# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email thiel@chemie.uni-kl.de _publ_contact_author_name 'Thiel, Werner' loop_ _publ_author_name 'Thomas Jozak' 'Yu Sun' 'Werner Thiel' data_1014o _database_code_depnum_ccdc_archive 'CCDC 814851' #TrackingRef '- 1014o.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H14 N4 O2' _chemical_formula_weight 234.26 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 7.7765(6) _cell_length_b 8.3430(6) _cell_length_c 9.3377(8) _cell_angle_alpha 91.786(6) _cell_angle_beta 106.387(7) _cell_angle_gamma 90.049(6) _cell_volume 580.90(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2250 _cell_measurement_theta_min 4.9384 _cell_measurement_theta_max 62.4676 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 248 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86108 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _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 16.1399 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3155 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.94 _diffrn_reflns_theta_max 62.62 _reflns_number_total 2248 _reflns_number_gt 2146 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0678P)^2^+0.1646P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(3) _refine_ls_number_reflns 2248 _refine_ls_number_parameters 311 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.067 _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 C1 C 0.7097(5) 0.3672(4) 0.6377(4) 0.0238(7) Uani 1 1 d . . . C2 C 0.5271(5) 0.3779(5) 0.6224(4) 0.0342(9) Uani 1 1 d . . . H2 H 0.4390 0.4300 0.5469 0.041 Uiso 1 1 calc R . . C3 C 0.5024(5) 0.2965(5) 0.7408(4) 0.0355(9) Uani 1 1 d . . . H3 H 0.3916 0.2797 0.7624 0.043 Uiso 1 1 calc R . . C4 C 0.8061(5) 0.4278(4) 0.5324(4) 0.0226(7) Uani 1 1 d . . . H4 H 0.7298 0.5078 0.4661 0.027 Uiso 1 1 calc R . . C5 C 0.9937(4) 0.4988(4) 0.6020(4) 0.0232(7) Uani 1 1 d . . . H5 H 1.0553 0.4397 0.6937 0.028 Uiso 1 1 calc R . . C6 C 0.9977(5) 0.6739(4) 0.6383(4) 0.0240(7) Uani 1 1 d . . . C7 C 0.9058(5) 0.7969(4) 0.5485(4) 0.0311(8) Uani 1 1 d . . . H7 H 0.8246 0.7869 0.4512 0.037 Uiso 1 1 calc R . . C8 C 0.9603(6) 0.9347(4) 0.6339(5) 0.0362(9) Uani 1 1 d . . . H8 H 0.9234 1.0407 0.6068 0.043 Uiso 1 1 calc R . . C9 C 0.9796(5) 0.3486(4) 0.3808(4) 0.0276(8) Uani 1 1 d . . . C10 C 1.0975(6) 0.2089(5) 0.3702(5) 0.0433(11) Uani 1 1 d . . . H10A H 1.1905 0.2428 0.3250 0.065 Uiso 1 1 calc R . . H10B H 1.0251 0.1225 0.3083 0.065 Uiso 1 1 calc R . . H10C H 1.1540 0.1702 0.4705 0.065 Uiso 1 1 calc R . . C11 C 0.9052(6) 0.4293(5) 0.2331(5) 0.0417(10) Uani 1 1 d . . . H11A H 0.8258 0.5165 0.2456 0.063 Uiso 1 1 calc R . . H11B H 0.8375 0.3507 0.1582 0.063 Uiso 1 1 calc R . . H11C H 1.0042 0.4729 0.2002 0.063 Uiso 1 1 calc R . . N1 N 0.6617(4) 0.2455(4) 0.8193(4) 0.0319(7) Uani 1 1 d . . . H1N H 0.6792 0.1909 0.9012 0.038 Uiso 1 1 calc R . . N2 N 0.7953(4) 0.2870(3) 0.7593(3) 0.0273(7) Uani 1 1 d . . . N3 N 1.0754(5) 0.8912(4) 0.7624(4) 0.0365(8) Uani 1 1 d . . . H3N H 1.1282 0.9598 0.8350 0.044 Uiso 1 1 calc R . . N4 N 1.1020(4) 0.7322(3) 0.7691(3) 0.0306(7) Uani 1 1 d . . . O1 O 0.8423(3) 0.2960(3) 0.4430(3) 0.0265(6) Uani 1 1 d . . . O2 O 1.0816(3) 0.4670(3) 0.4873(3) 0.0286(6) Uani 1 1 d . . . C12 C 0.4272(5) 0.8501(4) 0.2926(4) 0.0292(8) Uani 1 1 d . . . C13 C 0.4585(5) 0.9345(4) 0.4290(5) 0.0347(9) Uani 1 1 d . . . H13 H 0.5290 1.0289 0.4609 0.042 Uiso 1 1 calc R . . C14 C 0.3648(5) 0.8507(5) 0.5065(4) 0.0329(8) Uani 1 1 d . . . H14 H 0.3560 0.8764 0.6040 0.039 Uiso 1 1 calc R . . C15 C 0.4836(5) 0.8821(5) 0.1549(4) 0.0347(9) Uani 1 1 d . . . H15 H 0.3844 0.8529 0.0633 0.042 Uiso 1 1 calc R . . C16 C 0.5487(5) 1.0498(5) 0.1460(5) 0.0352(9) Uani 1 1 d . . . H16 H 0.6236 1.0879 0.2469 0.042 Uiso 1 1 calc R . . C17 C 0.4067(5) 1.1715(4) 0.0844(4) 0.0308(8) Uani 1 1 d . . . C18 C 0.4173(5) 1.3329(5) 0.1222(4) 0.0342(9) Uani 1 1 d . . . H18 H 0.5138 1.3878 0.1919 0.041 Uiso 1 1 calc R . . C19 C 0.2634(5) 1.3970(4) 0.0403(4) 0.0326(9) Uani 1 1 d . . . H19 H 0.2306 1.5066 0.0412 0.039 Uiso 1 1 calc R . . C20 C 0.7119(5) 0.8571(4) 0.0465(4) 0.0314(8) Uani 1 1 d . . . C21 C 0.9130(6) 0.8486(5) 0.0955(6) 0.0449(10) Uani 1 1 d . . . H21A H 0.9580 0.8897 0.1989 0.067 Uiso 1 1 calc R . . H21B H 0.9622 0.9137 0.0305 0.067 Uiso 1 1 calc R . . H21C H 0.9498 0.7369 0.0890 0.067 Uiso 1 1 calc R . . C22 C 0.6334(7) 0.7848(8) -0.1068(5) 0.0642(15) Uani 1 1 d . . . H22A H 0.6532 0.6688 -0.1050 0.096 Uiso 1 1 calc R . . H22B H 0.6913 0.8325 -0.1761 0.096 Uiso 1 1 calc R . . H22C H 0.5045 0.8057 -0.1396 0.096 Uiso 1 1 calc R . . N5 N 0.2884(4) 0.7265(4) 0.4191(4) 0.0344(8) Uani 1 1 d . . . H5N H 0.2214 0.6544 0.4453 0.041 Uiso 1 1 calc R . . N6 N 0.3245(5) 0.7227(4) 0.2866(4) 0.0362(8) Uani 1 1 d . . . N7 N 0.1653(4) 1.2777(3) -0.0424(3) 0.0303(7) Uani 1 1 d . . . H7N H 0.0586 1.2902 -0.1055 0.036 Uiso 1 1 calc R . . N8 N 0.2503(4) 1.1356(3) -0.0175(3) 0.0312(7) Uani 1 1 d . . . O3 O 0.6436(3) 0.7904(3) 0.1568(3) 0.0313(6) Uani 1 1 d . . . O4 O 0.6627(4) 1.0271(4) 0.0471(4) 0.0508(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0263(18) 0.0209(15) 0.0269(18) -0.0002(13) 0.0121(15) -0.0004(14) C2 0.0222(19) 0.045(2) 0.037(2) 0.0096(17) 0.0090(16) 0.0013(17) C3 0.0232(19) 0.048(2) 0.042(2) 0.0107(18) 0.0179(17) 0.0024(17) C4 0.0232(17) 0.0223(16) 0.0234(18) 0.0011(13) 0.0083(14) 0.0011(13) C5 0.0245(18) 0.0213(16) 0.0262(18) 0.0038(13) 0.0107(14) 0.0004(13) C6 0.0273(18) 0.0233(17) 0.0246(17) -0.0001(13) 0.0128(14) -0.0041(14) C7 0.034(2) 0.0268(17) 0.034(2) 0.0011(14) 0.0116(16) 0.0029(15) C8 0.044(2) 0.0235(18) 0.048(2) -0.0012(16) 0.025(2) 0.0001(16) C9 0.0264(19) 0.0291(18) 0.0298(19) -0.0030(14) 0.0122(15) -0.0039(15) C10 0.043(2) 0.030(2) 0.065(3) -0.0108(19) 0.031(2) -0.0005(18) C11 0.035(2) 0.060(3) 0.035(2) 0.0062(18) 0.0157(18) -0.005(2) N1 0.0336(18) 0.0367(16) 0.0318(17) 0.0114(13) 0.0187(14) 0.0009(14) N2 0.0269(16) 0.0309(15) 0.0278(16) 0.0059(12) 0.0132(13) -0.0014(13) N3 0.046(2) 0.0298(16) 0.0375(19) -0.0112(14) 0.0185(16) -0.0104(14) N4 0.0338(17) 0.0267(15) 0.0321(17) -0.0008(13) 0.0109(14) -0.0056(13) O1 0.0294(13) 0.0253(12) 0.0281(13) -0.0062(10) 0.0141(10) -0.0086(10) O2 0.0263(13) 0.0277(12) 0.0370(14) -0.0033(10) 0.0177(11) -0.0061(10) C12 0.032(2) 0.0232(18) 0.038(2) 0.0096(15) 0.0197(17) 0.0105(16) C13 0.031(2) 0.0312(19) 0.044(2) 0.0024(17) 0.0156(17) -0.0048(17) C14 0.035(2) 0.040(2) 0.029(2) 0.0053(16) 0.0159(17) 0.0060(17) C15 0.037(2) 0.0348(19) 0.037(2) 0.0080(16) 0.0170(17) 0.0086(17) C16 0.030(2) 0.042(2) 0.037(2) 0.0074(16) 0.0143(17) 0.0018(16) C17 0.028(2) 0.043(2) 0.0243(18) 0.0109(16) 0.0122(16) 0.0065(17) C18 0.028(2) 0.043(2) 0.033(2) -0.0073(17) 0.0115(17) -0.0107(17) C19 0.039(2) 0.0232(18) 0.043(2) -0.0025(16) 0.0240(19) 0.0011(16) C20 0.033(2) 0.0340(19) 0.033(2) 0.0082(15) 0.0168(17) 0.0082(16) C21 0.036(2) 0.043(2) 0.062(3) -0.001(2) 0.026(2) 0.0000(19) C22 0.050(3) 0.108(4) 0.038(3) -0.008(3) 0.018(2) -0.004(3) N5 0.0325(18) 0.0342(16) 0.042(2) 0.0117(14) 0.0182(15) 0.0001(14) N6 0.045(2) 0.0327(17) 0.0347(18) 0.0027(13) 0.0169(15) 0.0013(15) N7 0.0223(16) 0.0375(17) 0.0321(17) 0.0091(13) 0.0083(13) 0.0018(13) N8 0.0423(19) 0.0228(14) 0.0339(17) 0.0007(12) 0.0199(15) -0.0015(13) O3 0.0353(15) 0.0312(13) 0.0335(14) 0.0093(10) 0.0186(12) 0.0106(11) O4 0.0595(19) 0.0488(17) 0.065(2) 0.0315(15) 0.0476(16) 0.0261(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.342(5) . ? C1 C2 1.390(5) . ? C1 C4 1.493(4) . ? C2 C3 1.373(6) . ? C2 H2 0.9500 . ? C3 N1 1.327(5) . ? C3 H3 0.9500 . ? C4 O1 1.435(4) . ? C4 C5 1.530(5) . ? C4 H4 1.0000 . ? C5 O2 1.443(4) . ? C5 C6 1.488(4) . ? C5 H5 1.0000 . ? C6 N4 1.338(4) . ? C6 C7 1.408(5) . ? C7 C8 1.374(5) . ? C7 H7 0.9500 . ? C8 N3 1.339(6) . ? C8 H8 0.9500 . ? C9 O1 1.427(4) . ? C9 O2 1.444(4) . ? C9 C10 1.502(5) . ? C9 C11 1.516(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N1 N2 1.361(4) . ? N1 H1N 0.8800 . ? N3 N4 1.343(4) . ? N3 H3N 0.8800 . ? C12 N6 1.319(5) . ? C12 C13 1.395(6) . ? C12 C15 1.502(5) . ? C13 C14 1.368(5) . ? C13 H13 0.9500 . ? C14 N5 1.329(5) . ? C14 H14 0.9500 . ? C15 O3 1.458(4) . ? C15 C16 1.500(6) . ? C15 H15 1.0000 . ? C16 O4 1.457(5) . ? C16 C17 1.504(5) . ? C16 H16 1.0000 . ? C17 N8 1.343(5) . ? C17 C18 1.378(5) . ? C18 C19 1.347(6) . ? C18 H18 0.9500 . ? C19 N7 1.337(5) . ? C19 H19 0.9500 . ? C20 O3 1.413(4) . ? C20 O4 1.469(5) . ? C20 C22 1.496(6) . ? C20 C21 1.503(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N5 N6 1.344(5) . ? N5 H5N 0.8800 . ? N7 N8 1.352(4) . ? N7 H7N 0.8800 . ? 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 C1 C2 111.8(3) . . ? N2 C1 C4 121.6(3) . . ? C2 C1 C4 126.6(3) . . ? C3 C2 C1 104.7(3) . . ? C3 C2 H2 127.7 . . ? C1 C2 H2 127.7 . . ? N1 C3 C2 107.4(3) . . ? N1 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? O1 C4 C1 109.4(2) . . ? O1 C4 C5 101.9(3) . . ? C1 C4 C5 116.7(3) . . ? O1 C4 H4 109.5 . . ? C1 C4 H4 109.5 . . ? C5 C4 H4 109.5 . . ? O2 C5 C6 110.0(3) . . ? O2 C5 C4 102.7(3) . . ? C6 C5 C4 114.6(3) . . ? O2 C5 H5 109.8 . . ? C6 C5 H5 109.8 . . ? C4 C5 H5 109.8 . . ? N4 C6 C7 111.6(3) . . ? N4 C6 C5 120.1(3) . . ? C7 C6 C5 128.3(3) . . ? C8 C7 C6 104.2(3) . . ? C8 C7 H7 127.9 . . ? C6 C7 H7 127.9 . . ? N3 C8 C7 107.0(3) . . ? N3 C8 H8 126.5 . . ? C7 C8 H8 126.5 . . ? O1 C9 O2 105.1(3) . . ? O1 C9 C10 108.7(3) . . ? O2 C9 C10 109.3(3) . . ? O1 C9 C11 112.6(3) . . ? O2 C9 C11 107.9(3) . . ? C10 C9 C11 113.0(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C3 N1 N2 112.6(3) . . ? C3 N1 H1N 123.7 . . ? N2 N1 H1N 123.7 . . ? C1 N2 N1 103.5(3) . . ? C8 N3 N4 113.1(3) . . ? C8 N3 H3N 123.4 . . ? N4 N3 H3N 123.4 . . ? C6 N4 N3 104.0(3) . . ? C9 O1 C4 106.8(2) . . ? C5 O2 C9 109.5(2) . . ? N6 C12 C13 111.7(3) . . ? N6 C12 C15 116.6(3) . . ? C13 C12 C15 131.7(3) . . ? C14 C13 C12 104.5(3) . . ? C14 C13 H13 127.8 . . ? C12 C13 H13 127.8 . . ? N5 C14 C13 106.8(3) . . ? N5 C14 H14 126.6 . . ? C13 C14 H14 126.6 . . ? O3 C15 C16 101.0(3) . . ? O3 C15 C12 109.7(3) . . ? C16 C15 C12 115.1(3) . . ? O3 C15 H15 110.2 . . ? C16 C15 H15 110.2 . . ? C12 C15 H15 110.2 . . ? O4 C16 C15 101.9(3) . . ? O4 C16 C17 110.3(3) . . ? C15 C16 C17 116.1(3) . . ? O4 C16 H16 109.4 . . ? C15 C16 H16 109.4 . . ? C17 C16 H16 109.4 . . ? N8 C17 C18 110.6(3) . . ? N8 C17 C16 123.6(3) . . ? C18 C17 C16 125.7(4) . . ? C19 C18 C17 106.1(3) . . ? C19 C18 H18 126.9 . . ? C17 C18 H18 126.9 . . ? N7 C19 C18 107.3(3) . . ? N7 C19 H19 126.4 . . ? C18 C19 H19 126.4 . . ? O3 C20 O4 104.3(3) . . ? O3 C20 C22 114.0(3) . . ? O4 C20 C22 109.1(4) . . ? O3 C20 C21 109.1(3) . . ? O4 C20 C21 107.7(3) . . ? C22 C20 C21 112.2(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C14 N5 N6 112.8(3) . . ? C14 N5 H5N 123.6 . . ? N6 N5 H5N 123.6 . . ? C12 N6 N5 104.2(3) . . ? C19 N7 N8 111.7(3) . . ? C19 N7 H7N 124.1 . . ? N8 N7 H7N 124.1 . . ? C17 N8 N7 104.2(3) . . ? C20 O3 C15 105.5(3) . . ? C16 O4 C20 108.4(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 62.62 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.593 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.046 # Attachment '- 1018o.cif' data_1018o _database_code_depnum_ccdc_archive 'CCDC 814852' #TrackingRef '- 1018o.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H19 F6 N4 O2 P Pd' _chemical_formula_weight 526.70 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' F F 0.0727 0.0534 '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' 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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.8264(2) _cell_length_b 11.8915(2) _cell_length_c 16.8036(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.463(2) _cell_angle_gamma 90.00 _cell_volume 1930.86(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26081 _cell_measurement_theta_min 3.7154 _cell_measurement_theta_max 62.5659 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 9.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.37895 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _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 16.1399 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36000 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.58 _diffrn_reflns_theta_max 62.69 _reflns_number_total 6163 _reflns_number_gt 5979 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0343P)^2^+5.0259P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.029(9) _refine_ls_number_reflns 6163 _refine_ls_number_parameters 529 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _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 C1 C 0.7742(6) 0.3189(6) 0.4491(4) 0.0235(13) Uani 1 1 d . A . C2 C 0.7391(6) 0.3549(6) 0.5219(4) 0.0260(13) Uani 1 1 d . . . H2 H 0.7220 0.4297 0.5374 0.031 Uiso 1 1 calc R . . C3 C 0.7348(7) 0.2572(7) 0.5665(4) 0.0340(17) Uani 1 1 d . . . H3 H 0.7140 0.2518 0.6195 0.041 Uiso 1 1 calc R . . C4 C 0.7932(4) 0.3834(4) 0.3759(2) 0.0127(9) Uani 1 1 d . . . H4 H 0.8720 0.3519 0.3528 0.015 Uiso 1 1 calc R . . C5 C 0.6612(4) 0.3896(4) 0.3102(2) 0.0130(9) Uani 1 1 d . . . H5 H 0.5783 0.4019 0.3359 0.016 Uiso 1 1 calc R . . C6 C 0.6341(5) 0.2971(5) 0.2502(3) 0.0195(12) Uani 1 1 d . A . C7 C 0.5385(6) 0.2985(6) 0.1787(3) 0.0234(13) Uani 1 1 d . . . H7 H 0.4808 0.3594 0.1571 0.028 Uiso 1 1 calc R . . C8 C 0.5443(6) 0.1944(6) 0.1458(3) 0.0224(13) Uani 1 1 d . . . H8 H 0.4930 0.1692 0.0955 0.027 Uiso 1 1 calc R . . C9 C 0.7599(7) 0.5676(6) 0.3290(4) 0.0326(15) Uani 1 1 d . . . C10 C 0.6582(9) 0.6476(7) 0.3567(5) 0.065(2) Uani 1 1 d . . . H10A H 0.5817 0.6047 0.3719 0.098 Uiso 1 1 calc R . . H10B H 0.6218 0.6994 0.3126 0.098 Uiso 1 1 calc R . . H10C H 0.7051 0.6906 0.4035 0.098 Uiso 1 1 calc R . . C11 C 0.8745(8) 0.6236(7) 0.2950(4) 0.059(2) Uani 1 1 d . . . H11A H 0.9194 0.6804 0.3333 0.089 Uiso 1 1 calc R . . H11B H 0.8359 0.6598 0.2435 0.089 Uiso 1 1 calc R . . H11C H 0.9428 0.5671 0.2862 0.089 Uiso 1 1 calc R . . C12 C 0.9816(7) 0.0055(8) 0.4284(4) 0.0463(19) Uani 1 1 d DU . . H12A H 1.0463 0.0432 0.4723 0.056 Uiso 0.738(16) 1 calc PR A 1 H12B H 0.9463 -0.0673 0.4448 0.056 Uiso 0.738(16) 1 calc PR A 1 H12C H 1.0798 0.0285 0.4351 0.056 Uiso 0.262(16) 1 d PR A 2 H12D H 0.9549 -0.0210 0.4793 0.056 Uiso 0.262(16) 1 d PR A 2 C13 C 1.0155(10) 0.0098(9) 0.3513(5) 0.039(3) Uani 0.738(16) 1 d PDU A 1 H13 H 1.1063 0.0317 0.3458 0.047 Uiso 0.738(16) 1 calc PR A 1 C13A C 0.931(2) -0.0531(15) 0.3618(7) 0.037(6) Uani 0.262(16) 1 d PDU A 2 H13A H 0.8972 -0.1267 0.3690 0.045 Uiso 0.262(16) 1 calc PR A 2 C14 C 0.9227(7) -0.0162(6) 0.2846(4) 0.0353(15) Uani 1 1 d DU . . H14A H 0.8810 -0.0922 0.2829 0.042 Uiso 0.738(16) 1 calc PR A 1 H14B H 0.9448 0.0085 0.2321 0.042 Uiso 0.738(16) 1 calc PR A 1 H14C H 0.8565 -0.0552 0.2421 0.042 Uiso 0.262(16) 1 d PR A 2 H14D H 1.0113 0.0029 0.2678 0.042 Uiso 0.262(16) 1 d PR A 2 N1 N 0.7658(5) 0.1717(5) 0.5206(3) 0.0308(13) Uani 1 1 d . A . H1N H 0.7706 0.1008 0.5359 0.037 Uiso 1 1 calc R . . N2 N 0.7889(5) 0.2087(5) 0.4472(3) 0.0278(12) Uani 1 1 d . . . N3 N 0.6349(4) 0.1347(5) 0.1970(3) 0.0220(10) Uani 1 1 d . A . H3N H 0.6555 0.0641 0.1889 0.026 Uiso 1 1 calc R . . N4 N 0.6921(5) 0.1944(5) 0.2630(3) 0.0209(11) Uani 1 1 d . . . O1 O 0.8174(4) 0.4985(3) 0.3966(2) 0.0290(9) Uani 1 1 d . . . O2 O 0.6921(5) 0.4912(4) 0.2686(3) 0.0297(10) Uani 1 1 d . . . Pd1 Pd 0.83759(3) 0.10944(2) 0.35451(2) 0.02195(13) Uani 1 1 d D A . C15 C 0.3305(7) -0.0473(6) 0.2512(4) 0.0354(16) Uani 1 1 d . B . C16 C 0.4329(7) -0.0593(6) 0.3204(4) 0.0337(16) Uani 1 1 d . . . H16 H 0.4776 -0.1265 0.3415 0.040 Uiso 1 1 calc R . . C17 C 0.4544(6) 0.0485(7) 0.3511(4) 0.0323(16) Uani 1 1 d . . . H17 H 0.5185 0.0700 0.3980 0.039 Uiso 1 1 calc R . . C18 C 0.2474(7) -0.1321(5) 0.1928(4) 0.0392(14) Uani 1 1 d . . . H18 H 0.1460 -0.1150 0.1824 0.047 Uiso 1 1 calc R . . C19 C 0.3009(8) -0.1467(5) 0.1179(4) 0.0468(16) Uani 1 1 d . . . H19 H 0.4041 -0.1518 0.1307 0.056 Uiso 1 1 calc R . . C20 C 0.2594(6) -0.0696(5) 0.0490(4) 0.0267(14) Uani 1 1 d . B . C21 C 0.2785(7) -0.0921(7) -0.0289(4) 0.0356(17) Uani 1 1 d . . . H21 H 0.3071 -0.1615 -0.0486 0.043 Uiso 1 1 calc R . . C22 C 0.2488(7) 0.0037(8) -0.0717(4) 0.0396(18) Uani 1 1 d . . . H22 H 0.2519 0.0148 -0.1273 0.048 Uiso 1 1 calc R . . C23 C 0.2642(7) -0.3224(6) 0.1650(4) 0.0305(15) Uani 1 1 d . . . C24 C 0.3886(8) -0.3915(7) 0.1739(5) 0.064(2) Uani 1 1 d . . . H24A H 0.4651 -0.3527 0.2088 0.096 Uiso 1 1 calc R . . H24B H 0.4129 -0.4044 0.1206 0.096 Uiso 1 1 calc R . . H24C H 0.3716 -0.4638 0.1983 0.096 Uiso 1 1 calc R . . C25 C 0.1338(8) -0.3923(7) 0.1572(6) 0.070(2) Uani 1 1 d . . . H25A H 0.1324 -0.4318 0.2082 0.104 Uiso 1 1 calc R . . H25B H 0.1317 -0.4473 0.1135 0.104 Uiso 1 1 calc R . . H25C H 0.0527 -0.3431 0.1448 0.104 Uiso 1 1 calc R . . C26 C 0.0013(6) 0.2311(7) 0.0675(4) 0.0356(15) Uani 1 1 d DU . . H26A H 0.0272 0.2572 0.0164 0.043 Uiso 0.377(16) 1 calc PR B 1 H26B H -0.0951 0.2032 0.0606 0.043 Uiso 0.377(16) 1 calc PR B 1 H26C H 0.0327 0.3028 0.0471 0.043 Uiso 0.623(16) 1 d PR B 2 H26D H -0.0624 0.1882 0.0260 0.043 Uiso 0.623(16) 1 d PR B 2 C27 C 0.0447(14) 0.2945(11) 0.1328(6) 0.028(4) Uani 0.377(16) 1 d PDU B 1 H27 H 0.0668 0.3709 0.1245 0.034 Uiso 0.377(16) 1 calc PR B 1 C27A C -0.0324(10) 0.2329(11) 0.1455(5) 0.035(3) Uani 0.623(16) 1 d PDU B 2 H27A H -0.1247 0.2162 0.1512 0.041 Uiso 0.623(16) 1 calc PR B 2 C28 C 0.0596(8) 0.2569(8) 0.2109(4) 0.0468(19) Uani 1 1 d DU . . H28A H -0.0262 0.2333 0.2293 0.056 Uiso 0.377(16) 1 calc PR B 1 H28B H 0.1231 0.3005 0.2521 0.056 Uiso 0.377(16) 1 calc PR B 1 H28C H 0.0371 0.2315 0.2631 0.056 Uiso 0.623(16) 1 d PR B 2 H28D H 0.0999 0.3334 0.2135 0.056 Uiso 0.623(16) 1 d PR B 2 N5 N 0.3678(4) 0.1171(5) 0.3024(3) 0.0247(10) Uani 1 1 d . B . H5N H 0.3612 0.1900 0.3097 0.030 Uiso 1 1 calc R . . N6 N 0.2924(5) 0.0589(4) 0.2409(3) 0.0218(11) Uani 1 1 d . . . N7 N 0.2140(6) 0.0799(5) -0.0202(3) 0.0381(14) Uani 1 1 d . B . H7N H 0.1913 0.1499 -0.0336 0.046 Uiso 1 1 calc R . . N8 N 0.2176(5) 0.0375(5) 0.0543(3) 0.0253(12) Uani 1 1 d . . . O3 O 0.2773(7) -0.2416(5) 0.2294(3) 0.0631(18) Uani 1 1 d . . . O4 O 0.2432(5) -0.2571(4) 0.0937(3) 0.0430(12) Uani 1 1 d . . . Pd2 Pd 0.15256(3) 0.13605(2) 0.14549(2) 0.02047(12) Uani 1 1 d D B . F1 F 0.8281(4) 0.7994(4) 0.0921(3) 0.0462(11) Uani 1 1 d . . . F2 F 0.6757(4) 0.8974(4) 0.1532(2) 0.0419(10) Uani 1 1 d . . . F3 F 0.5987(4) 0.7922(4) 0.0429(3) 0.0534(12) Uani 1 1 d . . . F4 F 0.7386(4) 0.8839(5) -0.0266(2) 0.0588(13) Uani 1 1 d . . . F5 F 0.8186(4) 0.9905(4) 0.0844(3) 0.0482(11) Uani 1 1 d . . . F6 F 0.5896(4) 0.9816(4) 0.0350(3) 0.0535(12) Uani 1 1 d . . . P1 P 0.70832(16) 0.89138(16) 0.06273(11) 0.0317(4) Uani 1 1 d . . . F7 F 0.4260(4) 0.2790(4) 0.4507(3) 0.0582(13) Uani 1 1 d . . . F8 F 0.4132(4) 0.4688(4) 0.4342(3) 0.0570(13) Uani 1 1 d . . . F9 F 0.2919(5) 0.3847(5) 0.5183(3) 0.0650(14) Uani 1 1 d . . . F10 F 0.1954(4) 0.2685(4) 0.4170(3) 0.0482(11) Uani 1 1 d . . . F11 F 0.3186(4) 0.3521(4) 0.3323(3) 0.0469(10) Uani 1 1 d . . . F12 F 0.1811(4) 0.4548(4) 0.3992(3) 0.0538(12) Uani 1 1 d . . . P2 P 0.30426(16) 0.36755(17) 0.42602(11) 0.0337(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.022(3) 0.027(3) 0.020(3) 0.002(2) -0.002(2) -0.003(2) C2 0.028(3) 0.024(3) 0.024(3) -0.001(3) 0.000(2) -0.009(2) C3 0.052(4) 0.041(4) 0.008(3) 0.000(3) 0.004(3) -0.011(3) C4 0.015(2) 0.014(2) 0.008(2) 0.0000(17) 0.0009(17) 0.0008(18) C5 0.018(2) 0.014(2) 0.006(2) -0.0013(17) 0.0000(17) 0.0037(18) C6 0.016(2) 0.022(3) 0.020(3) 0.006(2) 0.002(2) 0.004(2) C7 0.026(3) 0.026(3) 0.018(3) 0.002(2) 0.002(2) 0.003(2) C8 0.029(3) 0.028(4) 0.010(3) -0.002(3) 0.003(2) -0.002(2) C9 0.056(4) 0.017(3) 0.023(3) 0.000(3) 0.003(3) 0.000(3) C10 0.085(5) 0.047(5) 0.054(5) -0.024(4) -0.013(4) 0.032(4) C11 0.095(5) 0.050(4) 0.035(4) 0.005(4) 0.017(3) -0.040(4) C12 0.042(4) 0.057(5) 0.039(3) 0.014(4) 0.005(3) 0.025(4) C13 0.051(6) 0.033(6) 0.030(4) -0.003(4) -0.001(4) 0.010(5) C13A 0.043(12) 0.028(12) 0.039(8) 0.006(7) 0.003(9) 0.034(10) C14 0.043(3) 0.025(4) 0.038(3) 0.004(3) 0.007(3) 0.019(3) N1 0.049(3) 0.028(3) 0.014(3) 0.004(2) 0.001(2) -0.002(2) N2 0.035(3) 0.031(4) 0.016(3) 0.008(2) 0.000(2) -0.001(2) N3 0.027(2) 0.017(3) 0.022(2) -0.005(3) 0.0044(17) 0.002(2) N4 0.024(2) 0.024(3) 0.015(2) -0.005(2) 0.0044(18) 0.000(2) O1 0.041(2) 0.020(2) 0.023(2) -0.0015(16) -0.0017(16) -0.0051(17) O2 0.055(3) 0.017(2) 0.016(2) 0.0014(18) 0.0034(17) 0.0031(19) Pd1 0.02225(19) 0.0228(3) 0.0194(2) 0.00415(19) -0.00004(15) 0.00491(16) C15 0.069(4) 0.018(3) 0.016(3) -0.003(2) -0.004(3) 0.009(3) C16 0.044(3) 0.035(4) 0.022(3) 0.006(3) 0.006(3) 0.020(3) C17 0.020(3) 0.047(5) 0.026(4) 0.005(3) -0.007(2) 0.002(3) C18 0.052(4) 0.022(3) 0.043(4) 0.002(3) 0.009(3) 0.001(3) C19 0.079(5) 0.022(3) 0.039(4) -0.002(3) 0.009(3) -0.009(3) C20 0.041(3) 0.020(3) 0.018(3) -0.001(2) 0.002(2) 0.001(3) C21 0.042(3) 0.044(4) 0.020(3) -0.014(3) 0.005(3) 0.003(3) C22 0.050(4) 0.051(5) 0.020(3) 0.003(3) 0.013(3) -0.018(4) C23 0.047(3) 0.021(3) 0.022(3) 0.001(3) 0.003(3) 0.002(3) C24 0.058(4) 0.040(4) 0.091(6) -0.006(5) 0.002(4) 0.021(4) C25 0.074(5) 0.039(5) 0.099(7) -0.001(5) 0.023(5) -0.018(4) C26 0.029(3) 0.036(4) 0.040(3) 0.012(3) 0.000(3) 0.008(3) C27 0.018(7) 0.026(9) 0.037(7) 0.001(6) -0.002(6) -0.009(6) C27A 0.020(5) 0.043(7) 0.040(5) 0.011(5) 0.004(4) 0.015(5) C28 0.059(4) 0.050(5) 0.036(3) 0.002(4) 0.020(3) 0.023(4) N5 0.031(2) 0.022(3) 0.021(2) -0.003(3) 0.0050(18) -0.004(2) N6 0.028(2) 0.018(3) 0.019(2) 0.001(2) 0.0008(19) 0.004(2) N7 0.058(3) 0.031(4) 0.026(3) 0.010(3) 0.007(2) -0.007(3) N8 0.035(3) 0.023(3) 0.018(3) 0.004(2) 0.004(2) 0.003(2) O3 0.153(6) 0.013(2) 0.022(3) 0.007(2) 0.012(3) 0.008(3) O4 0.075(3) 0.017(2) 0.026(2) -0.0030(17) -0.018(2) -0.002(2) Pd2 0.02112(19) 0.0175(3) 0.0218(2) 0.00099(18) 0.00122(15) 0.00124(16) F1 0.037(2) 0.044(3) 0.055(3) -0.012(2) -0.0003(18) 0.0102(19) F2 0.049(2) 0.040(3) 0.040(2) -0.0140(18) 0.0182(16) -0.0037(18) F3 0.042(2) 0.039(2) 0.074(3) -0.024(2) -0.0035(19) -0.0112(18) F4 0.059(2) 0.084(4) 0.033(2) -0.016(2) 0.0080(18) 0.008(2) F5 0.042(2) 0.040(3) 0.064(3) -0.012(2) 0.0131(19) -0.0172(19) F6 0.046(2) 0.045(3) 0.067(3) -0.010(2) 0.0045(19) 0.017(2) P1 0.0298(7) 0.0302(9) 0.0345(9) -0.0142(8) 0.0041(6) 0.0002(7) F7 0.044(2) 0.046(3) 0.078(3) -0.011(2) -0.006(2) 0.0124(19) F8 0.046(2) 0.040(2) 0.086(3) -0.026(2) 0.015(2) -0.0163(19) F9 0.069(3) 0.079(4) 0.047(3) -0.024(3) 0.011(2) -0.003(3) F10 0.050(2) 0.041(3) 0.057(3) -0.007(2) 0.016(2) -0.020(2) F11 0.053(2) 0.041(3) 0.050(2) -0.007(2) 0.0182(18) -0.007(2) F12 0.045(2) 0.044(3) 0.068(3) -0.021(2) -0.001(2) 0.018(2) P2 0.0312(8) 0.0288(9) 0.0418(10) -0.0104(8) 0.0080(7) -0.0009(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.319(9) . ? C1 C2 1.397(9) . ? C1 C4 1.490(7) . ? C2 C3 1.388(10) . ? C2 H2 0.9500 . ? C3 N1 1.344(10) . ? C3 H3 0.9500 . ? C4 O1 1.421(6) . ? C4 C5 1.544(6) . ? C4 H4 1.0000 . ? C5 O2 1.455(6) . ? C5 C6 1.483(7) . ? C5 H5 1.0000 . ? C6 N4 1.348(8) . ? C6 C7 1.385(8) . ? C7 C8 1.361(9) . ? C7 H7 0.9500 . ? C8 N3 1.327(8) . ? C8 H8 0.9500 . ? C9 O1 1.432(8) . ? C9 O2 1.433(8) . ? C9 C11 1.508(9) . ? C9 C10 1.513(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13A 1.337(14) . ? C12 C13 1.396(10) . ? C12 Pd1 2.105(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 H12C 0.9900 . ? C12 H12D 0.9900 . ? C13 C14 1.347(10) . ? C13 Pd1 2.121(9) . ? C13 H12C 1.4524 . ? C13 H13 0.9500 . ? C13 H14D 1.3996 . ? C13A C14 1.358(14) . ? C13A Pd1 2.132(15) . ? C13A H13A 0.9500 . ? C14 Pd1 2.161(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 H14C 0.9900 . ? C14 H14D 0.9900 . ? N1 N2 1.367(7) . ? N1 H1N 0.8800 . ? N2 Pd1 2.078(6) . ? N3 N4 1.350(7) . ? N3 H3N 0.8800 . ? N4 Pd1 2.152(5) . ? C15 N6 1.319(8) . ? C15 C16 1.400(9) . ? C15 C18 1.534(9) . ? C16 C17 1.383(11) . ? C16 H16 0.9500 . ? C17 N5 1.344(8) . ? C17 H17 0.9500 . ? C18 O3 1.447(8) . ? C18 C19 1.460(9) . ? C18 H18 1.0000 . ? C19 O4 1.459(7) . ? C19 C20 1.474(9) . ? C19 H19 1.0000 . ? C20 N8 1.346(9) . ? C20 C21 1.383(9) . ? C21 C22 1.350(12) . ? C21 H21 0.9500 . ? C22 N7 1.340(11) . ? C22 H22 0.9500 . ? C23 O4 1.411(8) . ? C23 O3 1.436(8) . ? C23 C24 1.459(9) . ? C23 C25 1.513(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.336(11) . ? C26 C27A 1.408(10) . ? C26 Pd2 2.120(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 H26C 0.9900 . ? C26 H26D 0.9900 . ? C27 C28 1.368(12) . ? C27 Pd2 2.153(13) . ? C27 H26C 1.4281 . ? C27 H27 0.9500 . ? C27 H28D 1.4411 . ? C27A C28 1.322(10) . ? C27A Pd2 2.152(9) . ? C27A H27A 0.9500 . ? C28 Pd2 2.114(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 H28C 0.9900 . ? C28 H28D 0.9900 . ? N5 N6 1.349(7) . ? N5 H5N 0.8800 . ? N6 Pd2 2.121(5) . ? N7 N8 1.344(7) . ? N7 H7N 0.8800 . ? N8 Pd2 2.118(5) . ? F1 P1 1.617(5) . ? F2 P1 1.611(4) . ? F3 P1 1.591(4) . ? F4 P1 1.585(4) . ? F5 P1 1.597(4) . ? F6 P1 1.591(5) . ? F7 P2 1.592(5) . ? F8 P2 1.600(4) . ? F9 P2 1.590(5) . ? F10 P2 1.580(4) . ? F11 P2 1.617(4) . ? F12 P2 1.596(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C2 111.8(6) . . ? N2 C1 C4 117.4(5) . . ? C2 C1 C4 130.7(6) . . ? C3 C2 C1 104.7(6) . . ? C3 C2 H2 127.7 . . ? C1 C2 H2 127.7 . . ? N1 C3 C2 106.9(5) . . ? N1 C3 H3 126.6 . . ? C2 C3 H3 126.6 . . ? O1 C4 C1 109.6(4) . . ? O1 C4 C5 102.2(3) . . ? C1 C4 C5 113.6(4) . . ? O1 C4 H4 110.4 . . ? C1 C4 H4 110.4 . . ? C5 C4 H4 110.4 . . ? O2 C5 C6 108.5(4) . . ? O2 C5 C4 99.3(3) . . ? C6 C5 C4 118.3(4) . . ? O2 C5 H5 110.0 . . ? C6 C5 H5 110.0 . . ? C4 C5 H5 110.0 . . ? N4 C6 C7 110.5(6) . . ? N4 C6 C5 123.0(5) . . ? C7 C6 C5 126.2(5) . . ? C8 C7 C6 105.6(5) . . ? C8 C7 H7 127.2 . . ? C6 C7 H7 127.2 . . ? N3 C8 C7 107.2(5) . . ? N3 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? O1 C9 O2 105.3(5) . . ? O1 C9 C11 109.8(6) . . ? O2 C9 C11 107.1(5) . . ? O1 C9 C10 107.8(6) . . ? O2 C9 C10 111.6(6) . . ? C11 C9 C10 114.8(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13A C12 C13 50.1(11) . . ? C13A C12 Pd1 72.7(7) . . ? C13 C12 Pd1 71.3(5) . . ? C13A C12 H12A 162.4 . . ? C13 C12 H12A 116.5 . . ? Pd1 C12 H12A 116.5 . . ? C13A C12 H12B 71.4 . . ? C13 C12 H12B 116.5 . . ? Pd1 C12 H12B 116.5 . . ? H12A C12 H12B 113.5 . . ? C13A C12 H12C 116.7 . . ? C13 C12 H12C 72.8 . . ? Pd1 C12 H12C 116.2 . . ? H12A C12 H12C 46.2 . . ? H12B C12 H12C 126.4 . . ? C13A C12 H12D 116.1 . . ? C13 C12 H12D 163.4 . . ? Pd1 C12 H12D 116.2 . . ? H12A C12 H12D 74.6 . . ? H12B C12 H12D 47.2 . . ? H12C C12 H12D 113.2 . . ? C14 C13 C12 121.6(9) . . ? C14 C13 Pd1 73.3(5) . . ? C12 C13 Pd1 70.1(5) . . ? C14 C13 H12C 162.2 . . ? C12 C13 H12C 40.6 . . ? Pd1 C13 H12C 96.1 . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? Pd1 C13 H13 130.0 . . ? H12C C13 H13 78.6 . . ? C14 C13 H14D 42.2 . . ? C12 C13 H14D 163.8 . . ? Pd1 C13 H14D 100.6 . . ? H12C C13 H14D 155.5 . . ? H13 C13 H14D 77.0 . . ? C12 C13A C14 125.4(16) . . ? C12 C13A Pd1 70.5(7) . . ? C14 C13A Pd1 72.7(7) . . ? C12 C13A H13A 117.3 . . ? C14 C13A H13A 117.3 . . ? Pd1 C13A H13A 133.4 . . ? C13 C14 C13A 50.7(11) . . ? C13 C14 Pd1 70.1(5) . . ? C13A C14 Pd1 70.4(7) . . ? C13 C14 H14A 116.6 . . ? C13A C14 H14A 71.6 . . ? Pd1 C14 H14A 116.6 . . ? C13 C14 H14B 116.6 . . ? C13A C14 H14B 164.3 . . ? Pd1 C14 H14B 116.6 . . ? H14A C14 H14B 113.6 . . ? C13 C14 H14C 164.9 . . ? C13A C14 H14C 117.0 . . ? Pd1 C14 H14C 116.6 . . ? H14A C14 H14C 48.5 . . ? H14B C14 H14C 73.6 . . ? C13 C14 H14D 71.8 . . ? C13A C14 H14D 116.5 . . ? Pd1 C14 H14D 116.4 . . ? H14A C14 H14D 125.5 . . ? H14B C14 H14D 48.0 . . ? H14C C14 H14D 113.5 . . ? C3 N1 N2 111.5(6) . . ? C3 N1 H1N 124.2 . . ? N2 N1 H1N 124.2 . . ? C1 N2 N1 105.1(5) . . ? C1 N2 Pd1 128.6(4) . . ? N1 N2 Pd1 126.3(4) . . ? C8 N3 N4 112.5(6) . . ? C8 N3 H3N 123.8 . . ? N4 N3 H3N 123.8 . . ? C6 N4 N3 104.2(5) . . ? C6 N4 Pd1 138.2(4) . . ? N3 N4 Pd1 117.6(4) . . ? C4 O1 C9 109.5(4) . . ? C9 O2 C5 107.3(4) . . ? N2 Pd1 C12 96.5(3) . . ? N2 Pd1 C13 129.8(2) . . ? C12 Pd1 C13 38.6(3) . . ? N2 Pd1 C13A 128.8(4) . . ? C12 Pd1 C13A 36.8(4) . . ? C13 Pd1 C13A 31.6(7) . . ? N2 Pd1 N4 93.15(19) . . ? C12 Pd1 N4 170.1(3) . . ? C13 Pd1 N4 133.5(2) . . ? C13A Pd1 N4 133.5(4) . . ? N2 Pd1 C14 164.8(2) . . ? C12 Pd1 C14 68.3(3) . . ? C13 Pd1 C14 36.6(3) . . ? C13A Pd1 C14 36.9(4) . . ? N4 Pd1 C14 102.1(2) . . ? N6 C15 C16 110.5(6) . . ? N6 C15 C18 116.1(5) . . ? C16 C15 C18 133.0(6) . . ? C17 C16 C15 104.7(6) . . ? C17 C16 H16 127.7 . . ? C15 C16 H16 127.7 . . ? N5 C17 C16 107.3(5) . . ? N5 C17 H17 126.3 . . ? C16 C17 H17 126.3 . . ? O3 C18 C19 100.5(5) . . ? O3 C18 C15 106.0(5) . . ? C19 C18 C15 113.3(5) . . ? O3 C18 H18 112.1 . . ? C19 C18 H18 112.1 . . ? C15 C18 H18 112.1 . . ? O4 C19 C18 99.5(5) . . ? O4 C19 C20 107.6(5) . . ? C18 C19 C20 120.7(6) . . ? O4 C19 H19 109.4 . . ? C18 C19 H19 109.4 . . ? C20 C19 H19 109.4 . . ? N8 C20 C21 110.0(6) . . ? N8 C20 C19 125.5(6) . . ? C21 C20 C19 123.8(6) . . ? C22 C21 C20 106.7(7) . . ? C22 C21 H21 126.7 . . ? C20 C21 H21 126.7 . . ? N7 C22 C21 106.5(6) . . ? N7 C22 H22 126.8 . . ? C21 C22 H22 126.8 . . ? O4 C23 O3 104.6(5) . . ? O4 C23 C24 112.8(6) . . ? O3 C23 C24 109.9(6) . . ? O4 C23 C25 103.8(6) . . ? O3 C23 C25 113.1(6) . . ? C24 C23 C25 112.4(7) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C27A 47.3(8) . . ? C27 C26 Pd2 73.1(6) . . ? C27A C26 Pd2 72.0(5) . . ? C27 C26 H26A 116.2 . . ? C27A C26 H26A 160.7 . . ? Pd2 C26 H26A 116.2 . . ? C27 C26 H26B 116.2 . . ? C27A C26 H26B 74.5 . . ? Pd2 C26 H26B 116.2 . . ? H26A C26 H26B 113.2 . . ? C27 C26 H26C 74.1 . . ? C27A C26 H26C 116.8 . . ? Pd2 C26 H26C 116.5 . . ? H26A C26 H26C 44.1 . . ? H26B C26 H26C 126.9 . . ? C27 C26 H26D 159.5 . . ? C27A C26 H26D 116.0 . . ? Pd2 C26 H26D 116.3 . . ? H26A C26 H26D 77.3 . . ? H26B C26 H26D 43.6 . . ? H26C C26 H26D 113.4 . . ? C26 C27 C28 124.4(11) . . ? C26 C27 Pd2 70.5(6) . . ? C28 C27 Pd2 69.8(6) . . ? C26 C27 H26C 41.8 . . ? C28 C27 H26C 164.8 . . ? Pd2 C27 H26C 96.3 . . ? C26 C27 H27 117.8 . . ? C28 C27 H27 117.8 . . ? Pd2 C27 H27 136.9 . . ? H26C C27 H27 76.4 . . ? C26 C27 H28D 164.4 . . ? C28 C27 H28D 41.2 . . ? Pd2 C27 H28D 95.4 . . ? H26C C27 H28D 151.0 . . ? H27 C27 H28D 77.0 . . ? C28 C27A C26 122.4(8) . . ? C28 C27A Pd2 70.4(5) . . ? C26 C27A Pd2 69.6(5) . . ? C28 C27A H27A 118.8 . . ? C26 C27A H27A 118.8 . . ? Pd2 C27A H27A 135.3 . . ? C27A C28 C27 48.3(8) . . ? C27A C28 Pd2 73.5(5) . . ? C27 C28 Pd2 72.8(6) . . ? C27A C28 H28A 72.8 . . ? C27 C28 H28A 116.3 . . ? Pd2 C28 H28A 116.3 . . ? C27A C28 H28B 160.6 . . ? C27 C28 H28B 116.3 . . ? Pd2 C28 H28B 116.3 . . ? H28A C28 H28B 113.3 . . ? C27A C28 H28C 116.2 . . ? C27 C28 H28C 161.2 . . ? Pd2 C28 H28C 116.2 . . ? H28A C28 H28C 45.3 . . ? H28B C28 H28C 75.8 . . ? C27A C28 H28D 116.3 . . ? C27 C28 H28D 73.4 . . ? Pd2 C28 H28D 116.1 . . ? H28A C28 H28D 127.1 . . ? H28B C28 H28D 44.9 . . ? H28C C28 H28D 113.1 . . ? C17 N5 N6 110.8(6) . . ? C17 N5 H5N 124.6 . . ? N6 N5 H5N 124.6 . . ? C15 N6 N5 106.7(5) . . ? C15 N6 Pd2 130.0(4) . . ? N5 N6 Pd2 123.2(4) . . ? C22 N7 N8 112.4(6) . . ? C22 N7 H7N 123.8 . . ? N8 N7 H7N 123.8 . . ? N7 N8 C20 104.5(5) . . ? N7 N8 Pd2 120.4(4) . . ? C20 N8 Pd2 135.0(4) . . ? C23 O3 C18 107.4(5) . . ? C23 O4 C19 105.6(5) . . ? C28 Pd2 N8 165.4(3) . . ? C28 Pd2 C26 68.8(3) . . ? N8 Pd2 C26 96.8(2) . . ? C28 Pd2 N6 100.5(2) . . ? N8 Pd2 N6 93.91(19) . . ? C26 Pd2 N6 169.3(2) . . ? C28 Pd2 C27A 36.1(3) . . ? N8 Pd2 C27A 131.5(3) . . ? C26 Pd2 C27A 38.5(3) . . ? N6 Pd2 C27A 131.5(3) . . ? C28 Pd2 C27 37.4(3) . . ? N8 Pd2 C27 128.4(3) . . ? C26 Pd2 C27 36.4(3) . . ? N6 Pd2 C27 133.8(3) . . ? C27A Pd2 C27 29.7(5) . . ? F4 P1 F6 90.8(3) . . ? F4 P1 F3 89.8(3) . . ? F6 P1 F3 90.4(2) . . ? F4 P1 F5 91.2(3) . . ? F6 P1 F5 90.0(3) . . ? F3 P1 F5 178.9(3) . . ? F4 P1 F2 179.1(3) . . ? F6 P1 F2 89.2(3) . . ? F3 P1 F2 89.2(3) . . ? F5 P1 F2 89.7(3) . . ? F4 P1 F1 90.0(3) . . ? F6 P1 F1 179.2(3) . . ? F3 P1 F1 89.4(3) . . ? F5 P1 F1 90.2(2) . . ? F2 P1 F1 90.0(3) . . ? F10 P2 F9 91.0(3) . . ? F10 P2 F7 89.7(3) . . ? F9 P2 F7 91.0(3) . . ? F10 P2 F12 89.5(2) . . ? F9 P2 F12 90.2(3) . . ? F7 P2 F12 178.6(3) . . ? F10 P2 F8 179.3(3) . . ? F9 P2 F8 89.3(3) . . ? F7 P2 F8 90.9(3) . . ? F12 P2 F8 89.8(3) . . ? F10 P2 F11 90.0(3) . . ? F9 P2 F11 179.0(3) . . ? F7 P2 F11 89.1(3) . . ? F12 P2 F11 89.7(3) . . ? F8 P2 F11 89.7(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 62.69 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.694 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.091 # Attachment '- 10122o.cif' data_10122o _database_code_depnum_ccdc_archive 'CCDC 814853' #TrackingRef '- 10122o.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H88 N8 O4 Rh4' _chemical_formula_weight 1421.04 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 Tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/4' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+1/4' '-y+1/2, x+1/2, z+3/4' _cell_length_a 12.4072(1) _cell_length_b 12.4072(1) _cell_length_c 39.0374(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6009.36(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30932 _cell_measurement_theta_min 3.3936 _cell_measurement_theta_max 62.5834 _exptl_crystal_description 'transparent block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 9.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.48663 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _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 16.1399 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50162 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 62.68 _reflns_number_total 4817 _reflns_number_gt 4724 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0161P)^2^+6.1458P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(7) _refine_ls_number_reflns 4817 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0416 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 C1 C 0.8329(2) 0.4086(2) 0.21258(7) 0.0193(7) Uani 1 1 d . . . C2 C 0.8913(2) 0.3216(3) 0.22496(8) 0.0236(7) Uani 1 1 d . . . H2 H 0.9516 0.3232 0.2400 0.028 Uiso 1 1 calc R . . C3 C 0.8429(2) 0.2328(3) 0.21077(8) 0.0228(7) Uani 1 1 d . . . H3 H 0.8655 0.1604 0.2142 0.027 Uiso 1 1 calc R . . C4 C 0.8434(2) 0.5253(2) 0.22112(7) 0.0198(7) Uani 1 1 d . . . H4 H 0.7795 0.5655 0.2121 0.024 Uiso 1 1 calc R . . C5 C 0.8535(2) 0.5440(2) 0.25979(7) 0.0191(6) Uani 1 1 d . . . H5 H 0.8996 0.4866 0.2702 0.023 Uiso 1 1 calc R . . C6 C 0.7476(2) 0.5469(3) 0.27725(7) 0.0203(6) Uani 1 1 d . . . C7 C 0.6548(2) 0.6055(3) 0.26989(8) 0.0275(8) Uani 1 1 d . . . H7 H 0.6472 0.6632 0.2541 0.033 Uiso 1 1 calc R . . C8 C 0.5762(2) 0.5616(3) 0.29064(8) 0.0271(7) Uani 1 1 d . . . H8 H 0.5035 0.5853 0.2917 0.033 Uiso 1 1 calc R . . C9 C 0.9862(2) 0.6422(3) 0.23325(8) 0.0241(7) Uani 1 1 d . . . C10 C 1.0000(3) 0.7547(3) 0.21847(9) 0.0317(8) Uani 1 1 d . . . H10A H 1.0361 0.8003 0.2358 0.038 Uiso 1 1 calc R . . H10B H 1.0484 0.7501 0.1984 0.038 Uiso 1 1 calc R . . C11 C 0.8965(3) 0.8101(3) 0.20756(9) 0.0355(8) Uani 1 1 d . . . H11A H 0.8436 0.7546 0.2005 0.043 Uiso 1 1 calc R . . H11B H 0.9116 0.8559 0.1874 0.043 Uiso 1 1 calc R . . C12 C 0.8465(4) 0.8794(4) 0.23543(11) 0.0604(13) Uani 1 1 d . . . H12A H 0.8216 0.8333 0.2542 0.091 Uiso 1 1 calc R . . H12B H 0.7852 0.9194 0.2260 0.091 Uiso 1 1 calc R . . H12C H 0.9004 0.9303 0.2441 0.091 Uiso 1 1 calc R . . C13 C 1.0923(3) 0.5912(3) 0.24524(9) 0.0309(8) Uani 1 1 d . . . H13A H 1.0781 0.5150 0.2512 0.037 Uiso 1 1 calc R . . H13B H 1.1434 0.5915 0.2258 0.037 Uiso 1 1 calc R . . C14 C 1.1463(3) 0.6447(3) 0.27551(9) 0.0397(8) Uani 1 1 d . . . H14A H 1.0952 0.6466 0.2950 0.048 Uiso 1 1 calc R . . H14B H 1.1642 0.7200 0.2694 0.048 Uiso 1 1 calc R . . C15 C 1.2486(3) 0.5871(4) 0.28668(11) 0.0547(12) Uani 1 1 d . . . H15A H 1.2318 0.5118 0.2921 0.082 Uiso 1 1 calc R . . H15B H 1.2782 0.6227 0.3070 0.082 Uiso 1 1 calc R . . H15C H 1.3016 0.5895 0.2681 0.082 Uiso 1 1 calc R . . C16 C 0.5099(3) 0.1555(3) 0.13160(9) 0.0290(8) Uani 1 1 d . . . H16 H 0.4822 0.2236 0.1384 0.035 Uiso 1 1 calc R . . C17 C 0.5057(2) 0.0722(3) 0.15540(8) 0.0243(7) Uani 1 1 d . . . H17 H 0.4747 0.0858 0.1772 0.029 Uiso 1 1 calc R . . C18 C 0.5486(3) -0.0389(3) 0.14774(11) 0.0435(10) Uani 1 1 d . . . H18A H 0.5101 -0.0917 0.1623 0.052 Uiso 1 1 calc R . . H18B H 0.5325 -0.0566 0.1236 0.052 Uiso 1 1 calc R . . C19 C 0.6672(3) -0.0514(3) 0.15354(12) 0.0453(10) Uani 1 1 d . . . H19A H 0.6781 -0.0884 0.1757 0.054 Uiso 1 1 calc R . . H19B H 0.6965 -0.0989 0.1354 0.054 Uiso 1 1 calc R . . C20 C 0.7312(2) 0.0507(3) 0.15379(9) 0.0302(8) Uani 1 1 d . . . H20 H 0.7744 0.0653 0.1733 0.036 Uiso 1 1 calc R . . C21 C 0.7319(3) 0.1253(3) 0.12743(9) 0.0339(8) Uani 1 1 d . . . H21 H 0.7741 0.1887 0.1300 0.041 Uiso 1 1 calc R . . C22 C 0.6682(4) 0.1105(4) 0.09450(9) 0.0595(13) Uani 1 1 d . . . H22A H 0.7047 0.1510 0.0760 0.071 Uiso 1 1 calc R . . H22B H 0.6696 0.0332 0.0882 0.071 Uiso 1 1 calc R . . C23 C 0.5544(4) 0.1463(4) 0.09629(9) 0.0553(12) Uani 1 1 d . . . H23A H 0.5095 0.0948 0.0832 0.066 Uiso 1 1 calc R . . H23B H 0.5484 0.2174 0.0849 0.066 Uiso 1 1 calc R . . C24 C 0.5346(3) 0.5643(3) 0.13924(8) 0.0282(7) Uani 1 1 d . . . H24 H 0.4957 0.5623 0.1602 0.034 Uiso 1 1 calc R . . C25 C 0.5281(3) 0.4744(3) 0.11851(9) 0.0298(8) Uani 1 1 d . . . H25 H 0.4871 0.4148 0.1265 0.036 Uiso 1 1 calc R . . C26 C 0.5823(3) 0.4647(4) 0.08383(9) 0.0487(11) Uani 1 1 d . . . H26A H 0.5397 0.4147 0.0694 0.058 Uiso 1 1 calc R . . H26B H 0.5812 0.5362 0.0726 0.058 Uiso 1 1 calc R . . C27 C 0.6955(3) 0.4257(3) 0.08509(9) 0.0452(10) Uani 1 1 d . . . H27A H 0.7369 0.4615 0.0666 0.054 Uiso 1 1 calc R . . H27B H 0.6961 0.3473 0.0804 0.054 Uiso 1 1 calc R . . C28 C 0.7509(3) 0.4457(3) 0.11843(8) 0.0268(7) Uani 1 1 d . . . H28 H 0.7827 0.3849 0.1292 0.032 Uiso 1 1 calc R . . C29 C 0.7610(3) 0.5435(3) 0.13547(8) 0.0276(7) Uani 1 1 d . . . H29 H 0.7993 0.5449 0.1565 0.033 Uiso 1 1 calc R . . C30 C 0.7142(3) 0.6473(3) 0.12211(11) 0.0460(10) Uani 1 1 d . . . H30A H 0.7205 0.6478 0.0968 0.055 Uiso 1 1 calc R . . H30B H 0.7575 0.7081 0.1310 0.055 Uiso 1 1 calc R . . C31 C 0.5977(3) 0.6652(3) 0.13166(11) 0.0432(10) Uani 1 1 d . . . H31A H 0.5951 0.7125 0.1521 0.052 Uiso 1 1 calc R . . H31B H 0.5618 0.7040 0.1126 0.052 Uiso 1 1 calc R . . N1 N 0.7588(2) 0.2633(2) 0.19133(6) 0.0207(6) Uani 1 1 d . . . N2 N 0.75306(19) 0.3728(2) 0.19240(6) 0.0198(5) Uani 1 1 d . . . N3 N 0.6179(2) 0.4802(2) 0.30915(6) 0.0216(6) Uani 1 1 d . . . N4 N 0.7237(2) 0.4720(2) 0.30126(6) 0.0207(5) Uani 1 1 d . . . O1 O 0.94078(17) 0.57208(17) 0.20766(5) 0.0249(5) Uani 1 1 d . . . O2 O 0.90953(16) 0.64573(17) 0.26067(5) 0.0217(4) Uani 1 1 d . . . Rh1 Rh 0.632645(17) 0.183139(17) 0.168352(5) 0.01757(6) Uani 1 1 d . . . Rh2 Rh 0.639027(18) 0.444592(17) 0.159558(5) 0.01740(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0201(17) 0.0188(15) 0.0190(15) 0.0010(12) 0.0004(12) -0.0026(12) C2 0.0190(16) 0.0269(17) 0.0251(16) -0.0005(13) -0.0072(12) -0.0019(13) C3 0.0195(18) 0.0225(16) 0.0264(17) 0.0021(13) -0.0016(13) 0.0018(12) C4 0.0187(17) 0.0202(16) 0.0205(15) 0.0011(12) 0.0009(12) -0.0023(12) C5 0.0190(15) 0.0171(15) 0.0212(15) -0.0001(11) 0.0005(12) -0.0030(12) C6 0.0220(17) 0.0197(16) 0.0192(14) 0.0012(13) 0.0016(12) -0.0023(13) C7 0.0258(19) 0.0270(17) 0.0296(17) 0.0134(13) 0.0024(14) 0.0026(13) C8 0.0175(17) 0.0273(18) 0.0364(18) 0.0090(14) 0.0026(14) 0.0079(13) C9 0.0227(16) 0.0247(17) 0.0249(16) -0.0030(14) 0.0047(13) -0.0082(14) C10 0.034(2) 0.0282(19) 0.0329(19) 0.0026(15) 0.0026(15) -0.0096(15) C11 0.039(2) 0.0313(19) 0.037(2) 0.0043(17) 0.0001(16) -0.0012(16) C12 0.079(3) 0.052(3) 0.050(3) 0.001(2) 0.005(2) 0.030(2) C13 0.0242(17) 0.0340(19) 0.0346(19) 0.0020(15) 0.0042(14) -0.0018(14) C14 0.0311(19) 0.050(2) 0.0382(19) 0.0026(17) -0.0024(16) -0.0033(18) C15 0.025(2) 0.090(4) 0.049(2) 0.008(2) -0.0012(18) 0.012(2) C16 0.0320(19) 0.022(2) 0.0328(18) 0.0007(14) -0.0136(15) -0.0107(14) C17 0.0208(17) 0.0220(17) 0.0302(17) -0.0024(14) -0.0043(13) -0.0036(12) C18 0.039(2) 0.0198(18) 0.072(3) -0.0028(17) 0.0023(19) -0.0060(17) C19 0.038(2) 0.0238(18) 0.074(3) -0.0066(19) -0.0100(19) -0.0001(16) C20 0.0219(17) 0.0247(18) 0.044(2) -0.0123(15) -0.0030(14) 0.0033(14) C21 0.0351(19) 0.0272(19) 0.039(2) -0.0078(16) 0.0122(15) 0.0014(16) C22 0.084(4) 0.069(3) 0.026(2) -0.0078(19) 0.007(2) 0.015(3) C23 0.065(3) 0.072(3) 0.029(2) 0.005(2) -0.0111(19) -0.036(3) C24 0.0279(18) 0.0295(19) 0.0273(17) 0.0075(15) 0.0052(14) 0.0090(15) C25 0.0236(18) 0.029(2) 0.0364(19) 0.0080(15) -0.0071(14) 0.0045(14) C26 0.058(3) 0.064(3) 0.0246(19) -0.0071(18) -0.0126(18) 0.017(2) C27 0.042(2) 0.066(3) 0.028(2) -0.0120(18) 0.0091(17) -0.017(2) C28 0.0257(18) 0.0298(19) 0.0248(16) 0.0046(15) 0.0071(14) -0.0018(14) C29 0.0269(18) 0.0281(19) 0.0276(17) 0.0063(14) 0.0034(14) -0.0078(15) C30 0.047(3) 0.026(2) 0.065(3) 0.0123(19) 0.015(2) -0.0021(17) C31 0.048(2) 0.024(2) 0.057(3) 0.0129(17) 0.0072(19) 0.0054(16) N1 0.0200(14) 0.0173(14) 0.0247(13) 0.0025(11) -0.0003(11) -0.0016(10) N2 0.0218(14) 0.0167(14) 0.0209(13) 0.0013(11) -0.0010(10) -0.0021(11) N3 0.0154(15) 0.0242(14) 0.0251(13) 0.0028(10) 0.0020(10) -0.0002(10) N4 0.0172(14) 0.0227(15) 0.0222(13) 0.0007(11) 0.0003(10) -0.0027(10) O1 0.0253(11) 0.0259(12) 0.0233(11) -0.0030(9) 0.0053(9) -0.0101(9) O2 0.0213(11) 0.0221(11) 0.0218(10) -0.0037(9) 0.0028(8) -0.0065(9) Rh1 0.01612(11) 0.01620(11) 0.02038(11) -0.00171(8) -0.00065(9) -0.00036(9) Rh2 0.01634(11) 0.01694(11) 0.01893(10) 0.00225(8) 0.00106(9) -0.00012(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.342(4) . ? C1 C2 1.386(4) . ? C1 C4 1.492(4) . ? C2 C3 1.372(5) . ? C2 H2 0.9500 . ? C3 N1 1.345(4) . ? C3 H3 0.9500 . ? C4 O1 1.440(3) . ? C4 C5 1.533(4) . ? C4 H4 1.0000 . ? C5 O2 1.441(3) . ? C5 C6 1.480(4) . ? C5 H5 1.0000 . ? C6 N4 1.353(4) . ? C6 C7 1.392(4) . ? C7 C8 1.379(4) . ? C7 H7 0.9500 . ? C8 N3 1.346(4) . ? C8 H8 0.9500 . ? C9 O2 1.433(3) . ? C9 O1 1.439(4) . ? C9 C10 1.520(5) . ? C9 C13 1.534(4) . ? C10 C11 1.518(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.520(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.512(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.520(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.390(5) . ? C16 C23 1.489(5) . ? C16 Rh1 2.120(3) . ? C16 H16 0.9500 . ? C17 C18 1.508(5) . ? C17 Rh1 2.152(3) . ? C17 H17 0.9500 . ? C18 C19 1.497(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.495(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.384(5) . ? C20 Rh1 2.126(3) . ? C20 H20 0.9500 . ? C21 C22 1.520(5) . ? C21 Rh1 2.141(3) . ? C21 H21 0.9500 . ? C22 C23 1.482(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.380(5) . ? C24 C31 1.506(5) . ? C24 Rh2 2.124(3) . ? C24 H24 0.9500 . ? C25 C26 1.516(5) . ? C25 Rh2 2.144(3) . ? C25 H25 0.9500 . ? C26 C27 1.486(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.492(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.389(5) . ? C28 Rh2 2.122(3) . ? C28 H28 0.9500 . ? C29 C30 1.506(5) . ? C29 Rh2 2.163(3) . ? C29 H29 0.9500 . ? C30 C31 1.509(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N1 N2 1.361(3) . ? N1 Rh1 2.060(3) . ? N2 Rh2 2.107(2) . ? N3 N4 1.352(4) . ? N3 Rh2 2.069(2) 5_665 ? N4 Rh1 2.104(2) 5_665 ? Rh1 N4 2.104(2) 5_665 ? Rh2 N3 2.069(2) 5_665 ? 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 C1 C2 109.5(3) . . ? N2 C1 C4 121.1(3) . . ? C2 C1 C4 129.2(3) . . ? C3 C2 C1 104.8(3) . . ? C3 C2 H2 127.6 . . ? C1 C2 H2 127.6 . . ? N1 C3 C2 110.0(3) . . ? N1 C3 H3 125.0 . . ? C2 C3 H3 125.0 . . ? O1 C4 C1 112.5(2) . . ? O1 C4 C5 103.3(2) . . ? C1 C4 C5 112.0(2) . . ? O1 C4 H4 109.6 . . ? C1 C4 H4 109.6 . . ? C5 C4 H4 109.6 . . ? O2 C5 C6 113.3(2) . . ? O2 C5 C4 101.3(2) . . ? C6 C5 C4 112.6(2) . . ? O2 C5 H5 109.8 . . ? C6 C5 H5 109.8 . . ? C4 C5 H5 109.8 . . ? N4 C6 C7 108.7(3) . . ? N4 C6 C5 119.8(3) . . ? C7 C6 C5 130.7(3) . . ? C8 C7 C6 104.9(3) . . ? C8 C7 H7 127.6 . . ? C6 C7 H7 127.6 . . ? N3 C8 C7 109.9(3) . . ? N3 C8 H8 125.1 . . ? C7 C8 H8 125.1 . . ? O2 C9 O1 106.1(2) . . ? O2 C9 C10 109.3(3) . . ? O1 C9 C10 109.6(3) . . ? O2 C9 C13 110.7(3) . . ? O1 C9 C13 107.4(3) . . ? C10 C9 C13 113.5(3) . . ? C11 C10 C9 115.3(3) . . ? C11 C10 H10A 108.5 . . ? C9 C10 H10A 108.5 . . ? C11 C10 H10B 108.5 . . ? C9 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C10 C11 C12 113.6(3) . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 116.0(3) . . ? C14 C13 H13A 108.3 . . ? C9 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? C9 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C13 C14 C15 112.8(3) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C23 125.2(3) . . ? C17 C16 Rh1 72.26(18) . . ? C23 C16 Rh1 111.8(2) . . ? C17 C16 H16 117.4 . . ? C23 C16 H16 117.4 . . ? Rh1 C16 H16 85.8 . . ? C16 C17 C18 122.2(3) . . ? C16 C17 Rh1 69.78(18) . . ? C18 C17 Rh1 111.9(2) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? Rh1 C17 H17 88.4 . . ? C19 C18 C17 114.3(3) . . ? C19 C18 H18A 108.7 . . ? C17 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C18 115.8(3) . . ? C20 C19 H19A 108.3 . . ? C18 C19 H19A 108.3 . . ? C20 C19 H19B 108.3 . . ? C18 C19 H19B 108.3 . . ? H19A C19 H19B 107.4 . . ? C21 C20 C19 124.4(3) . . ? C21 C20 Rh1 71.64(19) . . ? C19 C20 Rh1 110.5(2) . . ? C21 C20 H20 117.8 . . ? C19 C20 H20 117.8 . . ? Rh1 C20 H20 87.8 . . ? C20 C21 C22 123.0(4) . . ? C20 C21 Rh1 70.49(19) . . ? C22 C21 Rh1 111.9(2) . . ? C20 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? Rh1 C21 H21 87.7 . . ? C23 C22 C21 114.8(3) . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22B 108.6 . . ? C21 C22 H22B 108.6 . . ? H22A C22 H22B 107.5 . . ? C22 C23 C16 114.8(3) . . ? C22 C23 H23A 108.6 . . ? C16 C23 H23A 108.6 . . ? C22 C23 H23B 108.6 . . ? C16 C23 H23B 108.6 . . ? H23A C23 H23B 107.5 . . ? C25 C24 C31 125.9(3) . . ? C25 C24 Rh2 71.91(18) . . ? C31 C24 Rh2 109.7(2) . . ? C25 C24 H24 117.0 . . ? C31 C24 H24 117.0 . . ? Rh2 C24 H24 88.3 . . ? C24 C25 C26 124.1(3) . . ? C24 C25 Rh2 70.37(19) . . ? C26 C25 Rh2 111.7(2) . . ? C24 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? Rh2 C25 H25 88.0 . . ? C27 C26 C25 114.5(3) . . ? C27 C26 H26A 108.6 . . ? C25 C26 H26A 108.6 . . ? C27 C26 H26B 108.6 . . ? C25 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C26 C27 C28 114.2(3) . . ? C26 C27 H27A 108.7 . . ? C28 C27 H27A 108.7 . . ? C26 C27 H27B 108.7 . . ? C28 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? C29 C28 C27 127.2(3) . . ? C29 C28 Rh2 72.71(17) . . ? C27 C28 Rh2 110.9(2) . . ? C29 C28 H28 116.4 . . ? C27 C28 H28 116.4 . . ? Rh2 C28 H28 86.1 . . ? C28 C29 C30 123.1(3) . . ? C28 C29 Rh2 69.49(17) . . ? C30 C29 Rh2 111.4(2) . . ? C28 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? Rh2 C29 H29 89.1 . . ? C29 C30 C31 114.2(3) . . ? C29 C30 H30A 108.7 . . ? C31 C30 H30A 108.7 . . ? C29 C30 H30B 108.7 . . ? C31 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C24 C31 C30 115.1(3) . . ? C24 C31 H31A 108.5 . . ? C30 C31 H31A 108.5 . . ? C24 C31 H31B 108.5 . . ? C30 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? C3 N1 N2 107.7(3) . . ? C3 N1 Rh1 134.4(2) . . ? N2 N1 Rh1 117.10(19) . . ? C1 N2 N1 108.0(2) . . ? C1 N2 Rh2 135.5(2) . . ? N1 N2 Rh2 116.01(19) . . ? C8 N3 N4 107.9(2) . . ? C8 N3 Rh2 135.2(2) . 5_665 ? N4 N3 Rh2 116.39(18) . 5_665 ? N3 N4 C6 108.6(2) . . ? N3 N4 Rh1 116.83(18) . 5_665 ? C6 N4 Rh1 133.9(2) . 5_665 ? C9 O1 C4 108.6(2) . . ? C9 O2 C5 106.0(2) . . ? N1 Rh1 N4 87.58(10) . 5_665 ? N1 Rh1 C16 156.72(11) . . ? N4 Rh1 C16 91.57(12) 5_665 . ? N1 Rh1 C20 93.01(11) . . ? N4 Rh1 C20 158.47(12) 5_665 . ? C16 Rh1 C20 96.15(13) . . ? N1 Rh1 C21 92.84(12) . . ? N4 Rh1 C21 163.64(12) 5_665 . ? C16 Rh1 C21 81.61(14) . . ? C20 Rh1 C21 37.86(14) . . ? N1 Rh1 C17 165.29(11) . . ? N4 Rh1 C17 91.85(11) 5_665 . ? C16 Rh1 C17 37.97(12) . . ? C20 Rh1 C17 82.19(13) . . ? C21 Rh1 C17 91.81(13) . . ? N3 Rh2 N2 87.84(9) 5_665 . ? N3 Rh2 C28 156.43(12) 5_665 . ? N2 Rh2 C28 91.38(11) . . ? N3 Rh2 C24 92.67(11) 5_665 . ? N2 Rh2 C24 158.80(12) . . ? C28 Rh2 C24 96.41(12) . . ? N3 Rh2 C25 92.70(12) 5_665 . ? N2 Rh2 C25 163.45(12) . . ? C28 Rh2 C25 81.56(13) . . ? C24 Rh2 C25 37.73(13) . . ? N3 Rh2 C29 165.76(11) 5_665 . ? N2 Rh2 C29 91.98(11) . . ? C28 Rh2 C29 37.80(12) . . ? C24 Rh2 C29 82.41(13) . . ? C25 Rh2 C29 91.51(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 62.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.405 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.056