# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2261 data_global #====================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; 'Heck , J\"urgen' Institut f\"ur Anorganische und Angewandte Chemie Universit\"at Hamburg Martin-Luther-King-Platz 6 D-20146 Hamburg Bundesrepublik Deutschland ; _publ_contact_author_phone '049 40 42838 6375' _publ_contact_author_fax '049 40 42838 6348' _publ_contact_author_email 'heck@chemie.uni-hamburg.de' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Tucson, den 06.07.2000 Dear Mr and Mrs.! I send you the data of structures. Please give me a note if you received it. Best regards Timo Meyer-Friedrichsen (Co-Autor) e-mail: timo@u.arizona.edu ; #====================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _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 ; Azulenylium and guaiazulenylium cations as novel accepting moieties in extended sesquifulvalene type D-p-A chromophores ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address Deutschland ; Tony Farrell Timo Meyer-Friedrichsen Maik Malessa J\u"rgen Heck Institut f\"ur Anorganische und Angewandte Chemie Universit\"at Hamburg Martin-Luther-King-Platz 6 D-20146 Hamburg Bundesrepublik Deutschland Detlev Haase Wolgang Saak Universit\"at Oldenburg, FB Chemie Carl-von-Ossietzkystr. 9-11 D-26111 Oldenburg Bundesrepublik Deutschland Anthony R. Manning University College Dublin Belfield, Dublin 4 Ireland ; #====================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_experimental ; ; _publ_section_references ; Sheldrick, G.M. (1986). SHELXS-86 Program for crystal structure determination, University of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXS-97 Program for crystal structure refinement, University of G\"ottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; We thank Dr. Falk Olbrich for the X-ray measurement of the Fc-guaz (data_g1) complex at the Universit\"at Magdeburg. ; #====================================================================== data_g1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ferrocenylguaiazulenyliumtetrafluoroborat _chemical_formula_moiety 'C26 H27 B F4 Fe ' _chemical_formula_sum 'C28 H31 B F4 Fe O0.50' _chemical_formula_weight 518.19 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 11.20960(10) _cell_length_b 10.2163(2) _cell_length_c 22.1867(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.3430(10) _cell_angle_gamma 90.00 _cell_volume 2472.25(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Crystals were grown from THF-solution ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens axs SMART CCD System' _diffrn_measurement_method 'omega-scan' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15381 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5668 _reflns_number_gt 4181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens xscans' _computing_cell_refinement 'Siemens xscans' _computing_data_reduction 'Siemens axs SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1261P)^2^+2.4784P] 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 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5668 _refine_ls_number_parameters 424 _refine_ls_number_restraints 106 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2290 _refine_ls_wR_factor_gt 0.2098 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.092 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.62626(13) 0.69230(16) 0.59510(9) 0.0361(3) Uani 0.873(4) d P A 1 C1 C 0.4506(4) 0.6299(4) 0.5649(2) 0.0383(10) Uani 0.873(4) d P A 1 H1 H 0.4239 0.5415 0.5639 0.046 Uiso 0.873(4) calc PR A 1 C2 C 0.4887(4) 0.6967(5) 0.51611(18) 0.0405(11) Uani 0.873(4) d P A 1 H2 H 0.4909 0.6608 0.4769 0.049 Uiso 0.873(4) calc PR A 1 C3 C 0.5229(5) 0.8260(5) 0.5363(2) 0.0458(12) Uani 0.873(4) d P A 1 H3 H 0.5517 0.8916 0.5128 0.055 Uiso 0.873(4) calc PR A 1 C4 C 0.5065(4) 0.8409(5) 0.5980(2) 0.0398(10) Uani 0.873(4) d P A 1 H4 H 0.5238 0.9176 0.6227 0.048 Uiso 0.873(4) calc PR A 1 C5 C 0.4595(3) 0.7202(5) 0.61623(18) 0.0318(8) Uani 0.873(4) d P A 1 C6 C 0.4389(3) 0.6741(4) 0.67429(18) 0.0326(8) Uani 0.873(4) d P A 1 H6 H 0.4309 0.5820 0.6779 0.039 Uiso 0.873(4) calc PR A 1 C7 C 0.4293(5) 0.7467(4) 0.7256(2) 0.0292(8) Uani 0.873(4) d P A 1 C8 C 0.4284(4) 0.8883(4) 0.72856(19) 0.0374(9) Uani 0.873(4) d P A 1 H8 H 0.4384 0.9445 0.6960 0.045 Uiso 0.873(4) calc PR A 1 C9 C 0.4114(4) 0.9304(4) 0.7843(2) 0.0391(10) Uani 0.873(4) d P A 1 C10 C 0.3971(3) 0.8164(4) 0.82099(18) 0.0328(8) Uani 0.873(4) d P A 1 C11 C 0.4091(3) 0.6998(4) 0.78527(18) 0.0298(8) Uani 0.873(4) d P A 1 C12 C 0.4057(4) 0.5699(4) 0.8060(2) 0.0362(9) Uani 0.873(4) d P A 1 C13 C 0.3730(4) 0.5327(4) 0.8617(2) 0.0416(10) Uani 0.873(4) d P A 1 H13 H 0.3646 0.4409 0.8659 0.050 Uiso 0.873(4) calc PR A 1 C14 C 0.3509(4) 0.6039(5) 0.9110(2) 0.0423(10) Uani 0.873(4) d P A 1 H14 H 0.3272 0.5527 0.9420 0.051 Uiso 0.873(4) calc PR A 1 C15 C 0.3575(4) 0.7393(5) 0.9231(2) 0.0351(10) Uani 0.873(4) d P A 1 C16 C 0.3774(4) 0.8324(4) 0.88099(19) 0.0361(9) Uani 0.873(4) d P A 1 H16 H 0.3779 0.9205 0.8947 0.043 Uiso 0.873(4) calc PR A 1 C17 C 0.4070(6) 1.0690(5) 0.8043(2) 0.0608(14) Uani 0.873(4) d P A 1 H17A H 0.4116 1.1272 0.7698 0.091 Uiso 0.873(4) calc PR A 1 H17B H 0.4763 1.0863 0.8393 0.091 Uiso 0.873(4) calc PR A 1 H17C H 0.3300 1.0846 0.8169 0.091 Uiso 0.873(4) calc PR A 1 C18 C 0.4352(6) 0.4549(5) 0.7689(2) 0.0604(14) Uani 0.873(4) d P A 1 H18A H 0.3688 0.4429 0.7319 0.091 Uiso 0.873(4) calc PR A 1 H18B H 0.4438 0.3755 0.7943 0.091 Uiso 0.873(4) calc PR A 1 H18C H 0.5121 0.4718 0.7564 0.091 Uiso 0.873(4) calc PR A 1 C19 C 0.3399(4) 0.7787(5) 0.9870(2) 0.0448(11) Uani 0.873(4) d P A 1 H19 H 0.2678 0.7287 0.9943 0.054 Uiso 0.873(4) calc PR A 1 C20 C 0.3140(5) 0.9235(6) 0.9947(2) 0.0576(13) Uani 0.873(4) d P A 1 H20A H 0.3876 0.9747 0.9941 0.086 Uiso 0.873(4) calc PR A 1 H20B H 0.2912 0.9370 1.0343 0.086 Uiso 0.873(4) calc PR A 1 H20C H 0.2466 0.9519 0.9608 0.086 Uiso 0.873(4) calc PR A 1 C21 C 0.4537(6) 0.7336(6) 1.0366(2) 0.0622(15) Uani 0.873(4) d P A 1 H21A H 0.4642 0.6388 1.0332 0.093 Uiso 0.873(4) calc PR A 1 H21B H 0.4421 0.7548 1.0779 0.093 Uiso 0.873(4) calc PR A 1 H21C H 0.5268 0.7786 1.0299 0.093 Uiso 0.873(4) calc PR A 1 C22 C 0.7890(6) 0.7219(6) 0.6576(3) 0.051(2) Uani 0.611(2) d PG A 1 H22 H 0.8045 0.7907 0.6872 0.061 Uiso 0.611(2) calc PR A 1 C23 C 0.8047(5) 0.7284(9) 0.5959(4) 0.067(3) Uani 0.611(2) d PG A 1 H23 H 0.8326 0.8023 0.5771 0.080 Uiso 0.611(2) calc PR A 1 C24 C 0.7715(7) 0.6051(11) 0.5675(2) 0.072(3) Uani 0.611(2) d PG A 1 H24 H 0.7732 0.5820 0.5262 0.086 Uiso 0.611(2) calc PR A 1 C25 C 0.7353(7) 0.5224(5) 0.6115(4) 0.069(3) Uani 0.611(2) d PG A 1 H25 H 0.7085 0.4343 0.6049 0.083 Uiso 0.611(2) calc PR A 1 C26 C 0.7461(6) 0.5946(8) 0.6672(3) 0.058(3) Uani 0.611(2) d PG A 1 H26 H 0.7278 0.5633 0.7043 0.069 Uiso 0.611(2) calc PR A 1 C22 C 0.7558(17) 0.5598(15) 0.5906(8) 0.052(5) Uiso 0.2620(11) d PG A 3 H22A H 0.7421 0.4833 0.5656 0.062 Uiso 0.2620(11) calc PR A 3 C23 C 0.7938(14) 0.6836(19) 0.5728(5) 0.042(5) Uiso 0.2620(11) d PG A 3 H23A H 0.8100 0.7045 0.5338 0.051 Uiso 0.2620(11) calc PR A 3 C24 C 0.8033(12) 0.7706(12) 0.6236(9) 0.041(4) Uiso 0.2620(11) d PG A 3 H24A H 0.8271 0.8600 0.6245 0.049 Uiso 0.2620(11) calc PR A 3 C25 C 0.7712(17) 0.701(2) 0.6728(6) 0.045(5) Uiso 0.2620(11) d PG A 3 H25A H 0.7696 0.7348 0.7124 0.054 Uiso 0.2620(11) calc PR A 3 C26 C 0.7418(19) 0.5702(18) 0.6524(9) 0.051(6) Uiso 0.2620(11) d PG A 3 H26A H 0.7171 0.5020 0.6760 0.061 Uiso 0.2620(11) calc PR A 3 Fe1A Fe 0.6339(9) 0.7330(13) 0.5988(7) 0.061(5) Uani 0.127(4) d PD A 2 C1A C 0.5010(18) 0.8731(16) 0.5725(11) 0.038(2) Uiso 0.127(4) d PGD A 2 H1A H 0.5122 0.9650 0.5774 0.045 Uiso 0.127(4) calc PR A 2 C2A C 0.5138(19) 0.798(2) 0.5204(6) 0.038(2) Uiso 0.127(4) d PGD A 2 H2A H 0.5350 0.8316 0.4842 0.045 Uiso 0.127(4) calc PR A 2 C3A C 0.4893(17) 0.665(2) 0.5317(9) 0.038(2) Uiso 0.127(4) d PGD A 2 H3A H 0.4912 0.5941 0.5045 0.045 Uiso 0.127(4) calc PR A 2 C4A C 0.4614(13) 0.658(2) 0.5909(11) 0.038(2) Uiso 0.127(4) d PGD A 2 H4A H 0.4413 0.5806 0.6102 0.045 Uiso 0.127(4) calc PR A 2 C5A C 0.4686(14) 0.786(3) 0.6161(9) 0.038(2) Uiso 0.127(4) d PGD A 2 C6A C 0.455(2) 0.822(2) 0.6753(7) 0.038(2) Uiso 0.127(4) d PD A 2 H6A H 0.4659 0.9128 0.6842 0.045 Uiso 0.127(4) calc PR A 2 C7A C 0.427(3) 0.7476(19) 0.7236(9) 0.038(2) Uiso 0.127(4) d PGD A 2 C8A C 0.437(2) 0.6090(19) 0.7265(8) 0.038(2) Uiso 0.127(4) d PG A 2 H8A H 0.4505 0.5532 0.6946 0.045 Uiso 0.127(4) calc PR A 2 C9A C 0.422(2) 0.5686(14) 0.7856(8) 0.038(2) Uiso 0.127(4) d PGD A 2 C10A C 0.403(2) 0.6821(18) 0.8192(7) 0.038(2) Uiso 0.127(4) d PGD A 2 C11A C 0.407(2) 0.7928(14) 0.7809(9) 0.038(2) Uiso 0.127(4) d PGD A 2 C12A C 0.390(3) 0.9220(15) 0.7991(11) 0.038(2) Uiso 0.127(4) d PD A 2 C13A C 0.362(2) 0.968(3) 0.8538(8) 0.038(2) Uiso 0.127(4) d PD A 2 H13A H 0.3444 1.0595 0.8536 0.045 Uiso 0.127(4) calc PR A 2 C14A C 0.355(3) 0.903(2) 0.9087(11) 0.038(2) Uiso 0.127(4) d PD A 2 H14A H 0.3326 0.9561 0.9396 0.045 Uiso 0.127(4) calc PR A 2 C15A C 0.376(5) 0.770(2) 0.9238(13) 0.038(2) Uiso 0.127(4) d PD A 2 C16A C 0.386(3) 0.675(3) 0.8798(8) 0.038(2) Uiso 0.127(4) d PD A 2 H16A H 0.3797 0.5874 0.8938 0.045 Uiso 0.127(4) calc PR A 2 C17A C 0.442(3) 0.4283(16) 0.8100(13) 0.038(2) Uiso 0.127(4) d PD A 2 H17D H 0.5173 0.4239 0.8426 0.057 Uiso 0.127(4) calc PR A 2 H17E H 0.4482 0.3694 0.7760 0.057 Uiso 0.127(4) calc PR A 2 H17F H 0.3721 0.4016 0.8270 0.057 Uiso 0.127(4) calc PR A 2 C18A C 0.377(3) 1.035(2) 0.7528(12) 0.038(2) Uiso 0.127(4) d PD A 2 H18D H 0.4554 1.0498 0.7416 0.057 Uiso 0.127(4) calc PR A 2 H18E H 0.3528 1.1147 0.7717 0.057 Uiso 0.127(4) calc PR A 2 H18F H 0.3140 1.0134 0.7156 0.057 Uiso 0.127(4) calc PR A 2 C19A C 0.369(2) 0.728(3) 0.9891(11) 0.038(2) Uiso 0.127(4) d PD A 2 H19A H 0.3083 0.6548 0.9816 0.045 Uiso 0.127(4) calc PR A 2 C20A C 0.310(3) 0.829(3) 1.0243(13) 0.038(2) Uiso 0.127(4) d PD A 2 H20D H 0.2959 0.9106 1.0005 0.057 Uiso 0.127(4) calc PR A 2 H20E H 0.3653 0.8461 1.0648 0.057 Uiso 0.127(4) calc PR A 2 H20F H 0.2321 0.7950 1.0303 0.057 Uiso 0.127(4) calc PR A 2 C21A C 0.489(2) 0.661(3) 1.0210(13) 0.038(2) Uiso 0.127(4) d PD A 2 H21D H 0.5265 0.6213 0.9897 0.057 Uiso 0.127(4) calc PR A 2 H21E H 0.4724 0.5935 1.0492 0.057 Uiso 0.127(4) calc PR A 2 H21F H 0.5454 0.7264 1.0446 0.057 Uiso 0.127(4) calc PR A 2 C22A C 0.7941(15) 0.826(2) 0.6284(10) 0.038(2) Uiso 0.127(4) d PGD A 2 H22B H 0.8070 0.9177 0.6320 0.045 Uiso 0.127(4) calc PR A 2 C23A C 0.7701(17) 0.742(2) 0.6751(6) 0.038(2) Uiso 0.127(4) d PGD A 2 H23B H 0.7640 0.7672 0.7154 0.045 Uiso 0.127(4) calc PR A 2 C24A C 0.7568(19) 0.612(2) 0.6509(10) 0.038(2) Uiso 0.127(4) d PGD A 2 H24B H 0.7402 0.5363 0.6722 0.045 Uiso 0.127(4) calc PR A 2 C25A C 0.7726(18) 0.617(2) 0.5892(10) 0.038(2) Uiso 0.127(4) d PGD A 2 H25B H 0.7684 0.5441 0.5621 0.045 Uiso 0.127(4) calc PR A 2 C26A C 0.7957(15) 0.749(3) 0.5753(9) 0.038(2) Uiso 0.127(4) d PGD A 2 H26B H 0.8097 0.7799 0.5372 0.045 Uiso 0.127(4) calc PR A 2 B1 B 0.3569(2) 0.2582(2) 0.61900(11) 0.0472(17) Uani 0.800(8) d PD B 1 F1 F 0.3045(4) 0.2547(4) 0.66884(15) 0.0923(17) Uani 0.800(8) d PD B 1 F2 F 0.4580(4) 0.3373(4) 0.6320(2) 0.0950(19) Uani 0.800(8) d PD B 1 F3 F 0.2742(4) 0.3063(6) 0.56865(17) 0.140(3) Uani 0.800(8) d PD B 1 F4 F 0.3909(4) 0.1345(3) 0.6064(2) 0.119(2) Uani 0.800(8) d PD B 1 B2 B 0.3594(9) 0.2242(10) 0.6134(5) 0.029(5) Uiso 0.200(8) d PD B 2 F1A F 0.3583(16) 0.2006(17) 0.6739(5) 0.110(5) Uiso 0.200(8) d PD B 2 F23 F 0.3630(17) 0.3563(10) 0.6039(8) 0.110(5) Uiso 0.200(8) d PD B 2 F34 F 0.2558(12) 0.1731(18) 0.5758(7) 0.110(5) Uiso 0.200(8) d PD B 2 F24 F 0.4605(13) 0.1669(17) 0.6000(9) 0.110(5) Uiso 0.200(8) d PD B 2 O1 O 0.726(2) 0.0203(16) 0.7411(16) 0.144(11) Uani 0.30 d PD . 4 C27 C 0.775(3) 0.110(2) 0.7899(13) 0.15(2) Uani 0.30 d PD . 4 C28 C 0.745(4) 0.247(2) 0.7629(11) 0.094(8) Uani 0.30 d PD . 4 C29 C 0.760(3) 0.2185(16) 0.6973(8) 0.104(10) Uani 0.30 d PD . 4 C30 C 0.765(2) 0.0702(16) 0.6885(16) 0.101(9) Uani 0.30 d PD . 4 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 Fe1 0.0303(5) 0.0491(6) 0.0291(5) -0.0021(4) 0.0071(3) 0.0096(4) C1 0.038(2) 0.039(2) 0.037(2) -0.0075(18) 0.0065(17) 0.0013(17) C2 0.040(2) 0.055(3) 0.0254(18) 0.0001(18) 0.0047(16) 0.013(2) C3 0.049(3) 0.045(3) 0.045(3) 0.011(2) 0.016(2) 0.015(2) C4 0.044(2) 0.034(2) 0.046(2) -0.0037(18) 0.018(2) 0.0022(19) C5 0.0279(18) 0.036(2) 0.0324(19) -0.0070(17) 0.0088(14) 0.0019(15) C6 0.0311(18) 0.0313(19) 0.0366(19) -0.0041(15) 0.0099(15) -0.0010(15) C7 0.0232(16) 0.0299(18) 0.0337(19) -0.0025(15) 0.0053(14) -0.0008(14) C8 0.043(2) 0.032(2) 0.038(2) 0.0003(17) 0.0121(17) 0.0039(17) C9 0.047(3) 0.033(2) 0.038(2) -0.0041(18) 0.0124(18) 0.0025(18) C10 0.0283(18) 0.035(2) 0.0343(19) -0.0035(16) 0.0050(15) 0.0012(15) C11 0.0217(16) 0.032(2) 0.0347(19) -0.0056(16) 0.0053(14) -0.0018(14) C12 0.037(2) 0.034(2) 0.038(2) -0.0029(17) 0.0083(17) 0.0004(16) C13 0.045(2) 0.035(2) 0.044(2) -0.0013(18) 0.0088(18) -0.0038(18) C14 0.042(2) 0.045(2) 0.039(2) 0.0018(19) 0.0099(17) -0.0020(19) C15 0.025(2) 0.049(3) 0.0303(18) -0.0044(19) 0.0043(15) -0.004(2) C16 0.0320(19) 0.040(2) 0.035(2) -0.0045(17) 0.0047(15) 0.0022(16) C17 0.102(4) 0.034(2) 0.052(3) -0.002(2) 0.030(3) 0.013(3) C18 0.104(4) 0.031(2) 0.052(3) -0.003(2) 0.029(3) 0.000(3) C19 0.039(2) 0.063(3) 0.033(2) -0.005(2) 0.0084(18) -0.003(2) C20 0.063(3) 0.070(3) 0.042(2) -0.012(2) 0.017(2) 0.008(3) C21 0.073(4) 0.072(4) 0.034(2) 0.001(2) -0.002(2) 0.007(3) C22 0.026(3) 0.069(6) 0.053(5) -0.002(5) -0.002(3) 0.001(3) C23 0.028(3) 0.114(8) 0.058(6) 0.017(7) 0.009(3) 0.006(4) C24 0.051(4) 0.116(9) 0.051(5) -0.007(6) 0.017(4) 0.046(5) C25 0.061(5) 0.064(5) 0.071(6) 0.001(5) -0.008(4) 0.039(4) C26 0.056(5) 0.076(7) 0.034(4) 0.006(4) -0.003(3) 0.025(4) Fe1A 0.037(4) 0.116(13) 0.035(4) -0.003(6) 0.017(3) -0.003(5) B1 0.084(5) 0.026(3) 0.038(3) -0.002(2) 0.027(3) 0.002(3) F1 0.145(4) 0.091(3) 0.061(2) -0.006(2) 0.065(3) -0.035(3) F2 0.119(4) 0.071(3) 0.111(4) -0.023(2) 0.061(3) -0.045(3) F3 0.111(5) 0.222(9) 0.079(3) 0.035(4) 0.008(3) 0.067(5) F4 0.164(6) 0.039(2) 0.166(5) -0.022(3) 0.062(4) 0.013(3) O1 0.09(2) 0.059(8) 0.26(3) -0.03(2) -0.01(2) -0.007(11) C27 0.09(2) 0.065(18) 0.30(6) 0.06(3) 0.04(3) -0.004(16) C28 0.118(19) 0.105(16) 0.08(3) -0.002(14) 0.07(2) 0.016(18) C29 0.090(16) 0.041(11) 0.18(3) 0.033(15) 0.04(2) 0.023(10) C30 0.089(17) 0.040(11) 0.17(3) -0.008(15) 0.010(17) -0.024(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C23 2.030(5) . ? Fe1 C1 2.031(4) . ? Fe1 C4 2.037(4) . ? Fe1 C22 2.043(5) . ? Fe1 C5 2.049(4) . ? Fe1 C2 2.050(4) . ? Fe1 C3 2.053(5) . ? Fe1 C24 2.069(5) . ? Fe1 C26 2.089(6) . ? Fe1 C25 2.105(6) . ? C1 C2 1.426(6) . ? C1 C5 1.451(6) . ? C2 C3 1.419(7) . ? C3 C4 1.430(6) . ? C4 C5 1.436(6) . ? C5 C6 1.439(5) . ? C6 C7 1.383(6) . ? C7 C8 1.448(6) . ? C7 C11 1.474(6) . ? C8 C9 1.363(6) . ? C9 C10 1.451(6) . ? C9 C17 1.487(6) . ? C10 C16 1.408(6) . ? C10 C11 1.454(5) . ? C11 C12 1.408(6) . ? C12 C13 1.419(6) . ? C12 C18 1.514(6) . ? C13 C14 1.383(6) . ? C14 C15 1.408(7) . ? C15 C16 1.387(7) . ? C15 C19 1.530(6) . ? C19 C20 1.524(8) . ? C19 C21 1.550(7) . ? C22 C26 1.4200 . ? C22 C23 1.4200 . ? C23 C24 1.4200 . ? C24 C25 1.4200 . ? C25 C26 1.4200 . ? C22 C26 1.4200 . ? C22 C23 1.4200 . ? C23 C24 1.4200 . ? C24 C25 1.4200 . ? C25 C26 1.4200 . ? Fe1A C23A 2.003(8) . ? Fe1A C22A 2.003(8) . ? Fe1A C24A 2.005(8) . ? Fe1A C26A 2.005(8) . ? Fe1A C25A 2.006(8) . ? Fe1A C2A 2.0500 . ? Fe1A C3A 2.0501 . ? Fe1A C1A 2.0500 . ? Fe1A C4A 2.0501 . ? Fe1A C5A 2.0501 . ? C1A C2A 1.4200 . ? C1A C5A 1.4200 . ? C2A C3A 1.4200 . ? C3A C4A 1.4200 . ? C4A C5A 1.4200 . ? C5A C6A 1.406(9) . ? C6A C7A 1.406(9) . ? C7A C8A 1.4200 . ? C7A C11A 1.4200 . ? C8A C9A 1.4200 . ? C9A C10A 1.4200 . ? C9A C17A 1.5299(11) . ? C10A C16A 1.406(9) . ? C10A C11A 1.4200 . ? C11A C12A 1.406(9) . ? C12A C13A 1.406(9) . ? C12A C18A 1.5300(11) . ? C13A C14A 1.406(8) . ? C14A C15A 1.406(8) . ? C15A C16A 1.406(9) . ? C15A C19A 1.5300(10) . ? C19A C20A 1.5300(10) . ? C19A C21A 1.5300(11) . ? C22A C23A 1.4200 . ? C22A C26A 1.4200 . ? C23A C24A 1.4200 . ? C24A C25A 1.4200 . ? C25A C26A 1.4200 . ? B1 F1 1.367(2) . ? B1 F4 1.368(2) . ? B1 F3 1.368(2) . ? B1 F2 1.368(2) . ? B2 F1A 1.368(2) . ? B2 F23 1.368(2) . ? B2 F34 1.368(2) . ? B2 F24 1.368(2) . ? O1 O1 0.59(5) 2_656 ? O1 C27 1.15(4) 2_656 ? O1 C27 1.4300(11) . ? O1 C30 1.4300(10) . ? O1 C30 1.62(7) 2_656 ? C27 C30 0.84(4) 2_656 ? C27 O1 1.15(4) 2_656 ? C27 C29 1.23(4) 2_656 ? C27 C28 1.5300(11) . ? C27 C27 1.73(6) 2_656 ? C27 C28 1.81(3) 2_656 ? C28 C28 0.60(3) 2_656 ? C28 C29 0.95(3) 2_656 ? C28 C29 1.5300(10) . ? C28 C27 1.81(3) 2_656 ? C29 C28 0.95(3) 2_656 ? C29 C27 1.23(4) 2_656 ? C29 C30 1.5300(10) . ? C30 C27 0.84(4) 2_656 ? C30 O1 1.62(7) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 Fe1 C1 159.8(3) . . ? C23 Fe1 C4 121.3(3) . . ? C1 Fe1 C4 69.43(18) . . ? C23 Fe1 C22 40.80(10) . . ? C1 Fe1 C22 156.4(3) . . ? C4 Fe1 C22 111.1(2) . . ? C23 Fe1 C5 157.2(4) . . ? C1 Fe1 C5 41.66(16) . . ? C4 Fe1 C5 41.14(18) . . ? C22 Fe1 C5 122.9(3) . . ? C23 Fe1 C2 123.3(3) . . ? C1 Fe1 C2 40.90(18) . . ? C4 Fe1 C2 68.89(18) . . ? C22 Fe1 C2 162.6(3) . . ? C5 Fe1 C2 69.33(17) . . ? C23 Fe1 C3 107.2(2) . . ? C1 Fe1 C3 68.7(2) . . ? C4 Fe1 C3 40.93(19) . . ? C22 Fe1 C3 128.1(3) . . ? C5 Fe1 C3 69.02(18) . . ? C2 Fe1 C3 40.5(2) . . ? C23 Fe1 C24 40.52(9) . . ? C1 Fe1 C24 122.4(3) . . ? C4 Fe1 C24 154.1(4) . . ? C22 Fe1 C24 67.93(12) . . ? C5 Fe1 C24 161.7(4) . . ? C2 Fe1 C24 104.1(2) . . ? C3 Fe1 C24 117.8(3) . . ? C23 Fe1 C26 67.78(13) . . ? C1 Fe1 C26 120.4(2) . . ? C4 Fe1 C26 130.1(3) . . ? C22 Fe1 C26 40.17(10) . . ? C5 Fe1 C26 110.5(2) . . ? C2 Fe1 C26 152.7(3) . . ? C3 Fe1 C26 166.7(3) . . ? C24 Fe1 C26 67.07(13) . . ? C23 Fe1 C25 67.47(12) . . ? C1 Fe1 C25 106.1(2) . . ? C4 Fe1 C25 165.8(3) . . ? C22 Fe1 C25 67.24(13) . . ? C5 Fe1 C25 126.8(3) . . ? C2 Fe1 C25 117.2(2) . . ? C3 Fe1 C25 151.5(3) . . ? C24 Fe1 C25 39.76(9) . . ? C26 Fe1 C25 39.57(10) . . ? C2 C1 C5 108.3(4) . . ? C2 C1 Fe1 70.3(2) . . ? C5 C1 Fe1 69.8(2) . . ? C3 C2 C1 108.2(4) . . ? C3 C2 Fe1 69.9(3) . . ? C1 C2 Fe1 68.8(2) . . ? C2 C3 C4 108.4(4) . . ? C2 C3 Fe1 69.7(3) . . ? C4 C3 Fe1 68.9(3) . . ? C3 C4 C5 108.4(4) . . ? C3 C4 Fe1 70.1(2) . . ? C5 C4 Fe1 69.9(2) . . ? C4 C5 C6 132.7(4) . . ? C4 C5 C1 106.7(4) . . ? C6 C5 C1 119.9(4) . . ? C4 C5 Fe1 69.0(2) . . ? C6 C5 Fe1 120.2(3) . . ? C1 C5 Fe1 68.5(2) . . ? C7 C6 C5 128.3(4) . . ? C6 C7 C8 125.2(4) . . ? C6 C7 C11 128.4(4) . . ? C8 C7 C11 106.3(4) . . ? C9 C8 C7 111.1(4) . . ? C8 C9 C10 108.2(4) . . ? C8 C9 C17 126.3(4) . . ? C10 C9 C17 125.5(4) . . ? C16 C10 C9 119.9(4) . . ? C16 C10 C11 131.6(4) . . ? C9 C10 C11 108.4(3) . . ? C12 C11 C10 125.6(4) . . ? C12 C11 C7 128.4(4) . . ? C10 C11 C7 106.0(3) . . ? C11 C12 C13 124.6(4) . . ? C11 C12 C18 121.9(4) . . ? C13 C12 C18 113.5(4) . . ? C14 C13 C12 132.7(4) . . ? C13 C14 C15 131.0(4) . . ? C16 C15 C14 123.7(4) . . ? C16 C15 C19 121.3(4) . . ? C14 C15 C19 115.0(4) . . ? C15 C16 C10 129.9(4) . . ? C20 C19 C15 115.3(4) . . ? C20 C19 C21 110.8(4) . . ? C15 C19 C21 108.5(4) . . ? C26 C22 C23 108.0 . . ? C26 C22 Fe1 71.7(2) . . ? C23 C22 Fe1 69.1(2) . . ? C22 C23 C24 108.0 . . ? C22 C23 Fe1 70.1(2) . . ? C24 C23 Fe1 71.2(2) . . ? C25 C24 C23 108.0 . . ? C25 C24 Fe1 71.5(2) . . ? C23 C24 Fe1 68.3(2) . . ? C26 C25 C24 108.0 . . ? C26 C25 Fe1 69.6(2) . . ? C24 C25 Fe1 68.7(2) . . ? C25 C26 C22 108.0 . . ? C25 C26 Fe1 70.8(2) . . ? C22 C26 Fe1 68.2(2) . . ? C26 C22 C23 108.0 . . ? C24 C23 C22 108.0 . . ? C23 C24 C25 108.0 . . ? C26 C25 C24 108.0 . . ? C22 C26 C25 108.0 . . ? C23A Fe1A C22A 41.51(15) . . ? C23A Fe1A C24A 41.49(15) . . ? C22A Fe1A C24A 69.94(19) . . ? C23A Fe1A C26A 69.9(2) . . ? C22A Fe1A C26A 41.49(15) . . ? C24A Fe1A C26A 69.91(19) . . ? C23A Fe1A C25A 69.92(19) . . ? C22A Fe1A C25A 69.92(19) . . ? C24A Fe1A C25A 41.46(15) . . ? C26A Fe1A C25A 41.46(15) . . ? C23A Fe1A C2A 157.8(11) . . ? C22A Fe1A C2A 119.2(11) . . ? C24A Fe1A C2A 156.8(11) . . ? C26A Fe1A C2A 102.1(11) . . ? C25A Fe1A C2A 118.5(11) . . ? C23A Fe1A C3A 161.6(11) . . ? C22A Fe1A C3A 153.7(12) . . ? C24A Fe1A C3A 122.3(11) . . ? C26A Fe1A C3A 116.7(12) . . ? C25A Fe1A C3A 103.1(11) . . ? C2A Fe1A C3A 40.5 . . ? C23A Fe1A C1A 124.9(11) . . ? C22A Fe1A C1A 107.5(11) . . ? C24A Fe1A C1A 161.9(12) . . ? C26A Fe1A C1A 120.8(12) . . ? C25A Fe1A C1A 155.9(12) . . ? C2A Fe1A C1A 40.5 . . ? C3A Fe1A C1A 68.2 . . ? C23A Fe1A C4A 127.5(11) . . ? C22A Fe1A C4A 164.1(12) . . ? C24A Fe1A C4A 109.1(11) . . ? C26A Fe1A C4A 154.1(12) . . ? C25A Fe1A C4A 120.5(12) . . ? C2A Fe1A C4A 68.2 . . ? C3A Fe1A C4A 40.5 . . ? C1A Fe1A C4A 68.2 . . ? C23A Fe1A C5A 112.0(11) . . ? C22A Fe1A C5A 126.4(12) . . ? C24A Fe1A C5A 125.8(12) . . ? C26A Fe1A C5A 159.7(12) . . ? C25A Fe1A C5A 158.8(12) . . ? C2A Fe1A C5A 68.2 . . ? C3A Fe1A C5A 68.2 . . ? C1A Fe1A C5A 40.5 . . ? C4A Fe1A C5A 40.5 . . ? C2A C1A C5A 108.0 . . ? C2A C1A Fe1A 69.7 . . ? C5A C1A Fe1A 69.7 . . ? C1A C2A C3A 108.0 . . ? C1A C2A Fe1A 69.7 . . ? C3A C2A Fe1A 69.7 . . ? C4A C3A C2A 108.0 . . ? C4A C3A Fe1A 69.7 . . ? C2A C3A Fe1A 69.7 . . ? C3A C4A C5A 108.0 . . ? C3A C4A Fe1A 69.7 . . ? C5A C4A Fe1A 69.7 . . ? C6A C5A C4A 127(2) . . ? C6A C5A C1A 125(2) . . ? C4A C5A C1A 108.0 . . ? C6A C5A Fe1A 123.0(16) . . ? C4A C5A Fe1A 69.7 . . ? C1A C5A Fe1A 69.7 . . ? C7A C6A C5A 131(2) . . ? C6A C7A C8A 123.2(19) . . ? C6A C7A C11A 128.0(18) . . ? C8A C7A C11A 108.0 . . ? C9A C8A C7A 108.0 . . ? C8A C9A C10A 108.0 . . ? C8A C9A C17A 124.1(17) . . ? C10A C9A C17A 127.4(17) . . ? C16A C10A C11A 130.2(17) . . ? C16A C10A C9A 121.8(17) . . ? C11A C10A C9A 108.0 . . ? C12A C11A C10A 123.5(16) . . ? C12A C11A C7A 128.5(16) . . ? C10A C11A C7A 108.0 . . ? C11A C12A C13A 130(2) . . ? C11A C12A C18A 121.0(19) . . ? C13A C12A C18A 108.5(17) . . ? C12A C13A C14A 131(2) . . ? C15A C14A C13A 129(2) . . ? C14A C15A C16A 123(2) . . ? C14A C15A C19A 117.1(19) . . ? C16A C15A C19A 119.4(17) . . ? C10A C16A C15A 133(2) . . ? C15A C19A C20A 115(2) . . ? C15A C19A C21A 109(2) . . ? C20A C19A C21A 120(2) . . ? C23A C22A C26A 108.0 . . ? C23A C22A Fe1A 69.2(3) . . ? C26A C22A Fe1A 69.3(3) . . ? C22A C23A C24A 108.0 . . ? C22A C23A Fe1A 69.2(3) . . ? C24A C23A Fe1A 69.3(3) . . ? C23A C24A C25A 108.0 . . ? C23A C24A Fe1A 69.2(3) . . ? C25A C24A Fe1A 69.3(3) . . ? C26A C25A C24A 108.0 . . ? C26A C25A Fe1A 69.2(3) . . ? C24A C25A Fe1A 69.2(3) . . ? C25A C26A C22A 108.0 . . ? C25A C26A Fe1A 69.3(3) . . ? C22A C26A Fe1A 69.2(3) . . ? F1 B1 F4 109.52(6) . . ? F1 B1 F3 109.46(6) . . ? F4 B1 F3 109.47(6) . . ? F1 B1 F2 109.53(6) . . ? F4 B1 F2 109.46(6) . . ? F3 B1 F2 109.39(6) . . ? F1A B2 F23 109.48(7) . . ? F1A B2 F34 109.48(7) . . ? F23 B2 F34 109.47(7) . . ? F1A B2 F24 109.46(6) . . ? F23 B2 F24 109.47(7) . . ? F34 B2 F24 109.46(7) . . ? O1 O1 C27 107(4) 2_656 2_656 ? O1 O1 C27 50(4) 2_656 . ? C27 O1 C27 84(3) 2_656 . ? O1 O1 C30 98(7) 2_656 . ? C27 O1 C30 36(2) 2_656 . ? C27 O1 C30 105(2) . . ? O1 O1 C30 61(6) 2_656 2_656 ? C27 O1 C30 108(2) 2_656 2_656 ? C27 O1 C30 31.0(13) . 2_656 ? C30 O1 C30 135.2(19) . 2_656 ? C30 C27 O1 91(2) 2_656 2_656 ? C30 C27 C29 94(4) 2_656 2_656 ? O1 C27 C29 154(4) 2_656 2_656 ? C30 C27 O1 87(4) 2_656 . ? O1 C27 O1 23(2) 2_656 . ? C29 C27 O1 132(2) 2_656 . ? C30 C27 C28 125(4) 2_656 . ? O1 C27 C28 122(3) 2_656 . ? C29 C27 C28 38.2(13) 2_656 . ? O1 C27 C28 106.3(19) . . ? C30 C27 C27 120(4) 2_656 2_656 ? O1 C27 C27 55(2) 2_656 2_656 ? C29 C27 C27 101.0(17) 2_656 2_656 ? O1 C27 C27 41.2(13) . 2_656 ? C28 C27 C27 67.0(15) . 2_656 ? C30 C27 C28 138(4) 2_656 2_656 ? O1 C27 C28 105(3) 2_656 2_656 ? C29 C27 C28 56.8(9) 2_656 2_656 ? O1 C27 C28 92.2(17) . 2_656 ? C28 C27 C28 18.6(8) . 2_656 ? C27 C27 C28 51.2(11) 2_656 2_656 ? C28 C28 C29 161(3) 2_656 2_656 ? C28 C28 C27 107(2) 2_656 . ? C29 C28 C27 53(2) 2_656 . ? C28 C28 C29 12(2) 2_656 . ? C29 C28 C29 151(3) 2_656 . ? C27 C28 C29 97.7(18) . . ? C28 C28 C27 54(2) 2_656 2_656 ? C29 C28 C27 110(2) 2_656 2_656 ? C27 C28 C27 62(2) . 2_656 ? C29 C28 C27 42.2(17) . 2_656 ? C28 C29 C27 88(2) 2_656 2_656 ? C28 C29 C30 116(3) 2_656 . ? C27 C29 C30 33(2) 2_656 . ? C28 C29 C28 7.5(12) 2_656 . ? C27 C29 C28 81(2) 2_656 . ? C30 C29 C28 109(2) . . ? C27 C30 O1 53(3) 2_656 . ? C27 C30 C29 53(3) 2_656 . ? O1 C30 C29 102.8(18) . . ? C27 C30 O1 62(4) 2_656 2_656 ? O1 C30 O1 21.1(19) . 2_656 ? C29 C30 O1 101(2) . 2_656 ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.834 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.094 #============================================================================ data_guazru _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C31 H32 B2 F8 Fe Ru' _chemical_formula_sum 'C32 H35 B2 F8 Fe N O2 Ru' _chemical_formula_weight 796.15 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' 'B' 'B' 0.0013 0.0007 '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' 'Fe' 'Fe' 0.3463 0.8444 '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5080(7) _cell_length_b 13.3829(8) _cell_length_c 16.0531(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.941(5) _cell_angle_gamma 90.00 _cell_volume 3307.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.971 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7092 _exptl_absorpt_correction_T_max 0.8370 _exptl_special_details ; Crystals were grown from CH3NO2/Et2O diffusion ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24975 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.81 _reflns_number_total 6223 _reflns_number_gt 3917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'XRED (Stoe, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6223 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.918 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.00636(3) 0.38904(3) 0.23887(3) 0.03226(15) Uani 1 d . . . Fe1 Fe -0.43501(4) 0.38948(5) 0.21228(4) 0.03061(19) Uani 1 d . . . C1 C -0.3981(4) 0.2867(4) 0.3030(3) 0.0340(12) Uani 1 d . . . H1 H -0.3658 0.3000 0.3560 0.041 Uiso 1 calc R . . C2 C -0.4901(4) 0.2870(4) 0.2849(4) 0.0374(13) Uani 1 d . . . H2 H -0.5300 0.3000 0.3240 0.045 Uiso 1 calc R . . C3 C -0.5119(4) 0.2648(4) 0.1997(4) 0.0389(13) Uani 1 d . . . H3 H -0.5692 0.2605 0.1714 0.047 Uiso 1 calc R . . C4 C -0.4349(3) 0.2501(4) 0.1630(4) 0.0330(12) Uani 1 d . . . H4 H -0.4313 0.2346 0.1058 0.040 Uiso 1 calc R . . C5 C -0.3629(3) 0.2625(3) 0.2271(3) 0.0295(11) Uani 1 d . . . C6 C -0.2747(3) 0.2641(3) 0.2056(3) 0.0289(11) Uani 1 d . . . H6 H -0.2692 0.2602 0.1474 0.035 Uiso 1 calc R . . C7 C -0.1989(3) 0.2702(3) 0.2577(3) 0.0294(11) Uani 1 d . . . C8 C -0.1899(4) 0.2652(4) 0.3484(3) 0.0349(12) Uani 1 d . . . H8 H -0.2373 0.2640 0.3808 0.042 Uiso 1 calc R . . C9 C -0.1050(4) 0.2624(4) 0.3811(3) 0.0350(12) Uani 1 d . . . C10 C -0.0525(3) 0.2624(3) 0.3124(3) 0.0314(12) Uani 1 d . . . C11 C -0.1098(3) 0.2696(3) 0.2343(3) 0.0311(11) Uani 1 d . . . C12 C -0.0843(4) 0.2862(4) 0.1536(3) 0.0354(12) Uani 1 d . . . C13 C 0.0035(4) 0.2803(4) 0.1337(4) 0.0406(13) Uani 1 d . . . H13 H 0.0086 0.2860 0.0755 0.049 Uiso 1 calc R . . C14 C 0.0822(4) 0.2680(4) 0.1838(4) 0.0480(15) Uani 1 d . . . H14 H 0.1309 0.2628 0.1534 0.058 Uiso 1 calc R . . C15 C 0.1027(3) 0.2617(4) 0.2713(4) 0.0395(14) Uani 1 d . . . C16 C 0.0394(4) 0.2631(4) 0.3275(4) 0.0368(13) Uani 1 d . . . H16 H 0.0622 0.2647 0.3852 0.044 Uiso 1 calc R . . C17 C -0.0702(5) 0.2573(6) 0.4722(4) 0.0557(17) Uani 1 d . . . H17A H -0.0066 0.2556 0.4779 0.083 Uiso 1 calc R . . H17B H -0.0918 0.1967 0.4970 0.083 Uiso 1 calc R . . H17C H -0.0894 0.3161 0.5013 0.083 Uiso 1 calc R . . C18 C -0.1478(4) 0.3169(5) 0.0794(3) 0.0455(14) Uani 1 d . . . H18A H -0.1169 0.3247 0.0300 0.068 Uiso 1 calc R . . H18B H -0.1750 0.3804 0.0916 0.068 Uiso 1 calc R . . H18C H -0.1926 0.2654 0.0684 0.068 Uiso 1 calc R . . C19 C 0.1968(4) 0.2611(5) 0.3121(5) 0.0615(19) Uani 1 d . . . H19 H 0.1990 0.3023 0.3643 0.074 Uiso 1 calc R . . C20 C 0.2205(6) 0.1558(8) 0.3391(9) 0.135(5) Uani 1 d . . . H20A H 0.2808 0.1542 0.3659 0.203 Uiso 1 calc R . . H20B H 0.2145 0.1118 0.2899 0.203 Uiso 1 calc R . . H20C H 0.1818 0.1328 0.3791 0.203 Uiso 1 calc R . . C21 C 0.2606(5) 0.3102(12) 0.2559(8) 0.138(5) Uani 1 d . . . H21A H 0.2411 0.3783 0.2411 0.207 Uiso 1 calc R . . H21B H 0.2615 0.2707 0.2046 0.207 Uiso 1 calc R . . H21C H 0.3191 0.3124 0.2867 0.207 Uiso 1 calc R . . C22 C -0.3977(6) 0.5281(4) 0.2553(5) 0.065(2) Uani 1 d . . . H22 H -0.3664 0.5414 0.3087 0.078 Uiso 1 calc R . . C23 C -0.3638(5) 0.5110(5) 0.1825(6) 0.068(2) Uani 1 d . . . H23 H -0.3035 0.5115 0.1768 0.081 Uiso 1 calc R . . C24 C -0.4278(7) 0.4932(5) 0.1189(5) 0.076(3) Uani 1 d . . . H24 H -0.4197 0.4791 0.0624 0.092 Uiso 1 calc R . . C25 C -0.5065(6) 0.4989(5) 0.1499(6) 0.070(2) Uani 1 d . . . H25 H -0.5620 0.4891 0.1188 0.084 Uiso 1 calc R . . C26 C -0.4904(4) 0.5218(3) 0.2354(4) 0.072(3) Uani 1 d . . . H26 H -0.5326 0.5313 0.2730 0.087 Uiso 1 calc R . . C27 C 0.0147(4) 0.5165(3) 0.3223(4) 0.067(2) Uani 1 d R . . H27 H 0.0176 0.5097 0.3814 0.081 Uiso 1 calc R . . C28 C 0.0839(5) 0.5181(5) 0.2798(6) 0.065(2) Uani 1 d . . . H28 H 0.1429 0.5134 0.3038 0.079 Uiso 1 calc R . . C29 C 0.0552(8) 0.5277(5) 0.1946(6) 0.083(3) Uani 1 d . . . H29 H 0.0896 0.5305 0.1495 0.100 Uiso 1 calc R . . C30 C -0.0384(9) 0.5324(5) 0.1898(7) 0.103(4) Uani 1 d . . . H30 H -0.0783 0.5388 0.1403 0.124 Uiso 1 calc R . . C31 C -0.0586(5) 0.5258(5) 0.2707(8) 0.084(3) Uani 1 d . . . H31 H -0.1155 0.5276 0.2870 0.101 Uiso 1 calc R . . C32A C -0.3729(7) 0.4241(6) 0.4997(6) 0.093(3) Uani 0.50 d P A 1 H32A H -0.4010 0.4578 0.4493 0.139 Uiso 0.50 calc PR A 1 H32B H -0.4027 0.3608 0.5075 0.139 Uiso 0.50 calc PR A 1 H32C H -0.3120 0.4109 0.4931 0.139 Uiso 0.50 calc PR A 1 N1A N -0.3776(13) 0.4878(15) 0.5726(15) 0.100(5) Uiso 0.50 d P A 1 O1A O -0.3508(11) 0.4700(12) 0.6401(11) 0.117(5) Uiso 0.50 d P A 1 O2A O -0.4112(11) 0.5829(14) 0.5442(13) 0.114(5) Uiso 0.50 d P A 1 C32B C -0.3729(7) 0.4241(6) 0.4997(6) 0.093(3) Uani 0.50 d P B 2 H32D H -0.3755 0.4246 0.4384 0.139 Uiso 0.50 calc PR B 2 H32E H -0.4125 0.3730 0.5167 0.139 Uiso 0.50 calc PR B 2 H32F H -0.3135 0.4091 0.5245 0.139 Uiso 0.50 calc PR B 2 N1B N -0.3990(11) 0.5234(14) 0.5289(11) 0.080(4) Uiso 0.50 d P B 2 O1B O -0.4008(11) 0.5457(14) 0.5973(11) 0.111(5) Uiso 0.50 d P B 2 O2B O -0.4271(11) 0.5874(12) 0.4757(12) 0.121(5) Uiso 0.50 d P B 2 B1 B -0.1747(6) 0.5703(7) 0.4806(5) 0.064(2) Uani 1 d . . . F1 F -0.2038(3) 0.5302(4) 0.5494(3) 0.0988(17) Uani 1 d . . . F2 F -0.0892(4) 0.5436(5) 0.4789(4) 0.117(2) Uani 1 d . . . F3 F -0.2181(4) 0.5496(5) 0.4061(3) 0.118(2) Uani 1 d . . . F4 F -0.1668(4) 0.6757(4) 0.4922(3) 0.0940(15) Uani 1 d . . . F5 F 0.2098(3) 0.4250(4) -0.0683(3) 0.0878(15) Uani 1 d . . . F6A F 0.1637(10) 0.3040(8) 0.0050(7) 0.087(4) Uiso 0.519(17) d P C 1 F7A F 0.2742(14) 0.4304(14) 0.0501(12) 0.169(8) Uiso 0.519(17) d P C 1 F8A F 0.1322(9) 0.4639(10) 0.0336(7) 0.096(4) Uiso 0.519(17) d P C 1 B2A B 0.2106(11) 0.4079(9) 0.0219(9) 0.020(3) Uiso 0.519(17) d P C 1 F6B F 0.0981(9) 0.4240(10) 0.0086(8) 0.095(4) Uiso 0.481(17) d P C 2 F7B F 0.2092(9) 0.3001(7) 0.0255(7) 0.073(3) Uiso 0.481(17) d P C 2 F8B F 0.2155(12) 0.4381(12) 0.0869(11) 0.138(7) Uiso 0.481(17) d P C 2 B2B B 0.1873(12) 0.4000(11) 0.0085(10) 0.025(4) Uiso 0.481(17) d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0274(2) 0.0243(2) 0.0451(3) -0.0033(2) 0.00404(18) 0.00177(18) Fe1 0.0284(4) 0.0234(3) 0.0388(4) 0.0041(3) -0.0010(3) 0.0011(3) C1 0.035(3) 0.035(3) 0.032(3) 0.006(2) 0.003(2) 0.001(2) C2 0.031(3) 0.030(3) 0.052(4) 0.007(2) 0.010(3) 0.002(2) C3 0.028(3) 0.026(3) 0.060(4) -0.001(3) -0.005(3) -0.005(2) C4 0.031(3) 0.025(2) 0.040(3) -0.007(2) -0.006(2) 0.000(2) C5 0.029(3) 0.021(2) 0.037(3) 0.002(2) -0.003(2) 0.0018(19) C6 0.032(3) 0.023(2) 0.031(3) 0.0002(19) 0.001(2) 0.0042(19) C7 0.026(3) 0.025(2) 0.036(3) -0.002(2) -0.003(2) 0.000(2) C8 0.030(3) 0.040(3) 0.034(3) 0.003(2) 0.003(2) 0.000(2) C9 0.034(3) 0.033(3) 0.036(3) 0.002(2) -0.006(2) 0.001(2) C10 0.030(3) 0.018(2) 0.044(3) -0.001(2) -0.005(2) 0.0017(19) C11 0.030(3) 0.021(2) 0.040(3) -0.004(2) -0.001(2) 0.001(2) C12 0.035(3) 0.028(2) 0.043(3) -0.009(2) 0.007(3) -0.001(2) C13 0.038(3) 0.041(3) 0.044(3) -0.011(2) 0.011(3) 0.004(2) C14 0.033(3) 0.047(3) 0.065(4) -0.018(3) 0.007(3) 0.006(3) C15 0.022(3) 0.028(3) 0.068(4) -0.009(3) 0.004(3) 0.008(2) C16 0.031(3) 0.025(2) 0.050(3) 0.002(2) -0.013(3) 0.004(2) C17 0.048(4) 0.075(5) 0.040(3) 0.007(3) -0.012(3) -0.007(3) C18 0.037(3) 0.066(4) 0.034(3) 0.002(3) 0.003(3) -0.001(3) C19 0.028(3) 0.068(4) 0.085(5) -0.018(4) -0.008(4) 0.007(3) C20 0.063(6) 0.081(6) 0.242(15) -0.008(8) -0.063(8) 0.036(5) C21 0.029(5) 0.245(16) 0.140(10) -0.028(10) 0.012(6) -0.021(7) C22 0.100(6) 0.026(3) 0.063(5) 0.007(3) -0.019(4) -0.008(3) C23 0.061(5) 0.036(3) 0.108(7) 0.026(4) 0.017(5) -0.005(3) C24 0.119(8) 0.047(4) 0.066(5) 0.026(4) 0.022(6) 0.013(4) C25 0.071(5) 0.042(4) 0.090(6) 0.014(4) -0.023(5) 0.014(3) C26 0.095(6) 0.026(3) 0.106(7) 0.013(4) 0.051(5) 0.022(4) C27 0.110(7) 0.031(3) 0.064(5) -0.008(3) 0.024(5) -0.004(4) C28 0.047(4) 0.031(3) 0.114(7) -0.006(4) -0.007(4) -0.008(3) C29 0.153(10) 0.032(4) 0.075(6) -0.006(4) 0.053(6) -0.023(5) C30 0.149(10) 0.021(3) 0.112(8) 0.002(4) -0.091(8) 0.001(4) C31 0.057(5) 0.024(3) 0.177(11) -0.012(5) 0.034(6) 0.007(3) C32A 0.111(8) 0.064(5) 0.106(7) -0.027(5) 0.025(6) -0.016(5) C32B 0.111(8) 0.064(5) 0.106(7) -0.027(5) 0.025(6) -0.016(5) B1 0.072(6) 0.080(6) 0.040(4) 0.015(4) 0.012(4) 0.026(5) F1 0.090(4) 0.129(5) 0.076(3) 0.028(3) 0.008(3) -0.032(3) F2 0.079(4) 0.158(6) 0.116(4) 0.009(4) 0.018(3) 0.033(4) F3 0.131(5) 0.129(5) 0.083(4) 0.018(3) -0.032(4) -0.058(4) F4 0.115(4) 0.099(4) 0.068(3) 0.010(3) 0.013(3) 0.004(3) F5 0.081(3) 0.108(4) 0.082(3) 0.027(3) 0.039(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C30 2.156(7) . ? Ru1 C29 2.157(7) . ? Ru1 C28 2.161(6) . ? Ru1 C27 2.163(5) . ? Ru1 C31 2.180(6) . ? Ru1 C13 2.225(5) . ? Ru1 C16 2.226(5) . ? Ru1 C14 2.245(5) . ? Ru1 C15 2.284(5) . ? Ru1 C12 2.297(5) . ? Ru1 C10 2.315(5) . ? Ru1 C11 2.404(5) . ? Fe1 C26 2.022(5) . ? Fe1 C4 2.026(5) . ? Fe1 C25 2.027(7) . ? Fe1 C5 2.032(5) . ? Fe1 C1 2.035(5) . ? Fe1 C22 2.038(6) . ? Fe1 C3 2.046(5) . ? Fe1 C2 2.052(5) . ? Fe1 C23 2.055(6) . ? Fe1 C24 2.056(7) . ? C1 C2 1.421(8) . ? C1 C5 1.431(7) . ? C2 C3 1.400(8) . ? C3 C4 1.407(8) . ? C4 C5 1.434(8) . ? C5 C6 1.451(7) . ? C6 C7 1.360(7) . ? C7 C8 1.447(7) . ? C7 C11 1.474(7) . ? C8 C9 1.358(8) . ? C9 C10 1.449(7) . ? C9 C17 1.497(8) . ? C10 C16 1.416(7) . ? C10 C11 1.450(8) . ? C11 C12 1.417(7) . ? C12 C13 1.438(7) . ? C12 C18 1.508(8) . ? C13 C14 1.387(9) . ? C14 C15 1.405(9) . ? C15 C16 1.413(8) . ? C15 C19 1.525(9) . ? C19 C20 1.508(12) . ? C19 C21 1.562(13) . ? C22 C23 1.359(11) . ? C22 C26 1.437(10) . ? C23 C24 1.357(12) . ? C24 C25 1.374(12) . ? C25 C26 1.399(10) . ? C27 C31 1.328(12) . ? C27 C28 1.340(9) . ? C28 C29 1.392(12) . ? C29 C30 1.446(14) . ? C30 C31 1.375(14) . ? C32A N1A 1.46(2) . ? N1A O1A 1.14(2) . ? N1A O2A 1.43(3) . ? N1B O1B 1.14(2) . ? N1B O2B 1.25(2) . ? B1 F3 1.329(10) . ? B1 F1 1.353(9) . ? B1 F2 1.377(10) . ? B1 F4 1.426(11) . ? F5 B2B 1.363(14) . ? F5 B2A 1.463(13) . ? F6A B2A 1.578(19) . ? F7A B2A 1.08(2) . ? F8A B2A 1.460(18) . ? F6B B2B 1.42(2) . ? F7B B2B 1.398(17) . ? F8B B2B 1.38(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 Ru1 C29 39.2(4) . . ? C30 Ru1 C28 62.8(3) . . ? C29 Ru1 C28 37.6(3) . . ? C30 Ru1 C27 61.1(3) . . ? C29 Ru1 C27 61.9(3) . . ? C28 Ru1 C27 36.1(3) . . ? C30 Ru1 C31 37.0(4) . . ? C29 Ru1 C31 63.0(3) . . ? C28 Ru1 C31 60.9(3) . . ? C27 Ru1 C31 35.6(3) . . ? C30 Ru1 C13 109.2(3) . . ? C29 Ru1 C13 106.7(3) . . ? C28 Ru1 C13 135.4(3) . . ? C27 Ru1 C13 168.4(2) . . ? C31 Ru1 C13 139.4(4) . . ? C30 Ru1 C16 161.1(4) . . ? C29 Ru1 C16 143.1(4) . . ? C28 Ru1 C16 109.5(3) . . ? C27 Ru1 C16 102.1(2) . . ? C31 Ru1 C16 124.3(4) . . ? C13 Ru1 C16 88.4(2) . . ? C30 Ru1 C14 131.2(4) . . ? C29 Ru1 C14 105.6(3) . . ? C28 Ru1 C14 113.4(3) . . ? C27 Ru1 C14 144.9(2) . . ? C31 Ru1 C14 167.8(3) . . ? C13 Ru1 C14 36.1(2) . . ? C16 Ru1 C14 67.3(2) . . ? C30 Ru1 C15 156.9(4) . . ? C29 Ru1 C15 118.1(3) . . ? C28 Ru1 C15 101.7(2) . . ? C27 Ru1 C15 117.3(2) . . ? C31 Ru1 C15 151.8(4) . . ? C13 Ru1 C15 68.7(2) . . ? C16 Ru1 C15 36.5(2) . . ? C14 Ru1 C15 36.1(2) . . ? C30 Ru1 C12 99.7(3) . . ? C29 Ru1 C12 122.2(3) . . ? C28 Ru1 C12 159.7(3) . . ? C27 Ru1 C12 145.9(2) . . ? C31 Ru1 C12 112.1(3) . . ? C13 Ru1 C12 37.05(19) . . ? C16 Ru1 C12 90.2(2) . . ? C14 Ru1 C12 69.2(2) . . ? C15 Ru1 C12 91.4(2) . . ? C30 Ru1 C10 135.1(5) . . ? C29 Ru1 C10 166.8(2) . . ? C28 Ru1 C10 132.0(3) . . ? C27 Ru1 C10 105.04(18) . . ? C31 Ru1 C10 105.9(3) . . ? C13 Ru1 C10 86.3(2) . . ? C16 Ru1 C10 36.27(19) . . ? C14 Ru1 C10 86.0(2) . . ? C15 Ru1 C10 67.99(19) . . ? C12 Ru1 C10 67.34(19) . . ? C30 Ru1 C11 111.9(4) . . ? C29 Ru1 C11 148.7(4) . . ? C28 Ru1 C11 158.2(3) . . ? C27 Ru1 C11 122.14(19) . . ? C31 Ru1 C11 101.5(2) . . ? C13 Ru1 C11 66.18(19) . . ? C16 Ru1 C11 68.23(19) . . ? C14 Ru1 C11 86.2(2) . . ? C15 Ru1 C11 88.74(18) . . ? C12 Ru1 C11 35.00(18) . . ? C10 Ru1 C11 35.72(18) . . ? C26 Fe1 C4 153.9(2) . . ? C26 Fe1 C25 40.4(3) . . ? C4 Fe1 C25 119.9(3) . . ? C26 Fe1 C5 161.9(2) . . ? C4 Fe1 C5 41.4(2) . . ? C25 Fe1 C5 157.3(3) . . ? C26 Fe1 C1 123.3(2) . . ? C4 Fe1 C1 69.1(2) . . ? C25 Fe1 C1 158.7(3) . . ? C5 Fe1 C1 41.2(2) . . ? C26 Fe1 C22 41.4(3) . . ? C4 Fe1 C22 163.0(3) . . ? C25 Fe1 C22 68.0(3) . . ? C5 Fe1 C22 126.3(3) . . ? C1 Fe1 C22 109.2(3) . . ? C26 Fe1 C3 118.5(2) . . ? C4 Fe1 C3 40.4(2) . . ? C25 Fe1 C3 105.3(3) . . ? C5 Fe1 C3 68.6(2) . . ? C1 Fe1 C3 68.3(2) . . ? C22 Fe1 C3 156.0(3) . . ? C26 Fe1 C2 105.4(2) . . ? C4 Fe1 C2 68.1(2) . . ? C25 Fe1 C2 121.6(3) . . ? C5 Fe1 C2 68.6(2) . . ? C1 Fe1 C2 40.7(2) . . ? C22 Fe1 C2 122.4(3) . . ? C3 Fe1 C2 40.0(2) . . ? C26 Fe1 C23 66.6(3) . . ? C4 Fe1 C23 127.7(3) . . ? C25 Fe1 C23 65.8(3) . . ? C5 Fe1 C23 112.7(3) . . ? C1 Fe1 C23 126.1(3) . . ? C22 Fe1 C23 38.8(3) . . ? C3 Fe1 C23 161.0(3) . . ? C2 Fe1 C23 159.0(3) . . ? C26 Fe1 C24 66.7(3) . . ? C4 Fe1 C24 109.5(3) . . ? C25 Fe1 C24 39.3(3) . . ? C5 Fe1 C24 124.9(3) . . ? C1 Fe1 C24 160.6(3) . . ? C22 Fe1 C24 66.1(3) . . ? C3 Fe1 C24 124.1(3) . . ? C2 Fe1 C24 158.2(4) . . ? C23 Fe1 C24 38.6(3) . . ? C2 C1 C5 107.6(5) . . ? C2 C1 Fe1 70.3(3) . . ? C5 C1 Fe1 69.3(3) . . ? C3 C2 C1 108.5(5) . . ? C3 C2 Fe1 69.8(3) . . ? C1 C2 Fe1 69.0(3) . . ? C2 C3 C4 108.8(5) . . ? C2 C3 Fe1 70.3(3) . . ? C4 C3 Fe1 69.0(3) . . ? C3 C4 C5 108.0(5) . . ? C3 C4 Fe1 70.5(3) . . ? C5 C4 Fe1 69.5(3) . . ? C1 C5 C4 107.1(5) . . ? C1 C5 C6 131.8(5) . . ? C4 C5 C6 120.4(5) . . ? C1 C5 Fe1 69.5(3) . . ? C4 C5 Fe1 69.1(3) . . ? C6 C5 Fe1 118.8(3) . . ? C7 C6 C5 128.6(5) . . ? C6 C7 C8 125.9(5) . . ? C6 C7 C11 127.6(5) . . ? C8 C7 C11 106.1(5) . . ? C9 C8 C7 111.2(5) . . ? C8 C9 C10 108.3(5) . . ? C8 C9 C17 126.7(5) . . ? C10 C9 C17 125.0(5) . . ? C16 C10 C9 121.1(5) . . ? C16 C10 C11 130.3(5) . . ? C9 C10 C11 108.4(4) . . ? C16 C10 Ru1 68.4(3) . . ? C9 C10 Ru1 133.0(3) . . ? C11 C10 Ru1 75.5(3) . . ? C12 C11 C10 126.2(5) . . ? C12 C11 C7 127.3(5) . . ? C10 C11 C7 106.0(4) . . ? C12 C11 Ru1 68.4(3) . . ? C10 C11 Ru1 68.8(3) . . ? C7 C11 Ru1 135.3(3) . . ? C11 C12 C13 124.8(5) . . ? C11 C12 C18 122.5(5) . . ? C13 C12 C18 112.6(5) . . ? C11 C12 Ru1 76.6(3) . . ? C13 C12 Ru1 68.7(3) . . ? C18 C12 Ru1 127.0(4) . . ? C14 C13 C12 131.9(6) . . ? C14 C13 Ru1 72.7(3) . . ? C12 C13 Ru1 74.2(3) . . ? C13 C14 C15 131.6(5) . . ? C13 C14 Ru1 71.1(3) . . ? C15 C14 Ru1 73.5(3) . . ? C14 C15 C16 123.2(5) . . ? C14 C15 C19 121.3(5) . . ? C16 C15 C19 115.3(6) . . ? C14 C15 Ru1 70.4(3) . . ? C16 C15 Ru1 69.5(3) . . ? C19 C15 Ru1 131.8(4) . . ? C15 C16 C10 130.8(6) . . ? C15 C16 Ru1 74.0(3) . . ? C10 C16 Ru1 75.3(3) . . ? C20 C19 C15 108.4(6) . . ? C20 C19 C21 114.2(8) . . ? C15 C19 C21 112.9(7) . . ? C23 C22 C26 106.3(6) . . ? C23 C22 Fe1 71.3(4) . . ? C26 C22 Fe1 68.7(3) . . ? C24 C23 C22 110.6(7) . . ? C24 C23 Fe1 70.8(4) . . ? C22 C23 Fe1 69.9(4) . . ? C23 C24 C25 108.6(8) . . ? C23 C24 Fe1 70.7(4) . . ? C25 C24 Fe1 69.2(4) . . ? C24 C25 C26 107.9(7) . . ? C24 C25 Fe1 71.5(4) . . ? C26 C25 Fe1 69.6(4) . . ? C25 C26 C22 106.6(6) . . ? C25 C26 Fe1 70.0(3) . . ? C22 C26 Fe1 69.9(3) . . ? C31 C27 C28 111.1(7) . . ? C31 C27 Ru1 72.9(4) . . ? C28 C27 Ru1 71.9(4) . . ? C27 C28 C29 108.7(7) . . ? C27 C28 Ru1 72.0(4) . . ? C29 C28 Ru1 71.0(4) . . ? C28 C29 C30 104.8(7) . . ? C28 C29 Ru1 71.4(4) . . ? C30 C29 Ru1 70.4(4) . . ? C31 C30 C29 106.8(7) . . ? C31 C30 Ru1 72.4(4) . . ? C29 C30 Ru1 70.4(4) . . ? C27 C31 C30 108.6(8) . . ? C27 C31 Ru1 71.5(3) . . ? C30 C31 Ru1 70.6(4) . . ? O1A N1A O2A 125(2) . . ? O1A N1A C32A 127(2) . . ? O2A N1A C32A 108(2) . . ? O1B N1B O2B 116(2) . . ? F3 B1 F1 118.0(9) . . ? F3 B1 F2 108.2(7) . . ? F1 B1 F2 109.3(7) . . ? F3 B1 F4 110.5(7) . . ? F1 B1 F4 108.6(7) . . ? F2 B1 F4 101.0(8) . . ? B2B F5 B2A 16.3(7) . . ? F7A B2A F8A 122.5(16) . . ? F7A B2A F5 105.7(14) . . ? F8A B2A F5 98.0(10) . . ? F7A B2A F6A 134.3(16) . . ? F8A B2A F6A 95.7(12) . . ? F5 B2A F6A 91.1(10) . . ? F5 B2B F8B 130.3(15) . . ? F5 B2B F7B 109.2(10) . . ? F8B B2B F7B 97.6(13) . . ? F5 B2B F6B 107.5(12) . . ? F8B B2B F6B 96.8(12) . . ? F7B B2B F6B 115.5(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C26 Fe1 C1 C2 73.9(4) . . . . ? C4 Fe1 C1 C2 -80.2(3) . . . . ? C25 Fe1 C1 C2 39.2(9) . . . . ? C5 Fe1 C1 C2 -118.6(5) . . . . ? C22 Fe1 C1 C2 117.8(4) . . . . ? C3 Fe1 C1 C2 -36.7(3) . . . . ? C23 Fe1 C1 C2 157.6(4) . . . . ? C24 Fe1 C1 C2 -169.9(9) . . . . ? C26 Fe1 C1 C5 -167.4(3) . . . . ? C4 Fe1 C1 C5 38.4(3) . . . . ? C25 Fe1 C1 C5 157.9(7) . . . . ? C22 Fe1 C1 C5 -123.6(4) . . . . ? C3 Fe1 C1 C5 82.0(3) . . . . ? C2 Fe1 C1 C5 118.6(5) . . . . ? C23 Fe1 C1 C5 -83.7(4) . . . . ? C24 Fe1 C1 C5 -51.2(10) . . . . ? C5 C1 C2 C3 -0.7(6) . . . . ? Fe1 C1 C2 C3 58.8(4) . . . . ? C5 C1 C2 Fe1 -59.4(3) . . . . ? C26 Fe1 C2 C3 116.2(4) . . . . ? C4 Fe1 C2 C3 -37.2(3) . . . . ? C25 Fe1 C2 C3 75.4(4) . . . . ? C5 Fe1 C2 C3 -81.8(3) . . . . ? C1 Fe1 C2 C3 -120.2(5) . . . . ? C22 Fe1 C2 C3 157.9(4) . . . . ? C23 Fe1 C2 C3 -179.6(7) . . . . ? C24 Fe1 C2 C3 50.7(9) . . . . ? C26 Fe1 C2 C1 -123.6(3) . . . . ? C4 Fe1 C2 C1 83.1(3) . . . . ? C25 Fe1 C2 C1 -164.4(4) . . . . ? C5 Fe1 C2 C1 38.4(3) . . . . ? C22 Fe1 C2 C1 -81.9(4) . . . . ? C3 Fe1 C2 C1 120.2(5) . . . . ? C23 Fe1 C2 C1 -59.3(8) . . . . ? C24 Fe1 C2 C1 170.9(7) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? Fe1 C2 C3 C4 58.4(4) . . . . ? C1 C2 C3 Fe1 -58.3(4) . . . . ? C26 Fe1 C3 C2 -79.8(4) . . . . ? C4 Fe1 C3 C2 120.2(5) . . . . ? C25 Fe1 C3 C2 -121.3(4) . . . . ? C5 Fe1 C3 C2 81.8(3) . . . . ? C1 Fe1 C3 C2 37.3(3) . . . . ? C22 Fe1 C3 C2 -51.2(8) . . . . ? C23 Fe1 C3 C2 179.5(8) . . . . ? C24 Fe1 C3 C2 -159.7(4) . . . . ? C26 Fe1 C3 C4 159.9(3) . . . . ? C25 Fe1 C3 C4 118.5(4) . . . . ? C5 Fe1 C3 C4 -38.5(3) . . . . ? C1 Fe1 C3 C4 -82.9(4) . . . . ? C22 Fe1 C3 C4 -171.4(6) . . . . ? C2 Fe1 C3 C4 -120.2(5) . . . . ? C23 Fe1 C3 C4 59.3(9) . . . . ? C24 Fe1 C3 C4 80.1(5) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? Fe1 C3 C4 C5 59.6(3) . . . . ? C2 C3 C4 Fe1 -59.2(4) . . . . ? C26 Fe1 C4 C3 -43.4(6) . . . . ? C25 Fe1 C4 C3 -78.1(5) . . . . ? C5 Fe1 C4 C3 118.8(5) . . . . ? C1 Fe1 C4 C3 80.6(4) . . . . ? C22 Fe1 C4 C3 168.0(8) . . . . ? C2 Fe1 C4 C3 36.7(3) . . . . ? C23 Fe1 C4 C3 -159.3(4) . . . . ? C24 Fe1 C4 C3 -120.1(5) . . . . ? C26 Fe1 C4 C5 -162.2(4) . . . . ? C25 Fe1 C4 C5 163.1(4) . . . . ? C1 Fe1 C4 C5 -38.3(3) . . . . ? C22 Fe1 C4 C5 49.2(10) . . . . ? C3 Fe1 C4 C5 -118.8(5) . . . . ? C2 Fe1 C4 C5 -82.1(3) . . . . ? C23 Fe1 C4 C5 81.9(4) . . . . ? C24 Fe1 C4 C5 121.1(4) . . . . ? C2 C1 C5 C4 0.9(5) . . . . ? Fe1 C1 C5 C4 -59.1(3) . . . . ? C2 C1 C5 C6 170.9(5) . . . . ? Fe1 C1 C5 C6 110.9(5) . . . . ? C2 C1 C5 Fe1 60.1(4) . . . . ? C3 C4 C5 C1 -0.9(5) . . . . ? Fe1 C4 C5 C1 59.4(3) . . . . ? C3 C4 C5 C6 -172.2(4) . . . . ? Fe1 C4 C5 C6 -112.0(4) . . . . ? C3 C4 C5 Fe1 -60.3(3) . . . . ? C26 Fe1 C5 C1 35.8(8) . . . . ? C4 Fe1 C5 C1 -118.6(4) . . . . ? C25 Fe1 C5 C1 -159.3(7) . . . . ? C22 Fe1 C5 C1 77.3(4) . . . . ? C3 Fe1 C5 C1 -81.0(3) . . . . ? C2 Fe1 C5 C1 -37.9(3) . . . . ? C23 Fe1 C5 C1 119.5(4) . . . . ? C24 Fe1 C5 C1 161.6(4) . . . . ? C26 Fe1 C5 C4 154.4(6) . . . . ? C25 Fe1 C5 C4 -40.7(8) . . . . ? C1 Fe1 C5 C4 118.6(4) . . . . ? C22 Fe1 C5 C4 -164.1(4) . . . . ? C3 Fe1 C5 C4 37.6(3) . . . . ? C2 Fe1 C5 C4 80.6(3) . . . . ? C23 Fe1 C5 C4 -122.0(4) . . . . ? C24 Fe1 C5 C4 -79.9(5) . . . . ? C26 Fe1 C5 C6 -91.6(8) . . . . ? C4 Fe1 C5 C6 114.1(5) . . . . ? C25 Fe1 C5 C6 73.3(9) . . . . ? C1 Fe1 C5 C6 -127.4(6) . . . . ? C22 Fe1 C5 C6 -50.0(6) . . . . ? C3 Fe1 C5 C6 151.6(5) . . . . ? C2 Fe1 C5 C6 -165.3(5) . . . . ? C23 Fe1 C5 C6 -7.9(6) . . . . ? C24 Fe1 C5 C6 34.2(6) . . . . ? C1 C5 C6 C7 14.6(8) . . . . ? C4 C5 C6 C7 -176.5(5) . . . . ? Fe1 C5 C6 C7 102.1(5) . . . . ? C5 C6 C7 C8 7.6(8) . . . . ? C5 C6 C7 C11 178.6(5) . . . . ? C6 C7 C8 C9 173.1(5) . . . . ? C11 C7 C8 C9 0.4(6) . . . . ? C7 C8 C9 C10 -1.7(6) . . . . ? C7 C8 C9 C17 179.8(5) . . . . ? C8 C9 C10 C16 177.9(4) . . . . ? C17 C9 C10 C16 -3.6(8) . . . . ? C8 C9 C10 C11 2.3(6) . . . . ? C17 C9 C10 C11 -179.2(5) . . . . ? C8 C9 C10 Ru1 89.4(6) . . . . ? C17 C9 C10 Ru1 -92.1(7) . . . . ? C30 Ru1 C10 C16 -154.0(4) . . . . ? C29 Ru1 C10 C16 -96.2(16) . . . . ? C28 Ru1 C10 C16 -62.1(4) . . . . ? C27 Ru1 C10 C16 -90.0(3) . . . . ? C31 Ru1 C10 C16 -127.0(4) . . . . ? C13 Ru1 C10 C16 92.3(3) . . . . ? C14 Ru1 C10 C16 56.1(3) . . . . ? C15 Ru1 C10 C16 23.8(3) . . . . ? C12 Ru1 C10 C16 125.2(3) . . . . ? C11 Ru1 C10 C16 145.2(5) . . . . ? C30 Ru1 C10 C9 -41.0(7) . . . . ? C29 Ru1 C10 C9 16.7(18) . . . . ? C28 Ru1 C10 C9 50.8(6) . . . . ? C27 Ru1 C10 C9 22.9(6) . . . . ? C31 Ru1 C10 C9 -14.1(6) . . . . ? C13 Ru1 C10 C9 -154.7(5) . . . . ? C16 Ru1 C10 C9 113.0(6) . . . . ? C14 Ru1 C10 C9 169.1(5) . . . . ? C15 Ru1 C10 C9 136.8(6) . . . . ? C12 Ru1 C10 C9 -121.8(5) . . . . ? C11 Ru1 C10 C9 -101.8(6) . . . . ? C30 Ru1 C10 C11 60.8(5) . . . . ? C29 Ru1 C10 C11 118.6(16) . . . . ? C28 Ru1 C10 C11 152.6(3) . . . . ? C27 Ru1 C10 C11 124.7(3) . . . . ? C31 Ru1 C10 C11 87.7(4) . . . . ? C13 Ru1 C10 C11 -52.9(3) . . . . ? C16 Ru1 C10 C11 -145.2(5) . . . . ? C14 Ru1 C10 C11 -89.1(3) . . . . ? C15 Ru1 C10 C11 -121.4(3) . . . . ? C12 Ru1 C10 C11 -20.0(3) . . . . ? C16 C10 C11 C12 -4.8(8) . . . . ? C9 C10 C11 C12 170.3(5) . . . . ? Ru1 C10 C11 C12 39.3(4) . . . . ? C16 C10 C11 C7 -177.0(5) . . . . ? C9 C10 C11 C7 -2.0(5) . . . . ? Ru1 C10 C11 C7 -132.9(3) . . . . ? C16 C10 C11 Ru1 -44.1(5) . . . . ? C9 C10 C11 Ru1 131.0(4) . . . . ? C6 C7 C11 C12 16.3(8) . . . . ? C8 C7 C11 C12 -171.2(5) . . . . ? C6 C7 C11 C10 -171.5(5) . . . . ? C8 C7 C11 C10 1.0(5) . . . . ? C6 C7 C11 Ru1 112.7(6) . . . . ? C8 C7 C11 Ru1 -74.8(6) . . . . ? C30 Ru1 C11 C12 75.0(5) . . . . ? C29 Ru1 C11 C12 56.0(5) . . . . ? C28 Ru1 C11 C12 146.3(7) . . . . ? C27 Ru1 C11 C12 143.8(3) . . . . ? C31 Ru1 C11 C12 112.2(5) . . . . ? C13 Ru1 C11 C12 -27.1(3) . . . . ? C16 Ru1 C11 C12 -125.3(3) . . . . ? C14 Ru1 C11 C12 -58.2(3) . . . . ? C15 Ru1 C11 C12 -94.3(3) . . . . ? C10 Ru1 C11 C12 -146.6(4) . . . . ? C30 Ru1 C11 C10 -138.4(5) . . . . ? C29 Ru1 C11 C10 -157.4(4) . . . . ? C28 Ru1 C11 C10 -67.0(7) . . . . ? C27 Ru1 C11 C10 -69.6(3) . . . . ? C31 Ru1 C11 C10 -101.2(4) . . . . ? C13 Ru1 C11 C10 119.5(3) . . . . ? C16 Ru1 C11 C10 21.3(3) . . . . ? C14 Ru1 C11 C10 88.4(3) . . . . ? C15 Ru1 C11 C10 52.3(3) . . . . ? C12 Ru1 C11 C10 146.6(4) . . . . ? C30 Ru1 C11 C7 -46.7(7) . . . . ? C29 Ru1 C11 C7 -65.7(7) . . . . ? C28 Ru1 C11 C7 24.6(10) . . . . ? C27 Ru1 C11 C7 22.1(6) . . . . ? C31 Ru1 C11 C7 -9.5(7) . . . . ? C13 Ru1 C11 C7 -148.8(6) . . . . ? C16 Ru1 C11 C7 113.0(6) . . . . ? C14 Ru1 C11 C7 -180.0(6) . . . . ? C15 Ru1 C11 C7 144.0(6) . . . . ? C12 Ru1 C11 C7 -121.7(7) . . . . ? C10 Ru1 C11 C7 91.7(6) . . . . ? C10 C11 C12 C13 12.2(8) . . . . ? C7 C11 C12 C13 -177.1(5) . . . . ? Ru1 C11 C12 C13 51.7(5) . . . . ? C10 C11 C12 C18 -165.1(5) . . . . ? C7 C11 C12 C18 5.6(8) . . . . ? Ru1 C11 C12 C18 -125.6(5) . . . . ? C10 C11 C12 Ru1 -39.5(4) . . . . ? C7 C11 C12 Ru1 131.2(5) . . . . ? C30 Ru1 C12 C11 -114.6(5) . . . . ? C29 Ru1 C12 C11 -149.4(4) . . . . ? C28 Ru1 C12 C11 -143.7(6) . . . . ? C27 Ru1 C12 C11 -63.0(5) . . . . ? C31 Ru1 C12 C11 -78.3(4) . . . . ? C13 Ru1 C12 C11 136.3(5) . . . . ? C16 Ru1 C12 C11 49.3(3) . . . . ? C14 Ru1 C12 C11 114.8(4) . . . . ? C15 Ru1 C12 C11 85.7(3) . . . . ? C10 Ru1 C12 C11 20.4(3) . . . . ? C30 Ru1 C12 C13 109.1(5) . . . . ? C29 Ru1 C12 C13 74.4(5) . . . . ? C28 Ru1 C12 C13 80.0(8) . . . . ? C27 Ru1 C12 C13 160.7(4) . . . . ? C31 Ru1 C12 C13 145.5(4) . . . . ? C16 Ru1 C12 C13 -87.0(4) . . . . ? C14 Ru1 C12 C13 -21.5(4) . . . . ? C15 Ru1 C12 C13 -50.5(4) . . . . ? C10 Ru1 C12 C13 -115.9(4) . . . . ? C11 Ru1 C12 C13 -136.3(5) . . . . ? C30 Ru1 C12 C18 6.2(6) . . . . ? C29 Ru1 C12 C18 -28.6(6) . . . . ? C28 Ru1 C12 C18 -22.9(9) . . . . ? C27 Ru1 C12 C18 57.8(6) . . . . ? C31 Ru1 C12 C18 42.5(6) . . . . ? C13 Ru1 C12 C18 -102.9(6) . . . . ? C16 Ru1 C12 C18 170.1(4) . . . . ? C14 Ru1 C12 C18 -124.4(5) . . . . ? C15 Ru1 C12 C18 -153.5(4) . . . . ? C10 Ru1 C12 C18 141.2(5) . . . . ? C11 Ru1 C12 C18 120.8(6) . . . . ? C11 C12 C13 C14 -6.9(9) . . . . ? C18 C12 C13 C14 170.6(6) . . . . ? Ru1 C12 C13 C14 48.1(6) . . . . ? C11 C12 C13 Ru1 -55.0(5) . . . . ? C18 C12 C13 Ru1 122.5(4) . . . . ? C30 Ru1 C13 C14 134.9(5) . . . . ? C29 Ru1 C13 C14 93.8(5) . . . . ? C28 Ru1 C13 C14 64.6(5) . . . . ? C27 Ru1 C13 C14 103.2(12) . . . . ? C31 Ru1 C13 C14 161.5(5) . . . . ? C16 Ru1 C13 C14 -52.0(4) . . . . ? C15 Ru1 C13 C14 -20.5(4) . . . . ? C12 Ru1 C13 C14 -144.5(5) . . . . ? C10 Ru1 C13 C14 -88.3(4) . . . . ? C11 Ru1 C13 C14 -118.9(4) . . . . ? C30 Ru1 C13 C12 -80.5(5) . . . . ? C29 Ru1 C13 C12 -121.7(5) . . . . ? C28 Ru1 C13 C12 -150.9(4) . . . . ? C27 Ru1 C13 C12 -112.3(11) . . . . ? C31 Ru1 C13 C12 -53.9(5) . . . . ? C16 Ru1 C13 C12 92.5(3) . . . . ? C14 Ru1 C13 C12 144.5(5) . . . . ? C15 Ru1 C13 C12 124.1(4) . . . . ? C10 Ru1 C13 C12 56.3(3) . . . . ? C11 Ru1 C13 C12 25.7(3) . . . . ? C12 C13 C14 C15 -3.4(11) . . . . ? Ru1 C13 C14 C15 45.1(6) . . . . ? C12 C13 C14 Ru1 -48.6(6) . . . . ? C30 Ru1 C14 C13 -62.7(5) . . . . ? C29 Ru1 C14 C13 -97.1(5) . . . . ? C28 Ru1 C14 C13 -136.3(4) . . . . ? C27 Ru1 C14 C13 -160.1(4) . . . . ? C31 Ru1 C14 C13 -76.4(16) . . . . ? C16 Ru1 C14 C13 121.4(4) . . . . ? C15 Ru1 C14 C13 146.4(6) . . . . ? C12 Ru1 C14 C13 22.0(3) . . . . ? C10 Ru1 C14 C13 89.2(4) . . . . ? C11 Ru1 C14 C13 53.4(4) . . . . ? C30 Ru1 C14 C15 150.9(4) . . . . ? C29 Ru1 C14 C15 116.5(5) . . . . ? C28 Ru1 C14 C15 77.3(4) . . . . ? C27 Ru1 C14 C15 53.4(5) . . . . ? C31 Ru1 C14 C15 137.2(15) . . . . ? C13 Ru1 C14 C15 -146.4(6) . . . . ? C16 Ru1 C14 C15 -25.1(3) . . . . ? C12 Ru1 C14 C15 -124.5(4) . . . . ? C10 Ru1 C14 C15 -57.2(3) . . . . ? C11 Ru1 C14 C15 -93.0(3) . . . . ? C13 C14 C15 C16 3.0(10) . . . . ? Ru1 C14 C15 C16 47.4(5) . . . . ? C13 C14 C15 C19 -172.1(6) . . . . ? Ru1 C14 C15 C19 -127.7(5) . . . . ? C13 C14 C15 Ru1 -44.4(6) . . . . ? C30 Ru1 C15 C14 -68.8(8) . . . . ? C29 Ru1 C15 C14 -77.7(4) . . . . ? C28 Ru1 C15 C14 -113.9(4) . . . . ? C27 Ru1 C15 C14 -148.7(3) . . . . ? C31 Ru1 C15 C14 -162.3(5) . . . . ? C13 Ru1 C15 C14 20.5(3) . . . . ? C16 Ru1 C15 C14 138.9(5) . . . . ? C12 Ru1 C15 C14 50.4(4) . . . . ? C10 Ru1 C15 C14 115.2(4) . . . . ? C11 Ru1 C15 C14 85.3(4) . . . . ? C30 Ru1 C15 C16 152.4(7) . . . . ? C29 Ru1 C15 C16 143.4(4) . . . . ? C28 Ru1 C15 C16 107.2(4) . . . . ? C27 Ru1 C15 C16 72.4(4) . . . . ? C31 Ru1 C15 C16 58.9(7) . . . . ? C13 Ru1 C15 C16 -118.4(4) . . . . ? C14 Ru1 C15 C16 -138.9(5) . . . . ? C12 Ru1 C15 C16 -88.5(3) . . . . ? C10 Ru1 C15 C16 -23.7(3) . . . . ? C11 Ru1 C15 C16 -53.6(3) . . . . ? C30 Ru1 C15 C19 46.2(11) . . . . ? C29 Ru1 C15 C19 37.3(7) . . . . ? C28 Ru1 C15 C19 1.0(7) . . . . ? C27 Ru1 C15 C19 -33.7(7) . . . . ? C31 Ru1 C15 C19 -47.3(9) . . . . ? C13 Ru1 C15 C19 135.4(7) . . . . ? C16 Ru1 C15 C19 -106.2(7) . . . . ? C14 Ru1 C15 C19 115.0(7) . . . . ? C12 Ru1 C15 C19 165.4(6) . . . . ? C10 Ru1 C15 C19 -129.8(7) . . . . ? C11 Ru1 C15 C19 -159.7(6) . . . . ? C14 C15 C16 C10 5.7(9) . . . . ? C19 C15 C16 C10 -178.9(5) . . . . ? Ru1 C15 C16 C10 53.4(5) . . . . ? C14 C15 C16 Ru1 -47.8(5) . . . . ? C19 C15 C16 Ru1 127.6(5) . . . . ? C9 C10 C16 C15 178.9(5) . . . . ? C11 C10 C16 C15 -6.6(9) . . . . ? Ru1 C10 C16 C15 -53.0(5) . . . . ? C9 C10 C16 Ru1 -128.1(4) . . . . ? C11 C10 C16 Ru1 46.4(5) . . . . ? C30 Ru1 C16 C15 -145.7(11) . . . . ? C29 Ru1 C16 C15 -61.1(5) . . . . ? C28 Ru1 C16 C15 -83.2(4) . . . . ? C27 Ru1 C16 C15 -120.0(4) . . . . ? C31 Ru1 C16 C15 -150.7(4) . . . . ? C13 Ru1 C16 C15 55.1(3) . . . . ? C14 Ru1 C16 C15 24.8(3) . . . . ? C12 Ru1 C16 C15 92.1(3) . . . . ? C10 Ru1 C16 C15 141.0(5) . . . . ? C11 Ru1 C16 C15 120.0(4) . . . . ? C30 Ru1 C16 C10 73.3(11) . . . . ? C29 Ru1 C16 C10 157.8(4) . . . . ? C28 Ru1 C16 C10 135.8(4) . . . . ? C27 Ru1 C16 C10 99.0(3) . . . . ? C31 Ru1 C16 C10 68.3(4) . . . . ? C13 Ru1 C16 C10 -85.9(3) . . . . ? C14 Ru1 C16 C10 -116.2(4) . . . . ? C15 Ru1 C16 C10 -141.0(5) . . . . ? C12 Ru1 C16 C10 -48.9(3) . . . . ? C11 Ru1 C16 C10 -21.0(3) . . . . ? C14 C15 C19 C20 -104.0(9) . . . . ? C16 C15 C19 C20 80.5(9) . . . . ? Ru1 C15 C19 C20 164.9(7) . . . . ? C14 C15 C19 C21 23.5(9) . . . . ? C16 C15 C19 C21 -152.0(7) . . . . ? Ru1 C15 C19 C21 -67.6(9) . . . . ? C26 Fe1 C22 C23 -116.8(6) . . . . ? C4 Fe1 C22 C23 43.0(11) . . . . ? C25 Fe1 C22 C23 -78.3(5) . . . . ? C5 Fe1 C22 C23 81.4(5) . . . . ? C1 Fe1 C22 C23 124.2(5) . . . . ? C3 Fe1 C22 C23 -156.3(6) . . . . ? C2 Fe1 C22 C23 167.3(4) . . . . ? C24 Fe1 C22 C23 -35.5(5) . . . . ? C4 Fe1 C22 C26 159.8(7) . . . . ? C25 Fe1 C22 C26 38.5(4) . . . . ? C5 Fe1 C22 C26 -161.9(3) . . . . ? C1 Fe1 C22 C26 -119.0(3) . . . . ? C3 Fe1 C22 C26 -39.5(8) . . . . ? C2 Fe1 C22 C26 -75.9(4) . . . . ? C23 Fe1 C22 C26 116.8(6) . . . . ? C24 Fe1 C22 C26 81.3(4) . . . . ? C26 C22 C23 C24 -0.9(7) . . . . ? Fe1 C22 C23 C24 59.2(5) . . . . ? C26 C22 C23 Fe1 -60.1(4) . . . . ? C26 Fe1 C23 C24 -81.5(5) . . . . ? C4 Fe1 C23 C24 72.9(6) . . . . ? C25 Fe1 C23 C24 -37.1(5) . . . . ? C5 Fe1 C23 C24 118.1(5) . . . . ? C1 Fe1 C23 C24 163.3(5) . . . . ? C22 Fe1 C23 C24 -121.6(7) . . . . ? C3 Fe1 C23 C24 28.1(11) . . . . ? C2 Fe1 C23 C24 -152.7(7) . . . . ? C26 Fe1 C23 C22 40.1(4) . . . . ? C4 Fe1 C23 C22 -165.4(4) . . . . ? C25 Fe1 C23 C22 84.5(5) . . . . ? C5 Fe1 C23 C22 -120.2(5) . . . . ? C1 Fe1 C23 C22 -75.0(5) . . . . ? C3 Fe1 C23 C22 149.8(7) . . . . ? C2 Fe1 C23 C22 -31.1(10) . . . . ? C24 Fe1 C23 C22 121.6(7) . . . . ? C22 C23 C24 C25 0.3(8) . . . . ? Fe1 C23 C24 C25 59.0(5) . . . . ? C22 C23 C24 Fe1 -58.7(5) . . . . ? C26 Fe1 C24 C23 81.1(5) . . . . ? C4 Fe1 C24 C23 -126.7(5) . . . . ? C25 Fe1 C24 C23 119.6(7) . . . . ? C5 Fe1 C24 C23 -83.0(5) . . . . ? C1 Fe1 C24 C23 -44.2(11) . . . . ? C22 Fe1 C24 C23 35.7(5) . . . . ? C3 Fe1 C24 C23 -169.3(4) . . . . ? C2 Fe1 C24 C23 153.8(7) . . . . ? C26 Fe1 C24 C25 -38.5(5) . . . . ? C4 Fe1 C24 C25 113.7(5) . . . . ? C5 Fe1 C24 C25 157.4(5) . . . . ? C1 Fe1 C24 C25 -163.9(7) . . . . ? C22 Fe1 C24 C25 -84.0(6) . . . . ? C3 Fe1 C24 C25 71.0(6) . . . . ? C2 Fe1 C24 C25 34.2(11) . . . . ? C23 Fe1 C24 C25 -119.6(7) . . . . ? C23 C24 C25 C26 0.4(8) . . . . ? Fe1 C24 C25 C26 60.4(4) . . . . ? C23 C24 C25 Fe1 -59.9(5) . . . . ? C26 Fe1 C25 C24 118.1(7) . . . . ? C4 Fe1 C25 C24 -84.6(6) . . . . ? C5 Fe1 C25 C24 -54.8(10) . . . . ? C1 Fe1 C25 C24 165.2(7) . . . . ? C22 Fe1 C25 C24 78.7(6) . . . . ? C3 Fe1 C25 C24 -125.7(5) . . . . ? C2 Fe1 C25 C24 -165.8(5) . . . . ? C23 Fe1 C25 C24 36.4(5) . . . . ? C4 Fe1 C25 C26 157.3(4) . . . . ? C5 Fe1 C25 C26 -172.8(5) . . . . ? C1 Fe1 C25 C26 47.2(10) . . . . ? C22 Fe1 C25 C26 -39.4(4) . . . . ? C3 Fe1 C25 C26 116.2(4) . . . . ? C2 Fe1 C25 C26 76.1(5) . . . . ? C23 Fe1 C25 C26 -81.6(5) . . . . ? C24 Fe1 C25 C26 -118.1(7) . . . . ? C24 C25 C26 C22 -0.9(7) . . . . ? Fe1 C25 C26 C22 60.6(4) . . . . ? C24 C25 C26 Fe1 -61.6(5) . . . . ? C23 C22 C26 C25 1.1(6) . . . . ? Fe1 C22 C26 C25 -60.7(4) . . . . ? C23 C22 C26 Fe1 61.8(4) . . . . ? C4 Fe1 C26 C25 -49.5(7) . . . . ? C5 Fe1 C26 C25 171.1(7) . . . . ? C1 Fe1 C26 C25 -161.4(4) . . . . ? C22 Fe1 C26 C25 117.2(6) . . . . ? C3 Fe1 C26 C25 -79.9(5) . . . . ? C2 Fe1 C26 C25 -120.9(5) . . . . ? C23 Fe1 C26 C25 79.7(5) . . . . ? C24 Fe1 C26 C25 37.5(5) . . . . ? C4 Fe1 C26 C22 -166.7(5) . . . . ? C25 Fe1 C26 C22 -117.2(6) . . . . ? C5 Fe1 C26 C22 53.9(8) . . . . ? C1 Fe1 C26 C22 81.4(4) . . . . ? C3 Fe1 C26 C22 162.8(4) . . . . ? C2 Fe1 C26 C22 121.9(4) . . . . ? C23 Fe1 C26 C22 -37.5(4) . . . . ? C24 Fe1 C26 C22 -79.7(5) . . . . ? C30 Ru1 C27 C31 37.2(6) . . . . ? C29 Ru1 C27 C31 82.1(6) . . . . ? C28 Ru1 C27 C31 119.8(7) . . . . ? C13 Ru1 C27 C31 71.8(13) . . . . ? C16 Ru1 C27 C31 -133.6(5) . . . . ? C14 Ru1 C27 C31 158.8(6) . . . . ? C15 Ru1 C27 C31 -169.0(5) . . . . ? C12 Ru1 C27 C31 -24.7(6) . . . . ? C10 Ru1 C27 C31 -96.3(5) . . . . ? C11 Ru1 C27 C31 -61.8(5) . . . . ? C30 Ru1 C27 C28 -82.6(6) . . . . ? C29 Ru1 C27 C28 -37.7(5) . . . . ? C31 Ru1 C27 C28 -119.8(7) . . . . ? C13 Ru1 C27 C28 -47.9(13) . . . . ? C16 Ru1 C27 C28 106.6(4) . . . . ? C14 Ru1 C27 C28 39.0(6) . . . . ? C15 Ru1 C27 C28 71.2(5) . . . . ? C12 Ru1 C27 C28 -144.5(5) . . . . ? C10 Ru1 C27 C28 143.9(4) . . . . ? C11 Ru1 C27 C28 178.4(4) . . . . ? C31 C27 C28 C29 -0.8(7) . . . . ? Ru1 C27 C28 C29 61.9(5) . . . . ? C31 C27 C28 Ru1 -62.7(4) . . . . ? C30 Ru1 C28 C27 77.5(6) . . . . ? C29 Ru1 C28 C27 117.9(7) . . . . ? C31 Ru1 C28 C27 35.3(5) . . . . ? C13 Ru1 C28 C27 167.7(4) . . . . ? C16 Ru1 C28 C27 -83.7(4) . . . . ? C14 Ru1 C28 C27 -156.8(4) . . . . ? C15 Ru1 C28 C27 -120.8(4) . . . . ? C12 Ru1 C28 C27 110.0(7) . . . . ? C10 Ru1 C28 C27 -50.0(5) . . . . ? C11 Ru1 C28 C27 -3.7(10) . . . . ? C30 Ru1 C28 C29 -40.4(6) . . . . ? C27 Ru1 C28 C29 -117.9(7) . . . . ? C31 Ru1 C28 C29 -82.5(6) . . . . ? C13 Ru1 C28 C29 49.8(7) . . . . ? C16 Ru1 C28 C29 158.4(5) . . . . ? C14 Ru1 C28 C29 85.3(6) . . . . ? C15 Ru1 C28 C29 121.3(5) . . . . ? C12 Ru1 C28 C29 -7.9(10) . . . . ? C10 Ru1 C28 C29 -167.9(5) . . . . ? C11 Ru1 C28 C29 -121.6(8) . . . . ? C27 C28 C29 C30 0.3(7) . . . . ? Ru1 C28 C29 C30 62.9(4) . . . . ? C27 C28 C29 Ru1 -62.5(4) . . . . ? C30 Ru1 C29 C28 114.0(7) . . . . ? C27 Ru1 C29 C28 36.2(4) . . . . ? C31 Ru1 C29 C28 76.6(6) . . . . ? C13 Ru1 C29 C28 -145.9(5) . . . . ? C16 Ru1 C29 C28 -35.4(7) . . . . ? C14 Ru1 C29 C28 -108.3(5) . . . . ? C15 Ru1 C29 C28 -71.5(5) . . . . ? C12 Ru1 C29 C28 176.8(4) . . . . ? C10 Ru1 C29 C28 43.0(19) . . . . ? C11 Ru1 C29 C28 142.6(5) . . . . ? C28 Ru1 C29 C30 -114.0(7) . . . . ? C27 Ru1 C29 C30 -77.8(6) . . . . ? C31 Ru1 C29 C30 -37.5(5) . . . . ? C13 Ru1 C29 C30 100.1(6) . . . . ? C16 Ru1 C29 C30 -149.4(6) . . . . ? C14 Ru1 C29 C30 137.7(6) . . . . ? C15 Ru1 C29 C30 174.5(5) . . . . ? C12 Ru1 C29 C30 62.8(6) . . . . ? C10 Ru1 C29 C30 -71.0(19) . . . . ? C11 Ru1 C29 C30 28.6(8) . . . . ? C28 C29 C30 C31 0.2(8) . . . . ? Ru1 C29 C30 C31 63.8(5) . . . . ? C28 C29 C30 Ru1 -63.6(5) . . . . ? C29 Ru1 C30 C31 -115.8(7) . . . . ? C28 Ru1 C30 C31 -76.9(6) . . . . ? C27 Ru1 C30 C31 -35.9(5) . . . . ? C13 Ru1 C30 C31 151.1(5) . . . . ? C16 Ru1 C30 C31 -6.9(15) . . . . ? C14 Ru1 C30 C31 -175.2(5) . . . . ? C15 Ru1 C30 C31 -128.3(10) . . . . ? C12 Ru1 C30 C31 114.0(6) . . . . ? C10 Ru1 C30 C31 46.5(7) . . . . ? C11 Ru1 C30 C31 79.8(6) . . . . ? C28 Ru1 C30 C29 38.8(5) . . . . ? C27 Ru1 C30 C29 79.9(5) . . . . ? C31 Ru1 C30 C29 115.8(7) . . . . ? C13 Ru1 C30 C29 -93.2(5) . . . . ? C16 Ru1 C30 C29 108.9(13) . . . . ? C14 Ru1 C30 C29 -59.5(6) . . . . ? C15 Ru1 C30 C29 -12.5(11) . . . . ? C12 Ru1 C30 C29 -130.2(5) . . . . ? C10 Ru1 C30 C29 162.2(5) . . . . ? C11 Ru1 C30 C29 -164.4(5) . . . . ? C28 C27 C31 C30 1.0(7) . . . . ? Ru1 C27 C31 C30 -61.2(5) . . . . ? C28 C27 C31 Ru1 62.1(4) . . . . ? C29 C30 C31 C27 -0.7(7) . . . . ? Ru1 C30 C31 C27 61.7(4) . . . . ? C29 C30 C31 Ru1 -62.4(5) . . . . ? C30 Ru1 C31 C27 -118.3(7) . . . . ? C29 Ru1 C31 C27 -78.6(5) . . . . ? C28 Ru1 C31 C27 -35.8(4) . . . . ? C13 Ru1 C31 C27 -162.9(4) . . . . ? C16 Ru1 C31 C27 59.0(5) . . . . ? C14 Ru1 C31 C27 -101.1(17) . . . . ? C15 Ru1 C31 C27 21.0(8) . . . . ? C12 Ru1 C31 C27 165.4(4) . . . . ? C10 Ru1 C31 C27 93.8(4) . . . . ? C11 Ru1 C31 C27 130.4(4) . . . . ? C29 Ru1 C31 C30 39.7(5) . . . . ? C28 Ru1 C31 C30 82.5(6) . . . . ? C27 Ru1 C31 C30 118.3(7) . . . . ? C13 Ru1 C31 C30 -44.6(7) . . . . ? C16 Ru1 C31 C30 177.3(6) . . . . ? C14 Ru1 C31 C30 17.2(19) . . . . ? C15 Ru1 C31 C30 139.3(8) . . . . ? C12 Ru1 C31 C30 -76.3(6) . . . . ? C10 Ru1 C31 C30 -147.8(6) . . . . ? C11 Ru1 C31 C30 -111.3(6) . . . . ? B2B F5 B2A F7A 180(4) . . . . ? B2B F5 B2A F8A -53(3) . . . . ? B2B F5 B2A F6A 43(3) . . . . ? B2A F5 B2B F8B 29(3) . . . . ? B2A F5 B2B F7B -90(3) . . . . ? B2A F5 B2B F6B 144(4) . . . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.81 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 1.234 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.106 #============================================================================