# ja010647z.cif data_mn890 #Manuscript Title: A Remarkable Skeletal Rearrangement of a Coordinated Tetrapyrrole. #Chemical Consequences of Palladium pi-Coordination to a Bilindione. #Authors: Pamela A. Lord, Bruce C. Noll, Marilyn M. Olmstead and Alan L. Balch _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H42 N4 O3 Pd' _chemical_formula_weight 673.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 '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 13.868(3) _cell_length_b 14.966(2) _cell_length_c 15.018(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.527(11) _cell_angle_gamma 90.00 _cell_volume 3113.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 6784 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 31 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.8441 _exptl_absorpt_correction_T_max 0.9609 _exptl_absorpt_process_details ; Blessing, R. H., Acta Cryst. (1995). A51, 33-38. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28078 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 31.29 _reflns_number_total 9436 _reflns_number_gt 6813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.03, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0215P)^2^+5.2675P] 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 0.00014(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9436 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.007 _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 Pd Pd 0.632888(16) 0.986644(14) 0.211057(14) 0.02202(6) Uani 1 1 d . . . O1 O 0.72787(16) 0.83793(15) 0.06746(14) 0.0351(5) Uani 1 1 d . . . O2 O 0.7088(2) 0.75609(16) 0.46578(15) 0.0452(6) Uani 1 1 d . . . O3 O 0.55365(16) 0.79248(14) 0.14290(14) 0.0324(5) Uani 1 1 d . . . N1 N 0.63796(17) 0.96957(15) 0.07827(15) 0.0236(5) Uani 1 1 d . . . N2 N 0.61262(17) 1.11760(15) 0.19272(15) 0.0236(5) Uani 1 1 d . . . N3 N 0.64889(17) 1.00552(16) 0.33881(15) 0.0250(5) Uani 1 1 d . . . N4 N 0.63976(17) 0.85819(15) 0.25714(15) 0.0239(5) Uani 1 1 d . . . C1 C 0.6812(2) 0.8985(2) 0.03239(18) 0.0263(6) Uani 1 1 d . . . C2 C 0.6694(2) 0.9157(2) -0.06552(19) 0.0284(6) Uani 1 1 d . . . C3 C 0.6321(2) 0.99753(19) -0.07547(18) 0.0257(6) Uani 1 1 d . . . C4 C 0.6130(2) 1.03168(18) 0.01554(18) 0.0239(6) Uani 1 1 d . . . C5 C 0.5841(2) 1.11840(19) 0.03086(18) 0.0249(6) Uani 1 1 d . . . H5 H 0.5593 1.1523 -0.0185 0.030 Uiso 1 1 calc R . . C6 C 0.5891(2) 1.15952(18) 0.11461(18) 0.0240(6) Uani 1 1 d . . . C7 C 0.5778(2) 1.25556(19) 0.13067(19) 0.0269(6) Uani 1 1 d . . . C8 C 0.5958(2) 1.26877(19) 0.21913(19) 0.0278(6) Uani 1 1 d . . . C9 C 0.6170(2) 1.18171(19) 0.25931(19) 0.0252(6) Uani 1 1 d . . . C10 C 0.6374(2) 1.1665(2) 0.34821(19) 0.0273(6) Uani 1 1 d . . . H10 H 0.6410 1.2169 0.3867 0.033 Uiso 1 1 calc R . . C11 C 0.6534(2) 1.08126(19) 0.38661(18) 0.0257(6) Uani 1 1 d . . . C12 C 0.6779(2) 1.0584(2) 0.47868(19) 0.0277(6) Uani 1 1 d . . . C13 C 0.6902(2) 0.9671(2) 0.48370(19) 0.0289(6) Uani 1 1 d . . . C14 C 0.6714(2) 0.93321(19) 0.39284(19) 0.0267(6) Uani 1 1 d . . . C15 C 0.6642(2) 0.8520(2) 0.34643(18) 0.0259(6) Uani 1 1 d . . . C16 C 0.6755(2) 0.7628(2) 0.38912(19) 0.0275(6) Uani 1 1 d . . . C17 C 0.6496(2) 0.68338(19) 0.33653(19) 0.0250(6) Uani 1 1 d . . . C18 C 0.6221(2) 0.69312(19) 0.25046(19) 0.0271(6) Uani 1 1 d . . . C19 C 0.6029(2) 0.78381(19) 0.21171(19) 0.0259(6) Uani 1 1 d . . . C20 C 0.7035(3) 0.8519(2) -0.1334(2) 0.0420(8) Uani 1 1 d . . . H20A H 0.6996 0.7905 -0.1095 0.050 Uiso 1 1 calc R . . H20B H 0.6596 0.8554 -0.1872 0.050 Uiso 1 1 calc R . . C21 C 0.8039(4) 0.8690(3) -0.1598(4) 0.094(2) Uani 1 1 d . . . H21A H 0.8084 0.9294 -0.1843 0.140 Uiso 1 1 calc R . . H21B H 0.8214 0.8253 -0.2050 0.140 Uiso 1 1 calc R . . H21C H 0.8483 0.8634 -0.1074 0.140 Uiso 1 1 calc R . . C22 C 0.6192(2) 1.0521(2) -0.15862(19) 0.0300(6) Uani 1 1 d . . . H22A H 0.5576 1.0854 -0.1572 0.036 Uiso 1 1 calc R . . H22B H 0.6153 1.0117 -0.2109 0.036 Uiso 1 1 calc R . . C23 C 0.7022(3) 1.1184(2) -0.1691(2) 0.0442(9) Uani 1 1 d . . . H23A H 0.7060 1.1588 -0.1177 0.066 Uiso 1 1 calc R . . H23B H 0.6905 1.1532 -0.2238 0.066 Uiso 1 1 calc R . . H23C H 0.7630 1.0855 -0.1725 0.066 Uiso 1 1 calc R . . C24 C 0.5534(2) 1.3249(2) 0.0610(2) 0.0340(7) Uani 1 1 d . . . H24A H 0.5707 1.3017 0.0021 0.041 Uiso 1 1 calc R . . H24B H 0.5930 1.3789 0.0737 0.041 Uiso 1 1 calc R . . C25 C 0.4483(3) 1.3510(3) 0.0566(3) 0.0467(9) Uani 1 1 d . . . H25A H 0.4095 1.3014 0.0317 0.070 Uiso 1 1 calc R . . H25B H 0.4392 1.4038 0.0184 0.070 Uiso 1 1 calc R . . H25C H 0.4278 1.3648 0.1166 0.070 Uiso 1 1 calc R . . C26 C 0.5932(2) 1.3548(2) 0.2702(2) 0.0337(7) Uani 1 1 d . . . H26A H 0.5992 1.4055 0.2284 0.040 Uiso 1 1 calc R . . H26B H 0.6489 1.3570 0.3137 0.040 Uiso 1 1 calc R . . C27 C 0.4999(3) 1.3650(2) 0.3198(2) 0.0501(10) Uani 1 1 d . . . H27A H 0.4445 1.3632 0.2770 0.075 Uiso 1 1 calc R . . H27B H 0.5006 1.4223 0.3514 0.075 Uiso 1 1 calc R . . H27C H 0.4948 1.3162 0.3628 0.075 Uiso 1 1 calc R . . C28 C 0.6814(2) 1.1255(2) 0.5533(2) 0.0332(7) Uani 1 1 d . . . H28A H 0.7083 1.1824 0.5315 0.040 Uiso 1 1 calc R . . H28B H 0.7251 1.1033 0.6023 0.040 Uiso 1 1 calc R . . C29 C 0.5817(3) 1.1429(3) 0.5891(2) 0.0482(9) Uani 1 1 d . . . H29A H 0.5391 1.1676 0.5414 0.072 Uiso 1 1 calc R . . H29B H 0.5875 1.1856 0.6385 0.072 Uiso 1 1 calc R . . H29C H 0.5547 1.0867 0.6103 0.072 Uiso 1 1 calc R . . C30 C 0.7142(3) 0.9168(2) 0.5681(2) 0.0365(7) Uani 1 1 d . . . H30A H 0.7452 0.9581 0.6122 0.044 Uiso 1 1 calc R . . H30B H 0.7612 0.8692 0.5556 0.044 Uiso 1 1 calc R . . C31 C 0.6257(3) 0.8746(3) 0.6084(2) 0.0501(10) Uani 1 1 d . . . H31A H 0.5790 0.9214 0.6215 0.075 Uiso 1 1 calc R . . H31B H 0.6454 0.8434 0.6637 0.075 Uiso 1 1 calc R . . H31C H 0.5960 0.8319 0.5660 0.075 Uiso 1 1 calc R . . C32 C 0.6589(2) 0.5961(2) 0.38546(19) 0.0291(6) Uani 1 1 d . . . H32A H 0.7223 0.5938 0.4185 0.035 Uiso 1 1 calc R . . H32B H 0.6566 0.5464 0.3418 0.035 Uiso 1 1 calc R . . C33 C 0.5786(3) 0.5834(3) 0.4509(3) 0.0500(10) Uani 1 1 d . . . H33A H 0.5798 0.6330 0.4935 0.075 Uiso 1 1 calc R . . H33B H 0.5886 0.5269 0.4831 0.075 Uiso 1 1 calc R . . H33C H 0.5160 0.5820 0.4181 0.075 Uiso 1 1 calc R . . C34 C 0.6021(2) 0.6166(2) 0.1855(2) 0.0334(7) Uani 1 1 d . . . H34A H 0.6196 0.6355 0.1252 0.040 Uiso 1 1 calc R . . H34B H 0.6434 0.5651 0.2032 0.040 Uiso 1 1 calc R . . C35 C 0.4977(3) 0.5875(2) 0.1822(2) 0.0450(9) Uani 1 1 d . . . H35A H 0.4811 0.5645 0.2407 0.068 Uiso 1 1 calc R . . H35B H 0.4879 0.5404 0.1374 0.068 Uiso 1 1 calc R . . H35C H 0.4562 0.6386 0.1664 0.068 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 Pd 0.02730(11) 0.01944(10) 0.01922(10) 0.00017(8) -0.00019(7) -0.00065(9) O1 0.0449(13) 0.0346(12) 0.0258(11) 0.0011(9) -0.0003(9) 0.0119(10) O2 0.0715(18) 0.0353(13) 0.0273(12) 0.0054(9) -0.0140(11) 0.0011(12) O3 0.0432(13) 0.0247(11) 0.0281(11) 0.0020(8) -0.0107(9) -0.0002(9) N1 0.0288(12) 0.0231(12) 0.0185(11) 0.0028(8) -0.0022(9) -0.0001(9) N2 0.0270(12) 0.0186(11) 0.0251(12) 0.0003(9) 0.0018(9) -0.0014(9) N3 0.0314(12) 0.0226(12) 0.0209(11) -0.0001(9) 0.0005(9) -0.0016(10) N4 0.0316(13) 0.0208(12) 0.0192(11) 0.0023(8) -0.0008(9) 0.0000(10) C1 0.0290(15) 0.0274(15) 0.0225(14) -0.0014(11) -0.0003(11) -0.0017(12) C2 0.0329(16) 0.0300(16) 0.0217(14) 0.0008(11) -0.0037(12) -0.0005(12) C3 0.0267(13) 0.0303(16) 0.0199(12) -0.0020(10) -0.0008(10) -0.0035(11) C4 0.0232(13) 0.0266(15) 0.0214(13) 0.0015(10) -0.0026(10) -0.0038(11) C5 0.0268(14) 0.0260(15) 0.0215(13) 0.0026(10) -0.0030(11) -0.0010(11) C6 0.0250(14) 0.0223(14) 0.0249(14) 0.0027(10) 0.0029(11) 0.0013(11) C7 0.0302(15) 0.0223(14) 0.0283(15) -0.0015(11) 0.0031(12) 0.0002(11) C8 0.0324(15) 0.0221(14) 0.0290(15) -0.0006(11) 0.0026(12) 0.0020(12) C9 0.0261(14) 0.0238(14) 0.0258(14) -0.0008(11) 0.0032(11) -0.0017(11) C10 0.0317(15) 0.0244(15) 0.0260(14) -0.0036(11) 0.0039(12) -0.0010(12) C11 0.0283(15) 0.0270(15) 0.0215(14) -0.0011(11) -0.0013(11) -0.0012(12) C12 0.0287(15) 0.0293(16) 0.0249(14) -0.0004(11) 0.0000(11) -0.0033(12) C13 0.0324(15) 0.0316(17) 0.0227(14) 0.0021(11) -0.0009(11) -0.0042(12) C14 0.0289(15) 0.0248(15) 0.0262(14) 0.0030(11) -0.0015(11) -0.0025(11) C15 0.0281(15) 0.0285(15) 0.0209(13) 0.0035(11) 0.0001(11) -0.0002(12) C16 0.0325(15) 0.0278(15) 0.0223(14) 0.0041(11) 0.0011(11) 0.0026(12) C17 0.0212(13) 0.0246(14) 0.0292(15) 0.0034(11) 0.0012(11) 0.0036(11) C18 0.0311(15) 0.0227(14) 0.0274(15) 0.0039(11) 0.0001(12) 0.0000(12) C19 0.0314(15) 0.0208(14) 0.0253(14) 0.0016(10) -0.0011(12) -0.0011(11) C20 0.067(2) 0.0332(18) 0.0258(16) -0.0016(13) 0.0009(15) 0.0101(17) C21 0.106(4) 0.054(3) 0.128(5) -0.019(3) 0.078(4) 0.000(3) C22 0.0378(17) 0.0311(16) 0.0206(14) 0.0013(11) -0.0047(12) 0.0038(13) C23 0.054(2) 0.044(2) 0.0340(18) 0.0082(15) 0.0048(16) -0.0100(17) C24 0.0458(19) 0.0243(15) 0.0319(16) 0.0034(12) 0.0012(14) 0.0061(13) C25 0.047(2) 0.047(2) 0.045(2) 0.0053(16) -0.0015(16) 0.0081(17) C26 0.0462(19) 0.0228(15) 0.0320(16) -0.0016(12) 0.0003(14) 0.0031(13) C27 0.073(3) 0.037(2) 0.042(2) -0.0044(15) 0.0219(19) 0.0102(18) C28 0.0391(18) 0.0342(17) 0.0259(15) -0.0052(12) -0.0032(13) -0.0043(14) C29 0.045(2) 0.058(2) 0.041(2) -0.0158(17) -0.0001(16) 0.0069(18) C30 0.049(2) 0.0350(18) 0.0243(15) 0.0010(12) -0.0079(14) -0.0037(15) C31 0.065(3) 0.056(2) 0.0293(18) 0.0073(16) 0.0037(17) -0.012(2) C32 0.0307(16) 0.0287(15) 0.0280(15) 0.0048(11) 0.0022(12) 0.0032(12) C33 0.055(2) 0.048(2) 0.049(2) 0.0156(17) 0.0191(18) -0.0030(18) C34 0.0425(18) 0.0253(16) 0.0321(16) 0.0042(12) -0.0024(13) -0.0013(13) C35 0.052(2) 0.039(2) 0.044(2) 0.0006(15) -0.0024(17) -0.0074(17) _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 Pd N3 1.942(2) . ? Pd N2 1.997(2) . ? Pd N1 2.015(2) . ? Pd N4 2.044(2) . ? O1 C1 1.219(3) . ? O2 C16 1.225(3) . ? O3 C19 1.220(3) . ? N1 C4 1.357(3) . ? N1 C1 1.415(4) . ? N2 C6 1.357(3) . ? N2 C9 1.385(4) . ? N3 C11 1.342(4) . ? N3 C14 1.380(4) . ? N4 C15 1.372(3) . ? N4 C19 1.391(4) . ? C1 C2 1.495(4) . ? C2 C3 1.335(4) . ? C2 C20 1.489(4) . ? C3 C4 1.494(4) . ? C3 C22 1.496(4) . ? C4 C5 1.381(4) . ? C5 C6 1.399(4) . ? C6 C7 1.467(4) . ? C7 C8 1.355(4) . ? C7 C24 1.502(4) . ? C8 C9 1.460(4) . ? C8 C26 1.501(4) . ? C9 C10 1.371(4) . ? C10 C11 1.414(4) . ? C11 C12 1.450(4) . ? C12 C13 1.378(4) . ? C12 C28 1.504(4) . ? C13 C14 1.468(4) . ? C13 C30 1.499(4) . ? C14 C15 1.402(4) . ? C15 C16 1.487(4) . ? C16 C17 1.463(4) . ? C17 C18 1.340(4) . ? C17 C32 1.502(4) . ? C18 C19 1.496(4) . ? C18 C34 1.521(4) . ? C20 C21 1.488(6) . ? C22 C23 1.533(5) . ? C24 C25 1.508(5) . ? C26 C27 1.528(5) . ? C28 C29 1.527(5) . ? C30 C31 1.529(5) . ? C32 C33 1.530(4) . ? C34 C35 1.511(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 N3 Pd N2 90.16(9) . . ? N3 Pd N1 171.37(10) . . ? N2 Pd N1 89.94(9) . . ? N3 Pd N4 78.51(9) . . ? N2 Pd N4 166.84(9) . . ? N1 Pd N4 102.28(9) . . ? C4 N1 C1 106.1(2) . . ? C4 N1 Pd 125.53(19) . . ? C1 N1 Pd 127.68(18) . . ? C6 N2 C9 107.8(2) . . ? C6 N2 Pd 126.85(19) . . ? C9 N2 Pd 125.36(19) . . ? C11 N3 C14 110.1(2) . . ? C11 N3 Pd 130.7(2) . . ? C14 N3 Pd 118.67(19) . . ? C15 N4 C19 119.7(2) . . ? C15 N4 Pd 113.60(18) . . ? C19 N4 Pd 125.16(18) . . ? O1 C1 N1 125.2(3) . . ? O1 C1 C2 125.9(3) . . ? N1 C1 C2 108.6(2) . . ? C3 C2 C20 130.1(3) . . ? C3 C2 C1 107.1(3) . . ? C20 C2 C1 122.6(3) . . ? C2 C3 C4 107.1(2) . . ? C2 C3 C22 128.7(3) . . ? C4 C3 C22 123.9(3) . . ? N1 C4 C5 126.5(3) . . ? N1 C4 C3 110.5(2) . . ? C5 C4 C3 122.6(2) . . ? C4 C5 C6 124.1(3) . . ? N2 C6 C5 125.0(3) . . ? N2 C6 C7 109.5(2) . . ? C5 C6 C7 125.3(3) . . ? C8 C7 C6 106.7(3) . . ? C8 C7 C24 127.5(3) . . ? C6 C7 C24 125.8(3) . . ? C7 C8 C9 107.5(3) . . ? C7 C8 C26 128.2(3) . . ? C9 C8 C26 124.3(3) . . ? C10 C9 N2 126.1(3) . . ? C10 C9 C8 125.4(3) . . ? N2 C9 C8 108.5(2) . . ? C9 C10 C11 124.7(3) . . ? N3 C11 C10 122.8(3) . . ? N3 C11 C12 108.3(2) . . ? C10 C11 C12 128.9(3) . . ? C13 C12 C11 108.0(3) . . ? C13 C12 C28 128.4(3) . . ? C11 C12 C28 123.4(3) . . ? C12 C13 C14 106.0(3) . . ? C12 C13 C30 124.5(3) . . ? C14 C13 C30 129.5(3) . . ? N3 C14 C15 112.2(2) . . ? N3 C14 C13 107.6(2) . . ? C15 C14 C13 140.1(3) . . ? N4 C15 C14 115.9(3) . . ? N4 C15 C16 119.9(3) . . ? C14 C15 C16 124.1(3) . . ? O2 C16 C17 120.9(3) . . ? O2 C16 C15 120.4(3) . . ? C17 C16 C15 118.6(2) . . ? C18 C17 C16 119.0(3) . . ? C18 C17 C32 125.6(3) . . ? C16 C17 C32 115.4(2) . . ? C17 C18 C19 120.8(3) . . ? C17 C18 C34 124.9(3) . . ? C19 C18 C34 114.1(2) . . ? O3 C19 N4 120.7(3) . . ? O3 C19 C18 120.6(3) . . ? N4 C19 C18 118.7(2) . . ? C21 C20 C2 113.7(3) . . ? C3 C22 C23 112.1(3) . . ? C7 C24 C25 113.4(3) . . ? C8 C26 C27 112.0(3) . . ? C12 C28 C29 112.1(3) . . ? C13 C30 C31 113.0(3) . . ? C17 C32 C33 111.9(3) . . ? C35 C34 C18 112.7(3) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 31.29 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.258 _refine_diff_density_min -1.179 _refine_diff_density_rms 0.101 #===END