Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #=================================================================== _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Zuo, J.-L.' ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen ; 'Herdtweck, E.' ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen ; 'Kuhn, F. E.' ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen ; # 0. AUDIT DETAILS _audit_creation_date 16-Jul-01 _audit_creation_method 'PLATON option' _audit_update_record ; 5-Oct-01 Updated by the Author E.H. Textwriting by E.H. Checkcif OK 9-Oct-01 Updated by the Author E.H. ; #=================================================================== # 1. SUBMISSION DETAILS #=================================================================== # Name and address of author for X-ray correspondence _publ_contact_author_name 'Dr Fritz E Kuhn' _publ_contact_author_address ; Anorganisch-Chemisches Institut der Technischen Universitat Muchen Lichtenbergstrasse 4 Garching bei Muchen D-85747 GERMANY ; _publ_contact_author_email 'FRITZ.KUEHN@CH.TUM.DE' _publ_contact_author_fax ' +49(0)89 289 13473' _publ_contact_author_phone '+49(0)89 289 13143' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Diruthenium o-alkynyl complexes as potential building blocks for heterometallic molecular rods ; # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission october 2001 ; #=================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) #=================================================================== _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=================================================================== # 3. TITLE AND AUTHOR LIST #=================================================================== _publ_section_title ; Diruthenium \s-alkynyl complexes as potential building blocks for heterometallic molecular rods ; # 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_synopsis ? _publ_section_abstract ; Diruthenium(III) bis (\s-pyridylacetylide) complexes are introduced as straightforward building blocks for heterobimetallic units which can be utilized for the construction of molecular rods incorporating axially connected metal-metal units as well as monometallic organometallic units, they are stable to air, moisture and a broad variety of organic solvents and show electron delocalisation along the propagation axis. ; # Insert blank lines between paragraphs _publ_section_comment ? _publ_section_experimental ? # 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. (2000). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ? _publ_section_acknowledgements ? _publ_section_table_legends ? #=================================================================== data_ZUOI-4150-123 _database_code_CSD 173272 #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; Dichlorobis(triphenylphosphine oxide)zinc(II) ; _chemical_name_common ? _chemical_formula_moiety 'C116 H116 N14 O6 Re2 Ru2, C4 H10 O, 2(C F3 O3 S)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C122 H126 F6 N14 O13 Re2 Ru2 S2' _chemical_formula_weight 2749.08 _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 S S 0.1246 0.1234 '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' Re Re -1.0185 7.2310 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 48.4644(4) _cell_length_b 11.4260(1) _cell_length_c 23.0519(2) _cell_angle_alpha 90 _cell_angle_beta 108.2667(7) _cell_angle_gamma 90 _cell_volume 12121.83(19) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 10207 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 25.38 _exptl_crystal_description 'plate' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method none _exptl_crystal_F_000 5536 _exptl_absorpt_coefficient_mu 2.344 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.470 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2000b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 60 s per film repetition 1 dx 50 507 films measured in 2 data sets set 1: phi-scan with delta_phi = 1.0 set 2 to set 2 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: Nonius (2000b). ; #=================================================================== # 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 ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 49714 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -58 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.38 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measured_fraction_theta_full 0.957 # number of observed reflections (> n sig(I)) # number of unique reflections _reflns_number_total 10698 _reflns_number_gt 8503 _reflns_threshold_expression 'I>2\s(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, 2000)' _computing_publication_material 'PLATON (Spek, 2000)' #=================================================================== # 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^)+(0.0202P)^2^+30.5914P] 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 mixed # see text _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ' ? ' _refine_ls_number_reflns 10698 _refine_ls_number_parameters 731 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.802 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.087 #=================================================================== # 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 _atom_site_calc_flag _atom_site_refinement_flags Re Re Uani 0.22816(1) -0.00308(1) 0.31269(1) 1.000 0.0168(1) . . Ru Ru Uani 0.02765(1) -0.13072(3) 0.27546(1) 1.000 0.0197(1) . . O1 O Uani 0.29209(5) 0.0387(2) 0.32389(11) 1.000 0.0256(8) . . O2 O Uani 0.23612(5) -0.2489(2) 0.26673(12) 1.000 0.0309(9) . . O3 O Uani 0.24794(6) -0.0870(2) 0.44608(12) 1.000 0.0341(9) . . N1 N Uani 0.02564(6) -0.2705(3) 0.32676(13) 1.000 0.0220(9) . . N2 N Uani 0.02488(6) -0.2430(2) 0.20201(13) 1.000 0.0223(10) . . N3 N Uani 0.02330(6) 0.0112(2) 0.21600(13) 1.000 0.0209(9) . . N4 N Uani 0.02496(6) -0.0238(2) 0.34195(13) 1.000 0.0229(10) . . N11 N Uani 0.21962(6) 0.1777(2) 0.32880(12) 1.000 0.0168(9) . . N21 N Uani 0.21119(6) 0.0740(2) 0.22330(13) 1.000 0.0179(9) . . N31 N Uani 0.18209(6) -0.0325(2) 0.30459(13) 1.000 0.0177(9) . . C1 C Uani 0.26801(8) 0.0253(3) 0.31915(16) 1.000 0.0196(11) . . C2 C Uani 0.23286(7) -0.1579(3) 0.28547(16) 1.000 0.0218(11) . . C3 C Uani 0.24069(7) -0.0568(3) 0.39613(19) 1.000 0.0234(13) . . C4 C Uani -0.00067(8) -0.2936(3) 0.33081(16) 1.000 0.0246(12) . . C5 C Uani 0.00036(8) 0.0301(3) 0.16818(17) 1.000 0.0251(12) . . C12 C Uani 0.22626(7) 0.2281(3) 0.38391(16) 1.000 0.0219(11) . . C13 C Uani 0.21976(8) 0.3429(3) 0.39214(16) 1.000 0.0246(12) . . C14 C Uani 0.20500(7) 0.4111(3) 0.34218(16) 1.000 0.0205(11) . . C15 C Uani 0.19892(7) 0.3596(3) 0.28539(15) 1.000 0.0192(11) . . C16 C Uani 0.20656(7) 0.2446(3) 0.27921(15) 1.000 0.0172(11) . . C17 C Uani 0.19546(8) 0.5349(3) 0.35193(17) 1.000 0.0259(11) . . C18 C Uani 0.17966(9) 0.5962(3) 0.29207(17) 1.000 0.0327(12) . . C19 C Uani 0.22199(9) 0.6069(3) 0.38733(18) 1.000 0.0388(16) . . C20 C Uani 0.17419(10) 0.5254(3) 0.3894(2) 1.000 0.0427(17) . . C22 C Uani 0.20879(8) 0.0171(3) 0.17087(16) 1.000 0.0241(12) . . C23 C Uani 0.19754(8) 0.0671(3) 0.11502(17) 1.000 0.0292(12) . . C24 C Uani 0.18780(8) 0.1816(3) 0.10963(16) 1.000 0.0279(12) . . C25 C Uani 0.18983(7) 0.2404(3) 0.16375(16) 1.000 0.0241(11) . . C26 C Uani 0.20175(7) 0.1853(3) 0.21993(15) 1.000 0.0183(11) . . C27 C Uani 0.17509(9) 0.2361(3) 0.04631(17) 1.000 0.0337(14) . . C28 C Uani 0.17285(8) 0.3691(3) 0.04959(16) 1.000 0.0306(12) . . C29 C Uani 0.19515(10) 0.2056(4) 0.00714(19) 1.000 0.0485(17) . . C30 C Uani 0.14602(9) 0.1823(4) 0.0156(2) 1.000 0.0506(16) . . C32 C Uani 0.17162(8) -0.0051(3) 0.35044(17) 1.000 0.0261(11) . . C33 C Uani 0.14380(8) -0.0289(3) 0.34942(18) 1.000 0.0273(12) . . C34 C Uani 0.12430(7) -0.0840(3) 0.29870(17) 1.000 0.0230(11) . . C35 C Uani 0.13535(7) -0.1114(3) 0.25128(16) 1.000 0.0238(11) . . C36 C Uani 0.16329(7) -0.0848(3) 0.25550(16) 1.000 0.0220(11) . . C37 C Uani 0.09492(8) -0.1078(3) 0.29428(16) 1.000 0.0256(12) . . C38 C Uani 0.06939(8) -0.1219(3) 0.28649(16) 1.000 0.0245(12) . . C41 C Uani 0.04698(7) -0.3565(3) 0.35382(16) 1.000 0.0220(11) . . C42 C Uani 0.07485(8) -0.3247(3) 0.38872(17) 1.000 0.0311(12) . . C43 C Uani 0.09487(8) -0.4107(4) 0.41514(19) 1.000 0.0400(16) . . C44 C Uani 0.08808(8) -0.5285(3) 0.40885(19) 1.000 0.0333(16) . . C45 C Uani 0.06025(8) -0.5586(4) 0.37412(18) 1.000 0.0341(14) . . C46 C Uani 0.03995(8) -0.4746(3) 0.34622(18) 1.000 0.0301(12) . . C47 C Uani 0.11020(9) -0.6209(4) 0.4386(2) 1.000 0.0489(16) . . C51 C Uani 0.04915(7) -0.2802(3) 0.18256(17) 1.000 0.0250(11) . . C52 C Uani 0.07121(8) -0.3474(3) 0.22038(18) 1.000 0.0318(12) . . C53 C Uani 0.09313(9) -0.3882(4) 0.1996(2) 1.000 0.0416(16) . . C54 C Uani 0.09394(9) -0.3628(4) 0.1416(2) 1.000 0.0433(16) . . C55 C Uani 0.07216(9) -0.2948(4) 0.1051(2) 1.000 0.0440(17) . . C56 C Uani 0.04971(8) -0.2523(3) 0.12510(18) 1.000 0.0321(14) . . C57 C Uani 0.11812(11) -0.4093(5) 0.1193(3) 1.000 0.074(2) . . C61 C Uani 0.04751(7) 0.0872(3) 0.21953(16) 1.000 0.0231(11) . . C62 C Uani 0.05372(9) 0.1793(3) 0.25936(19) 1.000 0.0369(14) . . C63 C Uani 0.07831(9) 0.2470(4) 0.2659(2) 1.000 0.0461(17) . . C64 C Uani 0.09671(9) 0.2244(4) 0.2330(2) 1.000 0.0413(14) . . C65 C Uani 0.08947(9) 0.1351(4) 0.1910(2) 1.000 0.0411(14) . . C66 C Uani 0.06523(9) 0.0666(4) 0.18436(19) 1.000 0.0347(14) . . C67 C Uani 0.12449(10) 0.2920(4) 0.2430(3) 1.000 0.071(2) . . C71 C Uani 0.04612(7) -0.0060(3) 0.40089(16) 1.000 0.0238(11) . . C72 C Uani 0.03976(9) -0.0331(4) 0.45310(19) 1.000 0.0403(16) . . C73 C Uani 0.06033(10) -0.0145(4) 0.50965(19) 1.000 0.0486(18) . . C74 C Uani 0.08728(9) 0.0313(4) 0.51510(18) 1.000 0.0341(14) . . C75 C Uani 0.09337(8) 0.0577(3) 0.46170(18) 1.000 0.0312(14) . . C76 C Uani 0.07303(8) 0.0393(3) 0.40518(18) 1.000 0.0290(12) . . C77 C Uani 0.11004(9) 0.0521(4) 0.57607(19) 1.000 0.0493(17) . . C6A C Uiso 0.0175(4) 0.4281(16) 0.0310(9) 0.500 0.297(8) . . C6B C Uiso 0.0175(4) 0.4281(16) 0.0310(9) 0.500 0.297(8) . . C7 C Uiso 0.0290(4) 0.3863(18) 0.1046(9) 0.500 0.181(8) . . C8 C Uiso 0.0404(5) 0.359(2) 0.0221(10) 0.500 0.208(10) . . O7A O Uiso -0.0025(3) 0.5134(11) 0.0404(6) 0.250 0.138(4) . . O7B O Uiso -0.0025(3) 0.5134(11) 0.0404(6) 0.250 0.138(4) . . S S Uani 0.18311(2) 0.82167(8) -0.00937(4) 1.000 0.0292(3) . . F1 F Uani 0.20581(5) 0.7634(2) 0.10537(9) 1.000 0.0420(8) . . F2 F Uani 0.20936(5) 0.63090(19) 0.04171(10) 1.000 0.0423(8) . . F3 F Uani 0.16851(5) 0.6613(2) 0.05647(11) 1.000 0.0501(9) . . O4 O Uani 0.17086(6) 0.7542(2) -0.06387(11) 1.000 0.0357(9) . . O5 O Uani 0.16299(6) 0.8961(2) 0.00704(13) 1.000 0.0465(10) . . O6 O Uani 0.21076(6) 0.8751(2) -0.00299(12) 1.000 0.0384(9) . . C C Uani 0.19199(8) 0.7155(3) 0.05073(18) 1.000 0.0316(12) . . H41 H Uiso -0.00200 -0.35100 0.35960 1.000 0.0290 calc R H51 H Uiso 0.00200 0.08600 0.13900 1.000 0.0300 calc R H121 H Uiso 0.23590 0.18260 0.41890 1.000 0.0260 calc R H131 H Uiso 0.22540 0.37560 0.43200 1.000 0.0300 calc R H151 H Uiso 0.18930 0.40380 0.24990 1.000 0.0230 calc R H181 H Uiso 0.16270 0.54970 0.26940 1.000 0.0390 calc R H182 H Uiso 0.19280 0.60460 0.26760 1.000 0.0390 calc R H183 H Uiso 0.17330 0.67380 0.30070 1.000 0.0390 calc R H191 H Uiso 0.21580 0.68610 0.39390 1.000 0.0470 calc R H192 H Uiso 0.23570 0.61090 0.36390 1.000 0.0470 calc R H193 H Uiso 0.23140 0.56970 0.42690 1.000 0.0470 calc R H201 H Uiso 0.15820 0.47280 0.36860 1.000 0.0510 calc R H202 H Uiso 0.16640 0.60310 0.39340 1.000 0.0510 calc R H203 H Uiso 0.18450 0.49430 0.43010 1.000 0.0510 calc R H221 H Uiso 0.21530 -0.06170 0.17300 1.000 0.0290 calc R H231 H Uiso 0.19630 0.02310 0.07930 1.000 0.0350 calc R H251 H Uiso 0.18300 0.31860 0.16230 1.000 0.0290 calc R H281 H Uiso 0.19220 0.40200 0.06960 1.000 0.0370 calc R H282 H Uiso 0.15980 0.38960 0.07310 1.000 0.0370 calc R H283 H Uiso 0.16510 0.40100 0.00820 1.000 0.0370 calc R H291 H Uiso 0.21480 0.23520 0.02750 1.000 0.0590 calc R H292 H Uiso 0.18740 0.24180 -0.03330 1.000 0.0590 calc R H293 H Uiso 0.19590 0.12040 0.00260 1.000 0.0590 calc R H301 H Uiso 0.13890 0.20820 -0.02710 1.000 0.0610 calc R H302 H Uiso 0.13230 0.20660 0.03670 1.000 0.0610 calc R H303 H Uiso 0.14780 0.09680 0.01690 1.000 0.0610 calc R H321 H Uiso 0.18420 0.03270 0.38540 1.000 0.0310 calc R H331 H Uiso 0.13770 -0.00800 0.38330 1.000 0.0320 calc R H351 H Uiso 0.12320 -0.14900 0.21560 1.000 0.0280 calc R H361 H Uiso 0.16990 -0.10420 0.22200 1.000 0.0270 calc R H421 H Uiso 0.08010 -0.24450 0.39440 1.000 0.0370 calc R H431 H Uiso 0.11400 -0.38810 0.43850 1.000 0.0480 calc R H451 H Uiso 0.05490 -0.63890 0.36930 1.000 0.0410 calc R H461 H Uiso 0.02110 -0.49760 0.32170 1.000 0.0360 calc R H471 H Uiso 0.12730 -0.58370 0.46730 1.000 0.0590 calc R H472 H Uiso 0.11600 -0.66270 0.40720 1.000 0.0590 calc R H473 H Uiso 0.10170 -0.67630 0.46060 1.000 0.0590 calc R H521 H Uiso 0.07120 -0.36560 0.26060 1.000 0.0380 calc R H531 H Uiso 0.10810 -0.43490 0.22580 1.000 0.0500 calc R H551 H Uiso 0.07230 -0.27600 0.06510 1.000 0.0530 calc R H561 H Uiso 0.03490 -0.20440 0.09910 1.000 0.0390 calc R H571 H Uiso 0.12090 -0.49290 0.12880 1.000 0.0900 calc R H572 H Uiso 0.13620 -0.36700 0.13960 1.000 0.0900 calc R H573 H Uiso 0.11290 -0.39800 0.07500 1.000 0.0900 calc R H621 H Uiso 0.04120 0.19700 0.28260 1.000 0.0440 calc R H631 H Uiso 0.08240 0.31050 0.29400 1.000 0.0550 calc R H651 H Uiso 0.10140 0.12020 0.16600 1.000 0.0490 calc R H661 H Uiso 0.06080 0.00480 0.15530 1.000 0.0410 calc R H671 H Uiso 0.12470 0.32690 0.20430 1.000 0.0850 calc R H672 H Uiso 0.14110 0.23900 0.25810 1.000 0.0850 calc R H673 H Uiso 0.12570 0.35400 0.27310 1.000 0.0850 calc R H721 H Uiso 0.02130 -0.06470 0.45060 1.000 0.0480 calc R H731 H Uiso 0.05570 -0.03390 0.54560 1.000 0.0580 calc R H751 H Uiso 0.11180 0.08900 0.46400 1.000 0.0370 calc R H761 H Uiso 0.07760 0.05790 0.36910 1.000 0.0350 calc R H771 H Uiso 0.12350 0.11310 0.57180 1.000 0.0590 calc R H772 H Uiso 0.12080 -0.02050 0.59010 1.000 0.0590 calc R H773 H Uiso 0.10060 0.07710 0.60590 1.000 0.0590 calc R H62A H Uiso 0.00780 0.36450 0.00290 0.500 0.4450 calc R H61A H Uiso 0.03310 0.46340 0.01740 0.500 0.4450 calc R H61B H Uiso 0.01580 0.37760 0.06450 0.500 0.4450 calc R H72 H Uiso 0.01460 0.33410 0.11260 0.500 0.2720 calc R H73 H Uiso 0.03160 0.45540 0.13090 0.500 0.2720 calc R H81 H Uiso 0.05470 0.34160 0.06180 0.500 0.3120 calc R H82 H Uiso 0.04990 0.40270 -0.00310 0.500 0.3120 calc R H83 H Uiso 0.03250 0.28590 0.00150 0.500 0.3120 calc R H62B H Uiso 0.00290 0.39490 -0.00550 0.500 0.4450 calc R H71 H Uiso 0.04760 0.34490 0.11310 0.500 0.2720 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 Re 0.0144(1) 0.0168(1) 0.0189(1) 0.0004(1) 0.0048(1) 0.0005(1) Ru 0.0132(1) 0.0236(2) 0.0216(2) -0.0003(1) 0.0044(1) -0.0005(1) O1 0.0172(14) 0.0283(14) 0.0315(16) 0.0001(12) 0.0080(12) -0.0006(11) O2 0.0315(15) 0.0220(15) 0.0418(17) -0.0100(13) 0.0154(13) 0.0014(12) O3 0.0370(16) 0.0393(17) 0.0242(16) 0.0088(13) 0.0071(13) 0.0031(13) N1 0.0136(15) 0.0263(17) 0.0252(17) 0.0007(14) 0.0048(13) 0.0022(13) N2 0.0167(16) 0.0258(17) 0.0256(18) -0.0035(14) 0.0082(14) -0.0028(13) N3 0.0145(15) 0.0241(17) 0.0233(17) 0.0004(14) 0.0048(13) -0.0021(13) N4 0.0193(16) 0.0260(18) 0.0236(17) -0.0004(13) 0.0070(13) -0.0003(13) N11 0.0152(15) 0.0212(16) 0.0154(16) 0.0002(13) 0.0068(12) 0.0005(12) N21 0.0166(15) 0.0174(16) 0.0198(17) -0.0017(13) 0.0058(13) -0.0013(12) N31 0.0141(15) 0.0174(16) 0.0214(17) 0.0005(12) 0.0054(13) 0.0014(12) C1 0.025(2) 0.0150(19) 0.017(2) 0.0006(14) 0.0042(16) 0.0036(15) C2 0.0114(17) 0.034(2) 0.020(2) 0.0020(17) 0.0051(15) -0.0037(16) C3 0.0155(19) 0.0195(19) 0.036(3) -0.0025(18) 0.0092(18) 0.0000(15) C4 0.023(2) 0.027(2) 0.025(2) 0.0033(17) 0.0094(17) 0.0006(16) C5 0.023(2) 0.026(2) 0.028(2) 0.0042(16) 0.0103(18) 0.0011(16) C12 0.0236(19) 0.022(2) 0.019(2) 0.0003(16) 0.0052(16) 0.0002(16) C13 0.028(2) 0.027(2) 0.020(2) -0.0048(16) 0.0091(17) -0.0013(17) C14 0.0189(19) 0.0197(19) 0.027(2) 0.0003(16) 0.0133(16) -0.0028(15) C15 0.0195(18) 0.0211(19) 0.019(2) 0.0029(16) 0.0089(15) -0.0002(15) C16 0.0123(17) 0.0192(18) 0.021(2) 0.0005(15) 0.0066(15) -0.0029(14) C17 0.036(2) 0.0200(19) 0.026(2) 0.0003(16) 0.0158(18) 0.0013(16) C18 0.039(2) 0.023(2) 0.038(2) 0.0027(18) 0.015(2) 0.0066(18) C19 0.056(3) 0.022(2) 0.036(3) -0.0034(19) 0.011(2) -0.004(2) C20 0.059(3) 0.033(3) 0.048(3) -0.003(2) 0.034(2) 0.007(2) C22 0.031(2) 0.021(2) 0.019(2) -0.0014(17) 0.0061(17) -0.0012(16) C23 0.041(2) 0.024(2) 0.023(2) -0.0073(17) 0.0105(19) -0.0062(18) C24 0.036(2) 0.031(2) 0.014(2) 0.0028(17) 0.0040(17) -0.0039(18) C25 0.027(2) 0.0179(19) 0.025(2) 0.0015(16) 0.0045(17) -0.0013(16) C26 0.0170(18) 0.0229(19) 0.0161(19) -0.0008(15) 0.0066(15) -0.0047(15) C27 0.047(3) 0.023(2) 0.026(2) 0.0013(18) 0.004(2) -0.0065(19) C28 0.040(2) 0.026(2) 0.021(2) 0.0042(17) 0.0028(18) -0.0019(19) C29 0.073(3) 0.037(3) 0.038(3) 0.010(2) 0.021(3) 0.007(2) C30 0.053(3) 0.029(2) 0.049(3) 0.008(2) -0.014(2) -0.002(2) C32 0.0203(19) 0.034(2) 0.022(2) -0.0040(18) 0.0039(16) -0.0029(18) C33 0.019(2) 0.037(2) 0.029(2) -0.0040(17) 0.0119(17) -0.0009(16) C34 0.0163(19) 0.024(2) 0.028(2) 0.0045(17) 0.0059(17) 0.0027(15) C35 0.0185(19) 0.026(2) 0.023(2) -0.0018(16) 0.0010(16) 0.0002(16) C36 0.0212(19) 0.025(2) 0.020(2) -0.0017(16) 0.0068(16) -0.0002(16) C37 0.020(2) 0.028(2) 0.028(2) -0.0003(17) 0.0064(17) 0.0000(16) C38 0.024(2) 0.024(2) 0.025(2) -0.0001(17) 0.0071(17) 0.0001(17) C41 0.0217(19) 0.025(2) 0.022(2) 0.0016(16) 0.0109(16) 0.0019(16) C42 0.021(2) 0.028(2) 0.039(2) 0.0006(18) 0.0016(18) -0.0029(17) C43 0.020(2) 0.040(3) 0.050(3) 0.008(2) -0.0034(19) 0.0026(19) C44 0.027(2) 0.034(3) 0.038(3) 0.0055(19) 0.0088(19) 0.0081(18) C45 0.033(2) 0.027(2) 0.043(3) -0.001(2) 0.013(2) 0.0000(19) C46 0.022(2) 0.029(2) 0.038(2) -0.0034(18) 0.0075(18) 0.0017(16) C47 0.032(2) 0.041(3) 0.064(3) 0.007(2) 0.001(2) 0.008(2) C51 0.0181(19) 0.030(2) 0.029(2) -0.0069(18) 0.0102(17) -0.0048(16) C52 0.025(2) 0.037(2) 0.036(2) -0.0038(19) 0.0131(19) 0.0008(18) C53 0.028(2) 0.048(3) 0.052(3) -0.004(2) 0.017(2) 0.009(2) C54 0.027(2) 0.058(3) 0.053(3) -0.012(3) 0.024(2) 0.001(2) C55 0.037(3) 0.063(3) 0.041(3) -0.008(2) 0.025(2) -0.008(2) C56 0.025(2) 0.039(2) 0.034(3) 0.000(2) 0.0115(18) -0.0014(18) C57 0.053(3) 0.108(5) 0.078(4) -0.006(4) 0.044(3) 0.023(3) C61 0.0194(19) 0.025(2) 0.024(2) 0.0032(17) 0.0053(17) -0.0009(16) C62 0.037(2) 0.034(2) 0.046(3) -0.008(2) 0.022(2) -0.006(2) C63 0.045(3) 0.037(3) 0.057(3) -0.014(2) 0.017(2) -0.016(2) C64 0.029(2) 0.030(2) 0.065(3) 0.003(2) 0.015(2) -0.0073(19) C65 0.034(2) 0.033(2) 0.068(3) 0.004(2) 0.033(2) -0.002(2) C66 0.039(2) 0.032(2) 0.038(3) -0.002(2) 0.019(2) -0.005(2) C67 0.044(3) 0.057(3) 0.116(5) -0.008(3) 0.032(3) -0.022(3) C71 0.0193(19) 0.027(2) 0.022(2) -0.0039(18) 0.0019(16) 0.0049(17) C72 0.029(2) 0.061(3) 0.030(3) -0.004(2) 0.008(2) -0.007(2) C73 0.041(3) 0.084(4) 0.023(2) -0.003(2) 0.013(2) -0.011(3) C74 0.027(2) 0.046(3) 0.025(2) -0.0042(19) 0.0020(18) 0.0039(19) C75 0.025(2) 0.031(2) 0.035(3) -0.0071(19) 0.0056(19) -0.0013(18) C76 0.026(2) 0.034(2) 0.026(2) -0.0010(18) 0.0069(18) 0.0024(17) C77 0.037(3) 0.076(3) 0.029(3) -0.014(2) 0.002(2) -0.001(2) S 0.0295(5) 0.0262(5) 0.0295(6) -0.0015(4) 0.0057(4) 0.0002(4) F1 0.0528(15) 0.0388(14) 0.0278(13) -0.0014(11) 0.0033(11) -0.0035(12) F2 0.0422(14) 0.0308(13) 0.0457(14) -0.0003(11) 0.0018(11) 0.0085(11) F3 0.0429(15) 0.0604(17) 0.0465(15) 0.0104(13) 0.0133(12) -0.0182(13) O4 0.0396(16) 0.0372(16) 0.0253(15) -0.0042(13) 0.0029(13) -0.0042(13) O5 0.0389(17) 0.0411(18) 0.0495(19) -0.0088(15) -0.0004(14) 0.0175(14) O6 0.0379(16) 0.0391(17) 0.0359(16) 0.0001(14) 0.0081(13) -0.0141(14) C 0.023(2) 0.034(2) 0.033(2) -0.0075(19) 0.0019(18) -0.0066(18) #================================================================== # 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 Re N11 2.162(2) . . yes Re N21 2.153(3) . . yes Re N31 2.207(3) . . yes Re C1 1.917(4) . . yes Re C2 1.914(3) . . yes Re C3 1.927(4) . . yes Ru N1 2.008(3) . . yes Ru N2 2.095(3) . . yes Ru N3 2.091(3) . . yes Ru N4 1.996(3) . . yes Ru C38 1.961(4) . . yes Ru Ru 2.5666(4) . 2_555 yes S O6 1.438(3) . . yes S O4 1.434(3) . . yes S O5 1.431(3) . . yes S C 1.790(4) . . yes F1 C 1.344(4) . . yes F2 C 1.340(4) . . yes F3 C 1.338(5) . . yes O1 C1 1.148(5) . . yes O2 C2 1.156(4) . . yes O3 C3 1.147(5) . . yes O7A C6A 1.44(2) . . yes O7A C6B 1.44(2) . . yes O7B C6A 1.44(2) . . yes O7B C6B 1.44(2) . . yes N1 C41 1.421(5) . . yes N1 C4 1.334(5) . . yes N2 C51 1.448(5) . . yes N2 C4 1.314(5) . 2_555 yes N3 C5 1.315(5) . . yes N3 C61 1.441(5) . . yes N4 C71 1.437(5) . . yes N4 C5 1.327(5) . 2_555 yes N11 C16 1.356(4) . . yes N11 C12 1.339(4) . . yes N21 C26 1.345(4) . . yes N21 C22 1.345(4) . . yes N31 C36 1.350(4) . . yes N31 C32 1.345(5) . . yes C12 C13 1.376(5) . . no C13 C14 1.389(5) . . no C14 C17 1.527(5) . . no C14 C15 1.380(5) . . no C15 C16 1.385(5) . . no C16 C26 1.477(5) . . no C17 C18 1.523(5) . . no C17 C19 1.529(6) . . no C17 C20 1.542(6) . . no C22 C23 1.357(5) . . no C23 C24 1.383(5) . . no C24 C27 1.528(5) . . no C24 C25 1.393(5) . . no C25 C26 1.392(5) . . no C27 C30 1.496(6) . . no C27 C28 1.527(5) . . no C27 C29 1.560(6) . . no C32 C33 1.368(6) . . no C33 C34 1.401(5) . . no C34 C37 1.422(5) . . no C34 C35 1.395(5) . . no C35 C36 1.361(5) . . no C37 C38 1.204(6) . . no C41 C42 1.387(5) . . no C41 C46 1.389(5) . . no C42 C43 1.381(6) . . no C43 C44 1.382(6) . . no C44 C45 1.379(6) . . no C44 C47 1.508(6) . . no C45 C46 1.381(6) . . no C51 C56 1.371(5) . . no C51 C52 1.381(5) . . no C52 C53 1.376(6) . . no C53 C54 1.381(6) . . no C54 C55 1.367(6) . . no C54 C57 1.516(7) . . no C55 C56 1.395(6) . . no C61 C66 1.374(6) . . no C61 C62 1.367(5) . . no C62 C63 1.389(6) . . no C63 C64 1.364(6) . . no C64 C65 1.374(6) . . no C64 C67 1.506(7) . . no C65 C66 1.380(6) . . no C71 C76 1.378(5) . . no C71 C72 1.368(6) . . no C72 C73 1.387(6) . . no C73 C74 1.376(7) . . no C74 C75 1.386(6) . . no C74 C77 1.509(6) . . no C75 C76 1.381(6) . . no C4 H41 0.9495 . . no C5 H51 0.9488 . . no C12 H121 0.9502 . . no C13 H131 0.9493 . . no C15 H151 0.9501 . . no C18 H183 0.9794 . . no C18 H182 0.9788 . . no C18 H181 0.9807 . . no C19 H193 0.9798 . . no C19 H192 0.9799 . . no C19 H191 0.9800 . . no C20 H202 0.9803 . . no C20 H201 0.9791 . . no C20 H203 0.9810 . . no C22 H221 0.9502 . . no C23 H231 0.9504 . . no C25 H251 0.9498 . . no C28 H282 0.9816 . . no C28 H283 0.9796 . . no C28 H281 0.9810 . . no C29 H291 0.9805 . . no C29 H293 0.9810 . . no C29 H292 0.9807 . . no C30 H302 0.9791 . . no C30 H301 0.9811 . . no C30 H303 0.9804 . . no C32 H321 0.9485 . . no C33 H331 0.9482 . . no C35 H351 0.9509 . . no C36 H361 0.9504 . . no C42 H421 0.9491 . . no C43 H431 0.9504 . . no C45 H451 0.9504 . . no C46 H461 0.9484 . . no C47 H471 0.9805 . . no C47 H472 0.9791 . . no C47 H473 0.9791 . . no C52 H521 0.9503 . . no C53 H531 0.9493 . . no C55 H551 0.9489 . . no C56 H561 0.9509 . . no C57 H573 0.9806 . . no C57 H571 0.9798 . . no C57 H572 0.9815 . . no C62 H621 0.9486 . . no C63 H631 0.9512 . . no C65 H651 0.9509 . . no C66 H661 0.9504 . . no C67 H673 0.9804 . . no C67 H671 0.9801 . . no C67 H672 0.9799 . . no C72 H721 0.9496 . . no C73 H731 0.9502 . . no C75 H751 0.9481 . . no C76 H761 0.9494 . . no C77 H773 0.9803 . . no C77 H771 0.9804 . . no C77 H772 0.9792 . . no C6A C8 1.43(3) . . no C6A C7 1.68(3) . . no C6B C7 1.68(3) . . no C6B C8 1.43(3) . . no C6A H61A 0.9905 . . no C6A H62B 0.9896 . . no C6A H61B 0.9879 . . no C6A H62A 0.9888 . . no C6B H62B 0.9896 . . no C6B H61A 0.9905 . . no C6B H61B 0.9879 . . no C6B H62A 0.9888 . . no C7 H61B 0.9502 . . no C7 H71 0.9818 . . no C7 H72 0.9785 . . no C7 H73 0.9792 . . no C8 H61A 1.2393 . . no C8 H81 0.9797 . . no C8 H82 0.9831 . . no C8 H83 0.9776 . . 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 N11 Re N21 74.77(10) . . . yes N11 Re N31 85.23(10) . . . yes N11 Re C1 93.87(13) . . . yes N11 Re C2 171.21(13) . . . yes N11 Re C3 98.64(13) . . . yes N21 Re N31 84.75(11) . . . yes N21 Re C1 94.50(13) . . . yes N21 Re C2 96.51(12) . . . yes N21 Re C3 172.73(13) . . . yes N31 Re C1 178.96(12) . . . yes N31 Re C2 93.02(12) . . . yes N31 Re C3 91.71(13) . . . yes C1 Re C2 87.79(15) . . . yes C1 Re C3 88.96(15) . . . yes C2 Re C3 90.01(15) . . . yes N1 Ru N2 89.21(11) . . . yes N1 Ru N3 171.72(12) . . . yes N1 Ru N4 90.44(11) . . . yes N1 Ru C38 101.71(13) . . . yes Ru Ru N1 91.89(9) 2_555 . . yes N2 Ru N3 88.70(10) . . . yes N2 Ru N4 172.96(12) . . . yes N2 Ru C38 86.47(13) . . . yes Ru Ru N2 80.63(8) 2_555 . . yes N3 Ru N4 90.65(10) . . . yes N3 Ru C38 86.16(13) . . . yes Ru Ru N3 79.86(8) 2_555 . . yes N4 Ru C38 100.48(13) . . . yes Ru Ru N4 92.36(9) 2_555 . . yes Ru Ru C38 161.12(10) 2_555 . . yes O6 S C 102.62(17) . . . yes O4 S C 104.29(16) . . . yes O4 S O5 114.94(18) . . . yes O4 S O6 115.75(17) . . . yes O5 S O6 114.27(16) . . . yes O5 S C 102.51(17) . . . yes Ru N1 C41 130.2(2) . . . yes Ru N1 C4 115.0(2) . . . yes C4 N1 C41 114.4(3) . . . yes Ru N2 C4 123.7(3) . . 2_555 yes Ru N2 C51 125.3(2) . . . yes C4 N2 C51 111.0(3) 2_555 . . yes C5 N3 C61 114.1(3) . . . yes Ru N3 C5 124.2(2) . . . yes Ru N3 C61 121.1(2) . . . yes Ru N4 C5 115.4(2) . . 2_555 yes C5 N4 C71 116.6(3) 2_555 . . yes Ru N4 C71 127.9(2) . . . yes C12 N11 C16 117.9(3) . . . yes Re N11 C12 124.9(2) . . . yes Re N11 C16 117.2(2) . . . yes Re N21 C26 117.6(2) . . . yes Re N21 C22 124.2(2) . . . yes C22 N21 C26 118.2(3) . . . yes Re N31 C36 122.5(2) . . . yes Re N31 C32 121.3(2) . . . yes C32 N31 C36 116.1(3) . . . yes Re C1 O1 177.7(3) . . . yes Re C2 O2 176.6(3) . . . yes Re C3 O3 178.8(3) . . . yes N1 C4 N2 125.0(3) . . 2_555 yes N3 C5 N4 124.3(3) . . 2_555 yes N11 C12 C13 122.9(3) . . . yes C12 C13 C14 120.1(3) . . . no C13 C14 C15 116.7(3) . . . no C13 C14 C17 119.9(3) . . . no C15 C14 C17 123.4(3) . . . no C14 C15 C16 121.2(3) . . . no C15 C16 C26 124.1(3) . . . no N11 C16 C15 121.2(3) . . . yes N11 C16 C26 114.7(3) . . . yes C14 C17 C18 112.5(3) . . . no C18 C17 C19 109.6(3) . . . no C14 C17 C19 109.5(3) . . . no C14 C17 C20 107.7(3) . . . no C18 C17 C20 107.8(3) . . . no C19 C17 C20 109.7(3) . . . no N21 C22 C23 123.0(3) . . . yes C22 C23 C24 120.5(3) . . . no C23 C24 C27 119.7(3) . . . no C25 C24 C27 123.6(3) . . . no C23 C24 C25 116.7(3) . . . no C24 C25 C26 120.5(3) . . . no C16 C26 C25 123.5(3) . . . no N21 C26 C25 121.0(3) . . . yes N21 C26 C16 115.3(3) . . . yes C24 C27 C28 111.8(3) . . . no C28 C27 C29 108.5(3) . . . no C24 C27 C29 108.9(3) . . . no C24 C27 C30 108.8(3) . . . no C28 C27 C30 111.2(3) . . . no C29 C27 C30 107.4(3) . . . no N31 C32 C33 123.5(3) . . . yes C32 C33 C34 120.5(4) . . . no C33 C34 C35 115.5(3) . . . no C33 C34 C37 123.0(3) . . . no C35 C34 C37 121.5(3) . . . no C34 C35 C36 120.8(3) . . . no N31 C36 C35 123.6(3) . . . yes C34 C37 C38 174.6(4) . . . no Ru C38 C37 175.1(3) . . . yes N1 C41 C46 120.0(3) . . . yes N1 C41 C42 121.1(3) . . . yes C42 C41 C46 118.9(3) . . . no C41 C42 C43 119.4(3) . . . no C42 C43 C44 122.4(4) . . . no C45 C44 C47 121.1(4) . . . no C43 C44 C45 117.5(4) . . . no C43 C44 C47 121.5(4) . . . no C44 C45 C46 121.4(4) . . . no C41 C46 C45 120.4(4) . . . no N2 C51 C52 120.7(3) . . . yes N2 C51 C56 119.7(3) . . . yes C52 C51 C56 119.6(3) . . . no C51 C52 C53 119.8(4) . . . no C52 C53 C54 121.7(4) . . . no C53 C54 C57 121.0(4) . . . no C53 C54 C55 117.7(4) . . . no C55 C54 C57 121.4(4) . . . no C54 C55 C56 121.7(4) . . . no C51 C56 C55 119.5(4) . . . no C62 C61 C66 118.8(4) . . . no N3 C61 C62 120.4(3) . . . yes N3 C61 C66 120.8(3) . . . yes C61 C62 C63 120.2(4) . . . no C62 C63 C64 121.5(4) . . . no C65 C64 C67 120.5(4) . . . no C63 C64 C65 117.7(4) . . . no C63 C64 C67 121.8(4) . . . no C64 C65 C66 121.3(4) . . . no C61 C66 C65 120.4(4) . . . no C72 C71 C76 119.4(4) . . . no N4 C71 C72 120.6(3) . . . yes N4 C71 C76 120.0(3) . . . yes C71 C72 C73 119.9(4) . . . no C72 C73 C74 121.8(4) . . . no C73 C74 C77 122.7(4) . . . no C73 C74 C75 117.5(4) . . . no C75 C74 C77 119.7(4) . . . no C74 C75 C76 121.1(4) . . . no C71 C76 C75 120.3(4) . . . no N1 C4 H41 117.48 . . . no N2 C4 H41 117.54 2_555 . . no N3 C5 H51 117.91 . . . no N4 C5 H51 117.78 2_555 . . no C13 C12 H121 118.52 . . . no N11 C12 H121 118.56 . . . no C12 C13 H131 119.98 . . . no C14 C13 H131 119.93 . . . no C14 C15 H151 119.43 . . . no C16 C15 H151 119.39 . . . no H182 C18 H183 109.35 . . . no C17 C18 H181 109.46 . . . no C17 C18 H182 109.52 . . . no C17 C18 H183 109.47 . . . no H181 C18 H182 109.52 . . . no H181 C18 H183 109.52 . . . no H192 C19 H193 109.59 . . . no C17 C19 H192 109.45 . . . no C17 C19 H193 109.37 . . . no C17 C19 H191 109.41 . . . no H191 C19 H193 109.42 . . . no H191 C19 H192 109.60 . . . no C17 C20 H203 109.37 . . . no C17 C20 H202 109.49 . . . no C17 C20 H201 109.53 . . . no H202 C20 H203 109.50 . . . no H201 C20 H202 109.45 . . . no H201 C20 H203 109.49 . . . no N21 C22 H221 118.54 . . . no C23 C22 H221 118.43 . . . no C24 C23 H231 119.69 . . . no C22 C23 H231 119.79 . . . no C26 C25 H251 119.77 . . . no C24 C25 H251 119.75 . . . no H282 C28 H283 109.41 . . . no H281 C28 H283 109.49 . . . no C27 C28 H281 109.41 . . . no C27 C28 H282 109.45 . . . no C27 C28 H283 109.48 . . . no H281 C28 H282 109.60 . . . no C27 C29 H293 109.52 . . . no C27 C29 H291 109.51 . . . no C27 C29 H292 109.49 . . . no H292 C29 H293 109.46 . . . no H291 C29 H292 109.55 . . . no H291 C29 H293 109.30 . . . no C27 C30 H301 109.49 . . . no H302 C30 H303 109.53 . . . no H301 C30 H303 109.34 . . . no C27 C30 H302 109.50 . . . no C27 C30 H303 109.52 . . . no H301 C30 H302 109.44 . . . no C33 C32 H321 118.20 . . . no N31 C32 H321 118.25 . . . no C32 C33 H331 119.71 . . . no C34 C33 H331 119.83 . . . no C36 C35 H351 119.68 . . . no C34 C35 H351 119.56 . . . no N31 C36 H361 118.27 . . . no C35 C36 H361 118.10 . . . no C41 C42 H421 120.22 . . . no C43 C42 H421 120.35 . . . no C44 C43 H431 118.81 . . . no C42 C43 H431 118.83 . . . no C44 C45 H451 119.34 . . . no C46 C45 H451 119.22 . . . no C41 C46 H461 119.78 . . . no C45 C46 H461 119.85 . . . no H471 C47 H472 109.42 . . . no H471 C47 H473 109.55 . . . no C44 C47 H471 109.48 . . . no C44 C47 H472 109.47 . . . no C44 C47 H473 109.49 . . . no H472 C47 H473 109.42 . . . no C53 C52 H521 120.13 . . . no C51 C52 H521 120.02 . . . no C52 C53 H531 119.23 . . . no C54 C53 H531 119.09 . . . no C56 C55 H551 119.09 . . . no C54 C55 H551 119.17 . . . no C51 C56 H561 120.21 . . . no C55 C56 H561 120.32 . . . no C54 C57 H571 109.43 . . . no H571 C57 H573 109.49 . . . no H572 C57 H573 109.39 . . . no H571 C57 H572 109.50 . . . no C54 C57 H572 109.59 . . . no C54 C57 H573 109.42 . . . no C61 C62 H621 119.90 . . . no C63 C62 H621 119.93 . . . no C64 C63 H631 119.34 . . . no C62 C63 H631 119.17 . . . no C64 C65 H651 119.37 . . . no C66 C65 H651 119.31 . . . no C65 C66 H661 119.74 . . . no C61 C66 H661 119.90 . . . no H672 C67 H673 109.57 . . . no C64 C67 H673 109.34 . . . no C64 C67 H671 109.46 . . . no C64 C67 H672 109.44 . . . no H671 C67 H672 109.45 . . . no H671 C67 H673 109.56 . . . no C73 C72 H721 120.08 . . . no C71 C72 H721 120.03 . . . no C72 C73 H731 119.17 . . . no C74 C73 H731 119.08 . . . no C74 C75 H751 119.44 . . . no C76 C75 H751 119.43 . . . no C75 C76 H761 119.91 . . . no C71 C76 H761 119.79 . . . no C74 C77 H771 109.49 . . . no H772 C77 H773 109.42 . . . no C74 C77 H772 109.41 . . . no C74 C77 H773 109.49 . . . no H771 C77 H772 109.46 . . . no H771 C77 H773 109.56 . . . no C7 C6A C8 87.8(15) . . . no C7 C6B C8 87.8(15) . . . no C7 C6A H62A 113.05 . . . no H61A C6A H61B 138.09 . . . no H61A C6A H62A 110.20 . . . no C7 C6A H62B 132.21 . . . no C8 C6A H61A 58.34 . . . no C8 C6A H61B 92.77 . . . no C8 C6A H62A 74.39 . . . no C8 C6A H62B 92.68 . . . no C7 C6A H61A 113.00 . . . no H61B C6A H62A 86.78 . . . no H61B C6A H62B 103.19 . . . no H61A C6A H62B 107.47 . . . no C7 C6B H62A 113.05 . . . no C7 C6B H62B 132.21 . . . no H61A C6B H61B 138.09 . . . no H61A C6B H62A 110.20 . . . no H61A C6B H62B 107.47 . . . no C8 C6B H61A 58.34 . . . no C8 C6B H61B 92.77 . . . no C8 C6B H62A 74.39 . . . no C8 C6B H62B 92.68 . . . no C7 C6B H61A 113.00 . . . no H61B C6B H62A 86.78 . . . no H61B C6B H62B 103.19 . . . no C6A C7 H73 109.48 . . . no C6B C7 H71 109.37 . . . no H61B C7 H72 79.46 . . . no H61B C7 H73 127.11 . . . no H71 C7 H72 109.46 . . . no H71 C7 H73 109.45 . . . no C6B C7 H72 109.45 . . . no C6B C7 H73 109.48 . . . no H61B C7 H71 116.09 . . . no C6A C7 H71 109.37 . . . no C6A C7 H72 109.45 . . . no H72 C7 H73 109.62 . . . no C6B C8 H81 109.39 . . . no C6B C8 H82 109.45 . . . no H61A C8 H81 112.09 . . . no H61A C8 H82 68.48 . . . no H61A C8 H83 136.24 . . . no H81 C8 H82 109.26 . . . no H81 C8 H83 109.58 . . . no H82 C8 H83 109.36 . . . no C6B C8 H83 109.78 . . . no C6A C8 H81 109.39 . . . no C6A C8 H82 109.45 . . . no C6A C8 H83 109.78 . . . no S C F1 112.2(2) . . . yes S C F2 112.3(3) . . . yes S C F3 112.6(3) . . . yes F1 C F2 106.6(3) . . . yes F1 C F3 106.6(3) . . . yes F2 C F3 106.1(3) . . . yes # End of Crystallographic Information File