data_rueg13 _audit_creation_date 02-21-11 _audit_creation_method CRYSTALS_ver_12-03-99 _publ_contact_author_name 'Patricia Lozano-Casal' _publ_contact_author_address _publ_contact_author_phone '0131 650 4804' _publ_contact_author_email 'P.Lozano-Casal@ed.ac.uk' _publ_section_exptl_refinement ; H atoms placed geometrically after each cycle ; _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 8.2584(12) _cell_angle_alpha 73.815(2) _cell_length_b 10.0531(15) _cell_angle_beta 81.537(2) _cell_length_c 10.5557(16) _cell_angle_gamma 81.787(2) _cell_volume 827.7(2) _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration '.' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Ru ' -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International_Tables_Vol_IV_Table_2.2B' 'I ' -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International_Tables_Vol_IV_Table_2.2B' _cell_formula_units_Z 2 _chemical_formula_sum ' C11 H18 F6 I1 N2 P1 Ru1 ' _chemical_formula_moiety ' C11 H18 F6 I1 N2 P1 Ru1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 551.21 _cell_measurement_reflns_used 2471 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' lath ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.06 _exptl_crystal_density_diffrn 2.212 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 528.000 _exptl_absorpt_coefficient_mu 2.964 # Sheldrick geometric definitions 0.70 0.32 _diffrn_measurement_device_type ; Bruker SMART ; _diffrn_radiation_monochromator graphite _computing_data_collection ; SMART (Siemens, 1993) ; _computing_data_reduction ; SAINT (Siemens ,1995) ; _computing_cell_refinement ; SAINT (Siemens ,1995) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Siemens, 1996) ; _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.32 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 6838 _reflns_number_total 3735 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 3735 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4228 _diffrn_reflns_theta_min 2.022 _diffrn_reflns_theta_max 28.578 _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 22.791 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -10 _reflns_limit_h_max 11 _reflns_limit_k_min -12 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _refine_diff_density_min -1.34 _refine_diff_density_max 1.73 _refine_ls_number_reflns 3729 _refine_ls_number_parameters 199 #_refine_ls_R_factor_ref 0.0674 _refine_ls_wR_factor_ref 0.1107 _refine_ls_goodness_of_fit_ref 0.8866 #_reflns_number_all 3735 _refine_ls_R_factor_all 0.0678 _refine_ls_wR_factor_all 0.1131 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 2698 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_gt 0.1057 _refine_ls_shift/su_max 0.000256 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = SHELXL 97 (Sheldrick, 1997) W = q / [Sigma^2(F*)+(P(1)p)^2+P(2)p+P(4)+P(5)Sin(theta) ] 0.556E-01 0.00 0.00 0.00 0.00 0.333 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Siemens Industrial Automation, Inc (1993) SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_attached_hydrogens Ru1 Ru 0.23683(6) 0.27454(5) 0.69054(5) 0.0189 1.0000 Uani . C81 C 0.2969(8) 0.4865(6) 0.6736(7) 0.0236 1.0000 Uani . C91 C 0.4227(8) 0.3884(7) 0.7332(7) 0.0239 1.0000 Uani . C71 C 0.5015(8) 0.2859(7) 0.6684(7) 0.0272 1.0000 Uani . C61 C 0.4546(9) 0.2843(8) 0.5464(7) 0.0319 1.0000 Uani . C51 C 0.3264(9) 0.3809(8) 0.4881(7) 0.0311 1.0000 Uani . C41 C 0.2453(9) 0.4830(7) 0.5524(7) 0.0300 1.0000 Uani . C11 C 0.4472(9) 0.4120(8) 0.8612(7) 0.0325 1.0000 Uani . C21 C 0.2899(9) 0.5036(8) 0.8957(7) 0.0342 1.0000 Uani . C31 C 0.2322(9) 0.5816(7) 0.7598(7) 0.0288 1.0000 Uani . N22 N 0.1435(7) 0.1152(6) 0.6325(5) 0.0238 1.0000 Uani . C22 C 0.1954(9) -0.0250(7) 0.7183(8) 0.0314 1.0000 Uani . C12 C 0.1664(9) -0.0138(7) 0.8584(7) 0.0271 1.0000 Uani . N12 N 0.2509(7) 0.1053(6) 0.8665(5) 0.0243 1.0000 Uani . I1 I -0.07622(5) 0.33736(5) 0.79348(4) 0.0267 1.0000 Uani . P1 P 0.2800(2) 0.12702(19) 0.24492(17) 0.0216 1.0000 Uani . F5 F 0.1371(5) 0.1926(5) 0.3384(4) 0.0406 1.0000 Uani . F6 F 0.3833(5) 0.0640(5) 0.3678(4) 0.0441 1.0000 Uani . F2 F 0.4206(5) 0.0652(5) 0.1502(5) 0.0424 1.0000 Uani . F4 F 0.3679(6) 0.2669(5) 0.2087(5) 0.0523 1.0000 Uani . F3 F 0.1733(6) 0.1936(5) 0.1223(4) 0.0465 1.0000 Uani . F1 F 0.1923(6) -0.0096(5) 0.2790(5) 0.0500 1.0000 Uani . H711 H 0.5899 0.2152 0.7096 0.0316 1.0000 Uiso . H611 H 0.5125 0.2138 0.4999 0.0392 1.0000 Uiso . H511 H 0.2931 0.3773 0.4019 0.0367 1.0000 Uiso . H411 H 0.1536 0.5511 0.5129 0.0351 1.0000 Uiso . H111 H 0.5470 0.4615 0.8512 0.0402 1.0000 Uiso . H112 H 0.4588 0.3218 0.9311 0.0402 1.0000 Uiso . H211 H 0.3148 0.5705 0.9430 0.0432 1.0000 Uiso . H212 H 0.2045 0.4449 0.9522 0.0432 1.0000 Uiso . H311 H 0.2791 0.6729 0.7245 0.0339 1.0000 Uiso . H312 H 0.1093 0.5977 0.7664 0.0339 1.0000 Uiso . H121 H 0.1972 0.1390 0.9448 0.0272 1.0000 Uiso . H122 H 0.3693 0.0723 0.8778 0.0272 1.0000 Uiso . H123 H 0.2124 -0.1022 0.9190 0.0310 1.0000 Uiso . H124 H 0.0456 0.0033 0.8851 0.0310 1.0000 Uiso . H221 H 0.0206 0.1311 0.6410 0.0279 1.0000 Uiso . H222 H 0.1869 0.1193 0.5381 0.0279 1.0000 Uiso . H223 H 0.3148 -0.0526 0.6943 0.0375 1.0000 Uiso . H224 H 0.1285 -0.0957 0.7074 0.0375 1.0000 Uiso . 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 Ru1 0.0199(3) 0.0168(3) 0.0191(3) -0.0029(2) 0.0024(2) -0.0072(2) C81 0.024(3) 0.009(3) 0.036(4) -0.002(3) 0.003(3) -0.008(3) C91 0.017(3) 0.019(3) 0.037(4) -0.005(3) -0.003(3) -0.010(3) C71 0.022(3) 0.021(3) 0.037(4) -0.004(3) 0.004(3) -0.009(3) C61 0.032(4) 0.031(4) 0.035(4) -0.018(3) 0.022(3) -0.019(3) C51 0.040(4) 0.031(4) 0.021(3) -0.000(3) 0.007(3) -0.023(3) C41 0.036(4) 0.023(4) 0.029(4) 0.006(3) -0.009(3) -0.016(3) C11 0.028(4) 0.038(4) 0.034(4) -0.012(3) -0.004(3) -0.009(3) C21 0.032(4) 0.042(5) 0.033(4) -0.018(4) -0.002(3) -0.006(4) C31 0.029(4) 0.017(3) 0.038(4) -0.005(3) 0.001(3) -0.006(3) N22 0.031(3) 0.019(3) 0.019(3) -0.002(2) 0.003(2) -0.008(2) C22 0.034(4) 0.013(3) 0.046(5) -0.009(3) 0.003(3) -0.007(3) C12 0.027(4) 0.020(3) 0.030(4) 0.001(3) -0.001(3) -0.008(3) N12 0.022(3) 0.025(3) 0.022(3) 0.001(2) 0.001(2) -0.004(2) I1 0.0201(2) 0.0257(3) 0.0318(3) -0.0058(2) 0.00250(18) -0.00282(19) P1 0.0194(8) 0.0272(9) 0.0199(8) -0.0085(7) -0.0003(6) -0.0059(7) F5 0.039(3) 0.050(3) 0.031(2) -0.016(2) 0.0020(19) 0.003(2) F6 0.033(2) 0.059(3) 0.033(2) -0.000(2) -0.0103(19) -0.000(2) F2 0.030(2) 0.050(3) 0.047(3) -0.020(2) 0.004(2) 0.001(2) F4 0.063(3) 0.037(3) 0.059(3) -0.013(2) 0.007(3) -0.026(3) F3 0.050(3) 0.057(3) 0.031(2) -0.015(2) -0.011(2) 0.011(2) F1 0.041(3) 0.032(3) 0.076(4) -0.011(2) -0.002(2) -0.014(2) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . C81 . 2.209(6) yes Ru1 . C91 . 2.204(6) yes Ru1 . C71 . 2.179(7) yes Ru1 . C61 . 2.172(7) yes Ru1 . C51 . 2.178(7) yes Ru1 . C41 . 2.198(7) yes Ru1 . N22 . 2.138(5) yes Ru1 . N12 . 2.145(5) yes Ru1 . I1 . 2.7116(7) yes C81 . C91 . 1.415(9) yes C81 . C41 . 1.417(9) yes C81 . C31 . 1.491(9) yes C91 . C71 . 1.42(1) yes C91 . C11 . 1.48(1) yes C71 . C61 . 1.40(1) yes C71 . H711 . 1.000 no C61 . C51 . 1.417(11) yes C61 . H611 . 1.000 no C51 . C41 . 1.422(11) yes C51 . H511 . 1.000 no C41 . H411 . 1.000 no C11 . C21 . 1.54(1) yes C11 . H111 . 1.000 no C11 . H112 . 1.000 no C21 . C31 . 1.54(1) yes C21 . H211 . 1.000 no C21 . H212 . 1.000 no C31 . H311 . 1.000 no C31 . H312 . 1.000 no N22 . C22 . 1.490(9) yes N22 . H221 . 1.000 no N22 . H222 . 1.000 no C22 . C12 . 1.50(1) yes C22 . H223 . 1.000 no C22 . H224 . 1.000 no C12 . N12 . 1.497(9) yes C12 . H123 . 1.000 no C12 . H124 . 1.000 no N12 . H121 . 1.000 no N12 . H122 . 1.000 no P1 . F5 . 1.612(4) yes P1 . F6 . 1.589(4) yes P1 . F2 . 1.592(5) yes P1 . F4 . 1.600(5) yes P1 . F3 . 1.607(4) yes P1 . F1 . 1.572(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C81 . Ru1 . C91 . 37.4(2) yes C81 . Ru1 . C71 . 67.8(2) yes C91 . Ru1 . C71 . 37.9(2) yes C81 . Ru1 . C61 . 79.7(3) yes C91 . Ru1 . C61 . 67.9(3) yes C71 . Ru1 . C61 . 37.6(3) yes C81 . Ru1 . C51 . 67.6(3) yes C91 . Ru1 . C51 . 80.8(3) yes C71 . Ru1 . C51 . 68.6(3) yes C61 . Ru1 . C51 . 38.0(3) yes C81 . Ru1 . C41 . 37.5(2) yes C91 . Ru1 . C41 . 68.3(3) yes C71 . Ru1 . C41 . 81.2(3) yes C61 . Ru1 . C41 . 68.4(3) yes C51 . Ru1 . C41 . 37.9(3) yes C81 . Ru1 . N22 . 156.8(2) yes C91 . Ru1 . N22 . 157.5(2) yes C71 . Ru1 . N22 . 119.9(2) yes C61 . Ru1 . N22 . 94.4(2) yes C51 . Ru1 . N22 . 93.9(2) yes C81 . Ru1 . N12 . 124.2(2) yes C91 . Ru1 . N12 . 95.8(2) yes C71 . Ru1 . N12 . 91.7(2) yes C61 . Ru1 . N12 . 115.1(3) yes C51 . Ru1 . N12 . 152.1(3) yes C81 . Ru1 . I1 . 91.07(17) yes C91 . Ru1 . I1 . 115.15(18) yes C71 . Ru1 . I1 . 152.58(19) yes C61 . Ru1 . I1 . 158.6(2) yes C51 . Ru1 . I1 . 120.6(2) yes C41 . Ru1 . N22 . 119.5(2) yes C41 . Ru1 . N12 . 161.7(2) yes N22 . Ru1 . N12 . 78.7(2) yes C41 . Ru1 . I1 . 92.5(2) yes N22 . Ru1 . I1 . 86.50(15) yes N12 . Ru1 . I1 . 86.01(15) yes Ru1 . C81 . C91 . 71.1(3) yes Ru1 . C81 . C41 . 70.8(4) yes C91 . C81 . C41 . 121.5(6) yes Ru1 . C81 . C31 . 129.3(5) yes C91 . C81 . C31 . 109.4(6) yes C41 . C81 . C31 . 129.0(6) yes Ru1 . C91 . C81 . 71.5(3) yes Ru1 . C91 . C71 . 70.1(4) yes C81 . C91 . C71 . 119.1(6) yes Ru1 . C91 . C11 . 129.0(5) yes C81 . C91 . C11 . 110.3(6) yes C71 . C91 . C11 . 130.5(6) yes Ru1 . C71 . C91 . 72.0(4) yes Ru1 . C71 . C61 . 70.9(4) yes C91 . C71 . C61 . 119.7(6) yes Ru1 . C71 . H711 . 129.242 no C91 . C71 . H711 . 120.158 no C61 . C71 . H711 . 120.132 no Ru1 . C61 . C71 . 71.5(4) yes Ru1 . C61 . C51 . 71.2(4) yes C71 . C61 . C51 . 121.1(6) yes Ru1 . C61 . H611 . 130.579 no C71 . C61 . H611 . 119.457 no C51 . C61 . H611 . 119.453 no Ru1 . C51 . C61 . 70.8(4) yes Ru1 . C51 . C41 . 71.8(4) yes C61 . C51 . C41 . 119.8(6) yes Ru1 . C51 . H511 . 129.806 no C61 . C51 . H511 . 120.076 no C41 . C51 . H511 . 120.096 no Ru1 . C41 . C81 . 71.7(4) yes Ru1 . C41 . C51 . 70.3(4) yes C81 . C41 . C51 . 118.7(6) yes Ru1 . C41 . H411 . 129.726 no C81 . C41 . H411 . 120.664 no C51 . C41 . H411 . 120.669 no C91 . C11 . C21 . 104.0(6) yes C91 . C11 . H111 . 110.800 no C21 . C11 . H111 . 110.813 no C91 . C11 . H112 . 110.815 no C21 . C11 . H112 . 110.821 no H111 . C11 . H112 . 109.473 no C11 . C21 . C31 . 103.9(6) yes C11 . C21 . H211 . 110.836 no C31 . C21 . H211 . 110.847 no C11 . C21 . H212 . 110.843 no C31 . C21 . H212 . 110.859 no H211 . C21 . H212 . 109.475 no C81 . C31 . C21 . 104.2(6) yes C81 . C31 . H311 . 110.776 no C21 . C31 . H311 . 110.782 no C81 . C31 . H312 . 110.784 no C21 . C31 . H312 . 110.776 no H311 . C31 . H312 . 109.478 no Ru1 . N22 . C22 . 110.7(4) yes Ru1 . N22 . H221 . 109.172 no C22 . N22 . H221 . 109.160 no Ru1 . N22 . H222 . 109.178 no C22 . N22 . H222 . 109.176 no H221 . N22 . H222 . 109.468 no N22 . C22 . C12 . 106.8(5) yes N22 . C22 . H223 . 110.140 no C12 . C22 . H223 . 110.154 no N22 . C22 . H224 . 110.148 no C12 . C22 . H224 . 110.157 no H223 . C22 . H224 . 109.457 no C22 . C12 . N12 . 108.4(5) yes C22 . C12 . H123 . 109.739 no N12 . C12 . H123 . 109.732 no C22 . C12 . H124 . 109.736 no N12 . C12 . H124 . 109.726 no H123 . C12 . H124 . 109.462 no Ru1 . N12 . C12 . 111.5(4) yes Ru1 . N12 . H121 . 108.964 no C12 . N12 . H121 . 108.970 no Ru1 . N12 . H122 . 108.960 no C12 . N12 . H122 . 108.962 no H121 . N12 . H122 . 109.458 no F5 . P1 . F6 . 89.9(2) yes F5 . P1 . F2 . 178.8(3) yes F6 . P1 . F2 . 91.0(3) yes F5 . P1 . F4 . 89.7(3) yes F6 . P1 . F4 . 89.9(3) yes F2 . P1 . F4 . 89.5(3) yes F5 . P1 . F3 . 88.9(2) yes F6 . P1 . F3 . 178.6(3) yes F2 . P1 . F3 . 90.2(2) yes F4 . P1 . F3 . 89.5(3) yes F5 . P1 . F1 . 90.3(3) yes F6 . P1 . F1 . 90.8(3) yes F2 . P1 . F1 . 90.5(3) yes F4 . P1 . F1 . 179.3(3) yes F3 . P1 . F1 . 89.8(3) yes