Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'ProfD Alessia Bacchi' _publ_contact_author_address ; Parma ITALY ; _publ_contact_author_email ALESSIA.BACCHI@UNIPR.IT _publ_section_title ; Engineering of Organic/Inorganic Diols That Reversibly Capture and Release Volatile Guests ; loop_ _publ_author_name 'Alessia Bacchi' 'Elsa Bosetti' 'Mauro Carcelli' data_pdidmso _database_code_depnum_ccdc_archive 'CCDC 273903' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H42 I2 N2 O4 Pd S2' _chemical_formula_weight 1039.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' I I -0.4742 1.8119 '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' S S 0.1246 0.1234 '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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.4271(5) _cell_length_b 12.8450(10) _cell_length_c 13.1220(10) _cell_angle_alpha 87.4030(10) _cell_angle_beta 78.5920(10) _cell_angle_gamma 87.9160(10) _cell_volume 1060.39(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 2.031 _exptl_absorpt_correction_type 'symmetry-related measurements' _exptl_absorpt_correction_T_min 0.672757 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'as implemented in SAINT+/SADABS package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9911 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 24.89 _reflns_number_total 3685 _reflns_number_gt 3086 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_cell_refinement ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_data_reduction ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. SADABS: Siemens Area Detector Absorption Correction Software, Sheldrick G., 1996, University of Goettingen, Germany. ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; PARST - M. Nardelli, J. Appl. Crystallogr. 1995, 28, 659 ; _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^)+(0.0685P)^2^+2.7572P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3685 _refine_ls_number_parameters 238 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.777 _refine_ls_shift/su_mean 0.021 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 0.0000 0.0000 0.0000 0.04159(19) Uani 1 2 d S . . I1 I -0.16544(7) -0.16599(3) 0.10237(4) 0.0647(2) Uani 1 1 d . . . S1 S 0.6892(8) 0.0219(3) -0.3369(5) 0.197(2) Uani 1 1 d D . . O1 O 0.8314(6) -0.2695(4) -0.2980(4) 0.0537(10) Uani 1 1 d . . . O2 O 0.8570(13) -0.0654(5) -0.3601(6) 0.112(2) Uani 1 1 d . . . N1 N 0.2029(7) -0.0936(3) -0.0958(4) 0.0450(10) Uani 1 1 d . . . C1 C 0.6229(8) -0.3088(4) -0.2887(4) 0.0411(11) Uani 1 1 d . . . C2 C 0.4675(8) -0.2317(4) -0.2236(4) 0.0405(11) Uani 1 1 d . . . C3 C 0.5128(9) -0.2023(5) -0.1300(5) 0.0502(13) Uani 1 1 d . . . H3 H 0.6343 -0.2290 -0.1086 0.060 Uiso 1 1 calc R . . C4 C 0.3806(10) -0.1344(5) -0.0692(5) 0.0517(14) Uani 1 1 d . . . H4 H 0.4149 -0.1156 -0.0070 0.062 Uiso 1 1 calc R . . C5 C 0.1602(10) -0.1191(5) -0.1861(5) 0.0586(16) Uani 1 1 d . . . H5 H 0.0403 -0.0894 -0.2068 0.070 Uiso 1 1 calc R . . C6 C 0.2863(10) -0.1877(5) -0.2503(5) 0.0553(15) Uani 1 1 d . . . H6 H 0.2488 -0.2046 -0.3123 0.066 Uiso 1 1 calc R . . C7 C 0.6252(9) -0.4145(4) -0.2304(4) 0.0453(12) Uani 1 1 d . . . C8 C 0.4441(11) -0.4551(5) -0.1670(5) 0.0614(16) Uani 1 1 d . . . H8 H 0.3174 -0.4161 -0.1579 0.074 Uiso 1 1 calc R . . C9 C 0.4491(16) -0.5523(6) -0.1173(6) 0.079(2) Uani 1 1 d . . . H9 H 0.3257 -0.5786 -0.0765 0.095 Uiso 1 1 calc R . . C10 C 0.6342(18) -0.6095(6) -0.1281(6) 0.086(3) Uani 1 1 d . . . H10 H 0.6379 -0.6746 -0.0944 0.103 Uiso 1 1 calc R . . C11 C 0.8144(15) -0.5706(6) -0.1889(7) 0.085(2) Uani 1 1 d . . . H11 H 0.9413 -0.6093 -0.1958 0.102 Uiso 1 1 calc R . . C12 C 0.8100(12) -0.4745(5) -0.2400(6) 0.0688(18) Uani 1 1 d . . . H12 H 0.9338 -0.4497 -0.2817 0.083 Uiso 1 1 calc R . . C13 C 0.5720(9) -0.3252(4) -0.3969(4) 0.0453(12) Uani 1 1 d . . . C14 C 0.7174(12) -0.2999(7) -0.4851(5) 0.0724(19) Uani 1 1 d . . . H14 H 0.8450 -0.2710 -0.4795 0.087 Uiso 1 1 calc R . . C15 C 0.6755(17) -0.3172(8) -0.5833(6) 0.096(3) Uani 1 1 d . . . H15 H 0.7753 -0.2992 -0.6425 0.115 Uiso 1 1 calc R . . C16 C 0.4916(18) -0.3599(7) -0.5936(6) 0.086(3) Uani 1 1 d . . . H16 H 0.4656 -0.3711 -0.6594 0.104 Uiso 1 1 calc R . . C17 C 0.3444(14) -0.3865(6) -0.5071(6) 0.077(2) Uani 1 1 d . . . H17 H 0.2176 -0.4158 -0.5135 0.093 Uiso 1 1 calc R . . C18 C 0.3865(11) -0.3693(5) -0.4088(5) 0.0613(16) Uani 1 1 d . . . H18 H 0.2866 -0.3880 -0.3499 0.074 Uiso 1 1 calc R . . C19 C 0.844(3) 0.1097(17) -0.341(2) 0.38(2) Uani 1 1 d D . . H19A H 0.9870 0.0816 -0.3552 0.566 Uiso 1 1 calc R . . H19B H 0.8179 0.1427 -0.2752 0.566 Uiso 1 1 calc R . . H19C H 0.8252 0.1600 -0.3949 0.566 Uiso 1 1 calc R . . C20 C 0.657(8) 0.076(2) -0.450(3) 0.57(5) Uani 1 1 d D . . H20A H 0.6756 0.0243 -0.5017 0.854 Uiso 1 1 calc R . . H20B H 0.7592 0.1296 -0.4718 0.854 Uiso 1 1 calc R . . H20C H 0.5161 0.1070 -0.4430 0.854 Uiso 1 1 calc R . . H100 H 0.832(12) -0.206(6) -0.319(6) 0.07(2) Uiso 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 0.0505(3) 0.0329(3) 0.0420(3) -0.0087(2) -0.0108(2) 0.0090(2) I1 0.0808(3) 0.0454(3) 0.0671(3) 0.0024(2) -0.0132(2) -0.0029(2) S1 0.172(4) 0.090(2) 0.351(8) 0.032(3) -0.114(5) -0.003(2) O1 0.041(2) 0.049(3) 0.069(3) -0.006(2) -0.0056(18) -0.0034(18) O2 0.153(6) 0.054(3) 0.132(6) 0.016(3) -0.042(5) -0.004(4) N1 0.055(3) 0.037(2) 0.045(3) -0.0077(19) -0.013(2) 0.0071(19) C1 0.038(3) 0.039(3) 0.044(3) -0.005(2) -0.004(2) 0.001(2) C2 0.044(3) 0.032(2) 0.045(3) -0.004(2) -0.009(2) 0.001(2) C3 0.053(3) 0.049(3) 0.052(3) -0.012(3) -0.019(3) 0.013(3) C4 0.065(4) 0.046(3) 0.049(3) -0.013(3) -0.022(3) 0.011(3) C5 0.055(3) 0.068(4) 0.056(4) -0.015(3) -0.018(3) 0.021(3) C6 0.057(3) 0.062(4) 0.051(3) -0.022(3) -0.019(3) 0.015(3) C7 0.054(3) 0.038(3) 0.044(3) -0.007(2) -0.010(2) 0.003(2) C8 0.071(4) 0.049(3) 0.059(4) -0.003(3) 0.000(3) 0.003(3) C9 0.118(7) 0.056(4) 0.056(4) 0.002(3) 0.003(4) -0.015(4) C10 0.148(8) 0.046(4) 0.064(5) 0.004(3) -0.027(5) 0.011(5) C11 0.099(6) 0.062(5) 0.096(6) 0.001(4) -0.029(5) 0.028(4) C12 0.063(4) 0.055(4) 0.086(5) 0.000(3) -0.012(4) 0.014(3) C13 0.050(3) 0.040(3) 0.046(3) -0.011(2) -0.009(2) 0.007(2) C14 0.068(4) 0.092(5) 0.052(4) -0.007(4) 0.001(3) -0.002(4) C15 0.117(7) 0.116(7) 0.047(4) -0.010(4) 0.003(4) 0.001(6) C16 0.133(8) 0.078(5) 0.053(4) -0.023(4) -0.032(5) 0.030(5) C17 0.101(6) 0.066(4) 0.077(5) -0.023(4) -0.044(5) 0.011(4) C18 0.065(4) 0.064(4) 0.055(4) -0.010(3) -0.011(3) -0.001(3) C19 0.21(2) 0.43(4) 0.55(5) 0.32(4) -0.28(3) -0.16(2) C20 1.06(11) 0.24(3) 0.60(6) -0.10(4) -0.67(8) 0.29(5) _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 N1 2.025(4) 2 ? Pd1 N1 2.025(4) . ? Pd1 I1 2.6118(4) 2 ? Pd1 I1 2.6118(4) . ? S1 C19 1.523(15) . ? S1 O2 1.525(8) . ? S1 C20 1.66(3) . ? O1 C1 1.430(7) . ? N1 C5 1.325(7) . ? N1 C4 1.341(7) . ? C1 C7 1.530(8) . ? C1 C2 1.541(7) . ? C1 C13 1.543(8) . ? C2 C6 1.376(8) . ? C2 C3 1.388(8) . ? C3 C4 1.364(8) . ? C5 C6 1.375(8) . ? C7 C12 1.379(9) . ? C7 C8 1.393(9) . ? C8 C9 1.384(10) . ? C9 C10 1.362(12) . ? C10 C11 1.367(13) . ? C11 C12 1.380(11) . ? C13 C14 1.371(9) . ? C13 C18 1.377(9) . ? C14 C15 1.397(11) . ? C15 C16 1.354(13) . ? C16 C17 1.365(13) . ? C17 C18 1.398(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.0(4) 2 . ? N1 Pd1 I1 88.99(13) 2 2 ? N1 Pd1 I1 91.01(13) . 2 ? N1 Pd1 I1 91.01(13) 2 . ? N1 Pd1 I1 88.99(13) . . ? I1 Pd1 I1 180.00(2) 2 . ? C19 S1 O2 96.3(11) . . ? C19 S1 C20 83.0(14) . . ? O2 S1 C20 107.5(15) . . ? C5 N1 C4 117.8(5) . . ? C5 N1 Pd1 120.6(4) . . ? C4 N1 Pd1 121.6(4) . . ? O1 C1 C7 105.8(4) . . ? O1 C1 C2 107.1(4) . . ? C7 C1 C2 110.4(4) . . ? O1 C1 C13 110.9(4) . . ? C7 C1 C13 108.8(4) . . ? C2 C1 C13 113.5(4) . . ? C6 C2 C3 116.2(5) . . ? C6 C2 C1 125.7(5) . . ? C3 C2 C1 118.1(5) . . ? C4 C3 C2 120.5(5) . . ? N1 C4 C3 122.4(5) . . ? N1 C5 C6 122.5(5) . . ? C5 C6 C2 120.6(5) . . ? C12 C7 C8 117.2(6) . . ? C12 C7 C1 120.4(6) . . ? C8 C7 C1 122.4(5) . . ? C9 C8 C7 121.3(7) . . ? C10 C9 C8 120.2(8) . . ? C9 C10 C11 119.5(7) . . ? C10 C11 C12 120.6(8) . . ? C11 C12 C7 121.2(7) . . ? C14 C13 C18 117.7(6) . . ? C14 C13 C1 120.1(5) . . ? C18 C13 C1 122.1(5) . . ? C13 C14 C15 120.6(8) . . ? C16 C15 C14 120.9(8) . . ? C15 C16 C17 119.8(7) . . ? C16 C17 C18 119.3(8) . . ? C13 C18 C17 121.7(7) . . ? 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 O1 H100 O2 0.85(8) 1.87(8) 2.711(7) 174(8) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.89 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.936 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.109 #===END data_pdidmf2 _database_code_depnum_ccdc_archive 'CCDC 273904' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 I2 N4 O4 Pd' _chemical_formula_weight 1027.00 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' I I -0.4742 1.8119 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0847(4) _cell_length_b 12.3248(6) _cell_length_c 12.7151(7) _cell_angle_alpha 88.9990(10) _cell_angle_beta 74.2400(10) _cell_angle_gamma 86.5110(10) _cell_volume 1066.53(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism ' _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 506 _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type 'symmetry-related measurements' _exptl_absorpt_correction_T_min 0.769341 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'as implemented in SAINT+/SADABS package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10455 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.38 _reflns_number_total 3915 _reflns_number_gt 3310 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_cell_refinement ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_data_reduction ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. SADABS: Siemens Area Detector Absorption Correction Software, Sheldrick G., 1996, University of Goettingen, Germany. ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; PARST - M. Nardelli, J. Appl. Crystallogr. 1995, 28, 659 ; _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^)+(0.0439P)^2^+1.1205P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3915 _refine_ls_number_parameters 247 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 3.413 _refine_ls_shift/su_mean 0.084 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 0.0000 0.0000 0.5000 0.04187(11) Uani 1 2 d S . . I1 I 0.18105(4) 0.16158(2) 0.39100(2) 0.06651(12) Uani 1 1 d . . . O1 O 0.8723(4) -0.2521(3) 0.2205(2) 0.0670(8) Uani 1 1 d D . . O2 O 1.1501(12) -0.2132(15) 0.0477(6) 0.408(11) Uani 1 1 d . . . N1 N 0.2158(4) -0.1043(2) 0.4135(2) 0.0481(7) Uani 1 1 d . . . N2 N 1.2169(7) -0.1479(5) -0.1165(5) 0.1049(15) Uani 1 1 d . . . C1 C 0.7012(5) -0.3097(3) 0.2227(3) 0.0494(8) Uani 1 1 d . . . C2 C 0.5252(5) -0.2371(3) 0.2869(3) 0.0461(7) Uani 1 1 d . . . C3 C 0.5421(5) -0.1820(3) 0.3780(3) 0.0514(8) Uani 1 1 d . . . H3 H 0.6592 -0.1887 0.3980 0.062 Uiso 1 1 calc R . . C4 C 0.3883(6) -0.1181(3) 0.4383(3) 0.0523(8) Uani 1 1 d . . . H4 H 0.4035 -0.0825 0.4991 0.063 Uiso 1 1 calc R . . C5 C 0.1958(6) -0.1590(3) 0.3274(3) 0.0581(9) Uani 1 1 d . . . H5 H 0.0762 -0.1523 0.3102 0.070 Uiso 1 1 calc R . . C6 C 0.3456(5) -0.2248(3) 0.2634(3) 0.0569(9) Uani 1 1 d . . . H6 H 0.3259 -0.2611 0.2041 0.068 Uiso 1 1 calc R . . C7 C 0.7058(6) -0.4139(3) 0.2885(3) 0.0589(10) Uani 1 1 d . . . C8 C 0.8687(8) -0.4460(4) 0.3247(4) 0.0785(13) Uani 1 1 d . . . H8 H 0.9769 -0.4034 0.3089 0.094 Uiso 1 1 calc R . . C9 C 0.8713(12) -0.5419(5) 0.3848(5) 0.109(2) Uani 1 1 d . . . H9 H 0.9811 -0.5627 0.4087 0.131 Uiso 1 1 calc R . . C10 C 0.7155(15) -0.6043(5) 0.4085(6) 0.121(3) Uani 1 1 d . . . H10 H 0.7194 -0.6683 0.4477 0.145 Uiso 1 1 calc R . . C11 C 0.5506(12) -0.5740(5) 0.3750(6) 0.116(2) Uani 1 1 d . . . H11 H 0.4429 -0.6170 0.3924 0.139 Uiso 1 1 calc R . . C12 C 0.5455(8) -0.4791(4) 0.3152(5) 0.0824(14) Uani 1 1 d . . . H12 H 0.4340 -0.4588 0.2927 0.099 Uiso 1 1 calc R . . C13 C 0.6980(5) -0.3307(3) 0.1046(3) 0.0545(9) Uani 1 1 d . . . C14 C 0.7394(8) -0.4321(4) 0.0572(4) 0.0778(13) Uani 1 1 d . . . H14 H 0.7572 -0.4925 0.0991 0.093 Uiso 1 1 calc R . . C15 C 0.7546(9) -0.4441(5) -0.0542(5) 0.0995(18) Uani 1 1 d . . . H15 H 0.7836 -0.5129 -0.0855 0.119 Uiso 1 1 calc R . . C16 C 0.7285(8) -0.3596(6) -0.1164(4) 0.0952(18) Uani 1 1 d . . . H16 H 0.7376 -0.3697 -0.1900 0.114 Uiso 1 1 calc R . . C17 C 0.6884(8) -0.2579(5) -0.0718(4) 0.0901(16) Uani 1 1 d . . . H17 H 0.6709 -0.1986 -0.1152 0.108 Uiso 1 1 calc R . . C18 C 0.6738(7) -0.2427(4) 0.0382(4) 0.0716(11) Uani 1 1 d . . . H18 H 0.6475 -0.1731 0.0678 0.086 Uiso 1 1 calc R . . C19 C 1.1695(12) -0.2263(12) -0.0484(9) 0.185(5) Uani 1 1 d . . . C20 C 1.275(3) -0.0589(11) -0.075(3) 0.425(18) Uani 1 1 d . . . H20A H 1.2020 0.0047 -0.0900 0.637 Uiso 1 1 calc R . . H20B H 1.4127 -0.0515 -0.1073 0.637 Uiso 1 1 calc R . . H20C H 1.2515 -0.0672 0.0030 0.637 Uiso 1 1 calc R . . C21 C 1.2227(18) -0.161(2) -0.2181(10) 0.45(2) Uani 1 1 d . . . H21A H 1.1006 -0.1337 -0.2303 0.672 Uiso 1 1 calc R . . H21B H 1.2435 -0.2370 -0.2359 0.672 Uiso 1 1 calc R . . H21C H 1.3283 -0.1222 -0.2635 0.672 Uiso 1 1 calc R . . H100 H 0.948(7) -0.227(5) 0.160(3) 0.11(2) Uiso 1 1 d 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 0.0450(2) 0.0418(2) 0.03765(19) -0.00098(14) -0.00994(15) 0.00149(14) I1 0.0713(2) 0.05882(18) 0.06563(19) 0.01526(13) -0.01218(14) -0.00803(13) O1 0.0488(15) 0.089(2) 0.0618(18) -0.0071(15) -0.0097(13) -0.0193(14) O2 0.183(7) 0.98(3) 0.098(5) 0.133(10) -0.048(5) -0.302(13) N1 0.0502(16) 0.0483(16) 0.0448(15) -0.0026(12) -0.0119(13) 0.0006(13) N2 0.080(3) 0.111(4) 0.114(4) -0.003(3) -0.010(3) -0.007(3) C1 0.0442(18) 0.054(2) 0.0485(19) -0.0024(16) -0.0089(15) -0.0037(15) C2 0.0479(18) 0.0446(18) 0.0438(18) 0.0017(14) -0.0091(14) -0.0049(14) C3 0.052(2) 0.059(2) 0.0479(19) -0.0029(16) -0.0209(16) 0.0018(16) C4 0.058(2) 0.055(2) 0.0464(19) -0.0062(16) -0.0200(16) 0.0015(16) C5 0.047(2) 0.073(3) 0.058(2) -0.0151(19) -0.0198(17) 0.0018(18) C6 0.051(2) 0.068(2) 0.053(2) -0.0184(18) -0.0151(17) -0.0005(17) C7 0.065(2) 0.055(2) 0.049(2) -0.0030(17) -0.0064(18) 0.0105(18) C8 0.081(3) 0.081(3) 0.070(3) 0.000(2) -0.019(2) 0.019(3) C9 0.138(6) 0.094(4) 0.087(4) 0.011(3) -0.028(4) 0.046(4) C10 0.169(8) 0.074(4) 0.094(4) 0.024(3) -0.002(5) 0.032(5) C11 0.132(6) 0.066(3) 0.123(5) 0.018(3) 0.013(4) -0.013(4) C12 0.083(3) 0.061(3) 0.094(4) 0.009(2) -0.008(3) -0.009(2) C13 0.0443(19) 0.069(2) 0.0457(19) -0.0060(17) -0.0046(15) -0.0024(17) C14 0.091(3) 0.074(3) 0.063(3) -0.014(2) -0.014(2) 0.002(2) C15 0.120(5) 0.105(4) 0.068(3) -0.033(3) -0.015(3) 0.000(4) C16 0.087(4) 0.146(6) 0.051(3) -0.020(3) -0.017(2) -0.002(4) C17 0.088(4) 0.126(5) 0.054(3) 0.012(3) -0.016(2) 0.001(3) C18 0.076(3) 0.081(3) 0.055(2) 0.000(2) -0.015(2) 0.000(2) C19 0.089(5) 0.332(16) 0.142(8) 0.087(10) -0.038(5) -0.068(7) C20 0.27(2) 0.133(11) 0.88(6) -0.18(2) -0.18(3) 0.052(11) C21 0.127(9) 1.11(6) 0.107(8) 0.058(18) -0.015(7) -0.139(19) _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 N1 2.024(3) 2_556 ? Pd1 N1 2.024(3) . ? Pd1 I1 2.6040(3) . ? Pd1 I1 2.6040(3) 2_556 ? O1 C1 1.435(4) . ? O2 C19 1.205(12) . ? N1 C5 1.341(4) . ? N1 C4 1.343(5) . ? N2 C19 1.284(11) . ? N2 C21 1.294(13) . ? N2 C20 1.360(15) . ? C1 C7 1.525(6) . ? C1 C13 1.534(5) . ? C1 C2 1.535(5) . ? C2 C6 1.383(5) . ? C2 C3 1.390(5) . ? C3 C4 1.363(5) . ? C5 C6 1.376(5) . ? C7 C8 1.388(7) . ? C7 C12 1.394(7) . ? C8 C9 1.398(8) . ? C9 C10 1.347(10) . ? C10 C11 1.378(11) . ? C11 C12 1.387(8) . ? C13 C14 1.377(6) . ? C13 C18 1.395(6) . ? C14 C15 1.401(7) . ? C15 C16 1.332(8) . ? C16 C17 1.367(8) . ? C17 C18 1.389(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.00(15) 2_556 . ? N1 Pd1 I1 90.50(8) 2_556 . ? N1 Pd1 I1 89.50(8) . . ? N1 Pd1 I1 89.50(8) 2_556 2_556 ? N1 Pd1 I1 90.50(8) . 2_556 ? I1 Pd1 I1 180.000(7) . 2_556 ? C5 N1 C4 117.4(3) . . ? C5 N1 Pd1 121.8(2) . . ? C4 N1 Pd1 120.8(2) . . ? C19 N2 C21 119.9(14) . . ? C19 N2 C20 114.6(15) . . ? C21 N2 C20 125.2(17) . . ? O1 C1 C7 108.8(3) . . ? O1 C1 C13 108.6(3) . . ? C7 C1 C13 112.9(3) . . ? O1 C1 C2 105.8(3) . . ? C7 C1 C2 107.1(3) . . ? C13 C1 C2 113.4(3) . . ? C6 C2 C3 116.5(3) . . ? C6 C2 C1 124.9(3) . . ? C3 C2 C1 118.6(3) . . ? C4 C3 C2 120.4(3) . . ? N1 C4 C3 122.8(3) . . ? N1 C5 C6 122.5(3) . . ? C5 C6 C2 120.3(3) . . ? C8 C7 C12 118.1(5) . . ? C8 C7 C1 121.0(4) . . ? C12 C7 C1 120.9(4) . . ? C7 C8 C9 120.4(6) . . ? C10 C9 C8 120.4(7) . . ? C9 C10 C11 120.6(6) . . ? C10 C11 C12 119.8(7) . . ? C11 C12 C7 120.7(6) . . ? C14 C13 C18 117.8(4) . . ? C14 C13 C1 122.6(4) . . ? C18 C13 C1 119.2(4) . . ? C13 C14 C15 119.9(5) . . ? C16 C15 C14 121.6(5) . . ? C15 C16 C17 119.8(5) . . ? C16 C17 C18 120.2(5) . . ? C17 C18 C13 120.6(5) . . ? O2 C19 N2 120.7(15) . . ? 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 O1 H100 O2 0.87(2) 1.75(3) 2.581(7) 161(6) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.051 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.068 #===END data_pdidiox _database_code_depnum_ccdc_archive 'CCDC 273905' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 I2 N2 O5 Pd' _chemical_formula_weight 1014.98 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' I I -0.4742 1.8119 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3880(10) _cell_length_b 13.834(2) _cell_length_c 14.151(2) _cell_angle_alpha 64.580(2) _cell_angle_beta 67.931(2) _cell_angle_gamma 83.780(2) _cell_volume 2025.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 2.027 _exptl_absorpt_correction_type 'symmetry-related measurements' _exptl_absorpt_correction_T_min 0.580494 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'as implemented in SAINT+/SADABS package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18515 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 24.80 _reflns_number_total 6930 _reflns_number_gt 4132 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_cell_refinement ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_data_reduction ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. SADABS: Siemens Area Detector Absorption Correction Software, Sheldrick G., 1996, University of Goettingen, Germany. ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; PARST - M. Nardelli, J. Appl. Crystallogr. 1995, 28, 659 ; _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^)+(0.0745P)^2^+4.9308P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6930 _refine_ls_number_parameters 474 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.002 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 0.74097(6) 0.97281(4) 0.25844(5) 0.0590(2) Uani 1 1 d . . . I1 I 0.85858(9) 1.12587(6) 0.06753(5) 0.1310(4) Uani 1 1 d . . . I2 I 0.61730(6) 0.82344(4) 0.45064(4) 0.0797(2) Uani 1 1 d . . . N1 N 0.7803(6) 1.0471(4) 0.3384(5) 0.0563(15) Uani 1 1 d . . . N2 N 0.6960(7) 0.8988(5) 0.1799(5) 0.0704(19) Uani 1 1 d . . . O1 O 0.9995(5) 1.2632(5) 0.4039(5) 0.0752(17) Uani 1 1 d . . . O2 O 0.4332(6) 0.7201(5) 0.1110(7) 0.100(2) Uani 1 1 d . . . H2 H 0.4019 0.6608 0.1581 0.150 Uiso 1 1 calc R . . O3 O 0.2757(7) 0.5587(6) 0.1895(7) 0.124(3) Uani 1 1 d . . . O4 O 0.1103(6) 0.4325(5) 0.3972(5) 0.0849(17) Uani 1 1 d . . . C1 C 0.8809(6) 1.2366(5) 0.4713(6) 0.0529(17) Uani 1 1 d . . . C2 C 0.8415(6) 1.1674(5) 0.4287(6) 0.0508(16) Uani 1 1 d . . . C3 C 0.7322(7) 1.1648(6) 0.4280(7) 0.063(2) Uani 1 1 d . . . H3 H 0.6757 1.2047 0.4576 0.075 Uiso 1 1 calc R . . C4 C 0.7040(7) 1.1032(6) 0.3839(6) 0.0620(19) Uani 1 1 d . . . H4 H 0.6280 1.1017 0.3866 0.074 Uiso 1 1 calc R . . C5 C 0.8849(8) 1.0442(7) 0.3428(8) 0.081(3) Uani 1 1 d . . . H5 H 0.9387 1.0017 0.3146 0.098 Uiso 1 1 calc R . . C6 C 0.9179(7) 1.1025(6) 0.3880(8) 0.077(2) Uani 1 1 d . . . H6 H 0.9923 1.0974 0.3907 0.092 Uiso 1 1 calc R . . C7 C 0.8672(7) 1.1741(5) 0.5946(6) 0.0593(19) Uani 1 1 d . . . C8 C 0.9405(8) 1.1996(7) 0.6344(8) 0.078(2) Uani 1 1 d . . . H8 H 1.0014 1.2517 0.5850 0.093 Uiso 1 1 calc R . . C9 C 0.9243(11) 1.1482(9) 0.7477(9) 0.101(4) Uani 1 1 d . . . H9 H 0.9732 1.1675 0.7740 0.122 Uiso 1 1 calc R . . C10 C 0.8372(13) 1.0692(8) 0.8213(9) 0.112(4) Uani 1 1 d . . . H10 H 0.8265 1.0348 0.8972 0.134 Uiso 1 1 calc R . . C11 C 0.7670(11) 1.0423(7) 0.7816(8) 0.108(4) Uani 1 1 d . . . H11 H 0.7076 0.9888 0.8306 0.130 Uiso 1 1 calc R . . C12 C 0.7826(10) 1.0931(7) 0.6696(7) 0.088(3) Uani 1 1 d . . . H12 H 0.7345 1.0719 0.6440 0.106 Uiso 1 1 calc R . . C13 C 0.8124(7) 1.3378(5) 0.4570(6) 0.0580(19) Uani 1 1 d . . . C14 C 0.7134(9) 1.3463(8) 0.5363(8) 0.086(3) Uani 1 1 d . . . H14 H 0.6822 1.2865 0.6042 0.103 Uiso 1 1 calc R . . C18 C 0.8543(9) 1.4286(7) 0.3576(8) 0.085(3) Uani 1 1 d . . . H18 H 0.9221 1.4266 0.3004 0.101 Uiso 1 1 calc R . . C16 C 0.7036(14) 1.5300(10) 0.4205(14) 0.121(5) Uani 1 1 d . . . H16 H 0.6689 1.5951 0.4092 0.146 Uiso 1 1 calc R . . C15 C 0.6567(11) 1.4406(11) 0.5203(11) 0.109(4) Uani 1 1 d . . . H15 H 0.5880 1.4436 0.5761 0.131 Uiso 1 1 calc R . . C17 C 0.7979(14) 1.5219(8) 0.3418(13) 0.123(5) Uani 1 1 d . . . H17 H 0.8273 1.5812 0.2731 0.148 Uiso 1 1 calc R . . C19 C 0.5558(7) 0.7123(6) 0.0666(7) 0.067(2) Uani 1 1 d . . . C20 C 0.6089(7) 0.7817(6) 0.1058(6) 0.0624(19) Uani 1 1 d . . . C21 C 0.5420(9) 0.8481(7) 0.1437(8) 0.086(3) Uani 1 1 d . . . H21 H 0.4659 0.8563 0.1453 0.104 Uiso 1 1 calc R . . C22 C 0.5877(10) 0.9043(7) 0.1803(8) 0.094(3) Uani 1 1 d . . . H22 H 0.5396 0.9502 0.2078 0.112 Uiso 1 1 calc R . . C23 C 0.7650(9) 0.8372(7) 0.1375(7) 0.081(3) Uani 1 1 d . . . H23 H 0.8418 0.8326 0.1339 0.098 Uiso 1 1 calc R . . C24 C 0.7211(8) 0.7757(6) 0.0957(7) 0.073(2) Uani 1 1 d . . . H24 H 0.7699 0.7336 0.0629 0.088 Uiso 1 1 calc R . . C25 C 0.5863(8) 0.5942(6) 0.1128(7) 0.068(2) Uani 1 1 d . . . C26 C 0.5878(9) 0.5426(7) 0.2211(7) 0.087(3) Uani 1 1 d . . . H26 H 0.5851 0.5828 0.2604 0.105 Uiso 1 1 calc R . . C27 C 0.5932(10) 0.4347(7) 0.2702(8) 0.095(3) Uani 1 1 d . . . H27 H 0.5940 0.4022 0.3427 0.114 Uiso 1 1 calc R . . C28 C 0.5975(9) 0.3737(6) 0.2165(8) 0.086(3) Uani 1 1 d . . . H28 H 0.5968 0.2995 0.2530 0.103 Uiso 1 1 calc R . . C29 C 0.6031(8) 0.4222(6) 0.1068(8) 0.078(2) Uani 1 1 d . . . H29 H 0.6109 0.3813 0.0672 0.093 Uiso 1 1 calc R . . C30 C 0.5970(8) 0.5321(6) 0.0560(7) 0.073(2) Uani 1 1 d . . . H30 H 0.6003 0.5645 -0.0179 0.088 Uiso 1 1 calc R . . C31 C 0.5954(10) 0.7645(5) -0.0596(7) 0.072(2) Uani 1 1 d . . . C32 C 0.5158(12) 0.8156(7) -0.1129(10) 0.112(4) Uani 1 1 d . . . H32 H 0.4386 0.8189 -0.0699 0.134 Uiso 1 1 calc R . . C33 C 0.5522(19) 0.8607(10) -0.2288(14) 0.143(7) Uani 1 1 d . . . H33 H 0.5016 0.8976 -0.2652 0.172 Uiso 1 1 calc R . . C34 C 0.664(2) 0.8495(9) -0.2878(13) 0.151(8) Uani 1 1 d . . . H34 H 0.6885 0.8755 -0.3656 0.181 Uiso 1 1 calc R . . C35 C 0.7407(14) 0.8020(9) -0.2377(11) 0.125(4) Uani 1 1 d . . . H35 H 0.8177 0.7992 -0.2815 0.150 Uiso 1 1 calc R . . C36 C 0.7066(12) 0.7574(8) -0.1222(10) 0.099(3) Uani 1 1 d . . . H36 H 0.7595 0.7229 -0.0880 0.119 Uiso 1 1 calc R . . C38 C 0.2284(10) 0.4058(8) 0.3617(10) 0.099(3) Uani 1 1 d . . . H38A H 0.2321 0.3285 0.3952 0.119 Uiso 1 1 calc R . . H38B H 0.2728 0.4363 0.3873 0.119 Uiso 1 1 calc R . . C39 C 0.1057(9) 0.5450(7) 0.3489(9) 0.096(3) Uani 1 1 d . . . H39A H 0.1474 0.5764 0.3759 0.115 Uiso 1 1 calc R . . H39B H 0.0250 0.5635 0.3719 0.115 Uiso 1 1 calc R . . C40 C 0.1574(11) 0.5890(9) 0.2262(10) 0.112(4) Uani 1 1 d . . . H40A H 0.1113 0.5628 0.1987 0.134 Uiso 1 1 calc R . . H40B H 0.1566 0.6666 0.1950 0.134 Uiso 1 1 calc R . . C37 C 0.2796(10) 0.4464(9) 0.2401(11) 0.112(4) Uani 1 1 d . . . H37A H 0.3599 0.4271 0.2176 0.135 Uiso 1 1 calc R . . H37B H 0.2371 0.4138 0.2147 0.135 Uiso 1 1 calc R . . O100 O 0.0533(16) 0.4585(16) 0.0749(15) 0.316(10) Uani 1 1 d D . . C100 C -0.047(2) 0.4038(13) 0.0834(13) 0.287(16) Uani 1 1 d D . . H10A H -0.0486 0.3268 0.1253 0.344 Uiso 1 1 calc R . . H10B H -0.1202 0.4296 0.1196 0.344 Uiso 1 1 calc R . . C101 C 0.030(3) 0.5700(14) 0.0263(18) 0.41(3) Uani 1 1 d D . . H10C H -0.0494 0.5813 0.0662 0.493 Uiso 1 1 calc R . . H10D H 0.0827 0.6140 0.0304 0.493 Uiso 1 1 calc R . . H100 H 1.019(5) 1.312(4) 0.405(4) 0.020(15) Uiso 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 0.0960(5) 0.0441(3) 0.0546(3) -0.0301(3) -0.0329(3) -0.0039(3) I1 0.2205(10) 0.0996(5) 0.0617(4) -0.0279(4) -0.0246(5) -0.0741(6) I2 0.1191(5) 0.0601(3) 0.0629(4) -0.0239(3) -0.0342(3) -0.0110(3) N1 0.076(4) 0.048(3) 0.066(4) -0.037(3) -0.036(3) 0.012(3) N2 0.120(6) 0.046(3) 0.063(4) -0.025(3) -0.046(4) -0.006(4) O1 0.074(4) 0.077(4) 0.097(4) -0.059(4) -0.026(3) -0.003(3) O2 0.085(5) 0.075(4) 0.158(7) -0.060(4) -0.048(4) 0.003(3) O3 0.104(6) 0.098(5) 0.130(6) -0.042(5) 0.002(5) -0.029(5) O4 0.092(5) 0.074(4) 0.098(4) -0.049(3) -0.027(4) -0.003(3) C1 0.067(5) 0.051(4) 0.060(4) -0.035(3) -0.031(4) 0.006(3) C2 0.069(5) 0.042(3) 0.054(4) -0.026(3) -0.030(4) 0.008(3) C3 0.065(5) 0.064(4) 0.090(6) -0.059(4) -0.032(4) 0.013(4) C4 0.068(5) 0.059(4) 0.087(5) -0.046(4) -0.041(4) 0.015(4) C5 0.079(6) 0.082(6) 0.129(8) -0.086(6) -0.042(6) 0.025(5) C6 0.075(6) 0.074(5) 0.128(7) -0.072(6) -0.056(5) 0.025(4) C7 0.087(6) 0.045(4) 0.072(5) -0.037(4) -0.045(4) 0.017(4) C8 0.107(7) 0.077(5) 0.090(6) -0.054(5) -0.061(6) 0.027(5) C9 0.159(11) 0.101(8) 0.109(8) -0.072(7) -0.095(8) 0.052(8) C10 0.231(14) 0.057(6) 0.072(6) -0.032(5) -0.081(8) 0.031(7) C11 0.197(12) 0.061(5) 0.073(6) -0.022(5) -0.059(7) -0.009(6) C12 0.145(9) 0.057(5) 0.073(6) -0.024(4) -0.051(6) -0.009(5) C13 0.085(6) 0.044(4) 0.070(5) -0.034(4) -0.043(4) 0.008(4) C14 0.116(8) 0.085(6) 0.082(6) -0.054(5) -0.047(6) 0.024(6) C18 0.102(7) 0.065(5) 0.096(7) -0.026(5) -0.055(6) 0.002(5) C16 0.187(14) 0.081(8) 0.196(15) -0.092(10) -0.149(13) 0.065(9) C15 0.134(10) 0.133(10) 0.137(10) -0.108(9) -0.088(9) 0.074(8) C17 0.173(13) 0.057(6) 0.172(13) -0.031(7) -0.123(12) 0.023(7) C19 0.065(5) 0.063(5) 0.090(6) -0.046(4) -0.032(4) 0.008(4) C20 0.078(6) 0.056(4) 0.054(4) -0.026(4) -0.023(4) 0.007(4) C21 0.103(7) 0.081(6) 0.110(7) -0.057(6) -0.056(6) 0.011(5) C22 0.133(9) 0.085(6) 0.107(8) -0.063(6) -0.063(7) 0.006(6) C23 0.119(7) 0.069(5) 0.085(6) -0.048(5) -0.050(6) 0.012(5) C24 0.075(6) 0.064(5) 0.094(6) -0.050(5) -0.026(5) 0.007(4) C25 0.101(6) 0.049(4) 0.068(5) -0.023(4) -0.046(5) 0.000(4) C26 0.146(9) 0.060(5) 0.078(6) -0.034(5) -0.057(6) 0.002(5) C27 0.156(10) 0.060(5) 0.082(6) -0.020(5) -0.066(6) -0.002(6) C28 0.130(8) 0.044(4) 0.098(7) -0.021(5) -0.068(6) 0.004(5) C29 0.107(7) 0.056(5) 0.101(7) -0.049(5) -0.054(6) 0.014(4) C30 0.124(7) 0.052(4) 0.061(5) -0.027(4) -0.045(5) -0.003(4) C31 0.142(9) 0.033(4) 0.064(5) -0.022(4) -0.059(6) 0.001(4) C32 0.195(12) 0.061(5) 0.123(9) -0.043(6) -0.098(9) 0.005(7) C33 0.29(2) 0.066(7) 0.147(15) -0.047(9) -0.165(16) 0.034(11) C34 0.35(3) 0.046(6) 0.110(11) -0.025(7) -0.148(16) -0.002(11) C35 0.205(14) 0.074(7) 0.092(9) -0.041(6) -0.034(9) -0.026(8) C36 0.142(10) 0.069(6) 0.100(8) -0.046(6) -0.042(7) -0.011(6) C38 0.111(9) 0.098(7) 0.142(10) -0.076(7) -0.078(8) 0.025(6) C39 0.087(7) 0.085(7) 0.132(9) -0.072(7) -0.026(6) 0.005(5) C40 0.106(9) 0.092(8) 0.126(10) -0.040(7) -0.037(8) 0.004(6) C37 0.088(7) 0.114(9) 0.145(11) -0.085(9) -0.018(7) 0.003(6) O100 0.30(2) 0.237(18) 0.40(3) -0.056(19) -0.20(2) -0.023(15) C100 0.41(3) 0.27(2) 0.135(14) -0.026(15) -0.047(18) -0.26(3) C101 0.97(9) 0.145(18) 0.25(3) -0.102(19) -0.34(4) 0.02(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 N1 2.023(5) . ? Pd1 N2 2.040(6) . ? Pd1 I1 2.5893(9) . ? Pd1 I2 2.5970(8) . ? N1 C4 1.313(8) . ? N1 C5 1.316(10) . ? N2 C23 1.308(10) . ? N2 C22 1.334(11) . ? O1 C1 1.402(9) . ? O2 C19 1.420(10) . ? O3 C37 1.409(13) . ? O3 C40 1.440(12) . ? O4 C39 1.410(10) . ? O4 C38 1.421(11) . ? C1 C7 1.528(10) . ? C1 C2 1.529(9) . ? C1 C13 1.532(9) . ? C2 C3 1.362(10) . ? C2 C6 1.372(10) . ? C3 C4 1.386(9) . ? C5 C6 1.393(10) . ? C7 C12 1.371(12) . ? C7 C8 1.374(11) . ? C8 C9 1.389(12) . ? C9 C10 1.370(16) . ? C10 C11 1.351(15) . ? C11 C12 1.373(12) . ? C13 C14 1.351(11) . ? C13 C18 1.379(11) . ? C14 C15 1.383(13) . ? C18 C17 1.370(14) . ? C16 C17 1.311(17) . ? C16 C15 1.379(17) . ? C19 C31 1.504(11) . ? C19 C25 1.541(10) . ? C19 C20 1.590(11) . ? C20 C21 1.320(11) . ? C20 C24 1.339(11) . ? C21 C22 1.363(11) . ? C23 C24 1.465(11) . ? C25 C30 1.375(10) . ? C25 C26 1.393(11) . ? C26 C27 1.356(11) . ? C27 C28 1.343(12) . ? C28 C29 1.379(11) . ? C29 C30 1.382(10) . ? C31 C36 1.349(13) . ? C31 C32 1.411(13) . ? C32 C33 1.382(17) . ? C33 C34 1.35(2) . ? C34 C35 1.345(19) . ? C35 C36 1.378(14) . ? C38 C37 1.452(14) . ? C39 C40 1.462(14) . ? O100 C101 1.441(16) . ? O100 C100 1.470(14) . ? C100 C101 1.368(12) 2_565 ? C101 C100 1.368(12) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 178.2(3) . . ? N1 Pd1 I1 89.30(17) . . ? N2 Pd1 I1 91.45(18) . . ? N1 Pd1 I2 90.32(17) . . ? N2 Pd1 I2 88.89(18) . . ? I1 Pd1 I2 178.09(4) . . ? C4 N1 C5 117.6(6) . . ? C4 N1 Pd1 121.3(5) . . ? C5 N1 Pd1 121.0(5) . . ? C23 N2 C22 117.4(7) . . ? C23 N2 Pd1 123.1(6) . . ? C22 N2 Pd1 119.2(6) . . ? C37 O3 C40 110.3(8) . . ? C39 O4 C38 109.2(7) . . ? O1 C1 C7 109.7(6) . . ? O1 C1 C2 104.2(6) . . ? C7 C1 C2 111.4(6) . . ? O1 C1 C13 110.8(6) . . ? C7 C1 C13 109.6(6) . . ? C2 C1 C13 111.0(5) . . ? C3 C2 C6 115.8(6) . . ? C3 C2 C1 124.0(6) . . ? C6 C2 C1 120.2(6) . . ? C2 C3 C4 120.8(7) . . ? N1 C4 C3 122.7(7) . . ? N1 C5 C6 122.4(7) . . ? C2 C6 C5 120.5(7) . . ? C12 C7 C8 117.5(8) . . ? C12 C7 C1 122.6(7) . . ? C8 C7 C1 119.9(7) . . ? C7 C8 C9 120.4(10) . . ? C10 C9 C8 120.7(10) . . ? C11 C10 C9 118.8(9) . . ? C10 C11 C12 120.7(11) . . ? C7 C12 C11 121.8(9) . . ? C14 C13 C18 116.3(8) . . ? C14 C13 C1 124.8(7) . . ? C18 C13 C1 118.9(8) . . ? C13 C14 C15 122.5(10) . . ? C17 C18 C13 121.1(11) . . ? C17 C16 C15 119.0(11) . . ? C16 C15 C14 119.0(11) . . ? C16 C17 C18 122.0(13) . . ? O2 C19 C31 107.9(7) . . ? O2 C19 C25 110.3(7) . . ? C31 C19 C25 112.7(6) . . ? O2 C19 C20 104.8(6) . . ? C31 C19 C20 108.9(6) . . ? C25 C19 C20 111.9(6) . . ? C21 C20 C24 120.9(8) . . ? C21 C20 C19 118.8(8) . . ? C24 C20 C19 120.2(7) . . ? C20 C21 C22 118.1(9) . . ? N2 C22 C21 125.2(9) . . ? N2 C23 C24 119.9(9) . . ? C20 C24 C23 118.3(8) . . ? C30 C25 C26 117.2(7) . . ? C30 C25 C19 121.7(7) . . ? C26 C25 C19 120.5(7) . . ? C27 C26 C25 121.0(8) . . ? C28 C27 C26 121.5(9) . . ? C27 C28 C29 119.4(8) . . ? C28 C29 C30 119.6(7) . . ? C25 C30 C29 121.1(7) . . ? C36 C31 C32 119.6(9) . . ? C36 C31 C19 119.7(9) . . ? C32 C31 C19 120.6(10) . . ? C33 C32 C31 120.3(13) . . ? C34 C33 C32 117.8(15) . . ? C35 C34 C33 122.2(15) . . ? C34 C35 C36 120.9(15) . . ? C31 C36 C35 119.1(12) . . ? O4 C38 C37 110.8(9) . . ? O4 C39 C40 110.9(8) . . ? O3 C40 C39 110.9(9) . . ? O3 C37 C38 110.5(9) . . ? C101 O100 C100 102.7(14) . . ? C101 C100 O100 103.4(13) 2_565 . ? C100 C101 O100 106.7(14) 2_565 . ? 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 O2 H2 O3 0.82 2.01 2.686(9) 138.9 . O1 H100 O4 0.74(6) 2.06(6) 2.791(8) 167(6) 1_665 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.80 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.402 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.102 #===END data_pdi2cn _database_code_depnum_ccdc_archive 'CCDC 273906' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 I2 N2 O2 Pd' _chemical_formula_weight 882.82 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.955(2) _cell_length_b 11.153(2) _cell_length_c 14.248(3) _cell_angle_alpha 91.810(3) _cell_angle_beta 91.062(4) _cell_angle_gamma 105.529(3) _cell_volume 1675.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 2.430 _exptl_absorpt_correction_type 'symmetry-related measurements' _exptl_absorpt_correction_T_min 0.650788 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'as implemented in SAINT+/SADABS package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18347 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.33 _reflns_number_total 7432 _reflns_number_gt 4491 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_cell_refinement ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_data_reduction ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. SADABS: Siemens Area Detector Absorption Correction Software, Sheldrick G., 1996, University of Goettingen, Germany. ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; PARST - M. Nardelli, J. Appl. Crystallogr. 1995, 28, 659 ; _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^)+(0.2000P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7432 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1475 _refine_ls_R_factor_gt 0.1110 _refine_ls_wR_factor_ref 0.3703 _refine_ls_wR_factor_gt 0.3493 _refine_ls_goodness_of_fit_ref 1.308 _refine_ls_restrained_S_all 1.308 _refine_ls_shift/su_max 0.004 _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 0.09347(9) 0.20161(8) 0.16459(7) 0.0365(3) Uani 1 1 d . . . I1 I -0.04933(13) 0.06999(9) 0.28918(8) 0.0650(4) Uani 1 1 d . . . I2 I 0.22537(9) 0.33136(8) 0.03354(8) 0.0515(4) Uani 1 1 d . . . N1 N 0.1533(10) 0.0519(9) 0.1202(8) 0.038(2) Uani 1 1 d . . . N2 N 0.0446(10) 0.3526(10) 0.2161(8) 0.038(2) Uani 1 1 d . . . O1 O 0.1833(9) -0.3666(8) 0.0395(7) 0.046(2) Uani 1 1 d . . . H1 H 0.1950 -0.4245 0.0072 0.068 Uiso 1 1 calc R . . O2 O -0.0625(11) 0.7511(9) 0.2586(6) 0.047(2) Uani 1 1 d . . . H2 H -0.0932 0.8064 0.2778 0.070 Uiso 1 1 calc R . . C1 C 0.2924(12) -0.2627(11) 0.0377(9) 0.036(3) Uani 1 1 d . . . C2 C 0.2445(12) -0.1500(12) 0.0649(8) 0.037(3) Uani 1 1 d . . . C3 C 0.1148(12) -0.1593(11) 0.0605(9) 0.038(3) Uani 1 1 d . . . H3 H 0.0570 -0.2331 0.0395 0.046 Uiso 1 1 calc R . . C4 C 0.0736(11) -0.0568(10) 0.0881(9) 0.035(3) Uani 1 1 d . . . H4 H -0.0127 -0.0631 0.0842 0.042 Uiso 1 1 calc R . . C5 C 0.2792(13) 0.0609(13) 0.1241(11) 0.048(3) Uani 1 1 d . . . H5 H 0.3353 0.1352 0.1460 0.058 Uiso 1 1 calc R . . C6 C 0.3269(14) -0.0385(12) 0.0960(10) 0.046(3) Uani 1 1 d . . . H6 H 0.4138 -0.0297 0.0984 0.055 Uiso 1 1 calc R . . C7 C 0.3908(13) -0.2755(11) 0.1130(9) 0.041(3) Uani 1 1 d . . . C8 C 0.5171(15) -0.2257(16) 0.1060(11) 0.055(4) Uani 1 1 d . . . H8 H 0.5469 -0.1881 0.0506 0.066 Uiso 1 1 calc R . . C9 C 0.6042(19) -0.228(2) 0.1772(16) 0.078(6) Uani 1 1 d . . . H9 H 0.6902 -0.1888 0.1725 0.094 Uiso 1 1 calc R . . C10 C 0.554(2) -0.293(2) 0.2570(14) 0.087(7) Uani 1 1 d . . . H10 H 0.6101 -0.2980 0.3058 0.104 Uiso 1 1 calc R . . C11 C 0.427(2) -0.349(2) 0.2663(14) 0.085(7) Uani 1 1 d . . . H11 H 0.3969 -0.3924 0.3197 0.103 Uiso 1 1 calc R . . C12 C 0.3456(18) -0.3394(17) 0.1941(11) 0.065(5) Uani 1 1 d . . . H12 H 0.2592 -0.3757 0.1991 0.078 Uiso 1 1 calc R . . C13 C 0.3458(13) -0.2559(13) -0.0630(10) 0.042(3) Uani 1 1 d . . . C14 C 0.3992(15) -0.3501(18) -0.0967(11) 0.062(5) Uani 1 1 d . . . H14 H 0.4084 -0.4136 -0.0587 0.074 Uiso 1 1 calc R . . C15 C 0.4377(16) -0.344(2) -0.1894(13) 0.076(6) Uani 1 1 d . . . H15 H 0.4700 -0.4088 -0.2096 0.092 Uiso 1 1 calc R . . C16 C 0.436(3) -0.266(2) -0.2504(11) 0.145(16) Uani 1 1 d . . . H16 H 0.4678 -0.2690 -0.3104 0.174 Uiso 1 1 calc R . . C17 C 0.3765(18) -0.164(2) -0.2143(12) 0.070(5) Uani 1 1 d . . . H17 H 0.3687 -0.1011 -0.2536 0.084 Uiso 1 1 calc R . . C18 C 0.3333(15) -0.1651(16) -0.1212(10) 0.054(4) Uani 1 1 d . . . H18 H 0.2962 -0.1039 -0.0997 0.065 Uiso 1 1 calc R . . C19 C -0.0255(14) 0.6899(12) 0.3365(9) 0.040(3) Uani 1 1 d . . . C20 C -0.0059(12) 0.5695(10) 0.2950(8) 0.033(2) Uani 1 1 d . . . C21 C -0.0504(12) 0.5195(12) 0.2065(10) 0.041(3) Uani 1 1 d . . . H21 H -0.1008 0.5575 0.1713 0.049 Uiso 1 1 calc R . . C22 C -0.0219(15) 0.4155(13) 0.1696(10) 0.047(3) Uani 1 1 d . . . H22 H -0.0508 0.3879 0.1088 0.057 Uiso 1 1 calc R . . C23 C 0.0867(15) 0.3971(13) 0.3033(9) 0.048(3) Uani 1 1 d . . . H23 H 0.1326 0.3538 0.3378 0.058 Uiso 1 1 calc R . . C24 C 0.0652(14) 0.5035(12) 0.3442(9) 0.046(3) Uani 1 1 d . . . H24 H 0.0979 0.5310 0.4041 0.055 Uiso 1 1 calc R . . C25 C -0.1357(12) 0.6628(13) 0.4073(8) 0.036(3) Uani 1 1 d . . . C26 C -0.2155(14) 0.5438(15) 0.4203(11) 0.053(4) Uani 1 1 d . . . H26 H -0.2010 0.4754 0.3879 0.064 Uiso 1 1 calc R . . C27 C -0.3139(16) 0.527(2) 0.4799(15) 0.078(6) Uani 1 1 d . . . H27 H -0.3647 0.4470 0.4887 0.093 Uiso 1 1 calc R . . C28 C -0.3396(17) 0.628(3) 0.5279(15) 0.087(7) Uani 1 1 d . . . H28 H -0.4071 0.6165 0.5683 0.105 Uiso 1 1 calc R . . C29 C -0.2613(17) 0.745(2) 0.5134(11) 0.069(5) Uani 1 1 d . . . H29 H -0.2773 0.8137 0.5444 0.082 Uiso 1 1 calc R . . C30 C -0.1595(15) 0.7633(17) 0.4537(11) 0.057(4) Uani 1 1 d . . . H30 H -0.1079 0.8431 0.4455 0.068 Uiso 1 1 calc R . . C31 C 0.0978(13) 0.7673(13) 0.3830(10) 0.045(3) Uani 1 1 d . . . C32 C 0.1869(16) 0.8403(16) 0.3292(16) 0.070(5) Uani 1 1 d . . . H32 H 0.1677 0.8475 0.2662 0.085 Uiso 1 1 calc R . . C33 C 0.304(2) 0.904(3) 0.365(2) 0.119(11) Uani 1 1 d . . . H33 H 0.3651 0.9525 0.3275 0.143 Uiso 1 1 calc R . . C34 C 0.329(2) 0.892(3) 0.460(2) 0.124(11) Uani 1 1 d . . . H34 H 0.4079 0.9343 0.4853 0.149 Uiso 1 1 calc R . . C35 C 0.243(2) 0.821(2) 0.5176(18) 0.096(8) Uani 1 1 d . . . H35 H 0.2625 0.8155 0.5809 0.115 Uiso 1 1 calc R . . C36 C 0.1259(16) 0.7578(18) 0.4781(11) 0.062(4) Uani 1 1 d . . . H36 H 0.0653 0.7083 0.5155 0.074 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 0.0455(6) 0.0245(5) 0.0425(6) -0.0008(4) 0.0023(4) 0.0147(4) I1 0.0979(9) 0.0363(6) 0.0674(7) 0.0107(5) 0.0350(6) 0.0262(5) I2 0.0553(6) 0.0344(5) 0.0686(7) 0.0098(4) 0.0167(5) 0.0165(4) N1 0.039(6) 0.028(5) 0.048(6) -0.001(4) -0.006(5) 0.013(4) N2 0.042(6) 0.032(6) 0.042(6) -0.009(4) 0.001(5) 0.013(5) O1 0.046(5) 0.028(5) 0.066(7) -0.001(4) 0.008(5) 0.016(4) O2 0.078(7) 0.033(5) 0.035(5) -0.002(4) 0.004(5) 0.024(5) C1 0.037(7) 0.032(6) 0.038(7) -0.003(5) -0.001(5) 0.006(5) C2 0.043(7) 0.041(7) 0.026(6) -0.001(5) 0.009(5) 0.012(5) C3 0.041(7) 0.027(6) 0.047(7) -0.004(5) 0.007(6) 0.010(5) C4 0.032(6) 0.022(6) 0.051(7) -0.005(5) 0.000(5) 0.011(5) C5 0.042(8) 0.031(7) 0.069(10) -0.003(6) 0.001(7) 0.004(6) C6 0.046(8) 0.037(7) 0.057(8) 0.010(6) -0.001(6) 0.017(6) C7 0.052(8) 0.029(6) 0.045(7) -0.003(5) 0.001(6) 0.018(6) C8 0.056(9) 0.063(10) 0.050(9) 0.004(7) 0.008(7) 0.024(8) C9 0.065(12) 0.085(14) 0.090(15) -0.023(12) -0.019(10) 0.035(10) C10 0.13(2) 0.099(16) 0.053(11) -0.003(11) -0.023(12) 0.064(15) C11 0.083(14) 0.129(19) 0.058(11) 0.044(12) -0.005(10) 0.048(13) C12 0.083(12) 0.073(11) 0.044(9) 0.018(8) 0.002(8) 0.030(10) C13 0.039(7) 0.039(7) 0.046(8) -0.009(6) 0.000(6) 0.006(6) C14 0.051(9) 0.095(13) 0.051(9) 0.041(9) 0.011(7) 0.033(9) C15 0.057(10) 0.103(15) 0.066(11) -0.037(11) 0.027(9) 0.018(10) C16 0.21(3) 0.12(2) 0.019(8) 0.035(10) -0.042(12) -0.11(2) C17 0.071(12) 0.093(14) 0.044(9) -0.009(9) -0.017(8) 0.021(10) C18 0.056(9) 0.071(11) 0.043(8) -0.004(7) -0.008(7) 0.034(8) C19 0.064(9) 0.033(7) 0.029(6) 0.004(5) 0.000(6) 0.021(6) C20 0.041(7) 0.023(6) 0.035(6) -0.004(5) 0.002(5) 0.009(5) C21 0.042(7) 0.034(7) 0.048(8) -0.001(6) -0.003(6) 0.013(6) C22 0.070(10) 0.042(8) 0.036(7) 0.001(6) -0.010(6) 0.028(7) C23 0.074(10) 0.038(7) 0.039(7) 0.000(6) -0.008(7) 0.028(7) C24 0.071(10) 0.037(7) 0.031(7) -0.006(5) -0.011(6) 0.020(7) C25 0.038(7) 0.046(7) 0.028(6) 0.003(5) -0.001(5) 0.021(6) C26 0.046(8) 0.052(9) 0.060(9) -0.002(7) 0.000(7) 0.009(7) C27 0.043(9) 0.090(15) 0.087(14) 0.012(11) 0.003(9) -0.005(9) C28 0.044(10) 0.15(2) 0.074(13) 0.007(14) 0.017(9) 0.028(12) C29 0.061(10) 0.110(16) 0.046(9) 0.005(9) 0.019(8) 0.042(11) C30 0.049(9) 0.068(11) 0.058(9) 0.000(8) 0.014(7) 0.024(8) C31 0.043(8) 0.040(7) 0.050(8) -0.012(6) 0.005(6) 0.009(6) C32 0.051(10) 0.052(10) 0.104(15) -0.001(9) 0.015(10) 0.005(8) C33 0.064(14) 0.16(3) 0.101(19) -0.008(18) 0.018(13) -0.030(15) C34 0.065(15) 0.13(2) 0.14(3) -0.06(2) -0.010(16) -0.023(15) C35 0.094(17) 0.098(18) 0.090(16) -0.037(14) -0.038(14) 0.023(14) C36 0.056(10) 0.085(13) 0.040(8) -0.011(8) -0.006(7) 0.015(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 Pd N2 2.020(10) . ? Pd N1 2.037(10) . ? Pd I1 2.6060(14) . ? Pd I2 2.6115(13) . ? N1 C5 1.355(17) . ? N1 C4 1.351(15) . ? N2 C22 1.322(17) . ? N2 C23 1.349(17) . ? O1 C1 1.425(15) . ? O2 C19 1.429(15) . ? C1 C2 1.528(17) . ? C1 C7 1.544(18) . ? C1 C13 1.556(19) . ? C2 C6 1.381(19) . ? C2 C3 1.397(18) . ? C3 C4 1.385(16) . ? C5 C6 1.397(18) . ? C7 C8 1.35(2) . ? C7 C12 1.41(2) . ? C8 C9 1.38(2) . ? C9 C10 1.41(3) . ? C10 C11 1.38(3) . ? C11 C12 1.37(2) . ? C13 C18 1.36(2) . ? C13 C14 1.41(2) . ? C14 C15 1.39(2) . ? C15 C16 1.25(3) . ? C16 C17 1.54(4) . ? C17 C18 1.42(2) . ? C19 C31 1.521(19) . ? C19 C20 1.520(16) . ? C19 C25 1.560(18) . ? C20 C21 1.387(17) . ? C20 C24 1.400(18) . ? C21 C22 1.371(18) . ? C23 C24 1.383(18) . ? C25 C30 1.37(2) . ? C25 C26 1.40(2) . ? C26 C27 1.36(2) . ? C27 C28 1.39(3) . ? C28 C29 1.38(3) . ? C29 C30 1.39(2) . ? C31 C32 1.36(2) . ? C31 C36 1.40(2) . ? C32 C33 1.37(3) . ? C33 C34 1.39(4) . ? C34 C35 1.36(4) . ? C35 C36 1.39(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 N2 Pd N1 175.7(4) . . ? N2 Pd I1 88.5(3) . . ? N1 Pd I1 91.2(3) . . ? N2 Pd I2 91.3(3) . . ? N1 Pd I2 89.2(3) . . ? I1 Pd I2 176.80(5) . . ? C5 N1 C4 118.1(10) . . ? C5 N1 Pd 118.6(9) . . ? C4 N1 Pd 123.3(8) . . ? C22 N2 C23 116.5(11) . . ? C22 N2 Pd 125.1(9) . . ? C23 N2 Pd 118.3(9) . . ? O1 C1 C2 104.8(10) . . ? O1 C1 C7 109.8(10) . . ? C2 C1 C7 108.5(10) . . ? O1 C1 C13 108.5(10) . . ? C2 C1 C13 112.6(11) . . ? C7 C1 C13 112.3(11) . . ? C6 C2 C3 118.6(12) . . ? C6 C2 C1 121.3(11) . . ? C3 C2 C1 120.0(11) . . ? C4 C3 C2 118.8(12) . . ? N1 C4 C3 123.0(11) . . ? N1 C5 C6 121.7(12) . . ? C2 C6 C5 119.7(13) . . ? C8 C7 C12 118.6(14) . . ? C8 C7 C1 123.6(13) . . ? C12 C7 C1 117.8(13) . . ? C7 C8 C9 123.4(17) . . ? C8 C9 C10 116(2) . . ? C11 C10 C9 123.2(18) . . ? C12 C11 C10 117.7(18) . . ? C11 C12 C7 121.2(18) . . ? C18 C13 C14 119.6(14) . . ? C18 C13 C1 120.7(12) . . ? C14 C13 C1 119.4(13) . . ? C15 C14 C13 116.9(16) . . ? C16 C15 C14 131(2) . . ? C15 C16 C17 112(2) . . ? C18 C17 C16 120.1(17) . . ? C13 C18 C17 120.1(16) . . ? O2 C19 C31 111.5(11) . . ? O2 C19 C20 105.1(10) . . ? C31 C19 C20 109.4(11) . . ? O2 C19 C25 108.3(11) . . ? C31 C19 C25 111.5(10) . . ? C20 C19 C25 110.9(11) . . ? C21 C20 C24 115.2(11) . . ? C21 C20 C19 124.1(11) . . ? C24 C20 C19 120.7(11) . . ? C22 C21 C20 121.7(12) . . ? N2 C22 C21 123.2(12) . . ? N2 C23 C24 123.7(12) . . ? C23 C24 C20 119.7(12) . . ? C30 C25 C26 119.2(13) . . ? C30 C25 C19 117.1(13) . . ? C26 C25 C19 123.6(12) . . ? C27 C26 C25 120.7(16) . . ? C26 C27 C28 121.0(19) . . ? C29 C28 C27 117.7(17) . . ? C28 C29 C30 121.8(18) . . ? C25 C30 C29 119.5(17) . . ? C32 C31 C36 119.0(15) . . ? C32 C31 C19 119.1(15) . . ? C36 C31 C19 121.7(13) . . ? C31 C32 C33 122(2) . . ? C34 C33 C32 117(2) . . ? C33 C34 C35 124(2) . . ? C34 C35 C36 117(2) . . ? C35 C36 C31 120.9(19) . . ? 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 O1 H1 I2 0.82 2.87 3.519(9) 138.1 1_545 O2 H2 I1 0.82 2.85 3.533(9) 142.4 1_565 _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 7.371 _refine_diff_density_min -1.386 _refine_diff_density_rms 0.361