# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Amar Flood' _publ_contact_author_name 'Amar Flood' _publ_contact_author_address ; Chemistry Indiana University 800 East Kirkwood Avenue Bloomington IN 47405 UNITED STATES OF AMERICA ; _publ_contact_author_email AFLOOD@INDIANA.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Can Terdentate 2,6-Bis(1,2,3-Triazol-4-yl)Pyridines form Stable Coordination Compounds? ; data_06183 _database_code_depnum_ccdc_archive 'CCDC 639381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H69 Eu N21, 3(Cl O4), H2 O' _chemical_formula_sum 'C51 H71 Cl3 Eu N21 O13' _chemical_formula_weight 1444.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbcn ' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 19.2068(17) _cell_length_b 28.499(3) _cell_length_c 24.321(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13313(2) _cell_formula_units_Z 8 _cell_measurement_temperature 135(2) _cell_measurement_reflns_used 2045 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.08 _exptl_crystal_description triangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5936 _exptl_absorpt_coefficient_mu 1.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8312 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Bruker-AXS SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 135(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 30.16 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 348794 _diffrn_reflns_av_R_equivalents 0.1246 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.56 _reflns_number_total 15355 _reflns_number_gt 8465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Reciprocal Net (http://recipnet.org)' _computing_publication_material ? _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. Severe disorder in all perchlorate groups. A single atom assigned oxygen located in the lattice (O1) is assumed to be a water solvent. Closest neighbors to O1 are oxygen atoms in two of the perchlorate ions. Two of the n-(CH2)3Me chains are disordered as well. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+46.9293P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15355 _refine_ls_number_parameters 944 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1915 _refine_ls_wR_factor_gt 0.1577 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.072 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.734365(11) 0.118388(9) 0.516987(9) 0.04847(6) Uani 1 1 d . F . Cl1 Cl 0.71766(19) 0.11630(7) 0.90175(8) 0.1232(10) Uani 0.882(2) 1 d P A 1 O1 O 0.9141(7) 0.1222(4) 0.7928(4) 0.290(6) Uani 1 1 d . . . Cl1A Cl 0.7374(4) 0.1171(3) 0.9117(3) 0.0235(15) Uiso 0.118(2) 1 d P A 2 Cl2 Cl 0.5000 0.24174(7) 0.7500 0.0716(6) Uani 1 2 d S . 1 O2 O 0.7249(7) 0.1220(2) 0.9592(3) 0.228(6) Uani 0.882(2) 1 d P A 1 N2 N 0.6871(2) 0.12805(13) 0.61314(15) 0.0543(11) Uani 1 1 d . . . O2A O 0.6760(8) 0.1354(9) 0.9350(15) 0.245(14) Uani 0.283(13) 1 d P A 2 Cl3 Cl 0.36857(7) 0.13388(6) 0.36751(5) 0.0742(4) Uani 1 1 d . B 1 O3 O 0.7798(4) 0.13137(19) 0.8730(3) 0.128(2) Uani 0.882(2) 1 d P A 1 N3 N 0.7206(2) 0.12670(15) 0.65970(17) 0.0611(12) Uani 1 1 d . . . O3A O 0.7659(13) 0.1097(9) 0.9645(10) 0.039(6) Uiso 0.118(2) 1 d P A 2 Cl4 Cl 0.0000 0.00850(16) 0.7500 0.1384(14) Uani 1 2 d S . 2 O4 O 0.7065(3) 0.06867(14) 0.89148(18) 0.0813(14) Uani 0.882(2) 1 d P A 1 N4 N 0.6766(2) 0.14306(15) 0.69776(16) 0.0644(12) Uani 1 1 d . . . O15A O 0.0000 -0.0431(6) 0.7500 0.067(5) Uani 0.332(11) 2 d SP . . O4A O 0.806(3) 0.1270(17) 0.912(2) 0.131(17) Uiso 0.118(2) 1 d P A 2 O5 O 0.6616(5) 0.1437(2) 0.8823(3) 0.224(3) Uani 0.882(2) 1 d P A 1 C5 C 0.6154(3) 0.15440(17) 0.6762(2) 0.0631(14) Uani 1 1 d . . . H5 H 0.5757 0.1662 0.6949 0.076 Uiso 1 1 calc R . . O6 O 0.5441(7) 0.2657(3) 0.7189(4) 0.259(5) Uani 0.792(4) 1 d P C 1 C6 C 0.6217(2) 0.14545(15) 0.62057(19) 0.0489(12) Uani 1 1 d . . . O6A O 0.4759(12) 0.2854(9) 0.7201(10) 0.110(8) Uani 0.208(4) 1 d P . 2 O7 O 0.5361(2) 0.20742(18) 0.78428(19) 0.0760(16) Uani 0.792(4) 1 d P C 1 C7 C 0.5761(2) 0.15085(15) 0.5741(2) 0.0533(13) Uani 1 1 d . . . O7A O 0.5177(11) 0.2458(6) 0.6905(8) 0.090(7) Uani 0.208(4) 1 d P C 2 O8 O 0.4098(3) 0.09186(19) 0.3729(3) 0.1017(19) Uani 0.851(3) 1 d P B 1 N8 N 0.60444(19) 0.14128(13) 0.52485(14) 0.0475(10) Uani 1 1 d . . . O8A O 0.5752(9) 0.2436(6) 0.7505(7) 0.061(4) Uiso 0.208(4) 1 d P . 2 O9 O 0.3423(3) 0.1395(2) 0.4227(2) 0.111(2) Uani 0.851(3) 1 d P B 1 C9 C 0.5650(2) 0.14550(16) 0.4793(2) 0.0537(12) Uani 1 1 d . . . O9A O 0.3928(11) 0.1058(7) 0.4031(8) 0.045(5) Uiso 0.149(3) 1 d P B 2 O10 O 0.30971(19) 0.12424(15) 0.33390(16) 0.0663(13) Uani 0.851(3) 1 d P B 1 C10 C 0.5996(2) 0.13447(16) 0.4275(2) 0.0537(13) Uani 1 1 d . . . O10A O 0.3641(8) 0.1815(6) 0.3966(6) 0.030(4) Uiso 0.149(3) 1 d P B 2 O11 O 0.4118(3) 0.1646(2) 0.3441(3) 0.140(2) Uani 0.851(3) 1 d P B 1 C11 C 0.5769(3) 0.12943(17) 0.3748(2) 0.0597(14) Uani 1 1 d . . . H11 H 0.5304 0.1318 0.3618 0.072 Uiso 1 1 calc R . . O11A O -0.0104(6) -0.0502(11) 0.6983(4) 0.77(2) Uani 0.874(17) 1 d P . 2 O12 O -0.0048(17) 0.0544(15) 0.7212(11) 0.749(16) Uani 0.30 1 d P . 2 N12 N 0.6346(2) 0.12034(15) 0.34511(17) 0.0657(12) Uani 1 1 d . . . O13 O -0.0003(6) -0.0193(4) 0.7954(4) 0.047(2) Uiso 0.30 1 d P . 2 N13 N 0.6906(2) 0.11986(16) 0.37709(16) 0.0658(12) Uani 1 1 d . . . O13A O -0.0564(6) 0.0429(4) 0.7500(4) 0.101(4) Uani 0.362(8) 1 d P . 2 N14 N 0.6705(2) 0.12775(15) 0.42793(16) 0.0613(12) Uani 1 1 d . . . O14A O -0.0764(7) -0.0152(9) 0.7558(6) 0.201(11) Uani 0.410(11) 1 d P . . C15 C 0.5071(3) 0.16524(19) 0.5793(2) 0.0717(16) Uani 1 1 d . . . H15 H 0.4878 0.1720 0.6144 0.086 Uiso 1 1 calc R . . C16 C 0.4681(3) 0.1693(2) 0.5329(3) 0.089(2) Uani 1 1 d . . . H16 H 0.4207 0.1786 0.5356 0.107 Uiso 1 1 calc R . . C17 C 0.4963(3) 0.15998(19) 0.4816(2) 0.0710(16) Uani 1 1 d . . . H17 H 0.4693 0.1634 0.4491 0.085 Uiso 1 1 calc R . . C18 C 0.6990(4) 0.1491(2) 0.7547(2) 0.0813(18) Uani 1 1 d . . . H18A H 0.7377 0.1272 0.7627 0.098 Uiso 1 1 calc R . . H18B H 0.6599 0.1416 0.7797 0.098 Uiso 1 1 calc R . . C19 C 0.7231(4) 0.1997(2) 0.7648(2) 0.103(2) Uani 1 1 d . . . H19A H 0.6831 0.2207 0.7577 0.123 Uiso 1 1 calc R . . H19B H 0.7349 0.2027 0.8043 0.123 Uiso 1 1 calc R . . C20 C 0.7802(5) 0.2164(3) 0.7341(3) 0.131(3) Uani 1 1 d . . . H20A H 0.7689 0.2143 0.6944 0.158 Uiso 1 1 calc R . . H20B H 0.8209 0.1960 0.7411 0.158 Uiso 1 1 calc R . . C21 C 0.7998(5) 0.2682(3) 0.7483(4) 0.150(4) Uani 1 1 d . . . H21A H 0.7614 0.2890 0.7378 0.224 Uiso 1 1 calc R . . H21B H 0.8419 0.2771 0.7282 0.224 Uiso 1 1 calc R . . H21C H 0.8083 0.2710 0.7879 0.224 Uiso 1 1 calc R . . C22 C 0.6399(3) 0.1109(2) 0.2861(2) 0.0781(19) Uani 1 1 d . . . H22A H 0.6863 0.1210 0.2727 0.094 Uiso 1 1 calc R . . H22B H 0.6042 0.1294 0.2663 0.094 Uiso 1 1 calc R . . C23 C 0.6299(5) 0.0593(2) 0.2739(3) 0.127(3) Uani 1 1 d . . . H23A H 0.6240 0.0552 0.2337 0.152 Uiso 1 1 calc R . . H23B H 0.5866 0.0484 0.2919 0.152 Uiso 1 1 calc R . . C24 C 0.6913(8) 0.0282(3) 0.2935(3) 0.256(7) Uani 1 1 d . . . H24A H 0.7284 0.0507 0.3036 0.308 Uiso 1 1 calc R . . H24B H 0.6751 0.0144 0.3285 0.308 Uiso 1 1 calc R . . C25 C 0.7212(7) -0.0031(7) 0.2706(5) 0.293(10) Uani 1 1 d . . . H25A H 0.7579 -0.0153 0.2947 0.440 Uiso 1 1 calc R . . H25B H 0.7420 0.0087 0.2365 0.440 Uiso 1 1 calc R . . H25C H 0.6881 -0.0282 0.2620 0.440 Uiso 1 1 calc R . . N26 N 0.8408(2) 0.13354(17) 0.57429(18) 0.0668(13) Uani 1 1 d . . . N27 N 0.8704(2) 0.1746(2) 0.5861(2) 0.0907(17) Uani 1 1 d . . . N28 N 0.9135(3) 0.1659(2) 0.6282(2) 0.0941(18) Uani 1 1 d . . . C29 C 0.9110(3) 0.1210(3) 0.6431(2) 0.087(2) Uani 1 1 d . . . H29 H 0.9368 0.1067 0.6718 0.105 Uiso 1 1 calc R . . C30 C 0.8639(2) 0.0994(2) 0.6089(2) 0.0656(16) Uani 1 1 d . . . C31 C 0.8356(3) 0.0532(2) 0.6053(2) 0.0694(16) Uani 1 1 d . . . N32 N 0.78090(19) 0.04794(15) 0.57135(15) 0.0565(11) Uani 1 1 d . . . C33 C 0.7495(3) 0.0061(2) 0.5667(2) 0.0664(16) Uani 1 1 d . . . C34 C 0.6904(3) 0.00299(18) 0.5301(2) 0.0631(15) Uani 1 1 d . . . C35 C 0.6500(3) -0.03249(19) 0.5112(2) 0.0779(18) Uani 1 1 d . . . H35 H 0.6537 -0.0647 0.5207 0.093 Uiso 1 1 calc R . . N36 N 0.6049(2) -0.01368(15) 0.4772(2) 0.0688(13) Uani 1 1 d . . . N37 N 0.6146(2) 0.03262(14) 0.47323(18) 0.0617(12) Uani 1 1 d . . . N38 N 0.66724(19) 0.04319(14) 0.50542(16) 0.0535(11) Uani 1 1 d . . . C39 C 0.8615(4) 0.0167(3) 0.6359(3) 0.110(3) Uani 1 1 d . . . H39 H 0.9004 0.0208 0.6595 0.132 Uiso 1 1 calc R . . C40 C 0.8291(5) -0.0259(3) 0.6308(4) 0.139(3) Uani 1 1 d . . . H40 H 0.8458 -0.0517 0.6517 0.167 Uiso 1 1 calc R . . C41 C 0.7729(4) -0.0322(3) 0.5961(3) 0.110(3) Uani 1 1 d . . . H41 H 0.7510 -0.0620 0.5926 0.131 Uiso 1 1 calc R . . C42 C 0.9562(4) 0.2038(3) 0.6505(3) 0.134(3) Uani 1 1 d . . . H42A H 0.9714 0.1962 0.6883 0.160 Uiso 1 1 calc R . . H42B H 0.9291 0.2334 0.6516 0.160 Uiso 1 1 calc R . . C43 C 1.0249(3) 0.2098(3) 0.6095(4) 0.163(4) Uani 1 1 d . . . H43A H 1.0474 0.1790 0.6035 0.196 Uiso 1 1 calc R . . H43B H 1.0101 0.2223 0.5733 0.196 Uiso 1 1 calc R . . C44 C 1.0719(6) 0.2408(5) 0.6344(4) 0.192(5) Uani 1 1 d . . . H44A H 1.0879 0.2287 0.6704 0.230 Uiso 1 1 calc R . . H44B H 1.0508 0.2722 0.6396 0.230 Uiso 1 1 calc R . . C45 C 1.1322(5) 0.2428(4) 0.5929(5) 0.252(5) Uani 1 1 d . . . H45A H 1.1603 0.2142 0.5960 0.378 Uiso 1 1 calc R . . H45B H 1.1614 0.2702 0.6006 0.378 Uiso 1 1 calc R . . H45C H 1.1134 0.2452 0.5555 0.378 Uiso 1 1 calc R . . C46 C 0.5500(3) -0.0366(2) 0.4444(3) 0.092(2) Uani 1 1 d . . . H46A H 0.5704 -0.0643 0.4260 0.110 Uiso 1 1 calc R . . H46B H 0.5136 -0.0481 0.4699 0.110 Uiso 1 1 calc R . . C47 C 0.5174(4) -0.0081(3) 0.4037(3) 0.133(3) Uani 1 1 d . E . H47A H 0.5532 0.0027 0.3774 0.159 Uiso 1 1 calc R . . H47B H 0.4973 0.0199 0.4217 0.159 Uiso 1 1 calc R . . C48 C 0.4590(5) -0.0339(3) 0.3716(4) 0.164(4) Uani 1 1 d . . . H48A H 0.4782 -0.0645 0.3594 0.197 Uiso 1 1 calc R D 1 H48B H 0.4212 -0.0409 0.3980 0.197 Uiso 1 1 calc R D 1 C49A C 0.4867(9) -0.0463(5) 0.3252(6) 0.129(6) Uani 0.50 1 d P E 21 H49A H 0.4519 -0.0627 0.3028 0.193 Uiso 0.50 1 calc PR E 21 H49B H 0.5263 -0.0671 0.3321 0.193 Uiso 0.50 1 calc PR E 21 H49C H 0.5027 -0.0183 0.3055 0.193 Uiso 0.50 1 calc PR E 21 C49 C 0.4326(10) -0.0157(7) 0.3319(7) 0.158(8) Uani 0.50 1 d P E 1 H49D H 0.4679 -0.0111 0.3034 0.237 Uiso 0.50 1 calc PR E 1 H49E H 0.4130 0.0148 0.3425 0.237 Uiso 0.50 1 calc PR E 1 H49F H 0.3954 -0.0359 0.3178 0.237 Uiso 0.50 1 calc PR E 1 N50 N 0.8105(2) 0.07331(16) 0.45253(16) 0.0625(12) Uani 1 1 d . . . N51 N 0.8157(2) 0.02721(18) 0.44594(17) 0.0695(13) Uani 1 1 d . . . N52 N 0.8590(2) 0.02120(19) 0.40306(18) 0.0778(15) Uani 1 1 d . . . C53 C 0.8806(3) 0.0626(3) 0.3819(2) 0.089(2) Uani 1 1 d . . . H53 H 0.9109 0.0673 0.3515 0.107 Uiso 1 1 calc R . . C54 C 0.8495(2) 0.0961(2) 0.4134(2) 0.0711(17) Uani 1 1 d . . . C55 C 0.8491(3) 0.1482(2) 0.4128(2) 0.0759(17) Uani 1 1 d . . . N56 N 0.8114(2) 0.16857(16) 0.45174(15) 0.0646(12) Uani 1 1 d . . . C57 C 0.8080(3) 0.2158(2) 0.4526(2) 0.0722(16) Uani 1 1 d . . . C58 C 0.7672(3) 0.2353(2) 0.4978(2) 0.0719(16) Uani 1 1 d . F . C59 C 0.7575(3) 0.2794(2) 0.5157(3) 0.088(2) Uani 1 1 d . F . H59 H 0.7763 0.3074 0.5005 0.106 Uiso 1 1 calc R . . N60 N 0.7152(3) 0.27558(17) 0.5599(2) 0.0889(17) Uani 1 1 d D . . N61 N 0.6992(3) 0.23077(17) 0.5683(2) 0.0786(15) Uani 1 1 d . F . N62 N 0.7304(2) 0.20594(16) 0.53049(18) 0.0644(12) Uani 1 1 d . . . C63 C 0.8827(3) 0.1753(3) 0.3717(3) 0.095(2) Uani 1 1 d . . . H63 H 0.9086 0.1603 0.3434 0.114 Uiso 1 1 calc R . . C64 C 0.8777(4) 0.2220(3) 0.3731(3) 0.109(2) Uani 1 1 d . . . H64 H 0.9011 0.2405 0.3464 0.131 Uiso 1 1 calc R . . C65 C 0.8393(3) 0.2429(3) 0.4127(3) 0.099(2) Uani 1 1 d . . . H65 H 0.8338 0.2760 0.4130 0.119 Uiso 1 1 calc R . . C66 C 0.8770(3) -0.0270(3) 0.3865(3) 0.104(2) Uani 1 1 d . . . H66A H 0.8868 -0.0274 0.3465 0.125 Uiso 1 1 calc R . . H66B H 0.8365 -0.0476 0.3932 0.125 Uiso 1 1 calc R . . C67 C 0.9395(4) -0.0466(3) 0.4169(3) 0.125(3) Uani 1 1 d . . . H67A H 0.9533 -0.0766 0.3993 0.150 Uiso 1 1 calc R . . H67B H 0.9789 -0.0245 0.4128 0.150 Uiso 1 1 calc R . . C68 C 0.9274(5) -0.0552(4) 0.4767(3) 0.150(4) Uani 1 1 d . . . H68A H 0.8887 -0.0778 0.4813 0.180 Uiso 1 1 calc R . . H68B H 0.9140 -0.0254 0.4948 0.180 Uiso 1 1 calc R . . C69 C 0.9934(5) -0.0747(5) 0.5040(4) 0.200(5) Uani 1 1 d . . . H69A H 1.0097 -0.1023 0.4836 0.300 Uiso 1 1 calc R . . H69B H 0.9829 -0.0838 0.5420 0.300 Uiso 1 1 calc R . . H69C H 1.0298 -0.0506 0.5040 0.300 Uiso 1 1 calc R . . C70 C 0.6854(5) 0.3135(4) 0.5987(6) 0.140(7) Uani 0.50 1 d PD F 2 H70C H 0.7174 0.3143 0.6306 0.168 Uiso 0.50 1 calc PR F 2 H70D H 0.6921 0.3436 0.5791 0.168 Uiso 0.50 1 calc PR F 2 C70A C 0.6849(5) 0.3121(4) 0.5959(5) 0.143(6) Uani 0.50 1 d PD F 1 H70A H 0.7192 0.3371 0.6035 0.171 Uiso 0.50 1 calc PR F 1 H70B H 0.6692 0.2984 0.6312 0.171 Uiso 0.50 1 calc PR F 1 C71 C 0.6130(6) 0.3161(4) 0.6228(5) 0.190(9) Uani 0.50 1 d PD F 2 H71A H 0.5794 0.3139 0.5921 0.228 Uiso 0.50 1 calc PR F 2 H71B H 0.6062 0.2880 0.6461 0.228 Uiso 0.50 1 calc PR F 2 C71A C 0.6236(5) 0.3311(5) 0.5633(7) 0.189(9) Uani 0.50 1 d PD F 1 H71C H 0.6024 0.3576 0.5835 0.227 Uiso 0.50 1 calc PR F 1 H71D H 0.6403 0.3430 0.5274 0.227 Uiso 0.50 1 calc PR F 1 C72 C 0.5945(7) 0.3575(4) 0.6559(5) 0.154(8) Uani 0.50 1 d PD F 2 H72A H 0.5435 0.3575 0.6616 0.185 Uiso 0.50 1 calc PR F 2 H72B H 0.6062 0.3860 0.6345 0.185 Uiso 0.50 1 calc PR F 2 C72A C 0.5698(6) 0.2941(5) 0.5538(9) 0.217(10) Uani 0.50 1 d PD F 1 H72C H 0.5888 0.2711 0.5273 0.260 Uiso 0.50 1 calc PR F 1 H72D H 0.5619 0.2774 0.5889 0.260 Uiso 0.50 1 calc PR F 1 C73 C 0.6302(6) 0.3609(4) 0.7120(4) 0.098(4) Uani 0.50 1 d PD F 2 H73A H 0.6371 0.3292 0.7269 0.146 Uiso 0.50 1 calc PR F 2 H73B H 0.6009 0.3791 0.7372 0.146 Uiso 0.50 1 calc PR F 2 H73C H 0.6754 0.3764 0.7079 0.146 Uiso 0.50 1 calc PR F 2 C73A C 0.5024(6) 0.3102(8) 0.5332(9) 0.258(13) Uani 0.50 1 d PD F 1 H73D H 0.4691 0.3119 0.5637 0.388 Uiso 0.50 1 calc PR F 1 H73E H 0.4852 0.2882 0.5054 0.388 Uiso 0.50 1 calc PR F 1 H73F H 0.5077 0.3414 0.5167 0.388 Uiso 0.50 1 calc PR F 1 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 Eu1 0.03768(10) 0.06368(13) 0.04405(11) -0.00193(11) 0.00632(10) -0.01282(11) Cl1 0.246(3) 0.0708(11) 0.0528(10) 0.0063(9) 0.0178(14) 0.0227(16) O1 0.290(12) 0.349(14) 0.230(10) -0.026(9) -0.084(9) 0.018(10) Cl2 0.0905(13) 0.0736(12) 0.0508(9) 0.000 -0.0185(9) 0.000 O2 0.522(18) 0.069(4) 0.091(4) 0.010(3) -0.038(8) -0.050(7) N2 0.058(2) 0.063(2) 0.043(2) -0.0066(17) 0.0034(17) -0.0102(19) O2A 0.035(8) 0.223(19) 0.48(4) -0.23(2) 0.052(14) -0.038(10) Cl3 0.0632(7) 0.1073(10) 0.0520(7) -0.0129(7) -0.0109(6) 0.0255(7) O3 0.190(6) 0.093(4) 0.101(4) 0.035(3) -0.030(4) -0.039(4) N3 0.052(2) 0.083(3) 0.048(2) -0.007(2) 0.0100(18) -0.012(2) Cl4 0.0990(19) 0.252(4) 0.0638(14) 0.000 -0.0115(13) 0.000 O4 0.102(3) 0.057(2) 0.085(3) -0.023(2) 0.003(3) -0.004(2) N4 0.075(3) 0.074(3) 0.044(2) -0.010(2) 0.012(2) -0.020(2) O15A 0.070(10) 0.095(12) 0.036(7) 0.000 -0.011(7) 0.000 O5 0.332(7) 0.179(5) 0.161(5) 0.103(4) 0.157(5) 0.182(5) C5 0.068(3) 0.057(3) 0.065(3) -0.021(2) 0.022(2) -0.018(2) O6 0.446(14) 0.158(5) 0.173(7) 0.098(5) -0.039(9) -0.175(7) C6 0.047(2) 0.041(2) 0.059(3) -0.014(2) 0.017(2) -0.015(2) O6A 0.097(14) 0.127(18) 0.106(16) 0.011(14) -0.039(12) 0.050(13) O7 0.068(3) 0.091(3) 0.069(3) 0.008(3) 0.004(2) 0.004(3) C7 0.055(3) 0.040(2) 0.065(3) -0.011(2) 0.011(2) -0.010(2) O7A 0.113(16) 0.069(11) 0.089(13) -0.039(10) -0.011(12) 0.038(11) O8 0.073(3) 0.094(4) 0.139(5) -0.010(3) -0.001(3) 0.028(3) N8 0.0466(19) 0.047(2) 0.049(2) -0.0048(17) 0.0035(16) -0.0087(17) O9 0.104(4) 0.158(5) 0.072(3) -0.022(3) -0.006(3) 0.039(4) C9 0.048(2) 0.048(2) 0.065(3) -0.001(2) -0.002(2) -0.006(2) O10 0.041(2) 0.108(3) 0.050(2) -0.007(2) -0.0079(17) 0.011(2) C10 0.042(2) 0.054(3) 0.066(3) 0.002(2) -0.007(2) -0.012(2) O11 0.092(3) 0.148(4) 0.181(5) 0.104(4) -0.074(3) -0.055(3) C11 0.051(3) 0.067(3) 0.061(3) 0.006(2) -0.013(2) -0.011(2) O11A 0.231(9) 2.00(6) 0.094(7) 0.110(17) 0.056(6) 0.494(19) O12 0.17(2) 1.64(4) 0.437(16) 0.821(19) 0.081(16) 0.23(3) N12 0.066(3) 0.079(3) 0.053(2) 0.009(2) -0.005(2) -0.020(2) N13 0.050(2) 0.103(3) 0.045(2) 0.012(2) -0.0057(17) -0.026(2) O13A 0.103(7) 0.147(9) 0.052(6) 0.009(6) 0.013(5) 0.098(6) N14 0.054(2) 0.080(3) 0.049(2) 0.004(2) 0.0044(18) -0.024(2) O14A 0.089(10) 0.44(3) 0.078(9) 0.009(14) 0.009(7) -0.044(14) C15 0.058(3) 0.074(3) 0.083(4) -0.027(3) 0.005(3) 0.015(3) C16 0.059(3) 0.094(4) 0.114(5) -0.033(4) -0.003(3) 0.029(3) C17 0.057(3) 0.073(3) 0.084(4) -0.015(3) -0.008(3) 0.017(3) C18 0.111(4) 0.086(4) 0.046(3) -0.008(3) 0.011(3) -0.036(4) C19 0.149(6) 0.109(5) 0.050(3) -0.002(3) 0.000(4) -0.049(5) C20 0.192(8) 0.126(5) 0.075(4) 0.003(4) 0.009(5) -0.091(5) C21 0.205(9) 0.118(6) 0.126(7) -0.011(5) 0.014(7) -0.077(6) C22 0.093(4) 0.097(4) 0.044(3) 0.004(3) -0.004(3) -0.019(3) C23 0.216(9) 0.099(5) 0.066(4) 0.012(4) -0.036(5) -0.047(6) C24 0.566(19) 0.113(6) 0.090(5) -0.022(5) -0.123(8) 0.140(9) C25 0.186(11) 0.58(3) 0.114(9) 0.063(13) 0.024(8) 0.149(15) N26 0.0374(19) 0.101(3) 0.062(3) -0.001(2) -0.0021(18) -0.015(2) N27 0.056(3) 0.130(4) 0.086(3) 0.005(3) -0.020(2) -0.036(3) N28 0.058(3) 0.140(5) 0.085(3) -0.003(3) -0.017(3) -0.027(3) C29 0.046(3) 0.160(6) 0.056(3) 0.005(4) -0.001(2) -0.012(4) C30 0.040(2) 0.104(4) 0.053(3) 0.000(3) 0.002(2) 0.002(3) C31 0.053(3) 0.096(4) 0.060(3) 0.008(3) 0.006(2) 0.008(3) N32 0.046(2) 0.075(3) 0.048(2) -0.001(2) 0.0114(17) -0.0015(19) C33 0.063(3) 0.066(3) 0.071(3) 0.006(3) 0.015(3) 0.006(3) C34 0.058(3) 0.062(3) 0.069(3) -0.010(3) 0.018(2) -0.006(3) C35 0.089(4) 0.049(3) 0.095(4) -0.018(3) 0.025(3) -0.010(3) N36 0.060(2) 0.054(2) 0.093(3) -0.019(2) 0.013(2) -0.012(2) N37 0.042(2) 0.055(2) 0.088(3) -0.018(2) 0.007(2) -0.0136(18) N38 0.0414(19) 0.052(2) 0.067(2) -0.0080(19) 0.0108(18) -0.0049(18) C39 0.090(5) 0.122(6) 0.117(6) 0.035(5) -0.016(4) 0.005(4) C40 0.140(7) 0.104(5) 0.173(8) 0.050(5) -0.028(6) 0.030(5) C41 0.106(5) 0.077(4) 0.145(6) 0.032(4) -0.018(5) 0.004(4) C42 0.098(4) 0.175(7) 0.128(6) 0.006(5) -0.057(4) -0.059(5) C43 0.056(4) 0.170(7) 0.264(11) -0.064(7) -0.026(5) -0.054(4) C44 0.195(11) 0.237(13) 0.142(9) 0.025(9) -0.023(8) 0.040(10) C45 0.191(7) 0.245(10) 0.320(11) 0.147(8) 0.189(7) 0.135(7) C46 0.066(3) 0.080(4) 0.130(5) -0.051(4) 0.013(4) -0.024(3) C47 0.166(6) 0.113(5) 0.119(6) 0.024(4) -0.053(5) -0.081(5) C48 0.190(8) 0.167(7) 0.135(7) -0.059(6) 0.037(6) -0.110(6) C49A 0.157(13) 0.117(9) 0.113(10) 0.060(8) -0.004(10) -0.074(9) C49 0.179(15) 0.180(18) 0.114(11) 0.035(12) -0.087(11) -0.002(14) N50 0.044(2) 0.093(3) 0.050(2) -0.010(2) 0.0098(18) -0.012(2) N51 0.044(2) 0.102(3) 0.062(3) -0.012(2) 0.0180(19) -0.004(2) N52 0.057(2) 0.112(4) 0.064(3) -0.016(3) 0.023(2) 0.013(3) C53 0.053(3) 0.157(6) 0.058(3) 0.009(4) 0.021(3) 0.001(4) C54 0.037(2) 0.130(5) 0.047(3) -0.001(3) 0.013(2) -0.022(3) C55 0.052(3) 0.118(4) 0.057(3) 0.012(3) 0.007(2) -0.037(3) N56 0.048(2) 0.103(3) 0.043(2) 0.005(2) 0.0055(17) -0.035(2) C57 0.058(3) 0.081(3) 0.077(3) 0.020(3) -0.013(3) -0.046(3) C58 0.061(3) 0.080(3) 0.075(3) 0.014(3) -0.008(3) -0.035(3) C59 0.079(4) 0.067(3) 0.118(5) 0.001(4) -0.026(4) -0.033(3) N60 0.072(3) 0.076(3) 0.119(4) -0.007(3) -0.005(3) -0.028(3) N61 0.073(3) 0.069(3) 0.094(3) -0.011(3) 0.007(3) -0.020(3) N62 0.055(2) 0.066(3) 0.072(3) 0.002(2) -0.002(2) -0.023(2) C63 0.065(3) 0.140(6) 0.080(4) 0.016(4) 0.025(3) -0.031(4) C64 0.098(4) 0.136(5) 0.093(5) 0.040(4) 0.010(4) -0.060(4) C65 0.085(4) 0.123(5) 0.090(4) 0.036(4) -0.011(3) -0.064(4) C66 0.083(4) 0.139(6) 0.090(4) -0.023(4) 0.035(3) 0.023(4) C67 0.097(5) 0.168(7) 0.110(5) -0.013(5) 0.040(4) 0.032(5) C68 0.120(6) 0.217(10) 0.114(6) 0.021(6) 0.027(5) 0.061(7) C69 0.148(8) 0.309(14) 0.143(8) 0.019(9) -0.006(7) 0.107(9) C70 0.088(8) 0.055(8) 0.277(18) -0.009(10) -0.106(10) -0.009(7) C70A 0.146(11) 0.078(10) 0.204(13) -0.068(9) 0.125(10) -0.023(9) C71 0.081(9) 0.31(2) 0.180(16) 0.109(16) -0.035(10) -0.103(12) C71A 0.194(15) 0.128(12) 0.24(2) -0.043(13) 0.069(16) 0.097(12) C72 0.235(19) 0.035(7) 0.193(16) -0.014(8) -0.093(15) -0.004(10) C72A 0.24(2) 0.151(15) 0.26(2) -0.109(15) -0.112(19) 0.101(15) C73 0.064(6) 0.066(6) 0.163(12) 0.041(7) 0.036(7) -0.032(6) C73A 0.25(2) 0.15(2) 0.37(3) -0.02(2) 0.19(2) -0.010(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 N50 2.499(4) . ? Eu1 N14 2.503(4) . ? Eu1 N26 2.511(4) . ? Eu1 N38 2.517(4) . ? Eu1 N62 2.518(4) . ? Eu1 N2 2.524(4) . ? Eu1 N32 2.565(4) . ? Eu1 N8 2.586(4) . ? Eu1 N56 2.599(4) . ? Cl1 O4 1.397(4) . ? Cl1 O5 1.413(8) . ? Cl1 O2 1.414(8) . ? Cl1 O3 1.448(8) . ? Cl1A O4A 1.35(6) . ? Cl1A O2A 1.41(2) . ? Cl1A O3A 1.41(3) . ? Cl2 O6 1.323(9) . ? Cl2 O6 1.324(9) 4_656 ? Cl2 O7 1.460(5) 4_656 ? Cl2 O7 1.460(5) . ? N2 N3 1.303(5) . ? N2 C6 1.362(6) . ? Cl3 O11 1.333(6) . ? Cl3 O10 1.422(4) . ? Cl3 O8 1.441(5) . ? Cl3 O9 1.443(5) . ? N3 N4 1.337(6) . ? O3A O4A 1.58(6) . ? Cl4 O13 1.360(11) . ? Cl4 O13 1.360(11) 4_556 ? Cl4 O13A 1.460(10) 4_556 ? Cl4 O13A 1.460(10) . ? Cl4 O15A 1.471(17) . ? Cl4 O12 1.49(3) 4_556 ? Cl4 O12 1.49(3) . ? Cl4 O14A 1.622(16) 4_556 ? Cl4 O14A 1.622(16) . ? Cl4 O11A 2.10(3) 4_556 ? Cl4 O11A 2.10(3) . ? N4 C5 1.328(7) . ? N4 C18 1.459(6) . ? O15A O11A 1.290(12) . ? O15A O11A 1.290(12) 4_556 ? O15A O13 1.296(14) . ? O15A O13 1.296(14) 4_556 ? O15A O14A 1.68(2) 4_556 ? O15A O14A 1.68(2) . ? C5 C6 1.381(6) . ? C5 H5 0.9500 . ? C6 C7 1.439(7) . ? O6A O7A 1.56(3) . ? O6A O8A 1.70(3) 4_656 ? O6A O6A 1.72(4) 4_656 ? C7 N8 1.343(6) . ? C7 C15 1.394(7) . ? N8 C9 1.346(6) . ? O8A O6A 1.70(3) 4_656 ? C9 C17 1.384(7) . ? C9 C10 1.459(7) . ? C10 C11 1.361(7) . ? C10 N14 1.376(6) . ? C11 N12 1.348(7) . ? C11 H11 0.9500 . ? O11A O13 0.92(3) 4_556 ? O12 O13A 1.26(3) . ? O12 O12 1.41(5) 4_556 ? O12 O13A 1.41(3) 4_556 ? N12 N13 1.328(6) . ? N12 C22 1.464(6) . ? O13 O11A 0.92(3) 4_556 ? O13 O14A 1.756(18) . ? N13 N14 1.315(6) . ? O13A O12 1.41(3) 4_556 ? O13A O14A 1.71(3) . ? C15 C16 1.361(8) . ? C15 H15 0.9500 . ? C16 C17 1.385(8) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.535(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.409(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.564(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.514(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.550(14) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.197(17) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? N26 N27 1.331(7) . ? N26 C30 1.362(7) . ? N27 N28 1.342(7) . ? N28 C29 1.328(9) . ? N28 C42 1.462(9) . ? C29 C30 1.375(8) . ? C29 H29 0.9500 . ? C30 C31 1.426(8) . ? C31 N32 1.345(6) . ? C31 C39 1.372(9) . ? N32 C33 1.342(7) . ? C33 C41 1.379(9) . ? C33 C34 1.446(7) . ? C34 C35 1.355(7) . ? C34 N38 1.368(6) . ? C35 N36 1.311(7) . ? C35 H35 0.9500 . ? N36 N37 1.336(6) . ? N36 C46 1.475(7) . ? N37 N38 1.314(5) . ? C39 C40 1.369(11) . ? C39 H39 0.9500 . ? C40 C41 1.383(11) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.664(11) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.402(13) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.537(14) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.424(10) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.552(11) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.207(17) . ? C48 C49A 1.296(17) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49A H49A 0.9800 . ? C49A H49B 0.9800 . ? C49A H49C 0.9800 . ? C49 H49D 0.9800 . ? C49 H49E 0.9800 . ? C49 H49F 0.9800 . ? N50 N51 1.327(6) . ? N50 C54 1.373(6) . ? N51 N52 1.345(6) . ? N52 C53 1.352(8) . ? N52 C66 1.472(8) . ? C53 C54 1.363(9) . ? C53 H53 0.9500 . ? C54 C55 1.486(9) . ? C55 N56 1.325(7) . ? C55 C63 1.419(8) . ? N56 C57 1.348(7) . ? C57 C65 1.377(8) . ? C57 C58 1.461(8) . ? C58 C59 1.344(9) . ? C58 N62 1.354(7) . ? C59 N60 1.352(8) . ? C59 H59 0.9500 . ? N60 N61 1.329(7) . ? N60 C70A 1.478(11) . ? N60 C70 1.543(11) . ? N61 N62 1.307(6) . ? C63 C64 1.336(10) . ? C63 H63 0.9500 . ? C64 C65 1.350(10) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 C67 1.516(10) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.493(11) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.536(13) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.510(13) . ? C70 H70C 0.9900 . ? C70 H70D 0.9900 . ? C70A C71A 1.520(14) . ? C70A H70A 0.9900 . ? C70A H70B 0.9900 . ? C71 C72 1.471(12) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C71A C72A 1.493(14) . ? C71A H71C 0.9900 . ? C71A H71D 0.9900 . ? C72 C73 1.531(13) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C72A C73A 1.462(15) . ? C72A H72C 0.9900 . ? C72A H72D 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C73A H73D 0.9800 . ? C73A H73E 0.9800 . ? C73A H73F 0.9800 . ? 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 N50 Eu1 N14 78.37(13) . . ? N50 Eu1 N26 87.75(13) . . ? N14 Eu1 N26 149.38(14) . . ? N50 Eu1 N38 77.98(13) . . ? N14 Eu1 N38 75.12(13) . . ? N26 Eu1 N38 128.71(14) . . ? N50 Eu1 N62 127.52(14) . . ? N14 Eu1 N62 89.56(14) . . ? N26 Eu1 N62 77.40(15) . . ? N38 Eu1 N62 147.45(13) . . ? N50 Eu1 N2 147.98(13) . . ? N14 Eu1 N2 127.87(13) . . ? N26 Eu1 N2 76.09(13) . . ? N38 Eu1 N2 90.70(12) . . ? N62 Eu1 N2 76.12(13) . . ? N50 Eu1 N32 73.57(13) . . ? N14 Eu1 N32 134.45(13) . . ? N26 Eu1 N32 64.20(14) . . ? N38 Eu1 N32 64.51(13) . . ? N62 Eu1 N32 135.98(13) . . ? N2 Eu1 N32 74.52(12) . . ? N50 Eu1 N8 137.77(12) . . ? N14 Eu1 N8 64.18(12) . . ? N26 Eu1 N8 134.49(13) . . ? N38 Eu1 N8 74.27(12) . . ? N62 Eu1 N8 73.21(12) . . ? N2 Eu1 N8 63.69(12) . . ? N32 Eu1 N8 119.71(11) . . ? N50 Eu1 N56 64.32(14) . . ? N14 Eu1 N56 72.06(12) . . ? N26 Eu1 N56 77.34(13) . . ? N38 Eu1 N56 133.79(13) . . ? N62 Eu1 N56 63.36(14) . . ? N2 Eu1 N56 135.29(13) . . ? N32 Eu1 N56 123.16(13) . . ? N8 Eu1 N56 117.12(13) . . ? O4 Cl1 O5 111.2(5) . . ? O4 Cl1 O2 107.7(3) . . ? O5 Cl1 O2 110.0(6) . . ? O4 Cl1 O3 109.1(3) . . ? O5 Cl1 O3 107.6(4) . . ? O2 Cl1 O3 111.2(6) . . ? O4A Cl1A O2A 138(2) . . ? O4A Cl1A O3A 70(3) . . ? O2A Cl1A O3A 90.8(18) . . ? O6 Cl2 O6 118.0(9) . 4_656 ? O6 Cl2 O7 108.8(5) . 4_656 ? O6 Cl2 O7 111.6(6) 4_656 4_656 ? O6 Cl2 O7 111.6(6) . . ? O6 Cl2 O7 108.8(5) 4_656 . ? O7 Cl2 O7 95.9(4) 4_656 . ? N3 N2 C6 110.5(4) . . ? N3 N2 Eu1 128.6(3) . . ? C6 N2 Eu1 119.6(3) . . ? O11 Cl3 O10 112.1(3) . . ? O11 Cl3 O8 104.0(4) . . ? O10 Cl3 O8 109.1(3) . . ? O11 Cl3 O9 122.8(4) . . ? O10 Cl3 O9 106.2(3) . . ? O8 Cl3 O9 101.6(3) . . ? N2 N3 N4 106.2(4) . . ? O13 Cl4 O13 108.6(9) . 4_556 ? O13 Cl4 O12 97.6(15) . 4_556 ? O13 Cl4 O12 153.5(15) 4_556 4_556 ? O13 Cl4 O12 153.5(15) . . ? O13 Cl4 O12 97.6(15) 4_556 . ? O12 Cl4 O12 57(3) 4_556 . ? C5 N4 N3 111.7(4) . . ? C5 N4 C18 127.4(5) . . ? N3 N4 C18 120.8(5) . . ? N4 C5 C6 105.4(4) . . ? N4 C5 H5 127.3 . . ? C6 C5 H5 127.3 . . ? N2 C6 C5 106.1(4) . . ? N2 C6 C7 119.7(4) . . ? C5 C6 C7 134.1(4) . . ? O7A O6A O8A 89.1(16) . 4_656 ? O7A O6A O6A 96.5(15) . 4_656 ? O8A O6A O6A 87.5(15) 4_656 4_656 ? N8 C7 C15 121.8(5) . . ? N8 C7 C6 115.6(4) . . ? C15 C7 C6 122.6(4) . . ? C7 N8 C9 119.1(4) . . ? C7 N8 Eu1 120.5(3) . . ? C9 N8 Eu1 120.3(3) . . ? N8 C9 C17 122.0(5) . . ? N8 C9 C10 115.8(4) . . ? C17 C9 C10 122.2(5) . . ? C11 C10 N14 108.0(4) . . ? C11 C10 C9 133.7(4) . . ? N14 C10 C9 118.3(4) . . ? N12 C11 C10 105.2(4) . . ? N12 C11 H11 127.4 . . ? C10 C11 H11 127.4 . . ? O12 O12 Cl4 61.7(15) 4_556 . ? O13A O12 Cl4 60.5(12) 4_556 . ? N13 N12 C11 110.7(4) . . ? N13 N12 C22 121.1(5) . . ? C11 N12 C22 128.2(5) . . ? N14 N13 N12 108.2(4) . . ? N13 N14 C10 107.9(4) . . ? N13 N14 Eu1 130.7(3) . . ? C10 N14 Eu1 120.4(3) . . ? C16 C15 C7 118.2(5) . . ? C16 C15 H15 120.9 . . ? C7 C15 H15 120.9 . . ? C15 C16 C17 121.1(5) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C9 C17 C16 117.8(5) . . ? C9 C17 H17 121.1 . . ? C16 C17 H17 121.1 . . ? N4 C18 C19 110.6(5) . . ? N4 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C18 117.8(6) . . ? C20 C19 H19A 107.9 . . ? C18 C19 H19A 107.9 . . ? C20 C19 H19B 107.9 . . ? C18 C19 H19B 107.9 . . ? H19A C19 H19B 107.2 . . ? C19 C20 C21 112.8(7) . . ? C19 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N12 C22 C23 111.2(5) . . ? N12 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? N12 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 113.5(7) . . ? C22 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? C22 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C25 C24 C23 130.3(10) . . ? C25 C24 H24A 104.7 . . ? C23 C24 H24A 104.7 . . ? C25 C24 H24B 104.7 . . ? C23 C24 H24B 104.7 . . ? H24A C24 H24B 105.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N27 N26 C30 110.8(4) . . ? N27 N26 Eu1 128.2(4) . . ? C30 N26 Eu1 119.1(3) . . ? N26 N27 N28 105.4(5) . . ? C29 N28 N27 111.3(5) . . ? C29 N28 C42 129.2(6) . . ? N27 N28 C42 119.5(6) . . ? N28 C29 C30 107.0(5) . . ? N28 C29 H29 126.5 . . ? C30 C29 H29 126.5 . . ? N26 C30 C29 105.5(5) . . ? N26 C30 C31 119.8(5) . . ? C29 C30 C31 134.6(6) . . ? N32 C31 C39 122.1(6) . . ? N32 C31 C30 116.0(5) . . ? C39 C31 C30 121.8(6) . . ? C33 N32 C31 120.1(5) . . ? C33 N32 Eu1 119.8(3) . . ? C31 N32 Eu1 120.1(4) . . ? N32 C33 C41 120.9(6) . . ? N32 C33 C34 117.3(5) . . ? C41 C33 C34 121.8(6) . . ? C35 C34 N38 106.9(5) . . ? C35 C34 C33 134.7(5) . . ? N38 C34 C33 118.4(5) . . ? N36 C35 C34 106.7(5) . . ? N36 C35 H35 126.7 . . ? C34 C35 H35 126.7 . . ? C35 N36 N37 110.9(4) . . ? C35 N36 C46 129.2(5) . . ? N37 N36 C46 119.8(5) . . ? N38 N37 N36 106.9(4) . . ? N37 N38 C34 108.6(4) . . ? N37 N38 Eu1 131.0(3) . . ? C34 N38 Eu1 119.8(3) . . ? C40 C39 C31 117.3(7) . . ? C40 C39 H39 121.4 . . ? C31 C39 H39 121.4 . . ? C39 C40 C41 121.7(7) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C33 C41 C40 117.9(7) . . ? C33 C41 H41 121.1 . . ? C40 C41 H41 121.1 . . ? N28 C42 C43 107.3(6) . . ? N28 C42 H42A 110.2 . . ? C43 C42 H42A 110.2 . . ? N28 C42 H42B 110.2 . . ? C43 C42 H42B 110.2 . . ? H42A C42 H42B 108.5 . . ? C44 C43 C42 108.4(8) . . ? C44 C43 H43A 110.0 . . ? C42 C43 H43A 110.0 . . ? C44 C43 H43B 110.0 . . ? C42 C43 H43B 110.0 . . ? H43A C43 H43B 108.4 . . ? C43 C44 C45 103.0(9) . . ? C43 C44 H44A 111.2 . . ? C45 C44 H44A 111.2 . . ? C43 C44 H44B 111.2 . . ? C45 C44 H44B 111.2 . . ? H44A C44 H44B 109.1 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 N36 116.0(5) . . ? C47 C46 H46A 108.3 . . ? N36 C46 H46A 108.3 . . ? C47 C46 H46B 108.3 . . ? N36 C46 H46B 108.3 . . ? H46A C46 H46B 107.4 . . ? C46 C47 C48 113.5(6) . . ? C46 C47 H47A 108.9 . . ? C48 C47 H47A 108.9 . . ? C46 C47 H47B 108.9 . . ? C48 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? C49 C48 C49A 66.0(12) . . ? C49 C48 C47 120.1(12) . . ? C49A C48 C47 105.7(10) . . ? C49 C48 H48A 107.3 . . ? C49A C48 H48A 49.4 . . ? C47 C48 H48A 107.3 . . ? C49 C48 H48B 107.3 . . ? C49A C48 H48B 144.3 . . ? C47 C48 H48B 107.3 . . ? H48A C48 H48B 106.9 . . ? C48 C49A H49A 109.5 . . ? C48 C49A H49B 109.5 . . ? C48 C49A H49C 109.5 . . ? C48 C49 H49D 109.5 . . ? C48 C49 H49E 109.5 . . ? C48 C49 H49F 109.5 . . ? N51 N50 C54 110.0(4) . . ? N51 N50 Eu1 129.0(3) . . ? C54 N50 Eu1 120.7(4) . . ? N50 N51 N52 105.5(4) . . ? N51 N52 C53 112.0(5) . . ? N51 N52 C66 118.5(5) . . ? C53 N52 C66 129.6(5) . . ? N52 C53 C54 105.2(5) . . ? N52 C53 H53 127.4 . . ? C54 C53 H53 127.4 . . ? C53 C54 N50 107.4(6) . . ? C53 C54 C55 134.1(5) . . ? N50 C54 C55 118.5(5) . . ? N56 C55 C63 120.9(6) . . ? N56 C55 C54 115.7(5) . . ? C63 C55 C54 123.3(5) . . ? C55 N56 C57 118.3(5) . . ? C55 N56 Eu1 120.4(4) . . ? C57 N56 Eu1 120.9(3) . . ? N56 C57 C65 121.9(6) . . ? N56 C57 C58 114.6(4) . . ? C65 C57 C58 123.5(6) . . ? C59 C58 N62 108.4(5) . . ? C59 C58 C57 132.4(5) . . ? N62 C58 C57 119.2(5) . . ? C58 C59 N60 105.4(5) . . ? C58 C59 H59 127.3 . . ? N60 C59 H59 127.3 . . ? N61 N60 C59 109.8(5) . . ? N61 N60 C70A 119.6(7) . . ? C59 N60 C70A 130.6(7) . . ? N61 N60 C70 119.5(6) . . ? C59 N60 C70 130.7(6) . . ? C70A N60 C70 1.7(7) . . ? N62 N61 N60 107.8(5) . . ? N61 N62 C58 108.6(5) . . ? N61 N62 Eu1 130.0(3) . . ? C58 N62 Eu1 121.3(4) . . ? C64 C63 C55 119.4(6) . . ? C64 C63 H63 120.3 . . ? C55 C63 H63 120.3 . . ? C63 C64 C65 119.7(6) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C64 C65 C57 119.6(7) . . ? C64 C65 H65 120.2 . . ? C57 C65 H65 120.2 . . ? N52 C66 C67 113.4(6) . . ? N52 C66 H66A 108.9 . . ? C67 C66 H66A 108.9 . . ? N52 C66 H66B 108.9 . . ? C67 C66 H66B 108.9 . . ? H66A C66 H66B 107.7 . . ? C68 C67 C66 114.3(6) . . ? C68 C67 H67A 108.7 . . ? C66 C67 H67A 108.7 . . ? C68 C67 H67B 108.7 . . ? C66 C67 H67B 108.7 . . ? H67A C67 H67B 107.6 . . ? C67 C68 C69 110.7(7) . . ? C67 C68 H68A 109.5 . . ? C69 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? C69 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C71 C70 N60 127.9(8) . . ? C71 C70 H70C 105.3 . . ? N60 C70 H70C 105.3 . . ? C71 C70 H70D 105.3 . . ? N60 C70 H70D 105.3 . . ? H70C C70 H70D 106.0 . . ? N60 C70A C71A 104.3(9) . . ? N60 C70A H70A 110.9 . . ? C71A C70A H70A 110.9 . . ? N60 C70A H70B 110.9 . . ? C71A C70A H70B 110.9 . . ? H70A C70A H70B 108.9 . . ? C72 C71 C70 118.4(10) . . ? C72 C71 H71A 107.7 . . ? C70 C71 H71A 107.7 . . ? C72 C71 H71B 107.7 . . ? C70 C71 H71B 107.7 . . ? H71A C71 H71B 107.1 . . ? C72A C71A C70A 111.4(11) . . ? C72A C71A H71C 109.3 . . ? C70A C71A H71C 109.3 . . ? C72A C71A H71D 109.3 . . ? C70A C71A H71D 109.3 . . ? H71C C71A H71D 108.0 . . ? C71 C72 C73 115.4(10) . . ? C71 C72 H72A 108.4 . . ? C73 C72 H72A 108.4 . . ? C71 C72 H72B 108.4 . . ? C73 C72 H72B 108.4 . . ? H72A C72 H72B 107.5 . . ? C73A C72A C71A 116.3(13) . . ? C73A C72A H72C 108.2 . . ? C71A C72A H72C 108.2 . . ? C73A C72A H72D 108.2 . . ? C71A C72A H72D 108.2 . . ? H72C C72A H72D 107.4 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? 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 N50 Eu1 N2 N3 45.9(5) . . . . ? N14 Eu1 N2 N3 -174.4(3) . . . . ? N26 Eu1 N2 N3 -15.9(4) . . . . ? N38 Eu1 N2 N3 114.0(4) . . . . ? N62 Eu1 N2 N3 -96.1(4) . . . . ? N32 Eu1 N2 N3 50.7(4) . . . . ? N8 Eu1 N2 N3 -174.0(4) . . . . ? N56 Eu1 N2 N3 -71.1(4) . . . . ? N50 Eu1 N2 C6 -147.9(3) . . . . ? N14 Eu1 N2 C6 -8.3(4) . . . . ? N26 Eu1 N2 C6 150.3(3) . . . . ? N38 Eu1 N2 C6 -79.8(3) . . . . ? N62 Eu1 N2 C6 70.1(3) . . . . ? N32 Eu1 N2 C6 -143.1(3) . . . . ? N8 Eu1 N2 C6 -7.8(3) . . . . ? N56 Eu1 N2 C6 95.1(3) . . . . ? C6 N2 N3 N4 0.4(5) . . . . ? Eu1 N2 N3 N4 167.6(3) . . . . ? O2A Cl1A O3A O4A -142(2) . . . . ? N2 N3 N4 C5 0.6(5) . . . . ? N2 N3 N4 C18 -176.2(4) . . . . ? N3 N4 C5 C6 -1.2(6) . . . . ? C18 N4 C5 C6 175.3(5) . . . . ? N3 N2 C6 C5 -1.1(5) . . . . ? Eu1 N2 C6 C5 -169.6(3) . . . . ? N3 N2 C6 C7 178.8(4) . . . . ? Eu1 N2 C6 C7 10.3(5) . . . . ? N4 C5 C6 N2 1.4(5) . . . . ? N4 C5 C6 C7 -178.5(5) . . . . ? N2 C6 C7 N8 -5.0(6) . . . . ? C5 C6 C7 N8 174.8(5) . . . . ? N2 C6 C7 C15 175.3(4) . . . . ? C5 C6 C7 C15 -4.9(8) . . . . ? C15 C7 N8 C9 -0.3(7) . . . . ? C6 C7 N8 C9 180.0(4) . . . . ? C15 C7 N8 Eu1 177.2(4) . . . . ? C6 C7 N8 Eu1 -2.5(5) . . . . ? N50 Eu1 N8 C7 154.9(3) . . . . ? N14 Eu1 N8 C7 -175.1(4) . . . . ? N26 Eu1 N8 C7 -25.2(4) . . . . ? N38 Eu1 N8 C7 104.2(3) . . . . ? N62 Eu1 N8 C7 -77.2(3) . . . . ? N2 Eu1 N8 C7 5.3(3) . . . . ? N32 Eu1 N8 C7 56.7(4) . . . . ? N56 Eu1 N8 C7 -124.3(3) . . . . ? N50 Eu1 N8 C9 -27.6(4) . . . . ? N14 Eu1 N8 C9 2.4(3) . . . . ? N26 Eu1 N8 C9 152.3(3) . . . . ? N38 Eu1 N8 C9 -78.4(3) . . . . ? N62 Eu1 N8 C9 100.3(3) . . . . ? N2 Eu1 N8 C9 -177.2(4) . . . . ? N32 Eu1 N8 C9 -125.9(3) . . . . ? N56 Eu1 N8 C9 53.2(4) . . . . ? C7 N8 C9 C17 0.8(7) . . . . ? Eu1 N8 C9 C17 -176.7(4) . . . . ? C7 N8 C9 C10 -180.0(4) . . . . ? Eu1 N8 C9 C10 2.5(5) . . . . ? N8 C9 C10 C11 171.5(5) . . . . ? C17 C9 C10 C11 -9.3(9) . . . . ? N8 C9 C10 N14 -9.6(6) . . . . ? C17 C9 C10 N14 169.6(5) . . . . ? N14 C10 C11 N12 -0.6(5) . . . . ? C9 C10 C11 N12 178.4(5) . . . . ? N12 N13 N14 C10 -1.4(5) . . . . ? N12 N13 N14 Eu1 166.9(3) . . . . ? C11 C10 N14 N13 1.2(5) . . . . ? C9 C10 N14 N13 -177.9(4) . . . . ? C11 C10 N14 Eu1 -168.5(3) . . . . ? C9 C10 N14 Eu1 12.3(6) . . . . ? N50 Eu1 N14 N13 -14.7(4) . . . . ? N26 Eu1 N14 N13 50.0(6) . . . . ? N38 Eu1 N14 N13 -95.2(4) . . . . ? N62 Eu1 N14 N13 113.8(4) . . . . ? N2 Eu1 N14 N13 -174.2(4) . . . . ? N32 Eu1 N14 N13 -67.4(5) . . . . ? N8 Eu1 N14 N13 -174.7(5) . . . . ? N56 Eu1 N14 N13 51.8(4) . . . . ? N50 Eu1 N14 C10 152.3(4) . . . . ? N26 Eu1 N14 C10 -142.9(3) . . . . ? N38 Eu1 N14 C10 71.8(3) . . . . ? N62 Eu1 N14 C10 -79.1(4) . . . . ? N2 Eu1 N14 C10 -7.2(4) . . . . ? N32 Eu1 N14 C10 99.7(4) . . . . ? N8 Eu1 N14 C10 -7.6(3) . . . . ? N56 Eu1 N14 C10 -141.1(4) . . . . ? N8 C7 C15 C16 0.3(8) . . . . ? C6 C7 C15 C16 -180.0(5) . . . . ? C7 C15 C16 C17 -0.8(9) . . . . ? N8 C9 C17 C16 -1.3(8) . . . . ? C10 C9 C17 C16 179.5(5) . . . . ? C15 C16 C17 C9 1.3(9) . . . . ? C5 N4 C18 C19 -81.4(7) . . . . ? N3 N4 C18 C19 94.9(6) . . . . ? N4 C18 C19 C20 -61.2(8) . . . . ? C18 C19 C20 C21 -179.8(6) . . . . ? N13 N12 C22 C23 91.5(7) . . . . ? C11 N12 C22 C23 -87.2(7) . . . . ? N12 C22 C23 C24 -70.3(8) . . . . ? C22 C23 C24 C25 -135.3(17) . . . . ? N50 Eu1 N26 N27 117.3(4) . . . . ? N14 Eu1 N26 N27 54.9(6) . . . . ? N38 Eu1 N26 N27 -170.1(4) . . . . ? N62 Eu1 N26 N27 -12.0(4) . . . . ? N2 Eu1 N26 N27 -90.6(4) . . . . ? N32 Eu1 N26 N27 -169.9(5) . . . . ? N8 Eu1 N26 N27 -62.6(5) . . . . ? N56 Eu1 N26 N27 53.1(4) . . . . ? N50 Eu1 N26 C30 -80.0(4) . . . . ? N14 Eu1 N26 C30 -142.4(4) . . . . ? N38 Eu1 N26 C30 -7.3(4) . . . . ? N62 Eu1 N26 C30 150.7(4) . . . . ? N2 Eu1 N26 C30 72.1(4) . . . . ? N32 Eu1 N26 C30 -7.2(3) . . . . ? N8 Eu1 N26 C30 100.1(4) . . . . ? N56 Eu1 N26 C30 -144.1(4) . . . . ? C30 N26 N27 N28 0.8(6) . . . . ? Eu1 N26 N27 N28 164.7(3) . . . . ? N26 N27 N28 C29 -0.5(6) . . . . ? N26 N27 N28 C42 178.3(5) . . . . ? N27 N28 C29 C30 0.0(7) . . . . ? C42 N28 C29 C30 -178.7(6) . . . . ? N27 N26 C30 C29 -0.8(6) . . . . ? Eu1 N26 C30 C29 -166.3(3) . . . . ? N27 N26 C30 C31 176.4(5) . . . . ? Eu1 N26 C30 C31 10.9(6) . . . . ? N28 C29 C30 N26 0.5(6) . . . . ? N28 C29 C30 C31 -176.1(6) . . . . ? N26 C30 C31 N32 -7.5(7) . . . . ? C29 C30 C31 N32 168.7(6) . . . . ? N26 C30 C31 C39 174.1(6) . . . . ? C29 C30 C31 C39 -9.7(10) . . . . ? C39 C31 N32 C33 0.5(8) . . . . ? C30 C31 N32 C33 -177.9(5) . . . . ? C39 C31 N32 Eu1 178.9(5) . . . . ? C30 C31 N32 Eu1 0.6(6) . . . . ? N50 Eu1 N32 C33 -82.6(4) . . . . ? N14 Eu1 N32 C33 -28.3(4) . . . . ? N26 Eu1 N32 C33 -178.2(4) . . . . ? N38 Eu1 N32 C33 1.6(3) . . . . ? N62 Eu1 N32 C33 149.9(3) . . . . ? N2 Eu1 N32 C33 100.0(4) . . . . ? N8 Eu1 N32 C33 53.5(4) . . . . ? N56 Eu1 N32 C33 -125.5(3) . . . . ? N50 Eu1 N32 C31 98.9(4) . . . . ? N14 Eu1 N32 C31 153.2(3) . . . . ? N26 Eu1 N32 C31 3.3(3) . . . . ? N38 Eu1 N32 C31 -176.9(4) . . . . ? N62 Eu1 N32 C31 -28.6(4) . . . . ? N2 Eu1 N32 C31 -78.5(4) . . . . ? N8 Eu1 N32 C31 -125.0(3) . . . . ? N56 Eu1 N32 C31 56.0(4) . . . . ? C31 N32 C33 C41 -0.5(8) . . . . ? Eu1 N32 C33 C41 -179.0(5) . . . . ? C31 N32 C33 C34 179.1(5) . . . . ? Eu1 N32 C33 C34 0.6(6) . . . . ? N32 C33 C34 C35 173.2(6) . . . . ? C41 C33 C34 C35 -7.1(10) . . . . ? N32 C33 C34 N38 -4.3(7) . . . . ? C41 C33 C34 N38 175.3(6) . . . . ? N38 C34 C35 N36 -0.4(6) . . . . ? C33 C34 C35 N36 -178.1(6) . . . . ? C34 C35 N36 N37 0.2(6) . . . . ? C34 C35 N36 C46 178.7(5) . . . . ? C35 N36 N37 N38 0.2(6) . . . . ? C46 N36 N37 N38 -178.5(4) . . . . ? N36 N37 N38 C34 -0.4(5) . . . . ? N36 N37 N38 Eu1 171.2(3) . . . . ? C35 C34 N38 N37 0.5(6) . . . . ? C33 C34 N38 N37 178.7(4) . . . . ? C35 C34 N38 Eu1 -172.2(3) . . . . ? C33 C34 N38 Eu1 6.0(6) . . . . ? N50 Eu1 N38 N37 -97.4(4) . . . . ? N14 Eu1 N38 N37 -16.4(4) . . . . ? N26 Eu1 N38 N37 -174.6(4) . . . . ? N62 Eu1 N38 N37 48.1(5) . . . . ? N2 Eu1 N38 N37 112.8(4) . . . . ? N32 Eu1 N38 N37 -174.8(4) . . . . ? N8 Eu1 N38 N37 50.4(4) . . . . ? N56 Eu1 N38 N37 -62.3(4) . . . . ? N50 Eu1 N38 C34 73.4(3) . . . . ? N14 Eu1 N38 C34 154.4(4) . . . . ? N26 Eu1 N38 C34 -3.7(4) . . . . ? N62 Eu1 N38 C34 -141.1(3) . . . . ? N2 Eu1 N38 C34 -76.4(3) . . . . ? N32 Eu1 N38 C34 -3.9(3) . . . . ? N8 Eu1 N38 C34 -138.8(4) . . . . ? N56 Eu1 N38 C34 108.5(4) . . . . ? N32 C31 C39 C40 -0.4(10) . . . . ? C30 C31 C39 C40 177.9(7) . . . . ? C31 C39 C40 C41 0.5(13) . . . . ? N32 C33 C41 C40 0.6(11) . . . . ? C34 C33 C41 C40 -179.0(7) . . . . ? C39 C40 C41 C33 -0.6(13) . . . . ? C29 N28 C42 C43 97.9(8) . . . . ? N27 N28 C42 C43 -80.7(8) . . . . ? N28 C42 C43 C44 -171.0(8) . . . . ? C42 C43 C44 C45 179.6(8) . . . . ? C35 N36 C46 C47 -169.0(6) . . . . ? N37 N36 C46 C47 9.5(8) . . . . ? N36 C46 C47 C48 -178.8(6) . . . . ? C46 C47 C48 C49 -171.7(14) . . . . ? C46 C47 C48 C49A -100.6(11) . . . . ? N14 Eu1 N50 N51 -102.5(4) . . . . ? N26 Eu1 N50 N51 104.9(4) . . . . ? N38 Eu1 N50 N51 -25.5(4) . . . . ? N62 Eu1 N50 N51 177.1(4) . . . . ? N2 Eu1 N50 N51 46.0(5) . . . . ? N32 Eu1 N50 N51 41.2(4) . . . . ? N8 Eu1 N50 N51 -75.2(4) . . . . ? N56 Eu1 N50 N51 -178.1(4) . . . . ? N14 Eu1 N50 C54 70.6(3) . . . . ? N26 Eu1 N50 C54 -81.9(4) . . . . ? N38 Eu1 N50 C54 147.7(4) . . . . ? N62 Eu1 N50 C54 -9.7(4) . . . . ? N2 Eu1 N50 C54 -140.8(3) . . . . ? N32 Eu1 N50 C54 -145.6(4) . . . . ? N8 Eu1 N50 C54 98.0(4) . . . . ? N56 Eu1 N50 C54 -4.9(3) . . . . ? C54 N50 N51 N52 0.9(5) . . . . ? Eu1 N50 N51 N52 174.6(3) . . . . ? N50 N51 N52 C53 -0.8(6) . . . . ? N50 N51 N52 C66 178.2(5) . . . . ? N51 N52 C53 C54 0.4(6) . . . . ? C66 N52 C53 C54 -178.4(5) . . . . ? N52 C53 C54 N50 0.2(6) . . . . ? N52 C53 C54 C55 -178.7(5) . . . . ? N51 N50 C54 C53 -0.6(6) . . . . ? Eu1 N50 C54 C53 -175.0(3) . . . . ? N51 N50 C54 C55 178.4(4) . . . . ? Eu1 N50 C54 C55 4.0(6) . . . . ? C53 C54 C55 N56 -179.7(6) . . . . ? N50 C54 C55 N56 1.5(7) . . . . ? C53 C54 C55 C63 4.0(10) . . . . ? N50 C54 C55 C63 -174.7(5) . . . . ? C63 C55 N56 C57 -2.4(7) . . . . ? C54 C55 N56 C57 -178.7(4) . . . . ? C63 C55 N56 Eu1 170.1(4) . . . . ? C54 C55 N56 Eu1 -6.2(6) . . . . ? N50 Eu1 N56 C55 5.9(4) . . . . ? N14 Eu1 N56 C55 -79.5(4) . . . . ? N26 Eu1 N56 C55 99.5(4) . . . . ? N38 Eu1 N56 C55 -32.7(4) . . . . ? N62 Eu1 N56 C55 -178.4(4) . . . . ? N2 Eu1 N56 C55 154.3(3) . . . . ? N32 Eu1 N56 C55 52.3(4) . . . . ? N8 Eu1 N56 C55 -126.7(4) . . . . ? N50 Eu1 N56 C57 178.3(4) . . . . ? N14 Eu1 N56 C57 92.8(4) . . . . ? N26 Eu1 N56 C57 -88.1(4) . . . . ? N38 Eu1 N56 C57 139.6(3) . . . . ? N62 Eu1 N56 C57 -6.0(3) . . . . ? N2 Eu1 N56 C57 -33.3(4) . . . . ? N32 Eu1 N56 C57 -135.3(4) . . . . ? N8 Eu1 N56 C57 45.7(4) . . . . ? C55 N56 C57 C65 3.5(8) . . . . ? Eu1 N56 C57 C65 -169.0(4) . . . . ? C55 N56 C57 C58 -178.2(5) . . . . ? Eu1 N56 C57 C58 9.2(6) . . . . ? N56 C57 C58 C59 172.2(6) . . . . ? C65 C57 C58 C59 -9.6(10) . . . . ? N56 C57 C58 N62 -7.5(7) . . . . ? C65 C57 C58 N62 170.7(5) . . . . ? N62 C58 C59 N60 0.8(7) . . . . ? C57 C58 C59 N60 -178.9(6) . . . . ? C58 C59 N60 N61 -0.5(7) . . . . ? C58 C59 N60 C70A -178.2(7) . . . . ? C58 C59 N60 C70 179.6(7) . . . . ? C59 N60 N61 N62 0.0(6) . . . . ? C70A N60 N61 N62 178.0(6) . . . . ? C70 N60 N61 N62 179.9(6) . . . . ? N60 N61 N62 C58 0.5(6) . . . . ? N60 N61 N62 Eu1 176.8(3) . . . . ? C59 C58 N62 N61 -0.8(6) . . . . ? C57 C58 N62 N61 178.9(5) . . . . ? C59 C58 N62 Eu1 -177.5(4) . . . . ? C57 C58 N62 Eu1 2.2(7) . . . . ? N50 Eu1 N62 N61 -169.4(4) . . . . ? N14 Eu1 N62 N61 115.7(4) . . . . ? N26 Eu1 N62 N61 -92.2(4) . . . . ? N38 Eu1 N62 N61 55.0(6) . . . . ? N2 Eu1 N62 N61 -13.7(4) . . . . ? N32 Eu1 N62 N61 -63.0(5) . . . . ? N8 Eu1 N62 N61 52.6(4) . . . . ? N56 Eu1 N62 N61 -174.2(5) . . . . ? N50 Eu1 N62 C58 6.5(5) . . . . ? N14 Eu1 N62 C58 -68.4(4) . . . . ? N26 Eu1 N62 C58 83.7(4) . . . . ? N38 Eu1 N62 C58 -129.1(4) . . . . ? N2 Eu1 N62 C58 162.2(4) . . . . ? N32 Eu1 N62 C58 112.9(4) . . . . ? N8 Eu1 N62 C58 -131.5(4) . . . . ? N56 Eu1 N62 C58 1.7(4) . . . . ? N56 C55 C63 C64 1.6(9) . . . . ? C54 C55 C63 C64 177.6(6) . . . . ? C55 C63 C64 C65 -1.7(10) . . . . ? C63 C64 C65 C57 2.8(10) . . . . ? N56 C57 C65 C64 -3.7(9) . . . . ? C58 C57 C65 C64 178.2(6) . . . . ? N51 N52 C66 C67 -87.8(7) . . . . ? C53 N52 C66 C67 90.9(8) . . . . ? N52 C66 C67 C68 67.9(10) . . . . ? C66 C67 C68 C69 -179.7(9) . . . . ? N61 N60 C70 C71 -39.9(15) . . . . ? C59 N60 C70 C71 140.0(11) . . . . ? C70A N60 C70 C71 53(27) . . . . ? N61 N60 C70A C71A -98.3(10) . . . . ? C59 N60 C70A C71A 79.2(11) . . . . ? C70 N60 C70A C71A 174(100) . . . . ? N60 C70 C71 C72 -175.7(11) . . . . ? N60 C70A C71A C72A 63.3(15) . . . . ? C70 C71 C72 C73 -70.6(15) . . . . ? C70A C71A C72A C73A 167.6(16) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.983 _refine_diff_density_min -1.446 _refine_diff_density_rms 0.101 # Attachment 'Fe.cif' data_06168 _database_code_depnum_ccdc_archive 'CCDC 639382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H38 Fe N14 O4, 2(F6 P), H2 O' _chemical_formula_sum 'C30 H40 F12 Fe N14 O5 P2' _chemical_formula_weight 1022.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.156(3) _cell_length_b 26.836(6) _cell_length_c 14.153(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.726(5) _cell_angle_gamma 90.00 _cell_volume 4097.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 872 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.46 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.65 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _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_details ' 0.30 degree frames measured for 15.16 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 16775 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.0900 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4723 _reflns_number_gt 2881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Reciprocal Net (http://recipnet.org)' _computing_publication_material ? _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. Disorder is present in one PF6 anion. Hydrogen atoms on disordered water solvent not located, and hydroxy hydrogens are most likely disordered. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^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 4723 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.68705(2) 0.7500 0.01822(14) Uani 1 2 d S . . O1S O 0.4724(5) 1.0070(2) 0.9553(4) 0.0681(17) Uani 0.50 1 d P . . N2 N 0.61640(19) 0.63585(8) 0.73509(14) 0.0191(5) Uani 1 1 d . . . N3 N 0.62877(19) 0.60704(8) 0.66334(15) 0.0218(5) Uani 1 1 d . . . N4 N 0.7247(2) 0.57642(8) 0.70215(15) 0.0224(5) Uani 1 1 d . . . C5 C 0.7738(3) 0.58598(10) 0.79796(18) 0.0224(6) Uani 1 1 d . . . C6 C 0.7047(2) 0.62400(10) 0.81968(17) 0.0198(6) Uani 1 1 d . . . C7 C 0.6991(2) 0.65380(9) 0.90385(18) 0.0200(5) Uani 1 1 d . . . N8 N 0.60260(18) 0.68612(8) 0.88146(14) 0.0181(4) Uani 1 1 d . . . C9 C 0.5770(2) 0.71599(9) 0.95020(17) 0.0203(6) Uani 1 1 d . . . C10 C 0.4677(2) 0.74635(9) 0.90762(17) 0.0201(6) Uani 1 1 d . . . C11 C 0.3979(3) 0.78211(10) 0.93631(19) 0.0246(6) Uani 1 1 d . . . N12 N 0.3076(2) 0.79296(8) 0.85499(15) 0.0220(5) Uani 1 1 d . . . N13 N 0.31884(19) 0.76591(8) 0.77833(15) 0.0212(5) Uani 1 1 d . . . N14 N 0.41691(19) 0.73724(8) 0.80966(14) 0.0187(5) Uani 1 1 d . . . C15 C 0.7760(2) 0.65224(10) 0.99803(18) 0.0220(6) Uani 1 1 d . . . C16 C 0.7503(2) 0.68315(10) 1.06868(18) 0.0230(6) Uani 1 1 d . . . C17 C 0.6495(3) 0.71529(10) 1.04640(18) 0.0230(6) Uani 1 1 d . . . C18 C 0.7680(3) 0.54147(11) 0.6393(2) 0.0271(6) Uani 1 1 d . . . C19 C 0.6644(3) 0.50890(13) 0.5804(2) 0.0363(8) Uani 1 1 d . . . C20 C 0.7080(3) 0.47838(13) 0.5052(2) 0.0383(8) Uani 1 1 d . . . O21 O 0.7528(3) 0.50892(10) 0.43893(17) 0.0644(8) Uani 1 1 d . . . H21 H 0.6981 0.5297 0.4129 0.15(3) Uiso 1 1 calc R . . C22 C 0.2076(3) 0.83040(12) 0.8368(2) 0.0292(7) Uani 1 1 d . . . C23 C 0.1757(3) 0.84866(13) 0.9274(2) 0.0323(7) Uani 1 1 d . . . C24 C 0.0599(3) 0.88169(12) 0.9006(2) 0.0328(7) Uani 1 1 d . . . O25 O 0.0763(2) 0.92318(8) 0.84361(17) 0.0394(6) Uani 1 1 d . . . H25 H 0.0067 0.9341 0.8130 0.23(8) Uiso 1 1 calc R . . P26 P 0.0000 0.68390(4) 0.7500 0.0277(2) Uani 1 2 d S . . F27 F 0.0000 0.62448(9) 0.7500 0.0370(6) Uani 1 2 d S . . F28 F 0.0000 0.74344(10) 0.7500 0.0609(9) Uani 1 2 d S . . F29 F 0.13727(15) 0.68356(7) 0.81989(13) 0.0449(5) Uani 1 1 d . . . F30 F -0.05594(16) 0.68432(7) 0.84364(12) 0.0429(5) Uani 1 1 d . . . P31 P 0.5000 0.91143(4) 0.7500 0.0338(3) Uani 1 2 d S . . F32 F 0.5000 0.85155(13) 0.7500 0.060(2) Uani 0.848(14) 2 d SP . . F33 F 0.5000 0.97016(11) 0.7500 0.085(3) Uani 1 2 d SP . . F34 F 0.64763(15) 0.91187(7) 0.79142(13) 0.0418(5) Uani 1 1 d . . . F35 F 0.4839(2) 0.90939(15) 0.85884(16) 0.0671(15) Uani 0.847(9) 1 d P . . F36 F 0.4909(18) 0.8698(10) 0.8137(18) 0.035(9) Uiso 0.088(9) 1 d P . . F37 F 0.492(2) 0.9519(12) 0.836(2) 0.097(11) Uiso 0.150(11) 1 d P . . H36 H 0.841(2) 0.5656(10) 0.8361(19) 0.021(7) Uiso 1 1 d . . . H37 H 0.401(2) 0.7987(10) 0.992(2) 0.020(7) Uiso 1 1 d . . . H38 H 0.842(2) 0.6315(9) 1.0093(18) 0.013(7) Uiso 1 1 d . . . H39 H 0.798(3) 0.6818(10) 1.135(2) 0.031(8) Uiso 1 1 d . . . H40 H 0.633(2) 0.7360(9) 1.0918(18) 0.008(6) Uiso 1 1 d . . . H41 H 0.839(3) 0.5188(11) 0.682(2) 0.040(9) Uiso 1 1 d . . . H42 H 0.803(3) 0.5605(11) 0.599(2) 0.029(8) Uiso 1 1 d . . . H43 H 0.595(3) 0.5295(12) 0.547(2) 0.035(9) Uiso 1 1 d . . . H44 H 0.635(3) 0.4873(12) 0.618(2) 0.041(10) Uiso 1 1 d . . . H45 H 0.644(3) 0.4562(13) 0.475(3) 0.055(11) Uiso 1 1 d . . . H46 H 0.783(3) 0.4585(11) 0.536(2) 0.038(9) Uiso 1 1 d . . . H48 H 0.236(3) 0.8573(13) 0.807(3) 0.047(10) Uiso 1 1 d . . . H49 H 0.137(3) 0.8108(11) 0.792(2) 0.040(9) Uiso 1 1 d . . . H50 H 0.246(3) 0.8676(14) 0.970(3) 0.061(11) Uiso 1 1 d . . . H51 H 0.153(3) 0.8187(13) 0.965(3) 0.057(11) Uiso 1 1 d . . . H52 H -0.009(3) 0.8618(12) 0.863(3) 0.053(10) Uiso 1 1 d . . . H53 H 0.039(3) 0.8922(12) 0.963(3) 0.047(10) Uiso 1 1 d . . . 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 0.0246(3) 0.0178(3) 0.0073(2) 0.000 -0.00493(19) 0.000 O1S 0.044(3) 0.090(4) 0.065(4) -0.014(3) 0.005(3) 0.015(3) N2 0.0254(11) 0.0174(11) 0.0098(10) 0.0015(8) -0.0041(8) -0.0023(9) N3 0.0275(12) 0.0199(12) 0.0143(11) -0.0009(9) -0.0017(9) 0.0014(9) N4 0.0271(12) 0.0228(13) 0.0128(11) -0.0005(9) -0.0032(9) 0.0036(9) C5 0.0279(14) 0.0229(14) 0.0118(12) 0.0011(11) -0.0039(10) 0.0012(12) C6 0.0245(13) 0.0198(14) 0.0096(12) 0.0039(10) -0.0061(10) -0.0016(10) C7 0.0260(13) 0.0193(13) 0.0113(12) 0.0009(10) -0.0015(10) -0.0018(11) N8 0.0249(11) 0.0169(10) 0.0087(9) 0.0008(8) -0.0024(8) -0.0036(9) C9 0.0262(14) 0.0179(13) 0.0128(12) 0.0009(10) -0.0022(10) -0.0032(10) C10 0.0285(14) 0.0187(14) 0.0087(12) 0.0002(10) -0.0032(10) -0.0033(11) C11 0.0343(16) 0.0225(15) 0.0117(13) -0.0003(11) -0.0042(11) -0.0015(12) N12 0.0287(12) 0.0198(12) 0.0123(10) -0.0004(9) -0.0043(9) 0.0015(9) N13 0.0271(12) 0.0200(12) 0.0122(10) 0.0005(9) -0.0028(9) 0.0008(9) N14 0.0259(11) 0.0166(11) 0.0093(10) 0.0014(8) -0.0034(8) -0.0015(9) C15 0.0260(14) 0.0210(14) 0.0131(13) 0.0034(10) -0.0055(10) 0.0015(11) C16 0.0313(14) 0.0222(14) 0.0097(12) 0.0007(10) -0.0057(10) -0.0029(11) C17 0.0331(15) 0.0212(15) 0.0107(12) -0.0017(10) -0.0019(11) -0.0036(11) C18 0.0323(16) 0.0261(16) 0.0190(14) -0.0024(12) -0.0005(12) 0.0045(13) C19 0.0376(18) 0.0312(19) 0.0334(18) -0.0115(14) -0.0032(15) 0.0046(15) C20 0.047(2) 0.0302(18) 0.0295(17) -0.0105(14) -0.0063(14) 0.0069(15) O21 0.135(3) 0.0352(15) 0.0211(12) -0.0006(10) 0.0165(15) 0.0184(16) C22 0.0364(17) 0.0264(16) 0.0194(14) -0.0001(12) -0.0029(12) 0.0078(13) C23 0.0407(18) 0.0351(18) 0.0178(14) 0.0017(13) 0.0012(13) 0.0104(14) C24 0.0380(17) 0.0349(18) 0.0220(15) -0.0009(13) 0.0012(13) 0.0078(14) O25 0.0455(13) 0.0274(12) 0.0434(13) 0.0068(10) 0.0078(11) 0.0096(9) P26 0.0290(5) 0.0286(6) 0.0231(5) 0.000 0.0021(4) 0.000 F27 0.0407(14) 0.0282(14) 0.0438(15) 0.000 0.0135(11) 0.000 F28 0.0578(18) 0.0288(16) 0.103(3) 0.000 0.0338(17) 0.000 F29 0.0303(9) 0.0618(13) 0.0359(10) -0.0021(9) -0.0041(8) -0.0080(9) F30 0.0443(10) 0.0555(12) 0.0298(10) -0.0155(9) 0.0112(8) -0.0108(9) P31 0.0359(6) 0.0301(6) 0.0245(6) 0.000 -0.0121(5) 0.000 F32 0.050(2) 0.031(2) 0.084(4) 0.000 -0.0103(19) 0.000 F33 0.058(2) 0.033(2) 0.130(5) 0.000 -0.038(2) 0.000 F34 0.0355(10) 0.0411(11) 0.0357(10) -0.0026(8) -0.0153(8) 0.0005(8) F35 0.0529(16) 0.114(4) 0.0243(13) 0.0044(14) -0.0084(10) 0.0174(15) _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 N8 1.9208(19) . ? Fe1 N8 1.9209(19) 2_656 ? Fe1 N2 1.938(2) 2_656 ? Fe1 N2 1.938(2) . ? Fe1 N14 1.945(2) . ? Fe1 N14 1.945(2) 2_656 ? O1S O1S 1.313(10) 5_677 ? N2 N3 1.311(3) . ? N2 C6 1.380(3) . ? N3 N4 1.350(3) . ? N4 C5 1.352(3) . ? N4 C18 1.457(4) . ? C5 C6 1.360(4) . ? C5 H36 0.98(3) . ? C6 C7 1.450(4) . ? C7 N8 1.356(3) . ? C7 C15 1.390(3) . ? N8 C9 1.346(3) . ? C9 C17 1.396(3) . ? C9 C10 1.463(4) . ? C10 C11 1.361(4) . ? C10 N14 1.380(3) . ? C11 N12 1.354(3) . ? C11 H37 0.90(3) . ? N12 N13 1.337(3) . ? N12 C22 1.475(4) . ? N13 N14 1.319(3) . ? C15 C16 1.384(4) . ? C15 H38 0.91(2) . ? C16 C17 1.388(4) . ? C16 H39 0.95(3) . ? C17 H40 0.90(3) . ? C18 C19 1.518(4) . ? C18 H41 1.06(3) . ? C18 H42 0.92(3) . ? C19 C20 1.517(5) . ? C19 H43 0.97(3) . ? C19 H44 0.90(3) . ? C20 O21 1.428(4) . ? C20 H45 0.94(4) . ? C20 H46 1.00(3) . ? O21 H21 0.8400 . ? C22 C23 1.497(4) . ? C22 H48 0.94(3) . ? C22 H49 1.02(3) . ? C23 C24 1.533(4) . ? C23 H50 1.00(4) . ? C23 H51 1.03(4) . ? C24 O25 1.413(4) . ? C24 H52 0.97(3) . ? C24 H53 1.02(4) . ? O25 H25 0.8400 . ? P26 F27 1.595(3) . ? P26 F29 1.5980(16) . ? P26 F29 1.5980(16) 2_556 ? P26 F28 1.598(3) . ? P26 F30 1.6021(18) 2_556 ? P26 F30 1.6021(18) . ? P31 F36 1.46(2) 2_656 ? P31 F36 1.46(2) . ? P31 F33 1.576(3) . ? P31 F35 1.596(2) 2_656 ? P31 F35 1.596(2) . ? P31 F34 1.6016(17) 2_656 ? P31 F34 1.6016(17) . ? P31 F32 1.607(4) . ? P31 F37 1.65(2) 2_656 ? P31 F37 1.65(2) . ? F32 F36 1.05(3) . ? F32 F36 1.05(3) 2_656 ? F33 F37 1.34(3) . ? F33 F37 1.34(3) 2_656 ? F35 F37 1.20(3) . ? F35 F36 1.25(3) . ? 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 N8 Fe1 N8 178.51(13) . 2_656 ? N8 Fe1 N2 97.82(9) . 2_656 ? N8 Fe1 N2 81.12(9) 2_656 2_656 ? N8 Fe1 N2 81.11(9) . . ? N8 Fe1 N2 97.82(9) 2_656 . ? N2 Fe1 N2 89.73(13) 2_656 . ? N8 Fe1 N14 79.68(9) . . ? N8 Fe1 N14 101.37(8) 2_656 . ? N2 Fe1 N14 92.14(9) 2_656 . ? N2 Fe1 N14 160.78(8) . . ? N8 Fe1 N14 101.37(8) . 2_656 ? N8 Fe1 N14 79.68(9) 2_656 2_656 ? N2 Fe1 N14 160.78(8) 2_656 2_656 ? N2 Fe1 N14 92.14(9) . 2_656 ? N14 Fe1 N14 92.35(13) . 2_656 ? N3 N2 C6 110.1(2) . . ? N3 N2 Fe1 135.03(16) . . ? C6 N2 Fe1 114.78(17) . . ? N2 N3 N4 105.81(19) . . ? N3 N4 C5 111.7(2) . . ? N3 N4 C18 119.7(2) . . ? C5 N4 C18 128.5(2) . . ? N4 C5 C6 105.1(2) . . ? N4 C5 H36 120.5(16) . . ? C6 C5 H36 134.3(16) . . ? C5 C6 N2 107.3(2) . . ? C5 C6 C7 138.2(2) . . ? N2 C6 C7 114.5(2) . . ? N8 C7 C15 120.2(2) . . ? N8 C7 C6 111.0(2) . . ? C15 C7 C6 128.8(2) . . ? C9 N8 C7 120.9(2) . . ? C9 N8 Fe1 120.57(17) . . ? C7 N8 Fe1 118.49(17) . . ? N8 C9 C17 121.3(2) . . ? N8 C9 C10 110.0(2) . . ? C17 C9 C10 128.7(3) . . ? C11 C10 N14 107.7(2) . . ? C11 C10 C9 138.6(2) . . ? N14 C10 C9 113.7(2) . . ? N12 C11 C10 104.8(2) . . ? N12 C11 H37 119.5(17) . . ? C10 C11 H37 135.7(17) . . ? N13 N12 C11 111.7(2) . . ? N13 N12 C22 116.80(19) . . ? C11 N12 C22 131.4(2) . . ? N14 N13 N12 106.53(18) . . ? N13 N14 C10 109.2(2) . . ? N13 N14 Fe1 134.76(16) . . ? C10 N14 Fe1 116.08(16) . . ? C16 C15 C7 118.9(2) . . ? C16 C15 H38 123.4(16) . . ? C7 C15 H38 117.6(16) . . ? C15 C16 C17 120.8(2) . . ? C15 C16 H39 121.1(18) . . ? C17 C16 H39 118.0(18) . . ? C16 C17 C9 117.7(3) . . ? C16 C17 H40 121.2(15) . . ? C9 C17 H40 121.0(15) . . ? N4 C18 C19 112.4(3) . . ? N4 C18 H41 109.5(17) . . ? C19 C18 H41 110.0(16) . . ? N4 C18 H42 106.2(19) . . ? C19 C18 H42 111.1(18) . . ? H41 C18 H42 107(2) . . ? C18 C19 C20 111.2(3) . . ? C18 C19 H43 109.9(18) . . ? C20 C19 H43 109.3(18) . . ? C18 C19 H44 113(2) . . ? C20 C19 H44 107(2) . . ? H43 C19 H44 107(3) . . ? O21 C20 C19 112.3(3) . . ? O21 C20 H45 115(2) . . ? C19 C20 H45 109(2) . . ? O21 C20 H46 101.3(18) . . ? C19 C20 H46 111.5(18) . . ? H45 C20 H46 108(3) . . ? C20 O21 H21 109.5 . . ? N12 C22 C23 114.0(2) . . ? N12 C22 H48 106(2) . . ? C23 C22 H48 109(2) . . ? N12 C22 H49 100.9(17) . . ? C23 C22 H49 112.6(19) . . ? H48 C22 H49 114(3) . . ? C22 C23 C24 110.2(2) . . ? C22 C23 H50 111(2) . . ? C24 C23 H50 110(2) . . ? C22 C23 H51 109(2) . . ? C24 C23 H51 106(2) . . ? H50 C23 H51 110(3) . . ? O25 C24 C23 112.0(3) . . ? O25 C24 H52 109(2) . . ? C23 C24 H52 108(2) . . ? O25 C24 H53 111.8(19) . . ? C23 C24 H53 108.3(18) . . ? H52 C24 H53 107(3) . . ? C24 O25 H25 109.5 . . ? F27 P26 F29 89.67(8) . . ? F27 P26 F29 89.67(8) . 2_556 ? F29 P26 F29 179.33(16) . 2_556 ? F27 P26 F28 180.000(1) . . ? F29 P26 F28 90.33(8) . . ? F29 P26 F28 90.33(8) 2_556 . ? F27 P26 F30 90.40(8) . 2_556 ? F29 P26 F30 89.92(9) . 2_556 ? F29 P26 F30 90.08(9) 2_556 2_556 ? F28 P26 F30 89.60(8) . 2_556 ? F27 P26 F30 90.40(8) . . ? F29 P26 F30 90.08(9) . . ? F29 P26 F30 89.92(9) 2_556 . ? F28 P26 F30 89.60(8) . . ? F30 P26 F30 179.20(16) 2_556 . ? F36 P31 F36 80(2) 2_656 . ? F36 P31 F33 140.2(12) 2_656 . ? F36 P31 F33 140.2(12) . . ? F36 P31 F35 48.2(12) 2_656 2_656 ? F36 P31 F35 127.9(12) . 2_656 ? F33 P31 F35 91.96(15) . 2_656 ? F36 P31 F35 127.9(12) 2_656 . ? F36 P31 F35 48.2(12) . . ? F33 P31 F35 91.96(15) . . ? F35 P31 F35 176.1(3) 2_656 . ? F36 P31 F34 90.4(8) 2_656 2_656 ? F36 P31 F34 90.3(8) . 2_656 ? F33 P31 F34 89.58(7) . 2_656 ? F35 P31 F34 90.24(11) 2_656 2_656 ? F35 P31 F34 89.79(11) . 2_656 ? F36 P31 F34 90.3(8) 2_656 . ? F36 P31 F34 90.4(8) . . ? F33 P31 F34 89.57(7) . . ? F35 P31 F34 89.79(11) 2_656 . ? F35 P31 F34 90.24(11) . . ? F34 P31 F34 179.15(15) 2_656 . ? F36 P31 F32 39.8(12) 2_656 . ? F36 P31 F32 39.8(12) . . ? F33 P31 F32 180.000(1) . . ? F35 P31 F32 88.04(15) 2_656 . ? F35 P31 F32 88.04(15) . . ? F34 P31 F32 90.42(7) 2_656 . ? F34 P31 F32 90.43(7) . . ? F36 P31 F37 91.3(18) 2_656 2_656 ? F36 P31 F37 170.9(17) . 2_656 ? F33 P31 F37 48.8(13) . 2_656 ? F35 P31 F37 43.2(12) 2_656 2_656 ? F35 P31 F37 140.7(14) . 2_656 ? F34 P31 F37 88.1(8) 2_656 2_656 ? F34 P31 F37 91.3(8) . 2_656 ? F32 P31 F37 131.2(13) . 2_656 ? F36 P31 F37 170.9(17) 2_656 . ? F36 P31 F37 91.4(18) . . ? F33 P31 F37 48.8(13) . . ? F35 P31 F37 140.7(14) 2_656 . ? F35 P31 F37 43.2(12) . . ? F34 P31 F37 91.3(8) 2_656 . ? F34 P31 F37 88.1(8) . . ? F32 P31 F37 131.2(13) . . ? F37 P31 F37 98(3) 2_656 . ? F36 F32 F36 125(2) . 2_656 ? F36 F32 P31 62.3(12) . . ? F36 F32 P31 62.3(12) 2_656 . ? F37 F33 F37 137(2) . 2_656 ? F37 F33 P31 68.5(12) . . ? F37 F33 P31 68.5(12) 2_656 . ? F37 F35 F36 130.8(16) . . ? F37 F35 P31 70.9(12) . . ? F36 F35 P31 60.0(10) . . ? F32 F36 F35 150(2) . . ? F32 F36 P31 77.9(14) . . ? F35 F36 P31 71.8(12) . . ? F35 F37 F33 128.5(19) . . ? F35 F37 P31 66.0(12) . . ? F33 F37 P31 62.6(10) . . ? 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 N8 Fe1 N2 N3 177.8(3) . . . . ? N8 Fe1 N2 N3 -1.2(3) 2_656 . . . ? N2 Fe1 N2 N3 79.8(2) 2_656 . . . ? N14 Fe1 N2 N3 175.5(2) . . . . ? N14 Fe1 N2 N3 -81.1(2) 2_656 . . . ? N8 Fe1 N2 C6 1.98(18) . . . . ? N8 Fe1 N2 C6 -176.97(18) 2_656 . . . ? N2 Fe1 N2 C6 -95.98(19) 2_656 . . . ? N14 Fe1 N2 C6 -0.3(4) . . . . ? N14 Fe1 N2 C6 103.16(18) 2_656 . . . ? C6 N2 N3 N4 0.4(3) . . . . ? Fe1 N2 N3 N4 -175.52(19) . . . . ? N2 N3 N4 C5 -0.5(3) . . . . ? N2 N3 N4 C18 -176.1(2) . . . . ? N3 N4 C5 C6 0.4(3) . . . . ? C18 N4 C5 C6 175.5(3) . . . . ? N4 C5 C6 N2 -0.2(3) . . . . ? N4 C5 C6 C7 179.6(3) . . . . ? N3 N2 C6 C5 -0.2(3) . . . . ? Fe1 N2 C6 C5 176.67(18) . . . . ? N3 N2 C6 C7 -180.0(2) . . . . ? Fe1 N2 C6 C7 -3.1(3) . . . . ? C5 C6 C7 N8 -177.0(3) . . . . ? N2 C6 C7 N8 2.7(3) . . . . ? C5 C6 C7 C15 2.3(5) . . . . ? N2 C6 C7 C15 -178.0(3) . . . . ? C15 C7 N8 C9 -2.2(4) . . . . ? C6 C7 N8 C9 177.2(2) . . . . ? C15 C7 N8 Fe1 179.56(19) . . . . ? C6 C7 N8 Fe1 -1.1(3) . . . . ? N2 Fe1 N8 C9 -90.2(2) 2_656 . . . ? N2 Fe1 N8 C9 -178.7(2) . . . . ? N14 Fe1 N8 C9 0.55(19) . . . . ? N14 Fe1 N8 C9 90.9(2) 2_656 . . . ? N2 Fe1 N8 C7 88.0(2) 2_656 . . . ? N2 Fe1 N8 C7 -0.45(19) . . . . ? N14 Fe1 N8 C7 178.8(2) . . . . ? N14 Fe1 N8 C7 -90.9(2) 2_656 . . . ? C7 N8 C9 C17 0.9(4) . . . . ? Fe1 N8 C9 C17 179.1(2) . . . . ? C7 N8 C9 C10 -178.9(2) . . . . ? Fe1 N8 C9 C10 -0.7(3) . . . . ? N8 C9 C10 C11 -179.8(3) . . . . ? C17 C9 C10 C11 0.4(5) . . . . ? N8 C9 C10 N14 0.5(3) . . . . ? C17 C9 C10 N14 -179.3(3) . . . . ? N14 C10 C11 N12 0.3(3) . . . . ? C9 C10 C11 N12 -179.4(3) . . . . ? C10 C11 N12 N13 -0.2(3) . . . . ? C10 C11 N12 C22 -176.1(3) . . . . ? C11 N12 N13 N14 0.0(3) . . . . ? C22 N12 N13 N14 176.6(2) . . . . ? N12 N13 N14 C10 0.2(3) . . . . ? N12 N13 N14 Fe1 179.71(19) . . . . ? C11 C10 N14 N13 -0.3(3) . . . . ? C9 C10 N14 N13 179.5(2) . . . . ? C11 C10 N14 Fe1 -179.93(18) . . . . ? C9 C10 N14 Fe1 -0.1(3) . . . . ? N8 Fe1 N14 N13 -179.6(3) . . . . ? N8 Fe1 N14 N13 -0.7(3) 2_656 . . . ? N2 Fe1 N14 N13 -82.1(2) 2_656 . . . ? N2 Fe1 N14 N13 -177.4(2) . . . . ? N14 Fe1 N14 N13 79.2(2) 2_656 . . . ? N8 Fe1 N14 C10 -0.19(18) . . . . ? N8 Fe1 N14 C10 178.73(18) 2_656 . . . ? N2 Fe1 N14 C10 97.37(18) 2_656 . . . ? N2 Fe1 N14 C10 2.1(4) . . . . ? N14 Fe1 N14 C10 -101.32(19) 2_656 . . . ? N8 C7 C15 C16 1.7(4) . . . . ? C6 C7 C15 C16 -177.5(3) . . . . ? C7 C15 C16 C17 0.0(4) . . . . ? C15 C16 C17 C9 -1.3(4) . . . . ? N8 C9 C17 C16 0.9(4) . . . . ? C10 C9 C17 C16 -179.4(3) . . . . ? N3 N4 C18 C19 -53.7(4) . . . . ? C5 N4 C18 C19 131.6(3) . . . . ? N4 C18 C19 C20 171.7(3) . . . . ? C18 C19 C20 O21 -58.5(4) . . . . ? N13 N12 C22 C23 163.1(3) . . . . ? C11 N12 C22 C23 -21.1(5) . . . . ? N12 C22 C23 C24 -172.2(3) . . . . ? C22 C23 C24 O25 -58.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.704 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.076 # Attachment 'Ru.cif' data_06172 _database_code_depnum_ccdc_archive 'CCDC 639383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H38 N14 O4 Ru, 2(F6 P)' _chemical_formula_sum 'C30 H38 F12 N14 O4 P2 Ru' _chemical_formula_weight 1049.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2491(8) _cell_length_b 23.2119(15) _cell_length_c 14.9526(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.375(2) _cell_angle_gamma 90.00 _cell_volume 4034.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 1965 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 29.99 _exptl_crystal_description 'triangular plate' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 5.16 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 54482 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 30.03 _reflns_number_total 11770 _reflns_number_gt 8443 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Reciprocal Net (http://recipnet.org)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^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 11770 _refine_ls_number_parameters 720 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.734304(11) 0.557304(6) 0.247813(9) 0.01082(4) Uani 1 1 d . . . N2 N 0.84952(12) 0.61715(6) 0.23353(10) 0.0125(3) Uani 1 1 d . . . N3 N 0.86733(12) 0.64438(6) 0.16198(10) 0.0147(3) Uani 1 1 d . . . N4 N 0.96878(12) 0.67143(6) 0.19874(10) 0.0145(3) Uani 1 1 d . . . C5 C 1.01522(15) 0.66223(8) 0.29166(13) 0.0151(4) Uani 1 1 d . . . C6 C 0.93902(14) 0.62690(8) 0.31507(12) 0.0136(3) Uani 1 1 d . . . C7 C 0.93468(14) 0.59713(8) 0.39952(12) 0.0132(3) Uani 1 1 d . . . N8 N 0.84377(12) 0.56061(6) 0.38042(10) 0.0116(3) Uani 1 1 d . . . C9 C 0.82362(15) 0.52905(8) 0.44972(12) 0.0134(3) Uani 1 1 d . . . C10 C 0.72214(15) 0.49263(8) 0.41183(12) 0.0147(3) Uani 1 1 d . . . C11 C 0.66481(17) 0.45267(8) 0.44747(13) 0.0192(4) Uani 1 1 d . . . N12 N 0.57620(14) 0.43514(7) 0.37282(11) 0.0196(3) Uani 1 1 d . . . N13 N 0.57575(13) 0.46192(7) 0.29297(10) 0.0176(3) Uani 1 1 d . . . N14 N 0.66497(12) 0.49663(6) 0.31651(10) 0.0136(3) Uani 1 1 d . . . C15 C 1.01030(16) 0.60257(8) 0.49039(12) 0.0158(4) Uani 1 1 d . . . C16 C 0.98956(16) 0.57029(8) 0.56188(12) 0.0167(4) Uani 1 1 d . . . C17 C 0.89554(16) 0.53355(8) 0.54227(12) 0.0160(4) Uani 1 1 d . . . C18 C 1.01348(16) 0.70841(8) 0.13879(13) 0.0172(4) Uani 1 1 d . . . C19 C 0.94784(17) 0.76487(9) 0.11480(14) 0.0214(4) Uani 1 1 d . . . C20 C 0.94772(18) 0.80120(9) 0.19859(15) 0.0241(4) Uani 1 1 d . . . O21 O 0.86436(13) 0.78318(6) 0.24237(10) 0.0244(3) Uani 1 1 d . . . C22 C 0.48583(19) 0.39227(10) 0.36835(15) 0.0252(5) Uani 1 1 d . . . C23 C 0.42865(18) 0.40232(10) 0.44336(14) 0.0228(4) Uani 1 1 d . . . C24 C 0.32053(18) 0.36612(10) 0.42435(15) 0.0252(4) Uani 1 1 d . . . O25 O 0.33890(13) 0.30667(7) 0.40624(11) 0.0274(3) Uani 1 1 d . . . N26 N 0.80857(12) 0.49961(6) 0.17935(10) 0.0130(3) Uani 1 1 d . . . N27 N 0.89928(13) 0.46572(7) 0.20423(10) 0.0150(3) Uani 1 1 d . . . N28 N 0.90487(13) 0.44192(7) 0.12384(10) 0.0160(3) Uani 1 1 d . . . C29 C 0.81911(15) 0.46021(8) 0.04785(13) 0.0160(4) Uani 1 1 d . . . C30 C 0.75645(14) 0.49776(8) 0.08322(12) 0.0133(3) Uani 1 1 d . . . C31 C 0.65444(14) 0.53344(7) 0.04443(12) 0.0123(3) Uani 1 1 d . . . N32 N 0.62793(11) 0.56195(6) 0.11392(10) 0.0113(3) Uani 1 1 d . . . C33 C 0.53748(14) 0.59854(7) 0.09390(12) 0.0128(3) Uani 1 1 d . . . C34 C 0.52839(14) 0.62616(7) 0.17855(12) 0.0128(3) Uani 1 1 d . . . C35 C 0.45034(15) 0.66114(8) 0.20001(12) 0.0153(4) Uani 1 1 d . . . N36 N 0.49302(12) 0.66940(6) 0.29350(10) 0.0144(3) Uani 1 1 d . . . N37 N 0.59362(12) 0.64191(6) 0.33208(10) 0.0144(3) Uani 1 1 d . . . N38 N 0.61489(12) 0.61526(6) 0.26146(10) 0.0124(3) Uani 1 1 d . . . C39 C 0.58813(15) 0.54039(8) -0.04918(12) 0.0143(3) Uani 1 1 d . . . C40 C 0.49356(15) 0.57718(8) -0.06965(12) 0.0156(4) Uani 1 1 d . . . C41 C 0.46742(15) 0.60684(8) 0.00178(12) 0.0146(3) Uani 1 1 d . . . C42 C 0.99795(17) 0.40095(9) 0.12922(14) 0.0195(4) Uani 1 1 d . . . C43 C 1.06354(17) 0.41464(9) 0.06114(14) 0.0198(4) Uani 1 1 d . . . C44 C 1.17160(17) 0.37802(9) 0.08482(15) 0.0226(4) Uani 1 1 d . . . O45 O 1.14811(12) 0.31740(6) 0.07966(10) 0.0215(3) Uani 1 1 d . . . C46 C 0.44525(16) 0.70637(8) 0.35175(13) 0.0164(4) Uani 1 1 d . . . C47 C 0.46258(17) 0.76969(9) 0.33452(14) 0.0204(4) Uani 1 1 d . . . C48 C 0.58662(17) 0.78540(9) 0.35004(14) 0.0215(4) Uani 1 1 d . . . O49 O 0.65397(13) 0.77063(7) 0.44384(10) 0.0279(3) Uani 1 1 d . . . P50 P 0.23730(4) 0.55172(2) 0.25278(3) 0.01887(10) Uani 1 1 d . . . F51 F 0.18020(11) 0.56138(5) 0.33436(9) 0.0315(3) Uani 1 1 d . . . F52 F 0.29552(12) 0.54251(6) 0.17195(9) 0.0412(4) Uani 1 1 d . . . F53 F 0.36217(10) 0.55701(6) 0.32899(8) 0.0318(3) Uani 1 1 d . . . F54 F 0.11259(11) 0.54644(6) 0.17645(9) 0.0380(3) Uani 1 1 d . . . F55 F 0.23454(10) 0.61968(5) 0.23534(8) 0.0277(3) Uani 1 1 d . . . F56 F 0.23932(12) 0.48368(6) 0.27059(10) 0.0429(4) Uani 1 1 d . . . P57 P 0.23485(4) 0.75047(2) -0.00369(4) 0.01965(10) Uani 1 1 d . . . F58 F 0.24549(10) 0.81806(5) -0.02216(9) 0.0345(3) Uani 1 1 d . . . F59 F 0.22479(10) 0.68279(5) 0.01438(9) 0.0336(3) Uani 1 1 d . . . F60 F 0.37134(9) 0.74407(5) 0.02278(8) 0.0272(3) Uani 1 1 d . . . F61 F 0.09847(9) 0.75678(5) -0.03042(9) 0.0299(3) Uani 1 1 d . . . F62 F 0.24862(11) 0.76286(6) 0.10465(8) 0.0356(3) Uani 1 1 d . . . F63 F 0.22087(10) 0.73781(6) -0.11221(8) 0.0314(3) Uani 1 1 d . . . H64 H 1.0855(16) 0.6787(8) 0.3268(13) 0.013(5) Uiso 1 1 d . . . H65 H 0.6776(19) 0.4398(9) 0.5021(17) 0.031(6) Uiso 1 1 d . . . H66 H 1.0699(17) 0.6286(9) 0.5012(14) 0.020(5) Uiso 1 1 d . . . H67 H 1.0383(17) 0.5723(8) 0.6235(15) 0.019(5) Uiso 1 1 d . . . H68 H 0.8804(16) 0.5103(8) 0.5893(14) 0.013(5) Uiso 1 1 d . . . H69 H 1.0930(18) 0.7139(9) 0.1716(14) 0.020(5) Uiso 1 1 d . . . H70 H 1.0092(16) 0.6858(9) 0.0828(14) 0.017(5) Uiso 1 1 d . . . H71 H 0.8651(17) 0.7563(8) 0.0784(14) 0.016(5) Uiso 1 1 d . . . H72 H 0.989(2) 0.7887(10) 0.0788(16) 0.037(7) Uiso 1 1 d . . . H73 H 0.9346(16) 0.8430(9) 0.1815(14) 0.017(5) Uiso 1 1 d . . . H74 H 1.0300(19) 0.7997(9) 0.2469(16) 0.029(6) Uiso 1 1 d . . . H75 H 0.803(2) 0.7822(11) 0.2040(19) 0.049(9) Uiso 1 1 d . . . H76 H 0.4303(19) 0.3970(9) 0.3059(16) 0.029(6) Uiso 1 1 d . . . H77 H 0.5225(18) 0.3541(10) 0.3775(15) 0.025(6) Uiso 1 1 d . . . H78 H 0.4085(16) 0.4422(9) 0.4424(14) 0.013(5) Uiso 1 1 d . . . H79 H 0.4804(18) 0.3917(9) 0.5047(16) 0.027(6) Uiso 1 1 d . . . H80 H 0.2876(18) 0.3695(9) 0.4754(16) 0.026(6) Uiso 1 1 d . . . H81 H 0.2641(17) 0.3815(9) 0.3622(15) 0.023(6) Uiso 1 1 d . . . H82 H 0.351(3) 0.2866(14) 0.453(2) 0.077(11) Uiso 1 1 d . . . H83 H 0.8130(18) 0.4495(9) -0.0088(16) 0.024(6) Uiso 1 1 d . . . H84 H 0.3816(19) 0.6759(9) 0.1637(16) 0.032(6) Uiso 1 1 d . . . H85 H 0.6090(15) 0.5207(8) -0.0982(13) 0.013(5) Uiso 1 1 d . . . H86 H 0.4508(16) 0.5816(8) -0.1292(14) 0.014(5) Uiso 1 1 d . . . H87 H 0.4088(17) 0.6332(9) -0.0120(14) 0.018(5) Uiso 1 1 d . . . H88 H 1.0491(16) 0.4041(8) 0.1940(14) 0.016(5) Uiso 1 1 d . . . H89 H 0.9642(16) 0.3641(9) 0.1164(13) 0.012(5) Uiso 1 1 d . . . H90 H 1.0836(17) 0.4539(9) 0.0671(14) 0.017(5) Uiso 1 1 d . . . H91 H 1.0179(18) 0.4042(9) -0.0021(16) 0.025(6) Uiso 1 1 d . . . H92 H 1.2144(18) 0.3844(9) 0.0405(15) 0.024(6) Uiso 1 1 d . . . H93 H 1.2229(18) 0.3886(9) 0.1491(16) 0.025(6) Uiso 1 1 d . . . H94 H 1.140(2) 0.3070(11) 0.1263(18) 0.043(8) Uiso 1 1 d . . . H95 H 0.3665(16) 0.6958(8) 0.3371(13) 0.012(5) Uiso 1 1 d . . . H96 H 0.4825(16) 0.6928(8) 0.4152(14) 0.012(5) Uiso 1 1 d . . . H97 H 0.4174(17) 0.7817(9) 0.2698(15) 0.021(5) Uiso 1 1 d . . . H98 H 0.4304(19) 0.7917(10) 0.3765(16) 0.034(6) Uiso 1 1 d . . . H99 H 0.6169(18) 0.7666(9) 0.3038(15) 0.026(6) Uiso 1 1 d . . . H100 H 0.5910(17) 0.8265(9) 0.3389(14) 0.020(5) Uiso 1 1 d . . . H101 H 0.720(2) 0.7758(12) 0.449(2) 0.055(9) Uiso 1 1 d . . . 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 0.01233(6) 0.01286(7) 0.00699(6) 0.00001(5) 0.00263(4) 0.00011(5) N2 0.0147(7) 0.0144(7) 0.0086(7) 0.0000(5) 0.0041(5) 0.0002(6) N3 0.0161(7) 0.0159(8) 0.0127(7) 0.0005(6) 0.0053(6) -0.0020(6) N4 0.0159(7) 0.0150(8) 0.0129(7) 0.0005(6) 0.0052(6) -0.0018(6) C5 0.0150(8) 0.0163(9) 0.0135(9) -0.0013(7) 0.0038(6) -0.0002(7) C6 0.0150(8) 0.0135(9) 0.0113(8) -0.0010(6) 0.0025(6) -0.0001(6) C7 0.0145(8) 0.0132(9) 0.0116(8) -0.0004(6) 0.0036(6) 0.0016(6) N8 0.0144(7) 0.0117(7) 0.0085(7) -0.0003(5) 0.0035(5) 0.0007(6) C9 0.0172(8) 0.0139(9) 0.0092(8) 0.0000(6) 0.0046(6) 0.0007(7) C10 0.0193(9) 0.0163(9) 0.0093(8) -0.0009(7) 0.0056(6) -0.0002(7) C11 0.0259(10) 0.0207(11) 0.0105(9) 0.0001(7) 0.0047(7) -0.0061(7) N12 0.0256(8) 0.0211(9) 0.0134(8) -0.0021(6) 0.0082(6) -0.0083(7) N13 0.0218(8) 0.0194(8) 0.0126(8) -0.0005(6) 0.0070(6) -0.0043(6) N14 0.0157(7) 0.0156(8) 0.0093(7) -0.0013(6) 0.0037(5) -0.0007(6) C15 0.0174(9) 0.0162(9) 0.0115(8) -0.0020(7) 0.0013(6) -0.0007(7) C16 0.0197(9) 0.0182(10) 0.0093(8) -0.0009(7) 0.0005(6) 0.0006(7) C17 0.0217(9) 0.0162(9) 0.0100(8) 0.0014(7) 0.0049(7) 0.0017(7) C18 0.0196(9) 0.0186(10) 0.0157(9) 0.0009(7) 0.0088(7) -0.0031(7) C19 0.0251(10) 0.0225(11) 0.0178(10) 0.0019(8) 0.0085(8) -0.0010(8) C20 0.0282(11) 0.0207(11) 0.0258(11) -0.0019(8) 0.0120(8) -0.0015(8) O21 0.0267(8) 0.0286(8) 0.0198(7) 0.0012(6) 0.0097(6) 0.0019(6) C22 0.0312(11) 0.0272(12) 0.0190(10) -0.0041(8) 0.0106(8) -0.0154(9) C23 0.0260(10) 0.0265(11) 0.0154(10) -0.0010(8) 0.0059(8) -0.0064(8) C24 0.0240(10) 0.0292(12) 0.0234(11) -0.0003(9) 0.0088(8) -0.0065(9) O25 0.0279(8) 0.0259(8) 0.0271(9) 0.0050(7) 0.0070(6) -0.0054(6) N26 0.0137(7) 0.0151(8) 0.0099(7) 0.0013(6) 0.0034(5) 0.0004(6) N27 0.0175(7) 0.0164(8) 0.0123(7) 0.0003(6) 0.0065(6) 0.0018(6) N28 0.0195(7) 0.0186(8) 0.0108(7) 0.0011(6) 0.0059(5) 0.0056(6) C29 0.0186(9) 0.0188(9) 0.0099(8) 0.0008(7) 0.0036(6) 0.0027(7) C30 0.0153(8) 0.0152(9) 0.0093(8) 0.0010(6) 0.0037(6) -0.0004(7) C31 0.0154(8) 0.0119(8) 0.0106(8) -0.0003(6) 0.0056(6) -0.0012(6) N32 0.0126(6) 0.0117(7) 0.0099(7) 0.0000(5) 0.0040(5) -0.0009(6) C33 0.0141(8) 0.0135(9) 0.0109(8) 0.0004(6) 0.0039(6) -0.0011(6) C34 0.0141(8) 0.0129(9) 0.0110(8) 0.0003(6) 0.0034(6) -0.0012(6) C35 0.0167(9) 0.0159(9) 0.0127(9) 0.0012(7) 0.0038(7) 0.0010(7) N36 0.0147(7) 0.0158(8) 0.0134(7) -0.0014(6) 0.0054(6) 0.0010(6) N37 0.0157(7) 0.0160(8) 0.0115(7) -0.0021(6) 0.0045(5) 0.0003(6) N38 0.0146(7) 0.0135(7) 0.0094(7) -0.0002(5) 0.0040(5) -0.0004(6) C39 0.0182(9) 0.0156(9) 0.0092(8) -0.0014(6) 0.0045(6) -0.0013(7) C40 0.0189(9) 0.0166(9) 0.0089(8) 0.0013(7) 0.0011(7) -0.0012(7) C41 0.0170(9) 0.0136(9) 0.0121(8) 0.0013(7) 0.0029(6) 0.0023(7) C42 0.0221(10) 0.0193(10) 0.0184(10) 0.0023(8) 0.0085(7) 0.0084(8) C43 0.0219(10) 0.0200(11) 0.0191(10) -0.0002(8) 0.0085(7) 0.0024(8) C44 0.0194(10) 0.0245(11) 0.0260(11) -0.0021(8) 0.0101(8) 0.0008(8) O45 0.0233(7) 0.0221(8) 0.0204(8) -0.0015(6) 0.0087(6) 0.0042(6) C46 0.0163(9) 0.0185(10) 0.0161(9) -0.0043(7) 0.0077(7) 0.0005(7) C47 0.0213(9) 0.0194(10) 0.0205(10) -0.0027(8) 0.0066(8) 0.0015(8) C48 0.0230(10) 0.0221(11) 0.0188(10) 0.0019(8) 0.0058(7) -0.0021(8) O49 0.0225(8) 0.0350(9) 0.0228(8) 0.0066(6) 0.0022(6) -0.0091(7) P50 0.0226(2) 0.0205(2) 0.0123(2) -0.0009(2) 0.00386(17) 0.0002(2) F51 0.0379(7) 0.0378(8) 0.0251(7) 0.0089(6) 0.0188(5) 0.0032(6) F52 0.0481(8) 0.0595(10) 0.0194(7) -0.0039(6) 0.0153(6) 0.0178(7) F53 0.0248(6) 0.0442(8) 0.0209(6) -0.0002(6) -0.0009(5) 0.0010(6) F54 0.0302(7) 0.0395(8) 0.0328(8) -0.0043(6) -0.0064(5) -0.0038(6) F55 0.0322(6) 0.0227(6) 0.0312(7) 0.0060(5) 0.0145(5) -0.0005(5) F56 0.0528(9) 0.0203(7) 0.0492(9) 0.0013(6) 0.0071(7) 0.0024(6) P57 0.0179(2) 0.0240(3) 0.0180(2) 0.00676(19) 0.00705(18) 0.00544(19) F58 0.0327(7) 0.0244(7) 0.0435(8) 0.0111(6) 0.0079(6) 0.0046(5) F59 0.0287(7) 0.0273(7) 0.0410(8) 0.0116(6) 0.0056(5) 0.0019(5) F60 0.0166(6) 0.0359(7) 0.0282(7) 0.0081(5) 0.0057(5) 0.0050(5) F61 0.0188(6) 0.0420(8) 0.0311(7) 0.0123(6) 0.0111(5) 0.0090(5) F62 0.0358(7) 0.0530(9) 0.0197(6) 0.0006(6) 0.0109(5) 0.0051(6) F63 0.0266(6) 0.0493(8) 0.0193(6) 0.0015(6) 0.0088(5) 0.0038(6) _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 N8 2.0148(14) . ? Ru1 N32 2.0181(14) . ? Ru1 N2 2.0389(14) . ? Ru1 N38 2.0442(14) . ? Ru1 N26 2.0629(14) . ? Ru1 N14 2.0760(15) . ? N2 N3 1.3186(19) . ? N2 C6 1.377(2) . ? N3 N4 1.345(2) . ? N4 C5 1.342(2) . ? N4 C18 1.466(2) . ? C5 C6 1.368(2) . ? C5 H64 0.937(19) . ? C6 C7 1.455(2) . ? C7 N8 1.356(2) . ? C7 C15 1.388(2) . ? N8 C9 1.354(2) . ? C9 C17 1.390(2) . ? C9 C10 1.462(2) . ? C10 C11 1.369(3) . ? C10 N14 1.379(2) . ? C11 N12 1.351(2) . ? C11 H65 0.84(2) . ? N12 N13 1.345(2) . ? N12 C22 1.474(2) . ? N13 N14 1.313(2) . ? C15 C16 1.393(3) . ? C15 H66 0.92(2) . ? C16 C17 1.388(3) . ? C16 H67 0.93(2) . ? C17 H68 0.950(19) . ? C18 C19 1.520(3) . ? C18 H69 0.95(2) . ? C18 H70 0.97(2) . ? C19 C20 1.511(3) . ? C19 H71 1.01(2) . ? C19 H72 1.01(2) . ? C20 O21 1.438(2) . ? C20 H73 1.00(2) . ? C20 H74 1.04(2) . ? O21 H75 0.79(3) . ? C22 C23 1.516(3) . ? C22 H76 0.97(2) . ? C22 H77 0.98(2) . ? C23 C24 1.518(3) . ? C23 H78 0.957(19) . ? C23 H79 0.97(2) . ? C24 O25 1.438(3) . ? C24 H80 0.97(2) . ? C24 H81 1.03(2) . ? O25 H82 0.82(3) . ? N26 N27 1.316(2) . ? N26 C30 1.377(2) . ? N27 N28 1.344(2) . ? N28 C29 1.350(2) . ? N28 C42 1.467(2) . ? C29 C30 1.373(2) . ? C29 H83 0.86(2) . ? C30 C31 1.458(2) . ? C31 N32 1.355(2) . ? C31 C39 1.389(2) . ? N32 C33 1.352(2) . ? C33 C41 1.388(2) . ? C33 C34 1.454(2) . ? C34 C35 1.367(2) . ? C34 N38 1.377(2) . ? C35 N36 1.343(2) . ? C35 H84 0.91(2) . ? N36 N37 1.345(2) . ? N36 C46 1.469(2) . ? N37 N38 1.3188(19) . ? C39 C40 1.393(3) . ? C39 H85 0.964(19) . ? C40 C41 1.390(2) . ? C40 H86 0.89(2) . ? C41 H87 0.92(2) . ? C42 C43 1.516(3) . ? C42 H88 0.98(2) . ? C42 H89 0.94(2) . ? C43 C44 1.518(3) . ? C43 H90 0.94(2) . ? C43 H91 0.97(2) . ? C44 O45 1.433(2) . ? C44 H92 0.98(2) . ? C44 H93 1.00(2) . ? O45 H94 0.77(3) . ? C46 C47 1.519(3) . ? C46 H95 0.951(19) . ? C46 H96 0.966(19) . ? C47 C48 1.508(3) . ? C47 H97 0.99(2) . ? C47 H98 0.98(2) . ? C48 O49 1.427(2) . ? C48 H99 0.98(2) . ? C48 H100 0.97(2) . ? O49 H101 0.80(3) . ? P50 F55 1.5975(13) . ? P50 F54 1.5975(13) . ? P50 F53 1.5982(12) . ? P50 F52 1.5995(13) . ? P50 F56 1.6007(14) . ? P50 F51 1.6016(12) . ? P57 F61 1.5971(12) . ? P57 F60 1.5989(12) . ? P57 F62 1.6010(13) . ? P57 F63 1.6043(13) . ? P57 F59 1.6053(13) . ? P57 F58 1.6055(13) . ? 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 N8 Ru1 N32 174.58(6) . . ? N8 Ru1 N2 79.00(6) . . ? N32 Ru1 N2 96.40(6) . . ? N8 Ru1 N38 98.73(6) . . ? N32 Ru1 N38 78.77(6) . . ? N2 Ru1 N38 95.90(6) . . ? N8 Ru1 N26 104.62(6) . . ? N32 Ru1 N26 77.89(6) . . ? N2 Ru1 N26 87.84(6) . . ? N38 Ru1 N26 156.64(6) . . ? N8 Ru1 N14 77.76(6) . . ? N32 Ru1 N14 106.87(6) . . ? N2 Ru1 N14 156.73(6) . . ? N38 Ru1 N14 88.85(6) . . ? N26 Ru1 N14 96.79(6) . . ? N3 N2 C6 110.51(14) . . ? N3 N2 Ru1 135.11(11) . . ? C6 N2 Ru1 113.78(11) . . ? N2 N3 N4 105.06(13) . . ? C5 N4 N3 112.59(14) . . ? C5 N4 C18 127.44(15) . . ? N3 N4 C18 119.89(14) . . ? N4 C5 C6 105.04(15) . . ? N4 C5 H64 122.0(12) . . ? C6 C5 H64 132.9(12) . . ? C5 C6 N2 106.78(15) . . ? C5 C6 C7 136.15(16) . . ? N2 C6 C7 116.97(15) . . ? N8 C7 C15 120.88(16) . . ? N8 C7 C6 111.48(14) . . ? C15 C7 C6 127.63(16) . . ? C9 N8 C7 120.85(14) . . ? C9 N8 Ru1 120.49(11) . . ? C7 N8 Ru1 118.59(11) . . ? N8 C9 C17 120.66(16) . . ? N8 C9 C10 110.75(14) . . ? C17 C9 C10 128.59(16) . . ? C11 C10 N14 107.01(15) . . ? C11 C10 C9 135.97(16) . . ? N14 C10 C9 117.03(15) . . ? N12 C11 C10 105.04(16) . . ? N12 C11 H65 123.6(16) . . ? C10 C11 H65 131.3(16) . . ? N13 N12 C11 111.82(15) . . ? N13 N12 C22 118.61(15) . . ? C11 N12 C22 129.56(17) . . ? N14 N13 N12 106.00(14) . . ? N13 N14 C10 110.13(14) . . ? N13 N14 Ru1 135.99(11) . . ? C10 N14 Ru1 113.80(11) . . ? C7 C15 C16 118.39(17) . . ? C7 C15 H66 118.6(13) . . ? C16 C15 H66 122.9(13) . . ? C17 C16 C15 120.55(16) . . ? C17 C16 H67 118.2(13) . . ? C15 C16 H67 121.3(13) . . ? C16 C17 C9 118.66(17) . . ? C16 C17 H68 122.4(12) . . ? C9 C17 H68 118.9(12) . . ? N4 C18 C19 112.17(15) . . ? N4 C18 H69 106.4(12) . . ? C19 C18 H69 112.7(12) . . ? N4 C18 H70 106.3(12) . . ? C19 C18 H70 112.3(12) . . ? H69 C18 H70 106.5(16) . . ? C20 C19 C18 115.11(17) . . ? C20 C19 H71 107.2(11) . . ? C18 C19 H71 108.9(11) . . ? C20 C19 H72 105.5(13) . . ? C18 C19 H72 106.5(13) . . ? H71 C19 H72 113.8(17) . . ? O21 C20 C19 113.68(17) . . ? O21 C20 H73 108.5(11) . . ? C19 C20 H73 111.7(11) . . ? O21 C20 H74 110.3(12) . . ? C19 C20 H74 107.7(12) . . ? H73 C20 H74 104.5(16) . . ? C20 O21 H75 109(2) . . ? N12 C22 C23 112.21(16) . . ? N12 C22 H76 104.8(13) . . ? C23 C22 H76 110.3(13) . . ? N12 C22 H77 107.3(12) . . ? C23 C22 H77 109.4(12) . . ? H76 C22 H77 112.7(18) . . ? C22 C23 C24 110.83(17) . . ? C22 C23 H78 108.3(12) . . ? C24 C23 H78 109.1(12) . . ? C22 C23 H79 110.2(13) . . ? C24 C23 H79 108.0(13) . . ? H78 C23 H79 110.4(17) . . ? O25 C24 C23 112.81(17) . . ? O25 C24 H80 110.8(13) . . ? C23 C24 H80 111.1(13) . . ? O25 C24 H81 105.3(12) . . ? C23 C24 H81 105.9(11) . . ? H80 C24 H81 110.7(17) . . ? C24 O25 H82 113(2) . . ? N27 N26 C30 110.41(14) . . ? N27 N26 Ru1 135.48(11) . . ? C30 N26 Ru1 113.97(11) . . ? N26 N27 N28 105.63(13) . . ? N27 N28 C29 112.21(15) . . ? N27 N28 C42 118.37(14) . . ? C29 N28 C42 129.41(16) . . ? N28 C29 C30 104.87(16) . . ? N28 C29 H83 122.7(14) . . ? C30 C29 H83 132.4(14) . . ? C29 C30 N26 106.88(15) . . ? C29 C30 C31 136.09(16) . . ? N26 C30 C31 117.03(15) . . ? N32 C31 C39 120.72(16) . . ? N32 C31 C30 110.78(14) . . ? C39 C31 C30 128.50(16) . . ? C33 N32 C31 120.97(14) . . ? C33 N32 Ru1 118.74(11) . . ? C31 N32 Ru1 119.92(11) . . ? N32 C33 C41 120.94(16) . . ? N32 C33 C34 111.49(14) . . ? C41 C33 C34 127.57(16) . . ? C35 C34 N38 107.12(15) . . ? C35 C34 C33 135.82(16) . . ? N38 C34 C33 117.03(15) . . ? N36 C35 C34 104.92(15) . . ? N36 C35 H84 123.3(14) . . ? C34 C35 H84 131.7(14) . . ? C35 N36 N37 112.46(14) . . ? C35 N36 C46 127.11(15) . . ? N37 N36 C46 120.32(14) . . ? N38 N37 N36 105.34(13) . . ? N37 N38 C34 110.15(14) . . ? N37 N38 Ru1 135.79(11) . . ? C34 N38 Ru1 113.75(11) . . ? C31 C39 C40 118.32(16) . . ? C31 C39 H85 120.0(11) . . ? C40 C39 H85 121.6(11) . . ? C41 C40 C39 120.77(16) . . ? C41 C40 H86 120.6(13) . . ? C39 C40 H86 118.6(13) . . ? C33 C41 C40 118.28(16) . . ? C33 C41 H87 120.8(13) . . ? C40 C41 H87 120.8(13) . . ? N28 C42 C43 113.24(16) . . ? N28 C42 H88 104.5(11) . . ? C43 C42 H88 109.9(12) . . ? N28 C42 H89 107.1(12) . . ? C43 C42 H89 110.1(12) . . ? H88 C42 H89 111.9(16) . . ? C42 C43 C44 109.50(16) . . ? C42 C43 H90 108.5(12) . . ? C44 C43 H90 109.8(12) . . ? C42 C43 H91 109.8(13) . . ? C44 C43 H91 106.3(12) . . ? H90 C43 H91 112.9(17) . . ? O45 C44 C43 113.05(16) . . ? O45 C44 H92 104.7(12) . . ? C43 C44 H92 111.8(12) . . ? O45 C44 H93 110.3(12) . . ? C43 C44 H93 109.0(12) . . ? H92 C44 H93 107.9(17) . . ? C44 O45 H94 109.8(19) . . ? N36 C46 C47 111.20(15) . . ? N36 C46 H95 106.2(11) . . ? C47 C46 H95 113.3(11) . . ? N36 C46 H96 103.8(11) . . ? C47 C46 H96 115.7(11) . . ? H95 C46 H96 105.8(15) . . ? C48 C47 C46 113.32(16) . . ? C48 C47 H97 107.9(12) . . ? C46 C47 H97 111.9(12) . . ? C48 C47 H98 111.3(13) . . ? C46 C47 H98 106.8(13) . . ? H97 C47 H98 105.3(17) . . ? O49 C48 C47 109.61(17) . . ? O49 C48 H99 110.8(13) . . ? C47 C48 H99 111.7(13) . . ? O49 C48 H100 110.9(12) . . ? C47 C48 H100 108.5(12) . . ? H99 C48 H100 105.2(17) . . ? C48 O49 H101 109(2) . . ? F55 P50 F54 89.59(7) . . ? F55 P50 F53 90.39(7) . . ? F54 P50 F53 179.89(9) . . ? F55 P50 F52 90.01(7) . . ? F54 P50 F52 90.20(8) . . ? F53 P50 F52 89.69(7) . . ? F55 P50 F56 179.58(8) . . ? F54 P50 F56 90.24(7) . . ? F53 P50 F56 89.77(7) . . ? F52 P50 F56 90.38(8) . . ? F55 P50 F51 89.67(7) . . ? F54 P50 F51 90.35(7) . . ? F53 P50 F51 89.76(7) . . ? F52 P50 F51 179.36(8) . . ? F56 P50 F51 89.94(7) . . ? F61 P57 F60 179.84(9) . . ? F61 P57 F62 90.29(7) . . ? F60 P57 F62 89.87(7) . . ? F61 P57 F63 89.65(7) . . ? F60 P57 F63 90.19(6) . . ? F62 P57 F63 179.77(8) . . ? F61 P57 F59 90.12(7) . . ? F60 P57 F59 89.84(7) . . ? F62 P57 F59 89.69(7) . . ? F63 P57 F59 90.09(7) . . ? F61 P57 F58 90.15(7) . . ? F60 P57 F58 89.89(7) . . ? F62 P57 F58 90.59(7) . . ? F63 P57 F58 89.63(7) . . ? F59 P57 F58 179.61(8) . . ? 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 N8 Ru1 N2 N3 172.27(17) . . . . ? N32 Ru1 N2 N3 -10.63(17) . . . . ? N38 Ru1 N2 N3 -89.95(16) . . . . ? N26 Ru1 N2 N3 66.93(16) . . . . ? N14 Ru1 N2 N3 169.15(14) . . . . ? N8 Ru1 N2 C6 2.14(12) . . . . ? N32 Ru1 N2 C6 179.24(12) . . . . ? N38 Ru1 N2 C6 99.93(12) . . . . ? N26 Ru1 N2 C6 -103.20(12) . . . . ? N14 Ru1 N2 C6 -1.0(2) . . . . ? C6 N2 N3 N4 0.03(18) . . . . ? Ru1 N2 N3 N4 -170.32(12) . . . . ? N2 N3 N4 C5 -0.30(19) . . . . ? N2 N3 N4 C18 -177.37(15) . . . . ? N3 N4 C5 C6 0.4(2) . . . . ? C18 N4 C5 C6 177.24(16) . . . . ? N4 C5 C6 N2 -0.39(19) . . . . ? N4 C5 C6 C7 175.84(19) . . . . ? N3 N2 C6 C5 0.2(2) . . . . ? Ru1 N2 C6 C5 172.80(11) . . . . ? N3 N2 C6 C7 -176.84(14) . . . . ? Ru1 N2 C6 C7 -4.27(19) . . . . ? C5 C6 C7 N8 -171.5(2) . . . . ? N2 C6 C7 N8 4.5(2) . . . . ? C5 C6 C7 C15 8.2(3) . . . . ? N2 C6 C7 C15 -175.83(17) . . . . ? C15 C7 N8 C9 0.8(3) . . . . ? C6 C7 N8 C9 -179.43(15) . . . . ? C15 C7 N8 Ru1 177.68(13) . . . . ? C6 C7 N8 Ru1 -2.58(19) . . . . ? N38 Ru1 N8 C9 82.84(13) . . . . ? N26 Ru1 N8 C9 -97.99(13) . . . . ? N14 Ru1 N8 C9 -4.05(13) . . . . ? N2 Ru1 N8 C7 0.34(12) . . . . ? N38 Ru1 N8 C7 -94.02(13) . . . . ? N26 Ru1 N8 C7 85.15(13) . . . . ? N14 Ru1 N8 C7 179.08(13) . . . . ? C7 N8 C9 C17 0.3(3) . . . . ? Ru1 N8 C9 C17 -176.52(13) . . . . ? C7 N8 C9 C10 -179.32(15) . . . . ? Ru1 N8 C9 C10 3.89(19) . . . . ? N8 C9 C10 C11 178.7(2) . . . . ? C17 C9 C10 C11 -0.9(4) . . . . ? N8 C9 C10 N14 -0.9(2) . . . . ? C17 C9 C10 N14 179.59(17) . . . . ? N14 C10 C11 N12 -0.6(2) . . . . ? C9 C10 C11 N12 179.9(2) . . . . ? C10 C11 N12 N13 0.2(2) . . . . ? C10 C11 N12 C22 179.52(19) . . . . ? C11 N12 N13 N14 0.3(2) . . . . ? C22 N12 N13 N14 -179.13(16) . . . . ? N12 N13 N14 C10 -0.66(19) . . . . ? N12 N13 N14 Ru1 -177.11(13) . . . . ? C11 C10 N14 N13 0.8(2) . . . . ? C9 C10 N14 N13 -179.56(15) . . . . ? C11 C10 N14 Ru1 178.09(12) . . . . ? C9 C10 N14 Ru1 -2.25(19) . . . . ? N8 Ru1 N14 N13 179.56(18) . . . . ? N32 Ru1 N14 N13 2.47(18) . . . . ? N2 Ru1 N14 N13 -177.31(15) . . . . ? N38 Ru1 N14 N13 80.37(17) . . . . ? N26 Ru1 N14 N13 -76.89(17) . . . . ? N8 Ru1 N14 C10 3.20(12) . . . . ? N32 Ru1 N14 C10 -173.89(11) . . . . ? N2 Ru1 N14 C10 6.3(2) . . . . ? N38 Ru1 N14 C10 -95.99(12) . . . . ? N26 Ru1 N14 C10 106.74(12) . . . . ? N8 C7 C15 C16 -1.0(3) . . . . ? C6 C7 C15 C16 179.29(17) . . . . ? C7 C15 C16 C17 0.1(3) . . . . ? C15 C16 C17 C9 0.9(3) . . . . ? N8 C9 C17 C16 -1.1(3) . . . . ? C10 C9 C17 C16 178.37(18) . . . . ? C5 N4 C18 C19 -103.5(2) . . . . ? N3 N4 C18 C19 73.1(2) . . . . ? N4 C18 C19 C20 58.5(2) . . . . ? C18 C19 C20 O21 -81.0(2) . . . . ? N13 N12 C22 C23 -130.83(19) . . . . ? C11 N12 C22 C23 49.9(3) . . . . ? N12 C22 C23 C24 167.94(18) . . . . ? C22 C23 C24 O25 49.4(2) . . . . ? N8 Ru1 N26 N27 4.84(17) . . . . ? N32 Ru1 N26 N27 179.90(17) . . . . ? N2 Ru1 N26 N27 82.89(16) . . . . ? N38 Ru1 N26 N27 -177.22(14) . . . . ? N14 Ru1 N26 N27 -74.23(17) . . . . ? N8 Ru1 N26 C30 -170.28(11) . . . . ? N32 Ru1 N26 C30 4.77(11) . . . . ? N2 Ru1 N26 C30 -92.24(12) . . . . ? N38 Ru1 N26 C30 7.7(2) . . . . ? N14 Ru1 N26 C30 110.64(12) . . . . ? C30 N26 N27 N28 -0.28(18) . . . . ? Ru1 N26 N27 N28 -175.53(12) . . . . ? N26 N27 N28 C29 0.1(2) . . . . ? N26 N27 N28 C42 -179.34(15) . . . . ? N27 N28 C29 C30 0.1(2) . . . . ? C42 N28 C29 C30 179.47(18) . . . . ? N28 C29 C30 N26 -0.3(2) . . . . ? N28 C29 C30 C31 179.81(19) . . . . ? N27 N26 C30 C29 0.3(2) . . . . ? Ru1 N26 C30 C29 176.70(12) . . . . ? N27 N26 C30 C31 -179.71(14) . . . . ? Ru1 N26 C30 C31 -3.35(19) . . . . ? C29 C30 C31 N32 178.6(2) . . . . ? N26 C30 C31 N32 -1.3(2) . . . . ? C29 C30 C31 C39 -1.7(3) . . . . ? N26 C30 C31 C39 178.37(17) . . . . ? C39 C31 N32 C33 -1.0(2) . . . . ? C30 C31 N32 C33 178.71(15) . . . . ? C39 C31 N32 Ru1 -173.95(13) . . . . ? C30 C31 N32 Ru1 5.78(19) . . . . ? N2 Ru1 N32 C33 -92.71(13) . . . . ? N26 Ru1 N32 C33 -179.11(13) . . . . ? N14 Ru1 N32 C33 87.37(13) . . . . ? N2 Ru1 N32 C31 80.37(13) . . . . ? N38 Ru1 N32 C31 175.14(13) . . . . ? N26 Ru1 N32 C31 -6.03(12) . . . . ? N14 Ru1 N32 C31 -99.54(13) . . . . ? C31 N32 C33 C41 1.6(3) . . . . ? Ru1 N32 C33 C41 174.64(13) . . . . ? C31 N32 C33 C34 -177.42(15) . . . . ? Ru1 N32 C33 C34 -4.42(19) . . . . ? N32 C33 C34 C35 -172.41(19) . . . . ? C41 C33 C34 C35 8.6(3) . . . . ? N32 C33 C34 N38 5.2(2) . . . . ? C41 C33 C34 N38 -173.75(17) . . . . ? N38 C34 C35 N36 -0.09(19) . . . . ? C33 C34 C35 N36 177.72(19) . . . . ? C34 C35 N36 N37 0.3(2) . . . . ? C34 C35 N36 C46 176.52(16) . . . . ? C35 N36 N37 N38 -0.41(19) . . . . ? C46 N36 N37 N38 -176.91(15) . . . . ? N36 N37 N38 C34 0.34(18) . . . . ? N36 N37 N38 Ru1 -172.77(12) . . . . ? C35 C34 N38 N37 -0.16(19) . . . . ? C33 C34 N38 N37 -178.45(14) . . . . ? C35 C34 N38 Ru1 174.60(11) . . . . ? C33 C34 N38 Ru1 -3.69(19) . . . . ? N8 Ru1 N38 N37 -10.97(17) . . . . ? N32 Ru1 N38 N37 173.91(17) . . . . ? N2 Ru1 N38 N37 -90.71(16) . . . . ? N26 Ru1 N38 N37 171.04(14) . . . . ? N14 Ru1 N38 N37 66.46(16) . . . . ? N8 Ru1 N38 C34 176.09(12) . . . . ? N32 Ru1 N38 C34 0.98(11) . . . . ? N2 Ru1 N38 C34 96.35(12) . . . . ? N26 Ru1 N38 C34 -1.9(2) . . . . ? N14 Ru1 N38 C34 -106.48(12) . . . . ? N32 C31 C39 C40 -0.3(3) . . . . ? C30 C31 C39 C40 -179.97(17) . . . . ? C31 C39 C40 C41 1.0(3) . . . . ? N32 C33 C41 C40 -0.9(3) . . . . ? C34 C33 C41 C40 178.00(17) . . . . ? C39 C40 C41 C33 -0.4(3) . . . . ? N27 N28 C42 C43 -129.49(18) . . . . ? C29 N28 C42 C43 51.2(3) . . . . ? N28 C42 C43 C44 168.68(16) . . . . ? C42 C43 C44 O45 59.5(2) . . . . ? C35 N36 C46 C47 -72.2(2) . . . . ? N37 N36 C46 C47 103.74(18) . . . . ? N36 C46 C47 C48 -55.8(2) . . . . ? C46 C47 C48 O49 -57.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.988 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.084