# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global #=================================================================== # 0. AUDIT DETAILS _audit_creation_date 28-Feb-01 _audit_creation_method 'PLATON option' _audit_update_record ; 25-Apr-01 Updated by the Author E.H. 16-May-01 Updated by the Author E.H. 23-Oct-01 Updated by the Author E.H. Textwriting by E.H. Checkcif OK 24-Oct-01 Updated by the Author E.H. ; #=================================================================== # 1. SUBMISSION DETAILS #=================================================================== _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Kuhn, Fritz E.' 'de Biani, F.F.' 'Herdtweck, Eberhardt' 'Santos, Ana M.' 'Zuo, J.-L.' _publ_contact_author_name 'Dr Fritz E Kuhn' _publ_contact_author_address ; Anorganisch-Chemisches Institut Technishe Universitat Munchen Litchtenbergstr 4 Muchen D-85747 Graching b. GERMANY ; _publ_contact_author_email 'FRITZ.KUEHN@CH.TUM.DE' _publ_requested_journal ' New J. Chem. ' _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; November 2001 ; _publ_section_title ; Ruthenium(II) Alkynyl-Hydride and Ruthenium(II) bis-(\s-Pyridylacetylide) as ligands and linkers for Metal-Metal Bonded Complexes ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. #===================================================================== # 4. TEXT #===================================================================== _publ_section_abstract ; The syntheses of new linear \p-conjugated building blocks, ruthenium (II) alkynyl-hydride... ; # Insert blank lines between paragraphs _publ_section_comment ; none ; _publ_section_experimental ; none ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Nonius (2000a). Data Collection Software for Nonius Kappa-CCD devices. Nonius BV, Delft, The Netherlands. Nonius (2000b). DENZO Processing Software for Nonius Kappa-CCD devices, Nonius BV, Delft, The Netherlands. Sheldrick, G. M. (1998). SHELXL97, University of Gottingen, Gottingen, Germany. Spek, A. L. (2001). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; View of the title compound with the appropriate atom numbering scheme Displacement ellipsoids for non-H atoms are drawn at the 50% probability level ; _publ_section_acknowledgements ; none ; _publ_section_table_legends ; none ; #=================================================================== data_ZUOD-4113-123 _database_code_CSD 184199 #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[(C126 H116 N2 O8 P8 Rh2 Ru2)H1.82 / Cl0.18], 3.764(C H Cl3)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C129.76 H121.59 Cl11.47 N2 O8 P8 Rh2 Ru2' _chemical_formula_weight 2899.50 _chemical_compound_source 'see text' 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.6709(1) _cell_length_b 16.4638(1) _cell_length_c 17.1025(1) _cell_angle_alpha 105.3292(3) _cell_angle_beta 109.3507(3) _cell_angle_gamma 99.4126(5) _cell_volume 3120.36(4) _cell_formula_units_Z 1 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 11394 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 25.54 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'red-brown' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method none _exptl_crystal_F_000 1471.1 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.6814 _exptl_absorpt_correction_T_max 0.7991 _exptl_absorpt_process_details ; not applied ; _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 20 s per film repetition 1 913 films measured in 7 data sets set 1: phi-scan with delta_phi = 1.0 set 2 to set 7 omega-scan with delta_omega = 1.0 ; _publ_section_exptl_prep ; the crystal was fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS; source: 'Denzo-SMN (Nonius)' The hydride hydrogen atom could be located in the difference Fourier maps and refined freely. All other hydrogen atoms were calculated in ideal positions (riding model). The crystal exhibits a second compound to be incorporated - the chloro analogue. Two phenyl groups are disordered over two positions. Both solvent molecules show a SOF less than 1.0. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Kappa CCD (Nonius)' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 59877 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.54 _reflns_number_total 11463 _reflns_number_gt 10438 # number of observed reflections (> n sig(I)) _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2000a)' _computing_cell_refinement 'DENZO (Nonius, 2000b)' _computing_data_reduction 'DENZO (Nonius, 2000b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+4.9224P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # see text _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 11463 _refine_ls_number_parameters 781 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.54 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.119 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.068 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Rh Rh Uani 0.45138(1) 0.45942(1) 0.92250(1) 1.000 0.0150(1) Ru Ru Uani 0.04346(1) 0.13639(1) 0.29437(1) 1.000 0.0131(1) P1 P Uani -0.02477(5) 0.24972(4) 0.26028(4) 1.000 0.0159(2) P2 P Uani 0.18814(5) 0.19273(4) 0.25203(4) 1.000 0.0170(2) P3 P Uani 0.10858(5) 0.01663(4) 0.31891(4) 1.000 0.0173(2) P4 P Uani -0.11010(5) 0.07543(4) 0.32530(4) 1.000 0.0159(2) O1 O Uani 0.34037(14) 0.53676(10) 0.91743(10) 1.000 0.0204(5) O2 O Uani 0.56006(14) 0.54983(11) 0.90211(10) 1.000 0.0211(5) O3 O Uani 0.56888(14) 0.38766(11) 0.93650(10) 1.000 0.0214(5) O4 O Uani 0.34912(14) 0.37405(10) 0.95223(10) 1.000 0.0206(5) N11 N Uani 0.35848(17) 0.38183(12) 0.77947(12) 1.000 0.0186(6) C1 C Uani 0.3539(2) 0.59559(15) 0.98751(16) 1.000 0.0212(7) C2 C Uani 0.2701(2) 0.65119(17) 0.97980(18) 1.000 0.0292(8) C3 C Uani 0.6358(2) 0.61254(16) 0.96789(15) 1.000 0.0206(7) C4 C Uani 0.7149(2) 0.67640(17) 0.94974(17) 1.000 0.0292(8) C5 C Uani 0.1699(2) 0.23402(17) 0.50795(16) 1.000 0.0233(7) C6 C Uani 0.12285(19) 0.20047(14) 0.42947(15) 1.000 0.0162(7) C7 C Uani 0.0086(2) 0.25959(16) 0.16571(15) 1.000 0.0217(7) C8 C Uani 0.1338(2) 0.25944(17) 0.18199(16) 1.000 0.0235(7) C9 C Uani 0.0012(2) -0.04866(17) 0.34672(19) 1.000 0.0302(9) C10 C Uani -0.0532(2) 0.01176(16) 0.39514(16) 1.000 0.0217(7) C12 C Uani 0.3475(2) 0.41832(16) 0.71698(16) 1.000 0.0233(7) C13 C Uani 0.2885(2) 0.37214(17) 0.62846(16) 1.000 0.0246(8) C14 C Uani 0.2341(2) 0.28254(16) 0.59938(15) 1.000 0.0211(7) C15 C Uani 0.2470(2) 0.24464(16) 0.66478(16) 1.000 0.0266(7) C16 C Uani 0.3087(2) 0.29551(16) 0.75227(16) 1.000 0.0263(8) C21 C Uani -0.1793(2) 0.24603(16) 0.21738(15) 1.000 0.0197(7) C22 C Uani -0.2209(2) 0.31748(18) 0.24302(17) 1.000 0.0282(8) C23 C Uani -0.3385(3) 0.3107(2) 0.2048(2) 1.000 0.0376(9) C24 C Uani -0.4155(2) 0.2337(2) 0.14254(18) 1.000 0.0367(9) C25 C Uani -0.3753(2) 0.16221(19) 0.11574(17) 1.000 0.0309(8) C26 C Uani -0.2578(2) 0.16866(17) 0.15271(16) 1.000 0.0237(7) C31 C Uani 0.0426(2) 0.35854(15) 0.34457(15) 1.000 0.0198(7) C32 C Uani 0.1023(2) 0.42933(16) 0.33193(18) 1.000 0.0273(8) C33 C Uani 0.1573(2) 0.50893(17) 0.4007(2) 1.000 0.0325(9) C34 C Uani 0.1532(2) 0.51897(17) 0.48212(18) 1.000 0.0303(8) C35 C Uani 0.0930(2) 0.44880(17) 0.49518(17) 1.000 0.0275(8) C36 C Uani 0.0382(2) 0.36932(16) 0.42696(16) 1.000 0.0223(7) C41 C Uani 0.2366(2) 0.11517(17) 0.18262(18) 1.000 0.0278(8) C42 C Uani 0.1639(3) 0.07023(18) 0.09333(19) 1.000 0.0361(9) C43 C Uani 0.1946(3) 0.0086(2) 0.0398(2) 1.000 0.0461(11) C44 C Uani 0.2976(4) -0.0089(2) 0.0741(3) 1.000 0.0591(14) C45 C Uani 0.3717(4) 0.0319(3) 0.1621(3) 1.000 0.0753(18) C46 C Uani 0.3397(3) 0.0951(2) 0.2177(3) 1.000 0.0545(11) C51 C Uani 0.3242(5) 0.2750(4) 0.3292(3) 0.736(6) 0.0214(16) C52 C Uani 0.4129(4) 0.3005(4) 0.3017(3) 0.736(6) 0.0275(14) C53 C Uani 0.5131(4) 0.3663(4) 0.3592(4) 0.736(6) 0.0330(14) C54 C Uani 0.5277(4) 0.4069(3) 0.4445(4) 0.736(6) 0.0364(14) C55 C Uani 0.4409(4) 0.3823(3) 0.4726(3) 0.736(6) 0.0395(12) C56 C Uani 0.3400(3) 0.3173(2) 0.4149(2) 0.736(6) 0.0306(12) C61 C Uani 0.1184(2) -0.07073(15) 0.23118(16) 1.000 0.0215(7) C62 C Uani 0.0355(3) -0.09587(18) 0.14647(17) 1.000 0.0329(8) C63 C Uani 0.0332(3) -0.16585(19) 0.07916(18) 1.000 0.0357(9) C64 C Uani 0.1159(3) -0.2093(2) 0.0946(2) 1.000 0.0430(10) C65 C Uani 0.2029(3) -0.1825(3) 0.1770(2) 1.000 0.0630(12) C66 C Uani 0.2034(3) -0.1141(2) 0.2451(2) 1.000 0.0504(11) C71 C Uani 0.2404(4) 0.0357(3) 0.4141(2) 0.744(3) 0.0208(11) C72 C Uani 0.3282(3) 0.1119(2) 0.4415(2) 0.744(3) 0.0251(10) C73 C Uani 0.4325(3) 0.1304(3) 0.5137(2) 0.744(3) 0.0341(11) C74 C Uani 0.4491(3) 0.0726(3) 0.5584(2) 0.744(3) 0.0377(13) C75 C Uani 0.3635(3) -0.0045(3) 0.5308(2) 0.744(3) 0.0374(14) C76 C Uani 0.2601(3) -0.0233(3) 0.4590(2) 0.744(3) 0.0298(11) C81 C Uani -0.2395(2) -0.01061(16) 0.23967(16) 1.000 0.0231(7) C82 C Uani -0.3262(2) -0.05078(18) 0.26116(18) 1.000 0.0322(8) C83 C Uani -0.4199(3) -0.1196(2) 0.1970(2) 1.000 0.0422(10) C84 C Uani -0.4276(3) -0.1487(2) 0.1116(2) 1.000 0.0424(9) C85 C Uani -0.3428(3) -0.10977(18) 0.08953(18) 1.000 0.0365(9) C86 C Uani -0.2488(2) -0.04128(17) 0.15321(16) 1.000 0.0270(8) C91 C Uani -0.1744(2) 0.14421(15) 0.38844(16) 1.000 0.0204(7) C92 C Uani -0.1168(2) 0.18504(16) 0.47921(17) 1.000 0.0265(8) C93 C Uani -0.1659(3) 0.23749(18) 0.5270(2) 1.000 0.0370(9) C94 C Uani -0.2720(3) 0.24973(18) 0.4848(2) 1.000 0.0398(10) C95 C Uani -0.3291(3) 0.2109(2) 0.3944(2) 1.000 0.0381(10) C96 C Uani -0.2808(2) 0.15862(18) 0.34676(19) 1.000 0.0295(8) Cl Cl Uani -0.0360(6) 0.0645(4) 0.1346(4) 0.089(4) 0.027(2) C55A C Uiso 0.4732(6) 0.3305(5) 0.4838(4) 0.264(6) 0.024(2) C56A C Uiso 0.3714(6) 0.2698(5) 0.4192(4) 0.264(6) 0.019(2) C71A C Uiso 0.2655(4) 0.0463(5) 0.4031(3) 0.256(3) 0.009(3) C72A C Uiso 0.3588(5) 0.0482(4) 0.3773(3) 0.256(3) 0.025(2) C73A C Uiso 0.4721(4) 0.0802(5) 0.4405(4) 0.256(3) 0.029(2) C74A C Uiso 0.4923(4) 0.1103(5) 0.5296(4) 0.256(3) 0.030(2) C75A C Uiso 0.3990(5) 0.1084(4) 0.5554(3) 0.256(3) 0.026(2) C76A C Uiso 0.2857(5) 0.0764(4) 0.4922(4) 0.256(3) 0.020(2) C53A C Uiso 0.5050(8) 0.3871(6) 0.3748(6) 0.264(6) 0.025(5) C54A C Uiso 0.5400(6) 0.3892(5) 0.4616(5) 0.264(6) 0.021(4) C51A C Uiso 0.3364(7) 0.2678(6) 0.3324(4) 0.264(6) 0.012(5) C52A C Uiso 0.4032(9) 0.3264(7) 0.3102(5) 0.264(6) 0.026(4) Cl1 Cl Uani 0.36324(7) 0.50885(6) 0.28074(5) 0.949(2) 0.0430(3) Cl2 Cl Uani 0.41939(8) 0.68975(6) 0.29180(6) 0.949(2) 0.0526(3) Cl3 Cl Uani 0.20249(8) 0.56841(8) 0.16135(7) 0.949(2) 0.0628(4) C20 C Uani 0.3495(3) 0.5812(2) 0.22090(19) 0.949(2) 0.0321(9) Cl4 Cl Uani 0.91524(7) 0.56763(5) 0.07214(5) 0.933(2) 0.0387(2) Cl5 Cl Uani 0.96155(9) 0.72196(6) 0.22176(7) 0.933(2) 0.0565(3) Cl6 Cl Uani 0.95005(8) 0.55609(6) 0.24490(6) 0.933(2) 0.0505(3) C30 C Uani 0.8954(3) 0.60998(19) 0.17088(19) 0.933(2) 0.0307(9) H92 H Uiso 0.04050 -0.08010 0.38440 1.000 0.0360 H82 H Uiso 0.14000 0.23580 0.12460 1.000 0.0280 H91 H Uiso -0.06020 -0.09260 0.29200 1.000 0.0360 H72 H Uiso -0.00390 0.31470 0.15640 1.000 0.0260 H81 H Uiso 0.18400 0.32050 0.21130 1.000 0.0280 H151 H Uiso 0.21310 0.18370 0.64900 1.000 0.0320 H161 H Uiso 0.31630 0.26800 0.79540 1.000 0.0320 H221 H Uiso -0.16870 0.37090 0.28670 1.000 0.0340 H231 H Uiso -0.36610 0.36000 0.22190 1.000 0.0450 H241 H Uiso -0.49620 0.22950 0.11790 1.000 0.0440 H251 H Uiso -0.42810 0.10900 0.07220 1.000 0.0370 H261 H Uiso -0.23020 0.11980 0.13380 1.000 0.0280 H321 H Uiso 0.10560 0.42330 0.27600 1.000 0.0330 H331 H Uiso 0.19810 0.55690 0.39150 1.000 0.0390 H341 H Uiso 0.19130 0.57350 0.52900 1.000 0.0360 H351 H Uiso 0.08950 0.45540 0.55110 1.000 0.0330 H101 H Uiso 0.00580 0.05130 0.45340 1.000 0.0260 H102 H Uiso -0.11690 -0.02290 0.40420 1.000 0.0260 H121 H Uiso 0.38240 0.47940 0.73480 1.000 0.0280 H131 H Uiso 0.28460 0.40120 0.58690 1.000 0.0300 H451 H Uiso 0.44290 0.01780 0.18490 1.000 0.0900 H461 H Uiso 0.38890 0.12330 0.27840 1.000 0.0650 H521 H Uiso 0.40410 0.27220 0.24290 0.736(6) 0.0330 H531 H Uiso 0.57210 0.38350 0.33930 0.736(6) 0.0400 H541 H Uiso 0.59710 0.45160 0.48420 0.736(6) 0.0440 H551 H Uiso 0.45060 0.41020 0.53170 0.736(6) 0.0470 H561 H Uiso 0.28060 0.30160 0.43480 0.736(6) 0.0370 H621 H Uiso -0.02110 -0.06460 0.13410 1.000 0.0390 H631 H Uiso -0.02650 -0.18350 0.02190 1.000 0.0430 H641 H Uiso 0.11350 -0.25790 0.04860 1.000 0.0520 H651 H Uiso 0.26310 -0.21080 0.18750 1.000 0.0760 H661 H Uiso 0.26330 -0.09690 0.30220 1.000 0.0610 H721 H Uiso 0.31750 0.15220 0.41070 0.744(3) 0.0300 H731 H Uiso 0.49180 0.18300 0.53190 0.744(3) 0.0410 H741 H Uiso 0.51930 0.08550 0.60820 0.744(3) 0.0450 H751 H Uiso 0.37560 -0.04500 0.56120 0.744(3) 0.0450 H761 H Uiso 0.20210 -0.07690 0.44020 0.744(3) 0.0350 H821 H Uiso -0.32140 -0.03110 0.32000 1.000 0.0390 H831 H Uiso -0.47880 -0.14660 0.21230 1.000 0.0510 H841 H Uiso -0.49160 -0.19570 0.06800 1.000 0.0510 H851 H Uiso -0.34830 -0.12970 0.03050 1.000 0.0440 H861 H Uiso -0.19020 -0.01510 0.13740 1.000 0.0320 H921 H Uiso -0.04330 0.17710 0.50890 1.000 0.0320 H931 H Uiso -0.12590 0.26500 0.58900 1.000 0.0440 H941 H Uiso -0.30590 0.28470 0.51770 1.000 0.0480 H951 H Uiso -0.40170 0.22010 0.36490 1.000 0.0460 H961 H Uiso -0.32080 0.13210 0.28460 1.000 0.0350 H361 H Uiso -0.00300 0.32160 0.43640 1.000 0.0270 H421 H Uiso 0.09190 0.08270 0.06930 1.000 0.0430 H431 H Uiso 0.14430 -0.02130 -0.02040 1.000 0.0550 H441 H Uiso 0.31970 -0.05030 0.03670 1.000 0.0710 H H Uiso -0.018(3) 0.084(2) 0.190(3) 0.911(4) 0.031(9) H21 H Uiso 0.19300 0.61530 0.93560 1.000 0.0350 H22 H Uiso 0.29770 0.69950 0.96180 1.000 0.0350 H23 H Uiso 0.26500 0.67490 1.03700 1.000 0.0350 H41 H Uiso 0.75280 0.73000 1.00150 1.000 0.0350 H42 H Uiso 0.66950 0.69060 0.89890 1.000 0.0350 H43 H Uiso 0.77420 0.65040 0.93690 1.000 0.0350 H71 H Uiso -0.04440 0.21010 0.11180 1.000 0.0260 H52A H Uiso 0.37930 0.32500 0.25090 0.264(6) 0.0310 H53A H Uiso 0.55060 0.42720 0.35960 0.264(6) 0.0300 H54A H Uiso 0.60950 0.43060 0.50570 0.264(6) 0.0250 H55A H Uiso 0.49710 0.33190 0.54310 0.264(6) 0.0290 H56A H Uiso 0.32580 0.22970 0.43440 0.264(6) 0.0230 H72A H Uiso 0.34500 0.02760 0.31640 0.256(3) 0.0300 H73A H Uiso 0.53580 0.08150 0.42290 0.256(3) 0.0350 H74A H Uiso 0.56970 0.13210 0.57280 0.256(3) 0.0360 H75A H Uiso 0.41280 0.12900 0.61630 0.256(3) 0.0310 H76A H Uiso 0.22190 0.07510 0.50980 0.256(3) 0.0240 H201 H Uiso 0.38750 0.56640 0.17820 0.949(2) 0.0380 H301 H Uiso 0.81000 0.59980 0.15610 0.933(2) 0.0370 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 Rh 0.0156(1) 0.0162(1) 0.0093(1) 0.0019(1) 0.0032(1) 0.0021(1) Ru 0.0138(1) 0.0133(1) 0.0095(1) 0.0030(1) 0.0025(1) 0.0026(1) P1 0.0167(3) 0.0168(3) 0.0145(3) 0.0069(2) 0.0050(2) 0.0049(2) P2 0.0176(3) 0.0187(3) 0.0147(3) 0.0056(2) 0.0066(2) 0.0044(2) P3 0.0199(3) 0.0160(3) 0.0142(3) 0.0044(2) 0.0044(2) 0.0061(2) P4 0.0169(3) 0.0159(3) 0.0125(3) 0.0044(2) 0.0044(2) 0.0020(2) O1 0.0199(8) 0.0219(8) 0.0162(8) 0.0049(7) 0.0042(7) 0.0064(7) O2 0.0236(9) 0.0224(9) 0.0143(8) 0.0052(7) 0.0066(7) 0.0019(7) O3 0.0221(9) 0.0228(9) 0.0167(8) 0.0031(7) 0.0069(7) 0.0072(7) O4 0.0213(8) 0.0204(8) 0.0150(8) 0.0042(7) 0.0051(7) 0.0000(7) N11 0.0201(10) 0.0184(10) 0.0127(9) 0.0024(8) 0.0039(8) 0.0041(8) C1 0.0215(12) 0.0205(12) 0.0232(13) 0.0086(10) 0.0101(10) 0.0054(10) C2 0.0295(14) 0.0288(14) 0.0283(14) 0.0078(11) 0.0092(11) 0.0134(11) C3 0.0201(12) 0.0219(12) 0.0204(12) 0.0071(10) 0.0083(10) 0.0065(10) C4 0.0300(14) 0.0291(14) 0.0256(13) 0.0093(11) 0.0116(11) -0.0006(11) C5 0.0195(12) 0.0289(13) 0.0169(12) 0.0037(10) 0.0053(10) 0.0059(10) C6 0.0152(11) 0.0162(11) 0.0206(12) 0.0089(9) 0.0078(9) 0.0068(9) C7 0.0252(13) 0.0258(13) 0.0167(11) 0.0106(10) 0.0081(10) 0.0088(10) C8 0.0255(13) 0.0296(13) 0.0209(12) 0.0136(11) 0.0115(10) 0.0083(11) C9 0.0416(16) 0.0226(13) 0.0407(16) 0.0184(12) 0.0253(13) 0.0142(12) C10 0.0282(13) 0.0219(12) 0.0199(12) 0.0108(10) 0.0117(10) 0.0086(10) C12 0.0284(13) 0.0195(12) 0.0199(12) 0.0062(10) 0.0071(10) 0.0070(10) C13 0.0310(14) 0.0272(13) 0.0160(12) 0.0096(10) 0.0069(10) 0.0104(11) C14 0.0172(12) 0.0297(13) 0.0124(11) 0.0019(10) 0.0047(9) 0.0075(10) C15 0.0337(14) 0.0201(12) 0.0185(12) 0.0025(10) 0.0081(11) -0.0004(11) C16 0.0362(15) 0.0230(13) 0.0154(12) 0.0067(10) 0.0073(11) 0.0033(11) C21 0.0195(12) 0.0248(12) 0.0175(11) 0.0117(10) 0.0063(9) 0.0080(10) C22 0.0261(13) 0.0296(14) 0.0275(13) 0.0090(11) 0.0075(11) 0.0121(11) C23 0.0329(16) 0.0435(17) 0.0385(16) 0.0112(14) 0.0132(13) 0.0227(13) C24 0.0211(14) 0.0566(19) 0.0296(15) 0.0134(14) 0.0052(11) 0.0162(13) C25 0.0225(13) 0.0394(16) 0.0230(13) 0.0083(12) 0.0031(11) 0.0049(11) C26 0.0228(13) 0.0263(13) 0.0208(12) 0.0091(10) 0.0057(10) 0.0081(10) C31 0.0167(11) 0.0191(12) 0.0215(12) 0.0070(10) 0.0040(9) 0.0066(9) C32 0.0296(14) 0.0207(12) 0.0319(14) 0.0086(11) 0.0138(11) 0.0050(11) C33 0.0294(14) 0.0209(13) 0.0453(17) 0.0088(12) 0.0161(13) 0.0029(11) C34 0.0244(13) 0.0192(13) 0.0346(15) -0.0018(11) 0.0059(11) 0.0036(10) C35 0.0266(13) 0.0281(13) 0.0234(13) 0.0041(11) 0.0060(11) 0.0118(11) C36 0.0220(12) 0.0206(12) 0.0248(13) 0.0086(10) 0.0077(10) 0.0087(10) C41 0.0342(15) 0.0225(13) 0.0325(14) 0.0073(11) 0.0214(12) 0.0084(11) C42 0.0523(19) 0.0294(15) 0.0300(15) 0.0061(12) 0.0249(14) 0.0081(13) C43 0.062(2) 0.0393(17) 0.0399(18) 0.0052(14) 0.0327(17) 0.0083(16) C44 0.069(3) 0.045(2) 0.060(2) -0.0052(17) 0.043(2) 0.0080(18) C45 0.048(2) 0.062(3) 0.119(4) 0.019(3) 0.038(3) 0.032(2) C46 0.0443(19) 0.0436(19) 0.064(2) -0.0016(17) 0.0182(17) 0.0219(16) C51 0.016(2) 0.022(3) 0.027(3) 0.0101(18) 0.0072(15) 0.0073(19) C52 0.023(2) 0.032(3) 0.030(2) 0.0155(17) 0.0108(17) 0.0052(19) C53 0.022(2) 0.035(2) 0.045(3) 0.017(2) 0.016(2) 0.004(2) C54 0.023(2) 0.031(2) 0.045(3) 0.013(2) 0.0058(18) -0.0029(18) C55 0.041(2) 0.032(2) 0.030(2) -0.0006(17) 0.0129(18) -0.0087(18) C56 0.028(2) 0.026(2) 0.032(2) 0.0042(16) 0.0149(16) -0.0045(15) C61 0.0245(12) 0.0174(11) 0.0223(12) 0.0048(10) 0.0104(10) 0.0061(10) C62 0.0393(16) 0.0337(15) 0.0241(13) 0.0057(12) 0.0088(12) 0.0210(13) C63 0.0455(17) 0.0339(15) 0.0210(13) 0.0012(12) 0.0105(12) 0.0126(13) C64 0.0519(19) 0.0343(16) 0.0352(16) -0.0040(13) 0.0172(15) 0.0188(14) C65 0.061(2) 0.066(2) 0.053(2) -0.0002(18) 0.0143(18) 0.046(2) C66 0.0435(19) 0.058(2) 0.0344(17) -0.0011(15) 0.0021(14) 0.0309(17) C71 0.0181(17) 0.029(2) 0.0219(19) 0.0091(16) 0.0130(17) 0.0116(15) C72 0.0237(18) 0.0299(19) 0.0214(17) 0.0083(14) 0.0071(14) 0.0110(15) C73 0.0200(18) 0.040(2) 0.029(2) -0.0015(17) 0.0039(15) 0.0086(16) C74 0.028(2) 0.064(3) 0.0179(17) 0.0093(18) 0.0041(15) 0.023(2) C75 0.036(2) 0.063(3) 0.030(2) 0.028(2) 0.0167(17) 0.029(2) C76 0.0302(19) 0.038(2) 0.033(2) 0.0215(17) 0.0165(16) 0.0159(16) C81 0.0223(12) 0.0197(12) 0.0206(12) 0.0067(10) 0.0034(10) -0.0002(10) C82 0.0281(14) 0.0359(15) 0.0260(14) 0.0114(12) 0.0074(11) -0.0028(12) C83 0.0291(15) 0.0392(17) 0.0469(18) 0.0193(14) 0.0060(13) -0.0085(13) C84 0.0362(17) 0.0314(16) 0.0332(16) 0.0069(13) -0.0059(13) -0.0105(13) C85 0.0386(16) 0.0297(15) 0.0236(14) 0.0036(12) 0.0006(12) -0.0020(12) C86 0.0278(14) 0.0244(13) 0.0212(13) 0.0045(10) 0.0055(11) 0.0017(11) C91 0.0212(12) 0.0173(11) 0.0248(12) 0.0090(10) 0.0115(10) 0.0026(9) C92 0.0217(13) 0.0245(13) 0.0271(13) 0.0007(11) 0.0108(11) 0.0013(10) C93 0.0371(16) 0.0263(14) 0.0341(15) -0.0076(12) 0.0175(13) -0.0033(12) C94 0.0398(17) 0.0235(14) 0.062(2) 0.0052(14) 0.0352(16) 0.0076(12) C95 0.0350(16) 0.0409(17) 0.057(2) 0.0267(15) 0.0276(15) 0.0216(13) C96 0.0285(14) 0.0381(15) 0.0324(14) 0.0210(12) 0.0154(12) 0.0139(12) Cl 0.031(4) 0.025(4) 0.011(4) 0.000(3) -0.002(3) 0.007(3) Cl1 0.0450(5) 0.0466(5) 0.0356(4) 0.0158(4) 0.0173(4) 0.0024(4) Cl2 0.0589(6) 0.0362(5) 0.0484(5) 0.0008(4) 0.0158(4) 0.0106(4) Cl3 0.0335(5) 0.0912(8) 0.0514(6) 0.0180(5) 0.0065(4) 0.0178(5) C20 0.0308(15) 0.0375(16) 0.0274(15) 0.0060(13) 0.0147(12) 0.0095(13) Cl4 0.0356(4) 0.0417(4) 0.0368(4) 0.0112(3) 0.0139(3) 0.0098(3) Cl5 0.0638(6) 0.0347(5) 0.0590(6) 0.0073(4) 0.0238(5) -0.0022(4) Cl6 0.0468(5) 0.0604(6) 0.0413(5) 0.0267(4) 0.0059(4) 0.0162(4) C30 0.0251(15) 0.0272(15) 0.0298(15) 0.0064(12) 0.0028(12) 0.0040(12) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh O1 2.0423(18) . . yes Rh O2 2.0385(19) . . yes Rh O3 2.0392(19) . . yes Rh O4 2.0327(18) . . yes Rh N11 2.2246(18) . . yes Rh Rh 2.3991(2) . 2_667 yes Ru P1 2.3103(7) . . yes Ru P2 2.3290(7) . . yes Ru P3 2.3419(7) . . yes Ru P4 2.3231(7) . . yes Ru C6 2.071(2) . . yes Ru Cl 2.441(6) . . yes Ru H 1.61(5) . . no Cl1 C20 1.758(3) . . yes Cl2 C20 1.753(3) . . yes Cl3 C20 1.747(4) . . yes Cl4 C30 1.766(3) . . yes Cl5 C30 1.738(3) . . yes Cl6 C30 1.756(3) . . yes P1 C31 1.826(3) . . yes P1 C7 1.841(3) . . yes P1 C21 1.833(3) . . yes P2 C51A 1.891(8) . . yes P2 C41 1.832(3) . . yes P2 C8 1.874(3) . . yes P2 C51 1.825(6) . . yes P3 C71 1.815(4) . . yes P3 C61 1.838(3) . . yes P3 C9 1.858(3) . . yes P3 C71A 1.918(5) . . yes P4 C10 1.840(3) . . yes P4 C91 1.830(3) . . yes P4 C81 1.842(3) . . yes O1 C1 1.265(3) . . yes O2 C3 1.264(3) . . yes O3 C1 1.266(3) . 2_667 yes O4 C3 1.267(3) . 2_667 yes N11 C16 1.340(3) . . yes N11 C12 1.338(3) . . yes C1 C2 1.507(4) . . no C3 C4 1.497(4) . . no C5 C14 1.424(3) . . no C5 C6 1.197(3) . . no C7 C8 1.518(4) . . no C9 C10 1.522(4) . . no C12 C13 1.373(3) . . no C13 C14 1.397(4) . . no C14 C15 1.396(4) . . no C15 C16 1.378(3) . . no C21 C26 1.395(4) . . no C21 C22 1.392(4) . . no C22 C23 1.386(5) . . no C23 C24 1.373(4) . . no C24 C25 1.386(4) . . no C25 C26 1.384(4) . . no C31 C32 1.389(4) . . no C31 C36 1.394(3) . . no C32 C33 1.389(4) . . no C33 C34 1.378(4) . . no C34 C35 1.388(4) . . no C35 C36 1.384(4) . . no C41 C42 1.405(4) . . no C41 C46 1.379(5) . . no C42 C43 1.376(5) . . no C43 C44 1.355(6) . . no C44 C45 1.386(7) . . no C45 C46 1.422(7) . . no C51 C52 1.400(9) . . no C51 C56 1.376(6) . . no C51A C56A 1.391(9) . . no C51A C52A 1.390(15) . . no C52 C53 1.383(8) . . no C52A C53A 1.390(14) . . no C53 C54 1.369(9) . . no C53A C54A 1.390(12) . . no C54 C55 1.383(8) . . no C54A C55A 1.391(12) . . no C55 C56 1.383(6) . . no C55A C56A 1.390(10) . . no C61 C62 1.381(4) . . no C61 C66 1.378(5) . . no C62 C63 1.385(4) . . no C63 C64 1.357(5) . . no C64 C65 1.371(5) . . no C65 C66 1.387(5) . . no C71 C76 1.394(7) . . no C71 C72 1.385(6) . . no C71A C76A 1.391(8) . . no C71A C72A 1.391(9) . . no C72 C73 1.397(5) . . no C72A C73A 1.389(8) . . no C73 C74 1.370(6) . . no C73A C74A 1.391(9) . . no C74 C75 1.380(7) . . no C74A C75A 1.391(9) . . no C75 C76 1.386(5) . . no C75A C76A 1.389(9) . . no C81 C86 1.388(3) . . no C81 C82 1.392(4) . . no C82 C83 1.392(4) . . no C83 C84 1.376(4) . . no C84 C85 1.371(5) . . no C85 C86 1.389(4) . . no C91 C96 1.393(4) . . no C91 C92 1.390(4) . . no C92 C93 1.393(5) . . no C93 C94 1.375(5) . . no C94 C95 1.381(4) . . no C95 C96 1.382(5) . . no C2 H22 0.9795 . . no C2 H21 0.9801 . . no C2 H23 0.9807 . . no C4 H43 0.9802 . . no C4 H41 0.9796 . . no C4 H42 0.9806 . . no C7 H72 0.9901 . . no C7 H71 0.9892 . . no C8 H81 0.9897 . . no C8 H82 0.9900 . . no C9 H91 0.9899 . . no C9 H92 0.9895 . . no C10 H101 0.9898 . . no C10 H102 0.9900 . . no C12 H121 0.9502 . . no C13 H131 0.9491 . . no C15 H151 0.9503 . . no C16 H161 0.9499 . . no C22 H221 0.9508 . . no C23 H231 0.9496 . . no C24 H241 0.9507 . . no C25 H251 0.9501 . . no C26 H261 0.9505 . . no C32 H321 0.9509 . . no C33 H331 0.9496 . . no C34 H341 0.9503 . . no C35 H351 0.9503 . . no C36 H361 0.9511 . . no C42 H421 0.9491 . . no C43 H431 0.9503 . . no C44 H441 0.9501 . . no C45 H451 0.9503 . . no C46 H461 0.9505 . . no C52 H521 0.9496 . . no C52A H52A 0.9501 . . no C53 H531 0.9514 . . no C53A H53A 0.9502 . . no C54 H541 0.9510 . . no C54A H54A 0.9490 . . no C55 H551 0.9495 . . no C55A H55A 0.9501 . . no C56 H561 0.9496 . . no C56A H56A 0.9502 . . no C62 H621 0.9497 . . no C63 H631 0.9499 . . no C64 H641 0.9505 . . no C65 H651 0.9492 . . no C66 H661 0.9498 . . no C72 H721 0.9502 . . no C72A H72A 0.9506 . . no C73 H731 0.9492 . . no C73A H73A 0.9494 . . no C74 H741 0.9499 . . no C74A H74A 0.9492 . . no C75 H751 0.9499 . . no C75A H75A 0.9506 . . no C76 H761 0.9505 . . no C76A H76A 0.9506 . . no C82 H821 0.9497 . . no C83 H831 0.9516 . . no C84 H841 0.9494 . . no C85 H851 0.9500 . . no C86 H861 0.9488 . . no C92 H921 0.9507 . . no C93 H931 0.9493 . . no C94 H941 0.9499 . . no C95 H951 0.9498 . . no C96 H961 0.9502 . . no C20 H201 1.0009 . . no C30 H301 1.0000 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Rh O2 89.00(7) . . . yes O1 Rh O3 175.99(6) . . . yes O1 Rh O4 90.94(7) . . . yes O1 Rh N11 92.36(7) . . . yes Rh Rh O1 87.67(4) 2_667 . . yes O2 Rh O3 90.40(7) . . . yes O2 Rh O4 175.90(6) . . . yes O2 Rh N11 93.42(7) . . . yes Rh Rh O2 87.97(4) 2_667 . . yes O3 Rh O4 89.38(7) . . . yes O3 Rh N11 91.63(7) . . . yes Rh Rh O3 88.35(4) 2_667 . . yes O4 Rh N11 90.68(7) . . . yes Rh Rh O4 87.93(4) 2_667 . . yes Rh Rh N11 178.61(6) 2_667 . . yes P1 Ru P2 81.59(2) . . . yes P1 Ru P3 176.21(2) . . . yes P1 Ru P4 97.36(2) . . . yes P1 Ru C6 96.32(7) . . . yes Cl Ru P1 84.06(17) . . . yes P2 Ru P3 97.28(2) . . . yes P2 Ru P4 175.64(2) . . . yes P2 Ru C6 100.10(7) . . . yes Cl Ru P2 75.70(18) . . . yes P3 Ru P4 83.50(2) . . . yes P3 Ru C6 87.43(7) . . . yes Cl Ru P3 92.15(17) . . . yes P4 Ru C6 84.21(7) . . . yes Cl Ru P4 100.01(18) . . . yes Cl Ru C6 175.7(2) . . . yes P2 Ru H 80.6(14) . . . no P3 Ru H 91.0(14) . . . no P1 Ru H 85.3(14) . . . no C6 Ru H 178.3(15) . . . no P4 Ru H 95.1(15) . . . no Ru P1 C21 123.86(9) . . . yes Ru P1 C7 106.61(9) . . . yes C7 P1 C21 99.13(11) . . . yes C7 P1 C31 104.93(12) . . . yes Ru P1 C31 116.77(8) . . . yes C21 P1 C31 102.81(12) . . . yes Ru P2 C41 118.04(10) . . . yes Ru P2 C51 123.42(18) . . . yes Ru P2 C8 109.62(9) . . . yes C41 P2 C51A 97.9(3) . . . yes C41 P2 C51 102.7(2) . . . yes C8 P2 C51A 101.9(3) . . . yes Ru P2 C51A 123.9(2) . . . yes C8 P2 C41 102.52(12) . . . yes C8 P2 C51 96.8(2) . . . yes Ru P3 C71 119.22(16) . . . yes Ru P3 C71A 114.8(2) . . . yes C9 P3 C61 99.72(13) . . . yes Ru P3 C61 122.52(8) . . . yes Ru P3 C9 107.78(9) . . . yes C9 P3 C71A 113.2(2) . . . yes C61 P3 C71 103.75(17) . . . yes C9 P3 C71 99.87(18) . . . yes C61 P3 C71A 97.9(2) . . . yes Ru P4 C81 122.04(9) . . . yes Ru P4 C91 121.37(9) . . . yes Ru P4 C10 105.93(9) . . . yes C10 P4 C81 98.83(12) . . . yes C10 P4 C91 102.90(12) . . . yes C81 P4 C91 102.00(12) . . . yes Rh O1 C1 119.14(16) . . . yes Rh O2 C3 119.01(16) . . . yes Rh O3 C1 118.56(16) . . 2_667 yes Rh O4 C3 119.29(16) . . 2_667 yes Rh N11 C12 122.40(17) . . . yes C12 N11 C16 116.9(2) . . . yes Rh N11 C16 120.68(16) . . . yes O1 C1 C2 116.9(2) . . . yes O3 C1 C2 116.8(2) 2_667 . . yes O1 C1 O3 126.3(2) . . 2_667 yes O2 C3 O4 125.8(2) . . 2_667 yes O2 C3 C4 117.1(2) . . . yes O4 C3 C4 117.1(2) 2_667 . . yes C6 C5 C14 172.8(3) . . . no Ru C6 C5 177.0(2) . . . yes P1 C7 C8 110.45(17) . . . yes P2 C8 C7 112.80(19) . . . yes P3 C9 C10 109.7(2) . . . yes P4 C10 C9 106.51(18) . . . yes N11 C12 C13 123.4(2) . . . yes C12 C13 C14 120.2(2) . . . no C5 C14 C15 122.9(2) . . . no C13 C14 C15 116.1(2) . . . no C5 C14 C13 121.0(2) . . . no C14 C15 C16 120.1(2) . . . no N11 C16 C15 123.2(2) . . . yes P1 C21 C26 117.8(2) . . . yes P1 C21 C22 123.3(2) . . . yes C22 C21 C26 118.8(2) . . . no C21 C22 C23 119.9(3) . . . no C22 C23 C24 120.9(3) . . . no C23 C24 C25 119.9(3) . . . no C24 C25 C26 119.7(3) . . . no C21 C26 C25 120.8(3) . . . no P1 C31 C36 117.8(2) . . . yes P1 C31 C32 123.37(19) . . . yes C32 C31 C36 118.8(2) . . . no C31 C32 C33 120.3(2) . . . no C32 C33 C34 120.6(3) . . . no C33 C34 C35 119.5(3) . . . no C34 C35 C36 120.1(2) . . . no C31 C36 C35 120.7(2) . . . no P2 C41 C42 119.7(2) . . . yes C42 C41 C46 119.0(3) . . . no P2 C41 C46 121.2(3) . . . yes C41 C42 C43 121.6(3) . . . no C42 C43 C44 119.1(3) . . . no C43 C44 C45 121.9(4) . . . no C44 C45 C46 119.1(5) . . . no C41 C46 C45 119.3(4) . . . no P2 C51 C56 120.9(4) . . . yes C52 C51 C56 118.0(5) . . . no P2 C51 C52 121.0(4) . . . yes P2 C51A C56A 116.9(7) . . . yes P2 C51A C52A 122.6(5) . . . yes C52A C51A C56A 120.0(7) . . . no C51 C52 C53 120.8(5) . . . no C51A C52A C53A 120.0(8) . . . no C52 C53 C54 120.3(5) . . . no C52A C53A C54A 120.0(9) . . . no C53 C54 C55 119.5(5) . . . no C53A C54A C55A 120.0(8) . . . no C54 C55 C56 120.2(4) . . . no C54A C55A C56A 120.0(6) . . . no C51 C56 C55 121.2(4) . . . no C51A C56A C55A 120.0(8) . . . no P3 C61 C66 123.7(2) . . . yes P3 C61 C62 118.8(2) . . . yes C62 C61 C66 117.5(3) . . . no C61 C62 C63 121.3(3) . . . no C62 C63 C64 120.3(3) . . . no C63 C64 C65 119.5(3) . . . no C64 C65 C66 120.3(4) . . . no C61 C66 C65 121.0(3) . . . no C72 C71 C76 118.2(4) . . . no P3 C71 C76 123.9(4) . . . yes P3 C71 C72 117.9(3) . . . yes P3 C71A C76A 118.0(4) . . . yes C72A C71A C76A 120.0(5) . . . no P3 C71A C72A 121.6(3) . . . yes C71 C72 C73 121.0(4) . . . no C71A C72A C73A 120.0(5) . . . no C72 C73 C74 119.9(4) . . . no C72A C73A C74A 120.0(5) . . . no C73 C74 C75 119.8(3) . . . no C73A C74A C75A 120.0(5) . . . no C74 C75 C76 120.5(4) . . . no C74A C75A C76A 120.0(5) . . . no C71 C76 C75 120.6(4) . . . no C71A C76A C75A 120.0(6) . . . no P4 C81 C82 120.89(19) . . . yes P4 C81 C86 120.6(2) . . . yes C82 C81 C86 118.3(2) . . . no C81 C82 C83 120.4(3) . . . no C82 C83 C84 120.2(3) . . . no C83 C84 C85 119.9(3) . . . no C84 C85 C86 120.2(3) . . . no C81 C86 C85 120.8(3) . . . no P4 C91 C92 120.7(2) . . . yes P4 C91 C96 121.0(2) . . . yes C92 C91 C96 118.2(2) . . . no C91 C92 C93 120.5(3) . . . no C92 C93 C94 120.3(3) . . . no C93 C94 C95 119.7(3) . . . no C94 C95 C96 120.1(3) . . . no C91 C96 C95 121.0(3) . . . no C1 C2 H21 109.51 . . . no C1 C2 H22 109.48 . . . no C1 C2 H23 109.47 . . . no H21 C2 H22 109.42 . . . no H21 C2 H23 109.42 . . . no H22 C2 H23 109.53 . . . no C3 C4 H41 109.48 . . . no C3 C4 H42 109.51 . . . no C3 C4 H43 109.44 . . . no H41 C4 H42 109.44 . . . no H41 C4 H43 109.48 . . . no H42 C4 H43 109.48 . . . no P1 C7 H71 109.55 . . . no P1 C7 H72 109.60 . . . no C8 C7 H71 109.58 . . . no C8 C7 H72 109.51 . . . no H71 C7 H72 108.12 . . . no P2 C8 H81 109.01 . . . no P2 C8 H82 109.04 . . . no C7 C8 H81 109.03 . . . no C7 C8 H82 109.03 . . . no H81 C8 H82 107.80 . . . no P3 C9 H91 109.66 . . . no P3 C9 H92 109.64 . . . no C10 C9 H91 109.75 . . . no C10 C9 H92 109.77 . . . no H91 C9 H92 108.28 . . . no P4 C10 H101 110.40 . . . no P4 C10 H102 110.43 . . . no C9 C10 H101 110.47 . . . no C9 C10 H102 110.39 . . . no H101 C10 H102 108.63 . . . no N11 C12 H121 118.29 . . . no C13 C12 H121 118.26 . . . no C12 C13 H131 119.89 . . . no C14 C13 H131 119.91 . . . no C14 C15 H151 119.99 . . . no C16 C15 H151 119.92 . . . no N11 C16 H161 118.41 . . . no C15 C16 H161 118.34 . . . no C21 C22 H221 120.03 . . . no C23 C22 H221 120.03 . . . no C22 C23 H231 119.50 . . . no C24 C23 H231 119.62 . . . no C23 C24 H241 120.02 . . . no C25 C24 H241 120.12 . . . no C24 C25 H251 120.19 . . . no C26 C25 H251 120.12 . . . no C21 C26 H261 119.55 . . . no C25 C26 H261 119.62 . . . no C31 C32 H321 119.91 . . . no C33 C32 H321 119.82 . . . no C32 C33 H331 119.68 . . . no C34 C33 H331 119.68 . . . no C33 C34 H341 120.27 . . . no C35 C34 H341 120.24 . . . no C34 C35 H351 119.90 . . . no C36 C35 H351 119.98 . . . no C31 C36 H361 119.70 . . . no C35 C36 H361 119.60 . . . no C41 C42 H421 119.26 . . . no C43 C42 H421 119.13 . . . no C42 C43 H431 120.51 . . . no C44 C43 H431 120.42 . . . no C43 C44 H441 119.02 . . . no C45 C44 H441 119.06 . . . no C44 C45 H451 120.40 . . . no C46 C45 H451 120.52 . . . no C41 C46 H461 120.33 . . . no C45 C46 H461 120.35 . . . no C51 C52 H521 119.57 . . . no C53 C52 H521 119.68 . . . no C53A C52A H52A 120.01 . . . no C51A C52A H52A 120.00 . . . no C54 C53 H531 119.87 . . . no C52 C53 H531 119.78 . . . no C52A C53A H53A 119.95 . . . no C54A C53A H53A 120.01 . . . no C53 C54 H541 120.27 . . . no C55 C54 H541 120.21 . . . no C53A C54A H54A 120.06 . . . no C55A C54A H54A 119.96 . . . no C54 C55 H551 119.87 . . . no C56 C55 H551 119.90 . . . no C54A C55A H55A 120.00 . . . no C56A C55A H55A 120.01 . . . no C51 C56 H561 119.47 . . . no C55 C56 H561 119.38 . . . no C51A C56A H56A 120.05 . . . no C55A C56A H56A 119.95 . . . no C61 C62 H621 119.36 . . . no C63 C62 H621 119.35 . . . no C64 C63 H631 119.81 . . . no C62 C63 H631 119.88 . . . no C65 C64 H641 120.31 . . . no C63 C64 H641 120.22 . . . no C64 C65 H651 119.88 . . . no C66 C65 H651 119.86 . . . no C61 C66 H661 119.51 . . . no C65 C66 H661 119.47 . . . no C73 C72 H721 119.42 . . . no C71 C72 H721 119.57 . . . no C73A C72A H72A 120.02 . . . no C71A C72A H72A 119.96 . . . no C72 C73 H731 120.10 . . . no C74 C73 H731 119.96 . . . no C74A C73A H73A 119.94 . . . no C72A C73A H73A 120.03 . . . no C75 C74 H741 120.06 . . . no C73 C74 H741 120.16 . . . no C73A C74A H74A 120.05 . . . no C75A C74A H74A 120.00 . . . no C74 C75 H751 119.75 . . . no C76 C75 H751 119.78 . . . no C76A C75A H75A 120.02 . . . no C74A C75A H75A 119.96 . . . no C75 C76 H761 119.73 . . . no C71 C76 H761 119.70 . . . no C75A C76A H76A 120.05 . . . no C71A C76A H76A 119.92 . . . no C83 C82 H821 119.76 . . . no C81 C82 H821 119.79 . . . no C82 C83 H831 119.85 . . . no C84 C83 H831 119.93 . . . no C83 C84 H841 120.01 . . . no C85 C84 H841 120.05 . . . no C86 C85 H851 119.86 . . . no C84 C85 H851 119.94 . . . no C81 C86 H861 119.58 . . . no C85 C86 H861 119.58 . . . no C93 C92 H921 119.76 . . . no C91 C92 H921 119.71 . . . no C92 C93 H931 119.86 . . . no C94 C93 H931 119.81 . . . no C93 C94 H941 120.14 . . . no C95 C94 H941 120.14 . . . no C96 C95 H951 119.93 . . . no C94 C95 H951 119.95 . . . no C95 C96 H961 119.51 . . . no C91 C96 H961 119.46 . . . no Cl1 C20 Cl2 110.59(16) . . . yes Cl1 C20 Cl3 109.9(2) . . . yes Cl2 C20 Cl3 110.8(2) . . . yes Cl1 C20 H201 108.48 . . . no Cl2 C20 H201 108.48 . . . no Cl3 C20 H201 108.47 . . . no Cl4 C30 Cl5 111.89(19) . . . yes Cl4 C30 Cl6 111.0(2) . . . yes Cl5 C30 Cl6 109.22(17) . . . yes Cl4 C30 H301 108.17 . . . no Cl5 C30 H301 108.19 . . . no Cl6 C30 H301 108.25 . . . no # End of Crystallographic Information File