data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Shane Telfer' _publ_contact_author_email S.TELFER@MASSEY.AC.NZ _publ_section_title ; Chromophoric Dipyrrin Complexes Capable of Binding to TiO2: Synthesis, Structure and Spectroscopy ; loop_ _publ_author_name 'Shane Telfer' 'Jeremy D. Hall' 'Tracey M. McLean' 'Serena J. Smalley' 'Mark Waterland' # Attachment 'B912332F X-ray revised.cif' data_[Ru(bipy)(1b)2] _database_code_depnum_ccdc_archive 'CCDC 737429' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '0.5(C42H30RuN6O4), (C5H12)' _chemical_formula_sum 'C52 H54 N6 O4 Ru' _chemical_formula_weight 928.08 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' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 12.4091(12) _cell_length_b 10.8412(8) _cell_length_c 33.848(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4553.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1139 _cell_measurement_theta_min 13.39 _cell_measurement_theta_max 143.42 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 3.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5667 _exptl_absorpt_correction_T_max 0.9387 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rigaku MM007 rotating anode' _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21994 _diffrn_reflns_av_R_equivalents 0.1398 _diffrn_reflns_av_sigmaI/netI 0.1231 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 6.69 _diffrn_reflns_theta_max 58.93 _reflns_number_total 3247 _reflns_number_gt 2307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1366P)^2^+22.6792P] 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 SHELXL _refine_ls_extinction_coef 0.00007(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3247 _refine_ls_number_parameters 278 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.1215 _refine_ls_wR_factor_ref 0.2901 _refine_ls_wR_factor_gt 0.2716 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.16224(9) 0.2500 0.0398(5) Uani 1 2 d S . . O1 O 0.8773(7) 0.4213(9) 0.0066(2) 0.090(3) Uani 1 1 d . . . H1A H 0.9231 0.4482 -0.0095 0.108 Uiso 1 1 calc . . . O2 O 0.9766(7) 0.5349(9) 0.0481(2) 0.081(3) Uani 1 1 d . . . H2A H 1.0108 0.5481 0.0271 0.097 Uiso 1 1 calc . . . N1 N 0.5302(6) 0.0182(7) 0.2864(2) 0.0437(18) Uani 1 1 d . . . N3 N 0.6579(6) 0.1596(7) 0.2309(2) 0.047(2) Uani 1 1 d . . . N4 N 0.4694(6) 0.2948(7) 0.2081(2) 0.0425(17) Uani 1 1 d . . . C2 C 0.5687(7) 0.0231(9) 0.3242(3) 0.049(2) Uani 1 1 d . . . H2 H 0.5755 0.1020 0.3361 0.059 Uiso 1 1 calc R . . C3 C 0.5979(8) -0.0768(9) 0.3459(3) 0.054(3) Uani 1 1 d . . . H3 H 0.6238 -0.0675 0.3722 0.065 Uiso 1 1 calc R . . C4 C 0.5892(8) -0.1922(9) 0.3289(3) 0.054(3) Uani 1 1 d . . . H4 H 0.6090 -0.2639 0.3433 0.065 Uiso 1 1 calc R . . C5 C 0.5512(8) -0.2017(9) 0.2909(3) 0.049(2) Uani 1 1 d . . . H5 H 0.5466 -0.2803 0.2786 0.059 Uiso 1 1 calc R . . C6 C 0.5196(8) -0.0973(10) 0.2704(3) 0.047(2) Uani 1 1 d . . . C20 C 0.7391(8) 0.0868(8) 0.2459(2) 0.044(2) Uani 1 1 d . . . H20 H 0.7337 0.0395 0.2694 0.053 Uiso 1 1 calc R . . C21 C 0.8313(7) 0.0917(9) 0.2217(3) 0.050(2) Uani 1 1 d . . . H21 H 0.8974 0.0498 0.2262 0.060 Uiso 1 1 calc R . . C22 C 0.8081(8) 0.1677(8) 0.1907(3) 0.046(2) Uani 1 1 d . . . H22 H 0.8549 0.1878 0.1694 0.055 Uiso 1 1 calc R . . C23 C 0.6433(7) 0.2937(8) 0.1719(2) 0.044(2) Uani 1 1 d . . . C24 C 0.5366(8) 0.3354(8) 0.1772(3) 0.042(2) Uani 1 1 d . . . C25 C 0.4823(8) 0.4257(9) 0.1547(3) 0.048(2) Uani 1 1 d . . . H25 H 0.5094 0.4676 0.1322 0.058 Uiso 1 1 calc R . . C26 C 0.3830(7) 0.4414(9) 0.1717(3) 0.052(2) Uani 1 1 d . . . H26 H 0.3282 0.4963 0.1631 0.062 Uiso 1 1 calc R . . C27 C 0.3774(8) 0.3619(9) 0.2040(3) 0.049(2) Uani 1 1 d . . . H27 H 0.3168 0.3552 0.2210 0.059 Uiso 1 1 calc R . . C28 C 0.7055(8) 0.3417(8) 0.1370(3) 0.045(2) Uani 1 1 d . . . C29 C 0.6787(8) 0.3076(9) 0.0991(3) 0.052(2) Uani 1 1 d . . . H29 H 0.6177 0.2564 0.0947 0.062 Uiso 1 1 calc R . . C30 C 0.7400(9) 0.3472(10) 0.0670(3) 0.060(3) Uani 1 1 d . . . H30 H 0.7227 0.3211 0.0410 0.072 Uiso 1 1 calc R . . C31 C 0.8277(8) 0.4261(10) 0.0737(3) 0.056(3) Uani 1 1 d . . . C32 C 0.8982(9) 0.4628(11) 0.0411(3) 0.067(3) Uani 1 1 d . . . C33 C 0.8501(8) 0.4643(9) 0.1117(3) 0.052(2) Uani 1 1 d . . . H33 H 0.9075 0.5206 0.1161 0.062 Uiso 1 1 calc R . . C34 C 0.7910(8) 0.4225(8) 0.1431(3) 0.049(2) Uani 1 1 d . . . H34 H 0.8085 0.4486 0.1691 0.058 Uiso 1 1 calc R . . C41 C 0.7005(7) 0.2114(8) 0.1961(3) 0.043(2) Uani 1 1 d . . . C100 C 0.298(2) 0.222(3) 0.0835(7) 0.209(14) Uani 1 1 d D . . C101 C 0.224(2) 0.288(2) 0.0546(7) 0.211(12) Uani 1 1 d D . . C102 C 0.134(2) 0.201(3) 0.0413(8) 0.200(7) Uani 1 1 d DU . . C103 C 0.045(2) 0.175(3) 0.0712(8) 0.200(7) Uani 0.79(3) 1 d PDU . . C104 C 0.027(5) 0.171(11) 0.0207(17) 0.200(7) Uani 0.21(3) 1 d PDU . . C105 C -0.044(2) 0.100(3) 0.0504(8) 0.200(7) Uani 1 1 d DU . . 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 0.0358(8) 0.0385(7) 0.0452(7) 0.000 0.0025(4) 0.000 O1 0.082(6) 0.131(8) 0.057(5) 0.003(5) 0.017(4) -0.039(6) O2 0.069(5) 0.112(7) 0.061(5) -0.001(4) 0.016(4) -0.041(5) N1 0.038(4) 0.039(5) 0.054(5) 0.001(4) 0.012(3) -0.005(4) N3 0.053(5) 0.050(5) 0.038(4) -0.004(3) -0.003(4) 0.004(4) N4 0.038(4) 0.039(4) 0.050(4) -0.004(4) 0.005(3) -0.001(4) C2 0.041(6) 0.053(6) 0.052(5) -0.001(4) 0.000(4) 0.000(5) C3 0.057(7) 0.053(6) 0.054(5) 0.008(5) -0.008(5) 0.000(5) C4 0.040(6) 0.043(6) 0.079(7) 0.012(5) 0.004(5) -0.005(5) C5 0.044(6) 0.042(5) 0.062(6) 0.001(5) 0.001(5) 0.005(5) C6 0.035(6) 0.049(7) 0.055(6) 0.003(5) 0.001(4) 0.000(5) C20 0.048(7) 0.042(6) 0.044(5) -0.001(4) -0.001(4) 0.006(5) C21 0.031(5) 0.055(6) 0.063(6) -0.005(5) 0.005(4) 0.008(5) C22 0.041(6) 0.042(5) 0.055(6) 0.000(4) 0.005(4) -0.004(4) C23 0.044(6) 0.040(5) 0.049(5) -0.005(4) 0.001(4) -0.007(4) C24 0.038(5) 0.042(5) 0.047(5) 0.001(4) 0.008(4) -0.001(4) C25 0.063(7) 0.039(6) 0.042(5) 0.007(4) -0.006(4) -0.006(4) C26 0.030(5) 0.052(6) 0.074(6) 0.009(5) 0.005(4) 0.003(5) C27 0.045(6) 0.056(6) 0.048(5) 0.003(4) 0.003(4) 0.007(5) C28 0.038(5) 0.049(6) 0.047(5) -0.003(4) 0.001(4) 0.009(4) C29 0.048(6) 0.055(6) 0.051(6) 0.001(5) 0.007(4) -0.011(5) C30 0.057(7) 0.071(7) 0.052(6) 0.000(5) 0.001(5) -0.007(6) C31 0.054(6) 0.059(6) 0.056(6) 0.002(5) 0.008(5) -0.003(5) C32 0.063(8) 0.086(8) 0.051(6) 0.001(5) 0.009(5) -0.015(7) C33 0.038(6) 0.050(6) 0.067(6) 0.006(5) 0.004(4) -0.004(5) C34 0.051(6) 0.047(5) 0.048(5) -0.005(4) 0.005(4) 0.004(5) C41 0.024(5) 0.047(5) 0.057(5) -0.005(4) 0.004(4) -0.002(4) C100 0.21(3) 0.27(3) 0.146(19) -0.11(2) -0.036(17) 0.13(2) C101 0.22(3) 0.26(3) 0.15(2) -0.08(2) 0.06(2) 0.01(3) C102 0.190(18) 0.181(13) 0.229(19) -0.002(13) 0.011(13) -0.081(13) C103 0.190(18) 0.181(13) 0.229(19) -0.002(13) 0.011(13) -0.081(13) C104 0.190(18) 0.181(13) 0.229(19) -0.002(13) 0.011(13) -0.081(13) C105 0.190(18) 0.181(13) 0.229(19) -0.002(13) 0.011(13) -0.081(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 N1 2.025(8) 4_655 ? Ru1 N1 2.025(8) . ? Ru1 N4 2.055(8) 4_655 ? Ru1 N4 2.055(8) . ? Ru1 N3 2.063(8) . ? Ru1 N3 2.063(8) 4_655 ? O1 C32 1.277(12) . ? O1 H1A 0.8400 . ? O2 C32 1.269(13) . ? O2 H2A 0.8400 . ? N1 C2 1.365(11) . ? N1 C6 1.372(12) . ? N3 C20 1.377(12) . ? N3 C41 1.408(11) . ? N4 C27 1.361(12) . ? N4 C24 1.407(12) . ? C2 C3 1.358(13) . ? C2 H2 0.9500 . ? C3 C4 1.381(13) . ? C3 H3 0.9500 . ? C4 C5 1.376(13) . ? C4 H4 0.9500 . ? C5 C6 1.383(13) . ? C5 H5 0.9500 . ? C6 C6 1.463(18) 4_655 ? C20 C21 1.406(13) . ? C20 H20 0.9500 . ? C21 C22 1.366(13) . ? C21 H21 0.9500 . ? C22 C41 1.429(12) . ? C22 H22 0.9500 . ? C23 C41 1.404(12) . ? C23 C24 1.410(13) . ? C23 C28 1.504(12) . ? C24 C25 1.412(13) . ? C25 C26 1.370(13) . ? C25 H25 0.9500 . ? C26 C27 1.392(13) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.378(12) . ? C28 C34 1.391(13) . ? C29 C30 1.393(13) . ? C29 H29 0.9500 . ? C30 C31 1.403(14) . ? C30 H30 0.9500 . ? C31 C33 1.379(13) . ? C31 C32 1.464(14) . ? C33 C34 1.369(12) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C100 C101 1.525(10) . ? C101 C102 1.532(10) . ? C102 C103 1.526(10) . ? C102 C104 1.538(10) . ? C103 C105 1.537(10) . ? C104 C105 1.538(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N1 79.1(4) 4_655 . ? N1 Ru1 N4 173.8(3) 4_655 4_655 ? N1 Ru1 N4 94.9(3) . 4_655 ? N1 Ru1 N4 94.9(3) 4_655 . ? N1 Ru1 N4 173.8(3) . . ? N4 Ru1 N4 91.2(4) 4_655 . ? N1 Ru1 N3 88.5(3) 4_655 . ? N1 Ru1 N3 90.2(3) . . ? N4 Ru1 N3 92.9(3) 4_655 . ? N4 Ru1 N3 88.2(3) . . ? N1 Ru1 N3 90.2(3) 4_655 4_655 ? N1 Ru1 N3 88.5(3) . 4_655 ? N4 Ru1 N3 88.2(3) 4_655 4_655 ? N4 Ru1 N3 92.9(3) . 4_655 ? N3 Ru1 N3 178.4(4) . 4_655 ? C32 O1 H1A 109.5 . . ? C32 O2 H2A 109.5 . . ? C2 N1 C6 116.1(8) . . ? C2 N1 Ru1 127.2(6) . . ? C6 N1 Ru1 116.4(6) . . ? C20 N3 C41 105.1(7) . . ? C20 N3 Ru1 126.0(6) . . ? C41 N3 Ru1 127.8(6) . . ? C27 N4 C24 104.7(8) . . ? C27 N4 Ru1 126.8(6) . . ? C24 N4 Ru1 128.4(6) . . ? C3 C2 N1 124.7(9) . . ? C3 C2 H2 117.6 . . ? N1 C2 H2 117.6 . . ? C2 C3 C4 118.4(9) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 119.0(9) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 120.3(9) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? N1 C6 C5 121.4(9) . . ? N1 C6 C6 113.9(5) . 4_655 ? C5 C6 C6 124.5(6) . 4_655 ? N3 C20 C21 111.1(8) . . ? N3 C20 H20 124.5 . . ? C21 C20 H20 124.5 . . ? C22 C21 C20 107.4(8) . . ? C22 C21 H21 126.3 . . ? C20 C21 H21 126.3 . . ? C21 C22 C41 107.3(8) . . ? C21 C22 H22 126.4 . . ? C41 C22 H22 126.4 . . ? C41 C23 C24 127.2(8) . . ? C41 C23 C28 114.8(8) . . ? C24 C23 C28 118.1(8) . . ? N4 C24 C23 123.4(9) . . ? N4 C24 C25 109.5(8) . . ? C23 C24 C25 127.0(9) . . ? C26 C25 C24 106.8(8) . . ? C26 C25 H25 126.6 . . ? C24 C25 H25 126.6 . . ? C25 C26 C27 107.3(9) . . ? C25 C26 H26 126.4 . . ? C27 C26 H26 126.4 . . ? N4 C27 C26 111.7(8) . . ? N4 C27 H27 124.2 . . ? C26 C27 H27 124.2 . . ? C29 C28 C34 119.4(8) . . ? C29 C28 C23 121.1(9) . . ? C34 C28 C23 119.5(8) . . ? C28 C29 C30 120.8(10) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C31 119.1(10) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C33 C31 C30 119.4(9) . . ? C33 C31 C32 120.0(10) . . ? C30 C31 C32 120.5(9) . . ? O2 C32 O1 123.0(9) . . ? O2 C32 C31 118.9(9) . . ? O1 C32 C31 118.1(10) . . ? C34 C33 C31 121.1(10) . . ? C34 C33 H33 119.5 . . ? C31 C33 H33 119.5 . . ? C33 C34 C28 120.2(9) . . ? C33 C34 H34 119.9 . . ? C28 C34 H34 119.9 . . ? C23 C41 N3 123.5(8) . . ? C23 C41 C22 127.4(8) . . ? N3 C41 C22 109.1(8) . . ? C100 C101 C102 110(2) . . ? C103 C102 C101 117(2) . . ? C103 C102 C104 69(3) . . ? C101 C102 C104 154(5) . . ? C102 C103 C105 108(2) . . ? C102 C103 C104 56.1(14) . . ? C105 C103 C104 55.9(14) . . ? C102 C104 C105 108(2) . . ? C102 C104 C103 55.4(14) . . ? C105 C104 C103 55.8(14) . . ? C103 C105 C104 68(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ru1 N1 C2 175.5(9) 4_655 . . . ? N4 Ru1 N1 C2 -5.9(8) 4_655 . . . ? N4 Ru1 N1 C2 163(2) . . . . ? N3 Ru1 N1 C2 87.0(8) . . . . ? N3 Ru1 N1 C2 -94.0(8) 4_655 . . . ? N1 Ru1 N1 C6 1.5(5) 4_655 . . . ? N4 Ru1 N1 C6 -179.9(6) 4_655 . . . ? N4 Ru1 N1 C6 -11(3) . . . . ? N3 Ru1 N1 C6 -87.0(7) . . . . ? N3 Ru1 N1 C6 92.0(7) 4_655 . . . ? N1 Ru1 N3 C20 -85.2(7) 4_655 . . . ? N1 Ru1 N3 C20 -6.1(7) . . . . ? N4 Ru1 N3 C20 88.7(7) 4_655 . . . ? N4 Ru1 N3 C20 179.9(7) . . . . ? N3 Ru1 N3 C20 -45.7(7) 4_655 . . . ? N1 Ru1 N3 C41 81.4(7) 4_655 . . . ? N1 Ru1 N3 C41 160.5(7) . . . . ? N4 Ru1 N3 C41 -104.6(7) 4_655 . . . ? N4 Ru1 N3 C41 -13.5(7) . . . . ? N3 Ru1 N3 C41 121.0(7) 4_655 . . . ? N1 Ru1 N4 C27 100.3(8) 4_655 . . . ? N1 Ru1 N4 C27 113(3) . . . . ? N4 Ru1 N4 C27 -78.5(7) 4_655 . . . ? N3 Ru1 N4 C27 -171.3(8) . . . . ? N3 Ru1 N4 C27 9.8(8) 4_655 . . . ? N1 Ru1 N4 C24 -78.6(8) 4_655 . . . ? N1 Ru1 N4 C24 -66(3) . . . . ? N4 Ru1 N4 C24 102.7(8) 4_655 . . . ? N3 Ru1 N4 C24 9.8(8) . . . . ? N3 Ru1 N4 C24 -169.1(8) 4_655 . . . ? C6 N1 C2 C3 1.1(14) . . . . ? Ru1 N1 C2 C3 -172.9(7) . . . . ? N1 C2 C3 C4 0.4(15) . . . . ? C2 C3 C4 C5 -0.1(14) . . . . ? C3 C4 C5 C6 -1.7(14) . . . . ? C2 N1 C6 C5 -2.9(13) . . . . ? Ru1 N1 C6 C5 171.7(7) . . . . ? C2 N1 C6 C6 -178.7(9) . . . 4_655 ? Ru1 N1 C6 C6 -4.1(13) . . . 4_655 ? C4 C5 C6 N1 3.3(14) . . . . ? C4 C5 C6 C6 178.6(11) . . . 4_655 ? C41 N3 C20 C21 0.3(10) . . . . ? Ru1 N3 C20 C21 169.4(6) . . . . ? N3 C20 C21 C22 -0.6(11) . . . . ? C20 C21 C22 C41 0.7(10) . . . . ? C27 N4 C24 C23 176.5(8) . . . . ? Ru1 N4 C24 C23 -4.4(13) . . . . ? C27 N4 C24 C25 -0.7(10) . . . . ? Ru1 N4 C24 C25 178.4(6) . . . . ? C41 C23 C24 N4 -2.3(15) . . . . ? C28 C23 C24 N4 178.3(8) . . . . ? C41 C23 C24 C25 174.4(9) . . . . ? C28 C23 C24 C25 -5.0(14) . . . . ? N4 C24 C25 C26 0.4(11) . . . . ? C23 C24 C25 C26 -176.6(9) . . . . ? C24 C25 C26 C27 0.0(11) . . . . ? C24 N4 C27 C26 0.7(11) . . . . ? Ru1 N4 C27 C26 -178.4(6) . . . . ? C25 C26 C27 N4 -0.5(11) . . . . ? C41 C23 C28 C29 111.0(10) . . . . ? C24 C23 C28 C29 -69.5(12) . . . . ? C41 C23 C28 C34 -69.4(11) . . . . ? C24 C23 C28 C34 110.1(10) . . . . ? C34 C28 C29 C30 3.8(14) . . . . ? C23 C28 C29 C30 -176.6(9) . . . . ? C28 C29 C30 C31 -2.2(15) . . . . ? C29 C30 C31 C33 -1.0(15) . . . . ? C29 C30 C31 C32 175.8(10) . . . . ? C33 C31 C32 O2 -3.5(17) . . . . ? C30 C31 C32 O2 179.7(11) . . . . ? C33 C31 C32 O1 177.1(10) . . . . ? C30 C31 C32 O1 0.3(17) . . . . ? C30 C31 C33 C34 2.7(15) . . . . ? C32 C31 C33 C34 -174.2(10) . . . . ? C31 C33 C34 C28 -1.1(14) . . . . ? C29 C28 C34 C33 -2.1(14) . . . . ? C23 C28 C34 C33 178.3(8) . . . . ? C24 C23 C41 N3 -1.7(15) . . . . ? C28 C23 C41 N3 177.7(8) . . . . ? C24 C23 C41 C22 179.3(9) . . . . ? C28 C23 C41 C22 -1.3(13) . . . . ? C20 N3 C41 C23 -179.0(8) . . . . ? Ru1 N3 C41 C23 12.1(13) . . . . ? C20 N3 C41 C22 0.2(10) . . . . ? Ru1 N3 C41 C22 -168.7(6) . . . . ? C21 C22 C41 C23 178.6(9) . . . . ? C21 C22 C41 N3 -0.5(10) . . . . ? C100 C101 C102 C103 74(3) . . . . ? C100 C101 C102 C104 170(8) . . . . ? C101 C102 C103 C105 173(3) . . . . ? C104 C102 C103 C105 21(6) . . . . ? C101 C102 C103 C104 152(6) . . . . ? C103 C102 C104 C105 -21(6) . . . . ? C101 C102 C104 C105 -128(5) . . . . ? C101 C102 C104 C103 -107(7) . . . . ? C105 C103 C104 C102 -156(6) . . . . ? C102 C103 C104 C105 156(6) . . . . ? C102 C103 C105 C104 -21(6) . . . . ? C102 C104 C105 C103 21(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 58.93 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.737 _refine_diff_density_min -1.392 _refine_diff_density_rms 0.131 # END data_[Rh(La)3] _database_code_depnum_ccdc_archive 'CCDC 737430' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (C51H39N6O6Rh) _chemical_formula_sum 'C51 H39 N6 O6 Rh' _chemical_formula_weight 934.79 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' Rh Rh 0.0927 3.6045 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.8323(6) _cell_length_b 9.7313(3) _cell_length_c 28.7614(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.025(2) _cell_angle_gamma 90.00 _cell_volume 4148.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6844 _cell_measurement_theta_min 13.25 _cell_measurement_theta_max 142.77 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 3.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rigaku MM007 rotating anode' _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32827 _diffrn_reflns_av_R_equivalents 0.1002 _diffrn_reflns_av_sigmaI/netI 0.1288 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 6.62 _diffrn_reflns_theta_max 68.24 _reflns_number_total 7430 _reflns_number_gt 4558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+7.8691P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7430 _refine_ls_number_parameters 580 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1628 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.009 _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 Rh1 Rh 0.84172(4) 0.05181(5) 0.118274(15) 0.0372(2) Uani 1 1 d . . . N1 N 0.9120(4) -0.0537(5) 0.07082(17) 0.0388(14) Uani 1 1 d . . . N2 N 0.9422(4) 0.0238(6) 0.16736(17) 0.0417(15) Uani 1 1 d . . . N3 N 0.7837(4) -0.1234(6) 0.14066(17) 0.0419(15) Uani 1 1 d . . . N4 N 0.7688(4) 0.1605(6) 0.16396(16) 0.0360(13) Uani 1 1 d . . . N5 N 0.7395(4) 0.0768(6) 0.07080(18) 0.0410(14) Uani 1 1 d . . . N6 N 0.8998(4) 0.2274(5) 0.09533(16) 0.0401(15) Uani 1 1 d . . . O1 O 1.4597(4) -0.3082(6) 0.08635(19) 0.0681(17) Uani 1 1 d . . . O2 O 1.4135(4) -0.4631(6) 0.13833(17) 0.0580(15) Uani 1 1 d . . . O3 O 0.3415(3) -0.1460(5) 0.32951(15) 0.0557(14) Uani 1 1 d . . . O4 O 0.2811(3) -0.2253(5) 0.26209(16) 0.0560(14) Uani 1 1 d . . . O5 O 0.5501(4) 0.7778(6) -0.06935(17) 0.0677(16) Uani 1 1 d . . . O6 O 0.6859(4) 0.8238(6) -0.09592(19) 0.0731(18) Uani 1 1 d . . . C1 C 0.8848(6) -0.0846(7) 0.0266(2) 0.047(2) Uani 1 1 d . . . H1 H 0.8289 -0.0576 0.0123 0.057 Uiso 1 1 calc R . . C2 C 0.9523(5) -0.1638(7) 0.0045(2) 0.047(2) Uani 1 1 d . . . H2 H 0.9498 -0.1975 -0.0265 0.057 Uiso 1 1 calc R . . C3 C 1.0210(5) -0.1815(7) 0.0369(2) 0.0456(19) Uani 1 1 d . . . H3 H 1.0753 -0.2311 0.0326 0.055 Uiso 1 1 calc R . . C4 C 0.9969(5) -0.1129(7) 0.0777(2) 0.0406(17) Uani 1 1 d . . . C5 C 1.0482(5) -0.1071(7) 0.1195(2) 0.0443(18) Uani 1 1 d . . . C6 C 1.1408(5) -0.1721(8) 0.1190(2) 0.0433(18) Uani 1 1 d . . . C7 C 1.2109(6) -0.1043(8) 0.0971(2) 0.054(2) Uani 1 1 d . . . H7 H 1.2010 -0.0168 0.0831 0.064 Uiso 1 1 calc R . . C8 C 1.2946(6) -0.1660(9) 0.0960(3) 0.057(2) Uani 1 1 d . . . H8 H 1.3426 -0.1200 0.0815 0.068 Uiso 1 1 calc R . . C9 C 1.3094(5) -0.2929(8) 0.1157(2) 0.0473(19) Uani 1 1 d . . . C10 C 1.4031(6) -0.3530(9) 0.1112(3) 0.054(2) Uani 1 1 d . . . C11 C 1.5031(6) -0.5262(10) 0.1361(3) 0.078(3) Uani 1 1 d . . . H11A H 1.5111 -0.5630 0.1048 0.117 Uiso 1 1 calc R . . H11B H 1.5085 -0.6009 0.1588 0.117 Uiso 1 1 calc R . . H11C H 1.5495 -0.4568 0.1431 0.117 Uiso 1 1 calc R . . C12 C 1.2422(5) -0.3577(8) 0.1384(2) 0.0471(19) Uani 1 1 d . . . H12 H 1.2535 -0.4441 0.1529 0.057 Uiso 1 1 calc R . . C13 C 1.1578(5) -0.2980(7) 0.1406(2) 0.0470(19) Uani 1 1 d . . . H13 H 1.1114 -0.3429 0.1567 0.056 Uiso 1 1 calc R . . C14 C 1.0756(6) -0.0409(7) 0.2036(2) 0.047(2) Uani 1 1 d . . . H14 H 1.1343 -0.0780 0.2092 0.057 Uiso 1 1 calc R . . C15 C 1.0250(6) 0.0272(7) 0.2350(2) 0.051(2) Uani 1 1 d . . . H15 H 1.0415 0.0458 0.2666 0.062 Uiso 1 1 calc R . . C16 C 0.9443(5) 0.0642(7) 0.2117(2) 0.0418(18) Uani 1 1 d . . . H16 H 0.8966 0.1123 0.2258 0.050 Uiso 1 1 calc R . . C17 C 1.0237(5) -0.0458(7) 0.1611(2) 0.0395(17) Uani 1 1 d . . . C20 C 0.8078(5) -0.2509(8) 0.1291(2) 0.0475(19) Uani 1 1 d . . . H20 H 0.8580 -0.2726 0.1108 0.057 Uiso 1 1 calc R . . C21 C 0.7497(5) -0.3478(8) 0.1474(2) 0.048(2) Uani 1 1 d . . . H21 H 0.7525 -0.4447 0.1437 0.058 Uiso 1 1 calc R . . C22 C 0.6879(5) -0.2757(7) 0.1719(2) 0.0452(19) Uani 1 1 d . . . H22 H 0.6401 -0.3140 0.1888 0.054 Uiso 1 1 calc R . . C23 C 0.7076(5) -0.1340(7) 0.1677(2) 0.0361(16) Uani 1 1 d . . . C24 C 0.6646(5) -0.0226(7) 0.1877(2) 0.0368(17) Uani 1 1 d . . . C25 C 0.5805(5) -0.0554(7) 0.2128(2) 0.0382(17) Uani 1 1 d . . . C26 C 0.5724(5) -0.0233(7) 0.2601(2) 0.0425(18) Uani 1 1 d . . . H26 H 0.6208 0.0223 0.2762 0.051 Uiso 1 1 calc R . . C27 C 0.4958(5) -0.0560(7) 0.2839(2) 0.0411(18) Uani 1 1 d . . . H27 H 0.4923 -0.0344 0.3160 0.049 Uiso 1 1 calc R . . C28 C 0.4239(5) -0.1210(7) 0.2603(2) 0.0415(17) Uani 1 1 d . . . C29 C 0.4290(5) -0.1501(7) 0.2131(2) 0.0431(18) Uani 1 1 d . . . H29 H 0.3795 -0.1923 0.1968 0.052 Uiso 1 1 calc R . . C30 C 0.5058(5) -0.1177(7) 0.1900(2) 0.0403(17) Uani 1 1 d . . . H30 H 0.5085 -0.1380 0.1578 0.048 Uiso 1 1 calc R . . C31 C 0.3452(5) -0.1635(7) 0.2881(2) 0.0412(17) Uani 1 1 d . . . C32 C 0.2062(5) -0.2794(9) 0.2880(3) 0.066(2) Uani 1 1 d . . . H32A H 0.2291 -0.3455 0.3113 0.099 Uiso 1 1 calc R . . H32B H 0.1631 -0.3253 0.2666 0.099 Uiso 1 1 calc R . . H32C H 0.1759 -0.2037 0.3037 0.099 Uiso 1 1 calc R . . C33 C 0.6907(5) 0.1145(7) 0.1868(2) 0.0405(17) Uani 1 1 d . . . C34 C 0.6546(5) 0.2288(7) 0.2100(2) 0.0404(17) Uani 1 1 d . . . H34 H 0.6020 0.2283 0.2279 0.049 Uiso 1 1 calc R . . C35 C 0.7079(5) 0.3398(7) 0.2022(2) 0.0448(18) Uani 1 1 d . . . H35 H 0.7004 0.4303 0.2139 0.054 Uiso 1 1 calc R . . C36 C 0.7759(5) 0.2935(7) 0.1737(2) 0.0401(17) Uani 1 1 d . . . H36 H 0.8222 0.3509 0.1625 0.048 Uiso 1 1 calc R . . C40 C 0.6800(5) -0.0208(8) 0.0564(2) 0.052(2) Uani 1 1 d . . . H40 H 0.6782 -0.1116 0.0685 0.063 Uiso 1 1 calc R . . C41 C 0.6215(6) 0.0301(9) 0.0212(3) 0.056(2) Uani 1 1 d . . . H41 H 0.5747 -0.0194 0.0052 0.067 Uiso 1 1 calc R . . C42 C 0.6446(5) 0.1659(9) 0.0140(2) 0.055(2) Uani 1 1 d . . . H42 H 0.6158 0.2279 -0.0073 0.066 Uiso 1 1 calc R . . C43 C 0.7195(5) 0.1953(8) 0.0446(2) 0.0445(19) Uani 1 1 d . . . C44 C 0.7734(5) 0.3140(8) 0.0448(2) 0.0439(18) Uani 1 1 d . . . C45 C 0.7393(5) 0.4321(7) 0.0157(2) 0.0398(17) Uani 1 1 d . . . C46 C 0.6551(6) 0.4900(8) 0.0243(3) 0.055(2) Uani 1 1 d . . . H46 H 0.6200 0.4547 0.0486 0.065 Uiso 1 1 calc R . . C47 C 0.6231(5) 0.5989(8) -0.0026(3) 0.056(2) Uani 1 1 d . . . H47 H 0.5661 0.6381 0.0037 0.067 Uiso 1 1 calc R . . C48 C 0.6726(5) 0.6515(7) -0.0386(2) 0.0464(19) Uani 1 1 d . . . C49 C 0.6406(6) 0.7604(8) -0.0705(3) 0.055(2) Uani 1 1 d . . . C50 C 0.5122(7) 0.8745(10) -0.1032(3) 0.088(3) Uani 1 1 d . . . H50A H 0.5154 0.9676 -0.0902 0.132 Uiso 1 1 calc R . . H50B H 0.4491 0.8505 -0.1104 0.132 Uiso 1 1 calc R . . H50C H 0.5466 0.8705 -0.1316 0.132 Uiso 1 1 calc R . . C51 C 0.7561(6) 0.5923(7) -0.0470(2) 0.049(2) Uani 1 1 d . . . H51 H 0.7908 0.6269 -0.0715 0.058 Uiso 1 1 calc R . . C52 C 0.7894(6) 0.4836(8) -0.0201(2) 0.048(2) Uani 1 1 d . . . H52 H 0.8465 0.4446 -0.0263 0.058 Uiso 1 1 calc R . . C53 C 0.8581(5) 0.3313(7) 0.0679(2) 0.0383(17) Uani 1 1 d . . . C54 C 0.9168(5) 0.4451(6) 0.0669(2) 0.0363(17) Uani 1 1 d . . . H54 H 0.9047 0.5302 0.0518 0.044 Uiso 1 1 calc R . . C55 C 0.9937(5) 0.4114(7) 0.0914(2) 0.0403(17) Uani 1 1 d . . . H55 H 1.0462 0.4664 0.0958 0.048 Uiso 1 1 calc R . . C56 C 0.9793(5) 0.2781(7) 0.1089(2) 0.0378(17) Uani 1 1 d . . . H56 H 1.0219 0.2300 0.1283 0.045 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 Rh1 0.0583(4) 0.0290(4) 0.0242(3) 0.0012(2) 0.0012(2) -0.0011(3) N1 0.056(4) 0.033(4) 0.027(3) 0.009(2) -0.002(3) -0.002(3) N2 0.064(4) 0.031(4) 0.030(3) -0.002(2) 0.000(3) 0.001(3) N3 0.068(4) 0.027(4) 0.030(3) 0.004(2) 0.000(3) 0.012(3) N4 0.056(4) 0.024(3) 0.028(3) 0.006(2) 0.005(2) -0.002(3) N5 0.049(4) 0.038(4) 0.036(3) 0.007(3) 0.002(3) -0.002(3) N6 0.068(4) 0.030(4) 0.022(3) 0.001(2) -0.001(3) 0.017(3) O1 0.062(4) 0.086(5) 0.056(3) -0.003(3) 0.006(3) 0.006(3) O2 0.062(4) 0.064(4) 0.047(3) -0.006(3) -0.003(3) 0.014(3) O3 0.057(3) 0.074(4) 0.037(3) -0.002(3) 0.011(2) 0.002(3) O4 0.060(3) 0.067(4) 0.042(3) 0.003(3) 0.002(2) -0.013(3) O5 0.092(5) 0.062(4) 0.049(3) 0.014(3) -0.005(3) 0.019(3) O6 0.111(5) 0.053(4) 0.056(3) 0.020(3) 0.013(3) 0.011(4) C1 0.077(6) 0.040(5) 0.024(3) 0.004(3) -0.005(3) 0.005(4) C2 0.080(6) 0.038(5) 0.025(3) -0.007(3) 0.013(3) -0.006(4) C3 0.068(5) 0.035(5) 0.034(4) -0.002(3) 0.006(3) 0.000(4) C4 0.064(5) 0.029(4) 0.029(3) -0.002(3) 0.003(3) 0.000(4) C5 0.058(5) 0.038(5) 0.036(4) 0.001(3) 0.001(3) -0.002(4) C6 0.055(5) 0.039(5) 0.036(4) -0.002(3) -0.006(3) 0.000(4) C7 0.070(6) 0.041(5) 0.051(4) 0.011(4) 0.003(4) -0.002(4) C8 0.059(5) 0.058(6) 0.054(5) 0.002(4) 0.006(4) 0.003(5) C9 0.060(5) 0.044(5) 0.038(4) -0.002(3) -0.001(3) -0.005(4) C10 0.062(6) 0.063(6) 0.037(4) -0.018(4) -0.005(4) 0.009(5) C11 0.067(6) 0.093(8) 0.073(6) -0.013(5) -0.006(5) 0.029(6) C12 0.072(6) 0.030(5) 0.039(4) 0.003(3) -0.007(4) 0.007(4) C13 0.069(5) 0.030(5) 0.041(4) 0.005(3) 0.002(4) -0.002(4) C14 0.074(6) 0.030(5) 0.036(4) 0.004(3) -0.006(4) 0.006(4) C15 0.086(6) 0.042(5) 0.025(3) 0.000(3) -0.009(4) -0.006(4) C16 0.069(5) 0.027(4) 0.029(3) -0.003(3) 0.000(3) 0.004(4) C17 0.063(5) 0.023(4) 0.032(3) 0.001(3) -0.001(3) -0.002(3) C20 0.068(5) 0.039(5) 0.036(4) -0.001(3) 0.003(3) 0.003(4) C21 0.083(6) 0.023(4) 0.039(4) 0.002(3) 0.009(4) 0.005(4) C22 0.068(5) 0.032(5) 0.036(4) 0.000(3) 0.007(3) -0.008(4) C23 0.060(5) 0.024(4) 0.025(3) 0.004(3) 0.008(3) -0.005(3) C24 0.053(4) 0.037(5) 0.020(3) 0.006(3) 0.001(3) -0.006(4) C25 0.054(5) 0.031(4) 0.030(3) 0.008(3) 0.005(3) -0.001(3) C26 0.062(5) 0.040(5) 0.025(3) 0.004(3) 0.002(3) -0.009(4) C27 0.063(5) 0.036(5) 0.025(3) 0.001(3) 0.003(3) 0.008(4) C28 0.056(5) 0.037(5) 0.032(3) 0.002(3) 0.006(3) 0.001(4) C29 0.058(5) 0.037(5) 0.034(3) 0.007(3) 0.001(3) -0.006(4) C30 0.060(5) 0.033(4) 0.028(3) 0.006(3) 0.005(3) -0.003(4) C31 0.047(4) 0.037(5) 0.040(4) 0.004(3) 0.009(3) -0.002(4) C32 0.071(6) 0.079(7) 0.049(4) 0.012(4) 0.016(4) -0.025(5) C33 0.066(5) 0.029(4) 0.026(3) 0.003(3) -0.004(3) -0.004(4) C34 0.054(5) 0.036(5) 0.032(3) 0.001(3) 0.001(3) 0.001(4) C35 0.076(5) 0.024(4) 0.034(3) 0.003(3) 0.002(3) 0.005(4) C36 0.064(5) 0.019(4) 0.037(4) -0.002(3) 0.010(3) 0.005(4) C40 0.064(5) 0.044(5) 0.048(4) 0.008(4) 0.004(4) 0.000(4) C41 0.059(5) 0.060(6) 0.049(4) 0.007(4) -0.011(4) -0.010(4) C42 0.062(5) 0.055(6) 0.048(4) 0.014(4) -0.005(4) -0.006(4) C43 0.064(5) 0.045(5) 0.025(3) 0.002(3) 0.003(3) 0.005(4) C44 0.066(5) 0.036(5) 0.030(3) 0.000(3) 0.006(3) 0.001(4) C45 0.056(5) 0.036(5) 0.028(3) 0.003(3) 0.002(3) -0.004(4) C46 0.066(6) 0.053(5) 0.046(4) 0.019(4) 0.012(4) 0.011(4) C47 0.060(5) 0.058(6) 0.051(4) 0.016(4) 0.007(4) 0.017(4) C48 0.070(5) 0.034(5) 0.035(4) 0.003(3) 0.001(3) 0.006(4) C49 0.077(6) 0.043(6) 0.046(4) 0.012(4) 0.008(4) 0.010(5) C50 0.133(9) 0.081(7) 0.050(5) 0.026(5) -0.011(5) 0.032(7) C51 0.077(6) 0.038(5) 0.031(4) 0.002(3) 0.007(4) 0.000(4) C52 0.074(6) 0.037(5) 0.034(4) 0.002(3) 0.007(4) 0.005(4) C53 0.053(5) 0.030(4) 0.033(3) 0.000(3) 0.008(3) 0.008(3) C54 0.065(5) 0.013(4) 0.032(3) -0.003(3) 0.016(3) -0.003(3) C55 0.054(5) 0.033(5) 0.034(3) -0.004(3) 0.003(3) -0.012(4) C56 0.048(4) 0.040(5) 0.025(3) -0.007(3) -0.003(3) 0.003(4) _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 Rh1 N5 2.018(5) . ? Rh1 N3 2.026(6) . ? Rh1 N1 2.026(6) . ? Rh1 N4 2.029(5) . ? Rh1 N2 2.034(6) . ? Rh1 N6 2.034(6) . ? N1 C1 1.355(7) . ? N1 C4 1.392(8) . ? N2 C16 1.335(8) . ? N2 C17 1.404(9) . ? N3 C20 1.337(8) . ? N3 C23 1.396(8) . ? N4 C36 1.327(8) . ? N4 C33 1.426(8) . ? N5 C40 1.351(9) . ? N5 C43 1.405(8) . ? N6 C56 1.324(8) . ? N6 C53 1.412(8) . ? O1 C10 1.203(9) . ? O2 C10 1.332(9) . ? O2 C11 1.467(9) . ? O3 C31 1.208(7) . ? O4 C31 1.331(8) . ? O4 C32 1.459(8) . ? O5 C49 1.355(9) . ? O5 C50 1.451(8) . ? O6 C49 1.185(9) . ? C1 C2 1.429(10) . ? C2 C3 1.367(9) . ? C3 C4 1.408(8) . ? C4 C5 1.402(9) . ? C5 C17 1.395(9) . ? C5 C6 1.514(10) . ? C6 C13 1.392(9) . ? C6 C7 1.401(10) . ? C7 C8 1.381(10) . ? C8 C9 1.372(10) . ? C9 C12 1.366(10) . ? C9 C10 1.517(11) . ? C12 C13 1.384(10) . ? C14 C15 1.365(10) . ? C14 C17 1.424(9) . ? C15 C16 1.398(10) . ? C20 C21 1.394(9) . ? C21 C22 1.370(9) . ? C22 C23 1.415(9) . ? C23 C24 1.393(9) . ? C24 C33 1.389(9) . ? C24 C25 1.499(9) . ? C25 C26 1.404(8) . ? C25 C30 1.404(9) . ? C26 C27 1.383(9) . ? C27 C28 1.395(9) . ? C28 C29 1.392(8) . ? C28 C31 1.496(9) . ? C29 C30 1.375(9) . ? C33 C34 1.411(9) . ? C34 C35 1.362(9) . ? C35 C36 1.397(9) . ? C40 C41 1.401(10) . ? C41 C42 1.383(10) . ? C42 C43 1.421(9) . ? C43 C44 1.405(10) . ? C44 C53 1.410(9) . ? C44 C45 1.500(9) . ? C45 C52 1.385(9) . ? C45 C46 1.400(10) . ? C46 C47 1.386(10) . ? C47 C48 1.387(9) . ? C48 C51 1.395(10) . ? C48 C49 1.469(10) . ? C51 C52 1.391(9) . ? C53 C54 1.409(9) . ? C54 C55 1.360(9) . ? C55 C56 1.411(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Rh1 N3 89.9(2) . . ? N5 Rh1 N1 89.8(2) . . ? N3 Rh1 N1 91.3(2) . . ? N5 Rh1 N4 88.3(2) . . ? N3 Rh1 N4 89.5(2) . . ? N1 Rh1 N4 178.02(19) . . ? N5 Rh1 N2 178.3(2) . . ? N3 Rh1 N2 88.6(2) . . ? N1 Rh1 N2 91.0(2) . . ? N4 Rh1 N2 90.8(2) . . ? N5 Rh1 N6 89.8(2) . . ? N3 Rh1 N6 179.6(2) . . ? N1 Rh1 N6 88.5(2) . . ? N4 Rh1 N6 90.8(2) . . ? N2 Rh1 N6 91.7(2) . . ? C1 N1 C4 106.2(6) . . ? C1 N1 Rh1 127.1(5) . . ? C4 N1 Rh1 126.7(4) . . ? C16 N2 C17 105.9(6) . . ? C16 N2 Rh1 128.0(5) . . ? C17 N2 Rh1 126.1(4) . . ? C20 N3 C23 107.4(6) . . ? C20 N3 Rh1 125.5(5) . . ? C23 N3 Rh1 126.9(5) . . ? C36 N4 C33 105.6(6) . . ? C36 N4 Rh1 127.3(5) . . ? C33 N4 Rh1 126.6(4) . . ? C40 N5 C43 106.8(6) . . ? C40 N5 Rh1 126.1(5) . . ? C43 N5 Rh1 127.0(5) . . ? C56 N6 C53 105.5(6) . . ? C56 N6 Rh1 126.9(4) . . ? C53 N6 Rh1 126.9(5) . . ? C10 O2 C11 113.4(7) . . ? C31 O4 C32 114.7(5) . . ? C49 O5 C50 115.2(7) . . ? N1 C1 C2 110.3(7) . . ? C3 C2 C1 106.4(6) . . ? C2 C3 C4 107.6(7) . . ? N1 C4 C5 124.4(6) . . ? N1 C4 C3 109.5(6) . . ? C5 C4 C3 126.1(7) . . ? C17 C5 C4 127.1(7) . . ? C17 C5 C6 116.8(6) . . ? C4 C5 C6 116.1(6) . . ? C13 C6 C7 119.4(7) . . ? C13 C6 C5 120.9(7) . . ? C7 C6 C5 119.7(7) . . ? C8 C7 C6 119.2(7) . . ? C9 C8 C7 120.9(8) . . ? C12 C9 C8 120.2(8) . . ? C12 C9 C10 123.3(8) . . ? C8 C9 C10 116.5(8) . . ? O1 C10 O2 124.8(8) . . ? O1 C10 C9 124.8(8) . . ? O2 C10 C9 110.4(8) . . ? C9 C12 C13 120.3(7) . . ? C12 C13 C6 119.9(7) . . ? C15 C14 C17 106.9(7) . . ? C14 C15 C16 106.9(6) . . ? N2 C16 C15 111.9(7) . . ? C5 C17 N2 124.6(6) . . ? C5 C17 C14 127.0(7) . . ? N2 C17 C14 108.4(6) . . ? N3 C20 C21 111.0(7) . . ? C22 C21 C20 106.4(7) . . ? C21 C22 C23 108.1(7) . . ? C24 C23 N3 124.3(6) . . ? C24 C23 C22 128.6(7) . . ? N3 C23 C22 107.0(6) . . ? C33 C24 C23 127.5(7) . . ? C33 C24 C25 116.8(6) . . ? C23 C24 C25 115.8(6) . . ? C26 C25 C30 117.1(6) . . ? C26 C25 C24 121.4(6) . . ? C30 C25 C24 121.5(6) . . ? C27 C26 C25 121.8(7) . . ? C26 C27 C28 119.4(6) . . ? C29 C28 C27 119.9(7) . . ? C29 C28 C31 122.3(6) . . ? C27 C28 C31 117.7(6) . . ? C30 C29 C28 119.9(7) . . ? C29 C30 C25 121.8(6) . . ? O3 C31 O4 124.1(7) . . ? O3 C31 C28 123.4(7) . . ? O4 C31 C28 112.4(6) . . ? C24 C33 C34 129.6(7) . . ? C24 C33 N4 122.8(6) . . ? C34 C33 N4 107.4(6) . . ? C35 C34 C33 108.4(7) . . ? C34 C35 C36 106.0(6) . . ? N4 C36 C35 112.7(7) . . ? N5 C40 C41 110.8(7) . . ? C42 C41 C40 107.1(7) . . ? C41 C42 C43 107.1(7) . . ? N5 C43 C44 124.3(6) . . ? N5 C43 C42 108.2(7) . . ? C44 C43 C42 127.0(7) . . ? C43 C44 C53 126.7(7) . . ? C43 C44 C45 116.5(6) . . ? C53 C44 C45 116.7(6) . . ? C52 C45 C46 119.5(6) . . ? C52 C45 C44 120.9(7) . . ? C46 C45 C44 119.7(6) . . ? C47 C46 C45 120.0(7) . . ? C46 C47 C48 121.2(7) . . ? C47 C48 C51 118.3(7) . . ? C47 C48 C49 124.3(7) . . ? C51 C48 C49 117.3(7) . . ? O6 C49 O5 122.2(8) . . ? O6 C49 C48 125.8(9) . . ? O5 C49 C48 112.0(7) . . ? C52 C51 C48 121.2(7) . . ? C45 C52 C51 119.9(7) . . ? C54 C53 C44 128.6(6) . . ? C54 C53 N6 108.4(6) . . ? C44 C53 N6 122.9(6) . . ? C55 C54 C53 107.9(6) . . ? C54 C55 C56 105.8(6) . . ? N6 C56 C55 112.4(6) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.249 _refine_diff_density_min -2.673 _refine_diff_density_rms 0.121 __exptl_crystal_density_method 'not measured' # END data_[Rh(Lb)3] _database_code_depnum_ccdc_archive 'CCDC 737431' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 0.5(C48H33RhN6O6) _chemical_formula_sum 'C48 H37 N6 O8 Rh' _chemical_formula_weight 928.75 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' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Ibca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' _cell_length_a 13.5452(8) _cell_length_b 16.1898(9) _cell_length_c 40.0972(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8793.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 255 _cell_measurement_theta_min 26.11 _cell_measurement_theta_max 137.81 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3808 _exptl_absorpt_coefficient_mu 3.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5289 _exptl_absorpt_correction_T_max 0.9644 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rigaku MM007 rotating anode' _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3770 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 6.54 _diffrn_reflns_theta_max 71.93 _reflns_number_total 3770 _reflns_number_gt 2806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+62.4156P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3770 _refine_ls_number_parameters 278 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1714 _refine_ls_wR_factor_gt 0.1649 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.5000 0.2500 0.190728(14) 0.0430(2) Uani 1 2 d S . . N1 N 0.5920(4) 0.2123(3) 0.15366(11) 0.0467(12) Uani 1 1 d . . . N2 N 0.4354(4) 0.1354(3) 0.19079(11) 0.0456(12) Uani 1 1 d . . . N3 N 0.5950(4) 0.2102(3) 0.22660(11) 0.0454(12) Uani 1 1 d . . . O1 O -0.0080(4) 0.0111(4) 0.04454(12) 0.0794(15) Uani 1 1 d U . . H1 H -0.0392 -0.0021 0.0272 0.119 Uiso 1 1 calc . . . O2 O 0.1137(4) 0.0211(4) 0.00851(13) 0.0956(18) Uani 1 1 d U . . O3 O 0.5687(6) 0.2883(5) 0.43475(16) 0.113(2) Uani 1 1 d U . . H3 H 0.5637 0.2843 0.4556 0.170 Uiso 0.50 1 calc P . . C29 C 0.5000 0.2500 0.4213(3) 0.079(3) Uani 1 2 d S . . C5 C 0.4570(5) 0.0734(4) 0.21117(15) 0.0513(16) Uani 1 1 d . . . H5 H 0.5002 0.0771 0.2298 0.062 Uiso 1 1 calc R . . C13 C 0.1469(5) 0.0512(5) 0.06510(15) 0.0584(18) Uani 1 1 d . . . C22 C 0.6592(5) 0.1698(4) 0.27644(15) 0.0544(17) Uani 1 1 d . . . H22 H 0.6681 0.1616 0.2997 0.065 Uiso 1 1 calc R . . C7 C 0.3535(5) 0.0206(4) 0.17346(15) 0.0559(17) Uani 1 1 d . . . H7 H 0.3127 -0.0158 0.1610 0.067 Uiso 1 1 calc R . . C23 C 0.5814(5) 0.2132(4) 0.26108(14) 0.0471(15) Uani 1 1 d . . . C20 C 0.6785(5) 0.1681(4) 0.22127(15) 0.0527(16) Uani 1 1 d . . . H20 H 0.7061 0.1575 0.1999 0.063 Uiso 1 1 calc R . . C8 C 0.3706(4) 0.1047(4) 0.16674(14) 0.0478(15) Uani 1 1 d . . . C10 C 0.2678(5) 0.1096(4) 0.11542(14) 0.0505(15) Uani 1 1 d . . . C27 C 0.5675(6) 0.2975(5) 0.36627(17) 0.068(2) Uani 1 1 d . . . H27 H 0.6130 0.3307 0.3783 0.081 Uiso 1 1 calc R . . C14 C 0.2460(6) 0.0616(6) 0.05947(16) 0.074(2) Uani 1 1 d . . . H14 H 0.2732 0.0490 0.0382 0.089 Uiso 1 1 calc R . . C21 C 0.7197(5) 0.1419(5) 0.25162(16) 0.0591(18) Uani 1 1 d . . . H21 H 0.7785 0.1106 0.2544 0.071 Uiso 1 1 calc R . . C4 C 0.6014(5) 0.1368(5) 0.14121(15) 0.0578(18) Uani 1 1 d . . . H4 H 0.5685 0.0894 0.1497 0.069 Uiso 1 1 calc R . . C9 C 0.3327(5) 0.1518(4) 0.14045(14) 0.0486(15) Uani 1 1 d . . . C12 C 0.1083(5) 0.0673(4) 0.09628(15) 0.0577(18) Uani 1 1 d . . . H12 H 0.0401 0.0583 0.1005 0.069 Uiso 1 1 calc R . . C1 C 0.6523(5) 0.2648(4) 0.13444(14) 0.0507(16) Uani 1 1 d . . . C11 C 0.1688(5) 0.0965(4) 0.12128(15) 0.0553(17) Uani 1 1 d . . . H11 H 0.1421 0.1076 0.1427 0.066 Uiso 1 1 calc R . . C26 C 0.5691(5) 0.2968(4) 0.33152(15) 0.0592(18) Uani 1 1 d . . . H26 H 0.6172 0.3283 0.3199 0.071 Uiso 1 1 calc R . . C6 C 0.4067(5) 0.0013(4) 0.20136(15) 0.0584(18) Uani 1 1 d . . . H6 H 0.4093 -0.0510 0.2121 0.070 Uiso 1 1 calc R . . C2 C 0.6968(5) 0.2153(5) 0.10943(16) 0.0623(19) Uani 1 1 d . . . H2 H 0.7404 0.2344 0.0925 0.075 Uiso 1 1 calc R . . C16 C 0.0819(6) 0.0264(5) 0.03699(16) 0.067(2) Uani 1 1 d . . . C3 C 0.6665(5) 0.1358(5) 0.11371(16) 0.065(2) Uani 1 1 d . . . H103 H 0.6854 0.0892 0.1008 0.078 Uiso 1 1 calc R . . C25 C 0.5000 0.2500 0.31368(19) 0.051(2) Uani 1 2 d S . . C24 C 0.5000 0.2500 0.27628(18) 0.0431(19) Uani 1 2 d S . . C15 C 0.3061(6) 0.0903(5) 0.08462(17) 0.073(2) Uani 1 1 d . . . H15 H 0.3748 0.0970 0.0807 0.088 Uiso 1 1 calc R . . C28 C 0.5000 0.2500 0.3829(2) 0.069(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0427(4) 0.0531(5) 0.0331(3) 0.000 0.000 -0.0087(3) N1 0.053(3) 0.052(3) 0.035(2) -0.002(2) -0.002(2) -0.005(2) N2 0.047(3) 0.053(3) 0.037(2) 0.000(2) -0.001(2) -0.009(2) N3 0.043(3) 0.055(3) 0.039(2) -0.005(2) 0.000(2) -0.012(2) O1 0.067(3) 0.113(4) 0.058(2) -0.011(3) -0.006(2) -0.022(3) O2 0.081(3) 0.143(4) 0.062(3) -0.017(3) -0.003(3) -0.030(3) O3 0.124(4) 0.135(4) 0.081(3) -0.010(3) -0.014(3) -0.001(4) C29 0.087(9) 0.084(9) 0.065(7) 0.000 0.000 0.000(7) C5 0.053(4) 0.058(5) 0.043(3) 0.004(3) -0.002(3) -0.009(3) C13 0.057(4) 0.075(5) 0.043(3) -0.008(3) -0.006(3) -0.012(4) C22 0.049(4) 0.072(5) 0.042(3) 0.004(3) -0.004(3) 0.001(3) C7 0.057(4) 0.061(5) 0.049(3) -0.006(3) -0.006(3) -0.018(3) C23 0.048(4) 0.054(4) 0.039(3) 0.002(3) -0.004(3) -0.008(3) C20 0.041(4) 0.071(5) 0.046(3) -0.007(3) 0.002(3) -0.004(3) C8 0.044(4) 0.056(4) 0.043(3) -0.002(3) -0.002(3) -0.010(3) C10 0.054(4) 0.058(4) 0.039(3) -0.004(3) -0.004(3) -0.004(3) C27 0.081(6) 0.074(6) 0.049(4) -0.006(4) -0.015(4) 0.005(4) C14 0.054(5) 0.124(7) 0.045(4) -0.024(4) 0.000(3) -0.015(4) C21 0.050(4) 0.072(5) 0.055(4) 0.000(3) -0.008(3) 0.006(3) C4 0.066(5) 0.065(5) 0.042(3) -0.002(3) 0.005(3) -0.007(3) C9 0.046(4) 0.062(5) 0.038(3) -0.005(3) -0.005(3) -0.006(3) C12 0.052(4) 0.075(5) 0.046(3) -0.008(3) -0.002(3) -0.010(3) C1 0.049(4) 0.071(5) 0.032(3) 0.002(3) 0.008(3) -0.006(3) C11 0.054(4) 0.073(5) 0.039(3) -0.008(3) 0.003(3) -0.008(3) C26 0.067(5) 0.069(5) 0.042(3) -0.001(3) -0.007(3) -0.001(4) C6 0.071(5) 0.053(5) 0.052(3) 0.007(3) -0.001(3) -0.015(3) C2 0.068(5) 0.077(5) 0.042(3) -0.005(3) 0.011(3) -0.006(4) C16 0.061(5) 0.104(6) 0.037(3) -0.011(3) -0.004(3) -0.022(4) C3 0.071(5) 0.073(6) 0.052(4) -0.014(3) 0.014(4) 0.000(4) C25 0.057(6) 0.062(6) 0.034(4) 0.000 0.000 0.004(5) C24 0.044(5) 0.058(6) 0.027(3) 0.000 0.000 -0.010(4) C15 0.051(4) 0.114(7) 0.053(4) -0.020(4) 0.003(3) -0.011(4) C28 0.083(8) 0.081(8) 0.043(5) 0.000 0.000 0.009(6) _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 Rh1 N1 2.034(5) 6_554 ? Rh1 N1 2.034(5) . ? Rh1 N3 2.034(5) . ? Rh1 N3 2.034(5) 6_554 ? Rh1 N2 2.051(5) 6_554 ? Rh1 N2 2.051(5) . ? N1 C4 1.327(8) . ? N1 C1 1.409(8) . ? N2 C5 1.327(8) . ? N2 C8 1.395(7) . ? N3 C20 1.338(8) . ? N3 C23 1.396(7) . ? O1 C16 1.278(8) . ? O2 C16 1.224(8) . ? O3 C29 1.242(8) . ? C29 O3 1.242(8) 6_554 ? C29 C28 1.539(15) . ? C5 C6 1.408(9) . ? C13 C14 1.372(10) . ? C13 C12 1.380(8) . ? C13 C16 1.486(8) . ? C22 C21 1.366(9) . ? C22 C23 1.409(8) . ? C7 C6 1.367(9) . ? C7 C8 1.408(9) . ? C23 C24 1.393(7) . ? C20 C21 1.405(9) . ? C8 C9 1.398(8) . ? C10 C15 1.375(8) . ? C10 C11 1.377(9) . ? C10 C9 1.499(8) . ? C27 C28 1.368(9) . ? C27 C26 1.393(9) . ? C14 C15 1.376(9) . ? C4 C3 1.413(9) . ? C9 C1 1.387(9) 6_554 ? C12 C11 1.379(8) . ? C1 C9 1.387(9) 6_554 ? C1 C2 1.418(9) . ? C26 C25 1.401(8) . ? C2 C3 1.362(10) . ? C25 C26 1.401(8) 6_554 ? C25 C24 1.500(10) . ? C24 C23 1.393(7) 6_554 ? C28 C27 1.368(9) 6_554 ? 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 Rh1 N1 86.1(3) 6_554 . ? N1 Rh1 N3 178.0(2) 6_554 . ? N1 Rh1 N3 92.0(2) . . ? N1 Rh1 N3 92.0(2) 6_554 6_554 ? N1 Rh1 N3 178.00(19) . 6_554 ? N3 Rh1 N3 90.0(3) . 6_554 ? N1 Rh1 N2 89.5(2) 6_554 6_554 ? N1 Rh1 N2 90.6(2) . 6_554 ? N3 Rh1 N2 90.88(19) . 6_554 ? N3 Rh1 N2 89.01(19) 6_554 6_554 ? N1 Rh1 N2 90.6(2) 6_554 . ? N1 Rh1 N2 89.5(2) . . ? N3 Rh1 N2 89.01(19) . . ? N3 Rh1 N2 90.88(19) 6_554 . ? N2 Rh1 N2 179.9(2) 6_554 . ? C4 N1 C1 107.2(5) . . ? C4 N1 Rh1 127.6(4) . . ? C1 N1 Rh1 125.0(4) . . ? C5 N2 C8 107.1(5) . . ? C5 N2 Rh1 126.2(4) . . ? C8 N2 Rh1 126.1(4) . . ? C20 N3 C23 106.7(5) . . ? C20 N3 Rh1 125.7(4) . . ? C23 N3 Rh1 127.3(4) . . ? O3 C29 O3 128.5(12) . 6_554 ? O3 C29 C28 115.8(6) . . ? O3 C29 C28 115.8(6) 6_554 . ? N2 C5 C6 110.4(6) . . ? C14 C13 C12 119.8(6) . . ? C14 C13 C16 119.2(6) . . ? C12 C13 C16 120.9(6) . . ? C21 C22 C23 107.2(5) . . ? C6 C7 C8 106.9(6) . . ? C24 C23 N3 123.5(6) . . ? C24 C23 C22 127.9(5) . . ? N3 C23 C22 108.5(6) . . ? N3 C20 C21 110.6(6) . . ? N2 C8 C9 123.9(6) . . ? N2 C8 C7 108.4(5) . . ? C9 C8 C7 127.6(6) . . ? C15 C10 C11 119.0(6) . . ? C15 C10 C9 118.9(6) . . ? C11 C10 C9 121.8(5) . . ? C28 C27 C26 119.6(8) . . ? C13 C14 C15 120.0(6) . . ? C22 C21 C20 107.0(6) . . ? N1 C4 C3 111.3(6) . . ? C1 C9 C8 127.4(6) 6_554 . ? C1 C9 C10 114.4(5) 6_554 . ? C8 C9 C10 118.2(6) . . ? C11 C12 C13 119.9(6) . . ? C9 C1 N1 125.3(5) 6_554 . ? C9 C1 C2 127.7(6) 6_554 . ? N1 C1 C2 107.0(6) . . ? C10 C11 C12 120.5(6) . . ? C27 C26 C25 120.3(7) . . ? C7 C6 C5 107.1(6) . . ? C3 C2 C1 108.5(6) . . ? O2 C16 O1 122.9(6) . . ? O2 C16 C13 121.2(7) . . ? O1 C16 C13 115.9(6) . . ? C2 C3 C4 106.0(6) . . ? C26 C25 C26 118.6(8) . 6_554 ? C26 C25 C24 120.7(4) . . ? C26 C25 C24 120.7(4) 6_554 . ? C23 C24 C23 128.1(7) 6_554 . ? C23 C24 C25 115.9(4) 6_554 . ? C23 C24 C25 115.9(4) . . ? C10 C15 C14 120.8(7) . . ? C27 C28 C27 121.6(9) 6_554 . ? C27 C28 C29 119.2(5) 6_554 . ? C27 C28 C29 119.2(5) . . ? 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 -0.021 0.750 0.000 327 39 ' ' 2 -0.027 0.250 0.500 327 39 ' ' 3 -0.016 0.750 0.500 327 39 ' ' 4 -0.027 0.250 1.000 327 39 ' ' _platon_squeeze_details ; The final R factor was obtained after implementing the squeeze routine in Platon to account for severely disordered solvent H2O molecules, which appeared to be H-bonded to one of the carboxyl groups (O3). A void space of 1301 \%A3 was calculated (15% of the unit cell volume) along an electron count per cell of 158. This corresponds almost exactly to 16 H2O molecules per unit cell hence the molecular weight, density and F000 were calculated using the formula C48H33RhN6O6?2H2O. ; _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 71.93 _diffrn_measured_fraction_theta_full 0.872 _refine_diff_density_max 0.628 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.084 # END data_[Pd(La)2] _database_code_depnum_ccdc_archive 'CCDC 737432' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (C34H26PdN4O4) _chemical_formula_sum 'C34 H26 N4 O4 Pd' _chemical_formula_weight 660.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' Pd Pd 0.1215 3.9337 '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 22.40416(82) _cell_length_b 12.56646(51) _cell_length_c 10.03459(46) _cell_angle_alpha 90.00 _cell_angle_beta 90.4148(25) _cell_angle_gamma 90.00 _cell_volume 2825.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4035 _cell_measurement_theta_min 13.75 _cell_measurement_theta_max 138.05 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.003 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 5.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7265 _exptl_absorpt_correction_T_max 0.9831 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rigaku MM007 rotating anode' _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39410 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.0911 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 6.87 _diffrn_reflns_theta_max 66.60 _reflns_number_total 4970 _reflns_number_gt 3618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+9.7782P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00020(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4970 _refine_ls_number_parameters 391 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1887 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.005 _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 Pd1 Pd 0.25082(2) 0.01288(4) 0.28929(6) 0.0322(2) Uani 1 1 d . . . N1 N 0.2434(2) 0.1459(5) 0.1779(6) 0.0369(15) Uani 1 1 d . . . N2 N 0.3355(2) 0.0540(4) 0.3193(5) 0.0284(13) Uani 1 1 d . . . N3 N 0.2589(2) -0.1202(4) 0.3990(7) 0.0401(16) Uani 1 1 d . . . N4 N 0.1658(2) -0.0275(4) 0.2592(6) 0.0303(14) Uani 1 1 d . . . O1 O 0.4632(3) 0.6555(4) 0.5324(6) 0.0540(15) Uani 1 1 d . . . O2 O 0.4551(2) 0.7031(3) 0.3184(5) 0.0366(12) Uani 1 1 d . . . O3 O 0.0480(3) -0.6362(4) 0.0533(6) 0.0572(16) Uani 1 1 d . . . O4 O 0.0701(3) -0.7021(4) 0.2562(6) 0.0579(16) Uani 1 1 d . . . C1 C 0.2051(3) 0.1657(6) 0.0776(8) 0.0368(18) Uani 1 1 d . . . H1 H 0.1821 0.1132 0.0326 0.044 Uiso 1 1 calc R . . C2 C 0.2040(3) 0.2756(6) 0.0483(8) 0.0399(19) Uani 1 1 d . . . H2 H 0.1805 0.3092 -0.0186 0.048 Uiso 1 1 calc R . . C3 C 0.2431(3) 0.3250(6) 0.1341(8) 0.0384(18) Uani 1 1 d . . . H3 H 0.2507 0.3992 0.1400 0.046 Uiso 1 1 calc R . . C4 C 0.2703(3) 0.2427(5) 0.2130(8) 0.0324(17) Uani 1 1 d . . . C5 C 0.3215(3) 0.2487(5) 0.2914(7) 0.0292(15) Uani 1 1 d . . . C6 C 0.3548(3) 0.1596(5) 0.3345(7) 0.0307(16) Uani 1 1 d . . . C7 C 0.4164(3) 0.1586(5) 0.3682(7) 0.0346(17) Uani 1 1 d . . . H7 H 0.4407 0.2189 0.3864 0.042 Uiso 1 1 calc R . . C8 C 0.4342(3) 0.0551(5) 0.3694(7) 0.0331(17) Uani 1 1 d . . . H8 H 0.4733 0.0296 0.3877 0.040 Uiso 1 1 calc R . . C9 C 0.3837(3) -0.0072(5) 0.3385(7) 0.0295(16) Uani 1 1 d . . . H9 H 0.3838 -0.0827 0.3320 0.035 Uiso 1 1 calc R . . C10 C 0.3689(3) 0.4222(5) 0.2186(7) 0.0266(15) Uani 1 1 d . . . H10 H 0.3612 0.4047 0.1279 0.032 Uiso 1 1 calc R . . C11 C 0.3988(3) 0.5145(5) 0.2511(8) 0.0290(16) Uani 1 1 d . . . H11 H 0.4116 0.5605 0.1819 0.035 Uiso 1 1 calc R . . C12 C 0.3608(3) 0.3827(5) 0.4534(8) 0.0351(17) Uani 1 1 d . . . H12 H 0.3476 0.3374 0.5230 0.042 Uiso 1 1 calc R . . C13 C 0.3907(3) 0.4759(5) 0.4848(8) 0.0353(17) Uani 1 1 d . . . H13 H 0.3977 0.4949 0.5752 0.042 Uiso 1 1 calc R . . C14 C 0.4104(3) 0.5415(5) 0.3820(7) 0.0297(15) Uani 1 1 d . . . C15 C 0.4454(3) 0.6376(6) 0.4207(9) 0.0367(18) Uani 1 1 d . . . C16 C 0.4929(3) 0.7936(5) 0.3490(8) 0.0418(19) Uani 1 1 d . . . H16A H 0.4758 0.8336 0.4234 0.063 Uiso 1 1 calc R . . H16B H 0.4956 0.8398 0.2706 0.063 Uiso 1 1 calc R . . H16C H 0.5329 0.7685 0.3738 0.063 Uiso 1 1 calc R . . C17 C 0.3498(3) 0.3542(5) 0.3211(7) 0.0306(16) Uani 1 1 d . . . C20 C 0.2983(3) -0.1433(6) 0.4969(8) 0.0370(18) Uani 1 1 d . . . H20 H 0.3217 -0.0918 0.5430 0.044 Uiso 1 1 calc R . . C21 C 0.3005(3) -0.2536(5) 0.5222(8) 0.0380(18) Uani 1 1 d . . . H21 H 0.3250 -0.2887 0.5862 0.046 Uiso 1 1 calc R . . C22 C 0.2608(3) -0.2997(6) 0.4374(8) 0.0380(18) Uani 1 1 d . . . H22 H 0.2533 -0.3739 0.4296 0.046 Uiso 1 1 calc R . . C23 C 0.2322(3) -0.2173(5) 0.3613(7) 0.0297(16) Uani 1 1 d . . . C24 C 0.1798(3) -0.2224(5) 0.2892(8) 0.0332(17) Uani 1 1 d . . . C25 C 0.1463(3) -0.1340(5) 0.2484(7) 0.0322(16) Uani 1 1 d . . . C26 C 0.0842(3) -0.1318(6) 0.2139(7) 0.0375(18) Uani 1 1 d . . . H26 H 0.0595 -0.1917 0.1966 0.045 Uiso 1 1 calc R . . C27 C 0.0670(3) -0.0272(6) 0.2106(8) 0.0360(18) Uani 1 1 d . . . H27 H 0.0280 -0.0011 0.1921 0.043 Uiso 1 1 calc R . . C28 C 0.1182(3) 0.0351(6) 0.2398(8) 0.0363(17) Uani 1 1 d . . . H28 H 0.1187 0.1105 0.2450 0.044 Uiso 1 1 calc R . . C29 C 0.1523(3) -0.3285(5) 0.2615(8) 0.0352(17) Uani 1 1 d . . . C30 C 0.1423(3) -0.3600(5) 0.1295(8) 0.0393(18) Uani 1 1 d . . . H30 H 0.1538 -0.3143 0.0586 0.047 Uiso 1 1 calc R . . C31 C 0.1160(3) -0.4565(6) 0.1014(9) 0.0425(19) Uani 1 1 d . . . H31 H 0.1089 -0.4761 0.0112 0.051 Uiso 1 1 calc R . . C32 C 0.0997(3) -0.5255(5) 0.2026(9) 0.0363(18) Uani 1 1 d . . . C33 C 0.1094(3) -0.4944(5) 0.3319(9) 0.039(2) Uani 1 1 d . . . H33 H 0.0979 -0.5409 0.4018 0.047 Uiso 1 1 calc R . . C34 C 0.1353(3) -0.3978(5) 0.3644(8) 0.0336(16) Uani 1 1 d . . . H34 H 0.1414 -0.3785 0.4550 0.040 Uiso 1 1 calc R . . C35 C 0.0719(3) -0.6307(6) 0.1752(10) 0.047(2) Uani 1 1 d . . . C36 C 0.0181(4) -0.7360(8) 0.0258(11) 0.072(3) Uani 1 1 d U . . H36A H 0.0470 -0.7944 0.0301 0.108 Uiso 1 1 calc R . . H36B H 0.0000 -0.7335 -0.0634 0.108 Uiso 1 1 calc R . . H36C H -0.0132 -0.7478 0.0921 0.108 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 Pd1 0.0298(3) 0.0284(3) 0.0384(4) 0.0004(2) 0.0000(3) -0.00349(19) N1 0.030(3) 0.037(3) 0.044(4) -0.006(3) 0.004(3) -0.007(2) N2 0.034(3) 0.025(3) 0.026(4) 0.000(2) 0.001(3) -0.005(2) N3 0.026(3) 0.029(3) 0.065(5) -0.010(3) 0.006(3) -0.005(2) N4 0.031(3) 0.027(3) 0.033(4) -0.003(2) 0.005(3) -0.002(2) O1 0.077(4) 0.042(3) 0.042(4) 0.003(3) -0.009(3) -0.020(3) O2 0.044(3) 0.028(2) 0.038(3) 0.001(2) -0.001(2) -0.009(2) O3 0.059(4) 0.056(4) 0.056(4) -0.022(3) -0.002(3) -0.017(3) O4 0.068(4) 0.041(3) 0.066(5) -0.007(3) 0.015(3) -0.014(3) C1 0.031(4) 0.040(4) 0.039(5) -0.002(3) -0.005(3) -0.007(3) C2 0.035(4) 0.046(4) 0.039(5) 0.005(4) -0.001(4) 0.004(3) C3 0.034(4) 0.038(4) 0.044(5) 0.007(4) 0.007(3) -0.001(3) C4 0.036(4) 0.022(3) 0.039(5) 0.002(3) 0.007(3) -0.003(3) C5 0.031(3) 0.029(3) 0.028(4) -0.002(3) 0.001(3) -0.008(3) C6 0.032(3) 0.034(4) 0.026(4) -0.001(3) -0.002(3) -0.006(3) C7 0.029(3) 0.032(4) 0.042(5) 0.004(3) -0.008(3) -0.012(3) C8 0.033(4) 0.029(4) 0.038(5) 0.008(3) 0.003(3) -0.004(3) C9 0.031(4) 0.034(4) 0.024(4) -0.005(3) 0.003(3) 0.002(3) C10 0.033(3) 0.033(4) 0.013(4) -0.004(3) -0.005(3) -0.001(3) C11 0.036(4) 0.027(3) 0.024(5) 0.000(3) 0.008(3) 0.003(3) C12 0.044(4) 0.034(4) 0.027(5) -0.005(3) 0.007(3) -0.006(3) C13 0.047(4) 0.036(4) 0.023(5) 0.003(3) 0.008(3) -0.003(3) C14 0.033(3) 0.031(3) 0.025(4) 0.002(3) 0.002(3) -0.003(3) C15 0.035(4) 0.034(4) 0.041(5) 0.000(3) -0.001(4) -0.007(3) C16 0.046(4) 0.029(4) 0.050(6) -0.008(3) 0.004(4) -0.009(3) C17 0.032(3) 0.026(3) 0.034(5) 0.001(3) 0.005(3) -0.001(3) C20 0.028(3) 0.037(4) 0.046(5) -0.004(3) -0.006(3) -0.005(3) C21 0.038(4) 0.034(4) 0.042(5) 0.011(3) 0.001(4) -0.001(3) C22 0.041(4) 0.030(4) 0.043(5) -0.002(3) 0.000(4) -0.005(3) C23 0.029(3) 0.026(3) 0.034(5) 0.006(3) -0.002(3) -0.005(3) C24 0.032(4) 0.026(3) 0.042(5) 0.001(3) 0.004(3) -0.011(3) C25 0.032(3) 0.038(4) 0.027(4) 0.006(3) 0.004(3) -0.007(3) C26 0.034(4) 0.043(4) 0.035(5) 0.005(3) -0.005(3) -0.006(3) C27 0.028(4) 0.044(4) 0.036(5) 0.006(3) 0.001(3) 0.000(3) C28 0.035(4) 0.036(4) 0.038(5) -0.001(3) 0.008(3) -0.003(3) C29 0.037(4) 0.030(4) 0.038(5) 0.001(3) 0.009(3) -0.005(3) C30 0.050(4) 0.031(4) 0.037(5) 0.004(3) 0.008(4) -0.006(3) C31 0.045(4) 0.041(4) 0.041(5) -0.003(4) 0.000(4) -0.006(4) C32 0.035(4) 0.031(4) 0.043(6) -0.008(3) 0.006(4) -0.002(3) C33 0.037(4) 0.030(4) 0.050(6) 0.002(3) 0.011(4) -0.007(3) C34 0.032(4) 0.041(4) 0.027(5) -0.003(3) -0.003(3) -0.003(3) C35 0.044(4) 0.035(4) 0.062(7) -0.011(4) 0.020(4) -0.005(3) C36 0.070(4) 0.071(4) 0.076(5) -0.024(4) 0.001(4) -0.018(4) _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 Pd1 N2 1.988(5) . ? Pd1 N4 1.992(5) . ? Pd1 N3 2.009(6) . ? Pd1 N1 2.017(6) . ? N1 C1 1.340(9) . ? N1 C4 1.402(8) . ? N2 C9 1.338(8) . ? N2 C6 1.403(8) . ? N3 C20 1.349(9) . ? N3 C23 1.409(8) . ? N4 C28 1.337(9) . ? N4 C25 1.412(8) . ? O1 C15 1.208(9) . ? O2 C15 1.335(8) . ? O2 C16 1.450(7) . ? O3 C35 1.333(10) . ? O3 C36 1.449(10) . ? O4 C35 1.212(10) . ? C1 C2 1.413(10) . ? C2 C3 1.372(10) . ? C3 C4 1.435(9) . ? C4 C5 1.389(9) . ? C5 C6 1.412(9) . ? C5 C17 1.498(8) . ? C6 C7 1.420(9) . ? C7 C8 1.360(9) . ? C8 C9 1.408(9) . ? C10 C11 1.378(9) . ? C10 C17 1.407(9) . ? C11 C14 1.379(10) . ? C12 C13 1.384(9) . ? C12 C17 1.395(10) . ? C13 C14 1.395(10) . ? C14 C15 1.489(9) . ? C20 C21 1.410(9) . ? C21 C22 1.356(10) . ? C22 C23 1.436(9) . ? C23 C24 1.376(9) . ? C24 C25 1.400(9) . ? C24 C29 1.494(9) . ? C25 C26 1.432(9) . ? C26 C27 1.371(10) . ? C27 C28 1.418(10) . ? C29 C30 1.399(10) . ? C29 C34 1.405(9) . ? C30 C31 1.377(10) . ? C31 C32 1.386(11) . ? C32 C33 1.371(11) . ? C32 C35 1.486(10) . ? C33 C34 1.383(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 N4 179.7(2) . . ? N2 Pd1 N3 93.0(2) . . ? N4 Pd1 N3 87.3(2) . . ? N2 Pd1 N1 86.8(2) . . ? N4 Pd1 N1 93.0(2) . . ? N3 Pd1 N1 179.4(2) . . ? C1 N1 C4 107.4(6) . . ? C1 N1 Pd1 128.3(5) . . ? C4 N1 Pd1 123.1(5) . . ? C9 N2 C6 106.4(5) . . ? C9 N2 Pd1 129.8(4) . . ? C6 N2 Pd1 123.7(4) . . ? C20 N3 C23 106.5(6) . . ? C20 N3 Pd1 129.3(5) . . ? C23 N3 Pd1 122.5(5) . . ? C28 N4 C25 107.5(6) . . ? C28 N4 Pd1 129.2(5) . . ? C25 N4 Pd1 123.2(4) . . ? C15 O2 C16 114.7(6) . . ? C35 O3 C36 113.7(7) . . ? N1 C1 C2 110.4(6) . . ? C3 C2 C1 107.6(7) . . ? C2 C3 C4 106.6(6) . . ? C5 C4 N1 122.8(6) . . ? C5 C4 C3 128.2(6) . . ? N1 C4 C3 107.9(6) . . ? C4 C5 C6 124.3(6) . . ? C4 C5 C17 120.5(6) . . ? C6 C5 C17 114.8(6) . . ? N2 C6 C5 123.8(6) . . ? N2 C6 C7 108.4(6) . . ? C5 C6 C7 126.2(6) . . ? C8 C7 C6 107.1(6) . . ? C7 C8 C9 107.2(6) . . ? N2 C9 C8 110.9(6) . . ? C11 C10 C17 119.2(6) . . ? C10 C11 C14 121.4(7) . . ? C13 C12 C17 121.0(7) . . ? C12 C13 C14 119.2(7) . . ? C11 C14 C13 120.0(6) . . ? C11 C14 C15 123.0(6) . . ? C13 C14 C15 117.0(7) . . ? O1 C15 O2 122.9(6) . . ? O1 C15 C14 124.3(7) . . ? O2 C15 C14 112.8(7) . . ? C12 C17 C10 119.2(6) . . ? C12 C17 C5 119.2(6) . . ? C10 C17 C5 121.5(6) . . ? N3 C20 C21 111.4(6) . . ? C22 C21 C20 106.6(7) . . ? C21 C22 C23 108.3(6) . . ? C24 C23 N3 122.7(6) . . ? C24 C23 C22 128.4(6) . . ? N3 C23 C22 107.2(6) . . ? C23 C24 C25 124.7(6) . . ? C23 C24 C29 119.3(6) . . ? C25 C24 C29 115.7(6) . . ? C24 C25 N4 124.5(6) . . ? C24 C25 C26 127.2(6) . . ? N4 C25 C26 107.4(6) . . ? C27 C26 C25 107.3(6) . . ? C26 C27 C28 107.3(6) . . ? N4 C28 C27 110.4(6) . . ? C30 C29 C34 118.6(6) . . ? C30 C29 C24 119.4(6) . . ? C34 C29 C24 122.0(7) . . ? C31 C30 C29 120.5(7) . . ? C30 C31 C32 121.0(8) . . ? C33 C32 C31 118.3(7) . . ? C33 C32 C35 119.5(7) . . ? C31 C32 C35 122.2(8) . . ? C32 C33 C34 122.4(7) . . ? C33 C34 C29 119.1(7) . . ? O4 C35 O3 124.2(8) . . ? O4 C35 C32 123.3(9) . . ? O3 C35 C32 112.4(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 66.60 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.184 _refine_diff_density_min -1.970 _refine_diff_density_rms 0.156 # END