# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Jared J. Paul' _publ_contact_author_address ;Department of Chemistry Villanova University 800 Lancaster Ave. Villanova, PA 19085 ; _publ_contact_author_email jared.paul@villanova.edu _publ_contact_author_phone 610-519-6220 _publ_contact_author_fax 610-519-7167 loop_ _publ_author_name _publ_author_address M.J.Fuentes ;Department of Chemistry Villanova University 800 Lancaster Ave. Villanova, PA 19085 ; R.J.Bognanno ;Department of Chemistry Villanova University 800 Lancaster Ave. Villanova, PA 19085 ; W.G.Dougherty ;Department of Chemistry Villanova University 800 Lancaster Ave. Villanova, PA 19085 ; W.S.Kassel ;Department of Chemistry Villanova University 800 Lancaster Ave. Villanova, PA 19085 ; T.J.Dudley ;Department of Chemistry Villanova University 800 Lancaster Ave. Villanova, PA 19085 ; ; J.J.Paul ; ;Department of Chemistry Villanova University 800 Lancaster Ave. Villanova, PA 19085 ; data_paul003s _database_code_depnum_ccdc_archive 'CCDC 871572' #TrackingRef '- paul003s.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H9 Cl0.33 N O1.50 Ru0.17' _chemical_formula_weight 159.81 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 12.7647(13) _cell_length_b 12.7647(13) _cell_length_c 16.2308(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2290.3(4) _cell_formula_units_Z 12 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 9927 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 33.05 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8947 _exptl_absorpt_correction_T_max 0.9036 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28899 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 33.15 _reflns_number_total 2922 _reflns_number_gt 2182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.002 984.7 223.1 _platon_squeeze_details ; Squeeze results consistent with a disordered molecule of diethylether solvent disordered about a 2-fold symmetry element. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _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^)+(0.0861P)^2^+0.7886P] 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 2922 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _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 0.3333 0.6667 0.7500 0.01854(13) Uani 1 6 d S . . Cl1 Cl 0.6667 0.3333 0.60641(7) 0.0300(2) Uani 1 3 d S . . N1 N 0.46278(17) 0.65167(16) 0.68303(9) 0.0200(3) Uani 1 1 d . . . O1 O 0.67926(18) 0.56302(19) 0.54361(11) 0.0369(5) Uani 1 1 d . . . H1A H 0.688(3) 0.507(3) 0.575(2) 0.035(8) Uiso 1 1 d . . . C1 C 0.4893(2) 0.56646(19) 0.71021(11) 0.0211(4) Uani 1 1 d . . . C2 C 0.5615(2) 0.5337(2) 0.66582(12) 0.0248(4) Uani 1 1 d . . . H2A H 0.5772 0.4730 0.6860 0.030 Uiso 1 1 calc R . . C3 C 0.6107(2) 0.5915(2) 0.59091(13) 0.0266(4) Uani 1 1 d . . . C4 C 0.5873(2) 0.6807(2) 0.56458(13) 0.0290(5) Uani 1 1 d . . . H4A H 0.6212 0.7227 0.5145 0.035 Uiso 1 1 calc R . . C5 C 0.5140(2) 0.7084(2) 0.61171(12) 0.0261(4) Uani 1 1 d . . . H5A H 0.4990 0.7703 0.5929 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02260(15) 0.02260(15) 0.01041(16) 0.000 0.000 0.01130(8) Cl1 0.0267(3) 0.0267(3) 0.0366(5) 0.000 0.000 0.01334(14) N1 0.0246(8) 0.0261(9) 0.0121(6) 0.0030(6) 0.0018(6) 0.0148(7) O1 0.0528(12) 0.0473(11) 0.0268(8) 0.0130(7) 0.0218(8) 0.0372(10) C1 0.0265(10) 0.0256(10) 0.0137(7) 0.0040(6) 0.0042(7) 0.0150(8) C2 0.0328(11) 0.0312(11) 0.0179(8) 0.0066(7) 0.0076(7) 0.0216(10) C3 0.0312(11) 0.0338(12) 0.0189(8) 0.0052(8) 0.0096(8) 0.0194(10) C4 0.0371(12) 0.0383(13) 0.0187(8) 0.0113(8) 0.0127(8) 0.0242(11) C5 0.0355(12) 0.0297(11) 0.0192(8) 0.0086(8) 0.0058(8) 0.0209(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 Ru1 N1 2.0651(18) 5_556 ? Ru1 N1 2.0651(18) 2_665 ? Ru1 N1 2.0651(18) 6_566 ? Ru1 N1 2.0651(18) 3_565 ? Ru1 N1 2.0651(18) 4_666 ? Ru1 N1 2.0651(18) . ? N1 C5 1.348(2) . ? N1 C1 1.364(3) . ? O1 C3 1.343(3) . ? O1 H1A 0.93(3) . ? C1 C2 1.390(3) . ? C1 C1 1.475(4) 4_666 ? C2 C3 1.398(3) . ? C2 H2A 0.9500 . ? C3 C4 1.382(3) . ? C4 C5 1.385(3) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? 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 N1 Ru1 N1 92.28(10) 5_556 2_665 ? N1 Ru1 N1 94.84(6) 5_556 6_566 ? N1 Ru1 N1 78.72(9) 2_665 6_566 ? N1 Ru1 N1 78.72(9) 5_556 3_565 ? N1 Ru1 N1 94.84(6) 2_665 3_565 ? N1 Ru1 N1 170.79(10) 6_566 3_565 ? N1 Ru1 N1 94.84(6) 5_556 4_666 ? N1 Ru1 N1 170.79(10) 2_665 4_666 ? N1 Ru1 N1 94.84(6) 6_566 4_666 ? N1 Ru1 N1 92.28(10) 3_565 4_666 ? N1 Ru1 N1 170.79(10) 5_556 . ? N1 Ru1 N1 94.84(6) 2_665 . ? N1 Ru1 N1 92.28(10) 6_566 . ? N1 Ru1 N1 94.84(6) 3_565 . ? N1 Ru1 N1 78.72(9) 4_666 . ? C5 N1 C1 117.34(18) . . ? C5 N1 Ru1 126.67(15) . . ? C1 N1 Ru1 115.64(12) . . ? C3 O1 H1A 104(2) . . ? N1 C1 C2 122.64(17) . . ? N1 C1 C1 114.57(10) . 4_666 ? C2 C1 C1 122.78(12) . 4_666 ? C1 C2 C3 118.8(2) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? O1 C3 C4 118.99(18) . . ? O1 C3 C2 122.4(2) . . ? C4 C3 C2 118.6(2) . . ? C5 C4 C3 119.49(19) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? N1 C5 C4 123.0(2) . . ? N1 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A Cl1 0.93(3) 2.15(3) 3.031(2) 156(3) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.153 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.110 # Attachment '- paul009.cif' data_paul009 _database_code_depnum_ccdc_archive 'CCDC 871573' #TrackingRef '- paul009.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H42 F12 N6 O7 P2 Ru' _chemical_formula_weight 1097.80 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6201(10) _cell_length_b 13.0428(11) _cell_length_c 14.8647(12) _cell_angle_alpha 76.681(3) _cell_angle_beta 83.234(3) _cell_angle_gamma 78.748(3) _cell_volume 2143.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9784 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 33.10 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9220 _exptl_absorpt_correction_T_max 0.9677 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 72892 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 33.21 _reflns_number_total 16295 _reflns_number_gt 12592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0463P)^2^+1.4536P] 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 16295 _refine_ls_number_parameters 676 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.034 _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 Ru1 Ru 0.261305(13) 0.178576(12) 0.198824(10) 0.01131(4) Uani 1 1 d . . . P1 P 0.66549(18) 0.32130(15) 0.33211(13) 0.0214(3) Uani 0.816(3) 1 d PDU A 1 F1 F 0.5905(3) 0.2301(3) 0.3472(3) 0.0716(11) Uani 0.816(3) 1 d PDU A 1 F2 F 0.5517(2) 0.4010(2) 0.3573(3) 0.0838(11) Uani 0.816(3) 1 d PDU A 1 F3 F 0.6930(2) 0.28882(17) 0.43931(13) 0.0440(6) Uani 0.816(3) 1 d PDU A 1 F4 F 0.7802(2) 0.2429(3) 0.3099(3) 0.0826(11) Uani 0.816(3) 1 d PDU A 1 F5 F 0.6430(4) 0.3524(3) 0.22567(18) 0.0734(10) Uani 0.816(3) 1 d PDU A 1 F6 F 0.7384(3) 0.4153(3) 0.31911(18) 0.0473(8) Uani 0.816(3) 1 d PDU A 1 P1' P 0.6568(11) 0.3222(10) 0.3236(8) 0.044(2) Uani 0.184(3) 1 d PDU A 2 F1' F 0.5850(13) 0.2429(11) 0.2996(12) 0.066(3) Uani 0.184(3) 1 d PDU A 2 F2' F 0.5691(12) 0.3229(11) 0.4110(8) 0.081(3) Uani 0.184(3) 1 d PDU A 2 F3' F 0.7396(11) 0.2276(12) 0.3787(12) 0.095(4) Uani 0.184(3) 1 d PDU A 2 F4' F 0.7383(13) 0.3184(10) 0.2327(9) 0.067(3) Uani 0.184(3) 1 d PDU A 2 F5' F 0.5688(11) 0.4137(9) 0.2630(11) 0.075(3) Uani 0.184(3) 1 d PDU A 2 F6' F 0.7010(18) 0.4190(14) 0.3392(12) 0.085(4) Uani 0.184(3) 1 d PDU A 2 P2 P 0.94273(5) 0.78343(4) 0.21042(4) 0.01945(11) Uani 1 1 d . . . F7 F 0.81784(16) 0.76759(17) 0.18746(15) 0.0575(5) Uani 1 1 d . . . F8 F 0.92257(17) 0.72193(14) 0.31501(10) 0.0455(4) Uani 1 1 d . . . F9 F 0.8825(2) 0.89339(14) 0.23717(13) 0.0570(5) Uani 1 1 d . . . F10 F 0.96352(15) 0.84317(13) 0.10435(10) 0.0373(4) Uani 1 1 d . . . F11 F 1.00110(19) 0.67258(13) 0.18279(12) 0.0504(5) Uani 1 1 d . . . F12 F 1.06660(17) 0.80042(18) 0.23131(14) 0.0592(6) Uani 1 1 d . . . N1 N 0.27317(14) 0.07804(12) 0.10819(11) 0.0129(3) Uani 1 1 d . . . N2 N 0.38313(14) 0.23713(12) 0.09833(11) 0.0128(3) Uani 1 1 d . . . N3 N 0.12323(14) 0.28648(12) 0.13885(11) 0.0126(3) Uani 1 1 d . . . N4 N 0.23892(14) 0.29565(13) 0.27489(11) 0.0126(3) Uani 1 1 d . . . N5 N 0.38492(14) 0.07120(12) 0.27651(11) 0.0123(3) Uani 1 1 d . . . N6 N 0.15669(14) 0.09350(13) 0.29864(11) 0.0128(3) Uani 1 1 d . . . O1 O 0.28234(13) -0.07110(12) -0.11037(10) 0.0205(3) Uani 1 1 d . . . O2 O 0.64457(14) 0.30992(12) -0.10777(11) 0.0222(3) Uani 1 1 d . . . O3 O -0.18140(13) 0.48884(12) 0.05048(10) 0.0208(3) Uani 1 1 d . . . O4 O 0.13258(14) 0.51595(12) 0.44101(10) 0.0219(3) Uani 1 1 d . . . O5 O 0.60354(12) -0.13311(12) 0.46509(10) 0.0195(3) Uani 1 1 d . . . O6 O -0.02889(13) -0.13035(12) 0.46109(11) 0.0210(3) Uani 1 1 d . . . C1 C 0.20867(17) 0.00137(15) 0.11517(13) 0.0156(4) Uani 1 1 d . . . H1A H 0.1618 -0.0173 0.1713 0.019 Uiso 1 1 calc R . . C2 C 0.20662(18) -0.05178(16) 0.04552(14) 0.0169(4) Uani 1 1 d . . . H2A H 0.1588 -0.1050 0.0532 0.020 Uiso 1 1 calc R . . C3 C 0.27624(17) -0.02587(15) -0.03646(13) 0.0152(3) Uani 1 1 d . . . C4 C 0.34673(17) 0.05124(15) -0.04435(13) 0.0151(3) Uani 1 1 d . . . H4A H 0.3965 0.0691 -0.0990 0.018 Uiso 1 1 calc R . . C5 C 0.34312(16) 0.10126(14) 0.02851(13) 0.0127(3) Uani 1 1 d . . . C6 C 0.41149(16) 0.18583(14) 0.02628(12) 0.0123(3) Uani 1 1 d . . . C7 C 0.49872(17) 0.21075(15) -0.04198(13) 0.0151(3) Uani 1 1 d . . . H7A H 0.5171 0.1731 -0.0909 0.018 Uiso 1 1 calc R . . C8 C 0.55986(17) 0.29168(15) -0.03877(13) 0.0154(3) Uani 1 1 d . . . C9 C 0.53225(18) 0.34369(16) 0.03454(14) 0.0168(4) Uani 1 1 d . . . H9A H 0.5727 0.3987 0.0391 0.020 Uiso 1 1 calc R . . C10 C 0.44420(18) 0.31340(16) 0.10088(13) 0.0163(4) Uani 1 1 d . . . H10A H 0.4260 0.3488 0.1512 0.020 Uiso 1 1 calc R . . C11 C 0.1975(2) -0.13739(19) -0.11000(16) 0.0263(5) Uani 1 1 d . . . H11A H 0.2073 -0.1612 -0.1688 0.039 Uiso 1 1 calc R . . H11B H 0.1180 -0.0965 -0.1024 0.039 Uiso 1 1 calc R . . H11C H 0.2091 -0.1998 -0.0586 0.039 Uiso 1 1 calc R . . C12 C 0.6987(2) 0.40087(19) -0.11591(17) 0.0279(5) Uani 1 1 d . . . H12A H 0.7630 0.4007 -0.1649 0.042 Uiso 1 1 calc R . . H12B H 0.7301 0.3983 -0.0569 0.042 Uiso 1 1 calc R . . H12C H 0.6403 0.4662 -0.1315 0.042 Uiso 1 1 calc R . . C13 C 0.07089(18) 0.27961(15) 0.06467(13) 0.0152(3) Uani 1 1 d . . . H13A H 0.1052 0.2253 0.0318 0.018 Uiso 1 1 calc R . . C14 C -0.02956(18) 0.34737(16) 0.03433(13) 0.0166(4) Uani 1 1 d . . . H14A H -0.0631 0.3402 -0.0187 0.020 Uiso 1 1 calc R . . C15 C -0.08182(17) 0.42684(16) 0.08243(13) 0.0157(4) Uani 1 1 d . . . C16 C -0.02757(17) 0.43716(15) 0.15762(13) 0.0152(3) Uani 1 1 d . . . H16A H -0.0600 0.4915 0.1909 0.018 Uiso 1 1 calc R . . C17 C 0.07469(17) 0.36658(14) 0.18313(12) 0.0130(3) Uani 1 1 d . . . C18 C 0.14059(17) 0.37212(15) 0.26062(12) 0.0131(3) Uani 1 1 d . . . C19 C 0.10686(18) 0.44736(15) 0.31481(13) 0.0157(3) Uani 1 1 d . . . H19A H 0.0381 0.4999 0.3032 0.019 Uiso 1 1 calc R . . C20 C 0.17458(18) 0.44562(16) 0.38683(13) 0.0167(4) Uani 1 1 d . . . C21 C 0.27905(18) 0.37209(16) 0.39765(14) 0.0172(4) Uani 1 1 d . . . H21A H 0.3301 0.3720 0.4431 0.021 Uiso 1 1 calc R . . C22 C 0.30669(18) 0.29942(16) 0.34068(13) 0.0162(4) Uani 1 1 d . . . H22A H 0.3778 0.2492 0.3486 0.019 Uiso 1 1 calc R . . C23 C -0.24192(19) 0.56666(18) 0.10244(15) 0.0223(4) Uani 1 1 d . . . H23A H -0.3138 0.6050 0.0731 0.033 Uiso 1 1 calc R . . H23B H -0.1906 0.6176 0.1036 0.033 Uiso 1 1 calc R . . H23C H -0.2626 0.5303 0.1660 0.033 Uiso 1 1 calc R . . C24 C 0.1882(2) 0.50128(19) 0.52570(15) 0.0258(5) Uani 1 1 d . . . H24A H 0.1449 0.5522 0.5622 0.039 Uiso 1 1 calc R . . H24B H 0.2695 0.5135 0.5110 0.039 Uiso 1 1 calc R . . H24C H 0.1879 0.4281 0.5615 0.039 Uiso 1 1 calc R . . C25 C 0.50205(17) 0.06533(16) 0.26264(13) 0.0160(4) Uani 1 1 d . . . H25A H 0.5323 0.1109 0.2094 0.019 Uiso 1 1 calc R . . C26 C 0.58098(17) -0.00268(16) 0.32079(13) 0.0167(4) Uani 1 1 d . . . H26A H 0.6633 -0.0052 0.3073 0.020 Uiso 1 1 calc R . . C27 C 0.53681(17) -0.06783(15) 0.40012(13) 0.0148(3) Uani 1 1 d . . . C28 C 0.41539(17) -0.06584(15) 0.41407(13) 0.0147(3) Uani 1 1 d . . . H28A H 0.3833 -0.1109 0.4668 0.018 Uiso 1 1 calc R . . C29 C 0.34299(16) 0.00193(15) 0.35081(13) 0.0130(3) Uani 1 1 d . . . C30 C 0.21414(16) 0.00839(15) 0.35652(12) 0.0127(3) Uani 1 1 d . . . C31 C 0.15716(17) -0.06963(15) 0.41326(13) 0.0146(3) Uani 1 1 d . . . H31A H 0.2002 -0.1293 0.4524 0.017 Uiso 1 1 calc R . . C32 C 0.03636(17) -0.05918(16) 0.41196(13) 0.0160(4) Uani 1 1 d . . . C33 C -0.02447(17) 0.03252(16) 0.35762(14) 0.0170(4) Uani 1 1 d . . . H33A H -0.1079 0.0442 0.3589 0.020 Uiso 1 1 calc R . . C34 C 0.03808(17) 0.10562(16) 0.30221(13) 0.0155(3) Uani 1 1 d . . . H34A H -0.0038 0.1675 0.2647 0.019 Uiso 1 1 calc R . . C35 C 0.72672(18) -0.12587(18) 0.45325(15) 0.0219(4) Uani 1 1 d . . . H35A H 0.7659 -0.1701 0.5075 0.033 Uiso 1 1 calc R . . H35B H 0.7356 -0.0513 0.4467 0.033 Uiso 1 1 calc R . . H35C H 0.7624 -0.1513 0.3975 0.033 Uiso 1 1 calc R . . C36 C 0.0317(2) -0.23486(17) 0.49995(17) 0.0260(5) Uani 1 1 d . . . H36A H -0.0257 -0.2820 0.5257 0.039 Uiso 1 1 calc R . . H36B H 0.0784 -0.2306 0.5493 0.039 Uiso 1 1 calc R . . H36C H 0.0839 -0.2636 0.4515 0.039 Uiso 1 1 calc R . . O7 O 0.4371(2) -0.17419(16) 0.24071(13) 0.0501(6) Uani 1 1 d . . . C37 C 0.5657(3) -0.3145(3) 0.3287(4) 0.0704(12) Uani 1 1 d . . . H37A H 0.6269 -0.2748 0.2956 0.106 Uiso 1 1 calc R . . H37B H 0.5828 -0.3874 0.3179 0.106 Uiso 1 1 calc R . . H37C H 0.5639 -0.3171 0.3953 0.106 Uiso 1 1 calc R . . C38 C 0.4492(3) -0.2599(2) 0.29438(18) 0.0356(6) Uani 1 1 d . . . C39 C 0.3464(3) -0.3142(3) 0.3318(2) 0.0436(7) Uani 1 1 d . . . H39A H 0.2772 -0.2759 0.2988 0.065 Uiso 1 1 calc R . . H39B H 0.3302 -0.3143 0.3980 0.065 Uiso 1 1 calc R . . H39C H 0.3643 -0.3881 0.3232 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01142(7) 0.01101(7) 0.01117(6) -0.00216(5) -0.00007(5) -0.00190(5) P1 0.0192(5) 0.0199(5) 0.0284(5) -0.0081(4) -0.0048(4) -0.0060(4) F1 0.070(2) 0.0467(16) 0.109(3) -0.0015(18) -0.034(2) -0.0383(15) F2 0.0434(15) 0.0564(18) 0.151(3) -0.043(2) -0.0079(18) 0.0183(13) F3 0.0657(16) 0.0418(12) 0.0251(9) 0.0016(8) -0.0032(9) -0.0216(11) F4 0.0476(16) 0.115(3) 0.087(2) -0.065(2) -0.0113(15) 0.0384(17) F5 0.115(3) 0.0737(19) 0.0462(14) -0.0065(13) -0.0507(17) -0.031(2) F6 0.0637(18) 0.0619(16) 0.0270(11) 0.0013(11) -0.0086(11) -0.0464(14) P1' 0.036(4) 0.045(3) 0.053(4) -0.017(3) -0.004(3) -0.007(3) F1' 0.045(6) 0.040(5) 0.120(10) -0.027(6) -0.001(6) -0.011(4) F2' 0.082(6) 0.066(6) 0.069(5) -0.002(4) 0.031(5) 0.012(5) F3' 0.047(6) 0.098(6) 0.105(7) 0.021(7) -0.013(5) 0.026(5) F4' 0.077(6) 0.067(6) 0.070(5) -0.041(4) 0.028(5) -0.031(5) F5' 0.075(6) 0.041(5) 0.090(7) 0.018(5) -0.013(5) 0.000(4) F6' 0.132(10) 0.078(6) 0.069(8) -0.048(6) 0.013(6) -0.051(6) P2 0.0214(3) 0.0190(2) 0.0187(2) -0.00491(19) -0.0008(2) -0.0046(2) F7 0.0371(10) 0.0679(13) 0.0683(13) 0.0029(10) -0.0124(9) -0.0267(9) F8 0.0663(12) 0.0396(9) 0.0218(7) 0.0017(6) 0.0070(7) -0.0044(8) F9 0.0884(16) 0.0317(9) 0.0461(10) -0.0161(8) -0.0048(10) 0.0106(9) F10 0.0433(9) 0.0412(9) 0.0221(7) 0.0044(6) -0.0005(6) -0.0092(7) F11 0.0807(14) 0.0290(8) 0.0354(9) -0.0113(7) -0.0029(9) 0.0095(9) F12 0.0407(10) 0.0778(14) 0.0630(12) 0.0022(11) -0.0232(9) -0.0288(10) N1 0.0126(7) 0.0113(7) 0.0144(7) -0.0025(5) 0.0002(5) -0.0022(6) N2 0.0136(7) 0.0119(7) 0.0123(7) -0.0022(5) -0.0004(5) -0.0019(6) N3 0.0131(7) 0.0117(7) 0.0124(7) -0.0014(5) -0.0017(5) -0.0019(6) N4 0.0127(7) 0.0129(7) 0.0122(6) -0.0029(5) -0.0006(5) -0.0024(6) N5 0.0109(7) 0.0118(7) 0.0141(7) -0.0027(5) 0.0000(5) -0.0019(6) N6 0.0115(7) 0.0139(7) 0.0127(7) -0.0033(5) 0.0002(5) -0.0017(6) O1 0.0230(8) 0.0232(7) 0.0205(7) -0.0120(6) 0.0036(6) -0.0111(6) O2 0.0230(8) 0.0225(7) 0.0239(7) -0.0080(6) 0.0089(6) -0.0134(6) O3 0.0184(7) 0.0206(7) 0.0225(7) -0.0050(6) -0.0090(6) 0.0038(6) O4 0.0297(9) 0.0190(7) 0.0182(7) -0.0100(6) -0.0075(6) 0.0032(6) O5 0.0108(6) 0.0224(7) 0.0212(7) 0.0047(6) -0.0035(5) -0.0030(5) O6 0.0121(7) 0.0183(7) 0.0291(8) 0.0030(6) 0.0000(6) -0.0049(5) C1 0.0159(9) 0.0133(8) 0.0168(8) -0.0023(7) 0.0019(7) -0.0038(7) C2 0.0168(9) 0.0148(8) 0.0205(9) -0.0047(7) 0.0007(7) -0.0061(7) C3 0.0147(9) 0.0141(8) 0.0178(8) -0.0059(7) -0.0005(7) -0.0023(7) C4 0.0145(9) 0.0152(8) 0.0160(8) -0.0047(7) 0.0014(7) -0.0036(7) C5 0.0121(8) 0.0107(8) 0.0146(8) -0.0024(6) -0.0003(6) -0.0017(6) C6 0.0119(8) 0.0116(8) 0.0134(7) -0.0021(6) -0.0006(6) -0.0026(6) C7 0.0158(9) 0.0152(8) 0.0147(8) -0.0035(7) 0.0019(7) -0.0053(7) C8 0.0146(9) 0.0154(8) 0.0161(8) -0.0022(7) 0.0010(7) -0.0050(7) C9 0.0181(9) 0.0150(8) 0.0187(9) -0.0030(7) -0.0003(7) -0.0073(7) C10 0.0191(9) 0.0152(8) 0.0156(8) -0.0039(7) -0.0002(7) -0.0050(7) C11 0.0280(12) 0.0289(11) 0.0289(11) -0.0126(9) 0.0005(9) -0.0157(10) C12 0.0284(12) 0.0277(11) 0.0317(11) -0.0083(9) 0.0077(9) -0.0185(10) C13 0.0172(9) 0.0147(8) 0.0141(8) -0.0039(7) -0.0012(7) -0.0026(7) C14 0.0184(9) 0.0175(9) 0.0150(8) -0.0036(7) -0.0040(7) -0.0037(7) C15 0.0130(9) 0.0161(9) 0.0169(8) -0.0010(7) -0.0033(7) -0.0018(7) C16 0.0157(9) 0.0144(8) 0.0152(8) -0.0031(7) -0.0014(7) -0.0018(7) C17 0.0155(9) 0.0110(8) 0.0121(7) -0.0009(6) -0.0015(6) -0.0027(6) C18 0.0130(8) 0.0132(8) 0.0129(7) -0.0013(6) -0.0017(6) -0.0028(6) C19 0.0174(9) 0.0142(8) 0.0151(8) -0.0038(7) -0.0024(7) -0.0005(7) C20 0.0214(10) 0.0145(8) 0.0150(8) -0.0042(7) -0.0018(7) -0.0036(7) C21 0.0183(9) 0.0186(9) 0.0164(8) -0.0046(7) -0.0049(7) -0.0040(7) C22 0.0153(9) 0.0180(9) 0.0151(8) -0.0029(7) -0.0034(7) -0.0014(7) C23 0.0175(10) 0.0219(10) 0.0252(10) -0.0059(8) -0.0035(8) 0.0044(8) C24 0.0370(13) 0.0257(11) 0.0165(9) -0.0089(8) -0.0081(9) -0.0012(10) C25 0.0133(9) 0.0165(9) 0.0164(8) -0.0011(7) 0.0025(7) -0.0036(7) C26 0.0114(8) 0.0193(9) 0.0184(9) -0.0022(7) 0.0004(7) -0.0034(7) C27 0.0118(8) 0.0154(8) 0.0169(8) -0.0029(7) -0.0020(6) -0.0017(7) C28 0.0134(8) 0.0151(8) 0.0151(8) -0.0017(7) 0.0000(6) -0.0037(7) C29 0.0120(8) 0.0125(8) 0.0147(8) -0.0038(6) 0.0006(6) -0.0028(6) C30 0.0104(8) 0.0151(8) 0.0126(7) -0.0040(6) 0.0001(6) -0.0019(6) C31 0.0131(8) 0.0134(8) 0.0164(8) -0.0015(7) -0.0008(6) -0.0027(7) C32 0.0133(9) 0.0164(9) 0.0175(8) -0.0017(7) 0.0007(7) -0.0043(7) C33 0.0106(8) 0.0200(9) 0.0191(9) -0.0015(7) -0.0001(7) -0.0028(7) C34 0.0118(8) 0.0154(8) 0.0181(8) -0.0028(7) -0.0008(7) -0.0007(7) C35 0.0104(9) 0.0278(11) 0.0241(10) 0.0016(8) -0.0033(7) -0.0024(8) C36 0.0184(10) 0.0185(10) 0.0363(12) 0.0055(9) -0.0020(9) -0.0053(8) O7 0.1012(19) 0.0325(10) 0.0231(9) -0.0122(8) -0.0007(10) -0.0223(12) C37 0.045(2) 0.047(2) 0.122(4) -0.031(2) -0.001(2) -0.0017(16) C38 0.0531(17) 0.0320(13) 0.0249(11) -0.0155(10) 0.0063(11) -0.0093(12) C39 0.0492(18) 0.0482(17) 0.0352(14) -0.0115(13) 0.0055(13) -0.0146(14) _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 N2 2.0534(15) . ? Ru1 N5 2.0540(16) . ? Ru1 N3 2.0560(16) . ? Ru1 N4 2.0613(16) . ? Ru1 N1 2.0623(16) . ? Ru1 N6 2.0624(15) . ? P1 F4 1.566(3) . ? P1 F1 1.569(3) . ? P1 F2 1.579(3) . ? P1 F5 1.580(3) . ? P1 F6 1.586(3) . ? P1 F3 1.605(3) . ? P1' F6' 1.525(13) . ? P1' F3' 1.541(13) . ? P1' F2' 1.554(13) . ? P1' F4' 1.562(13) . ? P1' F1' 1.571(13) . ? P1' F5' 1.589(13) . ? P2 F12 1.5744(18) . ? P2 F9 1.5843(18) . ? P2 F8 1.5900(16) . ? P2 F7 1.5910(18) . ? P2 F11 1.5950(17) . ? P2 F10 1.6029(15) . ? N1 C1 1.341(2) . ? N1 C5 1.364(2) . ? N2 C10 1.339(2) . ? N2 C6 1.365(2) . ? N3 C13 1.349(2) . ? N3 C17 1.357(2) . ? N4 C22 1.341(2) . ? N4 C18 1.364(2) . ? N5 C25 1.342(2) . ? N5 C29 1.363(2) . ? N6 C30 1.351(2) . ? N6 C34 1.352(2) . ? O1 C3 1.351(2) . ? O1 C11 1.431(2) . ? O2 C8 1.348(2) . ? O2 C12 1.423(2) . ? O3 C15 1.344(2) . ? O3 C23 1.441(3) . ? O4 C20 1.342(2) . ? O4 C24 1.439(3) . ? O5 C27 1.341(2) . ? O5 C35 1.440(2) . ? O6 C32 1.342(2) . ? O6 C36 1.430(3) . ? C1 C2 1.377(3) . ? C1 H1A 0.9500 . ? C2 C3 1.392(3) . ? C2 H2A 0.9500 . ? C3 C4 1.393(3) . ? C4 C5 1.380(3) . ? C4 H4A 0.9500 . ? C5 C6 1.472(2) . ? C6 C7 1.377(2) . ? C7 C8 1.395(3) . ? C7 H7A 0.9500 . ? C8 C9 1.387(3) . ? C9 C10 1.384(3) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.373(3) . ? C13 H13A 0.9500 . ? C14 C15 1.396(3) . ? C14 H14A 0.9500 . ? C15 C16 1.390(3) . ? C16 C17 1.386(3) . ? C16 H16A 0.9500 . ? C17 C18 1.479(3) . ? C18 C19 1.380(3) . ? C19 C20 1.395(3) . ? C19 H19A 0.9500 . ? C20 C21 1.393(3) . ? C21 C22 1.380(3) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.375(3) . ? C25 H25A 0.9500 . ? C26 C27 1.394(3) . ? C26 H26A 0.9500 . ? C27 C28 1.398(3) . ? C28 C29 1.374(3) . ? C28 H28A 0.9500 . ? C29 C30 1.477(3) . ? C30 C31 1.386(2) . ? C31 C32 1.386(3) . ? C31 H31A 0.9500 . ? C32 C33 1.394(3) . ? C33 C34 1.372(3) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O7 C38 1.208(3) . ? C37 C38 1.489(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.494(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 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 N2 Ru1 N5 94.20(6) . . ? N2 Ru1 N3 93.02(6) . . ? N5 Ru1 N3 171.74(6) . . ? N2 Ru1 N4 98.15(6) . . ? N5 Ru1 N4 96.92(6) . . ? N3 Ru1 N4 78.08(6) . . ? N2 Ru1 N1 78.70(6) . . ? N5 Ru1 N1 90.67(6) . . ? N3 Ru1 N1 94.66(6) . . ? N4 Ru1 N1 172.00(6) . . ? N2 Ru1 N6 169.80(6) . . ? N5 Ru1 N6 78.37(6) . . ? N3 Ru1 N6 94.93(6) . . ? N4 Ru1 N6 89.74(6) . . ? N1 Ru1 N6 94.28(6) . . ? F4 P1 F1 91.1(2) . . ? F4 P1 F2 178.1(2) . . ? F1 P1 F2 89.8(2) . . ? F4 P1 F5 89.5(2) . . ? F1 P1 F5 90.20(19) . . ? F2 P1 F5 92.1(2) . . ? F4 P1 F6 90.5(2) . . ? F1 P1 F6 178.2(2) . . ? F2 P1 F6 88.53(19) . . ? F5 P1 F6 90.70(17) . . ? F4 P1 F3 88.79(18) . . ? F1 P1 F3 90.73(17) . . ? F2 P1 F3 89.6(2) . . ? F5 P1 F3 178.1(2) . . ? F6 P1 F3 88.41(15) . . ? F6' P1' F3' 102.6(12) . . ? F6' P1' F2' 90.8(10) . . ? F3' P1' F2' 90.0(10) . . ? F6' P1' F4' 92.7(10) . . ? F3' P1' F4' 91.4(10) . . ? F2' P1' F4' 175.9(12) . . ? F6' P1' F1' 166.3(13) . . ? F3' P1' F1' 90.6(10) . . ? F2' P1' F1' 85.6(10) . . ? F4' P1' F1' 90.5(10) . . ? F6' P1' F5' 81.5(11) . . ? F3' P1' F5' 175.7(12) . . ? F2' P1' F5' 91.1(9) . . ? F4' P1' F5' 87.2(9) . . ? F1' P1' F5' 85.4(9) . . ? F12 P2 F9 90.65(12) . . ? F12 P2 F8 89.79(11) . . ? F9 P2 F8 90.53(10) . . ? F12 P2 F7 178.94(11) . . ? F9 P2 F7 89.24(12) . . ? F8 P2 F7 91.27(11) . . ? F12 P2 F11 90.40(12) . . ? F9 P2 F11 178.93(12) . . ? F8 P2 F11 89.65(9) . . ? F7 P2 F11 89.71(12) . . ? F12 P2 F10 90.52(10) . . ? F9 P2 F10 90.58(10) . . ? F8 P2 F10 178.85(10) . . ? F7 P2 F10 88.43(10) . . ? F11 P2 F10 89.24(9) . . ? C1 N1 C5 117.45(16) . . ? C1 N1 Ru1 126.18(13) . . ? C5 N1 Ru1 115.85(12) . . ? C10 N2 C6 117.35(16) . . ? C10 N2 Ru1 126.45(13) . . ? C6 N2 Ru1 115.91(12) . . ? C13 N3 C17 117.43(17) . . ? C13 N3 Ru1 125.93(13) . . ? C17 N3 Ru1 116.38(12) . . ? C22 N4 C18 117.51(17) . . ? C22 N4 Ru1 126.40(13) . . ? C18 N4 Ru1 115.92(12) . . ? C25 N5 C29 117.40(16) . . ? C25 N5 Ru1 126.17(12) . . ? C29 N5 Ru1 116.39(12) . . ? C30 N6 C34 117.69(16) . . ? C30 N6 Ru1 115.74(12) . . ? C34 N6 Ru1 125.80(13) . . ? C3 O1 C11 117.13(16) . . ? C8 O2 C12 118.15(17) . . ? C15 O3 C23 117.52(16) . . ? C20 O4 C24 116.99(17) . . ? C27 O5 C35 115.72(15) . . ? C32 O6 C36 117.41(16) . . ? N1 C1 C2 123.64(17) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C1 C2 C3 118.53(17) . . ? C1 C2 H2A 120.7 . . ? C3 C2 H2A 120.7 . . ? O1 C3 C2 124.81(17) . . ? O1 C3 C4 116.26(17) . . ? C2 C3 C4 118.93(18) . . ? C5 C4 C3 118.90(17) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 122.50(17) . . ? N1 C5 C6 114.22(16) . . ? C4 C5 C6 123.25(16) . . ? N2 C6 C7 122.15(17) . . ? N2 C6 C5 114.76(15) . . ? C7 C6 C5 123.08(17) . . ? C6 C7 C8 119.52(18) . . ? C6 C7 H7A 120.2 . . ? C8 C7 H7A 120.2 . . ? O2 C8 C9 125.73(17) . . ? O2 C8 C7 115.52(17) . . ? C9 C8 C7 118.72(17) . . ? C10 C9 C8 118.32(18) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? N2 C10 C9 123.92(18) . . ? N2 C10 H10A 118.0 . . ? C9 C10 H10A 118.0 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 123.15(18) . . ? N3 C13 H13A 118.4 . . ? C14 C13 H13A 118.4 . . ? C13 C14 C15 119.15(18) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? O3 C15 C16 125.18(19) . . ? O3 C15 C14 116.19(18) . . ? C16 C15 C14 118.62(18) . . ? C17 C16 C15 118.73(18) . . ? C17 C16 H16A 120.6 . . ? C15 C16 H16A 120.6 . . ? N3 C17 C16 122.83(17) . . ? N3 C17 C18 114.15(17) . . ? C16 C17 C18 123.02(17) . . ? N4 C18 C19 122.06(17) . . ? N4 C18 C17 114.22(16) . . ? C19 C18 C17 123.72(18) . . ? C18 C19 C20 119.46(19) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? O4 C20 C21 124.99(18) . . ? O4 C20 C19 116.50(18) . . ? C21 C20 C19 118.51(18) . . ? C22 C21 C20 118.42(18) . . ? C22 C21 H21A 120.8 . . ? C20 C21 H21A 120.8 . . ? N4 C22 C21 123.78(19) . . ? N4 C22 H22A 118.1 . . ? C21 C22 H22A 118.1 . . ? O3 C23 H23A 109.5 . . ? O3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O4 C24 H24A 109.5 . . ? O4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 123.99(17) . . ? N5 C25 H25A 118.0 . . ? C26 C25 H25A 118.0 . . ? C25 C26 C27 118.14(18) . . ? C25 C26 H26A 120.9 . . ? C27 C26 H26A 120.9 . . ? O5 C27 C26 124.18(18) . . ? O5 C27 C28 117.10(16) . . ? C26 C27 C28 118.72(18) . . ? C29 C28 C27 119.31(17) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? N5 C29 C28 122.19(17) . . ? N5 C29 C30 113.64(16) . . ? C28 C29 C30 124.16(16) . . ? N6 C30 C31 122.50(17) . . ? N6 C30 C29 114.75(15) . . ? C31 C30 C29 122.66(17) . . ? C32 C31 C30 118.91(18) . . ? C32 C31 H31A 120.5 . . ? C30 C31 H31A 120.5 . . ? O6 C32 C31 124.96(18) . . ? O6 C32 C33 116.27(17) . . ? C31 C32 C33 118.76(17) . . ? C34 C33 C32 118.93(18) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? N6 C34 C33 122.92(18) . . ? N6 C34 H34A 118.5 . . ? C33 C34 H34A 118.5 . . ? O5 C35 H35A 109.5 . . ? O5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O6 C36 H36A 109.5 . . ? O6 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O6 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O7 C38 C37 122.0(3) . . ? O7 C38 C39 121.1(3) . . ? C37 C38 C39 116.9(3) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.047 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.108