# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_General _journal_name_full 'Dalton Trans.' #TrackingRef '- cif.cif' _journal_coden_Cambridge 0222 _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? _publ_contact_author_name 'T. S. Andy Hor' _publ_contact_author_email andyhor@nus.edu.sg _publ_contact_author_address ; Department of Chemistry, National University of Singapore, 3 Science Drive 3, 117543 Singapore ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category FM _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER SECTION ABSTRACT ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_address N.Ding ; Department of Chemistry, National University of Singapore, 3 Science Drive 3, 117543 Singapore ; 'H.T. S. Andy' ; Department of Chemistry, National University of Singapore, 3 Science Drive 3, 117543 Singapore Institute of Materials Research and Engineering, Agency for Science, Technology and Research, 3 Research Link, S117602, Singapore ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 778716' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62.50 H56 Br N O2 P2 Ru S' _chemical_formula_weight 1128.06 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.359(4) _cell_length_b 14.753(5) _cell_length_c 17.270(6) _cell_angle_alpha 93.390(9) _cell_angle_beta 104.451(8) _cell_angle_gamma 107.960(10) _cell_volume 2636.8(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1521 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 17.89 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 1.421 _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1158 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7615 _exptl_absorpt_correction_T_max 0.9649 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28965 _diffrn_reflns_av_R_equivalents 0.1091 _diffrn_reflns_av_sigmaI/netI 0.1210 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9311 _reflns_number_gt 6098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The bond distances for the disordered toluene were restrainted to 1.39(0.02) angstroms for C2X-C3X, C2X-C7X, C4X-C5X and C5X-C6X, 1.35(0.02) angstroms for C3X-C4X and C6X-C7X, 1.50(0.02)angstroms for C1X-C2X. The atoms C1X, C2X, C3X and C7X in the toluene molecule were also restrainted to be in the sample plane. 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^)+(0.0554P)^2^+0.8067P] 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 9311 _refine_ls_number_parameters 607 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1570 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.31392(5) 0.28786(4) 0.27759(3) 0.02329(16) Uani 1 1 d . . . Br1 Br 0.06992(6) 0.24439(5) 0.23901(4) 0.0345(2) Uani 1 1 d . . . P1 P 0.32259(17) 0.40670(13) 0.18869(10) 0.0290(4) Uani 1 1 d . . . P2 P 0.29798(17) 0.18089(12) 0.37491(10) 0.0274(4) Uani 1 1 d . . . S1 S 0.14414(17) 0.10292(13) 0.13698(10) 0.0334(4) Uani 1 1 d . . . O1 O 0.5149(4) 0.3540(3) 0.3353(3) 0.0301(11) Uani 1 1 d . . . O2 O 0.3828(5) 0.4160(3) 0.3739(2) 0.0330(11) Uani 1 1 d . . . N1 N 0.3868(5) 0.1496(4) 0.1755(3) 0.0303(13) Uani 1 1 d . . . C1 C 0.2958(6) 0.1824(5) 0.1952(4) 0.0275(16) Uani 1 1 d . . . C2 C 0.3429(7) 0.0653(4) 0.1174(4) 0.0293(16) Uani 1 1 d . . . C3 C 0.4165(8) 0.0189(5) 0.0926(4) 0.0416(19) Uani 1 1 d . . . H3 H 0.5060 0.0411 0.1126 0.050 Uiso 1 1 calc R . . C4 C 0.3496(9) -0.0651(5) 0.0344(5) 0.054(2) Uani 1 1 d . . . H4 H 0.3960 -0.0992 0.0156 0.065 Uiso 1 1 calc R . . C5 C 0.2169(8) -0.0970(6) 0.0052(5) 0.053(2) Uani 1 1 d . . . H5 H 0.1756 -0.1518 -0.0335 0.064 Uiso 1 1 calc R . . C6 C 0.1451(7) -0.0501(5) 0.0319(4) 0.044(2) Uani 1 1 d . . . H6 H 0.0557 -0.0727 0.0122 0.053 Uiso 1 1 calc R . . C7 C 0.2075(7) 0.0315(5) 0.0888(4) 0.0336(17) Uani 1 1 d . . . C8 C 0.5261(6) 0.1938(5) 0.2125(4) 0.0361(18) Uani 1 1 d . . . H8A H 0.5604 0.1445 0.2329 0.043 Uiso 1 1 calc R . . H8B H 0.5408 0.2413 0.2583 0.043 Uiso 1 1 calc R . . C9 C 0.6001(6) 0.2423(5) 0.1556(4) 0.0330(17) Uani 1 1 d . . . C10 C 0.5414(7) 0.2563(5) 0.0798(4) 0.0376(18) Uani 1 1 d . . . H10 H 0.4521 0.2312 0.0598 0.045 Uiso 1 1 calc R . . C11 C 0.6129(8) 0.3072(5) 0.0327(5) 0.048(2) Uani 1 1 d . . . H11 H 0.5719 0.3180 -0.0180 0.058 Uiso 1 1 calc R . . C12 C 0.7475(9) 0.3424(6) 0.0619(6) 0.059(2) Uani 1 1 d . . . H12 H 0.7966 0.3776 0.0312 0.071 Uiso 1 1 calc R . . C13 C 0.8066(8) 0.3247(6) 0.1362(6) 0.055(2) Uani 1 1 d . . . H13 H 0.8962 0.3462 0.1551 0.066 Uiso 1 1 calc R . . C14 C 0.7342(7) 0.2755(5) 0.1823(5) 0.046(2) Uani 1 1 d . . . H14 H 0.7753 0.2640 0.2326 0.055 Uiso 1 1 calc R . . C15 C 0.4975(7) 0.4208(5) 0.3787(4) 0.0313(16) Uani 1 1 d . . . C16 C 0.6110(7) 0.5009(5) 0.4308(4) 0.045(2) Uani 1 1 d . . . H16A H 0.6012 0.5615 0.4195 0.067 Uiso 1 1 calc R . . H16B H 0.6882 0.4971 0.4198 0.067 Uiso 1 1 calc R . . H16C H 0.6166 0.4956 0.4867 0.067 Uiso 1 1 calc R . . C1A C 0.4819(7) 0.4999(5) 0.2143(4) 0.0308(16) Uani 1 1 d . . . C2A C 0.5880(7) 0.4730(5) 0.2123(4) 0.0375(18) Uani 1 1 d . . . H2A H 0.5748 0.4096 0.1925 0.045 Uiso 1 1 calc R . . C3A C 0.7134(7) 0.5377(6) 0.2388(4) 0.0422(19) Uani 1 1 d . . . H3A H 0.7829 0.5181 0.2361 0.051 Uiso 1 1 calc R . . C4A C 0.7329(8) 0.6307(6) 0.2689(4) 0.047(2) Uani 1 1 d . . . H4A H 0.8164 0.6740 0.2889 0.057 Uiso 1 1 calc R . . C5A C 0.6301(9) 0.6603(6) 0.2697(5) 0.056(2) Uani 1 1 d . . . H5A H 0.6442 0.7241 0.2888 0.068 Uiso 1 1 calc R . . C6A C 0.5055(8) 0.5959(5) 0.2424(4) 0.047(2) Uani 1 1 d . . . H6A H 0.4366 0.6171 0.2428 0.056 Uiso 1 1 calc R . . C1B C 0.2143(7) 0.4774(5) 0.1864(4) 0.0348(17) Uani 1 1 d . . . C2B C 0.1772(7) 0.4964(5) 0.2542(4) 0.0388(18) Uani 1 1 d . . . H2B H 0.2059 0.4719 0.3010 0.047 Uiso 1 1 calc R . . C3B C 0.0978(8) 0.5512(5) 0.2533(5) 0.048(2) Uani 1 1 d . . . H3B H 0.0737 0.5639 0.2994 0.057 Uiso 1 1 calc R . . C4B C 0.0546(8) 0.5869(5) 0.1838(5) 0.052(2) Uani 1 1 d . . . H4B H 0.0012 0.6238 0.1832 0.062 Uiso 1 1 calc R . . C5B C 0.0888(9) 0.5691(7) 0.1168(5) 0.066(3) Uani 1 1 d . . . H5B H 0.0578 0.5927 0.0700 0.079 Uiso 1 1 calc R . . C6B C 0.1708(9) 0.5151(6) 0.1174(5) 0.059(2) Uani 1 1 d . . . H6B H 0.1962 0.5044 0.0714 0.071 Uiso 1 1 calc R . . C1C C 0.2825(6) 0.3652(4) 0.0795(4) 0.0292(16) Uani 1 1 d . . . C2C C 0.1593(7) 0.2992(5) 0.0433(4) 0.0400(19) Uani 1 1 d . . . H2C H 0.1030 0.2773 0.0744 0.048 Uiso 1 1 calc R . . C3C C 0.1209(8) 0.2663(5) -0.0388(4) 0.049(2) Uani 1 1 d . . . H3C H 0.0400 0.2207 -0.0628 0.059 Uiso 1 1 calc R . . C4C C 0.2028(7) 0.3014(5) -0.0843(4) 0.045(2) Uani 1 1 d . . . H4C H 0.1760 0.2794 -0.1396 0.054 Uiso 1 1 calc R . . C5C C 0.3228(8) 0.3678(5) -0.0510(4) 0.0436(19) Uani 1 1 d . . . H5C H 0.3764 0.3913 -0.0834 0.052 Uiso 1 1 calc R . . C6C C 0.3642(7) 0.4002(5) 0.0321(4) 0.0357(17) Uani 1 1 d . . . H6C H 0.4459 0.4450 0.0556 0.043 Uiso 1 1 calc R . . C1D C 0.1972(6) 0.1886(5) 0.4421(4) 0.0298(16) Uani 1 1 d . . . C2D C 0.1564(7) 0.2665(5) 0.4497(4) 0.0376(18) Uani 1 1 d . . . H2D H 0.1742 0.3152 0.4182 0.045 Uiso 1 1 calc R . . C3D C 0.0880(7) 0.2707(6) 0.5057(5) 0.049(2) Uani 1 1 d . . . H3D H 0.0626 0.3241 0.5125 0.059 Uiso 1 1 calc R . . C4D C 0.0574(7) 0.1997(6) 0.5505(4) 0.047(2) Uani 1 1 d . . . H4D H 0.0069 0.2025 0.5848 0.056 Uiso 1 1 calc R . . C5D C 0.1008(8) 0.1239(6) 0.5452(4) 0.048(2) Uani 1 1 d . . . H5D H 0.0832 0.0760 0.5775 0.058 Uiso 1 1 calc R . . C6D C 0.1710(7) 0.1189(5) 0.4916(4) 0.0420(19) Uani 1 1 d . . . H6D H 0.2017 0.0675 0.4885 0.050 Uiso 1 1 calc R . . C1E C 0.4472(7) 0.1955(5) 0.4550(4) 0.0334(17) Uani 1 1 d . . . C2E C 0.5108(8) 0.1311(7) 0.4693(5) 0.065(3) Uani 1 1 d . . . H2E H 0.4825 0.0736 0.4342 0.078 Uiso 1 1 calc R . . C3E C 0.6199(10) 0.1509(8) 0.5372(6) 0.087(3) Uani 1 1 d . . . H3E H 0.6612 0.1054 0.5461 0.105 Uiso 1 1 calc R . . C4E C 0.6655(9) 0.2335(7) 0.5889(6) 0.070(3) Uani 1 1 d . . . H4E H 0.7404 0.2478 0.6313 0.085 Uiso 1 1 calc R . . C5E C 0.5977(8) 0.2952(7) 0.5768(5) 0.064(3) Uani 1 1 d . . . H5E H 0.6239 0.3508 0.6139 0.076 Uiso 1 1 calc R . . C6E C 0.4913(8) 0.2781(6) 0.5112(5) 0.058(2) Uani 1 1 d . . . H6E H 0.4484 0.3229 0.5047 0.069 Uiso 1 1 calc R . . C1F C 0.2313(6) 0.0530(4) 0.3301(4) 0.0268(15) Uani 1 1 d . . . C2F C 0.3037(7) 0.0082(5) 0.2997(4) 0.0358(18) Uani 1 1 d . . . H2F H 0.3911 0.0409 0.3078 0.043 Uiso 1 1 calc R . . C3F C 0.2498(9) -0.0839(6) 0.2576(4) 0.049(2) Uani 1 1 d . . . H3F H 0.3001 -0.1137 0.2382 0.059 Uiso 1 1 calc R . . C4F C 0.1199(9) -0.1308(5) 0.2448(4) 0.054(2) Uani 1 1 d . . . H4F H 0.0831 -0.1934 0.2171 0.065 Uiso 1 1 calc R . . C5F C 0.0440(8) -0.0882(5) 0.2715(4) 0.050(2) Uani 1 1 d . . . H5F H -0.0439 -0.1209 0.2611 0.060 Uiso 1 1 calc R . . C6F C 0.0990(7) 0.0051(5) 0.3146(4) 0.0410(19) Uani 1 1 d . . . H6F H 0.0479 0.0350 0.3328 0.049 Uiso 1 1 calc R . . C1S C 0.6852(9) 0.9440(6) 0.2072(5) 0.100(4) Uani 1 1 d G . . C2S C 0.7840(7) 1.0311(6) 0.2389(5) 0.077(3) Uani 1 1 d G . . H2S H 0.8410 1.0581 0.2095 0.092 Uiso 1 1 calc R . . C3S C 0.7976(7) 1.0779(5) 0.3145(6) 0.102(4) Uani 1 1 d G . . H3S H 0.8638 1.1362 0.3356 0.122 Uiso 1 1 calc R . . C4S C 0.7124(11) 1.0376(8) 0.3584(4) 0.134(6) Uani 1 1 d G . . H4S H 0.7215 1.0690 0.4090 0.161 Uiso 1 1 calc R . . C5S C 0.6135(8) 0.9505(8) 0.3268(7) 0.153(9) Uani 1 1 d G . . H5S H 0.5565 0.9236 0.3562 0.184 Uiso 1 1 calc R . . C6S C 0.5999(6) 0.9037(5) 0.2512(8) 0.133(7) Uani 1 1 d G . . H6S H 0.5338 0.8454 0.2300 0.159 Uiso 1 1 calc R . . C7S C 0.6744(17) 0.8973(10) 0.1323(7) 0.206(10) Uani 1 1 d . . . H7S1 H 0.7213 0.9423 0.1036 0.309 Uiso 1 1 calc R . . H7S2 H 0.5852 0.8714 0.1018 0.309 Uiso 1 1 calc R . . H7S3 H 0.7094 0.8459 0.1397 0.309 Uiso 1 1 calc R . . C1X C 0.820(2) 0.3527(10) 0.4166(7) 0.166(13) Uiso 0.50 1 d PRD A -1 H1X1 H 0.7516 0.3260 0.4402 0.248 Uiso 0.50 1 calc PR B -1 H1X2 H 0.8608 0.3057 0.4091 0.248 Uiso 0.50 1 calc PR C -1 H1X3 H 0.7865 0.3702 0.3652 0.248 Uiso 0.50 1 calc PR D -1 C2X C 0.9202(15) 0.4422(10) 0.4727(10) 0.115(9) Uiso 0.50 1 d PGD A -1 C3X C 1.021(2) 0.4849(13) 0.4404(8) 0.111(8) Uiso 0.50 1 d PGD A -1 H3X H 1.0189 0.4606 0.3889 0.133 Uiso 0.50 1 calc PR A -1 C4X C 1.1246(15) 0.5639(13) 0.4849(11) 0.101(8) Uiso 0.50 1 d PGD A -1 H4X H 1.1919 0.5924 0.4633 0.121 Uiso 0.50 1 calc PR A -1 C5X C 1.1276(13) 0.6002(9) 0.5618(10) 0.119(9) Uiso 0.50 1 d PGD A -1 H5X H 1.1970 0.6530 0.5916 0.143 Uiso 0.50 1 calc PR A -1 C6X C 1.0270(16) 0.5575(10) 0.5941(7) 0.072(6) Uiso 0.50 1 d PGD A -1 H6X H 1.0290 0.5818 0.6455 0.086 Uiso 0.50 1 calc PR A -1 C7X C 0.9233(13) 0.4785(10) 0.5496(10) 0.062(5) Uiso 0.50 1 d PGD A -1 H7X H 0.8559 0.4499 0.5712 0.074 Uiso 0.50 1 calc PR A -1 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 0.0255(3) 0.0227(3) 0.0189(3) 0.0032(2) 0.0036(2) 0.0065(2) Br1 0.0273(4) 0.0375(4) 0.0372(4) 0.0074(3) 0.0072(3) 0.0098(3) P1 0.0326(11) 0.0280(10) 0.0242(10) 0.0049(8) 0.0056(8) 0.0091(8) P2 0.0327(10) 0.0249(10) 0.0230(9) 0.0032(8) 0.0045(8) 0.0101(8) S1 0.0305(10) 0.0323(10) 0.0295(10) -0.0020(8) 0.0003(8) 0.0073(8) O1 0.028(3) 0.035(3) 0.030(3) 0.001(2) 0.011(2) 0.012(2) O2 0.041(3) 0.034(3) 0.023(3) -0.001(2) 0.007(2) 0.014(2) N1 0.031(3) 0.031(3) 0.032(3) 0.007(3) 0.012(3) 0.012(3) C1 0.026(4) 0.030(4) 0.022(4) 0.008(3) 0.001(3) 0.006(3) C2 0.038(4) 0.018(4) 0.026(4) 0.002(3) 0.005(3) 0.003(3) C3 0.055(5) 0.029(4) 0.042(5) 0.003(4) 0.018(4) 0.014(4) C4 0.073(7) 0.037(5) 0.057(6) -0.005(4) 0.024(5) 0.023(5) C5 0.063(6) 0.039(5) 0.047(5) -0.014(4) 0.011(5) 0.009(4) C6 0.042(5) 0.032(4) 0.043(5) -0.009(4) 0.006(4) -0.001(4) C7 0.048(5) 0.030(4) 0.019(4) 0.004(3) 0.008(3) 0.009(4) C8 0.037(4) 0.038(4) 0.023(4) -0.005(3) -0.005(3) 0.009(4) C9 0.028(4) 0.029(4) 0.040(4) -0.003(3) 0.011(3) 0.008(3) C10 0.038(4) 0.034(4) 0.035(4) 0.004(3) 0.004(4) 0.010(4) C11 0.053(6) 0.051(5) 0.043(5) 0.013(4) 0.014(4) 0.019(4) C12 0.061(6) 0.054(6) 0.077(7) 0.025(5) 0.039(5) 0.022(5) C13 0.030(5) 0.048(5) 0.090(7) 0.016(5) 0.024(5) 0.013(4) C14 0.037(5) 0.040(5) 0.054(5) 0.006(4) 0.005(4) 0.013(4) C15 0.041(5) 0.026(4) 0.018(4) 0.001(3) 0.006(3) 0.001(3) C16 0.045(5) 0.041(5) 0.037(4) -0.007(4) 0.008(4) 0.005(4) C1A 0.037(4) 0.029(4) 0.022(4) 0.005(3) 0.007(3) 0.007(3) C2A 0.045(5) 0.037(4) 0.027(4) 0.009(3) 0.010(4) 0.009(4) C3A 0.039(5) 0.052(5) 0.035(4) 0.007(4) 0.008(4) 0.015(4) C4A 0.047(5) 0.058(6) 0.019(4) 0.005(4) 0.006(4) -0.004(4) C5A 0.076(7) 0.030(5) 0.052(5) -0.001(4) 0.020(5) 0.001(5) C6A 0.053(5) 0.030(4) 0.051(5) 0.003(4) 0.011(4) 0.008(4) C1B 0.036(4) 0.035(4) 0.037(4) 0.005(3) 0.011(3) 0.016(4) C2B 0.048(5) 0.032(4) 0.039(4) 0.005(3) 0.008(4) 0.022(4) C3B 0.064(6) 0.034(4) 0.048(5) 0.000(4) 0.018(4) 0.019(4) C4B 0.059(6) 0.040(5) 0.061(6) 0.010(4) 0.014(5) 0.025(4) C5B 0.085(7) 0.074(7) 0.053(6) 0.027(5) 0.016(5) 0.048(6) C6B 0.091(7) 0.066(6) 0.046(5) 0.033(5) 0.029(5) 0.050(6) C1C 0.029(4) 0.025(4) 0.027(4) 0.008(3) -0.001(3) 0.006(3) C2C 0.034(4) 0.037(4) 0.035(4) 0.012(4) 0.001(4) -0.001(4) C3C 0.047(5) 0.045(5) 0.030(4) 0.009(4) -0.004(4) -0.010(4) C4C 0.051(5) 0.045(5) 0.021(4) 0.000(4) -0.001(4) 0.001(4) C5C 0.052(5) 0.054(5) 0.024(4) 0.009(4) 0.011(4) 0.016(4) C6C 0.031(4) 0.038(4) 0.030(4) 0.010(3) 0.005(3) 0.002(3) C1D 0.030(4) 0.033(4) 0.024(4) 0.000(3) 0.010(3) 0.005(3) C2D 0.044(5) 0.041(5) 0.030(4) 0.007(3) 0.014(4) 0.014(4) C3D 0.053(5) 0.050(5) 0.048(5) -0.001(4) 0.016(4) 0.023(4) C4D 0.046(5) 0.052(5) 0.037(5) -0.003(4) 0.020(4) 0.002(4) C5D 0.059(6) 0.041(5) 0.038(5) 0.012(4) 0.024(4) -0.001(4) C6D 0.051(5) 0.036(4) 0.038(4) 0.007(4) 0.016(4) 0.010(4) C1E 0.042(4) 0.032(4) 0.025(4) 0.004(3) 0.003(3) 0.016(4) C2E 0.064(6) 0.065(6) 0.054(6) -0.005(5) -0.013(5) 0.033(5) C3E 0.075(7) 0.100(9) 0.086(8) 0.014(7) -0.017(6) 0.060(7) C4E 0.060(6) 0.048(6) 0.061(6) 0.007(5) -0.026(5) -0.006(5) C5E 0.052(6) 0.076(7) 0.042(5) -0.001(5) -0.005(4) 0.009(5) C6E 0.057(6) 0.070(6) 0.044(5) 0.000(5) 0.006(4) 0.028(5) C1F 0.033(4) 0.018(3) 0.027(4) 0.005(3) 0.005(3) 0.007(3) C2F 0.043(5) 0.024(4) 0.034(4) 0.006(3) 0.001(4) 0.011(3) C3F 0.070(6) 0.041(5) 0.034(4) 0.004(4) 0.007(4) 0.022(5) C4F 0.085(7) 0.026(4) 0.035(5) -0.008(4) -0.005(5) 0.015(5) C5F 0.061(6) 0.032(5) 0.036(5) 0.005(4) 0.005(4) -0.008(4) C6F 0.053(5) 0.041(5) 0.032(4) 0.014(4) 0.016(4) 0.014(4) C1S 0.070(8) 0.076(9) 0.143(12) 0.029(9) -0.005(8) 0.037(7) C2S 0.082(8) 0.073(8) 0.088(8) 0.033(6) 0.031(7) 0.034(7) C3S 0.077(9) 0.120(10) 0.128(12) 0.043(10) 0.020(8) 0.064(8) C4S 0.150(14) 0.24(2) 0.103(10) 0.088(12) 0.063(11) 0.157(15) C5S 0.047(8) 0.191(18) 0.27(2) 0.169(17) 0.067(12) 0.062(10) C6S 0.097(11) 0.115(11) 0.214(19) 0.105(13) 0.052(12) 0.053(9) C7S 0.31(2) 0.207(18) 0.095(11) -0.054(11) -0.074(13) 0.191(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.970(6) . ? Ru1 O1 2.130(4) . ? Ru1 O2 2.241(4) . ? Ru1 P2 2.3742(19) . ? Ru1 P1 2.3933(19) . ? Ru1 Br1 2.5434(12) . ? Ru1 C15 2.549(7) . ? P1 C1A 1.832(7) . ? P1 C1B 1.837(7) . ? P1 C1C 1.844(7) . ? P2 C1F 1.841(6) . ? P2 C1D 1.843(6) . ? P2 C1E 1.844(7) . ? S1 C7 1.726(7) . ? S1 C1 1.762(6) . ? O1 C15 1.296(7) . ? O2 C15 1.264(8) . ? N1 C1 1.373(8) . ? N1 C2 1.421(8) . ? N1 C8 1.466(8) . ? C2 C3 1.360(9) . ? C2 C7 1.407(9) . ? C3 C4 1.420(10) . ? C4 C5 1.379(11) . ? C5 C6 1.363(10) . ? C6 C7 1.380(9) . ? C8 C9 1.520(9) . ? C9 C10 1.372(9) . ? C9 C14 1.391(9) . ? C10 C11 1.382(10) . ? C11 C12 1.399(11) . ? C12 C13 1.372(11) . ? C13 C14 1.367(10) . ? C15 C16 1.492(9) . ? C1A C2A 1.388(9) . ? C1A C6A 1.389(9) . ? C2A C3A 1.391(10) . ? C3A C4A 1.368(10) . ? C4A C5A 1.370(11) . ? C5A C6A 1.383(11) . ? C1B C2B 1.382(9) . ? C1B C6B 1.389(9) . ? C2B C3B 1.383(9) . ? C3B C4B 1.378(10) . ? C4B C5B 1.346(11) . ? C5B C6B 1.398(11) . ? C1C C6C 1.390(9) . ? C1C C2C 1.396(9) . ? C2C C3C 1.384(9) . ? C3C C4C 1.367(10) . ? C4C C5C 1.367(10) . ? C5C C6C 1.398(9) . ? C1D C2D 1.376(9) . ? C1D C6D 1.385(9) . ? C2D C3D 1.394(9) . ? C3D C4D 1.350(10) . ? C4D C5D 1.360(10) . ? C5D C6D 1.378(10) . ? C1E C2E 1.360(10) . ? C1E C6E 1.386(10) . ? C2E C3E 1.416(11) . ? C3E C4E 1.343(12) . ? C4E C5E 1.355(12) . ? C5E C6E 1.379(11) . ? C1F C2F 1.378(9) . ? C1F C6F 1.397(9) . ? C2F C3F 1.377(9) . ? C3F C4F 1.376(11) . ? C4F C5F 1.361(11) . ? C5F C6F 1.398(10) . ? C1S C7S 1.389(13) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C1X C2X 1.532(16) . ? C2X C3X 1.3900 . ? C2X C7X 1.3900 . ? C3X C4X 1.3900 . ? C4X C5X 1.3900 . ? C5X C6X 1.3900 . ? C6X C7X 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 O1 106.8(2) . . ? C1 Ru1 O2 166.9(2) . . ? O1 Ru1 O2 60.19(16) . . ? C1 Ru1 P2 90.52(18) . . ? O1 Ru1 P2 90.31(12) . . ? O2 Ru1 P2 91.38(12) . . ? C1 Ru1 P1 95.38(18) . . ? O1 Ru1 P1 90.28(12) . . ? O2 Ru1 P1 83.42(12) . . ? P2 Ru1 P1 173.63(6) . . ? C1 Ru1 Br1 89.86(18) . . ? O1 Ru1 Br1 163.32(12) . . ? O2 Ru1 Br1 103.18(12) . . ? P2 Ru1 Br1 88.64(5) . . ? P1 Ru1 Br1 88.97(5) . . ? C1 Ru1 C15 137.2(3) . . ? O1 Ru1 C15 30.52(19) . . ? O2 Ru1 C15 29.73(18) . . ? P2 Ru1 C15 92.28(15) . . ? P1 Ru1 C15 85.03(15) . . ? Br1 Ru1 C15 132.90(17) . . ? C1A P1 C1B 102.7(3) . . ? C1A P1 C1C 105.4(3) . . ? C1B P1 C1C 99.5(3) . . ? C1A P1 Ru1 112.1(2) . . ? C1B P1 Ru1 117.5(2) . . ? C1C P1 Ru1 117.7(2) . . ? C1F P2 C1D 102.8(3) . . ? C1F P2 C1E 106.6(3) . . ? C1D P2 C1E 97.0(3) . . ? C1F P2 Ru1 113.4(2) . . ? C1D P2 Ru1 118.0(2) . . ? C1E P2 Ru1 116.8(2) . . ? C7 S1 C1 94.4(3) . . ? C15 O1 Ru1 92.9(4) . . ? C15 O2 Ru1 88.8(4) . . ? C1 N1 C2 117.9(6) . . ? C1 N1 C8 124.2(5) . . ? C2 N1 C8 117.8(5) . . ? N1 C1 S1 106.6(5) . . ? N1 C1 Ru1 130.8(5) . . ? S1 C1 Ru1 122.3(4) . . ? C3 C2 C7 122.4(6) . . ? C3 C2 N1 127.0(7) . . ? C7 C2 N1 110.6(6) . . ? C2 C3 C4 116.4(7) . . ? C5 C4 C3 121.1(7) . . ? C6 C5 C4 121.4(7) . . ? C5 C6 C7 118.8(7) . . ? C6 C7 C2 119.9(7) . . ? C6 C7 S1 129.7(6) . . ? C2 C7 S1 110.4(5) . . ? N1 C8 C9 114.3(5) . . ? C10 C9 C14 118.4(7) . . ? C10 C9 C8 123.4(6) . . ? C14 C9 C8 118.2(6) . . ? C9 C10 C11 121.2(7) . . ? C10 C11 C12 119.3(7) . . ? C13 C12 C11 119.7(8) . . ? C14 C13 C12 120.1(8) . . ? C13 C14 C9 121.3(8) . . ? O2 C15 O1 117.9(6) . . ? O2 C15 C16 122.2(6) . . ? O1 C15 C16 119.9(6) . . ? O2 C15 Ru1 61.5(3) . . ? O1 C15 Ru1 56.5(3) . . ? C16 C15 Ru1 174.0(5) . . ? C2A C1A C6A 117.1(7) . . ? C2A C1A P1 118.8(5) . . ? C6A C1A P1 123.9(6) . . ? C1A C2A C3A 122.2(7) . . ? C4A C3A C2A 118.8(7) . . ? C3A C4A C5A 120.4(8) . . ? C4A C5A C6A 120.4(8) . . ? C5A C6A C1A 121.0(8) . . ? C2B C1B C6B 118.5(7) . . ? C2B C1B P1 120.5(5) . . ? C6B C1B P1 120.9(6) . . ? C1B C2B C3B 120.8(7) . . ? C4B C3B C2B 119.6(7) . . ? C5B C4B C3B 120.7(8) . . ? C4B C5B C6B 120.2(8) . . ? C1B C6B C5B 120.1(8) . . ? C6C C1C C2C 119.6(6) . . ? C6C C1C P1 123.7(5) . . ? C2C C1C P1 116.5(5) . . ? C3C C2C C1C 120.0(7) . . ? C4C C3C C2C 119.5(7) . . ? C5C C4C C3C 121.9(7) . . ? C4C C5C C6C 119.4(7) . . ? C1C C6C C5C 119.6(7) . . ? C2D C1D C6D 118.7(6) . . ? C2D C1D P2 121.5(5) . . ? C6D C1D P2 119.5(5) . . ? C1D C2D C3D 118.4(7) . . ? C4D C3D C2D 122.1(8) . . ? C3D C4D C5D 119.8(7) . . ? C4D C5D C6D 119.3(7) . . ? C5D C6D C1D 121.5(7) . . ? C2E C1E C6E 116.8(7) . . ? C2E C1E P2 127.6(6) . . ? C6E C1E P2 115.2(5) . . ? C1E C2E C3E 120.6(8) . . ? C4E C3E C2E 121.9(9) . . ? C3E C4E C5E 117.2(9) . . ? C4E C5E C6E 122.2(9) . . ? C5E C6E C1E 121.1(8) . . ? C2F C1F C6F 118.9(6) . . ? C2F C1F P2 121.5(5) . . ? C6F C1F P2 118.7(5) . . ? C3F C2F C1F 121.6(7) . . ? C4F C3F C2F 118.6(8) . . ? C5F C4F C3F 121.8(7) . . ? C4F C5F C6F 119.5(8) . . ? C1F C6F C5F 119.6(7) . . ? C7S C1S C2S 119.3(11) . . ? C7S C1S C6S 120.7(11) . . ? C2S C1S C6S 120.0 . . ? C3S C2S C1S 120.0 . . ? C4S C3S C2S 120.0 . . ? C3S C4S C5S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? C3X C2X C7X 120.0 . . ? C3X C2X C1X 111.8(15) . . ? C7X C2X C1X 128.1(15) . . ? C2X C3X C4X 120.0 . . ? C5X C4X C3X 120.0 . . ? C6X C5X C4X 120.0 . . ? C5X C6X C7X 120.0 . . ? C6X C7X C2X 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.883 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.106 data_5 _database_code_depnum_ccdc_archive 'CCDC 778717' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H46 Br N O2 P2 Ru S' _chemical_formula_weight 1003.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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' Br Br -0.2901 2.4595 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9427(4) _cell_length_b 24.1566(10) _cell_length_c 18.7354(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.8130(10) _cell_angle_gamma 90.00 _cell_volume 4476.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4536 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.35 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 1.404 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7665 _exptl_absorpt_correction_T_max 0.8723 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31658 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10257 _reflns_number_gt 7837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10257 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 0.35679(2) 0.416039(10) 0.245081(12) 0.02074(8) Uani 1 1 d . . . Br1 Br 0.58753(3) 0.448958(14) 0.301752(17) 0.03027(10) Uani 1 1 d . . . S1 S 0.39020(9) 0.43914(4) 0.41898(4) 0.0320(2) Uani 1 1 d . . . P1 P 0.44204(8) 0.32432(3) 0.23725(4) 0.02395(18) Uani 1 1 d . . . P2 P 0.29021(8) 0.51054(3) 0.23199(4) 0.02215(18) Uani 1 1 d . . . N1 N 0.1684(3) 0.40208(11) 0.36135(13) 0.0279(6) Uani 1 1 d . . . O1 O 0.1881(2) 0.39211(9) 0.16934(10) 0.0258(5) Uani 1 1 d . . . O2 O 0.3793(2) 0.41130(9) 0.12687(11) 0.0272(5) Uani 1 1 d . . . C1 C 0.2927(3) 0.41490(13) 0.34121(16) 0.0252(7) Uani 1 1 d . . . C2 C 0.1426(4) 0.41558(14) 0.43185(16) 0.0308(8) Uani 1 1 d . . . C3 C 0.0201(4) 0.41069(16) 0.46160(18) 0.0400(9) Uani 1 1 d . . . H3 H -0.0572 0.3964 0.4348 0.048 Uiso 1 1 calc R . . C4 C 0.0165(5) 0.42767(17) 0.5321(2) 0.0496(11) Uani 1 1 d . . . H4 H -0.0644 0.4243 0.5537 0.059 Uiso 1 1 calc R . . C5 C 0.1298(5) 0.44946(17) 0.5714(2) 0.0495(11) Uani 1 1 d . . . H5 H 0.1241 0.4609 0.6189 0.059 Uiso 1 1 calc R . . C6 C 0.2505(4) 0.45458(15) 0.54202(18) 0.0413(9) Uani 1 1 d . . . H6 H 0.3271 0.4697 0.5685 0.050 Uiso 1 1 calc R . . C7 C 0.2555(4) 0.43656(14) 0.47140(17) 0.0320(8) Uani 1 1 d . . . C8 C 0.0638(3) 0.37319(15) 0.31439(17) 0.0322(8) Uani 1 1 d . . . H8A H 0.0947 0.3690 0.2666 0.039 Uiso 1 1 calc R . . H8B H -0.0186 0.3957 0.3094 0.039 Uiso 1 1 calc R . . C9 C 0.0316(3) 0.31687(14) 0.34294(15) 0.0293(7) Uani 1 1 d . . . C10 C 0.1304(4) 0.28293(15) 0.37718(18) 0.0362(8) Uani 1 1 d . . . H10 H 0.2197 0.2959 0.3859 0.043 Uiso 1 1 calc R . . C11 C 0.0986(4) 0.23028(16) 0.39866(19) 0.0453(10) Uani 1 1 d . . . H11 H 0.1667 0.2077 0.4217 0.054 Uiso 1 1 calc R . . C12 C -0.0305(4) 0.21060(17) 0.3869(2) 0.0490(10) Uani 1 1 d . . . H12 H -0.0513 0.1748 0.4020 0.059 Uiso 1 1 calc R . . C13 C -0.1302(4) 0.24364(18) 0.3527(2) 0.0533(11) Uani 1 1 d . . . H13 H -0.2191 0.2303 0.3440 0.064 Uiso 1 1 calc R . . C14 C -0.0993(4) 0.29624(17) 0.33122(19) 0.0438(10) Uani 1 1 d . . . H14 H -0.1679 0.3186 0.3082 0.053 Uiso 1 1 calc R . . C15 C 0.2567(3) 0.39716(13) 0.11561(16) 0.0260(7) Uani 1 1 d . . . C16 C 0.1893(4) 0.38657(15) 0.04115(17) 0.0366(8) Uani 1 1 d . . . H16A H 0.2584 0.3783 0.0089 0.044 Uiso 1 1 calc R . . H16B H 0.1300 0.3542 0.0421 0.044 Uiso 1 1 calc R . . C17 C 0.1075(5) 0.43579(19) 0.0128(2) 0.0602(13) Uani 1 1 d . . . H17A H 0.0321 0.4412 0.0412 0.090 Uiso 1 1 calc R . . H17B H 0.0735 0.4293 -0.0368 0.090 Uiso 1 1 calc R . . H17C H 0.1642 0.4686 0.0159 0.090 Uiso 1 1 calc R . . C1A C 0.4793(3) 0.28287(14) 0.31892(16) 0.0288(7) Uani 1 1 d . . . C2A C 0.5465(4) 0.30894(15) 0.37845(16) 0.0342(8) Uani 1 1 d . . . H2A H 0.5654 0.3470 0.3769 0.041 Uiso 1 1 calc R . . C3A C 0.5859(4) 0.27873(17) 0.44041(18) 0.0470(10) Uani 1 1 d . . . H3A H 0.6321 0.2964 0.4803 0.056 Uiso 1 1 calc R . . C4A C 0.5574(4) 0.22309(17) 0.44351(19) 0.0461(10) Uani 1 1 d . . . H4A H 0.5834 0.2030 0.4856 0.055 Uiso 1 1 calc R . . C5A C 0.4907(4) 0.19688(17) 0.3849(2) 0.0476(10) Uani 1 1 d . . . H5A H 0.4717 0.1588 0.3869 0.057 Uiso 1 1 calc R . . C6A C 0.4515(4) 0.22657(15) 0.32280(19) 0.0402(9) Uani 1 1 d . . . H6A H 0.4057 0.2085 0.2831 0.048 Uiso 1 1 calc R . . C1B C 0.3324(3) 0.27963(13) 0.17703(16) 0.0269(7) Uani 1 1 d . . . C2B C 0.2157(4) 0.25679(14) 0.19872(19) 0.0347(8) Uani 1 1 d . . . H2B H 0.1919 0.2639 0.2451 0.042 Uiso 1 1 calc R . . C3B C 0.1335(4) 0.22340(16) 0.1524(2) 0.0461(10) Uani 1 1 d . . . H3B H 0.0551 0.2077 0.1681 0.055 Uiso 1 1 calc R . . C4B C 0.1655(4) 0.21295(16) 0.0833(2) 0.0478(11) Uani 1 1 d . . . H4B H 0.1107 0.1897 0.0524 0.057 Uiso 1 1 calc R . . C5B C 0.2777(4) 0.23699(16) 0.0611(2) 0.0451(10) Uani 1 1 d . . . H5B H 0.2985 0.2313 0.0138 0.054 Uiso 1 1 calc R . . C6B C 0.3621(4) 0.26980(14) 0.10706(17) 0.0333(8) Uani 1 1 d . . . H6B H 0.4399 0.2855 0.0908 0.040 Uiso 1 1 calc R . . C1C C 0.6020(3) 0.31691(14) 0.19657(16) 0.0273(7) Uani 1 1 d . . . C2C C 0.6555(4) 0.26383(15) 0.18832(19) 0.0378(9) Uani 1 1 d . . . H2C H 0.6123 0.2329 0.2061 0.045 Uiso 1 1 calc R . . C3C C 0.7713(4) 0.25658(17) 0.1542(2) 0.0504(11) Uani 1 1 d . . . H3C H 0.8041 0.2207 0.1471 0.061 Uiso 1 1 calc R . . C4C C 0.8390(4) 0.30215(18) 0.1306(2) 0.0486(10) Uani 1 1 d . . . H4C H 0.9188 0.2974 0.1084 0.058 Uiso 1 1 calc R . . C5C C 0.7887(4) 0.35412(17) 0.13977(18) 0.0396(9) Uani 1 1 d . . . H5C H 0.8358 0.3850 0.1247 0.048 Uiso 1 1 calc R . . C6C C 0.6694(3) 0.36192(14) 0.17090(16) 0.0299(8) Uani 1 1 d . . . H6C H 0.6341 0.3978 0.1746 0.036 Uiso 1 1 calc R . . C1D C 0.1103(3) 0.53037(13) 0.22630(16) 0.0254(7) Uani 1 1 d . . . C2D C 0.0106(4) 0.49138(15) 0.21005(18) 0.0352(8) Uani 1 1 d . . . H2D H 0.0345 0.4543 0.2026 0.042 Uiso 1 1 calc R . . C3D C -0.1242(4) 0.50632(17) 0.2046(2) 0.0480(10) Uani 1 1 d . . . H3D H -0.1914 0.4793 0.1943 0.058 Uiso 1 1 calc R . . C4D C -0.1609(4) 0.56054(18) 0.2141(2) 0.0505(11) Uani 1 1 d . . . H4D H -0.2527 0.5706 0.2104 0.061 Uiso 1 1 calc R . . C5D C -0.0624(4) 0.59980(17) 0.2291(2) 0.0451(10) Uani 1 1 d . . . H5D H -0.0868 0.6370 0.2346 0.054 Uiso 1 1 calc R . . C6D C 0.0722(4) 0.58493(15) 0.23600(19) 0.0388(9) Uani 1 1 d . . . H6D H 0.1388 0.6120 0.2474 0.047 Uiso 1 1 calc R . . C1E C 0.3624(3) 0.55969(13) 0.29980(16) 0.0244(7) Uani 1 1 d . . . C2E C 0.3073(4) 0.56196(15) 0.36510(17) 0.0320(8) Uani 1 1 d . . . H2E H 0.2316 0.5402 0.3724 0.038 Uiso 1 1 calc R . . C3E C 0.3641(4) 0.59630(16) 0.41947(18) 0.0409(9) Uani 1 1 d . . . H3E H 0.3268 0.5975 0.4636 0.049 Uiso 1 1 calc R . . C4E C 0.4744(4) 0.62865(15) 0.40917(18) 0.0389(9) Uani 1 1 d . . . H4E H 0.5120 0.6519 0.4462 0.047 Uiso 1 1 calc R . . C5E C 0.5301(4) 0.62712(15) 0.34456(18) 0.0369(8) Uani 1 1 d . . . H5E H 0.6052 0.6494 0.3375 0.044 Uiso 1 1 calc R . . C6E C 0.4743(3) 0.59234(14) 0.28982(17) 0.0311(8) Uani 1 1 d . . . H6E H 0.5125 0.5910 0.2460 0.037 Uiso 1 1 calc R . . C1F C 0.3429(3) 0.53814(13) 0.14802(16) 0.0261(7) Uani 1 1 d . . . C2F C 0.2572(4) 0.56755(14) 0.09902(17) 0.0346(8) Uani 1 1 d . . . H2F H 0.1683 0.5751 0.1090 0.041 Uiso 1 1 calc R . . C3F C 0.3013(4) 0.58589(16) 0.03528(18) 0.0442(10) Uani 1 1 d . . . H3F H 0.2421 0.6060 0.0027 0.053 Uiso 1 1 calc R . . C4F C 0.4298(5) 0.57515(15) 0.01922(19) 0.0430(10) Uani 1 1 d . . . H4F H 0.4584 0.5873 -0.0244 0.052 Uiso 1 1 calc R . . C5F C 0.5172(4) 0.54629(14) 0.06764(19) 0.0390(9) Uani 1 1 d . . . H5F H 0.6063 0.5395 0.0574 0.047 Uiso 1 1 calc R . . C6F C 0.4741(4) 0.52725(14) 0.13153(17) 0.0309(8) Uani 1 1 d . . . H6F H 0.5336 0.5069 0.1638 0.037 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 0.02146(14) 0.02183(14) 0.01852(12) 0.00013(10) -0.00002(9) -0.00077(10) Br1 0.02463(18) 0.0341(2) 0.03135(17) -0.00355(14) -0.00094(13) -0.00330(14) S1 0.0345(5) 0.0403(5) 0.0204(4) -0.0038(4) -0.0010(3) -0.0026(4) P1 0.0238(4) 0.0236(4) 0.0238(4) 0.0001(3) -0.0007(3) 0.0010(3) P2 0.0221(4) 0.0222(4) 0.0221(4) -0.0003(3) 0.0022(3) -0.0008(3) N1 0.0300(16) 0.0309(16) 0.0230(13) 0.0020(12) 0.0039(11) -0.0002(12) O1 0.0273(12) 0.0276(12) 0.0220(10) -0.0011(9) -0.0007(9) 0.0009(10) O2 0.0310(13) 0.0270(12) 0.0236(11) -0.0001(9) 0.0029(9) 0.0019(10) C1 0.0285(18) 0.0228(16) 0.0235(15) -0.0003(13) -0.0011(13) 0.0005(14) C2 0.036(2) 0.0310(19) 0.0259(16) 0.0053(14) 0.0074(14) 0.0061(16) C3 0.039(2) 0.047(2) 0.0356(19) 0.0019(17) 0.0120(16) 0.0047(18) C4 0.058(3) 0.053(3) 0.042(2) 0.003(2) 0.028(2) 0.010(2) C5 0.074(3) 0.046(3) 0.0305(19) -0.0001(18) 0.019(2) 0.016(2) C6 0.054(3) 0.040(2) 0.0293(18) -0.0028(16) 0.0045(17) 0.0061(19) C7 0.040(2) 0.0323(19) 0.0242(16) 0.0027(14) 0.0058(15) 0.0050(16) C8 0.0276(18) 0.041(2) 0.0276(16) 0.0043(15) 0.0016(14) -0.0059(16) C9 0.0296(18) 0.037(2) 0.0221(15) 0.0004(14) 0.0049(13) -0.0063(15) C10 0.032(2) 0.042(2) 0.0342(18) 0.0032(16) 0.0003(15) -0.0064(17) C11 0.058(3) 0.041(2) 0.035(2) 0.0005(17) -0.0041(18) 0.000(2) C12 0.060(3) 0.036(2) 0.051(2) 0.0000(19) 0.003(2) -0.017(2) C13 0.040(2) 0.056(3) 0.063(3) -0.002(2) 0.005(2) -0.019(2) C14 0.033(2) 0.052(3) 0.044(2) 0.0030(19) -0.0020(17) -0.0079(19) C15 0.0330(19) 0.0195(16) 0.0249(16) 0.0002(13) -0.0007(14) 0.0037(14) C16 0.043(2) 0.039(2) 0.0265(17) -0.0031(16) -0.0055(15) 0.0002(17) C17 0.064(3) 0.074(3) 0.037(2) 0.000(2) -0.019(2) 0.017(3) C1A 0.0267(18) 0.0321(19) 0.0269(16) 0.0047(14) -0.0006(13) 0.0058(15) C2A 0.043(2) 0.032(2) 0.0267(16) -0.0017(15) -0.0017(15) 0.0089(16) C3A 0.065(3) 0.048(3) 0.0257(18) -0.0048(17) -0.0040(18) 0.020(2) C4A 0.061(3) 0.048(3) 0.0291(18) 0.0090(18) 0.0039(18) 0.021(2) C5A 0.060(3) 0.037(2) 0.045(2) 0.0152(18) -0.001(2) 0.003(2) C6A 0.050(2) 0.033(2) 0.0368(19) 0.0066(16) -0.0031(17) -0.0003(18) C1B 0.0291(18) 0.0213(17) 0.0289(16) 0.0005(13) -0.0038(13) 0.0014(14) C2B 0.031(2) 0.035(2) 0.0373(19) 0.0045(16) -0.0036(15) 0.0007(16) C3B 0.028(2) 0.039(2) 0.067(3) 0.014(2) -0.0116(19) -0.0074(17) C4B 0.052(3) 0.032(2) 0.053(2) -0.0057(18) -0.025(2) -0.0031(19) C5B 0.056(3) 0.040(2) 0.035(2) -0.0067(17) -0.0151(18) 0.009(2) C6B 0.032(2) 0.035(2) 0.0310(17) -0.0029(15) -0.0059(14) 0.0054(16) C1C 0.0250(17) 0.0319(19) 0.0239(15) -0.0015(14) -0.0027(13) 0.0028(14) C2C 0.033(2) 0.036(2) 0.044(2) -0.0007(17) 0.0019(16) 0.0028(16) C3C 0.041(2) 0.042(2) 0.068(3) -0.003(2) 0.008(2) 0.016(2) C4C 0.037(2) 0.059(3) 0.052(2) 0.002(2) 0.0162(18) 0.008(2) C5C 0.036(2) 0.050(2) 0.0332(18) 0.0072(17) 0.0063(16) 0.0026(18) C6C 0.0332(19) 0.0323(19) 0.0239(16) -0.0018(14) 0.0006(14) 0.0013(15) C1D 0.0228(17) 0.0281(18) 0.0254(15) 0.0019(13) 0.0023(13) 0.0030(14) C2D 0.030(2) 0.0299(19) 0.046(2) 0.0029(16) 0.0063(16) 0.0023(15) C3D 0.025(2) 0.046(2) 0.073(3) 0.001(2) 0.0052(19) -0.0005(18) C4D 0.029(2) 0.057(3) 0.067(3) -0.004(2) 0.0059(19) 0.006(2) C5D 0.040(2) 0.040(2) 0.055(2) -0.0067(19) 0.0013(18) 0.0154(19) C6D 0.034(2) 0.033(2) 0.048(2) -0.0049(17) -0.0020(17) 0.0026(17) C1E 0.0278(18) 0.0210(16) 0.0237(15) -0.0021(13) 0.0003(13) 0.0030(14) C2E 0.0299(19) 0.034(2) 0.0319(17) -0.0028(15) 0.0035(15) -0.0038(15) C3E 0.047(2) 0.047(2) 0.0290(18) -0.0075(17) 0.0060(16) 0.0018(19) C4E 0.047(2) 0.033(2) 0.0352(19) -0.0105(16) -0.0054(17) -0.0028(18) C5E 0.039(2) 0.034(2) 0.0363(19) 0.0002(16) -0.0031(16) -0.0069(17) C6E 0.0334(19) 0.0314(19) 0.0281(16) -0.0013(14) 0.0019(14) -0.0022(15) C1F 0.0304(18) 0.0250(17) 0.0230(15) -0.0014(13) 0.0037(13) -0.0018(14) C2F 0.039(2) 0.035(2) 0.0298(17) 0.0048(15) 0.0017(15) -0.0033(16) C3F 0.059(3) 0.043(2) 0.0293(18) 0.0099(17) -0.0031(18) -0.008(2) C4F 0.064(3) 0.039(2) 0.0276(18) -0.0005(16) 0.0117(18) -0.020(2) C5F 0.051(2) 0.030(2) 0.039(2) -0.0064(16) 0.0183(18) -0.0079(17) C6F 0.036(2) 0.0241(18) 0.0336(18) 0.0006(14) 0.0083(15) -0.0018(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 C1 1.970(3) . ? Ru1 O1 2.163(2) . ? Ru1 O2 2.251(2) . ? Ru1 P1 2.3820(9) . ? Ru1 P2 2.3825(9) . ? Ru1 Br1 2.5553(4) . ? Ru1 C15 2.568(3) . ? S1 C7 1.740(4) . ? S1 C1 1.766(3) . ? P1 C1A 1.835(3) . ? P1 C1B 1.838(3) . ? P1 C1C 1.840(3) . ? P2 C1E 1.831(3) . ? P2 C1F 1.833(3) . ? P2 C1D 1.845(3) . ? N1 C1 1.364(4) . ? N1 C2 1.409(4) . ? N1 C8 1.468(4) . ? O1 C15 1.278(4) . ? O2 C15 1.263(4) . ? C2 C7 1.377(5) . ? C2 C3 1.395(5) . ? C3 C4 1.387(5) . ? C4 C5 1.386(6) . ? C5 C6 1.375(6) . ? C6 C7 1.399(4) . ? C8 C9 1.508(5) . ? C9 C10 1.386(5) . ? C9 C14 1.390(5) . ? C10 C11 1.380(5) . ? C11 C12 1.366(6) . ? C12 C13 1.379(6) . ? C13 C14 1.377(6) . ? C15 C16 1.507(4) . ? C16 C17 1.506(5) . ? C1A C6A 1.391(5) . ? C1A C2A 1.391(4) . ? C2A C3A 1.393(5) . ? C3A C4A 1.376(6) . ? C4A C5A 1.378(5) . ? C5A C6A 1.388(5) . ? C1B C2B 1.382(5) . ? C1B C6B 1.393(4) . ? C2B C3B 1.389(5) . ? C3B C4B 1.388(6) . ? C4B C5B 1.360(6) . ? C5B C6B 1.388(5) . ? C1C C6C 1.389(5) . ? C1C C2C 1.403(5) . ? C2C C3C 1.383(5) . ? C3C C4C 1.386(6) . ? C4C C5C 1.368(5) . ? C5C C6C 1.387(5) . ? C1D C2D 1.379(5) . ? C1D C6D 1.388(5) . ? C2D C3D 1.382(5) . ? C3D C4D 1.376(6) . ? C4D C5D 1.372(6) . ? C5D C6D 1.379(5) . ? C1E C6E 1.391(5) . ? C1E C2E 1.391(4) . ? C2E C3E 1.388(5) . ? C3E C4E 1.376(5) . ? C4E C5E 1.382(5) . ? C5E C6E 1.397(4) . ? C1F C2F 1.384(4) . ? C1F C6F 1.395(5) . ? C2F C3F 1.386(5) . ? C3F C4F 1.367(6) . ? C4F C5F 1.380(6) . ? C5F C6F 1.390(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 C1 Ru1 O1 107.15(11) . . ? C1 Ru1 O2 166.40(11) . . ? O1 Ru1 O2 59.25(8) . . ? C1 Ru1 P1 101.15(9) . . ? O1 Ru1 P1 88.18(6) . . ? O2 Ru1 P1 79.67(6) . . ? C1 Ru1 P2 89.73(9) . . ? O1 Ru1 P2 89.97(6) . . ? O2 Ru1 P2 90.10(6) . . ? P1 Ru1 P2 169.03(3) . . ? C1 Ru1 Br1 89.10(9) . . ? O1 Ru1 Br1 163.67(6) . . ? O2 Ru1 Br1 104.49(6) . . ? P1 Ru1 Br1 90.28(2) . . ? P2 Ru1 Br1 88.45(2) . . ? C1 Ru1 C15 136.94(12) . . ? O1 Ru1 C15 29.79(9) . . ? O2 Ru1 C15 29.46(9) . . ? P1 Ru1 C15 83.28(7) . . ? P2 Ru1 C15 89.76(7) . . ? Br1 Ru1 C15 133.92(8) . . ? C7 S1 C1 93.69(16) . . ? C1A P1 C1B 104.38(15) . . ? C1A P1 C1C 100.51(15) . . ? C1B P1 C1C 99.93(15) . . ? C1A P1 Ru1 119.95(11) . . ? C1B P1 Ru1 113.05(11) . . ? C1C P1 Ru1 116.35(11) . . ? C1E P2 C1F 103.49(14) . . ? C1E P2 C1D 100.46(15) . . ? C1F P2 C1D 102.46(15) . . ? C1E P2 Ru1 117.67(10) . . ? C1F P2 Ru1 109.64(11) . . ? C1D P2 Ru1 120.83(11) . . ? C1 N1 C2 117.5(3) . . ? C1 N1 C8 123.3(3) . . ? C2 N1 C8 119.1(3) . . ? C15 O1 Ru1 92.93(19) . . ? C15 O2 Ru1 89.30(18) . . ? N1 C1 S1 106.5(2) . . ? N1 C1 Ru1 129.9(2) . . ? S1 C1 Ru1 123.25(18) . . ? C7 C2 C3 120.9(3) . . ? C7 C2 N1 112.0(3) . . ? C3 C2 N1 127.1(3) . . ? C4 C3 C2 117.6(4) . . ? C5 C4 C3 121.3(4) . . ? C6 C5 C4 121.2(3) . . ? C5 C6 C7 117.8(4) . . ? C2 C7 C6 121.2(3) . . ? C2 C7 S1 110.0(2) . . ? C6 C7 S1 128.8(3) . . ? N1 C8 C9 112.3(3) . . ? C10 C9 C14 118.0(3) . . ? C10 C9 C8 122.2(3) . . ? C14 C9 C8 119.8(3) . . ? C11 C10 C9 120.5(4) . . ? C12 C11 C10 120.8(4) . . ? C11 C12 C13 119.6(4) . . ? C14 C13 C12 119.9(4) . . ? C13 C14 C9 121.2(4) . . ? O2 C15 O1 118.5(3) . . ? O2 C15 C16 122.1(3) . . ? O1 C15 C16 119.4(3) . . ? O2 C15 Ru1 61.24(15) . . ? O1 C15 Ru1 57.28(15) . . ? C16 C15 Ru1 176.4(3) . . ? C17 C16 C15 111.4(3) . . ? C6A C1A C2A 118.8(3) . . ? C6A C1A P1 123.6(3) . . ? C2A C1A P1 117.5(3) . . ? C1A C2A C3A 120.2(3) . . ? C4A C3A C2A 120.3(4) . . ? C3A C4A C5A 120.0(3) . . ? C4A C5A C6A 120.1(4) . . ? C5A C6A C1A 120.6(4) . . ? C2B C1B C6B 118.2(3) . . ? C2B C1B P1 121.2(3) . . ? C6B C1B P1 120.6(3) . . ? C1B C2B C3B 120.5(3) . . ? C4B C3B C2B 120.8(4) . . ? C5B C4B C3B 118.7(3) . . ? C4B C5B C6B 121.1(4) . . ? C5B C6B C1B 120.6(4) . . ? C6C C1C C2C 118.4(3) . . ? C6C C1C P1 122.3(3) . . ? C2C C1C P1 119.2(3) . . ? C3C C2C C1C 120.6(4) . . ? C2C C3C C4C 120.1(4) . . ? C5C C4C C3C 119.5(4) . . ? C4C C5C C6C 121.1(4) . . ? C5C C6C C1C 120.2(3) . . ? C2D C1D C6D 118.5(3) . . ? C2D C1D P2 120.4(3) . . ? C6D C1D P2 121.0(3) . . ? C1D C2D C3D 120.5(3) . . ? C4D C3D C2D 120.5(4) . . ? C5D C4D C3D 119.4(4) . . ? C4D C5D C6D 120.3(4) . . ? C5D C6D C1D 120.7(4) . . ? C6E C1E C2E 119.1(3) . . ? C6E C1E P2 122.5(2) . . ? C2E C1E P2 118.3(3) . . ? C3E C2E C1E 120.1(3) . . ? C4E C3E C2E 120.4(3) . . ? C3E C4E C5E 120.2(3) . . ? C4E C5E C6E 119.6(3) . . ? C1E C6E C5E 120.4(3) . . ? C2F C1F C6F 118.5(3) . . ? C2F C1F P2 123.0(3) . . ? C6F C1F P2 118.5(2) . . ? C1F C2F C3F 120.5(4) . . ? C4F C3F C2F 120.9(4) . . ? C3F C4F C5F 119.4(3) . . ? C4F C5F C6F 120.3(4) . . ? C5F C6F C1F 120.3(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.268 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.097 data_6 _database_code_depnum_ccdc_archive 'CCDC 778718' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H52 I N O2 P2 Ru S' _chemical_formula_weight 1080.95 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' S S 0.1246 0.1234 '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' I I -0.4742 1.8119 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.0266(6) _cell_length_b 15.0002(6) _cell_length_c 20.3236(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.5390(10) _cell_angle_gamma 90.00 _cell_volume 4860.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9266 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.51 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 1.109 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6781 _exptl_absorpt_correction_T_max 0.8254 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57081 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11151 _reflns_number_gt 10310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+4.9162P] 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 contr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11151 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 0.780702(12) 0.687446(13) 0.419065(10) 0.01959(6) Uani 1 1 d . . . I1 I 0.711518(12) 0.746359(12) 0.513198(10) 0.03058(6) Uani 1 1 d . . . S1 S 0.58141(4) 0.73757(5) 0.34782(4) 0.03126(16) Uani 1 1 d . . . P1 P 0.72201(4) 0.54544(4) 0.42509(3) 0.02261(14) Uani 1 1 d . . . P2 P 0.86598(4) 0.81846(4) 0.44306(3) 0.02302(14) Uani 1 1 d . . . N1 N 0.67243(14) 0.75025(15) 0.27333(12) 0.0266(5) Uani 1 1 d . . . O2 O 0.90403(11) 0.61539(13) 0.47600(10) 0.0299(4) Uani 1 1 d . . . O1 O 0.85229(11) 0.63098(12) 0.36216(9) 0.0267(4) Uani 1 1 d . . . C1 C 0.68077(16) 0.73018(16) 0.34108(14) 0.0229(5) Uani 1 1 d . . . C2 C 0.59029(18) 0.76303(19) 0.22570(16) 0.0330(6) Uani 1 1 d . . . C3 C 0.5638(2) 0.7779(3) 0.15357(18) 0.0468(8) Uani 1 1 d . . . H3 H 0.6024 0.7822 0.1301 0.056 Uiso 1 1 calc R . . C4 C 0.4784(2) 0.7863(3) 0.1177(2) 0.0587(10) Uani 1 1 d . . . H4 H 0.4593 0.7968 0.0690 0.070 Uiso 1 1 calc R . . C5 C 0.4205(2) 0.7798(3) 0.1502(2) 0.0587(11) Uani 1 1 d . . . H5 H 0.3631 0.7852 0.1237 0.070 Uiso 1 1 calc R . . C6 C 0.4459(2) 0.7656(2) 0.2213(2) 0.0471(9) Uani 1 1 d . . . H6 H 0.4066 0.7611 0.2442 0.057 Uiso 1 1 calc R . . C7 C 0.53169(18) 0.75790(19) 0.25870(17) 0.0344(7) Uani 1 1 d . . . C8 C 0.74685(18) 0.76018(19) 0.25224(15) 0.0306(6) Uani 1 1 d . . . H8 H 0.7964 0.7554 0.2959 0.037 Uiso 1 1 calc R . . C9 C 0.7547(2) 0.6853(2) 0.20483(16) 0.0419(8) Uani 1 1 d . . . H9A H 0.7607 0.6289 0.2295 0.063 Uiso 1 1 calc R . . H9B H 0.8036 0.6954 0.1918 0.063 Uiso 1 1 calc R . . H9C H 0.7049 0.6836 0.1628 0.063 Uiso 1 1 calc R . . C10 C 0.7508(2) 0.8531(2) 0.22235(17) 0.0431(8) Uani 1 1 d . . . H10A H 0.7139 0.8553 0.1736 0.065 Uiso 1 1 calc R . . H10B H 0.8079 0.8656 0.2254 0.065 Uiso 1 1 calc R . . H10C H 0.7331 0.8972 0.2491 0.065 Uiso 1 1 calc R . . C11 C 0.90998(17) 0.60198(19) 0.41648(15) 0.0296(6) Uani 1 1 d . . . C12 C 0.9830(2) 0.5532(3) 0.40865(19) 0.0486(9) Uani 1 1 d . . . H12A H 1.0248 0.5958 0.4064 0.073 Uiso 1 1 calc R . . H12B H 0.9641 0.5181 0.3658 0.073 Uiso 1 1 calc R . . H12C H 1.0074 0.5140 0.4487 0.073 Uiso 1 1 calc R . . C1A C 0.75692(17) 0.46076(18) 0.37599(15) 0.0269(5) Uani 1 1 d . . . C2A C 0.80534(19) 0.3872(2) 0.40727(17) 0.0356(6) Uani 1 1 d . . . H2A H 0.8198 0.3777 0.4558 0.043 Uiso 1 1 calc R . . C3A C 0.8325(2) 0.3276(2) 0.3676(2) 0.0486(8) Uani 1 1 d . . . H3A H 0.8660 0.2787 0.3894 0.058 Uiso 1 1 calc R . . C4A C 0.8105(3) 0.3400(3) 0.2957(2) 0.0536(9) Uani 1 1 d . . . H4A H 0.8276 0.2987 0.2687 0.064 Uiso 1 1 calc R . . C5A C 0.7632(2) 0.4133(2) 0.26404(18) 0.0476(8) Uani 1 1 d . . . H5A H 0.7482 0.4220 0.2154 0.057 Uiso 1 1 calc R . . C6A C 0.7380(2) 0.4738(2) 0.30398(16) 0.0355(7) Uani 1 1 d . . . H6A H 0.7076 0.5246 0.2823 0.043 Uiso 1 1 calc R . . C1B C 0.60776(16) 0.53166(18) 0.39501(15) 0.0271(6) Uani 1 1 d . . . C2B C 0.56003(19) 0.5046(2) 0.32753(16) 0.0379(7) Uani 1 1 d . . . H2B H 0.5869 0.4860 0.2966 0.046 Uiso 1 1 calc R . . C3B C 0.4731(2) 0.5048(3) 0.30504(19) 0.0505(9) Uani 1 1 d . . . H3B H 0.4416 0.4872 0.2589 0.061 Uiso 1 1 calc R . . C4B C 0.4329(2) 0.5306(2) 0.3499(2) 0.0474(8) Uani 1 1 d . . . H4B H 0.3740 0.5309 0.3344 0.057 Uiso 1 1 calc R . . C5B C 0.47907(19) 0.5561(2) 0.41757(19) 0.0407(7) Uani 1 1 d . . . H5B H 0.4516 0.5733 0.4484 0.049 Uiso 1 1 calc R . . C6B C 0.56605(18) 0.55653(19) 0.44040(16) 0.0328(6) Uani 1 1 d . . . H6B H 0.5972 0.5736 0.4867 0.039 Uiso 1 1 calc R . . C1C C 0.75400(17) 0.49700(18) 0.51382(14) 0.0269(5) Uani 1 1 d . . . C2C C 0.71425(19) 0.4203(2) 0.52553(17) 0.0355(7) Uani 1 1 d . . . H2C H 0.6713 0.3938 0.4880 0.043 Uiso 1 1 calc R . . C3C C 0.7375(2) 0.3829(2) 0.59204(18) 0.0438(8) Uani 1 1 d . . . H3C H 0.7099 0.3317 0.5995 0.053 Uiso 1 1 calc R . . C4C C 0.8013(2) 0.4208(2) 0.64722(17) 0.0440(8) Uani 1 1 d . . . H4C H 0.8173 0.3953 0.6923 0.053 Uiso 1 1 calc R . . C5C C 0.8412(2) 0.4959(2) 0.63617(16) 0.0383(7) Uani 1 1 d . . . H5C H 0.8849 0.5214 0.6738 0.046 Uiso 1 1 calc R . . C6C C 0.81766(18) 0.5343(2) 0.57015(15) 0.0310(6) Uani 1 1 d . . . H6C H 0.8450 0.5860 0.5634 0.037 Uiso 1 1 calc R . . C1D C 0.82264(17) 0.92506(18) 0.40194(13) 0.0266(5) Uani 1 1 d . . . C2D C 0.74040(18) 0.9463(2) 0.39424(16) 0.0331(6) Uani 1 1 d . . . H2D H 0.7079 0.9058 0.4091 0.040 Uiso 1 1 calc R . . C3D C 0.7062(2) 1.0271(2) 0.36472(17) 0.0398(7) Uani 1 1 d . . . H3D H 0.6509 1.0415 0.3604 0.048 Uiso 1 1 calc R . . C4D C 0.7528(2) 1.0866(2) 0.34163(18) 0.0429(8) Uani 1 1 d . . . H4D H 0.7289 1.1409 0.3210 0.052 Uiso 1 1 calc R . . C5D C 0.8344(2) 1.0661(2) 0.34894(16) 0.0387(7) Uani 1 1 d . . . H5D H 0.8662 1.1065 0.3333 0.046 Uiso 1 1 calc R . . C6D C 0.86984(18) 0.98574(19) 0.37933(15) 0.0314(6) Uani 1 1 d . . . H6D H 0.9257 0.9724 0.3846 0.038 Uiso 1 1 calc R . . C1E C 0.96652(16) 0.81210(18) 0.42778(14) 0.0259(5) Uani 1 1 d . . . C2E C 0.9694(2) 0.7871(3) 0.36318(17) 0.0431(8) Uani 1 1 d . . . H2E H 0.9193 0.7728 0.3265 0.052 Uiso 1 1 calc R . . C3E C 1.0449(2) 0.7829(3) 0.35165(19) 0.0513(9) Uani 1 1 d . . . H3E H 1.0452 0.7665 0.3071 0.062 Uiso 1 1 calc R . . C4E C 1.1190(2) 0.8023(2) 0.40429(19) 0.0424(8) Uani 1 1 d . . . H4E H 1.1701 0.7988 0.3963 0.051 Uiso 1 1 calc R . . C5E C 1.11779(19) 0.8268(2) 0.46881(18) 0.0438(8) Uani 1 1 d . . . H5E H 1.1683 0.8402 0.5053 0.053 Uiso 1 1 calc R . . C6E C 1.04236(18) 0.8319(2) 0.48062(16) 0.0358(7) Uani 1 1 d . . . H6E H 1.0426 0.8491 0.5251 0.043 Uiso 1 1 calc R . . C1F C 0.90338(16) 0.84471(19) 0.53734(14) 0.0269(6) Uani 1 1 d . . . C2F C 0.89534(19) 0.9286(2) 0.56322(16) 0.0352(6) Uani 1 1 d . . . H2F H 0.8713 0.9755 0.5319 0.042 Uiso 1 1 calc R . . C3F C 0.9228(2) 0.9436(3) 0.63546(18) 0.0477(8) Uani 1 1 d . . . H3F H 0.9164 1.0003 0.6526 0.057 Uiso 1 1 calc R . . C4F C 0.9593(2) 0.8758(3) 0.68185(17) 0.0500(9) Uani 1 1 d . . . H4F H 0.9779 0.8860 0.7305 0.060 Uiso 1 1 calc R . . C5F C 0.9683(2) 0.7929(3) 0.65630(16) 0.0446(8) Uani 1 1 d . . . H5F H 0.9938 0.7467 0.6879 0.054 Uiso 1 1 calc R . . C6F C 0.94046(19) 0.7767(2) 0.58480(16) 0.0358(7) Uani 1 1 d . . . H6F H 0.9466 0.7196 0.5681 0.043 Uiso 1 1 calc R . . C1S C 0.4282(3) 0.9748(3) 0.4074(2) 0.0655(12) Uani 1 1 d . . . C2S C 0.3634(4) 1.0015(3) 0.4304(3) 0.0909(19) Uani 1 1 d . . . H2S H 0.3466 1.0615 0.4278 0.109 Uiso 1 1 calc R . . C3S C 0.3227(3) 0.9333(4) 0.4588(3) 0.0775(14) Uani 1 1 d . . . H3S H 0.2783 0.9468 0.4746 0.093 Uiso 1 1 calc R . . C4S C 0.3524(4) 0.8507(4) 0.4609(3) 0.0861(16) Uani 1 1 d . . . H4S H 0.3289 0.8049 0.4796 0.103 Uiso 1 1 calc R . . C5S C 0.4127(5) 0.8307(5) 0.4381(4) 0.111(2) Uani 1 1 d . . . H5S H 0.4300 0.7710 0.4398 0.133 Uiso 1 1 calc R . . C6S C 0.4488(4) 0.8888(4) 0.4137(3) 0.0921(17) Uani 1 1 d . . . H6S H 0.4928 0.8702 0.3991 0.111 Uiso 1 1 calc R . . C7S C 0.4740(5) 1.0374(6) 0.3780(4) 0.168(4) Uani 1 1 d . . . H7S1 H 0.5158 1.0050 0.3651 0.253 Uiso 1 1 calc R . . H7S2 H 0.5015 1.0822 0.4129 0.253 Uiso 1 1 calc R . . H7S3 H 0.4350 1.0661 0.3367 0.253 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 0.01928(10) 0.02158(10) 0.01811(10) 0.00131(7) 0.00682(8) 0.00118(7) I1 0.03477(10) 0.03363(11) 0.02877(10) -0.00555(7) 0.01793(8) -0.00244(7) S1 0.0227(3) 0.0348(4) 0.0377(4) 0.0086(3) 0.0123(3) 0.0060(3) P1 0.0233(3) 0.0229(3) 0.0220(3) 0.0019(3) 0.0084(3) 0.0005(3) P2 0.0217(3) 0.0254(3) 0.0207(3) 0.0009(3) 0.0059(3) -0.0016(3) N1 0.0233(11) 0.0316(12) 0.0223(11) 0.0016(9) 0.0047(9) 0.0008(9) O2 0.0278(9) 0.0374(11) 0.0234(10) 0.0065(8) 0.0074(8) 0.0066(8) O1 0.0242(9) 0.0315(10) 0.0249(9) 0.0016(8) 0.0095(8) 0.0047(8) C1 0.0233(12) 0.0197(12) 0.0264(13) 0.0014(10) 0.0097(10) 0.0008(10) C2 0.0275(14) 0.0310(15) 0.0348(16) 0.0074(12) 0.0037(12) 0.0049(11) C3 0.0410(18) 0.057(2) 0.0324(17) 0.0091(16) 0.0000(14) 0.0040(16) C4 0.042(2) 0.074(3) 0.041(2) 0.0139(19) -0.0104(16) 0.0055(19) C5 0.0299(17) 0.063(2) 0.062(3) 0.015(2) -0.0106(17) 0.0033(16) C6 0.0247(15) 0.0458(19) 0.062(2) 0.0137(17) 0.0041(15) 0.0042(13) C7 0.0248(14) 0.0330(15) 0.0402(17) 0.0070(13) 0.0049(12) 0.0029(11) C8 0.0255(13) 0.0413(16) 0.0240(14) 0.0092(12) 0.0073(11) 0.0010(11) C9 0.0495(19) 0.053(2) 0.0291(16) 0.0113(14) 0.0206(14) 0.0145(16) C10 0.0451(18) 0.050(2) 0.0318(16) 0.0097(14) 0.0104(14) -0.0101(15) C11 0.0259(13) 0.0315(14) 0.0335(15) 0.0045(12) 0.0130(12) 0.0030(11) C12 0.0414(18) 0.064(2) 0.046(2) 0.0151(17) 0.0225(16) 0.0270(17) C1A 0.0277(13) 0.0242(13) 0.0298(14) -0.0009(11) 0.0114(11) -0.0013(10) C2A 0.0388(16) 0.0314(15) 0.0363(16) 0.0009(13) 0.0127(13) 0.0055(13) C3A 0.055(2) 0.0357(18) 0.056(2) -0.0017(16) 0.0212(18) 0.0148(15) C4A 0.067(2) 0.047(2) 0.054(2) -0.0145(17) 0.0297(19) 0.0084(18) C5A 0.060(2) 0.055(2) 0.0327(17) -0.0068(15) 0.0216(16) 0.0023(17) C6A 0.0417(16) 0.0337(16) 0.0326(16) 0.0021(12) 0.0149(13) 0.0036(13) C1B 0.0259(13) 0.0241(13) 0.0305(14) 0.0045(11) 0.0089(11) 0.0003(10) C2B 0.0316(15) 0.0466(18) 0.0328(16) 0.0001(14) 0.0079(13) 0.0005(13) C3B 0.0331(16) 0.066(2) 0.0407(19) -0.0009(17) -0.0014(14) -0.0014(16) C4B 0.0236(14) 0.054(2) 0.060(2) 0.0044(17) 0.0095(15) -0.0002(14) C5B 0.0317(15) 0.0435(18) 0.053(2) 0.0074(15) 0.0231(15) -0.0002(13) C6B 0.0333(15) 0.0323(15) 0.0356(16) 0.0027(12) 0.0158(13) -0.0029(12) C1C 0.0290(13) 0.0290(14) 0.0261(13) 0.0033(11) 0.0139(11) 0.0053(11) C2C 0.0397(16) 0.0311(15) 0.0374(17) 0.0053(13) 0.0158(13) 0.0025(12) C3C 0.054(2) 0.0385(17) 0.047(2) 0.0191(15) 0.0278(17) 0.0088(15) C4C 0.056(2) 0.051(2) 0.0307(17) 0.0149(15) 0.0220(15) 0.0193(16) C5C 0.0409(17) 0.0499(19) 0.0245(14) 0.0022(13) 0.0119(13) 0.0126(14) C6C 0.0320(14) 0.0351(15) 0.0267(14) 0.0012(12) 0.0112(12) 0.0033(12) C1D 0.0291(13) 0.0269(13) 0.0185(12) -0.0007(10) 0.0019(10) 0.0004(11) C2D 0.0297(14) 0.0331(15) 0.0338(16) 0.0009(12) 0.0075(12) -0.0019(12) C3D 0.0322(15) 0.0385(17) 0.0419(18) -0.0013(14) 0.0044(13) 0.0050(13) C4D 0.0487(19) 0.0310(16) 0.0390(18) 0.0048(13) 0.0026(15) 0.0036(14) C5D 0.0474(18) 0.0328(16) 0.0316(16) 0.0053(13) 0.0084(14) -0.0082(14) C6D 0.0306(14) 0.0320(15) 0.0283(15) 0.0040(12) 0.0061(12) -0.0053(12) C1E 0.0239(12) 0.0265(13) 0.0269(13) 0.0017(11) 0.0084(11) -0.0012(10) C2E 0.0295(15) 0.070(2) 0.0293(16) -0.0094(15) 0.0093(13) -0.0136(15) C3E 0.0405(18) 0.079(3) 0.0412(19) -0.0192(18) 0.0228(16) -0.0152(18) C4E 0.0304(15) 0.050(2) 0.051(2) -0.0055(16) 0.0193(14) -0.0023(14) C5E 0.0252(14) 0.064(2) 0.0378(18) -0.0015(16) 0.0059(13) -0.0025(14) C6E 0.0291(14) 0.0485(18) 0.0270(15) -0.0011(13) 0.0063(12) -0.0018(13) C1F 0.0229(12) 0.0347(15) 0.0230(13) -0.0028(11) 0.0082(10) -0.0053(11) C2F 0.0377(16) 0.0375(16) 0.0299(15) -0.0027(12) 0.0111(13) -0.0012(13) C3F 0.053(2) 0.053(2) 0.0379(18) -0.0174(16) 0.0163(16) -0.0073(17) C4F 0.050(2) 0.074(3) 0.0240(16) -0.0092(16) 0.0103(14) -0.0145(18) C5F 0.0468(19) 0.056(2) 0.0256(16) 0.0058(15) 0.0059(14) -0.0072(16) C6F 0.0392(16) 0.0382(16) 0.0273(15) 0.0001(13) 0.0083(13) -0.0034(13) C1S 0.058(2) 0.079(3) 0.055(2) -0.009(2) 0.015(2) -0.026(2) C2S 0.109(4) 0.063(3) 0.067(3) -0.022(2) -0.012(3) 0.034(3) C3S 0.057(3) 0.116(4) 0.065(3) -0.006(3) 0.028(2) 0.006(3) C4S 0.073(3) 0.080(4) 0.093(4) 0.013(3) 0.014(3) -0.010(3) C5S 0.095(5) 0.090(5) 0.137(6) -0.017(4) 0.028(4) 0.003(4) C6S 0.072(3) 0.086(4) 0.113(5) -0.025(4) 0.026(3) 0.015(3) C7S 0.150(7) 0.245(10) 0.097(5) 0.010(6) 0.027(5) -0.122(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.981(3) . ? Ru1 O1 2.1283(18) . ? Ru1 O2 2.2829(18) . ? Ru1 P1 2.3741(7) . ? Ru1 P2 2.3898(7) . ? Ru1 I1 2.7221(3) . ? S1 C7 1.736(3) . ? S1 C1 1.748(3) . ? P1 C1B 1.835(3) . ? P1 C1A 1.838(3) . ? P1 C1C 1.841(3) . ? P2 C1D 1.835(3) . ? P2 C1F 1.837(3) . ? P2 C1E 1.846(3) . ? N1 C1 1.367(3) . ? N1 C2 1.407(4) . ? N1 C8 1.481(4) . ? O2 C11 1.265(3) . ? O1 C11 1.270(3) . ? C2 C7 1.386(4) . ? C2 C3 1.392(4) . ? C3 C4 1.385(5) . ? C4 C5 1.369(6) . ? C5 C6 1.372(6) . ? C6 C7 1.395(4) . ? C8 C9 1.516(4) . ? C8 C10 1.531(4) . ? C11 C12 1.499(4) . ? C1A C2A 1.391(4) . ? C1A C6A 1.398(4) . ? C2A C3A 1.388(4) . ? C3A C4A 1.386(5) . ? C4A C5A 1.381(5) . ? C5A C6A 1.382(4) . ? C1B C2B 1.387(4) . ? C1B C6B 1.398(4) . ? C2B C3B 1.387(4) . ? C3B C4B 1.373(5) . ? C4B C5B 1.378(5) . ? C5B C6B 1.388(4) . ? C1C C6C 1.388(4) . ? C1C C2C 1.397(4) . ? C2C C3C 1.387(4) . ? C3C C4C 1.380(5) . ? C4C C5C 1.375(5) . ? C5C C6C 1.384(4) . ? C1D C2D 1.390(4) . ? C1D C6D 1.394(4) . ? C2D C3D 1.387(4) . ? C3D C4D 1.380(5) . ? C4D C5D 1.380(5) . ? C5D C6D 1.391(4) . ? C1E C2E 1.383(4) . ? C1E C6E 1.391(4) . ? C2E C3E 1.387(4) . ? C3E C4E 1.369(5) . ? C4E C5E 1.369(5) . ? C5E C6E 1.389(4) . ? C1F C2F 1.390(4) . ? C1F C6F 1.393(4) . ? C2F C3F 1.394(4) . ? C3F C4F 1.378(5) . ? C4F C5F 1.376(5) . ? C5F C6F 1.383(4) . ? C1S C6S 1.331(7) . ? C1S C2S 1.399(7) . ? C1S C7S 1.475(7) . ? C2S C3S 1.464(8) . ? C3S C4S 1.334(7) . ? C4S C5S 1.300(8) . ? C5S C6S 1.264(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 O1 100.89(9) . . ? C1 Ru1 O2 159.66(9) . . ? O1 Ru1 O2 59.12(7) . . ? C1 Ru1 P1 94.16(7) . . ? O1 Ru1 P1 90.15(5) . . ? O2 Ru1 P1 83.00(5) . . ? C1 Ru1 P2 100.77(7) . . ? O1 Ru1 P2 90.88(5) . . ? O2 Ru1 P2 84.32(5) . . ? P1 Ru1 P2 164.55(2) . . ? C1 Ru1 I1 89.73(7) . . ? O1 Ru1 I1 169.31(5) . . ? O2 Ru1 I1 110.21(5) . . ? P1 Ru1 I1 87.781(17) . . ? P2 Ru1 I1 88.360(18) . . ? C7 S1 C1 93.47(14) . . ? C1B P1 C1A 104.37(13) . . ? C1B P1 C1C 101.35(12) . . ? C1A P1 C1C 102.60(12) . . ? C1B P1 Ru1 120.01(9) . . ? C1A P1 Ru1 111.71(9) . . ? C1C P1 Ru1 114.80(9) . . ? C1D P2 C1F 103.01(12) . . ? C1D P2 C1E 102.52(12) . . ? C1F P2 C1E 100.60(12) . . ? C1D P2 Ru1 120.35(9) . . ? C1F P2 Ru1 110.64(9) . . ? C1E P2 Ru1 117.13(9) . . ? C1 N1 C2 116.7(2) . . ? C1 N1 C8 121.1(2) . . ? C2 N1 C8 122.2(2) . . ? C11 O2 Ru1 87.63(15) . . ? C11 O1 Ru1 94.57(16) . . ? N1 C1 S1 107.67(18) . . ? N1 C1 Ru1 129.30(19) . . ? S1 C1 Ru1 122.75(14) . . ? C7 C2 C3 119.7(3) . . ? C7 C2 N1 111.7(3) . . ? C3 C2 N1 128.5(3) . . ? C4 C3 C2 117.5(4) . . ? C5 C4 C3 122.7(4) . . ? C4 C5 C6 120.4(3) . . ? C5 C6 C7 118.0(3) . . ? C2 C7 C6 121.8(3) . . ? C2 C7 S1 110.1(2) . . ? C6 C7 S1 128.1(3) . . ? N1 C8 C9 112.6(2) . . ? N1 C8 C10 111.6(2) . . ? C9 C8 C10 113.4(2) . . ? O2 C11 O1 118.7(2) . . ? O2 C11 C12 121.8(3) . . ? O1 C11 C12 119.5(3) . . ? C2A C1A C6A 118.1(3) . . ? C2A C1A P1 123.6(2) . . ? C6A C1A P1 118.2(2) . . ? C3A C2A C1A 120.7(3) . . ? C4A C3A C2A 120.2(3) . . ? C5A C4A C3A 119.8(3) . . ? C4A C5A C6A 119.9(3) . . ? C5A C6A C1A 121.2(3) . . ? C2B C1B C6B 118.3(3) . . ? C2B C1B P1 123.2(2) . . ? C6B C1B P1 118.3(2) . . ? C3B C2B C1B 120.8(3) . . ? C4B C3B C2B 120.3(3) . . ? C3B C4B C5B 119.9(3) . . ? C4B C5B C6B 120.2(3) . . ? C5B C6B C1B 120.5(3) . . ? C6C C1C C2C 118.4(3) . . ? C6C C1C P1 121.7(2) . . ? C2C C1C P1 119.8(2) . . ? C3C C2C C1C 120.6(3) . . ? C4C C3C C2C 120.0(3) . . ? C5C C4C C3C 119.9(3) . . ? C4C C5C C6C 120.5(3) . . ? C5C C6C C1C 120.6(3) . . ? C2D C1D C6D 119.2(3) . . ? C2D C1D P2 118.6(2) . . ? C6D C1D P2 122.2(2) . . ? C3D C2D C1D 120.2(3) . . ? C4D C3D C2D 120.5(3) . . ? C5D C4D C3D 119.7(3) . . ? C4D C5D C6D 120.3(3) . . ? C5D C6D C1D 120.1(3) . . ? C2E C1E C6E 117.3(3) . . ? C2E C1E P2 121.2(2) . . ? C6E C1E P2 121.6(2) . . ? C1E C2E C3E 121.1(3) . . ? C4E C3E C2E 120.9(3) . . ? C5E C4E C3E 119.1(3) . . ? C4E C5E C6E 120.4(3) . . ? C5E C6E C1E 121.2(3) . . ? C2F C1F C6F 118.8(3) . . ? C2F C1F P2 123.0(2) . . ? C6F C1F P2 118.2(2) . . ? C1F C2F C3F 120.2(3) . . ? C4F C3F C2F 120.4(3) . . ? C5F C4F C3F 119.5(3) . . ? C4F C5F C6F 120.8(3) . . ? C5F C6F C1F 120.3(3) . . ? C6S C1S C2S 117.2(5) . . ? C6S C1S C7S 119.7(6) . . ? C2S C1S C7S 123.1(6) . . ? C1S C2S C3S 118.1(4) . . ? C4S C3S C2S 115.8(5) . . ? C5S C4S C3S 122.8(6) . . ? C6S C5S C4S 122.3(7) . . ? C5S C6S C1S 123.9(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.798 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.083 data_7 _database_code_depnum_ccdc_archive 'CCDC 778719' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H61 I N O2 P2 Ru S' _chemical_formula_weight 1186.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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' I I -0.4742 1.8119 '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 10.7883(5) _cell_length_b 13.8789(7) _cell_length_c 18.6293(9) _cell_angle_alpha 90.8480(10) _cell_angle_beta 94.2400(10) _cell_angle_gamma 96.8600(10) _cell_volume 2761.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6910 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.47 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1210 _exptl_absorpt_coefficient_mu 0.983 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6945 _exptl_absorpt_correction_T_max 0.9081 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35988 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12643 _reflns_number_gt 11067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.6275P] 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 12643 _refine_ls_number_parameters 645 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.009224(17) 0.295510(13) 0.273800(10) 0.02345(6) Uani 1 1 d . . . I1 I -0.189051(15) 0.378952(12) 0.319780(9) 0.03476(6) Uani 1 1 d . . . P1 P 0.00020(6) 0.38459(4) 0.16560(3) 0.02748(13) Uani 1 1 d . . . P2 P -0.00260(6) 0.18652(4) 0.37220(3) 0.02552(13) Uani 1 1 d . . . O1 O 0.11338(16) 0.19675(13) 0.22054(9) 0.0327(4) Uani 1 1 d . . . O2 O -0.09001(16) 0.17027(12) 0.20662(9) 0.0336(4) Uani 1 1 d . . . S1 S 0.08170(7) 0.49502(5) 0.37157(4) 0.04001(16) Uani 1 1 d . . . N1 N 0.2593(2) 0.40730(15) 0.33589(11) 0.0327(5) Uani 1 1 d . . . C1 C 0.1324(2) 0.39642(18) 0.32644(12) 0.0284(5) Uani 1 1 d . . . C2 C 0.3178(2) 0.4887(2) 0.37768(14) 0.0372(6) Uani 1 1 d . . . C3 C 0.4460(3) 0.5153(2) 0.39704(17) 0.0508(8) Uani 1 1 d . . . H3 H 0.5071 0.4784 0.3817 0.061 Uiso 1 1 calc R . . C4 C 0.4782(3) 0.5987(3) 0.43988(19) 0.0589(9) Uani 1 1 d . . . H4 H 0.5633 0.6175 0.4539 0.071 Uiso 1 1 calc R . . C5 C 0.3915(3) 0.6550(3) 0.46269(19) 0.0606(9) Uani 1 1 d . . . H5 H 0.4179 0.7114 0.4910 0.073 Uiso 1 1 calc R . . C6 C 0.2665(3) 0.6289(2) 0.44412(19) 0.0573(9) Uani 1 1 d . . . H6 H 0.2062 0.6666 0.4596 0.069 Uiso 1 1 calc R . . C7 C 0.2309(3) 0.5450(2) 0.40156(15) 0.0410(6) Uani 1 1 d . . . C8 C 0.3336(2) 0.3383(2) 0.30291(15) 0.0386(6) Uani 1 1 d . . . H8 H 0.2735 0.2892 0.2756 0.046 Uiso 1 1 calc R . . C9 C 0.4184(3) 0.3881(2) 0.24846(17) 0.0511(8) Uani 1 1 d . . . H9A H 0.3725 0.4317 0.2197 0.077 Uiso 1 1 calc R . . H9B H 0.4454 0.3393 0.2173 0.077 Uiso 1 1 calc R . . H9C H 0.4911 0.4247 0.2739 0.077 Uiso 1 1 calc R . . C10 C 0.4065(3) 0.2840(2) 0.35939(19) 0.0519(8) Uani 1 1 d . . . H10A H 0.4806 0.3257 0.3784 0.078 Uiso 1 1 calc R . . H10B H 0.4312 0.2261 0.3374 0.078 Uiso 1 1 calc R . . H10C H 0.3540 0.2657 0.3982 0.078 Uiso 1 1 calc R . . C11 C 0.0155(3) 0.14647(19) 0.19295(14) 0.0355(6) Uani 1 1 d . . . C12 C 0.0284(4) 0.0614(3) 0.1445(2) 0.0676(11) Uani 1 1 d . . . H12 H 0.1037 0.0337 0.1443 0.081 Uiso 1 1 calc R . . C13 C -0.0791(5) 0.0250(4) 0.0989(3) 0.121(2) Uani 1 1 d . . . H13A H -0.1436 -0.0049 0.1279 0.182 Uiso 1 1 calc R . . H13B H -0.0568 -0.0229 0.0653 0.182 Uiso 1 1 calc R . . H13C H -0.1103 0.0780 0.0725 0.182 Uiso 1 1 calc R . . C1A C 0.0785(2) 0.50940(18) 0.16815(14) 0.0341(6) Uani 1 1 d . . . C2A C 0.0313(3) 0.5765(2) 0.21123(16) 0.0442(7) Uani 1 1 d . . . H2A H -0.0383 0.5571 0.2374 0.053 Uiso 1 1 calc R . . C3A C 0.0862(3) 0.6720(2) 0.21581(18) 0.0556(9) Uani 1 1 d . . . H3A H 0.0537 0.7172 0.2451 0.067 Uiso 1 1 calc R . . C4A C 0.1883(3) 0.7012(2) 0.17769(19) 0.0579(9) Uani 1 1 d . . . H4A H 0.2257 0.7660 0.1812 0.070 Uiso 1 1 calc R . . C5A C 0.2346(3) 0.6360(2) 0.1350(2) 0.0592(9) Uani 1 1 d . . . H5A H 0.3038 0.6562 0.1088 0.071 Uiso 1 1 calc R . . C6A C 0.1807(3) 0.5393(2) 0.12969(17) 0.0471(7) Uani 1 1 d . . . H6A H 0.2137 0.4947 0.1002 0.056 Uiso 1 1 calc R . . C1B C 0.0686(2) 0.32761(18) 0.09039(13) 0.0311(5) Uani 1 1 d . . . C2B C 0.1911(3) 0.3056(2) 0.10027(14) 0.0377(6) Uani 1 1 d . . . H2B H 0.2369 0.3207 0.1447 0.045 Uiso 1 1 calc R . . C3B C 0.2468(3) 0.2615(2) 0.04555(16) 0.0443(7) Uani 1 1 d . . . H3B H 0.3298 0.2475 0.0531 0.053 Uiso 1 1 calc R . . C4B C 0.1809(3) 0.2385(2) -0.01956(16) 0.0495(8) Uani 1 1 d . . . H4B H 0.2184 0.2092 -0.0568 0.059 Uiso 1 1 calc R . . C5B C 0.0593(3) 0.2587(2) -0.02954(16) 0.0536(8) Uani 1 1 d . . . H5B H 0.0136 0.2419 -0.0738 0.064 Uiso 1 1 calc R . . C6B C 0.0027(3) 0.3033(2) 0.02414(15) 0.0410(6) Uani 1 1 d . . . H6B H -0.0803 0.3173 0.0159 0.049 Uiso 1 1 calc R . . C1C C -0.1552(2) 0.39991(18) 0.12403(13) 0.0302(5) Uani 1 1 d . . . C2C C -0.2537(3) 0.3265(2) 0.12920(15) 0.0389(6) Uani 1 1 d . . . H2C H -0.2411 0.2718 0.1567 0.047 Uiso 1 1 calc R . . C3C C -0.3698(3) 0.3332(2) 0.09428(16) 0.0445(7) Uani 1 1 d . . . H3C H -0.4351 0.2825 0.0971 0.053 Uiso 1 1 calc R . . C4C C -0.3901(3) 0.4143(2) 0.05525(17) 0.0481(7) Uani 1 1 d . . . H4C H -0.4696 0.4196 0.0325 0.058 Uiso 1 1 calc R . . C5C C -0.2942(3) 0.4871(2) 0.04979(17) 0.0474(7) Uani 1 1 d . . . H5C H -0.3082 0.5421 0.0230 0.057 Uiso 1 1 calc R . . C6C C -0.1766(3) 0.48065(19) 0.08327(15) 0.0378(6) Uani 1 1 d . . . H6C H -0.1112 0.5308 0.0785 0.045 Uiso 1 1 calc R . . C1D C 0.0558(2) 0.06964(17) 0.35382(13) 0.0285(5) Uani 1 1 d . . . C2D C 0.1779(2) 0.07099(18) 0.33458(14) 0.0336(5) Uani 1 1 d . . . H2D H 0.2272 0.1308 0.3298 0.040 Uiso 1 1 calc R . . C3D C 0.2282(3) -0.0146(2) 0.32232(15) 0.0387(6) Uani 1 1 d . . . H3D H 0.3112 -0.0126 0.3097 0.046 Uiso 1 1 calc R . . C4D C 0.1561(3) -0.1027(2) 0.32858(16) 0.0414(6) Uani 1 1 d . . . H4D H 0.1900 -0.1609 0.3204 0.050 Uiso 1 1 calc R . . C5D C 0.0348(3) -0.1051(2) 0.34687(17) 0.0440(7) Uani 1 1 d . . . H5D H -0.0144 -0.1652 0.3508 0.053 Uiso 1 1 calc R . . C6D C -0.0160(3) -0.01965(19) 0.35965(15) 0.0364(6) Uani 1 1 d . . . H6D H -0.0991 -0.0222 0.3723 0.044 Uiso 1 1 calc R . . C1E C 0.0829(2) 0.22472(18) 0.45844(13) 0.0286(5) Uani 1 1 d . . . C2E C 0.1686(2) 0.1718(2) 0.49419(14) 0.0376(6) Uani 1 1 d . . . H2E H 0.1840 0.1120 0.4746 0.045 Uiso 1 1 calc R . . C3E C 0.2320(3) 0.2066(2) 0.55882(15) 0.0447(7) Uani 1 1 d . . . H3E H 0.2895 0.1698 0.5825 0.054 Uiso 1 1 calc R . . C4E C 0.2118(3) 0.2933(2) 0.58832(16) 0.0459(7) Uani 1 1 d . . . H4E H 0.2554 0.3163 0.6320 0.055 Uiso 1 1 calc R . . C5E C 0.1266(3) 0.3473(2) 0.55351(16) 0.0446(7) Uani 1 1 d . . . H5E H 0.1128 0.4075 0.5732 0.053 Uiso 1 1 calc R . . C6E C 0.0615(3) 0.3123(2) 0.48933(14) 0.0371(6) Uani 1 1 d . . . H6E H 0.0023 0.3485 0.4666 0.044 Uiso 1 1 calc R . . C1F C -0.1606(2) 0.14452(17) 0.39808(14) 0.0295(5) Uani 1 1 d . . . C2F C -0.1865(3) 0.1301(2) 0.46934(14) 0.0380(6) Uani 1 1 d . . . H2F H -0.1226 0.1442 0.5064 0.046 Uiso 1 1 calc R . . C3F C -0.3069(3) 0.0948(2) 0.48606(16) 0.0500(8) Uani 1 1 d . . . H3F H -0.3243 0.0859 0.5344 0.060 Uiso 1 1 calc R . . C4F C -0.4003(3) 0.0729(2) 0.43215(18) 0.0496(8) Uani 1 1 d . . . H4F H -0.4816 0.0492 0.4436 0.060 Uiso 1 1 calc R . . C5F C -0.3752(3) 0.0856(2) 0.36155(16) 0.0423(7) Uani 1 1 d . . . H5F H -0.4390 0.0695 0.3247 0.051 Uiso 1 1 calc R . . C6F C -0.2564(2) 0.1219(2) 0.34430(15) 0.0367(6) Uani 1 1 d . . . H6F H -0.2404 0.1314 0.2958 0.044 Uiso 1 1 calc R . . C1S C 0.5636(3) 0.7742(3) 0.26415(18) 0.0531(8) Uani 1 1 d . . . C2S C 0.5426(3) 0.6773(3) 0.2447(2) 0.0597(9) Uani 1 1 d . . . H2S H 0.4668 0.6410 0.2546 0.072 Uiso 1 1 calc R . . C3S C 0.6305(4) 0.6325(3) 0.2110(2) 0.0657(10) Uani 1 1 d . . . H3S H 0.6147 0.5662 0.1980 0.079 Uiso 1 1 calc R . . C4S C 0.7405(4) 0.6852(3) 0.1966(2) 0.0649(10) Uani 1 1 d . . . H4S H 0.8002 0.6550 0.1731 0.078 Uiso 1 1 calc R . . C5S C 0.7652(4) 0.7818(3) 0.21610(19) 0.0645(10) Uani 1 1 d . . . H5S H 0.8417 0.8175 0.2067 0.077 Uiso 1 1 calc R . . C6S C 0.6765(4) 0.8259(3) 0.24957(18) 0.0576(9) Uani 1 1 d . . . H6S H 0.6929 0.8921 0.2627 0.069 Uiso 1 1 calc R . . C7S C 0.4678(4) 0.8222(3) 0.2999(3) 0.0876(14) Uani 1 1 d . . . H7S1 H 0.4218 0.8578 0.2647 0.131 Uiso 1 1 calc R . . H7S2 H 0.5087 0.8667 0.3374 0.131 Uiso 1 1 calc R . . H7S3 H 0.4103 0.7734 0.3210 0.131 Uiso 1 1 calc R . . C8S C 0.4473(4) 0.9436(2) 0.09118(18) 0.0597(9) Uani 1 1 d . . . C9S C 0.5688(4) 0.9808(3) 0.1108(2) 0.0634(9) Uani 1 1 d . . . H9S H 0.6339 0.9487 0.0947 0.076 Uiso 1 1 calc R . . C10S C 0.5986(4) 1.0628(3) 0.1529(2) 0.0664(10) Uani 1 1 d . . . H10S H 0.6829 1.0866 0.1650 0.080 Uiso 1 1 calc R . . C11S C 0.5062(4) 1.1097(3) 0.17732(18) 0.0590(9) Uani 1 1 d . . . H11S H 0.5267 1.1658 0.2067 0.071 Uiso 1 1 calc R . . C12S C 0.3836(4) 1.0759(3) 0.1594(2) 0.0675(10) Uani 1 1 d . . . H12S H 0.3197 1.1086 0.1762 0.081 Uiso 1 1 calc R . . C13S C 0.3539(4) 0.9930(3) 0.1161(2) 0.0742(11) Uani 1 1 d . . . H13S H 0.2694 0.9699 0.1035 0.089 Uiso 1 1 calc R . . C14S C 0.4178(5) 0.8533(3) 0.0453(3) 0.1010(17) Uani 1 1 d . . . H14A H 0.4558 0.8628 0.0000 0.152 Uiso 1 1 calc R . . H14B H 0.3277 0.8387 0.0362 0.152 Uiso 1 1 calc R . . H14C H 0.4507 0.7997 0.0701 0.152 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 0.02197(10) 0.02459(10) 0.02381(10) -0.00075(7) 0.00047(7) 0.00378(7) I1 0.02665(9) 0.03636(10) 0.04250(11) -0.00229(7) 0.00396(7) 0.00837(7) P1 0.0288(3) 0.0263(3) 0.0264(3) 0.0007(2) -0.0015(2) 0.0023(2) P2 0.0236(3) 0.0274(3) 0.0252(3) 0.0005(2) 0.0003(2) 0.0027(2) O1 0.0347(10) 0.0326(9) 0.0317(9) -0.0028(7) 0.0025(7) 0.0087(8) O2 0.0323(9) 0.0333(9) 0.0340(9) -0.0023(7) -0.0036(7) 0.0029(7) S1 0.0343(3) 0.0377(4) 0.0467(4) -0.0144(3) 0.0002(3) 0.0024(3) N1 0.0304(11) 0.0364(12) 0.0307(11) -0.0008(9) 0.0033(9) 0.0013(9) C1 0.0293(12) 0.0318(12) 0.0235(12) 0.0021(9) 0.0011(9) 0.0009(10) C2 0.0336(14) 0.0409(15) 0.0332(14) -0.0047(11) -0.0015(11) -0.0082(11) C3 0.0376(16) 0.0585(19) 0.0516(18) -0.0071(15) -0.0017(14) -0.0088(14) C4 0.0457(19) 0.062(2) 0.060(2) -0.0059(17) -0.0097(16) -0.0228(16) C5 0.062(2) 0.052(2) 0.059(2) -0.0178(16) -0.0082(17) -0.0170(17) C6 0.061(2) 0.0482(18) 0.059(2) -0.0205(16) 0.0007(17) -0.0035(16) C7 0.0380(15) 0.0420(15) 0.0397(15) -0.0054(12) -0.0001(12) -0.0059(12) C8 0.0294(13) 0.0416(15) 0.0435(15) -0.0080(12) 0.0003(11) 0.0018(11) C9 0.0345(15) 0.067(2) 0.0511(19) -0.0081(16) 0.0077(13) 0.0011(14) C10 0.0338(15) 0.0504(18) 0.069(2) 0.0020(16) -0.0109(14) 0.0055(13) C11 0.0439(16) 0.0323(13) 0.0316(13) -0.0018(11) 0.0014(11) 0.0118(12) C12 0.065(2) 0.062(2) 0.076(3) -0.0390(19) -0.0116(19) 0.0243(18) C13 0.100(4) 0.111(4) 0.148(5) -0.095(4) -0.025(3) 0.024(3) C1A 0.0375(14) 0.0296(13) 0.0328(13) 0.0030(10) -0.0075(11) 0.0000(11) C2A 0.0542(18) 0.0344(15) 0.0417(16) -0.0038(12) -0.0006(13) -0.0015(13) C3A 0.072(2) 0.0372(16) 0.0532(19) -0.0076(14) -0.0064(17) -0.0026(16) C4A 0.068(2) 0.0368(16) 0.061(2) 0.0039(15) -0.0157(18) -0.0148(16) C5A 0.053(2) 0.0469(19) 0.073(2) 0.0130(17) 0.0048(17) -0.0139(15) C6A 0.0482(17) 0.0394(16) 0.0520(18) 0.0053(13) 0.0046(14) -0.0023(13) C1B 0.0374(14) 0.0277(12) 0.0278(12) 0.0034(10) 0.0016(10) 0.0022(10) C2B 0.0388(15) 0.0446(15) 0.0296(13) -0.0009(11) 0.0020(11) 0.0049(12) C3B 0.0458(17) 0.0468(17) 0.0435(16) 0.0065(13) 0.0143(13) 0.0107(13) C4B 0.068(2) 0.0471(17) 0.0369(16) -0.0019(13) 0.0145(15) 0.0155(15) C5B 0.070(2) 0.061(2) 0.0294(15) -0.0093(13) -0.0058(14) 0.0144(17) C6B 0.0480(17) 0.0406(15) 0.0344(14) -0.0022(12) -0.0052(12) 0.0107(13) C1C 0.0314(13) 0.0311(13) 0.0278(12) -0.0001(10) -0.0034(10) 0.0067(10) C2C 0.0378(15) 0.0367(14) 0.0406(15) 0.0068(12) -0.0064(12) 0.0035(11) C3C 0.0356(15) 0.0438(16) 0.0511(17) 0.0019(13) -0.0082(13) -0.0005(12) C4C 0.0389(16) 0.0569(19) 0.0489(18) 0.0051(14) -0.0100(13) 0.0144(14) C5C 0.0498(18) 0.0439(17) 0.0495(18) 0.0127(13) -0.0064(14) 0.0149(14) C6C 0.0412(15) 0.0335(14) 0.0386(15) 0.0048(11) -0.0020(12) 0.0063(11) C1D 0.0302(12) 0.0283(12) 0.0263(12) -0.0001(9) -0.0024(10) 0.0040(10) C2D 0.0312(13) 0.0286(13) 0.0402(14) 0.0027(11) 0.0003(11) 0.0017(10) C3D 0.0335(14) 0.0400(15) 0.0434(16) -0.0002(12) 0.0032(12) 0.0084(12) C4D 0.0472(17) 0.0328(14) 0.0452(16) -0.0057(12) -0.0009(13) 0.0120(12) C5D 0.0476(17) 0.0270(13) 0.0560(18) -0.0043(12) 0.0041(14) -0.0010(12) C6D 0.0340(14) 0.0336(14) 0.0408(15) -0.0015(11) 0.0041(11) 0.0004(11) C1E 0.0248(12) 0.0330(13) 0.0265(12) 0.0008(10) 0.0018(9) -0.0020(10) C2E 0.0356(14) 0.0411(15) 0.0353(14) 0.0020(11) -0.0024(11) 0.0043(11) C3E 0.0343(15) 0.0628(19) 0.0357(15) 0.0026(13) -0.0065(12) 0.0059(13) C4E 0.0347(15) 0.065(2) 0.0335(15) -0.0055(13) -0.0016(12) -0.0081(14) C5E 0.0465(17) 0.0472(17) 0.0381(15) -0.0099(13) 0.0058(13) -0.0023(13) C6E 0.0378(14) 0.0381(14) 0.0352(14) -0.0017(11) 0.0008(11) 0.0056(11) C1F 0.0253(12) 0.0285(12) 0.0347(13) 0.0026(10) 0.0038(10) 0.0030(9) C2F 0.0331(14) 0.0471(16) 0.0323(14) 0.0036(12) 0.0011(11) -0.0012(12) C3F 0.0431(17) 0.067(2) 0.0383(16) 0.0099(14) 0.0085(13) -0.0064(15) C4F 0.0310(15) 0.0568(19) 0.060(2) 0.0134(15) 0.0089(13) -0.0051(13) C5F 0.0287(13) 0.0509(17) 0.0442(16) 0.0081(13) -0.0040(12) -0.0043(12) C6F 0.0309(13) 0.0427(15) 0.0353(14) 0.0059(11) -0.0006(11) 0.0005(11) C1S 0.054(2) 0.060(2) 0.0472(18) -0.0022(15) -0.0068(15) 0.0238(16) C2S 0.055(2) 0.060(2) 0.063(2) -0.0015(17) -0.0019(17) 0.0037(17) C3S 0.082(3) 0.054(2) 0.062(2) -0.0062(17) 0.007(2) 0.011(2) C4S 0.075(3) 0.069(2) 0.055(2) -0.0034(18) 0.0141(19) 0.021(2) C5S 0.064(2) 0.077(3) 0.051(2) 0.0096(18) 0.0104(17) 0.003(2) C6S 0.069(2) 0.0507(19) 0.053(2) 0.0037(15) -0.0053(17) 0.0121(17) C7S 0.066(3) 0.107(4) 0.094(3) -0.025(3) -0.001(2) 0.039(3) C8S 0.092(3) 0.0402(17) 0.0467(19) 0.0057(14) 0.0114(18) 0.0015(18) C9S 0.063(2) 0.060(2) 0.069(2) 0.0001(18) 0.0067(19) 0.0140(18) C10S 0.064(2) 0.071(2) 0.062(2) -0.0067(19) -0.0032(18) 0.0103(19) C11S 0.078(3) 0.053(2) 0.0488(19) 0.0053(15) 0.0063(17) 0.0167(18) C12S 0.073(3) 0.068(2) 0.066(2) 0.005(2) 0.018(2) 0.020(2) C13S 0.055(2) 0.077(3) 0.090(3) 0.011(2) 0.011(2) 0.000(2) C14S 0.139(5) 0.065(3) 0.091(3) -0.012(2) 0.014(3) -0.022(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 C1 2.003(2) . ? Ru1 O1 2.1490(17) . ? Ru1 O2 2.2420(17) . ? Ru1 P1 2.3821(6) . ? Ru1 P2 2.3949(6) . ? Ru1 C11 2.551(3) . ? Ru1 I1 2.7356(3) . ? P1 C1C 1.831(2) . ? P1 C1A 1.833(3) . ? P1 C1B 1.842(3) . ? P2 C1E 1.831(2) . ? P2 C1F 1.835(2) . ? P2 C1D 1.845(2) . ? O1 C11 1.265(3) . ? O2 C11 1.265(3) . ? S1 C7 1.724(3) . ? S1 C1 1.758(3) . ? N1 C1 1.357(3) . ? N1 C2 1.419(3) . ? N1 C8 1.475(3) . ? C2 C7 1.384(4) . ? C2 C3 1.406(4) . ? C3 C4 1.391(4) . ? C4 C5 1.374(5) . ? C5 C6 1.371(5) . ? C6 C7 1.398(4) . ? C8 C10 1.529(4) . ? C8 C9 1.533(4) . ? C11 C12 1.501(4) . ? C12 C13 1.423(6) . ? C1A C6A 1.385(4) . ? C1A C2A 1.386(4) . ? C2A C3A 1.385(4) . ? C3A C4A 1.378(5) . ? C4A C5A 1.359(5) . ? C5A C6A 1.396(4) . ? C1B C2B 1.391(4) . ? C1B C6B 1.394(4) . ? C2B C3B 1.391(4) . ? C3B C4B 1.373(4) . ? C4B C5B 1.373(5) . ? C5B C6B 1.386(4) . ? C1C C2C 1.392(4) . ? C1C C6C 1.395(3) . ? C2C C3C 1.383(4) . ? C3C C4C 1.379(4) . ? C4C C5C 1.367(4) . ? C5C C6C 1.385(4) . ? C1D C2D 1.389(3) . ? C1D C6D 1.391(3) . ? C2D C3D 1.385(4) . ? C3D C4D 1.380(4) . ? C4D C5D 1.374(4) . ? C5D C6D 1.390(4) . ? C1E C2E 1.387(4) . ? C1E C6E 1.389(4) . ? C2E C3E 1.390(4) . ? C3E C4E 1.364(4) . ? C4E C5E 1.384(4) . ? C5E C6E 1.391(4) . ? C1F C2F 1.389(4) . ? C1F C6F 1.390(4) . ? C2F C3F 1.391(4) . ? C3F C4F 1.373(4) . ? C4F C5F 1.372(4) . ? C5F C6F 1.382(4) . ? C1S C2S 1.376(5) . ? C1S C6S 1.385(5) . ? C1S C7S 1.486(5) . ? C2S C3S 1.377(5) . ? C3S C4S 1.365(5) . ? C4S C5S 1.374(5) . ? C5S C6S 1.376(5) . ? C8S C9S 1.371(5) . ? C8S C13S 1.388(6) . ? C8S C14S 1.495(5) . ? C9S C10S 1.364(5) . ? C10S C11S 1.355(5) . ? C11S C12S 1.366(6) . ? C12S C13S 1.387(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 O1 107.77(9) . . ? C1 Ru1 O2 167.14(8) . . ? O1 Ru1 O2 59.39(7) . . ? C1 Ru1 P1 93.91(7) . . ? O1 Ru1 P1 88.31(5) . . ? O2 Ru1 P1 85.51(5) . . ? C1 Ru1 P2 94.97(7) . . ? O1 Ru1 P2 88.37(5) . . ? O2 Ru1 P2 85.68(5) . . ? P1 Ru1 P2 171.09(2) . . ? C1 Ru1 C11 137.44(10) . . ? O1 Ru1 C11 29.68(8) . . ? O2 Ru1 C11 29.71(8) . . ? P1 Ru1 C11 86.20(6) . . ? P2 Ru1 C11 86.82(6) . . ? C1 Ru1 I1 91.78(7) . . ? O1 Ru1 I1 160.45(5) . . ? O2 Ru1 I1 101.07(5) . . ? P1 Ru1 I1 90.446(17) . . ? P2 Ru1 I1 89.928(16) . . ? C11 Ru1 I1 130.78(6) . . ? C1C P1 C1A 101.78(12) . . ? C1C P1 C1B 100.83(11) . . ? C1A P1 C1B 103.09(12) . . ? C1C P1 Ru1 117.33(8) . . ? C1A P1 Ru1 117.80(8) . . ? C1B P1 Ru1 113.62(8) . . ? C1E P2 C1F 102.98(11) . . ? C1E P2 C1D 101.97(11) . . ? C1F P2 C1D 100.82(11) . . ? C1E P2 Ru1 118.79(8) . . ? C1F P2 Ru1 116.02(8) . . ? C1D P2 Ru1 113.79(8) . . ? C11 O1 Ru1 93.06(15) . . ? C11 O2 Ru1 88.81(15) . . ? C7 S1 C1 94.23(13) . . ? C1 N1 C2 117.4(2) . . ? C1 N1 C8 121.4(2) . . ? C2 N1 C8 121.2(2) . . ? N1 C1 S1 106.84(17) . . ? N1 C1 Ru1 132.25(18) . . ? S1 C1 Ru1 120.91(13) . . ? C7 C2 C3 119.6(3) . . ? C7 C2 N1 111.5(2) . . ? C3 C2 N1 128.8(3) . . ? C4 C3 C2 117.0(3) . . ? C5 C4 C3 123.0(3) . . ? C6 C5 C4 120.0(3) . . ? C5 C6 C7 118.3(3) . . ? C2 C7 C6 121.9(3) . . ? C2 C7 S1 110.0(2) . . ? C6 C7 S1 128.0(3) . . ? N1 C8 C10 112.1(2) . . ? N1 C8 C9 111.5(2) . . ? C10 C8 C9 112.2(2) . . ? O2 C11 O1 118.7(2) . . ? O2 C11 C12 122.3(3) . . ? O1 C11 C12 119.0(3) . . ? O2 C11 Ru1 61.48(13) . . ? O1 C11 Ru1 57.26(12) . . ? C12 C11 Ru1 176.0(2) . . ? C13 C12 C11 116.6(3) . . ? C6A C1A C2A 119.2(3) . . ? C6A C1A P1 123.6(2) . . ? C2A C1A P1 117.2(2) . . ? C3A C2A C1A 120.2(3) . . ? C4A C3A C2A 120.3(3) . . ? C5A C4A C3A 119.8(3) . . ? C4A C5A C6A 120.8(3) . . ? C1A C6A C5A 119.7(3) . . ? C2B C1B C6B 118.0(2) . . ? C2B C1B P1 118.78(19) . . ? C6B C1B P1 123.2(2) . . ? C1B C2B C3B 121.1(3) . . ? C4B C3B C2B 120.1(3) . . ? C5B C4B C3B 119.2(3) . . ? C4B C5B C6B 121.5(3) . . ? C5B C6B C1B 120.0(3) . . ? C2C C1C C6C 118.5(2) . . ? C2C C1C P1 119.44(19) . . ? C6C C1C P1 122.0(2) . . ? C3C C2C C1C 120.7(3) . . ? C4C C3C C2C 120.1(3) . . ? C5C C4C C3C 119.8(3) . . ? C4C C5C C6C 120.8(3) . . ? C5C C6C C1C 120.1(3) . . ? C2D C1D C6D 118.6(2) . . ? C2D C1D P2 118.36(19) . . ? C6D C1D P2 123.1(2) . . ? C3D C2D C1D 121.0(2) . . ? C4D C3D C2D 119.9(3) . . ? C5D C4D C3D 119.8(3) . . ? C4D C5D C6D 120.7(3) . . ? C5D C6D C1D 120.1(3) . . ? C2E C1E C6E 118.2(2) . . ? C2E C1E P2 123.8(2) . . ? C6E C1E P2 117.95(19) . . ? C1E C2E C3E 120.5(3) . . ? C4E C3E C2E 121.0(3) . . ? C3E C4E C5E 119.5(3) . . ? C4E C5E C6E 119.9(3) . . ? C1E C6E C5E 120.9(3) . . ? C2F C1F C6F 118.7(2) . . ? C2F C1F P2 122.3(2) . . ? C6F C1F P2 118.84(19) . . ? C1F C2F C3F 120.2(3) . . ? C4F C3F C2F 120.2(3) . . ? C5F C4F C3F 120.1(3) . . ? C4F C5F C6F 120.3(3) . . ? C5F C6F C1F 120.5(3) . . ? C2S C1S C6S 118.2(3) . . ? C2S C1S C7S 120.9(4) . . ? C6S C1S C7S 120.9(3) . . ? C1S C2S C3S 121.3(4) . . ? C4S C3S C2S 119.4(4) . . ? C3S C4S C5S 120.8(4) . . ? C4S C5S C6S 119.2(4) . . ? C5S C6S C1S 121.1(3) . . ? C9S C8S C13S 117.1(3) . . ? C9S C8S C14S 121.0(4) . . ? C13S C8S C14S 121.8(4) . . ? C10S C9S C8S 122.3(4) . . ? C11S C10S C9S 119.8(4) . . ? C10S C11S C12S 120.3(4) . . ? C11S C12S C13S 119.6(4) . . ? C12S C13S C8S 120.8(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.088 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.091 data_8 _database_code_depnum_ccdc_archive 'CCDC 778720' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H46 I N O2 P2 Ru S' _chemical_formula_weight 1002.84 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' S S 0.1246 0.1234 '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' I I -0.4742 1.8119 '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 11.1382(5) _cell_length_b 12.3698(6) _cell_length_c 18.7464(8) _cell_angle_alpha 74.5240(10) _cell_angle_beta 81.5730(10) _cell_angle_gamma 63.4010(10) _cell_volume 2224.63(18) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9511 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.55 _exptl_crystal_description 'Thin Plate' _exptl_crystal_colour Orange _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 1.205 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4860 _exptl_absorpt_correction_T_max 0.8689 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28984 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10201 _reflns_number_gt 9528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+1.2163P] 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 10201 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.150703(14) 0.034476(13) 0.265127(7) 0.01782(4) Uani 1 1 d . . . I1 I -0.021037(12) -0.069127(12) 0.270869(7) 0.02613(4) Uani 1 1 d . . . P1 P 0.32236(5) -0.17078(4) 0.29735(3) 0.02085(9) Uani 1 1 d . . . P2 P -0.04207(5) 0.23325(4) 0.24943(3) 0.02107(9) Uani 1 1 d . . . S1 S 0.14116(5) -0.03108(5) 0.10855(3) 0.02703(10) Uani 1 1 d . . . O1 O 0.27677(13) 0.10433(12) 0.29373(7) 0.0247(3) Uani 1 1 d . . . O2 O 0.16299(14) 0.03661(13) 0.38454(7) 0.0287(3) Uani 1 1 d . . . N1 N 0.21143(16) 0.13772(15) 0.10563(8) 0.0224(3) Uani 1 1 d . . . C1 C 0.17656(17) 0.05379(16) 0.15719(10) 0.0204(3) Uani 1 1 d . . . C2 C 0.19828(19) 0.14535(19) 0.03064(10) 0.0256(4) Uani 1 1 d . . . C3 C 0.2135(2) 0.2311(2) -0.03072(11) 0.0363(5) Uani 1 1 d . . . H3 H 0.2424 0.2893 -0.0256 0.044 Uiso 1 1 calc R . . C4 C 0.1852(3) 0.2285(2) -0.09951(12) 0.0435(6) Uani 1 1 d . . . H4 H 0.1936 0.2868 -0.1415 0.052 Uiso 1 1 calc R . . C5 C 0.1449(2) 0.1423(3) -0.10794(12) 0.0420(6) Uani 1 1 d . . . H5 H 0.1250 0.1434 -0.1552 0.050 Uiso 1 1 calc R . . C6 C 0.1333(2) 0.0544(2) -0.04745(11) 0.0336(5) Uani 1 1 d . . . H6 H 0.1080 -0.0057 -0.0532 0.040 Uiso 1 1 calc R . . C7 C 0.16014(19) 0.05690(19) 0.02230(10) 0.0264(4) Uani 1 1 d . . . C8 C 0.2528(2) 0.22315(18) 0.12506(10) 0.0250(4) Uani 1 1 d . . . H8A H 0.2078 0.2420 0.1721 0.030 Uiso 1 1 calc R . . H8B H 0.2208 0.3010 0.0872 0.030 Uiso 1 1 calc R . . C9 C 0.4027(2) 0.1771(2) 0.13232(14) 0.0398(5) Uani 1 1 d . . . H9 H 0.4275 0.1137 0.1795 0.048 Uiso 1 1 calc R . . C10 C 0.4289(3) 0.2833(3) 0.1408(2) 0.0715(9) Uani 1 1 d . . . H10A H 0.5218 0.2520 0.1535 0.107 Uiso 1 1 calc R . . H10B H 0.3701 0.3203 0.1797 0.107 Uiso 1 1 calc R . . H10C H 0.4117 0.3454 0.0945 0.107 Uiso 1 1 calc R . . C11 C 0.4901(3) 0.1156(3) 0.07252(18) 0.0665(9) Uani 1 1 d . . . H11A H 0.4693 0.0491 0.0688 0.100 Uiso 1 1 calc R . . H11B H 0.5838 0.0818 0.0845 0.100 Uiso 1 1 calc R . . H11C H 0.4738 0.1762 0.0256 0.100 Uiso 1 1 calc R . . C12 C 0.2450(2) 0.08412(18) 0.36226(11) 0.0272(4) Uani 1 1 d . . . C13 C 0.3048(3) 0.1180(2) 0.41485(13) 0.0462(6) Uani 1 1 d . . . H13A H 0.2764 0.0910 0.4652 0.069 Uiso 1 1 calc R . . H13B H 0.2746 0.2073 0.4032 0.069 Uiso 1 1 calc R . . H13C H 0.4020 0.0775 0.4102 0.069 Uiso 1 1 calc R . . C1A C -0.10345(19) 0.29672(18) 0.15482(10) 0.0254(4) Uani 1 1 d . . . C2A C -0.1577(2) 0.2356(2) 0.12563(12) 0.0350(5) Uani 1 1 d . . . H2A H -0.1677 0.1658 0.1557 0.042 Uiso 1 1 calc R . . C3A C -0.1970(3) 0.2774(2) 0.05258(14) 0.0463(6) Uani 1 1 d . . . H3A H -0.2355 0.2373 0.0338 0.056 Uiso 1 1 calc R . . C4A C -0.1794(3) 0.3776(2) 0.00762(13) 0.0489(6) Uani 1 1 d . . . H4A H -0.2049 0.4049 -0.0420 0.059 Uiso 1 1 calc R . . C5A C -0.1250(3) 0.4375(2) 0.03502(13) 0.0425(5) Uani 1 1 d . . . H5A H -0.1126 0.5055 0.0039 0.051 Uiso 1 1 calc R . . C6A C -0.0880(2) 0.39865(19) 0.10841(11) 0.0315(4) Uani 1 1 d . . . H6A H -0.0523 0.4414 0.1269 0.038 Uiso 1 1 calc R . . C1B C -0.0407(2) 0.36986(18) 0.27180(10) 0.0256(4) Uani 1 1 d . . . C2B C 0.0779(2) 0.3790(2) 0.27606(13) 0.0343(5) Uani 1 1 d . . . H2B H 0.1609 0.3138 0.2680 0.041 Uiso 1 1 calc R . . C3B C 0.0753(3) 0.4839(2) 0.29213(15) 0.0445(6) Uani 1 1 d . . . H3B H 0.1562 0.4886 0.2952 0.053 Uiso 1 1 calc R . . C4B C -0.0458(3) 0.5807(2) 0.30358(14) 0.0430(6) Uani 1 1 d . . . H4B H -0.0475 0.6517 0.3140 0.052 Uiso 1 1 calc R . . C5B C -0.1636(2) 0.5729(2) 0.29974(13) 0.0393(5) Uani 1 1 d . . . H5B H -0.2461 0.6388 0.3077 0.047 Uiso 1 1 calc R . . C6B C -0.1621(2) 0.4685(2) 0.28418(12) 0.0337(5) Uani 1 1 d . . . H6B H -0.2436 0.4643 0.2820 0.040 Uiso 1 1 calc R . . C1C C -0.18765(19) 0.22557(18) 0.30664(11) 0.0262(4) Uani 1 1 d . . . C2C C -0.3178(2) 0.2822(2) 0.28117(13) 0.0398(5) Uani 1 1 d . . . H2C H -0.3352 0.3280 0.2320 0.048 Uiso 1 1 calc R . . C3C C -0.4220(2) 0.2709(3) 0.32859(15) 0.0523(7) Uani 1 1 d . . . H3C H -0.5099 0.3090 0.3114 0.063 Uiso 1 1 calc R . . C4C C -0.3969(3) 0.2039(3) 0.40073(14) 0.0489(6) Uani 1 1 d . . . H4C H -0.4674 0.1949 0.4321 0.059 Uiso 1 1 calc R . . C5C C -0.2695(3) 0.1504(2) 0.42706(12) 0.0410(5) Uani 1 1 d . . . H5C H -0.2534 0.1070 0.4767 0.049 Uiso 1 1 calc R . . C6C C -0.1646(2) 0.1604(2) 0.38015(11) 0.0327(4) Uani 1 1 d . . . H6C H -0.0773 0.1228 0.3981 0.039 Uiso 1 1 calc R . . C1D C 0.47256(18) -0.16988(17) 0.32561(11) 0.0240(4) Uani 1 1 d . . . C2D C 0.5378(2) -0.10687(19) 0.27500(12) 0.0310(4) Uani 1 1 d . . . H2D H 0.5105 -0.0745 0.2257 0.037 Uiso 1 1 calc R . . C3D C 0.6422(2) -0.0910(2) 0.29600(13) 0.0363(5) Uani 1 1 d . . . H3D H 0.6846 -0.0478 0.2612 0.044 Uiso 1 1 calc R . . C4D C 0.6837(2) -0.1394(2) 0.36874(13) 0.0367(5) Uani 1 1 d . . . H4D H 0.7543 -0.1290 0.3835 0.044 Uiso 1 1 calc R . . C5D C 0.6210(2) -0.2025(2) 0.41894(12) 0.0370(5) Uani 1 1 d . . . H5D H 0.6498 -0.2360 0.4680 0.044 Uiso 1 1 calc R . . C6D C 0.5155(2) -0.2176(2) 0.39843(11) 0.0294(4) Uani 1 1 d . . . H6D H 0.4729 -0.2600 0.4337 0.035 Uiso 1 1 calc R . . C1E C 0.3842(2) -0.26848(17) 0.22920(10) 0.0260(4) Uani 1 1 d . . . C2E C 0.5049(2) -0.2932(2) 0.18991(13) 0.0395(5) Uani 1 1 d . . . H2E H 0.5605 -0.2580 0.1968 0.047 Uiso 1 1 calc R . . C3E C 0.5450(3) -0.3698(3) 0.14015(15) 0.0527(7) Uani 1 1 d . . . H3E H 0.6280 -0.3870 0.1142 0.063 Uiso 1 1 calc R . . C4E C 0.4641(3) -0.4207(2) 0.12861(14) 0.0500(6) Uani 1 1 d . . . H4E H 0.4911 -0.4715 0.0945 0.060 Uiso 1 1 calc R . . C5E C 0.3432(3) -0.3966(2) 0.16737(14) 0.0430(6) Uani 1 1 d . . . H5E H 0.2879 -0.4317 0.1600 0.052 Uiso 1 1 calc R . . C6E C 0.3029(2) -0.3207(2) 0.21714(13) 0.0356(5) Uani 1 1 d . . . H6E H 0.2200 -0.3042 0.2431 0.043 Uiso 1 1 calc R . . C1F C 0.2883(2) -0.27780(19) 0.37735(11) 0.0278(4) Uani 1 1 d . . . C2F C 0.1820(2) -0.2360(2) 0.42702(11) 0.0348(5) Uani 1 1 d . . . H2F H 0.1243 -0.1509 0.4199 0.042 Uiso 1 1 calc R . . C3F C 0.1609(3) -0.3203(3) 0.48740(13) 0.0507(7) Uani 1 1 d . . . H3F H 0.0880 -0.2917 0.5206 0.061 Uiso 1 1 calc R . . C4F C 0.2452(4) -0.4444(3) 0.49914(14) 0.0615(8) Uani 1 1 d . . . H4F H 0.2302 -0.5006 0.5402 0.074 Uiso 1 1 calc R . . C5F C 0.3522(3) -0.4868(2) 0.45036(15) 0.0575(7) Uani 1 1 d . . . H5F H 0.4103 -0.5719 0.4584 0.069 Uiso 1 1 calc R . . C6F C 0.3741(3) -0.4045(2) 0.38992(13) 0.0404(5) Uani 1 1 d . . . H6F H 0.4472 -0.4339 0.3570 0.048 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 0.01877(7) 0.01986(7) 0.01730(7) -0.00504(5) -0.00024(5) -0.01008(6) I1 0.02562(7) 0.02965(7) 0.02980(7) -0.00799(5) 0.00067(5) -0.01742(5) P1 0.0214(2) 0.0206(2) 0.0212(2) -0.00350(17) -0.00142(17) -0.01004(18) P2 0.0215(2) 0.0214(2) 0.0203(2) -0.00602(18) 0.00099(17) -0.00893(19) S1 0.0357(3) 0.0301(2) 0.0236(2) -0.00912(19) -0.00036(19) -0.0198(2) O1 0.0248(7) 0.0256(7) 0.0276(7) -0.0080(5) -0.0027(5) -0.0127(6) O2 0.0354(8) 0.0348(8) 0.0211(6) -0.0071(6) -0.0003(6) -0.0192(7) N1 0.0262(8) 0.0259(8) 0.0190(7) -0.0071(6) 0.0015(6) -0.0140(7) C1 0.0178(8) 0.0211(8) 0.0227(8) -0.0070(7) -0.0014(7) -0.0074(7) C2 0.0270(9) 0.0320(10) 0.0193(9) -0.0079(8) 0.0011(7) -0.0132(8) C3 0.0491(13) 0.0415(12) 0.0240(10) -0.0054(9) 0.0016(9) -0.0264(11) C4 0.0566(15) 0.0563(15) 0.0199(10) -0.0040(10) 0.0014(9) -0.0296(13) C5 0.0438(13) 0.0640(16) 0.0215(10) -0.0148(10) 0.0000(9) -0.0236(12) C6 0.0332(11) 0.0481(13) 0.0268(10) -0.0172(9) 0.0017(8) -0.0199(10) C7 0.0254(9) 0.0337(10) 0.0215(9) -0.0107(8) 0.0032(7) -0.0126(8) C8 0.0323(10) 0.0255(9) 0.0226(9) -0.0063(7) 0.0011(7) -0.0172(8) C9 0.0344(12) 0.0384(12) 0.0492(14) -0.0046(10) -0.0052(10) -0.0199(10) C10 0.0607(19) 0.073(2) 0.107(3) -0.0253(19) -0.0096(18) -0.0474(18) C11 0.0321(13) 0.101(3) 0.0677(19) -0.0390(18) 0.0093(13) -0.0217(15) C12 0.0323(10) 0.0261(10) 0.0270(9) -0.0078(8) -0.0070(8) -0.0130(8) C13 0.0647(17) 0.0525(15) 0.0382(12) -0.0130(11) -0.0150(11) -0.0341(13) C1A 0.0229(9) 0.0242(9) 0.0241(9) -0.0064(7) 0.0003(7) -0.0055(7) C2A 0.0412(12) 0.0297(11) 0.0330(11) -0.0058(9) -0.0099(9) -0.0123(9) C3A 0.0561(15) 0.0402(13) 0.0411(13) -0.0098(11) -0.0203(11) -0.0133(12) C4A 0.0596(16) 0.0463(14) 0.0275(11) -0.0031(10) -0.0153(11) -0.0100(12) C5A 0.0485(14) 0.0364(12) 0.0298(11) 0.0034(9) -0.0030(10) -0.0125(11) C6A 0.0301(10) 0.0305(11) 0.0288(10) -0.0045(8) -0.0002(8) -0.0099(9) C1B 0.0317(10) 0.0235(9) 0.0218(9) -0.0074(7) 0.0022(7) -0.0117(8) C2B 0.0344(11) 0.0269(10) 0.0448(12) -0.0145(9) 0.0038(9) -0.0138(9) C3B 0.0469(14) 0.0358(13) 0.0613(16) -0.0205(11) 0.0021(12) -0.0228(11) C4B 0.0607(16) 0.0289(11) 0.0458(13) -0.0170(10) 0.0047(11) -0.0219(11) C5B 0.0439(13) 0.0273(11) 0.0405(12) -0.0151(9) 0.0059(10) -0.0081(10) C6B 0.0336(11) 0.0299(11) 0.0361(11) -0.0126(9) 0.0034(9) -0.0108(9) C1C 0.0260(9) 0.0282(10) 0.0271(9) -0.0116(8) 0.0053(7) -0.0128(8) C2C 0.0272(11) 0.0535(14) 0.0372(12) -0.0119(10) 0.0024(9) -0.0161(10) C3C 0.0280(12) 0.082(2) 0.0539(15) -0.0253(14) 0.0085(11) -0.0272(13) C4C 0.0457(14) 0.0769(19) 0.0436(14) -0.0283(13) 0.0214(11) -0.0418(14) C5C 0.0508(14) 0.0552(15) 0.0281(11) -0.0152(10) 0.0130(10) -0.0334(12) C6C 0.0338(11) 0.0378(12) 0.0281(10) -0.0110(9) 0.0040(8) -0.0164(9) C1D 0.0214(9) 0.0224(9) 0.0275(9) -0.0061(7) -0.0009(7) -0.0086(7) C2D 0.0297(10) 0.0284(10) 0.0337(11) -0.0004(8) -0.0037(8) -0.0143(9) C3D 0.0298(11) 0.0338(11) 0.0488(13) -0.0071(10) 0.0036(9) -0.0193(9) C4D 0.0263(10) 0.0462(13) 0.0464(13) -0.0217(11) 0.0009(9) -0.0176(10) C5D 0.0319(11) 0.0530(14) 0.0318(11) -0.0165(10) -0.0025(9) -0.0189(10) C6D 0.0278(10) 0.0363(11) 0.0265(10) -0.0092(8) 0.0013(8) -0.0153(9) C1E 0.0291(10) 0.0211(9) 0.0241(9) -0.0035(7) -0.0037(7) -0.0075(8) C2E 0.0421(13) 0.0446(13) 0.0383(12) -0.0162(10) 0.0089(10) -0.0234(11) C3E 0.0585(17) 0.0582(17) 0.0453(14) -0.0276(13) 0.0224(12) -0.0267(14) C4E 0.0711(18) 0.0418(14) 0.0387(13) -0.0216(11) 0.0058(12) -0.0210(13) C5E 0.0539(15) 0.0370(12) 0.0459(13) -0.0170(11) -0.0072(11) -0.0204(11) C6E 0.0367(12) 0.0331(11) 0.0409(12) -0.0149(9) -0.0010(9) -0.0149(10) C1F 0.0332(10) 0.0309(10) 0.0241(9) -0.0007(8) -0.0042(8) -0.0200(9) C2F 0.0457(13) 0.0372(12) 0.0271(10) -0.0050(9) 0.0007(9) -0.0245(10) C3F 0.0742(19) 0.0576(16) 0.0299(12) -0.0088(11) 0.0139(12) -0.0419(15) C4F 0.107(3) 0.0503(16) 0.0323(13) 0.0058(12) 0.0040(14) -0.0487(18) C5F 0.086(2) 0.0328(13) 0.0430(14) 0.0061(11) -0.0025(14) -0.0241(14) C6F 0.0495(14) 0.0294(11) 0.0362(12) 0.0004(9) -0.0022(10) -0.0159(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.9665(18) . ? Ru1 O1 2.1354(12) . ? Ru1 O2 2.2706(13) . ? Ru1 P1 2.3749(5) . ? Ru1 P2 2.4112(5) . ? Ru1 C12 2.5555(18) . ? Ru1 I1 2.7156(2) . ? P1 C1D 1.8328(19) . ? P1 C1F 1.836(2) . ? P1 C1E 1.8406(19) . ? P2 C1A 1.833(2) . ? P2 C1C 1.834(2) . ? P2 C1B 1.8533(19) . ? S1 C7 1.735(2) . ? S1 C1 1.7539(18) . ? O1 C12 1.270(2) . ? O2 C12 1.262(2) . ? N1 C1 1.371(2) . ? N1 C2 1.409(2) . ? N1 C8 1.467(2) . ? C2 C7 1.389(3) . ? C2 C3 1.389(3) . ? C3 C4 1.383(3) . ? C4 C5 1.380(4) . ? C5 C6 1.382(3) . ? C6 C7 1.394(3) . ? C8 C9 1.518(3) . ? C9 C11 1.502(4) . ? C9 C10 1.518(4) . ? C12 C13 1.501(3) . ? C1A C6A 1.393(3) . ? C1A C2A 1.401(3) . ? C2A C3A 1.389(3) . ? C3A C4A 1.376(4) . ? C4A C5A 1.371(4) . ? C5A C6A 1.389(3) . ? C1B C2B 1.391(3) . ? C1B C6B 1.398(3) . ? C2B C3B 1.395(3) . ? C3B C4B 1.381(3) . ? C4B C5B 1.371(4) . ? C5B C6B 1.391(3) . ? C1C C2C 1.391(3) . ? C1C C6C 1.393(3) . ? C2C C3C 1.390(3) . ? C3C C4C 1.378(4) . ? C4C C5C 1.372(4) . ? C5C C6C 1.387(3) . ? C1D C2D 1.395(3) . ? C1D C6D 1.396(3) . ? C2D C3D 1.387(3) . ? C3D C4D 1.391(3) . ? C4D C5D 1.374(3) . ? C5D C6D 1.389(3) . ? C1E C2E 1.381(3) . ? C1E C6E 1.396(3) . ? C2E C3E 1.393(3) . ? C3E C4E 1.375(4) . ? C4E C5E 1.378(4) . ? C5E C6E 1.386(3) . ? C1F C2F 1.386(3) . ? C1F C6F 1.398(3) . ? C2F C3F 1.391(3) . ? C3F C4F 1.370(4) . ? C4F C5F 1.382(4) . ? C5F C6F 1.380(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 O1 104.32(6) . . ? C1 Ru1 O2 163.61(6) . . ? O1 Ru1 O2 59.29(5) . . ? C1 Ru1 P1 96.56(5) . . ? O1 Ru1 P1 89.90(4) . . ? O2 Ru1 P1 84.24(4) . . ? C1 Ru1 P2 90.85(5) . . ? O1 Ru1 P2 93.10(4) . . ? O2 Ru1 P2 90.06(4) . . ? P1 Ru1 P2 171.072(17) . . ? C1 Ru1 C12 134.04(7) . . ? O1 Ru1 C12 29.72(6) . . ? O2 Ru1 C12 29.57(6) . . ? P1 Ru1 C12 86.70(5) . . ? P2 Ru1 C12 91.74(5) . . ? C1 Ru1 I1 91.87(5) . . ? O1 Ru1 I1 163.77(4) . . ? O2 Ru1 I1 104.52(3) . . ? P1 Ru1 I1 87.152(13) . . ? P2 Ru1 I1 87.632(13) . . ? C12 Ru1 I1 134.08(5) . . ? C1D P1 C1F 101.90(9) . . ? C1D P1 C1E 105.03(9) . . ? C1F P1 C1E 100.06(9) . . ? C1D P1 Ru1 110.68(6) . . ? C1F P1 Ru1 117.26(7) . . ? C1E P1 Ru1 119.75(6) . . ? C1A P2 C1C 104.21(9) . . ? C1A P2 C1B 101.84(9) . . ? C1C P2 C1B 99.95(9) . . ? C1A P2 Ru1 113.67(6) . . ? C1C P2 Ru1 112.36(7) . . ? C1B P2 Ru1 122.50(7) . . ? C7 S1 C1 93.96(9) . . ? C12 O1 Ru1 93.79(11) . . ? C12 O2 Ru1 87.83(11) . . ? C1 N1 C2 116.96(15) . . ? C1 N1 C8 123.36(15) . . ? C2 N1 C8 119.57(15) . . ? N1 C1 S1 107.07(12) . . ? N1 C1 Ru1 129.46(13) . . ? S1 C1 Ru1 123.23(10) . . ? C7 C2 C3 120.47(18) . . ? C7 C2 N1 111.91(16) . . ? C3 C2 N1 127.56(18) . . ? C4 C3 C2 118.2(2) . . ? C5 C4 C3 121.5(2) . . ? C4 C5 C6 120.6(2) . . ? C5 C6 C7 118.5(2) . . ? C2 C7 C6 120.71(19) . . ? C2 C7 S1 109.79(14) . . ? C6 C7 S1 129.30(17) . . ? N1 C8 C9 115.84(17) . . ? C11 C9 C8 115.4(2) . . ? C11 C9 C10 112.4(2) . . ? C8 C9 C10 108.7(2) . . ? O2 C12 O1 119.09(16) . . ? O2 C12 C13 121.44(19) . . ? O1 C12 C13 119.47(19) . . ? O2 C12 Ru1 62.60(9) . . ? O1 C12 Ru1 56.49(9) . . ? C13 C12 Ru1 175.91(16) . . ? C6A C1A C2A 118.32(18) . . ? C6A C1A P2 121.98(15) . . ? C2A C1A P2 119.49(15) . . ? C3A C2A C1A 120.5(2) . . ? C4A C3A C2A 120.1(2) . . ? C5A C4A C3A 120.2(2) . . ? C4A C5A C6A 120.5(2) . . ? C5A C6A C1A 120.4(2) . . ? C2B C1B C6B 118.08(18) . . ? C2B C1B P2 122.23(15) . . ? C6B C1B P2 119.68(16) . . ? C1B C2B C3B 120.8(2) . . ? C4B C3B C2B 120.2(2) . . ? C5B C4B C3B 119.7(2) . . ? C4B C5B C6B 120.6(2) . . ? C5B C6B C1B 120.7(2) . . ? C2C C1C C6C 119.06(19) . . ? C2C C1C P2 123.91(16) . . ? C6C C1C P2 117.02(15) . . ? C3C C2C C1C 119.9(2) . . ? C4C C3C C2C 120.3(2) . . ? C5C C4C C3C 120.4(2) . . ? C4C C5C C6C 119.8(2) . . ? C5C C6C C1C 120.5(2) . . ? C2D C1D C6D 118.19(18) . . ? C2D C1D P1 119.03(15) . . ? C6D C1D P1 122.36(15) . . ? C3D C2D C1D 121.3(2) . . ? C2D C3D C4D 119.7(2) . . ? C5D C4D C3D 119.6(2) . . ? C4D C5D C6D 121.1(2) . . ? C5D C6D C1D 120.20(19) . . ? C2E C1E C6E 118.50(19) . . ? C2E C1E P1 124.24(16) . . ? C6E C1E P1 117.26(15) . . ? C1E C2E C3E 120.5(2) . . ? C4E C3E C2E 120.6(2) . . ? C3E C4E C5E 119.6(2) . . ? C4E C5E C6E 120.2(2) . . ? C5E C6E C1E 120.7(2) . . ? C2F C1F C6F 118.94(19) . . ? C2F C1F P1 121.83(16) . . ? C6F C1F P1 119.20(16) . . ? C1F C2F C3F 119.9(2) . . ? C4F C3F C2F 120.8(2) . . ? C3F C4F C5F 119.7(2) . . ? C6F C5F C4F 120.2(3) . . ? C5F C6F C1F 120.4(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.638 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.065 data_9 _database_code_depnum_ccdc_archive 'CCDC 778721' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H48 I N O2 P2 Ru S' _chemical_formula_weight 1016.86 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' S S 0.1246 0.1234 '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' I I -0.4742 1.8119 '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 11.5401(16) _cell_length_b 12.3535(17) _cell_length_c 17.615(3) _cell_angle_alpha 72.444(2) _cell_angle_beta 76.977(2) _cell_angle_gamma 69.123(2) _cell_volume 2217.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7550 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.52 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 1.210 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7129 _exptl_absorpt_correction_T_max 0.9094 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28850 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10157 _reflns_number_gt 9304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The bond distances for C8-C9A, C8-C9B, C9A-C10A, C9B-C10B, C9A-C11A, and C9B-C11B in the disordered isopropyl part were restrainted to be 1.52(0.02) angstroms. 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^)+(0.0264P)^2^+1.4816P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10157 _refine_ls_number_parameters 548 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _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 I1 I 0.062233(12) 0.473628(12) 0.243458(8) 0.02761(5) Uani 1 1 d . . . Ru1 Ru 0.316569(14) 0.380102(14) 0.241698(9) 0.01983(5) Uani 1 1 d . . . N1 N 0.37790(17) 0.28337(16) 0.41241(10) 0.0269(4) Uani 1 1 d . A . O1 O 0.51389(13) 0.33000(13) 0.20566(9) 0.0274(3) Uani 1 1 d . . . O2 O 0.39486(14) 0.44446(14) 0.11403(9) 0.0309(3) Uani 1 1 d . . . P1 P 0.30684(5) 0.21876(5) 0.19832(3) 0.02323(11) Uani 1 1 d . . . P2 P 0.31688(5) 0.56324(5) 0.26292(3) 0.02234(11) Uani 1 1 d . . . S1 S 0.16031(5) 0.28134(6) 0.41476(3) 0.03307(13) Uani 1 1 d . . . C1 C 0.29756(19) 0.30846(18) 0.35859(12) 0.0238(4) Uani 1 1 d . . . C2 C 0.3301(2) 0.25901(19) 0.49421(13) 0.0311(5) Uani 1 1 d . . . C3 C 0.3873(3) 0.2491(3) 0.55900(15) 0.0454(6) Uani 1 1 d . . . H3 H 0.4687 0.2540 0.5512 0.054 Uiso 1 1 calc R . . C4 C 0.3204(3) 0.2318(3) 0.63512(16) 0.0557(8) Uani 1 1 d . . . H4 H 0.3570 0.2258 0.6794 0.067 Uiso 1 1 calc R . . C5 C 0.2011(3) 0.2232(3) 0.64742(15) 0.0522(8) Uani 1 1 d . . . H5 H 0.1580 0.2113 0.6998 0.063 Uiso 1 1 calc R . . C6 C 0.1448(3) 0.2318(2) 0.58375(15) 0.0449(6) Uani 1 1 d . . . H6 H 0.0641 0.2250 0.5920 0.054 Uiso 1 1 calc R . . C7 C 0.2106(2) 0.2510(2) 0.50674(13) 0.0325(5) Uani 1 1 d . . . C8 C 0.5069(2) 0.2842(2) 0.38791(16) 0.0346(5) Uani 1 1 d D . . H8A H 0.522(3) 0.327(3) 0.4209(18) 0.047(8) Uiso 1 1 d . . . H8B H 0.513(3) 0.323(3) 0.3387(19) 0.047(8) Uiso 1 1 d . . . C9A C 0.5970(5) 0.1634(5) 0.4232(5) 0.0417(19) Uani 0.458(10) 1 d PD A 1 H9AA H 0.5810 0.1491 0.4825 0.050 Uiso 0.458(10) 1 calc PR A 1 C10A C 0.5824(8) 0.0649(8) 0.4016(7) 0.084(3) Uani 0.458(10) 1 d PD A 1 H10A H 0.4984 0.0602 0.4217 0.127 Uiso 0.458(10) 1 calc PR A 1 H10B H 0.6428 -0.0092 0.4250 0.127 Uiso 0.458(10) 1 calc PR A 1 H10C H 0.5961 0.0779 0.3436 0.127 Uiso 0.458(10) 1 calc PR A 1 C11A C 0.7279(8) 0.1751(9) 0.3956(7) 0.084(3) Uani 0.458(10) 1 d PD A 1 H11A H 0.7892 0.1001 0.4166 0.127 Uiso 0.458(10) 1 calc PR A 1 H11B H 0.7347 0.2377 0.4153 0.127 Uiso 0.458(10) 1 calc PR A 1 H11C H 0.7432 0.1951 0.3374 0.127 Uiso 0.458(10) 1 calc PR A 1 C9B C 0.6064(5) 0.1683(6) 0.3731(5) 0.057(2) Uani 0.542(10) 1 d PD A 2 H9BA H 0.5778 0.1417 0.3350 0.068 Uiso 0.542(10) 1 calc PR A 2 C10B C 0.6226(9) 0.0720(10) 0.4474(7) 0.140(5) Uani 0.542(10) 1 d PD A 2 H10D H 0.6857 0.0005 0.4354 0.210 Uiso 0.542(10) 1 calc PR A 2 H10E H 0.5439 0.0556 0.4692 0.210 Uiso 0.542(10) 1 calc PR A 2 H10F H 0.6489 0.0966 0.4864 0.210 Uiso 0.542(10) 1 calc PR A 2 C11B C 0.7295(8) 0.1839(10) 0.3374(8) 0.140(5) Uani 0.542(10) 1 d PD A 2 H11D H 0.7883 0.1083 0.3291 0.210 Uiso 0.542(10) 1 calc PR A 2 H11E H 0.7593 0.2112 0.3733 0.210 Uiso 0.542(10) 1 calc PR A 2 H11F H 0.7218 0.2426 0.2863 0.210 Uiso 0.542(10) 1 calc PR A 2 C12 C 0.5035(2) 0.3880(2) 0.13317(13) 0.0316(5) Uani 1 1 d . . . C13 C 0.6170(3) 0.3898(3) 0.07186(18) 0.0613(9) Uani 1 1 d . . . H13A H 0.6122 0.3566 0.0291 0.074 Uiso 1 1 calc R . . H13B H 0.6139 0.4733 0.0478 0.074 Uiso 1 1 calc R . . C14 C 0.7403(2) 0.3234(3) 0.1017(2) 0.0554(8) Uani 1 1 d . . . H14A H 0.7494 0.3589 0.1413 0.083 Uiso 1 1 calc R . . H14B H 0.8069 0.3277 0.0571 0.083 Uiso 1 1 calc R . . H14C H 0.7450 0.2406 0.1260 0.083 Uiso 1 1 calc R . . C1A C 0.2521(2) 0.10094(19) 0.27330(13) 0.0282(4) Uani 1 1 d . . . C2A C 0.1262(2) 0.1290(2) 0.30521(16) 0.0417(6) Uani 1 1 d . . . H2A H 0.0712 0.2054 0.2862 0.050 Uiso 1 1 calc R . . C3A C 0.0810(3) 0.0451(3) 0.36494(18) 0.0505(7) Uani 1 1 d . . . H3A H -0.0041 0.0652 0.3862 0.061 Uiso 1 1 calc R . . C4A C 0.1600(3) -0.0669(3) 0.39306(17) 0.0529(8) Uani 1 1 d . . . H4A H 0.1295 -0.1231 0.4339 0.063 Uiso 1 1 calc R . . C5A C 0.2831(3) -0.0960(3) 0.36131(19) 0.0553(8) Uani 1 1 d . . . H5A H 0.3370 -0.1731 0.3798 0.066 Uiso 1 1 calc R . . C6A C 0.3297(3) -0.0130(2) 0.30193(17) 0.0428(6) Uani 1 1 d . . . H6A H 0.4149 -0.0344 0.2810 0.051 Uiso 1 1 calc R . . C1B C 0.4584(2) 0.13710(19) 0.15014(13) 0.0272(4) Uani 1 1 d . . . C2B C 0.5595(2) 0.0817(2) 0.19397(15) 0.0345(5) Uani 1 1 d . . . H2B H 0.5485 0.0859 0.2476 0.041 Uiso 1 1 calc R . . C3B C 0.6756(2) 0.0207(2) 0.16013(17) 0.0404(6) Uani 1 1 d . . . H3B H 0.7419 -0.0178 0.1912 0.048 Uiso 1 1 calc R . . C4B C 0.6944(2) 0.0162(2) 0.08089(17) 0.0424(6) Uani 1 1 d . . . H4B H 0.7735 -0.0247 0.0577 0.051 Uiso 1 1 calc R . . C5B C 0.5972(3) 0.0718(3) 0.03623(17) 0.0461(6) Uani 1 1 d . . . H5B H 0.6101 0.0691 -0.0179 0.055 Uiso 1 1 calc R . . C6B C 0.4792(2) 0.1323(2) 0.06993(14) 0.0368(5) Uani 1 1 d . . . H6B H 0.4133 0.1699 0.0385 0.044 Uiso 1 1 calc R . . C1C C 0.21014(19) 0.25855(19) 0.11854(13) 0.0267(4) Uani 1 1 d . . . C2C C 0.1596(2) 0.1775(2) 0.10902(14) 0.0337(5) Uani 1 1 d . . . H2C H 0.1681 0.1038 0.1469 0.040 Uiso 1 1 calc R . . C3C C 0.0967(2) 0.2048(2) 0.04381(15) 0.0384(5) Uani 1 1 d . . . H3C H 0.0621 0.1497 0.0383 0.046 Uiso 1 1 calc R . . C4C C 0.0846(2) 0.3118(2) -0.01292(15) 0.0372(5) Uani 1 1 d . . . H4C H 0.0418 0.3300 -0.0569 0.045 Uiso 1 1 calc R . . C5C C 0.1362(2) 0.3921(2) -0.00440(14) 0.0361(5) Uani 1 1 d . . . H5C H 0.1297 0.4646 -0.0434 0.043 Uiso 1 1 calc R . . C6C C 0.1975(2) 0.3666(2) 0.06117(14) 0.0309(5) Uani 1 1 d . . . H6C H 0.2306 0.4226 0.0669 0.037 Uiso 1 1 calc R . . C1D C 0.28053(19) 0.57179(18) 0.36811(13) 0.0250(4) Uani 1 1 d . . . C2D C 0.3645(2) 0.5804(2) 0.40936(14) 0.0314(5) Uani 1 1 d . . . H2D H 0.4423 0.5881 0.3821 0.038 Uiso 1 1 calc R . . C3D C 0.3345(3) 0.5779(2) 0.49105(15) 0.0406(6) Uani 1 1 d . . . H3D H 0.3923 0.5839 0.5184 0.049 Uiso 1 1 calc R . . C4D C 0.2213(3) 0.5668(2) 0.53189(15) 0.0405(6) Uani 1 1 d . . . H4D H 0.2016 0.5652 0.5869 0.049 Uiso 1 1 calc R . . C5D C 0.1370(2) 0.5582(2) 0.49159(14) 0.0347(5) Uani 1 1 d . . . H5D H 0.0593 0.5507 0.5193 0.042 Uiso 1 1 calc R . . C6D C 0.1657(2) 0.5604(2) 0.41040(14) 0.0298(5) Uani 1 1 d . . . H6D H 0.1074 0.5541 0.3836 0.036 Uiso 1 1 calc R . . C1E C 0.2016(2) 0.69610(19) 0.21209(13) 0.0269(4) Uani 1 1 d . . . C2E C 0.1273(2) 0.7881(2) 0.24809(15) 0.0351(5) Uani 1 1 d . . . H2E H 0.1310 0.7813 0.3022 0.042 Uiso 1 1 calc R . . C3E C 0.0474(2) 0.8903(2) 0.20470(18) 0.0451(6) Uani 1 1 d . . . H3E H -0.0030 0.9520 0.2296 0.054 Uiso 1 1 calc R . . C4E C 0.0418(3) 0.9013(2) 0.12535(18) 0.0460(7) Uani 1 1 d . . . H4E H -0.0130 0.9700 0.0963 0.055 Uiso 1 1 calc R . . C5E C 0.1168(3) 0.8112(2) 0.08875(16) 0.0424(6) Uani 1 1 d . . . H5E H 0.1143 0.8194 0.0343 0.051 Uiso 1 1 calc R . . C6E C 0.1957(2) 0.7087(2) 0.13148(14) 0.0343(5) Uani 1 1 d . . . H6E H 0.2456 0.6472 0.1061 0.041 Uiso 1 1 calc R . . C1G C 0.4574(2) 0.6135(2) 0.22764(13) 0.0285(4) Uani 1 1 d . . . C2G C 0.4463(2) 0.7335(2) 0.19340(16) 0.0409(6) Uani 1 1 d . . . H2G H 0.3667 0.7890 0.1858 0.049 Uiso 1 1 calc R . . C3G C 0.5505(3) 0.7727(3) 0.17022(17) 0.0497(7) Uani 1 1 d . . . H3G H 0.5411 0.8541 0.1470 0.060 Uiso 1 1 calc R . . C4G C 0.6676(3) 0.6926(3) 0.18114(17) 0.0478(7) Uani 1 1 d . . . H4G H 0.7383 0.7192 0.1657 0.057 Uiso 1 1 calc R . . C5G C 0.6810(2) 0.5741(3) 0.2146(2) 0.0509(7) Uani 1 1 d . . . H5G H 0.7611 0.5194 0.2222 0.061 Uiso 1 1 calc R . . C6G C 0.5769(2) 0.5339(2) 0.23749(18) 0.0427(6) Uani 1 1 d . . . H6G H 0.5875 0.4522 0.2599 0.051 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 I1 0.02016(7) 0.03014(8) 0.03185(8) -0.00772(6) -0.00590(5) -0.00537(5) Ru1 0.01756(8) 0.02229(8) 0.01942(8) -0.00576(6) -0.00238(6) -0.00541(6) N1 0.0276(9) 0.0269(9) 0.0237(9) -0.0041(7) -0.0061(7) -0.0057(7) O1 0.0211(7) 0.0317(8) 0.0295(8) -0.0094(6) -0.0002(6) -0.0086(6) O2 0.0285(8) 0.0378(9) 0.0242(7) -0.0033(6) -0.0012(6) -0.0124(7) P1 0.0230(3) 0.0233(3) 0.0238(3) -0.0068(2) -0.0044(2) -0.0059(2) P2 0.0207(2) 0.0236(3) 0.0238(3) -0.0069(2) -0.0036(2) -0.0067(2) S1 0.0262(3) 0.0442(3) 0.0246(3) -0.0046(2) -0.0008(2) -0.0106(2) C1 0.0230(10) 0.0225(10) 0.0260(10) -0.0080(8) -0.0026(8) -0.0057(8) C2 0.0376(12) 0.0259(11) 0.0230(10) -0.0032(8) -0.0075(9) -0.0021(9) C3 0.0517(16) 0.0519(16) 0.0324(13) -0.0058(12) -0.0150(12) -0.0139(13) C4 0.073(2) 0.0622(19) 0.0263(13) -0.0072(12) -0.0167(13) -0.0120(16) C5 0.0581(18) 0.0528(17) 0.0235(12) -0.0045(11) -0.0007(12) 0.0019(14) C6 0.0413(14) 0.0448(15) 0.0281(12) -0.0011(11) 0.0010(10) 0.0010(12) C7 0.0343(12) 0.0297(11) 0.0237(11) -0.0033(9) -0.0050(9) -0.0003(9) C8 0.0271(11) 0.0441(14) 0.0321(13) -0.0056(11) -0.0093(10) -0.0100(10) C9A 0.031(3) 0.048(4) 0.036(4) -0.007(3) -0.016(3) 0.006(2) C10A 0.052(3) 0.071(4) 0.111(6) -0.022(4) -0.030(4) 0.017(3) C11A 0.052(3) 0.071(4) 0.111(6) -0.022(4) -0.030(4) 0.017(3) C9B 0.033(3) 0.089(5) 0.058(5) -0.049(4) -0.014(3) 0.000(3) C10B 0.058(4) 0.115(6) 0.139(8) 0.031(5) 0.026(4) 0.025(4) C11B 0.058(4) 0.115(6) 0.139(8) 0.031(5) 0.026(4) 0.025(4) C12 0.0282(11) 0.0391(13) 0.0280(11) -0.0092(10) 0.0030(9) -0.0142(10) C13 0.0368(15) 0.094(3) 0.0412(16) -0.0073(16) 0.0113(12) -0.0230(16) C14 0.0295(13) 0.0666(19) 0.068(2) -0.0282(16) 0.0157(13) -0.0166(13) C1A 0.0351(12) 0.0269(11) 0.0266(11) -0.0066(9) -0.0057(9) -0.0132(9) C2A 0.0389(14) 0.0365(13) 0.0462(15) -0.0080(11) -0.0001(11) -0.0129(11) C3A 0.0487(16) 0.0586(18) 0.0483(16) -0.0103(14) 0.0068(13) -0.0316(14) C4A 0.075(2) 0.0546(18) 0.0389(15) 0.0041(13) -0.0106(14) -0.0424(17) C5A 0.0623(19) 0.0362(14) 0.0618(19) 0.0124(13) -0.0236(16) -0.0196(14) C6A 0.0416(14) 0.0355(13) 0.0469(15) -0.0013(11) -0.0095(12) -0.0119(11) C1B 0.0264(10) 0.0241(10) 0.0310(11) -0.0087(9) -0.0041(9) -0.0059(8) C2B 0.0303(12) 0.0367(13) 0.0358(12) -0.0113(10) -0.0072(10) -0.0060(10) C3B 0.0274(12) 0.0373(13) 0.0549(16) -0.0133(12) -0.0095(11) -0.0042(10) C4B 0.0282(12) 0.0384(14) 0.0580(17) -0.0201(12) 0.0070(11) -0.0081(10) C5B 0.0421(15) 0.0554(17) 0.0390(14) -0.0205(13) 0.0080(11) -0.0136(13) C6B 0.0337(12) 0.0434(14) 0.0305(12) -0.0119(10) -0.0021(10) -0.0078(11) C1C 0.0236(10) 0.0301(11) 0.0265(10) -0.0101(9) -0.0042(8) -0.0053(8) C2C 0.0352(12) 0.0327(12) 0.0369(13) -0.0086(10) -0.0100(10) -0.0113(10) C3C 0.0352(13) 0.0457(14) 0.0433(14) -0.0162(11) -0.0102(11) -0.0157(11) C4C 0.0307(12) 0.0513(15) 0.0319(12) -0.0137(11) -0.0094(10) -0.0093(11) C5C 0.0332(12) 0.0422(13) 0.0288(12) -0.0053(10) -0.0068(10) -0.0081(10) C6C 0.0295(11) 0.0323(12) 0.0322(12) -0.0091(9) -0.0065(9) -0.0088(9) C1D 0.0261(10) 0.0220(10) 0.0268(10) -0.0074(8) -0.0047(8) -0.0053(8) C2D 0.0306(11) 0.0353(12) 0.0321(12) -0.0087(10) -0.0084(9) -0.0120(9) C3D 0.0450(14) 0.0504(15) 0.0349(13) -0.0137(11) -0.0137(11) -0.0171(12) C4D 0.0506(15) 0.0456(14) 0.0268(12) -0.0122(11) -0.0041(11) -0.0146(12) C5D 0.0335(12) 0.0372(13) 0.0325(12) -0.0131(10) 0.0023(10) -0.0101(10) C6D 0.0266(11) 0.0334(12) 0.0321(11) -0.0130(9) -0.0030(9) -0.0088(9) C1E 0.0251(10) 0.0241(10) 0.0323(11) -0.0035(9) -0.0076(9) -0.0090(8) C2E 0.0326(12) 0.0292(11) 0.0404(13) -0.0082(10) -0.0044(10) -0.0065(9) C3E 0.0376(14) 0.0268(12) 0.0622(18) -0.0072(12) -0.0053(12) -0.0036(10) C4E 0.0382(14) 0.0336(13) 0.0615(18) 0.0069(12) -0.0238(13) -0.0106(11) C5E 0.0472(15) 0.0386(14) 0.0426(14) 0.0035(11) -0.0216(12) -0.0165(12) C6E 0.0371(13) 0.0321(12) 0.0354(12) -0.0056(10) -0.0124(10) -0.0103(10) C1G 0.0270(11) 0.0346(12) 0.0281(11) -0.0115(9) -0.0007(9) -0.0131(9) C2G 0.0388(14) 0.0414(14) 0.0432(14) -0.0031(11) -0.0043(11) -0.0197(11) C3G 0.0530(17) 0.0526(17) 0.0494(16) -0.0042(13) -0.0006(13) -0.0337(14) C4G 0.0423(15) 0.0711(19) 0.0485(16) -0.0306(14) 0.0135(12) -0.0380(14) C5G 0.0259(12) 0.0588(18) 0.080(2) -0.0373(16) 0.0013(13) -0.0158(12) C6G 0.0261(12) 0.0414(14) 0.0661(18) -0.0207(13) -0.0035(11) -0.0122(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ru1 2.7412(4) . ? Ru1 C1 1.976(2) . ? Ru1 O1 2.1336(14) . ? Ru1 O2 2.2413(15) . ? Ru1 P1 2.3846(6) . ? Ru1 P2 2.4031(6) . ? Ru1 C12 2.549(2) . ? N1 C1 1.367(3) . ? N1 C2 1.403(3) . ? N1 C8 1.457(3) . ? O1 C12 1.271(3) . ? O2 C12 1.264(3) . ? P1 C1C 1.833(2) . ? P1 C1A 1.839(2) . ? P1 C1B 1.840(2) . ? P2 C1D 1.832(2) . ? P2 C1E 1.833(2) . ? P2 C1G 1.853(2) . ? S1 C7 1.734(2) . ? S1 C1 1.753(2) . ? C2 C7 1.380(3) . ? C2 C3 1.397(3) . ? C3 C4 1.385(4) . ? C4 C5 1.382(5) . ? C5 C6 1.378(4) . ? C6 C7 1.394(3) . ? C8 C9A 1.523(6) . ? C8 C9B 1.534(6) . ? C9A C10A 1.452(11) . ? C9A C11A 1.524(10) . ? C9B C11B 1.472(10) . ? C9B C10B 1.475(12) . ? C12 C13 1.500(3) . ? C13 C14 1.490(4) . ? C1A C6A 1.384(3) . ? C1A C2A 1.392(3) . ? C2A C3A 1.390(4) . ? C3A C4A 1.372(4) . ? C4A C5A 1.363(5) . ? C5A C6A 1.388(4) . ? C1B C2B 1.394(3) . ? C1B C6B 1.395(3) . ? C2B C3B 1.382(3) . ? C3B C4B 1.378(4) . ? C4B C5B 1.368(4) . ? C5B C6B 1.394(3) . ? C1C C2C 1.390(3) . ? C1C C6C 1.392(3) . ? C2C C3C 1.388(3) . ? C3C C4C 1.379(4) . ? C4C C5C 1.382(4) . ? C5C C6C 1.387(3) . ? C1D C2D 1.384(3) . ? C1D C6D 1.399(3) . ? C2D C3D 1.396(3) . ? C3D C4D 1.374(4) . ? C4D C5D 1.376(3) . ? C5D C6D 1.387(3) . ? C1E C2E 1.387(3) . ? C1E C6E 1.396(3) . ? C2E C3E 1.391(3) . ? C3E C4E 1.377(4) . ? C4E C5E 1.378(4) . ? C5E C6E 1.382(3) . ? C1G C2G 1.392(3) . ? C1G C6G 1.392(3) . ? C2G C3G 1.386(4) . ? C3G C4G 1.376(4) . ? C4G C5G 1.369(4) . ? C5G C6G 1.392(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 O1 104.50(7) . . ? C1 Ru1 O2 163.84(7) . . ? O1 Ru1 O2 59.55(6) . . ? C1 Ru1 P1 97.83(6) . . ? O1 Ru1 P1 89.79(4) . . ? O2 Ru1 P1 85.40(4) . . ? C1 Ru1 P2 91.48(6) . . ? O1 Ru1 P2 91.19(4) . . ? O2 Ru1 P2 86.60(4) . . ? P1 Ru1 P2 170.085(19) . . ? C1 Ru1 C12 134.28(8) . . ? O1 Ru1 C12 29.83(7) . . ? O2 Ru1 C12 29.72(6) . . ? P1 Ru1 C12 87.26(5) . . ? P2 Ru1 C12 88.68(5) . . ? C1 Ru1 I1 91.41(6) . . ? O1 Ru1 I1 164.09(4) . . ? O2 Ru1 I1 104.57(4) . . ? P1 Ru1 I1 87.709(15) . . ? P2 Ru1 I1 88.657(14) . . ? C12 Ru1 I1 134.28(5) . . ? C1 N1 C2 117.03(18) . . ? C1 N1 C8 122.79(19) . . ? C2 N1 C8 120.17(19) . . ? C12 O1 Ru1 93.50(13) . . ? C12 O2 Ru1 88.75(13) . . ? C1C P1 C1A 102.30(10) . . ? C1C P1 C1B 100.01(10) . . ? C1A P1 C1B 104.12(10) . . ? C1C P1 Ru1 116.52(7) . . ? C1A P1 Ru1 118.41(7) . . ? C1B P1 Ru1 113.13(7) . . ? C1D P2 C1E 103.87(10) . . ? C1D P2 C1G 102.50(10) . . ? C1E P2 C1G 99.22(10) . . ? C1D P2 Ru1 114.63(7) . . ? C1E P2 Ru1 113.61(7) . . ? C1G P2 Ru1 120.64(7) . . ? C7 S1 C1 94.27(11) . . ? N1 C1 S1 106.55(15) . . ? N1 C1 Ru1 128.79(15) . . ? S1 C1 Ru1 124.27(11) . . ? C7 C2 C3 120.3(2) . . ? C7 C2 N1 112.38(19) . . ? C3 C2 N1 127.2(2) . . ? C4 C3 C2 118.0(3) . . ? C5 C4 C3 121.5(3) . . ? C6 C5 C4 120.7(3) . . ? C5 C6 C7 118.3(3) . . ? C2 C7 C6 121.2(2) . . ? C2 C7 S1 109.28(16) . . ? C6 C7 S1 129.2(2) . . ? N1 C8 C9A 110.6(3) . . ? N1 C8 C9B 117.7(3) . . ? C9A C8 C9B 32.3(3) . . ? C10A C9A C8 113.2(6) . . ? C10A C9A C11A 112.9(7) . . ? C8 C9A C11A 106.2(5) . . ? C11B C9B C10B 108.3(6) . . ? C11B C9B C8 113.0(7) . . ? C10B C9B C8 112.1(7) . . ? O2 C12 O1 118.19(19) . . ? O2 C12 C13 120.8(2) . . ? O1 C12 C13 121.0(2) . . ? O2 C12 Ru1 61.53(11) . . ? O1 C12 Ru1 56.66(10) . . ? C13 C12 Ru1 177.7(2) . . ? C14 C13 C12 116.2(2) . . ? C6A C1A C2A 118.0(2) . . ? C6A C1A P1 123.77(19) . . ? C2A C1A P1 118.21(18) . . ? C3A C2A C1A 120.6(3) . . ? C4A C3A C2A 120.4(3) . . ? C5A C4A C3A 119.5(3) . . ? C4A C5A C6A 120.8(3) . . ? C1A C6A C5A 120.7(3) . . ? C2B C1B C6B 117.8(2) . . ? C2B C1B P1 119.19(17) . . ? C6B C1B P1 122.99(17) . . ? C3B C2B C1B 121.4(2) . . ? C4B C3B C2B 120.1(2) . . ? C5B C4B C3B 119.6(2) . . ? C4B C5B C6B 120.9(3) . . ? C5B C6B C1B 120.3(2) . . ? C2C C1C C6C 118.8(2) . . ? C2C C1C P1 121.10(17) . . ? C6C C1C P1 119.79(17) . . ? C3C C2C C1C 120.4(2) . . ? C4C C3C C2C 120.7(2) . . ? C3C C4C C5C 119.3(2) . . ? C4C C5C C6C 120.6(2) . . ? C5C C6C C1C 120.4(2) . . ? C2D C1D C6D 118.3(2) . . ? C2D C1D P2 123.24(17) . . ? C6D C1D P2 118.27(16) . . ? C1D C2D C3D 120.5(2) . . ? C4D C3D C2D 120.6(2) . . ? C3D C4D C5D 119.5(2) . . ? C4D C5D C6D 120.5(2) . . ? C5D C6D C1D 120.6(2) . . ? C2E C1E C6E 118.8(2) . . ? C2E C1E P2 123.08(18) . . ? C6E C1E P2 117.92(17) . . ? C1E C2E C3E 120.4(2) . . ? C4E C3E C2E 120.2(3) . . ? C3E C4E C5E 119.7(2) . . ? C4E C5E C6E 120.6(3) . . ? C5E C6E C1E 120.2(2) . . ? C2G C1G C6G 117.7(2) . . ? C2G C1G P2 120.89(18) . . ? C6G C1G P2 121.36(18) . . ? C3G C2G C1G 121.3(3) . . ? C4G C3G C2G 120.0(3) . . ? C5G C4G C3G 119.8(2) . . ? C4G C5G C6G 120.5(3) . . ? C5G C6G C1G 120.7(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.618 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.070