX 0 PART -2 C49 1 0.537968 0.146336 0.894176 10.25000 0.10363 S1 6 0.500926 0.218303 0.902679 10.25000 0.12196 S2 6 0.573322 0.062167 0.919315 10.25000 0.12839 PART 0 HKLF 5 REM aa97 {(e(N2C4H8)2C60)(Rh2(O2CCH3)4)2}n 0.5CS2 REM R1 = 0.0762 for 4699 Fo > 4sig(Fo) and 0.0799 for all 4926 data REM 500 parameters refined using 473 restraints END WGHT 0.0952 137.4351 REM Highest difference peak 1.759, deepest hole -1.903, 1-sigma level 0.198 Q1 1 0.7085 0.3094 0.7988 11.00000 0.05 1.76 Q2 1 0.7783 0.1934 0.8109 11.00000 0.05 1.62 Q3 1 -0.0588 0.5000 0.9570 10.50000 0.05 1.20 Q4 1 0.0780 0.5000 0.9251 10.50000 0.05 1.05 Q5 1 0.6785 0.3093 0.7406 11.00000 0.05 1.05 Q6 1 0.2213 0.5000 0.5148 10.50000 0.05 1.02 Q7 1 0.2954 0.3168 0.7527 11.00000 0.05 0.87 Q8 1 0.0130 0.5334 0.9592 11.00000 0.05 0.86 Q9 1 0.0261 0.3669 1.0269 11.00000 0.05 0.83 Q10 1 0.6787 0.1687 0.6982 11.00000 0.05 0.83 Q11 1 0.1018 0.5271 0.9397 11.00000 0.05 0.83 Q12 1 0.5169 0.1692 0.7579 11.00000 0.05 0.82 Q13 1 -0.0382 0.2899 0.9594 11.00000 0.05 0.81 Q14 1 0.5747 0.0000 0.9312 10.50000 0.05 0.81 Q15 1 0.7548 0.3314 0.7063 11.00000 0.05 0.81 Q16 1 0.5468 0.0000 0.9751 10.50000 0.05 0.78 Q17 1 0.2199 0.5000 0.4567 10.50000 0.05 0.77 Q18 1 0.0385 0.3834 0.9547 11.00000 0.05 0.75 Q19 1 -0.0197 0.5243 0.9262 11.00000 0.05 0.73 Q20 1 -0.0896 0.5347 0.9225 11.00000 0.05 0.72 ; _shelx_res_checksum 18693 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z' 3 'x+1/2, y+1/2, z+1/2' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z' 7 '-x+1/2, -y+1/2, -z+1/2' 8 'x+1/2, -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 0.72152(4) 0.30874(3) 0.74860(6) 0.0330(3) Uani 1 1 d . . . . . Rh2 Rh 0.07342(9) 0.500000 0.98501(10) 0.0503(5) Uani 1 2 d S TU P . . O1 O 0.6143(10) 0.2687(9) 0.7896(9) 0.035(2) Uani 0.5 1 d . U P A 1 O2 O 0.6626(11) 0.1586(9) 0.7795(10) 0.033(2) Uani 0.5 1 d . U P A 1 O3 O 0.7693(13) 0.3142(9) 0.8452(9) 0.042(3) Uani 0.5 1 d . U P A 1 O4 O 0.8190(13) 0.1998(9) 0.8422(9) 0.039(3) Uani 0.5 1 d . U P A 1 O5 O 0.7027(11) 0.3034(9) 0.8506(9) 0.036(2) Uani 0.5 1 d . U P A 2 O6 O 0.7605(12) 0.1957(9) 0.8571(9) 0.036(3) Uani 0.5 1 d . U P A 2 O7 O 0.6055(9) 0.2605(7) 0.7320(8) 0.027(2) Uani 0.5 1 d . U P A 2 O8 O 0.6634(9) 0.1521(8) 0.7378(9) 0.027(2) Uani 0.5 1 d . U P A 2 O9 O 0.0343(11) 0.500000 0.8860(10) 0.077(4) Uani 1 2 d S TU P . . O10 O -0.1019(12) 0.500000 0.9138(10) 0.084(4) Uani 1 2 d S TU P . . O12 O 0.0698(9) 0.3962(6) 0.9864(8) 0.078(3) Uani 1 1 d . U . . . N1 N 0.6737(5) 0.4309(4) 0.7423(6) 0.0306(17) Uani 1 1 d . U . . . N2 N 0.2284(13) 0.500000 0.9631(11) 0.072(3) Uani 1 2 d S TU P . . N3 N 0.3903(13) 0.500000 0.9770(13) 0.080(4) Uani 1 2 d S TU P . . C1 C 0.3697(14) 0.500000 0.9021(13) 0.063(3) Uani 1 2 d S TU P . . C2 C 0.2676(13) 0.500000 0.8960(12) 0.059(3) Uani 1 2 d S TU P . . C3 C 0.2330(7) 0.4381(7) 0.8527(8) 0.048(2) Uani 1 1 d . U . . . C4 C 0.1686(8) 0.4625(7) 0.8067(9) 0.047(2) Uani 1 1 d . U . . . C5 C 0.1487(7) 0.4247(6) 0.7478(11) 0.051(2) Uani 1 1 d . U . . . C6 C 0.1302(9) 0.4636(8) 0.6854(10) 0.057(3) Uani 1 1 d . U . . . C7 C 0.1654(10) 0.4269(10) 0.6301(11) 0.068(3) Uani 1 1 d . U . . . C8 C 0.1991(10) 0.4626(11) 0.5746(11) 0.076(3) Uani 1 1 d . U . . . C9 C 0.2774(11) 0.4382(11) 0.5459(10) 0.076(3) Uani 1 1 d . U . . . C10 C 0.3245(15) 0.500000 0.5305(15) 0.072(4) Uani 1 2 d S TU P . . C11 C 0.4148(14) 0.500000 0.5411(14) 0.068(4) Uani 1 2 d S TU P . . C12 C 0.4559(9) 0.4381(9) 0.5699(9) 0.060(3) Uani 1 1 d . U . . . C13 C 0.5254(8) 0.4621(8) 0.6115(8) 0.050(3) Uani 1 1 d . U . . . C14 C 0.5458(7) 0.4247(6) 0.6706(8) 0.042(2) Uani 1 1 d . U . . . C15 C 0.5843(6) 0.4570(5) 0.7337(7) 0.034(2) Uani 1 1 d . U . . . C16 C 0.5283(7) 0.4244(6) 0.7888(7) 0.038(2) Uani 1 1 d . U . . . C17 C 0.4917(8) 0.4605(6) 0.8410(8) 0.044(2) Uani 1 1 d . U . . . C18 C 0.4137(8) 0.4392(8) 0.8689(8) 0.051(2) Uani 1 1 d . U . . . C19 C 0.3728(8) 0.3805(7) 0.8450(8) 0.051(2) Uani 1 1 d . U . . . C20 C 0.2789(8) 0.3798(7) 0.8336(8) 0.050(2) Uani 1 1 d . U . . . C21 C 0.2608(7) 0.3410(6) 0.7737(8) 0.050(2) Uani 1 1 d . U . . . C22 C 0.1978(7) 0.3632(6) 0.7317(9) 0.052(2) Uani 1 1 d . U . . . C23 C 0.2054(9) 0.3621(8) 0.6572(10) 0.061(3) Uani 1 1 d . U . . . C24 C 0.2822(10) 0.3414(8) 0.6283(10) 0.063(2) Uani 1 1 d . U . . . C25 C 0.3162(10) 0.3791(10) 0.5741(10) 0.069(3) Uani 1 1 d . U . . . C26 C 0.4105(9) 0.3807(10) 0.5839(10) 0.064(3) Uani 1 1 d . U . . . C27 C 0.4291(9) 0.3403(7) 0.6449(10) 0.058(2) Uani 1 1 d . U . . . C28 C 0.4955(8) 0.3648(6) 0.6899(9) 0.045(2) Uani 1 1 d . U . . . C29 C 0.4863(7) 0.3652(5) 0.7620(8) 0.041(2) Uani 1 1 d . U . . . C30 C 0.4094(8) 0.3426(6) 0.7886(9) 0.049(2) Uani 1 1 d . U . . . C31 C 0.3409(7) 0.3184(5) 0.7446(11) 0.051(2) Uani 1 1 d . U . . . C32 C 0.3505(9) 0.3171(7) 0.6762(10) 0.057(2) Uani 1 1 d . U . . . C33 C 0.3522(11) 0.4355(12) 1.0081(11) 0.086(4) Uani 1 1 d . U . . . H33A H 0.368160 0.432922 1.056647 0.104 Uiso 1 1 calc R U . . . H33B H 0.374452 0.392988 0.985056 0.104 Uiso 1 1 calc R U . . . C34 C 0.2584(10) 0.4370(12) 1.0018(10) 0.084(4) Uani 1 1 d . U . . . H34A H 0.239142 0.393623 0.978538 0.101 Uiso 1 1 calc R U . . . H34B H 0.233175 0.437614 1.047814 0.101 Uiso 1 1 calc R U . . . C35 C 0.7107(7) 0.4595(6) 0.8098(7) 0.032(2) Uani 1 1 d . U . . . H35A H 0.676657 0.442029 0.848434 0.039 Uiso 1 1 calc R U . . . H35B H 0.768968 0.442033 0.815615 0.039 Uiso 1 1 calc R U . . . C36 C 0.7243(8) 0.4599(5) 0.6872(7) 0.033(2) Uani 1 1 d . U . . . H36A H 0.701930 0.442764 0.643209 0.040 Uiso 1 1 calc R U . . . H36B H 0.782912 0.442765 0.691684 0.040 Uiso 1 1 calc R U . . . C37 C 0.6071(16) 0.2088(14) 0.8000(13) 0.035(2) Uiso 0.5 1 d . U P A 1 C38 C 0.519(3) 0.176(2) 0.818(2) 0.079(7) Uiso 0.5 1 d . U P A 1 H38A H 0.517570 0.126256 0.804376 0.118 Uiso 0.5 1 calc R U P A 1 H38B H 0.474432 0.201761 0.793569 0.118 Uiso 0.5 1 calc R U P A 1 H38C H 0.508989 0.179686 0.866963 0.118 Uiso 0.5 1 calc R U P A 1 C39 C 0.8094(16) 0.2567(14) 0.8748(13) 0.042(3) Uiso 0.5 1 d D U P A 1 C40 C 0.866(2) 0.269(2) 0.9388(16) 0.086(10) Uiso 0.5 1 d D U P A 1 H40A H 0.851741 0.314832 0.959094 0.129 Uiso 0.5 1 calc R U P A 1 H40B H 0.855176 0.231494 0.972034 0.129 Uiso 0.5 1 calc R U P A 1 H40C H 0.925000 0.268526 0.925568 0.129 Uiso 0.5 1 calc R U P A 1 C41 C 0.7245(15) 0.2508(13) 0.8815(9) 0.036(2) Uiso 0.5 1 d D U P A 2 C42 C 0.7103(16) 0.2520(13) 0.9597(9) 0.037(5) Uiso 0.5 1 d D U P A 2 H42A H 0.692906 0.205016 0.975020 0.056 Uiso 0.5 1 calc R U P A 2 H42B H 0.666335 0.286368 0.970727 0.056 Uiso 0.5 1 calc R U P A 2 H42C H 0.762831 0.265334 0.982475 0.056 Uiso 0.5 1 calc R U P A 2 C43 C 0.5984(15) 0.1946(12) 0.7284(11) 0.030(2) Uiso 0.5 1 d . U P A 2 C44 C 0.5170(19) 0.1642(16) 0.7171(16) 0.049(6) Uiso 0.5 1 d . U P A 2 H44A H 0.521945 0.124695 0.685287 0.074 Uiso 0.5 1 calc R U P A 2 H44B H 0.479281 0.200050 0.698030 0.074 Uiso 0.5 1 calc R U P A 2 H44C H 0.494091 0.147207 0.760341 0.074 Uiso 0.5 1 calc R U P A 2 C45 C -0.040(2) 0.500000 0.8776(15) 0.085(4) Uiso 1 2 d DS U P . . C46 C -0.068(3) 0.500000 0.8013(16) 0.139(11) Uiso 1 2 d DS U P . . H46A H -0.016620 0.500000 0.770170 0.208 Uiso 1 2 d S U P . . H46B H -0.098970 0.458630 0.788560 0.208 Uiso 1 1 d . U . . . C47 C 0.000000 0.3627(16) 1.000000 0.088(5) Uiso 1 2 d DS U P . . C48 C 0.000000 0.2800(16) 1.000000 0.164(13) Uiso 1 2 d DS U P . . H48A H 0.056515 0.262796 0.988948 0.245 Uiso 0.5 1 calc R U P . . H48B H -0.016345 0.262796 1.045040 0.245 Uiso 0.5 1 calc R U P . . H48C H -0.040171 0.262795 0.966013 0.245 Uiso 0.5 1 calc R U P . . C49 C 0.538(7) 0.146(6) 0.894(5) 0.104(10) Uiso 0.25 1 d . U P B -2 S1 S 0.501(2) 0.2183(18) 0.9027(18) 0.122(8) Uiso 0.25 1 d . U P B -2 S2 S 0.573(2) 0.0622(19) 0.9193(18) 0.128(9) Uiso 0.25 1 d . U P B -2 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 0.0159(4) 0.0086(4) 0.0746(6) 0.0005(4) 0.0163(7) 0.0017(3) Rh2 0.0365(8) 0.0343(7) 0.0801(11) 0.000 0.0331(8) 0.000 O1 0.031(4) 0.027(4) 0.047(4) 0.006(4) 0.005(4) 0.006(4) O2 0.031(4) 0.021(4) 0.047(5) 0.002(4) -0.002(5) 0.002(4) O3 0.044(5) 0.035(5) 0.045(5) 0.000(4) -0.003(4) 0.004(4) O4 0.041(5) 0.034(4) 0.042(5) 0.001(4) 0.002(4) 0.005(4) O5 0.036(4) 0.029(4) 0.044(4) 0.001(4) 0.004(4) 0.008(4) O6 0.037(5) 0.029(4) 0.041(5) -0.001(4) -0.001(4) 0.005(4) O7 0.023(4) 0.016(4) 0.043(5) 0.003(4) 0.001(4) 0.006(4) O8 0.026(4) 0.018(4) 0.035(5) 0.004(4) -0.003(4) 0.003(4) O9 0.058(7) 0.088(7) 0.085(7) 0.000 0.022(6) 0.000 O10 0.066(7) 0.108(8) 0.078(7) 0.000 0.027(6) 0.000 O12 0.076(5) 0.058(4) 0.102(5) 0.012(4) 0.034(4) 0.001(4) N1 0.014(3) 0.012(3) 0.066(4) 0.002(4) 0.013(4) -0.002(3) N2 0.042(6) 0.096(7) 0.079(7) 0.000 0.030(6) 0.000 N3 0.045(6) 0.110(8) 0.086(7) 0.000 0.026(6) 0.000 C1 0.033(5) 0.076(6) 0.080(6) 0.000 0.031(5) 0.000 C2 0.029(5) 0.068(6) 0.079(6) 0.000 0.031(5) 0.000 C3 0.021(4) 0.037(4) 0.085(5) 0.008(4) 0.029(4) -0.003(4) C4 0.020(4) 0.029(5) 0.091(6) -0.001(5) 0.023(5) -0.005(4) C5 0.020(4) 0.032(4) 0.102(6) -0.008(5) 0.018(5) -0.006(3) C6 0.025(5) 0.046(5) 0.100(6) -0.011(5) 0.017(5) -0.007(4) C7 0.035(5) 0.061(5) 0.106(6) -0.016(5) 0.011(5) -0.006(4) C8 0.040(6) 0.085(6) 0.101(7) -0.021(6) 0.011(5) -0.001(5) C9 0.043(5) 0.088(6) 0.095(6) -0.022(5) 0.013(5) 0.000(5) C10 0.040(6) 0.087(7) 0.090(7) 0.000 0.014(6) 0.000 C11 0.035(6) 0.080(7) 0.088(7) 0.000 0.016(6) 0.000 C12 0.033(5) 0.066(5) 0.082(6) -0.014(5) 0.015(5) 0.002(4) C13 0.025(5) 0.047(5) 0.078(6) -0.011(5) 0.020(5) -0.002(4) C14 0.021(4) 0.023(4) 0.082(5) -0.012(4) 0.016(4) 0.001(4) C15 0.018(4) 0.010(4) 0.074(5) -0.004(4) 0.015(4) 0.002(3) C16 0.021(4) 0.011(4) 0.081(5) -0.002(4) 0.017(4) -0.004(3) C17 0.022(4) 0.031(5) 0.079(6) 0.004(5) 0.019(4) -0.006(4) C18 0.027(4) 0.046(5) 0.081(5) 0.012(4) 0.024(4) -0.005(4) C19 0.026(4) 0.031(4) 0.097(5) 0.015(4) 0.026(4) 0.000(4) C20 0.022(4) 0.031(4) 0.099(5) 0.018(4) 0.022(4) -0.004(4) C21 0.024(4) 0.018(4) 0.108(6) 0.005(4) 0.016(4) -0.010(4) C22 0.023(4) 0.025(4) 0.109(6) -0.009(4) 0.017(4) -0.009(4) C23 0.030(4) 0.043(5) 0.112(6) -0.019(5) 0.013(5) -0.009(4) C24 0.036(4) 0.046(5) 0.108(6) -0.028(5) 0.015(5) -0.011(4) C25 0.038(5) 0.071(5) 0.098(6) -0.037(5) 0.010(5) -0.008(4) C26 0.034(5) 0.063(5) 0.096(6) -0.033(5) 0.012(5) -0.002(4) C27 0.033(4) 0.034(4) 0.106(5) -0.026(4) 0.016(5) -0.004(4) C28 0.024(4) 0.018(4) 0.094(5) -0.018(4) 0.017(4) 0.004(4) C29 0.022(4) 0.008(3) 0.093(5) -0.004(4) 0.017(4) 0.000(3) C30 0.025(4) 0.018(4) 0.106(5) 0.003(4) 0.022(4) -0.003(3) C31 0.029(4) 0.015(4) 0.111(5) -0.004(5) 0.016(5) -0.004(3) C32 0.034(4) 0.023(4) 0.113(6) -0.023(4) 0.015(5) -0.008(4) C33 0.049(6) 0.122(8) 0.088(7) 0.015(6) 0.030(6) 0.007(5) C34 0.046(6) 0.117(8) 0.090(7) 0.012(6) 0.030(6) 0.011(5) C35 0.019(5) 0.017(5) 0.060(6) 0.005(4) 0.012(5) 0.001(4) C36 0.028(5) 0.015(5) 0.057(6) -0.002(4) 0.015(5) -0.005(4) 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' 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' S S 0.3331 0.5567 '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 O4 Rh1 O8 117.8(8) 7_656 7_656 O4 Rh1 O2 94.4(8) 7_656 7_656 O8 Rh1 O5 91.3(7) 7_656 . O4 Rh1 O1 93.3(8) 7_656 . O2 Rh1 O1 170.9(7) 7_656 . O4 Rh1 O3 177.2(7) 7_656 . O2 Rh1 O3 84.3(8) 7_656 . O1 Rh1 O3 87.8(8) . . O8 Rh1 O7 175.6(6) 7_656 . O5 Rh1 O7 90.1(7) . . O4 Rh1 O6 27.7(7) 7_656 7_656 O2 Rh1 O6 67.4(8) 7_656 7_656 O1 Rh1 O6 119.5(7) . 7_656 O3 Rh1 O6 150.4(8) . 7_656 O4 Rh1 Rh1 94.0(5) 7_656 7_656 O2 Rh1 Rh1 86.9(5) 7_656 7_656 O1 Rh1 Rh1 87.7(5) . 7_656 O3 Rh1 Rh1 83.5(5) . 7_656 O4 Rh1 N1 85.9(6) 7_656 . O8 Rh1 N1 86.5(5) 7_656 . O2 Rh1 N1 88.8(5) 7_656 . O5 Rh1 N1 92.9(5) . . O1 Rh1 N1 96.5(5) . . O3 Rh1 N1 96.6(6) . . O7 Rh1 N1 97.6(4) . . O6 Rh1 N1 91.7(5) 7_656 . Rh1 Rh1 N1 175.72(19) 7_656 . O12 Rh2 O12 176.3(7) . 6_565 O12 Rh2 O10 89.6(5) . 5_567 O12 Rh2 O10 89.6(5) 6_565 5_567 O12 Rh2 O9 90.2(5) . . O12 Rh2 O9 90.2(5) 6_565 . O10 Rh2 O9 175.1(7) 5_567 . O12 Rh2 Rh2 88.2(4) . 5_567 O12 Rh2 Rh2 88.2(4) 6_565 5_567 O10 Rh2 Rh2 88.5(5) 5_567 5_567 O9 Rh2 Rh2 86.6(5) . 5_567 O12 Rh2 N2 91.8(4) . . O12 Rh2 N2 91.8(4) 6_565 . O10 Rh2 N2 87.2(7) 5_567 . O9 Rh2 N2 97.7(7) . . Rh2 Rh2 N2 175.7(6) 5_567 . C37 O1 Rh1 121.3(17) . . C37 O2 Rh1 117.4(15) . 7_656 C39 O3 Rh1 121.3(15) . . C39 O4 Rh1 120.5(17) . 7_656 C41 O5 Rh1 119.5(14) . . C43 O7 Rh1 121.6(14) . . C45 O9 Rh2 115.6(18) . . C45 O10 Rh2 113(2) . 5_567 C47 O12 Rh2 120.9(14) . . C36 N1 C15 108.2(10) . . C36 N1 C35 107.3(8) . . C15 N1 C35 109.6(9) . . C36 N1 Rh1 102.9(6) . . C15 N1 Rh1 127.4(6) . . C35 N1 Rh1 99.8(6) . . C2 N2 C34 109.0(12) . 6_565 C2 N2 C34 109.0(12) . . C34 N2 C34 106(2) 6_565 . C2 N2 Rh2 125.2(16) . . C34 N2 Rh2 103.0(9) 6_565 . C34 N2 Rh2 103.0(9) . . C33 N3 C33 110(2) . 6_565 C33 N3 C1 108.2(16) . . C33 N3 C1 108.2(16) 6_565 . C18 C1 C18 100.5(14) 6_565 . C18 C1 N3 108.9(15) 6_565 . C18 C1 N3 108.9(15) . . C18 C1 C2 115.7(14) 6_565 . C18 C1 C2 115.7(14) . . N3 C1 C2 106.8(16) . . N2 C2 C3 110.3(11) . . N2 C2 C3 110.3(11) . 6_565 C3 C2 C3 98.3(18) . 6_565 N2 C2 C1 111(2) . . C3 C2 C1 113.2(10) . . C3 C2 C1 113.2(10) 6_565 . C20 C3 C4 117.5(14) . . C20 C3 C2 124.7(13) . . C4 C3 C2 110.7(13) . . C5 C4 C4 120.8(9) . 6_565 C5 C4 C3 121.0(12) . . C4 C4 C3 108.7(7) 6_565 . C4 C5 C22 118.4(15) . . C4 C5 C6 118.9(12) . . C22 C5 C6 109.4(15) . . C6 C6 C7 119.7(10) 6_565 . C6 C6 C5 120.3(8) 6_565 . C7 C6 C5 108.7(15) . . C8 C7 C6 121.2(17) . . C8 C7 C23 121.3(15) . . C6 C7 C23 107.6(18) . . C7 C8 C8 119.1(11) . 6_565 C7 C8 C9 119.0(19) . . C8 C8 C9 108.7(12) 6_565 . C25 C9 C10 121.0(18) . . C25 C9 C8 118.8(18) . . C10 C9 C8 105.9(17) . . C9 C10 C9 111(2) . 6_565 C9 C10 C11 119.4(15) . . C9 C10 C11 119.4(15) 6_565 . C10 C11 C12 119.9(11) . . C10 C11 C12 119.9(11) . 6_565 C12 C11 C12 107(2) . 6_565 C26 C12 C13 123.5(18) . . C26 C12 C11 119.7(15) . . C13 C12 C11 108.0(16) . . C14 C13 C13 120.5(8) . 6_565 C14 C13 C12 119.1(13) . . C13 C13 C12 108.3(10) 6_565 . C13 C14 C28 119.4(14) . . C13 C14 C15 124.7(11) . . C28 C14 C15 109.1(13) . . N1 C15 C14 109.8(9) . . N1 C15 C16 109.6(10) . . C14 C15 C16 100.5(9) . . N1 C15 C15 109.0(5) . 6_565 C14 C15 C15 113.9(6) . 6_565 C16 C15 C15 113.8(6) . 6_565 C17 C16 C29 118.5(10) . . C17 C16 C15 125.3(10) . . C29 C16 C15 109.4(12) . . C16 C17 C18 121.7(13) . . C16 C17 C17 120.0(7) . 6_565 C18 C17 C17 106.5(8) . 6_565 C19 C18 C17 120.8(13) . . C19 C18 C1 123.6(12) . . C17 C18 C1 111.2(12) . . C18 C19 C30 118.5(11) . . C18 C19 C20 121.7(12) . . C30 C19 C20 106.2(14) . . C3 C20 C21 122.4(14) . . C3 C20 C19 118.5(13) . . C21 C20 C19 109.1(12) . . C22 C21 C20 119.5(12) . . C22 C21 C31 119.5(15) . . C20 C21 C31 107.6(12) . . C21 C22 C5 120.9(15) . . C21 C22 C23 122.6(12) . . C5 C22 C23 106.1(15) . . C24 C23 C22 118.8(16) . . C24 C23 C7 117.3(16) . . C22 C23 C7 108.1(13) . . C25 C24 C23 120.4(18) . . C25 C24 C32 110.9(14) . . C23 C24 C32 117.1(17) . . C24 C25 C9 123.1(15) . . C24 C25 C26 107.3(19) . . C9 C25 C26 118.2(17) . . C12 C26 C27 119.4(16) . . C12 C26 C25 121.7(18) . . C27 C26 C25 107.2(16) . . C28 C27 C26 118.9(13) . . C28 C27 C32 117.3(15) . . C26 C27 C32 109.5(15) . . C29 C28 C14 108.4(12) . . C29 C28 C27 122.3(11) . . C14 C28 C27 119.6(15) . . C30 C29 C16 121.3(12) . . C30 C29 C28 117.5(13) . . C16 C29 C28 109.2(11) . . C29 C30 C19 119.2(12) . . C29 C30 C31 121.6(15) . . C19 C30 C31 108.2(11) . . C32 C31 C21 119.6(15) . . C32 C31 C30 120.7(12) . . C21 C31 C30 108.9(14) . . C31 C32 C27 120.6(15) . . C31 C32 C24 122.3(13) . . C27 C32 C24 105.0(15) . . N3 C33 C34 110.8(19) . . N3 C33 H33A 109.5 . . C34 C33 H33A 109.5 . . N3 C33 H33B 109.5 . . C34 C33 H33B 109.5 . . H33A C33 H33B 108.1 . . N2 C34 C33 112.0(17) . . N2 C34 H34A 109.2 . . C33 C34 H34A 109.2 . . N2 C34 H34B 109.2 . . C33 C34 H34B 109.2 . . H34A C34 H34B 107.9 . . C35 C35 N1 110.4(5) 6_565 . C35 C35 H35A 109.6 6_565 . N1 C35 H35A 109.6 . . C35 C35 H35B 109.6 6_565 . N1 C35 H35B 109.6 . . H35A C35 H35B 108.1 . . N1 C36 C36 112.1(5) . 6_565 N1 C36 H36A 109.2 . . C36 C36 H36A 109.2 6_565 . N1 C36 H36B 109.2 . . C36 C36 H36B 109.2 6_565 . H36A C36 H36B 107.9 . . O1 C37 O2 125(2) . . O1 C37 C38 121(3) . . O2 C37 C38 112(2) . . C37 C38 H38A 109.5 . . C37 C38 H38B 109.5 . . H38A C38 H38B 109.5 . . C37 C38 H38C 109.5 . . H38A C38 H38C 109.5 . . H38B C38 H38C 109.5 . . O4 C39 O3 121(2) . . O4 C39 C40 118(3) . . O3 C39 C40 119(3) . . C39 C40 H40A 109.5 . . C39 C40 H40B 109.5 . . H40A C40 H40B 109.5 . . C39 C40 H40C 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . O5 C41 O6 127.2(18) . . O5 C41 C42 116(2) . . O6 C41 C42 117(2) . . C41 C42 H42A 109.5 . . C41 C42 H42B 109.5 . . H42A C42 H42B 109.5 . . C41 C42 H42C 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . O7 C43 O8 122(2) . . O7 C43 C44 119(2) . . O8 C43 C44 119(2) . . C43 C44 H44A 109.5 . . C43 C44 H44B 109.5 . . H44A C44 H44B 109.5 . . C43 C44 H44C 109.5 . . H44A C44 H44C 109.5 . . H44B C44 H44C 109.5 . . O9 C45 O10 136(3) . . O9 C45 C46 114(3) . . O10 C45 C46 110(3) . . C45 C46 H46A 111.0 . . C45 C46 H46B 113.2 . . H46A C46 H46B 104.8 . . C45 C46 H46B 113(2) . 6_565 H46A C46 H46B 104.8 . 6_565 H46B C46 H46B 109.2 . 6_565 O12 C47 O12 122(2) 2_557 . O12 C47 C48 119.1(12) 2_557 . O12 C47 C48 119.1(12) . . C47 C48 H48A 109.5 . . C47 C48 H48B 109.5 . . H48A C48 H48B 109.5 . . C47 C48 H48C 109.5 . . H48A C48 H48C 109.5 . . H48B C48 H48C 109.5 . . C47 C48 H48A 109.470(6) . 2_557 H48A C48 H48A 141.1 . 2_557 H48B C48 H48A 56.2 . 2_557 H48C C48 H48A 56.3 . 2_557 C47 C48 H48B 109.471(10) . 2_557 H48A C48 H48B 56.3 . 2_557 H48B C48 H48B 141.1 . 2_557 H48C C48 H48B 56.2 . 2_557 H48A C48 H48B 109.5 2_557 2_557 C47 C48 H48C 109.472(14) . 2_557 H48A C48 H48C 56.3 . 2_557 H48B C48 H48C 56.2 . 2_557 H48C C48 H48C 141.1 . 2_557 H48A C48 H48C 109.5 2_557 2_557 H48B C48 H48C 109.5 2_557 2_557 S1 C49 S2 157(8) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Rh1 O4 1.91(2) 7_656 Rh1 O8 1.991(15) 7_656 Rh1 O2 2.020(17) 7_656 Rh1 O5 2.032(17) . Rh1 O1 2.033(16) . Rh1 O3 2.049(19) . Rh1 O7 2.083(15) . Rh1 O6 2.101(17) 7_656 Rh1 Rh1 2.4034(13) 7_656 Rh1 N1 2.440(8) . Rh2 O12 1.967(11) . Rh2 O12 1.968(11) 6_565 Rh2 O10 2.04(2) 5_567 Rh2 O9 2.04(2) . Rh2 Rh2 2.407(3) 5_567 Rh2 N2 2.500(19) . O1 C37 1.16(3) . O2 C37 1.36(3) . O3 C39 1.39(3) . O4 C39 1.26(3) . O5 C41 1.22(3) . O6 C41 1.28(3) . O7 C43 1.26(3) . O8 C43 1.32(3) . O9 C45 1.20(3) . O10 C45 1.21(3) . O12 C47 1.306(18) . N1 C36 1.458(15) . N1 C15 1.513(13) . N1 C35 1.551(17) . N2 C2 1.46(3) . N2 C34 1.49(2) 6_565 N2 C34 1.49(2) . N3 C33 1.49(2) . N3 C33 1.49(2) 6_565 N3 C1 1.51(4) . C1 C18 1.497(18) 6_565 C1 C18 1.498(18) . C1 C2 1.63(3) . C2 C3 1.55(2) . C2 C3 1.55(2) 6_565 C3 C20 1.377(18) . C3 C4 1.44(2) . C4 C5 1.40(2) . C4 C4 1.42(3) 6_565 C5 C22 1.437(17) . C5 C6 1.46(3) . C6 C6 1.38(3) 6_565 C6 C7 1.41(2) . C7 C8 1.39(3) . C7 C23 1.48(3) . C8 C8 1.42(4) 6_565 C8 C9 1.44(2) . C9 C25 1.39(3) . C9 C10 1.42(2) . C10 C11 1.45(3) . C11 C12 1.46(2) . C11 C12 1.46(2) 6_565 C12 C26 1.33(2) . C12 C13 1.45(2) . C13 C14 1.40(2) . C13 C13 1.44(3) 6_565 C14 C28 1.439(17) . C14 C15 1.514(19) . C15 C16 1.533(16) . C15 C15 1.629(18) 6_565 C16 C17 1.366(18) . C16 C29 1.407(17) . C17 C18 1.414(16) . C17 C17 1.50(2) 6_565 C18 C19 1.37(2) . C19 C30 1.44(2) . C19 C20 1.510(19) . C20 C21 1.42(2) . C21 C22 1.36(2) . C21 C31 1.461(17) . C22 C23 1.47(2) . C23 C24 1.40(2) . C24 C25 1.39(3) . C24 C32 1.51(3) . C25 C26 1.51(2) . C26 C27 1.45(3) . C27 C28 1.45(2) . C27 C32 1.462(19) . C28 C29 1.43(2) . C29 C30 1.397(15) . C30 C31 1.46(2) . C31 C32 1.36(3) . C33 C34 1.50(2) . C33 H33A 0.9900 . C33 H33B 0.9900 . C34 H34A 0.9900 . C34 H34B 0.9900 . C35 C35 1.53(2) 6_565 C35 H35A 0.9900 . C35 H35B 0.9900 . C36 C36 1.52(2) 6_565 C36 H36A 0.9900 . C36 H36B 0.9900 . C37 C38 1.58(5) . C38 H38A 0.9800 . C38 H38B 0.9800 . C38 H38C 0.9800 . C39 C40 1.560(10) . C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . C41 C42 1.554(10) . C42 H42A 0.9800 . C42 H42B 0.9800 . C42 H42C 0.9800 . C43 C44 1.43(4) . C44 H44A 0.9800 . C44 H44B 0.9800 . C44 H44C 0.9800 . C45 C46 1.562(10) . C46 H46A 1.0169 . C46 H46B 0.9617 . C47 C48 1.566(10) . C48 H48A 0.9800 . C48 H48B 0.9800 . C48 H48C 0.9800 . C49 S1 1.49(11) . C49 S2 1.76(11) . 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_4 C33 N3 C1 C18 -175.0(13) . 6_565 C33 N3 C1 C18 66.3(17) 6_565 6_565 C33 N3 C1 C18 -66.3(17) . . C33 N3 C1 C18 175.0(13) 6_565 . C33 N3 C1 C2 59.3(12) . . C33 N3 C1 C2 -59.3(12) 6_565 . C34 N2 C2 C3 -176.1(15) 6_565 . C34 N2 C2 C3 69(2) . . Rh2 N2 C2 C3 -53.7(12) . . C34 N2 C2 C3 -69(2) 6_565 6_565 C34 N2 C2 C3 176.1(15) . 6_565 Rh2 N2 C2 C3 53.7(12) . 6_565 C34 N2 C2 C1 57.6(14) 6_565 . C34 N2 C2 C1 -57.6(14) . . Rh2 N2 C2 C1 180.000(7) . . C18 C1 C2 N2 -121.4(15) 6_565 . C18 C1 C2 N2 121.4(15) . . N3 C1 C2 N2 0.000(8) . . C18 C1 C2 C3 113.9(15) 6_565 . C18 C1 C2 C3 -3(2) . . N3 C1 C2 C3 -124.6(13) . . C18 C1 C2 C3 3(2) 6_565 6_565 C18 C1 C2 C3 -113.9(15) . 6_565 N3 C1 C2 C3 124.6(13) . 6_565 N2 C2 C3 C20 -111.0(17) . . C3 C2 C3 C20 133.8(12) 6_565 . C1 C2 C3 C20 14(2) . . N2 C2 C3 C4 99.3(16) . . C3 C2 C3 C4 -15.9(15) 6_565 . C1 C2 C3 C4 -135.6(14) . . C20 C3 C4 C5 5.4(17) . . C2 C3 C4 C5 157.5(12) . . C20 C3 C4 C4 -141.2(8) . 6_565 C2 C3 C4 C4 10.9(11) . 6_565 C4 C4 C5 C22 138.6(10) 6_565 . C3 C4 C5 C22 -4.0(18) . . C4 C4 C5 C6 1.7(13) 6_565 . C3 C4 C5 C6 -140.9(11) . . C4 C5 C6 C6 -1.7(13) . 6_565 C22 C5 C6 C6 -142.1(7) . 6_565 C4 C5 C6 C7 141.6(12) . . C22 C5 C6 C7 1.2(15) . . C6 C6 C7 C8 -1(2) 6_565 . C5 C6 C7 C8 -144.7(17) . . C6 C6 C7 C23 145.0(9) 6_565 . C5 C6 C7 C23 1.4(16) . . C6 C7 C8 C8 1(2) . 6_565 C23 C7 C8 C8 -140.5(13) . 6_565 C6 C7 C8 C9 137.7(19) . . C23 C7 C8 C9 -4(3) . . C7 C8 C9 C25 1(3) . . C8 C8 C9 C25 141.5(14) 6_565 . C7 C8 C9 C10 -139(2) . . C8 C8 C9 C10 1(2) 6_565 . C25 C9 C10 C9 -141.4(17) . 6_565 C8 C9 C10 C9 -2(3) . 6_565 C25 C9 C10 C11 3(4) . . C8 C9 C10 C11 142(2) . . C9 C10 C11 C12 -3(4) . . C9 C10 C11 C12 139(2) 6_565 . C9 C10 C11 C12 -139(2) . 6_565 C9 C10 C11 C12 3(4) 6_565 6_565 C10 C11 C12 C26 3(3) . . C12 C11 C12 C26 144.0(13) 6_565 . C10 C11 C12 C13 -146(2) . . C12 C11 C12 C13 -5(2) 6_565 . C26 C12 C13 C14 -2(2) . . C11 C12 C13 C14 145.5(15) . . C26 C12 C13 C13 -144.2(12) . 6_565 C11 C12 C13 C13 2.8(14) . 6_565 C13 C13 C14 C28 135.9(8) 6_565 . C12 C13 C14 C28 -2.1(18) . . C13 C13 C14 C15 -12.0(13) 6_565 . C12 C13 C14 C15 -150.0(12) . . C36 N1 C15 C14 67.6(11) . . C35 N1 C15 C14 -175.6(9) . . Rh1 N1 C15 C14 -55.6(13) . . C36 N1 C15 C16 177.1(9) . . C35 N1 C15 C16 -66.2(10) . . Rh1 N1 C15 C16 53.8(13) . . C36 N1 C15 C15 -57.8(9) . 6_565 C35 N1 C15 C15 59.0(7) . 6_565 Rh1 N1 C15 C15 179.0(6) . 6_565 C13 C14 C15 N1 -111.3(12) . . C28 C14 C15 N1 98.0(10) . . C13 C14 C15 C16 133.3(11) . . C28 C14 C15 C16 -17.3(11) . . C13 C14 C15 C15 11.3(12) . 6_565 C28 C14 C15 C15 -139.4(7) . 6_565 N1 C15 C16 C17 111.9(14) . . C14 C15 C16 C17 -132.6(15) . . C15 C15 C16 C17 -10.5(17) 6_565 . N1 C15 C16 C29 -97.5(12) . . C14 C15 C16 C29 18.0(12) . . C15 C15 C16 C29 140.1(7) 6_565 . C29 C16 C17 C18 1(2) . . C15 C16 C17 C18 149.0(14) . . C29 C16 C17 C17 -137.1(10) . 6_565 C15 C16 C17 C17 11.1(17) . 6_565 C16 C17 C18 C19 1(2) . . C17 C17 C18 C19 144.0(13) 6_565 . C16 C17 C18 C1 -155.7(17) . . C17 C17 C18 C1 -13.0(17) 6_565 . C18 C1 C18 C19 -136.5(13) 6_565 . N3 C1 C18 C19 109.1(19) . . C2 C1 C18 C19 -11(3) . . C18 C1 C18 C17 20(3) 6_565 . N3 C1 C18 C17 -94.7(16) . . C2 C1 C18 C17 145.0(16) . . C17 C18 C19 C30 -3(2) . . C1 C18 C19 C30 151.2(17) . . C17 C18 C19 C20 -137.9(15) . . C1 C18 C19 C20 16(3) . . C4 C3 C20 C21 -4.6(16) . . C2 C3 C20 C21 -152.4(14) . . C4 C3 C20 C19 137.2(13) . . C2 C3 C20 C19 -11(2) . . C18 C19 C20 C3 -5(2) . . C30 C19 C20 C3 -144.7(13) . . C18 C19 C20 C21 141.5(14) . . C30 C19 C20 C21 1.8(15) . . C3 C20 C21 C22 2.5(18) . . C19 C20 C21 C22 -142.4(12) . . C3 C20 C21 C31 143.0(12) . . C19 C20 C21 C31 -1.9(15) . . C20 C21 C22 C5 -0.9(18) . . C31 C21 C22 C5 -136.8(13) . . C20 C21 C22 C23 139.0(13) . . C31 C21 C22 C23 3.2(18) . . C4 C5 C22 C21 1.8(18) . . C6 C5 C22 C21 142.4(13) . . C4 C5 C22 C23 -143.9(13) . . C6 C5 C22 C23 -3.3(14) . . C21 C22 C23 C24 -4(2) . . C5 C22 C23 C24 141.0(13) . . C21 C22 C23 C7 -140.8(13) . . C5 C22 C23 C7 4.1(14) . . C8 C7 C23 C24 5(3) . . C6 C7 C23 C24 -141.1(15) . . C8 C7 C23 C22 142.6(17) . . C6 C7 C23 C22 -3.5(16) . . C22 C23 C24 C25 -136.0(17) . . C7 C23 C24 C25 -3(2) . . C22 C23 C24 C32 4(2) . . C7 C23 C24 C32 136.9(16) . . C23 C24 C25 C9 0(3) . . C32 C24 C25 C9 -142.0(17) . . C23 C24 C25 C26 142.6(16) . . C32 C24 C25 C26 0.5(18) . . C10 C9 C25 C24 135(2) . . C8 C9 C25 C24 1(3) . . C10 C9 C25 C26 -4(3) . . C8 C9 C25 C26 -137.7(18) . . C13 C12 C26 C27 2(2) . . C11 C12 C26 C27 -141.6(18) . . C13 C12 C26 C25 140.2(17) . . C11 C12 C26 C25 -3(3) . . C24 C25 C26 C12 -140.8(18) . . C9 C25 C26 C12 4(3) . . C24 C25 C26 C27 1.8(18) . . C9 C25 C26 C27 146.5(16) . . C12 C26 C27 C28 2(2) . . C25 C26 C27 C28 -142.2(13) . . C12 C26 C27 C32 140.2(14) . . C25 C26 C27 C32 -3.5(17) . . C13 C14 C28 C29 -141.3(12) . . C15 C14 C28 C29 11.2(13) . . C13 C14 C28 C27 5.4(16) . . C15 C14 C28 C27 157.8(10) . . C26 C27 C28 C29 136.8(13) . . C32 C27 C28 C29 1.2(19) . . C26 C27 C28 C14 -5.1(17) . . C32 C27 C28 C14 -140.7(13) . . C17 C16 C29 C30 -1(2) . . C15 C16 C29 C30 -154.0(13) . . C17 C16 C29 C28 140.4(13) . . C15 C16 C29 C28 -12.5(13) . . C14 C28 C29 C30 144.0(11) . . C27 C28 C29 C30 -1.5(17) . . C14 C28 C29 C16 0.9(14) . . C27 C28 C29 C16 -144.7(12) . . C16 C29 C30 C19 0(2) . . C28 C29 C30 C19 -139.0(14) . . C16 C29 C30 C31 139.3(14) . . C28 C29 C30 C31 0.8(16) . . C18 C19 C30 C29 2(2) . . C20 C19 C30 C29 143.7(14) . . C18 C19 C30 C31 -142.2(14) . . C20 C19 C30 C31 -0.9(15) . . C22 C21 C31 C32 -2.7(17) . . C20 C21 C31 C32 -143.2(12) . . C22 C21 C31 C30 141.8(13) . . C20 C21 C31 C30 1.3(15) . . C29 C30 C31 C32 0.2(18) . . C19 C30 C31 C32 143.8(12) . . C29 C30 C31 C21 -143.8(12) . . C19 C30 C31 C21 -0.2(15) . . C21 C31 C32 C27 139.8(13) . . C30 C31 C32 C27 0(2) . . C21 C31 C32 C24 2.9(18) . . C30 C31 C32 C24 -137.4(13) . . C28 C27 C32 C31 0(2) . . C26 C27 C32 C31 -139.6(15) . . C28 C27 C32 C24 143.1(13) . . C26 C27 C32 C24 3.7(16) . . C25 C24 C32 C31 139.9(14) . . C23 C24 C32 C31 -4(2) . . C25 C24 C32 C27 -2.6(16) . . C23 C24 C32 C27 -146.1(13) . . C33 N3 C33 C34 55(3) 6_565 . C1 N3 C33 C34 -63(2) . . C2 N2 C34 C33 57(2) . . C34 N2 C34 C33 -60(2) 6_565 . Rh2 N2 C34 C33 -167.8(15) . . N3 C33 C34 N2 3(3) . . C36 N1 C35 C35 57.5(7) . 6_565 C15 N1 C35 C35 -59.8(7) . 6_565 Rh1 N1 C35 C35 164.4(7) . 6_565 C15 N1 C36 C36 59.7(9) . 6_565 C35 N1 C36 C36 -58.5(7) . 6_565 Rh1 N1 C36 C36 -163.3(2) . 6_565 Rh1 O1 C37 O2 -8(4) . . Rh1 O1 C37 C38 -168(2) . . Rh1 O2 C37 O1 17(4) 7_656 . Rh1 O2 C37 C38 178(2) 7_656 . Rh1 O4 C39 O3 0(3) 7_656 . Rh1 O4 C39 C40 -162(2) 7_656 . Rh1 O3 C39 O4 2(3) . . Rh1 O3 C39 C40 163(2) . . Rh1 O5 C41 O6 1(4) . . Rh1 O5 C41 C42 178.2(16) . . Rh1 O6 C41 O5 -4(4) 7_656 . Rh1 O6 C41 C42 178.8(16) 7_656 . Rh1 O7 C43 O8 3(3) . . Rh1 O7 C43 C44 179.8(18) . . Rh1 O8 C43 O7 -5(3) 7_656 . Rh1 O8 C43 C44 178.4(18) 7_656 . Rh2 O9 C45 O10 0.000(12) . . Rh2 O9 C45 C46 180.000(8) . . Rh2 O10 C45 O9 0.000(12) 5_567 . Rh2 O10 C45 C46 180.000(8) 5_567 . Rh2 O12 C47 O12 -0.4(6) . 2_557 Rh2 O12 C47 C48 179.6(6) . .