# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2203 data_[Ru([9]aneS3)(dipa)Cl]PF6 #6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H21 Cl F6 N3 P Ru S3' _chemical_formula_weight 633.03 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' 0.0000 0.0000 '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' 'Ru' 'Ru' -1.2594 0.8363 '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' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 7.698(11) _cell_length_b 15.134(17) _cell_length_c 19.061(23) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2221(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.241 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3769 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.98 _reflns_number_total 1810 _reflns_number_gt 1448 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+4.3412P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1810 _refine_ls_number_parameters 151 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.59578(8) 0.54287(3) 0.2500 0.0237(3) Uani 1 d S . . Cl Cl 0.7941(3) 0.41629(11) 0.2500 0.0383(5) Uani 1 d S . . S1 S 0.4069(3) 0.65932(11) 0.2500 0.0313(5) Uani 1 d S . . C2 C 0.4723(17) 0.7281(7) 0.3217(5) 0.112(5) Uani 1 d . . . H2A H 0.4873 0.7874 0.3034 0.134 Uiso 1 calc R . . H2B H 0.3759 0.7303 0.3544 0.134 Uiso 1 calc R . . C3 C 0.6219(12) 0.7077(5) 0.3606(4) 0.067(2) Uani 1 d . . . H3A H 0.5857 0.6963 0.4085 0.080 Uiso 1 calc R . . H3B H 0.6942 0.7601 0.3615 0.080 Uiso 1 calc R . . S4 S 0.7564(2) 0.61700(9) 0.33352(8) 0.0401(4) Uani 1 d . . . C5 C 0.9228(12) 0.6776(6) 0.2865(5) 0.091(4) Uani 1 d . . . H5A H 0.9165 0.7387 0.3017 0.109 Uiso 1 calc R . . H5B H 1.0345 0.6549 0.3017 0.109 Uiso 1 calc R . . N31 N 0.1963(9) 0.4728(4) 0.2500 0.0314(14) Uani 1 d SD . . H31 H 0.086(2) 0.462(5) 0.2500 0.038 Uiso 1 d SD . . C16 C 0.2742(7) 0.4614(3) 0.3163(3) 0.0267(11) Uani 1 d . . . N11 N 0.4432(6) 0.4749(3) 0.3249(2) 0.0273(10) Uani 1 d . . . C12 C 0.5134(9) 0.4531(3) 0.3878(3) 0.0352(13) Uani 1 d . . . H12 H 0.6331 0.4573 0.3936 0.042 Uiso 1 calc R . . C13 C 0.4132(10) 0.4248(4) 0.4439(3) 0.0442(16) Uani 1 d . . . H13 H 0.4649 0.4098 0.4863 0.053 Uiso 1 calc R . . C14 C 0.2347(11) 0.4192(4) 0.4356(4) 0.0534(19) Uani 1 d . . . H14 H 0.1639 0.4045 0.4733 0.064 Uiso 1 calc R . . C15 C 0.1642(10) 0.4358(4) 0.3709(3) 0.0423(15) Uani 1 d . . . H15 H 0.0453 0.4301 0.3636 0.051 Uiso 1 calc R . . P P 1.1530(4) 0.7500 0.0000 0.0620(8) Uani 1 d S . . F1 F 1.1536(11) 0.8098(5) 0.0663(4) 0.132(3) Uani 1 d . . . F2 F 0.9480(12) 0.7500 0.0000 0.184(7) Uani 1 d S . . F3 F 1.1520(16) 0.6652(5) 0.0437(5) 0.166(4) Uani 1 d . . . F4 F 1.3578(10) 0.7500 0.0000 0.0758(18) Uani 1 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0171(4) 0.0213(3) 0.0325(4) 0.000 0.000 -0.0018(2) Cl 0.0202(10) 0.0284(9) 0.0664(14) 0.000 0.000 0.0016(7) S1 0.0224(10) 0.0250(8) 0.0467(11) 0.000 0.000 0.0019(7) C2 0.130(10) 0.100(7) 0.106(7) -0.075(6) -0.077(8) 0.080(7) C3 0.051(5) 0.086(5) 0.062(5) -0.046(4) -0.001(4) 0.005(4) S4 0.0365(9) 0.0317(7) 0.0521(9) -0.0009(6) -0.0162(8) -0.0061(6) C5 0.045(5) 0.109(6) 0.119(8) -0.066(5) 0.022(5) -0.046(5) N31 0.021(4) 0.037(3) 0.037(4) 0.000 0.000 -0.004(3) C16 0.024(3) 0.025(2) 0.031(3) 0.0019(18) 0.001(2) 0.0008(18) N11 0.028(3) 0.0219(19) 0.032(2) -0.0025(16) -0.001(2) -0.0033(16) C12 0.042(4) 0.029(3) 0.035(3) 0.004(2) -0.011(3) -0.003(2) C13 0.070(5) 0.038(3) 0.025(3) 0.002(2) 0.000(3) -0.007(3) C14 0.069(6) 0.051(4) 0.040(3) 0.003(3) 0.017(4) -0.015(3) C15 0.036(4) 0.046(3) 0.045(4) 0.001(3) 0.009(3) -0.011(3) P 0.0416(17) 0.0626(16) 0.082(2) -0.0340(15) 0.000 0.000 F1 0.087(5) 0.173(6) 0.137(6) -0.101(5) -0.017(5) 0.022(5) F2 0.046(6) 0.162(9) 0.343(19) -0.169(12) 0.000 0.000 F3 0.172(10) 0.117(6) 0.208(9) 0.056(5) 0.067(8) -0.015(5) F4 0.037(4) 0.105(5) 0.086(5) -0.012(4) 0.000 0.000 _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 Ru N11 2.116(5) 6_556 ? Ru N11 2.116(5) . ? Ru S1 2.285(3) . ? Ru S4 2.307(2) . ? Ru S4 2.307(2) 6_556 ? Ru Cl 2.450(3) . ? S1 C2 1.790(8) . ? S1 C2 1.790(8) 6_556 ? C2 C3 1.403(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.795(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.813(9) . ? C5 C5 1.39(2) 6_556 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N31 C16 1.409(6) . ? N31 C16 1.409(6) 6_556 ? N31 H31 0.861(11) . ? C16 N11 1.328(7) . ? C16 C15 1.397(8) . ? N11 C12 1.356(7) . ? C12 C13 1.385(9) . ? C12 H12 0.9300 . ? C13 C14 1.386(11) . ? C13 H13 0.9300 . ? C14 C15 1.369(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? P F3 1.530(7) 3_565 ? P F3 1.530(7) . ? P F1 1.555(5) 3_565 ? P F1 1.555(5) . ? P F4 1.577(8) . ? P F2 1.578(10) . ? 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 N11 Ru N11 84.9(2) 6_556 . ? N11 Ru S1 91.23(14) 6_556 . ? N11 Ru S1 91.23(14) . . ? N11 Ru S4 178.62(13) 6_556 . ? N11 Ru S4 93.90(15) . . ? S1 Ru S4 88.06(9) . . ? N11 Ru S4 93.90(15) 6_556 6_556 ? N11 Ru S4 178.62(13) . 6_556 ? S1 Ru S4 88.06(9) . 6_556 ? S4 Ru S4 87.27(12) . 6_556 ? N11 Ru Cl 88.05(14) 6_556 . ? N11 Ru Cl 88.05(14) . . ? S1 Ru Cl 179.02(7) . . ? S4 Ru Cl 92.65(9) . . ? S4 Ru Cl 92.65(9) 6_556 . ? C2 S1 C2 99.6(9) . 6_556 ? C2 S1 Ru 105.6(3) . . ? C2 S1 Ru 105.6(3) 6_556 . ? C3 C2 S1 120.4(6) . . ? C3 C2 H2A 107.2 . . ? S1 C2 H2A 107.2 . . ? C3 C2 H2B 107.2 . . ? S1 C2 H2B 107.2 . . ? H2A C2 H2B 106.9 . . ? C2 C3 S4 119.3(5) . . ? C2 C3 H3A 107.5 . . ? S4 C3 H3A 107.5 . . ? C2 C3 H3B 107.5 . . ? S4 C3 H3B 107.5 . . ? H3A C3 H3B 107.0 . . ? C3 S4 C5 99.4(5) . . ? C3 S4 Ru 105.1(3) . . ? C5 S4 Ru 106.5(3) . . ? C5 C5 S4 119.7(3) 6_556 . ? C5 C5 H5A 107.4 6_556 . ? S4 C5 H5A 107.4 . . ? C5 C5 H5B 107.4 6_556 . ? S4 C5 H5B 107.4 . . ? H5A C5 H5B 106.9 . . ? C16 N31 C16 127.4(7) . 6_556 ? C16 N31 H31 113.3(12) . . ? C16 N31 H31 113.3(12) 6_556 . ? N11 C16 C15 123.0(5) . . ? N11 C16 N31 120.6(5) . . ? C15 C16 N31 116.4(6) . . ? C16 N11 C12 117.5(5) . . ? C16 N11 Ru 122.4(4) . . ? C12 N11 Ru 119.6(4) . . ? N11 C12 C13 122.4(6) . . ? N11 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C12 C13 C14 118.9(6) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 119.0(6) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 118.8(7) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? F3 P F3 179.4(10) 3_565 . ? F3 P F1 92.6(5) 3_565 3_565 ? F3 P F1 87.4(5) . 3_565 ? F3 P F1 87.4(5) 3_565 . ? F3 P F1 92.6(5) . . ? F1 P F1 179.6(6) 3_565 . ? F3 P F4 90.3(5) 3_565 . ? F3 P F4 90.3(5) . . ? F1 P F4 89.8(3) 3_565 . ? F1 P F4 89.8(3) . . ? F3 P F2 89.7(5) 3_565 . ? F3 P F2 89.7(5) . . ? F1 P F2 90.2(3) 3_565 . ? F1 P F2 90.2(3) . . ? F4 P F2 180.0 . . ? _diffrn_measured_fraction_theta_max 0.724 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.724 _refine_diff_density_max 0.739 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.114 #===END data_[Ru([9]aneS3)(bpym)Cl]PF6 #7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 Cl F6 N4 P Ru S3' _chemical_formula_weight 619.99 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' 0.0000 0.0000 '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' '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.914(11) _cell_length_b 11.821(14) _cell_length_c 10.167(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.370(10) _cell_angle_gamma 90.00 _cell_volume 1050(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3716 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.95 _reflns_number_total 2145 _reflns_number_gt 1662 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+1.6479P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2145 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.31756(6) 0.2500 0.23862(5) 0.0290(2) Uani 1 d S . . Cl Cl 0.5957(2) 0.2500 0.25560(18) 0.0377(4) Uani 1 d S . . S1 S 0.0594(2) 0.2500 0.2349(2) 0.0431(5) Uani 1 d S . . C2 C 0.0318(7) 0.1286(6) 0.3396(7) 0.0646(18) Uani 1 d . . . H2A H -0.0593 0.1419 0.3761 0.078 Uiso 1 calc R . . H2B H 0.0127 0.0623 0.2826 0.078 Uiso 1 calc R . . C3 C 0.1609(7) 0.1024(5) 0.4534(7) 0.0587(16) Uani 1 d . . . H3A H 0.1494 0.0257 0.4839 0.070 Uiso 1 calc R . . H3B H 0.1561 0.1531 0.5274 0.070 Uiso 1 calc R . . S4 S 0.34750(15) 0.11642(10) 0.40665(12) 0.0368(3) Uani 1 d . . . C5 C 0.4555(8) 0.1884(5) 0.5538(5) 0.0621(18) Uani 1 d . . . H5A H 0.4162 0.1633 0.6313 0.075 Uiso 1 calc R . . H5B H 0.5610 0.1633 0.5664 0.075 Uiso 1 calc R . . N11 N 0.3034(4) 0.1377(3) 0.0751(4) 0.0280(8) Uani 1 d . . . C12 C 0.2858(6) 0.0247(4) 0.0736(5) 0.0388(12) Uani 1 d . . . H12 H 0.2680 -0.0120 0.1499 0.047 Uiso 1 calc R . . C13 C 0.3281(6) 0.0199(4) -0.1456(5) 0.0436(12) Uani 1 d . . . H13 H 0.3398 -0.0215 -0.2206 0.052 Uiso 1 calc R . . C14 C 0.2938(6) -0.0367(4) -0.0385(5) 0.0445(13) Uani 1 d . . . H14 H 0.2766 -0.1143 -0.0417 0.053 Uiso 1 calc R . . N15 N 0.3455(5) 0.1319(4) -0.1480(4) 0.0400(10) Uani 1 d . . . C16 C 0.3289(5) 0.1871(4) -0.0390(5) 0.0322(11) Uani 1 d . . . P P -0.0976(2) 0.2500 -0.2400(2) 0.0444(5) Uani 1 d S . . F1 F 0.0530(7) 0.2500 -0.2979(6) 0.098(2) Uani 1 d S . . F2 F -0.2485(7) 0.2500 -0.1808(8) 0.107(2) Uani 1 d S . . F3 F -0.0243(5) 0.1568(4) -0.1347(5) 0.1066(17) Uani 1 d . . . F4 F -0.1702(6) 0.1561(5) -0.3388(6) 0.127(2) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0353(3) 0.0267(3) 0.0270(3) 0.000 0.0114(2) 0.000 Cl 0.0388(10) 0.0346(9) 0.0430(10) 0.000 0.0163(8) 0.000 S1 0.0329(10) 0.0509(12) 0.0467(11) 0.000 0.0109(8) 0.000 C2 0.053(4) 0.061(4) 0.089(5) 0.006(4) 0.038(4) -0.018(3) C3 0.062(4) 0.050(3) 0.074(4) 0.013(3) 0.037(3) -0.013(3) S4 0.0495(8) 0.0324(7) 0.0311(6) 0.0058(5) 0.0144(5) -0.0011(6) C5 0.089(5) 0.060(4) 0.028(3) 0.009(3) -0.012(3) -0.013(3) N11 0.033(2) 0.0270(19) 0.0244(19) 0.0001(16) 0.0073(16) -0.0002(16) C12 0.053(3) 0.028(2) 0.036(3) 0.000(2) 0.009(2) -0.005(2) C13 0.053(3) 0.038(3) 0.039(3) -0.009(2) 0.009(2) 0.004(3) C14 0.062(4) 0.028(3) 0.043(3) -0.009(2) 0.009(3) 0.000(2) N15 0.051(3) 0.036(2) 0.035(2) -0.005(2) 0.015(2) 0.000(2) C16 0.038(3) 0.031(3) 0.031(2) 0.000(2) 0.013(2) 0.005(2) P 0.0426(12) 0.0391(11) 0.0516(12) 0.000 0.0098(9) 0.000 F1 0.076(4) 0.151(6) 0.080(4) 0.000 0.042(3) 0.000 F2 0.056(4) 0.134(6) 0.145(6) 0.000 0.050(4) 0.000 F3 0.083(3) 0.105(4) 0.125(4) 0.060(3) 0.003(3) 0.008(3) F4 0.103(4) 0.110(4) 0.152(5) -0.078(4) -0.012(3) -0.004(3) _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 Ru N11 2.112(4) . ? Ru N11 2.112(4) 4_565 ? Ru S1 2.294(3) . ? Ru S4 2.303(2) 4_565 ? Ru S4 2.303(2) . ? Ru Cl 2.452(4) . ? S1 C2 1.833(6) 4_565 ? S1 C2 1.833(6) . ? C2 C3 1.494(9) . ? C3 S4 1.826(6) . ? S4 C5 1.823(6) . ? C5 C5 1.456(12) 4_565 ? N11 C12 1.345(6) . ? N11 C16 1.356(6) . ? C12 C14 1.365(7) . ? C13 N15 1.333(7) . ? C13 C14 1.363(7) . ? N15 C16 1.320(6) . ? C16 C16 1.487(9) 4_565 ? P F4 1.550(5) . ? P F4 1.550(5) 4_565 ? P F1 1.568(6) . ? P F2 1.578(6) . ? P F3 1.584(4) . ? P F3 1.585(4) 4_565 ? 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 N11 Ru N11 77.9(2) . 4_565 ? N11 Ru S1 94.76(11) . . ? N11 Ru S1 94.76(11) 4_565 . ? N11 Ru S4 174.41(11) . 4_565 ? N11 Ru S4 97.67(14) 4_565 4_565 ? S1 Ru S4 88.93(5) . 4_565 ? N11 Ru S4 97.67(14) . . ? N11 Ru S4 174.41(11) 4_565 . ? S1 Ru S4 88.93(5) . . ? S4 Ru S4 86.57(12) 4_565 . ? N11 Ru Cl 87.60(10) . . ? N11 Ru Cl 87.60(10) 4_565 . ? S1 Ru Cl 176.96(7) . . ? S4 Ru Cl 88.86(5) 4_565 . ? S4 Ru Cl 88.86(5) . . ? C2 S1 C2 103.1(5) 4_565 . ? C2 S1 Ru 103.9(2) 4_565 . ? C2 S1 Ru 103.9(2) . . ? C3 C2 S1 116.2(4) . . ? C2 C3 S4 112.5(4) . . ? C5 S4 C3 100.9(3) . . ? C5 S4 Ru 104.7(2) . . ? C3 S4 Ru 106.1(2) . . ? C5 C5 S4 117.84(19) 4_565 . ? C12 N11 C16 117.2(4) . . ? C12 N11 Ru 128.4(3) . . ? C16 N11 Ru 114.1(3) . . ? N11 C12 C14 120.8(5) . . ? N15 C13 C14 123.2(5) . . ? C13 C14 C12 117.5(5) . . ? C16 N15 C13 116.3(4) . . ? N15 C16 N11 124.8(4) . . ? N15 C16 C16 119.6(3) . 4_565 ? N11 C16 C16 115.5(2) . 4_565 ? F4 P F4 91.4(5) . 4_565 ? F4 P F1 92.0(3) . . ? F4 P F1 92.0(3) 4_565 . ? F4 P F2 88.2(3) . . ? F4 P F2 88.2(3) 4_565 . ? F1 P F2 179.7(4) . . ? F4 P F3 90.2(3) . . ? F4 P F3 178.0(3) 4_565 . ? F1 P F3 89.1(3) . . ? F2 P F3 90.7(3) . . ? F4 P F3 178.0(3) . 4_565 ? F4 P F3 90.2(3) 4_565 4_565 ? F1 P F3 89.1(3) . 4_565 ? F2 P F3 90.7(3) . 4_565 ? F3 P F3 88.1(4) . 4_565 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.660 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.111 #===END data_[Ru([9]aneS3)(tpy)Cl]PF6 #8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H23 Cl F6 N3 P Ru S3' _chemical_formula_weight 695.09 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' 0.0000 0.0000 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 14.866(17) _cell_length_b 17.311(20) _cell_length_c 20.639(24) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5311(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 1.046 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16364 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.96 _reflns_number_total 5069 _reflns_number_gt 3735 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+9.5828P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00056(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5069 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.38934(2) 0.03336(2) 0.293595(16) 0.02596(14) Uani 1 d . . . S1 S 0.28943(8) -0.01880(8) 0.36512(6) 0.0406(3) Uani 1 d . . . C2 C 0.2161(6) 0.0592(5) 0.3899(4) 0.104(3) Uani 1 d . . . H2A H 0.1573 0.0499 0.3711 0.125 Uiso 1 calc R . . H2B H 0.2094 0.0565 0.4366 0.125 Uiso 1 calc R . . C3 C 0.2420(5) 0.1343(4) 0.3739(5) 0.102(3) Uani 1 d . . . H3A H 0.2717 0.1563 0.4115 0.122 Uiso 1 calc R . . H3B H 0.1877 0.1641 0.3667 0.122 Uiso 1 calc R . . S4 S 0.31562(9) 0.14934(7) 0.30406(7) 0.0451(3) Uani 1 d . . . C5 C 0.2343(8) 0.1531(4) 0.2400(5) 0.144(5) Uani 1 d . . . H5A H 0.1752 0.1540 0.2599 0.173 Uiso 1 calc R . . H5B H 0.2419 0.2022 0.2180 0.173 Uiso 1 calc R . . C6 C 0.2331(4) 0.0976(4) 0.1940(3) 0.0620(17) Uani 1 d . . . H6A H 0.2607 0.1188 0.1554 0.074 Uiso 1 calc R . . H6B H 0.1706 0.0871 0.1836 0.074 Uiso 1 calc R . . S7 S 0.28785(7) 0.00468(7) 0.21119(5) 0.0326(3) Uani 1 d . . . C8 C 0.1970(4) -0.0489(4) 0.2511(3) 0.0575(16) Uani 1 d . . . H8A H 0.1441 -0.0161 0.2520 0.069 Uiso 1 calc R . . H8B H 0.1827 -0.0934 0.2244 0.069 Uiso 1 calc R . . C9 C 0.2134(5) -0.0749(5) 0.3142(3) 0.090(3) Uani 1 d . . . H9A H 0.2371 -0.1270 0.3113 0.108 Uiso 1 calc R . . H9B H 0.1560 -0.0782 0.3364 0.108 Uiso 1 calc R . . N11 N 0.4819(2) 0.0554(2) 0.36766(18) 0.0334(9) Uani 1 d . . . C12 C 0.4999(3) 0.1247(3) 0.3945(2) 0.0418(12) Uani 1 d . . . H12 H 0.4701 0.1681 0.3789 0.050 Uiso 1 calc R . . C13 C 0.5609(4) 0.1337(3) 0.4443(2) 0.0493(13) Uani 1 d . . . H13 H 0.5711 0.1822 0.4622 0.059 Uiso 1 calc R . . C14 C 0.6064(4) 0.0704(4) 0.4670(2) 0.0523(15) Uani 1 d . . . H14 H 0.6479 0.0755 0.5005 0.063 Uiso 1 calc R . . C15 C 0.5899(3) -0.0015(3) 0.4395(2) 0.0461(13) Uani 1 d . . . H15 H 0.6203 -0.0451 0.4542 0.055 Uiso 1 calc R . . C16 C 0.5273(3) -0.0072(3) 0.3900(2) 0.0357(11) Uani 1 d . . . N21 N 0.4634(2) -0.0733(2) 0.29767(17) 0.0282(8) Uani 1 d . . . C22 C 0.5087(3) -0.0809(3) 0.3553(2) 0.0338(10) Uani 1 d . . . C23 C 0.5388(4) -0.1510(3) 0.3782(3) 0.0501(14) Uani 1 d . . . H23 H 0.5681 -0.1542 0.4180 0.060 Uiso 1 calc R . . C24 C 0.5248(4) -0.2165(3) 0.3415(3) 0.0581(16) Uani 1 d . . . H24 H 0.5416 -0.2649 0.3571 0.070 Uiso 1 calc R . . C25 C 0.4858(4) -0.2090(3) 0.2817(3) 0.0512(14) Uani 1 d . . . H25 H 0.4791 -0.2522 0.2554 0.061 Uiso 1 calc R . . C26 C 0.4560(3) -0.1369(3) 0.2598(2) 0.0355(10) Uani 1 d . . . N31 N 0.3493(4) -0.1804(3) 0.1819(2) 0.0566(13) Uani 1 d . . . C32 C 0.4173(3) -0.1323(3) 0.1937(2) 0.0360(11) Uani 1 d . . . C33 C 0.4545(4) -0.0854(3) 0.1466(3) 0.0472(13) Uani 1 d . . . H33 H 0.5020 -0.0525 0.1564 0.057 Uiso 1 calc R . . C34 C 0.4198(5) -0.0884(4) 0.0844(3) 0.0612(16) Uani 1 d . . . H34 H 0.4443 -0.0583 0.0515 0.073 Uiso 1 calc R . . C35 C 0.3491(5) -0.1364(4) 0.0723(3) 0.076(2) Uani 1 d . . . H35 H 0.3238 -0.1388 0.0312 0.091 Uiso 1 calc R . . C36 C 0.3160(5) -0.1806(4) 0.1214(3) 0.073(2) Uani 1 d . . . H36 H 0.2675 -0.2129 0.1126 0.088 Uiso 1 calc R . . Cl Cl 0.49451(8) 0.09126(7) 0.21733(6) 0.0412(3) Uani 1 d . . . P P 0.14980(11) -0.19108(9) 0.48740(7) 0.0524(4) Uani 1 d . . . F1 F 0.1442(3) -0.1011(2) 0.4736(2) 0.0860(12) Uani 1 d . . . F2 F 0.1140(3) -0.2078(2) 0.41654(18) 0.0923(14) Uani 1 d . . . F3 F 0.0503(3) -0.1908(3) 0.5139(2) 0.1013(15) Uani 1 d . . . F4 F 0.1554(3) -0.2832(2) 0.50031(19) 0.0805(11) Uani 1 d . . . F5 F 0.1858(4) -0.1766(3) 0.55803(19) 0.1076(16) Uani 1 d . . . F6 F 0.2502(3) -0.1928(3) 0.4606(2) 0.0985(14) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0219(2) 0.0261(2) 0.0299(2) 0.00135(14) -0.00414(15) -0.00010(13) S1 0.0311(6) 0.0582(8) 0.0325(6) 0.0071(5) 0.0006(5) -0.0012(6) C2 0.144(8) 0.101(6) 0.069(4) 0.020(4) 0.063(5) 0.061(6) C3 0.081(5) 0.066(5) 0.158(8) -0.046(5) 0.070(6) -0.006(4) S4 0.0384(7) 0.0327(7) 0.0642(9) -0.0072(6) -0.0091(6) 0.0079(5) C5 0.210(11) 0.058(5) 0.165(9) -0.033(5) -0.145(9) 0.070(6) C6 0.067(4) 0.059(4) 0.060(4) 0.007(3) -0.029(3) 0.021(3) S7 0.0257(6) 0.0408(7) 0.0312(6) 0.0016(5) -0.0054(5) 0.0003(5) C8 0.051(3) 0.073(4) 0.048(3) -0.003(3) 0.000(3) -0.031(3) C9 0.073(5) 0.132(7) 0.065(4) 0.029(4) -0.014(4) -0.070(5) N11 0.0284(19) 0.041(2) 0.0308(19) -0.0048(17) -0.0020(17) -0.0030(17) C12 0.042(3) 0.040(3) 0.043(3) -0.008(2) -0.007(2) -0.003(2) C13 0.049(3) 0.058(4) 0.040(3) -0.013(3) -0.004(3) -0.014(3) C14 0.045(3) 0.077(4) 0.035(3) -0.002(3) -0.011(2) -0.021(3) C15 0.044(3) 0.057(3) 0.038(3) 0.008(2) -0.010(2) -0.006(2) C16 0.033(2) 0.039(3) 0.035(2) 0.005(2) 0.000(2) -0.001(2) N21 0.0210(17) 0.030(2) 0.0337(19) 0.0034(15) -0.0017(16) -0.0025(15) C22 0.028(2) 0.039(3) 0.034(2) 0.0065(19) -0.004(2) 0.0028(19) C23 0.053(3) 0.047(3) 0.051(3) 0.015(3) -0.017(3) 0.011(3) C24 0.073(4) 0.036(3) 0.065(4) 0.005(3) -0.019(3) 0.014(3) C25 0.063(4) 0.033(3) 0.058(3) -0.004(2) -0.015(3) 0.005(3) C26 0.037(3) 0.029(2) 0.040(3) 0.002(2) -0.005(2) -0.001(2) N31 0.070(3) 0.046(3) 0.053(3) 0.003(2) -0.022(3) -0.019(3) C32 0.038(3) 0.029(2) 0.041(3) -0.007(2) -0.006(2) 0.002(2) C33 0.041(3) 0.051(3) 0.050(3) -0.004(2) 0.001(3) -0.003(2) C34 0.075(4) 0.071(4) 0.038(3) 0.002(3) 0.007(3) 0.006(3) C35 0.101(6) 0.085(5) 0.041(3) -0.009(3) -0.015(4) -0.004(4) C36 0.092(5) 0.062(4) 0.065(4) -0.001(3) -0.038(4) -0.026(4) Cl 0.0326(6) 0.0360(6) 0.0551(7) 0.0097(5) 0.0039(5) -0.0044(5) P 0.0578(9) 0.0576(9) 0.0419(8) 0.0112(6) -0.0048(7) -0.0108(7) F1 0.126(3) 0.049(2) 0.083(3) 0.0081(19) 0.007(3) -0.008(2) F2 0.138(4) 0.086(3) 0.053(2) 0.005(2) -0.030(2) -0.019(3) F3 0.071(3) 0.114(4) 0.119(4) 0.039(3) 0.019(3) 0.007(3) F4 0.094(3) 0.065(2) 0.082(3) 0.026(2) 0.003(2) -0.007(2) F5 0.140(4) 0.126(4) 0.057(2) -0.013(2) -0.040(3) 0.016(3) F6 0.068(3) 0.094(3) 0.134(4) -0.008(3) 0.025(3) -0.020(2) _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 Ru N11 2.092(4) . ? Ru N21 2.152(4) . ? Ru S1 2.280(2) . ? Ru S4 2.297(2) . ? Ru S7 2.327(2) . ? Ru Cl 2.434(2) . ? S1 C2 1.808(7) . ? S1 C9 1.824(7) . ? C2 C3 1.396(10) . ? C3 S4 1.828(8) . ? S4 C5 1.793(7) . ? C5 C6 1.350(9) . ? C6 S7 1.837(6) . ? S7 C8 1.833(5) . ? C8 C9 1.400(8) . ? N11 C12 1.348(6) . ? N11 C16 1.358(6) . ? C12 C13 1.379(7) . ? C13 C14 1.370(8) . ? C14 C15 1.389(8) . ? C15 C16 1.386(7) . ? C16 C22 1.489(7) . ? N21 C26 1.355(6) . ? N21 C22 1.373(6) . ? C22 C23 1.377(7) . ? C23 C24 1.379(8) . ? C24 C25 1.371(8) . ? C25 C26 1.399(7) . ? C26 C32 1.483(7) . ? N31 C32 1.333(6) . ? N31 C36 1.342(8) . ? C32 C33 1.381(7) . ? C33 C34 1.384(8) . ? C34 C35 1.363(9) . ? C35 C36 1.363(9) . ? P F5 1.573(4) . ? P F3 1.576(5) . ? P F2 1.583(4) . ? P F1 1.585(4) . ? P F6 1.593(5) . ? P F4 1.619(4) . ? 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 N11 Ru N21 77.96(15) . . ? N11 Ru S1 91.58(14) . . ? N21 Ru S1 88.19(12) . . ? N11 Ru S4 94.90(12) . . ? N21 Ru S4 172.06(10) . . ? S1 Ru S4 88.54(8) . . ? N11 Ru S7 178.17(11) . . ? N21 Ru S7 100.22(11) . . ? S1 Ru S7 88.08(10) . . ? S4 Ru S7 86.90(7) . . ? N11 Ru Cl 88.56(14) . . ? N21 Ru Cl 92.85(11) . . ? S1 Ru Cl 178.96(5) . . ? S4 Ru Cl 90.42(8) . . ? S7 Ru Cl 91.81(9) . . ? C2 S1 C9 100.8(5) . . ? C2 S1 Ru 106.3(3) . . ? C9 S1 Ru 104.0(2) . . ? C3 C2 S1 117.5(6) . . ? C2 C3 S4 119.0(5) . . ? C5 S4 C3 100.6(6) . . ? C5 S4 Ru 106.5(2) . . ? C3 S4 Ru 103.6(3) . . ? C6 C5 S4 120.1(5) . . ? C5 C6 S7 118.8(5) . . ? C8 S7 C6 101.7(3) . . ? C8 S7 Ru 104.9(2) . . ? C6 S7 Ru 104.0(2) . . ? C9 C8 S7 116.9(4) . . ? C8 C9 S1 118.2(5) . . ? C12 N11 C16 118.1(4) . . ? C12 N11 Ru 126.4(3) . . ? C16 N11 Ru 115.4(3) . . ? N11 C12 C13 122.5(5) . . ? C14 C13 C12 119.3(5) . . ? C13 C14 C15 119.3(5) . . ? C16 C15 C14 118.9(5) . . ? N11 C16 C15 121.8(5) . . ? N11 C16 C22 115.4(4) . . ? C15 C16 C22 122.7(4) . . ? C26 N21 C22 117.5(4) . . ? C26 N21 Ru 129.3(3) . . ? C22 N21 Ru 111.6(3) . . ? N21 C22 C23 122.8(5) . . ? N21 C22 C16 115.2(4) . . ? C23 C22 C16 122.0(4) . . ? C22 C23 C24 119.2(5) . . ? C25 C24 C23 118.7(5) . . ? C24 C25 C26 120.7(5) . . ? N21 C26 C25 120.8(4) . . ? N21 C26 C32 121.2(4) . . ? C25 C26 C32 117.9(4) . . ? C32 N31 C36 116.9(5) . . ? N31 C32 C33 122.8(5) . . ? N31 C32 C26 115.4(4) . . ? C33 C32 C26 121.6(4) . . ? C32 C33 C34 118.8(5) . . ? C35 C34 C33 118.6(6) . . ? C36 C35 C34 119.1(6) . . ? N31 C36 C35 123.8(6) . . ? F5 P F3 89.9(3) . . ? F5 P F2 178.6(3) . . ? F3 P F2 90.3(3) . . ? F5 P F1 91.6(3) . . ? F3 P F1 90.6(3) . . ? F2 P F1 89.8(2) . . ? F5 P F6 90.3(3) . . ? F3 P F6 179.1(3) . . ? F2 P F6 89.5(3) . . ? F1 P F6 90.3(2) . . ? F5 P F4 89.2(3) . . ? F3 P F4 89.6(2) . . ? F2 P F4 89.4(2) . . ? F1 P F4 179.1(2) . . ? F6 P F4 89.5(2) . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 1.073 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.104 #===END data_[Ru([9]aneS3)(bq)Cl]PF6.CH3CN #9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H27 Cl F6 N3 P Ru S3' _chemical_formula_weight 759.18 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' 0.0000 0.0000 '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' 'Ru' 'Ru' -1.2594 0.8363 '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' 'S' 'S' 0.1246 0.1234 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.930(11) _cell_length_b 30.024(37) _cell_length_c 12.918(14) _cell_angle_alpha 90.00 _cell_angle_beta 105.750(10) _cell_angle_gamma 90.00 _cell_volume 2960(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.947 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5732 _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_sigmaI/netI 0.1660 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.12 _reflns_number_total 3297 _reflns_number_gt 1552 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.1533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3297 _refine_ls_number_parameters 309 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.2181 _refine_ls_R_factor_gt 0.0936 _refine_ls_wR_factor_ref 0.2801 _refine_ls_wR_factor_gt 0.2305 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.03984(17) 0.93120(5) 0.26776(14) 0.0459(7) Uani 1 d . . . Cl Cl -0.2156(5) 0.97725(16) 0.2674(5) 0.0598(16) Uani 1 d . . . S1 S 0.2761(6) 0.88629(16) 0.2761(5) 0.0557(16) Uani 1 d . . . C2 C 0.210(3) 0.8321(6) 0.317(2) 0.088(8) Uani 1 d . . . H2A H 0.1479 0.8159 0.2534 0.106 Uiso 1 calc R . . H2B H 0.3152 0.8153 0.3512 0.106 Uiso 1 calc R . . C3 C 0.099(3) 0.8337(7) 0.392(2) 0.105(10) Uani 1 d . . . H3A H 0.1745 0.8362 0.4646 0.126 Uiso 1 calc R . . H3B H 0.0368 0.8056 0.3870 0.126 Uiso 1 calc R . . S4 S -0.0592(6) 0.87834(16) 0.3696(5) 0.0574(17) Uani 1 d . . . C5 C -0.007(3) 0.9005(11) 0.503(2) 0.126(12) Uani 1 d . . . H5A H -0.1039 0.9189 0.5088 0.151 Uiso 1 calc R . . H5B H 0.0024 0.8759 0.5523 0.151 Uiso 1 calc R . . C6 C 0.152(3) 0.9267(7) 0.5370(16) 0.078(7) Uani 1 d . . . H6A H 0.2507 0.9068 0.5637 0.093 Uiso 1 calc R . . H6B H 0.1440 0.9458 0.5960 0.093 Uiso 1 calc R . . S7 S 0.1953(6) 0.96114(17) 0.4314(5) 0.0594(16) Uani 1 d . . . C8 C 0.420(3) 0.9452(11) 0.438(3) 0.163(16) Uani 1 d . . . H8A H 0.4689 0.9679 0.4013 0.196 Uiso 1 calc R . . H8B H 0.4872 0.9458 0.5132 0.196 Uiso 1 calc R . . C9 C 0.448(2) 0.9040(7) 0.3960(18) 0.071(7) Uani 1 d . . . H9A H 0.4579 0.8816 0.4515 0.085 Uiso 1 calc R . . H9B H 0.5585 0.9050 0.3778 0.085 Uiso 1 calc R . . N21 N 0.1344(16) 0.9740(4) 0.1602(13) 0.048(4) Uiso 1 d . . . C22 C 0.2139(19) 1.0154(5) 0.1866(16) 0.043(4) Uiso 1 d . . . C23 C 0.314(2) 1.0329(5) 0.1159(17) 0.047(5) Uiso 1 d . . . C24 C 0.310(2) 1.0112(6) 0.0249(17) 0.052(5) Uiso 1 d . . . H24 H 0.3690 1.0235 -0.0217 0.063 Uiso 1 calc R . . C25 C 0.224(2) 0.9719(6) -0.0023(17) 0.059(5) Uiso 1 d . . . H25 H 0.2217 0.9581 -0.0672 0.071 Uiso 1 calc R . . C26 C 0.138(2) 0.9522(6) 0.0695(17) 0.048(5) Uiso 1 d . . . C31 C -0.334(2) 0.8672(5) 0.1338(16) 0.051(5) Uiso 1 d . . . H31 H -0.3341 0.8854 0.1920 0.061 Uiso 1 calc R . . C32 C -0.462(2) 0.8368(6) 0.0981(18) 0.066(6) Uiso 1 d . . . H32 H -0.5520 0.8345 0.1310 0.079 Uiso 1 calc R . . C33 C -0.460(3) 0.8085(6) 0.0119(18) 0.071(6) Uiso 1 d . . . H33 H -0.5506 0.7880 -0.0105 0.085 Uiso 1 calc R . . C34 C -0.331(2) 0.8094(6) -0.0414(16) 0.052(5) Uiso 1 d . . . H34 H -0.3300 0.7890 -0.0954 0.063 Uiso 1 calc R . . C41 C 0.192(2) 1.0424(6) 0.2686(17) 0.062(6) Uani 1 d . . . H41 H 0.1176 1.0324 0.3086 0.074 Uiso 1 calc R . . C42 C 0.269(2) 1.0821(5) 0.2942(18) 0.062(6) Uani 1 d . . . H42 H 0.2409 1.1004 0.3451 0.074 Uiso 1 calc R . . C43 C 0.397(2) 1.0954(6) 0.241(2) 0.062(7) Uani 1 d . . . H43 H 0.4698 1.1195 0.2661 0.075 Uiso 1 calc R . . C44 C 0.410(2) 1.0724(6) 0.153(2) 0.064(7) Uani 1 d . . . H44 H 0.4863 1.0831 0.1157 0.077 Uiso 1 calc R . . N11 N -0.0675(17) 0.9029(4) 0.1099(12) 0.044(4) Uani 1 d . . . C12 C -0.1966(19) 0.8709(5) 0.0800(14) 0.034(5) Uani 1 d . . . C13 C -0.199(2) 0.8434(6) -0.0098(19) 0.061(6) Uani 1 d . . . C14 C -0.071(2) 0.8491(5) -0.0668(16) 0.048(5) Uani 1 d . . . H14 H -0.0655 0.8291 -0.1209 0.058 Uiso 1 calc R . . C15 C 0.043(2) 0.8837(6) -0.0425(16) 0.056(6) Uani 1 d . . . H15 H 0.1215 0.8889 -0.0834 0.067 Uiso 1 calc R . . C16 C 0.044(2) 0.9125(6) 0.0467(17) 0.046(5) Uani 1 d U . . P P 0.1343(6) 0.72053(17) 0.0848(5) 0.071(2) Uani 1 d D . . F11 F 0.263(2) 0.7034(7) 0.1940(13) 0.150(9) Uiso 0.57(3) d PD A 1 F21 F 0.007(2) 0.6794(5) 0.0850(17) 0.150(9) Uiso 0.57(3) d PD A 1 F31 F 0.257(2) 0.7623(5) 0.0866(17) 0.150(9) Uiso 0.57(3) d PD A 1 F41 F 0.003(2) 0.7380(7) -0.0239(13) 0.150(9) Uiso 0.57(3) d PD A 1 F51 F 0.237(3) 0.6927(6) 0.0182(17) 0.150(9) Uiso 0.57(3) d PD A 1 F61 F 0.027(3) 0.7486(6) 0.1516(17) 0.150(9) Uiso 0.57(3) d PD A 1 F12 F 0.186(4) 0.7171(9) 0.2115(10) 0.150(12) Uiso 0.43(3) d PD A 2 F22 F 0.095(4) 0.6686(4) 0.074(2) 0.150(12) Uiso 0.43(3) d PD A 2 F32 F 0.174(4) 0.7726(4) 0.093(2) 0.150(12) Uiso 0.43(3) d PD A 2 F42 F 0.083(4) 0.7242(9) -0.0438(10) 0.150(12) Uiso 0.43(3) d PD A 2 F52 F 0.332(2) 0.7111(9) 0.085(2) 0.150(12) Uiso 0.43(3) d PD A 2 F62 F -0.064(2) 0.7302(9) 0.082(2) 0.150(12) Uiso 0.43(3) d PD A 2 N101 N 0.191(3) 0.7658(9) 0.749(2) 0.148(10) Uani 1 d . . . C102 C 0.203(3) 0.8138(11) 0.749(2) 0.097(11) Uani 1 d . . . C103 C 0.195(3) 0.8510(9) 0.746(2) 0.086(9) Uani 1 d . . . H10A H 0.1077 0.8609 0.7797 0.104 Uiso 1 calc R . . H10B H 0.1644 0.8607 0.6725 0.104 Uiso 1 calc R . . H10C H 0.3067 0.8634 0.7835 0.104 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0385(9) 0.0535(9) 0.0473(15) -0.0015(9) 0.0143(9) 0.0015(6) Cl 0.050(3) 0.069(3) 0.063(5) 0.000(3) 0.021(3) 0.009(2) S1 0.046(3) 0.069(3) 0.050(5) 0.006(3) 0.010(3) 0.010(2) C2 0.099(18) 0.070(14) 0.12(3) 0.004(14) 0.075(18) 0.021(11) C3 0.086(17) 0.061(14) 0.16(3) 0.014(16) 0.029(19) 0.013(11) S4 0.058(3) 0.066(3) 0.053(5) 0.007(3) 0.021(3) 0.002(2) C5 0.084(19) 0.26(4) 0.04(2) 0.00(2) 0.034(18) -0.04(2) C6 0.15(2) 0.075(14) 0.003(15) 0.014(11) 0.005(15) 0.011(14) S7 0.068(3) 0.072(4) 0.036(4) -0.007(3) 0.011(3) -0.003(2) C8 0.10(2) 0.22(3) 0.14(3) -0.09(3) -0.02(2) 0.08(2) C9 0.056(13) 0.092(16) 0.06(2) 0.033(14) 0.014(13) 0.014(11) C41 0.075(14) 0.073(14) 0.040(17) 0.032(12) 0.019(13) -0.008(10) C42 0.054(13) 0.043(11) 0.066(19) 0.002(10) -0.020(13) -0.001(8) C43 0.044(11) 0.051(12) 0.07(2) 0.017(12) -0.013(12) -0.031(9) C44 0.030(11) 0.070(13) 0.08(2) 0.011(14) -0.014(12) 0.012(9) N11 0.042(9) 0.054(9) 0.029(12) 0.009(8) -0.003(9) 0.008(6) C12 0.021(9) 0.058(11) 0.014(14) 0.003(9) -0.014(9) 0.003(7) C13 0.036(12) 0.074(14) 0.07(2) -0.019(13) 0.012(13) 0.016(9) C14 0.045(11) 0.050(11) 0.046(17) -0.007(10) 0.006(12) 0.001(8) C15 0.048(12) 0.087(15) 0.028(16) -0.014(12) 0.005(12) -0.003(10) C16 0.033(7) 0.064(8) 0.049(10) -0.003(7) 0.027(8) 0.004(6) P 0.059(3) 0.072(4) 0.077(6) 0.004(3) 0.011(4) -0.008(2) N101 0.126(19) 0.14(2) 0.18(3) -0.04(2) 0.046(19) 0.000(16) C102 0.086(17) 0.13(3) 0.09(3) 0.00(2) 0.049(17) 0.050(19) C103 0.058(15) 0.16(3) 0.05(2) 0.01(2) 0.034(15) 0.016(16) _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 Ru N11 2.158(15) . ? Ru N21 2.171(14) . ? Ru S1 2.287(5) . ? Ru S7 2.320(6) . ? Ru S4 2.329(6) . ? Ru Cl 2.451(5) . ? S1 C2 1.83(2) . ? S1 C9 1.84(2) . ? C2 C3 1.47(3) . ? C3 S4 1.805(19) . ? S4 C5 1.78(3) . ? C5 C6 1.45(3) . ? C6 S7 1.82(2) . ? S7 C8 1.83(2) . ? C8 C9 1.39(3) . ? N21 C26 1.35(2) . ? N21 C22 1.39(2) . ? C22 C41 1.38(2) . ? C22 C23 1.46(2) . ? C23 C24 1.34(2) . ? C23 C44 1.42(3) . ? C24 C25 1.36(2) . ? C25 C26 1.42(2) . ? C26 C16 1.40(2) . ? C31 C32 1.35(2) . ? C31 C12 1.45(2) . ? C32 C33 1.40(3) . ? C33 C34 1.38(2) . ? C34 C13 1.44(2) . ? C41 C42 1.34(2) . ? C42 C43 1.42(3) . ? C43 C44 1.35(3) . ? N11 C12 1.382(19) . ? N11 C16 1.38(2) . ? C12 C13 1.42(2) . ? C13 C14 1.41(2) . ? C14 C15 1.36(2) . ? C15 C16 1.44(2) . ? P F51 1.577(11) . ? P F12 1.579(11) . ? P F31 1.585(11) . ? P F62 1.587(11) . ? P F11 1.587(11) . ? P F22 1.587(11) . ? P F52 1.591(11) . ? P F32 1.593(11) . ? P F41 1.594(11) . ? P F21 1.595(11) . ? P F42 1.603(11) . ? P F61 1.604(11) . ? N101 C102 1.45(3) . ? C102 C103 1.12(3) . ? 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 N11 Ru N21 75.2(6) . . ? N11 Ru S1 85.5(4) . . ? N21 Ru S1 87.6(4) . . ? N11 Ru S7 171.4(4) . . ? N21 Ru S7 99.4(4) . . ? S1 Ru S7 87.7(2) . . ? N11 Ru S4 99.1(4) . . ? N21 Ru S4 173.2(4) . . ? S1 Ru S4 88.2(2) . . ? S7 Ru S4 85.8(2) . . ? N11 Ru Cl 96.1(4) . . ? N21 Ru Cl 95.4(4) . . ? S1 Ru Cl 176.9(2) . . ? S7 Ru Cl 91.0(2) . . ? S4 Ru Cl 88.87(19) . . ? C2 S1 C9 102.5(11) . . ? C2 S1 Ru 104.1(7) . . ? C9 S1 Ru 106.2(7) . . ? C3 C2 S1 115.4(14) . . ? C2 C3 S4 115.7(17) . . ? C5 S4 C3 98.8(14) . . ? C5 S4 Ru 105.3(9) . . ? C3 S4 Ru 105.6(8) . . ? C6 C5 S4 117.0(16) . . ? C5 C6 S7 113.8(17) . . ? C6 S7 C8 101.2(15) . . ? C6 S7 Ru 107.6(7) . . ? C8 S7 Ru 102.3(10) . . ? C9 C8 S7 118(2) . . ? C8 C9 S1 115.4(16) . . ? C26 N21 C22 122.1(16) . . ? C26 N21 Ru 111.2(11) . . ? C22 N21 Ru 125.6(13) . . ? C41 C22 N21 124.5(17) . . ? C41 C22 C23 118.2(15) . . ? N21 C22 C23 117.0(17) . . ? C24 C23 C44 126.1(19) . . ? C24 C23 C22 119.2(16) . . ? C44 C23 C22 114.7(18) . . ? C23 C24 C25 122.6(19) . . ? C24 C25 C26 119.2(19) . . ? N21 C26 C16 117.5(17) . . ? N21 C26 C25 119.5(16) . . ? C16 C26 C25 122.8(19) . . ? C32 C31 C12 118.7(18) . . ? C31 C32 C33 121(2) . . ? C34 C33 C32 123.5(19) . . ? C33 C34 C13 117.0(18) . . ? C42 C41 C22 124.3(19) . . ? C41 C42 C43 118(2) . . ? C44 C43 C42 119.1(17) . . ? C43 C44 C23 124(2) . . ? C12 N11 C16 121.4(15) . . ? C12 N11 Ru 127.6(12) . . ? C16 N11 Ru 109.0(11) . . ? N11 C12 C13 118.5(16) . . ? N11 C12 C31 121.0(16) . . ? C13 C12 C31 120.4(15) . . ? C14 C13 C12 120.4(17) . . ? C14 C13 C34 120.4(18) . . ? C12 C13 C34 119.2(18) . . ? C15 C14 C13 119.9(18) . . ? C14 C15 C16 119.9(18) . . ? N11 C16 C26 116.3(17) . . ? N11 C16 C15 119.1(16) . . ? C26 C16 C15 124.4(18) . . ? F51 P F12 120.2(10) . . ? F51 P F31 91.2(6) . . ? F12 P F31 92.9(13) . . ? F51 P F62 137.7(10) . . ? F12 P F62 90.7(6) . . ? F31 P F62 117.1(10) . . ? F51 P F11 90.5(5) . . ? F12 P F11 30.0(10) . . ? F31 P F11 89.9(6) . . ? F62 P F11 118.3(10) . . ? F51 P F22 63.4(10) . . ? F12 P F22 90.7(6) . . ? F31 P F22 152.2(10) . . ? F62 P F22 90.4(6) . . ? F11 P F22 79.7(12) . . ? F51 P F52 41.4(10) . . ? F12 P F52 90.7(6) . . ? F31 P F52 62.6(10) . . ? F62 P F52 178.6(7) . . ? F11 P F52 63.0(10) . . ? F22 P F52 89.9(6) . . ? F51 P F32 115.7(10) . . ? F12 P F32 90.2(6) . . ? F31 P F32 27.3(10) . . ? F62 P F32 90.0(6) . . ? F11 P F32 101.0(12) . . ? F22 P F32 179.0(7) . . ? F52 P F32 89.7(6) . . ? F51 P F41 90.4(6) . . ? F12 P F41 149.1(10) . . ? F31 P F41 90.3(5) . . ? F62 P F41 60.8(10) . . ? F11 P F41 179.1(7) . . ? F22 P F41 100.5(12) . . ? F52 P F41 117.8(10) . . ? F32 P F41 78.9(12) . . ? F51 P F21 90.6(5) . . ? F12 P F21 86.2(13) . . ? F31 P F21 178.2(7) . . ? F62 P F21 61.3(10) . . ? F11 P F21 90.1(5) . . ? F22 P F21 29.5(9) . . ? F52 P F21 119.0(10) . . ? F32 P F21 151.0(10) . . ? F41 P F21 89.6(6) . . ? F51 P F42 59.7(10) . . ? F12 P F42 179.7(9) . . ? F31 P F42 86.8(13) . . ? F62 P F42 89.5(6) . . ? F11 P F42 149.9(10) . . ? F22 P F42 89.5(6) . . ? F52 P F42 89.2(6) . . ? F32 P F42 89.6(6) . . ? F41 P F42 31.0(10) . . ? F21 P F42 94.0(13) . . ? F51 P F61 179.2(7) . . ? F12 P F61 60.2(10) . . ? F31 P F61 89.4(5) . . ? F62 P F61 41.5(10) . . ? F11 P F61 90.0(5) . . ? F22 P F61 116.1(10) . . ? F52 P F61 139.3(10) . . ? F32 P F61 64.8(10) . . ? F41 P F61 89.2(5) . . ? F21 P F61 88.8(5) . . ? F42 P F61 119.8(10) . . ? C103 C102 N101 173(3) . . ? _diffrn_measured_fraction_theta_max 0.549 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.549 _refine_diff_density_max 0.700 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.139 #===END data_[Ru([9]aneS3)(dip)Cl]BF4 #11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 B Cl F4 N2 Ru S3' _chemical_formula_weight 736.05 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' 0.0000 0.0000 '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' 'B' 'B' 0.0013 0.0007 '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' 'S' 'S' 0.1246 0.1234 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, -y, z+1/2' _cell_length_a 8.158(10) _cell_length_b 15.575(17) _cell_length_c 24.244(26) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3080(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6794 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.98 _reflns_number_total 3971 _reflns_number_gt 3355 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+7.7421P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(7) _refine_ls_number_reflns 3971 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.80806(7) -0.00586(4) 0.07623(2) 0.0358(2) Uani 1 d . . . Cl Cl 1.1042(2) -0.00352(17) 0.07429(9) 0.0607(5) Uani 1 d . . . S1 S 0.5296(2) -0.01272(14) 0.07559(8) 0.0464(5) Uani 1 d . . . C2 C 0.4875(11) -0.0999(6) 0.0272(4) 0.063(3) Uani 1 d . . . H2A H 0.3764 -0.1199 0.0333 0.075 Uiso 1 calc R . . H2B H 0.4926 -0.0770 -0.0100 0.075 Uiso 1 calc R . . C3 C 0.6025(12) -0.1763(7) 0.0309(4) 0.069(3) Uani 1 d . . . H3A H 0.5925 -0.2107 -0.0023 0.083 Uiso 1 calc R . . H3B H 0.5713 -0.2118 0.0620 0.083 Uiso 1 calc R . . S4 S 0.8142(3) -0.14219(12) 0.03906(7) 0.0461(5) Uani 1 d . . . C5 C 0.8823(13) -0.2092(6) 0.0965(3) 0.067(3) Uani 1 d . . . H5A H 0.8540 -0.2684 0.0886 0.080 Uiso 1 calc R . . H5B H 1.0008 -0.2058 0.0990 0.080 Uiso 1 calc R . . C6 C 0.8121(15) -0.1857(5) 0.1499(3) 0.062(2) Uani 1 d . . . H6A H 0.8762 -0.2124 0.1789 0.075 Uiso 1 calc R . . H6B H 0.7016 -0.2083 0.1521 0.075 Uiso 1 calc R . . S7 S 0.8057(3) -0.06909(12) 0.16201(7) 0.0459(5) Uani 1 d . . . C8 C 0.5947(12) -0.0542(7) 0.1846(4) 0.066(3) Uani 1 d . . . H8A H 0.5721 -0.0946 0.2141 0.079 Uiso 1 calc R . . H8B H 0.5837 0.0032 0.1997 0.079 Uiso 1 calc R . . C9 C 0.4705(12) -0.0657(7) 0.1409(4) 0.071(3) Uani 1 d . . . H9A H 0.3668 -0.0422 0.1534 0.085 Uiso 1 calc R . . H9B H 0.4549 -0.1266 0.1342 0.085 Uiso 1 calc R . . N21 N 0.8172(8) 0.1215(3) 0.10493(19) 0.0342(13) Uani 1 d . . . C22 C 0.8263(11) 0.1483(5) 0.1566(3) 0.047(2) Uani 1 d . . . H22 H 0.8217 0.1078 0.1847 0.057 Uiso 1 calc R . . C23 C 0.8428(10) 0.2353(5) 0.1708(3) 0.049(2) Uani 1 d . . . H23 H 0.8465 0.2513 0.2077 0.058 Uiso 1 calc R . . C24 C 0.8534(9) 0.2969(5) 0.1303(3) 0.0433(19) Uani 1 d . . . C25 C 0.8574(9) 0.2693(4) 0.0740(3) 0.0408(17) Uani 1 d . . . N11 N 0.8131(8) 0.0619(4) 0.0015(2) 0.0340(12) Uani 1 d . . . C12 C 0.8103(11) 0.0312(5) -0.0493(3) 0.0440(17) Uani 1 d . . . H12 H 0.8026 -0.0279 -0.0542 0.053 Uiso 1 calc R . . C13 C 0.8185(12) 0.0836(5) -0.0958(3) 0.051(2) Uani 1 d . . . H13 H 0.8127 0.0591 -0.1307 0.062 Uiso 1 calc R . . C14 C 0.8350(9) 0.1708(5) -0.0908(3) 0.0423(18) Uani 1 d . . . C15 C 0.8499(9) 0.2055(4) -0.0371(3) 0.0401(18) Uani 1 d . . . C16 C 0.8323(9) 0.1496(4) 0.0081(3) 0.0378(17) Uani 1 d . . . C17 C 0.8839(11) 0.2938(5) -0.0241(3) 0.052(2) Uani 1 d . . . H17 H 0.9041 0.3317 -0.0530 0.063 Uiso 1 calc R . . C18 C 0.8876(10) 0.3237(5) 0.0271(3) 0.050(2) Uani 1 d . . . H18 H 0.9104 0.3815 0.0329 0.060 Uiso 1 calc R . . C26 C 0.8358(9) 0.1812(5) 0.0638(3) 0.0389(17) Uani 1 d . . . C31 C 0.8470(10) 0.2273(5) -0.1406(3) 0.048(2) Uani 1 d . . . C32 C 0.9485(11) 0.2011(6) -0.1851(3) 0.054(2) Uani 1 d . . . H32 H 1.0032 0.1487 -0.1840 0.065 Uiso 1 calc R . . C33 C 0.9645(12) 0.2550(7) -0.2303(3) 0.065(3) Uani 1 d . . . H33 H 1.0347 0.2391 -0.2587 0.078 Uiso 1 calc R . . C34 C 0.8797(12) 0.3318(6) -0.2346(4) 0.063(2) Uani 1 d . . . H354 H 0.8931 0.3671 -0.2651 0.076 Uiso 1 calc R . . C35 C 0.7747(12) 0.3545(6) -0.1923(3) 0.061(2) Uani 1 d . . . H35 H 0.7126 0.4044 -0.1951 0.073 Uiso 1 calc R . . C36 C 0.7613(10) 0.3027(5) -0.1452(3) 0.052(2) Uani 1 d . . . H36 H 0.6930 0.3198 -0.1165 0.062 Uiso 1 calc R . . C41 C 0.8668(10) 0.3896(5) 0.1452(3) 0.0451(19) Uani 1 d . . . C42 C 0.9711(13) 0.4161(7) 0.1862(4) 0.067(3) Uani 1 d . . . H42 H 1.0352 0.3759 0.2046 0.080 Uiso 1 calc R . . C43 C 0.9825(15) 0.5014(7) 0.2006(4) 0.080(3) Uani 1 d . . . H43 H 1.0548 0.5185 0.2281 0.096 Uiso 1 calc R . . C44 C 0.8864(16) 0.5613(7) 0.1740(4) 0.085(4) Uani 1 d . . . H44 H 0.8958 0.6190 0.1833 0.102 Uiso 1 calc R . . C45 C 0.7776(15) 0.5367(6) 0.1342(4) 0.074(3) Uani 1 d . . . H45 H 0.7107 0.5773 0.1172 0.088 Uiso 1 calc R . . C46 C 0.7675(12) 0.4509(5) 0.1192(4) 0.062(3) Uani 1 d . . . H46 H 0.6944 0.4340 0.0919 0.074 Uiso 1 calc R . . B B 1.2879(19) -0.3239(8) 0.1475(4) 0.073(3) Uani 1 d . . . F1 F 1.1954(9) -0.3462(4) 0.1030(2) 0.101(2) Uani 1 d . . . F2 F 1.4372(11) -0.2903(6) 0.1368(3) 0.129(3) Uani 1 d . . . F3 F 1.3257(12) -0.4008(5) 0.1747(4) 0.151(4) Uani 1 d . . . F4 F 1.2026(11) -0.2766(6) 0.1835(3) 0.145(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0318(3) 0.0309(4) 0.0446(3) 0.0034(3) -0.0016(2) -0.0014(3) Cl 0.0287(10) 0.0630(15) 0.0905(13) -0.0012(17) -0.0030(8) -0.0014(11) S1 0.0395(11) 0.0422(13) 0.0577(11) 0.0079(12) 0.0010(7) -0.0004(10) C2 0.035(5) 0.060(7) 0.093(7) -0.008(5) -0.014(4) -0.011(4) C3 0.069(7) 0.065(7) 0.073(6) -0.024(5) 0.004(5) -0.020(6) S4 0.0503(11) 0.0347(11) 0.0534(10) -0.0008(8) 0.0029(10) 0.0002(12) C5 0.093(8) 0.043(5) 0.065(5) -0.004(4) 0.000(5) 0.018(5) C6 0.090(7) 0.035(5) 0.063(5) 0.017(4) -0.004(5) 0.010(6) S7 0.0519(12) 0.0351(11) 0.0506(10) 0.0062(7) -0.0041(9) 0.0050(13) C8 0.072(7) 0.064(6) 0.061(5) 0.011(5) 0.012(5) -0.005(5) C9 0.048(6) 0.073(7) 0.092(7) 0.017(6) 0.031(5) -0.004(5) N21 0.031(3) 0.035(3) 0.036(3) 0.004(2) 0.000(2) -0.002(3) C22 0.060(5) 0.043(5) 0.039(4) 0.003(3) 0.000(4) -0.010(5) C23 0.056(6) 0.039(5) 0.050(4) 0.002(3) 0.000(3) 0.003(4) C24 0.040(5) 0.042(5) 0.047(4) 0.001(3) 0.000(3) 0.005(4) C25 0.048(5) 0.026(4) 0.049(4) 0.002(3) -0.004(3) -0.005(4) N11 0.027(3) 0.030(3) 0.044(3) 0.000(2) 0.002(2) -0.003(3) C12 0.054(5) 0.036(4) 0.042(4) -0.004(3) 0.000(4) -0.008(4) C13 0.062(5) 0.043(5) 0.049(4) -0.002(3) 0.001(4) -0.004(6) C14 0.037(5) 0.043(5) 0.046(4) 0.002(3) 0.001(3) -0.003(4) C15 0.045(5) 0.020(4) 0.055(4) 0.001(3) -0.001(3) -0.006(4) C16 0.030(4) 0.019(4) 0.064(4) 0.003(3) 0.003(3) -0.006(4) C17 0.066(6) 0.035(5) 0.056(5) 0.012(4) -0.007(4) -0.006(4) C18 0.064(5) 0.028(4) 0.057(5) 0.004(4) -0.004(4) -0.007(4) C26 0.038(4) 0.035(4) 0.044(4) 0.004(3) -0.003(3) 0.005(4) C31 0.053(6) 0.040(5) 0.050(4) -0.001(3) -0.010(3) -0.009(5) C32 0.052(5) 0.060(6) 0.051(4) -0.009(4) -0.002(3) -0.009(4) C33 0.068(6) 0.093(8) 0.035(4) 0.003(4) 0.007(4) -0.014(6) C34 0.075(6) 0.053(6) 0.061(5) 0.020(4) -0.007(4) -0.011(5) C35 0.071(6) 0.049(5) 0.064(5) 0.014(4) -0.007(4) 0.000(5) C36 0.054(6) 0.050(5) 0.051(4) 0.006(3) -0.003(3) 0.011(5) C41 0.046(5) 0.030(4) 0.060(5) -0.007(3) 0.007(3) 0.007(4) C42 0.077(7) 0.068(7) 0.056(5) -0.007(5) -0.003(4) -0.012(6) C43 0.112(9) 0.051(6) 0.077(6) -0.011(6) 0.014(5) -0.028(8) C44 0.129(11) 0.045(6) 0.082(7) -0.023(5) 0.048(7) -0.019(7) C45 0.086(9) 0.036(5) 0.099(7) 0.001(5) 0.012(6) 0.010(6) C46 0.069(7) 0.037(5) 0.079(6) -0.004(4) 0.008(4) 0.000(5) B 0.095(10) 0.055(7) 0.069(6) 0.002(5) 0.011(7) -0.004(8) F1 0.095(4) 0.117(5) 0.090(4) -0.044(3) -0.027(4) 0.019(5) F2 0.128(7) 0.140(7) 0.120(6) 0.025(5) 0.010(5) -0.061(6) F3 0.127(7) 0.094(6) 0.232(10) 0.050(6) -0.061(7) -0.032(5) F4 0.116(6) 0.202(9) 0.117(5) -0.092(6) -0.029(5) 0.051(7) _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 Ru N11 2.098(5) . ? Ru N21 2.104(6) . ? Ru S1 2.274(3) . ? Ru S7 2.301(3) . ? Ru S4 2.307(3) . ? Ru Cl 2.417(4) . ? S1 C2 1.827(9) . ? S1 C9 1.849(9) . ? C2 C3 1.518(13) . ? C3 S4 1.818(10) . ? S4 C5 1.827(9) . ? C5 C6 1.461(12) . ? C6 S7 1.840(8) . ? S7 C8 1.821(10) . ? C8 C9 1.477(13) . ? N21 C22 1.322(8) . ? N21 C26 1.372(8) . ? C22 C23 1.404(10) . ? C23 C24 1.375(10) . ? C24 C25 1.433(10) . ? C24 C41 1.491(10) . ? C25 C26 1.406(10) . ? C25 C18 1.438(10) . ? N11 C12 1.321(8) . ? N11 C16 1.384(9) . ? C12 C13 1.394(10) . ? C13 C14 1.370(10) . ? C14 C15 1.415(10) . ? C14 C31 1.498(10) . ? C15 C16 1.407(10) . ? C15 C17 1.438(10) . ? C16 C26 1.438(10) . ? C17 C18 1.327(11) . ? C31 C36 1.371(11) . ? C31 C32 1.419(11) . ? C32 C33 1.387(12) . ? C33 C34 1.385(13) . ? C34 C35 1.383(13) . ? C35 C36 1.402(11) . ? C41 C42 1.373(12) . ? C41 C46 1.401(12) . ? C42 C43 1.375(14) . ? C43 C44 1.378(16) . ? C44 C45 1.367(16) . ? C45 C46 1.388(11) . ? B F4 1.337(13) . ? B F2 1.351(16) . ? B F1 1.362(14) . ? B F3 1.401(14) . ? 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 N11 Ru N21 79.1(2) . . ? N11 Ru S1 92.13(18) . . ? N21 Ru S1 94.69(18) . . ? N11 Ru S7 175.08(15) . . ? N21 Ru S7 96.02(15) . . ? S1 Ru S7 88.72(8) . . ? N11 Ru S4 97.19(17) . . ? N21 Ru S4 175.09(16) . . ? S1 Ru S4 88.61(9) . . ? S7 Ru S4 87.67(9) . . ? N11 Ru Cl 87.48(18) . . ? N21 Ru Cl 87.53(18) . . ? S1 Ru Cl 177.63(7) . . ? S7 Ru Cl 91.86(8) . . ? S4 Ru Cl 89.12(9) . . ? C2 S1 C9 99.8(5) . . ? C2 S1 Ru 103.1(3) . . ? C9 S1 Ru 106.0(3) . . ? C3 C2 S1 115.4(6) . . ? C2 C3 S4 111.4(7) . . ? C3 S4 C5 101.8(5) . . ? C3 S4 Ru 106.9(3) . . ? C5 S4 Ru 103.6(3) . . ? C6 C5 S4 114.3(7) . . ? C5 C6 S7 113.6(6) . . ? C8 S7 C6 101.6(5) . . ? C8 S7 Ru 103.0(3) . . ? C6 S7 Ru 106.1(3) . . ? C9 C8 S7 114.7(6) . . ? C8 C9 S1 112.4(7) . . ? C22 N21 C26 117.9(6) . . ? C22 N21 Ru 127.8(5) . . ? C26 N21 Ru 113.7(4) . . ? N21 C22 C23 122.9(7) . . ? C24 C23 C22 120.3(7) . . ? C23 C24 C25 118.2(7) . . ? C23 C24 C41 120.5(7) . . ? C25 C24 C41 121.2(6) . . ? C26 C25 C24 117.2(6) . . ? C26 C25 C18 117.3(7) . . ? C24 C25 C18 125.5(7) . . ? C12 N11 C16 117.9(6) . . ? C12 N11 Ru 128.5(5) . . ? C16 N11 Ru 113.5(4) . . ? N11 C12 C13 122.7(7) . . ? C14 C13 C12 121.0(7) . . ? C13 C14 C15 117.9(6) . . ? C13 C14 C31 121.2(6) . . ? C15 C14 C31 120.8(7) . . ? C16 C15 C14 118.1(6) . . ? C16 C15 C17 116.2(7) . . ? C14 C15 C17 125.7(7) . . ? N11 C16 C15 122.2(6) . . ? N11 C16 C26 116.6(6) . . ? C15 C16 C26 121.2(6) . . ? C18 C17 C15 123.0(7) . . ? C17 C18 C25 122.0(8) . . ? N21 C26 C25 123.2(6) . . ? N21 C26 C16 116.7(6) . . ? C25 C26 C16 120.1(6) . . ? C36 C31 C32 118.9(7) . . ? C36 C31 C14 122.3(7) . . ? C32 C31 C14 118.8(7) . . ? C33 C32 C31 118.7(9) . . ? C34 C33 C32 122.3(8) . . ? C35 C34 C33 118.4(8) . . ? C34 C35 C36 120.3(8) . . ? C31 C36 C35 121.2(8) . . ? C42 C41 C46 118.6(8) . . ? C42 C41 C24 120.8(8) . . ? C46 C41 C24 120.6(7) . . ? C41 C42 C43 121.0(10) . . ? C42 C43 C44 119.8(10) . . ? C45 C44 C43 120.6(10) . . ? C44 C45 C46 119.5(10) . . ? C45 C46 C41 120.3(9) . . ? F4 B F2 112.4(11) . . ? F4 B F1 111.6(12) . . ? F2 B F1 116.5(9) . . ? F4 B F3 106.2(10) . . ? F2 B F3 102.9(11) . . ? F1 B F3 106.0(10) . . ? _diffrn_measured_fraction_theta_max 0.704 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.704 _refine_diff_density_max 0.995 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.082 #===END data_[Ru([9]aneS3)(dppz)Cl]PF6.0.125H2O #13 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22.12 Cl F6 N4 O0.12 P Ru S3' _chemical_formula_weight 746.25 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' 0.0000 0.0000 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'P' 'P' 0.1023 0.0942 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.619(11) _cell_length_b 30.542(34) _cell_length_c 25.273(28) _cell_angle_alpha 90.00 _cell_angle_beta 96.700(10) _cell_angle_gamma 90.00 _cell_volume 5841(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2985 _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17917 _diffrn_reflns_av_R_equivalents 0.1585 _diffrn_reflns_av_sigmaI/netI 0.1915 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 26.12 _reflns_number_total 9949 _reflns_number_gt 4741 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.1664P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9949 _refine_ls_number_parameters 697 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.2446 _refine_ls_R_factor_gt 0.1243 _refine_ls_wR_factor_ref 0.3389 _refine_ls_wR_factor_gt 0.2840 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 RuA Ru 0.34427(14) 0.57368(4) 0.31721(5) 0.0429(4) Uani 1 d . . . ClA Cl 0.0626(5) 0.60602(13) 0.28289(17) 0.0596(11) Uani 1 d . . . S1A S 0.6082(5) 0.54325(13) 0.35107(16) 0.0523(10) Uani 1 d . . . C2A C 0.751(2) 0.5897(6) 0.3781(8) 0.077(5) Uani 1 d . . . H2A1 H 0.7421 0.5929 0.4159 0.092 Uiso 1 calc R . . H2A2 H 0.8728 0.5835 0.3736 0.092 Uiso 1 calc R . . C3A C 0.694(2) 0.6332(6) 0.3492(7) 0.069(5) Uani 1 d . . . H3A1 H 0.7343 0.6331 0.3142 0.082 Uiso 1 calc R . . H3A2 H 0.7508 0.6575 0.3691 0.082 Uiso 1 calc R . . S4A S 0.4595(5) 0.64179(12) 0.34171(17) 0.0533(10) Uani 1 d . . . C5A C 0.414(2) 0.6512(5) 0.4105(7) 0.066(5) Uani 1 d . . . H5A1 H 0.5161 0.6429 0.4349 0.080 Uiso 1 calc R . . H5A2 H 0.3918 0.6822 0.4156 0.080 Uiso 1 calc R . . C6A C 0.259(2) 0.6257(5) 0.4229(7) 0.069(5) Uani 1 d . . . H6A1 H 0.1524 0.6403 0.4067 0.082 Uiso 1 calc R . . H6A2 H 0.2557 0.6261 0.4612 0.082 Uiso 1 calc R . . S7A S 0.2535(5) 0.56885(12) 0.40050(16) 0.0500(9) Uani 1 d . . . C8A C 0.441(2) 0.5458(5) 0.4433(6) 0.061(4) Uani 1 d . . . H8A1 H 0.5117 0.5694 0.4603 0.073 Uiso 1 calc R . . H8A2 H 0.3978 0.5283 0.4710 0.073 Uiso 1 calc R . . C9A C 0.556(2) 0.5178(6) 0.4122(7) 0.070(5) Uani 1 d . . . H9A1 H 0.4957 0.4902 0.4034 0.084 Uiso 1 calc R . . H9A2 H 0.6651 0.5112 0.4344 0.084 Uiso 1 calc R . . N11A N 0.3993(14) 0.5752(3) 0.2373(4) 0.037(3) Uani 1 d . . . C12A C 0.442(2) 0.6093(5) 0.2109(6) 0.058(4) Uani 1 d . . . H12A H 0.4636 0.6358 0.2287 0.069 Uiso 1 calc R . . C13A C 0.458(2) 0.6073(6) 0.1559(8) 0.076(5) Uani 1 d . . . H13A H 0.4923 0.6318 0.1379 0.091 Uiso 1 calc R . . C14A C 0.423(2) 0.5696(5) 0.1301(7) 0.064(5) Uani 1 d . . . H14A H 0.4326 0.5679 0.0938 0.076 Uiso 1 calc R . . C15A C 0.3728(17) 0.5330(4) 0.1570(6) 0.049(4) Uani 1 d . . . C16A C 0.3571(16) 0.5368(4) 0.2113(6) 0.040(3) Uani 1 d . . . N21A N 0.2526(13) 0.5119(3) 0.2895(4) 0.035(2) Uani 1 d . . . C22A C 0.1671(17) 0.4821(4) 0.3159(6) 0.046(4) Uani 1 d . . . H22A H 0.1391 0.4889 0.3497 0.056 Uiso 1 calc R . . C23A C 0.1187(19) 0.4414(5) 0.2945(7) 0.056(4) Uani 1 d . . . H23A H 0.0643 0.4208 0.3142 0.067 Uiso 1 calc R . . C24A C 0.1531(18) 0.4327(4) 0.2443(6) 0.049(4) Uani 1 d . . . H24A H 0.1223 0.4055 0.2293 0.059 Uiso 1 calc R . . C25A C 0.2323(15) 0.4630(4) 0.2150(6) 0.038(3) Uani 1 d . . . C26A C 0.2770(16) 0.5017(5) 0.2395(6) 0.042(3) Uani 1 d . . . C27A C 0.3301(17) 0.4893(5) 0.1299(6) 0.050(4) Uani 1 d . . . C28A C 0.2564(17) 0.4556(5) 0.1593(7) 0.052(4) Uani 1 d . . . N29A N 0.2186(14) 0.4180(4) 0.1374(5) 0.049(3) Uani 1 d . . . C30A C 0.248(2) 0.4104(5) 0.0866(7) 0.054(4) Uani 1 d . . . C31A C 0.207(2) 0.3703(6) 0.0612(7) 0.072(5) Uani 1 d . . . H31A H 0.1535 0.3481 0.0788 0.087 Uiso 1 calc R . . C32A C 0.244(3) 0.3646(8) 0.0116(9) 0.113(8) Uani 1 d . . . H32A H 0.2256 0.3372 -0.0040 0.135 Uiso 1 calc R . . C33A C 0.312(3) 0.3987(6) -0.0188(8) 0.088(6) Uani 1 d . . . H33A H 0.3301 0.3939 -0.0541 0.106 Uiso 1 calc R . . C34A C 0.351(2) 0.4380(5) 0.0043(7) 0.073(5) Uani 1 d . . . H34A H 0.3955 0.4602 -0.0155 0.088 Uiso 1 calc R . . C35A C 0.325(2) 0.4458(6) 0.0585(7) 0.061(4) Uani 1 d . . . N36A N 0.3605(15) 0.4852(4) 0.0789(5) 0.055(3) Uani 1 d . . . RuB Ru 0.70075(15) 0.77123(4) 0.20535(6) 0.0523(4) Uani 1 d . . . ClB Cl 0.4384(5) 0.72768(13) 0.1780(2) 0.0682(12) Uani 1 d . . . S1B S 0.9579(5) 0.80841(13) 0.23071(19) 0.0613(12) Uani 1 d . . . C2B C 1.090(3) 0.7711(6) 0.2727(10) 0.108(8) Uani 1 d . . . H2B1 H 1.2120 0.7752 0.2659 0.129 Uiso 1 calc R . . H2B2 H 1.0837 0.7800 0.3092 0.129 Uiso 1 calc R . . C3B C 1.056(2) 0.7263(6) 0.2699(10) 0.102(8) Uani 1 d . . . H3B1 H 1.0678 0.7150 0.3060 0.122 Uiso 1 calc R . . H3B2 H 1.1485 0.7127 0.2521 0.122 Uiso 1 calc R . . S4B S 0.8410(5) 0.70772(12) 0.23597(18) 0.0548(11) Uani 1 d . . . C5B C 0.915(3) 0.6814(6) 0.1801(7) 0.077(5) Uani 1 d . . . H5B1 H 1.0358 0.6720 0.1901 0.093 Uiso 1 calc R . . H5B2 H 0.8442 0.6552 0.1728 0.093 Uiso 1 calc R . . C6B C 0.910(3) 0.7055(7) 0.1325(9) 0.115(9) Uani 1 d . . . H6B1 H 0.8557 0.6868 0.1041 0.138 Uiso 1 calc R . . H6B2 H 1.0313 0.7100 0.1258 0.138 Uiso 1 calc R . . S7B S 0.8015(5) 0.75751(15) 0.12474(19) 0.0653(12) Uani 1 d . . . C8B C 0.988(4) 0.7925(8) 0.1235(11) 0.129(10) Uani 1 d . . . H8B1 H 1.0764 0.7764 0.1067 0.155 Uiso 1 calc R . . H8B2 H 0.9517 0.8170 0.1003 0.155 Uiso 1 calc R . . C9B C 1.070(3) 0.8094(8) 0.1696(9) 0.103(8) Uani 1 d . . . H9B1 H 1.0983 0.8397 0.1628 0.124 Uiso 1 calc R . . H9B2 H 1.1817 0.7941 0.1776 0.124 Uiso 1 calc R . . N11B N 0.5973(16) 0.7880(4) 0.2764(5) 0.052(3) Uani 1 d . . . C12B C 0.597(2) 0.7661(5) 0.3220(8) 0.068(5) Uani 1 d . . . H12B H 0.6518 0.7389 0.3245 0.082 Uiso 1 calc R . . C13B C 0.522(2) 0.7804(6) 0.3651(8) 0.076(5) Uani 1 d . . . H13B H 0.5168 0.7619 0.3942 0.091 Uiso 1 calc R . . C14B C 0.454(2) 0.8209(6) 0.3658(8) 0.072(5) Uani 1 d . . . H14B H 0.4116 0.8319 0.3962 0.087 Uiso 1 calc R . . C15B C 0.450(2) 0.8463(4) 0.3194(8) 0.064(5) Uani 1 d . . . C16B C 0.5195(17) 0.8283(5) 0.2752(6) 0.048(4) Uani 1 d . . . N21B N 0.5703(14) 0.8295(4) 0.1838(5) 0.049(3) Uani 1 d . . . C22B C 0.5415(19) 0.8488(6) 0.1361(8) 0.074(5) Uani 1 d . . . H22B H 0.5805 0.8347 0.1071 0.089 Uiso 1 calc R . . C23B C 0.456(2) 0.8890(6) 0.1276(9) 0.076(6) Uani 1 d . . . H23B H 0.4401 0.9009 0.0935 0.091 Uiso 1 calc R . . C24B C 0.3964(19) 0.9107(6) 0.1679(8) 0.062(5) Uani 1 d . . . H24B H 0.3410 0.9377 0.1623 0.075 Uiso 1 calc R . . C25B C 0.419(2) 0.8921(5) 0.2186(8) 0.066(5) Uani 1 d . . . C26B C 0.5053(16) 0.8517(5) 0.2234(6) 0.048(4) Uani 1 d . . . C27B C 0.3694(18) 0.8894(6) 0.3163(8) 0.061(5) Uani 1 d . . . C28B C 0.3621(17) 0.9140(5) 0.2646(9) 0.067(5) Uani 1 d . . . N29B N 0.2963(17) 0.9548(4) 0.2587(7) 0.073(4) Uani 1 d . . . C30B C 0.239(2) 0.9731(5) 0.3006(11) 0.075(6) Uani 1 d . . . C31B C 0.172(2) 1.0157(6) 0.3003(11) 0.094(8) Uani 1 d . . . H31B H 0.1710 1.0318 0.2690 0.113 Uiso 1 calc R . . C32B C 0.109(3) 1.0349(8) 0.3410(14) 0.114(10) Uani 1 d . . . H32B H 0.0614 1.0629 0.3373 0.137 Uiso 1 calc R . . C33B C 0.115(2) 1.0134(8) 0.3887(12) 0.099(8) Uani 1 d . . . H33B H 0.0731 1.0275 0.4174 0.118 Uiso 1 calc R . . C34B C 0.180(3) 0.9726(7) 0.3954(10) 0.107(8) Uani 1 d . . . H34B H 0.1804 0.9590 0.4283 0.128 Uiso 1 calc R . . C35B C 0.2503(18) 0.9488(7) 0.3512(10) 0.083(7) Uani 1 d . . . N36B N 0.3125(17) 0.9085(4) 0.3564(7) 0.077(5) Uani 1 d . . . P1 P 1.0467(9) 0.7525(2) -0.0531(3) 0.108(2) Uani 1 d D . . F111 F 1.052(3) 0.7956(5) -0.0179(8) 0.190(9) Uiso 0.54(2) d PD A 1 F121 F 1.043(3) 0.7097(5) -0.0895(8) 0.190(9) Uiso 0.54(2) d PD A 1 F131 F 1.059(3) 0.7819(7) -0.1051(6) 0.190(9) Uiso 0.54(2) d PD A 1 F141 F 1.2574(16) 0.7498(9) -0.0440(10) 0.190(9) Uiso 0.54(2) d PD A 1 F151 F 0.8373(15) 0.7549(9) -0.0630(10) 0.190(9) Uiso 0.54(2) d PD A 1 F161 F 1.035(3) 0.7232(7) -0.0019(6) 0.190(9) Uiso 0.54(2) d PD A 1 F112 F 0.927(3) 0.7940(5) -0.0699(8) 0.137(9) Uiso 0.46(2) d PD A 2 F122 F 0.922(2) 0.7394(7) -0.0099(7) 0.137(9) Uiso 0.46(2) d PD A 2 F132 F 1.169(2) 0.7110(5) -0.0375(8) 0.137(9) Uiso 0.46(2) d PD A 2 F142 F 1.165(3) 0.7814(6) -0.0105(7) 0.137(9) Uiso 0.46(2) d PD A 2 F152 F 0.929(3) 0.7240(6) -0.0968(7) 0.137(9) Uiso 0.46(2) d PD A 2 F162 F 1.173(3) 0.7653(7) -0.0971(7) 0.137(9) Uiso 0.46(2) d PD A 2 P2 P -0.0580(7) 0.57603(17) 0.54573(19) 0.0894(18) Uani 1 d D . . F211 F 0.0671(19) 0.5452(5) 0.5824(6) 0.125(6) Uiso 0.56(2) d PD B 1 F221 F -0.1940(19) 0.6083(5) 0.5095(6) 0.125(6) Uiso 0.56(2) d PD B 1 F231 F -0.124(2) 0.5993(5) 0.5973(5) 0.125(6) Uiso 0.56(2) d PD B 1 F241 F 0.0904(19) 0.6121(5) 0.5456(7) 0.125(6) Uiso 0.56(2) d PD B 1 F251 F -0.2166(18) 0.5418(5) 0.5464(7) 0.125(6) Uiso 0.56(2) d PD B 1 F261 F -0.004(2) 0.5549(6) 0.4934(5) 0.125(6) Uiso 0.56(2) d PD B 1 F212 F 0.010(3) 0.5345(5) 0.5826(8) 0.135(8) Uiso 0.44(2) d PD B 2 F222 F -0.118(3) 0.6155(5) 0.5081(7) 0.135(8) Uiso 0.44(2) d PD B 2 F232 F -0.2449(18) 0.5720(8) 0.5659(10) 0.135(8) Uiso 0.44(2) d PD B 2 F242 F -0.121(3) 0.5422(6) 0.4988(7) 0.135(8) Uiso 0.44(2) d PD B 2 F252 F 0.010(3) 0.6076(6) 0.5930(7) 0.135(8) Uiso 0.44(2) d PD B 2 F262 F 0.1346(18) 0.5771(8) 0.5254(9) 0.135(8) Uiso 0.44(2) d PD B 2 O1 O 1.438(5) 0.6884(13) 0.0577(16) 0.058(11) Uiso 0.25 d P . . 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 RuA 0.0393(7) 0.0351(7) 0.0553(8) 0.0026(5) 0.0096(5) 0.0003(5) ClA 0.045(2) 0.053(2) 0.082(3) 0.011(2) 0.0116(18) 0.0087(16) S1A 0.047(2) 0.050(2) 0.059(3) -0.0001(19) 0.0057(17) 0.0061(16) C2A 0.062(12) 0.094(14) 0.080(14) -0.017(11) 0.029(9) -0.012(9) C3A 0.084(12) 0.077(13) 0.047(11) -0.005(9) 0.014(8) 0.012(9) S4A 0.052(2) 0.043(2) 0.067(3) -0.0013(19) 0.0117(18) -0.0040(16) C5A 0.061(10) 0.047(10) 0.094(14) -0.018(9) 0.020(9) -0.018(8) C6A 0.099(13) 0.036(9) 0.077(13) -0.004(8) 0.036(10) -0.003(8) S7A 0.047(2) 0.042(2) 0.063(3) 0.0033(18) 0.0160(17) 0.0005(15) C8A 0.075(11) 0.052(10) 0.056(11) 0.011(8) 0.003(8) -0.001(8) C9A 0.050(10) 0.082(13) 0.077(13) 0.009(10) 0.001(8) -0.001(8) N11A 0.047(7) 0.029(6) 0.037(7) -0.001(5) 0.013(5) 0.002(5) C12A 0.086(11) 0.042(9) 0.046(10) -0.002(8) 0.016(8) -0.015(8) C13A 0.089(13) 0.050(11) 0.094(16) -0.011(10) 0.033(11) -0.029(9) C14A 0.096(13) 0.039(10) 0.060(11) 0.010(8) 0.030(9) -0.015(8) C15A 0.034(8) 0.039(8) 0.075(12) 0.014(8) 0.008(7) 0.009(6) C16A 0.036(7) 0.038(8) 0.047(10) 0.000(7) 0.004(6) 0.005(6) N21A 0.042(6) 0.036(6) 0.027(7) 0.014(5) -0.002(5) -0.001(5) C22A 0.046(8) 0.041(9) 0.052(10) -0.001(7) 0.006(6) -0.012(6) C23A 0.062(10) 0.045(9) 0.062(12) 0.014(8) 0.012(8) -0.018(7) C24A 0.046(9) 0.034(8) 0.064(12) -0.006(7) -0.006(7) -0.013(6) C25A 0.025(7) 0.028(7) 0.060(10) -0.007(6) 0.002(6) -0.004(5) C26A 0.031(8) 0.055(10) 0.038(9) 0.010(7) -0.006(6) 0.010(6) C27A 0.036(8) 0.051(9) 0.063(11) -0.005(8) 0.012(7) 0.001(6) C28A 0.035(8) 0.037(9) 0.086(13) 0.013(8) 0.015(7) -0.005(6) N29A 0.035(7) 0.036(7) 0.075(10) 0.002(6) -0.005(6) -0.005(5) C30A 0.074(11) 0.034(8) 0.053(11) -0.001(7) 0.002(8) -0.012(7) C31A 0.092(13) 0.070(12) 0.055(12) 0.000(9) 0.006(9) -0.039(10) C32A 0.16(2) 0.093(17) 0.084(18) -0.010(13) 0.023(15) -0.064(16) C33A 0.138(18) 0.065(13) 0.067(13) -0.020(10) 0.037(12) -0.036(12) C34A 0.097(14) 0.049(10) 0.072(14) -0.023(9) 0.005(10) -0.025(9) C35A 0.052(10) 0.065(12) 0.064(12) -0.003(9) -0.005(8) -0.012(8) N36A 0.056(8) 0.042(8) 0.068(10) 0.000(7) 0.011(6) -0.007(6) RuB 0.0378(7) 0.0389(7) 0.0801(10) 0.0083(6) 0.0064(6) 0.0006(5) ClB 0.038(2) 0.057(3) 0.109(4) -0.003(2) 0.006(2) -0.0067(16) S1B 0.042(2) 0.042(2) 0.099(4) 0.003(2) 0.003(2) -0.0067(16) C2B 0.088(15) 0.064(14) 0.16(2) 0.014(13) -0.042(14) -0.021(11) C3B 0.064(13) 0.062(13) 0.16(2) -0.004(13) -0.053(12) 0.011(9) S4B 0.040(2) 0.039(2) 0.086(3) 0.011(2) 0.0075(18) 0.0021(15) C5B 0.122(16) 0.053(11) 0.056(12) 0.013(9) 0.004(10) 0.017(10) C6B 0.19(3) 0.075(15) 0.090(17) 0.006(12) 0.069(16) 0.067(16) S7B 0.052(2) 0.067(3) 0.077(3) 0.012(2) 0.008(2) -0.0004(19) C8B 0.15(2) 0.104(19) 0.14(2) -0.028(17) 0.035(18) -0.083(17) C9B 0.090(16) 0.109(18) 0.11(2) 0.052(16) 0.014(13) -0.021(13) N11B 0.063(8) 0.032(7) 0.064(9) -0.008(6) 0.018(6) -0.009(6) C12B 0.051(10) 0.043(10) 0.109(17) 0.014(10) -0.002(9) 0.010(7) C13B 0.082(13) 0.051(11) 0.099(16) 0.014(10) 0.035(11) 0.008(9) C14B 0.069(12) 0.072(13) 0.074(14) -0.019(10) 0.002(9) -0.007(9) C15B 0.060(10) 0.021(8) 0.108(16) 0.016(9) -0.006(9) -0.009(7) C16B 0.033(8) 0.053(10) 0.062(11) 0.003(8) 0.020(7) -0.003(6) N21B 0.036(7) 0.040(7) 0.071(10) 0.024(7) 0.007(6) 0.000(5) C22B 0.036(9) 0.082(13) 0.101(16) 0.018(11) -0.006(8) -0.004(8) C23B 0.064(11) 0.058(12) 0.105(16) 0.038(11) 0.005(10) 0.010(9) C24B 0.036(9) 0.055(10) 0.094(15) 0.009(10) 0.001(8) -0.010(7) C25B 0.059(11) 0.040(10) 0.100(15) 0.021(10) 0.014(9) 0.001(8) C26B 0.023(7) 0.042(9) 0.077(12) 0.021(8) -0.002(6) 0.011(6) C27B 0.025(8) 0.061(11) 0.099(14) 0.002(10) 0.013(8) -0.002(7) C28B 0.018(8) 0.038(9) 0.141(18) -0.001(10) -0.010(8) 0.007(6) N29B 0.043(8) 0.036(8) 0.136(15) -0.011(8) -0.005(8) -0.008(6) C30B 0.029(9) 0.043(11) 0.15(2) 0.013(12) 0.013(10) -0.002(7) C31B 0.051(11) 0.033(10) 0.19(3) -0.010(13) -0.026(12) -0.014(8) C32B 0.083(16) 0.055(15) 0.20(3) -0.024(18) -0.011(18) 0.008(12) C33B 0.043(12) 0.083(17) 0.17(3) -0.048(17) 0.012(12) -0.001(10) C34B 0.079(14) 0.084(16) 0.16(2) -0.075(16) 0.017(13) -0.025(12) C35B 0.011(8) 0.085(15) 0.15(2) -0.061(14) 0.000(8) -0.014(7) N36B 0.043(8) 0.047(8) 0.136(15) -0.029(9) -0.009(8) 0.010(6) P1 0.124(5) 0.091(4) 0.110(5) 0.003(4) 0.016(4) -0.032(4) P2 0.118(5) 0.100(4) 0.049(3) -0.001(3) 0.006(3) -0.040(3) _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 RuA N21A 2.104(11) . ? RuA N11A 2.110(11) . ? RuA S1A 2.289(5) . ? RuA S7A 2.296(5) . ? RuA S4A 2.314(4) . ? RuA ClA 2.429(5) . ? S1A C9A 1.814(17) . ? S1A C2A 1.867(18) . ? C2A C3A 1.55(2) . ? C3A S4A 1.791(17) . ? S4A C5A 1.836(17) . ? C5A C6A 1.48(2) . ? C6A S7A 1.827(15) . ? S7A C8A 1.830(16) . ? C8A C9A 1.51(2) . ? N11A C12A 1.301(17) . ? N11A C16A 1.365(16) . ? C12A C13A 1.41(2) . ? C13A C14A 1.33(2) . ? C14A C15A 1.387(19) . ? C15A C16A 1.395(19) . ? C15A C27A 1.52(2) . ? C16A C26A 1.458(19) . ? N21A C26A 1.336(17) . ? N21A C22A 1.340(16) . ? C22A C23A 1.39(2) . ? C23A C24A 1.35(2) . ? C24A C25A 1.369(19) . ? C25A C26A 1.359(18) . ? C25A C28A 1.46(2) . ? C27A N36A 1.342(18) . ? C27A C28A 1.425(19) . ? C28A N29A 1.291(18) . ? N29A C30A 1.349(19) . ? C30A C31A 1.40(2) . ? C30A C35A 1.45(2) . ? C31A C32A 1.33(3) . ? C32A C33A 1.42(3) . ? C33A C34A 1.35(2) . ? C34A C35A 1.43(2) . ? C35A N36A 1.324(19) . ? RuB N21B 2.081(11) . ? RuB N11B 2.108(12) . ? RuB S1B 2.290(5) . ? RuB S7B 2.298(5) . ? RuB S4B 2.305(4) . ? RuB ClB 2.433(5) . ? S1B C2B 1.79(2) . ? S1B C9B 1.85(2) . ? C2B C3B 1.39(2) . ? C3B S4B 1.849(17) . ? S4B C5B 1.772(18) . ? C5B C6B 1.41(2) . ? C6B S7B 1.791(18) . ? S7B C8B 1.78(2) . ? C8B C9B 1.36(3) . ? N11B C12B 1.33(2) . ? N11B C16B 1.364(18) . ? C12B C13B 1.36(2) . ? C13B C14B 1.34(2) . ? C14B C15B 1.40(2) . ? C15B C16B 1.40(2) . ? C15B C27B 1.45(2) . ? C16B C26B 1.49(2) . ? N21B C22B 1.33(2) . ? N21B C26B 1.350(18) . ? C22B C23B 1.40(2) . ? C23B C24B 1.34(2) . ? C24B C25B 1.39(2) . ? C25B C26B 1.39(2) . ? C25B C28B 1.45(2) . ? C27B N36B 1.29(2) . ? C27B C28B 1.50(2) . ? C28B N29B 1.347(19) . ? N29B C30B 1.32(2) . ? C30B C31B 1.40(2) . ? C30B C35B 1.47(3) . ? C31B C32B 1.32(3) . ? C32B C33B 1.37(3) . ? C33B C34B 1.34(3) . ? C34B C35B 1.48(3) . ? C35B N36B 1.32(2) . ? P1 F122 1.580(10) . ? P1 F161 1.583(10) . ? P1 F111 1.586(10) . ? P1 F151 1.588(10) . ? P1 F142 1.588(10) . ? P1 F112 1.592(10) . ? P1 F132 1.594(10) . ? P1 F152 1.595(10) . ? P1 F141 1.597(10) . ? P1 F121 1.598(10) . ? P1 F131 1.603(10) . ? P1 F162 1.605(10) . ? P2 F211 1.564(9) . ? P2 F261 1.569(9) . ? P2 F222 1.570(10) . ? P2 F232 1.572(10) . ? P2 F252 1.576(10) . ? P2 F241 1.580(9) . ? P2 F251 1.599(9) . ? P2 F242 1.604(10) . ? P2 F262 1.610(10) . ? P2 F231 1.617(9) . ? P2 F212 1.621(10) . ? P2 F221 1.631(9) . ? 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 N21A RuA N11A 78.3(4) . . ? N21A RuA S1A 90.2(3) . . ? N11A RuA S1A 95.9(3) . . ? N21A RuA S7A 97.1(3) . . ? N11A RuA S7A 173.5(3) . . ? S1A RuA S7A 88.65(16) . . ? N21A RuA S4A 175.2(3) . . ? N11A RuA S4A 97.2(3) . . ? S1A RuA S4A 88.61(16) . . ? S7A RuA S4A 87.58(15) . . ? N21A RuA ClA 90.0(3) . . ? N11A RuA ClA 85.2(3) . . ? S1A RuA ClA 178.96(15) . . ? S7A RuA ClA 90.31(15) . . ? S4A RuA ClA 91.24(16) . . ? C9A S1A C2A 101.0(8) . . ? C9A S1A RuA 102.8(5) . . ? C2A S1A RuA 106.0(6) . . ? C3A C2A S1A 111.1(12) . . ? C2A C3A S4A 113.2(12) . . ? C3A S4A C5A 102.7(8) . . ? C3A S4A RuA 103.8(6) . . ? C5A S4A RuA 106.7(5) . . ? C6A C5A S4A 111.3(12) . . ? C5A C6A S7A 115.1(11) . . ? C6A S7A C8A 101.3(8) . . ? C6A S7A RuA 103.0(5) . . ? C8A S7A RuA 105.6(5) . . ? C9A C8A S7A 111.7(12) . . ? C8A C9A S1A 113.5(12) . . ? C12A N11A C16A 120.0(12) . . ? C12A N11A RuA 126.9(10) . . ? C16A N11A RuA 112.3(8) . . ? N11A C12A C13A 121.8(14) . . ? C14A C13A C12A 119.0(15) . . ? C13A C14A C15A 120.4(17) . . ? C14A C15A C16A 118.5(14) . . ? C14A C15A C27A 122.9(15) . . ? C16A C15A C27A 118.6(12) . . ? N11A C16A C15A 120.1(12) . . ? N11A C16A C26A 118.9(12) . . ? C15A C16A C26A 120.6(12) . . ? C26A N21A C22A 116.2(12) . . ? C26A N21A RuA 116.4(8) . . ? C22A N21A RuA 127.3(9) . . ? N21A C22A C23A 122.5(14) . . ? C24A C23A C22A 118.0(13) . . ? C23A C24A C25A 121.3(13) . . ? C26A C25A C24A 116.5(13) . . ? C26A C25A C28A 121.5(12) . . ? C24A C25A C28A 121.9(12) . . ? N21A C26A C25A 125.3(13) . . ? N21A C26A C16A 113.9(12) . . ? C25A C26A C16A 120.8(13) . . ? N36A C27A C28A 123.8(14) . . ? N36A C27A C15A 117.7(13) . . ? C28A C27A C15A 118.4(14) . . ? N29A C28A C27A 120.0(15) . . ? N29A C28A C25A 120.4(12) . . ? C27A C28A C25A 119.5(13) . . ? C28A N29A C30A 120.5(13) . . ? N29A C30A C31A 122.2(14) . . ? N29A C30A C35A 117.2(13) . . ? C31A C30A C35A 120.6(16) . . ? C32A C31A C30A 119.0(17) . . ? C31A C32A C33A 123(2) . . ? C34A C33A C32A 119.4(19) . . ? C33A C34A C35A 121.0(17) . . ? N36A C35A C34A 118.7(15) . . ? N36A C35A C30A 124.2(16) . . ? C34A C35A C30A 117.0(15) . . ? C35A N36A C27A 114.1(13) . . ? N21B RuB N11B 78.5(5) . . ? N21B RuB S1B 90.9(3) . . ? N11B RuB S1B 91.9(4) . . ? N21B RuB S7B 97.0(4) . . ? N11B RuB S7B 175.5(4) . . ? S1B RuB S7B 88.58(18) . . ? N21B RuB S4B 175.5(4) . . ? N11B RuB S4B 97.1(4) . . ? S1B RuB S4B 88.58(16) . . ? S7B RuB S4B 87.39(17) . . ? N21B RuB ClB 92.4(3) . . ? N11B RuB ClB 89.9(3) . . ? S1B RuB ClB 176.49(15) . . ? S7B RuB ClB 89.82(17) . . ? S4B RuB ClB 88.22(16) . . ? C2B S1B C9B 102.8(12) . . ? C2B S1B RuB 104.8(6) . . ? C9B S1B RuB 103.8(8) . . ? C3B C2B S1B 120.5(15) . . ? C2B C3B S4B 118.3(13) . . ? C5B S4B C3B 99.3(10) . . ? C5B S4B RuB 107.0(6) . . ? C3B S4B RuB 104.4(6) . . ? C6B C5B S4B 117.7(13) . . ? C5B C6B S7B 121.5(14) . . ? C8B S7B C6B 100.1(14) . . ? C8B S7B RuB 104.8(9) . . ? C6B S7B RuB 105.2(7) . . ? C9B C8B S7B 120(2) . . ? C8B C9B S1B 119.9(18) . . ? C12B N11B C16B 115.3(13) . . ? C12B N11B RuB 130.8(11) . . ? C16B N11B RuB 113.8(10) . . ? N11B C12B C13B 125.1(15) . . ? C14B C13B C12B 120.3(18) . . ? C13B C14B C15B 118.0(17) . . ? C14B C15B C16B 118.4(14) . . ? C14B C15B C27B 121.0(18) . . ? C16B C15B C27B 120.5(16) . . ? N11B C16B C15B 122.5(14) . . ? N11B C16B C26B 116.2(13) . . ? C15B C16B C26B 121.2(14) . . ? C22B N21B C26B 114.3(13) . . ? C22B N21B RuB 129.6(12) . . ? C26B N21B RuB 116.2(9) . . ? N21B C22B C23B 123.4(19) . . ? C24B C23B C22B 120.8(19) . . ? C23B C24B C25B 118.7(17) . . ? C26B C25B C24B 116.5(17) . . ? C26B C25B C28B 121.4(16) . . ? C24B C25B C28B 122.1(16) . . ? N21B C26B C25B 126.2(15) . . ? N21B C26B C16B 114.6(12) . . ? C25B C26B C16B 119.1(15) . . ? N36B C27B C15B 123.2(18) . . ? N36B C27B C28B 118.4(16) . . ? C15B C27B C28B 118.3(16) . . ? N29B C28B C25B 118.7(18) . . ? N29B C28B C27B 122.4(18) . . ? C25B C28B C27B 118.8(14) . . ? C30B N29B C28B 117.3(18) . . ? N29B C30B C31B 123(2) . . ? N29B C30B C35B 119.6(15) . . ? C31B C30B C35B 117(2) . . ? C32B C31B C30B 125(3) . . ? C31B C32B C33B 120(2) . . ? C34B C33B C32B 122(2) . . ? C33B C34B C35B 121(3) . . ? N36B C35B C30B 122.7(18) . . ? N36B C35B C34B 123(2) . . ? C30B C35B C34B 115(2) . . ? C27B N36B C35B 119.7(19) . . ? F122 P1 F161 36.7(9) . . ? F122 P1 F111 78.6(11) . . ? F161 P1 F111 90.7(6) . . ? F122 P1 F151 56.4(9) . . ? F161 P1 F151 90.3(6) . . ? F111 P1 F151 90.6(6) . . ? F122 P1 F142 90.7(6) . . ? F161 P1 F142 80.9(11) . . ? F111 P1 F142 35.1(9) . . ? F151 P1 F142 124.1(10) . . ? F122 P1 F112 90.7(6) . . ? F161 P1 F112 125.7(10) . . ? F111 P1 F112 57.7(10) . . ? F151 P1 F112 52.1(10) . . ? F142 P1 F112 90.0(5) . . ? F122 P1 F132 90.5(5) . . ? F161 P1 F132 55.5(9) . . ? F111 P1 F132 123.0(10) . . ? F151 P1 F132 128.5(10) . . ? F142 P1 F132 90.4(6) . . ? F112 P1 F132 178.7(7) . . ? F122 P1 F152 90.3(6) . . ? F161 P1 F152 100.2(11) . . ? F111 P1 F152 144.8(10) . . ? F151 P1 F152 56.2(10) . . ? F142 P1 F152 178.9(7) . . ? F112 P1 F152 89.5(6) . . ? F132 P1 F152 90.1(5) . . ? F122 P1 F141 124.3(10) . . ? F161 P1 F141 90.2(6) . . ? F111 P1 F141 90.1(6) . . ? F151 P1 F141 179.1(7) . . ? F142 P1 F141 56.8(10) . . ? F112 P1 F141 128.1(10) . . ? F132 P1 F141 51.3(10) . . ? F152 P1 F141 122.9(10) . . ? F122 P1 F121 102.7(11) . . ? F161 P1 F121 90.5(6) . . ? F111 P1 F121 178.7(7) . . ? F151 P1 F121 89.9(6) . . ? F142 P1 F121 144.6(10) . . ? F112 P1 F121 121.9(10) . . ? F132 P1 F121 57.4(10) . . ? F152 P1 F121 35.4(9) . . ? F141 P1 F121 89.3(5) . . ? F122 P1 F131 143.7(9) . . ? F161 P1 F131 179.5(7) . . ? F111 P1 F131 89.7(6) . . ? F151 P1 F131 89.9(5) . . ? F142 P1 F131 99.3(11) . . ? F112 P1 F131 54.7(9) . . ? F132 P1 F131 124.0(10) . . ? F152 P1 F131 79.6(11) . . ? F141 P1 F131 89.6(5) . . ? F121 P1 F131 89.1(6) . . ? F122 P1 F162 179.4(7) . . ? F161 P1 F162 143.0(9) . . ? F111 P1 F162 102.0(11) . . ? F151 P1 F162 123.6(10) . . ? F142 P1 F162 89.7(6) . . ? F112 P1 F162 89.6(5) . . ? F132 P1 F162 89.1(5) . . ? F152 P1 F162 89.3(5) . . ? F141 P1 F162 55.7(10) . . ? F121 P1 F162 76.7(11) . . ? F131 P1 F162 36.6(9) . . ? F211 P2 F261 93.0(5) . . ? F211 P2 F222 159.2(10) . . ? F261 P2 F222 83.8(11) . . ? F211 P2 F232 105.8(10) . . ? F261 P2 F232 125.2(10) . . ? F222 P2 F232 92.6(6) . . ? F211 P2 F252 78.2(11) . . ? F261 P2 F252 142.9(9) . . ? F222 P2 F252 92.1(6) . . ? F232 P2 F252 91.8(7) . . ? F211 P2 F241 92.0(5) . . ? F261 P2 F241 91.7(5) . . ? F222 P2 F241 67.7(9) . . ? F232 P2 F241 136.9(9) . . ? F252 P2 F241 53.3(9) . . ? F211 P2 F251 90.6(5) . . ? F261 P2 F251 90.7(5) . . ? F222 P2 F251 109.9(9) . . ? F232 P2 F251 39.7(9) . . ? F252 P2 F251 125.0(9) . . ? F241 P2 F251 176.5(6) . . ? F211 P2 F242 99.1(11) . . ? F261 P2 F242 36.4(9) . . ? F222 P2 F242 90.4(6) . . ? F232 P2 F242 89.3(11) . . ? F252 P2 F242 177.3(7) . . ? F241 P2 F242 126.9(9) . . ? F251 P2 F242 55.0(9) . . ? F211 P2 F262 71.8(10) . . ? F261 P2 F262 53.3(8) . . ? F222 P2 F262 90.1(5) . . ? F232 P2 F262 176.7(7) . . ? F252 P2 F262 89.9(6) . . ? F241 P2 F262 46.1(8) . . ? F251 P2 F262 137.3(8) . . ? F242 P2 F262 88.9(6) . . ? F211 P2 F231 90.7(5) . . ? F261 P2 F231 176.2(6) . . ? F222 P2 F231 93.2(11) . . ? F232 P2 F231 52.6(9) . . ? F252 P2 F231 39.2(8) . . ? F241 P2 F231 89.2(5) . . ? F251 P2 F231 88.3(5) . . ? F242 P2 F231 141.8(9) . . ? F262 P2 F231 129.0(8) . . ? F211 P2 F212 19.6(9) . . ? F261 P2 F212 93.8(11) . . ? F222 P2 F212 177.4(7) . . ? F232 P2 F212 89.5(5) . . ? F252 P2 F212 89.3(5) . . ? F241 P2 F212 111.6(9) . . ? F251 P2 F212 70.9(9) . . ? F242 P2 F212 88.2(5) . . ? F262 P2 F212 87.6(5) . . ? F231 P2 F212 89.3(11) . . ? F211 P2 F221 177.5(6) . . ? F261 P2 F221 89.2(5) . . ? F222 P2 F221 22.5(9) . . ? F232 P2 F221 71.8(10) . . ? F252 P2 F221 100.8(11) . . ? F241 P2 F221 89.2(5) . . ? F251 P2 F221 88.2(5) . . ? F242 P2 F221 81.9(11) . . ? F262 P2 F221 110.6(10) . . ? F231 P2 F221 87.1(5) . . ? F212 P2 F221 158.9(9) . . ? _diffrn_measured_fraction_theta_max 0.838 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.838 _refine_diff_density_max 1.613 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.170 #===END