# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _audit_creation_method maXus _journal_coden_Cambridge 0182 _publ_contact_author_name 'Gwenael Rapenne' _publ_contact_author_address ; NanoSciences group, CEMES-CNRS, 29 rue Jeanne Marvig, BP4347, F-31055 Toulouse Cedex 4 France. ; _publ_contact_author_email rapenne@cemes.fr _publ_contact_author_fax (+33)562257999 _publ_contact_author_phone (+33)562257841 _publ_section_title ; Technomimetic molecules : Synthesis of ruthenium(II) 1,2,3,4,5-penta(p- bromophenyl)cyclopentadienyl hydrotris(indazolyl)borate, an organometallic molecular turnstile ; _publ_section_abstract ; We present the crystal and molecular structure of (1-bromo-1,2,3,4,5-penta(p-bromo)phenylcyclopendiene) hydrotris(indazolyl)borate ruthenium ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All diagrams and calculations were performed using maXus (Bruker Nonius, Delft & MacScience, Japan). ; loop_ _publ_author_name _publ_author_address 'Alexandre Carella' ; NanoSciences group, CEMES-CNRS, 29 rue Jeanne Marvig, BP4347, F-31055 Toulouse Cedex 4 France. ; 'Joel Jaud' ; NanoSciences group, CEMES-CNRS, 29 rue Jeanne Marvig, BP4347, F-31055 Toulouse Cedex 4 France. ; 'Gwenael Rapenne' ; NanoSciences group, CEMES-CNRS, 29 rue Jeanne Marvig, BP4347, F-31055 Toulouse Cedex 4 France. ; 'Jean-Pierre Launay' ; NanoSciences group, CEMES-CNRS, 29 rue Jeanne Marvig, BP4347, F-31055 Toulouse Cedex 4 France. ; _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Beurskens, P.T., Beurskens, G., Bosman, W.P., de Gelder, R. S. Garc\'ia-Granda, S., Gould, R.O. & Smits, J.M.M. (1996). The DIRDIF96 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Waasmaier, D. & Kirfel, A. (1995). Acta Cryst. A51, 416-431. Blessing, R.H. (1995), Acta. Cryst. A51, 33-38. ; data_1 _database_code_CSD 207452 _chemical_compound_source 'Local laboratory' _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.344 _exptl_crystal_size_mid 0.197 _exptl_crystal_size_min 0.087 _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment mixed _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1460.600 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z '-X+ 1/2,-Y,+Z+ 1/2' '+X+ 1/2,+Y,-Z+ 1/2' '+X+ 1/2,-Y+ 1/2,-Z' '-X+ 1/2,+Y+ 1/2,+Z' '-X,+Y+ 1/2,-Z+ 1/2' '+X,-Y+ 1/2,+Z+ 1/2' _symmetry_space_group_name_H-M 'P b c a ' _symmetry_cell_setting Orthorhombic _chemical_formula_moiety 'C68 H48 B Br5 N6 Ru ' _chemical_formula_sum 'C68 H48 B Br5 N6 Ru ' _chemical_name_systematic ; ? ; _cell_length_a 14.271(2) _cell_length_b 21.144(7) _cell_length_c 40.875(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12333.(5) _diffrn_reflns_number 83381 _diffrn_reflns_theta_max 28.00 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_full 28.00 _diffrn_reflns_av_R_equivalents 0.111 _computing_structure_solution 'DIRDIF (Buerskens et al., 1992)' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary difmap # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_absorpt_coefficient_mu 3.48 _exptl_crystal_F_000 5102 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 'Waasmaier & Kirfel, 1995' 'H ' 'H ' 0.0000 0.0000 'Waasmaier & Kirfel, 1995' 'N ' 'N ' 0.0061 0.0033 'Waasmaier & Kirfel, 1995' 'B ' 'B ' 0.0013 0.0007 'Waasmaier & Kirfel, 1995' Ru Ru -1.2594 0.8363 'Waasmaier & Kirfel, 1995' Br Br -0.2901 2.4595 'Waasmaier & Kirfel, 1995' # Refinement statistics _reflns_d_resolution_low 1.84 _reflns_d_resolution_high 0.62 _reflns_limit_h_max 18 _reflns_limit_h_min 0 _reflns_limit_k_max 27 _reflns_limit_k_min 0 _reflns_limit_l_max 53 _reflns_limit_l_min 0 _refine_ls_matrix_type full _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.002 _reflns_number_total 18144 _refine_ls_R_factor_all 0.484 _refine_ls_wR_factor_all 0.366 _refine_ls_goodness_of_fit_all 5.290 _reflns_number_gt 2938 _reflns_threshold_expression 'I> 3.00 sigma(I)' _refine_ls_R_factor_gt 0.088 _refine_ls_wR_factor_gt 0.144 _refine_ls_goodness_of_fit_gt 4.557 _refine_ls_number_reflns 2840 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_number_constraints 36 _refine_ls_wR_factor_ref 0.139 _refine_ls_goodness_of_fit_ref 4.390 _refine_ls_structure_factor_coef F^2^ _refine_special_details ; Refinement on F^2^. ; _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = 1 / ( s^2^(Fo^2^) + 0.10000 * Fo^2^) ; _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; equation(22) p292 'Crystallographic Computing' (1970) coefficient is multiplied by 10^4 ; _refine_ls_extinction_coef 2E4(5) _computing_structure_refinement 'maXus(Mackay et al., 1999)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material 'maXus(Mackay et al., 1999)' _atom_sites_solution_hydrogens geom _refine_diff_density_max 10.55 _refine_diff_density_min -8.63 _refine_diff_density_rms 1.19 #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ru1 0.03955(12) 0.23501(8) 0.13559(4) 0.0289(12) 1.00 Uij Br1 0.1516(5) -0.0795(3) 0.2219(5) 0.0667(19) 1.00 Uij Br2 -0.4055(6) 0.0441(6) 0.16794(15) 0.106(3) 1.00 Uij Br3 -0.4076(5) 0.4431(4) 0.1736(8) 0.098(2) 1.00 Uij Br4 0.1504(12) 0.5760(3) 0.2074(2) 0.0603(18) 1.00 Uij Br5 0.5173(3) 0.2590(9) 0.2188(3) 0.079(2) 1.00 Uij N1 0.0342(12) 0.3043(8) 0.0971(4) 0.047(5) 1.00 Uiso N2 0.0687(12) 0.2859(9) 0.0670(5) 0.052(6) 1.00 Uiso N3 -0.0172(10) 0.1719(8) 0.0994(4) 0.029(5) 1.00 Uiso N4 0.0140(11) 0.1765(8) 0.0679(4) 0.039(5) 1.00 Uiso N5 0.1640(12) 0.1981(8) 0.1148(4) 0.042(5) 1.00 Uiso N6 0.1783(13) 0.2005(8) 0.0822(4) 0.049(6) 1.00 Uiso C1 0.0378(5) 0.1903(3) 0.1837(4) 0.018(5) 1.00 Uiso C2 -0.0559(6) 0.2113(5) 0.17520(17) 0.021(5) 1.00 Uiso C3 -0.0530(5) 0.2800(4) 0.1709(8) 0.027(6) 1.00 Uiso C4 0.0425(11) 0.2987(3) 0.17608(18) 0.037(6) 1.00 Uiso C5 0.0998(3) 0.2451(9) 0.1848(3) 0.029(6) 1.00 Uiso C6 0.0694(4) 0.1254(2) 0.1918(3) 0.018(5) 1.00 Uiso C7 0.0863(9) 0.0790(3) 0.16893(17) 0.023(6) 1.00 Uiso C8 0.1110(9) 0.0190(2) 0.1782(2) 0.018(5) 1.00 Uiso C9 0.1184(4) 0.0032(2) 0.2094(3) 0.023(6) 1.00 Uiso C10 0.0963(9) 0.0475(3) 0.23371(16) 0.038(6) 1.00 Uiso C11 0.0751(9) 0.1092(2) 0.2241(2) 0.032(6) 1.00 Uiso C12 -0.1401(4) 0.1725(4) 0.17414(15) 0.032(6) 1.00 Uiso C13 -0.2123(4) 0.1848(5) 0.1521(3) 0.047(7) 1.00 Uiso C14 -0.2914(5) 0.1481(6) 0.1518(3) 0.050(7) 1.00 Uiso C15 -0.2998(4) 0.0966(4) 0.17180(15) 0.055(7) 1.00 Uiso C16 -0.2323(4) 0.0871(5) 0.1942(3) 0.047(7) 1.00 Uiso C17 -0.1496(6) 0.1247(7) 0.1955(3) 0.046(7) 1.00 Uiso C18 -0.1387(4) 0.3203(3) 0.1703(5) 0.019(5) 1.00 Uiso C19 -0.1773(8) 0.3405(6) 0.1414(3) 0.053(7) 1.00 Uiso C20 -0.2612(6) 0.3792(7) 0.1425(3) 0.063(8) 1.00 Uiso C21 -0.2944(4) 0.3933(3) 0.1720(4) 0.059(8) 1.00 Uiso C22 -0.2600(8) 0.3738(6) 0.2005(3) 0.081(9) 1.00 Uiso C23 -0.1784(6) 0.3363(7) 0.1986(3) 0.040(6) 1.00 Uiso C24 0.0724(8) 0.3685(2) 0.18212(17) 0.027(6) 1.00 Uiso C25 0.0480(7) 0.39512(16) 0.2116(2) 0.028(6) 1.00 Uiso C26 0.0750(11) 0.4563(2) 0.2188(2) 0.035(6) 1.00 Uiso C27 0.1225(7) 0.4899(2) 0.19617(16) 0.029(6) 1.00 Uiso C28 0.1480(7) 0.46850(16) 0.1671(2) 0.038(6) 1.00 Uiso C29 0.1213(11) 0.4037(2) 0.1602(2) 0.037(6) 1.00 Uiso C30 0.2003(2) 0.2507(6) 0.1924(2) 0.026(6) 1.00 Uiso C31 0.2287(2) 0.2269(5) 0.2209(2) 0.037(6) 1.00 Uiso C32 0.3249(3) 0.2286(8) 0.2303(3) 0.032(6) 1.00 Uiso C33 0.3865(2) 0.2553(5) 0.2087(2) 0.032(6) 1.00 Uiso C34 0.3607(2) 0.2828(5) 0.1803(2) 0.044(7) 1.00 Uiso C35 0.2632(3) 0.2799(8) 0.1725(3) 0.036(6) 1.00 Uiso C36 0.0693(16) 0.3401(13) 0.0480(6) 0.063(8) 1.00 Uiso C37 0.1094(17) 0.3484(14) 0.0165(7) 0.084(9) 1.00 Uiso C38 0.108(2) 0.4120(17) 0.0047(8) 0.126(12) 1.00 Uiso C39 0.078(2) 0.4583(15) 0.0238(8) 0.108(11) 1.00 Uiso C40 0.036(2) 0.4545(14) 0.0544(7) 0.101(10) 1.00 Uiso C41 0.0403(17) 0.3895(13) 0.0652(6) 0.069(8) 1.00 Uiso C42 0.0139(15) 0.3667(12) 0.0959(6) 0.059(8) 1.00 Uiso C43 -0.0272(16) 0.1325(11) 0.0500(6) 0.053(7) 1.00 Uiso C44 -0.0219(18) 0.1177(12) 0.0157(6) 0.082(9) 1.00 Uiso C45 -0.085(2) 0.0681(14) 0.0044(7) 0.105(11) 1.00 Uiso C46 -0.139(2) 0.0387(14) 0.0246(8) 0.098(10) 1.00 Uiso C47 -0.1488(17) 0.0476(12) 0.0576(6) 0.070(8) 1.00 Uiso C48 -0.0886(14) 0.0991(10) 0.0699(5) 0.040(6) 1.00 Uiso C49 -0.0749(15) 0.1251(12) 0.1024(5) 0.054(7) 1.00 Uiso C50 0.2685(16) 0.1765(10) 0.0751(6) 0.051(7) 1.00 Uiso C51 0.3083(18) 0.1733(12) 0.0426(6) 0.081(9) 1.00 Uiso C52 0.397(2) 0.1441(14) 0.0455(7) 0.099(10) 1.00 Uiso C53 0.435(2) 0.1263(15) 0.0740(8) 0.108(11) 1.00 Uiso C54 0.3985(18) 0.1311(12) 0.1043(6) 0.077(9) 1.00 Uiso C55 0.3029(16) 0.1542(11) 0.1031(5) 0.049(7) 1.00 Uiso C56 0.2387(15) 0.1709(9) 0.1275(5) 0.039(6) 1.00 Uiso C61 0.369(3) 0.4936(8) 0.0848(7) 0.140(14) 1.00 Uiso C62 0.2868(16) 0.462(2) 0.0774(8) 0.176(18) 1.00 Uiso C63 0.281(2) 0.397(2) 0.0813(4) 0.154(16) 1.00 Uiso C64 0.358(3) 0.3631(8) 0.0925(7) 0.138(14) 1.00 Uiso C65 0.4407(16) 0.395(2) 0.0999(8) 0.121(13) 1.00 Uiso C66 0.446(2) 0.460(2) 0.0960(4) 0.126(13) 1.00 Uiso C71 0.668(2) 0.2413(12) 0.0606(4) 0.146(14) 1.00 Uiso C72 0.764(3) 0.2382(14) 0.0556(8) 0.110(11) 1.00 Uiso C73 0.8138(13) 0.2928(18) 0.0485(7) 0.132(13) 1.00 Uiso C74 0.768(2) 0.3507(12) 0.0463(4) 0.132(13) 1.00 Uiso C75 0.672(3) 0.3538(14) 0.0513(8) 0.122(12) 1.00 Uiso C76 0.6220(13) 0.2991(18) 0.0584(7) 0.120(12) 1.00 Uiso B1 0.099(2) 0.2177(13) 0.0585(7) 0.05(2) 1.00 Uij H1 0.111806 0.209729 0.035978 0.065270 1.00 Uiso H7 0.082722 0.092251 0.146627 0.017680 1.00 Uiso H8 0.120546 -0.013344 0.162148 0.015768 1.00 Uiso H10 0.101704 0.033337 0.255837 0.022451 1.00 Uiso H11 0.061429 0.141083 0.239986 0.020482 1.00 Uiso H13 -0.203575 0.220296 0.137985 0.025392 1.00 Uiso H14 -0.352(12) 0.161(8) 0.139(4) 0.026449 1.00 Uiso H16 -0.241146 0.053298 0.209490 0.025596 1.00 Uiso H17 -0.101268 0.118399 0.211294 0.025011 1.00 Uiso H19 -0.146106 0.330080 0.121411 0.027473 1.00 Uiso H20 -0.290082 0.391961 0.122447 0.030760 1.00 Uiso H22 -0.293356 0.384845 0.219936 0.036654 1.00 Uiso H23 -0.148129 0.322397 0.218157 0.023159 1.00 Uiso H25 0.013838 0.370434 0.227155 0.019238 1.00 Uiso H26 0.059338 0.472037 0.240019 0.021519 1.00 Uiso H29 0.139(12) 0.384(8) 0.140(4) 0.022321 1.00 Uiso H37 0.133825 0.310764 0.006722 0.037830 1.00 Uiso H38 0.129310 0.421419 -0.016953 0.052266 1.00 Uiso H39 0.081693 0.501493 0.016954 0.045862 1.00 Uiso H40 0.013(12) 0.492(8) 0.065(4) 0.043358 1.00 Uiso H42 -0.011971 0.384618 0.115374 0.029318 1.00 Uiso H44 0.022787 0.142362 0.003860 0.037318 1.00 Uiso H45 -0.077(16) 0.075(12) -0.017(7) 0.044682 1.00 Uiso H46 -0.177927 0.005995 0.015860 0.042617 1.00 Uiso H47 -0.188704 0.020779 0.070245 0.033253 1.00 Uiso H49 -0.100713 0.114839 0.123300 0.027695 1.00 Uiso H51 0.271715 0.187350 0.024453 0.036835 1.00 Uiso H52 0.436(16) 0.138(12) 0.027(7) 0.043080 1.00 Uiso H53 0.496256 0.108264 0.073876 0.045777 1.00 Uiso H54 0.434590 0.118504 0.122900 0.035552 1.00 Uiso H56 0.239513 0.164665 0.150627 0.022772 1.00 Uiso H61 0.371979 0.538287 0.081022 0.056894 1.00 Uiso H66 0.50(2) 0.483(16) 0.101(8) 0.052239 1.00 Uiso H65 0.49(2) 0.373(16) 0.108(7) 0.050503 1.00 Uiso H64 0.36(2) 0.318(14) 0.096(7) 0.056260 1.00 Uiso H63 0.23(2) 0.374(14) 0.077(7) 0.061536 1.00 Uiso H62 0.23(2) 0.484(14) 0.069(7) 0.068872 1.00 Uiso H75 0.64(2) 0.395(14) 0.049(7) 0.050929 1.00 Uiso H74 0.81(2) 0.386(14) 0.041(7) 0.054113 1.00 Uiso H73 0.88(2) 0.288(14) 0.046(7) 0.053977 1.00 Uiso H76 0.56(2) 0.304(14) 0.061(7) 0.050141 1.00 Uiso H71 0.63(2) 0.206(14) 0.066(7) 0.058752 1.00 Uiso H72 0.79(2) 0.197(14) 0.058(7) 0.046811 1.00 Uiso H28 0.18(2) 0.495(14) 0.152(7) 0.022643 1.00 Uiso H31 0.18(2) 0.208(14) 0.235(7) 0.022359 1.00 Uiso H32 0.34(2) 0.211(14) 0.251(7) 0.020662 1.00 Uiso H34 0.41(2) 0.303(14) 0.167(7) 0.024657 1.00 Uiso H35 0.24(2) 0.299(14) 0.153(7) 0.021903 1.00 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.0311(12) 0.0204(11) 0.0352(11) 0.0056(10) -.0012(10) -.0027(11) Br1 0.073(2) 0.0272(17) 0.100(2) 0.0074(16) 0.0116(18) 0.0286(17) Br2 0.058(2) 0.133(3) 0.126(3) -.056(2) -.015(2) 0.028(2) Br3 0.060(2) 0.104(3) 0.129(3) 0.053(2) -.022(2) -.035(2) Br4 0.0526(19) 0.0286(17) 0.100(2) -.0069(15) 0.0002(16) -.0154(17) Br5 0.0399(18) 0.069(2) 0.129(3) -.0047(16) -.0332(17) 0.011(2) B1 0.07(2) 0.05(2) 0.05(2) 0.000(19) 0.015(18) -.013(18) _geom_special_details ; All standard uncertainties (except dihedral angles between l.s. planes) are estimated using the full covariance matrix. The standard uncertainties in cell dimensions are are used in calculating the standard uncertainties of bond distances, angles and torsion angles. Angles between l.s. planes have standard uncertainties calculated from atomic positional standard uncertainties; the errors in cell dimensions are not used in this case. ; 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 Ru1 N1 2.158(5) . . ? Ru1 N3 2.159(4) . . ? Ru1 N5 2.131(5) . . ? Ru1 C1 2.1917(5) . . ? Ru1 C2 2.1868(5) . . ? Ru1 C3 2.1860(5) . . ? Ru1 C4 2.1421(5) . . ? Ru1 C5 2.2072(5) . . ? Br1 C9 1.8879 . . ? Br2 C15 1.8909 . . ? Br3 C21 1.9401 . . ? Br4 C27 1.9249 . . ? Br5 C33 1.9264 . . ? N1 N2 1.389(6) . . ? N1 C42 1.356(7) . . ? N2 C36 1.388(7) . . ? N2 B1 1.549(8) . . ? N3 N4 1.375(5) . . ? N3 C49 1.299(7) . . ? N4 C43 1.327(6) . . ? N4 B1 1.546(8) . . ? N5 N6 1.359(6) . . ? N5 C56 1.324(6) . . ? N6 C50 1.423(7) . . ? N6 B1 1.545(9) . . ? C1 C2 1.4608 . . ? C1 C5 1.4643 . . ? C1 C6 1.4879 . . ? C2 C3 1.4663 . . ? C2 C12 1.4637 . . ? C3 C4 1.4439 . . ? C3 C18 1.5006 . . ? C4 C5 1.4478 . . ? C4 C24 1.5622 . . ? C5 C30 1.4832 . . ? C6 C7 1.3822 . . ? C6 C11 1.3723 . . ? C7 C8 1.3736 . . ? C8 C9 1.3311 . . ? C9 C10 1.4058 . . ? C10 C11 1.3998 . . ? C12 C13 1.3997 . . ? C12 C17 1.3481 . . ? C13 C14 1.3774 . . ? C14 C15 1.3729 . . ? C15 C16 1.3535 . . ? C16 C17 1.4309 . . ? C18 C19 1.3801 . . ? C18 C23 1.3379 . . ? C19 C20 1.4588 . . ? C20 C21 1.3358 . . ? C21 C22 1.3390 . . ? C22 C23 1.4185 . . ? C24 C25 1.3824 . . ? C24 C29 1.3643 . . ? C25 C26 1.3855 . . ? C26 C27 1.3555 . . ? C27 C28 1.3289 . . ? C28 C29 1.4537 . . ? C30 C31 1.3391 . . ? C30 C35 1.3667 . . ? C31 C32 1.4354 . . ? C32 C33 1.3754 . . ? C33 C34 1.3572 . . ? C34 C35 1.4393 . . ? C36 C37 1.427(9) . . ? C36 C41 1.332(8) . . ? C37 C38 1.433(9) . . ? C38 C39 1.328(10) . . ? C39 C40 1.394(9) . . ? C40 C41 1.449(9) . . ? C41 C42 1.402(8) . . ? C43 C44 1.447(8) . . ? C43 C48 1.393(7) . . ? C44 C45 1.462(9) . . ? C45 C46 1.297(9) . . ? C46 C47 1.378(9) . . ? C47 C48 1.481(8) . . ? C48 C49 1.459(7) . . ? C50 C51 1.452(8) . . ? C50 C55 1.341(7) . . ? C51 C52 1.419(9) . . ? C52 C53 1.350(9) . . ? C53 C54 1.354(9) . . ? C54 C55 1.460(8) . . ? C55 C56 1.405(7) . . ? C61 C62 1.3950 . . ? C61 C66 1.3950 . . ? C62 C63 1.3949 . . ? C63 C64 1.3950 . . ? C64 C65 1.3950 . . ? C65 C66 1.3950 . . ? C71 C72 1.3950 . . ? C71 C76 1.3950 . . ? C72 C73 1.3950 . . ? C73 C74 1.3951 . . ? C74 C75 1.3950 . . ? C75 C76 1.3950 . . ? 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 N5 Ru1 N3 78.7(3) . . . ? N5 Ru1 C3 159.9(4) . . . ? N3 Ru1 C3 119.9(4) . . . ? N5 Ru1 N1 88.8(4) . . . ? N3 Ru1 N1 84.9(4) . . . ? C3 Ru1 N1 99.9(4) . . . ? N5 Ru1 C4 122.2(4) . . . ? N3 Ru1 C4 158.8(4) . . . ? C3 Ru1 C4 38.9(4) . . . ? N1 Ru1 C4 98.0(4) . . . ? N5 Ru1 C5 94.8(4) . . . ? N3 Ru1 C5 147.8(4) . . . ? C3 Ru1 C5 65.5(4) . . . ? N1 Ru1 C5 126.8(4) . . . ? C4 Ru1 C5 38.0(4) . . . ? N5 Ru1 C1 102.0(4) . . . ? N3 Ru1 C1 110.4(4) . . . ? C3 Ru1 C1 65.6(4) . . . ? N1 Ru1 C1 162.6(4) . . . ? C4 Ru1 C1 64.7(4) . . . ? C5 Ru1 C1 39.6(3) . . . ? N5 Ru1 C2 137.7(4) . . . ? N3 Ru1 C2 97.3(4) . . . ? C3 Ru1 C2 39.4(4) . . . ? N1 Ru1 C2 133.2(4) . . . ? C4 Ru1 C2 65.4(4) . . . ? C5 Ru1 C2 66.4(4) . . . ? C1 Ru1 C2 39.5(3) . . . ? C42 N1 N2 106.9(10) . . . ? C42 N1 Ru1 134.5(9) . . . ? N2 N1 Ru1 118.2(8) . . . ? C36 N2 N1 107.8(11) . . . ? C36 N2 B1 129.9(12) . . . ? N1 N2 B1 122.3(11) . . . ? C49 N3 N4 106.5(9) . . . ? C49 N3 Ru1 134.1(8) . . . ? N4 N3 Ru1 119.3(7) . . . ? C43 N4 N3 109.1(10) . . . ? C43 N4 B1 128.8(11) . . . ? N3 N4 B1 121.2(10) . . . ? C56 N5 N6 106.9(10) . . . ? C56 N5 Ru1 132.8(8) . . . ? N6 N5 Ru1 120.2(8) . . . ? N5 N6 C50 108.6(10) . . . ? N5 N6 B1 120.8(10) . . . ? C50 N6 B1 130.1(11) . . . ? C5 C1 C2 109.2(9) . . . ? C5 C1 C6 124.7(9) . . . ? C2 C1 C6 125.9(9) . . . ? C5 C1 Ru1 71.0(6) . . . ? C2 C1 Ru1 71.7(5) . . . ? C6 C1 Ru1 128.1(7) . . . ? C3 C2 C12 125.5(10) . . . ? C3 C2 C1 105.4(9) . . . ? C12 C2 C1 129.1(10) . . . ? C3 C2 Ru1 68.9(6) . . . ? C12 C2 Ru1 128.5(7) . . . ? C1 C2 Ru1 68.8(5) . . . ? C2 C3 C4 108.1(10) . . . ? C2 C3 C18 121.9(10) . . . ? C4 C3 C18 127.4(11) . . . ? C2 C3 Ru1 71.7(6) . . . ? C4 C3 Ru1 70.5(6) . . . ? C18 C3 Ru1 138.0(8) . . . ? C5 C4 C3 110.8(10) . . . ? C5 C4 C24 123.3(11) . . . ? C3 C4 C24 124.2(11) . . . ? C5 C4 Ru1 71.9(6) . . . ? C3 C4 Ru1 70.6(6) . . . ? C24 C4 Ru1 136.3(8) . . . ? C4 C5 C1 106.4(9) . . . ? C4 C5 C30 125.3(11) . . . ? C1 C5 C30 128.2(10) . . . ? C4 C5 Ru1 70.1(6) . . . ? C1 C5 Ru1 69.3(5) . . . ? C30 C5 Ru1 127.5(7) . . . ? C11 C6 C7 118.8(9) . . . ? C11 C6 C1 118.5(9) . . . ? C7 C6 C1 122.6(9) . . . ? C6 C7 C8 122.4(10) . . . ? C9 C8 C7 117.8(11) . . . ? C8 C9 C10 123.1(11) . . . ? C8 C9 Br1 119.6(9) . . . ? C10 C9 Br1 117.3(8) . . . ? C9 C10 C11 118.9(11) . . . ? C6 C11 C10 119.0(11) . . . ? C17 C12 C13 118.7(11) . . . ? C17 C12 C2 118.6(10) . . . ? C13 C12 C2 122.6(11) . . . ? C14 C13 C12 123.2(12) . . . ? C13 C14 C15 118.9(12) . . . ? C16 C15 C14 118.9(13) . . . ? C16 C15 Br2 120.9(11) . . . ? C14 C15 Br2 120.2(10) . . . ? C15 C16 C17 121.2(13) . . . ? C12 C17 C16 118.8(11) . . . ? C23 C18 C19 119.4(12) . . . ? C23 C18 C3 118.5(11) . . . ? C19 C18 C3 122.1(11) . . . ? C18 C19 C20 120.7(12) . . . ? C21 C20 C19 115.9(13) . . . ? C20 C21 C22 125.7(13) . . . ? C20 C21 Br3 116.5(10) . . . ? C22 C21 Br3 117.8(10) . . . ? C21 C22 C23 116.0(13) . . . ? C18 C23 C22 122.3(12) . . . ? C29 C24 C25 120.3(12) . . . ? C29 C24 C4 123.4(11) . . . ? C25 C24 C4 116.3(11) . . . ? C24 C25 C26 122.0(12) . . . ? C27 C26 C25 116.3(11) . . . ? C28 C27 C26 123.8(12) . . . ? C28 C27 Br4 119.2(10) . . . ? C26 C27 Br4 116.9(9) . . . ? C27 C28 C29 118.8(12) . . . ? C24 C29 C28 118.7(11) . . . ? C31 C30 C35 117.1(10) . . . ? C31 C30 C5 120.3(10) . . . ? C35 C30 C5 122.6(10) . . . ? C30 C31 C32 120.7(11) . . . ? C33 C32 C31 118.8(11) . . . ? C34 C33 C32 124.1(11) . . . ? C34 C33 Br5 115.8(9) . . . ? C32 C33 Br5 120.1(9) . . . ? C33 C34 C35 114.8(11) . . . ? C30 C35 C34 124.4(11) . . . ? C41 C36 N2 107.6(14) . . . ? C41 C36 C37 123.3(16) . . . ? N2 C36 C37 128.3(15) . . . ? C36 C37 C38 115.7(16) . . . ? C39 C38 C37 116.5(17) . . . ? C38 C39 C40 132.5(18) . . . ? C39 C40 C41 105.5(15) . . . ? C36 C41 C42 110.2(15) . . . ? C36 C41 C40 126.4(15) . . . ? C42 C41 C40 123.4(15) . . . ? N1 C42 C41 107.3(12) . . . ? N4 C43 C48 108.1(12) . . . ? N4 C43 C44 129.2(13) . . . ? C48 C43 C44 122.6(14) . . . ? C43 C44 C45 113.6(14) . . . ? C46 C45 C44 122.0(17) . . . ? C45 C46 C47 126.7(17) . . . ? C46 C47 C48 114.1(14) . . . ? C43 C48 C49 105.7(12) . . . ? C43 C48 C47 121.0(13) . . . ? C49 C48 C47 133.2(12) . . . ? N3 C49 C48 110.3(11) . . . ? C55 C50 N6 107.5(12) . . . ? C55 C50 C51 126.2(14) . . . ? N6 C50 C51 125.9(13) . . . ? C52 C51 C50 109.8(14) . . . ? C53 C52 C51 124.7(16) . . . ? C54 C53 C52 125.2(17) . . . ? C53 C54 C55 111.7(14) . . . ? C50 C55 C56 106.3(13) . . . ? C50 C55 C54 121.3(13) . . . ? C56 C55 C54 130.2(13) . . . ? N5 C56 C55 109.7(11) . . . ? C62 C61 C66 111(2) . . . ? C63 C62 C61 115(2) . . . ? C62 C63 C64 134(2) . . . ? C63 C64 C65 113(2) . . . ? C66 C65 C64 117(2) . . . ? C65 C66 C61 130(2) . . . ? C72 C71 C76 117(2) . . . ? C73 C72 C71 124(2) . . . ? C72 C73 C74 124(2) . . . ? C73 C74 C75 112(2) . . . ? C76 C75 C74 127(2) . . . ? C75 C76 C71 116.5(19) . . . ? N2 B1 N6 107.5(11) . . . ? N2 B1 N4 106.9(10) . . . ? N6 B1 N4 106.0(10) . . . ? #===================================================