# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Tai-Chu Lau' _publ_contact_author_email BHTCLAU@CITYU.EDU.HK _publ_section_title ; A novel tricyanoruthenium(III) building block for the construction of bimetallic coordination polymers ; loop_ _publ_author_name 'Tai-Chu Lau.' 'Song Gao.' 'Junfang Guo.' 'Gene-Hsiang Lee.' 'Wai-Lun Man.' ; Shie-Ming Peng ; 'Jing Xiang.' 'Guancheng Xu.' 'Shek-Man Yiu.' # Attachment 'Compounds_1-41.cif' #================================================================= data_1 _database_code_depnum_ccdc_archive 'CCDC 764141' #TrackingRef 'Compounds_1-41.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H9 Cl N2 O2 Ru' _chemical_formula_sum 'C13 H9 Cl N2 O2 Ru' _chemical_formula_weight 361.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7794(7) _cell_length_b 12.5674(11) _cell_length_c 13.3405(12) _cell_angle_alpha 90.00 _cell_angle_beta 106.133(2) _cell_angle_gamma 90.00 _cell_volume 1252.90(19) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2853 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 26.73 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7114 _exptl_absorpt_correction_T_max 0.8676 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART ApexCCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7956 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2868 _reflns_number_gt 2548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0519P)^2^+0.5406P] 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_extinction_coef ? _refine_ls_number_reflns 2868 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.27364(3) 0.217581(19) 0.837396(17) 0.03385(11) Uani 1 1 d . . . Cl1 Cl 0.22140(11) 0.19122(8) 0.66061(6) 0.0475(2) Uani 1 1 d . . . O1 O 0.4606(3) 0.31753(19) 0.82594(18) 0.0452(5) Uani 1 1 d . . . O2 O 0.2209(3) 0.06623(18) 0.84332(16) 0.0439(5) Uani 1 1 d . . . N1 N 0.1036(4) 0.2829(2) 0.8473(3) 0.0487(7) Uani 1 1 d . . . N2 N 0.4327(4) 0.2127(2) 0.9868(2) 0.0416(6) Uani 1 1 d . . . C1 C 0.5618(4) 0.3531(2) 0.9193(3) 0.0401(7) Uani 1 1 d . . . C2 C 0.6767(5) 0.4386(3) 0.9256(3) 0.0502(8) Uani 1 1 d . . . H2A H 0.6839 0.4731 0.8652 0.060 Uiso 1 1 calc R . . C3 C 0.7794(5) 0.4718(3) 1.0211(3) 0.0527(9) Uani 1 1 d . . . H3A H 0.8558 0.5295 1.0253 0.063 Uiso 1 1 calc R . . C4 C 0.7713(5) 0.4201(3) 1.1126(3) 0.0564(9) Uani 1 1 d . . . H4A H 0.8423 0.4431 1.1771 0.068 Uiso 1 1 calc R . . C5 C 0.6573(5) 0.3350(3) 1.1062(3) 0.0492(8) Uani 1 1 d . . . H5A H 0.6505 0.3000 1.1665 0.059 Uiso 1 1 calc R . . C6 C 0.5535(4) 0.3020(2) 1.0100(3) 0.0389(7) Uani 1 1 d . . . C7 C 0.4257(4) 0.1417(3) 1.0536(3) 0.0420(7) Uani 1 1 d . . . H7A H 0.4962 0.1514 1.1217 0.050 Uiso 1 1 calc R . . C8 C 0.3176(4) 0.0481(2) 1.0315(2) 0.0371(6) Uani 1 1 d . . . C9 C 0.3170(4) -0.0162(3) 1.1174(3) 0.0443(7) Uani 1 1 d . . . H9A H 0.3805 0.0052 1.1841 0.053 Uiso 1 1 calc R . . C10 C 0.2239(5) -0.1102(3) 1.1041(3) 0.0459(8) Uani 1 1 d . . . H10A H 0.2232 -0.1522 1.1614 0.055 Uiso 1 1 calc R . . C11 C 0.1317(4) -0.1415(3) 1.0052(3) 0.0422(7) Uani 1 1 d . . . H11A H 0.0684 -0.2052 0.9964 0.051 Uiso 1 1 calc R . . C12 C 0.1302(4) -0.0820(3) 0.9195(2) 0.0397(7) Uani 1 1 d . . . H12A H 0.0675 -0.1057 0.8535 0.048 Uiso 1 1 calc R . . C13 C 0.2229(4) 0.0149(2) 0.9306(2) 0.0366(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 Ru 0.03552(16) 0.03261(17) 0.03262(16) 0.00209(9) 0.00816(11) 0.00171(9) Cl1 0.0585(5) 0.0500(5) 0.0330(4) 0.0027(3) 0.0108(4) -0.0043(4) O1 0.0456(12) 0.0410(12) 0.0472(13) -0.0003(11) 0.0102(10) -0.0102(10) O2 0.0595(14) 0.0334(12) 0.0395(12) 0.0048(9) 0.0151(10) -0.0023(10) N1 0.0461(16) 0.0439(18) 0.0553(18) 0.0013(13) 0.0126(14) 0.0073(12) N2 0.0410(14) 0.0407(16) 0.0441(15) -0.0024(11) 0.0136(12) 0.0023(11) C1 0.0382(16) 0.0304(15) 0.0498(18) -0.0050(13) 0.0093(14) -0.0018(12) C2 0.0517(19) 0.0385(18) 0.062(2) 0.0026(16) 0.0190(17) -0.0072(15) C3 0.0450(18) 0.0403(19) 0.073(2) -0.0119(17) 0.0176(18) -0.0140(15) C4 0.047(2) 0.054(2) 0.064(2) -0.0188(18) 0.0089(17) -0.0058(17) C5 0.0518(19) 0.050(2) 0.0461(19) -0.0063(16) 0.0135(15) -0.0042(16) C6 0.0374(15) 0.0291(15) 0.0507(18) -0.0055(13) 0.0130(14) -0.0020(12) C7 0.0432(17) 0.0427(18) 0.0400(16) -0.0023(14) 0.0116(13) 0.0028(14) C8 0.0320(14) 0.0342(16) 0.0460(17) -0.0040(13) 0.0123(13) 0.0016(12) C9 0.0431(17) 0.049(2) 0.0394(16) -0.0044(14) 0.0091(14) 0.0019(14) C10 0.0487(18) 0.0458(19) 0.0446(18) 0.0084(15) 0.0151(15) 0.0017(15) C11 0.0395(16) 0.0366(17) 0.0527(19) 0.0021(14) 0.0165(14) -0.0055(13) C12 0.0382(15) 0.0354(17) 0.0430(17) -0.0032(13) 0.0071(13) -0.0025(13) C13 0.0345(14) 0.0340(16) 0.0419(16) 0.0034(13) 0.0116(13) 0.0044(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N1 1.593(3) . ? Ru O2 1.952(2) . ? Ru O1 1.959(2) . ? Ru N2 2.034(3) . ? Ru Cl1 2.3031(8) . ? O1 C1 1.351(4) . ? O2 C13 1.327(4) . ? N2 C7 1.273(4) . ? N2 C6 1.441(4) . ? C1 C2 1.385(4) . ? C1 C6 1.386(5) . ? C2 C3 1.368(5) . ? C3 C4 1.398(5) . ? C4 C5 1.378(5) . ? C5 C6 1.377(5) . ? C7 C8 1.427(4) . ? C8 C9 1.403(4) . ? C8 C13 1.407(4) . ? C9 C10 1.371(5) . ? C10 C11 1.372(5) . ? C11 C12 1.364(4) . ? C12 C13 1.401(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 N1 Ru O2 108.06(13) . . ? N1 Ru O1 109.10(14) . . ? O2 Ru O1 142.82(10) . . ? N1 Ru N2 103.13(14) . . ? O2 Ru N2 90.47(10) . . ? O1 Ru N2 80.40(10) . . ? N1 Ru Cl1 104.18(12) . . ? O2 Ru Cl1 85.53(7) . . ? O1 Ru Cl1 86.33(7) . . ? N2 Ru Cl1 152.29(8) . . ? C1 O1 Ru 113.24(19) . . ? C13 O2 Ru 123.90(19) . . ? C7 N2 C6 123.2(3) . . ? C7 N2 Ru 125.1(2) . . ? C6 N2 Ru 111.7(2) . . ? O1 C1 C2 120.8(3) . . ? O1 C1 C6 119.7(3) . . ? C2 C1 C6 119.5(3) . . ? C3 C2 C1 119.5(3) . . ? C2 C3 C4 121.0(3) . . ? C5 C4 C3 119.4(3) . . ? C6 C5 C4 119.5(3) . . ? C5 C6 C1 121.1(3) . . ? C5 C6 N2 127.8(3) . . ? C1 C6 N2 111.1(3) . . ? N2 C7 C8 124.8(3) . . ? C9 C8 C13 119.4(3) . . ? C9 C8 C7 116.2(3) . . ? C13 C8 C7 124.3(3) . . ? C10 C9 C8 120.8(3) . . ? C9 C10 C11 119.2(3) . . ? C12 C11 C10 121.9(3) . . ? C11 C12 C13 120.3(3) . . ? O2 C13 C12 116.7(3) . . ? O2 C13 C8 124.8(3) . . ? C12 C13 C8 118.4(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.022 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.089 #================================================================= data_2 _database_code_depnum_ccdc_archive 'CCDC 764142' #TrackingRef 'Compounds_1-41.cif' _audit_update_record ; 2010-05-11 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H48 N5 O2 P2 Ru' _chemical_formula_weight 1094.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.17150(10) _cell_length_b 27.0344(3) _cell_length_c 17.9058(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.2730(10) _cell_angle_gamma 90.00 _cell_volume 5844.48(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16596 _cell_measurement_theta_min 3.6608 _cell_measurement_theta_max 71.3469 _exptl_crystal_description rectangle _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2252 _exptl_absorpt_coefficient_mu 3.053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.50202 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23453 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 67.00 _reflns_number_total 10291 _reflns_number_gt 8780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep-3 _computing_publication_material wingx _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. Since the nature of the solvent couldn't be unambiguously identified, therefore the residual electron density has been smoothed away using PLATON SQUEEZE. The squeeze results have been appended to the last paragraph of the cif. ; _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^)+(0.0514P)^2^+1.3540P] 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_extinction_coef ? _refine_ls_number_reflns 10291 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.257942(14) 0.351571(6) 0.829971(9) 0.03966(6) Uani 1 1 d . . . P1 P 0.70635(5) 0.26629(2) 0.09924(3) 0.04473(13) Uani 1 1 d . . . P2 P 0.79052(5) 0.53711(2) 0.74765(3) 0.04616(14) Uani 1 1 d . . . O1 O 0.17851(14) 0.29197(6) 0.79005(10) 0.0537(4) Uani 1 1 d . . . O2 O 0.34213(14) 0.40982(6) 0.87874(9) 0.0499(4) Uani 1 1 d . . . N1 N 0.25571(16) 0.33245(7) 0.94151(12) 0.0490(4) Uani 1 1 d . . . N2 N 0.0264(2) 0.40932(11) 0.82999(15) 0.0766(7) Uani 1 1 d . . . N3 N 0.48765(18) 0.29212(8) 0.82850(13) 0.0569(5) Uani 1 1 d . . . N4 N 0.2613(2) 0.39502(11) 0.66640(13) 0.0764(7) Uani 1 1 d . . . N5 N 0.1318(2) 0.30075(10) 1.09814(13) 0.0670(6) Uani 1 1 d . . . C1 C 0.1089(2) 0.38888(10) 0.83045(14) 0.0523(6) Uani 1 1 d . . . C2 C 0.40756(19) 0.31401(8) 0.82853(12) 0.0423(5) Uani 1 1 d . . . C3 C 0.2615(2) 0.37815(9) 0.72497(14) 0.0506(5) Uani 1 1 d . . . C4 C 0.13278(17) 0.26036(8) 0.83259(14) 0.0442(5) Uani 1 1 d . . . C5 C 0.08000(19) 0.21932(9) 0.79440(14) 0.0480(5) Uani 1 1 d . . . H5 H 0.0820 0.2160 0.7429 0.058 Uiso 1 1 calc R . . C6 C 0.0264(2) 0.18453(10) 0.83102(16) 0.0567(6) Uani 1 1 d . . . H6 H -0.0080 0.1581 0.8044 0.068 Uiso 1 1 calc R . . C7 C 0.0229(2) 0.18835(10) 0.90818(16) 0.0613(7) Uani 1 1 d . . . H7 H -0.0140 0.1646 0.9331 0.074 Uiso 1 1 calc R . . C8 C 0.0736(2) 0.22691(9) 0.94695(15) 0.0527(6) Uani 1 1 d . . . H8 H 0.0703 0.2290 0.9985 0.063 Uiso 1 1 calc R . . C9 C 0.13080(18) 0.26392(8) 0.91236(13) 0.0446(5) Uani 1 1 d . . . C10 C 0.18777(19) 0.30094(9) 0.96257(14) 0.0482(5) Uani 1 1 d . . . C11 C 0.1629(2) 0.30180(9) 1.04110(14) 0.0510(5) Uani 1 1 d . . . C12 C 0.32876(18) 0.36384(8) 0.99144(13) 0.0433(5) Uani 1 1 d . . . C13 C 0.36785(19) 0.35614(9) 1.06656(14) 0.0492(5) Uani 1 1 d . . . H13 H 0.3439 0.3287 1.0913 0.059 Uiso 1 1 calc R . . C14 C 0.4419(2) 0.38871(10) 1.10529(14) 0.0554(6) Uani 1 1 d . . . H14 H 0.4672 0.3834 1.1559 0.066 Uiso 1 1 calc R . . C15 C 0.4782(2) 0.42938(10) 1.06806(15) 0.0571(6) Uani 1 1 d . . . H15 H 0.5265 0.4519 1.0941 0.069 Uiso 1 1 calc R . . C16 C 0.4434(2) 0.43656(9) 0.99315(14) 0.0510(5) Uani 1 1 d . . . H16 H 0.4689 0.4638 0.9688 0.061 Uiso 1 1 calc R . . C17 C 0.37016(19) 0.40363(8) 0.95272(13) 0.0436(5) Uani 1 1 d . . . C18 C 0.7523(3) 0.43817(10) 0.71841(17) 0.0709(8) Uani 1 1 d . . . H18 H 0.8214 0.4378 0.7014 0.085 Uiso 1 1 calc R . . C19 C 0.6898(4) 0.39515(12) 0.7178(2) 0.0998(14) Uani 1 1 d . . . H19 H 0.7171 0.3659 0.6998 0.120 Uiso 1 1 calc R . . C20 C 0.5892(4) 0.39522(14) 0.7432(2) 0.1005(14) Uani 1 1 d . . . H20 H 0.5479 0.3662 0.7417 0.121 Uiso 1 1 calc R . . C21 C 0.5487(3) 0.43717(15) 0.7706(2) 0.0924(11) Uani 1 1 d . . . H21 H 0.4804 0.4367 0.7888 0.111 Uiso 1 1 calc R . . C22 C 0.6088(3) 0.48093(12) 0.77183(19) 0.0743(8) Uani 1 1 d . . . H22 H 0.5811 0.5097 0.7908 0.089 Uiso 1 1 calc R . . C23 C 0.7104(2) 0.48140(9) 0.74455(14) 0.0530(6) Uani 1 1 d . . . C24 C 0.8621(2) 0.54704(9) 0.84040(14) 0.0541(6) Uani 1 1 d . . . C25 C 0.8151(3) 0.53183(13) 0.90286(16) 0.0700(8) Uani 1 1 d . . . H25 H 0.7483 0.5147 0.8972 0.084 Uiso 1 1 calc R . . C26 C 0.8690(3) 0.54248(15) 0.97432(18) 0.0847(10) Uani 1 1 d . . . H26 H 0.8375 0.5326 1.0166 0.102 Uiso 1 1 calc R . . C27 C 0.9671(3) 0.56707(15) 0.98306(19) 0.0833(10) Uani 1 1 d . . . H27 H 1.0029 0.5733 1.0311 0.100 Uiso 1 1 calc R . . C28 C 1.0131(3) 0.58253(15) 0.9219(2) 0.0882(10) Uani 1 1 d . . . H28 H 1.0797 0.5998 0.9283 0.106 Uiso 1 1 calc R . . C29 C 0.9613(3) 0.57274(12) 0.85027(17) 0.0728(8) Uani 1 1 d . . . H29 H 0.9931 0.5835 0.8086 0.087 Uiso 1 1 calc R . . C30 C 0.8926(2) 0.53321(9) 0.68381(14) 0.0516(6) Uani 1 1 d . . . C31 C 0.9849(2) 0.50363(12) 0.70188(19) 0.0704(8) Uani 1 1 d . . . H31 H 0.9940 0.4858 0.7467 0.084 Uiso 1 1 calc R . . C32 C 1.0641(3) 0.50074(15) 0.6523(3) 0.0938(12) Uani 1 1 d . . . H32 H 1.1265 0.4810 0.6640 0.113 Uiso 1 1 calc R . . C33 C 1.0500(4) 0.52696(16) 0.5866(3) 0.1019(14) Uani 1 1 d . . . H33 H 1.1038 0.5255 0.5542 0.122 Uiso 1 1 calc R . . C34 C 0.9580(4) 0.55512(15) 0.5682(2) 0.0968(12) Uani 1 1 d . . . H34 H 0.9487 0.5722 0.5227 0.116 Uiso 1 1 calc R . . C35 C 0.8777(3) 0.55874(11) 0.61651(17) 0.0719(8) Uani 1 1 d . . . H35 H 0.8149 0.5781 0.6038 0.086 Uiso 1 1 calc R . . C36 C 0.6998(2) 0.58845(9) 0.72253(13) 0.0489(5) Uani 1 1 d . . . C37 C 0.7257(2) 0.63470(9) 0.75288(15) 0.0531(6) Uani 1 1 d . . . H37 H 0.7894 0.6390 0.7869 0.064 Uiso 1 1 calc R . . C38 C 0.6576(2) 0.67439(10) 0.73294(17) 0.0628(7) Uani 1 1 d . . . H38 H 0.6763 0.7056 0.7525 0.075 Uiso 1 1 calc R . . C39 C 0.5628(3) 0.66821(12) 0.68459(19) 0.0720(8) Uani 1 1 d . . . H39 H 0.5161 0.6950 0.6724 0.086 Uiso 1 1 calc R . . C40 C 0.5359(3) 0.62256(13) 0.6538(2) 0.0817(9) Uani 1 1 d . . . H40 H 0.4715 0.6186 0.6204 0.098 Uiso 1 1 calc R . . C41 C 0.6048(3) 0.58236(11) 0.67230(18) 0.0719(8) Uani 1 1 d . . . H41 H 0.5872 0.5515 0.6511 0.086 Uiso 1 1 calc R . . C42 C 0.7981(2) 0.21403(9) 0.10357(13) 0.0496(5) Uani 1 1 d . . . C43 C 0.9014(2) 0.21670(12) 0.14687(18) 0.0692(8) Uani 1 1 d . . . H43 H 0.9210 0.2449 0.1753 0.083 Uiso 1 1 calc R . . C44 C 0.9750(3) 0.17775(13) 0.14792(19) 0.0786(9) Uani 1 1 d . . . H44 H 1.0433 0.1794 0.1776 0.094 Uiso 1 1 calc R . . C45 C 0.9468(3) 0.13678(13) 0.10503(19) 0.0767(9) Uani 1 1 d . . . H45 H 0.9966 0.1107 0.1053 0.092 Uiso 1 1 calc R . . C46 C 0.8457(3) 0.13377(12) 0.06151(18) 0.0750(8) Uani 1 1 d . . . H46 H 0.8273 0.1057 0.0327 0.090 Uiso 1 1 calc R . . C47 C 0.7709(2) 0.17255(10) 0.06048(16) 0.0605(6) Uani 1 1 d . . . H47 H 0.7027 0.1706 0.0308 0.073 Uiso 1 1 calc R . . C48 C 0.56485(19) 0.24583(9) 0.08114(13) 0.0455(5) Uani 1 1 d . . . C49 C 0.5139(2) 0.24083(10) 0.00738(14) 0.0558(6) Uani 1 1 d . . . H49 H 0.5508 0.2503 -0.0327 0.067 Uiso 1 1 calc R . . C50 C 0.4081(2) 0.22169(11) -0.00559(16) 0.0629(7) Uani 1 1 d . . . H50 H 0.3734 0.2186 -0.0547 0.075 Uiso 1 1 calc R . . C51 C 0.3536(2) 0.20716(10) 0.05333(17) 0.0633(7) Uani 1 1 d . . . H51 H 0.2833 0.1933 0.0438 0.076 Uiso 1 1 calc R . . C52 C 0.4030(2) 0.21312(10) 0.12699(16) 0.0592(6) Uani 1 1 d . . . H52 H 0.3653 0.2041 0.1669 0.071 Uiso 1 1 calc R . . C53 C 0.5083(2) 0.23243(9) 0.14051(14) 0.0524(6) Uani 1 1 d . . . H53 H 0.5417 0.2365 0.1898 0.063 Uiso 1 1 calc R . . C54 C 0.73745(19) 0.30582(9) 0.02401(14) 0.0482(5) Uani 1 1 d . . . C55 C 0.8364(2) 0.29963(10) -0.00640(16) 0.0577(6) Uani 1 1 d . . . H55 H 0.8854 0.2746 0.0112 0.069 Uiso 1 1 calc R . . C56 C 0.8610(2) 0.33093(12) -0.06299(17) 0.0680(7) Uani 1 1 d . . . H56 H 0.9265 0.3266 -0.0840 0.082 Uiso 1 1 calc R . . C57 C 0.7904(3) 0.36802(13) -0.08825(18) 0.0742(8) Uani 1 1 d . . . H57 H 0.8083 0.3894 -0.1255 0.089 Uiso 1 1 calc R . . C58 C 0.6921(3) 0.37375(13) -0.0584(2) 0.0806(9) Uani 1 1 d . . . H58 H 0.6436 0.3989 -0.0762 0.097 Uiso 1 1 calc R . . C59 C 0.6649(2) 0.34273(11) -0.00284(17) 0.0662(7) Uani 1 1 d . . . H59 H 0.5981 0.3466 0.0165 0.079 Uiso 1 1 calc R . . C60 C 0.7274(2) 0.29816(10) 0.18848(14) 0.0534(6) Uani 1 1 d . . . C61 C 0.7330(2) 0.27169(12) 0.25515(15) 0.0660(7) Uani 1 1 d . . . H61 H 0.7310 0.2373 0.2542 0.079 Uiso 1 1 calc R . . C62 C 0.7416(3) 0.29649(18) 0.32296(17) 0.0851(11) Uani 1 1 d . . . H62 H 0.7452 0.2787 0.3676 0.102 Uiso 1 1 calc R . . C63 C 0.7450(3) 0.34668(18) 0.3251(2) 0.0931(13) Uani 1 1 d . . . H63 H 0.7504 0.3629 0.3712 0.112 Uiso 1 1 calc R . . C64 C 0.7404(3) 0.37362(15) 0.2599(2) 0.0929(12) Uani 1 1 d . . . H64 H 0.7438 0.4080 0.2620 0.112 Uiso 1 1 calc R . . C65 C 0.7308(2) 0.34950(11) 0.19018(19) 0.0681(7) Uani 1 1 d . . . H65 H 0.7267 0.3676 0.1457 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.04749(10) 0.03799(9) 0.03466(9) 0.00208(7) 0.00969(6) -0.00154(7) P1 0.0452(3) 0.0468(3) 0.0416(3) 0.0027(2) 0.0035(2) 0.0024(2) P2 0.0560(3) 0.0392(3) 0.0449(3) -0.0019(2) 0.0124(3) -0.0017(2) O1 0.0606(10) 0.0496(9) 0.0518(9) -0.0053(8) 0.0101(8) -0.0118(8) O2 0.0627(10) 0.0413(8) 0.0454(9) -0.0016(7) 0.0054(7) -0.0030(7) N1 0.0511(11) 0.0451(10) 0.0519(11) 0.0022(9) 0.0102(9) 0.0044(9) N2 0.0663(15) 0.0973(19) 0.0689(15) 0.0100(14) 0.0187(12) 0.0244(14) N3 0.0579(13) 0.0520(12) 0.0615(13) 0.0002(10) 0.0102(10) 0.0036(10) N4 0.0967(19) 0.0857(18) 0.0508(14) 0.0219(13) 0.0243(13) 0.0206(15) N5 0.0781(15) 0.0785(16) 0.0477(12) -0.0062(11) 0.0207(11) -0.0225(13) C1 0.0586(15) 0.0572(14) 0.0428(12) 0.0066(11) 0.0125(11) 0.0013(12) C2 0.0529(13) 0.0401(11) 0.0344(10) 0.0012(9) 0.0080(9) -0.0050(10) C3 0.0547(13) 0.0510(13) 0.0477(13) 0.0037(11) 0.0130(10) 0.0038(11) C4 0.0346(10) 0.0416(11) 0.0565(13) -0.0032(10) 0.0061(9) 0.0009(9) C5 0.0455(12) 0.0483(12) 0.0498(13) -0.0105(11) 0.0046(10) -0.0013(10) C6 0.0540(14) 0.0492(13) 0.0667(16) -0.0124(12) 0.0069(12) -0.0114(11) C7 0.0668(16) 0.0513(14) 0.0676(17) 0.0000(13) 0.0156(13) -0.0113(12) C8 0.0560(14) 0.0519(13) 0.0500(13) -0.0013(11) 0.0063(11) 0.0027(11) C9 0.0384(11) 0.0421(11) 0.0512(13) -0.0069(10) -0.0023(9) 0.0048(9) C10 0.0469(12) 0.0452(12) 0.0531(13) 0.0015(10) 0.0087(10) 0.0026(10) C11 0.0592(14) 0.0508(13) 0.0448(13) 0.0026(11) 0.0134(11) -0.0021(11) C12 0.0437(11) 0.0376(11) 0.0484(12) -0.0053(9) 0.0052(9) 0.0009(9) C13 0.0466(12) 0.0477(12) 0.0549(14) 0.0036(11) 0.0127(10) -0.0035(10) C14 0.0569(14) 0.0650(15) 0.0439(13) -0.0042(11) 0.0048(11) 0.0012(12) C15 0.0598(14) 0.0508(14) 0.0596(15) -0.0133(12) 0.0032(12) -0.0108(11) C16 0.0592(14) 0.0387(11) 0.0560(14) -0.0041(10) 0.0108(11) -0.0113(10) C17 0.0477(12) 0.0379(11) 0.0457(12) -0.0030(9) 0.0085(9) 0.0015(9) C18 0.101(2) 0.0457(14) 0.0719(18) -0.0060(13) 0.0354(17) -0.0098(14) C19 0.170(4) 0.0503(17) 0.090(2) -0.0155(17) 0.059(3) -0.033(2) C20 0.156(4) 0.077(2) 0.075(2) -0.0110(18) 0.040(2) -0.059(2) C21 0.096(2) 0.102(3) 0.086(2) -0.007(2) 0.038(2) -0.043(2) C22 0.0772(19) 0.0694(18) 0.082(2) -0.0097(16) 0.0328(16) -0.0133(15) C23 0.0690(16) 0.0443(12) 0.0478(13) -0.0006(11) 0.0151(11) -0.0101(11) C24 0.0678(15) 0.0474(13) 0.0474(13) -0.0018(11) 0.0089(11) 0.0094(12) C25 0.0706(18) 0.087(2) 0.0535(15) 0.0044(15) 0.0130(13) 0.0134(16) C26 0.100(3) 0.107(3) 0.0493(16) 0.0072(17) 0.0183(16) 0.032(2) C27 0.087(2) 0.100(3) 0.0595(18) -0.0167(18) -0.0042(16) 0.020(2) C28 0.092(2) 0.099(3) 0.071(2) -0.0203(19) 0.0002(18) -0.012(2) C29 0.084(2) 0.0763(19) 0.0578(16) -0.0068(15) 0.0071(15) -0.0177(16) C30 0.0628(15) 0.0416(12) 0.0533(14) -0.0075(11) 0.0188(11) -0.0070(11) C31 0.0624(16) 0.0708(18) 0.080(2) -0.0089(16) 0.0156(15) 0.0037(14) C32 0.070(2) 0.095(3) 0.122(3) -0.036(2) 0.034(2) -0.0013(18) C33 0.114(3) 0.090(3) 0.117(3) -0.031(2) 0.073(3) -0.022(2) C34 0.140(4) 0.082(2) 0.080(2) -0.0024(19) 0.060(2) -0.011(2) C35 0.102(2) 0.0556(15) 0.0643(17) 0.0010(14) 0.0329(16) -0.0005(15) C36 0.0559(13) 0.0454(12) 0.0468(12) 0.0010(10) 0.0119(10) 0.0017(10) C37 0.0603(14) 0.0450(12) 0.0559(14) -0.0010(11) 0.0143(12) -0.0032(11) C38 0.0771(18) 0.0427(13) 0.0732(18) 0.0022(13) 0.0273(15) 0.0005(12) C39 0.079(2) 0.0595(16) 0.081(2) 0.0153(15) 0.0235(17) 0.0178(15) C40 0.075(2) 0.080(2) 0.085(2) -0.0009(18) -0.0104(17) 0.0136(17) C41 0.0761(19) 0.0571(16) 0.0777(19) -0.0131(15) -0.0083(15) 0.0058(14) C42 0.0531(13) 0.0490(13) 0.0460(12) 0.0069(10) 0.0038(10) 0.0064(10) C43 0.0616(16) 0.0672(17) 0.0742(19) -0.0039(15) -0.0087(14) 0.0122(14) C44 0.0689(18) 0.091(2) 0.0727(19) 0.0066(18) -0.0037(15) 0.0297(17) C45 0.090(2) 0.074(2) 0.0702(19) 0.0185(16) 0.0236(17) 0.0360(17) C46 0.102(2) 0.0581(16) 0.0676(18) -0.0061(14) 0.0225(18) 0.0119(16) C47 0.0672(16) 0.0571(15) 0.0572(15) -0.0005(13) 0.0083(12) 0.0037(13) C48 0.0460(12) 0.0462(12) 0.0432(12) 0.0038(10) 0.0010(9) 0.0028(10) C49 0.0548(14) 0.0687(16) 0.0440(13) 0.0010(12) 0.0070(11) 0.0031(12) C50 0.0569(15) 0.0741(17) 0.0542(15) -0.0075(13) -0.0059(12) 0.0049(13) C51 0.0510(14) 0.0606(16) 0.0769(19) -0.0025(14) 0.0031(13) -0.0041(12) C52 0.0567(14) 0.0613(15) 0.0597(15) 0.0122(13) 0.0084(12) -0.0055(12) C53 0.0560(14) 0.0552(14) 0.0450(12) 0.0083(11) 0.0033(10) -0.0023(11) C54 0.0472(12) 0.0485(13) 0.0491(13) 0.0047(10) 0.0072(10) 0.0006(10) C55 0.0503(13) 0.0584(15) 0.0650(16) 0.0064(13) 0.0096(12) 0.0050(11) C56 0.0596(16) 0.0772(19) 0.0708(18) 0.0105(16) 0.0221(14) -0.0014(14) C57 0.0721(19) 0.085(2) 0.0674(18) 0.0256(16) 0.0161(15) -0.0066(16) C58 0.078(2) 0.083(2) 0.083(2) 0.0384(19) 0.0174(17) 0.0207(17) C59 0.0593(15) 0.0721(18) 0.0700(17) 0.0232(15) 0.0195(13) 0.0147(13) C60 0.0459(12) 0.0622(15) 0.0513(14) -0.0079(12) 0.0027(10) 0.0005(11) C61 0.0652(16) 0.0809(19) 0.0500(15) -0.0017(14) 0.0004(12) -0.0013(14) C62 0.073(2) 0.132(3) 0.0477(16) -0.0085(19) -0.0003(14) 0.005(2) C63 0.074(2) 0.135(4) 0.067(2) -0.041(2) -0.0034(17) 0.018(2) C64 0.089(2) 0.083(2) 0.104(3) -0.044(2) 0.000(2) 0.0147(19) C65 0.0692(17) 0.0633(17) 0.0699(18) -0.0127(14) 0.0014(14) 0.0063(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 1.9664(16) . ? Ru1 O2 2.0164(16) . ? Ru1 C3 2.018(2) . ? Ru1 N1 2.067(2) . ? Ru1 C1 2.076(3) . ? Ru1 C2 2.088(2) . ? P1 C42 1.796(2) . ? P1 C54 1.797(2) . ? P1 C48 1.799(2) . ? P1 C60 1.805(3) . ? P2 C23 1.791(2) . ? P2 C30 1.795(2) . ? P2 C24 1.795(3) . ? P2 C36 1.795(2) . ? O1 C4 1.314(3) . ? O2 C17 1.336(3) . ? N1 C10 1.277(3) . ? N1 C12 1.452(3) . ? N2 C1 1.146(3) . ? N3 C2 1.141(3) . ? N4 C3 1.143(3) . ? N5 C11 1.134(3) . ? C4 C5 1.414(3) . ? C4 C9 1.435(3) . ? C5 C6 1.359(4) . ? C5 H5 0.9300 . ? C6 C7 1.391(4) . ? C6 H6 0.9300 . ? C7 C8 1.356(4) . ? C7 H7 0.9300 . ? C8 C9 1.407(3) . ? C8 H8 0.9300 . ? C9 C10 1.460(3) . ? C10 C11 1.476(3) . ? C12 C13 1.384(3) . ? C12 C17 1.407(3) . ? C13 C14 1.382(3) . ? C13 H13 0.9300 . ? C14 C15 1.387(4) . ? C14 H14 0.9300 . ? C15 C16 1.369(4) . ? C15 H15 0.9300 . ? C16 C17 1.395(3) . ? C16 H16 0.9300 . ? C18 C23 1.380(4) . ? C18 C19 1.390(4) . ? C18 H18 0.9300 . ? C19 C20 1.359(6) . ? C19 H19 0.9300 . ? C20 C21 1.353(6) . ? C20 H20 0.9300 . ? C21 C22 1.390(4) . ? C21 H21 0.9300 . ? C22 C23 1.386(4) . ? C22 H22 0.9300 . ? C24 C25 1.382(4) . ? C24 C29 1.384(4) . ? C25 C26 1.392(4) . ? C25 H25 0.9300 . ? C26 C27 1.358(5) . ? C26 H26 0.9300 . ? C27 C28 1.357(5) . ? C27 H27 0.9300 . ? C28 C29 1.381(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C35 1.381(4) . ? C30 C31 1.384(4) . ? C31 C32 1.392(5) . ? C31 H31 0.9300 . ? C32 C33 1.366(6) . ? C32 H32 0.9300 . ? C33 C34 1.360(6) . ? C33 H33 0.9300 . ? C34 C35 1.388(5) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.382(4) . ? C36 C37 1.384(3) . ? C37 C38 1.375(4) . ? C37 H37 0.9300 . ? C38 C39 1.362(4) . ? C38 H38 0.9300 . ? C39 C40 1.374(5) . ? C39 H39 0.9300 . ? C40 C41 1.387(4) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C47 1.378(4) . ? C42 C43 1.393(4) . ? C43 C44 1.381(4) . ? C43 H43 0.9300 . ? C44 C45 1.366(5) . ? C44 H44 0.9300 . ? C45 C46 1.373(5) . ? C45 H45 0.9300 . ? C46 C47 1.386(4) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C53 1.386(3) . ? C48 C49 1.393(3) . ? C49 C50 1.379(4) . ? C49 H49 0.9300 . ? C50 C51 1.373(4) . ? C50 H50 0.9300 . ? C51 C52 1.388(4) . ? C51 H51 0.9300 . ? C52 C53 1.376(4) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 C59 1.378(4) . ? C54 C55 1.393(3) . ? C55 C56 1.382(4) . ? C55 H55 0.9300 . ? C56 C57 1.361(4) . ? C56 H56 0.9300 . ? C57 C58 1.379(4) . ? C57 H57 0.9300 . ? C58 C59 1.373(4) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 C61 1.386(4) . ? C60 C65 1.389(4) . ? C61 C62 1.379(4) . ? C61 H61 0.9300 . ? C62 C63 1.358(6) . ? C62 H62 0.9300 . ? C63 C64 1.372(6) . ? C63 H63 0.9300 . ? C64 C65 1.400(5) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? 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 O1 Ru1 O2 175.45(7) . . ? O1 Ru1 C3 91.19(9) . . ? O2 Ru1 C3 93.19(9) . . ? O1 Ru1 N1 94.61(8) . . ? O2 Ru1 N1 81.08(7) . . ? C3 Ru1 N1 173.61(9) . . ? O1 Ru1 C1 90.58(9) . . ? O2 Ru1 C1 90.86(9) . . ? C3 Ru1 C1 87.30(9) . . ? N1 Ru1 C1 89.95(8) . . ? O1 Ru1 C2 89.22(8) . . ? O2 Ru1 C2 89.37(8) . . ? C3 Ru1 C2 92.28(9) . . ? N1 Ru1 C2 90.49(8) . . ? C1 Ru1 C2 179.53(9) . . ? C42 P1 C54 108.14(11) . . ? C42 P1 C48 109.98(11) . . ? C54 P1 C48 109.60(11) . . ? C42 P1 C60 108.62(12) . . ? C54 P1 C60 111.10(12) . . ? C48 P1 C60 109.38(11) . . ? C23 P2 C30 110.42(11) . . ? C23 P2 C24 110.67(12) . . ? C30 P2 C24 107.69(13) . . ? C23 P2 C36 109.10(12) . . ? C30 P2 C36 109.83(12) . . ? C24 P2 C36 109.11(11) . . ? C4 O1 Ru1 123.15(15) . . ? C17 O2 Ru1 112.55(14) . . ? C10 N1 C12 125.2(2) . . ? C10 N1 Ru1 122.72(18) . . ? C12 N1 Ru1 111.52(15) . . ? N2 C1 Ru1 179.3(3) . . ? N3 C2 Ru1 177.7(2) . . ? N4 C3 Ru1 177.0(2) . . ? O1 C4 C5 115.4(2) . . ? O1 C4 C9 126.5(2) . . ? C5 C4 C9 118.0(2) . . ? C6 C5 C4 121.7(2) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 120.3(2) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 119.8(2) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 122.6(2) . . ? C7 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C8 C9 C4 117.5(2) . . ? C8 C9 C10 116.1(2) . . ? C4 C9 C10 126.3(2) . . ? N1 C10 C9 123.4(2) . . ? N1 C10 C11 119.3(2) . . ? C9 C10 C11 117.3(2) . . ? N5 C11 C10 172.1(3) . . ? C13 C12 C17 119.5(2) . . ? C13 C12 N1 128.2(2) . . ? C17 C12 N1 111.9(2) . . ? C14 C13 C12 120.9(2) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 119.4(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.4(2) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 121.1(2) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? O2 C17 C16 120.0(2) . . ? O2 C17 C12 121.5(2) . . ? C16 C17 C12 118.5(2) . . ? C23 C18 C19 119.0(3) . . ? C23 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C18 C23 C22 119.8(3) . . ? C18 C23 P2 120.0(2) . . ? C22 C23 P2 120.2(2) . . ? C25 C24 C29 119.3(3) . . ? C25 C24 P2 120.1(2) . . ? C29 C24 P2 120.4(2) . . ? C24 C25 C26 119.1(3) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 120.8(3) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.3(4) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C24 120.2(3) . . ? C28 C29 H29 119.9 . . ? C24 C29 H29 119.9 . . ? C35 C30 C31 120.4(3) . . ? C35 C30 P2 120.1(2) . . ? C31 C30 P2 119.5(2) . . ? C30 C31 C32 119.4(3) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C33 C32 C31 119.9(4) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C34 C33 C32 120.6(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 120.8(4) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C30 C35 C34 118.9(3) . . ? C30 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C41 C36 C37 119.6(2) . . ? C41 C36 P2 120.6(2) . . ? C37 C36 P2 119.9(2) . . ? C38 C37 C36 120.2(3) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C39 C38 C37 120.2(3) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 120.3(3) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C41 120.1(3) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C36 C41 C40 119.5(3) . . ? C36 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C47 C42 C43 119.3(2) . . ? C47 C42 P1 120.82(19) . . ? C43 C42 P1 119.7(2) . . ? C44 C43 C42 120.4(3) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 119.6(3) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 120.7(3) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C45 C46 C47 120.1(3) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C42 C47 C46 119.9(3) . . ? C42 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C53 C48 C49 119.8(2) . . ? C53 C48 P1 119.96(18) . . ? C49 C48 P1 120.15(19) . . ? C50 C49 C48 119.4(2) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C51 C50 C49 120.6(2) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C52 120.2(3) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C53 C52 C51 119.5(3) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C52 C53 C48 120.4(2) . . ? C52 C53 H53 119.8 . . ? C48 C53 H53 119.8 . . ? C59 C54 C55 119.9(2) . . ? C59 C54 P1 120.38(19) . . ? C55 C54 P1 119.74(19) . . ? C56 C55 C54 119.4(2) . . ? C56 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? C57 C56 C55 120.5(3) . . ? C57 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C56 C57 C58 119.8(3) . . ? C56 C57 H57 120.1 . . ? C58 C57 H57 120.1 . . ? C59 C58 C57 120.8(3) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C58 C59 C54 119.5(3) . . ? C58 C59 H59 120.2 . . ? C54 C59 H59 120.2 . . ? C61 C60 C65 119.9(3) . . ? C61 C60 P1 120.1(2) . . ? C65 C60 P1 119.8(2) . . ? C62 C61 C60 119.8(3) . . ? C62 C61 H61 120.1 . . ? C60 C61 H61 120.1 . . ? C63 C62 C61 120.6(4) . . ? C63 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C62 C63 C64 120.6(3) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C63 C64 C65 120.1(4) . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? C60 C65 C64 118.9(3) . . ? C60 C65 H65 120.5 . . ? C64 C65 H65 120.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.911 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.046 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 365 71 ' ' 2 0.500 0.500 0.500 365 71 ' ' _platon_squeeze_details ; ; #================================================================= data_3 _database_code_depnum_ccdc_archive 'CCDC 764143' #TrackingRef 'Compounds_1-41.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 Mn N5 O7 Ru' _chemical_formula_weight 630.50 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' Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3995(9) _cell_length_b 10.7092(9) _cell_length_c 13.0677(13) _cell_angle_alpha 73.171(8) _cell_angle_beta 79.489(8) _cell_angle_gamma 76.269(7) _cell_volume 1343.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5628 _cell_measurement_theta_min 3.6392 _cell_measurement_theta_max 27.9345 _exptl_crystal_description cube _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99347 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8165 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _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 3.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4722 _reflns_number_gt 3842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material WINGX _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. The substitutional disorder of the tridentate ligand has been fixed by split model. Restraints on displacement parameters such as ISOR and DELU have been applied to make the ADPs of those disordered atoms arriving at more appropriate values. The disordered methyl groups of coordinated methanol molecules have also been fixed using split model by applying restraints such as ISOR and DFIX. ; _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^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4722 _refine_ls_number_parameters 505 _refine_ls_number_restraints 310 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0459 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.834913(16) 0.714911(16) 0.687329(14) 0.01558(6) Uani 1 1 d . . . Mn1 Mn 0.84719(3) 1.21408(3) 0.67672(3) 0.01637(8) Uani 1 1 d . A . O1 O 0.96318(15) 0.66837(15) 0.79125(12) 0.0289(4) Uani 1 1 d . A . O2 O 0.69323(14) 0.76285(14) 0.58862(13) 0.0268(4) Uani 1 1 d . A . O3 O 1.05287(14) 1.12296(14) 0.71920(13) 0.0293(4) Uani 1 1 d D . . H3O H 1.1006 1.1809 0.6881 0.035 Uiso 1 1 d R B . O4 O 0.63615(14) 1.28972(14) 0.65793(14) 0.0324(4) Uani 1 1 d D . . H4O H 0.5944 1.2277 0.6921 0.039 Uiso 1 1 d R B . O5 O 0.78571(18) 1.16677(16) 0.85577(13) 0.0410(4) Uani 1 1 d D . . H5O H 0.7089 1.2134 0.8676 0.049 Uiso 1 1 d R B . O6 O 0.44073(18) 0.15749(18) 0.73524(17) 0.0586(6) Uani 1 1 d . . . H6O H 0.3740 0.1833 0.7000 0.070 Uiso 1 1 d R . . O7 O 0.76455(14) 0.72411(15) 0.38892(13) 0.0295(4) Uani 1 1 d . . . H7O H 0.7405 0.7435 0.4491 0.035 Uiso 1 1 d R . . N3 N 0.80827(18) 1.02127(18) 0.68155(16) 0.0265(5) Uani 1 1 d . . . N4 N 0.86073(17) 1.40836(17) 0.69291(15) 0.0231(4) Uani 1 1 d . . . N5 N 0.93796(18) 1.25626(17) 0.50993(15) 0.0232(4) Uani 1 1 d . . . N1B N 0.7123(5) 0.6926(5) 0.8361(5) 0.0178(10) Uani 0.40 1 d PU A 1 N2B N 0.4317(9) 0.6499(8) 1.0256(7) 0.057(2) Uani 0.40 1 d PU A 1 C1B C 0.9275(15) 0.679(5) 0.890(2) 0.022(3) Uani 0.40 1 d PU A 1 C2B C 1.0063(16) 0.677(3) 0.9627(18) 0.028(3) Uani 0.40 1 d PU A 1 H2BA H 1.0983 0.6777 0.9404 0.033 Uiso 0.40 1 calc PR A 1 C3B C 0.9544(11) 0.673(2) 1.0708(11) 0.036(3) Uani 0.40 1 d PU A 1 H3BA H 1.0122 0.6595 1.1231 0.043 Uiso 0.40 1 calc PR A 1 C4B C 0.8171(9) 0.6886(16) 1.0995(9) 0.042(3) Uani 0.40 1 d PU A 1 H4BA H 0.7798 0.6972 1.1697 0.050 Uiso 0.40 1 calc PR A 1 C5B C 0.7349(9) 0.6921(15) 1.0267(8) 0.032(2) Uani 0.40 1 d PU A 1 H5BA H 0.6414 0.7023 1.0476 0.039 Uiso 0.40 1 calc PR A 1 C6B C 0.7865(11) 0.681(3) 0.9230(10) 0.019(2) Uani 0.40 1 d PU A 1 C7B C 0.5029(7) 0.6659(8) 0.9486(6) 0.0353(16) Uani 0.40 1 d PU A 1 C8B C 0.5877(6) 0.6850(5) 0.8434(5) 0.0202(9) Uani 0.40 1 d PU A 1 C9B C 0.5658(18) 0.743(3) 0.6464(9) 0.020(2) Uani 0.40 1 d PU A 1 C10B C 0.472(3) 0.782(4) 0.5633(17) 0.026(3) Uani 0.40 1 d PU A 1 H10A H 0.5010 0.8240 0.4908 0.031 Uiso 0.40 1 calc PR A 1 C11B C 0.3483(12) 0.7582(19) 0.5912(8) 0.026(2) Uani 0.40 1 d PU A 1 H11A H 0.2905 0.7802 0.5373 0.031 Uiso 0.40 1 calc PR A 1 C12B C 0.3023(10) 0.7015(16) 0.6984(10) 0.030(2) Uani 0.40 1 d PU A 1 H12A H 0.2151 0.6823 0.7168 0.036 Uiso 0.40 1 calc PR A 1 C13B C 0.3832(9) 0.6740(12) 0.7759(8) 0.0269(17) Uani 0.40 1 d PU A 1 H13A H 0.3492 0.6375 0.8483 0.032 Uiso 0.40 1 calc PR A 1 C14B C 0.5165(12) 0.697(2) 0.7548(8) 0.0215(16) Uani 0.40 1 d PU A 1 N1A N 0.6651(4) 0.7005(4) 0.7946(3) 0.0215(7) Uani 0.60 1 d PU A 2 N2A N 0.4426(6) 0.7246(6) 1.0220(5) 0.0624(16) Uani 0.60 1 d PU A 2 C1A C 0.9137(11) 0.672(3) 0.8926(16) 0.0211(17) Uani 0.60 1 d PU A 2 C2A C 1.0212(12) 0.661(2) 0.9528(11) 0.0307(18) Uani 0.60 1 d PU A 2 H2AA H 1.1108 0.6413 0.9209 0.037 Uiso 0.60 1 calc PR A 2 C3A C 0.9965(7) 0.6774(13) 1.0543(7) 0.0389(18) Uani 0.60 1 d PU A 2 H3AA H 1.0681 0.6756 1.0911 0.047 Uiso 0.60 1 calc PR A 2 C4A C 0.8687(9) 0.6966(10) 1.1031(6) 0.0458(16) Uani 0.60 1 d PU A 2 H4AA H 0.8524 0.7063 1.1746 0.055 Uiso 0.60 1 calc PR A 2 C5A C 0.7646(7) 0.7021(9) 1.0526(5) 0.0387(14) Uani 0.60 1 d PU A 2 H5AA H 0.6775 0.7109 1.0910 0.046 Uiso 0.60 1 calc PR A 2 C6A C 0.7812(8) 0.6952(19) 0.9429(8) 0.0273(17) Uani 0.60 1 d PU A 2 C7A C 0.6664(4) 0.6985(4) 0.8936(4) 0.0252(8) Uani 0.60 1 d PU A 2 C8A C 0.5387(5) 0.7098(5) 0.9653(4) 0.0391(12) Uani 0.60 1 d PU A 2 C9A C 0.5736(13) 0.750(2) 0.6278(5) 0.0195(15) Uani 0.60 1 d PU A 2 C10A C 0.471(2) 0.765(2) 0.5711(12) 0.031(2) Uani 0.60 1 d PU A 2 H10B H 0.4833 0.7974 0.4950 0.037 Uiso 0.60 1 calc PR A 2 C11A C 0.3481(10) 0.7322(13) 0.6219(7) 0.0381(19) Uani 0.60 1 d PU A 2 H11B H 0.2772 0.7455 0.5807 0.046 Uiso 0.60 1 calc PR A 2 C12A C 0.3311(7) 0.6814(9) 0.7307(6) 0.0387(15) Uani 0.60 1 d PU A 2 H12B H 0.2498 0.6545 0.7652 0.046 Uiso 0.60 1 calc PR A 2 C13A C 0.4311(7) 0.6689(9) 0.7907(5) 0.0304(13) Uani 0.60 1 d PU A 2 H13B H 0.4181 0.6334 0.8665 0.036 Uiso 0.60 1 calc PR A 2 C14A C 0.5515(7) 0.7076(15) 0.7421(5) 0.0231(12) Uani 0.60 1 d PU A 2 C15 C 0.8534(2) 0.5175(2) 0.69118(17) 0.0199(5) Uani 1 1 d . . . C16 C 0.9805(2) 0.73320(19) 0.56260(17) 0.0178(5) Uani 1 1 d . . . C17 C 0.8151(2) 0.9128(2) 0.68246(17) 0.0195(5) Uani 1 1 d . A . C18A C 1.1232(10) 1.0017(7) 0.6865(6) 0.0406(18) Uani 0.65 1 d PDU B 1 H18A H 1.2132 0.9759 0.7079 0.061 Uiso 0.65 1 calc PR B 1 H18B H 1.1289 1.0186 0.6081 0.061 Uiso 0.65 1 calc PR B 1 H18C H 1.0742 0.9297 0.7216 0.061 Uiso 0.65 1 calc PR B 1 C18B C 1.118(2) 0.9888(15) 0.7297(11) 0.047(4) Uani 0.35 1 d PDU B 2 H18D H 1.0760 0.9323 0.7942 0.071 Uiso 0.35 1 calc PR B 2 H18E H 1.2122 0.9795 0.7362 0.071 Uiso 0.35 1 calc PR B 2 H18F H 1.1100 0.9615 0.6660 0.071 Uiso 0.35 1 calc PR B 2 C19A C 0.5524(9) 1.4112(8) 0.6690(6) 0.0441(19) Uani 0.65 1 d PDU B 1 H19A H 0.5979 1.4849 0.6305 0.066 Uiso 0.65 1 calc PR B 1 H19B H 0.5319 1.4099 0.7455 0.066 Uiso 0.65 1 calc PR B 1 H19C H 0.4695 1.4229 0.6387 0.066 Uiso 0.65 1 calc PR B 1 C19B C 0.5611(17) 1.4211(14) 0.6254(9) 0.034(3) Uani 0.35 1 d PDU B 2 H19D H 0.4802 1.4321 0.6763 0.051 Uiso 0.35 1 calc PR B 2 H19E H 0.5366 1.4363 0.5532 0.051 Uiso 0.35 1 calc PR B 2 H19F H 0.6150 1.4853 0.6241 0.051 Uiso 0.35 1 calc PR B 2 C20A C 0.8417(8) 1.0492(10) 0.9325(8) 0.053(2) Uani 0.65 1 d PDU B 1 H20A H 0.8300 1.0674 1.0033 0.079 Uiso 0.65 1 calc PR B 1 H20B H 0.9370 1.0230 0.9093 0.079 Uiso 0.65 1 calc PR B 1 H20C H 0.7963 0.9769 0.9373 0.079 Uiso 0.65 1 calc PR B 1 C20B C 0.7929(16) 1.0513(18) 0.9396(16) 0.057(5) Uani 0.35 1 d PDU B 2 H20D H 0.8534 0.9777 0.9148 0.086 Uiso 0.35 1 calc PR B 2 H20E H 0.7039 1.0298 0.9631 0.086 Uiso 0.35 1 calc PR B 2 H20F H 0.8265 1.0650 1.0001 0.086 Uiso 0.35 1 calc PR B 2 C21 C 0.4480(3) 0.0297(3) 0.7936(3) 0.0856(13) Uani 1 1 d . . . H21A H 0.5168 0.0065 0.8418 0.128 Uiso 1 1 calc R . . H21B H 0.4707 -0.0290 0.7450 0.128 Uiso 1 1 calc R . . H21C H 0.3617 0.0189 0.8364 0.128 Uiso 1 1 calc R . . C22 C 0.8051(2) 0.5819(2) 0.4100(2) 0.0352(6) Uani 1 1 d . . . H22A H 0.8809 0.5519 0.4519 0.053 Uiso 1 1 calc R . . H22B H 0.8314 0.5569 0.3416 0.053 Uiso 1 1 calc R . . H22C H 0.7307 0.5400 0.4508 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01723(10) 0.01244(9) 0.01814(10) -0.00655(7) 0.00210(7) -0.00497(6) Mn1 0.01882(18) 0.01219(16) 0.01918(19) -0.00686(14) 0.00224(14) -0.00506(13) O1 0.0367(10) 0.0307(9) 0.0189(9) -0.0106(7) -0.0068(7) 0.0024(7) O2 0.0184(9) 0.0245(9) 0.0403(10) -0.0107(8) -0.0060(7) -0.0049(6) O3 0.0237(9) 0.0227(9) 0.0395(11) -0.0054(8) -0.0029(7) -0.0045(7) O4 0.0204(9) 0.0215(9) 0.0548(12) -0.0103(8) -0.0020(8) -0.0045(7) O5 0.0550(12) 0.0363(10) 0.0225(10) -0.0036(8) 0.0074(8) -0.0055(8) O6 0.0340(11) 0.0527(13) 0.0772(16) 0.0196(11) -0.0216(11) -0.0192(9) O7 0.0255(9) 0.0336(9) 0.0270(10) -0.0049(8) -0.0025(7) -0.0053(7) N3 0.0295(11) 0.0180(11) 0.0350(12) -0.0118(9) 0.0017(9) -0.0087(8) N4 0.0272(11) 0.0147(10) 0.0294(12) -0.0076(9) -0.0034(9) -0.0052(8) N5 0.0247(10) 0.0245(10) 0.0210(11) -0.0075(8) 0.0025(9) -0.0077(8) N1B 0.0213(18) 0.013(2) 0.018(3) -0.009(3) 0.0003(18) 0.002(2) N2B 0.049(4) 0.082(6) 0.033(3) -0.009(4) 0.013(2) -0.019(4) C1B 0.027(3) 0.017(9) 0.018(4) 0.002(5) -0.003(3) -0.007(5) C2B 0.026(3) 0.028(7) 0.030(5) -0.014(4) -0.007(2) 0.002(4) C3B 0.032(4) 0.049(6) 0.028(4) -0.015(5) -0.011(4) 0.005(5) C4B 0.034(4) 0.072(6) 0.021(3) -0.016(4) -0.006(3) -0.005(5) C5B 0.031(3) 0.049(5) 0.017(3) -0.009(4) -0.003(2) -0.008(4) C6B 0.028(2) 0.012(5) 0.021(4) -0.010(4) -0.0004(19) -0.006(3) C7B 0.026(3) 0.050(5) 0.028(2) -0.011(3) 0.003(2) -0.007(3) C8B 0.0210(18) 0.011(2) 0.0247(19) -0.002(2) -0.0013(14) 0.000(2) C9B 0.013(4) 0.021(6) 0.028(2) -0.008(5) -0.004(3) -0.001(4) C10B 0.014(4) 0.033(8) 0.032(3) -0.015(4) -0.006(3) 0.001(4) C11B 0.012(3) 0.035(7) 0.029(3) -0.012(4) -0.005(3) 0.004(3) C12B 0.020(3) 0.039(5) 0.030(4) -0.013(4) -0.003(2) 0.001(4) C13B 0.018(4) 0.031(4) 0.027(3) -0.004(3) -0.001(2) -0.001(5) C14B 0.022(4) 0.015(5) 0.029(2) -0.010(3) 0.000(2) -0.004(5) N1A 0.0263(18) 0.0153(16) 0.0218(14) -0.0063(16) 0.0015(13) -0.0034(16) N2A 0.047(2) 0.092(4) 0.037(3) -0.023(3) 0.0140(18) 0.002(3) C1A 0.0371(18) 0.012(4) 0.019(3) -0.005(4) -0.005(2) -0.009(5) C2A 0.043(2) 0.027(6) 0.028(3) -0.008(3) -0.012(2) -0.010(4) C3A 0.053(3) 0.048(4) 0.022(3) -0.004(3) -0.015(3) -0.019(4) C4A 0.059(4) 0.060(4) 0.023(2) -0.011(3) -0.008(2) -0.017(5) C5A 0.046(3) 0.049(3) 0.025(3) -0.016(4) 0.001(2) -0.013(4) C6A 0.0389(16) 0.020(5) 0.025(3) -0.011(3) -0.0033(16) -0.004(2) C7A 0.0335(14) 0.019(2) 0.0230(16) -0.0091(19) 0.0019(11) -0.0050(18) C8A 0.0372(17) 0.050(3) 0.025(2) -0.012(2) 0.0056(16) -0.004(2) C9A 0.026(3) 0.012(4) 0.0233(18) -0.012(3) 0.0018(18) -0.001(3) C10A 0.032(3) 0.030(6) 0.032(2) -0.013(3) -0.006(2) -0.001(3) C11A 0.028(3) 0.037(5) 0.051(4) -0.013(4) -0.012(3) -0.002(3) C12A 0.017(3) 0.042(4) 0.052(4) -0.013(4) 0.002(2) 0.000(3) C13A 0.029(3) 0.035(3) 0.032(2) -0.019(2) 0.009(2) -0.012(4) C14A 0.026(3) 0.020(3) 0.0246(19) -0.009(2) 0.0036(16) -0.008(3) C15 0.0171(11) 0.0213(12) 0.0224(13) -0.0082(10) 0.0001(9) -0.0049(9) C16 0.0222(12) 0.0123(11) 0.0215(13) -0.0064(9) -0.0043(10) -0.0044(9) C17 0.0185(12) 0.0231(12) 0.0190(12) -0.0096(10) 0.0024(9) -0.0064(9) C18A 0.030(3) 0.022(3) 0.066(5) -0.012(3) -0.011(4) 0.007(2) C18B 0.039(6) 0.039(6) 0.061(9) -0.005(6) -0.018(7) -0.005(4) C19A 0.029(3) 0.029(3) 0.070(5) -0.010(4) -0.010(4) 0.003(2) C19B 0.031(5) 0.028(5) 0.042(7) -0.008(5) -0.001(6) -0.005(4) C20A 0.063(5) 0.053(3) 0.026(3) 0.009(2) 0.004(4) -0.013(4) C20B 0.065(9) 0.053(6) 0.051(7) -0.005(5) -0.005(7) -0.018(7) C21 0.056(2) 0.046(2) 0.128(4) 0.029(2) -0.020(2) -0.0138(16) C22 0.0369(15) 0.0331(14) 0.0332(16) -0.0032(12) -0.0035(12) -0.0096(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 1.9559(15) . ? Ru1 C16 2.010(2) . ? Ru1 O2 2.0123(15) . ? Ru1 N1A 2.051(4) . ? Ru1 C17 2.063(2) . ? Ru1 C15 2.063(2) . ? Ru1 N1B 2.106(6) . ? Mn1 N5 2.1741(19) . ? Mn1 N3 2.1780(17) . ? Mn1 O4 2.1842(15) . ? Mn1 N4 2.1905(17) . ? Mn1 O3 2.2281(15) . ? Mn1 O5 2.2499(16) . ? O1 C1B 1.30(2) . ? O1 C1A 1.340(15) . ? O2 C9A 1.278(10) . ? O2 C9B 1.431(14) . ? O3 C18B 1.413(14) . ? O3 C18A 1.470(7) . ? O3 H3O 0.8501 . ? O4 C19A 1.413(7) . ? O4 C19B 1.422(13) . ? O4 H4O 0.8500 . ? O5 C20B 1.392(15) . ? O5 C20A 1.437(8) . ? O5 H5O 0.8500 . ? O6 C21 1.352(3) . ? O6 H6O 0.8500 . ? O7 C22 1.438(3) . ? O7 H7O 0.8501 . ? N3 C17 1.144(2) . ? N4 C15 1.147(2) 1_565 ? N5 C16 1.149(3) 2_776 ? N1B C8B 1.302(8) . ? N1B C6B 1.447(10) . ? N2B C7B 1.131(10) . ? C1B C2B 1.36(3) . ? C1B C6B 1.448(18) . ? C2B C3B 1.409(15) . ? C2B H2BA 0.9500 . ? C3B C4B 1.391(12) . ? C3B H3BA 0.9500 . ? C4B C5B 1.379(10) . ? C4B H4BA 0.9500 . ? C5B C6B 1.391(10) . ? C5B H5BA 0.9500 . ? C7B C8B 1.480(9) . ? C8B C14B 1.444(10) . ? C9B C14B 1.400(12) . ? C9B C10B 1.49(3) . ? C10B C11B 1.34(2) . ? C10B H10A 0.9500 . ? C11B C12B 1.401(12) . ? C11B H11A 0.9500 . ? C12B C13B 1.356(11) . ? C12B H12A 0.9500 . ? C13B C14B 1.429(11) . ? C13B H13A 0.9500 . ? N1A C7A 1.291(5) . ? N1A C14A 1.448(6) . ? N2A C8A 1.138(7) . ? C1A C6A 1.412(12) . ? C1A C2A 1.442(17) . ? C2A C3A 1.360(11) . ? C2A H2AA 0.9500 . ? C3A C4A 1.361(8) . ? C3A H3AA 0.9500 . ? C4A C5A 1.347(8) . ? C4A H4AA 0.9500 . ? C5A C6A 1.434(7) . ? C5A H5AA 0.9500 . ? C6A C7A 1.444(8) . ? C7A C8A 1.481(6) . ? C9A C10A 1.36(2) . ? C9A C14A 1.421(8) . ? C10A C11A 1.401(16) . ? C10A H10B 0.9500 . ? C11A C12A 1.362(9) . ? C11A H11B 0.9500 . ? C12A C13A 1.373(7) . ? C12A H12B 0.9500 . ? C13A C14A 1.395(7) . ? C13A H13B 0.9500 . ? C15 N4 1.147(2) 1_545 ? C16 N5 1.149(3) 2_776 ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 O1 Ru1 C16 91.73(8) . . ? O1 Ru1 O2 176.20(6) . . ? C16 Ru1 O2 92.05(7) . . ? O1 Ru1 N1A 98.24(12) . . ? C16 Ru1 N1A 169.95(13) . . ? O2 Ru1 N1A 77.99(12) . . ? O1 Ru1 C17 89.24(7) . . ? C16 Ru1 C17 90.03(8) . . ? O2 Ru1 C17 90.38(7) . . ? N1A Ru1 C17 91.38(11) . . ? O1 Ru1 C15 91.31(7) . . ? C16 Ru1 C15 89.98(8) . . ? O2 Ru1 C15 89.07(7) . . ? N1A Ru1 C15 88.52(11) . . ? C17 Ru1 C15 179.45(9) . . ? O1 Ru1 N1B 77.15(17) . . ? C16 Ru1 N1B 168.74(17) . . ? O2 Ru1 N1B 99.06(17) . . ? N1A Ru1 N1B 21.31(13) . . ? C17 Ru1 N1B 88.12(15) . . ? C15 Ru1 N1B 91.99(16) . . ? N5 Mn1 N3 95.76(7) . . ? N5 Mn1 O4 101.39(7) . . ? N3 Mn1 O4 85.75(6) . . ? N5 Mn1 N4 92.55(7) . . ? N3 Mn1 N4 170.93(7) . . ? O4 Mn1 N4 89.06(6) . . ? N5 Mn1 O3 86.30(7) . . ? N3 Mn1 O3 91.61(6) . . ? O4 Mn1 O3 172.07(6) . . ? N4 Mn1 O3 92.54(6) . . ? N5 Mn1 O5 171.00(7) . . ? N3 Mn1 O5 87.35(7) . . ? O4 Mn1 O5 87.25(7) . . ? N4 Mn1 O5 84.97(6) . . ? O3 Mn1 O5 85.16(6) . . ? C1B O1 C1A 7(2) . . ? C1B O1 Ru1 122.1(9) . . ? C1A O1 Ru1 116.9(6) . . ? C9A O2 C9B 7.8(9) . . ? C9A O2 Ru1 119.8(4) . . ? C9B O2 Ru1 112.1(6) . . ? C18B O3 C18A 21.4(7) . . ? C18B O3 Mn1 126.8(9) . . ? C18A O3 Mn1 118.9(4) . . ? C18B O3 H3O 116.0 . . ? C18A O3 H3O 105.4 . . ? Mn1 O3 H3O 106.4 . . ? C19A O4 C19B 22.1(6) . . ? C19A O4 Mn1 130.6(4) . . ? C19B O4 Mn1 132.0(8) . . ? C19A O4 H4O 107.5 . . ? C19B O4 H4O 118.3 . . ? Mn1 O4 H4O 107.6 . . ? C20B O5 C20A 20.1(9) . . ? C20B O5 Mn1 135.3(10) . . ? C20A O5 Mn1 125.2(4) . . ? C20B O5 H5O 105.7 . . ? C20A O5 H5O 123.4 . . ? Mn1 O5 H5O 108.2 . . ? C21 O6 H6O 111.0 . . ? C22 O7 H7O 108.0 . . ? C17 N3 Mn1 166.25(17) . . ? C15 N4 Mn1 169.73(17) 1_565 . ? C16 N5 Mn1 159.34(18) 2_776 . ? C8B N1B C6B 127.4(7) . . ? C8B N1B Ru1 121.2(5) . . ? C6B N1B Ru1 111.3(6) . . ? O1 C1B C2B 128.2(13) . . ? O1 C1B C6B 112.4(14) . . ? C2B C1B C6B 119.1(18) . . ? C1B C2B C3B 121.4(16) . . ? C1B C2B H2BA 119.3 . . ? C3B C2B H2BA 119.3 . . ? C4B C3B C2B 118.9(10) . . ? C4B C3B H3BA 120.6 . . ? C2B C3B H3BA 120.6 . . ? C5B C4B C3B 120.3(8) . . ? C5B C4B H4BA 119.8 . . ? C3B C4B H4BA 119.8 . . ? C4B C5B C6B 121.1(8) . . ? C4B C5B H5BA 119.4 . . ? C6B C5B H5BA 119.4 . . ? C5B C6B N1B 127.2(9) . . ? C5B C6B C1B 118.4(12) . . ? N1B C6B C1B 113.6(11) . . ? N2B C7B C8B 175.3(8) . . ? N1B C8B C14B 126.0(7) . . ? N1B C8B C7B 121.0(6) . . ? C14B C8B C7B 113.0(6) . . ? O2 C9B C14B 135.4(12) . . ? O2 C9B C10B 105.8(11) . . ? C14B C9B C10B 118.8(14) . . ? C11B C10B C9B 119.9(15) . . ? C11B C10B H10A 120.1 . . ? C9B C10B H10A 120.1 . . ? C10B C11B C12B 121.1(12) . . ? C10B C11B H11A 119.5 . . ? C12B C11B H11A 119.5 . . ? C13B C12B C11B 119.5(8) . . ? C13B C12B H12A 120.2 . . ? C11B C12B H12A 120.2 . . ? C12B C13B C14B 123.7(8) . . ? C12B C13B H13A 118.1 . . ? C14B C13B H13A 118.1 . . ? C9B C14B C13B 116.4(9) . . ? C9B C14B C8B 123.6(9) . . ? C13B C14B C8B 119.8(9) . . ? C7A N1A C14A 127.9(5) . . ? C7A N1A Ru1 119.9(4) . . ? C14A N1A Ru1 111.9(3) . . ? O1 C1A C6A 131.4(11) . . ? O1 C1A C2A 109.6(9) . . ? C6A C1A C2A 118.8(11) . . ? C3A C2A C1A 121.2(10) . . ? C3A C2A H2AA 119.4 . . ? C1A C2A H2AA 119.4 . . ? C2A C3A C4A 119.6(7) . . ? C2A C3A H3AA 120.2 . . ? C4A C3A H3AA 120.2 . . ? C5A C4A C3A 121.8(5) . . ? C5A C4A H4AA 119.1 . . ? C3A C4A H4AA 119.1 . . ? C4A C5A C6A 122.1(6) . . ? C4A C5A H5AA 118.9 . . ? C6A C5A H5AA 118.9 . . ? C1A C6A C5A 116.3(9) . . ? C1A C6A C7A 123.7(7) . . ? C5A C6A C7A 119.8(7) . . ? N1A C7A C6A 126.6(5) . . ? N1A C7A C8A 119.0(4) . . ? C6A C7A C8A 114.3(5) . . ? N2A C8A C7A 175.8(6) . . ? O2 C9A C10A 126.5(9) . . ? O2 C9A C14A 115.0(8) . . ? C10A C9A C14A 118.3(9) . . ? C9A C10A C11A 121.9(11) . . ? C9A C10A H10B 119.0 . . ? C11A C10A H10B 119.0 . . ? C12A C11A C10A 119.4(9) . . ? C12A C11A H11B 120.3 . . ? C10A C11A H11B 120.3 . . ? C11A C12A C13A 120.2(6) . . ? C11A C12A H12B 119.9 . . ? C13A C12A H12B 119.9 . . ? C12A C13A C14A 121.0(5) . . ? C12A C13A H13B 119.5 . . ? C14A C13A H13B 119.5 . . ? C13A C14A C9A 118.8(6) . . ? C13A C14A N1A 127.2(5) . . ? C9A C14A N1A 113.9(5) . . ? N4 C15 Ru1 178.46(18) 1_545 . ? N5 C16 Ru1 178.75(19) 2_776 . ? N3 C17 Ru1 177.47(19) . . ? O3 C18A H18A 109.5 . . ? O3 C18A H18B 109.5 . . ? O3 C18A H18C 109.5 . . ? O3 C18B H18D 109.5 . . ? O3 C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? O3 C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? O4 C19A H19A 109.5 . . ? O4 C19A H19B 109.5 . . ? O4 C19A H19C 109.5 . . ? O4 C19B H19D 109.5 . . ? O4 C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? O4 C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? O5 C20A H20A 109.5 . . ? O5 C20A H20B 109.5 . . ? O5 C20A H20C 109.5 . . ? O5 C20B H20D 109.5 . . ? O5 C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? O5 C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? O6 C21 H21A 109.5 . . ? O6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O7 C22 H22A 109.5 . . ? O7 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O7 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.448 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.055 #================================================================= data_4 _database_code_depnum_ccdc_archive 'CCDC 764144' #TrackingRef 'Compounds_1-41.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 Co N5 O7 Ru' _chemical_formula_weight 634.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2969(6) _cell_length_b 10.5624(8) _cell_length_c 13.0000(11) _cell_angle_alpha 73.227(4) _cell_angle_beta 79.510(5) _cell_angle_gamma 75.456(5) _cell_volume 1301.15(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4731 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details 'SORTAV, (Blessing, 1995)' _exptl_special_details ; According to search higher METRIC symmetry (SHELXTL/XPREP), only Triclinic is less than 0.15 and the spece group of P-1 was choiced. The cocrystallized solvents were lost easily, result that the Rint factor is higher than 0.1. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12825 _diffrn_reflns_av_R_equivalents 0.1235 _diffrn_reflns_av_sigmaI/netI 0.1225 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _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 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4580 _reflns_number_gt 2682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4580 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1364 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2315 _refine_ls_wR_factor_gt 0.1980 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 Ru Ru -0.33887(7) 0.78220(8) 0.81718(6) 0.0328(3) Uani 1 1 d . . . Co Co -0.34732(11) 0.28455(12) 0.82027(10) 0.0310(4) Uani 1 1 d . . . O1 O -0.1954(6) 0.7307(7) 0.9155(6) 0.0467(18) Uani 1 1 d . A . O2 O -0.4689(7) 0.8305(7) 0.7145(5) 0.0433(17) Uani 1 1 d . A . O3 O -0.5464(6) 0.3695(7) 0.7737(6) 0.0434(17) Uani 1 1 d . . . H3 H -0.6070 0.3161 0.8045 0.065 Uiso 1 1 d R . . O4 O -0.1454(6) 0.2084(7) 0.8469(6) 0.0470(18) Uani 1 1 d . . . H4 H -0.1135 0.2700 0.7907 0.070 Uiso 1 1 d R . . O5 O -0.2808(8) 0.3268(7) 0.6499(5) 0.052(2) Uani 1 1 d . . . H5 H -0.2405 0.2723 0.6062 0.079 Uiso 1 1 d R . . N1 N -0.3193(8) 0.4757(9) 0.8175(7) 0.039(2) Uani 1 1 d . . . N2 N -0.5640(8) 0.7523(8) 1.0200(6) 0.0323(17) Uani 1 1 d . . . N3 N -0.3604(8) 1.0930(8) 0.8104(6) 0.0361(18) Uani 1 1 d . . . N4 N -0.174(2) 0.7970(18) 0.7127(14) 0.033(3) Uani 0.50 1 d P A 1 N5 N 0.061(4) 0.787(3) 0.480(3) 0.069(10) Uani 0.50 1 d P A 1 N4' N -0.214(2) 0.8072(18) 0.6639(16) 0.033(3) Uani 0.50 1 d P A 2 N5' N 0.060(4) 0.855(3) 0.476(3) 0.066(10) Uani 0.50 1 d P A 2 C1 C -0.3205(9) 0.5823(10) 0.8218(7) 0.033(2) Uani 1 1 d . A . C2 C -0.4848(9) 0.7637(9) 0.9440(8) 0.031(2) Uani 1 1 d . A . C3 C -0.3556(9) 0.9816(10) 0.8123(7) 0.030(2) Uani 1 1 d . A . C4 C -0.0700(9) 0.7424(10) 0.8700(9) 0.042(2) Uani 1 1 d . . . C5 C 0.0288(10) 0.7171(11) 0.9382(9) 0.047(3) Uani 1 1 d . A . H5A H 0.0092 0.6791 1.0135 0.057 Uiso 1 1 calc R . . C6 C 0.1530(11) 0.7461(14) 0.8985(13) 0.067(4) Uani 1 1 d . . . H6 H 0.2198 0.7258 0.9458 0.080 Uiso 1 1 calc R A . C7 C 0.1820(14) 0.8048(16) 0.7898(14) 0.083(5) Uani 1 1 d . A . H7 H 0.2656 0.8321 0.7638 0.099 Uiso 1 1 calc R . . C8 C 0.0909(16) 0.8239(13) 0.7190(11) 0.073(4) Uani 1 1 d . . . H8 H 0.1136 0.8588 0.6436 0.087 Uiso 1 1 calc R A . C9 C -0.0371(11) 0.7912(11) 0.7591(9) 0.051(3) Uani 1 1 d . A . C10 C -0.2892(10) 0.8118(10) 0.5688(9) 0.045(3) Uani 1 1 d . . . C11 C -0.2545(15) 0.8027(14) 0.4630(12) 0.078(4) Uani 1 1 d . A . H11 H -0.1623 0.7920 0.4330 0.094 Uiso 1 1 calc R . . C12 C -0.3530(19) 0.8089(15) 0.3994(11) 0.082(5) Uani 1 1 d . . . H12 H -0.3280 0.8039 0.3264 0.098 Uiso 1 1 calc R A . C13 C -0.4831(16) 0.8219(13) 0.4422(10) 0.068(4) Uani 1 1 d . A . H13 H -0.5496 0.8233 0.3996 0.081 Uiso 1 1 calc R . . C14 C -0.5209(12) 0.8330(11) 0.5446(9) 0.049(3) Uani 1 1 d . . . H14 H -0.6141 0.8470 0.5716 0.059 Uiso 1 1 calc R A . C15 C -0.4244(10) 0.8244(9) 0.6131(8) 0.038(2) Uani 1 1 d . A . C16 C -0.166(3) 0.803(2) 0.6063(17) 0.040(5) Uani 0.50 1 d P A 1 C17 C -0.038(3) 0.794(4) 0.539(3) 0.046(8) Uani 0.50 1 d P A 1 C16' C -0.096(2) 0.814(2) 0.6593(19) 0.040(5) Uani 0.50 1 d P A 2 C17' C -0.003(3) 0.832(4) 0.556(3) 0.057(9) Uani 0.50 1 d P A 2 C18 C -0.6199(12) 0.4979(12) 0.7915(13) 0.078(4) Uani 1 1 d . . . H18A H -0.6145 0.4997 0.8655 0.117 Uiso 1 1 calc R . . H18B H -0.7147 0.5109 0.7810 0.117 Uiso 1 1 calc R . . H18C H -0.5806 0.5705 0.7400 0.117 Uiso 1 1 calc R . . C19 C -0.0620(13) 0.0818(14) 0.8439(15) 0.098(6) Uani 1 1 d . . . H19A H -0.1037 0.0102 0.8944 0.146 Uiso 1 1 calc R . . H19B H 0.0264 0.0767 0.8647 0.146 Uiso 1 1 calc R . . H19C H -0.0504 0.0701 0.7704 0.146 Uiso 1 1 calc R . . C20 C -0.3196(15) 0.4465(14) 0.5703(10) 0.076(4) Uani 1 1 d . . . H20A H -0.3969 0.5055 0.6010 0.113 Uiso 1 1 calc R . . H20B H -0.3450 0.4246 0.5094 0.113 Uiso 1 1 calc R . . H20C H -0.2440 0.4930 0.5449 0.113 Uiso 1 1 calc R . . O6 O -0.7353(7) 0.2245(7) 0.8834(6) 0.0464(18) Uani 1 1 d . . . H6A H -0.7546 0.2482 0.9416 0.070 Uiso 1 1 calc R . . C21 C -0.6965(11) 0.0790(11) 0.9067(9) 0.050(3) Uani 1 1 d . . . H21A H -0.6720 0.0514 0.8387 0.076 Uiso 1 1 calc R . . H21B H -0.7723 0.0396 0.9490 0.076 Uiso 1 1 calc R . . H21C H -0.6188 0.0473 0.9481 0.076 Uiso 1 1 calc R . . O7 O 0.0544(8) 0.3378(10) 0.7597(7) 0.075(3) Uani 1 1 d . . . H7A H 0.0453 0.3379 0.8253 0.113 Uiso 1 1 calc R . . C22 C 0.0437(14) 0.4649(14) 0.6982(13) 0.087(5) Uani 1 1 d . . . H22A H -0.0375 0.4909 0.6612 0.131 Uiso 1 1 calc R . . H22B H 0.1236 0.4710 0.6445 0.131 Uiso 1 1 calc R . . H22C H 0.0371 0.5261 0.7440 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0259(4) 0.0316(5) 0.0408(5) -0.0106(3) -0.0065(3) -0.0024(3) Co 0.0274(7) 0.0284(7) 0.0373(7) -0.0096(6) -0.0050(5) -0.0037(5) O1 0.029(4) 0.044(4) 0.070(5) -0.015(4) -0.012(3) -0.009(3) O2 0.043(4) 0.041(4) 0.041(4) -0.009(3) -0.014(3) 0.005(3) O3 0.030(3) 0.038(4) 0.062(5) -0.013(3) -0.018(3) 0.002(3) O4 0.028(3) 0.044(4) 0.066(5) -0.011(4) -0.011(3) -0.002(3) O5 0.063(5) 0.047(4) 0.036(4) -0.002(3) -0.003(4) -0.002(4) N1 0.026(4) 0.037(5) 0.048(5) -0.007(4) -0.005(3) 0.003(4) N2 0.028(4) 0.037(5) 0.029(4) -0.004(3) -0.004(3) -0.006(3) N3 0.036(4) 0.032(5) 0.043(5) -0.013(4) -0.008(4) -0.005(3) N4 0.048(10) 0.028(6) 0.016(10) 0.001(7) -0.011(6) 0.000(6) N5 0.055(16) 0.063(19) 0.057(17) -0.011(19) -0.009(13) 0.043(19) N4' 0.048(10) 0.028(6) 0.016(10) 0.001(7) -0.011(6) 0.000(6) N5' 0.056(15) 0.048(16) 0.054(16) 0.023(17) -0.012(12) 0.024(17) C1 0.034(5) 0.029(5) 0.033(5) -0.007(4) -0.005(4) -0.002(4) C2 0.031(5) 0.024(5) 0.042(6) -0.011(4) -0.016(4) -0.002(4) C3 0.029(5) 0.031(5) 0.033(5) -0.006(4) -0.011(4) -0.007(4) C4 0.024(5) 0.041(6) 0.064(7) -0.021(5) -0.007(5) 0.000(4) C5 0.034(5) 0.055(7) 0.056(7) -0.021(5) -0.019(5) 0.000(5) C6 0.023(5) 0.088(10) 0.099(11) -0.046(8) -0.011(6) 0.000(6) C7 0.057(9) 0.090(11) 0.118(14) -0.070(10) 0.026(9) -0.021(8) C8 0.104(12) 0.055(8) 0.059(8) -0.028(7) 0.020(8) -0.023(8) C9 0.052(7) 0.044(6) 0.061(8) -0.020(6) -0.021(6) -0.001(5) C10 0.036(6) 0.035(6) 0.059(7) -0.006(5) -0.010(5) -0.004(4) C11 0.062(8) 0.058(9) 0.090(11) -0.008(8) 0.018(8) -0.001(7) C12 0.126(14) 0.074(10) 0.050(8) -0.025(7) -0.001(9) -0.025(10) C13 0.094(11) 0.063(9) 0.051(8) -0.015(6) -0.044(8) -0.001(7) C14 0.053(6) 0.045(6) 0.055(7) -0.009(5) -0.029(5) -0.009(5) C15 0.052(6) 0.028(5) 0.032(5) 0.000(4) -0.014(5) -0.007(4) C16 0.062(15) 0.035(11) 0.021(12) -0.017(9) 0.008(12) -0.006(10) C17 0.024(14) 0.07(2) 0.043(15) -0.027(14) -0.013(12) 0.016(14) C16' 0.061(14) 0.027(11) 0.039(13) -0.013(10) -0.032(12) 0.003(10) C17' 0.053(19) 0.07(2) 0.042(19) 0.009(16) -0.008(14) -0.026(15) C18 0.044(7) 0.042(7) 0.148(14) -0.026(8) -0.026(8) 0.003(5) C19 0.057(8) 0.059(9) 0.183(17) -0.039(10) -0.055(10) 0.015(7) C20 0.096(11) 0.070(9) 0.048(7) -0.002(6) -0.004(7) -0.012(8) O6 0.030(4) 0.053(5) 0.051(4) -0.008(4) -0.013(3) -0.001(3) C21 0.048(6) 0.044(6) 0.062(7) -0.010(5) -0.013(5) -0.012(5) O7 0.042(4) 0.087(7) 0.077(6) 0.021(5) -0.016(5) -0.023(5) C22 0.060(8) 0.057(9) 0.121(13) 0.011(9) -0.024(8) -0.002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru O2 1.936(7) . ? Ru O1 1.999(7) . ? Ru C2 2.018(10) . ? Ru N4 1.98(2) . ? Ru C3 2.053(10) . ? Ru C1 2.056(10) . ? Ru N4' 2.15(2) . ? Co N2 2.078(8) 2_467 ? Co O4 2.086(6) . ? Co N1 2.100(9) . ? Co N3 2.103(8) 1_545 ? Co O3 2.142(6) . ? Co O5 2.146(7) . ? O1 C4 1.339(11) . ? O2 C15 1.329(11) . ? O3 C18 1.437(13) . ? O4 C19 1.402(14) . ? O5 C20 1.404(13) . ? N1 C1 1.140(13) . ? N2 C2 1.160(12) . ? N2 Co 2.078(8) 2_467 ? N3 C3 1.158(12) . ? N3 Co 2.103(8) 1_565 ? N4 C16 1.35(3) . ? N4 C9 1.61(2) . ? N5 C17 1.16(5) . ? N4' C16' 1.23(3) . ? N4' C10 1.55(2) . ? N5' C17' 1.13(5) . ? C4 C9 1.392(15) . ? C4 C5 1.396(14) . ? C5 C6 1.364(15) . ? C6 C7 1.38(2) . ? C7 C8 1.37(2) . ? C8 C9 1.415(18) . ? C9 C16' 1.46(2) . ? C10 C11 1.382(18) . ? C10 C15 1.395(14) . ? C10 C16 1.42(3) . ? C11 C12 1.40(2) . ? C12 C13 1.34(2) . ? C13 C14 1.347(16) . ? C14 C15 1.421(14) . ? C16 C17 1.44(4) . ? C16' C17' 1.49(4) . ? O6 C21 1.442(12) . ? O7 C22 1.339(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ru O1 176.4(3) . . ? O2 Ru C2 92.0(3) . . ? O1 Ru C2 91.5(3) . . ? O2 Ru N4 98.4(5) . . ? O1 Ru N4 78.1(5) . . ? C2 Ru N4 169.5(6) . . ? O2 Ru C3 91.5(3) . . ? O1 Ru C3 89.2(3) . . ? C2 Ru C3 91.0(3) . . ? N4 Ru C3 87.0(6) . . ? O2 Ru C1 88.8(3) . . ? O1 Ru C1 90.5(3) . . ? C2 Ru C1 89.3(4) . . ? N4 Ru C1 92.6(6) . . ? C3 Ru C1 179.6(4) . . ? O2 Ru N4' 77.0(6) . . ? O1 Ru N4' 99.4(6) . . ? C2 Ru N4' 168.9(6) . . ? N4 Ru N4' 21.6(6) . . ? C3 Ru N4' 90.5(5) . . ? C1 Ru N4' 89.2(5) . . ? N2 Co O4 99.0(3) 2_467 . ? N2 Co N1 93.8(3) 2_467 . ? O4 Co N1 87.7(3) . . ? N2 Co N3 91.4(3) 2_467 1_545 ? O4 Co N3 89.4(3) . 1_545 ? N1 Co N3 174.4(3) . 1_545 ? N2 Co O3 87.5(3) 2_467 . ? O4 Co O3 173.4(3) . . ? N1 Co O3 91.4(3) . . ? N3 Co O3 90.9(3) 1_545 . ? N2 Co O5 172.8(3) 2_467 . ? O4 Co O5 88.0(3) . . ? N1 Co O5 88.2(3) . . ? N3 Co O5 86.9(3) 1_545 . ? O3 Co O5 85.5(3) . . ? C4 O1 Ru 117.4(6) . . ? C15 O2 Ru 118.7(6) . . ? C18 O3 Co 120.9(7) . . ? C19 O4 Co 130.3(7) . . ? C20 O5 Co 127.8(7) . . ? C1 N1 Co 171.4(8) . . ? C2 N2 Co 162.3(7) . 2_467 ? C3 N3 Co 172.1(8) . 1_565 ? C16 N4 C9 117.6(19) . . ? C16 N4 Ru 124.6(19) . . ? C9 N4 Ru 117.7(11) . . ? C16' N4' C10 127(2) . . ? C16' N4' Ru 119.5(19) . . ? C10 N4' Ru 113.3(12) . . ? N1 C1 Ru 173.4(9) . . ? N2 C2 Ru 176.7(8) . . ? N3 C3 Ru 177.6(8) . . ? O1 C4 C9 123.1(10) . . ? O1 C4 C5 118.0(10) . . ? C9 C4 C5 118.6(10) . . ? C6 C5 C4 121.1(11) . . ? C5 C6 C7 120.2(12) . . ? C8 C7 C6 120.5(13) . . ? C7 C8 C9 119.5(12) . . ? C4 C9 C8 119.7(11) . . ? C4 C9 C16' 138.2(14) . . ? C8 C9 C16' 101.9(14) . . ? C4 C9 N4 102.0(11) . . ? C8 C9 N4 138.2(12) . . ? C16' C9 N4 36.8(10) . . ? C11 C10 C15 119.2(11) . . ? C11 C10 C16 105.1(13) . . ? C15 C10 C16 135.8(13) . . ? C11 C10 N4' 137.0(13) . . ? C15 C10 N4' 103.8(11) . . ? C16 C10 N4' 32.0(10) . . ? C10 C11 C12 121.0(13) . . ? C13 C12 C11 119.6(12) . . ? C12 C13 C14 121.0(13) . . ? C13 C14 C15 121.5(12) . . ? O2 C15 C10 124.4(9) . . ? O2 C15 C14 118.0(10) . . ? C10 C15 C14 117.7(10) . . ? N4 C16 C10 115(2) . . ? N4 C16 C17 122(3) . . ? C10 C16 C17 123.0(19) . . ? N5 C17 C16 177(3) . . ? N4' C16' C9 120(2) . . ? N4' C16' C17' 123(2) . . ? C9 C16' C17' 117(2) . . ? N5' C17' C16' 175(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.263 _refine_diff_density_min -1.807 _refine_diff_density_rms 0.224 #=================================================================