Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'M. I. Bruce' 'Benjamin G. Ellis' 'Maryka Gaudio' 'Claude Lapinte' 'Giovanni Melino' 'Frederic Paul' 'Brian W. Skelton' 'Mark E. Smith' 'Loic Toupet' 'Allan H. White' _publ_contact_author_name 'Prof M I Bruce' _publ_contact_author_address ; Department of Chemistry University of Adelaide Adelaide 5005 AUSTRALIA ; _publ_contact_author_email MICHAEL.BRUCE@ADELAIDE.EDU.AU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Preparation, structures and some reactions of novel diynyl complexes of iron and ruthenium ; data_br749 _database_code_depnum_ccdc_archive 'CCDC 223445' _audit_creation_method Xtal3.6 _audit_creation_date 00-07-26 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C14 H14 O2 Ru1 Si1' _chemical_formula_moiety 'C14 H14 O2 Ru1 Si1' _chemical_formula_weight 343.42 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 6.6958(6) _cell_length_b 16.1190(10) _cell_length_c 21.291(2) _cell_angle_alpha 82.120(2) _cell_angle_beta 88.887(2) _cell_angle_gamma 89.629(2) _cell_volume 2275.8(3) _cell_formula_units_Z 6 _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6143 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 33.5 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 1.103 _exptl_crystal_description block _exptl_crystal_size_max .45 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .09 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .66 _exptl_absorpt_correction_T_max .90 _diffrn_reflns_number 34494 _reflns_number_total 17462 _reflns_Friedel_coverage 0 _reflns_number_gt 13797 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 34.2 _diffrn_reflns_theta_full 32.2 _diffrn_measured_fraction_theta_max 0.92 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .030 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .048 _refine_ls_wR_factor_ref .055 _refine_ls_goodness_of_fit_ref 1.27 _refine_ls_number_reflns 13797 _refine_ls_number_parameters 487 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .044 _refine_diff_density_min -1.928 _refine_diff_density_max 2.296 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _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 84 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 84 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 12 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 6 .072 .071 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 6 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 -.05849(4) .063577(16) .105084(11) .01960(12) Uani ? ? 1.00000 ? ? C110 .1089(5) -.0298(2) .09755(16) .0277(17) Uani ? ? 1.00000 ? ? O110 .2083(4) -.08617(18) .09267(14) .0399(16) Uani ? ? 1.00000 ? ? C120 .1126(5) .1033(2) .16369(15) .0274(17) Uani ? ? 1.00000 ? ? O120 .2100(4) .1275(2) .20028(13) .0429(18) Uani ? ? 1.00000 ? ? C11 .0976(5) .1268(2) .03243(14) .0232(15) Uani ? ? 1.00000 ? ? C12 .1856(5) .1645(2) -.01317(15) .0263(17) Uani ? ? 1.00000 ? ? C13 .2859(5) .2046(2) -.06611(16) .0294(18) Uani ? ? 1.00000 ? ? C14 .3751(7) .2379(2) -.11249(18) .038(2) Uani ? ? 1.00000 ? ? Si1 .5109(2) .28478(7) -.18458(5) .0419(7) Uani ? ? 1.00000 ? ? C141 .5980(7) .1996(3) -.2288(2) .046(3) Uani ? ? 1.00000 ? ? C142 .3357(11) .3545(4) -.2334(3) .080(4) Uani ? ? 1.00000 ? ? C143 .7278(12) .3434(4) -.1612(3) .093(5) Uani ? ? 1.00000 ? ? C101 -.3451(5) .1104(2) .05802(16) .0284(18) Uani ? ? 1.00000 ? ? C102 -.3440(5) .0222(2) .06584(18) .0302(19) Uani ? ? 1.00000 ? ? C103 -.3401(5) -.0069(2) .1329(2) .033(2) Uani ? ? 1.00000 ? ? C104 -.3367(5) .0631(3) .16496(17) .032(2) Uani ? ? 1.00000 ? ? C105 -.3376(5) .1372(2) .11836(17) .0290(18) Uani ? ? 1.00000 ? ? Ru2 .56121(4) .438422(16) .392351(12) .02265(13) Uani ? ? 1.00000 ? ? C210 .3749(5) .3871(2) .45245(17) .0294(18) Uani ? ? 1.00000 ? ? O210 .2646(4) .3555(2) .48935(15) .0445(18) Uani ? ? 1.00000 ? ? C220 .4045(5) .4123(2) .32518(18) .033(2) Uani ? ? 1.00000 ? ? O220 .3099(5) .3975(2) .28443(15) .050(2) Uani ? ? 1.00000 ? ? C21 .3999(5) .5449(2) .38885(16) .0264(17) Uani ? ? 1.00000 ? ? C22 .2984(5) .6080(2) .38618(17) .0288(17) Uani ? ? 1.00000 ? ? C23 .1787(5) .6784(2) .38460(17) .0297(18) Uani ? ? 1.00000 ? ? C24 .0711(5) .7395(2) .38272(18) .0323(19) Uani ? ? 1.00000 ? ? Si2 -.09547(14) .83061(6) .37771(5) .0289(5) Uani ? ? 1.00000 ? ? C241 -.0356(7) .8917(3) .4430(2) .053(3) Uani ? ? 1.00000 ? ? C242 -.3585(6) .7928(3) .3858(2) .037(2) Uani ? ? 1.00000 ? ? C243 -.0505(7) .8954(3) .2990(2) .046(2) Uani ? ? 1.00000 ? ? C201 .8476(5) .5102(3) .3952(2) .044(2) Uani ? ? 1.00000 ? ? C202 .8266(5) .4542(3) .45150(19) .037(2) Uani ? ? 1.00000 ? ? C203 .8304(6) .3729(3) .4358(2) .041(2) Uani ? ? 1.00000 ? ? C204 .8506(6) .3771(3) .3698(2) .047(3) Uani ? ? 1.00000 ? ? C205 .8593(6) .4641(4) .3441(2) .050(3) Uani ? ? 1.00000 ? ? Ru3 .06286(4) .384565(16) .097565(12) .02224(12) Uani ? ? 1.00000 ? ? C310 -.1143(5) .3440(2) .04106(16) .0299(18) Uani ? ? 1.00000 ? ? O310 -.2176(4) .3200(2) .00597(14) .0444(18) Uani ? ? 1.00000 ? ? C320 -.0969(6) .4802(2) .10214(17) .033(2) Uani ? ? 1.00000 ? ? O320 -.1923(5) .5384(2) .10530(17) .052(2) Uani ? ? 1.00000 ? ? C31 -.0996(5) .3253(2) .17056(16) .0253(16) Uani ? ? 1.00000 ? ? C341 -.5601(8) .0275(3) .3462(2) .052(3) Uani ? ? 1.00000 ? ? C342 -.8165(6) .1810(3) .3635(2) .046(3) Uani ? ? 1.00000 ? ? C343 -.4405(7) .1418(4) .4415(2) .053(3) Uani ? ? 1.00000 ? ? C32 -.1966(5) .2869(2) .21410(15) .0251(16) Uani ? ? 1.00000 ? ? C33 -.3074(5) .2406(2) .26114(15) .0252(16) Uani ? ? 1.00000 ? ? C34 -.4078(5) .2000(2) .30229(17) .0290(18) Uani ? ? 1.00000 ? ? Si3 -.55895(14) .13766(6) .36408(5) .0291(5) Uani ? ? 1.00000 ? ? C301 .3455(5) .3354(2) .14603(17) .0293(18) Uani ? ? 1.00000 ? ? C302 .3313(5) .3034(2) .08730(18) .0309(19) Uani ? ? 1.00000 ? ? C303 .3372(5) .3729(3) .03770(17) .034(2) Uani ? ? 1.00000 ? ? C304 .3526(5) .4468(2) .0660(2) .036(2) Uani ? ? 1.00000 ? ? C305 .3574(5) .4236(2) .13324(18) .034(2) Uani ? ? 1.00000 ? ? H141a .66186 .22447 -.26479 .07174 Uiso ? ? 1.00000 ? ? H141b .47923 .16769 -.24282 .06578 Uiso ? ? 1.00000 ? ? H141c .68029 .16414 -.20398 .06638 Uiso ? ? 1.00000 ? ? H142a .41031 .37816 -.26395 .11904 Uiso ? ? 1.00000 ? ? H142b .29211 .40244 -.21324 .11406 Uiso ? ? 1.00000 ? ? H142c .23470 .32461 -.24925 .11119 Uiso ? ? 1.00000 ? ? H143a .77187 .37144 -.19135 .15971 Uiso ? ? 1.00000 ? ? H143b .82015 .31163 -.13142 .14606 Uiso ? ? 1.00000 ? ? H143c .69388 .38358 -.13452 .09885 Uiso ? ? 1.00000 ? ? H101 -.34151 .14290 .01917 .02381 Uiso ? ? 1.00000 ? ? H102 -.34329 -.01503 .03562 .03563 Uiso ? ? 1.00000 ? ? H103 -.33959 -.06204 .14825 .04995 Uiso ? ? 1.00000 ? ? H104 -.32432 .07124 .20609 .05085 Uiso ? ? 1.00000 ? ? H105 -.34369 .19078 .12625 .03529 Uiso ? ? 1.00000 ? ? H241a -.12131 .93942 .44135 .08000 Uiso ? ? 1.00000 ? ? H241b .09922 .90968 .43919 .08000 Uiso ? ? 1.00000 ? ? H241c -.05546 .85764 .48304 .08000 Uiso ? ? 1.00000 ? ? H242a -.44748 .83940 .38337 .05700 Uiso ? ? 1.00000 ? ? H242b -.37765 .75870 .42559 .05700 Uiso ? ? 1.00000 ? ? H242c -.38657 .76088 .35263 .05700 Uiso ? ? 1.00000 ? ? H243a -.13614 .94322 .29475 .07100 Uiso ? ? 1.00000 ? ? H243b -.07961 .86292 .26566 .07100 Uiso ? ? 1.00000 ? ? H243c .08418 .91286 .29469 .07100 Uiso ? ? 1.00000 ? ? H201 .85292 .57040 .39246 .05500 Uiso ? ? 1.00000 ? ? H202 .81260 .46900 .49364 .04700 Uiso ? ? 1.00000 ? ? H203 .82078 .32209 .46525 .05100 Uiso ? ? 1.00000 ? ? H204 .85655 .33064 .34624 .05900 Uiso ? ? 1.00000 ? ? H205 .87261 .48603 .29998 .06300 Uiso ? ? 1.00000 ? ? H341a -.42719 .00623 .34679 .07900 Uiso ? ? 1.00000 ? ? H341b -.61471 .02582 .30561 .07900 Uiso ? ? 1.00000 ? ? H341c -.63886 -.00631 .37743 .07900 Uiso ? ? 1.00000 ? ? H342a -.81510 .23735 .37264 .07000 Uiso ? ? 1.00000 ? ? H342b -.89848 .14833 .39472 .07000 Uiso ? ? 1.00000 ? ? H342c -.87432 .18046 .32291 .07000 Uiso ? ? 1.00000 ? ? H343a -.44005 .19843 .45103 .07900 Uiso ? ? 1.00000 ? ? H343b -.30644 .12224 .44088 .07900 Uiso ? ? 1.00000 ? ? H343c -.51316 .10823 .47471 .07900 Uiso ? ? 1.00000 ? ? H301 .34649 .30286 .18717 .03700 Uiso ? ? 1.00000 ? ? H302 .31947 .24539 .08205 .03900 Uiso ? ? 1.00000 ? ? H303 .33167 .36962 -.00682 .04300 Uiso ? ? 1.00000 ? ? H304 .35867 .50282 .04390 .04500 Uiso ? ? 1.00000 ? ? H305 .36674 .46118 .16443 .04300 Uiso ? ? 1.00000 ? ? 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 Ru1 .01564(10) .02440(11) .01830(11) .00134(8) .00061(8) -.00142(8) C110 .0224(15) .0332(17) .0267(15) .0032(13) -.0028(12) -.0011(13) O110 .0365(15) .0413(15) .0421(15) .0162(12) -.0055(12) -.0068(12) C120 .0211(14) .0386(18) .0222(14) -.0011(13) .0009(11) -.0039(13) O120 .0331(14) .063(2) .0357(15) -.0033(13) -.0080(11) -.0148(13) C11 .0219(14) .0285(15) .0197(13) .0023(11) -.0002(10) -.0048(11) C12 .0261(15) .0291(15) .0239(15) .0039(12) .0007(12) -.0052(12) C13 .0335(18) .0279(16) .0265(16) .0032(13) .0053(13) -.0034(13) C14 .048(2) .0352(19) .0300(18) -.0011(16) .0142(16) .0006(15) Si1 .0576(7) .0351(5) .0297(5) .0011(5) .0194(5) .0041(4) C141 .054(3) .051(2) .030(2) .012(2) .0114(18) .0051(17) C142 .113(5) .069(4) .047(3) .046(3) .036(3) .022(3) C143 .130(6) .089(5) .062(4) -.068(5) .025(4) -.018(3) C101 .0178(14) .0381(18) .0293(16) .0061(13) -.0038(11) -.0037(13) C102 .0187(14) .0352(17) .0397(19) .0001(13) -.0024(13) -.0155(15) C103 .0200(15) .0303(17) .047(2) -.0047(13) .0041(14) .0004(15) C104 .0213(15) .050(2) .0262(16) .0019(14) .0059(12) -.0079(15) C105 .0215(15) .0311(16) .0362(18) .0067(12) -.0007(12) -.0115(14) Ru2 .01652(11) .02674(12) .02480(12) .00219(9) -.00189(8) -.00383(9) C210 .0220(15) .0308(16) .0335(17) .0047(12) -.0024(13) .0025(13) O210 .0290(14) .0529(18) .0463(17) -.0011(12) .0035(12) .0116(14) C220 .0246(16) .043(2) .0317(17) .0063(14) -.0014(13) -.0094(15) O220 .0390(16) .076(2) .0394(16) .0068(15) -.0128(13) -.0213(15) C21 .0200(14) .0301(16) .0284(16) .0007(12) .0012(11) -.0013(12) C22 .0218(15) .0307(16) .0321(17) -.0010(12) .0026(12) .0018(13) C23 .0218(15) .0305(16) .0338(17) -.0009(12) .0021(12) .0056(13) C24 .0270(16) .0318(17) .0359(18) .0042(13) .0040(14) .0027(14) Si2 .0232(4) .0289(5) .0326(5) .0045(4) .0025(4) .0025(4) C241 .043(2) .064(3) .054(3) -.004(2) .002(2) -.019(2) C242 .0256(17) .039(2) .042(2) -.0030(14) -.0034(15) .0099(16) C243 .038(2) .045(2) .049(2) .0129(18) .0102(18) .0139(19) C201 .0183(16) .036(2) .075(3) -.0057(14) .0016(17) -.004(2) C202 .0212(16) .055(2) .036(2) -.0018(15) -.0047(13) -.0146(17) C203 .0224(16) .041(2) .057(3) .0030(15) -.0138(16) .0019(18) C204 .0230(17) .064(3) .060(3) .0148(18) -.0105(17) -.035(2) C205 .0184(16) .092(4) .036(2) .003(2) .0053(14) .005(2) Ru3 .01766(11) .02567(12) .02221(12) .00099(8) .00250(8) .00043(9) C310 .0235(15) .0376(18) .0276(16) .0044(13) .0014(12) -.0012(14) O310 .0315(14) .065(2) .0378(15) .0031(13) -.0083(12) -.0109(14) C320 .0322(18) .0327(17) .0317(17) .0022(14) .0029(14) -.0017(14) O320 .053(2) .0418(17) .061(2) .0191(14) .0032(16) -.0073(15) C31 .0199(14) .0284(15) .0275(15) .0001(11) .0011(11) -.0035(12) C341 .057(3) .033(2) .063(3) -.002(2) .021(2) .000(2) C342 .0283(19) .064(3) .045(2) .0105(19) .0084(16) -.003(2) C343 .039(2) .080(3) .035(2) -.006(2) -.0003(18) .007(2) C32 .0217(14) .0291(15) .0251(15) .0001(12) .0001(11) -.0065(12) C33 .0224(14) .0314(16) .0215(14) .0006(12) .0000(11) -.0032(12) C34 .0250(15) .0316(16) .0297(16) -.0013(13) .0023(12) -.0020(13) Si3 .0235(4) .0310(5) .0306(5) -.0010(4) .0067(4) .0024(4) C301 .0181(14) .0358(17) .0325(17) .0033(12) -.0037(12) .0005(14) C302 .0197(14) .0357(18) .0373(18) .0055(13) .0001(13) -.0059(14) C303 .0210(15) .049(2) .0302(17) .0015(14) .0073(13) -.0005(15) C304 .0250(16) .038(2) .040(2) -.0045(14) .0078(14) .0061(16) C305 .0237(16) .040(2) .038(2) -.0068(14) .0006(14) -.0095(15) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 C110 . . 1.893(4) ? Ru1 C120 . . 1.888(4) ? Ru1 C11 . . 2.010(3) ? Ru1 C101 . . 2.260(3) ? Ru1 C102 . . 2.243(4) ? Ru1 C103 . . 2.235(3) ? Ru1 C104 . . 2.236(3) ? Ru1 C105 . . 2.241(3) ? C110 O110 . . 1.138(5) ? C120 O120 . . 1.136(5) ? C11 C12 . . 1.216(4) ? C12 C13 . . 1.384(5) ? C13 C14 . . 1.207(5) ? C14 Si1 . . 1.841(4) ? Si1 C141 . . 1.853(5) ? Si1 C142 . . 1.853(6) ? Si1 C143 . . 1.851(8) ? C141 H141a . . .915 ? C141 H141b . . 1.021 ? C141 H141c . . .913 ? C142 H142a . . .860 ? C142 H142b . . .974 ? C142 H142c . . .928 ? C143 H143a . . .787 ? C143 H143b . . .984 ? C143 H143c . . .941 ? C101 C102 . . 1.408(5) ? C101 C105 . . 1.412(5) ? C101 H101 . . .917 ? C102 C103 . . 1.441(5) ? C102 H102 . . .938 ? C103 C104 . . 1.397(6) ? C103 H103 . . .904 ? C104 C105 . . 1.444(5) ? C104 H104 . . .908 ? C105 H105 . . .903 ? Ru2 C210 . . 1.881(3) ? Ru2 C220 . . 1.885(4) ? Ru2 C21 . . 2.015(3) ? Ru2 C201 . . 2.252(4) ? Ru2 C202 . . 2.234(4) ? Ru2 C203 . . 2.235(4) ? Ru2 C204 . . 2.242(4) ? Ru2 C205 . . 2.242(4) ? C210 O210 . . 1.138(4) ? C220 O220 . . 1.137(5) ? C21 C22 . . 1.215(5) ? C22 C23 . . 1.382(5) ? C23 C24 . . 1.213(5) ? C24 Si2 . . 1.831(4) ? Si2 C241 . . 1.861(6) ? Si2 C242 . . 1.864(4) ? Si2 C243 . . 1.870(4) ? C241 H241a . . .954 ? C241 H241b . . .949 ? C241 H241c . . .956 ? C242 H242a . . .952 ? C242 H242b . . .951 ? C242 H242c . . .952 ? C243 H243a . . .953 ? C243 H243b . . .961 ? C243 H243c . . .946 ? C201 C202 . . 1.404(6) ? C201 C205 . . 1.399(7) ? C201 H201 . . .964 ? C202 C203 . . 1.396(6) ? C202 H202 . . .962 ? C203 C204 . . 1.402(7) ? C203 H203 . . .962 ? C204 C205 . . 1.435(7) ? C204 H204 . . .958 ? C205 H205 . . .960 ? Ru3 C310 . . 1.887(4) ? Ru3 C320 . . 1.882(4) ? Ru3 C31 . . 2.013(3) ? Ru3 C301 . . 2.260(3) ? Ru3 C302 . . 2.242(4) ? Ru3 C303 . . 2.237(4) ? Ru3 C304 . . 2.239(4) ? Ru3 C305 . . 2.251(4) ? C310 O310 . . 1.136(5) ? C320 O320 . . 1.141(5) ? C31 C32 . . 1.220(4) ? C341 Si3 . . 1.867(5) ? C341 H341a . . .951 ? C341 H341b . . .949 ? C341 H341c . . .952 ? C342 Si3 . . 1.856(4) ? C342 H342a . . .955 ? C342 H342b . . .956 ? C342 H342c . . .954 ? C343 Si3 . . 1.853(5) ? C343 H343a . . .962 ? C343 H343b . . .950 ? C343 H343c . . .956 ? C32 C33 . . 1.373(4) ? C33 C34 . . 1.214(5) ? C34 Si3 . . 1.834(3) ? C301 C302 . . 1.422(6) ? C301 C305 . . 1.413(5) ? C301 H301 . . .957 ? C302 C303 . . 1.430(5) ? C302 H302 . . .960 ? C303 C304 . . 1.414(6) ? C303 H303 . . .958 ? C304 C305 . . 1.430(6) ? C304 H304 . . .960 ? C305 H305 . . .962 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C110 Ru1 C120 . . . 92.14(15) ? C110 Ru1 C11 . . . 87.85(13) ? C110 Ru1 C101 . . . 133.16(15) ? C110 Ru1 C102 . . . 101.06(14) ? C110 Ru1 C103 . . . 97.69(14) ? C110 Ru1 C104 . . . 126.06(14) ? C110 Ru1 C105 . . . 159.36(14) ? C120 Ru1 C11 . . . 90.60(13) ? C120 Ru1 C101 . . . 134.65(15) ? C120 Ru1 C102 . . . 158.01(14) ? C120 Ru1 C103 . . . 123.67(15) ? C120 Ru1 C104 . . . 96.29(14) ? C120 Ru1 C105 . . . 101.45(14) ? C11 Ru1 C101 . . . 89.46(12) ? C11 Ru1 C102 . . . 107.25(13) ? C11 Ru1 C103 . . . 144.80(14) ? C11 Ru1 C104 . . . 144.87(13) ? C11 Ru1 C105 . . . 107.25(12) ? C101 Ru1 C102 . . . 36.45(13) ? C101 Ru1 C103 . . . 61.56(12) ? C101 Ru1 C104 . . . 61.58(12) ? C101 Ru1 C105 . . . 36.58(13) ? C102 Ru1 C103 . . . 37.55(14) ? C102 Ru1 C104 . . . 61.72(14) ? C102 Ru1 C105 . . . 61.52(14) ? C103 Ru1 C104 . . . 36.42(15) ? C103 Ru1 C105 . . . 61.85(13) ? C104 Ru1 C105 . . . 37.62(13) ? Ru1 C110 O110 . . . 179.4(4) ? Ru1 C120 O120 . . . 177.6(3) ? Ru1 C11 C12 . . . 177.3(3) ? C11 C12 C13 . . . 177.8(4) ? C12 C13 C14 . . . 178.6(4) ? C13 C14 Si1 . . . 177.7(4) ? C14 Si1 C141 . . . 108.6(2) ? C14 Si1 C142 . . . 107.9(2) ? C14 Si1 C143 . . . 108.8(2) ? C141 Si1 C142 . . . 110.0(2) ? C141 Si1 C143 . . . 109.9(3) ? C142 Si1 C143 . . . 111.5(3) ? Si1 C141 H141a . . . 107.0 ? Si1 C141 H141b . . . 110.5 ? Si1 C141 H141c . . . 109.8 ? H141a C141 H141b . . . 107.0 ? H141a C141 H141c . . . 112.0 ? H141b C141 H141c . . . 110.5 ? Si1 C142 H142a . . . 103.4 ? Si1 C142 H142b . . . 113.1 ? Si1 C142 H142c . . . 111.8 ? H142a C142 H142b . . . 101.5 ? H142a C142 H142c . . . 110.1 ? H142b C142 H142c . . . 115.6 ? Si1 C143 H143a . . . 109.0 ? Si1 C143 H143b . . . 116.0 ? Si1 C143 H143c . . . 113.7 ? H143a C143 H143b . . . 119.0 ? H143a C143 H143c . . . 102.0 ? H143b C143 H143c . . . 95.5 ? Ru1 C101 C102 . . . 71.1(2) ? Ru1 C101 C105 . . . 71.00(19) ? Ru1 C101 H101 . . . 120.3 ? C102 C101 C105 . . . 108.8(3) ? C102 C101 H101 . . . 123.4 ? C105 C101 H101 . . . 127.7 ? Ru1 C102 C101 . . . 72.4(2) ? Ru1 C102 C103 . . . 70.9(2) ? Ru1 C102 H102 . . . 121.2 ? C101 C102 C103 . . . 107.6(3) ? C101 C102 H102 . . . 130.5 ? C103 C102 H102 . . . 121.9 ? Ru1 C103 C102 . . . 71.5(2) ? Ru1 C103 C104 . . . 71.8(2) ? Ru1 C103 H103 . . . 122.1 ? C102 C103 C104 . . . 108.1(3) ? C102 C103 H103 . . . 121.9 ? C104 C103 H103 . . . 130.1 ? Ru1 C104 C103 . . . 71.8(2) ? Ru1 C104 C105 . . . 71.4(2) ? Ru1 C104 H104 . . . 117.9 ? C103 C104 C105 . . . 108.1(3) ? C103 C104 H104 . . . 135.0 ? C105 C104 H104 . . . 116.7 ? Ru1 C105 C101 . . . 72.4(2) ? Ru1 C105 C104 . . . 71.0(2) ? Ru1 C105 H105 . . . 126.1 ? C101 C105 C104 . . . 107.4(3) ? C101 C105 H105 . . . 125.9 ? C104 C105 H105 . . . 126.5 ? C210 Ru2 C220 . . . 91.08(16) ? C210 Ru2 C21 . . . 88.34(14) ? C210 Ru2 C201 . . . 136.05(17) ? C210 Ru2 C202 . . . 102.54(15) ? C210 Ru2 C203 . . . 96.27(15) ? C210 Ru2 C204 . . . 122.64(16) ? C210 Ru2 C205 . . . 157.55(16) ? C220 Ru2 C21 . . . 86.86(16) ? C220 Ru2 C201 . . . 132.77(17) ? C220 Ru2 C202 . . . 160.83(15) ? C220 Ru2 C203 . . . 129.58(17) ? C220 Ru2 C204 . . . 100.25(17) ? C220 Ru2 C205 . . . 101.81(16) ? C21 Ru2 C201 . . . 90.98(14) ? C21 Ru2 C202 . . . 106.71(15) ? C21 Ru2 C203 . . . 142.96(15) ? C21 Ru2 C204 . . . 147.69(15) ? C21 Ru2 C205 . . . 110.43(17) ? C201 Ru2 C202 . . . 36.48(16) ? C201 Ru2 C203 . . . 60.69(15) ? C201 Ru2 C204 . . . 61.05(17) ? C201 Ru2 C205 . . . 36.28(19) ? C202 Ru2 C203 . . . 36.41(16) ? C202 Ru2 C204 . . . 61.06(17) ? C202 Ru2 C205 . . . 61.14(15) ? C203 Ru2 C204 . . . 36.49(17) ? C203 Ru2 C205 . . . 61.35(16) ? C204 Ru2 C205 . . . 37.32(19) ? Ru2 C210 O210 . . . 178.9(3) ? Ru2 C220 O220 . . . 179.2(4) ? Ru2 C21 C22 . . . 178.3(3) ? C21 C22 C23 . . . 178.1(4) ? C22 C23 C24 . . . 178.9(4) ? C23 C24 Si2 . . . 178.1(4) ? C24 Si2 C241 . . . 108.5(2) ? C24 Si2 C242 . . . 108.47(17) ? C24 Si2 C243 . . . 107.96(19) ? C241 Si2 C242 . . . 110.5(2) ? C241 Si2 C243 . . . 110.3(2) ? C242 Si2 C243 . . . 110.95(19) ? Si2 C241 H241a . . . 109.9 ? Si2 C241 H241b . . . 110.2 ? Si2 C241 H241c . . . 109.9 ? H241a C241 H241b . . . 109.2 ? H241a C241 H241c . . . 108.6 ? H241b C241 H241c . . . 109.1 ? Si2 C242 H242a . . . 109.7 ? Si2 C242 H242b . . . 109.8 ? Si2 C242 H242c . . . 109.8 ? H242a C242 H242b . . . 109.2 ? H242a C242 H242c . . . 109.1 ? H242b C242 H242c . . . 109.2 ? Si2 C243 H243a . . . 110.0 ? Si2 C243 H243b . . . 109.6 ? Si2 C243 H243c . . . 110.4 ? H243a C243 H243b . . . 108.3 ? H243a C243 H243c . . . 109.6 ? H243b C243 H243c . . . 108.9 ? Ru2 C201 C202 . . . 71.0(2) ? Ru2 C201 C205 . . . 71.5(2) ? Ru2 C201 H201 . . . 123.4 ? C202 C201 C205 . . . 108.6(4) ? C202 C201 H201 . . . 125.4 ? C205 C201 H201 . . . 126.1 ? Ru2 C202 C201 . . . 72.5(2) ? Ru2 C202 C203 . . . 71.8(2) ? Ru2 C202 H202 . . . 121.6 ? C201 C202 C203 . . . 108.1(4) ? C201 C202 H202 . . . 126.2 ? C203 C202 H202 . . . 125.7 ? Ru2 C203 C202 . . . 71.7(2) ? Ru2 C203 C204 . . . 72.1(2) ? Ru2 C203 H203 . . . 122.2 ? C202 C203 C204 . . . 108.7(4) ? C202 C203 H203 . . . 126.0 ? C204 C203 H203 . . . 125.3 ? Ru2 C204 C203 . . . 71.5(2) ? Ru2 C204 C205 . . . 71.3(2) ? Ru2 C204 H204 . . . 122.3 ? C203 C204 C205 . . . 107.3(4) ? C203 C204 H204 . . . 126.4 ? C205 C204 H204 . . . 126.4 ? Ru2 C205 C201 . . . 72.3(2) ? Ru2 C205 C204 . . . 71.4(2) ? Ru2 C205 H205 . . . 122.4 ? C201 C205 C204 . . . 107.3(4) ? C201 C205 H205 . . . 126.8 ? C204 C205 H205 . . . 125.8 ? C310 Ru3 C320 . . . 91.65(16) ? C310 Ru3 C31 . . . 89.03(14) ? C310 Ru3 C301 . . . 134.70(15) ? C310 Ru3 C302 . . . 101.09(15) ? C310 Ru3 C303 . . . 95.40(15) ? C310 Ru3 C304 . . . 123.00(15) ? C310 Ru3 C305 . . . 157.06(15) ? C320 Ru3 C31 . . . 88.19(14) ? C320 Ru3 C301 . . . 133.55(15) ? C320 Ru3 C302 . . . 160.97(15) ? C320 Ru3 C303 . . . 128.15(15) ? C320 Ru3 C304 . . . 99.45(15) ? C320 Ru3 C305 . . . 102.18(16) ? C31 Ru3 C301 . . . 89.65(12) ? C31 Ru3 C302 . . . 105.92(13) ? C31 Ru3 C303 . . . 143.07(14) ? C31 Ru3 C304 . . . 146.47(14) ? C31 Ru3 C305 . . . 109.38(13) ? C301 Ru3 C302 . . . 36.82(14) ? C301 Ru3 C303 . . . 61.65(13) ? C301 Ru3 C304 . . . 61.49(13) ? C301 Ru3 C305 . . . 36.50(13) ? C302 Ru3 C303 . . . 37.25(13) ? C302 Ru3 C304 . . . 61.76(13) ? C302 Ru3 C305 . . . 61.47(14) ? C303 Ru3 C304 . . . 36.81(15) ? C303 Ru3 C305 . . . 61.66(14) ? C304 Ru3 C305 . . . 37.13(14) ? Ru3 C310 O310 . . . 178.4(3) ? Ru3 C320 O320 . . . 179.3(4) ? Ru3 C31 C32 . . . 177.9(3) ? Si3 C341 H341a . . . 109.5 ? Si3 C341 H341b . . . 109.7 ? Si3 C341 H341c . . . 109.5 ? H341a C341 H341b . . . 109.5 ? H341a C341 H341c . . . 109.2 ? H341b C341 H341c . . . 109.4 ? Si3 C342 H342a . . . 110.3 ? Si3 C342 H342b . . . 110.3 ? Si3 C342 H342c . . . 110.4 ? H342a C342 H342b . . . 108.5 ? H342a C342 H342c . . . 108.6 ? H342b C342 H342c . . . 108.6 ? Si3 C343 H343a . . . 110.1 ? Si3 C343 H343b . . . 110.8 ? Si3 C343 H343c . . . 110.5 ? H343a C343 H343b . . . 108.4 ? H343a C343 H343c . . . 107.9 ? H343b C343 H343c . . . 109.0 ? C31 C32 C33 . . . 177.1(4) ? C32 C33 C34 . . . 179.1(4) ? C33 C34 Si3 . . . 179.4(3) ? C341 Si3 C342 . . . 110.7(2) ? C341 Si3 C343 . . . 109.8(2) ? C341 Si3 C34 . . . 107.7(2) ? C342 Si3 C343 . . . 111.1(2) ? C342 Si3 C34 . . . 109.16(18) ? C343 Si3 C34 . . . 108.3(2) ? Ru3 C301 C302 . . . 70.9(2) ? Ru3 C301 C305 . . . 71.4(2) ? Ru3 C301 H301 . . . 123.3 ? C302 C301 C305 . . . 108.2(3) ? C302 C301 H301 . . . 126.0 ? C305 C301 H301 . . . 125.8 ? Ru3 C302 C301 . . . 72.3(2) ? Ru3 C302 C303 . . . 71.2(2) ? Ru3 C302 H302 . . . 122.0 ? C301 C302 C303 . . . 107.8(3) ? C301 C302 H302 . . . 125.9 ? C303 C302 H302 . . . 126.3 ? Ru3 C303 C302 . . . 71.5(2) ? Ru3 C303 C304 . . . 71.7(2) ? Ru3 C303 H303 . . . 122.4 ? C302 C303 C304 . . . 107.9(3) ? C302 C303 H303 . . . 125.9 ? C304 C303 H303 . . . 126.2 ? Ru3 C304 C303 . . . 71.5(2) ? Ru3 C304 C305 . . . 71.9(2) ? Ru3 C304 H304 . . . 122.2 ? C303 C304 C305 . . . 108.0(3) ? C303 C304 H304 . . . 125.8 ? C305 C304 H304 . . . 126.2 ? Ru3 C305 C301 . . . 72.1(2) ? Ru3 C305 C304 . . . 71.0(2) ? Ru3 C305 H305 . . . 122.5 ? C301 C305 C304 . . . 108.0(4) ? C301 C305 H305 . . . 125.8 ? C304 C305 H305 . . . 126.2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1032 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min -24 _reflns_limit_k_max 25 _reflns_limit_l_min -33 _reflns_limit_l_max 33 _reflns_number_observed ? _reflns_d_resolution_high .632 _reflns_d_resolution_low 13.625 _diffrn_reflns_av_sigmaI/netI .063 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .067 _refine_ls_wR_factor_all .059 _refine_ls_goodness_of_fit_all 1.205 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? data_br805 _database_code_depnum_ccdc_archive 'CCDC 223446' _audit_creation_method Xtal3.6 _audit_creation_date 01-05-10 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C53 H56 P2 Ru1 Si1' _chemical_formula_moiety 'C48 H44 P2 Ru1 Si1, C5 H12' _chemical_formula_weight 884.14 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 11.1851(8) _cell_length_b 17.1710(10) _cell_length_c 24.241(2) _cell_angle_alpha 90.00000 _cell_angle_beta 95.572(2) _cell_angle_gamma 90.00000 _cell_volume 4633.7(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6011 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 36.4 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu .467 _exptl_crystal_description plate _exptl_crystal_size_max .25 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .07 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .76 _exptl_absorpt_correction_T_max .86 _diffrn_reflns_number 96657 _reflns_number_total 24383 _reflns_Friedel_coverage 0 _reflns_number_gt 14615 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.8 _diffrn_reflns_theta_full 36.5 _diffrn_measured_fraction_theta_max .98 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .070 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .041 _refine_ls_wR_factor_ref .035 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_number_reflns 14615 _refine_ls_number_parameters 690 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .023 _refine_diff_density_min -.978 _refine_diff_density_max 1.287 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 212 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 224 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 4 .072 .071 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru .167732(11) .134772(7) .179457(6) .01483(5) Uani ? ? 1.00000 ? ? P1 .05655(4) .05966(2) .234051(18) .01681(18) Uani ? ? 1.00000 ? ? C111 .13143(14) .00509(10) .29246(7) .0201(7) Uani ? ? 1.00000 ? ? C112 .16713(17) .03987(12) .34321(8) .0279(9) Uani ? ? 1.00000 ? ? C113 .22893(19) -.00324(15) .38553(9) .0380(12) Uani ? ? 1.00000 ? ? C114 .25411(19) -.08124(14) .37757(10) .0405(12) Uani ? ? 1.00000 ? ? C115 .22000(18) -.11607(12) .32742(10) .0352(11) Uani ? ? 1.00000 ? ? C116 .16058(16) -.07348(11) .28479(9) .0261(9) Uani ? ? 1.00000 ? ? C121 -.05285(14) .12285(9) .26530(7) .0201(8) Uani ? ? 1.00000 ? ? C122 -.01186(17) .19074(11) .29277(8) .0258(9) Uani ? ? 1.00000 ? ? C123 -.09132(18) .24166(12) .31459(9) .0310(10) Uani ? ? 1.00000 ? ? C124 -.21368(19) .22665(13) .30857(9) .0345(10) Uani ? ? 1.00000 ? ? C125 -.25596(18) .16080(13) .28066(9) .0344(10) Uani ? ? 1.00000 ? ? C126 -.17662(16) .10879(11) .25933(8) .0258(9) Uani ? ? 1.00000 ? ? C131 -.04115(14) -.01647(9) .20059(7) .0199(7) Uani ? ? 1.00000 ? ? C132 -.10631(16) -.06683(10) .23233(9) .0264(9) Uani ? ? 1.00000 ? ? C133 -.18107(17) -.12315(11) .20668(10) .0334(10) Uani ? ? 1.00000 ? ? C134 -.19220(17) -.13095(12) .14973(10) .0340(10) Uani ? ? 1.00000 ? ? C135 -.12780(17) -.08249(11) .11789(9) .0298(10) Uani ? ? 1.00000 ? ? C136 -.05257(15) -.02533(10) .14337(8) .0228(8) Uani ? ? 1.00000 ? ? P2 .32488(4) .05234(2) .167392(18) .01585(18) Uani ? ? 1.00000 ? ? C211 .39619(14) -.01783(9) .21763(7) .0186(7) Uani ? ? 1.00000 ? ? C212 .43549(16) .01016(11) .27010(8) .0252(9) Uani ? ? 1.00000 ? ? C213 .50643(17) -.03555(11) .30734(9) .0294(9) Uani ? ? 1.00000 ? ? C214 .53762(17) -.11034(11) .29267(9) .0308(9) Uani ? ? 1.00000 ? ? C215 .49737(17) -.13912(12) .24140(9) .0313(9) Uani ? ? 1.00000 ? ? C216 .42758(16) -.09343(10) .20349(8) .0246(8) Uani ? ? 1.00000 ? ? C221 .46318(14) .10384(9) .15287(7) .0178(7) Uani ? ? 1.00000 ? ? C222 .46980(15) .18466(10) .15502(7) .0205(8) Uani ? ? 1.00000 ? ? C223 .57224(15) .22337(10) .14171(8) .0238(8) Uani ? ? 1.00000 ? ? C224 .67021(16) .18197(11) .12706(8) .0244(9) Uani ? ? 1.00000 ? ? C225 .66664(15) .10121(11) .12692(7) .0227(8) Uani ? ? 1.00000 ? ? C226 .56447(15) .06232(10) .13950(7) .0212(8) Uani ? ? 1.00000 ? ? C231 .29005(14) -.00466(9) .10402(7) .0200(7) Uani ? ? 1.00000 ? ? C232 .32835(17) .01754(11) .05363(8) .0259(9) Uani ? ? 1.00000 ? ? C233 .2878(2) -.02066(13) .00496(8) .0340(10) Uani ? ? 1.00000 ? ? C234 .20782(19) -.08158(13) .00597(9) .0365(11) Uani ? ? 1.00000 ? ? C235 .16877(18) -.10474(12) .05592(9) .0334(10) Uani ? ? 1.00000 ? ? C236 .20924(16) -.06684(10) .10447(8) .0249(9) Uani ? ? 1.00000 ? ? C1 .26199(14) .16908(9) .24896(7) .0191(7) Uani ? ? 1.00000 ? ? C2 .32011(15) .18970(9) .29190(7) .0211(8) Uani ? ? 1.00000 ? ? C3 .38467(16) .20088(10) .34247(8) .0241(8) Uani ? ? 1.00000 ? ? C4 .44051(18) .20855(11) .38758(8) .0326(10) Uani ? ? 1.00000 ? ? C41 .4500(4) .1453(3) .50303(16) .080(3) Uani ? ? 1.00000 ? ? C42 .6758(2) .2074(2) .46013(14) .0513(16) Uani ? ? 1.00000 ? ? C43 .4740(3) .3196(2) .48167(15) .066(2) Uani ? ? 1.00000 ? ? Si .51090(5) .22026(4) .45817(2) .0350(3) Uani ? ? 1.00000 ? ? C01 .16130(16) .25291(10) .13992(8) .0258(9) Uani ? ? 1.00000 ? ? C02 .18389(17) .19805(11) .09936(8) .0258(9) Uani ? ? 1.00000 ? ? C03 .08361(16) .14664(11) .09143(8) .0253(9) Uani ? ? 1.00000 ? ? C04 .00055(16) .17071(11) .12855(8) .0258(9) Uani ? ? 1.00000 ? ? C05 .04700(16) .23668(10) .15866(8) .0262(9) Uani ? ? 1.00000 ? ? C10 .0651(6) .2945(3) -.04087(16) .173(5) Uani ? ? 1.00000 ? ? C20 .0177(4) .3448(3) .00378(18) .113(3) Uani ? ? 1.00000 ? ? C30 .1106(2) .39686(16) .03246(11) .0550(15) Uani ? ? 1.00000 ? ? C40 .0695(3) .4478(2) .07732(14) .075(2) Uani ? ? 1.00000 ? ? C50 .1653(4) .4974(2) .10556(15) .098(3) Uani ? ? 1.00000 ? ? H112 .1492(16) .0930(11) .3488(8) .024(5) Uiso ? ? 1.00000 ? ? H113 .250(2) .0213(13) .4188(10) .049(7) Uiso ? ? 1.00000 ? ? H114 .291(2) -.1105(13) .4074(10) .048(7) Uiso ? ? 1.00000 ? ? H115 .2360(19) -.1660(13) .3217(9) .036(6) Uiso ? ? 1.00000 ? ? H116 .1390(17) -.0965(11) .2503(8) .026(5) Uiso ? ? 1.00000 ? ? H122 .0690(17) .2015(11) .2975(8) .025(5) Uiso ? ? 1.00000 ? ? H123 -.0598(17) .2856(12) .3335(8) .032(6) Uiso ? ? 1.00000 ? ? H124 -.2673(19) .2630(12) .3236(9) .040(6) Uiso ? ? 1.00000 ? ? H125 -.336(2) .1493(12) .2754(9) .041(6) Uiso ? ? 1.00000 ? ? H126 -.2051(17) .0605(11) .2408(8) .025(5) Uiso ? ? 1.00000 ? ? H132 -.1016(16) -.0601(10) .2718(8) .021(5) Uiso ? ? 1.00000 ? ? H133 -.222(2) -.1570(13) .2295(9) .040(6) Uiso ? ? 1.00000 ? ? H134 -.2407(18) -.1695(12) .1334(8) .033(6) Uiso ? ? 1.00000 ? ? H135 -.1310(18) -.0888(12) .0785(9) .034(6) Uiso ? ? 1.00000 ? ? H136 -.0052(17) .0068(11) .1210(8) .025(5) Uiso ? ? 1.00000 ? ? H212 .4172(18) .0591(12) .2809(8) .030(6) Uiso ? ? 1.00000 ? ? H213 .532(2) -.0162(12) .3412(9) .038(6) Uiso ? ? 1.00000 ? ? H214 .5854(19) -.1402(12) .3194(9) .036(6) Uiso ? ? 1.00000 ? ? H215 .5163(19) -.1874(12) .2329(9) .036(6) Uiso ? ? 1.00000 ? ? H216 .4042(17) -.1144(11) .1680(8) .025(5) Uiso ? ? 1.00000 ? ? H222 .4028(16) .2140(10) .1664(7) .021(5) Uiso ? ? 1.00000 ? ? H223 .5742(17) .2741(11) .1427(8) .026(5) Uiso ? ? 1.00000 ? ? H224 .7374(18) .2080(11) .1169(8) .029(5) Uiso ? ? 1.00000 ? ? H225 .7340(17) .0728(11) .1192(8) .023(5) Uiso ? ? 1.00000 ? ? H226 .5618(14) .0061(10) .1393(7) .011(4) Uiso ? ? 1.00000 ? ? H232 .3785(18) .0555(12) .0515(8) .031(6) Uiso ? ? 1.00000 ? ? H233 .3105(18) -.0066(12) -.0283(9) .032(6) Uiso ? ? 1.00000 ? ? H234 .1833(18) -.1073(12) -.0286(9) .038(6) Uiso ? ? 1.00000 ? ? H235 .113(2) -.1439(12) .0576(9) .040(6) Uiso ? ? 1.00000 ? ? H236 .1837(16) -.0820(10) .1382(8) .018(5) Uiso ? ? 1.00000 ? ? H41a .477(3) .151(2) .5400(17) .117(14) Uiso ? ? 1.00000 ? ? H41b .469(4) .098(2) .4893(17) .13(2) Uiso ? ? 1.00000 ? ? H41c .366(3) .153(2) .5035(14) .099(13) Uiso ? ? 1.00000 ? ? H42a .714(2) .2152(15) .4976(12) .067(8) Uiso ? ? 1.00000 ? ? H42b .709(3) .2398(17) .4361(12) .074(10) Uiso ? ? 1.00000 ? ? H42c .695(3) .1610(19) .4475(13) .080(10) Uiso ? ? 1.00000 ? ? H43a .512(3) .3276(17) .5181(13) .083(10) Uiso ? ? 1.00000 ? ? H43b .391(3) .3218(17) .4787(12) .080(10) Uiso ? ? 1.00000 ? ? H43c .502(3) .357(2) .4587(15) .108(16) Uiso ? ? 1.00000 ? ? H01 .2110(17) .2920(11) .1537(8) .026(5) Uiso ? ? 1.00000 ? ? H02 .2479(19) .1966(12) .0801(8) .034(6) Uiso ? ? 1.00000 ? ? H03 .0720(17) .1064(11) .0656(8) .027(5) Uiso ? ? 1.00000 ? ? H04 -.0721(18) .1483(11) .1339(8) .028(5) Uiso ? ? 1.00000 ? ? H05 .0126(18) .2640(12) .1866(8) .033(6) Uiso ? ? 1.00000 ? ? H10a .00593 .26217 -.05912 .24100 Uiso ? ? 1.00000 ? ? H10b .12988 .26180 -.02433 .24100 Uiso ? ? 1.00000 ? ? H10c .09948 .32638 -.06817 .24100 Uiso ? ? 1.00000 ? ? H20a -.01650 .31271 .03011 .13700 Uiso ? ? 1.00000 ? ? H20b -.04690 .37729 -.01372 .13700 Uiso ? ? 1.00000 ? ? H30a .14335 .42974 .00573 .06900 Uiso ? ? 1.00000 ? ? H30b .17526 .36460 .04896 .06900 Uiso ? ? 1.00000 ? ? H40a .03698 .41502 .10433 .09000 Uiso ? ? 1.00000 ? ? H40b .00588 .48038 .06118 .09000 Uiso ? ? 1.00000 ? ? H50a .13454 .52842 .13357 .14600 Uiso ? ? 1.00000 ? ? H50b .19757 .53083 .07937 .14600 Uiso ? ? 1.00000 ? ? H50c .22867 .46547 .12252 .14600 Uiso ? ? 1.00000 ? ? 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 .01179(5) .01328(5) .01926(6) .00016(5) .00063(4) .00065(6) P1 .01401(18) .01530(18) .0212(2) .00043(15) .00222(16) .00001(16) C111 .0153(7) .0213(8) .0241(8) .0006(6) .0039(6) .0042(7) C112 .0244(9) .0327(10) .0269(10) .0042(8) .0044(7) .0020(8) C113 .0295(11) .0577(15) .0263(11) .0054(10) .0009(9) .0040(10) C114 .0286(11) .0515(14) .0409(13) .0100(10) .0003(9) .0220(11) C115 .0247(10) .0288(10) .0520(14) .0072(8) .0035(9) .0142(9) C116 .0197(8) .0230(9) .0355(11) .0010(7) .0029(8) .0042(8) C121 .0177(7) .0220(8) .0209(8) .0033(6) .0043(6) .0018(6) C122 .0216(9) .0240(9) .0322(10) .0031(7) .0049(8) -.0032(7) C123 .0318(10) .0262(9) .0352(11) .0066(8) .0045(9) -.0057(8) C124 .0319(10) .0380(11) .0348(11) .0160(9) .0093(9) -.0014(9) C125 .0177(9) .0448(12) .0412(12) .0095(8) .0051(8) -.0016(10) C126 .0189(8) .0304(9) .0280(10) .0027(7) .0018(7) -.0008(8) C131 .0140(7) .0168(7) .0287(9) -.0003(6) .0019(6) -.0006(6) C132 .0228(9) .0226(8) .0344(11) -.0034(7) .0062(8) .0009(8) C133 .0239(9) .0251(10) .0518(13) -.0064(7) .0066(9) .0033(9) C134 .0243(9) .0239(9) .0525(13) -.0067(8) -.0035(9) -.0051(9) C135 .0279(10) .0262(9) .0340(11) -.0024(7) -.0032(8) -.0058(8) C136 .0194(8) .0190(8) .0298(10) -.0008(6) .0013(7) .0000(7) P2 .01372(18) .01401(18) .0199(2) -.00048(14) .00201(15) -.00093(15) C211 .0139(7) .0172(7) .0251(9) .0006(6) .0034(6) .0018(6) C212 .0242(9) .0214(8) .0295(10) .0051(7) -.0004(7) .0004(7) C213 .0271(10) .0290(10) .0310(10) .0039(8) -.0036(8) .0042(8) C214 .0209(9) .0284(9) .0428(12) .0054(7) .0015(8) .0120(9) C215 .0295(9) .0197(8) .0453(12) .0062(8) .0072(8) .0042(9) C216 .0242(9) .0176(8) .0324(10) .0020(7) .0048(8) -.0002(7) C221 .0136(7) .0204(7) .0193(8) -.0003(6) .0016(6) -.0012(6) C222 .0153(7) .0192(8) .0270(9) -.0006(6) .0020(7) -.0026(7) C223 .0181(8) .0187(8) .0348(10) -.0028(6) .0030(7) -.0023(7) C224 .0163(8) .0292(9) .0277(10) -.0045(7) .0032(7) -.0016(7) C225 .0148(8) .0274(9) .0263(9) .0019(7) .0037(7) -.0035(7) C226 .0186(8) .0199(8) .0253(9) .0000(6) .0021(7) -.0027(7) C231 .0160(7) .0188(7) .0250(9) .0015(6) .0015(6) -.0023(6) C232 .0281(9) .0248(9) .0246(9) -.0049(7) .0019(7) -.0027(7) C233 .0367(11) .0431(12) .0218(10) -.0039(9) .0014(8) -.0038(9) C234 .0328(11) .0442(12) .0315(11) -.0040(9) -.0016(9) -.0152(10) C235 .0260(10) .0319(10) .0426(12) -.0088(8) .0044(9) -.0141(9) C236 .0219(8) .0237(8) .0299(10) -.0043(7) .0065(7) -.0062(7) C1 .0152(7) .0139(7) .0285(9) .0017(6) .0038(6) .0006(6) C2 .0190(8) .0159(7) .0284(9) .0015(6) .0018(7) -.0026(7) C3 .0239(9) .0196(8) .0287(9) .0022(7) .0020(7) -.0028(7) C4 .0341(11) .0303(10) .0322(11) .0032(8) -.0039(9) -.0050(8) C41 .067(2) .120(4) .050(2) -.032(2) -.0088(17) .024(2) C42 .0364(14) .0594(18) .0557(18) .0049(13) -.0070(13) -.0066(15) C43 .061(2) .080(2) .0521(18) .0239(17) -.0214(16) -.0362(18) Si .0315(3) .0445(3) .0271(3) -.0002(3) -.0065(2) -.0040(3) C01 .0237(9) .0174(8) .0349(10) -.0011(7) -.0047(8) .0080(7) C02 .0207(8) .0296(9) .0267(9) .0008(7) .0012(7) .0119(8) C03 .0247(9) .0259(9) .0239(9) .0006(7) -.0053(7) .0042(7) C04 .0156(8) .0269(9) .0336(10) .0008(7) -.0046(7) .0088(8) C05 .0230(9) .0220(8) .0336(10) .0078(7) .0015(8) .0049(8) C10 .329(8) .128(4) .052(2) -.133(5) -.024(3) .003(2) C20 .112(3) .111(3) .103(3) -.057(3) -.053(3) .054(3) C30 .0539(16) .0590(16) .0516(15) -.0067(13) .0021(13) .0229(13) C40 .072(2) .077(2) .082(2) .0302(18) .0324(18) .0281(18) C50 .140(4) .085(3) .070(2) -.011(3) .013(2) -.013(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru P1 . . 2.2980(5) ? Ru P2 . . 2.2975(4) ? Ru C1 . . 1.9881(17) ? Ru C01 . . 2.2417(18) ? Ru C02 . . 2.248(2) ? Ru C03 . . 2.2561(18) ? Ru C04 . . 2.2254(18) ? Ru C05 . . 2.2378(18) ? P1 C111 . . 1.8315(17) ? P1 C121 . . 1.8515(17) ? P1 C131 . . 1.8409(16) ? C111 C112 . . 1.391(3) ? C111 C116 . . 1.405(2) ? C112 C113 . . 1.393(3) ? C112 H112 . . .95(2) ? C113 C114 . . 1.386(3) ? C113 H113 . . .92(2) ? C114 C115 . . 1.375(3) ? C114 H114 . . .94(2) ? C115 C116 . . 1.382(3) ? C115 H115 . . .89(2) ? C116 H116 . . .93(2) ? C121 C122 . . 1.398(2) ? C121 C126 . . 1.399(2) ? C122 C123 . . 1.388(3) ? C122 H122 . . .92(2) ? C123 C124 . . 1.386(3) ? C123 H123 . . .93(2) ? C124 C125 . . 1.378(3) ? C124 H124 . . .96(2) ? C125 C126 . . 1.393(3) ? C125 H125 . . .91(2) ? C126 H126 . . .982(19) ? C131 C132 . . 1.407(3) ? C131 C136 . . 1.389(3) ? C132 C133 . . 1.386(3) ? C132 H132 . . .96(2) ? C133 C134 . . 1.381(3) ? C133 H133 . . .95(2) ? C134 C135 . . 1.384(3) ? C134 H134 . . .92(2) ? C135 C136 . . 1.397(3) ? C135 H135 . . .96(2) ? C136 H136 . . .97(2) ? P2 C211 . . 1.8391(16) ? P2 C221 . . 1.8451(17) ? P2 C231 . . 1.8312(17) ? C211 C212 . . 1.391(2) ? C211 C216 . . 1.396(2) ? C212 C213 . . 1.386(3) ? C212 H212 . . .91(2) ? C213 C214 . . 1.386(3) ? C213 H213 . . .91(2) ? C214 C215 . . 1.372(3) ? C214 H214 . . .95(2) ? C215 C216 . . 1.389(3) ? C215 H215 . . .88(2) ? C216 H216 . . .95(2) ? C221 C222 . . 1.391(2) ? C221 C226 . . 1.403(2) ? C222 C223 . . 1.389(2) ? C222 H222 . . .965(19) ? C223 C224 . . 1.381(3) ? C223 H223 . . .87(2) ? C224 C225 . . 1.387(3) ? C224 H224 . . .93(2) ? C225 C226 . . 1.383(2) ? C225 H225 . . .932(19) ? C226 H226 . . .966(17) ? C231 C232 . . 1.387(3) ? C231 C236 . . 1.400(2) ? C232 C233 . . 1.387(3) ? C232 H232 . . .86(2) ? C233 C234 . . 1.378(3) ? C233 H233 . . .90(2) ? C234 C235 . . 1.385(3) ? C234 H234 . . .96(2) ? C235 C236 . . 1.382(3) ? C235 H235 . . .92(2) ? C236 H236 . . .928(19) ? C1 C2 . . 1.225(2) ? C2 C3 . . 1.375(2) ? C3 C4 . . 1.213(3) ? C4 Si . . 1.824(2) ? C41 Si . . 1.856(5) ? C41 H41a . . .92(4) ? C41 H41b . . .91(4) ? C41 H41c . . .95(4) ? C42 Si . . 1.854(3) ? C42 H42a . . .97(3) ? C42 H42b . . .91(3) ? C42 H42c . . .89(3) ? C43 Si . . 1.857(4) ? C43 H43a . . .95(3) ? C43 H43b . . .93(3) ? C43 H43c . . .92(4) ? C01 C02 . . 1.402(3) ? C01 C05 . . 1.425(3) ? C01 H01 . . .914(19) ? C02 C03 . . 1.426(3) ? C02 H02 . . .89(2) ? C03 C04 . . 1.416(3) ? C03 H03 . . .93(2) ? C04 C05 . . 1.418(3) ? C04 H04 . . .92(2) ? C05 H05 . . .94(2) ? C10 C20 . . 1.520(7) ? C10 H10a . . .941 ? C10 H10b . . .972 ? C10 H10c . . .967 ? C20 C30 . . 1.490(5) ? C20 H20a . . .952 ? C20 H20b . . .976 ? C30 C40 . . 1.502(4) ? C30 H30a . . .959 ? C30 H30b . . .966 ? C40 C50 . . 1.484(5) ? C40 H40a . . .961 ? C40 H40b . . .959 ? C50 H50a . . .953 ? C50 H50b . . .952 ? C50 H50c . . .957 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published P1 Ru P2 . . . 101.015(16) ? P1 Ru C1 . . . 87.15(5) ? P1 Ru C01 . . . 139.23(5) ? P1 Ru C02 . . . 149.57(5) ? P1 Ru C03 . . . 113.33(5) ? P1 Ru C04 . . . 90.14(5) ? P1 Ru C05 . . . 102.72(5) ? P2 Ru C1 . . . 86.62(5) ? P2 Ru C01 . . . 119.75(5) ? P2 Ru C02 . . . 93.51(5) ? P2 Ru C03 . . . 100.91(5) ? P2 Ru C04 . . . 135.42(5) ? P2 Ru C05 . . . 154.89(5) ? C1 Ru C01 . . . 94.97(7) ? C1 Ru C02 . . . 120.56(7) ? C1 Ru C03 . . . 155.91(6) ? C1 Ru C04 . . . 137.37(7) ? C1 Ru C05 . . . 102.59(7) ? C01 Ru C02 . . . 36.40(7) ? C01 Ru C03 . . . 61.37(7) ? C01 Ru C04 . . . 61.42(7) ? C01 Ru C05 . . . 37.10(7) ? C02 Ru C03 . . . 36.91(7) ? C02 Ru C04 . . . 61.35(7) ? C02 Ru C05 . . . 61.62(7) ? C03 Ru C04 . . . 36.84(7) ? C03 Ru C05 . . . 61.91(7) ? C04 Ru C05 . . . 37.06(7) ? Ru P1 C111 . . . 120.00(6) ? Ru P1 C121 . . . 108.84(5) ? Ru P1 C131 . . . 118.43(6) ? C111 P1 C121 . . . 104.74(8) ? C111 P1 C131 . . . 100.64(7) ? C121 P1 C131 . . . 102.05(7) ? P1 C111 C112 . . . 122.32(13) ? P1 C111 C116 . . . 118.93(13) ? C112 C111 C116 . . . 118.63(16) ? C111 C112 C113 . . . 120.17(19) ? C111 C112 H112 . . . 119.6(11) ? C113 C112 H112 . . . 120.3(11) ? C112 C113 C114 . . . 120.3(2) ? C112 C113 H113 . . . 118.0(14) ? C114 C113 H113 . . . 121.7(14) ? C113 C114 C115 . . . 120.0(2) ? C113 C114 H114 . . . 119.2(14) ? C115 C114 H114 . . . 120.7(14) ? C114 C115 C116 . . . 120.2(2) ? C114 C115 H115 . . . 121.0(13) ? C116 C115 H115 . . . 118.8(13) ? C111 C116 C115 . . . 120.67(18) ? C111 C116 H116 . . . 118.7(12) ? C115 C116 H116 . . . 120.6(12) ? P1 C121 C122 . . . 118.97(13) ? P1 C121 C126 . . . 122.91(13) ? C122 C121 C126 . . . 117.96(16) ? C121 C122 C123 . . . 120.97(17) ? C121 C122 H122 . . . 120.1(12) ? C123 C122 H122 . . . 118.9(12) ? C122 C123 C124 . . . 120.33(18) ? C122 C123 H123 . . . 118.1(12) ? C124 C123 H123 . . . 121.5(12) ? C123 C124 C125 . . . 119.5(2) ? C123 C124 H124 . . . 119.1(13) ? C125 C124 H124 . . . 121.4(13) ? C124 C125 C126 . . . 120.52(18) ? C124 C125 H125 . . . 122.1(14) ? C126 C125 H125 . . . 117.4(14) ? C121 C126 C125 . . . 120.70(17) ? C121 C126 H126 . . . 117.9(11) ? C125 C126 H126 . . . 121.4(11) ? P1 C131 C132 . . . 120.82(14) ? P1 C131 C136 . . . 120.73(13) ? C132 C131 C136 . . . 118.45(15) ? C131 C132 C133 . . . 120.37(19) ? C131 C132 H132 . . . 119.3(11) ? C133 C132 H132 . . . 120.2(11) ? C132 C133 C134 . . . 120.5(2) ? C132 C133 H133 . . . 118.2(13) ? C134 C133 H133 . . . 121.3(13) ? C133 C134 C135 . . . 119.88(18) ? C133 C134 H134 . . . 119.4(13) ? C135 C134 H134 . . . 120.7(13) ? C134 C135 C136 . . . 120.0(2) ? C134 C135 H135 . . . 121.1(12) ? C136 C135 H135 . . . 118.9(12) ? C131 C136 C135 . . . 120.77(17) ? C131 C136 H136 . . . 119.8(11) ? C135 C136 H136 . . . 119.4(11) ? Ru P2 C211 . . . 127.40(6) ? Ru P2 C221 . . . 113.27(5) ? Ru P2 C231 . . . 109.45(5) ? C211 P2 C221 . . . 97.04(7) ? C211 P2 C231 . . . 104.39(7) ? C221 P2 C231 . . . 102.13(8) ? P2 C211 C212 . . . 117.23(12) ? P2 C211 C216 . . . 123.35(13) ? C212 C211 C216 . . . 118.77(16) ? C211 C212 C213 . . . 120.68(17) ? C211 C212 H212 . . . 121.5(12) ? C213 C212 H212 . . . 117.8(12) ? C212 C213 C214 . . . 119.99(18) ? C212 C213 H213 . . . 119.4(13) ? C214 C213 H213 . . . 120.6(13) ? C213 C214 C215 . . . 119.83(18) ? C213 C214 H214 . . . 117.6(13) ? C215 C214 H214 . . . 122.5(13) ? C214 C215 C216 . . . 120.64(18) ? C214 C215 H215 . . . 118.9(13) ? C216 C215 H215 . . . 120.5(13) ? C211 C216 C215 . . . 120.07(18) ? C211 C216 H216 . . . 121.6(11) ? C215 C216 H216 . . . 118.3(11) ? P2 C221 C222 . . . 120.91(12) ? P2 C221 C226 . . . 120.76(12) ? C222 C221 C226 . . . 118.33(15) ? C221 C222 C223 . . . 120.72(16) ? C221 C222 H222 . . . 119.4(11) ? C223 C222 H222 . . . 119.8(11) ? C222 C223 C224 . . . 120.41(16) ? C222 C223 H223 . . . 119.4(13) ? C224 C223 H223 . . . 120.2(13) ? C223 C224 C225 . . . 119.45(17) ? C223 C224 H224 . . . 120.2(12) ? C225 C224 H224 . . . 120.4(12) ? C224 C225 C226 . . . 120.42(16) ? C224 C225 H225 . . . 120.0(11) ? C226 C225 H225 . . . 119.5(11) ? C221 C226 C225 . . . 120.58(16) ? C221 C226 H226 . . . 119.0(10) ? C225 C226 H226 . . . 120.4(10) ? P2 C231 C232 . . . 122.23(13) ? P2 C231 C236 . . . 119.09(14) ? C232 C231 C236 . . . 118.14(16) ? C231 C232 C233 . . . 121.05(18) ? C231 C232 H232 . . . 121.2(13) ? C233 C232 H232 . . . 117.7(13) ? C232 C233 C234 . . . 120.2(2) ? C232 C233 H233 . . . 122.5(13) ? C234 C233 H233 . . . 117.3(13) ? C233 C234 C235 . . . 119.6(2) ? C233 C234 H234 . . . 117.6(13) ? C235 C234 H234 . . . 122.8(13) ? C234 C235 C236 . . . 120.3(2) ? C234 C235 H235 . . . 121.4(14) ? C236 C235 H235 . . . 118.3(14) ? C231 C236 C235 . . . 120.72(18) ? C231 C236 H236 . . . 118.3(11) ? C235 C236 H236 . . . 120.9(11) ? Ru C1 C2 . . . 179.57(14) ? C1 C2 C3 . . . 171.08(18) ? C2 C3 C4 . . . 178.0(2) ? C3 C4 Si . . . 174.60(19) ? Si C41 H41a . . . 113(2) ? Si C41 H41b . . . 107(3) ? Si C41 H41c . . . 109(2) ? H41a C41 H41b . . . 112(3) ? H41a C41 H41c . . . 102(3) ? H41b C41 H41c . . . 114(3) ? Si C42 H42a . . . 110.7(16) ? Si C42 H42b . . . 112.3(18) ? Si C42 H42c . . . 112(2) ? H42a C42 H42b . . . 110(2) ? H42a C42 H42c . . . 110(2) ? H42b C42 H42c . . . 102(3) ? Si C43 H43a . . . 109.0(18) ? Si C43 H43b . . . 105.4(18) ? Si C43 H43c . . . 111(2) ? H43a C43 H43b . . . 115(3) ? H43a C43 H43c . . . 108(3) ? H43b C43 H43c . . . 109(3) ? C4 Si C41 . . . 108.89(14) ? C4 Si C42 . . . 110.41(12) ? C4 Si C43 . . . 107.49(13) ? C41 Si C42 . . . 108.86(17) ? C41 Si C43 . . . 110.6(2) ? C42 Si C43 . . . 110.58(16) ? Ru C01 C02 . . . 72.02(11) ? Ru C01 C05 . . . 71.30(10) ? Ru C01 H01 . . . 121.0(12) ? C02 C01 C05 . . . 108.68(16) ? C02 C01 H01 . . . 127.3(13) ? C05 C01 H01 . . . 124.0(13) ? Ru C02 C01 . . . 71.57(11) ? Ru C02 C03 . . . 71.88(11) ? Ru C02 H02 . . . 125.1(13) ? C01 C02 C03 . . . 108.51(17) ? C01 C02 H02 . . . 126.4(13) ? C03 C02 H02 . . . 125.0(13) ? Ru C03 C02 . . . 71.22(10) ? Ru C03 C04 . . . 70.40(10) ? Ru C03 H03 . . . 125.9(12) ? C02 C03 C04 . . . 106.84(16) ? C02 C03 H03 . . . 127.2(12) ? C04 C03 H03 . . . 125.8(12) ? Ru C04 C03 . . . 72.76(10) ? Ru C04 C05 . . . 71.95(10) ? Ru C04 H04 . . . 120.8(12) ? C03 C04 C05 . . . 109.26(16) ? C03 C04 H04 . . . 127.6(12) ? C05 C04 H04 . . . 123.1(12) ? Ru C05 C01 . . . 71.60(10) ? Ru C05 C04 . . . 70.99(10) ? Ru C05 H05 . . . 120.6(12) ? C01 C05 C04 . . . 106.69(17) ? C01 C05 H05 . . . 125.2(12) ? C04 C05 H05 . . . 128.0(12) ? C20 C10 H10a . . . 113.1 ? C20 C10 H10b . . . 109.4 ? C20 C10 H10c . . . 110.8 ? H10a C10 H10b . . . 108.3 ? H10a C10 H10c . . . 108.7 ? H10b C10 H10c . . . 106.2 ? C10 C20 C30 . . . 113.4(4) ? C10 C20 H20a . . . 109.8 ? C10 C20 H20b . . . 108.0 ? C30 C20 H20a . . . 110.0 ? C30 C20 H20b . . . 108.3 ? H20a C20 H20b . . . 107.0 ? C20 C30 C40 . . . 116.0(3) ? C20 C30 H30a . . . 109.4 ? C20 C30 H30b . . . 108.0 ? C40 C30 H30a . . . 108.1 ? C40 C30 H30b . . . 107.7 ? H30a C30 H30b . . . 107.3 ? C30 C40 C50 . . . 114.2(3) ? C30 C40 H40a . . . 108.4 ? C30 C40 H40b . . . 108.2 ? C50 C40 H40a . . . 109.0 ? C50 C40 H40b . . . 109.1 ? H40a C40 H40b . . . 107.8 ? C40 C50 H50a . . . 110.8 ? C40 C50 H50b . . . 110.0 ? C40 C50 H50c . . . 109.9 ? H50a C50 H50b . . . 109.0 ? H50a C50 H50c . . . 108.5 ? H50b C50 H50c . . . 108.6 ? 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 #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1848 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 29 _reflns_limit_l_min -41 _reflns_limit_l_max 41 _reflns_number_observed ? _reflns_d_resolution_high .58 _reflns_d_resolution_low 13.951 _diffrn_reflns_av_sigmaI/netI .154 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .094 _refine_ls_wR_factor_all .041 _refine_ls_goodness_of_fit_all .954 _refine_ls_shift/su_mean .0005 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? data_br807 _database_code_depnum_ccdc_archive 'CCDC 223447' _audit_creation_method Xtal3.6 _audit_creation_date 01-06-04 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C43 H48 P2 Ru1 Si1' _chemical_formula_moiety 'C43 H48 P2 Ru1 Si1' _chemical_formula_weight 755.96 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 15.6527(8) _cell_length_b 13.9997(7) _cell_length_c 18.9093(9) _cell_angle_alpha 90.00000 _cell_angle_beta 110.9770(10) _cell_angle_gamma 90.00000 _cell_volume 3869.0(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 37.2 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu .547 _exptl_crystal_description prism _exptl_crystal_size_max .38 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .16 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .74 _exptl_absorpt_correction_T_max .86 _diffrn_reflns_number 80261 _reflns_number_total 20314 _reflns_Friedel_coverage 0 _reflns_number_gt 14141 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.6 _diffrn_reflns_theta_full 36.0 _diffrn_measured_fraction_theta_max .990 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .040 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .032 _refine_ls_wR_factor_ref .034 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_number_reflns 14141 _refine_ls_number_parameters 616 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .033 _refine_diff_density_min -.733 _refine_diff_density_max 1.312 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 172 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 192 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 4 .072 .071 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru .050788(7) .208685(7) .228924(5) .01513(4) Uani ? ? 1.00000 ? ? P1 -.00955(2) .12920(2) .117993(18) .01711(13) Uani ? ? 1.00000 ? ? C111 -.12946(9) .08956(10) .08563(7) .0201(5) Uani ? ? 1.00000 ? ? C112 -.16477(10) .02655(11) .02483(8) .0251(6) Uani ? ? 1.00000 ? ? C113 -.25254(10) -.01053(12) .00566(9) .0299(7) Uani ? ? 1.00000 ? ? C114 -.30625(10) .01636(13) .04671(9) .0346(7) Uani ? ? 1.00000 ? ? C115 -.27317(11) .08066(14) .10549(10) .0370(8) Uani ? ? 1.00000 ? ? C116 -.18472(10) .11657(12) .12540(8) .0279(6) Uani ? ? 1.00000 ? ? C121 -.00244(9) .17945(9) .03101(7) .0191(5) Uani ? ? 1.00000 ? ? C122 .08190(10) .18561(10) .02154(8) .0225(5) Uani ? ? 1.00000 ? ? C123 .08743(10) .22262(11) -.04503(8) .0264(6) Uani ? ? 1.00000 ? ? C124 .00981(11) .25638(11) -.10183(8) .0279(6) Uani ? ? 1.00000 ? ? C125 -.07393(11) .25327(11) -.09225(8) .0272(6) Uani ? ? 1.00000 ? ? C126 -.07997(10) .21497(10) -.02652(8) .0236(5) Uani ? ? 1.00000 ? ? C10 .04898(9) .01284(10) .13005(8) .0208(5) Uani ? ? 1.00000 ? ? C20 .04375(11) -.03345(10) .20185(8) .0251(6) Uani ? ? 1.00000 ? ? P2 .05748(2) .05839(2) .276716(19) .01809(13) Uani ? ? 1.00000 ? ? C211 -.02962(9) .02766(10) .31741(8) .0226(5) Uani ? ? 1.00000 ? ? C212 -.11534(11) -.01038(13) .27544(9) .0339(7) Uani ? ? 1.00000 ? ? C213 -.18261(13) -.02043(16) .30674(11) .0457(9) Uani ? ? 1.00000 ? ? C214 -.16681(13) .00860(15) .38025(11) .0445(9) Uani ? ? 1.00000 ? ? C215 -.08190(12) .04508(13) .42318(10) .0339(7) Uani ? ? 1.00000 ? ? C216 -.01419(10) .05372(11) .39231(8) .0263(6) Uani ? ? 1.00000 ? ? C221 .15989(9) .01728(9) .35389(7) .0206(5) Uani ? ? 1.00000 ? ? C222 .23276(10) .07831(10) .38883(8) .0229(5) Uani ? ? 1.00000 ? ? C223 .30846(10) .04549(11) .44923(8) .0269(6) Uani ? ? 1.00000 ? ? C224 .31164(11) -.04781(12) .47421(9) .0297(6) Uani ? ? 1.00000 ? ? C225 .23986(11) -.10948(11) .43889(9) .0327(7) Uani ? ? 1.00000 ? ? C226 .16431(11) -.07719(11) .37910(9) .0292(6) Uani ? ? 1.00000 ? ? C1 .17043(9) .18457(9) .21827(7) .0190(5) Uani ? ? 1.00000 ? ? C2 .24562(9) .17903(10) .21155(8) .0219(5) Uani ? ? 1.00000 ? ? C3 .32750(10) .17616(10) .20048(8) .0230(5) Uani ? ? 1.00000 ? ? C4 .39984(11) .17467(12) .18958(9) .0293(6) Uani ? ? 1.00000 ? ? Si .50263(3) .16153(3) .16644(3) .02824(18) Uani ? ? 1.00000 ? ? C41 .51511(15) .03268(14) .15020(16) .0461(10) Uani ? ? 1.00000 ? ? C42 .4908(3) .2307(3) .0797(2) .086(2) Uani ? ? 1.00000 ? ? C43 .60522(17) .2052(3) .2451(2) .0788(18) Uani ? ? 1.00000 ? ? C01 .04437(10) .36625(9) .20903(8) .0222(5) Uani ? ? 1.00000 ? ? C011 .06586(15) .41790(13) .14758(11) .0373(8) Uani ? ? 1.00000 ? ? C02 -.04438(9) .33558(10) .20533(8) .0221(5) Uani ? ? 1.00000 ? ? C021 -.13079(12) .35481(14) .13928(10) .0358(8) Uani ? ? 1.00000 ? ? C03 -.03676(9) .29810(9) .27727(8) .0221(5) Uani ? ? 1.00000 ? ? C031 -.11402(13) .27271(13) .30327(11) .0337(8) Uani ? ? 1.00000 ? ? C04 .05793(10) .30642(9) .32619(8) .0228(5) Uani ? ? 1.00000 ? ? C041 .09385(15) .28916(13) .40993(9) .0352(7) Uani ? ? 1.00000 ? ? C05 .10659(10) .34995(9) .28411(8) .0230(5) Uani ? ? 1.00000 ? ? C051 .20439(12) .38244(13) .31362(12) .0359(8) Uani ? ? 1.00000 ? ? H112 -.1292(11) .0103(12) -.0035(9) .028(4) Uiso ? ? 1.00000 ? ? H113 -.2749(12) -.0557(13) -.0350(10) .031(5) Uiso ? ? 1.00000 ? ? H114 -.3678(14) -.0099(14) .0326(11) .047(6) Uiso ? ? 1.00000 ? ? H115 -.3072(14) .1031(15) .1342(11) .053(6) Uiso ? ? 1.00000 ? ? H116 -.1623(13) .1594(13) .1663(10) .038(5) Uiso ? ? 1.00000 ? ? H122 .1357(12) .1652(12) .0600(9) .026(4) Uiso ? ? 1.00000 ? ? H123 .1443(12) .2241(12) -.0509(10) .033(5) Uiso ? ? 1.00000 ? ? H124 .0109(12) .2808(12) -.1453(10) .032(5) Uiso ? ? 1.00000 ? ? H125 -.1259(14) .2791(13) -.1306(11) .046(6) Uiso ? ? 1.00000 ? ? H126 -.1345(12) .2122(11) -.0213(10) .026(4) Uiso ? ? 1.00000 ? ? H10a .0189(11) -.0268(12) .0839(9) .026(4) Uiso ? ? 1.00000 ? ? H10b .1108(12) .0247(12) .1357(9) .027(4) Uiso ? ? 1.00000 ? ? H20a .0888(13) -.0798(13) .2226(10) .037(5) Uiso ? ? 1.00000 ? ? H20b -.0144(13) -.0661(13) .1908(10) .041(5) Uiso ? ? 1.00000 ? ? H212 -.1287(12) -.0333(13) .2235(10) .039(5) Uiso ? ? 1.00000 ? ? H213 -.2425(15) -.0490(15) .2754(12) .060(6) Uiso ? ? 1.00000 ? ? H214 -.2125(14) -.0003(14) .4020(11) .048(6) Uiso ? ? 1.00000 ? ? H215 -.0688(12) .0646(13) .4737(10) .038(5) Uiso ? ? 1.00000 ? ? H216 .0448(13) .0758(13) .4216(10) .040(5) Uiso ? ? 1.00000 ? ? H222 .2304(11) .1424(12) .3699(9) .024(4) Uiso ? ? 1.00000 ? ? H223 .3551(12) .0857(12) .4698(9) .026(4) Uiso ? ? 1.00000 ? ? H224 .3640(12) -.0657(12) .5119(10) .032(5) Uiso ? ? 1.00000 ? ? H225 .2403(12) -.1730(13) .4553(10) .033(5) Uiso ? ? 1.00000 ? ? H226 .1179(13) -.1219(13) .3556(10) .040(5) Uiso ? ? 1.00000 ? ? H41a .560(2) .020(2) .1359(16) .103(10) Uiso ? ? 1.00000 ? ? H41b .458(2) .006(2) .1139(15) .090(9) Uiso ? ? 1.00000 ? ? H41c .5216(17) .0002(18) .1951(16) .077(8) Uiso ? ? 1.00000 ? ? H42a .539(2) .2188(19) .0606(16) .090(9) Uiso ? ? 1.00000 ? ? H42b .478(2) .286(2) .079(2) .108(12) Uiso ? ? 1.00000 ? ? H42c .438(2) .203(2) .0443(17) .091(13) Uiso ? ? 1.00000 ? ? H43a .6564(19) .2013(17) .2329(15) .083(9) Uiso ? ? 1.00000 ? ? H43b .606(2) .159(2) .2787(17) .100(13) Uiso ? ? 1.00000 ? ? H43c .6014(18) .262(2) .2631(15) .077(8) Uiso ? ? 1.00000 ? ? H011a .0609(14) .4874(16) .1525(11) .053(6) Uiso ? ? 1.00000 ? ? H011b .0286(16) .4009(16) .0980(13) .063(7) Uiso ? ? 1.00000 ? ? H011c .1265(16) .4082(16) .1515(12) .062(7) Uiso ? ? 1.00000 ? ? H021a -.1372(13) .4219(14) .1357(10) .038(5) Uiso ? ? 1.00000 ? ? H021b -.1847(14) .3265(15) .1454(11) .045(6) Uiso ? ? 1.00000 ? ? H021c -.1298(13) .3275(14) .0942(11) .042(5) Uiso ? ? 1.00000 ? ? H031a -.1275(15) .3225(16) .3298(12) .061(7) Uiso ? ? 1.00000 ? ? H031b -.1145(16) .2138(16) .3214(13) .059(7) Uiso ? ? 1.00000 ? ? H031c -.1764(17) .2645(18) .2591(14) .076(8) Uiso ? ? 1.00000 ? ? H041a .0863(14) .3419(15) .4349(12) .050(6) Uiso ? ? 1.00000 ? ? H041b .1539(17) .2763(16) .4303(13) .065(8) Uiso ? ? 1.00000 ? ? H041c .0658(17) .2385(19) .4256(14) .072(8) Uiso ? ? 1.00000 ? ? H051a .2067(13) .4489(15) .3210(11) .041(5) Uiso ? ? 1.00000 ? ? H051b .2338(15) .3722(15) .2786(12) .056(6) Uiso ? ? 1.00000 ? ? H051c .2374(16) .3568(17) .3610(13) .066(7) Uiso ? ? 1.00000 ? ? 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 .01533(4) .01634(4) .01481(4) .00103(4) .00671(3) .00014(4) P1 .01583(14) .02070(15) .01583(14) .00076(11) .00693(11) -.00094(11) C111 .0172(6) .0242(6) .0196(6) .0003(5) .0073(5) .0008(5) C112 .0225(6) .0291(7) .0251(7) -.0020(5) .0103(5) -.0045(5) C113 .0229(7) .0348(8) .0289(7) -.0048(6) .0056(6) -.0039(6) C114 .0193(7) .0483(10) .0351(8) -.0066(7) .0086(6) -.0001(7) C115 .0223(7) .0583(11) .0350(8) -.0029(7) .0159(6) -.0068(8) C116 .0221(6) .0378(8) .0257(7) -.0008(6) .0111(5) -.0059(6) C121 .0213(6) .0201(5) .0171(5) -.0010(5) .0086(5) -.0030(4) C122 .0210(6) .0281(7) .0192(6) -.0040(5) .0080(5) -.0034(5) C123 .0264(7) .0321(8) .0241(6) -.0087(6) .0131(5) -.0040(5) C124 .0378(8) .0275(7) .0208(6) -.0055(6) .0134(6) -.0003(5) C125 .0312(8) .0278(7) .0215(6) .0030(6) .0081(6) .0033(5) C126 .0228(6) .0281(7) .0211(6) .0032(5) .0095(5) .0007(5) C10 .0206(6) .0208(6) .0217(6) .0013(5) .0086(5) -.0033(5) C20 .0329(8) .0190(6) .0236(6) -.0001(5) .0104(6) -.0018(5) P2 .01938(15) .01762(14) .01747(14) -.00051(12) .00684(12) .00044(11) C211 .0226(6) .0219(6) .0238(6) -.0027(5) .0090(5) .0029(5) C212 .0287(8) .0423(9) .0299(8) -.0124(7) .0095(6) -.0016(7) C213 .0298(9) .0648(13) .0445(10) -.0191(9) .0157(8) -.0021(9) C214 .0357(9) .0583(12) .0484(11) -.0106(8) .0261(9) .0055(9) C215 .0380(9) .0391(9) .0310(8) -.0024(7) .0200(7) .0038(7) C216 .0267(7) .0277(7) .0263(7) -.0036(6) .0116(6) .0022(5) C221 .0219(6) .0190(6) .0211(6) .0019(5) .0081(5) .0021(5) C222 .0259(7) .0201(6) .0226(6) .0002(5) .0084(5) -.0001(5) C223 .0254(7) .0275(7) .0240(7) -.0001(6) .0044(5) -.0017(5) C224 .0274(7) .0332(8) .0249(7) .0077(6) .0049(6) .0048(6) C225 .0361(8) .0231(7) .0354(8) .0047(6) .0083(7) .0095(6) C226 .0271(7) .0220(7) .0341(8) -.0011(5) .0057(6) .0059(6) C1 .0200(6) .0198(5) .0170(5) .0002(4) .0065(5) -.0003(4) C2 .0208(6) .0253(6) .0201(6) .0000(5) .0078(5) -.0021(5) C3 .0229(6) .0247(6) .0228(6) .0015(5) .0101(5) .0003(5) C4 .0271(7) .0309(7) .0351(8) .0031(6) .0175(6) .0019(6) Si .0276(2) .0238(2) .0430(2) .00036(16) .02440(19) .00081(17) C41 .0418(11) .0287(9) .0834(16) -.0029(8) .0414(12) -.0035(10) C42 .107(3) .084(2) .111(3) .055(2) .091(3) .061(2) C43 .0396(12) .104(2) .109(3) -.0321(14) .0465(15) -.067(2) C01 .0260(7) .0163(6) .0278(6) .0034(5) .0140(5) .0047(5) C011 .0529(11) .0295(8) .0400(10) .0036(8) .0294(9) .0113(7) C02 .0241(6) .0204(6) .0236(6) .0062(5) .0105(5) .0011(5) C021 .0315(8) .0382(9) .0334(8) .0146(7) .0065(7) .0041(7) C03 .0270(7) .0197(6) .0246(6) .0026(5) .0153(5) -.0011(5) C031 .0380(9) .0319(9) .0438(10) .0009(7) .0300(8) -.0010(7) C04 .0312(7) .0186(6) .0198(6) .0028(5) .0104(5) -.0019(4) C041 .0546(11) .0300(8) .0189(6) .0046(8) .0104(7) -.0030(6) C05 .0253(7) .0171(6) .0273(7) .0006(5) .0104(5) -.0038(5) C051 .0288(8) .0301(8) .0471(10) -.0054(6) .0114(8) -.0114(7) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru P1 . . 2.2610(3) ? Ru P2 . . 2.2775(4) ? Ru C1 . . 1.9828(15) ? Ru C01 . . 2.2339(13) ? Ru C02 . . 2.2579(14) ? Ru C03 . . 2.2754(16) ? Ru C04 . . 2.2628(14) ? Ru C05 . . 2.2607(13) ? P1 C111 . . 1.8393(13) ? P1 C121 . . 1.8285(15) ? P1 C10 . . 1.8426(14) ? C111 C112 . . 1.396(2) ? C111 C116 . . 1.387(2) ? C112 C113 . . 1.390(2) ? C112 H112 . . .93(2) ? C113 C114 . . 1.385(3) ? C113 H113 . . .959(17) ? C114 C115 . . 1.379(2) ? C114 H114 . . .98(2) ? C115 C116 . . 1.392(2) ? C115 H115 . . .94(2) ? C116 H116 . . .942(18) ? C121 C122 . . 1.397(2) ? C121 C126 . . 1.3995(17) ? C122 C123 . . 1.392(2) ? C122 H122 . . .938(15) ? C123 C124 . . 1.385(2) ? C123 H123 . . .94(2) ? C124 C125 . . 1.387(3) ? C124 H124 . . .90(2) ? C125 C126 . . 1.388(2) ? C125 H125 . . .947(18) ? C126 H126 . . .89(2) ? C10 C20 . . 1.533(2) ? C10 H10a . . .998(15) ? C10 H10b . . .949(18) ? C20 P2 . . 1.8669(16) ? C20 H20a . . .935(18) ? C20 H20b . . .97(2) ? P2 C211 . . 1.8404(17) ? P2 C221 . . 1.8318(12) ? C211 C212 . . 1.397(2) ? C211 C216 . . 1.397(2) ? C212 C213 . . 1.387(3) ? C212 H212 . . .98(2) ? C213 C214 . . 1.383(3) ? C213 H213 . . 1.00(2) ? C214 C215 . . 1.383(2) ? C214 H214 . . .95(2) ? C215 C216 . . 1.386(3) ? C215 H215 . . .94(2) ? C216 H216 . . .943(17) ? C221 C222 . . 1.3885(18) ? C221 C226 . . 1.399(2) ? C222 C223 . . 1.3967(18) ? C222 H222 . . .962(17) ? C223 C224 . . 1.384(2) ? C223 H223 . . .893(16) ? C224 C225 . . 1.384(2) ? C224 H224 . . .908(15) ? C225 C226 . . 1.387(2) ? C225 H225 . . .941(19) ? C226 H226 . . .942(18) ? C1 C2 . . 1.231(2) ? C2 C3 . . 1.371(2) ? C3 C4 . . 1.222(2) ? C4 Si . . 1.822(2) ? Si C41 . . 1.852(2) ? Si C42 . . 1.855(4) ? Si C43 . . 1.859(3) ? C41 H41a . . .85(4) ? C41 H41b . . .98(3) ? C41 H41c . . .94(3) ? C42 H42a . . .95(4) ? C42 H42b . . .80(3) ? C42 H42c . . .94(3) ? C43 H43a . . .91(3) ? C43 H43b . . .90(3) ? C43 H43c . . .88(3) ? C01 C011 . . 1.505(3) ? C01 C02 . . 1.432(2) ? C01 C05 . . 1.4234(18) ? C011 H011a . . .98(2) ? C011 H011b . . .94(2) ? C011 H011c . . .93(3) ? C02 C021 . . 1.501(2) ? C02 C03 . . 1.423(2) ? C021 H021a . . .94(2) ? C021 H021b . . .98(2) ? C021 H021c . . .94(2) ? C03 C031 . . 1.502(3) ? C03 C04 . . 1.4438(18) ? C031 H031a . . .93(2) ? C031 H031b . . .89(2) ? C031 H031c . . 1.04(2) ? C04 C041 . . 1.498(2) ? C04 C05 . . 1.421(2) ? C041 H041a . . .91(2) ? C041 H041b . . .90(3) ? C041 H041c . . .94(3) ? C05 C051 . . 1.500(2) ? C051 H051a . . .94(2) ? C051 H051b . . .94(3) ? C051 H051c . . .93(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published P1 Ru P2 . . . 81.838(12) ? P1 Ru C1 . . . 85.30(4) ? P1 Ru C01 . . . 110.56(4) ? P1 Ru C02 . . . 100.20(3) ? P1 Ru C03 . . . 122.13(3) ? P1 Ru C04 . . . 159.13(4) ? P1 Ru C05 . . . 145.37(4) ? P2 Ru C1 . . . 88.40(4) ? P2 Ru C01 . . . 166.40(4) ? P2 Ru C02 . . . 137.62(4) ? P2 Ru C03 . . . 107.31(4) ? P2 Ru C04 . . . 104.73(4) ? P2 Ru C05 . . . 132.05(3) ? C1 Ru C01 . . . 97.94(6) ? C1 Ru C02 . . . 133.96(6) ? C1 Ru C03 . . . 149.43(5) ? C1 Ru C04 . . . 114.32(5) ? C1 Ru C05 . . . 88.45(5) ? C01 Ru C02 . . . 37.17(5) ? C01 Ru C03 . . . 61.78(6) ? C01 Ru C04 . . . 61.70(5) ? C01 Ru C05 . . . 36.92(4) ? C02 Ru C03 . . . 36.57(5) ? C02 Ru C04 . . . 61.44(5) ? C02 Ru C05 . . . 61.41(5) ? C03 Ru C04 . . . 37.10(5) ? C03 Ru C05 . . . 61.45(5) ? C04 Ru C05 . . . 36.61(6) ? Ru P1 C111 . . . 119.66(5) ? Ru P1 C121 . . . 120.36(4) ? Ru P1 C10 . . . 107.24(4) ? C111 P1 C121 . . . 101.55(6) ? C111 P1 C10 . . . 100.22(6) ? C121 P1 C10 . . . 105.29(7) ? P1 C111 C112 . . . 121.37(12) ? P1 C111 C116 . . . 119.85(10) ? C112 C111 C116 . . . 118.61(13) ? C111 C112 C113 . . . 120.90(16) ? C111 C112 H112 . . . 119.2(9) ? C113 C112 H112 . . . 119.9(9) ? C112 C113 C114 . . . 119.60(15) ? C112 C113 H113 . . . 119.8(12) ? C114 C113 H113 . . . 120.6(12) ? C113 C114 C115 . . . 120.07(16) ? C113 C114 H114 . . . 118.9(13) ? C115 C114 H114 . . . 121.0(13) ? C114 C115 C116 . . . 120.25(18) ? C114 C115 H115 . . . 123.8(12) ? C116 C115 H115 . . . 115.9(12) ? C111 C116 C115 . . . 120.53(15) ? C111 C116 H116 . . . 119.9(13) ? C115 C116 H116 . . . 119.6(13) ? P1 C121 C122 . . . 120.25(9) ? P1 C121 C126 . . . 121.39(12) ? C122 C121 C126 . . . 118.34(13) ? C121 C122 C123 . . . 120.42(12) ? C121 C122 H122 . . . 120.6(13) ? C123 C122 H122 . . . 118.9(13) ? C122 C123 C124 . . . 120.45(16) ? C122 C123 H123 . . . 119.0(11) ? C124 C123 H123 . . . 120.5(11) ? C123 C124 C125 . . . 119.71(16) ? C123 C124 H124 . . . 122.8(12) ? C125 C124 H124 . . . 117.5(12) ? C124 C125 C126 . . . 119.99(13) ? C124 C125 H125 . . . 118.8(15) ? C126 C125 H125 . . . 121.2(15) ? C121 C126 C125 . . . 121.03(15) ? C121 C126 H126 . . . 119.6(10) ? C125 C126 H126 . . . 119.3(10) ? P1 C10 C20 . . . 107.55(11) ? P1 C10 H10a . . . 109.0(9) ? P1 C10 H10b . . . 107.5(10) ? C20 C10 H10a . . . 112.4(10) ? C20 C10 H10b . . . 110.5(10) ? H10a C10 H10b . . . 109.8(15) ? C10 C20 P2 . . . 110.63(10) ? C10 C20 H20a . . . 113.2(14) ? C10 C20 H20b . . . 110.5(11) ? P2 C20 H20a . . . 107.2(11) ? P2 C20 H20b . . . 109.4(13) ? H20a C20 H20b . . . 105.7(16) ? Ru P2 C20 . . . 111.03(5) ? Ru P2 C211 . . . 116.49(5) ? Ru P2 C221 . . . 120.61(4) ? C20 P2 C211 . . . 104.75(7) ? C20 P2 C221 . . . 102.60(6) ? C211 P2 C221 . . . 99.29(7) ? P2 C211 C212 . . . 123.80(12) ? P2 C211 C216 . . . 118.53(10) ? C212 C211 C216 . . . 117.24(16) ? C211 C212 C213 . . . 121.18(16) ? C211 C212 H212 . . . 120.7(12) ? C213 C212 H212 . . . 118.1(12) ? C212 C213 C214 . . . 120.60(17) ? C212 C213 H213 . . . 118.8(15) ? C214 C213 H213 . . . 120.6(15) ? C213 C214 C215 . . . 119.1(2) ? C213 C214 H214 . . . 120.3(11) ? C215 C214 H214 . . . 120.5(11) ? C214 C215 C216 . . . 120.26(17) ? C214 C215 H215 . . . 121.0(12) ? C216 C215 H215 . . . 118.7(12) ? C211 C216 C215 . . . 121.55(13) ? C211 C216 H216 . . . 117.3(14) ? C215 C216 H216 . . . 121.1(14) ? P2 C221 C222 . . . 121.42(10) ? P2 C221 C226 . . . 119.39(10) ? C222 C221 C226 . . . 119.18(11) ? C221 C222 C223 . . . 119.90(13) ? C221 C222 H222 . . . 118.8(8) ? C223 C222 H222 . . . 121.3(8) ? C222 C223 C224 . . . 120.40(13) ? C222 C223 H223 . . . 118.1(10) ? C224 C223 H223 . . . 121.5(10) ? C223 C224 C225 . . . 120.01(13) ? C223 C224 H224 . . . 116.2(11) ? C225 C224 H224 . . . 123.7(11) ? C224 C225 C226 . . . 119.85(14) ? C224 C225 H225 . . . 121.4(9) ? C226 C225 H225 . . . 118.7(9) ? C221 C226 C225 . . . 120.64(13) ? C221 C226 H226 . . . 122.1(10) ? C225 C226 H226 . . . 117.2(10) ? Ru C1 C2 . . . 173.81(12) ? C1 C2 C3 . . . 176.72(14) ? C2 C3 C4 . . . 178.88(14) ? C3 C4 Si . . . 173.76(14) ? C4 Si C41 . . . 107.03(10) ? C4 Si C42 . . . 110.03(15) ? C4 Si C43 . . . 111.02(13) ? C41 Si C42 . . . 110.18(16) ? C41 Si C43 . . . 109.95(14) ? C42 Si C43 . . . 108.63(18) ? Si C41 H41a . . . 114(2) ? Si C41 H41b . . . 111.1(17) ? Si C41 H41c . . . 107.9(17) ? H41a C41 H41b . . . 110(3) ? H41a C41 H41c . . . 111(3) ? H41b C41 H41c . . . 103(2) ? Si C42 H42a . . . 113.6(16) ? Si C42 H42b . . . 118(3) ? Si C42 H42c . . . 101(2) ? H42a C42 H42b . . . 113(3) ? H42a C42 H42c . . . 105(3) ? H42b C42 H42c . . . 103(3) ? Si C43 H43a . . . 111.3(15) ? Si C43 H43b . . . 96.7(18) ? Si C43 H43c . . . 116.8(16) ? H43a C43 H43b . . . 110(3) ? H43a C43 H43c . . . 110(3) ? H43b C43 H43c . . . 111(3) ? Ru C01 C011 . . . 126.53(12) ? Ru C01 C02 . . . 72.33(8) ? Ru C01 C05 . . . 72.56(7) ? C011 C01 C02 . . . 125.97(12) ? C011 C01 C05 . . . 125.78(14) ? C02 C01 C05 . . . 107.83(14) ? C01 C011 H011a . . . 110.8(14) ? C01 C011 H011b . . . 114.6(16) ? C01 C011 H011c . . . 111.8(14) ? H011a C011 H011b . . . 107.6(17) ? H011a C011 H011c . . . 104.4(19) ? H011b C011 H011c . . . 107(2) ? Ru C02 C01 . . . 70.51(8) ? Ru C02 C021 . . . 129.78(11) ? Ru C02 C03 . . . 72.38(8) ? C01 C02 C021 . . . 123.81(14) ? C01 C02 C03 . . . 108.43(11) ? C021 C02 C03 . . . 127.16(15) ? C02 C021 H021a . . . 106.2(10) ? C02 C021 H021b . . . 112.8(11) ? C02 C021 H021c . . . 112.3(11) ? H021a C021 H021b . . . 109.8(18) ? H021a C021 H021c . . . 112.0(17) ? H021b C021 H021c . . . 103.8(18) ? Ru C03 C02 . . . 71.05(9) ? Ru C03 C031 . . . 132.27(10) ? Ru C03 C04 . . . 70.98(9) ? C02 C03 C031 . . . 126.77(12) ? C02 C03 C04 . . . 107.36(13) ? C031 C03 C04 . . . 124.85(13) ? C03 C031 H031a . . . 111.4(16) ? C03 C031 H031b . . . 117.5(17) ? C03 C031 H031c . . . 113.5(17) ? H031a C031 H031b . . . 117(2) ? H031a C031 H031c . . . 101(2) ? H031b C031 H031c . . . 94(2) ? Ru C04 C03 . . . 71.92(8) ? Ru C04 C041 . . . 130.71(11) ? Ru C04 C05 . . . 71.61(8) ? C03 C04 C041 . . . 125.09(16) ? C03 C04 C05 . . . 108.00(12) ? C041 C04 C05 . . . 125.99(14) ? C04 C041 H041a . . . 110.5(13) ? C04 C041 H041b . . . 115.1(17) ? C04 C041 H041c . . . 114.5(14) ? H041a C041 H041b . . . 105(2) ? H041a C041 H041c . . . 107(2) ? H041b C041 H041c . . . 104(2) ? Ru C05 C01 . . . 70.52(7) ? Ru C05 C04 . . . 71.78(8) ? Ru C05 C051 . . . 127.68(11) ? C01 C05 C04 . . . 108.35(12) ? C01 C05 C051 . . . 124.42(15) ? C04 C05 C051 . . . 127.01(13) ? C05 C051 H051a . . . 109.6(12) ? C05 C051 H051b . . . 112.5(12) ? C05 C051 H051c . . . 112.4(16) ? H051a C051 H051b . . . 105(2) ? H051a C051 H051c . . . 105.1(18) ? H051b C051 H051c . . . 112(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1576 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min -32 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .582 _reflns_d_resolution_low 13.944 _diffrn_reflns_av_sigmaI/netI .095 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .062 _refine_ls_wR_factor_all .038 _refine_ls_goodness_of_fit_all .967 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? data_br801 _database_code_depnum_ccdc_archive 'CCDC 223448' _audit_creation_method Xtal3.6 _audit_creation_date 01-04-20 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C40 H40 P2 Ru1' _chemical_formula_moiety 'C40 H40 P2 Ru1' _chemical_formula_weight 683.78 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 10.3440(10) _cell_length_b 22.719(2) _cell_length_c 14.810(2) _cell_angle_alpha 90.00000 _cell_angle_beta 109.681(2) _cell_angle_gamma 90.00000 _cell_volume 3277.1(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 2842 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 33.5 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu .604 _exptl_crystal_description prism _exptl_crystal_size_max .15 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .06 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .72 _exptl_absorpt_correction_T_max .86 _diffrn_reflns_number 58294 _reflns_number_total 13397 _reflns_Friedel_coverage 0 _reflns_number_gt 6738 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 34.0 _diffrn_reflns_theta_full 34.0 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .098 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .054 _refine_ls_wR_factor_ref .043 _refine_ls_goodness_of_fit_ref 1.243 _refine_ls_number_reflns 6738 _refine_ls_number_parameters 388 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .011 _refine_diff_density_min -1.06 _refine_diff_density_max 1.264 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 160 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 160 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru .65260(3) .103786(14) .27175(2) .01730(12) Uani ? ? 1.00000 ? ? C1 .4599(4) .07709(17) .1987(3) .0241(19) Uani ? ? 1.00000 ? ? C2 .3448(4) .06683(18) .1506(3) .028(2) Uani ? ? 1.00000 ? ? C3 .2113(5) .0613(2) .0879(3) .034(2) Uani ? ? 1.00000 ? ? C4 .0965(5) .0588(3) .0331(4) .055(3) Uani ? ? 1.00000 ? ? P1 .65719(10) .12986(5) .12426(7) .0197(5) Uani ? ? 1.00000 ? ? C111 .7858(4) .18404(18) .1193(3) .0233(19) Uani ? ? 1.00000 ? ? C112 .9237(4) .1687(2) .1440(3) .033(2) Uani ? ? 1.00000 ? ? C113 1.0237(5) .2114(2) .1534(3) .044(3) Uani ? ? 1.00000 ? ? C114 .9876(5) .2699(2) .1394(3) .045(3) Uani ? ? 1.00000 ? ? C115 .8511(5) .2860(2) .1133(3) .039(2) Uani ? ? 1.00000 ? ? C116 .7518(4) .24351(19) .1026(3) .029(2) Uani ? ? 1.00000 ? ? C121 .4992(4) .16094(16) .0384(3) .0198(17) Uani ? ? 1.00000 ? ? C122 .4045(4) .18906(18) .0715(3) .026(2) Uani ? ? 1.00000 ? ? C123 .2818(4) .21088(18) .0091(3) .030(2) Uani ? ? 1.00000 ? ? C124 .2511(4) .20460(18) -.0892(3) .031(2) Uani ? ? 1.00000 ? ? C125 .3440(4) .17784(18) -.1232(3) .029(2) Uani ? ? 1.00000 ? ? C126 .4660(4) .15664(17) -.0605(3) .024(2) Uani ? ? 1.00000 ? ? C11 .6932(4) .06390(18) .0619(3) .024(2) Uani ? ? 1.00000 ? ? C21 .6501(4) .00821(17) .1022(3) .0219(18) Uani ? ? 1.00000 ? ? P2 .71786(10) .01519(4) .23332(7) .0187(4) Uani ? ? 1.00000 ? ? C211 .9002(4) -.00128(17) .2564(3) .0215(18) Uani ? ? 1.00000 ? ? C212 .9426(4) -.05524(18) .2285(3) .028(2) Uani ? ? 1.00000 ? ? C213 1.0795(4) -.0644(2) .2409(3) .032(2) Uani ? ? 1.00000 ? ? C214 1.1747(4) -.0213(2) .2803(3) .034(2) Uani ? ? 1.00000 ? ? C215 1.1354(4) .0319(2) .3069(3) .031(2) Uani ? ? 1.00000 ? ? C216 .9975(4) .04199(18) .2944(3) .025(2) Uani ? ? 1.00000 ? ? C221 .6589(4) -.04968(15) .2818(3) .0191(17) Uani ? ? 1.00000 ? ? C222 .5206(4) -.06514(17) .2485(3) .0224(18) Uani ? ? 1.00000 ? ? C223 .4742(4) -.11229(17) .2896(3) .025(2) Uani ? ? 1.00000 ? ? C224 .5642(4) -.14328(17) .3651(3) .029(2) Uani ? ? 1.00000 ? ? C225 .6999(5) -.12730(18) .3994(3) .031(2) Uani ? ? 1.00000 ? ? C226 .7476(4) -.08171(18) .3578(3) .026(2) Uani ? ? 1.00000 ? ? C01 .6368(4) .10251(19) .4173(2) .0216(17) Uani ? ? 1.00000 ? ? C011 .5694(5) .05541(19) .4563(3) .031(2) Uani ? ? 1.00000 ? ? C02 .7785(4) .10607(18) .4274(2) .0211(16) Uani ? ? 1.00000 ? ? C021 .8862(4) .0630(2) .4851(3) .031(2) Uani ? ? 1.00000 ? ? C03 .8031(4) .15947(17) .3872(3) .0230(19) Uani ? ? 1.00000 ? ? C031 .9383(4) .1864(2) .3925(3) .033(2) Uani ? ? 1.00000 ? ? C04 .6742(4) .19091(17) .3521(3) .0217(18) Uani ? ? 1.00000 ? ? C041 .6568(5) .25241(18) .3153(3) .030(2) Uani ? ? 1.00000 ? ? C05 .5727(4) .15543(17) .3715(3) .0232(19) Uani ? ? 1.00000 ? ? C051 .4258(4) .17186(18) .3531(3) .031(2) Uani ? ? 1.00000 ? ? H4 .00011 .05514 -.01218 .07500 Uiso ? ? 1.00000 ? ? H112 .94847 .12660 .15489 .04000 Uiso ? ? 1.00000 ? ? H113 1.12207 .19992 .17234 .05000 Uiso ? ? 1.00000 ? ? H114 1.05907 .29945 .14726 .05300 Uiso ? ? 1.00000 ? ? H115 .82361 .32757 .10244 .04400 Uiso ? ? 1.00000 ? ? H116 .65462 .25357 .08202 .03900 Uiso ? ? 1.00000 ? ? H122 .42538 .19437 .14027 .03300 Uiso ? ? 1.00000 ? ? H123 .21825 .23058 .03628 .03700 Uiso ? ? 1.00000 ? ? H124 .16089 .21908 -.13251 .04000 Uiso ? ? 1.00000 ? ? H125 .32710 .17461 -.19164 .03700 Uiso ? ? 1.00000 ? ? H126 .52908 .13733 -.08804 .03100 Uiso ? ? 1.00000 ? ? H11a .64292 .06638 -.00647 .03200 Uiso ? ? 1.00000 ? ? H11b .78854 .06167 .06947 .03200 Uiso ? ? 1.00000 ? ? H21a .68680 -.02651 .08227 .02700 Uiso ? ? 1.00000 ? ? H21b .55216 .00432 .07982 .02700 Uiso ? ? 1.00000 ? ? H212 .87377 -.08514 .20064 .03500 Uiso ? ? 1.00000 ? ? H213 1.10780 -.10165 .22218 .04000 Uiso ? ? 1.00000 ? ? H214 1.26919 -.02785 .28862 .04600 Uiso ? ? 1.00000 ? ? H215 1.20365 .06171 .33527 .03800 Uiso ? ? 1.00000 ? ? H216 .96814 .07995 .31011 .02900 Uiso ? ? 1.00000 ? ? H222 .45637 -.04314 .19626 .02600 Uiso ? ? 1.00000 ? ? H223 .37611 -.12241 .26491 .03500 Uiso ? ? 1.00000 ? ? H224 .53036 -.17547 .39402 .03600 Uiso ? ? 1.00000 ? ? H225 .76293 -.14923 .45244 .03900 Uiso ? ? 1.00000 ? ? H226 .84352 -.07075 .38042 .03800 Uiso ? ? 1.00000 ? ? H011a .63254 .02304 .47721 .04300 Uiso ? ? 1.00000 ? ? H011b .49081 .04115 .40515 .04300 Uiso ? ? 1.00000 ? ? H011c .54493 .06888 .50882 .04300 Uiso ? ? 1.00000 ? ? H021a .88468 .06240 .55005 .04600 Uiso ? ? 1.00000 ? ? H021b .97445 .07615 .48752 .04600 Uiso ? ? 1.00000 ? ? H021c .86804 .02401 .46000 .04600 Uiso ? ? 1.00000 ? ? H031a 1.00972 .15760 .40931 .04200 Uiso ? ? 1.00000 ? ? H031b .96435 .21687 .44064 .04200 Uiso ? ? 1.00000 ? ? H031c .93324 .20389 .33255 .04200 Uiso ? ? 1.00000 ? ? H041a .69179 .27969 .36933 .04000 Uiso ? ? 1.00000 ? ? H041b .56184 .26208 .28463 .04000 Uiso ? ? 1.00000 ? ? H041c .70517 .25963 .27285 .04000 Uiso ? ? 1.00000 ? ? H051a .41241 .21200 .33009 .04500 Uiso ? ? 1.00000 ? ? H051b .40670 .17060 .41175 .04500 Uiso ? ? 1.00000 ? ? H051c .36326 .14756 .30497 .04500 Uiso ? ? 1.00000 ? ? 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 .01777(14) .01687(14) .01654(13) -.00024(16) .00482(10) .00047(16) C1 .030(2) .021(2) .019(2) .0103(18) .0058(18) .0017(17) C2 .031(2) .021(2) .035(2) .003(2) .013(2) .002(2) C3 .032(3) .041(3) .031(3) -.001(2) .011(2) -.002(2) C4 .035(3) .082(4) .041(3) -.005(3) .004(2) -.008(3) P1 .0207(5) .0205(5) .0170(5) -.0008(4) .0050(4) .0009(4) C111 .027(2) .029(2) .0151(19) -.0037(18) .0078(17) .0004(17) C112 .029(2) .045(3) .027(2) -.002(2) .013(2) .010(2) C113 .030(3) .069(4) .034(3) -.012(3) .012(2) .012(3) C114 .047(3) .054(3) .030(3) -.031(3) .009(2) .004(2) C115 .056(3) .031(3) .033(3) -.014(2) .017(2) .000(2) C116 .037(3) .029(2) .024(2) -.006(2) .013(2) .0009(19) C121 .019(2) .015(2) .022(2) -.0004(16) .0040(16) .0017(16) C122 .031(2) .025(2) .021(2) .0016(19) .0071(18) .0016(18) C123 .027(2) .026(2) .037(3) .0057(19) .011(2) .004(2) C124 .029(2) .027(2) .032(2) .001(2) .005(2) .005(2) C125 .036(3) .025(2) .021(2) -.002(2) .0031(19) .0030(18) C126 .028(2) .022(2) .025(2) -.0017(18) .0116(18) -.0014(17) C11 .030(2) .023(2) .019(2) .0030(18) .0085(17) -.0001(17) C21 .022(2) .023(2) .018(2) .0037(17) .0040(16) -.0026(16) P2 .0180(5) .0182(5) .0183(5) -.0003(4) .0038(4) -.0002(4) C211 .021(2) .023(2) .021(2) .0011(17) .0080(16) .0019(17) C212 .027(2) .028(2) .029(2) .0022(18) .0089(19) .0004(19) C213 .032(3) .030(2) .037(3) .012(2) .014(2) .002(2) C214 .023(2) .042(3) .038(3) .009(2) .014(2) .007(2) C215 .023(2) .033(3) .036(2) -.005(2) .009(2) .003(2) C216 .025(2) .028(2) .021(2) -.0001(18) .0047(17) .0052(17) C221 .025(2) .0134(17) .019(2) .0006(17) .0069(16) -.0022(16) C222 .025(2) .020(2) .023(2) .0029(17) .0095(17) -.0012(17) C223 .023(2) .020(2) .036(2) -.0032(17) .0131(18) -.0044(18) C224 .038(3) .019(2) .035(2) -.003(2) .018(2) .0038(19) C225 .038(3) .026(2) .027(2) -.002(2) .006(2) .0064(19) C226 .027(2) .026(2) .022(2) -.0031(18) .0039(18) -.0000(18) C01 .027(2) .022(2) .0170(17) .000(2) .0084(15) .000(2) C011 .040(3) .028(2) .029(2) -.005(2) .019(2) .004(2) C02 .029(2) .022(2) .0119(16) .004(2) .0062(15) -.0020(18) C021 .031(2) .036(3) .022(2) .006(2) .0037(18) .001(2) C03 .029(2) .024(2) .0141(18) -.0030(18) .0049(17) -.0073(16) C031 .030(2) .039(3) .032(2) -.011(2) .013(2) -.012(2) C04 .028(2) .021(2) .018(2) .0002(17) .0110(17) -.0045(17) C041 .043(3) .019(2) .031(2) .002(2) .015(2) -.0012(19) C05 .029(2) .022(2) .019(2) .0008(18) .0091(18) -.0029(17) C051 .031(2) .027(2) .037(3) .006(2) .013(2) -.000(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru C1 . . 2.015(4) ? Ru P1 . . 2.2791(12) ? Ru P2 . . 2.2561(11) ? Ru C01 . . 2.216(4) ? Ru C02 . . 2.234(3) ? Ru C03 . . 2.271(3) ? Ru C04 . . 2.281(4) ? Ru C05 . . 2.250(4) ? C1 C2 . . 1.186(5) ? C2 C3 . . 1.387(6) ? C3 C4 . . 1.193(6) ? C4 H4 . . 1.000 ? P1 C111 . . 1.832(4) ? P1 C121 . . 1.840(3) ? P1 C11 . . 1.863(4) ? C111 C112 . . 1.393(6) ? C111 C116 . . 1.397(6) ? C112 C113 . . 1.391(7) ? C112 H112 . . .989 ? C113 C114 . . 1.377(8) ? C113 H113 . . .995 ? C114 C115 . . 1.382(7) ? C114 H114 . . .976 ? C115 C116 . . 1.379(7) ? C115 H115 . . .984 ? C116 H116 . . .974 ? C121 C122 . . 1.390(6) ? C121 C126 . . 1.390(6) ? C122 C123 . . 1.387(5) ? C122 H122 . . .975 ? C123 C124 . . 1.389(6) ? C123 H123 . . .986 ? C124 C125 . . 1.369(7) ? C124 H124 . . .994 ? C125 C126 . . 1.378(5) ? C125 H125 . . .971 ? C126 H126 . . .982 ? C11 C21 . . 1.528(6) ? C11 H11a . . .971 ? C11 H11b . . .955 ? C21 P2 . . 1.836(4) ? C21 H21a . . .964 ? C21 H21b . . .958 ? P2 C211 . . 1.838(4) ? P2 C221 . . 1.831(4) ? C211 C212 . . 1.410(6) ? C211 C216 . . 1.384(5) ? C212 C213 . . 1.381(6) ? C212 H212 . . .970 ? C213 C214 . . 1.372(6) ? C213 H213 . . .966 ? C214 C215 . . 1.375(7) ? C214 H214 . . .955 ? C215 C216 . . 1.394(6) ? C215 H215 . . .967 ? C216 H216 . . .968 ? C221 C222 . . 1.393(6) ? C221 C226 . . 1.394(5) ? C222 C223 . . 1.394(6) ? C222 H222 . . .971 ? C223 C224 . . 1.383(5) ? C223 H223 . . .983 ? C224 C225 . . 1.371(6) ? C224 H224 . . .970 ? C225 C226 . . 1.378(6) ? C225 H225 . . .972 ? C226 H226 . . .966 ? C01 C011 . . 1.495(6) ? C01 C02 . . 1.424(6) ? C01 C05 . . 1.429(5) ? C011 H011a . . .963 ? C011 H011b . . .962 ? C011 H011c . . .947 ? C02 C021 . . 1.512(5) ? C02 C03 . . 1.412(6) ? C021 H021a . . .968 ? C021 H021b . . .949 ? C021 H021c . . .955 ? C03 C031 . . 1.504(6) ? C03 C04 . . 1.446(5) ? C031 H031a . . .955 ? C031 H031b . . .964 ? C031 H031c . . .958 ? C04 C041 . . 1.489(6) ? C04 C05 . . 1.428(6) ? C041 H041a . . .980 ? C041 H041b . . .958 ? C041 H041c . . .940 ? C05 C051 . . 1.498(6) ? C051 H051a . . .967 ? C051 H051b . . .955 ? C051 H051c . . .960 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C1 Ru P1 . . . 84.24(13) ? C1 Ru P2 . . . 85.52(12) ? C1 Ru C01 . . . 97.74(16) ? C1 Ru C02 . . . 133.52(17) ? C1 Ru C03 . . . 151.12(17) ? C1 Ru C04 . . . 116.54(16) ? C1 Ru C05 . . . 89.66(16) ? P1 Ru P2 . . . 83.43(4) ? P1 Ru C01 . . . 165.42(11) ? P1 Ru C02 . . . 142.18(11) ? P1 Ru C03 . . . 110.29(11) ? P1 Ru C04 . . . 104.14(11) ? P1 Ru C05 . . . 128.64(10) ? P2 Ru C01 . . . 111.10(11) ? P2 Ru C02 . . . 99.27(11) ? P2 Ru C03 . . . 119.97(10) ? P2 Ru C04 . . . 157.01(9) ? P2 Ru C05 . . . 146.93(11) ? C01 Ru C02 . . . 37.33(14) ? C01 Ru C03 . . . 62.04(15) ? C01 Ru C04 . . . 62.00(15) ? C01 Ru C05 . . . 37.31(14) ? C02 Ru C03 . . . 36.52(15) ? C02 Ru C04 . . . 61.38(14) ? C02 Ru C05 . . . 61.69(14) ? C03 Ru C04 . . . 37.04(14) ? C03 Ru C05 . . . 61.66(15) ? C04 Ru C05 . . . 36.72(15) ? Ru C1 C2 . . . 173.1(4) ? C1 C2 C3 . . . 172.7(5) ? C2 C3 C4 . . . 177.4(5) ? C3 C4 H4 . . . 177.8 ? Ru P1 C111 . . . 117.59(12) ? Ru P1 C121 . . . 117.50(15) ? Ru P1 C11 . . . 109.79(14) ? C111 P1 C121 . . . 101.66(17) ? C111 P1 C11 . . . 104.5(2) ? C121 P1 C11 . . . 104.20(16) ? P1 C111 C112 . . . 121.0(3) ? P1 C111 C116 . . . 120.9(3) ? C112 C111 C116 . . . 117.6(4) ? C111 C112 C113 . . . 120.8(4) ? C111 C112 H112 . . . 118.1 ? C113 C112 H112 . . . 121.0 ? C112 C113 C114 . . . 120.3(4) ? C112 C113 H113 . . . 120.0 ? C114 C113 H113 . . . 119.7 ? C113 C114 C115 . . . 119.8(5) ? C113 C114 H114 . . . 119.3 ? C115 C114 H114 . . . 120.9 ? C114 C115 C116 . . . 119.9(4) ? C114 C115 H115 . . . 120.8 ? C116 C115 H115 . . . 119.4 ? C111 C116 C115 . . . 121.6(4) ? C111 C116 H116 . . . 117.0 ? C115 C116 H116 . . . 121.4 ? P1 C121 C122 . . . 120.0(3) ? P1 C121 C126 . . . 123.2(3) ? C122 C121 C126 . . . 116.8(3) ? C121 C122 C123 . . . 121.7(4) ? C121 C122 H122 . . . 119.4 ? C123 C122 H122 . . . 118.9 ? C122 C123 C124 . . . 119.8(4) ? C122 C123 H123 . . . 118.5 ? C124 C123 H123 . . . 121.7 ? C123 C124 C125 . . . 119.4(4) ? C123 C124 H124 . . . 118.4 ? C125 C124 H124 . . . 122.2 ? C124 C125 C126 . . . 120.3(4) ? C124 C125 H125 . . . 121.0 ? C126 C125 H125 . . . 118.7 ? C121 C126 C125 . . . 122.1(4) ? C121 C126 H126 . . . 120.4 ? C125 C126 H126 . . . 117.5 ? P1 C11 C21 . . . 109.8(3) ? P1 C11 H11a . . . 110.1 ? P1 C11 H11b . . . 110.8 ? C21 C11 H11a . . . 109.3 ? C21 C11 H11b . . . 109.6 ? H11a C11 H11b . . . 107.2 ? C11 C21 P2 . . . 106.5(2) ? C11 C21 H21a . . . 111.2 ? C11 C21 H21b . . . 110.8 ? P2 C21 H21a . . . 110.2 ? P2 C21 H21b . . . 110.9 ? H21a C21 H21b . . . 107.4 ? Ru P2 C21 . . . 107.68(13) ? Ru P2 C211 . . . 120.67(13) ? Ru P2 C221 . . . 116.87(15) ? C21 P2 C211 . . . 100.46(19) ? C21 P2 C221 . . . 106.62(17) ? C211 P2 C221 . . . 102.67(18) ? P2 C211 C212 . . . 121.6(3) ? P2 C211 C216 . . . 119.4(3) ? C212 C211 C216 . . . 118.8(4) ? C211 C212 C213 . . . 119.9(4) ? C211 C212 H212 . . . 118.5 ? C213 C212 H212 . . . 121.6 ? C212 C213 C214 . . . 120.4(4) ? C212 C213 H213 . . . 119.4 ? C214 C213 H213 . . . 120.2 ? C213 C214 C215 . . . 120.7(4) ? C213 C214 H214 . . . 120.1 ? C215 C214 H214 . . . 119.2 ? C214 C215 C216 . . . 119.7(4) ? C214 C215 H215 . . . 119.8 ? C216 C215 H215 . . . 120.5 ? C211 C216 C215 . . . 120.5(4) ? C211 C216 H216 . . . 119.1 ? C215 C216 H216 . . . 120.3 ? P2 C221 C222 . . . 120.2(3) ? P2 C221 C226 . . . 121.4(3) ? C222 C221 C226 . . . 118.2(4) ? C221 C222 C223 . . . 120.2(3) ? C221 C222 H222 . . . 119.8 ? C223 C222 H222 . . . 120.0 ? C222 C223 C224 . . . 120.5(4) ? C222 C223 H223 . . . 118.8 ? C224 C223 H223 . . . 120.7 ? C223 C224 C225 . . . 119.4(4) ? C223 C224 H224 . . . 119.7 ? C225 C224 H224 . . . 120.9 ? C224 C225 C226 . . . 120.6(4) ? C224 C225 H225 . . . 119.1 ? C226 C225 H225 . . . 120.2 ? C221 C226 C225 . . . 121.1(4) ? C221 C226 H226 . . . 117.7 ? C225 C226 H226 . . . 121.2 ? Ru C01 C011 . . . 125.6(3) ? Ru C01 C02 . . . 72.0(2) ? Ru C01 C05 . . . 72.6(2) ? C011 C01 C02 . . . 126.7(3) ? C011 C01 C05 . . . 125.7(4) ? C02 C01 C05 . . . 107.4(4) ? C01 C011 H011a . . . 108.5 ? C01 C011 H011b . . . 108.5 ? C01 C011 H011c . . . 112.0 ? H011a C011 H011b . . . 107.4 ? H011a C011 H011c . . . 108.8 ? H011b C011 H011c . . . 111.5 ? Ru C02 C01 . . . 70.66(18) ? Ru C02 C021 . . . 129.1(3) ? Ru C02 C03 . . . 73.16(19) ? C01 C02 C021 . . . 124.0(4) ? C01 C02 C03 . . . 109.3(3) ? C021 C02 C03 . . . 126.2(4) ? C02 C021 H021a . . . 108.4 ? C02 C021 H021b . . . 109.5 ? C02 C021 H021c . . . 111.7 ? H021a C021 H021b . . . 107.7 ? H021a C021 H021c . . . 107.9 ? H021b C021 H021c . . . 111.5 ? Ru C03 C02 . . . 70.3(2) ? Ru C03 C031 . . . 131.0(3) ? Ru C03 C04 . . . 71.9(2) ? C02 C03 C031 . . . 128.6(3) ? C02 C03 C04 . . . 107.5(4) ? C031 C03 C04 . . . 123.1(4) ? C03 C031 H031a . . . 111.0 ? C03 C031 H031b . . . 110.7 ? C03 C031 H031c . . . 111.1 ? H031a C031 H031b . . . 107.5 ? H031a C031 H031c . . . 108.7 ? H031b C031 H031c . . . 107.6 ? Ru C04 C03 . . . 71.1(2) ? Ru C04 C041 . . . 130.2(3) ? Ru C04 C05 . . . 70.5(2) ? C03 C04 C041 . . . 125.4(4) ? C03 C04 C05 . . . 107.5(3) ? C041 C04 C05 . . . 126.7(4) ? C04 C041 H041a . . . 109.2 ? C04 C041 H041b . . . 111.5 ? C04 C041 H041c . . . 112.5 ? H041a C041 H041b . . . 106.2 ? H041a C041 H041c . . . 107.6 ? H041b C041 H041c . . . 109.6 ? Ru C05 C01 . . . 70.1(2) ? Ru C05 C04 . . . 72.8(2) ? Ru C05 C051 . . . 125.8(3) ? C01 C05 C04 . . . 108.4(3) ? C01 C05 C051 . . . 125.2(4) ? C04 C05 C051 . . . 126.3(3) ? C05 C051 H051a . . . 108.4 ? C05 C051 H051b . . . 109.6 ? C05 C051 H051c . . . 112.4 ? H051a C051 H051b . . . 107.4 ? H051a C051 H051c . . . 107.5 ? H051b C051 H051c . . . 111.3 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1416 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 35 _reflns_limit_l_min -23 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .635 _reflns_d_resolution_low 11.856 _diffrn_reflns_av_sigmaI/netI .233 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .138 _refine_ls_wR_factor_all .051 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_shift/su_mean .0002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? data_br922 _database_code_depnum_ccdc_archive 'CCDC 223449' _audit_creation_method Xtal3.6 _audit_creation_date 02-10-04 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C63 H50 Au1 P3 Ru1' _chemical_formula_moiety 'C63 H50 Au1 P3 Ru1' _chemical_formula_weight 1198.05 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 8.8840(10) _cell_length_b 31.781(4) _cell_length_c 20.480(3) _cell_angle_alpha 90.00000 _cell_angle_beta 98.529(2) _cell_angle_gamma 90.00000 _cell_volume 5718.4(13) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7736 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 24.5 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 2.947 _exptl_crystal_description flake _exptl_crystal_size_max .21 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .79 _exptl_absorpt_correction_T_max 1.0 _diffrn_reflns_number 53241 _reflns_number_total 10090 _reflns_Friedel_coverage 0 _reflns_number_gt 7035 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .094 _refine_ls_wR_factor_ref .13 _refine_ls_goodness_of_fit_ref 1.313 _refine_ls_number_reflns 7035 _refine_ls_number_parameters 298 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .012 _refine_diff_density_min -2.923 _refine_diff_density_max 3.708 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics 'xtal PIG' _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 252 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 200 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 4 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 12 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au 1.10168(7) .51545(2) .33737(3) .0356(4) Uani ? ? 1.00000 ? ? Ru .71411(12) .72005(4) .20148(6) .0247(6) Uani ? ? 1.00000 ? ? P1 .5194(4) .69090(13) .13030(18) .027(2) Uani ? ? 1.00000 ? ? C111 .4107(17) .7329(5) .0856(7) .029(3) Uiso ? ? 1.00000 ? ? C112 .4567(17) .7529(5) .0317(7) .032(3) Uiso ? ? 1.00000 ? ? C113 .3912(19) .7884(5) .0048(8) .039(4) Uiso ? ? 1.00000 ? ? C114 .275(2) .8081(5) .0328(8) .043(4) Uiso ? ? 1.00000 ? ? C115 .223(2) .7890(5) .0872(9) .043(4) Uiso ? ? 1.00000 ? ? C116 .2943(17) .7525(5) .1143(7) .032(3) Uiso ? ? 1.00000 ? ? C121 .5754(17) .6578(5) .0645(7) .032(3) Uiso ? ? 1.00000 ? ? C122 .709(2) .6344(5) .0776(9) .044(4) Uiso ? ? 1.00000 ? ? C123 .738(2) .6042(6) .0331(10) .055(5) Uiso ? ? 1.00000 ? ? C124 .647(2) .6003(6) -.0246(10) .061(5) Uiso ? ? 1.00000 ? ? C125 .518(2) .6222(6) -.0397(9) .049(5) Uiso ? ? 1.00000 ? ? C126 .4820(18) .6516(5) .0044(8) .038(4) Uiso ? ? 1.00000 ? ? C131 .3803(16) .6538(5) .1541(7) .028(3) Uiso ? ? 1.00000 ? ? C132 .434(2) .6218(6) .1966(9) .049(5) Uiso ? ? 1.00000 ? ? C133 .339(2) .5896(6) .2119(10) .059(5) Uiso ? ? 1.00000 ? ? C134 .187(2) .5899(6) .1839(10) .060(5) Uiso ? ? 1.00000 ? ? C135 .140(2) .6213(6) .1393(10) .060(5) Uiso ? ? 1.00000 ? ? C136 .229(2) .6530(6) .1240(9) .047(4) Uiso ? ? 1.00000 ? ? P2 .5923(4) .73111(12) .29142(18) .0257(19) Uani ? ? 1.00000 ? ? C211 .4532(17) .7738(5) .2888(8) .032(3) Uiso ? ? 1.00000 ? ? C212 .4478(17) .8026(5) .2363(7) .031(3) Uiso ? ? 1.00000 ? ? C213 .343(2) .8367(6) .2322(9) .050(5) Uiso ? ? 1.00000 ? ? C214 .250(2) .8396(6) .2821(10) .056(5) Uiso ? ? 1.00000 ? ? C215 .256(2) .8134(5) .3330(9) .046(4) Uiso ? ? 1.00000 ? ? C216 .3584(18) .7805(5) .3370(8) .037(4) Uiso ? ? 1.00000 ? ? C221 .7353(15) .7469(4) .3619(7) .024(3) Uiso ? ? 1.00000 ? ? C222 .8762(18) .7238(5) .3702(8) .034(4) Uiso ? ? 1.00000 ? ? C223 .9929(19) .7369(5) .4213(8) .039(4) Uiso ? ? 1.00000 ? ? C224 .976(2) .7699(5) .4590(9) .043(4) Uiso ? ? 1.00000 ? ? C225 .841(2) .7934(6) .4503(9) .049(5) Uiso ? ? 1.00000 ? ? C226 .7237(17) .7812(5) .4023(7) .033(4) Uiso ? ? 1.00000 ? ? C231 .4895(16) .6884(4) .3263(7) .027(3) Uiso ? ? 1.00000 ? ? C232 .5698(17) .6579(5) .3675(7) .032(3) Uiso ? ? 1.00000 ? ? C233 .490(2) .6253(5) .3918(9) .044(4) Uiso ? ? 1.00000 ? ? C234 .331(2) .6227(6) .3768(9) .054(5) Uiso ? ? 1.00000 ? ? C235 .2507(19) .6527(5) .3359(8) .040(4) Uiso ? ? 1.00000 ? ? C236 .3306(17) .6851(5) .3100(7) .031(3) Uiso ? ? 1.00000 ? ? C1 .7770(15) .6637(4) .2381(7) .023(3) Uiso ? ? 1.00000 ? ? C2 .8362(17) .6323(5) .2644(7) .031(3) Uiso ? ? 1.00000 ? ? C3 .9053(16) .5963(4) .2894(7) .026(3) Uiso ? ? 1.00000 ? ? C4 .9763(17) .5665(5) .3119(7) .033(4) Uiso ? ? 1.00000 ? ? P 1.2347(5) .45514(13) .3548(2) .034(2) Uani ? ? 1.00000 ? ? C11 1.2048(19) .4253(5) .2792(8) .040(4) Uiso ? ? 1.00000 ? ? C12 1.315(2) .4007(7) .2569(10) .062(5) Uiso ? ? 1.00000 ? ? C13 1.286(3) .3764(7) .1973(12) .074(6) Uiso ? ? 1.00000 ? ? C14 1.150(3) .3838(7) .1582(11) .070(6) Uiso ? ? 1.00000 ? ? C15 1.044(3) .4094(7) .1777(11) .067(6) Uiso ? ? 1.00000 ? ? C16 1.065(2) .4306(6) .2384(10) .055(5) Uiso ? ? 1.00000 ? ? C21 1.438(2) .4606(5) .3748(9) .047(4) Uiso ? ? 1.00000 ? ? C22 1.511(2) .4942(5) .3517(9) .045(4) Uiso ? ? 1.00000 ? ? C23 1.669(2) .4983(7) .3615(10) .059(5) Uiso ? ? 1.00000 ? ? C24 1.759(2) .4684(6) .3987(10) .058(5) Uiso ? ? 1.00000 ? ? C25 1.689(2) .4354(6) .4232(10) .057(5) Uiso ? ? 1.00000 ? ? C26 1.530(2) .4313(6) .4136(9) .047(4) Uiso ? ? 1.00000 ? ? C31 1.1759(16) .4228(5) .4195(7) .029(3) Uiso ? ? 1.00000 ? ? C32 1.1493(18) .4421(5) .4771(8) .038(4) Uiso ? ? 1.00000 ? ? C33 1.1092(19) .4201(5) .5278(8) .040(4) Uiso ? ? 1.00000 ? ? C34 1.0887(18) .3778(5) .5224(8) .036(4) Uiso ? ? 1.00000 ? ? C35 1.1066(19) .3571(5) .4653(8) .041(4) Uiso ? ? 1.00000 ? ? C36 1.1536(18) .3793(5) .4135(8) .035(4) Uiso ? ? 1.00000 ? ? C101 .937(2) .7275(6) .1637(9) .052(5) Uiso ? ? 1.00000 ? ? C102 .822(2) .7448(5) .1170(9) .044(4) Uiso ? ? 1.00000 ? ? C103 .758(2) .7784(5) .1468(9) .045(4) Uiso ? ? 1.00000 ? ? C104 .8303(18) .7825(5) .2133(8) .038(4) Uiso ? ? 1.00000 ? ? C105 .940(2) .7519(5) .2249(8) .044(4) Uiso ? ? 1.00000 ? ? H112 .53581 .73920 .01254 .03800 Uiso ? ? 1.00000 ? ? H113 .42869 .80123 -.03373 .05200 Uiso ? ? 1.00000 ? ? H114 .23420 .83515 .01567 .06100 Uiso ? ? 1.00000 ? ? H115 .13918 .80220 .10702 .06300 Uiso ? ? 1.00000 ? ? H116 .26000 .73873 .15213 .04300 Uiso ? ? 1.00000 ? ? H122 .77870 .63918 .11896 .06000 Uiso ? ? 1.00000 ? ? H123 .82947 .58599 .04356 .06400 Uiso ? ? 1.00000 ? ? H124 .67402 .58006 -.05692 .07300 Uiso ? ? 1.00000 ? ? H125 .44939 .61807 -.08140 .06700 Uiso ? ? 1.00000 ? ? H126 .38811 .66776 -.00545 .05100 Uiso ? ? 1.00000 ? ? H132 .54017 .62357 .21809 .06900 Uiso ? ? 1.00000 ? ? H133 .37863 .56655 .24189 .07800 Uiso ? ? 1.00000 ? ? H134 .11828 .56740 .19161 .07300 Uiso ? ? 1.00000 ? ? H135 .03560 .62018 .11755 .07800 Uiso ? ? 1.00000 ? ? H136 .19229 .67420 .09292 .06600 Uiso ? ? 1.00000 ? ? H212 .51482 .79935 .20388 .04500 Uiso ? ? 1.00000 ? ? H213 .33261 .85747 .19663 .06700 Uiso ? ? 1.00000 ? ? H214 .17695 .86253 .27897 .06800 Uiso ? ? 1.00000 ? ? H215 .18894 .81768 .36552 .06300 Uiso ? ? 1.00000 ? ? H216 .36353 .76029 .37324 .05000 Uiso ? ? 1.00000 ? ? H222 .89201 .70125 .34131 .05800 Uiso ? ? 1.00000 ? ? H223 1.08690 .72149 .42902 .05700 Uiso ? ? 1.00000 ? ? H224 1.05765 .77960 .49105 .05800 Uiso ? ? 1.00000 ? ? H225 .82903 .81654 .47885 .05600 Uiso ? ? 1.00000 ? ? H226 .63066 .79714 .39646 .04400 Uiso ? ? 1.00000 ? ? H232 .67941 .66036 .37748 .04000 Uiso ? ? 1.00000 ? ? H233 .54886 .60367 .42098 .05700 Uiso ? ? 1.00000 ? ? H234 .28052 .59984 .39522 .06200 Uiso ? ? 1.00000 ? ? H235 .14370 .65041 .32325 .05500 Uiso ? ? 1.00000 ? ? H236 .27714 .70543 .28045 .03900 Uiso ? ? 1.00000 ? ? H12 1.41269 .39679 .28480 .08900 Uiso ? ? 1.00000 ? ? H13 1.35865 .35850 .18180 .10000 Uiso ? ? 1.00000 ? ? H14 1.12341 .36975 .11524 .09800 Uiso ? ? 1.00000 ? ? H15 .94358 .41330 .14836 .08900 Uiso ? ? 1.00000 ? ? H16 .98908 .44846 .25279 .07600 Uiso ? ? 1.00000 ? ? H22 1.44870 .51482 .32439 .06500 Uiso ? ? 1.00000 ? ? H23 1.71353 .52186 .34304 .08400 Uiso ? ? 1.00000 ? ? H24 1.86561 .47089 .40512 .07400 Uiso ? ? 1.00000 ? ? H25 1.75296 .41523 .45127 .07900 Uiso ? ? 1.00000 ? ? H26 1.48065 .40744 .43417 .06300 Uiso ? ? 1.00000 ? ? H32 1.15808 .47255 .47898 .04700 Uiso ? ? 1.00000 ? ? H33 1.09227 .43444 .56800 .05200 Uiso ? ? 1.00000 ? ? H34 1.06152 .36197 .55914 .05100 Uiso ? ? 1.00000 ? ? H35 1.09105 .32725 .45988 .05300 Uiso ? ? 1.00000 ? ? H36 1.17156 .36585 .37356 .04700 Uiso ? ? 1.00000 ? ? H101 1.00282 .70441 .15802 .06800 Uiso ? ? 1.00000 ? ? H102 .79057 .73523 .07302 .06200 Uiso ? ? 1.00000 ? ? H103 .67687 .79604 .12653 .05900 Uiso ? ? 1.00000 ? ? H104 .80765 .80442 .24447 .05100 Uiso ? ? 1.00000 ? ? H105 1.00609 .74712 .26571 .05400 Uiso ? ? 1.00000 ? ? 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 Au .0268(4) .0381(4) .0443(4) .0037(3) .0135(3) .0096(3) Ru .0147(6) .0365(7) .0243(6) -.0001(5) .0078(5) .0042(5) P1 .0158(18) .045(2) .0213(19) .0003(16) .0031(15) .0032(17) P2 .0151(18) .038(2) .024(2) .0007(15) .0023(15) .0031(16) P .032(2) .035(2) .040(2) .0009(18) .0178(19) .0045(18) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C4 . . 1.993(15) ? Au P . . 2.253(4) ? Ru P1 . . 2.286(4) ? Ru P2 . . 2.297(4) ? Ru C1 . . 1.990(13) ? Ru C101 . . 2.24(2) ? Ru C102 . . 2.242(18) ? Ru C103 . . 2.230(18) ? Ru C104 . . 2.233(16) ? Ru C105 . . 2.235(17) ? P1 C111 . . 1.814(14) ? P1 C121 . . 1.836(16) ? P1 C131 . . 1.826(15) ? C111 C112 . . 1.39(2) ? C111 C116 . . 1.41(2) ? C112 C113 . . 1.35(2) ? C112 H112 . . .959 ? C113 C114 . . 1.40(3) ? C113 H113 . . .988 ? C114 C115 . . 1.40(3) ? C114 H114 . . .978 ? C115 C116 . . 1.40(2) ? C115 H115 . . .992 ? C116 H116 . . .978 ? C121 C122 . . 1.39(2) ? C121 C126 . . 1.39(2) ? C122 C123 . . 1.38(3) ? C122 H122 . . .984 ? C123 C124 . . 1.34(3) ? C123 H123 . . .99 ? C124 C125 . . 1.34(3) ? C124 H124 . . .98 ? C125 C126 . . 1.37(2) ? C125 H125 . . .980 ? C126 H126 . . .976 ? C131 C132 . . 1.38(2) ? C131 C136 . . 1.39(2) ? C132 C133 . . 1.39(3) ? C132 H132 . . .980 ? C133 C134 . . 1.39(3) ? C133 H133 . . .98 ? C134 C135 . . 1.37(3) ? C134 H134 . . .97 ? C135 C136 . . 1.34(3) ? C135 H135 . . .97 ? C136 H136 . . .952 ? P2 C211 . . 1.831(15) ? P2 C221 . . 1.846(13) ? P2 C231 . . 1.840(15) ? C211 C212 . . 1.41(2) ? C211 C216 . . 1.41(2) ? C212 C213 . . 1.42(2) ? C212 H212 . . .961 ? C213 C214 . . 1.41(3) ? C213 H213 . . .977 ? C214 C215 . . 1.33(3) ? C214 H214 . . .97 ? C215 C216 . . 1.38(2) ? C215 H215 . . .96 ? C216 H216 . . .977 ? C221 C222 . . 1.44(2) ? C221 C226 . . 1.38(2) ? C222 C223 . . 1.42(2) ? C222 H222 . . .953 ? C223 C224 . . 1.32(2) ? C223 H223 . . .961 ? C224 C225 . . 1.40(3) ? C224 H224 . . .951 ? C225 C226 . . 1.38(2) ? C225 H225 . . .956 ? C226 H226 . . .962 ? C231 C232 . . 1.41(2) ? C231 C236 . . 1.41(2) ? C232 C233 . . 1.39(2) ? C232 H232 . . .968 ? C233 C234 . . 1.41(3) ? C233 H233 . . 1.004 ? C234 C235 . . 1.39(2) ? C234 H234 . . .96 ? C235 C236 . . 1.40(2) ? C235 H235 . . .950 ? C236 H236 . . .961 ? C1 C2 . . 1.22(2) ? C2 C3 . . 1.36(2) ? C3 C4 . . 1.19(2) ? P C11 . . 1.802(17) ? P C21 . . 1.802(18) ? P C31 . . 1.812(16) ? C11 C12 . . 1.39(3) ? C11 C16 . . 1.40(2) ? C12 C13 . . 1.43(3) ? C12 H12 . . .97 ? C13 C14 . . 1.37(3) ? C13 H13 . . .95 ? C14 C15 . . 1.35(3) ? C14 H14 . . .98 ? C15 C16 . . 1.40(3) ? C15 H15 . . 1.01 ? C16 H16 . . .96 ? C21 C22 . . 1.37(3) ? C21 C26 . . 1.41(2) ? C22 C23 . . 1.39(3) ? C22 H22 . . .980 ? C23 C24 . . 1.39(3) ? C23 H23 . . .95 ? C24 C25 . . 1.35(3) ? C24 H24 . . .94 ? C25 C26 . . 1.40(3) ? C25 H25 . . .98 ? C26 H26 . . 1.000 ? C31 C32 . . 1.38(2) ? C31 C36 . . 1.40(2) ? C32 C33 . . 1.34(2) ? C32 H32 . . .970 ? C33 C34 . . 1.36(2) ? C33 H33 . . .971 ? C34 C35 . . 1.37(2) ? C34 H34 . . .966 ? C35 C36 . . 1.39(2) ? C35 H35 . . .963 ? C36 H36 . . .957 ? C101 C102 . . 1.40(2) ? C101 C105 . . 1.47(3) ? C101 H101 . . .96 ? C102 C103 . . 1.39(3) ? C102 H102 . . .953 ? C103 C104 . . 1.42(2) ? C103 H103 . . .959 ? C104 C105 . . 1.37(2) ? C104 H104 . . .986 ? C105 H105 . . .961 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C4 Au P . . . 173.7(4) ? P1 Ru P2 . . . 99.88(14) ? P1 Ru C1 . . . 91.1(4) ? P1 Ru C101 . . . 116.5(5) ? P1 Ru C102 . . . 91.1(4) ? P1 Ru C103 . . . 100.9(4) ? P1 Ru C104 . . . 136.3(4) ? P1 Ru C105 . . . 152.9(5) ? P2 Ru C1 . . . 88.6(4) ? P2 Ru C101 . . . 143.6(5) ? P2 Ru C102 . . . 150.6(5) ? P2 Ru C103 . . . 114.5(5) ? P2 Ru C104 . . . 92.4(5) ? P2 Ru C105 . . . 105.9(5) ? C1 Ru C101 . . . 90.7(6) ? C1 Ru C102 . . . 118.6(6) ? C1 Ru C103 . . . 151.3(6) ? C1 Ru C104 . . . 131.3(5) ? C1 Ru C105 . . . 97.7(6) ? C101 Ru C102 . . . 36.5(6) ? C101 Ru C103 . . . 60.6(7) ? C101 Ru C104 . . . 61.7(7) ? C101 Ru C105 . . . 38.3(7) ? C102 Ru C103 . . . 36.3(7) ? C102 Ru C104 . . . 61.8(6) ? C102 Ru C105 . . . 62.2(6) ? C103 Ru C104 . . . 37.2(6) ? C103 Ru C105 . . . 60.8(6) ? C104 Ru C105 . . . 35.7(6) ? Ru P1 C111 . . . 108.6(5) ? Ru P1 C121 . . . 116.0(5) ? Ru P1 C131 . . . 124.7(5) ? C111 P1 C121 . . . 103.5(7) ? C111 P1 C131 . . . 106.2(7) ? C121 P1 C131 . . . 95.3(7) ? P1 C111 C112 . . . 122.8(12) ? P1 C111 C116 . . . 119.0(11) ? C112 C111 C116 . . . 116.7(13) ? C111 C112 C113 . . . 123.3(15) ? C111 C112 H112 . . . 116.0 ? C113 C112 H112 . . . 120.7 ? C112 C113 C114 . . . 120.3(16) ? C112 C113 H113 . . . 119.6 ? C114 C113 H113 . . . 120.0 ? C113 C114 C115 . . . 118.8(15) ? C113 C114 H114 . . . 120.0 ? C115 C114 H114 . . . 121.2 ? C114 C115 C116 . . . 119.4(16) ? C114 C115 H115 . . . 119.7 ? C116 C115 H115 . . . 120.8 ? C111 C116 C115 . . . 121.4(15) ? C111 C116 H116 . . . 117.8 ? C115 C116 H116 . . . 120.7 ? P1 C121 C122 . . . 118.7(11) ? P1 C121 C126 . . . 122.6(12) ? C122 C121 C126 . . . 118.3(15) ? C121 C122 C123 . . . 119.1(15) ? C121 C122 H122 . . . 119.6 ? C123 C122 H122 . . . 121.3 ? C122 C123 C124 . . . 119.9(18) ? C122 C123 H123 . . . 119.5 ? C124 C123 H123 . . . 121 ? C123 C124 C125 . . . 123(2) ? C123 C124 H124 . . . 118 ? C125 C124 H124 . . . 118.5 ? C124 C125 C126 . . . 118.5(17) ? C124 C125 H125 . . . 121.9 ? C126 C125 H125 . . . 119.6 ? C121 C126 C125 . . . 121.0(15) ? C121 C126 H126 . . . 119.1 ? C125 C126 H126 . . . 119.8 ? P1 C131 C132 . . . 117.4(12) ? P1 C131 C136 . . . 122.7(12) ? C132 C131 C136 . . . 119.2(15) ? C131 C132 C133 . . . 121.3(16) ? C131 C132 H132 . . . 117.6 ? C133 C132 H132 . . . 120.9 ? C132 C133 C134 . . . 119.1(18) ? C132 C133 H133 . . . 121.1 ? C134 C133 H133 . . . 120 ? C133 C134 C135 . . . 117(2) ? C133 C134 H134 . . . 122 ? C135 C134 H134 . . . 121 ? C134 C135 C136 . . . 124.9(19) ? C134 C135 H135 . . . 117 ? C136 C135 H135 . . . 118.4 ? C131 C136 C135 . . . 118.1(16) ? C131 C136 H136 . . . 119.7 ? C135 C136 H136 . . . 122.2 ? Ru P2 C211 . . . 119.1(5) ? Ru P2 C221 . . . 108.5(5) ? Ru P2 C231 . . . 121.2(5) ? C211 P2 C221 . . . 101.8(6) ? C211 P2 C231 . . . 100.8(7) ? C221 P2 C231 . . . 102.8(6) ? P2 C211 C212 . . . 116.8(12) ? P2 C211 C216 . . . 124.2(11) ? C212 C211 C216 . . . 118.9(14) ? C211 C212 C213 . . . 119.2(15) ? C211 C212 H212 . . . 120.3 ? C213 C212 H212 . . . 120.4 ? C212 C213 C214 . . . 117.1(16) ? C212 C213 H213 . . . 123.1 ? C214 C213 H213 . . . 119.8 ? C213 C214 C215 . . . 124.9(18) ? C213 C214 H214 . . . 117.3 ? C215 C214 H214 . . . 118 ? C214 C215 C216 . . . 117.8(18) ? C214 C215 H215 . . . 119.9 ? C216 C215 H215 . . . 122.3 ? C211 C216 C215 . . . 122.1(15) ? C211 C216 H216 . . . 118.1 ? C215 C216 H216 . . . 119.8 ? P2 C221 C222 . . . 116.0(10) ? P2 C221 C226 . . . 125.4(10) ? C222 C221 C226 . . . 118.2(12) ? C221 C222 C223 . . . 117.6(14) ? C221 C222 H222 . . . 121.1 ? C223 C222 H222 . . . 121.3 ? C222 C223 C224 . . . 122.1(15) ? C222 C223 H223 . . . 119.4 ? C224 C223 H223 . . . 118.5 ? C223 C224 C225 . . . 120.9(15) ? C223 C224 H224 . . . 121.4 ? C225 C224 H224 . . . 117.6 ? C224 C225 C226 . . . 119.0(16) ? C224 C225 H225 . . . 120.2 ? C226 C225 H225 . . . 120.7 ? C221 C226 C225 . . . 122.2(14) ? C221 C226 H226 . . . 118.7 ? C225 C226 H226 . . . 119.1 ? P2 C231 C232 . . . 120.2(11) ? P2 C231 C236 . . . 120.1(10) ? C232 C231 C236 . . . 119.6(13) ? C231 C232 C233 . . . 119.3(14) ? C231 C232 H232 . . . 118.5 ? C233 C232 H232 . . . 122.2 ? C232 C233 C234 . . . 120.9(15) ? C232 C233 H233 . . . 118.7 ? C234 C233 H233 . . . 120.4 ? C233 C234 C235 . . . 119.9(17) ? C233 C234 H234 . . . 118.0 ? C235 C234 H234 . . . 122.1 ? C234 C235 C236 . . . 119.3(15) ? C234 C235 H235 . . . 120.7 ? C236 C235 H235 . . . 119.8 ? C231 C236 C235 . . . 120.8(13) ? C231 C236 H236 . . . 119.0 ? C235 C236 H236 . . . 120.1 ? Ru C1 C2 . . . 169.9(12) ? C1 C2 C3 . . . 175.7(17) ? C2 C3 C4 . . . 174.9(16) ? Au C4 C3 . . . 172.3(14) ? Au P C11 . . . 107.7(5) ? Au P C21 . . . 116.0(6) ? Au P C31 . . . 113.4(5) ? C11 P C21 . . . 105.1(8) ? C11 P C31 . . . 107.9(7) ? C21 P C31 . . . 106.1(7) ? P C11 C12 . . . 124.1(13) ? P C11 C16 . . . 117.0(14) ? C12 C11 C16 . . . 118.7(16) ? C11 C12 C13 . . . 122.5(18) ? C11 C12 H12 . . . 119 ? C13 C12 H12 . . . 118 ? C12 C13 C14 . . . 116(2) ? C12 C13 H13 . . . 124 ? C14 C13 H13 . . . 120 ? C13 C14 C15 . . . 122(2) ? C13 C14 H14 . . . 121 ? C15 C14 H14 . . . 117 ? C14 C15 C16 . . . 123(2) ? C14 C15 H15 . . . 120 ? C16 C15 H15 . . . 117 ? C11 C16 C15 . . . 117.5(18) ? C11 C16 H16 . . . 119.3 ? C15 C16 H16 . . . 123.2 ? P C21 C22 . . . 120.5(13) ? P C21 C26 . . . 122.9(14) ? C22 C21 C26 . . . 116.6(16) ? C21 C22 C23 . . . 122.8(17) ? C21 C22 H22 . . . 117.5 ? C23 C22 H22 . . . 119.5 ? C22 C23 C24 . . . 120(2) ? C22 C23 H23 . . . 119 ? C24 C23 H23 . . . 121 ? C23 C24 C25 . . . 118.3(19) ? C23 C24 H24 . . . 120 ? C25 C24 H24 . . . 121 ? C24 C25 C26 . . . 121.8(18) ? C24 C25 H25 . . . 118 ? C26 C25 H25 . . . 120 ? C21 C26 C25 . . . 120.4(17) ? C21 C26 H26 . . . 119.1 ? C25 C26 H26 . . . 120.5 ? P C31 C32 . . . 118.5(11) ? P C31 C36 . . . 123.3(12) ? C32 C31 C36 . . . 118.3(14) ? C31 C32 C33 . . . 121.9(15) ? C31 C32 H32 . . . 117.0 ? C33 C32 H32 . . . 121.1 ? C32 C33 C34 . . . 120.0(16) ? C32 C33 H33 . . . 120.2 ? C34 C33 H33 . . . 119.8 ? C33 C34 C35 . . . 120.9(16) ? C33 C34 H34 . . . 119.9 ? C35 C34 H34 . . . 119.2 ? C34 C35 C36 . . . 119.6(15) ? C34 C35 H35 . . . 122.6 ? C36 C35 H35 . . . 117.8 ? C31 C36 C35 . . . 119.3(15) ? C31 C36 H36 . . . 118.5 ? C35 C36 H36 . . . 122.2 ? Ru C101 C102 . . . 71.8(11) ? Ru C101 C105 . . . 70.6(11) ? Ru C101 H101 . . . 123.3 ? C102 C101 C105 . . . 107.1(16) ? C102 C101 H101 . . . 127.9 ? C105 C101 H101 . . . 125.0 ? Ru C102 C101 . . . 71.8(11) ? Ru C102 C103 . . . 71.4(11) ? Ru C102 H102 . . . 121.2 ? C101 C102 C103 . . . 107.7(15) ? C101 C102 H102 . . . 127.0 ? C103 C102 H102 . . . 125.2 ? Ru C103 C102 . . . 72.3(10) ? Ru C103 C104 . . . 71.5(10) ? Ru C103 H103 . . . 121.8 ? C102 C103 C104 . . . 109.6(15) ? C102 C103 H103 . . . 126.1 ? C104 C103 H103 . . . 124.3 ? Ru C104 C103 . . . 71.3(9) ? Ru C104 C105 . . . 72.2(10) ? Ru C104 H104 . . . 124.3 ? C103 C104 C105 . . . 107.9(15) ? C103 C104 H104 . . . 125.4 ? C105 C104 H104 . . . 126.7 ? Ru C105 C101 . . . 71.1(10) ? Ru C105 C104 . . . 72.1(10) ? Ru C105 H105 . . . 121.9 ? C101 C105 C104 . . . 107.7(14) ? C101 C105 H105 . . . 126.1 ? C104 C105 H105 . . . 126.1 ? 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 #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2384 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 37 _reflns_limit_l_min -24 _reflns_limit_l_max 24 _reflns_number_observed ? _reflns_d_resolution_high .84 _reflns_d_resolution_low 12.471 _diffrn_reflns_av_sigmaI/netI .121 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .137 _refine_ls_wR_factor_all .145 _refine_ls_goodness_of_fit_all 1.228 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? data_br903 _database_code_depnum_ccdc_archive 'CCDC 223450' _audit_creation_method Xtal3.6 _audit_creation_date 02-08-01 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C60 H58 Au1 Cl4 P3 Ru1' _chemical_formula_moiety 'C58 H54 Au1 P3 Ru1, C2 H4 Cl4' _chemical_formula_weight 1311.89 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 17.414(2) _cell_length_b 17.739(2) _cell_length_c 17.806(2) _cell_angle_alpha 90.00000 _cell_angle_beta 91.051(3) _cell_angle_gamma 90.00000 _cell_volume 5499.5(11) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 35.5 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 3.259 _exptl_crystal_description prism _exptl_crystal_size_max .2 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .14 _exptl_crystal_size_rad ? _exptl_crystal_colour pale_yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .65 _exptl_absorpt_correction_T_max .75 _diffrn_reflns_number 115669 _reflns_number_total 28997 _reflns_Friedel_coverage 0 _reflns_number_gt 17913 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.6 _diffrn_reflns_theta_full 37.6 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_av_R_equivalents .062 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .041 _refine_ls_wR_factor_ref .043 _refine_ls_goodness_of_fit_ref 1.1 _refine_ls_number_reflns 17913 _refine_ls_number_parameters 663 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .044 _refine_diff_density_min -1.057 _refine_diff_density_max 2.486 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 240 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 232 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 4 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 16 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 12 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .777952(7) -.021046(7) -.041501(7) .01881(5) Uani ? ? 1.00000 ? ? Ru .646429(15) .304099(14) .216156(14) .01808(11) Uani ? ? 1.00000 ? ? P1 .64541(5) .39261(5) .12473(4) .0196(4) Uani ? ? 1.00000 ? ? C111 .61017(19) .48802(18) .14308(18) .0217(15) Uani ? ? 1.00000 ? ? C112 .5970(2) .5411(2) .08526(19) .0269(17) Uani ? ? 1.00000 ? ? C113 .5702(2) .6120(2) .1014(2) .0298(18) Uani ? ? 1.00000 ? ? C114 .5544(2) .63276(19) .1747(2) .0272(17) Uani ? ? 1.00000 ? ? C115 .5669(2) .5821(2) .2321(2) .0275(17) Uani ? ? 1.00000 ? ? C116 .5943(2) .50929(18) .21594(18) .0222(15) Uani ? ? 1.00000 ? ? C121 .7350(2) .4111(2) .07504(17) .0241(16) Uani ? ? 1.00000 ? ? C122 .7695(2) .3538(2) .0340(2) .0300(18) Uani ? ? 1.00000 ? ? C123 .8401(2) .3649(2) .0003(2) .037(2) Uani ? ? 1.00000 ? ? C124 .8775(2) .4335(3) .0068(3) .043(2) Uani ? ? 1.00000 ? ? C125 .8436(3) .4905(3) .0469(3) .050(3) Uani ? ? 1.00000 ? ? C126 .7736(2) .4788(2) .0815(2) .035(2) Uani ? ? 1.00000 ? ? C10 .5750(2) .3623(2) .05236(17) .0250(16) Uani ? ? 1.00000 ? ? C20 .5004(2) .3459(2) .09485(18) .0278(17) Uani ? ? 1.00000 ? ? P2 .52327(5) .28371(5) .17590(5) .0208(4) Uani ? ? 1.00000 ? ? C211 .44540(19) .3026(2) .24102(18) .0226(15) Uani ? ? 1.00000 ? ? C212 .4323(2) .3770(2) .2637(2) .0308(19) Uani ? ? 1.00000 ? ? C213 .3771(2) .3929(2) .3173(2) .036(2) Uani ? ? 1.00000 ? ? C214 .3344(2) .3348(3) .3479(2) .040(2) Uani ? ? 1.00000 ? ? C215 .3462(2) .2619(2) .3257(2) .034(2) Uani ? ? 1.00000 ? ? C216 .4015(2) .2462(2) .2720(2) .0265(17) Uani ? ? 1.00000 ? ? C221 .4952(2) .1904(2) .1397(2) .0276(17) Uani ? ? 1.00000 ? ? C222 .5395(2) .1274(2) .1550(2) .038(2) Uani ? ? 1.00000 ? ? C223 .5207(3) .0579(2) .1242(3) .051(3) Uani ? ? 1.00000 ? ? C224 .4550(3) .0508(3) .0783(3) .053(3) Uani ? ? 1.00000 ? ? C225 .4098(2) .1113(3) .0651(3) .048(3) Uani ? ? 1.00000 ? ? C226 .4284(2) .1822(2) .0946(2) .037(2) Uani ? ? 1.00000 ? ? C1 .6776(2) .23268(19) .13592(18) .0233(15) Uani ? ? 1.00000 ? ? C2 .6992(2) .18311(19) .09367(19) .0242(16) Uani ? ? 1.00000 ? ? C3 .72107(19) .12181(18) .05162(18) .0224(15) Uani ? ? 1.00000 ? ? C4 .7400(2) .06748(19) .01584(18) .0233(16) Uani ? ? 1.00000 ? ? P .82221(5) -.11802(4) -.11140(5) .0184(4) Uani ? ? 1.00000 ? ? C11 .92497(18) -.13665(18) -.09790(17) .0215(15) Uani ? ? 1.00000 ? ? C12 .9548(2) -.2085(2) -.1087(2) .035(2) Uani ? ? 1.00000 ? ? C13 1.0320(2) -.2226(2) -.0952(3) .041(2) Uani ? ? 1.00000 ? ? C14 1.0799(2) -.1658(2) -.0693(2) .034(2) Uani ? ? 1.00000 ? ? C15 1.0503(2) -.0944(2) -.0592(2) .0293(18) Uani ? ? 1.00000 ? ? C16 .9733(2) -.07937(19) -.07328(18) .0234(16) Uani ? ? 1.00000 ? ? C21 .77795(18) -.20870(17) -.09388(18) .0198(14) Uani ? ? 1.00000 ? ? C22 .7626(2) -.2284(2) -.0203(2) .0308(18) Uani ? ? 1.00000 ? ? C23 .7336(2) -.2991(2) -.0037(2) .037(2) Uani ? ? 1.00000 ? ? C24 .7191(2) -.3505(2) -.0607(2) .037(2) Uani ? ? 1.00000 ? ? C25 .7342(2) -.3317(2) -.1346(2) .0308(18) Uani ? ? 1.00000 ? ? C26 .7634(2) -.2611(2) -.1511(2) .0250(16) Uani ? ? 1.00000 ? ? C31 .8070(2) -.09860(17) -.21038(17) .0217(15) Uani ? ? 1.00000 ? ? C32 .7356(2) -.0714(2) -.2334(2) .038(2) Uani ? ? 1.00000 ? ? C33 .7225(3) -.0509(3) -.3082(2) .047(3) Uani ? ? 1.00000 ? ? C34 .7804(3) -.0562(3) -.3588(2) .045(2) Uani ? ? 1.00000 ? ? C35 .8516(3) -.0814(4) -.3361(2) .060(3) Uani ? ? 1.00000 ? ? C36 .8643(2) -.1025(3) -.2616(2) .045(2) Uani ? ? 1.00000 ? ? C101 .7575(2) .2935(2) .2785(2) .0260(16) Uani ? ? 1.00000 ? ? C1011 .8335(2) .2872(2) .2417(2) .037(2) Uani ? ? 1.00000 ? ? C102 .7218(2) .3610(2) .30450(19) .0281(17) Uani ? ? 1.00000 ? ? C1021 .7603(2) .4371(2) .3035(2) .042(2) Uani ? ? 1.00000 ? ? C103 .6516(2) .3421(2) .33869(18) .0277(17) Uani ? ? 1.00000 ? ? C1031 .6007(3) .3923(3) .3833(2) .045(2) Uani ? ? 1.00000 ? ? C104 .6436(2) .2621(2) .33555(18) .0276(17) Uani ? ? 1.00000 ? ? C1041 .5819(2) .2176(3) .3738(2) .042(2) Uani ? ? 1.00000 ? ? C105 .7086(2) .2314(2) .29974(19) .0265(17) Uani ? ? 1.00000 ? ? C1051 .7274(2) .1495(2) .2892(2) .034(2) Uani ? ? 1.00000 ? ? Cl11 .63232(11) .24153(11) -.11348(11) .0507(11) Uani ? ? .6094(14) ? ? Cl12 .48901(14) .15645(13) -.11318(15) .0722(15) Uani ? ? .6094(14) ? ? C01 .5828(5) .1639(5) -.0743(5) .054(5) Uani ? ? .6094(14) ? ? Cl11' .6250(5) .1454(6) -.2001(4) .200(8) Uani ? ? .3906(14) ? ? Cl12' .5248(4) .1863(3) -.0794(3) .118(4) Uani ? ? .3906(14) ? ? C01' .6171(13) .1756(13) -.1137(12) .117(7) Uiso ? ? .3906(14) ? ? Cl21 .50366(16) -.03945(14) -.32635(16) .0771(16) Uani ? ? .6094(14) ? ? Cl22 .56898(15) .09197(13) -.39207(19) .0854(18) Uani ? ? .6094(14) ? ? C02 .4942(9) .0597(9) -.3043(9) .130(5) Uiso ? ? .6094(14) ? ? Cl21' .4841(6) .0007(4) -.2977(6) .204(9) Uani ? ? .3906(14) ? ? Cl22' .5805(4) .1064(3) -.2975(5) .161(6) Uani ? ? .3906(14) ? ? C02' .4924(8) .0719(8) -.3382(8) .060(3) Uiso ? ? .3906(14) ? ? H112 .60852 .52748 .03447 .03400 Uiso ? ? 1.00000 ? ? H113 .56205 .64770 .06092 .03700 Uiso ? ? 1.00000 ? ? H114 .53534 .68243 .18522 .03300 Uiso ? ? 1.00000 ? ? H115 .55650 .59581 .28295 .03300 Uiso ? ? 1.00000 ? ? H116 .60208 .47423 .25620 .02700 Uiso ? ? 1.00000 ? ? H122 .74224 .30642 .02715 .03800 Uiso ? ? 1.00000 ? ? H123 .86280 .32357 -.02785 .04700 Uiso ? ? 1.00000 ? ? H124 .92723 .44023 -.01579 .05300 Uiso ? ? 1.00000 ? ? H125 .86855 .53936 .05120 .06200 Uiso ? ? 1.00000 ? ? H126 .75136 .51996 .10879 .04500 Uiso ? ? 1.00000 ? ? H10a .56812 .40105 .01601 .03100 Uiso ? ? 1.00000 ? ? H10b .59253 .31781 .02844 .03100 Uiso ? ? 1.00000 ? ? H20a .46363 .32384 .06193 .03600 Uiso ? ? 1.00000 ? ? H20b .47949 .39364 .11236 .03600 Uiso ? ? 1.00000 ? ? H212 .46163 .41781 .24123 .03800 Uiso ? ? 1.00000 ? ? H213 .36959 .44399 .33294 .04500 Uiso ? ? 1.00000 ? ? H214 .29519 .34671 .38410 .04800 Uiso ? ? 1.00000 ? ? H215 .31757 .22112 .34672 .04000 Uiso ? ? 1.00000 ? ? H216 .40869 .19510 .25568 .03200 Uiso ? ? 1.00000 ? ? H222 .58453 .13185 .18624 .04700 Uiso ? ? 1.00000 ? ? H223 .55338 .01523 .13408 .06100 Uiso ? ? 1.00000 ? ? H224 .44281 .00286 .05636 .06700 Uiso ? ? 1.00000 ? ? H225 .36492 .10707 .03221 .05900 Uiso ? ? 1.00000 ? ? H226 .39598 .22500 .08535 .04700 Uiso ? ? 1.00000 ? ? H12 .92105 -.24805 -.12512 .04400 Uiso ? ? 1.00000 ? ? H13 1.05203 -.27308 -.10384 .04900 Uiso ? ? 1.00000 ? ? H14 1.13330 -.17693 -.05577 .04300 Uiso ? ? 1.00000 ? ? H15 1.08289 -.05345 -.04203 .03600 Uiso ? ? 1.00000 ? ? H16 .95397 -.02924 -.06684 .02900 Uiso ? ? 1.00000 ? ? H22 .77144 -.19232 .01989 .03600 Uiso ? ? 1.00000 ? ? H23 .72357 -.31233 .04647 .04500 Uiso ? ? 1.00000 ? ? H24 .69842 -.39863 -.04880 .04800 Uiso ? ? 1.00000 ? ? H25 .72381 -.36705 -.17460 .03600 Uiso ? ? 1.00000 ? ? H26 .77408 -.24813 -.20204 .03100 Uiso ? ? 1.00000 ? ? H32 .69462 -.06650 -.19799 .04700 Uiso ? ? 1.00000 ? ? H33 .67179 -.03424 -.32474 .05600 Uiso ? ? 1.00000 ? ? H34 .76954 -.04303 -.41006 .05400 Uiso ? ? 1.00000 ? ? H35 .89151 -.08357 -.37184 .07200 Uiso ? ? 1.00000 ? ? H36 .91532 -.12091 -.24578 .05400 Uiso ? ? 1.00000 ? ? H1011a .85358 .33489 .22663 .05500 Uiso ? ? 1.00000 ? ? H1011b .83175 .25486 .19833 .05500 Uiso ? ? 1.00000 ? ? H1011c .87081 .26702 .27606 .05500 Uiso ? ? 1.00000 ? ? H1021a .72460 .47642 .29299 .06300 Uiso ? ? 1.00000 ? ? H1021b .79998 .43870 .26702 .06300 Uiso ? ? 1.00000 ? ? H1021c .78328 .44757 .35170 .06300 Uiso ? ? 1.00000 ? ? H1031a .55310 .40019 .35725 .06900 Uiso ? ? 1.00000 ? ? H1031b .62489 .44047 .39098 .06900 Uiso ? ? 1.00000 ? ? H1031c .59118 .37067 .43098 .06900 Uiso ? ? 1.00000 ? ? H1041a .53426 .24465 .36962 .06300 Uiso ? ? 1.00000 ? ? H1041b .59479 .21196 .42573 .06300 Uiso ? ? 1.00000 ? ? H1041c .57631 .16878 .35163 .06300 Uiso ? ? 1.00000 ? ? H1051a .76153 .13329 .32848 .05100 Uiso ? ? 1.00000 ? ? H1051b .75191 .14263 .24220 .05100 Uiso ? ? 1.00000 ? ? H1051c .68166 .11956 .29064 .05100 Uiso ? ? 1.00000 ? ? H01a .61183 .11867 -.08573 .07200 Uiso ? ? .6094(14) ? ? H01b .58236 .16965 -.02161 .07200 Uiso ? ? .6094(14) ? ? H02a .44358 .08135 -.31063 .31700 Uiso ? ? .6094(14) ? ? H02b .51303 .07508 -.25516 .31700 Uiso ? ? .6094(14) ? ? H01'a .64523 .13713 -.08451 .16300 Uiso ? ? .3906(14) ? ? H01'b .64594 .22027 -.11149 .16300 Uiso ? ? .3906(14) ? ? H02'a .45525 .11024 -.32277 .07100 Uiso ? ? .3906(14) ? ? H02'b .49844 .06884 -.38607 .07100 Uiso ? ? .3906(14) ? ? 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 Au .01977(5) .01808(5) .01861(5) -.00013(5) .00139(4) -.00456(5) Ru .02094(12) .01858(11) .01469(11) .00305(9) -.00024(9) -.00289(9) P1 .0209(4) .0233(4) .0148(3) .0000(3) .0006(3) -.0022(3) C111 .0209(15) .0257(16) .0186(14) -.0010(12) .0006(11) .0009(12) C112 .035(2) .0271(16) .0186(15) -.0006(14) .0013(14) .0027(13) C113 .032(2) .0297(18) .0278(18) .0018(15) -.0049(15) .0093(14) C114 .0246(17) .0222(16) .0348(19) .0022(13) -.0002(14) .0039(14) C115 .033(2) .0241(16) .0255(17) .0029(14) .0040(14) -.0012(13) C116 .0238(16) .0240(16) .0190(14) .0013(12) .0018(12) .0024(12) C121 .0263(17) .0306(17) .0154(14) -.0019(13) .0010(12) -.0007(13) C122 .031(2) .0300(18) .0295(18) .0053(15) .0085(15) .0014(15) C123 .033(2) .049(2) .0284(19) .0078(18) .0088(16) .0025(17) C124 .024(2) .058(3) .048(3) -.0045(18) .0093(17) .002(2) C125 .034(2) .057(3) .059(3) -.018(2) .013(2) -.013(2) C126 .0275(18) .041(2) .038(2) -.0041(17) .0042(15) -.0138(18) C10 .0290(18) .0312(17) .0147(14) -.0022(14) -.0013(12) -.0015(12) C20 .0260(17) .038(2) .0194(15) -.0063(15) -.0055(13) .0034(14) P2 .0212(4) .0236(4) .0178(4) -.0016(3) .0011(3) -.0024(3) C211 .0215(15) .0277(16) .0187(14) .0017(13) .0003(12) -.0002(12) C212 .0284(19) .0302(18) .034(2) .0013(15) .0008(15) -.0066(15) C213 .030(2) .034(2) .043(2) .0033(16) .0044(17) -.0145(17) C214 .037(2) .051(2) .033(2) .0034(19) .0118(17) -.0117(19) C215 .035(2) .041(2) .0253(17) -.0020(17) .0069(15) -.0003(16) C216 .0312(18) .0239(16) .0246(16) .0013(14) .0020(14) -.0006(13) C221 .0268(17) .0298(17) .0263(17) -.0082(14) .0088(14) -.0091(14) C222 .038(2) .029(2) .048(2) -.0071(16) .0081(19) -.0075(17) C223 .048(3) .027(2) .080(4) -.0047(18) .016(2) -.013(2) C224 .049(3) .039(2) .073(3) -.020(2) .021(2) -.025(2) C225 .031(2) .053(3) .059(3) -.017(2) .013(2) -.030(2) C226 .029(2) .041(2) .043(2) -.0094(16) .0078(17) -.0171(18) C1 .0249(16) .0249(16) .0200(15) .0008(13) .0012(12) -.0009(12) C2 .0267(17) .0236(16) .0224(16) .0017(13) .0001(13) -.0033(12) C3 .0216(15) .0234(15) .0222(16) .0010(13) .0007(12) -.0022(12) C4 .0242(16) .0231(15) .0227(16) -.0003(13) .0033(13) -.0033(12) P .0197(4) .0178(4) .0177(4) -.0010(3) .0005(3) -.0031(3) C11 .0215(16) .0244(15) .0185(14) -.0019(12) .0005(12) -.0016(12) C12 .0241(18) .0278(18) .053(2) .0015(14) -.0043(17) -.0046(17) C13 .024(2) .035(2) .063(3) .0076(16) -.0049(18) -.001(2) C14 .0178(16) .048(2) .037(2) .0006(15) -.0041(14) .0066(18) C15 .0219(17) .042(2) .0239(17) -.0067(15) -.0005(13) -.0013(15) C16 .0241(16) .0243(16) .0218(15) -.0026(13) .0008(12) -.0046(12) C21 .0168(14) .0186(14) .0241(15) -.0008(11) .0007(12) -.0017(12) C22 .032(2) .036(2) .0245(17) -.0112(16) -.0023(14) -.0042(15) C23 .045(2) .038(2) .029(2) -.0124(18) -.0009(17) .0086(17) C24 .036(2) .0293(19) .045(2) -.0101(16) -.0042(18) .0093(17) C25 .0297(19) .0238(17) .039(2) -.0043(14) -.0021(15) -.0064(15) C26 .0233(16) .0256(16) .0262(16) -.0010(13) -.0008(13) -.0037(13) C31 .0279(17) .0189(14) .0182(14) -.0037(12) -.0022(12) -.0025(11) C32 .036(2) .048(2) .030(2) .0096(18) -.0021(16) .0012(18) C33 .046(3) .054(3) .039(2) .008(2) -.016(2) .005(2) C34 .058(3) .052(3) .024(2) -.012(2) -.0089(19) .0075(18) C35 .045(3) .110(5) .026(2) .013(3) .009(2) .013(3) C36 .032(2) .079(3) .0225(18) .011(2) .0045(16) .007(2) C101 .0284(18) .0257(16) .0236(16) .0077(13) -.0058(13) -.0022(13) C1011 .026(2) .039(2) .044(2) .0019(16) -.0027(17) -.0005(18) C102 .037(2) .0240(16) .0224(16) .0073(14) -.0113(14) -.0041(13) C1021 .043(2) .034(2) .047(2) .0014(18) -.021(2) -.0071(18) C103 .0330(19) .0350(18) .0147(14) .0133(15) -.0076(13) -.0048(13) C1031 .059(3) .060(3) .0155(16) .031(2) -.0041(17) -.0100(17) C104 .0321(19) .0331(18) .0173(15) .0021(15) -.0021(13) .0031(13) C1041 .040(2) .058(3) .029(2) .001(2) .0026(17) .015(2) C105 .0319(19) .0251(16) .0222(16) .0044(14) -.0047(14) .0012(13) C1051 .039(2) .0248(17) .037(2) .0071(15) -.0069(17) .0023(15) Cl11 .0518(11) .0432(10) .0571(12) -.0019(8) .0011(9) -.0026(9) Cl12 .0655(14) .0586(13) .0910(17) -.0124(11) -.0368(13) .0272(12) C01 .047(4) .051(5) .064(5) .007(4) -.023(4) .020(4) Cl11' .163(7) .341(12) .096(4) -.121(8) .017(4) -.015(6) Cl12' .148(5) .094(4) .113(4) .031(3) .032(4) -.001(3) Cl21 .0812(18) .0698(15) .0801(17) -.0211(13) -.0045(14) .0225(13) Cl22 .0637(15) .0460(12) .147(3) .0024(11) .0171(16) .0073(15) Cl21' .202(9) .124(5) .284(12) .002(6) -.026(8) .102(7) Cl22' .146(6) .055(3) .281(9) -.026(3) .043(6) .011(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C4 . . 1.992(3) ? Au P . . 2.2666(8) ? Ru P1 . . 2.2616(9) ? Ru P2 . . 2.2777(9) ? Ru C1 . . 1.992(3) ? Ru C101 . . 2.220(3) ? Ru C102 . . 2.267(4) ? Ru C103 . . 2.284(3) ? Ru C104 . . 2.254(3) ? Ru C105 . . 2.234(3) ? P1 C111 . . 1.832(3) ? P1 C121 . . 1.836(3) ? P1 C10 . . 1.842(3) ? C111 C112 . . 1.411(5) ? C111 C116 . . 1.384(5) ? C112 C113 . . 1.374(5) ? C112 H112 . . .961 ? C113 C114 . . 1.388(5) ? C113 H113 . . .968 ? C114 C115 . . 1.375(5) ? C114 H114 . . .961 ? C115 C116 . . 1.409(5) ? C115 H115 . . .958 ? C116 H116 . . .957 ? C121 C122 . . 1.393(5) ? C121 C126 . . 1.381(5) ? C122 C123 . . 1.392(5) ? C122 H122 . . .972 ? C123 C124 . . 1.385(6) ? C123 H123 . . .975 ? C124 C125 . . 1.376(7) ? C124 H124 . . .969 ? C125 C126 . . 1.392(6) ? C125 H125 . . .972 ? C126 H126 . . .962 ? C10 C20 . . 1.544(5) ? C10 H10a . . .951 ? C10 H10b . . .949 ? C20 P2 . . 1.854(4) ? C20 H20a . . .945 ? C20 H20b . . .976 ? P2 C211 . . 1.831(3) ? P2 C221 . . 1.839(4) ? C211 C212 . . 1.400(5) ? C211 C216 . . 1.381(5) ? C212 C213 . . 1.397(6) ? C212 H212 . . .975 ? C213 C214 . . 1.387(6) ? C213 H213 . . .957 ? C214 C215 . . 1.369(6) ? C214 H214 . . .972 ? C215 C216 . . 1.397(5) ? C215 H215 . . .958 ? C216 H216 . . .961 ? C221 C222 . . 1.382(5) ? C221 C226 . . 1.409(5) ? C222 C223 . . 1.387(6) ? C222 H222 . . .956 ? C223 C224 . . 1.399(7) ? C223 H223 . . .962 ? C224 C225 . . 1.349(6) ? C224 H224 . . .958 ? C225 C226 . . 1.399(6) ? C225 H225 . . .971 ? C226 H226 . . .958 ? C1 C2 . . 1.221(5) ? C2 C3 . . 1.378(5) ? C3 C4 . . 1.205(5) ? P C11 . . 1.831(3) ? P C21 . . 1.813(3) ? P C31 . . 1.811(3) ? C11 C12 . . 1.391(5) ? C11 C16 . . 1.385(5) ? C12 C13 . . 1.383(5) ? C12 H12 . . .959 ? C13 C14 . . 1.383(6) ? C13 H13 . . .974 ? C14 C15 . . 1.380(6) ? C14 H14 . . .977 ? C15 C16 . . 1.386(5) ? C15 H15 . . .967 ? C16 H16 . . .959 ? C21 C22 . . 1.386(5) ? C21 C26 . . 1.399(5) ? C22 C23 . . 1.386(6) ? C22 H22 . . .970 ? C23 C24 . . 1.385(6) ? C23 H23 . . .943 ? C24 C25 . . 1.388(6) ? C24 H24 . . .952 ? C25 C26 . . 1.386(5) ? C25 H25 . . .963 ? C26 H26 . . .957 ? C31 C32 . . 1.388(5) ? C31 C36 . . 1.366(5) ? C32 C33 . . 1.396(6) ? C32 H32 . . .965 ? C33 C34 . . 1.367(6) ? C33 H33 . . .972 ? C34 C35 . . 1.372(7) ? C34 H34 . . .957 ? C35 C36 . . 1.391(6) ? C35 H35 . . .953 ? C36 H36 . . .984 ? C101 C1011 . . 1.492(5) ? C101 C102 . . 1.430(5) ? C101 C105 . . 1.447(5) ? C1011 H1011a . . .955 ? C1011 H1011b . . .963 ? C1011 H1011c . . .954 ? C102 C1021 . . 1.507(5) ? C102 C103 . . 1.415(5) ? C1021 H1021a . . .951 ? C1021 H1021b . . .958 ? C1021 H1021c . . .958 ? C103 C1031 . . 1.496(6) ? C103 C104 . . 1.428(5) ? C1031 H1031a . . .953 ? C1031 H1031b . . .961 ? C1031 H1031c . . .949 ? C104 C1041 . . 1.506(6) ? C104 C105 . . 1.417(5) ? C1041 H1041a . . .959 ? C1041 H1041b . . .953 ? C1041 H1041c . . .956 ? C105 C1051 . . 1.501(5) ? C1051 H1051a . . .953 ? C1051 H1051b . . .955 ? C1051 H1051c . . .959 ? Cl11 C01 . . 1.774(8) ? Cl12 C01 . . 1.767(8) ? C01 H01a . . .973 ? C01 H01b . . .944 ? Cl11' C01' . . 1.64(2) ? Cl12' C01' . . 1.74(2) ? C01' H01'a . . .98 ? C01' H01'b . . .94 ? Cl21 C02 . . 1.811(16) ? Cl22 C02 . . 2.132(16) ? C02 H02a . . .965 ? C02 H02b . . .968 ? Cl21' C02' . . 1.463(16) ? Cl22' C02' . . 1.794(16) ? C02' H02'a . . .981 ? C02' H02'b . . .862 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C4 Au P . . . 177.26(12) ? P1 Ru P2 . . . 83.62(3) ? P1 Ru C1 . . . 85.64(10) ? P1 Ru C101 . . . 114.45(9) ? P1 Ru C102 . . . 100.79(9) ? P1 Ru C103 . . . 118.83(9) ? P1 Ru C104 . . . 155.29(10) ? P1 Ru C105 . . . 151.36(9) ? P2 Ru C1 . . . 86.59(10) ? P2 Ru C101 . . . 161.90(9) ? P2 Ru C102 . . . 144.97(9) ? P2 Ru C103 . . . 111.60(9) ? P2 Ru C104 . . . 101.99(9) ? P2 Ru C105 . . . 124.05(10) ? C1 Ru C101 . . . 93.36(13) ? C1 Ru C102 . . . 128.23(13) ? C1 Ru C103 . . . 150.04(13) ? C1 Ru C104 . . . 118.48(13) ? C1 Ru C105 . . . 88.61(13) ? C101 Ru C102 . . . 37.14(13) ? C101 Ru C103 . . . 61.87(13) ? C101 Ru C104 . . . 62.25(13) ? C101 Ru C105 . . . 37.92(13) ? C102 Ru C103 . . . 36.23(13) ? C102 Ru C104 . . . 61.00(13) ? C102 Ru C105 . . . 61.80(12) ? C103 Ru C104 . . . 36.68(13) ? C103 Ru C105 . . . 61.57(13) ? C104 Ru C105 . . . 36.81(13) ? Ru P1 C111 . . . 120.75(11) ? Ru P1 C121 . . . 118.36(11) ? Ru P1 C10 . . . 107.28(11) ? C111 P1 C121 . . . 102.22(15) ? C111 P1 C10 . . . 100.01(15) ? C121 P1 C10 . . . 105.95(15) ? P1 C111 C112 . . . 122.5(2) ? P1 C111 C116 . . . 119.5(2) ? C112 C111 C116 . . . 118.0(3) ? C111 C112 C113 . . . 120.6(3) ? C111 C112 H112 . . . 119.0 ? C113 C112 H112 . . . 120.3 ? C112 C113 C114 . . . 120.9(3) ? C112 C113 H113 . . . 119.2 ? C114 C113 H113 . . . 119.9 ? C113 C114 C115 . . . 119.6(3) ? C113 C114 H114 . . . 120.1 ? C115 C114 H114 . . . 120.3 ? C114 C115 C116 . . . 119.8(3) ? C114 C115 H115 . . . 120.5 ? C116 C115 H115 . . . 119.7 ? C111 C116 C115 . . . 121.0(3) ? C111 C116 H116 . . . 119.8 ? C115 C116 H116 . . . 119.2 ? P1 C121 C122 . . . 120.1(3) ? P1 C121 C126 . . . 122.1(3) ? C122 C121 C126 . . . 117.6(3) ? C121 C122 C123 . . . 121.1(3) ? C121 C122 H122 . . . 118.8 ? C123 C122 H122 . . . 120.0 ? C122 C123 C124 . . . 120.4(4) ? C122 C123 H123 . . . 119.0 ? C124 C123 H123 . . . 120.6 ? C123 C124 C125 . . . 118.9(4) ? C123 C124 H124 . . . 119.7 ? C125 C124 H124 . . . 121.3 ? C124 C125 C126 . . . 120.6(4) ? C124 C125 H125 . . . 120.0 ? C126 C125 H125 . . . 119.4 ? C121 C126 C125 . . . 121.4(4) ? C121 C126 H126 . . . 120.2 ? C125 C126 H126 . . . 118.3 ? P1 C10 C20 . . . 105.5(2) ? P1 C10 H10a . . . 109.8 ? P1 C10 H10b . . . 110.0 ? C20 C10 H10a . . . 111.9 ? C20 C10 H10b . . . 110.1 ? H10a C10 H10b . . . 109.5 ? C10 C20 P2 . . . 108.9(2) ? C10 C20 H20a . . . 109.9 ? C10 C20 H20b . . . 108.4 ? P2 C20 H20a . . . 111.8 ? P2 C20 H20b . . . 110.1 ? H20a C20 H20b . . . 107.7 ? Ru P2 C20 . . . 109.77(12) ? Ru P2 C211 . . . 118.40(11) ? Ru P2 C221 . . . 119.75(12) ? C20 P2 C211 . . . 103.48(15) ? C20 P2 C221 . . . 102.14(16) ? C211 P2 C221 . . . 101.04(16) ? P2 C211 C212 . . . 118.8(3) ? P2 C211 C216 . . . 122.9(3) ? C212 C211 C216 . . . 118.3(3) ? C211 C212 C213 . . . 120.3(3) ? C211 C212 H212 . . . 119.5 ? C213 C212 H212 . . . 120.2 ? C212 C213 C214 . . . 119.9(4) ? C212 C213 H213 . . . 119.3 ? C214 C213 H213 . . . 120.8 ? C213 C214 C215 . . . 120.4(4) ? C213 C214 H214 . . . 119.2 ? C215 C214 H214 . . . 120.4 ? C214 C215 C216 . . . 119.6(4) ? C214 C215 H215 . . . 121.3 ? C216 C215 H215 . . . 119.1 ? C211 C216 C215 . . . 121.5(3) ? C211 C216 H216 . . . 119.1 ? C215 C216 H216 . . . 119.4 ? P2 C221 C222 . . . 120.9(3) ? P2 C221 C226 . . . 120.3(3) ? C222 C221 C226 . . . 118.8(3) ? C221 C222 C223 . . . 120.9(4) ? C221 C222 H222 . . . 119.8 ? C223 C222 H222 . . . 119.3 ? C222 C223 C224 . . . 119.8(4) ? C222 C223 H223 . . . 119.5 ? C224 C223 H223 . . . 120.7 ? C223 C224 C225 . . . 119.8(4) ? C223 C224 H224 . . . 119.4 ? C225 C224 H224 . . . 120.7 ? C224 C225 C226 . . . 121.4(4) ? C224 C225 H225 . . . 120.2 ? C226 C225 H225 . . . 118.3 ? C221 C226 C225 . . . 119.3(4) ? C221 C226 H226 . . . 119.6 ? C225 C226 H226 . . . 121.1 ? Ru C1 C2 . . . 172.2(3) ? C1 C2 C3 . . . 174.0(4) ? C2 C3 C4 . . . 179.0(3) ? Au C4 C3 . . . 176.5(3) ? Au P C11 . . . 113.97(11) ? Au P C21 . . . 115.40(11) ? Au P C31 . . . 110.17(11) ? C11 P C21 . . . 103.58(14) ? C11 P C31 . . . 106.70(15) ? C21 P C31 . . . 106.32(15) ? P C11 C12 . . . 120.9(3) ? P C11 C16 . . . 119.7(2) ? C12 C11 C16 . . . 119.3(3) ? C11 C12 C13 . . . 120.5(3) ? C11 C12 H12 . . . 119.0 ? C13 C12 H12 . . . 120.6 ? C12 C13 C14 . . . 120.2(4) ? C12 C13 H13 . . . 119.3 ? C14 C13 H13 . . . 120.5 ? C13 C14 C15 . . . 119.2(3) ? C13 C14 H14 . . . 120.0 ? C15 C14 H14 . . . 120.6 ? C14 C15 C16 . . . 121.0(3) ? C14 C15 H15 . . . 120.8 ? C16 C15 H15 . . . 118.2 ? C11 C16 C15 . . . 119.8(3) ? C11 C16 H16 . . . 120.4 ? C15 C16 H16 . . . 119.8 ? P C21 C22 . . . 118.4(3) ? P C21 C26 . . . 122.4(2) ? C22 C21 C26 . . . 119.0(3) ? C21 C22 C23 . . . 120.5(3) ? C21 C22 H22 . . . 120.1 ? C23 C22 H22 . . . 119.5 ? C22 C23 C24 . . . 120.1(4) ? C22 C23 H23 . . . 120.2 ? C24 C23 H23 . . . 119.7 ? C23 C24 C25 . . . 120.1(4) ? C23 C24 H24 . . . 119.5 ? C25 C24 H24 . . . 120.3 ? C24 C25 C26 . . . 119.6(3) ? C24 C25 H25 . . . 120.6 ? C26 C25 H25 . . . 119.7 ? C21 C26 C25 . . . 120.6(3) ? C21 C26 H26 . . . 119.6 ? C25 C26 H26 . . . 119.8 ? P C31 C32 . . . 117.9(3) ? P C31 C36 . . . 123.0(3) ? C32 C31 C36 . . . 118.8(3) ? C31 C32 C33 . . . 120.2(4) ? C31 C32 H32 . . . 120.5 ? C33 C32 H32 . . . 119.4 ? C32 C33 C34 . . . 120.1(4) ? C32 C33 H33 . . . 120.0 ? C34 C33 H33 . . . 119.9 ? C33 C34 C35 . . . 120.1(4) ? C33 C34 H34 . . . 118.4 ? C35 C34 H34 . . . 121.5 ? C34 C35 C36 . . . 119.7(4) ? C34 C35 H35 . . . 118.9 ? C36 C35 H35 . . . 121.4 ? C31 C36 C35 . . . 121.2(4) ? C31 C36 H36 . . . 119.5 ? C35 C36 H36 . . . 119.3 ? Ru C101 C1011 . . . 124.0(3) ? Ru C101 C102 . . . 73.2(2) ? Ru C101 C105 . . . 71.6(2) ? C1011 C101 C102 . . . 126.8(3) ? C1011 C101 C105 . . . 126.1(3) ? C102 C101 C105 . . . 106.9(3) ? C101 C1011 H1011a . . . 112.9 ? C101 C1011 H1011b . . . 112.4 ? C101 C1011 H1011c . . . 110.2 ? H1011a C1011 H1011b . . . 108.0 ? H1011a C1011 H1011c . . . 105.4 ? H1011b C1011 H1011c . . . 107.6 ? Ru C102 C101 . . . 69.6(2) ? Ru C102 C1021 . . . 130.0(3) ? Ru C102 C103 . . . 72.5(2) ? C101 C102 C1021 . . . 123.4(3) ? C101 C102 C103 . . . 109.0(3) ? C1021 C102 C103 . . . 127.2(3) ? C102 C1021 H1021a . . . 111.7 ? C102 C1021 H1021b . . . 111.2 ? C102 C1021 H1021c . . . 110.0 ? H1021a C1021 H1021b . . . 108.7 ? H1021a C1021 H1021c . . . 107.1 ? H1021b C1021 H1021c . . . 107.9 ? Ru C103 C102 . . . 71.24(19) ? Ru C103 C1031 . . . 132.1(3) ? Ru C103 C104 . . . 70.53(18) ? C102 C103 C1031 . . . 127.8(3) ? C102 C103 C104 . . . 107.6(3) ? C1031 C103 C104 . . . 123.7(3) ? C103 C1031 H1031a . . . 110.3 ? C103 C1031 H1031b . . . 110.0 ? C103 C1031 H1031c . . . 110.4 ? H1031a C1031 H1031b . . . 108.3 ? H1031a C1031 H1031c . . . 109.3 ? H1031b C1031 H1031c . . . 108.4 ? Ru C104 C103 . . . 72.79(19) ? Ru C104 C1041 . . . 128.9(3) ? Ru C104 C105 . . . 70.81(19) ? C103 C104 C1041 . . . 124.9(3) ? C103 C104 C105 . . . 108.7(3) ? C1041 C104 C105 . . . 125.8(3) ? C104 C1041 H1041a . . . 109.1 ? C104 C1041 H1041b . . . 109.6 ? C104 C1041 H1041c . . . 110.8 ? H1041a C1041 H1041b . . . 108.4 ? H1041a C1041 H1041c . . . 109.9 ? H1041b C1041 H1041c . . . 108.9 ? Ru C105 C101 . . . 70.5(2) ? Ru C105 C104 . . . 72.4(2) ? Ru C105 C1051 . . . 125.4(2) ? C101 C105 C104 . . . 107.7(3) ? C101 C105 C1051 . . . 125.0(3) ? C104 C105 C1051 . . . 127.2(3) ? C105 C1051 H1051a . . . 109.6 ? C105 C1051 H1051b . . . 109.6 ? C105 C1051 H1051c . . . 110.5 ? H1051a C1051 H1051b . . . 108.8 ? H1051a C1051 H1051c . . . 108.7 ? H1051b C1051 H1051c . . . 109.7 ? Cl11 C01 Cl12 . . . 110.9(4) ? Cl11 C01 H01a . . . 107.4(6) ? Cl11 C01 H01b . . . 108.7(6) ? Cl12 C01 H01a . . . 109.7(6) ? Cl12 C01 H01b . . . 112.0(6) ? H01a C01 H01b . . . 108.1(8) ? Cl11' C01' Cl12' . . . 117.4(13) ? Cl11' C01' H01'a . . . 102.7(17) ? Cl11' C01' H01'b . . . 105.1(18) ? Cl12' C01' H01'a . . . 110.2(17) ? Cl12' C01' H01'b . . . 113.0(18) ? H01'a C01' H01'b . . . 108(2) ? Cl21 C02 Cl22 . . . 92.4(7) ? Cl21 C02 H02a . . . 116.6(12) ? Cl21 C02 H02b . . . 116.0(12) ? Cl22 C02 H02a . . . 112.1(11) ? Cl22 C02 H02b . . . 112.7(12) ? H02a C02 H02b . . . 106.8(15) ? Cl21' C02' Cl22' . . . 100.7(9) ? Cl21' C02' H02'a . . . 112.9(12) ? Cl21' C02' H02'b . . . 116.7(13) ? Cl22' C02' H02'a . . . 102.3(10) ? Cl22' C02' H02'b . . . 107.5(12) ? H02'a C02' H02'b . . . 114.5(15) ? 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 #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2616 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 29 _reflns_limit_k_min 0 _reflns_limit_k_max 30 _reflns_limit_l_min -30 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .582 _reflns_d_resolution_low 12.534 _diffrn_reflns_av_sigmaI/netI .145 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .089 _refine_ls_wR_factor_all .049 _refine_ls_goodness_of_fit_all .976 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? data_br896 _database_code_depnum_ccdc_archive 'CCDC 223451' _audit_creation_method Xtal3.6 _audit_creation_date 02-07-03 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C61.125 H60.25 Au1 Cl.25 P3 Ru1' _chemical_formula_moiety ? _chemical_formula_weight 1194.73 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 17.3282(7) _cell_length_b 12.8802(5) _cell_length_c 23.7007(10) _cell_angle_alpha 90.00000 _cell_angle_beta 96.4230(10) _cell_angle_gamma 90.00000 _cell_volume 5256.6(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 35.4 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 3.217 _exptl_crystal_description prism _exptl_crystal_size_max .2 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .14 _exptl_crystal_size_rad ? _exptl_crystal_colour golden _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .63 _exptl_absorpt_correction_T_max .77 _diffrn_reflns_number 108768 _reflns_number_total 27598 _reflns_Friedel_coverage 0 _reflns_number_gt 20068 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.6 _diffrn_reflns_theta_full 37.6 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_av_R_equivalents .033 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .027 _refine_ls_wR_factor_ref .027 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_number_reflns 20068 _refine_ls_number_parameters 608 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .014 _refine_diff_density_min -.626 _refine_diff_density_max 1.68 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 244.5 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 241 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 4 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 1 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 12 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au -.177341(4) .414309(5) .218976(3) .02395(3) Uani ? ? 1.00000 ? ? Ru .183790(7) .187231(9) .095418(5) .01603(5) Uani ? ? 1.00000 ? ? P1 .23188(2) .34796(3) .084555(17) .01753(16) Uani ? ? 1.00000 ? ? C111 .33077(9) .36459(13) .06471(7) .0222(7) Uani ? ? 1.00000 ? ? C112 .36217(11) .46403(15) .05886(8) .0297(9) Uani ? ? 1.00000 ? ? C113 .44092(13) .47660(18) .05590(10) .0407(11) Uani ? ? 1.00000 ? ? C114 .48946(12) .3909(2) .05764(10) .0428(11) Uani ? ? 1.00000 ? ? C115 .45904(11) .29269(17) .06113(9) .0365(10) Uani ? ? 1.00000 ? ? C116 .37972(10) .27945(14) .06449(8) .0264(8) Uani ? ? 1.00000 ? ? C121 .17753(10) .44365(13) .03963(7) .0234(7) Uani ? ? 1.00000 ? ? C122 .12191(15) .5045(2) .06050(9) .0575(14) Uani ? ? 1.00000 ? ? C123 .0798(2) .5751(3) .02510(12) .094(2) Uani ? ? 1.00000 ? ? C124 .09168(18) .5835(2) -.03181(11) .0617(16) Uani ? ? 1.00000 ? ? C125 .14468(13) .52104(16) -.05310(8) .0350(9) Uani ? ? 1.00000 ? ? C126 .18751(12) .45159(14) -.01780(8) .0293(8) Uani ? ? 1.00000 ? ? C10 .24601(9) .40900(12) .15525(7) .0190(6) Uani ? ? 1.00000 ? ? C20 .29381(9) .33289(12) .19428(7) .0198(6) Uani ? ? 1.00000 ? ? P2 .25447(2) .19896(3) .182187(17) .01613(16) Uani ? ? 1.00000 ? ? C211 .33984(9) .11525(12) .19690(7) .0190(6) Uani ? ? 1.00000 ? ? C212 .41211(10) .14210(14) .18142(7) .0261(8) Uani ? ? 1.00000 ? ? C213 .47313(11) .07102(17) .18672(9) .0345(9) Uani ? ? 1.00000 ? ? C214 .46281(12) -.02606(17) .20853(9) .0377(10) Uani ? ? 1.00000 ? ? C215 .39155(13) -.05423(15) .22503(8) .0334(9) Uani ? ? 1.00000 ? ? C216 .33049(10) .01608(13) .21921(7) .0238(7) Uani ? ? 1.00000 ? ? C221 .20684(9) .17766(12) .24695(7) .0202(7) Uani ? ? 1.00000 ? ? C222 .13190(10) .13681(14) .24328(8) .0260(8) Uani ? ? 1.00000 ? ? C223 .09406(11) .12855(17) .29183(9) .0357(10) Uani ? ? 1.00000 ? ? C224 .13013(13) .16149(16) .34374(9) .0370(10) Uani ? ? 1.00000 ? ? C225 .20508(13) .19852(15) .34829(8) .0324(9) Uani ? ? 1.00000 ? ? C226 .24387(11) .20527(13) .30014(7) .0250(8) Uani ? ? 1.00000 ? ? C1 .09907(9) .26266(12) .12865(7) .0193(6) Uani ? ? 1.00000 ? ? C2 .04136(9) .29865(12) .14694(7) .0208(7) Uani ? ? 1.00000 ? ? C3 -.02574(9) .33173(13) .16772(7) .0213(7) Uani ? ? 1.00000 ? ? C4 -.08488(10) .36041(14) .18575(7) .0242(7) Uani ? ? 1.00000 ? ? P -.28236(3) .48033(4) .25562(2) .0252(2) Uani ? ? 1.00000 ? ? C11 -.33646(10) .56692(13) .20536(8) .0243(7) Uani ? ? 1.00000 ? ? C12 -.37732(10) .65158(14) .22351(7) .0269(8) Uani ? ? 1.00000 ? ? C13 -.41495(11) .71937(15) .18453(8) .0302(9) Uani ? ? 1.00000 ? ? C14 -.41335(11) .70648(16) .12667(8) .0312(9) Uani ? ? 1.00000 ? ? C141 -.45413(15) .7833(2) .08535(10) .0479(13) Uani ? ? 1.00000 ? ? C15 -.37266(12) .62188(18) .10854(8) .0360(10) Uani ? ? 1.00000 ? ? C16 -.33447(11) .55306(16) .14729(8) .0327(9) Uani ? ? 1.00000 ? ? C21 -.34986(10) .38261(14) .27591(8) .0259(8) Uani ? ? 1.00000 ? ? C22 -.31943(11) .29353(15) .30363(9) .0312(9) Uani ? ? 1.00000 ? ? C23 -.36803(12) .21812(16) .32238(9) .0336(9) Uani ? ? 1.00000 ? ? C24 -.44819(11) .22886(15) .31322(8) .0302(9) Uani ? ? 1.00000 ? ? C241 -.50103(14) .14808(18) .33443(9) .0416(11) Uani ? ? 1.00000 ? ? C25 -.47788(11) .31713(17) .28504(10) .0375(10) Uani ? ? 1.00000 ? ? C26 -.42986(11) .39322(16) .26618(10) .0363(10) Uani ? ? 1.00000 ? ? C31 -.26014(10) .56071(14) .31839(8) .0266(8) Uani ? ? 1.00000 ? ? C32 -.19702(11) .62850(18) .32005(9) .0354(10) Uani ? ? 1.00000 ? ? C33 -.18054(12) .69639(18) .36513(9) .0396(11) Uani ? ? 1.00000 ? ? C34 -.22591(12) .69829(16) .41040(9) .0355(10) Uani ? ? 1.00000 ? ? C341 -.20682(15) .77240(19) .45940(10) .0472(12) Uani ? ? 1.00000 ? ? C35 -.28818(12) .63089(17) .40859(9) .0362(10) Uani ? ? 1.00000 ? ? C36 -.30565(11) .56253(16) .36327(9) .0334(9) Uani ? ? 1.00000 ? ? C101 .11731(10) .13798(13) .01381(7) .0248(7) Uani ? ? 1.00000 ? ? C1011 .06509(13) .20548(16) -.02509(9) .0393(10) Uani ? ? 1.00000 ? ? C102 .19770(11) .11628(13) .01033(7) .0255(8) Uani ? ? 1.00000 ? ? C1021 .24341(14) .15621(18) -.03562(8) .0394(11) Uani ? ? 1.00000 ? ? C103 .22344(10) .04227(13) .05288(8) .0260(8) Uani ? ? 1.00000 ? ? C1031 .30100(13) -.01204(16) .05963(10) .0408(11) Uani ? ? 1.00000 ? ? C104 .15844(11) .01519(13) .08264(7) .0266(8) Uani ? ? 1.00000 ? ? C1041 .15700(16) -.07043(15) .12519(10) .0435(11) Uani ? ? 1.00000 ? ? C105 .09304(10) .07351(13) .05827(8) .0268(8) Uani ? ? 1.00000 ? ? C1051 .01203(13) .06548(17) .07412(10) .0420(11) Uani ? ? 1.00000 ? ? Cl -.0619(3) .5491(3) .46074(19) .104(3) Uani ? ? .25000 ? ? C0 .0185(11) .5154(14) .4692(8) .040(4) Uiso ? ? .12500 ? ? H112 .32852 .52408 .05627 .03700 Uiso ? ? 1.00000 ? ? H113 .46268 .54461 .05327 .05100 Uiso ? ? 1.00000 ? ? H114 .54430 .39938 .05710 .05200 Uiso ? ? 1.00000 ? ? H115 .49285 .23340 .06165 .04500 Uiso ? ? 1.00000 ? ? H116 .35886 .21071 .06628 .03300 Uiso ? ? 1.00000 ? ? H122 .11147 .49713 .09936 .07100 Uiso ? ? 1.00000 ? ? H123 .04091 .61792 .04006 .12100 Uiso ? ? 1.00000 ? ? H124 .06215 .63265 -.05604 .08000 Uiso ? ? 1.00000 ? ? H125 .15281 .52578 -.09225 .04500 Uiso ? ? 1.00000 ? ? H126 .22527 .40818 -.03295 .03600 Uiso ? ? 1.00000 ? ? H10a .27330 .47353 .15352 .02400 Uiso ? ? 1.00000 ? ? H10b .19737 .42234 .16892 .02400 Uiso ? ? 1.00000 ? ? H20a .29144 .35211 .23286 .02500 Uiso ? ? 1.00000 ? ? H20b .34649 .33460 .18643 .02500 Uiso ? ? 1.00000 ? ? H212 .42064 .21064 .16745 .03300 Uiso ? ? 1.00000 ? ? H213 .52226 .08995 .17456 .04300 Uiso ? ? 1.00000 ? ? H214 .50556 -.07428 .21267 .04500 Uiso ? ? 1.00000 ? ? H215 .38475 -.12231 .24033 .04200 Uiso ? ? 1.00000 ? ? H216 .28098 -.00290 .23123 .03000 Uiso ? ? 1.00000 ? ? H222 .10630 .11477 .20713 .03300 Uiso ? ? 1.00000 ? ? H223 .04250 .10092 .28927 .04400 Uiso ? ? 1.00000 ? ? H224 .10306 .15880 .37678 .04500 Uiso ? ? 1.00000 ? ? H225 .23021 .21984 .38445 .04100 Uiso ? ? 1.00000 ? ? H226 .29668 .22886 .30325 .03200 Uiso ? ? 1.00000 ? ? H12 -.37901 .66293 .26317 .03400 Uiso ? ? 1.00000 ? ? H13 -.44287 .77707 .19810 .03700 Uiso ? ? 1.00000 ? ? H141a -.46056 .84707 .10449 .07100 Uiso ? ? 1.00000 ? ? H141b -.50460 .75642 .07201 .07100 Uiso ? ? 1.00000 ? ? H141c -.42561 .79310 .05379 .07100 Uiso ? ? 1.00000 ? ? H15 -.37163 .61207 .06836 .04500 Uiso ? ? 1.00000 ? ? H16 -.30591 .49495 .13448 .04100 Uiso ? ? 1.00000 ? ? H22 -.26382 .28512 .31008 .03800 Uiso ? ? 1.00000 ? ? H23 -.34521 .15785 .34192 .04200 Uiso ? ? 1.00000 ? ? H241a -.55021 .15181 .31181 .06300 Uiso ? ? 1.00000 ? ? H241b -.50802 .16424 .37270 .06300 Uiso ? ? 1.00000 ? ? H241c -.47966 .08067 .33115 .06300 Uiso ? ? 1.00000 ? ? H25 -.53340 .32507 .27741 .04600 Uiso ? ? 1.00000 ? ? H26 -.45209 .45294 .24654 .04500 Uiso ? ? 1.00000 ? ? H32 -.16476 .62789 .29000 .04300 Uiso ? ? 1.00000 ? ? H33 -.13772 .74286 .36483 .04900 Uiso ? ? 1.00000 ? ? H341a -.24586 .76636 .48473 .07200 Uiso ? ? 1.00000 ? ? H341b -.20622 .84118 .44552 .07200 Uiso ? ? 1.00000 ? ? H341c -.15768 .75507 .47960 .07200 Uiso ? ? 1.00000 ? ? H35 -.32012 .63105 .43896 .04400 Uiso ? ? 1.00000 ? ? H36 -.34922 .51660 .36295 .04200 Uiso ? ? 1.00000 ? ? H1011a .04909 .16937 -.05929 .06100 Uiso ? ? 1.00000 ? ? H1011b .09145 .26723 -.03327 .06100 Uiso ? ? 1.00000 ? ? H1011c .01994 .22376 -.00702 .06100 Uiso ? ? 1.00000 ? ? H1021a .21643 .21301 -.05473 .05900 Uiso ? ? 1.00000 ? ? H1021b .24967 .10267 -.06227 .05900 Uiso ? ? 1.00000 ? ? H1021c .29330 .17988 -.01936 .05900 Uiso ? ? 1.00000 ? ? H1031a .31552 -.02639 .09902 .06200 Uiso ? ? 1.00000 ? ? H1031b .33939 .03273 .04665 .06200 Uiso ? ? 1.00000 ? ? H1031c .29862 -.07445 .03840 .06200 Uiso ? ? 1.00000 ? ? H1041a .12294 -.05313 .15270 .06500 Uiso ? ? 1.00000 ? ? H1041b .20777 -.08203 .14415 .06500 Uiso ? ? 1.00000 ? ? H1041c .13891 -.13278 .10666 .06500 Uiso ? ? 1.00000 ? ? H1051a -.00927 .13402 .07500 .06400 Uiso ? ? 1.00000 ? ? H1051b .01363 .03550 .11066 .06400 Uiso ? ? 1.00000 ? ? H1051c -.01891 .02363 .04717 .06400 Uiso ? ? 1.00000 ? ? H0a .05231 .57026 .46343 .16100 Uiso ? ? .12500 ? ? H0b .02504 .46212 .44027 .16100 Uiso ? ? .12500 ? ? 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 Au .01774(3) .02920(3) .02565(3) .00489(2) .00564(2) .00179(3) Ru .01615(5) .01510(5) .01643(5) .00184(4) .00000(4) -.00126(4) P1 .01919(18) .01723(17) .01622(17) .00182(14) .00225(14) .00111(14) C111 .0228(7) .0258(8) .0185(7) -.0012(6) .0045(6) -.0008(6) C112 .0318(9) .0298(9) .0296(9) -.0040(7) .0120(7) -.0010(7) C113 .0368(11) .0429(11) .0455(12) -.0134(9) .0181(9) -.0047(10) C114 .0250(9) .0618(15) .0437(12) -.0064(9) .0125(9) -.0010(11) C115 .0260(9) .0479(12) .0367(11) .0060(8) .0082(8) .0016(9) C116 .0237(8) .0315(9) .0249(8) .0036(7) .0060(6) .0022(7) C121 .0262(8) .0224(7) .0209(7) .0029(6) -.0001(6) .0039(6) C122 .0655(16) .0798(18) .0293(10) .0522(14) .0147(10) .0207(11) C123 .115(3) .131(3) .0418(14) .102(2) .0281(16) .0358(17) C124 .0733(19) .0749(18) .0365(12) .0457(15) .0046(12) .0223(12) C125 .0455(12) .0370(10) .0216(8) .0052(9) .0003(8) .0077(8) C126 .0408(10) .0263(8) .0206(8) .0046(7) .0033(7) .0019(7) C10 .0222(7) .0166(6) .0183(7) .0008(5) .0028(5) .0002(5) C20 .0217(7) .0178(7) .0194(7) -.0010(5) .0009(6) -.0000(5) P2 .01630(16) .01526(16) .01662(17) .00111(13) .00093(13) .00080(13) C211 .0204(7) .0199(7) .0159(7) .0040(5) -.0005(5) .0007(5) C212 .0217(8) .0315(9) .0249(8) .0054(7) .0017(6) .0037(7) C213 .0219(8) .0476(12) .0338(10) .0115(8) .0027(7) .0036(9) C214 .0370(11) .0406(11) .0335(10) .0229(9) -.0041(8) -.0039(9) C215 .0451(11) .0237(8) .0301(9) .0124(8) -.0025(8) .0023(7) C216 .0277(8) .0198(7) .0233(8) .0033(6) .0000(6) .0013(6) C221 .0225(7) .0179(7) .0204(7) .0029(5) .0043(6) .0023(6) C222 .0228(8) .0259(8) .0298(9) .0013(6) .0047(6) .0057(7) C223 .0272(9) .0379(10) .0443(12) .0032(8) .0139(8) .0123(9) C224 .0440(11) .0353(10) .0360(10) .0120(9) .0232(9) .0109(8) C225 .0483(12) .0279(9) .0225(8) .0061(8) .0100(8) .0005(7) C226 .0305(9) .0241(8) .0207(7) -.0004(6) .0039(6) .0002(6) C1 .0192(7) .0188(7) .0193(7) .0013(5) -.0006(5) .0003(5) C2 .0198(7) .0217(7) .0202(7) .0014(6) -.0002(6) .0016(6) C3 .0207(7) .0223(7) .0204(7) .0026(6) .0001(6) .0017(6) C4 .0210(7) .0287(8) .0228(8) .0027(6) .0028(6) .0020(7) P .01863(19) .0292(2) .0282(2) .00355(16) .00497(16) -.00087(18) C11 .0188(7) .0281(8) .0265(8) .0011(6) .0047(6) -.0013(6) C12 .0271(8) .0295(8) .0244(8) .0029(7) .0036(7) -.0028(7) C13 .0307(9) .0283(9) .0314(9) .0053(7) .0025(7) -.0031(7) C14 .0270(9) .0371(10) .0291(9) .0020(7) .0019(7) .0029(8) C141 .0520(14) .0559(14) .0357(12) .0147(11) .0043(10) .0110(11) C15 .0328(10) .0505(12) .0250(9) .0080(9) .0047(7) -.0031(9) C16 .0300(9) .0393(10) .0289(9) .0086(8) .0041(7) -.0076(8) C21 .0207(7) .0284(8) .0289(9) .0026(6) .0043(6) -.0030(7) C22 .0262(9) .0351(10) .0327(10) .0048(7) .0049(7) .0040(8) C23 .0345(10) .0346(10) .0320(10) .0034(8) .0044(8) .0020(8) C24 .0340(10) .0334(9) .0238(8) -.0070(7) .0060(7) -.0043(7) C241 .0497(13) .0437(12) .0312(10) -.0188(10) .0040(9) -.0002(9) C25 .0229(9) .0390(11) .0500(13) -.0036(8) .0011(8) .0029(10) C26 .0246(9) .0342(10) .0499(12) .0017(7) .0033(8) .0083(9) C31 .0214(8) .0316(9) .0266(8) .0036(6) .0018(6) .0006(7) C32 .0273(9) .0477(12) .0316(10) -.0045(8) .0047(7) -.0024(9) C33 .0324(10) .0468(12) .0384(11) -.0101(9) -.0010(8) -.0028(10) C34 .0357(10) .0364(10) .0328(10) .0040(8) -.0025(8) -.0018(8) C341 .0538(14) .0444(13) .0427(13) -.0011(11) .0019(11) -.0101(10) C35 .0349(10) .0436(11) .0310(10) .0016(9) .0077(8) -.0044(9) C36 .0283(9) .0393(10) .0334(10) -.0014(8) .0071(8) -.0027(8) C101 .0286(8) .0203(7) .0237(8) .0007(6) -.0054(6) -.0055(6) C1011 .0450(12) .0295(10) .0380(11) .0039(8) -.0191(9) .0002(8) C102 .0332(9) .0221(7) .0206(8) .0012(6) .0008(7) -.0062(6) C1021 .0521(13) .0421(11) .0251(9) -.0055(10) .0094(9) -.0091(8) C103 .0299(9) .0210(7) .0261(8) .0061(6) -.0019(7) -.0069(6) C1031 .0401(11) .0342(10) .0456(12) .0172(9) -.0062(9) -.0142(9) C104 .0373(9) .0196(7) .0218(8) -.0042(7) -.0021(7) -.0039(6) C1041 .0704(16) .0217(9) .0361(11) -.0086(9) -.0048(11) .0029(8) C105 .0260(8) .0225(8) .0306(9) -.0052(6) -.0018(7) -.0079(7) C1051 .0318(10) .0441(12) .0500(13) -.0150(9) .0044(9) -.0182(10) Cl .161(4) .0450(16) .118(3) -.012(2) .073(3) .0065(19) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C4 . . 1.9878(17) ? Au P . . 2.2677(5) ? Ru P1 . . 2.2571(4) ? Ru P2 . . 2.2778(4) ? Ru C1 . . 1.9945(16) ? Ru C101 . . 2.2297(17) ? Ru C102 . . 2.2514(18) ? Ru C103 . . 2.2649(18) ? Ru C104 . . 2.2728(17) ? Ru C105 . . 2.2546(17) ? P1 C111 . . 1.8395(17) ? P1 C121 . . 1.8209(17) ? P1 C10 . . 1.8422(16) ? C111 C112 . . 1.404(3) ? C111 C116 . . 1.387(2) ? C112 C113 . . 1.384(3) ? C112 H112 . . .9665 ? C113 C114 . . 1.385(3) ? C113 H113 . . .958 ? C114 C115 . . 1.377(3) ? C114 H114 . . .958 ? C115 C116 . . 1.396(3) ? C115 H115 . . .962 ? C116 H116 . . .9591 ? C121 C122 . . 1.376(3) ? C121 C126 . . 1.395(3) ? C122 C123 . . 1.388(4) ? C122 H122 . . .963 ? C123 C124 . . 1.391(4) ? C123 H123 . . .968 ? C124 C125 . . 1.360(4) ? C124 H124 . . .963 ? C125 C126 . . 1.383(3) ? C125 H125 . . .956 ? C126 H126 . . .960 ? C10 C20 . . 1.527(2) ? C10 H10a . . .9594 ? C10 H10b . . .9518 ? C20 P2 . . 1.8652(16) ? C20 H20a . . .9525 ? C20 H20b . . .9521 ? P2 C211 . . 1.8323(16) ? P2 C221 . . 1.8428(17) ? C211 C212 . . 1.388(2) ? C211 C216 . . 1.399(2) ? C212 C213 . . 1.394(3) ? C212 H212 . . .9601 ? C213 C214 . . 1.372(3) ? C213 H213 . . .960 ? C214 C215 . . 1.385(3) ? C214 H214 . . .963 ? C215 C216 . . 1.388(3) ? C215 H215 . . .961 ? C216 H216 . . .9652 ? C221 C222 . . 1.395(2) ? C221 C226 . . 1.395(2) ? C222 C223 . . 1.391(3) ? C222 H222 . . .9625 ? C223 C224 . . 1.383(3) ? C223 H223 . . .957 ? C224 C225 . . 1.376(3) ? C224 H224 . . .957 ? C225 C226 . . 1.390(3) ? C225 H225 . . .9571 ? C226 H226 . . .9593 ? C1 C2 . . 1.225(2) ? C2 C3 . . 1.380(2) ? C3 C4 . . 1.211(2) ? P C11 . . 1.8143(17) ? P C21 . . 1.8192(19) ? P C31 . . 1.8181(19) ? C11 C12 . . 1.394(3) ? C11 C16 . . 1.392(3) ? C12 C13 . . 1.381(3) ? C12 H12 . . .9551 ? C13 C14 . . 1.385(3) ? C13 H13 . . .962 ? C14 C141 . . 1.511(3) ? C14 C15 . . 1.392(3) ? C141 H141a . . .950 ? C141 H141b . . .961 ? C141 H141c . . .950 ? C15 C16 . . 1.390(3) ? C15 H15 . . .963 ? C16 H16 . . .965 ? C21 C22 . . 1.396(3) ? C21 C26 . . 1.386(3) ? C22 C23 . . 1.390(3) ? C22 H22 . . .9647 ? C23 C24 . . 1.389(3) ? C23 H23 . . .966 ? C24 C241 . . 1.509(3) ? C24 C25 . . 1.388(3) ? C241 H241a . . .956 ? C241 H241b . . .951 ? C241 H241c . . .950 ? C25 C26 . . 1.391(3) ? C25 H25 . . .964 ? C26 H26 . . .957 ? C31 C32 . . 1.397(3) ? C31 C36 . . 1.393(3) ? C32 C33 . . 1.385(3) ? C32 H32 . . .953 ? C33 C34 . . 1.400(3) ? C33 H33 . . .954 ? C34 C341 . . 1.511(3) ? C34 C35 . . 1.382(3) ? C341 H341a . . .957 ? C341 H341b . . .946 ? C341 H341c . . .955 ? C35 C36 . . 1.396(3) ? C35 H35 . . .956 ? C36 H36 . . .959 ? C101 C1011 . . 1.496(3) ? C101 C102 . . 1.432(3) ? C101 C105 . . 1.441(3) ? C1011 H1011a . . .949 ? C1011 H1011b . . .948 ? C1011 H1011c . . .962 ? C102 C1021 . . 1.507(3) ? C102 C103 . . 1.423(2) ? C1021 H1021a . . .955 ? C1021 H1021b . . .950 ? C1021 H1021c . . .956 ? C103 C1031 . . 1.508(3) ? C103 C104 . . 1.437(3) ? C1031 H1031a . . .957 ? C1031 H1031b . . .957 ? C1031 H1031c . . .947 ? C104 C1041 . . 1.496(3) ? C104 C105 . . 1.427(2) ? C1041 H1041a . . .953 ? C1041 H1041b . . .954 ? C1041 H1041c . . .951 ? C105 C1051 . . 1.497(3) ? C1051 H1051a . . .958 ? C1051 H1051b . . .946 ? C1051 H1051c . . .954 ? Cl C0 . . 1.451(19) ? Cl C0 . '3 566' 1.933(18) ? C0 H0a . . .938 ? C0 H0b . . .985 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C4 Au P . . . 178.32(5) ? P1 Ru P2 . . . 82.766(15) ? P1 Ru C1 . . . 84.01(5) ? P1 Ru C101 . . . 108.88(5) ? P1 Ru C102 . . . 101.09(5) ? P1 Ru C103 . . . 124.83(5) ? P1 Ru C104 . . . 161.33(5) ? P1 Ru C105 . . . 143.28(5) ? P2 Ru C1 . . . 87.50(4) ? P2 Ru C101 . . . 167.27(4) ? P2 Ru C102 . . . 137.31(5) ? P2 Ru C103 . . . 107.30(4) ? P2 Ru C104 . . . 105.15(4) ? P2 Ru C105 . . . 132.59(5) ? C1 Ru C101 . . . 98.60(6) ? C1 Ru C102 . . . 135.13(6) ? C1 Ru C103 . . . 148.29(6) ? C1 Ru C104 . . . 112.81(7) ? C1 Ru C105 . . . 87.63(6) ? C101 Ru C102 . . . 37.27(7) ? C101 Ru C103 . . . 62.12(6) ? C101 Ru C104 . . . 62.20(6) ? C101 Ru C105 . . . 37.48(7) ? C102 Ru C103 . . . 36.72(6) ? C102 Ru C104 . . . 61.53(6) ? C102 Ru C105 . . . 61.73(7) ? C103 Ru C104 . . . 36.93(7) ? C103 Ru C105 . . . 61.56(7) ? C104 Ru C105 . . . 36.74(6) ? Ru P1 C111 . . . 120.15(6) ? Ru P1 C121 . . . 120.94(6) ? Ru P1 C10 . . . 107.51(5) ? C111 P1 C121 . . . 101.96(8) ? C111 P1 C10 . . . 98.63(7) ? C121 P1 C10 . . . 104.50(7) ? P1 C111 C112 . . . 120.92(13) ? P1 C111 C116 . . . 119.77(13) ? C112 C111 C116 . . . 118.48(16) ? C111 C112 C113 . . . 120.46(18) ? C111 C112 H112 . . . 119.89 ? C113 C112 H112 . . . 119.6 ? C112 C113 C114 . . . 120.3(2) ? C112 C113 H113 . . . 120.5 ? C114 C113 H113 . . . 119.2 ? C113 C114 C115 . . . 119.9(2) ? C113 C114 H114 . . . 120.6 ? C115 C114 H114 . . . 119.5 ? C114 C115 C116 . . . 120.1(2) ? C114 C115 H115 . . . 119.6 ? C116 C115 H115 . . . 120.3 ? C111 C116 C115 . . . 120.67(18) ? C111 C116 H116 . . . 119.75 ? C115 C116 H116 . . . 119.57 ? P1 C121 C122 . . . 120.82(15) ? P1 C121 C126 . . . 120.52(14) ? C122 C121 C126 . . . 118.51(17) ? C121 C122 C123 . . . 119.8(2) ? C121 C122 H122 . . . 120.1 ? C123 C122 H122 . . . 120.0 ? C122 C123 C124 . . . 120.8(3) ? C122 C123 H123 . . . 119.5 ? C124 C123 H123 . . . 119.7 ? C123 C124 C125 . . . 119.5(3) ? C123 C124 H124 . . . 120.2 ? C125 C124 H124 . . . 120.3 ? C124 C125 C126 . . . 119.8(2) ? C124 C125 H125 . . . 120.1 ? C126 C125 H125 . . . 120.1 ? C121 C126 C125 . . . 121.41(18) ? C121 C126 H126 . . . 119.09 ? C125 C126 H126 . . . 119.50 ? P1 C10 C20 . . . 106.56(10) ? P1 C10 H10a . . . 110.29 ? P1 C10 H10b . . . 110.72 ? C20 C10 H10a . . . 110.22 ? C20 C10 H10b . . . 110.53 ? H10a C10 H10b . . . 108.52 ? C10 C20 P2 . . . 109.66(10) ? C10 C20 H20a . . . 109.63 ? C10 C20 H20b . . . 109.49 ? P2 C20 H20a . . . 109.49 ? P2 C20 H20b . . . 109.47 ? H20a C20 H20b . . . 109.08 ? Ru P2 C20 . . . 110.52(5) ? Ru P2 C211 . . . 118.29(5) ? Ru P2 C221 . . . 119.77(5) ? C20 P2 C211 . . . 103.98(7) ? C20 P2 C221 . . . 101.52(7) ? C211 P2 C221 . . . 100.44(7) ? P2 C211 C212 . . . 122.44(12) ? P2 C211 C216 . . . 118.95(12) ? C212 C211 C216 . . . 118.27(15) ? C211 C212 C213 . . . 120.70(17) ? C211 C212 H212 . . . 119.91 ? C213 C212 H212 . . . 119.39 ? C212 C213 C214 . . . 120.21(19) ? C212 C213 H213 . . . 119.7 ? C214 C213 H213 . . . 120.1 ? C213 C214 C215 . . . 120.2(2) ? C213 C214 H214 . . . 119.7 ? C215 C214 H214 . . . 120.1 ? C214 C215 C216 . . . 119.68(18) ? C214 C215 H215 . . . 119.8 ? C216 C215 H215 . . . 120.6 ? C211 C216 C215 . . . 120.94(17) ? C211 C216 H216 . . . 119.16 ? C215 C216 H216 . . . 119.89 ? P2 C221 C222 . . . 120.32(12) ? P2 C221 C226 . . . 120.74(13) ? C222 C221 C226 . . . 118.90(16) ? C221 C222 C223 . . . 119.94(16) ? C221 C222 H222 . . . 119.99 ? C223 C222 H222 . . . 120.07 ? C222 C223 C224 . . . 120.31(18) ? C222 C223 H223 . . . 119.9 ? C224 C223 H223 . . . 119.7 ? C223 C224 C225 . . . 120.3(2) ? C223 C224 H224 . . . 120.2 ? C225 C224 H224 . . . 119.5 ? C224 C225 C226 . . . 119.73(17) ? C224 C225 H225 . . . 120.0 ? C226 C225 H225 . . . 120.3 ? C221 C226 C225 . . . 120.67(17) ? C221 C226 H226 . . . 119.25 ? C225 C226 H226 . . . 120.08 ? Ru C1 C2 . . . 172.05(14) ? C1 C2 C3 . . . 175.72(17) ? C2 C3 C4 . . . 179.6(2) ? Au C4 C3 . . . 175.92(15) ? Au P C11 . . . 110.91(6) ? Au P C21 . . . 114.14(6) ? Au P C31 . . . 114.92(6) ? C11 P C21 . . . 107.37(8) ? C11 P C31 . . . 103.52(8) ? C21 P C31 . . . 105.14(9) ? P C11 C12 . . . 121.41(14) ? P C11 C16 . . . 120.14(14) ? C12 C11 C16 . . . 118.36(16) ? C11 C12 C13 . . . 120.43(17) ? C11 C12 H12 . . . 119.74 ? C13 C12 H12 . . . 119.83 ? C12 C13 C14 . . . 121.77(18) ? C12 C13 H13 . . . 118.86 ? C14 C13 H13 . . . 119.37 ? C13 C14 C141 . . . 120.23(18) ? C13 C14 C15 . . . 117.81(17) ? C141 C14 C15 . . . 121.96(18) ? C14 C141 H141a . . . 109.1 ? C14 C141 H141b . . . 108.6 ? C14 C141 H141c . . . 110.5 ? H141a C141 H141b . . . 108.5 ? H141a C141 H141c . . . 111.1 ? H141b C141 H141c . . . 108.8 ? C14 C15 C16 . . . 121.05(18) ? C14 C15 H15 . . . 118.3 ? C16 C15 H15 . . . 120.7 ? C11 C16 C15 . . . 120.59(19) ? C11 C16 H16 . . . 118.74 ? C15 C16 H16 . . . 120.7 ? P C21 C22 . . . 118.23(13) ? P C21 C26 . . . 123.25(15) ? C22 C21 C26 . . . 118.51(17) ? C21 C22 C23 . . . 120.94(17) ? C21 C22 H22 . . . 119.00 ? C23 C22 H22 . . . 120.1 ? C22 C23 C24 . . . 120.76(18) ? C22 C23 H23 . . . 119.0 ? C24 C23 H23 . . . 120.3 ? C23 C24 C241 . . . 120.86(18) ? C23 C24 C25 . . . 117.86(18) ? C241 C24 C25 . . . 121.27(18) ? C24 C241 H241a . . . 108.34 ? C24 C241 H241b . . . 108.3 ? C24 C241 H241c . . . 110.3 ? H241a C241 H241b . . . 108.9 ? H241a C241 H241c . . . 109.3 ? H241b C241 H241c . . . 111.7 ? C24 C25 C26 . . . 121.92(18) ? C24 C25 H25 . . . 119.0 ? C26 C25 H25 . . . 119.0 ? C21 C26 C25 . . . 120.00(18) ? C21 C26 H26 . . . 120.0 ? C25 C26 H26 . . . 120.0 ? P C31 C32 . . . 118.20(15) ? P C31 C36 . . . 123.24(14) ? C32 C31 C36 . . . 118.45(18) ? C31 C32 C33 . . . 120.6(2) ? C31 C32 H32 . . . 119.8 ? C33 C32 H32 . . . 119.6 ? C32 C33 C34 . . . 121.1(2) ? C32 C33 H33 . . . 118.9 ? C34 C33 H33 . . . 119.9 ? C33 C34 C341 . . . 120.4(2) ? C33 C34 C35 . . . 118.0(2) ? C341 C34 C35 . . . 121.6(2) ? C34 C341 H341a . . . 108.8 ? C34 C341 H341b . . . 109.5 ? C34 C341 H341c . . . 110.1 ? H341a C341 H341b . . . 109.3 ? H341a C341 H341c . . . 108.7 ? H341b C341 H341c . . . 110.5 ? C34 C35 C36 . . . 121.4(2) ? C34 C35 H35 . . . 119.4 ? C36 C35 H35 . . . 119.1 ? C31 C36 C35 . . . 120.37(19) ? C31 C36 H36 . . . 119.8 ? C35 C36 H36 . . . 119.9 ? Ru C101 C1011 . . . 125.97(12) ? Ru C101 C102 . . . 72.19(10) ? Ru C101 C105 . . . 72.20(10) ? C1011 C101 C102 . . . 127.09(17) ? C1011 C101 C105 . . . 125.43(17) ? C102 C101 C105 . . . 107.16(15) ? C101 C1011 H1011a . . . 109.90 ? C101 C1011 H1011b . . . 109.97 ? C101 C1011 H1011c . . . 109.5 ? H1011a C1011 H1011b . . . 109.8 ? H1011a C1011 H1011c . . . 109.0 ? H1011b C1011 H1011c . . . 108.7 ? Ru C102 C101 . . . 70.54(10) ? Ru C102 C1021 . . . 128.78(13) ? Ru C102 C103 . . . 72.15(10) ? C101 C102 C1021 . . . 124.64(16) ? C101 C102 C103 . . . 108.65(16) ? C1021 C102 C103 . . . 126.33(17) ? C102 C1021 H1021a . . . 109.6 ? C102 C1021 H1021b . . . 110.0 ? C102 C1021 H1021c . . . 110.02 ? H1021a C1021 H1021b . . . 109.1 ? H1021a C1021 H1021c . . . 108.6 ? H1021b C1021 H1021c . . . 109.5 ? Ru C103 C102 . . . 71.12(10) ? Ru C103 C1031 . . . 130.27(13) ? Ru C103 C104 . . . 71.83(10) ? C102 C103 C1031 . . . 126.25(18) ? C102 C103 C104 . . . 108.04(15) ? C1031 C103 C104 . . . 124.99(16) ? C103 C1031 H1031a . . . 109.1 ? C103 C1031 H1031b . . . 109.26 ? C103 C1031 H1031c . . . 110.62 ? H1031a C1031 H1031b . . . 108.3 ? H1031a C1031 H1031c . . . 110.2 ? H1031b C1031 H1031c . . . 109.3 ? Ru C104 C103 . . . 71.24(10) ? Ru C104 C1041 . . . 130.26(13) ? Ru C104 C105 . . . 70.94(10) ? C103 C104 C1041 . . . 125.64(18) ? C103 C104 C105 . . . 107.71(15) ? C1041 C104 C105 . . . 126.04(19) ? C104 C1041 H1041a . . . 110.30 ? C104 C1041 H1041b . . . 110.4 ? C104 C1041 H1041c . . . 109.9 ? H1041a C1041 H1041b . . . 108.9 ? H1041a C1041 H1041c . . . 108.4 ? H1041b C1041 H1041c . . . 108.9 ? Ru C105 C101 . . . 70.32(9) ? Ru C105 C104 . . . 72.32(10) ? Ru C105 C1051 . . . 125.43(14) ? C101 C105 C104 . . . 108.41(16) ? C101 C105 C1051 . . . 125.60(16) ? C104 C105 C1051 . . . 125.93(17) ? C105 C1051 H1051a . . . 108.4 ? C105 C1051 H1051b . . . 109.01 ? C105 C1051 H1051c . . . 110.1 ? H1051a C1051 H1051b . . . 109.2 ? H1051a C1051 H1051c . . . 110.3 ? H1051b C1051 H1051c . . . 109.8 ? Cl C0 H0a . . . 111.2 ? Cl C0 H0b . . . 107.3 ? Cl C0 Cl . . '3 566' 121.5(12) ? H0a C0 H0b . . . 107.6 ? H0a C0 Cl . . '3 566' 105.0 ? H0b C0 Cl . . '3 566' 103.5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2397 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 29 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min -40 _reflns_limit_l_max 40 _reflns_number_observed ? _reflns_d_resolution_high .582 _reflns_d_resolution_low 14.663 _diffrn_reflns_av_sigmaI/netI .078 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .051 _refine_ls_wR_factor_all .03 _refine_ls_goodness_of_fit_all .962 _refine_ls_shift/su_mean .0002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? data_br640 _database_code_depnum_ccdc_archive 'CCDC 223452' _audit_creation_method Xtal3.6 _audit_creation_date 03-06-12 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C106 H110 O5 P4 Ru2' _chemical_formula_moiety 'C106 H110 O5 P4 Ru2' _chemical_formula_weight 1790.08 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 15.673(2) _cell_length_b 26.344(3) _cell_length_c 22.802(2) _cell_angle_alpha 90.00000 _cell_angle_beta 100.819(2) _cell_angle_gamma 90.00000 _cell_volume 9247.4(18) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7746 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 28.5 _cell_measurement_temperature 293(2) _exptl_absorpt_coefficient_mu .449 _exptl_crystal_description block _exptl_crystal_size_max .70 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .25 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .63 _exptl_absorpt_correction_T_max .91 _diffrn_reflns_number 91349 _reflns_number_total 23308 _reflns_number_gt 23308 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.1 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_max .940 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .074 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .061 _refine_ls_wR_factor_ref .062 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_number_reflns 13098 _refine_ls_number_parameters 1054 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .042 _refine_diff_density_min -.66 _refine_diff_density_max 1.1 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF' _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 424 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 440 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 20 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 16 .090027 .094971 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 8 -1.42 .835999 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 1.16049(2) .775980(10) .45642(2) .0365(2) Uani ? ? 1.00000 ? ? P11 1.15191(8) .85998(4) .43204(5) .0378(6) Uani ? ? 1.00000 ? ? C1111 1.0473(3) .89067(18) .4375(2) .044(3) Uani ? ? 1.00000 ? ? C1112 .9761(3) .8618(2) .4450(2) .058(3) Uani ? ? 1.00000 ? ? C1113 .8964(3) .8848(3) .4468(3) .078(4) Uani ? ? 1.00000 ? ? C1114 .8893(4) .9372(3) .4406(3) .082(5) Uani ? ? 1.00000 ? ? C1115 .9594(5) .9658(2) .4323(3) .075(4) Uani ? ? 1.00000 ? ? C1116 1.0375(3) .9428(2) .4300(3) .061(3) Uani ? ? 1.00000 ? ? C1121 1.2289(3) .89571(17) .4869(2) .045(3) Uani ? ? 1.00000 ? ? C1122 1.2065(3) .92104(19) .5344(2) .057(3) Uani ? ? 1.00000 ? ? C1123 1.2695(5) .9436(2) .5780(3) .078(4) Uani ? ? 1.00000 ? ? C1124 1.3554(4) .9405(3) .5741(3) .085(4) Uani ? ? 1.00000 ? ? C1125 1.3796(4) .9149(2) .5277(3) .077(4) Uani ? ? 1.00000 ? ? C1126 1.3171(3) .8924(2) .4848(3) .059(3) Uani ? ? 1.00000 ? ? C1131 1.1625(3) .88784(17) .3602(2) .045(3) Uani ? ? 1.00000 ? ? C1132 1.1014(3) .87368(19) .3098(2) .057(3) Uani ? ? 1.00000 ? ? C1133 1.1011(4) .8957(2) .2552(3) .071(4) Uani ? ? 1.00000 ? ? C1134 1.1608(5) .9337(3) .2495(3) .080(4) Uani ? ? 1.00000 ? ? C1135 1.2214(5) .9475(2) .2983(3) .076(4) Uani ? ? 1.00000 ? ? C1136 1.2224(4) .92538(19) .3526(3) .057(3) Uani ? ? 1.00000 ? ? P12 1.24903(8) .74371(4) .39632(5) .0376(6) Uani ? ? 1.00000 ? ? C1211 1.2383(3) .67440(18) .3945(2) .046(3) Uani ? ? 1.00000 ? ? C1212 1.1578(4) .6516(2) .3733(3) .066(4) Uani ? ? 1.00000 ? ? C1213 1.1456(4) .6000(2) .3728(3) .087(5) Uani ? ? 1.00000 ? ? C1214 1.2140(6) .5685(2) .3930(4) .103(6) Uani ? ? 1.00000 ? ? C1215 1.2932(5) .5894(3) .4161(4) .105(6) Uani ? ? 1.00000 ? ? C1216 1.3053(4) .6418(2) .4165(3) .075(4) Uani ? ? 1.00000 ? ? C1221 1.3680(3) .75090(17) .4187(2) .043(3) Uani ? ? 1.00000 ? ? C1222 1.4226(4) .7334(2) .3811(2) .058(3) Uani ? ? 1.00000 ? ? C1223 1.5111(4) .7373(3) .3975(3) .073(4) Uani ? ? 1.00000 ? ? C1224 1.5463(4) .7580(3) .4514(3) .087(4) Uani ? ? 1.00000 ? ? C1225 1.4950(4) .7751(3) .4884(3) .097(5) Uani ? ? 1.00000 ? ? C1226 1.4051(3) .7715(2) .4718(2) .065(3) Uani ? ? 1.00000 ? ? C1231 1.2368(3) .76148(17) .3174(2) .039(2) Uani ? ? 1.00000 ? ? C1232 1.2790(3) .80472(19) .3035(2) .048(3) Uani ? ? 1.00000 ? ? C1233 1.2705(4) .8211(2) .2450(3) .061(3) Uani ? ? 1.00000 ? ? C1234 1.2200(4) .7939(3) .2002(3) .063(4) Uani ? ? 1.00000 ? ? C1235 1.1781(4) .7547(3) .2129(3) .078(4) Uani ? ? 1.00000 ? ? C1236 1.1849(4) .7357(2) .2710(2) .060(3) Uani ? ? 1.00000 ? ? C101 1.0808(3) .7454(2) .5202(2) .059(3) Uani ? ? 1.00000 ? ? C102 1.1230(4) .7895(2) .5451(2) .066(4) Uani ? ? 1.00000 ? ? C103 1.2142(4) .7810(2) .5547(2) .066(4) Uani ? ? 1.00000 ? ? C104 1.2283(4) .7327(3) .5356(3) .069(4) Uani ? ? 1.00000 ? ? C105 1.1466(5) .7096(2) .5144(3) .073(4) Uani ? ? 1.00000 ? ? C1 1.0699(3) .76466(16) .3836(2) .040(2) Uani ? ? 1.00000 ? ? C2 1.0183(3) .75578(17) .3370(2) .045(3) Uani ? ? 1.00000 ? ? C3 .9638(3) .74493(17) .2837(2) .044(3) Uani ? ? 1.00000 ? ? C4 .9122(3) .73415(16) .2385(2) .041(2) Uani ? ? 1.00000 ? ? Ru2 .81902(2) .717770(10) .16909(2) .0364(2) Uani ? ? 1.00000 ? ? P21 .83551(8) .63508(4) .20030(6) .0404(7) Uani ? ? 1.00000 ? ? C2111 .9415(3) .60650(18) .1960(2) .044(3) Uani ? ? 1.00000 ? ? C2112 1.0101(3) .63518(19) .1853(3) .057(3) Uani ? ? 1.00000 ? ? C2113 1.0916(4) .6128(2) .1855(3) .076(4) Uani ? ? 1.00000 ? ? C2114 1.1028(4) .5618(3) .1967(3) .083(4) Uani ? ? 1.00000 ? ? C2115 1.0348(4) .5327(2) .2079(3) .076(4) Uani ? ? 1.00000 ? ? C2116 .9549(3) .5545(2) .2079(3) .062(3) Uani ? ? 1.00000 ? ? C2121 .7605(3) .59410(18) .1504(2) .050(3) Uani ? ? 1.00000 ? ? C2122 .7838(4) .56739(19) .1029(3) .060(3) Uani ? ? 1.00000 ? ? C2123 .7219(5) .5410(2) .0633(3) .075(4) Uani ? ? 1.00000 ? ? C2124 .6377(5) .5403(3) .0693(3) .090(5) Uani ? ? 1.00000 ? ? C2125 .6118(4) .5660(3) .1149(4) .095(5) Uani ? ? 1.00000 ? ? C2126 .6729(4) .5939(2) .1550(3) .070(4) Uani ? ? 1.00000 ? ? C2131 .8309(3) .61123(17) .2753(2) .045(3) Uani ? ? 1.00000 ? ? C2132 .8905(3) .6314(2) .3225(3) .060(3) Uani ? ? 1.00000 ? ? C2133 .8985(4) .6133(3) .3802(3) .076(4) Uani ? ? 1.00000 ? ? C2134 .8474(6) .5743(3) .3916(3) .095(5) Uani ? ? 1.00000 ? ? C2135 .7855(6) .5537(2) .3459(4) .091(5) Uani ? ? 1.00000 ? ? C2136 .7786(4) .5721(2) .2881(3) .069(4) Uani ? ? 1.00000 ? ? P22 .73219(8) .75135(4) .22928(6) .0388(6) Uani ? ? 1.00000 ? ? C2211 .7416(3) .82145(18) .2285(2) .050(3) Uani ? ? 1.00000 ? ? C2212 .8220(4) .84407(19) .2497(3) .068(4) Uani ? ? 1.00000 ? ? C2213 .8330(5) .8962(2) .2491(3) .090(5) Uani ? ? 1.00000 ? ? C2214 .7634(6) .9266(2) .2246(4) .102(6) Uani ? ? 1.00000 ? ? C2215 .6857(5) .9047(3) .2022(4) .104(5) Uani ? ? 1.00000 ? ? C2216 .6736(4) .8530(2) .2034(3) .075(4) Uani ? ? 1.00000 ? ? C2221 .6144(3) .74283(18) .2087(2) .046(3) Uani ? ? 1.00000 ? ? C2222 .5591(3) .7634(2) .2434(2) .059(3) Uani ? ? 1.00000 ? ? C2223 .4707(4) .7574(3) .2290(3) .079(4) Uani ? ? 1.00000 ? ? C2224 .4347(3) .7290(3) .1793(3) .088(5) Uani ? ? 1.00000 ? ? C2225 .4876(4) .7071(3) .1460(3) .086(4) Uani ? ? 1.00000 ? ? C2226 .5776(3) .7139(2) .1599(2) .059(3) Uani ? ? 1.00000 ? ? C2231 .7463(3) .73566(18) .3094(2) .042(3) Uani ? ? 1.00000 ? ? C2232 .7042(3) .69260(19) .3247(2) .047(3) Uani ? ? 1.00000 ? ? C2233 .7127(3) .6781(2) .3838(3) .059(3) Uani ? ? 1.00000 ? ? C2234 .7651(4) .7064(3) .4280(2) .074(4) Uani ? ? 1.00000 ? ? C2235 .8077(5) .7497(3) .4145(3) .079(4) Uani ? ? 1.00000 ? ? C2236 .7982(3) .7623(2) .3539(2) .059(3) Uani ? ? 1.00000 ? ? C201 .8920(4) .7469(2) .1013(2) .060(3) Uani ? ? 1.00000 ? ? C202 .8533(4) .7010(2) .0799(2) .066(4) Uani ? ? 1.00000 ? ? C203 .7620(4) .7068(2) .0722(2) .062(3) Uani ? ? 1.00000 ? ? C204 .7453(4) .7559(2) .0886(2) .061(3) Uani ? ? 1.00000 ? ? C205 .8259(4) .7812(2) .1061(2) .065(4) Uani ? ? 1.00000 ? ? O301 -.0513(17) .6080(7) .5789(13) .45(3) Uani ? ? 1.00000 ? ? C302 .0240(16) .6021(10) .5613(14) .34(3) Uani ? ? 1.00000 ? ? C303 .0461(11) .5550(10) .5704(11) .28(2) Uani ? ? 1.00000 ? ? C304 -.0194(15) .5310(5) .5917(10) .257(17) Uani ? ? 1.00000 ? ? C305 -.0805(10) .5609(13) .5888(15) .37(3) Uani ? ? 1.00000 ? ? O401 .3746(16) .8744(7) .0941(10) .37(2) Uani ? ? 1.00000 ? ? C402 .4389(13) .8905(14) .1354(15) .34(3) Uani ? ? 1.00000 ? ? C403 .4099(17) .9257(14) .1617(8) .33(3) Uani ? ? 1.00000 ? ? C404 .3346(19) .9417(6) .1265(16) .43(4) Uani ? ? 1.00000 ? ? C405 .3052(8) .9068(12) .0966(12) .28(2) Uani ? ? 1.00000 ? ? O501 .6212(9) .8887(7) .3628(9) .40(2) Uani ? ? 1.00000 ? ? C502 .5328(17) .8875(8) .3301(8) .32(2) Uani ? ? 1.00000 ? ? C503 .4863(7) .9125(9) .3632(10) .28(2) Uani ? ? 1.00000 ? ? C504 .5376(15) .9384(6) .3961(11) .35(2) Uani ? ? 1.00000 ? ? C505 .6172(14) .9104(9) .4088(10) .39(3) Uani ? ? 1.00000 ? ? O601 .5715(16) .6124(9) .5060(15) .52(3) Uani ? ? 1.00000 ? ? C602 .658(2) .6083(9) .5269(8) .27(2) Uani ? ? 1.00000 ? ? C603 .6735(10) .5590(11) .5230(13) .29(2) Uani ? ? 1.00000 ? ? C604 .610(2) .5406(5) .4949(18) .40(4) Uani ? ? 1.00000 ? ? C605 .5532(15) .5788(12) .4741(10) .42(3) Uani ? ? 1.00000 ? ? O701 .5047(8) .5705(8) .2716(9) .43(2) Uani ? ? 1.00000 ? ? C702 .4471(18) .5331(4) .2723(12) .44(3) Uani ? ? 1.00000 ? ? C703 .3700(12) .5515(8) .2507(8) .245(17) Uani ? ? 1.00000 ? ? C704 .3760(12) .6032(7) .2594(9) .249(18) Uani ? ? 1.00000 ? ? C705 .4653(16) .6114(6) .2856(9) .277(18) Uani ? ? 1.00000 ? ? H1112 .98184 .82569 .44927 .07300 Uiso ? ? 1.00000 ? ? H1113 .84712 .86419 .45277 .09500 Uiso ? ? 1.00000 ? ? H1114 .83385 .95288 .44164 .10000 Uiso ? ? 1.00000 ? ? H1115 .95309 1.00200 .42847 .09500 Uiso ? ? 1.00000 ? ? H1116 1.08629 .96339 .42393 .07600 Uiso ? ? 1.00000 ? ? H1122 1.14529 .92378 .53778 .07300 Uiso ? ? 1.00000 ? ? H1123 1.25189 .96236 .61052 .09300 Uiso ? ? 1.00000 ? ? H1124 1.39801 .95563 .60507 .10800 Uiso ? ? 1.00000 ? ? H1125 1.44094 .91263 .52540 .09700 Uiso ? ? 1.00000 ? ? H1126 1.33496 .87315 .45262 .07800 Uiso ? ? 1.00000 ? ? H1132 1.05909 .84700 .31375 .07200 Uiso ? ? 1.00000 ? ? H1133 1.05833 .88582 .22063 .09100 Uiso ? ? 1.00000 ? ? H1134 1.15860 .94990 .21132 .09900 Uiso ? ? 1.00000 ? ? H1135 1.26423 .97253 .29314 .09600 Uiso ? ? 1.00000 ? ? H1136 1.26572 .93574 .38667 .08000 Uiso ? ? 1.00000 ? ? H1212 1.10782 .67343 .35977 .08300 Uiso ? ? 1.00000 ? ? H1213 1.08927 .58493 .35785 .11000 Uiso ? ? 1.00000 ? ? H1214 1.20667 .53221 .39100 .12800 Uiso ? ? 1.00000 ? ? H1215 1.34196 .56694 .43146 .12900 Uiso ? ? 1.00000 ? ? H1216 1.36282 .65523 .43309 .09600 Uiso ? ? 1.00000 ? ? H1222 1.39685 .71784 .34358 .07300 Uiso ? ? 1.00000 ? ? H1223 1.54705 .72582 .37045 .09100 Uiso ? ? 1.00000 ? ? H1224 1.60996 .76122 .46205 .10700 Uiso ? ? 1.00000 ? ? H1225 1.52062 .78898 .52735 .11600 Uiso ? ? 1.00000 ? ? H1226 1.36831 .78415 .49810 .08100 Uiso ? ? 1.00000 ? ? H1232 1.31514 .82385 .33546 .06400 Uiso ? ? 1.00000 ? ? H1233 1.29904 .85153 .23374 .08000 Uiso ? ? 1.00000 ? ? H1234 1.21730 .80159 .15880 .07600 Uiso ? ? 1.00000 ? ? H1235 1.13729 .73823 .18040 .09500 Uiso ? ? 1.00000 ? ? H1236 1.15402 .70485 .27885 .07800 Uiso ? ? 1.00000 ? ? H101 1.01808 .74039 .50827 .07900 Uiso ? ? 1.00000 ? ? H102 1.09488 .82033 .55481 .08200 Uiso ? ? 1.00000 ? ? H103 1.25857 .80584 .57132 .08500 Uiso ? ? 1.00000 ? ? H104 1.28415 .71717 .53747 .09000 Uiso ? ? 1.00000 ? ? H105 1.13720 .67555 .49926 .09500 Uiso ? ? 1.00000 ? ? H2112 1.00184 .67096 .17700 .07300 Uiso ? ? 1.00000 ? ? H2113 1.13990 .63386 .17843 .09400 Uiso ? ? 1.00000 ? ? H2114 1.15864 .54682 .19592 .10000 Uiso ? ? 1.00000 ? ? H2115 1.04369 .49679 .21583 .09500 Uiso ? ? 1.00000 ? ? H2116 .90662 .53401 .21568 .08000 Uiso ? ? 1.00000 ? ? H2122 .84420 .56796 .09736 .07900 Uiso ? ? 1.00000 ? ? H2123 .74062 .52218 .03125 .09600 Uiso ? ? 1.00000 ? ? H2124 .59556 .52201 .04044 .11400 Uiso ? ? 1.00000 ? ? H2125 .55079 .56579 .12004 .12000 Uiso ? ? 1.00000 ? ? H2126 .65489 .61289 .18775 .09000 Uiso ? ? 1.00000 ? ? H2132 .92767 .65927 .31411 .07800 Uiso ? ? 1.00000 ? ? H2133 .94059 .62861 .41230 .10000 Uiso ? ? 1.00000 ? ? H2134 .85402 .55948 .43153 .11700 Uiso ? ? 1.00000 ? ? H2135 .74667 .52759 .35430 .11100 Uiso ? ? 1.00000 ? ? H2136 .73445 .55761 .25542 .08900 Uiso ? ? 1.00000 ? ? H2212 .87119 .82293 .26702 .08700 Uiso ? ? 1.00000 ? ? H2213 .88952 .91170 .26423 .10900 Uiso ? ? 1.00000 ? ? H2214 .76986 .96297 .22420 .12600 Uiso ? ? 1.00000 ? ? H2215 .63751 .92662 .18471 .12400 Uiso ? ? 1.00000 ? ? H2216 .61735 .83838 .18776 .09500 Uiso ? ? 1.00000 ? ? H2222 .58387 .78217 .27933 .07800 Uiso ? ? 1.00000 ? ? H2223 .43308 .77319 .25322 .09700 Uiso ? ? 1.00000 ? ? H2224 .37248 .72463 .16886 .10800 Uiso ? ? 1.00000 ? ? H2225 .46189 .68695 .11151 .10400 Uiso ? ? 1.00000 ? ? H2226 .61400 .69812 .13548 .07400 Uiso ? ? 1.00000 ? ? H2232 .66838 .67290 .29344 .06100 Uiso ? ? 1.00000 ? ? H2233 .68268 .64818 .39526 .08100 Uiso ? ? 1.00000 ? ? H2234 .77326 .69676 .46866 .09500 Uiso ? ? 1.00000 ? ? H2235 .84460 .77110 .44622 .11100 Uiso ? ? 1.00000 ? ? H2236 .82975 .79162 .34272 .07500 Uiso ? ? 1.00000 ? ? H201 .95487 .75391 .11232 .07600 Uiso ? ? 1.00000 ? ? H202 .88402 .67092 .07183 .08800 Uiso ? ? 1.00000 ? ? H203 .71805 .68111 .05789 .07800 Uiso ? ? 1.00000 ? ? H204 .68850 .77070 .08811 .07700 Uiso ? ? 1.00000 ? ? H205 .83336 .81641 .11889 .08200 Uiso ? ? 1.00000 ? ? H302a .06835 .62213 .58353 .41000 Uiso ? ? 1.00000 ? ? H302b .01983 .60857 .51974 .41000 Uiso ? ? 1.00000 ? ? H303a .09768 .55124 .59911 .34700 Uiso ? ? 1.00000 ? ? H303b .05210 .53797 .53452 .34700 Uiso ? ? 1.00000 ? ? H304a -.00139 .52160 .63293 .31600 Uiso ? ? 1.00000 ? ? H304b -.04005 .50173 .56946 .31600 Uiso ? ? 1.00000 ? ? H305a -.10203 .56275 .62525 .48100 Uiso ? ? 1.00000 ? ? H305b -.12694 .55266 .55715 .48100 Uiso ? ? 1.00000 ? ? H402a .49175 .90182 .12880 .36300 Uiso ? ? 1.00000 ? ? H402b .45493 .86892 .17471 .36300 Uiso ? ? 1.00000 ? ? H403a .44022 .96114 .16101 .36300 Uiso ? ? 1.00000 ? ? H403b .39132 .92697 .19919 .36300 Uiso ? ? 1.00000 ? ? H404a .33538 .96721 .09441 .48000 Uiso ? ? 1.00000 ? ? H404b .28307 .94958 .14213 .48000 Uiso ? ? 1.00000 ? ? H405a .28651 .90989 .05232 .32900 Uiso ? ? 1.00000 ? ? H405b .26427 .88449 .10897 .32900 Uiso ? ? 1.00000 ? ? H502a .51254 .85300 .32629 .40200 Uiso ? ? 1.00000 ? ? H502b .52801 .90238 .29273 .40200 Uiso ? ? 1.00000 ? ? H503a .46014 .89037 .38709 .34400 Uiso ? ? 1.00000 ? ? H503b .44520 .93308 .33943 .34400 Uiso ? ? 1.00000 ? ? H504a .51959 .94607 .43095 .44000 Uiso ? ? 1.00000 ? ? H504b .54785 .96923 .37503 .44000 Uiso ? ? 1.00000 ? ? H505a .61717 .88699 .43921 .48100 Uiso ? ? 1.00000 ? ? H505b .66655 .93237 .41785 .48100 Uiso ? ? 1.00000 ? ? H602a .66050 .62316 .56567 .37400 Uiso ? ? 1.00000 ? ? H602b .68272 .63260 .50308 .37400 Uiso ? ? 1.00000 ? ? H603a .69647 .54910 .56170 .38000 Uiso ? ? 1.00000 ? ? H603b .71905 .55859 .49922 .38000 Uiso ? ? 1.00000 ? ? H604a .59089 .52242 .53073 .48900 Uiso ? ? 1.00000 ? ? H604b .62826 .51649 .47274 .48900 Uiso ? ? 1.00000 ? ? H605a .49885 .56108 .47246 .51200 Uiso ? ? 1.00000 ? ? H605b .56477 .57923 .43396 .51200 Uiso ? ? 1.00000 ? ? H702a .45098 .52108 .31079 .57200 Uiso ? ? 1.00000 ? ? H702b .46249 .50722 .24661 .57200 Uiso ? ? 1.00000 ? ? H703a .33004 .53659 .27052 .31000 Uiso ? ? 1.00000 ? ? H703b .35614 .54467 .20884 .31000 Uiso ? ? 1.00000 ? ? H704a .33780 .61262 .28599 .30200 Uiso ? ? 1.00000 ? ? H704b .36170 .62082 .22366 .30200 Uiso ? ? 1.00000 ? ? H705a .46996 .61326 .32984 .34400 Uiso ? ? 1.00000 ? ? H705b .48563 .64137 .27303 .34400 Uiso ? ? 1.00000 ? ? 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 Ru1 .0327(2) .0472(2) .0302(2) .00444(17) .00768(16) .00167(17) P11 .0323(6) .0454(7) .0356(7) .0029(5) .0063(5) -.0039(5) C1111 .040(3) .052(3) .039(3) .013(2) .006(2) -.006(2) C1112 .044(3) .073(4) .060(4) .008(3) .016(3) -.000(3) C1113 .035(3) .103(5) .099(5) .020(3) .020(3) .007(4) C1114 .060(4) .100(5) .090(5) .040(4) .022(4) .006(4) C1115 .077(5) .062(4) .087(5) .030(3) .020(4) .000(3) C1116 .056(4) .059(3) .068(4) .008(3) .012(3) -.001(3) C1121 .040(3) .049(3) .045(3) .002(2) .002(2) -.004(2) C1122 .054(3) .062(3) .052(4) .000(3) .003(3) -.014(3) C1123 .082(5) .088(5) .058(4) .005(4) -.003(4) -.030(3) C1124 .064(4) .095(5) .083(5) -.009(4) -.019(4) -.027(4) C1125 .043(3) .095(5) .085(5) -.011(3) -.008(3) -.019(4) C1126 .044(3) .069(4) .063(4) -.003(3) .005(3) -.014(3) C1131 .045(3) .044(3) .046(3) .010(2) .009(2) .000(2) C1132 .060(4) .064(3) .048(3) .001(3) .009(3) .005(3) C1133 .077(4) .087(4) .048(4) .019(4) .006(3) .016(3) C1134 .111(6) .078(4) .058(4) .020(4) .034(4) .028(3) C1135 .094(5) .056(4) .086(5) -.003(3) .037(4) .014(3) C1136 .065(4) .050(3) .060(4) -.002(3) .024(3) .002(3) P12 .0330(7) .0464(7) .0338(7) .0051(5) .0071(5) -.0023(5) C1211 .048(3) .050(3) .044(3) .008(2) .017(2) .002(2) C1212 .063(4) .048(3) .093(5) .011(3) .025(3) -.005(3) C1213 .080(5) .059(4) .124(6) -.007(3) .020(4) -.005(4) C1214 .111(7) .050(4) .150(8) .006(4) .027(6) .004(4) C1215 .096(6) .067(5) .148(8) .026(4) .015(5) .031(5) C1216 .068(4) .065(4) .087(5) .005(3) .006(4) .006(3) C1221 .030(3) .054(3) .045(3) .010(2) .008(2) .001(2) C1222 .052(3) .075(4) .050(3) .007(3) .016(3) -.006(3) C1223 .052(4) .116(5) .056(4) .037(3) .025(3) .007(4) C1224 .041(3) .160(7) .059(4) .014(4) .003(3) -.012(4) C1225 .044(4) .188(8) .055(4) .007(4) -.005(3) -.027(5) C1226 .040(3) .104(5) .049(3) .010(3) .003(3) -.013(3) C1231 .035(3) .053(3) .032(3) .005(2) .010(2) -.005(2) C1232 .045(3) .056(3) .044(3) .008(2) .015(2) -.000(2) C1233 .068(4) .059(3) .063(4) .010(3) .028(3) .012(3) C1234 .058(4) .095(5) .040(3) .016(3) .021(3) -.000(3) C1235 .072(5) .124(6) .037(4) .007(4) .006(3) -.018(4) C1236 .061(4) .072(4) .047(3) -.008(3) .009(3) -.009(3) C101 .047(3) .086(4) .052(4) .008(3) .027(3) .017(3) C102 .088(5) .081(4) .033(3) .020(3) .026(3) .004(3) C103 .069(4) .093(4) .033(3) .002(3) .002(3) .014(3) C104 .065(4) .096(5) .049(4) .024(4) .015(3) .029(3) C105 .109(6) .064(4) .055(4) .009(4) .036(4) .025(3) C1 .035(3) .044(3) .042(3) .003(2) .012(2) .002(2) C2 .035(3) .050(3) .050(3) -.002(2) .004(2) -.006(2) C3 .037(3) .048(3) .047(3) -.003(2) .008(2) -.006(2) C4 .035(3) .047(3) .044(3) -.002(2) .013(2) -.004(2) Ru2 .0330(2) .0459(2) .0306(2) .00059(17) .00726(16) -.00201(17) P21 .0334(7) .0447(7) .0435(8) .0001(5) .0084(6) -.0055(6) C2111 .037(3) .055(3) .040(3) -.000(2) .010(2) -.007(2) C2112 .041(3) .059(3) .072(4) .002(3) .014(3) -.012(3) C2113 .045(4) .089(5) .097(5) .006(3) .023(3) -.005(4) C2114 .053(4) .096(5) .102(6) .030(4) .018(4) -.009(4) C2115 .069(4) .064(4) .097(5) .023(3) .022(4) .005(3) C2116 .054(4) .063(3) .073(4) .005(3) .019(3) -.000(3) C2121 .041(3) .048(3) .058(4) -.003(2) .004(3) -.004(2) C2122 .066(4) .054(3) .057(4) -.005(3) .007(3) -.005(3) C2123 .087(5) .064(4) .065(4) -.001(3) -.008(4) -.017(3) C2124 .083(5) .080(5) .092(6) -.016(4) -.022(4) -.020(4) C2125 .056(4) .097(5) .123(7) -.018(4) -.008(4) -.020(5) C2126 .047(3) .067(4) .090(5) -.003(3) .002(3) -.018(3) C2131 .047(3) .043(3) .048(3) .007(2) .017(2) .004(2) C2132 .051(3) .077(4) .051(4) .011(3) .011(3) .013(3) C2133 .071(4) .092(5) .064(4) .015(4) .012(3) .020(4) C2134 .123(7) .102(6) .069(5) .032(5) .038(5) .034(4) C2135 .132(7) .068(4) .088(6) -.009(4) .061(5) .012(4) C2136 .085(5) .060(4) .068(4) -.007(3) .032(4) -.007(3) P22 .0338(7) .0463(7) .0368(7) .0016(5) .0074(5) -.0043(6) C2211 .052(3) .050(3) .051(3) .007(2) .020(3) -.004(2) C2212 .062(4) .047(3) .095(5) -.000(3) .017(3) -.005(3) C2213 .084(5) .060(4) .127(7) -.001(4) .022(4) -.012(4) C2214 .112(7) .055(4) .145(8) -.001(4) .040(6) -.003(4) C2215 .102(6) .060(4) .144(8) .023(4) .006(5) .024(4) C2216 .072(4) .056(4) .089(5) .003(3) -.002(4) .008(3) C2221 .041(3) .054(3) .044(3) .007(2) .013(2) .003(2) C2222 .042(3) .087(4) .049(3) .014(3) .009(3) -.001(3) C2223 .052(4) .117(5) .075(5) .028(4) .030(3) .015(4) C2224 .033(3) .159(7) .071(5) -.004(4) .008(3) .005(5) C2225 .043(3) .157(7) .057(4) -.018(4) .004(3) -.013(4) C2226 .038(3) .088(4) .051(3) -.005(3) .009(2) -.011(3) C2231 .036(3) .055(3) .037(3) .011(2) .009(2) -.006(2) C2232 .040(3) .057(3) .047(3) .008(2) .011(2) .000(2) C2233 .052(3) .074(4) .057(4) .013(3) .025(3) .014(3) C2234 .079(5) .112(5) .030(3) .032(4) .010(3) .004(3) C2235 .104(6) .088(5) .044(4) .025(4) .011(4) -.007(3) C2236 .061(4) .078(4) .040(3) -.010(3) .012(3) -.013(3) C201 .058(4) .083(4) .044(3) .003(3) .026(3) .012(3) C202 .089(5) .085(4) .028(3) .022(4) .025(3) .003(3) C203 .070(4) .085(4) .029(3) -.003(3) .003(3) -.001(3) C204 .062(4) .078(4) .041(3) .015(3) .004(3) .012(3) C205 .091(5) .062(3) .048(3) .004(3) .025(3) .014(3) O301 .52(4) .28(2) .56(4) .17(2) .10(3) -.06(2) C302 .36(4) .23(2) .41(3) -.15(2) .03(3) .16(3) C303 .217(18) .23(2) .43(3) .025(17) .18(2) .01(2) C304 .163(15) .148(11) .47(3) -.023(11) .09(2) .041(14) C305 .124(14) .42(4) .61(4) .043(19) .17(2) .13(4) O401 .255(18) .39(2) .44(3) -.055(17) .012(18) -.17(2) C402 .18(2) .44(5) .35(4) .13(3) -.06(2) -.01(3) C403 .33(4) .47(5) .161(15) -.20(3) .03(2) -.07(2) C404 .45(5) .127(14) .70(6) .12(2) .08(4) -.11(2) C405 .117(12) .32(3) .39(3) .011(16) .017(15) .13(3) O501 .203(13) .61(3) .38(2) .051(16) .010(14) -.27(2) C502 .23(2) .43(3) .27(2) .08(2) -.046(17) -.20(2) C503 .127(12) .36(3) .37(3) -.061(14) .092(15) -.16(2) C504 .200(18) .211(16) .62(4) .035(14) -.00(2) -.24(2) C505 .36(3) .39(3) .33(3) .11(2) -.15(2) -.26(2) O601 .32(3) .49(3) .79(5) .16(3) .27(3) .00(3) C602 .42(4) .205(17) .200(16) -.16(2) .10(2) -.067(15) C603 .149(15) .27(3) .40(3) .014(15) -.083(16) -.01(2) C604 .36(4) .162(15) .61(6) .02(2) -.04(3) -.16(2) C605 .36(4) .44(4) .33(3) -.12(3) -.26(3) .10(3) O701 .298(17) .274(17) .79(4) -.006(14) .28(2) -.09(2) C702 .30(3) .145(14) .76(5) -.019(16) -.19(3) .06(2) C703 .25(2) .198(16) .27(2) -.116(15) .004(15) -.039(15) C704 .207(18) .200(17) .33(2) .009(13) .022(16) -.045(16) C705 .25(2) .185(15) .36(2) -.046(14) -.047(19) -.115(15) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 P11 . . 2.2795(11) ? Ru1 P12 . . 2.2892(13) ? Ru1 C101 . . 2.238(6) ? Ru1 C102 . . 2.238(6) ? Ru1 C103 . . 2.244(5) ? Ru1 C104 . . 2.230(6) ? Ru1 C105 . . 2.227(6) ? Ru1 C1 . . 1.995(4) ? P11 C1111 . . 1.853(5) ? P11 C1121 . . 1.827(5) ? P11 C1131 . . 1.830(5) ? C1111 C1112 . . 1.387(7) ? C1111 C1116 . . 1.390(7) ? C1112 C1113 . . 1.397(8) ? C1112 H1112 . . .959 ? C1113 C1114 . . 1.390(10) ? C1113 H1113 . . .974 ? C1114 C1115 . . 1.374(10) ? C1114 H1114 . . .967 ? C1115 C1116 . . 1.374(9) ? C1115 H1115 . . .962 ? C1116 H1116 . . .968 ? C1121 C1122 . . 1.373(8) ? C1121 C1126 . . 1.396(7) ? C1122 C1123 . . 1.396(8) ? C1122 H1122 . . .980 ? C1123 C1124 . . 1.368(10) ? C1123 H1123 . . .973 ? C1124 C1125 . . 1.367(10) ? C1124 H1124 . . .962 ? C1125 C1126 . . 1.381(8) ? C1125 H1125 . . .975 ? C1126 H1126 . . .974 ? C1131 C1132 . . 1.401(7) ? C1131 C1136 . . 1.397(7) ? C1132 C1133 . . 1.373(8) ? C1132 H1132 . . .982 ? C1133 C1134 . . 1.393(10) ? C1133 H1133 . . .970 ? C1134 C1135 . . 1.370(9) ? C1134 H1134 . . .964 ? C1135 C1136 . . 1.364(9) ? C1135 H1135 . . .964 ? C1136 H1136 . . .970 ? P12 C1211 . . 1.833(5) ? P12 C1221 . . 1.849(4) ? P12 C1231 . . 1.834(5) ? C1211 C1212 . . 1.400(7) ? C1211 C1216 . . 1.376(7) ? C1212 C1213 . . 1.371(8) ? C1212 H1212 . . .975 ? C1213 C1214 . . 1.365(10) ? C1213 H1213 . . .970 ? C1214 C1215 . . 1.369(11) ? C1214 H1214 . . .963 ? C1215 C1216 . . 1.394(9) ? C1215 H1215 . . .978 ? C1216 H1216 . . .976 ? C1221 C1222 . . 1.398(8) ? C1221 C1226 . . 1.355(7) ? C1222 C1223 . . 1.372(8) ? C1222 H1222 . . .966 ? C1223 C1224 . . 1.362(9) ? C1223 H1223 . . .960 ? C1224 C1225 . . 1.349(10) ? C1224 H1224 . . .985 ? C1225 C1226 . . 1.391(8) ? C1225 H1225 . . .974 ? C1226 H1226 . . .966 ? C1231 C1232 . . 1.383(7) ? C1231 C1236 . . 1.387(7) ? C1232 C1233 . . 1.384(8) ? C1232 H1232 . . .976 ? C1233 C1234 . . 1.371(8) ? C1233 H1233 . . .976 ? C1234 C1235 . . 1.286(10) ? C1234 H1234 . . .959 ? C1235 C1236 . . 1.401(8) ? C1235 H1235 . . .983 ? C1236 H1236 . . .979 ? C101 C102 . . 1.405(8) ? C101 C105 . . 1.421(9) ? C101 H101 . . .978 ? C102 C103 . . 1.423(9) ? C102 H102 . . .969 ? C103 C104 . . 1.375(9) ? C103 H103 . . .979 ? C104 C105 . . 1.418(9) ? C104 H104 . . .959 ? C105 H105 . . .963 ? C1 C2 . . 1.231(6) ? C2 C3 . . 1.377(6) ? C3 C4 . . 1.219(6) ? C4 Ru2 . . 1.989(4) ? Ru2 P21 . . 2.2912(11) ? Ru2 P22 . . 2.2846(14) ? Ru2 C201 . . 2.225(6) ? Ru2 C202 . . 2.242(6) ? Ru2 C203 . . 2.242(5) ? Ru2 C204 . . 2.217(5) ? Ru2 C205 . . 2.219(6) ? P21 C2111 . . 1.844(5) ? P21 C2121 . . 1.828(5) ? P21 C2131 . . 1.836(5) ? C2111 C2112 . . 1.372(7) ? C2111 C2116 . . 1.403(7) ? C2112 C2113 . . 1.407(8) ? C2112 H2112 . . .965 ? C2113 C2114 . . 1.373(9) ? C2113 H2113 . . .977 ? C2114 C2115 . . 1.374(10) ? C2114 H2114 . . .963 ? C2115 C2116 . . 1.379(9) ? C2115 H2115 . . .968 ? C2116 H2116 . . .973 ? C2121 C2122 . . 1.397(8) ? C2121 C2126 . . 1.396(8) ? C2122 C2123 . . 1.383(8) ? C2122 H2122 . . .978 ? C2123 C2124 . . 1.352(11) ? C2123 H2123 . . .973 ? C2124 C2125 . . 1.365(12) ? C2124 H2124 . . .968 ? C2125 C2126 . . 1.402(9) ? C2125 H2125 . . .985 ? C2126 H2126 . . .983 ? C2131 C2132 . . 1.391(7) ? C2131 C2136 . . 1.382(8) ? C2132 C2133 . . 1.382(9) ? C2132 H2132 . . .978 ? C2133 C2134 . . 1.357(11) ? C2133 H2133 . . .976 ? C2134 C2135 . . 1.394(11) ? C2134 H2134 . . .979 ? C2135 C2136 . . 1.388(10) ? C2135 H2135 . . .961 ? C2136 H2136 . . .993 ? P22 C2211 . . 1.853(5) ? P22 C2221 . . 1.832(5) ? P22 C2231 . . 1.845(5) ? C2211 C2212 . . 1.395(7) ? C2211 C2216 . . 1.388(7) ? C2212 C2213 . . 1.383(8) ? C2212 H2212 . . .973 ? C2213 C2214 . . 1.384(10) ? C2213 H2213 . . .978 ? C2214 C2215 . . 1.357(11) ? C2214 H2214 . . .965 ? C2215 C2216 . . 1.376(9) ? C2215 H2215 . . .975 ? C2216 H2216 . . .967 ? C2221 C2222 . . 1.388(8) ? C2221 C2226 . . 1.382(7) ? C2222 C2223 . . 1.371(8) ? C2222 H2222 . . .973 ? C2223 C2224 . . 1.387(9) ? C2223 H2223 . . .974 ? C2224 C2225 . . 1.355(10) ? C2224 H2224 . . .966 ? C2225 C2226 . . 1.399(8) ? C2225 H2225 . . .970 ? C2226 H2226 . . .963 ? C2231 C2232 . . 1.390(7) ? C2231 C2236 . . 1.369(7) ? C2232 C2233 . . 1.384(8) ? C2232 H2232 . . .970 ? C2233 C2234 . . 1.389(8) ? C2233 H2233 . . .978 ? C2234 C2235 . . 1.385(10) ? C2234 H2234 . . .947 ? C2235 C2236 . . 1.403(8) ? C2235 H2235 . . 1.009 ? C2236 H2236 . . .975 ? C201 C202 . . 1.400(8) ? C201 C205 . . 1.393(9) ? C201 H201 . . .988 ? C202 C203 . . 1.417(9) ? C202 H202 . . .962 ? C203 C204 . . 1.386(8) ? C203 H203 . . .977 ? C204 C205 . . 1.417(9) ? C204 H204 . . .969 ? C205 H205 . . .974 ? O301 C302 . . 1.33(4) ? O301 C305 . . 1.36(4) ? C302 C303 . . 1.29(3) ? C302 H302a . . .94 ? C302 H302b . . .95 ? C303 C304 . . 1.37(3) ? C303 H303a . . .944 ? C303 H303b . . .95 ? C304 C305 . . 1.23(3) ? C304 H304a . . .96 ? C304 H304b . . .946 ? C305 H305a . . .95 ? C305 H305b . . .95 ? O401 C402 . . 1.31(3) ? O401 C405 . . 1.39(3) ? C402 C403 . . 1.24(5) ? C402 H402a . . .92 ? C402 H402b . . 1.05 ? C403 C404 . . 1.36(4) ? C403 H403a . . 1.05 ? C403 H403b . . .96 ? C404 C405 . . 1.18(4) ? C404 H404a . . 1.00 ? C404 H404b . . .97 ? C405 H405a . . 1.00 ? C405 H405b . . .95 ? O501 C502 . . 1.45(3) ? O501 C505 . . 1.21(3) ? C502 C503 . . 1.32(3) ? C502 H502a . . .96 ? C502 H502b . . .928 ? C503 C504 . . 1.20(3) ? C503 H503a . . .94 ? C503 H503b . . .934 ? C504 C505 . . 1.43(3) ? C504 H504a . . .92 ? C504 H504b . . .97 ? C505 H505a . . .93 ? C505 H505b . . .96 ? O601 C602 . . 1.35(4) ? O601 C605 . . 1.15(4) ? C602 C603 . . 1.33(4) ? C602 H602a . . .96 ? C602 H602b . . .97 ? C603 C604 . . 1.19(4) ? C603 H603a . . .93 ? C603 H603b . . .97 ? C604 C605 . . 1.36(4) ? C604 H604a . . 1.04 ? C604 H604b . . .89 ? C605 H605a . . .96 ? C605 H605b . . .97 ? O701 C702 . . 1.34(3) ? O701 C705 . . 1.31(3) ? C702 C703 . . 1.31(3) ? C702 H702a . . .92 ? C702 H702b . . .96 ? C703 C704 . . 1.38(3) ? C703 H703a . . .93 ? C703 H703b . . .955 ? C704 C705 . . 1.43(3) ? C704 H704a . . .96 ? C704 H704b . . .93 ? C705 H705a . . 1.00 ? C705 H705b . . .917 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published P11 Ru1 P12 . . . 103.25(5) ? P11 Ru1 C101 . . . 119.59(16) ? P11 Ru1 C102 . . . 92.98(15) ? P11 Ru1 C103 . . . 100.41(16) ? P11 Ru1 C104 . . . 133.76(17) ? P11 Ru1 C105 . . . 154.02(17) ? P11 Ru1 C1 . . . 86.67(13) ? P12 Ru1 C101 . . . 136.91(16) ? P12 Ru1 C102 . . . 153.08(15) ? P12 Ru1 C103 . . . 117.59(16) ? P12 Ru1 C104 . . . 92.55(17) ? P12 Ru1 C105 . . . 101.64(18) ? P12 Ru1 C1 . . . 82.11(14) ? C101 Ru1 C102 . . . 36.6(2) ? C101 Ru1 C103 . . . 61.5(2) ? C101 Ru1 C104 . . . 61.9(2) ? C101 Ru1 C105 . . . 37.1(2) ? C101 Ru1 C1 . . . 95.20(19) ? C102 Ru1 C103 . . . 37.0(2) ? C102 Ru1 C104 . . . 61.0(2) ? C102 Ru1 C105 . . . 61.1(2) ? C102 Ru1 C1 . . . 120.7(2) ? C103 Ru1 C104 . . . 35.8(2) ? C103 Ru1 C105 . . . 60.9(2) ? C103 Ru1 C1 . . . 156.2(2) ? C104 Ru1 C105 . . . 37.1(2) ? C104 Ru1 C1 . . . 139.0(2) ? C105 Ru1 C1 . . . 104.1(2) ? Ru1 P11 C1111 . . . 114.82(16) ? Ru1 P11 C1121 . . . 109.41(15) ? Ru1 P11 C1131 . . . 126.61(16) ? C1111 P11 C1121 . . . 102.0(2) ? C1111 P11 C1131 . . . 96.6(2) ? C1121 P11 C1131 . . . 104.3(2) ? P11 C1111 C1112 . . . 120.8(4) ? P11 C1111 C1116 . . . 120.2(4) ? C1112 C1111 C1116 . . . 118.9(5) ? C1111 C1112 C1113 . . . 120.8(5) ? C1111 C1112 H1112 . . . 119.6 ? C1113 C1112 H1112 . . . 119.6 ? C1112 C1113 C1114 . . . 118.8(6) ? C1112 C1113 H1113 . . . 119.9 ? C1114 C1113 H1113 . . . 121.2 ? C1113 C1114 C1115 . . . 120.5(6) ? C1113 C1114 H1114 . . . 118.4 ? C1115 C1114 H1114 . . . 121.1 ? C1114 C1115 C1116 . . . 120.3(5) ? C1114 C1115 H1115 . . . 119.0 ? C1116 C1115 H1115 . . . 120.7 ? C1111 C1116 C1115 . . . 120.6(5) ? C1111 C1116 H1116 . . . 119.8 ? C1115 C1116 H1116 . . . 119.5 ? P11 C1121 C1122 . . . 123.9(4) ? P11 C1121 C1126 . . . 118.4(4) ? C1122 C1121 C1126 . . . 117.3(4) ? C1121 C1122 C1123 . . . 121.2(5) ? C1121 C1122 H1122 . . . 119.8 ? C1123 C1122 H1122 . . . 119.0 ? C1122 C1123 C1124 . . . 120.1(6) ? C1122 C1123 H1123 . . . 119.6 ? C1124 C1123 H1123 . . . 120.3 ? C1123 C1124 C1125 . . . 119.9(6) ? C1123 C1124 H1124 . . . 118.8 ? C1125 C1124 H1124 . . . 121.2 ? C1124 C1125 C1126 . . . 119.9(6) ? C1124 C1125 H1125 . . . 119.4 ? C1126 C1125 H1125 . . . 120.7 ? C1121 C1126 C1125 . . . 121.6(5) ? C1121 C1126 H1126 . . . 119.0 ? C1125 C1126 H1126 . . . 119.4 ? P11 C1131 C1132 . . . 117.6(4) ? P11 C1131 C1136 . . . 124.9(4) ? C1132 C1131 C1136 . . . 117.2(5) ? C1131 C1132 C1133 . . . 121.1(5) ? C1131 C1132 H1132 . . . 119.0 ? C1133 C1132 H1132 . . . 119.8 ? C1132 C1133 C1134 . . . 120.0(5) ? C1132 C1133 H1133 . . . 120.6 ? C1134 C1133 H1133 . . . 119.3 ? C1133 C1134 C1135 . . . 119.3(6) ? C1133 C1134 H1134 . . . 119.5 ? C1135 C1134 H1134 . . . 121.2 ? C1134 C1135 C1136 . . . 120.8(6) ? C1134 C1135 H1135 . . . 118.3 ? C1136 C1135 H1135 . . . 120.9 ? C1131 C1136 C1135 . . . 121.4(5) ? C1131 C1136 H1136 . . . 119.0 ? C1135 C1136 H1136 . . . 119.6 ? Ru1 P12 C1211 . . . 108.71(18) ? Ru1 P12 C1221 . . . 119.37(17) ? Ru1 P12 C1231 . . . 121.95(15) ? C1211 P12 C1221 . . . 101.0(2) ? C1211 P12 C1231 . . . 103.8(2) ? C1221 P12 C1231 . . . 99.1(2) ? P12 C1211 C1212 . . . 120.6(4) ? P12 C1211 C1216 . . . 123.6(4) ? C1212 C1211 C1216 . . . 115.7(5) ? C1211 C1212 C1213 . . . 123.0(5) ? C1211 C1212 H1212 . . . 118.3 ? C1213 C1212 H1212 . . . 118.7 ? C1212 C1213 C1214 . . . 120.0(6) ? C1212 C1213 H1213 . . . 121.7 ? C1214 C1213 H1213 . . . 118.4 ? C1213 C1214 C1215 . . . 118.9(6) ? C1213 C1214 H1214 . . . 120.6 ? C1215 C1214 H1214 . . . 120.5 ? C1214 C1215 C1216 . . . 120.8(6) ? C1214 C1215 H1215 . . . 119.1 ? C1216 C1215 H1215 . . . 120.0 ? C1211 C1216 C1215 . . . 121.5(6) ? C1211 C1216 H1216 . . . 120.1 ? C1215 C1216 H1216 . . . 118.4 ? P12 C1221 C1222 . . . 119.9(4) ? P12 C1221 C1226 . . . 121.9(4) ? C1222 C1221 C1226 . . . 118.1(4) ? C1221 C1222 C1223 . . . 120.8(5) ? C1221 C1222 H1222 . . . 118.8 ? C1223 C1222 H1222 . . . 120.4 ? C1222 C1223 C1224 . . . 119.6(6) ? C1222 C1223 H1223 . . . 119.1 ? C1224 C1223 H1223 . . . 121.2 ? C1223 C1224 C1225 . . . 120.6(6) ? C1223 C1224 H1224 . . . 118.5 ? C1225 C1224 H1224 . . . 120.8 ? C1224 C1225 C1226 . . . 120.0(6) ? C1224 C1225 H1225 . . . 120.2 ? C1226 C1225 H1225 . . . 119.8 ? C1221 C1226 C1225 . . . 120.9(6) ? C1221 C1226 H1226 . . . 119.1 ? C1225 C1226 H1226 . . . 120.0 ? P12 C1231 C1232 . . . 118.0(3) ? P12 C1231 C1236 . . . 124.2(4) ? C1232 C1231 C1236 . . . 117.7(4) ? C1231 C1232 C1233 . . . 121.0(4) ? C1231 C1232 H1232 . . . 119.2 ? C1233 C1232 H1232 . . . 119.8 ? C1232 C1233 C1234 . . . 119.5(5) ? C1232 C1233 H1233 . . . 122.9 ? C1234 C1233 H1233 . . . 117.6 ? C1233 C1234 C1235 . . . 120.0(6) ? C1233 C1234 H1234 . . . 122.4 ? C1235 C1234 H1234 . . . 117.5 ? C1234 C1235 C1236 . . . 123.2(6) ? C1234 C1235 H1235 . . . 118.1 ? C1236 C1235 H1235 . . . 118.6 ? C1231 C1236 C1235 . . . 118.5(5) ? C1231 C1236 H1236 . . . 120.4 ? C1235 C1236 H1236 . . . 121.1 ? Ru1 C101 C102 . . . 71.7(3) ? Ru1 C101 C105 . . . 71.0(4) ? Ru1 C101 H101 . . . 121.4 ? C102 C101 C105 . . . 107.0(5) ? C102 C101 H101 . . . 126.6 ? C105 C101 H101 . . . 126.4 ? Ru1 C102 C101 . . . 71.7(3) ? Ru1 C102 C103 . . . 71.7(3) ? Ru1 C102 H102 . . . 123.2 ? C101 C102 C103 . . . 108.3(5) ? C101 C102 H102 . . . 125.9 ? C103 C102 H102 . . . 125.8 ? Ru1 C103 C102 . . . 71.3(3) ? Ru1 C103 C104 . . . 71.6(3) ? Ru1 C103 H103 . . . 122.2 ? C102 C103 C104 . . . 108.4(5) ? C102 C103 H103 . . . 124.9 ? C104 C103 H103 . . . 126.7 ? Ru1 C104 C103 . . . 72.6(3) ? Ru1 C104 C105 . . . 71.3(3) ? Ru1 C104 H104 . . . 123.0 ? C103 C104 C105 . . . 108.4(6) ? C103 C104 H104 . . . 125.4 ? C105 C104 H104 . . . 126.2 ? Ru1 C105 C101 . . . 71.9(3) ? Ru1 C105 C104 . . . 71.6(4) ? Ru1 C105 H105 . . . 123.0 ? C101 C105 C104 . . . 108.0(5) ? C101 C105 H105 . . . 125.9 ? C104 C105 H105 . . . 126.1 ? Ru1 C1 C2 . . . 175.5(4) ? C1 C2 C3 . . . 177.3(5) ? C2 C3 C4 . . . 176.2(6) ? C3 C4 Ru2 . . . 174.5(5) ? C4 Ru2 P21 . . . 86.33(13) ? C4 Ru2 P22 . . . 82.49(15) ? C4 Ru2 C201 . . . 94.7(2) ? C4 Ru2 C202 . . . 119.9(2) ? C4 Ru2 C203 . . . 155.5(2) ? C4 Ru2 C204 . . . 138.7(2) ? C4 Ru2 C205 . . . 103.6(2) ? P21 Ru2 P22 . . . 103.11(5) ? P21 Ru2 C201 . . . 120.10(16) ? P21 Ru2 C202 . . . 93.54(16) ? P21 Ru2 C203 . . . 100.63(15) ? P21 Ru2 C204 . . . 134.33(16) ? P21 Ru2 C205 . . . 154.21(16) ? P22 Ru2 C201 . . . 136.49(16) ? P22 Ru2 C202 . . . 153.16(16) ? P22 Ru2 C203 . . . 118.04(16) ? P22 Ru2 C204 . . . 92.56(16) ? P22 Ru2 C205 . . . 101.79(17) ? C201 Ru2 C202 . . . 36.5(2) ? C201 Ru2 C203 . . . 61.4(2) ? C201 Ru2 C204 . . . 61.6(2) ? C201 Ru2 C205 . . . 36.5(2) ? C202 Ru2 C203 . . . 36.8(2) ? C202 Ru2 C204 . . . 61.0(2) ? C202 Ru2 C205 . . . 60.8(2) ? C203 Ru2 C204 . . . 36.2(2) ? C203 Ru2 C205 . . . 61.1(2) ? C204 Ru2 C205 . . . 37.3(2) ? Ru2 P21 C2111 . . . 114.95(16) ? Ru2 P21 C2121 . . . 110.26(16) ? Ru2 P21 C2131 . . . 126.35(16) ? C2111 P21 C2121 . . . 101.9(2) ? C2111 P21 C2131 . . . 95.9(2) ? C2121 P21 C2131 . . . 104.2(2) ? P21 C2111 C2112 . . . 121.9(4) ? P21 C2111 C2116 . . . 119.4(4) ? C2112 C2111 C2116 . . . 118.6(5) ? C2111 C2112 C2113 . . . 120.6(5) ? C2111 C2112 H2112 . . . 119.5 ? C2113 C2112 H2112 . . . 119.9 ? C2112 C2113 C2114 . . . 119.7(6) ? C2112 C2113 H2113 . . . 119.5 ? C2114 C2113 H2113 . . . 120.8 ? C2113 C2114 C2115 . . . 120.3(6) ? C2113 C2114 H2114 . . . 118.8 ? C2115 C2114 H2114 . . . 121.0 ? C2114 C2115 C2116 . . . 120.2(6) ? C2114 C2115 H2115 . . . 119.4 ? C2116 C2115 H2115 . . . 120.4 ? C2111 C2116 C2115 . . . 120.6(5) ? C2111 C2116 H2116 . . . 119.0 ? C2115 C2116 H2116 . . . 120.4 ? P21 C2121 C2122 . . . 123.3(4) ? P21 C2121 C2126 . . . 118.8(4) ? C2122 C2121 C2126 . . . 117.4(5) ? C2121 C2122 C2123 . . . 120.4(6) ? C2121 C2122 H2122 . . . 119.5 ? C2123 C2122 H2122 . . . 120.1 ? C2122 C2123 C2124 . . . 121.3(6) ? C2122 C2123 H2123 . . . 118.2 ? C2124 C2123 H2123 . . . 120.5 ? C2123 C2124 C2125 . . . 120.4(6) ? C2123 C2124 H2124 . . . 119.5 ? C2125 C2124 H2124 . . . 120.1 ? C2124 C2125 C2126 . . . 119.5(6) ? C2124 C2125 H2125 . . . 121.4 ? C2126 C2125 H2125 . . . 119.0 ? C2121 C2126 C2125 . . . 120.9(6) ? C2121 C2126 H2126 . . . 118.8 ? C2125 C2126 H2126 . . . 120.2 ? P21 C2131 C2132 . . . 116.8(4) ? P21 C2131 C2136 . . . 125.5(4) ? C2132 C2131 C2136 . . . 117.4(5) ? C2131 C2132 C2133 . . . 122.1(5) ? C2131 C2132 H2132 . . . 118.3 ? C2133 C2132 H2132 . . . 119.6 ? C2132 C2133 C2134 . . . 119.4(6) ? C2132 C2133 H2133 . . . 120.0 ? C2134 C2133 H2133 . . . 120.6 ? C2133 C2134 C2135 . . . 120.3(7) ? C2133 C2134 H2134 . . . 121.1 ? C2135 C2134 H2134 . . . 118.5 ? C2134 C2135 C2136 . . . 119.5(7) ? C2134 C2135 H2135 . . . 120.5 ? C2136 C2135 H2135 . . . 120.0 ? C2131 C2136 C2135 . . . 121.2(5) ? C2131 C2136 H2136 . . . 119.0 ? C2135 C2136 H2136 . . . 119.8 ? Ru2 P22 C2211 . . . 108.80(19) ? Ru2 P22 C2221 . . . 118.97(17) ? Ru2 P22 C2231 . . . 122.24(16) ? C2211 P22 C2221 . . . 101.4(2) ? C2211 P22 C2231 . . . 103.8(2) ? C2221 P22 C2231 . . . 98.9(2) ? P22 C2211 C2212 . . . 119.4(4) ? P22 C2211 C2216 . . . 123.0(4) ? C2212 C2211 C2216 . . . 117.4(5) ? C2211 C2212 C2213 . . . 121.8(5) ? C2211 C2212 H2212 . . . 119.4 ? C2213 C2212 H2212 . . . 118.7 ? C2212 C2213 C2214 . . . 119.1(6) ? C2212 C2213 H2213 . . . 121.3 ? C2214 C2213 H2213 . . . 119.6 ? C2213 C2214 C2215 . . . 119.4(6) ? C2213 C2214 H2214 . . . 120.2 ? C2215 C2214 H2214 . . . 120.5 ? C2214 C2215 C2216 . . . 122.0(7) ? C2214 C2215 H2215 . . . 118.3 ? C2216 C2215 H2215 . . . 119.7 ? C2211 C2216 C2215 . . . 120.2(6) ? C2211 C2216 H2216 . . . 119.4 ? C2215 C2216 H2216 . . . 120.4 ? P22 C2221 C2222 . . . 120.9(4) ? P22 C2221 C2226 . . . 121.4(4) ? C2222 C2221 C2226 . . . 117.7(5) ? C2221 C2222 C2223 . . . 121.9(5) ? C2221 C2222 H2222 . . . 119.0 ? C2223 C2222 H2222 . . . 119.1 ? C2222 C2223 C2224 . . . 119.8(6) ? C2222 C2223 H2223 . . . 120.4 ? C2224 C2223 H2223 . . . 119.8 ? C2223 C2224 C2225 . . . 119.4(5) ? C2223 C2224 H2224 . . . 120.2 ? C2225 C2224 H2224 . . . 120.5 ? C2224 C2225 C2226 . . . 121.0(6) ? C2224 C2225 H2225 . . . 118.9 ? C2226 C2225 H2225 . . . 120.1 ? C2221 C2226 C2225 . . . 120.3(5) ? C2221 C2226 H2226 . . . 120.1 ? C2225 C2226 H2226 . . . 119.6 ? P22 C2231 C2232 . . . 117.2(3) ? P22 C2231 C2236 . . . 124.3(4) ? C2232 C2231 C2236 . . . 118.5(4) ? C2231 C2232 C2233 . . . 120.4(4) ? C2231 C2232 H2232 . . . 119.3 ? C2233 C2232 H2232 . . . 120.3 ? C2232 C2233 C2234 . . . 119.6(5) ? C2232 C2233 H2233 . . . 121.2 ? C2234 C2233 H2233 . . . 119.1 ? C2233 C2234 C2235 . . . 121.6(5) ? C2233 C2234 H2234 . . . 121.3 ? C2235 C2234 H2234 . . . 117.1 ? C2234 C2235 C2236 . . . 116.6(5) ? C2234 C2235 H2235 . . . 122.5 ? C2236 C2235 H2235 . . . 120.9 ? C2231 C2236 C2235 . . . 123.2(5) ? C2231 C2236 H2236 . . . 118.2 ? C2235 C2236 H2236 . . . 118.7 ? Ru2 C201 C202 . . . 72.4(4) ? Ru2 C201 C205 . . . 71.5(3) ? Ru2 C201 H201 . . . 120.4 ? C202 C201 C205 . . . 107.9(5) ? C202 C201 H201 . . . 126.5 ? C205 C201 H201 . . . 125.6 ? Ru2 C202 C201 . . . 71.0(3) ? Ru2 C202 C203 . . . 71.6(3) ? Ru2 C202 H202 . . . 123.4 ? C201 C202 C203 . . . 108.1(5) ? C201 C202 H202 . . . 125.4 ? C203 C202 H202 . . . 126.5 ? Ru2 C203 C202 . . . 71.6(3) ? Ru2 C203 C204 . . . 70.9(3) ? Ru2 C203 H203 . . . 122.9 ? C202 C203 C204 . . . 107.8(5) ? C202 C203 H203 . . . 126.8 ? C204 C203 H203 . . . 125.4 ? Ru2 C204 C203 . . . 72.9(3) ? Ru2 C204 C205 . . . 71.4(3) ? Ru2 C204 H204 . . . 121.8 ? C203 C204 C205 . . . 108.1(5) ? C203 C204 H204 . . . 126.3 ? C205 C204 H204 . . . 125.6 ? Ru2 C205 C201 . . . 72.0(3) ? Ru2 C205 C204 . . . 71.3(3) ? Ru2 C205 H205 . . . 122.8 ? C201 C205 C204 . . . 108.2(5) ? C201 C205 H205 . . . 126.2 ? C204 C205 H205 . . . 125.6 ? C302 O301 C305 . . . 107(2) ? O301 C302 C303 . . . 107(2) ? O301 C302 H302a . . . 112 ? O301 C302 H302b . . . 112 ? C303 C302 H302a . . . 108 ? C303 C302 H302b . . . 107 ? H302a C302 H302b . . . 110 ? C302 C303 C304 . . . 108(2) ? C302 C303 H303a . . . 112 ? C302 C303 H303b . . . 112 ? C304 C303 H303a . . . 108 ? C304 C303 H303b . . . 107 ? H303a C303 H303b . . . 110 ? C303 C304 C305 . . . 108(2) ? C303 C304 H304a . . . 111 ? C303 C304 H304b . . . 113 ? C305 C304 H304a . . . 107 ? C305 C304 H304b . . . 108 ? H304a C304 H304b . . . 108.9 ? O301 C305 C304 . . . 108(2) ? O301 C305 H305a . . . 106 ? O301 C305 H305b . . . 108 ? C304 C305 H305a . . . 113 ? C304 C305 H305b . . . 112 ? H305a C305 H305b . . . 109.2 ? C402 O401 C405 . . . 106(2) ? O401 C402 C403 . . . 107(2) ? O401 C402 H402a . . . 126 ? O401 C402 H402b . . . 118 ? C403 C402 H402a . . . 105 ? C403 C402 H402b . . . 92 ? H402a C402 H402b . . . 104 ? C402 C403 C404 . . . 108(2) ? C402 C403 H403a . . . 117 ? C402 C403 H403b . . . 131 ? C404 C403 H403a . . . 94 ? C404 C403 H403b . . . 98 ? H403a C403 H403b . . . 101 ? C403 C404 C405 . . . 107(2) ? C403 C404 H404a . . . 121 ? C403 C404 H404b . . . 123 ? C405 C404 H404a . . . 99 ? C405 C404 H404b . . . 97 ? H404a C404 H404b . . . 105 ? O401 C405 C404 . . . 106.1(19) ? O401 C405 H405a . . . 95 ? O401 C405 H405b . . . 102 ? C404 C405 H405a . . . 122 ? C404 C405 H405b . . . 121 ? H405a C405 H405b . . . 105 ? C502 O501 C505 . . . 105.0(17) ? O501 C502 C503 . . . 105.8(16) ? O501 C502 H502a . . . 110 ? O501 C502 H502b . . . 112 ? C503 C502 H502a . . . 108 ? C503 C502 H502b . . . 111 ? H502a C502 H502b . . . 110.5 ? C502 C503 C504 . . . 105.3(18) ? C502 C503 H503a . . . 112 ? C502 C503 H503b . . . 111 ? C504 C503 H503a . . . 108 ? C504 C503 H503b . . . 110 ? H503a C503 H503b . . . 111.5 ? C503 C504 C505 . . . 106.8(18) ? C503 C504 H504a . . . 113 ? C503 C504 H504b . . . 109 ? C505 C504 H504a . . . 110 ? C505 C504 H504b . . . 108 ? H504a C504 H504b . . . 110.5 ? O501 C505 C504 . . . 104.6(18) ? O501 C505 H505a . . . 110 ? O501 C505 H505b . . . 108 ? C504 C505 H505a . . . 112 ? C504 C505 H505b . . . 112 ? H505a C505 H505b . . . 111 ? C602 O601 C605 . . . 106(2) ? O601 C602 C603 . . . 104(2) ? O601 C602 H602a . . . 99 ? O601 C602 H602b . . . 104 ? C603 C602 H602a . . . 119 ? C603 C602 H602b . . . 121 ? C605 C602 H602a . . . 127 ? C605 C602 H602b . . . 107.0 ? H602a C602 H602b . . . 107 ? C602 C603 C604 . . . 107(2) ? C602 C603 H603a . . . 105 ? C602 C603 H603b . . . 102 ? C604 C603 H603a . . . 123 ? C604 C603 H603b . . . 109 ? H603a C603 H603b . . . 109.4 ? C603 C604 C605 . . . 108(2) ? C603 C604 H604a . . . 96 ? C603 C604 H604b . . . 105 ? C605 C604 H604a . . . 111 ? C605 C604 H604b . . . 126 ? H604a C604 H604b . . . 106.8 ? O601 C605 C604 . . . 106(2) ? O601 C605 H605a . . . 121 ? O601 C605 H605b . . . 121 ? C604 C605 H605a . . . 100 ? C604 C605 H605b . . . 97 ? H605a C605 H605b . . . 107 ? C702 O701 C705 . . . 104.7(17) ? O701 C702 C703 . . . 107.4(15) ? O701 C702 H702a . . . 110 ? O701 C702 H702b . . . 105 ? C703 C702 H702a . . . 112 ? C703 C702 H702b . . . 111 ? H702a C702 H702b . . . 111.0 ? C702 C703 C704 . . . 106.2(16) ? C702 C703 H703a . . . 109 ? C702 C703 H703b . . . 109 ? C704 C703 H703a . . . 112 ? C704 C703 H703b . . . 109.1 ? H703a C703 H703b . . . 111.1 ? C703 C704 C705 . . . 104.1(15) ? C703 C704 H704a . . . 108.3 ? C703 C704 H704b . . . 111.7 ? C705 C704 H704a . . . 111.9 ? C705 C704 H704b . . . 110.2 ? H704a C704 H704b . . . 110.4 ? O701 C705 C704 . . . 104.0(15) ? O701 C705 H705a . . . 109.8 ? O701 C705 H705b . . . 115 ? C704 C705 H705a . . . 108 ? C704 C705 H705b . . . 111.7 ? H705a C705 H705b . . . 108.1 ? 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 #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _exptl_crystal_F_000 3736 _reflns_limit_h_min 0 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 36 _reflns_limit_l_min -31 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 13.291 _diffrn_reflns_av_sigmaI/netI .166 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 50 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .138 _refine_ls_wR_factor_all .069 _refine_ls_goodness_of_fit_all 1.231 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? data_br858 _database_code_depnum_ccdc_archive 'CCDC 223453' _audit_creation_method Xtal3.6 _audit_creation_date 02-01-13 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C66 H58 P4 Ru2' _chemical_formula_moiety 'C66 H58 P4 Ru2' _chemical_formula_weight 1177.23 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21_1 _symmetry_space_group_name_Hall p_2yb loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,-z _cell_length_a 9.434(2) _cell_length_b 18.936(4) _cell_length_c 15.324(4) _cell_angle_alpha 90.00000 _cell_angle_beta 106.405(4) _cell_angle_gamma 90.00000 _cell_volume 2626.1(10) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4902 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 24.5 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu .74 _exptl_crystal_description prism _exptl_crystal_size_max .14 _exptl_crystal_size_mid .11 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour orange _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .53 _exptl_absorpt_correction_T_max .84 _diffrn_reflns_number 9069 _reflns_number_total 4763 _reflns_number_gt 4186 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_av_R_equivalents .033 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .048 _refine_ls_wR_factor_ref .055 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_number_reflns 4186 _refine_ls_number_parameters 648 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .006 _refine_diff_density_min -2.079 _refine_diff_density_max 1.424 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration unk # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 132 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 116 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 .64605(7) .50000(5) .95021(5) .0209(3) Uani ? ? 1.00000 ? ? Ru2 .02193(7) .52188(5) .49657(5) .0226(3) Uani ? ? 1.00000 ? ? P11 .7167(3) .41891(14) .86573(17) .0229(12) Uani ? ? 1.00000 ? ? C1111 .9089(11) .3897(5) .9111(7) .028(5) Uani ? ? 1.00000 ? ? C1112 .9451(11) .3384(6) .9779(7) .027(5) Uani ? ? 1.00000 ? ? C1113 1.0909(12) .3199(5) 1.0180(7) .031(5) Uani ? ? 1.00000 ? ? C1114 1.2020(11) .3540(5) .9911(8) .032(5) Uani ? ? 1.00000 ? ? C1115 1.1705(11) .4052(6) .9264(9) .038(6) Uani ? ? 1.00000 ? ? C1116 1.0227(11) .4243(5) .8848(7) .029(5) Uani ? ? 1.00000 ? ? C1121 .6230(11) .3345(5) .8444(7) .024(5) Uani ? ? 1.00000 ? ? C1122 .4962(11) .3215(5) .8733(7) .029(5) Uani ? ? 1.00000 ? ? C1123 .4285(12) .2567(6) .8597(8) .036(6) Uani ? ? 1.00000 ? ? C1124 .4774(12) .2033(5) .8136(8) .035(5) Uani ? ? 1.00000 ? ? C1125 .6042(11) .2150(5) .7856(7) .028(5) Uani ? ? 1.00000 ? ? C1126 .6740(11) .2793(6) .8013(7) .030(5) Uani ? ? 1.00000 ? ? C110 .7010(12) .4522(5) .7498(8) .031(5) Uani ? ? 1.00000 ? ? C120 .7052(11) .5325(7) .7468(7) .035(5) Uani ? ? 1.00000 ? ? P12 .7253(3) .57407(14) .85856(17) .0229(12) Uani ? ? 1.00000 ? ? C1211 .9169(10) .6045(5) .9002(7) .024(5) Uani ? ? 1.00000 ? ? C1212 1.0234(11) .6013(6) .8488(7) .034(5) Uani ? ? 1.00000 ? ? C1213 1.1646(12) .6252(6) .8882(8) .038(6) Uani ? ? 1.00000 ? ? C1214 1.2084(12) .6518(6) .9742(9) .039(6) Uani ? ? 1.00000 ? ? C1215 1.1054(12) .6560(7) 1.0251(8) .041(6) Uani ? ? 1.00000 ? ? C1216 .9615(11) .6331(6) .9851(7) .032(5) Uani ? ? 1.00000 ? ? C1221 .6319(11) .6602(5) .8304(7) .025(5) Uani ? ? 1.00000 ? ? C1222 .5413(11) .6852(6) .8810(7) .031(5) Uani ? ? 1.00000 ? ? C1223 .4807(12) .7523(5) .8642(8) .031(6) Uani ? ? 1.00000 ? ? C1224 .5042(12) .7933(6) .7991(8) .037(6) Uani ? ? 1.00000 ? ? C1225 .5899(14) .7685(7) .7457(8) .044(6) Uani ? ? 1.00000 ? ? C1226 .6561(12) .7032(6) .7626(7) .034(6) Uani ? ? 1.00000 ? ? C1 .4594(9) .5052(5) .8462(6) .021(4) Uani ? ? 1.00000 ? ? C2 .3505(9) .5090(5) .7810(6) .022(4) Uani ? ? 1.00000 ? ? C3 .2327(9) .5145(5) .7021(6) .025(4) Uani ? ? 1.00000 ? ? C4 .1436(9) .5191(6) .6271(6) .025(4) Uani ? ? 1.00000 ? ? P21 .1068(3) .63301(14) .50021(17) .0244(12) Uani ? ? 1.00000 ? ? C2111 .0446(10) .6843(6) .3951(7) .029(5) Uani ? ? 1.00000 ? ? C2112 .0371(12) .7590(5) .3927(8) .032(5) Uani ? ? 1.00000 ? ? C2113 -.0062(12) .7940(6) .3104(7) .034(6) Uani ? ? 1.00000 ? ? C2114 -.0377(12) .7582(6) .2298(8) .035(6) Uani ? ? 1.00000 ? ? C2115 -.0286(11) .6849(6) .2315(7) .035(5) Uani ? ? 1.00000 ? ? C2116 .0088(11) .6492(5) .3124(7) .029(5) Uani ? ? 1.00000 ? ? C2121 .0635(11) .6918(5) .5829(6) .026(5) Uani ? ? 1.00000 ? ? C2122 .1575(12) .7095(6) .6658(7) .034(5) Uani ? ? 1.00000 ? ? C2123 .1116(14) .7521(6) .7270(9) .046(7) Uani ? ? 1.00000 ? ? C2124 -.0311(13) .7770(6) .7040(8) .037(6) Uani ? ? 1.00000 ? ? C2125 -.1280(13) .7618(6) .6217(8) .037(6) Uani ? ? 1.00000 ? ? C2126 -.0834(12) .7182(6) .5609(7) .034(5) Uani ? ? 1.00000 ? ? C210 .3108(12) .6371(6) .5206(8) .033(5) Uani ? ? 1.00000 ? ? C220 .3772(10) .5633(6) .5330(7) .029(5) Uani ? ? 1.00000 ? ? P22 .2430(2) .49640(15) .47439(15) .0226(10) Uani ? ? 1.00000 ? ? C2211 .2560(9) .4953(6) .3578(6) .027(4) Uani ? ? 1.00000 ? ? C2212 .3667(11) .5301(6) .3291(7) .035(5) Uani ? ? 1.00000 ? ? C2213 .3760(13) .5238(7) .2420(8) .048(6) Uani ? ? 1.00000 ? ? C2214 .2727(14) .4847(6) .1795(8) .045(7) Uani ? ? 1.00000 ? ? C2215 .1578(11) .4496(6) .2052(8) .035(5) Uani ? ? 1.00000 ? ? C2216 .1548(11) .4553(6) .2935(7) .031(5) Uani ? ? 1.00000 ? ? C2221 .3361(11) .4148(6) .5158(7) .026(5) Uani ? ? 1.00000 ? ? C2222 .2894(12) .3709(6) .5742(7) .032(5) Uani ? ? 1.00000 ? ? C2223 .3608(12) .3080(6) .6054(7) .038(6) Uani ? ? 1.00000 ? ? C2224 .4823(13) .2863(6) .5759(8) .043(6) Uani ? ? 1.00000 ? ? C2225 .5295(12) .3288(6) .5161(7) .039(6) Uani ? ? 1.00000 ? ? C2226 .4615(11) .3917(6) .4875(8) .034(5) Uani ? ? 1.00000 ? ? C101 .5706(12) .4549(5) 1.0654(7) .033(6) Uani ? ? 1.00000 ? ? C102 .7252(12) .4474(5) 1.0855(7) .030(5) Uani ? ? 1.00000 ? ? C103 .7905(9) .5134(6) 1.0935(6) .029(5) Uani ? ? 1.00000 ? ? C104 .6763(12) .5641(5) 1.0776(7) .028(5) Uani ? ? 1.00000 ? ? C105 .5396(10) .5288(7) 1.0590(6) .032(5) Uani ? ? 1.00000 ? ? C201 -.2105(9) .5214(7) .5071(6) .035(5) Uani ? ? 1.00000 ? ? C202 -.2110(10) .5437(6) .4187(7) .034(5) Uani ? ? 1.00000 ? ? C203 -.1622(10) .4904(7) .3746(7) .036(5) Uani ? ? 1.00000 ? ? C204 -.1290(11) .4310(6) .4346(7) .034(5) Uani ? ? 1.00000 ? ? C205 -.1560(11) .4502(7) .5156(8) .043(6) Uani ? ? 1.00000 ? ? H1112 .86717 .31535 .99765 .03200 Uiso ? ? 1.00000 ? ? H1113 1.11663 .28255 1.06414 .04000 Uiso ? ? 1.00000 ? ? H1114 1.30373 .34137 1.02138 .04200 Uiso ? ? 1.00000 ? ? H1115 1.24747 .42848 .90773 .04700 Uiso ? ? 1.00000 ? ? H1116 .99858 .46097 .83941 .03700 Uiso ? ? 1.00000 ? ? H1122 .46095 .35726 .90591 .03500 Uiso ? ? 1.00000 ? ? H1123 .34425 .24707 .88308 .04900 Uiso ? ? 1.00000 ? ? H1124 .42513 .15897 .79991 .04400 Uiso ? ? 1.00000 ? ? H1125 .64158 .17794 .75484 .03600 Uiso ? ? 1.00000 ? ? H1126 .76096 .28632 .78118 .03900 Uiso ? ? 1.00000 ? ? H110a .78011 .43333 .72908 .04100 Uiso ? ? 1.00000 ? ? H110b .60951 .43570 .70890 .04100 Uiso ? ? 1.00000 ? ? H120a .61550 .54947 .70520 .04000 Uiso ? ? 1.00000 ? ? H120b .78604 .54710 .72504 .04000 Uiso ? ? 1.00000 ? ? H1212 .99368 .58191 .78807 .04200 Uiso ? ? 1.00000 ? ? H1213 1.23499 .62219 .85459 .05000 Uiso ? ? 1.00000 ? ? H1214 1.30896 .66711 .99958 .04700 Uiso ? ? 1.00000 ? ? H1215 1.13434 .67309 1.08670 .05100 Uiso ? ? 1.00000 ? ? H1216 .89054 .63614 1.01768 .03900 Uiso ? ? 1.00000 ? ? H1222 .52204 .65626 .92811 .03800 Uiso ? ? 1.00000 ? ? H1223 .41855 .76905 .90004 .03700 Uiso ? ? 1.00000 ? ? H1224 .46533 .84016 .79163 .04700 Uiso ? ? 1.00000 ? ? H1225 .59908 .79558 .69375 .05300 Uiso ? ? 1.00000 ? ? H1226 .72155 .68639 .72819 .04400 Uiso ? ? 1.00000 ? ? H2112 .06412 .78442 .44932 .04100 Uiso ? ? 1.00000 ? ? H2113 -.01668 .84454 .31015 .04400 Uiso ? ? 1.00000 ? ? H2114 -.06362 .78223 .17119 .04800 Uiso ? ? 1.00000 ? ? H2115 -.05270 .65815 .17615 .04300 Uiso ? ? 1.00000 ? ? H2116 .01159 .59856 .31247 .03700 Uiso ? ? 1.00000 ? ? H2122 .25659 .69006 .68210 .04500 Uiso ? ? 1.00000 ? ? H2123 .17900 .76446 .78475 .05800 Uiso ? ? 1.00000 ? ? H2124 -.06501 .80427 .74731 .04600 Uiso ? ? 1.00000 ? ? H2125 -.22403 .78195 .60559 .05000 Uiso ? ? 1.00000 ? ? H2126 -.15389 .70549 .50118 .04300 Uiso ? ? 1.00000 ? ? H210a .33480 .65955 .47012 .04200 Uiso ? ? 1.00000 ? ? H210b .35535 .66480 .57399 .04200 Uiso ? ? 1.00000 ? ? H220a .40931 .55207 .59653 .04000 Uiso ? ? 1.00000 ? ? H220b .46125 .56127 .50976 .04000 Uiso ? ? 1.00000 ? ? H2212 .43894 .55886 .37356 .04600 Uiso ? ? 1.00000 ? ? H2213 .45552 .54496 .22341 .06100 Uiso ? ? 1.00000 ? ? H2214 .27518 .48028 .11641 .05300 Uiso ? ? 1.00000 ? ? H2215 .08292 .42178 .16164 .04400 Uiso ? ? 1.00000 ? ? H2216 .08113 .43022 .31311 .04200 Uiso ? ? 1.00000 ? ? H2222 .20428 .38269 .59337 .03600 Uiso ? ? 1.00000 ? ? H2223 .32825 .27969 .64840 .04500 Uiso ? ? 1.00000 ? ? H2224 .52797 .24066 .59599 .05700 Uiso ? ? 1.00000 ? ? H2225 .61145 .31450 .49467 .04700 Uiso ? ? 1.00000 ? ? H2226 .49752 .41993 .44689 .04100 Uiso ? ? 1.00000 ? ? H101 .49972 .41743 1.05699 .04400 Uiso ? ? 1.00000 ? ? H102 .77603 .40210 1.09384 .04000 Uiso ? ? 1.00000 ? ? H103 .89546 .52303 1.10567 .03400 Uiso ? ? 1.00000 ? ? H104 .68895 .61381 1.08151 .04000 Uiso ? ? 1.00000 ? ? H105 .44482 .55077 1.04463 .03700 Uiso ? ? 1.00000 ? ? H201 -.23929 .54813 .55266 .04500 Uiso ? ? 1.00000 ? ? H202 -.24191 .58848 .39256 .04400 Uiso ? ? 1.00000 ? ? H203 -.15215 .49313 .31274 .04600 Uiso ? ? 1.00000 ? ? H204 -.09700 .38419 .42044 .04700 Uiso ? ? 1.00000 ? ? H205 -.13974 .42076 .56995 .05300 Uiso ? ? 1.00000 ? ? 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 Ru1 .0155(3) .0269(4) .0242(4) .0000(3) .0119(3) -.0003(3) Ru2 .0146(3) .0315(4) .0253(4) .0004(3) .0115(3) .0008(3) P11 .0163(13) .0285(14) .0270(14) .0011(10) .0112(11) -.0020(10) C1111 .019(5) .027(6) .043(6) .001(4) .014(5) -.007(4) C1112 .021(5) .037(6) .027(5) -.002(4) .014(4) -.002(4) C1113 .030(6) .035(6) .028(5) .004(4) .008(5) -.004(4) C1114 .020(6) .031(6) .046(7) .001(4) .013(5) -.007(5) C1115 .018(6) .033(6) .069(9) -.006(4) .022(6) -.012(6) C1116 .018(5) .028(5) .048(6) .001(4) .022(5) .003(5) C1121 .020(5) .029(6) .024(5) .003(4) .008(4) -.005(4) C1122 .020(6) .035(6) .040(6) -.001(4) .020(5) -.008(4) C1123 .028(6) .040(7) .051(8) -.005(5) .030(6) -.007(5) C1124 .027(6) .028(6) .050(7) -.007(4) .009(5) .001(5) C1125 .026(5) .029(6) .032(6) .001(4) .012(5) .001(4) C1126 .023(6) .036(6) .035(6) -.005(5) .014(5) -.003(5) C110 .034(6) .031(6) .034(6) .001(4) .019(5) -.003(4) C120 .030(5) .052(7) .026(5) -.007(5) .014(4) -.003(5) P12 .0168(13) .0280(14) .0268(14) -.0017(10) .0107(11) .0000(10) C1211 .012(5) .027(5) .038(6) .001(4) .018(4) .006(4) C1212 .025(6) .042(6) .039(6) -.000(5) .019(5) -.008(5) C1213 .026(6) .043(7) .054(8) -.007(5) .025(5) -.008(5) C1214 .021(6) .038(7) .060(8) -.004(5) .017(6) .004(6) C1215 .026(6) .061(8) .039(7) -.010(5) .015(5) -.007(6) C1216 .025(6) .046(7) .029(6) -.012(5) .014(5) -.013(5) C1221 .019(5) .029(5) .030(6) -.001(4) .011(4) -.002(4) C1222 .024(6) .042(6) .029(6) -.001(4) .012(5) .005(5) C1223 .025(6) .032(7) .043(7) .004(4) .020(5) -.005(4) C1224 .031(7) .041(7) .040(6) .006(5) .012(5) -.000(5) C1225 .044(7) .046(7) .048(7) .002(6) .024(6) .011(6) C1226 .030(6) .041(7) .040(6) .004(5) .025(5) .011(5) C1 .024(4) .020(5) .028(4) -.007(4) .021(4) -.002(4) C2 .023(4) .017(5) .032(5) -.003(4) .021(4) -.003(4) C3 .021(4) .027(6) .034(5) .001(4) .017(4) -.001(4) C4 .015(4) .034(6) .033(5) .006(4) .019(4) -.001(5) P21 .0191(12) .0285(14) .0296(13) .0005(10) .0132(10) -.0007(11) C2111 .015(5) .040(6) .036(6) .001(4) .015(4) -.000(5) C2112 .035(6) .029(6) .038(6) -.003(4) .019(5) -.003(4) C2113 .035(7) .032(6) .045(7) -.000(5) .027(5) .007(5) C2114 .030(6) .041(7) .038(6) -.001(5) .017(5) .011(5) C2115 .031(6) .037(6) .043(6) -.007(5) .020(5) -.005(5) C2116 .030(5) .028(5) .031(6) .003(4) .014(4) .003(4) C2121 .026(5) .024(5) .028(5) .001(4) .010(4) .004(4) C2122 .035(6) .034(6) .037(6) .001(5) .015(5) -.011(5) C2123 .046(7) .052(8) .043(7) -.003(6) .015(6) -.013(5) C2124 .044(7) .031(6) .044(7) .003(5) .026(6) .005(5) C2125 .038(7) .037(6) .045(7) .007(5) .026(6) .005(5) C2126 .036(6) .039(6) .034(6) .007(5) .020(5) .003(5) C210 .028(6) .030(6) .045(7) -.006(4) .017(5) -.004(5) C220 .009(5) .041(6) .040(6) .002(4) .010(4) .002(5) P22 .0156(10) .0274(12) .0291(12) -.0010(10) .0132(9) .0000(11) C2211 .025(5) .027(5) .034(5) .007(4) .017(4) -.001(5) C2212 .036(5) .032(5) .043(6) -.012(5) .023(5) -.010(5) C2213 .057(7) .053(7) .051(7) -.022(7) .043(6) -.004(6) C2214 .064(8) .038(7) .052(7) .001(6) .046(6) -.003(5) C2215 .021(5) .036(6) .050(7) .003(4) .011(5) -.010(5) C2216 .023(5) .042(6) .031(6) -.007(4) .013(4) -.002(5) C2221 .017(5) .038(6) .024(5) -.004(4) .009(4) -.002(4) C2222 .034(6) .034(6) .033(6) .009(5) .016(5) .001(5) C2223 .041(7) .033(6) .045(6) .005(5) .022(5) .005(5) C2224 .048(7) .033(7) .047(7) .016(5) .012(6) -.002(5) C2225 .027(6) .049(7) .044(7) .012(5) .018(5) .005(5) C2226 .024(5) .037(6) .050(7) .010(5) .023(5) .013(5) C101 .042(7) .029(6) .032(6) -.006(5) .018(5) .002(4) C102 .034(6) .034(6) .021(5) -.000(5) .008(5) -.001(4) C103 .021(4) .045(7) .024(4) .005(5) .011(4) .004(5) C104 .040(7) .027(6) .021(5) -.008(4) .018(5) -.007(4) C105 .020(5) .062(7) .019(5) .003(5) .015(4) -.000(5) C201 .009(4) .066(8) .032(5) -.004(5) .009(4) -.007(6) C202 .015(5) .042(7) .044(6) -.001(4) .005(4) .007(5) C203 .016(5) .055(7) .036(5) -.002(5) .008(4) -.005(5) C204 .029(6) .039(6) .037(6) -.008(5) .012(5) -.004(5) C205 .016(5) .055(8) .056(8) -.012(5) .007(5) .008(6) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 P11 . . 2.228(3) ? Ru1 P12 . . 2.256(3) ? Ru1 C1 . . 2.016(7) ? Ru1 C101 . . 2.250(12) ? Ru1 C102 . . 2.230(10) ? Ru1 C103 . . 2.248(8) ? Ru1 C104 . . 2.247(10) ? Ru1 C105 . . 2.244(10) ? Ru2 C4 . . 2.007(8) ? Ru2 P21 . . 2.246(3) ? Ru2 P22 . . 2.258(3) ? Ru2 C201 . . 2.244(9) ? Ru2 C202 . . 2.223(9) ? Ru2 C203 . . 2.243(9) ? Ru2 C204 . . 2.265(10) ? Ru2 C205 . . 2.241(12) ? P11 C1111 . . 1.834(10) ? P11 C1121 . . 1.811(10) ? P11 C110 . . 1.851(12) ? C1111 C1112 . . 1.383(14) ? C1111 C1116 . . 1.410(16) ? C1112 C1113 . . 1.384(14) ? C1112 H1112 . . .973 ? C1113 C1114 . . 1.388(17) ? C1113 H1113 . . .981 ? C1114 C1115 . . 1.359(16) ? C1114 H1114 . . .970 ? C1115 C1116 . . 1.407(13) ? C1115 H1115 . . .959 ? C1116 H1116 . . .964 ? C1121 C1122 . . 1.411(17) ? C1121 C1126 . . 1.393(16) ? C1122 C1123 . . 1.371(15) ? C1122 H1122 . . .956 ? C1123 C1124 . . 1.385(17) ? C1123 H1123 . . .977 ? C1124 C1125 . . 1.398(17) ? C1124 H1124 . . .966 ? C1125 C1126 . . 1.372(15) ? C1125 H1125 . . .966 ? C1126 H1126 . . .963 ? C110 C120 . . 1.522(16) ? C110 H110a . . .959 ? C110 H110b . . .965 ? C120 P12 . . 1.845(11) ? C120 H120a . . .959 ? C120 H120b . . .955 ? P12 C1211 . . 1.831(9) ? P12 C1221 . . 1.846(10) ? C1211 C1212 . . 1.443(17) ? C1211 C1216 . . 1.362(14) ? C1212 C1213 . . 1.375(15) ? C1212 H1212 . . .965 ? C1213 C1214 . . 1.361(17) ? C1213 H1213 . . .950 ? C1214 C1215 . . 1.41(2) ? C1214 H1214 . . .963 ? C1215 C1216 . . 1.392(15) ? C1215 H1215 . . .961 ? C1216 H1216 . . .942 ? C1221 C1222 . . 1.390(16) ? C1221 C1226 . . 1.389(16) ? C1222 C1223 . . 1.388(15) ? C1222 H1222 . . .963 ? C1223 C1224 . . 1.330(18) ? C1223 H1223 . . .964 ? C1224 C1225 . . 1.39(2) ? C1224 H1224 . . .955 ? C1225 C1226 . . 1.376(17) ? C1225 H1225 . . .971 ? C1226 H1226 . . .972 ? C1 C2 . . 1.216(10) ? C2 C3 . . 1.396(10) ? C3 C4 . . 1.220(11) ? P21 C2111 . . 1.831(10) ? P21 C2121 . . 1.818(11) ? P21 C210 . . 1.863(11) ? C2111 C2112 . . 1.415(15) ? C2111 C2116 . . 1.386(14) ? C2112 C2113 . . 1.381(15) ? C2112 H2112 . . .962 ? C2113 C2114 . . 1.367(16) ? C2113 H2113 . . .961 ? C2114 C2115 . . 1.390(15) ? C2114 H2114 . . .975 ? C2115 C2116 . . 1.368(14) ? C2115 H2115 . . .958 ? C2116 H2116 . . .959 ? C2121 C2122 . . 1.371(13) ? C2121 C2126 . . 1.421(15) ? C2122 C2123 . . 1.394(18) ? C2122 H2122 . . .970 ? C2123 C2124 . . 1.375(17) ? C2123 H2123 . . .962 ? C2124 C2125 . . 1.364(15) ? C2124 H2124 . . .964 ? C2125 C2126 . . 1.395(17) ? C2125 H2125 . . .949 ? C2126 H2126 . . .997 ? C210 C220 . . 1.522(15) ? C210 H210a . . .964 ? C210 H210b . . .962 ? C220 P22 . . 1.836(10) ? C220 H220a . . .958 ? C220 H220b . . .958 ? P22 C2211 . . 1.825(10) ? P22 C2221 . . 1.803(11) ? C2211 C2212 . . 1.406(15) ? C2211 C2216 . . 1.387(13) ? C2212 C2213 . . 1.368(16) ? C2212 H2212 . . .981 ? C2213 C2214 . . 1.374(16) ? C2213 H2213 . . .962 ? C2214 C2215 . . 1.419(18) ? C2214 H2214 . . .977 ? C2215 C2216 . . 1.366(16) ? C2215 H2215 . . .978 ? C2216 H2216 . . .957 ? C2221 C2222 . . 1.381(16) ? C2221 C2226 . . 1.438(16) ? C2222 C2223 . . 1.384(15) ? C2222 H2222 . . .957 ? C2223 C2224 . . 1.407(18) ? C2223 H2223 . . .964 ? C2224 C2225 . . 1.385(18) ? C2224 H2224 . . .975 ? C2225 C2226 . . 1.364(16) ? C2225 H2225 . . .961 ? C2226 H2226 . . .953 ? C101 C102 . . 1.410(16) ? C101 C105 . . 1.428(16) ? C101 H101 . . .959 ? C102 C103 . . 1.384(15) ? C102 H102 . . .974 ? C103 C104 . . 1.412(14) ? C103 H103 . . .971 ? C104 C105 . . 1.409(15) ? C104 H104 . . .948 ? C105 H105 . . .953 ? C201 C202 . . 1.418(15) ? C201 C205 . . 1.436(18) ? C201 H201 . . .961 ? C202 C203 . . 1.364(16) ? C202 H202 . . .948 ? C203 C204 . . 1.431(16) ? C203 H203 . . .980 ? C204 C205 . . 1.384(18) ? C204 H204 . . .980 ? C205 H205 . . .978 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published P11 Ru1 P12 . . . 81.99(10) ? P11 Ru1 C1 . . . 85.0(3) ? P11 Ru1 C101 . . . 114.0(3) ? P11 Ru1 C102 . . . 99.0(3) ? P11 Ru1 C103 . . . 116.6(3) ? P11 Ru1 C104 . . . 153.1(3) ? P11 Ru1 C105 . . . 150.4(3) ? P12 Ru1 C1 . . . 81.2(3) ? P12 Ru1 C101 . . . 163.3(3) ? P12 Ru1 C102 . . . 140.7(3) ? P12 Ru1 C103 . . . 108.8(3) ? P12 Ru1 C104 . . . 102.8(3) ? P12 Ru1 C105 . . . 127.4(3) ? C1 Ru1 C101 . . . 103.8(4) ? C1 Ru1 C102 . . . 138.1(4) ? C1 Ru1 C103 . . . 156.9(4) ? C1 Ru1 C104 . . . 121.9(4) ? C1 Ru1 C105 . . . 95.8(3) ? C101 Ru1 C102 . . . 36.7(4) ? C101 Ru1 C103 . . . 61.0(4) ? C101 Ru1 C104 . . . 60.9(4) ? C101 Ru1 C105 . . . 37.1(4) ? C102 Ru1 C103 . . . 36.0(4) ? C102 Ru1 C104 . . . 60.5(4) ? C102 Ru1 C105 . . . 61.3(4) ? C103 Ru1 C104 . . . 36.6(4) ? C103 Ru1 C105 . . . 61.4(3) ? C104 Ru1 C105 . . . 36.6(4) ? C4 Ru2 P21 . . . 84.3(3) ? C4 Ru2 P22 . . . 81.5(3) ? C4 Ru2 C201 . . . 102.9(4) ? C4 Ru2 C202 . . . 137.8(4) ? C4 Ru2 C203 . . . 156.1(4) ? C4 Ru2 C204 . . . 120.9(4) ? C4 Ru2 C205 . . . 95.4(4) ? P21 Ru2 P22 . . . 82.31(10) ? P21 Ru2 C201 . . . 110.5(4) ? P21 Ru2 C202 . . . 97.5(3) ? P21 Ru2 C203 . . . 117.1(3) ? P21 Ru2 C204 . . . 154.1(3) ? P21 Ru2 C205 . . . 147.0(3) ? P22 Ru2 C201 . . . 166.7(3) ? P22 Ru2 C202 . . . 140.7(3) ? P22 Ru2 C203 . . . 110.4(3) ? P22 Ru2 C204 . . . 105.8(3) ? P22 Ru2 C205 . . . 130.4(3) ? C201 Ru2 C202 . . . 37.0(4) ? C201 Ru2 C203 . . . 61.1(4) ? C201 Ru2 C204 . . . 61.0(4) ? C201 Ru2 C205 . . . 37.4(5) ? C202 Ru2 C203 . . . 35.6(4) ? C202 Ru2 C204 . . . 60.5(4) ? C202 Ru2 C205 . . . 61.3(4) ? C203 Ru2 C204 . . . 37.0(4) ? C203 Ru2 C205 . . . 61.0(4) ? C204 Ru2 C205 . . . 35.8(5) ? Ru1 P11 C1111 . . . 114.4(4) ? Ru1 P11 C1121 . . . 120.2(4) ? Ru1 P11 C110 . . . 111.5(4) ? C1111 P11 C1121 . . . 100.5(4) ? C1111 P11 C110 . . . 105.6(5) ? C1121 P11 C110 . . . 103.0(5) ? P11 C1111 C1112 . . . 120.2(8) ? P11 C1111 C1116 . . . 120.2(7) ? C1112 C1111 C1116 . . . 119.3(9) ? C1111 C1112 C1113 . . . 120.8(10) ? C1111 C1112 H1112 . . . 119.7 ? C1113 C1112 H1112 . . . 119.5 ? C1112 C1113 C1114 . . . 119.3(9) ? C1112 C1113 H1113 . . . 121.0 ? C1114 C1113 H1113 . . . 119.7 ? C1113 C1114 C1115 . . . 121.4(9) ? C1113 C1114 H1114 . . . 118.1 ? C1115 C1114 H1114 . . . 120.5 ? C1114 C1115 C1116 . . . 119.9(11) ? C1114 C1115 H1115 . . . 121.2 ? C1116 C1115 H1115 . . . 118.9 ? C1111 C1116 C1115 . . . 119.2(10) ? C1111 C1116 H1116 . . . 119.8 ? C1115 C1116 H1116 . . . 120.9 ? P11 C1121 C1122 . . . 120.8(8) ? P11 C1121 C1126 . . . 122.2(9) ? C1122 C1121 C1126 . . . 117.0(9) ? C1121 C1122 C1123 . . . 120.6(11) ? C1121 C1122 H1122 . . . 119.4 ? C1123 C1122 H1122 . . . 119.9 ? C1122 C1123 C1124 . . . 121.5(12) ? C1122 C1123 H1123 . . . 120.2 ? C1124 C1123 H1123 . . . 118.2 ? C1123 C1124 C1125 . . . 118.5(10) ? C1123 C1124 H1124 . . . 121.5 ? C1125 C1124 H1124 . . . 120.0 ? C1124 C1125 C1126 . . . 119.8(10) ? C1124 C1125 H1125 . . . 119.8 ? C1126 C1125 H1125 . . . 120.4 ? C1121 C1126 C1125 . . . 122.4(11) ? C1121 C1126 H1126 . . . 119.1 ? C1125 C1126 H1126 . . . 118.5 ? P11 C110 C120 . . . 112.0(8) ? P11 C110 H110a . . . 109.4 ? P11 C110 H110b . . . 109.1 ? C120 C110 H110a . . . 109.5 ? C120 C110 H110b . . . 109.3 ? H110a C110 H110b . . . 107.5 ? C110 C120 P12 . . . 113.2(8) ? C110 C120 H120a . . . 109.2 ? C110 C120 H120b . . . 109.2 ? P12 C120 H120a . . . 108.3 ? P12 C120 H120b . . . 108.5 ? H120a C120 H120b . . . 108.2 ? Ru1 P12 C120 . . . 110.3(4) ? Ru1 P12 C1211 . . . 116.5(3) ? Ru1 P12 C1221 . . . 118.3(4) ? C120 P12 C1211 . . . 106.9(5) ? C120 P12 C1221 . . . 104.0(5) ? C1211 P12 C1221 . . . 99.4(4) ? P12 C1211 C1212 . . . 124.6(7) ? P12 C1211 C1216 . . . 117.8(9) ? C1212 C1211 C1216 . . . 117.6(9) ? C1211 C1212 C1213 . . . 119.0(10) ? C1211 C1212 H1212 . . . 119.0 ? C1213 C1212 H1212 . . . 122.0 ? C1212 C1213 C1214 . . . 122.6(12) ? C1212 C1213 H1213 . . . 118.7 ? C1214 C1213 H1213 . . . 118.7 ? C1213 C1214 C1215 . . . 119.3(10) ? C1213 C1214 H1214 . . . 119.9 ? C1215 C1214 H1214 . . . 120.9 ? C1214 C1215 C1216 . . . 118.5(10) ? C1214 C1215 H1215 . . . 120.9 ? C1216 C1215 H1215 . . . 120.5 ? C1211 C1216 C1215 . . . 123.0(11) ? C1211 C1216 H1216 . . . 117.2 ? C1215 C1216 H1216 . . . 119.9 ? P12 C1221 C1222 . . . 119.8(8) ? P12 C1221 C1226 . . . 121.7(9) ? C1222 C1221 C1226 . . . 118.4(9) ? C1221 C1222 C1223 . . . 119.6(11) ? C1221 C1222 H1222 . . . 120.1 ? C1223 C1222 H1222 . . . 120.4 ? C1222 C1223 C1224 . . . 121.8(12) ? C1222 C1223 H1223 . . . 118.7 ? C1224 C1223 H1223 . . . 119.5 ? C1223 C1224 C1225 . . . 119.6(11) ? C1223 C1224 H1224 . . . 119.5 ? C1225 C1224 H1224 . . . 120.8 ? C1224 C1225 C1226 . . . 120.2(12) ? C1224 C1225 H1225 . . . 120.5 ? C1226 C1225 H1225 . . . 119.3 ? C1221 C1226 C1225 . . . 120.4(11) ? C1221 C1226 H1226 . . . 118.5 ? C1225 C1226 H1226 . . . 121.1 ? Ru1 C1 C2 . . . 177.1(9) ? C1 C2 C3 . . . 175.7(10) ? C2 C3 C4 . . . 171.6(10) ? Ru2 C4 C3 . . . 171.4(9) ? Ru2 P21 C2111 . . . 116.9(3) ? Ru2 P21 C2121 . . . 116.3(4) ? Ru2 P21 C210 . . . 112.8(3) ? C2111 P21 C2121 . . . 102.0(5) ? C2111 P21 C210 . . . 100.6(5) ? C2121 P21 C210 . . . 106.4(5) ? P21 C2111 C2112 . . . 123.7(8) ? P21 C2111 C2116 . . . 119.0(8) ? C2112 C2111 C2116 . . . 117.3(9) ? C2111 C2112 C2113 . . . 120.2(10) ? C2111 C2112 H2112 . . . 118.6 ? C2113 C2112 H2112 . . . 121.2 ? C2112 C2113 C2114 . . . 121.3(10) ? C2112 C2113 H2113 . . . 119.1 ? C2114 C2113 H2113 . . . 119.6 ? C2113 C2114 C2115 . . . 118.9(10) ? C2113 C2114 H2114 . . . 122.3 ? C2115 C2114 H2114 . . . 118.8 ? C2114 C2115 C2116 . . . 120.6(10) ? C2114 C2115 H2115 . . . 120.8 ? C2116 C2115 H2115 . . . 118.5 ? C2111 C2116 C2115 . . . 121.7(10) ? C2111 C2116 H2116 . . . 118.7 ? C2115 C2116 H2116 . . . 119.6 ? P21 C2121 C2122 . . . 125.6(8) ? P21 C2121 C2126 . . . 116.5(7) ? C2122 C2121 C2126 . . . 117.8(10) ? C2121 C2122 C2123 . . . 121.5(10) ? C2121 C2122 H2122 . . . 118.0 ? C2123 C2122 H2122 . . . 120.5 ? C2122 C2123 C2124 . . . 119.6(10) ? C2122 C2123 H2123 . . . 120.6 ? C2124 C2123 H2123 . . . 119.8 ? C2123 C2124 C2125 . . . 121.1(12) ? C2123 C2124 H2124 . . . 119.9 ? C2125 C2124 H2124 . . . 118.9 ? C2124 C2125 C2126 . . . 119.5(11) ? C2124 C2125 H2125 . . . 119.8 ? C2126 C2125 H2125 . . . 120.7 ? C2121 C2126 C2125 . . . 120.5(9) ? C2121 C2126 H2126 . . . 119.1 ? C2125 C2126 H2126 . . . 120.4 ? P21 C210 C220 . . . 110.6(7) ? P21 C210 H210a . . . 110.4 ? P21 C210 H210b . . . 110.4 ? C220 C210 H210a . . . 108.9 ? C220 C210 H210b . . . 109.2 ? H210a C210 H210b . . . 107.3 ? C210 C220 P22 . . . 111.7(6) ? C210 C220 H220a . . . 109.4 ? C210 C220 H220b . . . 110.2 ? P22 C220 H220a . . . 108.7 ? P22 C220 H220b . . . 108.6 ? H220a C220 H220b . . . 108.1 ? Ru2 P22 C220 . . . 108.5(4) ? Ru2 P22 C2211 . . . 118.0(3) ? Ru2 P22 C2221 . . . 120.6(4) ? C220 P22 C2211 . . . 105.0(5) ? C220 P22 C2221 . . . 102.7(4) ? C2211 P22 C2221 . . . 100.0(5) ? P22 C2211 C2212 . . . 124.2(7) ? P22 C2211 C2216 . . . 118.6(8) ? C2212 C2211 C2216 . . . 117.2(9) ? C2211 C2212 C2213 . . . 121.5(9) ? C2211 C2212 H2212 . . . 118.4 ? C2213 C2212 H2212 . . . 120.2 ? C2212 C2213 C2214 . . . 120.0(12) ? C2212 C2213 H2213 . . . 121.5 ? C2214 C2213 H2213 . . . 118.5 ? C2213 C2214 C2215 . . . 120.4(12) ? C2213 C2214 H2214 . . . 121.7 ? C2215 C2214 H2214 . . . 117.9 ? C2214 C2215 C2216 . . . 118.0(9) ? C2214 C2215 H2215 . . . 121.6 ? C2216 C2215 H2215 . . . 120.4 ? C2211 C2216 C2215 . . . 122.9(10) ? C2211 C2216 H2216 . . . 117.6 ? C2215 C2216 H2216 . . . 119.5 ? P22 C2221 C2222 . . . 122.1(9) ? P22 C2221 C2226 . . . 121.0(8) ? C2222 C2221 C2226 . . . 116.9(10) ? C2221 C2222 C2223 . . . 121.9(11) ? C2221 C2222 H2222 . . . 120.5 ? C2223 C2222 H2222 . . . 117.6 ? C2222 C2223 C2224 . . . 120.1(11) ? C2222 C2223 H2223 . . . 119.8 ? C2224 C2223 H2223 . . . 120.1 ? C2223 C2224 C2225 . . . 119.1(10) ? C2223 C2224 H2224 . . . 119.0 ? C2225 C2224 H2224 . . . 121.9 ? C2224 C2225 C2226 . . . 120.7(12) ? C2224 C2225 H2225 . . . 120.1 ? C2226 C2225 H2225 . . . 119.2 ? C2221 C2226 C2225 . . . 121.4(11) ? C2221 C2226 H2226 . . . 120.1 ? C2225 C2226 H2226 . . . 118.5 ? Ru1 C101 C102 . . . 70.9(7) ? Ru1 C101 C105 . . . 71.3(6) ? Ru1 C101 H101 . . . 122.6 ? C102 C101 C105 . . . 107.1(9) ? C102 C101 H101 . . . 126.4 ? C105 C101 H101 . . . 126.5 ? Ru1 C102 C101 . . . 72.4(6) ? Ru1 C102 C103 . . . 72.7(5) ? Ru1 C102 H102 . . . 122.6 ? C101 C102 C103 . . . 109.6(9) ? C101 C102 H102 . . . 123.9 ? C103 C102 H102 . . . 126.5 ? Ru1 C103 C102 . . . 71.3(5) ? Ru1 C103 C104 . . . 71.7(5) ? Ru1 C103 H103 . . . 120.8 ? C102 C103 C104 . . . 107.5(8) ? C102 C103 H103 . . . 126.2 ? C104 C103 H103 . . . 126.3 ? Ru1 C104 C103 . . . 71.7(5) ? Ru1 C104 C105 . . . 71.6(6) ? Ru1 C104 H104 . . . 125.1 ? C103 C104 C105 . . . 108.8(9) ? C103 C104 H104 . . . 126.0 ? C105 C104 H104 . . . 125.1 ? Ru1 C105 C101 . . . 71.7(7) ? Ru1 C105 C104 . . . 71.9(6) ? Ru1 C105 H105 . . . 121.4 ? C101 C105 C104 . . . 107.0(9) ? C101 C105 H105 . . . 127.1 ? C104 C105 H105 . . . 125.8 ? Ru2 C201 C202 . . . 70.7(5) ? Ru2 C201 C205 . . . 71.2(6) ? Ru2 C201 H201 . . . 122.1 ? C202 C201 C205 . . . 105.7(10) ? C202 C201 H201 . . . 127.8 ? C205 C201 H201 . . . 126.6 ? Ru2 C202 C201 . . . 72.3(5) ? Ru2 C202 C203 . . . 73.0(5) ? Ru2 C202 H202 . . . 122.2 ? C201 C202 C203 . . . 110.1(10) ? C201 C202 H202 . . . 125.9 ? C203 C202 H202 . . . 124.0 ? Ru2 C203 C202 . . . 71.4(5) ? Ru2 C203 C204 . . . 72.3(5) ? Ru2 C203 H203 . . . 121.9 ? C202 C203 C204 . . . 107.9(10) ? C202 C203 H203 . . . 125.3 ? C204 C203 H203 . . . 126.8 ? Ru2 C204 C203 . . . 70.7(6) ? Ru2 C204 C205 . . . 71.2(6) ? Ru2 C204 H204 . . . 125.7 ? C203 C204 C205 . . . 107.9(10) ? C203 C204 H204 . . . 126.5 ? C205 C204 H204 . . . 125.6 ? Ru2 C205 C201 . . . 71.4(6) ? Ru2 C205 C204 . . . 73.0(7) ? Ru2 C205 H205 . . . 120.9 ? C201 C205 C204 . . . 108.5(10) ? C201 C205 H205 . . . 125.3 ? C204 C205 H205 . . . 126.2 ? _exptl_crystal_F_000 1204 _refine_special_details ; The absolute structure parameter refined to a value not significantly different from 0.5. Refinement was completed on data in which the Friedel equivalents were averaged. ; _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min -18 _reflns_limit_l_max 17 _reflns_number_observed ? _reflns_d_resolution_high .842 _reflns_d_resolution_low 14.657 _diffrn_reflns_av_sigmaI/netI .056 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .057 _refine_ls_wR_factor_all .057 _refine_ls_goodness_of_fit_all 1.145 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END data_ben5rev _database_code_depnum_ccdc_archive 'CCDC 224446' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H56 Fe P2 Si' _chemical_formula_weight 802.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4576(6) _cell_length_b 14.5424(6) _cell_length_c 15.4074(6) _cell_angle_alpha 70.850(2) _cell_angle_beta 76.356(2) _cell_angle_gamma 78.567(2) _cell_volume 2132.29(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9770 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9770 _reflns_number_gt 7484 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+4.0889P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9770 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1678 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 1.724 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C44 C 0.5042(9) 0.2995(7) 0.1132(9) 0.078(3) Uani 0.70 1 d P A 1 C45 C 0.510(2) 0.3194(17) 0.0370(14) 0.151(9) Uani 0.70 1 d P A 1 H45 H 0.4543 0.3741 0.0090 0.181 Uiso 0.70 1 calc PR A 1 C47 C 0.6751(16) 0.1734(10) 0.0251(8) 0.066(3) Uani 0.70 1 d P A 1 H47 H 0.7350 0.1344 -0.0075 0.080 Uiso 0.70 1 calc PR A 1 C46 C 0.6014(14) 0.2634(10) -0.0232(9) 0.119(4) Uani 0.70 1 d P A 1 H46 H 0.6108 0.2848 -0.0880 0.143 Uiso 0.70 1 calc PR A 1 C48 C 0.6554(11) 0.1503(8) 0.1113(10) 0.091(3) Uani 0.70 1 d P A 1 H48 H 0.6978 0.0911 0.1444 0.109 Uiso 0.70 1 calc PR A 1 C49 C 0.5758(14) 0.2078(8) 0.1567(13) 0.103(6) Uani 0.70 1 d P A 1 H49 H 0.5652 0.1877 0.2216 0.123 Uiso 0.70 1 calc PR A 1 C50 C 0.4136(7) 0.3679(8) 0.1576(7) 0.070(2) Uani 0.70 1 d P A 1 H50A H 0.4100 0.3438 0.2240 0.106 Uiso 0.70 1 calc PR A 1 H50B H 0.3266 0.3740 0.1443 0.106 Uiso 0.70 1 calc PR A 1 H50C H 0.4446 0.4310 0.1338 0.106 Uiso 0.70 1 calc PR A 1 C51 C 0.5914(12) 0.2359(10) 0.0859(10) 0.032(2) Uani 0.30 1 d P B 2 C52 C 0.5665(18) 0.2458(12) 0.1686(9) 0.036(4) Uani 0.30 1 d P B 2 H52 H 0.6047 0.1976 0.2154 0.044 Uiso 0.30 1 calc PR B 2 C53 C 0.4774(18) 0.3329(12) 0.1918(9) 0.050(4) Uani 0.30 1 d P B 2 H53 H 0.4497 0.3378 0.2523 0.060 Uiso 0.30 1 calc PR B 2 C54 C 0.4397 0.4080 0.1104 0.32(4) Uani 0.30 1 d P B 2 H54 H 0.4111 0.4713 0.1148 0.389 Uiso 0.30 1 calc PR B 2 C55 C 0.4428(19) 0.3940(14) 0.0376(14) 0.074(6) Uani 0.30 1 d P B 2 H55 H 0.3879 0.4344 -0.0032 0.089 Uiso 0.30 1 calc PR B 2 C56 C 0.5292(15) 0.3168(8) 0.0151(8) 0.021(3) Uani 0.30 1 d P B 2 H56 H 0.5490 0.3156 -0.0466 0.025 Uiso 0.30 1 calc PR B 2 C57 C 0.683(3) 0.155(2) 0.0557(11) 0.042(5) Uani 0.30 1 d P B 2 H57A H 0.6712 0.1567 -0.0049 0.063 Uiso 0.30 1 calc PR B 2 H57B H 0.6632 0.0928 0.0999 0.063 Uiso 0.30 1 calc PR B 2 H57C H 0.7730 0.1625 0.0527 0.063 Uiso 0.30 1 calc PR B 2 Fe1 Fe 0.17332(4) 0.21871(3) 0.66553(3) 0.02037(13) Uani 1 1 d . . . P1 P 0.32745(8) 0.16028(5) 0.56753(5) 0.02080(17) Uani 1 1 d . . . P2 P 0.32691(8) 0.18165(5) 0.75083(5) 0.02193(18) Uani 1 1 d . . . Si1 Si 0.01700(10) -0.30034(6) 0.85050(7) 0.0308(2) Uani 1 1 d . . . C1 C -0.0325(3) 0.2605(2) 0.7051(2) 0.0271(6) Uani 1 1 d . . . C2 C 0.0002(3) 0.2682(2) 0.6075(2) 0.0245(6) Uani 1 1 d . . . C3 C 0.0903(3) 0.3401(2) 0.5639(2) 0.0258(6) Uani 1 1 d . . . C4 C 0.1155(3) 0.3742(2) 0.6342(2) 0.0248(6) Uani 1 1 d . . . C5 C 0.0388(3) 0.3245(2) 0.7220(2) 0.0257(6) Uani 1 1 d . . . C6 C -0.1329(3) 0.2015(3) 0.7767(3) 0.0363(8) Uani 1 1 d . . . H6A H -0.1674 0.1641 0.7486 0.044 Uiso 1 1 calc R . . H6B H -0.2040 0.2449 0.8004 0.044 Uiso 1 1 calc R . . H6C H -0.0914 0.1577 0.8272 0.044 Uiso 1 1 calc R . . C7 C -0.0575(4) 0.2171(3) 0.5591(3) 0.0362(8) Uani 1 1 d . . . H7A H -0.0193 0.2352 0.4938 0.043 Uiso 1 1 calc R . . H7B H -0.1519 0.2358 0.5669 0.043 Uiso 1 1 calc R . . H7C H -0.0384 0.1473 0.5856 0.043 Uiso 1 1 calc R . . C8 C 0.1335(4) 0.3824(2) 0.4598(2) 0.0330(7) Uani 1 1 d . . . H8A H 0.1036 0.3463 0.4279 0.040 Uiso 1 1 calc R . . H8B H 0.2285 0.3777 0.4447 0.040 Uiso 1 1 calc R . . H8C H 0.0957 0.4500 0.4405 0.040 Uiso 1 1 calc R . . C9 C 0.1870(3) 0.4597(2) 0.6184(2) 0.0304(7) Uani 1 1 d . . . H9A H 0.1906 0.4667 0.6775 0.037 Uiso 1 1 calc R . . H9B H 0.1406 0.5185 0.5827 0.037 Uiso 1 1 calc R . . H9C H 0.2756 0.4486 0.5847 0.037 Uiso 1 1 calc R . . C10 C 0.0174(4) 0.3495(3) 0.8118(2) 0.0365(8) Uani 1 1 d . . . H10A H 0.0775 0.3942 0.8058 0.044 Uiso 1 1 calc R . . H10B H 0.0334 0.2907 0.8615 0.044 Uiso 1 1 calc R . . H10C H -0.0724 0.3797 0.8254 0.044 Uiso 1 1 calc R . . C11 C 0.4294(3) 0.0559(2) 0.6366(2) 0.0242(6) Uani 1 1 d . . . H11A H 0.3835 -0.0017 0.6598 0.029 Uiso 1 1 calc R . . H11B H 0.5131 0.0408 0.5974 0.029 Uiso 1 1 calc R . . C12 C 0.4551(3) 0.0825(2) 0.7187(2) 0.0296(7) Uani 1 1 d . . . H12A H 0.5420 0.1041 0.7023 0.035 Uiso 1 1 calc R . . H12B H 0.4556 0.0244 0.7724 0.035 Uiso 1 1 calc R . . C13 C 0.2789(3) 0.1093(2) 0.4873(2) 0.0246(6) Uani 1 1 d . . . C14 C 0.2196(3) 0.0234(2) 0.5233(2) 0.0289(7) Uani 1 1 d . . . H14 H 0.2095 -0.0094 0.5870 0.035 Uiso 1 1 calc R . . C15 C 0.1753(4) -0.0138(3) 0.4643(3) 0.0349(8) Uani 1 1 d . . . H15 H 0.1360 -0.0712 0.4889 0.042 Uiso 1 1 calc R . . C16 C 0.1897(4) 0.0345(3) 0.3696(3) 0.0388(8) Uani 1 1 d . . . H16 H 0.1589 0.0101 0.3306 0.047 Uiso 1 1 calc R . . C17 C 0.2497(4) 0.1189(3) 0.3331(3) 0.0383(8) Uani 1 1 d . . . H17 H 0.2611 0.1507 0.2692 0.046 Uiso 1 1 calc R . . C18 C 0.2933(4) 0.1568(2) 0.3915(2) 0.0323(7) Uani 1 1 d . . . H18 H 0.3325 0.2142 0.3664 0.039 Uiso 1 1 calc R . . C19 C 0.4563(3) 0.2334(2) 0.4898(2) 0.0229(6) Uani 1 1 d . . . C20 C 0.4559(3) 0.3289(2) 0.4908(2) 0.0252(6) Uani 1 1 d . . . H20 H 0.3875 0.3562 0.5294 0.030 Uiso 1 1 calc R . . C21 C 0.5555(3) 0.3839(2) 0.4352(2) 0.0318(7) Uani 1 1 d . . . H21 H 0.5534 0.4476 0.4365 0.038 Uiso 1 1 calc R . . C22 C 0.6576(4) 0.3442(3) 0.3780(3) 0.0374(8) Uani 1 1 d . . . H22 H 0.7232 0.3818 0.3396 0.045 Uiso 1 1 calc R . . C23 C 0.6629(4) 0.2480(3) 0.3774(3) 0.0396(8) Uani 1 1 d . . . H23 H 0.7335 0.2203 0.3405 0.048 Uiso 1 1 calc R . . C24 C 0.5622(3) 0.1940(2) 0.4322(2) 0.0316(7) Uani 1 1 d . . . H24 H 0.5648 0.1302 0.4307 0.038 Uiso 1 1 calc R . . C25 C 0.2843(3) 0.1304(2) 0.8789(2) 0.0268(6) Uani 1 1 d . . . C26 C 0.3800(4) 0.1151(3) 0.9335(2) 0.0327(7) Uani 1 1 d . . . H26 H 0.4649 0.1313 0.9054 0.039 Uiso 1 1 calc R . . C27 C 0.3484(4) 0.0754(3) 1.0303(2) 0.0356(8) Uani 1 1 d . . . H27 H 0.4121 0.0657 1.0667 0.043 Uiso 1 1 calc R . . C28 C 0.2224(4) 0.0504(3) 1.0725(2) 0.0342(7) Uani 1 1 d . . . H28 H 0.2017 0.0239 1.1371 0.041 Uiso 1 1 calc R . . C29 C 0.1277(4) 0.0650(3) 1.0185(2) 0.0333(7) Uani 1 1 d . . . H29 H 0.0430 0.0486 1.0467 0.040 Uiso 1 1 calc R . . C30 C 0.1590(3) 0.1042(2) 0.9219(2) 0.0277(6) Uani 1 1 d . . . H30 H 0.0953 0.1129 0.8857 0.033 Uiso 1 1 calc R . . C31 C 0.4270(3) 0.2761(2) 0.7439(2) 0.0261(6) Uani 1 1 d . . . C32 C 0.3802(4) 0.3379(2) 0.8007(3) 0.0340(7) Uani 1 1 d . . . H32 H 0.3020 0.3284 0.8444 0.041 Uiso 1 1 calc R . . C33 C 0.4492(4) 0.4135(3) 0.7925(3) 0.0459(10) Uani 1 1 d . . . H33 H 0.4158 0.4547 0.8301 0.055 Uiso 1 1 calc R . . C34 C 0.5662(4) 0.4282(3) 0.7298(3) 0.0463(10) Uani 1 1 d . . . H34 H 0.6125 0.4784 0.7255 0.056 Uiso 1 1 calc R . . C35 C 0.6143(4) 0.3679(3) 0.6731(3) 0.0421(9) Uani 1 1 d . . . H35 H 0.6933 0.3775 0.6303 0.051 Uiso 1 1 calc R . . C36 C 0.5451(3) 0.2927(3) 0.6800(2) 0.0322(7) Uani 1 1 d . . . H36 H 0.5781 0.2528 0.6412 0.039 Uiso 1 1 calc R . . C37 C 0.1374(3) 0.0886(2) 0.7187(2) 0.0227(6) Uani 1 1 d . . . C38 C 0.1081(3) 0.0048(2) 0.7501(2) 0.0252(6) Uani 1 1 d . . . C39 C 0.0798(3) -0.0901(2) 0.7786(2) 0.0265(6) Uani 1 1 d . . . C40 C 0.0546(3) -0.1743(2) 0.8035(2) 0.0299(7) Uani 1 1 d . . . C41 C -0.0193(4) -0.3404(3) 0.7566(3) 0.0422(9) Uani 1 1 d . . . H41A H -0.0390 -0.4068 0.7818 0.051 Uiso 1 1 calc R . . H41B H 0.0567 -0.3367 0.7070 0.051 Uiso 1 1 calc R . . H41C H -0.0941 -0.2982 0.7327 0.051 Uiso 1 1 calc R . . C42 C -0.1306(5) -0.3079(3) 0.9463(3) 0.0467(10) Uani 1 1 d . . . H42A H -0.1503 -0.3744 0.9710 0.056 Uiso 1 1 calc R . . H42B H -0.2053 -0.2657 0.9223 0.056 Uiso 1 1 calc R . . H42C H -0.1124 -0.2876 0.9950 0.056 Uiso 1 1 calc R . . C43 C 0.1625(5) -0.3816(3) 0.8958(4) 0.0591(12) Uani 1 1 d . . . H43A H 0.1432 -0.4481 0.9207 0.071 Uiso 1 1 calc R . . H43B H 0.1815 -0.3612 0.9442 0.071 Uiso 1 1 calc R . . H43C H 0.2381 -0.3774 0.8458 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C44 0.056(5) 0.065(5) 0.126(8) -0.034(6) -0.021(6) -0.022(4) C45 0.142(15) 0.182(19) 0.139(16) -0.097(14) 0.024(12) -0.019(13) C47 0.081(6) 0.057(7) 0.049(8) -0.012(6) 0.003(7) -0.004(5) C46 0.127(10) 0.118(10) 0.102(8) -0.015(8) -0.028(8) -0.013(8) C48 0.074(7) 0.068(6) 0.133(10) -0.004(7) -0.040(7) -0.034(5) C49 0.076(7) 0.044(6) 0.165(15) -0.002(8) -0.033(8) 0.007(6) C50 0.036(4) 0.104(7) 0.087(6) -0.049(6) -0.007(4) -0.015(4) C51 0.034(6) 0.028(6) 0.041(7) -0.014(5) -0.020(6) 0.001(5) C52 0.042(8) 0.041(9) 0.009(5) 0.005(5) 0.001(4) 0.009(7) C53 0.068(11) 0.065(10) 0.025(6) -0.018(6) 0.019(7) -0.056(9) C54 0.75(11) 0.29(4) 0.026(9) 0.029(16) -0.04(2) -0.47(7) C55 0.075(12) 0.078(12) 0.083(12) -0.056(11) -0.041(10) 0.048(10) C56 0.039(7) 0.014(5) 0.007(4) -0.002(4) -0.018(5) 0.016(4) C57 0.065(12) 0.048(12) 0.000(7) 0.008(8) 0.012(8) -0.025(9) Fe1 0.0218(2) 0.0164(2) 0.0243(2) -0.00856(16) -0.00319(16) -0.00285(15) P1 0.0242(4) 0.0163(3) 0.0233(4) -0.0081(3) -0.0026(3) -0.0041(3) P2 0.0232(4) 0.0194(4) 0.0242(4) -0.0083(3) -0.0039(3) -0.0024(3) Si1 0.0371(5) 0.0185(4) 0.0353(5) -0.0065(3) -0.0039(4) -0.0066(3) C1 0.0223(15) 0.0258(15) 0.0327(16) -0.0106(12) -0.0055(12) 0.0019(12) C2 0.0216(14) 0.0204(14) 0.0340(16) -0.0108(12) -0.0074(12) -0.0007(11) C3 0.0263(15) 0.0195(14) 0.0329(16) -0.0097(12) -0.0092(13) 0.0014(11) C4 0.0253(15) 0.0174(13) 0.0336(16) -0.0101(12) -0.0077(12) 0.0004(11) C5 0.0248(15) 0.0221(14) 0.0305(16) -0.0115(12) -0.0060(12) 0.0042(11) C6 0.0263(17) 0.0352(18) 0.044(2) -0.0090(15) -0.0024(14) -0.0046(14) C7 0.0341(19) 0.0366(18) 0.046(2) -0.0182(16) -0.0121(15) -0.0068(15) C8 0.0359(18) 0.0295(17) 0.0317(17) -0.0066(13) -0.0109(14) 0.0012(14) C9 0.0322(17) 0.0188(14) 0.0444(19) -0.0145(13) -0.0105(14) 0.0001(12) C10 0.0386(19) 0.0347(18) 0.0370(18) -0.0205(15) -0.0030(15) 0.0050(15) C11 0.0248(15) 0.0189(13) 0.0282(15) -0.0090(11) -0.0026(12) -0.0006(11) C12 0.0322(17) 0.0245(15) 0.0336(17) -0.0137(13) -0.0089(13) 0.0045(12) C13 0.0267(15) 0.0211(14) 0.0294(15) -0.0136(12) -0.0043(12) -0.0013(11) C14 0.0332(17) 0.0280(16) 0.0300(16) -0.0149(13) 0.0000(13) -0.0101(13) C15 0.0385(19) 0.0333(17) 0.0424(19) -0.0225(15) -0.0039(15) -0.0112(14) C16 0.044(2) 0.041(2) 0.045(2) -0.0251(17) -0.0187(17) -0.0036(16) C17 0.055(2) 0.0340(18) 0.0306(17) -0.0126(14) -0.0158(16) -0.0017(16) C18 0.044(2) 0.0246(15) 0.0302(17) -0.0091(13) -0.0091(14) -0.0046(14) C19 0.0244(15) 0.0190(13) 0.0252(14) -0.0082(11) -0.0032(11) -0.0018(11) C20 0.0271(16) 0.0222(14) 0.0276(15) -0.0100(12) -0.0038(12) -0.0030(12) C21 0.0367(18) 0.0225(15) 0.0371(18) -0.0102(13) -0.0018(14) -0.0091(13) C22 0.0376(19) 0.0317(18) 0.0414(19) -0.0113(15) 0.0052(15) -0.0149(15) C23 0.038(2) 0.0335(18) 0.045(2) -0.0189(16) 0.0102(16) -0.0091(15) C24 0.0355(18) 0.0256(15) 0.0342(17) -0.0140(13) 0.0039(14) -0.0084(13) C25 0.0300(16) 0.0225(14) 0.0282(15) -0.0097(12) -0.0046(12) -0.0012(12) C26 0.0310(17) 0.0348(17) 0.0317(17) -0.0097(14) -0.0070(14) -0.0017(14) C27 0.041(2) 0.0344(18) 0.0312(17) -0.0083(14) -0.0129(15) 0.0013(15) C28 0.046(2) 0.0314(17) 0.0231(15) -0.0091(13) -0.0028(14) -0.0029(15) C29 0.0370(19) 0.0346(17) 0.0300(17) -0.0143(14) 0.0000(14) -0.0078(14) C30 0.0318(17) 0.0269(15) 0.0271(15) -0.0121(12) -0.0039(13) -0.0046(13) C31 0.0250(15) 0.0236(14) 0.0323(16) -0.0086(12) -0.0104(12) -0.0021(12) C32 0.0331(18) 0.0313(17) 0.0433(19) -0.0186(15) -0.0091(15) -0.0020(14) C33 0.055(2) 0.0321(19) 0.064(3) -0.0250(18) -0.022(2) -0.0032(17) C34 0.050(2) 0.0318(19) 0.065(3) -0.0094(18) -0.025(2) -0.0137(17) C35 0.038(2) 0.040(2) 0.047(2) -0.0018(16) -0.0139(17) -0.0140(16) C36 0.0313(17) 0.0333(17) 0.0340(17) -0.0090(14) -0.0101(14) -0.0056(13) C37 0.0233(15) 0.0236(14) 0.0219(14) -0.0098(11) -0.0009(11) -0.0035(11) C38 0.0285(16) 0.0237(15) 0.0232(14) -0.0092(12) -0.0003(12) -0.0048(12) C39 0.0304(16) 0.0257(15) 0.0242(15) -0.0110(12) -0.0012(12) -0.0040(12) C40 0.0371(18) 0.0235(15) 0.0295(16) -0.0098(12) -0.0019(13) -0.0067(13) C41 0.046(2) 0.0349(19) 0.054(2) -0.0261(17) -0.0057(18) -0.0065(16) C42 0.062(3) 0.0329(19) 0.041(2) -0.0111(16) 0.0085(18) -0.0188(18) C43 0.062(3) 0.038(2) 0.071(3) 0.000(2) -0.027(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C44 C45 1.103(19) . ? C44 C49 1.429(15) . ? C44 C50 1.457(13) . ? C45 C46 1.49(2) . ? C45 H45 0.9300 . ? C47 C48 1.234(14) . ? C47 C46 1.446(18) . ? C47 H47 0.9300 . ? C46 H46 0.9300 . ? C48 C49 1.311(18) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.29(2) . ? C51 C56 1.479(16) . ? C51 C57 1.49(3) . ? C52 C53 1.51(2) . ? C52 H52 0.9300 . ? C53 C54 1.444(18) . ? C53 H53 0.9300 . ? C54 C55 1.197(17) . ? C54 H54 0.9300 . ? C55 C56 1.378(19) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? Fe1 C37 1.875(3) . ? Fe1 C2 2.102(3) . ? Fe1 C1 2.117(3) . ? Fe1 C3 2.131(3) . ? Fe1 C5 2.132(3) . ? Fe1 C4 2.142(3) . ? Fe1 P1 2.1795(9) . ? Fe1 P2 2.1876(9) . ? P1 C19 1.831(3) . ? P1 C13 1.840(3) . ? P1 C11 1.845(3) . ? P2 C25 1.844(3) . ? P2 C31 1.848(3) . ? P2 C12 1.874(3) . ? Si1 C40 1.821(3) . ? Si1 C43 1.856(4) . ? Si1 C42 1.860(4) . ? Si1 C41 1.863(4) . ? C1 C5 1.421(4) . ? C1 C2 1.432(4) . ? C1 C6 1.498(5) . ? C2 C3 1.436(4) . ? C2 C7 1.492(4) . ? C3 C4 1.423(4) . ? C3 C8 1.509(5) . ? C4 C5 1.439(4) . ? C4 C9 1.500(4) . ? C5 C10 1.499(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.531(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.394(4) . ? C13 C14 1.395(4) . ? C14 C15 1.397(4) . ? C14 H14 0.9300 . ? C15 C16 1.382(5) . ? C15 H15 0.9300 . ? C16 C17 1.380(5) . ? C16 H16 0.9300 . ? C17 C18 1.392(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.392(4) . ? C19 C24 1.401(4) . ? C20 C21 1.385(5) . ? C20 H20 0.9300 . ? C21 C22 1.376(5) . ? C21 H21 0.9300 . ? C22 C23 1.393(5) . ? C22 H22 0.9300 . ? C23 C24 1.382(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.387(5) . ? C25 C26 1.395(5) . ? C26 C27 1.394(5) . ? C26 H26 0.9300 . ? C27 C28 1.386(5) . ? C27 H27 0.9300 . ? C28 C29 1.381(5) . ? C28 H28 0.9300 . ? C29 C30 1.391(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.393(5) . ? C31 C32 1.398(5) . ? C32 C33 1.387(5) . ? C32 H32 0.9300 . ? C33 C34 1.374(6) . ? C33 H33 0.9300 . ? C34 C35 1.380(6) . ? C34 H34 0.9300 . ? C35 C36 1.390(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.226(4) . ? C38 C39 1.375(4) . ? C39 C40 1.220(4) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C45 C44 C49 117.3(17) . . ? C45 C44 C50 114.2(15) . . ? C49 C44 C50 128.2(13) . . ? C44 C45 C46 123(2) . . ? C44 C45 H45 118.3 . . ? C46 C45 H45 118.3 . . ? C48 C47 C46 117.5(14) . . ? C48 C47 H47 121.2 . . ? C46 C47 H47 121.2 . . ? C47 C46 C45 115.9(14) . . ? C47 C46 H46 122.0 . . ? C45 C46 H46 122.1 . . ? C47 C48 C49 121.0(14) . . ? C47 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C48 C49 C44 124.3(16) . . ? C48 C49 H49 117.9 . . ? C44 C49 H49 117.9 . . ? C44 C50 H50A 109.5 . . ? C44 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C44 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C56 115.4(12) . . ? C52 C51 C57 125.7(14) . . ? C56 C51 C57 118.7(13) . . ? C51 C52 C53 122.1(13) . . ? C51 C52 H52 118.9 . . ? C53 C52 H52 118.9 . . ? C54 C53 C52 113.0(10) . . ? C54 C53 H53 123.5 . . ? C52 C53 H53 123.5 . . ? C55 C54 C53 124.2(10) . . ? C55 C54 H54 117.9 . . ? C53 C54 H54 117.9 . . ? C54 C55 C56 118.9(13) . . ? C54 C55 H55 120.6 . . ? C56 C55 H55 120.6 . . ? C55 C56 C51 122.2(13) . . ? C55 C56 H56 118.9 . . ? C51 C56 H56 118.9 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C37 Fe1 C2 94.53(12) . . ? C37 Fe1 C1 86.58(13) . . ? C2 Fe1 C1 39.68(12) . . ? C37 Fe1 C3 132.26(12) . . ? C2 Fe1 C3 39.66(12) . . ? C1 Fe1 C3 65.92(12) . . ? C37 Fe1 C5 115.70(13) . . ? C2 Fe1 C5 66.27(12) . . ? C1 Fe1 C5 39.07(12) . . ? C3 Fe1 C5 65.63(12) . . ? C37 Fe1 C4 152.28(13) . . ? C2 Fe1 C4 66.25(11) . . ? C1 Fe1 C4 65.83(12) . . ? C3 Fe1 C4 38.89(11) . . ? C5 Fe1 C4 39.35(12) . . ? C37 Fe1 P1 84.69(9) . . ? C2 Fe1 P1 108.42(9) . . ? C1 Fe1 P1 145.93(9) . . ? C3 Fe1 P1 96.80(9) . . ? C5 Fe1 P1 158.80(9) . . ? C4 Fe1 P1 119.45(9) . . ? C37 Fe1 P2 87.71(9) . . ? C2 Fe1 P2 166.92(9) . . ? C1 Fe1 P2 127.89(9) . . ? C3 Fe1 P2 140.03(9) . . ? C5 Fe1 P2 101.16(9) . . ? C4 Fe1 P2 106.75(8) . . ? P1 Fe1 P2 84.61(3) . . ? C19 P1 C13 101.79(14) . . ? C19 P1 C11 100.70(14) . . ? C13 P1 C11 103.93(13) . . ? C19 P1 Fe1 121.08(10) . . ? C13 P1 Fe1 119.09(10) . . ? C11 P1 Fe1 107.62(10) . . ? C25 P2 C31 99.52(14) . . ? C25 P2 C12 101.81(14) . . ? C31 P2 C12 103.16(15) . . ? C25 P2 Fe1 120.20(11) . . ? C31 P2 Fe1 120.00(10) . . ? C12 P2 Fe1 109.52(11) . . ? C40 Si1 C43 109.11(19) . . ? C40 Si1 C42 109.55(16) . . ? C43 Si1 C42 110.0(2) . . ? C40 Si1 C41 109.81(17) . . ? C43 Si1 C41 109.2(2) . . ? C42 Si1 C41 109.08(19) . . ? C5 C1 C2 108.4(3) . . ? C5 C1 C6 125.0(3) . . ? C2 C1 C6 126.4(3) . . ? C5 C1 Fe1 71.06(17) . . ? C2 C1 Fe1 69.60(17) . . ? C6 C1 Fe1 128.8(2) . . ? C1 C2 C3 107.4(3) . . ? C1 C2 C7 126.1(3) . . ? C3 C2 C7 126.4(3) . . ? C1 C2 Fe1 70.71(17) . . ? C3 C2 Fe1 71.27(17) . . ? C7 C2 Fe1 127.1(2) . . ? C4 C3 C2 108.5(3) . . ? C4 C3 C8 126.1(3) . . ? C2 C3 C8 124.9(3) . . ? C4 C3 Fe1 70.97(17) . . ? C2 C3 Fe1 69.07(17) . . ? C8 C3 Fe1 132.5(2) . . ? C3 C4 C5 107.7(3) . . ? C3 C4 C9 126.4(3) . . ? C5 C4 C9 125.0(3) . . ? C3 C4 Fe1 70.14(16) . . ? C5 C4 Fe1 69.96(16) . . ? C9 C4 Fe1 134.1(2) . . ? C1 C5 C4 108.0(3) . . ? C1 C5 C10 125.2(3) . . ? C4 C5 C10 125.8(3) . . ? C1 C5 Fe1 69.87(17) . . ? C4 C5 Fe1 70.69(17) . . ? C10 C5 Fe1 133.6(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 P1 109.4(2) . . ? C12 C11 H11A 109.8 . . ? P1 C11 H11A 109.8 . . ? C12 C11 H11B 109.8 . . ? P1 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? C11 C12 P2 112.4(2) . . ? C11 C12 H12A 109.1 . . ? P2 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? P2 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? C18 C13 C14 118.6(3) . . ? C18 C13 P1 121.9(2) . . ? C14 C13 P1 119.3(2) . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.8(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.6(3) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C20 C19 C24 117.9(3) . . ? C20 C19 P1 120.4(2) . . ? C24 C19 P1 121.7(2) . . ? C21 C20 C19 121.1(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.4(3) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C19 121.3(3) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? C30 C25 C26 119.3(3) . . ? C30 C25 P2 120.9(2) . . ? C26 C25 P2 119.8(3) . . ? C27 C26 C25 119.9(3) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C29 C28 C27 119.9(3) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.1(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C25 C30 C29 120.6(3) . . ? C25 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C36 C31 C32 117.7(3) . . ? C36 C31 P2 122.7(2) . . ? C32 C31 P2 119.5(3) . . ? C33 C32 C31 120.6(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 120.9(4) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C35 C34 C33 119.4(3) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 120.1(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 121.2(3) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? C38 C37 Fe1 176.0(3) . . ? C37 C38 C39 175.6(3) . . ? C40 C39 C38 179.7(4) . . ? C39 C40 Si1 175.2(3) . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C49 C44 C45 C46 -9(3) . . . . ? C50 C44 C45 C46 176.4(14) . . . . ? C48 C47 C46 C45 1(2) . . . . ? C44 C45 C46 C47 6(3) . . . . ? C46 C47 C48 C49 -3(2) . . . . ? C47 C48 C49 C44 1(2) . . . . ? C45 C44 C49 C48 6(2) . . . . ? C50 C44 C49 C48 179.7(10) . . . . ? C56 C51 C52 C53 1(2) . . . . ? C57 C51 C52 C53 177.1(18) . . . . ? C51 C52 C53 C54 -8(2) . . . . ? C52 C53 C54 C55 21.1(19) . . . . ? C53 C54 C55 C56 -25(3) . . . . ? C54 C55 C56 C51 17(3) . . . . ? C52 C51 C56 C55 -4(2) . . . . ? C57 C51 C56 C55 179.4(19) . . . . ? C37 Fe1 P1 C19 -167.16(15) . . . . ? C2 Fe1 P1 C19 99.81(14) . . . . ? C1 Fe1 P1 C19 116.98(19) . . . . ? C3 Fe1 P1 C19 60.84(14) . . . . ? C5 Fe1 P1 C19 28.1(3) . . . . ? C4 Fe1 P1 C19 27.23(15) . . . . ? P2 Fe1 P1 C19 -78.97(12) . . . . ? C37 Fe1 P1 C13 65.37(15) . . . . ? C2 Fe1 P1 C13 -27.65(15) . . . . ? C1 Fe1 P1 C13 -10.5(2) . . . . ? C3 Fe1 P1 C13 -66.63(14) . . . . ? C5 Fe1 P1 C13 -99.3(3) . . . . ? C4 Fe1 P1 C13 -100.23(15) . . . . ? P2 Fe1 P1 C13 153.56(12) . . . . ? C37 Fe1 P1 C11 -52.39(14) . . . . ? C2 Fe1 P1 C11 -145.42(14) . . . . ? C1 Fe1 P1 C11 -128.25(19) . . . . ? C3 Fe1 P1 C11 175.61(13) . . . . ? C5 Fe1 P1 C11 142.9(3) . . . . ? C4 Fe1 P1 C11 142.00(14) . . . . ? P2 Fe1 P1 C11 35.80(11) . . . . ? C37 Fe1 P2 C25 -56.17(14) . . . . ? C2 Fe1 P2 C25 44.1(4) . . . . ? C1 Fe1 P2 C25 27.70(16) . . . . ? C3 Fe1 P2 C25 124.79(18) . . . . ? C5 Fe1 P2 C25 59.58(15) . . . . ? C4 Fe1 P2 C25 99.78(15) . . . . ? P1 Fe1 P2 C25 -141.05(12) . . . . ? C37 Fe1 P2 C31 179.99(15) . . . . ? C2 Fe1 P2 C31 -79.8(4) . . . . ? C1 Fe1 P2 C31 -96.15(17) . . . . ? C3 Fe1 P2 C31 0.95(19) . . . . ? C5 Fe1 P2 C31 -64.27(15) . . . . ? C4 Fe1 P2 C31 -24.06(16) . . . . ? P1 Fe1 P2 C31 95.11(13) . . . . ? C37 Fe1 P2 C12 61.07(15) . . . . ? C2 Fe1 P2 C12 161.3(4) . . . . ? C1 Fe1 P2 C12 144.94(16) . . . . ? C3 Fe1 P2 C12 -117.97(18) . . . . ? C5 Fe1 P2 C12 176.82(15) . . . . ? C4 Fe1 P2 C12 -142.98(15) . . . . ? P1 Fe1 P2 C12 -23.81(12) . . . . ? C37 Fe1 C1 C5 139.71(19) . . . . ? C2 Fe1 C1 C5 -119.0(3) . . . . ? C3 Fe1 C1 C5 -80.42(19) . . . . ? C4 Fe1 C1 C5 -37.63(18) . . . . ? P1 Fe1 C1 C5 -144.99(16) . . . . ? P2 Fe1 C1 C5 55.3(2) . . . . ? C37 Fe1 C1 C2 -101.31(19) . . . . ? C3 Fe1 C1 C2 38.56(17) . . . . ? C5 Fe1 C1 C2 119.0(3) . . . . ? C4 Fe1 C1 C2 81.35(19) . . . . ? P1 Fe1 C1 C2 -26.0(3) . . . . ? P2 Fe1 C1 C2 174.27(14) . . . . ? C37 Fe1 C1 C6 19.6(3) . . . . ? C2 Fe1 C1 C6 120.9(4) . . . . ? C3 Fe1 C1 C6 159.5(3) . . . . ? C5 Fe1 C1 C6 -120.1(4) . . . . ? C4 Fe1 C1 C6 -157.8(3) . . . . ? P1 Fe1 C1 C6 94.9(3) . . . . ? P2 Fe1 C1 C6 -64.8(3) . . . . ? C5 C1 C2 C3 -1.5(3) . . . . ? C6 C1 C2 C3 173.9(3) . . . . ? Fe1 C1 C2 C3 -62.2(2) . . . . ? C5 C1 C2 C7 -176.9(3) . . . . ? C6 C1 C2 C7 -1.5(5) . . . . ? Fe1 C1 C2 C7 122.4(3) . . . . ? C5 C1 C2 Fe1 60.7(2) . . . . ? C6 C1 C2 Fe1 -123.8(3) . . . . ? C37 Fe1 C2 C1 79.09(19) . . . . ? C3 Fe1 C2 C1 -116.9(3) . . . . ? C5 Fe1 C2 C1 -37.04(18) . . . . ? C4 Fe1 C2 C1 -80.19(19) . . . . ? P1 Fe1 C2 C1 164.99(16) . . . . ? P2 Fe1 C2 C1 -20.4(5) . . . . ? C37 Fe1 C2 C3 -164.01(18) . . . . ? C1 Fe1 C2 C3 116.9(3) . . . . ? C5 Fe1 C2 C3 79.87(19) . . . . ? C4 Fe1 C2 C3 36.72(18) . . . . ? P1 Fe1 C2 C3 -78.10(17) . . . . ? P2 Fe1 C2 C3 96.5(4) . . . . ? C37 Fe1 C2 C7 -42.1(3) . . . . ? C1 Fe1 C2 C7 -121.2(4) . . . . ? C3 Fe1 C2 C7 121.9(4) . . . . ? C5 Fe1 C2 C7 -158.2(3) . . . . ? C4 Fe1 C2 C7 158.6(3) . . . . ? P1 Fe1 C2 C7 43.8(3) . . . . ? P2 Fe1 C2 C7 -141.5(3) . . . . ? C1 C2 C3 C4 1.6(3) . . . . ? C7 C2 C3 C4 177.0(3) . . . . ? Fe1 C2 C3 C4 -60.3(2) . . . . ? C1 C2 C3 C8 -170.1(3) . . . . ? C7 C2 C3 C8 5.3(5) . . . . ? Fe1 C2 C3 C8 128.0(3) . . . . ? C1 C2 C3 Fe1 61.9(2) . . . . ? C7 C2 C3 Fe1 -122.8(3) . . . . ? C37 Fe1 C3 C4 141.1(2) . . . . ? C2 Fe1 C3 C4 119.4(3) . . . . ? C1 Fe1 C3 C4 80.8(2) . . . . ? C5 Fe1 C3 C4 37.75(19) . . . . ? P1 Fe1 C3 C4 -129.86(17) . . . . ? P2 Fe1 C3 C4 -40.1(2) . . . . ? C37 Fe1 C3 C2 21.8(3) . . . . ? C1 Fe1 C3 C2 -38.59(18) . . . . ? C5 Fe1 C3 C2 -81.61(19) . . . . ? C4 Fe1 C3 C2 -119.4(3) . . . . ? P1 Fe1 C3 C2 110.78(17) . . . . ? P2 Fe1 C3 C2 -159.51(14) . . . . ? C37 Fe1 C3 C8 -96.9(3) . . . . ? C2 Fe1 C3 C8 -118.7(4) . . . . ? C1 Fe1 C3 C8 -157.3(3) . . . . ? C5 Fe1 C3 C8 159.7(3) . . . . ? C4 Fe1 C3 C8 121.9(4) . . . . ? P1 Fe1 C3 C8 -7.9(3) . . . . ? P2 Fe1 C3 C8 81.8(3) . . . . ? C2 C3 C4 C5 -1.1(3) . . . . ? C8 C3 C4 C5 170.5(3) . . . . ? Fe1 C3 C4 C5 -60.2(2) . . . . ? C2 C3 C4 C9 -170.2(3) . . . . ? C8 C3 C4 C9 1.4(5) . . . . ? Fe1 C3 C4 C9 130.7(3) . . . . ? C2 C3 C4 Fe1 59.1(2) . . . . ? C8 C3 C4 Fe1 -129.3(3) . . . . ? C37 Fe1 C4 C3 -86.7(3) . . . . ? C2 Fe1 C4 C3 -37.42(19) . . . . ? C1 Fe1 C4 C3 -81.0(2) . . . . ? C5 Fe1 C4 C3 -118.4(3) . . . . ? P1 Fe1 C4 C3 61.1(2) . . . . ? P2 Fe1 C4 C3 154.37(17) . . . . ? C37 Fe1 C4 C5 31.6(3) . . . . ? C2 Fe1 C4 C5 80.97(19) . . . . ? C1 Fe1 C4 C5 37.37(18) . . . . ? C3 Fe1 C4 C5 118.4(3) . . . . ? P1 Fe1 C4 C5 179.48(15) . . . . ? P2 Fe1 C4 C5 -87.23(17) . . . . ? C37 Fe1 C4 C9 151.4(3) . . . . ? C2 Fe1 C4 C9 -159.3(4) . . . . ? C1 Fe1 C4 C9 157.1(4) . . . . ? C3 Fe1 C4 C9 -121.8(4) . . . . ? C5 Fe1 C4 C9 119.8(4) . . . . ? P1 Fe1 C4 C9 -60.8(3) . . . . ? P2 Fe1 C4 C9 32.5(3) . . . . ? C2 C1 C5 C4 0.9(3) . . . . ? C6 C1 C5 C4 -174.7(3) . . . . ? Fe1 C1 C5 C4 60.7(2) . . . . ? C2 C1 C5 C10 170.4(3) . . . . ? C6 C1 C5 C10 -5.2(5) . . . . ? Fe1 C1 C5 C10 -129.8(3) . . . . ? C2 C1 C5 Fe1 -59.8(2) . . . . ? C6 C1 C5 Fe1 124.7(3) . . . . ? C3 C4 C5 C1 0.1(3) . . . . ? C9 C4 C5 C1 169.4(3) . . . . ? Fe1 C4 C5 C1 -60.2(2) . . . . ? C3 C4 C5 C10 -169.3(3) . . . . ? C9 C4 C5 C10 0.0(5) . . . . ? Fe1 C4 C5 C10 130.4(3) . . . . ? C3 C4 C5 Fe1 60.3(2) . . . . ? C9 C4 C5 Fe1 -130.4(3) . . . . ? C37 Fe1 C5 C1 -45.8(2) . . . . ? C2 Fe1 C5 C1 37.60(18) . . . . ? C3 Fe1 C5 C1 81.21(19) . . . . ? C4 Fe1 C5 C1 118.5(3) . . . . ? P1 Fe1 C5 C1 117.3(3) . . . . ? P2 Fe1 C5 C1 -138.60(17) . . . . ? C37 Fe1 C5 C4 -164.29(18) . . . . ? C2 Fe1 C5 C4 -80.93(19) . . . . ? C1 Fe1 C5 C4 -118.5(3) . . . . ? C3 Fe1 C5 C4 -37.33(18) . . . . ? P1 Fe1 C5 C4 -1.2(4) . . . . ? P2 Fe1 C5 C4 102.86(17) . . . . ? C37 Fe1 C5 C10 74.2(4) . . . . ? C2 Fe1 C5 C10 157.5(4) . . . . ? C1 Fe1 C5 C10 119.9(4) . . . . ? C3 Fe1 C5 C10 -158.9(4) . . . . ? C4 Fe1 C5 C10 -121.5(4) . . . . ? P1 Fe1 C5 C10 -122.8(3) . . . . ? P2 Fe1 C5 C10 -18.7(3) . . . . ? C19 P1 C11 C12 85.4(2) . . . . ? C13 P1 C11 C12 -169.4(2) . . . . ? Fe1 P1 C11 C12 -42.3(2) . . . . ? P1 C11 C12 P2 23.2(3) . . . . ? C25 P2 C12 C11 132.5(2) . . . . ? C31 P2 C12 C11 -124.6(2) . . . . ? Fe1 P2 C12 C11 4.3(3) . . . . ? C19 P1 C13 C18 -26.5(3) . . . . ? C11 P1 C13 C18 -130.8(3) . . . . ? Fe1 P1 C13 C18 109.5(3) . . . . ? C19 P1 C13 C14 156.8(3) . . . . ? C11 P1 C13 C14 52.5(3) . . . . ? Fe1 P1 C13 C14 -67.2(3) . . . . ? C18 C13 C14 C15 -0.3(5) . . . . ? P1 C13 C14 C15 176.5(3) . . . . ? C13 C14 C15 C16 -0.1(5) . . . . ? C14 C15 C16 C17 0.9(6) . . . . ? C15 C16 C17 C18 -1.4(6) . . . . ? C16 C17 C18 C13 1.0(6) . . . . ? C14 C13 C18 C17 -0.1(5) . . . . ? P1 C13 C18 C17 -176.9(3) . . . . ? C13 P1 C19 C20 133.4(3) . . . . ? C11 P1 C19 C20 -119.8(3) . . . . ? Fe1 P1 C19 C20 -1.5(3) . . . . ? C13 P1 C19 C24 -50.6(3) . . . . ? C11 P1 C19 C24 56.3(3) . . . . ? Fe1 P1 C19 C24 174.6(2) . . . . ? C24 C19 C20 C21 1.2(5) . . . . ? P1 C19 C20 C21 177.4(2) . . . . ? C19 C20 C21 C22 -0.3(5) . . . . ? C20 C21 C22 C23 -1.5(6) . . . . ? C21 C22 C23 C24 2.3(6) . . . . ? C22 C23 C24 C19 -1.4(6) . . . . ? C20 C19 C24 C23 -0.4(5) . . . . ? P1 C19 C24 C23 -176.5(3) . . . . ? C31 P2 C25 C30 140.6(3) . . . . ? C12 P2 C25 C30 -113.7(3) . . . . ? Fe1 P2 C25 C30 7.4(3) . . . . ? C31 P2 C25 C26 -41.2(3) . . . . ? C12 P2 C25 C26 64.5(3) . . . . ? Fe1 P2 C25 C26 -174.3(2) . . . . ? C30 C25 C26 C27 -1.1(5) . . . . ? P2 C25 C26 C27 -179.4(3) . . . . ? C25 C26 C27 C28 0.5(5) . . . . ? C26 C27 C28 C29 -0.1(5) . . . . ? C27 C28 C29 C30 0.4(5) . . . . ? C26 C25 C30 C29 1.4(5) . . . . ? P2 C25 C30 C29 179.6(2) . . . . ? C28 C29 C30 C25 -1.0(5) . . . . ? C25 P2 C31 C36 137.5(3) . . . . ? C12 P2 C31 C36 32.9(3) . . . . ? Fe1 P2 C31 C36 -89.2(3) . . . . ? C25 P2 C31 C32 -46.4(3) . . . . ? C12 P2 C31 C32 -151.0(3) . . . . ? Fe1 P2 C31 C32 86.9(3) . . . . ? C36 C31 C32 C33 0.5(5) . . . . ? P2 C31 C32 C33 -175.8(3) . . . . ? C31 C32 C33 C34 -1.2(6) . . . . ? C32 C33 C34 C35 1.0(6) . . . . ? C33 C34 C35 C36 -0.2(6) . . . . ? C34 C35 C36 C31 -0.5(5) . . . . ? C32 C31 C36 C35 0.3(5) . . . . ? P2 C31 C36 C35 176.5(3) . . . . ? C2 Fe1 C37 C38 15(4) . . . . ? C1 Fe1 C37 C38 54(4) . . . . ? C3 Fe1 C37 C38 1(4) . . . . ? C5 Fe1 C37 C38 81(4) . . . . ? C4 Fe1 C37 C38 59(4) . . . . ? P1 Fe1 C37 C38 -93(4) . . . . ? P2 Fe1 C37 C38 -178(100) . . . . ? Fe1 C37 C38 C39 70(7) . . . . ? C37 C38 C39 C40 -36(100) . . . . ? C38 C39 C40 Si1 -170(100) . . . . ? C43 Si1 C40 C39 -67(4) . . . . ? C42 Si1 C40 C39 53(4) . . . . ? C41 Si1 C40 C39 173(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.410 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.087