# 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 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'K. Natarajan' _publ_contact_author_email 'k natraj6@yahoo.com' loop_ _publ_author_name S.Thangavel C.Nataraj 'Hyosun Lee.' C.F.Fronczek F.Fronczek ; K.Natarajan ; # Attachment '- [RuII-hpa-P].txt' data_2PA _database_code_depnum_ccdc_archive 'CCDC 797111' #TrackingRef '- [RuII-hpa-P].txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H33 N O6 P2 Ru, 2(C2 H6 O), 0.64(C H Cl3)' _chemical_formula_sum 'C48.64 H45.64 Cl1.92 N O8 P2 Ru' _chemical_formula_weight 1003.26 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_cell_setting Triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0057(14) _cell_length_b 14.0262(15) _cell_length_c 15.237(2) _cell_angle_alpha 89.650(5) _cell_angle_beta 81.378(5) _cell_angle_gamma 71.638(6) _cell_volume 2405.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(5) _cell_measurement_reflns_used 17695 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 34.3 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1030 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69185 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.7 _diffrn_reflns_theta_max 34.2 _reflns_number_total 18649 _reflns_number_gt 13944 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0564P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 18649 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.066 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.114 _refine_ls_wR_factor_gt 0.107 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.410179(12) 0.208813(9) 0.331253(9) 0.01141(4) Uani 1 1 d . . . P1 P 0.60177(4) 0.22942(3) 0.30472(3) 0.01319(8) Uani 1 1 d . . . P2 P 0.21550(4) 0.19865(3) 0.36889(3) 0.01158(8) Uani 1 1 d . . . O1 O 0.34060(16) 0.32720(10) -0.04790(9) 0.0305(3) Uani 1 1 d . . . H1 H 0.3677 0.2774 -0.0841 0.046 Uiso 1 1 calc R . . O2 O 0.48972(13) -0.00484(10) 0.12625(9) 0.0245(3) Uani 1 1 d . . . O3 O 0.46937(11) 0.06773(9) 0.26090(8) 0.0148(2) Uani 1 1 d . . . O4 O 0.34246(11) 0.36829(9) 0.34114(8) 0.0147(2) Uani 1 1 d . . . O5 O 0.26757(12) 0.50396(9) 0.26471(9) 0.0205(3) Uani 1 1 d . . . O6 O 0.43990(12) 0.14315(10) 0.51781(9) 0.0225(3) Uani 1 1 d . . . N1 N 0.38424(12) 0.24623(10) 0.20498(9) 0.0123(3) Uani 1 1 d . . . C1 C 0.35434(17) 0.29683(14) 0.03406(12) 0.0196(4) Uani 1 1 d . . . C2 C 0.40177(16) 0.19489(13) 0.05392(12) 0.0164(3) Uani 1 1 d . . . H2 H 0.4245 0.1429 0.0089 0.020 Uiso 1 1 calc R . . C3 C 0.41389(15) 0.17362(12) 0.14154(11) 0.0134(3) Uani 1 1 d . . . C4 C 0.46194(16) 0.07031(13) 0.17716(12) 0.0156(3) Uani 1 1 d . . . C5 C 0.31313(15) 0.41250(12) 0.26900(12) 0.0149(3) Uani 1 1 d . . . C6 C 0.33867(15) 0.34328(12) 0.18743(12) 0.0144(3) Uani 1 1 d . . . C7 C 0.32137(17) 0.37142(13) 0.10253(12) 0.0183(3) Uani 1 1 d . . . H7 H 0.2877 0.4402 0.0905 0.022 Uiso 1 1 calc R . . C8 C 0.43005(15) 0.17002(13) 0.44681(12) 0.0149(3) Uani 1 1 d . . . C9 C 0.63598(16) 0.29720(13) 0.39385(12) 0.0161(3) Uani 1 1 d . . . C10 C 0.74948(17) 0.30717(14) 0.38795(13) 0.0208(4) Uani 1 1 d . . . H10 H 0.8083 0.2784 0.3380 0.025 Uiso 1 1 calc R . . C11 C 0.77597(19) 0.35905(15) 0.45496(14) 0.0243(4) Uani 1 1 d . . . H11 H 0.8527 0.3662 0.4503 0.029 Uiso 1 1 calc R . . C12 C 0.69095(19) 0.40080(14) 0.52924(13) 0.0241(4) Uani 1 1 d . . . H12 H 0.7101 0.4352 0.5754 0.029 Uiso 1 1 calc R . . C13 C 0.57912(19) 0.39166(14) 0.53508(13) 0.0225(4) Uani 1 1 d . . . H13 H 0.5212 0.4196 0.5857 0.027 Uiso 1 1 calc R . . C14 C 0.55012(17) 0.34169(14) 0.46726(12) 0.0192(3) Uani 1 1 d . . . H14 H 0.4719 0.3379 0.4709 0.023 Uiso 1 1 calc R . . C15 C 0.72516(16) 0.11239(13) 0.28560(13) 0.0191(4) Uani 1 1 d . . . C16 C 0.71176(18) 0.02717(14) 0.32760(15) 0.0247(4) Uani 1 1 d . . . H16 H 0.6394 0.0313 0.3650 0.030 Uiso 1 1 calc R . . C17 C 0.8035(2) -0.06380(16) 0.31510(19) 0.0365(6) Uani 1 1 d . . . H17 H 0.7936 -0.1213 0.3442 0.044 Uiso 1 1 calc R . . C18 C 0.9076(2) -0.07101(17) 0.2614(2) 0.0413(7) Uani 1 1 d . . . H18 H 0.9698 -0.1335 0.2530 0.050 Uiso 1 1 calc R . . C19 C 0.92302(18) 0.01347(17) 0.21844(17) 0.0337(5) Uani 1 1 d . . . H19 H 0.9954 0.0082 0.1807 0.040 Uiso 1 1 calc R . . C20 C 0.83246(17) 0.10508(16) 0.23107(14) 0.0240(4) Uani 1 1 d . . . H20 H 0.8434 0.1627 0.2027 0.029 Uiso 1 1 calc R . . C21 C 0.61964(15) 0.30426(14) 0.20882(12) 0.0166(3) Uani 1 1 d . . . C22 C 0.64762(17) 0.25899(16) 0.12337(13) 0.0231(4) Uani 1 1 d . . . H22 H 0.6653 0.1883 0.1159 0.028 Uiso 1 1 calc R . . C23 C 0.6495(2) 0.3172(2) 0.04963(15) 0.0350(5) Uani 1 1 d . . . H23 H 0.6690 0.2863 -0.0084 0.042 Uiso 1 1 calc R . . C24 C 0.6229(2) 0.4206(2) 0.06054(16) 0.0396(6) Uani 1 1 d . . . H24 H 0.6243 0.4603 0.0099 0.047 Uiso 1 1 calc R . . C25 C 0.5944(2) 0.46634(18) 0.14514(17) 0.0351(5) Uani 1 1 d . . . H25 H 0.5758 0.5371 0.1523 0.042 Uiso 1 1 calc R . . C26 C 0.59300(18) 0.40836(15) 0.21909(14) 0.0239(4) Uani 1 1 d . . . H26 H 0.5739 0.4395 0.2770 0.029 Uiso 1 1 calc R . . C27 C 0.20505(15) 0.07281(12) 0.38371(11) 0.0136(3) Uani 1 1 d . . . C28 C 0.09801(16) 0.05292(14) 0.38076(12) 0.0175(3) Uani 1 1 d . . . H28 H 0.0322 0.1036 0.3638 0.021 Uiso 1 1 calc R . . C29 C 0.08837(18) -0.04087(14) 0.40272(13) 0.0207(4) Uani 1 1 d . . . H29 H 0.0157 -0.0539 0.4009 0.025 Uiso 1 1 calc R . . C30 C 0.18401(19) -0.11541(15) 0.42713(13) 0.0239(4) Uani 1 1 d . . . H30 H 0.1763 -0.1787 0.4436 0.029 Uiso 1 1 calc R . . C31 C 0.29153(18) -0.09739(14) 0.42755(13) 0.0220(4) Uani 1 1 d . . . H31 H 0.3579 -0.1492 0.4424 0.026 Uiso 1 1 calc R . . C32 C 0.30190(16) -0.00366(13) 0.40618(12) 0.0175(3) Uani 1 1 d . . . H32 H 0.3753 0.0084 0.4069 0.021 Uiso 1 1 calc R . . C33 C 0.13858(15) 0.26663(12) 0.47420(11) 0.0138(3) Uani 1 1 d . . . C34 C 0.04991(17) 0.23899(15) 0.52788(13) 0.0215(4) Uani 1 1 d . . . H34 H 0.0305 0.1819 0.5108 0.026 Uiso 1 1 calc R . . C35 C -0.01050(17) 0.29367(15) 0.60593(13) 0.0229(4) Uani 1 1 d . . . H35 H -0.0708 0.2738 0.6414 0.027 Uiso 1 1 calc R . . C36 C 0.01652(16) 0.37663(14) 0.63227(12) 0.0197(4) Uani 1 1 d . . . H36 H -0.0248 0.4140 0.6856 0.024 Uiso 1 1 calc R . . C37 C 0.10481(18) 0.40491(15) 0.57987(14) 0.0248(4) Uani 1 1 d . . . H37 H 0.1241 0.4618 0.5976 0.030 Uiso 1 1 calc R . . C38 C 0.16541(17) 0.35049(14) 0.50140(13) 0.0216(4) Uani 1 1 d . . . H38 H 0.2256 0.3707 0.4661 0.026 Uiso 1 1 calc R . . C39 C 0.11624(15) 0.25384(13) 0.28949(11) 0.0145(3) Uani 1 1 d . . . C40 C 0.11761(17) 0.19755(14) 0.21341(12) 0.0192(3) Uani 1 1 d . . . H40 H 0.1684 0.1299 0.2042 0.023 Uiso 1 1 calc R . . C41 C 0.04402(18) 0.24107(15) 0.15103(13) 0.0234(4) Uani 1 1 d . . . H41 H 0.0449 0.2029 0.0995 0.028 Uiso 1 1 calc R . . C42 C -0.02924(18) 0.33860(16) 0.16417(13) 0.0251(4) Uani 1 1 d . . . H42 H -0.0804 0.3672 0.1224 0.030 Uiso 1 1 calc R . . C43 C -0.02913(18) 0.39576(15) 0.23803(13) 0.0259(4) Uani 1 1 d . . . H43 H -0.0790 0.4637 0.2460 0.031 Uiso 1 1 calc R . . C44 C 0.04386(17) 0.35380(14) 0.30055(12) 0.0200(4) Uani 1 1 d . . . H44 H 0.0443 0.3934 0.3508 0.024 Uiso 1 1 calc R . . O7 O 0.41473(19) 0.19113(11) 0.82681(10) 0.0465(5) Uani 1 1 d . . . H7A H 0.4564 0.1313 0.8316 0.070 Uiso 1 1 calc R . . C45 C 0.3909(3) 0.20446(18) 0.74203(17) 0.0525(8) Uani 1 1 d . . . H45A H 0.3289 0.1735 0.7353 0.063 Uiso 1 1 calc R . . H45B H 0.4636 0.1662 0.7014 0.063 Uiso 1 1 calc R . . C46 C 0.3530(3) 0.3039(2) 0.71265(18) 0.0606(9) Uani 1 1 d . . . H46A H 0.3395 0.3023 0.6509 0.091 Uiso 1 1 calc R . . H46B H 0.4143 0.3355 0.7165 0.091 Uiso 1 1 calc R . . H46C H 0.2789 0.3427 0.7502 0.091 Uiso 1 1 calc R . . C48 C 0.2722(2) 0.84000(18) 0.18658(17) 0.0397(6) Uani 1 1 d . . . H48A H 0.3282 0.8729 0.2016 0.060 Uiso 1 1 calc R . . H48B H 0.1933 0.8735 0.2203 0.060 Uiso 1 1 calc R . . H48C H 0.2684 0.8444 0.1228 0.060 Uiso 1 1 calc R . . C47 C 0.3130(3) 0.73243(19) 0.2094(2) 0.0450(6) Uani 1 1 d . . . H47A H 0.3929 0.6982 0.1756 0.054 Uiso 1 1 calc R . . H47B H 0.3181 0.7275 0.2736 0.054 Uiso 1 1 calc R . . O8 O 0.2309(3) 0.68563(18) 0.1879(2) 0.0829(9) Uani 1 1 d . . . H8 H 0.2488 0.6270 0.2063 0.124 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01275(7) 0.00950(6) 0.01225(6) -0.00010(4) -0.00184(4) -0.00396(5) P1 0.0133(2) 0.01259(19) 0.0145(2) -0.00121(15) -0.00198(15) -0.00531(16) P2 0.01187(19) 0.00945(18) 0.01346(19) 0.00151(15) -0.00189(15) -0.00350(15) O1 0.0565(10) 0.0159(6) 0.0136(6) 0.0019(5) -0.0043(6) -0.0041(7) O2 0.0393(8) 0.0130(6) 0.0176(6) -0.0032(5) -0.0078(6) -0.0014(6) O3 0.0176(6) 0.0117(5) 0.0150(6) 0.0012(4) -0.0052(5) -0.0033(5) O4 0.0184(6) 0.0109(5) 0.0147(6) -0.0003(4) -0.0001(5) -0.0057(5) O5 0.0281(7) 0.0099(5) 0.0207(6) 0.0002(5) -0.0002(5) -0.0039(5) O6 0.0277(7) 0.0253(7) 0.0161(6) 0.0027(5) -0.0053(5) -0.0100(6) N1 0.0112(6) 0.0109(6) 0.0145(6) 0.0003(5) -0.0014(5) -0.0035(5) C1 0.0266(9) 0.0161(8) 0.0146(8) 0.0020(6) -0.0002(7) -0.0059(7) C2 0.0210(8) 0.0129(7) 0.0156(8) 0.0004(6) -0.0018(6) -0.0063(7) C3 0.0137(7) 0.0107(7) 0.0162(8) -0.0002(6) -0.0029(6) -0.0042(6) C4 0.0163(8) 0.0126(7) 0.0177(8) -0.0006(6) -0.0035(6) -0.0037(6) C5 0.0156(8) 0.0115(7) 0.0167(8) -0.0007(6) 0.0016(6) -0.0050(6) C6 0.0150(8) 0.0104(7) 0.0173(8) -0.0008(6) 0.0011(6) -0.0047(6) C7 0.0243(9) 0.0128(8) 0.0158(8) 0.0014(6) 0.0005(7) -0.0047(7) C8 0.0163(8) 0.0131(7) 0.0160(8) -0.0007(6) -0.0022(6) -0.0058(6) C9 0.0205(8) 0.0126(7) 0.0174(8) -0.0006(6) -0.0052(6) -0.0072(7) C10 0.0213(9) 0.0203(9) 0.0224(9) -0.0006(7) -0.0035(7) -0.0090(7) C11 0.0290(10) 0.0223(9) 0.0287(10) 0.0014(8) -0.0120(8) -0.0147(8) C12 0.0377(11) 0.0175(9) 0.0214(9) -0.0002(7) -0.0120(8) -0.0115(8) C13 0.0330(11) 0.0170(8) 0.0182(9) -0.0030(7) -0.0044(8) -0.0087(8) C14 0.0237(9) 0.0161(8) 0.0188(8) -0.0010(7) -0.0029(7) -0.0080(7) C15 0.0165(8) 0.0166(8) 0.0246(9) -0.0061(7) -0.0085(7) -0.0033(7) C16 0.0211(9) 0.0194(9) 0.0367(11) 0.0024(8) -0.0150(8) -0.0059(7) C17 0.0291(11) 0.0183(10) 0.0657(17) 0.0035(10) -0.0267(12) -0.0037(9) C18 0.0234(11) 0.0231(10) 0.0746(19) -0.0167(11) -0.0225(12) 0.0038(9) C19 0.0160(9) 0.0343(12) 0.0469(14) -0.0161(10) -0.0093(9) -0.0001(8) C20 0.0161(8) 0.0263(10) 0.0293(10) -0.0071(8) -0.0066(7) -0.0046(8) C21 0.0140(8) 0.0201(8) 0.0170(8) 0.0015(6) -0.0001(6) -0.0083(7) C22 0.0178(9) 0.0300(10) 0.0209(9) -0.0018(8) 0.0010(7) -0.0084(8) C23 0.0313(12) 0.0557(15) 0.0190(10) 0.0045(10) 0.0017(8) -0.0176(11) C24 0.0388(13) 0.0557(16) 0.0313(12) 0.0257(11) -0.0069(10) -0.0249(12) C25 0.0384(13) 0.0321(12) 0.0440(14) 0.0189(10) -0.0133(11) -0.0215(10) C26 0.0256(10) 0.0213(9) 0.0269(10) 0.0040(8) -0.0049(8) -0.0103(8) C27 0.0175(8) 0.0106(7) 0.0135(7) 0.0010(6) -0.0024(6) -0.0053(6) C28 0.0185(8) 0.0178(8) 0.0176(8) 0.0015(6) -0.0033(6) -0.0075(7) C29 0.0256(9) 0.0206(9) 0.0213(9) -0.0009(7) -0.0018(7) -0.0157(8) C30 0.0349(11) 0.0176(9) 0.0237(9) 0.0038(7) -0.0022(8) -0.0158(8) C31 0.0288(10) 0.0139(8) 0.0248(9) 0.0059(7) -0.0094(8) -0.0067(7) C32 0.0187(8) 0.0151(8) 0.0203(8) 0.0029(6) -0.0054(7) -0.0066(7) C33 0.0132(7) 0.0130(7) 0.0138(7) 0.0006(6) -0.0025(6) -0.0019(6) C34 0.0232(9) 0.0223(9) 0.0209(9) -0.0025(7) 0.0035(7) -0.0130(8) C35 0.0222(9) 0.0258(10) 0.0201(9) -0.0032(7) 0.0056(7) -0.0108(8) C36 0.0204(9) 0.0196(8) 0.0157(8) -0.0018(7) -0.0005(7) -0.0025(7) C37 0.0287(10) 0.0194(9) 0.0254(10) -0.0074(7) 0.0051(8) -0.0102(8) C38 0.0246(9) 0.0185(9) 0.0220(9) -0.0027(7) 0.0043(7) -0.0107(8) C39 0.0136(7) 0.0151(8) 0.0147(7) 0.0032(6) -0.0015(6) -0.0046(6) C40 0.0217(9) 0.0174(8) 0.0171(8) 0.0005(7) -0.0019(7) -0.0049(7) C41 0.0262(10) 0.0272(10) 0.0175(9) 0.0003(7) -0.0068(7) -0.0081(8) C42 0.0246(10) 0.0284(10) 0.0198(9) 0.0063(8) -0.0089(8) -0.0024(8) C43 0.0278(10) 0.0214(9) 0.0203(9) 0.0027(7) -0.0051(8) 0.0041(8) C44 0.0219(9) 0.0180(8) 0.0168(8) 0.0011(7) -0.0023(7) -0.0019(7) O7 0.0926(16) 0.0155(7) 0.0165(7) 0.0020(6) -0.0101(8) 0.0044(9) C45 0.100(2) 0.0243(11) 0.0319(13) -0.0009(10) -0.0401(15) -0.0044(13) C46 0.115(3) 0.0329(14) 0.0288(13) 0.0123(11) -0.0249(16) -0.0108(16) C48 0.0516(15) 0.0298(12) 0.0366(13) -0.0007(10) 0.0015(11) -0.0152(11) C47 0.0484(16) 0.0293(12) 0.0506(16) 0.0001(11) -0.0045(13) -0.0045(11) O8 0.132(2) 0.0531(14) 0.0878(19) 0.0421(14) -0.0420(18) -0.0533(16) _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 C8 1.8669(18) . ? Ru1 N1 2.0343(14) . ? Ru1 O3 2.1170(12) . ? Ru1 O4 2.1234(12) . ? Ru1 P2 2.3704(5) . ? Ru1 P1 2.3825(5) . ? P1 C21 1.8200(18) . ? P1 C15 1.8216(19) . ? P1 C9 1.8292(17) . ? P2 C27 1.8188(16) . ? P2 C39 1.8229(17) . ? P2 C33 1.8321(17) . ? O1 C1 1.334(2) . ? O1 H1 0.8400 . ? O2 C4 1.239(2) . ? O3 C4 1.292(2) . ? O4 C5 1.299(2) . ? O5 C5 1.231(2) . ? O6 C8 1.154(2) . ? N1 C3 1.334(2) . ? N1 C6 1.339(2) . ? C1 C7 1.403(2) . ? C1 C2 1.412(2) . ? C2 C3 1.385(2) . ? C2 H2 0.9500 . ? C3 C4 1.512(2) . ? C5 C6 1.515(2) . ? C6 C7 1.377(2) . ? C7 H7 0.9500 . ? C9 C14 1.400(3) . ? C9 C10 1.403(3) . ? C10 C11 1.387(3) . ? C10 H10 0.9500 . ? C11 C12 1.397(3) . ? C11 H11 0.9500 . ? C12 C13 1.378(3) . ? C12 H12 0.9500 . ? C13 C14 1.397(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.395(3) . ? C15 C20 1.399(3) . ? C16 C17 1.390(3) . ? C16 H16 0.9500 . ? C17 C18 1.363(4) . ? C17 H17 0.9500 . ? C18 C19 1.400(4) . ? C18 H18 0.9500 . ? C19 C20 1.389(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.397(3) . ? C21 C22 1.398(3) . ? C22 C23 1.386(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(4) . ? C23 H23 0.9500 . ? C24 C25 1.389(4) . ? C24 H24 0.9500 . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.396(2) . ? C27 C28 1.405(2) . ? C28 C29 1.391(2) . ? C28 H28 0.9500 . ? C29 C30 1.385(3) . ? C29 H29 0.9500 . ? C30 C31 1.392(3) . ? C30 H30 0.9500 . ? C31 C32 1.391(2) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.394(2) . ? C33 C34 1.396(2) . ? C34 C35 1.389(3) . ? C34 H34 0.9500 . ? C35 C36 1.380(3) . ? C35 H35 0.9500 . ? C36 C37 1.388(3) . ? C36 H36 0.9500 . ? C37 C38 1.394(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.393(2) . ? C39 C40 1.402(2) . ? C40 C41 1.401(3) . ? C40 H40 0.9500 . ? C41 C42 1.370(3) . ? C41 H41 0.9500 . ? C42 C43 1.386(3) . ? C42 H42 0.9500 . ? C43 C44 1.393(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? O7 C45 1.364(3) . ? O7 H7A 0.8400 . ? C45 C46 1.416(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C48 C47 1.489(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C47 O8 1.420(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? O8 H8 0.8400 . ? 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 C8 Ru1 N1 177.24(6) . . ? C8 Ru1 O3 101.39(6) . . ? N1 Ru1 O3 76.86(5) . . ? C8 Ru1 O4 104.97(6) . . ? N1 Ru1 O4 76.82(5) . . ? O3 Ru1 O4 153.64(5) . . ? C8 Ru1 P2 85.86(5) . . ? N1 Ru1 P2 92.04(4) . . ? O3 Ru1 P2 91.57(3) . . ? O4 Ru1 P2 90.66(3) . . ? C8 Ru1 P1 91.24(5) . . ? N1 Ru1 P1 90.99(4) . . ? O3 Ru1 P1 93.21(4) . . ? O4 Ru1 P1 85.94(3) . . ? P2 Ru1 P1 174.813(15) . . ? C21 P1 C15 106.15(9) . . ? C21 P1 C9 102.92(8) . . ? C15 P1 C9 104.75(8) . . ? C21 P1 Ru1 112.31(6) . . ? C15 P1 Ru1 114.64(6) . . ? C9 P1 Ru1 114.97(6) . . ? C27 P2 C39 105.06(8) . . ? C27 P2 C33 104.00(8) . . ? C39 P2 C33 103.94(8) . . ? C27 P2 Ru1 115.90(6) . . ? C39 P2 Ru1 114.47(6) . . ? C33 P2 Ru1 112.22(5) . . ? C1 O1 H1 109.5 . . ? C4 O3 Ru1 115.80(11) . . ? C5 O4 Ru1 116.08(10) . . ? C3 N1 C6 121.59(15) . . ? C3 N1 Ru1 119.22(11) . . ? C6 N1 Ru1 119.19(11) . . ? O1 C1 C7 117.23(16) . . ? O1 C1 C2 123.25(16) . . ? C7 C1 C2 119.51(16) . . ? C3 C2 C1 117.49(16) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? N1 C3 C2 121.73(15) . . ? N1 C3 C4 112.14(15) . . ? C2 C3 C4 126.13(15) . . ? O2 C4 O3 124.65(16) . . ? O2 C4 C3 119.38(16) . . ? O3 C4 C3 115.97(14) . . ? O5 C5 O4 124.05(16) . . ? O5 C5 C6 120.66(16) . . ? O4 C5 C6 115.29(14) . . ? N1 C6 C7 120.75(15) . . ? N1 C6 C5 112.53(15) . . ? C7 C6 C5 126.71(15) . . ? C6 C7 C1 118.91(16) . . ? C6 C7 H7 120.5 . . ? C1 C7 H7 120.5 . . ? O6 C8 Ru1 177.13(15) . . ? C14 C9 C10 119.01(16) . . ? C14 C9 P1 121.33(13) . . ? C10 C9 P1 119.65(14) . . ? C11 C10 C9 120.04(18) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.66(18) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 119.48(17) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.59(18) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C9 120.16(18) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? C16 C15 C20 119.03(18) . . ? C16 C15 P1 118.39(15) . . ? C20 C15 P1 122.58(15) . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 120.4(2) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.1(2) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.0(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C15 119.9(2) . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C26 C21 C22 119.49(18) . . ? C26 C21 P1 120.52(14) . . ? C22 C21 P1 119.62(15) . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0(2) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.3(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 120.3(2) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? C32 C27 C28 119.05(15) . . ? C32 C27 P2 119.44(12) . . ? C28 C27 P2 121.26(13) . . ? C29 C28 C27 120.07(17) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 120.42(17) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 119.87(17) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 120.13(18) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C27 120.40(16) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C38 C33 C34 118.07(16) . . ? C38 C33 P2 120.01(13) . . ? C34 C33 P2 121.89(13) . . ? C35 C34 C33 121.09(17) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C34 120.45(17) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 119.21(17) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C36 C37 C38 120.55(17) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C33 120.63(17) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C44 C39 C40 119.20(16) . . ? C44 C39 P2 120.71(13) . . ? C40 C39 P2 119.97(13) . . ? C41 C40 C39 119.94(17) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 120.13(18) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 120.41(18) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C42 C43 C44 120.20(18) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 120.08(17) . . ? C43 C44 H44 120.0 . . ? C39 C44 H44 120.0 . . ? C45 O7 H7A 109.5 . . ? O7 C45 C46 118.2(2) . . ? O7 C45 H45A 107.8 . . ? C46 C45 H45A 107.8 . . ? O7 C45 H45B 107.8 . . ? C46 C45 H45B 107.8 . . ? H45A C45 H45B 107.1 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O8 C47 C48 109.0(2) . . ? O8 C47 H47A 109.9 . . ? C48 C47 H47A 109.9 . . ? O8 C47 H47B 109.9 . . ? C48 C47 H47B 109.9 . . ? H47A C47 H47B 108.3 . . ? C47 O8 H8 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 Ru1 P1 C21 -162.80(8) . . . . ? N1 Ru1 P1 C21 18.83(8) . . . . ? O3 Ru1 P1 C21 95.72(7) . . . . ? O4 Ru1 P1 C21 -57.88(7) . . . . ? C8 Ru1 P1 C15 75.94(9) . . . . ? N1 Ru1 P1 C15 -102.43(8) . . . . ? O3 Ru1 P1 C15 -25.54(8) . . . . ? O4 Ru1 P1 C15 -179.14(8) . . . . ? C8 Ru1 P1 C9 -45.57(8) . . . . ? N1 Ru1 P1 C9 136.06(7) . . . . ? O3 Ru1 P1 C9 -147.05(7) . . . . ? O4 Ru1 P1 C9 59.35(7) . . . . ? C8 Ru1 P2 C27 -69.54(8) . . . . ? N1 Ru1 P2 C27 108.67(7) . . . . ? O3 Ru1 P2 C27 31.77(7) . . . . ? O4 Ru1 P2 C27 -174.50(7) . . . . ? C8 Ru1 P2 C39 167.88(8) . . . . ? N1 Ru1 P2 C39 -13.91(7) . . . . ? O3 Ru1 P2 C39 -90.81(7) . . . . ? O4 Ru1 P2 C39 62.92(7) . . . . ? C8 Ru1 P2 C33 49.73(8) . . . . ? N1 Ru1 P2 C33 -132.06(7) . . . . ? O3 Ru1 P2 C33 151.04(7) . . . . ? O4 Ru1 P2 C33 -55.23(7) . . . . ? C8 Ru1 O3 C4 177.62(12) . . . . ? N1 Ru1 O3 C4 -0.20(11) . . . . ? O4 Ru1 O3 C4 -3.13(18) . . . . ? P2 Ru1 O3 C4 91.53(11) . . . . ? P1 Ru1 O3 C4 -90.47(11) . . . . ? C8 Ru1 O4 C5 -175.12(12) . . . . ? N1 Ru1 O4 C5 2.71(11) . . . . ? O3 Ru1 O4 C5 5.64(18) . . . . ? P2 Ru1 O4 C5 -89.23(11) . . . . ? P1 Ru1 O4 C5 94.69(11) . . . . ? O3 Ru1 N1 C3 -0.64(12) . . . . ? O4 Ru1 N1 C3 178.03(13) . . . . ? P2 Ru1 N1 C3 -91.78(12) . . . . ? P1 Ru1 N1 C3 92.43(12) . . . . ? O3 Ru1 N1 C6 179.89(13) . . . . ? O4 Ru1 N1 C6 -1.45(12) . . . . ? P2 Ru1 N1 C6 88.75(12) . . . . ? P1 Ru1 N1 C6 -87.04(12) . . . . ? O1 C1 C2 C3 178.54(18) . . . . ? C7 C1 C2 C3 -0.3(3) . . . . ? C6 N1 C3 C2 1.6(2) . . . . ? Ru1 N1 C3 C2 -177.90(12) . . . . ? C6 N1 C3 C4 -179.30(14) . . . . ? Ru1 N1 C3 C4 1.23(18) . . . . ? C1 C2 C3 N1 -1.2(3) . . . . ? C1 C2 C3 C4 179.76(16) . . . . ? Ru1 O3 C4 O2 -178.19(15) . . . . ? Ru1 O3 C4 C3 0.89(19) . . . . ? N1 C3 C4 O2 177.76(16) . . . . ? C2 C3 C4 O2 -3.2(3) . . . . ? N1 C3 C4 O3 -1.4(2) . . . . ? C2 C3 C4 O3 177.71(16) . . . . ? Ru1 O4 C5 O5 176.53(14) . . . . ? Ru1 O4 C5 C6 -3.42(18) . . . . ? C3 N1 C6 C7 -0.3(2) . . . . ? Ru1 N1 C6 C7 179.15(13) . . . . ? C3 N1 C6 C5 -179.28(14) . . . . ? Ru1 N1 C6 C5 0.18(18) . . . . ? O5 C5 C6 N1 -177.77(15) . . . . ? O4 C5 C6 N1 2.2(2) . . . . ? O5 C5 C6 C7 3.3(3) . . . . ? O4 C5 C6 C7 -176.71(16) . . . . ? N1 C6 C7 C1 -1.2(3) . . . . ? C5 C6 C7 C1 177.64(17) . . . . ? O1 C1 C7 C6 -177.44(17) . . . . ? C2 C1 C7 C6 1.4(3) . . . . ? C21 P1 C9 C14 116.28(16) . . . . ? C15 P1 C9 C14 -132.90(16) . . . . ? Ru1 P1 C9 C14 -6.16(17) . . . . ? C21 P1 C9 C10 -62.17(16) . . . . ? C15 P1 C9 C10 48.65(17) . . . . ? Ru1 P1 C9 C10 175.39(12) . . . . ? C14 C9 C10 C11 1.1(3) . . . . ? P1 C9 C10 C11 179.56(15) . . . . ? C9 C10 C11 C12 0.7(3) . . . . ? C10 C11 C12 C13 -1.1(3) . . . . ? C11 C12 C13 C14 -0.4(3) . . . . ? C12 C13 C14 C9 2.2(3) . . . . ? C10 C9 C14 C13 -2.5(3) . . . . ? P1 C9 C14 C13 178.99(14) . . . . ? C21 P1 C15 C16 -155.52(14) . . . . ? C9 P1 C15 C16 96.01(15) . . . . ? Ru1 P1 C15 C16 -30.94(16) . . . . ? C21 P1 C15 C20 24.86(17) . . . . ? C9 P1 C15 C20 -83.61(16) . . . . ? Ru1 P1 C15 C20 149.44(13) . . . . ? C20 C15 C16 C17 -0.3(3) . . . . ? P1 C15 C16 C17 -179.94(16) . . . . ? C15 C16 C17 C18 -0.2(3) . . . . ? C16 C17 C18 C19 0.2(4) . . . . ? C17 C18 C19 C20 0.5(3) . . . . ? C18 C19 C20 C15 -1.0(3) . . . . ? C16 C15 C20 C19 0.9(3) . . . . ? P1 C15 C20 C19 -179.44(15) . . . . ? C15 P1 C21 C26 -142.26(15) . . . . ? C9 P1 C21 C26 -32.49(17) . . . . ? Ru1 P1 C21 C26 91.73(15) . . . . ? C15 P1 C21 C22 44.79(16) . . . . ? C9 P1 C21 C22 154.56(14) . . . . ? Ru1 P1 C21 C22 -81.22(15) . . . . ? C26 C21 C22 C23 0.4(3) . . . . ? P1 C21 C22 C23 173.42(16) . . . . ? C21 C22 C23 C24 -0.4(3) . . . . ? C22 C23 C24 C25 0.0(4) . . . . ? C23 C24 C25 C26 0.3(3) . . . . ? C24 C25 C26 C21 -0.3(3) . . . . ? C22 C21 C26 C25 -0.1(3) . . . . ? P1 C21 C26 C25 -173.01(16) . . . . ? C39 P2 C27 C32 151.55(14) . . . . ? C33 P2 C27 C32 -99.53(15) . . . . ? Ru1 P2 C27 C32 24.14(16) . . . . ? C39 P2 C27 C28 -34.15(16) . . . . ? C33 P2 C27 C28 74.76(15) . . . . ? Ru1 P2 C27 C28 -161.57(12) . . . . ? C32 C27 C28 C29 2.0(3) . . . . ? P2 C27 C28 C29 -172.33(14) . . . . ? C27 C28 C29 C30 -0.3(3) . . . . ? C28 C29 C30 C31 -1.7(3) . . . . ? C29 C30 C31 C32 2.0(3) . . . . ? C30 C31 C32 C27 -0.4(3) . . . . ? C28 C27 C32 C31 -1.6(3) . . . . ? P2 C27 C32 C31 172.79(15) . . . . ? C27 P2 C33 C38 155.67(15) . . . . ? C39 P2 C33 C38 -94.58(16) . . . . ? Ru1 P2 C33 C38 29.64(16) . . . . ? C27 P2 C33 C34 -26.38(17) . . . . ? C39 P2 C33 C34 83.36(16) . . . . ? Ru1 P2 C33 C34 -152.41(14) . . . . ? C38 C33 C34 C35 0.4(3) . . . . ? P2 C33 C34 C35 -177.62(15) . . . . ? C33 C34 C35 C36 -0.3(3) . . . . ? C34 C35 C36 C37 0.0(3) . . . . ? C35 C36 C37 C38 0.2(3) . . . . ? C36 C37 C38 C33 -0.1(3) . . . . ? C34 C33 C38 C37 -0.2(3) . . . . ? P2 C33 C38 C37 177.85(16) . . . . ? C27 P2 C39 C44 139.35(15) . . . . ? C33 P2 C39 C44 30.38(16) . . . . ? Ru1 P2 C39 C44 -92.37(15) . . . . ? C27 P2 C39 C40 -44.68(16) . . . . ? C33 P2 C39 C40 -153.64(14) . . . . ? Ru1 P2 C39 C40 83.61(14) . . . . ? C44 C39 C40 C41 -1.9(3) . . . . ? P2 C39 C40 C41 -177.98(14) . . . . ? C39 C40 C41 C42 0.1(3) . . . . ? C40 C41 C42 C43 1.6(3) . . . . ? C41 C42 C43 C44 -1.3(3) . . . . ? C42 C43 C44 C39 -0.6(3) . . . . ? C40 C39 C44 C43 2.2(3) . . . . ? P2 C39 C44 C43 178.22(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O7 0.84 1.73 2.558(2) 169.3 1_554 O7 H7A O2 0.84 1.83 2.644(2) 161.3 2_656 O8 H8 O5 0.84 1.90 2.733(2) 170.0 . _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.92 _refine_diff_density_min -1.14 _refine_diff_density_rms 0.107 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.000 -0.001 0.000 368 74 ' ' _platon_squeeze_details ; The appearance of difference maps suggested disordered chloroform, which was used in crystallization, along with ethanol. The 74 electrons removed by SQUEEZE corresponds to 1.28 molecules of CHCl~3~ per cell, or 0.64 per complex. This solvent is included in the formula, FW, density, etc., but is not in the model. ; # END OF CIF # Attachment '- [RuIII-hpa-P].txt' data_3PA _database_code_depnum_ccdc_archive 'CCDC 797112' #TrackingRef '- [RuIII-hpa-P].txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H33 Cl N O5 P2 Ru, 0.90(C2 H3 N), 0.10(C H2 Cl2)' _chemical_formula_sum 'C44.90 H35.90 Cl1.20 N1.90 O5 P2 Ru' _chemical_formula_weight 887.61 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_cell_setting Triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0311(15) _cell_length_b 13.5729(15) _cell_length_c 13.996(2) _cell_angle_alpha 84.593(7) _cell_angle_beta 71.947(6) _cell_angle_gamma 64.431(7) _cell_volume 1958.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(5) _cell_measurement_reflns_used 12349 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 32.0 _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53880 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 32.0 _reflns_number_total 13603 _reflns_number_gt 10568 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0731P)^2^+0.2151P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13603 _refine_ls_number_parameters 530 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.065 _refine_ls_R_factor_gt 0.040 _refine_ls_wR_factor_ref 0.129 _refine_ls_wR_factor_gt 0.102 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.005 _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 0.480104(16) 0.290127(13) 0.707944(12) 0.01060(5) Uani 1 1 d . . . Cl1 Cl 0.45093(5) 0.46627(4) 0.65584(4) 0.01704(11) Uani 1 1 d . . . P1 P 0.68327(5) 0.26138(5) 0.72685(4) 0.01198(11) Uani 1 1 d . . . P2 P 0.26904(5) 0.33790(4) 0.69725(4) 0.01085(11) Uani 1 1 d . . . O1 O 0.5968(2) -0.18503(14) 0.80697(13) 0.0274(4) Uani 1 1 d . . . H1 H 0.5924 -0.1934 0.8666 0.041 Uiso 1 1 calc R . . O2 O 0.64252(17) 0.04867(13) 0.48706(12) 0.0201(4) Uani 1 1 d . . . O3 O 0.56084(15) 0.21093(12) 0.56937(11) 0.0140(3) Uani 1 1 d . . . O4 O 0.41540(15) 0.29719(12) 0.86433(11) 0.0134(3) Uani 1 1 d . . . O5 O 0.38710(17) 0.19955(13) 1.00113(12) 0.0191(3) Uani 1 1 d . . . N1 N 0.50962(17) 0.13488(15) 0.74165(13) 0.0118(3) Uani 1 1 d . . . C1 C 0.5634(2) -0.07835(18) 0.78728(17) 0.0183(5) Uani 1 1 d . . . C2 C 0.5924(2) -0.05004(18) 0.68678(17) 0.0173(4) Uani 1 1 d . . . H2 H 0.6297 -0.1028 0.6347 0.021 Uiso 1 1 calc R . . C3 C 0.5643(2) 0.05829(18) 0.66694(16) 0.0135(4) Uani 1 1 d . . . C4 C 0.5933(2) 0.10527(18) 0.56428(16) 0.0145(4) Uani 1 1 d . . . C5 C 0.4213(2) 0.20775(18) 0.90948(16) 0.0140(4) Uani 1 1 d . . . C6 C 0.4773(2) 0.10988(17) 0.83787(15) 0.0134(4) Uani 1 1 d . . . C7 C 0.5010(2) 0.00375(18) 0.86393(17) 0.0176(4) Uani 1 1 d . . . H7 H 0.4761 -0.0129 0.9309 0.021 Uiso 1 1 calc R . . C8 C 0.7944(3) 0.4510(2) 0.85244(18) 0.0213(5) Uani 1 1 d . . . H8 H 0.8716 0.4471 0.8573 0.026 Uiso 1 1 calc R . . C9 C 0.7955(2) 0.36946(19) 0.79848(18) 0.0190(5) Uani 1 1 d . . . H9 H 0.8735 0.3119 0.7664 0.023 Uiso 1 1 calc R . . C10 C 0.6797(2) 0.37362(18) 0.79211(16) 0.0139(4) Uani 1 1 d . . . C11 C 0.5636(2) 0.46035(18) 0.84179(17) 0.0168(4) Uani 1 1 d . . . H11 H 0.4856 0.4628 0.8405 0.020 Uiso 1 1 calc R . . C12 C 0.5640(3) 0.5431(2) 0.89313(17) 0.0215(5) Uani 1 1 d . . . H12 H 0.4866 0.6021 0.9236 0.026 Uiso 1 1 calc R . . C13 C 0.6787(3) 0.5380(2) 0.89905(18) 0.0232(5) Uani 1 1 d . . . H13 H 0.6784 0.5930 0.9343 0.028 Uiso 1 1 calc R . . C14 C 1.0415(3) 0.1380(2) 0.5156(2) 0.0255(5) Uani 1 1 d . . . H14 H 1.1263 0.0915 0.5129 0.031 Uiso 1 1 calc R . . C15 C 0.9434(2) 0.1603(2) 0.60617(19) 0.0205(5) Uani 1 1 d . . . H15 H 0.9625 0.1283 0.6642 0.025 Uiso 1 1 calc R . . C16 C 0.8159(2) 0.23055(19) 0.61047(17) 0.0160(4) Uani 1 1 d . . . C17 C 0.7881(2) 0.2789(2) 0.52314(17) 0.0194(5) Uani 1 1 d . . . H17 H 0.7037 0.3262 0.5255 0.023 Uiso 1 1 calc R . . C18 C 0.8871(3) 0.2562(2) 0.43241(19) 0.0252(5) Uani 1 1 d . . . H18 H 0.8688 0.2884 0.3742 0.030 Uiso 1 1 calc R . . C19 C 1.0122(3) 0.1858(2) 0.4291(2) 0.0272(6) Uani 1 1 d . . . H19 H 1.0776 0.1701 0.3682 0.033 Uiso 1 1 calc R . . C20 C 0.7975(2) 0.04008(19) 0.76644(18) 0.0199(5) Uani 1 1 d . . . H20 H 0.8159 0.0268 0.6980 0.024 Uiso 1 1 calc R . . C21 C 0.7386(2) 0.14724(18) 0.80594(16) 0.0146(4) Uani 1 1 d . . . C22 C 0.7121(2) 0.1653(2) 0.90897(18) 0.0190(5) Uani 1 1 d . . . H22 H 0.6736 0.2365 0.9361 0.023 Uiso 1 1 calc R . . C23 C 0.7427(3) 0.0781(2) 0.97107(19) 0.0240(5) Uani 1 1 d . . . H23 H 0.7249 0.0908 1.0395 0.029 Uiso 1 1 calc R . . C24 C 0.7998(3) -0.0281(2) 0.9313(2) 0.0287(6) Uani 1 1 d . . . H24 H 0.8186 -0.0866 0.9732 0.034 Uiso 1 1 calc R . . C25 C 0.8286(3) -0.0470(2) 0.8293(2) 0.0270(6) Uani 1 1 d . . . H25 H 0.8692 -0.1184 0.8024 0.032 Uiso 1 1 calc R . . C26 C 0.1503(2) 0.46692(17) 0.76670(16) 0.0134(4) Uani 1 1 d . . . C27 C 0.1646(2) 0.49700(19) 0.85303(17) 0.0197(5) Uani 1 1 d . . . H27 H 0.2372 0.4534 0.8730 0.024 Uiso 1 1 calc R . . C28 C 0.0714(2) 0.5916(2) 0.90965(18) 0.0222(5) Uani 1 1 d . . . H28 H 0.0822 0.6110 0.9670 0.027 Uiso 1 1 calc R . . C29 C -0.0378(2) 0.65721(19) 0.88097(18) 0.0190(5) Uani 1 1 d . . . H29 H -0.1012 0.7194 0.9199 0.023 Uiso 1 1 calc R . . C30 C -0.0515(2) 0.6295(2) 0.79425(19) 0.0215(5) Uani 1 1 d . . . H30 H -0.1238 0.6741 0.7742 0.026 Uiso 1 1 calc R . . C31 C 0.0421(2) 0.53504(19) 0.73628(18) 0.0187(5) Uani 1 1 d . . . H31 H 0.0326 0.5175 0.6776 0.022 Uiso 1 1 calc R . . C32 C 0.2494(2) 0.35665(17) 0.57181(16) 0.0130(4) Uani 1 1 d . . . C33 C 0.3277(2) 0.39495(19) 0.49714(17) 0.0174(4) Uani 1 1 d . . . H33 H 0.3947 0.4035 0.5096 0.021 Uiso 1 1 calc R . . C34 C 0.3050(2) 0.4202(2) 0.40444(17) 0.0212(5) Uani 1 1 d . . . H34 H 0.3565 0.4464 0.3552 0.025 Uiso 1 1 calc R . . C35 C 0.2062(3) 0.4067(2) 0.38485(18) 0.0220(5) Uani 1 1 d . . . H35 H 0.1918 0.4235 0.3225 0.026 Uiso 1 1 calc R . . C36 C 0.1288(3) 0.3680(2) 0.45846(18) 0.0215(5) Uani 1 1 d . . . H36 H 0.0625 0.3590 0.4454 0.026 Uiso 1 1 calc R . . C37 C 0.1503(2) 0.34273(19) 0.55177(17) 0.0167(4) Uani 1 1 d . . . H37 H 0.0985 0.3166 0.6008 0.020 Uiso 1 1 calc R . . C38 C 0.2032(2) 0.23971(17) 0.75088(16) 0.0123(4) Uani 1 1 d . . . C39 C 0.2442(2) 0.14186(18) 0.69628(16) 0.0157(4) Uani 1 1 d . . . H39 H 0.3050 0.1274 0.6330 0.019 Uiso 1 1 calc R . . C40 C 0.1942(2) 0.06696(19) 0.73667(18) 0.0178(4) Uani 1 1 d . . . H40 H 0.2222 0.0023 0.7004 0.021 Uiso 1 1 calc R . . C41 C 0.1024(2) 0.08781(19) 0.83119(17) 0.0182(4) Uani 1 1 d . . . H41 H 0.0683 0.0378 0.8574 0.022 Uiso 1 1 calc R . . C42 C 0.0623(2) 0.18339(19) 0.88585(17) 0.0177(4) Uani 1 1 d . . . H42 H 0.0009 0.1977 0.9488 0.021 Uiso 1 1 calc R . . C43 C 0.1137(2) 0.25801(18) 0.84680(16) 0.0149(4) Uani 1 1 d . . . H43 H 0.0883 0.3208 0.8849 0.018 Uiso 1 1 calc R . . C44 C 0.6355(4) 0.2459(3) 0.2997(3) 0.0429(10) Uani 0.899(2) 1 d P A 1 H44A H 0.5649 0.2418 0.2846 0.064 Uiso 0.899(2) 1 calc PR A 1 H44B H 0.6093 0.3185 0.3246 0.064 Uiso 0.899(2) 1 calc PR A 1 H44C H 0.6600 0.1947 0.3498 0.064 Uiso 0.899(2) 1 calc PR A 1 C45 C 0.7440(4) 0.2197(3) 0.2095(3) 0.0351(8) Uani 0.899(2) 1 d P A 1 N2 N 0.8286(4) 0.1986(3) 0.1380(3) 0.0603(11) Uani 0.899(2) 1 d P A 1 Cl2 Cl 0.5830(7) 0.2209(5) 0.2484(5) 0.0300(19) Uani 0.101(2) 1 d P A 2 Cl3 Cl 0.8518(8) 0.1860(7) 0.2162(6) 0.041(2) Uani 0.101(2) 1 d P A 2 C46 C 0.692(2) 0.233(2) 0.3025(18) 0.010(4) Uiso 0.101(2) 1 d P A 2 H46A H 0.6942 0.1908 0.3623 0.012 Uiso 0.101(2) 1 calc PR A 2 H46B H 0.6617 0.3090 0.3226 0.012 Uiso 0.101(2) 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 Ru1 0.01179(9) 0.01012(9) 0.00827(8) 0.00173(6) -0.00279(6) -0.00360(6) Cl1 0.0193(3) 0.0145(2) 0.0183(2) 0.00468(19) -0.0070(2) -0.0080(2) P1 0.0121(3) 0.0123(2) 0.0103(2) 0.00099(19) -0.0038(2) -0.0038(2) P2 0.0112(2) 0.0111(2) 0.0087(2) 0.00147(18) -0.00294(19) -0.0037(2) O1 0.0510(13) 0.0123(8) 0.0134(8) 0.0033(6) -0.0092(8) -0.0092(8) O2 0.0281(9) 0.0162(8) 0.0109(7) -0.0005(6) -0.0028(7) -0.0066(7) O3 0.0170(8) 0.0130(7) 0.0102(7) 0.0022(6) -0.0025(6) -0.0062(6) O4 0.0165(8) 0.0112(7) 0.0093(7) 0.0016(5) -0.0031(6) -0.0036(6) O5 0.0273(9) 0.0155(8) 0.0086(7) 0.0019(6) -0.0023(6) -0.0062(7) N1 0.0128(8) 0.0113(8) 0.0097(8) 0.0010(6) -0.0037(7) -0.0035(7) C1 0.0266(12) 0.0108(10) 0.0135(10) 0.0013(8) -0.0059(9) -0.0046(9) C2 0.0216(11) 0.0132(10) 0.0137(10) -0.0006(8) -0.0049(9) -0.0042(9) C3 0.0139(10) 0.0145(10) 0.0096(9) -0.0003(7) -0.0019(7) -0.0048(8) C4 0.0135(10) 0.0161(10) 0.0117(9) 0.0000(8) -0.0031(8) -0.0048(8) C5 0.0148(10) 0.0125(10) 0.0117(9) 0.0004(7) -0.0037(8) -0.0033(8) C6 0.0165(10) 0.0132(10) 0.0080(8) 0.0015(7) -0.0029(8) -0.0048(8) C7 0.0245(12) 0.0143(10) 0.0113(9) 0.0014(8) -0.0038(9) -0.0070(9) C8 0.0290(13) 0.0225(12) 0.0208(11) 0.0041(9) -0.0134(10) -0.0152(10) C9 0.0226(12) 0.0170(11) 0.0179(11) 0.0016(9) -0.0084(9) -0.0076(9) C10 0.0178(10) 0.0135(10) 0.0109(9) 0.0019(7) -0.0050(8) -0.0069(8) C11 0.0190(11) 0.0152(10) 0.0137(10) 0.0011(8) -0.0036(8) -0.0060(9) C12 0.0280(13) 0.0165(11) 0.0141(10) -0.0031(8) -0.0017(9) -0.0066(10) C13 0.0395(15) 0.0194(12) 0.0173(11) 0.0014(9) -0.0111(10) -0.0168(11) C14 0.0175(12) 0.0241(13) 0.0273(13) -0.0068(10) 0.0015(10) -0.0061(10) C15 0.0160(11) 0.0220(12) 0.0209(11) -0.0017(9) -0.0040(9) -0.0064(9) C16 0.0165(10) 0.0171(10) 0.0146(10) -0.0042(8) -0.0020(8) -0.0081(8) C17 0.0184(11) 0.0232(12) 0.0154(10) 0.0013(9) -0.0025(9) -0.0095(9) C18 0.0291(14) 0.0320(14) 0.0158(11) 0.0008(10) -0.0025(10) -0.0170(11) C19 0.0257(13) 0.0298(14) 0.0205(12) -0.0081(10) 0.0059(10) -0.0138(11) C20 0.0251(12) 0.0150(11) 0.0174(11) -0.0008(8) -0.0110(9) -0.0030(9) C21 0.0161(10) 0.0129(10) 0.0146(10) 0.0028(8) -0.0078(8) -0.0042(8) C22 0.0226(12) 0.0156(11) 0.0182(11) 0.0016(8) -0.0071(9) -0.0071(9) C23 0.0352(15) 0.0217(12) 0.0166(11) 0.0042(9) -0.0135(10) -0.0101(11) C24 0.0432(17) 0.0178(12) 0.0263(13) 0.0063(10) -0.0200(12) -0.0085(11) C25 0.0386(16) 0.0154(11) 0.0250(13) 0.0010(10) -0.0170(12) -0.0045(11) C26 0.0132(10) 0.0120(9) 0.0124(9) 0.0010(7) -0.0017(8) -0.0045(8) C27 0.0181(11) 0.0192(11) 0.0161(10) -0.0019(9) -0.0073(9) -0.0008(9) C28 0.0244(12) 0.0216(12) 0.0142(10) -0.0045(9) -0.0049(9) -0.0036(10) C29 0.0197(11) 0.0131(10) 0.0179(10) -0.0017(8) -0.0024(9) -0.0031(9) C30 0.0190(11) 0.0160(11) 0.0243(12) 0.0001(9) -0.0084(10) -0.0014(9) C31 0.0207(11) 0.0159(11) 0.0189(11) 0.0000(8) -0.0092(9) -0.0050(9) C32 0.0146(10) 0.0123(9) 0.0105(9) 0.0002(7) -0.0044(8) -0.0037(8) C33 0.0192(11) 0.0218(11) 0.0137(10) 0.0052(8) -0.0067(8) -0.0104(9) C34 0.0248(12) 0.0276(13) 0.0137(10) 0.0078(9) -0.0066(9) -0.0142(10) C35 0.0272(13) 0.0260(13) 0.0153(10) 0.0076(9) -0.0114(10) -0.0116(10) C36 0.0251(12) 0.0279(13) 0.0191(11) 0.0056(9) -0.0132(10) -0.0146(10) C37 0.0178(11) 0.0185(11) 0.0158(10) 0.0038(8) -0.0063(8) -0.0095(9) C38 0.0117(9) 0.0112(9) 0.0128(9) 0.0023(7) -0.0044(7) -0.0036(7) C39 0.0170(11) 0.0153(10) 0.0115(9) -0.0001(8) -0.0027(8) -0.0047(8) C40 0.0219(12) 0.0148(10) 0.0178(10) 0.0014(8) -0.0073(9) -0.0080(9) C41 0.0226(12) 0.0185(11) 0.0157(10) 0.0057(8) -0.0055(9) -0.0119(9) C42 0.0172(11) 0.0193(11) 0.0130(10) 0.0035(8) -0.0024(8) -0.0065(9) C43 0.0165(10) 0.0148(10) 0.0114(9) -0.0002(8) -0.0034(8) -0.0052(8) C44 0.047(3) 0.0242(17) 0.041(2) -0.0023(15) 0.0065(19) -0.0124(18) C45 0.049(2) 0.0247(16) 0.0304(17) -0.0020(13) -0.0018(15) -0.0204(15) N2 0.081(3) 0.057(2) 0.043(2) -0.0153(17) 0.0162(19) -0.050(2) Cl2 0.033(4) 0.022(3) 0.034(4) -0.007(3) -0.016(3) -0.005(3) Cl3 0.038(4) 0.056(5) 0.037(4) -0.020(3) 0.011(3) -0.038(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.0147(18) . ? Ru1 O3 2.0456(15) . ? Ru1 O4 2.0796(15) . ? Ru1 Cl1 2.3403(6) . ? Ru1 P2 2.3848(6) . ? Ru1 P1 2.3990(7) . ? P1 C21 1.820(2) . ? P1 C16 1.821(2) . ? P1 C10 1.827(2) . ? P2 C38 1.823(2) . ? P2 C32 1.823(2) . ? P2 C26 1.831(2) . ? O1 C1 1.351(3) . ? O1 H1 0.8200 . ? O2 C4 1.215(3) . ? O3 C4 1.316(3) . ? O4 C5 1.299(3) . ? O5 C5 1.230(3) . ? N1 C6 1.335(3) . ? N1 C3 1.340(3) . ? C1 C2 1.399(3) . ? C1 C7 1.400(3) . ? C2 C3 1.380(3) . ? C2 H2 0.9300 . ? C3 C4 1.517(3) . ? C5 C6 1.511(3) . ? C6 C7 1.378(3) . ? C7 H7 0.9300 . ? C8 C13 1.387(4) . ? C8 C9 1.391(3) . ? C8 H8 0.9300 . ? C9 C10 1.401(3) . ? C9 H9 0.9300 . ? C10 C11 1.398(3) . ? C11 C12 1.392(3) . ? C11 H11 0.9300 . ? C12 C13 1.380(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.389(3) . ? C14 C19 1.389(4) . ? C14 H14 0.9300 . ? C15 C16 1.399(3) . ? C15 H15 0.9300 . ? C16 C17 1.396(3) . ? C17 C18 1.395(3) . ? C17 H17 0.9300 . ? C18 C19 1.380(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.392(3) . ? C20 C21 1.394(3) . ? C20 H20 0.9300 . ? C21 C22 1.398(3) . ? C22 C23 1.386(3) . ? C22 H22 0.9300 . ? C23 C24 1.386(4) . ? C23 H23 0.9300 . ? C24 C25 1.382(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.392(3) . ? C26 C31 1.400(3) . ? C27 C28 1.390(3) . ? C27 H27 0.9300 . ? C28 C29 1.389(3) . ? C28 H28 0.9300 . ? C29 C30 1.381(3) . ? C29 H29 0.9300 . ? C30 C31 1.398(3) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C37 1.396(3) . ? C32 C33 1.400(3) . ? C33 C34 1.389(3) . ? C33 H33 0.9300 . ? C34 C35 1.387(4) . ? C34 H34 0.9300 . ? C35 C36 1.389(4) . ? C35 H35 0.9300 . ? C36 C37 1.392(3) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C43 1.399(3) . ? C38 C39 1.408(3) . ? C39 C40 1.387(3) . ? C39 H39 0.9300 . ? C40 C41 1.395(3) . ? C40 H40 0.9300 . ? C41 C42 1.385(3) . ? C41 H41 0.9300 . ? C42 C43 1.390(3) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C45 1.444(5) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 N2 1.136(5) . ? Cl2 C46 1.77(2) . ? Cl3 C46 1.79(3) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 O3 77.20(7) . . ? N1 Ru1 O4 76.56(7) . . ? O3 Ru1 O4 153.75(6) . . ? N1 Ru1 Cl1 175.63(5) . . ? O3 Ru1 Cl1 98.45(5) . . ? O4 Ru1 Cl1 107.79(4) . . ? N1 Ru1 P2 93.09(5) . . ? O3 Ru1 P2 90.54(5) . . ? O4 Ru1 P2 91.91(5) . . ? Cl1 Ru1 P2 86.47(2) . . ? N1 Ru1 P1 91.79(5) . . ? O3 Ru1 P1 94.23(5) . . ? O4 Ru1 P1 85.55(5) . . ? Cl1 Ru1 P1 88.95(2) . . ? P2 Ru1 P1 173.83(2) . . ? C21 P1 C16 105.29(11) . . ? C21 P1 C10 102.36(10) . . ? C16 P1 C10 106.31(10) . . ? C21 P1 Ru1 111.39(8) . . ? C16 P1 Ru1 115.32(8) . . ? C10 P1 Ru1 114.94(8) . . ? C38 P2 C32 104.05(10) . . ? C38 P2 C26 104.19(10) . . ? C32 P2 C26 104.20(10) . . ? C38 P2 Ru1 114.26(7) . . ? C32 P2 Ru1 116.85(8) . . ? C26 P2 Ru1 111.99(8) . . ? C1 O1 H1 109.5 . . ? C4 O3 Ru1 118.62(13) . . ? C5 O4 Ru1 118.13(13) . . ? C6 N1 C3 121.36(19) . . ? C6 N1 Ru1 119.45(14) . . ? C3 N1 Ru1 119.17(14) . . ? O1 C1 C2 118.4(2) . . ? O1 C1 C7 122.1(2) . . ? C2 C1 C7 119.5(2) . . ? C3 C2 C1 118.3(2) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? N1 C3 C2 121.1(2) . . ? N1 C3 C4 112.13(19) . . ? C2 C3 C4 126.71(19) . . ? O2 C4 O3 125.2(2) . . ? O2 C4 C3 122.0(2) . . ? O3 C4 C3 112.87(18) . . ? O5 C5 O4 125.3(2) . . ? O5 C5 C6 121.3(2) . . ? O4 C5 C6 113.38(18) . . ? N1 C6 C7 121.1(2) . . ? N1 C6 C5 112.47(18) . . ? C7 C6 C5 126.39(19) . . ? C6 C7 C1 118.5(2) . . ? C6 C7 H7 120.7 . . ? C1 C7 H7 120.7 . . ? C13 C8 C9 120.2(2) . . ? C13 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 120.3(2) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 118.7(2) . . ? C11 C10 P1 121.79(18) . . ? C9 C10 P1 119.33(17) . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.3(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 120.0(2) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C15 C14 C19 119.5(2) . . ? C15 C14 H14 120.2 . . ? C19 C14 H14 120.2 . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 119.5(2) . . ? C17 C16 P1 118.35(18) . . ? C15 C16 P1 122.15(18) . . ? C18 C17 C16 119.9(2) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 120.0(2) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C14 120.8(2) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? C25 C20 C21 120.1(2) . . ? C25 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 119.0(2) . . ? C20 C21 P1 120.29(17) . . ? C22 C21 P1 120.47(17) . . ? C23 C22 C21 120.5(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 119.9(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C20 120.4(2) . . ? C24 C25 H25 119.8 . . ? C20 C25 H25 119.8 . . ? C27 C26 C31 118.9(2) . . ? C27 C26 P2 120.01(17) . . ? C31 C26 P2 121.04(17) . . ? C28 C27 C26 120.6(2) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C27 120.3(2) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 119.6(2) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 120.6(2) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C26 120.0(2) . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C37 C32 C33 119.5(2) . . ? C37 C32 P2 120.92(17) . . ? C33 C32 P2 119.29(17) . . ? C34 C33 C32 119.9(2) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 120.5(2) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.9(2) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C37 120.2(2) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C32 120.0(2) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C43 C38 C39 118.6(2) . . ? C43 C38 P2 121.49(17) . . ? C39 C38 P2 119.91(17) . . ? C40 C39 C38 120.1(2) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 120.6(2) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C42 C41 C40 119.7(2) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 120.1(2) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C42 C43 C38 120.8(2) . . ? C42 C43 H43 119.6 . . ? C38 C43 H43 119.6 . . ? N2 C45 C44 179.1(5) . . ? Cl2 C46 Cl3 111.7(13) . . ? Cl2 C46 H46A 109.3 . . ? Cl3 C46 H46A 109.3 . . ? Cl2 C46 H46B 109.3 . . ? Cl3 C46 H46B 109.3 . . ? H46A C46 H46B 107.9 . . ? 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 N1 Ru1 P1 C21 -22.51(9) . . . . ? O3 Ru1 P1 C21 -99.81(9) . . . . ? O4 Ru1 P1 C21 53.86(9) . . . . ? Cl1 Ru1 P1 C21 161.80(8) . . . . ? N1 Ru1 P1 C16 97.41(10) . . . . ? O3 Ru1 P1 C16 20.11(10) . . . . ? O4 Ru1 P1 C16 173.78(10) . . . . ? Cl1 Ru1 P1 C16 -78.28(9) . . . . ? N1 Ru1 P1 C10 -138.35(9) . . . . ? O3 Ru1 P1 C10 144.35(9) . . . . ? O4 Ru1 P1 C10 -61.97(9) . . . . ? Cl1 Ru1 P1 C10 45.96(8) . . . . ? N1 Ru1 P2 C38 14.47(9) . . . . ? O3 Ru1 P2 C38 91.68(9) . . . . ? O4 Ru1 P2 C38 -62.17(9) . . . . ? Cl1 Ru1 P2 C38 -169.89(8) . . . . ? N1 Ru1 P2 C32 -107.30(10) . . . . ? O3 Ru1 P2 C32 -30.09(9) . . . . ? O4 Ru1 P2 C32 176.06(9) . . . . ? Cl1 Ru1 P2 C32 68.34(8) . . . . ? N1 Ru1 P2 C26 132.63(9) . . . . ? O3 Ru1 P2 C26 -150.15(9) . . . . ? O4 Ru1 P2 C26 55.99(9) . . . . ? Cl1 Ru1 P2 C26 -51.72(8) . . . . ? N1 Ru1 O3 C4 -0.33(15) . . . . ? O4 Ru1 O3 C4 2.0(2) . . . . ? Cl1 Ru1 O3 C4 -179.88(15) . . . . ? P2 Ru1 O3 C4 -93.38(15) . . . . ? P1 Ru1 O3 C4 90.55(15) . . . . ? N1 Ru1 O4 C5 -0.45(16) . . . . ? O3 Ru1 O4 C5 -2.8(2) . . . . ? Cl1 Ru1 O4 C5 179.18(14) . . . . ? P2 Ru1 O4 C5 92.28(15) . . . . ? P1 Ru1 O4 C5 -93.36(15) . . . . ? O3 Ru1 N1 C6 179.31(18) . . . . ? O4 Ru1 N1 C6 0.38(16) . . . . ? P2 Ru1 N1 C6 -90.85(16) . . . . ? P1 Ru1 N1 C6 85.37(16) . . . . ? O3 Ru1 N1 C3 0.95(16) . . . . ? O4 Ru1 N1 C3 -177.97(18) . . . . ? P2 Ru1 N1 C3 90.80(16) . . . . ? P1 Ru1 N1 C3 -92.98(16) . . . . ? O1 C1 C2 C3 -176.6(2) . . . . ? C7 C1 C2 C3 3.4(4) . . . . ? C6 N1 C3 C2 -1.7(3) . . . . ? Ru1 N1 C3 C2 176.65(17) . . . . ? C6 N1 C3 C4 -179.64(19) . . . . ? Ru1 N1 C3 C4 -1.3(2) . . . . ? C1 C2 C3 N1 -0.6(3) . . . . ? C1 C2 C3 C4 177.1(2) . . . . ? Ru1 O3 C4 O2 -179.57(18) . . . . ? Ru1 O3 C4 C3 -0.2(2) . . . . ? N1 C3 C4 O2 -179.7(2) . . . . ? C2 C3 C4 O2 2.5(4) . . . . ? N1 C3 C4 O3 1.0(3) . . . . ? C2 C3 C4 O3 -176.9(2) . . . . ? Ru1 O4 C5 O5 179.74(18) . . . . ? Ru1 O4 C5 C6 0.4(2) . . . . ? C3 N1 C6 C7 1.0(3) . . . . ? Ru1 N1 C6 C7 -177.28(17) . . . . ? C3 N1 C6 C5 178.0(2) . . . . ? Ru1 N1 C6 C5 -0.3(2) . . . . ? O5 C5 C6 N1 -179.5(2) . . . . ? O4 C5 C6 N1 -0.1(3) . . . . ? O5 C5 C6 C7 -2.6(4) . . . . ? O4 C5 C6 C7 176.7(2) . . . . ? N1 C6 C7 C1 1.8(4) . . . . ? C5 C6 C7 C1 -174.7(2) . . . . ? O1 C1 C7 C6 176.0(2) . . . . ? C2 C1 C7 C6 -4.0(4) . . . . ? C13 C8 C9 C10 -1.0(4) . . . . ? C8 C9 C10 C11 -0.7(3) . . . . ? C8 C9 C10 P1 -176.49(18) . . . . ? C21 P1 C10 C11 -110.50(19) . . . . ? C16 P1 C10 C11 139.29(19) . . . . ? Ru1 P1 C10 C11 10.4(2) . . . . ? C21 P1 C10 C9 65.2(2) . . . . ? C16 P1 C10 C9 -45.0(2) . . . . ? Ru1 P1 C10 C9 -173.91(15) . . . . ? C9 C10 C11 C12 2.6(3) . . . . ? P1 C10 C11 C12 178.26(17) . . . . ? C10 C11 C12 C13 -2.7(4) . . . . ? C11 C12 C13 C8 1.0(4) . . . . ? C9 C8 C13 C12 0.9(4) . . . . ? C19 C14 C15 C16 -0.2(4) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C14 C15 C16 P1 179.3(2) . . . . ? C21 P1 C16 C17 156.77(19) . . . . ? C10 P1 C16 C17 -95.1(2) . . . . ? Ru1 P1 C16 C17 33.6(2) . . . . ? C21 P1 C16 C15 -23.1(2) . . . . ? C10 P1 C16 C15 85.1(2) . . . . ? Ru1 P1 C16 C15 -146.27(18) . . . . ? C15 C16 C17 C18 0.6(4) . . . . ? P1 C16 C17 C18 -179.28(19) . . . . ? C16 C17 C18 C19 0.1(4) . . . . ? C17 C18 C19 C14 -0.9(4) . . . . ? C15 C14 C19 C18 0.9(4) . . . . ? C25 C20 C21 C22 0.1(4) . . . . ? C25 C20 C21 P1 -174.0(2) . . . . ? C16 P1 C21 C20 -46.3(2) . . . . ? C10 P1 C21 C20 -157.3(2) . . . . ? Ru1 P1 C21 C20 79.4(2) . . . . ? C16 P1 C21 C22 139.7(2) . . . . ? C10 P1 C21 C22 28.7(2) . . . . ? Ru1 P1 C21 C22 -94.6(2) . . . . ? C20 C21 C22 C23 -0.6(4) . . . . ? P1 C21 C22 C23 173.5(2) . . . . ? C21 C22 C23 C24 -0.2(4) . . . . ? C22 C23 C24 C25 1.4(5) . . . . ? C23 C24 C25 C20 -1.9(5) . . . . ? C21 C20 C25 C24 1.1(4) . . . . ? C38 P2 C26 C27 92.2(2) . . . . ? C32 P2 C26 C27 -159.0(2) . . . . ? Ru1 P2 C26 C27 -31.8(2) . . . . ? C38 P2 C26 C31 -85.8(2) . . . . ? C32 P2 C26 C31 23.0(2) . . . . ? Ru1 P2 C26 C31 150.21(17) . . . . ? C31 C26 C27 C28 1.7(4) . . . . ? P2 C26 C27 C28 -176.3(2) . . . . ? C26 C27 C28 C29 0.3(4) . . . . ? C27 C28 C29 C30 -1.8(4) . . . . ? C28 C29 C30 C31 1.2(4) . . . . ? C29 C30 C31 C26 0.8(4) . . . . ? C27 C26 C31 C30 -2.2(4) . . . . ? P2 C26 C31 C30 175.8(2) . . . . ? C38 P2 C32 C37 28.1(2) . . . . ? C26 P2 C32 C37 -80.8(2) . . . . ? Ru1 P2 C32 C37 155.06(16) . . . . ? C38 P2 C32 C33 -157.65(18) . . . . ? C26 P2 C32 C33 93.4(2) . . . . ? Ru1 P2 C32 C33 -30.7(2) . . . . ? C37 C32 C33 C34 0.9(3) . . . . ? P2 C32 C33 C34 -173.43(18) . . . . ? C32 C33 C34 C35 -0.7(4) . . . . ? C33 C34 C35 C36 0.3(4) . . . . ? C34 C35 C36 C37 0.0(4) . . . . ? C35 C36 C37 C32 0.3(4) . . . . ? C33 C32 C37 C36 -0.7(3) . . . . ? P2 C32 C37 C36 173.55(18) . . . . ? C32 P2 C38 C43 -130.89(18) . . . . ? C26 P2 C38 C43 -22.0(2) . . . . ? Ru1 P2 C38 C43 100.55(17) . . . . ? C32 P2 C38 C39 50.42(19) . . . . ? C26 P2 C38 C39 159.33(17) . . . . ? Ru1 P2 C38 C39 -78.15(18) . . . . ? C43 C38 C39 C40 1.4(3) . . . . ? P2 C38 C39 C40 -179.89(17) . . . . ? C38 C39 C40 C41 0.4(3) . . . . ? C39 C40 C41 C42 -1.0(4) . . . . ? C40 C41 C42 C43 -0.2(3) . . . . ? C41 C42 C43 C38 2.1(3) . . . . ? C39 C38 C43 C42 -2.6(3) . . . . ? P2 C38 C43 C42 178.68(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O5 0.82 1.93 2.735(2) 166.2 2_657 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.86 _refine_diff_density_min -1.77 _refine_diff_density_rms 0.258 # END OF CIF # END OF CIF # Attachment '- [RuIII-hpa-As].txt' data_3AA _database_code_depnum_ccdc_archive 'CCDC 797113' #TrackingRef '- [RuIII-hpa-As].txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H33 As2 Cl N O5 Ru, C2 H3 N' _chemical_formula_sum 'C45 H36 As2 Cl N2 O5 Ru' _chemical_formula_weight 971.12 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' Cl Cl 0.1484 0.1585 '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' As As 0.0499 2.0058 '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_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_cell_setting Triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3411(14) _cell_length_b 13.6920(15) _cell_length_c 14.2068(15) _cell_angle_alpha 82.983(6) _cell_angle_beta 69.879(5) _cell_angle_gamma 63.268(5) _cell_volume 2011.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(5) _cell_measurement_reflns_used 14284 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 34.9 _exptl_crystal_description fragment _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 974 _exptl_absorpt_coefficient_mu 2.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.713 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(5) _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 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method '\w and \f scans ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57165 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.8 _diffrn_reflns_theta_max 34.9 _reflns_number_total 16343 _reflns_number_gt 11662 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0370P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16343 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.479965(14) 0.289946(12) 0.706329(11) 0.00898(4) Uani 1 1 d . . . As1 As 0.682904(19) 0.263160(16) 0.725393(15) 0.01070(5) Uani 1 1 d . . . As2 As 0.266791(19) 0.336614(16) 0.696412(14) 0.00957(5) Uani 1 1 d . . . Cl1 Cl 0.44832(5) 0.46588(4) 0.65148(4) 0.01497(10) Uani 1 1 d . . . O1 O 0.59622(18) -0.18402(12) 0.81158(11) 0.0254(4) Uani 1 1 d . . . H1 H 0.5850 -0.1919 0.8733 0.038 Uiso 1 1 calc R . . O2 O 0.64406(15) 0.04866(12) 0.48901(11) 0.0210(3) Uani 1 1 d . . . O3 O 0.56664(14) 0.20978(11) 0.56884(10) 0.0138(3) Uani 1 1 d . . . O4 O 0.41085(13) 0.29874(11) 0.86198(10) 0.0123(3) Uani 1 1 d . . . O5 O 0.38725(15) 0.20085(12) 0.99993(10) 0.0172(3) Uani 1 1 d . . . N1 N 0.51152(15) 0.13506(13) 0.74207(12) 0.0105(3) Uani 1 1 d . . . C1 C 0.5639(2) -0.07776(17) 0.79092(16) 0.0179(4) Uani 1 1 d . . . C2 C 0.5947(2) -0.04993(17) 0.68980(15) 0.0174(4) Uani 1 1 d . . . H2 H 0.6336 -0.1041 0.6374 0.021 Uiso 1 1 calc R . . C3 C 0.56666(19) 0.05836(16) 0.66872(14) 0.0128(4) Uani 1 1 d . . . C4 C 0.59658(19) 0.10517(16) 0.56508(15) 0.0134(4) Uani 1 1 d . . . C5 C 0.42000(19) 0.20897(16) 0.90813(14) 0.0123(4) Uani 1 1 d . . . C6 C 0.47818(19) 0.11031(16) 0.83881(14) 0.0127(4) Uani 1 1 d . . . C7 C 0.5008(2) 0.00446(17) 0.86602(15) 0.0162(4) Uani 1 1 d . . . H7 H 0.4740 -0.0122 0.9346 0.019 Uiso 1 1 calc R . . C8 C 0.6715(2) 0.38015(16) 0.79911(14) 0.0135(4) Uani 1 1 d . . . C9 C 0.7817(2) 0.37006(18) 0.81465(16) 0.0186(4) Uani 1 1 d . . . H9 H 0.8615 0.3085 0.7873 0.022 Uiso 1 1 calc R . . C10 C 0.7731(2) 0.45118(18) 0.87071(17) 0.0210(5) Uani 1 1 d . . . H10 H 0.8476 0.4442 0.8822 0.025 Uiso 1 1 calc R . . C11 C 0.6578(2) 0.54192(18) 0.91007(16) 0.0223(5) Uani 1 1 d . . . H11 H 0.6533 0.5972 0.9477 0.027 Uiso 1 1 calc R . . C12 C 0.5490(2) 0.55143(18) 0.89413(15) 0.0191(4) Uani 1 1 d . . . H12 H 0.4698 0.6141 0.9201 0.023 Uiso 1 1 calc R . . C13 C 0.5547(2) 0.47005(17) 0.84043(15) 0.0160(4) Uani 1 1 d . . . H13 H 0.4790 0.4757 0.8319 0.019 Uiso 1 1 calc R . . C14 C 0.8262(2) 0.23579(17) 0.60273(15) 0.0149(4) Uani 1 1 d . . . C15 C 0.9527(2) 0.16790(18) 0.59918(17) 0.0195(4) Uani 1 1 d . . . H15 H 0.9701 0.1351 0.6584 0.023 Uiso 1 1 calc R . . C16 C 1.0525(2) 0.14831(19) 0.50961(18) 0.0238(5) Uani 1 1 d . . . H16 H 1.1383 0.1017 0.5071 0.029 Uiso 1 1 calc R . . C17 C 1.0263(2) 0.1971(2) 0.42371(18) 0.0259(5) Uani 1 1 d . . . H17 H 1.0947 0.1837 0.3622 0.031 Uiso 1 1 calc R . . C18 C 0.9007(2) 0.2655(2) 0.42650(17) 0.0258(5) Uani 1 1 d . . . H18 H 0.8838 0.2989 0.3672 0.031 Uiso 1 1 calc R . . C19 C 0.8008(2) 0.28461(18) 0.51582(16) 0.0195(4) Uani 1 1 d . . . H19 H 0.7150 0.3309 0.5180 0.023 Uiso 1 1 calc R . . C20 C 0.7464(2) 0.13923(16) 0.80605(15) 0.0140(4) Uani 1 1 d . . . C21 C 0.8112(2) 0.03316(17) 0.76403(17) 0.0199(4) Uani 1 1 d . . . H21 H 0.8298 0.0216 0.6945 0.024 Uiso 1 1 calc R . . C22 C 0.8486(3) -0.05562(19) 0.82401(19) 0.0289(6) Uani 1 1 d . . . H22 H 0.8939 -0.1279 0.7953 0.035 Uiso 1 1 calc R . . C23 C 0.8199(3) -0.0390(2) 0.92546(19) 0.0295(6) Uani 1 1 d . . . H23 H 0.8449 -0.1001 0.9662 0.035 Uiso 1 1 calc R . . C24 C 0.7551(2) 0.06556(19) 0.96805(17) 0.0231(5) Uani 1 1 d . . . H24 H 0.7357 0.0764 1.0378 0.028 Uiso 1 1 calc R . . C25 C 0.7185(2) 0.15485(18) 0.90851(16) 0.0182(4) Uani 1 1 d . . . H25 H 0.6742 0.2269 0.9376 0.022 Uiso 1 1 calc R . . C26 C 0.13567(19) 0.47089(16) 0.77181(14) 0.0121(4) Uani 1 1 d . . . C27 C 0.1551(2) 0.50849(18) 0.84843(16) 0.0204(5) Uani 1 1 d . . . H27 H 0.2339 0.4699 0.8619 0.024 Uiso 1 1 calc R . . C28 C 0.0593(2) 0.60241(19) 0.90532(17) 0.0247(5) Uani 1 1 d . . . H28 H 0.0732 0.6282 0.9572 0.030 Uiso 1 1 calc R . . C29 C -0.0559(2) 0.65835(17) 0.88672(16) 0.0193(4) Uani 1 1 d . . . H29 H -0.1223 0.7209 0.9274 0.023 Uiso 1 1 calc R . . C30 C -0.0745(2) 0.62336(18) 0.80916(17) 0.0208(5) Uani 1 1 d . . . H30 H -0.1528 0.6630 0.7951 0.025 Uiso 1 1 calc R . . C31 C 0.0214(2) 0.52999(17) 0.75136(16) 0.0187(4) Uani 1 1 d . . . H31 H 0.0085 0.5065 0.6975 0.022 Uiso 1 1 calc R . . C32 C 0.2501(2) 0.36059(16) 0.56396(14) 0.0130(4) Uani 1 1 d . . . C33 C 0.3322(2) 0.39453(19) 0.49040(16) 0.0209(5) Uani 1 1 d . . . H33 H 0.3992 0.4007 0.5039 0.025 Uiso 1 1 calc R . . C34 C 0.3166(3) 0.4195(2) 0.39708(18) 0.0312(6) Uani 1 1 d . . . H34 H 0.3727 0.4434 0.3469 0.037 Uiso 1 1 calc R . . C35 C 0.2205(3) 0.4099(2) 0.37626(18) 0.0279(6) Uani 1 1 d . . . H35 H 0.2110 0.4264 0.3118 0.033 Uiso 1 1 calc R . . C36 C 0.1377(2) 0.3760(2) 0.44999(17) 0.0238(5) Uani 1 1 d . . . H36 H 0.0707 0.3701 0.4362 0.029 Uiso 1 1 calc R . . C37 C 0.1525(2) 0.35081(17) 0.54362(16) 0.0174(4) Uani 1 1 d . . . H37 H 0.0964 0.3269 0.5938 0.021 Uiso 1 1 calc R . . C38 C 0.19598(19) 0.23273(16) 0.75040(14) 0.0113(4) Uani 1 1 d . . . C39 C 0.2405(2) 0.13676(17) 0.69503(15) 0.0159(4) Uani 1 1 d . . . H39 H 0.3050 0.1226 0.6311 0.019 Uiso 1 1 calc R . . C40 C 0.1900(2) 0.06184(18) 0.73407(16) 0.0194(4) Uani 1 1 d . . . H40 H 0.2201 -0.0034 0.6965 0.023 Uiso 1 1 calc R . . C41 C 0.0961(2) 0.08235(18) 0.82747(16) 0.0182(4) Uani 1 1 d . . . H41 H 0.0618 0.0312 0.8536 0.022 Uiso 1 1 calc R . . C42 C 0.0522(2) 0.17713(17) 0.88279(16) 0.0175(4) Uani 1 1 d . . . H42 H -0.0126 0.1912 0.9465 0.021 Uiso 1 1 calc R . . C43 C 0.1032(2) 0.25176(16) 0.84471(15) 0.0146(4) Uani 1 1 d . . . H43 H 0.0744 0.3159 0.8833 0.017 Uiso 1 1 calc R . . N1S N 0.7904(4) 0.2223(3) 0.1254(2) 0.0814(12) Uani 1 1 d . . . C1S C 0.7341(3) 0.2328(2) 0.2069(2) 0.0366(7) Uani 1 1 d . . . C2S C 0.6630(5) 0.2439(3) 0.3121(3) 0.0884(17) Uani 1 1 d . . . H21S H 0.5987 0.2163 0.3244 0.133 Uiso 1 1 calc R . . H22S H 0.6199 0.3213 0.3339 0.133 Uiso 1 1 calc R . . H23S H 0.7217 0.2018 0.3498 0.133 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01058(7) 0.00879(7) 0.00823(7) 0.00187(5) -0.00418(5) -0.00436(6) As1 0.01155(10) 0.01089(10) 0.01094(9) 0.00141(7) -0.00536(8) -0.00498(8) As2 0.01054(9) 0.01001(9) 0.00871(9) 0.00119(7) -0.00441(7) -0.00423(7) Cl1 0.0199(2) 0.0118(2) 0.0170(2) 0.00499(18) -0.00957(19) -0.00864(19) O1 0.0435(11) 0.0125(7) 0.0166(8) 0.0021(6) -0.0105(8) -0.0091(7) O2 0.0295(9) 0.0176(8) 0.0124(7) -0.0027(6) -0.0033(6) -0.0092(7) O3 0.0182(7) 0.0132(7) 0.0094(6) 0.0017(5) -0.0036(6) -0.0072(6) O4 0.0166(7) 0.0100(6) 0.0100(6) 0.0013(5) -0.0047(5) -0.0055(6) O5 0.0237(8) 0.0146(7) 0.0098(6) 0.0012(5) -0.0043(6) -0.0065(6) N1 0.0111(8) 0.0097(7) 0.0103(7) -0.0001(6) -0.0036(6) -0.0040(6) C1 0.0243(11) 0.0115(9) 0.0183(10) 0.0017(8) -0.0079(9) -0.0077(9) C2 0.0225(11) 0.0132(10) 0.0136(9) -0.0016(8) -0.0046(8) -0.0057(8) C3 0.0153(9) 0.0117(9) 0.0100(8) -0.0004(7) -0.0050(7) -0.0039(8) C4 0.0139(9) 0.0130(9) 0.0116(9) 0.0000(7) -0.0038(7) -0.0047(8) C5 0.0128(9) 0.0118(9) 0.0116(9) 0.0008(7) -0.0043(7) -0.0048(7) C6 0.0141(9) 0.0117(9) 0.0113(9) 0.0010(7) -0.0046(7) -0.0045(7) C7 0.0218(11) 0.0136(10) 0.0105(9) 0.0018(7) -0.0021(8) -0.0082(8) C8 0.0209(10) 0.0117(9) 0.0108(9) 0.0027(7) -0.0066(8) -0.0091(8) C9 0.0223(11) 0.0160(10) 0.0220(11) 0.0023(8) -0.0124(9) -0.0089(9) C10 0.0299(12) 0.0217(11) 0.0231(11) 0.0040(9) -0.0154(10) -0.0170(10) C11 0.0400(14) 0.0179(11) 0.0160(10) 0.0019(9) -0.0105(10) -0.0179(10) C12 0.0262(12) 0.0151(10) 0.0131(9) -0.0011(8) -0.0054(9) -0.0070(9) C13 0.0190(10) 0.0163(10) 0.0122(9) 0.0018(8) -0.0048(8) -0.0077(8) C14 0.0153(10) 0.0141(9) 0.0164(9) -0.0007(8) -0.0046(8) -0.0076(8) C15 0.0161(10) 0.0194(11) 0.0235(11) -0.0008(9) -0.0067(9) -0.0078(9) C16 0.0167(11) 0.0237(12) 0.0280(12) -0.0049(10) -0.0025(9) -0.0085(9) C17 0.0238(12) 0.0310(13) 0.0208(11) -0.0080(10) 0.0035(9) -0.0159(10) C18 0.0267(13) 0.0349(14) 0.0166(10) 0.0012(10) -0.0034(9) -0.0169(11) C19 0.0199(11) 0.0220(11) 0.0162(10) 0.0018(9) -0.0056(8) -0.0094(9) C20 0.0152(9) 0.0134(9) 0.0162(9) 0.0032(8) -0.0100(8) -0.0057(8) C21 0.0268(12) 0.0156(10) 0.0194(10) 0.0009(8) -0.0133(9) -0.0067(9) C22 0.0464(16) 0.0135(11) 0.0309(13) 0.0031(10) -0.0235(12) -0.0092(11) C23 0.0517(17) 0.0189(12) 0.0289(13) 0.0107(10) -0.0273(13) -0.0167(12) C24 0.0376(14) 0.0221(12) 0.0175(10) 0.0067(9) -0.0153(10) -0.0165(11) C25 0.0251(11) 0.0163(10) 0.0168(10) 0.0026(8) -0.0084(9) -0.0114(9) C26 0.0122(9) 0.0101(9) 0.0123(9) 0.0009(7) -0.0027(7) -0.0046(7) C27 0.0185(11) 0.0205(11) 0.0185(10) -0.0052(9) -0.0081(9) -0.0027(9) C28 0.0256(12) 0.0246(12) 0.0218(11) -0.0080(9) -0.0055(10) -0.0088(10) C29 0.0174(10) 0.0114(9) 0.0217(11) -0.0009(8) -0.0026(9) -0.0025(8) C30 0.0165(10) 0.0151(10) 0.0273(12) 0.0006(9) -0.0083(9) -0.0031(8) C31 0.0169(10) 0.0165(10) 0.0220(11) -0.0006(8) -0.0094(9) -0.0043(8) C32 0.0166(10) 0.0122(9) 0.0117(9) 0.0024(7) -0.0081(8) -0.0054(8) C33 0.0293(12) 0.0289(12) 0.0172(10) 0.0091(9) -0.0135(9) -0.0210(11) C34 0.0462(16) 0.0482(17) 0.0193(11) 0.0172(11) -0.0187(11) -0.0355(14) C35 0.0424(15) 0.0359(14) 0.0209(11) 0.0142(10) -0.0230(11) -0.0240(12) C36 0.0315(13) 0.0302(13) 0.0221(11) 0.0064(10) -0.0179(10) -0.0186(11) C37 0.0190(10) 0.0187(10) 0.0171(10) 0.0034(8) -0.0085(8) -0.0091(9) C38 0.0121(9) 0.0119(9) 0.0112(8) 0.0025(7) -0.0058(7) -0.0054(7) C39 0.0179(10) 0.0154(10) 0.0138(9) -0.0004(8) -0.0038(8) -0.0077(8) C40 0.0265(12) 0.0152(10) 0.0190(10) -0.0002(8) -0.0080(9) -0.0106(9) C41 0.0230(11) 0.0190(11) 0.0182(10) 0.0063(8) -0.0090(9) -0.0134(9) C42 0.0200(11) 0.0196(11) 0.0129(9) 0.0037(8) -0.0045(8) -0.0099(9) C43 0.0170(10) 0.0142(10) 0.0120(9) 0.0004(7) -0.0049(8) -0.0063(8) N1S 0.125(3) 0.084(2) 0.0438(18) -0.0168(17) 0.0133(19) -0.077(2) C1S 0.0464(18) 0.0286(14) 0.0305(14) 0.0004(12) -0.0063(13) -0.0172(13) C2S 0.140(4) 0.0246(16) 0.045(2) -0.0087(15) 0.026(2) -0.027(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.0093(16) . ? Ru1 O3 2.0480(14) . ? Ru1 O4 2.0754(13) . ? Ru1 Cl1 2.3381(5) . ? Ru1 As2 2.4637(4) . ? Ru1 As1 2.4691(4) . ? As1 C14 1.936(2) . ? As1 C20 1.9372(19) . ? As1 C8 1.946(2) . ? As2 C32 1.9353(19) . ? As2 C26 1.939(2) . ? As2 C38 1.9406(19) . ? O1 C1 1.348(2) . ? O1 H1 0.8400 . ? O2 C4 1.213(2) . ? O3 C4 1.311(2) . ? O4 C5 1.297(2) . ? O5 C5 1.232(2) . ? N1 C3 1.337(2) . ? N1 C6 1.340(2) . ? C1 C7 1.395(3) . ? C1 C2 1.405(3) . ? C2 C3 1.382(3) . ? C2 H2 0.9500 . ? C3 C4 1.524(3) . ? C5 C6 1.509(3) . ? C6 C7 1.379(3) . ? C7 H7 0.9500 . ? C8 C13 1.392(3) . ? C8 C9 1.395(3) . ? C9 C10 1.390(3) . ? C9 H9 0.9500 . ? C10 C11 1.383(3) . ? C10 H10 0.9500 . ? C11 C12 1.384(3) . ? C11 H11 0.9500 . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.395(3) . ? C14 C15 1.398(3) . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.393(3) . ? C17 H17 0.9500 . ? C18 C19 1.383(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.394(3) . ? C20 C25 1.396(3) . ? C21 C22 1.389(3) . ? C21 H21 0.9500 . ? C22 C23 1.382(3) . ? C22 H22 0.9500 . ? C23 C24 1.380(3) . ? C23 H23 0.9500 . ? C24 C25 1.389(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.388(3) . ? C26 C27 1.391(3) . ? C27 C28 1.390(3) . ? C27 H27 0.9500 . ? C28 C29 1.381(3) . ? C28 H28 0.9500 . ? C29 C30 1.378(3) . ? C29 H29 0.9500 . ? C30 C31 1.391(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.382(3) . ? C32 C37 1.395(3) . ? C33 C34 1.384(3) . ? C33 H33 0.9500 . ? C34 C35 1.380(3) . ? C34 H34 0.9500 . ? C35 C36 1.389(3) . ? C35 H35 0.9500 . ? C36 C37 1.386(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C43 1.391(3) . ? C38 C39 1.397(3) . ? C39 C40 1.395(3) . ? C39 H39 0.9500 . ? C40 C41 1.387(3) . ? C40 H40 0.9500 . ? C41 C42 1.385(3) . ? C41 H41 0.9500 . ? C42 C43 1.394(3) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? N1S C1S 1.115(4) . ? C1S C2S 1.435(4) . ? C2S H21S 0.9800 . ? C2S H22S 0.9800 . ? C2S H23S 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 O3 77.33(6) . . ? N1 Ru1 O4 76.80(6) . . ? O3 Ru1 O4 154.10(5) . . ? N1 Ru1 Cl1 175.47(5) . . ? O3 Ru1 Cl1 98.19(4) . . ? O4 Ru1 Cl1 107.69(4) . . ? N1 Ru1 As2 92.68(5) . . ? O3 Ru1 As2 90.59(4) . . ? O4 Ru1 As2 91.88(4) . . ? Cl1 Ru1 As2 86.663(15) . . ? N1 Ru1 As1 92.10(5) . . ? O3 Ru1 As1 94.45(4) . . ? O4 Ru1 As1 85.23(4) . . ? Cl1 Ru1 As1 88.884(15) . . ? As2 Ru1 As1 173.706(9) . . ? C32 As2 C26 103.82(8) . . ? C32 As2 C38 103.22(8) . . ? C26 As2 C38 102.74(8) . . ? C32 As2 Ru1 116.52(6) . . ? C26 As2 Ru1 112.15(6) . . ? C38 As2 Ru1 116.68(6) . . ? C14 As1 C20 104.21(9) . . ? C14 As1 C8 106.07(9) . . ? C20 As1 C8 101.04(8) . . ? C14 As1 Ru1 116.20(6) . . ? C20 As1 Ru1 112.20(6) . . ? C8 As1 Ru1 115.48(6) . . ? C1 O1 H1 109.5 . . ? C4 O3 Ru1 118.49(12) . . ? C5 O4 Ru1 117.77(12) . . ? C3 N1 C6 121.26(17) . . ? C3 N1 Ru1 119.27(13) . . ? C6 N1 Ru1 119.47(13) . . ? O1 C1 C7 122.34(19) . . ? O1 C1 C2 118.19(19) . . ? C7 C1 C2 119.47(19) . . ? C3 C2 C1 118.14(19) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? N1 C3 C2 121.28(18) . . ? N1 C3 C4 112.03(16) . . ? C2 C3 C4 126.65(18) . . ? O2 C4 O3 125.45(18) . . ? O2 C4 C3 121.74(18) . . ? O3 C4 C3 112.81(16) . . ? O5 C5 O4 125.07(18) . . ? O5 C5 C6 121.00(17) . . ? O4 C5 C6 113.92(16) . . ? N1 C6 C7 120.98(18) . . ? N1 C6 C5 112.02(16) . . ? C7 C6 C5 126.98(17) . . ? C6 C7 C1 118.74(18) . . ? C6 C7 H7 120.6 . . ? C1 C7 H7 120.6 . . ? C13 C8 C9 120.00(19) . . ? C13 C8 As1 121.02(16) . . ? C9 C8 As1 118.89(16) . . ? C10 C9 C8 119.2(2) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 121.1(2) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.4(2) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C13 120.5(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 119.8(2) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? C19 C14 C15 119.8(2) . . ? C19 C14 As1 118.34(16) . . ? C15 C14 As1 121.84(16) . . ? C16 C15 C14 120.2(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.5(2) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 120.7(2) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 119.8(2) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C14 119.9(2) . . ? C18 C19 H19 120.1 . . ? C14 C19 H19 120.1 . . ? C21 C20 C25 119.42(19) . . ? C21 C20 As1 120.22(15) . . ? C25 C20 As1 120.15(16) . . ? C22 C21 C20 119.9(2) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 120.6(2) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.7(2) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C20 120.3(2) . . ? C24 C25 H25 119.8 . . ? C20 C25 H25 119.8 . . ? C31 C26 C27 119.14(19) . . ? C31 C26 As2 121.01(15) . . ? C27 C26 As2 119.85(15) . . ? C28 C27 C26 120.1(2) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 120.3(2) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C30 C29 C28 119.9(2) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.0(2) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C26 C31 C30 120.5(2) . . ? C26 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C33 C32 C37 119.85(18) . . ? C33 C32 As2 118.75(15) . . ? C37 C32 As2 121.27(15) . . ? C32 C33 C34 119.9(2) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 120.6(2) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 119.7(2) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C37 C36 C35 120.1(2) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C32 119.9(2) . . ? C36 C37 H37 120.1 . . ? C32 C37 H37 120.1 . . ? C43 C38 C39 119.65(18) . . ? C43 C38 As2 120.61(15) . . ? C39 C38 As2 119.73(15) . . ? C40 C39 C38 119.72(19) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 120.2(2) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C42 C41 C40 120.2(2) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 119.9(2) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C38 C43 C42 120.32(19) . . ? C38 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? N1S C1S C2S 178.8(4) . . ? C1S C2S H21S 109.5 . . ? C1S C2S H22S 109.5 . . ? H21S C2S H22S 109.5 . . ? C1S C2S H23S 109.5 . . ? H21S C2S H23S 109.5 . . ? H22S C2S H23S 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ru1 As1 C14 99.70(8) . . . . ? O3 Ru1 As1 C14 22.25(8) . . . . ? O4 Ru1 As1 C14 176.27(8) . . . . ? Cl1 Ru1 As1 C14 -75.88(7) . . . . ? N1 Ru1 As1 C20 -20.06(8) . . . . ? O3 Ru1 As1 C20 -97.50(8) . . . . ? O4 Ru1 As1 C20 56.51(8) . . . . ? Cl1 Ru1 As1 C20 164.37(7) . . . . ? N1 Ru1 As1 C8 -135.12(8) . . . . ? O3 Ru1 As1 C8 147.44(7) . . . . ? O4 Ru1 As1 C8 -58.55(7) . . . . ? Cl1 Ru1 As1 C8 49.31(6) . . . . ? N1 Ru1 As2 C32 -109.79(8) . . . . ? O3 Ru1 As2 C32 -32.45(8) . . . . ? O4 Ru1 As2 C32 173.34(8) . . . . ? Cl1 Ru1 As2 C32 65.72(7) . . . . ? N1 Ru1 As2 C26 130.77(8) . . . . ? O3 Ru1 As2 C26 -151.89(7) . . . . ? O4 Ru1 As2 C26 53.90(7) . . . . ? Cl1 Ru1 As2 C26 -53.72(6) . . . . ? N1 Ru1 As2 C38 12.67(8) . . . . ? O3 Ru1 As2 C38 90.01(7) . . . . ? O4 Ru1 As2 C38 -64.20(7) . . . . ? Cl1 Ru1 As2 C38 -171.82(7) . . . . ? N1 Ru1 O3 C4 2.38(14) . . . . ? O4 Ru1 O3 C4 5.3(2) . . . . ? Cl1 Ru1 O3 C4 -176.95(13) . . . . ? As2 Ru1 O3 C4 -90.24(14) . . . . ? As1 Ru1 O3 C4 93.54(14) . . . . ? N1 Ru1 O4 C5 1.03(14) . . . . ? O3 Ru1 O4 C5 -1.9(2) . . . . ? Cl1 Ru1 O4 C5 -179.55(13) . . . . ? As2 Ru1 O4 C5 93.35(13) . . . . ? As1 Ru1 O4 C5 -92.25(13) . . . . ? O3 Ru1 N1 C3 -0.92(14) . . . . ? O4 Ru1 N1 C3 -179.62(16) . . . . ? As2 Ru1 N1 C3 89.08(15) . . . . ? As1 Ru1 N1 C3 -95.01(15) . . . . ? O3 Ru1 N1 C6 178.41(16) . . . . ? O4 Ru1 N1 C6 -0.29(14) . . . . ? As2 Ru1 N1 C6 -91.59(14) . . . . ? As1 Ru1 N1 C6 84.32(15) . . . . ? O1 C1 C2 C3 -177.1(2) . . . . ? C7 C1 C2 C3 3.2(3) . . . . ? C6 N1 C3 C2 -1.8(3) . . . . ? Ru1 N1 C3 C2 177.50(15) . . . . ? C6 N1 C3 C4 -179.72(17) . . . . ? Ru1 N1 C3 C4 -0.4(2) . . . . ? C1 C2 C3 N1 -0.2(3) . . . . ? C1 C2 C3 C4 177.4(2) . . . . ? Ru1 O3 C4 O2 177.39(17) . . . . ? Ru1 O3 C4 C3 -3.2(2) . . . . ? N1 C3 C4 O2 -178.26(19) . . . . ? C2 C3 C4 O2 4.0(3) . . . . ? N1 C3 C4 O3 2.3(2) . . . . ? C2 C3 C4 O3 -175.47(19) . . . . ? Ru1 O4 C5 O5 177.41(16) . . . . ? Ru1 O4 C5 C6 -1.5(2) . . . . ? C3 N1 C6 C7 0.6(3) . . . . ? Ru1 N1 C6 C7 -178.68(15) . . . . ? C3 N1 C6 C5 178.95(17) . . . . ? Ru1 N1 C6 C5 -0.4(2) . . . . ? O5 C5 C6 N1 -177.76(18) . . . . ? O4 C5 C6 N1 1.2(2) . . . . ? O5 C5 C6 C7 0.4(3) . . . . ? O4 C5 C6 C7 179.40(19) . . . . ? N1 C6 C7 C1 2.5(3) . . . . ? C5 C6 C7 C1 -175.6(2) . . . . ? O1 C1 C7 C6 176.0(2) . . . . ? C2 C1 C7 C6 -4.4(3) . . . . ? C14 As1 C8 C13 132.38(16) . . . . ? C20 As1 C8 C13 -119.17(16) . . . . ? Ru1 As1 C8 C13 2.12(18) . . . . ? C14 As1 C8 C9 -50.92(17) . . . . ? C20 As1 C8 C9 57.53(17) . . . . ? Ru1 As1 C8 C9 178.82(13) . . . . ? C13 C8 C9 C10 -0.7(3) . . . . ? As1 C8 C9 C10 -177.40(16) . . . . ? C8 C9 C10 C11 -0.8(3) . . . . ? C9 C10 C11 C12 0.6(3) . . . . ? C10 C11 C12 C13 1.0(3) . . . . ? C11 C12 C13 C8 -2.4(3) . . . . ? C9 C8 C13 C12 2.2(3) . . . . ? As1 C8 C13 C12 178.91(15) . . . . ? C20 As1 C14 C19 156.34(16) . . . . ? C8 As1 C14 C19 -97.49(17) . . . . ? Ru1 As1 C14 C19 32.35(18) . . . . ? C20 As1 C14 C15 -22.76(19) . . . . ? C8 As1 C14 C15 83.41(18) . . . . ? Ru1 As1 C14 C15 -146.75(15) . . . . ? C19 C14 C15 C16 -0.5(3) . . . . ? As1 C14 C15 C16 178.57(17) . . . . ? C14 C15 C16 C17 0.5(3) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? C16 C17 C18 C19 -0.4(4) . . . . ? C17 C18 C19 C14 0.3(4) . . . . ? C15 C14 C19 C18 0.1(3) . . . . ? As1 C14 C19 C18 -178.98(18) . . . . ? C14 As1 C20 C21 -47.21(19) . . . . ? C8 As1 C20 C21 -157.10(18) . . . . ? Ru1 As1 C20 C21 79.32(18) . . . . ? C14 As1 C20 C25 138.06(17) . . . . ? C8 As1 C20 C25 28.17(19) . . . . ? Ru1 As1 C20 C25 -95.41(17) . . . . ? C25 C20 C21 C22 -0.8(3) . . . . ? As1 C20 C21 C22 -175.53(18) . . . . ? C20 C21 C22 C23 1.0(4) . . . . ? C21 C22 C23 C24 -0.6(4) . . . . ? C22 C23 C24 C25 0.0(4) . . . . ? C23 C24 C25 C20 0.3(4) . . . . ? C21 C20 C25 C24 0.1(3) . . . . ? As1 C20 C25 C24 174.90(17) . . . . ? C32 As2 C26 C31 32.49(19) . . . . ? C38 As2 C26 C31 -74.79(18) . . . . ? Ru1 As2 C26 C31 159.11(15) . . . . ? C32 As2 C26 C27 -148.24(17) . . . . ? C38 As2 C26 C27 104.48(17) . . . . ? Ru1 As2 C26 C27 -21.61(18) . . . . ? C31 C26 C27 C28 1.8(3) . . . . ? As2 C26 C27 C28 -177.48(17) . . . . ? C26 C27 C28 C29 0.6(4) . . . . ? C27 C28 C29 C30 -2.4(3) . . . . ? C28 C29 C30 C31 1.8(3) . . . . ? C27 C26 C31 C30 -2.4(3) . . . . ? As2 C26 C31 C30 176.88(16) . . . . ? C29 C30 C31 C26 0.6(3) . . . . ? C26 As2 C32 C33 97.95(18) . . . . ? C38 As2 C32 C33 -155.12(17) . . . . ? Ru1 As2 C32 C33 -25.88(19) . . . . ? C26 As2 C32 C37 -78.06(18) . . . . ? C38 As2 C32 C37 28.86(19) . . . . ? Ru1 As2 C32 C37 158.11(15) . . . . ? C37 C32 C33 C34 0.5(3) . . . . ? As2 C32 C33 C34 -175.6(2) . . . . ? C32 C33 C34 C35 -0.6(4) . . . . ? C33 C34 C35 C36 0.7(4) . . . . ? C34 C35 C36 C37 -0.7(4) . . . . ? C35 C36 C37 C32 0.6(4) . . . . ? C33 C32 C37 C36 -0.5(3) . . . . ? As2 C32 C37 C36 175.45(17) . . . . ? C32 As2 C38 C43 -129.64(16) . . . . ? C26 As2 C38 C43 -21.90(17) . . . . ? Ru1 As2 C38 C43 101.21(15) . . . . ? C32 As2 C38 C39 51.75(17) . . . . ? C26 As2 C38 C39 159.49(16) . . . . ? Ru1 As2 C38 C39 -77.40(16) . . . . ? C43 C38 C39 C40 1.1(3) . . . . ? As2 C38 C39 C40 179.71(15) . . . . ? C38 C39 C40 C41 -0.1(3) . . . . ? C39 C40 C41 C42 -0.2(3) . . . . ? C40 C41 C42 C43 -0.5(3) . . . . ? C39 C38 C43 C42 -1.8(3) . . . . ? As2 C38 C43 C42 179.62(15) . . . . ? C41 C42 C43 C38 1.5(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O5 0.84 1.93 2.729(2) 159.5 2_657 _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.14 _refine_diff_density_min -1.08 _refine_diff_density_rms 0.133