Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_palla _database_code_CSD 145279 _journal_coden_Cambridge 182 _journal_volume ? _journal_year 2000 _journal_page_first 1869 loop_ _publ_author_name 'Brunel, Jean Michel' 'Hirlemann, M.H.' 'Heumann, A.' 'Buono, Gerard' _publ_contact_author_name 'Dr Brunel Jean Michel' _publ_contact_author_address ; ENSSPICAM UMR 6516 CNRS Laboratoire de Synthese Asymetrique, 1er etage Av. escadrille normandie niemen 13397 Marseille cedex 20 FRANCE ; _publ_contact_author_email 'brunel@spi-chim.u-3mrs.fr' _publ_section_title ; Crystal and molecular structure of Compound X ; _publ_section_abstract ; We present the crystal and molecular structure of Compound X . ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All Diagrams and calculations were performed using maXus (MacScience, Japan). ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description '' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.5 _chemical_formula_sum 'C26 H28 I N2 O2 P1 Pd' _chemical_formula_weight 664.81 _cell_length_a 9.1514(2) _cell_length_b 10.8405(4) _cell_length_c 15.8227(6) _cell_angle_alpha 90.00(1) _cell_angle_beta 101.97(1) _cell_angle_gamma 90.00(1) _cell_volume 805.5(2) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '1' _cell_measurement_theta_max '??' _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.22 _exptl_crystal_density_meas 1.25 _exptl_absorpt_coefficient_mu 1.66 _cell_measurement_temperature '298' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 1688 _reflns_number_total 1685 _reflns_number_observed 1596 _reflns_observed_criterion 'refl_observed_if_I_>_3.00_sigma(I)' _diffrn_reflns_theta_max 25.45 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.045 _refine_ls_wR_factor_obs 0.082 _refine_ls_hydrogen_treatment 'refxyz' _refine_ls_number_reflns 1596 _refine_ls_number_parameters 189 _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_weighting_scheme 'Count statistics' _refine_ls_shift/esd_max 0.1272 _refine_ls_shift/esd_mean 0.0195 _refine_diff_density_min -0.29 _refine_diff_density_max 0.14 _refine_ls_extinction_method 'None' _atom_type_scat_source 'D.Waasmaier&A.Kirfel,Acta Cryst.1995,A51, 416-431' _computing_data_reduction 'maXus' _computing_molecular_graphics 'maXus' _computing_publication_material 'maXus' _computing_structure_refinement 'maXus' _computing_structure_solution 'maXus' _diffrn_measurement_device 'KappaCCD' _computing_data_collection 'KappaCCD' _diffrn_radiation_type 'xray' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_radiation_wavelength 0.71073 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.25 _chemical_formula_weight 664.81 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X+0.5,-Y,+Z+0.5 +X+0.5,-Y+0.5,-Z -X,+Y+0.5,-Z+0.5 _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_cell_setting 'Orthorhombic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type P1 3.796(2) 2.086(2) 9.395(2) 0.0492(1) 1.00 Uij N3 2.675(1) 2.530(1) 10.536(6) 0.0522(4) 1.00 Uij N4 4.305(9) 0.726(1) 10.209(6) 0.0569(4) 1.00 Uij C5 5.460(1) -0.002(1) 9.862(7) 0.0457(4) 1.00 Uij C6 5.154(9) 3.259(1) 9.425(6) 0.0498(4) 1.00 Uij C7 5.749(1) 3.639(1) 8.230(8) 0.0611(5) 1.00 Uij C8 2.433(1) 1.436(1) 11.497(7) 0.0521(4) 1.00 Uij C2 5.617(1) 3.805(1) 10.616(8) 0.0588(5) 1.00 Uij C10 6.779(1) 4.578(1) 8.236(7) 0.0565(4) 1.00 Uij C11 3.724(2) 0.662(2) 11.547(8) 0.0887(8) 1.00 Uij C12 6.153(1) -0.744(1) 10.810(9) 0.0621(5) 1.00 Uij C13 5.918(1) -0.020(2) 8.543(1) 0.0785(6) 1.00 Uij C14 1.329(1) 2.986(2) 10.045(1) 0.0687(5) 1.00 Uij C15 7.239(2) 5.086(2) 9.431(8) 0.0754(7) 1.00 Uij C16 6.665(1) 4.706(2) 10.616(9) 0.0699(6) 1.00 Uij C17 7.323(1) -1.437(2) 10.426(1) 0.0782(7) 1.00 Uij C18 7.035(2) -0.707(1) 8.206(8) 0.0673(5) 1.00 Uij C19 7.753(1) -1.425(2) 9.151(1) 0.0843(7) 1.00 Uij C20 1.214(2) 0.750(2) 11.006(1) 0.0870(8) 1.00 Uij C21 0.360(2) 1.902(2) 10.422(1) 0.0956(8) 1.00 Uij Pd0 3.952(2) 1.539(2) 7.145(2) 0.1344(1) 1.00 Uij C46 5.707(2) 2.849(2) 7.210(2) 0.0521(4) 1.00 Uij C49 3.643(2) 0.619(2) 6.408(2) 0.0635(5) 1.00 Uij C51 4.682(2) 0.028(2) 5.438(2) 0.0542(4) 1.00 Uij C52 4.293(2) -1.134(2) 4.506(2) 0.0129(2) 1.00 Uij C53 2.863(2) -1.705(2) 4.544(2) 0.0487(3) 1.00 Uij C54 1.823(2) -1.114(2) 5.513(2) 0.0254(6) 1.00 Uij C55 2.213(2) 0.048(2) 6.446(2) 0.0254(5) 1.00 Uij O56 2.860(2) 3.394(2) 6.823(2) 0.0554(2) 1.00 Uij C64 1.692(2) 3.599(2) 7.036(2) 0.0589(4) 1.00 Uij O65 0.941(2) 4.879(2) 6.813(2) 0.0780(4) 1.00 Uij C68 1.204(2) 2.721(2) 7.763(2) 0.0547(3) 1.00 Uij I69 5.461(2) 1.793(2) 3.492(2) 0.0498(4) 1.00 Uij loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 P1 0.0412(1) 0.0589(1) 0.0460(1) -.0038(1) 0.01150(7) 0.0006(1) N3 0.0555(4) 0.0508(4) 0.0501(4) -.0025(3) 0.0205(3) -.0039(3) N4 0.0477(4) 0.0640(5) 0.0585(4) 0.0148(3) 0.0195(3) 0.0144(3) C5 0.0469(4) 0.0393(4) 0.0492(4) -.0036(3) 0.0121(3) 0.0006(3) C6 0.0419(4) 0.0581(5) 0.0488(4) 0.0138(4) 0.0160(3) 0.0077(4) C7 0.0686(6) 0.0487(5) 0.0649(6) -.0023(4) 0.0222(4) -.0074(4) C8 0.0609(5) 0.0423(4) 0.0520(5) -.0006(4) 0.0177(4) 0.0014(3) C2 0.0525(5) 0.0649(6) 0.0568(5) 0.0059(4) 0.0129(4) 0.0086(4) C10 0.0504(5) 0.0590(5) 0.0568(5) 0.0087(4) 0.0065(4) -.0042(4) C11 0.1150(9) 0.098(1) 0.0541(5) 0.0450(8) 0.0376(6) 0.0148(6) C12 0.0623(6) 0.0475(5) 0.0773(6) 0.0044(4) 0.0323(5) 0.0069(4) C13 0.0594(6) 0.0680(8) 0.1072(9) 0.0174(5) 0.0303(6) -.0014(6) C14 0.0481(5) 0.0683(7) 0.0846(7) 0.0134(4) 0.0037(5) -.0004(5) C15 0.0878(8) 0.0848(8) 0.0499(5) -.0016(6) 0.0119(5) -.0118(5) C16 0.0784(7) 0.0613(6) 0.0716(6) 0.0062(5) 0.0382(5) -.0047(5) C17 0.0700(7) 0.0702(7) 0.0929(8) 0.0058(5) 0.0267(6) 0.0249(6) C18 0.0817(7) 0.0662(7) 0.0526(5) 0.0168(5) 0.0210(5) 0.0006(4) C19 0.0649(7) 0.103(1) 0.0837(8) 0.0409(6) 0.0243(6) 0.0179(7) C21 0.0945(8) 0.092(1) 0.0767(8) 0.0309(7) 0.0462(6) 0.0349(7) Pd0 0.122(1) 0.0532(7) 0.1137(9) 0.0160(7) 0.0569(8) 0.0187(7) C46 0.112(1) 0.114(2) 0.176(2) 0.066(1) 0.061(1) 0.060(1) C49 0.0623(6) 0.0475(5) 0.0773(6) 0.0044(4) 0.0323(5) 0.0069(4) C51 0.0594(6) 0.0680(8) 0.1072(9) 0.0174(5) 0.0303(6) -.0014(6) C52 0.0481(5) 0.0683(7) 0.0846(7) 0.0134(4) 0.0037(5) -.0004(5) C53 0.0878(8) 0.0848(8) 0.0499(5) -.0016(6) 0.0119(5) -.0118(5) C54 0.0784(7) 0.0613(6) 0.0716(6) 0.0062(5) 0.0382(5) -.0047(5) C55 0.0700(7) 0.0702(7) 0.0929(8) 0.0058(5) 0.0267(6) 0.0249(6) O56 0.0817(7) 0.0662(7) 0.0526(5) 0.0168(5) 0.0210(5) 0.0006(4) C64 0.0649(7) 0.103(1) 0.0837(8) 0.0409(6) 0.0243(6) 0.0179(7) O65 0.0945(8) 0.092(1) 0.0767(8) 0.0309(7) 0.0462(6) 0.0349(7) C68 0.122(1) 0.0532(7) 0.1137(9) 0.0160(7) 0.0569(8) 0.0187(7) I69 0.112(1) 0.114(2) 0.176(2) 0.066(1) 0.061(1) 0.060(1) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd0 O56 2.181(1) . . ? Pd0 C49 1.221(2) . . ? Pd0 C46 2.193(2) . . ? P1 N3 1.661(1) . . ? P1 N4 1.660(1) . . ? P1 Pd0 2.321(2) . . ? P1 C6 1.794(1) . . ? C2 C6 1.394(2) . . ? C2 C16 1.386(2) . . ? N3 C14 1.502(2) . . ? N3 C8 1.481(2) . . ? N4 C11 1.462(2) . . ? N4 C5 1.412(2) . . ? C5 C13 1.401(2) . . ? C5 C12 1.393(2) . . ? C6 C7 1.397(2) . . ? C7 C10 1.391(2) . . ? C7 C46 1.292(2) . . ? C8 C11 1.514(2) . . ? C8 C20 1.481(2) . . ? C10 C15 1.383(2) . . ? C12 C17 1.412(2) . . ? C13 C18 1.356(2) . . ? C14 C21 1.504(2) . . ? C15 C16 1.376(2) . . ? C17 C19 1.359(2) . . ? C18 C19 1.398(2) . . ? C20 C21 1.583(2) . . ? C49 C51 1.540(2) . . ? C49 C55 1.541(2) . . ? C51 C52 1.538(1) . . ? C53 C54 1.539(2) . . ? C54 C55 1.542(2) . . ? O56 C64 1.213(2) . . ? C64 O65 1.504(2) . . ? O65 C68 1.247(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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd0 P1 N3 140.8(2) . . . ? Pd0 P1 C6 96.9(2) . . ? Pd0 C49 C51 120.0(2) . . . ? Pd0 P1 N4 105.1(2) . . . ? P1 N4 C5 123.5(2) . . . ? P1 N4 C11 111.3(2) . . . ? P1 N3 C14 117.5(2) . . . ? P1 N3 C8 111.1(2) . . . ? P1 C6 C2 121.6(2) . . . ? P1 C6 C7 119.3(2) . . . ? C2 C16 C15 119.9(2) . . . ? N3 P1 N4 95.1(2) . .. ? N3 P1 C6 108.9(2) . .. ? N3 C14 C21 106.1(2) . . . ? N3 C8 C11 105.2(2) . . . ? N4 C5 C12 121.1(2) . . . ? N4 P1 C6 107.1(2) . . . ? C5 C12 C17 119.3(2) . . . ? C6 C2 C16 120.6(2) . . . ? C6 C7 C46 119.9(2) . . . ? C7 C46 Pd0 114.5(2) . . . ? C8 C11 N4 106.7(2) . . . ? C10 C7 C6 119.8(2) . . . ? C10 C7 C46 116.1(2) . . . ? C11 N4 C5 122.0(2) . . . ? C12 C17 C19 121.1(2) . . . ? C13 C5 C12 118.3(2) . . . ? C13 C5 N4 120.6(2) . . . ? C14 N3 C8 106.9(2) . . . ? C14 C21 C20 106.5(2) . . . ? C15 C10 C7 119.9(2) . . . ? C16 C15 C10 120.5(2) . . . ? C17 C19 C18 119.0(2) . . . ? C18 C13 C5 120.8(2) . . . ? C19 C18 C13 121.4(2) . . . ? C20 C8 N3 105.2(2) . . . ? C20 C8 C11 118.5(2) . . . ? C21 C20 C8 103.5(2) . . . ? C46 Pd0 P1 83.3(2) . . . ? C46 Pd0 C49 132.2(2) . . . ? C46 Pd0 O56 84.0(2) . . . ? C49 C51 C52 121.2(2) . . . ? C49 Pd0 P1 138.4(2) . . . ? C51 C52 C53 119.6(2) . . . ? C52 C53 C54 119.1(2) . . . ? C53 C54 C55 119.4(2) . . . ? C54 C55 C49 121.2(2) . . . ? C55 C49 Pd0 119.8(2) . . . ? O56 Pd0 P1 84.8(2) . . ? O56 Pd0 C49 115.2(2) . . . ? C64 O56 Pd0 127.3(2) . . . ? O65 C64 O56 127.2(2) . . . ? C68 C64 O65 119.6(2) . . . ? C68 C64 O56 111.3(2) . . . ? #===================================================