Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Andrew L. Gott' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Patrick C. McGowan' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Thomas J. Podesta' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_name 'Dr Patrick McGowan' _publ_contact_author_address ; Chemistry University of Leeds Woodhouse Lane Leeds LS2 9JT UNITED KINGDOM ; _publ_contact_author_phone '+44 (0)113 3436404' _publ_contact_author_fax '+44 (0)113 3436565' _publ_contact_author_email P.C.MCGOWAN@CHEM.LEEDS.AC.UK _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_contact_letter ; The following two sets of data are for the structures included in the paper below which we have just submitted to you. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of New Pendant Arm N-monofunctionalised 1,4,7 Triazacyclononane Fe(II)and Ru(II) Complexes ; #================================================================= data_tjp12 _database_code_CSD 188690 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12.50 H20 Cl3 Fe N4' _chemical_formula_weight 388.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'Fe' 'Fe' 0.3463 0.8444 '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 'C2/c' 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 20.3833(9) _cell_length_b 12.7418(5) _cell_length_c 14.6966(4) _cell_angle_alpha 90.00 _cell_angle_beta 118.778(2) _cell_angle_gamma 90.00 _cell_volume 3345.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.377 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7246 _exptl_absorpt_correction_T_max 0.9599 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17936 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3286 _reflns_number_gt 2561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0443P)^2^+0.5440P] 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 0.0011(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3286 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Fe1 Fe 0.21542(2) 0.43108(3) 0.19938(3) 0.02098(15) Uani 1 1 d . . . Cl2 Cl 0.17767(4) 0.58297(5) 0.08254(5) 0.02610(18) Uani 1 1 d . . . Cl3 Cl 0.32128(4) 0.37848(6) 0.18425(5) 0.0354(2) Uani 1 1 d . . . N1 N 0.25924(13) 0.5331(2) 0.33913(17) 0.0259(5) Uani 1 1 d . . . H13 H 0.2728(17) 0.581(2) 0.330(2) 0.020(9) Uiso 1 1 d . . . N2 N 0.12778(12) 0.33611(17) 0.07731(15) 0.0226(5) Uani 1 1 d . . . C1 C 0.17250(15) 0.2706(2) 0.31167(19) 0.0268(6) Uani 1 1 d . . . H1A H 0.1821 0.2254 0.3716 0.032 Uiso 1 1 calc R . . H1B H 0.1497 0.2269 0.2482 0.032 Uiso 1 1 calc R . . N3 N 0.24392(13) 0.31563(19) 0.32618(16) 0.0246(5) Uani 1 1 d . . . H14 H 0.2697(16) 0.268(2) 0.3252(19) 0.022(8) Uiso 1 1 d . . . N4 N 0.11596(12) 0.44432(16) 0.23064(15) 0.0217(5) Uani 1 1 d . . . C7 C 0.05811(15) 0.3496(2) 0.06379(18) 0.0214(6) Uani 1 1 d . . . C2 C 0.20104(16) 0.5687(2) 0.3656(2) 0.0292(6) Uani 1 1 d . . . H2A H 0.2078 0.6445 0.3826 0.035 Uiso 1 1 calc R . . H2B H 0.2071 0.5304 0.4278 0.035 Uiso 1 1 calc R . . C8 C 0.00731(16) 0.2248(2) -0.0744(2) 0.0320(7) Uani 1 1 d . . . H8 H -0.0337 0.1864 -0.1259 0.038 Uiso 1 1 calc R . . C3 C 0.28973(16) 0.3639(2) 0.43082(19) 0.0292(6) Uani 1 1 d . . . H3A H 0.3319 0.3167 0.4742 0.035 Uiso 1 1 calc R . . H3B H 0.2585 0.3722 0.4651 0.035 Uiso 1 1 calc R . . C9 C 0.04905(15) 0.4354(2) 0.12801(19) 0.0254(6) Uani 1 1 d . . . H9A H 0.0401 0.5032 0.0909 0.031 Uiso 1 1 calc R . . H9B H 0.0049 0.4200 0.1370 0.031 Uiso 1 1 calc R . . C4 C 0.32020(16) 0.4705(2) 0.42250(19) 0.0307(7) Uani 1 1 d . . . H4A H 0.3400 0.5081 0.4895 0.037 Uiso 1 1 calc R . . H4B H 0.3617 0.4610 0.4063 0.037 Uiso 1 1 calc R . . C10 C 0.07828(16) 0.2121(2) -0.0626(2) 0.0323(7) Uani 1 1 d . . . H10 H 0.0867 0.1657 -0.1065 0.039 Uiso 1 1 calc R . . C5 C 0.11872(15) 0.3590(2) 0.30209(19) 0.0259(6) Uani 1 1 d . . . H5A H 0.0679 0.3295 0.2761 0.031 Uiso 1 1 calc R . . H5B H 0.1346 0.3891 0.3717 0.031 Uiso 1 1 calc R . . C11 C 0.13693(16) 0.2681(2) 0.01426(19) 0.0267(6) Uani 1 1 d . . . H11 H 0.1858 0.2581 0.0229 0.032 Uiso 1 1 calc R . . C6 C 0.12244(16) 0.5499(2) 0.27600(19) 0.0261(6) Uani 1 1 d . . . H6A H 0.0856 0.5569 0.3014 0.031 Uiso 1 1 calc R . . H6B H 0.1108 0.6037 0.2217 0.031 Uiso 1 1 calc R . . C12 C -0.00302(15) 0.2940(2) -0.01060(19) 0.0268(6) Uani 1 1 d . . . H12 H -0.0513 0.3037 -0.0172 0.032 Uiso 1 1 calc R . . Cl4 Cl -0.00260(6) 0.10574(8) 0.14916(7) 0.0633(3) Uani 1 1 d . . . C13 C 0.0000 0.0275(4) 0.2500 0.0489(13) Uani 1 2 d S . . H15 H -0.046(2) -0.011(3) 0.224(3) 0.077(13) 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 Fe1 0.0202(2) 0.0242(2) 0.0194(2) 0.00067(14) 0.01022(16) 0.00057(15) Cl2 0.0302(4) 0.0245(4) 0.0256(3) 0.0035(3) 0.0151(3) 0.0011(3) Cl3 0.0266(4) 0.0472(5) 0.0370(4) 0.0013(3) 0.0189(3) 0.0054(3) N1 0.0268(14) 0.0250(14) 0.0249(12) 0.0004(10) 0.0117(10) -0.0023(11) N2 0.0239(13) 0.0234(12) 0.0222(11) 0.0029(9) 0.0124(9) 0.0022(9) C1 0.0294(16) 0.0280(15) 0.0234(13) 0.0064(11) 0.0130(12) 0.0024(12) N3 0.0239(13) 0.0256(13) 0.0250(12) 0.0015(9) 0.0123(10) 0.0041(11) N4 0.0208(12) 0.0247(12) 0.0196(11) 0.0006(8) 0.0097(9) 0.0016(9) C7 0.0234(15) 0.0222(14) 0.0188(12) 0.0048(10) 0.0102(11) 0.0027(11) C2 0.0324(17) 0.0302(16) 0.0246(14) -0.0045(11) 0.0135(12) 0.0010(12) C8 0.0307(17) 0.0325(17) 0.0268(15) -0.0051(12) 0.0091(13) -0.0038(13) C3 0.0312(16) 0.0323(16) 0.0206(13) 0.0024(11) 0.0096(12) 0.0045(13) C9 0.0207(15) 0.0295(15) 0.0245(13) 0.0014(11) 0.0097(11) 0.0040(11) C4 0.0274(16) 0.0363(17) 0.0220(13) 0.0005(12) 0.0067(12) 0.0014(13) C10 0.0350(18) 0.0334(17) 0.0288(14) -0.0077(12) 0.0155(13) 0.0020(13) C5 0.0258(15) 0.0330(16) 0.0223(13) 0.0021(11) 0.0143(11) 0.0005(12) C11 0.0291(16) 0.0275(15) 0.0272(14) 0.0028(11) 0.0165(12) 0.0047(12) C6 0.0298(16) 0.0254(15) 0.0238(14) -0.0023(10) 0.0134(12) 0.0033(12) C12 0.0206(15) 0.0286(16) 0.0278(14) 0.0017(11) 0.0090(12) 0.0004(12) Cl4 0.0547(6) 0.0656(7) 0.0473(5) 0.0146(4) 0.0068(4) -0.0149(5) C13 0.058(4) 0.034(3) 0.051(3) 0.000 0.023(3) 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 Fe1 N2 2.188(2) . ? Fe1 N3 2.221(2) . ? Fe1 N1 2.223(2) . ? Fe1 N4 2.290(2) . ? Fe1 Cl3 2.3699(8) . ? Fe1 Cl2 2.4525(7) . ? N1 C2 1.486(4) . ? N1 C4 1.489(3) . ? N2 C11 1.345(3) . ? N2 C7 1.347(3) . ? C1 N3 1.481(3) . ? C1 C5 1.530(4) . ? N3 C3 1.494(3) . ? N4 C9 1.472(3) . ? N4 C6 1.479(3) . ? N4 C5 1.494(3) . ? C7 C12 1.392(4) . ? C7 C9 1.513(3) . ? C2 C6 1.526(4) . ? C8 C12 1.375(4) . ? C8 C10 1.381(4) . ? C3 C4 1.523(4) . ? C10 C11 1.383(4) . ? Cl4 C13 1.766(3) . ? C13 Cl4 1.766(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N3 95.87(8) . . ? N2 Fe1 N1 152.55(9) . . ? N3 Fe1 N1 77.63(9) . . ? N2 Fe1 N4 75.71(8) . . ? N3 Fe1 N4 77.27(8) . . ? N1 Fe1 N4 76.84(8) . . ? N2 Fe1 Cl3 100.80(6) . . ? N3 Fe1 Cl3 90.53(7) . . ? N1 Fe1 Cl3 105.85(7) . . ? N4 Fe1 Cl3 166.76(6) . . ? N2 Fe1 Cl2 90.30(6) . . ? N3 Fe1 Cl2 167.81(7) . . ? N1 Fe1 Cl2 92.08(7) . . ? N4 Fe1 Cl2 94.17(5) . . ? Cl3 Fe1 Cl2 98.65(3) . . ? C2 N1 C4 113.8(2) . . ? C2 N1 Fe1 113.84(17) . . ? C4 N1 Fe1 104.59(17) . . ? C11 N2 C7 117.8(2) . . ? C11 N2 Fe1 126.27(18) . . ? C7 N2 Fe1 115.93(16) . . ? N3 C1 C5 109.8(2) . . ? C1 N3 C3 113.0(2) . . ? C1 N3 Fe1 107.07(15) . . ? C3 N3 Fe1 111.88(16) . . ? C9 N4 C6 111.7(2) . . ? C9 N4 C5 111.5(2) . . ? C6 N4 C5 112.35(19) . . ? C9 N4 Fe1 105.17(15) . . ? C6 N4 Fe1 105.18(16) . . ? C5 N4 Fe1 110.49(15) . . ? N2 C7 C12 122.2(2) . . ? N2 C7 C9 115.9(2) . . ? C12 C7 C9 121.7(2) . . ? N1 C2 C6 111.4(2) . . ? C12 C8 C10 119.0(3) . . ? N3 C3 C4 111.2(2) . . ? N4 C9 C7 111.3(2) . . ? N1 C4 C3 109.5(2) . . ? C8 C10 C11 118.9(3) . . ? N4 C5 C1 112.5(2) . . ? N2 C11 C10 122.9(3) . . ? N4 C6 C2 111.2(2) . . ? C8 C12 C7 119.3(3) . . ? Cl4 C13 Cl4 111.2(3) 2 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.407 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.098 #===END data_alg8b _database_code_CSD 188691 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H37 Cl4 N4 P Ru' _chemical_formula_weight 739.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0237(2) _cell_length_b 10.4847(2) _cell_length_c 18.6872(5) _cell_angle_alpha 80.5790(11) _cell_angle_beta 79.4510(10) _cell_angle_gamma 66.6670(9) _cell_volume 1587.82(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.909 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9066 _exptl_absorpt_correction_T_max 0.9645 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28938 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6191 _reflns_number_gt 5086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0239P)^2^+2.0222P] 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 0.0066(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6191 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 N1 N 0.7862(3) 0.3283(3) 0.20699(15) 0.0343(6) Uani 1 1 d . . . N2 N 0.8348(4) 0.5506(3) 0.11909(16) 0.0381(7) Uani 1 1 d . . . H2 H 0.8771 0.6191 0.1169 0.046 Uiso 1 1 calc R . . N3 N 0.5230(4) 0.5478(3) 0.15336(15) 0.0344(6) Uani 1 1 d . . . H3 H 0.4169 0.5956 0.1740 0.041 Uiso 1 1 calc R . . N4 N 0.8933(3) 0.4809(3) 0.27375(16) 0.0333(6) Uani 1 1 d . . . Ru1 Ru 0.68853(3) 0.54546(3) 0.220847(14) 0.02752(10) Uani 1 1 d . . . P1 P 0.56260(10) 0.77886(8) 0.23819(5) 0.02762(19) Uani 1 1 d . . . Cl1 Cl 0.51895(10) 0.50422(8) 0.33351(4) 0.03283(19) Uani 1 1 d . . . Cl3 Cl 0.80138(18) 0.18183(12) 0.47289(6) 0.0675(3) Uani 1 1 d . . . C1 C 0.7351(5) 0.5848(4) 0.0577(2) 0.0456(9) Uani 1 1 d . . . H1A H 0.7535 0.6620 0.0240 0.055 Uiso 1 1 calc R . . H1B H 0.7733 0.5024 0.0299 0.055 Uiso 1 1 calc R . . C2 C 0.5600(5) 0.6253(5) 0.0817(2) 0.0496(10) Uani 1 1 d . . . H2A H 0.5090 0.6075 0.0438 0.059 Uiso 1 1 calc R . . H2B H 0.5111 0.7268 0.0867 0.059 Uiso 1 1 calc R . . C3 C 0.5450(6) 0.4021(4) 0.1447(2) 0.0523(10) Uani 1 1 d . . . H3A H 0.6021 0.3788 0.0952 0.063 Uiso 1 1 calc R . . H3B H 0.4368 0.3964 0.1489 0.063 Uiso 1 1 calc R . . C4 C 0.6416(5) 0.2959(4) 0.2014(2) 0.0394(8) Uani 1 1 d . . . H4A H 0.5727 0.3004 0.2494 0.047 Uiso 1 1 calc R . . H4B H 0.6778 0.2005 0.1867 0.047 Uiso 1 1 calc R . . C5 C 0.9070(5) 0.2961(4) 0.1401(2) 0.0455(9) Uani 1 1 d . . . H5A H 0.8551 0.2851 0.1004 0.055 Uiso 1 1 calc R . . H5B H 0.9984 0.2068 0.1504 0.055 Uiso 1 1 calc R . . C6 C 0.9720(5) 0.4118(4) 0.1153(2) 0.0501(10) Uani 1 1 d . . . H6A H 1.0522 0.4042 0.1472 0.060 Uiso 1 1 calc R . . H6B H 1.0277 0.4025 0.0645 0.060 Uiso 1 1 calc R . . C7 C 0.8625(4) 0.2617(4) 0.2747(2) 0.0387(8) Uani 1 1 d . . . H7A H 0.9337 0.1630 0.2688 0.046 Uiso 1 1 calc R . . H7B H 0.7770 0.2635 0.3166 0.046 Uiso 1 1 calc R . . C8 C 0.9610(4) 0.3394(4) 0.2893(2) 0.0389(8) Uani 1 1 d . . . C9 C 1.1100(5) 0.2736(4) 0.3149(2) 0.0504(10) Uani 1 1 d . . . H9 H 1.1538 0.1748 0.3249 0.060 Uiso 1 1 calc R . . C10 C 1.1958(5) 0.3513(4) 0.3260(3) 0.0532(10) Uani 1 1 d . . . H10 H 1.2969 0.3075 0.3450 0.064 Uiso 1 1 calc R . . C11 C 1.1300(4) 0.4947(4) 0.3085(2) 0.0455(9) Uani 1 1 d . . . H11 H 1.1871 0.5508 0.3141 0.055 Uiso 1 1 calc R . . C12 C 0.9808(4) 0.5552(4) 0.2829(2) 0.0372(8) Uani 1 1 d . . . H12 H 0.9373 0.6535 0.2711 0.045 Uiso 1 1 calc R . . C13 C 0.3401(4) 0.8346(3) 0.25684(19) 0.0315(7) Uani 1 1 d . . . C14 C 0.2482(4) 0.8462(4) 0.2017(2) 0.0397(8) Uani 1 1 d . . . H14 H 0.2999 0.8355 0.1528 0.048 Uiso 1 1 calc R . . C15 C 0.0831(5) 0.8730(4) 0.2173(2) 0.0458(9) Uani 1 1 d . . . H15 H 0.0227 0.8809 0.1790 0.055 Uiso 1 1 calc R . . C16 C 0.0063(4) 0.8883(4) 0.2879(2) 0.0437(9) Uani 1 1 d . . . H16 H -0.1066 0.9052 0.2985 0.052 Uiso 1 1 calc R . . C17 C 0.0935(4) 0.8789(4) 0.3431(2) 0.0418(9) Uani 1 1 d . . . H17 H 0.0403 0.8908 0.3918 0.050 Uiso 1 1 calc R . . C18 C 0.2585(4) 0.8524(3) 0.3279(2) 0.0367(8) Uani 1 1 d . . . H18 H 0.3174 0.8462 0.3664 0.044 Uiso 1 1 calc R . . C19 C 0.5909(4) 0.9085(3) 0.16347(18) 0.0321(7) Uani 1 1 d . . . C20 C 0.4666(5) 1.0296(4) 0.1385(2) 0.0412(8) Uani 1 1 d . . . H20 H 0.3574 1.0506 0.1610 0.049 Uiso 1 1 calc R . . C21 C 0.5027(6) 1.1192(4) 0.0808(2) 0.0508(10) Uani 1 1 d . . . H21 H 0.4173 1.2010 0.0642 0.061 Uiso 1 1 calc R . . C22 C 0.6605(6) 1.0914(4) 0.0470(2) 0.0491(10) Uani 1 1 d . . . H22 H 0.6831 1.1525 0.0070 0.059 Uiso 1 1 calc R . . C23 C 0.7846(5) 0.9739(4) 0.0721(2) 0.0442(9) Uani 1 1 d . . . H23 H 0.8938 0.9547 0.0502 0.053 Uiso 1 1 calc R . . C24 C 0.7496(4) 0.8838(4) 0.12952(19) 0.0358(8) Uani 1 1 d . . . H24 H 0.8360 0.8030 0.1462 0.043 Uiso 1 1 calc R . . C25 C 0.6013(4) 0.8420(3) 0.31683(18) 0.0299(7) Uani 1 1 d . . . C26 C 0.6626(4) 0.7477(4) 0.37568(18) 0.0337(7) Uani 1 1 d . . . H26 H 0.6858 0.6513 0.3748 0.040 Uiso 1 1 calc R . . C27 C 0.6905(4) 0.7938(4) 0.43613(19) 0.0374(8) Uani 1 1 d . . . H27 H 0.7323 0.7287 0.4763 0.045 Uiso 1 1 calc R . . C28 C 0.6576(4) 0.9336(4) 0.4376(2) 0.0384(8) Uani 1 1 d . . . H28 H 0.6802 0.9642 0.4780 0.046 Uiso 1 1 calc R . . C29 C 0.5915(4) 1.0293(4) 0.38037(19) 0.0368(8) Uani 1 1 d . . . H29 H 0.5646 1.1260 0.3824 0.044 Uiso 1 1 calc R . . C30 C 0.5644(4) 0.9840(3) 0.31957(19) 0.0324(7) Uani 1 1 d . . . H30 H 0.5207 1.0497 0.2800 0.039 Uiso 1 1 calc R . . Cl2 Cl 1.15314(12) 0.65475(11) 0.07556(6) 0.0491(2) Uani 1 1 d . . . Cl4 Cl 0.87890(16) 0.41405(13) 0.49588(7) 0.0690(3) Uani 1 1 d . . . C40 C 0.7223(5) 0.3560(4) 0.4941(2) 0.0481(9) Uani 1 1 d . . . H40A H 0.6521 0.4166 0.4571 0.058 Uiso 1 1 calc R . . H40B H 0.6543 0.3631 0.5424 0.058 Uiso 1 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 N1 0.0359(16) 0.0351(15) 0.0336(15) -0.0046(12) 0.0015(12) -0.0172(13) N2 0.0385(16) 0.0324(15) 0.0398(17) -0.0051(13) 0.0033(13) -0.0126(13) N3 0.0358(16) 0.0371(16) 0.0324(15) -0.0070(12) -0.0012(12) -0.0161(13) N4 0.0289(15) 0.0282(14) 0.0419(16) -0.0030(12) -0.0026(12) -0.0110(12) Ru1 0.02672(15) 0.02849(15) 0.02847(16) -0.00253(10) -0.00090(10) -0.01288(11) P1 0.0259(4) 0.0288(4) 0.0301(4) -0.0019(3) -0.0038(3) -0.0127(3) Cl1 0.0342(4) 0.0374(4) 0.0293(4) -0.0019(3) -0.0010(3) -0.0180(3) Cl3 0.1134(10) 0.0573(7) 0.0484(6) -0.0075(5) -0.0109(6) -0.0486(7) C1 0.060(2) 0.051(2) 0.0310(19) -0.0040(17) 0.0001(17) -0.028(2) C2 0.053(2) 0.060(3) 0.033(2) 0.0030(18) -0.0073(18) -0.021(2) C3 0.061(3) 0.045(2) 0.063(3) -0.008(2) -0.023(2) -0.025(2) C4 0.051(2) 0.0351(19) 0.042(2) -0.0044(16) -0.0069(17) -0.0252(17) C5 0.050(2) 0.0342(19) 0.046(2) -0.0118(17) 0.0110(18) -0.0140(17) C6 0.042(2) 0.040(2) 0.054(2) -0.0089(18) 0.0191(19) -0.0102(17) C7 0.040(2) 0.0282(17) 0.045(2) 0.0013(15) -0.0081(16) -0.0109(15) C8 0.0368(19) 0.0317(18) 0.046(2) 0.0004(16) -0.0084(16) -0.0114(15) C9 0.041(2) 0.038(2) 0.066(3) -0.0029(19) -0.0115(19) -0.0076(17) C10 0.0293(19) 0.054(2) 0.073(3) -0.003(2) -0.0181(19) -0.0084(18) C11 0.0296(19) 0.048(2) 0.063(3) -0.0071(19) -0.0103(17) -0.0165(17) C12 0.0284(17) 0.0343(18) 0.049(2) -0.0038(16) -0.0049(15) -0.0123(15) C13 0.0278(17) 0.0277(16) 0.0404(19) -0.0030(14) -0.0050(14) -0.0118(13) C14 0.0349(19) 0.0390(19) 0.049(2) -0.0111(17) -0.0082(16) -0.0141(16) C15 0.035(2) 0.037(2) 0.071(3) -0.0121(19) -0.0181(19) -0.0125(16) C16 0.0264(18) 0.0340(19) 0.072(3) -0.0075(18) -0.0046(18) -0.0126(15) C17 0.0308(19) 0.039(2) 0.052(2) -0.0022(17) 0.0021(17) -0.0132(15) C18 0.0325(18) 0.0329(18) 0.045(2) -0.0001(15) -0.0041(15) -0.0147(15) C19 0.0381(19) 0.0330(17) 0.0317(17) -0.0019(14) -0.0079(14) -0.0191(15) C20 0.042(2) 0.0385(19) 0.045(2) 0.0050(16) -0.0120(17) -0.0178(16) C21 0.065(3) 0.043(2) 0.050(2) 0.0129(18) -0.026(2) -0.025(2) C22 0.069(3) 0.049(2) 0.040(2) 0.0102(18) -0.015(2) -0.035(2) C23 0.053(2) 0.049(2) 0.040(2) 0.0000(17) -0.0036(18) -0.0318(19) C24 0.0395(19) 0.0347(18) 0.0365(19) 0.0010(15) -0.0057(15) -0.0189(16) C25 0.0225(15) 0.0351(17) 0.0327(17) -0.0067(14) 0.0009(13) -0.0122(13) C26 0.0314(18) 0.0354(18) 0.0364(18) -0.0026(15) -0.0059(14) -0.0144(15) C27 0.0383(19) 0.043(2) 0.0330(18) -0.0025(15) -0.0073(15) -0.0171(16) C28 0.0351(19) 0.047(2) 0.039(2) -0.0137(17) -0.0009(15) -0.0194(16) C29 0.0330(18) 0.0371(19) 0.042(2) -0.0111(16) 0.0006(15) -0.0144(15) C30 0.0291(17) 0.0335(17) 0.0357(18) -0.0024(14) -0.0037(14) -0.0138(14) Cl2 0.0435(5) 0.0587(6) 0.0539(6) -0.0220(5) 0.0068(4) -0.0279(5) Cl4 0.0783(8) 0.0583(7) 0.0875(9) -0.0013(6) -0.0247(7) -0.0400(6) C40 0.052(2) 0.049(2) 0.045(2) -0.0027(18) -0.0095(18) -0.0211(19) _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 N1 C7 1.488(5) . ? N1 C5 1.488(4) . ? N1 C4 1.497(4) . ? N1 Ru1 2.133(3) . ? N2 C6 1.493(5) . ? N2 C1 1.498(5) . ? N2 Ru1 2.113(3) . ? N3 C3 1.492(5) . ? N3 C2 1.503(5) . ? N3 Ru1 2.115(3) . ? N4 C12 1.356(4) . ? N4 C8 1.365(4) . ? N4 Ru1 2.076(3) . ? Ru1 P1 2.3036(9) . ? Ru1 Cl1 2.4510(8) . ? P1 C13 1.838(3) . ? P1 C19 1.840(3) . ? P1 C25 1.847(3) . ? Cl3 C40 1.761(4) . ? C1 C2 1.466(6) . ? C3 C4 1.519(5) . ? C5 C6 1.520(5) . ? C7 C8 1.505(5) . ? C8 C9 1.380(5) . ? C9 C10 1.385(6) . ? C10 C11 1.387(6) . ? C11 C12 1.380(5) . ? C13 C18 1.398(5) . ? C13 C14 1.398(5) . ? C14 C15 1.386(5) . ? C15 C16 1.376(6) . ? C16 C17 1.377(6) . ? C17 C18 1.386(5) . ? C19 C24 1.395(5) . ? C19 C20 1.399(5) . ? C20 C21 1.391(5) . ? C21 C22 1.383(6) . ? C22 C23 1.379(6) . ? C23 C24 1.387(5) . ? C25 C26 1.388(5) . ? C25 C30 1.398(5) . ? C26 C27 1.397(5) . ? C27 C28 1.380(5) . ? C28 C29 1.384(5) . ? C29 C30 1.396(5) . ? Cl4 C40 1.753(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 C7 N1 C5 111.8(3) . . ? C7 N1 C4 113.8(3) . . ? C5 N1 C4 110.9(3) . . ? C7 N1 Ru1 103.4(2) . . ? C5 N1 Ru1 111.8(2) . . ? C4 N1 Ru1 104.7(2) . . ? C6 N2 C1 112.1(3) . . ? C6 N2 Ru1 107.7(2) . . ? C1 N2 Ru1 110.3(2) . . ? C3 N3 C2 112.0(3) . . ? C3 N3 Ru1 110.2(2) . . ? C2 N3 Ru1 105.4(2) . . ? C12 N4 C8 117.1(3) . . ? C12 N4 Ru1 128.9(2) . . ? C8 N4 Ru1 113.0(2) . . ? N4 Ru1 N2 89.69(11) . . ? N4 Ru1 N3 161.29(11) . . ? N2 Ru1 N3 82.22(11) . . ? N4 Ru1 N1 80.34(11) . . ? N2 Ru1 N1 81.09(11) . . ? N3 Ru1 N1 81.75(11) . . ? N4 Ru1 P1 103.01(8) . . ? N2 Ru1 P1 102.03(8) . . ? N3 Ru1 P1 95.19(8) . . ? N1 Ru1 P1 175.35(8) . . ? N4 Ru1 Cl1 92.57(8) . . ? N2 Ru1 Cl1 170.67(8) . . ? N3 Ru1 Cl1 92.91(8) . . ? N1 Ru1 Cl1 90.37(8) . . ? P1 Ru1 Cl1 86.28(3) . . ? C13 P1 C19 102.89(15) . . ? C13 P1 C25 99.98(15) . . ? C19 P1 C25 101.06(15) . . ? C13 P1 Ru1 112.12(10) . . ? C19 P1 Ru1 118.73(11) . . ? C25 P1 Ru1 119.27(11) . . ? C2 C1 N2 113.8(3) . . ? C1 C2 N3 112.9(3) . . ? N3 C3 C4 112.4(3) . . ? N1 C4 C3 108.5(3) . . ? N1 C5 C6 110.8(3) . . ? N2 C6 C5 109.7(3) . . ? N1 C7 C8 109.4(3) . . ? N4 C8 C9 122.2(3) . . ? N4 C8 C7 114.8(3) . . ? C9 C8 C7 123.0(3) . . ? C8 C9 C10 120.1(4) . . ? C9 C10 C11 118.2(4) . . ? C12 C11 C10 119.4(4) . . ? N4 C12 C11 123.1(3) . . ? C18 C13 C14 117.4(3) . . ? C18 C13 P1 121.3(3) . . ? C14 C13 P1 121.0(3) . . ? C15 C14 C13 121.1(4) . . ? C16 C15 C14 120.2(4) . . ? C15 C16 C17 119.8(3) . . ? C16 C17 C18 120.2(4) . . ? C17 C18 C13 121.2(4) . . ? C24 C19 C20 117.7(3) . . ? C24 C19 P1 117.0(3) . . ? C20 C19 P1 125.2(3) . . ? C21 C20 C19 120.0(4) . . ? C22 C21 C20 121.3(4) . . ? C23 C22 C21 119.2(4) . . ? C22 C23 C24 119.8(4) . . ? C23 C24 C19 121.8(3) . . ? C26 C25 C30 119.2(3) . . ? C26 C25 P1 119.5(2) . . ? C30 C25 P1 121.3(3) . . ? C25 C26 C27 120.4(3) . . ? C28 C27 C26 120.1(3) . . ? C27 C28 C29 120.1(3) . . ? C28 C29 C30 120.1(3) . . ? C29 C30 C25 120.1(3) . . ? Cl4 C40 Cl3 111.1(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.666 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.082