#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003574.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_2003574 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1112 _journal_page_last 1116 _publ_section_title ; fac- and mer-Dipyridiniomethane Trichlorotrifluoroosmate(IV), fac- and mer-[(C~5~H~5~N)~2~CH~2~][OsCl~3~F~3~] ; _chemical_formula_sum 'C11 H12 Cl3 F3 N2 Os' _chemical_formula_structural fac-[(C~5~H~5~N)~2~CH~2~][OsF~3~Cl~3~] _chemical_formula_weight 525.78 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 7.223(3) _cell_length_b 13.9130(15) _cell_length_c 14.9310(15) _cell_angle_alpha 100.655(9) _cell_angle_beta 101.33(3) _cell_angle_gamma 90.32(2) _cell_volume 1444.5(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.418 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.88 _cell_measurement_theta_max 10.43 _exptl_absorpt_coefficient_mu 9.404 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_colour orange _chemical_compound_source 'crystallized from water/acetone' _diffrn_measurement_device ; Enraf-Nonius CAD4-Turbo four-circle ; _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type 'empirical (\y scans)' _exptl_absorpt_correction_T_min 0.5209 _exptl_absorpt_correction_T_max 0.9986 _diffrn_reflns_number 5531 _reflns_number_total 5088 _reflns_number_observed 4709 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0128 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time 250 _diffrn_standards_decay_% 1.2 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0187 _refine_ls_wR_factor_obs 0.0503 _refine_ls_wR_factor_all 0.0525 _refine_ls_goodness_of_fit_obs 1.199 _refine_ls_goodness_of_fit_all 1.199 _refine_ls_number_reflns 5088 _refine_ls_number_parameters 458 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0247P)^2^ + 2.2353P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.002 _refine_diff_density_max 1.039 _refine_diff_density_min -.607 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0064(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0033 .0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0061 .0033 'F' 'F' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0171 .0103 'Cl' 'Cl' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1484 .158 'Os' 'Os' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -1.2165 7. ; CAD4-PC (Enraf-Nonius, 1993) ; ; CAD4-PC (Enraf-Nonius, 1993) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Os1 1 0.08135(2) 0.743535(11) 0.716558(10) 0.02207(7) Cl11 1 0.0457(2) 0.58840(8) 0.62422(7) 0.0320(2) Cl12 1 -0.2303(2) 0.74164(9) 0.73219(9) 0.0394(3) Cl13 1 0.1849(2) 0.68734(10) 0.85412(8) 0.0479(3) F11 1 0.0098(4) 0.7957(2) 0.6033(2) 0.0357(6) F12 1 0.1204(4) 0.8786(2) 0.7842(2) 0.0408(6) F13 1 0.3427(3) 0.7518(2) 0.7024(2) 0.0394(6) Os2 1 0.02144(2) 0.228196(11) 0.788450(11) 0.02409(7) Cl21 1 -0.2961(2) 0.22074(9) 0.71695(8) 0.0362(2) Cl22 1 0.0408(2) 0.39441(8) 0.78529(8) 0.0368(3) Cl23 1 0.1186(2) 0.18417(10) 0.64789(9) 0.0481(3) F21 1 0.0072(4) 0.0905(2) 0.7975(2) 0.0393(6) F22 1 -0.0482(4) 0.2566(2) 0.9096(2) 0.0404(6) F23 1 0.2838(4) 0.2317(2) 0.8551(2) 0.0420(7) C1 1 0.4389(7) 0.5242(3) 0.7390(3) 0.0305(10) N1 1 0.4770(5) 0.4584(3) 0.6562(2) 0.0250(7) N2 1 0.5584(5) 0.5044(3) 0.8245(2) 0.0249(7) C11 1 0.3386(6) 0.3968(3) 0.6020(3) 0.0319(10) C12 1 0.3661(7) 0.3425(4) 0.5201(3) 0.0362(11) C13 1 0.5364(8) 0.3504(4) 0.4942(3) 0.0372(11) C14 1 0.6781(8) 0.4107(4) 0.5525(4) 0.0397(12) C15 1 0.6469(7) 0.4653(4) 0.6329(3) 0.0336(10) C21 1 0.5385(7) 0.4175(3) 0.8507(3) 0.0298(9) C22 1 0.6380(7) 0.4019(4) 0.9333(3) 0.0354(10) C23 1 0.7562(7) 0.4754(4) 0.9912(3) 0.0403(12) C24 1 0.7749(8) 0.5627(4) 0.9640(3) 0.0415(12) C25 1 0.6752(7) 0.5766(4) 0.8796(3) 0.0350(10) C2 1 0.4345(7) 0.0317(4) 0.7720(3) 0.0361(11) N3 1 0.4748(5) -0.0236(3) 0.6853(3) 0.0286(8) N4 1 0.5655(5) 0.0096(3) 0.8539(2) 0.0291(8) C31 1 0.3276(7) -0.0660(4) 0.6189(4) 0.0377(11) C32 1 0.3550(9) -0.1103(4) 0.5335(4) 0.0446(13) C33 1 0.5337(9) -0.1131(4) 0.5165(4) 0.0432(13) C34 1 0.6842(8) -0.0722(4) 0.5853(4) 0.0377(11) C35 1 0.6523(7) -0.0270(3) 0.6698(3) 0.0303(9) C41 1 0.6735(7) 0.0827(4) 0.9121(4) 0.0398(11) C42 1 0.7793(8) 0.0663(5) 0.9931(4) 0.0507(15) C43 1 0.7785(8) -0.0249(5) 1.0145(4) 0.0500(14) C44 1 0.6716(8) -0.1007(5) 0.9521(4) 0.0464(13) C45 1 0.5634(7) -0.0819(4) 0.8717(3) 0.0357(10) H1A 1 0.4601(63) 0.5931(35) 0.7363(30) 0.023(11) H1B 1 0.3105(85) 0.5156(40) 0.7430(37) 0.044(15) H11 1 0.2127(78) 0.3913(38) 0.6221(36) 0.038(14) H12 1 0.2779(84) 0.3036(42) 0.4854(40) 0.046(16) H13 1 0.5604(74) 0.3167(38) 0.4385(38) 0.039(14) H14 1 0.7774(96) 0.4163(48) 0.5435(45) 0.059(20) H15 1 0.7255(75) 0.5057(38) 0.6648(35) 0.032(14) H21 1 0.4577(76) 0.3773(39) 0.8138(36) 0.036(14) H22 1 0.6291(72) 0.3452(39) 0.9528(35) 0.036(13) H23 1 0.8116(81) 0.4656(41) 1.0475(41) 0.048(16) H24 1 0.8655(84) 0.6106(42) 1.0045(40) 0.049(16) H25 1 0.6820(75) 0.6293(41) 0.8620(36) 0.036(14) H2A 1 0.3156(90) 0.0176(43) 0.7738(40) 0.049(16) H2B 1 0.4632(81) 0.1019(45) 0.7753(38) 0.050(16) H31 1 0.2104(78) -0.0622(37) 0.6359(35) 0.036(14) H32 1 0.2418(81) -0.1371(40) 0.4864(39) 0.046(15) H33 1 0.5547(94) -0.1348(49) 0.4632(48) 0.063(20) H34 1 0.7932(77) -0.0713(37) 0.5804(35) 0.032(14) H35 1 0.7452(66) 0.0019(32) 0.7111(31) 0.018(11) H41 1 0.6752(74) 0.1445(40) 0.8941(36) 0.038(14) H42 1 0.8275(80) 0.1128(42) 1.0272(40) 0.039(15) H43 1 0.8575(76) -0.0337(38) 1.0697(38) 0.040(14) H44 1 0.6566(90) -0.1568(48) 0.9680(44) 0.057(18) H45 1 0.4898(76) -0.1269(40) 0.8299(37) 0.038(14) 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 Os1 0.02029(10) 0.00038(6) 0.00335(6) 0.02234(10) 0.00428(7) 0.02314(10) Cl11 0.0313(5) 0.0006(4) 0.0033(4) 0.0271(5) -0.0007(4) 0.0338(5) Cl12 0.0277(6) 0.0051(5) 0.0187(5) 0.0445(7) 0.0119(5) 0.0517(7) Cl13 0.0700(9) 0.0169(6) 0.0046(6) 0.0470(7) 0.0121(5) 0.0266(6) F11 0.0323(14) -0.0022(12) 0.0011(11) 0.043(2) 0.0200(12) 0.0346(14) F12 0.049(2) -0.0037(12) 0.0057(13) 0.0234(13) -0.0042(11) 0.044(2) F13 0.0193(12) -0.0045(11) 0.0041(11) 0.051(2) 0.0019(13) 0.044(2) Os2 0.02351(10) -0.00171(7) 0.00263(7) 0.02291(10) 0.00282(7) 0.02426(10) Cl21 0.0260(5) -0.0014(5) -0.0013(4) 0.0387(6) 0.0046(5) 0.0395(6) Cl22 0.0402(6) -0.0034(5) 0.0065(5) 0.0260(5) 0.0085(5) 0.0442(6) Cl23 0.0537(8) 0.0064(6) 0.0202(6) 0.0556(8) 0.0024(6) 0.0373(6) F21 0.042(2) -0.0043(11) -0.0031(12) 0.0253(13) 0.0077(12) 0.046(2) F22 0.050(2) -0.0073(13) 0.0098(12) 0.043(2) 0.0019(11) 0.0266(13) F23 0.0279(14) -0.0014(12) -0.0041(12) 0.041(2) 0.0054(13) 0.051(2) C1 0.033(3) 0.005(2) 0.001(2) 0.031(3) 0.005(2) 0.025(2) N1 0.024(2) 0.0009(14) 0.0028(14) 0.027(2) 0.0048(14) 0.023(2) N2 0.026(2) 0.0005(14) 0.0052(14) 0.024(2) 0.0022(14) 0.023(2) C11 0.028(2) 0.001(2) 0.002(2) 0.030(2) 0.007(2) 0.037(2) C12 0.038(3) -0.003(2) -0.006(2) 0.029(2) 0.002(2) 0.034(2) C13 0.051(3) 0.005(2) 0.010(2) 0.032(2) 0.004(2) 0.029(2) C14 0.035(3) -0.004(2) 0.015(2) 0.045(3) 0.005(2) 0.041(3) C15 0.031(2) -0.007(2) 0.005(2) 0.036(3) 0.006(2) 0.033(2) C21 0.031(2) -0.002(2) 0.006(2) 0.023(2) 0.002(2) 0.034(2) C22 0.041(3) 0.005(2) 0.008(2) 0.032(3) 0.011(2) 0.035(3) C23 0.040(3) 0.012(2) 0.003(2) 0.054(3) 0.009(2) 0.026(2) C24 0.041(3) -0.009(2) 0.003(2) 0.047(3) -0.002(2) 0.030(2) C25 0.043(3) -0.006(2) 0.007(2) 0.027(2) 0.004(2) 0.034(2) C2 0.035(3) 0.009(2) 0.010(2) 0.043(3) 0.008(2) 0.033(2) N3 0.030(2) -0.001(2) 0.003(2) 0.026(2) 0.0072(15) 0.029(2) N4 0.027(2) 0.001(2) 0.011(2) 0.031(2) 0.003(2) 0.029(2) C31 0.033(3) -0.010(2) 0.000(2) 0.038(3) 0.016(2) 0.042(3) C32 0.059(4) -0.011(2) -0.010(2) 0.035(3) 0.009(2) 0.033(3) C33 0.073(4) 0.007(2) 0.008(3) 0.028(3) 0.007(2) 0.028(3) C34 0.040(3) 0.013(2) 0.013(2) 0.037(3) 0.015(2) 0.042(3) C35 0.026(2) 0.001(2) 0.000(2) 0.030(2) 0.006(2) 0.033(2) C41 0.041(3) -0.006(2) 0.014(2) 0.035(3) -0.007(2) 0.040(3) C42 0.040(3) -0.008(3) 0.008(2) 0.067(4) -0.016(3) 0.035(3) C43 0.036(3) 0.012(3) 0.010(2) 0.085(5) 0.007(3) 0.028(3) C44 0.045(3) 0.010(3) 0.016(3) 0.054(3) 0.020(3) 0.047(3) C45 0.035(3) -0.003(2) 0.009(2) 0.032(3) 0.002(2) 0.039(3)