# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '1_sanz.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2008-07-09 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Sanz Miguel, Pablo J.' _publ_contact_author_address ;Department of Inorganic Chemistry TU Dortmund University Otto-Hahn-Strasse 6 44227 Dortmund, Germany ; _publ_contact_author_email pablo.sanz@uni-dortmund.de _publ_contact_author_fax 49(231)7553797 _publ_contact_author_phone 49(231)7555034 _publ_requested_coeditor_name ? _publ_contact_letter ? _publ_requested_category FA #------------------ TITLE AND AUTHOR LIST------------------------------------# _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name 'Lars Holland' 'Wei-Zheng Shen.' 'P.von Grebe' 'Deepali Gupta' 'Pablo J. Sanz Miguel' ; Yuntao Huang ; 'Fabio Pichierri' 'Andreas Springer' 'Christoph A. Schalley' 'Bernhard Lippert' #Department of Inorganic Chemistry #TU Dortmund University #Otto-Hahn-Strasse 6 #44227 Dortmund, Germany #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_1 _database_code_depnum_ccdc_archive 'CCDC 794349' #TrackingRef '1_sanz.cif' _audit_creation_date 2008-07-09T16:43:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C8 H7 Cl2 N3 Pt, C3 H6 O' _chemical_formula_sum 'C11 H13 Cl2 N3 O Pt' _chemical_formula_weight 469.23 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9510(18) _cell_length_b 8.9970(18) _cell_length_c 9.6640(19) _cell_angle_alpha 102.00(3) _cell_angle_beta 98.89(3) _cell_angle_gamma 108.26(3) _cell_volume 702.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.5 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 10.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.356 _exptl_absorpt_correction_T_max 0.356 _exptl_absorpt_process_details sadabs #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 6032 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_max 0.808 _diffrn_measured_fraction_theta_full 0.808 _reflns_number_total 2611 _reflns_number_gt 1579 _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' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0147(19) _refine_ls_number_reflns 2611 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1497 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.547 _refine_diff_density_min -2.876 #------------------ 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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pt1 Pt 1.10204(8) 0.18962(8) 0.12413(7) 0.0350(3) Uani 1 d . . . Cl1 Cl 1.3020(5) 0.2615(7) 0.0033(5) 0.0578(13) Uani 1 d . . . Cl2 Cl 1.2639(5) 0.1228(6) 0.2891(5) 0.0519(12) Uani 1 d . . . N1 N 0.9125(17) 0.1386(17) 0.2179(14) 0.042(4) Uani 1 d . . . C2 C 0.780(2) 0.167(2) 0.150(2) 0.049(5) Uani 1 d . . . C3 C 0.635(2) 0.126(2) 0.195(2) 0.050(5) Uani 1 d . . . H1 H 0.5456 0.1414 0.1467 0.059 Uiso 1 calc R . . C4 C 0.629(2) 0.061(3) 0.312(2) 0.060(5) Uani 1 d . . . H2 H 0.5368 0.0392 0.3482 0.072 Uiso 1 calc R . . C5 C 0.758(2) 0.027(3) 0.374(2) 0.056(5) Uani 1 d . . . H3 H 0.7507 -0.0219 0.4498 0.068 Uiso 1 calc R . . C6 C 0.898(2) 0.066(2) 0.3263(18) 0.046(4) Uani 1 d . . . H4 H 0.9846 0.0417 0.3694 0.055 Uiso 1 calc R . . N1' N 0.9515(17) 0.3107(16) -0.1172(14) 0.040(3) Uani 1 d . . . H5 H 1.0302 0.3291 -0.1599 0.049 Uiso 1 calc R . . N2' N 0.9498(16) 0.2516(17) -0.0046(14) 0.040(3) Uani 1 d . . . C3' C 0.8011(18) 0.230(2) 0.0245(16) 0.034(3) Uani 1 d . . . C4' C 0.720(2) 0.288(2) -0.068(2) 0.052(5) Uani 1 d . . . H6 H 0.6177 0.2933 -0.0707 0.062 Uiso 1 calc R . . C5' C 0.821(2) 0.338(2) -0.1560(19) 0.051(5) Uani 1 d . . . H7 H 0.799 0.3833 -0.2311 0.061 Uiso 1 calc R . . C1A C 1.238(3) 0.445(3) 0.628(2) 0.061(5) Uani 1 d . . . C2A C 1.232(3) 0.512(3) 0.502(2) 0.071(6) Uani 1 d . . . H2AA H 1.1281 0.5206 0.4746 0.106 Uiso 1 calc R . . H2AB H 1.2496 0.4412 0.4219 0.106 Uiso 1 calc R . . H2AC H 1.315 0.6178 0.5267 0.106 Uiso 1 calc R . . C3A C 1.386(3) 0.424(3) 0.689(2) 0.077(7) Uani 1 d . . . H3AC H 1.3716 0.379 0.7704 0.115 Uiso 1 calc R . . H3AD H 1.473 0.5268 0.7213 0.115 Uiso 1 calc R . . H3AA H 1.4101 0.3505 0.6163 0.115 Uiso 1 calc R . . O1 O 1.122(2) 0.406(3) 0.6799(18) 0.087(5) Uani 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 0.0250(4) 0.0411(4) 0.0394(5) 0.0128(3) 0.0072(3) 0.0115(3) Cl1 0.035(2) 0.085(3) 0.069(3) 0.037(3) 0.026(2) 0.025(2) Cl2 0.038(2) 0.077(3) 0.053(3) 0.030(3) 0.011(2) 0.029(2) N1 0.047(9) 0.049(9) 0.052(9) 0.028(8) 0.024(7) 0.031(7) C2 0.027(9) 0.058(11) 0.074(13) 0.028(11) 0.020(9) 0.019(8) C3 0.042(10) 0.049(10) 0.073(13) 0.025(10) 0.028(10) 0.025(9) C4 0.041(11) 0.085(14) 0.080(14) 0.051(13) 0.045(10) 0.025(10) C5 0.046(11) 0.088(15) 0.048(11) 0.043(11) 0.020(9) 0.022(11) C6 0.035(10) 0.067(12) 0.042(10) 0.029(10) 0.012(8) 0.016(9) N1' 0.035(8) 0.046(8) 0.035(8) 0.013(7) 0.012(6) 0.005(7) N2' 0.037(8) 0.042(8) 0.046(9) 0.021(7) 0.011(7) 0.014(7) C3' 0.025(8) 0.043(9) 0.031(8) 0.006(8) 0.004(7) 0.014(7) C4' 0.046(11) 0.056(11) 0.074(13) 0.032(11) 0.016(10) 0.036(9) C5' 0.056(12) 0.066(13) 0.043(11) 0.024(10) 0.011(9) 0.033(11) C1A 0.062(14) 0.048(11) 0.077(15) 0.018(11) 0.026(12) 0.021(10) C2A 0.074(15) 0.090(17) 0.063(14) 0.028(13) 0.038(12) 0.034(14) C3A 0.059(15) 0.091(17) 0.061(15) 0.012(13) 0.004(12) 0.010(13) O1 0.067(10) 0.133(15) 0.081(11) 0.051(12) 0.034(9) 0.040(10) #------------------ 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 N2' 1.989(12) . ? Pt1 N1 2.017(13) . ? Pt1 Cl1 2.284(4) . ? Pt1 Cl2 2.287(4) . ? N1 C6 1.35(2) . ? N1 C2 1.39(2) . ? C2 C3 1.39(2) . ? C2 C3' 1.46(2) . ? C3 C4 1.38(3) . ? C3 H1 0.93 . ? C4 C5 1.36(3) . ? C4 H2 0.93 . ? C5 C6 1.37(2) . ? C5 H3 0.93 . ? C6 H4 0.93 . ? N1' C5' 1.28(2) . ? N1' N2' 1.307(17) . ? N1' H5 0.86 . ? N2' C3' 1.365(19) . ? C3' C4' 1.35(2) . ? C4' C5' 1.38(3) . ? C4' H6 0.93 . ? C5' H7 0.93 . ? C1A O1 1.21(3) . ? C1A C3A 1.44(3) . ? C1A C2A 1.47(3) . ? C2A H2AA 0.96 . ? C2A H2AB 0.96 . ? C2A H2AC 0.96 . ? C3A H3AC 0.96 . ? C3A H3AD 0.96 . ? C3A H3AA 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2' Pt1 N1 80.4(5) . . ? N2' Pt1 Cl1 93.3(4) . . ? N1 Pt1 Cl1 173.6(4) . . ? N2' Pt1 Cl2 174.5(4) . . ? N1 Pt1 Cl2 94.6(4) . . ? Cl1 Pt1 Cl2 91.68(16) . . ? C6 N1 C2 118.7(14) . . ? C6 N1 Pt1 126.5(11) . . ? C2 N1 Pt1 114.4(10) . . ? C3 C2 N1 121.2(16) . . ? C3 C2 C3' 123.9(15) . . ? N1 C2 C3' 114.7(14) . . ? C4 C3 C2 118.1(16) . . ? C4 C3 H1 121 . . ? C2 C3 H1 121 . . ? C3 C4 C5 120.3(15) . . ? C3 C4 H2 119.8 . . ? C5 C4 H2 119.8 . . ? C6 C5 C4 120.4(15) . . ? C6 C5 H3 119.8 . . ? C4 C5 H3 119.8 . . ? N1 C6 C5 121.1(15) . . ? N1 C6 H4 119.5 . . ? C5 C6 H4 119.5 . . ? C5' N1' N2' 111.6(14) . . ? C5' N1' H5 124.2 . . ? N2' N1' H5 124.2 . . ? N1' N2' C3' 106.6(12) . . ? N1' N2' Pt1 136.7(10) . . ? C3' N2' Pt1 116.8(10) . . ? C4' C3' N2' 107.9(14) . . ? C4' C3' C2 138.1(15) . . ? N2' C3' C2 113.7(12) . . ? C3' C4' C5' 105.5(15) . . ? C3' C4' H6 127.2 . . ? C5' C4' H6 127.2 . . ? N1' C5' C4' 108.3(14) . . ? N1' C5' H7 125.8 . . ? C4' C5' H7 125.8 . . ? O1 C1A C3A 120(2) . . ? O1 C1A C2A 121(2) . . ? C3A C1A C2A 119(2) . . ? C1A C2A H2AA 109.5 . . ? C1A C2A H2AB 109.5 . . ? H2AA C2A H2AB 109.5 . . ? C1A C2A H2AC 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? C1A C3A H3AC 109.5 . . ? C1A C3A H3AD 109.5 . . ? H3AC C3A H3AD 109.5 . . ? C1A C3A H3AA 109.5 . . ? H3AC C3A H3AA 109.5 . . ? H3AD C3A H3AA 109.5 . . ? 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 N2' Pt1 N1 C6 173.6(16) . . . . ? Cl2 Pt1 N1 C6 -8.7(15) . . . . ? N2' Pt1 N1 C2 1.1(13) . . . . ? Cl2 Pt1 N1 C2 178.8(13) . . . . ? C6 N1 C2 C3 2(3) . . . . ? Pt1 N1 C2 C3 174.9(15) . . . . ? C6 N1 C2 C3' -173.8(15) . . . . ? Pt1 N1 C2 C3' -1(2) . . . . ? N1 C2 C3 C4 2(3) . . . . ? C3' C2 C3 C4 177.3(18) . . . . ? C2 C3 C4 C5 -5(3) . . . . ? C3 C4 C5 C6 3(3) . . . . ? C2 N1 C6 C5 -3(3) . . . . ? Pt1 N1 C6 C5 -175.3(15) . . . . ? C4 C5 C6 N1 1(3) . . . . ? C5' N1' N2' C3' 4(2) . . . . ? C5' N1' N2' Pt1 -176.2(14) . . . . ? N1 Pt1 N2' N1' 179.0(17) . . . . ? Cl1 Pt1 N2' N1' 0.2(17) . . . . ? N1 Pt1 N2' C3' -1.3(12) . . . . ? Cl1 Pt1 N2' C3' 179.9(12) . . . . ? N1' N2' C3' C4' -4(2) . . . . ? Pt1 N2' C3' C4' 176.1(12) . . . . ? N1' N2' C3' C2 -178.9(14) . . . . ? Pt1 N2' C3' C2 1.3(19) . . . . ? C3 C2 C3' C4' 12(4) . . . . ? N1 C2 C3' C4' -173(2) . . . . ? C3 C2 C3' N2' -175.8(18) . . . . ? N1 C2 C3' N2' 0(2) . . . . ? N2' C3' C4' C5' 3(2) . . . . ? C2 C3' C4' C5' 176(2) . . . . ? N2' N1' C5' C4' -2(2) . . . . ? C3' C4' C5' N1' 0(2) . . . . ? # Attachment '2_sanz.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-07-30 at 15:00:03 # 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 794350' #TrackingRef '2_sanz.cif' _audit_creation_date 2010-07-30T15:00:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H12 N6 Pt' _chemical_formula_sum 'C16 H12 N6 Pt' _chemical_formula_weight 483.41 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7035(3) _cell_length_b 13.2662(5) _cell_length_c 16.4753(5) _cell_angle_alpha 90 _cell_angle_beta 99.019(3) _cell_angle_gamma 90 _cell_volume 2094.62(12) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6134 _cell_measurement_theta_min 1.981 _cell_measurement_theta_max 29.2324 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cubes _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 10.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.191 _exptl_absorpt_correction_T_max 0.221 _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 0.0392 _diffrn_reflns_av_unetI/netI 0.0689 _diffrn_reflns_number 13174 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 29.2 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.853 _reflns_number_total 4842 _reflns_number_gt 3582 _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. ; _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^)+(0.0134P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4842 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.046 _refine_ls_wR_factor_gt 0.0446 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.282 _refine_diff_density_min -1.135 _refine_diff_density_rms 0.176 #----------------------------------------------------------------------------# # 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' 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 0 0 0.01549(8) Uani 1 2 d S . . Pt2 Pt 0.04578(2) 0.173079(15) 0.145478(12) 0.01558(6) Uani 1 1 d . . . N1 N -0.1464(4) -0.0667(3) 0.0578(2) 0.0181(10) Uani 1 1 d . . . C2 C -0.0976(5) -0.1367(4) 0.1153(3) 0.0209(12) Uani 1 1 d . . . C3 C -0.1859(5) -0.1887(4) 0.1590(3) 0.0297(15) Uani 1 1 d . . . H3 H -0.1499 -0.2367 0.1996 0.036 Uiso 1 1 calc R . . C4 C -0.3272(5) -0.1692(5) 0.1424(3) 0.0317(14) Uani 1 1 d . . . H4 H -0.3895 -0.2046 0.1713 0.038 Uiso 1 1 calc R . . C5 C -0.3777(5) -0.0992(4) 0.0844(3) 0.0244(13) Uani 1 1 d . . . H5 H -0.4748 -0.0854 0.0727 0.029 Uiso 1 1 calc R . . C6 C -0.2848(5) -0.0490(4) 0.0430(3) 0.0217(13) Uani 1 1 d . . . H6 H -0.3199 -0.0002 0.0028 0.026 Uiso 1 1 calc R . . N1' N 0.2572(4) -0.1158(3) 0.0868(3) 0.0215(11) Uani 1 1 d . . . N2' N 0.1189(4) -0.0952(3) 0.0744(3) 0.0187(10) Uani 1 1 d . . . C3' C 0.0505(5) -0.1499(4) 0.1235(3) 0.0202(13) Uani 1 1 d . . . C4' C 0.1479(5) -0.2127(4) 0.1714(3) 0.0267(14) Uani 1 1 d . . . H4' H 0.1316 -0.2611 0.2113 0.032 Uiso 1 1 calc R . . C5' C 0.2730(6) -0.1871(4) 0.1465(3) 0.0284(14) Uani 1 1 d . . . H5' H 0.3602 -0.2162 0.1688 0.034 Uiso 1 1 calc R . . N1A N -0.1315(4) 0.2444(3) 0.0933(2) 0.0153(10) Uani 1 1 d . . . C2A C -0.1150(5) 0.3131(4) 0.0346(3) 0.0167(12) Uani 1 1 d . . . C3A C -0.2284(5) 0.3643(4) -0.0082(3) 0.0236(13) Uani 1 1 d . . . H3A H -0.2149 0.4146 -0.0472 0.028 Uiso 1 1 calc R . . C4A C -0.3602(5) 0.3415(4) 0.0065(3) 0.0297(14) Uani 1 1 d . . . H4A H -0.4391 0.3745 -0.0233 0.036 Uiso 1 1 calc R . . C5A C -0.3770(5) 0.2701(4) 0.0651(3) 0.0275(14) Uani 1 1 d . . . H5A H -0.4675 0.2539 0.0763 0.033 Uiso 1 1 calc R . . C6A C -0.2611(5) 0.2227(4) 0.1071(3) 0.0249(13) Uani 1 1 d . . . H6A H -0.2731 0.1731 0.147 0.03 Uiso 1 1 calc R . . N1A' N 0.2525(4) 0.2847(3) 0.0525(3) 0.0203(10) Uani 1 1 d . . . N2A' N 0.1236(4) 0.2657(3) 0.0688(2) 0.0140(10) Uani 1 1 d . . . C3A' C 0.0301(5) 0.3256(4) 0.0238(3) 0.0220(12) Uani 1 1 d . . . C4A' C 0.0986(5) 0.3887(4) -0.0249(3) 0.0226(13) Uani 1 1 d . . . H4A' H 0.0605 0.4392 -0.0628 0.027 Uiso 1 1 calc R . . C5A' C 0.2365(5) 0.3584(4) -0.0040(3) 0.0241(13) Uani 1 1 d . . . H5A' H 0.3115 0.3868 -0.0271 0.029 Uiso 1 1 calc R . . N1B N 0.2222(4) 0.0992(3) 0.1954(2) 0.0149(10) Uani 1 1 d . . . C2B C 0.2052(5) 0.0341(4) 0.2565(3) 0.0193(12) Uani 1 1 d . . . C3B C 0.3187(5) -0.0230(4) 0.2963(3) 0.0230(13) Uani 1 1 d . . . H3B H 0.3066 -0.0695 0.3385 0.028 Uiso 1 1 calc R . . C4B C 0.4469(5) -0.0097(4) 0.2728(3) 0.0275(14) Uani 1 1 d . . . H4B H 0.5251 -0.0463 0.2997 0.033 Uiso 1 1 calc R . . C5B C 0.4629(5) 0.0561(4) 0.2105(3) 0.0230(13) Uani 1 1 d . . . H5B H 0.5512 0.0654 0.1937 0.028 Uiso 1 1 calc R . . C6B C 0.3473(5) 0.1080(4) 0.1732(3) 0.0218(13) Uani 1 1 d . . . H6B H 0.3576 0.1524 0.1294 0.026 Uiso 1 1 calc R . . N1B' N -0.1564(4) 0.0771(3) 0.2503(3) 0.0243(11) Uani 1 1 d . . . N2B' N -0.0302(4) 0.0873(3) 0.2280(2) 0.0193(10) Uani 1 1 d . . . C3B' C 0.0654(5) 0.0301(4) 0.2749(3) 0.0212(13) Uani 1 1 d . . . C4B' C -0.0012(5) -0.0224(4) 0.3312(3) 0.0245(14) Uani 1 1 d . . . H4B' H 0.0378 -0.0691 0.3722 0.029 Uiso 1 1 calc R . . C5B' C -0.1389(6) 0.0106(4) 0.3125(3) 0.0310(15) Uani 1 1 d . . . H5B' H -0.2119 -0.0114 0.3406 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 0.01412(15) 0.01446(16) 0.01783(16) -0.00196(14) 0.00226(11) 0.00068(13) Pt2 0.01288(10) 0.01622(12) 0.01823(10) -0.00252(10) 0.00428(7) -0.00126(10) N1 0.014(2) 0.019(3) 0.020(2) -0.011(2) 0.0003(19) 0.000(2) C2 0.024(3) 0.016(3) 0.022(3) -0.005(2) 0.002(2) 0.000(3) C3 0.029(3) 0.033(4) 0.029(3) 0.005(3) 0.009(3) 0.007(3) C4 0.021(3) 0.037(4) 0.039(4) -0.001(3) 0.011(3) -0.001(3) C5 0.015(3) 0.024(3) 0.036(4) -0.004(3) 0.007(2) -0.002(3) C6 0.022(3) 0.018(3) 0.024(3) -0.008(2) 0.000(2) 0.007(3) N1' 0.014(2) 0.025(3) 0.024(3) -0.006(2) -0.0021(19) 0.003(2) N2' 0.018(2) 0.016(3) 0.020(3) 0.000(2) -0.0017(19) -0.003(2) C3' 0.022(3) 0.015(3) 0.023(3) -0.001(2) 0.002(2) -0.001(2) C4' 0.023(3) 0.032(4) 0.026(3) 0.004(3) 0.007(3) -0.001(3) C5' 0.023(3) 0.026(4) 0.036(4) 0.005(3) 0.002(3) 0.006(3) N1A 0.012(2) 0.011(2) 0.024(3) -0.0025(19) 0.0049(18) 0.0004(19) C2A 0.017(3) 0.011(3) 0.022(3) -0.001(2) 0.003(2) -0.002(2) C3A 0.022(3) 0.026(3) 0.024(3) 0.000(3) 0.006(2) -0.002(3) C4A 0.017(3) 0.027(4) 0.044(4) -0.001(3) 0.003(3) 0.003(3) C5A 0.013(3) 0.031(4) 0.041(4) -0.001(3) 0.010(3) 0.001(3) C6A 0.024(3) 0.025(3) 0.027(3) -0.007(3) 0.009(3) 0.000(3) N1A' 0.015(2) 0.023(3) 0.025(3) -0.001(2) 0.0076(19) -0.003(2) N2A' 0.009(2) 0.013(2) 0.021(2) -0.0033(19) 0.0030(18) -0.0044(18) C3A' 0.020(3) 0.023(3) 0.021(3) -0.002(3) 0.000(2) 0.001(3) C4A' 0.023(3) 0.019(3) 0.026(3) 0.008(3) 0.004(2) -0.003(3) C5A' 0.019(3) 0.028(3) 0.028(3) 0.001(3) 0.011(2) -0.004(3) N1B 0.015(2) 0.015(2) 0.016(2) -0.0026(19) 0.0049(18) -0.0021(19) C2B 0.026(3) 0.013(3) 0.019(3) -0.003(2) 0.001(2) -0.006(2) C3B 0.021(3) 0.027(4) 0.021(3) 0.002(3) 0.001(2) -0.002(3) C4B 0.020(3) 0.028(4) 0.031(3) -0.006(3) -0.005(2) 0.001(3) C5B 0.015(3) 0.021(3) 0.035(3) -0.007(3) 0.008(2) -0.002(2) C6B 0.022(3) 0.022(3) 0.021(3) -0.005(2) 0.004(2) -0.011(3) N1B' 0.015(2) 0.031(3) 0.029(3) 0.002(2) 0.009(2) -0.003(2) N2B' 0.016(2) 0.023(3) 0.021(3) -0.003(2) 0.0070(19) -0.002(2) C3B' 0.014(3) 0.027(3) 0.022(3) 0.001(2) 0.000(2) 0.005(2) C4B' 0.020(3) 0.031(4) 0.024(3) 0.006(3) 0.005(2) 0.001(3) C5B' 0.027(3) 0.044(4) 0.024(3) -0.001(3) 0.011(3) -0.010(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 N2' 1.996(4) 3 ? Pt1 N2' 1.996(4) . ? Pt1 N1 2.033(4) 3 ? Pt1 N1 2.033(4) . ? Pt2 N2A' 1.994(4) . ? Pt2 N2B' 2.001(4) . ? Pt2 N1B 2.032(4) . ? Pt2 N1A 2.033(4) . ? N1 C6 1.347(6) . ? N1 C2 1.358(6) . ? C2 C3 1.386(7) . ? C2 C3' 1.433(7) . ? C3 C4 1.379(7) . ? C3 H3 0.95 . ? C4 C5 1.367(7) . ? C4 H4 0.95 . ? C5 C6 1.383(7) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? N1' N2' 1.353(5) . ? N1' C5' 1.356(6) . ? N2' C3' 1.338(6) . ? C3' C4' 1.406(7) . ? C4' C5' 1.383(7) . ? C4' H4' 0.95 . ? C5' H5' 0.95 . ? N1A C6A 1.344(6) . ? N1A C2A 1.356(6) . ? C2A C3A 1.388(6) . ? C2A C3A' 1.456(6) . ? C3A C4A 1.372(7) . ? C3A H3A 0.95 . ? C4A C5A 1.379(7) . ? C4A H4A 0.95 . ? C5A C6A 1.377(7) . ? C5A H5A 0.95 . ? C6A H6A 0.95 . ? N1A' N2A' 1.343(5) . ? N1A' C5A' 1.342(6) . ? N2A' C3A' 1.340(6) . ? C3A' C4A' 1.398(7) . ? C4A' C5A' 1.388(7) . ? C4A' H4A' 0.95 . ? C5A' H5A' 0.95 . ? N1B C6B 1.326(6) . ? N1B C2B 1.356(6) . ? C2B C3B 1.411(7) . ? C2B C3B' 1.437(7) . ? C3B C4B 1.370(7) . ? C3B H3B 0.95 . ? C4B C5B 1.375(7) . ? C4B H4B 0.95 . ? C5B C6B 1.376(7) . ? C5B H5B 0.95 . ? C6B H6B 0.95 . ? N1B' N2B' 1.339(5) . ? N1B' C5B' 1.343(7) . ? N2B' C3B' 1.345(6) . ? C3B' C4B' 1.396(7) . ? C4B' C5B' 1.394(7) . ? C4B' H4B' 0.95 . ? C5B' H5B' 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 N2' Pt1 N2' 180 3 . ? N2' Pt1 N1 79.41(17) 3 3 ? N2' Pt1 N1 100.59(17) . 3 ? N2' Pt1 N1 100.59(17) 3 . ? N2' Pt1 N1 79.41(17) . . ? N1 Pt1 N1 180 3 . ? N2A' Pt2 N2B' 176.23(16) . . ? N2A' Pt2 N1B 100.07(16) . . ? N2B' Pt2 N1B 80.05(16) . . ? N2A' Pt2 N1A 79.91(16) . . ? N2B' Pt2 N1A 100.07(17) . . ? N1B Pt2 N1A 178.60(16) . . ? C6 N1 C2 118.3(5) . . ? C6 N1 Pt1 126.1(4) . . ? C2 N1 Pt1 115.6(3) . . ? N1 C2 C3 121.7(5) . . ? N1 C2 C3' 112.6(5) . . ? C3 C2 C3' 125.7(5) . . ? C4 C3 C2 118.7(5) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C5 C4 C3 120.1(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 118.8(5) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? N1 C6 C5 122.3(5) . . ? N1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? N2' N1' C5' 104.3(4) . . ? C3' N2' N1' 111.9(4) . . ? C3' N2' Pt1 114.8(3) . . ? N1' N2' Pt1 133.2(3) . . ? N2' C3' C4' 107.9(5) . . ? N2' C3' C2 117.6(5) . . ? C4' C3' C2 134.5(5) . . ? C5' C4' C3' 103.4(5) . . ? C5' C4' H4' 128.3 . . ? C3' C4' H4' 128.3 . . ? N1' C5' C4' 112.4(5) . . ? N1' C5' H5' 123.8 . . ? C4' C5' H5' 123.8 . . ? C6A N1A C2A 118.9(4) . . ? C6A N1A Pt2 125.5(4) . . ? C2A N1A Pt2 115.3(3) . . ? N1A C2A C3A 121.2(5) . . ? N1A C2A C3A' 112.9(4) . . ? C3A C2A C3A' 125.9(5) . . ? C4A C3A C2A 119.3(5) . . ? C4A C3A H3A 120.4 . . ? C2A C3A H3A 120.4 . . ? C3A C4A C5A 119.4(5) . . ? C3A C4A H4A 120.3 . . ? C5A C4A H4A 120.3 . . ? C6A C5A C4A 119.2(5) . . ? C6A C5A H5A 120.4 . . ? C4A C5A H5A 120.4 . . ? N1A C6A C5A 121.9(5) . . ? N1A C6A H6A 119 . . ? C5A C6A H6A 119 . . ? N2A' N1A' C5A' 105.4(4) . . ? N1A' N2A' C3A' 110.4(4) . . ? N1A' N2A' Pt2 134.4(3) . . ? C3A' N2A' Pt2 115.2(3) . . ? N2A' C3A' C4A' 109.3(4) . . ? N2A' C3A' C2A 116.7(5) . . ? C4A' C3A' C2A 134.0(5) . . ? C5A' C4A' C3A' 102.2(4) . . ? C5A' C4A' H4A' 128.9 . . ? C3A' C4A' H4A' 128.9 . . ? N1A' C5A' C4A' 112.6(5) . . ? N1A' C5A' H5A' 123.7 . . ? C4A' C5A' H5A' 123.7 . . ? C6B N1B C2B 118.9(4) . . ? C6B N1B Pt2 126.6(4) . . ? C2B N1B Pt2 114.5(3) . . ? N1B C2B C3B 120.7(5) . . ? N1B C2B C3B' 114.2(4) . . ? C3B C2B C3B' 125.2(5) . . ? C4B C3B C2B 118.5(5) . . ? C4B C3B H3B 120.8 . . ? C2B C3B H3B 120.8 . . ? C3B C4B C5B 120.4(5) . . ? C3B C4B H4B 119.8 . . ? C5B C4B H4B 119.8 . . ? C6B C5B C4B 118.1(5) . . ? C6B C5B H5B 120.9 . . ? C4B C5B H5B 120.9 . . ? N1B C6B C5B 123.4(5) . . ? N1B C6B H6B 118.3 . . ? C5B C6B H6B 118.3 . . ? N2B' N1B' C5B' 105.3(4) . . ? N1B' N2B' C3B' 111.3(4) . . ? N1B' N2B' Pt2 133.9(3) . . ? C3B' N2B' Pt2 114.7(3) . . ? N2B' C3B' C4B' 108.3(5) . . ? N2B' C3B' C2B 116.5(5) . . ? C4B' C3B' C2B 135.2(5) . . ? C5B' C4B' C3B' 102.9(5) . . ? C5B' C4B' H4B' 128.5 . . ? C3B' C4B' H4B' 128.5 . . ? N1B' C5B' C4B' 112.2(5) . . ? N1B' C5B' H5B' 123.9 . . ? C4B' C5B' H5B' 123.9 . . ? 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 N2' Pt1 N1 C6 2.3(4) 3 . . . ? N2' Pt1 N1 C6 -177.7(4) . . . . ? N2' Pt1 N1 C2 -179.0(3) 3 . . . ? N2' Pt1 N1 C2 1.0(3) . . . . ? C6 N1 C2 C3 -0.6(7) . . . . ? Pt1 N1 C2 C3 -179.5(4) . . . . ? C6 N1 C2 C3' 178.6(4) . . . . ? Pt1 N1 C2 C3' -0.3(5) . . . . ? N1 C2 C3 C4 0.9(8) . . . . ? C3' C2 C3 C4 -178.2(5) . . . . ? C2 C3 C4 C5 -0.6(8) . . . . ? C3 C4 C5 C6 0.2(8) . . . . ? C2 N1 C6 C5 0.1(7) . . . . ? Pt1 N1 C6 C5 178.8(4) . . . . ? C4 C5 C6 N1 0.1(8) . . . . ? C5' N1' N2' C3' 0.2(5) . . . . ? C5' N1' N2' Pt1 179.2(4) . . . . ? N1 Pt1 N2' C3' 178.4(4) 3 . . . ? N1 Pt1 N2' C3' -1.6(4) . . . . ? N1 Pt1 N2' N1' -0.6(4) 3 . . . ? N1 Pt1 N2' N1' 179.4(4) . . . . ? N1' N2' C3' C4' -1.0(6) . . . . ? Pt1 N2' C3' C4' 179.8(3) . . . . ? N1' N2' C3' C2 -178.8(4) . . . . ? Pt1 N2' C3' C2 2.0(6) . . . . ? N1 C2 C3' N2' -1.2(7) . . . . ? C3 C2 C3' N2' 178.0(5) . . . . ? N1 C2 C3' C4' -178.2(6) . . . . ? C3 C2 C3' C4' 1.0(10) . . . . ? N2' C3' C4' C5' 1.3(6) . . . . ? C2 C3' C4' C5' 178.5(6) . . . . ? N2' N1' C5' C4' 0.7(6) . . . . ? C3' C4' C5' N1' -1.2(6) . . . . ? N2A' Pt2 N1A C6A 175.5(4) . . . . ? N2B' Pt2 N1A C6A -8.3(4) . . . . ? N2A' Pt2 N1A C2A 1.7(3) . . . . ? N2B' Pt2 N1A C2A 177.9(3) . . . . ? C6A N1A C2A C3A 3.2(7) . . . . ? Pt2 N1A C2A C3A 177.5(4) . . . . ? C6A N1A C2A C3A' -177.4(4) . . . . ? Pt2 N1A C2A C3A' -3.1(5) . . . . ? N1A C2A C3A C4A -3.2(8) . . . . ? C3A' C2A C3A C4A 177.5(5) . . . . ? C2A C3A C4A C5A 1.8(8) . . . . ? C3A C4A C5A C6A -0.5(8) . . . . ? C2A N1A C6A C5A -1.9(8) . . . . ? Pt2 N1A C6A C5A -175.5(4) . . . . ? C4A C5A C6A N1A 0.6(8) . . . . ? C5A' N1A' N2A' C3A' 0.1(5) . . . . ? C5A' N1A' N2A' Pt2 -177.9(4) . . . . ? N1B Pt2 N2A' N1A' -3.3(5) . . . . ? N1A Pt2 N2A' N1A' 178.1(5) . . . . ? N1B Pt2 N2A' C3A' 178.8(3) . . . . ? N1A Pt2 N2A' C3A' 0.2(3) . . . . ? N1A' N2A' C3A' C4A' -0.3(6) . . . . ? Pt2 N2A' C3A' C4A' 178.1(3) . . . . ? N1A' N2A' C3A' C2A 179.6(4) . . . . ? Pt2 N2A' C3A' C2A -2.0(6) . . . . ? N1A C2A C3A' N2A' 3.4(7) . . . . ? C3A C2A C3A' N2A' -177.2(5) . . . . ? N1A C2A C3A' C4A' -176.7(5) . . . . ? C3A C2A C3A' C4A' 2.7(10) . . . . ? N2A' C3A' C4A' C5A' 0.5(6) . . . . ? C2A C3A' C4A' C5A' -179.5(6) . . . . ? N2A' N1A' C5A' C4A' 0.3(6) . . . . ? C3A' C4A' C5A' N1A' -0.5(6) . . . . ? N2A' Pt2 N1B C6B -5.8(4) . . . . ? N2B' Pt2 N1B C6B 178.0(4) . . . . ? N2A' Pt2 N1B C2B 175.2(3) . . . . ? N2B' Pt2 N1B C2B -1.0(3) . . . . ? C6B N1B C2B C3B 0.4(7) . . . . ? Pt2 N1B C2B C3B 179.5(4) . . . . ? C6B N1B C2B C3B' -179.5(4) . . . . ? Pt2 N1B C2B C3B' -0.5(5) . . . . ? N1B C2B C3B C4B 1.1(7) . . . . ? C3B' C2B C3B C4B -178.9(5) . . . . ? C2B C3B C4B C5B -1.5(8) . . . . ? C3B C4B C5B C6B 0.3(8) . . . . ? C2B N1B C6B C5B -1.7(7) . . . . ? Pt2 N1B C6B C5B 179.3(4) . . . . ? C4B C5B C6B N1B 1.4(8) . . . . ? C5B' N1B' N2B' C3B' -0.6(6) . . . . ? C5B' N1B' N2B' Pt2 -176.9(4) . . . . ? N1B Pt2 N2B' N1B' 178.6(5) . . . . ? N1A Pt2 N2B' N1B' -2.9(5) . . . . ? N1B Pt2 N2B' C3B' 2.4(4) . . . . ? N1A Pt2 N2B' C3B' -179.0(4) . . . . ? N1B' N2B' C3B' C4B' 0.8(6) . . . . ? Pt2 N2B' C3B' C4B' 177.8(3) . . . . ? N1B' N2B' C3B' C2B 179.6(4) . . . . ? Pt2 N2B' C3B' C2B -3.4(6) . . . . ? N1B C2B C3B' N2B' 2.5(7) . . . . ? C3B C2B C3B' N2B' -177.4(5) . . . . ? N1B C2B C3B' C4B' -179.1(6) . . . . ? C3B C2B C3B' C4B' 0.9(10) . . . . ? N2B' C3B' C4B' C5B' -0.6(6) . . . . ? C2B C3B' C4B' C5B' -179.0(6) . . . . ? N2B' N1B' C5B' C4B' 0.3(6) . . . . ? C3B' C4B' C5B' N1B' 0.2(6) . . . . ? # 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 '3_sanz.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-08-02 at 15:57:34 # 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 794351' #TrackingRef '3_sanz.cif' _audit_creation_date 2010-08-02T15:57:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H8 Cl6 N6 Pt, 2(C H Cl3)' _chemical_formula_sum 'C18 H10 Cl12 N6 Pt' _chemical_formula_weight 930.81 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.148(2) _cell_length_b 10.370(2) _cell_length_c 13.577(3) _cell_angle_alpha 90 _cell_angle_beta 97.78(3) _cell_angle_gamma 90 _cell_volume 1415.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7663 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cubes _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.112 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.1759 _diffrn_reflns_av_unetI/netI 0.2159 _diffrn_reflns_number 7663 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 3217 _reflns_number_gt 1579 _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. ; _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^)+(0.1003P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3217 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1808 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.2126 _refine_ls_wR_factor_gt 0.171 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.937 _refine_diff_density_min -2.71 _refine_diff_density_rms 0.311 #----------------------------------------------------------------------------# # 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' 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 0.5 0 0 0.03312(11) Uani 1 2 d S . . Cl1 Cl 0.4031(2) -0.1381(2) -0.12274(15) 0.0481(6) Uani 1 1 d . . . N1' N 0.6816(7) 0.1087(6) -0.1430(4) 0.045(2) Uani 1 1 d . . . N2' N 0.6519(7) 0.0231(5) -0.0735(5) 0.041(2) Uani 1 1 d . . . C3' C 0.7587(9) -0.0625(7) -0.0525(5) 0.039(2) Uani 1 1 d . . . C4' C 0.8535(8) -0.0271(7) -0.1104(6) 0.033(2) Uani 1 1 d . . . Cl4 Cl 1.0049(2) -0.0973(2) -0.11548(16) 0.0519(7) Uani 1 1 d . . . C5' C 0.8024(8) 0.0783(8) -0.1651(5) 0.038(2) Uani 1 1 d . . . Cl5' Cl 0.8714(3) 0.1670(2) -0.24819(17) 0.0597(7) Uani 1 1 d . . . N1 N 0.6239(6) -0.1428(6) 0.0607(4) 0.0320(18) Uani 1 1 d . . . C2 C 0.7405(8) -0.1540(7) 0.0241(6) 0.032(2) Uani 1 1 d . . . C3 C 0.8336(8) -0.2459(7) 0.0646(6) 0.038(2) Uani 1 1 d . . . H3 H 0.9157 -0.2509 0.0415 0.045 Uiso 1 1 calc R . . C4 C 0.8061(8) -0.3270(7) 0.1364(6) 0.042(2) Uani 1 1 d . . . H4 H 0.8679 -0.3884 0.1628 0.051 Uiso 1 1 calc R . . C5 C 0.6880(9) -0.3172(8) 0.1689(6) 0.053(3) Uani 1 1 d . . . H5 H 0.6675 -0.3759 0.2164 0.064 Uiso 1 1 calc R . . C6 C 0.5920(10) -0.2219(7) 0.1346(7) 0.051(3) Uani 1 1 d . . . H6 H 0.5123 -0.2138 0.1608 0.061 Uiso 1 1 calc R . . C10 C 0.2807(10) 0.5398(10) 0.1231(7) 0.064(3) Uani 1 1 d . . . H10 H 0.3115 0.604 0.174 0.076 Uiso 1 1 calc R A 1 Cl12 Cl 0.4094(3) 0.4340(4) 0.1179(3) 0.0965(12) Uani 1 1 d . B . Cl13 Cl 0.1476(4) 0.4590(4) 0.1636(3) 0.1066(12) Uani 1 1 d . B . Cl14 Cl 0.2721(6) 0.6156(6) 0.0105(4) 0.0707(16) Uiso 0.504(5) 1 d P B 1 Cl15 Cl 0.2013(6) 0.6130(5) 0.0127(4) 0.0633(15) Uiso 0.496(5) 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 0.0464(2) 0.02559(19) 0.02564(19) 0.0043(2) -0.00131(17) 0.0003(3) Cl1 0.0675(15) 0.0369(11) 0.0354(11) -0.0035(10) -0.0088(11) -0.0023(11) N1' 0.080(5) 0.032(3) 0.021(3) 0.010(3) 0.006(3) -0.003(4) N2' 0.060(4) 0.027(4) 0.032(3) -0.010(3) -0.005(3) -0.016(3) C3' 0.056(5) 0.029(4) 0.030(4) -0.006(4) -0.001(4) -0.007(4) C4' 0.030(4) 0.038(5) 0.029(4) -0.012(4) 0.000(3) 0.001(3) Cl4 0.0578(14) 0.0546(13) 0.0437(12) -0.0065(12) 0.0085(11) 0.0116(12) C5' 0.044(5) 0.043(5) 0.027(4) 0.005(4) 0.009(4) 0.009(4) Cl5' 0.0809(17) 0.0510(13) 0.0505(13) 0.0121(12) 0.0208(12) 0.0038(13) N1 0.037(4) 0.035(3) 0.023(3) 0.003(3) 0.000(3) -0.004(3) C2 0.037(5) 0.019(4) 0.038(4) -0.003(4) -0.009(4) -0.004(3) C3 0.024(4) 0.047(5) 0.043(5) -0.001(4) 0.006(4) 0.001(4) C4 0.046(5) 0.029(4) 0.054(5) -0.005(4) 0.012(4) 0.016(4) C5 0.061(6) 0.039(5) 0.054(5) 0.025(4) -0.016(5) 0.017(4) C6 0.066(6) 0.037(5) 0.047(5) 0.001(5) 0.000(5) 0.004(5) C10 0.080(7) 0.064(6) 0.050(5) -0.002(5) 0.019(5) -0.009(6) Cl12 0.091(2) 0.107(2) 0.091(2) -0.020(2) 0.0129(19) 0.005(2) Cl13 0.097(2) 0.103(2) 0.130(3) -0.003(2) 0.050(2) -0.014(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 Pt1 N2' 1.961(7) 3_655 ? Pt1 N2' 1.961(7) . ? Pt1 N1 2.042(6) 3_655 ? Pt1 N1 2.042(6) . ? Pt1 Cl1 2.313(2) . ? Pt1 Cl1 2.313(2) 3_655 ? N1' C5' 1.338(11) . ? N1' N2' 1.359(9) . ? N2' C3' 1.400(10) . ? C3' C4' 1.372(12) . ? C3' C2 1.439(11) . ? C4' C5' 1.383(10) . ? C4' Cl4 1.710(8) . ? C5' Cl5' 1.680(8) . ? N1 C2 1.350(10) . ? N1 C6 1.368(11) . ? C2 C3 1.401(10) . ? C3 C4 1.346(11) . ? C3 H3 0.93 . ? C4 C5 1.336(12) . ? C4 H4 0.93 . ? C5 C6 1.421(12) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C10 Cl14 1.710(11) . ? C10 Cl12 1.715(11) . ? C10 Cl13 1.741(11) . ? C10 Cl15 1.773(11) . ? C10 H10 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2' Pt1 N2' 180 3_655 . ? N2' Pt1 N1 79.1(2) 3_655 3_655 ? N2' Pt1 N1 100.9(2) . 3_655 ? N2' Pt1 N1 100.9(2) 3_655 . ? N2' Pt1 N1 79.1(2) . . ? N1 Pt1 N1 180 3_655 . ? N2' Pt1 Cl1 90.26(18) 3_655 . ? N2' Pt1 Cl1 89.74(18) . . ? N1 Pt1 Cl1 88.84(17) 3_655 . ? N1 Pt1 Cl1 91.16(17) . . ? N2' Pt1 Cl1 89.74(18) 3_655 3_655 ? N2' Pt1 Cl1 90.26(18) . 3_655 ? N1 Pt1 Cl1 91.16(17) 3_655 3_655 ? N1 Pt1 Cl1 88.84(17) . 3_655 ? Cl1 Pt1 Cl1 180 . 3_655 ? C5' N1' N2' 107.3(6) . . ? N1' N2' C3' 108.5(7) . . ? N1' N2' Pt1 134.2(5) . . ? C3' N2' Pt1 117.3(5) . . ? C4' C3' N2' 107.3(6) . . ? C4' C3' C2 139.4(8) . . ? N2' C3' C2 113.2(7) . . ? C3' C4' C5' 106.1(7) . . ? C3' C4' Cl4 127.8(6) . . ? C5' C4' Cl4 126.1(6) . . ? N1' C5' C4' 110.7(7) . . ? N1' C5' Cl5' 120.0(6) . . ? C4' C5' Cl5' 129.3(7) . . ? C2 N1 C6 121.6(7) . . ? C2 N1 Pt1 115.9(5) . . ? C6 N1 Pt1 122.5(6) . . ? N1 C2 C3 119.5(7) . . ? N1 C2 C3' 114.5(7) . . ? C3 C2 C3' 125.9(8) . . ? C4 C3 C2 121.0(8) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 118.3(8) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 123.4(8) . . ? C4 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? N1 C6 C5 116.0(9) . . ? N1 C6 H6 122 . . ? C5 C6 H6 122 . . ? Cl14 C10 Cl12 101.8(6) . . ? Cl14 C10 Cl13 123.8(6) . . ? Cl12 C10 Cl13 109.4(6) . . ? Cl12 C10 Cl15 120.0(6) . . ? Cl13 C10 Cl15 101.0(6) . . ? Cl14 C10 H10 106.9 . . ? Cl12 C10 H10 106.9 . . ? Cl13 C10 H10 106.9 . . ? Cl15 C10 H10 111.8 . . ? 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 C5' N1' N2' C3' 0.1(8) . . . . ? C5' N1' N2' Pt1 178.7(5) . . . . ? N1 Pt1 N2' N1' 2.8(7) 3_655 . . . ? N1 Pt1 N2' N1' -177.2(7) . . . . ? Cl1 Pt1 N2' N1' 91.6(6) . . . . ? Cl1 Pt1 N2' N1' -88.4(6) 3_655 . . . ? N1 Pt1 N2' C3' -178.7(5) 3_655 . . . ? N1 Pt1 N2' C3' 1.3(5) . . . . ? Cl1 Pt1 N2' C3' -89.9(5) . . . . ? Cl1 Pt1 N2' C3' 90.1(5) 3_655 . . . ? N1' N2' C3' C4' 0.0(8) . . . . ? Pt1 N2' C3' C4' -178.8(5) . . . . ? N1' N2' C3' C2 177.2(6) . . . . ? Pt1 N2' C3' C2 -1.7(8) . . . . ? N2' C3' C4' C5' -0.2(8) . . . . ? C2 C3' C4' C5' -176.1(9) . . . . ? N2' C3' C4' Cl4 179.9(5) . . . . ? C2 C3' C4' Cl4 4.0(14) . . . . ? N2' N1' C5' C4' -0.2(8) . . . . ? N2' N1' C5' Cl5' -179.1(5) . . . . ? C3' C4' C5' N1' 0.2(9) . . . . ? Cl4 C4' C5' N1' -179.9(6) . . . . ? C3' C4' C5' Cl5' 179.0(6) . . . . ? Cl4 C4' C5' Cl5' -1.1(11) . . . . ? N2' Pt1 N1 C2 179.3(5) 3_655 . . . ? N2' Pt1 N1 C2 -0.7(5) . . . . ? Cl1 Pt1 N1 C2 88.8(5) . . . . ? Cl1 Pt1 N1 C2 -91.2(5) 3_655 . . . ? N2' Pt1 N1 C6 -1.3(6) 3_655 . . . ? N2' Pt1 N1 C6 178.7(6) . . . . ? Cl1 Pt1 N1 C6 -91.8(6) . . . . ? Cl1 Pt1 N1 C6 88.2(6) 3_655 . . . ? C6 N1 C2 C3 -2.2(11) . . . . ? Pt1 N1 C2 C3 177.3(5) . . . . ? C6 N1 C2 C3' -179.4(7) . . . . ? Pt1 N1 C2 C3' 0.0(8) . . . . ? C4' C3' C2 N1 176.8(9) . . . . ? N2' C3' C2 N1 1.0(9) . . . . ? C4' C3' C2 C3 -0.3(15) . . . . ? N2' C3' C2 C3 -176.0(7) . . . . ? N1 C2 C3 C4 3.0(11) . . . . ? C3' C2 C3 C4 179.9(7) . . . . ? C2 C3 C4 C5 -0.5(12) . . . . ? C3 C4 C5 C6 -2.9(13) . . . . ? C2 N1 C6 C5 -1.0(11) . . . . ? Pt1 N1 C6 C5 179.6(6) . . . . ? C4 C5 C6 N1 3.6(13) . . . . ? # 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