# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ; Prof. Dr. Nicolai Burzlaff Department of Chemistry and Pharmacy University of Erlangen-N\"urnberg Egerlandstrasse 1 D-91058 Erlangen Germany ; _publ_contact_author_phone 49(9131)8528976 _publ_contact_author_fax 49(9131)8527387 _publ_contact_author_email burzlaff@chemie.uni-erlangen.de _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider these CIF submission (5 compounds) for structural data deposition. We are awaiting a notice about the assigned CSD numbers. ; #-------------------------------------------------------------------------- # 2. TITLE AND AUTHOR LIST _publ_section_title ; Transition metal complexe bearing a 2,2-bis(3,5-dimethylpyrazol-1-yl)propionate ligand: one methyl more matters ; loop_ _publ_author_name _publ_author_address G.Turkoglu ; Department of Chemistry and Pharmacy University of Erlangen-N\"urnberg Egerlandstrasse 1 D-91058 Erlangen Germany ; S.Tampier ; Department of Chemistry and Pharmacy University of Erlangen-N\"urnberg Egerlandstrasse 1 D-91058 Erlangen Germany; ; F.W.Heinemann ; Department of Chemistry and Pharmacy University of Erlangen-N\"urnberg Egerlandstrasse 1 D-91058 Erlangen Germany ; N.Burzlaff ; Department of Chemistry and Pharmacy University of Erlangen-N\"urnberg Egerlandstrasse 1 D-91058 Erlangen Germany ; _publ_contact_author_name 'Prof. Dr. Nicolai Burzlaff' #------------------------------------------------------------------------- data_gtbu07 _database_code_depnum_ccdc_archive 'CCDC 805960' _audit_creation_date 2010-04-23T14:09:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H17 Mn1 N4 O5' _chemical_formula_sum 'C16 H17 Mn N4 O5' _chemical_formula_weight 400.28 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2964(6) _cell_length_b 9.6530(3) _cell_length_c 11.393 _cell_angle_alpha 105.882(4) _cell_angle_beta 99.171(6) _cell_angle_gamma 104.865(3) _cell_volume 821.92(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 152 _cell_measurement_theta_min 6 _cell_measurement_theta_max 20 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_absorpt_correction_T_min 0.893648 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 2.00 \% and 40 sec per frame ; _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_av_unetI/netI 0.0512 _diffrn_reflns_number 20009 _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 -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 28.5 _diffrn_reflns_theta_full 28.5 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 4148 _reflns_number_gt 3168 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.5353P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 4148 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.351 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5234(2) 0.4110(2) 0.22359(16) 0.0131(4) Uani 1 1 d . . . C2 C 0.3244(2) 0.3430(2) 0.15332(16) 0.0119(4) Uani 1 1 d . . . C3 C 0.2900(3) 0.4333(2) 0.06794(18) 0.0182(4) Uani 1 1 d . . . H3A H 0.3618 0.4266 0.0097 0.027 Uiso 1 1 calc R . . H3B H 0.3151 0.5377 0.1178 0.027 Uiso 1 1 calc R . . H3C H 0.1713 0.393 0.0222 0.027 Uiso 1 1 calc R . . C11 C 0.1230(3) 0.2396(2) 0.51302(18) 0.0210(4) Uani 1 1 d . . . H11A H 0.1251 0.1368 0.4899 0.031 Uiso 1 1 calc R . . H11B H 0.0185 0.2437 0.5376 0.031 Uiso 1 1 calc R . . H11C H 0.2199 0.3028 0.5821 0.031 Uiso 1 1 calc R . . C12 C 0.1318(2) 0.2952(2) 0.40292(17) 0.0150(4) Uani 1 1 d . . . C13 C 0.0302(2) 0.3745(2) 0.35910(17) 0.0166(4) Uani 1 1 d . . . H13 H -0.0588 0.3994 0.3911 0.02 Uiso 1 1 calc R . . C14 C 0.0854(2) 0.4088(2) 0.26081(17) 0.0141(4) Uani 1 1 d . . . C15 C 0.0129(3) 0.4970(2) 0.1887(2) 0.0217(4) Uani 1 1 d . . . H15A H -0.085 0.516 0.2166 0.033 Uiso 1 1 calc R . . H15B H -0.0217 0.4397 0.1005 0.033 Uiso 1 1 calc R . . H15C H 0.099 0.5919 0.2029 0.033 Uiso 1 1 calc R . . C21 C 0.3590(3) -0.1716(2) 0.08751(19) 0.0200(4) Uani 1 1 d . . . H21A H 0.4779 -0.1364 0.1324 0.03 Uiso 1 1 calc R . . H21B H 0.3415 -0.2519 0.0105 0.03 Uiso 1 1 calc R . . H21C H 0.2885 -0.2088 0.1384 0.03 Uiso 1 1 calc R . . C22 C 0.3110(2) -0.0436(2) 0.05830(17) 0.0149(4) Uani 1 1 d . . . C23 C 0.2221(2) -0.0469(2) -0.05778(17) 0.0169(4) Uani 1 1 d . . . H23 H 0.1805 -0.1298 -0.1316 0.02 Uiso 1 1 calc R . . C24 C 0.2074(2) 0.0950(2) -0.04275(16) 0.0151(4) Uani 1 1 d . . . C25 C 0.1168(3) 0.1418(2) -0.14268(18) 0.0240(5) Uani 1 1 d . . . H25A H 0.0286 0.1796 -0.1142 0.036 Uiso 1 1 calc R . . H25B H 0.0658 0.0559 -0.2182 0.036 Uiso 1 1 calc R . . H25C H 0.198 0.2201 -0.1596 0.036 Uiso 1 1 calc R . . C31 C 0.5138(2) 0.2635(2) 0.50765(18) 0.0167(4) Uani 1 1 d . . . C41 C 0.3037(2) 0.0093(2) 0.35604(17) 0.0150(4) Uani 1 1 d . . . C51 C 0.6095(2) 0.0969(2) 0.34128(17) 0.0164(4) Uani 1 1 d . . . Mn1 Mn 0.43479(4) 0.17730(3) 0.33767(3) 0.01206(8) Uani 1 1 d . . . N11 N 0.24501(19) 0.27814(17) 0.33289(14) 0.0128(3) Uani 1 1 d . . . N12 N 0.21755(19) 0.34945(16) 0.24531(13) 0.0118(3) Uani 1 1 d . . . N21 N 0.34967(19) 0.09433(16) 0.14369(14) 0.0120(3) Uani 1 1 d . . . N22 N 0.28811(19) 0.18105(17) 0.08071(13) 0.0117(3) Uani 1 1 d . . . O1 O 0.57696(16) 0.36249(14) 0.31048(12) 0.0166(3) Uani 1 1 d . . . O2 O 0.61310(17) 0.50645(15) 0.18845(13) 0.0213(3) Uani 1 1 d . . . O31 O 0.56657(19) 0.31374(17) 0.61490(13) 0.0267(3) Uani 1 1 d . . . O41 O 0.22161(19) -0.10098(16) 0.36651(13) 0.0243(3) Uani 1 1 d . . . O51 O 0.71802(19) 0.04402(17) 0.34889(13) 0.0269(3) Uani 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 C1 0.0120(9) 0.0124(9) 0.0137(9) 0.0015(7) 0.0050(7) 0.0038(7) C2 0.0128(9) 0.0119(9) 0.0120(9) 0.0045(7) 0.0048(7) 0.0040(7) C3 0.0197(10) 0.0195(10) 0.0199(10) 0.0105(8) 0.0066(8) 0.0083(8) C11 0.0207(10) 0.0281(11) 0.0146(10) 0.0075(8) 0.0084(8) 0.0057(9) C12 0.0138(9) 0.0145(9) 0.0127(9) 0.0008(7) 0.0042(7) 0.0011(7) C13 0.0133(9) 0.0166(10) 0.0165(9) -0.0002(8) 0.0057(7) 0.0039(7) C14 0.0111(9) 0.0110(9) 0.0163(9) -0.0005(7) 0.0020(7) 0.0034(7) C15 0.0188(10) 0.0239(11) 0.0283(11) 0.0113(9) 0.0070(9) 0.0128(9) C21 0.0241(11) 0.0124(9) 0.0229(10) 0.0045(8) 0.0079(8) 0.0051(8) C22 0.0142(9) 0.0127(9) 0.0178(9) 0.0043(7) 0.0079(7) 0.0029(7) C23 0.0173(10) 0.0145(9) 0.0133(9) -0.0004(7) 0.0040(7) 0.0010(7) C24 0.0109(9) 0.0221(10) 0.0103(9) 0.0031(7) 0.0031(7) 0.0040(7) C25 0.0235(11) 0.0325(12) 0.0146(10) 0.0061(9) -0.0009(8) 0.0118(9) C31 0.0141(9) 0.0157(9) 0.0211(11) 0.0070(8) 0.0026(8) 0.0060(8) C41 0.0160(10) 0.0180(10) 0.0115(9) 0.0044(8) 0.0015(7) 0.0077(8) C51 0.0179(10) 0.0184(10) 0.0112(9) 0.0048(8) 0.0025(7) 0.0035(8) Mn1 0.01224(14) 0.01299(14) 0.01120(14) 0.00491(11) 0.00188(10) 0.00404(11) N11 0.0145(8) 0.0129(8) 0.0111(8) 0.0042(6) 0.0038(6) 0.0040(6) N12 0.0115(7) 0.0121(7) 0.0121(7) 0.0041(6) 0.0028(6) 0.0042(6) N21 0.0127(8) 0.0124(8) 0.0125(8) 0.0058(6) 0.0036(6) 0.0045(6) N22 0.0132(8) 0.0131(8) 0.0096(7) 0.0040(6) 0.0026(6) 0.0051(6) O1 0.0137(7) 0.0162(7) 0.0187(7) 0.0079(6) 0.0012(5) 0.0020(5) O2 0.0169(7) 0.0242(8) 0.0231(7) 0.0126(6) 0.0072(6) 0.0003(6) O31 0.0279(8) 0.0312(8) 0.0145(7) 0.0004(6) -0.0026(6) 0.0109(7) O41 0.0271(8) 0.0216(8) 0.0257(8) 0.0128(6) 0.0077(6) 0.0042(6) O51 0.0245(8) 0.0380(9) 0.0251(8) 0.0115(7) 0.0063(6) 0.0200(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.228(2) . ? C1 O1 1.272(2) . ? C1 C2 1.591(2) . ? C2 N12 1.475(2) . ? C2 N22 1.480(2) . ? C2 C3 1.513(2) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C11 C12 1.498(2) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 N11 1.338(2) . ? C12 C13 1.398(3) . ? C13 C14 1.364(3) . ? C13 H13 0.93 . ? C14 N12 1.375(2) . ? C14 C15 1.500(3) . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C21 C22 1.494(3) . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 N21 1.340(2) . ? C22 C23 1.396(3) . ? C23 C24 1.372(3) . ? C23 H23 0.93 . ? C24 N22 1.375(2) . ? C24 C25 1.500(3) . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C31 O31 1.147(2) . ? C31 Mn1 1.818(2) . ? C41 O41 1.155(2) . ? C41 Mn1 1.7918(19) . ? C51 O51 1.146(2) . ? C51 Mn1 1.811(2) . ? Mn1 O1 2.0051(13) . ? Mn1 N11 2.0537(15) . ? Mn1 N21 2.0658(15) . ? N11 N12 1.380(2) . ? N21 N22 1.3812(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 C1 O1 125.32(17) . . ? O2 C1 C2 116.69(16) . . ? O1 C1 C2 117.98(15) . . ? N12 C2 N22 107.37(13) . . ? N12 C2 C3 111.91(14) . . ? N22 C2 C3 111.54(14) . . ? N12 C2 C1 110.58(14) . . ? N22 C2 C1 107.94(14) . . ? C3 C2 C1 107.46(14) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N11 C12 C13 109.57(16) . . ? N11 C12 C11 123.73(17) . . ? C13 C12 C11 126.67(17) . . ? C14 C13 C12 107.54(16) . . ? C14 C13 H13 126.2 . . ? C12 C13 H13 126.2 . . ? C13 C14 N12 106.50(16) . . ? C13 C14 C15 124.72(17) . . ? N12 C14 C15 128.77(16) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N21 C22 C23 109.93(16) . . ? N21 C22 C21 123.32(17) . . ? C23 C22 C21 126.75(17) . . ? C24 C23 C22 107.32(16) . . ? C24 C23 H23 126.3 . . ? C22 C23 H23 126.3 . . ? C23 C24 N22 106.35(16) . . ? C23 C24 C25 125.60(17) . . ? N22 C24 C25 128.04(17) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O31 C31 Mn1 177.43(17) . . ? O41 C41 Mn1 178.34(17) . . ? O51 C51 Mn1 176.42(16) . . ? C41 Mn1 C51 88.24(8) . . ? C41 Mn1 C31 90.46(8) . . ? C51 Mn1 C31 87.29(8) . . ? C41 Mn1 O1 177.92(7) . . ? C51 Mn1 O1 92.25(7) . . ? C31 Mn1 O1 91.58(7) . . ? C41 Mn1 N11 94.65(7) . . ? C51 Mn1 N11 177.10(8) . . ? C31 Mn1 N11 92.57(7) . . ? O1 Mn1 N11 84.86(6) . . ? C41 Mn1 N21 93.21(7) . . ? C51 Mn1 N21 94.31(7) . . ? C31 Mn1 N21 176.04(7) . . ? O1 Mn1 N21 84.74(6) . . ? N11 Mn1 N21 85.65(6) . . ? C12 N11 N12 106.34(14) . . ? C12 N11 Mn1 133.08(12) . . ? N12 N11 Mn1 120.57(11) . . ? C14 N12 N11 110.05(14) . . ? C14 N12 C2 132.90(15) . . ? N11 N12 C2 117.00(14) . . ? C22 N21 N22 106.10(14) . . ? C22 N21 Mn1 133.20(12) . . ? N22 N21 Mn1 119.64(11) . . ? C24 N22 N21 110.27(14) . . ? C24 N22 C2 132.91(15) . . ? N21 N22 C2 116.77(13) . . ? C1 O1 Mn1 122.51(11) . . ? #------------------------------------------------------------------------- data_gtbu12 _database_code_depnum_ccdc_archive 'CCDC 805961' _audit_creation_date 2010-11-10T14:42:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H34 Cu N8 O4' _chemical_formula_sum 'C26 H34 Cu N8 O4' _chemical_formula_weight 586.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 8.8389(10) _cell_length_b 9.665(2) _cell_length_c 15.970(2) _cell_angle_alpha 90 _cell_angle_beta 94.446(10) _cell_angle_gamma 90 _cell_volume 1360.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.902 _cell_measurement_theta_max 15.942 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 614 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.851 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.110932 _diffrn_orient_matrix_ub_12 0.003089 _diffrn_orient_matrix_ub_13 0.008266 _diffrn_orient_matrix_ub_21 0.023907 _diffrn_orient_matrix_ub_22 0.014704 _diffrn_orient_matrix_ub_23 0.06156 _diffrn_orient_matrix_ub_31 -0.000082 _diffrn_orient_matrix_ub_32 0.102399 _diffrn_orient_matrix_ub_33 -0.009112 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 0 -2 1 2 -4 -2 1 -2 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_unetI/netI 0.067 _diffrn_reflns_number 2757 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 2657 _reflns_number_gt 1824 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines(Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+0.3731P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 2657 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1387 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.779 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.076 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5276(4) 0.2746(4) 0.0531(2) 0.0328(8) Uani 1 1 d . . . C2 C 0.6947(4) 0.2695(4) 0.0221(2) 0.0331(8) Uani 1 1 d . . . C3 C 0.7623(5) 0.4139(4) 0.0357(3) 0.0469(10) Uani 1 1 d . . . H3A H 0.7018 0.4798 0.0029 0.07 Uiso 1 1 calc R . . H3B H 0.8641 0.4148 0.0186 0.07 Uiso 1 1 calc R . . H3C H 0.7636 0.4378 0.094 0.07 Uiso 1 1 calc R . . C11 C 0.5979(5) -0.0556(5) -0.2110(3) 0.0490(10) Uani 1 1 d . . . H11A H 0.6649 -0.1288 -0.1913 0.073 Uiso 1 1 calc R . . H11B H 0.6039 -0.0437 -0.2704 0.073 Uiso 1 1 calc R . . H11C H 0.4957 -0.0788 -0.2001 0.073 Uiso 1 1 calc R . . C12 C 0.6429(4) 0.0746(4) -0.1669(2) 0.0366(9) Uani 1 1 d . . . C13 C 0.7037(4) 0.1917(4) -0.2018(2) 0.0408(9) Uani 1 1 d . . . H13 H 0.722 0.2036 -0.258 0.049 Uiso 1 1 calc R . . C14 C 0.7320(4) 0.2860(4) -0.1390(2) 0.0362(8) Uani 1 1 d . . . C15 C 0.7989(6) 0.4271(4) -0.1486(3) 0.0545(11) Uani 1 1 d . . . H15A H 0.8174 0.442 -0.2064 0.082 Uiso 1 1 calc R . . H15B H 0.8928 0.4338 -0.1144 0.082 Uiso 1 1 calc R . . H15C H 0.7294 0.4959 -0.1313 0.082 Uiso 1 1 calc R . . C21 C 0.7639(5) -0.1715(4) 0.1666(3) 0.0563(12) Uani 1 1 d . . . H21A H 0.6978 -0.1543 0.2104 0.085 Uiso 1 1 calc R . . H21B H 0.853 -0.2193 0.1895 0.085 Uiso 1 1 calc R . . H21C H 0.7121 -0.2274 0.1238 0.085 Uiso 1 1 calc R . . C22 C 0.8091(4) -0.0364(4) 0.1294(2) 0.0400(9) Uani 1 1 d . . . C23 C 0.9535(4) 0.0156(4) 0.1196(3) 0.0470(10) Uani 1 1 d . . . H23 H 1.045 -0.0271 0.1367 0.056 Uiso 1 1 calc R . . C24 C 0.9363(4) 0.1404(4) 0.0803(3) 0.0424(9) Uani 1 1 d . . . C25 C 1.0573(5) 0.2319(5) 0.0513(4) 0.0678(15) Uani 1 1 d . . . H25A H 1.1544 0.1888 0.0632 0.102 Uiso 1 1 calc R . . H25B H 1.0555 0.319 0.0801 0.102 Uiso 1 1 calc R . . H25C H 1.04 0.2469 -0.0081 0.102 Uiso 1 1 calc R . . Cu1 Cu 0.5 0 0 0.0322(2) Uani 1 2 d S . . N11 N 0.6326(3) 0.0939(3) -0.08503(19) 0.0338(7) Uani 1 1 d . . . N12 N 0.6862(3) 0.2261(3) -0.06768(18) 0.0331(7) Uani 1 1 d . . . N21 N 0.7047(3) 0.0532(3) 0.09976(19) 0.0362(7) Uani 1 1 d . . . N22 N 0.7830(3) 0.1639(3) 0.07092(18) 0.0325(7) Uani 1 1 d . . . O1 O 0.4314(3) 0.1849(3) 0.02429(16) 0.0391(6) Uani 1 1 d . . . O2 O 0.5020(3) 0.3681(3) 0.1009(2) 0.0570(8) Uani 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 C1 0.035(2) 0.0278(18) 0.035(2) 0.0009(16) 0.0019(16) 0.0033(15) C2 0.0331(19) 0.0308(18) 0.035(2) 0.0010(15) 0.0030(15) -0.0044(15) C3 0.051(2) 0.037(2) 0.053(3) -0.0043(19) 0.003(2) -0.0097(19) C11 0.057(3) 0.049(2) 0.042(2) -0.009(2) 0.009(2) -0.006(2) C12 0.0309(19) 0.040(2) 0.039(2) -0.0045(17) 0.0033(16) 0.0021(16) C13 0.046(2) 0.042(2) 0.035(2) 0.0025(17) 0.0076(17) 0.0026(18) C14 0.035(2) 0.035(2) 0.038(2) 0.0058(16) 0.0026(16) 0.0029(16) C15 0.071(3) 0.041(2) 0.052(3) 0.009(2) 0.009(2) -0.006(2) C21 0.063(3) 0.040(2) 0.065(3) 0.013(2) 0.000(2) -0.002(2) C22 0.040(2) 0.040(2) 0.040(2) 0.0024(16) -0.0021(17) 0.0023(17) C23 0.0329(19) 0.048(2) 0.059(3) -0.001(2) -0.0038(17) 0.0079(19) C24 0.030(2) 0.046(2) 0.050(2) -0.0063(19) -0.0015(17) -0.0011(17) C25 0.034(2) 0.058(3) 0.113(4) 0.001(3) 0.015(3) -0.009(2) Cu1 0.0265(3) 0.0317(3) 0.0389(4) -0.0033(3) 0.0065(2) -0.0033(3) N11 0.0308(16) 0.0347(16) 0.0359(17) -0.0029(13) 0.0031(13) -0.0046(13) N12 0.0307(16) 0.0341(16) 0.0346(16) 0.0005(13) 0.0031(13) -0.0057(13) N21 0.0324(16) 0.0368(16) 0.0392(18) 0.0054(14) 0.0008(13) -0.0048(14) N22 0.0279(15) 0.0330(16) 0.0363(17) -0.0009(13) 0.0017(12) -0.0050(13) O1 0.0293(14) 0.0358(14) 0.0525(16) -0.0065(13) 0.0047(12) 0.0012(12) O2 0.0542(19) 0.0476(18) 0.070(2) -0.0234(15) 0.0128(16) 0.0013(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.216(4) . ? C1 O1 1.275(4) . ? C1 C2 1.594(5) . ? C2 N22 1.471(5) . ? C2 N12 1.489(4) . ? C2 C3 1.527(5) . ? C11 C12 1.481(5) . ? C12 N11 1.332(5) . ? C12 C13 1.388(5) . ? C13 C14 1.365(5) . ? C14 N12 1.367(4) . ? C14 C15 1.499(5) . ? C21 C22 1.503(5) . ? C22 N21 1.326(5) . ? C22 C23 1.391(6) . ? C23 C24 1.362(6) . ? C24 N22 1.371(5) . ? C24 C25 1.489(6) . ? Cu1 O1 1.936(2) . ? Cu1 O1 1.936(2) 3_655 ? Cu1 N11 2.071(3) . ? Cu1 N11 2.071(3) 3_655 ? Cu1 N21 2.372(3) . ? Cu1 N21 2.372(3) 3_655 ? N11 N12 1.383(4) . ? N21 N22 1.373(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 O2 C1 O1 125.5(4) . . ? O2 C1 C2 116.2(3) . . ? O1 C1 C2 118.3(3) . . ? N22 C2 N12 107.5(3) . . ? N22 C2 C3 111.9(3) . . ? N12 C2 C3 112.6(3) . . ? N22 C2 C1 108.8(3) . . ? N12 C2 C1 109.3(3) . . ? C3 C2 C1 106.8(3) . . ? N11 C12 C13 109.8(3) . . ? N11 C12 C11 123.4(3) . . ? C13 C12 C11 126.9(3) . . ? C14 C13 C12 107.7(3) . . ? C13 C14 N12 106.3(3) . . ? C13 C14 C15 125.7(4) . . ? N12 C14 C15 128.0(4) . . ? N21 C22 C23 110.1(3) . . ? N21 C22 C21 120.7(4) . . ? C23 C22 C21 129.2(4) . . ? C24 C23 C22 107.5(3) . . ? C23 C24 N22 105.7(3) . . ? C23 C24 C25 127.7(4) . . ? N22 C24 C25 126.5(4) . . ? O1 Cu1 O1 180.00(19) . 3_655 ? O1 Cu1 N11 85.90(11) . . ? O1 Cu1 N11 94.10(11) 3_655 . ? O1 Cu1 N11 94.10(11) . 3_655 ? O1 Cu1 N11 85.90(11) 3_655 3_655 ? N11 Cu1 N11 180.0(2) . 3_655 ? O1 Cu1 N21 84.24(11) . . ? O1 Cu1 N21 95.76(11) 3_655 . ? N11 Cu1 N21 84.52(11) . . ? N11 Cu1 N21 95.48(11) 3_655 . ? O1 Cu1 N21 95.76(11) . 3_655 ? O1 Cu1 N21 84.24(11) 3_655 3_655 ? N11 Cu1 N21 95.48(11) . 3_655 ? N11 Cu1 N21 84.52(11) 3_655 3_655 ? N21 Cu1 N21 180.00(12) . 3_655 ? C12 N11 N12 106.2(3) . . ? C12 N11 Cu1 131.9(2) . . ? N12 N11 Cu1 118.4(2) . . ? C14 N12 N11 110.1(3) . . ? C14 N12 C2 133.4(3) . . ? N11 N12 C2 116.3(3) . . ? C22 N21 N22 105.9(3) . . ? C22 N21 Cu1 124.9(3) . . ? N22 N21 Cu1 108.8(2) . . ? C24 N22 N21 110.7(3) . . ? C24 N22 C2 130.7(3) . . ? N21 N22 C2 117.2(3) . . ? C1 O1 Cu1 119.3(2) . . ? #------------------------------------------------------------------------- data_gtbu08 _database_code_depnum_ccdc_archive 'CCDC 805962' _audit_creation_date 2010-11-10T18:17:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H32 Cl N6 O2 P Ru, C H2 Cl2' _chemical_formula_sum 'C32 H34 Cl3 N6 O2 P Ru' _chemical_formula_weight 773.04 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8965(8) _cell_length_b 11.6847(5) _cell_length_c 15.3070(10) _cell_angle_alpha 82.558(4) _cell_angle_beta 73.358(7) _cell_angle_gamma 76.584(5) _cell_volume 1645.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 235 _cell_measurement_theta_min 6 _cell_measurement_theta_max 20 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description collumn _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.56 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_absorpt_correction_T_min 0.804993 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 2.00 \% and 136 sec per frame ; _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_unetI/netI 0.0485 _diffrn_reflns_number 41656 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 28.5 _diffrn_reflns_theta_full 28.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 8336 _reflns_number_gt 6603 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Attempts to resolve a molecular disorder with Cl and N2 on exchanged posititions (aprox. 20% occupation) have not been successful. ; _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^)+(0.0353P)^2^+1.1907P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 8336 _refine_ls_number_parameters 406 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.081 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.849 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.09 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6281(3) 0.8660(2) 0.50846(17) 0.0217(5) Uani 1 1 d . . . C2 C 0.5268(3) 0.7850(2) 0.49813(16) 0.0187(5) Uani 1 1 d . . . C3 C 0.4804(3) 0.8310(2) 0.41123(17) 0.0247(6) Uani 1 1 d . . . H3A H 0.4262 0.9105 0.4176 0.037 Uiso 1 1 calc R . . H3B H 0.4215 0.7821 0.401 0.037 Uiso 1 1 calc R . . H3C H 0.5641 0.8295 0.3603 0.037 Uiso 1 1 calc R . . C11 C 0.8598(3) 0.4332(2) 0.5829(2) 0.0321(6) Uani 1 1 d . . . H11A H 0.8911 0.4802 0.6173 0.048 Uiso 1 1 calc R . . H11B H 0.9422 0.3898 0.5413 0.048 Uiso 1 1 calc R . . H11C H 0.8076 0.3793 0.6239 0.048 Uiso 1 1 calc R . . C12 C 0.7643(3) 0.5118(2) 0.53027(17) 0.0224(5) Uani 1 1 d . . . C13 C 0.7377(3) 0.4882(2) 0.45038(18) 0.0267(6) Uani 1 1 d . . . H13 H 0.7785 0.4203 0.4188 0.032 Uiso 1 1 calc R . . C14 C 0.6413(3) 0.5821(2) 0.42669(17) 0.0234(5) Uani 1 1 d . . . C15 C 0.5783(3) 0.5895(3) 0.3470(2) 0.0348(7) Uani 1 1 d . . . H15A H 0.6174 0.5183 0.3154 0.052 Uiso 1 1 calc R . . H15B H 0.6019 0.6557 0.3059 0.052 Uiso 1 1 calc R . . H15C H 0.4755 0.5991 0.3688 0.052 Uiso 1 1 calc R . . C21 C 0.2775(3) 0.6853(2) 0.81777(17) 0.0272(6) Uani 1 1 d . . . H21A H 0.3675 0.6404 0.8267 0.041 Uiso 1 1 calc R . . H21B H 0.2087 0.6353 0.8314 0.041 Uiso 1 1 calc R . . H21C H 0.2424 0.749 0.8575 0.041 Uiso 1 1 calc R . . C22 C 0.2993(3) 0.7337(2) 0.72100(17) 0.0195(5) Uani 1 1 d . . . C23 C 0.1916(3) 0.7763(2) 0.67634(17) 0.0204(5) Uani 1 1 d . . . H23 H 0.0932 0.7814 0.702 0.025 Uiso 1 1 calc R . . C24 C 0.2559(3) 0.8093(2) 0.58788(17) 0.0197(5) Uani 1 1 d . . . C25 C 0.1776(3) 0.8607(2) 0.51698(19) 0.0280(6) Uani 1 1 d . . . H25A H 0.1993 0.9367 0.4941 0.042 Uiso 1 1 calc R . . H25B H 0.0758 0.869 0.5437 0.042 Uiso 1 1 calc R . . H25C H 0.2077 0.8095 0.4677 0.042 Uiso 1 1 calc R . . C31 C 0.4067(3) 0.9150(2) 0.83341(17) 0.0185(5) Uani 1 1 d . . . C32 C 0.3413(3) 0.9742(2) 0.76556(17) 0.0206(5) Uani 1 1 d . . . H32 H 0.39 0.9663 0.7042 0.025 Uiso 1 1 calc R . . C33 C 0.2044(3) 1.0444(2) 0.7896(2) 0.0291(6) Uani 1 1 d . . . H33 H 0.1618 1.0843 0.7444 0.035 Uiso 1 1 calc R . . C34 C 0.1314(3) 1.0551(3) 0.8808(2) 0.0378(7) Uani 1 1 d . . . H34 H 0.0391 1.1016 0.8968 0.045 Uiso 1 1 calc R . . C35 C 0.1950(3) 0.9969(3) 0.9484(2) 0.0348(7) Uani 1 1 d . . . H35 H 0.1451 1.0045 1.0096 0.042 Uiso 1 1 calc R . . C36 C 0.3326(3) 0.9273(2) 0.92528(19) 0.0270(6) Uani 1 1 d . . . H36 H 0.3753 0.889 0.9708 0.032 Uiso 1 1 calc R . . C41 C 0.6833(3) 0.9634(2) 0.76943(16) 0.0187(5) Uani 1 1 d . . . C42 C 0.8114(3) 0.9644(2) 0.70293(18) 0.0230(5) Uani 1 1 d . . . H42 H 0.8497 0.9032 0.664 0.028 Uiso 1 1 calc R . . C43 C 0.8841(3) 1.0565(2) 0.69352(19) 0.0267(6) Uani 1 1 d . . . H43 H 0.9718 1.055 0.6498 0.032 Uiso 1 1 calc R . . C44 C 0.8262(3) 1.1494(2) 0.74880(19) 0.0273(6) Uani 1 1 d . . . H44 H 0.8747 1.2106 0.7425 0.033 Uiso 1 1 calc R . . C45 C 0.6962(3) 1.1514(2) 0.8135(2) 0.0349(7) Uani 1 1 d . . . H45 H 0.6562 1.2148 0.8502 0.042 Uiso 1 1 calc R . . C46 C 0.6247(3) 1.0597(2) 0.82418(19) 0.0306(6) Uani 1 1 d . . . H46 H 0.537 1.0619 0.868 0.037 Uiso 1 1 calc R . . C51 C 0.6435(3) 0.7621(2) 0.89505(16) 0.0206(5) Uani 1 1 d . . . C52 C 0.5636(3) 0.6821(2) 0.94974(18) 0.0264(6) Uani 1 1 d . . . H52 H 0.4853 0.6679 0.9339 0.032 Uiso 1 1 calc R . . C53 C 0.6000(4) 0.6238(3) 1.02723(19) 0.0343(7) Uani 1 1 d . . . H53 H 0.5453 0.5718 1.0636 0.041 Uiso 1 1 calc R . . C54 C 0.7170(4) 0.6429(3) 1.0504(2) 0.0439(9) Uani 1 1 d . . . H54 H 0.7407 0.6045 1.1028 0.053 Uiso 1 1 calc R . . C55 C 0.7995(4) 0.7192(3) 0.9956(3) 0.0489(9) Uani 1 1 d . . . H55 H 0.8796 0.7309 1.0108 0.059 Uiso 1 1 calc R . . C56 C 0.7631(3) 0.7790(3) 0.9176(2) 0.0346(7) Uani 1 1 d . . . H56 H 0.8191 0.8299 0.881 0.042 Uiso 1 1 calc R . . C61 C 0.0861(5) 0.5437(3) 0.1398(3) 0.0604(11) Uani 1 1 d . . . H61A H 0.0534 0.4974 0.1049 0.072 Uiso 1 1 calc R . . H61B H 0.1548 0.4907 0.1684 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.88517(7) 0.67872(6) 0.67170(5) 0.02883(15) Uani 1 1 d . . . Cl61 Cl 0.17199(9) 0.64944(7) 0.06553(6) 0.0443(2) Uani 1 1 d . . . Cl62 Cl -0.06036(9) 0.61008(9) 0.22426(6) 0.0525(2) Uani 1 1 d . . . N1 N 0.6185(3) 0.5692(2) 0.7550(2) 0.0258(6) Uani 1 1 d U . . N2 N 0.6185(5) 0.5066(5) 0.7818(3) 0.0715(13) Uani 1 1 d U . . N11 N 0.6865(2) 0.61819(18) 0.55577(14) 0.0201(4) Uani 1 1 d . . . N12 N 0.6109(2) 0.66217(17) 0.49134(14) 0.0182(4) Uani 1 1 d . . . N21 N 0.4276(2) 0.74135(17) 0.66274(13) 0.0170(4) Uani 1 1 d . . . N22 N 0.4012(2) 0.78677(17) 0.57970(13) 0.0173(4) Uani 1 1 d . . . O1 O 0.65713(19) 0.86095(15) 0.58603(12) 0.0215(4) Uani 1 1 d . . . O2 O 0.6732(2) 0.93082(19) 0.44274(13) 0.0378(5) Uani 1 1 d . . . P1 P 0.59289(7) 0.83665(5) 0.79251(4) 0.01602(13) Uani 1 1 d . . . Ru1 Ru 0.63756(2) 0.714082(17) 0.674156(13) 0.01389(6) Uani 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 C1 0.0242(14) 0.0210(12) 0.0211(12) -0.0043(10) -0.0051(11) -0.0062(10) C2 0.0195(12) 0.0199(12) 0.0178(11) -0.0032(10) -0.0050(10) -0.0050(10) C3 0.0288(15) 0.0267(13) 0.0208(12) -0.0004(11) -0.0081(11) -0.0087(11) C11 0.0338(16) 0.0217(13) 0.0365(16) -0.0048(12) -0.0084(13) 0.0032(12) C12 0.0227(13) 0.0181(12) 0.0240(13) -0.0047(10) -0.0002(10) -0.0052(10) C13 0.0271(15) 0.0223(13) 0.0293(14) -0.0132(11) 0.0010(12) -0.0064(11) C14 0.0230(14) 0.0281(13) 0.0208(12) -0.0085(11) -0.0008(10) -0.0113(11) C15 0.0379(17) 0.0400(17) 0.0311(15) -0.0184(13) -0.0100(13) -0.0074(13) C21 0.0270(15) 0.0328(15) 0.0233(13) -0.0006(11) -0.0065(11) -0.0100(12) C22 0.0187(13) 0.0182(12) 0.0232(12) -0.0066(10) -0.0057(10) -0.0035(9) C23 0.0139(12) 0.0217(12) 0.0284(13) -0.0092(10) -0.0063(10) -0.0038(9) C24 0.0183(12) 0.0170(11) 0.0263(13) -0.0066(10) -0.0093(10) -0.0018(9) C25 0.0245(14) 0.0316(14) 0.0303(14) -0.0034(12) -0.0125(12) -0.0034(11) C31 0.0185(12) 0.0157(11) 0.0221(12) -0.0047(10) -0.0042(10) -0.0043(9) C32 0.0191(13) 0.0185(12) 0.0239(13) -0.0050(10) -0.0049(10) -0.0026(10) C33 0.0218(14) 0.0237(13) 0.0411(16) -0.0055(12) -0.0105(12) 0.0015(11) C34 0.0207(15) 0.0355(16) 0.0495(19) -0.0122(14) -0.0017(13) 0.0045(12) C35 0.0300(16) 0.0371(16) 0.0288(15) -0.0118(13) 0.0066(12) -0.0028(13) C36 0.0268(14) 0.0255(13) 0.0264(13) -0.0067(11) -0.0029(11) -0.0036(11) C41 0.0224(13) 0.0169(11) 0.0195(12) -0.0014(9) -0.0104(10) -0.0031(10) C42 0.0219(13) 0.0214(12) 0.0285(13) -0.0067(11) -0.0083(11) -0.0050(10) C43 0.0238(14) 0.0293(14) 0.0303(14) -0.0009(12) -0.0081(11) -0.0114(11) C44 0.0368(16) 0.0210(13) 0.0315(14) 0.0015(11) -0.0164(13) -0.0129(12) C45 0.0447(19) 0.0240(14) 0.0390(17) -0.0142(13) -0.0071(14) -0.0114(13) C46 0.0328(16) 0.0279(14) 0.0301(14) -0.0118(12) 0.0000(12) -0.0094(12) C51 0.0257(14) 0.0188(12) 0.0180(12) -0.0044(10) -0.0088(10) -0.0003(10) C52 0.0283(15) 0.0253(13) 0.0255(13) -0.0029(11) -0.0075(11) -0.0044(11) C53 0.0486(19) 0.0266(14) 0.0243(14) 0.0015(12) -0.0095(13) -0.0033(13) C54 0.075(3) 0.0317(16) 0.0326(16) 0.0015(13) -0.0347(17) -0.0018(16) C55 0.069(2) 0.0373(18) 0.061(2) 0.0043(16) -0.051(2) -0.0124(17) C56 0.0417(18) 0.0286(15) 0.0435(17) 0.0048(13) -0.0279(15) -0.0098(13) C61 0.074(3) 0.0382(19) 0.053(2) -0.0046(17) 0.009(2) -0.0114(19) Cl1 0.0215(3) 0.0262(3) 0.0407(4) -0.0060(3) -0.0101(3) -0.0042(3) Cl61 0.0427(5) 0.0411(4) 0.0409(4) 0.0003(3) -0.0024(4) -0.0049(4) Cl62 0.0376(5) 0.0748(6) 0.0392(4) 0.0027(4) -0.0052(4) -0.0095(4) N1 0.0230(14) 0.0285(14) 0.0273(16) -0.0100(11) -0.0129(12) 0.0045(12) N2 0.043(2) 0.137(4) 0.040(2) -0.037(3) 0.0035(17) -0.030(3) N11 0.0193(11) 0.0199(10) 0.0216(10) -0.0044(9) -0.0060(9) -0.0027(8) N12 0.0187(11) 0.0176(10) 0.0189(10) -0.0044(8) -0.0041(8) -0.0044(8) N21 0.0157(10) 0.0178(10) 0.0193(10) -0.0039(8) -0.0064(8) -0.0032(8) N22 0.0163(10) 0.0171(10) 0.0202(10) -0.0042(8) -0.0055(8) -0.0042(8) O1 0.0274(10) 0.0189(8) 0.0217(9) -0.0004(7) -0.0097(8) -0.0078(7) O2 0.0518(14) 0.0438(12) 0.0285(11) 0.0065(9) -0.0146(10) -0.0310(11) P1 0.0155(3) 0.0160(3) 0.0172(3) -0.0030(2) -0.0051(2) -0.0024(2) Ru1 0.01289(10) 0.01435(9) 0.01492(9) -0.00231(7) -0.00435(7) -0.00219(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.220(3) . ? C1 O1 1.291(3) . ? C1 C2 1.580(3) . ? C2 N12 1.483(3) . ? C2 N22 1.486(3) . ? C2 C3 1.523(3) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C11 C12 1.492(4) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 N11 1.342(3) . ? C12 C13 1.395(4) . ? C13 C14 1.362(4) . ? C13 H13 0.93 . ? C14 N12 1.372(3) . ? C14 C15 1.505(4) . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C21 C22 1.489(3) . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 N21 1.341(3) . ? C22 C23 1.391(3) . ? C23 C24 1.368(4) . ? C23 H23 0.93 . ? C24 N22 1.373(3) . ? C24 C25 1.495(3) . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C31 C36 1.396(4) . ? C31 C32 1.403(3) . ? C31 P1 1.825(2) . ? C32 C33 1.385(3) . ? C32 H32 0.93 . ? C33 C34 1.383(4) . ? C33 H33 0.93 . ? C34 C35 1.387(4) . ? C34 H34 0.93 . ? C35 C36 1.388(4) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C41 C42 1.381(4) . ? C41 C46 1.402(4) . ? C41 P1 1.849(3) . ? C42 C43 1.399(4) . ? C42 H42 0.93 . ? C43 C44 1.376(4) . ? C43 H43 0.93 . ? C44 C45 1.378(4) . ? C44 H44 0.93 . ? C45 C46 1.385(4) . ? C45 H45 0.93 . ? C46 H46 0.93 . ? C51 C56 1.386(4) . ? C51 C52 1.400(4) . ? C51 P1 1.835(2) . ? C52 C53 1.387(4) . ? C52 H52 0.93 . ? C53 C54 1.375(5) . ? C53 H53 0.93 . ? C54 C55 1.385(5) . ? C54 H54 0.93 . ? C55 C56 1.398(4) . ? C55 H55 0.93 . ? C56 H56 0.93 . ? C61 Cl62 1.743(4) . ? C61 Cl61 1.764(4) . ? C61 H61A 0.97 . ? C61 H61B 0.97 . ? Cl1 Ru1 2.3787(7) . ? N1 N2 0.791(5) . ? N1 Ru1 1.976(3) . ? N11 N12 1.382(3) . ? N11 Ru1 2.132(2) . ? N21 N22 1.384(3) . ? N21 Ru1 2.082(2) . ? O1 Ru1 2.0511(17) . ? P1 Ru1 2.3341(6) . ? 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 C1 O1 123.7(2) . . ? O2 C1 C2 118.0(2) . . ? O1 C1 C2 118.4(2) . . ? N12 C2 N22 107.80(19) . . ? N12 C2 C3 111.4(2) . . ? N22 C2 C3 111.9(2) . . ? N12 C2 C1 108.02(19) . . ? N22 C2 C1 110.99(19) . . ? C3 C2 C1 106.7(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N11 C12 C13 109.1(2) . . ? N11 C12 C11 123.6(2) . . ? C13 C12 C11 127.3(2) . . ? C14 C13 C12 108.0(2) . . ? C14 C13 H13 126 . . ? C12 C13 H13 126 . . ? C13 C14 N12 106.4(2) . . ? C13 C14 C15 124.9(2) . . ? N12 C14 C15 128.6(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N21 C22 C23 109.3(2) . . ? N21 C22 C21 124.8(2) . . ? C23 C22 C21 125.9(2) . . ? C24 C23 C22 107.9(2) . . ? C24 C23 H23 126.1 . . ? C22 C23 H23 126.1 . . ? C23 C24 N22 106.5(2) . . ? C23 C24 C25 124.9(2) . . ? N22 C24 C25 128.6(2) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C36 C31 C32 119.4(2) . . ? C36 C31 P1 124.7(2) . . ? C32 C31 P1 115.64(18) . . ? C33 C32 C31 120.3(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 119.9(3) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.3(3) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 120.3(3) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 119.8(3) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C42 C41 C46 118.4(2) . . ? C42 C41 P1 122.26(18) . . ? C46 C41 P1 119.2(2) . . ? C41 C42 C43 120.6(2) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C44 C43 C42 120.2(3) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.7(3) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C44 C45 C46 120.4(3) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C41 120.6(3) . . ? C45 C46 H46 119.7 . . ? C41 C46 H46 119.7 . . ? C56 C51 C52 118.9(2) . . ? C56 C51 P1 121.5(2) . . ? C52 C51 P1 119.5(2) . . ? C53 C52 C51 120.7(3) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C54 C53 C52 120.0(3) . . ? C54 C53 H53 120 . . ? C52 C53 H53 120 . . ? C53 C54 C55 119.9(3) . . ? C53 C54 H54 120 . . ? C55 C54 H54 120 . . ? C54 C55 C56 120.4(3) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C51 C56 C55 119.9(3) . . ? C51 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? Cl62 C61 Cl61 111.5(2) . . ? Cl62 C61 H61A 109.3 . . ? Cl61 C61 H61A 109.3 . . ? Cl62 C61 H61B 109.3 . . ? Cl61 C61 H61B 109.3 . . ? H61A C61 H61B 108 . . ? N2 N1 Ru1 172.3(5) . . ? C12 N11 N12 106.4(2) . . ? C12 N11 Ru1 135.13(18) . . ? N12 N11 Ru1 117.83(14) . . ? C14 N12 N11 110.0(2) . . ? C14 N12 C2 132.2(2) . . ? N11 N12 C2 117.51(18) . . ? C22 N21 N22 106.56(19) . . ? C22 N21 Ru1 135.00(17) . . ? N22 N21 Ru1 118.22(15) . . ? C24 N22 N21 109.75(19) . . ? C24 N22 C2 131.4(2) . . ? N21 N22 C2 117.97(19) . . ? C1 O1 Ru1 119.56(15) . . ? C31 P1 C51 105.26(12) . . ? C31 P1 C41 99.08(11) . . ? C51 P1 C41 102.13(11) . . ? C31 P1 Ru1 115.74(8) . . ? C51 P1 Ru1 114.53(8) . . ? C41 P1 Ru1 117.95(8) . . ? N1 Ru1 O1 177.73(10) . . ? N1 Ru1 N21 92.78(11) . . ? O1 Ru1 N21 86.44(7) . . ? N1 Ru1 N11 91.24(11) . . ? O1 Ru1 N11 86.55(7) . . ? N21 Ru1 N11 83.08(8) . . ? N1 Ru1 P1 95.11(9) . . ? O1 Ru1 P1 87.12(5) . . ? N21 Ru1 P1 98.02(6) . . ? N11 Ru1 P1 173.49(6) . . ? N1 Ru1 Cl1 89.28(9) . . ? O1 Ru1 Cl1 91.31(5) . . ? N21 Ru1 Cl1 174.33(6) . . ? N11 Ru1 Cl1 91.59(6) . . ? P1 Ru1 Cl1 87.05(2) . . ? #------------------------------------------------------------------------- data_gtbu17 _database_code_depnum_ccdc_archive 'CCDC 805963' _audit_creation_date 2010-11-10T21:02:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H32 Cl1 N4 O3 P Ru, C H2 Cl2' _chemical_formula_sum 'C33 H34 Cl3 N4 O3 P Ru' _chemical_formula_weight 773.03 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0431(5) _cell_length_b 11.6105(5) _cell_length_c 15.3823(10) _cell_angle_alpha 82.767(4) _cell_angle_beta 73.575(5) _cell_angle_gamma 76.413(4) _cell_volume 1668.91(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 121 _cell_measurement_theta_min 6 _cell_measurement_theta_max 20 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_absorpt_correction_T_min 0.805693 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 2.00 \% and 90 sec per frame ; _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_unetI/netI 0.0289 _diffrn_reflns_number 56113 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 28.5 _diffrn_reflns_theta_full 28.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 8458 _reflns_number_gt 7312 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Attempts to resolve a molecular disorder with Cl and SO2 on exchanged posititions (aprox. 20% occupation) have not been successful. ; _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^)+(0.0350P)^2^+0.7845P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 8458 _refine_ls_number_parameters 434 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.54 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6243(2) 0.86596(15) 0.51043(12) 0.0162(3) Uani 1 1 d . . . C2 C 0.52585(19) 0.78330(15) 0.49878(12) 0.0153(3) Uani 1 1 d . . . C3 C 0.4814(2) 0.82757(17) 0.41196(13) 0.0206(4) Uani 1 1 d . . . H3A H 0.5644 0.8247 0.3617 0.031 Uiso 1 1 calc R . . H3B H 0.4283 0.9079 0.4173 0.031 Uiso 1 1 calc R . . H3C H 0.4235 0.7781 0.402 0.031 Uiso 1 1 calc R . . C11 C 0.2707(2) 0.69137(19) 0.81551(13) 0.0235(4) Uani 1 1 d . . . H11A H 0.36 0.6618 0.8301 0.035 Uiso 1 1 calc R . . H11B H 0.2202 0.6283 0.8249 0.035 Uiso 1 1 calc R . . H11C H 0.2154 0.7541 0.854 0.035 Uiso 1 1 calc R . . C12 C 0.2964(2) 0.73798(16) 0.71838(12) 0.0168(4) Uani 1 1 d . . . C13 C 0.1912(2) 0.78447(17) 0.67314(13) 0.0192(4) Uani 1 1 d . . . H13 H 0.0938 0.7939 0.6982 0.023 Uiso 1 1 calc R . . C14 C 0.2574(2) 0.81368(16) 0.58521(13) 0.0179(4) Uani 1 1 d . . . C15 C 0.1808(2) 0.86686(19) 0.51399(14) 0.0252(4) Uani 1 1 d . . . H15A H 0.2061 0.9415 0.4898 0.038 Uiso 1 1 calc R . . H15B H 0.0802 0.8793 0.5406 0.038 Uiso 1 1 calc R . . H15C H 0.2072 0.8138 0.466 0.038 Uiso 1 1 calc R . . C21 C 0.8627(2) 0.43418(18) 0.58388(15) 0.0287(5) Uani 1 1 d . . . H21A H 0.9197 0.481 0.5983 0.043 Uiso 1 1 calc R . . H21B H 0.9232 0.3711 0.5474 0.043 Uiso 1 1 calc R . . H21C H 0.8079 0.4011 0.639 0.043 Uiso 1 1 calc R . . C22 C 0.7647(2) 0.51105(16) 0.53225(13) 0.0194(4) Uani 1 1 d . . . C23 C 0.7412(2) 0.48503(17) 0.45209(14) 0.0232(4) Uani 1 1 d . . . H23 H 0.7842 0.4167 0.4208 0.028 Uiso 1 1 calc R . . C24 C 0.6432(2) 0.57840(17) 0.42801(13) 0.0195(4) Uani 1 1 d . . . C25 C 0.5834(2) 0.5830(2) 0.34848(14) 0.0281(5) Uani 1 1 d . . . H25A H 0.6212 0.5097 0.319 0.042 Uiso 1 1 calc R . . H25B H 0.6089 0.6476 0.3063 0.042 Uiso 1 1 calc R . . H25C H 0.4819 0.5947 0.3691 0.042 Uiso 1 1 calc R . . C31 C 0.6780(2) 0.96229(16) 0.77133(12) 0.0165(3) Uani 1 1 d . . . C32 C 0.8066(2) 0.96002(17) 0.70588(13) 0.0194(4) Uani 1 1 d . . . H32 H 0.8441 0.897 0.6683 0.023 Uiso 1 1 calc R . . C33 C 0.8799(2) 1.05126(18) 0.69588(14) 0.0232(4) Uani 1 1 d . . . H33 H 0.9669 1.0476 0.6529 0.028 Uiso 1 1 calc R . . C34 C 0.8236(2) 1.14712(18) 0.74973(14) 0.0257(4) Uani 1 1 d . . . H34 H 0.8727 1.2076 0.7432 0.031 Uiso 1 1 calc R . . C35 C 0.6935(3) 1.15256(19) 0.81336(16) 0.0320(5) Uani 1 1 d . . . H35 H 0.6543 1.2179 0.8485 0.038 Uiso 1 1 calc R . . C36 C 0.6212(2) 1.06055(19) 0.82490(15) 0.0270(4) Uani 1 1 d . . . H36 H 0.5347 1.0643 0.8684 0.032 Uiso 1 1 calc R . . C41 C 0.6343(2) 0.76372(16) 0.89828(12) 0.0179(4) Uani 1 1 d . . . C42 C 0.5557(2) 0.68336(17) 0.95234(13) 0.0227(4) Uani 1 1 d . . . H42 H 0.4788 0.6691 0.9362 0.027 Uiso 1 1 calc R . . C43 C 0.5914(3) 0.62482(19) 1.02965(14) 0.0298(5) Uani 1 1 d . . . H43 H 0.5377 0.5724 1.0654 0.036 Uiso 1 1 calc R . . C44 C 0.7067(3) 0.6445(2) 1.05340(16) 0.0364(6) Uani 1 1 d . . . H44 H 0.73 0.6058 1.1055 0.044 Uiso 1 1 calc R . . C45 C 0.7876(3) 0.7214(2) 0.99989(18) 0.0391(6) Uani 1 1 d . . . H45 H 0.8662 0.7332 1.0154 0.047 Uiso 1 1 calc R . . C46 C 0.7513(2) 0.78128(19) 0.92253(15) 0.0286(5) Uani 1 1 d . . . H46 H 0.8056 0.8333 0.8869 0.034 Uiso 1 1 calc R . . C51 C 0.4033(2) 0.91691(16) 0.83274(12) 0.0168(4) Uani 1 1 d . . . C52 C 0.3415(2) 0.97675(16) 0.76382(13) 0.0186(4) Uani 1 1 d . . . H52 H 0.3921 0.9699 0.7032 0.022 Uiso 1 1 calc R . . C53 C 0.2056(2) 1.04583(18) 0.78578(15) 0.0253(4) Uani 1 1 d . . . H53 H 0.1652 1.0856 0.74 0.03 Uiso 1 1 calc R . . C54 C 0.1292(2) 1.0560(2) 0.87602(16) 0.0314(5) Uani 1 1 d . . . H54 H 0.0374 1.1016 0.8906 0.038 Uiso 1 1 calc R . . C55 C 0.1898(2) 0.9980(2) 0.94450(15) 0.0297(5) Uani 1 1 d . . . H55 H 0.1385 1.0055 1.0049 0.036 Uiso 1 1 calc R . . C56 C 0.3266(2) 0.92895(18) 0.92356(13) 0.0223(4) Uani 1 1 d . . . H56 H 0.3669 0.8909 0.9698 0.027 Uiso 1 1 calc R . . C61 C 0.0974(3) 0.5515(2) 0.13289(18) 0.0403(6) Uani 1 1 d . . . H61A H 0.1696 0.5069 0.1619 0.048 Uiso 1 1 calc R . . H61B H 0.0723 0.4966 0.1007 0.048 Uiso 1 1 calc R . . O4 O 0.9356(5) 0.6573(3) 0.6882(3) 0.0341(7) Uani 0.840(9) 1 d PU A 1 C4 C 0.8214(6) 0.6819(3) 0.6827(3) 0.0209(8) Uani 0.840(9) 1 d PU A 1 Cl1 Cl 0.60826(9) 0.53375(10) 0.77068(6) 0.0210(5) Uani 0.840(9) 1 d P A 1 O5 O 0.6215(17) 0.489(2) 0.7937(15) 0.032(3) Uani 0.160(9) 1 d P A 2 C5 C 0.6222(18) 0.589(3) 0.7465(16) 0.027(4) Uani 0.160(9) 1 d P A 2 Cl2 Cl 0.8814(6) 0.6774(4) 0.6716(4) 0.018(2) Uani 0.160(9) 1 d P A 2 Cl3 Cl 0.16668(7) 0.66086(6) 0.05497(4) 0.04344(15) Uani 1 1 d . . . Cl4 Cl -0.05422(7) 0.61489(6) 0.21679(5) 0.04540(16) Uani 1 1 d . . . N11 N 0.42451(16) 0.74020(13) 0.66141(10) 0.0146(3) Uani 1 1 d . A . N12 N 0.40039(16) 0.78620(13) 0.57839(10) 0.0151(3) Uani 1 1 d . . . N21 N 0.68478(16) 0.61705(13) 0.55723(10) 0.0161(3) Uani 1 1 d . A . N22 N 0.61038(16) 0.65973(13) 0.49279(10) 0.0154(3) Uani 1 1 d . . . O1 O 0.65234(14) 0.86135(11) 0.58747(8) 0.0168(3) Uani 1 1 d . A . O2 O 0.66716(17) 0.93158(13) 0.44511(9) 0.0263(3) Uani 1 1 d . . . P1 P 0.58691(5) 0.83656(4) 0.79526(3) 0.01377(9) Uani 1 1 d . A . Ru1 Ru 0.636403(15) 0.712675(12) 0.676421(9) 0.01194(5) Uani 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 C1 0.0200(9) 0.0113(8) 0.0178(9) -0.0027(6) -0.0048(7) -0.0036(7) C2 0.0188(9) 0.0137(8) 0.0141(8) -0.0018(6) -0.0039(7) -0.0047(7) C3 0.0282(10) 0.0201(9) 0.0165(9) -0.0010(7) -0.0094(8) -0.0068(8) C11 0.0221(10) 0.0299(10) 0.0190(9) -0.0001(8) -0.0021(8) -0.0112(8) C12 0.0173(9) 0.0155(8) 0.0184(9) -0.0043(7) -0.0026(7) -0.0058(7) C13 0.0151(9) 0.0193(9) 0.0251(10) -0.0061(7) -0.0052(7) -0.0047(7) C14 0.0186(9) 0.0140(8) 0.0239(9) -0.0056(7) -0.0095(7) -0.0018(7) C15 0.0240(10) 0.0271(10) 0.0280(11) -0.0026(8) -0.0138(9) -0.0033(8) C21 0.0300(12) 0.0191(10) 0.0318(12) -0.0040(8) -0.0072(9) 0.0052(8) C22 0.0195(9) 0.0148(8) 0.0214(9) -0.0029(7) -0.0002(7) -0.0041(7) C23 0.0270(11) 0.0168(9) 0.0239(10) -0.0093(7) -0.0002(8) -0.0042(8) C24 0.0223(10) 0.0193(9) 0.0178(9) -0.0074(7) -0.0006(7) -0.0082(7) C25 0.0353(12) 0.0289(11) 0.0244(10) -0.0132(8) -0.0092(9) -0.0073(9) C31 0.0200(9) 0.0155(8) 0.0161(9) 0.0000(7) -0.0074(7) -0.0048(7) C32 0.0192(9) 0.0188(9) 0.0208(9) -0.0031(7) -0.0055(7) -0.0039(7) C33 0.0222(10) 0.0248(10) 0.0252(10) 0.0002(8) -0.0074(8) -0.0096(8) C34 0.0332(12) 0.0211(10) 0.0294(11) 0.0006(8) -0.0129(9) -0.0137(8) C35 0.0387(13) 0.0226(11) 0.0365(12) -0.0126(9) -0.0044(10) -0.0105(9) C36 0.0264(11) 0.0248(10) 0.0291(11) -0.0104(8) 0.0010(9) -0.0094(8) C41 0.0223(10) 0.0165(9) 0.0150(9) -0.0025(7) -0.0064(7) -0.0019(7) C42 0.0266(10) 0.0216(10) 0.0187(9) -0.0014(7) -0.0048(8) -0.0043(8) C43 0.0431(13) 0.0230(10) 0.0194(10) 0.0006(8) -0.0055(9) -0.0038(9) C44 0.0605(17) 0.0267(11) 0.0259(11) 0.0032(9) -0.0255(11) -0.0017(11) C45 0.0532(16) 0.0325(12) 0.0462(15) 0.0026(10) -0.0380(13) -0.0094(11) C46 0.0354(12) 0.0255(11) 0.0322(12) 0.0037(9) -0.0197(10) -0.0103(9) C51 0.0172(9) 0.0147(8) 0.0181(9) -0.0034(7) -0.0031(7) -0.0034(7) C52 0.0199(9) 0.0155(9) 0.0207(9) -0.0026(7) -0.0050(7) -0.0037(7) C53 0.0217(10) 0.0201(10) 0.0343(12) -0.0005(8) -0.0112(9) -0.0009(8) C54 0.0192(10) 0.0274(11) 0.0403(13) -0.0066(9) -0.0001(9) 0.0023(8) C55 0.0248(11) 0.0308(11) 0.0261(11) -0.0096(9) 0.0061(9) -0.0031(9) C56 0.0243(10) 0.0230(10) 0.0185(9) -0.0045(7) -0.0029(8) -0.0043(8) C61 0.0396(14) 0.0334(13) 0.0425(14) 0.0000(11) -0.0089(11) -0.0006(10) O4 0.0199(15) 0.0226(12) 0.0626(18) -0.0076(11) -0.0132(15) -0.0042(10) C4 0.023(2) 0.0138(12) 0.0258(16) -0.0035(10) -0.0049(17) -0.0032(17) Cl1 0.0255(4) 0.0179(10) 0.0205(5) 0.0013(5) -0.0075(3) -0.0061(4) O5 0.040(7) 0.015(7) 0.036(8) 0.002(6) -0.010(6) 0.000(6) C5 0.025(8) 0.018(9) 0.041(9) -0.003(8) -0.011(7) -0.003(7) Cl2 0.011(5) 0.0179(19) 0.027(2) -0.0047(13) -0.010(2) 0.002(2) Cl3 0.0383(3) 0.0426(3) 0.0394(3) 0.0004(3) -0.0003(3) -0.0026(3) Cl4 0.0343(3) 0.0539(4) 0.0399(3) 0.0048(3) -0.0042(3) -0.0044(3) N11 0.0166(8) 0.0144(7) 0.0135(7) -0.0011(5) -0.0047(6) -0.0036(6) N12 0.0172(8) 0.0154(7) 0.0141(7) -0.0013(6) -0.0060(6) -0.0039(6) N21 0.0180(8) 0.0144(7) 0.0159(7) -0.0024(6) -0.0038(6) -0.0035(6) N22 0.0193(8) 0.0142(7) 0.0135(7) -0.0034(6) -0.0037(6) -0.0045(6) O1 0.0238(7) 0.0142(6) 0.0145(6) -0.0002(5) -0.0063(5) -0.0072(5) O2 0.0403(9) 0.0271(8) 0.0178(7) 0.0047(6) -0.0097(6) -0.0200(7) P1 0.0149(2) 0.0138(2) 0.0133(2) -0.00169(16) -0.00425(17) -0.00328(17) Ru1 0.01222(7) 0.01108(7) 0.01286(7) -0.00141(5) -0.00323(5) -0.00285(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.221(2) . ? C1 O1 1.285(2) . ? C1 C2 1.588(2) . ? C2 N22 1.485(2) . ? C2 N12 1.485(2) . ? C2 C3 1.518(3) . ? C11 C12 1.495(3) . ? C12 N11 1.341(2) . ? C12 C13 1.394(3) . ? C13 C14 1.367(3) . ? C14 N12 1.372(2) . ? C14 C15 1.502(3) . ? C21 C22 1.499(3) . ? C22 N21 1.337(2) . ? C22 C23 1.400(3) . ? C23 C24 1.373(3) . ? C24 N22 1.378(2) . ? C24 C25 1.498(3) . ? C31 C32 1.391(3) . ? C31 C36 1.404(3) . ? C31 P1 1.8456(19) . ? C32 C33 1.397(3) . ? C33 C34 1.384(3) . ? C34 C35 1.386(3) . ? C35 C36 1.394(3) . ? C41 C46 1.393(3) . ? C41 C42 1.402(3) . ? C41 P1 1.8311(19) . ? C42 C43 1.388(3) . ? C43 C44 1.383(4) . ? C44 C45 1.382(4) . ? C45 C46 1.397(3) . ? C51 C56 1.398(3) . ? C51 C52 1.406(3) . ? C51 P1 1.8243(19) . ? C52 C53 1.384(3) . ? C53 C54 1.388(3) . ? C54 C55 1.387(3) . ? C55 C56 1.390(3) . ? C61 Cl3 1.759(3) . ? C61 Cl4 1.769(3) . ? O4 C4 1.139(10) . ? C4 Ru1 1.836(6) . ? Cl1 Ru1 2.4049(12) . ? O5 C5 1.29(5) . ? C5 Ru1 1.69(3) . ? Cl2 Ru1 2.379(5) . ? N11 N12 1.385(2) . ? N11 Ru1 2.1503(15) . ? N21 N22 1.381(2) . ? N21 Ru1 2.1413(15) . ? O1 Ru1 2.0710(12) . ? P1 Ru1 2.3388(5) . ? 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 C1 O1 124.13(17) . . ? O2 C1 C2 117.23(16) . . ? O1 C1 C2 118.64(15) . . ? N22 C2 N12 108.35(14) . . ? N22 C2 C3 111.18(14) . . ? N12 C2 C3 111.24(15) . . ? N22 C2 C1 107.84(14) . . ? N12 C2 C1 110.95(14) . . ? C3 C2 C1 107.25(14) . . ? N11 C12 C13 109.77(17) . . ? N11 C12 C11 124.95(17) . . ? C13 C12 C11 125.29(17) . . ? C14 C13 C12 107.51(17) . . ? C13 C14 N12 106.55(16) . . ? C13 C14 C15 124.08(18) . . ? N12 C14 C15 129.36(18) . . ? N21 C22 C23 109.30(17) . . ? N21 C22 C21 124.12(18) . . ? C23 C22 C21 126.58(18) . . ? C24 C23 C22 107.72(17) . . ? C23 C24 N22 106.16(17) . . ? C23 C24 C25 124.70(17) . . ? N22 C24 C25 129.09(18) . . ? C32 C31 C36 118.46(17) . . ? C32 C31 P1 122.29(14) . . ? C36 C31 P1 119.11(15) . . ? C31 C32 C33 120.80(18) . . ? C34 C33 C32 120.19(19) . . ? C33 C34 C35 119.73(19) . . ? C34 C35 C36 120.3(2) . . ? C35 C36 C31 120.5(2) . . ? C46 C41 C42 118.52(18) . . ? C46 C41 P1 121.82(15) . . ? C42 C41 P1 119.59(15) . . ? C43 C42 C41 120.8(2) . . ? C44 C43 C42 119.9(2) . . ? C45 C44 C43 120.2(2) . . ? C44 C45 C46 120.0(2) . . ? C41 C46 C45 120.5(2) . . ? C56 C51 C52 119.30(18) . . ? C56 C51 P1 124.58(15) . . ? C52 C51 P1 115.95(14) . . ? C53 C52 C51 120.24(18) . . ? C52 C53 C54 120.1(2) . . ? C55 C54 C53 120.0(2) . . ? C54 C55 C56 120.5(2) . . ? C55 C56 C51 119.77(19) . . ? Cl3 C61 Cl4 111.48(14) . . ? O4 C4 Ru1 176.6(4) . . ? O5 C5 Ru1 174.2(16) . . ? C12 N11 N12 106.05(15) . . ? C12 N11 Ru1 134.97(13) . . ? N12 N11 Ru1 118.33(11) . . ? C14 N12 N11 110.10(15) . . ? C14 N12 C2 131.77(15) . . ? N11 N12 C2 117.60(14) . . ? C22 N21 N22 106.80(15) . . ? C22 N21 Ru1 133.76(13) . . ? N22 N21 Ru1 118.94(11) . . ? C24 N22 N21 110.01(15) . . ? C24 N22 C2 132.06(16) . . ? N21 N22 C2 117.55(14) . . ? C1 O1 Ru1 120.36(11) . . ? C51 P1 C41 105.74(9) . . ? C51 P1 C31 99.67(8) . . ? C41 P1 C31 102.13(8) . . ? C51 P1 Ru1 115.92(6) . . ? C41 P1 Ru1 115.14(6) . . ? C31 P1 Ru1 116.18(6) . . ? C5 Ru1 C4 85.7(5) . . ? C5 Ru1 O1 178.2(5) . . ? C4 Ru1 O1 95.18(13) . . ? C5 Ru1 N21 92.8(5) . . ? C4 Ru1 N21 94.17(13) . . ? O1 Ru1 N21 85.51(5) . . ? C5 Ru1 N11 94.0(5) . . ? C4 Ru1 N11 175.94(13) . . ? O1 Ru1 N11 85.06(5) . . ? N21 Ru1 N11 81.81(6) . . ? C5 Ru1 P1 93.8(5) . . ? C4 Ru1 P1 86.09(12) . . ? O1 Ru1 P1 87.88(4) . . ? N21 Ru1 P1 173.39(4) . . ? N11 Ru1 P1 97.97(4) . . ? C5 Ru1 Cl2 89.2(5) . . ? C4 Ru1 Cl2 4.7(2) . . ? O1 Ru1 Cl2 91.52(14) . . ? N21 Ru1 Cl2 90.95(13) . . ? N11 Ru1 Cl2 172.20(14) . . ? P1 Ru1 Cl2 88.90(12) . . ? C5 Ru1 Cl1 3.4(5) . . ? C4 Ru1 Cl1 88.22(12) . . ? O1 Ru1 Cl1 174.81(4) . . ? N21 Ru1 Cl1 90.33(4) . . ? N11 Ru1 Cl1 91.27(4) . . ? P1 Ru1 Cl1 96.28(2) . . ? Cl2 Ru1 Cl1 91.66(13) . . ? #------------------------------------------------------------------------- data_gtbu16 _database_code_depnum_ccdc_archive 'CCDC 805964' _audit_creation_date 2010-11-16T19:59:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H30 Cl N4 O4 P Ru S, C H Cl3' _chemical_formula_sum 'C31 H31 Cl4 N4 O4 P Ru S' _chemical_formula_weight 829.5 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2222(9) _cell_length_b 11.7705(10) _cell_length_c 15.5181(13) _cell_angle_alpha 81.2780(10) _cell_angle_beta 71.1540(10) _cell_angle_gamma 77.0780(10) _cell_volume 1715.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4450 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.01 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_absorpt_correction_T_min 0.6589 _exptl_absorpt_correction_T_max 0.7455 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_unetI/netI 0.0479 _diffrn_reflns_number 19961 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.13 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 7394 _reflns_number_gt 5633 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A molecular disorder disorder with Cl and CO exchanging posititions (15% occupation) has been resolved. ; _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^)+(0.0826P)^2^+2.1188P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 7394 _refine_ls_number_parameters 433 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.139 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.21 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.111 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5227(5) 0.7920(4) 0.5081(3) 0.0387(11) Uani 1 1 d . . . H1 H 0.4893 0.8191 0.4547 0.046 Uiso 1 1 calc R . . C2 C 0.6181(5) 0.8750(4) 0.5125(3) 0.0387(11) Uani 1 1 d . . . C11 C 0.2613(6) 0.6931(5) 0.8253(4) 0.0493(13) Uani 1 1 d . . . H11A H 0.3474 0.6548 0.8377 0.074 Uiso 1 1 calc R . . H11B H 0.1983 0.6388 0.8396 0.074 Uiso 1 1 calc R . . H11C H 0.2185 0.758 0.8621 0.074 Uiso 1 1 calc R . . C12 C 0.2914(5) 0.7358(4) 0.7279(3) 0.0368(10) Uani 1 1 d . . . C13 C 0.1926(5) 0.7725(4) 0.6796(4) 0.0405(11) Uani 1 1 d . . . H13 H 0.0961 0.7748 0.7029 0.049 Uiso 1 1 calc R . . C14 C 0.2646(5) 0.8044(4) 0.5919(3) 0.0388(11) Uani 1 1 d . . . C15 C 0.2143(7) 0.8491(5) 0.5104(4) 0.0552(15) Uani 1 1 d . . . H15A H 0.2334 0.9265 0.4896 0.083 Uiso 1 1 calc R . . H15B H 0.1149 0.8512 0.5268 0.083 Uiso 1 1 calc R . . H15C H 0.2624 0.7982 0.4624 0.083 Uiso 1 1 calc R . . C21 C 0.8310(7) 0.4357(5) 0.5792(5) 0.0604(16) Uani 1 1 d . . . H21A H 0.9058 0.4705 0.582 0.091 Uiso 1 1 calc R . . H21B H 0.8702 0.3656 0.5481 0.091 Uiso 1 1 calc R . . H21C H 0.7737 0.4168 0.6401 0.091 Uiso 1 1 calc R . . C22 C 0.7440(6) 0.5189(4) 0.5290(3) 0.0433(12) Uani 1 1 d . . . C23 C 0.7252(6) 0.5068(5) 0.4459(4) 0.0526(14) Uani 1 1 d . . . H23 H 0.7655 0.4432 0.4109 0.063 Uiso 1 1 calc R . . C24 C 0.6363(6) 0.6056(5) 0.4252(3) 0.0494(13) Uani 1 1 d . . . C25 C 0.5776(8) 0.6417(6) 0.3467(4) 0.0671(18) Uani 1 1 d . . . H25A H 0.4783 0.671 0.3692 0.101 Uiso 1 1 calc R . . H25B H 0.5937 0.5755 0.3128 0.101 Uiso 1 1 calc R . . H25C H 0.623 0.7019 0.3075 0.101 Uiso 1 1 calc R . . C31 C 0.4045(5) 0.9204(4) 0.8290(3) 0.0349(10) Uani 1 1 d . . . C32 C 0.3492(5) 0.9799(4) 0.7600(3) 0.0382(10) Uani 1 1 d . . . H32 H 0.4029 0.9747 0.6992 0.046 Uiso 1 1 calc R . . C33 C 0.2143(5) 1.0469(4) 0.7814(4) 0.0457(12) Uani 1 1 d . . . H33 H 0.1776 1.0871 0.7355 0.055 Uiso 1 1 calc R . . C34 C 0.1359(6) 1.0529(5) 0.8722(4) 0.0556(14) Uani 1 1 d . . . H34 H 0.0447 1.096 0.8871 0.067 Uiso 1 1 calc R . . C35 C 0.1902(6) 0.9963(5) 0.9408(4) 0.0573(15) Uani 1 1 d . . . H35 H 0.1367 1.0031 1.0016 0.069 Uiso 1 1 calc R . . C36 C 0.3242(6) 0.9292(4) 0.9197(3) 0.0453(12) Uani 1 1 d . . . H36 H 0.3603 0.8899 0.9661 0.054 Uiso 1 1 calc R . . C41 C 0.6235(5) 0.7705(4) 0.8968(3) 0.0382(11) Uani 1 1 d . . . C42 C 0.5472(6) 0.6869(5) 0.9502(4) 0.0497(13) Uani 1 1 d . . . H42 H 0.4785 0.6667 0.9314 0.06 Uiso 1 1 calc R . . C43 C 0.5718(7) 0.6334(5) 1.0308(4) 0.0555(15) Uani 1 1 d . . . H43 H 0.52 0.5776 1.0655 0.067 Uiso 1 1 calc R . . C44 C 0.6711(8) 0.6625(5) 1.0589(4) 0.0668(19) Uani 1 1 d . . . H44 H 0.6867 0.6272 1.1134 0.08 Uiso 1 1 calc R . . C45 C 0.7495(9) 0.7439(6) 1.0075(5) 0.083(2) Uani 1 1 d . . . H45 H 0.8178 0.7632 1.0273 0.1 Uiso 1 1 calc R . . C46 C 0.7267(8) 0.7972(5) 0.9261(4) 0.0619(17) Uani 1 1 d . . . H46 H 0.781 0.8511 0.8911 0.074 Uiso 1 1 calc R . . C51 C 0.6816(5) 0.9621(4) 0.7616(3) 0.0335(10) Uani 1 1 d . . . C52 C 0.8094(6) 0.9591(4) 0.6960(4) 0.0460(12) Uani 1 1 d . . . H52 H 0.8466 0.896 0.6602 0.055 Uiso 1 1 calc R . . C53 C 0.8849(6) 1.0489(5) 0.6818(4) 0.0503(13) Uani 1 1 d . . . H53 H 0.9731 1.0441 0.6386 0.06 Uiso 1 1 calc R . . C54 C 0.8291(7) 1.1438(4) 0.7315(4) 0.0534(15) Uani 1 1 d . . . H54 H 0.8794 1.2036 0.7226 0.064 Uiso 1 1 calc R . . C55 C 0.6994(8) 1.1507(5) 0.7942(5) 0.0715(19) Uani 1 1 d . . . H55 H 0.66 1.2167 0.8265 0.086 Uiso 1 1 calc R . . C56 C 0.6254(7) 1.0602(5) 0.8106(5) 0.0587(16) Uani 1 1 d . . . H56 H 0.5378 1.0653 0.8546 0.07 Uiso 1 1 calc R . . C61 C 0.9073(6) 0.4285(5) 0.8468(4) 0.0608(16) Uani 1 1 d D . . H61 H 0.8379 0.4891 0.8266 0.073 Uiso 1 1 calc R A 1 Cl1 Cl 0.59813(14) 0.54439(10) 0.77099(9) 0.0430(3) Uani 1 1 d . . . Cl61 Cl 1.03140(18) 0.36506(14) 0.75285(12) 0.0681(4) Uani 1 1 d D B . Cl62 Cl 0.9838(3) 0.4886(3) 0.9092(2) 0.1108(10) Uani 0.85 1 d PDU B 1 Cl63 Cl 0.8206(2) 0.3193(2) 0.92327(14) 0.0613(5) Uani 0.85 1 d PD B 1 Cl65 Cl 0.986(2) 0.5446(10) 0.8613(8) 0.172(12) Uani 0.15 1 d PDU B 2 Cl64 Cl 0.873(2) 0.3483(18) 0.9428(8) 0.119(7) Uani 0.15 1 d PD B 2 N11 N 0.4196(4) 0.7465(3) 0.6716(2) 0.0315(8) Uani 1 1 d . . . N12 N 0.4014(4) 0.7885(3) 0.5877(3) 0.0339(8) Uani 1 1 d . . . N21 N 0.6708(4) 0.6220(3) 0.5582(2) 0.0360(9) Uani 1 1 d . . . N22 N 0.6060(5) 0.6752(3) 0.4953(3) 0.0391(9) Uani 1 1 d . . . O1 O 0.6519(3) 0.8662(3) 0.5862(2) 0.0338(7) Uani 1 1 d . . . O2 O 0.6554(4) 0.9427(3) 0.4449(2) 0.0476(9) Uani 1 1 d . . . O3 O 0.9022(6) 0.6528(5) 0.7399(5) 0.0995(18) Uani 1 1 d D . . O4 O 0.9474(6) 0.7009(5) 0.5769(4) 0.1025(19) Uani 1 1 d D . . P1 P 0.58513(13) 0.83955(9) 0.79238(8) 0.0308(3) Uani 1 1 d . . . Ru1 Ru 0.62947(4) 0.71751(3) 0.67503(2) 0.02916(13) Uani 1 1 d D . . S1 S 0.85373(15) 0.68230(11) 0.66530(10) 0.0471(3) Uani 1 1 d 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 C1 0.057(3) 0.040(2) 0.029(2) 0.0036(19) -0.018(2) -0.024(2) C2 0.051(3) 0.032(2) 0.033(3) 0.0005(19) -0.010(2) -0.017(2) C11 0.047(3) 0.064(3) 0.040(3) -0.001(2) -0.010(2) -0.023(3) C12 0.040(3) 0.033(2) 0.039(3) -0.0025(19) -0.012(2) -0.0108(19) C13 0.038(3) 0.040(2) 0.051(3) -0.006(2) -0.018(2) -0.013(2) C14 0.050(3) 0.032(2) 0.047(3) -0.002(2) -0.027(2) -0.014(2) C15 0.071(4) 0.051(3) 0.063(4) 0.001(3) -0.043(3) -0.020(3) C21 0.074(4) 0.034(3) 0.078(4) -0.019(3) -0.030(3) -0.001(3) C22 0.052(3) 0.035(2) 0.044(3) -0.013(2) -0.007(2) -0.015(2) C23 0.072(4) 0.043(3) 0.043(3) -0.018(2) -0.005(3) -0.019(3) C24 0.068(4) 0.053(3) 0.033(3) -0.011(2) -0.008(2) -0.029(3) C25 0.097(5) 0.077(4) 0.039(3) -0.010(3) -0.023(3) -0.034(4) C31 0.042(3) 0.031(2) 0.033(2) -0.0040(18) -0.013(2) -0.0070(19) C32 0.046(3) 0.031(2) 0.039(3) -0.0030(19) -0.014(2) -0.010(2) C33 0.044(3) 0.038(3) 0.055(3) -0.001(2) -0.020(3) -0.001(2) C34 0.042(3) 0.054(3) 0.061(4) -0.009(3) -0.008(3) 0.003(2) C35 0.061(4) 0.053(3) 0.047(3) -0.012(3) -0.002(3) -0.005(3) C36 0.052(3) 0.043(3) 0.038(3) -0.004(2) -0.011(2) -0.006(2) C41 0.055(3) 0.033(2) 0.029(2) -0.0013(18) -0.018(2) -0.005(2) C42 0.066(4) 0.045(3) 0.038(3) 0.001(2) -0.018(3) -0.011(3) C43 0.073(4) 0.050(3) 0.034(3) 0.005(2) -0.012(3) -0.004(3) C44 0.119(6) 0.047(3) 0.043(3) 0.007(3) -0.045(4) -0.006(3) C45 0.137(7) 0.064(4) 0.083(5) 0.013(4) -0.083(5) -0.028(4) C46 0.097(5) 0.044(3) 0.067(4) 0.011(3) -0.055(4) -0.022(3) C51 0.046(3) 0.028(2) 0.035(2) -0.0013(17) -0.025(2) -0.0065(19) C52 0.060(3) 0.033(2) 0.051(3) -0.007(2) -0.020(3) -0.016(2) C53 0.060(3) 0.050(3) 0.052(3) -0.003(2) -0.023(3) -0.024(3) C54 0.075(4) 0.034(3) 0.072(4) 0.001(2) -0.044(3) -0.022(3) C55 0.080(5) 0.039(3) 0.103(5) -0.024(3) -0.029(4) -0.015(3) C56 0.062(4) 0.038(3) 0.081(4) -0.024(3) -0.021(3) -0.009(3) C61 0.066(4) 0.055(3) 0.072(4) -0.013(3) -0.034(3) -0.007(3) Cl1 0.0524(7) 0.0357(6) 0.0452(7) 0.0048(5) -0.0194(6) -0.0154(5) Cl61 0.0675(10) 0.0601(9) 0.0691(10) -0.0025(7) -0.0053(8) -0.0214(8) Cl62 0.125(2) 0.116(2) 0.130(3) -0.035(2) -0.065(2) -0.0455(18) Cl63 0.0581(12) 0.0708(13) 0.0474(10) -0.0010(8) -0.0115(9) -0.0059(9) Cl65 0.46(4) 0.079(8) 0.090(9) 0.068(8) -0.186(17) -0.171(16) Cl64 0.118(16) 0.124(16) 0.118(16) 0.004(12) -0.038(12) -0.033(12) N11 0.042(2) 0.0293(18) 0.0280(19) 0.0015(14) -0.0146(17) -0.0129(16) N12 0.048(2) 0.0289(18) 0.032(2) 0.0037(15) -0.0187(18) -0.0153(16) N21 0.052(2) 0.0314(19) 0.029(2) -0.0036(15) -0.0122(18) -0.0167(17) N22 0.057(3) 0.036(2) 0.029(2) -0.0054(16) -0.0094(18) -0.0220(18) O1 0.0473(19) 0.0317(15) 0.0280(16) 0.0014(12) -0.0154(14) -0.0151(14) O2 0.070(3) 0.0441(19) 0.0346(19) 0.0097(15) -0.0180(18) -0.0289(18) O3 0.091(4) 0.078(3) 0.146(5) 0.010(3) -0.065(4) -0.020(3) O4 0.100(4) 0.097(4) 0.109(5) -0.036(3) -0.010(4) -0.027(3) P1 0.0416(7) 0.0259(5) 0.0282(6) -0.0019(4) -0.0149(5) -0.0066(5) Ru1 0.0384(2) 0.02322(18) 0.0288(2) -0.00147(13) -0.01155(15) -0.00997(14) S1 0.0576(8) 0.0385(6) 0.0493(8) -0.0091(5) -0.0104(7) -0.0217(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N12 1.444(6) . ? C1 N22 1.451(6) . ? C1 C2 1.549(6) . ? C1 H1 0.98 . ? C2 O2 1.227(5) . ? C2 O1 1.280(6) . ? C11 C12 1.474(7) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 N11 1.341(6) . ? C12 C13 1.401(7) . ? C13 C14 1.362(7) . ? C13 H13 0.93 . ? C14 N12 1.350(6) . ? C14 C15 1.496(7) . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C21 C22 1.479(8) . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 N21 1.334(6) . ? C22 C23 1.395(7) . ? C23 C24 1.373(8) . ? C23 H23 0.93 . ? C24 N22 1.374(6) . ? C24 C25 1.493(8) . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C31 C36 1.388(7) . ? C31 C32 1.393(7) . ? C31 P1 1.827(5) . ? C32 C33 1.389(7) . ? C32 H32 0.93 . ? C33 C34 1.380(8) . ? C33 H33 0.93 . ? C34 C35 1.374(8) . ? C34 H34 0.93 . ? C35 C36 1.383(8) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C41 C46 1.386(7) . ? C41 C42 1.393(7) . ? C41 P1 1.819(5) . ? C42 C43 1.384(7) . ? C42 H42 0.93 . ? C43 C44 1.351(9) . ? C43 H43 0.93 . ? C44 C45 1.376(10) . ? C44 H44 0.93 . ? C45 C46 1.388(8) . ? C45 H45 0.93 . ? C46 H46 0.93 . ? C51 C52 1.369(7) . ? C51 C56 1.389(7) . ? C51 P1 1.845(5) . ? C52 C53 1.395(7) . ? C52 H52 0.93 . ? C53 C54 1.364(8) . ? C53 H53 0.93 . ? C54 C55 1.362(9) . ? C54 H54 0.93 . ? C55 C56 1.388(8) . ? C55 H55 0.93 . ? C56 H56 0.93 . ? C61 Cl64 1.617(12) . ? C61 Cl62 1.729(6) . ? C61 Cl61 1.733(6) . ? C61 Cl63 1.792(6) . ? C61 Cl65 1.809(10) . ? C61 H61 0.98 . ? Cl1 Ru1 2.3528(12) . ? N11 N12 1.376(5) . ? N11 Ru1 2.112(4) . ? N21 N22 1.354(5) . ? N21 Ru1 2.154(4) . ? O1 Ru1 2.065(3) . ? O3 S1 1.370(6) . ? O4 S1 1.414(6) . ? P1 Ru1 2.3566(11) . ? Ru1 S1 2.1955(15) . ? 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 N12 C1 N22 109.8(4) . . ? N12 C1 C2 113.7(4) . . ? N22 C1 C2 108.9(4) . . ? N12 C1 H1 108.1 . . ? N22 C1 H1 108.1 . . ? C2 C1 H1 108.1 . . ? O2 C2 O1 125.7(4) . . ? O2 C2 C1 117.1(4) . . ? O1 C2 C1 117.1(4) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N11 C12 C13 109.3(4) . . ? N11 C12 C11 124.6(4) . . ? C13 C12 C11 126.2(5) . . ? C14 C13 C12 107.0(4) . . ? C14 C13 H13 126.5 . . ? C12 C13 H13 126.5 . . ? N12 C14 C13 107.0(4) . . ? N12 C14 C15 122.3(5) . . ? C13 C14 C15 130.7(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N21 C22 C23 109.0(5) . . ? N21 C22 C21 123.1(5) . . ? C23 C22 C21 127.9(5) . . ? C24 C23 C22 107.6(4) . . ? C24 C23 H23 126.2 . . ? C22 C23 H23 126.2 . . ? C23 C24 N22 105.5(5) . . ? C23 C24 C25 132.1(5) . . ? N22 C24 C25 122.4(5) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C36 C31 C32 119.5(5) . . ? C36 C31 P1 124.0(4) . . ? C32 C31 P1 116.5(4) . . ? C33 C32 C31 120.6(5) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 118.8(5) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C35 C34 C33 121.2(5) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 120.1(5) . . ? C34 C35 H35 120 . . ? C36 C35 H35 120 . . ? C35 C36 C31 119.9(5) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C46 C41 C42 117.8(5) . . ? C46 C41 P1 122.7(4) . . ? C42 C41 P1 119.5(4) . . ? C43 C42 C41 121.3(6) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C44 C43 C42 119.8(6) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.6(5) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C46 120.1(6) . . ? C44 C45 H45 120 . . ? C46 C45 H45 120 . . ? C41 C46 C45 120.4(6) . . ? C41 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C52 C51 C56 118.1(5) . . ? C52 C51 P1 123.4(3) . . ? C56 C51 P1 118.4(4) . . ? C51 C52 C53 121.1(5) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C54 C53 C52 119.9(6) . . ? C54 C53 H53 120 . . ? C52 C53 H53 120 . . ? C55 C54 C53 119.7(5) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C54 C55 C56 120.8(6) . . ? C54 C55 H55 119.6 . . ? C56 C55 H55 119.6 . . ? C55 C56 C51 120.3(6) . . ? C55 C56 H56 119.9 . . ? C51 C56 H56 119.9 . . ? Cl64 C61 Cl62 78.4(9) . . ? Cl64 C61 Cl61 117.8(8) . . ? Cl62 C61 Cl61 111.8(4) . . ? Cl64 C61 Cl63 28.0(8) . . ? Cl62 C61 Cl63 106.1(3) . . ? Cl61 C61 Cl63 109.9(3) . . ? Cl64 C61 Cl65 107.5(9) . . ? Cl62 C61 Cl65 29.8(3) . . ? Cl61 C61 Cl65 102.7(7) . . ? Cl63 C61 Cl65 134.2(5) . . ? Cl64 C61 H61 124.4 . . ? Cl62 C61 H61 109.6 . . ? Cl61 C61 H61 109.6 . . ? Cl63 C61 H61 109.6 . . ? Cl65 C61 H61 87.7 . . ? C12 N11 N12 105.9(4) . . ? C12 N11 Ru1 139.3(3) . . ? N12 N11 Ru1 114.8(3) . . ? C14 N12 N11 110.7(4) . . ? C14 N12 C1 128.7(4) . . ? N11 N12 C1 119.8(4) . . ? C22 N21 N22 107.1(4) . . ? C22 N21 Ru1 137.3(3) . . ? N22 N21 Ru1 115.6(3) . . ? N21 N22 C24 110.8(4) . . ? N21 N22 C1 118.9(3) . . ? C24 N22 C1 130.3(4) . . ? C2 O1 Ru1 119.2(3) . . ? C41 P1 C31 105.5(2) . . ? C41 P1 C51 102.8(2) . . ? C31 P1 C51 100.0(2) . . ? C41 P1 Ru1 116.85(15) . . ? C31 P1 Ru1 114.22(15) . . ? C51 P1 Ru1 115.46(15) . . ? O1 Ru1 N11 87.09(13) . . ? O1 Ru1 N21 87.84(13) . . ? N11 Ru1 N21 83.15(14) . . ? O1 Ru1 S1 91.27(10) . . ? N11 Ru1 S1 174.53(10) . . ? N21 Ru1 S1 91.58(11) . . ? O1 Ru1 Cl1 176.79(9) . . ? N11 Ru1 Cl1 90.77(10) . . ? N21 Ru1 Cl1 89.52(10) . . ? S1 Ru1 Cl1 90.65(5) . . ? O1 Ru1 P1 86.28(9) . . ? N11 Ru1 P1 96.11(10) . . ? N21 Ru1 P1 174.11(10) . . ? S1 Ru1 P1 88.98(5) . . ? Cl1 Ru1 P1 96.33(4) . . ? O3 S1 O4 120.7(4) . . ? O3 S1 Ru1 123.2(3) . . ? O4 S1 Ru1 115.9(3) . . ?