#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003265.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003265 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 361 _journal_page_last 364 _publ_section_title ; [Ru(\h^5^-C~5~H~5~)(\h^4^-C~5~H~4~O){As(CH~3~)~3~}]PF~6~ and [Ru(\h^5^-C~5~H~5~)(\h^4^-C~5~H~4~O){As(C~6~H~5~)~3~}]PF~6~ ; _chemical_formula_sum 'C13 H18 As F6 O P Ru' _chemical_formula_weight 511.24 _symmetry_space_group_name_H-M 'P 21/c' _cell_length_a 8.421(2) _cell_length_b 11.421(2) _cell_length_c 17.431(4) _cell_angle_alpha 90.00000 _cell_angle_beta 93.84(1) _cell_angle_gamma 90.00000 _cell_volume 1672.7(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.030 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14 _cell_measurement_theta_max 26 _exptl_absorpt_coefficient_mu 3.03 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.22 _exptl_crystal_colour yellow _diffrn_measurement_device 'Philips PW1100 diffractometer' _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type 'by Gaussian integration from crystal shape' _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.52 _diffrn_reflns_number 4087 _reflns_number_total 3657 _reflns_number_observed 2888 _reflns_observed_criterion '[F~o~ > 6\s(F~o~)]' _diffrn_reflns_av_R_equivalents 0.011 _diffrn_reflns_theta_max 27 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1.2 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.026 _refine_ls_wR_factor_obs 0.030 _refine_ls_goodness_of_fit_obs 1.31 _refine_ls_number_reflns 2888 _refine_ls_number_parameters 232 _refine_ls_hydrogen_treatment 'H-atom positions refined with riding model (C _refine_ls_weighting_scheme 'w=[\s^2^(F~o~)+0.0002F~o~^2^]' _refine_ls_shift/esd_max '<0.01' _refine_diff_density_max 0.45 _refine_diff_density_min -0.59 _refine_ls_extinction_method 'SHELX76 (Sheldrick, 1976)' _refine_ls_extinction_coef 'x = 0.00204(7)' _atom_type_scat_source International_Tables_Vol_IV_Table_2.2B loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Ru .29625(3) .39181(2) .23899(1) .0334(1) C(1) .5041(4) .4439(3) .3139(2) .053(2) C(2) .5577(4) .4148(3) .2426(2) .051(2) C(3) .4863(4) .4920(3) .1876(2) .049(2) C(4) .3879(4) .5713(3) .2252(2) .051(2) C(5) .3977(4) .5423(3) .3030(2) .052(2) C(6) .0505(4) .2561(3) .2075(2) .057(2) C(7) .2140(5) .2140(3) .1978(2) .061(2) C(8) .2776(6) .2793(4) .1401(2) .073(3) C(9) .1790(6) .3784(4) .1268(2) .076(3) C(10) .0556(5) .3753(3) .1768(2) .060(2) O -.0577(3) .2066(3) .2376(2) .078(2) As .16705(4) .34955(3) .36042(2) .0419(2) C(11) .2632(6) .4145(4) .4556(2) .074(3) C(12) -.0448(5) .4151(4) .3622(3) .076(3) C(13) .1526(5) .1880(3) .3907(3) .069(3) P .7063(1) .30149(8) .01187(5) .0471(5) F(1) .5433(3) .3669(3) -.0064(2) .112(2) F(2) .8680(3) .2348(2) .0307(1) .090(2) F(3) .626(1) .1771(5) .0024(7) .150(4) F(4) .734(1) .2997(9) -.0753(3) .126(4) F(5) .793(1) .4172(5) .0233(7) .150(4) F(6) .6864(9) .2956(9) .1003(3) .126(4) F(3') .657(1) .215(1) -.0518(9) .113(7) F(4') .788(2) .376(1) -.047(1) .116(7) F(5') .742(1) .395(1) .0761(9) .113(7) F(6') .610(1) .236(1) .0664(9) .116(7) H(1) .5328 .4054 .3618 .069 H(2) .6307 .3529 .2326 .068 H(3) .5016 .4911 .1335 .064 H(4) .3259 .6336 .2014 .068 H(5) .3432 .5811 .3424 .069 H(7) .2671 .1519 .2264 .080 H(8) .3712 .2606 .1140 .097 H(9) .1942 .4384 .0894 .098 H(10) -.0126 .4392 .1887 .080 H(11a) .2514 .4981 .4567 .098 H(11b) .3722 .3942 .4689 .098 H(11c) .1964 .3797 .4919 .098 H(12a) -.1084 .3821 .3199 .098 H(12b) -.0318 .4976 .3539 .098 H(12c) -.0967 .4029 .4089 .098 H(13a) .0992 .1365 .3538 .098 H(13b) .1001 .1854 .4379 .098 H(13c) .2612 .1634 .4001 .098 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Ru .0331(1) -.0038(1) .0021(1) .0307(1) .0007(1) .0364(1) C(1) .042(2) -.015(2) -.008(2) .063(2) .005(2) .052(2) C(2) .035(2) -.006(2) .007(2) .048(2) .001(2) .072(2) C(3) .049(2) -.017(2) .012(2) .048(2) .002(2) .051(2) C(4) .055(2) -.010(2) .002(2) .032(2) .004(2) .067(2) C(5) .054(2) -.015(2) .007(2) .048(2) -.015(2) .055(2) C(6) .051(2) -.021(2) -.011(2) .059(2) -.001(2) .061(2) C(7) .065(2) -.010(2) .006(2) .044(2) -.017(2) .075(3) C(8) .080(3) -.031(3) .015(2) .079(3) -.033(2) .060(3) C(9) .096(3) -.046(3) -.018(2) .088(3) .008(2) .041(2) C(10) .053(2) -.014(2) -.016(2) .059(3) .012(2) .066(3) O .057(2) -.038(2) -.002(2) .081(2) .012(2) .096(2) As .0405(2) .0051(1) .0101(1) .0404(2) .0087(1) .0458(2) C(11) .090(3) .003(3) .015(2) .088(3) -.002(2) .047(2) C(12) .055(2) .019(2) .033(2) .077(3) .025(3) .098(3) C(13) .074(3) .005(2) .017(2) .054(2) .029(2) .081(3) P .0520(5) .0022(4) .0071(4) .0481(5) .0037(4) .0417(5) F(1) .087(2) .053(2) -.010(2) .129(3) .004(2) .119(2) F(2) .070(2) .032(2) -.004(1) .113(2) -.006(2) .086(2) F(3) .160(5) -.045(3) -.061(5) .068(2) .025(4) .212(7) F(4) .139(5) .056(4) .017(2) .196(6) .007(3) .043(2) F(5) .160(5) -.045(3) -.061(5) .068(2) .025(4) .212(7) F(6) .139(5) .056(4) .017(2) .196(6) .007(3) .043(2) F(3') .083(5) .008(6) -.003(5) .125(8) -.094(7) .129(8) F(4') .116(7) -.010(5) .055(6) .120(8) .068(6) .120(8) F(5') .083(5) .008(6) -.003(5) .125(8) -.094(7) .129(8) F(6') .116(7) -.010(5) .055(6) .120(8) .068(6) .120(8)