# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Vicente, J' _publ_contact_author_email jvs1@um.es _publ_author_name J.Vicente data_jaj561s _database_code_depnum_ccdc_archive 'CCDC 874140' #TrackingRef '- jaj561s_joe6912.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H25 Cl N2 Pd' _chemical_formula_weight 459.29 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2021(7) _cell_length_b 10.3321(7) _cell_length_c 11.8365(9) _cell_angle_alpha 73.850(2) _cell_angle_beta 78.692(2) _cell_angle_gamma 65.084(2) _cell_volume 976.33(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8692 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.60 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 1.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7988 _exptl_absorpt_correction_T_max 0.9372 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11858 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.60 _reflns_number_total 4558 _reflns_number_gt 4424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. NH2 free with SADI, rigid methyls, others riding ; _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^)+(0.0218P)^2^+0.7336P] 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 'NH2 free with SADI, rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4558 _refine_ls_number_parameters 246 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.003 _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 0.725291(14) 0.161090(13) 0.861206(10) 0.01273(5) Uani 1 1 d . . . Cl1 Cl 0.53304(6) 0.16379(5) 1.03624(4) 0.02186(10) Uani 1 1 d . . . N1 N 0.61599(18) 0.07925(16) 0.77912(13) 0.0145(3) Uani 1 1 d D . . H01A H 0.578(2) 0.026(2) 0.8319(17) 0.014(5) Uiso 1 1 d D . . H01B H 0.685(2) 0.022(2) 0.7386(18) 0.020(5) Uiso 1 1 d D . . N2 N 0.84141(17) 0.24085(16) 0.93818(13) 0.0157(3) Uani 1 1 d . . . C1 C 0.8803(2) 0.15825(19) 0.71752(15) 0.0141(3) Uani 1 1 d . . . C2 C 0.8499(2) 0.28904(19) 0.63197(15) 0.0150(3) Uani 1 1 d . . . C3 C 0.7017(2) 0.41797(19) 0.65248(15) 0.0159(3) Uani 1 1 d . . . C4 C 0.5495(2) 0.41722(19) 0.65054(15) 0.0160(3) Uani 1 1 d . . . C5 C 0.5323(2) 0.29808(19) 0.60934(15) 0.0153(3) Uani 1 1 d . . . H5A H 0.6363 0.2474 0.5667 0.018 Uiso 1 1 calc R . . H5B H 0.4516 0.3471 0.5507 0.018 Uiso 1 1 calc R . . C6 C 0.4846(2) 0.17911(19) 0.69952(15) 0.0157(3) Uani 1 1 d . . . C7 C 0.9549(2) 0.2951(2) 0.52987(15) 0.0185(3) Uani 1 1 d . . . H7 H 0.9362 0.3852 0.4739 0.022 Uiso 1 1 calc R . . C8 C 1.0862(2) 0.1706(2) 0.50958(16) 0.0213(4) Uani 1 1 d . . . H8 H 1.1564 0.1751 0.4395 0.026 Uiso 1 1 calc R . . C9 C 1.1145(2) 0.0392(2) 0.59230(16) 0.0208(4) Uani 1 1 d . . . H9 H 1.2029 -0.0469 0.5779 0.025 Uiso 1 1 calc R . . C10 C 1.0134(2) 0.0337(2) 0.69644(16) 0.0181(3) Uani 1 1 d . . . H10 H 1.0353 -0.0558 0.7537 0.022 Uiso 1 1 calc R . . C11 C 0.4139(2) 0.5371(2) 0.67687(16) 0.0203(4) Uani 1 1 d . . . H11 H 0.3100 0.5402 0.6741 0.024 Uiso 1 1 calc R . . C12 C 0.4273(2) 0.6522(2) 0.70704(16) 0.0241(4) Uani 1 1 d . . . H12 H 0.3331 0.7306 0.7277 0.029 Uiso 1 1 calc R . . C13 C 0.5773(3) 0.6528(2) 0.70705(17) 0.0237(4) Uani 1 1 d . . . H13 H 0.5868 0.7319 0.7267 0.028 Uiso 1 1 calc R . . C14 C 0.7135(2) 0.5370(2) 0.67821(16) 0.0201(4) Uani 1 1 d . . . H14 H 0.8166 0.5385 0.6759 0.024 Uiso 1 1 calc R . . C15 C 0.4613(2) 0.0856(2) 0.63000(17) 0.0222(4) Uani 1 1 d . . . H15A H 0.5611 0.0428 0.5815 0.033 Uiso 1 1 calc R . . H15B H 0.3742 0.1469 0.5788 0.033 Uiso 1 1 calc R . . H15C H 0.4338 0.0072 0.6851 0.033 Uiso 1 1 calc R . . C16 C 0.3319(2) 0.2423(2) 0.77756(17) 0.0220(4) Uani 1 1 d . . . H16A H 0.3044 0.1626 0.8304 0.033 Uiso 1 1 calc R . . H16B H 0.2436 0.3069 0.7280 0.033 Uiso 1 1 calc R . . H16C H 0.3490 0.2983 0.8246 0.033 Uiso 1 1 calc R . . C22 C 0.7540(2) 0.3589(2) 0.98484(16) 0.0199(4) Uani 1 1 d . . . H22 H 0.6443 0.4116 0.9696 0.024 Uiso 1 1 calc R . . C23 C 0.8179(2) 0.4063(2) 1.05401(16) 0.0216(4) Uani 1 1 d . . . H23 H 0.7523 0.4908 1.0845 0.026 Uiso 1 1 calc R . . C24 C 0.9775(2) 0.3309(2) 1.07921(15) 0.0202(4) Uani 1 1 d . . . C25 C 1.0695(2) 0.2142(2) 1.02483(15) 0.0188(4) Uani 1 1 d . . . H25 H 1.1808 0.1628 1.0354 0.023 Uiso 1 1 calc R . . C26 C 0.9988(2) 0.17317(19) 0.95544(15) 0.0174(3) Uani 1 1 d . . . H26 H 1.0640 0.0940 0.9185 0.021 Uiso 1 1 calc R . . C27 C 1.0469(3) 0.3690(2) 1.16432(17) 0.0278(4) Uani 1 1 d . . . H27A H 0.9963 0.4748 1.1593 0.042 Uiso 1 1 calc R . . H27B H 1.1631 0.3397 1.1442 0.042 Uiso 1 1 calc R . . H27C H 1.0263 0.3174 1.2449 0.042 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 0.01441(7) 0.01391(7) 0.00998(7) -0.00240(5) -0.00015(4) -0.00617(5) Cl1 0.0292(2) 0.0277(2) 0.0148(2) -0.00794(17) 0.00667(16) -0.01854(19) N1 0.0157(7) 0.0145(7) 0.0128(7) -0.0027(6) 0.0006(5) -0.0063(6) N2 0.0175(7) 0.0177(7) 0.0127(7) -0.0027(5) 0.0001(5) -0.0086(6) C1 0.0146(8) 0.0174(8) 0.0125(8) -0.0038(6) -0.0009(6) -0.0081(6) C2 0.0149(8) 0.0181(8) 0.0139(8) -0.0038(6) -0.0021(6) -0.0077(7) C3 0.0200(8) 0.0151(8) 0.0102(8) 0.0002(6) -0.0016(6) -0.0063(7) C4 0.0195(8) 0.0154(8) 0.0099(7) 0.0000(6) -0.0008(6) -0.0058(7) C5 0.0149(8) 0.0176(8) 0.0121(8) -0.0022(6) -0.0017(6) -0.0055(6) C6 0.0145(8) 0.0184(8) 0.0147(8) -0.0035(6) -0.0013(6) -0.0070(7) C7 0.0191(8) 0.0217(9) 0.0135(8) 0.0008(7) -0.0016(6) -0.0096(7) C8 0.0165(8) 0.0294(10) 0.0150(8) -0.0035(7) 0.0015(6) -0.0082(7) C9 0.0169(8) 0.0227(9) 0.0185(9) -0.0050(7) -0.0006(7) -0.0037(7) C10 0.0188(8) 0.0175(8) 0.0164(8) -0.0015(7) -0.0017(7) -0.0070(7) C11 0.0195(9) 0.0189(9) 0.0155(8) 0.0011(7) 0.0000(7) -0.0046(7) C12 0.0305(10) 0.0144(8) 0.0159(9) -0.0016(7) 0.0026(7) -0.0009(7) C13 0.0377(11) 0.0158(8) 0.0177(9) -0.0044(7) -0.0021(8) -0.0103(8) C14 0.0259(9) 0.0195(9) 0.0161(8) -0.0020(7) -0.0037(7) -0.0103(7) C15 0.0243(9) 0.0247(9) 0.0225(9) -0.0055(7) -0.0057(7) -0.0125(8) C16 0.0173(9) 0.0229(9) 0.0226(9) -0.0041(7) 0.0035(7) -0.0078(7) C22 0.0179(8) 0.0209(9) 0.0208(9) -0.0067(7) 0.0022(7) -0.0079(7) C23 0.0256(9) 0.0231(9) 0.0196(9) -0.0103(7) 0.0055(7) -0.0124(8) C24 0.0286(10) 0.0247(9) 0.0118(8) -0.0016(7) -0.0003(7) -0.0170(8) C25 0.0198(9) 0.0211(9) 0.0147(8) 0.0014(7) -0.0034(7) -0.0097(7) C26 0.0186(8) 0.0170(8) 0.0147(8) -0.0021(6) 0.0008(6) -0.0071(7) C27 0.0390(12) 0.0354(11) 0.0171(9) -0.0056(8) -0.0041(8) -0.0217(9) _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 C1 1.9920(17) . ? Pd1 N2 2.0476(15) . ? Pd1 N1 2.0561(15) . ? Pd1 Cl1 2.4446(5) . ? N1 C6 1.506(2) . ? N2 C26 1.346(2) . ? N2 C22 1.346(2) . ? C1 C10 1.396(2) . ? C1 C2 1.400(2) . ? C2 C7 1.396(2) . ? C2 C3 1.488(2) . ? C3 C14 1.397(2) . ? C3 C4 1.409(2) . ? C4 C11 1.396(2) . ? C4 C5 1.519(2) . ? C5 C6 1.544(2) . ? C6 C16 1.519(2) . ? C6 C15 1.530(2) . ? C7 C8 1.386(3) . ? C8 C9 1.390(3) . ? C9 C10 1.394(3) . ? C11 C12 1.390(3) . ? C12 C13 1.383(3) . ? C13 C14 1.384(3) . ? C22 C23 1.382(3) . ? C23 C24 1.390(3) . ? C24 C25 1.394(3) . ? C24 C27 1.504(3) . ? C25 C26 1.383(2) . ? 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 C1 Pd1 N2 90.94(6) . . ? C1 Pd1 N1 86.93(6) . . ? N2 Pd1 N1 177.82(6) . . ? C1 Pd1 Cl1 179.27(5) . . ? N2 Pd1 Cl1 89.78(4) . . ? N1 Pd1 Cl1 92.34(4) . . ? C6 N1 Pd1 121.36(11) . . ? C26 N2 C22 117.50(15) . . ? C26 N2 Pd1 123.39(12) . . ? C22 N2 Pd1 118.76(12) . . ? C10 C1 C2 118.74(16) . . ? C10 C1 Pd1 123.96(13) . . ? C2 C1 Pd1 117.28(12) . . ? C7 C2 C1 120.21(16) . . ? C7 C2 C3 121.85(16) . . ? C1 C2 C3 117.92(15) . . ? C14 C3 C4 120.13(16) . . ? C14 C3 C2 119.97(16) . . ? C4 C3 C2 119.86(16) . . ? C11 C4 C3 117.74(17) . . ? C11 C4 C5 120.64(16) . . ? C3 C4 C5 121.34(15) . . ? C4 C5 C6 120.27(14) . . ? N1 C6 C16 107.65(14) . . ? N1 C6 C15 107.37(14) . . ? C16 C6 C15 109.79(15) . . ? N1 C6 C5 111.46(13) . . ? C16 C6 C5 112.87(15) . . ? C15 C6 C5 107.58(14) . . ? C8 C7 C2 120.49(16) . . ? C7 C8 C9 119.69(17) . . ? C8 C9 C10 120.05(17) . . ? C9 C10 C1 120.74(16) . . ? C12 C11 C4 121.57(18) . . ? C13 C12 C11 120.18(17) . . ? C12 C13 C14 119.32(18) . . ? C13 C14 C3 120.98(18) . . ? N2 C22 C23 122.54(17) . . ? C22 C23 C24 120.29(17) . . ? C23 C24 C25 116.72(16) . . ? C23 C24 C27 121.98(18) . . ? C25 C24 C27 121.27(18) . . ? C26 C25 C24 120.05(17) . . ? N2 C26 C25 122.64(17) . . ? 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 C1 Pd1 N1 C6 -88.69(13) . . . . ? N2 Pd1 N1 C6 -101.3(15) . . . . ? Cl1 Pd1 N1 C6 91.21(12) . . . . ? C1 Pd1 N2 C26 -56.73(14) . . . . ? N1 Pd1 N2 C26 -44.1(15) . . . . ? Cl1 Pd1 N2 C26 123.37(13) . . . . ? C1 Pd1 N2 C22 130.17(14) . . . . ? N1 Pd1 N2 C22 142.8(14) . . . . ? Cl1 Pd1 N2 C22 -49.73(13) . . . . ? N2 Pd1 C1 C10 97.82(15) . . . . ? N1 Pd1 C1 C10 -81.70(15) . . . . ? Cl1 Pd1 C1 C10 -90(4) . . . . ? N2 Pd1 C1 C2 -83.83(13) . . . . ? N1 Pd1 C1 C2 96.65(13) . . . . ? Cl1 Pd1 C1 C2 89(4) . . . . ? C10 C1 C2 C7 -2.4(2) . . . . ? Pd1 C1 C2 C7 179.16(13) . . . . ? C10 C1 C2 C3 176.10(16) . . . . ? Pd1 C1 C2 C3 -2.3(2) . . . . ? C7 C2 C3 C14 -71.5(2) . . . . ? C1 C2 C3 C14 110.03(19) . . . . ? C7 C2 C3 C4 111.0(2) . . . . ? C1 C2 C3 C4 -67.5(2) . . . . ? C14 C3 C4 C11 -1.0(2) . . . . ? C2 C3 C4 C11 176.45(16) . . . . ? C14 C3 C4 C5 172.92(15) . . . . ? C2 C3 C4 C5 -9.6(2) . . . . ? C11 C4 C5 C6 -79.1(2) . . . . ? C3 C4 C5 C6 107.08(19) . . . . ? Pd1 N1 C6 C16 -76.03(16) . . . . ? Pd1 N1 C6 C15 165.82(11) . . . . ? Pd1 N1 C6 C5 48.25(17) . . . . ? C4 C5 C6 N1 -68.0(2) . . . . ? C4 C5 C6 C16 53.3(2) . . . . ? C4 C5 C6 C15 174.53(15) . . . . ? C1 C2 C7 C8 2.8(3) . . . . ? C3 C2 C7 C8 -175.63(17) . . . . ? C2 C7 C8 C9 -0.8(3) . . . . ? C7 C8 C9 C10 -1.5(3) . . . . ? C8 C9 C10 C1 1.9(3) . . . . ? C2 C1 C10 C9 0.1(3) . . . . ? Pd1 C1 C10 C9 178.39(13) . . . . ? C3 C4 C11 C12 -1.6(3) . . . . ? C5 C4 C11 C12 -175.62(16) . . . . ? C4 C11 C12 C13 2.6(3) . . . . ? C11 C12 C13 C14 -0.8(3) . . . . ? C12 C13 C14 C3 -1.8(3) . . . . ? C4 C3 C14 C13 2.8(3) . . . . ? C2 C3 C14 C13 -174.69(16) . . . . ? C26 N2 C22 C23 -3.7(3) . . . . ? Pd1 N2 C22 C23 169.77(14) . . . . ? N2 C22 C23 C24 -0.7(3) . . . . ? C22 C23 C24 C25 4.4(3) . . . . ? C22 C23 C24 C27 -173.41(18) . . . . ? C23 C24 C25 C26 -3.7(3) . . . . ? C27 C24 C25 C26 174.11(17) . . . . ? C22 N2 C26 C25 4.4(3) . . . . ? Pd1 N2 C26 C25 -168.73(13) . . . . ? C24 C25 C26 N2 -0.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H01A Cl1 0.841(17) 2.581(17) 3.4112(16) 169.5(19) 2_657 _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.506 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.071 #===END data_joe6912s _database_code_depnum_ccdc_archive 'CCDC 874141' #TrackingRef '- jaj561s_joe6912.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H35 Br Cl2 N O2 P Pd' _chemical_formula_weight 789.82 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8675(7) _cell_length_b 13.5117(11) _cell_length_c 15.0521(12) _cell_angle_alpha 68.116(2) _cell_angle_beta 79.424(2) _cell_angle_gamma 75.791(2) _cell_volume 1613.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5425 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.56 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 2.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8292 _exptl_absorpt_correction_T_max 0.9407 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19839 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.71 _reflns_number_total 7568 _reflns_number_gt 7000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. NH2 free with SADI, rigid methyls, others riding ; _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^)+(0.0360P)^2^+1.8269P] 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 'NH2 free with SADI, rigid methyls others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7568 _refine_ls_number_parameters 398 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Pd1 Pd 0.707650(18) 0.338615(13) 0.119257(11) 0.01212(5) Uani 1 1 d . . . N1 N 0.8342(2) 0.37818(16) -0.01976(14) 0.0148(4) Uani 1 1 d D . . H01A H 0.861(3) 0.434(2) -0.025(2) 0.020(7) Uiso 1 1 d D . . H01B H 0.770(3) 0.392(2) -0.0576(19) 0.020(7) Uiso 1 1 d D . . P1 P 0.54363(6) 0.30636(4) 0.25737(4) 0.01334(11) Uani 1 1 d . . . Br1 Br 0.89490(3) 0.425895(19) 0.162650(17) 0.01983(6) Uani 1 1 d . . . C1 C 0.5754(2) 0.27490(18) 0.06967(15) 0.0146(4) Uani 1 1 d . . . C2 C 0.6157(2) 0.16502(18) 0.07791(15) 0.0147(4) Uani 1 1 d . . . C3 C 0.7620(2) 0.09466(17) 0.11995(15) 0.0136(4) Uani 1 1 d . . . C4 C 0.9071(2) 0.10932(17) 0.06804(15) 0.0140(4) Uani 1 1 d . . . C5 C 0.9266(3) 0.19203(18) -0.03213(15) 0.0149(4) Uani 1 1 d . . . H5A H 0.8273 0.2115 -0.0613 0.018 Uiso 1 1 calc R . . H5B H 1.0080 0.1572 -0.0716 0.018 Uiso 1 1 calc R . . C6 C 0.9712(3) 0.29682(18) -0.03783(16) 0.0163(4) Uani 1 1 d . . . H6A H 1.0457 0.2789 0.0100 0.020 Uiso 1 1 calc R . . H6B H 1.0250 0.3292 -0.1025 0.020 Uiso 1 1 calc R . . C7 C 0.5225(3) 0.12264(19) 0.04104(16) 0.0173(4) Uani 1 1 d . . . H7 H 0.5464 0.0474 0.0493 0.021 Uiso 1 1 calc R . . C8 C 0.3950(3) 0.1894(2) -0.00767(17) 0.0197(5) Uani 1 1 d . . . H8 H 0.3326 0.1599 -0.0326 0.024 Uiso 1 1 calc R . . C9 C 0.3596(3) 0.2992(2) -0.01961(16) 0.0188(5) Uani 1 1 d . . . H9 H 0.2748 0.3455 -0.0546 0.023 Uiso 1 1 calc R . . C10 C 0.4481(3) 0.34147(19) 0.01952(16) 0.0167(4) Uani 1 1 d . . . H10 H 0.4219 0.4164 0.0122 0.020 Uiso 1 1 calc R . . C11 C 1.0424(3) 0.04108(18) 0.10834(16) 0.0156(4) Uani 1 1 d . . . H11 H 1.1415 0.0509 0.0734 0.019 Uiso 1 1 calc R . . C12 C 1.0358(3) -0.03978(17) 0.19713(16) 0.0147(4) Uani 1 1 d . . . C13 C 0.8890(3) -0.05529(18) 0.24932(16) 0.0158(4) Uani 1 1 d . . . C14 C 0.7545(3) 0.01122(18) 0.21053(16) 0.0160(4) Uani 1 1 d . . . H14 H 0.6555 0.0006 0.2453 0.019 Uiso 1 1 calc R . . C15 C 1.3127(3) -0.0920(2) 0.19242(17) 0.0204(5) Uani 1 1 d . . . H15A H 1.3269 -0.1045 0.1311 0.031 Uiso 1 1 calc R . . H15B H 1.3938 -0.1422 0.2328 0.031 Uiso 1 1 calc R . . H15C H 1.3208 -0.0169 0.1803 0.031 Uiso 1 1 calc R . . O1 O 1.16238(18) -0.11002(13) 0.24047(11) 0.0178(3) Uani 1 1 d . . . C16 C 0.7544(3) -0.1492(2) 0.39807(18) 0.0263(5) Uani 1 1 d . . . H16A H 0.7133 -0.0824 0.4133 0.040 Uiso 1 1 calc R . . H16B H 0.7750 -0.2108 0.4576 0.040 Uiso 1 1 calc R . . H16C H 0.6775 -0.1615 0.3661 0.040 Uiso 1 1 calc R . . O2 O 0.89550(19) -0.13865(14) 0.33608(12) 0.0217(4) Uani 1 1 d . . . C21 C 0.4196(3) 0.20610(18) 0.28943(15) 0.0148(4) Uani 1 1 d . . . C22 C 0.4471(3) 0.10754(19) 0.36525(16) 0.0186(4) Uani 1 1 d . . . H22 H 0.5329 0.0912 0.4013 0.022 Uiso 1 1 calc R . . C23 C 0.3499(3) 0.0331(2) 0.38838(18) 0.0225(5) Uani 1 1 d . . . H23 H 0.3700 -0.0339 0.4400 0.027 Uiso 1 1 calc R . . C24 C 0.2237(3) 0.0561(2) 0.33672(17) 0.0217(5) Uani 1 1 d . . . H24 H 0.1570 0.0052 0.3531 0.026 Uiso 1 1 calc R . . C25 C 0.1953(3) 0.1537(2) 0.26092(17) 0.0195(5) Uani 1 1 d . . . H25 H 0.1092 0.1695 0.2251 0.023 Uiso 1 1 calc R . . C26 C 0.2923(3) 0.22810(19) 0.23735(16) 0.0178(4) Uani 1 1 d . . . H26 H 0.2722 0.2947 0.1853 0.021 Uiso 1 1 calc R . . C31 C 0.4019(3) 0.42960(18) 0.25856(16) 0.0153(4) Uani 1 1 d . . . C32 C 0.2497(3) 0.42888(19) 0.30466(17) 0.0210(5) Uani 1 1 d . . . H32 H 0.2132 0.3623 0.3336 0.025 Uiso 1 1 calc R . . C33 C 0.1516(3) 0.5252(2) 0.30833(18) 0.0229(5) Uani 1 1 d . . . H33 H 0.0486 0.5239 0.3399 0.027 Uiso 1 1 calc R . . C34 C 0.2031(3) 0.6229(2) 0.26635(17) 0.0221(5) Uani 1 1 d . . . H34 H 0.1362 0.6884 0.2697 0.027 Uiso 1 1 calc R . . C35 C 0.3533(3) 0.6245(2) 0.21929(18) 0.0223(5) Uani 1 1 d . . . H35 H 0.3887 0.6914 0.1897 0.027 Uiso 1 1 calc R . . C36 C 0.4516(3) 0.52856(19) 0.21546(16) 0.0181(4) Uani 1 1 d . . . H36 H 0.5540 0.5304 0.1831 0.022 Uiso 1 1 calc R . . C41 C 0.6408(3) 0.26870(18) 0.36532(16) 0.0158(4) Uani 1 1 d . . . C42 C 0.5641(3) 0.29557(19) 0.44534(17) 0.0200(5) Uani 1 1 d . . . H42 H 0.4572 0.3305 0.4453 0.024 Uiso 1 1 calc R . . C43 C 0.6422(3) 0.2718(2) 0.52481(17) 0.0227(5) Uani 1 1 d . . . H43 H 0.5890 0.2909 0.5787 0.027 Uiso 1 1 calc R . . C44 C 0.7978(3) 0.2203(2) 0.52575(17) 0.0235(5) Uani 1 1 d . . . H44 H 0.8522 0.2056 0.5795 0.028 Uiso 1 1 calc R . . C45 C 0.8738(3) 0.1903(2) 0.44796(18) 0.0258(5) Uani 1 1 d . . . H45 H 0.9796 0.1530 0.4493 0.031 Uiso 1 1 calc R . . C46 C 0.7958(3) 0.2147(2) 0.36777(17) 0.0217(5) Uani 1 1 d . . . H46 H 0.8489 0.1942 0.3145 0.026 Uiso 1 1 calc R . . C99 C 0.7011(4) 0.5427(2) 0.3561(2) 0.0330(6) Uani 1 1 d . . . H99A H 0.5913 0.5331 0.3663 0.040 Uiso 1 1 calc R . . H99B H 0.7664 0.4868 0.3302 0.040 Uiso 1 1 calc R . . Cl1 Cl 0.71539(8) 0.67352(6) 0.27151(5) 0.03491(15) Uani 1 1 d . . . Cl2 Cl 0.76285(8) 0.52402(6) 0.46750(5) 0.03292(15) 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 Pd1 0.01203(8) 0.01243(8) 0.01161(8) -0.00359(6) -0.00063(6) -0.00317(6) N1 0.0154(9) 0.0141(9) 0.0141(9) -0.0032(7) -0.0022(7) -0.0035(7) P1 0.0134(2) 0.0128(3) 0.0122(3) -0.0032(2) -0.0008(2) -0.0018(2) Br1 0.02024(12) 0.02098(12) 0.01980(12) -0.00687(9) -0.00272(9) -0.00647(9) C1 0.0149(10) 0.0168(10) 0.0110(10) -0.0037(8) 0.0013(8) -0.0047(8) C2 0.0129(10) 0.0190(11) 0.0117(10) -0.0047(8) 0.0013(8) -0.0053(8) C3 0.0159(10) 0.0133(10) 0.0128(10) -0.0051(8) -0.0016(8) -0.0039(8) C4 0.0163(10) 0.0133(10) 0.0122(10) -0.0042(8) -0.0004(8) -0.0033(8) C5 0.0154(10) 0.0158(10) 0.0117(10) -0.0028(8) -0.0004(8) -0.0036(8) C6 0.0143(10) 0.0173(11) 0.0155(10) -0.0036(8) 0.0003(8) -0.0044(8) C7 0.0187(11) 0.0166(11) 0.0170(11) -0.0054(9) 0.0022(8) -0.0073(9) C8 0.0166(11) 0.0284(12) 0.0172(11) -0.0070(10) -0.0011(8) -0.0119(9) C9 0.0120(10) 0.0240(12) 0.0166(11) -0.0020(9) -0.0013(8) -0.0047(9) C10 0.0151(10) 0.0172(10) 0.0150(10) -0.0029(8) 0.0003(8) -0.0036(8) C11 0.0158(10) 0.0163(10) 0.0150(10) -0.0055(8) 0.0004(8) -0.0051(8) C12 0.0159(10) 0.0137(10) 0.0153(10) -0.0061(8) -0.0024(8) -0.0021(8) C13 0.0207(11) 0.0133(10) 0.0126(10) -0.0028(8) -0.0009(8) -0.0050(8) C14 0.0161(10) 0.0163(10) 0.0159(11) -0.0054(9) 0.0004(8) -0.0053(8) C15 0.0162(11) 0.0211(11) 0.0210(12) -0.0061(9) -0.0003(9) -0.0012(9) O1 0.0145(7) 0.0168(8) 0.0173(8) -0.0018(6) -0.0017(6) -0.0009(6) C16 0.0269(13) 0.0261(13) 0.0163(12) 0.0015(10) 0.0038(10) -0.0063(10) O2 0.0202(8) 0.0194(8) 0.0165(8) 0.0031(7) -0.0001(6) -0.0038(7) C21 0.0159(10) 0.0142(10) 0.0135(10) -0.0050(8) 0.0022(8) -0.0039(8) C22 0.0218(11) 0.0175(11) 0.0156(11) -0.0052(9) -0.0024(9) -0.0027(9) C23 0.0302(13) 0.0167(11) 0.0198(12) -0.0040(9) -0.0009(10) -0.0079(10) C24 0.0259(12) 0.0199(11) 0.0200(12) -0.0076(9) 0.0045(9) -0.0097(10) C25 0.0167(11) 0.0227(12) 0.0199(11) -0.0086(9) 0.0015(9) -0.0058(9) C26 0.0166(10) 0.0187(11) 0.0158(11) -0.0046(9) 0.0011(8) -0.0035(9) C31 0.0171(10) 0.0151(10) 0.0128(10) -0.0039(8) -0.0037(8) -0.0012(8) C32 0.0195(11) 0.0180(11) 0.0222(12) -0.0051(9) 0.0019(9) -0.0040(9) C33 0.0173(11) 0.0257(12) 0.0245(12) -0.0104(10) 0.0015(9) -0.0020(9) C34 0.0232(12) 0.0200(11) 0.0210(12) -0.0078(9) -0.0068(9) 0.0042(9) C35 0.0255(12) 0.0160(11) 0.0236(12) -0.0045(9) -0.0050(10) -0.0028(9) C36 0.0174(10) 0.0176(11) 0.0170(11) -0.0038(9) -0.0027(8) -0.0023(9) C41 0.0189(10) 0.0137(10) 0.0127(10) -0.0008(8) -0.0021(8) -0.0049(8) C42 0.0214(11) 0.0198(11) 0.0162(11) -0.0053(9) -0.0020(9) -0.0006(9) C43 0.0310(13) 0.0224(12) 0.0148(11) -0.0061(9) -0.0019(9) -0.0059(10) C44 0.0298(13) 0.0231(12) 0.0169(11) 0.0002(9) -0.0083(10) -0.0108(10) C45 0.0202(12) 0.0295(13) 0.0218(12) -0.0012(10) -0.0060(9) -0.0034(10) C46 0.0193(11) 0.0232(12) 0.0178(11) -0.0039(9) -0.0001(9) -0.0016(9) C99 0.0352(15) 0.0381(16) 0.0309(15) -0.0164(13) -0.0066(12) -0.0066(12) Cl1 0.0355(4) 0.0403(4) 0.0293(3) -0.0138(3) -0.0014(3) -0.0064(3) Cl2 0.0342(3) 0.0411(4) 0.0271(3) -0.0179(3) -0.0028(3) -0.0043(3) _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 C1 1.992(2) . ? Pd1 N1 2.1267(19) . ? Pd1 P1 2.2701(6) . ? Pd1 Br1 2.5511(3) . ? N1 C6 1.485(3) . ? P1 C41 1.823(2) . ? P1 C21 1.824(2) . ? P1 C31 1.827(2) . ? C1 C10 1.401(3) . ? C1 C2 1.402(3) . ? C2 C7 1.399(3) . ? C2 C3 1.495(3) . ? C3 C4 1.395(3) . ? C3 C14 1.411(3) . ? C4 C11 1.402(3) . ? C4 C5 1.515(3) . ? C5 C6 1.530(3) . ? C7 C8 1.393(3) . ? C8 C9 1.388(3) . ? C9 C10 1.389(3) . ? C11 C12 1.377(3) . ? C12 O1 1.368(3) . ? C12 C13 1.411(3) . ? C13 O2 1.370(3) . ? C13 C14 1.382(3) . ? C15 O1 1.426(3) . ? C16 O2 1.420(3) . ? C21 C22 1.395(3) . ? C21 C26 1.401(3) . ? C22 C23 1.389(3) . ? C23 C24 1.387(4) . ? C24 C25 1.387(3) . ? C25 C26 1.387(3) . ? C31 C36 1.393(3) . ? C31 C32 1.400(3) . ? C32 C33 1.390(3) . ? C33 C34 1.386(4) . ? C34 C35 1.390(3) . ? C35 C36 1.388(3) . ? C41 C46 1.389(3) . ? C41 C42 1.396(3) . ? C42 C43 1.387(3) . ? C43 C44 1.384(4) . ? C44 C45 1.385(4) . ? C45 C46 1.393(3) . ? C99 Cl2 1.769(3) . ? C99 Cl1 1.770(3) . ? 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 C1 Pd1 N1 87.11(8) . . ? C1 Pd1 P1 87.88(6) . . ? N1 Pd1 P1 172.43(5) . . ? C1 Pd1 Br1 173.12(6) . . ? N1 Pd1 Br1 86.01(5) . . ? P1 Pd1 Br1 98.970(17) . . ? C6 N1 Pd1 118.00(14) . . ? C41 P1 C21 103.70(10) . . ? C41 P1 C31 103.17(10) . . ? C21 P1 C31 102.48(10) . . ? C41 P1 Pd1 113.83(7) . . ? C21 P1 Pd1 120.77(7) . . ? C31 P1 Pd1 110.94(7) . . ? C10 C1 C2 119.2(2) . . ? C10 C1 Pd1 120.16(17) . . ? C2 C1 Pd1 120.46(16) . . ? C7 C2 C1 119.4(2) . . ? C7 C2 C3 119.7(2) . . ? C1 C2 C3 120.84(19) . . ? C4 C3 C14 119.6(2) . . ? C4 C3 C2 119.78(19) . . ? C14 C3 C2 120.55(19) . . ? C3 C4 C11 118.7(2) . . ? C3 C4 C5 123.50(19) . . ? C11 C4 C5 117.76(19) . . ? C4 C5 C6 115.70(18) . . ? N1 C6 C5 112.91(18) . . ? C8 C7 C2 120.8(2) . . ? C9 C8 C7 119.7(2) . . ? C8 C9 C10 120.0(2) . . ? C9 C10 C1 120.8(2) . . ? C12 C11 C4 121.9(2) . . ? O1 C12 C11 125.2(2) . . ? O1 C12 C13 115.38(19) . . ? C11 C12 C13 119.4(2) . . ? O2 C13 C14 125.9(2) . . ? O2 C13 C12 114.71(19) . . ? C14 C13 C12 119.4(2) . . ? C13 C14 C3 121.0(2) . . ? C12 O1 C15 116.68(17) . . ? C13 O2 C16 117.54(18) . . ? C22 C21 C26 118.6(2) . . ? C22 C21 P1 121.79(17) . . ? C26 C21 P1 119.62(17) . . ? C23 C22 C21 120.5(2) . . ? C24 C23 C22 120.5(2) . . ? C23 C24 C25 119.7(2) . . ? C26 C25 C24 120.1(2) . . ? C25 C26 C21 120.7(2) . . ? C36 C31 C32 118.7(2) . . ? C36 C31 P1 117.76(17) . . ? C32 C31 P1 123.44(17) . . ? C33 C32 C31 120.3(2) . . ? C34 C33 C32 120.5(2) . . ? C33 C34 C35 119.5(2) . . ? C36 C35 C34 120.2(2) . . ? C35 C36 C31 120.8(2) . . ? C46 C41 C42 118.8(2) . . ? C46 C41 P1 119.74(18) . . ? C42 C41 P1 121.41(17) . . ? C43 C42 C41 120.7(2) . . ? C44 C43 C42 120.1(2) . . ? C43 C44 C45 119.7(2) . . ? C44 C45 C46 120.4(2) . . ? C41 C46 C45 120.3(2) . . ? Cl2 C99 Cl1 111.48(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C99 H99B Br1 0.99 2.89 3.766(3) 147.6 . C44 H44 O1 0.95 2.52 3.319(3) 141.2 2_756 C44 H44 O2 0.95 2.58 3.440(3) 151.4 2_756 _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.767 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.089 #===END