#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003575.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_2003575 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _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 mer-[(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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _symmetry_space_group_name_H-M 'P 21/n' _cell_length_a 9.676(5) _cell_length_b 14.046(3) _cell_length_c 10.476(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.357(4) _cell_angle_gamma 90.00 _cell_volume 1412.1(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.473 _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 4.18 _cell_measurement_theta_max 11.79 _exptl_absorpt_coefficient_mu 9.620 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_colour pink _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 0.6329 _exptl_absorpt_correction_T_max 0.9987 _diffrn_reflns_number 2627 _reflns_number_total 2474 _reflns_number_observed 2033 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time 250 _diffrn_standards_decay_% 2.1 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0183 _refine_ls_wR_factor_obs 0.0390 _refine_ls_wR_factor_all 0.0453 _refine_ls_goodness_of_fit_obs 1.094 _refine_ls_goodness_of_fit_all 1.139 _refine_ls_number_reflns 2474 _refine_ls_number_parameters 230 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0142P)^2^ + 0.4674P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.001 _refine_diff_density_max .518 _refine_diff_density_min -.537 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.00092(8) 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 Os 1 0.44963(2) 0.225211(13) 0.55497(2) 0.02124(8) Cl1 1 0.52155(13) 0.37830(9) 0.53482(12) 0.0323(3) Cl2 1 0.26497(14) 0.27513(10) 0.65670(14) 0.0411(3) Cl3 1 0.62901(14) 0.16791(10) 0.45067(13) 0.0423(3) F1 1 0.5627(3) 0.2095(2) 0.7206(3) 0.0395(7) F2 1 0.3839(3) 0.0931(2) 0.5714(3) 0.0398(7) F3 1 0.3345(3) 0.2371(2) 0.3892(3) 0.0414(8) N1 1 0.6841(4) 0.5026(3) 0.8098(3) 0.0261(9) N2 1 0.8449(4) 0.4624(3) 0.6601(4) 0.0275(9) CM 1 0.8323(5) 0.4957(4) 0.7934(5) 0.0328(12) C11 1 0.6200(7) 0.5884(4) 0.7916(5) 0.0407(14) C12 1 0.4815(7) 0.5958(5) 0.8046(5) 0.050(2) C13 1 0.4108(7) 0.5178(6) 0.8396(5) 0.052(2) C14 1 0.4773(6) 0.4304(5) 0.8561(5) 0.0418(14) C15 1 0.6148(6) 0.4248(4) 0.8400(5) 0.0323(12) C21 1 0.8126(5) 0.5226(4) 0.5602(5) 0.0305(11) C22 1 0.8210(6) 0.4917(4) 0.4376(5) 0.0343(12) C23 1 0.8646(5) 0.3999(4) 0.4177(5) 0.0375(13) C24 1 0.8983(6) 0.3411(4) 0.5213(6) 0.0431(14) C25 1 0.8866(6) 0.3729(4) 0.6428(5) 0.0367(13) HM1 1 0.8771(57) 0.4453(41) 0.8623(52) 0.051(17) HM2 1 0.8676(46) 0.5592(34) 0.7957(41) 0.019(12) H11 1 0.6843(60) 0.6412(45) 0.7760(56) 0.058(19) H12 1 0.4357(65) 0.6601(49) 0.8004(56) 0.064(20) H13 1 0.3279(65) 0.5222(44) 0.8578(55) 0.053(19) H14 1 0.4328(71) 0.3762(50) 0.8762(65) 0.076(24) H15 1 0.6629(59) 0.3703(43) 0.8568(52) 0.047(17) H21 1 0.7881(58) 0.5843(43) 0.5882(53) 0.050(17) H22 1 0.8086(51) 0.5354(36) 0.3713(46) 0.030(14) H23 1 0.8789(66) 0.3710(49) 0.3304(65) 0.076(22) H24 1 0.9364(62) 0.2718(45) 0.5064(60) 0.058(18) H25 1 0.9089(56) 0.3345(42) 0.7135(53) 0.044(16) 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 Os 0.02133(11) -0.00287(9) 0.00042(7) 0.02017(10) 0.00211(8) 0.02162(10) Cl1 0.0350(7) -0.0091(5) 0.0033(5) 0.0245(6) 0.0025(5) 0.0371(6) Cl2 0.0354(7) 0.0003(6) 0.0211(6) 0.0333(7) 0.0038(7) 0.0585(8) Cl3 0.0392(7) 0.0012(7) 0.0173(6) 0.0438(8) -0.0044(7) 0.0470(8) F1 0.040(2) 0.0004(15) -0.0069(13) 0.046(2) 0.0028(13) 0.0295(15) F2 0.043(2) -0.0089(14) 0.0072(15) 0.024(2) 0.0005(13) 0.052(2) F3 0.045(2) -0.0109(15) -0.0135(14) 0.040(2) 0.0066(14) 0.034(2) N1 0.034(2) 0.003(2) 0.004(2) 0.024(2) -0.001(2) 0.020(2) N2 0.022(2) -0.001(2) 0.004(2) 0.030(2) 0.000(2) 0.030(2) CM 0.028(3) -0.005(3) 0.001(2) 0.039(3) -0.006(2) 0.031(3) C11 0.058(4) 0.010(3) 0.009(3) 0.031(3) -0.005(2) 0.034(3) C12 0.054(4) 0.033(4) 0.002(3) 0.063(4) -0.004(3) 0.031(3) C13 0.032(3) 0.014(4) 0.004(3) 0.101(6) -0.010(3) 0.023(3) C14 0.039(3) -0.006(3) 0.007(2) 0.056(4) -0.005(3) 0.030(3) C15 0.037(3) -0.004(3) 0.003(2) 0.033(3) 0.003(2) 0.027(3) C21 0.025(3) -0.002(2) 0.002(2) 0.027(3) 0.003(2) 0.038(3) C22 0.033(3) -0.005(2) 0.003(2) 0.035(3) 0.004(2) 0.034(3) C23 0.032(3) -0.008(3) 0.008(2) 0.044(3) -0.013(3) 0.037(3) C24 0.044(3) 0.003(3) 0.004(3) 0.034(3) -0.010(3) 0.051(3) C25 0.041(3) 0.007(3) 0.005(3) 0.028(3) 0.007(2) 0.041(3)