Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Charset: us-ascii X-Sun-Content-Lines: 1390 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Hirano, Toshiyuki' 'Mukaida, Masao' 'Nagao, Hirotaka' 'Oi, Takao' 'Ueda, Koji' _publ_contact_author_name ' Hirotaka Nagao' _publ_contact_author_address ; Department of Chemistry, Faculty of Science and Technology, Sophia University, Kioi-cho 7-1, Chiyoda-ku, Tokyo 102-8554, Japan ; _publ_contact_author_email ' h-nagao@hoffman.cc.sophia.ac.jp' _publ_contact_author_fax ' 81-3-3238-3361' _publ_contact_author_phone ' 81-3-3238-3448' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Reactions of [RuCl2(NO)(terpy)]+ (terpy = 2,2':6',2"-terpyridine) with Mono Anions Such as NO2-, Br- and N3-, and Structural Studies on Terpyridineruthenium Having Nitrosyl Ligand ; #------------------------------------------------------------------------------ data_[Ru(NO)Cl2(terpy)]PF6 _database_code_CSD 165247 _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' #------------------------------------------------------------------------------ _chemical_formula_sum 'C15 H11 Cl2 F6 N4 O P Ru ' _chemical_formula_weight 580.22 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 9.0749(4) _cell_length_b 16.4893(9) _cell_length_c 12.8905(6) _cell_angle_alpha 90 _cell_angle_beta 95.753(2) _cell_angle_gamma 90 _cell_volume 1919.2(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 18860 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 2.008 _exptl_crystal_F_000 1136.00 _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.850 #------------------------------------------------------------------------------ _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_number 17377 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9957 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9957 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ _reflns_number_total 4387 _reflns_number_gt 3379 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0471 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3379 _refine_ls_number_parameters 271 _refine_ls_goodness_of_fit_ref 1.276 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0003 _refine_diff_density_max 0.58 _refine_diff_density_min -0.96 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ru' 'Ru' -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.12757(3) 0.22707(2) 0.43647(2) 0.03224(8) Uani 1.00 d . . . Cl(1) Cl 0.2702(1) 0.16050(7) 0.57575(8) 0.0528(3) Uani 1.00 d . . . Cl(2) Cl -0.0040(1) 0.27915(6) 0.28439(8) 0.0507(3) Uani 1.00 d . . . P P -0.2608(1) 0.05158(7) 0.07693(9) 0.0531(3) Uani 1.00 d . . . F(1) F -0.1324(4) -0.0125(2) 0.0971(3) 0.094(1) Uani 1.00 d . . . F(2) F -0.3397(3) -0.0056(2) -0.0107(2) 0.086(1) Uani 1.00 d . . . F(3) F -0.3504(4) 0.0102(2) 0.1632(2) 0.092(1) Uani 1.00 d . . . F(4) F -0.1817(4) 0.1099(2) 0.1629(3) 0.091(1) Uani 1.00 d . . . F(5) F -0.1746(4) 0.0954(2) -0.0104(2) 0.088(1) Uani 1.00 d . . . F(6) F -0.3888(3) 0.1176(2) 0.0579(2) 0.0809(10) Uani 1.00 d . . . O O 0.1244(4) 0.3686(2) 0.5687(3) 0.068(1) Uani 1.00 d . . . N(1) N 0.1233(3) 0.3156(2) 0.5131(2) 0.0407(8) Uani 1.00 d . . . N(2) N -0.0676(3) 0.1706(2) 0.4698(2) 0.0373(7) Uani 1.00 d . . . N(3) N 0.1387(3) 0.1216(2) 0.3588(2) 0.0359(7) Uani 1.00 d . . . N(4) N 0.3227(3) 0.2427(2) 0.3679(2) 0.0372(7) Uani 1.00 d . . . C(1) C -0.0919(4) 0.0970(2) 0.4226(3) 0.0390(9) Uani 1.00 d . . . C(2) C -0.2230(5) 0.0550(2) 0.4309(3) 0.052(1) Uani 1.00 d . . . C(3) C -0.3285(5) 0.0892(3) 0.4869(4) 0.061(1) Uani 1.00 d . . . C(4) C -0.3047(5) 0.1632(3) 0.5344(3) 0.056(1) Uani 1.00 d . . . C(5) C -0.1719(4) 0.2027(2) 0.5243(3) 0.0448(10) Uani 1.00 d . . . C(6) C 0.0272(4) 0.0679(2) 0.3629(3) 0.0386(9) Uani 1.00 d . . . C(7) C 0.0349(5) -0.0054(2) 0.3108(3) 0.050(1) Uani 1.00 d . . . C(8) C 0.1539(5) -0.0210(2) 0.2569(3) 0.054(1) Uani 1.00 d . . . C(9) C 0.2670(5) 0.0349(2) 0.2543(3) 0.049(1) Uani 1.00 d . . . C(10) C 0.2568(4) 0.1083(2) 0.3074(3) 0.0398(9) Uani 1.00 d . . . C(11) C 0.3621(4) 0.1771(2) 0.3125(3) 0.0403(9) Uani 1.00 d . . . C(12) C 0.4924(5) 0.1755(3) 0.2671(3) 0.054(1) Uani 1.00 d . . . C(13) C 0.5857(5) 0.2420(3) 0.2773(4) 0.061(1) Uani 1.00 d . . . C(14) C 0.5447(5) 0.3085(3) 0.3320(4) 0.062(1) Uani 1.00 d . . . C(15) C 0.4115(5) 0.3072(3) 0.3762(3) 0.050(1) Uani 1.00 d . . . H(1) H -0.2395 0.0032 0.3971 0.0622 Uiso 1.00 calc . . . H(2) H -0.4201 0.0609 0.4932 0.0734 Uiso 1.00 calc . . . H(3) H -0.3773 0.1875 0.5748 0.0678 Uiso 1.00 calc . . . H(4) H -0.1533 0.2544 0.5572 0.0549 Uiso 1.00 calc . . . H(5) H -0.0434 -0.0445 0.3134 0.0597 Uiso 1.00 calc . . . H(6) H 0.1586 -0.0713 0.2187 0.0658 Uiso 1.00 calc . . . H(7) H 0.3520 0.0242 0.2162 0.0592 Uiso 1.00 calc . . . H(8) H 0.5186 0.1283 0.2291 0.0659 Uiso 1.00 calc . . . H(9) H 0.6776 0.2416 0.2460 0.0721 Uiso 1.00 calc . . . H(10) H 0.6075 0.3557 0.3387 0.0759 Uiso 1.00 calc . . . H(11) H 0.3822 0.3541 0.4146 0.0603 Uiso 1.00 calc . . . #------------------------------------------------------------------------------ loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru 0.0352(1) 0.0266(1) 0.0351(2) -0.0028(1) 0.00419(10) -0.0038(1) Cl(1) 0.0582(5) 0.0500(6) 0.0488(5) -0.0011(4) -0.0016(4) 0.0040(4) Cl(2) 0.0542(5) 0.0447(5) 0.0519(5) -0.0002(4) -0.0016(4) 0.0054(4) P 0.0576(6) 0.0506(6) 0.0507(6) 0.0053(5) 0.0030(5) -0.0050(5) F(1) 0.096(2) 0.085(2) 0.097(2) 0.040(2) -0.017(2) -0.017(2) F(2) 0.069(2) 0.107(2) 0.080(2) -0.003(2) 0.003(1) -0.038(2) F(3) 0.135(3) 0.070(2) 0.078(2) -0.001(2) 0.044(2) 0.008(2) F(4) 0.108(3) 0.078(2) 0.081(2) 0.002(2) -0.022(2) -0.027(2) F(5) 0.085(2) 0.098(2) 0.086(2) -0.007(2) 0.029(2) 0.005(2) F(6) 0.085(2) 0.092(2) 0.067(2) 0.038(2) 0.012(1) 0.010(2) O 0.086(2) 0.052(2) 0.066(2) -0.008(2) 0.011(2) -0.028(2) N(1) 0.048(2) 0.032(1) 0.043(2) -0.003(1) 0.006(1) -0.007(1) N(2) 0.039(1) 0.034(1) 0.039(1) -0.004(1) 0.005(1) 0.001(1) N(3) 0.044(2) 0.027(1) 0.036(1) 0.002(1) 0.002(1) -0.005(1) N(4) 0.035(1) 0.037(1) 0.040(2) -0.002(1) 0.006(1) -0.001(1) C(1) 0.046(2) 0.032(2) 0.038(2) -0.004(1) -0.001(1) 0.005(1) C(2) 0.050(2) 0.043(2) 0.061(2) -0.014(2) -0.004(2) 0.004(2) C(3) 0.050(2) 0.062(3) 0.071(3) -0.018(2) 0.004(2) 0.015(2) C(4) 0.047(2) 0.072(3) 0.052(2) -0.004(2) 0.014(2) 0.008(2) C(5) 0.042(2) 0.045(2) 0.048(2) 0.001(2) 0.009(2) 0.000(2) C(6) 0.047(2) 0.028(2) 0.039(2) -0.003(1) -0.006(1) 0.003(1) C(7) 0.060(2) 0.031(2) 0.057(2) -0.001(2) -0.007(2) -0.007(2) C(8) 0.074(3) 0.036(2) 0.051(2) 0.007(2) -0.004(2) -0.012(2) C(9) 0.059(2) 0.045(2) 0.043(2) 0.014(2) 0.003(2) -0.009(2) C(10) 0.049(2) 0.037(2) 0.033(2) 0.006(2) 0.001(1) -0.001(1) C(11) 0.041(2) 0.042(2) 0.038(2) 0.004(2) 0.005(1) 0.000(2) C(12) 0.052(2) 0.063(3) 0.048(2) 0.008(2) 0.015(2) 0.004(2) C(13) 0.044(2) 0.087(3) 0.053(2) -0.002(2) 0.011(2) 0.009(2) C(14) 0.052(2) 0.079(3) 0.057(3) -0.023(2) 0.007(2) 0.006(2) C(15) 0.048(2) 0.049(2) 0.053(2) -0.013(2) 0.006(2) -0.002(2) #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Cl(1) 2.375(1) . . yes Ru Cl(2) 2.353(1) . . yes Ru N(1) 1.765(3) . . yes Ru N(2) 2.083(3) . . yes Ru N(3) 2.015(3) . . yes Ru N(4) 2.073(3) . . yes P F(1) 1.576(3) . . no P F(2) 1.586(3) . . no P F(3) 1.595(3) . . no P F(4) 1.584(3) . . no P F(5) 1.605(3) . . no P F(6) 1.593(3) . . no O N(1) 1.129(4) . . yes N(2) C(1) 1.365(4) . . no N(2) C(5) 1.344(5) . . no N(3) C(6) 1.350(4) . . no N(3) C(10) 1.334(5) . . no N(4) C(11) 1.363(4) . . no N(4) C(15) 1.333(5) . . no C(1) C(2) 1.390(5) . . no C(1) C(6) 1.469(5) . . no C(2) C(3) 1.376(7) . . no C(3) C(4) 1.373(7) . . no C(4) C(5) 1.387(6) . . no C(6) C(7) 1.387(5) . . no C(7) C(8) 1.366(6) . . no C(8) C(9) 1.383(6) . . no C(9) C(10) 1.398(5) . . no C(10) C(11) 1.481(5) . . no C(11) C(12) 1.372(5) . . no C(12) C(13) 1.385(7) . . no C(13) C(14) 1.374(8) . . no C(14) C(15) 1.387(6) . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ru Cl(2) 172.43(4) . 1_555 1_555 no Cl(1) Ru N(1) 90.0(1) . 1_555 1_555 no Cl(1) Ru N(2) 92.74(8) . 1_555 1_555 no Cl(1) Ru N(3) 85.74(8) . 1_555 1_555 no Cl(1) Ru N(4) 87.44(9) . 1_555 1_555 no Cl(2) Ru N(1) 97.3(1) . 1_555 1_555 no Cl(2) Ru N(2) 87.94(8) . 1_555 1_555 no Cl(2) Ru N(3) 87.00(8) . 1_555 1_555 no Cl(2) Ru N(4) 89.06(9) . 1_555 1_555 no N(1) Ru N(2) 100.8(1) . 1_555 1_555 no N(1) Ru N(3) 175.6(1) . 1_555 1_555 no N(1) Ru N(4) 101.8(1) . 1_555 1_555 no N(2) Ru N(3) 78.6(1) . 1_555 1_555 no N(2) Ru N(4) 157.4(1) . 1_555 1_555 yes N(3) Ru N(4) 78.9(1) . 1_555 1_555 no F(1) P F(2) 89.5(2) . 1_555 1_555 no F(1) P F(3) 91.0(2) . 1_555 1_555 no F(1) P F(4) 90.9(2) . 1_555 1_555 no F(1) P F(5) 90.8(2) . 1_555 1_555 no F(1) P F(6) 178.9(2) . 1_555 1_555 no F(2) P F(3) 91.0(2) . 1_555 1_555 no F(2) P F(4) 179.0(2) . 1_555 1_555 no F(2) P F(5) 89.2(2) . 1_555 1_555 no F(2) P F(6) 91.6(2) . 1_555 1_555 no F(3) P F(4) 89.9(2) . 1_555 1_555 no F(3) P F(5) 178.2(2) . 1_555 1_555 no F(3) P F(6) 89.2(2) . 1_555 1_555 no F(4) P F(5) 89.9(2) . 1_555 1_555 no F(4) P F(6) 88.0(2) . 1_555 1_555 no F(5) P F(6) 89.1(2) . 1_555 1_555 no Ru N(1) O 174.6(3) . 1_555 1_555 yes Ru N(2) C(1) 114.1(2) . 1_555 1_555 no Ru N(2) C(5) 126.1(3) . 1_555 1_555 no C(1) N(2) C(5) 119.5(3) . 1_555 1_555 no Ru N(3) C(6) 118.2(2) . 1_555 1_555 no Ru N(3) C(10) 118.1(2) . 1_555 1_555 no C(6) N(3) C(10) 123.7(3) . 1_555 1_555 no Ru N(4) C(11) 113.9(2) . 1_555 1_555 no Ru N(4) C(15) 126.9(3) . 1_555 1_555 no C(11) N(4) C(15) 119.1(3) . 1_555 1_555 no N(2) C(1) C(2) 120.7(4) . 1_555 1_555 no N(2) C(1) C(6) 115.5(3) . 1_555 1_555 no C(2) C(1) C(6) 123.9(3) . 1_555 1_555 no C(1) C(2) C(3) 118.8(4) . 1_555 1_555 no C(2) C(3) C(4) 120.7(4) . 1_555 1_555 no C(3) C(4) C(5) 118.4(4) . 1_555 1_555 no N(2) C(5) C(4) 121.9(4) . 1_555 1_555 no N(3) C(6) C(1) 113.5(3) . 1_555 1_555 no N(3) C(6) C(7) 118.6(4) . 1_555 1_555 no C(1) C(6) C(7) 127.9(3) . 1_555 1_555 no C(6) C(7) C(8) 119.4(4) . 1_555 1_555 no C(7) C(8) C(9) 121.0(4) . 1_555 1_555 no C(8) C(9) C(10) 118.6(4) . 1_555 1_555 no N(3) C(10) C(9) 118.8(3) . 1_555 1_555 no N(3) C(10) C(11) 113.5(3) . 1_555 1_555 no C(9) C(10) C(11) 127.6(4) . 1_555 1_555 no N(4) C(11) C(10) 115.4(3) . 1_555 1_555 no N(4) C(11) C(12) 121.5(4) . 1_555 1_555 no C(10) C(11) C(12) 123.1(4) . 1_555 1_555 no C(11) C(12) C(13) 119.3(4) . 1_555 1_555 no C(12) C(13) C(14) 119.1(4) . 1_555 1_555 no C(13) C(14) C(15) 119.4(4) . 1_555 1_555 no N(4) C(15) C(14) 121.6(4) . 1_555 1_555 no #===END #------------------------------------------------------------------------------ data_[Ru(OH)(NO2)(NO)(trpy)]PF6 _database_code_CSD 165248 _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' #------------------------------------------------------------------------------ _chemical_formula_sum 'C15 H12 F6 N5 O4 P Ru ' _chemical_formula_weight 572.33 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 9.7439(5) _cell_length_b 13.9922(8) _cell_length_c 14.654(1) _cell_angle_alpha 90 _cell_angle_beta 106.286(2) _cell_angle_gamma 90 _cell_volume 1917.7(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 22276 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.982 _exptl_crystal_F_000 1128.00 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.546 _exptl_absorpt_correction_T_max 0.820 #------------------------------------------------------------------------------ _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_reflns_number 14814 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9914 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9914 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ _reflns_number_total 4365 _reflns_number_gt 3657 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.0957 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3657 _refine_ls_number_parameters 289 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00706|Fo|^2^]' _refine_ls_shift/su_max 0.0023 _refine_diff_density_max 0.74 _refine_diff_density_min -1.88 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ru' 'Ru' -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru -0.01163(3) 0.20407(2) 0.11204(2) 0.0382(1) Uani 1.00 d . . . P P -0.5219(2) 0.18864(10) 0.4049(1) 0.0508(3) Uani 1.00 d . . . F(1) F -0.6016(5) 0.2588(3) 0.3215(3) 0.083(1) Uani 1.00 d . . . F(2) F -0.6744(6) 0.1426(4) 0.3976(4) 0.115(2) Uani 1.00 d . . . F(3) F -0.5009(7) 0.1158(4) 0.3278(3) 0.123(2) Uani 1.00 d . . . F(4) F -0.3768(7) 0.2381(7) 0.4144(6) 0.147(3) Uani 1.00 d . . . F(5) F -0.5489(5) 0.2590(3) 0.4833(3) 0.093(1) Uani 1.00 d . . . F(6) F -0.4464(6) 0.1160(4) 0.4855(3) 0.113(2) Uani 1.00 d . . . O(1) O -0.0944(7) 0.2043(3) -0.0941(3) 0.079(2) Uani 1.00 d . . . O(2) O 0.1455(9) 0.0275(5) 0.0967(6) 0.135(3) Uani 1.00 d . . . O(3) O 0.2665(9) 0.1495(7) 0.1061(9) 0.183(5) Uani 1.00 d . . . O(4) O 0.0616(5) 0.1981(3) 0.2495(3) 0.053(1) Uani 1.00 d . . . N(1) N -0.0707(5) 0.2060(2) -0.0138(3) 0.046(1) Uani 1.00 d . . . N(2) N 0.1722(4) 0.1102(2) 0.1066(3) 0.0376(9) Uani 1.00 d . . . N(3) N -0.1612(5) 0.1006(3) 0.1253(3) 0.048(1) Uani 1.00 d . . . N(4) N -0.1601(5) 0.2880(3) 0.1419(3) 0.044(1) Uani 1.00 d . . . N(5) N 0.0847(4) 0.3391(3) 0.1154(3) 0.0450(10) Uani 1.00 d . . . C(1) C -0.2802(5) 0.1405(4) 0.1414(3) 0.050(1) Uani 1.00 d . . . C(2) C -0.3944(6) 0.0865(5) 0.1439(4) 0.065(2) Uani 1.00 d . . . C(3) C -0.3865(9) -0.0165(6) 0.1289(5) 0.088(2) Uani 1.00 d . . . C(4) C -0.2682(9) -0.0537(4) 0.1137(5) 0.077(2) Uani 1.00 d . . . C(5) C -0.1570(7) 0.0064(4) 0.1115(4) 0.061(2) Uani 1.00 d . . . C(6) C -0.2704(5) 0.2436(3) 0.1606(3) 0.044(1) Uani 1.00 d . . . C(7) C -0.3656(7) 0.3004(4) 0.1942(4) 0.058(2) Uani 1.00 d . . . C(8) C -0.3370(7) 0.3945(5) 0.2083(4) 0.073(2) Uani 1.00 d . . . C(9) C -0.2170(7) 0.4384(4) 0.1921(4) 0.060(1) Uani 1.00 d . . . C(10) C -0.1275(6) 0.3805(3) 0.1577(3) 0.047(1) Uani 1.00 d . . . C(11) C 0.0064(5) 0.4124(3) 0.1385(3) 0.046(1) Uani 1.00 d . . . C(12) C 0.0495(7) 0.5050(3) 0.1384(4) 0.057(1) Uani 1.00 d . . . C(13) C 0.1747(8) 0.5291(4) 0.1169(5) 0.070(2) Uani 1.00 d . . . C(14) C 0.2518(6) 0.4549(5) 0.0927(5) 0.065(2) Uani 1.00 d . . . C(15) C 0.2055(6) 0.3608(4) 0.0931(4) 0.057(1) Uani 1.00 d . . . H(1) H -0.4812 0.1156 0.1549 0.0806 Uiso 1.00 calc . . . H(2) H -0.4666 -0.0576 0.1288 0.1012 Uiso 1.00 calc . . . H(3) H -0.2603 -0.1206 0.1058 0.0914 Uiso 1.00 calc . . . H(4) H -0.0743 -0.0202 0.0977 0.0728 Uiso 1.00 calc . . . H(5) H -0.4478 0.2727 0.2072 0.0684 Uiso 1.00 calc . . . H(6) H -0.4008 0.4347 0.2301 0.0809 Uiso 1.00 calc . . . H(7) H -0.1978 0.5052 0.2034 0.0711 Uiso 1.00 calc . . . H(8) H -0.0067 0.5547 0.1558 0.0699 Uiso 1.00 calc . . . H(9) H 0.2027 0.5948 0.1161 0.0839 Uiso 1.00 calc . . . H(10) H 0.3397 0.4676 0.0772 0.0778 Uiso 1.00 calc . . . H(11) H 0.2599 0.3105 0.0761 0.0657 Uiso 1.00 calc . . . #------------------------------------------------------------------------------ loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru 0.0323(3) 0.0411(3) 0.0422(3) -0.0018(1) 0.0122(2) 0.0002(1) P 0.0465(7) 0.0492(6) 0.0556(7) 0.0105(5) 0.0126(6) -0.0023(5) F(1) 0.095(3) 0.071(2) 0.079(3) 0.023(2) 0.019(2) 0.016(2) F(2) 0.085(3) 0.138(5) 0.125(4) -0.040(3) 0.037(3) -0.008(3) F(3) 0.160(5) 0.133(4) 0.066(2) 0.077(4) 0.016(3) -0.026(2) F(4) 0.078(4) 0.196(6) 0.169(7) -0.043(4) 0.040(4) 0.004(5) F(5) 0.104(3) 0.092(3) 0.074(2) 0.027(3) 0.011(2) -0.018(2) F(6) 0.166(5) 0.100(3) 0.060(2) 0.071(3) 0.010(3) 0.010(2) O(1) 0.086(4) 0.108(4) 0.043(2) 0.005(2) 0.019(2) 0.003(2) O(2) 0.124(6) 0.087(4) 0.214(10) 0.037(4) 0.081(6) 0.016(4) O(3) 0.099(6) 0.137(7) 0.34(2) 0.018(5) 0.104(8) -0.032(7) O(4) 0.044(2) 0.070(2) 0.045(2) -0.004(1) 0.012(2) 0.001(1) N(1) 0.043(2) 0.047(2) 0.047(2) 0.002(1) 0.012(2) 0.003(1) N(2) 0.040(2) 0.035(2) 0.042(2) 0.002(1) 0.019(1) 0.001(1) N(3) 0.049(2) 0.044(2) 0.051(2) -0.011(2) 0.015(2) -0.003(2) N(4) 0.038(2) 0.051(2) 0.044(2) 0.004(2) 0.011(2) 0.000(1) N(5) 0.040(2) 0.046(2) 0.048(2) -0.003(2) 0.011(2) 0.000(2) C(1) 0.041(2) 0.064(3) 0.045(2) -0.011(2) 0.011(2) 0.007(2) C(2) 0.049(3) 0.092(4) 0.057(3) -0.014(3) 0.020(2) 0.009(3) C(3) 0.093(5) 0.099(5) 0.076(4) -0.052(4) 0.028(4) 0.001(4) C(4) 0.104(5) 0.055(3) 0.086(4) -0.031(3) 0.047(4) -0.012(3) C(5) 0.074(4) 0.045(2) 0.069(3) -0.010(3) 0.026(3) -0.004(2) C(6) 0.033(2) 0.054(2) 0.044(2) 0.001(2) 0.009(2) 0.004(2) C(7) 0.046(3) 0.074(4) 0.057(3) 0.010(2) 0.021(2) 0.002(2) C(8) 0.065(4) 0.099(5) 0.060(3) 0.038(3) 0.028(3) 0.008(3) C(9) 0.064(3) 0.061(3) 0.055(3) 0.019(3) 0.015(2) -0.002(2) C(10) 0.051(3) 0.042(2) 0.049(2) 0.009(2) 0.015(2) 0.002(2) C(11) 0.050(2) 0.038(2) 0.045(2) -0.003(2) 0.006(2) -0.001(2) C(12) 0.068(3) 0.041(2) 0.061(3) -0.003(2) 0.014(2) -0.009(2) C(13) 0.077(4) 0.053(3) 0.074(4) -0.020(3) 0.009(3) -0.002(3) C(14) 0.049(3) 0.073(4) 0.076(4) -0.022(3) 0.023(3) -0.007(3) C(15) 0.046(3) 0.062(3) 0.065(3) -0.014(2) 0.019(2) -0.009(2) #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru O(4) 1.941(4) . . yes Ru N(1) 1.771(5) . . yes Ru N(2) 2.241(4) . . yes Ru N(3) 2.102(4) . . yes Ru N(4) 2.005(5) . . yes Ru N(5) 2.104(4) . . yes P F(1) 1.590(4) . . no P F(2) 1.595(6) . . no P F(3) 1.577(6) . . no P F(4) 1.545(8) . . no P F(5) 1.590(5) . . no P F(6) 1.577(5) . . no O(1) N(1) 1.134(7) . . yes O(2) N(2) 1.186(7) . . no O(3) N(2) 1.07(1) . . no N(3) C(1) 1.366(7) . . no N(3) C(5) 1.336(7) . . no N(4) C(6) 1.335(7) . . no N(4) C(10) 1.337(6) . . no N(5) C(11) 1.376(7) . . no N(5) C(15) 1.342(8) . . no C(1) C(2) 1.353(8) . . no C(1) C(6) 1.468(7) . . no C(2) C(3) 1.46(1) . . no C(3) C(4) 1.34(1) . . no C(4) C(5) 1.38(1) . . no C(6) C(7) 1.412(9) . . no C(7) C(8) 1.350(9) . . no C(8) C(9) 1.399(10) . . no C(9) C(10) 1.384(9) . . no C(10) C(11) 1.479(8) . . no C(11) C(12) 1.361(7) . . no C(12) C(13) 1.39(1) . . no C(13) C(14) 1.385(10) . . no C(14) C(15) 1.393(9) . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(4) Ru N(1) 177.0(2) . 1_555 1_555 no O(4) Ru N(2) 87.0(2) . 1_555 1_555 no O(4) Ru N(3) 86.4(2) . 1_555 1_555 no O(4) Ru N(4) 82.9(2) . 1_555 1_555 no O(4) Ru N(5) 89.0(2) . 1_555 1_555 no N(1) Ru N(2) 90.1(2) . 1_555 1_555 no N(1) Ru N(3) 94.4(2) . 1_555 1_555 no N(1) Ru N(4) 100.1(2) . 1_555 1_555 no N(1) Ru N(5) 91.3(2) . 1_555 1_555 no N(2) Ru N(3) 100.5(2) . 1_555 1_555 no N(2) Ru N(4) 169.8(1) . 1_555 1_555 no N(2) Ru N(5) 99.9(1) . 1_555 1_555 no N(3) Ru N(4) 79.7(2) . 1_555 1_555 no N(3) Ru N(5) 158.9(2) . 1_555 1_555 yes N(4) Ru N(5) 79.2(2) . 1_555 1_555 no F(1) P F(2) 87.3(3) . 1_555 1_555 no F(1) P F(3) 89.0(3) . 1_555 1_555 no F(1) P F(4) 91.7(4) . 1_555 1_555 no F(1) P F(5) 91.6(2) . 1_555 1_555 no F(1) P F(6) 177.9(2) . 1_555 1_555 no F(2) P F(3) 89.8(3) . 1_555 1_555 no F(2) P F(4) 176.9(4) . 1_555 1_555 no F(2) P F(5) 87.6(3) . 1_555 1_555 no F(2) P F(6) 91.1(3) . 1_555 1_555 no F(3) P F(4) 93.1(4) . 1_555 1_555 no F(3) P F(5) 177.4(3) . 1_555 1_555 no F(3) P F(6) 89.6(3) . 1_555 1_555 no F(4) P F(5) 89.4(4) . 1_555 1_555 no F(4) P F(6) 89.9(4) . 1_555 1_555 no F(5) P F(6) 89.7(3) . 1_555 1_555 no Ru N(1) O(1) 172.8(5) . 1_555 1_555 yes Ru N(2) O(2) 115.2(5) . 1_555 1_555 no Ru N(2) O(3) 113.2(6) . 1_555 1_555 no O(2) N(2) O(3) 131.2(8) . 1_555 1_555 yes Ru N(3) C(1) 112.3(3) . 1_555 1_555 no Ru N(3) C(5) 127.9(4) . 1_555 1_555 no C(1) N(3) C(5) 119.5(5) . 1_555 1_555 no Ru N(4) C(6) 116.3(3) . 1_555 1_555 no Ru N(4) C(10) 117.0(4) . 1_555 1_555 no C(6) N(4) C(10) 125.6(5) . 1_555 1_555 no Ru N(5) C(11) 113.7(3) . 1_555 1_555 no Ru N(5) C(15) 127.8(4) . 1_555 1_555 no C(11) N(5) C(15) 118.4(4) . 1_555 1_555 no N(3) C(1) C(2) 121.4(5) . 1_555 1_555 no N(3) C(1) C(6) 114.9(4) . 1_555 1_555 no C(2) C(1) C(6) 123.6(5) . 1_555 1_555 no C(1) C(2) C(3) 117.8(6) . 1_555 1_555 no C(2) C(3) C(4) 119.5(7) . 1_555 1_555 no C(3) C(4) C(5) 119.0(6) . 1_555 1_555 no N(3) C(5) C(4) 122.8(7) . 1_555 1_555 no N(4) C(6) C(1) 115.6(5) . 1_555 1_555 no N(4) C(6) C(7) 117.0(5) . 1_555 1_555 no C(1) C(6) C(7) 127.4(5) . 1_555 1_555 no C(6) C(7) C(8) 118.4(6) . 1_555 1_555 no C(7) C(8) C(9) 123.2(7) . 1_555 1_555 no C(8) C(9) C(10) 116.6(5) . 1_555 1_555 no N(4) C(10) C(9) 119.1(5) . 1_555 1_555 no N(4) C(10) C(11) 116.1(5) . 1_555 1_555 no C(9) C(10) C(11) 124.9(4) . 1_555 1_555 no N(5) C(11) C(10) 113.6(4) . 1_555 1_555 no N(5) C(11) C(12) 121.1(5) . 1_555 1_555 no C(10) C(11) C(12) 125.2(5) . 1_555 1_555 no C(11) C(12) C(13) 121.6(5) . 1_555 1_555 no C(12) C(13) C(14) 116.8(5) . 1_555 1_555 no C(13) C(14) C(15) 120.6(6) . 1_555 1_555 no N(5) C(15) C(14) 121.5(6) . 1_555 1_555 no #===END #------------------------------------------------------------------------------ data_[RuCl(OCH3)(NO)(terpy)]PF6 _database_code_CSD 165249 _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' #------------------------------------------------------------------------------ _chemical_formula_sum 'C16 H15 Cl F6 N4 O2.50 P Ru ' _chemical_formula_weight 584.81 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/n 1' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,-y,1/2+z -x,-y,-z 1/2-x,y,1/2-z _cell_length_a 10.254(2) _cell_length_b 8.545(2) _cell_length_c 24.593(2) _cell_angle_alpha 90 _cell_angle_beta 96.93(1) _cell_angle_gamma 90 _cell_volume 2139.1(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.816 _exptl_crystal_F_000 1156.00 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochrometor 'graphite' _diffrn_reflns_number 10001 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9988 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 #------------------------------------------------------------------------------ _reflns_number_total 4907 _reflns_number_gt 3728 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0603 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3728 _refine_ls_number_parameters 288 _refine_ls_goodness_of_fit_ref 1.970 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00038|Fo|^2^]' _refine_ls_shift/su_max 0.0116 _refine_diff_density_max 0.47 _refine_diff_density_min -0.79 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ru' 'Ru' -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.19839(3) 0.12134(4) 0.40307(1) 0.03600(9) Uani 1.00 d . . . Cl Cl 0.1178(1) -0.1233(1) 0.43199(6) 0.0602(4) Uani 1.00 d . . . P(1) P 0.0000 -0.5000 0.0000 0.0439(4) Uani 1.00 d S . . P(2) P -0.2500 -0.4291(3) 0.2500 0.0603(6) Uani 1.00 d S . . F(1) F -0.0300(4) -0.4359(5) 0.0576(1) 0.081(1) Uani 1.00 d . . . F(2) F -0.0191(3) -0.6744(4) 0.0208(2) 0.077(1) Uani 1.00 d . . . F(3) F 0.1523(3) -0.5122(4) 0.0217(1) 0.0684(10) Uani 1.00 d . . . F(4) F -0.2861(5) -0.423(1) 0.3079(2) 0.213(3) Uani 1.00 d . . . F(5) F -0.1036(5) -0.429(1) 0.2685(2) 0.211(3) Uani 1.00 d . . . F(6) F -0.2500 -0.590(1) 0.2500 0.37(1) Uani 1.00 d S . . F(7) F -0.2500 -0.262(2) 0.2500 0.39(1) Uani 1.00 d S . . O(1) O 0.2818(5) 0.1569(5) 0.5180(2) 0.088(2) Uani 1.00 d . . . O(2) O 0.1239(3) 0.0741(4) 0.3286(1) 0.0473(9) Uani 1.00 d . . . O(3) O 0.7500 0.0888(6) 0.7500 0.063(2) Uani 1.00 d S . . N(1) N 0.2600(4) 0.1519(5) 0.4719(2) 0.050(1) Uani 1.00 d . . . N(2) N 0.3773(3) 0.0493(4) 0.3789(1) 0.0401(10) Uani 1.00 d . . . N(3) N 0.2546(3) 0.3184(4) 0.3703(1) 0.0384(9) Uani 1.00 d . . . N(4) N 0.0365(4) 0.2611(4) 0.4114(1) 0.0433(10) Uani 1.00 d . . . C(1) C -0.0099(6) 0.0372(9) 0.3130(2) 0.073(2) Uani 1.00 d . . . C(2) C 0.4380(4) 0.1678(6) 0.3535(2) 0.044(1) Uani 1.00 d . . . C(3) C 0.5579(5) 0.1400(7) 0.3348(2) 0.058(2) Uani 1.00 d . . . C(4) C 0.6153(5) -0.0074(8) 0.3407(2) 0.063(2) Uani 1.00 d . . . C(5) C 0.5527(5) -0.1233(7) 0.3656(2) 0.059(2) Uani 1.00 d . . . C(6) C 0.4343(5) -0.0907(6) 0.3851(2) 0.049(1) Uani 1.00 d . . . C(7) C 0.3669(4) 0.3165(6) 0.3471(2) 0.044(1) Uani 1.00 d . . . C(8) C 0.3996(5) 0.4484(6) 0.3185(2) 0.050(1) Uani 1.00 d . . . C(9) C 0.3173(5) 0.5760(6) 0.3155(2) 0.053(1) Uani 1.00 d . . . C(10) C 0.2004(5) 0.5733(6) 0.3389(2) 0.050(1) Uani 1.00 d . . . C(11) C 0.1688(4) 0.4396(5) 0.3659(2) 0.041(1) Uani 1.00 d . . . C(12) C 0.0489(5) 0.4095(5) 0.3924(2) 0.044(1) Uani 1.00 d . . . C(13) C -0.0456(5) 0.5216(6) 0.3973(2) 0.056(1) Uani 1.00 d . . . C(14) C -0.1554(5) 0.4809(7) 0.4220(2) 0.068(2) Uani 1.00 d . . . C(15) C -0.1668(6) 0.3302(7) 0.4417(2) 0.069(2) Uani 1.00 d . . . C(16) C -0.0700(5) 0.2248(6) 0.4359(2) 0.057(2) Uani 1.00 d . . . H(1) H -0.0639 0.1218 0.3219 0.0881 Uiso 1.00 calc . . . H(2) H -0.0250 0.0178 0.2747 0.0881 Uiso 1.00 calc . . . H(3) H -0.0329 -0.0542 0.3321 0.0881 Uiso 1.00 calc . . . H(4) H 0.6012 0.2237 0.3175 0.0692 Uiso 1.00 calc . . . H(5) H 0.6979 -0.0279 0.3271 0.0755 Uiso 1.00 calc . . . H(6) H 0.5897 -0.2273 0.3691 0.0709 Uiso 1.00 calc . . . H(7) H 0.3913 -0.1711 0.4043 0.0594 Uiso 1.00 calc . . . H(8) H 0.4775 0.4503 0.3007 0.0606 Uiso 1.00 calc . . . H(9) H 0.3417 0.6688 0.2971 0.0620 Uiso 1.00 calc . . . H(10) H 0.1426 0.6636 0.3362 0.0606 Uiso 1.00 calc . . . H(11) H -0.0371 0.6248 0.3832 0.0677 Uiso 1.00 calc . . . H(12) H -0.2221 0.5571 0.4261 0.0807 Uiso 1.00 calc . . . H(13) H -0.2414 0.3000 0.4597 0.0790 Uiso 1.00 calc . . . H(14) H -0.0784 0.1202 0.4500 0.0697 Uiso 1.00 calc . . . #------------------------------------------------------------------------------ loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru 0.0425(2) 0.0348(2) 0.0319(2) -0.0028(2) 0.0094(1) -0.0011(1) Cl 0.0797(9) 0.0438(6) 0.0609(7) -0.0111(6) 0.0235(6) 0.0013(6) P(1) 0.0422(8) 0.0479(9) 0.0424(9) 0.0018(7) 0.0084(7) 0.0072(7) P(2) 0.049(1) 0.077(1) 0.057(1) 0.0000 0.0164(9) 0.0000 F(1) 0.092(2) 0.102(3) 0.053(2) 0.008(2) 0.023(2) -0.012(2) F(2) 0.068(2) 0.056(2) 0.110(3) 0.002(2) 0.020(2) 0.025(2) F(3) 0.045(2) 0.084(2) 0.075(2) 0.002(2) 0.000(1) 0.020(2) F(4) 0.091(3) 0.48(1) 0.073(3) 0.050(6) 0.022(2) -0.019(5) F(5) 0.068(3) 0.47(1) 0.100(4) 0.023(5) 0.015(3) -0.044(6) F(6) 0.42(2) 0.061(6) 0.68(4) 0.0000 0.22(2) 0.0000 F(7) 0.36(2) 0.14(1) 0.72(3) 0.0000 0.32(2) 0.0000 O(1) 0.131(4) 0.093(3) 0.036(2) -0.032(3) -0.003(2) 0.002(2) O(2) 0.047(2) 0.059(2) 0.037(2) -0.007(2) 0.010(1) -0.008(1) O(3) 0.092(4) 0.045(3) 0.055(3) 0.0000 0.025(3) 0.0000 N(1) 0.065(3) 0.046(2) 0.039(2) -0.012(2) 0.007(2) 0.001(2) N(2) 0.042(2) 0.042(2) 0.036(2) 0.000(2) 0.006(1) -0.005(2) N(3) 0.044(2) 0.039(2) 0.033(2) -0.004(2) 0.009(1) -0.002(2) N(4) 0.049(2) 0.045(2) 0.039(2) 0.000(2) 0.016(2) 0.000(2) C(1) 0.057(3) 0.106(5) 0.058(3) -0.012(3) 0.006(3) -0.013(3) C(2) 0.043(2) 0.051(3) 0.039(2) -0.005(2) 0.007(2) -0.001(2) C(3) 0.045(3) 0.070(4) 0.062(3) -0.005(3) 0.015(2) -0.002(3) C(4) 0.044(3) 0.081(4) 0.064(3) 0.012(3) 0.010(2) -0.006(3) C(5) 0.053(3) 0.065(3) 0.058(3) 0.018(3) 0.001(2) -0.004(3) C(6) 0.050(3) 0.048(3) 0.047(3) 0.004(2) 0.000(2) -0.002(2) C(7) 0.046(2) 0.047(2) 0.039(2) -0.008(2) 0.010(2) -0.001(2) C(8) 0.053(3) 0.054(3) 0.045(3) -0.012(2) 0.010(2) 0.005(2) C(9) 0.071(3) 0.048(3) 0.039(2) -0.017(2) 0.005(2) 0.008(2) C(10) 0.067(3) 0.042(2) 0.041(2) 0.000(2) 0.007(2) 0.004(2) C(11) 0.051(2) 0.037(2) 0.034(2) -0.002(2) 0.006(2) -0.002(2) C(12) 0.051(3) 0.042(2) 0.039(2) 0.002(2) 0.007(2) -0.005(2) C(13) 0.065(3) 0.046(3) 0.058(3) 0.010(2) 0.009(2) -0.002(2) C(14) 0.061(3) 0.075(4) 0.071(4) 0.022(3) 0.021(3) 0.000(3) C(15) 0.065(3) 0.075(4) 0.074(4) 0.011(3) 0.037(3) 0.006(3) C(16) 0.062(3) 0.058(3) 0.058(3) 0.005(2) 0.031(2) 0.009(2) #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Cl 2.387(1) . . yes Ru O(2) 1.940(3) . . yes Ru N(1) 1.753(4) . . yes Ru N(2) 2.087(4) . . yes Ru N(3) 1.982(4) . . yes Ru N(4) 2.075(4) . . yes P(1) F(1) 1.583(3) . . no P(1) F(1) 1.583(3) . 3_545 no P(1) F(2) 1.595(3) . . no P(1) F(2) 1.595(3) . 3_545 no P(1) F(3) 1.592(3) . . no P(1) F(3) 1.592(3) . 3_545 no P(2) F(4) 1.515(5) . . no P(2) F(4) 1.515(5) . 4_455 no P(2) F(5) 1.515(5) . . no P(2) F(5) 1.515(5) . 4_455 no P(2) F(6) 1.374(10) . . no P(2) F(7) 1.43(1) . . no O(1) N(1) 1.129(5) . . yes O(2) C(1) 1.416(6) . . no N(2) C(2) 1.378(6) . . no N(2) C(6) 1.332(6) . . no N(3) C(7) 1.345(5) . . no N(3) C(11) 1.355(6) . . no N(4) C(12) 1.364(6) . . no N(4) C(16) 1.344(6) . . no C(2) C(3) 1.383(7) . . no C(2) C(7) 1.464(7) . . no C(3) C(4) 1.390(8) . . no C(4) C(5) 1.365(8) . . no C(5) C(6) 1.387(7) . . no C(7) C(8) 1.391(7) . . no C(8) C(9) 1.375(7) . . no C(9) C(10) 1.392(7) . . no C(10) C(11) 1.380(6) . . no C(11) C(12) 1.481(6) . . no C(12) C(13) 1.378(7) . . no C(13) C(14) 1.386(7) . . no C(14) C(15) 1.386(8) . . no C(15) C(16) 1.361(7) . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Ru O(2) 89.3(1) . 1_555 1_555 no Cl Ru N(1) 86.6(1) . 1_555 1_555 no Cl Ru N(2) 100.0(1) . 1_555 1_555 no Cl Ru N(3) 173.2(1) . 1_555 1_555 no Cl Ru N(4) 99.5(1) . 1_555 1_555 no O(2) Ru N(1) 175.9(2) . 1_555 1_555 no O(2) Ru N(2) 86.0(1) . 1_555 1_555 no O(2) Ru N(3) 83.9(1) . 1_555 1_555 no O(2) Ru N(4) 89.1(1) . 1_555 1_555 no N(1) Ru N(2) 95.2(2) . 1_555 1_555 no N(1) Ru N(3) 100.2(2) . 1_555 1_555 no N(1) Ru N(4) 91.0(2) . 1_555 1_555 no N(2) Ru N(3) 80.0(1) . 1_555 1_555 no N(2) Ru N(4) 159.8(1) . 1_555 1_555 yes N(3) Ru N(4) 80.0(1) . 1_555 1_555 no F(1) P(1) F(1) 180.0 . 1_555 3_545 no F(1) P(1) F(2) 89.5(2) . 1_555 1_555 no F(1) P(1) F(2) 90.5(2) . 1_555 3_545 no F(1) P(1) F(3) 90.7(2) . 1_555 1_555 no F(1) P(1) F(3) 89.3(2) . 1_555 3_545 no F(1) P(1) F(2) 90.5(2) . 3_545 1_555 no F(1) P(1) F(2) 89.5(2) . 3_545 3_545 no F(1) P(1) F(3) 89.3(2) . 3_545 1_555 no F(1) P(1) F(3) 90.7(2) . 3_545 3_545 no F(2) P(1) F(2) 180.0 . 1_555 3_545 no F(2) P(1) F(3) 89.1(2) . 1_555 1_555 no F(2) P(1) F(3) 90.9(2) . 1_555 3_545 no F(2) P(1) F(3) 90.9(2) . 3_545 1_555 no F(2) P(1) F(3) 89.1(2) . 3_545 3_545 no F(3) P(1) F(3) 180.0 . 1_555 3_545 no F(4) P(2) F(4) 176.2(8) . 1_555 4_455 no F(4) P(2) F(5) 93.6(3) . 1_555 1_555 no F(4) P(2) F(5) 86.4(3) . 1_555 4_455 no F(4) P(2) F(6) 91.9(4) . 1_555 1_555 no F(4) P(2) F(7) 88.1(4) . 1_555 1_555 no F(4) P(2) F(5) 86.4(3) . 4_455 1_555 no F(4) P(2) F(5) 93.6(3) . 4_455 4_455 no F(4) P(2) F(6) 91.9(4) . 4_455 1_555 no F(4) P(2) F(7) 88.1(4) . 4_455 1_555 no F(5) P(2) F(5) 180.0(8) . 1_555 4_455 no F(5) P(2) F(6) 90.0(4) . 1_555 1_555 no F(5) P(2) F(7) 90.0(4) . 1_555 1_555 no F(5) P(2) F(6) 90.0(4) . 4_455 1_555 no F(5) P(2) F(7) 90.0(4) . 4_455 1_555 no F(6) P(2) F(7) 180.0 . 1_555 1_555 no Ru O(2) C(1) 124.1(3) . 1_555 1_555 no Ru N(1) O(1) 168.3(4) . 1_555 1_555 yes Ru N(2) C(2) 111.9(3) . 1_555 1_555 no Ru N(2) C(6) 128.4(3) . 1_555 1_555 no C(2) N(2) C(6) 119.6(4) . 1_555 1_555 no Ru N(3) C(7) 117.9(3) . 1_555 1_555 no Ru N(3) C(11) 117.6(3) . 1_555 1_555 no C(7) N(3) C(11) 123.8(4) . 1_555 1_555 no Ru N(4) C(12) 113.1(3) . 1_555 1_555 no Ru N(4) C(16) 127.9(3) . 1_555 1_555 no C(12) N(4) C(16) 118.9(4) . 1_555 1_555 no N(2) C(2) C(3) 119.6(5) . 1_555 1_555 no N(2) C(2) C(7) 116.0(4) . 1_555 1_555 no C(3) C(2) C(7) 124.4(4) . 1_555 1_555 no C(2) C(3) C(4) 120.2(5) . 1_555 1_555 no C(3) C(4) C(5) 119.2(5) . 1_555 1_555 no C(4) C(5) C(6) 119.2(5) . 1_555 1_555 no N(2) C(6) C(5) 122.2(5) . 1_555 1_555 no N(3) C(7) C(2) 114.0(4) . 1_555 1_555 no N(3) C(7) C(8) 118.4(4) . 1_555 1_555 no C(2) C(7) C(8) 127.6(4) . 1_555 1_555 no C(7) C(8) C(9) 119.1(4) . 1_555 1_555 no C(8) C(9) C(10) 121.2(4) . 1_555 1_555 no C(9) C(10) C(11) 118.5(5) . 1_555 1_555 no N(3) C(11) C(10) 118.9(4) . 1_555 1_555 no N(3) C(11) C(12) 113.4(4) . 1_555 1_555 no C(10) C(11) C(12) 127.6(4) . 1_555 1_555 no N(4) C(12) C(11) 115.4(4) . 1_555 1_555 no N(4) C(12) C(13) 121.3(4) . 1_555 1_555 no C(11) C(12) C(13) 123.2(4) . 1_555 1_555 no C(12) C(13) C(14) 118.8(5) . 1_555 1_555 no C(13) C(14) C(15) 119.6(5) . 1_555 1_555 no C(14) C(15) C(16) 119.0(5) . 1_555 1_555 no N(4) C(16) C(15) 122.4(5) . 1_555 1_555 no #===END #------------------------------------------------------------------------------ data_[RuBr2(NO)(terpy)]PF6 _database_code_CSD 165250 _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' #------------------------------------------------------------------------------ _chemical_formula_sum 'C15 H11 Br2 F6 N4 O P Ru ' _chemical_formula_weight 669.12 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 9.187(1) _cell_length_b 16.638(1) _cell_length_c 13.1219(9) _cell_angle_alpha 90 _cell_angle_beta 95.479(5) _cell_angle_gamma 90 _cell_volume 1996.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14301 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 298.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'chip' _exptl_crystal_colour 'reddish-brown' _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.070 _exptl_crystal_density_diffrn 2.226 _exptl_crystal_F_000 1280.00 _exptl_absorpt_coefficient_mu 4.951 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.492 _exptl_absorpt_correction_T_max 0.778 #------------------------------------------------------------------------------ _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_reflns_number 18624 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9983 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ _reflns_number_total 4576 _reflns_number_gt 2934 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0389 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2934 _refine_ls_number_parameters 271 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0015 _refine_diff_density_max 0.40 _refine_diff_density_min -0.53 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ru' 'Ru' -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.13944(4) 0.22902(2) 0.43619(3) 0.02936(9) Uani 1.00 d . . . Br(1) Br 0.28896(6) 0.15853(3) 0.58072(4) 0.0449(2) Uani 1.00 d . . . Br(2) Br 0.00233(6) 0.28522(3) 0.27853(4) 0.0439(1) Uani 1.00 d . . . P P -0.2606(2) 0.05233(9) 0.0794(1) 0.0527(5) Uani 1.00 d . . . F(1) F -0.1826(5) 0.1095(3) 0.1646(4) 0.103(2) Uani 1.00 d . . . F(2) F -0.3491(6) 0.0115(3) 0.1627(4) 0.109(2) Uani 1.00 d . . . F(3) F -0.3380(5) -0.0032(3) -0.0074(4) 0.096(2) Uani 1.00 d . . . F(4) F -0.1741(5) 0.0953(3) -0.0058(4) 0.100(2) Uani 1.00 d . . . F(5) F -0.1344(5) -0.0116(3) 0.0985(4) 0.105(2) Uani 1.00 d . . . F(6) F -0.3851(5) 0.1181(3) 0.0600(3) 0.086(1) Uani 1.00 d . . . O O 0.1312(5) 0.3676(3) 0.5653(3) 0.066(1) Uani 1.00 d . . . N(1) N 0.1337(5) 0.3177(3) 0.5124(3) 0.039(1) Uani 1.00 d . . . N(2) N -0.0538(4) 0.1726(2) 0.4681(3) 0.032(1) Uani 1.00 d . . . N(3) N 0.1501(4) 0.1252(2) 0.3581(3) 0.032(1) Uani 1.00 d . . . N(4) N 0.3329(4) 0.2448(3) 0.3681(3) 0.037(1) Uani 1.00 d . . . C(1) C -0.0771(5) 0.1004(3) 0.4203(4) 0.036(1) Uani 1.00 d . . . C(2) C -0.2053(7) 0.0578(3) 0.4287(4) 0.051(2) Uani 1.00 d . . . C(3) C -0.3096(6) 0.0911(4) 0.4856(5) 0.061(2) Uani 1.00 d . . . C(4) C -0.2863(6) 0.1644(4) 0.5316(4) 0.054(2) Uani 1.00 d . . . C(5) C -0.1569(6) 0.2032(3) 0.5217(4) 0.043(1) Uani 1.00 d . . . C(6) C 0.0402(5) 0.0723(3) 0.3607(3) 0.034(1) Uani 1.00 d . . . C(7) C 0.0462(6) 0.0005(3) 0.3083(4) 0.046(2) Uani 1.00 d . . . C(8) C 0.1628(7) -0.0134(3) 0.2529(5) 0.053(2) Uani 1.00 d . . . C(9) C 0.2766(6) 0.0416(3) 0.2512(4) 0.046(2) Uani 1.00 d . . . C(10) C 0.2679(5) 0.1129(3) 0.3065(4) 0.038(1) Uani 1.00 d . . . C(11) C 0.3725(5) 0.1800(3) 0.3131(4) 0.038(1) Uani 1.00 d . . . C(12) C 0.5005(6) 0.1794(4) 0.2685(4) 0.051(2) Uani 1.00 d . . . C(13) C 0.5929(7) 0.2458(5) 0.2799(5) 0.063(2) Uani 1.00 d . . . C(14) C 0.5524(7) 0.3100(5) 0.3342(5) 0.062(2) Uani 1.00 d . . . C(15) C 0.4214(6) 0.3088(4) 0.3777(4) 0.050(2) Uani 1.00 d . . . H(1) H -0.2203 0.0059 0.3961 0.0617 Uiso 1.00 calc . . . H(2) H -0.3998 0.0625 0.4919 0.0738 Uiso 1.00 calc . . . H(3) H -0.3592 0.1886 0.5715 0.0645 Uiso 1.00 calc . . . H(4) H -0.1384 0.2546 0.5546 0.0526 Uiso 1.00 calc . . . H(5) H -0.0314 -0.0386 0.3098 0.0566 Uiso 1.00 calc . . . H(6) H 0.1661 -0.0629 0.2142 0.0633 Uiso 1.00 calc . . . H(7) H 0.3592 0.0313 0.2118 0.0565 Uiso 1.00 calc . . . H(8) H 0.5260 0.1329 0.2295 0.0625 Uiso 1.00 calc . . . H(9) H 0.6852 0.2468 0.2501 0.0739 Uiso 1.00 calc . . . H(10) H 0.6157 0.3563 0.3423 0.0741 Uiso 1.00 calc . . . H(11) H 0.3917 0.3552 0.4155 0.0615 Uiso 1.00 calc . . . #------------------------------------------------------------------------------ loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru 0.0306(2) 0.0270(2) 0.0308(2) -0.0036(2) 0.0043(1) -0.0036(1) Br(1) 0.0466(3) 0.0481(3) 0.0390(3) -0.0012(2) -0.0017(2) 0.0034(2) Br(2) 0.0454(3) 0.0422(3) 0.0434(3) 0.0004(2) 0.0002(2) 0.0065(2) P 0.0560(10) 0.0511(9) 0.0501(8) 0.0058(8) 0.0002(7) -0.0051(7) F(1) 0.117(4) 0.091(3) 0.095(3) 0.010(3) -0.028(3) -0.038(3) F(2) 0.158(5) 0.078(3) 0.100(3) -0.001(3) 0.061(3) 0.014(3) F(3) 0.073(3) 0.125(4) 0.088(3) -0.003(3) -0.001(2) -0.048(3) F(4) 0.101(3) 0.104(4) 0.101(3) -0.004(3) 0.047(3) 0.005(3) F(5) 0.110(4) 0.097(3) 0.102(3) 0.053(3) -0.021(3) -0.022(3) F(6) 0.090(3) 0.103(3) 0.068(2) 0.045(3) 0.014(2) 0.007(2) O 0.086(3) 0.052(3) 0.062(3) -0.011(2) 0.010(2) -0.021(2) N(1) 0.041(2) 0.035(2) 0.041(2) -0.002(2) 0.005(2) 0.001(2) N(2) 0.031(2) 0.031(2) 0.034(2) -0.001(2) 0.005(2) 0.001(2) N(3) 0.033(2) 0.030(2) 0.031(2) 0.001(2) -0.001(2) -0.004(2) N(4) 0.034(2) 0.042(2) 0.035(2) -0.005(2) 0.005(2) 0.000(2) C(1) 0.036(3) 0.033(3) 0.037(2) 0.000(2) -0.001(2) 0.003(2) C(2) 0.050(3) 0.045(3) 0.057(3) -0.016(3) 0.000(3) 0.007(3) C(3) 0.045(3) 0.076(5) 0.062(4) -0.020(3) 0.011(3) 0.024(3) C(4) 0.042(3) 0.069(4) 0.050(3) -0.002(3) 0.010(3) 0.004(3) C(5) 0.035(3) 0.054(3) 0.043(3) -0.001(2) 0.009(2) 0.001(2) C(6) 0.039(3) 0.027(2) 0.035(2) 0.002(2) -0.007(2) -0.002(2) C(7) 0.054(4) 0.032(3) 0.050(3) -0.002(2) -0.009(3) -0.005(2) C(8) 0.071(4) 0.033(3) 0.055(3) 0.008(3) -0.002(3) -0.011(2) C(9) 0.055(3) 0.042(3) 0.042(3) 0.013(3) 0.007(2) -0.006(2) C(10) 0.039(3) 0.041(3) 0.033(2) 0.006(2) 0.004(2) 0.002(2) C(11) 0.038(3) 0.043(3) 0.032(2) 0.003(2) 0.001(2) 0.003(2) C(12) 0.041(3) 0.070(4) 0.044(3) 0.005(3) 0.012(2) 0.002(3) C(13) 0.041(3) 0.102(5) 0.047(3) -0.008(4) 0.010(3) 0.008(3) C(14) 0.047(4) 0.080(5) 0.059(4) -0.027(3) 0.003(3) 0.013(4) C(15) 0.048(3) 0.055(3) 0.046(3) -0.019(3) 0.003(2) -0.002(3) #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Br(1) 2.5222(6) . . yes Ru Br(2) 2.4986(6) . . yes Ru N(1) 1.786(4) . . yes Ru N(2) 2.086(4) . . yes Ru N(3) 2.015(4) . . yes Ru N(4) 2.081(4) . . yes P F(1) 1.586(4) . . no P F(2) 1.577(5) . . no P F(3) 1.581(4) . . no P F(4) 1.599(4) . . no P F(5) 1.577(4) . . no P F(6) 1.586(4) . . no O N(1) 1.083(5) . . yes N(2) C(1) 1.362(6) . . no N(2) C(5) 1.335(6) . . no N(3) C(6) 1.343(6) . . no N(3) C(10) 1.347(6) . . no N(4) C(11) 1.365(6) . . no N(4) C(15) 1.339(7) . . no C(1) C(2) 1.388(7) . . no C(1) C(6) 1.467(7) . . no C(2) C(3) 1.385(9) . . no C(3) C(4) 1.369(9) . . no C(4) C(5) 1.370(8) . . no C(6) C(7) 1.383(7) . . no C(7) C(8) 1.371(8) . . no C(8) C(9) 1.392(8) . . no C(9) C(10) 1.397(7) . . no C(10) C(11) 1.470(7) . . no C(11) C(12) 1.363(7) . . no C(12) C(13) 1.393(9) . . no C(13) C(14) 1.36(1) . . no C(14) C(15) 1.380(8) . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br(1) Ru Br(2) 172.69(2) . 1_555 1_555 no Br(1) Ru N(1) 90.4(1) . 1_555 1_555 no Br(1) Ru N(2) 93.0(1) . 1_555 1_555 no Br(1) Ru N(3) 86.2(1) . 1_555 1_555 no Br(1) Ru N(4) 87.4(1) . 1_555 1_555 no Br(2) Ru N(1) 96.6(1) . 1_555 1_555 no Br(2) Ru N(2) 87.9(1) . 1_555 1_555 no Br(2) Ru N(3) 86.8(1) . 1_555 1_555 no Br(2) Ru N(4) 88.9(1) . 1_555 1_555 no N(1) Ru N(2) 100.9(2) . 1_555 1_555 no N(1) Ru N(3) 176.5(2) . 1_555 1_555 no N(1) Ru N(4) 102.0(2) . 1_555 1_555 no N(2) Ru N(3) 78.4(2) . 1_555 1_555 no N(2) Ru N(4) 157.1(2) . 1_555 1_555 yes N(3) Ru N(4) 78.7(2) . 1_555 1_555 no F(1) P F(2) 89.8(3) . 1_555 1_555 no F(1) P F(3) 178.7(3) . 1_555 1_555 no F(1) P F(4) 90.2(3) . 1_555 1_555 no F(1) P F(5) 90.9(3) . 1_555 1_555 no F(1) P F(6) 88.3(3) . 1_555 1_555 no F(2) P F(3) 91.3(3) . 1_555 1_555 no F(2) P F(4) 178.6(3) . 1_555 1_555 no F(2) P F(5) 91.1(3) . 1_555 1_555 no F(2) P F(6) 89.8(3) . 1_555 1_555 no F(3) P F(4) 88.7(3) . 1_555 1_555 no F(3) P F(5) 89.6(3) . 1_555 1_555 no F(3) P F(6) 91.1(3) . 1_555 1_555 no F(4) P F(5) 90.3(3) . 1_555 1_555 no F(4) P F(6) 88.8(3) . 1_555 1_555 no F(5) P F(6) 178.8(3) . 1_555 1_555 no Ru N(1) O 174.3(4) . 1_555 1_555 yes Ru N(2) C(1) 113.8(3) . 1_555 1_555 no Ru N(2) C(5) 126.5(3) . 1_555 1_555 no C(1) N(2) C(5) 119.5(4) . 1_555 1_555 no Ru N(3) C(6) 118.4(3) . 1_555 1_555 no Ru N(3) C(10) 117.9(3) . 1_555 1_555 no C(6) N(3) C(10) 123.7(4) . 1_555 1_555 no Ru N(4) C(11) 114.2(3) . 1_555 1_555 no Ru N(4) C(15) 126.6(4) . 1_555 1_555 no C(11) N(4) C(15) 119.2(4) . 1_555 1_555 no N(2) C(1) C(2) 120.7(5) . 1_555 1_555 no N(2) C(1) C(6) 115.8(4) . 1_555 1_555 no C(2) C(1) C(6) 123.5(5) . 1_555 1_555 no C(1) C(2) C(3) 118.3(5) . 1_555 1_555 no C(2) C(3) C(4) 120.4(5) . 1_555 1_555 no C(3) C(4) C(5) 118.6(6) . 1_555 1_555 no N(2) C(5) C(4) 122.4(5) . 1_555 1_555 no N(3) C(6) C(1) 113.4(4) . 1_555 1_555 no N(3) C(6) C(7) 119.2(5) . 1_555 1_555 no C(1) C(6) C(7) 127.4(5) . 1_555 1_555 no C(6) C(7) C(8) 118.7(5) . 1_555 1_555 no C(7) C(8) C(9) 121.6(5) . 1_555 1_555 no C(8) C(9) C(10) 118.0(5) . 1_555 1_555 no N(3) C(10) C(9) 118.7(5) . 1_555 1_555 no N(3) C(10) C(11) 114.0(4) . 1_555 1_555 no C(9) C(10) C(11) 127.3(5) . 1_555 1_555 no N(4) C(11) C(10) 115.2(4) . 1_555 1_555 no N(4) C(11) C(12) 121.2(5) . 1_555 1_555 no C(10) C(11) C(12) 123.7(5) . 1_555 1_555 no C(11) C(12) C(13) 119.3(6) . 1_555 1_555 no C(12) C(13) C(14) 119.1(5) . 1_555 1_555 no C(13) C(14) C(15) 120.0(6) . 1_555 1_555 no N(4) C(15) C(14) 121.2(6) . 1_555 1_555 no #===END