data_complex_4b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H32 Cl F3 N3 O8 Ru' _chemical_formula_sum 'C20 H32 Cl F3 N3 O8 Ru' _chemical_formula_weight 636.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ru' 'Ru' -1.2594 0.8363 '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' 'O' 'O' 0.0106 0.0060 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.671(6) _cell_length_b 7.705(2) _cell_length_c 20.991(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.95(3) _cell_angle_gamma 90.00 _cell_volume 5094.8(19) _cell_formula_units_Z 8 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4793 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.2088 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 23.47 _reflns_number_total 2089 _reflns_number_gt 1003 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution 'SIR-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1008P)^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 2089 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.2036 _refine_ls_wR_factor_gt 0.1743 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.88393(5) 0.14543(17) 0.09093(6) 0.0415(7) Uani 1 1 d . . . F1 F 0.9015(4) -0.1381(14) -0.0995(5) 0.102(4) Uiso 1 1 d . . . F2 F 0.8390(4) -0.2290(16) -0.1065(5) 0.108(4) Uiso 1 1 d . . . F3 F 0.8538(4) 0.0001(15) -0.1536(5) 0.107(4) Uiso 1 1 d . . . O1 O 0.8165(3) 0.1877(13) 0.0739(5) 0.044(3) Uani 1 1 d . . . O2 O 0.8650(3) -0.0619(12) 0.1326(5) 0.043(3) Uani 1 1 d . . . O3 O 0.8824(4) 0.0215(12) 0.0018(5) 0.047(4) Uani 1 1 d . . . O4 O 0.8168(5) 0.0876(15) -0.0446(5) 0.071(4) Uiso 1 1 d . . . N1 N 0.8939(5) 0.2716(16) 0.1810(6) 0.047(5) Uani 1 1 d . . . N2 N 0.9016(4) 0.3906(16) 0.0541(6) 0.047(4) Uani 1 1 d . . . N3 N 0.9485(4) 0.1006(15) 0.1051(6) 0.047(4) Uani 1 1 d . . . C1 C 0.7488(6) 0.033(2) 0.0734(8) 0.066(6) Uiso 1 1 d . . . H1A H 0.7338 0.1408 0.0744 0.100 Uiso 1 1 calc R . . H1B H 0.7339 -0.0552 0.0944 0.100 Uiso 1 1 calc R . . H1C H 0.7508 -0.0006 0.0297 0.100 Uiso 1 1 calc R . . C2 C 0.7927(6) 0.054(2) 0.1073(8) 0.063(6) Uiso 1 1 d . . . H2 H 0.7900 0.0950 0.1509 0.076 Uiso 1 1 calc R . . C3 C 0.8203(6) -0.113(2) 0.1121(8) 0.046(5) Uiso 1 1 d . . . H3 H 0.8190 -0.1669 0.0698 0.055 Uiso 1 1 calc R . . C4 C 0.8062(6) -0.241(2) 0.1586(8) 0.042(5) Uiso 1 1 d . . . C5 C 0.8203(5) -0.246(2) 0.2224(7) 0.044(5) Uiso 1 1 d . . . H5 H 0.8423 -0.1728 0.2378 0.053 Uiso 1 1 calc R . . C6 C 0.8033(6) -0.357(2) 0.2654(8) 0.049(5) Uiso 1 1 d . . . H6 H 0.8131 -0.3546 0.3087 0.059 Uiso 1 1 calc R . . C7 C 0.7723(6) -0.469(2) 0.2434(8) 0.054(5) Uiso 1 1 d . . . H7 H 0.7610 -0.5453 0.2717 0.064 Uiso 1 1 calc R . . C8 C 0.7575(6) -0.472(2) 0.1804(8) 0.069(6) Uiso 1 1 d . . . H8 H 0.7364 -0.5501 0.1657 0.082 Uiso 1 1 calc R . . C9 C 0.7741(6) -0.3570(19) 0.1374(8) 0.050(5) Uiso 1 1 d . . . H9 H 0.7635 -0.3587 0.0944 0.060 Uiso 1 1 calc R . . C10 C 0.8510(8) 0.020(2) -0.0423(9) 0.060(6) Uiso 1 1 d . . . C11 C 0.8627(8) -0.088(3) -0.0997(11) 0.094(8) Uiso 1 1 d . . . C12 C 0.9035(6) 0.457(2) 0.1675(8) 0.063(6) Uiso 1 1 d . . . H12A H 0.8918 0.5294 0.1990 0.075 Uiso 1 1 calc R . . H12B H 0.9341 0.4728 0.1723 0.075 Uiso 1 1 calc R . . C13 C 0.8866(6) 0.513(2) 0.1036(7) 0.057(6) Uiso 1 1 d . . . H13A H 0.8963 0.6302 0.0960 0.069 Uiso 1 1 calc R . . H13B H 0.8559 0.5141 0.1003 0.069 Uiso 1 1 calc R . . C14 C 0.9486(6) 0.388(2) 0.0499(9) 0.064(6) Uiso 1 1 d . . . H14A H 0.9626 0.4566 0.0848 0.076 Uiso 1 1 calc R . . H14B H 0.9545 0.4422 0.0100 0.076 Uiso 1 1 calc R . . C15 C 0.9672(6) 0.205(2) 0.0531(8) 0.065(6) Uiso 1 1 d . . . H15A H 0.9608 0.1476 0.0120 0.078 Uiso 1 1 calc R . . H15B H 0.9978 0.2107 0.0623 0.078 Uiso 1 1 calc R . . C16 C 0.9652(6) 0.163(2) 0.1716(8) 0.059(6) Uiso 1 1 d . . . H16A H 0.9864 0.0819 0.1903 0.071 Uiso 1 1 calc R . . H16B H 0.9785 0.2751 0.1685 0.071 Uiso 1 1 calc R . . C17 C 0.9299(6) 0.176(2) 0.2138(8) 0.049(5) Uiso 1 1 d . . . H17A H 0.9208 0.0608 0.2249 0.059 Uiso 1 1 calc R . . H17B H 0.9400 0.2358 0.2532 0.059 Uiso 1 1 calc R . . C18 C 0.8561(6) 0.268(2) 0.2212(8) 0.068(6) Uiso 1 1 d . . . H18A H 0.8485 0.1503 0.2290 0.101 Uiso 1 1 calc R . . H18B H 0.8324 0.3268 0.1984 0.101 Uiso 1 1 calc R . . H18C H 0.8638 0.3261 0.2612 0.101 Uiso 1 1 calc R . . C19 C 0.8785(6) 0.436(2) -0.0098(8) 0.065(6) Uiso 1 1 d . . . H19A H 0.8874 0.3598 -0.0419 0.097 Uiso 1 1 calc R . . H19B H 0.8849 0.5539 -0.0203 0.097 Uiso 1 1 calc R . . H19C H 0.8485 0.4241 -0.0078 0.097 Uiso 1 1 calc R . . C20 C 0.9588(6) -0.082(2) 0.0946(8) 0.075(6) Uiso 1 1 d . . . H20A H 0.9471 -0.1171 0.0525 0.112 Uiso 1 1 calc R . . H20B H 0.9470 -0.1531 0.1260 0.112 Uiso 1 1 calc R . . H20C H 0.9891 -0.0968 0.0984 0.112 Uiso 1 1 calc R . . Cl1 Cl 0.9444(2) 0.3599(10) -0.1624(3) 0.101(2) Uani 1 1 d . . . O5 O 0.9554(6) 0.320(2) -0.1013(9) 0.160(7) Uiso 1 1 d . . . O6 O 0.9486(7) 0.218(3) -0.2094(11) 0.199(9) Uiso 1 1 d . . . O7 O 0.9007(6) 0.434(2) -0.1659(7) 0.132(6) Uiso 1 1 d . . . O8 O 0.9725(8) 0.477(3) -0.1820(11) 0.198(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0503(14) 0.0400(10) 0.0332(9) -0.0003(8) -0.0006(8) 0.0008(10) O1 0.022(8) 0.058(8) 0.050(7) 0.003(6) 0.001(6) -0.003(6) O2 0.043(9) 0.042(7) 0.044(7) 0.001(5) 0.005(6) 0.003(6) O3 0.042(9) 0.060(8) 0.038(7) -0.004(6) -0.002(7) 0.005(7) N1 0.059(13) 0.040(9) 0.039(9) -0.005(7) -0.014(9) -0.003(9) N2 0.033(11) 0.053(10) 0.057(9) 0.005(8) 0.017(9) -0.013(8) N3 0.042(12) 0.044(10) 0.054(9) -0.003(8) -0.001(9) 0.004(8) Cl1 0.084(6) 0.145(6) 0.074(4) 0.046(5) 0.008(4) 0.022(5) _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 Ru1 O2 1.945(10) . ? Ru1 N3 2.065(13) . ? Ru1 O3 2.097(10) . ? Ru1 N1 2.120(12) . ? Ru1 N2 2.138(12) . ? Ru1 O1 2.154(10) . ? F1 C11 1.29(2) . ? F2 C11 1.32(2) . ? F3 C11 1.33(2) . ? O1 C2 1.494(19) . ? O2 C3 1.490(18) . ? O3 C10 1.29(2) . ? O4 C10 1.20(2) . ? N1 C17 1.466(18) . ? N1 C12 1.491(18) . ? N1 C18 1.53(2) . ? N2 C14 1.50(2) . ? N2 C19 1.501(17) . ? N2 C13 1.518(19) . ? N3 C20 1.470(18) . ? N3 C16 1.517(18) . ? N3 C15 1.52(2) . ? C1 C2 1.50(2) . ? C2 C3 1.55(2) . ? C3 C4 1.49(2) . ? C4 C5 1.369(18) . ? C4 C9 1.394(19) . ? C5 C6 1.39(2) . ? C6 C7 1.352(19) . ? C7 C8 1.355(19) . ? C8 C9 1.40(2) . ? C10 C11 1.54(3) . ? C12 C13 1.458(18) . ? C14 C15 1.53(2) . ? C16 C17 1.50(2) . ? Cl1 O5 1.330(18) . ? Cl1 O8 1.36(2) . ? Cl1 O6 1.49(2) . ? Cl1 O7 1.491(19) . ? 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 O2 Ru1 N3 98.3(5) . . ? O2 Ru1 O3 92.7(4) . . ? N3 Ru1 O3 89.0(5) . . ? O2 Ru1 N1 90.0(5) . . ? N3 Ru1 N1 83.9(5) . . ? O3 Ru1 N1 172.7(5) . . ? O2 Ru1 N2 173.1(5) . . ? N3 Ru1 N2 84.7(5) . . ? O3 Ru1 N2 93.6(4) . . ? N1 Ru1 N2 84.1(5) . . ? O2 Ru1 O1 81.5(4) . . ? N3 Ru1 O1 178.5(4) . . ? O3 Ru1 O1 89.4(4) . . ? N1 Ru1 O1 97.6(5) . . ? N2 Ru1 O1 95.7(5) . . ? C2 O1 Ru1 110.9(9) . . ? C3 O2 Ru1 114.4(8) . . ? C10 O3 Ru1 126.2(12) . . ? C17 N1 C12 113.9(13) . . ? C17 N1 C18 110.2(12) . . ? C12 N1 C18 107.8(13) . . ? C17 N1 Ru1 103.1(9) . . ? C12 N1 Ru1 106.5(9) . . ? C18 N1 Ru1 115.4(10) . . ? C14 N2 C19 110.2(13) . . ? C14 N2 C13 115.5(13) . . ? C19 N2 C13 107.9(12) . . ? C14 N2 Ru1 108.0(9) . . ? C19 N2 Ru1 114.1(9) . . ? C13 N2 Ru1 101.0(9) . . ? C20 N3 C16 112.2(12) . . ? C20 N3 C15 106.8(14) . . ? C16 N3 C15 111.7(12) . . ? C20 N3 Ru1 111.8(10) . . ? C16 N3 Ru1 109.0(10) . . ? C15 N3 Ru1 105.2(9) . . ? O1 C2 C1 109.8(13) . . ? O1 C2 C3 107.2(15) . . ? C1 C2 C3 115.4(15) . . ? C4 C3 O2 109.0(12) . . ? C4 C3 C2 112.8(16) . . ? O2 C3 C2 108.4(12) . . ? C5 C4 C9 116.4(16) . . ? C5 C4 C3 125.0(16) . . ? C9 C4 C3 118.4(14) . . ? C4 C5 C6 123.1(16) . . ? C7 C6 C5 119.2(16) . . ? C6 C7 C8 120.4(18) . . ? C7 C8 C9 120.3(18) . . ? C4 C9 C8 120.6(16) . . ? O4 C10 O3 130.8(19) . . ? O4 C10 C11 120(2) . . ? O3 C10 C11 110(2) . . ? F1 C11 F2 106.6(19) . . ? F1 C11 F3 106(2) . . ? F2 C11 F3 105.1(18) . . ? F1 C11 C10 118(2) . . ? F2 C11 C10 110(2) . . ? F3 C11 C10 110.1(18) . . ? C13 C12 N1 113.4(13) . . ? C12 C13 N2 109.4(14) . . ? N2 C14 C15 112.8(14) . . ? N3 C15 C14 109.9(15) . . ? C17 C16 N3 110.9(14) . . ? N1 C17 C16 110.3(14) . . ? O5 Cl1 O8 109.5(13) . . ? O5 Cl1 O6 115.8(13) . . ? O8 Cl1 O6 100.4(14) . . ? O5 Cl1 O7 106.6(12) . . ? O8 Cl1 O7 111.4(13) . . ? O6 Cl1 O7 113.2(12) . . ? _diffrn_measured_fraction_theta_max 0.555 _diffrn_reflns_theta_full 23.47 _diffrn_measured_fraction_theta_full 0.555 _refine_diff_density_max 0.998 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.131