# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Benedetti, Michele' 'Barone, Carmen' 'Antonucci, Daniela' 'Vecchio, Vita' 'Ienco, Andrea' 'Maresca, Luciana' 'Natile, Giovanni' 'Fanizzi, Francesco' _publ_contact_author_name 'Dr Michele Benedetti' _publ_contact_author_email michele.benedetti@unisalento.it _publ_section_title ; Modulation of Properties in Analogues of Zeise's Anion on Changing the Ligand trans to ethene. X-Ray Crystal Structures of trans-[PtCl2(OH)(e2-C2H4)]- and trans-[PtCl2(e1-CH2NO2)(e2-C2H4)]- ; # Attachment '- cif_c2_c3.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-12-13 at 14:58:27 # 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 : barieter struct psi_scan dreduc #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# #TrackingRef '- cif_c2_c3.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2010-12-13 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_c2 _database_code_depnum_ccdc_archive 'CCDC 848868' #TrackingRef '- cif_c2_c3.cif' _audit_creation_date 2010-12-13T14:58:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H20 P, C2 H5 Cl2 O Pt' _chemical_formula_sum 'C26 H25 Cl2 O P Pt' _chemical_formula_weight 650.42 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.956(2) _cell_length_b 11.887(2) _cell_length_c 13.184(2) _cell_angle_alpha 91.152(16) _cell_angle_beta 90.206(18) _cell_angle_gamma 100.160(16) _cell_volume 1227.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 6.5 _cell_measurement_theta_max 9.19 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.225 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.76 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.017 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.2759 _exptl_absorpt_correction_T_max 0.4047 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 0.098675 _diffrn_orient_matrix_ub_12 0.047741 _diffrn_orient_matrix_ub_13 -0.034416 _diffrn_orient_matrix_ub_21 -0.00321 _diffrn_orient_matrix_ub_22 0.063352 _diffrn_orient_matrix_ub_23 0.050631 _diffrn_orient_matrix_ub_31 0.080987 _diffrn_orient_matrix_ub_32 -0.031866 _diffrn_orient_matrix_ub_33 0.044808 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 16 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -1 4 -2 -1 4 -2 -1 2 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_unetI/netI 0.0394 _diffrn_reflns_number 3575 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 22.97 _diffrn_reflns_theta_full 22.97 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 3400 _reflns_number_gt 2883 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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. ; _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^)+(0.0169P)^2^+8.8909P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3400 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.059 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.52 _refine_ls_restrained_S_all 1.52 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.613 _refine_diff_density_min -2.003 _refine_diff_density_rms 0.16 #----------------------------------------------------------------------------# # 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' 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' Cl Cl 0.1484 0.1585 '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 0.69492(7) 0.74888(5) 0.24969(5) 0.0641(2) Uani 1 1 d . . . P1 P 0.5137(4) 0.2717(3) 0.2571(2) 0.0443(8) Uani 1 1 d . . . Cl1 Cl 0.7011(6) 0.7089(4) 0.0795(3) 0.0949(13) Uani 1 1 d . . . Cl2 Cl 0.6975(6) 0.7912(7) 0.4186(4) 0.152(3) Uani 1 1 d . . . O1 O 0.8334(13) 0.6276(10) 0.2736(9) 0.089(3) Uani 1 1 d . . . C1 C 0.479(2) 0.8253(16) 0.2296(15) 0.099(6) Uani 1 1 d . . . H1A H 0.4127 0.8042 0.1683 0.13(4) Uiso 1 1 calc R . . H1B H 0.4108 0.8328 0.2892 0.13(4) Uiso 1 1 calc R . . C2 C 0.630(3) 0.9063(17) 0.2199(19) 0.117(7) Uani 1 1 d . . . H2A H 0.654 0.9643 0.2734 0.13(4) Uiso 1 1 calc R . . H2B H 0.6559 0.9357 0.1526 0.13(4) Uiso 1 1 calc R . . C3 C 0.3582(15) 0.1470(10) 0.2281(10) 0.048(3) Uani 1 1 d . . . C4 C 0.3530(17) 0.0938(12) 0.1342(11) 0.064(4) Uani 1 1 d . . . H4 H 0.4345 0.1194 0.0855 0.077 Uiso 1 1 calc R . . C5 C 0.226(2) 0.0030(14) 0.1137(14) 0.088(5) Uani 1 1 d . . . H5 H 0.2238 -0.0343 0.0509 0.106 Uiso 1 1 calc R . . C6 C 0.102(2) -0.0350(15) 0.1840(15) 0.090(5) Uani 1 1 d . . . H6 H 0.0158 -0.0964 0.1677 0.108 Uiso 1 1 calc R . . C7 C 0.1052(18) 0.0166(14) 0.2761(13) 0.077(5) Uani 1 1 d . . . H7 H 0.024 -0.01 0.3246 0.093 Uiso 1 1 calc R . . C8 C 0.2304(18) 0.1091(12) 0.2970(11) 0.067(4) Uani 1 1 d . . . H8 H 0.2297 0.1476 0.3591 0.08 Uiso 1 1 calc R . . C9 C 0.6508(15) 0.2506(11) 0.3613(9) 0.047(3) Uani 1 1 d . . . C10 C 0.6237(17) 0.1476(12) 0.4128(11) 0.062(4) Uani 1 1 d . . . H10 H 0.5299 0.0913 0.3972 0.075 Uiso 1 1 calc R . . C11 C 0.7383(19) 0.1307(14) 0.4871(12) 0.078(5) Uani 1 1 d . . . H11 H 0.7212 0.0635 0.5235 0.094 Uiso 1 1 calc R . . C12 C 0.878(2) 0.2139(16) 0.5069(12) 0.079(5) Uani 1 1 d . . . H12 H 0.955 0.2022 0.5571 0.095 Uiso 1 1 calc R . . C13 C 0.9063(18) 0.3134(14) 0.4550(11) 0.068(4) Uani 1 1 d . . . H13 H 1.003 0.3681 0.4685 0.082 Uiso 1 1 calc R . . C14 C 0.7902(16) 0.3319(13) 0.3822(10) 0.060(4) Uani 1 1 d . . . H14 H 0.8072 0.4001 0.3473 0.072 Uiso 1 1 calc R . . C15 C 0.3954(15) 0.3838(11) 0.2823(8) 0.045(3) Uani 1 1 d . . . C16 C 0.2518(17) 0.3844(12) 0.2233(10) 0.060(4) Uani 1 1 d . . . H16 H 0.2198 0.3279 0.1738 0.071 Uiso 1 1 calc R . . C17 C 0.1559(17) 0.4693(13) 0.2383(11) 0.063(4) Uani 1 1 d . . . H17 H 0.0582 0.469 0.1993 0.075 Uiso 1 1 calc R . . C18 C 0.203(2) 0.5538(14) 0.3097(12) 0.070(4) Uani 1 1 d . . . H18 H 0.1379 0.6108 0.32 0.084 Uiso 1 1 calc R . . C19 C 0.348(2) 0.5533(13) 0.3658(12) 0.077(5) Uani 1 1 d . . . H19 H 0.3807 0.6109 0.4143 0.092 Uiso 1 1 calc R . . C20 C 0.4443(17) 0.4711(12) 0.3528(11) 0.063(4) Uani 1 1 d . . . H20 H 0.5432 0.4734 0.3911 0.075 Uiso 1 1 calc R . . C21 C 0.6535(14) 0.3029(10) 0.1509(9) 0.044(3) Uani 1 1 d . . . C22 C 0.6427(17) 0.3911(13) 0.0881(10) 0.065(4) Uani 1 1 d . . . H22 H 0.5616 0.4372 0.1005 0.078 Uiso 1 1 calc R . . C23 C 0.750(2) 0.4127(14) 0.0066(12) 0.081(5) Uani 1 1 d . . . H23 H 0.7412 0.4726 -0.0362 0.097 Uiso 1 1 calc R . . C24 C 0.8708(19) 0.3455(14) -0.0109(11) 0.070(4) Uani 1 1 d . . . H24 H 0.9436 0.3602 -0.066 0.084 Uiso 1 1 calc R . . C25 C 0.8856(16) 0.2572(13) 0.0510(11) 0.065(4) Uani 1 1 d . . . H25 H 0.9667 0.2113 0.0379 0.078 Uiso 1 1 calc R . . C26 C 0.7779(16) 0.2365(11) 0.1343(10) 0.059(4) Uani 1 1 d . . . H26 H 0.7894 0.1783 0.1785 0.071 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 Pt1 0.0372(3) 0.0750(4) 0.0797(4) -0.0018(3) 0.0085(2) 0.0089(2) P1 0.0415(17) 0.0494(19) 0.0409(18) 0.0037(15) 0.0089(14) 0.0041(14) Cl1 0.087(3) 0.118(4) 0.082(3) 0.010(3) 0.022(2) 0.021(3) Cl2 0.070(3) 0.287(9) 0.092(4) -0.058(5) -0.005(3) 0.019(4) O1 0.066(6) 0.103(8) 0.109(9) 0.022(7) 0.004(6) 0.039(6) C1 0.059(10) 0.124(16) 0.124(16) -0.012(13) -0.005(10) 0.045(11) C2 0.099(15) 0.087(14) 0.17(2) -0.009(13) 0.014(14) 0.021(12) C3 0.047(7) 0.041(7) 0.054(8) 0.008(6) 0.009(6) 0.006(6) C4 0.059(8) 0.062(9) 0.066(10) -0.003(8) 0.003(7) -0.001(7) C5 0.079(11) 0.075(11) 0.099(13) -0.021(10) 0.005(10) -0.016(9) C6 0.068(11) 0.082(12) 0.105(15) 0.002(11) -0.018(10) -0.025(9) C7 0.047(8) 0.092(12) 0.085(12) 0.034(10) 0.005(8) -0.016(8) C8 0.067(9) 0.070(10) 0.061(9) 0.011(8) 0.014(7) 0.002(8) C9 0.041(7) 0.062(8) 0.038(7) 0.007(6) 0.010(5) 0.007(6) C10 0.050(8) 0.069(10) 0.068(10) 0.011(8) 0.006(7) 0.008(7) C11 0.060(9) 0.095(12) 0.081(12) 0.044(10) 0.008(8) 0.011(9) C12 0.063(10) 0.121(15) 0.061(10) 0.007(10) -0.007(8) 0.034(10) C13 0.054(8) 0.088(12) 0.060(10) 0.002(9) 0.005(7) 0.003(8) C14 0.049(8) 0.077(10) 0.052(8) 0.001(7) 0.007(7) 0.008(7) C15 0.045(7) 0.060(8) 0.029(7) 0.007(6) 0.012(5) 0.008(6) C16 0.055(8) 0.067(9) 0.055(9) -0.001(7) 0.015(7) 0.008(7) C17 0.050(8) 0.083(11) 0.055(9) 0.006(8) 0.009(7) 0.013(8) C18 0.071(10) 0.080(11) 0.066(10) 0.013(9) 0.013(8) 0.032(8) C19 0.091(12) 0.070(10) 0.072(11) -0.014(8) 0.025(9) 0.020(9) C20 0.055(8) 0.072(10) 0.062(9) 0.000(8) 0.010(7) 0.013(7) C21 0.034(6) 0.057(8) 0.038(7) 0.005(6) 0.012(5) 0.002(6) C22 0.053(8) 0.091(11) 0.056(9) 0.023(8) 0.027(7) 0.020(8) C23 0.083(11) 0.095(12) 0.069(11) 0.041(9) 0.029(9) 0.026(9) C24 0.067(9) 0.086(11) 0.057(9) 0.008(9) 0.020(7) 0.010(8) C25 0.045(8) 0.081(11) 0.064(10) -0.019(8) 0.016(7) 0.001(7) C26 0.058(8) 0.059(9) 0.063(9) 0.003(7) 0.016(7) 0.016(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 O1 1.991(10) . ? Pt1 C2 2.071(19) . ? Pt1 C1 2.096(15) . ? Pt1 Cl2 2.272(5) . ? Pt1 Cl1 2.287(5) . ? P1 C15 1.788(12) . ? P1 C21 1.795(11) . ? P1 C3 1.789(12) . ? P1 C9 1.800(12) . ? C1 C2 1.41(2) . ? C1 H1A 0.97 . ? C1 H1B 0.97 . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C8 1.387(17) . ? C3 C4 1.376(18) . ? C4 C5 1.361(19) . ? C4 H4 0.93 . ? C5 C6 1.38(2) . ? C5 H5 0.93 . ? C6 C7 1.35(2) . ? C6 H6 0.93 . ? C7 C8 1.37(2) . ? C7 H7 0.93 . ? C8 H8 0.93 . ? C9 C14 1.360(17) . ? C9 C10 1.395(18) . ? C10 C11 1.377(19) . ? C10 H10 0.93 . ? C11 C12 1.37(2) . ? C11 H11 0.93 . ? C12 C13 1.36(2) . ? C12 H12 0.93 . ? C13 C14 1.377(19) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C16 1.381(17) . ? C15 C20 1.381(18) . ? C16 C17 1.380(18) . ? C16 H16 0.93 . ? C17 C18 1.37(2) . ? C17 H17 0.93 . ? C18 C19 1.37(2) . ? C18 H18 0.93 . ? C19 C20 1.354(19) . ? C19 H19 0.93 . ? C20 H20 0.93 . ? C21 C22 1.363(18) . ? C21 C26 1.386(16) . ? C22 C23 1.376(18) . ? C22 H22 0.93 . ? C23 C24 1.37(2) . ? C23 H23 0.93 . ? C24 C25 1.36(2) . ? C24 H24 0.93 . ? C25 C26 1.394(18) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? 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 O1 Pt1 C2 161.2(6) . . ? O1 Pt1 C1 159.3(6) . . ? C2 Pt1 C1 39.5(7) . . ? O1 Pt1 Cl2 90.5(4) . . ? C2 Pt1 Cl2 89.7(7) . . ? C1 Pt1 Cl2 90.5(6) . . ? O1 Pt1 Cl1 88.9(4) . . ? C2 Pt1 Cl1 90.2(7) . . ? C1 Pt1 Cl1 90.6(6) . . ? Cl2 Pt1 Cl1 178.20(19) . . ? C15 P1 C21 111.7(6) . . ? C15 P1 C3 105.9(6) . . ? C21 P1 C3 109.3(6) . . ? C15 P1 C9 112.5(6) . . ? C21 P1 C9 105.1(5) . . ? C3 P1 C9 112.4(6) . . ? C2 C1 Pt1 69.3(10) . . ? C2 C1 H1A 116.7 . . ? Pt1 C1 H1A 116.7 . . ? C2 C1 H1B 116.7 . . ? Pt1 C1 H1B 116.7 . . ? H1A C1 H1B 113.7 . . ? C1 C2 Pt1 71.2(11) . . ? C1 C2 H2A 116.5 . . ? Pt1 C2 H2A 116.5 . . ? C1 C2 H2B 116.5 . . ? Pt1 C2 H2B 116.5 . . ? H2A C2 H2B 113.5 . . ? C8 C3 C4 118.8(12) . . ? C8 C3 P1 120.0(11) . . ? C4 C3 P1 120.9(10) . . ? C5 C4 C3 118.8(14) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C6 C5 C4 121.7(16) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 120.1(15) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C8 118.7(14) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? C3 C8 C7 121.8(14) . . ? C3 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C14 C9 C10 120.7(12) . . ? C14 C9 P1 118.7(10) . . ? C10 C9 P1 120.3(10) . . ? C11 C10 C9 118.9(13) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C12 C11 C10 119.4(14) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C13 C12 C11 121.7(14) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C14 C13 C12 119.2(14) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C9 120.1(14) . . ? C13 C14 H14 120 . . ? C9 C14 H14 120 . . ? C16 C15 C20 119.1(12) . . ? C16 C15 P1 116.9(10) . . ? C20 C15 P1 123.9(10) . . ? C17 C16 C15 119.8(13) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 120.7(14) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 118.8(14) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 121.8(15) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C15 119.8(14) . . ? C19 C20 H20 120.1 . . ? C15 C20 H20 120.1 . . ? C22 C21 C26 119.5(11) . . ? C22 C21 P1 121.9(9) . . ? C26 C21 P1 118.6(10) . . ? C21 C22 C23 120.8(13) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.5(14) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 121.0(13) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 119.3(14) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C21 C26 C25 119.8(13) . . ? C21 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_c3 _database_code_depnum_ccdc_archive 'CCDC 848869' #TrackingRef '- cif_c2_c3.cif' _audit_creation_date 2011-03-03T14:30:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H20 P, C3 H6 Cl2 N O2 Pt' _chemical_formula_sum 'C27 H26 Cl2 N O2 P Pt' _chemical_formula_weight 693.45 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.8100(4) _cell_length_b 7.41700(10) _cell_length_c 19.2250(6) _cell_angle_alpha 90 _cell_angle_beta 91.915(2) _cell_angle_gamma 90 _cell_volume 2538.14(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5617 _cell_measurement_theta_min 4.3208 _cell_measurement_theta_max 29.158 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cubic _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.49531 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.4547 _diffrn_orient_matrix_ub_11 -0.003497 _diffrn_orient_matrix_ub_12 0.0215259 _diffrn_orient_matrix_ub_13 -0.0359248 _diffrn_orient_matrix_ub_21 -0.0072502 _diffrn_orient_matrix_ub_22 0.0912577 _diffrn_orient_matrix_ub_23 0.0085405 _diffrn_orient_matrix_ub_31 0.0390134 _diffrn_orient_matrix_ub_32 0.0188587 _diffrn_orient_matrix_ub_33 -0.0003704 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_unetI/netI 0.053 _diffrn_reflns_number 9451 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.33 _diffrn_reflns_theta_max 29.22 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.867 _reflns_number_total 4760 _reflns_number_gt 4405 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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. ; _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^)+(0.0335P)^2^+0.6461P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4760 _refine_ls_number_parameters 308 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.077 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.569(9) _refine_diff_density_max 1.401 _refine_diff_density_min -1.209 _refine_diff_density_rms 0.123 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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 0.40563(6) 0.23766(3) 0.94923(7) 0.02744(8) Uani 1 1 d . . . Cl1 Cl 0.4631(2) 0.2734(3) 0.8452(2) 0.0418(7) Uani 1 1 d . . . Cl2 Cl 0.3481(2) 0.2068(3) 1.0540(2) 0.0411(6) Uani 1 1 d . . . N1 N 0.2807(4) 0.4575(8) 0.9071(5) 0.0465(19) Uani 1 1 d . . . O1 O 0.2232(3) 0.4346(8) 0.9346(4) 0.069(2) Uani 1 1 d . . . O2 O 0.2790(4) 0.4431(10) 0.8404(4) 0.067(2) Uani 1 1 d . . . P1 P 0.64886(11) -0.11540(19) 1.19648(14) 0.0198(3) Uani 1 1 d . . . C1 C 0.4918(4) 0.0364(10) 0.9819(5) 0.049(2) Uani 1 1 d . . . H1A H 0.5397 0.0401 0.9572 0.059 Uiso 1 1 calc R . . H1B H 0.4985 0.0153 1.0326 0.059 Uiso 1 1 calc R . . C2 C 0.4340(5) -0.0511(9) 0.9492(5) 0.046(2) Uani 1 1 d . . . H2A H 0.4033 -0.1297 0.9787 0.055 Uiso 1 1 calc R . . H2B H 0.4444 -0.105 0.9035 0.055 Uiso 1 1 calc R . . C3 C 0.3503(4) 0.4827(9) 0.9362(5) 0.046(2) Uani 1 1 d . . . H3A H 0.3462 0.5426 0.9819 0.055 Uiso 1 1 calc R . . H3B H 0.3797 0.5622 0.906 0.055 Uiso 1 1 calc R . . C10 C 0.6144(10) -0.2533(8) 1.1235(9) 0.022(3) Uani 1 1 d U . . C11 C 0.5605(3) -0.3870(8) 1.1411(4) 0.0275(16) Uani 1 1 d U . . H11 H 0.5448 -0.402 1.1875 0.033 Uiso 1 1 calc R . . C12 C 0.5322(4) -0.4934(10) 1.0872(5) 0.0353(19) Uani 1 1 d U . . H12 H 0.4966 -0.5852 1.0964 0.042 Uiso 1 1 calc R . . C13 C 0.5559(4) -0.4663(9) 1.0193(5) 0.0343(18) Uani 1 1 d U . . H13 H 0.5347 -0.5362 0.9821 0.041 Uiso 1 1 calc R . . C14 C 0.6084(4) -0.3417(9) 1.0065(4) 0.0308(16) Uani 1 1 d U . . H14 H 0.627 -0.3284 0.9611 0.037 Uiso 1 1 calc R . . C15 C 0.6354(8) -0.2328(10) 1.0606(10) 0.025(3) Uani 1 1 d U . . H15 H 0.6704 -0.1402 1.0508 0.03 Uiso 1 1 calc R . . C20 C 0.5763(3) 0.0324(7) 1.2260(4) 0.0209(14) Uani 1 1 d . . . C21 C 0.5042(4) 0.0233(9) 1.1994(4) 0.0282(17) Uani 1 1 d . . . H21 H 0.4905 -0.0665 1.166 0.034 Uiso 1 1 calc R . . C22 C 0.4509(4) 0.1462(9) 1.2214(5) 0.0352(19) Uani 1 1 d . . . H22 H 0.4006 0.139 1.2034 0.042 Uiso 1 1 calc R . . C23 C 0.4704(9) 0.2795(13) 1.2697(11) 0.034(3) Uani 1 1 d . . . H23 H 0.4343 0.3654 1.2834 0.041 Uiso 1 1 calc R . . C24 C 0.5431(6) 0.2857(11) 1.2974(6) 0.029(2) Uani 1 1 d . . . H24 H 0.5561 0.3724 1.3322 0.034 Uiso 1 1 calc R . . C25 C 0.5978(4) 0.1655(8) 1.2747(4) 0.0249(15) Uani 1 1 d . . . H25 H 0.6483 0.1737 1.2919 0.03 Uiso 1 1 calc R . . C30 C 0.7221(3) 0.0312(8) 1.1672(4) 0.0211(14) Uani 1 1 d . . . C31 C 0.7957(3) 0.0100(8) 1.1896(4) 0.0260(16) Uani 1 1 d . . . H31 H 0.8096 -0.0862 1.2201 0.031 Uiso 1 1 calc R . . C32 C 0.8492(3) 0.1298(10) 1.1675(5) 0.0309(17) Uani 1 1 d . . . H32 H 0.8998 0.119 1.1843 0.037 Uiso 1 1 calc R . . C33 C 0.8299(8) 0.2635(10) 1.1218(9) 0.025(3) Uani 1 1 d . . . H33 H 0.8676 0.341 1.1048 0.03 Uiso 1 1 calc R . . C34 C 0.7557(6) 0.2874(12) 1.0998(6) 0.030(2) Uani 1 1 d . . . H34 H 0.7424 0.3845 1.0696 0.036 Uiso 1 1 calc R . . C35 C 0.7012(4) 0.1706(9) 1.1216(4) 0.0316(17) Uani 1 1 d . . . H35 H 0.6504 0.1844 1.1059 0.038 Uiso 1 1 calc R . . C40 C 0.6848(8) -0.2616(8) 1.2620(7) 0.016(2) Uani 1 1 d U . . C41 C 0.6598(8) -0.2432(8) 1.3333(10) 0.020(2) Uani 1 1 d U . . H41 H 0.6225 -0.1576 1.3448 0.024 Uiso 1 1 calc R . . C42 C 0.6924(4) -0.3548(9) 1.3838(5) 0.0329(17) Uani 1 1 d U . . H42 H 0.6798 -0.342 1.4312 0.04 Uiso 1 1 calc R . . C43 C 0.7442(4) -0.4870(9) 1.3642(5) 0.0338(18) Uani 1 1 d U . . H43 H 0.7658 -0.564 1.399 0.041 Uiso 1 1 calc R . . C44 C 0.7641(4) -0.5076(9) 1.2985(5) 0.0349(19) Uani 1 1 d U . . H44 H 0.7988 -0.5994 1.2872 0.042 Uiso 1 1 calc R . . C45 C 0.7347(4) -0.3966(8) 1.2464(5) 0.0310(16) Uani 1 1 d U . . H45 H 0.749 -0.4137 1.1997 0.037 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 Pt1 0.02369(12) 0.02111(11) 0.03727(16) -0.0005(3) -0.00280(9) -0.0041(2) Cl1 0.0373(13) 0.0426(13) 0.0459(18) 0.0073(16) 0.0063(11) 0.0007(14) Cl2 0.0469(14) 0.0365(11) 0.0403(17) 0.0021(17) 0.0078(11) -0.0003(16) N1 0.047(4) 0.027(3) 0.065(6) 0.014(4) -0.007(4) 0.006(3) O1 0.037(3) 0.075(4) 0.096(6) 0.056(4) 0.018(3) 0.015(3) O2 0.085(5) 0.070(5) 0.046(5) -0.002(4) -0.011(4) 0.023(4) P1 0.0187(7) 0.0164(7) 0.0245(9) 0.0003(7) 0.0018(6) -0.0008(6) C1 0.051(5) 0.039(4) 0.057(7) 0.021(4) -0.008(5) 0.019(4) C2 0.076(6) 0.021(3) 0.042(6) 0.007(4) 0.009(5) 0.016(3) C3 0.049(5) 0.020(3) 0.071(8) 0.006(4) 0.019(4) 0.004(3) C10 0.023(6) 0.017(4) 0.025(6) -0.003(3) -0.014(4) 0.002(2) C11 0.030(4) 0.021(3) 0.032(4) 0.000(3) 0.004(3) -0.005(3) C12 0.026(3) 0.030(4) 0.050(6) 0.001(4) -0.001(4) -0.012(3) C13 0.035(4) 0.030(4) 0.037(5) -0.010(4) -0.009(4) -0.001(3) C14 0.036(4) 0.030(3) 0.026(4) -0.006(3) 0.001(3) -0.003(3) C15 0.013(6) 0.025(4) 0.037(6) -0.003(4) -0.002(4) 0.001(3) C20 0.024(3) 0.019(3) 0.020(4) 0.002(3) 0.002(3) 0.001(2) C21 0.028(3) 0.028(3) 0.029(5) 0.000(3) 0.001(3) -0.005(3) C22 0.025(4) 0.034(4) 0.046(6) 0.003(4) -0.004(4) 0.009(3) C23 0.028(5) 0.032(4) 0.042(8) 0.001(6) -0.003(4) 0.012(5) C24 0.036(5) 0.023(3) 0.027(5) -0.008(4) 0.010(4) 0.009(4) C25 0.024(3) 0.023(3) 0.027(5) -0.004(3) -0.003(3) 0.002(3) C30 0.020(3) 0.021(3) 0.023(4) 0.001(3) 0.002(3) -0.004(2) C31 0.026(3) 0.022(3) 0.029(5) 0.006(3) 0.002(3) 0.002(3) C32 0.017(3) 0.034(4) 0.042(6) 0.002(4) 0.002(3) 0.002(3) C33 0.029(7) 0.023(4) 0.024(6) -0.002(4) 0.012(5) -0.013(4) C34 0.031(5) 0.025(4) 0.033(6) 0.002(5) -0.004(4) -0.003(4) C35 0.028(4) 0.026(3) 0.040(5) 0.002(3) -0.008(3) -0.003(3) C40 0.013(5) 0.022(4) 0.013(5) 0.002(3) -0.004(4) -0.003(2) C41 0.011(5) 0.025(4) 0.024(5) 0.001(3) 0.001(4) 0.001(2) C42 0.038(4) 0.029(3) 0.032(5) 0.006(3) -0.008(3) -0.010(3) C43 0.027(4) 0.030(3) 0.044(5) 0.016(3) -0.011(3) 0.000(3) C44 0.028(4) 0.030(4) 0.047(6) 0.012(3) 0.004(4) 0.006(3) C45 0.027(3) 0.028(3) 0.038(5) -0.003(3) 0.002(3) 0.007(3) #----------------------------------------------------------------------------# # 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 C3 2.078(7) . ? Pt1 C2 2.200(6) . ? Pt1 C1 2.217(7) . ? Pt1 Cl1 2.293(5) . ? Pt1 Cl2 2.301(5) . ? N1 O1 1.180(9) . ? N1 O2 1.286(10) . ? N1 C3 1.356(10) . ? P1 C40 1.765(11) . ? P1 C20 1.801(6) . ? P1 C30 1.803(6) . ? P1 C10 1.826(13) . ? C1 C2 1.354(11) . ? C10 C15 1.29(3) . ? C10 C11 1.429(16) . ? C11 C12 1.384(10) . ? C12 C13 1.400(12) . ? C13 C14 1.344(10) . ? C14 C15 1.389(17) . ? C20 C21 1.369(9) . ? C20 C25 1.406(9) . ? C21 C22 1.392(9) . ? C22 C23 1.392(18) . ? C23 C24 1.38(2) . ? C24 C25 1.400(10) . ? C30 C31 1.374(9) . ? C30 C35 1.399(10) . ? C31 C32 1.381(9) . ? C32 C33 1.361(14) . ? C33 C34 1.386(19) . ? C34 C35 1.376(12) . ? C40 C45 1.379(14) . ? C40 C41 1.46(2) . ? C41 C42 1.388(16) . ? C42 C43 1.406(10) . ? C43 C44 1.333(12) . ? C44 C45 1.386(10) . ? 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 C3 Pt1 C2 163.5(3) . . ? C3 Pt1 C1 160.7(3) . . ? C2 Pt1 C1 35.7(3) . . ? C3 Pt1 Cl1 91.0(3) . . ? C2 Pt1 Cl1 90.2(3) . . ? C1 Pt1 Cl1 90.0(3) . . ? C3 Pt1 Cl2 88.3(3) . . ? C2 Pt1 Cl2 90.7(3) . . ? C1 Pt1 Cl2 90.5(3) . . ? Cl1 Pt1 Cl2 179.06(11) . . ? O1 N1 O2 116.3(8) . . ? O1 N1 C3 129.1(10) . . ? O2 N1 C3 114.4(8) . . ? C40 P1 C20 113.3(6) . . ? C40 P1 C30 110.1(5) . . ? C20 P1 C30 105.4(3) . . ? C40 P1 C10 108.0(4) . . ? C20 P1 C10 110.9(6) . . ? C30 P1 C10 109.0(6) . . ? C2 C1 Pt1 71.5(4) . . ? C1 C2 Pt1 72.8(4) . . ? N1 C3 Pt1 110.6(5) . . ? C15 C10 C11 121.6(11) . . ? C15 C10 P1 123.7(11) . . ? C11 C10 P1 114.7(12) . . ? C12 C11 C10 116.7(9) . . ? C11 C12 C13 120.2(7) . . ? C14 C13 C12 120.1(7) . . ? C13 C14 C15 119.3(10) . . ? C10 C15 C14 122.0(12) . . ? C21 C20 C25 121.0(6) . . ? C21 C20 P1 121.8(5) . . ? C25 C20 P1 117.1(5) . . ? C20 C21 C22 119.6(7) . . ? C23 C22 C21 120.7(9) . . ? C24 C23 C22 119.4(12) . . ? C23 C24 C25 120.6(10) . . ? C24 C25 C20 118.6(7) . . ? C31 C30 C35 120.8(6) . . ? C31 C30 P1 121.7(5) . . ? C35 C30 P1 117.5(5) . . ? C30 C31 C32 119.4(6) . . ? C33 C32 C31 120.4(8) . . ? C32 C33 C34 120.5(11) . . ? C35 C34 C33 120.1(9) . . ? C34 C35 C30 118.7(7) . . ? C45 C40 C41 119.3(9) . . ? C45 C40 P1 120.8(11) . . ? C41 C40 P1 119.9(9) . . ? C42 C41 C40 117.9(10) . . ? C41 C42 C43 119.4(10) . . ? C44 C43 C42 122.1(7) . . ? C43 C44 C45 120.8(7) . . ? C40 C45 C44 120.4(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