#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000274.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_4000274 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_formula_sum 'C12 H16 F12 N2 O6 Ru' _chemical_formula_weight 613.34 _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbcn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.4585(3) _cell_length_b 9.9702(1) _cell_length_c 12.2534(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2132.88(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.812 _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 10252 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2446 _reflns_number_gt 1677 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0143(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2446 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.5000 0.02996(3) 0.2500 0.02454(17) Uani 1 2 d S . . O1 O 0.40131(14) -0.1823(3) 0.1476(2) 0.0474(7) Uani 1 1 d . . . O2 O 0.42604(11) 0.1809(2) 0.19837(18) 0.0302(5) Uani 1 1 d . . . O3 O 0.44107(14) 0.2005(2) -0.01232(19) 0.0389(6) Uani 1 1 d . . . H3A H 0.4300 0.2045 0.0543 0.030(10) Uiso 1 1 calc R . . N1 N 0.43257(14) 0.0561(2) 0.3907(2) 0.0295(6) Uani 1 1 d . . . H1A H 0.4283 -0.0241 0.4274 0.035 Uiso 1 1 calc R . . H1B H 0.4554 0.1173 0.4365 0.035 Uiso 1 1 calc R . . C1 C 0.43720(18) -0.1018(3) 0.1903(3) 0.0323(7) Uani 1 1 d . . . C2 C 0.35567(18) 0.1045(3) 0.3586(3) 0.0365(8) Uani 1 1 d . . . H2A H 0.3305 0.1480 0.4218 0.044 Uiso 1 1 calc R . . H2B H 0.3236 0.0278 0.3353 0.044 Uiso 1 1 calc R . . C3 C 0.36346(19) 0.2060(3) 0.2640(3) 0.0339(8) Uani 1 1 d . . . C4 C 0.2904(2) 0.1964(4) 0.1952(3) 0.0491(10) Uani 1 1 d . . . C5 C 0.3731(2) 0.3485(3) 0.3107(3) 0.0460(9) Uani 1 1 d . . . C6 C 0.4299(2) 0.3296(3) -0.0614(3) 0.0515(10) Uani 1 1 d . . . H6A H 0.3780 0.3351 -0.0916 0.077 Uiso 1 1 calc R . . H6B H 0.4674 0.3424 -0.1200 0.077 Uiso 1 1 calc R . . H6C H 0.4367 0.3997 -0.0061 0.077 Uiso 1 1 calc R . . F1 F 0.28825(13) 0.0802(2) 0.1423(2) 0.0654(7) Uani 1 1 d . . . F2 F 0.22674(14) 0.2034(3) 0.25660(19) 0.0748(9) Uani 1 1 d . . . F3 F 0.28522(12) 0.2944(2) 0.1201(2) 0.0599(7) Uani 1 1 d . . . F4 F 0.30928(14) 0.3927(2) 0.3619(2) 0.0707(8) Uani 1 1 d . . . F5 F 0.38993(17) 0.4388(2) 0.23535(18) 0.0572(7) Uani 1 1 d . . . F6 F 0.42879(13) 0.3508(2) 0.38548(18) 0.0540(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0216(2) 0.0218(2) 0.0302(2) 0.000 -0.00047(14) 0.000 O1 0.0450(15) 0.0464(16) 0.0507(15) -0.0099(13) 0.0036(12) -0.0188(13) O2 0.0261(12) 0.0289(11) 0.0355(12) 0.0058(10) -0.0002(10) 0.0027(9) O3 0.0543(16) 0.0278(12) 0.0345(13) 0.0005(10) -0.0025(12) 0.0029(10) N1 0.0269(14) 0.0278(14) 0.0338(14) 0.0023(11) 0.0004(11) 0.0037(11) C1 0.0312(17) 0.0310(17) 0.0347(18) 0.0005(15) 0.0046(14) -0.0013(15) C2 0.0299(18) 0.0371(18) 0.0424(18) 0.0038(16) 0.0041(15) 0.0048(16) C3 0.0231(16) 0.0345(18) 0.044(2) 0.0051(14) -0.0010(14) 0.0065(14) C4 0.031(2) 0.054(3) 0.062(3) 0.020(2) -0.0058(18) 0.0006(18) C5 0.043(2) 0.034(2) 0.061(3) 0.0040(19) 0.0066(19) 0.0135(17) C6 0.072(3) 0.033(2) 0.049(2) 0.0094(17) -0.007(2) 0.0107(19) F1 0.0500(14) 0.0620(16) 0.0842(17) 0.0065(14) -0.0325(12) -0.0144(12) F2 0.0229(11) 0.107(2) 0.095(2) 0.0384(14) 0.0004(11) 0.0083(13) F3 0.0425(13) 0.0677(16) 0.0695(15) 0.0243(12) -0.0152(11) 0.0079(11) F4 0.0672(16) 0.0556(15) 0.0893(18) 0.0002(14) 0.0210(14) 0.0331(13) F5 0.0719(18) 0.0309(11) 0.0689(16) 0.0091(10) 0.0029(12) 0.0067(12) F6 0.0659(15) 0.0360(12) 0.0602(13) -0.0101(10) -0.0127(12) 0.0084(10)