# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1614 # Note CIF contains data for 4 out of the 6 structures reported in the paper data_dm5a #----------------------------------------------------------------------- _audit_creation_date '1999-07-15' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_requested_journal ' Dalton' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Anthony C. Willis' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address ' Martin A. Bennett ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Guandolina Chung ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' David C.R. Hockless ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Horst Neumann ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; dm5a ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 40.162(3) _cell_length_b 9.466(4) _cell_length_c 19.354(3) _cell_angle_alpha 90 _cell_angle_beta 112.937(7) _cell_angle_gamma 90 _cell_volume 6777(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13.8 _cell_measurement_theta_max 18.6 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 699.73 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H40 O4 P2 Ru ' _chemical_formula_moiety 'C36 H40 O4 P2 Ru ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2896.00 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_correction_T_min 0.90 _exptl_special_details ; The scan width was (0.80+0.34tan\q)\% with an \w scan speed of 2\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.11 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 0 0 3 1 4 0 0 2 _diffrn_reflns_number 6598 _reflns_number_total 6395 _reflns_number_gt 4070 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01655 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01934 _diffrn_orient_matrix_UB_12 0.02253 _diffrn_orient_matrix_UB_13 0.05002 _diffrn_orient_matrix_UB_21 0.01884 _diffrn_orient_matrix_UB_22 -0.03081 _diffrn_orient_matrix_UB_23 -0.01863 _diffrn_orient_matrix_UB_31 0.00147 _diffrn_orient_matrix_UB_32 0.09850 _diffrn_orient_matrix_UB_33 -0.01727 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 288 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 320 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 32 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 16 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 8 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.0000 0.0000 0.0000 0.0387(1) 1.000 S Uani d ? Ru(2) 0.2500 0.2500 0.5000 0.0400(1) 1.000 S Uani d ? P(1) -0.04691(3) 0.0753(1) -0.11046(6) 0.0421(3) 1.000 . Uani d ? P(2) 0.21779(3) 0.1567(1) 0.38003(6) 0.0453(3) 1.000 . Uani d ? O(11) -0.02032(7) 0.1295(3) 0.0598(1) 0.0466(9) 1.000 . Uani d ? O(12) -0.03037(6) -0.1715(3) 0.0052(1) 0.0460(8) 1.000 . Uani d ? O(21) 0.29707(6) 0.1670(3) 0.4976(1) 0.0485(9) 1.000 . Uani d ? O(22) 0.24058(6) 0.0770(3) 0.5544(1) 0.0455(9) 1.000 . Uani d ? C(101) -0.0413(1) 0.0832(5) 0.0897(2) 0.049(1) 1.000 . Uani d ? C(102) -0.0546(1) 0.1942(5) 0.1288(2) 0.075(2) 1.000 . Uani d ? C(103) -0.0525(1) -0.0575(5) 0.0883(2) 0.054(1) 1.000 . Uani d ? C(104) -0.0480(1) -0.1717(5) 0.0475(2) 0.049(1) 1.000 . Uani d ? C(105) -0.0650(1) -0.3125(5) 0.0514(3) 0.075(2) 1.000 . Uani d ? C(106) -0.04287(9) 0.2574(4) -0.1377(2) 0.041(1) 1.000 . Uani d ? C(107) -0.0357(1) 0.3634(5) -0.0841(2) 0.054(1) 1.000 . Uani d ? C(108) -0.0308(1) 0.5021(5) -0.1015(3) 0.066(2) 1.000 . Uani d ? C(109) -0.0316(1) 0.5344(5) -0.1711(3) 0.071(2) 1.000 . Uani d ? C(110) -0.0380(1) 0.4325(5) -0.2239(3) 0.064(2) 1.000 . Uani d ? C(111) -0.0437(1) 0.2945(5) -0.2081(2) 0.055(1) 1.000 . Uani d ? C(112) -0.0922(1) 0.0648(4) -0.1085(2) 0.043(1) 1.000 . Uani d ? C(113) -0.1087(1) 0.1767(5) -0.0889(2) 0.058(2) 1.000 . Uani d ? C(114) -0.1421(1) 0.1623(6) -0.0850(3) 0.073(2) 1.000 . Uani d ? C(115) -0.1594(1) 0.0345(7) -0.1001(3) 0.074(2) 1.000 . Uani d ? C(116) -0.1437(1) -0.0790(6) -0.1183(3) 0.074(2) 1.000 . Uani d ? C(117) -0.1099(1) -0.0646(5) -0.1218(2) 0.061(2) 1.000 . Uani d ? C(118) -0.0522(1) -0.0291(5) -0.1928(2) 0.059(2) 1.000 . Uani d ? C(201) 0.3066(1) 0.0407(5) 0.5185(2) 0.052(1) 1.000 . Uani d ? C(202) 0.3410(1) -0.0061(5) 0.5108(3) 0.083(2) 1.000 . Uani d ? C(203) 0.2894(1) -0.0559(4) 0.5470(2) 0.057(2) 1.000 . Uani d ? C(204) 0.2592(1) -0.0348(4) 0.5647(2) 0.046(1) 1.000 . Uani d ? C(205) 0.2477(1) -0.1545(5) 0.6017(3) 0.070(2) 1.000 . Uani d ? C(206) 0.1874(1) 0.2812(4) 0.3120(2) 0.050(1) 1.000 . Uani d ? C(207) 0.1984(1) 0.3657(5) 0.2673(3) 0.076(2) 1.000 . Uani d ? C(208) 0.1745(2) 0.4586(6) 0.2173(3) 0.105(2) 1.000 . Uani d ? C(209) 0.1401(2) 0.4693(6) 0.2112(3) 0.108(2) 1.000 . Uani d ? C(210) 0.1291(1) 0.3897(6) 0.2565(3) 0.098(2) 1.000 . Uani d ? C(211) 0.1523(1) 0.2968(5) 0.3071(3) 0.073(2) 1.000 . Uani d ? C(212) 0.1867(1) 0.0113(4) 0.3691(2) 0.046(1) 1.000 . Uani d ? C(213) 0.1709(1) -0.0038(5) 0.4205(2) 0.054(1) 1.000 . Uani d ? C(214) 0.1451(1) -0.1064(5) 0.4117(2) 0.066(2) 1.000 . Uani d ? C(215) 0.1346(1) -0.1950(5) 0.3511(3) 0.071(2) 1.000 . Uani d ? C(216) 0.1499(1) -0.1826(5) 0.2994(3) 0.073(2) 1.000 . Uani d ? C(217) 0.1757(1) -0.0801(5) 0.3084(2) 0.062(2) 1.000 . Uani d ? C(218) 0.2466(1) 0.0971(5) 0.3332(2) 0.074(2) 1.000 . Uani d ? H(102b) -0.0677 0.2645 0.0936 0.090 1.000 . Uiso c ? H(102c) -0.0700 0.1516 0.1497 0.090 1.000 . Uiso c ? H(102a) -0.0346 0.2366 0.1676 0.090 1.000 . Uiso c ? H(103) -0.0650 -0.0779 0.1199 0.065 1.000 . Uiso c ? H(105b) -0.0816 -0.3385 0.0027 0.091 1.000 . Uiso c ? H(105c) -0.0467 -0.3824 0.0699 0.091 1.000 . Uiso c ? H(105a) -0.0775 -0.3049 0.0841 0.091 1.000 . Uiso c ? H(107) -0.0341 0.3408 -0.0351 0.065 1.000 . Uiso c ? H(108) -0.0269 0.5745 -0.0652 0.079 1.000 . Uiso c ? H(109) -0.0276 0.6290 -0.1825 0.085 1.000 . Uiso c ? H(110) -0.0387 0.4561 -0.2721 0.077 1.000 . Uiso c ? H(111) -0.0482 0.2239 -0.2456 0.066 1.000 . Uiso c ? H(113) -0.0968 0.2657 -0.0779 0.070 1.000 . Uiso c ? H(114) -0.1531 0.2409 -0.0719 0.087 1.000 . Uiso c ? H(115) -0.1825 0.0249 -0.0978 0.089 1.000 . Uiso c ? H(116) -0.1557 -0.1677 -0.1286 0.088 1.000 . Uiso c ? H(117) -0.0988 -0.1446 -0.1335 0.073 1.000 . Uiso c ? H(118c) -0.0301 -0.0299 -0.1998 0.071 1.000 . Uiso c ? H(118b) -0.0706 0.0112 -0.2357 0.071 1.000 . Uiso c ? H(118a) -0.0587 -0.1230 -0.1861 0.071 1.000 . Uiso c ? H(202c) 0.3604 0.0535 0.5402 0.099 1.000 . Uiso c ? H(202a) 0.3463 -0.1009 0.5276 0.099 1.000 . Uiso c ? H(202b) 0.3380 -0.0002 0.4597 0.099 1.000 . Uiso c ? H(203) 0.2993 -0.1484 0.5556 0.069 1.000 . Uiso c ? H(205c) 0.2634 -0.2327 0.6079 0.084 1.000 . Uiso c ? H(205a) 0.2487 -0.1247 0.6494 0.084 1.000 . Uiso c ? H(205b) 0.2236 -0.1814 0.5712 0.084 1.000 . Uiso c ? H(207) 0.2226 0.3603 0.2706 0.091 1.000 . Uiso c ? H(208) 0.1825 0.5162 0.1867 0.126 1.000 . Uiso c ? H(209) 0.1237 0.5318 0.1756 0.129 1.000 . Uiso c ? H(210) 0.1049 0.3981 0.2533 0.117 1.000 . Uiso c ? H(211) 0.1442 0.2429 0.3389 0.088 1.000 . Uiso c ? H(213) 0.1779 0.0575 0.4626 0.065 1.000 . Uiso c ? H(214) 0.1345 -0.1154 0.4477 0.079 1.000 . Uiso c ? H(215) 0.1168 -0.2652 0.3450 0.085 1.000 . Uiso c ? H(216) 0.1427 -0.2443 0.2574 0.088 1.000 . Uiso c ? H(217) 0.1862 -0.0721 0.2722 0.074 1.000 . Uiso c ? H(218c) 0.2591 0.1756 0.3241 0.088 1.000 . Uiso c ? H(218a) 0.2636 0.0306 0.3641 0.088 1.000 . Uiso c ? H(218b) 0.2322 0.0539 0.2868 0.088 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0360(3) 0.0447(3) 0.0356(3) 0.0040(2) 0.0140(2) 0.0033(2) Ru(2) 0.0316(2) 0.0413(3) 0.0442(3) 0.0068(2) 0.0114(2) 0.0063(3) P(1) 0.0418(6) 0.0449(7) 0.0366(6) 0.0044(6) 0.0122(5) 0.0006(5) P(2) 0.0405(6) 0.0491(7) 0.0450(7) 0.0062(6) 0.0153(5) 0.0043(6) O(11) 0.045(2) 0.055(2) 0.042(2) 0.004(1) 0.020(1) 0.002(1) O(12) 0.041(2) 0.050(2) 0.047(2) 0.002(1) 0.016(1) 0.004(1) O(21) 0.036(2) 0.053(2) 0.055(2) 0.011(1) 0.016(1) 0.010(2) O(22) 0.039(2) 0.043(2) 0.052(2) 0.006(1) 0.015(1) 0.007(1) C(101) 0.043(3) 0.066(3) 0.038(3) 0.013(2) 0.014(2) 0.004(2) C(102) 0.085(4) 0.088(4) 0.068(3) 0.016(3) 0.047(3) -0.001(3) C(103) 0.046(3) 0.074(4) 0.050(3) 0.000(3) 0.027(2) 0.005(3) C(104) 0.038(2) 0.058(3) 0.048(3) 0.001(2) 0.013(2) 0.010(2) C(105) 0.069(3) 0.073(4) 0.094(4) -0.012(3) 0.044(3) 0.008(3) C(106) 0.031(2) 0.048(3) 0.039(2) 0.005(2) 0.007(2) 0.006(2) C(107) 0.051(3) 0.053(3) 0.053(3) 0.004(2) 0.013(2) 0.000(2) C(108) 0.053(3) 0.051(3) 0.080(4) 0.001(3) 0.013(3) -0.004(3) C(109) 0.048(3) 0.057(4) 0.101(4) 0.001(3) 0.022(3) 0.021(3) C(110) 0.057(3) 0.067(4) 0.068(3) 0.003(3) 0.023(3) 0.023(3) C(111) 0.047(3) 0.063(3) 0.052(3) 0.002(2) 0.015(2) 0.001(2) C(112) 0.039(2) 0.053(3) 0.028(2) 0.002(2) 0.005(2) 0.003(2) C(113) 0.057(3) 0.061(3) 0.061(3) 0.004(3) 0.027(2) 0.000(3) C(114) 0.066(3) 0.086(4) 0.076(4) 0.010(3) 0.038(3) -0.002(3) C(115) 0.049(3) 0.116(5) 0.059(3) -0.007(3) 0.023(3) 0.006(3) C(116) 0.054(3) 0.094(4) 0.063(3) -0.025(3) 0.014(3) -0.008(3) C(117) 0.053(3) 0.064(3) 0.058(3) -0.002(3) 0.013(2) -0.004(3) C(118) 0.063(3) 0.062(3) 0.049(3) 0.008(3) 0.020(2) -0.008(2) C(201) 0.043(3) 0.061(3) 0.049(3) 0.021(2) 0.016(2) 0.009(2) C(202) 0.075(3) 0.083(4) 0.105(4) 0.043(3) 0.050(3) 0.038(3) C(203) 0.058(3) 0.048(3) 0.066(3) 0.018(2) 0.024(3) 0.010(2) C(204) 0.044(3) 0.040(3) 0.046(3) 0.002(2) 0.008(2) 0.005(2) C(205) 0.068(3) 0.052(3) 0.086(4) 0.009(3) 0.027(3) 0.017(3) C(206) 0.053(3) 0.046(3) 0.041(3) -0.001(2) 0.008(2) 0.001(2) C(207) 0.081(4) 0.072(4) 0.062(3) -0.009(3) 0.015(3) 0.019(3) C(208) 0.142(6) 0.075(5) 0.066(4) -0.007(5) 0.007(4) 0.031(3) C(209) 0.115(5) 0.058(4) 0.084(5) 0.011(4) -0.033(4) 0.012(3) C(210) 0.066(4) 0.067(4) 0.117(5) 0.009(3) -0.012(3) 0.004(4) C(211) 0.058(3) 0.062(4) 0.085(4) 0.012(3) 0.012(3) 0.012(3) C(212) 0.042(2) 0.046(3) 0.043(2) 0.010(2) 0.006(2) 0.002(2) C(213) 0.045(3) 0.060(3) 0.053(3) -0.004(3) 0.014(2) -0.005(3) C(214) 0.046(3) 0.081(4) 0.059(3) -0.008(3) 0.007(2) 0.005(3) C(215) 0.058(3) 0.061(3) 0.063(3) -0.008(3) -0.009(3) 0.013(3) C(216) 0.090(4) 0.052(3) 0.050(3) -0.005(3) -0.003(3) -0.005(3) C(217) 0.078(3) 0.054(3) 0.045(3) 0.004(3) 0.015(3) 0.004(2) C(218) 0.062(3) 0.103(4) 0.063(3) 0.012(3) 0.032(3) -0.004(3) #----------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.000001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4070 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0230 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.780 _refine_ls_shift/su_max 0.0450 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.40 _refine_diff_density_max 0.40 #----------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) P(1) 2.343(1) . . yes Ru(1) P(1) 2.343(1) . 3 yes Ru(1) O(11) 2.060(2) . . yes Ru(1) O(11) 2.060(2) . 3 yes Ru(1) O(12) 2.057(2) . . yes Ru(1) O(12) 2.057(2) . 3 yes Ru(2) P(2) 2.346(1) . . yes Ru(2) P(2) 2.346(1) . 7_556 yes Ru(2) O(21) 2.064(2) . . yes Ru(2) O(21) 2.064(2) . 7_556 yes Ru(2) O(22) 2.060(2) . . yes Ru(2) O(22) 2.060(2) . 7_556 yes P(1) C(106) 1.828(4) . . yes P(1) C(112) 1.837(4) . . yes P(1) C(118) 1.816(4) . . yes P(2) C(206) 1.832(4) . . yes P(2) C(212) 1.816(4) . . yes P(2) C(218) 1.816(4) . . yes O(11) C(101) 1.273(4) . . yes O(12) C(104) 1.273(4) . . yes O(21) C(201) 1.271(4) . . yes O(22) C(204) 1.266(4) . . yes C(101) C(102) 1.509(5) . . yes C(101) C(103) 1.402(5) . . yes C(102) H(102b 0.95 . . no C(102) H(102c 0.95 . . no C(102) H(102a 0.95 . . no C(103) C(104) 1.392(5) . . yes C(103) H(103) 0.95 . . no C(104) C(105) 1.513(5) . . yes C(105) H(105b 0.95 . . no C(105) H(105c 0.95 . . no C(105) H(105a 0.95 . . no C(106) C(107) 1.390(5) . . yes C(106) C(111) 1.395(5) . . yes C(107) C(108) 1.388(6) . . yes C(107) H(107) 0.95 . . no C(108) C(109) 1.370(6) . . yes C(108) H(108) 0.95 . . no C(109) C(110) 1.355(6) . . yes C(109) H(109) 0.95 . . no C(110) C(111) 1.381(6) . . yes C(110) H(110) 0.95 . . no C(111) H(111) 0.95 . . no C(112) C(113) 1.379(5) . . yes C(112) C(117) 1.390(5) . . yes C(113) C(114) 1.380(5) . . yes C(113) H(113) 0.95 . . no C(114) C(115) 1.367(6) . . yes C(114) H(114) 0.95 . . no C(115) C(116) 1.360(6) . . yes C(115) H(115) 0.95 . . no C(116) C(117) 1.389(5) . . yes C(116) H(116) 0.95 . . no C(117) H(117) 0.95 . . no C(118) H(118c 0.95 . . no C(118) H(118b 0.95 . . no C(118) H(118a 0.95 . . no C(201) C(202) 1.516(5) . . yes C(201) C(203) 1.384(5) . . yes C(202) H(202c 0.95 . . no C(202) H(202a 0.95 . . no C(202) H(202b 0.95 . . no C(203) C(204) 1.395(5) . . yes C(203) H(203) 0.95 . . no C(204) C(205) 1.507(5) . . yes C(205) H(205c 0.95 . . no C(205) H(205a 0.95 . . no C(205) H(205b 0.95 . . no C(206) C(207) 1.372(5) . . yes C(206) C(211) 1.384(5) . . yes C(207) C(208) 1.380(6) . . yes C(207) H(207) 0.95 . . no C(208) C(209) 1.343(8) . . yes C(208) H(208) 0.95 . . no C(209) C(210) 1.355(8) . . yes C(209) H(209) 0.95 . . no C(210) C(211) 1.375(6) . . yes C(210) H(210) 0.95 . . no C(211) H(211) 0.95 . . no C(212) C(213) 1.378(5) . . yes C(212) C(217) 1.385(5) . . yes C(213) C(214) 1.383(5) . . yes C(213) H(213) 0.95 . . no C(214) C(215) 1.367(6) . . yes C(214) H(214) 0.95 . . no C(215) C(216) 1.368(6) . . yes C(215) H(215) 0.95 . . no C(216) C(217) 1.381(6) . . yes C(216) H(216) 0.95 . . no C(217) H(217) 0.95 . . no C(218) H(218c 0.95 . . no C(218) H(218a 0.95 . . no C(218) H(218b 0.95 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Ru(1) P(1) 180.00 . . 3 yes P(1) Ru(1) O(11) 88.72(7) . . . yes P(1) Ru(1) O(11) 91.28(7) . . 3 yes P(1) Ru(1) O(12) 90.22(7) . . . yes P(1) Ru(1) O(12) 89.78(7) . . 3 yes P(1) Ru(1) O(11) 91.28(7) 3 . . yes P(1) Ru(1) O(11) 88.72(7) 3 . 3 yes P(1) Ru(1) O(12) 89.78(7) 3 . . yes P(1) Ru(1) O(12) 90.22(7) 3 . 3 yes O(11) Ru(1) O(11) 180.00 . . 3 yes O(11) Ru(1) O(12) 94.0(1) . . . yes O(11) Ru(1) O(12) 86.0(1) . . 3 yes O(11) Ru(1) O(12) 86.0(1) 3 . . yes O(11) Ru(1) O(12) 94.0(1) 3 . 3 yes O(12) Ru(1) O(12) 180.00 . . 3 yes P(2) Ru(2) P(2) 180.0000(1) . . 7_556 yes P(2) Ru(2) O(21) 89.49(7) . . . yes P(2) Ru(2) O(21) 90.51(7) . . 7_556 yes P(2) Ru(2) O(22) 93.79(7) . . . yes P(2) Ru(2) O(22) 86.21(7) . . 7_556 yes P(2) Ru(2) O(21) 90.51(7) 7_556 . . yes P(2) Ru(2) O(21) 89.49(7) 7_556 . 7_556 yes P(2) Ru(2) O(22) 86.21(7) 7_556 . . yes P(2) Ru(2) O(22) 93.79(7) 7_556 . 7_556 yes O(21) Ru(2) O(21) 180.00 . . 7_556 yes O(21) Ru(2) O(22) 93.5(1) . . . yes O(21) Ru(2) O(22) 86.5(1) . . 7_556 yes O(21) Ru(2) O(22) 86.5(1) 7_556 . . yes O(21) Ru(2) O(22) 93.5(1) 7_556 . 7_556 yes O(22) Ru(2) O(22) 180.00 . . 7_556 yes Ru(1) P(1) C(106) 114.8(1) . . . yes Ru(1) P(1) C(112) 114.6(1) . . . yes Ru(1) P(1) C(118) 114.4(1) . . . yes C(106) P(1) C(112) 104.9(2) . . . yes C(106) P(1) C(118) 104.7(2) . . . yes C(112) P(1) C(118) 102.1(2) . . . yes Ru(2) P(2) C(206) 115.1(1) . . . yes Ru(2) P(2) C(212) 119.3(1) . . . yes Ru(2) P(2) C(218) 113.5(1) . . . yes C(206) P(2) C(212) 99.7(2) . . . yes C(206) P(2) C(218) 102.5(2) . . . yes C(212) P(2) C(218) 104.5(2) . . . yes Ru(1) O(11) C(101) 121.9(3) . . . yes Ru(1) O(12) C(104) 121.5(3) . . . yes Ru(2) O(21) C(201) 120.9(3) . . . yes Ru(2) O(22) C(204) 122.0(3) . . . yes O(11) C(101) C(102) 114.5(4) . . . yes O(11) C(101) C(103) 125.6(4) . . . yes C(102) C(101) C(103) 119.9(4) . . . yes C(101) C(102) H(102b 109.5 . . . no C(101) C(102) H(102c 109.5 . . . no C(101) C(102) H(102a 109.5 . . . no H(102b C(102) H(102c 109.5 . . . no H(102b C(102) H(102a 109.5 . . . no H(102c C(102) H(102a 109.5 . . . no C(101) C(103) C(104) 129.7(4) . . . yes C(101) C(103) H(103) 115.2 . . . no C(104) C(103) H(103) 115.2 . . . no O(12) C(104) C(103) 126.2(4) . . . yes O(12) C(104) C(105) 114.2(4) . . . yes C(103) C(104) C(105) 119.7(4) . . . yes C(104) C(105) H(105b 109.5 . . . no C(104) C(105) H(105c 109.5 . . . no C(104) C(105) H(105a 109.5 . . . no H(105b C(105) H(105c 109.5 . . . no H(105b C(105) H(105a 109.5 . . . no H(105c C(105) H(105a 109.5 . . . no P(1) C(106) C(107) 118.8(3) . . . yes P(1) C(106) C(111) 123.2(3) . . . yes C(107) C(106) C(111) 117.8(4) . . . yes C(106) C(107) C(108) 120.6(4) . . . yes C(106) C(107) H(107) 119.7 . . . no C(108) C(107) H(107) 119.7 . . . no C(107) C(108) C(109) 119.9(5) . . . yes C(107) C(108) H(108) 120.0 . . . no C(109) C(108) H(108) 120.0 . . . no C(108) C(109) C(110) 120.4(5) . . . yes C(108) C(109) H(109) 119.8 . . . no C(110) C(109) H(109) 119.8 . . . no C(109) C(110) C(111) 120.4(4) . . . yes C(109) C(110) H(110) 119.8 . . . no C(111) C(110) H(110) 119.8 . . . no C(106) C(111) C(110) 120.7(4) . . . yes C(106) C(111) H(111) 119.6 . . . no C(110) C(111) H(111) 119.6 . . . no P(1) C(112) C(113) 123.4(3) . . . yes P(1) C(112) C(117) 119.0(3) . . . yes C(113) C(112) C(117) 117.5(4) . . . yes C(112) C(113) C(114) 121.4(4) . . . yes C(112) C(113) H(113) 119.3 . . . no C(114) C(113) H(113) 119.3 . . . no C(113) C(114) C(115) 119.9(5) . . . yes C(113) C(114) H(114) 120.1 . . . no C(115) C(114) H(114) 120.0 . . . no C(114) C(115) C(116) 120.4(5) . . . yes C(114) C(115) H(115) 119.8 . . . no C(116) C(115) H(115) 119.8 . . . no C(115) C(116) C(117) 119.7(5) . . . yes C(115) C(116) H(116) 120.2 . . . no C(117) C(116) H(116) 120.2 . . . no C(112) C(117) C(116) 121.1(4) . . . yes C(112) C(117) H(117) 119.4 . . . no C(116) C(117) H(117) 119.5 . . . no P(1) C(118) H(118c 109.5 . . . no P(1) C(118) H(118b 109.5 . . . no P(1) C(118) H(118a 109.5 . . . no H(118c C(118) H(118b 109.5 . . . no H(118c C(118) H(118a 109.5 . . . no H(118b C(118) H(118a 109.5 . . . no O(21) C(201) C(202) 114.5(4) . . . yes O(21) C(201) C(203) 127.9(4) . . . yes C(202) C(201) C(203) 117.6(4) . . . yes C(201) C(202) H(202c 109.5 . . . no C(201) C(202) H(202a 109.5 . . . no C(201) C(202) H(202b 109.5 . . . no H(202c C(202) H(202a 109.5 . . . no H(202c C(202) H(202b 109.5 . . . no H(202a C(202) H(202b 109.5 . . . no C(201) C(203) C(204) 128.2(4) . . . yes C(201) C(203) H(203) 115.9 . . . no C(204) C(203) H(203) 115.9 . . . no O(22) C(204) C(203) 126.7(4) . . . yes O(22) C(204) C(205) 115.5(4) . . . yes C(203) C(204) C(205) 117.8(4) . . . yes C(204) C(205) H(205c 109.5 . . . no C(204) C(205) H(205a 109.5 . . . no C(204) C(205) H(205b 109.5 . . . no H(205c C(205) H(205a 109.5 . . . no H(205c C(205) H(205b 109.5 . . . no H(205a C(205) H(205b 109.5 . . . no P(2) C(206) C(207) 122.8(4) . . . yes P(2) C(206) C(211) 119.5(4) . . . yes C(207) C(206) C(211) 117.6(4) . . . yes C(206) C(207) C(208) 120.5(5) . . . yes C(206) C(207) H(207) 119.8 . . . no C(208) C(207) H(207) 119.7 . . . no C(207) C(208) C(209) 121.4(6) . . . yes C(207) C(208) H(208) 119.3 . . . no C(209) C(208) H(208) 119.3 . . . no C(208) C(209) C(210) 119.0(6) . . . yes C(208) C(209) H(209) 120.5 . . . no C(210) C(209) H(209) 120.5 . . . no C(209) C(210) C(211) 121.0(6) . . . yes C(209) C(210) H(210) 119.5 . . . no C(211) C(210) H(210) 119.5 . . . no C(206) C(211) C(210) 120.5(5) . . . yes C(206) C(211) H(211) 119.8 . . . no C(210) C(211) H(211) 119.7 . . . no P(2) C(212) C(213) 118.9(3) . . . yes P(2) C(212) C(217) 123.3(3) . . . yes C(213) C(212) C(217) 117.6(4) . . . yes C(212) C(213) C(214) 121.2(4) . . . yes C(212) C(213) H(213) 119.4 . . . no C(214) C(213) H(213) 119.4 . . . no C(213) C(214) C(215) 120.1(4) . . . yes C(213) C(214) H(214) 120.0 . . . no C(215) C(214) H(214) 120.0 . . . no C(214) C(215) C(216) 120.0(5) . . . yes C(214) C(215) H(215) 120.0 . . . no C(216) C(215) H(215) 120.0 . . . no C(215) C(216) C(217) 119.7(5) . . . yes C(215) C(216) H(216) 120.1 . . . no C(217) C(216) H(216) 120.1 . . . no C(212) C(217) C(216) 121.4(4) . . . yes C(212) C(217) H(217) 119.3 . . . no C(216) C(217) H(217) 119.3 . . . no P(2) C(218) H(218c 109.5 . . . no P(2) C(218) H(218a 109.5 . . . no P(2) C(218) H(218b 109.5 . . . no H(218c C(218) H(218a 109.5 . . . no H(218c C(218) H(218b 109.5 . . . no H(218a C(218) H(218b 109.5 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(110) C(110) 3.573(9) . 2_554 no #----------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) P(1) C(106) C(107) . . . . -48.9(3) no Ru(1) P(1) C(106) C(111) . . . . 125.7(3) no Ru(1) P(1) C(112) C(113) . . . . 94.2(3) no Ru(1) P(1) C(112) C(117) . . . . -80.7(3) no Ru(1) P(1) C(106) C(107) . 3 3 3 48.9(3) no Ru(1) P(1) C(106) C(111) . 3 3 3 -125.7(3) no Ru(1) P(1) C(112) C(113) . 3 3 3 -94.2(3) no Ru(1) P(1) C(112) C(117) . 3 3 3 80.7(3) no Ru(1) O(11) C(101) C(102) . . . . -177.8(3) no Ru(1) O(11) C(101) C(103) . . . . 1.7(6) no Ru(1) O(11) C(101) C(102) . 3 3 3 177.8(3) no Ru(1) O(11) C(101) C(103) . 3 3 3 -1.7(6) no Ru(1) O(12) C(104) C(103) . . . . 7.0(6) no Ru(1) O(12) C(104) C(105) . . . . -172.9(3) no Ru(1) O(12) C(104) C(103) . 3 3 3 -7.0(6) no Ru(1) O(12) C(104) C(105) . 3 3 3 172.9(3) no Ru(2) P(2) C(206) C(207) . . . . 89.0(4) no Ru(2) P(2) C(206) C(211) . . . . -88.0(4) no Ru(2) P(2) C(212) C(213) . . . . 26.9(4) no Ru(2) P(2) C(212) C(217) . . . . -158.0(3) no Ru(2) P(2) C(206) C(207) . 7_556 7_556 7_556 -89.0(4) no Ru(2) P(2) C(206) C(211) . 7_556 7_556 7_556 88.0(4) no Ru(2) P(2) C(212) C(213) . 7_556 7_556 7_556 -26.9(4) no Ru(2) P(2) C(212) C(217) . 7_556 7_556 7_556 158.0(3) no Ru(2) O(21) C(201) C(202) . . . . 177.9(3) no Ru(2) O(21) C(201) C(203) . . . . -2.3(6) no Ru(2) O(21) C(201) C(202) . 7_556 7_556 7_556 -177.9(3) no Ru(2) O(21) C(201) C(203) . 7_556 7_556 7_556 2.3(6) no Ru(2) O(22) C(204) C(203) . . . . 4.7(6) no Ru(2) O(22) C(204) C(205) . . . . -176.9(3) no Ru(2) O(22) C(204) C(203) . 7_556 7_556 7_556 -4.7(6) no Ru(2) O(22) C(204) C(205) . 7_556 7_556 7_556 176.9(3) no P(1) Ru(1) P(1) C(106) . . 3 3 176.9(3) no P(1) Ru(1) P(1) C(112) . . 3 3 176.9(3) no P(1) Ru(1) P(1) C(118) . . 3 3 176.9(3) no P(1) Ru(1) O(11) C(101) . . . . 96.3(3) no P(1) Ru(1) O(11) C(101) . . 3 3 83.7(3) no P(1) Ru(1) O(12) C(104) . . . . -99.0(3) no P(1) Ru(1) O(12) C(104) . . 3 3 -81.0(3) no P(1) C(106) C(107) C(108) . . . . 177.1(3) no P(1) C(106) C(111) C(110) . . . . -175.5(3) no P(1) C(112) C(113) C(114) . . . . -177.1(3) no P(1) C(112) C(117) C(116) . . . . 177.7(3) no P(2) Ru(2) P(2) C(206) . . 7_556 7_556 177.7(3) no P(2) Ru(2) P(2) C(212) . . 7_556 7_556 177.7(3) no P(2) Ru(2) P(2) C(218) . . 7_556 7_556 177.7(3) no P(2) Ru(2) O(21) C(201) . . . . -86.4(3) no P(2) Ru(2) O(21) C(201) . . 7_556 7_556 -93.6(3) no P(2) Ru(2) O(22) C(204) . . . . 81.2(3) no P(2) Ru(2) O(22) C(204) . . 7_556 7_556 98.8(3) no P(2) C(206) C(207) C(208) . . . . -179.5(4) no P(2) C(206) C(211) C(210) . . . . 180.0(4) no P(2) C(212) C(213) C(214) . . . . 175.3(3) no P(2) C(212) C(217) C(216) . . . . -175.0(3) no O(11) Ru(1) P(1) C(106) . . . . 71.3(2) no O(11) Ru(1) P(1) C(112) . . . . -50.2(2) no O(11) Ru(1) P(1) C(118) . . . . -167.6(2) no O(11) Ru(1) P(1) C(106) . . 3 3 108.7(2) no O(11) Ru(1) P(1) C(112) . . 3 3 -129.8(2) no O(11) Ru(1) P(1) C(118) . . 3 3 -12.4(2) no O(11) Ru(1) O(11) C(101) . . 3 3 -12.4(2) no O(11) Ru(1) O(12) C(104) . . . . -10.3(3) no O(11) Ru(1) O(12) C(104) . . 3 3 -169.7(3) no O(11) C(101) C(103) C(104) . . . . -9.7(8) no O(12) Ru(1) P(1) C(106) . . . . 165.3(2) no O(12) Ru(1) P(1) C(112) . . . . 43.8(2) no O(12) Ru(1) P(1) C(118) . . . . -73.6(2) no O(12) Ru(1) P(1) C(106) . . 3 3 14.7(2) no O(12) Ru(1) P(1) C(112) . . 3 3 136.2(2) no O(12) Ru(1) P(1) C(118) . . 3 3 -106.4(2) no O(12) Ru(1) O(11) C(101) . . . . 6.1(3) no O(12) Ru(1) O(11) C(101) . . 3 3 173.9(3) no O(12) Ru(1) O(12) C(104) . . 3 3 173.9(3) no O(12) C(104) C(103) C(101) . . . . 4.5(8) no O(21) Ru(2) P(2) C(206) . . . . -130.8(2) no O(21) Ru(2) P(2) C(212) . . . . 110.7(2) no O(21) Ru(2) P(2) C(218) . . . . -13.1(2) no O(21) Ru(2) P(2) C(206) . . 7_556 7_556 -49.2(2) no O(21) Ru(2) P(2) C(212) . . 7_556 7_556 69.3(2) no O(21) Ru(2) P(2) C(218) . . 7_556 7_556 -166.9(2) no O(21) Ru(2) O(21) C(201) . . 7_556 7_556 -166.9(2) no O(21) Ru(2) O(22) C(204) . . . . -8.5(3) no O(21) Ru(2) O(22) C(204) . . 7_556 7_556 -171.5(3) no O(21) C(201) C(203) C(204) . . . . -5.2(8) no O(22) Ru(2) P(2) C(206) . . . . 135.7(2) no O(22) Ru(2) P(2) C(212) . . . . 17.3(2) no O(22) Ru(2) P(2) C(218) . . . . -106.6(2) no O(22) Ru(2) P(2) C(206) . . 7_556 7_556 44.3(2) no O(22) Ru(2) P(2) C(212) . . 7_556 7_556 162.7(2) no O(22) Ru(2) P(2) C(218) . . 7_556 7_556 -73.4(2) no O(22) Ru(2) O(21) C(201) . . . . 7.3(3) no O(22) Ru(2) O(21) C(201) . . 7_556 7_556 172.7(3) no O(22) Ru(2) O(22) C(204) . . 7_556 7_556 172.7(3) no O(22) C(204) C(203) C(201) . . . . 3.8(8) no C(101) C(103) C(104) C(105) . . . . -175.6(4) no C(102) C(101) C(103) C(104) . . . . 169.8(4) no C(106) P(1) C(112) C(113) . . . . -32.6(4) no C(106) P(1) C(112) C(117) . . . . 152.5(3) no C(106) C(107) C(108) C(109) . . . . -2.7(7) no C(106) C(111) C(110) C(109) . . . . -0.1(7) no C(107) C(106) P(1) C(112) . . . . 77.7(3) no C(107) C(106) P(1) C(118) . . . . -175.2(3) no C(107) C(106) C(111) C(110) . . . . -0.8(6) no C(107) C(108) C(109) C(110) . . . . 1.7(7) no C(108) C(107) C(106) C(111) . . . . 2.2(6) no C(108) C(109) C(110) C(111) . . . . -0.3(7) no C(111) C(106) P(1) C(112) . . . . -107.7(3) no C(111) C(106) P(1) C(118) . . . . -0.6(4) no C(112) C(113) C(114) C(115) . . . . 0.6(7) no C(112) C(117) C(116) C(115) . . . . -1.4(7) no C(113) C(112) P(1) C(118) . . . . -141.5(4) no C(113) C(112) C(117) C(116) . . . . 2.5(7) no C(113) C(114) C(115) C(116) . . . . 0.6(8) no C(114) C(113) C(112) C(117) . . . . -2.1(6) no C(114) C(115) C(116) C(117) . . . . -0.2(8) no C(117) C(112) P(1) C(118) . . . . 43.6(4) no C(201) C(203) C(204) C(205) . . . . -174.6(4) no C(202) C(201) C(203) C(204) . . . . 174.5(4) no C(206) P(2) C(212) C(213) . . . . -99.3(3) no C(206) P(2) C(212) C(217) . . . . 75.8(4) no C(206) C(207) C(208) C(209) . . . . 0.2(9) no C(206) C(211) C(210) C(209) . . . . -1.0(9) no C(207) C(206) P(2) C(212) . . . . -142.0(4) no C(207) C(206) P(2) C(218) . . . . -34.7(4) no C(207) C(206) C(211) C(210) . . . . 2.8(7) no C(207) C(208) C(209) C(210) . . . . 2(1) no C(208) C(207) C(206) C(211) . . . . -2.4(8) no C(208) C(209) C(210) C(211) . . . . -1(1) no C(211) C(206) P(2) C(212) . . . . 41.0(4) no C(211) C(206) P(2) C(218) . . . . 148.3(4) no C(212) C(213) C(214) C(215) . . . . -0.2(7) no C(212) C(217) C(216) C(215) . . . . 0.0(7) no C(213) C(212) P(2) C(218) . . . . 155.0(3) no C(213) C(212) C(217) C(216) . . . . 0.1(7) no C(213) C(214) C(215) C(216) . . . . 0.3(7) no C(214) C(213) C(212) C(217) . . . . 0.0(6) no C(214) C(215) C(216) C(217) . . . . -0.2(8) no C(217) C(212) P(2) C(218) . . . . -29.9(4) no #----------------------------------------------------------------------- #===END data_dm5b #----------------------------------------------------------------------- _audit_creation_date '1999-07-15' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_requested_journal ' Dalton ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Anthony C. Willis ' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address ' Martin A. Bennett ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Guandolina Chung ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' David C.R. Hockless ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Horst Neumann ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; dm5b ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 12.270(2) _cell_length_b 15.443(4) _cell_length_c 17.748(3) _cell_angle_alpha 90 _cell_angle_beta 90.46(1) _cell_angle_gamma 90 _cell_volume 3363(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.7 _cell_measurement_theta_max 18.1 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 699.73 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H40 O4 P2 Ru ' _chemical_formula_moiety 'C36 H40 O4 P2 Ru ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1448.00 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_correction_T_min 0.90 _exptl_special_details ; The scan width was (0.90+0.34tan\q)\% with an \w scan speed of 2\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.19 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 0 0 2 0 0 0 2 _diffrn_reflns_number 3262 _reflns_number_total 3103 _reflns_number_gt 2263 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01127 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01671 _diffrn_orient_matrix_UB_12 0.03275 _diffrn_orient_matrix_UB_13 0.04731 _diffrn_orient_matrix_UB_21 -0.06033 _diffrn_orient_matrix_UB_22 0.04146 _diffrn_orient_matrix_UB_23 -0.01190 _diffrn_orient_matrix_UB_31 -0.05219 _diffrn_orient_matrix_UB_32 -0.03744 _diffrn_orient_matrix_UB_33 0.02820 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 144 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 160 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.0000 0.25356(3) 0.2500 0.0282(1) 1.0 ST Uani d ? P(1) 0.00311(7) 0.15514(6) 0.34548(5) 0.0338(2) 1.000 . Uani d ? O(1) 0.1662(1) 0.2613(1) 0.2315(1) 0.0362(6) 1.000 . Uani d ? O(2) 0.0107(2) 0.3559(1) 0.3280(1) 0.0372(7) 1.000 . Uani d ? C(1) 0.2301(2) 0.3111(2) 0.2676(2) 0.038(1) 1.000 . Uani d ? C(2) 0.3484(3) 0.3036(3) 0.2449(2) 0.062(1) 1.000 . Uani d ? C(3) 0.2033(3) 0.3680(2) 0.3242(2) 0.047(1) 1.000 . Uani d ? C(4) 0.0992(3) 0.3888(2) 0.3501(2) 0.039(1) 1.000 . Uani d ? C(5) 0.0904(3) 0.4569(2) 0.4108(2) 0.067(1) 1.000 . Uani d ? C(6) 0.0016(2) 0.2087(2) 0.4378(2) 0.0343(9) 1.000 . Uani d ? C(7) 0.0913(3) 0.2104(2) 0.4859(2) 0.052(1) 1.000 . Uani d ? C(8) 0.0880(3) 0.2548(3) 0.5533(2) 0.062(1) 1.000 . Uani d ? C(9) -0.0043(3) 0.2983(2) 0.5740(2) 0.059(1) 1.000 . Uani d ? C(10) -0.0941(3) 0.2977(2) 0.5274(2) 0.053(1) 1.000 . Uani d ? C(11) -0.0903(2) 0.2539(2) 0.4596(2) 0.045(1) 1.000 . Uani d ? C(12) 0.1114(3) 0.0750(2) 0.3600(2) 0.038(1) 1.000 . Uani d ? C(13) 0.2124(3) 0.0869(2) 0.3280(2) 0.047(1) 1.000 . Uani d ? C(14) 0.2959(3) 0.0284(3) 0.3389(2) 0.058(1) 1.000 . Uani d ? C(15) 0.2798(3) -0.0426(2) 0.3834(2) 0.063(1) 1.000 . Uani d ? C(16) 0.1804(4) -0.0557(2) 0.4161(2) 0.071(2) 1.000 . Uani d ? C(17) 0.0972(3) 0.0022(2) 0.4044(2) 0.059(1) 1.000 . Uani d ? C(18) -0.1197(3) 0.0887(2) 0.3523(2) 0.051(1) 1.000 . Uani d ? H(2a) 0.3731 0.2461 0.2535 0.075 1.000 . Uiso c ? H(2b) 0.3552 0.3173 0.1929 0.075 1.000 . Uiso c ? H(2c) 0.3911 0.3428 0.2739 0.075 1.000 . Uiso c ? H(3) 0.2625 0.3965 0.3486 0.056 1.000 . Uiso c ? H(5a) 0.1611 0.4778 0.4233 0.080 1.000 . Uiso c ? H(5b) 0.0466 0.5034 0.3931 0.080 1.000 . Uiso c ? H(5c) 0.0580 0.4322 0.4543 0.080 1.000 . Uiso c ? H(7) 0.1559 0.1805 0.4723 0.062 1.000 . Uiso c ? H(8) 0.1502 0.2553 0.5856 0.074 1.000 . Uiso c ? H(9) -0.0062 0.3288 0.6204 0.071 1.000 . Uiso c ? H(10) -0.1586 0.3272 0.5417 0.063 1.000 . Uiso c ? H(11) -0.1523 0.2549 0.4271 0.054 1.000 . Uiso c ? H(13) 0.2247 0.1366 0.2976 0.057 1.000 . Uiso c ? H(14) 0.3644 0.0373 0.3156 0.069 1.000 . Uiso c ? H(15) 0.3374 -0.0827 0.3917 0.076 1.000 . Uiso c ? H(16) 0.1691 -0.1051 0.4470 0.085 1.000 . Uiso c ? H(17) 0.0285 -0.0079 0.4272 0.071 1.000 . Uiso c ? H(18a) -0.1812 0.1250 0.3593 0.061 1.000 . Uiso c ? H(18b) -0.1289 0.0563 0.3072 0.061 1.000 . Uiso c ? H(18c) -0.1128 0.0502 0.3938 0.061 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0257(2) 0.0294(2) 0.0296(2) 0.0000 -0.0014(1) 0.0000 P(1) 0.0345(5) 0.0344(5) 0.0324(5) 0.0003(4) -0.0010(4) 0.0012(4) O(1) 0.028(1) 0.041(1) 0.040(1) 0.000(1) 0.0014(9) 0.001(1) O(2) 0.039(1) 0.033(1) 0.040(1) 0.000(1) -0.001(1) -0.005(1) C(1) 0.027(2) 0.045(2) 0.042(2) -0.004(2) -0.003(2) 0.012(2) C(2) 0.033(2) 0.087(3) 0.066(3) -0.007(2) 0.003(2) 0.004(2) C(3) 0.037(2) 0.049(2) 0.053(2) -0.013(2) -0.008(2) -0.005(2) C(4) 0.048(2) 0.029(2) 0.041(2) -0.006(2) -0.006(2) 0.000(2) C(5) 0.067(3) 0.056(3) 0.077(3) -0.008(2) -0.005(2) -0.027(2) C(6) 0.038(2) 0.034(2) 0.031(2) -0.001(2) -0.001(1) 0.004(1) C(7) 0.047(2) 0.061(3) 0.047(2) 0.008(2) -0.003(2) -0.006(2) C(8) 0.068(3) 0.074(3) 0.042(2) 0.002(3) -0.016(2) -0.010(2) C(9) 0.085(3) 0.056(3) 0.037(2) 0.004(2) 0.004(2) -0.010(2) C(10) 0.059(3) 0.051(2) 0.048(2) 0.012(2) 0.015(2) -0.002(2) C(11) 0.041(2) 0.047(2) 0.046(2) 0.004(2) 0.000(2) 0.002(2) C(12) 0.049(2) 0.033(2) 0.032(2) 0.008(2) -0.004(2) 0.000(2) C(13) 0.048(2) 0.044(2) 0.050(2) 0.007(2) -0.006(2) 0.006(2) C(14) 0.049(2) 0.062(3) 0.062(3) 0.012(2) -0.007(2) 0.003(2) C(15) 0.075(3) 0.048(2) 0.066(3) 0.027(2) -0.013(2) 0.001(2) C(16) 0.098(4) 0.049(3) 0.067(3) 0.026(3) 0.010(3) 0.017(2) C(17) 0.070(3) 0.048(2) 0.060(3) 0.017(2) 0.016(2) 0.013(2) C(18) 0.054(2) 0.052(2) 0.047(2) -0.014(2) -0.006(2) 0.007(2) #----------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.000001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000000046 _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2263 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0220 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.860 _refine_ls_shift/su_max 0.0050 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.41 _refine_diff_density_max 0.35 #----------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) P(1) 2.2765(9) . . yes Ru(1) P(1) 2.2765(9) . 2 yes Ru(1) O(1) 2.072(2) . . yes Ru(1) O(1) 2.072(2) . 2 yes Ru(1) O(2) 2.104(2) . . yes Ru(1) O(2) 2.104(2) . 2 yes P(1) C(6) 1.835(3) . . yes P(1) C(12) 1.833(3) . . yes P(1) C(18) 1.828(3) . . yes O(1) C(1) 1.269(3) . . yes O(2) C(4) 1.260(4) . . yes C(1) C(2) 1.513(4) . . yes C(1) C(3) 1.378(4) . . yes C(2) H(2a) 0.95 . . no C(2) H(2b) 0.95 . . no C(2) H(2c) 0.95 . . no C(3) C(4) 1.399(4) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.509(4) . . yes C(5) H(5a) 0.95 . . no C(5) H(5b) 0.95 . . no C(5) H(5c) 0.95 . . no C(6) C(7) 1.389(4) . . yes C(6) C(11) 1.384(4) . . yes C(7) C(8) 1.380(4) . . yes C(7) H(7) 0.95 . . no C(8) C(9) 1.369(5) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.373(5) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.380(4) . . yes C(10) H(10) 0.95 . . no C(11) H(11) 0.95 . . no C(12) C(13) 1.380(4) . . yes C(12) C(17) 1.386(4) . . yes C(13) C(14) 1.379(4) . . yes C(13) H(13) 0.95 . . no C(14) C(15) 1.366(5) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.370(5) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.372(5) . . yes C(16) H(16) 0.95 . . no C(17) H(17) 0.95 . . no C(18) H(18a) 0.95 . . no C(18) H(18b) 0.95 . . no C(18) H(18c) 0.95 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Ru(1) P(1) 96.23(5) . . 2 yes P(1) Ru(1) O(1) 98.38(6) . . . yes P(1) Ru(1) O(1) 86.03(6) . . 2 yes P(1) Ru(1) O(2) 90.63(6) . . . yes P(1) Ru(1) O(2) 172.62(6) . . 2 yes P(1) Ru(1) O(1) 86.03(6) 2 . . yes P(1) Ru(1) O(1) 98.38(6) 2 . 2 yes P(1) Ru(1) O(2) 172.62(6) 2 . . yes P(1) Ru(1) O(2) 90.63(6) 2 . 2 yes O(1) Ru(1) O(1) 173.4(1) . . 2 yes O(1) Ru(1) O(2) 90.30(8) . . . yes O(1) Ru(1) O(2) 84.75(8) . . 2 yes O(1) Ru(1) O(2) 84.75(8) 2 . . yes O(1) Ru(1) O(2) 90.30(8) 2 . 2 yes O(2) Ru(1) O(2) 82.7(1) . . 2 yes Ru(1) P(1) C(6) 111.3(1) . . . yes Ru(1) P(1) C(12) 124.3(1) . . . yes Ru(1) P(1) C(18) 114.5(1) . . . yes C(6) P(1) C(12) 101.0(1) . . . yes C(6) P(1) C(18) 100.4(1) . . . yes C(12) P(1) C(18) 102.1(2) . . . yes Ru(1) O(1) C(1) 124.0(2) . . . yes Ru(1) O(2) C(4) 123.9(2) . . . yes O(1) C(1) C(2) 114.1(3) . . . yes O(1) C(1) C(3) 127.3(3) . . . yes C(2) C(1) C(3) 118.5(3) . . . yes C(1) C(2) H(2a) 109.5 . . . no C(1) C(2) H(2b) 109.5 . . . no C(1) C(2) H(2c) 109.5 . . . no H(2a) C(2) H(2b) 109.4 . . . no H(2a) C(2) H(2c) 109.4 . . . no H(2b) C(2) H(2c) 109.5 . . . no C(1) C(3) C(4) 127.6(3) . . . yes C(1) C(3) H(3) 116.2 . . . no C(4) C(3) H(3) 116.2 . . . no O(2) C(4) C(3) 126.3(3) . . . yes O(2) C(4) C(5) 115.9(3) . . . yes C(3) C(4) C(5) 117.7(3) . . . yes C(4) C(5) H(5a) 109.5 . . . no C(4) C(5) H(5b) 109.5 . . . no C(4) C(5) H(5c) 109.5 . . . no H(5a) C(5) H(5b) 109.5 . . . no H(5a) C(5) H(5c) 109.4 . . . no H(5b) C(5) H(5c) 109.4 . . . no P(1) C(6) C(7) 123.0(3) . . . yes P(1) C(6) C(11) 119.5(2) . . . yes C(7) C(6) C(11) 117.5(3) . . . yes C(6) C(7) C(8) 121.0(3) . . . yes C(6) C(7) H(7) 119.5 . . . no C(8) C(7) H(7) 119.5 . . . no C(7) C(8) C(9) 120.4(3) . . . yes C(7) C(8) H(8) 119.8 . . . no C(9) C(8) H(8) 119.8 . . . no C(8) C(9) C(10) 119.8(3) . . . yes C(8) C(9) H(9) 120.1 . . . no C(10) C(9) H(9) 120.1 . . . no C(9) C(10) C(11) 119.8(3) . . . yes C(9) C(10) H(10) 120.1 . . . no C(11) C(10) H(10) 120.1 . . . no C(6) C(11) C(10) 121.6(3) . . . yes C(6) C(11) H(11) 119.2 . . . no C(10) C(11) H(11) 119.2 . . . no P(1) C(12) C(13) 120.3(3) . . . yes P(1) C(12) C(17) 122.2(3) . . . yes C(13) C(12) C(17) 117.5(3) . . . yes C(12) C(13) C(14) 121.5(3) . . . yes C(12) C(13) H(13) 119.2 . . . no C(14) C(13) H(13) 119.2 . . . no C(13) C(14) C(15) 119.8(4) . . . yes C(13) C(14) H(14) 120.1 . . . no C(15) C(14) H(14) 120.1 . . . no C(14) C(15) C(16) 119.9(4) . . . yes C(14) C(15) H(15) 120.1 . . . no C(16) C(15) H(15) 120.1 . . . no C(15) C(16) C(17) 120.2(4) . . . yes C(15) C(16) H(16) 119.9 . . . no C(17) C(16) H(16) 119.9 . . . no C(12) C(17) C(16) 121.2(4) . . . yes C(12) C(17) H(17) 119.4 . . . no C(16) C(17) H(17) 119.4 . . . no P(1) C(18) H(18a) 109.5 . . . no P(1) C(18) H(18b) 109.5 . . . no P(1) C(18) H(18c) 109.5 . . . no H(18a) C(18) H(18b) 109.5 . . . no H(18a) C(18) H(18c) 109.5 . . . no H(18b) C(18) H(18c) 109.5 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(2) C(15) 3.391(4) . 5_455 no C(1) C(15) 3.507(5) . 6 no #----------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) P(1) C(6) C(7) . . . . -109.1(3) no Ru(1) P(1) C(6) C(11) . . . . 67.1(3) no Ru(1) P(1) C(12) C(13) . . . . 20.0(3) no Ru(1) P(1) C(12) C(17) . . . . -161.7(3) no Ru(1) P(1) C(6) C(7) . 2 2 2 -109.1(3) no Ru(1) P(1) C(6) C(11) . 2 2 2 67.1(3) no Ru(1) P(1) C(12) C(13) . 2 2 2 20.0(3) no Ru(1) P(1) C(12) C(17) . 2 2 2 -161.7(3) no Ru(1) O(1) C(1) C(2) . . . . 178.8(2) no Ru(1) O(1) C(1) C(3) . . . . 0.0(5) no Ru(1) O(1) C(1) C(2) . 2 2 2 178.8(2) no Ru(1) O(1) C(1) C(3) . 2 2 2 0.0(5) no Ru(1) O(2) C(4) C(3) . . . . 4.3(5) no Ru(1) O(2) C(4) C(5) . . . . -175.3(2) no Ru(1) O(2) C(4) C(3) . 2 2 2 4.3(5) no Ru(1) O(2) C(4) C(5) . 2 2 2 -175.3(2) no P(1) Ru(1) P(1) C(6) . . 2 2 -178.1(1) no P(1) Ru(1) P(1) C(12) . . 2 2 60.9(1) no P(1) Ru(1) P(1) C(18) . . 2 2 -65.2(1) no P(1) Ru(1) O(1) C(1) . . . . -85.9(2) no P(1) Ru(1) O(1) C(1) . . 2 2 178.4(2) no P(1) Ru(1) O(2) C(4) . . . . 91.5(2) no P(1) Ru(1) O(2) C(4) . . 2 2 -67.0(6) no P(1) C(6) C(7) C(8) . . . . 177.0(3) no P(1) C(6) C(11) C(10) . . . . -177.8(3) no P(1) C(12) C(13) C(14) . . . . 179.0(3) no P(1) C(12) C(17) C(16) . . . . -178.2(3) no O(1) Ru(1) P(1) C(6) . . . . 95.0(1) no O(1) Ru(1) P(1) C(12) . . . . -26.0(1) no O(1) Ru(1) P(1) C(18) . . . . -152.1(1) no O(1) Ru(1) P(1) C(6) . . 2 2 -80.1(1) no O(1) Ru(1) P(1) C(12) . . 2 2 158.9(1) no O(1) Ru(1) P(1) C(18) . . 2 2 32.8(1) no O(1) Ru(1) O(1) C(1) . . 2 2 46.0(2) no O(1) Ru(1) O(2) C(4) . . . . -6.9(3) no O(1) Ru(1) O(2) C(4) . . 2 2 177.5(3) no O(1) C(1) C(3) C(4) . . . . -5.8(6) no O(2) Ru(1) P(1) C(6) . . . . 4.6(1) no O(2) Ru(1) P(1) C(12) . . . . -116.4(2) no O(2) Ru(1) P(1) C(18) . . . . 117.5(1) no O(2) Ru(1) P(1) C(6) . . 2 2 -19.7(5) no O(2) Ru(1) P(1) C(12) . . 2 2 -140.7(5) no O(2) Ru(1) P(1) C(18) . . 2 2 93.2(5) no O(2) Ru(1) O(1) C(1) . . . . 4.8(2) no O(2) Ru(1) O(1) C(1) . . 2 2 87.4(2) no O(2) Ru(1) O(2) C(4) . . 2 2 -91.5(3) no O(2) C(4) C(3) C(1) . . . . 3.3(6) no C(1) C(3) C(4) C(5) . . . . -177.1(3) no C(2) C(1) C(3) C(4) . . . . 175.4(3) no C(6) P(1) C(12) C(13) . . . . -105.5(3) no C(6) P(1) C(12) C(17) . . . . 72.7(3) no C(6) C(7) C(8) C(9) . . . . -0.1(6) no C(6) C(11) C(10) C(9) . . . . 1.4(6) no C(7) C(6) P(1) C(12) . . . . 24.7(3) no C(7) C(6) P(1) C(18) . . . . 129.3(3) no C(7) C(6) C(11) C(10) . . . . -1.4(5) no C(7) C(8) C(9) C(10) . . . . 0.0(6) no C(8) C(7) C(6) C(11) . . . . 0.7(5) no C(8) C(9) C(10) C(11) . . . . -0.7(6) no C(11) C(6) P(1) C(12) . . . . -159.1(3) no C(11) C(6) P(1) C(18) . . . . -54.5(3) no C(12) C(13) C(14) C(15) . . . . -1.1(6) no C(12) C(17) C(16) C(15) . . . . -0.3(7) no C(13) C(12) P(1) C(18) . . . . 151.2(3) no C(13) C(12) C(17) C(16) . . . . 0.1(6) no C(13) C(14) C(15) C(16) . . . . 0.9(6) no C(14) C(13) C(12) C(17) . . . . 0.6(6) no C(14) C(15) C(16) C(17) . . . . -0.2(7) no C(17) C(12) P(1) C(18) . . . . -30.5(3) no #----------------------------------------------------------------------- #===END data_hxn20 #----------------------------------------------------------------------- _audit_creation_date '1998-09-29' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_requested_journal ' Dalton ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Anthony C. Willis ' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address ' Martin A. Bennett ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Guandolina Chung ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' David C.R. Hockless ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Horst Neumann ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; hxn20 ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 10.571(3) _cell_length_b 13.108(4) _cell_length_c 13.278(4) _cell_angle_alpha 61.84(2) _cell_angle_beta 69.52(2) _cell_angle_gamma 85.32(3) _cell_volume 1511.8(8) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.2 _cell_measurement_theta_max 21.9 #----------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'red/orange' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1237.95 _chemical_formula_analytical ? _chemical_formula_sum 'C62 H62 Cl4 O4 P4 Ru ' _chemical_formula_moiety 'C60 H58 O4 P4 Ru, 2(C H2 Cl2)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 638.00 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_correction_T_min 0.876 _exptl_special_details ; The scan width was (1.21+0.34tan\q)\% with an \w scan speed of 4\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -19.65 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 7361 _reflns_number_total 6985 _reflns_number_gt 5317 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.01562 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06321 _diffrn_orient_matrix_UB_12 -0.02032 _diffrn_orient_matrix_UB_13 0.08457 _diffrn_orient_matrix_UB_21 0.02275 _diffrn_orient_matrix_UB_22 0.07948 _diffrn_orient_matrix_UB_23 -0.01444 _diffrn_orient_matrix_UB_31 -0.07609 _diffrn_orient_matrix_UB_32 0.02890 _diffrn_orient_matrix_UB_33 -0.03139 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 62 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 62 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 4 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 1 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.0000 0.0000 0.0000 0.0377(1) 1.0 S Uani d ? Cl(1) -0.0710(2) 0.4507(1) -0.0971(1) 0.1426(6) 1.000 . Uani d ? Cl(2) -0.2983(2) 0.3346(2) 0.1224(2) 0.1389(7) 1.000 . Uani d ? P(1) 0.19949(9) 0.13124(7) -0.13438(8) 0.0417(2) 1.000 . Uani d ? P(2) 0.3050(1) 0.38368(8) -0.36533(9) 0.0493(3) 1.000 . Uani d ? O(1) 0.1177(2) -0.1312(2) 0.0666(2) 0.0491(7) 1.000 . Uani d ? O(2) -0.0117(2) 0.0542(2) 0.1257(2) 0.0502(7) 1.000 . Uani d ? C(1) 0.1455(4) -0.1541(3) 0.1604(4) 0.057(1) 1.000 . Uani d ? C(2) 0.2286(5) -0.2554(4) 0.1976(4) 0.084(2) 1.000 . Uani d ? C(3) 0.1062(4) -0.0972(4) 0.2301(3) 0.064(1) 1.000 . Uani d ? C(4) 0.0378(4) 0.0005(3) 0.2105(3) 0.059(1) 1.000 . Uani d ? C(5) 0.0151(6) 0.0530(5) 0.2939(5) 0.099(2) 1.000 . Uani d ? C(6) 0.3468(4) 0.0882(3) -0.2243(3) 0.047(1) 1.000 . Uani d ? C(7) 0.3315(4) -0.0040(3) -0.2449(4) 0.058(1) 1.000 . Uani d ? C(8) 0.4391(5) -0.0294(4) -0.3229(4) 0.073(2) 1.000 . Uani d ? C(9) 0.5625(5) 0.0351(4) -0.3796(4) 0.081(2) 1.000 . Uani d ? C(10) 0.5804(4) 0.1247(4) -0.3573(4) 0.071(1) 1.000 . Uani d ? C(11) 0.4738(4) 0.1508(3) -0.2807(3) 0.057(1) 1.000 . Uani d ? C(12) 0.2767(4) 0.1795(3) -0.0582(3) 0.047(1) 1.000 . Uani d ? C(13) 0.2480(4) 0.2821(3) -0.0502(4) 0.065(1) 1.000 . Uani d ? C(14) 0.3026(5) 0.3108(4) 0.0150(5) 0.082(2) 1.000 . Uani d ? C(15) 0.3859(5) 0.2396(4) 0.0713(4) 0.083(2) 1.000 . Uani d ? C(16) 0.4146(4) 0.1378(4) 0.0644(4) 0.070(1) 1.000 . Uani d ? C(17) 0.3611(4) 0.1091(3) 0.0011(3) 0.055(1) 1.000 . Uani d ? C(18) 0.1645(3) 0.2658(3) -0.2505(3) 0.047(1) 1.000 . Uani d ? C(19) 0.3251(4) 0.3811(3) -0.5068(3) 0.052(1) 1.000 . Uani d ? C(20) 0.3091(5) 0.2805(4) -0.5121(4) 0.076(2) 1.000 . Uani d ? C(21) 0.3352(6) 0.2844(5) -0.6249(5) 0.099(2) 1.000 . Uani d ? C(22) 0.3775(6) 0.3884(6) -0.7301(5) 0.106(2) 1.000 . Uani d ? C(23) 0.3969(5) 0.4872(5) -0.7263(4) 0.089(2) 1.000 . Uani d ? C(24) 0.3723(4) 0.4838(3) -0.6160(4) 0.066(1) 1.000 . Uani d ? C(25) 0.2086(4) 0.5101(3) -0.3826(3) 0.051(1) 1.000 . Uani d ? C(26) 0.0940(5) 0.5265(3) -0.4147(4) 0.068(1) 1.000 . Uani d ? C(27) 0.0212(5) 0.6191(4) -0.4199(4) 0.085(2) 1.000 . Uani d ? C(28) 0.0606(6) 0.6980(4) -0.3943(4) 0.086(2) 1.000 . Uani d ? C(29) 0.1725(6) 0.6839(4) -0.3614(4) 0.087(2) 1.000 . Uani d ? C(30) 0.2465(5) 0.5897(3) -0.3552(4) 0.069(1) 1.000 . Uani d ? C(31) -0.1347(6) 0.3293(5) 0.0397(5) 0.122(2) 1.000 . Uani d ? H(1) 0.3170 -0.2357 0.1372 0.101 1.000 . Uiso c ? H(2) 0.1862 -0.3212 0.2054 0.101 1.000 . Uiso c ? H(3) 0.2350 -0.2731 0.2737 0.101 1.000 . Uiso c ? H(4) 0.1296 -0.1302 0.3013 0.077 1.000 . Uiso c ? H(5) 0.0588 0.0118 0.3512 0.119 1.000 . Uiso c ? H(6) -0.0795 0.0482 0.3361 0.119 1.000 . Uiso c ? H(7) 0.0517 0.1323 0.2470 0.119 1.000 . Uiso c ? H(8) 0.2466 -0.0499 -0.2050 0.070 1.000 . Uiso c ? H(9) 0.4272 -0.0919 -0.3372 0.087 1.000 . Uiso c ? H(10) 0.6356 0.0183 -0.4342 0.097 1.000 . Uiso c ? H(11) 0.6665 0.1683 -0.3949 0.086 1.000 . Uiso c ? H(12) 0.4871 0.2127 -0.2660 0.068 1.000 . Uiso c ? H(13) 0.1909 0.3323 -0.0897 0.078 1.000 . Uiso c ? H(14) 0.2821 0.3802 0.0207 0.098 1.000 . Uiso c ? H(15) 0.4239 0.2602 0.1151 0.100 1.000 . Uiso c ? H(16) 0.4718 0.0880 0.1041 0.084 1.000 . Uiso c ? H(17) 0.3817 0.0389 -0.0031 0.066 1.000 . Uiso c ? H(18) 0.1285 0.2444 -0.2949 0.056 1.000 . Uiso c ? H(19) 0.0974 0.2986 -0.2082 0.056 1.000 . Uiso c ? H(20) 0.2804 0.2083 -0.4390 0.091 1.000 . Uiso c ? H(21) 0.3235 0.2152 -0.6284 0.119 1.000 . Uiso c ? H(22) 0.3934 0.3914 -0.8064 0.127 1.000 . Uiso c ? H(23) 0.4276 0.5588 -0.7998 0.107 1.000 . Uiso c ? H(24) 0.3880 0.5534 -0.6145 0.079 1.000 . Uiso c ? H(25) 0.0656 0.4725 -0.4334 0.081 1.000 . Uiso c ? H(26) -0.0572 0.6284 -0.4416 0.102 1.000 . Uiso c ? H(27) 0.0104 0.7626 -0.3992 0.103 1.000 . Uiso c ? H(28) 0.1997 0.7384 -0.3429 0.104 1.000 . Uiso c ? H(29) 0.3238 0.5800 -0.3320 0.083 1.000 . Uiso c ? H(30) -0.1320 0.2644 0.0256 0.147 1.000 . Uiso c ? H(31) -0.0793 0.3198 0.0860 0.147 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0419(2) 0.0335(2) 0.0382(2) 0.0096(2) -0.0183(2) -0.0154(2) Cl(1) 0.166(2) 0.097(1) 0.096(1) 0.034(1) 0.000(1) -0.0290(9) Cl(2) 0.103(1) 0.128(1) 0.157(2) -0.004(1) -0.004(1) -0.072(1) P(1) 0.0452(5) 0.0357(4) 0.0427(5) 0.0091(4) -0.0193(4) -0.0158(4) P(2) 0.0518(6) 0.0399(5) 0.0518(6) 0.0054(4) -0.0252(5) -0.0139(4) O(1) 0.047(1) 0.042(1) 0.051(1) 0.015(1) -0.022(1) -0.015(1) O(2) 0.057(2) 0.050(1) 0.049(1) 0.009(1) -0.020(1) -0.028(1) C(1) 0.048(2) 0.046(2) 0.059(2) 0.003(2) -0.025(2) -0.006(2) C(2) 0.075(3) 0.071(3) 0.090(3) 0.027(2) -0.050(3) -0.016(3) C(3) 0.071(3) 0.067(3) 0.049(2) 0.003(2) -0.037(2) -0.014(2) C(4) 0.063(3) 0.068(3) 0.046(2) -0.004(2) -0.019(2) -0.025(2) C(5) 0.134(5) 0.118(4) 0.080(3) 0.015(4) -0.054(3) -0.062(3) C(6) 0.050(2) 0.042(2) 0.042(2) 0.012(2) -0.017(2) -0.015(2) C(7) 0.058(2) 0.058(2) 0.060(2) 0.015(2) -0.023(2) -0.030(2) C(8) 0.079(3) 0.077(3) 0.073(3) 0.027(3) -0.025(3) -0.048(3) C(9) 0.068(3) 0.095(4) 0.067(3) 0.028(3) -0.012(2) -0.041(3) C(10) 0.049(2) 0.083(3) 0.057(3) 0.008(2) -0.010(2) -0.021(2) C(11) 0.051(2) 0.055(2) 0.053(2) 0.010(2) -0.017(2) -0.020(2) C(12) 0.050(2) 0.040(2) 0.045(2) 0.005(2) -0.018(2) -0.016(2) C(13) 0.078(3) 0.054(2) 0.073(3) 0.014(2) -0.033(2) -0.035(2) C(14) 0.108(4) 0.073(3) 0.098(4) 0.019(3) -0.049(3) -0.060(3) C(15) 0.104(4) 0.091(4) 0.079(3) 0.003(3) -0.046(3) -0.049(3) C(16) 0.074(3) 0.078(3) 0.071(3) 0.016(2) -0.045(2) -0.035(2) C(17) 0.059(2) 0.053(2) 0.059(2) 0.011(2) -0.029(2) -0.026(2) C(18) 0.046(2) 0.043(2) 0.046(2) 0.008(2) -0.020(2) -0.014(2) C(19) 0.049(2) 0.051(2) 0.052(2) 0.018(2) -0.021(2) -0.021(2) C(20) 0.106(4) 0.060(3) 0.070(3) 0.033(3) -0.044(3) -0.034(2) C(21) 0.147(5) 0.086(4) 0.096(4) 0.053(4) -0.059(4) -0.063(3) C(22) 0.131(5) 0.126(5) 0.068(3) 0.070(4) -0.038(3) -0.060(4) C(23) 0.092(4) 0.094(4) 0.051(3) 0.035(3) -0.013(2) -0.024(3) C(24) 0.061(3) 0.064(3) 0.056(2) 0.012(2) -0.015(2) -0.021(2) C(25) 0.064(2) 0.039(2) 0.044(2) 0.006(2) -0.020(2) -0.013(2) C(26) 0.084(3) 0.064(3) 0.077(3) 0.033(2) -0.049(3) -0.040(2) C(27) 0.099(4) 0.088(3) 0.085(3) 0.050(3) -0.049(3) -0.048(3) C(28) 0.119(5) 0.057(3) 0.072(3) 0.034(3) -0.029(3) -0.032(2) C(29) 0.120(5) 0.058(3) 0.079(3) 0.008(3) -0.022(3) -0.039(3) C(30) 0.085(3) 0.053(2) 0.067(3) 0.004(2) -0.026(2) -0.028(2) C(31) 0.125(5) 0.092(4) 0.092(4) 0.036(4) 0.001(4) -0.032(3) #----------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5317 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_all 0.0528 _refine_ls_wR_factor_ref 0.0507 _refine_ls_goodness_of_fit_all 2.092 _refine_ls_goodness_of_fit_ref 2.319 _refine_ls_shift/su_max 0.0140 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -0.74 _refine_diff_density_max 0.71 #----------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) P(1) 2.377(1) . . yes Ru(1) P(1) 2.377(1) . 2 yes Ru(1) O(1) 2.067(2) . . yes Ru(1) O(1) 2.067(2) . 2 yes Ru(1) O(2) 2.066(2) . . yes Ru(1) O(2) 2.066(2) . 2 yes Cl(1) C(31) 1.695(6) . . yes Cl(2) C(31) 1.711(6) . . yes P(1) C(6) 1.833(3) . . yes P(1) C(12) 1.832(4) . . yes P(1) C(18) 1.830(3) . . yes P(2) C(18) 1.866(4) . . yes P(2) C(19) 1.832(4) . . yes P(2) C(25) 1.835(4) . . yes O(1) C(1) 1.272(4) . . yes O(2) C(4) 1.282(4) . . yes C(1) C(2) 1.508(5) . . yes C(1) C(3) 1.385(5) . . yes C(2) H(1) 0.95 . . no C(2) H(2) 0.95 . . no C(2) H(3) 0.95 . . no C(3) C(4) 1.378(5) . . yes C(3) H(4) 0.95 . . no C(4) C(5) 1.504(5) . . yes C(5) H(5) 0.95 . . no C(5) H(6) 0.95 . . no C(5) H(7) 0.95 . . no C(6) C(7) 1.391(5) . . yes C(6) C(11) 1.390(5) . . yes C(7) C(8) 1.385(5) . . yes C(7) H(8) 0.95 . . no C(8) C(9) 1.370(6) . . yes C(8) H(9) 0.95 . . no C(9) C(10) 1.381(6) . . yes C(9) H(10) 0.95 . . no C(10) C(11) 1.372(5) . . yes C(10) H(11) 0.95 . . no C(11) H(12) 0.95 . . no C(12) C(13) 1.400(5) . . yes C(12) C(17) 1.392(5) . . yes C(13) C(14) 1.384(6) . . yes C(13) H(13) 0.95 . . no C(14) C(15) 1.369(6) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.382(6) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.355(5) . . yes C(16) H(16) 0.95 . . no C(17) H(17) 0.95 . . no C(18) H(18) 0.95 . . no C(18) H(19) 0.95 . . no C(19) C(20) 1.380(5) . . yes C(19) C(24) 1.388(5) . . yes C(20) C(21) 1.401(6) . . yes C(20) H(20) 0.95 . . no C(21) C(22) 1.369(7) . . yes C(21) H(21) 0.95 . . no C(22) C(23) 1.353(7) . . yes C(22) H(22) 0.95 . . no C(23) C(24) 1.374(6) . . yes C(23) H(23) 0.95 . . no C(24) H(24) 0.95 . . no C(25) C(26) 1.388(5) . . yes C(25) C(30) 1.382(5) . . yes C(26) C(27) 1.370(5) . . yes C(26) H(25) 0.95 . . no C(27) C(28) 1.365(7) . . yes C(27) H(26) 0.95 . . no C(28) C(29) 1.369(7) . . yes C(28) H(27) 0.95 . . no C(29) C(30) 1.391(6) . . yes C(29) H(28) 0.95 . . no C(30) H(29) 0.95 . . no C(31) H(30) 0.95 . . no C(31) H(31) 0.95 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Ru(1) P(1) 180.00 . . 2 yes P(1) Ru(1) O(1) 89.91(7) . . . yes P(1) Ru(1) O(1) 90.09(7) . . 2 yes P(1) Ru(1) O(2) 88.22(7) . . . yes P(1) Ru(1) O(2) 91.78(7) . . 2 yes P(1) Ru(1) O(1) 90.09(7) 2 . . yes P(1) Ru(1) O(1) 89.91(7) 2 . 2 yes P(1) Ru(1) O(2) 91.78(7) 2 . . yes P(1) Ru(1) O(2) 88.22(7) 2 . 2 yes O(1) Ru(1) O(1) 180.00 . . 2 yes O(1) Ru(1) O(2) 92.45(9) . . . yes O(1) Ru(1) O(2) 87.55(9) . . 2 yes O(1) Ru(1) O(2) 87.55(9) 2 . . yes O(1) Ru(1) O(2) 92.45(9) 2 . 2 yes O(2) Ru(1) O(2) 180.00 . . 2 yes Ru(1) P(1) C(6) 120.6(1) . . . yes Ru(1) P(1) C(12) 113.7(1) . . . yes Ru(1) P(1) C(18) 111.8(1) . . . yes C(6) P(1) C(12) 101.4(2) . . . yes C(6) P(1) C(18) 103.0(2) . . . yes C(12) P(1) C(18) 104.5(2) . . . yes C(18) P(2) C(19) 102.1(2) . . . yes C(18) P(2) C(25) 98.9(2) . . . yes C(19) P(2) C(25) 100.7(2) . . . yes Ru(1) O(1) C(1) 122.4(2) . . . yes Ru(1) O(2) C(4) 122.8(2) . . . yes O(1) C(1) C(2) 114.7(4) . . . yes O(1) C(1) C(3) 126.9(3) . . . yes C(2) C(1) C(3) 118.4(4) . . . yes C(1) C(2) H(1) 109.5 . . . no C(1) C(2) H(2) 109.5 . . . no C(1) C(2) H(3) 109.5 . . . no H(1) C(2) H(2) 109.5 . . . no H(1) C(2) H(3) 109.5 . . . no H(2) C(2) H(3) 109.5 . . . no C(1) C(3) C(4) 128.9(3) . . . yes C(1) C(3) H(4) 115.5 . . . no C(4) C(3) H(4) 115.5 . . . no O(2) C(4) C(3) 126.2(4) . . . yes O(2) C(4) C(5) 114.1(4) . . . yes C(3) C(4) C(5) 119.7(4) . . . yes C(4) C(5) H(5) 109.5 . . . no C(4) C(5) H(6) 109.5 . . . no C(4) C(5) H(7) 109.5 . . . no H(5) C(5) H(6) 109.5 . . . no H(5) C(5) H(7) 109.5 . . . no H(6) C(5) H(7) 109.5 . . . no P(1) C(6) C(7) 120.1(3) . . . yes P(1) C(6) C(11) 121.6(3) . . . yes C(7) C(6) C(11) 118.1(3) . . . yes C(6) C(7) C(8) 120.5(4) . . . yes C(6) C(7) H(8) 119.8 . . . no C(8) C(7) H(8) 119.8 . . . no C(7) C(8) C(9) 120.3(4) . . . yes C(7) C(8) H(9) 119.8 . . . no C(9) C(8) H(9) 119.8 . . . no C(8) C(9) C(10) 119.8(4) . . . yes C(8) C(9) H(10) 120.1 . . . no C(10) C(9) H(10) 120.1 . . . no C(9) C(10) C(11) 120.1(4) . . . yes C(9) C(10) H(11) 120.0 . . . no C(11) C(10) H(11) 120.0 . . . no C(6) C(11) C(10) 121.1(4) . . . yes C(6) C(11) H(12) 119.5 . . . no C(10) C(11) H(12) 119.5 . . . no P(1) C(12) C(13) 122.6(3) . . . yes P(1) C(12) C(17) 119.6(3) . . . yes C(13) C(12) C(17) 117.7(3) . . . yes C(12) C(13) C(14) 120.2(4) . . . yes C(12) C(13) H(13) 119.9 . . . no C(14) C(13) H(13) 119.9 . . . no C(13) C(14) C(15) 120.3(4) . . . yes C(13) C(14) H(14) 119.8 . . . no C(15) C(14) H(14) 119.8 . . . no C(14) C(15) C(16) 120.0(4) . . . yes C(14) C(15) H(15) 120.0 . . . no C(16) C(15) H(15) 120.0 . . . no C(15) C(16) C(17) 119.9(4) . . . yes C(15) C(16) H(16) 120.1 . . . no C(17) C(16) H(16) 120.1 . . . no C(12) C(17) C(16) 121.9(3) . . . yes C(12) C(17) H(17) 119.1 . . . no C(16) C(17) H(17) 119.1 . . . no P(1) C(18) P(2) 119.8(2) . . . yes P(1) C(18) H(18) 106.8 . . . no P(1) C(18) H(19) 106.8 . . . no P(2) C(18) H(18) 106.8 . . . no P(2) C(18) H(19) 106.8 . . . no H(18) C(18) H(19) 109.5 . . . no P(2) C(19) C(20) 123.5(3) . . . yes P(2) C(19) C(24) 118.1(3) . . . yes C(20) C(19) C(24) 118.0(4) . . . yes C(19) C(20) C(21) 120.2(4) . . . yes C(19) C(20) H(20) 119.9 . . . no C(21) C(20) H(20) 119.9 . . . no C(20) C(21) C(22) 119.7(5) . . . yes C(20) C(21) H(21) 120.2 . . . no C(22) C(21) H(21) 120.2 . . . no C(21) C(22) C(23) 120.6(5) . . . yes C(21) C(22) H(22) 119.7 . . . no C(23) C(22) H(22) 119.7 . . . no C(22) C(23) C(24) 120.0(4) . . . yes C(22) C(23) H(23) 120.0 . . . no C(24) C(23) H(23) 120.0 . . . no C(19) C(24) C(23) 121.4(4) . . . yes C(19) C(24) H(24) 119.3 . . . no C(23) C(24) H(24) 119.3 . . . no P(2) C(25) C(26) 123.3(3) . . . yes P(2) C(25) C(30) 118.6(3) . . . yes C(26) C(25) C(30) 118.0(4) . . . yes C(25) C(26) C(27) 121.1(4) . . . yes C(25) C(26) H(25) 119.5 . . . no C(27) C(26) H(25) 119.5 . . . no C(26) C(27) C(28) 120.5(5) . . . yes C(26) C(27) H(26) 119.8 . . . no C(28) C(27) H(26) 119.8 . . . no C(27) C(28) C(29) 119.9(4) . . . yes C(27) C(28) H(27) 120.0 . . . no C(29) C(28) H(27) 120.0 . . . no C(28) C(29) C(30) 119.9(4) . . . yes C(28) C(29) H(28) 120.0 . . . no C(30) C(29) H(28) 120.0 . . . no C(25) C(30) C(29) 120.6(4) . . . yes C(25) C(30) H(29) 119.7 . . . no C(29) C(30) H(29) 119.7 . . . no Cl(1) C(31) Cl(2) 113.3(3) . . . yes Cl(1) C(31) H(30) 108.5 . . . no Cl(1) C(31) H(31) 108.5 . . . no Cl(2) C(31) H(30) 108.5 . . . no Cl(2) C(31) H(31) 108.5 . . . no H(30) C(31) H(31) 109.5 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(27) 3.563(5) . . no Cl(1) C(28) 3.583(5) . . no Cl(2) C(22) 3.506(6) . 1_456 no O(1) C(31) 3.460(7) . 2 no O(2) C(31) 3.519(6) . . no C(2) C(23) 3.554(6) . 1_546 no C(10) C(29) 3.531(6) . 2_664 no P(1) P(2) 3.198(1) . . no #----------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) P(1) C(6) C(7) . . . . 19.9(3) no Ru(1) P(1) C(6) C(11) . . . . -164.7(2) no Ru(1) P(1) C(12) C(13) . . . . -93.9(3) no Ru(1) P(1) C(12) C(17) . . . . 82.1(3) no Ru(1) P(1) C(18) P(2) . . . . 179.0(1) no Ru(1) P(1) C(6) C(7) . 2 2 2 -19.9(3) no Ru(1) P(1) C(6) C(11) . 2 2 2 164.7(2) no Ru(1) P(1) C(12) C(13) . 2 2 2 93.9(3) no Ru(1) P(1) C(12) C(17) . 2 2 2 -82.1(3) no Ru(1) P(1) C(18) P(2) . 2 2 2 -179.0(1) no Ru(1) O(1) C(1) C(2) . . . . 178.0(2) no Ru(1) O(1) C(1) C(3) . . . . -1.1(5) no Ru(1) O(1) C(1) C(2) . 2 2 2 -178.0(2) no Ru(1) O(1) C(1) C(3) . 2 2 2 1.1(5) no Ru(1) O(2) C(4) C(3) . . . . 1.0(5) no Ru(1) O(2) C(4) C(5) . . . . -178.6(3) no Ru(1) O(2) C(4) C(3) . 2 2 2 -1.0(5) no Ru(1) O(2) C(4) C(5) . 2 2 2 178.6(3) no P(1) Ru(1) P(1) C(6) . . 2 2 178.6(3) no P(1) Ru(1) P(1) C(12) . . 2 2 178.6(3) no P(1) Ru(1) P(1) C(18) . . 2 2 178.6(3) no P(1) Ru(1) O(1) C(1) . . . . 93.0(3) no P(1) Ru(1) O(1) C(1) . . 2 2 87.0(3) no P(1) Ru(1) O(2) C(4) . . . . -94.6(3) no P(1) Ru(1) O(2) C(4) . . 2 2 -85.4(3) no P(1) C(6) C(7) C(8) . . . . 173.3(3) no P(1) C(6) C(11) C(10) . . . . -173.7(3) no P(1) C(12) C(13) C(14) . . . . 175.9(4) no P(1) C(12) C(17) C(16) . . . . -176.3(3) no P(1) C(18) P(2) C(19) . . . . 111.2(2) no P(1) C(18) P(2) C(25) . . . . -145.8(2) no P(2) C(18) P(1) C(6) . . . . -50.0(2) no P(2) C(18) P(1) C(12) . . . . 55.6(2) no P(2) C(19) C(20) C(21) . . . . -175.6(4) no P(2) C(19) C(24) C(23) . . . . 176.4(4) no P(2) C(25) C(26) C(27) . . . . 176.4(4) no P(2) C(25) C(30) C(29) . . . . -176.9(3) no O(1) Ru(1) P(1) C(6) . . . . 45.9(1) no O(1) Ru(1) P(1) C(12) . . . . -74.9(1) no O(1) Ru(1) P(1) C(18) . . . . 167.2(1) no O(1) Ru(1) P(1) C(6) . . 2 2 134.1(1) no O(1) Ru(1) P(1) C(12) . . 2 2 -105.1(1) no O(1) Ru(1) P(1) C(18) . . 2 2 12.8(1) no O(1) Ru(1) O(1) C(1) . . 2 2 12.8(1) no O(1) Ru(1) O(2) C(4) . . . . -4.7(3) no O(1) Ru(1) O(2) C(4) . . 2 2 -175.3(3) no O(1) C(1) C(3) C(4) . . . . -5.2(7) no O(2) Ru(1) P(1) C(6) . . . . 138.4(1) no O(2) Ru(1) P(1) C(12) . . . . 17.6(1) no O(2) Ru(1) P(1) C(18) . . . . -100.4(1) no O(2) Ru(1) P(1) C(6) . . 2 2 41.6(1) no O(2) Ru(1) P(1) C(12) . . 2 2 162.4(1) no O(2) Ru(1) P(1) C(18) . . 2 2 -79.6(1) no O(2) Ru(1) O(1) C(1) . . . . 4.7(3) no O(2) Ru(1) O(1) C(1) . . 2 2 175.3(3) no O(2) Ru(1) O(2) C(4) . . 2 2 175.3(3) no O(2) C(4) C(3) C(1) . . . . 5.2(7) no C(1) C(3) C(4) C(5) . . . . -175.2(4) no C(2) C(1) C(3) C(4) . . . . 175.8(4) no C(6) P(1) C(12) C(13) . . . . 135.1(3) no C(6) P(1) C(12) C(17) . . . . -48.9(3) no C(6) C(7) C(8) C(9) . . . . 0.9(6) no C(6) C(11) C(10) C(9) . . . . 0.1(6) no C(7) C(6) P(1) C(12) . . . . 146.5(3) no C(7) C(6) P(1) C(18) . . . . -105.5(3) no C(7) C(6) C(11) C(10) . . . . 1.8(5) no C(7) C(8) C(9) C(10) . . . . 1.1(7) no C(8) C(7) C(6) C(11) . . . . -2.3(5) no C(8) C(9) C(10) C(11) . . . . -1.6(7) no C(11) C(6) P(1) C(12) . . . . -38.1(3) no C(11) C(6) P(1) C(18) . . . . 69.9(3) no C(12) C(13) C(14) C(15) . . . . 0.6(7) no C(12) C(17) C(16) C(15) . . . . -0.1(7) no C(13) C(12) P(1) C(18) . . . . 28.2(4) no C(13) C(12) C(17) C(16) . . . . -0.1(6) no C(13) C(14) C(15) C(16) . . . . -0.8(8) no C(14) C(13) C(12) C(17) . . . . -0.1(6) no C(14) C(15) C(16) C(17) . . . . 0.6(8) no C(17) C(12) P(1) C(18) . . . . -155.8(3) no C(18) P(2) C(19) C(20) . . . . -35.6(4) no C(18) P(2) C(19) C(24) . . . . 151.2(3) no C(18) P(2) C(25) C(26) . . . . -55.7(4) no C(18) P(2) C(25) C(30) . . . . 120.2(3) no C(19) P(2) C(25) C(26) . . . . 48.5(4) no C(19) P(2) C(25) C(30) . . . . -135.6(3) no C(19) C(20) C(21) C(22) . . . . 0.5(8) no C(19) C(24) C(23) C(22) . . . . -1.2(8) no C(20) C(19) P(2) C(25) . . . . -137.3(4) no C(20) C(19) C(24) C(23) . . . . 2.9(6) no C(20) C(21) C(22) C(23) . . . . 1.3(9) no C(21) C(20) C(19) C(24) . . . . -2.5(7) no C(21) C(22) C(23) C(24) . . . . -0.9(9) no C(24) C(19) P(2) C(25) . . . . 49.6(3) no C(25) C(26) C(27) C(28) . . . . 0.4(8) no C(25) C(30) C(29) C(28) . . . . 0.4(7) no C(26) C(25) C(30) C(29) . . . . -0.8(6) no C(26) C(27) C(28) C(29) . . . . -0.9(8) no C(27) C(26) C(25) C(30) . . . . 0.4(6) no C(27) C(28) C(29) C(30) . . . . 0.5(8) no #----------------------------------------------------------------------- #===END data_hxn19 #----------------------------------------------------------------------- _audit_creation_date '1999-07-16' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_requested_journal ' Dalton' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Anthony C. Willis ' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address ' Martin A. Bennett ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Guandolina Chung ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' David C.R. Hockless ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Horst Neumann ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; hxn19 ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 10.774(2) _cell_length_b 11.362(3) _cell_length_c 13.463(3) _cell_angle_alpha 66.78(2) _cell_angle_beta 74.20(1) _cell_angle_gamma 86.95(2) _cell_volume 1454.8(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 15.8 _cell_measurement_theta_max 19.3 #----------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1153.01 _chemical_formula_analytical ? _chemical_formula_sum 'C61 H60 Cl2 O4 P4 Ru ' _chemical_formula_moiety 'C60 H58 O4 P4 Ru , (C H2 Cl2) ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 596.00 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_correction_T_min 0.881 _exptl_special_details ; The scan width was (1.31+0.34tan\q)\% with an \w scan speed of 4\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.11 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 7063 _reflns_number_total 6707 _reflns_number_gt 4527 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.01849 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00365 _diffrn_orient_matrix_UB_12 0.03715 _diffrn_orient_matrix_UB_13 -0.07989 _diffrn_orient_matrix_UB_21 -0.00984 _diffrn_orient_matrix_UB_22 0.08696 _diffrn_orient_matrix_UB_23 0.00233 _diffrn_orient_matrix_UB_31 0.09606 _diffrn_orient_matrix_UB_32 0.01623 _diffrn_orient_matrix_UB_33 -0.02594 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 61 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 60 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 2 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 1 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.0000 0.0000 0.0000 0.0449(1) 1.0 S Uani d ? Cl(1) 0.0185(4) 0.5572(3) -0.1131(2) 0.342(2) 1.000 . Uani d ? P(1) -0.19703(7) 0.00456(8) 0.12837(6) 0.0474(2) 1.000 . Uani d ? P(2) -0.30435(8) 0.02704(9) 0.36581(7) 0.0552(3) 1.000 . Uani d ? O(1) -0.0961(2) -0.0879(2) -0.0680(2) 0.0649(7) 1.000 . Uani d ? O(2) -0.0288(2) 0.1798(2) -0.1090(2) 0.0632(7) 1.000 . Uani d ? C(1) -0.1467(3) -0.0253(5) -0.1475(3) 0.078(1) 1.000 . Uani d ? C(2) -0.2149(4) -0.1080(6) -0.1837(4) 0.134(2) 1.000 . Uani d ? C(3) -0.1435(4) 0.1063(5) -0.2030(3) 0.088(2) 1.000 . Uani d ? C(4) -0.0886(3) 0.1985(4) -0.1826(3) 0.076(1) 1.000 . Uani d ? C(5) -0.0989(5) 0.3372(5) -0.2529(4) 0.129(2) 1.000 . Uani d ? C(6) -0.3120(3) -0.1349(3) 0.1927(2) 0.0538(9) 1.000 . Uani d ? C(7) -0.2707(3) -0.2490(4) 0.1857(3) 0.067(1) 1.000 . Uani d ? C(8) -0.3527(4) -0.3599(4) 0.2413(4) 0.092(2) 1.000 . Uani d ? C(9) -0.4757(5) -0.3541(5) 0.3033(4) 0.111(2) 1.000 . Uani d ? C(10) -0.5191(4) -0.2412(6) 0.3091(3) 0.102(2) 1.000 . Uani d ? C(11) -0.4385(3) -0.1311(4) 0.2535(3) 0.075(1) 1.000 . Uani d ? C(12) -0.2965(3) 0.1367(3) 0.0752(2) 0.056(1) 1.000 . Uani d ? C(13) -0.2795(4) 0.2543(4) 0.0778(3) 0.087(2) 1.000 . Uani d ? C(14) -0.3482(5) 0.3567(4) 0.0281(4) 0.109(2) 1.000 . Uani d ? C(15) -0.4351(5) 0.3422(5) -0.0243(4) 0.105(2) 1.000 . Uani d ? C(16) -0.4532(4) 0.2268(5) -0.0276(3) 0.091(2) 1.000 . Uani d ? C(17) -0.3840(3) 0.1247(4) 0.0200(3) 0.070(1) 1.000 . Uani d ? C(18) -0.1666(3) 0.0240(3) 0.2487(2) 0.0520(9) 1.000 . Uani d ? C(19) -0.2975(3) -0.1274(3) 0.4791(2) 0.0515(9) 1.000 . Uani d ? C(20) -0.2535(4) -0.2361(4) 0.4621(3) 0.072(1) 1.000 . Uani d ? C(21) -0.2594(4) -0.3522(4) 0.5514(4) 0.087(2) 1.000 . Uani d ? C(22) -0.3103(5) -0.3617(4) 0.6586(4) 0.094(2) 1.000 . Uani d ? C(23) -0.3559(4) -0.2563(4) 0.6779(3) 0.085(1) 1.000 . Uani d ? C(24) -0.3500(3) -0.1404(4) 0.5890(3) 0.067(1) 1.000 . Uani d ? C(25) -0.2302(3) 0.1373(3) 0.4059(2) 0.057(1) 1.000 . Uani d ? C(26) -0.1129(4) 0.1178(4) 0.4316(3) 0.079(1) 1.000 . Uani d ? C(27) -0.0562(4) 0.2071(4) 0.4534(4) 0.096(2) 1.000 . Uani d ? C(28) -0.1168(6) 0.3161(4) 0.4517(3) 0.095(2) 1.000 . Uani d ? C(29) -0.2328(6) 0.3371(4) 0.4277(4) 0.097(2) 1.000 . Uani d ? C(30) -0.2895(4) 0.2477(4) 0.4046(3) 0.077(1) 1.000 . Uani d ? C(31) -0.051(1) 0.5938(9) 0.009(1) 0.134(4) 0.500 . Uani d ? H(1) -0.2919 -0.1479 -0.1266 0.161 1.000 . Uiso c ? H(2) -0.2358 -0.0561 -0.2513 0.161 1.000 . Uiso c ? H(3) -0.1598 -0.1720 -0.1958 0.161 1.000 . Uiso c ? H(4) -0.1840 0.1370 -0.2622 0.105 1.000 . Uiso c ? H(5) -0.1320 0.3814 -0.2052 0.155 1.000 . Uiso c ? H(6) -0.1554 0.3436 -0.2978 0.155 1.000 . Uiso c ? H(7) -0.0158 0.3742 -0.3001 0.155 1.000 . Uiso c ? H(8) -0.1856 -0.2521 0.1426 0.081 1.000 . Uiso c ? H(9) -0.3240 -0.4385 0.2364 0.111 1.000 . Uiso c ? H(10) -0.5313 -0.4298 0.3427 0.133 1.000 . Uiso c ? H(11) -0.6048 -0.2386 0.3515 0.123 1.000 . Uiso c ? H(12) -0.4693 -0.0524 0.2566 0.089 1.000 . Uiso c ? H(13) -0.2198 0.2654 0.1144 0.104 1.000 . Uiso c ? H(14) -0.3349 0.4374 0.0304 0.131 1.000 . Uiso c ? H(15) -0.4824 0.4125 -0.0582 0.126 1.000 . Uiso c ? H(16) -0.5143 0.2163 -0.0632 0.110 1.000 . Uiso c ? H(17) -0.3961 0.0451 0.0151 0.084 1.000 . Uiso c ? H(18) -0.1169 0.1028 0.2197 0.062 1.000 . Uiso c ? H(19) -0.1167 -0.0450 0.2805 0.062 1.000 . Uiso c ? H(20) -0.2184 -0.2310 0.3876 0.086 1.000 . Uiso c ? H(21) -0.2278 -0.4258 0.5379 0.105 1.000 . Uiso c ? H(22) -0.3140 -0.4416 0.7200 0.112 1.000 . Uiso c ? H(23) -0.3919 -0.2629 0.7527 0.102 1.000 . Uiso c ? H(24) -0.3826 -0.0677 0.6035 0.081 1.000 . Uiso c ? H(25) -0.0709 0.0415 0.4342 0.095 1.000 . Uiso c ? H(26) 0.0251 0.1930 0.4696 0.115 1.000 . Uiso c ? H(27) -0.0778 0.3776 0.4672 0.113 1.000 . Uiso c ? H(28) -0.2749 0.4130 0.4268 0.116 1.000 . Uiso c ? H(29) -0.3704 0.2630 0.3877 0.093 1.000 . Uiso c ? H(30) -0.0070 0.6658 0.0064 0.161 0.500 . Uiso d ? H(31) -0.1402 0.6069 0.0199 0.161 0.500 . Uiso d ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0381(2) 0.0631(3) 0.0328(2) -0.0072(2) -0.0116(1) -0.0156(2) Cl(1) 0.401(5) 0.360(4) 0.263(3) -0.172(4) -0.026(3) -0.140(3) P(1) 0.0381(4) 0.0666(6) 0.0372(4) -0.0034(4) -0.0103(3) -0.0194(4) P(2) 0.0446(5) 0.0810(7) 0.0475(5) 0.0126(4) -0.0168(4) -0.0314(5) O(1) 0.055(1) 0.099(2) 0.046(1) -0.023(1) -0.010(1) -0.033(1) O(2) 0.057(1) 0.074(2) 0.043(1) 0.002(1) -0.013(1) -0.007(1) C(1) 0.040(2) 0.153(4) 0.055(2) -0.016(2) -0.008(2) -0.056(3) C(2) 0.085(3) 0.253(6) 0.106(3) -0.041(4) -0.027(3) -0.107(4) C(3) 0.062(2) 0.160(5) 0.052(2) 0.026(3) -0.031(2) -0.045(3) C(4) 0.064(2) 0.109(3) 0.039(2) 0.026(2) -0.014(2) -0.015(2) C(5) 0.151(5) 0.138(4) 0.069(3) 0.064(4) -0.041(3) -0.011(3) C(6) 0.043(2) 0.073(2) 0.041(2) -0.012(2) -0.012(1) -0.015(2) C(7) 0.061(2) 0.074(3) 0.059(2) -0.015(2) -0.021(2) -0.014(2) C(8) 0.099(3) 0.077(3) 0.090(3) -0.029(3) -0.041(3) -0.010(2) C(9) 0.101(4) 0.121(4) 0.081(3) -0.064(3) -0.029(3) 0.002(3) C(10) 0.061(3) 0.158(5) 0.063(3) -0.046(3) -0.005(2) -0.021(3) C(11) 0.049(2) 0.115(3) 0.055(2) -0.017(2) -0.010(2) -0.030(2) C(12) 0.048(2) 0.076(2) 0.043(2) 0.006(2) -0.011(1) -0.022(2) C(13) 0.091(3) 0.086(3) 0.097(3) 0.018(2) -0.043(3) -0.040(3) C(14) 0.124(4) 0.087(3) 0.125(4) 0.034(3) -0.048(3) -0.045(3) C(15) 0.099(4) 0.113(4) 0.091(3) 0.050(3) -0.035(3) -0.028(3) C(16) 0.070(3) 0.130(4) 0.072(3) 0.033(3) -0.033(2) -0.032(3) C(17) 0.063(2) 0.094(3) 0.063(2) 0.015(2) -0.028(2) -0.034(2) C(18) 0.044(2) 0.074(2) 0.040(2) 0.000(2) -0.011(1) -0.024(2) C(19) 0.043(2) 0.070(2) 0.046(2) -0.004(1) -0.013(1) -0.026(2) C(20) 0.084(3) 0.077(3) 0.060(2) 0.002(2) -0.022(2) -0.031(2) C(21) 0.118(4) 0.066(3) 0.087(3) 0.000(2) -0.042(3) -0.030(2) C(22) 0.121(4) 0.079(3) 0.070(3) -0.034(3) -0.034(3) -0.008(2) C(23) 0.092(3) 0.104(3) 0.048(2) -0.032(3) -0.006(2) -0.022(2) C(24) 0.063(2) 0.086(3) 0.050(2) -0.009(2) -0.006(2) -0.030(2) C(25) 0.067(2) 0.063(2) 0.041(2) 0.009(2) -0.016(2) -0.021(2) C(26) 0.089(3) 0.068(3) 0.106(3) 0.016(2) -0.055(2) -0.043(2) C(27) 0.114(4) 0.083(3) 0.110(4) -0.003(3) -0.058(3) -0.039(3) C(28) 0.152(5) 0.068(3) 0.065(3) -0.015(3) -0.031(3) -0.024(2) C(29) 0.148(5) 0.063(3) 0.075(3) 0.021(3) -0.019(3) -0.031(2) C(30) 0.091(3) 0.078(3) 0.066(2) 0.025(2) -0.023(2) -0.034(2) C(31) 0.18(1) 0.071(6) 0.125(8) -0.023(7) 0.040(8) -0.067(6) #----------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4527 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_all 0.0411 _refine_ls_wR_factor_ref 0.0371 _refine_ls_goodness_of_fit_all 1.459 _refine_ls_goodness_of_fit_ref 1.620 _refine_ls_shift/su_max 0.0300 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -0.41 _refine_diff_density_max 0.65 #----------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) P(1) 2.3575(8) . . yes Ru(1) P(1) 2.3575(8) . 2 yes Ru(1) O(1) 2.062(2) . . yes Ru(1) O(1) 2.062(2) . 2 yes Ru(1) O(2) 2.059(2) . . yes Ru(1) O(2) 2.059(2) . 2 yes Cl(1) C(31) 1.806(9) . . yes Cl(1) C(31) 1.83(1) . 2_565 yes P(1) C(6) 1.827(3) . . yes P(1) C(12) 1.821(3) . . yes P(1) C(18) 1.833(3) . . yes P(2) C(18) 1.858(3) . . yes P(2) C(19) 1.830(3) . . yes P(2) C(25) 1.837(3) . . yes O(1) C(1) 1.275(4) . . yes O(2) C(4) 1.268(4) . . yes C(1) C(2) 1.513(5) . . yes C(1) C(3) 1.380(6) . . yes C(2) H(1) 0.95 . . no C(2) H(2) 0.95 . . no C(2) H(3) 0.95 . . no C(3) C(4) 1.379(6) . . yes C(3) H(4) 0.95 . . no C(4) C(5) 1.501(5) . . yes C(5) H(5) 0.95 . . no C(5) H(6) 0.95 . . no C(5) H(7) 0.95 . . no C(6) C(7) 1.378(4) . . yes C(6) C(11) 1.395(4) . . yes C(7) C(8) 1.394(5) . . yes C(7) H(8) 0.95 . . no C(8) C(9) 1.374(7) . . yes C(8) H(9) 0.95 . . no C(9) C(10) 1.365(7) . . yes C(9) H(10) 0.95 . . no C(10) C(11) 1.380(5) . . yes C(10) H(11) 0.95 . . no C(11) H(12) 0.95 . . no C(12) C(13) 1.373(5) . . yes C(12) C(17) 1.391(4) . . yes C(13) C(14) 1.383(5) . . yes C(13) H(13) 0.95 . . no C(14) C(15) 1.367(6) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.355(6) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.377(5) . . yes C(16) H(16) 0.95 . . no C(17) H(17) 0.95 . . no C(18) H(18) 0.95 . . no C(18) H(19) 0.95 . . no C(19) C(20) 1.380(4) . . yes C(19) C(24) 1.383(4) . . yes C(20) C(21) 1.380(5) . . yes C(20) H(20) 0.95 . . no C(21) C(22) 1.360(5) . . yes C(21) H(21) 0.95 . . no C(22) C(23) 1.362(6) . . yes C(22) H(22) 0.95 . . no C(23) C(24) 1.377(5) . . yes C(23) H(23) 0.95 . . no C(24) H(24) 0.95 . . no C(25) C(26) 1.382(4) . . yes C(25) C(30) 1.373(4) . . yes C(26) C(27) 1.373(5) . . yes C(26) H(25) 0.95 . . no C(27) C(28) 1.364(6) . . yes C(27) H(26) 0.95 . . no C(28) C(29) 1.360(6) . . yes C(28) H(27) 0.95 . . no C(29) C(30) 1.385(6) . . yes C(29) H(28) 0.95 . . no C(30) H(29) 0.95 . . no C(31) H(30) 0.95 . . no C(31) H(31) 0.95 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Ru(1) P(1) 180.00 . . 2 yes P(1) Ru(1) O(1) 89.79(6) . . . yes P(1) Ru(1) O(1) 90.21(6) . . 2 yes P(1) Ru(1) O(2) 89.27(6) . . . yes P(1) Ru(1) O(2) 90.73(6) . . 2 yes P(1) Ru(1) O(1) 90.21(6) 2 . . yes P(1) Ru(1) O(1) 89.79(6) 2 . 2 yes P(1) Ru(1) O(2) 90.73(6) 2 . . yes P(1) Ru(1) O(2) 89.27(6) 2 . 2 yes O(1) Ru(1) O(1) 180.00 . . 2 yes O(1) Ru(1) O(2) 91.88(9) . . . yes O(1) Ru(1) O(2) 88.12(9) . . 2 yes O(1) Ru(1) O(2) 88.12(9) 2 . . yes O(1) Ru(1) O(2) 91.88(9) 2 . 2 yes O(2) Ru(1) O(2) 180.00 . . 2 yes C(31) Cl(1) C(31) 83.0(5) . . 2_565 yes Ru(1) P(1) C(6) 118.8(1) . . . yes Ru(1) P(1) C(12) 115.7(1) . . . yes Ru(1) P(1) C(18) 110.2(1) . . . yes C(6) P(1) C(12) 102.7(1) . . . yes C(6) P(1) C(18) 103.8(1) . . . yes C(12) P(1) C(18) 104.0(1) . . . yes C(18) P(2) C(19) 102.2(1) . . . yes C(18) P(2) C(25) 98.8(1) . . . yes C(19) P(2) C(25) 101.4(1) . . . yes Ru(1) O(1) C(1) 122.9(3) . . . yes Ru(1) O(2) C(4) 123.3(3) . . . yes O(1) C(1) C(2) 114.5(4) . . . yes O(1) C(1) C(3) 127.1(3) . . . yes C(2) C(1) C(3) 118.4(4) . . . yes C(1) C(2) H(1) 109.5 . . . no C(1) C(2) H(2) 109.5 . . . no C(1) C(2) H(3) 109.5 . . . no H(1) C(2) H(2) 109.5 . . . no H(1) C(2) H(3) 109.5 . . . no H(2) C(2) H(3) 109.5 . . . no C(1) C(3) C(4) 127.8(3) . . . yes C(1) C(3) H(4) 116.1 . . . no C(4) C(3) H(4) 116.1 . . . no O(2) C(4) C(3) 127.0(4) . . . yes O(2) C(4) C(5) 114.5(4) . . . yes C(3) C(4) C(5) 118.5(4) . . . yes C(4) C(5) H(5) 109.5 . . . no C(4) C(5) H(6) 109.5 . . . no C(4) C(5) H(7) 109.5 . . . no H(5) C(5) H(6) 109.5 . . . no H(5) C(5) H(7) 109.5 . . . no H(6) C(5) H(7) 109.5 . . . no P(1) C(6) C(7) 119.1(2) . . . yes P(1) C(6) C(11) 121.9(3) . . . yes C(7) C(6) C(11) 118.9(3) . . . yes C(6) C(7) C(8) 120.6(4) . . . yes C(6) C(7) H(8) 119.7 . . . no C(8) C(7) H(8) 119.7 . . . no C(7) C(8) C(9) 119.1(4) . . . yes C(7) C(8) H(9) 120.5 . . . no C(9) C(8) H(9) 120.5 . . . no C(8) C(9) C(10) 121.1(4) . . . yes C(8) C(9) H(10) 119.5 . . . no C(10) C(9) H(10) 119.5 . . . no C(9) C(10) C(11) 120.0(4) . . . yes C(9) C(10) H(11) 120.0 . . . no C(11) C(10) H(11) 120.0 . . . no C(6) C(11) C(10) 120.3(4) . . . yes C(6) C(11) H(12) 119.9 . . . no C(10) C(11) H(12) 119.9 . . . no P(1) C(12) C(13) 121.9(3) . . . yes P(1) C(12) C(17) 120.1(3) . . . yes C(13) C(12) C(17) 117.7(3) . . . yes C(12) C(13) C(14) 121.0(4) . . . yes C(12) C(13) H(13) 119.5 . . . no C(14) C(13) H(13) 119.5 . . . no C(13) C(14) C(15) 120.3(5) . . . yes C(13) C(14) H(14) 119.8 . . . no C(15) C(14) H(14) 119.8 . . . no C(14) C(15) C(16) 119.5(4) . . . yes C(14) C(15) H(15) 120.2 . . . no C(16) C(15) H(15) 120.2 . . . no C(15) C(16) C(17) 120.7(4) . . . yes C(15) C(16) H(16) 119.6 . . . no C(17) C(16) H(16) 119.6 . . . no C(12) C(17) C(16) 120.7(4) . . . yes C(12) C(17) H(17) 119.7 . . . no C(16) C(17) H(17) 119.7 . . . no P(1) C(18) P(2) 120.0(2) . . . yes P(1) C(18) H(18) 106.8 . . . no P(1) C(18) H(19) 106.8 . . . no P(2) C(18) H(18) 106.8 . . . no P(2) C(18) H(19) 106.8 . . . no H(18) C(18) H(19) 109.5 . . . no P(2) C(19) C(20) 124.0(2) . . . yes P(2) C(19) C(24) 118.5(3) . . . yes C(20) C(19) C(24) 117.2(3) . . . yes C(19) C(20) C(21) 121.3(3) . . . yes C(19) C(20) H(20) 119.4 . . . no C(21) C(20) H(20) 119.4 . . . no C(20) C(21) C(22) 120.2(4) . . . yes C(20) C(21) H(21) 119.9 . . . no C(22) C(21) H(21) 119.9 . . . no C(21) C(22) C(23) 119.8(4) . . . yes C(21) C(22) H(22) 120.1 . . . no C(23) C(22) H(22) 120.1 . . . no C(22) C(23) C(24) 120.1(4) . . . yes C(22) C(23) H(23) 119.9 . . . no C(24) C(23) H(23) 119.9 . . . no C(19) C(24) C(23) 121.4(4) . . . yes C(19) C(24) H(24) 119.3 . . . no C(23) C(24) H(24) 119.3 . . . no P(2) C(25) C(26) 122.9(3) . . . yes P(2) C(25) C(30) 119.0(3) . . . yes C(26) C(25) C(30) 118.1(3) . . . yes C(25) C(26) C(27) 121.1(4) . . . yes C(25) C(26) H(25) 119.5 . . . no C(27) C(26) H(25) 119.5 . . . no C(26) C(27) C(28) 119.9(4) . . . yes C(26) C(27) H(26) 120.0 . . . no C(28) C(27) H(26) 120.0 . . . no C(27) C(28) C(29) 120.2(4) . . . yes C(27) C(28) H(27) 119.9 . . . no C(29) C(28) H(27) 119.9 . . . no C(28) C(29) C(30) 120.0(4) . . . yes C(28) C(29) H(28) 120.0 . . . no C(30) C(29) H(28) 120.0 . . . no C(25) C(30) C(29) 120.8(4) . . . yes C(25) C(30) H(29) 119.6 . . . no C(29) C(30) H(29) 119.6 . . . no Cl(1) C(31) Cl(1) 97.0(5) . . 2_565 yes Cl(1) C(31) H(30) 112.5 . . . no Cl(1) C(31) H(31) 112.5 . . . no Cl(1) C(31) H(30) 112.5 2_565 . . no Cl(1) C(31) H(31) 112.5 2_565 . . no H(30) C(31) H(31) 109.5 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(31) 3.40(1) . 1_545 no O(2) C(31) 3.57(1) . 2_565 no C(2) C(23) 3.594(5) . 1_554 no #----------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) P(1) C(6) C(7) . . . . 14.7(3) no Ru(1) P(1) C(6) C(11) . . . . -168.6(2) no Ru(1) P(1) C(12) C(13) . . . . -86.0(3) no Ru(1) P(1) C(12) C(17) . . . . 87.5(3) no Ru(1) P(1) C(18) P(2) . . . . -178.6(1) no Ru(1) P(1) C(6) C(7) . 2 2 2 -14.7(3) no Ru(1) P(1) C(6) C(11) . 2 2 2 168.6(2) no Ru(1) P(1) C(12) C(13) . 2 2 2 86.0(3) no Ru(1) P(1) C(12) C(17) . 2 2 2 -87.5(3) no Ru(1) P(1) C(18) P(2) . 2 2 2 178.6(1) no Ru(1) O(1) C(1) C(2) . . . . -178.9(2) no Ru(1) O(1) C(1) C(3) . . . . 2.2(5) no Ru(1) O(1) C(1) C(2) . 2 2 2 178.9(2) no Ru(1) O(1) C(1) C(3) . 2 2 2 -2.2(5) no Ru(1) O(2) C(4) C(3) . . . . 0.1(5) no Ru(1) O(2) C(4) C(5) . . . . 179.8(2) no Ru(1) O(2) C(4) C(3) . 2 2 2 -0.1(5) no Ru(1) O(2) C(4) C(5) . 2 2 2 -179.8(2) no Cl(1) C(31) Cl(1) C(31) . . 2_565 2_565 0.0000 no Cl(1) C(31) Cl(1) C(31) . 2_565 2_565 . 0.0000 no P(1) Ru(1) P(1) C(6) . . 2 2 0.0000 no P(1) Ru(1) P(1) C(12) . . 2 2 0.0000 no P(1) Ru(1) P(1) C(18) . . 2 2 0.0000 no P(1) Ru(1) O(1) C(1) . . . . 88.2(2) no P(1) Ru(1) O(1) C(1) . . 2 2 91.8(2) no P(1) Ru(1) O(2) C(4) . . . . -89.7(2) no P(1) Ru(1) O(2) C(4) . . 2 2 -90.3(2) no P(1) C(6) C(7) C(8) . . . . 174.9(3) no P(1) C(6) C(11) C(10) . . . . -174.3(3) no P(1) C(12) C(13) C(14) . . . . 174.2(3) no P(1) C(12) C(17) C(16) . . . . -175.4(3) no P(1) C(18) P(2) C(19) . . . . 108.6(2) no P(1) C(18) P(2) C(25) . . . . -147.7(2) no P(2) C(18) P(1) C(6) . . . . -50.3(2) no P(2) C(18) P(1) C(12) . . . . 56.8(2) no P(2) C(19) C(20) C(21) . . . . -175.3(3) no P(2) C(19) C(24) C(23) . . . . 175.5(3) no P(2) C(25) C(26) C(27) . . . . 175.3(3) no P(2) C(25) C(30) C(29) . . . . -176.1(3) no O(1) Ru(1) P(1) C(6) . . . . 40.4(1) no O(1) Ru(1) P(1) C(12) . . . . -82.5(1) no O(1) Ru(1) P(1) C(18) . . . . 160.0(1) no O(1) Ru(1) P(1) C(6) . . 2 2 139.6(1) no O(1) Ru(1) P(1) C(12) . . 2 2 -97.5(1) no O(1) Ru(1) P(1) C(18) . . 2 2 20.0(1) no O(1) Ru(1) O(1) C(1) . . 2 2 20.0(1) no O(1) Ru(1) O(2) C(4) . . . . 0.1(2) no O(1) Ru(1) O(2) C(4) . . 2 2 179.9(2) no O(1) C(1) C(3) C(4) . . . . -2.1(7) no O(2) Ru(1) P(1) C(6) . . . . 132.3(1) no O(2) Ru(1) P(1) C(12) . . . . 9.4(1) no O(2) Ru(1) P(1) C(18) . . . . -108.1(1) no O(2) Ru(1) P(1) C(6) . . 2 2 47.7(1) no O(2) Ru(1) P(1) C(12) . . 2 2 170.6(1) no O(2) Ru(1) P(1) C(18) . . 2 2 -71.9(1) no O(2) Ru(1) O(1) C(1) . . . . -1.1(2) no O(2) Ru(1) O(1) C(1) . . 2 2 -178.9(2) no O(2) Ru(1) O(2) C(4) . . 2 2 -178.9(2) no O(2) C(4) C(3) C(1) . . . . 0.8(7) no C(1) C(3) C(4) C(5) . . . . -179.0(4) no C(2) C(1) C(3) C(4) . . . . 179.0(4) no C(6) P(1) C(12) C(13) . . . . 143.0(3) no C(6) P(1) C(12) C(17) . . . . -43.5(3) no C(6) C(7) C(8) C(9) . . . . 0.1(6) no C(6) C(11) C(10) C(9) . . . . -1.0(6) no C(7) C(6) P(1) C(12) . . . . 143.8(2) no C(7) C(6) P(1) C(18) . . . . -108.1(3) no C(7) C(6) C(11) C(10) . . . . 2.4(5) no C(7) C(8) C(9) C(10) . . . . 1.4(7) no C(8) C(7) C(6) C(11) . . . . -1.9(5) no C(8) C(9) C(10) C(11) . . . . -0.9(7) no C(11) C(6) P(1) C(12) . . . . -39.5(3) no C(11) C(6) P(1) C(18) . . . . 68.6(3) no C(12) C(13) C(14) C(15) . . . . 0.3(8) no C(12) C(17) C(16) C(15) . . . . 1.7(6) no C(13) C(12) P(1) C(18) . . . . 35.0(3) no C(13) C(12) C(17) C(16) . . . . -1.6(5) no C(13) C(14) C(15) C(16) . . . . -0.2(8) no C(14) C(13) C(12) C(17) . . . . 0.6(6) no C(14) C(15) C(16) C(17) . . . . -0.8(7) no C(17) C(12) P(1) C(18) . . . . -151.5(3) no C(18) P(2) C(19) C(20) . . . . -30.7(3) no C(18) P(2) C(19) C(24) . . . . 155.4(2) no C(18) P(2) C(25) C(26) . . . . -53.7(3) no C(18) P(2) C(25) C(30) . . . . 122.6(3) no C(19) P(2) C(25) C(26) . . . . 50.7(3) no C(19) P(2) C(25) C(30) . . . . -133.0(3) no C(19) C(20) C(21) C(22) . . . . 0.6(6) no C(19) C(24) C(23) C(22) . . . . -0.4(6) no C(20) C(19) P(2) C(25) . . . . -132.4(3) no C(20) C(19) C(24) C(23) . . . . 1.1(5) no C(20) C(21) C(22) C(23) . . . . 0.2(7) no C(21) C(20) C(19) C(24) . . . . -1.2(5) no C(21) C(22) C(23) C(24) . . . . -0.3(7) no C(24) C(19) P(2) C(25) . . . . 53.7(3) no C(25) C(26) C(27) C(28) . . . . 1.1(7) no C(25) C(30) C(29) C(28) . . . . 0.2(6) no C(26) C(25) C(30) C(29) . . . . 0.4(6) no C(26) C(27) C(28) C(29) . . . . -0.4(7) no C(27) C(26) C(25) C(30) . . . . -1.0(6) no C(27) C(28) C(29) C(30) . . . . -0.2(7) no C(31) Cl(1) C(31) Cl(1) . . 2_565 2_565 0.0000 no C(31) Cl(1) C(31) Cl(1) . 2_565 2_565 . 0.0000 no #----------------------------------------------------------------------- #===END