# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email xile.hu@epfl.ch _publ_contact_author_name 'Xile Hu' loop_ _publ_author_name 'Peng Ren' 'Oleg Vechorkin' 'Zsolt Csok' 'Isuf Salihu' 'Rosario Scopelliti' 'Xile Hu' data_ov-1039 _database_code_depnum_ccdc_archive 'CCDC 812106' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H20 Cl N3 Pd' _chemical_formula_sum 'C16 H20 Cl N3 Pd' _chemical_formula_weight 396.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' _symmetry_space_group_name_Hall 'P 4nw 2abw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 9.6434(10) _cell_length_b 9.6434(10) _cell_length_c 34.840(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3239.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 76 _cell_measurement_theta_min 3.081 _cell_measurement_theta_max 20.839 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7102 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS V2.10, G.M.Sheldrick, 2003' _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40537 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 26.01 _reflns_number_total 3140 _reflns_number_gt 2938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs, 1990-2000)' _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^)+(0.0120P)^2^+3.0041P] 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, 1195 Friedel pairs' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 3140 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 1.281 _refine_ls_restrained_S_all 1.281 _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 Pd1 Pd 0.20806(3) 0.56495(3) 0.062143(7) 0.01267(8) Uani 1 1 d . . . Cl1 Cl 0.25021(10) 0.63950(11) -0.00114(2) 0.0222(2) Uani 1 1 d . . . N1 N 0.3994(3) 0.6278(3) 0.08235(8) 0.0148(7) Uani 1 1 d . . . N2 N 0.1754(3) 0.5033(3) 0.11498(7) 0.0152(7) Uani 1 1 d . . . N3 N 0.0140(3) 0.4836(3) 0.05132(7) 0.0156(7) Uani 1 1 d . . . C1 C 0.4051(4) 0.5895(4) 0.12408(9) 0.0134(8) Uani 1 1 d . . . C2 C 0.5229(4) 0.6169(4) 0.14556(11) 0.0200(9) Uani 1 1 d . . . H2 H 0.5984 0.6652 0.1342 0.024 Uiso 1 1 calc R . . C3 C 0.5311(4) 0.5740(4) 0.18372(11) 0.0259(10) Uani 1 1 d . . . H3 H 0.6116 0.5927 0.1986 0.031 Uiso 1 1 calc R . . C4 C 0.4203(5) 0.5041(5) 0.19944(10) 0.0270(11) Uani 1 1 d . . . H4 H 0.4249 0.4744 0.2254 0.032 Uiso 1 1 calc R . . C5 C 0.3012(4) 0.4761(4) 0.17791(9) 0.0228(9) Uani 1 1 d . . . H5 H 0.2275 0.4257 0.1895 0.027 Uiso 1 1 calc R . . C6 C 0.2874(4) 0.5203(4) 0.13970(9) 0.0149(8) Uani 1 1 d . . . C7 C 0.0459(4) 0.4437(4) 0.12126(9) 0.0150(8) Uani 1 1 d . . . C8 C -0.0097(4) 0.3932(4) 0.15644(10) 0.0182(9) Uani 1 1 d . . . H8 H 0.0462 0.3940 0.1789 0.022 Uiso 1 1 calc R . . C9 C -0.1438(4) 0.3428(4) 0.15847(10) 0.0201(9) Uani 1 1 d . . . H9 H -0.1780 0.3098 0.1823 0.024 Uiso 1 1 calc R . . C10 C -0.2294(4) 0.3393(4) 0.12653(11) 0.0228(9) Uani 1 1 d . . . H10 H -0.3223 0.3072 0.1285 0.027 Uiso 1 1 calc R . . C11 C -0.1762(4) 0.3839(4) 0.09156(11) 0.0186(9) Uani 1 1 d . . . H11 H -0.2321 0.3786 0.0692 0.022 Uiso 1 1 calc R . . C12 C -0.0427(4) 0.4359(4) 0.08898(9) 0.0149(8) Uani 1 1 d . . . C13 C 0.5091(4) 0.5503(4) 0.06114(10) 0.0222(9) Uani 1 1 d . . . H13A H 0.6006 0.5793 0.0704 0.033 Uiso 1 1 calc R . . H13B H 0.5014 0.5701 0.0336 0.033 Uiso 1 1 calc R . . H13C H 0.4974 0.4506 0.0655 0.033 Uiso 1 1 calc R . . C14 C 0.4196(4) 0.7800(4) 0.07755(10) 0.0216(8) Uani 1 1 d . . . H14A H 0.3530 0.8298 0.0937 0.032 Uiso 1 1 calc R . . H14B H 0.4050 0.8052 0.0506 0.032 Uiso 1 1 calc R . . H14C H 0.5142 0.8050 0.0852 0.032 Uiso 1 1 calc R . . C15 C -0.0806(4) 0.5863(4) 0.03288(10) 0.0231(9) Uani 1 1 d . . . H15A H -0.1679 0.5407 0.0260 0.035 Uiso 1 1 calc R . . H15B H -0.0367 0.6234 0.0097 0.035 Uiso 1 1 calc R . . H15C H -0.0993 0.6622 0.0509 0.035 Uiso 1 1 calc R . . C16 C 0.0302(4) 0.3615(4) 0.02479(10) 0.0236(10) Uani 1 1 d . . . H16A H -0.0607 0.3193 0.0201 0.035 Uiso 1 1 calc R . . H16B H 0.0920 0.2930 0.0366 0.035 Uiso 1 1 calc R . . H16C H 0.0699 0.3927 0.0004 0.035 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 Pd1 0.01269(16) 0.01562(17) 0.00970(12) 0.00152(12) -0.00125(12) -0.00073(13) Cl1 0.0223(6) 0.0324(6) 0.0118(4) 0.0055(4) -0.0016(4) -0.0028(4) N1 0.0158(19) 0.0168(18) 0.0119(14) -0.0012(13) 0.0019(13) -0.0022(13) N2 0.0163(19) 0.0186(17) 0.0109(15) 0.0017(13) -0.0007(12) -0.0028(14) N3 0.0146(17) 0.0195(18) 0.0126(17) 0.0006(13) -0.0010(13) -0.0033(13) C1 0.017(2) 0.014(2) 0.0097(17) 0.0023(15) -0.0026(15) 0.0000(16) C2 0.016(2) 0.020(2) 0.024(2) 0.0002(17) -0.0017(17) -0.0043(17) C3 0.028(2) 0.028(2) 0.022(2) -0.002(2) -0.0114(18) 0.000(2) C4 0.041(3) 0.031(2) 0.0087(18) 0.0026(17) -0.0062(19) -0.010(2) C5 0.031(2) 0.024(2) 0.0140(18) 0.0027(15) -0.0046(17) -0.0103(19) C6 0.019(2) 0.011(2) 0.0149(17) -0.0024(14) -0.0027(17) -0.0012(16) C7 0.016(2) 0.0128(19) 0.0164(17) -0.0032(16) 0.0019(15) -0.0005(17) C8 0.022(2) 0.019(2) 0.0142(18) 0.0013(15) -0.0002(16) -0.0026(16) C9 0.023(2) 0.019(2) 0.0176(19) 0.0029(16) 0.0076(18) -0.0010(18) C10 0.018(2) 0.019(2) 0.032(2) 0.0000(18) 0.0067(18) -0.0058(17) C11 0.016(2) 0.015(2) 0.024(2) -0.0028(16) -0.0011(16) -0.0021(15) C12 0.017(2) 0.014(2) 0.0135(17) 0.0015(16) 0.0025(15) -0.0021(18) C13 0.014(2) 0.033(2) 0.0195(19) -0.003(2) 0.0018(18) 0.0020(18) C14 0.022(2) 0.018(2) 0.0243(19) 0.0028(17) -0.0024(17) -0.0106(18) C15 0.014(2) 0.034(3) 0.022(2) 0.0094(18) -0.0052(17) 0.0018(18) C16 0.025(3) 0.026(2) 0.020(2) -0.0047(18) 0.0014(17) -0.0046(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 Pd1 N2 1.960(3) . ? Pd1 N3 2.064(3) . ? Pd1 N1 2.066(3) . ? Pd1 Cl1 2.3544(10) . ? N1 C14 1.490(5) . ? N1 C13 1.491(5) . ? N1 C1 1.501(4) . ? N2 C6 1.391(4) . ? N2 C7 1.391(5) . ? N3 C15 1.491(5) . ? N3 C12 1.494(4) . ? N3 C16 1.505(5) . ? C1 C2 1.386(5) . ? C1 C6 1.425(5) . ? C2 C3 1.395(5) . ? C2 H2 0.9500 . ? C3 C4 1.377(6) . ? C3 H3 0.9500 . ? C4 C5 1.399(5) . ? C4 H4 0.9500 . ? C5 C6 1.404(5) . ? C5 H5 0.9500 . ? C7 C12 1.415(5) . ? C7 C8 1.424(5) . ? C8 C9 1.383(6) . ? C8 H8 0.9500 . ? C9 C10 1.386(5) . ? C9 H9 0.9500 . ? C10 C11 1.390(5) . ? C10 H10 0.9500 . ? C11 C12 1.384(5) . ? C11 H11 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 Pd1 N3 84.86(11) . . ? N2 Pd1 N1 84.99(11) . . ? N3 Pd1 N1 169.63(11) . . ? N2 Pd1 Cl1 179.29(9) . . ? N3 Pd1 Cl1 95.83(8) . . ? N1 Pd1 Cl1 94.32(8) . . ? C14 N1 C13 110.2(3) . . ? C14 N1 C1 110.3(3) . . ? C13 N1 C1 109.3(3) . . ? C14 N1 Pd1 111.6(2) . . ? C13 N1 Pd1 108.5(2) . . ? C1 N1 Pd1 106.9(2) . . ? C6 N2 C7 130.4(3) . . ? C6 N2 Pd1 114.9(2) . . ? C7 N2 Pd1 114.7(2) . . ? C15 N3 C12 111.1(3) . . ? C15 N3 C16 108.6(3) . . ? C12 N3 C16 109.7(3) . . ? C15 N3 Pd1 112.4(2) . . ? C12 N3 Pd1 106.8(2) . . ? C16 N3 Pd1 108.4(2) . . ? C2 C1 C6 122.4(3) . . ? C2 C1 N1 120.4(3) . . ? C6 C1 N1 117.2(3) . . ? C1 C2 C3 120.3(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 118.7(4) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 121.3(3) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 121.8(4) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? N2 C6 C5 128.7(3) . . ? N2 C6 C1 115.9(3) . . ? C5 C6 C1 115.4(4) . . ? N2 C7 C12 116.0(3) . . ? N2 C7 C8 127.9(3) . . ? C12 C7 C8 116.0(3) . . ? C9 C8 C7 121.1(3) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 121.6(3) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C9 C10 C11 118.4(4) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? C12 C11 C10 120.8(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C7 122.0(3) . . ? C11 C12 N3 120.6(3) . . ? C7 C12 N3 117.4(3) . . ? N1 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 N1 C14 -119.6(2) . . . . ? N3 Pd1 N1 C14 -131.5(7) . . . . ? Cl1 Pd1 N1 C14 60.5(2) . . . . ? N2 Pd1 N1 C13 118.8(2) . . . . ? N3 Pd1 N1 C13 106.9(7) . . . . ? Cl1 Pd1 N1 C13 -61.1(2) . . . . ? N2 Pd1 N1 C1 1.0(2) . . . . ? N3 Pd1 N1 C1 -10.9(8) . . . . ? Cl1 Pd1 N1 C1 -178.9(2) . . . . ? N3 Pd1 N2 C6 174.7(3) . . . . ? N1 Pd1 N2 C6 -3.2(3) . . . . ? N3 Pd1 N2 C7 -2.5(3) . . . . ? N1 Pd1 N2 C7 179.6(3) . . . . ? N2 Pd1 N3 C15 126.0(2) . . . . ? N1 Pd1 N3 C15 137.9(7) . . . . ? Cl1 Pd1 N3 C15 -54.1(2) . . . . ? N2 Pd1 N3 C12 4.0(2) . . . . ? N1 Pd1 N3 C12 15.9(8) . . . . ? Cl1 Pd1 N3 C12 -176.1(2) . . . . ? N2 Pd1 N3 C16 -114.0(2) . . . . ? N1 Pd1 N3 C16 -102.1(7) . . . . ? Cl1 Pd1 N3 C16 65.9(2) . . . . ? C14 N1 C1 C2 -59.6(5) . . . . ? C13 N1 C1 C2 61.7(4) . . . . ? Pd1 N1 C1 C2 179.0(3) . . . . ? C14 N1 C1 C6 122.7(3) . . . . ? C13 N1 C1 C6 -116.0(4) . . . . ? Pd1 N1 C1 C6 1.2(4) . . . . ? C6 C1 C2 C3 1.4(6) . . . . ? N1 C1 C2 C3 -176.2(3) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? C3 C4 C5 C6 -1.5(7) . . . . ? C7 N2 C6 C5 2.7(7) . . . . ? Pd1 N2 C6 C5 -174.0(3) . . . . ? C7 N2 C6 C1 -178.6(3) . . . . ? Pd1 N2 C6 C1 4.8(4) . . . . ? C4 C5 C6 N2 -178.5(4) . . . . ? C4 C5 C6 C1 2.8(6) . . . . ? C2 C1 C6 N2 178.4(3) . . . . ? N1 C1 C6 N2 -3.9(5) . . . . ? C2 C1 C6 C5 -2.7(5) . . . . ? N1 C1 C6 C5 175.0(3) . . . . ? C6 N2 C7 C12 -176.5(4) . . . . ? Pd1 N2 C7 C12 0.2(4) . . . . ? C6 N2 C7 C8 5.3(6) . . . . ? Pd1 N2 C7 C8 -178.0(3) . . . . ? N2 C7 C8 C9 176.7(4) . . . . ? C12 C7 C8 C9 -1.5(5) . . . . ? C7 C8 C9 C10 0.0(6) . . . . ? C8 C9 C10 C11 2.0(6) . . . . ? C9 C10 C11 C12 -2.6(6) . . . . ? C10 C11 C12 C7 1.2(6) . . . . ? C10 C11 C12 N3 180.0(3) . . . . ? N2 C7 C12 C11 -177.5(3) . . . . ? C8 C7 C12 C11 0.9(5) . . . . ? N2 C7 C12 N3 3.6(5) . . . . ? C8 C7 C12 N3 -178.0(3) . . . . ? C15 N3 C12 C11 53.0(4) . . . . ? C16 N3 C12 C11 -66.9(4) . . . . ? Pd1 N3 C12 C11 175.9(3) . . . . ? C15 N3 C12 C7 -128.1(4) . . . . ? C16 N3 C12 C7 111.9(4) . . . . ? Pd1 N3 C12 C7 -5.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.448 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.086 # Attachment '- 8.cif' data_ov-1040 _database_code_depnum_ccdc_archive 'CCDC 812107' #TrackingRef '- 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H20 F3 N3 O3 Pd S' _chemical_formula_sum 'C17 H20 F3 N3 O3 Pd S' _chemical_formula_weight 509.82 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' 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 7.0359(4) _cell_length_b 14.7010(8) _cell_length_c 19.4779(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2014.68(17) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 12379 _cell_measurement_theta_min 2.9560 _cell_measurement_theta_max 27.3750 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_T_min 0.81154 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction, KM4/Sapphire CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2812 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15442 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0085 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2143 _reflns_number_gt 2038 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _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^)+(0.0239P)^2^+1.4080P] 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 2143 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0185 _refine_ls_R_factor_gt 0.0171 _refine_ls_wR_factor_ref 0.0452 _refine_ls_wR_factor_gt 0.0446 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Pd1 Pd 0.22064(2) 0.2500 0.433532(8) 0.01350(6) Uani 1 2 d S . . S1 S -0.16516(9) 0.2500 0.53791(3) 0.02387(13) Uani 1 2 d S . . F1 F -0.3146(4) 0.2500 0.65961(12) 0.0776(7) Uani 1 2 d S . . F2 F -0.0521(3) 0.17706(10) 0.65295(7) 0.0627(4) Uani 1 1 d . . . O1 O 0.0353(2) 0.2500 0.51847(9) 0.0299(4) Uani 1 2 d S . . O2 O -0.2615(2) 0.16702(10) 0.52218(8) 0.0414(4) Uani 1 1 d . . . N1 N 0.23846(18) 0.11186(9) 0.42832(6) 0.0174(3) Uani 1 1 d . . . N2 N 0.4103(3) 0.2500 0.36163(9) 0.0161(3) Uani 1 2 d S . . C1 C 0.3943(2) 0.09061(10) 0.37999(7) 0.0161(3) Uani 1 1 d . . . C2 C 0.4475(2) 0.00127(10) 0.36907(8) 0.0195(3) Uani 1 1 d . . . H2 H 0.3841 -0.0464 0.3927 0.023 Uiso 1 1 calc R . . C3 C 0.5935(2) -0.01897(11) 0.32357(8) 0.0211(3) Uani 1 1 d . . . H3 H 0.6327 -0.0801 0.3163 0.025 Uiso 1 1 calc R . . C4 C 0.6802(2) 0.05175(11) 0.28911(8) 0.0219(3) Uani 1 1 d . . . H4 H 0.7798 0.0386 0.2577 0.026 Uiso 1 1 calc R . . C5 C 0.6262(2) 0.14147(11) 0.29900(8) 0.0213(3) Uani 1 1 d . . . H5 H 0.6879 0.1883 0.2739 0.026 Uiso 1 1 calc R . . C6 C 0.4812(2) 0.16418(10) 0.34580(7) 0.0153(3) Uani 1 1 d . . . C7 C 0.2816(3) 0.07556(12) 0.49815(8) 0.0267(4) Uani 1 1 d . . . H7A H 0.2918 0.0091 0.4961 0.040 Uiso 1 1 calc R . . H7B H 0.1793 0.0925 0.5298 0.040 Uiso 1 1 calc R . . H7C H 0.4020 0.1012 0.5144 0.040 Uiso 1 1 calc R . . C8 C 0.0562(2) 0.07351(12) 0.40216(10) 0.0292(4) Uani 1 1 d . . . H8A H 0.0312 0.0972 0.3560 0.044 Uiso 1 1 calc R . . H8B H -0.0478 0.0911 0.4329 0.044 Uiso 1 1 calc R . . H8C H 0.0653 0.0070 0.4004 0.044 Uiso 1 1 calc R . . C9 C -0.1429(5) 0.2500 0.63131(15) 0.0419(7) Uani 1 2 d S . . 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 Pd1 0.01167(9) 0.01467(9) 0.01415(9) 0.000 0.00264(5) 0.000 S1 0.0233(3) 0.0178(3) 0.0305(3) 0.000 0.0133(2) 0.000 F1 0.0817(16) 0.0932(17) 0.0579(13) 0.000 0.0546(12) 0.000 F2 0.0965(12) 0.0544(8) 0.0373(7) 0.0158(6) 0.0079(7) 0.0120(8) O1 0.0246(9) 0.0380(10) 0.0271(9) 0.000 0.0135(7) 0.000 O2 0.0406(8) 0.0305(7) 0.0531(9) -0.0049(7) 0.0131(7) -0.0131(6) N1 0.0182(6) 0.0164(6) 0.0177(6) 0.0000(5) 0.0048(5) -0.0020(5) N2 0.0144(8) 0.0173(8) 0.0165(8) 0.000 0.0044(7) 0.000 C1 0.0142(7) 0.0201(7) 0.0140(6) 0.0000(5) 0.0011(5) 0.0010(6) C2 0.0223(8) 0.0179(7) 0.0182(7) 0.0017(6) -0.0010(6) 0.0009(6) C3 0.0219(7) 0.0201(7) 0.0213(7) -0.0018(6) -0.0021(6) 0.0061(6) C4 0.0178(7) 0.0259(8) 0.0219(7) -0.0028(6) 0.0039(6) 0.0050(6) C5 0.0198(8) 0.0213(8) 0.0228(7) 0.0001(6) 0.0063(6) -0.0006(6) C6 0.0136(7) 0.0183(7) 0.0140(6) -0.0008(5) -0.0025(5) 0.0010(6) C7 0.0406(10) 0.0210(8) 0.0184(7) 0.0059(6) 0.0096(7) 0.0046(7) C8 0.0190(8) 0.0280(9) 0.0406(10) -0.0127(8) 0.0089(7) -0.0082(7) C9 0.0571(19) 0.0351(15) 0.0334(14) 0.000 0.0221(14) 0.000 _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 Pd1 N2 1.9344(17) . ? Pd1 N1 2.0371(14) 7_565 ? Pd1 N1 2.0372(14) . ? Pd1 O1 2.1067(16) . ? S1 O2 1.4288(14) 7_565 ? S1 O2 1.4288(14) . ? S1 O1 1.4600(18) . ? S1 C9 1.826(3) . ? F1 C9 1.328(4) . ? F2 C9 1.318(2) . ? N1 C1 1.4783(18) . ? N1 C8 1.491(2) . ? N1 C7 1.492(2) . ? N2 C6 1.3913(16) . ? N2 C6 1.3913(16) 7_565 ? C1 C2 1.382(2) . ? C1 C6 1.410(2) . ? C2 C3 1.389(2) . ? C2 H2 0.9500 . ? C3 C4 1.380(2) . ? C3 H3 0.9500 . ? C4 C5 1.386(2) . ? C4 H4 0.9500 . ? C5 C6 1.409(2) . ? C5 H5 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 F2 1.318(2) 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 N2 Pd1 N1 85.49(3) . 7_565 ? N2 Pd1 N1 85.49(3) . . ? N1 Pd1 N1 170.91(7) 7_565 . ? N2 Pd1 O1 174.64(7) . . ? N1 Pd1 O1 94.43(3) 7_565 . ? N1 Pd1 O1 94.43(3) . . ? O2 S1 O2 117.25(14) 7_565 . ? O2 S1 O1 113.74(7) 7_565 . ? O2 S1 O1 113.74(7) . . ? O2 S1 C9 104.73(9) 7_565 . ? O2 S1 C9 104.73(9) . . ? O1 S1 C9 100.12(13) . . ? S1 O1 Pd1 143.29(12) . . ? C1 N1 C8 109.90(12) . . ? C1 N1 C7 110.74(12) . . ? C8 N1 C7 110.56(13) . . ? C1 N1 Pd1 106.75(9) . . ? C8 N1 Pd1 109.95(10) . . ? C7 N1 Pd1 108.88(10) . . ? C6 N2 C6 130.16(18) . 7_565 ? C6 N2 Pd1 114.06(9) . . ? C6 N2 Pd1 114.06(9) 7_565 . ? C2 C1 C6 122.61(13) . . ? C2 C1 N1 119.98(13) . . ? C6 C1 N1 117.40(13) . . ? C1 C2 C3 120.14(14) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 118.43(14) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 121.89(14) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 120.93(14) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? N2 C6 C5 128.17(14) . . ? N2 C6 C1 115.83(13) . . ? C5 C6 C1 115.99(14) . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? F2 C9 F2 109.0(3) 7_565 . ? F2 C9 F1 107.96(17) 7_565 . ? F2 C9 F1 107.96(17) . . ? F2 C9 S1 111.12(14) 7_565 . ? F2 C9 S1 111.12(14) . . ? F1 C9 S1 109.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 O1 Pd1 -68.85(9) 7_565 . . . ? O2 S1 O1 Pd1 68.86(9) . . . . ? C9 S1 O1 Pd1 180.0 . . . . ? N1 Pd1 O1 S1 91.00(4) 7_565 . . . ? N1 Pd1 O1 S1 -91.00(4) . . . . ? N2 Pd1 N1 C1 5.72(10) . . . . ? O1 Pd1 N1 C1 -168.90(10) . . . . ? N2 Pd1 N1 C8 -113.44(11) . . . . ? O1 Pd1 N1 C8 71.94(11) . . . . ? N2 Pd1 N1 C7 125.31(11) . . . . ? O1 Pd1 N1 C7 -49.32(11) . . . . ? N1 Pd1 N2 C6 172.71(13) 7_565 . . . ? N1 Pd1 N2 C6 -6.13(12) . . . . ? N1 Pd1 N2 C6 6.13(12) 7_565 . . 7_565 ? N1 Pd1 N2 C6 -172.71(13) . . . 7_565 ? C8 N1 C1 C2 -64.63(18) . . . . ? C7 N1 C1 C2 57.81(18) . . . . ? Pd1 N1 C1 C2 176.18(12) . . . . ? C8 N1 C1 C6 114.43(15) . . . . ? C7 N1 C1 C6 -123.13(15) . . . . ? Pd1 N1 C1 C6 -4.77(15) . . . . ? C6 C1 C2 C3 0.8(2) . . . . ? N1 C1 C2 C3 179.83(13) . . . . ? C1 C2 C3 C4 -1.2(2) . . . . ? C2 C3 C4 C5 0.3(2) . . . . ? C3 C4 C5 C6 0.9(2) . . . . ? C6 N2 C6 C5 -12.5(3) 7_565 . . . ? Pd1 N2 C6 C5 -176.35(13) . . . . ? C6 N2 C6 C1 168.87(14) 7_565 . . . ? Pd1 N2 C6 C1 4.97(19) . . . . ? C4 C5 C6 N2 -179.91(16) . . . . ? C4 C5 C6 C1 -1.2(2) . . . . ? C2 C1 C6 N2 179.22(15) . . . . ? N1 C1 C6 N2 0.2(2) . . . . ? C2 C1 C6 C5 0.4(2) . . . . ? N1 C1 C6 C5 -178.65(13) . . . . ? O2 S1 C9 F2 -57.3(2) 7_565 . . 7_565 ? O2 S1 C9 F2 178.77(18) . . . 7_565 ? O1 S1 C9 F2 60.75(19) . . . 7_565 ? O2 S1 C9 F2 -178.77(18) 7_565 . . . ? O2 S1 C9 F2 57.3(2) . . . . ? O1 S1 C9 F2 -60.75(19) . . . . ? O2 S1 C9 F1 61.98(7) 7_565 . . . ? O2 S1 C9 F1 -61.98(7) . . . . ? O1 S1 C9 F1 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.306 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.055 # Attachment '- 9.cif' data_cz1028b _database_code_depnum_ccdc_archive 'CCDC 812108' #TrackingRef '- 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H20 Cl N3 Pt' _chemical_formula_sum 'C16 H20 Cl N3 Pt' _chemical_formula_weight 484.89 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' _symmetry_space_group_name_Hall 'P 4nw 2abw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 9.63408(10) _cell_length_b 9.63408(10) _cell_length_c 34.6217(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3213.43(7) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 15781 _cell_measurement_theta_min 2.9359 _cell_measurement_theta_max 27.5250 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 8.896 _exptl_absorpt_correction_T_min 0.74234 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction, KM4/Sapphire CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2812 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29193 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3261 _reflns_number_gt 2995 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _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^)+(0.0167P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 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 -0.004(7) _refine_ls_number_reflns 3261 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0177 _refine_ls_wR_factor_ref 0.0318 _refine_ls_wR_factor_gt 0.0313 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 Pt1 Pt 0.209691(14) 0.563766(15) 0.062231(4) 0.01535(4) Uani 1 1 d . . . Cl1 Cl 0.25242(11) 0.63924(12) -0.00083(3) 0.0274(3) Uani 1 1 d . . . N1 N 0.3994(3) 0.6262(3) 0.08266(8) 0.0173(7) Uani 1 1 d . . . N2 N 0.1758(3) 0.5001(3) 0.11516(8) 0.0172(7) Uani 1 1 d . . . N3 N 0.0168(3) 0.4841(3) 0.05101(8) 0.0192(8) Uani 1 1 d . . . C1 C 0.4041(4) 0.5863(4) 0.12426(10) 0.0188(9) Uani 1 1 d . . . C2 C 0.5213(4) 0.6141(4) 0.14610(11) 0.0232(10) Uani 1 1 d . . . H2 H 0.5967 0.6631 0.1348 0.028 Uiso 1 1 calc R . . C3 C 0.5296(4) 0.5710(4) 0.18422(13) 0.0309(10) Uani 1 1 d . . . H3 H 0.6100 0.5891 0.1993 0.037 Uiso 1 1 calc R . . C4 C 0.4182(5) 0.5013(5) 0.19962(11) 0.0282(10) Uani 1 1 d . . . H4 H 0.4228 0.4701 0.2256 0.034 Uiso 1 1 calc R . . C5 C 0.2998(4) 0.4755(4) 0.17832(11) 0.0272(10) Uani 1 1 d . . . H5 H 0.2251 0.4268 0.1901 0.033 Uiso 1 1 calc R . . C6 C 0.2868(4) 0.5188(4) 0.14003(10) 0.0173(8) Uani 1 1 d . . . C7 C 0.0461(4) 0.4425(4) 0.12136(10) 0.0169(8) Uani 1 1 d . . . C8 C -0.0098(4) 0.3922(4) 0.15604(11) 0.0207(9) Uani 1 1 d . . . H8 H 0.0455 0.3923 0.1788 0.025 Uiso 1 1 calc R . . C9 C -0.1435(4) 0.3427(4) 0.15760(12) 0.0250(10) Uani 1 1 d . . . H9 H -0.1785 0.3094 0.1815 0.030 Uiso 1 1 calc R . . C10 C -0.2282(4) 0.3399(4) 0.12558(12) 0.0253(10) Uani 1 1 d . . . H10 H -0.3214 0.3083 0.1273 0.030 Uiso 1 1 calc R . . C11 C -0.1738(4) 0.3844(4) 0.09097(12) 0.0243(9) Uani 1 1 d . . . H11 H -0.2291 0.3794 0.0683 0.029 Uiso 1 1 calc R . . C12 C -0.0411(4) 0.4359(4) 0.08854(10) 0.0173(8) Uani 1 1 d . . . C13 C 0.5121(4) 0.5520(5) 0.06163(12) 0.0269(9) Uani 1 1 d . . . H13A H 0.6025 0.5845 0.0710 0.040 Uiso 1 1 calc R . . H13B H 0.5042 0.5709 0.0339 0.040 Uiso 1 1 calc R . . H13C H 0.5038 0.4520 0.0662 0.040 Uiso 1 1 calc R . . C14 C 0.4204(4) 0.7796(4) 0.07826(11) 0.0247(9) Uani 1 1 d . . . H14A H 0.3531 0.8293 0.0944 0.037 Uiso 1 1 calc R . . H14B H 0.4072 0.8058 0.0512 0.037 Uiso 1 1 calc R . . H14C H 0.5148 0.8041 0.0864 0.037 Uiso 1 1 calc R . . C15 C -0.0775(4) 0.5887(4) 0.03296(12) 0.0283(10) Uani 1 1 d . . . H15A H -0.1655 0.5442 0.0261 0.042 Uiso 1 1 calc R . . H15B H -0.0338 0.6265 0.0097 0.042 Uiso 1 1 calc R . . H15C H -0.0950 0.6641 0.0513 0.042 Uiso 1 1 calc R . . C16 C 0.0296(4) 0.3618(4) 0.02398(11) 0.0280(10) Uani 1 1 d . . . H16A H -0.0626 0.3221 0.0193 0.042 Uiso 1 1 calc R . . H16B H 0.0896 0.2912 0.0357 0.042 Uiso 1 1 calc R . . H16C H 0.0700 0.3925 -0.0006 0.042 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 Pt1 0.01548(8) 0.01829(8) 0.01227(6) 0.00153(7) -0.00103(7) -0.00037(7) Cl1 0.0285(6) 0.0385(6) 0.0153(5) 0.0072(4) -0.0012(4) -0.0039(5) N1 0.0139(17) 0.0252(19) 0.0128(16) -0.0005(15) 0.0010(14) -0.0025(13) N2 0.0214(19) 0.0213(17) 0.0091(15) 0.0037(14) 0.0037(13) -0.0029(14) N3 0.0168(17) 0.0261(19) 0.015(2) -0.0007(14) -0.0032(14) -0.0040(14) C1 0.023(2) 0.018(2) 0.016(2) 0.0026(17) -0.0025(17) -0.0016(17) C2 0.018(2) 0.028(2) 0.023(2) -0.0010(18) -0.0049(18) -0.0036(17) C3 0.030(2) 0.034(2) 0.028(2) -0.005(2) -0.014(2) -0.001(2) C4 0.040(3) 0.033(2) 0.012(2) 0.0042(18) -0.009(2) -0.008(2) C5 0.031(2) 0.030(2) 0.021(2) 0.0043(17) -0.0051(19) -0.0130(19) C6 0.020(2) 0.0149(19) 0.0169(19) -0.0039(15) -0.0048(18) 0.0001(16) C7 0.022(2) 0.0115(17) 0.0172(19) -0.0006(16) -0.0010(16) 0.0018(18) C8 0.026(2) 0.017(2) 0.019(2) 0.0027(16) -0.0002(17) -0.0014(17) C9 0.032(2) 0.021(2) 0.022(2) 0.0033(19) 0.015(2) -0.0050(19) C10 0.017(2) 0.024(2) 0.035(3) 0.000(2) 0.005(2) -0.0063(18) C11 0.022(2) 0.025(2) 0.026(2) -0.0067(19) -0.0037(19) 0.0005(17) C12 0.018(2) 0.0166(19) 0.017(2) 0.0012(17) 0.0003(16) 0.0002(19) C13 0.0169(19) 0.042(3) 0.021(2) -0.001(3) 0.003(2) 0.0053(19) C14 0.028(2) 0.019(2) 0.027(2) 0.0033(18) -0.0033(19) -0.0108(19) C15 0.020(2) 0.037(3) 0.028(2) 0.008(2) -0.0066(19) 0.0023(19) C16 0.027(3) 0.034(3) 0.023(2) -0.010(2) -0.0025(19) -0.0084(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 1.960(3) . ? Pt1 N3 2.048(3) . ? Pt1 N1 2.050(3) . ? Pt1 Cl1 2.3378(10) . ? N1 C13 1.490(5) . ? N1 C1 1.491(4) . ? N1 C14 1.500(4) . ? N2 C6 1.384(4) . ? N2 C7 1.384(5) . ? N3 C12 1.489(5) . ? N3 C15 1.494(5) . ? N3 C16 1.510(5) . ? C1 C2 1.384(5) . ? C1 C6 1.414(5) . ? C2 C3 1.386(6) . ? C2 H2 0.9500 . ? C3 C4 1.373(5) . ? C3 H3 0.9500 . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? C5 C6 1.396(5) . ? C5 H5 0.9500 . ? C7 C8 1.402(5) . ? C7 C12 1.414(5) . ? C8 C9 1.375(6) . ? C8 H8 0.9500 . ? C9 C10 1.377(6) . ? C9 H9 0.9500 . ? C10 C11 1.377(5) . ? C10 H10 0.9500 . ? C11 C12 1.374(5) . ? C11 H11 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 Pt1 N3 84.79(12) . . ? N2 Pt1 N1 85.26(12) . . ? N3 Pt1 N1 169.90(12) . . ? N2 Pt1 Cl1 179.43(9) . . ? N3 Pt1 Cl1 95.68(9) . . ? N1 Pt1 Cl1 94.25(8) . . ? C13 N1 C1 109.0(3) . . ? C13 N1 C14 108.9(3) . . ? C1 N1 C14 110.3(3) . . ? C13 N1 Pt1 109.9(2) . . ? C1 N1 Pt1 106.6(2) . . ? C14 N1 Pt1 112.0(2) . . ? C6 N2 C7 130.8(3) . . ? C6 N2 Pt1 114.4(2) . . ? C7 N2 Pt1 114.9(2) . . ? C12 N3 C15 110.4(3) . . ? C12 N3 C16 109.1(3) . . ? C15 N3 C16 108.5(3) . . ? C12 N3 Pt1 106.9(2) . . ? C15 N3 Pt1 112.2(2) . . ? C16 N3 Pt1 109.6(2) . . ? C2 C1 C6 122.0(3) . . ? C2 C1 N1 120.2(3) . . ? C6 C1 N1 117.8(3) . . ? C1 C2 C3 120.6(4) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 118.1(4) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 121.7(4) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 121.8(4) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? N2 C6 C5 128.4(3) . . ? N2 C6 C1 115.9(3) . . ? C5 C6 C1 115.6(4) . . ? N2 C7 C8 128.2(3) . . ? N2 C7 C12 115.5(3) . . ? C8 C7 C12 116.4(3) . . ? C9 C8 C7 120.9(4) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 122.1(4) . . ? C8 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C11 C10 C9 117.9(4) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? C12 C11 C10 121.4(4) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C7 121.3(3) . . ? C11 C12 N3 121.0(3) . . ? C7 C12 N3 117.7(3) . . ? N1 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pt1 N1 C13 119.1(3) . . . . ? N3 Pt1 N1 C13 109.1(7) . . . . ? Cl1 Pt1 N1 C13 -60.6(2) . . . . ? N2 Pt1 N1 C1 1.1(2) . . . . ? N3 Pt1 N1 C1 -8.9(9) . . . . ? Cl1 Pt1 N1 C1 -178.6(2) . . . . ? N2 Pt1 N1 C14 -119.6(2) . . . . ? N3 Pt1 N1 C14 -129.7(7) . . . . ? Cl1 Pt1 N1 C14 60.6(2) . . . . ? N3 Pt1 N2 C6 176.0(3) . . . . ? N1 Pt1 N2 C6 -2.3(3) . . . . ? N3 Pt1 N2 C7 -3.3(3) . . . . ? N1 Pt1 N2 C7 178.5(3) . . . . ? N2 Pt1 N3 C12 4.3(2) . . . . ? N1 Pt1 N3 C12 14.4(9) . . . . ? Cl1 Pt1 N3 C12 -176.0(2) . . . . ? N2 Pt1 N3 C15 125.5(3) . . . . ? N1 Pt1 N3 C15 135.6(7) . . . . ? Cl1 Pt1 N3 C15 -54.8(2) . . . . ? N2 Pt1 N3 C16 -113.8(3) . . . . ? N1 Pt1 N3 C16 -103.8(7) . . . . ? Cl1 Pt1 N3 C16 65.8(2) . . . . ? C13 N1 C1 C2 60.8(4) . . . . ? C14 N1 C1 C2 -58.8(5) . . . . ? Pt1 N1 C1 C2 179.4(3) . . . . ? C13 N1 C1 C6 -118.5(4) . . . . ? C14 N1 C1 C6 121.9(4) . . . . ? Pt1 N1 C1 C6 0.1(4) . . . . ? C6 C1 C2 C3 2.6(6) . . . . ? N1 C1 C2 C3 -176.6(4) . . . . ? C1 C2 C3 C4 -0.5(6) . . . . ? C2 C3 C4 C5 -0.8(7) . . . . ? C3 C4 C5 C6 -0.1(7) . . . . ? C7 N2 C6 C5 4.4(7) . . . . ? Pt1 N2 C6 C5 -174.6(3) . . . . ? C7 N2 C6 C1 -178.0(4) . . . . ? Pt1 N2 C6 C1 2.9(4) . . . . ? C4 C5 C6 N2 179.7(4) . . . . ? C4 C5 C6 C1 2.1(6) . . . . ? C2 C1 C6 N2 178.8(4) . . . . ? N1 C1 C6 N2 -2.0(5) . . . . ? C2 C1 C6 C5 -3.3(6) . . . . ? N1 C1 C6 C5 175.9(3) . . . . ? C6 N2 C7 C8 3.1(7) . . . . ? Pt1 N2 C7 C8 -177.8(3) . . . . ? C6 N2 C7 C12 -177.9(4) . . . . ? Pt1 N2 C7 C12 1.1(4) . . . . ? N2 C7 C8 C9 177.4(4) . . . . ? C12 C7 C8 C9 -1.5(5) . . . . ? C7 C8 C9 C10 0.1(6) . . . . ? C8 C9 C10 C11 2.1(6) . . . . ? C9 C10 C11 C12 -2.8(6) . . . . ? C10 C11 C12 C7 1.4(6) . . . . ? C10 C11 C12 N3 -179.8(3) . . . . ? N2 C7 C12 C11 -178.3(3) . . . . ? C8 C7 C12 C11 0.8(5) . . . . ? N2 C7 C12 N3 2.9(5) . . . . ? C8 C7 C12 N3 -178.0(3) . . . . ? C15 N3 C12 C11 53.7(5) . . . . ? C16 N3 C12 C11 -65.4(4) . . . . ? Pt1 N3 C12 C11 176.1(3) . . . . ? C15 N3 C12 C7 -127.5(4) . . . . ? C16 N3 C12 C7 113.4(4) . . . . ? Pt1 N3 C12 C7 -5.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.738 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.083 # Attachment '- 10.cif' data_rp200573 _database_code_depnum_ccdc_archive 'CCDC 812109' #TrackingRef '- 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H35 Cl N3 P Ru' _chemical_formula_sum 'C34 H35 Cl N3 P Ru' _chemical_formula_weight 653.14 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' P P 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.0619(8) _cell_length_b 17.4995(5) _cell_length_c 19.9241(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.823(5) _cell_angle_gamma 90.00 _cell_volume 5886.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 11843 _cell_measurement_theta_min 2.8435 _cell_measurement_theta_max 27.4570 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_T_min 0.93585 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction, KM4/Sapphire CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2812 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52434 _diffrn_reflns_av_R_equivalents 0.0999 _diffrn_reflns_av_sigmaI/netI 0.1267 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11960 _reflns_number_gt 6807 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _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^)+(0.0174P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11960 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 0.813 _refine_ls_restrained_S_all 0.813 _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 0.337644(17) 0.289007(16) 0.346686(15) 0.01365(7) Uani 1 1 d . . . Cl1 Cl 0.36628(5) 0.29947(5) 0.47453(4) 0.0246(2) Uani 1 1 d . . . P1 P 0.34366(5) 0.16573(5) 0.33437(5) 0.0140(2) Uani 1 1 d . . . N1 N 0.45234(15) 0.32602(15) 0.35223(15) 0.0157(7) Uani 1 1 d . . . N2 N 0.31339(16) 0.31635(15) 0.24407(14) 0.0153(7) Uani 1 1 d . . . N3 N 0.21340(16) 0.30489(15) 0.31619(15) 0.0186(7) Uani 1 1 d . . . C1 C 0.4535(2) 0.32184(18) 0.27903(18) 0.0143(8) Uani 1 1 d . . . C2 C 0.5232(2) 0.3232(2) 0.2657(2) 0.0254(9) Uani 1 1 d . . . H2 H 0.5723 0.3272 0.3046 0.031 Uiso 1 1 calc R . . C3 C 0.5225(2) 0.3188(2) 0.1966(2) 0.0336(11) Uani 1 1 d . . . H3 H 0.5707 0.3202 0.1876 0.040 Uiso 1 1 calc R . . C4 C 0.4513(3) 0.3123(2) 0.1407(2) 0.0347(11) Uani 1 1 d . . . H4 H 0.4507 0.3077 0.0930 0.042 Uiso 1 1 calc R . . C5 C 0.3805(2) 0.3125(2) 0.15273(19) 0.0245(9) Uani 1 1 d . . . H5 H 0.3321 0.3083 0.1131 0.029 Uiso 1 1 calc R . . C6 C 0.3787(2) 0.31851(19) 0.22194(19) 0.0191(9) Uani 1 1 d . . . C7 C 0.2337(2) 0.31830(18) 0.20120(19) 0.0178(9) Uani 1 1 d . . . C8 C 0.2004(2) 0.3348(2) 0.12789(19) 0.0268(10) Uani 1 1 d . . . H8 H 0.2339 0.3498 0.1027 0.032 Uiso 1 1 calc R . . C9 C 0.1201(3) 0.3299(2) 0.0915(2) 0.0376(11) Uani 1 1 d . . . H9 H 0.0996 0.3399 0.0414 0.045 Uiso 1 1 calc R . . C10 C 0.0690(2) 0.3108(2) 0.1259(2) 0.0389(12) Uani 1 1 d . . . H10 H 0.0139 0.3050 0.0996 0.047 Uiso 1 1 calc R . . C11 C 0.0989(2) 0.3003(2) 0.1992(2) 0.0291(10) Uani 1 1 d . . . H11 H 0.0639 0.2896 0.2241 0.035 Uiso 1 1 calc R . . C12 C 0.1797(2) 0.30526(18) 0.23700(19) 0.0184(9) Uani 1 1 d . . . C13 C 0.4472(2) 0.40851(18) 0.36991(18) 0.0213(9) Uani 1 1 d . . . H13A H 0.4932 0.4360 0.3668 0.032 Uiso 1 1 calc R . . H13B H 0.4466 0.4129 0.4187 0.032 Uiso 1 1 calc R . . H13C H 0.3985 0.4306 0.3358 0.032 Uiso 1 1 calc R . . C14 C 0.52519(19) 0.2947(2) 0.40681(17) 0.0227(9) Uani 1 1 d . . . H14A H 0.5342 0.2426 0.3933 0.034 Uiso 1 1 calc R . . H14B H 0.5190 0.2939 0.4537 0.034 Uiso 1 1 calc R . . H14C H 0.5705 0.3269 0.4094 0.034 Uiso 1 1 calc R . . C15 C 0.1651(2) 0.2596(2) 0.34936(19) 0.0265(10) Uani 1 1 d . . . H15A H 0.1120 0.2819 0.3357 0.040 Uiso 1 1 calc R . . H15B H 0.1906 0.2607 0.4018 0.040 Uiso 1 1 calc R . . H15C H 0.1609 0.2067 0.3324 0.040 Uiso 1 1 calc R . . C16 C 0.21356(19) 0.38595(18) 0.34011(18) 0.0220(9) Uani 1 1 d . . . H16A H 0.2460 0.4171 0.3203 0.033 Uiso 1 1 calc R . . H16B H 0.2356 0.3883 0.3927 0.033 Uiso 1 1 calc R . . H16C H 0.1592 0.4056 0.3230 0.033 Uiso 1 1 calc R . . C17 C 0.28365(19) 0.10126(18) 0.36815(18) 0.0143(8) Uani 1 1 d . . . C18 C 0.27250(19) 0.1179(2) 0.43204(17) 0.0174(8) Uani 1 1 d . . . H18 H 0.2904 0.1653 0.4553 0.021 Uiso 1 1 calc R . . C19 C 0.2356(2) 0.0661(2) 0.46220(18) 0.0206(9) Uani 1 1 d . . . H19 H 0.2289 0.0783 0.5061 0.025 Uiso 1 1 calc R . . C20 C 0.20849(19) -0.0028(2) 0.42958(19) 0.0187(9) Uani 1 1 d . . . H20 H 0.1825 -0.0378 0.4503 0.022 Uiso 1 1 calc R . . C21 C 0.2196(2) -0.0204(2) 0.36643(19) 0.0237(9) Uani 1 1 d . . . H21 H 0.2013 -0.0679 0.3435 0.028 Uiso 1 1 calc R . . C22 C 0.2570(2) 0.03066(19) 0.33612(18) 0.0200(9) Uani 1 1 d . . . H22 H 0.2647 0.0175 0.2928 0.024 Uiso 1 1 calc R . . C23 C 0.43769(19) 0.11473(19) 0.38009(19) 0.0183(9) Uani 1 1 d . . . C24 C 0.4774(2) 0.1315(2) 0.4517(2) 0.0296(10) Uani 1 1 d . . . H24 H 0.4580 0.1711 0.4735 0.036 Uiso 1 1 calc R . . C25 C 0.5444(2) 0.0922(2) 0.4922(2) 0.0402(12) Uani 1 1 d . . . H25 H 0.5714 0.1054 0.5411 0.048 Uiso 1 1 calc R . . C26 C 0.5722(2) 0.0337(3) 0.4612(3) 0.0509(15) Uani 1 1 d . . . H26 H 0.6184 0.0063 0.4889 0.061 Uiso 1 1 calc R . . C27 C 0.5332(2) 0.0149(2) 0.3907(3) 0.0401(12) Uani 1 1 d . . . H27 H 0.5526 -0.0253 0.3694 0.048 Uiso 1 1 calc R . . C28 C 0.4653(2) 0.0545(2) 0.3503(2) 0.0286(10) Uani 1 1 d . . . H28 H 0.4375 0.0402 0.3018 0.034 Uiso 1 1 calc R . . C29 C 0.3152(2) 0.13986(17) 0.24036(18) 0.0139(8) Uani 1 1 d . . . C30 C 0.3695(2) 0.14038(18) 0.20501(19) 0.0202(9) Uani 1 1 d . . . H30 H 0.4239 0.1490 0.2318 0.024 Uiso 1 1 calc R . . C31 C 0.3455(2) 0.12866(19) 0.1318(2) 0.0253(10) Uani 1 1 d . . . H31 H 0.3836 0.1287 0.1090 0.030 Uiso 1 1 calc R . . C32 C 0.2675(2) 0.1171(2) 0.09217(19) 0.0258(9) Uani 1 1 d . . . H32 H 0.2514 0.1088 0.0419 0.031 Uiso 1 1 calc R . . C33 C 0.2119(2) 0.1174(2) 0.12477(18) 0.0248(9) Uani 1 1 d . . . H33 H 0.1574 0.1100 0.0971 0.030 Uiso 1 1 calc R . . C34 C 0.2358(2) 0.12855(19) 0.19813(18) 0.0191(9) Uani 1 1 d . . . H34 H 0.1972 0.1285 0.2203 0.023 Uiso 1 1 calc R . . Ru2 Ru 0.166015(17) 0.617987(16) 0.179147(15) 0.01373(7) Uani 1 1 d . . . Cl2 Cl 0.13068(5) 0.61286(5) 0.04964(4) 0.0238(2) Uani 1 1 d . . . P2 P 0.16290(5) 0.74075(5) 0.19599(5) 0.0137(2) Uani 1 1 d . . . N4 N 0.29022(16) 0.60118(15) 0.20613(15) 0.0169(7) Uani 1 1 d . . . N5 N 0.19362(16) 0.58629(15) 0.28121(14) 0.0130(7) Uani 1 1 d . . . N6 N 0.05170(16) 0.58285(15) 0.17713(15) 0.0162(7) Uani 1 1 d . . . C35 C 0.3258(2) 0.59923(18) 0.28519(19) 0.0164(8) Uani 1 1 d . . . C36 C 0.4061(2) 0.6088(2) 0.3222(2) 0.0244(9) Uani 1 1 d . . . H36 H 0.4396 0.6226 0.2967 0.029 Uiso 1 1 calc R . . C37 C 0.4381(2) 0.5986(2) 0.3952(2) 0.0304(10) Uani 1 1 d . . . H37 H 0.4926 0.6086 0.4206 0.036 Uiso 1 1 calc R . . C38 C 0.3895(2) 0.5734(2) 0.4312(2) 0.0258(10) Uani 1 1 d . . . H38 H 0.4117 0.5621 0.4810 0.031 Uiso 1 1 calc R . . C39 C 0.3095(2) 0.56478(18) 0.39518(18) 0.0186(9) Uani 1 1 d . . . H39 H 0.2776 0.5457 0.4204 0.022 Uiso 1 1 calc R . . C40 C 0.2739(2) 0.58309(18) 0.32301(18) 0.0142(8) Uani 1 1 d . . . C41 C 0.1301(2) 0.58864(18) 0.30621(18) 0.0131(8) Uani 1 1 d . . . C42 C 0.1326(2) 0.59557(18) 0.37667(19) 0.0207(9) Uani 1 1 d . . . H42 H 0.1822 0.5927 0.4150 0.025 Uiso 1 1 calc R . . C43 C 0.0641(2) 0.60658(19) 0.3920(2) 0.0253(10) Uani 1 1 d . . . H43 H 0.0677 0.6119 0.4406 0.030 Uiso 1 1 calc R . . C44 C -0.0086(2) 0.6099(2) 0.3384(2) 0.0264(10) Uani 1 1 d . . . H44 H -0.0550 0.6183 0.3493 0.032 Uiso 1 1 calc R . . C45 C -0.0133(2) 0.6010(2) 0.2681(2) 0.0248(10) Uani 1 1 d . . . H45 H -0.0638 0.6012 0.2307 0.030 Uiso 1 1 calc R . . C46 C 0.0544(2) 0.59177(18) 0.25118(18) 0.0155(8) Uani 1 1 d . . . C47 C 0.3371(2) 0.6475(2) 0.17231(19) 0.0257(10) Uani 1 1 d . . . H47A H 0.3472 0.6983 0.1944 0.039 Uiso 1 1 calc R . . H47B H 0.3073 0.6525 0.1207 0.039 Uiso 1 1 calc R . . H47C H 0.3877 0.6219 0.1796 0.039 Uiso 1 1 calc R . . C48 C 0.2885(2) 0.52060(19) 0.18047(18) 0.0233(9) Uani 1 1 d . . . H48A H 0.3427 0.5006 0.1957 0.035 Uiso 1 1 calc R . . H48B H 0.2648 0.5194 0.1279 0.035 Uiso 1 1 calc R . . H48C H 0.2570 0.4890 0.2009 0.035 Uiso 1 1 calc R . . C49 C 0.0549(2) 0.49909(18) 0.16086(18) 0.0223(9) Uani 1 1 d . . . H49A H 0.1028 0.4764 0.1956 0.034 Uiso 1 1 calc R . . H49B H 0.0558 0.4930 0.1123 0.034 Uiso 1 1 calc R . . H49C H 0.0081 0.4734 0.1641 0.034 Uiso 1 1 calc R . . C50 C -0.02190(19) 0.6136(2) 0.12307(18) 0.0236(9) Uani 1 1 d . . . H50A H -0.0673 0.5831 0.1235 0.035 Uiso 1 1 calc R . . H50B H -0.0180 0.6110 0.0753 0.035 Uiso 1 1 calc R . . H50C H -0.0291 0.6668 0.1347 0.035 Uiso 1 1 calc R . . C51 C 0.07145(19) 0.79610(19) 0.15207(18) 0.0165(8) Uani 1 1 d . . . C52 C 0.0288(2) 0.7795(2) 0.08070(18) 0.0214(9) Uani 1 1 d . . . H52 H 0.0424 0.7357 0.0593 0.026 Uiso 1 1 calc R . . C53 C -0.0334(2) 0.8255(2) 0.03997(19) 0.0250(9) Uani 1 1 d . . . H53 H -0.0627 0.8128 -0.0086 0.030 Uiso 1 1 calc R . . C54 C -0.0526(2) 0.8901(2) 0.0706(2) 0.0288(10) Uani 1 1 d . . . H54 H -0.0951 0.9220 0.0430 0.035 Uiso 1 1 calc R . . C55 C -0.0100(2) 0.90788(19) 0.1409(2) 0.0228(9) Uani 1 1 d . . . H55 H -0.0234 0.9521 0.1618 0.027 Uiso 1 1 calc R . . C56 C 0.0517(2) 0.86230(18) 0.18134(19) 0.0184(9) Uani 1 1 d . . . H56 H 0.0813 0.8759 0.2296 0.022 Uiso 1 1 calc R . . C57 C 0.22332(19) 0.80641(18) 0.16406(17) 0.0150(8) Uani 1 1 d . . . C58 C 0.22673(19) 0.79457(19) 0.09606(18) 0.0169(8) Uani 1 1 d . . . H58 H 0.2047 0.7492 0.0706 0.020 Uiso 1 1 calc R . . C59 C 0.26132(19) 0.8472(2) 0.06481(19) 0.0201(9) Uani 1 1 d . . . H59 H 0.2634 0.8374 0.0186 0.024 Uiso 1 1 calc R . . C60 C 0.29291(19) 0.9140(2) 0.10037(19) 0.0215(9) Uani 1 1 d . . . H60 H 0.3164 0.9506 0.0788 0.026 Uiso 1 1 calc R . . C61 C 0.2898(2) 0.9269(2) 0.16772(19) 0.0223(9) Uani 1 1 d . . . H61 H 0.3113 0.9728 0.1926 0.027 Uiso 1 1 calc R . . C62 C 0.25591(19) 0.87390(19) 0.19930(18) 0.0178(8) Uani 1 1 d . . . H62 H 0.2548 0.8836 0.2458 0.021 Uiso 1 1 calc R . . C63 C 0.1943(2) 0.76434(18) 0.29127(17) 0.0138(8) Uani 1 1 d . . . C64 C 0.2741(2) 0.76562(18) 0.33133(19) 0.0196(9) Uani 1 1 d . . . H64 H 0.3109 0.7569 0.3079 0.023 Uiso 1 1 calc R . . C65 C 0.3023(2) 0.77913(19) 0.40436(19) 0.0275(10) Uani 1 1 d . . . H65 H 0.3576 0.7786 0.4308 0.033 Uiso 1 1 calc R . . C66 C 0.2492(3) 0.7934(2) 0.4386(2) 0.0319(10) Uani 1 1 d . . . H66 H 0.2679 0.8064 0.4881 0.038 Uiso 1 1 calc R . . C67 C 0.1690(2) 0.7886(2) 0.40034(19) 0.0295(10) Uani 1 1 d . . . H67 H 0.1326 0.7959 0.4244 0.035 Uiso 1 1 calc R . . C68 C 0.1409(2) 0.77341(18) 0.32775(19) 0.0212(9) Uani 1 1 d . . . H68 H 0.0855 0.7690 0.3023 0.025 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 0.01474(17) 0.01204(16) 0.01313(17) -0.00023(13) 0.00366(13) -0.00100(14) Cl1 0.0339(6) 0.0255(5) 0.0147(5) -0.0044(4) 0.0088(4) -0.0043(5) P1 0.0139(6) 0.0126(5) 0.0146(6) 0.0003(4) 0.0039(4) 0.0005(4) N1 0.0144(17) 0.0146(16) 0.0169(18) -0.0004(13) 0.0039(14) 0.0005(14) N2 0.0137(17) 0.0165(17) 0.0128(17) 0.0047(13) 0.0012(14) -0.0025(14) N3 0.0167(18) 0.0121(17) 0.0267(19) -0.0019(13) 0.0074(14) -0.0021(14) C1 0.016(2) 0.0113(18) 0.016(2) -0.0001(15) 0.0066(17) -0.0025(17) C2 0.023(2) 0.028(2) 0.025(2) -0.0020(18) 0.0097(19) -0.0014(19) C3 0.028(3) 0.038(3) 0.043(3) -0.002(2) 0.023(2) 0.000(2) C4 0.061(3) 0.030(2) 0.025(3) 0.0013(19) 0.030(2) -0.004(2) C5 0.030(3) 0.027(2) 0.016(2) 0.0006(17) 0.0077(19) -0.0057(19) C6 0.027(2) 0.0105(19) 0.019(2) 0.0010(15) 0.0065(19) -0.0056(18) C7 0.022(2) 0.0057(18) 0.018(2) -0.0001(15) -0.0029(18) -0.0021(17) C8 0.028(3) 0.022(2) 0.020(2) 0.0038(17) -0.0041(19) -0.0048(19) C9 0.046(3) 0.022(2) 0.025(3) 0.0006(19) -0.012(2) 0.001(2) C10 0.024(3) 0.025(3) 0.046(3) -0.007(2) -0.013(2) 0.002(2) C11 0.015(2) 0.022(2) 0.044(3) -0.002(2) 0.002(2) -0.0001(19) C12 0.020(2) 0.009(2) 0.023(2) -0.0004(15) 0.0028(18) -0.0019(17) C13 0.022(2) 0.018(2) 0.023(2) -0.0021(16) 0.0068(18) -0.0036(17) C14 0.014(2) 0.025(2) 0.022(2) 0.0031(18) -0.0014(17) -0.0047(19) C15 0.017(2) 0.025(2) 0.040(3) 0.0106(18) 0.0135(19) 0.0024(18) C16 0.024(2) 0.0134(19) 0.029(2) -0.0048(17) 0.0096(17) 0.0011(19) C17 0.010(2) 0.014(2) 0.020(2) 0.0019(15) 0.0074(16) 0.0000(16) C18 0.020(2) 0.0155(19) 0.014(2) 0.0008(16) 0.0031(16) 0.0043(18) C19 0.029(2) 0.023(2) 0.014(2) 0.0074(16) 0.0134(18) 0.0074(19) C20 0.013(2) 0.020(2) 0.023(2) 0.0114(17) 0.0075(17) 0.0015(17) C21 0.030(2) 0.013(2) 0.026(2) -0.0022(17) 0.0083(19) -0.0064(18) C22 0.026(2) 0.019(2) 0.022(2) -0.0001(17) 0.0173(18) -0.0010(18) C23 0.011(2) 0.0125(19) 0.030(2) 0.0043(18) 0.0056(17) -0.0053(17) C24 0.032(3) 0.019(2) 0.030(3) 0.0073(18) 0.001(2) -0.0034(19) C25 0.019(3) 0.033(3) 0.048(3) 0.022(2) -0.014(2) -0.013(2) C26 0.014(3) 0.043(3) 0.083(4) 0.043(3) 0.002(3) 0.004(2) C27 0.027(3) 0.025(3) 0.073(4) 0.023(2) 0.024(3) 0.010(2) C28 0.022(2) 0.019(2) 0.045(3) 0.0117(19) 0.013(2) 0.0011(19) C29 0.020(2) 0.0085(18) 0.014(2) 0.0010(14) 0.0083(17) -0.0001(16) C30 0.027(2) 0.015(2) 0.020(2) 0.0005(16) 0.0104(19) -0.0006(17) C31 0.040(3) 0.018(2) 0.028(3) -0.0022(18) 0.025(2) -0.003(2) C32 0.048(3) 0.018(2) 0.010(2) 0.0002(17) 0.010(2) -0.001(2) C33 0.030(2) 0.024(2) 0.015(2) -0.0006(18) 0.0002(18) 0.007(2) C34 0.023(2) 0.019(2) 0.018(2) 0.0012(16) 0.0099(18) 0.0057(18) Ru2 0.01673(17) 0.01110(15) 0.01349(17) -0.00105(13) 0.00551(13) 0.00016(14) Cl2 0.0361(6) 0.0210(5) 0.0152(5) -0.0035(4) 0.0101(4) -0.0003(5) P2 0.0160(6) 0.0125(5) 0.0126(5) -0.0014(4) 0.0050(4) -0.0006(4) N4 0.0201(18) 0.0115(16) 0.0236(19) 0.0016(13) 0.0135(14) 0.0021(14) N5 0.0130(17) 0.0122(16) 0.0123(17) -0.0003(12) 0.0028(14) -0.0021(14) N6 0.0130(17) 0.0140(16) 0.0190(18) -0.0005(13) 0.0026(14) 0.0006(14) C35 0.018(2) 0.0093(19) 0.021(2) -0.0034(15) 0.0067(18) 0.0011(16) C36 0.019(2) 0.020(2) 0.038(3) 0.0003(19) 0.015(2) -0.0016(19) C37 0.019(2) 0.026(2) 0.037(3) -0.0089(19) -0.002(2) -0.0004(19) C38 0.023(2) 0.025(2) 0.023(2) -0.0065(18) -0.0002(19) 0.004(2) C39 0.018(2) 0.016(2) 0.019(2) -0.0023(16) 0.0027(18) 0.0001(17) C40 0.014(2) 0.0093(18) 0.018(2) -0.0025(15) 0.0044(17) 0.0014(16) C41 0.015(2) 0.0068(18) 0.017(2) 0.0022(15) 0.0050(17) -0.0014(16) C42 0.021(2) 0.018(2) 0.020(2) 0.0008(16) 0.0036(18) -0.0031(17) C43 0.035(3) 0.021(2) 0.029(2) -0.0026(18) 0.023(2) -0.001(2) C44 0.025(2) 0.026(2) 0.038(3) 0.006(2) 0.023(2) 0.004(2) C45 0.014(2) 0.027(2) 0.033(3) 0.0104(18) 0.0075(19) 0.0020(18) C46 0.017(2) 0.0096(18) 0.020(2) 0.0018(15) 0.0065(17) -0.0023(16) C47 0.021(2) 0.026(2) 0.035(3) 0.0046(18) 0.016(2) 0.0032(19) C48 0.027(2) 0.017(2) 0.026(2) 0.0016(17) 0.0102(18) 0.0070(18) C49 0.025(2) 0.017(2) 0.023(2) -0.0024(16) 0.0055(18) -0.0048(18) C50 0.012(2) 0.024(2) 0.028(2) 0.0067(18) -0.0009(17) 0.0003(18) C51 0.015(2) 0.014(2) 0.022(2) 0.0031(16) 0.0078(17) -0.0003(17) C52 0.025(2) 0.019(2) 0.020(2) 0.0012(17) 0.0083(18) 0.0026(19) C53 0.028(2) 0.026(2) 0.015(2) -0.0006(17) -0.0007(18) 0.003(2) C54 0.023(2) 0.028(2) 0.034(3) 0.011(2) 0.009(2) 0.010(2) C55 0.024(2) 0.014(2) 0.033(3) -0.0003(17) 0.0130(19) 0.0012(18) C56 0.020(2) 0.013(2) 0.021(2) -0.0005(15) 0.0050(17) 0.0004(17) C57 0.020(2) 0.012(2) 0.013(2) 0.0020(15) 0.0056(16) 0.0034(16) C58 0.018(2) 0.0106(19) 0.021(2) 0.0002(16) 0.0057(17) 0.0014(17) C59 0.021(2) 0.022(2) 0.018(2) 0.0022(17) 0.0068(18) 0.0040(18) C60 0.018(2) 0.020(2) 0.031(2) 0.0080(18) 0.0143(19) 0.0007(18) C61 0.025(2) 0.016(2) 0.025(2) -0.0038(17) 0.0080(19) 0.0004(18) C62 0.020(2) 0.018(2) 0.016(2) 0.0032(16) 0.0067(16) 0.0023(18) C63 0.019(2) 0.0099(18) 0.012(2) 0.0003(14) 0.0050(17) -0.0013(16) C64 0.025(2) 0.0120(19) 0.023(2) -0.0017(16) 0.0100(18) -0.0004(18) C65 0.038(3) 0.013(2) 0.023(2) -0.0008(17) 0.001(2) -0.0039(19) C66 0.060(3) 0.015(2) 0.016(2) -0.0029(17) 0.007(2) -0.012(2) C67 0.056(3) 0.018(2) 0.024(2) -0.0048(18) 0.026(2) -0.012(2) C68 0.030(2) 0.010(2) 0.024(2) -0.0021(16) 0.0112(19) -0.0027(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 Ru1 N2 1.991(3) . ? Ru1 N3 2.124(3) . ? Ru1 N1 2.136(3) . ? Ru1 P1 2.1782(9) . ? Ru1 Cl1 2.4191(9) . ? P1 C29 1.815(3) . ? P1 C23 1.847(3) . ? P1 C17 1.849(3) . ? N1 C1 1.467(4) . ? N1 C14 1.482(4) . ? N1 C13 1.496(4) . ? N2 C7 1.389(4) . ? N2 C6 1.399(4) . ? N3 C12 1.475(4) . ? N3 C15 1.495(4) . ? N3 C16 1.496(4) . ? C1 C2 1.377(4) . ? C1 C6 1.424(4) . ? C2 C3 1.374(5) . ? C2 H2 0.9500 . ? C3 C4 1.374(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.395(4) . ? C5 H5 0.9500 . ? C7 C8 1.398(4) . ? C7 C12 1.416(5) . ? C8 C9 1.374(5) . ? C8 H8 0.9500 . ? C9 C10 1.373(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 C12 1.387(4) . ? C11 H11 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.388(4) . ? C17 C22 1.395(4) . ? C18 C19 1.382(4) . ? C18 H18 0.9500 . ? C19 C20 1.375(4) . ? C19 H19 0.9500 . ? C20 C21 1.377(4) . ? C20 H20 0.9500 . ? C21 C22 1.382(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.381(4) . ? C23 C28 1.387(5) . ? C24 C25 1.376(5) . ? C24 H24 0.9500 . ? C25 C26 1.379(6) . ? C25 H25 0.9500 . ? C26 C27 1.370(6) . ? C26 H26 0.9500 . ? C27 C28 1.390(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.394(4) . ? C29 C30 1.396(4) . ? C30 C31 1.380(4) . ? C30 H30 0.9500 . ? C31 C32 1.364(5) . ? C31 H31 0.9500 . ? C32 C33 1.376(5) . ? C32 H32 0.9500 . ? C33 C34 1.383(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? Ru2 N5 1.993(3) . ? Ru2 N4 2.133(3) . ? Ru2 N6 2.141(3) . ? Ru2 P2 2.1781(9) . ? Ru2 Cl2 2.4295(9) . ? P2 C63 1.825(3) . ? P2 C51 1.845(3) . ? P2 C57 1.847(3) . ? N4 C35 1.475(4) . ? N4 C47 1.495(4) . ? N4 C48 1.497(4) . ? N5 C40 1.393(4) . ? N5 C41 1.404(4) . ? N6 C46 1.467(4) . ? N6 C50 1.482(4) . ? N6 C49 1.507(4) . ? C35 C36 1.384(4) . ? C35 C40 1.425(4) . ? C36 C37 1.372(5) . ? C36 H36 0.9500 . ? C37 C38 1.387(5) . ? C37 H37 0.9500 . ? C38 C39 1.375(4) . ? C38 H38 0.9500 . ? C39 C40 1.388(4) . ? C39 H39 0.9500 . ? C41 C42 1.394(4) . ? C41 C46 1.418(4) . ? C42 C43 1.391(4) . ? C42 H42 0.9500 . ? C43 C44 1.367(5) . ? C43 H43 0.9500 . ? C44 C45 1.381(4) . ? C44 H44 0.9500 . ? C45 C46 1.388(4) . ? C45 H45 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.386(4) . ? C51 C56 1.399(4) . ? C52 C53 1.386(4) . ? C52 H52 0.9500 . ? C53 C54 1.387(5) . ? C53 H53 0.9500 . ? C54 C55 1.373(4) . ? C54 H54 0.9500 . ? C55 C56 1.375(4) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C62 1.393(4) . ? C57 C58 1.393(4) . ? C58 C59 1.379(4) . ? C58 H58 0.9500 . ? C59 C60 1.382(4) . ? C59 H59 0.9500 . ? C60 C61 1.381(4) . ? C60 H60 0.9500 . ? C61 C62 1.381(4) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.377(4) . ? C63 C68 1.408(4) . ? C64 C65 1.380(4) . ? C64 H64 0.9500 . ? C65 C66 1.383(5) . ? C65 H65 0.9500 . ? C66 C67 1.380(5) . ? C66 H66 0.9500 . ? C67 C68 1.378(4) . ? C67 H67 0.9500 . ? C68 H68 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 N2 Ru1 N3 81.39(11) . . ? N2 Ru1 N1 80.53(11) . . ? N3 Ru1 N1 151.86(10) . . ? N2 Ru1 P1 97.12(8) . . ? N3 Ru1 P1 100.79(8) . . ? N1 Ru1 P1 102.70(8) . . ? N2 Ru1 Cl1 161.74(8) . . ? N3 Ru1 Cl1 95.74(8) . . ? N1 Ru1 Cl1 94.72(8) . . ? P1 Ru1 Cl1 101.13(3) . . ? C29 P1 C23 105.20(16) . . ? C29 P1 C17 103.63(15) . . ? C23 P1 C17 94.64(15) . . ? C29 P1 Ru1 110.86(10) . . ? C23 P1 Ru1 119.80(11) . . ? C17 P1 Ru1 120.27(11) . . ? C1 N1 C14 112.9(3) . . ? C1 N1 C13 107.8(3) . . ? C14 N1 C13 107.3(3) . . ? C1 N1 Ru1 106.81(19) . . ? C14 N1 Ru1 121.2(2) . . ? C13 N1 Ru1 99.48(19) . . ? C7 N2 C6 127.7(3) . . ? C7 N2 Ru1 116.0(2) . . ? C6 N2 Ru1 115.3(2) . . ? C12 N3 C15 113.0(3) . . ? C12 N3 C16 106.8(2) . . ? C15 N3 C16 107.2(3) . . ? C12 N3 Ru1 107.4(2) . . ? C15 N3 Ru1 121.8(2) . . ? C16 N3 Ru1 98.67(19) . . ? C2 C1 C6 121.3(3) . . ? C2 C1 N1 121.8(3) . . ? C6 C1 N1 116.9(3) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 119.4(4) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 121.1(4) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 121.3(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 N2 128.9(3) . . ? C5 C6 C1 116.4(3) . . ? N2 C6 C1 114.6(3) . . ? N2 C7 C8 127.9(3) . . ? N2 C7 C12 115.8(3) . . ? C8 C7 C12 116.2(3) . . ? C9 C8 C7 121.3(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 121.6(4) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 118.8(4) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 121.1(3) . . ? C11 C12 N3 122.3(3) . . ? C7 C12 N3 116.3(3) . . ? N1 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 117.8(3) . . ? C18 C17 P1 120.1(3) . . ? C22 C17 P1 121.7(3) . . ? C19 C18 C17 120.7(3) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 121.0(3) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 119.0(3) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C17 121.0(3) . . ? C21 C22 H22 119.5 . . ? C17 C22 H22 119.5 . . ? C24 C23 C28 118.0(3) . . ? C24 C23 P1 117.1(3) . . ? C28 C23 P1 124.3(3) . . ? C25 C24 C23 121.7(4) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 119.5(4) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C27 C26 C25 120.1(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.0(4) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C23 C28 C27 120.6(4) . . ? C23 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C34 C29 C30 116.9(3) . . ? C34 C29 P1 120.8(3) . . ? C30 C29 P1 121.8(3) . . ? C31 C30 C29 121.3(3) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C32 C31 C30 120.4(3) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 120.2(4) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C34 119.5(4) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C33 C34 C29 121.8(3) . . ? C33 C34 H34 119.1 . . ? C29 C34 H34 119.1 . . ? N5 Ru2 N4 81.09(11) . . ? N5 Ru2 N6 80.16(11) . . ? N4 Ru2 N6 152.36(10) . . ? N5 Ru2 P2 97.36(8) . . ? N4 Ru2 P2 100.34(8) . . ? N6 Ru2 P2 102.04(8) . . ? N5 Ru2 Cl2 161.72(8) . . ? N4 Ru2 Cl2 96.79(8) . . ? N6 Ru2 Cl2 94.70(8) . . ? P2 Ru2 Cl2 100.88(3) . . ? C63 P2 C51 105.61(16) . . ? C63 P2 C57 102.39(15) . . ? C51 P2 C57 92.81(15) . . ? C63 P2 Ru2 111.59(11) . . ? C51 P2 Ru2 120.83(11) . . ? C57 P2 Ru2 120.66(11) . . ? C35 N4 C47 113.1(3) . . ? C35 N4 C48 106.9(2) . . ? C47 N4 C48 107.6(3) . . ? C35 N4 Ru2 107.01(19) . . ? C47 N4 Ru2 121.7(2) . . ? C48 N4 Ru2 98.73(19) . . ? C40 N5 C41 126.7(3) . . ? C40 N5 Ru2 116.8(2) . . ? C41 N5 Ru2 114.5(2) . . ? C46 N6 C50 113.1(3) . . ? C46 N6 C49 109.2(2) . . ? C50 N6 C49 106.8(3) . . ? C46 N6 Ru2 105.31(19) . . ? C50 N6 Ru2 121.3(2) . . ? C49 N6 Ru2 99.98(19) . . ? C36 C35 C40 120.3(3) . . ? C36 C35 N4 122.9(3) . . ? C40 C35 N4 116.8(3) . . ? C37 C36 C35 121.0(3) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C38 119.0(4) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C39 C38 C37 120.4(4) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 121.9(3) . . ? C38 C39 H39 119.0 . . ? C40 C39 H39 119.0 . . ? C39 C40 N5 129.0(3) . . ? C39 C40 C35 116.4(3) . . ? N5 C40 C35 114.6(3) . . ? C42 C41 N5 128.4(3) . . ? C42 C41 C46 116.9(3) . . ? N5 C41 C46 114.4(3) . . ? C43 C42 C41 121.4(3) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C44 C43 C42 121.1(3) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C43 C44 C45 119.0(3) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C44 C45 C46 121.1(3) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C45 C46 C41 120.5(3) . . ? C45 C46 N6 122.6(3) . . ? C41 C46 N6 116.8(3) . . ? N4 C47 H47A 109.5 . . ? N4 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N4 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N4 C48 H48A 109.5 . . ? N4 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N4 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N6 C49 H49A 109.5 . . ? N6 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N6 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N6 C50 H50A 109.5 . . ? N6 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N6 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C56 118.1(3) . . ? C52 C51 P2 117.0(3) . . ? C56 C51 P2 123.7(3) . . ? C53 C52 C51 121.2(3) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C52 C53 C54 119.6(3) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C55 C54 C53 119.8(3) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 120.7(3) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C55 C56 C51 120.7(3) . . ? C55 C56 H56 119.7 . . ? C51 C56 H56 119.7 . . ? C62 C57 C58 117.3(3) . . ? C62 C57 P2 123.3(3) . . ? C58 C57 P2 118.6(2) . . ? C59 C58 C57 121.6(3) . . ? C59 C58 H58 119.2 . . ? C57 C58 H58 119.2 . . ? C58 C59 C60 120.3(3) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C61 C60 C59 119.0(3) . . ? C61 C60 H60 120.5 . . ? C59 C60 H60 120.5 . . ? C62 C61 C60 120.7(3) . . ? C62 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? C61 C62 C57 121.1(3) . . ? C61 C62 H62 119.4 . . ? C57 C62 H62 119.4 . . ? C64 C63 C68 117.8(3) . . ? C64 C63 P2 118.7(3) . . ? C68 C63 P2 123.1(3) . . ? C63 C64 C65 122.1(3) . . ? C63 C64 H64 118.9 . . ? C65 C64 H64 118.9 . . ? C64 C65 C66 119.3(4) . . ? C64 C65 H65 120.3 . . ? C66 C65 H65 120.3 . . ? C67 C66 C65 119.5(4) . . ? C67 C66 H66 120.3 . . ? C65 C66 H66 120.3 . . ? C68 C67 C66 121.0(4) . . ? C68 C67 H67 119.5 . . ? C66 C67 H67 119.5 . . ? C67 C68 C63 119.9(4) . . ? C67 C68 H68 120.0 . . ? C63 C68 H68 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru1 P1 C29 -5.93(15) . . . . ? N3 Ru1 P1 C29 76.62(15) . . . . ? N1 Ru1 P1 C29 -87.78(15) . . . . ? Cl1 Ru1 P1 C29 174.74(12) . . . . ? N2 Ru1 P1 C23 116.87(15) . . . . ? N3 Ru1 P1 C23 -160.59(15) . . . . ? N1 Ru1 P1 C23 35.02(15) . . . . ? Cl1 Ru1 P1 C23 -62.47(14) . . . . ? N2 Ru1 P1 C17 -126.89(15) . . . . ? N3 Ru1 P1 C17 -44.34(15) . . . . ? N1 Ru1 P1 C17 151.26(15) . . . . ? Cl1 Ru1 P1 C17 53.78(13) . . . . ? N2 Ru1 N1 C1 -20.36(19) . . . . ? N3 Ru1 N1 C1 -71.1(3) . . . . ? P1 Ru1 N1 C1 74.87(19) . . . . ? Cl1 Ru1 N1 C1 177.41(18) . . . . ? N2 Ru1 N1 C14 -151.4(3) . . . . ? N3 Ru1 N1 C14 157.9(2) . . . . ? P1 Ru1 N1 C14 -56.2(2) . . . . ? Cl1 Ru1 N1 C14 46.3(2) . . . . ? N2 Ru1 N1 C13 91.6(2) . . . . ? N3 Ru1 N1 C13 40.9(3) . . . . ? P1 Ru1 N1 C13 -173.14(17) . . . . ? Cl1 Ru1 N1 C13 -70.60(19) . . . . ? N3 Ru1 N2 C7 -11.0(2) . . . . ? N1 Ru1 N2 C7 -169.3(3) . . . . ? P1 Ru1 N2 C7 88.9(2) . . . . ? Cl1 Ru1 N2 C7 -93.2(3) . . . . ? N3 Ru1 N2 C6 179.3(2) . . . . ? N1 Ru1 N2 C6 20.9(2) . . . . ? P1 Ru1 N2 C6 -80.8(2) . . . . ? Cl1 Ru1 N2 C6 97.1(3) . . . . ? N2 Ru1 N3 C12 15.11(19) . . . . ? N1 Ru1 N3 C12 65.6(3) . . . . ? P1 Ru1 N3 C12 -80.56(18) . . . . ? Cl1 Ru1 N3 C12 176.93(18) . . . . ? N2 Ru1 N3 C15 147.7(3) . . . . ? N1 Ru1 N3 C15 -161.7(2) . . . . ? P1 Ru1 N3 C15 52.1(3) . . . . ? Cl1 Ru1 N3 C15 -50.4(2) . . . . ? N2 Ru1 N3 C16 -95.7(2) . . . . ? N1 Ru1 N3 C16 -45.1(3) . . . . ? P1 Ru1 N3 C16 168.66(17) . . . . ? Cl1 Ru1 N3 C16 66.15(19) . . . . ? C14 N1 C1 C2 -27.9(4) . . . . ? C13 N1 C1 C2 90.4(4) . . . . ? Ru1 N1 C1 C2 -163.5(3) . . . . ? C14 N1 C1 C6 153.8(3) . . . . ? C13 N1 C1 C6 -87.9(3) . . . . ? Ru1 N1 C1 C6 18.2(3) . . . . ? C6 C1 C2 C3 -2.2(5) . . . . ? N1 C1 C2 C3 179.7(3) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? C2 C3 C4 C5 1.9(6) . . . . ? C3 C4 C5 C6 -0.5(6) . . . . ? C4 C5 C6 N2 -177.0(3) . . . . ? C4 C5 C6 C1 -2.1(5) . . . . ? C7 N2 C6 C5 -9.8(6) . . . . ? Ru1 N2 C6 C5 158.5(3) . . . . ? C7 N2 C6 C1 175.2(3) . . . . ? Ru1 N2 C6 C1 -16.5(4) . . . . ? C2 C1 C6 C5 3.4(5) . . . . ? N1 C1 C6 C5 -178.3(3) . . . . ? C2 C1 C6 N2 179.1(3) . . . . ? N1 C1 C6 N2 -2.6(4) . . . . ? C6 N2 C7 C8 -11.0(6) . . . . ? Ru1 N2 C7 C8 -179.3(3) . . . . ? C6 N2 C7 C12 172.0(3) . . . . ? Ru1 N2 C7 C12 3.8(4) . . . . ? N2 C7 C8 C9 175.9(3) . . . . ? C12 C7 C8 C9 -7.2(5) . . . . ? C7 C8 C9 C10 2.0(6) . . . . ? C8 C9 C10 C11 3.4(6) . . . . ? C9 C10 C11 C12 -3.2(6) . . . . ? C10 C11 C12 C7 -2.4(5) . . . . ? C10 C11 C12 N3 171.5(3) . . . . ? N2 C7 C12 C11 -175.3(3) . . . . ? C8 C7 C12 C11 7.4(5) . . . . ? N2 C7 C12 N3 10.4(4) . . . . ? C8 C7 C12 N3 -166.8(3) . . . . ? C15 N3 C12 C11 30.6(4) . . . . ? C16 N3 C12 C11 -87.1(4) . . . . ? Ru1 N3 C12 C11 167.8(3) . . . . ? C15 N3 C12 C7 -155.2(3) . . . . ? C16 N3 C12 C7 87.0(3) . . . . ? Ru1 N3 C12 C7 -18.0(3) . . . . ? C29 P1 C17 C18 -162.0(3) . . . . ? C23 P1 C17 C18 91.1(3) . . . . ? Ru1 P1 C17 C18 -37.6(3) . . . . ? C29 P1 C17 C22 26.2(3) . . . . ? C23 P1 C17 C22 -80.7(3) . . . . ? Ru1 P1 C17 C22 150.7(2) . . . . ? C22 C17 C18 C19 -0.5(5) . . . . ? P1 C17 C18 C19 -172.6(3) . . . . ? C17 C18 C19 C20 -0.5(5) . . . . ? C18 C19 C20 C21 0.9(5) . . . . ? C19 C20 C21 C22 -0.3(5) . . . . ? C20 C21 C22 C17 -0.7(5) . . . . ? C18 C17 C22 C21 1.1(5) . . . . ? P1 C17 C22 C21 173.0(3) . . . . ? C29 P1 C23 C24 172.7(3) . . . . ? C17 P1 C23 C24 -81.8(3) . . . . ? Ru1 P1 C23 C24 47.2(3) . . . . ? C29 P1 C23 C28 -16.0(3) . . . . ? C17 P1 C23 C28 89.5(3) . . . . ? Ru1 P1 C23 C28 -141.5(3) . . . . ? C28 C23 C24 C25 2.7(5) . . . . ? P1 C23 C24 C25 174.6(3) . . . . ? C23 C24 C25 C26 -1.2(6) . . . . ? C24 C25 C26 C27 0.0(6) . . . . ? C25 C26 C27 C28 -0.4(6) . . . . ? C24 C23 C28 C27 -3.0(5) . . . . ? P1 C23 C28 C27 -174.3(3) . . . . ? C26 C27 C28 C23 2.0(6) . . . . ? C23 P1 C29 C34 143.1(3) . . . . ? C17 P1 C29 C34 44.3(3) . . . . ? Ru1 P1 C29 C34 -86.0(3) . . . . ? C23 P1 C29 C30 -45.6(3) . . . . ? C17 P1 C29 C30 -144.3(3) . . . . ? Ru1 P1 C29 C30 85.3(3) . . . . ? C34 C29 C30 C31 -1.3(5) . . . . ? P1 C29 C30 C31 -172.9(3) . . . . ? C29 C30 C31 C32 0.7(5) . . . . ? C30 C31 C32 C33 0.4(5) . . . . ? C31 C32 C33 C34 -0.8(5) . . . . ? C32 C33 C34 C29 0.3(5) . . . . ? C30 C29 C34 C33 0.8(5) . . . . ? P1 C29 C34 C33 172.5(3) . . . . ? N5 Ru2 P2 C63 5.31(15) . . . . ? N4 Ru2 P2 C63 -76.93(14) . . . . ? N6 Ru2 P2 C63 86.76(15) . . . . ? Cl2 Ru2 P2 C63 -175.99(12) . . . . ? N5 Ru2 P2 C51 -119.67(15) . . . . ? N4 Ru2 P2 C51 158.10(14) . . . . ? N6 Ru2 P2 C51 -38.22(15) . . . . ? Cl2 Ru2 P2 C51 59.04(13) . . . . ? N5 Ru2 P2 C57 125.50(15) . . . . ? N4 Ru2 P2 C57 43.26(15) . . . . ? N6 Ru2 P2 C57 -153.05(14) . . . . ? Cl2 Ru2 P2 C57 -55.80(13) . . . . ? N5 Ru2 N4 C35 -16.26(19) . . . . ? N6 Ru2 N4 C35 -64.0(3) . . . . ? P2 Ru2 N4 C35 79.66(18) . . . . ? Cl2 Ru2 N4 C35 -177.93(17) . . . . ? N5 Ru2 N4 C47 -148.4(3) . . . . ? N6 Ru2 N4 C47 163.8(2) . . . . ? P2 Ru2 N4 C47 -52.5(2) . . . . ? Cl2 Ru2 N4 C47 49.9(2) . . . . ? N5 Ru2 N4 C48 94.54(19) . . . . ? N6 Ru2 N4 C48 46.8(3) . . . . ? P2 Ru2 N4 C48 -169.54(17) . . . . ? Cl2 Ru2 N4 C48 -67.13(18) . . . . ? N4 Ru2 N5 C40 11.4(2) . . . . ? N6 Ru2 N5 C40 171.0(2) . . . . ? P2 Ru2 N5 C40 -87.9(2) . . . . ? Cl2 Ru2 N5 C40 96.1(3) . . . . ? N4 Ru2 N5 C41 176.2(2) . . . . ? N6 Ru2 N5 C41 -24.2(2) . . . . ? P2 Ru2 N5 C41 76.8(2) . . . . ? Cl2 Ru2 N5 C41 -99.1(3) . . . . ? N5 Ru2 N6 C46 25.43(19) . . . . ? N4 Ru2 N6 C46 73.4(3) . . . . ? P2 Ru2 N6 C46 -70.08(19) . . . . ? Cl2 Ru2 N6 C46 -172.26(18) . . . . ? N5 Ru2 N6 C50 155.4(3) . . . . ? N4 Ru2 N6 C50 -156.7(2) . . . . ? P2 Ru2 N6 C50 59.9(2) . . . . ? Cl2 Ru2 N6 C50 -42.3(2) . . . . ? N5 Ru2 N6 C49 -87.8(2) . . . . ? N4 Ru2 N6 C49 -39.9(3) . . . . ? P2 Ru2 N6 C49 176.65(17) . . . . ? Cl2 Ru2 N6 C49 74.46(18) . . . . ? C47 N4 C35 C36 -26.3(4) . . . . ? C48 N4 C35 C36 92.0(4) . . . . ? Ru2 N4 C35 C36 -163.0(3) . . . . ? C47 N4 C35 C40 156.7(3) . . . . ? C48 N4 C35 C40 -85.0(3) . . . . ? Ru2 N4 C35 C40 20.0(3) . . . . ? C40 C35 C36 C37 3.8(5) . . . . ? N4 C35 C36 C37 -173.0(3) . . . . ? C35 C36 C37 C38 4.3(5) . . . . ? C36 C37 C38 C39 -5.2(5) . . . . ? C37 C38 C39 C40 -2.3(5) . . . . ? C38 C39 C40 N5 -171.7(3) . . . . ? C38 C39 C40 C35 10.0(5) . . . . ? C41 N5 C40 C39 15.7(5) . . . . ? Ru2 N5 C40 C39 178.4(3) . . . . ? C41 N5 C40 C35 -165.9(3) . . . . ? Ru2 N5 C40 C35 -3.3(4) . . . . ? C36 C35 C40 C39 -10.8(5) . . . . ? N4 C35 C40 C39 166.3(3) . . . . ? C36 C35 C40 N5 170.7(3) . . . . ? N4 C35 C40 N5 -12.3(4) . . . . ? C40 N5 C41 C42 6.7(5) . . . . ? Ru2 N5 C41 C42 -156.3(3) . . . . ? C40 N5 C41 C46 180.0(3) . . . . ? Ru2 N5 C41 C46 16.9(3) . . . . ? N5 C41 C42 C43 171.9(3) . . . . ? C46 C41 C42 C43 -1.3(5) . . . . ? C41 C42 C43 C44 0.9(5) . . . . ? C42 C43 C44 C45 1.0(5) . . . . ? C43 C44 C45 C46 -2.5(5) . . . . ? C44 C45 C46 C41 2.2(5) . . . . ? C44 C45 C46 N6 -179.4(3) . . . . ? C42 C41 C46 C45 -0.3(5) . . . . ? N5 C41 C46 C45 -174.4(3) . . . . ? C42 C41 C46 N6 -178.8(3) . . . . ? N5 C41 C46 N6 7.1(4) . . . . ? C50 N6 C46 C45 22.2(4) . . . . ? C49 N6 C46 C45 -96.6(4) . . . . ? Ru2 N6 C46 C45 156.8(3) . . . . ? C50 N6 C46 C41 -159.4(3) . . . . ? C49 N6 C46 C41 81.8(3) . . . . ? Ru2 N6 C46 C41 -24.8(3) . . . . ? C63 P2 C51 C52 -170.4(3) . . . . ? C57 P2 C51 C52 85.9(3) . . . . ? Ru2 P2 C51 C52 -42.7(3) . . . . ? C63 P2 C51 C56 22.7(3) . . . . ? C57 P2 C51 C56 -81.0(3) . . . . ? Ru2 P2 C51 C56 150.4(2) . . . . ? C56 C51 C52 C53 -2.2(5) . . . . ? P2 C51 C52 C53 -169.8(3) . . . . ? C51 C52 C53 C54 1.2(5) . . . . ? C52 C53 C54 C55 -0.2(5) . . . . ? C53 C54 C55 C56 0.2(5) . . . . ? C54 C55 C56 C51 -1.3(5) . . . . ? C52 C51 C56 C55 2.2(5) . . . . ? P2 C51 C56 C55 169.0(3) . . . . ? C63 P2 C57 C62 -22.6(3) . . . . ? C51 P2 C57 C62 84.1(3) . . . . ? Ru2 P2 C57 C62 -147.2(2) . . . . ? C63 P2 C57 C58 167.6(3) . . . . ? C51 P2 C57 C58 -85.8(3) . . . . ? Ru2 P2 C57 C58 43.0(3) . . . . ? C62 C57 C58 C59 0.4(5) . . . . ? P2 C57 C58 C59 170.8(3) . . . . ? C57 C58 C59 C60 -0.8(5) . . . . ? C58 C59 C60 C61 0.5(5) . . . . ? C59 C60 C61 C62 0.1(5) . . . . ? C60 C61 C62 C57 -0.6(5) . . . . ? C58 C57 C62 C61 0.3(5) . . . . ? P2 C57 C62 C61 -169.6(3) . . . . ? C51 P2 C63 C64 -147.6(3) . . . . ? C57 P2 C63 C64 -51.1(3) . . . . ? Ru2 P2 C63 C64 79.4(3) . . . . ? C51 P2 C63 C68 39.4(3) . . . . ? C57 P2 C63 C68 135.9(3) . . . . ? Ru2 P2 C63 C68 -93.7(3) . . . . ? C68 C63 C64 C65 -3.3(5) . . . . ? P2 C63 C64 C65 -176.6(3) . . . . ? C63 C64 C65 C66 -1.3(5) . . . . ? C64 C65 C66 C67 4.6(5) . . . . ? C65 C66 C67 C68 -3.1(5) . . . . ? C66 C67 C68 C63 -1.5(5) . . . . ? C64 C63 C68 C67 4.7(5) . . . . ? P2 C63 C68 C67 177.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.613 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.091