#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/20/2002089.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_2002089 loop_ _publ_author_name 'Blake, A. J.' 'Fotheringham, J. D.' 'Stephenson, T. A.' _publ_section_title '[{(\h^6^-C~6~H~6~)(PMe~2~Ph)RuCl}~2~(\m-Ph~2~PCH~2~CH~2~PPh~2~)]^2+^.2PF~6~^{-^}.CH~3~NO~2~' _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 142 _journal_page_last 144 _journal_paper_doi 10.1107/S0108270192008163 _journal_volume 49 _journal_year 1993 _chemical_formula_moiety 'C54 H58 Cl2 P4 Ru2,C1 H3 N1 O2,F12 P2' _chemical_formula_sum 'C55 H61 Cl2 F12 N O2 P6 Ru2' _chemical_formula_weight 1454.8 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/c 1 1' _atom_type_scat_source 'inlaid except for Ru (Cromer & Mann, 1968)' _cell_angle_alpha 90 _cell_angle_beta 105.999(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 28.325(6) _cell_length_b 9.790(5) _cell_length_c 23.042(6) _cell_measurement_reflns_used 15 _cell_measurement_temperature 293 _cell_measurement_theta_max 17.5 _cell_measurement_theta_min 3.5 _cell_volume 6142(4) _diffrn_measurement_device 'Sto\"e Stadi-2' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_theta_max 25.0 _diffrn_standards_number No _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type none _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.573 _exptl_crystal_description Needle _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.98 _refine_diff_density_min -0.64 _refine_ls_goodness_of_fit_obs 1.406 _refine_ls_hydrogen_treatment 'H atoms in calculated positions' _refine_ls_number_parameters 167 _refine_ls_number_reflns 4031 _refine_ls_R_factor_obs 0.0611 _refine_ls_shift/esd_max 0.10 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s(F)+0.000243F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.0753 _reflns_number_observed 4031 _reflns_number_total 5811 _reflns_observed_criterion F>6.0\s(F) _cod_data_source_file ha1003.cif _cod_data_source_block ha1003_structure_1_of_1 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/[\s(F)+0.000243F^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s(F)+0.000243F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 6142 _cod_original_sg_symbol_H-M I2/c _cod_original_formula_sum 'C55 H61 Cl2 F12 N1 O2 P6 Ru2' _cod_database_code 2002089 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Ru -.12962(2) .08718(5) .36020(2) .0314(3) Cl -.06788(7) .2604(2) .37346(9) .0559(12) P(1) -.07333(6) -.04528(17) .43236(8) .0312(9) P(2) -.15877(8) .1950(2) .43426(9) .0523(13) C(1) -.12595(15) -.0110(5) .2728(2) .0507(19) C(2) -.15011(15) -.0992(5) .3027(2) .0524(19) C(3) -.19136(15) -.0543(5) .3191(2) .055(2) C(4) -.20840(15) .0789(5) .3058(2) .0517(19) C(5) -.18424(15) .1671(5) .2759(2) .053(2) C(6) -.14301(15) .1222(5) .2595(2) .052(2) C(1M) -.0215(2) .0462(7) .4826(3) .0354(15) C(111) -.04055(16) -.1669(4) .3971(2) .0358(15) C(112) -.01479(16) -.1116(4) .3591(2) .0442(17) C(113) .01443(16) -.1956(4) .3344(2) .062(2) C(114) .01786(16) -.3349(4) .3477(2) .078(3) C(115) -.00790(16) -.3902(4) .3857(2) .077(3) C(116) -.03712(16) -.3062(4) .4104(2) .056(2) C(121) -.10027(17) -.1487(5) .4817(2) .0375(16) C(122) -.13601(17) -.2446(5) .4546(2) .0495(19) C(123) -.15869(17) -.3222(5) .4900(2) .060(2) C(124) -.14559(17) -.3041(5) .5525(2) .074(3) C(125) -.10983(17) -.2083(5) .5795(2) .072(3) C(126) -.08716(17) -.1306(5) .5441(2) .054(2) C(2M) -.1966(4) .0850(10) .4676(4) .076(3) C(3M) -.1175(3) .2706(10) .4996(4) .077(3) C(211) -.19950(16) .3378(4) .4026(2) .0438(17) C(212) -.18479(16) .4327(4) .3659(2) .0522(19) C(213) -.21555(16) .5414(4) .3411(2) .058(2) C(214) -.26102(16) .5554(4) .3530(2) .065(2) C(215) -.27572(16) .4606(4) .3897(2) .065(2) C(216) -.24496(16) .3518(4) .4145(2) .057(2) P(3) -.34688(8) -.0715(2) .30998(12) .0627(15) F(1) -.3054(2) -.1508(6) .2902(3) .101(5) F(2)* -.3613(4) -.2199(12) .3310(6) .089(3) F(3) -.3183(5) -.0862(13) .3745(4) .238(12) F(4)* -.3141(4) .0667(11) .3294(6) .077(3) F(5)* -.3854(6) -.1016(18) .2482(8) .132(5) F(6)* -.3913(4) .0252(10) .3160(5) .058(3) F(2')* -.3823(5) -.1966(14) .2905(7) .100(4) F(4')* -.3271(5) .0658(14) .2906(7) .105(4) F(5')* -.3646(6) -.0189(17) .2391(7) .121(5) F(6')* -.3842(5) -.0115(14) .3447(6) .095(4) N(1) .0000 -.1948(11) .7500 .065(3) O(1) -.0356(3) -.1323(8) .7217(4) .100(2) C(1S) .0000 -.3411(17) .7500 .099(5) H(1) -.0997 -.0255 .2625 ? H(2) -.1448 -.1815 .3129 ? H(3) -.2149 -.0952 .3469 ? H(4) -.2399 .1471 .3304 ? H(5) -.1949 .3031 .2800 ? H(6) -.1248 .2168 .2461 ? H(1M1) -.0349 .1019 .5152 ? H(1M2) -.0073 .1172 .4556 ? H(112) -.0175 -.0038 .3488 ? H(113) .0344 -.1528 .3049 ? H(114) .0405 -.3999 .3285 ? H(115) -.0052 -.4980 .3960 ? H(116) -.0571 -.3490 .4399 ? H(122) -.1461 -.2586 .4063 ? H(123) -.1864 -.3964 .4691 ? H(124) -.1631 -.3643 .5799 ? H(125) -.0997 -.1942 .6279 ? H(126) -.0595 -.0564 .5650 ? H(1M2') -.1774 -.0095 .4823 ? H(2M2) -.2309 .0635 .4343 ? H(3M2 -.2038 .1361 .5058 ? H(1M3) -.0911 .1953 .5227 ? H(2M3) -.1381 .3072 .5296 ? H(3M3) -.0985 .3550 .4859 ? H(212) -.1496 .4219 .3567 ? H(213) -.2042 .6149 .3126 ? H(214) -.2848 .6396 .3337 ? H(215) -.3109 .4713 .3989 ? H(216) -.2564 .2783 .4429 ? H(1SA) -.0028 -.3505 .7956 ? H(1SB) .0257 -.4158 .7424 ? H(1SC) -.0356 -.3584 .7186 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Cl Ru P(1) 88.36(7) Cl Ru P(2) 88.83(7) P(1) Ru P(2) 92.29(7) Ru P(1) C(1M) 116.5(2) Ru P(1) C(111) 111.90(16) Ru P(1) C(121) 115.15(17) C(1M) P(1) C(111) 100.4(3) C(1M) P(1) C(121) 106.0(3) C(111) P(1) C(121) 105.3(2) P(1) C(1M) C(1M') 114.8(5) P(1) C(111) C(112) 116.3(3) P(1) C(111) C(116) 123.5(3) P(1) C(121) C(122) 117.9(4) P(1) C(121) C(126) 122.0(4) Ru P(2) C(2M) 113.9(3) Ru P(2) C(3M) 121.3(3) Ru P(2) C(211) 111.36(18) C(2M) P(2) C(3M) 102.3(5) C(2M) P(2) C(211) 103.8(4) C(3M) P(2) C(211) 102.3(4) P(2) C(211) C(212) 119.3(4) P(2) C(211) C(216) 120.7(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ru Cl 2.394(2) Ru C(1) 2.259(5) Ru C(2) 2.236(5) Ru C(3) 2.227(5) Ru C(4) 2.240(5) Ru C(5) 2.263(5) Ru C(6) 2.273(5) Ru P(1) 2.3509(18) Ru P(2) 2.342(2) P(1) C(1M) 1.834(7) P(1) C(111) 1.832(5) P(1) C(121) 1.837(5) P(2) C(2M) 1.831(10) P(2) C(3M) 1.792(10) P(2) C(211) 1.831(5)