#------------------------------------------------------------------------------ #$Date: 2018-06-14 13:53:24 +0100 (Thu, 14 Jun 2018) $ #$Revision: 208377 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003266.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003266 loop_ _publ_author_name 'Kirchner, K.' 'Schmid, R.' 'Mereiter, K.' _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~ ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 361 _journal_page_last 364 _journal_paper_doi 10.1107/S0108270194005688 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C28 H24 As F6 O P Ru' _chemical_formula_weight 697.45 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_type_scat_source International_Tables_Vol_IV_Table_2.2B _audit_creation_method from_xtal_archive_file_using_CIFIO _cell_angle_alpha 90.00000 _cell_angle_beta 96.52(1) _cell_angle_gamma 90.00000 _cell_formula_units_Z 4 _cell_length_a 8.076(1) _cell_length_b 24.399(4) _cell_length_c 13.337(2) _cell_measurement_reflns_used 48 _cell_measurement_temperature 295 _cell_measurement_theta_max 22 _cell_measurement_theta_min 6 _cell_volume 2611.0(7) _diffrn_measurement_device 'Philips PW1100 diffractometer' _diffrn_measurement_method \q/2\q _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71069 _diffrn_reflns_av_R_equivalents 0.010 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 4735 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% 0.8 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.967 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_type 'by Gaussian integration from crystal shape' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.774 _exptl_crystal_description plate _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.47 _refine_diff_density_min -0.29 _refine_ls_extinction_coef 0.00031(4) _refine_ls_extinction_method 'SHELX76 (Sheldrick, 1976)' _refine_ls_goodness_of_fit_obs 1.14 _refine_ls_hydrogen_treatment 'H-atom positions refined with riding model' _refine_ls_number_parameters 345 _refine_ls_number_reflns 3220 _refine_ls_R_factor_obs 0.028 _refine_ls_shift/esd_max <0.01 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w=[\s^2^(F~o~)+0.0001F~o~^2^] _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.027 _reflns_number_observed 3220 _reflns_number_total 4586 _reflns_observed_criterion '[F~o~ > 6\s(F~o~)]' _cod_data_source_file ka1055.cif _cod_data_source_block II _cod_depositor_comments ; Updating space group information and adding the symmetry operation list. Antanas Vaitkus, 2018-06-15 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w=[\s^2^(F~o~)+0.0001F~o~^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=[\s^2^(F~o~)+0.0001F~o~^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2003266 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y+1/2,-z+1/2 3 -x,-y,-z 4 x,-y+1/2,z+1/2 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 .0352(2) -.0087(2) .0064(1) .0402(2) -.0002(2) .0335(2) C(1) .040(3) -.030(3) -.007(3) .091(4) .015(3) .077(4) C(2) .041(3) -.033(3) .023(3) .109(5) -.023(4) .093(4) C(3) .084(4) -.068(4) .004(3) .099(5) .013(3) .062(4) C(4) .090(4) -.039(3) .008(3) .051(3) -.006(3) .086(4) C(5) .079(4) -.047(3) -.003(3) .077(4) -.005(3) .051(3) C(6) .042(2) -.010(2) -.008(2) .066(3) .007(2) .029(2) C(7) .050(3) -.002(2) .003(2) .043(3) -.003(2) .036(2) C(8) .045(2) -.009(2) .008(2) .070(3) -.004(2) .032(2) C(9) .061(3) -.006(2) -.002(2) .051(3) .008(2) .042(3) C(10) .046(3) .009(2) .004(2) .060(3) -.001(2) .046(3) O .044(2) -.030(2) -.012(2) .099(3) .022(2) .059(2) As .0284(2) .0007(2) .0048(2) .0352(2) -.0007(2) .0312(2) C(11) .028(2) -.004(2) .002(2) .046(3) -.000(2) .030(2) C(12) .038(2) .002(2) .004(2) .054(3) -.007(2) .042(2) C(13) .045(3) -.009(3) .000(2) .079(4) -.015(2) .036(2) C(14) .037(2) .000(2) -.006(2) .077(3) .007(2) .038(2) C(15) .037(2) .014(2) .001(2) .060(3) .004(2) .051(3) C(16) .038(2) .008(2) -.001(2) .056(3) -.008(2) .038(2) C(17) .032(2) -.005(2) -.001(2) .041(2) .002(2) .034(2) C(18) .040(2) -.000(2) .001(2) .047(3) -.008(2) .044(2) C(19) .059(3) .003(2) -.006(2) .043(3) -.009(2) .053(3) C(20) .072(3) -.017(3) -.005(2) .041(3) .001(2) .048(3) C(21) .052(3) -.023(3) .006(2) .068(4) .002(2) .048(3) C(22) .038(2) -.006(2) .006(2) .055(3) -.006(2) .041(2) C(23) .034(2) .007(2) .005(2) .043(3) -.005(2) .036(2) C(24) .054(3) .014(2) .014(2) .048(3) .007(2) .042(2) C(25) .081(4) .030(3) .023(3) .052(3) .011(3) .065(3) C(26) .062(3) .028(3) .018(2) .069(4) -.004(3) .054(3) C(27) .043(2) .007(2) .012(2) .068(3) .003(2) .040(2) C(28) .040(2) .006(2) .009(2) .046(3) .005(2) .041(2) P .0596(7) .0006(6) .0121(6) .0441(7) .0006(6) .0542(7) F(1) .113(2) -.006(2) .023(2) .048(2) .011(1) .087(2) F(2) .095(2) .009(2) .050(2) .082(2) -.006(2) .102(2) F(3) .076(2) -.015(2) -.015(2) .100(2) .028(2) .090(2) F(4) .140(3) .019(2) .080(2) .096(2) .004(2) .108(2) F(5) .124(3) .004(2) -.044(2) .113(3) -.012(2) .098(2) F(6) .091(2) -.007(2) .028(2) .042(2) .001(2) .132(3) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Ru .60922(4) .37680(1) .20020(2) .0361(2) Uani C(1) .8523(6) .3781(3) .2937(4) .070(3) Uani C(2) .8806(6) .3882(3) .1951(5) .080(4) Uani C(3) .7956(7) .4374(3) .1652(4) .082(4) Uani C(4) .7175(7) .4570(2) .2470(4) .076(4) Uani C(5) .7530(7) .4200(2) .3254(4) .070(3) Uani C(6) .3347(5) .3272(2) .1216(3) .047(2) Uani C(7) .4995(5) .3107(2) .0936(3) .043(2) Uani C(8) .5615(5) .3546(2) .0426(3) .049(2) Uani C(9) .4677(5) .4019(2) .0607(3) .052(3) Uani C(10) .3460(5) .3875(2) .1226(3) .051(3) Uani O .2203(3) .2987(1) .1415(2) .068(2) Uani As .49669(4) .32769(2) .34355(3) .0315(2) Uani C(11) .6674(4) .3097(2) .4544(3) .035(2) Uani C(12) .6869(5) .3398(2) .5429(3) .045(2) Uani C(13) .8057(5) .3255(2) .6217(3) .053(3) Uani C(14) .9059(5) .2810(2) .6127(3) .051(3) Uani C(15) .8913(5) .2515(2) .5252(3) .049(3) Uani C(16) .7738(5) .2654(2) .4463(3) .044(2) Uani C(17) .3936(4) .2556(2) .3251(3) .036(2) Uani C(18) .4813(5) .2149(2) .2808(3) .044(2) Uani C(19) .4234(5) .1616(2) .2760(3) .053(3) Uani C(20) .2775(6) .1488(2) .3143(3) .055(3) Uani C(21) .1869(6) .1888(2) .3549(3) .056(3) Uani C(22) .2434(5) .2429(2) .3603(3) .044(2) Uani C(23) .3467(4) .3722(2) .4137(3) .037(2) Uani C(24) .3111(5) .4248(2) .3795(3) .047(2) Uani C(25) .2134(6) .4591(2) .4311(3) .065(3) Uani C(26) .1523(6) .4410(2) .5169(3) .060(3) Uani C(27) .1867(5) .3888(2) .5512(3) .050(3) Uani C(28) .2843(5) .3543(2) .5009(3) .042(2) Uani P .8345(2) .44766(5) -.15989(9) .0522(7) Uani F(1) .7998(4) .3841(1) -.1432(2) .082(2) Uani F(2) .9583(3) .4326(1) -.2382(2) .090(2) Uani F(3) .6871(3) .4490(1) -.2474(2) .090(2) Uani F(4) .7086(4) .4629(1) -.0808(2) .110(2) Uani F(5) .9827(4) .4451(1) -.0724(2) .116(3) Uani F(6) .8678(3) .5104(1) -.1770(2) .087(2) Uani H(1) .8939 .3473 .3337 .078 Uiso H(2) .9455 .3661 .1545 .089 Uiso H(3) .7920 .4544 .1001 .091 Uiso H(4) .6521 .4898 .2484 .084 Uiso H(5) .7154 .4229 .3910 .077 Uiso H(7) .5537 .2761 .1081 .048 Uiso H(8) .6523 .3530 .0020 .054 Uiso H(9) .4848 .4379 .0347 .058 Uiso H(10) .2820 .4122 .1589 .057 Uiso H(12) .6170 .3711 .5497 .050 Uiso H(13) .8177 .3468 .6825 .059 Uiso H(14) .9865 .2705 .6678 .057 Uiso H(15) .9635 .2207 .5187 .054 Uiso H(16) .7652 .2444 .3851 .049 Uiso H(18) .5827 .2239 .2534 .049 Uiso H(19) .4851 .1336 .2460 .059 Uiso H(20) .2389 .1116 .3126 .061 Uiso H(21) .0834 .1796 .3797 .062 Uiso H(22) .1790 .2709 .3882 .049 Uiso H(24) .3542 .4377 .3196 .052 Uiso H(25) .1886 .4955 .4068 .072 Uiso H(26) .0853 .4649 .5529 .067 Uiso H(27) .1425 .3762 .6109 .055 Uiso H(28) .3090 .3180 .5261 .047 Uiso loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C(1) Ru C(2) 36.4(2) no C(1) Ru C(3) 61.5(2) no C(1) Ru C(4) 61.8(2) no C(1) Ru C(5) 37.0(2) no C(1) Ru C(6) 152.5(2) no C(1) Ru C(7) 128.7(2) no C(1) Ru C(8) 127.1(2) no C(1) Ru C(9) 146.5(2) no C(1) Ru C(10) 169.8(2) no C(1) Ru As 87.30(10) no C(2) Ru C(3) 37.4(2) no C(2) Ru C(4) 62.3(2) no C(2) Ru C(5) 61.5(2) no C(2) Ru C(6) 146.6(2) no C(2) Ru C(7) 112.8(2) no C(2) Ru C(8) 94.0(2) no C(2) Ru C(9) 111.5(2) no C(2) Ru C(10) 148.0(2) no C(2) Ru As 121.8(2) no C(3) Ru C(4) 37.2(2) no C(3) Ru C(5) 61.4(2) no C(3) Ru C(6) 142.1(2) no C(3) Ru C(7) 125.1(2) no C(3) Ru C(8) 90.7(2) no C(3) Ru C(9) 86.2(2) no C(3) Ru C(10) 117.0(2) no C(3) Ru As 143.00(10) no C(4) Ru C(5) 36.7(2) no C(4) Ru C(6) 144.0(2) no C(4) Ru C(7) 157.7(2) no C(4) Ru C(8) 121.3(2) no C(4) Ru C(9) 98.4(2) no C(4) Ru C(10) 110.3(2) no C(4) Ru As 112.0(2) no C(5) Ru C(6) 150.7(2) no C(5) Ru C(7) 163.1(2) no C(5) Ru C(8) 151.8(2) no C(5) Ru C(9) 134.6(2) no C(5) Ru C(10) 132.8(2) no C(5) Ru As 81.70(10) no C(6) Ru C(7) 34.00(10) no C(6) Ru C(8) 56.60(10) no C(6) Ru C(9) 56.5(2) no C(6) Ru C(10) 33.9(2) no C(6) Ru As 73.94(9) no C(7) Ru C(8) 36.6(2) no C(7) Ru C(9) 61.9(2) no C(7) Ru C(10) 61.0(2) no C(7) Ru As 89.30(10) no C(8) Ru C(9) 38.3(2) no C(8) Ru C(10) 62.1(2) no C(8) Ru As 125.50(10) no C(9) Ru C(10) 36.7(2) no C(9) Ru As 126.10(10) no C(10) Ru As 90.10(10) no Ru C(1) C(2) 72.4(3) no Ru C(1) C(5) 71.1(3) no C(2) C(1) C(5) 108.7(5) yes Ru C(2) C(1) 71.2(3) no Ru C(2) C(3) 70.5(3) no C(1) C(2) C(3) 107.0(5) yes Ru C(3) C(2) 72.1(3) no Ru C(3) C(4) 71.7(3) no C(2) C(3) C(4) 108.4(5) yes Ru C(4) C(3) 71.1(3) no Ru C(4) C(5) 71.2(3) no C(3) C(4) C(5) 106.9(5) yes Ru C(5) C(1) 71.9(3) no Ru C(5) C(4) 72.1(3) no C(1) C(5) C(4) 109.0(5) yes Ru C(6) C(7) 59.0(2) no Ru C(6) C(10) 59.3(2) no Ru C(6) O 143.6(3) no C(7) C(6) C(10) 102.6(4) yes C(7) C(6) O 129.1(4) yes C(10) C(6) O 128.3(4) yes Ru C(7) C(6) 87.0(2) no Ru C(7) C(8) 67.8(2) no C(6) C(7) C(8) 107.3(4) yes Ru C(8) C(7) 75.6(2) no Ru C(8) C(9) 70.7(2) no C(7) C(8) C(9) 108.3(4) yes Ru C(9) C(8) 71.0(2) no Ru C(9) C(10) 76.0(2) no C(8) C(9) C(10) 108.7(4) yes Ru C(10) C(6) 86.8(2) no Ru C(10) C(9) 67.3(2) no C(6) C(10) C(9) 107.0(4) yes Ru As C(11) 113.40(10) yes Ru As C(17) 121.40(10) yes Ru As C(23) 113.50(10) yes C(11) As C(17) 98.5(2) yes C(11) As C(23) 100.80(10) yes C(17) As C(23) 106.5(2) yes As C(11) C(12) 121.9(3) no As C(11) C(16) 120.4(3) no C(12) C(11) C(16) 117.8(3) no C(11) C(12) C(13) 121.0(4) no C(12) C(13) C(14) 119.9(4) no C(13) C(14) C(15) 119.9(4) no C(14) C(15) C(16) 120.6(4) no C(11) C(16) C(15) 120.7(4) no As C(17) C(18) 117.9(3) no As C(17) C(22) 122.6(3) no C(18) C(17) C(22) 119.4(4) no C(17) C(18) C(19) 120.4(4) no C(18) C(19) C(20) 119.8(4) no C(19) C(20) C(21) 120.4(4) no C(20) C(21) C(22) 120.5(4) no C(17) C(22) C(21) 119.3(4) no As C(23) C(24) 118.6(3) no As C(23) C(28) 122.1(3) no C(24) C(23) C(28) 119.1(4) no C(23) C(24) C(25) 120.4(4) no C(24) C(25) C(26) 120.0(4) no C(25) C(26) C(27) 119.9(4) no C(26) C(27) C(28) 120.7(4) no C(23) C(28) C(27) 119.8(4) no F(1) P F(2) 89.8(2) no F(1) P F(3) 89.4(2) no F(1) P F(4) 90.3(2) no F(1) P F(5) 89.7(2) no F(1) P F(6) 178.8(2) no F(2) P F(3) 89.2(2) no F(2) P F(4) 179.2(2) no F(2) P F(5) 89.7(2) no F(2) P F(6) 89.5(2) no F(3) P F(4) 90.1(2) no F(3) P F(5) 178.6(2) no F(3) P F(6) 89.6(2) no F(4) P F(5) 91.0(2) no F(4) P F(6) 90.4(2) no F(5) P F(6) 91.2(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ru C(1) 2.203(4) yes Ru C(2) 2.218(5) yes Ru C(3) 2.197(6) yes Ru C(4) 2.205(5) yes Ru C(5) 2.193(5) yes Ru C(6) 2.636(4) yes Ru C(7) 2.262(4) yes Ru C(8) 2.163(4) yes Ru C(9) 2.159(4) yes Ru C(10) 2.271(4) yes Ru As 2.5123(6) yes C(1) C(2) 1.382(8) yes C(1) C(5) 1.395(8) yes C(2) C(3) 1.417(9) yes C(3) C(4) 1.405(8) yes C(4) C(5) 1.386(7) yes C(6) C(7) 1.478(6) yes C(6) C(10) 1.473(7) yes C(6) O 1.210(5) yes C(7) C(8) 1.392(6) yes C(8) C(9) 1.416(6) yes C(9) C(10) 1.398(6) yes As C(11) 1.953(3) yes As C(17) 1.949(4) yes As C(23) 1.944(4) yes C(11) C(12) 1.384(5) yes C(11) C(16) 1.391(6) yes C(12) C(13) 1.384(5) yes C(13) C(14) 1.369(7) yes C(14) C(15) 1.363(6) yes C(15) C(16) 1.377(5) yes C(17) C(18) 1.390(6) yes C(17) C(22) 1.385(5) yes C(18) C(19) 1.381(6) yes C(19) C(20) 1.373(7) yes C(20) C(21) 1.368(7) yes C(21) C(22) 1.395(6) yes C(23) C(24) 1.381(6) yes C(23) C(28) 1.391(5) yes C(24) C(25) 1.385(6) yes C(25) C(26) 1.369(7) yes C(26) C(27) 1.371(7) yes C(27) C(28) 1.378(6) yes P F(1) 1.594(3) yes P F(2) 1.578(3) yes P F(3) 1.578(3) yes P F(4) 1.581(4) yes P F(5) 1.567(3) yes P F(6) 1.578(3) yes