# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Bernhard Lippert' _publ_contact_author_email BERNHARD.LIPPERT@TU-DORTMUND.DE _publ_section_title ; Hybrids between classical and metallacalix[4]arenes based on uracil and cis-PtIIL2 entities (L = P(Ph)3 or L2 = 2,2'-bipyridine) ; loop_ _publ_author_name 'B Lippert' 'Neeladri Das' 'Anupam Khutia' 'Martina Lazar' 'Pablo J. Sanz Miguel' # Attachment 'CCDC_735159_revised.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-10-15 at 15:55:22 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : 1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_1 _database_code_depnum_ccdc_archive 'CCDC 735159' _audit_creation_date 2008-10-15T15:55:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C11 H12 N4 O4, H2 O' _chemical_formula_sum 'C11 H14 N4 O5' _chemical_formula_weight 282.26 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 7.6960(15) _cell_length_b 8.3560(17) _cell_length_c 10.801(2) _cell_angle_alpha 101.54(3) _cell_angle_beta 90.19(3) _cell_angle_gamma 112.92(3) _cell_volume 624.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8484 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.988 _exptl_absorpt_correction_T_max 0.988 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'profile fitled' _diffrn_standards_number N/A _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_unetI/netI 0.1429 _diffrn_reflns_number 8484 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 2832 _reflns_number_gt 1162 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. DFIX and DANG restrains were used to fix the proton atoms on the water molecules. ; _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^)+(0.0701P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2832 _refine_ls_number_parameters 191 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.2041 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1572 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.96 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.216 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.048 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1A N 0.5766(3) 0.2783(3) 0.5052(2) 0.0437(7) Uani 1 1 d . . . C1A C 0.7733(5) 0.3441(5) 0.5588(3) 0.0657(11) Uani 1 1 d . . . H11 H 0.8168 0.4684 0.5979 0.099 Uiso 1 1 calc R . . H12 H 0.8515 0.328 0.4924 0.099 Uiso 1 1 calc R . . H13 H 0.7805 0.2792 0.6212 0.099 Uiso 1 1 calc R . . C2A C 0.4365(5) 0.1749(4) 0.5671(3) 0.0426(8) Uani 1 1 d . . . O2A O 0.4652(3) 0.1342(3) 0.6650(2) 0.0649(8) Uani 1 1 d . . . N3A N 0.2567(3) 0.1181(3) 0.5093(2) 0.0422(7) Uani 1 1 d . . . H31 H 0.1656 0.0549 0.5474 0.051 Uiso 1 1 calc R . . C4A C 0.2056(5) 0.1506(4) 0.3976(3) 0.0356(8) Uani 1 1 d . . . O4A O 0.0364(3) 0.0939(3) 0.35930(17) 0.0454(6) Uani 1 1 d . . . C5A C 0.3618(4) 0.2509(4) 0.3340(2) 0.0343(8) Uani 1 1 d . . . C6A C 0.5364(5) 0.3104(4) 0.3915(3) 0.0431(8) Uani 1 1 d . . . H61 H 0.6371 0.378 0.3515 0.052 Uiso 1 1 calc R . . C5 C 0.3255(4) 0.2781(4) 0.2048(2) 0.0405(8) Uani 1 1 d . . . H51 H 0.4349 0.3759 0.1871 0.049 Uiso 1 1 calc R . . H52 H 0.2181 0.3115 0.2048 0.049 Uiso 1 1 calc R . . C1B C 0.2801(5) -0.3414(4) 0.0494(3) 0.0489(9) Uani 1 1 d . . . H14 H 0.1576 -0.4252 0.0618 0.073 Uiso 1 1 calc R . . H15 H 0.3639 -0.3078 0.1248 0.073 Uiso 1 1 calc R . . H16 H 0.3302 -0.395 -0.0207 0.073 Uiso 1 1 calc R . . N1B N 0.2629(3) -0.1822(3) 0.0220(2) 0.0369(7) Uani 1 1 d . . . C2B C 0.1911(4) -0.1923(4) -0.0967(3) 0.0386(8) Uani 1 1 d . . . O2B O 0.1437(3) -0.3251(3) -0.18262(19) 0.0549(7) Uani 1 1 d . . . N3B N 0.1778(3) -0.0390(3) -0.1142(2) 0.0401(7) Uani 1 1 d . . . H32 H 0.1404 -0.0395 -0.1894 0.048 Uiso 1 1 calc R . . C4B C 0.2180(4) 0.1159(4) -0.0236(3) 0.0363(8) Uani 1 1 d . . . O4B O 0.1926(3) 0.2419(3) -0.05112(18) 0.0541(7) Uani 1 1 d . . . C5B C 0.2860(4) 0.1151(4) 0.1004(2) 0.0336(8) Uani 1 1 d . . . C6B C 0.3051(4) -0.0320(4) 0.1163(3) 0.0330(8) Uani 1 1 d . . . H62 H 0.3497 -0.0328 0.1963 0.04 Uiso 1 1 calc R . . O1W O 0.1158(5) -0.6673(4) -0.2789(3) 0.1008(12) Uani 1 1 d D . . H1W H 0.126(9) -0.715(7) -0.212(4) 0.21(3) Uiso 1 1 d D . . H2W H 0.115(8) -0.560(5) -0.236(4) 0.18(3) 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 N1A 0.0373(17) 0.0557(19) 0.0323(15) 0.0058(13) -0.0008(13) 0.0142(15) C1A 0.043(2) 0.083(3) 0.058(2) 0.009(2) -0.0068(18) 0.014(2) C2A 0.042(2) 0.055(2) 0.0343(19) 0.0087(16) 0.0006(17) 0.0236(19) O2A 0.0593(17) 0.097(2) 0.0455(15) 0.0301(14) -0.0052(12) 0.0320(15) N3A 0.0387(16) 0.0597(18) 0.0293(14) 0.0178(12) 0.0053(12) 0.0168(14) C4A 0.045(2) 0.038(2) 0.0258(17) 0.0062(14) 0.0039(16) 0.0186(17) O4A 0.0363(14) 0.0628(16) 0.0349(13) 0.0167(11) -0.0002(10) 0.0147(12) C5A 0.042(2) 0.0329(18) 0.0243(16) 0.0043(13) 0.0021(15) 0.0116(15) C6A 0.047(2) 0.043(2) 0.0334(18) 0.0061(15) 0.0072(16) 0.0123(17) C5 0.052(2) 0.037(2) 0.0303(17) 0.0084(15) 0.0057(15) 0.0153(17) C1B 0.064(2) 0.047(2) 0.046(2) 0.0133(17) -0.0002(17) 0.0302(19) N1B 0.0481(17) 0.0385(17) 0.0325(14) 0.0116(13) 0.0032(12) 0.0241(14) C2B 0.043(2) 0.046(2) 0.0315(18) 0.0107(17) 0.0057(15) 0.0218(17) O2B 0.0841(18) 0.0474(16) 0.0360(13) -0.0015(12) -0.0042(12) 0.0345(13) N3B 0.0604(19) 0.0445(18) 0.0218(13) 0.0104(13) 0.0009(12) 0.0261(14) C4B 0.042(2) 0.039(2) 0.0307(17) 0.0091(16) 0.0060(14) 0.0180(16) O4B 0.0906(19) 0.0463(15) 0.0378(13) 0.0143(11) -0.0014(12) 0.0380(14) C5B 0.0392(19) 0.038(2) 0.0258(17) 0.0118(14) 0.0059(13) 0.0152(15) C6B 0.0352(18) 0.037(2) 0.0262(16) 0.0087(15) 0.0030(14) 0.0124(15) O1W 0.187(4) 0.082(2) 0.0554(18) 0.0019(17) -0.016(2) 0.082(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N1A C2A 1.366(4) . ? N1A C6A 1.367(3) . ? N1A C1A 1.465(4) . ? C1A H11 0.96 . ? C1A H12 0.96 . ? C1A H13 0.96 . ? C2A O2A 1.218(3) . ? C2A N3A 1.376(3) . ? N3A C4A 1.377(3) . ? N3A H31 0.86 . ? C4A O4A 1.237(3) . ? C4A C5A 1.439(4) . ? C5A C6A 1.338(4) . ? C5A C5 1.500(3) . ? C6A H61 0.93 . ? C5 C5B 1.510(4) . ? C5 H51 0.97 . ? C5 H52 0.97 . ? C1B N1B 1.473(3) . ? C1B H14 0.96 . ? C1B H15 0.96 . ? C1B H16 0.96 . ? N1B C2B 1.368(3) . ? N1B C6B 1.374(4) . ? C2B O2B 1.223(3) . ? C2B N3B 1.373(4) . ? N3B C4B 1.381(4) . ? N3B H32 0.86 . ? C4B O4B 1.233(3) . ? C4B C5B 1.439(4) . ? C5B C6B 1.337(4) . ? C6B H62 0.93 . ? O1W H1W 0.91(2) . ? O1W H2W 0.93(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 C2A N1A C6A 121.0(3) . . ? C2A N1A C1A 118.5(2) . . ? C6A N1A C1A 120.4(3) . . ? N1A C1A H11 109.5 . . ? N1A C1A H12 109.5 . . ? H11 C1A H12 109.5 . . ? N1A C1A H13 109.5 . . ? H11 C1A H13 109.5 . . ? H12 C1A H13 109.5 . . ? O2A C2A N1A 123.8(3) . . ? O2A C2A N3A 121.8(3) . . ? N1A C2A N3A 114.4(3) . . ? C2A N3A C4A 127.6(3) . . ? C2A N3A H31 116.2 . . ? C4A N3A H31 116.2 . . ? O4A C4A N3A 119.9(3) . . ? O4A C4A C5A 125.3(2) . . ? N3A C4A C5A 114.7(3) . . ? C6A C5A C4A 117.8(3) . . ? C6A C5A C5 122.5(3) . . ? C4A C5A C5 119.7(3) . . ? C5A C6A N1A 124.3(3) . . ? C5A C6A H61 117.8 . . ? N1A C6A H61 117.8 . . ? C5A C5 C5B 113.3(2) . . ? C5A C5 H51 108.9 . . ? C5B C5 H51 108.9 . . ? C5A C5 H52 108.9 . . ? C5B C5 H52 108.9 . . ? H51 C5 H52 107.7 . . ? N1B C1B H14 109.5 . . ? N1B C1B H15 109.5 . . ? H14 C1B H15 109.5 . . ? N1B C1B H16 109.5 . . ? H14 C1B H16 109.5 . . ? H15 C1B H16 109.5 . . ? C2B N1B C6B 121.0(2) . . ? C2B N1B C1B 118.4(2) . . ? C6B N1B C1B 120.5(2) . . ? O2B C2B N1B 123.8(3) . . ? O2B C2B N3B 121.4(3) . . ? N1B C2B N3B 114.8(3) . . ? C2B N3B C4B 126.9(2) . . ? C2B N3B H32 116.6 . . ? C4B N3B H32 116.6 . . ? O4B C4B N3B 120.2(3) . . ? O4B C4B C5B 124.4(3) . . ? N3B C4B C5B 115.4(3) . . ? C6B C5B C4B 117.7(3) . . ? C6B C5B C5 124.4(2) . . ? C4B C5B C5 117.9(2) . . ? C5B C6B N1B 124.1(2) . . ? C5B C6B H62 117.9 . . ? N1B C6B H62 117.9 . . ? H1W O1W H2W 100(4) . . ? 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 C6A N1A C2A O2A 175.9(3) . . . . ? C1A N1A C2A O2A 0.2(5) . . . . ? C6A N1A C2A N3A -3.7(4) . . . . ? C1A N1A C2A N3A -179.5(3) . . . . ? O2A C2A N3A C4A -178.2(3) . . . . ? N1A C2A N3A C4A 1.5(4) . . . . ? C2A N3A C4A O4A -178.1(3) . . . . ? C2A N3A C4A C5A 2.2(4) . . . . ? O4A C4A C5A C6A 176.6(3) . . . . ? N3A C4A C5A C6A -3.7(4) . . . . ? O4A C4A C5A C5 -6.1(5) . . . . ? N3A C4A C5A C5 173.6(2) . . . . ? C4A C5A C6A N1A 1.7(5) . . . . ? C5 C5A C6A N1A -175.5(3) . . . . ? C2A N1A C6A C5A 2.3(5) . . . . ? C1A N1A C6A C5A 177.9(3) . . . . ? C6A C5A C5 C5B 101.0(3) . . . . ? C4A C5A C5 C5B -76.1(4) . . . . ? C6B N1B C2B O2B -176.8(3) . . . . ? C1B N1B C2B O2B -1.5(5) . . . . ? C6B N1B C2B N3B 4.0(4) . . . . ? C1B N1B C2B N3B 179.3(3) . . . . ? O2B C2B N3B C4B 176.7(3) . . . . ? N1B C2B N3B C4B -4.1(4) . . . . ? C2B N3B C4B O4B -177.1(3) . . . . ? C2B N3B C4B C5B 1.9(4) . . . . ? O4B C4B C5B C6B 179.4(3) . . . . ? N3B C4B C5B C6B 0.5(4) . . . . ? O4B C4B C5B C5 1.2(4) . . . . ? N3B C4B C5B C5 -177.8(3) . . . . ? C5A C5 C5B C6B -8.4(4) . . . . ? C5A C5 C5B C4B 169.7(3) . . . . ? C4B C5B C6B N1B -0.4(4) . . . . ? C5 C5B C6B N1B 177.8(3) . . . . ? C2B N1B C6B C5B -2.1(4) . . . . ? C1B N1B C6B C5B -177.3(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 O1W H2W O2B 0.93(2) 1.85(2) 2.763(4) 166(5) . # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'CCDC_735160_revised.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-18 at 10:42:06 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : 1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_2 _database_code_depnum_ccdc_archive 'CCDC 735160' _audit_creation_date 2009-05-18T10:42:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C94 H80 N8 O8 P4 Pt2, 4(H2O)' _chemical_formula_sum 'C94 H88 N8 O12 P4 Pt2' _chemical_formula_weight 2035.78 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.0455(5) _cell_length_b 21.4205(7) _cell_length_c 28.9487(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 9329.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12995 _cell_measurement_theta_min 2.0266 _cell_measurement_theta_max 29.0824 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cubes _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.490 _exptl_absorpt_correction_T_max 0.535 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_unetI/netI 0.0926 _diffrn_reflns_number 41126 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 29.07 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.865 _reflns_number_total 10815 _reflns_number_gt 6222 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. No SQUEEZE was used for this structure. Voids can be due to the large cavity within diuracil boxes in the structure (no residual density was found there). ; _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^)+(0.1007P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10815 _refine_ls_number_parameters 530 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.063 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1737 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.318 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.181 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pt1 Pt 0.70147(2) 0.405844(14) 0.134495(10) 0.02861(12) Uani 1 1 d . . . N1A N 0.7164(6) 0.3363(4) 0.2710(3) 0.057(2) Uani 1 1 d . . . C1A C 0.7763(9) 0.3472(6) 0.3097(4) 0.092(5) Uani 1 1 d . . . H1AA H 0.8262 0.3732 0.2996 0.138 Uiso 1 1 calc R . . H1AB H 0.7988 0.3072 0.3212 0.138 Uiso 1 1 calc R . . H1AC H 0.7441 0.3686 0.3345 0.138 Uiso 1 1 calc R . . C2A C 0.7375(7) 0.3631(5) 0.2285(3) 0.044(2) Uani 1 1 d . . . O2A O 0.8069(4) 0.3912(3) 0.2226(2) 0.0491(17) Uani 1 1 d . . . N3A N 0.6751(4) 0.3536(3) 0.1937(2) 0.0311(16) Uani 1 1 d . . . C4A C 0.6015(6) 0.3192(4) 0.1976(3) 0.034(2) Uani 1 1 d . . . O4A O 0.5516(4) 0.3106(3) 0.16472(19) 0.0391(14) Uani 1 1 d . . . C5A C 0.5819(6) 0.2922(4) 0.2430(3) 0.039(2) Uani 1 1 d . . . C51A C 0.5 0.2540(5) 0.25 0.042(3) Uani 1 2 d S . . H5A H 0.5074 0.2276 0.2765 0.05 Uiso 1 1 d R . . C6A C 0.6411(7) 0.3012(5) 0.2765(3) 0.053(3) Uani 1 1 d . . . H6AA H 0.6306 0.2824 0.3057 0.063 Uiso 1 1 calc R . . N1B N 0.4377(5) 0.4723(5) 0.1401(3) 0.062(3) Uani 1 1 d . . . C1B C 0.3569(7) 0.4622(7) 0.1091(4) 0.095(5) Uani 1 1 d . . . H1BA H 0.3736 0.4358 0.0829 0.143 Uiso 1 1 calc R . . H1BB H 0.3356 0.5026 0.0977 0.143 Uiso 1 1 calc R . . H1BC H 0.3097 0.4418 0.1268 0.143 Uiso 1 1 calc R . . C2B C 0.5171(6) 0.4455(4) 0.1252(3) 0.042(2) Uani 1 1 d . . . O2B O 0.5198(4) 0.4172(3) 0.0890(2) 0.0466(16) Uani 1 1 d . . . N3B N 0.5899(5) 0.4561(3) 0.1532(2) 0.0341(16) Uani 1 1 d . . . C4B C 0.5901(7) 0.4903(4) 0.1939(4) 0.044(2) Uani 1 1 d . . . O4B O 0.6590(5) 0.4999(3) 0.2141(2) 0.0484(17) Uani 1 1 d . . . C5B C 0.5073(8) 0.5176(4) 0.2075(4) 0.055(3) Uani 1 1 d . . . C51B C 0.5 0.5567(6) 0.25 0.070(5) Uani 1 2 d S . . H51A H 0.4485 0.5832 0.2495 0.084 Uiso 1 1 d R . . C6B C 0.4380(8) 0.5084(5) 0.1823(5) 0.072(4) Uani 1 1 d . . . H6BA H 0.3836 0.5266 0.1921 0.087 Uiso 1 1 calc R . . P1 P 0.73652(14) 0.48026(10) 0.08170(7) 0.0295(5) Uani 1 1 d . . . C11 C 0.8216(5) 0.5316(4) 0.1050(3) 0.034(2) Uani 1 1 d . . . C12 C 0.8470(7) 0.5840(4) 0.0805(3) 0.047(3) Uani 1 1 d . . . H12A H 0.8196 0.5933 0.0517 0.057 Uiso 1 1 calc R . . C13 C 0.9130(7) 0.6235(5) 0.0980(3) 0.047(2) Uani 1 1 d . . . H13A H 0.929 0.6604 0.0818 0.056 Uiso 1 1 calc R . . C14 C 0.9550(7) 0.6085(4) 0.1394(4) 0.054(3) Uani 1 1 d . . . H14A H 1.0015 0.6344 0.1505 0.065 Uiso 1 1 calc R . . C15 C 0.9301(7) 0.5559(5) 0.1649(4) 0.057(3) Uani 1 1 d . . . H15A H 0.9587 0.5454 0.1931 0.068 Uiso 1 1 calc R . . C16 C 0.8607(6) 0.5191(4) 0.1469(3) 0.035(2) Uani 1 1 d . . . H16A H 0.8401 0.4844 0.1644 0.042 Uiso 1 1 calc R . . C21 C 0.6497(5) 0.5379(4) 0.0701(3) 0.0324(19) Uani 1 1 d . . . C22 C 0.6046(6) 0.5412(4) 0.0285(3) 0.039(2) Uani 1 1 d . . . H22A H 0.6196 0.5139 0.0039 0.047 Uiso 1 1 calc R . . C23 C 0.5347(7) 0.5864(4) 0.0231(4) 0.057(3) Uani 1 1 d . . . H23A H 0.504 0.589 -0.0055 0.068 Uiso 1 1 calc R . . C24 C 0.5116(6) 0.6253(5) 0.0578(4) 0.054(3) Uani 1 1 d . . . H24A H 0.4642 0.6542 0.0539 0.065 Uiso 1 1 calc R . . C25 C 0.5596(6) 0.6223(4) 0.1005(4) 0.048(2) Uani 1 1 d . . . H25A H 0.5453 0.6497 0.1252 0.058 Uiso 1 1 calc R . . C26 C 0.6273(6) 0.5786(4) 0.1054(3) 0.037(2) Uani 1 1 d . . . H26A H 0.6591 0.5766 0.1337 0.044 Uiso 1 1 calc R . . C31 C 0.7744(5) 0.4551(4) 0.0253(3) 0.035(2) Uani 1 1 d . . . C32 C 0.7193(6) 0.4181(4) -0.0001(3) 0.037(2) Uani 1 1 d . . . H32A H 0.6626 0.4076 0.0121 0.045 Uiso 1 1 calc R . . C33 C 0.7436(9) 0.3947(6) -0.0441(5) 0.085(3) Uani 1 1 d . . . H33A H 0.704 0.3693 -0.0614 0.102 Uiso 1 1 calc R . . C34 C 0.8299(8) 0.4106(5) -0.0620(4) 0.060(3) Uani 1 1 d . . . H34A H 0.8488 0.395 -0.0912 0.072 Uiso 1 1 calc R . . C35 C 0.8844(7) 0.4484(5) -0.0366(4) 0.061(3) Uani 1 1 d . . . H35A H 0.9409 0.4602 -0.0484 0.074 Uiso 1 1 calc R . . C36 C 0.8560(6) 0.4704(5) 0.0082(4) 0.055(3) Uani 1 1 d . . . H36A H 0.8947 0.4958 0.0259 0.066 Uiso 1 1 calc R . . P2 P 0.80207(15) 0.33336(11) 0.11287(9) 0.0374(5) Uani 1 1 d . . . C41 C 0.9127(6) 0.3602(4) 0.0982(3) 0.047(2) Uani 1 1 d . . . C42 C 0.9454(7) 0.3554(6) 0.0538(5) 0.077(4) Uani 1 1 d . . . H42A H 0.9111 0.3368 0.0299 0.093 Uiso 1 1 calc R . . C43 C 1.0283(11) 0.3781(6) 0.0453(5) 0.095(3) Uani 1 1 d . . . H43A H 1.0537 0.373 0.0155 0.114 Uiso 1 1 calc R . . C44 C 1.0783(8) 0.4097(6) 0.0810(6) 0.087(4) Uani 1 1 d . . . H44A H 1.1347 0.4274 0.0742 0.105 Uiso 1 1 calc R . . C45 C 1.0444(8) 0.4139(5) 0.1239(5) 0.068(3) Uani 1 1 d . . . H45A H 1.0764 0.4333 0.1483 0.081 Uiso 1 1 calc R . . C46 C 0.9610(7) 0.3888(5) 0.1308(4) 0.054(3) Uani 1 1 d . . . H46A H 0.936 0.392 0.1609 0.065 Uiso 1 1 calc R . . C51 C 0.7610(7) 0.2901(4) 0.0633(3) 0.043(2) Uani 1 1 d . . . C52 C 0.8141(9) 0.2436(5) 0.0420(4) 0.078(4) Uani 1 1 d . . . H52A H 0.8717 0.2359 0.0541 0.094 Uiso 1 1 calc R . . C53 C 0.7870(11) 0.2098(5) 0.0055(4) 0.087(4) Uani 1 1 d . . . H53A H 0.8259 0.1821 -0.0102 0.104 Uiso 1 1 calc R . . C54 C 0.7020(11) 0.2173(7) -0.0076(5) 0.095(3) Uani 1 1 d . . . H54A H 0.6814 0.1932 -0.033 0.114 Uiso 1 1 calc R . . C55 C 0.6395(9) 0.2596(5) 0.0142(4) 0.069(4) Uani 1 1 d . . . H55A H 0.5795 0.2634 0.0044 0.083 Uiso 1 1 calc R . . C56 C 0.6742(7) 0.2947(4) 0.0511(3) 0.047(2) Uani 1 1 d . . . H56 H 0.6363 0.3221 0.0677 0.056 Uiso 1 1 calc R . . C61 C 0.8153(6) 0.2671(4) 0.1532(4) 0.044(2) Uani 1 1 d . . . C62 C 0.7471(7) 0.2275(4) 0.1595(3) 0.048(2) Uani 1 1 d . . . H62A H 0.6943 0.2337 0.1421 0.058 Uiso 1 1 calc R . . C63 C 0.7503(9) 0.1785(5) 0.1899(4) 0.064(3) Uani 1 1 d . . . H63A H 0.701 0.1509 0.1917 0.077 Uiso 1 1 calc R . . C64 C 0.8184(9) 0.1685(6) 0.2164(6) 0.102(5) Uani 1 1 d . . . H64A H 0.8202 0.1341 0.2371 0.123 Uiso 1 1 calc R . . C65 C 0.8882(9) 0.2102(6) 0.2131(4) 0.085(3) Uani 1 1 d . . . H65A H 0.9376 0.2045 0.2332 0.102 Uiso 1 1 calc R . . C66 C 0.8907(9) 0.2607(5) 0.1817(5) 0.091(4) Uani 1 1 d . . . H66A H 0.9399 0.2884 0.1799 0.109 Uiso 1 1 calc R . . O1 O 0.9145(7) 0.4699(5) 0.2687(3) 0.032(3) Uiso 0.504(12) 1 d P A 1 O1' O 0.7870(9) 0.5364(7) 0.2821(5) 0.071(5) Uiso 0.496(12) 1 d P A 2 O2 O 0.4259(9) 0.2365(6) 0.1263(4) 0.026(5) Uiso 0.386(17) 1 d P B 1 O2' O 0.4095(11) 0.2626(8) 0.0905(6) 0.108(7) Uiso 0.614(17) 1 d P B 2 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 Pt1 0.03140(19) 0.02143(17) 0.03299(18) -0.00270(15) -0.00298(14) 0.00415(14) N1A 0.073(6) 0.058(6) 0.040(5) 0.006(4) -0.018(4) -0.018(5) C1A 0.121(11) 0.108(12) 0.048(7) 0.017(7) -0.031(7) -0.043(9) C2A 0.057(6) 0.044(6) 0.031(5) -0.010(4) -0.002(4) 0.001(5) O2A 0.058(5) 0.036(4) 0.053(4) 0.006(3) -0.013(3) -0.012(3) N3A 0.032(4) 0.032(4) 0.028(4) 0.001(3) -0.010(3) 0.004(3) C4A 0.042(5) 0.023(4) 0.039(5) -0.001(4) 0.005(4) 0.008(4) O4A 0.052(4) 0.030(3) 0.035(3) 0.003(3) -0.010(3) -0.008(3) C5A 0.051(6) 0.025(4) 0.040(5) 0.003(4) 0.005(4) 0.003(4) C51A 0.063(9) 0.023(6) 0.040(7) 0 0.004(6) 0 C6A 0.080(8) 0.042(6) 0.037(5) 0.002(5) -0.004(5) -0.001(6) N1B 0.044(5) 0.073(6) 0.070(6) 0.033(5) 0.008(4) 0.031(5) C1B 0.051(8) 0.141(14) 0.095(10) 0.019(10) 0.005(7) 0.030(8) C2B 0.040(6) 0.034(5) 0.053(6) 0.023(5) 0.010(4) 0.007(4) O2B 0.043(4) 0.045(4) 0.051(4) 0.013(3) -0.010(3) 0.004(3) N3B 0.044(4) 0.020(3) 0.038(4) 0.002(3) 0.005(3) 0.013(3) C4B 0.057(7) 0.019(4) 0.057(6) 0.018(4) 0.030(5) 0.009(4) O4B 0.067(5) 0.028(3) 0.050(4) -0.007(3) 0.015(4) -0.005(3) C5B 0.061(7) 0.032(5) 0.071(8) 0.008(5) 0.038(6) 0.011(5) C51B 0.110(14) 0.023(7) 0.077(11) 0 0.051(10) 0 C6B 0.070(9) 0.046(7) 0.100(11) 0.039(7) 0.054(8) 0.031(6) P1 0.0296(11) 0.0248(11) 0.0341(12) -0.0014(10) -0.0028(9) 0.0045(9) C11 0.036(5) 0.028(4) 0.038(5) -0.003(4) -0.006(4) -0.002(4) C12 0.058(7) 0.040(6) 0.044(6) -0.005(5) 0.024(5) -0.006(5) C13 0.057(6) 0.042(6) 0.041(5) 0.000(5) 0.003(5) 0.007(5) C14 0.047(6) 0.033(5) 0.081(8) -0.016(5) -0.012(5) -0.016(4) C15 0.061(7) 0.043(6) 0.066(7) -0.010(5) -0.029(5) 0.003(5) C16 0.041(5) 0.028(4) 0.035(5) -0.002(4) -0.006(4) -0.011(4) C21 0.033(5) 0.017(4) 0.047(5) 0.009(4) 0.001(4) -0.003(4) C22 0.046(5) 0.024(4) 0.048(5) 0.003(4) -0.006(4) -0.001(4) C23 0.047(6) 0.046(6) 0.076(8) 0.009(6) -0.024(5) 0.003(5) C24 0.036(6) 0.036(6) 0.090(9) 0.014(6) -0.005(6) 0.003(5) C25 0.049(6) 0.028(5) 0.067(7) -0.001(5) 0.013(5) 0.000(4) C26 0.049(6) 0.021(4) 0.040(5) 0.010(4) 0.002(4) -0.013(4) C31 0.034(5) 0.043(5) 0.029(4) 0.007(4) 0.006(3) 0.000(4) C32 0.045(6) 0.024(5) 0.043(5) -0.002(4) 0.009(4) 0.002(4) C33 0.081(7) 0.077(7) 0.095(7) 0.033(6) -0.036(6) 0.009(5) C34 0.069(7) 0.069(8) 0.043(6) -0.012(6) 0.017(5) -0.007(6) C35 0.057(7) 0.067(7) 0.061(7) -0.013(6) 0.020(6) -0.007(6) C36 0.047(6) 0.046(6) 0.072(7) -0.010(6) 0.005(5) -0.004(5) P2 0.0391(14) 0.0294(12) 0.0438(13) -0.0044(11) -0.0064(11) 0.0116(11) C41 0.050(6) 0.043(6) 0.048(6) 0.007(5) -0.005(5) 0.017(5) C42 0.037(7) 0.106(11) 0.089(10) 0.034(8) 0.011(6) 0.010(7) C43 0.142(10) 0.076(7) 0.066(6) -0.012(5) 0.002(7) 0.007(7) C44 0.046(7) 0.096(11) 0.120(12) 0.024(9) 0.007(7) 0.016(7) C45 0.052(7) 0.062(8) 0.089(9) -0.003(7) 0.000(6) 0.022(6) C46 0.041(6) 0.061(7) 0.059(7) -0.005(6) 0.004(5) 0.025(5) C51 0.062(6) 0.019(4) 0.048(6) -0.003(4) -0.005(5) 0.012(4) C52 0.138(12) 0.045(6) 0.053(7) -0.010(6) 0.000(7) 0.031(7) C53 0.152(14) 0.039(7) 0.069(8) -0.014(6) -0.006(9) 0.020(8) C54 0.142(10) 0.076(7) 0.066(6) -0.012(5) 0.002(7) 0.007(7) C55 0.109(10) 0.048(7) 0.052(7) 0.007(6) -0.029(6) -0.020(7) C56 0.076(7) 0.017(4) 0.048(6) 0.004(4) -0.009(5) -0.004(4) C61 0.045(6) 0.033(5) 0.055(6) 0.002(5) 0.010(4) 0.027(4) C62 0.059(7) 0.033(5) 0.053(6) 0.010(5) 0.004(5) 0.008(5) C63 0.091(9) 0.037(6) 0.064(7) 0.004(6) -0.007(7) 0.001(6) C64 0.087(11) 0.056(8) 0.165(15) 0.048(9) -0.042(10) -0.001(7) C65 0.081(7) 0.077(7) 0.095(7) 0.033(6) -0.036(6) 0.009(5) C66 0.084(9) 0.056(8) 0.134(12) 0.041(8) -0.038(9) 0.001(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pt1 N3B 2.067(6) . ? Pt1 N3A 2.084(7) . ? Pt1 P2 2.257(2) . ? Pt1 P1 2.270(2) . ? N1A C6A 1.369(12) . ? N1A C2A 1.393(12) . ? N1A C1A 1.458(12) . ? C1A H1AA 0.98 . ? C1A H1AB 0.98 . ? C1A H1AC 0.98 . ? C2A O2A 1.217(11) . ? C2A N3A 1.393(11) . ? N3A C4A 1.336(10) . ? C4A O4A 1.226(10) . ? C4A C5A 1.465(11) . ? C5A C6A 1.332(12) . ? C5A C51A 1.493(10) . ? C51A C5A 1.493(11) 3_655 ? C51A H5A 0.9599 . ? C6A H6AA 0.95 . ? N1B C2B 1.393(12) . ? N1B C6B 1.447(15) . ? N1B C1B 1.526(14) . ? C1B H1BA 0.98 . ? C1B H1BB 0.98 . ? C1B H1BC 0.98 . ? C2B O2B 1.212(11) . ? C2B N3B 1.382(12) . ? N3B C4B 1.386(12) . ? C4B O4B 1.208(11) . ? C4B C5B 1.431(13) . ? C5B C6B 1.286(15) . ? C5B C51B 1.493(12) . ? C51B C5B 1.493(12) 3_655 ? C51B H51A 0.96 . ? C6B H6BA 0.95 . ? P1 C31 1.812(8) . ? P1 C11 1.818(8) . ? P1 C21 1.829(8) . ? C11 C16 1.374(11) . ? C11 C12 1.383(12) . ? C12 C13 1.399(13) . ? C12 H12A 0.95 . ? C13 C14 1.393(13) . ? C13 H13A 0.95 . ? C14 C15 1.397(14) . ? C14 H14A 0.95 . ? C15 C16 1.408(12) . ? C15 H15A 0.95 . ? C16 H16A 0.95 . ? C21 C22 1.382(11) . ? C21 C26 1.384(11) . ? C22 C23 1.440(12) . ? C22 H22A 0.95 . ? C23 C24 1.349(14) . ? C23 H23A 0.95 . ? C24 C25 1.434(14) . ? C24 H24A 0.95 . ? C25 C26 1.390(12) . ? C25 H25A 0.95 . ? C26 H26A 0.95 . ? C31 C32 1.363(12) . ? C31 C36 1.364(12) . ? C32 C33 1.417(16) . ? C32 H32A 0.95 . ? C33 C34 1.438(17) . ? C33 H33A 0.95 . ? C34 C35 1.367(14) . ? C34 H34A 0.95 . ? C35 C36 1.443(13) . ? C35 H35A 0.95 . ? C36 H36A 0.95 . ? P2 C51 1.817(9) . ? P2 C41 1.811(10) . ? P2 C61 1.849(10) . ? C41 C46 1.341(13) . ? C41 C42 1.379(14) . ? C42 C43 1.361(17) . ? C42 H42A 0.95 . ? C43 C44 1.447(18) . ? C43 H43A 0.95 . ? C44 C45 1.347(17) . ? C44 H44A 0.95 . ? C45 C46 1.380(16) . ? C45 H45A 0.95 . ? C46 H46A 0.95 . ? C51 C56 1.356(13) . ? C51 C52 1.418(13) . ? C52 C53 1.343(16) . ? C52 H52A 0.95 . ? C53 C54 1.343(17) . ? C53 H53A 0.95 . ? C54 C55 1.452(17) . ? C54 H54A 0.95 . ? C55 C56 1.405(13) . ? C55 H55A 0.95 . ? C56 H56 0.95 . ? C61 C62 1.344(13) . ? C61 C66 1.410(14) . ? C62 C63 1.371(13) . ? C62 H62A 0.95 . ? C63 C64 1.298(15) . ? C63 H63A 0.95 . ? C64 C65 1.382(17) . ? C64 H64A 0.95 . ? C65 C66 1.413(16) . ? C65 H65A 0.95 . ? C66 H66A 0.95 . ? 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 N3B Pt1 N3A 84.8(3) . . ? N3B Pt1 P2 167.4(2) . . ? N3A Pt1 P2 89.21(19) . . ? N3B Pt1 P1 89.96(19) . . ? N3A Pt1 P1 167.01(19) . . ? P2 Pt1 P1 98.08(8) . . ? C6A N1A C2A 121.2(8) . . ? C6A N1A C1A 120.6(9) . . ? C2A N1A C1A 118.2(9) . . ? N1A C1A H1AA 109.5 . . ? N1A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? N1A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? O2A C2A N3A 123.3(9) . . ? O2A C2A N1A 121.5(9) . . ? N3A C2A N1A 115.2(9) . . ? C4A N3A C2A 125.3(8) . . ? C4A N3A Pt1 121.6(5) . . ? C2A N3A Pt1 112.9(6) . . ? O4A C4A N3A 121.7(8) . . ? O4A C4A C5A 120.9(8) . . ? N3A C4A C5A 117.5(8) . . ? C6A C5A C4A 117.5(8) . . ? C6A C5A C51A 122.2(8) . . ? C4A C5A C51A 120.3(7) . . ? C5A C51A C5A 113.6(10) . 3_655 ? C5A C51A H5A 109.7 . . ? C5A C51A H5A 108 3_655 . ? C5A C6A N1A 123.2(9) . . ? C5A C6A H6AA 118.4 . . ? N1A C6A H6AA 118.4 . . ? C2B N1B C6B 118.6(9) . . ? C2B N1B C1B 116.3(10) . . ? C6B N1B C1B 125.1(9) . . ? N1B C1B H1BA 109.5 . . ? N1B C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? N1B C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? O2B C2B N3B 124.3(8) . . ? O2B C2B N1B 120.2(9) . . ? N3B C2B N1B 115.5(9) . . ? C2B N3B C4B 125.9(8) . . ? C2B N3B Pt1 113.8(6) . . ? C4B N3B Pt1 119.8(6) . . ? O4B C4B N3B 120.2(8) . . ? O4B C4B C5B 123.0(10) . . ? N3B C4B C5B 116.6(10) . . ? C6B C5B C4B 119.1(11) . . ? C6B C5B C51B 119.5(9) . . ? C4B C5B C51B 121.3(11) . . ? C5B C51B C5B 111.7(11) . 3_655 ? C5B C51B H51A 112.2 . . ? C5B C51B H51A 106.6 3_655 . ? C5B C6B N1B 124.3(10) . . ? C5B C6B H6BA 117.9 . . ? N1B C6B H6BA 117.9 . . ? C31 P1 C11 107.1(4) . . ? C31 P1 C21 105.1(4) . . ? C11 P1 C21 99.4(4) . . ? C31 P1 Pt1 118.1(3) . . ? C11 P1 Pt1 109.8(3) . . ? C21 P1 Pt1 115.6(3) . . ? C16 C11 C12 119.6(8) . . ? C16 C11 P1 120.7(6) . . ? C12 C11 P1 119.6(7) . . ? C11 C12 C13 120.0(10) . . ? C11 C12 H12A 120 . . ? C13 C12 H12A 120 . . ? C14 C13 C12 119.6(9) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 121.3(9) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C14 C15 C16 117.1(9) . . ? C14 C15 H15A 121.4 . . ? C16 C15 H15A 121.4 . . ? C11 C16 C15 122.2(8) . . ? C11 C16 H16A 118.9 . . ? C15 C16 H16A 118.9 . . ? C22 C21 C26 119.4(8) . . ? C22 C21 P1 123.0(7) . . ? C26 C21 P1 117.6(7) . . ? C21 C22 C23 119.2(9) . . ? C21 C22 H22A 120.4 . . ? C23 C22 H22A 120.4 . . ? C24 C23 C22 121.5(10) . . ? C24 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? C23 C24 C25 118.9(9) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? C26 C25 C24 119.1(9) . . ? C26 C25 H25A 120.4 . . ? C24 C25 H25A 120.4 . . ? C25 C26 C21 121.9(9) . . ? C25 C26 H26A 119.1 . . ? C21 C26 H26A 119.1 . . ? C32 C31 C36 119.4(8) . . ? C32 C31 P1 117.9(6) . . ? C36 C31 P1 122.7(7) . . ? C31 C32 C33 122.2(10) . . ? C31 C32 H32A 118.9 . . ? C33 C32 H32A 118.9 . . ? C34 C33 C32 118.3(11) . . ? C34 C33 H33A 120.8 . . ? C32 C33 H33A 120.8 . . ? C35 C34 C33 119.1(10) . . ? C35 C34 H34A 120.5 . . ? C33 C34 H34A 120.5 . . ? C34 C35 C36 120.0(10) . . ? C34 C35 H35A 120 . . ? C36 C35 H35A 120 . . ? C31 C36 C35 121.0(9) . . ? C31 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C51 P2 C41 106.8(5) . . ? C51 P2 C61 98.3(4) . . ? C41 P2 C61 107.1(4) . . ? C51 P2 Pt1 110.0(3) . . ? C41 P2 Pt1 117.6(3) . . ? C61 P2 Pt1 115.1(3) . . ? C46 C41 C42 119.8(11) . . ? C46 C41 P2 118.5(8) . . ? C42 C41 P2 121.5(9) . . ? C43 C42 C41 117.9(13) . . ? C43 C42 H42A 121 . . ? C41 C42 H42A 121 . . ? C42 C43 C44 121.0(13) . . ? C42 C43 H43A 119.5 . . ? C44 C43 H43A 119.5 . . ? C45 C44 C43 119.6(13) . . ? C45 C44 H44A 120.2 . . ? C43 C44 H44A 120.2 . . ? C46 C45 C44 116.9(12) . . ? C46 C45 H45A 121.6 . . ? C44 C45 H45A 121.6 . . ? C41 C46 C45 124.7(11) . . ? C41 C46 H46A 117.6 . . ? C45 C46 H46A 117.6 . . ? C56 C51 C52 118.7(10) . . ? C56 C51 P2 119.8(7) . . ? C52 C51 P2 120.7(8) . . ? C53 C52 C51 123.3(13) . . ? C53 C52 H52A 118.3 . . ? C51 C52 H52A 118.3 . . ? C52 C53 C54 116.5(13) . . ? C52 C53 H53A 121.7 . . ? C54 C53 H53A 121.7 . . ? C53 C54 C55 124.6(13) . . ? C53 C54 H54A 117.7 . . ? C55 C54 H54A 117.7 . . ? C56 C55 C54 115.1(12) . . ? C56 C55 H55A 122.5 . . ? C54 C55 H55A 122.5 . . ? C51 C56 C55 121.1(10) . . ? C51 C56 H56 119.4 . . ? C55 C56 H56 119.4 . . ? C62 C61 C66 118.2(10) . . ? C62 C61 P2 119.2(8) . . ? C66 C61 P2 122.1(8) . . ? C61 C62 C63 122.9(11) . . ? C61 C62 H62A 118.5 . . ? C63 C62 H62A 118.5 . . ? C64 C63 C62 122.2(12) . . ? C64 C63 H63A 118.9 . . ? C62 C63 H63A 118.9 . . ? C63 C64 C65 116.9(12) . . ? C63 C64 H64A 121.5 . . ? C65 C64 H64A 121.5 . . ? C64 C65 C66 124.0(12) . . ? C64 C65 H65A 118 . . ? C66 C65 H65A 118 . . ? C65 C66 C61 115.5(12) . . ? C65 C66 H66A 122.3 . . ? C61 C66 H66A 122.3 . . ? 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 C6A N1A C2A O2A -175.6(9) . . . . ? C1A N1A C2A O2A 5.1(15) . . . . ? C6A N1A C2A N3A 2.6(13) . . . . ? C1A N1A C2A N3A -176.7(10) . . . . ? O2A C2A N3A C4A 174.7(8) . . . . ? N1A C2A N3A C4A -3.5(13) . . . . ? O2A C2A N3A Pt1 -10.5(12) . . . . ? N1A C2A N3A Pt1 171.3(6) . . . . ? N3B Pt1 N3A C4A 64.8(6) . . . . ? P2 Pt1 N3A C4A -104.1(6) . . . . ? P1 Pt1 N3A C4A 131.5(7) . . . . ? N3B Pt1 N3A C2A -110.2(6) . . . . ? P2 Pt1 N3A C2A 80.9(6) . . . . ? P1 Pt1 N3A C2A -43.5(12) . . . . ? C2A N3A C4A O4A -176.6(8) . . . . ? Pt1 N3A C4A O4A 9.1(11) . . . . ? C2A N3A C4A C5A 3.8(12) . . . . ? Pt1 N3A C4A C5A -170.5(5) . . . . ? O4A C4A C5A C6A 177.1(8) . . . . ? N3A C4A C5A C6A -3.3(12) . . . . ? O4A C4A C5A C51A -0.6(12) . . . . ? N3A C4A C5A C51A 179.0(7) . . . . ? C6A C5A C51A C5A 101.9(9) . . . 3_655 ? C4A C5A C51A C5A -80.5(7) . . . 3_655 ? C4A C5A C6A N1A 2.8(14) . . . . ? C51A C5A C6A N1A -179.6(9) . . . . ? C2A N1A C6A C5A -2.6(15) . . . . ? C1A N1A C6A C5A 176.7(11) . . . . ? C6B N1B C2B O2B -176.9(8) . . . . ? C1B N1B C2B O2B 1.4(13) . . . . ? C6B N1B C2B N3B 0.5(12) . . . . ? C1B N1B C2B N3B 178.8(9) . . . . ? O2B C2B N3B C4B 177.3(8) . . . . ? N1B C2B N3B C4B 0.0(12) . . . . ? O2B C2B N3B Pt1 -10.6(11) . . . . ? N1B C2B N3B Pt1 172.1(6) . . . . ? N3A Pt1 N3B C2B -107.9(6) . . . . ? P2 Pt1 N3B C2B -45.9(12) . . . . ? P1 Pt1 N3B C2B 84.0(5) . . . . ? N3A Pt1 N3B C4B 64.8(6) . . . . ? P2 Pt1 N3B C4B 126.7(9) . . . . ? P1 Pt1 N3B C4B -103.3(6) . . . . ? C2B N3B C4B O4B -175.3(8) . . . . ? Pt1 N3B C4B O4B 13.0(10) . . . . ? C2B N3B C4B C5B -0.8(12) . . . . ? Pt1 N3B C4B C5B -172.5(6) . . . . ? O4B C4B C5B C6B 175.4(9) . . . . ? N3B C4B C5B C6B 1.1(13) . . . . ? O4B C4B C5B C51B -4.1(14) . . . . ? N3B C4B C5B C51B -178.5(8) . . . . ? C6B C5B C51B C5B 99.9(10) . . . 3_655 ? C4B C5B C51B C5B -80.5(9) . . . 3_655 ? C4B C5B C6B N1B -0.6(16) . . . . ? C51B C5B C6B N1B 178.9(9) . . . . ? C2B N1B C6B C5B -0.2(15) . . . . ? C1B N1B C6B C5B -178.4(11) . . . . ? N3B Pt1 P1 C31 -137.2(4) . . . . ? N3A Pt1 P1 C31 156.7(9) . . . . ? P2 Pt1 P1 C31 33.1(3) . . . . ? N3B Pt1 P1 C11 99.7(4) . . . . ? N3A Pt1 P1 C11 33.6(9) . . . . ? P2 Pt1 P1 C11 -90.0(3) . . . . ? N3B Pt1 P1 C21 -11.6(4) . . . . ? N3A Pt1 P1 C21 -77.7(9) . . . . ? P2 Pt1 P1 C21 158.7(3) . . . . ? C31 P1 C11 C16 -123.4(7) . . . . ? C21 P1 C11 C16 127.5(7) . . . . ? Pt1 P1 C11 C16 5.9(8) . . . . ? C31 P1 C11 C12 56.9(8) . . . . ? C21 P1 C11 C12 -52.1(8) . . . . ? Pt1 P1 C11 C12 -173.8(6) . . . . ? C16 C11 C12 C13 0.9(13) . . . . ? P1 C11 C12 C13 -179.5(7) . . . . ? C11 C12 C13 C14 2.3(14) . . . . ? C12 C13 C14 C15 -2.7(15) . . . . ? C13 C14 C15 C16 -0.2(15) . . . . ? C12 C11 C16 C15 -3.9(14) . . . . ? P1 C11 C16 C15 176.5(7) . . . . ? C14 C15 C16 C11 3.5(14) . . . . ? C31 P1 C21 C22 20.9(8) . . . . ? C11 P1 C21 C22 131.6(7) . . . . ? Pt1 P1 C21 C22 -111.1(7) . . . . ? C31 P1 C21 C26 -160.9(6) . . . . ? C11 P1 C21 C26 -50.2(7) . . . . ? Pt1 P1 C21 C26 67.1(7) . . . . ? C26 C21 C22 C23 -0.7(12) . . . . ? P1 C21 C22 C23 177.5(7) . . . . ? C21 C22 C23 C24 -0.6(14) . . . . ? C22 C23 C24 C25 1.6(15) . . . . ? C23 C24 C25 C26 -1.3(14) . . . . ? C24 C25 C26 C21 0.0(13) . . . . ? C22 C21 C26 C25 1.0(12) . . . . ? P1 C21 C26 C25 -177.3(6) . . . . ? C11 P1 C31 C32 -177.1(7) . . . . ? C21 P1 C31 C32 -72.0(8) . . . . ? Pt1 P1 C31 C32 58.6(8) . . . . ? C11 P1 C31 C36 4.6(9) . . . . ? C21 P1 C31 C36 109.7(8) . . . . ? Pt1 P1 C31 C36 -119.7(8) . . . . ? C36 C31 C32 C33 -0.1(14) . . . . ? P1 C31 C32 C33 -178.5(7) . . . . ? C31 C32 C33 C34 0.5(15) . . . . ? C32 C33 C34 C35 -1.3(16) . . . . ? C33 C34 C35 C36 1.7(17) . . . . ? C32 C31 C36 C35 0.5(15) . . . . ? P1 C31 C36 C35 178.8(8) . . . . ? C34 C35 C36 C31 -1.4(17) . . . . ? N3B Pt1 P2 C51 48.1(10) . . . . ? N3A Pt1 P2 C51 109.6(4) . . . . ? P1 Pt1 P2 C51 -81.2(3) . . . . ? N3B Pt1 P2 C41 170.5(10) . . . . ? N3A Pt1 P2 C41 -127.9(4) . . . . ? P1 Pt1 P2 C41 41.3(4) . . . . ? N3B Pt1 P2 C61 -61.8(10) . . . . ? N3A Pt1 P2 C61 -0.3(4) . . . . ? P1 Pt1 P2 C61 168.9(4) . . . . ? C51 P2 C41 C46 -174.1(8) . . . . ? C61 P2 C41 C46 -69.6(9) . . . . ? Pt1 P2 C41 C46 61.8(8) . . . . ? C51 P2 C41 C42 10.1(10) . . . . ? C61 P2 C41 C42 114.6(9) . . . . ? Pt1 P2 C41 C42 -114.0(9) . . . . ? C46 C41 C42 C43 2.6(17) . . . . ? P2 C41 C42 C43 178.4(9) . . . . ? C41 C42 C43 C44 -3.8(19) . . . . ? C42 C43 C44 C45 4(2) . . . . ? C43 C44 C45 C46 -1.9(18) . . . . ? C42 C41 C46 C45 -1.2(16) . . . . ? P2 C41 C46 C45 -177.1(8) . . . . ? C44 C45 C46 C41 0.9(17) . . . . ? C41 P2 C51 C56 -142.2(7) . . . . ? C61 P2 C51 C56 107.1(8) . . . . ? Pt1 P2 C51 C56 -13.5(8) . . . . ? C41 P2 C51 C52 48.6(9) . . . . ? C61 P2 C51 C52 -62.1(9) . . . . ? Pt1 P2 C51 C52 177.3(8) . . . . ? C56 C51 C52 C53 10.2(17) . . . . ? P2 C51 C52 C53 179.5(10) . . . . ? C51 C52 C53 C54 -7(2) . . . . ? C52 C53 C54 C55 1(2) . . . . ? C53 C54 C55 C56 0.9(19) . . . . ? C52 C51 C56 C55 -7.6(14) . . . . ? P2 C51 C56 C55 -177.0(7) . . . . ? C54 C55 C56 C51 2.5(14) . . . . ? C51 P2 C61 C62 -50.8(8) . . . . ? C41 P2 C61 C62 -161.3(8) . . . . ? Pt1 P2 C61 C62 65.9(8) . . . . ? C51 P2 C61 C66 136.6(10) . . . . ? C41 P2 C61 C66 26.1(11) . . . . ? Pt1 P2 C61 C66 -106.6(9) . . . . ? C66 C61 C62 C63 -4.9(15) . . . . ? P2 C61 C62 C63 -177.8(8) . . . . ? C61 C62 C63 C64 3.1(19) . . . . ? C62 C63 C64 C65 1(2) . . . . ? C63 C64 C65 C66 -3(2) . . . . ? C64 C65 C66 C61 1(2) . . . . ? C62 C61 C66 C65 2.9(17) . . . . ? P2 C61 C66 C65 175.6(9) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'CCDC_735161_revised.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-04-15 at 16:04:25 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : 1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_3 _database_code_depnum_ccdc_archive 'CCDC 735161' _audit_creation_date 2009-04-15T16:04:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C62 H52 N16 O8 Pt4, 4(N O3), 8(H2 O)' _chemical_formula_sum 'C62 H68 N20 O28 Pt4' _chemical_formula_weight 2321.72 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 11.4361(6) _cell_length_b 26.9523(8) _cell_length_c 47.507(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 14643.1(12) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6422 _cell_measurement_theta_min 1.9806 _cell_measurement_theta_max 28.1435 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8928 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.330 _exptl_absorpt_correction_T_max 0.463 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_unetI/netI 0.0978 _diffrn_reflns_number 17431 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.2 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.869 _reflns_number_total 3930 _reflns_number_gt 2552 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. The disordered nitrate was defined with DFIX restrains. ; _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^)+(0.0734P)^2^+1610.1252P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3930 _refine_ls_number_parameters 229 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.127 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.067 _refine_diff_density_min -2.289 _refine_diff_density_rms 0.279 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pt1 Pt 0.57012(6) 0.07736(2) 0.046965(14) 0.0308(2) Uani 1 1 d . . . O2 O 0.6307(14) -0.0173(4) 0.0763(3) 0.056(4) Uani 1 1 d . . . O4 O 0.7693(9) 0.1404(4) 0.0789(2) 0.032(3) Uani 1 1 d . . . N1 N 0.7697(14) 0.0019(5) 0.1074(4) 0.047(4) Uani 1 1 d . . . N3 N 0.6960(11) 0.0610(4) 0.0766(3) 0.028(3) Uani 1 1 d . . . N11 N 0.6423(12) 0.0445(4) 0.0137(3) 0.033(3) Uani 1 1 d . . . N21 N 0.4497(11) 0.0945(4) 0.0177(3) 0.032(3) Uani 1 1 d . . . C1 C 0.781(2) -0.0507(6) 0.1159(5) 0.069(7) Uani 1 1 d . . . H1A H 0.7237 -0.0583 0.1306 0.104 Uiso 1 1 calc R . . H1B H 0.8602 -0.0566 0.1232 0.104 Uiso 1 1 calc R . . H1C H 0.7675 -0.0721 0.0995 0.104 Uiso 1 1 calc R . . C2 C 0.6935(17) 0.0135(6) 0.0863(4) 0.044(5) Uani 1 1 d . . . C4 C 0.7618(15) 0.0957(6) 0.0883(4) 0.032(4) Uani 1 1 d . . . C5 C 0.8356(14) 0.0843(6) 0.1113(4) 0.035(4) Uani 1 1 d . . . C6 C 0.8384(16) 0.0374(7) 0.1200(4) 0.051(6) Uani 1 1 d . . . H6 H 0.8886 0.0283 0.135 0.061 Uiso 1 1 calc R . . C12 C 0.5818(17) 0.0524(6) -0.0109(4) 0.041(3) Uani 1 1 d . . . C13 C 0.6247(18) 0.0312(7) -0.0362(5) 0.055(6) Uani 1 1 d . . . H13 H 0.5813 0.0348 -0.0531 0.066 Uiso 1 1 calc R . . C14 C 0.723(2) 0.0066(8) -0.0364(5) 0.056(6) Uani 1 1 d . . . H14 H 0.7523 -0.0059 -0.0537 0.068 Uiso 1 1 calc R . . C15 C 0.7870(18) -0.0016(6) -0.0116(6) 0.064(8) Uani 1 1 d . . . H15 H 0.8577 -0.0202 -0.0116 0.076 Uiso 1 1 calc R . . C16 C 0.7393(18) 0.0196(6) 0.0140(5) 0.054(6) Uani 1 1 d . . . H16 H 0.7799 0.0152 0.0313 0.065 Uiso 1 1 calc R . . C22 C 0.4792(17) 0.0817(6) -0.0091(4) 0.041(3) Uani 1 1 d . . . C23 C 0.406(2) 0.0958(8) -0.0312(5) 0.063(7) Uani 1 1 d . . . H23 H 0.4238 0.086 -0.0499 0.076 Uiso 1 1 calc R . . C24 C 0.305(2) 0.1242(9) -0.0260(6) 0.075(7) Uani 1 1 d . . . H24 H 0.2564 0.1351 -0.0409 0.089 Uiso 1 1 calc R . . C25 C 0.2803(19) 0.1355(8) 0.0008(6) 0.063(7) Uani 1 1 d . . . H25 H 0.2112 0.1534 0.0052 0.076 Uiso 1 1 calc R . . C26 C 0.3554(17) 0.1209(6) 0.0218(4) 0.048(5) Uani 1 1 d . . . H26 H 0.3376 0.1307 0.0406 0.057 Uiso 1 1 calc R . . C51 C 0.907(2) 0.125 0.125 0.041(6) Uani 1 2 d S . . H51A H 0.9567 0.1401 0.1111 0.05 Uiso 1 1 d R . . N1N N 0.285(4) 0.2699(9) 0.0575(8) 0.134(4) Uani 0.5 1 d PD . . N1N' N 0.221(4) 0.2385(9) 0.0734(8) 0.134(4) Uani 0.5 1 d PD . . O11 O 0.357(3) 0.2997(11) 0.0438(7) 0.134(4) Uani 0.5 1 d PD . . O11' O 0.149(3) 0.2092(11) 0.0875(7) 0.134(4) Uani 0.5 1 d PD . . O12 O 0.2296(19) 0.2859(7) 0.0800(5) 0.134(4) Uani 1 1 d D . . O13 O 0.2777(19) 0.2225(8) 0.0510(5) 0.134(4) Uani 1 1 d D . . O1W O 0.625 0.125 -0.0785(8) 0.134(4) Uani 1 2 d S . . O2W O 0.125 0.125 0.0624(8) 0.134(4) Uani 1 2 d S . . O3W O 0.0835(19) 0.3428(9) 0.1001(6) 0.134(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0371(4) 0.0188(3) 0.0365(4) -0.0076(3) 0.0056(3) 0.0049(3) O2 0.083(10) 0.023(6) 0.060(9) -0.005(6) 0.011(8) -0.007(7) O4 0.024(6) 0.034(6) 0.039(7) 0.014(5) 0.001(5) 0.006(5) N1 0.055(10) 0.017(6) 0.069(12) 0.004(7) 0.019(10) 0.017(7) N3 0.020(7) 0.022(6) 0.042(8) 0.008(6) 0.003(6) 0.008(5) N11 0.033(8) 0.008(5) 0.058(10) -0.006(6) 0.012(7) -0.004(5) N21 0.028(8) 0.013(5) 0.053(9) -0.014(6) -0.015(7) 0.001(5) C1 0.081(16) 0.028(9) 0.098(19) 0.036(11) 0.014(15) 0.013(10) C2 0.049(12) 0.032(9) 0.051(12) 0.001(8) -0.005(10) 0.020(9) C4 0.033(9) 0.029(8) 0.035(10) 0.013(7) 0.003(8) 0.009(7) C5 0.028(9) 0.041(9) 0.035(9) 0.015(8) 0.005(8) 0.004(7) C6 0.040(11) 0.058(12) 0.054(13) 0.038(10) 0.017(10) 0.017(9) C12 0.053(8) 0.024(6) 0.044(7) -0.014(5) 0.004(7) -0.025(5) C13 0.039(12) 0.065(13) 0.062(14) -0.033(11) 0.004(11) -0.018(10) C14 0.056(14) 0.052(12) 0.060(14) 0.003(11) -0.001(12) -0.015(11) C15 0.038(12) 0.028(9) 0.12(2) -0.004(11) 0.059(14) -0.007(8) C16 0.059(13) 0.016(7) 0.088(16) 0.008(9) 0.031(12) 0.011(8) C22 0.053(8) 0.024(6) 0.044(7) -0.014(5) 0.004(7) -0.025(5) C23 0.088(19) 0.056(12) 0.045(13) -0.010(10) -0.027(13) -0.029(12) C24 0.069(17) 0.068(15) 0.087(19) -0.005(14) -0.048(16) 0.000(13) C25 0.046(13) 0.053(12) 0.090(19) -0.001(12) -0.040(13) 0.001(10) C26 0.063(13) 0.029(9) 0.051(12) -0.021(8) -0.016(11) 0.006(9) C51 0.032(14) 0.057(15) 0.035(14) 0.034(12) 0 0 N1N 0.097(8) 0.145(10) 0.161(11) -0.016(10) -0.021(9) -0.007(7) N1N' 0.097(8) 0.145(10) 0.161(11) -0.016(10) -0.021(9) -0.007(7) O11 0.097(8) 0.145(10) 0.161(11) -0.016(10) -0.021(9) -0.007(7) O11' 0.097(8) 0.145(10) 0.161(11) -0.016(10) -0.021(9) -0.007(7) O12 0.097(8) 0.145(10) 0.161(11) -0.016(10) -0.021(9) -0.007(7) O13 0.097(8) 0.145(10) 0.161(11) -0.016(10) -0.021(9) -0.007(7) O1W 0.097(8) 0.145(10) 0.161(11) -0.016(10) -0.021(9) -0.007(7) O2W 0.097(8) 0.145(10) 0.161(11) -0.016(10) -0.021(9) -0.007(7) O3W 0.097(8) 0.145(10) 0.161(11) -0.016(10) -0.021(9) -0.007(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pt1 N11 1.989(14) . ? Pt1 N21 2.010(13) . ? Pt1 O4 2.023(11) 14_545 ? Pt1 N3 2.062(13) . ? Pt1 Pt1 2.8583(12) 14_545 ? O2 C2 1.20(2) . ? O4 C4 1.289(17) . ? O4 Pt1 2.023(11) 14_545 ? N1 C2 1.37(2) . ? N1 C6 1.37(3) . ? N1 C1 1.48(2) . ? N3 C4 1.32(2) . ? N3 C2 1.36(2) . ? N11 C16 1.30(2) . ? N11 C12 1.38(2) . ? N21 C26 1.31(2) . ? N21 C22 1.36(2) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C4 C5 1.41(2) . ? C5 C6 1.33(2) . ? C5 C51 1.52(2) . ? C6 H6 0.95 . ? C12 C22 1.42(3) . ? C12 C13 1.42(3) . ? C13 C14 1.31(3) . ? C13 H13 0.95 . ? C14 C15 1.40(3) . ? C14 H14 0.95 . ? C15 C16 1.45(3) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C22 C23 1.40(3) . ? C23 C24 1.40(3) . ? C23 H23 0.95 . ? C24 C25 1.34(3) . ? C24 H24 0.95 . ? C25 C26 1.38(3) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C51 C5 1.52(2) 8_544 ? C51 H51A 0.9599 . ? N1N O12 1.315(9) . ? N1N O13 1.315(9) . ? N1N O11 1.321(9) . ? N1N N1N' 1.348(18) . ? N1N' O12 1.318(9) . ? N1N' O13 1.318(9) . ? N1N' O11' 1.321(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 N11 Pt1 N21 80.7(6) . . ? N11 Pt1 O4 174.2(5) . 14_545 ? N21 Pt1 O4 94.2(5) . 14_545 ? N11 Pt1 N3 99.1(6) . . ? N21 Pt1 N3 178.7(5) . . ? O4 Pt1 N3 86.1(5) 14_545 . ? N11 Pt1 Pt1 102.6(3) . 14_545 ? N21 Pt1 Pt1 95.4(3) . 14_545 ? O4 Pt1 Pt1 80.6(3) 14_545 14_545 ? N3 Pt1 Pt1 83.4(3) . 14_545 ? C4 O4 Pt1 129.0(11) . 14_545 ? C2 N1 C6 121.6(14) . . ? C2 N1 C1 118.5(17) . . ? C6 N1 C1 119.9(18) . . ? C4 N3 C2 122.4(15) . . ? C4 N3 Pt1 122.3(10) . . ? C2 N3 Pt1 114.6(12) . . ? C16 N11 C12 121.3(17) . . ? C16 N11 Pt1 125.3(15) . . ? C12 N11 Pt1 113.4(11) . . ? C26 N21 C22 118.8(17) . . ? C26 N21 Pt1 126.0(13) . . ? C22 N21 Pt1 114.8(12) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 N1 121.0(16) . . ? O2 C2 N3 122.2(18) . . ? N1 C2 N3 116.7(17) . . ? O4 C4 N3 123.5(15) . . ? O4 C4 C5 115.7(15) . . ? N3 C4 C5 120.7(14) . . ? C6 C5 C4 117.3(17) . . ? C6 C5 C51 122.9(16) . . ? C4 C5 C51 119.8(13) . . ? C5 C6 N1 121.0(18) . . ? C5 C6 H6 119.5 . . ? N1 C6 H6 119.5 . . ? N11 C12 C22 117.0(16) . . ? N11 C12 C13 118.9(18) . . ? C22 C12 C13 124.1(19) . . ? C14 C13 C12 121(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 121(2) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C16 116.5(19) . . ? C14 C15 H15 121.7 . . ? C16 C15 H15 121.7 . . ? N11 C16 C15 121(2) . . ? N11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? N21 C22 C23 119.0(18) . . ? N21 C22 C12 113.6(17) . . ? C23 C22 C12 127.3(18) . . ? C22 C23 C24 120(2) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 118(2) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? C24 C25 C26 120(2) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N21 C26 C25 124(2) . . ? N21 C26 H26 117.9 . . ? C25 C26 H26 117.9 . . ? C5 C51 C5 114(2) 8_544 . ? C5 C51 H51A 107.8 8_544 . ? C5 C51 H51A 109.3 . . ? O12 N1N O13 118.6(10) . . ? O12 N1N O11 120.0(10) . . ? O13 N1N O11 120.9(10) . . ? O12 N1N N1N' 59.3(6) . . ? O13 N1N N1N' 59.3(6) . . ? O11 N1N N1N' 174(6) . . ? O12 N1N' O13 118.2(10) . . ? O12 N1N' O11' 120.2(10) . . ? O13 N1N' O11' 121.3(10) . . ? O12 N1N' N1N 59.1(6) . . ? O13 N1N' N1N 59.1(6) . . ? O11' N1N' N1N 175(6) . . ? N1N O12 N1N' 61.6(9) . . ? N1N O13 N1N' 61.6(9) . . ? 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 N11 Pt1 N3 C4 113.1(12) . . . . ? O4 Pt1 N3 C4 -69.6(13) 14_545 . . . ? Pt1 Pt1 N3 C4 11.4(12) 14_545 . . . ? N11 Pt1 N3 C2 -76.6(12) . . . . ? O4 Pt1 N3 C2 100.8(12) 14_545 . . . ? Pt1 Pt1 N3 C2 -178.3(12) 14_545 . . . ? N21 Pt1 N11 C16 -179.1(13) . . . . ? N3 Pt1 N11 C16 2.2(13) . . . . ? Pt1 Pt1 N11 C16 87.4(13) 14_545 . . . ? N21 Pt1 N11 C12 3.8(10) . . . . ? N3 Pt1 N11 C12 -174.9(10) . . . . ? Pt1 Pt1 N11 C12 -89.7(10) 14_545 . . . ? N11 Pt1 N21 C26 -178.8(15) . . . . ? O4 Pt1 N21 C26 4.0(14) 14_545 . . . ? Pt1 Pt1 N21 C26 -76.9(14) 14_545 . . . ? N11 Pt1 N21 C22 -6.9(10) . . . . ? O4 Pt1 N21 C22 175.9(10) 14_545 . . . ? Pt1 Pt1 N21 C22 95.0(10) 14_545 . . . ? C6 N1 C2 O2 -176.9(18) . . . . ? C1 N1 C2 O2 6(3) . . . . ? C6 N1 C2 N3 5(3) . . . . ? C1 N1 C2 N3 -171.9(17) . . . . ? C4 N3 C2 O2 177.1(17) . . . . ? Pt1 N3 C2 O2 7(2) . . . . ? C4 N3 C2 N1 -5(2) . . . . ? Pt1 N3 C2 N1 -175.4(12) . . . . ? Pt1 O4 C4 N3 5(2) 14_545 . . . ? Pt1 O4 C4 C5 -179.3(10) 14_545 . . . ? C2 N3 C4 O4 177.0(16) . . . . ? Pt1 N3 C4 O4 -13(2) . . . . ? C2 N3 C4 C5 2(2) . . . . ? Pt1 N3 C4 C5 171.1(12) . . . . ? O4 C4 C5 C6 -173.9(16) . . . . ? N3 C4 C5 C6 2(2) . . . . ? O4 C4 C5 C51 6(2) . . . . ? N3 C4 C5 C51 -178.1(15) . . . . ? C4 C5 C6 N1 -2(3) . . . . ? C51 C5 C6 N1 178.4(16) . . . . ? C2 N1 C6 C5 -2(3) . . . . ? C1 N1 C6 C5 175.2(18) . . . . ? C16 N11 C12 C22 -177.6(14) . . . . ? Pt1 N11 C12 C22 -0.4(17) . . . . ? C16 N11 C12 C13 2(2) . . . . ? Pt1 N11 C12 C13 179.7(12) . . . . ? N11 C12 C13 C14 -4(3) . . . . ? C22 C12 C13 C14 176.6(17) . . . . ? C12 C13 C14 C15 3(3) . . . . ? C13 C14 C15 C16 -2(3) . . . . ? C12 N11 C16 C15 -1(2) . . . . ? Pt1 N11 C16 C15 -177.9(11) . . . . ? C14 C15 C16 N11 1(2) . . . . ? C26 N21 C22 C23 -2(2) . . . . ? Pt1 N21 C22 C23 -174.7(12) . . . . ? C26 N21 C22 C12 -179.0(14) . . . . ? Pt1 N21 C22 C12 8.5(16) . . . . ? N11 C12 C22 N21 -5.3(19) . . . . ? C13 C12 C22 N21 174.6(15) . . . . ? N11 C12 C22 C23 178.2(16) . . . . ? C13 C12 C22 C23 -2(3) . . . . ? N21 C22 C23 C24 2(3) . . . . ? C12 C22 C23 C24 178.6(18) . . . . ? C22 C23 C24 C25 -3(3) . . . . ? C23 C24 C25 C26 3(3) . . . . ? C22 N21 C26 C25 2(3) . . . . ? Pt1 N21 C26 C25 174.1(14) . . . . ? C24 C25 C26 N21 -3(3) . . . . ? C6 C5 C51 C5 -116.8(18) . . . 8_544 ? C4 C5 C51 C5 63.3(13) . . . 8_544 ? O13 N1N N1N' O12 179(5) . . . . ? O12 N1N N1N' O13 -179(5) . . . . ? O13 N1N O12 N1N' -1(5) . . . . ? O11 N1N O12 N1N' -173(7) . . . . ? O13 N1N' O12 N1N 1(5) . . . . ? O11' N1N' O12 N1N -174(7) . . . . ? O12 N1N O13 N1N' 1(5) . . . . ? O11 N1N O13 N1N' 173(7) . . . . ? O12 N1N' O13 N1N -1(5) . . . . ? O11' N1N' O13 N1N 174(7) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF