Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #============================================================================= # 1 SUBMISSION DETAILS _publ_contact_author ; Professor Liang-Nian Ji Department of Chemistry Zhongshan University Guangzhou 510275 CHINA ; _publ_contact_auther_phone 86-20-84110115 _publ_contact_author_fax 86-20-84035497 _publ_contact_author_email cesjln@zsu.edu.cn _publ_requested_journal J. Chem.Soc., Dalton Trans. _journal_coden_Cambridge 186 _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for deposition as a full paper in J. Chem.Soc., Dalton Trans. Nov. 29th., 2000 ; #============================================================================= # 3 TITLE AND AUTHOR LIST _publ_section_title ; Ruthenium(II) complexes containing novel asymmetric terdentate ligands: synthesis, structure, electrochemical and spectroscopic properties ; loop_ _publ_author_name _publ_author_address 'Hui Chao' ;State Key Laboratory of Ultrafast Laser Spectroscopy Department of Chemistry Zhongshan University Guangzhou 510275 P. R. China ; 'Guang Yang' ;State Key Laboratory of Ultrafast Laser Spectroscopy Department of Chemistry Zhongshan University Guangzhou 510275 P. R. China ; 'Geng-Qiang Xue' ;State Key Laboratory of Ultrafast Laser Spectroscopy Department of Chemistry Zhongshan University Guangzhou 510275 P. R. China ; 'Hong Li' ;State Key Laboratory of Ultrafast Laser Spectroscopy Department of Chemistry Zhongshan University Guangzhou 510275 P. R. China ; 'Ian D. Williams' ; Department of Chemistry Hong Kong University of Science and Technology Kowloon Hong Kong P. R. China ; 'Liang-Nian Ji' ;State Key Laboratory of Ultrafast Laser Spectroscopy Department of Chemistry Zhongshan University Guangzhou 510275 P. R. China ; 'Xiao-Ming Chen' ;State Key Laboratory of Ultrafast Laser Spectroscopy Department of Chemistry Zhongshan University Guangzhou 510275 P. R. China ; 'Xiao-Yuan Li' ;Department of Chemistry Hong Kong University of Science and Technology Kowloon Hong Kong P. R. China ; #============================================================================= data_Rudppt _database_code_CSD 154059 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(tpy)(dppt)][ClO~4~]~2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H28 Cl2 N8 O8 Ru' _chemical_formula_weight 944.69 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0480(10) _cell_length_b 12.9520(10) _cell_length_c 15.721(2) _cell_angle_alpha 73.770(10) _cell_angle_beta 73.610(10) _cell_angle_gamma 68.150(10) _cell_volume 1964.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Bar _exptl_crystal_colour Brownish-red _exptl_crystal_size_max 1.2 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.8 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method ? _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.97 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6856 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6464 _reflns_number_observed 4721 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 20 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+1.8000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6444 _refine_ls_number_parameters 523 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_obs 0.0579 _refine_ls_wR_factor_all 0.1565 _refine_ls_wR_factor_obs 0.1272 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.140 _refine_ls_restrained_S_obs 1.105 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.53776(5) 0.62767(4) 0.24095(3) 0.0341(2) Uani 1 d . . N1 N 0.6630(5) 0.5334(4) 0.3311(3) 0.0363(11) Uani 1 d . . N2 N 0.4327(5) 0.6865(4) 0.3528(3) 0.0427(12) Uani 1 d . . N3 N 0.3703(5) 0.7434(4) 0.1952(3) 0.0404(12) Uani 1 d . . N4 N 0.6433(5) 0.7451(4) 0.1991(3) 0.0411(12) Uani 1 d . . N5 N 0.6483(5) 0.5845(4) 0.1258(3) 0.0346(11) Uani 1 d . . N6 N 0.4887(4) 0.4896(4) 0.2372(3) 0.0333(10) Uani 1 d . . N7 N 0.4202(5) 0.4299(4) 0.3054(3) 0.0345(11) Uani 1 d . . N8 N 0.5157(5) 0.3674(4) 0.1386(3) 0.0364(11) Uani 1 d . . C11 C 0.7815(6) 0.4512(5) 0.3163(4) 0.0459(15) Uani 1 d . . H11A H 0.8123(6) 0.4303(5) 0.2601(4) 0.055 Uiso 1 calc R . C12 C 0.8584(7) 0.3972(6) 0.3815(4) 0.054(2) Uani 1 d . . H12A H 0.9396(7) 0.3413(6) 0.3686(4) 0.064 Uiso 1 calc R . C13 C 0.8145(8) 0.4263(6) 0.4664(5) 0.060(2) Uani 1 d . . H13A H 0.8652(8) 0.3912(6) 0.5110(5) 0.072 Uiso 1 calc R . C14 C 0.6927(7) 0.5093(6) 0.4820(4) 0.054(2) Uani 1 d . . H14A H 0.6602(7) 0.5295(6) 0.5385(4) 0.065 Uiso 1 calc R . C15 C 0.6184(6) 0.5627(5) 0.4155(4) 0.0424(15) Uani 1 d . . C21 C 0.4902(7) 0.6532(5) 0.4256(4) 0.046(2) Uani 1 d . . C22 C 0.4265(8) 0.7086(6) 0.4982(4) 0.059(2) Uani 1 d . . H22A H 0.4640(8) 0.6865(6) 0.5491(4) 0.071 Uiso 1 calc R . C23 C 0.3091(9) 0.7952(6) 0.4948(5) 0.069(2) Uani 1 d . . H23A H 0.2674(9) 0.8323(6) 0.5432(5) 0.083 Uiso 1 calc R . C24 C 0.2519(8) 0.8282(6) 0.4196(5) 0.062(2) Uani 1 d . . H24A H 0.1717(8) 0.8869(6) 0.4174(5) 0.074 Uiso 1 calc R . C25 C 0.3156(7) 0.7726(5) 0.3473(4) 0.047(2) Uani 1 d . . C31 C 0.2769(6) 0.8002(5) 0.2586(4) 0.046(2) Uani 1 d . . C32 C 0.1579(7) 0.8775(6) 0.2394(6) 0.062(2) Uani 1 d . . H32A H 0.0958(7) 0.9149(6) 0.2838(6) 0.074 Uiso 1 calc R . C33 C 0.1304(8) 0.8996(6) 0.1553(6) 0.066(2) Uani 1 d . . H33A H 0.0500(8) 0.9514(6) 0.1421(6) 0.079 Uiso 1 calc R . C34 C 0.2253(7) 0.8430(6) 0.0900(5) 0.062(2) Uani 1 d . . H34A H 0.2104(7) 0.8569(6) 0.0319(5) 0.075 Uiso 1 calc R . C35 C 0.3422(7) 0.7657(5) 0.1133(4) 0.0461(15) Uani 1 d . . H35A H 0.4048(7) 0.7270(5) 0.0698(4) 0.055 Uiso 1 calc R . C41 C 0.6441(7) 0.8246(5) 0.2382(4) 0.051(2) Uani 1 d . . H41A H 0.5862(7) 0.8364(5) 0.2930(4) 0.061 Uiso 1 calc R . C42 C 0.7288(7) 0.8901(6) 0.1994(5) 0.060(2) Uani 1 d . . H42A H 0.7249(7) 0.9459(6) 0.2276(5) 0.072 Uiso 1 calc R . C43 C 0.8169(7) 0.8727(6) 0.1207(5) 0.059(2) Uani 1 d . . H43A H 0.8729(7) 0.9167(6) 0.0950(5) 0.071 Uiso 1 calc R . C44 C 0.8234(7) 0.7887(5) 0.0782(4) 0.049(2) Uani 1 d . . C45 C 0.7332(6) 0.7279(5) 0.1198(4) 0.0398(14) Uani 1 d . . C51 C 0.9139(7) 0.7594(6) -0.0031(4) 0.058(2) Uani 1 d . . H51A H 0.9761(7) 0.7974(6) -0.0303(4) 0.069 Uiso 1 calc R . C52 C 0.9133(7) 0.6795(6) -0.0417(4) 0.058(2) Uani 1 d . . H52A H 0.9728(7) 0.6650(6) -0.0955(4) 0.069 Uiso 1 calc R . C61 C 0.7358(6) 0.6422(5) 0.0790(4) 0.0376(13) Uani 1 d . . C62 C 0.8221(6) 0.6160(5) -0.0012(4) 0.0461(15) Uani 1 d . . C63 C 0.8090(7) 0.5311(6) -0.0352(4) 0.056(2) Uani 1 d . . H63A H 0.8622(7) 0.5132(6) -0.0899(4) 0.067 Uiso 1 calc R . C64 C 0.7190(6) 0.4744(5) 0.0114(4) 0.047(2) Uani 1 d . . H64A H 0.7118(6) 0.4181(5) -0.0111(4) 0.057 Uiso 1 calc R . C65 C 0.6382(6) 0.5032(5) 0.0935(3) 0.0365(13) Uani 1 d . . C71 C 0.5419(6) 0.4498(4) 0.1578(3) 0.0344(13) Uani 1 d . . C72 C 0.4406(6) 0.3143(5) 0.2042(4) 0.0367(13) Uani 1 d . . C73 C 0.4011(5) 0.3413(4) 0.2914(3) 0.0337(12) Uani 1 d . . C81 C 0.4068(6) 0.2260(4) 0.1801(4) 0.0369(13) Uani 1 d . . C82 C 0.2840(6) 0.2093(5) 0.2134(4) 0.048(2) Uani 1 d . . H82A H 0.2194(6) 0.2533(5) 0.2529(4) 0.057 Uiso 1 calc R . C83 C 0.2571(7) 0.1273(6) 0.1880(5) 0.057(2) Uani 1 d . . H83A H 0.1747(7) 0.1159(6) 0.2102(5) 0.069 Uiso 1 calc R . C84 C 0.3548(8) 0.0622(6) 0.1289(5) 0.061(2) Uani 1 d . . H84A H 0.3369(8) 0.0070(6) 0.1118(5) 0.073 Uiso 1 calc R . C85 C 0.4765(8) 0.0774(6) 0.0956(5) 0.059(2) Uani 1 d . . H85A H 0.5412(8) 0.0327(6) 0.0565(5) 0.071 Uiso 1 calc R . C86 C 0.5023(6) 0.1607(5) 0.1207(4) 0.0429(14) Uani 1 d . . H86A H 0.5843(6) 0.1727(5) 0.0975(4) 0.051 Uiso 1 calc R . C91 C 0.3417(6) 0.2721(5) 0.3735(4) 0.0412(14) Uani 1 d . . C92 C 0.3989(7) 0.1550(5) 0.3940(4) 0.055(2) Uani 1 d . . H92A H 0.4738(7) 0.1188(5) 0.3550(4) 0.066 Uiso 1 calc R . C93 C 0.3448(9) 0.0912(7) 0.4724(6) 0.077(2) Uani 1 d . . H93A H 0.3828(9) 0.0128(7) 0.4853(6) 0.093 Uiso 1 calc R . C94 C 0.2357(10) 0.1443(8) 0.5305(6) 0.086(3) Uani 1 d . . H94A H 0.2006(10) 0.1016(8) 0.5832(6) 0.103 Uiso 1 calc R . C95 C 0.1778(8) 0.2592(8) 0.5119(5) 0.072(2) Uani 1 d . . H95A H 0.1035(8) 0.2942(8) 0.5519(5) 0.087 Uiso 1 calc R . C96 C 0.22914(12) 0.32403(9) 0.43361(8) 0.049(2) Uani 1 d . . H96A H 0.18869(12) 0.40220(9) 0.42101(8) 0.059 Uiso 1 calc R . Cl1 Cl 0.81733(12) 0.16158(9) 0.23798(8) 0.0558(4) Uani 1 d RD . O11 O 0.83174(12) 0.12651(9) 0.15733(8) 0.122(2) Uani 1 d RD . O12 O 0.81339(12) 0.27389(9) 0.20275(8) 0.117(4) Uani 0.60 d PRD . O13 O 0.69818(12) 0.15517(9) 0.29175(8) 0.131(5) Uani 0.60 d PRD . O14 O 0.92028(12) 0.10526(9) 0.28307(8) 0.115(4) Uani 0.60 d PRD . O15 O 0.70640(12) 0.24000(9) 0.27164(8) 0.091(5) Uiso 0.40 d PRD . O16 O 0.83576(12) 0.05882(9) 0.30032(8) 0.141(7) Uiso 0.40 d PRD . O17 O 0.92177(12) 0.20081(9) 0.22991(8) 0.119(6) Uiso 0.40 d PRD . Cl2 Cl 0.92675(12) 0.40834(9) 0.74492(8) 0.0599(5) Uani 1 d RD . O21 O 0.89747(12) 0.52566(9) 0.74106(8) 0.079(2) Uani 1 d RD . O22 O 0.88624(12) 0.39068(9) 0.67496(8) 0.106(2) Uani 1 d RD . O23 O 0.86509(12) 0.36297(9) 0.82611(8) 0.208(6) Uani 1 d RD . O24 O 1.06345(12) 0.35905(9) 0.73401(8) 0.165(4) Uani 1 d RD . 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 0.0409(3) 0.0331(2) 0.0335(2) -0.0094(2) -0.0043(2) -0.0179(2) N1 0.040(3) 0.040(3) 0.037(2) -0.009(2) -0.005(2) -0.023(2) N2 0.051(3) 0.042(3) 0.041(3) -0.015(2) 0.000(2) -0.024(3) N3 0.044(3) 0.036(3) 0.047(3) -0.010(2) -0.008(2) -0.019(2) N4 0.048(3) 0.039(3) 0.044(3) -0.006(2) -0.012(2) -0.021(2) N5 0.040(3) 0.033(2) 0.033(2) -0.006(2) -0.005(2) -0.016(2) N6 0.039(3) 0.036(2) 0.030(2) -0.010(2) -0.004(2) -0.016(2) N7 0.039(3) 0.034(2) 0.032(2) -0.006(2) -0.006(2) -0.014(2) N8 0.044(3) 0.035(2) 0.038(2) -0.012(2) -0.012(2) -0.015(2) C11 0.047(4) 0.050(4) 0.047(3) -0.008(3) -0.009(3) -0.024(3) C12 0.049(4) 0.056(4) 0.059(4) -0.002(3) -0.016(3) -0.023(3) C13 0.070(5) 0.067(5) 0.058(4) -0.002(3) -0.027(4) -0.036(4) C14 0.078(5) 0.067(4) 0.035(3) -0.005(3) -0.016(3) -0.042(4) C15 0.059(4) 0.046(3) 0.037(3) -0.008(3) -0.007(3) -0.035(3) C21 0.063(5) 0.045(3) 0.040(3) -0.014(3) -0.002(3) -0.032(3) C22 0.083(6) 0.068(5) 0.042(4) -0.023(3) 0.005(3) -0.043(4) C23 0.097(6) 0.063(5) 0.055(4) -0.032(4) 0.006(4) -0.035(5) C24 0.067(5) 0.050(4) 0.063(4) -0.024(3) 0.006(4) -0.016(4) C25 0.053(4) 0.040(3) 0.053(4) -0.015(3) 0.004(3) -0.025(3) C31 0.043(4) 0.035(3) 0.060(4) -0.014(3) -0.002(3) -0.015(3) C32 0.045(5) 0.048(4) 0.093(6) -0.024(4) -0.006(4) -0.014(3) C33 0.053(5) 0.054(4) 0.097(6) -0.011(4) -0.024(4) -0.019(4) C34 0.059(5) 0.059(4) 0.078(5) -0.004(4) -0.030(4) -0.025(4) C35 0.052(4) 0.038(3) 0.058(4) -0.009(3) -0.019(3) -0.019(3) C41 0.062(5) 0.043(3) 0.056(4) -0.010(3) -0.016(3) -0.024(3) C42 0.071(5) 0.046(4) 0.083(5) -0.008(3) -0.032(4) -0.030(4) C43 0.059(5) 0.052(4) 0.076(5) 0.009(3) -0.025(4) -0.036(4) C44 0.048(4) 0.050(4) 0.055(4) 0.005(3) -0.020(3) -0.025(3) C45 0.038(4) 0.042(3) 0.042(3) 0.002(2) -0.016(3) -0.018(3) C51 0.056(5) 0.072(5) 0.052(4) 0.010(3) -0.013(3) -0.041(4) C52 0.050(5) 0.077(5) 0.044(4) 0.003(3) 0.000(3) -0.036(4) C61 0.035(4) 0.041(3) 0.037(3) 0.001(2) -0.013(3) -0.014(3) C62 0.046(4) 0.058(4) 0.033(3) -0.001(3) -0.007(3) -0.021(3) C63 0.056(5) 0.070(4) 0.035(3) -0.015(3) 0.006(3) -0.021(4) C64 0.051(4) 0.055(4) 0.036(3) -0.011(3) -0.006(3) -0.018(3) C65 0.044(4) 0.038(3) 0.030(3) -0.005(2) -0.007(2) -0.018(3) C71 0.040(4) 0.034(3) 0.037(3) -0.009(2) -0.011(2) -0.015(3) C72 0.036(3) 0.036(3) 0.042(3) -0.010(2) -0.010(3) -0.013(3) C73 0.032(3) 0.034(3) 0.037(3) -0.007(2) -0.007(2) -0.011(2) C81 0.041(4) 0.035(3) 0.041(3) -0.006(2) -0.016(3) -0.015(3) C82 0.040(4) 0.050(4) 0.062(4) -0.023(3) -0.015(3) -0.012(3) C83 0.056(5) 0.055(4) 0.075(5) -0.014(3) -0.018(4) -0.029(4) C84 0.081(6) 0.056(4) 0.069(5) -0.019(3) -0.024(4) -0.036(4) C85 0.077(5) 0.055(4) 0.060(4) -0.029(3) -0.010(4) -0.026(4) C86 0.043(4) 0.048(3) 0.048(3) -0.016(3) -0.008(3) -0.021(3) C91 0.053(4) 0.043(3) 0.042(3) -0.001(3) -0.020(3) -0.028(3) C92 0.052(4) 0.049(4) 0.063(4) 0.001(3) -0.013(3) -0.023(3) C93 0.092(7) 0.058(5) 0.087(6) 0.021(4) -0.038(5) -0.040(5) C94 0.095(7) 0.098(7) 0.067(5) 0.024(5) -0.020(5) -0.061(6) C95 0.065(5) 0.108(7) 0.050(4) -0.012(4) 0.002(4) -0.048(5) C96 0.052(4) 0.060(4) 0.041(3) -0.010(3) -0.006(3) -0.026(3) Cl1 0.0410(10) 0.0465(9) 0.0743(11) -0.0136(8) -0.0021(8) -0.0135(7) O11 0.118(6) 0.164(7) 0.116(5) -0.068(5) -0.007(4) -0.062(5) O12 0.167(11) 0.046(5) 0.150(10) -0.012(6) -0.050(9) -0.039(6) O13 0.045(6) 0.258(16) 0.089(7) -0.010(8) 0.011(5) -0.082(8) O14 0.041(6) 0.126(9) 0.162(10) -0.041(8) -0.058(6) 0.027(6) Cl2 0.0745(13) 0.0575(10) 0.0526(10) -0.0086(8) -0.0134(9) -0.0276(9) O21 0.105(4) 0.063(3) 0.072(3) -0.011(3) -0.017(3) -0.031(3) O22 0.132(6) 0.095(4) 0.108(5) -0.046(4) -0.052(4) -0.017(4) O23 0.409(15) 0.213(9) 0.084(5) -0.049(5) 0.061(7) -0.257(11) O24 0.124(7) 0.124(7) 0.249(11) -0.035(7) -0.104(7) 0.008(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 Ru1 N5 1.973(4) . ? Ru1 N2 1.990(4) . ? Ru1 N3 2.067(5) . ? Ru1 N1 2.073(5) . ? Ru1 N6 2.072(4) . ? Ru1 N4 2.106(4) . ? N1 C11 1.353(8) . ? N1 C15 1.386(7) . ? N2 C21 1.353(8) . ? N2 C25 1.364(8) . ? N3 C35 1.337(7) . ? N3 C31 1.365(7) . ? N4 C41 1.342(7) . ? N4 C45 1.372(7) . ? N5 C65 1.340(7) . ? N5 C61 1.365(7) . ? N6 N7 1.354(6) . ? N6 C71 1.376(6) . ? N7 C73 1.326(7) . ? N8 C72 1.331(7) . ? N8 C71 1.332(6) . ? C11 C12 1.383(9) . ? C12 C13 1.393(9) . ? C13 C14 1.383(9) . ? C14 C15 1.379(9) . ? C15 C21 1.466(9) . ? C21 C22 1.393(8) . ? C22 C23 1.366(10) . ? C23 C24 1.385(10) . ? C24 C25 1.390(8) . ? C25 C31 1.484(9) . ? C31 C32 1.377(9) . ? C32 C33 1.368(10) . ? C33 C34 1.389(10) . ? C34 C35 1.380(9) . ? C41 C42 1.396(9) . ? C42 C43 1.357(10) . ? C43 C44 1.399(9) . ? C44 C45 1.404(8) . ? C44 C51 1.429(9) . ? C45 C61 1.416(8) . ? C51 C52 1.342(9) . ? C52 C62 1.435(8) . ? C61 C62 1.391(8) . ? C62 C63 1.417(9) . ? C63 C64 1.377(9) . ? C64 C65 1.405(7) . ? C65 C71 1.477(7) . ? C72 C73 1.417(7) . ? C72 C81 1.493(7) . ? C73 C91 1.487(7) . ? C81 C82 1.385(8) . ? C81 C86 1.386(8) . ? C82 C83 1.384(8) . ? C83 C84 1.391(9) . ? C84 C85 1.364(9) . ? C85 C86 1.390(8) . ? C91 C92 1.391(8) . ? C91 C96 1.400(6) . ? C92 C93 1.393(9) . ? C93 C94 1.368(12) . ? C94 C95 1.365(12) . ? C95 C96 1.388(7) . ? Cl1 O15 1.35 . ? Cl1 O13 1.37 . ? Cl1 O14 1.37 . ? Cl1 O17 1.39 . ? Cl1 O12 1.39 . ? Cl1 O16 1.40 . ? Cl1 O11 1.41 . ? O12 O17 1.32 . ? O12 O15 1.47 . ? O13 O15 1.09 . ? O13 O16 1.58 . ? O14 O16 1.22 . ? O14 O17 1.29 . ? Cl2 O23 1.35 . ? Cl2 O24 1.38 . ? Cl2 O22 1.40 . ? Cl2 O21 1.42 . ? 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 N2 173.6(2) . . ? N5 Ru1 N3 99.6(2) . . ? N2 Ru1 N3 79.4(2) . . ? N5 Ru1 N1 102.1(2) . . ? N2 Ru1 N1 78.8(2) . . ? N3 Ru1 N1 158.2(2) . . ? N5 Ru1 N6 77.1(2) . . ? N2 Ru1 N6 109.2(2) . . ? N3 Ru1 N6 93.1(2) . . ? N1 Ru1 N6 93.4(2) . . ? N5 Ru1 N4 79.9(2) . . ? N2 Ru1 N4 93.8(2) . . ? N3 Ru1 N4 93.6(2) . . ? N1 Ru1 N4 88.5(2) . . ? N6 Ru1 N4 156.8(2) . . ? C11 N1 C15 117.8(5) . . ? C11 N1 Ru1 128.0(4) . . ? C15 N1 Ru1 114.1(4) . . ? C21 N2 C25 122.7(5) . . ? C21 N2 Ru1 118.5(4) . . ? C25 N2 Ru1 117.8(4) . . ? C35 N3 C31 117.5(5) . . ? C35 N3 Ru1 127.9(4) . . ? C31 N3 Ru1 114.5(4) . . ? C41 N4 C45 117.0(5) . . ? C41 N4 Ru1 132.1(4) . . ? C45 N4 Ru1 110.7(3) . . ? C65 N5 C61 120.8(5) . . ? C65 N5 Ru1 122.2(4) . . ? C61 N5 Ru1 117.0(4) . . ? N7 N6 C71 117.1(4) . . ? N7 N6 Ru1 127.7(3) . . ? C71 N6 Ru1 115.0(3) . . ? C73 N7 N6 119.4(4) . . ? C72 N8 C71 116.9(5) . . ? N1 C11 C12 122.5(6) . . ? C11 C12 C13 120.1(7) . . ? C14 C13 C12 117.5(6) . . ? C15 C14 C13 121.3(6) . . ? C14 C15 N1 120.8(6) . . ? C14 C15 C21 124.8(5) . . ? N1 C15 C21 114.3(5) . . ? N2 C21 C22 118.6(6) . . ? N2 C21 C15 113.6(5) . . ? C22 C21 C15 127.8(6) . . ? C23 C22 C21 120.2(7) . . ? C22 C23 C24 120.4(6) . . ? C25 C24 C23 119.3(7) . . ? N2 C25 C24 118.9(6) . . ? N2 C25 C31 113.2(5) . . ? C24 C25 C31 127.7(6) . . ? N3 C31 C32 121.5(6) . . ? N3 C31 C25 114.6(6) . . ? C32 C31 C25 123.9(6) . . ? C33 C32 C31 120.4(7) . . ? C32 C33 C34 118.6(7) . . ? C35 C34 C33 118.5(7) . . ? N3 C35 C34 123.5(6) . . ? N4 C41 C42 122.3(6) . . ? C43 C42 C41 120.2(6) . . ? C42 C43 C44 120.1(6) . . ? C43 C44 C45 116.6(6) . . ? C43 C44 C51 125.8(6) . . ? C45 C44 C51 117.6(6) . . ? N4 C45 C44 123.8(5) . . ? N4 C45 C61 117.5(5) . . ? C44 C45 C61 118.7(5) . . ? C52 C51 C44 123.0(6) . . ? C51 C52 C62 120.9(6) . . ? N5 C61 C62 121.9(5) . . ? N5 C61 C45 114.8(5) . . ? C62 C61 C45 123.4(5) . . ? C61 C62 C63 116.6(5) . . ? C61 C62 C52 116.5(6) . . ? C63 C62 C52 126.9(6) . . ? C64 C63 C62 121.2(5) . . ? C63 C64 C65 118.7(6) . . ? N5 C65 C64 120.6(5) . . ? N5 C65 C71 110.8(4) . . ? C64 C65 C71 128.5(5) . . ? N8 C71 N6 124.9(5) . . ? N8 C71 C65 120.7(5) . . ? N6 C71 C65 114.4(4) . . ? N8 C72 C73 119.5(5) . . ? N8 C72 C81 116.1(5) . . ? C73 C72 C81 124.3(5) . . ? N7 C73 C72 121.0(5) . . ? N7 C73 C91 115.1(4) . . ? C72 C73 C91 123.8(5) . . ? C82 C81 C86 119.6(5) . . ? C82 C81 C72 122.4(5) . . ? C86 C81 C72 118.0(5) . . ? C83 C82 C81 120.1(6) . . ? C82 C83 C84 119.2(6) . . ? C85 C84 C83 121.4(6) . . ? C84 C85 C86 119.0(6) . . ? C85 C86 C81 120.6(6) . . ? C92 C91 C96 118.4(5) . . ? C92 C91 C73 120.9(6) . . ? C96 C91 C73 120.7(4) . . ? C93 C92 C91 120.5(7) . . ? C94 C93 C92 119.8(7) . . ? C93 C94 C95 120.8(7) . . ? C94 C95 C96 120.3(7) . . ? C95 C96 C91 120.2(4) . . ? O15 Cl1 O13 47.1 . . ? O15 Cl1 O14 122.0 . . ? O13 Cl1 O14 111.8 . . ? O15 Cl1 O17 105.7 . . ? O13 Cl1 O17 142.7 . . ? O14 Cl1 O17 55.7 . . ? O15 Cl1 O12 64.8 . . ? O13 Cl1 O12 111.3 . . ? O14 Cl1 O12 110.3 . . ? O17 Cl1 O12 56.5 . . ? O15 Cl1 O16 109.4 . . ? O13 Cl1 O16 69.7 . . ? O14 Cl1 O16 52.3 . . ? O17 Cl1 O16 108.0 . . ? O12 Cl1 O16 157.2 . . ? O15 Cl1 O11 122.5 . . ? O13 Cl1 O11 108.0 . . ? O14 Cl1 O11 115.4 . . ? O17 Cl1 O11 108.9 . . ? O12 Cl1 O11 99.6 . . ? O16 Cl1 O11 101.7 . . ? O17 O12 Cl1 61.5 . . ? O17 O12 O15 102.9 . . ? Cl1 O12 O15 56.2 . . ? O15 O13 Cl1 65.6 . . ? O15 O13 O16 113.2 . . ? Cl1 O13 O16 56.1 . . ? O16 O14 O17 127.8 . . ? O16 O14 Cl1 65.0 . . ? O17 O14 Cl1 62.8 . . ? O13 O15 Cl1 67.3 . . ? O13 O15 O12 125.4 . . ? Cl1 O15 O12 59.0 . . ? O14 O16 Cl1 62.6 . . ? O14 O16 O13 107.3 . . ? Cl1 O16 O13 54.2 . . ? O14 O17 O12 121.1 . . ? O14 O17 Cl1 61.5 . . ? O12 O17 Cl1 62.0 . . ? O23 Cl2 O24 110.8 . . ? O23 Cl2 O22 110.4 . . ? O24 Cl2 O22 108.2 . . ? O23 Cl2 O21 108.8 . . ? O24 Cl2 O21 107.5 . . ? O22 Cl2 O21 111.2 . . ? _refine_diff_density_max 0.719 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.091 #============================================================================= data_Rupta _database_code_CSD 154060 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(tpy)(pta)][ClO~4~]~2~(CH~3~CN) _chemical_formula_sum 'C42 H27 Cl2 N9 O8 Ru' _chemical_formula_weight 957.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/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 12.3635(19) _cell_length_b 26.210(4) _cell_length_c 12.4622(19) _cell_angle_alpha 90.00 _cell_angle_beta 102.797(3) _cell_angle_gamma 90.00 _cell_volume 3938.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour dark brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker SMART 1000 CCD _diffrn_measurement_method omega scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28124 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 30.03 _reflns_number_total 11384 _reflns_number_gt 7113 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1062P)^2^+1.5024P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11384 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1666 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 4.145 _refine_ls_shift/su_mean 0.046 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.27584(2) 0.114803(10) 0.15361(2) 0.03466(10) Uani 1 d . . . Cl1 Cl 0.88589(9) 0.17831(4) 0.88537(9) 0.0599(3) Uani 1 d . . . Cl2 Cl -0.13117(11) 0.44362(5) 0.26707(10) 0.0722(3) Uani 1 d . . . N1 N 0.1887(2) 0.07467(12) 0.0184(2) 0.0447(7) Uani 1 d . . . N2 N 0.2763(2) 0.04493(11) 0.2157(2) 0.0393(6) Uani 1 d . . . N3 N 0.1329(2) 0.14809(10) 0.1806(2) 0.0357(6) Uani 1 d . . . N4 N 0.3559(2) 0.12725(11) 0.3161(2) 0.0377(6) Uani 1 d . . . N5 N 0.2865(2) 0.18512(10) 0.1007(2) 0.0376(6) Uani 1 d . . . N6 N 0.4244(2) 0.11020(11) 0.0969(2) 0.0427(7) Uani 1 d . . . N7 N 0.0507(2) 0.12283(10) 0.2161(2) 0.0369(6) Uani 1 d . . . N8 N 0.0383(2) 0.22933(11) 0.1700(2) 0.0412(6) Uani 1 d . . . O1 O 0.9881(3) 0.20517(15) 0.9033(4) 0.0987(13) Uani 1 d . . . O2 O 0.8927(3) 0.14122(13) 0.9713(3) 0.0780(10) Uani 1 d . . . O3 O 0.8016(4) 0.21323(18) 0.8840(5) 0.136(2) Uani 1 d . . . O4 O 0.8735(5) 0.15129(17) 0.7844(3) 0.1299(19) Uani 1 d . . . O5 O -0.1533(9) 0.3950(2) 0.2605(8) 0.227(5) Uani 1 d . . . O6 O -0.2078(7) 0.4642(4) 0.1817(5) 0.220(4) Uani 1 d . . . O7 O -0.0357(5) 0.4569(4) 0.2468(5) 0.227(5) Uani 1 d . . . O8 O -0.1462(3) 0.46453(18) 0.3669(3) 0.1020(13) Uani 1 d . . . C1 C 0.1381(3) 0.09325(19) -0.0804(3) 0.0589(10) Uani 1 d . . . H1A H 0.1455 0.1290 -0.0941 0.080 Uiso 1 d R . . C2 C 0.0760(4) 0.0628(2) -0.1623(4) 0.0687(13) Uani 1 d . . . H2A H 0.0414 0.0776 -0.2320 0.080 Uiso 1 d R . . C3 C 0.0659(4) 0.0121(2) -0.1442(4) 0.0705(13) Uani 1 d . . . H3A H 0.0220 -0.0090 -0.2003 0.080 Uiso 1 d R . . C4 C 0.1174(3) -0.00793(18) -0.0441(4) 0.0606(11) Uani 1 d . . . H4A H 0.1129 -0.0438 -0.0301 0.080 Uiso 1 d R . . C5 C 0.1769(3) 0.02334(14) 0.0371(3) 0.0467(8) Uani 1 d . . . C6 C 0.2290(3) 0.00633(14) 0.1489(3) 0.0475(8) Uani 1 d . . . C7 C 0.2311(4) -0.04218(16) 0.1905(4) 0.0654(12) Uani 1 d . . . H7A H 0.1982 -0.0698 0.1441 0.080 Uiso 1 d R . . C8 C 0.2801(4) -0.05113(17) 0.2966(5) 0.0719(13) Uani 1 d . . . H8A H 0.2805 -0.0850 0.3260 0.080 Uiso 1 d R . . C9 C 0.3290(4) -0.01183(17) 0.3651(4) 0.0633(11) Uani 1 d . . . H9A H 0.3653 -0.0179 0.4405 0.080 Uiso 1 d R . . C10 C 0.3259(3) 0.03694(14) 0.3213(3) 0.0429(8) Uani 1 d . . . C11 C 0.3707(3) 0.08419(14) 0.3790(3) 0.0426(8) Uani 1 d . . . C12 C 0.4206(3) 0.08626(17) 0.4902(3) 0.0554(10) Uani 1 d . . . H12A H 0.4316 0.0554 0.5325 0.080 Uiso 1 d R . . C13 C 0.4539(4) 0.1323(2) 0.5393(4) 0.0649(11) Uani 1 d . . . H13A H 0.4898 0.1338 0.6159 0.080 Uiso 1 d R . . C14 C 0.4358(3) 0.17624(17) 0.4765(3) 0.0570(10) Uani 1 d . . . H14A H 0.4558 0.2090 0.5092 0.080 Uiso 1 d R . . C15 C 0.3872(3) 0.17201(14) 0.3649(3) 0.0453(8) Uani 1 d . . . H15A H 0.3757 0.2024 0.3209 0.080 Uiso 1 d R . . C16 C -0.0346(3) 0.15105(13) 0.2260(3) 0.0385(7) Uani 1 d . . . C17 C -0.1351(3) 0.13576(15) 0.2619(3) 0.0429(8) Uani 1 d . . . C18 C -0.1762(3) 0.09101(17) 0.2946(3) 0.0538(9) Uani 1 d . . . H18A H -0.1366 0.0595 0.2951 0.080 Uiso 1 d R . . C19 C -0.2787(3) 0.0927(2) 0.3262(4) 0.0635(11) Uani 1 d . . . H19A H -0.3077 0.0619 0.3507 0.080 Uiso 1 d R . . C20 C -0.3395(3) 0.1368(2) 0.3237(4) 0.0655(12) Uani 1 d . . . H20A H -0.4094 0.1363 0.3450 0.080 Uiso 1 d R . . C21 C -0.3000(3) 0.18300(18) 0.2901(3) 0.0566(11) Uani 1 d . . . C22 C -0.3490(4) 0.2322(2) 0.2846(4) 0.0667(13) Uani 1 d . . . H22A H -0.4197 0.2358 0.3037 0.080 Uiso 1 d R . . C23 C -0.2979(4) 0.2742(2) 0.2531(4) 0.0676(13) Uani 1 d . . . H23A H -0.3332 0.3069 0.2514 0.080 Uiso 1 d R . . C24 C -0.1941(3) 0.27131(17) 0.2223(3) 0.0569(10) Uani 1 d . . . H24A H -0.1584 0.3010 0.2013 0.080 Uiso 1 d R . . C25 C -0.1453(3) 0.22404(14) 0.2253(3) 0.0454(8) Uani 1 d . . . C26 C -0.1975(3) 0.18108(16) 0.2585(3) 0.0480(9) Uani 1 d . . . C27 C -0.0407(3) 0.20493(13) 0.2034(3) 0.0410(7) Uani 1 d . . . C28 C 0.1226(3) 0.19880(13) 0.1571(3) 0.0389(7) Uani 1 d . . . C29 C 0.2133(3) 0.22087(13) 0.1138(3) 0.0385(7) Uani 1 d . . . C30 C 0.2293(3) 0.27183(14) 0.0885(3) 0.0481(8) Uani 1 d . . . H30A H 0.1762 0.2971 0.0981 0.080 Uiso 1 d R . . C31 C 0.3205(3) 0.28543(15) 0.0489(3) 0.0527(9) Uani 1 d . . . H31A H 0.3320 0.3205 0.0318 0.080 Uiso 1 d R . . C32 C 0.3977(3) 0.24787(15) 0.0338(3) 0.0477(8) Uani 1 d . . . C33 C 0.4965(4) 0.25584(18) -0.0076(3) 0.0607(11) Uani 1 d . . . H33A H 0.5137 0.2897 -0.0284 0.080 Uiso 1 d R . . C34 C 0.5654(3) 0.21719(19) -0.0153(4) 0.0627(11) Uani 1 d . . . H34A H 0.6296 0.2234 -0.0448 0.080 Uiso 1 d R . . C35 C 0.5458(3) 0.16621(18) 0.0171(3) 0.0550(10) Uani 1 d . . . C36 C 0.6167(4) 0.1241(2) 0.0150(4) 0.0670(12) Uani 1 d . . . H36A H 0.6843 0.1285 -0.0098 0.080 Uiso 1 d R . . C37 C 0.5903(3) 0.0780(2) 0.0512(4) 0.0638(12) Uani 1 d . . . H37A H 0.6367 0.0490 0.0472 0.080 Uiso 1 d R . . C38 C 0.4937(3) 0.07142(17) 0.0930(3) 0.0540(9) Uani 1 d . . . H38A H 0.4767 0.0387 0.1198 0.080 Uiso 1 d R . . C39 C 0.4508(3) 0.15704(15) 0.0582(3) 0.0441(8) Uani 1 d . . . C40 C 0.3776(3) 0.19808(14) 0.0631(3) 0.0421(7) Uani 1 d . . . C100 C 0.0488(13) 0.0833(6) -0.4749(12) 0.226(6) Uiso 1 d . . . N100 N -0.0485(15) 0.0438(7) -0.4461(14) 0.324(7) Uiso 1 d . . . C101 C 0.0883(11) 0.0245(6) -0.5327(11) 0.206(5) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02943(14) 0.03528(15) 0.04153(16) -0.00061(11) 0.01273(10) 0.00192(10) Cl1 0.0647(6) 0.0463(5) 0.0698(6) 0.0036(5) 0.0176(5) -0.0138(4) Cl2 0.0761(8) 0.0761(8) 0.0658(7) -0.0099(6) 0.0186(6) -0.0134(6) N1 0.0363(15) 0.0527(18) 0.0480(17) -0.0077(13) 0.0153(12) 0.0039(12) N2 0.0308(13) 0.0394(15) 0.0516(17) -0.0013(12) 0.0173(12) 0.0007(11) N3 0.0316(13) 0.0368(14) 0.0403(14) 0.0002(11) 0.0114(11) 0.0022(11) N4 0.0288(12) 0.0398(15) 0.0469(16) -0.0010(12) 0.0136(11) 0.0030(10) N5 0.0323(13) 0.0420(15) 0.0401(15) 0.0035(11) 0.0116(11) -0.0032(11) N6 0.0339(14) 0.0508(18) 0.0459(16) -0.0041(13) 0.0139(12) 0.0013(12) N7 0.0324(13) 0.0399(15) 0.0403(14) -0.0001(11) 0.0124(11) 0.0027(11) N8 0.0378(14) 0.0404(15) 0.0453(16) 0.0008(12) 0.0087(12) 0.0081(11) O1 0.083(2) 0.075(2) 0.153(4) 0.005(2) 0.058(3) -0.0258(19) O2 0.101(3) 0.071(2) 0.0615(19) 0.0099(16) 0.0177(17) -0.0248(19) O3 0.080(3) 0.096(3) 0.253(6) 0.039(4) 0.080(4) 0.015(2) O4 0.226(6) 0.082(3) 0.069(2) 0.006(2) 0.007(3) -0.028(3) O5 0.380(13) 0.065(3) 0.298(10) -0.048(5) 0.207(10) -0.034(5) O6 0.278(10) 0.252(9) 0.097(4) -0.002(5) -0.030(5) 0.073(7) O7 0.141(5) 0.413(12) 0.165(5) -0.157(7) 0.114(5) -0.142(6) O8 0.108(3) 0.133(4) 0.073(2) -0.026(2) 0.039(2) -0.031(3) C1 0.053(2) 0.074(3) 0.051(2) -0.005(2) 0.0150(19) 0.008(2) C2 0.058(3) 0.098(4) 0.047(2) -0.018(2) 0.0058(19) 0.006(2) C3 0.048(2) 0.096(4) 0.068(3) -0.036(3) 0.013(2) -0.001(2) C4 0.049(2) 0.063(3) 0.074(3) -0.026(2) 0.024(2) -0.0062(19) C5 0.0343(16) 0.050(2) 0.060(2) -0.0137(17) 0.0189(16) -0.0022(15) C6 0.0391(18) 0.0400(19) 0.068(2) -0.0078(17) 0.0210(17) -0.0007(14) C7 0.065(3) 0.038(2) 0.096(4) -0.007(2) 0.023(3) -0.0082(18) C8 0.074(3) 0.041(2) 0.102(4) 0.016(2) 0.021(3) 0.001(2) C9 0.064(3) 0.051(2) 0.075(3) 0.014(2) 0.015(2) 0.004(2) C10 0.0358(17) 0.0432(19) 0.052(2) 0.0066(15) 0.0143(15) 0.0055(14) C11 0.0366(17) 0.048(2) 0.0457(19) 0.0048(15) 0.0138(14) 0.0059(14) C12 0.054(2) 0.063(3) 0.049(2) 0.0083(19) 0.0113(18) 0.0065(19) C13 0.060(3) 0.085(3) 0.046(2) -0.004(2) 0.0050(19) 0.003(2) C14 0.052(2) 0.064(3) 0.054(2) -0.0144(19) 0.0090(18) -0.0005(19) C15 0.0385(17) 0.047(2) 0.052(2) -0.0044(16) 0.0122(15) 0.0023(14) C16 0.0339(15) 0.0435(18) 0.0388(17) -0.0017(14) 0.0093(13) 0.0039(13) C17 0.0327(16) 0.055(2) 0.0426(18) -0.0057(16) 0.0119(14) 0.0039(15) C18 0.045(2) 0.060(2) 0.060(2) -0.0050(19) 0.0210(18) -0.0017(18) C19 0.051(2) 0.076(3) 0.072(3) -0.008(2) 0.030(2) -0.012(2) C20 0.037(2) 0.094(3) 0.070(3) -0.019(3) 0.0238(19) -0.007(2) C21 0.0360(18) 0.084(3) 0.051(2) -0.019(2) 0.0120(16) 0.0101(19) C22 0.046(2) 0.092(4) 0.064(3) -0.013(2) 0.016(2) 0.024(2) C23 0.059(3) 0.080(3) 0.063(3) -0.012(2) 0.014(2) 0.032(2) C24 0.055(2) 0.061(3) 0.056(2) -0.0072(18) 0.0129(18) 0.0221(19) C25 0.0402(18) 0.051(2) 0.0446(19) -0.0059(15) 0.0090(15) 0.0106(15) C26 0.0363(17) 0.067(2) 0.0414(19) -0.0112(17) 0.0090(14) 0.0083(16) C27 0.0378(17) 0.0441(19) 0.0413(18) -0.0044(14) 0.0096(14) 0.0070(14) C28 0.0350(16) 0.0400(18) 0.0416(17) 0.0020(14) 0.0083(13) 0.0058(13) C29 0.0374(16) 0.0383(17) 0.0400(17) 0.0015(13) 0.0086(13) 0.0005(13) C30 0.048(2) 0.0411(19) 0.053(2) 0.0077(16) 0.0066(17) -0.0005(15) C31 0.052(2) 0.047(2) 0.057(2) 0.0115(17) 0.0070(18) -0.0085(17) C32 0.0456(19) 0.056(2) 0.0423(19) 0.0081(16) 0.0106(15) -0.0112(16) C33 0.054(2) 0.072(3) 0.058(2) 0.014(2) 0.0150(19) -0.018(2) C34 0.047(2) 0.087(3) 0.059(2) 0.009(2) 0.0222(19) -0.016(2) C35 0.0408(19) 0.085(3) 0.042(2) -0.0002(19) 0.0157(16) -0.0075(19) C36 0.041(2) 0.099(4) 0.067(3) -0.005(2) 0.027(2) 0.001(2) C37 0.042(2) 0.082(3) 0.073(3) -0.009(2) 0.026(2) 0.011(2) C38 0.043(2) 0.062(2) 0.061(2) -0.0080(19) 0.0191(17) 0.0079(17) C39 0.0350(16) 0.059(2) 0.0403(18) 0.0019(16) 0.0140(14) 0.0020(15) C40 0.0387(17) 0.051(2) 0.0375(17) 0.0025(14) 0.0105(14) -0.0065(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N5 1.972(3) . ? Ru1 N2 1.988(3) . ? Ru1 N3 2.064(2) . ? Ru1 N4 2.074(3) . ? Ru1 N1 2.074(3) . ? Ru1 N6 2.112(3) . ? Cl1 O3 1.384(4) . ? Cl1 O1 1.420(3) . ? Cl1 O4 1.422(4) . ? Cl1 O2 1.435(3) . ? Cl2 O5 1.302(5) . ? Cl2 O7 1.308(5) . ? Cl2 O6 1.369(7) . ? Cl2 O8 1.409(4) . ? N1 C1 1.343(5) . ? N1 C5 1.379(5) . ? N2 C6 1.357(5) . ? N2 C10 1.339(4) . ? N3 C28 1.361(4) . ? N3 N7 1.366(4) . ? N4 C15 1.338(5) . ? N4 C11 1.363(4) . ? N5 C29 1.337(4) . ? N5 C40 1.357(4) . ? N6 C38 1.337(5) . ? N6 C39 1.384(5) . ? N7 C16 1.317(4) . ? N8 C27 1.310(4) . ? N8 C28 1.351(4) . ? C1 C2 1.385(6) . ? C2 C3 1.359(7) . ? C3 C4 1.374(7) . ? C4 C5 1.380(5) . ? C5 C6 1.469(6) . ? C6 C7 1.371(6) . ? C7 C8 1.348(7) . ? C8 C9 1.388(7) . ? C9 C10 1.387(5) . ? C10 C11 1.477(5) . ? C11 C12 1.387(5) . ? C12 C13 1.374(6) . ? C13 C14 1.382(6) . ? C14 C15 1.392(5) . ? C16 C27 1.439(5) . ? C16 C17 1.466(5) . ? C17 C18 1.376(6) . ? C17 C26 1.412(5) . ? C18 C19 1.409(5) . ? C19 C20 1.373(7) . ? C20 C21 1.404(7) . ? C21 C26 1.409(5) . ? C21 C22 1.420(6) . ? C22 C23 1.369(7) . ? C23 C24 1.420(6) . ? C24 C25 1.375(5) . ? C25 C26 1.404(5) . ? C25 C27 1.468(4) . ? C28 C29 1.467(4) . ? C29 C30 1.397(5) . ? C30 C31 1.374(5) . ? C31 C32 1.412(6) . ? C32 C40 1.392(5) . ? C32 C33 1.443(5) . ? C33 C34 1.341(6) . ? C34 C35 1.432(6) . ? C35 C36 1.412(6) . ? C35 C39 1.403(5) . ? C36 C37 1.356(7) . ? C37 C38 1.415(5) . ? C39 C40 1.415(5) . ? C100 N100 1.685(19) . ? C100 C101 1.813(18) . ? 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 N2 175.45(11) . . ? N5 Ru1 N3 77.42(11) . . ? N2 Ru1 N3 104.74(10) . . ? N5 Ru1 N4 97.29(11) . . ? N2 Ru1 N4 78.76(12) . . ? N3 Ru1 N4 90.83(10) . . ? N5 Ru1 N1 105.28(12) . . ? N2 Ru1 N1 78.76(12) . . ? N3 Ru1 N1 92.16(10) . . ? N4 Ru1 N1 157.35(12) . . ? N5 Ru1 N6 79.30(11) . . ? N2 Ru1 N6 98.63(11) . . ? N3 Ru1 N6 156.62(11) . . ? N4 Ru1 N6 94.22(11) . . ? N1 Ru1 N6 91.89(11) . . ? O3 Cl1 O1 108.4(3) . . ? O3 Cl1 O4 112.7(4) . . ? O1 Cl1 O4 107.7(3) . . ? O3 Cl1 O2 112.1(3) . . ? O1 Cl1 O2 108.4(2) . . ? O4 Cl1 O2 107.5(2) . . ? O5 Cl2 O7 115.7(6) . . ? O5 Cl2 O6 103.7(6) . . ? O7 Cl2 O6 104.2(6) . . ? O5 Cl2 O8 111.7(4) . . ? O7 Cl2 O8 111.6(3) . . ? O6 Cl2 O8 109.2(4) . . ? C1 N1 C5 117.6(3) . . ? C1 N1 Ru1 127.8(3) . . ? C5 N1 Ru1 114.4(2) . . ? C6 N2 C10 121.8(3) . . ? C6 N2 Ru1 118.9(3) . . ? C10 N2 Ru1 119.2(2) . . ? C28 N3 N7 120.1(2) . . ? C28 N3 Ru1 114.9(2) . . ? N7 N3 Ru1 125.0(2) . . ? C15 N4 C11 118.5(3) . . ? C15 N4 Ru1 127.5(2) . . ? C11 N4 Ru1 113.9(2) . . ? C29 N5 C40 120.2(3) . . ? C29 N5 Ru1 121.1(2) . . ? C40 N5 Ru1 118.1(2) . . ? C38 N6 C39 117.3(3) . . ? C38 N6 Ru1 131.9(3) . . ? C39 N6 Ru1 110.8(2) . . ? C16 N7 N3 115.3(3) . . ? C27 N8 C28 113.4(3) . . ? N1 C1 C2 122.4(5) . . ? C3 C2 C1 119.8(5) . . ? C2 C3 C4 118.9(4) . . ? C3 C4 C5 120.2(4) . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C6 114.5(3) . . ? C4 C5 C6 124.4(4) . . ? N2 C6 C7 119.3(4) . . ? N2 C6 C5 113.3(3) . . ? C7 C6 C5 127.4(4) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 120.9(4) . . ? C10 C9 C8 118.1(4) . . ? N2 C10 C9 119.8(4) . . ? N2 C10 C11 112.8(3) . . ? C9 C10 C11 127.3(4) . . ? N4 C11 C12 121.0(4) . . ? N4 C11 C10 115.2(3) . . ? C12 C11 C10 123.7(3) . . ? C13 C12 C11 120.2(4) . . ? C12 C13 C14 119.0(4) . . ? C13 C14 C15 118.6(4) . . ? N4 C15 C14 122.7(4) . . ? N7 C16 C27 122.8(3) . . ? N7 C16 C17 128.7(3) . . ? C27 C16 C17 108.5(3) . . ? C18 C17 C26 119.4(3) . . ? C18 C17 C16 135.9(3) . . ? C26 C17 C16 104.8(3) . . ? C17 C18 C19 118.0(4) . . ? C20 C19 C18 122.8(5) . . ? C19 C20 C21 120.5(4) . . ? C20 C21 C26 116.5(4) . . ? C20 C21 C22 128.7(4) . . ? C26 C21 C22 114.8(4) . . ? C23 C22 C21 121.6(4) . . ? C22 C23 C24 122.5(4) . . ? C25 C24 C23 117.2(4) . . ? C24 C25 C26 120.2(3) . . ? C24 C25 C27 134.6(4) . . ? C26 C25 C27 105.2(3) . . ? C25 C26 C21 123.6(4) . . ? C25 C26 C17 113.6(3) . . ? C21 C26 C17 122.7(4) . . ? N8 C27 C16 122.1(3) . . ? N8 C27 C25 130.0(3) . . ? C16 C27 C25 108.0(3) . . ? N8 C28 N3 126.2(3) . . ? N8 C28 C29 118.9(3) . . ? N3 C28 C29 114.9(3) . . ? N5 C29 C30 120.6(3) . . ? N5 C29 C28 111.2(3) . . ? C30 C29 C28 128.2(3) . . ? C31 C30 C29 119.9(4) . . ? C30 C31 C32 120.0(3) . . ? C40 C32 C31 117.0(3) . . ? C40 C32 C33 116.3(4) . . ? C31 C32 C33 126.7(4) . . ? C34 C33 C32 121.2(4) . . ? C33 C34 C35 122.3(4) . . ? C36 C35 C39 116.5(4) . . ? C36 C35 C34 125.4(4) . . ? C39 C35 C34 118.1(4) . . ? C37 C36 C35 119.6(4) . . ? C36 C37 C38 121.1(4) . . ? N6 C38 C37 121.4(4) . . ? N6 C39 C35 124.1(3) . . ? N6 C39 C40 117.2(3) . . ? C35 C39 C40 118.7(4) . . ? N5 C40 C32 122.4(3) . . ? N5 C40 C39 114.3(3) . . ? C32 C40 C39 123.3(3) . . ? N100 C100 C101 80.2(10) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.167 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.088 #============================================================================= data_Ruptp _database_code_CSD 154061 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(tpy)(ptp)][ClO~4~]~2~(H~2~O) _chemical_formula_sum 'C42 H28 Cl2 N8 O9 Ru' _chemical_formula_weight 960.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/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 14.758(7) _cell_length_b 16.920(7) _cell_length_c 16.887(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.68 _cell_angle_gamma 90.00 _cell_volume 4216(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description prismatic _exptl_crystal_colour dark brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 0.770 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method /w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 2 _diffrn_standards_interval_time 200 _diffrn_standards_decay_% ? _diffrn_reflns_number 7712 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7417 _reflns_number_gt 4734 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1284P)^2^+12.4186P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7417 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2406 _refine_ls_wR_factor_gt 0.2075 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.125 _refine_ls_shift/su_mean 0.009 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.22338(4) 0.22750(4) 0.44262(4) 0.0359(2) Uani 1 d . . . Cl1 Cl 0.17472(17) 0.40151(16) 0.71529(17) 0.0652(7) Uani 1 d . . . Cl2 Cl 0.1602(3) 0.44438(19) 0.1860(2) 0.0993(11) Uani 1 d . . . O1 O 0.1080(8) 0.3903(7) 0.6572(6) 0.136(4) Uani 1 d . . . O2 O 0.1561(8) 0.3682(12) 0.7852(6) 0.209(9) Uani 1 d . . . O3 O 0.191(2) 0.4755(10) 0.7151(12) 0.363(18) Uani 1 d . . . O4 O 0.2509(10) 0.378(2) 0.6893(11) 0.40(2) Uani 1 d . . . O5 O 0.1332(8) 0.3676(5) 0.1690(8) 0.149(5) Uani 1 d . . . O6 O 0.1809(8) 0.4876(7) 0.1169(7) 0.137(4) Uani 1 d . . . O7 O 0.2155(13) 0.4493(8) 0.2452(10) 0.259(11) Uani 1 d . . . O8 O 0.0722(14) 0.4867(10) 0.2029(10) 0.224(8) Uani 1 d . . . N1 N 0.2508(5) 0.4664(4) 0.5085(4) 0.0451(17) Uani 1 d . . . N2 N 0.3611(4) 0.3323(4) 0.5231(4) 0.0417(16) Uani 1 d . . . N3 N 0.2795(4) 0.3282(4) 0.4884(4) 0.0389(15) Uani 1 d . . . N4 N 0.1274(4) 0.3074(4) 0.4195(4) 0.0403(15) Uani 1 d . . . N5 N 0.1217(4) 0.1567(4) 0.3871(4) 0.0435(16) Uani 1 d . . . N6 N 0.1887(4) 0.1871(4) 0.5551(4) 0.0419(16) Uani 1 d . . . N7 N 0.3290(4) 0.1581(4) 0.4699(4) 0.0400(15) Uani 1 d . . . N8 N 0.2962(4) 0.2300(4) 0.3377(4) 0.0431(16) Uani 1 d . . . C1 C 0.3090(8) 0.6144(6) 0.5673(6) 0.067(3) Uani 1 d . . . H1 H 0.2491 0.6063 0.5459 0.080 Uiso 1 d R . . C2 C 0.3368(9) 0.6861(7) 0.5947(7) 0.081(3) Uani 1 d . . . H2 H 0.2987 0.7318 0.5891 0.080 Uiso 1 d R . . C3 C 0.4237(10) 0.6939(7) 0.6250(7) 0.085(4) Uani 1 d . . . H3 H 0.4449 0.7441 0.6441 0.080 Uiso 1 d R . . C4 C 0.4815(8) 0.6308(7) 0.6296(6) 0.067(3) Uani 1 d . . . H4 H 0.5409 0.6386 0.6522 0.080 Uiso 1 d R . . C5 C 0.4533(7) 0.5541(6) 0.6045(5) 0.057(3) Uani 1 d . . . C6 C 0.3645(6) 0.5488(6) 0.5718(5) 0.054(2) Uani 1 d . . . C7 C 0.5112(6) 0.4838(6) 0.6120(5) 0.054(2) Uani 1 d . . . C8 C 0.6008(7) 0.4856(8) 0.6435(6) 0.069(3) Uani 1 d . . . H8 H 0.6255 0.5352 0.6607 0.080 Uiso 1 d R . . C9 C 0.6500(7) 0.4191(9) 0.6529(7) 0.081(4) Uani 1 d . . . H9 H 0.7109 0.4233 0.6729 0.080 Uiso 1 d R . . C10 C 0.6169(7) 0.3479(9) 0.6306(6) 0.080(3) Uani 1 d . . . H10 H 0.6542 0.3023 0.6401 0.080 Uiso 1 d R . . C11 C 0.5308(6) 0.3412(7) 0.5974(6) 0.065(3) Uani 1 d . . . H11 H 0.5059 0.2903 0.5843 0.080 Uiso 1 d R . . C12 C 0.4780(6) 0.4085(6) 0.5877(5) 0.048(2) Uani 1 d . . . C13 C 0.3877(5) 0.4039(5) 0.5512(4) 0.0398(18) Uani 1 d . . . C14 C 0.3323(6) 0.4708(5) 0.5440(5) 0.049(2) Uani 1 d . . . C15 C 0.2273(6) 0.3955(5) 0.4823(5) 0.0427(19) Uani 1 d . . . C16 C 0.1384(5) 0.3834(5) 0.4412(5) 0.0424(19) Uani 1 d . . . C17 C 0.0721(7) 0.4403(6) 0.4234(6) 0.061(3) Uani 1 d . . . H17 H 0.0830 0.4945 0.4372 0.080 Uiso 1 d R . . C18 C -0.0044(7) 0.4177(7) 0.3827(6) 0.070(3) Uani 1 d . . . H18 H -0.0532 0.4542 0.3735 0.080 Uiso 1 d R . . C19 C -0.0174(6) 0.3384(6) 0.3601(5) 0.057(2) Uani 1 d . . . C20 C 0.0521(5) 0.2842(5) 0.3804(5) 0.044(2) Uani 1 d . . . C21 C -0.0929(7) 0.3053(8) 0.3180(7) 0.074(3) Uani 1 d . . . H21 H -0.1412 0.3411 0.3049 0.080 Uiso 1 d R . . C22 C -0.0978(6) 0.2281(8) 0.2981(6) 0.070(3) Uani 1 d . . . H22 H -0.1512 0.2093 0.2711 0.080 Uiso 1 d R . . C23 C -0.0272(6) 0.1727(6) 0.3208(5) 0.057(2) Uani 1 d . . . C24 C 0.0495(5) 0.2029(6) 0.3626(5) 0.047(2) Uani 1 d . . . C25 C -0.0277(7) 0.0901(7) 0.3073(6) 0.071(3) Uani 1 d . . . H25 H -0.0757 0.0630 0.2796 0.080 Uiso 1 d R . . C26 C 0.0423(7) 0.0450(7) 0.3320(6) 0.070(3) Uani 1 d . . . H26 H 0.0430 -0.0112 0.3246 0.080 Uiso 1 d R . . C27 C 0.1176(7) 0.0788(6) 0.3707(6) 0.056(2) Uani 1 d . . . H27 H 0.1684 0.0470 0.3867 0.080 Uiso 1 d R . . C28 C 0.1104(7) 0.1963(5) 0.5929(5) 0.054(2) Uani 1 d . . . H28 H 0.0648 0.2286 0.5680 0.080 Uiso 1 d R . . C29 C 0.0923(8) 0.1613(7) 0.6652(6) 0.068(3) Uani 1 d . . . H29 H 0.0351 0.1683 0.6908 0.080 Uiso 1 d R . . C30 C 0.1600(8) 0.1157(6) 0.7000(6) 0.069(3) Uani 1 d . . . H30 H 0.1486 0.0894 0.7492 0.080 Uiso 1 d R . . C31 C 0.2405(7) 0.1068(6) 0.6640(5) 0.058(2) Uani 1 d . . . H31 H 0.2881 0.0777 0.6900 0.080 Uiso 1 d R . . C32 C 0.2547(6) 0.1424(5) 0.5911(5) 0.046(2) Uani 1 d . . . C33 C 0.3375(6) 0.1316(5) 0.5446(5) 0.047(2) Uani 1 d . . . C34 C 0.4198(7) 0.0992(6) 0.5700(6) 0.059(2) Uani 1 d . . . H34 H 0.4241 0.0796 0.6233 0.080 Uiso 1 d R . . C35 C 0.4907(7) 0.0920(6) 0.5172(7) 0.067(3) Uani 1 d . . . H35 H 0.5472 0.0708 0.5362 0.080 Uiso 1 d R . . C36 C 0.4793(6) 0.1181(5) 0.4398(6) 0.054(2) Uani 1 d . . . H36 H 0.5280 0.1142 0.4027 0.080 Uiso 1 d R . . C37 C 0.3969(5) 0.1515(5) 0.4175(5) 0.044(2) Uani 1 d . . . C38 C 0.3741(5) 0.1842(5) 0.3396(5) 0.0433(19) Uani 1 d . . . C39 C 0.4241(7) 0.1711(6) 0.2710(6) 0.057(2) Uani 1 d . . . H39 H 0.4758 0.1367 0.2731 0.080 Uiso 1 d R . . C40 C 0.3974(7) 0.2058(7) 0.2010(6) 0.068(3) Uani 1 d . . . H40 H 0.4330 0.1996 0.1542 0.080 Uiso 1 d R . . C41 C 0.3201(7) 0.2525(7) 0.1997(6) 0.073(3) Uani 1 d . . . H41 H 0.3000 0.2751 0.1504 0.080 Uiso 1 d R . . C42 C 0.2715(6) 0.2631(6) 0.2688(5) 0.057(2) Uani 1 d . . . H42 H 0.2194 0.2970 0.2679 0.080 Uiso 1 d R . . O1W O 0.3812(16) 0.322(2) 0.0104(11) 0.144(11) Uani 0.50 d P . . O1W' O 0.310(3) 0.391(2) -0.0278(15) 0.25(2) Uani 0.50 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0338(3) 0.0350(4) 0.0389(4) 0.0004(3) -0.0068(2) 0.0005(3) Cl1 0.0537(14) 0.0653(16) 0.0766(18) 0.0077(14) -0.0014(12) -0.0032(12) Cl2 0.154(3) 0.0597(18) 0.084(2) 0.0093(16) -0.023(2) -0.010(2) O1 0.158(10) 0.148(10) 0.100(7) 0.013(7) -0.051(7) -0.043(8) O2 0.111(8) 0.43(3) 0.084(7) 0.099(11) -0.003(6) -0.094(12) O3 0.69(5) 0.118(13) 0.28(2) -0.054(14) -0.26(3) -0.08(2) O4 0.126(11) 0.83(6) 0.244(18) 0.34(3) 0.087(12) 0.21(2) O5 0.166(10) 0.062(6) 0.217(12) 0.030(7) -0.115(9) -0.004(6) O6 0.127(9) 0.151(10) 0.133(9) 0.045(8) -0.017(7) -0.029(8) O7 0.37(2) 0.131(11) 0.273(18) 0.056(11) -0.246(18) -0.104(13) O8 0.29(2) 0.164(14) 0.215(16) 0.009(12) 0.069(15) 0.091(15) N1 0.054(4) 0.038(4) 0.043(4) -0.001(3) -0.001(3) -0.006(3) N2 0.034(3) 0.048(4) 0.043(4) 0.000(3) -0.007(3) -0.004(3) N3 0.038(4) 0.040(4) 0.039(4) 0.000(3) -0.004(3) 0.005(3) N4 0.035(3) 0.044(4) 0.043(4) 0.004(3) -0.004(3) 0.002(3) N5 0.040(4) 0.048(4) 0.042(4) -0.006(3) -0.003(3) -0.005(3) N6 0.041(4) 0.040(4) 0.045(4) -0.002(3) 0.002(3) -0.004(3) N7 0.039(4) 0.035(4) 0.046(4) -0.002(3) -0.007(3) -0.002(3) N8 0.043(4) 0.039(4) 0.047(4) 0.001(3) -0.014(3) -0.004(3) C1 0.075(7) 0.051(6) 0.074(7) -0.007(5) 0.008(6) -0.010(5) C2 0.088(8) 0.050(6) 0.105(9) -0.010(6) -0.001(7) -0.008(6) C3 0.123(11) 0.050(6) 0.083(8) -0.014(6) 0.019(8) -0.038(7) C4 0.077(7) 0.077(8) 0.048(6) -0.011(5) 0.007(5) -0.034(6) C5 0.069(6) 0.064(6) 0.039(5) -0.003(4) 0.012(4) -0.028(5) C6 0.062(6) 0.052(6) 0.048(5) -0.012(4) 0.012(4) -0.018(5) C7 0.048(5) 0.080(7) 0.034(4) -0.013(5) 0.004(4) -0.022(5) C8 0.057(6) 0.104(9) 0.046(6) -0.015(6) 0.003(5) -0.031(6) C9 0.047(6) 0.123(11) 0.073(8) -0.029(8) -0.016(5) -0.010(7) C10 0.056(6) 0.118(10) 0.065(7) -0.014(7) -0.018(5) 0.009(7) C11 0.050(5) 0.087(8) 0.057(6) -0.009(6) -0.021(5) 0.002(5) C12 0.045(5) 0.065(6) 0.033(4) -0.005(4) -0.005(4) -0.012(4) C13 0.043(4) 0.045(5) 0.032(4) -0.004(4) 0.000(3) -0.012(4) C14 0.061(6) 0.041(5) 0.044(5) -0.006(4) 0.004(4) -0.019(4) C15 0.048(5) 0.040(5) 0.041(5) -0.001(4) 0.003(4) 0.001(4) C16 0.040(4) 0.042(5) 0.045(5) 0.001(4) -0.004(4) 0.003(4) C17 0.061(6) 0.046(5) 0.076(7) 0.008(5) -0.004(5) 0.010(5) C18 0.052(6) 0.072(7) 0.085(8) 0.006(6) -0.021(5) 0.014(5) C19 0.039(5) 0.077(7) 0.053(6) 0.006(5) -0.012(4) 0.003(5) C20 0.039(4) 0.056(6) 0.038(4) 0.000(4) -0.003(3) -0.005(4) C21 0.048(6) 0.097(9) 0.077(7) 0.004(7) -0.018(5) 0.017(6) C22 0.044(5) 0.101(9) 0.063(6) -0.003(6) -0.023(5) -0.008(6) C23 0.047(5) 0.077(7) 0.047(5) -0.010(5) -0.003(4) -0.012(5) C24 0.038(4) 0.064(6) 0.040(5) 0.000(4) -0.003(4) -0.008(4) C25 0.062(7) 0.091(8) 0.059(6) -0.018(6) 0.000(5) -0.033(6) C26 0.070(7) 0.063(7) 0.077(7) -0.025(6) -0.006(6) -0.010(6) C27 0.060(6) 0.049(5) 0.061(6) -0.009(5) 0.002(5) -0.009(5) C28 0.062(6) 0.048(5) 0.051(5) 0.000(4) 0.000(5) 0.002(5) C29 0.072(7) 0.071(7) 0.062(6) 0.005(5) 0.020(5) 0.001(6) C30 0.103(9) 0.058(6) 0.045(6) 0.014(5) 0.014(6) 0.004(6) C31 0.078(7) 0.055(6) 0.041(5) 0.002(4) -0.006(5) 0.001(5) C32 0.052(5) 0.040(5) 0.046(5) -0.001(4) -0.005(4) -0.001(4) C33 0.054(5) 0.040(5) 0.046(5) 0.006(4) -0.007(4) 0.003(4) C34 0.067(6) 0.057(6) 0.052(6) 0.005(5) -0.014(5) 0.009(5) C35 0.054(6) 0.062(7) 0.085(8) 0.005(6) -0.015(6) 0.013(5) C36 0.043(5) 0.042(5) 0.077(7) -0.004(5) 0.000(5) 0.001(4) C37 0.039(4) 0.036(4) 0.059(5) 0.000(4) -0.007(4) -0.001(4) C38 0.038(4) 0.041(5) 0.051(5) 0.001(4) -0.003(4) -0.002(4) C39 0.055(5) 0.055(6) 0.061(6) 0.000(5) 0.009(5) -0.006(4) C40 0.052(6) 0.091(8) 0.061(6) -0.006(6) 0.010(5) -0.011(5) C41 0.069(7) 0.110(9) 0.041(5) 0.027(5) -0.003(5) -0.018(6) C42 0.048(5) 0.070(6) 0.054(6) 0.010(5) -0.002(4) -0.004(5) O1W 0.117(17) 0.26(3) 0.057(11) -0.002(15) 0.062(11) -0.015(19) O1W' 0.32(4) 0.30(4) 0.13(2) -0.16(2) 0.19(3) -0.24(3) _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 N4 1.994(6) . ? Ru1 N7 2.000(6) . ? Ru1 N3 2.042(6) . ? Ru1 N8 2.084(7) . ? Ru1 N6 2.088(7) . ? Ru1 N5 2.130(7) . ? Cl1 O4 1.278(15) . ? Cl1 O3 1.275(16) . ? Cl1 O2 1.339(10) . ? Cl1 O1 1.395(10) . ? Cl2 O7 1.286(11) . ? Cl2 O5 1.387(10) . ? Cl2 O6 1.413(11) . ? Cl2 O8 1.514(16) . ? N1 C14 1.340(11) . ? N1 C15 1.323(10) . ? N2 N3 1.335(8) . ? N2 C13 1.357(10) . ? N3 C15 1.379(10) . ? N4 C20 1.344(10) . ? N4 C16 1.345(10) . ? N5 C27 1.347(11) . ? N5 C24 1.380(11) . ? N6 C28 1.336(11) . ? N6 C32 1.371(10) . ? N7 C33 1.343(10) . ? N7 C37 1.349(10) . ? N8 C42 1.337(11) . ? N8 C38 1.387(10) . ? C1 C2 1.361(14) . ? C1 C6 1.380(14) . ? C2 C3 1.381(17) . ? C3 C4 1.368(16) . ? C4 C5 1.427(14) . ? C5 C6 1.419(13) . ? C5 C7 1.469(14) . ? C6 C14 1.478(11) . ? C7 C8 1.419(13) . ? C7 C12 1.425(13) . ? C8 C9 1.347(16) . ? C9 C10 1.351(17) . ? C10 C11 1.387(13) . ? C11 C12 1.389(14) . ? C12 C13 1.463(11) . ? C13 C14 1.402(12) . ? C15 C16 1.491(11) . ? C16 C17 1.403(12) . ? C17 C18 1.369(13) . ? C18 C19 1.407(15) . ? C19 C20 1.415(12) . ? C19 C21 1.429(14) . ? C20 C24 1.409(12) . ? C21 C22 1.350(16) . ? C22 C23 1.449(14) . ? C23 C24 1.422(11) . ? C23 C25 1.417(15) . ? C25 C26 1.346(15) . ? C26 C27 1.403(13) . ? C28 C29 1.385(13) . ? C29 C30 1.388(15) . ? C30 C31 1.349(14) . ? C31 C32 1.389(12) . ? C32 C33 1.471(12) . ? C33 C34 1.396(12) . ? C34 C35 1.388(14) . ? C35 C36 1.387(14) . ? C36 C37 1.390(11) . ? C37 C38 1.461(11) . ? C38 C39 1.400(12) . ? C39 C40 1.372(14) . ? C40 C41 1.388(15) . ? C41 C42 1.388(14) . ? O1W O1W' 1.70(5) . ? 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 N4 Ru1 N7 173.2(3) . . ? N4 Ru1 N3 78.0(3) . . ? N7 Ru1 N3 95.2(2) . . ? N4 Ru1 N8 101.1(3) . . ? N7 Ru1 N8 78.5(3) . . ? N3 Ru1 N8 95.4(3) . . ? N4 Ru1 N6 102.6(3) . . ? N7 Ru1 N6 78.3(3) . . ? N3 Ru1 N6 91.8(3) . . ? N8 Ru1 N6 156.2(3) . . ? N4 Ru1 N5 78.5(3) . . ? N7 Ru1 N5 108.3(3) . . ? N3 Ru1 N5 156.5(3) . . ? N8 Ru1 N5 90.3(2) . . ? N6 Ru1 N5 92.1(3) . . ? O4 Cl1 O3 98.1(19) . . ? O4 Cl1 O2 111.1(10) . . ? O3 Cl1 O2 117.1(13) . . ? O4 Cl1 O1 109.4(14) . . ? O3 Cl1 O1 105.4(11) . . ? O2 Cl1 O1 114.3(7) . . ? O7 Cl2 O5 113.5(7) . . ? O7 Cl2 O6 117.8(10) . . ? O5 Cl2 O6 112.3(8) . . ? O7 Cl2 O8 111.1(13) . . ? O5 Cl2 O8 103.7(10) . . ? O6 Cl2 O8 96.1(8) . . ? C14 N1 C15 115.5(7) . . ? N3 N2 C13 117.2(7) . . ? N2 N3 C15 119.4(7) . . ? N2 N3 Ru1 124.7(5) . . ? C15 N3 Ru1 115.9(5) . . ? C20 N4 C16 120.6(7) . . ? C20 N4 Ru1 118.6(6) . . ? C16 N4 Ru1 120.8(5) . . ? C27 N5 C24 117.4(7) . . ? C27 N5 Ru1 132.1(6) . . ? C24 N5 Ru1 110.5(5) . . ? C28 N6 C32 117.8(7) . . ? C28 N6 Ru1 128.3(6) . . ? C32 N6 Ru1 113.8(5) . . ? C33 N7 C37 121.7(7) . . ? C33 N7 Ru1 118.5(6) . . ? C37 N7 Ru1 118.7(5) . . ? C42 N8 C38 118.2(8) . . ? C42 N8 Ru1 127.6(6) . . ? C38 N8 Ru1 113.8(5) . . ? C2 C1 C6 121.4(11) . . ? C1 C2 C3 119.1(12) . . ? C4 C3 C2 121.5(10) . . ? C3 C4 C5 120.8(11) . . ? C6 C5 C4 116.0(10) . . ? C6 C5 C7 121.1(8) . . ? C4 C5 C7 122.9(9) . . ? C1 C6 C5 121.1(9) . . ? C1 C6 C14 120.8(9) . . ? C5 C6 C14 118.1(9) . . ? C8 C7 C12 116.2(10) . . ? C8 C7 C5 123.7(10) . . ? C12 C7 C5 120.1(8) . . ? C9 C8 C7 121.7(11) . . ? C8 C9 C10 121.3(10) . . ? C9 C10 C11 120.8(12) . . ? C12 C11 C10 119.4(11) . . ? C11 C12 C7 120.6(8) . . ? C11 C12 C13 120.8(8) . . ? C7 C12 C13 118.5(9) . . ? N2 C13 C14 121.6(7) . . ? N2 C13 C12 117.0(8) . . ? C14 C13 C12 121.4(8) . . ? N1 C14 C13 120.9(7) . . ? N1 C14 C6 118.4(9) . . ? C13 C14 C6 120.6(8) . . ? N1 C15 N3 125.4(8) . . ? N1 C15 C16 120.4(7) . . ? N3 C15 C16 114.1(7) . . ? N4 C16 C17 121.0(8) . . ? N4 C16 C15 111.2(7) . . ? C17 C16 C15 127.8(8) . . ? C18 C17 C16 119.0(9) . . ? C17 C18 C19 120.8(9) . . ? C20 C19 C21 115.2(10) . . ? C20 C19 C18 117.1(8) . . ? C21 C19 C18 127.7(9) . . ? N4 C20 C19 121.5(8) . . ? N4 C20 C24 114.3(7) . . ? C19 C20 C24 124.2(8) . . ? C22 C21 C19 122.8(10) . . ? C21 C22 C23 121.5(9) . . ? C24 C23 C25 115.9(9) . . ? C24 C23 C22 117.7(9) . . ? C25 C23 C22 126.4(9) . . ? N5 C24 C20 118.0(7) . . ? N5 C24 C23 123.5(9) . . ? C20 C24 C23 118.4(8) . . ? C26 C25 C23 120.4(9) . . ? C25 C26 C27 120.9(10) . . ? N5 C27 C26 121.8(9) . . ? N6 C28 C29 123.3(9) . . ? C28 C29 C30 117.7(10) . . ? C31 C30 C29 120.3(9) . . ? C30 C31 C32 119.6(9) . . ? N6 C32 C31 121.2(8) . . ? N6 C32 C33 115.0(7) . . ? C31 C32 C33 123.7(8) . . ? N7 C33 C34 119.4(8) . . ? N7 C33 C32 113.0(7) . . ? C34 C33 C32 127.6(8) . . ? C33 C34 C35 119.8(9) . . ? C36 C35 C34 119.6(9) . . ? C37 C36 C35 118.7(9) . . ? N7 C37 C36 120.7(8) . . ? N7 C37 C38 113.2(7) . . ? C36 C37 C38 126.1(8) . . ? N8 C38 C39 120.9(8) . . ? N8 C38 C37 114.5(7) . . ? C39 C38 C37 124.6(8) . . ? C40 C39 C38 119.8(9) . . ? C39 C40 C41 119.0(10) . . ? C42 C41 C40 119.5(9) . . ? N8 C42 C41 122.6(9) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.245 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.121