# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'pet-final.cif' _publ_contact_author ; Peter G. Jones Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; _publ_contact_author_phone '049 531 391-5382' _publ_contact_author_fax '049 531 391-5387' _publ_contact_author_email p.jones@tu-bs.de #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The Use of Diaminoalkynes as Bottle-Able Diaminodicarbenes. ; loop_ _publ_author_name _publ_author_address A.R.Petrov ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; C.G.Daniliuc ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; P.G.Jones ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; M.Tamm ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; _publ_contact_author_name 'Peter G. Jones' #============================================================================= # cif data for "pet09" (compound 2a) #============================================================================= data_pet09 _database_code_depnum_ccdc_archive 'CCDC 819865' #TrackingRef 'pet-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H20 Cr2 N2 O10' _chemical_formula_weight 576.40 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' Cr Cr 0.3209 0.6236 '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 9.4757(8) _cell_length_b 9.6051(6) _cell_length_c 15.9506(14) _cell_angle_alpha 103.107(6) _cell_angle_beta 94.293(6) _cell_angle_gamma 118.080(8) _cell_volume 1219.32(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13880 _cell_measurement_theta_min 2.2653 _cell_measurement_theta_max 30.7761 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98419 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36726 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6041 _reflns_number_gt 4653 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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^)+(0.0313P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6041 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.76821(3) 0.73584(3) 0.837303(16) 0.01371(6) Uani 1 1 d . . . Cr2 Cr 0.79433(3) 0.37076(3) 0.629258(15) 0.01200(6) Uani 1 1 d . . . N1 N 0.70522(14) 0.38524(15) 0.84827(8) 0.0122(3) Uani 1 1 d . . . N2 N 0.45903(14) 0.33111(14) 0.68251(8) 0.0127(3) Uani 1 1 d . . . O1 O 0.43240(13) 0.70335(13) 0.80775(8) 0.0235(3) Uani 1 1 d . . . O2 O 0.73515(14) 0.76185(15) 1.02734(8) 0.0278(3) Uani 1 1 d . . . O3 O 0.90625(14) 1.10430(14) 0.89586(8) 0.0281(3) Uani 1 1 d . . . O4 O 1.12214(13) 0.81135(15) 0.87463(8) 0.0276(3) Uani 1 1 d . . . O5 O 0.74089(13) 0.75855(14) 0.64954(8) 0.0258(3) Uani 1 1 d . . . O6 O 1.00777(13) 0.36977(14) 0.78037(7) 0.0224(3) Uani 1 1 d . . . O7 O 1.07093(13) 0.72649(13) 0.67284(7) 0.0225(3) Uani 1 1 d . . . O8 O 1.01648(13) 0.30415(13) 0.52257(7) 0.0207(2) Uani 1 1 d . . . O9 O 0.65920(14) 0.40176(15) 0.45835(8) 0.0292(3) Uani 1 1 d . . . O10 O 0.57528(14) -0.00154(13) 0.58832(7) 0.0226(3) Uani 1 1 d . . . C1 C 0.69236(16) 0.47547(18) 0.80055(9) 0.0120(3) Uani 1 1 d . . . C2 C 0.61772(17) 0.39163(17) 0.70655(9) 0.0117(3) Uani 1 1 d . . . C3 C 0.80549(17) 0.45142(19) 0.93818(9) 0.0154(3) Uani 1 1 d . . . H3A H 0.8615 0.5737 0.9566 0.019 Uiso 1 1 calc R . . H3B H 0.8903 0.4188 0.9386 0.019 Uiso 1 1 calc R . . C4 C 0.69952(19) 0.38638(19) 1.00313(10) 0.0184(3) Uani 1 1 d . . . H4A H 0.7694 0.4300 1.0627 0.022 Uiso 1 1 calc R . . H4B H 0.6194 0.4251 1.0058 0.022 Uiso 1 1 calc R . . C5 C 0.60917(19) 0.19818(19) 0.97480(10) 0.0193(3) Uani 1 1 d . . . H5A H 0.5326 0.1573 1.0139 0.023 Uiso 1 1 calc R . . H5B H 0.6888 0.1597 0.9803 0.023 Uiso 1 1 calc R . . C6 C 0.51418(18) 0.12850(19) 0.87985(10) 0.0161(3) Uani 1 1 d . . . H6A H 0.4237 0.1529 0.8764 0.019 Uiso 1 1 calc R . . H6B H 0.4656 0.0069 0.8607 0.019 Uiso 1 1 calc R . . C7 C 0.62407(17) 0.20203(17) 0.81777(10) 0.0139(3) Uani 1 1 d . . . H7A H 0.7080 0.1683 0.8162 0.017 Uiso 1 1 calc R . . H7B H 0.5576 0.1595 0.7574 0.017 Uiso 1 1 calc R . . C8 C 0.34831(17) 0.32263(18) 0.74501(10) 0.0155(3) Uani 1 1 d . . . H8A H 0.3001 0.3920 0.7376 0.019 Uiso 1 1 calc R . . H8B H 0.4121 0.3668 0.8062 0.019 Uiso 1 1 calc R . . C9 C 0.21147(17) 0.14480(18) 0.72903(10) 0.0172(3) Uani 1 1 d . . . H9A H 0.2591 0.0767 0.7400 0.021 Uiso 1 1 calc R . . H9B H 0.1381 0.1422 0.7704 0.021 Uiso 1 1 calc R . . C10 C 0.11381(18) 0.07339(19) 0.63486(10) 0.0177(3) Uani 1 1 d . . . H10A H 0.0574 0.1347 0.6254 0.021 Uiso 1 1 calc R . . H10B H 0.0297 -0.0439 0.6241 0.021 Uiso 1 1 calc R . . C11 C 0.22808(18) 0.08638(19) 0.57125(10) 0.0188(3) Uani 1 1 d . . . H11A H 0.1653 0.0479 0.5103 0.023 Uiso 1 1 calc R . . H11B H 0.2732 0.0134 0.5758 0.023 Uiso 1 1 calc R . . C12 C 0.36831(18) 0.26284(19) 0.59032(10) 0.0176(3) Uani 1 1 d . . . H12A H 0.4442 0.2648 0.5506 0.021 Uiso 1 1 calc R . . H12B H 0.3242 0.3331 0.5782 0.021 Uiso 1 1 calc R . . C13 C 0.55480(19) 0.70642(18) 0.81829(10) 0.0165(3) Uani 1 1 d . . . C14 C 0.75006(18) 0.74605(19) 0.95556(11) 0.0187(3) Uani 1 1 d . . . C15 C 0.85194(18) 0.9627(2) 0.87222(11) 0.0201(3) Uani 1 1 d . . . C16 C 0.98984(19) 0.78087(18) 0.85900(10) 0.0168(3) Uani 1 1 d . . . C17 C 0.75715(18) 0.74274(18) 0.71782(11) 0.0179(3) Uani 1 1 d . . . C18 C 0.91965(18) 0.36781(18) 0.72608(10) 0.0154(3) Uani 1 1 d . . . C19 C 0.95930(18) 0.59782(19) 0.65817(10) 0.0161(3) Uani 1 1 d . . . C20 C 0.93049(18) 0.32895(18) 0.56295(10) 0.0152(3) Uani 1 1 d . . . C21 C 0.70174(18) 0.38992(19) 0.52368(11) 0.0184(3) Uani 1 1 d . . . C22 C 0.65262(18) 0.1386(2) 0.60200(10) 0.0159(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.01082(12) 0.01110(13) 0.01682(13) 0.00236(10) 0.00163(9) 0.00463(10) Cr2 0.01108(12) 0.01150(12) 0.01185(12) 0.00412(9) 0.00253(9) 0.00416(10) N1 0.0104(6) 0.0125(6) 0.0119(6) 0.0029(5) 0.0019(5) 0.0048(5) N2 0.0110(6) 0.0112(6) 0.0139(6) 0.0042(5) 0.0008(5) 0.0042(5) O1 0.0172(6) 0.0208(6) 0.0312(7) 0.0035(5) 0.0027(5) 0.0107(5) O2 0.0265(7) 0.0367(7) 0.0204(6) 0.0021(5) 0.0044(5) 0.0190(6) O3 0.0213(6) 0.0140(6) 0.0428(8) 0.0026(5) -0.0015(5) 0.0077(5) O4 0.0166(6) 0.0369(7) 0.0278(7) 0.0113(6) 0.0036(5) 0.0117(5) O5 0.0250(6) 0.0306(7) 0.0282(7) 0.0164(6) 0.0083(5) 0.0150(6) O6 0.0184(6) 0.0321(7) 0.0198(6) 0.0098(5) 0.0027(5) 0.0143(5) O7 0.0191(6) 0.0163(6) 0.0261(6) 0.0066(5) 0.0050(5) 0.0039(5) O8 0.0194(6) 0.0210(6) 0.0206(6) 0.0068(5) 0.0091(5) 0.0085(5) O9 0.0213(6) 0.0316(7) 0.0265(7) 0.0187(6) -0.0008(5) 0.0033(5) O10 0.0254(6) 0.0143(6) 0.0216(6) 0.0042(5) 0.0044(5) 0.0054(5) C1 0.0065(6) 0.0148(8) 0.0148(7) 0.0046(6) 0.0043(5) 0.0050(6) C2 0.0119(7) 0.0069(7) 0.0153(7) 0.0048(6) 0.0015(6) 0.0036(6) C3 0.0130(7) 0.0183(8) 0.0122(7) 0.0033(6) -0.0004(6) 0.0067(6) C4 0.0191(8) 0.0222(9) 0.0116(7) 0.0051(6) 0.0022(6) 0.0087(7) C5 0.0229(8) 0.0215(8) 0.0162(8) 0.0092(7) 0.0062(6) 0.0115(7) C6 0.0179(8) 0.0146(8) 0.0173(8) 0.0067(6) 0.0051(6) 0.0083(6) C7 0.0160(7) 0.0123(7) 0.0140(7) 0.0041(6) 0.0038(6) 0.0074(6) C8 0.0120(7) 0.0158(8) 0.0176(8) 0.0036(6) 0.0026(6) 0.0068(6) C9 0.0121(7) 0.0170(8) 0.0199(8) 0.0069(6) 0.0032(6) 0.0047(6) C10 0.0112(7) 0.0137(8) 0.0238(9) 0.0061(7) -0.0002(6) 0.0032(6) C11 0.0152(8) 0.0189(8) 0.0153(8) 0.0013(6) -0.0025(6) 0.0058(7) C12 0.0137(7) 0.0220(8) 0.0140(8) 0.0071(6) 0.0001(6) 0.0062(7) C13 0.0185(8) 0.0098(7) 0.0173(8) 0.0022(6) 0.0030(6) 0.0049(6) C14 0.0134(7) 0.0158(8) 0.0234(9) 0.0005(7) 0.0005(6) 0.0075(6) C15 0.0137(8) 0.0211(9) 0.0253(9) 0.0059(7) 0.0020(7) 0.0094(7) C16 0.0173(8) 0.0135(8) 0.0163(8) 0.0040(6) 0.0025(6) 0.0057(6) C17 0.0123(7) 0.0137(8) 0.0272(9) 0.0058(7) 0.0049(6) 0.0062(6) C18 0.0140(7) 0.0139(8) 0.0175(8) 0.0053(6) 0.0085(6) 0.0055(6) C19 0.0172(8) 0.0191(8) 0.0151(8) 0.0064(6) 0.0053(6) 0.0106(7) C20 0.0154(7) 0.0107(7) 0.0136(7) 0.0038(6) -0.0004(6) 0.0024(6) C21 0.0120(7) 0.0141(8) 0.0231(9) 0.0070(7) 0.0037(6) 0.0013(6) C22 0.0153(7) 0.0215(9) 0.0115(7) 0.0048(6) 0.0032(6) 0.0097(7) _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 Cr1 C15 1.8558(17) . ? Cr1 C14 1.8915(17) . ? Cr1 C13 1.8954(16) . ? Cr1 C17 1.9187(17) . ? Cr1 C16 1.9197(16) . ? Cr1 C1 2.1666(15) . ? Cr2 C20 1.8558(16) . ? Cr2 C18 1.8902(16) . ? Cr2 C22 1.9019(16) . ? Cr2 C19 1.9076(16) . ? Cr2 C21 1.9264(16) . ? Cr2 C2 2.2076(15) . ? N1 C1 1.3154(18) . ? N1 C3 1.4757(18) . ? N1 C7 1.4854(18) . ? N2 C2 1.3175(18) . ? N2 C12 1.4745(18) . ? N2 C8 1.4879(19) . ? O1 C13 1.1448(18) . ? O2 C14 1.1488(19) . ? O3 C15 1.1559(19) . ? O4 C16 1.1376(18) . ? O5 C17 1.1423(18) . ? O6 C18 1.1476(18) . ? O7 C19 1.1411(18) . ? O8 C20 1.1520(18) . ? O9 C21 1.1382(18) . ? O10 C22 1.1452(18) . ? C1 C2 1.468(2) . ? C3 C4 1.527(2) . ? C4 C5 1.523(2) . ? C5 C6 1.524(2) . ? C6 C7 1.531(2) . ? C8 C9 1.527(2) . ? C9 C10 1.520(2) . ? C10 C11 1.521(2) . ? C11 C12 1.522(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Cr1 C14 86.44(7) . . ? C15 Cr1 C13 88.72(7) . . ? C14 Cr1 C13 86.36(7) . . ? C15 Cr1 C17 87.85(7) . . ? C14 Cr1 C17 168.46(7) . . ? C13 Cr1 C17 83.50(6) . . ? C15 Cr1 C16 87.55(7) . . ? C14 Cr1 C16 93.36(7) . . ? C13 Cr1 C16 176.27(6) . . ? C17 Cr1 C16 96.41(6) . . ? C15 Cr1 C1 174.89(6) . . ? C14 Cr1 C1 93.08(6) . . ? C13 Cr1 C1 96.33(6) . . ? C17 Cr1 C1 93.49(6) . . ? C16 Cr1 C1 87.40(6) . . ? C20 Cr2 C18 86.24(6) . . ? C20 Cr2 C22 88.63(6) . . ? C18 Cr2 C22 90.04(6) . . ? C20 Cr2 C19 85.65(6) . . ? C18 Cr2 C19 84.82(6) . . ? C22 Cr2 C19 172.54(6) . . ? C20 Cr2 C21 85.48(7) . . ? C18 Cr2 C21 170.05(6) . . ? C22 Cr2 C21 95.25(6) . . ? C19 Cr2 C21 89.07(6) . . ? C20 Cr2 C2 173.81(6) . . ? C18 Cr2 C2 92.77(6) . . ? C22 Cr2 C2 85.26(6) . . ? C19 Cr2 C2 100.35(6) . . ? C21 Cr2 C2 96.05(6) . . ? C1 N1 C3 124.97(12) . . ? C1 N1 C7 124.43(12) . . ? C3 N1 C7 110.57(11) . . ? C2 N2 C12 124.39(13) . . ? C2 N2 C8 124.29(12) . . ? C12 N2 C8 111.32(11) . . ? N1 C1 C2 116.90(13) . . ? N1 C1 Cr1 130.39(10) . . ? C2 C1 Cr1 112.70(10) . . ? N2 C2 C1 117.28(13) . . ? N2 C2 Cr2 130.32(11) . . ? C1 C2 Cr2 112.18(9) . . ? N1 C3 C4 110.86(12) . . ? C5 C4 C3 110.33(13) . . ? C4 C5 C6 110.49(12) . . ? C5 C6 C7 111.66(13) . . ? N1 C7 C6 110.06(12) . . ? N2 C8 C9 110.90(12) . . ? C10 C9 C8 110.34(12) . . ? C9 C10 C11 109.63(12) . . ? C10 C11 C12 111.74(13) . . ? N2 C12 C11 111.67(12) . . ? O1 C13 Cr1 173.94(13) . . ? O2 C14 Cr1 174.29(14) . . ? O3 C15 Cr1 178.32(14) . . ? O4 C16 Cr1 177.61(15) . . ? O5 C17 Cr1 171.15(14) . . ? O6 C18 Cr2 173.30(13) . . ? O7 C19 Cr2 171.45(13) . . ? O8 C20 Cr2 179.23(14) . . ? O9 C21 Cr2 173.64(14) . . ? O10 C22 Cr2 175.66(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 C1 C2 166.68(13) . . . . ? C7 N1 C1 C2 -11.5(2) . . . . ? C3 N1 C1 Cr1 -12.2(2) . . . . ? C7 N1 C1 Cr1 169.70(10) . . . . ? C15 Cr1 C1 N1 57.5(8) . . . . ? C14 Cr1 C1 N1 -26.93(14) . . . . ? C13 Cr1 C1 N1 -113.61(13) . . . . ? C17 Cr1 C1 N1 162.56(13) . . . . ? C16 Cr1 C1 N1 66.29(13) . . . . ? C15 Cr1 C1 C2 -121.4(7) . . . . ? C14 Cr1 C1 C2 154.18(10) . . . . ? C13 Cr1 C1 C2 67.51(11) . . . . ? C17 Cr1 C1 C2 -16.33(10) . . . . ? C16 Cr1 C1 C2 -112.59(11) . . . . ? C12 N2 C2 C1 171.70(13) . . . . ? C8 N2 C2 C1 -8.4(2) . . . . ? C12 N2 C2 Cr2 -14.2(2) . . . . ? C8 N2 C2 Cr2 165.69(10) . . . . ? N1 C1 C2 N2 93.24(16) . . . . ? Cr1 C1 C2 N2 -87.71(13) . . . . ? N1 C1 C2 Cr2 -81.91(14) . . . . ? Cr1 C1 C2 Cr2 97.14(9) . . . . ? C20 Cr2 C2 N2 -65.2(6) . . . . ? C18 Cr2 C2 N2 -145.84(13) . . . . ? C22 Cr2 C2 N2 -56.03(13) . . . . ? C19 Cr2 C2 N2 128.92(13) . . . . ? C21 Cr2 C2 N2 38.77(14) . . . . ? C20 Cr2 C2 C1 109.1(5) . . . . ? C18 Cr2 C2 C1 28.50(11) . . . . ? C22 Cr2 C2 C1 118.31(11) . . . . ? C19 Cr2 C2 C1 -56.73(11) . . . . ? C21 Cr2 C2 C1 -146.89(10) . . . . ? C1 N1 C3 C4 120.62(15) . . . . ? C7 N1 C3 C4 -61.03(16) . . . . ? N1 C3 C4 C5 57.88(16) . . . . ? C3 C4 C5 C6 -53.59(17) . . . . ? C4 C5 C6 C7 53.29(17) . . . . ? C1 N1 C7 C6 -122.19(14) . . . . ? C3 N1 C7 C6 59.45(15) . . . . ? C5 C6 C7 N1 -55.91(16) . . . . ? C2 N2 C8 C9 -122.07(15) . . . . ? C12 N2 C8 C9 57.83(15) . . . . ? N2 C8 C9 C10 -58.10(16) . . . . ? C8 C9 C10 C11 56.00(17) . . . . ? C9 C10 C11 C12 -54.52(17) . . . . ? C2 N2 C12 C11 123.95(15) . . . . ? C8 N2 C12 C11 -55.95(16) . . . . ? C10 C11 C12 N2 54.81(17) . . . . ? C15 Cr1 C13 O1 10.6(13) . . . . ? C14 Cr1 C13 O1 97.1(13) . . . . ? C17 Cr1 C13 O1 -77.4(13) . . . . ? C16 Cr1 C13 O1 11(2) . . . . ? C1 Cr1 C13 O1 -170.2(13) . . . . ? C15 Cr1 C14 O2 38.5(14) . . . . ? C13 Cr1 C14 O2 -50.5(14) . . . . ? C17 Cr1 C14 O2 -22.0(16) . . . . ? C16 Cr1 C14 O2 125.8(14) . . . . ? C1 Cr1 C14 O2 -146.6(14) . . . . ? C14 Cr1 C15 O3 41(5) . . . . ? C13 Cr1 C15 O3 127(5) . . . . ? C17 Cr1 C15 O3 -149(5) . . . . ? C16 Cr1 C15 O3 -53(5) . . . . ? C1 Cr1 C15 O3 -44(6) . . . . ? C15 Cr1 C16 O4 48(3) . . . . ? C14 Cr1 C16 O4 -38(3) . . . . ? C13 Cr1 C16 O4 47(4) . . . . ? C17 Cr1 C16 O4 136(3) . . . . ? C1 Cr1 C16 O4 -131(3) . . . . ? C15 Cr1 C17 O5 -48.8(9) . . . . ? C14 Cr1 C17 O5 11.6(11) . . . . ? C13 Cr1 C17 O5 40.2(9) . . . . ? C16 Cr1 C17 O5 -136.1(9) . . . . ? C1 Cr1 C17 O5 136.2(9) . . . . ? C20 Cr2 C18 O6 23.6(11) . . . . ? C22 Cr2 C18 O6 112.2(11) . . . . ? C19 Cr2 C18 O6 -62.4(11) . . . . ? C21 Cr2 C18 O6 -10.1(14) . . . . ? C2 Cr2 C18 O6 -162.6(11) . . . . ? C20 Cr2 C19 O7 -22.4(9) . . . . ? C18 Cr2 C19 O7 64.2(9) . . . . ? C22 Cr2 C19 O7 17.6(12) . . . . ? C21 Cr2 C19 O7 -107.9(9) . . . . ? C2 Cr2 C19 O7 156.1(9) . . . . ? C18 Cr2 C20 O8 -38(10) . . . . ? C22 Cr2 C20 O8 -128(10) . . . . ? C19 Cr2 C20 O8 47(10) . . . . ? C21 Cr2 C20 O8 137(10) . . . . ? C2 Cr2 C20 O8 -119(10) . . . . ? C20 Cr2 C21 O9 -13.1(12) . . . . ? C18 Cr2 C21 O9 20.6(15) . . . . ? C22 Cr2 C21 O9 -101.3(12) . . . . ? C19 Cr2 C21 O9 72.6(12) . . . . ? C2 Cr2 C21 O9 172.9(12) . . . . ? C20 Cr2 C22 O10 62.3(18) . . . . ? C18 Cr2 C22 O10 -23.9(18) . . . . ? C19 Cr2 C22 O10 22(2) . . . . ? C21 Cr2 C22 O10 147.6(18) . . . . ? C2 Cr2 C22 O10 -116.7(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.367 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.055 #============================================================================= # end of cif data for "pet09" (compound 2a) #============================================================================= #============================================================================= # cif data for "pet20" (compound 2b) #============================================================================= data_pet20 _database_code_depnum_ccdc_archive 'CCDC 819866' #TrackingRef 'pet-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H20 N2 O10 W2' _chemical_formula_weight 840.10 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _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 9.5233(4) _cell_length_b 9.7656(4) _cell_length_c 15.9927(6) _cell_angle_alpha 102.934(4) _cell_angle_beta 94.073(4) _cell_angle_gamma 118.147(4) _cell_volume 1250.88(9) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 21466 _cell_measurement_theta_min 2.4381 _cell_measurement_theta_max 30.8563 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 9.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63113 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48699 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7185 _reflns_number_gt 5478 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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^)+(0.0042P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7185 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_ref 0.0236 _refine_ls_wR_factor_gt 0.0231 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _refine_ls_shift/su_max 0.004 _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 W1 W 0.767013(12) 0.738059(12) 0.838857(7) 0.01263(3) Uani 1 1 d . . . W2 W 0.800824(12) 0.368426(12) 0.626462(6) 0.01109(3) Uani 1 1 d . . . N1 N 0.7028(2) 0.3801(2) 0.84800(12) 0.0111(4) Uani 1 1 d . . . N2 N 0.4577(2) 0.3288(2) 0.68333(12) 0.0107(4) Uani 1 1 d . . . O1 O 0.4148(2) 0.6980(2) 0.80475(11) 0.0236(4) Uani 1 1 d . . . O2 O 0.7349(2) 0.7576(2) 1.03675(11) 0.0272(5) Uani 1 1 d . . . O3 O 0.9070(2) 1.1156(2) 0.90103(12) 0.0286(5) Uani 1 1 d . . . O4 O 1.1365(2) 0.8220(2) 0.87663(12) 0.0298(5) Uani 1 1 d . . . O5 O 0.7397(2) 0.7541(2) 0.64144(11) 0.0262(5) Uani 1 1 d . . . O6 O 1.0191(2) 0.3741(2) 0.78793(11) 0.0233(4) Uani 1 1 d . . . O7 O 1.0855(2) 0.7362(2) 0.67263(11) 0.0226(4) Uani 1 1 d . . . O8 O 1.0310(2) 0.2948(2) 0.51663(11) 0.0197(4) Uani 1 1 d . . . O9 O 0.6564(2) 0.3935(2) 0.44693(11) 0.0277(5) Uani 1 1 d . . . O10 O 0.5747(2) -0.0137(2) 0.58676(11) 0.0245(4) Uani 1 1 d . . . C1 C 0.6894(3) 0.4696(3) 0.80111(15) 0.0107(5) Uani 1 1 d . . . C2 C 0.6141(3) 0.3871(3) 0.70664(15) 0.0111(5) Uani 1 1 d . . . C3 C 0.8003(3) 0.4457(3) 0.93764(14) 0.0146(5) Uani 1 1 d . . . H3A H 0.8548 0.5658 0.9557 0.018 Uiso 1 1 calc R . . H3B H 0.8855 0.4148 0.9390 0.018 Uiso 1 1 calc R . . C4 C 0.6923(3) 0.3803(3) 1.00165(15) 0.0186(6) Uani 1 1 d . . . H4A H 0.7600 0.4231 1.0613 0.022 Uiso 1 1 calc R . . H4B H 0.6119 0.4174 1.0033 0.022 Uiso 1 1 calc R . . C5 C 0.6038(3) 0.1953(3) 0.97368(15) 0.0189(6) Uani 1 1 d . . . H5A H 0.5252 0.1543 1.0117 0.023 Uiso 1 1 calc R . . H5B H 0.6833 0.1585 0.9809 0.023 Uiso 1 1 calc R . . C6 C 0.5135(3) 0.1261(3) 0.87816(15) 0.0155(6) Uani 1 1 d . . . H6A H 0.4682 0.0071 0.8593 0.019 Uiso 1 1 calc R . . H6B H 0.4216 0.1470 0.8731 0.019 Uiso 1 1 calc R . . C7 C 0.6245(3) 0.2009(3) 0.81819(15) 0.0126(5) Uani 1 1 d . . . H7A H 0.7092 0.1694 0.8177 0.015 Uiso 1 1 calc R . . H7B H 0.5605 0.1590 0.7576 0.015 Uiso 1 1 calc R . . C8 C 0.3468(3) 0.3201(3) 0.74510(15) 0.0139(5) Uani 1 1 d . . . H8A H 0.2988 0.3880 0.7373 0.017 Uiso 1 1 calc R . . H8B H 0.4094 0.3637 0.8061 0.017 Uiso 1 1 calc R . . C9 C 0.2115(3) 0.1459(3) 0.72961(15) 0.0155(6) Uani 1 1 d . . . H9A H 0.1379 0.1430 0.7707 0.019 Uiso 1 1 calc R . . H9B H 0.2588 0.0791 0.7407 0.019 Uiso 1 1 calc R . . C10 C 0.1153(3) 0.0763(3) 0.63550(15) 0.0161(6) Uani 1 1 d . . . H10A H 0.0586 0.1361 0.6261 0.019 Uiso 1 1 calc R . . H10B H 0.0323 -0.0393 0.6246 0.019 Uiso 1 1 calc R . . C11 C 0.2306(3) 0.0912(3) 0.57218(16) 0.0184(6) Uani 1 1 d . . . H11A H 0.2761 0.0199 0.5767 0.022 Uiso 1 1 calc R . . H11B H 0.1689 0.0540 0.5114 0.022 Uiso 1 1 calc R . . C12 C 0.3684(3) 0.2638(3) 0.59117(15) 0.0150(6) Uani 1 1 d . . . H12A H 0.4444 0.2671 0.5515 0.018 Uiso 1 1 calc R . . H12B H 0.3242 0.3330 0.5797 0.018 Uiso 1 1 calc R . . C13 C 0.5385(3) 0.7057(3) 0.81714(16) 0.0161(6) Uani 1 1 d . . . C14 C 0.7497(3) 0.7470(3) 0.96478(18) 0.0192(6) Uani 1 1 d . . . C15 C 0.8531(3) 0.9763(3) 0.87643(17) 0.0181(6) Uani 1 1 d . . . C16 C 1.0035(3) 0.7882(3) 0.86153(16) 0.0169(6) Uani 1 1 d . . . C17 C 0.7565(3) 0.7432(3) 0.71094(18) 0.0181(6) Uani 1 1 d . . . C18 C 0.9331(3) 0.3691(3) 0.73110(16) 0.0156(6) Uani 1 1 d . . . C19 C 0.9755(3) 0.6074(3) 0.65641(15) 0.0152(6) Uani 1 1 d . . . C20 C 0.9468(3) 0.3237(3) 0.55671(15) 0.0146(6) Uani 1 1 d . . . C21 C 0.7012(3) 0.3842(3) 0.51288(17) 0.0186(6) Uani 1 1 d . . . C22 C 0.6512(3) 0.1241(3) 0.59919(15) 0.0157(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01057(6) 0.01024(6) 0.01517(6) 0.00182(5) 0.00120(5) 0.00475(5) W2 0.01047(6) 0.01076(6) 0.01107(6) 0.00345(5) 0.00213(5) 0.00449(5) N1 0.0121(11) 0.0129(11) 0.0096(11) 0.0043(9) 0.0031(9) 0.0068(9) N2 0.0095(11) 0.0112(10) 0.0094(11) 0.0025(9) 0.0009(8) 0.0039(9) O1 0.0168(10) 0.0238(11) 0.0307(11) 0.0038(9) 0.0027(9) 0.0126(9) O2 0.0276(12) 0.0409(13) 0.0166(11) 0.0038(9) 0.0062(9) 0.0217(11) O3 0.0207(11) 0.0162(10) 0.0451(13) 0.0040(10) -0.0006(10) 0.0093(9) O4 0.0162(11) 0.0454(13) 0.0264(11) 0.0122(10) 0.0016(9) 0.0140(10) O5 0.0252(11) 0.0338(12) 0.0256(11) 0.0168(10) 0.0066(9) 0.0157(10) O6 0.0195(11) 0.0358(12) 0.0186(10) 0.0102(9) 0.0032(9) 0.0160(10) O7 0.0220(11) 0.0168(10) 0.0211(10) 0.0046(8) 0.0040(9) 0.0041(9) O8 0.0198(10) 0.0211(10) 0.0195(10) 0.0066(8) 0.0101(8) 0.0103(9) O9 0.0222(11) 0.0295(12) 0.0228(11) 0.0142(9) -0.0035(9) 0.0046(9) O10 0.0288(12) 0.0142(10) 0.0234(11) 0.0034(8) 0.0042(9) 0.0064(9) C1 0.0068(12) 0.0136(12) 0.0133(13) 0.0038(10) 0.0043(10) 0.0062(10) C2 0.0124(13) 0.0061(11) 0.0150(13) 0.0048(10) 0.0011(10) 0.0043(10) C3 0.0117(13) 0.0166(13) 0.0138(13) 0.0032(11) -0.0022(11) 0.0068(11) C4 0.0191(15) 0.0223(15) 0.0117(13) 0.0045(11) 0.0011(11) 0.0087(12) C5 0.0233(15) 0.0213(15) 0.0161(14) 0.0098(12) 0.0056(12) 0.0122(13) C6 0.0165(14) 0.0138(13) 0.0192(14) 0.0084(11) 0.0050(11) 0.0082(11) C7 0.0160(13) 0.0104(12) 0.0132(13) 0.0039(10) 0.0035(11) 0.0079(11) C8 0.0113(13) 0.0142(13) 0.0153(14) 0.0026(11) 0.0035(11) 0.0065(11) C9 0.0095(13) 0.0180(14) 0.0173(14) 0.0040(11) 0.0024(11) 0.0061(11) C10 0.0108(13) 0.0104(13) 0.0226(15) 0.0035(11) 0.0010(11) 0.0027(11) C11 0.0144(14) 0.0165(14) 0.0163(14) 0.0011(11) -0.0030(11) 0.0040(12) C12 0.0098(13) 0.0196(14) 0.0138(14) 0.0053(11) -0.0001(11) 0.0061(11) C13 0.0206(15) 0.0100(13) 0.0159(14) 0.0016(11) 0.0037(12) 0.0071(12) C14 0.0109(14) 0.0157(14) 0.0277(16) -0.0021(12) 0.0002(12) 0.0084(12) C15 0.0104(13) 0.0197(14) 0.0250(15) 0.0047(12) 0.0014(12) 0.0094(12) C16 0.0189(15) 0.0155(14) 0.0153(14) 0.0063(11) 0.0024(12) 0.0072(12) C17 0.0088(13) 0.0141(13) 0.0328(17) 0.0066(12) 0.0048(12) 0.0068(11) C18 0.0137(13) 0.0157(13) 0.0186(14) 0.0042(11) 0.0098(12) 0.0077(11) C19 0.0209(15) 0.0197(14) 0.0123(13) 0.0063(11) 0.0060(11) 0.0148(13) C20 0.0146(14) 0.0114(13) 0.0111(13) 0.0049(11) -0.0043(11) 0.0016(11) C21 0.0126(14) 0.0126(13) 0.0239(16) 0.0044(12) 0.0035(12) 0.0017(11) C22 0.0154(14) 0.0240(15) 0.0109(14) 0.0061(12) 0.0068(11) 0.0115(13) _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 W1 C15 1.987(3) . ? W1 C14 2.018(3) . ? W1 C13 2.037(3) . ? W1 C16 2.052(3) . ? W1 C17 2.054(3) . ? W1 C1 2.277(2) . ? W2 C20 1.985(3) . ? W2 C18 2.018(3) . ? W2 C22 2.038(3) . ? W2 C19 2.041(3) . ? W2 C21 2.060(3) . ? W2 C2 2.316(2) . ? N1 C1 1.315(3) . ? N1 C3 1.472(3) . ? N1 C7 1.480(3) . ? N2 C2 1.306(3) . ? N2 C12 1.481(3) . ? N2 C8 1.483(3) . ? O1 C13 1.145(3) . ? O2 C14 1.157(3) . ? O3 C15 1.159(3) . ? O4 C16 1.139(3) . ? O5 C17 1.147(3) . ? O6 C18 1.156(3) . ? O7 C19 1.148(3) . ? O8 C20 1.158(3) . ? O9 C21 1.148(3) . ? O10 C22 1.147(3) . ? C1 C2 1.484(3) . ? C3 C4 1.529(3) . ? C4 C5 1.524(3) . ? C5 C6 1.527(3) . ? C6 C7 1.516(3) . ? C8 C9 1.521(3) . ? C9 C10 1.525(3) . ? C10 C11 1.525(3) . ? C11 C12 1.510(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 W1 C14 86.36(10) . . ? C15 W1 C13 88.30(9) . . ? C14 W1 C13 87.87(10) . . ? C15 W1 C16 87.62(10) . . ? C14 W1 C16 92.75(10) . . ? C13 W1 C16 175.83(9) . . ? C15 W1 C17 88.90(10) . . ? C14 W1 C17 170.07(9) . . ? C13 W1 C17 83.26(9) . . ? C16 W1 C17 95.78(9) . . ? C15 W1 C1 175.19(9) . . ? C14 W1 C1 92.54(9) . . ? C13 W1 C1 96.35(9) . . ? C16 W1 C1 87.75(9) . . ? C17 W1 C1 92.88(9) . . ? C20 W2 C18 86.63(9) . . ? C20 W2 C22 88.43(10) . . ? C18 W2 C22 90.22(10) . . ? C20 W2 C19 85.95(10) . . ? C18 W2 C19 84.35(10) . . ? C22 W2 C19 172.40(10) . . ? C20 W2 C21 85.66(9) . . ? C18 W2 C21 170.64(10) . . ? C22 W2 C21 94.88(10) . . ? C19 W2 C21 89.80(9) . . ? C20 W2 C2 172.99(9) . . ? C18 W2 C2 92.07(9) . . ? C22 W2 C2 84.69(9) . . ? C19 W2 C2 100.78(9) . . ? C21 W2 C2 96.21(9) . . ? C1 N1 C3 124.2(2) . . ? C1 N1 C7 125.13(19) . . ? C3 N1 C7 110.65(17) . . ? C2 N2 C12 124.1(2) . . ? C2 N2 C8 124.8(2) . . ? C12 N2 C8 111.13(18) . . ? N1 C1 C2 116.7(2) . . ? N1 C1 W1 131.03(17) . . ? C2 C1 W1 112.28(15) . . ? N2 C2 C1 117.4(2) . . ? N2 C2 W2 130.96(17) . . ? C1 C2 W2 111.43(15) . . ? N1 C3 C4 110.52(19) . . ? C5 C4 C3 110.4(2) . . ? C4 C5 C6 110.72(19) . . ? C7 C6 C5 111.7(2) . . ? N1 C7 C6 110.66(18) . . ? N2 C8 C9 110.90(18) . . ? C8 C9 C10 110.10(19) . . ? C9 C10 C11 109.62(19) . . ? C12 C11 C10 111.9(2) . . ? N2 C12 C11 111.23(19) . . ? O1 C13 W1 175.4(2) . . ? O2 C14 W1 175.7(2) . . ? O3 C15 W1 177.4(2) . . ? O4 C16 W1 177.1(2) . . ? O5 C17 W1 172.2(2) . . ? O6 C18 W2 174.7(2) . . ? O7 C19 W2 172.7(2) . . ? O8 C20 W2 178.5(2) . . ? O9 C21 W2 174.4(2) . . ? O10 C22 W2 175.8(2) . . ? 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 C3 N1 C1 C2 168.1(2) . . . . ? C7 N1 C1 C2 -11.1(3) . . . . ? C3 N1 C1 W1 -10.7(3) . . . . ? C7 N1 C1 W1 170.16(16) . . . . ? C15 W1 C1 N1 50.0(12) . . . . ? C14 W1 C1 N1 -26.7(2) . . . . ? C13 W1 C1 N1 -114.8(2) . . . . ? C16 W1 C1 N1 66.0(2) . . . . ? C17 W1 C1 N1 161.7(2) . . . . ? C15 W1 C1 C2 -128.8(11) . . . . ? C14 W1 C1 C2 154.57(17) . . . . ? C13 W1 C1 C2 66.44(17) . . . . ? C16 W1 C1 C2 -112.77(17) . . . . ? C17 W1 C1 C2 -17.10(17) . . . . ? C12 N2 C2 C1 171.2(2) . . . . ? C8 N2 C2 C1 -8.2(3) . . . . ? C12 N2 C2 W2 -14.3(3) . . . . ? C8 N2 C2 W2 166.25(16) . . . . ? N1 C1 C2 N2 93.8(3) . . . . ? W1 C1 C2 N2 -87.2(2) . . . . ? N1 C1 C2 W2 -81.7(2) . . . . ? W1 C1 C2 W2 97.26(13) . . . . ? C20 W2 C2 N2 -68.1(8) . . . . ? C18 W2 C2 N2 -147.2(2) . . . . ? C22 W2 C2 N2 -57.2(2) . . . . ? C19 W2 C2 N2 128.1(2) . . . . ? C21 W2 C2 N2 37.1(2) . . . . ? C20 W2 C2 C1 106.7(7) . . . . ? C18 W2 C2 C1 27.51(16) . . . . ? C22 W2 C2 C1 117.54(16) . . . . ? C19 W2 C2 C1 -57.13(16) . . . . ? C21 W2 C2 C1 -148.11(16) . . . . ? C1 N1 C3 C4 119.5(2) . . . . ? C7 N1 C3 C4 -61.2(2) . . . . ? N1 C3 C4 C5 57.7(3) . . . . ? C3 C4 C5 C6 -52.9(3) . . . . ? C4 C5 C6 C7 52.2(3) . . . . ? C1 N1 C7 C6 -120.9(2) . . . . ? C3 N1 C7 C6 59.8(2) . . . . ? C5 C6 C7 N1 -55.3(3) . . . . ? C2 N2 C8 C9 -121.7(2) . . . . ? C12 N2 C8 C9 58.8(2) . . . . ? N2 C8 C9 C10 -58.4(2) . . . . ? C8 C9 C10 C11 55.5(3) . . . . ? C9 C10 C11 C12 -54.5(3) . . . . ? C2 N2 C12 C11 123.6(2) . . . . ? C8 N2 C12 C11 -56.9(2) . . . . ? C10 C11 C12 N2 55.2(3) . . . . ? C15 W1 C13 O1 19(3) . . . . ? C14 W1 C13 O1 106(3) . . . . ? C16 W1 C13 O1 7(4) . . . . ? C17 W1 C13 O1 -70(3) . . . . ? C1 W1 C13 O1 -162(3) . . . . ? C15 W1 C14 O2 49(3) . . . . ? C13 W1 C14 O2 -39(3) . . . . ? C16 W1 C14 O2 137(3) . . . . ? C17 W1 C14 O2 -13(4) . . . . ? C1 W1 C14 O2 -136(3) . . . . ? C14 W1 C15 O3 46(5) . . . . ? C13 W1 C15 O3 134(5) . . . . ? C16 W1 C15 O3 -47(5) . . . . ? C17 W1 C15 O3 -143(5) . . . . ? C1 W1 C15 O3 -31(6) . . . . ? C15 W1 C16 O4 26(5) . . . . ? C14 W1 C16 O4 -60(5) . . . . ? C13 W1 C16 O4 39(5) . . . . ? C17 W1 C16 O4 115(5) . . . . ? C1 W1 C16 O4 -152(5) . . . . ? C15 W1 C17 O5 -55.9(16) . . . . ? C14 W1 C17 O5 6(2) . . . . ? C13 W1 C17 O5 32.5(16) . . . . ? C16 W1 C17 O5 -143.4(16) . . . . ? C1 W1 C17 O5 128.6(16) . . . . ? C20 W2 C18 O6 31(2) . . . . ? C22 W2 C18 O6 120(2) . . . . ? C19 W2 C18 O6 -55(2) . . . . ? C21 W2 C18 O6 -3(3) . . . . ? C2 W2 C18 O6 -156(2) . . . . ? C20 W2 C19 O7 -31.6(17) . . . . ? C18 W2 C19 O7 55.4(17) . . . . ? C22 W2 C19 O7 11(2) . . . . ? C21 W2 C19 O7 -117.3(17) . . . . ? C2 W2 C19 O7 146.4(16) . . . . ? C18 W2 C20 O8 57(8) . . . . ? C22 W2 C20 O8 -34(8) . . . . ? C19 W2 C20 O8 141(8) . . . . ? C21 W2 C20 O8 -129(8) . . . . ? C2 W2 C20 O8 -23(9) . . . . ? C20 W2 C21 O9 -13(2) . . . . ? C18 W2 C21 O9 21(3) . . . . ? C22 W2 C21 O9 -101(2) . . . . ? C19 W2 C21 O9 73(2) . . . . ? C2 W2 C21 O9 174(2) . . . . ? C20 W2 C22 O10 65(3) . . . . ? C18 W2 C22 O10 -22(3) . . . . ? C19 W2 C22 O10 23(3) . . . . ? C21 W2 C22 O10 150(3) . . . . ? C2 W2 C22 O10 -114(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.626 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.117 #============================================================================= # end of cif data for "pet20" (compound 2b) #============================================================================= #============================================================================= # cif data for "pet10" (compound 3) #============================================================================= data_pet10 _database_code_depnum_ccdc_archive 'CCDC 819867' #TrackingRef 'pet-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H54 Cl4 N2 Ru2' _chemical_formula_weight 882.77 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' 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.3697(6) _cell_length_b 9.7250(2) _cell_length_c 22.3104(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.454(2) _cell_angle_gamma 90.00 _cell_volume 3751.62(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15428 _cell_measurement_theta_min 2.3491 _cell_measurement_theta_max 29.2439 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98008 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64425 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4458 _reflns_number_gt 2813 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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^)+(0.0191P)^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 'methyls rigid and other riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4458 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0429 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 0.785 _refine_ls_restrained_S_all 0.785 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.011321(9) 0.49939(2) 0.347200(7) 0.01153(5) Uani 1 1 d . . . Cl1 Cl -0.12579(3) 0.49039(7) 0.316437(19) 0.01563(11) Uani 1 1 d . . . Cl2 Cl -0.00618(3) 0.29765(6) 0.40751(2) 0.01715(13) Uani 1 1 d . . . N N 0.08311(10) 0.26795(17) 0.27964(7) 0.0125(4) Uani 1 1 d . . . C1 C 0.02801(12) 0.3597(2) 0.27798(8) 0.0108(5) Uani 1 1 d . . . C2 C 0.09804(13) 0.1743(2) 0.22959(9) 0.0177(5) Uani 1 1 d . . . H2A H 0.1454 0.2045 0.2120 0.021 Uiso 1 1 calc R . . H2B H 0.0544 0.1802 0.1977 0.021 Uiso 1 1 calc R . . C3 C 0.10787(12) 0.0257(2) 0.25022(9) 0.0198(6) Uani 1 1 d . . . H3A H 0.1222 -0.0311 0.2162 0.024 Uiso 1 1 calc R . . H3B H 0.0579 -0.0088 0.2622 0.024 Uiso 1 1 calc R . . C4 C 0.16954(12) 0.0100(3) 0.30301(9) 0.0209(5) Uani 1 1 d . . . H4A H 0.1703 -0.0860 0.3179 0.025 Uiso 1 1 calc R . . H4B H 0.2211 0.0314 0.2899 0.025 Uiso 1 1 calc R . . C5 C 0.15164(13) 0.1072(2) 0.35282(9) 0.0206(5) Uani 1 1 d . . . H5A H 0.1934 0.1018 0.3862 0.025 Uiso 1 1 calc R . . H5B H 0.1027 0.0790 0.3687 0.025 Uiso 1 1 calc R . . C6 C 0.14434(12) 0.2541(2) 0.33017(9) 0.0165(5) Uani 1 1 d . . . H6A H 0.1322 0.3150 0.3636 0.020 Uiso 1 1 calc R . . H6B H 0.1944 0.2840 0.3167 0.020 Uiso 1 1 calc R . . C7 C -0.01318(13) 0.7065(2) 0.38964(9) 0.0131(5) Uani 1 1 d . . . C8 C 0.01091(12) 0.7192(2) 0.32995(9) 0.0149(5) Uani 1 1 d . . . H8 H -0.0217 0.7659 0.3000 0.018 Uiso 1 1 calc R . . C9 C 0.08102(12) 0.6646(2) 0.31489(9) 0.0161(5) Uani 1 1 d . . . H9 H 0.0952 0.6751 0.2750 0.019 Uiso 1 1 calc R . . C10 C 0.13134(13) 0.5937(2) 0.35815(9) 0.0159(5) Uani 1 1 d . . . C11 C 0.10406(13) 0.5707(2) 0.41464(9) 0.0158(5) Uani 1 1 d . . . H11 H 0.1335 0.5141 0.4430 0.019 Uiso 1 1 calc R . . C12 C 0.03360(13) 0.6296(2) 0.43080(9) 0.0148(5) Uani 1 1 d . . . H12 H 0.0186 0.6158 0.4702 0.018 Uiso 1 1 calc R . . C13 C -0.08795(13) 0.7737(2) 0.40320(9) 0.0187(5) Uani 1 1 d . . . H13 H -0.1232 0.7757 0.3651 0.022 Uiso 1 1 calc R . . C14 C -0.12951(13) 0.6985(3) 0.45030(9) 0.0245(6) Uani 1 1 d . . . H14A H -0.1383 0.6027 0.4378 0.029 Uiso 1 1 calc R . . H14B H -0.1793 0.7432 0.4545 0.029 Uiso 1 1 calc R . . H14C H -0.0977 0.7009 0.4890 0.029 Uiso 1 1 calc R . . C15 C -0.07011(14) 0.9221(2) 0.42190(11) 0.0304(6) Uani 1 1 d . . . H15A H -0.0375 0.9231 0.4603 0.036 Uiso 1 1 calc R . . H15B H -0.1185 0.9710 0.4265 0.036 Uiso 1 1 calc R . . H15C H -0.0428 0.9676 0.3909 0.036 Uiso 1 1 calc R . . C16 C 0.21135(12) 0.5553(2) 0.34455(10) 0.0204(5) Uani 1 1 d . . . H16A H 0.2097 0.5195 0.3034 0.025 Uiso 1 1 calc R . . H16B H 0.2320 0.4845 0.3730 0.025 Uiso 1 1 calc R . . H16C H 0.2447 0.6366 0.3484 0.025 Uiso 1 1 calc R . . C17 C 0.20008(14) 0.8533(2) 0.47906(10) 0.0249(6) Uani 1 1 d . . . H17 H 0.1655 0.9244 0.4648 0.030 Uiso 1 1 calc R . . C18 C 0.18325(13) 0.7717(2) 0.52676(10) 0.0242(6) Uani 1 1 d . . . H18 H 0.1369 0.7869 0.5453 0.029 Uiso 1 1 calc R . . C19 C 0.23275(14) 0.6690(2) 0.54763(9) 0.0226(6) Uani 1 1 d . . . H19 H 0.2207 0.6132 0.5805 0.027 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 Ru 0.01307(8) 0.01545(8) 0.00598(7) -0.00021(10) 0.00040(5) -0.00110(11) Cl1 0.0119(2) 0.0224(3) 0.0126(2) -0.0022(3) 0.00081(17) 0.0004(3) Cl2 0.0218(3) 0.0211(3) 0.0086(3) 0.0027(3) 0.0018(2) -0.0035(3) N 0.0142(10) 0.0152(10) 0.0077(9) 0.0010(7) -0.0012(7) -0.0012(8) C1 0.0094(12) 0.0152(12) 0.0081(11) 0.0031(9) 0.0020(8) -0.0036(9) C2 0.0187(13) 0.0238(13) 0.0109(11) -0.0033(10) 0.0034(9) 0.0049(11) C3 0.0147(11) 0.0221(17) 0.0221(12) -0.0054(10) -0.0005(9) 0.0029(10) C4 0.0149(11) 0.0174(12) 0.0294(12) 0.0064(13) -0.0026(8) 0.0038(13) C5 0.0214(14) 0.0221(14) 0.0171(12) 0.0053(10) -0.0051(10) 0.0024(11) C6 0.0120(12) 0.0222(13) 0.0145(11) -0.0006(9) -0.0034(9) -0.0006(10) C7 0.0147(13) 0.0090(12) 0.0157(12) -0.0051(9) 0.0008(10) -0.0040(10) C8 0.0231(13) 0.0105(12) 0.0106(11) -0.0009(9) -0.0015(10) -0.0013(10) C9 0.0214(13) 0.0165(13) 0.0105(11) -0.0013(9) 0.0024(9) -0.0072(10) C10 0.0172(12) 0.0169(13) 0.0132(11) -0.0046(9) -0.0005(9) -0.0053(10) C11 0.0191(13) 0.0175(12) 0.0095(11) -0.0027(9) -0.0049(9) -0.0025(10) C12 0.0225(13) 0.0138(12) 0.0078(10) -0.0036(9) 0.0008(9) -0.0048(10) C13 0.0210(13) 0.0211(13) 0.0138(11) -0.0032(10) 0.0009(9) 0.0019(11) C14 0.0215(14) 0.0362(15) 0.0161(12) -0.0054(11) 0.0042(10) 0.0014(12) C15 0.0305(16) 0.0245(15) 0.0360(15) -0.0111(12) 0.0021(12) 0.0048(12) C16 0.0184(13) 0.0238(13) 0.0195(12) -0.0051(10) 0.0037(10) -0.0062(10) C17 0.0280(15) 0.0198(14) 0.0256(13) -0.0033(11) -0.0040(11) 0.0016(11) C18 0.0201(14) 0.0284(15) 0.0253(13) -0.0115(11) 0.0079(11) -0.0067(12) C19 0.0351(16) 0.0207(14) 0.0122(11) -0.0001(10) 0.0030(10) -0.0103(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C1 2.097(2) . ? Ru C8 2.172(2) . ? Ru C9 2.175(2) . ? Ru C11 2.209(2) . ? Ru C12 2.257(2) . ? Ru C10 2.270(2) . ? Ru C7 2.283(2) . ? Ru Cl2 2.4144(6) . ? Ru Cl1 2.4166(5) . ? N C1 1.307(2) . ? N C6 1.481(2) . ? N C2 1.483(2) . ? C1 C1 1.508(4) 2 ? C2 C3 1.521(3) . ? C3 C4 1.523(3) . ? C4 C5 1.514(3) . ? C5 C6 1.517(3) . ? C7 C12 1.386(3) . ? C7 C8 1.439(3) . ? C7 C13 1.510(3) . ? C8 C9 1.398(3) . ? C9 C10 1.418(3) . ? C10 C11 1.406(3) . ? C10 C16 1.498(3) . ? C11 C12 1.428(3) . ? C13 C14 1.518(3) . ? C13 C15 1.526(3) . ? C17 C19 1.377(3) 7_566 ? C17 C18 1.381(3) . ? C18 C19 1.371(3) . ? C19 C17 1.377(3) 7_566 ? 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 C1 Ru C8 120.35(7) . . ? C1 Ru C9 96.55(8) . . ? C8 Ru C9 37.53(8) . . ? C1 Ru C11 124.20(8) . . ? C8 Ru C11 78.55(8) . . ? C9 Ru C11 66.48(8) . . ? C1 Ru C12 161.24(8) . . ? C8 Ru C12 65.91(7) . . ? C9 Ru C12 78.61(8) . . ? C11 Ru C12 37.28(8) . . ? C1 Ru C10 98.70(8) . . ? C8 Ru C10 66.96(8) . . ? C9 Ru C10 37.12(7) . . ? C11 Ru C10 36.56(7) . . ? C12 Ru C10 66.47(8) . . ? C1 Ru C7 157.08(8) . . ? C8 Ru C7 37.58(7) . . ? C9 Ru C7 67.50(8) . . ? C11 Ru C7 65.98(8) . . ? C12 Ru C7 35.55(7) . . ? C10 Ru C7 78.71(8) . . ? C1 Ru Cl2 85.27(5) . . ? C8 Ru Cl2 154.16(5) . . ? C9 Ru Cl2 152.66(6) . . ? C11 Ru Cl2 89.88(6) . . ? C12 Ru Cl2 90.92(6) . . ? C10 Ru Cl2 115.57(6) . . ? C7 Ru Cl2 116.59(6) . . ? C1 Ru Cl1 88.22(6) . . ? C8 Ru Cl1 89.93(6) . . ? C9 Ru Cl1 119.81(6) . . ? C11 Ru Cl1 147.14(6) . . ? C12 Ru Cl1 109.99(6) . . ? C10 Ru Cl1 156.29(6) . . ? C7 Ru Cl1 86.11(6) . . ? Cl2 Ru Cl1 87.48(2) . . ? C1 N C6 123.71(17) . . ? C1 N C2 125.33(17) . . ? C6 N C2 110.68(17) . . ? N C1 C1 115.88(16) . 2 ? N C1 Ru 125.01(14) . . ? C1 C1 Ru 119.09(13) 2 . ? N C2 C3 112.21(17) . . ? C2 C3 C4 112.35(19) . . ? C5 C4 C3 109.06(18) . . ? C4 C5 C6 111.11(18) . . ? N C6 C5 111.76(17) . . ? C12 C7 C8 117.1(2) . . ? C12 C7 C13 124.20(19) . . ? C8 C7 C13 118.67(19) . . ? C12 C7 Ru 71.20(12) . . ? C8 C7 Ru 67.01(12) . . ? C13 C7 Ru 131.52(15) . . ? C9 C8 C7 121.77(19) . . ? C9 C8 Ru 71.38(12) . . ? C7 C8 Ru 75.41(12) . . ? C8 C9 C10 121.04(19) . . ? C8 C9 Ru 71.09(12) . . ? C10 C9 Ru 75.05(12) . . ? C11 C10 C9 116.7(2) . . ? C11 C10 C16 122.7(2) . . ? C9 C10 C16 120.49(19) . . ? C11 C10 Ru 69.37(12) . . ? C9 C10 Ru 67.83(12) . . ? C16 C10 Ru 137.54(15) . . ? C10 C11 C12 122.2(2) . . ? C10 C11 Ru 74.07(12) . . ? C12 C11 Ru 73.19(12) . . ? C7 C12 C11 120.8(2) . . ? C7 C12 Ru 73.25(12) . . ? C11 C12 Ru 69.53(11) . . ? C7 C13 C14 113.87(19) . . ? C7 C13 C15 107.95(19) . . ? C14 C13 C15 111.36(19) . . ? C19 C17 C18 119.5(2) 7_566 . ? C19 C18 C17 120.6(2) . . ? C18 C19 C17 119.9(2) . 7_566 ? 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 C6 N C1 C1 178.70(18) . . . 2 ? C2 N C1 C1 5.4(3) . . . 2 ? C6 N C1 Ru -3.0(3) . . . . ? C2 N C1 Ru -176.27(15) . . . . ? C8 Ru C1 N 122.28(17) . . . . ? C9 Ru C1 N 91.35(18) . . . . ? C11 Ru C1 N 25.4(2) . . . . ? C12 Ru C1 N 17.6(3) . . . . ? C10 Ru C1 N 53.95(18) . . . . ? C7 Ru C1 N 135.50(19) . . . . ? Cl2 Ru C1 N -61.23(17) . . . . ? Cl1 Ru C1 N -148.84(17) . . . . ? C8 Ru C1 C1 -59.45(18) . . . 2 ? C9 Ru C1 C1 -90.38(16) . . . 2 ? C11 Ru C1 C1 -156.33(15) . . . 2 ? C12 Ru C1 C1 -164.1(2) . . . 2 ? C10 Ru C1 C1 -127.78(16) . . . 2 ? C7 Ru C1 C1 -46.2(3) . . . 2 ? Cl2 Ru C1 C1 117.04(15) . . . 2 ? Cl1 Ru C1 C1 29.43(15) . . . 2 ? C1 N C2 C3 -131.4(2) . . . . ? C6 N C2 C3 54.6(2) . . . . ? N C2 C3 C4 -53.9(2) . . . . ? C2 C3 C4 C5 53.5(2) . . . . ? C3 C4 C5 C6 -55.4(2) . . . . ? C1 N C6 C5 128.9(2) . . . . ? C2 N C6 C5 -57.0(2) . . . . ? C4 C5 C6 N 58.5(2) . . . . ? C1 Ru C7 C12 -150.74(18) . . . . ? C8 Ru C7 C12 -131.85(19) . . . . ? C9 Ru C7 C12 -102.23(14) . . . . ? C11 Ru C7 C12 -28.99(13) . . . . ? C10 Ru C7 C12 -65.11(13) . . . . ? Cl2 Ru C7 C12 47.98(14) . . . . ? Cl1 Ru C7 C12 133.20(13) . . . . ? C1 Ru C7 C8 -18.9(3) . . . . ? C9 Ru C7 C8 29.62(12) . . . . ? C11 Ru C7 C8 102.87(13) . . . . ? C12 Ru C7 C8 131.85(19) . . . . ? C10 Ru C7 C8 66.74(12) . . . . ? Cl2 Ru C7 C8 179.83(10) . . . . ? Cl1 Ru C7 C8 -94.95(12) . . . . ? C1 Ru C7 C13 89.8(3) . . . . ? C8 Ru C7 C13 108.7(2) . . . . ? C9 Ru C7 C13 138.3(2) . . . . ? C11 Ru C7 C13 -148.4(2) . . . . ? C12 Ru C7 C13 -119.4(3) . . . . ? C10 Ru C7 C13 175.4(2) . . . . ? Cl2 Ru C7 C13 -71.5(2) . . . . ? Cl1 Ru C7 C13 13.75(19) . . . . ? C12 C7 C8 C9 -4.3(3) . . . . ? C13 C7 C8 C9 177.3(2) . . . . ? Ru C7 C8 C9 -56.68(18) . . . . ? C12 C7 C8 Ru 52.39(18) . . . . ? C13 C7 C8 Ru -126.06(19) . . . . ? C1 Ru C8 C9 -56.96(14) . . . . ? C11 Ru C8 C9 66.13(12) . . . . ? C12 Ru C8 C9 103.12(14) . . . . ? C10 Ru C8 C9 29.69(11) . . . . ? C7 Ru C8 C9 131.44(18) . . . . ? Cl2 Ru C8 C9 131.09(13) . . . . ? Cl1 Ru C8 C9 -144.85(11) . . . . ? C1 Ru C8 C7 171.60(12) . . . . ? C9 Ru C8 C7 -131.44(18) . . . . ? C11 Ru C8 C7 -65.31(12) . . . . ? C12 Ru C8 C7 -28.32(12) . . . . ? C10 Ru C8 C7 -101.75(13) . . . . ? Cl2 Ru C8 C7 -0.3(2) . . . . ? Cl1 Ru C8 C7 83.71(12) . . . . ? C7 C8 C9 C10 0.2(3) . . . . ? Ru C8 C9 C10 -58.37(19) . . . . ? C7 C8 C9 Ru 58.58(18) . . . . ? C1 Ru C9 C8 133.27(12) . . . . ? C11 Ru C9 C8 -102.19(13) . . . . ? C12 Ru C9 C8 -65.09(12) . . . . ? C10 Ru C9 C8 -130.96(18) . . . . ? C7 Ru C9 C8 -29.66(12) . . . . ? Cl2 Ru C9 C8 -134.35(12) . . . . ? Cl1 Ru C9 C8 41.57(13) . . . . ? C1 Ru C9 C10 -95.77(13) . . . . ? C8 Ru C9 C10 130.96(18) . . . . ? C11 Ru C9 C10 28.77(12) . . . . ? C12 Ru C9 C10 65.88(13) . . . . ? C7 Ru C9 C10 101.30(13) . . . . ? Cl2 Ru C9 C10 -3.4(2) . . . . ? Cl1 Ru C9 C10 172.53(10) . . . . ? C8 C9 C10 C11 5.6(3) . . . . ? Ru C9 C10 C11 -50.90(17) . . . . ? C8 C9 C10 C16 -170.3(2) . . . . ? Ru C9 C10 C16 133.20(19) . . . . ? C8 C9 C10 Ru 56.49(18) . . . . ? C1 Ru C10 C11 -138.43(13) . . . . ? C8 Ru C10 C11 102.20(14) . . . . ? C9 Ru C10 C11 132.19(19) . . . . ? C12 Ru C10 C11 29.58(13) . . . . ? C7 Ru C10 C11 64.69(13) . . . . ? Cl2 Ru C10 C11 -49.53(14) . . . . ? Cl1 Ru C10 C11 115.90(15) . . . . ? C1 Ru C10 C9 89.37(13) . . . . ? C8 Ru C10 C9 -29.99(12) . . . . ? C11 Ru C10 C9 -132.19(19) . . . . ? C12 Ru C10 C9 -102.62(14) . . . . ? C7 Ru C10 C9 -67.50(13) . . . . ? Cl2 Ru C10 C9 178.27(10) . . . . ? Cl1 Ru C10 C9 -16.3(2) . . . . ? C1 Ru C10 C16 -22.1(2) . . . . ? C8 Ru C10 C16 -141.5(2) . . . . ? C9 Ru C10 C16 -111.5(3) . . . . ? C11 Ru C10 C16 116.3(3) . . . . ? C12 Ru C10 C16 145.9(2) . . . . ? C7 Ru C10 C16 -179.0(2) . . . . ? Cl2 Ru C10 C16 66.8(2) . . . . ? Cl1 Ru C10 C16 -127.8(2) . . . . ? C9 C10 C11 C12 -7.5(3) . . . . ? C16 C10 C11 C12 168.3(2) . . . . ? Ru C10 C11 C12 -57.67(18) . . . . ? C9 C10 C11 Ru 50.17(17) . . . . ? C16 C10 C11 Ru -134.0(2) . . . . ? C1 Ru C11 C10 52.46(16) . . . . ? C8 Ru C11 C10 -66.60(13) . . . . ? C9 Ru C11 C10 -29.19(13) . . . . ? C12 Ru C11 C10 -131.66(19) . . . . ? C7 Ru C11 C10 -103.94(14) . . . . ? Cl2 Ru C11 C10 136.66(13) . . . . ? Cl1 Ru C11 C10 -138.18(11) . . . . ? C1 Ru C11 C12 -175.88(12) . . . . ? C8 Ru C11 C12 65.07(13) . . . . ? C9 Ru C11 C12 102.48(14) . . . . ? C10 Ru C11 C12 131.66(19) . . . . ? C7 Ru C11 C12 27.72(12) . . . . ? Cl2 Ru C11 C12 -91.68(12) . . . . ? Cl1 Ru C11 C12 -6.52(19) . . . . ? C8 C7 C12 C11 2.4(3) . . . . ? C13 C7 C12 C11 -179.2(2) . . . . ? Ru C7 C12 C11 52.82(18) . . . . ? C8 C7 C12 Ru -50.38(17) . . . . ? C13 C7 C12 Ru 128.0(2) . . . . ? C10 C11 C12 C7 3.5(3) . . . . ? Ru C11 C12 C7 -54.53(19) . . . . ? C10 C11 C12 Ru 58.08(18) . . . . ? C1 Ru C12 C7 143.7(2) . . . . ? C8 Ru C12 C7 29.84(13) . . . . ? C9 Ru C12 C7 67.08(14) . . . . ? C11 Ru C12 C7 133.05(19) . . . . ? C10 Ru C12 C7 104.01(14) . . . . ? Cl2 Ru C12 C7 -138.36(12) . . . . ? Cl1 Ru C12 C7 -50.71(13) . . . . ? C1 Ru C12 C11 10.7(3) . . . . ? C8 Ru C12 C11 -103.21(14) . . . . ? C9 Ru C12 C11 -65.96(13) . . . . ? C10 Ru C12 C11 -29.04(12) . . . . ? C7 Ru C12 C11 -133.05(19) . . . . ? Cl2 Ru C12 C11 88.59(12) . . . . ? Cl1 Ru C12 C11 176.24(11) . . . . ? C12 C7 C13 C14 -29.4(3) . . . . ? C8 C7 C13 C14 148.9(2) . . . . ? Ru C7 C13 C14 65.2(3) . . . . ? C12 C7 C13 C15 94.8(3) . . . . ? C8 C7 C13 C15 -86.9(2) . . . . ? Ru C7 C13 C15 -170.57(16) . . . . ? C19 C17 C18 C19 0.0(4) 7_566 . . . ? C17 C18 C19 C17 0.0(4) . . . 7_566 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.609 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.070 #============================================================================= # end of cif data for "pet10" (compound 3) #============================================================================= #============================================================================= # cif data for "pet12" (compound 4a) #============================================================================= data_pet12 _database_code_depnum_ccdc_archive 'CCDC 819868' #TrackingRef 'pet-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H53 Cl11 N2 P2 Ru' _chemical_formula_weight 1246.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 '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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.3361(2) _cell_length_b 23.2191(2) _cell_length_c 17.3423(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.837(2) _cell_angle_gamma 90.00 _cell_volume 5495.27(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 69613 _cell_measurement_theta_min 3.2820 _cell_measurement_theta_max 75.9246 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 8.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73918 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90022 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0116 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 76.01 _reflns_number_total 11424 _reflns_number_gt 11030 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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^)+(0.0307P)^2^+4.1215P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11424 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.329796(8) 0.220787(4) 0.223260(6) 0.01164(4) Uani 1 1 d . . . Cl1 Cl 0.18662(3) 0.222905(15) 0.10829(2) 0.02046(8) Uani 1 1 d . . . Cl2 Cl 0.25783(3) 0.386342(15) 0.79256(2) 0.02072(8) Uani 1 1 d . . . Cl3 Cl 0.38249(4) 0.31110(2) 0.64985(3) 0.03712(10) Uani 1 1 d . . . Cl4 Cl 0.28947(4) 0.41755(2) 0.57694(3) 0.04074(11) Uani 1 1 d . . . Cl5 Cl 0.19051(4) 0.30811(2) 0.53184(3) 0.04198(11) Uani 1 1 d . . . Cl6 Cl -0.01562(4) 0.20714(2) 0.45656(4) 0.04768(13) Uani 1 1 d . . . Cl7 Cl 0.05868(4) 0.14124(3) 0.34632(3) 0.04123(11) Uani 1 1 d . . . Cl8 Cl 0.03854(4) 0.08786(3) 0.49024(4) 0.05434(16) Uani 1 1 d . . . Cl9 Cl 0.25774(4) 0.06302(2) 0.65900(3) 0.03827(11) Uani 1 1 d . . . Cl10 Cl 0.28133(3) 0.054973(19) 0.82995(3) 0.03245(9) Uani 1 1 d . . . Cl11 Cl 0.09134(3) 0.03268(2) 0.71204(3) 0.04047(11) Uani 1 1 d . . . P1 P 0.34630(3) 0.121383(15) 0.19566(2) 0.01312(7) Uani 1 1 d . . . P2 P 0.30208(3) 0.320614(15) 0.24149(2) 0.01246(7) Uani 1 1 d . . . N1 N 0.55303(9) 0.23663(6) 0.27932(8) 0.0178(3) Uani 1 1 d . . . N2 N 0.40803(9) 0.20107(6) 0.40768(7) 0.0169(3) Uani 1 1 d . . . C1 C 0.46584(11) 0.22669(6) 0.28453(9) 0.0149(3) Uani 1 1 d . . . C2 C 0.40865(11) 0.21290(6) 0.33441(9) 0.0147(3) Uani 1 1 d . . . C3 C 0.64414(12) 0.23399(8) 0.34888(11) 0.0256(3) Uani 1 1 d . . . H3A H 0.6725 0.1949 0.3520 0.031 Uiso 1 1 calc R . . H3B H 0.6278 0.2410 0.3996 0.031 Uiso 1 1 calc R . . C4 C 0.72014(13) 0.27789(8) 0.34223(14) 0.0343(5) Uani 1 1 d . . . H4A H 0.6989 0.3168 0.3534 0.041 Uiso 1 1 calc R . . H4B H 0.7832 0.2694 0.3840 0.041 Uiso 1 1 calc R . . C5 C 0.73572(14) 0.27806(8) 0.25947(15) 0.0365(5) Uani 1 1 d . . . H5A H 0.7638 0.2407 0.2501 0.044 Uiso 1 1 calc R . . H5B H 0.7824 0.3089 0.2571 0.044 Uiso 1 1 calc R . . C6 C 0.63835(15) 0.28801(8) 0.19444(14) 0.0341(4) Uani 1 1 d . . . H6A H 0.6484 0.2879 0.1404 0.041 Uiso 1 1 calc R . . H6B H 0.6119 0.3261 0.2026 0.041 Uiso 1 1 calc R . . C7 C 0.56534(13) 0.24123(8) 0.19779(11) 0.0251(3) Uani 1 1 d . . . H7A H 0.5012 0.2499 0.1576 0.030 Uiso 1 1 calc R . . H7B H 0.5883 0.2038 0.1830 0.030 Uiso 1 1 calc R . . C8 C 0.49498(13) 0.20315(8) 0.48071(10) 0.0258(4) Uani 1 1 d . . . H8A H 0.4931 0.2389 0.5113 0.031 Uiso 1 1 calc R . . H8B H 0.5551 0.2040 0.4641 0.031 Uiso 1 1 calc R . . C9 C 0.49846(13) 0.15145(8) 0.53513(10) 0.0261(4) Uani 1 1 d . . . H9A H 0.5538 0.1559 0.5856 0.031 Uiso 1 1 calc R . . H9B H 0.5098 0.1161 0.5074 0.031 Uiso 1 1 calc R . . C10 C 0.40346(14) 0.14534(8) 0.55609(10) 0.0280(4) Uani 1 1 d . . . H10A H 0.3941 0.1794 0.5873 0.034 Uiso 1 1 calc R . . H10B H 0.4065 0.1107 0.5900 0.034 Uiso 1 1 calc R . . C11 C 0.31759(13) 0.14014(8) 0.47840(10) 0.0262(3) Uani 1 1 d . . . H11A H 0.3246 0.1044 0.4495 0.031 Uiso 1 1 calc R . . H11B H 0.2556 0.1376 0.4921 0.031 Uiso 1 1 calc R . . C12 C 0.31383(12) 0.19178(7) 0.42358(10) 0.0220(3) Uani 1 1 d . . . H12A H 0.2617 0.1857 0.3715 0.026 Uiso 1 1 calc R . . H12B H 0.2969 0.2266 0.4493 0.026 Uiso 1 1 calc R . . C13 C 0.40542(11) 0.10943(6) 0.11725(9) 0.0163(3) Uani 1 1 d . . . C14 C 0.37819(12) 0.14473(7) 0.04860(9) 0.0213(3) Uani 1 1 d . . . H14 H 0.3297 0.1736 0.0435 0.026 Uiso 1 1 calc R . . C15 C 0.42177(13) 0.13773(8) -0.01202(10) 0.0260(3) Uani 1 1 d . . . H15 H 0.4026 0.1617 -0.0587 0.031 Uiso 1 1 calc R . . C16 C 0.49314(13) 0.09603(8) -0.00502(10) 0.0250(3) Uani 1 1 d . . . H16 H 0.5230 0.0916 -0.0466 0.030 Uiso 1 1 calc R . . C17 C 0.52068(13) 0.06092(8) 0.06262(10) 0.0246(3) Uani 1 1 d . . . H17 H 0.5697 0.0324 0.0676 0.030 Uiso 1 1 calc R . . C18 C 0.47692(12) 0.06729(7) 0.12328(10) 0.0211(3) Uani 1 1 d . . . H18 H 0.4957 0.0428 0.1693 0.025 Uiso 1 1 calc R . . C19 C 0.41916(11) 0.07842(6) 0.28116(9) 0.0151(3) Uani 1 1 d . . . C20 C 0.52052(11) 0.08699(7) 0.31088(9) 0.0182(3) Uani 1 1 d . . . H20 H 0.5505 0.1159 0.2876 0.022 Uiso 1 1 calc R . . C21 C 0.57736(12) 0.05360(7) 0.37399(10) 0.0212(3) Uani 1 1 d . . . H21 H 0.6463 0.0592 0.3932 0.025 Uiso 1 1 calc R . . C22 C 0.53396(13) 0.01193(7) 0.40929(10) 0.0240(3) Uani 1 1 d . . . H22 H 0.5732 -0.0110 0.4524 0.029 Uiso 1 1 calc R . . C23 C 0.43326(13) 0.00390(7) 0.38146(10) 0.0236(3) Uani 1 1 d . . . H23 H 0.4035 -0.0243 0.4060 0.028 Uiso 1 1 calc R . . C24 C 0.37587(12) 0.03706(7) 0.31765(9) 0.0187(3) Uani 1 1 d . . . H24 H 0.3069 0.0315 0.2988 0.022 Uiso 1 1 calc R . . C25 C 0.23275(11) 0.08017(6) 0.16166(9) 0.0162(3) Uani 1 1 d . . . C26 C 0.22390(12) 0.03214(7) 0.11162(10) 0.0212(3) Uani 1 1 d . . . H26 H 0.2765 0.0214 0.0921 0.025 Uiso 1 1 calc R . . C27 C 0.13774(13) -0.00001(7) 0.09027(10) 0.0255(4) Uani 1 1 d . . . H27 H 0.1315 -0.0325 0.0558 0.031 Uiso 1 1 calc R . . C28 C 0.06110(12) 0.01531(7) 0.11910(10) 0.0254(4) Uani 1 1 d . . . H28 H 0.0024 -0.0066 0.1041 0.030 Uiso 1 1 calc R . . C29 C 0.06980(12) 0.06260(7) 0.16979(10) 0.0240(3) Uani 1 1 d . . . H29 H 0.0176 0.0727 0.1902 0.029 Uiso 1 1 calc R . . C30 C 0.15534(11) 0.09518(7) 0.19059(9) 0.0194(3) Uani 1 1 d . . . H30 H 0.1611 0.1278 0.2247 0.023 Uiso 1 1 calc R . . C31 C 0.30829(11) 0.37153(6) 0.16242(9) 0.0153(3) Uani 1 1 d . . . C32 C 0.29474(12) 0.35215(7) 0.08357(9) 0.0196(3) Uani 1 1 d . . . H32 H 0.2828 0.3125 0.0711 0.024 Uiso 1 1 calc R . . C33 C 0.29866(12) 0.39066(8) 0.02316(10) 0.0239(3) Uani 1 1 d . . . H33 H 0.2889 0.3772 -0.0305 0.029 Uiso 1 1 calc R . . C34 C 0.31664(12) 0.44851(8) 0.04076(10) 0.0242(3) Uani 1 1 d . . . H34 H 0.3187 0.4747 -0.0008 0.029 Uiso 1 1 calc R . . C35 C 0.33170(12) 0.46833(7) 0.11912(10) 0.0219(3) Uani 1 1 d . . . H35 H 0.3447 0.5080 0.1313 0.026 Uiso 1 1 calc R . . C36 C 0.32778(11) 0.43011(7) 0.17993(9) 0.0182(3) Uani 1 1 d . . . H36 H 0.3384 0.4438 0.2336 0.022 Uiso 1 1 calc R . . C37 C 0.39473(11) 0.34811(6) 0.33083(9) 0.0149(3) Uani 1 1 d . . . C38 C 0.48506(11) 0.36628(7) 0.32462(9) 0.0177(3) Uani 1 1 d . . . H38 H 0.4946 0.3689 0.2729 0.021 Uiso 1 1 calc R . . C39 C 0.56099(12) 0.38058(7) 0.39362(10) 0.0212(3) Uani 1 1 d . . . H39 H 0.6216 0.3940 0.3889 0.025 Uiso 1 1 calc R . . C40 C 0.54823(13) 0.37518(7) 0.46938(10) 0.0233(3) Uani 1 1 d . . . H40 H 0.6008 0.3838 0.5167 0.028 Uiso 1 1 calc R . . C41 C 0.45936(13) 0.35725(7) 0.47611(9) 0.0234(3) Uani 1 1 d . . . H41 H 0.4508 0.3539 0.5281 0.028 Uiso 1 1 calc R . . C42 C 0.38192(12) 0.34396(6) 0.40722(9) 0.0188(3) Uani 1 1 d . . . H42 H 0.3206 0.3321 0.4123 0.023 Uiso 1 1 calc R . . C43 C 0.18559(11) 0.33611(7) 0.26029(9) 0.0160(3) Uani 1 1 d . . . C44 C 0.12539(12) 0.29092(7) 0.26861(10) 0.0220(3) Uani 1 1 d . . . H44 H 0.1450 0.2523 0.2642 0.026 Uiso 1 1 calc R . . C45 C 0.03691(13) 0.30186(8) 0.28323(11) 0.0259(3) Uani 1 1 d . . . H45 H -0.0031 0.2707 0.2896 0.031 Uiso 1 1 calc R . . C46 C 0.00711(12) 0.35797(8) 0.28851(10) 0.0246(3) Uani 1 1 d . . . H46 H -0.0537 0.3655 0.2979 0.030 Uiso 1 1 calc R . . C47 C 0.06615(14) 0.40300(8) 0.28008(13) 0.0320(4) Uani 1 1 d . . . H47 H 0.0457 0.4416 0.2835 0.038 Uiso 1 1 calc R . . C48 C 0.15517(13) 0.39221(7) 0.26664(12) 0.0274(4) Uani 1 1 d . . . H48 H 0.1957 0.4235 0.2617 0.033 Uiso 1 1 calc R . . C49 C 0.27023(14) 0.34832(8) 0.61100(12) 0.0309(4) Uani 1 1 d . . . H49 H 0.2396 0.3526 0.6553 0.037 Uiso 1 1 calc R . . C50 C -0.01172(13) 0.13843(8) 0.41395(12) 0.0301(4) Uani 1 1 d . . . H50 H -0.0800 0.1264 0.3833 0.036 Uiso 1 1 calc R . . C51 C 0.21931(13) 0.02640(8) 0.73319(12) 0.0281(4) Uani 1 1 d . . . H51 H 0.2365 -0.0153 0.7323 0.034 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 Ru 0.01137(6) 0.01084(6) 0.01094(6) -0.00051(3) 0.00078(4) 0.00013(4) Cl1 0.01818(17) 0.01607(16) 0.01959(17) -0.00142(12) -0.00537(14) 0.00069(12) Cl2 0.02321(18) 0.01799(16) 0.02243(17) 0.00084(13) 0.00917(14) -0.00011(13) Cl3 0.0351(2) 0.0404(2) 0.0383(2) 0.01146(19) 0.01477(19) 0.00383(19) Cl4 0.0380(3) 0.0321(2) 0.0589(3) 0.0090(2) 0.0248(2) 0.00400(19) Cl5 0.0358(2) 0.0455(3) 0.0447(3) -0.0132(2) 0.0124(2) -0.0014(2) Cl6 0.0495(3) 0.0417(3) 0.0493(3) -0.0114(2) 0.0114(2) -0.0030(2) Cl7 0.0330(2) 0.0589(3) 0.0338(2) 0.0053(2) 0.01319(19) 0.0000(2) Cl8 0.0447(3) 0.0645(4) 0.0611(3) 0.0340(3) 0.0270(3) 0.0208(3) Cl9 0.0425(3) 0.0401(3) 0.0360(2) -0.00141(19) 0.0175(2) 0.0008(2) Cl10 0.0347(2) 0.0283(2) 0.0317(2) -0.00085(17) 0.00637(18) -0.00067(17) Cl11 0.0232(2) 0.0406(3) 0.0568(3) -0.0102(2) 0.0112(2) -0.00069(18) P1 0.01362(17) 0.01150(16) 0.01254(16) -0.00050(12) 0.00152(13) 0.00009(13) P2 0.01312(16) 0.01178(16) 0.01135(15) -0.00047(12) 0.00207(13) 0.00048(13) N1 0.0118(6) 0.0178(6) 0.0229(7) -0.0029(5) 0.0039(5) -0.0012(5) N2 0.0182(6) 0.0181(6) 0.0114(6) 0.0012(5) 0.0000(5) -0.0007(5) C1 0.0162(7) 0.0096(6) 0.0174(7) -0.0014(5) 0.0028(6) 0.0006(5) C2 0.0142(7) 0.0100(6) 0.0178(7) -0.0020(5) 0.0019(6) 0.0003(5) C3 0.0134(7) 0.0301(9) 0.0292(9) -0.0061(7) 0.0004(7) -0.0003(6) C4 0.0164(8) 0.0280(9) 0.0564(13) -0.0179(8) 0.0083(8) -0.0060(7) C5 0.0242(9) 0.0246(9) 0.0680(15) -0.0090(9) 0.0249(10) -0.0069(7) C6 0.0328(10) 0.0267(9) 0.0515(12) 0.0011(8) 0.0260(9) -0.0036(8) C7 0.0242(8) 0.0259(8) 0.0290(9) -0.0012(7) 0.0141(7) -0.0023(7) C8 0.0246(8) 0.0287(9) 0.0167(8) 0.0034(7) -0.0046(6) -0.0066(7) C9 0.0300(9) 0.0265(9) 0.0160(7) 0.0048(6) -0.0018(6) 0.0016(7) C10 0.0391(10) 0.0266(9) 0.0177(8) 0.0054(6) 0.0078(7) 0.0022(7) C11 0.0287(9) 0.0291(9) 0.0221(8) 0.0047(7) 0.0095(7) -0.0024(7) C12 0.0207(8) 0.0275(8) 0.0181(7) 0.0032(6) 0.0062(6) 0.0022(6) C13 0.0171(7) 0.0151(7) 0.0154(7) -0.0022(5) 0.0032(6) -0.0015(5) C14 0.0241(8) 0.0215(8) 0.0174(7) 0.0015(6) 0.0050(6) 0.0059(6) C15 0.0319(9) 0.0286(9) 0.0180(8) 0.0052(6) 0.0082(7) 0.0062(7) C16 0.0271(8) 0.0302(9) 0.0192(7) -0.0012(7) 0.0093(7) 0.0025(7) C17 0.0253(8) 0.0256(8) 0.0228(8) -0.0010(6) 0.0072(7) 0.0073(7) C18 0.0254(8) 0.0185(7) 0.0189(7) 0.0017(6) 0.0061(6) 0.0045(6) C19 0.0169(7) 0.0136(7) 0.0132(6) -0.0015(5) 0.0021(5) 0.0014(5) C20 0.0183(7) 0.0158(7) 0.0185(7) -0.0004(6) 0.0028(6) -0.0002(6) C21 0.0185(7) 0.0221(8) 0.0191(7) -0.0018(6) 0.0000(6) 0.0028(6) C22 0.0283(9) 0.0226(8) 0.0171(7) 0.0043(6) 0.0009(6) 0.0067(7) C23 0.0297(9) 0.0206(8) 0.0191(8) 0.0044(6) 0.0051(7) -0.0008(7) C24 0.0195(7) 0.0172(7) 0.0179(7) 0.0006(6) 0.0037(6) -0.0008(6) C25 0.0162(7) 0.0144(7) 0.0140(7) 0.0021(5) -0.0014(5) -0.0009(5) C26 0.0228(8) 0.0154(7) 0.0211(7) -0.0006(6) 0.0004(6) 0.0001(6) C27 0.0290(9) 0.0157(7) 0.0241(8) -0.0012(6) -0.0033(7) -0.0045(6) C28 0.0224(8) 0.0195(8) 0.0264(8) 0.0058(6) -0.0040(7) -0.0086(6) C29 0.0199(8) 0.0248(8) 0.0256(8) 0.0049(7) 0.0042(6) -0.0028(6) C30 0.0193(7) 0.0178(7) 0.0190(7) -0.0001(6) 0.0028(6) -0.0024(6) C31 0.0131(7) 0.0170(7) 0.0146(7) 0.0019(5) 0.0025(5) 0.0007(5) C32 0.0201(7) 0.0209(8) 0.0170(7) -0.0004(6) 0.0043(6) -0.0012(6) C33 0.0243(8) 0.0322(9) 0.0145(7) 0.0022(6) 0.0049(6) -0.0007(7) C34 0.0215(8) 0.0287(9) 0.0219(8) 0.0117(7) 0.0058(6) 0.0008(7) C35 0.0193(8) 0.0190(7) 0.0269(8) 0.0044(6) 0.0062(6) 0.0001(6) C36 0.0180(7) 0.0179(7) 0.0179(7) 0.0013(6) 0.0045(6) 0.0016(6) C37 0.0170(7) 0.0113(6) 0.0141(7) -0.0002(5) 0.0014(5) 0.0019(5) C38 0.0180(7) 0.0168(7) 0.0174(7) -0.0024(6) 0.0042(6) 0.0011(6) C39 0.0169(7) 0.0165(7) 0.0266(8) -0.0047(6) 0.0011(6) 0.0012(6) C40 0.0255(8) 0.0163(7) 0.0197(7) -0.0033(6) -0.0054(6) 0.0047(6) C41 0.0352(9) 0.0179(7) 0.0135(7) 0.0000(6) 0.0022(6) 0.0030(7) C42 0.0236(8) 0.0155(7) 0.0167(7) 0.0006(6) 0.0054(6) 0.0012(6) C43 0.0151(7) 0.0180(7) 0.0138(6) 0.0006(5) 0.0030(5) 0.0011(6) C44 0.0218(8) 0.0181(7) 0.0273(8) 0.0000(6) 0.0095(7) -0.0002(6) C45 0.0217(8) 0.0275(9) 0.0306(9) -0.0020(7) 0.0110(7) -0.0049(7) C46 0.0195(8) 0.0319(9) 0.0244(8) -0.0019(7) 0.0097(6) 0.0027(7) C47 0.0309(9) 0.0223(8) 0.0491(11) -0.0006(8) 0.0218(9) 0.0064(7) C48 0.0270(9) 0.0183(8) 0.0426(10) -0.0003(7) 0.0189(8) -0.0006(7) C49 0.0311(9) 0.0324(10) 0.0338(10) 0.0003(8) 0.0166(8) -0.0014(8) C50 0.0230(8) 0.0343(10) 0.0325(9) 0.0026(8) 0.0076(7) 0.0003(7) C51 0.0255(9) 0.0224(8) 0.0362(10) -0.0039(7) 0.0091(7) 0.0006(7) _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 Ru C1 1.9188(15) . ? Ru C2 1.9215(15) . ? Ru P1 2.3836(4) . ? Ru Cl1 2.3840(4) . ? Ru P2 2.3890(4) . ? Cl3 C49 1.768(2) . ? Cl4 C49 1.763(2) . ? Cl5 C49 1.761(2) . ? Cl6 C50 1.766(2) . ? Cl7 C50 1.7673(19) . ? Cl8 C50 1.751(2) . ? Cl9 C51 1.7653(19) . ? Cl10 C51 1.7700(19) . ? Cl11 C51 1.7633(18) . ? P1 C25 1.8234(15) . ? P1 C19 1.8264(15) . ? P1 C13 1.8305(15) . ? P2 C37 1.8199(15) . ? P2 C43 1.8326(15) . ? P2 C31 1.8332(15) . ? N1 C1 1.301(2) . ? N1 C7 1.481(2) . ? N1 C3 1.483(2) . ? N2 C2 1.303(2) . ? N2 C12 1.475(2) . ? N2 C8 1.4808(19) . ? C1 C2 1.399(2) . ? C3 C4 1.522(2) . ? C4 C5 1.519(3) . ? C5 C6 1.520(3) . ? C6 C7 1.522(2) . ? C8 C9 1.518(2) . ? C9 C10 1.520(3) . ? C10 C11 1.526(2) . ? C11 C12 1.521(2) . ? C13 C18 1.398(2) . ? C13 C14 1.399(2) . ? C14 C15 1.387(2) . ? C15 C16 1.387(2) . ? C16 C17 1.383(2) . ? C17 C18 1.388(2) . ? C19 C24 1.396(2) . ? C19 C20 1.399(2) . ? C20 C21 1.385(2) . ? C21 C22 1.390(2) . ? C22 C23 1.387(2) . ? C23 C24 1.391(2) . ? C25 C30 1.395(2) . ? C25 C26 1.395(2) . ? C26 C27 1.393(2) . ? C27 C28 1.386(3) . ? C28 C29 1.388(2) . ? C29 C30 1.391(2) . ? C31 C32 1.396(2) . ? C31 C36 1.403(2) . ? C32 C33 1.392(2) . ? C33 C34 1.384(3) . ? C34 C35 1.388(2) . ? C35 C36 1.393(2) . ? C37 C42 1.395(2) . ? C37 C38 1.397(2) . ? C38 C39 1.389(2) . ? C39 C40 1.387(2) . ? C40 C41 1.379(3) . ? C41 C42 1.394(2) . ? C43 C48 1.389(2) . ? C43 C44 1.394(2) . ? C44 C45 1.391(2) . ? C45 C46 1.383(3) . ? C46 C47 1.381(3) . ? C47 C48 1.388(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru C2 42.73(6) . . ? C1 Ru P1 91.94(4) . . ? C2 Ru P1 92.59(4) . . ? C1 Ru Cl1 158.48(5) . . ? C2 Ru Cl1 158.78(5) . . ? P1 Ru Cl1 87.995(12) . . ? C1 Ru P2 92.26(4) . . ? C2 Ru P2 91.74(4) . . ? P1 Ru P2 175.422(13) . . ? Cl1 Ru P2 87.429(12) . . ? C25 P1 C19 101.99(7) . . ? C25 P1 C13 104.53(7) . . ? C19 P1 C13 103.91(7) . . ? C25 P1 Ru 116.06(5) . . ? C19 P1 Ru 115.66(5) . . ? C13 P1 Ru 113.14(5) . . ? C37 P2 C43 104.29(7) . . ? C37 P2 C31 102.74(7) . . ? C43 P2 C31 105.20(7) . . ? C37 P2 Ru 110.21(5) . . ? C43 P2 Ru 114.31(5) . . ? C31 P2 Ru 118.59(5) . . ? C1 N1 C7 118.48(13) . . ? C1 N1 C3 124.17(14) . . ? C7 N1 C3 116.52(13) . . ? C2 N2 C12 119.56(13) . . ? C2 N2 C8 124.89(14) . . ? C12 N2 C8 115.09(13) . . ? N1 C1 C2 147.23(15) . . ? N1 C1 Ru 144.03(12) . . ? C2 C1 Ru 68.73(9) . . ? N2 C2 C1 146.27(15) . . ? N2 C2 Ru 145.18(12) . . ? C1 C2 Ru 68.53(9) . . ? N1 C3 C4 112.54(16) . . ? C5 C4 C3 112.90(15) . . ? C4 C5 C6 109.52(15) . . ? C5 C6 C7 110.45(16) . . ? N1 C7 C6 111.85(15) . . ? N2 C8 C9 111.39(14) . . ? C8 C9 C10 111.17(15) . . ? C9 C10 C11 109.61(14) . . ? C12 C11 C10 110.74(14) . . ? N2 C12 C11 111.90(13) . . ? C18 C13 C14 118.75(14) . . ? C18 C13 P1 123.12(12) . . ? C14 C13 P1 118.13(12) . . ? C15 C14 C13 120.22(15) . . ? C16 C15 C14 120.46(15) . . ? C17 C16 C15 119.81(16) . . ? C16 C17 C18 120.15(15) . . ? C17 C18 C13 120.61(15) . . ? C24 C19 C20 119.12(14) . . ? C24 C19 P1 121.38(12) . . ? C20 C19 P1 119.50(11) . . ? C21 C20 C19 120.32(15) . . ? C20 C21 C22 120.24(15) . . ? C23 C22 C21 119.92(15) . . ? C22 C23 C24 120.07(15) . . ? C23 C24 C19 120.30(15) . . ? C30 C25 C26 119.51(14) . . ? C30 C25 P1 118.84(11) . . ? C26 C25 P1 121.53(12) . . ? C27 C26 C25 119.88(16) . . ? C28 C27 C26 120.20(16) . . ? C27 C28 C29 120.28(15) . . ? C28 C29 C30 119.69(16) . . ? C29 C30 C25 120.41(15) . . ? C32 C31 C36 118.91(14) . . ? C32 C31 P2 120.06(12) . . ? C36 C31 P2 121.02(11) . . ? C33 C32 C31 120.33(15) . . ? C34 C33 C32 120.35(15) . . ? C33 C34 C35 120.03(15) . . ? C34 C35 C36 120.01(15) . . ? C35 C36 C31 120.36(15) . . ? C42 C37 C38 119.26(14) . . ? C42 C37 P2 120.66(12) . . ? C38 C37 P2 119.49(11) . . ? C39 C38 C37 120.40(14) . . ? C40 C39 C38 119.91(15) . . ? C41 C40 C39 120.07(15) . . ? C40 C41 C42 120.56(15) . . ? C41 C42 C37 119.77(15) . . ? C48 C43 C44 118.58(15) . . ? C48 C43 P2 121.58(12) . . ? C44 C43 P2 119.83(12) . . ? C45 C44 C43 120.64(15) . . ? C46 C45 C44 120.10(16) . . ? C47 C46 C45 119.64(16) . . ? C46 C47 C48 120.39(16) . . ? C47 C48 C43 120.65(16) . . ? Cl5 C49 Cl4 110.67(11) . . ? Cl5 C49 Cl3 109.61(11) . . ? Cl4 C49 Cl3 110.84(10) . . ? Cl8 C50 Cl6 110.37(11) . . ? Cl8 C50 Cl7 109.87(10) . . ? Cl6 C50 Cl7 110.00(10) . . ? Cl11 C51 Cl9 110.22(10) . . ? Cl11 C51 Cl10 110.77(10) . . ? Cl9 C51 Cl10 109.40(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru P1 C25 162.65(7) . . . . ? C2 Ru P1 C25 119.89(7) . . . . ? Cl1 Ru P1 C25 -38.88(5) . . . . ? P2 Ru P1 C25 -40.82(18) . . . . ? C1 Ru P1 C19 43.20(7) . . . . ? C2 Ru P1 C19 0.44(7) . . . . ? Cl1 Ru P1 C19 -158.33(6) . . . . ? P2 Ru P1 C19 -160.27(16) . . . . ? C1 Ru P1 C13 -76.50(7) . . . . ? C2 Ru P1 C13 -119.27(7) . . . . ? Cl1 Ru P1 C13 81.97(5) . . . . ? P2 Ru P1 C13 80.03(17) . . . . ? C1 Ru P2 C37 -23.00(7) . . . . ? C2 Ru P2 C37 19.75(7) . . . . ? P1 Ru P2 C37 -180(12) . . . . ? Cl1 Ru P2 C37 178.53(5) . . . . ? C1 Ru P2 C43 -140.06(7) . . . . ? C2 Ru P2 C43 -97.31(7) . . . . ? P1 Ru P2 C43 63.41(17) . . . . ? Cl1 Ru P2 C43 61.47(5) . . . . ? C1 Ru P2 C31 94.91(7) . . . . ? C2 Ru P2 C31 137.67(7) . . . . ? P1 Ru P2 C31 -61.61(18) . . . . ? Cl1 Ru P2 C31 -63.55(6) . . . . ? C7 N1 C1 C2 170.6(2) . . . . ? C3 N1 C1 C2 1.4(3) . . . . ? C7 N1 C1 Ru -8.0(3) . . . . ? C3 N1 C1 Ru -177.20(14) . . . . ? C2 Ru C1 N1 179.2(2) . . . . ? P1 Ru C1 N1 87.45(19) . . . . ? Cl1 Ru C1 N1 -2.0(3) . . . . ? P2 Ru C1 N1 -90.72(19) . . . . ? P1 Ru C1 C2 -91.71(8) . . . . ? Cl1 Ru C1 C2 178.84(9) . . . . ? P2 Ru C1 C2 90.11(8) . . . . ? C12 N2 C2 C1 177.2(2) . . . . ? C8 N2 C2 C1 5.4(3) . . . . ? C12 N2 C2 Ru -5.2(3) . . . . ? C8 N2 C2 Ru -177.00(15) . . . . ? N1 C1 C2 N2 -0.5(4) . . . . ? Ru C1 C2 N2 178.6(3) . . . . ? N1 C1 C2 Ru -179.1(3) . . . . ? C1 Ru C2 N2 -178.6(2) . . . . ? P1 Ru C2 N2 -88.5(2) . . . . ? Cl1 Ru C2 N2 2.6(3) . . . . ? P2 Ru C2 N2 90.0(2) . . . . ? P1 Ru C2 C1 90.06(8) . . . . ? Cl1 Ru C2 C1 -178.82(9) . . . . ? P2 Ru C2 C1 -91.45(8) . . . . ? C1 N1 C3 C4 -146.06(15) . . . . ? C7 N1 C3 C4 44.55(19) . . . . ? N1 C3 C4 C5 -47.9(2) . . . . ? C3 C4 C5 C6 55.8(2) . . . . ? C4 C5 C6 C7 -58.9(2) . . . . ? C1 N1 C7 C6 141.48(15) . . . . ? C3 N1 C7 C6 -48.5(2) . . . . ? C5 C6 C7 N1 55.0(2) . . . . ? C2 N2 C8 C9 -136.68(16) . . . . ? C12 N2 C8 C9 51.2(2) . . . . ? N2 C8 C9 C10 -53.9(2) . . . . ? C8 C9 C10 C11 57.54(19) . . . . ? C9 C10 C11 C12 -57.06(19) . . . . ? C2 N2 C12 C11 136.20(15) . . . . ? C8 N2 C12 C11 -51.19(19) . . . . ? C10 C11 C12 N2 53.52(19) . . . . ? C25 P1 C13 C18 -95.75(14) . . . . ? C19 P1 C13 C18 10.83(15) . . . . ? Ru P1 C13 C18 137.06(12) . . . . ? C25 P1 C13 C14 84.97(13) . . . . ? C19 P1 C13 C14 -168.45(12) . . . . ? Ru P1 C13 C14 -42.21(14) . . . . ? C18 C13 C14 C15 0.0(2) . . . . ? P1 C13 C14 C15 179.27(13) . . . . ? C13 C14 C15 C16 -0.4(3) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? C15 C16 C17 C18 0.1(3) . . . . ? C16 C17 C18 C13 -0.6(3) . . . . ? C14 C13 C18 C17 0.6(2) . . . . ? P1 C13 C18 C17 -178.71(13) . . . . ? C25 P1 C19 C24 -16.80(14) . . . . ? C13 P1 C19 C24 -125.28(13) . . . . ? Ru P1 C19 C24 110.10(12) . . . . ? C25 P1 C19 C20 163.17(12) . . . . ? C13 P1 C19 C20 54.70(13) . . . . ? Ru P1 C19 C20 -69.93(13) . . . . ? C24 C19 C20 C21 2.0(2) . . . . ? P1 C19 C20 C21 -177.98(12) . . . . ? C19 C20 C21 C22 -1.1(2) . . . . ? C20 C21 C22 C23 -0.3(2) . . . . ? C21 C22 C23 C24 0.7(3) . . . . ? C22 C23 C24 C19 0.2(2) . . . . ? C20 C19 C24 C23 -1.5(2) . . . . ? P1 C19 C24 C23 178.45(12) . . . . ? C19 P1 C25 C30 94.31(13) . . . . ? C13 P1 C25 C30 -157.69(12) . . . . ? Ru P1 C25 C30 -32.33(13) . . . . ? C19 P1 C25 C26 -81.74(13) . . . . ? C13 P1 C25 C26 26.27(14) . . . . ? Ru P1 C25 C26 151.62(11) . . . . ? C30 C25 C26 C27 0.7(2) . . . . ? P1 C25 C26 C27 176.71(12) . . . . ? C25 C26 C27 C28 -0.5(2) . . . . ? C26 C27 C28 C29 -0.3(2) . . . . ? C27 C28 C29 C30 1.0(2) . . . . ? C28 C29 C30 C25 -0.8(2) . . . . ? C26 C25 C30 C29 0.0(2) . . . . ? P1 C25 C30 C29 -176.15(12) . . . . ? C37 P2 C31 C32 144.03(12) . . . . ? C43 P2 C31 C32 -107.09(13) . . . . ? Ru P2 C31 C32 22.25(14) . . . . ? C37 P2 C31 C36 -35.19(14) . . . . ? C43 P2 C31 C36 73.70(14) . . . . ? Ru P2 C31 C36 -156.96(11) . . . . ? C36 C31 C32 C33 -1.2(2) . . . . ? P2 C31 C32 C33 179.53(12) . . . . ? C31 C32 C33 C34 0.4(3) . . . . ? C32 C33 C34 C35 0.5(3) . . . . ? C33 C34 C35 C36 -0.6(2) . . . . ? C34 C35 C36 C31 -0.2(2) . . . . ? C32 C31 C36 C35 1.2(2) . . . . ? P2 C31 C36 C35 -179.62(12) . . . . ? C43 P2 C37 C42 36.10(14) . . . . ? C31 P2 C37 C42 145.68(12) . . . . ? Ru P2 C37 C42 -87.02(12) . . . . ? C43 P2 C37 C38 -152.71(12) . . . . ? C31 P2 C37 C38 -43.14(13) . . . . ? Ru P2 C37 C38 84.16(12) . . . . ? C42 C37 C38 C39 -0.6(2) . . . . ? P2 C37 C38 C39 -171.92(12) . . . . ? C37 C38 C39 C40 1.9(2) . . . . ? C38 C39 C40 C41 -1.9(2) . . . . ? C39 C40 C41 C42 0.5(2) . . . . ? C40 C41 C42 C37 0.8(2) . . . . ? C38 C37 C42 C41 -0.8(2) . . . . ? P2 C37 C42 C41 170.43(12) . . . . ? C37 P2 C43 C48 64.08(15) . . . . ? C31 P2 C43 C48 -43.68(15) . . . . ? Ru P2 C43 C48 -175.51(12) . . . . ? C37 P2 C43 C44 -115.87(13) . . . . ? C31 P2 C43 C44 136.37(13) . . . . ? Ru P2 C43 C44 4.54(14) . . . . ? C48 C43 C44 C45 -0.2(2) . . . . ? P2 C43 C44 C45 179.74(13) . . . . ? C43 C44 C45 C46 0.9(3) . . . . ? C44 C45 C46 C47 -0.7(3) . . . . ? C45 C46 C47 C48 -0.2(3) . . . . ? C46 C47 C48 C43 0.9(3) . . . . ? C44 C43 C48 C47 -0.7(3) . . . . ? P2 C43 C48 C47 179.33(15) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 72.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.377 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.056 #============================================================================= # end of cif data for "pet12" (compound 4a) #============================================================================= #============================================================================= # cif data for "pet19a" (compound 4b) #============================================================================= data_pet19a _database_code_depnum_ccdc_archive 'CCDC 819869' #TrackingRef 'pet-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H94 B Cl N2 O3 P2 Ru' _chemical_formula_weight 1388.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3816(2) _cell_length_b 26.5861(2) _cell_length_c 18.6904(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.387(2) _cell_angle_gamma 90.00 _cell_volume 7086.97(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 50831 _cell_measurement_theta_min 3.5138 _cell_measurement_theta_max 75.7483 _exptl_crystal_description prism _exptl_crystal_colour wine-red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 2.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.87715 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84768 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 75.94 _reflns_number_total 14703 _reflns_number_gt 12917 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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. Three badly disordered THF molecules were found in the asymmetrical unit. For this reason, the program SQUEEZE (A.L. Spek, University of Utrecht, Netherlands) was used to remove mathematically the effects of the solvents. ; _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^)+(0.0516P)^2^+1.0084P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14703 _refine_ls_number_parameters 712 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.316595(7) 0.479830(4) 0.820507(6) 0.02571(5) Uani 1 1 d . . . Cl Cl 0.38262(3) 0.547463(15) 0.89411(2) 0.03825(9) Uani 1 1 d . . . P1 P 0.19895(3) 0.476319(14) 0.89933(2) 0.02664(8) Uani 1 1 d . . . P2 P 0.44537(3) 0.485288(14) 0.75130(2) 0.02635(8) Uani 1 1 d . . . N1 N 0.18686(10) 0.44337(6) 0.68650(8) 0.0346(3) Uani 1 1 d . . . N2 N 0.32009(9) 0.36475(5) 0.81863(7) 0.0302(3) Uani 1 1 d . . . B B 1.08131(14) 0.16944(7) 0.84848(11) 0.0355(4) Uani 1 1 d . . . C1 C 0.24267(11) 0.44110(6) 0.74681(9) 0.0297(3) Uani 1 1 d . . . C2 C 0.29569(10) 0.41012(6) 0.79750(9) 0.0286(3) Uani 1 1 d . . . C3 C 0.16523(13) 0.49297(7) 0.65241(10) 0.0392(4) Uani 1 1 d . . . H3A H 0.1977 0.4961 0.6090 0.047 Uiso 1 1 calc R . . H3B H 0.1888 0.5199 0.6866 0.047 Uiso 1 1 calc R . . C4 C 0.06071(13) 0.49966(7) 0.63104(11) 0.0412(4) Uani 1 1 d . . . H4A H 0.0488 0.5317 0.6045 0.049 Uiso 1 1 calc R . . H4B H 0.0289 0.5012 0.6749 0.049 Uiso 1 1 calc R . . C5 C 0.02101(13) 0.45580(8) 0.58326(11) 0.0437(4) Uani 1 1 d . . . H5A H -0.0477 0.4596 0.5716 0.052 Uiso 1 1 calc R . . H5B H 0.0489 0.4560 0.5375 0.052 Uiso 1 1 calc R . . C6 C 0.04333(13) 0.40611(7) 0.62261(11) 0.0419(4) Uani 1 1 d . . . H6A H 0.0119 0.4051 0.6667 0.050 Uiso 1 1 calc R . . H6B H 0.0189 0.3779 0.5911 0.050 Uiso 1 1 calc R . . C7 C 0.14830(14) 0.39990(7) 0.64314(11) 0.0430(4) Uani 1 1 d . . . H7A H 0.1610 0.3686 0.6713 0.052 Uiso 1 1 calc R . . H7B H 0.1792 0.3973 0.5989 0.052 Uiso 1 1 calc R . . C8 C 0.39299(12) 0.35776(6) 0.88109(9) 0.0336(3) Uani 1 1 d . . . H8A H 0.3662 0.3397 0.9200 0.040 Uiso 1 1 calc R . . H8B H 0.4156 0.3910 0.9000 0.040 Uiso 1 1 calc R . . C9 C 0.47449(12) 0.32777(6) 0.85830(11) 0.0377(4) Uani 1 1 d . . . H9A H 0.5217 0.3217 0.9008 0.045 Uiso 1 1 calc R . . H9B H 0.5048 0.3474 0.8227 0.045 Uiso 1 1 calc R . . C10 C 0.44020(13) 0.27753(6) 0.82515(11) 0.0404(4) Uani 1 1 d . . . H10A H 0.4931 0.2598 0.8071 0.048 Uiso 1 1 calc R . . H10B H 0.4174 0.2562 0.8627 0.048 Uiso 1 1 calc R . . C11 C 0.36148(13) 0.28512(6) 0.76328(11) 0.0394(4) Uani 1 1 d . . . H11A H 0.3365 0.2520 0.7461 0.047 Uiso 1 1 calc R . . H11B H 0.3868 0.3020 0.7227 0.047 Uiso 1 1 calc R . . C12 C 0.28214(12) 0.31689(6) 0.78669(10) 0.0364(4) Uani 1 1 d . . . H12A H 0.2350 0.3240 0.7445 0.044 Uiso 1 1 calc R . . H12B H 0.2508 0.2981 0.8226 0.044 Uiso 1 1 calc R . . C13 C 0.23746(11) 0.44645(6) 0.98630(9) 0.0306(3) Uani 1 1 d . . . C14 C 0.33200(12) 0.44603(6) 1.01403(9) 0.0338(3) Uani 1 1 d . . . H14 H 0.3767 0.4620 0.9883 0.041 Uiso 1 1 calc R . . C15 C 0.36108(13) 0.42224(7) 1.07956(10) 0.0412(4) Uani 1 1 d . . . H15 H 0.4256 0.4222 1.0985 0.049 Uiso 1 1 calc R . . C16 C 0.29661(15) 0.39866(7) 1.11715(10) 0.0436(4) Uani 1 1 d . . . H16 H 0.3170 0.3821 1.1614 0.052 Uiso 1 1 calc R . . C17 C 0.20213(14) 0.39929(7) 1.09004(10) 0.0407(4) Uani 1 1 d . . . H17 H 0.1576 0.3833 1.1159 0.049 Uiso 1 1 calc R . . C18 C 0.17270(12) 0.42334(7) 1.02511(9) 0.0356(3) Uani 1 1 d . . . H18 H 0.1079 0.4241 1.0070 0.043 Uiso 1 1 calc R . . C19 C 0.14700(11) 0.53638(6) 0.92077(9) 0.0296(3) Uani 1 1 d . . . C20 C 0.12227(11) 0.54666(7) 0.98876(9) 0.0334(3) Uani 1 1 d . . . H20 H 0.1342 0.5224 1.0262 0.040 Uiso 1 1 calc R . . C21 C 0.08017(12) 0.59224(7) 1.00232(10) 0.0379(4) Uani 1 1 d . . . H21 H 0.0635 0.5990 1.0490 0.046 Uiso 1 1 calc R . . C22 C 0.06254(13) 0.62761(7) 0.94844(11) 0.0407(4) Uani 1 1 d . . . H22 H 0.0337 0.6586 0.9579 0.049 Uiso 1 1 calc R . . C23 C 0.08689(16) 0.61789(7) 0.88075(11) 0.0480(4) Uani 1 1 d . . . H23 H 0.0743 0.6422 0.8435 0.058 Uiso 1 1 calc R . . C24 C 0.12997(15) 0.57250(7) 0.86676(10) 0.0417(4) Uani 1 1 d . . . H24 H 0.1477 0.5663 0.8203 0.050 Uiso 1 1 calc R . . C25 C 0.09851(11) 0.43741(6) 0.86371(8) 0.0287(3) Uani 1 1 d . . . C26 C 0.10927(11) 0.38515(6) 0.86370(9) 0.0315(3) Uani 1 1 d . . . H26 H 0.1659 0.3706 0.8862 0.038 Uiso 1 1 calc R . . C27 C 0.03817(12) 0.35417(6) 0.83116(10) 0.0344(3) Uani 1 1 d . . . H27 H 0.0467 0.3187 0.8309 0.041 Uiso 1 1 calc R . . C28 C -0.04528(12) 0.37518(7) 0.79898(10) 0.0365(4) Uani 1 1 d . . . H28 H -0.0940 0.3542 0.7765 0.044 Uiso 1 1 calc R . . C29 C -0.05723(12) 0.42680(7) 0.79984(10) 0.0367(4) Uani 1 1 d . . . H29 H -0.1149 0.4410 0.7787 0.044 Uiso 1 1 calc R . . C30 C 0.01404(11) 0.45817(6) 0.83128(9) 0.0324(3) Uani 1 1 d . . . H30 H 0.0054 0.4936 0.8307 0.039 Uiso 1 1 calc R . . C31 C 0.54864(11) 0.45189(6) 0.79466(9) 0.0293(3) Uani 1 1 d . . . C32 C 0.60893(11) 0.42543(6) 0.75548(10) 0.0349(3) Uani 1 1 d . . . H32 H 0.5964 0.4238 0.7044 0.042 Uiso 1 1 calc R . . C33 C 0.68714(13) 0.40150(7) 0.79122(12) 0.0423(4) Uani 1 1 d . . . H33 H 0.7281 0.3835 0.7645 0.051 Uiso 1 1 calc R . . C34 C 0.70582(13) 0.40377(7) 0.86581(12) 0.0436(4) Uani 1 1 d . . . H34 H 0.7593 0.3871 0.8900 0.052 Uiso 1 1 calc R . . C35 C 0.64697(13) 0.43025(7) 0.90523(10) 0.0393(4) Uani 1 1 d . . . H35 H 0.6603 0.4321 0.9563 0.047 Uiso 1 1 calc R . . C36 C 0.56805(11) 0.45414(6) 0.86966(9) 0.0320(3) Uani 1 1 d . . . H36 H 0.5272 0.4721 0.8966 0.038 Uiso 1 1 calc R . . C37 C 0.42297(11) 0.45701(6) 0.66117(9) 0.0322(3) Uani 1 1 d . . . C38 C 0.40537(13) 0.40543(7) 0.65521(10) 0.0386(4) Uani 1 1 d . . . H38 H 0.4097 0.3854 0.6976 0.046 Uiso 1 1 calc R . . C39 C 0.38152(15) 0.38306(8) 0.58809(11) 0.0472(4) Uani 1 1 d . . . H39 H 0.3691 0.3480 0.5848 0.057 Uiso 1 1 calc R . . C40 C 0.37596(15) 0.41192(9) 0.52626(11) 0.0516(5) Uani 1 1 d . . . H40 H 0.3596 0.3968 0.4803 0.062 Uiso 1 1 calc R . . C41 C 0.39424(15) 0.46285(9) 0.53133(11) 0.0499(5) Uani 1 1 d . . . H41 H 0.3912 0.4825 0.4887 0.060 Uiso 1 1 calc R . . C42 C 0.41707(13) 0.48568(7) 0.59840(10) 0.0400(4) Uani 1 1 d . . . H42 H 0.4286 0.5209 0.6013 0.048 Uiso 1 1 calc R . . C43 C 0.49057(11) 0.54702(6) 0.73030(9) 0.0299(3) Uani 1 1 d . . . C44 C 0.58077(11) 0.55208(6) 0.71258(9) 0.0321(3) Uani 1 1 d . . . H44 H 0.6222 0.5241 0.7175 0.039 Uiso 1 1 calc R . . C45 C 0.61106(12) 0.59787(6) 0.68764(10) 0.0353(3) Uani 1 1 d . . . H45 H 0.6729 0.6011 0.6754 0.042 Uiso 1 1 calc R . . C46 C 0.55105(15) 0.63828(7) 0.68078(12) 0.0470(4) Uani 1 1 d . . . H46 H 0.5712 0.6695 0.6633 0.056 Uiso 1 1 calc R . . C47 C 0.46119(17) 0.63372(8) 0.69929(17) 0.0655(7) Uani 1 1 d . . . H47 H 0.4199 0.6618 0.6946 0.079 Uiso 1 1 calc R . . C48 C 0.43130(14) 0.58800(8) 0.72482(14) 0.0525(5) Uani 1 1 d . . . H48 H 0.3701 0.5851 0.7384 0.063 Uiso 1 1 calc R . . C49 C 0.97846(13) 0.15615(6) 0.87257(10) 0.0371(4) Uani 1 1 d . . . C50 C 0.90536(14) 0.13955(7) 0.82088(11) 0.0447(4) Uani 1 1 d . . . H50 H 0.9148 0.1396 0.7715 0.054 Uiso 1 1 calc R . . C51 C 0.82065(15) 0.12316(8) 0.83880(13) 0.0517(5) Uani 1 1 d . . . H51 H 0.7724 0.1134 0.8019 0.062 Uiso 1 1 calc R . . C52 C 0.80547(14) 0.12077(8) 0.90941(14) 0.0523(5) Uani 1 1 d . . . H52 H 0.7474 0.1088 0.9218 0.063 Uiso 1 1 calc R . . C53 C 0.87630(15) 0.13607(9) 0.96299(13) 0.0504(5) Uani 1 1 d . . . H53 H 0.8670 0.1343 1.0123 0.061 Uiso 1 1 calc R . . C54 C 0.96065(13) 0.15391(8) 0.94387(11) 0.0427(4) Uani 1 1 d . . . H54 H 1.0078 0.1650 0.9809 0.051 Uiso 1 1 calc R . . C55 C 1.07317(14) 0.20205(6) 0.77263(10) 0.0398(4) Uani 1 1 d . . . C56 C 0.99502(16) 0.23124(7) 0.74620(10) 0.0458(4) Uani 1 1 d . . . H56 H 0.9425 0.2319 0.7723 0.055 Uiso 1 1 calc R . . C57 C 0.9919(2) 0.25951(8) 0.68231(12) 0.0570(6) Uani 1 1 d . . . H57 H 0.9376 0.2787 0.6658 0.068 Uiso 1 1 calc R . . C58 C 1.0670(2) 0.25954(8) 0.64363(11) 0.0575(6) Uani 1 1 d . . . H58 H 1.0646 0.2782 0.6001 0.069 Uiso 1 1 calc R . . C59 C 1.14603(18) 0.23214(8) 0.66899(11) 0.0516(5) Uani 1 1 d . . . H59 H 1.1988 0.2324 0.6432 0.062 Uiso 1 1 calc R . . C60 C 1.14858(15) 0.20418(7) 0.73223(10) 0.0443(4) Uani 1 1 d . . . H60 H 1.2038 0.1858 0.7487 0.053 Uiso 1 1 calc R . . C61 C 1.12638(12) 0.11333(6) 0.83964(10) 0.0344(3) Uani 1 1 d . . . C62 C 1.15762(12) 0.08427(7) 0.90102(10) 0.0368(4) Uani 1 1 d . . . H62 H 1.1569 0.0988 0.9474 0.044 Uiso 1 1 calc R . . C63 C 1.18930(13) 0.03538(7) 0.89643(11) 0.0403(4) Uani 1 1 d . . . H63 H 1.2090 0.0170 0.9393 0.048 Uiso 1 1 calc R . . C64 C 1.19257(13) 0.01294(7) 0.82965(12) 0.0413(4) Uani 1 1 d . . . H64 H 1.2153 -0.0204 0.8263 0.050 Uiso 1 1 calc R . . C65 C 1.16197(13) 0.04038(7) 0.76808(11) 0.0405(4) Uani 1 1 d . . . H65 H 1.1637 0.0257 0.7219 0.049 Uiso 1 1 calc R . . C66 C 1.12866(12) 0.08929(7) 0.77326(10) 0.0374(4) Uani 1 1 d . . . H66 H 1.1067 0.1070 0.7302 0.045 Uiso 1 1 calc R . . C67 C 1.14741(13) 0.20413(6) 0.90746(9) 0.0349(3) Uani 1 1 d . . . C68 C 1.11130(14) 0.24644(7) 0.93910(10) 0.0402(4) Uani 1 1 d . . . H68 H 1.0460 0.2531 0.9293 0.048 Uiso 1 1 calc R . . C69 C 1.16716(15) 0.27895(7) 0.98415(10) 0.0447(4) Uani 1 1 d . . . H69 H 1.1397 0.3073 1.0041 0.054 Uiso 1 1 calc R . . C70 C 1.26241(15) 0.27044(7) 1.00025(10) 0.0448(4) Uani 1 1 d . . . H70 H 1.3006 0.2926 1.0312 0.054 Uiso 1 1 calc R . . C71 C 1.30101(14) 0.22889(7) 0.97029(10) 0.0413(4) Uani 1 1 d . . . H71 H 1.3662 0.2222 0.9810 0.050 Uiso 1 1 calc R . . C72 C 1.24444(13) 0.19691(6) 0.92450(10) 0.0373(4) Uani 1 1 d . . . H72 H 1.2727 0.1690 0.9039 0.045 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 Ru 0.02317(7) 0.02165(7) 0.03130(7) -0.00188(4) -0.00038(4) -0.00217(4) Cl 0.03526(19) 0.03208(19) 0.0468(2) -0.01022(16) 0.00300(16) -0.00838(15) P1 0.02396(17) 0.02398(17) 0.03106(19) -0.00179(13) -0.00004(14) -0.00183(13) P2 0.02397(17) 0.02296(17) 0.03118(19) -0.00005(14) 0.00002(14) -0.00184(13) N1 0.0341(7) 0.0297(7) 0.0368(7) -0.0022(6) -0.0078(6) -0.0010(5) N2 0.0306(6) 0.0207(6) 0.0382(7) -0.0017(5) 0.0002(5) -0.0004(5) B 0.0405(10) 0.0303(9) 0.0341(9) 0.0007(7) -0.0010(8) -0.0008(7) C1 0.0261(7) 0.0271(7) 0.0354(8) -0.0011(6) 0.0021(6) -0.0009(6) C2 0.0250(7) 0.0274(7) 0.0329(8) -0.0015(6) 0.0013(6) -0.0017(6) C3 0.0375(9) 0.0350(9) 0.0423(9) 0.0045(7) -0.0053(7) 0.0001(7) C4 0.0364(9) 0.0392(9) 0.0448(10) -0.0021(8) -0.0067(7) 0.0032(7) C5 0.0371(9) 0.0458(10) 0.0446(10) -0.0064(8) -0.0086(8) 0.0044(8) C6 0.0399(9) 0.0403(9) 0.0425(10) -0.0091(8) -0.0062(7) -0.0059(7) C7 0.0453(10) 0.0357(9) 0.0437(10) -0.0091(7) -0.0108(8) 0.0035(7) C8 0.0363(8) 0.0266(7) 0.0363(8) 0.0021(6) -0.0015(7) 0.0007(6) C9 0.0333(8) 0.0270(8) 0.0511(10) 0.0033(7) -0.0014(7) 0.0029(6) C10 0.0386(9) 0.0257(8) 0.0573(11) 0.0003(7) 0.0075(8) 0.0041(7) C11 0.0439(9) 0.0244(8) 0.0500(10) -0.0058(7) 0.0066(8) -0.0005(7) C12 0.0364(8) 0.0230(7) 0.0479(10) -0.0055(7) -0.0011(7) -0.0020(6) C13 0.0320(8) 0.0254(7) 0.0327(8) -0.0024(6) -0.0018(6) -0.0012(6) C14 0.0327(8) 0.0278(7) 0.0393(8) -0.0034(6) -0.0013(6) -0.0035(6) C15 0.0392(9) 0.0364(9) 0.0433(10) -0.0033(7) -0.0130(7) -0.0040(7) C16 0.0570(11) 0.0370(9) 0.0330(9) 0.0003(7) -0.0088(8) -0.0046(8) C17 0.0483(10) 0.0384(9) 0.0346(9) -0.0003(7) 0.0015(7) -0.0087(8) C18 0.0346(8) 0.0371(9) 0.0342(8) -0.0020(7) 0.0013(7) -0.0048(7) C19 0.0248(7) 0.0269(7) 0.0358(8) -0.0041(6) -0.0013(6) -0.0016(6) C20 0.0267(7) 0.0372(8) 0.0353(8) -0.0018(6) -0.0001(6) 0.0021(6) C21 0.0311(8) 0.0417(9) 0.0407(9) -0.0074(7) 0.0031(7) 0.0035(7) C22 0.0384(9) 0.0343(9) 0.0481(10) -0.0073(7) 0.0001(7) 0.0051(7) C23 0.0646(12) 0.0329(9) 0.0456(10) 0.0031(8) 0.0039(9) 0.0084(8) C24 0.0566(11) 0.0309(8) 0.0378(9) -0.0010(7) 0.0070(8) 0.0047(8) C25 0.0264(7) 0.0275(7) 0.0317(7) -0.0015(6) 0.0015(6) -0.0021(6) C26 0.0262(7) 0.0299(8) 0.0377(8) -0.0012(6) 0.0012(6) -0.0001(6) C27 0.0338(8) 0.0266(7) 0.0419(9) -0.0031(6) 0.0017(7) -0.0032(6) C28 0.0325(8) 0.0345(8) 0.0404(9) -0.0042(7) -0.0031(7) -0.0062(7) C29 0.0304(8) 0.0352(9) 0.0421(9) 0.0030(7) -0.0039(7) -0.0009(6) C30 0.0307(8) 0.0283(7) 0.0366(8) 0.0004(6) -0.0015(6) -0.0006(6) C31 0.0261(7) 0.0224(7) 0.0384(8) -0.0004(6) -0.0001(6) -0.0030(5) C32 0.0296(8) 0.0313(8) 0.0434(9) -0.0022(7) 0.0029(7) 0.0006(6) C33 0.0320(8) 0.0369(9) 0.0572(11) -0.0059(8) 0.0031(8) 0.0054(7) C34 0.0331(8) 0.0352(9) 0.0582(12) -0.0007(8) -0.0114(8) 0.0043(7) C35 0.0396(9) 0.0324(8) 0.0422(9) -0.0014(7) -0.0089(7) -0.0015(7) C36 0.0299(7) 0.0266(7) 0.0380(8) -0.0025(6) -0.0016(6) -0.0022(6) C37 0.0265(7) 0.0351(8) 0.0337(8) -0.0029(6) -0.0004(6) -0.0038(6) C38 0.0437(9) 0.0361(9) 0.0363(9) -0.0059(7) 0.0054(7) -0.0077(7) C39 0.0508(11) 0.0449(10) 0.0464(10) -0.0136(8) 0.0080(8) -0.0128(8) C40 0.0499(11) 0.0662(13) 0.0370(10) -0.0132(9) -0.0014(8) -0.0123(10) C41 0.0493(11) 0.0621(13) 0.0353(9) 0.0026(9) -0.0056(8) -0.0067(10) C42 0.0392(9) 0.0437(10) 0.0350(9) 0.0035(7) -0.0037(7) -0.0055(7) C43 0.0297(7) 0.0247(7) 0.0345(8) 0.0006(6) 0.0004(6) -0.0024(6) C44 0.0296(7) 0.0278(8) 0.0377(8) 0.0021(6) -0.0003(6) -0.0014(6) C45 0.0334(8) 0.0332(8) 0.0391(9) 0.0025(7) 0.0033(7) -0.0058(6) C46 0.0528(11) 0.0273(8) 0.0628(12) 0.0094(8) 0.0145(9) -0.0029(8) C47 0.0569(13) 0.0326(10) 0.113(2) 0.0225(12) 0.0332(13) 0.0145(9) C48 0.0382(10) 0.0345(9) 0.0879(16) 0.0140(10) 0.0204(10) 0.0051(8) C49 0.0391(9) 0.0279(8) 0.0430(9) 0.0029(7) 0.0002(7) 0.0050(7) C50 0.0473(10) 0.0373(9) 0.0478(10) -0.0021(8) -0.0010(8) -0.0004(8) C51 0.0439(10) 0.0438(11) 0.0644(13) 0.0000(9) -0.0044(9) -0.0013(8) C52 0.0339(9) 0.0431(11) 0.0795(15) 0.0068(10) 0.0060(9) 0.0033(8) C53 0.0453(10) 0.0524(12) 0.0546(12) 0.0132(9) 0.0104(9) 0.0084(9) C54 0.0388(9) 0.0436(10) 0.0448(10) 0.0067(8) 0.0018(8) 0.0054(8) C55 0.0561(11) 0.0267(8) 0.0344(8) -0.0030(6) -0.0027(8) -0.0047(7) C56 0.0681(13) 0.0306(9) 0.0368(9) -0.0015(7) 0.0000(9) 0.0054(9) C57 0.0923(17) 0.0313(9) 0.0431(11) -0.0007(8) -0.0072(11) 0.0105(10) C58 0.1052(19) 0.0338(9) 0.0324(9) 0.0006(7) 0.0048(11) -0.0077(11) C59 0.0780(15) 0.0394(10) 0.0365(10) -0.0006(8) 0.0046(9) -0.0160(10) C60 0.0581(11) 0.0362(9) 0.0375(9) -0.0011(7) 0.0022(8) -0.0130(8) C61 0.0330(8) 0.0297(8) 0.0396(9) 0.0010(7) 0.0020(7) -0.0044(6) C62 0.0356(8) 0.0331(8) 0.0408(9) 0.0008(7) 0.0022(7) -0.0032(7) C63 0.0355(9) 0.0315(8) 0.0521(11) 0.0058(7) -0.0006(8) -0.0031(7) C64 0.0344(9) 0.0289(8) 0.0599(12) -0.0026(8) 0.0034(8) -0.0027(7) C65 0.0370(9) 0.0346(9) 0.0501(10) -0.0070(7) 0.0060(8) -0.0074(7) C66 0.0373(9) 0.0336(8) 0.0404(9) -0.0007(7) 0.0019(7) -0.0052(7) C67 0.0438(9) 0.0302(8) 0.0301(8) 0.0044(6) 0.0022(7) -0.0024(7) C68 0.0482(10) 0.0356(9) 0.0357(9) 0.0007(7) 0.0016(7) 0.0034(7) C69 0.0632(12) 0.0337(9) 0.0368(9) -0.0026(7) 0.0047(8) 0.0019(8) C70 0.0623(12) 0.0370(9) 0.0337(9) -0.0017(7) 0.0005(8) -0.0120(8) C71 0.0420(9) 0.0406(9) 0.0398(9) 0.0063(7) -0.0001(7) -0.0071(7) C72 0.0448(9) 0.0286(8) 0.0385(9) 0.0019(6) 0.0051(7) -0.0016(7) _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 Ru C2 1.9174(16) . ? Ru C1 1.9265(16) . ? Ru P1 2.3839(4) . ? Ru Cl 2.3856(4) . ? Ru P2 2.3959(4) . ? P1 C19 1.8291(16) . ? P1 C13 1.8298(17) . ? P1 C25 1.8310(16) . ? P2 C43 1.8265(16) . ? P2 C31 1.8279(16) . ? P2 C37 1.8349(17) . ? N1 C1 1.298(2) . ? N1 C7 1.478(2) . ? N1 C3 1.480(2) . ? N2 C2 1.303(2) . ? N2 C8 1.477(2) . ? N2 C12 1.480(2) . ? B C49 1.639(3) . ? B C67 1.643(3) . ? B C61 1.643(3) . ? B C55 1.653(3) . ? C1 C2 1.404(2) . ? C3 C4 1.515(2) . ? C4 C5 1.534(3) . ? C5 C6 1.526(3) . ? C6 C7 1.518(3) . ? C8 C9 1.523(2) . ? C9 C10 1.527(2) . ? C10 C11 1.524(3) . ? C11 C12 1.528(2) . ? C13 C14 1.391(2) . ? C13 C18 1.394(2) . ? C14 C15 1.394(3) . ? C15 C16 1.383(3) . ? C16 C17 1.388(3) . ? C17 C18 1.389(3) . ? C19 C20 1.390(2) . ? C19 C24 1.392(2) . ? C20 C21 1.392(2) . ? C21 C22 1.377(3) . ? C22 C23 1.380(3) . ? C23 C24 1.397(3) . ? C25 C26 1.398(2) . ? C25 C30 1.399(2) . ? C26 C27 1.391(2) . ? C27 C28 1.389(2) . ? C28 C29 1.383(3) . ? C29 C30 1.391(2) . ? C31 C36 1.395(2) . ? C31 C32 1.395(2) . ? C32 C33 1.387(2) . ? C33 C34 1.387(3) . ? C34 C35 1.384(3) . ? C35 C36 1.393(2) . ? C37 C42 1.393(3) . ? C37 C38 1.396(2) . ? C38 C39 1.391(3) . ? C39 C40 1.381(3) . ? C40 C41 1.380(3) . ? C41 C42 1.394(3) . ? C43 C48 1.379(2) . ? C43 C44 1.386(2) . ? C44 C45 1.393(2) . ? C45 C46 1.374(3) . ? C46 C47 1.385(3) . ? C47 C48 1.394(3) . ? C49 C54 1.390(3) . ? C49 C50 1.404(3) . ? C50 C51 1.375(3) . ? C51 C52 1.367(4) . ? C52 C53 1.394(3) . ? C53 C54 1.391(3) . ? C55 C60 1.400(3) . ? C55 C56 1.402(3) . ? C56 C57 1.407(3) . ? C57 C58 1.375(4) . ? C58 C59 1.381(4) . ? C59 C60 1.393(3) . ? C61 C66 1.400(3) . ? C61 C62 1.408(2) . ? C62 C63 1.384(3) . ? C63 C64 1.390(3) . ? C64 C65 1.386(3) . ? C65 C66 1.393(3) . ? C67 C68 1.401(3) . ? C67 C72 1.404(3) . ? C68 C69 1.388(3) . ? C69 C70 1.383(3) . ? C70 C71 1.386(3) . ? C71 C72 1.392(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ru C1 42.85(7) . . ? C2 Ru P1 89.86(5) . . ? C1 Ru P1 92.90(5) . . ? C2 Ru Cl 153.78(5) . . ? C1 Ru Cl 163.19(5) . . ? P1 Ru Cl 86.253(14) . . ? C2 Ru P2 92.71(5) . . ? C1 Ru P2 92.30(5) . . ? P1 Ru P2 174.475(14) . . ? Cl Ru P2 89.294(14) . . ? C19 P1 C13 105.66(7) . . ? C19 P1 C25 104.33(7) . . ? C13 P1 C25 102.26(7) . . ? C19 P1 Ru 116.33(6) . . ? C13 P1 Ru 114.09(6) . . ? C25 P1 Ru 112.76(5) . . ? C43 P2 C31 103.91(7) . . ? C43 P2 C37 101.32(8) . . ? C31 P2 C37 104.17(8) . . ? C43 P2 Ru 119.45(6) . . ? C31 P2 Ru 111.82(5) . . ? C37 P2 Ru 114.46(5) . . ? C1 N1 C7 125.89(15) . . ? C1 N1 C3 119.17(14) . . ? C7 N1 C3 114.66(14) . . ? C2 N2 C8 119.48(13) . . ? C2 N2 C12 127.06(14) . . ? C8 N2 C12 113.46(13) . . ? C49 B C67 113.65(15) . . ? C49 B C61 102.33(14) . . ? C67 B C61 112.05(14) . . ? C49 B C55 112.44(15) . . ? C67 B C55 104.59(14) . . ? C61 B C55 112.04(15) . . ? N1 C1 C2 146.56(16) . . ? N1 C1 Ru 144.95(13) . . ? C2 C1 Ru 68.23(9) . . ? N2 C2 C1 148.11(15) . . ? N2 C2 Ru 142.96(12) . . ? C1 C2 Ru 68.92(9) . . ? N1 C3 C4 111.38(15) . . ? C3 C4 C5 110.28(16) . . ? C6 C5 C4 109.76(15) . . ? C7 C6 C5 110.90(16) . . ? N1 C7 C6 110.15(15) . . ? N2 C8 C9 109.78(14) . . ? C8 C9 C10 110.57(14) . . ? C11 C10 C9 111.20(14) . . ? C10 C11 C12 111.41(15) . . ? N2 C12 C11 109.91(14) . . ? C14 C13 C18 119.26(15) . . ? C14 C13 P1 120.26(13) . . ? C18 C13 P1 120.48(12) . . ? C13 C14 C15 119.95(16) . . ? C16 C15 C14 120.45(17) . . ? C15 C16 C17 119.86(17) . . ? C16 C17 C18 119.90(18) . . ? C17 C18 C13 120.57(16) . . ? C20 C19 C24 119.04(16) . . ? C20 C19 P1 122.11(13) . . ? C24 C19 P1 118.83(13) . . ? C19 C20 C21 120.40(16) . . ? C22 C21 C20 120.29(17) . . ? C21 C22 C23 119.87(17) . . ? C22 C23 C24 120.29(18) . . ? C19 C24 C23 120.09(18) . . ? C26 C25 C30 118.81(14) . . ? C26 C25 P1 118.64(12) . . ? C30 C25 P1 122.35(12) . . ? C27 C26 C25 120.88(15) . . ? C28 C27 C26 119.82(16) . . ? C29 C28 C27 119.72(15) . . ? C28 C29 C30 120.90(16) . . ? C29 C30 C25 119.86(15) . . ? C36 C31 C32 119.44(15) . . ? C36 C31 P2 118.10(12) . . ? C32 C31 P2 122.45(13) . . ? C33 C32 C31 119.92(17) . . ? C34 C33 C32 120.30(17) . . ? C35 C34 C33 120.31(16) . . ? C34 C35 C36 119.64(17) . . ? C35 C36 C31 120.38(16) . . ? C42 C37 C38 118.65(16) . . ? C42 C37 P2 122.25(14) . . ? C38 C37 P2 118.97(13) . . ? C39 C38 C37 120.88(18) . . ? C40 C39 C38 119.88(19) . . ? C41 C40 C39 119.85(19) . . ? C40 C41 C42 120.64(19) . . ? C37 C42 C41 120.09(18) . . ? C48 C43 C44 119.62(16) . . ? C48 C43 P2 119.49(13) . . ? C44 C43 P2 120.56(12) . . ? C43 C44 C45 120.47(16) . . ? C46 C45 C44 119.66(16) . . ? C45 C46 C47 120.21(17) . . ? C46 C47 C48 120.04(19) . . ? C43 C48 C47 119.96(18) . . ? C54 C49 C50 115.60(18) . . ? C54 C49 B 123.82(16) . . ? C50 C49 B 120.06(17) . . ? C51 C50 C49 122.7(2) . . ? C52 C51 C50 120.4(2) . . ? C51 C52 C53 119.2(2) . . ? C54 C53 C52 119.7(2) . . ? C49 C54 C53 122.34(19) . . ? C60 C55 C56 115.40(18) . . ? C60 C55 B 120.62(17) . . ? C56 C55 B 123.89(18) . . ? C55 C56 C57 122.1(2) . . ? C58 C57 C56 120.3(2) . . ? C57 C58 C59 119.13(19) . . ? C58 C59 C60 120.2(2) . . ? C59 C60 C55 122.8(2) . . ? C66 C61 C62 115.50(16) . . ? C66 C61 B 123.92(16) . . ? C62 C61 B 120.31(16) . . ? C63 C62 C61 122.54(18) . . ? C62 C63 C64 120.56(18) . . ? C65 C64 C63 118.42(17) . . ? C64 C65 C66 120.61(18) . . ? C65 C66 C61 122.34(18) . . ? C68 C67 C72 115.18(16) . . ? C68 C67 B 121.33(16) . . ? C72 C67 B 123.21(16) . . ? C69 C68 C67 122.60(18) . . ? C70 C69 C68 120.66(18) . . ? C69 C70 C71 118.64(18) . . ? C70 C71 C72 120.15(18) . . ? C71 C72 C67 122.76(17) . . ? 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 C2 Ru P1 C19 -159.11(7) . . . . ? C1 Ru P1 C19 -116.35(7) . . . . ? Cl Ru P1 C19 46.83(6) . . . . ? P2 Ru P1 C19 83.20(15) . . . . ? C2 Ru P1 C13 77.45(7) . . . . ? C1 Ru P1 C13 120.21(7) . . . . ? Cl Ru P1 C13 -76.61(6) . . . . ? P2 Ru P1 C13 -40.24(16) . . . . ? C2 Ru P1 C25 -38.65(7) . . . . ? C1 Ru P1 C25 4.12(7) . . . . ? Cl Ru P1 C25 167.30(6) . . . . ? P2 Ru P1 C25 -156.33(14) . . . . ? C2 Ru P2 C43 166.83(8) . . . . ? C1 Ru P2 C43 123.94(8) . . . . ? P1 Ru P2 C43 -75.60(16) . . . . ? Cl Ru P2 C43 -39.32(6) . . . . ? C2 Ru P2 C31 -71.61(7) . . . . ? C1 Ru P2 C31 -114.50(7) . . . . ? P1 Ru P2 C31 45.96(16) . . . . ? Cl Ru P2 C31 82.23(5) . . . . ? C2 Ru P2 C37 46.54(8) . . . . ? C1 Ru P2 C37 3.64(8) . . . . ? P1 Ru P2 C37 164.10(14) . . . . ? Cl Ru P2 C37 -159.62(6) . . . . ? C7 N1 C1 C2 4.7(4) . . . . ? C3 N1 C1 C2 -168.9(2) . . . . ? C7 N1 C1 Ru 175.39(17) . . . . ? C3 N1 C1 Ru 1.8(3) . . . . ? C2 Ru C1 N1 -174.5(3) . . . . ? P1 Ru C1 N1 98.9(2) . . . . ? Cl Ru C1 N1 12.2(4) . . . . ? P2 Ru C1 N1 -83.0(2) . . . . ? P1 Ru C1 C2 -86.65(9) . . . . ? Cl Ru C1 C2 -173.30(13) . . . . ? P2 Ru C1 C2 91.50(9) . . . . ? C8 N2 C2 C1 174.7(2) . . . . ? C12 N2 C2 C1 -5.5(4) . . . . ? C8 N2 C2 Ru -3.6(3) . . . . ? C12 N2 C2 Ru 176.19(15) . . . . ? N1 C1 C2 N2 -4.7(5) . . . . ? Ru C1 C2 N2 -178.9(3) . . . . ? N1 C1 C2 Ru 174.3(3) . . . . ? C1 Ru C2 N2 179.1(3) . . . . ? P1 Ru C2 N2 -86.5(2) . . . . ? Cl Ru C2 N2 -5.3(3) . . . . ? P2 Ru C2 N2 88.6(2) . . . . ? P1 Ru C2 C1 94.43(9) . . . . ? Cl Ru C2 C1 175.62(8) . . . . ? P2 Ru C2 C1 -90.47(9) . . . . ? C1 N1 C3 C4 -131.43(17) . . . . ? C7 N1 C3 C4 54.3(2) . . . . ? N1 C3 C4 C5 -54.2(2) . . . . ? C3 C4 C5 C6 56.6(2) . . . . ? C4 C5 C6 C7 -57.8(2) . . . . ? C1 N1 C7 C6 131.73(18) . . . . ? C3 N1 C7 C6 -54.4(2) . . . . ? C5 C6 C7 N1 55.7(2) . . . . ? C2 N2 C8 C9 -120.86(16) . . . . ? C12 N2 C8 C9 59.31(18) . . . . ? N2 C8 C9 C10 -56.30(19) . . . . ? C8 C9 C10 C11 54.5(2) . . . . ? C9 C10 C11 C12 -53.4(2) . . . . ? C2 N2 C12 C11 122.35(18) . . . . ? C8 N2 C12 C11 -57.84(19) . . . . ? C10 C11 C12 N2 53.9(2) . . . . ? C19 P1 C13 C14 -103.65(14) . . . . ? C25 P1 C13 C14 147.44(13) . . . . ? Ru P1 C13 C14 25.38(15) . . . . ? C19 P1 C13 C18 77.11(15) . . . . ? C25 P1 C13 C18 -31.79(15) . . . . ? Ru P1 C13 C18 -153.85(12) . . . . ? C18 C13 C14 C15 0.7(2) . . . . ? P1 C13 C14 C15 -178.59(13) . . . . ? C13 C14 C15 C16 0.4(3) . . . . ? C14 C15 C16 C17 -1.0(3) . . . . ? C15 C16 C17 C18 0.4(3) . . . . ? C16 C17 C18 C13 0.8(3) . . . . ? C14 C13 C18 C17 -1.3(3) . . . . ? P1 C13 C18 C17 177.99(14) . . . . ? C13 P1 C19 C20 -15.37(15) . . . . ? C25 P1 C19 C20 92.04(14) . . . . ? Ru P1 C19 C20 -143.08(12) . . . . ? C13 P1 C19 C24 166.00(14) . . . . ? C25 P1 C19 C24 -86.59(15) . . . . ? Ru P1 C19 C24 38.29(15) . . . . ? C24 C19 C20 C21 0.7(2) . . . . ? P1 C19 C20 C21 -177.97(13) . . . . ? C19 C20 C21 C22 0.0(3) . . . . ? C20 C21 C22 C23 -0.1(3) . . . . ? C21 C22 C23 C24 -0.5(3) . . . . ? C20 C19 C24 C23 -1.3(3) . . . . ? P1 C19 C24 C23 177.41(16) . . . . ? C22 C23 C24 C19 1.2(3) . . . . ? C19 P1 C25 C26 -159.68(13) . . . . ? C13 P1 C25 C26 -49.77(15) . . . . ? Ru P1 C25 C26 73.20(14) . . . . ? C19 P1 C25 C30 25.61(16) . . . . ? C13 P1 C25 C30 135.52(14) . . . . ? Ru P1 C25 C30 -101.51(14) . . . . ? C30 C25 C26 C27 1.0(2) . . . . ? P1 C25 C26 C27 -173.90(13) . . . . ? C25 C26 C27 C28 -0.9(3) . . . . ? C26 C27 C28 C29 -0.3(3) . . . . ? C27 C28 C29 C30 1.3(3) . . . . ? C28 C29 C30 C25 -1.2(3) . . . . ? C26 C25 C30 C29 0.0(3) . . . . ? P1 C25 C30 C29 174.70(14) . . . . ? C43 P2 C31 C36 92.25(13) . . . . ? C37 P2 C31 C36 -162.03(12) . . . . ? Ru P2 C31 C36 -37.90(13) . . . . ? C43 P2 C31 C32 -86.43(14) . . . . ? C37 P2 C31 C32 19.30(15) . . . . ? Ru P2 C31 C32 143.43(12) . . . . ? C36 C31 C32 C33 0.3(2) . . . . ? P2 C31 C32 C33 178.91(13) . . . . ? C31 C32 C33 C34 -0.1(3) . . . . ? C32 C33 C34 C35 -0.5(3) . . . . ? C33 C34 C35 C36 0.8(3) . . . . ? C34 C35 C36 C31 -0.6(3) . . . . ? C32 C31 C36 C35 0.1(2) . . . . ? P2 C31 C36 C35 -178.64(13) . . . . ? C43 P2 C37 C42 -17.04(16) . . . . ? C31 P2 C37 C42 -124.70(15) . . . . ? Ru P2 C37 C42 112.89(14) . . . . ? C43 P2 C37 C38 167.08(14) . . . . ? C31 P2 C37 C38 59.42(15) . . . . ? Ru P2 C37 C38 -62.99(15) . . . . ? C42 C37 C38 C39 -0.6(3) . . . . ? P2 C37 C38 C39 175.41(15) . . . . ? C37 C38 C39 C40 0.7(3) . . . . ? C38 C39 C40 C41 0.1(3) . . . . ? C39 C40 C41 C42 -0.9(3) . . . . ? C38 C37 C42 C41 -0.2(3) . . . . ? P2 C37 C42 C41 -176.06(15) . . . . ? C40 C41 C42 C37 0.9(3) . . . . ? C31 P2 C43 C48 -153.71(17) . . . . ? C37 P2 C43 C48 98.43(18) . . . . ? Ru P2 C43 C48 -28.30(19) . . . . ? C31 P2 C43 C44 32.97(16) . . . . ? C37 P2 C43 C44 -74.89(15) . . . . ? Ru P2 C43 C44 158.38(12) . . . . ? C48 C43 C44 C45 -1.6(3) . . . . ? P2 C43 C44 C45 171.72(13) . . . . ? C43 C44 C45 C46 0.2(3) . . . . ? C44 C45 C46 C47 0.7(3) . . . . ? C45 C46 C47 C48 -0.1(4) . . . . ? C44 C43 C48 C47 2.1(4) . . . . ? P2 C43 C48 C47 -171.2(2) . . . . ? C46 C47 C48 C43 -1.3(4) . . . . ? C67 B C49 C54 -26.6(2) . . . . ? C61 B C49 C54 94.4(2) . . . . ? C55 B C49 C54 -145.21(17) . . . . ? C67 B C49 C50 162.07(16) . . . . ? C61 B C49 C50 -76.92(19) . . . . ? C55 B C49 C50 43.5(2) . . . . ? C54 C49 C50 C51 1.4(3) . . . . ? B C49 C50 C51 173.44(18) . . . . ? C49 C50 C51 C52 -2.3(3) . . . . ? C50 C51 C52 C53 1.2(3) . . . . ? C51 C52 C53 C54 0.6(3) . . . . ? C50 C49 C54 C53 0.5(3) . . . . ? B C49 C54 C53 -171.21(18) . . . . ? C52 C53 C54 C49 -1.5(3) . . . . ? C49 B C55 C60 -160.86(16) . . . . ? C67 B C55 C60 75.4(2) . . . . ? C61 B C55 C60 -46.2(2) . . . . ? C49 B C55 C56 22.8(2) . . . . ? C67 B C55 C56 -101.02(19) . . . . ? C61 B C55 C56 137.38(17) . . . . ? C60 C55 C56 C57 1.8(3) . . . . ? B C55 C56 C57 178.30(17) . . . . ? C55 C56 C57 C58 -0.5(3) . . . . ? C56 C57 C58 C59 -1.1(3) . . . . ? C57 C58 C59 C60 1.1(3) . . . . ? C58 C59 C60 C55 0.3(3) . . . . ? C56 C55 C60 C59 -1.7(3) . . . . ? B C55 C60 C59 -178.34(17) . . . . ? C49 B C61 C66 100.72(19) . . . . ? C67 B C61 C66 -137.17(17) . . . . ? C55 B C61 C66 -20.0(2) . . . . ? C49 B C61 C62 -73.09(19) . . . . ? C67 B C61 C62 49.0(2) . . . . ? C55 B C61 C62 166.24(15) . . . . ? C66 C61 C62 C63 0.5(3) . . . . ? B C61 C62 C63 174.85(16) . . . . ? C61 C62 C63 C64 0.8(3) . . . . ? C62 C63 C64 C65 -1.0(3) . . . . ? C63 C64 C65 C66 -0.1(3) . . . . ? C64 C65 C66 C61 1.5(3) . . . . ? C62 C61 C66 C65 -1.7(3) . . . . ? B C61 C66 C65 -175.76(16) . . . . ? C49 B C67 C68 -45.5(2) . . . . ? C61 B C67 C68 -160.94(16) . . . . ? C55 B C67 C68 77.5(2) . . . . ? C49 B C67 C72 140.84(17) . . . . ? C61 B C67 C72 25.4(2) . . . . ? C55 B C67 C72 -96.16(19) . . . . ? C72 C67 C68 C69 -0.1(3) . . . . ? B C67 C68 C69 -174.18(17) . . . . ? C67 C68 C69 C70 -0.5(3) . . . . ? C68 C69 C70 C71 0.2(3) . . . . ? C69 C70 C71 C72 0.6(3) . . . . ? C70 C71 C72 C67 -1.2(3) . . . . ? C68 C67 C72 C71 0.9(3) . . . . ? B C67 C72 C71 174.87(16) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 72.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.503 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.049 #============================================================================= # end of cif data for "pet19a" (compound 4b) #============================================================================= #============================================================================= # cif data for "pet27" (compound 5) #============================================================================= data_pet27 _database_code_depnum_ccdc_archive 'CCDC 819870' #TrackingRef 'pet-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100.99 H97.49 B2 N4.49 P2 Ru' _chemical_formula_weight 1558.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 '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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6660(2) _cell_length_b 26.9068(6) _cell_length_c 26.0151(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.058(2) _cell_angle_gamma 90.00 _cell_volume 8104.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22229 _cell_measurement_theta_min 3.2823 _cell_measurement_theta_max 75.9112 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3276 _exptl_absorpt_coefficient_mu 2.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83168 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93253 _diffrn_reflns_av_R_equivalents 0.0925 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 76.10 _reflns_number_total 16852 _reflns_number_gt 11688 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0465P)^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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16852 _refine_ls_number_parameters 939 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.091 _refine_ls_shift/su_mean 0.001 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 Ru Ru 0.927740(15) 0.717785(6) 0.123799(7) 0.01560(5) Uani 1 1 d . . . P1 P 1.13272(5) 0.71627(2) 0.11998(2) 0.01609(11) Uani 1 1 d . . . P2 P 0.71851(5) 0.72271(2) 0.11705(2) 0.01847(12) Uani 1 1 d . . . B1 B 0.3471(3) 0.41625(10) 0.14810(11) 0.0223(5) Uani 1 1 d . . . B2 B 0.7169(3) 0.58448(13) 0.40615(12) 0.0324(7) Uani 1 1 d . . . N1 N 0.88565(18) 0.60178(7) 0.11696(8) 0.0205(4) Uani 1 1 d . . . N2 N 0.96993(19) 0.66721(8) 0.23119(8) 0.0241(4) Uani 1 1 d . . . N3 N 0.91690(18) 0.75302(7) 0.04881(8) 0.0215(4) Uani 1 1 d . . . N4 N 0.93653(17) 0.79195(7) 0.15156(8) 0.0209(4) Uani 1 1 d . . . C1 C 0.91780(19) 0.64579(9) 0.13349(9) 0.0191(5) Uani 1 1 d . . . C2 C 0.9437(2) 0.67217(9) 0.18107(10) 0.0207(5) Uani 1 1 d . . . C3 C 0.8620(2) 0.59047(9) 0.06106(9) 0.0223(5) Uani 1 1 d . . . H3A H 0.8734 0.6207 0.0406 0.027 Uiso 1 1 calc R . . H3B H 0.7809 0.5795 0.0526 0.027 Uiso 1 1 calc R . . C4 C 0.9437(2) 0.54952(10) 0.04730(10) 0.0273(5) Uani 1 1 d . . . H4A H 1.0238 0.5625 0.0513 0.033 Uiso 1 1 calc R . . H4B H 0.9231 0.5399 0.0106 0.033 Uiso 1 1 calc R . . C5 C 0.9384(2) 0.50352(10) 0.08159(11) 0.0294(6) Uani 1 1 d . . . H5A H 1.0003 0.4801 0.0750 0.035 Uiso 1 1 calc R . . H5B H 0.8633 0.4866 0.0725 0.035 Uiso 1 1 calc R . . C6 C 0.9526(2) 0.51727(9) 0.13916(10) 0.0253(5) Uani 1 1 d . . . H6A H 0.9394 0.4875 0.1600 0.030 Uiso 1 1 calc R . . H6B H 1.0324 0.5291 0.1498 0.030 Uiso 1 1 calc R . . C7 C 0.8667(2) 0.55794(9) 0.14924(11) 0.0256(5) Uani 1 1 d . . . H7A H 0.7868 0.5456 0.1405 0.031 Uiso 1 1 calc R . . H7B H 0.8778 0.5673 0.1863 0.031 Uiso 1 1 calc R . . C8 C 0.9685(2) 0.71195(10) 0.26413(10) 0.0296(6) Uani 1 1 d . . . H8A H 0.8950 0.7129 0.2795 0.036 Uiso 1 1 calc R . . H8B H 0.9717 0.7419 0.2423 0.036 Uiso 1 1 calc R . . C9 C 1.0685(3) 0.71330(12) 0.30734(11) 0.0366(6) Uani 1 1 d . . . H9A H 1.0605 0.7425 0.3298 0.044 Uiso 1 1 calc R . . H9B H 1.1422 0.7165 0.2924 0.044 Uiso 1 1 calc R . . C10 C 1.0701(3) 0.66584(12) 0.33940(11) 0.0384(7) Uani 1 1 d . . . H10A H 1.1353 0.6668 0.3676 0.046 Uiso 1 1 calc R . . H10B H 0.9974 0.6629 0.3552 0.046 Uiso 1 1 calc R . . C11 C 1.0832(3) 0.62182(11) 0.30427(11) 0.0347(6) Uani 1 1 d . . . H11A H 1.0835 0.5908 0.3247 0.042 Uiso 1 1 calc R . . H11B H 1.1582 0.6242 0.2903 0.042 Uiso 1 1 calc R . . C12 C 0.9865(3) 0.61932(10) 0.25946(10) 0.0294(6) Uani 1 1 d . . . H12A H 1.0044 0.5930 0.2351 0.035 Uiso 1 1 calc R . . H12B H 0.9136 0.6101 0.2730 0.035 Uiso 1 1 calc R . . C13 C 1.1773(2) 0.68779(8) 0.06128(9) 0.0184(4) Uani 1 1 d . . . C14 C 1.0970(2) 0.66738(9) 0.02336(9) 0.0215(5) Uani 1 1 d . . . H14 H 1.0170 0.6694 0.0268 0.026 Uiso 1 1 calc R . . C15 C 1.1329(2) 0.64386(10) -0.01977(10) 0.0269(5) Uani 1 1 d . . . H15 H 1.0776 0.6289 -0.0449 0.032 Uiso 1 1 calc R . . C16 C 1.2493(2) 0.64235(9) -0.02590(10) 0.0259(5) Uani 1 1 d . . . H16 H 1.2737 0.6274 -0.0558 0.031 Uiso 1 1 calc R . . C17 C 1.3298(2) 0.66284(9) 0.01194(10) 0.0255(5) Uani 1 1 d . . . H17 H 1.4096 0.6618 0.0079 0.031 Uiso 1 1 calc R . . C18 C 1.2949(2) 0.68485(9) 0.05562(9) 0.0225(5) Uani 1 1 d . . . H18 H 1.3508 0.6980 0.0817 0.027 Uiso 1 1 calc R . . C19 C 1.19605(19) 0.77842(9) 0.12312(9) 0.0194(4) Uani 1 1 d . . . C20 C 1.2322(2) 0.80071(9) 0.07939(10) 0.0234(5) Uani 1 1 d . . . H20 H 1.2285 0.7828 0.0478 0.028 Uiso 1 1 calc R . . C21 C 1.2740(3) 0.84941(10) 0.08221(10) 0.0304(6) Uani 1 1 d . . . H21 H 1.2973 0.8648 0.0523 0.036 Uiso 1 1 calc R . . C22 C 1.2816(2) 0.87544(10) 0.12846(11) 0.0302(6) Uani 1 1 d . . . H22 H 1.3119 0.9083 0.1303 0.036 Uiso 1 1 calc R . . C23 C 1.2451(2) 0.85381(10) 0.17192(10) 0.0251(5) Uani 1 1 d . . . H23 H 1.2495 0.8719 0.2035 0.030 Uiso 1 1 calc R . . C24 C 1.2019(2) 0.80549(9) 0.16933(9) 0.0208(5) Uani 1 1 d . . . H24 H 1.1763 0.7908 0.1991 0.025 Uiso 1 1 calc R . . C25 C 1.2224(2) 0.67957(9) 0.16904(9) 0.0196(5) Uani 1 1 d . . . C26 C 1.3113(2) 0.69931(10) 0.20380(9) 0.0226(5) Uani 1 1 d . . . H26 H 1.3277 0.7339 0.2033 0.027 Uiso 1 1 calc R . . C27 C 1.3761(2) 0.66836(10) 0.23925(10) 0.0278(5) Uani 1 1 d . . . H27 H 1.4357 0.6821 0.2632 0.033 Uiso 1 1 calc R . . C28 C 1.3543(2) 0.61788(10) 0.23972(10) 0.0264(5) Uani 1 1 d . . . H28 H 1.3985 0.5970 0.2641 0.032 Uiso 1 1 calc R . . C29 C 1.2675(2) 0.59763(10) 0.20452(10) 0.0247(5) Uani 1 1 d . . . H29 H 1.2534 0.5629 0.2044 0.030 Uiso 1 1 calc R . . C30 C 1.2018(2) 0.62821(9) 0.16966(10) 0.0220(5) Uani 1 1 d . . . H30 H 1.1421 0.6143 0.1459 0.026 Uiso 1 1 calc R . . C31 C 0.6401(2) 0.73269(9) 0.05202(10) 0.0225(5) Uani 1 1 d . . . C32 C 0.6740(2) 0.70820(10) 0.00920(10) 0.0270(5) Uani 1 1 d . . . H32 H 0.7406 0.6876 0.0135 0.032 Uiso 1 1 calc R . . C33 C 0.6122(2) 0.71341(11) -0.03971(10) 0.0293(5) Uani 1 1 d . . . H33 H 0.6353 0.6959 -0.0684 0.035 Uiso 1 1 calc R . . C34 C 0.5156(2) 0.74459(11) -0.04633(11) 0.0300(6) Uani 1 1 d . . . H34 H 0.4740 0.7491 -0.0797 0.036 Uiso 1 1 calc R . . C35 C 0.4812(2) 0.76876(10) -0.00415(11) 0.0301(6) Uani 1 1 d . . . H35 H 0.4150 0.7896 -0.0086 0.036 Uiso 1 1 calc R . . C36 C 0.5422(2) 0.76315(10) 0.04495(10) 0.0255(5) Uani 1 1 d . . . H36 H 0.5173 0.7800 0.0737 0.031 Uiso 1 1 calc R . . C37 C 0.6595(2) 0.77273(9) 0.15390(10) 0.0215(5) Uani 1 1 d . . . C38 C 0.6771(2) 0.82159(9) 0.13810(10) 0.0251(5) Uani 1 1 d . . . H38 H 0.7212 0.8277 0.1104 0.030 Uiso 1 1 calc R . . C39 C 0.6302(2) 0.86132(10) 0.16291(12) 0.0309(6) Uani 1 1 d . . . H39 H 0.6412 0.8944 0.1517 0.037 Uiso 1 1 calc R . . C40 C 0.5673(2) 0.85262(10) 0.20394(12) 0.0330(6) Uani 1 1 d . . . H40 H 0.5363 0.8798 0.2210 0.040 Uiso 1 1 calc R . . C41 C 0.5498(2) 0.80448(11) 0.22003(12) 0.0336(6) Uani 1 1 d . . . H41 H 0.5069 0.7986 0.2482 0.040 Uiso 1 1 calc R . . C42 C 0.5953(2) 0.76443(10) 0.19478(10) 0.0262(5) Uani 1 1 d . . . H42 H 0.5823 0.7314 0.2056 0.031 Uiso 1 1 calc R . . C43 C 0.6539(2) 0.66593(9) 0.13913(10) 0.0229(5) Uani 1 1 d . . . C44 C 0.5814(2) 0.63573(10) 0.10531(11) 0.0285(6) Uani 1 1 d . . . H44 H 0.5633 0.6451 0.0700 0.034 Uiso 1 1 calc R . . C45 C 0.5361(3) 0.59219(10) 0.12317(13) 0.0363(7) Uani 1 1 d . . . H45 H 0.4870 0.5720 0.1000 0.044 Uiso 1 1 calc R . . C46 C 0.5616(3) 0.57796(10) 0.17402(14) 0.0391(7) Uani 1 1 d . . . H46 H 0.5292 0.5484 0.1860 0.047 Uiso 1 1 calc R . . C47 C 0.6350(3) 0.60713(10) 0.20789(12) 0.0344(6) Uani 1 1 d . . . H47 H 0.6536 0.5972 0.2430 0.041 Uiso 1 1 calc R . . C48 C 0.6809(2) 0.65078(9) 0.19036(11) 0.0266(5) Uani 1 1 d . . . H48 H 0.7313 0.6705 0.2136 0.032 Uiso 1 1 calc R . . C49 C 0.9039(3) 0.77593(10) 0.01269(11) 0.0312(6) Uani 1 1 d . . . C50 C 0.8817(4) 0.80515(13) -0.03495(13) 0.0587(11) Uani 1 1 d . . . H50A H 0.8242 0.7881 -0.0594 0.070 Uiso 1 1 calc R . . H50B H 0.9536 0.8089 -0.0505 0.070 Uiso 1 1 calc R . . H50C H 0.8526 0.8380 -0.0269 0.070 Uiso 1 1 calc R . . C51 C 0.9388(2) 0.83134(10) 0.16741(11) 0.0268(5) Uani 1 1 d . . . C52 C 0.9409(3) 0.88175(11) 0.18812(14) 0.0410(7) Uani 1 1 d . . . H52A H 0.9186 0.8811 0.2232 0.049 Uiso 1 1 calc R . . H52B H 0.8865 0.9026 0.1659 0.049 Uiso 1 1 calc R . . H52C H 1.0190 0.8954 0.1892 0.049 Uiso 1 1 calc R . . C53 C 0.3297(2) 0.45201(9) 0.09665(9) 0.0225(5) Uani 1 1 d . . . C54 C 0.3766(2) 0.43814(10) 0.05150(10) 0.0260(5) Uani 1 1 d . . . H54 H 0.4105 0.4061 0.0502 0.031 Uiso 1 1 calc R . . C55 C 0.3757(2) 0.46905(10) 0.00872(10) 0.0271(5) Uani 1 1 d . . . H55 H 0.4093 0.4582 -0.0208 0.032 Uiso 1 1 calc R . . C56 C 0.3254(2) 0.51595(10) 0.00899(10) 0.0270(5) Uani 1 1 d . . . H56 H 0.3261 0.5376 -0.0198 0.032 Uiso 1 1 calc R . . C57 C 0.2744(2) 0.53072(10) 0.05198(11) 0.0277(5) Uani 1 1 d . . . H57 H 0.2379 0.5623 0.0524 0.033 Uiso 1 1 calc R . . C58 C 0.2768(2) 0.49913(9) 0.09464(10) 0.0232(5) Uani 1 1 d . . . H58 H 0.2411 0.5099 0.1236 0.028 Uiso 1 1 calc R . . C59 C 0.4851(2) 0.40109(9) 0.15753(9) 0.0229(5) Uani 1 1 d . . . C60 C 0.5704(2) 0.43647(10) 0.15036(12) 0.0312(6) Uani 1 1 d . . . H60 H 0.5465 0.4688 0.1389 0.037 Uiso 1 1 calc R . . C61 C 0.6886(3) 0.42630(11) 0.15926(12) 0.0341(6) Uani 1 1 d . . . H61 H 0.7429 0.4515 0.1540 0.041 Uiso 1 1 calc R . . C62 C 0.7267(2) 0.37980(12) 0.17569(11) 0.0340(6) Uani 1 1 d . . . H62 H 0.8069 0.3727 0.1823 0.041 Uiso 1 1 calc R . . C63 C 0.6459(3) 0.34376(12) 0.18235(14) 0.0442(8) Uani 1 1 d . . . H63 H 0.6705 0.3114 0.1934 0.053 Uiso 1 1 calc R . . C64 C 0.5277(2) 0.35449(11) 0.17298(12) 0.0347(6) Uani 1 1 d . . . H64 H 0.4741 0.3287 0.1774 0.042 Uiso 1 1 calc R . . C65 C 0.3108(2) 0.44612(9) 0.19912(9) 0.0230(5) Uani 1 1 d . . . C66 C 0.3890(2) 0.46701(9) 0.23847(10) 0.0250(5) Uani 1 1 d . . . H66 H 0.4692 0.4658 0.2352 0.030 Uiso 1 1 calc R . . C67 C 0.3537(3) 0.48945(9) 0.28215(10) 0.0288(6) Uani 1 1 d . . . H67 H 0.4099 0.5027 0.3081 0.035 Uiso 1 1 calc R . . C68 C 0.2381(3) 0.49269(10) 0.28816(10) 0.0307(6) Uani 1 1 d . . . H68 H 0.2141 0.5077 0.3181 0.037 Uiso 1 1 calc R . . C69 C 0.1570(3) 0.47344(11) 0.24916(11) 0.0319(6) Uani 1 1 d . . . H69 H 0.0768 0.4759 0.2522 0.038 Uiso 1 1 calc R . . C70 C 0.1933(2) 0.45087(10) 0.20622(10) 0.0277(5) Uani 1 1 d . . . H70 H 0.1366 0.4380 0.1803 0.033 Uiso 1 1 calc R . . C71 C 0.2629(2) 0.36702(9) 0.14178(9) 0.0216(5) Uani 1 1 d . . . C72 C 0.1884(2) 0.35496(10) 0.09748(10) 0.0264(5) Uani 1 1 d . . . H72 H 0.1868 0.3755 0.0677 0.032 Uiso 1 1 calc R . . C73 C 0.1158(3) 0.31347(11) 0.09554(11) 0.0331(6) Uani 1 1 d . . . H73 H 0.0669 0.3062 0.0645 0.040 Uiso 1 1 calc R . . C74 C 0.1140(2) 0.28295(11) 0.13817(11) 0.0321(6) Uani 1 1 d . . . H74 H 0.0646 0.2548 0.1367 0.039 Uiso 1 1 calc R . . C75 C 0.1863(2) 0.29429(10) 0.18331(10) 0.0282(6) Uani 1 1 d . . . H75 H 0.1864 0.2739 0.2132 0.034 Uiso 1 1 calc R . . C76 C 0.2581(2) 0.33550(10) 0.18440(10) 0.0254(5) Uani 1 1 d . . . H76 H 0.3064 0.3427 0.2156 0.031 Uiso 1 1 calc R . . C77 C 0.8093(2) 0.57536(10) 0.45867(10) 0.0265(5) Uani 1 1 d . A . C78 C 0.9113(3) 0.60319(12) 0.46764(12) 0.0368(7) Uani 1 1 d . . . H78 H 0.9227 0.6293 0.4442 0.044 Uiso 1 1 calc R A . C79 C 0.9967(3) 0.59485(12) 0.50880(12) 0.0381(7) Uani 1 1 d . A . H79 H 1.0638 0.6152 0.5131 0.046 Uiso 1 1 calc R . . C80 C 0.9840(3) 0.55714(12) 0.54332(13) 0.0410(7) Uani 1 1 d . . . H80 H 1.0419 0.5509 0.5716 0.049 Uiso 1 1 calc R A . C81 C 0.8849(3) 0.52864(13) 0.53584(16) 0.0530(9) Uani 1 1 d . A . H81 H 0.8741 0.5026 0.5595 0.064 Uiso 1 1 calc R . . C82 C 0.8003(3) 0.53748(11) 0.49408(13) 0.0368(7) Uani 1 1 d . . . H82 H 0.7340 0.5167 0.4897 0.044 Uiso 1 1 calc R A . C83 C 0.7139(2) 0.64414(11) 0.39296(10) 0.0302(6) Uani 1 1 d . A . C84 C 0.7159(3) 0.66514(12) 0.34398(11) 0.0351(6) Uani 1 1 d . . . H84 H 0.7276 0.6440 0.3159 0.042 Uiso 1 1 calc R A . C85 C 0.7015(3) 0.71555(13) 0.33481(12) 0.0426(7) Uani 1 1 d . A . H85 H 0.7026 0.7281 0.3007 0.051 Uiso 1 1 calc R . . C86 C 0.6855(3) 0.74802(13) 0.37474(13) 0.0417(7) Uani 1 1 d . . . H86 H 0.6767 0.7827 0.3685 0.050 Uiso 1 1 calc R A . C87 C 0.6828(3) 0.72880(13) 0.42397(12) 0.0404(7) Uani 1 1 d . A . H87 H 0.6719 0.7503 0.4519 0.048 Uiso 1 1 calc R . . C88 C 0.6959(3) 0.67834(12) 0.43238(11) 0.0355(6) Uani 1 1 d . . . H88 H 0.6926 0.6660 0.4664 0.043 Uiso 1 1 calc R A . C89 C 0.7745(3) 0.54691(13) 0.35754(11) 0.0326(14) Uiso 0.545(9) 1 d PGU A 1 C90 C 0.8876(2) 0.52967(17) 0.36235(11) 0.0248(12) Uiso 0.545(9) 1 d PGU A 1 H90 H 0.9400 0.5384 0.3919 0.030 Uiso 0.545(9) 1 calc PR A 1 C91 C 0.9241(2) 0.49972(16) 0.32396(12) 0.0263(12) Uiso 0.545(9) 1 d PGU A 1 H91 H 1.0014 0.4879 0.3273 0.032 Uiso 0.545(9) 1 calc PR A 1 C92 C 0.8474(3) 0.48701(11) 0.28077(11) 0.0214(11) Uiso 0.545(9) 1 d PGU A 1 H92 H 0.8724 0.4665 0.2545 0.026 Uiso 0.545(9) 1 calc PR A 1 C93 C 0.7343(3) 0.50424(14) 0.27596(12) 0.0273(12) Uiso 0.545(9) 1 d PGU A 1 H93 H 0.6819 0.4956 0.2464 0.033 Uiso 0.545(9) 1 calc PR A 1 C94 C 0.6978(3) 0.53419(14) 0.31434(14) 0.0263(12) Uiso 0.545(9) 1 d PGU A 1 H94 H 0.6205 0.5460 0.3111 0.032 Uiso 0.545(9) 1 calc PR A 1 C95 C 0.7502(3) 0.55224(13) 0.35999(12) 0.0124(12) Uiso 0.455(9) 1 d PGU A 2 C96 C 0.8669(3) 0.54970(18) 0.35418(15) 0.0257(14) Uiso 0.455(9) 1 d PGU A 2 H96 H 0.9213 0.5691 0.3758 0.031 Uiso 0.455(9) 1 calc PR A 2 C97 C 0.9042(3) 0.51878(19) 0.31676(17) 0.0300(15) Uiso 0.455(9) 1 d PGU A 2 H97 H 0.9839 0.5170 0.3128 0.036 Uiso 0.455(9) 1 calc PR A 2 C98 C 0.8247(4) 0.49039(15) 0.28516(15) 0.0348(18) Uiso 0.455(9) 1 d PGU A 2 H98 H 0.8501 0.4693 0.2596 0.042 Uiso 0.455(9) 1 calc PR A 2 C99 C 0.7079(3) 0.49293(15) 0.29097(17) 0.0250(14) Uiso 0.455(9) 1 d PGU A 2 H99 H 0.6536 0.4735 0.2694 0.030 Uiso 0.455(9) 1 calc PR A 2 C100 C 0.6707(3) 0.52385(15) 0.32839(17) 0.0260(14) Uiso 0.455(9) 1 d PGU A 2 H100 H 0.5910 0.5256 0.3324 0.031 Uiso 0.455(9) 1 calc PR A 2 C101 C 0.5698(2) 0.58366(14) 0.41577(12) 0.0257(11) Uiso 0.495(3) 1 d PGU A 1 C102 C 0.5338(2) 0.56988(14) 0.46271(10) 0.0294(12) Uiso 0.495(3) 1 d PG A 1 H102 H 0.5892 0.5626 0.4916 0.035 Uiso 0.495(3) 1 calc PR A 1 C103 C 0.4166(3) 0.56673(15) 0.46738(10) 0.0334(13) Uiso 0.495(3) 1 d PG A 1 H103 H 0.3919 0.5573 0.4995 0.040 Uiso 0.495(3) 1 calc PR A 1 C104 C 0.3354(2) 0.57735(15) 0.42509(13) 0.0339(13) Uiso 0.495(3) 1 d PGU A 1 H104 H 0.2553 0.5752 0.4283 0.041 Uiso 0.495(3) 1 calc PR A 1 C105 C 0.3715(2) 0.59112(15) 0.37814(11) 0.0330(13) Uiso 0.495(3) 1 d PG A 1 H105 H 0.3160 0.5984 0.3492 0.040 Uiso 0.495(3) 1 calc PR A 1 C106 C 0.4887(3) 0.59428(14) 0.37348(10) 0.0282(11) Uiso 0.495(3) 1 d PGU A 1 H106 H 0.5133 0.6037 0.3414 0.034 Uiso 0.495(3) 1 calc PR A 1 N5 N 0.6657(6) 0.3889(3) 0.4403(3) 0.0565(16) Uiso 0.495(3) 1 d P A 1 C113 C 0.5853(6) 0.4122(2) 0.4440(2) 0.0377(14) Uiso 0.495(3) 1 d P A 1 C114 C 0.4817(7) 0.4417(3) 0.4490(3) 0.0511(17) Uiso 0.495(3) 1 d P A 1 H11C H 0.4685 0.4652 0.4201 0.061 Uiso 0.495(3) 1 calc PR A 1 H11D H 0.4924 0.4601 0.4818 0.061 Uiso 0.495(3) 1 calc PR A 1 H11E H 0.4148 0.4196 0.4486 0.061 Uiso 0.495(3) 1 calc PR A 1 C107 C 0.5896(2) 0.55571(11) 0.40926(14) 0.0257(11) Uiso 0.505(3) 1 d PGU A 2 C108 C 0.4922(3) 0.58578(9) 0.40663(15) 0.0299(12) Uiso 0.505(3) 1 d PGU A 2 H108 H 0.4994 0.6207 0.4030 0.036 Uiso 0.505(3) 1 calc PR A 2 C109 C 0.3843(2) 0.56470(12) 0.40931(16) 0.0386(14) Uiso 0.505(3) 1 d PGU A 2 H109 H 0.3177 0.5853 0.4075 0.046 Uiso 0.505(3) 1 calc PR A 2 C110 C 0.3739(2) 0.51356(12) 0.41461(16) 0.0392(14) Uiso 0.505(3) 1 d PG A 2 H110 H 0.3001 0.4992 0.4164 0.047 Uiso 0.505(3) 1 calc PR A 2 C111 C 0.4713(3) 0.48349(9) 0.41725(16) 0.0348(13) Uiso 0.505(3) 1 d PG A 2 H111 H 0.4642 0.4485 0.4209 0.042 Uiso 0.505(3) 1 calc PR A 2 C112 C 0.5792(2) 0.50456(11) 0.41457(15) 0.0304(12) Uiso 0.505(3) 1 d PG A 2 H112 H 0.6458 0.4840 0.4164 0.037 Uiso 0.505(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01607(8) 0.01416(8) 0.01667(8) 0.00032(7) 0.00241(5) -0.00023(7) P1 0.0169(3) 0.0154(2) 0.0160(2) 0.0007(2) 0.00228(19) -0.0006(2) P2 0.0168(3) 0.0161(3) 0.0227(3) -0.0019(2) 0.0030(2) -0.0004(2) B1 0.0280(15) 0.0194(13) 0.0184(13) -0.0035(10) -0.0017(11) 0.0039(10) B2 0.0304(16) 0.0460(19) 0.0204(14) -0.0003(13) 0.0014(12) -0.0121(13) N1 0.0224(10) 0.0142(9) 0.0257(10) 0.0003(8) 0.0064(8) 0.0015(7) N2 0.0310(11) 0.0239(11) 0.0184(10) 0.0028(8) 0.0074(8) 0.0059(8) N3 0.0229(11) 0.0201(10) 0.0212(10) 0.0016(8) 0.0019(8) 0.0016(8) N4 0.0188(10) 0.0187(11) 0.0250(10) -0.0029(8) 0.0014(8) -0.0007(7) C1 0.0146(11) 0.0213(11) 0.0220(12) -0.0003(9) 0.0049(9) 0.0029(9) C2 0.0168(11) 0.0223(12) 0.0238(12) 0.0012(9) 0.0058(9) 0.0007(9) C3 0.0231(12) 0.0192(11) 0.0238(12) -0.0025(9) -0.0006(9) -0.0021(9) C4 0.0311(14) 0.0235(13) 0.0281(13) -0.0055(10) 0.0065(11) 0.0009(10) C5 0.0315(14) 0.0216(13) 0.0350(15) -0.0044(10) 0.0041(11) 0.0036(10) C6 0.0245(13) 0.0180(12) 0.0337(14) 0.0013(10) 0.0051(10) 0.0009(9) C7 0.0291(13) 0.0162(11) 0.0336(14) 0.0032(10) 0.0124(11) 0.0009(9) C8 0.0399(15) 0.0279(14) 0.0218(12) -0.0009(10) 0.0064(11) 0.0080(11) C9 0.0434(16) 0.0397(16) 0.0264(13) -0.0047(12) 0.0026(12) 0.0011(13) C10 0.0426(17) 0.0472(18) 0.0248(14) 0.0042(12) 0.0012(12) 0.0106(13) C11 0.0372(16) 0.0416(16) 0.0264(14) 0.0115(12) 0.0084(12) 0.0142(12) C12 0.0397(15) 0.0270(13) 0.0225(12) 0.0065(10) 0.0075(11) 0.0093(11) C13 0.0223(12) 0.0134(10) 0.0195(11) 0.0039(8) 0.0022(9) 0.0001(8) C14 0.0226(12) 0.0180(11) 0.0241(12) -0.0013(9) 0.0036(10) -0.0007(9) C15 0.0320(14) 0.0243(12) 0.0232(12) -0.0035(10) -0.0017(10) 0.0003(10) C16 0.0353(14) 0.0220(12) 0.0210(12) -0.0024(9) 0.0062(10) 0.0053(10) C17 0.0255(13) 0.0243(12) 0.0276(13) 0.0016(10) 0.0074(10) 0.0046(10) C18 0.0243(12) 0.0233(12) 0.0197(11) 0.0004(9) 0.0024(9) 0.0009(9) C19 0.0168(10) 0.0217(11) 0.0193(10) 0.0003(9) 0.0012(8) 0.0006(9) C20 0.0300(13) 0.0206(11) 0.0194(11) 0.0009(9) 0.0030(10) -0.0023(10) C21 0.0436(16) 0.0243(13) 0.0247(13) 0.0025(10) 0.0104(11) -0.0102(11) C22 0.0377(15) 0.0227(13) 0.0304(14) -0.0016(10) 0.0047(11) -0.0099(11) C23 0.0267(13) 0.0261(13) 0.0221(12) -0.0038(10) 0.0010(10) -0.0043(10) C24 0.0217(12) 0.0226(12) 0.0179(11) 0.0010(9) 0.0017(9) -0.0025(9) C25 0.0206(12) 0.0228(12) 0.0158(11) 0.0012(9) 0.0037(9) 0.0010(9) C26 0.0204(12) 0.0249(12) 0.0224(12) 0.0026(9) 0.0027(9) 0.0003(9) C27 0.0218(13) 0.0346(14) 0.0262(13) 0.0052(10) 0.0002(10) 0.0007(10) C28 0.0194(12) 0.0336(14) 0.0263(13) 0.0110(10) 0.0036(10) 0.0079(10) C29 0.0277(13) 0.0218(12) 0.0258(12) 0.0033(10) 0.0085(10) 0.0048(9) C30 0.0220(12) 0.0228(12) 0.0215(12) 0.0006(9) 0.0043(9) 0.0019(9) C31 0.0193(12) 0.0198(11) 0.0281(12) -0.0009(9) 0.0012(9) -0.0017(9) C32 0.0224(12) 0.0294(14) 0.0283(13) -0.0043(10) -0.0003(10) 0.0037(10) C33 0.0281(13) 0.0328(14) 0.0266(12) -0.0037(11) 0.0016(10) 0.0010(11) C34 0.0253(14) 0.0356(15) 0.0275(13) 0.0055(11) -0.0030(11) 0.0003(11) C35 0.0221(13) 0.0298(14) 0.0374(15) 0.0036(11) -0.0009(11) 0.0046(10) C36 0.0199(12) 0.0267(12) 0.0296(13) -0.0016(10) 0.0021(10) 0.0011(9) C37 0.0189(11) 0.0184(12) 0.0265(12) -0.0041(9) 0.0005(9) 0.0020(8) C38 0.0218(12) 0.0220(12) 0.0310(13) -0.0031(10) 0.0014(10) 0.0008(9) C39 0.0269(14) 0.0203(12) 0.0442(16) -0.0042(11) -0.0005(12) 0.0033(10) C40 0.0260(14) 0.0265(14) 0.0464(17) -0.0157(12) 0.0046(12) 0.0041(10) C41 0.0290(14) 0.0313(14) 0.0425(16) -0.0088(12) 0.0130(12) 0.0017(11) C42 0.0237(13) 0.0250(12) 0.0310(13) -0.0048(10) 0.0078(10) -0.0008(10) C43 0.0176(11) 0.0182(11) 0.0342(14) -0.0059(10) 0.0090(10) -0.0002(9) C44 0.0189(12) 0.0259(13) 0.0406(15) -0.0053(11) 0.0031(11) -0.0014(10) C45 0.0284(14) 0.0235(13) 0.0591(19) -0.0139(13) 0.0141(13) -0.0071(11) C46 0.0426(17) 0.0207(13) 0.061(2) -0.0074(13) 0.0330(15) -0.0076(11) C47 0.0457(17) 0.0199(13) 0.0427(16) -0.0024(11) 0.0266(14) -0.0030(11) C48 0.0271(13) 0.0217(12) 0.0333(14) -0.0016(10) 0.0131(11) -0.0034(10) C49 0.0428(16) 0.0213(13) 0.0292(14) 0.0014(11) 0.0033(11) -0.0020(11) C50 0.107(3) 0.0329(17) 0.0329(17) 0.0113(14) -0.0060(19) -0.0093(19) C51 0.0220(13) 0.0254(14) 0.0321(14) -0.0046(11) 0.0001(10) -0.0020(10) C52 0.0410(17) 0.0259(15) 0.055(2) -0.0185(13) 0.0024(14) -0.0031(12) C53 0.0230(12) 0.0221(12) 0.0217(12) -0.0034(9) 0.0002(9) -0.0003(9) C54 0.0290(13) 0.0237(12) 0.0251(13) -0.0022(10) 0.0028(10) 0.0001(10) C55 0.0288(14) 0.0298(14) 0.0230(12) -0.0030(10) 0.0049(10) -0.0065(10) C56 0.0245(13) 0.0281(13) 0.0270(13) 0.0059(10) -0.0022(10) -0.0078(10) C57 0.0243(13) 0.0251(13) 0.0330(14) 0.0039(10) -0.0001(11) -0.0020(10) C58 0.0220(12) 0.0237(12) 0.0236(12) -0.0003(9) 0.0020(9) 0.0012(9) C59 0.0271(13) 0.0243(12) 0.0170(11) -0.0041(9) 0.0024(9) 0.0007(10) C60 0.0303(14) 0.0201(12) 0.0414(16) -0.0061(11) -0.0028(12) -0.0022(10) C61 0.0313(15) 0.0313(15) 0.0388(16) -0.0104(12) 0.0008(12) -0.0084(11) C62 0.0231(14) 0.0449(17) 0.0335(15) -0.0039(12) 0.0016(11) 0.0026(11) C63 0.0308(16) 0.0386(17) 0.064(2) 0.0204(15) 0.0071(14) 0.0089(13) C64 0.0266(14) 0.0311(15) 0.0472(17) 0.0132(12) 0.0076(12) 0.0030(11) C65 0.0307(13) 0.0182(11) 0.0192(11) 0.0029(9) -0.0006(10) 0.0069(9) C66 0.0325(14) 0.0189(12) 0.0223(12) -0.0007(9) -0.0021(10) 0.0060(10) C67 0.0429(16) 0.0205(12) 0.0208(12) -0.0003(10) -0.0056(11) 0.0079(11) C68 0.0483(17) 0.0240(13) 0.0195(12) -0.0014(10) 0.0025(11) 0.0111(11) C69 0.0347(15) 0.0331(15) 0.0278(14) -0.0013(11) 0.0036(11) 0.0125(11) C70 0.0308(14) 0.0271(13) 0.0244(13) -0.0038(10) -0.0003(11) 0.0052(10) C71 0.0223(12) 0.0216(12) 0.0209(12) -0.0040(9) 0.0028(9) 0.0051(9) C72 0.0304(14) 0.0248(13) 0.0224(12) -0.0017(10) -0.0032(10) 0.0048(10) C73 0.0322(15) 0.0304(14) 0.0328(14) -0.0037(11) -0.0113(12) -0.0005(11) C74 0.0246(12) 0.0324(14) 0.0386(14) -0.0001(13) 0.0009(11) -0.0044(11) C75 0.0262(13) 0.0336(15) 0.0259(13) 0.0036(10) 0.0069(10) -0.0026(10) C76 0.0238(13) 0.0315(14) 0.0208(12) -0.0018(10) 0.0017(10) -0.0028(10) C77 0.0278(13) 0.0315(14) 0.0208(12) -0.0071(10) 0.0058(10) 0.0001(10) C78 0.0348(16) 0.0425(17) 0.0319(15) 0.0032(12) -0.0004(12) -0.0105(12) C79 0.0347(16) 0.0365(16) 0.0415(17) -0.0090(13) -0.0013(13) -0.0019(12) C80 0.0399(17) 0.0329(16) 0.0462(18) -0.0018(13) -0.0102(14) 0.0121(12) C81 0.045(2) 0.0419(19) 0.068(2) 0.0264(17) -0.0111(17) -0.0006(15) C82 0.0307(15) 0.0262(14) 0.0517(18) 0.0032(12) -0.0026(13) 0.0002(11) C83 0.0218(13) 0.0444(16) 0.0242(13) -0.0017(11) 0.0021(10) 0.0026(11) C84 0.0353(16) 0.0465(17) 0.0243(13) -0.0022(12) 0.0069(11) 0.0097(12) C85 0.0464(18) 0.0501(18) 0.0331(15) 0.0060(14) 0.0126(13) 0.0203(15) C86 0.0347(16) 0.0453(18) 0.0448(17) -0.0019(13) 0.0034(13) 0.0180(13) C87 0.0330(15) 0.055(2) 0.0317(15) -0.0113(13) -0.0004(12) 0.0148(13) C88 0.0303(15) 0.0508(18) 0.0248(14) -0.0043(12) 0.0008(11) 0.0040(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C2 1.922(2) . ? Ru C1 1.959(2) . ? Ru N4 2.1204(19) . ? Ru N3 2.159(2) . ? Ru P1 2.4059(6) . ? Ru P2 2.4291(6) . ? P1 C19 1.826(2) . ? P1 C25 1.836(2) . ? P1 C13 1.839(2) . ? P2 C43 1.827(3) . ? P2 C37 1.835(2) . ? P2 C31 1.841(3) . ? B1 C53 1.641(4) . ? B1 C71 1.645(4) . ? B1 C59 1.650(4) . ? B1 C65 1.650(4) . ? B2 C95 1.568(4) . ? B2 C83 1.641(5) . ? B2 C77 1.651(4) . ? B2 C107 1.685(4) . ? B2 C101 1.765(4) . ? B2 C89 1.811(4) . ? N1 C1 1.299(3) . ? N1 C3 1.478(3) . ? N1 C7 1.480(3) . ? N2 C2 1.309(3) . ? N2 C8 1.479(3) . ? N2 C12 1.485(3) . ? N3 C49 1.118(4) . ? N4 C51 1.136(3) . ? C1 C2 1.427(3) . ? C3 C4 1.528(3) . ? C4 C5 1.531(4) . ? C5 C6 1.532(4) . ? C6 C7 1.528(3) . ? C8 C9 1.518(4) . ? C9 C10 1.524(4) . ? C10 C11 1.515(4) . ? C11 C12 1.521(4) . ? C13 C14 1.388(3) . ? C13 C18 1.400(4) . ? C14 C15 1.397(4) . ? C15 C16 1.387(4) . ? C16 C17 1.389(4) . ? C17 C18 1.386(4) . ? C19 C20 1.396(3) . ? C19 C24 1.400(3) . ? C20 C21 1.397(4) . ? C21 C22 1.385(4) . ? C22 C23 1.384(4) . ? C23 C24 1.393(4) . ? C25 C26 1.394(4) . ? C25 C30 1.403(3) . ? C26 C27 1.394(4) . ? C27 C28 1.382(4) . ? C28 C29 1.390(4) . ? C29 C30 1.384(4) . ? C31 C32 1.393(4) . ? C31 C36 1.400(4) . ? C32 C33 1.391(4) . ? C33 C34 1.398(4) . ? C34 C35 1.377(4) . ? C35 C36 1.392(4) . ? C37 C42 1.392(4) . ? C37 C38 1.400(4) . ? C38 C39 1.395(4) . ? C39 C40 1.387(4) . ? C40 C41 1.384(4) . ? C41 C42 1.400(4) . ? C43 C48 1.392(4) . ? C43 C44 1.402(4) . ? C44 C45 1.388(4) . ? C45 C46 1.374(5) . ? C46 C47 1.393(5) . ? C47 C48 1.391(4) . ? C49 C50 1.464(4) . ? C51 C52 1.458(4) . ? C53 C54 1.406(4) . ? C53 C58 1.408(4) . ? C54 C55 1.388(4) . ? C55 C56 1.392(4) . ? C56 C57 1.388(4) . ? C57 C58 1.396(4) . ? C59 C64 1.390(4) . ? C59 C60 1.406(4) . ? C60 C61 1.397(4) . ? C61 C62 1.378(4) . ? C62 C63 1.378(5) . ? C63 C64 1.400(4) . ? C65 C66 1.402(4) . ? C65 C70 1.412(4) . ? C66 C67 1.393(4) . ? C67 C68 1.380(4) . ? C68 C69 1.399(4) . ? C69 C70 1.383(4) . ? C71 C72 1.394(4) . ? C71 C76 1.402(4) . ? C72 C73 1.398(4) . ? C73 C74 1.382(4) . ? C74 C75 1.393(4) . ? C75 C76 1.388(4) . ? C77 C82 1.386(4) . ? C77 C78 1.401(4) . ? C78 C79 1.388(4) . ? C79 C80 1.375(5) . ? C80 C81 1.382(5) . ? C81 C82 1.395(5) . ? C83 C84 1.396(4) . ? C83 C88 1.413(4) . ? C84 C85 1.384(5) . ? C85 C86 1.387(5) . ? C86 C87 1.385(5) . ? C87 C88 1.381(5) . ? C89 C90 1.3900 . ? C89 C94 1.3900 . ? C90 C91 1.3900 . ? C91 C92 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C95 C96 1.3900 . ? C95 C100 1.3900 . ? C96 C97 1.3900 . ? C97 C98 1.3900 . ? C98 C99 1.3900 . ? C99 C100 1.3900 . ? C101 C102 1.3900 . ? C101 C106 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C105 C106 1.3900 . ? N5 C113 1.141(9) . ? C113 C114 1.466(10) . ? C107 C108 1.3900 . ? C107 C112 1.3900 . ? C108 C109 1.3900 . ? C109 C110 1.3900 . ? C110 C111 1.3900 . ? C111 C112 1.3900 . ? 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 C2 Ru C1 43.13(10) . . ? C2 Ru N4 109.93(9) . . ? C1 Ru N4 152.63(9) . . ? C2 Ru N3 166.05(9) . . ? C1 Ru N3 123.56(9) . . ? N4 Ru N3 83.66(8) . . ? C2 Ru P1 91.10(7) . . ? C1 Ru P1 93.63(7) . . ? N4 Ru P1 91.34(6) . . ? N3 Ru P1 85.31(6) . . ? C2 Ru P2 95.25(7) . . ? C1 Ru P2 89.33(7) . . ? N4 Ru P2 88.82(6) . . ? N3 Ru P2 87.93(6) . . ? P1 Ru P2 173.18(2) . . ? C19 P1 C25 105.58(11) . . ? C19 P1 C13 105.34(10) . . ? C25 P1 C13 99.10(11) . . ? C19 P1 Ru 112.42(8) . . ? C25 P1 Ru 117.70(8) . . ? C13 P1 Ru 115.14(8) . . ? C43 P2 C37 104.68(11) . . ? C43 P2 C31 103.49(12) . . ? C37 P2 C31 101.38(11) . . ? C43 P2 Ru 112.41(8) . . ? C37 P2 Ru 116.12(8) . . ? C31 P2 Ru 117.10(8) . . ? C53 B1 C71 112.2(2) . . ? C53 B1 C59 106.7(2) . . ? C71 B1 C59 112.0(2) . . ? C53 B1 C65 110.6(2) . . ? C71 B1 C65 105.3(2) . . ? C59 B1 C65 110.0(2) . . ? C95 B2 C83 112.5(2) . . ? C95 B2 C77 110.7(3) . . ? C83 B2 C77 108.3(2) . . ? C95 B2 C107 94.9(2) . . ? C83 B2 C107 117.6(3) . . ? C77 B2 C107 112.4(2) . . ? C95 B2 C101 116.0(3) . . ? C83 B2 C101 92.6(2) . . ? C77 B2 C101 115.3(2) . . ? C107 B2 C101 27.06(16) . . ? C95 B2 C89 7.61(18) . . ? C83 B2 C89 113.6(2) . . ? C77 B2 C89 103.6(2) . . ? C107 B2 C89 100.5(2) . . ? C101 B2 C89 122.8(2) . . ? C1 N1 C3 121.6(2) . . ? C1 N1 C7 126.6(2) . . ? C3 N1 C7 111.80(19) . . ? C2 N2 C8 118.4(2) . . ? C2 N2 C12 125.6(2) . . ? C8 N2 C12 115.4(2) . . ? C49 N3 Ru 171.2(2) . . ? C51 N4 Ru 177.9(2) . . ? N1 C1 C2 139.7(2) . . ? N1 C1 Ru 151.4(2) . . ? C2 C1 Ru 67.05(13) . . ? N2 C2 C1 144.3(2) . . ? N2 C2 Ru 145.7(2) . . ? C1 C2 Ru 69.82(14) . . ? N1 C3 C4 109.4(2) . . ? C3 C4 C5 112.0(2) . . ? C4 C5 C6 111.5(2) . . ? C7 C6 C5 110.3(2) . . ? N1 C7 C6 109.1(2) . . ? N2 C8 C9 112.7(2) . . ? C8 C9 C10 110.0(3) . . ? C11 C10 C9 108.7(2) . . ? C10 C11 C12 112.1(2) . . ? N2 C12 C11 112.4(2) . . ? C14 C13 C18 119.2(2) . . ? C14 C13 P1 121.36(19) . . ? C18 C13 P1 119.43(18) . . ? C13 C14 C15 120.5(2) . . ? C16 C15 C14 120.0(2) . . ? C15 C16 C17 119.6(2) . . ? C18 C17 C16 120.6(2) . . ? C17 C18 C13 120.1(2) . . ? C20 C19 C24 119.2(2) . . ? C20 C19 P1 121.20(18) . . ? C24 C19 P1 119.45(18) . . ? C19 C20 C21 119.9(2) . . ? C22 C21 C20 120.3(2) . . ? C23 C22 C21 120.2(2) . . ? C22 C23 C24 119.9(2) . . ? C23 C24 C19 120.4(2) . . ? C26 C25 C30 118.8(2) . . ? C26 C25 P1 124.11(19) . . ? C30 C25 P1 116.99(19) . . ? C27 C26 C25 120.1(2) . . ? C28 C27 C26 120.5(3) . . ? C27 C28 C29 120.0(2) . . ? C30 C29 C28 119.9(2) . . ? C29 C30 C25 120.7(2) . . ? C32 C31 C36 118.6(2) . . ? C32 C31 P2 120.54(19) . . ? C36 C31 P2 120.8(2) . . ? C33 C32 C31 121.2(2) . . ? C32 C33 C34 119.5(3) . . ? C35 C34 C33 119.6(3) . . ? C34 C35 C36 121.0(2) . . ? C35 C36 C31 120.0(2) . . ? C42 C37 C38 119.1(2) . . ? C42 C37 P2 123.58(19) . . ? C38 C37 P2 117.22(19) . . ? C39 C38 C37 120.2(3) . . ? C40 C39 C38 120.1(3) . . ? C41 C40 C39 120.2(2) . . ? C40 C41 C42 120.0(3) . . ? C37 C42 C41 120.4(3) . . ? C48 C43 C44 118.6(2) . . ? C48 C43 P2 119.47(19) . . ? C44 C43 P2 121.8(2) . . ? C45 C44 C43 120.3(3) . . ? C46 C45 C44 120.7(3) . . ? C45 C46 C47 119.7(3) . . ? C48 C47 C46 120.0(3) . . ? C47 C48 C43 120.6(3) . . ? N3 C49 C50 177.6(3) . . ? N4 C51 C52 179.4(3) . . ? C54 C53 C58 115.0(2) . . ? C54 C53 B1 120.3(2) . . ? C58 C53 B1 124.6(2) . . ? C55 C54 C53 123.0(2) . . ? C54 C55 C56 120.1(2) . . ? C57 C56 C55 119.1(2) . . ? C56 C57 C58 119.9(2) . . ? C57 C58 C53 122.9(2) . . ? C64 C59 C60 114.6(2) . . ? C64 C59 B1 125.0(2) . . ? C60 C59 B1 120.4(2) . . ? C61 C60 C59 123.1(3) . . ? C62 C61 C60 120.2(3) . . ? C61 C62 C63 118.6(3) . . ? C62 C63 C64 120.5(3) . . ? C59 C64 C63 123.1(3) . . ? C66 C65 C70 115.0(2) . . ? C66 C65 B1 125.1(2) . . ? C70 C65 B1 119.9(2) . . ? C67 C66 C65 122.6(3) . . ? C68 C67 C66 120.7(3) . . ? C67 C68 C69 118.6(3) . . ? C70 C69 C68 120.1(3) . . ? C69 C70 C65 123.0(3) . . ? C72 C71 C76 115.5(2) . . ? C72 C71 B1 125.0(2) . . ? C76 C71 B1 119.3(2) . . ? C71 C72 C73 122.0(2) . . ? C74 C73 C72 120.9(3) . . ? C73 C74 C75 118.7(3) . . ? C76 C75 C74 119.6(3) . . ? C75 C76 C71 123.4(2) . . ? C82 C77 C78 114.5(3) . . ? C82 C77 B2 124.3(3) . . ? C78 C77 B2 120.9(3) . . ? C79 C78 C77 123.8(3) . . ? C80 C79 C78 119.9(3) . . ? C79 C80 C81 118.2(3) . . ? C80 C81 C82 121.0(3) . . ? C77 C82 C81 122.6(3) . . ? C84 C83 C88 114.8(3) . . ? C84 C83 B2 125.7(3) . . ? C88 C83 B2 119.1(3) . . ? C85 C84 C83 122.6(3) . . ? C84 C85 C86 120.8(3) . . ? C87 C86 C85 118.5(3) . . ? C88 C87 C86 119.9(3) . . ? C87 C88 C83 123.3(3) . . ? C90 C89 C94 120.0 . . ? C90 C89 B2 123.5(2) . . ? C94 C89 B2 116.4(2) . . ? C89 C90 C91 120.0 . . ? C92 C91 C90 120.0 . . ? C91 C92 C93 120.0 . . ? C92 C93 C94 120.0 . . ? C93 C94 C89 120.0 . . ? C96 C95 C100 120.0 . . ? C96 C95 B2 116.7(2) . . ? C100 C95 B2 123.1(2) . . ? C97 C96 C95 120.0 . . ? C96 C97 C98 120.0 . . ? C97 C98 C99 120.0 . . ? C100 C99 C98 120.0 . . ? C99 C100 C95 120.0 . . ? C102 C101 C106 120.0 . . ? C102 C101 B2 122.2(2) . . ? C106 C101 B2 117.7(2) . . ? C101 C102 C103 120.0 . . ? C102 C103 C104 120.0 . . ? C105 C104 C103 120.0 . . ? C106 C105 C104 120.0 . . ? C105 C106 C101 120.0 . . ? N5 C113 C114 179.4(8) . . ? C108 C107 C112 120.0 . . ? C108 C107 B2 116.8(2) . . ? C112 C107 B2 123.2(2) . . ? C109 C108 C107 120.0 . . ? C110 C109 C108 120.0 . . ? C109 C110 C111 120.0 . . ? C112 C111 C110 120.0 . . ? C111 C112 C107 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 C2 Ru P1 C19 -125.97(11) . . . . ? C1 Ru P1 C19 -169.07(11) . . . . ? N4 Ru P1 C19 -16.00(10) . . . . ? N3 Ru P1 C19 67.53(10) . . . . ? P2 Ru P1 C19 75.3(2) . . . . ? C2 Ru P1 C25 -2.97(12) . . . . ? C1 Ru P1 C25 -46.07(11) . . . . ? N4 Ru P1 C25 107.00(11) . . . . ? N3 Ru P1 C25 -169.47(10) . . . . ? P2 Ru P1 C25 -161.74(19) . . . . ? C2 Ru P1 C13 113.38(11) . . . . ? C1 Ru P1 C13 70.28(11) . . . . ? N4 Ru P1 C13 -136.65(10) . . . . ? N3 Ru P1 C13 -53.12(10) . . . . ? P2 Ru P1 C13 -45.4(2) . . . . ? C2 Ru P2 C43 -28.59(12) . . . . ? C1 Ru P2 C43 14.19(11) . . . . ? N4 Ru P2 C43 -138.50(11) . . . . ? N3 Ru P2 C43 137.80(11) . . . . ? P1 Ru P2 C43 130.1(2) . . . . ? C2 Ru P2 C37 91.91(12) . . . . ? C1 Ru P2 C37 134.69(11) . . . . ? N4 Ru P2 C37 -18.00(11) . . . . ? N3 Ru P2 C37 -101.70(11) . . . . ? P1 Ru P2 C37 -109.4(2) . . . . ? C2 Ru P2 C31 -148.23(11) . . . . ? C1 Ru P2 C31 -105.45(11) . . . . ? N4 Ru P2 C31 101.86(10) . . . . ? N3 Ru P2 C31 18.16(10) . . . . ? P1 Ru P2 C31 10.5(2) . . . . ? C2 Ru N3 C49 159.2(13) . . . . ? C1 Ru N3 C49 143.5(14) . . . . ? N4 Ru N3 C49 -33.4(15) . . . . ? P1 Ru N3 C49 -125.3(15) . . . . ? P2 Ru N3 C49 55.6(15) . . . . ? C2 Ru N4 C51 -50(6) . . . . ? C1 Ru N4 C51 -41(6) . . . . ? N3 Ru N4 C51 133(6) . . . . ? P1 Ru N4 C51 -141(6) . . . . ? P2 Ru N4 C51 45(6) . . . . ? C3 N1 C1 C2 176.8(3) . . . . ? C7 N1 C1 C2 -2.5(5) . . . . ? C3 N1 C1 Ru 22.4(5) . . . . ? C7 N1 C1 Ru -156.8(3) . . . . ? C2 Ru C1 N1 162.3(4) . . . . ? N4 Ru C1 N1 150.0(3) . . . . ? N3 Ru C1 N1 -23.2(4) . . . . ? P1 Ru C1 N1 -110.0(4) . . . . ? P2 Ru C1 N1 63.9(4) . . . . ? N4 Ru C1 C2 -12.3(2) . . . . ? N3 Ru C1 C2 174.51(12) . . . . ? P1 Ru C1 C2 87.73(12) . . . . ? P2 Ru C1 C2 -98.41(12) . . . . ? C8 N2 C2 C1 -169.7(3) . . . . ? C12 N2 C2 C1 1.7(5) . . . . ? C8 N2 C2 Ru 18.2(5) . . . . ? C12 N2 C2 Ru -170.4(2) . . . . ? N1 C1 C2 N2 17.7(6) . . . . ? Ru C1 C2 N2 -175.3(4) . . . . ? N1 C1 C2 Ru -167.0(3) . . . . ? C1 Ru C2 N2 175.1(4) . . . . ? N4 Ru C2 N2 -10.9(4) . . . . ? N3 Ru C2 N2 155.8(3) . . . . ? P1 Ru C2 N2 81.0(3) . . . . ? P2 Ru C2 N2 -101.5(3) . . . . ? N4 Ru C2 C1 174.04(12) . . . . ? N3 Ru C2 C1 -19.3(4) . . . . ? P1 Ru C2 C1 -94.14(12) . . . . ? P2 Ru C2 C1 83.39(12) . . . . ? C1 N1 C3 C4 119.7(2) . . . . ? C7 N1 C3 C4 -61.0(3) . . . . ? N1 C3 C4 C5 53.9(3) . . . . ? C3 C4 C5 C6 -50.8(3) . . . . ? C4 C5 C6 C7 52.5(3) . . . . ? C1 N1 C7 C6 -117.1(3) . . . . ? C3 N1 C7 C6 63.6(3) . . . . ? C5 C6 C7 N1 -58.0(3) . . . . ? C2 N2 C8 C9 -139.4(2) . . . . ? C12 N2 C8 C9 48.4(3) . . . . ? N2 C8 C9 C10 -55.0(3) . . . . ? C8 C9 C10 C11 59.7(3) . . . . ? C9 C10 C11 C12 -58.3(3) . . . . ? C2 N2 C12 C11 142.7(3) . . . . ? C8 N2 C12 C11 -45.7(3) . . . . ? C10 C11 C12 N2 51.0(3) . . . . ? C19 P1 C13 C14 -126.6(2) . . . . ? C25 P1 C13 C14 124.4(2) . . . . ? Ru P1 C13 C14 -2.1(2) . . . . ? C19 P1 C13 C18 56.0(2) . . . . ? C25 P1 C13 C18 -53.0(2) . . . . ? Ru P1 C13 C18 -179.57(16) . . . . ? C18 C13 C14 C15 0.5(4) . . . . ? P1 C13 C14 C15 -176.98(19) . . . . ? C13 C14 C15 C16 -2.4(4) . . . . ? C14 C15 C16 C17 2.2(4) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? C16 C17 C18 C13 -1.7(4) . . . . ? C14 C13 C18 C17 1.6(4) . . . . ? P1 C13 C18 C17 179.05(19) . . . . ? C25 P1 C19 C20 123.5(2) . . . . ? C13 P1 C19 C20 19.2(2) . . . . ? Ru P1 C19 C20 -106.9(2) . . . . ? C25 P1 C19 C24 -60.5(2) . . . . ? C13 P1 C19 C24 -164.81(19) . . . . ? Ru P1 C19 C24 69.1(2) . . . . ? C24 C19 C20 C21 0.2(4) . . . . ? P1 C19 C20 C21 176.2(2) . . . . ? C19 C20 C21 C22 1.1(4) . . . . ? C20 C21 C22 C23 -1.6(5) . . . . ? C21 C22 C23 C24 0.8(4) . . . . ? C22 C23 C24 C19 0.6(4) . . . . ? C20 C19 C24 C23 -1.0(4) . . . . ? P1 C19 C24 C23 -177.10(19) . . . . ? C19 P1 C25 C26 6.1(2) . . . . ? C13 P1 C25 C26 115.0(2) . . . . ? Ru P1 C25 C26 -120.29(19) . . . . ? C19 P1 C25 C30 -171.33(18) . . . . ? C13 P1 C25 C30 -62.5(2) . . . . ? Ru P1 C25 C30 62.3(2) . . . . ? C30 C25 C26 C27 -1.6(4) . . . . ? P1 C25 C26 C27 -178.99(19) . . . . ? C25 C26 C27 C28 1.1(4) . . . . ? C26 C27 C28 C29 0.3(4) . . . . ? C27 C28 C29 C30 -1.1(4) . . . . ? C28 C29 C30 C25 0.6(4) . . . . ? C26 C25 C30 C29 0.7(4) . . . . ? P1 C25 C30 C29 178.34(19) . . . . ? C43 P2 C31 C32 -83.5(2) . . . . ? C37 P2 C31 C32 168.1(2) . . . . ? Ru P2 C31 C32 40.7(2) . . . . ? C43 P2 C31 C36 93.4(2) . . . . ? C37 P2 C31 C36 -14.9(2) . . . . ? Ru P2 C31 C36 -142.29(18) . . . . ? C36 C31 C32 C33 -0.3(4) . . . . ? P2 C31 C32 C33 176.7(2) . . . . ? C31 C32 C33 C34 1.4(4) . . . . ? C32 C33 C34 C35 -1.6(4) . . . . ? C33 C34 C35 C36 0.9(4) . . . . ? C34 C35 C36 C31 0.2(4) . . . . ? C32 C31 C36 C35 -0.4(4) . . . . ? P2 C31 C36 C35 -177.5(2) . . . . ? C43 P2 C37 C42 9.0(3) . . . . ? C31 P2 C37 C42 116.4(2) . . . . ? Ru P2 C37 C42 -115.6(2) . . . . ? C43 P2 C37 C38 -168.38(19) . . . . ? C31 P2 C37 C38 -61.0(2) . . . . ? Ru P2 C37 C38 67.0(2) . . . . ? C42 C37 C38 C39 -0.4(4) . . . . ? P2 C37 C38 C39 177.1(2) . . . . ? C37 C38 C39 C40 1.1(4) . . . . ? C38 C39 C40 C41 -0.8(4) . . . . ? C39 C40 C41 C42 -0.1(5) . . . . ? C38 C37 C42 C41 -0.5(4) . . . . ? P2 C37 C42 C41 -177.9(2) . . . . ? C40 C41 C42 C37 0.8(4) . . . . ? C37 P2 C43 C48 -65.1(2) . . . . ? C31 P2 C43 C48 -170.9(2) . . . . ? Ru P2 C43 C48 61.8(2) . . . . ? C37 P2 C43 C44 117.8(2) . . . . ? C31 P2 C43 C44 12.0(2) . . . . ? Ru P2 C43 C44 -115.3(2) . . . . ? C48 C43 C44 C45 1.3(4) . . . . ? P2 C43 C44 C45 178.4(2) . . . . ? C43 C44 C45 C46 -0.1(4) . . . . ? C44 C45 C46 C47 -0.9(4) . . . . ? C45 C46 C47 C48 0.8(4) . . . . ? C46 C47 C48 C43 0.3(4) . . . . ? C44 C43 C48 C47 -1.4(4) . . . . ? P2 C43 C48 C47 -178.6(2) . . . . ? Ru N3 C49 C50 -78(8) . . . . ? Ru N4 C51 C52 2(47) . . . . ? C71 B1 C53 C54 -75.6(3) . . . . ? C59 B1 C53 C54 47.5(3) . . . . ? C65 B1 C53 C54 167.2(2) . . . . ? C71 B1 C53 C58 109.4(3) . . . . ? C59 B1 C53 C58 -127.6(2) . . . . ? C65 B1 C53 C58 -7.9(3) . . . . ? C58 C53 C54 C55 2.6(4) . . . . ? B1 C53 C54 C55 -172.9(2) . . . . ? C53 C54 C55 C56 -0.8(4) . . . . ? C54 C55 C56 C57 -1.4(4) . . . . ? C55 C56 C57 C58 1.7(4) . . . . ? C56 C57 C58 C53 0.2(4) . . . . ? C54 C53 C58 C57 -2.3(4) . . . . ? B1 C53 C58 C57 173.0(2) . . . . ? C53 B1 C59 C64 -140.4(3) . . . . ? C71 B1 C59 C64 -17.2(4) . . . . ? C65 B1 C59 C64 99.6(3) . . . . ? C53 B1 C59 C60 40.1(3) . . . . ? C71 B1 C59 C60 163.3(2) . . . . ? C65 B1 C59 C60 -80.0(3) . . . . ? C64 C59 C60 C61 -1.6(4) . . . . ? B1 C59 C60 C61 178.0(3) . . . . ? C59 C60 C61 C62 0.2(5) . . . . ? C60 C61 C62 C63 0.9(5) . . . . ? C61 C62 C63 C64 -0.5(5) . . . . ? C60 C59 C64 C63 2.0(4) . . . . ? B1 C59 C64 C63 -177.6(3) . . . . ? C62 C63 C64 C59 -1.0(5) . . . . ? C53 B1 C65 C66 -102.2(3) . . . . ? C71 B1 C65 C66 136.3(2) . . . . ? C59 B1 C65 C66 15.4(3) . . . . ? C53 B1 C65 C70 79.6(3) . . . . ? C71 B1 C65 C70 -41.9(3) . . . . ? C59 B1 C65 C70 -162.8(2) . . . . ? C70 C65 C66 C67 1.9(4) . . . . ? B1 C65 C66 C67 -176.4(2) . . . . ? C65 C66 C67 C68 -0.9(4) . . . . ? C66 C67 C68 C69 -0.7(4) . . . . ? C67 C68 C69 C70 1.3(4) . . . . ? C68 C69 C70 C65 -0.2(4) . . . . ? C66 C65 C70 C69 -1.3(4) . . . . ? B1 C65 C70 C69 177.0(2) . . . . ? C53 B1 C71 C72 2.7(3) . . . . ? C59 B1 C71 C72 -117.3(3) . . . . ? C65 B1 C71 C72 123.1(3) . . . . ? C53 B1 C71 C76 -173.1(2) . . . . ? C59 B1 C71 C76 66.9(3) . . . . ? C65 B1 C71 C76 -52.7(3) . . . . ? C76 C71 C72 C73 -1.4(4) . . . . ? B1 C71 C72 C73 -177.4(2) . . . . ? C71 C72 C73 C74 0.9(4) . . . . ? C72 C73 C74 C75 0.0(4) . . . . ? C73 C74 C75 C76 -0.2(4) . . . . ? C74 C75 C76 C71 -0.4(4) . . . . ? C72 C71 C76 C75 1.2(4) . . . . ? B1 C71 C76 C75 177.4(2) . . . . ? C95 B2 C77 C82 -86.2(3) . . . . ? C83 B2 C77 C82 150.1(3) . . . . ? C107 B2 C77 C82 18.5(4) . . . . ? C101 B2 C77 C82 48.0(4) . . . . ? C89 B2 C77 C82 -89.0(3) . . . . ? C95 B2 C77 C78 86.9(3) . . . . ? C83 B2 C77 C78 -36.8(4) . . . . ? C107 B2 C77 C78 -168.3(3) . . . . ? C101 B2 C77 C78 -138.9(3) . . . . ? C89 B2 C77 C78 84.1(3) . . . . ? C82 C77 C78 C79 -1.1(5) . . . . ? B2 C77 C78 C79 -174.8(3) . . . . ? C77 C78 C79 C80 0.6(5) . . . . ? C78 C79 C80 C81 -0.4(5) . . . . ? C79 C80 C81 C82 0.7(6) . . . . ? C78 C77 C82 C81 1.4(5) . . . . ? B2 C77 C82 C81 174.9(3) . . . . ? C80 C81 C82 C77 -1.3(6) . . . . ? C95 B2 C83 C84 12.8(4) . . . . ? C77 B2 C83 C84 135.5(3) . . . . ? C107 B2 C83 C84 -95.8(4) . . . . ? C101 B2 C83 C84 -106.7(3) . . . . ? C89 B2 C83 C84 21.0(4) . . . . ? C95 B2 C83 C88 -174.1(3) . . . . ? C77 B2 C83 C88 -51.5(3) . . . . ? C107 B2 C83 C88 77.2(3) . . . . ? C101 B2 C83 C88 66.3(3) . . . . ? C89 B2 C83 C88 -165.9(2) . . . . ? C88 C83 C84 C85 0.1(4) . . . . ? B2 C83 C84 C85 173.4(3) . . . . ? C83 C84 C85 C86 0.7(5) . . . . ? C84 C85 C86 C87 -0.8(5) . . . . ? C85 C86 C87 C88 0.0(5) . . . . ? C86 C87 C88 C83 0.8(5) . . . . ? C84 C83 C88 C87 -0.9(4) . . . . ? B2 C83 C88 C87 -174.7(3) . . . . ? C95 B2 C89 C90 -178.0(17) . . . . ? C83 B2 C89 C90 99.0(3) . . . . ? C77 B2 C89 C90 -18.2(3) . . . . ? C107 B2 C89 C90 -134.5(3) . . . . ? C101 B2 C89 C90 -151.0(3) . . . . ? C95 B2 C89 C94 0.1(15) . . . . ? C83 B2 C89 C94 -82.9(3) . . . . ? C77 B2 C89 C94 159.9(2) . . . . ? C107 B2 C89 C94 43.6(3) . . . . ? C101 B2 C89 C94 27.1(4) . . . . ? C94 C89 C90 C91 0.0 . . . . ? B2 C89 C90 C91 178.0(3) . . . . ? C89 C90 C91 C92 0.0 . . . . ? C90 C91 C92 C93 0.0 . . . . ? C91 C92 C93 C94 0.0 . . . . ? C92 C93 C94 C89 0.0 . . . . ? C90 C89 C94 C93 0.0 . . . . ? B2 C89 C94 C93 -178.2(3) . . . . ? C83 B2 C95 C96 79.6(3) . . . . ? C77 B2 C95 C96 -41.7(4) . . . . ? C107 B2 C95 C96 -157.9(3) . . . . ? C101 B2 C95 C96 -175.6(3) . . . . ? C89 B2 C95 C96 -20.7(14) . . . . ? C83 B2 C95 C100 -105.7(3) . . . . ? C77 B2 C95 C100 133.1(3) . . . . ? C107 B2 C95 C100 16.9(4) . . . . ? C101 B2 C95 C100 -0.8(4) . . . . ? C89 B2 C95 C100 154.1(17) . . . . ? C100 C95 C96 C97 0.0 . . . . ? B2 C95 C96 C97 174.9(3) . . . . ? C95 C96 C97 C98 0.0 . . . . ? C96 C97 C98 C99 0.0 . . . . ? C97 C98 C99 C100 0.0 . . . . ? C98 C99 C100 C95 0.0 . . . . ? C96 C95 C100 C99 0.0 . . . . ? B2 C95 C100 C99 -174.6(4) . . . . ? C95 B2 C101 C102 123.7(3) . . . . ? C83 B2 C101 C102 -119.7(2) . . . . ? C77 B2 C101 C102 -8.1(4) . . . . ? C107 B2 C101 C102 81.9(4) . . . . ? C89 B2 C101 C102 119.8(3) . . . . ? C95 B2 C101 C106 -52.2(4) . . . . ? C83 B2 C101 C106 64.4(3) . . . . ? C77 B2 C101 C106 176.0(2) . . . . ? C107 B2 C101 C106 -94.0(4) . . . . ? C89 B2 C101 C106 -56.1(4) . . . . ? C106 C101 C102 C103 0.0 . . . . ? B2 C101 C102 C103 -175.8(3) . . . . ? C101 C102 C103 C104 0.0 . . . . ? C102 C103 C104 C105 0.0 . . . . ? C103 C104 C105 C106 0.0 . . . . ? C104 C105 C106 C101 0.0 . . . . ? C102 C101 C106 C105 0.0 . . . . ? B2 C101 C106 C105 176.0(3) . . . . ? C95 B2 C107 C108 -126.1(3) . . . . ? C83 B2 C107 C108 -7.6(3) . . . . ? C77 B2 C107 C108 119.2(3) . . . . ? C101 B2 C107 C108 17.0(3) . . . . ? C89 B2 C107 C108 -131.3(2) . . . . ? C95 B2 C107 C112 54.4(3) . . . . ? C83 B2 C107 C112 172.9(2) . . . . ? C77 B2 C107 C112 -60.4(3) . . . . ? C101 B2 C107 C112 -162.5(5) . . . . ? C89 B2 C107 C112 49.1(3) . . . . ? C112 C107 C108 C109 0.0 . . . . ? B2 C107 C108 C109 -179.6(3) . . . . ? C107 C108 C109 C110 0.0 . . . . ? C108 C109 C110 C111 0.0 . . . . ? C109 C110 C111 C112 0.0 . . . . ? C110 C111 C112 C107 0.0 . . . . ? C108 C107 C112 C111 0.0 . . . . ? B2 C107 C112 C111 179.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 72.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.504 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.066 #============================================================================= # end of cif data for "pet27" (compound 5) #============================================================================= #============================================================================= # cif data for "pet15a" (compound 6) #============================================================================= data_pet15a _database_code_depnum_ccdc_archive 'CCDC 819871' #TrackingRef 'pet-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H62 Cl4 N11 P Pd Ru' _chemical_formula_weight 1173.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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 9.5899(8) _cell_length_b 15.9641(18) _cell_length_c 17.390(2) _cell_angle_alpha 80.429(9) _cell_angle_beta 76.303(8) _cell_angle_gamma 86.480(8) _cell_volume 2550.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9714 _cell_measurement_theta_min 3.5431 _cell_measurement_theta_max 75.8906 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 7.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62510 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27607 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 70.06 _reflns_number_total 9682 _reflns_number_gt 7293 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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. Three distorted molecules of acetonitrile, which could not be refined satisfactorily, was removed using the program SQUEEZE (A.L. Spek, University of Utrecht, Netherlands). The quoted formula and derived parameters are based on a total of nine molecules of acetonitrile (two coordinated, four free, three Squeezed) per asymmetric unit. ; 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 -0.031 0.000 1.000 282.1 54.4 _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^)+(0.0930P)^2^+1.8746P] 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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9682 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1478 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Ru Ru 0.68022(4) 0.26178(3) 0.21089(2) 0.02845(12) Uani 1 1 d . . . Pd Pd 0.80992(4) 0.35570(3) 0.36456(3) 0.03748(14) Uani 1 1 d . . . Cl1 Cl 0.89336(13) 0.27181(10) 0.26600(8) 0.0360(3) Uani 1 1 d . . . Cl2 Cl 0.74967(15) 0.39191(9) 0.11972(8) 0.0375(3) Uani 1 1 d . . . Cl3 Cl 1.00587(14) 0.31431(12) 0.42551(9) 0.0457(4) Uani 1 1 d . . . Cl4 Cl 0.70624(17) 0.43626(14) 0.46328(11) 0.0563(5) Uani 1 1 d . . . P P 0.49470(14) 0.25744(9) 0.14866(8) 0.0291(3) Uani 1 1 d . . . N1 N 0.4539(5) 0.3053(4) 0.3585(3) 0.0382(11) Uani 1 1 d . . . N2 N 0.6438(5) 0.4711(3) 0.2734(3) 0.0388(11) Uani 1 1 d . . . N3 N 0.6485(5) 0.1493(3) 0.2842(3) 0.0369(11) Uani 1 1 d . . . N4 N 0.8211(5) 0.1933(3) 0.1299(3) 0.0384(11) Uani 1 1 d . . . N6 N 0.0948(10) 0.2799(6) 0.9075(6) 0.092(3) Uani 1 1 d . . . N7 N 0.9541(9) 0.9318(9) 0.3895(8) 0.140(6) Uani 1 1 d . . . N8 N 0.0774(8) 0.6757(6) 0.2815(5) 0.078(2) Uani 1 1 d . . . C1 C 0.5709(5) 0.3250(4) 0.3004(3) 0.0300(11) Uani 1 1 d . . . C2 C 0.6569(6) 0.3949(4) 0.3072(3) 0.0358(13) Uani 1 1 d . . . C3 C 0.4004(6) 0.3571(5) 0.4232(4) 0.0476(16) Uani 1 1 d . . . H3A H 0.3009 0.3773 0.4225 0.057 Uiso 1 1 calc R . . H3B H 0.4610 0.4074 0.4139 0.057 Uiso 1 1 calc R . . C4 C 0.4034(9) 0.3052(6) 0.5040(4) 0.066(2) Uani 1 1 d . . . H4A H 0.3592 0.3393 0.5466 0.079 Uiso 1 1 calc R . . H4B H 0.5044 0.2924 0.5071 0.079 Uiso 1 1 calc R . . C5 C 0.3232(8) 0.2213(6) 0.5196(4) 0.065(2) Uani 1 1 d . . . H5A H 0.2190 0.2332 0.5255 0.078 Uiso 1 1 calc R . . H5B H 0.3380 0.1865 0.5699 0.078 Uiso 1 1 calc R . . C6 C 0.3806(7) 0.1724(5) 0.4488(4) 0.0557(19) Uani 1 1 d . . . H6A H 0.4819 0.1548 0.4471 0.067 Uiso 1 1 calc R . . H6B H 0.3242 0.1205 0.4565 0.067 Uiso 1 1 calc R . . C7 C 0.3703(6) 0.2270(4) 0.3710(4) 0.0404(14) Uani 1 1 d . . . H7A H 0.4080 0.1948 0.3262 0.048 Uiso 1 1 calc R . . H7B H 0.2685 0.2425 0.3717 0.048 Uiso 1 1 calc R . . C8 C 0.5215(7) 0.5030(5) 0.2374(4) 0.0458(15) Uani 1 1 d . . . H8A H 0.4515 0.4573 0.2463 0.055 Uiso 1 1 calc R . . H8B H 0.5563 0.5204 0.1789 0.055 Uiso 1 1 calc R . . C9 C 0.4486(8) 0.5792(5) 0.2757(6) 0.061(2) Uani 1 1 d . . . H9A H 0.3699 0.6022 0.2498 0.073 Uiso 1 1 calc R . . H9B H 0.4065 0.5603 0.3333 0.073 Uiso 1 1 calc R . . C10 C 0.5558(11) 0.6483(6) 0.2666(7) 0.078(3) Uani 1 1 d . . . H10A H 0.5084 0.6949 0.2952 0.094 Uiso 1 1 calc R . . H10B H 0.5893 0.6720 0.2092 0.094 Uiso 1 1 calc R . . C11 C 0.6836(10) 0.6132(6) 0.3005(7) 0.081(3) Uani 1 1 d . . . H11A H 0.6516 0.5970 0.3593 0.097 Uiso 1 1 calc R . . H11B H 0.7556 0.6581 0.2898 0.097 Uiso 1 1 calc R . . C12 C 0.7531(8) 0.5362(4) 0.2642(5) 0.0513(17) Uani 1 1 d . . . H12A H 0.7973 0.5536 0.2066 0.062 Uiso 1 1 calc R . . H12B H 0.8297 0.5119 0.2912 0.062 Uiso 1 1 calc R . . C13 C 0.6421(7) 0.0849(5) 0.3239(4) 0.0450(15) Uani 1 1 d . . . C14 C 0.6268(10) 0.0027(5) 0.3771(6) 0.070(2) Uani 1 1 d . . . H14A H 0.6706 0.0050 0.4222 0.083 Uiso 1 1 calc R . . H14B H 0.6749 -0.0420 0.3472 0.083 Uiso 1 1 calc R . . H14C H 0.5247 -0.0099 0.3974 0.083 Uiso 1 1 calc R . . C15 C 0.8984(7) 0.1532(4) 0.0907(4) 0.0431(14) Uani 1 1 d . . . C16 C 0.9938(10) 0.1010(6) 0.0385(6) 0.074(3) Uani 1 1 d . . . H16A H 0.9502 0.0459 0.0434 0.088 Uiso 1 1 calc R . . H16B H 1.0859 0.0924 0.0542 0.088 Uiso 1 1 calc R . . H16C H 1.0095 0.1297 -0.0171 0.088 Uiso 1 1 calc R . . C17 C 0.3830(6) 0.1628(4) 0.1810(4) 0.0366(12) Uani 1 1 d . . . C18 C 0.4540(7) 0.0846(4) 0.1868(4) 0.0450(15) Uani 1 1 d . . . H18 H 0.5558 0.0827 0.1766 0.054 Uiso 1 1 calc R . . C19 C 0.3813(9) 0.0096(5) 0.2069(6) 0.067(2) Uani 1 1 d . . . H19 H 0.4320 -0.0434 0.2106 0.081 Uiso 1 1 calc R . . C20 C 0.2315(10) 0.0126(6) 0.2218(7) 0.085(3) Uani 1 1 d . . . H20 H 0.1794 -0.0385 0.2371 0.102 Uiso 1 1 calc R . . C21 C 0.1609(8) 0.0885(5) 0.2145(6) 0.070(3) Uani 1 1 d . . . H21 H 0.0591 0.0898 0.2238 0.083 Uiso 1 1 calc R . . C22 C 0.2330(6) 0.1637(4) 0.1939(4) 0.0439(15) Uani 1 1 d . . . H22 H 0.1813 0.2162 0.1883 0.053 Uiso 1 1 calc R . . C23 C 0.5461(7) 0.2520(4) 0.0401(4) 0.0368(12) Uani 1 1 d . . . C24 C 0.4441(7) 0.2248(5) 0.0043(4) 0.0471(15) Uani 1 1 d . . . H24 H 0.3503 0.2118 0.0357 0.057 Uiso 1 1 calc R . . C25 C 0.4776(8) 0.2164(6) -0.0764(5) 0.060(2) Uani 1 1 d . . . H25 H 0.4074 0.1979 -0.0999 0.072 Uiso 1 1 calc R . . C26 C 0.6156(8) 0.2356(5) -0.1226(4) 0.0535(18) Uani 1 1 d . . . H26 H 0.6401 0.2294 -0.1776 0.064 Uiso 1 1 calc R . . C27 C 0.7149(7) 0.2632(4) -0.0884(4) 0.0420(14) Uani 1 1 d . . . H27 H 0.8082 0.2768 -0.1200 0.050 Uiso 1 1 calc R . . C28 C 0.6808(6) 0.2715(4) -0.0075(3) 0.0334(12) Uani 1 1 d . . . H28 H 0.7513 0.2910 0.0152 0.040 Uiso 1 1 calc R . . C29 C 0.3711(6) 0.3502(4) 0.1514(3) 0.0328(12) Uani 1 1 d . . . C30 C 0.3939(6) 0.4167(4) 0.0883(4) 0.0398(14) Uani 1 1 d . . . H30 H 0.4684 0.4119 0.0421 0.048 Uiso 1 1 calc R . . C31 C 0.3084(7) 0.4911(4) 0.0916(4) 0.0453(15) Uani 1 1 d . . . H31 H 0.3254 0.5365 0.0478 0.054 Uiso 1 1 calc R . . C32 C 0.2006(7) 0.4984(4) 0.1576(4) 0.0406(14) Uani 1 1 d . . . H32 H 0.1438 0.5493 0.1601 0.049 Uiso 1 1 calc R . . C33 C 0.1739(6) 0.4315(4) 0.2211(4) 0.0394(13) Uani 1 1 d . . . H33 H 0.0979 0.4359 0.2667 0.047 Uiso 1 1 calc R . . C34 C 0.2594(6) 0.3578(4) 0.2176(3) 0.0347(12) Uani 1 1 d . . . H34 H 0.2411 0.3122 0.2610 0.042 Uiso 1 1 calc R . . C37 C 0.0975(8) 0.3292(6) 0.9450(6) 0.062(2) Uani 1 1 d . . . C38 C 0.1060(10) 0.3924(7) 0.9956(7) 0.083(3) Uani 1 1 d . . . H38A H 0.1717 0.3715 1.0303 0.099 Uiso 1 1 calc R . . H38B H 0.0104 0.4025 1.0287 0.099 Uiso 1 1 calc R . . H38C H 0.1417 0.4457 0.9617 0.099 Uiso 1 1 calc R . . C39 C 0.9909(11) 1.0100(9) 0.3927(6) 0.094(4) Uani 1 1 d . . . C40 C 1.0360(12) 1.0967(6) 0.4138(8) 0.103(4) Uani 1 1 d . . . H40A H 1.0095 1.0954 0.4720 0.123 Uiso 1 1 calc R . . H40B H 0.9862 1.1447 0.3878 0.123 Uiso 1 1 calc R . . H40C H 1.1400 1.1033 0.3945 0.123 Uiso 1 1 calc R . . C41 C 0.0568(8) 0.6260(5) 0.3372(5) 0.0524(17) Uani 1 1 d . . . C42 C 0.0350(10) 0.5621(6) 0.4077(5) 0.064(2) Uani 1 1 d . . . H42A H 0.0109 0.5084 0.3942 0.077 Uiso 1 1 calc R . . H42B H -0.0437 0.5803 0.4492 0.077 Uiso 1 1 calc R . . H42C H 0.1231 0.5541 0.4276 0.077 Uiso 1 1 calc R . . N5 N 0.6985(9) 0.0861(7) 0.5371(7) 0.103(3) Uani 1 1 d . . . C35 C 0.7216(10) 0.1430(8) 0.5662(6) 0.080(3) Uani 1 1 d . . . C36 C 0.7629(11) 0.2139(7) 0.6022(6) 0.079(3) Uani 1 1 d . . . H36A H 0.8529 0.1986 0.6190 0.095 Uiso 1 1 calc R . . H36B H 0.6870 0.2238 0.6487 0.095 Uiso 1 1 calc R . . H36C H 0.7758 0.2656 0.5623 0.095 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 Ru 0.01767(19) 0.0394(2) 0.0269(2) -0.00418(16) -0.00264(15) -0.00311(15) Pd 0.0204(2) 0.0594(3) 0.0358(2) -0.0153(2) -0.00766(16) 0.00005(17) Cl1 0.0169(5) 0.0556(8) 0.0375(7) -0.0135(6) -0.0059(5) 0.0009(5) Cl2 0.0335(7) 0.0415(7) 0.0345(7) -0.0060(6) 0.0005(5) -0.0088(5) Cl3 0.0219(6) 0.0783(11) 0.0400(7) -0.0121(7) -0.0120(5) 0.0020(6) Cl4 0.0361(8) 0.0920(13) 0.0530(9) -0.0387(9) -0.0187(7) 0.0119(8) P 0.0219(6) 0.0362(7) 0.0288(6) -0.0024(5) -0.0065(5) -0.0028(5) N1 0.020(2) 0.063(3) 0.031(2) -0.009(2) -0.0061(19) 0.006(2) N2 0.029(2) 0.047(3) 0.045(3) -0.015(2) -0.014(2) 0.000(2) N3 0.021(2) 0.051(3) 0.037(3) -0.002(2) -0.0086(19) 0.002(2) N4 0.031(2) 0.053(3) 0.029(2) -0.004(2) -0.005(2) 0.001(2) N6 0.082(6) 0.105(7) 0.091(6) -0.029(6) -0.014(5) -0.018(5) N7 0.046(5) 0.228(14) 0.178(12) -0.134(12) -0.011(6) -0.027(6) N8 0.068(5) 0.098(6) 0.053(4) 0.008(4) -0.003(3) 0.010(4) C1 0.017(2) 0.040(3) 0.028(3) 0.003(2) -0.003(2) 0.004(2) C2 0.021(3) 0.058(4) 0.030(3) -0.019(3) -0.003(2) 0.004(2) C3 0.024(3) 0.080(5) 0.039(3) -0.015(3) -0.004(2) 0.005(3) C4 0.051(4) 0.113(7) 0.033(4) -0.019(4) -0.007(3) 0.017(4) C5 0.045(4) 0.110(7) 0.028(3) 0.006(4) 0.001(3) 0.009(4) C6 0.036(3) 0.074(5) 0.040(4) 0.015(3) 0.008(3) 0.006(3) C7 0.019(2) 0.062(4) 0.035(3) 0.000(3) 0.000(2) 0.001(2) C8 0.036(3) 0.059(4) 0.047(4) -0.016(3) -0.015(3) 0.005(3) C9 0.044(4) 0.072(5) 0.080(6) -0.039(4) -0.026(4) 0.022(4) C10 0.081(6) 0.058(5) 0.115(8) -0.042(5) -0.048(6) 0.019(4) C11 0.072(6) 0.083(6) 0.118(8) -0.061(6) -0.053(6) 0.017(5) C12 0.046(4) 0.049(4) 0.068(5) -0.019(3) -0.023(3) -0.004(3) C13 0.032(3) 0.058(4) 0.043(3) -0.001(3) -0.011(3) 0.000(3) C14 0.065(5) 0.061(5) 0.073(6) 0.016(4) -0.015(4) -0.007(4) C15 0.037(3) 0.041(3) 0.049(4) -0.004(3) -0.008(3) 0.003(3) C16 0.069(5) 0.066(5) 0.082(6) -0.029(5) -0.001(5) 0.019(4) C17 0.036(3) 0.036(3) 0.038(3) -0.002(2) -0.010(2) -0.008(2) C18 0.039(3) 0.039(3) 0.059(4) -0.002(3) -0.019(3) -0.008(3) C19 0.050(4) 0.044(4) 0.108(7) 0.012(4) -0.033(5) -0.010(3) C20 0.065(5) 0.054(5) 0.131(9) 0.027(5) -0.037(6) -0.034(4) C21 0.039(4) 0.051(4) 0.109(7) 0.020(4) -0.019(4) -0.008(3) C22 0.023(3) 0.050(4) 0.060(4) -0.005(3) -0.014(3) -0.010(2) C23 0.039(3) 0.037(3) 0.037(3) -0.010(2) -0.011(2) 0.001(2) C24 0.035(3) 0.067(4) 0.045(4) -0.012(3) -0.015(3) -0.002(3) C25 0.047(4) 0.089(6) 0.054(4) -0.027(4) -0.021(3) -0.004(4) C26 0.057(4) 0.074(5) 0.036(3) -0.019(3) -0.018(3) 0.010(4) C27 0.043(3) 0.047(3) 0.033(3) -0.006(3) -0.003(3) 0.010(3) C28 0.031(3) 0.040(3) 0.029(3) -0.004(2) -0.009(2) 0.002(2) C29 0.024(3) 0.039(3) 0.033(3) -0.001(2) -0.005(2) -0.005(2) C30 0.029(3) 0.037(3) 0.046(3) 0.001(3) 0.000(3) -0.001(2) C31 0.040(3) 0.040(3) 0.051(4) 0.001(3) -0.009(3) 0.004(3) C32 0.036(3) 0.033(3) 0.054(4) -0.007(3) -0.012(3) 0.003(2) C33 0.026(3) 0.053(4) 0.038(3) -0.010(3) -0.006(2) 0.005(2) C34 0.026(3) 0.045(3) 0.032(3) -0.003(2) -0.008(2) -0.004(2) C37 0.041(4) 0.068(5) 0.083(6) -0.023(5) -0.016(4) -0.001(3) C38 0.061(5) 0.089(7) 0.096(8) -0.039(6) 0.002(5) -0.005(5) C39 0.061(6) 0.148(11) 0.064(6) 0.014(6) -0.016(5) -0.004(6) C40 0.084(7) 0.066(6) 0.135(11) 0.025(6) -0.001(7) -0.025(5) C41 0.042(4) 0.070(5) 0.048(4) -0.011(4) -0.014(3) -0.002(3) C42 0.074(5) 0.078(6) 0.044(4) -0.008(4) -0.018(4) -0.016(4) N5 0.062(5) 0.126(8) 0.126(8) 0.012(7) -0.043(5) -0.046(5) C35 0.057(5) 0.115(8) 0.061(5) 0.013(5) -0.011(4) -0.025(5) C36 0.069(6) 0.104(7) 0.060(5) -0.010(5) -0.005(4) -0.021(5) _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 Ru N3 2.016(5) . ? Ru C1 2.040(5) . ? Ru N4 2.106(5) . ? Ru P 2.3007(14) . ? Ru Cl2 2.4182(15) . ? Ru Cl1 2.4780(13) . ? Pd C2 1.978(6) . ? Pd Cl1 2.3139(14) . ? Pd Cl4 2.3150(16) . ? Pd Cl3 2.3767(14) . ? P C17 1.838(6) . ? P C29 1.839(6) . ? P C23 1.851(6) . ? N1 C1 1.334(7) . ? N1 C3 1.482(8) . ? N1 C7 1.484(9) . ? N2 C2 1.273(8) . ? N2 C8 1.482(8) . ? N2 C12 1.484(8) . ? N3 C13 1.135(9) . ? N4 C15 1.127(8) . ? N6 C37 1.108(12) . ? N7 C39 1.331(18) . ? N8 C41 1.131(11) . ? C1 C2 1.463(8) . ? C3 C4 1.514(10) . ? C4 C5 1.538(13) . ? C5 C6 1.540(11) . ? C6 C7 1.504(9) . ? C8 C9 1.535(9) . ? C9 C10 1.518(12) . ? C10 C11 1.520(12) . ? C11 C12 1.521(10) . ? C13 C14 1.469(10) . ? C15 C16 1.456(10) . ? C17 C18 1.385(9) . ? C17 C22 1.403(8) . ? C18 C19 1.374(10) . ? C19 C20 1.397(12) . ? C20 C21 1.353(12) . ? C21 C22 1.375(10) . ? C23 C28 1.382(8) . ? C23 C24 1.402(9) . ? C24 C25 1.390(10) . ? C25 C26 1.398(11) . ? C26 C27 1.365(10) . ? C27 C28 1.393(8) . ? C29 C30 1.381(8) . ? C29 C34 1.391(8) . ? C30 C31 1.404(9) . ? C31 C32 1.367(9) . ? C32 C33 1.391(9) . ? C33 C34 1.392(9) . ? C37 C38 1.463(12) . ? C39 C40 1.599(17) . ? C41 C42 1.441(11) . ? N5 C35 1.167(15) . ? C35 C36 1.495(15) . ? 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 N3 Ru C1 91.3(2) . . ? N3 Ru N4 85.6(2) . . ? C1 Ru N4 170.0(2) . . ? N3 Ru P 98.26(14) . . ? C1 Ru P 97.13(15) . . ? N4 Ru P 92.71(14) . . ? N3 Ru Cl2 172.88(13) . . ? C1 Ru Cl2 92.90(16) . . ? N4 Ru Cl2 89.32(15) . . ? P Ru Cl2 86.92(5) . . ? N3 Ru Cl1 85.65(14) . . ? C1 Ru Cl1 86.08(15) . . ? N4 Ru Cl1 84.23(14) . . ? P Ru Cl1 174.86(5) . . ? Cl2 Ru Cl1 88.91(5) . . ? C2 Pd Cl1 86.25(16) . . ? C2 Pd Cl4 89.98(16) . . ? Cl1 Pd Cl4 174.96(5) . . ? C2 Pd Cl3 175.79(18) . . ? Cl1 Pd Cl3 92.34(5) . . ? Cl4 Pd Cl3 91.64(6) . . ? Pd Cl1 Ru 102.99(5) . . ? C17 P C29 106.7(3) . . ? C17 P C23 98.3(3) . . ? C29 P C23 101.5(3) . . ? C17 P Ru 116.3(2) . . ? C29 P Ru 115.43(19) . . ? C23 P Ru 116.3(2) . . ? C1 N1 C3 122.6(6) . . ? C1 N1 C7 125.2(5) . . ? C3 N1 C7 112.0(5) . . ? C2 N2 C8 123.8(5) . . ? C2 N2 C12 122.7(5) . . ? C8 N2 C12 113.4(6) . . ? C13 N3 Ru 174.6(5) . . ? C15 N4 Ru 175.5(5) . . ? N1 C1 C2 117.5(5) . . ? N1 C1 Ru 131.6(5) . . ? C2 C1 Ru 109.8(3) . . ? N2 C2 C1 123.7(5) . . ? N2 C2 Pd 123.5(4) . . ? C1 C2 Pd 112.5(4) . . ? N1 C3 C4 110.4(6) . . ? C3 C4 C5 112.8(7) . . ? C4 C5 C6 109.2(6) . . ? C7 C6 C5 110.6(6) . . ? N1 C7 C6 110.3(6) . . ? N2 C8 C9 109.5(5) . . ? C10 C9 C8 110.8(6) . . ? C9 C10 C11 110.7(8) . . ? C10 C11 C12 112.0(7) . . ? N2 C12 C11 110.0(6) . . ? N3 C13 C14 177.3(7) . . ? N4 C15 C16 177.7(8) . . ? C18 C17 C22 117.9(6) . . ? C18 C17 P 117.0(5) . . ? C22 C17 P 124.9(5) . . ? C19 C18 C17 121.9(7) . . ? C18 C19 C20 118.9(8) . . ? C21 C20 C19 119.9(7) . . ? C20 C21 C22 121.5(7) . . ? C21 C22 C17 119.9(7) . . ? C28 C23 C24 118.0(6) . . ? C28 C23 P 123.6(5) . . ? C24 C23 P 118.4(5) . . ? C25 C24 C23 121.2(6) . . ? C24 C25 C26 119.3(7) . . ? C27 C26 C25 119.8(6) . . ? C26 C27 C28 120.7(6) . . ? C23 C28 C27 121.0(6) . . ? C30 C29 C34 118.6(6) . . ? C30 C29 P 119.5(4) . . ? C34 C29 P 121.8(5) . . ? C29 C30 C31 120.7(6) . . ? C32 C31 C30 120.1(6) . . ? C31 C32 C33 120.0(6) . . ? C32 C33 C34 119.6(6) . . ? C29 C34 C33 121.0(6) . . ? N6 C37 C38 177.7(11) . . ? N7 C39 C40 169.1(12) . . ? N8 C41 C42 178.3(9) . . ? N5 C35 C36 175.7(12) . . ? 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 C2 Pd Cl1 Ru -20.59(19) . . . . ? Cl4 Pd Cl1 Ru 21.3(8) . . . . ? Cl3 Pd Cl1 Ru 163.38(6) . . . . ? N3 Ru Cl1 Pd -97.44(15) . . . . ? C1 Ru Cl1 Pd -5.83(16) . . . . ? N4 Ru Cl1 Pd 176.58(15) . . . . ? P Ru Cl1 Pd 122.9(6) . . . . ? Cl2 Ru Cl1 Pd 87.16(6) . . . . ? N3 Ru P C17 0.3(3) . . . . ? C1 Ru P C17 -92.1(3) . . . . ? N4 Ru P C17 86.2(3) . . . . ? Cl2 Ru P C17 175.4(2) . . . . ? Cl1 Ru P C17 139.5(6) . . . . ? N3 Ru P C29 126.4(2) . . . . ? C1 Ru P C29 34.1(3) . . . . ? N4 Ru P C29 -147.6(2) . . . . ? Cl2 Ru P C29 -58.5(2) . . . . ? Cl1 Ru P C29 -94.3(6) . . . . ? N3 Ru P C23 -114.7(3) . . . . ? C1 Ru P C23 152.9(3) . . . . ? N4 Ru P C23 -28.8(3) . . . . ? Cl2 Ru P C23 60.3(2) . . . . ? Cl1 Ru P C23 24.5(7) . . . . ? C1 Ru N3 C13 -126(6) . . . . ? N4 Ru N3 C13 45(6) . . . . ? P Ru N3 C13 137(6) . . . . ? Cl2 Ru N3 C13 1(7) . . . . ? Cl1 Ru N3 C13 -40(6) . . . . ? N3 Ru N4 C15 -32(7) . . . . ? C1 Ru N4 C15 40(7) . . . . ? P Ru N4 C15 -130(7) . . . . ? Cl2 Ru N4 C15 143(7) . . . . ? Cl1 Ru N4 C15 54(7) . . . . ? C3 N1 C1 C2 7.2(8) . . . . ? C7 N1 C1 C2 -167.1(5) . . . . ? C3 N1 C1 Ru 173.5(4) . . . . ? C7 N1 C1 Ru -0.8(9) . . . . ? N3 Ru C1 N1 -38.0(5) . . . . ? N4 Ru C1 N1 -109.6(12) . . . . ? P Ru C1 N1 60.5(5) . . . . ? Cl2 Ru C1 N1 147.7(5) . . . . ? Cl1 Ru C1 N1 -123.6(5) . . . . ? N3 Ru C1 C2 129.1(4) . . . . ? N4 Ru C1 C2 57.5(14) . . . . ? P Ru C1 C2 -132.4(4) . . . . ? Cl2 Ru C1 C2 -45.2(4) . . . . ? Cl1 Ru C1 C2 43.5(4) . . . . ? C8 N2 C2 C1 13.4(9) . . . . ? C12 N2 C2 C1 -164.7(6) . . . . ? C8 N2 C2 Pd -173.7(4) . . . . ? C12 N2 C2 Pd 8.3(8) . . . . ? N1 C1 C2 N2 -95.5(7) . . . . ? Ru C1 C2 N2 95.3(6) . . . . ? N1 C1 C2 Pd 90.8(5) . . . . ? Ru C1 C2 Pd -78.3(4) . . . . ? Cl1 Pd C2 N2 -115.0(5) . . . . ? Cl4 Pd C2 N2 68.4(5) . . . . ? Cl3 Pd C2 N2 -44(3) . . . . ? Cl1 Pd C2 C1 58.7(4) . . . . ? Cl4 Pd C2 C1 -117.9(4) . . . . ? Cl3 Pd C2 C1 129(2) . . . . ? C1 N1 C3 C4 -117.9(7) . . . . ? C7 N1 C3 C4 57.0(7) . . . . ? N1 C3 C4 C5 -53.8(8) . . . . ? C3 C4 C5 C6 52.6(8) . . . . ? C4 C5 C6 C7 -54.8(8) . . . . ? C1 N1 C7 C6 114.4(6) . . . . ? C3 N1 C7 C6 -60.4(6) . . . . ? C5 C6 C7 N1 59.0(7) . . . . ? C2 N2 C8 C9 123.5(7) . . . . ? C12 N2 C8 C9 -58.3(8) . . . . ? N2 C8 C9 C10 56.5(9) . . . . ? C8 C9 C10 C11 -55.0(11) . . . . ? C9 C10 C11 C12 54.1(12) . . . . ? C2 N2 C12 C11 -124.7(7) . . . . ? C8 N2 C12 C11 57.0(9) . . . . ? C10 C11 C12 N2 -54.0(12) . . . . ? Ru N3 C13 C14 165(13) . . . . ? Ru N4 C15 C16 126(19) . . . . ? C29 P C17 C18 -177.4(5) . . . . ? C23 P C17 C18 77.8(6) . . . . ? Ru P C17 C18 -47.0(6) . . . . ? C29 P C17 C22 8.0(6) . . . . ? C23 P C17 C22 -96.8(6) . . . . ? Ru P C17 C22 138.4(5) . . . . ? C22 C17 C18 C19 -2.0(11) . . . . ? P C17 C18 C19 -177.0(7) . . . . ? C17 C18 C19 C20 0.1(14) . . . . ? C18 C19 C20 C21 1.6(17) . . . . ? C19 C20 C21 C22 -1.1(18) . . . . ? C20 C21 C22 C17 -0.9(15) . . . . ? C18 C17 C22 C21 2.4(11) . . . . ? P C17 C22 C21 177.0(7) . . . . ? C17 P C23 C28 -141.6(5) . . . . ? C29 P C23 C28 109.4(5) . . . . ? Ru P C23 C28 -16.8(6) . . . . ? C17 P C23 C24 36.9(6) . . . . ? C29 P C23 C24 -72.1(6) . . . . ? Ru P C23 C24 161.7(5) . . . . ? C28 C23 C24 C25 0.9(11) . . . . ? P C23 C24 C25 -177.7(6) . . . . ? C23 C24 C25 C26 0.0(13) . . . . ? C24 C25 C26 C27 -0.9(13) . . . . ? C25 C26 C27 C28 0.8(11) . . . . ? C24 C23 C28 C27 -1.0(9) . . . . ? P C23 C28 C27 177.5(5) . . . . ? C26 C27 C28 C23 0.1(10) . . . . ? C17 P C29 C30 -135.3(5) . . . . ? C23 P C29 C30 -33.0(6) . . . . ? Ru P C29 C30 93.7(5) . . . . ? C17 P C29 C34 48.6(6) . . . . ? C23 P C29 C34 151.0(5) . . . . ? Ru P C29 C34 -82.3(5) . . . . ? C34 C29 C30 C31 1.4(10) . . . . ? P C29 C30 C31 -174.8(5) . . . . ? C29 C30 C31 C32 -0.2(11) . . . . ? C30 C31 C32 C33 -1.1(10) . . . . ? C31 C32 C33 C34 1.2(10) . . . . ? C30 C29 C34 C33 -1.2(9) . . . . ? P C29 C34 C33 174.9(5) . . . . ? C32 C33 C34 C29 0.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 70.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.712 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.120 #============================================================================= # end of cif data for "pet15a" (compound 6) #============================================================================= #============================================================================= # cif data for "pet13" (compound 7) #============================================================================= data_pet13 _database_code_depnum_ccdc_archive 'CCDC 819872' #TrackingRef 'pet-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H84 Cl16 N6 P2 Pd2 Ru2' _chemical_formula_weight 2029.49 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' Pd Pd -0.9988 1.0072 '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 17.1006(4) _cell_length_b 18.8239(4) _cell_length_c 21.0090(6) _cell_angle_alpha 94.226(2) _cell_angle_beta 110.213(2) _cell_angle_gamma 98.865(2) _cell_volume 6211.5(3) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 51586 _cell_measurement_theta_min 2.2047 _cell_measurement_theta_max 29.3300 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3048 _exptl_absorpt_coefficient_mu 1.382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95975 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 196062 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.37 _reflns_number_total 25393 _reflns_number_gt 17593 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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^)+(0.0332P)^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 'methyls rigid and other riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25393 _refine_ls_number_parameters 1270 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.007 _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 0.089883(15) 0.657010(13) 0.314024(12) 0.01382(6) Uani 1 1 d . . . Ru2 Ru -0.118275(15) 0.665350(13) 0.341189(12) 0.01460(6) Uani 1 1 d . . . Ru3 Ru 0.896717(15) 1.004366(14) 1.013223(12) 0.01511(6) Uani 1 1 d . . . Pd1 Pd 0.224101(15) 0.832501(13) 0.316758(12) 0.01891(6) Uani 1 1 d . . . Pd2 Pd -0.239864(16) 0.479295(14) 0.331371(13) 0.02345(7) Uani 1 1 d . . . Pd3 Pd 0.755301(15) 0.824199(14) 0.979683(13) 0.02112(6) Uani 1 1 d . . . Cl1 Cl 0.35838(5) 0.89267(5) 0.38584(4) 0.0368(2) Uani 1 1 d . . . Cl2 Cl 0.23423(6) 0.88755(5) 0.22109(4) 0.0343(2) Uani 1 1 d . . . Cl3 Cl 0.08588(5) 0.76721(4) 0.25861(4) 0.01951(17) Uani 1 1 d . . . Cl4 Cl -0.06595(5) 0.61219(4) 0.25624(4) 0.02052(17) Uani 1 1 d . . . Cl5 Cl 0.03512(5) 0.71722(4) 0.39264(4) 0.02107(18) Uani 1 1 d . . . Cl6 Cl -0.10645(5) 0.55252(4) 0.39149(4) 0.02164(18) Uani 1 1 d . . . Cl7 Cl -0.37024(6) 0.41328(5) 0.26036(5) 0.0446(3) Uani 1 1 d . . . Cl8 Cl -0.23871(6) 0.40933(5) 0.42155(5) 0.0447(3) Uani 1 1 d . . . Cl9 Cl 0.61753(6) 0.78067(5) 0.90618(5) 0.0393(2) Uani 1 1 d . . . Cl10 Cl 0.74810(6) 0.73661(5) 1.05440(5) 0.0408(2) Uani 1 1 d . . . Cl11 Cl 0.89276(5) 0.88299(4) 1.04775(4) 0.02116(17) Uani 1 1 d . . . Cl12 Cl 1.05167(5) 1.04061(4) 1.07451(4) 0.02171(18) Uani 1 1 d . . . N1 N 0.28061(16) 0.67369(14) 0.39794(12) 0.0211(6) Uani 1 1 d . . . N2 N 0.21546(15) 0.80473(14) 0.44918(12) 0.0199(6) Uani 1 1 d . . . N3 N -0.31321(16) 0.64204(14) 0.27301(12) 0.0221(6) Uani 1 1 d . . . N4 N -0.24659(16) 0.52742(14) 0.20047(13) 0.0210(6) Uani 1 1 d . . . N5 N 0.09207(16) 0.57558(14) 0.36878(12) 0.0210(6) Uani 1 1 d . . . N6 N -0.12945(16) 0.74919(14) 0.28794(12) 0.0205(6) Uani 1 1 d . . . N7 N 0.76475(15) 0.88230(14) 0.85819(12) 0.0200(6) Uani 1 1 d . . . N8 N 0.70766(16) 1.00257(14) 0.93344(12) 0.0211(6) Uani 1 1 d . . . N9 N 0.90275(16) 1.09803(15) 0.97473(12) 0.0211(6) Uani 1 1 d . . . P1 P 0.10646(5) 0.58570(4) 0.22657(4) 0.01756(18) Uani 1 1 d . . . P2 P -0.12816(5) 0.73076(5) 0.43483(4) 0.01866(19) Uani 1 1 d . . . P3 P 0.88419(5) 1.05529(5) 1.11198(4) 0.01845(18) Uani 1 1 d . . . C1 C 0.21806(18) 0.77874(17) 0.39116(14) 0.0163(7) Uani 1 1 d . . . C2 C 0.21073(18) 0.70015(16) 0.37232(14) 0.0151(7) Uani 1 1 d . . . C3 C 0.2158(2) 0.76242(19) 0.50664(15) 0.0266(8) Uani 1 1 d . . . H3A H 0.2229 0.7124 0.4952 0.032 Uiso 1 1 calc R . . H3B H 0.1607 0.7594 0.5131 0.032 Uiso 1 1 calc R . . C4 C 0.2875(2) 0.7985(2) 0.57254(16) 0.0333(9) Uani 1 1 d . . . H4A H 0.3427 0.7967 0.5677 0.040 Uiso 1 1 calc R . . H4B H 0.2846 0.7716 0.6107 0.040 Uiso 1 1 calc R . . C5 C 0.2813(2) 0.8772(2) 0.58894(18) 0.0417(10) Uani 1 1 d . . . H5A H 0.2289 0.8789 0.5987 0.050 Uiso 1 1 calc R . . H5B H 0.3305 0.9008 0.6302 0.050 Uiso 1 1 calc R . . C6 C 0.2800(2) 0.9180(2) 0.52899(17) 0.0381(10) Uani 1 1 d . . . H6A H 0.2726 0.9681 0.5392 0.046 Uiso 1 1 calc R . . H6B H 0.3350 0.9207 0.5225 0.046 Uiso 1 1 calc R . . C7 C 0.2090(2) 0.88102(18) 0.46390(17) 0.0283(8) Uani 1 1 d . . . H7A H 0.1537 0.8828 0.4686 0.034 Uiso 1 1 calc R . . H7B H 0.2118 0.9071 0.4253 0.034 Uiso 1 1 calc R . . C8 C 0.36228(19) 0.71779(19) 0.44621(16) 0.0282(8) Uani 1 1 d . . . H8A H 0.3741 0.7028 0.4923 0.034 Uiso 1 1 calc R . . H8B H 0.3577 0.7696 0.4496 0.034 Uiso 1 1 calc R . . C9 C 0.4354(2) 0.7086(2) 0.42262(19) 0.0356(9) Uani 1 1 d . . . H9A H 0.4262 0.7275 0.3784 0.043 Uiso 1 1 calc R . . H9B H 0.4893 0.7369 0.4566 0.043 Uiso 1 1 calc R . . C10 C 0.4417(2) 0.6289(2) 0.41437(19) 0.0408(10) Uani 1 1 d . . . H10A H 0.4878 0.6232 0.3972 0.049 Uiso 1 1 calc R . . H10B H 0.4551 0.6107 0.4592 0.049 Uiso 1 1 calc R . . C11 C 0.3576(2) 0.5855(2) 0.36403(18) 0.0382(10) Uani 1 1 d . . . H11A H 0.3604 0.5333 0.3604 0.046 Uiso 1 1 calc R . . H11B H 0.3473 0.6008 0.3182 0.046 Uiso 1 1 calc R . . C12 C 0.2843(2) 0.59670(18) 0.38676(17) 0.0281(8) Uani 1 1 d . . . H12A H 0.2302 0.5707 0.3514 0.034 Uiso 1 1 calc R . . H12B H 0.2910 0.5757 0.4297 0.034 Uiso 1 1 calc R . . C13 C -0.24009(19) 0.61996(17) 0.28916(14) 0.0165(7) Uani 1 1 d . . . C14 C -0.24436(18) 0.54380(17) 0.26234(15) 0.0192(7) Uani 1 1 d . . . C15 C -0.3200(2) 0.71748(18) 0.28879(17) 0.0280(8) Uani 1 1 d . . . H15A H -0.3337 0.7404 0.2463 0.034 Uiso 1 1 calc R . . H15B H -0.2645 0.7445 0.3215 0.034 Uiso 1 1 calc R . . C16 C -0.3882(2) 0.7232(2) 0.31956(18) 0.0354(9) Uani 1 1 d . . . H16A H -0.3700 0.7077 0.3657 0.043 Uiso 1 1 calc R . . H16B H -0.3948 0.7744 0.3247 0.043 Uiso 1 1 calc R . . C17 C -0.4733(2) 0.6762(2) 0.27483(19) 0.0397(10) Uani 1 1 d . . . H17A H -0.5152 0.6782 0.2974 0.048 Uiso 1 1 calc R . . H17B H -0.4949 0.6944 0.2302 0.048 Uiso 1 1 calc R . . C18 C -0.4617(2) 0.5988(2) 0.26377(19) 0.0391(10) Uani 1 1 d . . . H18A H -0.5166 0.5681 0.2340 0.047 Uiso 1 1 calc R . . H18B H -0.4433 0.5800 0.3083 0.047 Uiso 1 1 calc R . . C19 C -0.3961(2) 0.59422(19) 0.23088(17) 0.0302(9) Uani 1 1 d . . . H19A H -0.3881 0.5434 0.2259 0.036 Uiso 1 1 calc R . . H19B H -0.4167 0.6090 0.1846 0.036 Uiso 1 1 calc R . . C20 C -0.2563(2) 0.57860(19) 0.14884(15) 0.0279(8) Uani 1 1 d . . . H20A H -0.2039 0.5883 0.1382 0.033 Uiso 1 1 calc R . . H20B H -0.2651 0.6252 0.1676 0.033 Uiso 1 1 calc R . . C21 C -0.3316(2) 0.5464(2) 0.08389(16) 0.0373(10) Uani 1 1 d . . . H21A H -0.3358 0.5796 0.0490 0.045 Uiso 1 1 calc R . . H21B H -0.3845 0.5409 0.0938 0.045 Uiso 1 1 calc R . . C22 C -0.3217(3) 0.4726(2) 0.05598(18) 0.0467(11) Uani 1 1 d . . . H22A H -0.3728 0.4512 0.0153 0.056 Uiso 1 1 calc R . . H22B H -0.2720 0.4787 0.0416 0.056 Uiso 1 1 calc R . . C23 C -0.3099(3) 0.4223(2) 0.10981(18) 0.0448(11) Uani 1 1 d . . . H23A H -0.2998 0.3758 0.0919 0.054 Uiso 1 1 calc R . . H23B H -0.3624 0.4119 0.1203 0.054 Uiso 1 1 calc R . . C24 C -0.2353(2) 0.45579(19) 0.17524(17) 0.0326(9) Uani 1 1 d . . . H24A H -0.2312 0.4232 0.2107 0.039 Uiso 1 1 calc R . . H24B H -0.1818 0.4613 0.1660 0.039 Uiso 1 1 calc R . . C25 C 0.0904(2) 0.53015(19) 0.40125(16) 0.0275(8) Uani 1 1 d . . . C26 C 0.0874(3) 0.4698(2) 0.44021(19) 0.0523(12) Uani 1 1 d . . . H26A H 0.0327 0.4606 0.4464 0.063 Uiso 1 1 calc R . . H26B H 0.1335 0.4818 0.4851 0.063 Uiso 1 1 calc R . . H26C H 0.0941 0.4264 0.4154 0.063 Uiso 1 1 calc R . . C27 C -0.1339(2) 0.79360(19) 0.25443(17) 0.0270(8) Uani 1 1 d . . . C28 C -0.1383(3) 0.8523(2) 0.2130(2) 0.0604(13) Uani 1 1 d . . . H28A H -0.1118 0.8986 0.2429 0.073 Uiso 1 1 calc R . . H28B H -0.1978 0.8530 0.1865 0.073 Uiso 1 1 calc R . . H28C H -0.1082 0.8449 0.1816 0.073 Uiso 1 1 calc R . . C29 C 0.19248(19) 0.61285(18) 0.19551(15) 0.0211(7) Uani 1 1 d . . . C30 C 0.2395(2) 0.68231(19) 0.21568(17) 0.0301(8) Uani 1 1 d . . . H30 H 0.2311 0.7134 0.2495 0.036 Uiso 1 1 calc R . . C31 C 0.2987(2) 0.7076(2) 0.1875(2) 0.0419(10) Uani 1 1 d . . . H31 H 0.3296 0.7560 0.2013 0.050 Uiso 1 1 calc R . . C32 C 0.3130(2) 0.6626(2) 0.13920(19) 0.0434(11) Uani 1 1 d . . . H32 H 0.3543 0.6796 0.1203 0.052 Uiso 1 1 calc R . . C33 C 0.2668(3) 0.5927(2) 0.1189(2) 0.0532(12) Uani 1 1 d . . . H33 H 0.2763 0.5613 0.0859 0.064 Uiso 1 1 calc R . . C34 C 0.2066(2) 0.5683(2) 0.14646(19) 0.0446(11) Uani 1 1 d . . . H34 H 0.1744 0.5203 0.1316 0.054 Uiso 1 1 calc R . . C35 C 0.1104(2) 0.49142(18) 0.24384(15) 0.0260(8) Uani 1 1 d . . . C36 C 0.1816(3) 0.4607(2) 0.25437(19) 0.0417(10) Uani 1 1 d . . . H36 H 0.2299 0.4871 0.2483 0.050 Uiso 1 1 calc R . . C37 C 0.1832(3) 0.3922(2) 0.2735(2) 0.0660(15) Uani 1 1 d . . . H37 H 0.2330 0.3722 0.2817 0.079 Uiso 1 1 calc R . . C38 C 0.1130(4) 0.3530(2) 0.2808(2) 0.0709(16) Uani 1 1 d . . . H38 H 0.1142 0.3057 0.2936 0.085 Uiso 1 1 calc R . . C39 C 0.0407(3) 0.3818(2) 0.2698(2) 0.0545(13) Uani 1 1 d . . . H39 H -0.0082 0.3545 0.2744 0.065 Uiso 1 1 calc R . . C40 C 0.0406(3) 0.45105(19) 0.25196(17) 0.0359(9) Uani 1 1 d . . . H40 H -0.0088 0.4714 0.2451 0.043 Uiso 1 1 calc R . . C41 C 0.01579(19) 0.57137(17) 0.14442(15) 0.0191(7) Uani 1 1 d . . . C42 C -0.0234(2) 0.62923(18) 0.12234(15) 0.0240(8) Uani 1 1 d . . . H42 H -0.0048 0.6749 0.1506 0.029 Uiso 1 1 calc R . . C43 C -0.0893(2) 0.6211(2) 0.05946(16) 0.0305(9) Uani 1 1 d . . . H43 H -0.1157 0.6610 0.0451 0.037 Uiso 1 1 calc R . . C44 C -0.1162(2) 0.5557(2) 0.01814(17) 0.0355(9) Uani 1 1 d . . . H44 H -0.1615 0.5502 -0.0248 0.043 Uiso 1 1 calc R . . C45 C -0.0776(2) 0.4976(2) 0.03888(17) 0.0372(9) Uani 1 1 d . . . H45 H -0.0958 0.4523 0.0100 0.045 Uiso 1 1 calc R . . C46 C -0.0126(2) 0.50574(19) 0.10173(16) 0.0287(8) Uani 1 1 d . . . H46 H 0.0132 0.4655 0.1160 0.034 Uiso 1 1 calc R . . C47 C -0.0336(2) 0.74364(19) 0.51468(15) 0.0235(8) Uani 1 1 d . . . C48 C 0.0101(2) 0.6875(2) 0.53242(16) 0.0282(8) Uani 1 1 d . . . H48 H -0.0061 0.6437 0.5016 0.034 Uiso 1 1 calc R . . C49 C 0.0774(2) 0.6943(2) 0.59464(17) 0.0363(10) Uani 1 1 d . . . H49 H 0.1067 0.6554 0.6062 0.044 Uiso 1 1 calc R . . C50 C 0.1008(2) 0.7575(2) 0.63899(17) 0.0422(11) Uani 1 1 d . . . H50 H 0.1465 0.7623 0.6816 0.051 Uiso 1 1 calc R . . C51 C 0.0589(2) 0.8143(2) 0.62234(18) 0.0454(11) Uani 1 1 d . . . H51 H 0.0760 0.8582 0.6531 0.055 Uiso 1 1 calc R . . C52 C -0.0079(2) 0.8072(2) 0.56073(17) 0.0354(9) Uani 1 1 d . . . H52 H -0.0368 0.8465 0.5496 0.042 Uiso 1 1 calc R . . C53 C -0.1337(2) 0.82582(18) 0.42205(15) 0.0242(8) Uani 1 1 d . . . C54 C -0.0635(2) 0.86843(19) 0.41573(18) 0.0346(9) Uani 1 1 d . . . H54 H -0.0138 0.8490 0.4213 0.042 Uiso 1 1 calc R . . C55 C -0.0652(3) 0.9385(2) 0.4014(2) 0.0517(11) Uani 1 1 d . . . H55 H -0.0164 0.9674 0.3981 0.062 Uiso 1 1 calc R . . C56 C -0.1377(3) 0.9667(2) 0.3919(2) 0.0635(14) Uani 1 1 d . . . H56 H -0.1391 1.0149 0.3817 0.076 Uiso 1 1 calc R . . C57 C -0.2074(3) 0.9249(2) 0.3972(2) 0.0515(12) Uani 1 1 d . . . H57 H -0.2575 0.9442 0.3900 0.062 Uiso 1 1 calc R . . C58 C -0.2062(2) 0.8550(2) 0.41292(17) 0.0357(9) Uani 1 1 d . . . H58 H -0.2546 0.8270 0.4175 0.043 Uiso 1 1 calc R . . C59 C -0.2100(2) 0.69932(19) 0.46955(15) 0.0236(8) Uani 1 1 d . . . C60 C -0.2536(2) 0.62833(19) 0.45075(17) 0.0281(8) Uani 1 1 d . . . H60 H -0.2452 0.5980 0.4164 0.034 Uiso 1 1 calc R . . C61 C -0.3094(2) 0.6010(2) 0.48166(19) 0.0398(10) Uani 1 1 d . . . H61 H -0.3383 0.5519 0.4689 0.048 Uiso 1 1 calc R . . C62 C -0.3233(2) 0.6445(2) 0.5305(2) 0.0463(11) Uani 1 1 d . . . H62 H -0.3624 0.6256 0.5509 0.056 Uiso 1 1 calc R . . C63 C -0.2806(2) 0.7152(2) 0.55003(19) 0.0464(11) Uani 1 1 d . . . H63 H -0.2905 0.7453 0.5837 0.056 Uiso 1 1 calc R . . C64 C -0.2229(2) 0.7431(2) 0.52059(17) 0.0370(10) Uani 1 1 d . . . H64 H -0.1924 0.7916 0.5351 0.044 Uiso 1 1 calc R . . C65 C 0.76277(18) 0.89640(17) 0.91885(15) 0.0181(7) Uani 1 1 d . . . C66 C 0.77447(19) 0.97193(17) 0.95155(14) 0.0173(7) Uani 1 1 d . . . C67 C 0.7686(2) 0.80922(18) 0.82984(16) 0.0280(8) Uani 1 1 d . . . H67A H 0.7636 0.7745 0.8620 0.034 Uiso 1 1 calc R . . H67B H 0.8242 0.8103 0.8247 0.034 Uiso 1 1 calc R . . C68 C 0.6981(2) 0.78402(19) 0.76095(16) 0.0337(9) Uani 1 1 d . . . H68A H 0.6427 0.7768 0.7670 0.040 Uiso 1 1 calc R . . H68B H 0.7049 0.7368 0.7414 0.040 Uiso 1 1 calc R . . C69 C 0.6991(2) 0.83899(19) 0.71149(17) 0.0353(9) Uani 1 1 d . . . H69A H 0.7518 0.8423 0.7013 0.042 Uiso 1 1 calc R . . H69B H 0.6502 0.8228 0.6680 0.042 Uiso 1 1 calc R . . C70 C 0.6946(2) 0.91271(19) 0.74232(15) 0.0317(9) Uani 1 1 d . . . H70A H 0.6396 0.9102 0.7488 0.038 Uiso 1 1 calc R . . H70B H 0.6978 0.9485 0.7106 0.038 Uiso 1 1 calc R . . C71 C 0.7668(2) 0.93725(18) 0.81079(15) 0.0255(8) Uani 1 1 d . . . H71A H 0.8218 0.9437 0.8039 0.031 Uiso 1 1 calc R . . H71B H 0.7615 0.9845 0.8312 0.031 Uiso 1 1 calc R . . C72 C 0.6230(2) 0.96725(19) 0.88228(16) 0.0303(9) Uani 1 1 d . . . H72A H 0.6242 0.9165 0.8673 0.036 Uiso 1 1 calc R . . H72B H 0.6098 0.9931 0.8416 0.036 Uiso 1 1 calc R . . C73 C 0.5545(2) 0.9682(2) 0.91255(19) 0.0393(10) Uani 1 1 d . . . H73A H 0.5651 0.9387 0.9508 0.047 Uiso 1 1 calc R . . H73B H 0.4986 0.9461 0.8772 0.047 Uiso 1 1 calc R . . C74 C 0.5525(2) 1.0451(2) 0.93870(19) 0.0406(10) Uani 1 1 d . . . H74A H 0.5104 1.0439 0.9614 0.049 Uiso 1 1 calc R . . H74B H 0.5353 1.0732 0.8998 0.049 Uiso 1 1 calc R . . C75 C 0.6402(2) 1.0817(2) 0.98952(18) 0.0364(9) Uani 1 1 d . . . H75A H 0.6397 1.1331 1.0028 0.044 Uiso 1 1 calc R . . H75B H 0.6534 1.0577 1.0313 0.044 Uiso 1 1 calc R . . C76 C 0.7092(2) 1.07810(18) 0.95970(17) 0.0299(8) Uani 1 1 d . . . H76A H 0.7008 1.1081 0.9220 0.036 Uiso 1 1 calc R . . H76B H 0.7654 1.0983 0.9955 0.036 Uiso 1 1 calc R . . C77 C 0.9112(2) 1.14895(19) 0.95021(16) 0.0251(8) Uani 1 1 d . . . C78 C 0.9249(3) 1.2161(2) 0.92192(19) 0.0470(11) Uani 1 1 d . . . H78A H 0.9335 1.2576 0.9562 0.056 Uiso 1 1 calc R . . H78B H 0.8752 1.2172 0.8812 0.056 Uiso 1 1 calc R . . H78C H 0.9753 1.2187 0.9093 0.056 Uiso 1 1 calc R . . C79 C 0.79786(19) 1.01718(19) 1.14010(16) 0.0231(8) Uani 1 1 d . . . C80 C 0.7372(2) 0.95806(18) 1.10153(16) 0.0256(8) Uani 1 1 d . . . H80 H 0.7394 0.9378 1.0595 0.031 Uiso 1 1 calc R . . C81 C 0.6731(2) 0.9277(2) 1.12310(19) 0.0372(9) Uani 1 1 d . . . H81 H 0.6321 0.8866 1.0963 0.045 Uiso 1 1 calc R . . C82 C 0.6691(2) 0.9573(3) 1.1834(2) 0.0520(12) Uani 1 1 d . . . H82 H 0.6250 0.9369 1.1981 0.062 Uiso 1 1 calc R . . C83 C 0.7292(3) 1.0169(3) 1.2226(2) 0.0530(12) Uani 1 1 d . . . H83 H 0.7260 1.0377 1.2640 0.064 Uiso 1 1 calc R . . C84 C 0.7938(2) 1.0460(2) 1.20167(17) 0.0389(10) Uani 1 1 d . . . H84 H 0.8358 1.0861 1.2294 0.047 Uiso 1 1 calc R . . C85 C 0.97574(19) 1.05565(18) 1.19148(15) 0.0222(8) Uani 1 1 d . . . C86 C 1.0098(2) 0.99328(19) 1.20303(16) 0.0273(8) Uani 1 1 d . . . H86 H 0.9882 0.9522 1.1686 0.033 Uiso 1 1 calc R . . C87 C 1.0749(2) 0.9898(2) 1.26423(18) 0.0379(10) Uani 1 1 d . . . H87 H 1.0971 0.9465 1.2715 0.046 Uiso 1 1 calc R . . C88 C 1.1069(2) 1.0493(2) 1.31414(18) 0.0407(10) Uani 1 1 d . . . H88 H 1.1511 1.0473 1.3561 0.049 Uiso 1 1 calc R . . C89 C 1.0745(2) 1.1115(2) 1.30301(18) 0.0420(10) Uani 1 1 d . . . H89 H 1.0970 1.1526 1.3374 0.050 Uiso 1 1 calc R . . C90 C 1.0093(2) 1.1152(2) 1.24221(16) 0.0329(9) Uani 1 1 d . . . H90 H 0.9876 1.1587 1.2354 0.039 Uiso 1 1 calc R . . C91 C 0.8820(2) 1.15264(18) 1.11448(15) 0.0238(8) Uani 1 1 d . . . C92 C 0.9502(2) 1.19832(19) 1.10829(16) 0.0324(9) Uani 1 1 d . . . H92 H 0.9971 1.1791 1.1051 0.039 Uiso 1 1 calc R . . C93 C 0.9502(3) 1.2716(2) 1.10670(19) 0.0485(11) Uani 1 1 d . . . H93 H 0.9972 1.3024 1.1026 0.058 Uiso 1 1 calc R . . C94 C 0.8821(3) 1.3001(2) 1.1110(2) 0.0602(13) Uani 1 1 d . . . H94 H 0.8819 1.3505 1.1098 0.072 Uiso 1 1 calc R . . C95 C 0.8152(3) 1.2554(2) 1.1171(2) 0.0593(13) Uani 1 1 d . . . H95 H 0.7683 1.2748 1.1200 0.071 Uiso 1 1 calc R . . C96 C 0.8145(2) 1.1825(2) 1.11915(18) 0.0368(9) Uani 1 1 d . . . H96 H 0.7674 1.1523 1.1238 0.044 Uiso 1 1 calc R . . C97 C 0.4658(4) 0.8960(3) 0.2807(3) 0.0920(18) Uiso 1 1 d . . . H97A H 0.4101 0.9112 0.2633 0.110 Uiso 1 1 calc R . . H97B H 0.4636 0.8626 0.3145 0.110 Uiso 1 1 calc R . . Cl13 Cl 0.48118(8) 0.84970(8) 0.21325(7) 0.0789(4) Uani 1 1 d U . . Cl14 Cl 0.53913(13) 0.96755(13) 0.31920(14) 0.2151(15) Uani 1 1 d U . . C98 C 0.5679(3) 0.9289(2) 0.5184(2) 0.0553(12) Uiso 1 1 d . . . H98A H 0.5258 0.9296 0.4723 0.066 Uiso 1 1 calc R . . H98B H 0.5940 0.9797 0.5393 0.066 Uiso 1 1 calc R . . Cl15 Cl 0.64618(10) 0.88327(9) 0.51080(10) 0.1072(6) Uani 1 1 d U . . Cl16 Cl 0.51653(7) 0.88728(7) 0.56851(6) 0.0680(4) Uani 1 1 d U . . C99 C 0.4726(4) 0.6195(3) 0.6321(3) 0.0896(18) Uiso 1 1 d . . . H99A H 0.4099 0.6114 0.6108 0.108 Uiso 1 1 calc R . . H99B H 0.4878 0.6230 0.6823 0.108 Uiso 1 1 calc R . . Cl17 Cl 0.51453(8) 0.69961(7) 0.61292(7) 0.0794(4) Uani 1 1 d U . . Cl18 Cl 0.50714(11) 0.54673(8) 0.60462(13) 0.1436(9) Uani 1 1 d U . . C100 C 0.4164(3) 0.7765(3) 0.7738(2) 0.0685(14) Uiso 1 1 d . . . H10C H 0.4583 0.7702 0.8183 0.082 Uiso 1 1 calc R . . H10D H 0.3964 0.7289 0.7444 0.082 Uiso 1 1 calc R . . Cl19 Cl 0.46434(9) 0.83751(10) 0.73576(7) 0.1037(6) Uani 1 1 d U . . Cl20 Cl 0.33141(9) 0.80510(12) 0.78722(8) 0.1284(8) Uani 1 1 d U . . C101 C 0.5962(4) 0.6002(4) 0.8667(4) 0.133(3) Uiso 1 1 d . . . H10E H 0.6194 0.6431 0.9025 0.160 Uiso 1 1 calc R . . H10F H 0.5472 0.6120 0.8301 0.160 Uiso 1 1 calc R . . Cl21 Cl 0.44787(9) 0.76418(9) 0.97059(9) 0.1021(5) Uani 1 1 d U . . Cl22 Cl 0.52169(13) 0.70301(17) 1.09074(10) 0.1968(14) Uani 1 1 d U . . C102 C 0.5229(3) 0.7140(2) 1.0124(2) 0.0582(12) Uiso 1 1 d . . . H10G H 0.5108 0.6658 0.9849 0.070 Uiso 1 1 calc R . . H10H H 0.5800 0.7392 1.0166 0.070 Uiso 1 1 calc R . . Cl23 Cl 0.67406(16) 0.59075(11) 0.83171(12) 0.1601(9) Uani 1 1 d U . . Cl24 Cl 0.56006(10) 0.53549(9) 0.89971(7) 0.1024(5) Uani 1 1 d U . . 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 0.01479(13) 0.01454(13) 0.01235(13) 0.00140(10) 0.00586(11) 0.00144(11) Ru2 0.01550(13) 0.01610(14) 0.01303(13) 0.00202(10) 0.00661(11) 0.00203(11) Ru3 0.01546(13) 0.01694(14) 0.01357(12) 0.00206(10) 0.00661(10) 0.00179(11) Pd1 0.01972(13) 0.01595(13) 0.02004(13) 0.00248(10) 0.00703(11) 0.00078(11) Pd2 0.02550(15) 0.01861(14) 0.02951(15) 0.00687(11) 0.01389(12) 0.00287(12) Pd3 0.02005(14) 0.01796(14) 0.02603(14) 0.00617(11) 0.00902(11) 0.00249(11) Cl1 0.0267(5) 0.0415(6) 0.0313(5) -0.0025(4) 0.0068(4) -0.0128(4) Cl2 0.0389(5) 0.0298(5) 0.0334(5) 0.0155(4) 0.0123(4) 0.0007(4) Cl3 0.0191(4) 0.0184(4) 0.0190(4) 0.0043(3) 0.0044(3) 0.0028(3) Cl4 0.0181(4) 0.0266(4) 0.0162(4) -0.0028(3) 0.0087(3) -0.0005(3) Cl5 0.0169(4) 0.0278(5) 0.0171(4) -0.0049(3) 0.0078(3) -0.0001(3) Cl6 0.0224(4) 0.0231(4) 0.0221(4) 0.0080(3) 0.0097(3) 0.0060(4) Cl7 0.0386(6) 0.0378(6) 0.0476(6) 0.0044(5) 0.0134(5) -0.0157(5) Cl8 0.0463(6) 0.0400(6) 0.0568(6) 0.0319(5) 0.0236(5) 0.0111(5) Cl9 0.0254(5) 0.0392(6) 0.0424(6) 0.0100(4) 0.0040(4) -0.0082(4) Cl10 0.0374(5) 0.0345(5) 0.0541(6) 0.0277(5) 0.0166(5) 0.0069(4) Cl11 0.0197(4) 0.0213(4) 0.0227(4) 0.0070(3) 0.0071(3) 0.0042(3) Cl12 0.0173(4) 0.0303(5) 0.0158(4) -0.0026(3) 0.0070(3) -0.0002(4) N1 0.0204(15) 0.0223(15) 0.0192(14) 0.0016(12) 0.0047(12) 0.0065(12) N2 0.0173(14) 0.0215(15) 0.0194(14) -0.0003(12) 0.0065(12) 0.0009(12) N3 0.0177(15) 0.0245(16) 0.0209(14) 0.0011(12) 0.0038(12) 0.0035(12) N4 0.0200(15) 0.0187(15) 0.0231(15) -0.0019(12) 0.0096(12) -0.0013(12) N5 0.0224(15) 0.0234(16) 0.0166(14) 0.0020(12) 0.0076(12) 0.0013(13) N6 0.0182(15) 0.0241(16) 0.0166(14) 0.0016(12) 0.0046(12) 0.0006(12) N7 0.0185(14) 0.0193(15) 0.0195(14) 0.0020(12) 0.0050(12) 0.0000(12) N8 0.0188(15) 0.0208(15) 0.0212(14) 0.0028(12) 0.0043(12) 0.0039(12) N9 0.0209(15) 0.0237(16) 0.0162(14) -0.0001(12) 0.0064(12) -0.0010(13) P1 0.0203(4) 0.0169(4) 0.0155(4) 0.0002(3) 0.0076(4) 0.0021(4) P2 0.0181(4) 0.0232(5) 0.0159(4) 0.0005(4) 0.0079(4) 0.0040(4) P3 0.0184(4) 0.0221(5) 0.0160(4) 0.0011(3) 0.0080(4) 0.0037(4) C1 0.0087(15) 0.0205(17) 0.0160(16) -0.0018(13) 0.0015(13) 0.0010(13) C2 0.0155(16) 0.0200(17) 0.0105(15) 0.0035(13) 0.0058(13) 0.0023(14) C3 0.0267(19) 0.034(2) 0.0167(17) -0.0002(15) 0.0085(15) -0.0026(16) C4 0.031(2) 0.045(2) 0.0162(18) -0.0042(16) 0.0044(16) -0.0020(18) C5 0.038(2) 0.053(3) 0.026(2) -0.0133(19) 0.0104(18) -0.003(2) C6 0.039(2) 0.032(2) 0.037(2) -0.0179(18) 0.0152(18) -0.0046(18) C7 0.027(2) 0.026(2) 0.031(2) -0.0059(16) 0.0119(16) 0.0058(16) C8 0.0195(18) 0.032(2) 0.0252(19) -0.0017(16) -0.0009(15) 0.0066(16) C9 0.0191(19) 0.042(2) 0.040(2) -0.0039(18) 0.0066(17) 0.0045(17) C10 0.028(2) 0.051(3) 0.043(2) 0.001(2) 0.0090(18) 0.016(2) C11 0.031(2) 0.039(2) 0.043(2) -0.0019(19) 0.0065(18) 0.0191(19) C12 0.027(2) 0.025(2) 0.0303(19) 0.0053(16) 0.0050(16) 0.0103(16) C13 0.0177(17) 0.0203(17) 0.0154(16) 0.0064(13) 0.0106(13) 0.0021(14) C14 0.0117(16) 0.0237(18) 0.0183(17) -0.0013(14) 0.0039(13) -0.0022(14) C15 0.0250(19) 0.026(2) 0.0304(19) 0.0021(16) 0.0035(16) 0.0124(16) C16 0.026(2) 0.040(2) 0.038(2) -0.0033(18) 0.0066(17) 0.0137(18) C17 0.026(2) 0.055(3) 0.041(2) 0.000(2) 0.0129(18) 0.016(2) C18 0.021(2) 0.048(3) 0.045(2) 0.000(2) 0.0111(18) 0.0016(18) C19 0.0192(18) 0.032(2) 0.029(2) -0.0057(16) 0.0002(15) 0.0020(16) C20 0.029(2) 0.032(2) 0.0182(17) 0.0022(15) 0.0069(15) -0.0046(16) C21 0.035(2) 0.049(3) 0.0203(19) 0.0001(17) 0.0059(17) -0.0027(19) C22 0.044(3) 0.058(3) 0.025(2) -0.013(2) 0.0049(18) 0.000(2) C23 0.053(3) 0.033(2) 0.039(2) -0.0161(19) 0.012(2) 0.001(2) C24 0.031(2) 0.030(2) 0.036(2) -0.0068(17) 0.0140(17) 0.0069(17) C25 0.033(2) 0.031(2) 0.0190(18) 0.0078(16) 0.0114(16) 0.0025(17) C26 0.078(3) 0.042(3) 0.040(2) 0.024(2) 0.023(2) 0.006(2) C27 0.030(2) 0.027(2) 0.0224(18) 0.0070(16) 0.0085(16) 0.0027(17) C28 0.092(4) 0.045(3) 0.048(3) 0.027(2) 0.026(3) 0.011(3) C29 0.0171(17) 0.029(2) 0.0168(17) 0.0014(14) 0.0061(14) 0.0039(15) C30 0.027(2) 0.031(2) 0.035(2) 0.0012(17) 0.0167(17) 0.0047(17) C31 0.038(2) 0.034(2) 0.060(3) 0.002(2) 0.031(2) -0.0014(19) C32 0.023(2) 0.071(3) 0.041(2) 0.003(2) 0.0226(18) -0.002(2) C33 0.045(3) 0.069(3) 0.045(3) -0.025(2) 0.030(2) -0.010(2) C34 0.038(2) 0.046(3) 0.045(2) -0.023(2) 0.026(2) -0.018(2) C35 0.035(2) 0.0212(19) 0.0163(17) -0.0023(14) 0.0043(15) 0.0028(16) C36 0.048(3) 0.028(2) 0.045(2) -0.0028(18) 0.011(2) 0.015(2) C37 0.081(4) 0.035(3) 0.070(3) 0.003(2) 0.006(3) 0.029(3) C38 0.117(5) 0.022(2) 0.060(3) 0.011(2) 0.010(3) 0.021(3) C39 0.086(4) 0.028(2) 0.040(3) 0.0034(19) 0.020(2) -0.011(2) C40 0.054(3) 0.023(2) 0.026(2) 0.0000(16) 0.0116(18) 0.0013(19) C41 0.0184(17) 0.0240(18) 0.0163(16) -0.0002(14) 0.0106(14) -0.0003(15) C42 0.0280(19) 0.0231(19) 0.0195(17) 0.0010(14) 0.0096(15) -0.0006(16) C43 0.029(2) 0.038(2) 0.0229(19) 0.0071(17) 0.0075(16) 0.0044(18) C44 0.027(2) 0.050(3) 0.0196(19) -0.0002(18) 0.0009(16) 0.0004(19) C45 0.038(2) 0.040(2) 0.0235(19) -0.0080(17) 0.0062(17) -0.0021(19) C46 0.031(2) 0.027(2) 0.0249(19) -0.0026(15) 0.0088(16) 0.0051(17) C47 0.0179(17) 0.038(2) 0.0139(16) 0.0040(15) 0.0060(14) 0.0033(16) C48 0.028(2) 0.038(2) 0.0215(18) 0.0058(16) 0.0134(16) 0.0024(17) C49 0.027(2) 0.057(3) 0.026(2) 0.0155(19) 0.0097(17) 0.008(2) C50 0.025(2) 0.078(3) 0.0157(19) 0.005(2) 0.0018(16) 0.000(2) C51 0.035(2) 0.067(3) 0.025(2) -0.014(2) 0.0063(18) 0.002(2) C52 0.033(2) 0.044(2) 0.025(2) -0.0087(17) 0.0077(17) 0.0081(19) C53 0.030(2) 0.0222(19) 0.0204(18) 0.0002(14) 0.0090(15) 0.0070(16) C54 0.039(2) 0.026(2) 0.042(2) 0.0007(17) 0.0191(19) 0.0041(18) C55 0.063(3) 0.029(2) 0.065(3) 0.004(2) 0.028(2) 0.002(2) C56 0.087(4) 0.026(2) 0.081(4) 0.008(2) 0.030(3) 0.020(3) C57 0.061(3) 0.035(3) 0.058(3) -0.003(2) 0.014(2) 0.027(2) C58 0.038(2) 0.031(2) 0.038(2) -0.0071(17) 0.0133(18) 0.0111(19) C59 0.0191(18) 0.035(2) 0.0176(17) 0.0053(15) 0.0067(14) 0.0065(16) C60 0.027(2) 0.034(2) 0.0289(19) 0.0045(16) 0.0147(16) 0.0095(17) C61 0.036(2) 0.041(2) 0.051(3) 0.012(2) 0.028(2) 0.0028(19) C62 0.035(2) 0.071(3) 0.046(3) 0.019(2) 0.030(2) 0.009(2) C63 0.045(3) 0.067(3) 0.038(2) -0.004(2) 0.029(2) 0.011(2) C64 0.034(2) 0.050(3) 0.029(2) -0.0063(18) 0.0184(18) 0.0016(19) C65 0.0102(16) 0.0208(18) 0.0196(17) -0.0007(14) 0.0033(13) -0.0008(14) C66 0.0207(17) 0.0196(17) 0.0151(16) 0.0068(13) 0.0101(14) 0.0031(14) C67 0.034(2) 0.0232(19) 0.0258(19) -0.0024(15) 0.0095(16) 0.0084(16) C68 0.037(2) 0.028(2) 0.029(2) -0.0090(16) 0.0075(17) 0.0026(18) C69 0.033(2) 0.041(2) 0.0213(19) -0.0112(17) 0.0020(16) -0.0006(18) C70 0.034(2) 0.035(2) 0.0156(17) 0.0033(15) 0.0010(16) -0.0046(17) C71 0.0282(19) 0.0255(19) 0.0178(17) 0.0027(15) 0.0065(15) -0.0052(16) C72 0.0211(19) 0.033(2) 0.0277(19) 0.0010(16) -0.0011(15) 0.0047(16) C73 0.020(2) 0.047(3) 0.046(2) -0.001(2) 0.0067(18) 0.0066(18) C74 0.025(2) 0.055(3) 0.045(2) 0.009(2) 0.0101(18) 0.022(2) C75 0.035(2) 0.035(2) 0.040(2) 0.0011(18) 0.0116(18) 0.0181(19) C76 0.030(2) 0.023(2) 0.033(2) 0.0015(16) 0.0053(16) 0.0116(16) C77 0.028(2) 0.024(2) 0.0181(17) 0.0038(15) 0.0053(15) -0.0015(16) C78 0.065(3) 0.032(2) 0.036(2) 0.0171(19) 0.012(2) -0.004(2) C79 0.0179(18) 0.036(2) 0.0202(17) 0.0090(15) 0.0099(14) 0.0096(16) C80 0.0234(19) 0.032(2) 0.0239(18) 0.0094(16) 0.0101(15) 0.0075(16) C81 0.026(2) 0.045(2) 0.044(2) 0.015(2) 0.0172(18) 0.0026(18) C82 0.029(2) 0.084(4) 0.054(3) 0.026(3) 0.028(2) 0.007(2) C83 0.039(3) 0.092(4) 0.036(2) 0.004(2) 0.026(2) 0.009(3) C84 0.034(2) 0.059(3) 0.026(2) -0.0009(19) 0.0175(18) 0.003(2) C85 0.0191(18) 0.034(2) 0.0165(17) 0.0028(15) 0.0093(14) 0.0063(16) C86 0.028(2) 0.037(2) 0.0194(18) 0.0059(16) 0.0100(15) 0.0080(17) C87 0.030(2) 0.058(3) 0.031(2) 0.019(2) 0.0115(18) 0.019(2) C88 0.026(2) 0.073(3) 0.022(2) 0.010(2) 0.0057(17) 0.012(2) C89 0.034(2) 0.063(3) 0.023(2) -0.0072(19) 0.0076(17) 0.005(2) C90 0.030(2) 0.044(2) 0.0219(19) -0.0052(17) 0.0072(16) 0.0088(18) C91 0.0286(19) 0.0217(18) 0.0153(16) -0.0057(14) 0.0043(15) 0.0008(16) C92 0.039(2) 0.028(2) 0.0260(19) -0.0047(16) 0.0113(17) 0.0011(18) C93 0.066(3) 0.028(2) 0.040(2) -0.0061(19) 0.016(2) -0.008(2) C94 0.074(4) 0.025(2) 0.074(3) 0.000(2) 0.018(3) 0.011(3) C95 0.053(3) 0.033(3) 0.081(3) -0.007(2) 0.010(3) 0.018(2) C96 0.033(2) 0.030(2) 0.042(2) -0.0064(18) 0.0088(18) 0.0080(18) Cl13 0.0717(9) 0.0799(10) 0.0857(9) 0.0152(8) 0.0409(8) -0.0144(7) Cl14 0.1252(17) 0.191(2) 0.300(3) -0.168(2) 0.132(2) -0.0884(16) Cl15 0.0899(11) 0.0896(12) 0.1859(17) 0.0398(12) 0.0867(12) 0.0490(10) Cl16 0.0432(7) 0.0903(10) 0.0633(8) 0.0113(7) 0.0110(6) 0.0107(7) Cl17 0.0696(9) 0.0509(8) 0.0788(9) -0.0080(7) -0.0138(7) 0.0017(7) Cl18 0.1030(13) 0.0632(10) 0.320(3) 0.0810(14) 0.1228(16) 0.0432(10) Cl19 0.0647(9) 0.1544(16) 0.0580(9) 0.0154(9) -0.0046(7) -0.0152(10) Cl20 0.0621(10) 0.240(2) 0.0898(11) -0.0054(13) 0.0249(8) 0.0688(13) Cl21 0.0765(10) 0.1064(13) 0.1477(15) 0.0471(11) 0.0496(10) 0.0530(10) Cl22 0.1329(17) 0.415(4) 0.1235(15) 0.161(2) 0.0951(14) 0.115(2) Cl23 0.227(3) 0.1188(17) 0.228(2) 0.0541(16) 0.175(2) 0.0754(17) Cl24 0.0977(12) 0.1210(14) 0.0539(8) -0.0094(8) 0.0066(8) -0.0205(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 N5 1.981(3) . ? Ru1 C2 2.004(3) . ? Ru1 P1 2.3176(8) . ? Ru1 Cl3 2.4511(8) . ? Ru1 Cl5 2.4515(8) . ? Ru1 Cl4 2.4915(8) . ? Ru2 N6 1.996(3) . ? Ru2 C13 2.001(3) . ? Ru2 P2 2.3133(8) . ? Ru2 Cl6 2.4462(8) . ? Ru2 Cl5 2.4695(8) . ? Ru2 Cl4 2.4705(8) . ? Ru3 N9 1.996(3) . ? Ru3 C66 2.010(3) . ? Ru3 P3 2.3124(8) . ? Ru3 Cl11 2.4458(8) . ? Ru3 Cl12 2.4532(8) 2_777 ? Ru3 Cl12 2.4699(8) . ? Pd1 C1 1.947(3) . ? Pd1 Cl1 2.3055(9) . ? Pd1 Cl3 2.3404(8) . ? Pd1 Cl2 2.3740(9) . ? Pd2 C14 1.948(3) . ? Pd2 Cl7 2.3055(9) . ? Pd2 Cl6 2.3416(8) . ? Pd2 Cl8 2.3821(9) . ? Pd3 C65 1.953(3) . ? Pd3 Cl9 2.3045(9) . ? Pd3 Cl11 2.3318(8) . ? Pd3 Cl10 2.3770(9) . ? Cl12 Ru3 2.4531(8) 2_777 ? N1 C2 1.321(4) . ? N1 C12 1.466(4) . ? N1 C8 1.486(4) . ? N2 C1 1.297(4) . ? N2 C7 1.475(4) . ? N2 C3 1.494(4) . ? N3 C13 1.319(4) . ? N3 C15 1.466(4) . ? N3 C19 1.492(4) . ? N4 C14 1.300(4) . ? N4 C24 1.477(4) . ? N4 C20 1.487(4) . ? N5 C25 1.136(4) . ? N6 C27 1.127(4) . ? N7 C65 1.296(4) . ? N7 C67 1.478(4) . ? N7 C71 1.493(4) . ? N8 C66 1.311(4) . ? N8 C76 1.480(4) . ? N8 C72 1.488(4) . ? N9 C77 1.134(4) . ? P1 C29 1.825(3) . ? P1 C35 1.844(3) . ? P1 C41 1.846(3) . ? P2 C59 1.832(3) . ? P2 C53 1.841(3) . ? P2 C47 1.852(3) . ? P3 C91 1.836(3) . ? P3 C79 1.839(3) . ? P3 C85 1.852(3) . ? C1 C2 1.478(4) . ? C3 C4 1.521(4) . ? C4 C5 1.525(5) . ? C5 C6 1.517(5) . ? C6 C7 1.510(4) . ? C8 C9 1.524(4) . ? C9 C10 1.523(5) . ? C10 C11 1.521(5) . ? C11 C12 1.524(5) . ? C13 C14 1.483(4) . ? C15 C16 1.529(5) . ? C16 C17 1.522(5) . ? C17 C18 1.511(5) . ? C18 C19 1.516(5) . ? C20 C21 1.520(4) . ? C21 C22 1.523(5) . ? C22 C23 1.508(5) . ? C23 C24 1.526(5) . ? C25 C26 1.453(5) . ? C27 C28 1.451(5) . ? C29 C30 1.376(4) . ? C29 C34 1.390(4) . ? C30 C31 1.382(5) . ? C31 C32 1.385(5) . ? C32 C33 1.378(5) . ? C33 C34 1.383(5) . ? C35 C40 1.383(5) . ? C35 C36 1.385(5) . ? C36 C37 1.380(5) . ? C37 C38 1.371(7) . ? C38 C39 1.381(6) . ? C39 C40 1.383(5) . ? C41 C46 1.385(4) . ? C41 C42 1.391(4) . ? C42 C43 1.388(4) . ? C43 C44 1.369(5) . ? C44 C45 1.384(5) . ? C45 C46 1.381(4) . ? C47 C48 1.386(5) . ? C47 C52 1.391(4) . ? C48 C49 1.393(4) . ? C49 C50 1.371(5) . ? C50 C51 1.377(5) . ? C51 C52 1.380(5) . ? C53 C54 1.389(5) . ? C53 C58 1.392(4) . ? C54 C55 1.376(5) . ? C55 C56 1.380(6) . ? C56 C57 1.368(6) . ? C57 C58 1.380(5) . ? C59 C60 1.381(5) . ? C59 C64 1.402(4) . ? C60 C61 1.387(5) . ? C61 C62 1.373(5) . ? C62 C63 1.373(5) . ? C63 C64 1.393(5) . ? C65 C66 1.485(4) . ? C67 C68 1.513(4) . ? C68 C69 1.522(5) . ? C69 C70 1.512(5) . ? C70 C71 1.519(4) . ? C72 C73 1.516(5) . ? C73 C74 1.519(5) . ? C74 C75 1.526(5) . ? C75 C76 1.522(5) . ? C77 C78 1.457(5) . ? C79 C80 1.379(5) . ? C79 C84 1.394(4) . ? C80 C81 1.387(5) . ? C81 C82 1.373(5) . ? C82 C83 1.385(6) . ? C83 C84 1.377(5) . ? C85 C90 1.388(4) . ? C85 C86 1.389(4) . ? C86 C87 1.395(4) . ? C87 C88 1.377(5) . ? C88 C89 1.371(5) . ? C89 C90 1.391(5) . ? C91 C96 1.389(4) . ? C91 C92 1.389(5) . ? C92 C93 1.381(5) . ? C93 C94 1.384(6) . ? C94 C95 1.361(6) . ? C95 C96 1.374(5) . ? C97 Cl14 1.631(6) . ? C97 Cl13 1.727(5) . ? C98 Cl15 1.743(4) . ? C98 Cl16 1.744(4) . ? C99 Cl17 1.704(5) . ? C99 Cl18 1.712(5) . ? C100 Cl19 1.711(5) . ? C100 Cl20 1.726(5) . ? C101 Cl24 1.592(7) . ? C101 Cl23 1.754(7) . ? Cl21 C102 1.740(4) . ? Cl22 C102 1.681(4) . ? 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 N5 Ru1 C2 90.61(11) . . ? N5 Ru1 P1 91.91(8) . . ? C2 Ru1 P1 101.67(9) . . ? N5 Ru1 Cl3 172.69(7) . . ? C2 Ru1 Cl3 87.58(9) . . ? P1 Ru1 Cl3 95.39(3) . . ? N5 Ru1 Cl5 85.97(8) . . ? C2 Ru1 Cl5 92.56(8) . . ? P1 Ru1 Cl5 165.64(3) . . ? Cl3 Ru1 Cl5 87.03(3) . . ? N5 Ru1 Cl4 87.89(8) . . ? C2 Ru1 Cl4 171.09(8) . . ? P1 Ru1 Cl4 87.16(3) . . ? Cl3 Ru1 Cl4 92.81(3) . . ? Cl5 Ru1 Cl4 78.57(2) . . ? N6 Ru2 C13 90.96(11) . . ? N6 Ru2 P2 92.62(7) . . ? C13 Ru2 P2 101.24(9) . . ? N6 Ru2 Cl6 171.94(7) . . ? C13 Ru2 Cl6 86.30(9) . . ? P2 Ru2 Cl6 95.35(3) . . ? N6 Ru2 Cl5 86.96(7) . . ? C13 Ru2 Cl5 173.09(8) . . ? P2 Ru2 Cl5 85.44(3) . . ? Cl6 Ru2 Cl5 94.87(3) . . ? N6 Ru2 Cl4 85.91(7) . . ? C13 Ru2 Cl4 94.65(8) . . ? P2 Ru2 Cl4 164.06(3) . . ? Cl6 Ru2 Cl4 86.76(3) . . ? Cl5 Ru2 Cl4 78.63(2) . . ? N9 Ru3 C66 91.04(11) . . ? N9 Ru3 P3 93.89(7) . . ? C66 Ru3 P3 101.79(9) . . ? N9 Ru3 Cl11 172.68(7) . . ? C66 Ru3 Cl11 88.11(9) . . ? P3 Ru3 Cl11 93.40(3) . . ? N9 Ru3 Cl12 85.74(7) . 2_777 ? C66 Ru3 Cl12 92.66(9) . 2_777 ? P3 Ru3 Cl12 165.54(3) . 2_777 ? Cl11 Ru3 Cl12 87.04(3) . 2_777 ? N9 Ru3 Cl12 86.84(8) . . ? C66 Ru3 Cl12 171.97(9) . . ? P3 Ru3 Cl12 86.09(3) . . ? Cl11 Ru3 Cl12 93.02(3) . . ? Cl12 Ru3 Cl12 79.46(3) 2_777 . ? C1 Pd1 Cl1 89.35(9) . . ? C1 Pd1 Cl3 84.04(8) . . ? Cl1 Pd1 Cl3 173.14(3) . . ? C1 Pd1 Cl2 174.32(9) . . ? Cl1 Pd1 Cl2 91.87(3) . . ? Cl3 Pd1 Cl2 94.90(3) . . ? C14 Pd2 Cl7 89.08(9) . . ? C14 Pd2 Cl6 84.12(9) . . ? Cl7 Pd2 Cl6 172.90(3) . . ? C14 Pd2 Cl8 174.33(9) . . ? Cl7 Pd2 Cl8 91.93(4) . . ? Cl6 Pd2 Cl8 95.04(3) . . ? C65 Pd3 Cl9 87.78(9) . . ? C65 Pd3 Cl11 84.98(9) . . ? Cl9 Pd3 Cl11 172.19(3) . . ? C65 Pd3 Cl10 179.28(9) . . ? Cl9 Pd3 Cl10 92.91(3) . . ? Cl11 Pd3 Cl10 94.34(3) . . ? Pd1 Cl3 Ru1 101.27(3) . . ? Ru2 Cl4 Ru1 100.64(3) . . ? Ru1 Cl5 Ru2 101.80(3) . . ? Pd2 Cl6 Ru2 102.69(3) . . ? Pd3 Cl11 Ru3 101.99(3) . . ? Ru3 Cl12 Ru3 100.54(3) 2_777 . ? C2 N1 C12 123.8(3) . . ? C2 N1 C8 123.4(3) . . ? C12 N1 C8 112.5(2) . . ? C1 N2 C7 122.0(3) . . ? C1 N2 C3 125.3(3) . . ? C7 N2 C3 112.7(2) . . ? C13 N3 C15 123.2(3) . . ? C13 N3 C19 123.0(3) . . ? C15 N3 C19 113.5(2) . . ? C14 N4 C24 122.7(3) . . ? C14 N4 C20 124.6(3) . . ? C24 N4 C20 112.7(3) . . ? C25 N5 Ru1 176.5(3) . . ? C27 N6 Ru2 174.7(3) . . ? C65 N7 C67 122.6(3) . . ? C65 N7 C71 124.5(3) . . ? C67 N7 C71 112.8(2) . . ? C66 N8 C76 123.3(3) . . ? C66 N8 C72 124.4(3) . . ? C76 N8 C72 112.2(2) . . ? C77 N9 Ru3 173.5(3) . . ? C29 P1 C35 105.81(16) . . ? C29 P1 C41 99.04(14) . . ? C35 P1 C41 101.11(15) . . ? C29 P1 Ru1 121.56(11) . . ? C35 P1 Ru1 112.40(11) . . ? C41 P1 Ru1 114.32(10) . . ? C59 P2 C53 106.52(15) . . ? C59 P2 C47 98.79(14) . . ? C53 P2 C47 100.53(15) . . ? C59 P2 Ru2 121.38(11) . . ? C53 P2 Ru2 111.62(10) . . ? C47 P2 Ru2 115.39(11) . . ? C91 P3 C79 104.73(16) . . ? C91 P3 C85 100.73(15) . . ? C79 P3 C85 99.03(14) . . ? C91 P3 Ru3 113.41(10) . . ? C79 P3 Ru3 121.45(11) . . ? C85 P3 Ru3 114.68(10) . . ? N2 C1 C2 121.7(3) . . ? N2 C1 Pd1 126.9(2) . . ? C2 C1 Pd1 111.3(2) . . ? N1 C2 C1 116.4(3) . . ? N1 C2 Ru1 134.5(2) . . ? C1 C2 Ru1 109.02(19) . . ? N2 C3 C4 110.5(3) . . ? C3 C4 C5 110.7(3) . . ? C6 C5 C4 110.2(3) . . ? C7 C6 C5 111.3(3) . . ? N2 C7 C6 110.9(3) . . ? N1 C8 C9 111.3(3) . . ? C10 C9 C8 110.4(3) . . ? C11 C10 C9 109.2(3) . . ? C10 C11 C12 111.2(3) . . ? N1 C12 C11 112.0(3) . . ? N3 C13 C14 115.9(3) . . ? N3 C13 Ru2 135.6(2) . . ? C14 C13 Ru2 108.5(2) . . ? N4 C14 C13 120.4(3) . . ? N4 C14 Pd2 127.7(2) . . ? C13 C14 Pd2 111.9(2) . . ? N3 C15 C16 112.2(3) . . ? C17 C16 C15 111.5(3) . . ? C18 C17 C16 109.0(3) . . ? C17 C18 C19 111.1(3) . . ? N3 C19 C18 111.0(3) . . ? N4 C20 C21 110.0(3) . . ? C20 C21 C22 110.7(3) . . ? C23 C22 C21 110.5(3) . . ? C22 C23 C24 111.2(3) . . ? N4 C24 C23 110.3(3) . . ? N5 C25 C26 177.5(4) . . ? N6 C27 C28 178.3(4) . . ? C30 C29 C34 118.3(3) . . ? C30 C29 P1 119.2(2) . . ? C34 C29 P1 122.1(3) . . ? C29 C30 C31 121.0(3) . . ? C30 C31 C32 120.3(4) . . ? C33 C32 C31 119.3(3) . . ? C32 C33 C34 120.1(4) . . ? C33 C34 C29 121.0(4) . . ? C40 C35 C36 118.1(3) . . ? C40 C35 P1 118.1(3) . . ? C36 C35 P1 123.6(3) . . ? C37 C36 C35 120.9(4) . . ? C38 C37 C36 120.0(4) . . ? C37 C38 C39 120.5(4) . . ? C38 C39 C40 118.9(4) . . ? C35 C40 C39 121.7(4) . . ? C46 C41 C42 118.1(3) . . ? C46 C41 P1 122.5(3) . . ? C42 C41 P1 119.4(2) . . ? C43 C42 C41 120.8(3) . . ? C44 C43 C42 120.1(3) . . ? C43 C44 C45 120.1(3) . . ? C46 C45 C44 119.7(3) . . ? C45 C46 C41 121.3(3) . . ? C48 C47 C52 118.0(3) . . ? C48 C47 P2 120.3(3) . . ? C52 C47 P2 121.6(3) . . ? C47 C48 C49 121.1(3) . . ? C50 C49 C48 119.4(4) . . ? C49 C50 C51 120.6(3) . . ? C50 C51 C52 119.7(4) . . ? C51 C52 C47 121.2(4) . . ? C54 C53 C58 118.7(3) . . ? C54 C53 P2 117.4(3) . . ? C58 C53 P2 123.6(3) . . ? C55 C54 C53 120.7(4) . . ? C54 C55 C56 120.0(4) . . ? C57 C56 C55 119.7(4) . . ? C56 C57 C58 121.0(4) . . ? C57 C58 C53 119.8(4) . . ? C60 C59 C64 118.9(3) . . ? C60 C59 P2 119.3(3) . . ? C64 C59 P2 121.4(3) . . ? C59 C60 C61 120.4(3) . . ? C62 C61 C60 120.5(4) . . ? C61 C62 C63 120.0(4) . . ? C62 C63 C64 120.3(4) . . ? C63 C64 C59 119.8(4) . . ? N7 C65 C66 121.9(3) . . ? N7 C65 Pd3 124.8(2) . . ? C66 C65 Pd3 113.0(2) . . ? N8 C66 C65 116.6(3) . . ? N8 C66 Ru3 134.9(2) . . ? C65 C66 Ru3 108.5(2) . . ? N7 C67 C68 111.0(3) . . ? C67 C68 C69 111.3(3) . . ? C70 C69 C68 110.2(3) . . ? C69 C70 C71 110.7(3) . . ? N7 C71 C70 110.1(3) . . ? N8 C72 C73 110.8(3) . . ? C72 C73 C74 111.3(3) . . ? C73 C74 C75 109.9(3) . . ? C76 C75 C74 112.0(3) . . ? N8 C76 C75 111.3(3) . . ? N9 C77 C78 177.2(4) . . ? C80 C79 C84 118.7(3) . . ? C80 C79 P3 120.5(2) . . ? C84 C79 P3 120.8(3) . . ? C79 C80 C81 121.0(3) . . ? C82 C81 C80 119.7(4) . . ? C81 C82 C83 120.1(4) . . ? C84 C83 C82 120.0(4) . . ? C83 C84 C79 120.5(4) . . ? C90 C85 C86 118.2(3) . . ? C90 C85 P3 122.2(3) . . ? C86 C85 P3 119.5(2) . . ? C85 C86 C87 121.3(3) . . ? C88 C87 C86 119.6(4) . . ? C89 C88 C87 119.7(3) . . ? C88 C89 C90 121.0(4) . . ? C85 C90 C89 120.2(4) . . ? C96 C91 C92 118.4(3) . . ? C96 C91 P3 123.7(3) . . ? C92 C91 P3 117.9(3) . . ? C93 C92 C91 120.4(4) . . ? C92 C93 C94 120.3(4) . . ? C95 C94 C93 119.3(4) . . ? C94 C95 C96 121.1(4) . . ? C95 C96 C91 120.5(4) . . ? Cl14 C97 Cl13 114.0(3) . . ? Cl15 C98 Cl16 111.3(2) . . ? Cl17 C99 Cl18 113.2(3) . . ? Cl19 C100 Cl20 111.5(3) . . ? Cl24 C101 Cl23 120.5(4) . . ? Cl22 C102 Cl21 111.2(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 C1 Pd1 Cl3 Ru1 -27.65(9) . . . . ? Cl1 Pd1 Cl3 Ru1 -43.2(3) . . . . ? Cl2 Pd1 Cl3 Ru1 146.74(3) . . . . ? N5 Ru1 Cl3 Pd1 76.2(6) . . . . ? C2 Ru1 Cl3 Pd1 0.38(9) . . . . ? P1 Ru1 Cl3 Pd1 -101.12(3) . . . . ? Cl5 Ru1 Cl3 Pd1 93.07(3) . . . . ? Cl4 Ru1 Cl3 Pd1 171.47(3) . . . . ? N6 Ru2 Cl4 Ru1 92.18(7) . . . . ? C13 Ru2 Cl4 Ru1 -177.19(9) . . . . ? P2 Ru2 Cl4 Ru1 7.01(12) . . . . ? Cl6 Ru2 Cl4 Ru1 -91.16(3) . . . . ? Cl5 Ru2 Cl4 Ru1 4.47(3) . . . . ? N5 Ru1 Cl4 Ru2 81.81(8) . . . . ? C2 Ru1 Cl4 Ru2 1.4(6) . . . . ? P1 Ru1 Cl4 Ru2 173.84(3) . . . . ? Cl3 Ru1 Cl4 Ru2 -90.90(3) . . . . ? Cl5 Ru1 Cl4 Ru2 -4.50(3) . . . . ? N5 Ru1 Cl5 Ru2 -84.13(8) . . . . ? C2 Ru1 Cl5 Ru2 -174.57(9) . . . . ? P1 Ru1 Cl5 Ru2 -2.18(13) . . . . ? Cl3 Ru1 Cl5 Ru2 97.99(3) . . . . ? Cl4 Ru1 Cl5 Ru2 4.52(3) . . . . ? N6 Ru2 Cl5 Ru1 -90.99(8) . . . . ? C13 Ru2 Cl5 Ru1 -18.4(7) . . . . ? P2 Ru2 Cl5 Ru1 176.14(3) . . . . ? Cl6 Ru2 Cl5 Ru1 81.14(3) . . . . ? Cl4 Ru2 Cl5 Ru1 -4.56(3) . . . . ? C14 Pd2 Cl6 Ru2 22.42(9) . . . . ? Cl7 Pd2 Cl6 Ru2 39.2(3) . . . . ? Cl8 Pd2 Cl6 Ru2 -151.95(3) . . . . ? N6 Ru2 Cl6 Pd2 -64.8(5) . . . . ? C13 Ru2 Cl6 Pd2 5.56(9) . . . . ? P2 Ru2 Cl6 Pd2 106.53(3) . . . . ? Cl5 Ru2 Cl6 Pd2 -167.61(3) . . . . ? Cl4 Ru2 Cl6 Pd2 -89.31(3) . . . . ? C65 Pd3 Cl11 Ru3 24.18(9) . . . . ? Cl9 Pd3 Cl11 Ru3 2.0(3) . . . . ? Cl10 Pd3 Cl11 Ru3 -156.05(3) . . . . ? N9 Ru3 Cl11 Pd3 -80.8(6) . . . . ? C66 Ru3 Cl11 Pd3 2.57(9) . . . . ? P3 Ru3 Cl11 Pd3 104.27(3) . . . . ? Cl12 Ru3 Cl11 Pd3 -90.20(3) 2_777 . . . ? Cl12 Ru3 Cl11 Pd3 -169.47(3) . . . . ? N9 Ru3 Cl12 Ru3 -86.25(7) . . . 2_777 ? C66 Ru3 Cl12 Ru3 -11.4(6) . . . 2_777 ? P3 Ru3 Cl12 Ru3 179.63(3) . . . 2_777 ? Cl11 Ru3 Cl12 Ru3 86.42(3) . . . 2_777 ? Cl12 Ru3 Cl12 Ru3 0.000(1) 2_777 . . 2_777 ? C2 Ru1 N5 C25 114(5) . . . . ? P1 Ru1 N5 C25 -144(5) . . . . ? Cl3 Ru1 N5 C25 39(5) . . . . ? Cl5 Ru1 N5 C25 22(5) . . . . ? Cl4 Ru1 N5 C25 -57(5) . . . . ? C13 Ru2 N6 C27 -91(3) . . . . ? P2 Ru2 N6 C27 168(3) . . . . ? Cl6 Ru2 N6 C27 -21(3) . . . . ? Cl5 Ru2 N6 C27 82(3) . . . . ? Cl4 Ru2 N6 C27 4(3) . . . . ? C66 Ru3 N9 C77 -112(2) . . . . ? P3 Ru3 N9 C77 146(2) . . . . ? Cl11 Ru3 N9 C77 -29(3) . . . . ? Cl12 Ru3 N9 C77 -19(2) 2_777 . . . ? Cl12 Ru3 N9 C77 60(2) . . . . ? N5 Ru1 P1 C29 -124.97(14) . . . . ? C2 Ru1 P1 C29 -33.95(15) . . . . ? Cl3 Ru1 P1 C29 54.68(12) . . . . ? Cl5 Ru1 P1 C29 153.82(15) . . . . ? Cl4 Ru1 P1 C29 147.24(12) . . . . ? N5 Ru1 P1 C35 1.82(14) . . . . ? C2 Ru1 P1 C35 92.85(15) . . . . ? Cl3 Ru1 P1 C35 -178.52(12) . . . . ? Cl5 Ru1 P1 C35 -79.39(17) . . . . ? Cl4 Ru1 P1 C35 -85.97(12) . . . . ? N5 Ru1 P1 C41 116.34(13) . . . . ? C2 Ru1 P1 C41 -152.63(14) . . . . ? Cl3 Ru1 P1 C41 -64.00(12) . . . . ? Cl5 Ru1 P1 C41 35.13(18) . . . . ? Cl4 Ru1 P1 C41 28.55(12) . . . . ? N6 Ru2 P2 C59 123.02(14) . . . . ? C13 Ru2 P2 C59 31.52(15) . . . . ? Cl6 Ru2 P2 C59 -55.77(12) . . . . ? Cl5 Ru2 P2 C59 -150.25(12) . . . . ? Cl4 Ru2 P2 C59 -152.74(14) . . . . ? N6 Ru2 P2 C53 -3.86(14) . . . . ? C13 Ru2 P2 C53 -95.36(15) . . . . ? Cl6 Ru2 P2 C53 177.36(12) . . . . ? Cl5 Ru2 P2 C53 82.88(12) . . . . ? Cl4 Ru2 P2 C53 80.38(16) . . . . ? N6 Ru2 P2 C47 -117.80(14) . . . . ? C13 Ru2 P2 C47 150.70(15) . . . . ? Cl6 Ru2 P2 C47 63.42(13) . . . . ? Cl5 Ru2 P2 C47 -31.06(12) . . . . ? Cl4 Ru2 P2 C47 -33.56(18) . . . . ? N9 Ru3 P3 C91 1.46(14) . . . . ? C66 Ru3 P3 C91 -90.42(15) . . . . ? Cl11 Ru3 P3 C91 -179.19(12) . . . . ? Cl12 Ru3 P3 C91 89.48(17) 2_777 . . . ? Cl12 Ru3 P3 C91 88.02(12) . . . . ? N9 Ru3 P3 C79 127.58(14) . . . . ? C66 Ru3 P3 C79 35.70(15) . . . . ? Cl11 Ru3 P3 C79 -53.07(12) . . . . ? Cl12 Ru3 P3 C79 -144.41(15) 2_777 . . . ? Cl12 Ru3 P3 C79 -145.87(12) . . . . ? N9 Ru3 P3 C85 -113.51(14) . . . . ? C66 Ru3 P3 C85 154.61(15) . . . . ? Cl11 Ru3 P3 C85 65.84(13) . . . . ? Cl12 Ru3 P3 C85 -25.49(19) 2_777 . . . ? Cl12 Ru3 P3 C85 -26.95(13) . . . . ? C7 N2 C1 C2 -170.1(3) . . . . ? C3 N2 C1 C2 7.9(4) . . . . ? C7 N2 C1 Pd1 5.7(4) . . . . ? C3 N2 C1 Pd1 -176.4(2) . . . . ? Cl1 Pd1 C1 N2 66.9(3) . . . . ? Cl3 Pd1 C1 N2 -111.2(3) . . . . ? Cl2 Pd1 C1 N2 169.3(7) . . . . ? Cl1 Pd1 C1 C2 -116.9(2) . . . . ? Cl3 Pd1 C1 C2 64.90(19) . . . . ? Cl2 Pd1 C1 C2 -14.5(10) . . . . ? C12 N1 C2 C1 177.7(3) . . . . ? C8 N1 C2 C1 3.2(4) . . . . ? C12 N1 C2 Ru1 0.6(5) . . . . ? C8 N1 C2 Ru1 -173.8(2) . . . . ? N2 C1 C2 N1 -81.3(4) . . . . ? Pd1 C1 C2 N1 102.3(3) . . . . ? N2 C1 C2 Ru1 96.4(3) . . . . ? Pd1 C1 C2 Ru1 -79.9(2) . . . . ? N5 Ru1 C2 N1 43.5(3) . . . . ? P1 Ru1 C2 N1 -48.6(3) . . . . ? Cl3 Ru1 C2 N1 -143.6(3) . . . . ? Cl5 Ru1 C2 N1 129.5(3) . . . . ? Cl4 Ru1 C2 N1 123.7(5) . . . . ? N5 Ru1 C2 C1 -133.7(2) . . . . ? P1 Ru1 C2 C1 134.19(18) . . . . ? Cl3 Ru1 C2 C1 39.19(19) . . . . ? Cl5 Ru1 C2 C1 -47.73(19) . . . . ? Cl4 Ru1 C2 C1 -53.5(7) . . . . ? C1 N2 C3 C4 125.3(3) . . . . ? C7 N2 C3 C4 -56.5(3) . . . . ? N2 C3 C4 C5 55.5(4) . . . . ? C3 C4 C5 C6 -55.5(4) . . . . ? C4 C5 C6 C7 55.7(4) . . . . ? C1 N2 C7 C6 -125.2(3) . . . . ? C3 N2 C7 C6 56.6(4) . . . . ? C5 C6 C7 N2 -55.9(4) . . . . ? C2 N1 C8 C9 -129.7(3) . . . . ? C12 N1 C8 C9 55.3(4) . . . . ? N1 C8 C9 C10 -56.9(4) . . . . ? C8 C9 C10 C11 57.2(4) . . . . ? C9 C10 C11 C12 -56.1(4) . . . . ? C2 N1 C12 C11 130.9(3) . . . . ? C8 N1 C12 C11 -54.1(4) . . . . ? C10 C11 C12 N1 54.9(4) . . . . ? C15 N3 C13 C14 -173.2(3) . . . . ? C19 N3 C13 C14 0.4(4) . . . . ? C15 N3 C13 Ru2 4.9(5) . . . . ? C19 N3 C13 Ru2 178.6(2) . . . . ? N6 Ru2 C13 N3 -49.8(3) . . . . ? P2 Ru2 C13 N3 43.1(3) . . . . ? Cl6 Ru2 C13 N3 137.8(3) . . . . ? Cl5 Ru2 C13 N3 -122.1(7) . . . . ? Cl4 Ru2 C13 N3 -135.7(3) . . . . ? N6 Ru2 C13 C14 128.4(2) . . . . ? P2 Ru2 C13 C14 -138.69(18) . . . . ? Cl6 Ru2 C13 C14 -43.96(19) . . . . ? Cl5 Ru2 C13 C14 56.1(8) . . . . ? Cl4 Ru2 C13 C14 42.5(2) . . . . ? C24 N4 C14 C13 168.6(3) . . . . ? C20 N4 C14 C13 -8.2(4) . . . . ? C24 N4 C14 Pd2 -7.8(4) . . . . ? C20 N4 C14 Pd2 175.3(2) . . . . ? N3 C13 C14 N4 83.6(4) . . . . ? Ru2 C13 C14 N4 -95.0(3) . . . . ? N3 C13 C14 Pd2 -99.4(3) . . . . ? Ru2 C13 C14 Pd2 81.9(2) . . . . ? Cl7 Pd2 C14 N4 -62.6(3) . . . . ? Cl6 Pd2 C14 N4 115.3(3) . . . . ? Cl8 Pd2 C14 N4 -162.9(7) . . . . ? Cl7 Pd2 C14 C13 120.7(2) . . . . ? Cl6 Pd2 C14 C13 -61.4(2) . . . . ? Cl8 Pd2 C14 C13 20.4(11) . . . . ? C13 N3 C15 C16 -134.1(3) . . . . ? C19 N3 C15 C16 51.7(4) . . . . ? N3 C15 C16 C17 -52.9(4) . . . . ? C15 C16 C17 C18 55.7(4) . . . . ? C16 C17 C18 C19 -58.1(4) . . . . ? C13 N3 C19 C18 132.1(3) . . . . ? C15 N3 C19 C18 -53.7(4) . . . . ? C17 C18 C19 N3 56.9(4) . . . . ? C14 N4 C20 C21 -125.0(3) . . . . ? C24 N4 C20 C21 57.9(4) . . . . ? N4 C20 C21 C22 -56.3(4) . . . . ? C20 C21 C22 C23 55.9(4) . . . . ? C21 C22 C23 C24 -55.3(4) . . . . ? C14 N4 C24 C23 125.6(3) . . . . ? C20 N4 C24 C23 -57.2(4) . . . . ? C22 C23 C24 N4 55.5(4) . . . . ? Ru1 N5 C25 C26 126(8) . . . . ? Ru2 N6 C27 C28 -134(12) . . . . ? C35 P1 C29 C30 -141.1(3) . . . . ? C41 P1 C29 C30 114.5(3) . . . . ? Ru1 P1 C29 C30 -11.4(3) . . . . ? C35 P1 C29 C34 45.8(3) . . . . ? C41 P1 C29 C34 -58.6(3) . . . . ? Ru1 P1 C29 C34 175.4(3) . . . . ? C34 C29 C30 C31 0.7(5) . . . . ? P1 C29 C30 C31 -172.7(3) . . . . ? C29 C30 C31 C32 -1.4(6) . . . . ? C30 C31 C32 C33 0.9(6) . . . . ? C31 C32 C33 C34 0.2(6) . . . . ? C32 C33 C34 C29 -1.0(7) . . . . ? C30 C29 C34 C33 0.5(6) . . . . ? P1 C29 C34 C33 173.7(3) . . . . ? C29 P1 C35 C40 -164.5(3) . . . . ? C41 P1 C35 C40 -61.7(3) . . . . ? Ru1 P1 C35 C40 60.7(3) . . . . ? C29 P1 C35 C36 20.7(3) . . . . ? C41 P1 C35 C36 123.5(3) . . . . ? Ru1 P1 C35 C36 -114.1(3) . . . . ? C40 C35 C36 C37 -1.1(5) . . . . ? P1 C35 C36 C37 173.7(3) . . . . ? C35 C36 C37 C38 1.5(7) . . . . ? C36 C37 C38 C39 -0.7(7) . . . . ? C37 C38 C39 C40 -0.6(7) . . . . ? C36 C35 C40 C39 -0.2(5) . . . . ? P1 C35 C40 C39 -175.3(3) . . . . ? C38 C39 C40 C35 1.1(6) . . . . ? C29 P1 C41 C46 87.5(3) . . . . ? C35 P1 C41 C46 -20.7(3) . . . . ? Ru1 P1 C41 C46 -141.7(2) . . . . ? C29 P1 C41 C42 -89.2(3) . . . . ? C35 P1 C41 C42 162.6(3) . . . . ? Ru1 P1 C41 C42 41.6(3) . . . . ? C46 C41 C42 C43 0.3(5) . . . . ? P1 C41 C42 C43 177.2(3) . . . . ? C41 C42 C43 C44 -0.3(5) . . . . ? C42 C43 C44 C45 -0.2(6) . . . . ? C43 C44 C45 C46 0.8(6) . . . . ? C44 C45 C46 C41 -0.8(6) . . . . ? C42 C41 C46 C45 0.2(5) . . . . ? P1 C41 C46 C45 -176.5(3) . . . . ? C59 P2 C47 C48 91.3(3) . . . . ? C53 P2 C47 C48 -160.0(3) . . . . ? Ru2 P2 C47 C48 -39.8(3) . . . . ? C59 P2 C47 C52 -84.2(3) . . . . ? C53 P2 C47 C52 24.6(3) . . . . ? Ru2 P2 C47 C52 144.8(3) . . . . ? C52 C47 C48 C49 0.5(5) . . . . ? P2 C47 C48 C49 -175.1(3) . . . . ? C47 C48 C49 C50 -0.2(5) . . . . ? C48 C49 C50 C51 -0.4(6) . . . . ? C49 C50 C51 C52 0.7(6) . . . . ? C50 C51 C52 C47 -0.3(6) . . . . ? C48 C47 C52 C51 -0.2(5) . . . . ? P2 C47 C52 C51 175.3(3) . . . . ? C59 P2 C53 C54 161.3(3) . . . . ? C47 P2 C53 C54 58.7(3) . . . . ? Ru2 P2 C53 C54 -64.1(3) . . . . ? C59 P2 C53 C58 -24.1(3) . . . . ? C47 P2 C53 C58 -126.7(3) . . . . ? Ru2 P2 C53 C58 110.5(3) . . . . ? C58 C53 C54 C55 0.7(5) . . . . ? P2 C53 C54 C55 175.5(3) . . . . ? C53 C54 C55 C56 -1.3(6) . . . . ? C54 C55 C56 C57 0.5(7) . . . . ? C55 C56 C57 C58 0.8(7) . . . . ? C56 C57 C58 C53 -1.4(6) . . . . ? C54 C53 C58 C57 0.6(5) . . . . ? P2 C53 C58 C57 -173.9(3) . . . . ? C53 P2 C59 C60 144.5(3) . . . . ? C47 P2 C59 C60 -111.6(3) . . . . ? Ru2 P2 C59 C60 15.4(3) . . . . ? C53 P2 C59 C64 -42.7(3) . . . . ? C47 P2 C59 C64 61.1(3) . . . . ? Ru2 P2 C59 C64 -171.9(2) . . . . ? C64 C59 C60 C61 0.3(5) . . . . ? P2 C59 C60 C61 173.3(3) . . . . ? C59 C60 C61 C62 1.1(5) . . . . ? C60 C61 C62 C63 -1.1(6) . . . . ? C61 C62 C63 C64 -0.3(6) . . . . ? C62 C63 C64 C59 1.7(6) . . . . ? C60 C59 C64 C63 -1.7(5) . . . . ? P2 C59 C64 C63 -174.5(3) . . . . ? C67 N7 C65 C66 168.8(3) . . . . ? C71 N7 C65 C66 -8.7(4) . . . . ? C67 N7 C65 Pd3 -5.2(4) . . . . ? C71 N7 C65 Pd3 177.3(2) . . . . ? Cl9 Pd3 C65 N7 -70.4(3) . . . . ? Cl11 Pd3 C65 N7 112.5(3) . . . . ? Cl10 Pd3 C65 N7 94(7) . . . . ? Cl9 Pd3 C65 C66 115.2(2) . . . . ? Cl11 Pd3 C65 C66 -61.9(2) . . . . ? Cl10 Pd3 C65 C66 -81(7) . . . . ? C76 N8 C66 C65 -178.2(3) . . . . ? C72 N8 C66 C65 -1.0(4) . . . . ? C76 N8 C66 Ru3 -1.1(5) . . . . ? C72 N8 C66 Ru3 176.0(2) . . . . ? N7 C65 C66 N8 81.4(4) . . . . ? Pd3 C65 C66 N8 -104.0(3) . . . . ? N7 C65 C66 Ru3 -96.4(3) . . . . ? Pd3 C65 C66 Ru3 78.2(2) . . . . ? N9 Ru3 C66 N8 -44.6(3) . . . . ? P3 Ru3 C66 N8 49.6(3) . . . . ? Cl11 Ru3 C66 N8 142.7(3) . . . . ? Cl12 Ru3 C66 N8 -130.4(3) 2_777 . . . ? Cl12 Ru3 C66 N8 -119.2(6) . . . . ? N9 Ru3 C66 C65 132.6(2) . . . . ? P3 Ru3 C66 C65 -133.17(19) . . . . ? Cl11 Ru3 C66 C65 -40.09(19) . . . . ? Cl12 Ru3 C66 C65 46.9(2) 2_777 . . . ? Cl12 Ru3 C66 C65 58.1(7) . . . . ? C65 N7 C67 C68 126.5(3) . . . . ? C71 N7 C67 C68 -55.7(4) . . . . ? N7 C67 C68 C69 54.6(4) . . . . ? C67 C68 C69 C70 -55.5(4) . . . . ? C68 C69 C70 C71 56.7(4) . . . . ? C65 N7 C71 C70 -125.5(3) . . . . ? C67 N7 C71 C70 56.8(3) . . . . ? C69 C70 C71 N7 -56.9(4) . . . . ? C66 N8 C72 C73 125.3(3) . . . . ? C76 N8 C72 C73 -57.2(4) . . . . ? N8 C72 C73 C74 57.0(4) . . . . ? C72 C73 C74 C75 -55.0(4) . . . . ? C73 C74 C75 C76 53.5(4) . . . . ? C66 N8 C76 C75 -127.0(3) . . . . ? C72 N8 C76 C75 55.5(4) . . . . ? C74 C75 C76 N8 -53.9(4) . . . . ? Ru3 N9 C77 C78 -102(8) . . . . ? C91 P3 C79 C80 128.3(3) . . . . ? C85 P3 C79 C80 -128.0(3) . . . . ? Ru3 P3 C79 C80 -1.7(3) . . . . ? C91 P3 C79 C84 -53.6(3) . . . . ? C85 P3 C79 C84 50.1(3) . . . . ? Ru3 P3 C79 C84 176.5(2) . . . . ? C84 C79 C80 C81 0.1(5) . . . . ? P3 C79 C80 C81 178.3(3) . . . . ? C79 C80 C81 C82 0.8(5) . . . . ? C80 C81 C82 C83 -0.5(6) . . . . ? C81 C82 C83 C84 -0.8(6) . . . . ? C82 C83 C84 C79 1.8(6) . . . . ? C80 C79 C84 C83 -1.4(5) . . . . ? P3 C79 C84 C83 -179.6(3) . . . . ? C91 P3 C85 C90 15.5(3) . . . . ? C79 P3 C85 C90 -91.5(3) . . . . ? Ru3 P3 C85 C90 137.6(3) . . . . ? C91 P3 C85 C86 -168.0(3) . . . . ? C79 P3 C85 C86 85.0(3) . . . . ? Ru3 P3 C85 C86 -45.8(3) . . . . ? C90 C85 C86 C87 1.0(5) . . . . ? P3 C85 C86 C87 -175.6(3) . . . . ? C85 C86 C87 C88 -0.6(5) . . . . ? C86 C87 C88 C89 -0.2(6) . . . . ? C87 C88 C89 C90 0.5(6) . . . . ? C86 C85 C90 C89 -0.7(5) . . . . ? P3 C85 C90 C89 175.8(3) . . . . ? C88 C89 C90 C85 0.0(6) . . . . ? C79 P3 C91 C96 -14.9(3) . . . . ? C85 P3 C91 C96 -117.3(3) . . . . ? Ru3 P3 C91 C96 119.7(3) . . . . ? C79 P3 C91 C92 168.1(2) . . . . ? C85 P3 C91 C92 65.6(3) . . . . ? Ru3 P3 C91 C92 -57.4(3) . . . . ? C96 C91 C92 C93 -0.1(5) . . . . ? P3 C91 C92 C93 177.1(3) . . . . ? C91 C92 C93 C94 -0.2(6) . . . . ? C92 C93 C94 C95 0.2(6) . . . . ? C93 C94 C95 C96 0.1(7) . . . . ? C94 C95 C96 C91 -0.5(6) . . . . ? C92 C91 C96 C95 0.5(5) . . . . ? P3 C91 C96 C95 -176.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.423 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.082 #============================================================================= # end of cif data for "pet13" (compound 7) #============================================================================= #============================================================================= # end of cif file #=============================================================================