# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Wiley J. Youngs' _publ_contact_author_address ;Department of Chemistry The University of Akron Akron, Ohio 44325-3601 ; _publ_contact_author_email youngs@uakron.edu _publ_contact_author_phone '(330) - 972 -5362' _publ_contact_author_fax '330-972-7370 ' loop_ _publ_author_name _publ_author_address J.C.Garrison ;Department of Chemistry The University of Akron Akron, Ohio 44325-3601 ; M.J.Panzner ;Department of Chemistry The University of Akron Akron, Ohio 44325-3601 ; P.D.Custer ;Department of Chemistry The University of Akron Akron, Ohio 44325-3601 ; D.Venkat.Reddy ;Department of Chemistry The University of Akron Akron, Ohio 44325-3601 ; P.Rinaldi ;Department of Chemistry The University of Akron Akron, Ohio 44325-3601 ; ; C.A.Tessier ; ;Department of Chemistry The University of Akron Akron, Ohio 44325-3601 ; W.J.Youngs ;Department of Chemistry The University of Akron Akron, Ohio 44325-3601 ; _publ_section_title ; Synthesis and Characterization of a Trigonal Bipyramidal Supramolecular Cage Based Upon Rhodium and Platinum Metal Centers ; data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 602644' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H33 N6 Rh' _chemical_formula_sum 'C30 H33 N6 Rh' _chemical_formula_weight 580.53 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.996(2) _cell_length_b 11.6667(11) _cell_length_c 24.063(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.499(2) _cell_angle_gamma 90.00 _cell_volume 5363.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5686 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.31 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7669 _exptl_absorpt_correction_T_max 0.9611 _exptl_absorpt_process_details SADABS _exptl_special_details ; Crystals grown from a conc. sample in DMSO. The Me3tacn chelated to Rh2 has a slight disorder. Modeling this disorder resulted in insignificant improvements to the R values and GOF. The result causes alerts for high Ueq(max)/Ueq(min) ratios for these carbon atoms. Cif check alert for long sp1 to sp2 bond distances may arise from the sp2 carbon being part of an aromatic ring. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46820 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.32 _reflns_number_total 12862 _reflns_number_gt 11613 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+19.4941P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12862 _refine_ls_number_parameters 673 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_restrained_S_all 1.242 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.191960(16) 0.33671(3) 0.653537(14) 0.01338(8) Uani 1 1 d . . . Rh2 Rh 0.281080(16) 0.15148(3) 0.346205(14) 0.01282(8) Uani 1 1 d . . . N1 N 0.24133(18) 0.4408(3) 0.60907(16) 0.0185(7) Uani 1 1 d . . . N2 N 0.16965(19) 0.5010(3) 0.68162(16) 0.0186(7) Uani 1 1 d . . . N3 N 0.09955(18) 0.3721(3) 0.57193(16) 0.0180(7) Uani 1 1 d . . . N4 N 0.5433(2) 0.3459(5) 0.9087(2) 0.0417(12) Uani 1 1 d . . . N5 N -0.0002(2) 0.0641(4) 0.8176(2) 0.0309(9) Uani 1 1 d . . . N6 N 0.2350(3) -0.2220(4) 0.5262(2) 0.0460(13) Uani 1 1 d . . . N7 N 0.2625(2) 0.1231(3) 0.42652(17) 0.0219(8) Uani 1 1 d . . . N8 N 0.3756(2) 0.0601(3) 0.39841(17) 0.0238(8) Uani 1 1 d . . . N9 N 0.2388(2) -0.0179(3) 0.32326(17) 0.0255(8) Uani 1 1 d . . . N10 N 0.4271(4) 0.7095(5) 0.4886(3) 0.0607(17) Uani 1 1 d . . . N11 N 0.4118(2) 0.0789(4) 0.10830(18) 0.0272(9) Uani 1 1 d . . . N12 N -0.0681(2) 0.3779(4) 0.1401(2) 0.0408(12) Uani 1 1 d . . . C1 C 0.2636(2) 0.5457(4) 0.6479(2) 0.0219(9) Uani 1 1 d . . . H1A H 0.2797 0.6043 0.6269 0.026 Uiso 1 1 calc R . . H1B H 0.3034 0.5265 0.6869 0.026 Uiso 1 1 calc R . . C2 C 0.2048(2) 0.5940(4) 0.6609(2) 0.0241(9) Uani 1 1 d . . . H2A H 0.1701 0.6306 0.6235 0.029 Uiso 1 1 calc R . . H2B H 0.2234 0.6534 0.6930 0.029 Uiso 1 1 calc R . . C3 C 0.0918(2) 0.5073(4) 0.6494(2) 0.0216(9) Uani 1 1 d . . . H3A H 0.0761 0.5852 0.6541 0.026 Uiso 1 1 calc R . . H3B H 0.0708 0.4522 0.6682 0.026 Uiso 1 1 calc R . . C4 C 0.0666(2) 0.4800(4) 0.5818(2) 0.0220(9) Uani 1 1 d . . . H4A H 0.0151 0.4711 0.5634 0.026 Uiso 1 1 calc R . . H4B H 0.0783 0.5446 0.5610 0.026 Uiso 1 1 calc R . . C5 C 0.1272(2) 0.3879(4) 0.52460(19) 0.0215(9) Uani 1 1 d . . . H5A H 0.0895 0.4179 0.4868 0.026 Uiso 1 1 calc R . . H5B H 0.1422 0.3128 0.5150 0.026 Uiso 1 1 calc R . . C6 C 0.1885(2) 0.4701(4) 0.54590(19) 0.0236(9) Uani 1 1 d . . . H6A H 0.2113 0.4672 0.5172 0.028 Uiso 1 1 calc R . . H6B H 0.1713 0.5492 0.5457 0.028 Uiso 1 1 calc R . . C7 C 0.3038(2) 0.3871(4) 0.6057(2) 0.0238(9) Uani 1 1 d . . . H7A H 0.3262 0.4421 0.5886 0.036 Uiso 1 1 calc R . . H7B H 0.2895 0.3191 0.5795 0.036 Uiso 1 1 calc R . . H7C H 0.3371 0.3647 0.6468 0.036 Uiso 1 1 calc R . . C8 C 0.1900(2) 0.5125(4) 0.74846(19) 0.0212(9) Uani 1 1 d . . . H8A H 0.1714 0.5845 0.7566 0.032 Uiso 1 1 calc R . . H8B H 0.2411 0.5126 0.7701 0.032 Uiso 1 1 calc R . . H8C H 0.1708 0.4479 0.7627 0.032 Uiso 1 1 calc R . . C9 C 0.0471(2) 0.2785(4) 0.5523(2) 0.0219(9) Uani 1 1 d . . . H9A H 0.0091 0.2983 0.5130 0.033 Uiso 1 1 calc R . . H9B H 0.0281 0.2680 0.5829 0.033 Uiso 1 1 calc R . . H9C H 0.0695 0.2073 0.5481 0.033 Uiso 1 1 calc R . . C10 C 0.2811(2) 0.3220(3) 0.72507(19) 0.0159(8) Uani 1 1 d . . . C11 C 0.3373(2) 0.3255(4) 0.7670(2) 0.0187(8) Uani 1 1 d . . . C12 C 0.4060(2) 0.3313(4) 0.81524(19) 0.0181(8) Uani 1 1 d . . . C13 C 0.4632(2) 0.2783(4) 0.8102(2) 0.0231(9) Uani 1 1 d . . . H13 H 0.4568 0.2357 0.7746 0.028 Uiso 1 1 calc R . . C14 C 0.5291(3) 0.2885(5) 0.8575(2) 0.0321(11) Uani 1 1 d . . . H14 H 0.5669 0.2515 0.8528 0.039 Uiso 1 1 calc R . . C15 C 0.4885(3) 0.3963(6) 0.9133(2) 0.0453(15) Uani 1 1 d . . . H15 H 0.4969 0.4377 0.9496 0.054 Uiso 1 1 calc R . . C16 C 0.4205(3) 0.3927(5) 0.8688(2) 0.0327(12) Uani 1 1 d . . . H16 H 0.3841 0.4316 0.8747 0.039 Uiso 1 1 calc R . . C17 C 0.1427(2) 0.2550(3) 0.69565(18) 0.0150(8) Uani 1 1 d . . . C18 C 0.1103(2) 0.2119(4) 0.7215(2) 0.0202(9) Uani 1 1 d . . . C19 C 0.0721(2) 0.1637(4) 0.7531(2) 0.0199(9) Uani 1 1 d . . . C20 C 0.0743(2) 0.2109(4) 0.8068(2) 0.0259(10) Uani 1 1 d . . . H20 H 0.1006 0.2787 0.8228 0.031 Uiso 1 1 calc R . . C21 C 0.0382(3) 0.1596(5) 0.8370(2) 0.0319(11) Uani 1 1 d . . . H21 H 0.0409 0.1941 0.8737 0.038 Uiso 1 1 calc R . . C22 C -0.0033(3) 0.0207(4) 0.7652(3) 0.0317(11) Uani 1 1 d . . . H22 H -0.0306 -0.0465 0.7499 0.038 Uiso 1 1 calc R . . C23 C 0.0305(2) 0.0664(4) 0.7313(2) 0.0235(9) Uani 1 1 d . . . H23 H 0.0253 0.0320 0.6939 0.028 Uiso 1 1 calc R . . C24 C 0.2061(2) 0.1903(4) 0.62048(18) 0.0175(8) Uani 1 1 d . . . C25 C 0.2095(2) 0.1007(4) 0.59656(19) 0.0187(8) Uani 1 1 d . . . C26 C 0.2169(2) -0.0076(4) 0.57196(18) 0.0174(8) Uani 1 1 d . . . C27 C 0.1602(3) -0.0705(4) 0.5316(2) 0.0281(10) Uani 1 1 d . . . H27 H 0.1139 -0.0414 0.5182 0.034 Uiso 1 1 calc R . . C28 C 0.1723(3) -0.1772(5) 0.5111(2) 0.0372(13) Uani 1 1 d . . . H28 H 0.1329 -0.2201 0.4846 0.045 Uiso 1 1 calc R . . C29 C 0.2885(3) -0.1589(5) 0.5630(2) 0.0481(17) Uani 1 1 d . . . H29 H 0.3342 -0.1881 0.5735 0.058 Uiso 1 1 calc R . . C30 C 0.2829(3) -0.0550(5) 0.5871(2) 0.0314(11) Uani 1 1 d . . . H30 H 0.3237 -0.0156 0.6140 0.038 Uiso 1 1 calc R . . C31 C 0.3338(3) 0.1093(7) 0.4763(3) 0.0560(19) Uani 1 1 d . . . H31A H 0.3536 0.1865 0.4900 0.067 Uiso 1 1 calc R . . H31B H 0.3292 0.0713 0.5113 0.067 Uiso 1 1 calc R . . C32 C 0.3814(3) 0.0469(8) 0.4617(3) 0.063(2) Uani 1 1 d . . . H32A H 0.3758 -0.0354 0.4688 0.075 Uiso 1 1 calc R . . H32B H 0.4293 0.0695 0.4903 0.075 Uiso 1 1 calc R . . C33 C 0.3643(3) -0.0547(5) 0.3675(4) 0.0548(19) Uani 1 1 d . . . H33A H 0.3777 -0.0483 0.3327 0.066 Uiso 1 1 calc R . . H33B H 0.3967 -0.1101 0.3967 0.066 Uiso 1 1 calc R . . C34 C 0.2959(4) -0.1015(6) 0.3452(4) 0.083(3) Uani 1 1 d . . . H34A H 0.2918 -0.1470 0.3783 0.099 Uiso 1 1 calc R . . H34B H 0.2899 -0.1548 0.3114 0.099 Uiso 1 1 calc R . . C35 C 0.1930(5) -0.0273(8) 0.3571(3) 0.079(3) Uani 1 1 d . . . H35A H 0.1479 0.0107 0.3325 0.095 Uiso 1 1 calc R . . H35B H 0.1829 -0.1095 0.3599 0.095 Uiso 1 1 calc R . . C36 C 0.2192(4) 0.0191(5) 0.4163(3) 0.0500(17) Uani 1 1 d . . . H36A H 0.2475 -0.0405 0.4454 0.060 Uiso 1 1 calc R . . H36B H 0.1791 0.0371 0.4264 0.060 Uiso 1 1 calc R . . C37 C 0.2288(3) 0.2188(4) 0.4440(2) 0.0277(10) Uani 1 1 d . . . H37A H 0.1826 0.2334 0.4112 0.041 Uiso 1 1 calc R . . H37B H 0.2578 0.2877 0.4510 0.041 Uiso 1 1 calc R . . H37C H 0.2237 0.1990 0.4815 0.041 Uiso 1 1 calc R . . C38 C 0.4399(2) 0.1124(5) 0.3980(2) 0.0298(11) Uani 1 1 d . . . H38A H 0.4470 0.1886 0.4167 0.045 Uiso 1 1 calc R . . H38B H 0.4348 0.1193 0.3557 0.045 Uiso 1 1 calc R . . H38C H 0.4803 0.0637 0.4211 0.045 Uiso 1 1 calc R . . C39 C 0.1944(2) -0.0372(4) 0.25735(19) 0.0226(9) Uani 1 1 d . . . H39A H 0.2233 -0.0318 0.2342 0.034 Uiso 1 1 calc R . . H39B H 0.1575 0.0210 0.2426 0.034 Uiso 1 1 calc R . . H39C H 0.1731 -0.1135 0.2517 0.034 Uiso 1 1 calc R . . C40 C 0.3228(2) 0.3044(4) 0.37582(18) 0.0176(8) Uani 1 1 d . . . C41 C 0.3483(2) 0.3925(4) 0.3989(2) 0.0219(9) Uani 1 1 d . . . C42 C 0.3757(2) 0.4995(4) 0.4288(2) 0.0238(9) Uani 1 1 d . . . C43 C 0.3419(3) 0.5603(6) 0.4576(3) 0.0551(19) Uani 1 1 d . . . H43 H 0.3001 0.5314 0.4586 0.066 Uiso 1 1 calc R . . C44 C 0.3692(4) 0.6637(7) 0.4850(4) 0.075(3) Uani 1 1 d . . . H44 H 0.3433 0.7049 0.5028 0.091 Uiso 1 1 calc R . . C45 C 0.4593(4) 0.6499(6) 0.4614(3) 0.061(2) Uani 1 1 d . . . H45 H 0.5022 0.6800 0.4631 0.074 Uiso 1 1 calc R . . C46 C 0.4364(3) 0.5476(5) 0.4305(3) 0.0422(14) Uani 1 1 d . . . H46 H 0.4620 0.5112 0.4109 0.051 Uiso 1 1 calc R . . C47 C 0.3044(2) 0.1597(4) 0.27579(19) 0.0171(8) Uani 1 1 d . . . C48 C 0.3224(2) 0.1506(4) 0.2344(2) 0.0194(8) Uani 1 1 d . . . C49 C 0.3501(2) 0.1302(4) 0.18995(18) 0.0173(8) Uani 1 1 d . . . C50 C 0.4041(2) 0.1961(4) 0.1876(2) 0.0193(8) Uani 1 1 d . . . H50 H 0.4216 0.2600 0.2141 0.023 Uiso 1 1 calc R . . C51 C 0.4322(2) 0.1682(4) 0.1466(2) 0.0251(10) Uani 1 1 d . . . H51 H 0.4684 0.2157 0.1455 0.030 Uiso 1 1 calc R . . C52 C 0.3600(3) 0.0156(4) 0.1113(2) 0.0281(10) Uani 1 1 d . . . H52 H 0.3447 -0.0492 0.0852 0.034 Uiso 1 1 calc R . . C53 C 0.3275(2) 0.0373(4) 0.1495(2) 0.0250(10) Uani 1 1 d . . . H53 H 0.2902 -0.0101 0.1484 0.030 Uiso 1 1 calc R . . C54 C 0.1903(2) 0.2245(4) 0.29807(18) 0.0167(8) Uani 1 1 d . . . C55 C 0.1331(2) 0.2630(4) 0.2661(2) 0.0209(9) Uani 1 1 d . . . C56 C 0.0651(2) 0.3022(4) 0.2247(2) 0.0212(9) Uani 1 1 d . . . C57 C 0.0237(2) 0.2373(4) 0.1735(2) 0.0270(10) Uani 1 1 d . . . H57 H 0.0400 0.1655 0.1660 0.032 Uiso 1 1 calc R . . C58 C -0.0410(3) 0.2783(5) 0.1339(2) 0.0354(12) Uani 1 1 d . . . H58 H -0.0682 0.2318 0.0999 0.043 Uiso 1 1 calc R . . C59 C -0.0289(3) 0.4385(5) 0.1893(3) 0.0401(14) Uani 1 1 d . . . H59 H -0.0469 0.5098 0.1954 0.048 Uiso 1 1 calc R . . C60 C 0.0361(2) 0.4051(4) 0.2322(3) 0.0313(11) Uani 1 1 d . . . H60 H 0.0609 0.4522 0.2666 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01281(15) 0.01390(15) 0.01278(15) -0.00040(11) 0.00465(12) 0.00122(12) Rh2 0.01161(15) 0.01389(15) 0.01300(15) 0.00028(11) 0.00516(12) 0.00075(11) N1 0.0157(17) 0.0246(18) 0.0136(16) 0.0023(14) 0.0044(14) 0.0007(14) N2 0.0189(18) 0.0190(17) 0.0168(17) -0.0012(14) 0.0065(15) 0.0028(14) N3 0.0155(17) 0.0206(18) 0.0171(17) 0.0025(14) 0.0059(14) 0.0039(14) N4 0.020(2) 0.067(3) 0.031(2) 0.005(2) 0.0035(19) -0.002(2) N5 0.030(2) 0.031(2) 0.040(2) 0.0067(19) 0.022(2) 0.0022(18) N6 0.078(4) 0.025(2) 0.027(2) 0.0006(19) 0.014(2) 0.015(2) N7 0.0225(19) 0.028(2) 0.0179(18) -0.0001(15) 0.0108(16) -0.0033(16) N8 0.0202(19) 0.033(2) 0.0165(18) 0.0062(16) 0.0061(15) 0.0094(16) N9 0.035(2) 0.0208(19) 0.0164(18) -0.0009(15) 0.0067(17) -0.0054(17) N10 0.085(5) 0.032(3) 0.043(3) -0.017(2) 0.005(3) -0.001(3) N11 0.026(2) 0.039(2) 0.0212(19) -0.0022(17) 0.0145(17) -0.0019(18) N12 0.018(2) 0.050(3) 0.046(3) 0.018(2) 0.005(2) 0.007(2) C1 0.023(2) 0.020(2) 0.018(2) 0.0000(17) 0.0046(18) -0.0069(18) C2 0.031(2) 0.017(2) 0.024(2) 0.0011(17) 0.011(2) 0.0010(18) C3 0.020(2) 0.024(2) 0.022(2) -0.0020(17) 0.0090(18) 0.0064(17) C4 0.017(2) 0.028(2) 0.019(2) 0.0025(18) 0.0057(17) 0.0084(18) C5 0.021(2) 0.027(2) 0.015(2) 0.0016(17) 0.0064(17) 0.0056(18) C6 0.025(2) 0.030(2) 0.016(2) 0.0028(18) 0.0092(18) -0.0012(19) C7 0.017(2) 0.035(3) 0.021(2) 0.0008(19) 0.0101(18) -0.0021(19) C8 0.027(2) 0.019(2) 0.017(2) -0.0022(16) 0.0086(18) 0.0018(18) C9 0.015(2) 0.031(2) 0.019(2) -0.0007(18) 0.0063(17) -0.0002(18) C10 0.0141(19) 0.0172(19) 0.0173(19) 0.0015(15) 0.0075(16) 0.0012(15) C11 0.018(2) 0.019(2) 0.021(2) 0.0031(16) 0.0099(18) 0.0006(16) C12 0.0149(19) 0.021(2) 0.0174(19) 0.0053(16) 0.0056(16) -0.0014(16) C13 0.018(2) 0.022(2) 0.029(2) 0.0050(18) 0.0102(19) -0.0015(17) C14 0.019(2) 0.037(3) 0.040(3) 0.009(2) 0.012(2) 0.002(2) C15 0.028(3) 0.085(5) 0.019(2) -0.008(3) 0.006(2) -0.006(3) C16 0.021(2) 0.056(3) 0.021(2) 0.001(2) 0.009(2) 0.002(2) C17 0.0106(18) 0.0180(19) 0.0155(19) -0.0006(15) 0.0046(15) 0.0016(15) C18 0.017(2) 0.021(2) 0.020(2) -0.0006(17) 0.0055(17) 0.0036(17) C19 0.016(2) 0.019(2) 0.023(2) 0.0064(17) 0.0059(17) 0.0048(16) C20 0.023(2) 0.028(2) 0.026(2) -0.0003(19) 0.0090(19) -0.0028(19) C21 0.033(3) 0.040(3) 0.027(3) 0.000(2) 0.017(2) 0.003(2) C22 0.027(3) 0.020(2) 0.052(3) 0.002(2) 0.019(2) 0.0001(19) C23 0.025(2) 0.017(2) 0.031(2) 0.0011(18) 0.014(2) 0.0036(17) C24 0.0142(19) 0.023(2) 0.0141(19) 0.0032(16) 0.0045(16) 0.0021(16) C25 0.016(2) 0.022(2) 0.017(2) 0.0017(16) 0.0067(17) 0.0013(16) C26 0.024(2) 0.0175(19) 0.0138(19) 0.0005(15) 0.0105(17) -0.0016(16) C27 0.026(2) 0.036(3) 0.027(2) -0.009(2) 0.016(2) -0.011(2) C28 0.056(4) 0.030(3) 0.032(3) -0.012(2) 0.025(3) -0.023(3) C29 0.054(4) 0.048(3) 0.025(3) -0.004(2) -0.001(3) 0.031(3) C30 0.031(3) 0.036(3) 0.019(2) -0.005(2) 0.001(2) 0.014(2) C31 0.039(3) 0.105(6) 0.022(3) 0.010(3) 0.010(3) 0.025(4) C32 0.036(3) 0.127(7) 0.021(3) 0.023(4) 0.008(3) 0.025(4) C33 0.050(4) 0.024(3) 0.108(6) 0.011(3) 0.050(4) 0.015(3) C34 0.070(5) 0.039(4) 0.078(5) -0.024(4) -0.031(4) 0.028(4) C35 0.110(6) 0.101(6) 0.038(4) -0.025(4) 0.042(4) -0.085(6) C36 0.069(4) 0.038(3) 0.072(4) -0.018(3) 0.057(4) -0.024(3) C37 0.027(2) 0.037(3) 0.024(2) -0.012(2) 0.016(2) -0.007(2) C38 0.013(2) 0.038(3) 0.031(3) 0.000(2) 0.0019(19) 0.0071(19) C39 0.028(2) 0.021(2) 0.018(2) -0.0048(17) 0.0093(19) -0.0053(18) C40 0.0114(18) 0.025(2) 0.0136(19) 0.0028(16) 0.0029(16) 0.0025(16) C41 0.017(2) 0.025(2) 0.019(2) -0.0001(18) 0.0036(17) 0.0008(18) C42 0.024(2) 0.022(2) 0.020(2) -0.0011(17) 0.0036(18) 0.0017(18) C43 0.030(3) 0.075(5) 0.055(4) -0.038(4) 0.013(3) -0.002(3) C44 0.053(4) 0.085(6) 0.068(5) -0.049(4) 0.004(4) 0.020(4) C45 0.088(6) 0.042(4) 0.053(4) -0.014(3) 0.027(4) -0.035(4) C46 0.058(4) 0.032(3) 0.044(3) -0.011(2) 0.029(3) -0.017(3) C47 0.0132(19) 0.0183(19) 0.0175(19) 0.0031(16) 0.0041(16) 0.0035(16) C48 0.018(2) 0.020(2) 0.022(2) 0.0030(17) 0.0101(18) 0.0011(17) C49 0.0148(19) 0.021(2) 0.0142(19) 0.0044(16) 0.0040(16) 0.0031(16) C50 0.020(2) 0.019(2) 0.019(2) -0.0011(16) 0.0084(17) 0.0000(17) C51 0.022(2) 0.032(2) 0.024(2) 0.0011(19) 0.0137(19) -0.0051(19) C52 0.036(3) 0.030(2) 0.019(2) -0.0060(19) 0.012(2) -0.007(2) C53 0.022(2) 0.030(2) 0.020(2) 0.0003(19) 0.0070(18) -0.0045(19) C54 0.017(2) 0.020(2) 0.0139(19) -0.0021(16) 0.0073(16) -0.0010(16) C55 0.017(2) 0.024(2) 0.023(2) 0.0012(17) 0.0100(18) -0.0007(17) C56 0.0130(19) 0.024(2) 0.027(2) 0.0052(18) 0.0088(18) -0.0024(17) C57 0.021(2) 0.033(3) 0.023(2) 0.006(2) 0.0053(19) 0.0000(19) C58 0.018(2) 0.050(3) 0.030(3) 0.005(2) 0.001(2) -0.007(2) C59 0.022(3) 0.032(3) 0.060(4) 0.013(3) 0.011(3) 0.008(2) C60 0.019(2) 0.024(2) 0.050(3) 0.008(2) 0.013(2) 0.0004(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C10 1.956(4) . ? Rh1 C24 1.958(4) . ? Rh1 C17 1.968(4) . ? Rh1 N2 2.148(4) . ? Rh1 N1 2.148(4) . ? Rh1 N3 2.152(3) . ? Rh2 C47 1.952(4) . ? Rh2 C54 1.967(4) . ? Rh2 C40 1.985(4) . ? Rh2 N8 2.141(4) . ? Rh2 N9 2.142(4) . ? Rh2 N7 2.150(4) . ? N1 C7 1.486(5) . ? N1 C1 1.492(5) . ? N1 C6 1.503(5) . ? N2 C8 1.489(5) . ? N2 C3 1.492(5) . ? N2 C2 1.509(6) . ? N3 C9 1.482(6) . ? N3 C5 1.489(5) . ? N3 C4 1.502(5) . ? N4 C14 1.323(7) . ? N4 C15 1.336(7) . ? N5 C22 1.336(7) . ? N5 C21 1.341(7) . ? N6 C28 1.319(8) . ? N6 C29 1.328(8) . ? N7 C36 1.473(6) . ? N7 C37 1.474(6) . ? N7 C31 1.488(7) . ? N8 C32 1.484(6) . ? N8 C38 1.485(6) . ? N8 C33 1.503(7) . ? N9 C34 1.463(7) . ? N9 C39 1.486(5) . ? N9 C35 1.502(8) . ? N10 C44 1.297(10) . ? N10 C45 1.319(10) . ? N11 C51 1.338(6) . ? N11 C52 1.340(6) . ? N12 C58 1.329(8) . ? N12 C59 1.330(8) . ? C1 C2 1.502(6) . ? C3 C4 1.520(6) . ? C5 C6 1.514(6) . ? C10 C11 1.193(6) . ? C11 C12 1.430(6) . ? C12 C16 1.393(7) . ? C12 C13 1.398(6) . ? C13 C14 1.385(7) . ? C15 C16 1.386(7) . ? C17 C18 1.206(6) . ? C18 C19 1.431(6) . ? C19 C20 1.386(6) . ? C19 C23 1.395(6) . ? C20 C21 1.386(7) . ? C22 C23 1.390(7) . ? C24 C25 1.210(6) . ? C25 C26 1.431(6) . ? C26 C27 1.393(6) . ? C26 C30 1.393(6) . ? C27 C28 1.401(7) . ? C29 C30 1.369(7) . ? C31 C32 1.394(9) . ? C33 C34 1.417(10) . ? C35 C36 1.406(8) . ? C40 C41 1.185(6) . ? C41 C42 1.437(6) . ? C42 C46 1.376(7) . ? C42 C43 1.377(7) . ? C43 C44 1.380(10) . ? C45 C46 1.382(8) . ? C47 C48 1.208(6) . ? C48 C49 1.432(6) . ? C49 C50 1.390(6) . ? C49 C53 1.402(6) . ? C50 C51 1.383(6) . ? C52 C53 1.376(7) . ? C54 C55 1.212(6) . ? C55 C56 1.436(6) . ? C56 C60 1.391(7) . ? C56 C57 1.399(6) . ? C57 C58 1.382(7) . ? C59 C60 1.383(7) . ? 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 C10 Rh1 C24 91.74(17) . . ? C10 Rh1 C17 91.14(16) . . ? C24 Rh1 C17 89.24(17) . . ? C10 Rh1 N2 93.17(15) . . ? C24 Rh1 N2 174.81(15) . . ? C17 Rh1 N2 92.33(15) . . ? C10 Rh1 N1 90.25(15) . . ? C24 Rh1 N1 96.06(16) . . ? C17 Rh1 N1 174.48(15) . . ? N2 Rh1 N1 82.26(14) . . ? C10 Rh1 N3 172.63(15) . . ? C24 Rh1 N3 91.59(15) . . ? C17 Rh1 N3 95.48(15) . . ? N2 Rh1 N3 83.34(13) . . ? N1 Rh1 N3 82.86(13) . . ? C47 Rh2 C54 89.93(16) . . ? C47 Rh2 C40 92.04(17) . . ? C54 Rh2 C40 89.85(17) . . ? C47 Rh2 N8 91.61(15) . . ? C54 Rh2 N8 175.61(17) . . ? C40 Rh2 N8 94.20(16) . . ? C47 Rh2 N9 92.72(16) . . ? C54 Rh2 N9 92.93(16) . . ? C40 Rh2 N9 174.48(16) . . ? N8 Rh2 N9 82.89(16) . . ? C47 Rh2 N7 172.95(16) . . ? C54 Rh2 N7 95.92(15) . . ? C40 Rh2 N7 91.91(16) . . ? N8 Rh2 N7 82.28(14) . . ? N9 Rh2 N7 83.07(15) . . ? C7 N1 C1 109.0(3) . . ? C7 N1 C6 109.8(3) . . ? C1 N1 C6 110.8(3) . . ? C7 N1 Rh1 114.1(3) . . ? C1 N1 Rh1 104.0(2) . . ? C6 N1 Rh1 109.0(3) . . ? C8 N2 C3 108.6(3) . . ? C8 N2 C2 109.4(3) . . ? C3 N2 C2 111.9(3) . . ? C8 N2 Rh1 114.7(3) . . ? C3 N2 Rh1 102.4(2) . . ? C2 N2 Rh1 109.7(3) . . ? C9 N3 C5 108.8(3) . . ? C9 N3 C4 109.8(3) . . ? C5 N3 C4 111.6(3) . . ? C9 N3 Rh1 114.7(3) . . ? C5 N3 Rh1 103.4(2) . . ? C4 N3 Rh1 108.5(3) . . ? C14 N4 C15 115.5(4) . . ? C22 N5 C21 115.5(4) . . ? C28 N6 C29 115.8(5) . . ? C36 N7 C37 109.6(4) . . ? C36 N7 C31 112.9(5) . . ? C37 N7 C31 107.1(4) . . ? C36 N7 Rh2 107.9(3) . . ? C37 N7 Rh2 115.3(3) . . ? C31 N7 Rh2 104.1(3) . . ? C32 N8 C38 111.2(4) . . ? C32 N8 C33 110.1(5) . . ? C38 N8 C33 108.7(4) . . ? C32 N8 Rh2 108.4(3) . . ? C38 N8 Rh2 114.6(3) . . ? C33 N8 Rh2 103.6(3) . . ? C34 N9 C39 110.0(4) . . ? C34 N9 C35 111.6(6) . . ? C39 N9 C35 107.9(4) . . ? C34 N9 Rh2 109.4(4) . . ? C39 N9 Rh2 115.1(3) . . ? C35 N9 Rh2 102.6(4) . . ? C44 N10 C45 114.2(6) . . ? C51 N11 C52 115.3(4) . . ? C58 N12 C59 115.4(4) . . ? N1 C1 C2 111.5(4) . . ? C1 C2 N2 110.9(4) . . ? N2 C3 C4 111.5(3) . . ? N3 C4 C3 111.4(3) . . ? N3 C5 C6 111.5(4) . . ? N1 C6 C5 111.5(4) . . ? C11 C10 Rh1 172.3(4) . . ? C10 C11 C12 177.4(5) . . ? C16 C12 C13 116.2(4) . . ? C16 C12 C11 122.3(4) . . ? C13 C12 C11 121.4(4) . . ? C14 C13 C12 119.4(5) . . ? N4 C14 C13 124.8(5) . . ? N4 C15 C16 124.7(5) . . ? C15 C16 C12 119.3(5) . . ? C18 C17 Rh1 175.5(4) . . ? C17 C18 C19 178.4(5) . . ? C20 C19 C23 116.6(4) . . ? C20 C19 C18 122.0(4) . . ? C23 C19 C18 121.4(4) . . ? C21 C20 C19 120.2(5) . . ? N5 C21 C20 123.8(5) . . ? N5 C22 C23 124.9(5) . . ? C22 C23 C19 118.9(5) . . ? C25 C24 Rh1 174.9(4) . . ? C24 C25 C26 176.3(5) . . ? C27 C26 C30 116.3(4) . . ? C27 C26 C25 123.1(4) . . ? C30 C26 C25 120.6(4) . . ? C26 C27 C28 119.1(5) . . ? N6 C28 C27 124.1(5) . . ? N6 C29 C30 125.2(6) . . ? C29 C30 C26 119.4(5) . . ? C32 C31 N7 116.2(5) . . ? C31 C32 N8 116.2(5) . . ? C34 C33 N8 117.3(5) . . ? C33 C34 N9 115.4(6) . . ? C36 C35 N9 116.9(5) . . ? C35 C36 N7 116.2(5) . . ? C41 C40 Rh2 173.8(4) . . ? C40 C41 C42 175.8(5) . . ? C46 C42 C43 116.0(5) . . ? C46 C42 C41 122.8(5) . . ? C43 C42 C41 121.2(5) . . ? C42 C43 C44 119.5(7) . . ? N10 C44 C43 125.7(7) . . ? N10 C45 C46 125.8(7) . . ? C42 C46 C45 118.8(6) . . ? C48 C47 Rh2 171.5(4) . . ? C47 C48 C49 173.0(4) . . ? C50 C49 C53 116.5(4) . . ? C50 C49 C48 121.9(4) . . ? C53 C49 C48 121.5(4) . . ? C51 C50 C49 119.6(4) . . ? N11 C51 C50 124.5(4) . . ? N11 C52 C53 125.0(4) . . ? C52 C53 C49 119.2(4) . . ? C55 C54 Rh2 175.7(4) . . ? C54 C55 C56 175.5(5) . . ? C60 C56 C57 115.9(4) . . ? C60 C56 C55 123.2(4) . . ? C57 C56 C55 120.9(4) . . ? C58 C57 C56 119.6(5) . . ? N12 C58 C57 124.7(5) . . ? N12 C59 C60 124.7(5) . . ? C59 C60 C56 119.7(5) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.293 _refine_diff_density_min -1.402 _refine_diff_density_rms 0.120 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 602645' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H210 N12 P6 Pt3 Rh2' _chemical_formula_sum 'C138 H210 N12 P6 Pt3 Rh2' _chemical_formula_weight 3014.09 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 19.541(3) _cell_length_b 22.799(3) _cell_length_c 23.890(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.095(2) _cell_angle_gamma 90.00 _cell_volume 10366(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6228 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.97 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 2.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4736 _exptl_absorpt_correction_T_max 0.7737 _exptl_absorpt_process_details SADABS _exptl_special_details ; Crystals were grown from a mixture of acetonitrile and toluene. The large yellow crystals were poorly diffracting(low resolution due to the size of the complex). No high angle data was observed with increased frame times. Only the hexacationic trigonal bipyramidal cage could be resolved. Anions and solvent molecules in the void space were impossible to model and the electron density was removed using PLATON SQUEEZE. 1742 e/cell were removed (see end of cif for squeeze report). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65598 _diffrn_reflns_av_R_equivalents 0.1246 _diffrn_reflns_av_sigmaI/netI 0.1640 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 23.50 _reflns_number_total 15784 _reflns_number_gt 6989 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15784 _refine_ls_number_parameters 733 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1375 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.1978 _refine_ls_wR_factor_gt 0.1775 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.21878(4) 0.7500 0.66888(3) 0.0612(2) Uani 1 2 d S . . Pt2 Pt 0.24872(3) 0.7500 0.37357(3) 0.0572(2) Uani 1 2 d S . . Pt3 Pt 0.37173(4) 0.7500 0.94684(3) 0.0651(3) Uani 1 2 d S . . Rh1 Rh 0.15192(5) 0.48779(4) 0.65372(4) 0.0555(3) Uani 1 1 d . . . P1 P -0.30057(18) 0.68167(15) 0.67413(19) 0.0735(11) Uani 1 1 d . . . P2 P 0.26273(19) 0.68214(15) 0.30809(17) 0.0726(11) Uani 1 1 d . . . P3 P 0.4214(2) 0.68278(16) 1.01161(17) 0.0762(11) Uani 1 1 d . . . N1 N 0.1294(6) 0.4270(5) 0.7155(5) 0.069(3) Uani 1 1 d . . . N2 N 0.2389(5) 0.4292(4) 0.6579(5) 0.065(3) Uani 1 1 d . . . N3 N 0.0999(5) 0.4244(4) 0.5940(4) 0.054(3) Uani 1 1 d . . . N4 N -0.1408(4) 0.6882(4) 0.6620(4) 0.042(2) Uani 1 1 d . . . N5 N 0.2317(5) 0.6879(4) 0.4329(4) 0.049(2) Uani 1 1 d . . . N6 N 0.3269(5) 0.6878(4) 0.8848(4) 0.053(3) Uani 1 1 d . . . C1 C 0.1945(9) 0.3894(8) 0.7358(8) 0.117(6) Uani 1 1 d . . . H1A H 0.2081 0.3909 0.7783 0.140 Uiso 1 1 calc R . . H1B H 0.1823 0.3482 0.7247 0.140 Uiso 1 1 calc R . . C2 C 0.2494(9) 0.4044(7) 0.7156(7) 0.103(5) Uani 1 1 d . . . H2A H 0.2791 0.3690 0.7168 0.123 Uiso 1 1 calc R . . H2B H 0.2769 0.4331 0.7426 0.123 Uiso 1 1 calc R . . C3 C 0.2217(7) 0.3889(6) 0.6109(6) 0.081(4) Uani 1 1 d . . . H3A H 0.2229 0.3487 0.6268 0.098 Uiso 1 1 calc R . . H3B H 0.2588 0.3912 0.5888 0.098 Uiso 1 1 calc R . . C4 C 0.1547(8) 0.3973(7) 0.5716(8) 0.113(6) Uani 1 1 d . . . H4A H 0.1623 0.4215 0.5391 0.135 Uiso 1 1 calc R . . H4B H 0.1375 0.3585 0.5557 0.135 Uiso 1 1 calc R . . C5 C 0.0628(10) 0.3814(8) 0.6233(8) 0.122(7) Uani 1 1 d . . . H5A H 0.0126 0.3807 0.6033 0.147 Uiso 1 1 calc R . . H5B H 0.0824 0.3419 0.6195 0.147 Uiso 1 1 calc R . . C6 C 0.0678(8) 0.3931(6) 0.6827(7) 0.090(5) Uani 1 1 d . . . H6A H 0.0671 0.3549 0.7023 0.108 Uiso 1 1 calc R . . H6B H 0.0247 0.4145 0.6859 0.108 Uiso 1 1 calc R . . C7 C 0.1125(10) 0.4547(7) 0.7665(7) 0.122(6) Uani 1 1 d . . . H7A H 0.0814 0.4883 0.7545 0.183 Uiso 1 1 calc R . . H7B H 0.1559 0.4680 0.7926 0.183 Uiso 1 1 calc R . . H7C H 0.0889 0.4261 0.7864 0.183 Uiso 1 1 calc R . . C8 C 0.3071(6) 0.4596(6) 0.6534(6) 0.081(4) Uani 1 1 d . . . H8A H 0.3451 0.4307 0.6585 0.122 Uiso 1 1 calc R . . H8B H 0.3189 0.4898 0.6832 0.122 Uiso 1 1 calc R . . H8C H 0.3010 0.4780 0.6155 0.122 Uiso 1 1 calc R . . C9 C 0.0480(6) 0.4480(5) 0.5446(6) 0.073(4) Uani 1 1 d . . . H9A H 0.0721 0.4722 0.5210 0.110 Uiso 1 1 calc R . . H9B H 0.0136 0.4720 0.5584 0.110 Uiso 1 1 calc R . . H9C H 0.0238 0.4155 0.5214 0.110 Uiso 1 1 calc R . . C10 C 0.0675(6) 0.5372(5) 0.6534(5) 0.049(3) Uani 1 1 d . . . C11 C 0.0184(6) 0.5656(6) 0.6532(6) 0.070(4) Uani 1 1 d . . . C12 C -0.0367(7) 0.6096(6) 0.6544(7) 0.064(4) Uani 1 1 d . . . C13 C -0.0468(7) 0.6246(5) 0.7085(7) 0.075(4) Uani 1 1 d . . . H13 H -0.0180 0.6093 0.7428 0.091 Uiso 1 1 calc R . . C14 C -0.1013(7) 0.6633(6) 0.7092(6) 0.065(4) Uani 1 1 d . . . H14 H -0.1113 0.6727 0.7453 0.078 Uiso 1 1 calc R . . C15 C -0.1279(6) 0.6710(6) 0.6138(6) 0.061(3) Uani 1 1 d . . . H15 H -0.1575 0.6855 0.5794 0.073 Uiso 1 1 calc R . . C16 C -0.0768(7) 0.6346(6) 0.6085(7) 0.066(4) Uani 1 1 d . . . H16 H -0.0688 0.6265 0.5715 0.080 Uiso 1 1 calc R . . C17 C 0.1745(5) 0.5391(5) 0.5930(5) 0.051(3) Uani 1 1 d . . . C18 C 0.1902(5) 0.5694(5) 0.5563(6) 0.053(3) Uani 1 1 d . . . C19 C 0.2025(6) 0.6085(5) 0.5136(6) 0.058(3) Uani 1 1 d . . . C20 C 0.2731(7) 0.6232(6) 0.5097(6) 0.082(4) Uani 1 1 d . . . H20 H 0.3124 0.6069 0.5359 0.099 Uiso 1 1 calc R . . C21 C 0.2819(7) 0.6592(6) 0.4692(6) 0.068(4) Uani 1 1 d . . . H21 H 0.3287 0.6655 0.4656 0.082 Uiso 1 1 calc R . . C22 C 0.1640(6) 0.6736(5) 0.4358(5) 0.055(3) Uani 1 1 d . . . H22 H 0.1258 0.6905 0.4088 0.066 Uiso 1 1 calc R . . C23 C 0.1504(7) 0.6367(5) 0.4757(6) 0.064(4) Uani 1 1 d . . . H23 H 0.1029 0.6300 0.4774 0.077 Uiso 1 1 calc R . . C24 C 0.2014(6) 0.5426(6) 0.7117(6) 0.064(4) Uani 1 1 d . . . C25 C 0.2320(7) 0.5759(6) 0.7510(7) 0.067(4) Uani 1 1 d . . . C26 C 0.2632(7) 0.6151(5) 0.7947(6) 0.061(3) Uani 1 1 d . . . C27 C 0.3292(7) 0.6371(6) 0.7981(6) 0.070(4) Uani 1 1 d . . . H27 H 0.3544 0.6277 0.7696 0.084 Uiso 1 1 calc R . . C28 C 0.3575(7) 0.6720(6) 0.8419(6) 0.068(4) Uani 1 1 d . . . H28 H 0.4031 0.6869 0.8431 0.082 Uiso 1 1 calc R . . C29 C 0.2605(7) 0.6662(6) 0.8800(7) 0.089(5) Uani 1 1 d . . . H29 H 0.2360 0.6754 0.9090 0.107 Uiso 1 1 calc R . . C30 C 0.2280(7) 0.6316(6) 0.8346(7) 0.082(4) Uani 1 1 d . . . H30 H 0.1808 0.6194 0.8313 0.098 Uiso 1 1 calc R . . C31 C -0.3872(7) 0.7213(6) 0.6749(9) 0.141(7) Uani 1 1 d . . . H31A H -0.4228 0.7081 0.6410 0.169 Uiso 1 1 calc R . . H31B H -0.4029 0.7081 0.7094 0.169 Uiso 1 1 calc R . . C32 C -0.2754(8) 0.6359(6) 0.7378(7) 0.082(5) Uani 1 1 d . . . H32 H -0.2356 0.6110 0.7315 0.099 Uiso 1 1 calc R . . C33 C -0.2472(10) 0.6696(7) 0.7923(8) 0.116(6) Uani 1 1 d . . . H33A H -0.2861 0.6903 0.8042 0.140 Uiso 1 1 calc R . . H33B H -0.2128 0.6992 0.7857 0.140 Uiso 1 1 calc R . . C34 C -0.2102(11) 0.6255(9) 0.8417(9) 0.144(8) Uani 1 1 d . . . H34A H -0.1721 0.6037 0.8297 0.173 Uiso 1 1 calc R . . H34B H -0.1897 0.6473 0.8773 0.173 Uiso 1 1 calc R . . C35 C -0.2634(13) 0.5852(8) 0.8515(9) 0.148(8) Uani 1 1 d . . . H35A H -0.2995 0.6074 0.8659 0.178 Uiso 1 1 calc R . . H35B H -0.2416 0.5568 0.8816 0.178 Uiso 1 1 calc R . . C36 C -0.3013(11) 0.5495(8) 0.7937(11) 0.150(8) Uani 1 1 d . . . H36A H -0.2667 0.5235 0.7816 0.180 Uiso 1 1 calc R . . H36B H -0.3396 0.5247 0.8018 0.180 Uiso 1 1 calc R . . C37 C -0.3323(10) 0.5941(9) 0.7440(8) 0.130(7) Uani 1 1 d . . . H37A H -0.3498 0.5727 0.7076 0.156 Uiso 1 1 calc R . . H37B H -0.3721 0.6159 0.7534 0.156 Uiso 1 1 calc R . . C38 C -0.3217(9) 0.6316(7) 0.6131(7) 0.092(5) Uani 1 1 d . . . H38 H -0.3691 0.6154 0.6136 0.110 Uiso 1 1 calc R . . C39 C -0.2758(9) 0.5803(8) 0.6158(7) 0.111(6) Uani 1 1 d . . . H39A H -0.2722 0.5606 0.6533 0.133 Uiso 1 1 calc R . . H39B H -0.2282 0.5940 0.6143 0.133 Uiso 1 1 calc R . . C40 C -0.3007(16) 0.5332(12) 0.5660(9) 0.219(13) Uani 1 1 d . . . H40A H -0.2648 0.5024 0.5670 0.263 Uiso 1 1 calc R . . H40B H -0.3457 0.5147 0.5687 0.263 Uiso 1 1 calc R . . C41 C -0.3098(17) 0.5722(13) 0.5105(9) 0.203(14) Uani 1 1 d . . . H41A H -0.2624 0.5853 0.5075 0.244 Uiso 1 1 calc R . . H41B H -0.3283 0.5467 0.4769 0.244 Uiso 1 1 calc R . . C42 C -0.3528(16) 0.6219(13) 0.5053(12) 0.205(13) Uani 1 1 d . . . H42A H -0.4020 0.6093 0.5021 0.246 Uiso 1 1 calc R . . H42B H -0.3506 0.6429 0.4695 0.246 Uiso 1 1 calc R . . C43 C -0.3315(8) 0.6650(7) 0.5571(7) 0.102(5) Uani 1 1 d . . . H43A H -0.2872 0.6852 0.5553 0.122 Uiso 1 1 calc R . . H43B H -0.3685 0.6951 0.5551 0.122 Uiso 1 1 calc R . . C44 C 0.2724(11) 0.7192(6) 0.2458(7) 0.149(8) Uani 1 1 d . . . H44A H 0.3171 0.7061 0.2370 0.179 Uiso 1 1 calc R . . H44B H 0.2340 0.7061 0.2137 0.179 Uiso 1 1 calc R . . C45 C 0.3429(9) 0.6384(8) 0.3322(9) 0.128(7) Uani 1 1 d . . . H45 H 0.3310 0.6116 0.3618 0.154 Uiso 1 1 calc R . . C46 C 0.4057(8) 0.6713(8) 0.3647(9) 0.132(7) Uani 1 1 d . . . H46A H 0.3946 0.6882 0.3998 0.158 Uiso 1 1 calc R . . H46B H 0.4154 0.7043 0.3407 0.158 Uiso 1 1 calc R . . C47 C 0.4706(10) 0.6342(10) 0.3818(10) 0.163(9) Uani 1 1 d . . . H47A H 0.4670 0.6120 0.4166 0.196 Uiso 1 1 calc R . . H47B H 0.5111 0.6611 0.3932 0.196 Uiso 1 1 calc R . . C48 C 0.4887(14) 0.5896(12) 0.3381(15) 0.251(17) Uani 1 1 d . . . H48A H 0.5061 0.6106 0.3078 0.301 Uiso 1 1 calc R . . H48B H 0.5258 0.5624 0.3579 0.301 Uiso 1 1 calc R . . C49 C 0.4233(11) 0.5562(10) 0.3121(13) 0.211(13) Uani 1 1 d . . . H49A H 0.4114 0.5306 0.3420 0.253 Uiso 1 1 calc R . . H49B H 0.4331 0.5306 0.2814 0.253 Uiso 1 1 calc R . . C50 C 0.3559(9) 0.5962(7) 0.2853(8) 0.123(6) Uani 1 1 d . . . H50A H 0.3645 0.6188 0.2521 0.147 Uiso 1 1 calc R . . H50B H 0.3142 0.5710 0.2716 0.147 Uiso 1 1 calc R . . C51 C 0.1898(7) 0.6307(6) 0.2943(7) 0.079(4) Uani 1 1 d . . . H51 H 0.1497 0.6530 0.3035 0.094 Uiso 1 1 calc R . . C52 C 0.1978(7) 0.5782(6) 0.3326(7) 0.086(5) Uani 1 1 d . . . H52A H 0.2141 0.5913 0.3730 0.103 Uiso 1 1 calc R . . H52B H 0.2344 0.5523 0.3235 0.103 Uiso 1 1 calc R . . C53 C 0.1300(9) 0.5429(7) 0.3272(10) 0.122(7) Uani 1 1 d . . . H53A H 0.1387 0.5084 0.3531 0.147 Uiso 1 1 calc R . . H53B H 0.0934 0.5674 0.3383 0.147 Uiso 1 1 calc R . . C54 C 0.1059(13) 0.5232(9) 0.2657(12) 0.173(10) Uani 1 1 d . . . H54A H 0.0617 0.5006 0.2613 0.207 Uiso 1 1 calc R . . H54B H 0.1418 0.4970 0.2558 0.207 Uiso 1 1 calc R . . C55 C 0.0934(11) 0.5760(11) 0.2238(9) 0.154(9) Uani 1 1 d . . . H55A H 0.0799 0.5622 0.1835 0.185 Uiso 1 1 calc R . . H55B H 0.0555 0.6015 0.2315 0.185 Uiso 1 1 calc R . . C56 C 0.1624(12) 0.6090(9) 0.2345(11) 0.162(9) Uani 1 1 d . . . H56A H 0.1983 0.5829 0.2243 0.195 Uiso 1 1 calc R . . H56B H 0.1567 0.6430 0.2081 0.195 Uiso 1 1 calc R . . C57 C 0.4718(9) 0.7226(7) 1.0757(7) 0.139(8) Uani 1 1 d . . . H57A H 0.4538 0.7095 1.1092 0.167 Uiso 1 1 calc R . . H57B H 0.5213 0.7095 1.0824 0.167 Uiso 1 1 calc R . . C58 C 0.4826(9) 0.6359(9) 0.9881(9) 0.126(7) Uani 1 1 d . . . H58 H 0.5107 0.6211 1.0258 0.151 Uiso 1 1 calc R . . C59 C 0.466(2) 0.5884(11) 0.9614(19) 0.38(3) Uani 1 1 d . . . H59A H 0.4387 0.5971 0.9221 0.459 Uiso 1 1 calc R . . H59B H 0.4364 0.5649 0.9813 0.459 Uiso 1 1 calc R . . C60 C 0.5353(18) 0.5505(9) 0.9572(13) 0.28(2) Uani 1 1 d . . . H60A H 0.5609 0.5389 0.9963 0.334 Uiso 1 1 calc R . . H60B H 0.5206 0.5143 0.9348 0.334 Uiso 1 1 calc R . . C61 C 0.5824(17) 0.5851(13) 0.9294(15) 0.230(16) Uani 1 1 d . . . H61A H 0.6234 0.5610 0.9257 0.276 Uiso 1 1 calc R . . H61B H 0.5570 0.5973 0.8904 0.276 Uiso 1 1 calc R . . C62 C 0.6036(18) 0.6314(12) 0.961(2) 0.32(3) Uani 1 1 d . . . H62A H 0.6375 0.6534 0.9440 0.384 Uiso 1 1 calc R . . H62B H 0.6286 0.6184 0.9999 0.384 Uiso 1 1 calc R . . C63 C 0.5399(12) 0.6748(10) 0.9670(12) 0.219(13) Uani 1 1 d . . . H63A H 0.5575 0.7062 0.9953 0.263 Uiso 1 1 calc R . . H63B H 0.5191 0.6933 0.9295 0.263 Uiso 1 1 calc R . . C64 C 0.3584(9) 0.6371(6) 1.0355(8) 0.094(5) Uani 1 1 d . . . H64 H 0.3350 0.6126 1.0018 0.113 Uiso 1 1 calc R . . C65 C 0.3911(18) 0.5943(15) 1.0840(13) 0.268(17) Uani 1 1 d . . . H65A H 0.4068 0.6147 1.1213 0.322 Uiso 1 1 calc R . . H65B H 0.4310 0.5723 1.0751 0.322 Uiso 1 1 calc R . . C66 C 0.3182(17) 0.5480(11) 1.0836(17) 0.31(2) Uani 1 1 d . . . H66A H 0.2999 0.5313 1.0448 0.368 Uiso 1 1 calc R . . H66B H 0.3315 0.5155 1.1114 0.368 Uiso 1 1 calc R . . C67 C 0.2633(16) 0.5873(12) 1.1009(15) 0.257(19) Uani 1 1 d . . . H67A H 0.2208 0.5637 1.1007 0.309 Uiso 1 1 calc R . . H67B H 0.2819 0.6011 1.1408 0.309 Uiso 1 1 calc R . . C68 C 0.2465(13) 0.6300(9) 1.0701(13) 0.196(13) Uani 1 1 d . . . H68A H 0.2153 0.6542 1.0881 0.235 Uiso 1 1 calc R . . H68B H 0.2175 0.6155 1.0332 0.235 Uiso 1 1 calc R . . C69 C 0.2999(11) 0.6695(7) 1.0562(9) 0.145(8) Uani 1 1 d . . . H69A H 0.3212 0.6927 1.0907 0.174 Uiso 1 1 calc R . . H69B H 0.2767 0.6972 1.0259 0.174 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0485(4) 0.0435(4) 0.1003(6) 0.000 0.0351(4) 0.000 Pt2 0.0523(4) 0.0364(4) 0.0883(6) 0.000 0.0272(4) 0.000 Pt3 0.0700(5) 0.0461(4) 0.0790(6) 0.000 0.0166(4) 0.000 Rh1 0.0519(6) 0.0294(5) 0.0873(8) 0.0017(5) 0.0201(5) -0.0004(4) P1 0.054(2) 0.050(2) 0.125(3) 0.004(2) 0.039(2) 0.0006(17) P2 0.080(3) 0.039(2) 0.104(3) -0.005(2) 0.033(2) -0.0101(18) P3 0.080(3) 0.059(2) 0.087(3) 0.002(2) 0.012(2) 0.006(2) N1 0.083(8) 0.057(7) 0.071(8) -0.001(6) 0.027(7) 0.007(6) N2 0.074(8) 0.039(6) 0.084(9) 0.001(6) 0.021(6) 0.008(5) N3 0.044(6) 0.042(6) 0.077(7) -0.001(5) 0.017(6) 0.002(5) N4 0.038(5) 0.050(6) 0.035(6) -0.006(5) 0.000(5) -0.013(4) N5 0.046(6) 0.033(5) 0.071(7) 0.002(5) 0.018(5) 0.006(5) N6 0.069(7) 0.025(5) 0.062(7) -0.003(5) 0.006(6) 0.009(5) C1 0.089(13) 0.119(15) 0.148(16) 0.053(13) 0.037(12) 0.015(11) C2 0.107(14) 0.077(11) 0.126(15) 0.042(11) 0.029(12) 0.031(10) C3 0.070(10) 0.063(9) 0.109(12) -0.024(9) 0.017(9) 0.006(8) C4 0.080(11) 0.088(12) 0.158(16) -0.057(12) 0.002(12) 0.016(9) C5 0.145(17) 0.103(14) 0.111(15) -0.013(12) 0.014(13) -0.061(12) C6 0.097(12) 0.053(9) 0.129(15) -0.024(10) 0.044(11) -0.038(8) C7 0.184(18) 0.080(12) 0.121(14) 0.013(11) 0.073(14) -0.037(12) C8 0.046(8) 0.065(9) 0.131(13) -0.005(9) 0.015(8) 0.021(7) C9 0.058(8) 0.051(8) 0.104(11) -0.029(8) 0.006(8) -0.007(7) C10 0.034(7) 0.046(7) 0.062(8) 0.003(6) 0.002(6) -0.013(6) C11 0.033(7) 0.058(8) 0.122(12) 0.021(8) 0.024(8) 0.013(7) C12 0.055(9) 0.054(8) 0.092(11) -0.022(8) 0.038(9) -0.010(7) C13 0.062(9) 0.054(9) 0.114(13) -0.001(9) 0.030(9) 0.025(7) C14 0.076(9) 0.062(9) 0.057(9) -0.007(8) 0.015(8) -0.013(7) C15 0.049(8) 0.067(9) 0.066(10) 0.004(8) 0.012(7) -0.007(7) C16 0.052(8) 0.065(9) 0.083(11) -0.010(8) 0.019(8) 0.014(7) C17 0.016(5) 0.051(7) 0.087(10) -0.035(7) 0.016(6) -0.016(5) C18 0.033(7) 0.047(8) 0.089(10) 0.000(7) 0.031(7) -0.012(6) C19 0.048(8) 0.024(6) 0.106(11) -0.008(7) 0.028(8) -0.002(6) C20 0.051(9) 0.082(11) 0.102(12) 0.014(10) -0.006(8) 0.002(7) C21 0.049(8) 0.072(9) 0.090(11) 0.044(9) 0.031(8) -0.003(7) C22 0.052(8) 0.030(7) 0.083(10) 0.019(7) 0.017(7) 0.004(6) C23 0.051(8) 0.032(7) 0.112(11) 0.006(8) 0.022(8) -0.010(6) C24 0.051(8) 0.093(11) 0.061(9) 0.044(8) 0.041(7) 0.024(8) C25 0.063(9) 0.057(9) 0.077(11) -0.002(8) 0.008(8) 0.009(7) C26 0.075(10) 0.045(8) 0.058(9) 0.014(7) 0.007(8) 0.009(7) C27 0.066(9) 0.060(9) 0.088(11) -0.016(8) 0.027(8) -0.020(7) C28 0.053(8) 0.065(9) 0.089(11) -0.017(9) 0.022(8) 0.000(7) C29 0.074(10) 0.083(11) 0.125(14) -0.017(10) 0.052(10) -0.019(9) C30 0.069(10) 0.070(10) 0.109(13) -0.029(10) 0.025(10) -0.028(8) C31 0.072(10) 0.081(11) 0.29(2) 0.009(13) 0.090(13) -0.004(8) C32 0.116(12) 0.038(8) 0.111(13) -0.018(9) 0.062(10) -0.019(8) C33 0.172(18) 0.063(11) 0.130(16) 0.021(12) 0.069(14) 0.003(11) C34 0.19(2) 0.091(15) 0.18(2) -0.020(15) 0.088(18) -0.047(15) C35 0.25(3) 0.066(12) 0.136(18) -0.003(13) 0.065(18) 0.007(15) C36 0.137(17) 0.082(14) 0.25(3) 0.039(18) 0.076(18) 0.011(13) C37 0.160(18) 0.104(15) 0.133(17) -0.029(14) 0.047(14) -0.005(14) C38 0.098(12) 0.081(12) 0.094(13) 0.013(10) 0.017(10) -0.009(10) C39 0.106(13) 0.122(16) 0.106(14) -0.019(12) 0.027(11) -0.033(12) C40 0.36(4) 0.21(3) 0.088(17) -0.080(19) 0.06(2) 0.00(3) C41 0.35(4) 0.21(3) 0.049(14) -0.025(17) 0.042(18) 0.07(3) C42 0.24(3) 0.19(3) 0.18(3) -0.01(3) 0.04(2) -0.09(3) C43 0.090(11) 0.100(13) 0.115(14) -0.027(13) 0.023(10) -0.031(10) C44 0.29(2) 0.058(10) 0.124(14) -0.021(10) 0.090(15) -0.054(13) C45 0.105(14) 0.108(14) 0.20(2) -0.062(14) 0.100(14) -0.016(11) C46 0.059(10) 0.101(14) 0.22(2) -0.026(14) -0.005(12) 0.019(10) C47 0.100(15) 0.143(19) 0.26(3) -0.042(19) 0.066(17) -0.007(14) C48 0.19(3) 0.17(3) 0.45(5) -0.10(3) 0.20(3) 0.00(2) C49 0.098(16) 0.14(2) 0.41(4) -0.08(2) 0.08(2) 0.001(15) C50 0.115(14) 0.072(11) 0.20(2) -0.021(13) 0.085(14) 0.001(10) C51 0.077(10) 0.044(9) 0.107(13) -0.017(9) 0.005(9) 0.006(7) C52 0.064(9) 0.063(10) 0.139(14) -0.014(10) 0.040(9) -0.014(7) C53 0.104(13) 0.064(11) 0.22(2) 0.018(14) 0.074(15) -0.022(10) C54 0.20(3) 0.064(14) 0.24(3) 0.013(18) 0.03(2) 0.005(15) C55 0.129(17) 0.16(2) 0.17(2) -0.050(18) 0.021(15) -0.050(17) C56 0.17(2) 0.081(15) 0.24(3) 0.016(17) 0.07(2) 0.008(15) C57 0.142(15) 0.122(17) 0.123(13) 0.030(11) -0.036(11) 0.002(11) C58 0.086(12) 0.108(15) 0.20(2) 0.019(15) 0.061(13) 0.031(11) C59 0.51(6) 0.090(18) 0.73(8) -0.10(3) 0.53(6) -0.04(3) C60 0.47(5) 0.085(16) 0.40(4) 0.06(2) 0.35(4) 0.10(2) C61 0.28(4) 0.16(3) 0.32(4) 0.08(3) 0.22(3) 0.05(3) C62 0.27(4) 0.12(2) 0.70(9) -0.03(4) 0.37(5) -0.02(2) C63 0.19(2) 0.16(2) 0.37(4) 0.10(2) 0.19(3) 0.066(19) C64 0.115(13) 0.058(9) 0.126(14) 0.010(10) 0.062(12) 0.010(9) C65 0.33(5) 0.26(4) 0.21(3) 0.02(3) 0.03(3) 0.11(4) C66 0.30(4) 0.10(2) 0.61(7) 0.07(3) 0.31(5) -0.01(2) C67 0.30(4) 0.13(2) 0.46(5) 0.07(3) 0.31(4) 0.08(2) C68 0.23(3) 0.084(15) 0.34(4) 0.08(2) 0.20(3) 0.029(17) C69 0.22(2) 0.068(12) 0.186(19) 0.015(12) 0.133(18) -0.003(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N4 2.109(9) 4_575 ? Pt1 N4 2.109(9) . ? Pt1 P1 2.256(3) . ? Pt1 P1 2.256(3) 4_575 ? Pt2 N5 2.084(9) 4_575 ? Pt2 N5 2.084(9) . ? Pt2 P2 2.260(4) . ? Pt2 P2 2.260(4) 4_575 ? Pt3 N6 2.094(9) . ? Pt3 N6 2.094(9) 4_575 ? Pt3 P3 2.237(4) 4_575 ? Pt3 P3 2.237(4) . ? Rh1 C24 1.951(17) . ? Rh1 C17 1.989(14) . ? Rh1 C10 1.995(12) . ? Rh1 N3 2.120(9) . ? Rh1 N1 2.141(10) . ? Rh1 N2 2.147(10) . ? P1 C32 1.817(15) . ? P1 C38 1.824(16) . ? P1 C31 1.923(13) . ? P2 C44 1.758(15) . ? P2 C51 1.818(14) . ? P2 C45 1.837(18) . ? P3 C58 1.786(17) . ? P3 C64 1.802(15) . ? P3 C57 1.859(15) . ? N1 C7 1.475(17) . ? N1 C6 1.496(16) . ? N1 C1 1.520(17) . ? N2 C3 1.431(14) . ? N2 C2 1.462(16) . ? N2 C8 1.526(15) . ? N3 C4 1.441(15) . ? N3 C9 1.473(14) . ? N3 C5 1.485(17) . ? N4 C15 1.294(14) . ? N4 C14 1.341(14) . ? N5 C21 1.324(14) . ? N5 C22 1.380(13) . ? N6 C28 1.346(14) . ? N6 C29 1.369(15) . ? C1 C2 1.317(18) . ? C3 C4 1.441(17) . ? C5 C6 1.426(18) . ? C10 C11 1.158(14) . ? C11 C12 1.476(17) . ? C12 C16 1.323(16) . ? C12 C13 1.394(17) . ? C13 C14 1.387(16) . ? C15 C16 1.327(16) . ? C17 C18 1.210(15) . ? C18 C19 1.416(16) . ? C19 C23 1.362(16) . ? C19 C20 1.442(16) . ? C20 C21 1.310(16) . ? C22 C23 1.342(15) . ? C24 C25 1.250(17) . ? C25 C26 1.404(18) . ? C26 C30 1.350(16) . ? C26 C27 1.370(16) . ? C27 C28 1.331(16) . ? C29 C30 1.374(17) . ? C31 C31 1.31(3) 4_575 ? C32 C37 1.50(2) . ? C32 C33 1.505(19) . ? C33 C34 1.59(2) . ? C34 C35 1.45(2) . ? C35 C36 1.63(3) . ? C36 C37 1.58(2) . ? C38 C39 1.47(2) . ? C38 C43 1.513(19) . ? C39 C40 1.59(2) . ? C40 C41 1.57(3) . ? C41 C42 1.40(3) . ? C42 C43 1.56(3) . ? C44 C44 1.40(3) 4_575 ? C45 C46 1.50(2) . ? C45 C50 1.54(2) . ? C46 C47 1.50(2) . ? C47 C48 1.55(3) . ? C48 C49 1.50(3) . ? C49 C50 1.61(2) . ? C51 C52 1.492(18) . ? C51 C56 1.49(2) . ? C52 C53 1.531(18) . ? C53 C54 1.51(2) . ? C54 C55 1.55(3) . ? C55 C56 1.52(2) . ? C57 C57 1.25(3) 4_575 ? C58 C59 1.26(3) . ? C58 C63 1.60(2) . ? C59 C60 1.62(3) . ? C60 C61 1.48(3) . ? C61 C62 1.31(4) . ? C62 C63 1.62(3) . ? C64 C69 1.53(2) . ? C64 C65 1.54(3) . ? C65 C66 1.77(4) . ? C66 C67 1.52(3) . ? C67 C68 1.22(3) . ? C68 C69 1.47(2) . ? 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 N4 Pt1 N4 83.8(4) 4_575 . ? N4 Pt1 P1 177.9(3) 4_575 . ? N4 Pt1 P1 94.4(2) . . ? N4 Pt1 P1 94.4(2) 4_575 4_575 ? N4 Pt1 P1 177.9(3) . 4_575 ? P1 Pt1 P1 87.37(17) . 4_575 ? N5 Pt2 N5 85.7(5) 4_575 . ? N5 Pt2 P2 177.8(3) 4_575 . ? N5 Pt2 P2 93.9(2) . . ? N5 Pt2 P2 93.9(2) 4_575 4_575 ? N5 Pt2 P2 177.8(3) . 4_575 ? P2 Pt2 P2 86.39(19) . 4_575 ? N6 Pt3 N6 85.2(5) . 4_575 ? N6 Pt3 P3 178.5(3) . 4_575 ? N6 Pt3 P3 94.2(3) 4_575 4_575 ? N6 Pt3 P3 94.2(3) . . ? N6 Pt3 P3 178.5(3) 4_575 . ? P3 Pt3 P3 86.5(2) 4_575 . ? C24 Rh1 C17 89.2(4) . . ? C24 Rh1 C10 85.3(4) . . ? C17 Rh1 C10 89.1(4) . . ? C24 Rh1 N3 176.8(4) . . ? C17 Rh1 N3 93.5(4) . . ? C10 Rh1 N3 96.4(4) . . ? C24 Rh1 N1 94.1(4) . . ? C17 Rh1 N1 175.7(4) . . ? C10 Rh1 N1 94.0(4) . . ? N3 Rh1 N1 83.2(4) . . ? C24 Rh1 N2 96.1(4) . . ? C17 Rh1 N2 95.4(4) . . ? C10 Rh1 N2 175.3(4) . . ? N3 Rh1 N2 82.0(4) . . ? N1 Rh1 N2 81.4(4) . . ? C32 P1 C38 106.2(7) . . ? C32 P1 C31 109.5(7) . . ? C38 P1 C31 105.2(8) . . ? C32 P1 Pt1 112.5(5) . . ? C38 P1 Pt1 115.0(5) . . ? C31 P1 Pt1 108.2(4) . . ? C44 P2 C51 112.8(8) . . ? C44 P2 C45 106.2(9) . . ? C51 P2 C45 106.5(7) . . ? C44 P2 Pt2 108.0(5) . . ? C51 P2 Pt2 110.8(5) . . ? C45 P2 Pt2 112.5(6) . . ? C58 P3 C64 107.9(8) . . ? C58 P3 C57 106.5(9) . . ? C64 P3 C57 107.1(8) . . ? C58 P3 Pt3 114.2(7) . . ? C64 P3 Pt3 113.2(6) . . ? C57 P3 Pt3 107.5(5) . . ? C7 N1 C6 110.4(12) . . ? C7 N1 C1 107.9(13) . . ? C6 N1 C1 113.0(12) . . ? C7 N1 Rh1 114.4(8) . . ? C6 N1 Rh1 103.9(8) . . ? C1 N1 Rh1 107.3(9) . . ? C3 N2 C2 116.6(11) . . ? C3 N2 C8 106.9(10) . . ? C2 N2 C8 107.8(11) . . ? C3 N2 Rh1 108.7(8) . . ? C2 N2 Rh1 103.0(8) . . ? C8 N2 Rh1 114.1(7) . . ? C4 N3 C9 107.0(10) . . ? C4 N3 C5 112.0(13) . . ? C9 N3 C5 107.4(10) . . ? C4 N3 Rh1 105.0(8) . . ? C9 N3 Rh1 115.4(7) . . ? C5 N3 Rh1 110.1(9) . . ? C15 N4 C14 115.5(11) . . ? C15 N4 Pt1 124.2(8) . . ? C14 N4 Pt1 120.3(8) . . ? C21 N5 C22 115.3(9) . . ? C21 N5 Pt2 124.9(8) . . ? C22 N5 Pt2 119.8(7) . . ? C28 N6 C29 114.5(11) . . ? C28 N6 Pt3 122.3(9) . . ? C29 N6 Pt3 122.6(10) . . ? C2 C1 N1 115.4(14) . . ? C1 C2 N2 119.7(15) . . ? N2 C3 C4 116.3(12) . . ? N3 C4 C3 117.2(13) . . ? C6 C5 N3 114.5(13) . . ? C5 C6 N1 118.9(13) . . ? C11 C10 Rh1 179.7(13) . . ? C10 C11 C12 171.2(13) . . ? C16 C12 C13 118.7(12) . . ? C16 C12 C11 125.1(13) . . ? C13 C12 C11 116.2(14) . . ? C14 C13 C12 116.1(13) . . ? N4 C14 C13 123.7(12) . . ? N4 C15 C16 125.2(13) . . ? C12 C16 C15 120.6(13) . . ? C18 C17 Rh1 178.0(10) . . ? C17 C18 C19 174.1(12) . . ? C23 C19 C18 123.6(11) . . ? C23 C19 C20 115.5(12) . . ? C18 C19 C20 120.9(12) . . ? C21 C20 C19 118.8(12) . . ? C20 C21 N5 126.2(12) . . ? C23 C22 N5 122.0(11) . . ? C22 C23 C19 122.0(12) . . ? C25 C24 Rh1 176.7(11) . . ? C24 C25 C26 177.0(14) . . ? C30 C26 C27 118.7(14) . . ? C30 C26 C25 119.9(13) . . ? C27 C26 C25 121.4(14) . . ? C28 C27 C26 118.8(13) . . ? C27 C28 N6 125.7(12) . . ? N6 C29 C30 122.1(13) . . ? C26 C30 C29 120.0(13) . . ? C31 C31 P1 118.1(4) 4_575 . ? C37 C32 C33 111.8(13) . . ? C37 C32 P1 112.5(13) . . ? C33 C32 P1 114.1(10) . . ? C32 C33 C34 109.5(13) . . ? C35 C34 C33 107.4(18) . . ? C34 C35 C36 112.7(17) . . ? C37 C36 C35 109.8(15) . . ? C32 C37 C36 108.6(15) . . ? C39 C38 C43 113.1(15) . . ? C39 C38 P1 116.0(12) . . ? C43 C38 P1 110.6(11) . . ? C38 C39 C40 115.1(16) . . ? C41 C40 C39 101.9(19) . . ? C42 C41 C40 119(2) . . ? C41 C42 C43 113(2) . . ? C38 C43 C42 110.0(16) . . ? C44 C44 P2 118.7(5) 4_575 . ? C46 C45 C50 116.1(14) . . ? C46 C45 P2 115.6(12) . . ? C50 C45 P2 112.3(14) . . ? C45 C46 C47 113.6(15) . . ? C46 C47 C48 120(2) . . ? C49 C48 C47 107.9(19) . . ? C48 C49 C50 115(2) . . ? C45 C50 C49 108.5(17) . . ? C52 C51 C56 106.7(13) . . ? C52 C51 P2 115.9(10) . . ? C56 C51 P2 118.9(13) . . ? C51 C52 C53 113.7(13) . . ? C54 C53 C52 108.2(17) . . ? C53 C54 C55 111.6(18) . . ? C56 C55 C54 105.9(18) . . ? C51 C56 C55 115.9(19) . . ? C57 C57 P3 119.2(5) 4_575 . ? C59 C58 C63 116(2) . . ? C59 C58 P3 124(2) . . ? C63 C58 P3 109.5(14) . . ? C58 C59 C60 112(3) . . ? C61 C60 C59 111(2) . . ? C62 C61 C60 108(3) . . ? C61 C62 C63 113(3) . . ? C58 C63 C62 107.2(17) . . ? C69 C64 C65 105.9(17) . . ? C69 C64 P3 115.8(11) . . ? C65 C64 P3 114.1(18) . . ? C64 C65 C66 100(2) . . ? C67 C66 C65 105(2) . . ? C68 C67 C66 115(3) . . ? C67 C68 C69 121(3) . . ? C68 C69 C64 113.3(15) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.021 -0.005 0.001 5246.6 1742.8 2 0.122 0.009 0.451 20.7 -7.3 3 0.122 0.491 0.451 20.7 -6.6 4 0.878 0.509 0.549 20.7 -2.5 5 0.878 0.991 0.549 20.7 -1.1 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.181 _refine_diff_density_min -2.098 _refine_diff_density_rms 0.161 #===End