# 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 #------------------ AUDIT DETAILS -------------------------------------------# #_audit_creation_date 2009-04-20 #_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 ? #============================================================================== # # SUBMISSION DETAILS _publ_contact_author_name 'Bernhard Lippert' _publ_contact_author_address ;Department of Bioinorganic Chemistry TU Dortmund University Otto-Hahn-Strasse 6 44227 Dortmund, Germany ; # Address of author for correspondence _publ_contact_author_email bernhard.lippert@uni-dortmund.de _publ_contact_author_fax '+49 231 755 3797' _publ_contact_author_phone '+49 231 755 3840' _publ_contact_letter ; Submission dated :2009-04-20 Please consider this CIF for submission to the Cambridge Crystallographic Data Centre. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. This CIF is submitted as a personal communication This CIF is submitted as part of a journal submission ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name #_publ_author_footnote _publ_author_address 'Wei-Zheng Shen.' ;Department of Bioinorganic Chemistry TU Dortmund University Otto-Hahn-Strasse 6 44227 Dortmund, Germany ; 'Gabriele Trotscher-Kaus' . B.Lippert . #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_718935_shen1 _database_code_depnum_ccdc_archive 'CCDC 718935' _audit_creation_date 2009-04-20 _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 ? #_audit_creation_date 2009-04-20T18:34:12-00:00 #_audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H28 N10 O2 Pd2, 2(Cl O4), 3(H2 O)' _chemical_formula_sum 'C30 H34 Cl2 N10 O13 Pd2' _chemical_formula_weight 1026.37 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 13.762(3) _cell_length_b 24.089(5) _cell_length_c 11.850(2) _cell_angle_alpha 90 _cell_angle_beta 112.13(3) _cell_angle_gamma 90 _cell_volume 3639.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2997 _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 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.886 _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_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetI/netI 0.1106 _diffrn_reflns_number 5884 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.41 _diffrn_reflns_theta_full 24.41 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2997 _reflns_number_gt 1736 _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^)+(0.0521P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2997 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.126 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.273 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # 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' Pd Pd -0.9988 1.0072 '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 Pd1 Pd -0.08636(5) 0.15479(2) -0.36427(5) 0.0425(3) Uani 1 1 d . . . O2A O -0.2511(4) 0.0715(2) -0.4860(5) 0.0585(16) Uani 1 1 d . . . N1A N -0.2570(5) 0.0163(3) -0.3330(7) 0.0546(19) Uani 1 1 d . . . N1P N -0.0363(5) 0.2250(3) -0.4203(6) 0.0518(18) Uani 1 1 d . . . N3A N -0.1363(5) 0.0892(2) -0.2934(6) 0.0418(16) Uani 1 1 d . . . N4B N -0.0124(5) 0.1042(3) -0.0983(6) 0.0480(18) Uani 1 1 d . . . H1 H 0.0013 0.0992 -0.0202 0.058 Uiso 1 1 d R . . N8P N -0.1836(5) 0.2098(3) -0.3337(6) 0.0477(17) Uani 1 1 d . . . C1A C -0.3394(7) -0.0189(4) -0.4192(9) 0.081(3) Uani 1 1 d . . . H11 H -0.3569 -0.049 -0.3746 0.121 Uiso 1 1 calc R . . H12 H -0.314 -0.0346 -0.4793 0.121 Uiso 1 1 calc R . . H13 H -0.4021 0.0036 -0.4611 0.121 Uiso 1 1 calc R . . C2A C -0.2166(7) 0.0593(4) -0.3779(9) 0.051(2) Uani 1 1 d . . . C2P C 0.0414(7) 0.2270(4) -0.4635(7) 0.063(3) Uani 1 1 d . . . H6 H 0.0709 0.1933 -0.4775 0.076 Uiso 1 1 calc R . . C3P C 0.0787(9) 0.2764(5) -0.4876(8) 0.081(3) Uani 1 1 d . . . H9 H 0.1334 0.277 -0.5182 0.098 Uiso 1 1 calc R . . C4B C -0.0953(6) 0.0771(3) -0.1723(8) 0.044(2) Uani 1 1 d . . . C4P C 0.0368(10) 0.3244(6) -0.4674(10) 0.093(4) Uani 1 1 d . . . H8 H 0.0635 0.3591 -0.4808 0.112 Uiso 1 1 calc R . . C5B C -0.1432(6) 0.0339(3) -0.1286(8) 0.050(2) Uani 1 1 d . . . H14 H -0.1203 0.0255 -0.0442 0.06 Uiso 1 1 calc R . . C5P C -0.0442(10) 0.3225(4) -0.4274(8) 0.088(4) Uani 1 1 d . . . H10 H -0.0758 0.356 -0.4161 0.106 Uiso 1 1 calc R . . C6A C -0.2217(7) 0.0060(3) -0.2114(10) 0.061(3) Uani 1 1 d . . . H2 H -0.2546 -0.0228 -0.1837 0.073 Uiso 1 1 calc R . . C6P C -0.0808(8) 0.2717(4) -0.4032(7) 0.059(2) Uani 1 1 d . . . C7P C -0.1668(7) 0.2645(4) -0.3565(7) 0.058(2) Uani 1 1 d . . . C9P C -0.2609(7) 0.1993(4) -0.2935(7) 0.057(2) Uani 1 1 d . . . H3 H -0.2742 0.1618 -0.279 0.069 Uiso 1 1 calc R . . C10P C -0.3208(7) 0.2397(5) -0.2726(8) 0.070(3) Uani 1 1 d . . . H7 H -0.3742 0.2303 -0.2433 0.084 Uiso 1 1 calc R . . C11P C -0.3041(9) 0.2934(5) -0.2937(9) 0.081(3) Uani 1 1 d . . . H5 H -0.3457 0.3219 -0.2792 0.097 Uiso 1 1 calc R . . C12P C -0.2251(10) 0.3067(4) -0.3372(8) 0.080(3) Uani 1 1 d . . . H4 H -0.2125 0.3442 -0.3528 0.096 Uiso 1 1 calc R . . Cl1 Cl 0 0.08649(18) -0.75 0.0783(11) Uani 1 2 d S . . O11 O 0.0631(14) 0.0950(8) -0.8252(17) 0.1337(19) Uani 0.5 1 d P . . O12 O -0.1079(14) 0.0845(8) -0.8422(17) 0.1337(19) Uani 0.5 1 d P . . O13 O 0.0451(13) 0.0353(8) -0.6740(15) 0.1337(19) Uani 0.5 1 d P . . O14 O 0.0164(15) 0.1298(8) -0.6770(16) 0.1337(19) Uani 0.5 1 d P . . Cl2 Cl -0.5 0.09322(14) -0.25 0.0654(9) Uani 1 2 d S . . O21 O -0.4107(7) 0.1262(4) -0.1966(8) 0.1337(19) Uani 1 1 d . . . O22 O -0.4853(7) 0.0628(4) -0.3403(8) 0.1337(19) Uani 1 1 d . . . O1W O -0.2241(8) 0.1521(4) -0.0052(11) 0.191(5) Uani 1 1 d . . . H1W H -0.2819 0.136 -0.0451 0.287 Uiso 1 1 d R . . H2W H -0.1867 0.1297 0.0491 0.287 Uiso 1 1 d R . . O2W O -0.4354(9) 0.0614(4) -0.6918(11) 0.071(4) Uani 0.5 1 d P . . H3W H -0.3853 0.0558 -0.6172 0.106 Uiso 0.5 1 d PR . . H4W H -0.4515 0.0268 -0.7201 0.106 Uiso 0.5 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0462(4) 0.0485(4) 0.0347(4) 0.0023(3) 0.0172(3) 0.0029(3) O2A 0.059(4) 0.070(4) 0.044(4) -0.014(3) 0.016(3) -0.004(3) N1A 0.052(5) 0.054(5) 0.063(5) -0.010(4) 0.029(4) -0.003(4) N1P 0.061(5) 0.057(5) 0.035(4) 0.006(4) 0.015(4) -0.008(4) N3A 0.045(4) 0.040(4) 0.042(4) -0.003(3) 0.017(4) -0.003(3) N4B 0.061(5) 0.063(4) 0.033(4) -0.002(3) 0.032(4) -0.008(4) N8P 0.054(5) 0.049(5) 0.035(4) -0.002(3) 0.012(4) 0.001(4) C1A 0.070(7) 0.078(7) 0.094(8) -0.037(6) 0.030(6) -0.029(6) C2A 0.054(6) 0.046(6) 0.062(7) -0.013(5) 0.033(6) 0.006(5) C2P 0.053(6) 0.091(7) 0.042(5) 0.011(5) 0.014(5) -0.017(6) C3P 0.089(8) 0.104(9) 0.042(6) 0.014(7) 0.015(6) -0.042(8) C4B 0.049(5) 0.039(5) 0.050(6) -0.005(4) 0.028(5) -0.002(4) C4P 0.122(11) 0.100(10) 0.050(7) 0.007(7) 0.023(7) -0.063(9) C5B 0.055(6) 0.050(5) 0.055(6) -0.004(5) 0.032(5) -0.006(5) C5P 0.149(12) 0.053(7) 0.035(6) 0.003(5) 0.003(7) -0.008(7) C6A 0.065(7) 0.038(5) 0.100(9) 0.004(6) 0.053(7) 0.007(5) C6P 0.084(7) 0.047(6) 0.032(5) 0.002(4) 0.005(5) -0.004(5) C7P 0.070(7) 0.059(7) 0.029(5) -0.001(4) 0.001(5) 0.010(5) C9P 0.062(6) 0.069(6) 0.037(5) 0.002(4) 0.014(5) 0.014(5) C10P 0.067(7) 0.091(8) 0.046(6) -0.005(6) 0.015(5) 0.029(6) C11P 0.096(9) 0.088(9) 0.046(6) -0.005(6) 0.012(6) 0.051(7) C12P 0.121(10) 0.053(6) 0.041(6) -0.012(5) 0.002(6) 0.035(7) Cl1 0.073(3) 0.093(3) 0.074(3) 0 0.034(2) 0 O11 0.121(4) 0.157(5) 0.125(4) -0.050(4) 0.048(4) -0.008(4) O12 0.121(4) 0.157(5) 0.125(4) -0.050(4) 0.048(4) -0.008(4) O13 0.121(4) 0.157(5) 0.125(4) -0.050(4) 0.048(4) -0.008(4) O14 0.121(4) 0.157(5) 0.125(4) -0.050(4) 0.048(4) -0.008(4) Cl2 0.084(3) 0.061(2) 0.0460(19) 0 0.0178(19) 0 O21 0.121(4) 0.157(5) 0.125(4) -0.050(4) 0.048(4) -0.008(4) O22 0.121(4) 0.157(5) 0.125(4) -0.050(4) 0.048(4) -0.008(4) O1W 0.155(10) 0.202(11) 0.229(13) 0.005(10) 0.085(10) 0.003(8) O2W 0.087(9) 0.048(7) 0.077(9) 0.003(6) 0.031(7) 0.008(6) #----------------------------------------------------------------------------# # 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 Pd1 N4B 1.995(6) 2_554 ? Pd1 N8P 2.011(6) . ? Pd1 N3A 2.028(6) . ? Pd1 N1P 2.031(6) . ? Pd1 Pd1 2.8521(17) 2_554 ? O2A C2A 1.223(10) . ? N1A C6A 1.360(11) . ? N1A C2A 1.374(10) . ? N1A C1A 1.475(10) . ? N1P C6P 1.330(10) . ? N1P C2P 1.349(10) . ? N3A C4B 1.361(9) . ? N3A C2A 1.381(10) . ? N4B C4B 1.320(9) . ? N4B Pd1 1.996(6) 2_554 ? N4B H1 0.88 . ? N8P C9P 1.343(10) . ? N8P C7P 1.381(10) . ? C1A H11 0.98 . ? C1A H12 0.98 . ? C1A H13 0.98 . ? C2P C3P 1.369(12) . ? C2P H6 0.95 . ? C3P C4P 1.353(15) . ? C3P H9 0.95 . ? C4B C5B 1.429(10) . ? C4P C5P 1.367(15) . ? C4P H8 0.95 . ? C5B C6A 1.336(11) . ? C5B H14 0.95 . ? C5P C6P 1.394(13) . ? C5P H10 0.95 . ? C6A H2 0.95 . ? C6P C7P 1.493(12) . ? C7P C12P 1.368(12) . ? C9P C10P 1.358(11) . ? C9P H3 0.95 . ? C10P C11P 1.353(13) . ? C10P H7 0.95 . ? C11P C12P 1.405(14) . ? C11P H5 0.95 . ? C12P H4 0.95 . ? Cl1 O14 1.319(16) . ? Cl1 O14 1.319(16) 2_553 ? Cl1 O11 1.475(18) . ? Cl1 O11 1.475(18) 2_553 ? Cl1 O12 1.476(19) 2_553 ? Cl1 O12 1.476(19) . ? Cl1 O13 1.515(19) 2_553 ? Cl1 O13 1.515(19) . ? O11 O14 1.39(2) 2_553 ? O12 O13 1.44(2) 2_553 ? O12 O14 1.62(2) 2_553 ? O13 O12 1.44(2) 2_553 ? O13 O13 1.76(3) 2_553 ? O14 O11 1.39(2) 2_553 ? O14 O14 1.61(3) 2_553 ? O14 O12 1.62(2) 2_553 ? Cl2 O22 1.373(8) 2_454 ? Cl2 O22 1.374(8) . ? Cl2 O21 1.398(9) . ? Cl2 O21 1.398(9) 2_454 ? O1W H1W 0.8498 . ? O1W H2W 0.8499 . ? O2W O2W 1.79(2) 2_453 ? O2W H3W 0.9029 . ? O2W H4W 0.8944 . ? 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 N4B Pd1 N8P 176.0(3) 2_554 . ? N4B Pd1 N3A 88.9(2) 2_554 . ? N8P Pd1 N3A 95.0(3) . . ? N4B Pd1 N1P 95.3(3) 2_554 . ? N8P Pd1 N1P 80.8(3) . . ? N3A Pd1 N1P 174.1(3) . . ? N4B Pd1 Pd1 79.48(19) 2_554 2_554 ? N8P Pd1 Pd1 101.67(18) . 2_554 ? N3A Pd1 Pd1 84.16(19) . 2_554 ? N1P Pd1 Pd1 92.66(18) . 2_554 ? C6A N1A C2A 120.9(8) . . ? C6A N1A C1A 120.2(8) . . ? C2A N1A C1A 118.9(8) . . ? C6P N1P C2P 120.2(8) . . ? C6P N1P Pd1 115.0(6) . . ? C2P N1P Pd1 124.6(7) . . ? C4B N3A C2A 123.6(7) . . ? C4B N3A Pd1 122.1(5) . . ? C2A N3A Pd1 114.2(6) . . ? C4B N4B Pd1 130.1(5) . 2_554 ? C4B N4B H1 114.8 . . ? Pd1 N4B H1 115 2_554 . ? C9P N8P C7P 117.6(7) . . ? C9P N8P Pd1 127.5(6) . . ? C7P N8P Pd1 114.9(6) . . ? 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 122.2(9) . . ? O2A C2A N3A 121.5(8) . . ? N1A C2A N3A 116.3(8) . . ? N1P C2P C3P 121.5(10) . . ? N1P C2P H6 119.2 . . ? C3P C2P H6 119.2 . . ? C4P C3P C2P 119.2(11) . . ? C4P C3P H9 120.4 . . ? C2P C3P H9 120.4 . . ? N4B C4B N3A 120.5(7) . . ? N4B C4B C5B 121.3(8) . . ? N3A C4B C5B 118.2(7) . . ? C3P C4P C5P 119.3(11) . . ? C3P C4P H8 120.3 . . ? C5P C4P H8 120.3 . . ? C6A C5B C4B 117.2(8) . . ? C6A C5B H14 121.4 . . ? C4B C5B H14 121.4 . . ? C4P C5P C6P 120.4(11) . . ? C4P C5P H10 119.8 . . ? C6P C5P H10 119.8 . . ? C5B C6A N1A 123.6(8) . . ? C5B C6A H2 118.2 . . ? N1A C6A H2 118.2 . . ? N1P C6P C5P 119.2(10) . . ? N1P C6P C7P 115.6(8) . . ? C5P C6P C7P 125.2(10) . . ? C12P C7P N8P 121.6(9) . . ? C12P C7P C6P 124.9(10) . . ? N8P C7P C6P 113.5(8) . . ? N8P C9P C10P 123.2(9) . . ? N8P C9P H3 118.4 . . ? C10P C9P H3 118.4 . . ? C11P C10P C9P 119.6(10) . . ? C11P C10P H7 120.2 . . ? C9P C10P H7 120.2 . . ? C10P C11P C12P 119.7(9) . . ? C10P C11P H5 120.2 . . ? C12P C11P H5 120.2 . . ? C7P C12P C11P 118.4(10) . . ? C7P C12P H4 120.8 . . ? C11P C12P H4 120.8 . . ? O14 Cl1 O14 75.5(16) . 2_553 ? O14 Cl1 O11 107.0(11) . . ? O14 Cl1 O11 59.2(10) 2_553 . ? O14 Cl1 O11 59.2(10) . 2_553 ? O14 Cl1 O11 107.0(11) 2_553 2_553 ? O11 Cl1 O11 164.0(15) . 2_553 ? O14 Cl1 O12 70.4(10) . 2_553 ? O14 Cl1 O12 112.8(11) 2_553 2_553 ? O11 Cl1 O12 78.1(9) . 2_553 ? O11 Cl1 O12 102.4(10) 2_553 2_553 ? O14 Cl1 O12 112.8(11) . . ? O14 Cl1 O12 70.4(10) 2_553 . ? O11 Cl1 O12 102.4(10) . . ? O11 Cl1 O12 78.1(9) 2_553 . ? O12 Cl1 O12 176.2(16) 2_553 . ? O14 Cl1 O13 164.6(11) . 2_553 ? O14 Cl1 O13 108.9(10) 2_553 2_553 ? O11 Cl1 O13 87.5(9) . 2_553 ? O11 Cl1 O13 105.7(10) 2_553 2_553 ? O12 Cl1 O13 119.1(12) 2_553 2_553 ? O12 Cl1 O13 57.4(8) . 2_553 ? O14 Cl1 O13 108.9(10) . . ? O14 Cl1 O13 164.6(11) 2_553 . ? O11 Cl1 O13 105.7(10) . . ? O11 Cl1 O13 87.5(9) 2_553 . ? O12 Cl1 O13 57.4(8) 2_553 . ? O12 Cl1 O13 119.1(12) . . ? O13 Cl1 O13 71.1(12) 2_553 . ? O14 O11 Cl1 54.8(9) 2_553 . ? O13 O12 Cl1 62.7(11) 2_553 . ? O13 O12 O14 98.1(15) 2_553 2_553 ? Cl1 O12 O14 50.2(9) . 2_553 ? O12 O13 Cl1 59.9(11) 2_553 . ? O12 O13 O13 107.0(13) 2_553 2_553 ? Cl1 O13 O13 54.5(6) . 2_553 ? Cl1 O14 O11 66.0(12) . 2_553 ? Cl1 O14 O14 52.3(8) . 2_553 ? O11 O14 O14 96.7(16) 2_553 2_553 ? Cl1 O14 O12 59.3(10) . 2_553 ? O11 O14 O12 99.6(15) 2_553 2_553 ? O14 O14 O12 92.3(13) 2_553 2_553 ? O22 Cl2 O22 115.5(8) 2_454 . ? O22 Cl2 O21 108.2(5) 2_454 . ? O22 Cl2 O21 107.1(5) . . ? O22 Cl2 O21 107.1(5) 2_454 2_454 ? O22 Cl2 O21 108.2(5) . 2_454 ? O21 Cl2 O21 110.8(8) . 2_454 ? H1W O1W H2W 107.7 . . ? O2W O2W H3W 157.4 2_453 . ? O2W O2W H4W 71.2 2_453 . ? H3W O2W H4W 102.7 . . ? 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 N4B Pd1 N1P C6P -176.2(6) 2_554 . . . ? N8P Pd1 N1P C6P 4.9(6) . . . . ? Pd1 Pd1 N1P C6P -96.5(6) 2_554 . . . ? N4B Pd1 N1P C2P -1.1(7) 2_554 . . . ? N8P Pd1 N1P C2P -180.0(7) . . . . ? Pd1 Pd1 N1P C2P 78.6(6) 2_554 . . . ? N4B Pd1 N3A C4B 94.6(6) 2_554 . . . ? N8P Pd1 N3A C4B -86.2(6) . . . . ? Pd1 Pd1 N3A C4B 15.0(5) 2_554 . . . ? N4B Pd1 N3A C2A -87.1(5) 2_554 . . . ? N8P Pd1 N3A C2A 92.1(5) . . . . ? Pd1 Pd1 N3A C2A -166.7(5) 2_554 . . . ? N3A Pd1 N8P C9P -7.0(7) . . . . ? N1P Pd1 N8P C9P 177.1(7) . . . . ? Pd1 Pd1 N8P C9P -92.1(7) 2_554 . . . ? N3A Pd1 N8P C7P 172.4(5) . . . . ? N1P Pd1 N8P C7P -3.5(5) . . . . ? Pd1 Pd1 N8P C7P 87.4(5) 2_554 . . . ? C6A N1A C2A O2A -175.6(7) . . . . ? C1A N1A C2A O2A 4.7(11) . . . . ? C6A N1A C2A N3A 2.6(10) . . . . ? C1A N1A C2A N3A -177.1(7) . . . . ? C4B N3A C2A O2A -180.0(7) . . . . ? Pd1 N3A C2A O2A 1.8(9) . . . . ? C4B N3A C2A N1A 1.8(10) . . . . ? Pd1 N3A C2A N1A -176.5(5) . . . . ? C6P N1P C2P C3P 1.9(12) . . . . ? Pd1 N1P C2P C3P -173.0(6) . . . . ? N1P C2P C3P C4P 0.2(14) . . . . ? Pd1 N4B C4B N3A -12.1(11) 2_554 . . . ? Pd1 N4B C4B C5B 166.8(5) 2_554 . . . ? C2A N3A C4B N4B 173.8(7) . . . . ? Pd1 N3A C4B N4B -8.0(10) . . . . ? C2A N3A C4B C5B -5.1(11) . . . . ? Pd1 N3A C4B C5B 173.1(5) . . . . ? C2P C3P C4P C5P -2.3(16) . . . . ? N4B C4B C5B C6A -175.0(7) . . . . ? N3A C4B C5B C6A 3.9(11) . . . . ? C3P C4P C5P C6P 2.5(16) . . . . ? C4B C5B C6A N1A 0.3(12) . . . . ? C2A N1A C6A C5B -3.7(12) . . . . ? C1A N1A C6A C5B 176.0(8) . . . . ? C2P N1P C6P C5P -1.7(12) . . . . ? Pd1 N1P C6P C5P 173.7(6) . . . . ? C2P N1P C6P C7P 179.3(7) . . . . ? Pd1 N1P C6P C7P -5.4(9) . . . . ? C4P C5P C6P N1P -0.5(14) . . . . ? C4P C5P C6P C7P 178.5(9) . . . . ? C9P N8P C7P C12P 1.0(12) . . . . ? Pd1 N8P C7P C12P -178.4(7) . . . . ? C9P N8P C7P C6P -178.8(7) . . . . ? Pd1 N8P C7P C6P 1.7(9) . . . . ? N1P C6P C7P C12P -177.4(8) . . . . ? C5P C6P C7P C12P 3.6(14) . . . . ? N1P C6P C7P N8P 2.5(11) . . . . ? C5P C6P C7P N8P -176.5(8) . . . . ? C7P N8P C9P C10P -1.2(12) . . . . ? Pd1 N8P C9P C10P 178.2(6) . . . . ? N8P C9P C10P C11P 0.7(14) . . . . ? C9P C10P C11P C12P 0.1(15) . . . . ? N8P C7P C12P C11P -0.3(13) . . . . ? C6P C7P C12P C11P 179.5(8) . . . . ? C10P C11P C12P C7P -0.2(15) . . . . ? O14 Cl1 O11 O14 -60.8(19) . . . 2_553 ? O11 Cl1 O11 O14 -32.2(10) 2_553 . . 2_553 ? O12 Cl1 O11 O14 -125.8(15) 2_553 . . 2_553 ? O12 Cl1 O11 O14 58.0(13) . . . 2_553 ? O13 Cl1 O11 O14 113.8(12) 2_553 . . 2_553 ? O13 Cl1 O11 O14 -176.7(12) . . . 2_553 ? O14 Cl1 O12 O13 -166.6(12) . . . 2_553 ? O14 Cl1 O12 O13 129.4(13) 2_553 . . 2_553 ? O11 Cl1 O12 O13 78.8(12) . . . 2_553 ? O11 Cl1 O12 O13 -117.5(13) 2_553 . . 2_553 ? O13 Cl1 O12 O13 -37.2(17) . . . 2_553 ? O14 Cl1 O12 O14 64.0(18) . . . 2_553 ? O11 Cl1 O12 O14 -50.6(11) . . . 2_553 ? O11 Cl1 O12 O14 113.1(13) 2_553 . . 2_553 ? O13 Cl1 O12 O14 -129.4(13) 2_553 . . 2_553 ? O13 Cl1 O12 O14 -166.6(11) . . . 2_553 ? O14 Cl1 O13 O12 -50.3(13) . . . 2_553 ? O14 Cl1 O13 O12 54(4) 2_553 . . 2_553 ? O11 Cl1 O13 O12 64.3(12) . . . 2_553 ? O11 Cl1 O13 O12 -106.5(12) 2_553 . . 2_553 ? O12 Cl1 O13 O12 178.6(6) . . . 2_553 ? O13 Cl1 O13 O12 146.0(16) 2_553 . . 2_553 ? O14 Cl1 O13 O13 163.7(11) . . . 2_553 ? O14 Cl1 O13 O13 -92(4) 2_553 . . 2_553 ? O11 Cl1 O13 O13 -81.7(12) . . . 2_553 ? O11 Cl1 O13 O13 107.5(12) 2_553 . . 2_553 ? O12 Cl1 O13 O13 -146.0(16) 2_553 . . 2_553 ? O12 Cl1 O13 O13 32.6(14) . . . 2_553 ? O14 Cl1 O14 O11 120.4(16) 2_553 . . 2_553 ? O11 Cl1 O14 O11 171.2(9) . . . 2_553 ? O12 Cl1 O14 O11 -118.5(12) 2_553 . . 2_553 ? O12 Cl1 O14 O11 59.4(14) . . . 2_553 ? O13 Cl1 O14 O11 12(4) 2_553 . . 2_553 ? O13 Cl1 O14 O11 -75.1(12) . . . 2_553 ? O11 Cl1 O14 O14 50.8(13) . . . 2_553 ? O11 Cl1 O14 O14 -120.4(16) 2_553 . . 2_553 ? O12 Cl1 O14 O14 121.1(14) 2_553 . . 2_553 ? O12 Cl1 O14 O14 -61.0(14) . . . 2_553 ? O13 Cl1 O14 O14 -108(4) 2_553 . . 2_553 ? O13 Cl1 O14 O14 164.5(11) . . . 2_553 ? O14 Cl1 O14 O12 -121.1(14) 2_553 . . 2_553 ? O11 Cl1 O14 O12 -70.3(12) . . . 2_553 ? O11 Cl1 O14 O12 118.5(13) 2_553 . . 2_553 ? O12 Cl1 O14 O12 177.9(9) . . . 2_553 ? O13 Cl1 O14 O12 131(4) 2_553 . . 2_553 ? O13 Cl1 O14 O12 43.4(10) . . . 2_553 ? # 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 '718936_shen.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-04-20 at 18:07:45 # 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_718936_shen _database_code_depnum_ccdc_archive 'CCDC 718936' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2009-04-20 _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 -------------------------# #_audit_creation_date 2009-04-20T18:07:45-00:00 #_audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C20 H22 N8 O2 Pt), 4(N O3), 5(H2 O)' _chemical_formula_sum 'C40 H54 N20 O21 Pt2' _chemical_formula_weight 1541.21 #----------------------------------------------------------------------------# # 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 12.533(3) _cell_length_b 14.493(3) _cell_length_c 15.835(3) _cell_angle_alpha 93.76(3) _cell_angle_beta 106.29(3) _cell_angle_gamma 95.93(3) _cell_volume 2732.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9967 _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 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.209 _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_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_unetI/netI 0.202 _diffrn_reflns_number 9967 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.37 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 9967 _reflns_number_gt 4719 _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^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9967 _refine_ls_number_parameters 747 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1169 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.047 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.173 #----------------------------------------------------------------------------# # 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 0.66166(4) 0.37346(3) 0.27181(3) 0.03657(15) Uani 1 1 d . . . O2A O 0.5453(6) 0.5266(5) 0.3272(5) 0.060(2) Uani 1 1 d . . . O2B O 0.7544(6) 0.2168(5) 0.3710(4) 0.056(2) Uani 1 1 d . . . N1A N 0.4127(8) 0.4555(6) 0.3808(6) 0.050(2) Uani 1 1 d . . . N1B N 0.8669(7) 0.2836(6) 0.5033(6) 0.047(3) Uani 1 1 d . . . N1P N 0.7820(8) 0.3830(5) 0.2113(6) 0.042(2) Uani 1 1 d . . . N3A N 0.5303(7) 0.3668(6) 0.3243(5) 0.036(2) Uani 1 1 d . . . N3B N 0.7676(7) 0.3729(5) 0.3942(5) 0.036(2) Uani 1 1 d . . . N4A N 0.5073(7) 0.2119(6) 0.3216(5) 0.054(3) Uani 1 1 d . . . H39 H 0.4751 0.1598 0.331 0.065 Uiso 1 1 d R . . H40 H 0.562 0.2123 0.2987 0.065 Uiso 1 1 d R . . N4B N 0.7939(7) 0.5350(6) 0.4199(5) 0.057(3) Uani 1 1 d . . . H43 H 0.8227 0.5859 0.4531 0.069 Uiso 1 1 d R . . H44 H 0.7507 0.5369 0.3673 0.069 Uiso 1 1 d R . . N8P N 0.5657(8) 0.3744(5) 0.1458(5) 0.037(2) Uani 1 1 d . . . C1A C 0.3758(10) 0.5442(8) 0.3984(8) 0.078(4) Uani 1 1 d . . . H29 H 0.3458 0.5699 0.3436 0.117 Uiso 1 1 calc R . . H30 H 0.4382 0.5861 0.4352 0.117 Uiso 1 1 calc R . . H31 H 0.3189 0.5353 0.428 0.117 Uiso 1 1 calc R . . C1B C 0.8970(9) 0.1933(7) 0.5317(7) 0.073(4) Uani 1 1 d . . . H7 H 0.8383 0.1622 0.5514 0.109 Uiso 1 1 calc R . . H8 H 0.9655 0.2026 0.5792 0.109 Uiso 1 1 calc R . . H9 H 0.9072 0.1557 0.483 0.109 Uiso 1 1 calc R . . C2A C 0.4989(10) 0.4541(9) 0.3427(6) 0.046(3) Uani 1 1 d . . . C2B C 0.7944(9) 0.2872(8) 0.4199(7) 0.044(3) Uani 1 1 d . . . C2P C 0.8934(11) 0.3813(7) 0.2505(7) 0.052(3) Uani 1 1 d . . . H42 H 0.917 0.3717 0.31 0.062 Uiso 1 1 calc R . . C3P C 0.9734(10) 0.3934(8) 0.2048(9) 0.069(4) Uani 1 1 d . . . H26 H 1.049 0.3927 0.2333 0.083 Uiso 1 1 calc R . . C4A C 0.4757(10) 0.2884(7) 0.3406(7) 0.042(3) Uani 1 1 d . . . C4B C 0.8148(9) 0.4538(8) 0.4481(7) 0.041(3) Uani 1 1 d . . . C4P C 0.9380(11) 0.4062(8) 0.1179(8) 0.064(4) Uani 1 1 d . . . H28 H 0.9891 0.4136 0.0855 0.077 Uiso 1 1 calc R . . C5A C 0.3867(10) 0.2893(8) 0.3758(8) 0.062(4) Uani 1 1 d . . . H32 H 0.3488 0.2343 0.3855 0.074 Uiso 1 1 calc R . . C5B C 0.8887(8) 0.4482(8) 0.5337(7) 0.048(3) Uani 1 1 d . . . H38 H 0.9206 0.5017 0.5718 0.058 Uiso 1 1 calc R . . C5P C 0.8243(12) 0.4082(8) 0.0775(7) 0.063(4) Uani 1 1 d . . . H34 H 0.8002 0.4191 0.0183 0.076 Uiso 1 1 calc R . . C6A C 0.3576(10) 0.3706(10) 0.3950(7) 0.067(4) Uani 1 1 d . . . H27 H 0.2981 0.3724 0.4191 0.081 Uiso 1 1 calc R . . C6B C 0.9113(10) 0.3618(8) 0.5583(7) 0.061(4) Uani 1 1 d . . . H37 H 0.9585 0.3569 0.6144 0.073 Uiso 1 1 calc R . . C6P C 0.7463(11) 0.3940(7) 0.1243(7) 0.044(3) Uani 1 1 d . . . C7P C 0.6250(9) 0.3876(6) 0.0870(7) 0.036(3) Uani 1 1 d . . . C9P C 0.4542(10) 0.3638(7) 0.1171(7) 0.048(3) Uani 1 1 d . . . H41 H 0.4134 0.3542 0.1573 0.057 Uiso 1 1 calc R . . C10P C 0.3988(10) 0.3668(7) 0.0304(7) 0.056(3) Uani 1 1 d . . . H35 H 0.3209 0.3614 0.0127 0.067 Uiso 1 1 calc R . . C11P C 0.4562(11) 0.3777(7) -0.0316(7) 0.055(3) Uani 1 1 d . . . H36 H 0.4189 0.3774 -0.0914 0.066 Uiso 1 1 calc R . . C12P C 0.5718(10) 0.3890(7) -0.0009(6) 0.049(3) Uani 1 1 d . . . H33 H 0.6138 0.3976 -0.0404 0.059 Uiso 1 1 calc R . . Pt2 Pt 0.39493(4) 0.84550(3) 0.11511(3) 0.03977(16) Uani 1 1 d . . . O2C O 0.2397(7) 0.6719(5) 0.1267(5) 0.060(2) Uani 1 1 d . . . O2D O 0.5260(6) 0.9983(5) 0.2551(4) 0.052(2) Uani 1 1 d . . . N1C N 0.1022(10) 0.7264(7) 0.1719(7) 0.069(3) Uani 1 1 d . . . N1D N 0.6359(8) 0.9245(6) 0.3627(6) 0.050(3) Uani 1 1 d . . . N1Y N 0.5214(8) 0.8642(5) 0.0586(5) 0.040(2) Uani 1 1 d . . . N3C N 0.2581(7) 0.8290(7) 0.1615(5) 0.042(2) Uani 1 1 d . . . N3D N 0.5017(7) 0.8381(6) 0.2388(5) 0.039(2) Uani 1 1 d . . . N4C N 0.2809(8) 0.9886(6) 0.2102(6) 0.073(3) Uani 1 1 d . . . H21 H 0.2575 1.0363 0.231 0.088 Uiso 1 1 d R . . H22 H 0.344 0.9946 0.1983 0.088 Uiso 1 1 d R . . N4D N 0.4700(7) 0.6789(5) 0.2279(5) 0.051(3) Uani 1 1 d . . . H24 H 0.4829 0.6257 0.2468 0.061 Uiso 1 1 d R . . H25 H 0.4193 0.6818 0.1789 0.061 Uiso 1 1 d R . . N8Y N 0.3039(9) 0.8551(6) -0.0110(5) 0.046(3) Uani 1 1 d . . . C1C C 0.0440(10) 0.6346(7) 0.1655(7) 0.082(3) Uani 1 1 d . . . H1 H 0.0109 0.612 0.1043 0.124 Uiso 1 1 calc R . . H2 H -0.0138 0.6366 0.1943 0.124 Uiso 1 1 calc R . . H3 H 0.0958 0.5936 0.1934 0.124 Uiso 1 1 calc R . . C1D C 0.6978(10) 1.0104(7) 0.4094(8) 0.082(3) Uani 1 1 d . . . H4 H 0.7526 0.9975 0.4618 0.124 Uiso 1 1 calc R . . H5 H 0.6475 1.049 0.4256 0.124 Uiso 1 1 calc R . . H6 H 0.7348 1.0423 0.3722 0.124 Uiso 1 1 calc R . . C2C C 0.2032(11) 0.7388(9) 0.1534(7) 0.053(3) Uani 1 1 d . . . C2D C 0.5516(10) 0.9260(7) 0.2837(7) 0.044(3) Uani 1 1 d . . . C2Y C 0.6308(10) 0.8696(7) 0.1001(7) 0.048(3) Uani 1 1 d . . . H20 H 0.6542 0.865 0.1607 0.058 Uiso 1 1 calc R . . C3Y C 0.7103(10) 0.8820(8) 0.0544(8) 0.060(3) Uani 1 1 d . . . H17 H 0.7859 0.8829 0.0839 0.072 Uiso 1 1 calc R . . C4C C 0.2211(12) 0.9092(10) 0.1960(7) 0.063(4) Uani 1 1 d . . . C4D C 0.5253(9) 0.7558(7) 0.2723(7) 0.038(3) Uani 1 1 d . . . C4Y C 0.6772(12) 0.8930(8) -0.0338(9) 0.069(4) Uani 1 1 d . . . H14 H 0.7296 0.9038 -0.0646 0.083 Uiso 1 1 calc R . . C5C C 0.1099(12) 0.8925(11) 0.2101(8) 0.087(5) Uani 1 1 d . . . H12 H 0.0758 0.9415 0.2274 0.105 Uiso 1 1 calc R . . C5D C 0.6091(9) 0.7565(7) 0.3507(7) 0.050(3) Uani 1 1 d . . . H23 H 0.6278 0.7011 0.374 0.06 Uiso 1 1 calc R . . C5Y C 0.5662(11) 0.8878(8) -0.0751(7) 0.057(4) Uani 1 1 d . . . H16 H 0.542 0.8929 -0.1356 0.069 Uiso 1 1 calc R . . C6C C 0.0564(12) 0.7996(12) 0.1968(9) 0.091(5) Uani 1 1 d . . . H11 H -0.0139 0.7887 0.2057 0.109 Uiso 1 1 calc R . . C6D C 0.6631(10) 0.8395(9) 0.3928(7) 0.059(3) Uani 1 1 d . . . H19 H 0.7214 0.8399 0.4444 0.071 Uiso 1 1 calc R . . C6Y C 0.4886(11) 0.8750(7) -0.0289(7) 0.043(3) Uani 1 1 d . . . C7Y C 0.3676(11) 0.8698(7) -0.0687(7) 0.043(3) Uani 1 1 d . . . C9Y C 0.1907(11) 0.8488(8) -0.0419(8) 0.059(3) Uani 1 1 d . . . H18 H 0.1486 0.8392 -0.0026 0.071 Uiso 1 1 calc R . . C10Y C 0.1351(11) 0.8562(8) -0.1298(8) 0.072(4) Uani 1 1 d . . . H10 H 0.0573 0.8516 -0.1494 0.086 Uiso 1 1 calc R . . C11Y C 0.1987(11) 0.8706(8) -0.1873(8) 0.064(4) Uani 1 1 d . . . H13 H 0.1636 0.8758 -0.2466 0.076 Uiso 1 1 calc R . . C12Y C 0.3132(11) 0.8771(7) -0.1575(7) 0.056(3) Uani 1 1 d . . . H15 H 0.3552 0.8865 -0.1969 0.067 Uiso 1 1 calc R . . O11 O 0.1326(9) 0.3044(7) 0.6966(6) 0.118(4) Uani 1 1 d . . . O12 O 0.2254(9) 0.2835(7) 0.8210(7) 0.130(5) Uani 1 1 d . . . O13 O 0.2689(9) 0.4070(7) 0.7692(6) 0.116(4) Uani 1 1 d . . . N1N N 0.2075(11) 0.3345(9) 0.7626(8) 0.076(3) Uani 1 1 d . . . O21 O 0.6104(11) 0.2389(8) 0.5212(7) 0.141(5) Uani 1 1 d . . . O22 O 0.7124(10) 0.2458(8) 0.6501(7) 0.132(4) Uani 1 1 d . . . O23 O 0.6003(11) 0.1197(8) 0.5930(7) 0.153(5) Uani 1 1 d . . . N2N N 0.6362(12) 0.1995(10) 0.5878(9) 0.092(4) Uani 1 1 d . . . O31 O 0.0859(9) 0.3328(8) 0.4164(7) 0.135(5) Uani 1 1 d . . . O32 O 0.0361(14) 0.2077(9) 0.3547(10) 0.198(7) Uani 1 1 d . . . O33 O 0.1622(12) 0.2314(11) 0.4618(12) 0.270(12) Uani 1 1 d . . . N3N N 0.0972(12) 0.2560(8) 0.4140(8) 0.075(4) Uani 1 1 d . . . O41 O 0.0677(11) 0.2153(13) 0.0328(10) 0.183(7) Uani 1 1 d . . . O42 O 0.2060(14) 0.2845(12) 0.1446(10) 0.172(7) Uani 1 1 d . . . O43 O 0.1326(11) 0.3543(12) 0.0324(8) 0.171(6) Uani 1 1 d . . . N4N N 0.1387(16) 0.2792(14) 0.0754(16) 0.137(7) Uani 1 1 d . . . O1W O 0.1625(8) 0.1368(7) 0.2373(6) 0.124(4) Uani 1 1 d . . . H1W H 0.1462 0.1666 0.1921 0.186 Uiso 1 1 d R . . H2W H 0.1157 0.1447 0.2658 0.186 Uiso 1 1 d R . . O2W O 0.4124(8) 0.0760(5) 0.4191(5) 0.100(3) Uani 1 1 d . . . H3W H 0.3948 0.0177 0.4103 0.151 Uiso 1 1 d R . . H4W H 0.419 0.0925 0.4733 0.151 Uiso 1 1 d R . . O3W O 0.1372(9) 0.0840(7) 0.7179(7) 0.146(4) Uani 1 1 d . . . H5W H 0.1331 0.1427 0.7279 0.219 Uiso 1 1 d R . . H6W H 0.1884 0.0809 0.6923 0.219 Uiso 1 1 d R . . O4W O 0.2753(10) 0.4847(8) 0.1781(8) 0.187(6) Uani 1 1 d . . . H7W H 0.2128 0.4508 0.1522 0.28 Uiso 1 1 d R . . H8W H 0.2901 0.4772 0.233 0.28 Uiso 1 1 d R . . O5W O 0.0301(11) 0.0088(6) 0.4156(7) 0.200(7) Uani 1 1 d . . . H9W H 0.0319 0.0104 0.4605 0.299 Uiso 1 1 d R . . H10W H 0.0251 0.0785 0.4024 0.299 Uiso 1 1 d 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 0.0365(3) 0.0342(3) 0.0378(3) 0.0045(2) 0.0090(2) 0.0033(2) O2A 0.053(6) 0.039(5) 0.092(6) 0.019(4) 0.028(5) 0.006(4) O2B 0.065(6) 0.033(5) 0.057(5) -0.005(4) 0.002(4) -0.002(4) N1A 0.042(7) 0.048(6) 0.063(6) 0.009(5) 0.017(6) 0.015(5) N1B 0.046(7) 0.031(6) 0.054(6) 0.001(5) -0.003(5) -0.001(5) N1P 0.033(7) 0.042(6) 0.051(6) 0.003(5) 0.014(5) 0.001(5) N3A 0.037(6) 0.032(5) 0.043(5) 0.006(4) 0.016(5) 0.007(5) N3B 0.043(6) 0.029(5) 0.035(5) 0.010(4) 0.008(5) 0.007(5) N4A 0.063(7) 0.037(6) 0.073(7) 0.015(5) 0.033(6) 0.009(5) N4B 0.065(8) 0.031(6) 0.061(6) -0.003(5) -0.003(5) -0.002(5) N8P 0.042(7) 0.035(5) 0.038(6) 0.007(4) 0.017(5) 0.000(5) C1A 0.080(11) 0.066(9) 0.103(11) 0.017(8) 0.045(9) 0.018(8) C1B 0.073(10) 0.051(8) 0.075(9) 0.017(6) -0.011(7) 0.011(7) C2A 0.030(8) 0.071(10) 0.035(7) 0.006(6) 0.006(6) 0.010(7) C2B 0.038(8) 0.045(8) 0.041(7) 0.005(6) 0.000(6) 0.004(6) C2P 0.049(10) 0.052(8) 0.050(8) -0.008(6) 0.011(8) 0.004(7) C3P 0.037(9) 0.088(10) 0.081(10) -0.006(8) 0.023(9) -0.005(7) C4A 0.048(9) 0.024(7) 0.061(8) 0.004(6) 0.023(7) 0.012(6) C4B 0.030(8) 0.051(8) 0.040(7) 0.003(6) 0.008(6) 0.001(6) C4P 0.054(11) 0.084(10) 0.058(9) -0.002(7) 0.030(8) -0.007(8) C5A 0.066(10) 0.030(7) 0.106(11) 0.010(7) 0.047(9) 0.014(7) C5B 0.031(8) 0.059(8) 0.047(7) -0.002(6) 0.003(6) -0.004(6) C5P 0.062(11) 0.080(10) 0.048(8) 0.001(7) 0.018(8) 0.003(8) C6A 0.041(9) 0.104(12) 0.062(9) 0.023(8) 0.024(7) -0.003(9) C6B 0.058(10) 0.068(9) 0.049(8) 0.022(7) 0.005(7) 0.002(8) C6P 0.061(10) 0.048(7) 0.027(7) -0.009(5) 0.024(7) -0.002(7) C7P 0.027(8) 0.037(6) 0.036(7) -0.006(5) -0.002(6) 0.005(6) C9P 0.032(8) 0.068(8) 0.040(8) 0.008(6) 0.004(6) 0.006(7) C10P 0.055(9) 0.063(8) 0.042(8) -0.002(6) 0.002(7) 0.006(7) C11P 0.067(11) 0.048(7) 0.040(7) 0.002(6) 0.000(8) 0.011(7) C12P 0.047(9) 0.068(8) 0.026(7) -0.006(6) 0.008(6) -0.005(7) Pt2 0.0472(4) 0.0370(3) 0.0370(3) 0.0073(2) 0.0139(3) 0.0063(3) O2C 0.070(7) 0.049(5) 0.062(5) -0.009(4) 0.028(5) 0.000(5) O2D 0.075(6) 0.025(4) 0.055(5) 0.010(4) 0.017(4) 0.004(4) N1C 0.083(10) 0.041(7) 0.093(8) -0.009(6) 0.048(7) 0.000(7) N1D 0.059(7) 0.037(6) 0.055(6) 0.013(5) 0.015(6) 0.006(5) N1Y 0.039(7) 0.043(6) 0.038(6) 0.010(4) 0.012(5) 0.007(5) N3C 0.033(6) 0.055(6) 0.041(6) 0.012(5) 0.018(5) 0.001(5) N3D 0.045(7) 0.053(6) 0.024(5) 0.012(4) 0.010(5) 0.019(5) N4C 0.091(9) 0.028(6) 0.114(9) 0.009(6) 0.056(7) -0.004(6) N4D 0.071(8) 0.031(5) 0.047(6) 0.007(4) 0.006(5) 0.012(5) N8Y 0.046(7) 0.045(6) 0.040(6) 0.007(4) -0.003(6) 0.012(5) C1C 0.093(8) 0.039(6) 0.104(8) -0.003(5) 0.025(6) -0.027(5) C1D 0.093(8) 0.039(6) 0.104(8) -0.003(5) 0.025(6) -0.027(5) C2C 0.057(10) 0.057(10) 0.046(8) 0.004(7) 0.018(7) 0.000(8) C2D 0.053(9) 0.036(7) 0.046(8) -0.001(6) 0.024(7) -0.004(7) C2Y 0.036(9) 0.057(8) 0.047(8) 0.000(6) 0.004(7) 0.009(7) C3Y 0.040(9) 0.075(9) 0.072(10) 0.019(7) 0.020(8) 0.015(7) C4C 0.076(12) 0.077(10) 0.050(8) 0.025(7) 0.029(8) 0.036(9) C4D 0.049(8) 0.027(7) 0.041(7) 0.008(6) 0.014(6) 0.009(6) C4Y 0.058(11) 0.090(10) 0.074(10) 0.036(8) 0.031(9) 0.024(9) C5C 0.059(11) 0.116(14) 0.108(12) 0.009(10) 0.051(10) 0.027(10) C5D 0.055(9) 0.039(7) 0.046(7) 0.007(6) -0.001(7) 0.001(6) C5Y 0.057(10) 0.075(9) 0.047(8) 0.010(7) 0.030(8) 0.004(8) C6C 0.076(12) 0.096(13) 0.108(12) 0.015(10) 0.045(10) -0.011(11) C6D 0.044(9) 0.078(10) 0.050(8) 0.003(7) 0.002(7) 0.016(8) C6Y 0.050(9) 0.039(7) 0.046(8) 0.015(6) 0.016(7) 0.015(6) C7Y 0.060(10) 0.038(7) 0.038(7) -0.003(5) 0.028(7) 0.003(6) C9Y 0.049(10) 0.071(9) 0.058(9) 0.017(7) 0.015(8) 0.003(7) C10Y 0.052(10) 0.094(11) 0.062(9) 0.018(8) 0.000(8) 0.012(8) C11Y 0.058(11) 0.083(10) 0.039(8) 0.007(7) 0.001(8) -0.006(8) C12Y 0.057(10) 0.072(9) 0.032(7) 0.002(6) 0.006(7) -0.001(7) O11 0.094(9) 0.142(10) 0.086(8) 0.036(7) -0.024(7) -0.007(7) O12 0.117(10) 0.123(9) 0.129(9) 0.077(8) -0.004(7) -0.011(7) O13 0.136(10) 0.069(7) 0.115(8) 0.014(6) 0.007(7) -0.033(7) N1N 0.075(10) 0.088(10) 0.059(8) 0.021(8) 0.009(7) -0.004(8) O21 0.187(13) 0.147(11) 0.088(8) 0.035(8) 0.034(9) 0.021(9) O22 0.151(12) 0.143(11) 0.083(8) 0.018(7) 0.009(8) 0.002(9) O23 0.232(15) 0.078(8) 0.179(12) 0.006(8) 0.126(11) -0.020(9) N2N 0.124(13) 0.086(11) 0.078(11) -0.003(8) 0.055(10) -0.004(9) O31 0.110(10) 0.071(8) 0.185(12) 0.006(8) -0.016(8) 0.008(7) O32 0.242(18) 0.132(12) 0.188(14) -0.080(10) 0.050(13) -0.022(12) O33 0.126(13) 0.28(2) 0.34(2) 0.236(19) -0.073(13) 0.019(12) N3N 0.104(12) 0.044(8) 0.065(8) 0.006(7) 0.009(8) -0.005(8) O41 0.082(11) 0.25(2) 0.205(15) -0.021(13) 0.054(11) -0.032(11) O42 0.150(16) 0.189(15) 0.153(15) 0.025(12) 0.008(11) 0.011(12) O43 0.116(11) 0.275(19) 0.169(13) 0.080(13) 0.086(10) 0.079(13) N4N 0.097(18) 0.117(16) 0.21(3) 0.029(17) 0.075(17) -0.001(13) O1W 0.107(9) 0.129(9) 0.141(9) -0.016(7) 0.039(7) 0.051(7) O2W 0.168(10) 0.066(6) 0.086(7) 0.019(5) 0.066(7) 0.011(6) O3W 0.136(11) 0.146(11) 0.169(11) 0.007(8) 0.058(9) 0.045(9) O4W 0.166(13) 0.155(12) 0.199(13) -0.019(9) -0.016(10) 0.053(10) O5W 0.310(18) 0.054(7) 0.169(11) 0.003(7) -0.036(11) 0.025(9) #----------------------------------------------------------------------------# # 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 N1P 2.000(8) . ? Pt1 N8P 2.022(8) . ? Pt1 N3B 2.020(7) . ? Pt1 N3A 2.038(8) . ? O2A C2A 1.222(12) . ? O2B C2B 1.210(11) . ? N1A C2A 1.377(12) . ? N1A C6A 1.410(13) . ? N1A C1A 1.446(12) . ? N1B C6B 1.350(12) . ? N1B C2B 1.384(11) . ? N1B C1B 1.464(11) . ? N1P C6P 1.349(11) . ? N1P C2P 1.363(12) . ? N3A C4A 1.343(11) . ? N3A C2A 1.400(13) . ? N3B C4B 1.376(11) . ? N3B C2B 1.378(12) . ? N4A C4A 1.262(11) . ? N4A H39 0.86 . ? N4A H40 0.86 . ? N4B C4B 1.312(11) . ? N4B H43 0.8599 . ? N4B H44 0.86 . ? N8P C9P 1.331(12) . ? N8P C7P 1.356(12) . ? C1A H29 0.96 . ? C1A H30 0.96 . ? C1A H31 0.96 . ? C1B H7 0.96 . ? C1B H8 0.96 . ? C1B H9 0.96 . ? C2P C3P 1.394(14) . ? C2P H42 0.93 . ? C3P C4P 1.354(14) . ? C3P H26 0.93 . ? C4A C5A 1.380(14) . ? C4B C5B 1.424(12) . ? C4P C5P 1.392(14) . ? C4P H28 0.93 . ? C5A C6A 1.311(14) . ? C5A H32 0.93 . ? C5B C6B 1.370(13) . ? C5B H38 0.93 . ? C5P C6P 1.390(14) . ? C5P H34 0.93 . ? C6A H27 0.93 . ? C6B H37 0.93 . ? C6P C7P 1.459(14) . ? C7P C12P 1.367(12) . ? C9P C10P 1.359(12) . ? C9P H41 0.93 . ? C10P C11P 1.379(14) . ? C10P H35 0.93 . ? C11P C12P 1.381(14) . ? C11P H36 0.93 . ? C12P H33 0.93 . ? Pt2 N8Y 2.025(8) . ? Pt2 N1Y 2.031(8) . ? Pt2 N3C 2.044(8) . ? Pt2 N3D 2.056(7) . ? O2C C2C 1.214(13) . ? O2D C2D 1.206(11) . ? N1C C6C 1.345(15) . ? N1C C2C 1.375(14) . ? N1C C1C 1.433(12) . ? N1D C6D 1.390(12) . ? N1D C2D 1.396(12) . ? N1D C1D 1.435(12) . ? N1Y C2Y 1.335(12) . ? N1Y C6Y 1.355(11) . ? N3C C2C 1.393(13) . ? N3C C4C 1.426(13) . ? N3D C4D 1.364(11) . ? N3D C2D 1.409(12) . ? N4C C4C 1.276(14) . ? N4C H21 0.8601 . ? N4C H22 0.8599 . ? N4D C4D 1.296(11) . ? N4D H24 0.8599 . ? N4D H25 0.86 . ? N8Y C9Y 1.357(13) . ? N8Y C7Y 1.385(12) . ? C1C H1 0.96 . ? C1C H2 0.96 . ? C1C H3 0.96 . ? C1D H4 0.96 . ? C1D H5 0.96 . ? C1D H6 0.96 . ? C2Y C3Y 1.391(13) . ? C2Y H20 0.93 . ? C3Y C4Y 1.366(13) . ? C3Y H17 0.93 . ? C4C C5C 1.471(16) . ? C4D C5D 1.382(12) . ? C4Y C5Y 1.352(14) . ? C4Y H14 0.93 . ? C5C C6C 1.415(17) . ? C5C H12 0.93 . ? C5D C6D 1.351(13) . ? C5D H23 0.93 . ? C5Y C6Y 1.377(13) . ? C5Y H16 0.93 . ? C6C H11 0.93 . ? C6D H19 0.93 . ? C6Y C7Y 1.462(14) . ? C7Y C12Y 1.396(13) . ? C9Y C10Y 1.387(13) . ? C9Y H18 0.93 . ? C10Y C11Y 1.380(14) . ? C10Y H10 0.93 . ? C11Y C12Y 1.370(14) . ? C11Y H13 0.93 . ? C12Y H15 0.93 . ? O11 N1N 1.212(12) . ? O12 N1N 1.207(11) . ? O13 N1N 1.217(12) . ? O21 N2N 1.212(13) . ? O22 N2N 1.260(14) . ? O23 N2N 1.214(13) . ? O31 N3N 1.135(12) . ? O32 N3N 1.165(14) . ? O33 N3N 1.056(14) . ? O41 N4N 1.23(2) . ? O42 N4N 1.17(2) . ? O43 N4N 1.32(2) . ? O1W H1W 0.8472 . ? O1W H2W 0.847 . ? O2W H3W 0.843 . ? O2W H4W 0.8538 . ? O3W H5W 0.8651 . ? O3W H6W 0.8535 . ? O4W H7W 0.8586 . ? O4W H8W 0.8528 . ? O5W H9W 0.704 . ? O5W H10W 1.0484 . ? 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 N1P Pt1 N8P 80.7(4) . . ? N1P Pt1 N3B 95.0(3) . . ? N8P Pt1 N3B 175.7(3) . . ? N1P Pt1 N3A 175.3(3) . . ? N8P Pt1 N3A 94.8(3) . . ? N3B Pt1 N3A 89.5(3) . . ? C2A N1A C6A 119.4(10) . . ? C2A N1A C1A 118.4(10) . . ? C6A N1A C1A 122.0(11) . . ? C6B N1B C2B 121.3(9) . . ? C6B N1B C1B 119.4(9) . . ? C2B N1B C1B 119.2(8) . . ? C6P N1P C2P 119.3(10) . . ? C6P N1P Pt1 114.8(8) . . ? C2P N1P Pt1 125.9(8) . . ? C4A N3A C2A 120.8(9) . . ? C4A N3A Pt1 125.6(8) . . ? C2A N3A Pt1 113.6(7) . . ? C4B N3B C2B 121.3(9) . . ? C4B N3B Pt1 122.2(6) . . ? C2B N3B Pt1 116.4(7) . . ? C4A N4A H39 121.2 . . ? C4A N4A H40 118.8 . . ? H39 N4A H40 120 . . ? C4B N4B H43 120.9 . . ? C4B N4B H44 119.1 . . ? H43 N4B H44 120 . . ? C9P N8P C7P 119.2(9) . . ? C9P N8P Pt1 126.8(7) . . ? C7P N8P Pt1 114.0(7) . . ? N1A C1A H29 109.5 . . ? N1A C1A H30 109.5 . . ? H29 C1A H30 109.5 . . ? N1A C1A H31 109.5 . . ? H29 C1A H31 109.5 . . ? H30 C1A H31 109.5 . . ? N1B C1B H7 109.5 . . ? N1B C1B H8 109.5 . . ? H7 C1B H8 109.5 . . ? N1B C1B H9 109.5 . . ? H7 C1B H9 109.5 . . ? H8 C1B H9 109.5 . . ? O2A C2A N1A 120.5(11) . . ? O2A C2A N3A 122.6(11) . . ? N1A C2A N3A 117.0(10) . . ? O2B C2B N3B 120.6(10) . . ? O2B C2B N1B 121.1(10) . . ? N3B C2B N1B 118.3(9) . . ? N1P C2P C3P 122.6(10) . . ? N1P C2P H42 118.7 . . ? C3P C2P H42 118.7 . . ? C4P C3P C2P 118.2(12) . . ? C4P C3P H26 120.9 . . ? C2P C3P H26 120.9 . . ? N4A C4A N3A 117.8(11) . . ? N4A C4A C5A 119.9(10) . . ? N3A C4A C5A 122.3(10) . . ? N4B C4B N3B 120.2(9) . . ? N4B C4B C5B 120.6(10) . . ? N3B C4B C5B 119.2(9) . . ? C3P C4P C5P 119.5(12) . . ? C3P C4P H28 120.3 . . ? C5P C4P H28 120.3 . . ? C6A C5A C4A 117.6(11) . . ? C6A C5A H32 121.2 . . ? C4A C5A H32 121.2 . . ? C6B C5B C4B 118.1(10) . . ? C6B C5B H38 120.9 . . ? C4B C5B H38 120.9 . . ? C6P C5P C4P 121.0(11) . . ? C6P C5P H34 119.5 . . ? C4P C5P H34 119.5 . . ? C5A C6A N1A 122.8(11) . . ? C5A C6A H27 118.6 . . ? N1A C6A H27 118.6 . . ? N1B C6B C5B 121.6(10) . . ? N1B C6B H37 119.2 . . ? C5B C6B H37 119.2 . . ? N1P C6P C5P 119.4(11) . . ? N1P C6P C7P 115.1(10) . . ? C5P C6P C7P 125.5(10) . . ? N8P C7P C12P 120.9(10) . . ? N8P C7P C6P 114.9(9) . . ? C12P C7P C6P 124.1(11) . . ? N8P C9P C10P 121.5(11) . . ? N8P C9P H41 119.3 . . ? C10P C9P H41 119.3 . . ? C9P C10P C11P 121.0(11) . . ? C9P C10P H35 119.5 . . ? C11P C10P H35 119.5 . . ? C10P C11P C12P 116.9(10) . . ? C10P C11P H36 121.5 . . ? C12P C11P H36 121.5 . . ? C7P C12P C11P 120.6(10) . . ? C7P C12P H33 119.7 . . ? C11P C12P H33 119.7 . . ? N8Y Pt2 N1Y 80.6(4) . . ? N8Y Pt2 N3C 94.3(4) . . ? N1Y Pt2 N3C 174.9(3) . . ? N8Y Pt2 N3D 174.1(4) . . ? N1Y Pt2 N3D 93.5(3) . . ? N3C Pt2 N3D 91.5(3) . . ? C6C N1C C2C 120.9(11) . . ? C6C N1C C1C 118.7(12) . . ? C2C N1C C1C 120.3(11) . . ? C6D N1D C2D 119.7(9) . . ? C6D N1D C1D 120.6(10) . . ? C2D N1D C1D 119.7(9) . . ? C2Y N1Y C6Y 118.8(10) . . ? C2Y N1Y Pt2 126.1(8) . . ? C6Y N1Y Pt2 115.0(8) . . ? C2C N3C C4C 123.8(10) . . ? C2C N3C Pt2 116.9(9) . . ? C4C N3C Pt2 119.2(8) . . ? C4D N3D C2D 123.6(9) . . ? C4D N3D Pt2 122.9(7) . . ? C2D N3D Pt2 113.5(7) . . ? C4C N4C H21 119.8 . . ? C4C N4C H22 120.2 . . ? H21 N4C H22 120 . . ? C4D N4D H24 121.1 . . ? C4D N4D H25 118.9 . . ? H24 N4D H25 120 . . ? C9Y N8Y C7Y 119.3(9) . . ? C9Y N8Y Pt2 126.5(8) . . ? C7Y N8Y Pt2 114.2(8) . . ? N1C C1C H1 109.5 . . ? N1C C1C H2 109.5 . . ? H1 C1C H2 109.5 . . ? N1C C1C H3 109.5 . . ? H1 C1C H3 109.5 . . ? H2 C1C H3 109.5 . . ? N1D C1D H4 109.5 . . ? N1D C1D H5 109.5 . . ? H4 C1D H5 109.5 . . ? N1D C1D H6 109.5 . . ? H4 C1D H6 109.5 . . ? H5 C1D H6 109.5 . . ? O2C C2C N1C 119.4(12) . . ? O2C C2C N3C 121.8(13) . . ? N1C C2C N3C 118.7(11) . . ? O2D C2D N1D 121.6(10) . . ? O2D C2D N3D 122.8(10) . . ? N1D C2D N3D 115.6(9) . . ? N1Y C2Y C3Y 121.1(10) . . ? N1Y C2Y H20 119.4 . . ? C3Y C2Y H20 119.4 . . ? C4Y C3Y C2Y 119.9(11) . . ? C4Y C3Y H17 120 . . ? C2Y C3Y H17 120 . . ? N4C C4C N3C 120.9(12) . . ? N4C C4C C5C 124.4(13) . . ? N3C C4C C5C 114.7(12) . . ? N4D C4D N3D 118.6(10) . . ? N4D C4D C5D 122.1(9) . . ? N3D C4D C5D 119.3(9) . . ? C5Y C4Y C3Y 118.4(12) . . ? C5Y C4Y H14 120.8 . . ? C3Y C4Y H14 120.8 . . ? C6C C5C C4C 118.1(13) . . ? C6C C5C H12 121 . . ? C4C C5C H12 121 . . ? C6D C5D C4D 118.5(10) . . ? C6D C5D H23 120.8 . . ? C4D C5D H23 120.8 . . ? C4Y C5Y C6Y 120.9(11) . . ? C4Y C5Y H16 119.6 . . ? C6Y C5Y H16 119.6 . . ? N1C C6C C5C 123.2(13) . . ? N1C C6C H11 118.4 . . ? C5C C6C H11 118.4 . . ? C5D C6D N1D 123.2(10) . . ? C5D C6D H19 118.4 . . ? N1D C6D H19 118.4 . . ? N1Y C6Y C5Y 120.7(11) . . ? N1Y C6Y C7Y 115.3(10) . . ? C5Y C6Y C7Y 124.0(11) . . ? N8Y C7Y C12Y 118.9(11) . . ? N8Y C7Y C6Y 114.9(10) . . ? C12Y C7Y C6Y 126.1(11) . . ? N8Y C9Y C10Y 122.6(11) . . ? N8Y C9Y H18 118.7 . . ? C10Y C9Y H18 118.7 . . ? C11Y C10Y C9Y 118.0(12) . . ? C11Y C10Y H10 121 . . ? C9Y C10Y H10 121 . . ? C12Y C11Y C10Y 120.4(11) . . ? C12Y C11Y H13 119.8 . . ? C10Y C11Y H13 119.8 . . ? C11Y C12Y C7Y 120.8(11) . . ? C11Y C12Y H15 119.6 . . ? C7Y C12Y H15 119.6 . . ? O13 N1N O12 120.2(13) . . ? O13 N1N O11 124.0(12) . . ? O12 N1N O11 115.5(13) . . ? O23 N2N O21 124.0(16) . . ? O23 N2N O22 121.8(15) . . ? O21 N2N O22 113.9(15) . . ? O33 N3N O31 120.9(17) . . ? O33 N3N O32 122.7(18) . . ? O31 N3N O32 116.4(16) . . ? O42 N4N O41 132(3) . . ? O42 N4N O43 117(2) . . ? O41 N4N O43 110(2) . . ? H1W O1W H2W 108.2 . . ? H3W O2W H4W 108 . . ? H5W O3W H6W 106 . . ? H7W O4W H8W 106.7 . . ? H9W O5W H10W 102.7 . . ? # 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 # Attachment '729008_shen.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-25 at 14:58:18 # 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_729008_shen _database_code_depnum_ccdc_archive 'CCDC 729008' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2009-05-25 _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 -------------------------# #_audit_creation_date 2009-05-25T14:58:18-00:00 #_audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H32 N10 O9 Pd2' _chemical_formula_sum 'C30 H32 N10 O9 Pd2' _chemical_formula_weight 889.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 14.188(3) _cell_length_b 16.115(3) _cell_length_c 17.888(7) _cell_angle_alpha 90 _cell_angle_beta 119.03(2) _cell_angle_gamma 90 _cell_volume 3576.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5239 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.1302 _diffrn_reflns_av_unetI/netI 0.2021 _diffrn_reflns_number 10021 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 23.74 _diffrn_reflns_theta_full 23.74 _diffrn_measured_fraction_theta_full 0.963 _diffrn_measured_fraction_theta_max 0.963 _reflns_number_total 5239 _reflns_number_gt 1846 _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^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5239 _refine_ls_number_parameters 424 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1795 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1767 _refine_ls_wR_factor_gt 0.154 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.853 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.596 _refine_diff_density_min -0.46 _refine_diff_density_rms 0.098 #----------------------------------------------------------------------------# # 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' Pd Pd -0.9988 1.0072 '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 Pd1 Pd -0.41126(8) 0.38747(6) -0.10508(6) 0.1002(4) Uani 1 1 d . . . Pd2 Pd -0.22050(8) 0.41204(6) -0.11965(6) 0.1043(4) Uani 1 1 d . . . N1A N -0.4257(8) 0.5088(6) -0.0807(9) 0.098(3) Uani 1 1 d . . . N1B N -0.1182(9) 0.4272(8) 0.0047(7) 0.107(3) Uani 1 1 d . . . N1C N -0.3297(14) 0.4056(6) -0.2474(7) 0.114(4) Uani 1 1 d . . . N1D N -0.3869(11) 0.2669(6) -0.1198(6) 0.102(3) Uani 1 1 d . . . N2C N -0.4787(10) 0.4011(7) -0.2292(7) 0.119(4) Uani 1 1 d . . . H23 H -0.5476 0.4067 -0.2545 0.143 Uiso 1 1 d R . . N2D N -0.2211(9) 0.2908(7) -0.1127(6) 0.120(3) Uani 1 1 d . . . H20 H -0.1632 0.2662 -0.1049 0.143 Uiso 1 1 d R . . N8A N -0.3415(7) 0.3840(7) 0.0243(6) 0.096(3) Uani 1 1 d . . . N8B N -0.2103(9) 0.5369(6) -0.1163(8) 0.099(3) Uani 1 1 d . . . C2A C -0.4720(11) 0.5691(11) -0.1383(9) 0.125(5) Uani 1 1 d . . . H8 H -0.5065 0.5556 -0.1961 0.15 Uiso 1 1 calc R . . C2B C -0.0763(14) 0.3692(12) 0.0602(13) 0.128(5) Uani 1 1 d . . . H7 H -0.0889 0.3147 0.0407 0.154 Uiso 1 1 calc R . . C2C C -0.4429(15) 0.4000(8) -0.2803(11) 0.109(5) Uani 1 1 d . . . C2D C -0.2968(14) 0.2378(9) -0.1168(7) 0.100(4) Uani 1 1 d . . . C3A C -0.4704(12) 0.6502(10) -0.1150(13) 0.121(5) Uani 1 1 d . . . H18 H -0.5029 0.6913 -0.1562 0.145 Uiso 1 1 calc R . . C3B C -0.0131(14) 0.3822(12) 0.1478(15) 0.145(6) Uani 1 1 d . . . H4 H 0.0159 0.338 0.1857 0.174 Uiso 1 1 calc R . . C3C C -0.5095(19) 0.3948(9) -0.3700(14) 0.138(8) Uani 1 1 d . . . H1 H -0.5835 0.3884 -0.3927 0.166 Uiso 1 1 calc R . . C3D C -0.2853(13) 0.1482(10) -0.1155(7) 0.115(5) Uani 1 1 d . . . H21 H -0.2225 0.125 -0.1105 0.138 Uiso 1 1 calc R . . C4A C -0.4228(15) 0.6683(10) -0.0350(16) 0.144(6) Uani 1 1 d . . . H11 H -0.4199 0.7237 -0.0196 0.172 Uiso 1 1 calc R . . C4B C 0.0045(13) 0.4626(17) 0.1756(10) 0.153(6) Uani 1 1 d . . . H10 H 0.0443 0.4738 0.2339 0.184 Uiso 1 1 calc R . . C4C C -0.470(2) 0.3989(10) -0.4200(16) 0.166(9) Uani 1 1 d . . . H3 H -0.5168 0.3962 -0.4785 0.2 Uiso 1 1 calc R . . C4D C -0.3630(17) 0.0996(9) -0.1212(8) 0.126(5) Uani 1 1 d . . . H22 H -0.3553 0.0424 -0.1221 0.151 Uiso 1 1 calc R . . C5A C -0.3762(12) 0.6109(12) 0.0288(10) 0.131(5) Uani 1 1 d . . . H5A H -0.3438 0.6252 0.0864 0.158 Uiso 1 1 calc R . . C5B C -0.0364(13) 0.5278(10) 0.1179(13) 0.139(5) Uani 1 1 d . . . H5B H -0.0213 0.583 0.1348 0.167 Uiso 1 1 calc R . . C5C C -0.359(2) 0.4073(10) -0.3931(13) 0.158(7) Uani 1 1 d . . . H2 H -0.3315 0.4111 -0.4309 0.19 Uiso 1 1 calc R . . C5D C -0.4501(17) 0.1302(11) -0.1256(9) 0.131(5) Uani 1 1 d . . . H12 H -0.5042 0.0951 -0.1292 0.158 Uiso 1 1 calc R . . C6A C -0.3807(10) 0.5271(9) 0.0008(11) 0.102(4) Uani 1 1 d . . . C6B C -0.1025(10) 0.5046(11) 0.0317(10) 0.104(4) Uani 1 1 d . . . C6C C -0.2929(14) 0.4094(8) -0.3032(15) 0.143(5) Uani 1 1 d . . . H6C H -0.2188 0.4137 -0.2815 0.172 Uiso 1 1 calc R . . C6D C -0.4617(14) 0.2139(12) -0.1249(7) 0.123(5) Uani 1 1 d . . . H13 H -0.5246 0.235 -0.1282 0.148 Uiso 1 1 calc R . . C7A C -0.3304(10) 0.4604(9) 0.0628(10) 0.091(3) Uani 1 1 d . . . C7B C -0.1545(12) 0.5678(10) -0.0367(11) 0.111(4) Uani 1 1 d . . . C9A C -0.3002(11) 0.3151(8) 0.0753(10) 0.108(4) Uani 1 1 d . . . H14 H -0.3082 0.2634 0.0497 0.13 Uiso 1 1 calc R . . C9B C -0.2568(10) 0.5895(9) -0.1833(9) 0.116(4) Uani 1 1 d . . . H19 H -0.2957 0.5677 -0.2381 0.139 Uiso 1 1 calc R . . C10A C -0.2472(11) 0.3205(10) 0.1630(11) 0.118(4) Uani 1 1 d . . . H17 H -0.2202 0.273 0.1963 0.142 Uiso 1 1 calc R . . C10B C -0.2483(12) 0.6770(10) -0.1730(11) 0.137(5) Uani 1 1 d . . . H15 H -0.2763 0.7128 -0.2196 0.164 Uiso 1 1 calc R . . C11A C -0.2349(11) 0.3968(13) 0.2006(9) 0.126(5) Uani 1 1 d . . . H9 H -0.1998 0.4016 0.2599 0.151 Uiso 1 1 calc R . . C11B C -0.1973(15) 0.7055(10) -0.0916(14) 0.146(6) Uani 1 1 d . . . H5 H -0.1983 0.7622 -0.082 0.176 Uiso 1 1 calc R . . C12A C -0.2749(12) 0.4667(9) 0.1499(12) 0.114(4) Uani 1 1 d . . . H6 H -0.2639 0.5186 0.1754 0.137 Uiso 1 1 calc R . . C12B C -0.1447(12) 0.6542(12) -0.0237(10) 0.126(5) Uani 1 1 d . . . H16 H -0.1028 0.6758 0.0309 0.151 Uiso 1 1 calc R . . N10 N -0.2362(15) 0.8375(12) 0.1080(16) 0.440(10) Uani 1 1 d D . . O11 O -0.3152(16) 0.8169(17) 0.1232(17) 0.440(10) Uani 1 1 d D . . O12 O -0.1547(16) 0.7849(14) 0.1321(16) 0.440(10) Uani 1 1 d D . . O13 O -0.213(2) 0.9178(12) 0.1105(15) 0.440(10) Uani 1 1 d D . . N20 N -0.0125(19) 0.354(4) -0.3290(14) 0.695(18) Uani 1 1 d D . . O21 O -0.092(3) 0.362(4) -0.311(3) 0.695(18) Uani 1 1 d D . . O22 O -0.036(3) 0.345(2) -0.4092(15) 0.695(18) Uani 1 1 d D . . O23 O 0.089(2) 0.363(3) -0.268(2) 0.695(18) Uani 1 1 d D . . O1W O -0.7382(13) 0.4005(11) -0.3096(14) 0.346(13) Uani 1 1 d . . . H1W H -0.7817 0.4105 -0.2903 0.52 Uiso 1 1 d R . . H2W H -0.7607 0.354 -0.3377 0.52 Uiso 1 1 d R . . O2W O -0.0365(10) 0.2080(17) -0.1241(14) 0.50(2) Uani 1 1 d . . . H3W H 0.0206 0.2272 -0.0825 0.753 Uiso 1 1 d R . . H4W H -0.0214 0.1813 -0.1564 0.753 Uiso 1 1 d R . . O3W O -0.117(4) 0.542(2) -0.511(4) 0.83(5) Uani 1 1 d . . . H5W H -0.0884 0.5759 -0.4731 1.246 Uiso 1 1 d R . . H6W H -0.0903 0.4938 -0.4942 1.246 Uiso 1 1 d 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 Pd1 0.1094(8) 0.0847(7) 0.0987(8) 0.0064(5) 0.0443(6) 0.0006(5) Pd2 0.1200(9) 0.0904(7) 0.1037(8) -0.0013(5) 0.0553(6) -0.0082(6) N1A 0.103(8) 0.083(7) 0.106(9) 0.015(7) 0.050(7) 0.009(6) N1B 0.121(9) 0.073(8) 0.118(9) 0.012(8) 0.051(7) -0.006(7) N1C 0.187(15) 0.085(7) 0.085(8) -0.007(6) 0.077(10) -0.007(8) N1D 0.107(10) 0.083(8) 0.115(8) -0.006(5) 0.054(7) -0.034(7) N2C 0.119(9) 0.141(10) 0.083(8) 0.016(7) 0.039(7) -0.002(7) N2D 0.113(9) 0.104(8) 0.149(9) -0.014(6) 0.070(7) -0.017(7) N8A 0.101(7) 0.090(8) 0.104(8) 0.011(7) 0.055(6) -0.007(6) N8B 0.114(8) 0.082(7) 0.104(8) -0.011(7) 0.055(7) -0.024(7) C2A 0.127(12) 0.105(13) 0.130(12) 0.023(11) 0.052(10) -0.005(9) C2B 0.122(13) 0.149(16) 0.115(13) -0.017(12) 0.059(11) -0.030(11) C2C 0.120(14) 0.092(9) 0.074(13) -0.004(8) 0.015(11) -0.014(9) C2D 0.102(13) 0.104(14) 0.091(9) -0.009(7) 0.044(9) 0.009(10) C3A 0.114(13) 0.087(12) 0.162(16) 0.024(10) 0.067(12) 0.012(9) C3B 0.118(14) 0.136(16) 0.19(2) 0.025(13) 0.080(14) -0.011(11) C3C 0.21(2) 0.070(9) 0.16(2) 0.011(10) 0.11(2) 0.009(10) C3D 0.152(14) 0.073(10) 0.123(11) -0.019(7) 0.070(10) -0.023(10) C4A 0.153(16) 0.091(12) 0.190(19) -0.008(14) 0.087(15) 0.002(11) C4B 0.130(14) 0.22(2) 0.091(12) 0.005(15) 0.038(10) -0.036(15) C4C 0.16(2) 0.090(12) 0.19(2) -0.021(12) 0.042(18) -0.008(13) C4D 0.184(18) 0.076(11) 0.116(11) -0.020(8) 0.071(12) 0.001(13) C5A 0.146(14) 0.112(13) 0.133(13) -0.003(11) 0.065(11) 0.001(10) C5B 0.150(14) 0.133(13) 0.122(14) 0.017(12) 0.055(12) 0.012(11) C5C 0.26(3) 0.121(13) 0.101(15) -0.006(10) 0.092(16) 0.007(15) C5D 0.190(19) 0.082(13) 0.143(13) -0.019(9) 0.097(13) -0.022(11) C6A 0.088(10) 0.109(13) 0.113(13) -0.003(10) 0.052(9) -0.009(8) C6B 0.098(10) 0.132(14) 0.084(12) -0.005(10) 0.044(9) -0.007(9) C6C 0.170(16) 0.106(11) 0.151(17) -0.010(11) 0.075(16) 0.010(10) C6D 0.156(15) 0.114(13) 0.094(10) -0.005(8) 0.056(9) 0.006(12) C7A 0.086(9) 0.093(11) 0.094(12) 0.000(9) 0.045(8) -0.004(8) C7B 0.126(12) 0.100(12) 0.113(13) -0.005(10) 0.063(10) -0.022(9) C9A 0.131(12) 0.088(10) 0.108(12) 0.014(9) 0.059(9) 0.012(8) C9B 0.127(12) 0.094(11) 0.118(11) 0.012(9) 0.052(9) 0.017(9) C10A 0.118(12) 0.126(14) 0.096(12) 0.023(10) 0.041(9) 0.001(9) C10B 0.140(14) 0.108(14) 0.133(14) 0.005(10) 0.042(11) -0.025(10) C11A 0.125(12) 0.150(15) 0.082(10) -0.004(12) 0.035(8) -0.013(11) C11B 0.172(17) 0.082(11) 0.172(17) 0.003(12) 0.073(14) -0.010(11) C12A 0.125(12) 0.103(11) 0.114(13) -0.008(10) 0.059(10) -0.006(9) C12B 0.131(13) 0.118(14) 0.129(14) -0.026(11) 0.063(11) -0.028(10) N10 0.38(2) 0.46(2) 0.364(12) -0.125(15) 0.088(14) 0.018(16) O11 0.38(2) 0.46(2) 0.364(12) -0.125(15) 0.088(14) 0.018(16) O12 0.38(2) 0.46(2) 0.364(12) -0.125(15) 0.088(14) 0.018(16) O13 0.38(2) 0.46(2) 0.364(12) -0.125(15) 0.088(14) 0.018(16) N20 0.66(4) 0.52(3) 0.76(4) -0.36(3) 0.24(3) -0.12(3) O21 0.66(4) 0.52(3) 0.76(4) -0.36(3) 0.24(3) -0.12(3) O22 0.66(4) 0.52(3) 0.76(4) -0.36(3) 0.24(3) -0.12(3) O23 0.66(4) 0.52(3) 0.76(4) -0.36(3) 0.24(3) -0.12(3) O1W 0.240(16) 0.249(18) 0.53(3) -0.25(2) 0.170(18) -0.074(14) O2W 0.095(9) 0.76(5) 0.54(3) -0.51(4) 0.066(14) -0.063(17) O3W 0.76(9) 0.27(4) 1.47(14) -0.15(6) 0.55(10) -0.05(4) #----------------------------------------------------------------------------# # 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 Pd1 N2C 1.957(11) . ? Pd1 N1D 2.014(11) . ? Pd1 N8A 2.029(9) . ? Pd1 N1A 2.034(10) . ? Pd1 Pd2 2.8695(15) . ? Pd2 N2D 1.958(11) . ? Pd2 N1B 1.996(11) . ? Pd2 N8B 2.016(9) . ? Pd2 N1C 2.049(11) . ? N1A C6A 1.310(13) . ? N1A C2A 1.335(14) . ? N1B C2B 1.281(18) . ? N1B C6B 1.317(16) . ? N1C C6C 1.333(19) . ? N1C C2C 1.420(17) . ? N1D C2D 1.337(15) . ? N1D C6D 1.330(17) . ? N2C C2C 1.244(17) . ? N2C H23 0.86 . ? N2D C2D 1.346(16) . ? N2D H20 0.86 . ? N8A C9A 1.374(14) . ? N8A C7A 1.381(14) . ? N8B C7B 1.344(14) . ? N8B C9B 1.350(13) . ? C2A C3A 1.368(18) . ? C2A H8 0.93 . ? C2B C3B 1.393(19) . ? C2B H7 0.93 . ? C2C C3C 1.41(2) . ? C2D C3D 1.452(18) . ? C3A C4A 1.286(17) . ? C3A H18 0.93 . ? C3B C4B 1.37(2) . ? C3B H4 0.93 . ? C3C C4C 1.27(2) . ? C3C H1 0.93 . ? C3D C4D 1.315(17) . ? C3D H21 0.93 . ? C4A C5A 1.364(19) . ? C4A H11 0.93 . ? C4B C5B 1.39(2) . ? C4B H10 0.93 . ? C4C C5C 1.41(2) . ? C4C H3 0.93 . ? C4D C5D 1.297(19) . ? C4D H22 0.93 . ? C5A C6A 1.431(18) . ? C5A H5A 0.93 . ? C5B C6B 1.411(17) . ? C5B H5B 0.93 . ? C5C C6C 1.416(19) . ? C5C H2 0.93 . ? C5D C6D 1.360(18) . ? C5D H12 0.93 . ? C6A C7A 1.459(16) . ? C6B C7B 1.484(18) . ? C6C H6C 0.93 . ? C6D H13 0.93 . ? C7A C12A 1.367(16) . ? C7B C12B 1.408(18) . ? C9A C10A 1.375(15) . ? C9A H14 0.93 . ? C9B C10B 1.420(17) . ? C9B H19 0.93 . ? C10A C11A 1.373(18) . ? C10A H17 0.93 . ? C10B C11B 1.353(18) . ? C10B H15 0.93 . ? C11A C12A 1.383(18) . ? C11A H9 0.93 . ? C11B C12B 1.355(17) . ? C11B H5 0.93 . ? C12A H6 0.93 . ? C12B H16 0.93 . ? N10 O11 1.318(10) . ? N10 O12 1.325(10) . ? N10 O13 1.332(10) . ? N20 O21 1.314(9) . ? N20 O22 1.317(9) . ? N20 O23 1.332(9) . ? O1W H1W 0.8558 . ? O1W H2W 0.8715 . ? O2W H3W 0.849 . ? O2W H4W 0.8271 . ? O3W H5W 0.8148 . ? O3W H6W 0.8453 . ? 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 N2C Pd1 N1D 88.9(4) . . ? N2C Pd1 N8A 175.1(5) . . ? N1D Pd1 N8A 95.9(4) . . ? N2C Pd1 N1A 95.2(5) . . ? N1D Pd1 N1A 175.5(5) . . ? N8A Pd1 N1A 80.0(5) . . ? N2C Pd1 Pd2 81.1(4) . . ? N1D Pd1 Pd2 83.8(4) . . ? N8A Pd1 Pd2 98.5(3) . . ? N1A Pd1 Pd2 94.8(3) . . ? N2D Pd2 N1B 94.3(5) . . ? N2D Pd2 N8B 175.1(5) . . ? N1B Pd2 N8B 80.9(5) . . ? N2D Pd2 N1C 89.8(4) . . ? N1B Pd2 N1C 175.5(5) . . ? N8B Pd2 N1C 95.0(5) . . ? N2D Pd2 Pd1 79.8(4) . . ? N1B Pd2 Pd1 97.1(3) . . ? N8B Pd2 Pd1 101.1(3) . . ? N1C Pd2 Pd1 81.8(5) . . ? C6A N1A C2A 119.1(13) . . ? C6A N1A Pd1 114.2(10) . . ? C2A N1A Pd1 126.7(12) . . ? C2B N1B C6B 118.4(13) . . ? C2B N1B Pd2 126.0(12) . . ? C6B N1B Pd2 115.3(10) . . ? C6C N1C C2C 117.9(14) . . ? C6C N1C Pd2 118.2(15) . . ? C2C N1C Pd2 123.9(12) . . ? C2D N1D C6D 119.6(13) . . ? C2D N1D Pd1 123.7(10) . . ? C6D N1D Pd1 116.5(12) . . ? C2C N2C Pd1 133.1(12) . . ? C2C N2C H23 112.3 . . ? Pd1 N2C H23 114.5 . . ? C2D N2D Pd2 131.1(10) . . ? C2D N2D H20 113 . . ? Pd2 N2D H20 115.9 . . ? C9A N8A C7A 118.8(10) . . ? C9A N8A Pd1 126.4(10) . . ? C7A N8A Pd1 114.7(9) . . ? C7B N8B C9B 119.3(12) . . ? C7B N8B Pd2 113.5(10) . . ? C9B N8B Pd2 127.1(10) . . ? N1A C2A C3A 122.1(14) . . ? N1A C2A H8 119 . . ? C3A C2A H8 119 . . ? N1B C2B C3B 124.4(16) . . ? N1B C2B H7 117.8 . . ? C3B C2B H7 117.8 . . ? N2C C2C C3C 123.3(19) . . ? N2C C2C N1C 118.5(15) . . ? C3C C2C N1C 118.2(17) . . ? N1D C2D N2D 120.1(13) . . ? N1D C2D C3D 116.5(14) . . ? N2D C2D C3D 123.3(15) . . ? C4A C3A C2A 118.6(16) . . ? C4A C3A H18 120.7 . . ? C2A C3A H18 120.7 . . ? C4B C3B C2B 117.2(17) . . ? C4B C3B H4 121.4 . . ? C2B C3B H4 121.4 . . ? C4C C3C C2C 121(2) . . ? C4C C3C H1 119.5 . . ? C2C C3C H1 119.5 . . ? C4D C3D C2D 120.5(16) . . ? C4D C3D H21 119.8 . . ? C2D C3D H21 119.8 . . ? C3A C4A C5A 123.9(17) . . ? C3A C4A H11 118.1 . . ? C5A C4A H11 118.1 . . ? C3B C4B C5B 120.6(16) . . ? C3B C4B H10 119.7 . . ? C5B C4B H10 119.7 . . ? C3C C4C C5C 125(3) . . ? C3C C4C H3 117.7 . . ? C5C C4C H3 117.7 . . ? C5D C4D C3D 121.1(16) . . ? C5D C4D H22 119.4 . . ? C3D C4D H22 119.4 . . ? C4A C5A C6A 115.1(15) . . ? C4A C5A H5A 122.4 . . ? C6A C5A H5A 122.4 . . ? C4B C5B C6B 115.4(16) . . ? C4B C5B H5B 122.3 . . ? C6B C5B H5B 122.3 . . ? C4C C5C C6C 114(2) . . ? C4C C5C H2 123.1 . . ? C6C C5C H2 123.1 . . ? C4D C5D C6D 119.5(17) . . ? C4D C5D H12 120.3 . . ? C6D C5D H12 120.3 . . ? N1A C6A C5A 121.2(13) . . ? N1A C6A C7A 118.3(14) . . ? C5A C6A C7A 120.4(15) . . ? N1B C6B C5B 123.8(14) . . ? N1B C6B C7B 114.8(14) . . ? C5B C6B C7B 121.3(16) . . ? N1C C6C C5C 124.5(17) . . ? N1C C6C H6C 117.7 . . ? C5C C6C H6C 117.7 . . ? N1D C6D C5D 122.7(16) . . ? N1D C6D H13 118.6 . . ? C5D C6D H13 118.6 . . ? C12A C7A N8A 119.8(12) . . ? C12A C7A C6A 127.6(14) . . ? N8A C7A C6A 112.5(13) . . ? N8B C7B C12B 120.1(13) . . ? N8B C7B C6B 114.9(14) . . ? C12B C7B C6B 124.9(16) . . ? C10A C9A N8A 121.8(12) . . ? C10A C9A H14 119.1 . . ? N8A C9A H14 119.1 . . ? N8B C9B C10B 122.4(13) . . ? N8B C9B H19 118.8 . . ? C10B C9B H19 118.8 . . ? C9A C10A C11A 119.0(13) . . ? C9A C10A H17 120.5 . . ? C11A C10A H17 120.5 . . ? C11B C10B C9B 116.3(14) . . ? C11B C10B H15 121.8 . . ? C9B C10B H15 121.8 . . ? C10A C11A C12A 119.6(13) . . ? C10A C11A H9 120.2 . . ? C12A C11A H9 120.2 . . ? C10B C11B C12B 122.1(16) . . ? C10B C11B H5 118.9 . . ? C12B C11B H5 118.9 . . ? C7A C12A C11A 120.9(13) . . ? C7A C12A H6 119.6 . . ? C11A C12A H6 119.6 . . ? C11B C12B C7B 119.2(14) . . ? C11B C12B H16 120.4 . . ? C7B C12B H16 120.4 . . ? O11 N10 O12 117.8(12) . . ? O11 N10 O13 117.4(12) . . ? O12 N10 O13 116.5(12) . . ? O21 N20 O22 119.2(11) . . ? O21 N20 O23 120.4(11) . . ? O22 N20 O23 120.1(11) . . ? H1W O1W H2W 105.3 . . ? H3W O2W H4W 110 . . ? H5W O3W H6W 111.5 . . ? 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 N2C Pd1 Pd2 N2D -98.4(4) . . . . ? N1D Pd1 Pd2 N2D -8.6(4) . . . . ? N8A Pd1 Pd2 N2D 86.5(5) . . . . ? N1A Pd1 Pd2 N2D 167.1(5) . . . . ? N2C Pd1 Pd2 N1B 168.5(5) . . . . ? N1D Pd1 Pd2 N1B -101.7(5) . . . . ? N8A Pd1 Pd2 N1B -6.6(5) . . . . ? N1A Pd1 Pd2 N1B 74.0(5) . . . . ? N2C Pd1 Pd2 N8B 86.4(5) . . . . ? N1D Pd1 Pd2 N8B 176.3(5) . . . . ? N8A Pd1 Pd2 N8B -88.7(5) . . . . ? N1A Pd1 Pd2 N8B -8.0(5) . . . . ? N2C Pd1 Pd2 N1C -7.1(4) . . . . ? N1D Pd1 Pd2 N1C 82.7(4) . . . . ? N8A Pd1 Pd2 N1C 177.8(4) . . . . ? N1A Pd1 Pd2 N1C -101.6(5) . . . . ? N2C Pd1 N1A C6A -175.5(9) . . . . ? N8A Pd1 N1A C6A 3.8(8) . . . . ? Pd2 Pd1 N1A C6A -94.0(8) . . . . ? N2C Pd1 N1A C2A 2.2(11) . . . . ? N8A Pd1 N1A C2A -178.6(11) . . . . ? Pd2 Pd1 N1A C2A 83.6(10) . . . . ? N2D Pd2 N1B C2B -0.3(13) . . . . ? N8B Pd2 N1B C2B -179.9(13) . . . . ? Pd1 Pd2 N1B C2B 80.0(12) . . . . ? N2D Pd2 N1B C6B -173.0(10) . . . . ? N8B Pd2 N1B C6B 7.4(9) . . . . ? Pd1 Pd2 N1B C6B -92.8(9) . . . . ? N2D Pd2 N1C C6C -97.2(10) . . . . ? N8B Pd2 N1C C6C 82.6(10) . . . . ? Pd1 Pd2 N1C C6C -176.9(10) . . . . ? N2D Pd2 N1C C2C 84.8(10) . . . . ? N8B Pd2 N1C C2C -95.4(10) . . . . ? Pd1 Pd2 N1C C2C 5.1(9) . . . . ? N2C Pd1 N1D C2D 91.9(10) . . . . ? N8A Pd1 N1D C2D -87.2(10) . . . . ? Pd2 Pd1 N1D C2D 10.7(9) . . . . ? N2C Pd1 N1D C6D -94.4(9) . . . . ? N8A Pd1 N1D C6D 86.5(9) . . . . ? Pd2 Pd1 N1D C6D -175.5(9) . . . . ? N1D Pd1 N2C C2C -69.5(14) . . . . ? N1A Pd1 N2C C2C 108.5(14) . . . . ? Pd2 Pd1 N2C C2C 14.4(13) . . . . ? N1B Pd2 N2D C2D 107.0(11) . . . . ? N1C Pd2 N2D C2D -71.2(12) . . . . ? Pd1 Pd2 N2D C2D 10.6(10) . . . . ? N1D Pd1 N8A C9A -3.0(10) . . . . ? N1A Pd1 N8A C9A 179.0(10) . . . . ? Pd2 Pd1 N8A C9A -87.6(9) . . . . ? N1D Pd1 N8A C7A 173.0(8) . . . . ? N1A Pd1 N8A C7A -5.0(8) . . . . ? Pd2 Pd1 N8A C7A 88.5(8) . . . . ? N1B Pd2 N8B C7B -7.1(9) . . . . ? N1C Pd2 N8B C7B 171.1(10) . . . . ? Pd1 Pd2 N8B C7B 88.4(9) . . . . ? N1B Pd2 N8B C9B 176.3(11) . . . . ? N1C Pd2 N8B C9B -5.5(12) . . . . ? Pd1 Pd2 N8B C9B -88.2(10) . . . . ? C6A N1A C2A C3A 3(2) . . . . ? Pd1 N1A C2A C3A -174.9(11) . . . . ? C6B N1B C2B C3B -1(2) . . . . ? Pd2 N1B C2B C3B -173.8(11) . . . . ? Pd1 N2C C2C C3C 166.9(10) . . . . ? Pd1 N2C C2C N1C -14(2) . . . . ? C6C N1C C2C N2C -176.0(12) . . . . ? Pd2 N1C C2C N2C 2.0(17) . . . . ? C6C N1C C2C C3C 2.8(18) . . . . ? Pd2 N1C C2C C3C -179.2(8) . . . . ? C6D N1D C2D N2D 179.2(10) . . . . ? Pd1 N1D C2D N2D -7.2(16) . . . . ? C6D N1D C2D C3D -2.8(17) . . . . ? Pd1 N1D C2D C3D 170.8(8) . . . . ? Pd2 N2D C2D N1D -6.0(18) . . . . ? Pd2 N2D C2D C3D 176.1(8) . . . . ? N1A C2A C3A C4A 0(2) . . . . ? N1B C2B C3B C4B 0(2) . . . . ? N2C C2C C3C C4C 175.7(17) . . . . ? N1C C2C C3C C4C -3(2) . . . . ? N1D C2D C3D C4D 3.2(18) . . . . ? N2D C2D C3D C4D -178.9(12) . . . . ? C2A C3A C4A C5A -2(3) . . . . ? C2B C3B C4B C5B -2(2) . . . . ? C2C C3C C4C C5C 1(3) . . . . ? C2D C3D C4D C5D -2(2) . . . . ? C3A C4A C5A C6A 2(3) . . . . ? C3B C4B C5B C6B 5(2) . . . . ? C3C C4C C5C C6C 1(3) . . . . ? C3D C4D C5D C6D 0(2) . . . . ? C2A N1A C6A C5A -2.8(18) . . . . ? Pd1 N1A C6A C5A 175.0(10) . . . . ? C2A N1A C6A C7A -179.9(11) . . . . ? Pd1 N1A C6A C7A -2.1(13) . . . . ? C4A C5A C6A N1A 1(2) . . . . ? C4A C5A C6A C7A 177.8(13) . . . . ? C2B N1B C6B C5B 4(2) . . . . ? Pd2 N1B C6B C5B 177.6(10) . . . . ? C2B N1B C6B C7B -179.6(12) . . . . ? Pd2 N1B C6B C7B -6.3(15) . . . . ? C4B C5B C6B N1B -6(2) . . . . ? C4B C5B C6B C7B 178.2(13) . . . . ? C2C N1C C6C C5C -0.7(19) . . . . ? Pd2 N1C C6C C5C -178.8(10) . . . . ? C4C C5C C6C N1C -1(2) . . . . ? C2D N1D C6D C5D 1.4(19) . . . . ? Pd1 N1D C6D C5D -172.7(10) . . . . ? C4D C5D C6D N1D 0(2) . . . . ? C9A N8A C7A C12A 2.9(16) . . . . ? Pd1 N8A C7A C12A -173.5(9) . . . . ? C9A N8A C7A C6A -178.4(10) . . . . ? Pd1 N8A C7A C6A 5.3(12) . . . . ? N1A C6A C7A C12A 176.5(12) . . . . ? C5A C6A C7A C12A -1(2) . . . . ? N1A C6A C7A N8A -2.1(15) . . . . ? C5A C6A C7A N8A -179.2(11) . . . . ? C9B N8B C7B C12B -0.1(19) . . . . ? Pd2 N8B C7B C12B -177.0(10) . . . . ? C9B N8B C7B C6B -177.3(11) . . . . ? Pd2 N8B C7B C6B 5.8(14) . . . . ? N1B C6B C7B N8B 0.2(17) . . . . ? C5B C6B C7B N8B 176.4(12) . . . . ? N1B C6B C7B C12B -176.8(13) . . . . ? C5B C6B C7B C12B -1(2) . . . . ? C7A N8A C9A C10A -0.8(17) . . . . ? Pd1 N8A C9A C10A 175.1(9) . . . . ? C7B N8B C9B C10B 1(2) . . . . ? Pd2 N8B C9B C10B 176.9(10) . . . . ? N8A C9A C10A C11A 0(2) . . . . ? N8B C9B C10B C11B -5(2) . . . . ? C9A C10A C11A C12A -1(2) . . . . ? C9B C10B C11B C12B 8(2) . . . . ? N8A C7A C12A C11A -3.8(19) . . . . ? C6A C7A C12A C11A 177.6(13) . . . . ? C10A C11A C12A C7A 3(2) . . . . ? C10B C11B C12B C7B -8(2) . . . . ? N8B C7B C12B C11B 4(2) . . . . ? C6B C7B C12B C11B -179.3(14) . . . . ? # 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