Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Mike Ward' _publ_contact_author_address ; Prof. Mike Ward Department of Chemistry University of Sheffield SHEFFIELD S3 7HF ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Three component Coordination Networks based on [Ru(phen)(Cn)4]-2 anions, lanthanide(III) cations and ancillary oligopyridine ligands ; _publ_contact_letter ; This CIF file contains details of the 3 crystal structures in the paper Three component coordination networks based on... by S. G. Baca et al, submitted to Cryst. Eng. Comm. for publication. ; loop_ _publ_author_name 'Mike Ward' 'Harry Adams' 'Svetlana G. Baca' #======================================================== data_imw538m _database_code_depnum_ccdc_archive 'CCDC 605806' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H82 N24 O18 Pr2 Ru3' _chemical_formula_weight 2228.71 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.956(2) _cell_length_b 27.560(6) _cell_length_c 31.900(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9632(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5806 _exptl_absorpt_correction_T_max 0.9141 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 195548 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 27.59 _reflns_number_total 22254 _reflns_number_gt 19108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0813P)^2^+27.0584P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.439(13) _refine_ls_number_reflns 22254 _refine_ls_number_parameters 1120 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.077 _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 Pr1 Pr 0.13963(3) 0.670399(11) 0.507068(12) 0.02407(8) Uani 1 1 d . . . Pr2 Pr 0.40047(3) 0.330705(12) 0.500153(16) 0.03751(12) Uani 1 1 d . . . Ru1 Ru 0.12415(5) 0.861409(17) 0.471268(19) 0.02745(12) Uani 1 1 d . . . Ru2 Ru 0.41566(4) 0.133069(17) 0.525718(18) 0.02434(12) Uani 1 1 d . A . Ru3 Ru 0.20264(8) 0.23825(3) 0.24935(2) 0.0551(2) Uani 1 1 d . . . C1 C 0.1175(7) 0.7921(3) 0.3923(3) 0.0413(18) Uani 1 1 d . . . H1 H 0.1070 0.7667 0.4111 0.050 Uiso 1 1 calc R . . C2 C 0.1160(9) 0.7821(4) 0.3499(3) 0.056(2) Uani 1 1 d . . . H2 H 0.1023 0.7505 0.3407 0.067 Uiso 1 1 calc R . . C3 C 0.1344(11) 0.8179(5) 0.3215(3) 0.074(3) Uani 1 1 d . . . H3 H 0.1341 0.8109 0.2929 0.089 Uiso 1 1 calc R . . C4 C 0.1545(10) 0.8673(5) 0.3358(3) 0.072(3) Uani 1 1 d . . . C5 C 0.1752(13) 0.9097(6) 0.3097(4) 0.091(5) Uani 1 1 d . . . H5 H 0.1727 0.9054 0.2808 0.109 Uiso 1 1 calc R . . C6 C 0.1961(13) 0.9518(5) 0.3233(4) 0.090(5) Uani 1 1 d . . . H6 H 0.2153 0.9764 0.3045 0.108 Uiso 1 1 calc R . . C7 C 0.1904(10) 0.9630(4) 0.3700(4) 0.077(4) Uani 1 1 d . . . C8 C 0.2068(10) 1.0080(4) 0.3872(4) 0.083(4) Uani 1 1 d . . . H8 H 0.2205 1.0349 0.3703 0.100 Uiso 1 1 calc R . . C9 C 0.2028(9) 1.0124(3) 0.4297(4) 0.071(4) Uani 1 1 d . . . H9 H 0.2141 1.0427 0.4420 0.086 Uiso 1 1 calc R . . C10 C 0.1816(7) 0.9715(3) 0.4548(4) 0.052(3) Uani 1 1 d . . . H10 H 0.1791 0.9755 0.4837 0.063 Uiso 1 1 calc R . . C11 C 0.1685(7) 0.9222(3) 0.3967(3) 0.049(2) Uani 1 1 d . . . C12 C 0.1518(8) 0.8747(3) 0.3798(3) 0.049(2) Uani 1 1 d . . . C13 C 0.0851(6) 0.7967(2) 0.4936(2) 0.0251(13) Uani 1 1 d . . . C14 C -0.0606(6) 0.8707(2) 0.4667(2) 0.0296(15) Uani 1 1 d . . . C15 C 0.3056(6) 0.8492(2) 0.4802(2) 0.0251(14) Uani 1 1 d . . . C16 C 0.1140(6) 0.8876(2) 0.5298(3) 0.0303(15) Uani 1 1 d . . . C17 C 0.0602(8) 0.7196(4) 0.6041(3) 0.050(2) Uani 1 1 d . . . H17 H 0.0877 0.7464 0.5891 0.060 Uiso 1 1 calc R . . C18 C 0.0111(12) 0.7285(6) 0.6433(3) 0.081(4) Uani 1 1 d . . . H18 H 0.0076 0.7593 0.6553 0.097 Uiso 1 1 calc R . . C19 C -0.0352(16) 0.6845(9) 0.6644(5) 0.133(8) Uani 1 1 d . . . H19 H -0.0731 0.6868 0.6904 0.160 Uiso 1 1 calc R . . C20 C -0.0213(12) 0.6385(7) 0.6447(4) 0.100(5) Uani 1 1 d . . . H20 H -0.0496 0.6107 0.6580 0.120 Uiso 1 1 calc R . . C21 C 0.0328(8) 0.6351(4) 0.6069(3) 0.058(3) Uani 1 1 d . . . C22 C 0.0523(8) 0.5882(4) 0.5876(4) 0.066(3) Uani 1 1 d . . . C23 C 0.0322(12) 0.5447(5) 0.6100(4) 0.090(5) Uani 1 1 d . . . H23 H 0.0086 0.5462 0.6380 0.108 Uiso 1 1 calc R . . C24 C 0.0465(15) 0.5017(5) 0.5920(6) 0.117(7) Uani 1 1 d . . . H24 H 0.0310 0.4734 0.6069 0.141 Uiso 1 1 calc R . . C25 C 0.0842(13) 0.4995(4) 0.5511(6) 0.111(7) Uani 1 1 d . . . H25 H 0.0956 0.4694 0.5384 0.133 Uiso 1 1 calc R . . C26 C 0.1068(8) 0.5438(3) 0.5271(4) 0.063(3) Uani 1 1 d . . . C27 C 0.1495(8) 0.5447(3) 0.4842(4) 0.060(3) Uani 1 1 d . . . C28 C 0.1727(10) 0.5005(3) 0.4619(6) 0.086(5) Uani 1 1 d . . . H28 H 0.1601 0.4709 0.4751 0.104 Uiso 1 1 calc R . . C29 C 0.2131(14) 0.5016(5) 0.4213(7) 0.134(9) Uani 1 1 d . . . H29 H 0.2272 0.4731 0.4064 0.160 Uiso 1 1 calc R . . C30 C 0.2323(13) 0.5465(5) 0.4032(5) 0.092(5) Uani 1 1 d . . . H30 H 0.2611 0.5491 0.3759 0.111 Uiso 1 1 calc R . . C31 C 0.2073(11) 0.5879(4) 0.4270(4) 0.071(3) Uani 1 1 d . . . H31 H 0.2183 0.6179 0.4143 0.085 Uiso 1 1 calc R . . C32 C 0.3943(8) 0.1855(3) 0.6128(3) 0.051(2) Uani 1 1 d . A . H32 H 0.3969 0.2142 0.5975 0.062 Uiso 1 1 calc R . . C33 C 0.3889(10) 0.1886(4) 0.6553(4) 0.066(3) Uani 1 1 d . . . H33 H 0.3886 0.2187 0.6685 0.079 Uiso 1 1 calc R . . C34 C 0.3839(10) 0.1474(6) 0.6780(4) 0.085(4) Uani 1 1 d . . . H34 H 0.3823 0.1493 0.7071 0.102 Uiso 1 1 calc R . . C35 C 0.3809(10) 0.0995(4) 0.6579(3) 0.061(3) Uani 1 1 d . . . C36 C 0.3714(12) 0.0560(5) 0.6792(3) 0.074(3) Uani 1 1 d . . . H36 H 0.3643 0.0557 0.7083 0.089 Uiso 1 1 calc R . . C37 C 0.3724(10) 0.0123(5) 0.6568(3) 0.075(4) Uani 1 1 d . . . H37 H 0.3712 -0.0168 0.6714 0.090 Uiso 1 1 calc R . . C38 C 0.3751(8) 0.0113(3) 0.6117(3) 0.049(2) Uani 1 1 d . . . C39 C 0.3677(8) -0.0309(3) 0.5878(3) 0.049(2) Uani 1 1 d . . . H39 H 0.3630 -0.0611 0.6006 0.059 Uiso 1 1 calc R . . C40 C 0.3678(8) -0.0269(3) 0.5460(3) 0.048(2) Uani 1 1 d . . . H40 H 0.3624 -0.0547 0.5296 0.058 Uiso 1 1 calc R . . C41 C 0.3759(7) 0.0195(2) 0.5263(3) 0.0373(17) Uani 1 1 d . A . H41 H 0.3751 0.0210 0.4971 0.045 Uiso 1 1 calc R . . C42 C 0.3812(7) 0.0576(3) 0.5910(2) 0.0352(16) Uani 1 1 d . A . C43 C 0.3853(7) 0.1013(3) 0.6137(3) 0.0435(19) Uani 1 1 d . A . C44 C 0.4505(6) 0.2012(2) 0.5138(3) 0.0345(17) Uani 1 1 d . . . C45 C 0.2327(6) 0.1475(2) 0.5145(2) 0.0296(15) Uani 1 1 d . . . C46 C 0.6005(6) 0.12558(19) 0.5308(2) 0.0233(13) Uani 1 1 d . . . C47 C 0.4327(7) 0.1178(2) 0.4650(3) 0.0350(16) Uani 1 1 d . . . C48 C 0.3945(10) 0.4270(3) 0.5728(3) 0.062(3) Uani 1 1 d . . . H48 H 0.3881 0.4006 0.5908 0.074 Uiso 1 1 calc R A . C49 C 0.3780(11) 0.4733(4) 0.5892(3) 0.064(3) Uani 1 1 d . A . H49 H 0.3608 0.4772 0.6175 0.077 Uiso 1 1 calc R . . C50 C 0.3870(9) 0.5122(3) 0.5642(3) 0.056(2) Uani 1 1 d . . . H50 H 0.3743 0.5432 0.5748 0.067 Uiso 1 1 calc R A . C51 C 0.4157(7) 0.5053(2) 0.5220(3) 0.0381(18) Uani 1 1 d . A . H51 H 0.4220 0.5319 0.5043 0.046 Uiso 1 1 calc R . . C52 C 0.4356(6) 0.4576(2) 0.5058(3) 0.0313(15) Uani 1 1 d . . . C53 C 0.4731(6) 0.4476(2) 0.4628(3) 0.0340(16) Uani 1 1 d . A . C54 C 0.5170(8) 0.4851(3) 0.4364(3) 0.0428(19) Uani 1 1 d . . . H54 H 0.5194 0.5168 0.4464 0.051 Uiso 1 1 calc R A . C55 C 0.5551(9) 0.4756(3) 0.3975(3) 0.052(2) Uani 1 1 d . A . H55 H 0.5831 0.5005 0.3804 0.062 Uiso 1 1 calc R . . C56 C 0.5524(9) 0.4274(4) 0.3826(3) 0.054(2) Uani 1 1 d . . . H56 H 0.5778 0.4198 0.3555 0.065 Uiso 1 1 calc R A . C57 C 0.5098(7) 0.3912(3) 0.4100(3) 0.0421(19) Uani 1 1 d . A . C58 C 0.5080(8) 0.3385(3) 0.3966(3) 0.049(2) Uani 1 1 d . . . C59 C 0.5587(13) 0.3239(5) 0.3593(4) 0.091(4) Uani 1 1 d . A . H59 H 0.5960 0.3456 0.3410 0.109 Uiso 1 1 calc R . . C60 C 0.5505(16) 0.2727(7) 0.3501(6) 0.116(7) Uani 1 1 d . . . H60 H 0.5872 0.2607 0.3260 0.139 Uiso 1 1 calc R A . C61 C 0.4946(19) 0.2435(6) 0.3742(6) 0.115(7) Uani 1 1 d . A . H61 H 0.4823 0.2114 0.3663 0.138 Uiso 1 1 calc R . . C62 C 0.4541(13) 0.2598(4) 0.4107(4) 0.081(4) Uani 1 1 d . . . H62 H 0.4230 0.2370 0.4293 0.097 Uiso 1 1 calc R A . C63 C 0.2037(11) 0.2887(6) 0.3373(3) 0.091(5) Uani 1 1 d . . . H63 H 0.2078 0.2583 0.3498 0.110 Uiso 1 1 calc R . . C64 C 0.2007(11) 0.3343(9) 0.3628(4) 0.127(9) Uani 1 1 d . . . H64 H 0.2110 0.3313 0.3916 0.152 Uiso 1 1 calc R . . C65 C 0.1861(14) 0.3737(8) 0.3491(7) 0.144(11) Uani 1 1 d . . . H65 H 0.1775 0.3999 0.3673 0.173 Uiso 1 1 calc R . . C66 C 0.1815(12) 0.3820(6) 0.3027(4) 0.083(4) Uani 1 1 d . . . C67 C 0.1719(16) 0.4269(7) 0.2850(6) 0.119(7) Uani 1 1 d . . . H67 H 0.1728 0.4540 0.3024 0.143 Uiso 1 1 calc R . . C68 C 0.1612(16) 0.4337(5) 0.2433(8) 0.139(9) Uani 1 1 d . . . H68 H 0.1476 0.4648 0.2330 0.167 Uiso 1 1 calc R . . C69 C 0.1710(11) 0.3919(6) 0.2131(5) 0.095(5) Uani 1 1 d . . . C70 C 0.1658(11) 0.3921(5) 0.1681(5) 0.080(4) Uani 1 1 d . . . H70 H 0.1555 0.4209 0.1534 0.096 Uiso 1 1 calc R . . C71 C 0.1762(9) 0.3494(5) 0.1477(4) 0.070(3) Uani 1 1 d . . . H71 H 0.1753 0.3493 0.1186 0.084 Uiso 1 1 calc R . . C72 C 0.1882(8) 0.3062(4) 0.1688(3) 0.055(2) Uani 1 1 d . . . H72 H 0.1950 0.2781 0.1529 0.066 Uiso 1 1 calc R . . C73 C 0.1826(9) 0.3436(4) 0.2345(4) 0.064(3) Uani 1 1 d . . . C74 C 0.1879(9) 0.3387(5) 0.2797(3) 0.071(4) Uani 1 1 d . . . C75 C 0.3888(9) 0.2381(4) 0.2478(3) 0.058(3) Uani 1 1 d . . . C76 C 0.2119(12) 0.1862(6) 0.2908(3) 0.084(4) Uani 1 1 d . . . C77 C 0.2023(10) 0.1930(4) 0.2016(3) 0.064(3) Uani 1 1 d . . . C78 C 0.0203(12) 0.2350(5) 0.2523(3) 0.072(3) Uani 1 1 d . . . N1 N 0.1650(5) 0.9276(2) 0.4391(2) 0.0394(16) Uani 1 1 d . . . N2 N 0.1336(5) 0.8377(2) 0.4077(2) 0.0366(14) Uani 1 1 d . . . N3 N 0.1075(7) 0.9005(2) 0.5645(2) 0.0448(17) Uani 1 1 d . . . N4 N 0.0576(5) 0.75763(19) 0.50569(19) 0.0285(12) Uani 1 1 d . . . N5 N 0.1691(7) 0.5873(2) 0.4664(3) 0.0498(19) Uani 1 1 d . . . N6 N 0.0877(6) 0.5869(3) 0.5468(3) 0.052(2) Uani 1 1 d . . . N7 N 0.0723(6) 0.6754(3) 0.5853(2) 0.0430(16) Uani 1 1 d . . . N8 N -0.1648(5) 0.87150(19) 0.4665(2) 0.0337(14) Uani 1 1 d . . . N9 N 0.3960(6) 0.1435(2) 0.5916(2) 0.0383(15) Uani 1 1 d . . . N10 N 0.4388(8) 0.1109(3) 0.4292(2) 0.052(2) Uani 1 1 d . A . N11 N 0.4722(6) 0.2422(2) 0.5073(3) 0.0499(19) Uani 1 1 d . A . N12 N 0.3848(5) 0.0607(2) 0.54775(19) 0.0287(12) Uani 1 1 d . . . N13 N 0.4683(6) 0.4013(2) 0.4490(2) 0.0355(14) Uani 1 1 d . A . N14 N 0.4196(7) 0.4185(2) 0.5318(2) 0.0454(17) Uani 1 1 d . A . N15 N 0.4539(7) 0.3069(2) 0.4232(3) 0.052(2) Uani 1 1 d . A . N16 N 0.7074(5) 0.12643(19) 0.5301(2) 0.0292(12) Uani 1 1 d . . . N17 N 0.2002(8) 0.2940(4) 0.2951(2) 0.062(2) Uani 1 1 d . . . N18 N 0.1909(7) 0.3013(3) 0.2122(2) 0.056(2) Uani 1 1 d . . . N19 N 0.4951(9) 0.2349(5) 0.2476(3) 0.089(4) Uani 1 1 d . . . N20 N -0.0896(10) 0.2346(4) 0.2554(3) 0.079(3) Uani 1 1 d . . . N21 N 0.4095(5) 0.84286(19) 0.48703(19) 0.0308(13) Uani 1 1 d . . . N22 N 0.2072(11) 0.1679(4) 0.1716(3) 0.087(3) Uani 1 1 d . . . N23 N 0.2176(13) 0.1531(6) 0.3153(4) 0.128(6) Uani 1 1 d . . . N24 N 0.1349(5) 0.1588(2) 0.5064(2) 0.0356(13) Uani 1 1 d . . . O1 O 0.0386(5) 0.67875(19) 0.43585(17) 0.0381(12) Uani 1 1 d . . . O2 O 0.2958(5) 0.7048(2) 0.45539(18) 0.0446(13) Uani 1 1 d . . . O3 O 0.2916(5) 0.72909(17) 0.54441(18) 0.0381(12) Uani 1 1 d . . . O4 O 0.2258(11) 0.3415(4) 0.5603(4) 0.042(3) Uiso 0.505(6) 1 d PU A 1 O4' O 0.2350(15) 0.3159(6) 0.5501(5) 0.069(4) Uiso 0.495(6) 1 d PU A 2 O5 O 0.4898(6) 0.3194(2) 0.5722(2) 0.0566(17) Uani 1 1 d . A . O6 O 0.2324(9) 0.2689(3) 0.4884(3) 0.0272(19) Uiso 0.505(6) 1 d PU A 1 O6' O 0.2355(12) 0.2723(4) 0.4601(4) 0.047(3) Uiso 0.495(6) 1 d PU A 2 O7 O 0.2144(6) 0.18182(18) 0.08313(17) 0.0402(13) Uani 1 1 d . . . O8 O 0.4361(11) 0.1015(3) 0.3420(2) 0.097(3) Uani 1 1 d . . . O9 O 0.0398(10) 0.6419(5) 0.3567(3) 0.119(4) Uani 1 1 d . . . O10 O 0.7086(15) 0.3395(6) 0.6020(5) 0.064(3) Uiso 0.505(6) 1 d PU A 1 O10' O 0.7386(14) 0.3182(5) 0.5917(5) 0.057(3) Uiso 0.495(6) 1 d PU A 2 O11 O 0.3845(16) 0.9125(7) 0.2220(5) 0.075(3) Uiso 0.505(6) 1 d PU A 1 O11' O 0.3948(16) 0.8852(6) 0.2280(5) 0.073(3) Uiso 0.495(6) 1 d PU A 2 O12 O 0.6861(15) 0.2961(6) 0.2616(4) 0.168(6) Uani 1 1 d . . . O13 O 0.748(2) 0.0360(8) 0.3102(7) 0.118(7) Uiso 0.505(6) 1 d P A 1 O13' O 0.5110(13) 0.0162(5) 0.3033(4) 0.059(4) Uiso 0.495(6) 1 d P A 2 O14 O 0.149(2) 0.0550(6) 0.2545(7) 0.243(10) Uani 1 1 d . . . O15 O 0.4286(17) 0.6696(6) 0.3960(5) 0.078(3) Uiso 0.505(6) 1 d PU A 1 O15' O 0.3315(16) 0.6763(6) 0.3746(5) 0.076(3) Uiso 0.495(6) 1 d PU A 2 O16 O 0.4326(15) 0.6537(5) 0.3095(5) 0.069(4) Uiso 0.505(6) 1 d P A 1 O16' O 0.2836(17) 0.6894(6) 0.2875(5) 0.080(5) Uiso 0.495(6) 1 d P A 2 O17 O 0.6355(16) 0.5868(6) 0.3444(5) 0.075(3) Uiso 0.505(6) 1 d PU A 1 O17' O 0.5508(17) 0.6152(6) 0.3578(5) 0.078(3) Uiso 0.495(6) 1 d PU A 2 O18 O 0.3782(19) 0.0027(8) 0.2320(4) 0.221(9) Uani 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 Pr1 0.01777(16) 0.01527(14) 0.03916(19) 0.00291(14) 0.00106(14) -0.00140(11) Pr2 0.01368(17) 0.01624(15) 0.0826(3) 0.01146(19) -0.00513(18) -0.00231(11) Ru1 0.0164(2) 0.0182(2) 0.0477(3) 0.0091(2) 0.0010(2) 0.00004(17) Ru2 0.0140(2) 0.0169(2) 0.0421(3) -0.0034(2) -0.0006(2) 0.00075(17) Ru3 0.0446(5) 0.0939(6) 0.0269(3) -0.0057(4) -0.0046(3) 0.0159(4) C1 0.032(4) 0.040(4) 0.052(5) 0.005(3) -0.001(4) -0.005(3) C2 0.055(6) 0.068(6) 0.044(5) -0.002(4) -0.006(4) -0.011(5) C3 0.065(7) 0.104(9) 0.053(6) 0.004(6) -0.009(5) -0.033(7) C4 0.050(6) 0.113(9) 0.053(6) 0.037(6) -0.010(5) -0.023(6) C5 0.096(10) 0.128(12) 0.049(6) 0.044(7) -0.019(6) -0.035(9) C6 0.097(10) 0.099(9) 0.074(8) 0.052(7) -0.029(7) -0.044(8) C7 0.056(6) 0.082(7) 0.092(8) 0.062(7) -0.029(6) -0.031(6) C8 0.059(7) 0.065(7) 0.126(11) 0.070(7) -0.048(7) -0.035(5) C9 0.041(5) 0.041(5) 0.131(11) 0.042(6) -0.032(6) -0.012(4) C10 0.023(4) 0.033(4) 0.101(8) 0.023(4) -0.013(4) -0.010(3) C11 0.026(4) 0.058(5) 0.064(6) 0.037(4) -0.009(4) -0.010(3) C12 0.033(4) 0.055(5) 0.059(6) 0.022(4) -0.006(4) -0.013(4) C13 0.018(3) 0.020(3) 0.038(4) -0.001(3) 0.001(3) 0.006(2) C14 0.020(3) 0.018(3) 0.052(4) 0.005(3) -0.002(3) -0.001(2) C15 0.016(3) 0.015(3) 0.044(4) 0.009(2) 0.002(3) 0.002(2) C16 0.022(3) 0.016(3) 0.052(5) 0.004(3) 0.002(3) -0.002(2) C17 0.033(5) 0.072(6) 0.046(5) 0.008(4) 0.010(4) 0.013(4) C18 0.072(8) 0.135(12) 0.036(6) -0.003(6) 0.009(5) 0.027(8) C19 0.097(12) 0.23(2) 0.074(10) 0.067(13) 0.044(9) 0.043(14) C20 0.061(8) 0.167(16) 0.072(9) 0.051(10) 0.011(7) -0.026(10) C21 0.025(4) 0.090(8) 0.059(6) 0.042(5) -0.004(4) -0.011(4) C22 0.032(5) 0.069(6) 0.096(8) 0.052(6) -0.022(5) -0.023(4) C23 0.077(9) 0.089(9) 0.104(10) 0.065(8) -0.036(7) -0.044(7) C24 0.119(13) 0.074(9) 0.159(15) 0.082(10) -0.063(11) -0.058(9) C25 0.099(10) 0.055(7) 0.180(16) 0.066(9) -0.096(11) -0.046(7) C26 0.039(5) 0.017(3) 0.135(10) 0.022(5) -0.036(6) -0.013(3) C27 0.036(5) 0.023(4) 0.122(10) -0.006(4) -0.034(6) -0.004(3) C28 0.052(6) 0.020(4) 0.188(15) -0.029(6) -0.054(8) 0.011(4) C29 0.071(10) 0.081(10) 0.25(2) -0.108(13) -0.086(13) 0.034(8) C30 0.084(9) 0.078(8) 0.114(11) -0.055(8) -0.037(8) 0.032(7) C31 0.074(8) 0.062(6) 0.077(8) -0.038(6) -0.009(6) 0.015(6) C32 0.039(5) 0.048(5) 0.067(6) -0.031(4) -0.013(4) 0.003(4) C33 0.059(7) 0.067(6) 0.071(7) -0.027(5) 0.004(5) -0.002(5) C34 0.045(6) 0.146(13) 0.064(7) -0.041(8) 0.003(5) 0.001(7) C35 0.054(6) 0.091(7) 0.039(5) -0.016(5) 0.004(4) -0.013(5) C36 0.071(8) 0.104(9) 0.046(6) 0.010(6) 0.002(5) -0.027(7) C37 0.044(6) 0.118(10) 0.064(7) 0.052(7) 0.000(5) -0.018(6) C38 0.036(5) 0.055(5) 0.057(5) 0.021(4) -0.002(4) -0.002(4) C39 0.037(5) 0.036(4) 0.073(6) 0.015(4) 0.008(4) -0.009(3) C40 0.037(4) 0.022(3) 0.085(7) -0.001(4) -0.005(4) -0.008(3) C41 0.035(4) 0.020(3) 0.057(5) -0.004(3) 0.003(4) 0.001(3) C42 0.024(4) 0.037(4) 0.044(4) 0.004(3) 0.001(3) -0.009(3) C43 0.028(4) 0.053(5) 0.049(5) -0.002(4) 0.001(3) -0.003(3) C44 0.023(4) 0.027(3) 0.053(5) 0.000(3) -0.010(3) 0.008(2) C45 0.024(3) 0.025(3) 0.039(4) 0.000(3) 0.003(3) 0.001(2) C46 0.022(3) 0.010(2) 0.037(4) 0.001(2) 0.002(3) 0.000(2) C47 0.029(4) 0.027(3) 0.049(5) 0.005(3) 0.003(3) 0.003(3) C48 0.074(7) 0.040(4) 0.072(6) 0.021(4) 0.039(6) 0.014(4) C49 0.078(8) 0.061(6) 0.054(6) 0.005(4) 0.020(5) 0.026(5) C50 0.043(5) 0.035(4) 0.088(7) -0.003(4) -0.001(5) 0.014(4) C51 0.035(4) 0.021(3) 0.058(5) -0.002(3) -0.011(4) 0.001(3) C52 0.019(3) 0.018(3) 0.056(5) 0.004(3) 0.001(3) -0.004(2) C53 0.024(3) 0.021(3) 0.058(5) 0.005(3) 0.001(3) -0.004(2) C54 0.043(5) 0.027(4) 0.059(5) 0.014(3) -0.003(4) -0.007(3) C55 0.044(5) 0.047(5) 0.066(6) 0.022(4) -0.004(4) -0.009(4) C56 0.048(5) 0.064(6) 0.051(5) 0.005(4) 0.001(4) 0.003(4) C57 0.026(4) 0.050(5) 0.051(5) -0.006(4) -0.011(4) -0.002(3) C58 0.046(5) 0.049(5) 0.052(5) -0.018(4) -0.019(4) 0.008(4) C59 0.081(9) 0.101(10) 0.090(9) -0.042(8) 0.001(7) -0.002(8) C60 0.088(12) 0.129(15) 0.129(15) -0.079(12) -0.011(11) 0.008(11) C61 0.135(16) 0.073(9) 0.138(16) -0.059(10) -0.063(13) 0.023(9) C62 0.110(10) 0.038(5) 0.095(9) -0.010(5) -0.063(8) -0.002(6) C63 0.052(7) 0.183(14) 0.039(6) -0.044(7) -0.008(5) 0.027(8) C64 0.037(6) 0.28(3) 0.061(8) -0.092(13) -0.018(6) 0.057(12) C65 0.056(9) 0.20(2) 0.18(2) -0.142(17) -0.049(10) 0.061(11) C66 0.059(7) 0.103(10) 0.086(9) -0.051(8) -0.006(6) 0.004(7) C67 0.092(12) 0.124(15) 0.141(15) -0.083(13) 0.034(11) -0.002(10) C68 0.091(12) 0.067(9) 0.26(3) -0.057(13) 0.048(16) -0.007(8) C69 0.034(6) 0.124(12) 0.126(13) -0.025(10) 0.002(7) 0.000(7) C70 0.043(6) 0.096(9) 0.100(10) 0.008(8) 0.015(6) 0.002(6) C71 0.031(5) 0.123(10) 0.057(6) 0.011(7) -0.001(4) 0.016(5) C72 0.029(4) 0.099(8) 0.036(5) -0.001(5) -0.002(4) 0.012(5) C73 0.031(5) 0.079(7) 0.082(7) -0.021(6) -0.003(5) 0.008(4) C74 0.033(5) 0.124(10) 0.057(6) -0.045(7) -0.008(4) 0.016(6) C75 0.041(6) 0.104(8) 0.029(4) -0.018(5) -0.008(4) 0.019(5) C76 0.069(8) 0.144(12) 0.038(6) 0.022(6) 0.000(5) 0.034(8) C77 0.044(6) 0.095(8) 0.054(6) -0.001(5) -0.007(5) -0.008(5) C78 0.064(8) 0.122(10) 0.029(5) -0.011(6) 0.001(5) 0.009(7) N1 0.018(3) 0.028(3) 0.072(5) 0.026(3) -0.008(3) -0.003(2) N2 0.018(3) 0.040(3) 0.052(4) 0.015(3) -0.004(3) -0.001(2) N3 0.045(4) 0.022(3) 0.067(5) -0.001(3) 0.005(4) -0.002(3) N4 0.027(3) 0.021(2) 0.038(3) 0.000(2) 0.003(3) 0.004(2) N5 0.056(5) 0.020(3) 0.074(5) -0.006(3) -0.021(4) 0.002(3) N6 0.022(3) 0.046(4) 0.090(6) 0.038(4) -0.018(4) -0.012(3) N7 0.015(3) 0.066(4) 0.048(4) 0.020(4) 0.000(3) -0.004(3) N8 0.013(3) 0.022(3) 0.066(4) 0.005(3) -0.001(3) 0.000(2) N9 0.022(3) 0.044(3) 0.049(4) -0.015(3) -0.004(3) 0.000(3) N10 0.066(5) 0.039(4) 0.051(5) 0.001(3) 0.012(4) 0.020(4) N11 0.026(3) 0.022(3) 0.101(6) 0.014(3) -0.012(4) 0.003(2) N12 0.014(3) 0.028(3) 0.044(3) 0.000(2) 0.002(2) 0.000(2) N13 0.024(3) 0.023(3) 0.060(4) 0.004(3) -0.004(3) -0.007(2) N14 0.044(4) 0.025(3) 0.067(5) 0.011(3) 0.014(4) 0.001(3) N15 0.055(5) 0.027(3) 0.073(5) -0.011(3) -0.031(4) -0.001(3) N16 0.019(3) 0.025(3) 0.043(3) 0.001(2) 0.000(3) -0.003(2) N17 0.042(5) 0.108(7) 0.035(4) -0.019(4) -0.011(3) 0.017(5) N18 0.029(4) 0.088(6) 0.052(5) -0.013(4) -0.010(3) 0.010(4) N19 0.051(6) 0.168(11) 0.048(5) -0.036(6) -0.019(4) 0.029(6) N20 0.052(6) 0.134(9) 0.052(5) -0.009(5) -0.007(4) 0.005(6) N21 0.026(3) 0.024(2) 0.042(3) 0.005(2) 0.005(3) -0.003(2) N22 0.101(8) 0.120(9) 0.041(5) -0.017(6) -0.012(5) 0.022(7) N23 0.103(10) 0.210(16) 0.071(7) 0.056(9) 0.013(7) 0.057(10) N24 0.023(3) 0.027(3) 0.057(4) 0.001(3) 0.001(3) 0.004(2) O1 0.041(3) 0.033(3) 0.041(3) 0.003(2) 0.003(2) -0.005(2) O2 0.032(3) 0.055(3) 0.047(3) 0.004(3) 0.004(3) -0.012(2) O3 0.024(3) 0.028(2) 0.061(4) -0.007(2) -0.002(2) 0.0012(19) O5 0.038(3) 0.050(4) 0.082(5) 0.009(3) -0.023(3) 0.005(3) O7 0.047(3) 0.031(3) 0.043(3) 0.000(2) -0.008(3) 0.002(2) O8 0.156(10) 0.079(5) 0.057(5) -0.002(4) 0.013(5) 0.047(6) O9 0.089(7) 0.198(12) 0.070(6) -0.035(7) -0.022(5) 0.026(8) O12 0.146(13) 0.223(15) 0.136(11) -0.046(11) 0.015(10) 0.030(12) O14 0.25(2) 0.166(15) 0.31(2) -0.093(16) 0.01(2) 0.020(14) O18 0.24(2) 0.32(2) 0.112(10) -0.021(13) -0.020(12) -0.091(18) _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 Pr1 O1 2.537(5) . ? Pr1 N21 2.554(6) 4_466 ? Pr1 O2 2.558(5) . ? Pr1 N4 2.567(5) . ? Pr1 N8 2.576(6) 4_566 ? Pr1 N7 2.607(7) . ? Pr1 O3 2.609(5) . ? Pr1 N5 2.651(7) . ? Pr1 N6 2.688(6) . ? Pr2 O4' 2.447(16) . ? Pr2 O5 2.518(7) . ? Pr2 O6 2.537(9) . ? Pr2 N11 2.573(6) . ? Pr2 N24 2.593(6) 4_556 ? Pr2 N16 2.608(6) 4_456 ? Pr2 N15 2.608(9) . ? Pr2 N14 2.630(7) . ? Pr2 N13 2.646(6) . ? Pr2 O4 2.728(12) . ? Pr2 O6' 2.736(13) . ? Ru1 C13 1.968(6) . ? Ru1 C16 2.004(8) . ? Ru1 C15 2.037(6) . ? Ru1 C14 2.046(7) . ? Ru1 N2 2.133(7) . ? Ru1 N1 2.141(5) . ? Ru2 C44 1.955(7) . ? Ru2 C47 1.991(8) . ? Ru2 C46 2.042(6) . ? Ru2 C45 2.075(7) . ? Ru2 N9 2.133(7) . ? Ru2 N12 2.141(6) . ? Ru3 C76 1.954(12) . ? Ru3 C77 1.969(12) . ? Ru3 C78 2.002(13) . ? Ru3 C75 2.040(10) . ? Ru3 N18 2.108(9) . ? Ru3 N17 2.120(9) . ? C1 N2 1.360(10) . ? C1 C2 1.382(13) . ? C1 H1 0.9300 . ? C2 C3 1.356(15) . ? C2 H2 0.9300 . ? C3 C4 1.454(17) . ? C3 H3 0.9300 . ? C4 C12 1.417(14) . ? C4 C5 1.453(15) . ? C5 C6 1.259(18) . ? C5 H5 0.9300 . ? C6 C7 1.523(19) . ? C6 H6 0.9300 . ? C7 C8 1.369(18) . ? C7 C11 1.432(11) . ? C8 C9 1.359(19) . ? C8 H8 0.9300 . ? C9 C10 1.403(12) . ? C9 H9 0.9300 . ? C10 N1 1.323(11) . ? C10 H10 0.9300 . ? C11 N1 1.361(12) . ? C11 C12 1.426(13) . ? C12 N2 1.368(10) . ? C13 N4 1.182(8) . ? C14 N8 1.141(9) . ? C15 N21 1.172(9) . ? C16 N3 1.166(10) . ? C17 N7 1.365(12) . ? C17 C18 1.383(14) . ? C17 H17 0.9300 . ? C18 C19 1.48(2) . ? C18 H18 0.9300 . ? C19 C20 1.42(3) . ? C19 H19 0.9300 . ? C20 C21 1.347(18) . ? C20 H20 0.9300 . ? C21 N7 1.376(11) . ? C21 C22 1.447(17) . ? C22 N6 1.359(15) . ? C22 C23 1.413(13) . ? C23 C24 1.33(2) . ? C23 H23 0.9300 . ? C24 C25 1.37(3) . ? C24 H24 0.9300 . ? C25 C26 1.463(13) . ? C25 H25 0.9300 . ? C26 N6 1.360(13) . ? C26 C27 1.447(17) . ? C27 N5 1.321(11) . ? C27 C28 1.433(14) . ? C28 C29 1.37(2) . ? C28 H28 0.9300 . ? C29 C30 1.38(2) . ? C29 H29 0.9300 . ? C30 C31 1.397(13) . ? C30 H30 0.9300 . ? C31 N5 1.325(14) . ? C31 H31 0.9300 . ? C32 N9 1.341(9) . ? C32 C33 1.360(15) . ? C32 H32 0.9300 . ? C33 C34 1.350(18) . ? C33 H33 0.9300 . ? C34 C35 1.468(17) . ? C34 H34 0.9300 . ? C35 C36 1.381(16) . ? C35 C43 1.414(13) . ? C36 C37 1.400(17) . ? C36 H36 0.9300 . ? C37 C38 1.438(14) . ? C37 H37 0.9300 . ? C38 C39 1.392(13) . ? C38 C42 1.438(11) . ? C39 C40 1.338(13) . ? C39 H39 0.9300 . ? C40 C41 1.428(10) . ? C40 H40 0.9300 . ? C41 N12 1.331(9) . ? C41 H41 0.9300 . ? C42 N12 1.383(10) . ? C42 C43 1.406(11) . ? C43 N9 1.363(11) . ? C44 N11 1.171(9) . ? C45 N24 1.145(9) . ? C46 N16 1.171(9) . ? C47 N10 1.161(10) . ? C48 N14 1.356(12) . ? C48 C49 1.391(13) . ? C48 H48 0.9300 . ? C49 C50 1.340(13) . ? C49 H49 0.9300 . ? C50 C51 1.395(13) . ? C50 H50 0.9300 . ? C51 C52 1.429(9) . ? C51 H51 0.9300 . ? C52 N14 1.370(9) . ? C52 C53 1.460(12) . ? C53 N13 1.351(9) . ? C53 C54 1.417(10) . ? C54 C55 1.336(13) . ? C54 H54 0.9300 . ? C55 C56 1.412(13) . ? C55 H55 0.9300 . ? C56 C57 1.406(13) . ? C56 H56 0.9300 . ? C57 N13 1.352(11) . ? C57 C58 1.514(11) . ? C58 N15 1.354(13) . ? C58 C59 1.373(15) . ? C59 C60 1.44(2) . ? C59 H59 0.9300 . ? C60 C61 1.27(2) . ? C60 H60 0.9300 . ? C61 C62 1.32(2) . ? C61 H61 0.9300 . ? C62 N15 1.358(11) . ? C62 H62 0.9300 . ? C63 N17 1.353(14) . ? C63 C64 1.50(2) . ? C63 H63 0.9300 . ? C64 C65 1.18(3) . ? C64 H64 0.9300 . ? C65 C66 1.50(3) . ? C65 H65 0.9300 . ? C66 C67 1.36(2) . ? C66 C74 1.404(16) . ? C67 C68 1.35(3) . ? C67 H67 0.9300 . ? C68 C69 1.51(2) . ? C68 H68 0.9300 . ? C69 C70 1.434(19) . ? C69 C73 1.501(19) . ? C70 C71 1.348(17) . ? C70 H70 0.9300 . ? C71 C72 1.374(15) . ? C71 H71 0.9300 . ? C72 N18 1.392(12) . ? C72 H72 0.9300 . ? C73 N18 1.369(13) . ? C73 C74 1.448(16) . ? C74 N17 1.333(16) . ? C75 N19 1.168(13) . ? C76 N23 1.202(17) . ? C77 N22 1.180(14) . ? C78 N20 1.208(15) . ? N8 Pr1 2.576(6) 4_466 ? N16 Pr2 2.608(6) 4_556 ? N21 Pr1 2.554(6) 4_566 ? N24 Pr2 2.593(6) 4_456 ? 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 O1 Pr1 N21 69.43(18) . 4_466 ? O1 Pr1 O2 71.41(18) . . ? N21 Pr1 O2 139.53(19) 4_466 . ? O1 Pr1 N4 75.35(18) . . ? N21 Pr1 N4 77.87(17) 4_466 . ? O2 Pr1 N4 82.87(19) . . ? O1 Pr1 N8 134.1(2) . 4_566 ? N21 Pr1 N8 137.12(18) 4_466 4_566 ? O2 Pr1 N8 79.7(2) . 4_566 ? N4 Pr1 N8 135.78(18) . 4_566 ? O1 Pr1 N7 136.83(19) . . ? N21 Pr1 N7 70.0(2) 4_466 . ? O2 Pr1 N7 141.9(2) . . ? N4 Pr1 N7 82.4(2) . . ? N8 Pr1 N7 86.9(2) 4_566 . ? O1 Pr1 O3 129.11(17) . . ? N21 Pr1 O3 133.22(17) 4_466 . ? O2 Pr1 O3 68.75(18) . . ? N4 Pr1 O3 69.54(17) . . ? N8 Pr1 O3 66.29(17) 4_566 . ? N7 Pr1 O3 73.2(2) . . ? O1 Pr1 N5 72.1(2) . . ? N21 Pr1 N5 91.9(2) 4_466 . ? O2 Pr1 N5 85.6(2) . . ? N4 Pr1 N5 147.5(2) . . ? N8 Pr1 N5 70.8(2) 4_566 . ? N7 Pr1 N5 123.3(2) . . ? O3 Pr1 N5 132.9(2) . . ? O1 Pr1 N6 114.1(2) . . ? N21 Pr1 N6 68.53(19) 4_466 . ? O2 Pr1 N6 139.7(2) . . ? N4 Pr1 N6 137.4(2) . . ? N8 Pr1 N6 68.77(19) 4_566 . ? N7 Pr1 N6 62.2(3) . . ? O3 Pr1 N6 116.8(2) . . ? N5 Pr1 N6 61.1(3) . . ? O4' Pr2 O5 70.9(4) . . ? O4' Pr2 O6 56.4(5) . . ? O5 Pr2 O6 109.5(3) . . ? O4' Pr2 N11 90.6(4) . . ? O5 Pr2 N11 71.5(2) . . ? O6 Pr2 N11 66.3(2) . . ? O4' Pr2 N24 143.6(4) . 4_556 ? O5 Pr2 N24 72.7(2) . 4_556 ? O6 Pr2 N24 141.5(2) . 4_556 ? N11 Pr2 N24 79.11(19) . 4_556 ? O4' Pr2 N16 73.4(4) . 4_456 ? O5 Pr2 N16 135.1(2) . 4_456 ? O6 Pr2 N16 70.2(2) . 4_456 ? N11 Pr2 N16 135.23(19) . 4_456 ? N24 Pr2 N16 136.28(19) 4_556 4_456 ? O4' Pr2 N15 137.5(4) . . ? O5 Pr2 N15 137.8(2) . . ? O6 Pr2 N15 81.7(3) . . ? N11 Pr2 N15 77.1(3) . . ? N24 Pr2 N15 74.3(2) 4_556 . ? N16 Pr2 N15 87.0(2) 4_456 . ? O4' Pr2 N14 87.8(4) . . ? O5 Pr2 N14 74.5(2) . . ? O6 Pr2 N14 137.1(3) . . ? N11 Pr2 N14 144.5(2) . . ? N24 Pr2 N14 81.3(2) 4_556 . ? N16 Pr2 N14 77.8(2) 4_456 . ? N15 Pr2 N14 125.1(2) . . ? O4' Pr2 N13 137.0(4) . . ? O5 Pr2 N13 123.0(2) . . ? O6 Pr2 N13 127.3(3) . . ? N11 Pr2 N13 131.8(2) . . ? N24 Pr2 N13 65.77(19) 4_556 . ? N16 Pr2 N13 70.52(18) 4_456 . ? N15 Pr2 N13 62.7(2) . . ? N14 Pr2 N13 62.5(2) . . ? O4' Pr2 O4 16.3(4) . . ? O5 Pr2 O4 69.1(3) . . ? O6 Pr2 O4 70.6(3) . . ? N11 Pr2 O4 104.8(3) . . ? N24 Pr2 O4 137.7(3) 4_556 . ? N16 Pr2 O4 69.0(3) 4_456 . ? N15 Pr2 O4 148.0(3) . . ? N14 Pr2 O4 71.7(3) . . ? N13 Pr2 O4 123.5(3) . . ? O4' Pr2 O6' 73.5(5) . . ? O5 Pr2 O6' 127.6(3) . . ? O6 Pr2 O6' 19.4(3) . . ? N11 Pr2 O6' 71.7(3) . . ? N24 Pr2 O6' 133.0(3) 4_556 . ? N16 Pr2 O6' 63.8(3) 4_456 . ? N15 Pr2 O6' 64.0(3) . . ? N14 Pr2 O6' 140.6(3) . . ? N13 Pr2 O6' 109.3(3) . . ? O4 Pr2 O6' 85.9(4) . . ? C13 Ru1 C16 88.7(3) . . ? C13 Ru1 C15 90.7(2) . . ? C16 Ru1 C15 89.0(3) . . ? C13 Ru1 C14 85.6(2) . . ? C16 Ru1 C14 88.1(3) . . ? C15 Ru1 C14 175.3(3) . . ? C13 Ru1 N2 94.4(3) . . ? C16 Ru1 N2 176.7(2) . . ? C15 Ru1 N2 92.0(3) . . ? C14 Ru1 N2 91.1(3) . . ? C13 Ru1 N1 172.5(3) . . ? C16 Ru1 N1 98.8(3) . . ? C15 Ru1 N1 90.2(2) . . ? C14 Ru1 N1 93.8(2) . . ? N2 Ru1 N1 78.2(3) . . ? C44 Ru2 C47 89.7(3) . . ? C44 Ru2 C46 85.3(3) . . ? C47 Ru2 C46 87.9(3) . . ? C44 Ru2 C45 88.3(3) . . ? C47 Ru2 C45 87.9(3) . . ? C46 Ru2 C45 172.4(3) . . ? C44 Ru2 N9 94.7(3) . . ? C47 Ru2 N9 175.5(3) . . ? C46 Ru2 N9 92.0(3) . . ? C45 Ru2 N9 92.6(3) . . ? C44 Ru2 N12 171.9(3) . . ? C47 Ru2 N12 97.9(3) . . ? C46 Ru2 N12 92.1(2) . . ? C45 Ru2 N12 94.7(2) . . ? N9 Ru2 N12 77.6(2) . . ? C76 Ru3 C77 93.3(5) . . ? C76 Ru3 C78 89.2(5) . . ? C77 Ru3 C78 90.4(4) . . ? C76 Ru3 C75 87.9(5) . . ? C77 Ru3 C75 88.9(4) . . ? C78 Ru3 C75 177.0(5) . . ? C76 Ru3 N18 171.6(4) . . ? C77 Ru3 N18 95.1(4) . . ? C78 Ru3 N18 90.2(4) . . ? C75 Ru3 N18 92.8(4) . . ? C76 Ru3 N17 93.8(5) . . ? C77 Ru3 N17 172.8(4) . . ? C78 Ru3 N17 89.3(4) . . ? C75 Ru3 N17 91.8(4) . . ? N18 Ru3 N17 77.8(3) . . ? N2 C1 C2 122.7(8) . . ? N2 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 120.5(10) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 119.6(10) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C12 C4 C5 117.1(12) . . ? C12 C4 C3 116.4(9) . . ? C5 C4 C3 126.5(11) . . ? C6 C5 C4 124.9(12) . . ? C6 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? C5 C6 C7 121.0(10) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C11 119.7(11) . . ? C8 C7 C6 124.9(10) . . ? C11 C7 C6 115.4(11) . . ? C9 C8 C7 118.6(9) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C8 C9 C10 120.1(11) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N1 C10 C9 122.8(11) . . ? N1 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N1 C11 C12 118.2(7) . . ? N1 C11 C7 120.6(9) . . ? C12 C11 C7 121.2(10) . . ? N2 C12 C4 122.6(9) . . ? N2 C12 C11 117.2(8) . . ? C4 C12 C11 120.2(8) . . ? N4 C13 Ru1 177.1(6) . . ? N8 C14 Ru1 172.9(6) . . ? N21 C15 Ru1 177.2(7) . . ? N3 C16 Ru1 176.8(6) . . ? N7 C17 C18 126.4(10) . . ? N7 C17 H17 116.8 . . ? C18 C17 H17 116.8 . . ? C17 C18 C19 113.6(14) . . ? C17 C18 H18 123.2 . . ? C19 C18 H18 123.2 . . ? C20 C19 C18 119.5(12) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 120.4(14) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 N7 122.0(13) . . ? C20 C21 C22 120.5(12) . . ? N7 C21 C22 117.5(9) . . ? N6 C22 C23 120.4(12) . . ? N6 C22 C21 118.2(8) . . ? C23 C22 C21 121.4(12) . . ? C24 C23 C22 121.4(14) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 119.2(11) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 120.8(14) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? N6 C26 C27 118.1(7) . . ? N6 C26 C25 117.5(13) . . ? C27 C26 C25 124.4(11) . . ? N5 C27 C28 121.0(12) . . ? N5 C27 C26 118.3(8) . . ? C28 C27 C26 120.7(10) . . ? C29 C28 C27 120.5(12) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 117.6(11) . . ? C28 C29 H29 121.2 . . ? C30 C29 H29 121.2 . . ? C29 C30 C31 118.3(16) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? N5 C31 C30 124.7(13) . . ? N5 C31 H31 117.7 . . ? C30 C31 H31 117.7 . . ? N9 C32 C33 123.9(10) . . ? N9 C32 H32 118.1 . . ? C33 C32 H32 118.1 . . ? C34 C33 C32 118.9(10) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 121.6(10) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C36 C35 C43 121.7(10) . . ? C36 C35 C34 124.6(10) . . ? C43 C35 C34 113.7(11) . . ? C35 C36 C37 119.6(10) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C36 C37 C38 121.9(10) . . ? C36 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C39 C38 C37 124.2(9) . . ? C39 C38 C42 119.5(8) . . ? C37 C38 C42 116.3(9) . . ? C40 C39 C38 118.5(7) . . ? C40 C39 H39 120.7 . . ? C38 C39 H39 120.7 . . ? C39 C40 C41 120.8(8) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? N12 C41 C40 122.8(8) . . ? N12 C41 H41 118.6 . . ? C40 C41 H41 118.6 . . ? N12 C42 C43 117.3(7) . . ? N12 C42 C38 121.0(7) . . ? C43 C42 C38 121.7(8) . . ? N9 C43 C42 117.9(7) . . ? N9 C43 C35 123.3(8) . . ? C42 C43 C35 118.8(8) . . ? N11 C44 Ru2 178.8(8) . . ? N24 C45 Ru2 174.3(6) . . ? N16 C46 Ru2 171.0(6) . . ? N10 C47 Ru2 176.5(7) . . ? N14 C48 C49 123.2(8) . . ? N14 C48 H48 118.4 . . ? C49 C48 H48 118.4 . . ? C50 C49 C48 120.0(9) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 118.8(8) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C50 C51 C52 120.6(7) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? N14 C52 C51 119.1(7) . . ? N14 C52 C53 117.2(6) . . ? C51 C52 C53 123.8(6) . . ? N13 C53 C54 120.6(8) . . ? N13 C53 C52 118.3(6) . . ? C54 C53 C52 121.1(7) . . ? C55 C54 C53 120.9(8) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C54 C55 C56 119.5(8) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C57 C56 C55 117.6(9) . . ? C57 C56 H56 121.2 . . ? C55 C56 H56 121.2 . . ? N13 C57 C56 122.6(8) . . ? N13 C57 C58 116.9(8) . . ? C56 C57 C58 120.5(8) . . ? N15 C58 C59 122.0(10) . . ? N15 C58 C57 116.5(8) . . ? C59 C58 C57 121.5(11) . . ? C58 C59 C60 115.9(15) . . ? C58 C59 H59 122.0 . . ? C60 C59 H59 122.0 . . ? C61 C60 C59 121.8(16) . . ? C61 C60 H60 119.1 . . ? C59 C60 H60 119.1 . . ? C60 C61 C62 118.6(14) . . ? C60 C61 H61 120.7 . . ? C62 C61 H61 120.7 . . ? C61 C62 N15 125.7(14) . . ? C61 C62 H62 117.2 . . ? N15 C62 H62 117.2 . . ? N17 C63 C64 116.7(15) . . ? N17 C63 H63 121.6 . . ? C64 C63 H63 121.6 . . ? C65 C64 C63 125.0(16) . . ? C65 C64 H64 117.5 . . ? C63 C64 H64 117.5 . . ? C64 C65 C66 120.6(14) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C67 C66 C74 123.9(14) . . ? C67 C66 C65 123.4(14) . . ? C74 C66 C65 112.6(15) . . ? C68 C67 C66 122.8(14) . . ? C68 C67 H67 118.6 . . ? C66 C67 H67 118.6 . . ? C67 C68 C69 121.2(17) . . ? C67 C68 H68 119.4 . . ? C69 C68 H68 119.4 . . ? C70 C69 C73 117.6(13) . . ? C70 C69 C68 129.3(17) . . ? C73 C69 C68 113.1(15) . . ? C71 C70 C69 118.4(13) . . ? C71 C70 H70 120.8 . . ? C69 C70 H70 120.8 . . ? C70 C71 C72 121.8(11) . . ? C70 C71 H71 119.1 . . ? C72 C71 H71 119.1 . . ? C71 C72 N18 125.0(10) . . ? C71 C72 H72 117.5 . . ? N18 C72 H72 117.5 . . ? N18 C73 C74 115.8(11) . . ? N18 C73 C69 121.5(11) . . ? C74 C73 C69 122.7(11) . . ? N17 C74 C66 126.8(11) . . ? N17 C74 C73 117.2(9) . . ? C66 C74 C73 116.0(13) . . ? N19 C75 Ru3 175.6(12) . . ? N23 C76 Ru3 177.9(13) . . ? N22 C77 Ru3 175.6(11) . . ? N20 C78 Ru3 177.2(11) . . ? C10 N1 C11 118.3(7) . . ? C10 N1 Ru1 128.8(7) . . ? C11 N1 Ru1 112.9(5) . . ? C1 N2 C12 118.2(7) . . ? C1 N2 Ru1 128.3(5) . . ? C12 N2 Ru1 113.4(6) . . ? C13 N4 Pr1 140.2(5) . . ? C27 N5 C31 117.9(9) . . ? C27 N5 Pr1 122.5(7) . . ? C31 N5 Pr1 119.6(6) . . ? C22 N6 C26 120.7(8) . . ? C22 N6 Pr1 119.3(6) . . ? C26 N6 Pr1 119.8(7) . . ? C17 N7 C21 118.0(8) . . ? C17 N7 Pr1 119.7(5) . . ? C21 N7 Pr1 121.7(7) . . ? C14 N8 Pr1 145.2(5) . 4_466 ? C32 N9 C43 118.4(8) . . ? C32 N9 Ru2 127.9(7) . . ? C43 N9 Ru2 113.7(5) . . ? C44 N11 Pr2 150.1(6) . . ? C41 N12 C42 117.3(6) . . ? C41 N12 Ru2 129.6(5) . . ? C42 N12 Ru2 113.0(4) . . ? C53 N13 C57 118.7(7) . . ? C53 N13 Pr2 120.3(5) . . ? C57 N13 Pr2 120.7(5) . . ? C48 N14 C52 118.2(7) . . ? C48 N14 Pr2 120.8(5) . . ? C52 N14 Pr2 120.1(5) . . ? C58 N15 C62 115.5(10) . . ? C58 N15 Pr2 121.8(5) . . ? C62 N15 Pr2 121.2(8) . . ? C46 N16 Pr2 145.8(5) . 4_556 ? C74 N17 C63 117.9(11) . . ? C74 N17 Ru3 114.7(6) . . ? C63 N17 Ru3 127.3(10) . . ? C73 N18 C72 115.7(10) . . ? C73 N18 Ru3 114.4(7) . . ? C72 N18 Ru3 129.8(7) . . ? C15 N21 Pr1 173.5(6) . 4_566 ? C45 N24 Pr2 167.3(6) . 4_456 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.906 _refine_diff_density_min -1.859 _refine_diff_density_rms 0.216 #===END data_imw521 _database_code_depnum_ccdc_archive 'CCDC 605807' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H60 K N16 O14 Ru2 Yb' _chemical_formula_weight 1595.48 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 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 14.2730(7) _cell_length_b 27.8052(14) _cell_length_c 17.0891(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.957(2) _cell_angle_gamma 90.00 _cell_volume 6634.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9715 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 23.21 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3188 _exptl_absorpt_coefficient_mu 1.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5696 _exptl_absorpt_correction_T_max 0.8903 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 105540 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.52 _reflns_number_total 14163 _reflns_number_gt 10279 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0900P)^2^+35.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14163 _refine_ls_number_parameters 813 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1726 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.022 _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 Yb1 Yb 0.231690(19) 0.480391(11) 0.854320(17) 0.02176(11) Uani 1 1 d . . . Ru1 Ru 0.43675(4) 0.61994(2) 1.03994(3) 0.02418(15) Uani 1 1 d . . . Ru2 Ru 0.07409(5) 0.63503(2) 0.68319(4) 0.03531(17) Uani 1 1 d . . . K1 K 0.60505(16) 0.55433(8) 0.50964(12) 0.0346(6) Uani 0.769(4) 1 d PU . 1 O20 O 0.4889(13) 0.5200(6) 0.5314(10) 0.085(5) Uiso 0.50 1 d P . 1 O21 O 0.6182(7) 0.4957(4) 0.5783(6) 0.037(2) Uiso 0.50 1 d P A 1 K1' K 0.5900(5) 0.5186(3) 0.5243(4) 0.0354(14) Uani 0.231(4) 1 d PU . 2 N1 N 0.4967(4) 0.6816(2) 1.1036(4) 0.0364(15) Uani 1 1 d . . . N2 N 0.3284(4) 0.6721(2) 1.0039(4) 0.0279(13) Uani 1 1 d . . . N3 N 0.3159(4) 0.5361(2) 0.9450(3) 0.0268(13) Uani 1 1 d . . . N4 N 0.3696(6) 0.5886(4) 1.1985(5) 0.065(2) Uani 1 1 d . . . N5 N 0.1871(5) 0.6855(2) 0.7168(4) 0.0381(16) Uani 1 1 d . . . N6 N 0.0233(6) 0.6941(3) 0.6072(4) 0.054(2) Uani 1 1 d . . . N7 N -0.1085(7) 0.5711(5) 0.6244(6) 0.097(4) Uani 1 1 d . . . N8 N -0.0345(5) 0.6848(3) 0.8077(5) 0.0458(18) Uani 1 1 d . . . N9 N 0.1794(6) 0.5943(3) 0.5512(4) 0.0506(19) Uani 1 1 d . . . N10 N 0.1671(4) 0.5537(2) 0.8013(3) 0.0251(13) Uani 1 1 d . . . N11 N 0.1928(4) 0.3918(2) 0.8366(3) 0.0275(13) Uani 1 1 d . . . N12 N 0.1606(4) 0.4550(2) 0.7149(3) 0.0269(13) Uani 1 1 d . . . N13 N 0.1932(4) 0.4539(2) 0.9828(4) 0.0303(14) Uani 1 1 d . . . N14 N 0.0556(4) 0.4744(2) 0.8516(3) 0.0248(13) Uani 1 1 d . . . N23 N 0.5217(6) 0.6433(3) 0.8860(5) 0.062(2) Uani 1 1 d . . . N24 N 0.6259(4) 0.5614(2) 1.0950(4) 0.0311(14) Uani 1 1 d . . . C1 C 0.5782(6) 0.6846(3) 1.1575(6) 0.053(3) Uani 1 1 d . . . H1 H 0.6166 0.6574 1.1680 0.063 Uiso 1 1 calc R . . C2 C 0.6086(7) 0.7273(4) 1.1994(7) 0.066(3) Uani 1 1 d . . . H2 H 0.6660 0.7281 1.2369 0.079 Uiso 1 1 calc R . . C3 C 0.5538(7) 0.7668(4) 1.1848(7) 0.070(3) Uani 1 1 d . . . H3 H 0.5738 0.7952 1.2119 0.084 Uiso 1 1 calc R . . C4 C 0.4673(6) 0.7657(3) 1.1293(6) 0.052(2) Uani 1 1 d . . . C5 C 0.4058(8) 0.8060(3) 1.1078(7) 0.065(3) Uani 1 1 d . . . H5 H 0.4237 0.8357 1.1312 0.079 Uiso 1 1 calc R . . C6 C 0.3226(8) 0.8022(3) 1.0546(7) 0.058(3) Uani 1 1 d . . . H6 H 0.2840 0.8293 1.0428 0.069 Uiso 1 1 calc R . . C7 C 0.2912(6) 0.7574(3) 1.0152(6) 0.047(2) Uani 1 1 d . . . C8 C 0.2055(6) 0.7504(3) 0.9601(6) 0.049(2) Uani 1 1 d . . . H8 H 0.1646 0.7763 0.9443 0.059 Uiso 1 1 calc R . . C9 C 0.1817(6) 0.7059(3) 0.9295(5) 0.042(2) Uani 1 1 d . . . H9 H 0.1237 0.7011 0.8938 0.050 Uiso 1 1 calc R . . C10 C 0.2445(5) 0.6672(3) 0.9515(4) 0.0330(17) Uani 1 1 d . . . H10 H 0.2276 0.6371 0.9292 0.040 Uiso 1 1 calc R . . C11 C 0.3518(5) 0.7165(3) 1.0354(5) 0.0350(18) Uani 1 1 d . . . C12 C 0.4405(5) 0.7216(3) 1.0900(5) 0.0371(19) Uani 1 1 d . . . C13 C 0.3635(5) 0.5661(3) 0.9802(4) 0.0249(15) Uani 1 1 d . . . C14 C 0.3903(5) 0.5999(3) 1.1403(5) 0.0370(19) Uani 1 1 d . . . C15 C 0.5531(5) 0.5809(3) 1.0742(4) 0.0270(15) Uani 1 1 d . . . C16 C 0.4897(5) 0.6365(3) 0.9409(5) 0.0357(18) Uani 1 1 d . . . C17 C 0.2694(6) 0.6805(3) 0.7662(5) 0.041(2) Uani 1 1 d . . . H17 H 0.2847 0.6502 0.7881 0.049 Uiso 1 1 calc R . . C18 C 0.3360(8) 0.7171(3) 0.7886(6) 0.058(3) Uani 1 1 d . . . H18 H 0.3939 0.7116 0.8239 0.069 Uiso 1 1 calc R . . C19 C 0.3123(9) 0.7626(4) 0.7558(8) 0.071(3) Uani 1 1 d . . . H19 H 0.3536 0.7884 0.7706 0.085 Uiso 1 1 calc R . . C20 C 0.2291(9) 0.7689(3) 0.7026(7) 0.065(3) Uani 1 1 d . . . C21 C 0.2002(13) 0.8144(4) 0.6641(10) 0.092(5) Uani 1 1 d . . . H21 H 0.2379 0.8415 0.6794 0.110 Uiso 1 1 calc R . . C22 C 0.1224(14) 0.8188(4) 0.6081(10) 0.104(6) Uani 1 1 d . . . H22 H 0.1082 0.8486 0.5837 0.124 Uiso 1 1 calc R . . C23 C 0.0568(10) 0.7781(5) 0.5824(7) 0.081(4) Uani 1 1 d . . . C24 C -0.0227(13) 0.7789(6) 0.5206(9) 0.101(6) Uani 1 1 d . . . H24 H -0.0387 0.8068 0.4908 0.121 Uiso 1 1 calc R . . C25 C -0.0772(11) 0.7392(6) 0.5036(7) 0.095(5) Uani 1 1 d . . . H25 H -0.1303 0.7397 0.4616 0.114 Uiso 1 1 calc R . . C26 C -0.0541(8) 0.6965(5) 0.5495(6) 0.073(4) Uani 1 1 d . . . H26 H -0.0941 0.6698 0.5387 0.088 Uiso 1 1 calc R . . C27 C 0.0793(8) 0.7336(4) 0.6234(6) 0.056(3) Uani 1 1 d . . . C28 C 0.1654(7) 0.7295(3) 0.6833(6) 0.052(2) Uani 1 1 d . . . C29 C 0.1322(5) 0.5846(3) 0.7584(4) 0.0270(16) Uani 1 1 d . . . C30 C 0.0049(6) 0.6652(3) 0.7640(5) 0.0388(19) Uani 1 1 d . . . C31 C 0.1407(6) 0.6082(3) 0.5999(5) 0.0393(19) Uani 1 1 d . . . C32 C -0.0391(7) 0.5930(4) 0.6460(5) 0.059(3) Uani 1 1 d . . . C33 C 0.2186(5) 0.3584(3) 0.8923(5) 0.0320(17) Uani 1 1 d . . . H33 H 0.2578 0.3676 0.9405 0.038 Uiso 1 1 calc R . . C34 C 0.1907(6) 0.3104(3) 0.8833(6) 0.045(2) Uani 1 1 d . . . H34 H 0.2141 0.2878 0.9227 0.054 Uiso 1 1 calc R . . C35 C 0.1274(6) 0.2971(3) 0.8144(5) 0.043(2) Uani 1 1 d . . . H35 H 0.1048 0.2657 0.8079 0.052 Uiso 1 1 calc R . . C36 C 0.0980(6) 0.3306(3) 0.7550(5) 0.0366(18) Uani 1 1 d . . . C37 C 0.0328(7) 0.3193(3) 0.6801(6) 0.052(2) Uani 1 1 d . . . H37 H 0.0041 0.2892 0.6730 0.063 Uiso 1 1 calc R . . C38 C 0.0134(7) 0.3517(3) 0.6213(6) 0.055(3) Uani 1 1 d . . . H38 H -0.0294 0.3437 0.5743 0.066 Uiso 1 1 calc R . . C39 C 0.0575(6) 0.3994(3) 0.6285(5) 0.043(2) Uani 1 1 d . . . C40 C 0.0474(6) 0.4315(3) 0.5657(5) 0.046(2) Uani 1 1 d . . . H40 H 0.0086 0.4240 0.5164 0.055 Uiso 1 1 calc R . . C41 C 0.0954(7) 0.4744(3) 0.5769(5) 0.046(2) Uani 1 1 d . . . H41 H 0.0917 0.4959 0.5347 0.055 Uiso 1 1 calc R . . C42 C 0.1500(6) 0.4855(3) 0.6524(4) 0.0324(17) Uani 1 1 d . . . H42 H 0.1804 0.5152 0.6598 0.039 Uiso 1 1 calc R . . C43 C 0.1160(5) 0.4120(3) 0.7025(4) 0.0320(17) Uani 1 1 d . . . C44 C 0.1352(5) 0.3770(3) 0.7669(4) 0.0269(15) Uani 1 1 d . . . C45 C 0.2603(6) 0.4438(3) 1.0470(4) 0.0351(18) Uani 1 1 d . . . H45 H 0.3237 0.4506 1.0456 0.042 Uiso 1 1 calc R . . C46 C 0.2405(6) 0.4233(3) 1.1167(5) 0.0387(19) Uani 1 1 d . . . H46 H 0.2897 0.4164 1.1601 0.046 Uiso 1 1 calc R . . C47 C 0.1482(6) 0.4139(3) 1.1196(5) 0.0396(19) Uani 1 1 d . . . H47 H 0.1340 0.4001 1.1654 0.048 Uiso 1 1 calc R . . C48 C 0.0738(6) 0.4246(3) 1.0543(5) 0.0315(17) Uani 1 1 d . . . C49 C -0.0262(6) 0.4187(3) 1.0545(5) 0.0364(19) Uani 1 1 d . . . H49 H -0.0442 0.4057 1.0993 0.044 Uiso 1 1 calc R . . C50 C -0.0940(6) 0.4317(3) 0.9913(5) 0.0365(18) Uani 1 1 d . . . H50 H -0.1582 0.4286 0.9939 0.044 Uiso 1 1 calc R . . C51 C -0.0704(5) 0.4495(2) 0.9220(5) 0.0306(17) Uani 1 1 d . . . C52 C -0.1398(5) 0.4617(3) 0.8530(5) 0.0373(19) Uani 1 1 d . . . H52 H -0.2045 0.4569 0.8520 0.045 Uiso 1 1 calc R . . C53 C -0.1112(5) 0.4805(3) 0.7876(5) 0.039(2) Uani 1 1 d . . . H53 H -0.1562 0.4892 0.7423 0.047 Uiso 1 1 calc R . . C54 C -0.0121(5) 0.4865(3) 0.7901(5) 0.0297(16) Uani 1 1 d . . . H54 H 0.0063 0.4999 0.7457 0.036 Uiso 1 1 calc R . . C55 C 0.0276(5) 0.4564(2) 0.9177(4) 0.0261(15) Uani 1 1 d . . . C56 C 0.0999(5) 0.4446(2) 0.9860(4) 0.0251(15) Uani 1 1 d . . . O1 O 0.3433(3) 0.5025(2) 0.7788(3) 0.0380(13) Uani 1 1 d . . . O2 O 0.7787(7) 0.7104(4) 0.8044(6) 0.062(2) Uiso 0.769(4) 1 d PU . 1 O2' O 0.762(2) 0.6910(12) 0.7742(19) 0.057(4) Uiso 0.231(4) 1 d PU . 2 O3 O 0.3530(7) 0.5625(4) 0.6579(6) 0.105(3) Uani 1 1 d . . . H3A H 0.4164 0.5645 0.6918 0.126 Uiso 1 1 calc R . . H3B H 0.3033 0.5824 0.6722 0.126 Uiso 1 1 calc R . . O4 O 0.5235(7) 0.5995(4) 0.7371(6) 0.115(3) Uani 1 1 d . . . H4A H 0.5872 0.5983 0.7707 0.139 Uiso 1 1 calc R . . H4B H 0.4785 0.6222 0.7518 0.139 Uiso 1 1 calc R . . O5 O 0.4798(5) 0.4779(3) 0.1237(5) 0.079(2) Uani 1 1 d . . . H5A H 0.5459 0.4787 0.1527 0.095 Uiso 1 1 calc R . . H5B H 0.4415 0.5050 0.1346 0.095 Uiso 1 1 calc R . . O6 O 0.3126(6) 0.2927(4) 0.0747(5) 0.099(3) Uani 1 1 d . . . H6A H 0.3778 0.2922 0.1055 0.119 Uiso 1 1 calc R . . H6B H 0.2753 0.3196 0.0878 0.119 Uiso 1 1 calc R . . O7 O 0.3908(13) 0.4967(5) 0.2677(11) 0.212(8) Uani 1 1 d . . . H7A H 0.4558 0.4990 0.2988 0.255 Uiso 1 1 calc R . . H7B H 0.3465 0.5206 0.2798 0.255 Uiso 1 1 calc R . . O8 O 0.7629(14) 0.6711(8) 0.6560(12) 0.106(5) Uiso 0.50 1 d PU B 1 O9 O 0.6470(17) 0.3772(8) 0.6466(14) 0.122(5) Uiso 0.50 1 d PU C 1 O8' O 0.7120(18) 0.6358(9) 0.6760(14) 0.129(6) Uiso 0.50 1 d PU . 2 O9' O 0.7611(16) 0.3858(9) 0.6449(13) 0.123(5) Uiso 0.50 1 d PU D 2 O10 O 0.400(2) 0.2134(10) 0.0684(17) 0.153(7) Uiso 0.50 1 d PU E 1 O10' O 0.325(2) 0.2043(9) -0.0042(16) 0.146(7) Uiso 0.50 1 d PU F 2 O11 O 0.7729(17) 0.4828(8) 0.5630(14) 0.123(6) Uiso 0.50 1 d PU G 1 O12 O 0.5840(18) 0.5773(9) 0.2902(15) 0.127(6) Uiso 0.50 1 d PU H 1 O11' O 0.7303(15) 0.5210(7) 0.5913(12) 0.099(5) Uiso 0.50 1 d PU I 2 O12' O 0.6467(19) 0.5999(9) 0.3171(15) 0.133(6) Uiso 0.50 1 d PU J 2 O22 O 0.6241(15) 0.6020(8) 0.6240(13) 0.114(7) Uiso 0.50 1 d P . . O23 O 0.7368(15) 0.6024(8) 0.4971(12) 0.109(6) Uiso 0.50 1 d P . . 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 Yb1 0.01996(15) 0.02170(19) 0.02225(16) -0.00153(12) 0.00121(11) 0.00036(11) Ru1 0.0179(3) 0.0234(3) 0.0303(3) -0.0039(2) 0.0029(2) -0.0008(2) Ru2 0.0386(3) 0.0369(4) 0.0303(3) 0.0142(3) 0.0070(3) 0.0066(3) K1 0.0412(12) 0.0297(14) 0.0278(11) -0.0120(10) -0.0043(9) 0.0038(9) K1' 0.031(2) 0.046(3) 0.029(2) 0.015(2) 0.005(2) -0.014(2) N1 0.024(3) 0.036(4) 0.049(4) -0.016(3) 0.008(3) -0.003(3) N2 0.021(3) 0.027(4) 0.037(3) 0.004(3) 0.010(2) -0.001(2) N3 0.023(3) 0.025(3) 0.030(3) -0.002(3) 0.001(2) 0.000(3) N4 0.045(4) 0.114(8) 0.036(4) 0.014(5) 0.010(4) -0.002(5) N5 0.052(4) 0.024(4) 0.045(4) 0.013(3) 0.025(3) 0.007(3) N6 0.064(5) 0.069(6) 0.035(4) 0.030(4) 0.021(4) 0.033(4) N7 0.065(6) 0.148(11) 0.066(6) 0.030(7) -0.012(5) -0.043(7) N8 0.043(4) 0.044(4) 0.053(4) 0.020(4) 0.016(4) 0.012(3) N9 0.066(5) 0.046(5) 0.040(4) 0.003(4) 0.010(4) -0.017(4) N10 0.026(3) 0.022(3) 0.026(3) 0.003(3) 0.002(2) -0.001(2) N11 0.026(3) 0.025(3) 0.031(3) -0.004(3) 0.006(2) 0.000(2) N12 0.031(3) 0.026(3) 0.023(3) -0.002(3) 0.004(2) 0.001(2) N13 0.035(3) 0.025(3) 0.031(3) -0.002(3) 0.006(3) 0.000(3) N14 0.025(3) 0.021(3) 0.028(3) -0.006(2) 0.005(2) 0.002(2) N23 0.047(4) 0.080(6) 0.066(6) 0.017(5) 0.027(4) 0.012(4) N24 0.028(3) 0.029(4) 0.032(3) -0.003(3) -0.001(3) 0.003(3) C1 0.028(4) 0.051(6) 0.077(7) -0.031(5) 0.006(4) -0.005(4) C2 0.037(5) 0.061(7) 0.096(8) -0.045(6) 0.006(5) -0.009(5) C3 0.042(5) 0.047(6) 0.121(10) -0.051(6) 0.019(6) -0.017(5) C4 0.042(5) 0.033(5) 0.084(7) -0.023(5) 0.022(5) -0.006(4) C5 0.063(6) 0.031(5) 0.110(9) -0.032(6) 0.033(6) -0.005(5) C6 0.070(7) 0.033(5) 0.082(7) -0.002(5) 0.043(6) 0.014(5) C7 0.043(5) 0.032(5) 0.072(6) -0.001(4) 0.029(5) 0.004(4) C8 0.049(5) 0.047(6) 0.057(6) 0.016(5) 0.024(4) 0.024(4) C9 0.032(4) 0.052(6) 0.044(5) 0.010(4) 0.011(4) 0.013(4) C10 0.030(4) 0.037(5) 0.033(4) 0.006(3) 0.008(3) 0.004(3) C11 0.031(4) 0.026(4) 0.053(5) -0.005(4) 0.020(4) 0.002(3) C12 0.029(4) 0.031(5) 0.055(5) -0.008(4) 0.017(4) -0.001(3) C13 0.024(3) 0.021(4) 0.029(4) 0.002(3) 0.003(3) 0.004(3) C14 0.025(4) 0.057(6) 0.027(4) -0.004(4) 0.000(3) -0.001(3) C15 0.026(4) 0.024(4) 0.029(4) -0.004(3) 0.001(3) -0.005(3) C16 0.022(3) 0.042(5) 0.045(5) 0.003(4) 0.011(3) 0.002(3) C17 0.046(5) 0.032(5) 0.049(5) 0.004(4) 0.020(4) 0.003(4) C18 0.066(6) 0.045(6) 0.071(7) -0.005(5) 0.031(5) -0.012(5) C19 0.080(8) 0.050(7) 0.098(9) -0.001(6) 0.051(7) -0.010(6) C20 0.104(9) 0.031(6) 0.083(8) 0.010(5) 0.071(7) 0.006(6) C21 0.157(14) 0.031(6) 0.120(12) 0.032(7) 0.103(11) 0.019(8) C22 0.195(18) 0.035(7) 0.117(12) 0.050(8) 0.117(13) 0.048(10) C23 0.117(10) 0.073(9) 0.074(8) 0.053(7) 0.071(8) 0.060(8) C24 0.156(15) 0.088(10) 0.082(10) 0.060(9) 0.082(11) 0.086(11) C25 0.117(11) 0.130(13) 0.042(6) 0.043(8) 0.028(7) 0.084(10) C26 0.084(8) 0.092(9) 0.046(6) 0.033(6) 0.020(5) 0.049(7) C27 0.079(7) 0.047(6) 0.058(6) 0.027(5) 0.048(6) 0.025(5) C28 0.069(6) 0.033(5) 0.064(6) 0.014(5) 0.042(5) 0.012(4) C29 0.023(3) 0.035(4) 0.024(3) -0.006(3) 0.008(3) -0.003(3) C30 0.042(4) 0.036(5) 0.040(5) 0.023(4) 0.013(4) 0.009(4) C31 0.050(5) 0.041(5) 0.026(4) 0.009(4) 0.009(4) -0.007(4) C32 0.051(6) 0.089(8) 0.036(5) 0.015(5) 0.004(4) -0.005(5) C33 0.037(4) 0.023(4) 0.035(4) 0.004(3) 0.006(3) 0.002(3) C34 0.050(5) 0.037(5) 0.054(5) 0.007(4) 0.022(4) 0.003(4) C35 0.052(5) 0.023(4) 0.060(6) -0.012(4) 0.022(4) -0.007(4) C36 0.044(4) 0.026(4) 0.040(4) -0.007(4) 0.009(4) -0.005(3) C37 0.065(6) 0.032(5) 0.056(6) -0.020(5) 0.005(5) -0.009(4) C38 0.061(6) 0.044(6) 0.052(6) -0.026(5) -0.008(5) -0.014(5) C39 0.046(5) 0.036(5) 0.042(5) -0.010(4) -0.001(4) -0.002(4) C40 0.054(5) 0.048(6) 0.029(4) -0.011(4) -0.007(4) 0.005(4) C41 0.062(6) 0.047(6) 0.024(4) -0.003(4) -0.004(4) 0.004(4) C42 0.043(4) 0.026(4) 0.027(4) -0.001(3) 0.002(3) 0.005(3) C43 0.033(4) 0.029(4) 0.033(4) -0.007(3) 0.004(3) -0.001(3) C44 0.028(3) 0.023(4) 0.030(4) -0.006(3) 0.006(3) 0.000(3) C45 0.036(4) 0.036(5) 0.032(4) 0.001(3) 0.006(3) -0.001(3) C46 0.052(5) 0.030(5) 0.030(4) 0.004(3) 0.000(4) 0.002(4) C47 0.060(5) 0.029(5) 0.033(4) 0.003(3) 0.016(4) -0.001(4) C48 0.047(4) 0.016(4) 0.036(4) -0.004(3) 0.018(3) -0.001(3) C49 0.051(5) 0.018(4) 0.049(5) -0.010(4) 0.031(4) -0.006(3) C50 0.039(4) 0.022(4) 0.054(5) -0.004(4) 0.023(4) -0.005(3) C51 0.033(4) 0.014(4) 0.050(5) -0.009(3) 0.019(3) -0.003(3) C52 0.026(4) 0.028(4) 0.060(5) -0.010(4) 0.014(4) -0.001(3) C53 0.021(3) 0.043(5) 0.051(5) -0.012(4) 0.000(3) 0.001(3) C54 0.030(4) 0.025(4) 0.033(4) -0.003(3) 0.004(3) -0.002(3) C55 0.030(4) 0.011(4) 0.040(4) -0.007(3) 0.015(3) -0.001(3) C56 0.030(3) 0.017(4) 0.031(4) -0.008(3) 0.015(3) -0.004(3) O1 0.025(3) 0.054(4) 0.037(3) -0.001(3) 0.011(2) -0.004(2) O3 0.086(6) 0.111(8) 0.110(7) 0.039(6) 0.001(5) -0.015(5) O4 0.110(8) 0.124(8) 0.094(7) -0.017(6) -0.022(6) 0.020(6) O5 0.049(4) 0.077(6) 0.105(6) 0.004(4) 0.001(4) -0.007(4) O6 0.062(5) 0.139(8) 0.091(6) -0.006(6) 0.001(4) -0.023(5) O7 0.246(19) 0.123(11) 0.32(2) -0.029(13) 0.168(18) 0.026(12) _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 Yb1 O1 2.330(5) . ? Yb1 N3 2.339(6) . ? Yb1 N10 2.340(6) . ? Yb1 N24 2.345(6) 3_667 ? Yb1 N13 2.482(6) . ? Yb1 N12 2.490(6) . ? Yb1 N14 2.510(6) . ? Yb1 N11 2.529(6) . ? Ru1 C15 1.969(7) . ? Ru1 C13 1.984(7) . ? Ru1 C14 2.040(8) . ? Ru1 C16 2.043(8) . ? Ru1 N1 2.115(6) . ? Ru1 N2 2.117(6) . ? Ru2 C29 1.965(8) . ? Ru2 C32 1.988(11) . ? Ru2 C31 2.012(9) . ? Ru2 C30 2.037(9) . ? Ru2 N5 2.125(7) . ? Ru2 N6 2.125(7) . ? K1 O21 1.995(11) . ? K1 O20 2.014(18) . ? K1 O22 2.33(2) . ? K1 O23 2.35(2) . ? K1 O20 2.484(17) 3_666 ? K1 O11 3.10(2) . ? K1 K1 4.221(5) 3_666 ? O20 O20 1.62(3) 3_666 ? O20 K1 2.484(17) 3_666 ? K1' O11' 2.09(2) . ? K1' K1' 2.733(14) 3_666 ? K1' O22 2.86(2) . ? K1' O23 3.23(2) . ? N1 C1 1.328(10) . ? N1 C12 1.363(10) . ? N2 C10 1.344(9) . ? N2 C11 1.361(10) . ? N3 C13 1.162(9) . ? N4 C14 1.139(10) . ? N5 C17 1.304(11) . ? N5 C28 1.360(11) . ? N6 C26 1.322(13) . ? N6 C27 1.353(13) . ? N7 C32 1.157(13) . ? N8 C30 1.160(10) . ? N9 C31 1.157(11) . ? N10 C29 1.173(9) . ? N11 C33 1.327(9) . ? N11 C44 1.363(9) . ? N12 C42 1.347(9) . ? N12 C43 1.352(9) . ? N13 C45 1.329(9) . ? N13 C56 1.370(9) . ? N14 C54 1.315(9) . ? N14 C55 1.369(9) . ? N23 C16 1.142(11) . ? N24 C15 1.161(9) . ? N24 Yb1 2.345(6) 3_667 ? C1 C2 1.409(12) . ? C1 H1 0.9300 . ? C2 C3 1.341(14) . ? C2 H2 0.9300 . ? C3 C4 1.393(14) . ? C3 H3 0.9300 . ? C4 C12 1.409(12) . ? C4 C5 1.425(14) . ? C5 C6 1.341(15) . ? C5 H5 0.9300 . ? C6 C7 1.443(13) . ? C6 H6 0.9300 . ? C7 C8 1.393(13) . ? C7 C11 1.427(11) . ? C8 C9 1.360(13) . ? C8 H8 0.9300 . ? C9 C10 1.400(11) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.417(11) . ? C17 C18 1.392(13) . ? C17 H17 0.9300 . ? C18 C19 1.396(15) . ? C18 H18 0.9300 . ? C19 C20 1.350(17) . ? C19 H19 0.9300 . ? C20 C28 1.418(15) . ? C20 C21 1.447(16) . ? C21 C22 1.31(2) . ? C21 H21 0.9300 . ? C22 C23 1.48(2) . ? C22 H22 0.9300 . ? C23 C24 1.38(2) . ? C23 C27 1.425(13) . ? C24 C25 1.35(2) . ? C24 H24 0.9300 . ? C25 C26 1.424(16) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.431(15) . ? C33 C34 1.393(11) . ? C33 H33 0.9300 . ? C34 C35 1.377(12) . ? C34 H34 0.9300 . ? C35 C36 1.379(12) . ? C35 H35 0.9300 . ? C36 C44 1.395(10) . ? C36 C37 1.452(12) . ? C37 C38 1.335(13) . ? C37 H37 0.9300 . ? C38 C39 1.462(12) . ? C38 H38 0.9300 . ? C39 C40 1.379(12) . ? C39 C43 1.408(11) . ? C40 C41 1.370(12) . ? C40 H40 0.9300 . ? C41 C42 1.396(10) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.450(10) . ? C45 C46 1.400(11) . ? C45 H45 0.9300 . ? C46 C47 1.353(12) . ? C46 H46 0.9300 . ? C47 C48 1.405(11) . ? C47 H47 0.9300 . ? C48 C56 1.409(10) . ? C48 C49 1.439(11) . ? C49 C50 1.342(12) . ? C49 H49 0.9300 . ? C50 C51 1.388(11) . ? C50 H50 0.9300 . ? C51 C52 1.415(11) . ? C51 C55 1.429(9) . ? C52 C53 1.370(12) . ? C52 H52 0.9300 . ? C53 C54 1.417(10) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.426(10) . ? O3 H3A 0.9700 . ? O3 H3B 0.9700 . ? O4 H4A 0.9700 . ? O4 H4B 0.9700 . ? O5 H5A 0.9700 . ? O5 H5B 0.9700 . ? O6 H6A 0.9700 . ? O6 H6B 0.9700 . ? O7 H7A 0.9700 . ? O7 H7B 0.9700 . ? O8' O22 1.67(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 O1 Yb1 N3 82.9(2) . . ? O1 Yb1 N10 79.4(2) . . ? N3 Yb1 N10 77.68(19) . . ? O1 Yb1 N24 72.3(2) . 3_667 ? N3 Yb1 N24 78.2(2) . 3_667 ? N10 Yb1 N24 144.7(2) . 3_667 ? O1 Yb1 N13 150.41(19) . . ? N3 Yb1 N13 77.8(2) . . ? N10 Yb1 N13 117.3(2) . . ? N24 Yb1 N13 82.0(2) 3_667 . ? O1 Yb1 N12 74.64(19) . . ? N3 Yb1 N12 150.8(2) . . ? N10 Yb1 N12 80.02(19) . . ? N24 Yb1 N12 111.3(2) 3_667 . ? N13 Yb1 N12 129.9(2) . . ? O1 Yb1 N14 143.51(19) . . ? N3 Yb1 N14 115.58(19) . . ? N10 Yb1 N14 74.82(19) . . ? N24 Yb1 N14 139.6(2) 3_667 . ? N13 Yb1 N14 65.96(19) . . ? N12 Yb1 N14 75.80(19) . . ? O1 Yb1 N11 110.4(2) . . ? N3 Yb1 N11 142.6(2) . . ? N10 Yb1 N11 137.95(19) . . ? N24 Yb1 N11 73.4(2) 3_667 . ? N13 Yb1 N11 74.57(19) . . ? N12 Yb1 N11 64.77(19) . . ? N14 Yb1 N11 74.83(18) . . ? C15 Ru1 C13 93.4(3) . . ? C15 Ru1 C14 90.0(3) . . ? C13 Ru1 C14 89.9(3) . . ? C15 Ru1 C16 86.3(3) . . ? C13 Ru1 C16 89.4(3) . . ? C14 Ru1 C16 176.3(3) . . ? C15 Ru1 N1 93.9(3) . . ? C13 Ru1 N1 172.3(3) . . ? C14 Ru1 N1 87.5(3) . . ? C16 Ru1 N1 93.6(3) . . ? C15 Ru1 N2 170.0(3) . . ? C13 Ru1 N2 95.3(2) . . ? C14 Ru1 N2 95.0(3) . . ? C16 Ru1 N2 88.7(3) . . ? N1 Ru1 N2 77.8(2) . . ? C29 Ru2 C32 89.7(3) . . ? C29 Ru2 C31 90.0(3) . . ? C32 Ru2 C31 91.6(4) . . ? C29 Ru2 C30 92.8(3) . . ? C32 Ru2 C30 89.0(4) . . ? C31 Ru2 C30 177.1(3) . . ? C29 Ru2 N5 95.8(3) . . ? C32 Ru2 N5 174.4(4) . . ? C31 Ru2 N5 89.6(3) . . ? C30 Ru2 N5 89.6(3) . . ? C29 Ru2 N6 174.1(3) . . ? C32 Ru2 N6 96.1(4) . . ? C31 Ru2 N6 90.3(3) . . ? C30 Ru2 N6 86.8(3) . . ? N5 Ru2 N6 78.4(3) . . ? O21 K1 O20 59.0(6) . . ? O21 K1 O22 89.5(6) . . ? O20 K1 O22 94.1(7) . . ? O21 K1 O23 122.6(6) . . ? O20 K1 O23 172.0(7) . . ? O22 K1 O23 78.3(7) . . ? O21 K1 O20 57.7(5) . 3_666 ? O20 K1 O20 40.6(8) . 3_666 ? O22 K1 O20 132.3(7) . 3_666 ? O23 K1 O20 147.3(7) . 3_666 ? O21 K1 O11 47.9(5) . . ? O20 K1 O11 104.9(6) . . ? O22 K1 O11 99.8(7) . . ? O23 K1 O11 79.0(7) . . ? O20 K1 O11 83.6(6) 3_666 . ? O21 K1 K1 55.9(3) . 3_666 ? O20 K1 K1 22.5(5) . 3_666 ? O22 K1 K1 115.5(5) . 3_666 ? O23 K1 K1 165.4(5) . 3_666 ? O20 K1 K1 18.1(4) 3_666 3_666 ? O11 K1 K1 93.3(4) . 3_666 ? O20 O20 K1 85.5(14) 3_666 . ? O20 O20 K1 53.9(10) 3_666 3_666 ? K1 O20 K1 139.4(8) . 3_666 ? O11' K1' K1' 155.7(7) . 3_666 ? O11' K1' O22 67.8(7) . . ? K1' K1' O22 121.4(6) 3_666 . ? O11' K1' O23 58.6(7) . . ? K1' K1' O23 145.6(6) 3_666 . ? O22 K1' O23 57.7(6) . . ? C1 N1 C12 117.8(7) . . ? C1 N1 Ru1 127.6(6) . . ? C12 N1 Ru1 114.4(5) . . ? C10 N2 C11 117.8(6) . . ? C10 N2 Ru1 128.4(5) . . ? C11 N2 Ru1 113.7(5) . . ? C13 N3 Yb1 169.6(6) . . ? C17 N5 C28 117.6(8) . . ? C17 N5 Ru2 129.5(5) . . ? C28 N5 Ru2 112.8(6) . . ? C26 N6 C27 118.6(9) . . ? C26 N6 Ru2 128.4(8) . . ? C27 N6 Ru2 113.0(6) . . ? C29 N10 Yb1 164.4(5) . . ? C33 N11 C44 116.3(6) . . ? C33 N11 Yb1 125.1(5) . . ? C44 N11 Yb1 118.4(5) . . ? C42 N12 C43 117.4(6) . . ? C42 N12 Yb1 122.5(5) . . ? C43 N12 Yb1 119.1(5) . . ? C45 N13 C56 117.8(6) . . ? C45 N13 Yb1 122.7(5) . . ? C56 N13 Yb1 119.1(5) . . ? C54 N14 C55 117.5(6) . . ? C54 N14 Yb1 124.4(5) . . ? C55 N14 Yb1 118.1(4) . . ? C15 N24 Yb1 175.5(6) . 3_667 ? N1 C1 C2 122.6(9) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.3(9) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 120.6(8) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C12 117.3(8) . . ? C3 C4 C5 124.7(9) . . ? C12 C4 C5 118.0(9) . . ? C6 C5 C4 121.6(9) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 122.0(9) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C11 117.1(8) . . ? C8 C7 C6 125.4(8) . . ? C11 C7 C6 117.4(9) . . ? C9 C8 C7 120.1(8) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.0(8) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? N2 C10 C9 122.3(8) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? N2 C11 C12 117.7(7) . . ? N2 C11 C7 122.7(7) . . ? C12 C11 C7 119.6(7) . . ? N1 C12 C4 122.4(7) . . ? N1 C12 C11 116.4(7) . . ? C4 C12 C11 121.2(7) . . ? N3 C13 Ru1 176.1(6) . . ? N4 C14 Ru1 176.1(7) . . ? N24 C15 Ru1 174.5(6) . . ? N23 C16 Ru1 176.2(8) . . ? N5 C17 C18 124.9(9) . . ? N5 C17 H17 117.5 . . ? C18 C17 H17 117.5 . . ? C17 C18 C19 117.2(11) . . ? C17 C18 H18 121.4 . . ? C19 C18 H18 121.4 . . ? C20 C19 C18 119.7(11) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C28 119.2(10) . . ? C19 C20 C21 123.3(13) . . ? C28 C20 C21 117.5(13) . . ? C22 C21 C20 122.1(15) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C21 C22 C23 122.3(11) . . ? C21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C24 C23 C27 117.1(14) . . ? C24 C23 C22 125.8(12) . . ? C27 C23 C22 117.1(13) . . ? C25 C24 C23 119.9(12) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.5(13) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? N6 C26 C25 121.0(14) . . ? N6 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? N6 C27 C23 122.8(11) . . ? N6 C27 C28 117.7(8) . . ? C23 C27 C28 119.5(12) . . ? N5 C28 C20 121.3(10) . . ? N5 C28 C27 117.3(9) . . ? C20 C28 C27 121.3(9) . . ? N10 C29 Ru2 178.0(6) . . ? N8 C30 Ru2 176.2(7) . . ? N9 C31 Ru2 177.7(7) . . ? N7 C32 Ru2 175.8(12) . . ? N11 C33 C34 124.1(8) . . ? N11 C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? C35 C34 C33 118.3(8) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C34 C35 C36 119.6(8) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C44 118.0(7) . . ? C35 C36 C37 123.0(8) . . ? C44 C36 C37 119.0(7) . . ? C38 C37 C36 120.8(8) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 122.1(8) . . ? C37 C38 H38 119.0 . . ? C39 C38 H38 119.0 . . ? C40 C39 C43 119.1(8) . . ? C40 C39 C38 123.1(8) . . ? C43 C39 C38 117.7(8) . . ? C41 C40 C39 119.0(7) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C40 C41 C42 119.3(8) . . ? C40 C41 H41 120.4 . . ? C42 C41 H41 120.4 . . ? N12 C42 C41 123.0(7) . . ? N12 C42 H42 118.5 . . ? C41 C42 H42 118.5 . . ? N12 C43 C39 122.1(7) . . ? N12 C43 C44 117.7(6) . . ? C39 C43 C44 120.0(7) . . ? N11 C44 C36 123.4(7) . . ? N11 C44 C43 116.5(6) . . ? C36 C44 C43 120.1(7) . . ? N13 C45 C46 123.5(7) . . ? N13 C45 H45 118.3 . . ? C46 C45 H45 118.3 . . ? C47 C46 C45 118.7(7) . . ? C47 C46 H46 120.7 . . ? C45 C46 H46 120.7 . . ? C46 C47 C48 120.6(7) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C47 C48 C56 117.2(7) . . ? C47 C48 C49 124.1(7) . . ? C56 C48 C49 118.7(7) . . ? C50 C49 C48 121.2(7) . . ? C50 C49 H49 119.4 . . ? C48 C49 H49 119.4 . . ? C49 C50 C51 121.4(7) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C50 C51 C52 123.0(7) . . ? C50 C51 C55 120.4(7) . . ? C52 C51 C55 116.7(7) . . ? C53 C52 C51 119.7(7) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C54 119.0(7) . . ? C52 C53 H53 120.5 . . ? C54 C53 H53 120.5 . . ? N14 C54 C53 123.9(7) . . ? N14 C54 H54 118.1 . . ? C53 C54 H54 118.1 . . ? N14 C55 C56 118.3(6) . . ? N14 C55 C51 123.2(7) . . ? C56 C55 C51 118.5(7) . . ? N13 C56 C48 122.2(7) . . ? N13 C56 C55 117.9(6) . . ? C48 C56 C55 119.9(6) . . ? H3A O3 H3B 117.2 . . ? H4A O4 H4B 117.3 . . ? H5A O5 H5B 114.4 . . ? H6A O6 H6B 113.3 . . ? H7A O7 H7B 115.4 . . ? O8' O22 K1 135.3(15) . . ? O8' O22 K1' 142.2(14) . . ? K1 O22 K1' 20.4(2) . . ? K1 O23 K1' 12.3(2) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 2.896 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.197 #===END data_imw451s _database_code_depnum_ccdc_archive 'CCDC 605808' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H51 N12 O14 Pr Ru1.50' _chemical_formula_weight 1204.43 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 21.5398(8) _cell_length_b 26.2480(8) _cell_length_c 17.1392(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9690.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4848 _exptl_absorpt_coefficient_mu 1.530 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 166900 _diffrn_reflns_av_R_equivalents 0.1617 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.26 _reflns_number_total 10016 _reflns_number_gt 6509 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0624P)^2^+208.1100P] 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 10016 _refine_ls_number_parameters 634 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2167 _refine_ls_wR_factor_gt 0.1964 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 Pr1 Pr 0.21314(2) 0.42476(2) 0.74613(3) 0.02211(16) Uani 1 1 d . . . Ru1 Ru 0.21207(6) 0.2500 0.07547(7) 0.0246(3) Uani 1 2 d S . . Ru2 Ru -0.04346(3) 0.47197(3) 0.75395(5) 0.02012(19) Uani 1 1 d . . . C1 C -0.0314(5) 0.5313(5) 0.9133(6) 0.031(3) Uani 1 1 d . . . H1A H -0.0404 0.4998 0.9379 0.037 Uiso 1 1 calc R . . C2 C -0.0245(6) 0.5732(5) 0.9595(7) 0.043(3) Uani 1 1 d . . . H2A H -0.0315 0.5708 1.0141 0.051 Uiso 1 1 calc R . . C3 C -0.0071(6) 0.6195(5) 0.9265(8) 0.044(3) Uani 1 1 d . . . H3A H 0.0003 0.6486 0.9583 0.053 Uiso 1 1 calc R . . C4 C -0.0008(5) 0.6221(5) 0.8456(7) 0.032(3) Uani 1 1 d . . . C5 C 0.0171(6) 0.6675(5) 0.8058(8) 0.041(3) Uani 1 1 d . . . H5A H 0.0257 0.6974 0.8351 0.049 Uiso 1 1 calc R . . C6 C 0.0221(6) 0.6688(5) 0.7273(8) 0.041(3) Uani 1 1 d . . . H6A H 0.0336 0.6998 0.7024 0.049 Uiso 1 1 calc R . . C7 C 0.0104(5) 0.6244(4) 0.6808(7) 0.030(3) Uani 1 1 d . . . C8 C 0.0138(5) 0.6225(5) 0.5997(7) 0.037(3) Uani 1 1 d . . . H8A H 0.0260 0.6520 0.5714 0.044 Uiso 1 1 calc R . . C9 C -0.0004(6) 0.5787(5) 0.5603(8) 0.045(3) Uani 1 1 d . . . H9A H 0.0020 0.5775 0.5050 0.054 Uiso 1 1 calc R . . C10 C -0.0184(5) 0.5359(5) 0.6023(7) 0.031(3) Uani 1 1 d . . . H10A H -0.0289 0.5060 0.5739 0.037 Uiso 1 1 calc R . . C11 C -0.0073(5) 0.5782(4) 0.7183(7) 0.028(2) Uani 1 1 d . . . C12 C -0.0114(5) 0.5768(4) 0.8013(7) 0.029(2) Uani 1 1 d . . . C13 C -0.0588(5) 0.4224(4) 0.6696(6) 0.025(2) Uani 1 1 d . . . C14 C -0.1375(5) 0.4849(4) 0.7599(6) 0.025(2) Uani 1 1 d . . . C15 C -0.0588(5) 0.4176(4) 0.8306(6) 0.026(2) Uani 1 1 d . . . C16 C 0.0488(4) 0.4493(4) 0.7510(6) 0.023(2) Uani 1 1 d . . . C17 C 0.1929(5) 0.4599(6) 0.9407(7) 0.045(3) Uani 1 1 d . . . H17A H 0.2066 0.4256 0.9455 0.053 Uiso 1 1 calc R . . C18 C 0.1751(6) 0.4856(7) 1.0086(8) 0.055(4) Uani 1 1 d . . . H18A H 0.1761 0.4698 1.0584 0.066 Uiso 1 1 calc R . . C19 C 0.1560(7) 0.5351(8) 0.9989(10) 0.066(5) Uani 1 1 d . . . H19A H 0.1444 0.5541 1.0438 0.079 Uiso 1 1 calc R . . C20 C 0.1530(6) 0.5586(7) 0.9264(10) 0.062(4) Uani 1 1 d . . . H20A H 0.1382 0.5925 0.9204 0.075 Uiso 1 1 calc R . . C21 C 0.1732(5) 0.5295(5) 0.8622(8) 0.039(3) Uani 1 1 d . . . C22 C 0.1740(6) 0.5530(5) 0.7834(9) 0.043(3) Uani 1 1 d . . . C23 C 0.1691(6) 0.6055(6) 0.7723(12) 0.064(5) Uani 1 1 d . . . H23A H 0.1659 0.6276 0.8160 0.076 Uiso 1 1 calc R . . C24 C 0.1689(6) 0.6243(5) 0.7015(12) 0.062(5) Uani 1 1 d . . . H24A H 0.1671 0.6602 0.6942 0.074 Uiso 1 1 calc R . . C25 C 0.1714(6) 0.5918(6) 0.6361(11) 0.056(4) Uani 1 1 d . . . H25A H 0.1699 0.6053 0.5847 0.067 Uiso 1 1 calc R . . C26 C 0.1762(5) 0.5395(5) 0.6486(8) 0.041(3) Uani 1 1 d . . . C27 C 0.1774(5) 0.5022(5) 0.5841(8) 0.040(3) Uani 1 1 d . . . C28 C 0.1614(6) 0.5179(7) 0.5076(9) 0.062(5) Uani 1 1 d . . . H28A H 0.1470 0.5512 0.4960 0.074 Uiso 1 1 calc R . . C29 C 0.1686(7) 0.4800(9) 0.4504(9) 0.069(5) Uani 1 1 d . . . H29A H 0.1579 0.4885 0.3982 0.083 Uiso 1 1 calc R . . C30 C 0.1891(7) 0.4336(8) 0.4638(9) 0.068(5) Uani 1 1 d . . . H30A H 0.1948 0.4098 0.4226 0.081 Uiso 1 1 calc R . . C31 C 0.2022(7) 0.4204(7) 0.5424(8) 0.057(4) Uani 1 1 d . . . H31A H 0.2157 0.3868 0.5541 0.068 Uiso 1 1 calc R . . C32 C 0.1797(6) 0.3514(5) 0.1608(8) 0.037(3) Uani 1 1 d . . . H32A H 0.1941 0.3682 0.1152 0.045 Uiso 1 1 calc R . . C33 C 0.1602(6) 0.3810(5) 0.2238(8) 0.046(3) Uani 1 1 d . . . H33A H 0.1613 0.4171 0.2209 0.055 Uiso 1 1 calc R . . C34 C 0.1396(6) 0.3573(5) 0.2897(9) 0.047(4) Uani 1 1 d . . . H34A H 0.1258 0.3770 0.3328 0.057 Uiso 1 1 calc R . . C35 C 0.1387(5) 0.3042(5) 0.2941(7) 0.039(3) Uani 1 1 d . . . C36 C 0.1177(6) 0.2758(5) 0.3611(7) 0.047(3) Uani 1 1 d . . . H36A H 0.1036 0.2936 0.4060 0.056 Uiso 1 1 calc R . . C37 C 0.1585(5) 0.2765(4) 0.2284(7) 0.031(3) Uani 1 1 d . . . C38 C 0.2405(5) 0.3036(5) 0.0029(7) 0.034(3) Uani 1 1 d . . . C39 C 0.1281(9) 0.2500 0.0219(10) 0.039(4) Uani 1 2 d S . . C40 C 0.2978(7) 0.2500 0.1261(9) 0.025(3) Uani 1 2 d S . . N1 N -0.0262(4) 0.5317(3) 0.8344(5) 0.0229(19) Uani 1 1 d . . . N2 N -0.0218(4) 0.5342(3) 0.6798(5) 0.0234(19) Uani 1 1 d . . . N3 N -0.0672(5) 0.3850(4) 0.8758(6) 0.037(2) Uani 1 1 d . . . N4 N -0.0680(4) 0.3923(4) 0.6207(6) 0.031(2) Uani 1 1 d . . . N5 N -0.1919(4) 0.4831(3) 0.7643(5) 0.026(2) Uani 1 1 d . . . N6 N 0.0969(4) 0.4356(4) 0.7483(6) 0.033(2) Uani 1 1 d . . . N7 N 0.1961(5) 0.4547(4) 0.6013(6) 0.040(3) Uani 1 1 d . . . N8 N 0.1801(4) 0.5199(4) 0.7221(6) 0.037(2) Uani 1 1 d . . . N9 N 0.1917(4) 0.4808(4) 0.8694(5) 0.033(2) Uani 1 1 d . . . N10 N 0.1791(4) 0.3007(3) 0.1618(5) 0.028(2) Uani 1 1 d . . . N11 N 0.2585(5) 0.3359(5) -0.0373(7) 0.049(3) Uani 1 1 d . . . N12 N 0.0776(7) 0.2500 -0.0072(10) 0.048(4) Uani 1 2 d S . . N13 N 0.3465(6) 0.2500 0.1571(8) 0.032(3) Uani 1 2 d S . . O1 O 0.2930(4) 0.3964(3) 0.8429(5) 0.040(2) Uani 1 1 d . . . O2 O 0.1720(4) 0.3591(4) 0.8406(5) 0.051(3) Uani 1 1 d . . . O3 O 0.2949(4) 0.3751(3) 0.6719(5) 0.039(2) Uani 1 1 d . . . O4 O 0.1670(4) 0.3471(3) 0.6755(5) 0.045(2) Uani 1 1 d . . . O5 O 0.0572(5) 0.2500 0.5381(7) 0.039(3) Uani 1 2 d S . . O6 O 0.9492(5) 0.2500 0.4510(7) 0.036(3) Uani 1 2 d S . . O7 O 0.9972(6) 0.2500 0.7557(8) 0.054(4) Uani 1 2 d S . . O8 O 0.9506(6) 0.2500 0.0206(12) 0.076(5) Uani 1 2 d S . . O9 O 0.0553(5) 0.3294(5) 0.8740(9) 0.103(5) Uani 1 1 d . . . O10 O 0.1986(8) 0.2500 0.7424(14) 0.107(7) Uani 1 2 d S . . O11 O 0.2926(10) 0.2500 0.3200(11) 0.101(6) Uani 1 2 d S . . O12 O 0.3864(8) 0.2977(6) 0.9297(10) 0.039(3) Uiso 0.50 1 d PU A 1 O12' O 0.4022(8) 0.2887(7) 0.8355(10) 0.041(3) Uiso 0.50 1 d PU B 2 O13 O 0.0409(8) 0.3235(7) 0.6566(10) 0.041(3) Uiso 0.50 1 d PU C 1 O13' O 0.0639(8) 0.3458(7) 0.6043(10) 0.045(3) Uiso 0.50 1 d PU D 2 O14 O 0.6869(8) 0.2729(6) 0.9549(10) 0.046(5) Uani 0.50 1 d P . . O15 O 0.8502(9) 0.3117(7) 0.0711(11) 0.051(4) Uiso 0.50 1 d PU E 1 O15' O 0.8789(9) 0.3324(7) 0.0072(11) 0.049(4) Uiso 0.50 1 d PU F 2 O16 O 0.7633(9) 0.3166(7) 0.0728(11) 0.053(5) Uiso 0.50 1 d P . . O17 O 0.3171(10) 0.2757(7) 0.7168(14) 0.065(6) Uani 0.50 1 d P . . O18 O 0.4127(9) 0.2775(7) 0.6344(14) 0.064(6) Uani 0.50 1 d P . . O19 O 0.758(3) 0.322(2) 0.964(3) 0.201(15) Uiso 0.50 1 d PU G 1 O19' O 0.774(3) 0.299(2) 0.926(3) 0.201(15) Uiso 0.50 1 d PU H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0149(3) 0.0268(3) 0.0246(3) 0.0026(2) 0.0001(2) -0.0019(2) Ru1 0.0197(6) 0.0297(6) 0.0243(6) 0.000 0.0011(5) 0.000 Ru2 0.0125(4) 0.0224(4) 0.0254(4) -0.0006(4) 0.0009(3) -0.0016(3) C1 0.034(6) 0.033(6) 0.025(6) 0.002(5) -0.002(5) 0.008(5) C2 0.057(8) 0.044(7) 0.027(6) 0.000(6) -0.015(6) 0.007(7) C3 0.053(8) 0.033(7) 0.046(8) -0.018(6) -0.020(7) 0.006(6) C4 0.015(5) 0.035(6) 0.047(7) -0.004(5) -0.005(5) 0.000(5) C5 0.033(7) 0.032(7) 0.057(8) -0.004(6) -0.011(6) -0.006(6) C6 0.036(7) 0.025(6) 0.062(9) 0.007(6) 0.002(6) -0.010(5) C7 0.030(6) 0.021(5) 0.040(7) 0.005(5) -0.002(5) 0.000(5) C8 0.020(6) 0.042(7) 0.049(8) 0.008(6) 0.006(5) -0.003(5) C9 0.044(8) 0.053(8) 0.037(7) 0.001(6) 0.004(6) 0.015(7) C10 0.017(5) 0.036(6) 0.039(7) -0.002(5) 0.004(5) 0.005(5) C11 0.022(6) 0.022(5) 0.040(6) 0.001(5) -0.005(5) 0.001(5) C12 0.018(5) 0.027(6) 0.043(7) -0.005(5) -0.002(5) 0.003(5) C13 0.015(5) 0.034(6) 0.027(6) 0.001(5) 0.000(4) 0.001(5) C14 0.037(6) 0.021(5) 0.017(5) -0.006(4) 0.001(4) -0.009(4) C15 0.023(6) 0.028(6) 0.028(6) -0.002(5) 0.000(4) 0.007(5) C16 0.011(5) 0.034(5) 0.024(5) 0.001(5) -0.001(5) -0.016(4) C17 0.022(6) 0.075(10) 0.036(7) -0.006(7) -0.001(5) 0.003(6) C18 0.024(7) 0.104(14) 0.035(7) -0.013(8) 0.007(6) -0.007(8) C19 0.035(8) 0.106(15) 0.057(10) -0.031(10) -0.004(7) -0.001(9) C20 0.024(7) 0.082(11) 0.080(12) -0.027(10) -0.002(7) 0.008(7) C21 0.021(6) 0.046(8) 0.051(8) -0.023(6) 0.005(5) 0.007(5) C22 0.021(6) 0.034(7) 0.073(9) -0.015(7) -0.007(6) 0.006(5) C23 0.028(7) 0.036(8) 0.126(16) -0.007(9) -0.012(8) 0.003(6) C24 0.017(6) 0.030(8) 0.138(17) 0.017(10) 0.000(8) 0.002(6) C25 0.020(6) 0.053(9) 0.094(12) 0.025(9) 0.004(7) 0.007(6) C26 0.018(6) 0.044(7) 0.061(9) 0.030(7) -0.002(6) 0.001(5) C27 0.016(6) 0.059(8) 0.045(7) 0.028(7) -0.007(5) -0.002(5) C28 0.028(7) 0.110(14) 0.048(9) 0.032(9) -0.005(6) -0.022(8) C29 0.030(8) 0.137(18) 0.040(9) 0.019(11) -0.005(6) -0.012(10) C30 0.036(8) 0.125(17) 0.042(9) -0.018(10) 0.004(7) -0.022(10) C31 0.047(9) 0.084(11) 0.040(8) -0.013(8) 0.003(6) -0.021(8) C32 0.033(7) 0.034(7) 0.046(7) 0.005(6) 0.003(6) 0.000(5) C33 0.047(8) 0.032(7) 0.060(9) -0.005(6) -0.003(7) 0.010(6) C34 0.026(7) 0.054(9) 0.061(9) -0.031(7) 0.001(6) 0.006(6) C35 0.019(6) 0.058(8) 0.038(7) -0.005(6) -0.004(5) 0.000(6) C36 0.034(7) 0.072(9) 0.035(7) -0.006(6) 0.004(6) 0.010(6) C37 0.022(6) 0.037(6) 0.034(6) -0.003(5) 0.000(5) -0.001(5) C38 0.025(6) 0.040(7) 0.037(7) 0.003(6) 0.003(5) 0.004(5) C39 0.045(11) 0.040(10) 0.033(9) 0.000 -0.010(8) 0.000 C40 0.024(8) 0.023(8) 0.027(8) 0.000 0.001(6) 0.000 N1 0.010(4) 0.031(5) 0.027(5) -0.002(4) -0.004(3) -0.001(4) N2 0.015(4) 0.029(5) 0.026(5) 0.003(4) 0.002(4) 0.001(4) N3 0.032(6) 0.035(6) 0.045(6) 0.001(5) 0.005(5) 0.002(5) N4 0.015(5) 0.039(6) 0.040(6) -0.013(5) 0.000(4) -0.003(4) N5 0.005(4) 0.030(5) 0.041(6) -0.004(4) 0.003(4) 0.002(3) N6 0.014(4) 0.041(5) 0.042(5) 0.000(5) -0.005(4) -0.009(4) N7 0.029(6) 0.059(7) 0.033(6) 0.001(5) 0.004(4) -0.003(5) N8 0.024(5) 0.032(5) 0.054(6) -0.002(5) 0.006(5) -0.002(4) N9 0.020(5) 0.055(7) 0.026(5) -0.009(5) -0.004(4) 0.000(4) N10 0.023(5) 0.027(5) 0.033(5) -0.001(4) 0.001(4) 0.006(4) N11 0.024(5) 0.071(8) 0.050(7) 0.030(6) 0.001(5) 0.002(5) N12 0.026(8) 0.065(11) 0.051(10) 0.000 -0.001(7) 0.000 N13 0.018(7) 0.041(8) 0.038(8) 0.000 -0.006(6) 0.000 O1 0.025(4) 0.054(5) 0.041(5) 0.021(4) -0.011(4) -0.009(4) O2 0.029(5) 0.068(6) 0.055(6) 0.030(5) -0.003(4) -0.009(4) O3 0.033(5) 0.041(5) 0.043(5) -0.009(4) 0.008(4) 0.002(4) O4 0.032(5) 0.046(5) 0.058(6) -0.016(4) 0.016(4) -0.013(4) O5 0.025(6) 0.050(8) 0.041(7) 0.000 0.004(5) 0.000 O6 0.021(6) 0.041(7) 0.046(7) 0.000 0.000(5) 0.000 O7 0.040(8) 0.064(9) 0.059(9) 0.000 -0.002(7) 0.000 O8 0.029(8) 0.055(10) 0.143(16) 0.000 -0.009(9) 0.000 O9 0.029(6) 0.112(10) 0.168(13) 0.091(10) 0.026(7) 0.006(6) O10 0.052(11) 0.095(14) 0.17(2) 0.000 -0.025(13) 0.000 O11 0.092(15) 0.135(18) 0.075(12) 0.000 -0.031(11) 0.000 O14 0.034(9) 0.055(11) 0.049(10) -0.001(8) -0.012(8) 0.009(8) O17 0.063(14) 0.038(10) 0.096(16) -0.006(11) -0.026(12) -0.006(10) O18 0.040(11) 0.059(13) 0.093(16) 0.008(11) -0.004(11) -0.014(10) _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 Pr1 O1 2.504(8) . ? Pr1 N6 2.521(9) . ? Pr1 O2 2.525(8) . ? Pr1 O3 2.534(8) . ? Pr1 N5 2.561(8) 6_657 ? Pr1 O4 2.571(8) . ? Pr1 N9 2.616(9) . ? Pr1 N8 2.629(10) . ? Pr1 N7 2.629(10) . ? Ru1 C38 1.974(12) 7_565 ? Ru1 C38 1.974(12) . ? Ru1 C39 2.029(18) . ? Ru1 C40 2.040(15) . ? Ru1 N10 2.113(9) . ? Ru1 N10 2.113(9) 7_565 ? Ru2 C15 1.969(11) . ? Ru2 C13 1.973(11) . ? Ru2 C14 2.055(11) . ? Ru2 C16 2.075(10) . ? Ru2 N1 2.121(9) . ? Ru2 N2 2.121(9) . ? C1 N1 1.357(13) . ? C1 C2 1.364(16) . ? C1 H1A 0.9500 . ? C2 C3 1.392(18) . ? C2 H2A 0.9500 . ? C3 C4 1.394(18) . ? C3 H3A 0.9500 . ? C4 C5 1.426(17) . ? C4 C12 1.431(16) . ? C5 C6 1.349(18) . ? C5 H5A 0.9500 . ? C6 C7 1.435(16) . ? C6 H6A 0.9500 . ? C7 C8 1.392(17) . ? C7 C11 1.425(15) . ? C8 C9 1.368(18) . ? C8 H8A 0.9500 . ? C9 C10 1.389(17) . ? C9 H9A 0.9500 . ? C10 N2 1.332(14) . ? C10 H10A 0.9500 . ? C11 N2 1.366(14) . ? C11 C12 1.425(16) . ? C12 N1 1.350(14) . ? C13 N4 1.168(14) . ? C14 N5 1.177(13) . ? C15 N3 1.168(14) . ? C16 N6 1.097(13) . ? C17 N9 1.340(16) . ? C17 C18 1.398(18) . ? C17 H17A 0.9500 . ? C18 C19 1.37(2) . ? C18 H18A 0.9500 . ? C19 C20 1.39(2) . ? C19 H19A 0.9500 . ? C20 C21 1.409(18) . ? C20 H20A 0.9500 . ? C21 N9 1.344(16) . ? C21 C22 1.48(2) . ? C22 N8 1.371(16) . ? C22 C23 1.394(19) . ? C23 C24 1.31(2) . ? C23 H23A 0.9500 . ? C24 C25 1.41(2) . ? C24 H24A 0.9500 . ? C25 C26 1.395(18) . ? C25 H25A 0.9500 . ? C26 N8 1.364(16) . ? C26 C27 1.48(2) . ? C27 N7 1.342(16) . ? C27 C28 1.417(18) . ? C28 C29 1.41(2) . ? C28 H28A 0.9500 . ? C29 C30 1.32(2) . ? C29 H29A 0.9500 . ? C30 C31 1.42(2) . ? C30 H30A 0.9500 . ? C31 N7 1.359(17) . ? C31 H31A 0.9500 . ? C32 N10 1.333(14) . ? C32 C33 1.395(18) . ? C32 H32A 0.9500 . ? C33 C34 1.36(2) . ? C33 H33A 0.9500 . ? C34 C35 1.395(19) . ? C34 H34A 0.9500 . ? C35 C37 1.407(16) . ? C35 C36 1.442(18) . ? C36 C36 1.36(3) 7_565 ? C36 H36A 0.9500 . ? C37 N10 1.378(14) . ? C37 C37 1.39(2) 7_565 ? C38 N11 1.161(15) . ? C39 N12 1.20(2) . ? C40 N13 1.176(19) . ? N5 Pr1 2.561(8) 6_557 ? O14 O14 1.20(3) 7_565 ? O17 O17 1.35(4) 7_565 ? O18 O18 1.44(4) 7_565 ? 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 O1 Pr1 N6 135.0(3) . . ? O1 Pr1 O2 67.2(3) . . ? N6 Pr1 O2 73.7(3) . . ? O1 Pr1 O3 72.7(3) . . ? N6 Pr1 O3 139.1(3) . . ? O2 Pr1 O3 102.4(3) . . ? O1 Pr1 N5 71.0(3) . 6_657 ? N6 Pr1 N5 136.6(3) . 6_657 ? O2 Pr1 N5 137.1(3) . 6_657 ? O3 Pr1 N5 73.6(3) . 6_657 ? O1 Pr1 O4 110.0(3) . . ? N6 Pr1 O4 73.3(3) . . ? O2 Pr1 O4 68.0(3) . . ? O3 Pr1 O4 67.9(3) . . ? N5 Pr1 O4 138.6(3) 6_657 . ? O1 Pr1 N9 75.7(3) . . ? N6 Pr1 N9 75.5(3) . . ? O2 Pr1 N9 78.7(3) . . ? O3 Pr1 N9 144.9(3) . . ? N5 Pr1 N9 82.0(3) 6_657 . ? O4 Pr1 N9 139.3(3) . . ? O1 Pr1 N8 124.9(3) . . ? N6 Pr1 N8 68.1(3) . . ? O2 Pr1 N8 130.8(3) . . ? O3 Pr1 N8 126.7(3) . . ? N5 Pr1 N8 68.7(3) 6_657 . ? O4 Pr1 N8 125.1(3) . . ? N9 Pr1 N8 62.9(3) . . ? O1 Pr1 N7 144.1(3) . . ? N6 Pr1 N7 80.9(3) . . ? O2 Pr1 N7 139.5(3) . . ? O3 Pr1 N7 77.1(3) . . ? N5 Pr1 N7 82.4(3) 6_657 . ? O4 Pr1 N7 74.8(3) . . ? N9 Pr1 N7 124.7(3) . . ? N8 Pr1 N7 62.0(3) . . ? C38 Ru1 C38 90.9(7) 7_565 . ? C38 Ru1 C39 89.5(5) 7_565 . ? C38 Ru1 C39 89.5(5) . . ? C38 Ru1 C40 89.3(4) 7_565 . ? C38 Ru1 C40 89.3(4) . . ? C39 Ru1 C40 178.3(7) . . ? C38 Ru1 N10 173.6(4) 7_565 . ? C38 Ru1 N10 95.6(4) . . ? C39 Ru1 N10 91.0(5) . . ? C40 Ru1 N10 90.4(4) . . ? C38 Ru1 N10 95.6(4) 7_565 7_565 ? C38 Ru1 N10 173.6(4) . 7_565 ? C39 Ru1 N10 91.0(5) . 7_565 ? C40 Ru1 N10 90.4(4) . 7_565 ? N10 Ru1 N10 78.0(5) . 7_565 ? C15 Ru2 C13 89.0(4) . . ? C15 Ru2 C14 85.5(4) . . ? C13 Ru2 C14 88.9(4) . . ? C15 Ru2 C16 88.2(4) . . ? C13 Ru2 C16 87.3(4) . . ? C14 Ru2 C16 172.7(4) . . ? C15 Ru2 N1 97.6(4) . . ? C13 Ru2 N1 173.4(4) . . ? C14 Ru2 N1 91.1(3) . . ? C16 Ru2 N1 93.4(4) . . ? C15 Ru2 N2 174.4(4) . . ? C13 Ru2 N2 96.0(4) . . ? C14 Ru2 N2 96.9(4) . . ? C16 Ru2 N2 89.8(4) . . ? N1 Ru2 N2 77.4(3) . . ? N1 C1 C2 124.3(11) . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? C1 C2 C3 119.9(12) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C2 C3 C4 118.2(11) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C3 C4 C5 122.9(11) . . ? C3 C4 C12 118.1(11) . . ? C5 C4 C12 118.9(11) . . ? C6 C5 C4 121.4(12) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C5 C6 C7 121.3(11) . . ? C5 C6 H6A 119.4 . . ? C7 C6 H6A 119.4 . . ? C8 C7 C11 115.7(11) . . ? C8 C7 C6 125.1(11) . . ? C11 C7 C6 119.2(11) . . ? C9 C8 C7 120.7(12) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 119.1(12) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? N2 C10 C9 124.0(11) . . ? N2 C10 H10A 118.0 . . ? C9 C10 H10A 118.0 . . ? N2 C11 C7 124.3(10) . . ? N2 C11 C12 116.5(10) . . ? C7 C11 C12 119.3(10) . . ? N1 C12 C11 117.1(10) . . ? N1 C12 C4 123.0(11) . . ? C11 C12 C4 119.9(11) . . ? N4 C13 Ru2 178.6(10) . . ? N5 C14 Ru2 168.2(9) . . ? N3 C15 Ru2 179.2(11) . . ? N6 C16 Ru2 177.3(10) . . ? N9 C17 C18 123.8(14) . . ? N9 C17 H17A 118.1 . . ? C18 C17 H17A 118.1 . . ? C19 C18 C17 116.0(15) . . ? C19 C18 H18A 122.0 . . ? C17 C18 H18A 122.0 . . ? C18 C19 C20 122.9(15) . . ? C18 C19 H19A 118.6 . . ? C20 C19 H19A 118.6 . . ? C19 C20 C21 116.3(16) . . ? C19 C20 H20A 121.8 . . ? C21 C20 H20A 121.8 . . ? N9 C21 C20 122.4(14) . . ? N9 C21 C22 118.5(10) . . ? C20 C21 C22 119.2(13) . . ? N8 C22 C23 122.0(15) . . ? N8 C22 C21 115.7(11) . . ? C23 C22 C21 122.4(14) . . ? C24 C23 C22 120.0(17) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.5(14) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C26 C25 C24 118.5(15) . . ? C26 C25 H25A 120.7 . . ? C24 C25 H25A 120.7 . . ? N8 C26 C25 121.2(14) . . ? N8 C26 C27 116.2(11) . . ? C25 C26 C27 122.7(13) . . ? N7 C27 C28 123.1(15) . . ? N7 C27 C26 117.2(10) . . ? C28 C27 C26 119.7(13) . . ? C29 C28 C27 114.4(16) . . ? C29 C28 H28A 122.8 . . ? C27 C28 H28A 122.8 . . ? C30 C29 C28 124.7(16) . . ? C30 C29 H29A 117.6 . . ? C28 C29 H29A 117.6 . . ? C29 C30 C31 117.3(17) . . ? C29 C30 H30A 121.3 . . ? C31 C30 H30A 121.3 . . ? N7 C31 C30 121.6(17) . . ? N7 C31 H31A 119.2 . . ? C30 C31 H31A 119.2 . . ? N10 C32 C33 122.9(12) . . ? N10 C32 H32A 118.6 . . ? C33 C32 H32A 118.6 . . ? C34 C33 C32 119.1(12) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C33 C34 C35 120.3(12) . . ? C33 C34 H34A 119.8 . . ? C35 C34 H34A 119.8 . . ? C34 C35 C37 117.9(12) . . ? C34 C35 C36 124.3(12) . . ? C37 C35 C36 117.7(12) . . ? C36 C36 C35 121.2(8) 7_565 . ? C36 C36 H36A 119.4 7_565 . ? C35 C36 H36A 119.4 . . ? N10 C37 C37 117.3(6) . 7_565 ? N10 C37 C35 121.6(11) . . ? C37 C37 C35 121.1(7) 7_565 . ? N11 C38 Ru1 177.3(12) . . ? N12 C39 Ru1 177.8(16) . . ? N13 C40 Ru1 178.3(13) . . ? C12 N1 C1 116.4(9) . . ? C12 N1 Ru2 114.6(7) . . ? C1 N1 Ru2 128.9(8) . . ? C10 N2 C11 116.2(10) . . ? C10 N2 Ru2 129.4(8) . . ? C11 N2 Ru2 114.3(7) . . ? C14 N5 Pr1 144.7(8) . 6_557 ? C16 N6 Pr1 167.3(9) . . ? C27 N7 C31 118.7(12) . . ? C27 N7 Pr1 121.8(8) . . ? C31 N7 Pr1 119.3(10) . . ? C26 N8 C22 117.6(11) . . ? C26 N8 Pr1 121.3(8) . . ? C22 N8 Pr1 120.6(9) . . ? C17 N9 C21 118.6(11) . . ? C17 N9 Pr1 120.2(9) . . ? C21 N9 Pr1 120.8(8) . . ? C32 N10 C37 118.3(10) . . ? C32 N10 Ru1 128.1(8) . . ? C37 N10 Ru1 113.5(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.607 _refine_diff_density_min -1.891 _refine_diff_density_rms 0.208 #===END