# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4b #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H11 Cl2 N4 O Ru, F6 P' _chemical_formula_sum 'C15 H11 Cl2 F6 N4 O P Ru' _chemical_formula_weight 580.22 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.2048(5) _cell_length_b 12.3116(4) _cell_length_c 19.4697(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3884.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9929 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.5 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8200 _exptl_absorpt_correction_T_max 0.8267 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _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 'Bruker Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_unetI/netI 0.019 _diffrn_reflns_number 58235 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.69 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 4526 _reflns_number_gt 3663 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0325P)^2^+7.8644P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4526 _refine_ls_number_parameters 336 _refine_ls_number_restraints 249 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.176 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.003 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.3261(2) 0.2992(3) 0.33395(17) 0.0332(7) Uani 1 1 d . . . H1 H 0.3737 0.3341 0.3518 0.04 Uiso 1 1 calc R . . C2 C 0.3325(3) 0.2410(3) 0.27338(19) 0.0407(9) Uani 1 1 d . . . H2 H 0.3839 0.2364 0.25 0.049 Uiso 1 1 calc R . . C3 C 0.2644(3) 0.1901(3) 0.2474(2) 0.0436(9) Uani 1 1 d . . . H3 H 0.2678 0.15 0.2058 0.052 Uiso 1 1 calc R . . C4 C 0.1904(2) 0.1974(3) 0.28233(18) 0.0376(8) Uani 1 1 d . . . H4 H 0.1424 0.1631 0.2648 0.045 Uiso 1 1 calc R . . C5 C 0.1870(2) 0.2553(3) 0.34320(16) 0.0275(7) Uani 1 1 d . . . C6 C 0.1125(2) 0.2651(3) 0.38574(16) 0.0268(7) Uani 1 1 d . . . C7 C 0.0353(2) 0.2204(3) 0.3731(2) 0.0376(8) Uani 1 1 d . . . H7 H 0.0256 0.1782 0.3331 0.045 Uiso 1 1 calc R . . C8 C -0.0271(2) 0.2384(3) 0.4200(2) 0.0422(9) Uani 1 1 d . . . H8 H -0.0801 0.208 0.4119 0.051 Uiso 1 1 calc R . . C9 C -0.0142(2) 0.2996(3) 0.4783(2) 0.0380(8) Uani 1 1 d . . . H9 H -0.0577 0.3121 0.5101 0.046 Uiso 1 1 calc R . . C10 C 0.0641(2) 0.3424(3) 0.48926(17) 0.0281(7) Uani 1 1 d . . . C11 C 0.0909(2) 0.4099(3) 0.54751(16) 0.0288(7) Uani 1 1 d . . . C12 C 0.0417(3) 0.4341(3) 0.60361(19) 0.0429(9) Uani 1 1 d . . . H12 H -0.0134 0.4081 0.6061 0.051 Uiso 1 1 calc R . . C13 C 0.0742(3) 0.4967(4) 0.6560(2) 0.0532(12) Uani 1 1 d . . . H13 H 0.0413 0.5146 0.6948 0.064 Uiso 1 1 calc R . . C14 C 0.1538(3) 0.5326(3) 0.6517(2) 0.0487(11) Uani 1 1 d . . . H14 H 0.1767 0.5749 0.6878 0.058 Uiso 1 1 calc R . . C15 C 0.2008(3) 0.5073(3) 0.59496(17) 0.0358(8) Uani 1 1 d . . . H15 H 0.2561 0.5327 0.5922 0.043 Uiso 1 1 calc R . . N1 N 0.25479(17) 0.3076(2) 0.36798(13) 0.0254(6) Uani 1 1 d . . . N2 N 0.12399(16) 0.3236(2) 0.44329(13) 0.0238(5) Uani 1 1 d . . . N3 N 0.16968(18) 0.4475(2) 0.54350(13) 0.0263(6) Uani 1 1 d . . . N4 N 0.32789(19) 0.4667(2) 0.46669(14) 0.0323(6) Uani 1 1 d . . . O1 O 0.38435(19) 0.5191(3) 0.46913(15) 0.0594(9) Uani 1 1 d . . . Cl1 Cl 0.27032(5) 0.24214(7) 0.52363(4) 0.03257(19) Uani 1 1 d . . . Cl2 Cl 0.17788(6) 0.53487(7) 0.39039(4) 0.03456(19) Uani 1 1 d . . . Ru1 Ru 0.234015(15) 0.39467(2) 0.457881(12) 0.02179(8) Uani 1 1 d . . . P1 P 0.0605(3) 0.4113(5) 0.1664(3) 0.0384(7) Uani 0.633(7) 1 d PDU A 1 F1 F 0.0145(4) 0.3638(6) 0.0998(3) 0.0821(17) Uani 0.633(7) 1 d PDU A 1 F2 F -0.0244(4) 0.4741(6) 0.1825(3) 0.0504(13) Uani 0.633(7) 1 d PDU A 1 F3 F 0.0996(4) 0.4540(6) 0.2339(3) 0.0865(16) Uani 0.633(7) 1 d PDU A 1 F4 F 0.1391(3) 0.3414(4) 0.1495(3) 0.0678(14) Uani 0.633(7) 1 d PDU A 1 F5 F 0.0237(4) 0.3098(5) 0.2081(3) 0.0662(16) Uani 0.633(7) 1 d PDU A 1 F6 F 0.0988(6) 0.5136(6) 0.1269(4) 0.0683(18) Uani 0.633(7) 1 d PDU A 1 P1' P 0.0647(7) 0.4231(9) 0.1695(6) 0.0478(14) Uani 0.367(7) 1 d PDU A 2 F1' F 0.0470(8) 0.3325(9) 0.1157(6) 0.087(2) Uani 0.367(7) 1 d PDU A 2 F2' F -0.0260(6) 0.4696(10) 0.1548(6) 0.059(2) Uani 0.367(7) 1 d PDU A 2 F3' F 0.0744(6) 0.5239(7) 0.2199(4) 0.066(2) Uani 0.367(7) 1 d PDU A 2 F4' F 0.1555(5) 0.3886(9) 0.1837(6) 0.073(2) Uani 0.367(7) 1 d PDU A 2 F5' F 0.0329(7) 0.3517(8) 0.2307(5) 0.057(2) Uani 0.367(7) 1 d PDU A 2 F6' F 0.0900(10) 0.4966(12) 0.1051(5) 0.063(2) Uani 0.367(7) 1 d PDU A 2 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 C1 0.0329(18) 0.0341(18) 0.0325(17) 0.0034(14) 0.0061(14) 0.0006(15) C2 0.047(2) 0.040(2) 0.0347(18) 0.0047(16) 0.0125(17) 0.0075(18) C3 0.059(3) 0.042(2) 0.0296(17) -0.0046(16) -0.0008(17) 0.0103(19) C4 0.045(2) 0.0333(19) 0.0346(18) -0.0042(15) -0.0080(16) 0.0018(16) C5 0.0323(18) 0.0228(15) 0.0274(15) 0.0025(12) -0.0056(13) 0.0016(13) C6 0.0257(16) 0.0223(15) 0.0325(16) 0.0031(13) -0.0045(13) -0.0022(13) C7 0.036(2) 0.0304(18) 0.047(2) 0.0025(16) -0.0113(16) -0.0062(15) C8 0.0247(18) 0.041(2) 0.061(2) 0.0092(19) -0.0072(17) -0.0096(16) C9 0.0243(18) 0.040(2) 0.050(2) 0.0124(17) 0.0027(15) -0.0018(15) C10 0.0237(16) 0.0276(16) 0.0332(17) 0.0101(13) 0.0016(13) 0.0021(13) C11 0.0289(17) 0.0261(16) 0.0313(16) 0.0076(13) 0.0043(13) 0.0080(13) C12 0.044(2) 0.044(2) 0.040(2) 0.0115(17) 0.0144(17) 0.0130(18) C13 0.076(3) 0.050(2) 0.034(2) 0.0033(18) 0.017(2) 0.027(2) C14 0.075(3) 0.039(2) 0.0319(19) -0.0048(16) -0.001(2) 0.012(2) C15 0.050(2) 0.0278(17) 0.0299(17) -0.0018(14) -0.0044(16) 0.0045(16) N1 0.0281(14) 0.0237(13) 0.0243(12) 0.0019(11) 0.0025(11) 0.0001(11) N2 0.0201(13) 0.0212(12) 0.0300(13) 0.0058(10) -0.0020(10) 0.0000(10) N3 0.0322(15) 0.0213(13) 0.0252(13) 0.0027(10) -0.0008(11) 0.0037(11) N4 0.0329(16) 0.0352(16) 0.0289(14) -0.0013(12) -0.0002(12) -0.0098(13) O1 0.0466(18) 0.078(2) 0.0539(18) -0.0072(16) 0.0029(14) -0.0349(17) Cl1 0.0300(4) 0.0309(4) 0.0367(4) 0.0070(3) -0.0018(3) 0.0053(3) Cl2 0.0427(5) 0.0254(4) 0.0356(4) 0.0077(3) -0.0043(4) -0.0018(3) Ru1 0.02003(14) 0.02154(13) 0.02380(13) 0.00142(9) -0.00055(9) -0.00290(9) P1 0.0353(12) 0.0516(16) 0.0285(11) 0.0023(11) 0.0052(10) 0.0052(11) F1 0.083(4) 0.107(4) 0.056(3) -0.026(3) -0.019(2) 0.017(3) F2 0.050(2) 0.051(2) 0.049(3) -0.003(2) 0.013(2) 0.012(2) F3 0.081(3) 0.111(4) 0.068(3) -0.016(3) -0.023(2) -0.010(3) F4 0.056(3) 0.068(3) 0.079(3) 0.014(2) 0.030(2) 0.023(2) F5 0.050(3) 0.070(4) 0.079(4) 0.030(3) 0.012(3) 0.005(3) F6 0.066(3) 0.062(3) 0.076(4) 0.020(3) 0.014(3) 0.011(2) P1' 0.050(2) 0.052(2) 0.042(2) 0.009(2) 0.008(2) 0.012(2) F1' 0.114(5) 0.073(4) 0.074(4) -0.031(4) -0.003(4) 0.018(4) F2' 0.044(3) 0.053(4) 0.079(5) 0.010(4) -0.015(4) -0.011(3) F3' 0.083(5) 0.056(4) 0.059(4) -0.010(3) -0.016(4) -0.018(4) F4' 0.048(3) 0.086(5) 0.087(5) 0.047(4) 0.016(3) 0.017(3) F5' 0.060(4) 0.059(4) 0.053(4) 0.016(3) 0.018(3) 0.009(4) F6' 0.075(5) 0.074(5) 0.039(4) 0.022(4) 0.019(4) 0.016(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.336(4) . ? C1 C2 1.384(5) . ? C1 H1 0.95 . ? C2 C3 1.367(6) . ? C2 H2 0.95 . ? C3 C4 1.380(6) . ? C3 H3 0.95 . ? C4 C5 1.384(5) . ? C4 H4 0.95 . ? C5 N1 1.361(4) . ? C5 C6 1.470(5) . ? C6 N2 1.345(4) . ? C6 C7 1.389(5) . ? C7 C8 1.379(5) . ? C7 H7 0.95 . ? C8 C9 1.378(6) . ? C8 H8 0.95 . ? C9 C10 1.391(5) . ? C9 H9 0.95 . ? C10 N2 1.340(4) . ? C10 C11 1.472(5) . ? C11 N3 1.360(5) . ? C11 C12 1.384(5) . ? C12 C13 1.383(6) . ? C12 H12 0.95 . ? C13 C14 1.366(7) . ? C13 H13 0.95 . ? C14 C15 1.378(5) . ? C14 H14 0.95 . ? C15 N3 1.342(4) . ? C15 H15 0.95 . ? N1 Ru1 2.080(3) . ? N2 Ru1 2.006(3) . ? N3 Ru1 2.071(3) . ? N4 O1 1.121(4) . ? N4 Ru1 1.769(3) . ? Cl1 Ru1 2.3475(8) . ? Cl2 Ru1 2.3524(8) . ? P1 F3 1.551(7) . ? P1 F4 1.572(6) . ? P1 F6 1.601(7) . ? P1 F5 1.605(7) . ? P1 F1 1.605(6) . ? P1 F2 1.609(7) . ? P1' F4' 1.556(12) . ? P1' F1' 1.557(12) . ? P1' F5' 1.566(12) . ? P1' F3' 1.590(11) . ? P1' F6' 1.600(12) . ? P1' F2' 1.602(12) . ? 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_3 _geom_angle_publ_flag N1 C1 C2 121.9(3) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.4(4) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.3(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 115.1(3) . . ? C4 C5 C6 123.9(3) . . ? N2 C6 C7 119.0(3) . . ? N2 C6 C5 113.5(3) . . ? C7 C6 C5 127.5(3) . . ? C8 C7 C6 118.6(3) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C9 C8 C7 121.5(3) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 118.1(3) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N2 C10 C9 119.5(3) . . ? N2 C10 C11 113.5(3) . . ? C9 C10 C11 127.0(3) . . ? N3 C11 C12 120.8(3) . . ? N3 C11 C10 115.1(3) . . ? C12 C11 C10 124.0(3) . . ? C13 C12 C11 118.9(4) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 C12 119.6(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N3 C15 C14 121.0(4) . . ? N3 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C1 N1 C5 119.0(3) . . ? C1 N1 Ru1 126.7(2) . . ? C5 N1 Ru1 114.3(2) . . ? C10 N2 C6 123.2(3) . . ? C10 N2 Ru1 118.3(2) . . ? C6 N2 Ru1 118.3(2) . . ? C15 N3 C11 119.8(3) . . ? C15 N3 Ru1 125.7(3) . . ? C11 N3 Ru1 114.3(2) . . ? O1 N4 Ru1 174.1(3) . . ? N4 Ru1 N2 175.18(12) . . ? N4 Ru1 N3 101.38(12) . . ? N2 Ru1 N3 78.67(11) . . ? N4 Ru1 N1 101.57(12) . . ? N2 Ru1 N1 78.47(11) . . ? N3 Ru1 N1 157.04(11) . . ? N4 Ru1 Cl1 97.62(10) . . ? N2 Ru1 Cl1 87.20(7) . . ? N3 Ru1 Cl1 86.47(7) . . ? N1 Ru1 Cl1 90.36(8) . . ? N4 Ru1 Cl2 91.08(10) . . ? N2 Ru1 Cl2 84.10(7) . . ? N3 Ru1 Cl2 91.41(7) . . ? N1 Ru1 Cl2 88.31(8) . . ? Cl1 Ru1 Cl2 171.29(3) . . ? F3 P1 F4 91.9(4) . . ? F3 P1 F6 88.9(4) . . ? F4 P1 F6 91.0(5) . . ? F3 P1 F5 89.3(4) . . ? F4 P1 F5 88.9(4) . . ? F6 P1 F5 178.2(5) . . ? F3 P1 F1 175.8(5) . . ? F4 P1 F1 90.5(4) . . ? F6 P1 F1 94.5(5) . . ? F5 P1 F1 87.3(4) . . ? F3 P1 F2 91.2(4) . . ? F4 P1 F2 175.3(5) . . ? F6 P1 F2 92.6(5) . . ? F5 P1 F2 87.6(4) . . ? F1 P1 F2 86.2(4) . . ? F4' P1' F1' 95.6(8) . . ? F4' P1' F5' 91.3(8) . . ? F1' P1' F5' 92.9(8) . . ? F4' P1' F3' 90.6(8) . . ? F1' P1' F3' 173.1(10) . . ? F5' P1' F3' 90.1(7) . . ? F4' P1' F6' 92.9(9) . . ? F1' P1' F6' 85.7(9) . . ? F5' P1' F6' 175.6(11) . . ? F3' P1' F6' 90.9(8) . . ? F4' P1' F2' 174.9(10) . . ? F1' P1' F2' 88.1(8) . . ? F5' P1' F2' 92.0(8) . . ? F3' P1' F2' 85.6(7) . . ? F6' P1' F2' 83.8(9) . . ? _database_code_depnum_ccdc_archive 'CCDC 939959' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[RUII(DEAP-terpy)Cl2(NO)](PF6) #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H24 Cl2 N5 O Ru, F6 P, O' _chemical_formula_sum 'C25 H24 Cl2 F6 N5 O2 P Ru' _chemical_formula_weight 743.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_Int_Tables_number 60 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 25.5380(16) _cell_length_b 15.5011(9) _cell_length_c 14.6239(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5789.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7681 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 21.92 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9030 _exptl_absorpt_correction_T_max 0.9666 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _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 'Bruker Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_unetI/netI 0.0447 _diffrn_reflns_number 65294 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.43 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 5335 _reflns_number_gt 3376 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0808P)^2^+17.9125P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5335 _refine_ls_number_parameters 454 _refine_ls_number_restraints 233 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1741 _refine_ls_wR_factor_gt 0.142 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.064 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.111 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.4401(3) 0.0324(4) 0.5941(5) 0.0495(17) Uani 1 1 d . . . H1 H 0.407 0.0094 0.5775 0.059 Uiso 1 1 calc R . . C2 C 0.4798(3) -0.0227(4) 0.6172(5) 0.0561(19) Uani 1 1 d . . . H2 H 0.474 -0.0832 0.6174 0.067 Uiso 1 1 calc R . . C3 C 0.5277(3) 0.0096(4) 0.6398(5) 0.0518(17) Uani 1 1 d . . . H3 H 0.5556 -0.0285 0.6545 0.062 Uiso 1 1 calc R . . C4 C 0.5358(3) 0.0978(4) 0.6415(4) 0.0444(15) Uani 1 1 d . . . H4 H 0.5689 0.1209 0.658 0.053 Uiso 1 1 calc R . . C5 C 0.4950(2) 0.1512(4) 0.6189(4) 0.0406(15) Uani 1 1 d . . . C6 C 0.4981(2) 0.2466(4) 0.6197(4) 0.0386(14) Uani 1 1 d . . . C7 C 0.5418(2) 0.2955(4) 0.6384(4) 0.0368(14) Uani 1 1 d . . . H7 H 0.5741 0.2678 0.6522 0.044 Uiso 1 1 calc R . . C8 C 0.5390(2) 0.3861(4) 0.6371(4) 0.0382(14) Uani 1 1 d . . . C9 C 0.4906(2) 0.4240(4) 0.6181(4) 0.0402(15) Uani 1 1 d . . . H9 H 0.4874 0.485 0.6178 0.048 Uiso 1 1 calc R . . C10 C 0.4473(2) 0.3738(4) 0.5998(4) 0.0383(14) Uani 1 1 d . . . C11 C 0.3937(2) 0.4019(4) 0.5778(4) 0.0405(15) Uani 1 1 d . . . C12 C 0.3777(2) 0.4864(4) 0.5788(5) 0.0453(16) Uani 1 1 d . . . H12 H 0.4022 0.531 0.591 0.054 Uiso 1 1 calc R . . C13 C 0.3259(2) 0.5063(4) 0.5619(5) 0.0499(16) Uani 1 1 d . . . H13 H 0.3142 0.5645 0.5617 0.06 Uiso 1 1 calc R . . C14 C 0.2916(3) 0.4395(5) 0.5455(5) 0.0530(18) Uani 1 1 d . . . H14 H 0.2556 0.4513 0.5351 0.064 Uiso 1 1 calc R . . C15 C 0.3092(2) 0.3562(4) 0.5440(4) 0.0463(16) Uani 1 1 d . . . H15 H 0.2852 0.3108 0.532 0.056 Uiso 1 1 calc R . . C16 C 0.5864(2) 0.4367(4) 0.6552(4) 0.0396(14) Uani 1 1 d . . . C17 C 0.6360(2) 0.3997(4) 0.6492(5) 0.0467(16) Uani 1 1 d . . . H17 H 0.6387 0.3403 0.6338 0.056 Uiso 1 1 calc R . . C18 C 0.6806(2) 0.4452(4) 0.6647(5) 0.0471(16) Uani 1 1 d . . . H18 H 0.7135 0.4174 0.6584 0.057 Uiso 1 1 calc R . . C19 C 0.6790(2) 0.5325(4) 0.6898(5) 0.0447(16) Uani 1 1 d . . . C20 C 0.6291(2) 0.5708(4) 0.6958(5) 0.0439(15) Uani 1 1 d . . . H20 H 0.6262 0.6299 0.712 0.053 Uiso 1 1 calc R . . C21 C 0.5847(2) 0.5240(4) 0.6785(4) 0.0426(15) Uani 1 1 d . . . H21 H 0.5517 0.552 0.6825 0.051 Uiso 1 1 calc R . . C22 C 0.7764(3) 0.5441(5) 0.6808(5) 0.061(2) Uani 1 1 d . . . H22A H 0.7732 0.5061 0.6267 0.074 Uiso 1 1 calc R . . H22B H 0.8 0.5924 0.6648 0.074 Uiso 1 1 calc R . . C23 C 0.7987(3) 0.4954(5) 0.7569(6) 0.075(2) Uani 1 1 d . . . H23A H 0.8036 0.5338 0.8095 0.113 Uiso 1 1 calc R . . H23B H 0.8326 0.4714 0.7386 0.113 Uiso 1 1 calc R . . H23C H 0.7749 0.4484 0.7737 0.113 Uiso 1 1 calc R . . C24 C 0.7229(2) 0.6642(4) 0.7479(5) 0.0511(18) Uani 1 1 d . . . H24A H 0.754 0.6706 0.7877 0.061 Uiso 1 1 calc R . . H24B H 0.6914 0.6688 0.7869 0.061 Uiso 1 1 calc R . . C25 C 0.7225(3) 0.7359(5) 0.6786(6) 0.069(2) Uani 1 1 d . . . H25A H 0.754 0.7324 0.6407 0.104 Uiso 1 1 calc R . . H25B H 0.7216 0.7916 0.7102 0.104 Uiso 1 1 calc R . . H25C H 0.6914 0.7304 0.6397 0.104 Uiso 1 1 calc R . . N2 N 0.4470(2) 0.1196(3) 0.5942(4) 0.0425(13) Uani 1 1 d . A . N3 N 0.45217(18) 0.2859(3) 0.6007(4) 0.0394(12) Uani 1 1 d . A . N4 N 0.35928(19) 0.3374(3) 0.5590(3) 0.0421(12) Uani 1 1 d . A . N5 N 0.7240(2) 0.5788(3) 0.7048(5) 0.0570(16) Uani 1 1 d . . . Cl1 Cl 0.36512(6) 0.20783(11) 0.71593(13) 0.0552(5) Uani 1 1 d . A . Ru1 Ru 0.391375(19) 0.21358(3) 0.56420(4) 0.0419(2) Uani 1 1 d D . . Cl2 Cl 0.42510(13) 0.22055(19) 0.4182(2) 0.0566(7) Uani 0.680(5) 1 d PD A 1 N1 N 0.3390(4) 0.1470(6) 0.5300(7) 0.0566(7) Uani 0.680(5) 1 d PD A 1 O1 O 0.3075(4) 0.1156(6) 0.5035(7) 0.0566(7) Uani 0.680(5) 1 d PD A 1 Cl2' Cl 0.3138(3) 0.1331(5) 0.5250(5) 0.0566(7) Uani 0.320(5) 1 d PD A 2 N1' N 0.4001(10) 0.2122(14) 0.4385(13) 0.0566(7) Uani 0.320(5) 1 d PD A 2 O1' O 0.4072(7) 0.2062(10) 0.3661(11) 0.0566(7) Uani 0.320(5) 1 d PD A 2 P1 P 0.3590(4) 0.8025(7) 0.5534(6) 0.0563(16) Uani 0.57 1 d PDU B 1 F1 F 0.3738(6) 0.7016(7) 0.5513(8) 0.073(3) Uani 0.57 1 d PDU B 1 F2 F 0.3682(5) 0.8032(8) 0.6609(7) 0.091(3) Uani 0.57 1 d PDU B 1 F3 F 0.3451(8) 0.9027(8) 0.5523(12) 0.085(3) Uani 0.57 1 d PDU B 1 F4 F 0.3517(4) 0.7983(7) 0.4451(6) 0.063(2) Uani 0.57 1 d PDU B 1 F5 F 0.4203(4) 0.8243(14) 0.5406(10) 0.074(3) Uani 0.57 1 d PDU B 1 F6 F 0.2996(4) 0.7780(9) 0.5655(9) 0.088(3) Uani 0.57 1 d PDU B 1 P1' P 0.3548(6) 0.8120(10) 0.5602(9) 0.066(2) Uani 0.43 1 d PDU C 2 F1' F 0.3680(9) 0.7135(10) 0.5843(12) 0.077(4) Uani 0.43 1 d PDU C 2 F2' F 0.3773(6) 0.8426(10) 0.6562(9) 0.077(3) Uani 0.43 1 d PDU C 2 F3' F 0.3431(11) 0.9105(10) 0.5322(16) 0.084(4) Uani 0.43 1 d PDU C 2 F4' F 0.3320(6) 0.7852(12) 0.4637(10) 0.087(4) Uani 0.43 1 d PDU C 2 F5' F 0.4124(6) 0.8217(19) 0.5173(13) 0.078(4) Uani 0.43 1 d PDU C 2 F6' F 0.2989(5) 0.8023(11) 0.6042(11) 0.080(4) Uani 0.43 1 d PDU C 2 O2 O 0.4774(3) 0.6467(6) 0.6098(7) 0.088(3) Uani 0.733(14) 1 d PU D 1 O2' O 0.4759(9) 0.7011(18) 0.654(2) 0.090(5) Uani 0.267(14) 1 d PU D 2 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 C1 0.056(4) 0.036(4) 0.057(4) -0.007(3) 0.007(3) -0.019(3) C2 0.074(5) 0.033(4) 0.060(5) -0.001(3) 0.003(4) -0.011(3) C3 0.059(4) 0.041(4) 0.056(4) -0.004(3) 0.003(4) -0.001(3) C4 0.051(4) 0.039(4) 0.043(4) -0.005(3) 0.003(3) -0.006(3) C5 0.044(4) 0.033(3) 0.044(4) -0.005(3) 0.007(3) -0.013(3) C6 0.040(3) 0.031(3) 0.045(4) -0.001(3) 0.010(3) -0.004(3) C7 0.031(3) 0.036(3) 0.044(4) 0.003(3) -0.003(3) -0.007(3) C8 0.038(3) 0.036(3) 0.040(4) 0.000(3) -0.001(3) -0.007(3) C9 0.038(3) 0.030(3) 0.053(4) 0.002(3) -0.004(3) -0.011(3) C10 0.038(3) 0.037(3) 0.040(3) 0.005(3) 0.004(3) -0.005(3) C11 0.036(3) 0.045(4) 0.041(4) 0.001(3) 0.003(3) -0.009(3) C12 0.044(4) 0.041(4) 0.051(4) -0.004(3) -0.001(3) -0.001(3) C13 0.045(4) 0.047(4) 0.057(4) -0.003(3) -0.006(3) 0.004(3) C14 0.040(4) 0.067(5) 0.052(4) -0.006(4) -0.008(3) -0.003(3) C15 0.038(4) 0.048(4) 0.053(4) -0.007(3) 0.000(3) -0.009(3) C16 0.033(3) 0.036(3) 0.050(4) 0.003(3) -0.006(3) -0.006(3) C17 0.045(4) 0.028(3) 0.067(5) 0.003(3) -0.005(3) -0.004(3) C18 0.033(3) 0.038(4) 0.070(5) -0.008(3) -0.003(3) -0.002(3) C19 0.037(3) 0.034(3) 0.063(4) -0.002(3) 0.001(3) -0.008(3) C20 0.037(3) 0.029(3) 0.066(5) -0.004(3) -0.003(3) -0.003(3) C21 0.032(3) 0.031(3) 0.064(4) 0.005(3) -0.001(3) -0.005(3) C22 0.065(5) 0.053(4) 0.066(5) 0.003(4) -0.008(4) -0.020(4) C23 0.088(6) 0.060(5) 0.079(6) 0.005(4) -0.021(5) -0.021(5) C24 0.035(4) 0.041(4) 0.078(5) -0.013(4) -0.002(3) -0.008(3) C25 0.071(5) 0.054(5) 0.084(6) -0.018(4) 0.011(4) -0.020(4) N2 0.048(3) 0.036(3) 0.044(3) -0.004(2) 0.007(2) -0.010(2) N3 0.033(3) 0.035(3) 0.050(3) -0.002(2) 0.002(2) -0.010(2) N4 0.033(3) 0.048(3) 0.045(3) -0.002(2) -0.001(2) -0.016(2) N5 0.031(3) 0.041(3) 0.099(5) -0.018(3) -0.004(3) -0.008(2) Cl1 0.0442(9) 0.0597(11) 0.0616(11) -0.0054(9) -0.0001(8) -0.0129(8) Ru1 0.0358(3) 0.0389(3) 0.0510(3) -0.0058(2) 0.0018(2) -0.0132(2) Cl2 0.0591(16) 0.0545(14) 0.0563(16) 0.0003(11) -0.0059(12) -0.0083(12) N1 0.0591(16) 0.0545(14) 0.0563(16) 0.0003(11) -0.0059(12) -0.0083(12) O1 0.0591(16) 0.0545(14) 0.0563(16) 0.0003(11) -0.0059(12) -0.0083(12) Cl2' 0.0591(16) 0.0545(14) 0.0563(16) 0.0003(11) -0.0059(12) -0.0083(12) N1' 0.0591(16) 0.0545(14) 0.0563(16) 0.0003(11) -0.0059(12) -0.0083(12) O1' 0.0591(16) 0.0545(14) 0.0563(16) 0.0003(11) -0.0059(12) -0.0083(12) P1 0.044(3) 0.061(3) 0.064(3) -0.007(2) 0.006(2) -0.004(2) F1 0.070(6) 0.057(4) 0.091(8) 0.009(5) -0.017(6) -0.006(4) F2 0.095(6) 0.113(8) 0.065(4) -0.002(5) 0.008(4) -0.027(6) F3 0.094(6) 0.063(5) 0.098(8) -0.011(5) 0.011(7) 0.000(5) F4 0.060(6) 0.063(5) 0.065(4) 0.000(4) 0.000(4) -0.008(4) F5 0.053(4) 0.089(6) 0.080(8) -0.020(6) 0.006(4) -0.030(4) F6 0.050(4) 0.108(8) 0.105(8) 0.010(6) 0.009(5) -0.015(4) P1' 0.058(4) 0.067(4) 0.073(4) 0.005(4) 0.002(3) -0.018(4) F1' 0.064(7) 0.069(6) 0.099(10) 0.011(6) 0.007(7) 0.000(5) F2' 0.064(6) 0.097(9) 0.070(5) -0.009(6) 0.004(5) -0.003(7) F3' 0.092(8) 0.068(6) 0.093(10) 0.010(6) -0.009(7) -0.012(6) F4' 0.087(9) 0.087(7) 0.089(7) -0.007(6) -0.020(6) -0.021(7) F5' 0.069(6) 0.091(7) 0.074(8) -0.014(7) 0.019(6) -0.023(6) F6' 0.049(5) 0.085(9) 0.106(10) 0.022(8) 0.005(6) -0.004(5) O2 0.082(5) 0.053(5) 0.129(8) 0.013(5) -0.013(5) 0.022(4) O2' 0.074(9) 0.076(10) 0.120(12) -0.006(9) 0.008(9) -0.005(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.362(8) . ? C1 C2 1.368(10) . ? C1 H1 0.95 . ? C2 C3 1.364(9) . ? C2 H2 0.95 . ? C3 C4 1.382(9) . ? C3 H3 0.95 . ? C4 C5 1.372(9) . ? C4 H4 0.95 . ? C5 N2 1.369(8) . ? C5 C6 1.482(8) . ? C6 N3 1.351(8) . ? C6 C7 1.376(8) . ? C7 C8 1.407(8) . ? C7 H7 0.95 . ? C8 C9 1.396(8) . ? C8 C16 1.466(8) . ? C9 C10 1.376(8) . ? C9 H9 0.95 . ? C10 N3 1.369(7) . ? C10 C11 1.472(8) . ? C11 N4 1.360(7) . ? C11 C12 1.372(9) . ? C12 C13 1.382(9) . ? C12 H12 0.95 . ? C13 C14 1.377(9) . ? C13 H13 0.95 . ? C14 C15 1.367(9) . ? C14 H14 0.95 . ? C15 N4 1.330(8) . ? C15 H15 0.95 . ? C16 C17 1.394(8) . ? C16 C21 1.397(8) . ? C17 C18 1.359(8) . ? C17 H17 0.95 . ? C18 C19 1.402(9) . ? C18 H18 0.95 . ? C19 N5 1.373(7) . ? C19 C20 1.408(8) . ? C20 C21 1.368(8) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 C23 1.460(10) . ? C22 N5 1.484(9) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 N5 1.465(8) . ? C24 C25 1.505(10) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? N2 Ru1 2.081(5) . ? N3 Ru1 1.988(5) . ? N4 Ru1 2.089(5) . ? Cl1 Ru1 2.3197(19) . ? Ru1 N1 1.762(10) . ? Ru1 N1' 1.852(18) . ? Ru1 Cl2 2.305(3) . ? Ru1 Cl2' 2.411(7) . ? N1 O1 1.017(12) . ? N1' O1' 1.078(17) . ? P1 F6 1.573(9) . ? P1 F2 1.589(10) . ? P1 F3 1.592(10) . ? P1 F4 1.597(9) . ? P1 F1 1.610(9) . ? P1 F5 1.613(9) . ? P1' F6' 1.573(12) . ? P1' F4' 1.583(12) . ? P1' F2' 1.588(12) . ? P1' F1' 1.603(12) . ? P1' F5' 1.605(12) . ? P1' F3' 1.608(12) . ? 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_3 _geom_angle_publ_flag N2 C1 C2 121.6(6) . . ? N2 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 119.7(6) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 120.1(7) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 118.6(6) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N2 C5 C4 121.9(5) . . ? N2 C5 C6 114.1(6) . . ? C4 C5 C6 124.0(6) . . ? N3 C6 C7 119.9(5) . . ? N3 C6 C5 113.6(5) . . ? C7 C6 C5 126.5(6) . . ? C6 C7 C8 120.3(6) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 117.9(5) . . ? C9 C8 C16 122.8(5) . . ? C7 C8 C16 119.3(5) . . ? C10 C9 C8 120.8(5) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? N3 C10 C9 119.2(5) . . ? N3 C10 C11 112.4(5) . . ? C9 C10 C11 128.4(6) . . ? N4 C11 C12 120.7(6) . . ? N4 C11 C10 115.4(5) . . ? C12 C11 C10 123.9(6) . . ? C11 C12 C13 119.8(6) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 118.2(6) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C15 C14 C13 120.3(6) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? N4 C15 C14 121.4(6) . . ? N4 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C21 116.2(5) . . ? C17 C16 C8 121.3(5) . . ? C21 C16 C8 122.6(5) . . ? C18 C17 C16 122.5(6) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C17 C18 C19 121.3(6) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? N5 C19 C18 121.5(6) . . ? N5 C19 C20 121.7(5) . . ? C18 C19 C20 116.7(5) . . ? C21 C20 C19 121.0(5) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C16 122.3(6) . . ? C20 C21 H21 118.9 . . ? C16 C21 H21 118.9 . . ? C23 C22 N5 111.1(7) . . ? C23 C22 H22A 109.4 . . ? N5 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? N5 C22 H22B 109.4 . . ? H22A C22 H22B 108 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C25 112.2(6) . . ? N5 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? N5 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C1 N2 C5 118.1(6) . . ? C1 N2 Ru1 127.3(5) . . ? C5 N2 Ru1 114.6(4) . . ? C6 N3 C10 121.9(5) . . ? C6 N3 Ru1 118.7(4) . . ? C10 N3 Ru1 119.2(4) . . ? C15 N4 C11 119.6(6) . . ? C15 N4 Ru1 125.8(4) . . ? C11 N4 Ru1 114.5(4) . . ? C19 N5 C24 121.7(5) . . ? C19 N5 C22 121.8(5) . . ? C24 N5 C22 116.5(5) . . ? N1 Ru1 N1' 78.6(8) . . ? N1 Ru1 N3 178.0(4) . . ? N1' Ru1 N3 100.3(7) . . ? N1 Ru1 N2 99.7(3) . . ? N1' Ru1 N2 96.8(7) . . ? N3 Ru1 N2 78.8(2) . . ? N1 Ru1 N4 103.3(3) . . ? N1' Ru1 N4 91.3(7) . . ? N3 Ru1 N4 78.34(19) . . ? N2 Ru1 N4 156.77(19) . . ? N1 Ru1 Cl2 92.8(3) . . ? N1' Ru1 Cl2 15.4(7) . . ? N3 Ru1 Cl2 86.01(17) . . ? N2 Ru1 Cl2 88.45(16) . . ? N4 Ru1 Cl2 94.00(15) . . ? N1 Ru1 Cl1 91.7(3) . . ? N1' Ru1 Cl1 169.7(7) . . ? N3 Ru1 Cl1 89.46(16) . . ? N2 Ru1 Cl1 88.22(15) . . ? N4 Ru1 Cl1 87.51(14) . . ? Cl2 Ru1 Cl1 174.83(9) . . ? N1 Ru1 Cl2' 5.9(4) . . ? N1' Ru1 Cl2' 81.8(8) . . ? N3 Ru1 Cl2' 176.0(2) . . ? N2 Ru1 Cl2' 104.4(2) . . ? N4 Ru1 Cl2' 98.3(2) . . ? Cl2 Ru1 Cl2' 96.4(2) . . ? Cl1 Ru1 Cl2' 88.3(2) . . ? O1 N1 Ru1 171.5(10) . . ? O1' N1' Ru1 175(2) . . ? F6 P1 F2 91.9(7) . . ? F6 P1 F3 91.3(8) . . ? F2 P1 F3 92.1(8) . . ? F6 P1 F4 89.4(6) . . ? F2 P1 F4 177.3(8) . . ? F3 P1 F4 90.2(8) . . ? F6 P1 F1 89.7(7) . . ? F2 P1 F1 89.4(7) . . ? F3 P1 F1 178.1(9) . . ? F4 P1 F1 88.2(6) . . ? F6 P1 F5 178.1(9) . . ? F2 P1 F5 88.3(7) . . ? F3 P1 F5 90.6(8) . . ? F4 P1 F5 90.3(7) . . ? F1 P1 F5 88.4(8) . . ? F6' P1' F4' 90.2(9) . . ? F6' P1' F2' 89.7(9) . . ? F4' P1' F2' 177.8(12) . . ? F6' P1' F1' 90.5(9) . . ? F4' P1' F1' 91.3(10) . . ? F2' P1' F1' 90.8(9) . . ? F6' P1' F5' 178.9(11) . . ? F4' P1' F5' 90.7(10) . . ? F2' P1' F5' 89.3(10) . . ? F1' P1' F5' 89.0(11) . . ? F6' P1' F3' 91.5(11) . . ? F4' P1' F3' 87.3(10) . . ? F2' P1' F3' 90.5(10) . . ? F1' P1' F3' 177.6(12) . . ? F5' P1' F3' 89.0(11) . . ? _database_code_depnum_ccdc_archive 'CCDC 939960'