# The Royal Society of Chemistry, 1998 data_General #==================================================================== _audit_creation_date '1998-01-21' _audit_creation_method 'by teXsan for Windows v1.0' #==================================================================== # SUBMISSION DETAILS _publ_requested_journal ' DALTON TRANSACTIONS' _publ_contact_author_name ' Jorma Arpalahti' _publ_contact_author_address ; Department of Chemistry, University of Turku, Fin-20014, Finland ; _publ_contact_author_phone ' -358-2-3336732 ' _publ_contact_author_fax ' -358-2-3336700 ' _publ_contact_author_email ' Jorma.Arpalahti@utu.fi ' #==================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #==================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Dynamic Processes in Pt(II)-Adenosine Complexes. Preparation, NMR Spectroscopic Characterisation and X-Ray Crystal Structure Determination of Isomeric Pt(II)(dien)Adenosine Complexes ; loop_ _publ_author_name _publ_author_address ' Jorma Arpalahti ' ; Department of Chemistry, University of Turku, Fin-20014, Finland ; ' Karel D. Klika ' ; Department of Chemistry, University of Turku, Fin-20014, Finland ; ' Reijo Sillanp\a\a ' ; Department of Chemistry, University of Turku, Fin-20014, Finland ; ' Raikko Kivek\as ' ; Department of Chemistry, University of Helsinki, Fin-00014, Finland ; #==================================================================== data_[Pt(dien)(Ado-N7)](ClO4) #==================================================================== _computing_data_collection ; Molecular Structure Corporation (1995), MSC/AFC Diffractomer Controll Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_cell_refinement ; Molecular Structure Corporation (1995), MSC/AFC Diffractomer Controll Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_data_reduction ; Molecular Structure Corporation (1989), TEXSAN. Single Crystal Structure Analysis Software. Version 5.0. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_structure_solution ; Molecular Structure Corporation (1989), TEXSAN. Single Crystal Structure Analysis Software. Version 5.0. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_structure_refinement ; Molecular Structure Corporation (1989), TEXSAN. Single Crystal Structure Analysis Software. Version 5.0. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_publication_material ; Molecular Structure Corporation (1997). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.01. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_molecular_graphics ; ORTEPII (Johnson, C.K (1976). Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA) ; #--------------------------------------------------------------------- _cell_length_a 13.520(6) _cell_length_b 14.23(1) _cell_length_c 12.914(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2484(4) _cell_formula_units_Z 4 _cell_measurement_temperature 294.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16.0 _cell_measurement_theta_max 19.2 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz #------------------------------------------------------------------------------ 'x, y, z' '1/2-x, -y, 1/2+z' '1/2+x, 1/2-y, -z' '-x, 1/2+y, 1/2-z' _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 782.42 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H28 Cl2 N8 O13 Pt ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1536.00 _exptl_absorpt_coefficient_mu 5.999 _exptl_absorpt_correction_type ; \y scans (North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.787 _exptl_special_details ; The scan width was (1.52+0.30tan\q)\% with an \w scan speed of 4\% per minute (up to 4 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #==================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S ' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.60 _diffrn_reflns_number 3230 _reflns_number_total 3230 _reflns_number_gt 2145 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.088 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05174 _diffrn_orient_matrix_UB_12 -0.02609 _diffrn_orient_matrix_UB_13 -0.04728 _diffrn_orient_matrix_UB_21 -0.02656 _diffrn_orient_matrix_UB_22 -0.06476 _diffrn_orient_matrix_UB_23 0.01152 _diffrn_orient_matrix_UB_31 -0.04570 _diffrn_orient_matrix_UB_32 0.00809 _diffrn_orient_matrix_UB_33 -0.06023 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 56 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 112 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 52 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 32 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pt 0 4 -2.352 8.388 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #==================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag Pt(1) Pt 0.06822(6) 0.37734(6) 0.02376(5) 0.0323(2) 1.000 Uani d Cl(1) Cl 0.8944(4) 0.1708(4) 0.2582(4) 0.041(2) 1.000 Uani d Cl(2) Cl 0.8269(5) 0.1997(7) 0.8543(5) 0.081(3) 1.000 Uani d O(1) O 0.875(1) 0.143(2) 0.158(1) 0.108(8) 1.000 Uani d O(2) O 0.849(1) 0.111(1) 0.329(1) 0.109(7) 1.000 Uani d O(2') O -0.062(1) 0.427(1) 0.6079(8) 0.064(5) 1.000 Uani d O(3) O 0.999(1) 0.181(1) 0.275(1) 0.085(6) 1.000 Uani d O(3') O -0.026(1) 0.239(1) 0.604(1) 0.104(7) 1.000 Uani d O(4) O 0.850(1) 0.261(1) 0.273(2) 0.110(8) 1.000 Uani d O(4') O 0.1132(8) 0.4047(8) 0.4514(9) 0.034(4) 1.000 Uani d O(5') O 0.742(2) 0.210(2) 0.805(2) 0.15(1) 1.000 Uani d O(5') O 0.202(1) 0.201(2) 0.567(2) 0.16(1) 1.000 Uani d O(6) O 0.830(2) 0.232(2) 0.948(1) 0.16(1) 1.000 Uani d O(7) O 0.870(3) 0.119(2) 0.855(3) 0.34(2) 1.000 Uani d O(8) O 0.890(2) 0.252(4) 0.801(3) 0.37(2) 1.000 Uani d O(9) O 0.066(2) 0.071(1) 0.674(1) 0.119(7) 1.000 Uiso d N(1) N -0.242(1) 0.530(1) 0.160(1) 0.040(5) 1.000 Uani d N(3) N -0.171(1) 0.518(1) 0.330(1) 0.049(6) 1.000 Uani d N(6) N -0.1743(9) 0.467(1) 0.015(1) 0.040(5) 1.000 Uani d N(7) N -0.001(1) 0.410(1) 0.160(1) 0.032(5) 1.000 Uani d N(9) N -0.013(1) 0.439(1) 0.329(1) 0.025(4) 1.000 Uani d N(10) N 0.050(1) 0.234(1) 0.038(1) 0.059(6) 1.000 Uani d N(11) N 0.145(1) 0.344(1) -0.101(1) 0.052(6) 1.000 Uani d N(12) N 0.088(1) 0.511(1) -0.019(1) 0.048(5) 1.000 Uani d C(1') C 0.016(1) 0.447(1) 0.439(1) 0.036(6) 1.000 Uani d C(2) C -0.240(1) 0.542(1) 0.263(2) 0.050(7) 1.000 Uani d C(2') C -0.046(1) 0.388(1) 0.507(1) 0.036(6) 1.000 Uani d C(3') C -0.001(2) 0.296(2) 0.521(2) 0.064(8) 1.000 Uani d C(4) C -0.091(1) 0.473(1) 0.283(1) 0.029(6) 1.000 Uani d C(4') C 0.113(1) 0.323(1) 0.518(2) 0.033(5) 1.000 Uani d C(5) C -0.089(1) 0.456(1) 0.177(1) 0.031(6) 1.000 Uani d C(5') C 0.194(3) 0.258(2) 0.478(2) 0.13(1) 1.000 Uani d C(6) C -0.166(2) 0.482(1) 0.117(1) 0.039(6) 1.000 Uani d C(8) C 0.042(1) 0.402(1) 0.248(1) 0.045(7) 1.000 Uani d C(10) C 0.110(2) 0.183(2) -0.050(2) 0.073(9) 1.000 Uani d C(11) C 0.120(2) 0.256(2) -0.140(2) 0.057(8) 1.000 Uani d C(12) C 0.140(2) 0.425(2) -0.173(2) 0.054(8) 1.000 Uani d C(13) C 0.163(2) 0.512(2) -0.109(2) 0.056(8) 1.000 Uani d H(1') H 0.0164 0.5110 0.4614 0.043 1.000 Uiso c H(2) H -0.2955 0.5733 0.2912 0.059 1.000 Uiso c H(2') H -0.1086 0.3803 0.4749 0.043 1.000 Uiso c H(3') H -0.0141 0.2609 0.4595 0.077 1.000 Uiso c H(4') H 0.1314 0.3433 0.5858 0.040 1.000 Uiso c H(5') H 0.2536 0.2907 0.4629 0.157 1.000 Uiso c H(6A) H -0.1245 0.4350 -0.0212 0.048 1.000 Uiso c H(6B) H -0.2300 0.4888 -0.0214 0.048 1.000 Uiso c H(5'') H 0.1735 0.2239 0.4184 0.157 1.000 Uiso c H(8) H 0.1052 0.3735 0.2574 0.054 1.000 Uiso c H(10A) H 0.0738 0.2141 0.1039 0.071 1.000 Uiso c H(10B) H -0.0183 0.2188 0.0323 0.071 1.000 Uiso c H(11) H 0.2121 0.3394 -0.0798 0.063 1.000 Uiso c H(12A) H 0.0269 0.5369 -0.0414 0.057 1.000 Uiso c H(12B) H 0.1131 0.5462 0.0372 0.057 1.000 Uiso c H(101) H 0.1732 0.1651 -0.0255 0.088 1.000 Uiso c H(102) H 0.0749 0.1289 -0.0730 0.088 1.000 Uiso c H(111) H 0.1696 0.2359 -0.1870 0.069 1.000 Uiso c H(112) H 0.0584 0.2608 -0.1760 0.069 1.000 Uiso c H(121) H 0.1877 0.4179 -0.2270 0.065 1.000 Uiso c H(122) H 0.0759 0.4294 -0.2030 0.065 1.000 Uiso c H(131) H 0.2283 0.5091 -0.0831 0.068 1.000 Uiso c H(132) H 0.1545 0.5669 -0.1495 0.068 1.000 Uiso c loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0303(3) 0.0424(4) 0.0241(3) -0.0038(5) 0.0058(4) -0.0071(5) Cl(1) 0.038(3) 0.047(3) 0.039(3) -0.003(3) -0.002(2) 0.004(3) Cl(2) 0.059(5) 0.137(8) 0.046(4) 0.003(5) 0.006(4) -0.006(5) O(1) 0.07(1) 0.20(2) 0.05(1) -0.03(2) -0.005(8) -0.01(1) O(2) 0.10(1) 0.12(2) 0.10(1) -0.02(2) -0.01(1) 0.06(2) O(2') 0.037(8) 0.13(1) 0.022(6) 0.02(1) 0.000(8) -0.020(8) O(3) 0.024(8) 0.11(2) 0.12(1) 0.01(1) -0.028(9) -0.02(1) O(3') 0.05(1) 0.14(2) 0.11(1) 0.00(1) 0.02(1) 0.10(1) O(4) 0.06(1) 0.05(1) 0.22(2) 0.02(1) 0.00(2) -0.03(1) O(4') 0.027(6) 0.040(9) 0.034(8) -0.011(6) -0.009(6) 0.011(6) O(5) 0.08(2) 0.21(3) 0.16(2) -0.05(2) -0.06(2) 0.00(2) O(5') 0.06(1) 0.16(2) 0.25(3) -0.01(2) 0.06(2) -0.02(2) O(6) 0.14(2) 0.28(3) 0.07(2) 0.05(2) -0.03(2) -0.08(2) O(7) 0.58(8) 0.11(2) 0.33(4) 0.19(4) -0.27(4) -0.12(3) O(8) 0.11(3) 0.71(9) 0.29(4) 0.10(4) 0.06(2) 0.31(5) N(1) 0.024(9) 0.08(1) 0.010(7) 0.01(1) -0.007(7) 0.000(8) N(3) 0.04(1) 0.08(2) 0.022(9) 0.01(1) -0.003(8) 0.01(1) N(6) 0.005(7) 0.09(1) 0.029(9) 0.011(8) -0.008(7) -0.03(1) N(7) 0.023(8) 0.05(1) 0.024(8) 0.011(8) -0.003(7) -0.004(7) N(9) 0.010(7) 0.05(1) 0.020(8) 0.007(7) -0.005(6) 0.004(7) N(10) 0.06(1) 0.06(1) 0.06(1) -0.02(1) 0.03(1) 0.02(1) N(11) 0.05(1) 0.06(1) 0.04(1) -0.01(1) 0.007(9) -0.02(1) N(12) 0.04(1) 0.06(1) 0.040(9) -0.001(9) -0.02(1) -0.01(1) C(1') 0.03(1) 0.05(1) 0.03(1) 0.01(1) -0.006(9) -0.00(1) C(2) 0.03(1) 0.07(2) 0.06(1) 0.03(1) 0.00(1) 0.02(1) C(2') 0.06(1) 0.03(1) 0.02(1) 0.01(1) -0.022(8) 0.000(9) C(3') 0.08(2) 0.05(2) 0.06(1) -0.01(1) -0.00(2) 0.02(2) C(4) 0.03(1) 0.03(1) 0.03(1) 0.003(9) 0.005(9) -0.001(8) C(4') 0.04(1) 0.04(1) 0.025(9) -0.014(9) -0.02(1) 0.03(1) C(5) 0.03(1) 0.05(1) 0.016(8) -0.00(1) 0.011(8) 0.004(8) C(5') 0.27(4) 0.07(2) 0.05(2) 0.12(2) 0.01(3) 0.03(2) C(6) 0.05(1) 0.05(1) 0.02(1) 0.00(1) -0.00(1) -0.01(1) C(8) 0.02(1) 0.07(2) 0.04(1) 0.01(1) -0.000(9) -0.00(1) C(10) 0.05(1) 0.08(2) 0.09(2) 0.01(1) 0.03(1) 0.01(2) C(11) 0.05(2) 0.06(2) 0.06(2) 0.00(1) 0.02(1) -0.03(1) C(12) 0.04(1) 0.08(2) 0.05(1) -0.01(1) -0.00(1) -0.00(1) C(13) 0.03(1) 0.07(2) 0.07(2) -0.03(1) 0.01(1) 0.02(1) #==================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2145 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0395 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.960 _refine_ls_shift/su_max 0.0537 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.98 _refine_diff_density_max 1.00 #==================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) N(7) 2.05(1) . . ? Pt(1) N(10) 2.06(2) . . ? Pt(1) N(11) 1.98(2) . . ? Pt(1) N(12) 2.00(1) . . ? Cl(1) O(1) 1.37(2) . . ? Cl(1) O(2) 1.39(2) . . ? Cl(1) O(3) 1.44(2) . . ? Cl(1) O(4) 1.43(2) . . ? Cl(2) O(5) 1.33(2) . . ? Cl(2) O(6) 1.30(2) . . ? Cl(2) O(7) 1.29(3) . . ? Cl(2) O(8) 1.32(4) . . ? O(2') C(2') 1.42(2) . . ? O(3') C(3') 1.38(3) . . ? O(4') C(1') 1.45(2) . . ? O(4') C(4') 1.44(2) . . ? O(5') C(5') 1.41(4) . . ? N(1) C(2) 1.33(3) . . ? N(1) C(6) 1.35(3) . . ? N(3) C(2) 1.32(3) . . ? N(3) C(4) 1.40(2) . . ? N(6) C(6) 1.34(2) . . ? N(6) H(6A) 0.94 . . no N(6) H(6B) 0.94 . . no N(7) C(5) 1.36(2) . . ? N(7) C(8) 1.29(2) . . ? N(9) C(1') 1.49(2) . . ? N(9) C(4) 1.31(2) . . ? N(9) C(8) 1.38(2) . . ? N(10) C(10) 1.57(3) . . ? N(10) H(10A) 0.95 . . no N(10) H(10B) 0.95 . . no N(11) C(11) 1.39(3) . . ? N(11) C(12) 1.48(3) . . ? N(11) H(11) 0.95 . . no N(12) C(13) 1.53(3) . . ? N(12) H(12A) 0.95 . . no N(12) H(12B) 0.95 . . no C(1') C(2') 1.48(3) . . ? C(1') H(1') 0.95 . . no C(2) H(2) 0.95 . . no C(2') C(3') 1.47(3) . . ? C(2') H(2') 0.95 . . no C(3') C(4') 1.59(3) . . ? C(3') H(3') 0.95 . . no C(4) C(5) 1.39(2) . . ? C(4') C(5') 1.52(4) . . ? C(4') H(4') 0.95 . . no C(5) C(6) 1.36(3) . . ? C(5') H(5') 0.95 . . no C(5') H(5'') 0.95 . . no C(8) H(8) 0.95 . . no C(10) C(11) 1.57(3) . . ? C(10) H(101) 0.95 . . no C(10) H(102) 0.95 . . no C(11) H(111) 0.95 . . no C(11) H(112) 0.95 . . no C(12) C(13) 1.52(3) . . ? C(12) H(121) 0.95 . . no C(12) H(122) 0.95 . . no C(13) H(131) 0.95 . . no C(13) H(132) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(7) Pt(1) N(10) 95.4(6) . . . ? N(7) Pt(1) N(11) 175.3(6) . . . ? N(7) Pt(1) N(12) 94.7(6) . . . ? N(10) Pt(1) N(11) 84.2(7) . . . ? N(10) Pt(1) N(12) 169.0(7) . . . ? N(11) Pt(1) N(12) 86.0(7) . . . ? O(1) Cl(1) O(2) 111(1) . . . ? O(1) Cl(1) O(3) 111(1) . . . ? O(1) Cl(1) O(4) 108(1) . . . ? O(2) Cl(1) O(3) 113(1) . . . ? O(2) Cl(1) O(4) 106(1) . . . ? O(3) Cl(1) O(4) 107(1) . . . ? O(5) Cl(2) O(6) 116(2) . . . ? O(5) Cl(2) O(7) 120(2) . . . ? O(5) Cl(2) O(8) 104(2) . . . ? O(6) Cl(2) O(7) 107(2) . . . ? O(6) Cl(2) O(8) 105(2) . . . ? O(7) Cl(2) O(8) 103(3) . . . ? C(1') O(4') C(4') 113(1) . . . ? C(2) N(1) C(6) 117(2) . . . ? C(2) N(3) C(4) 112(2) . . . ? C(6) N(6) H(6A) 120.4 . . . no C(6) N(6) H(6B) 120.4 . . . no H(6A) N(6) H(6B) 119.1 . . . no Pt(1) N(7) C(5) 130(1) . . . ? Pt(1) N(7) C(8) 122(1) . . . ? C(5) N(7) C(8) 107(1) . . . ? C(1') N(9) C(4) 128(2) . . . ? C(1') N(9) C(8) 128(1) . . . ? C(4) N(9) C(8) 103(1) . . . ? Pt(1) N(10) C(10) 109(1) . . . ? Pt(1) N(10) H(10A) 109.6 . . . no Pt(1) N(10) H(10B) 109.5 . . . no C(10) N(10) H(10A) 109.5 . . . no C(10) N(10) H(10B) 109.5 . . . no H(10A) N(10) H(10B) 109.5 . . . no Pt(1) N(11) C(11) 113(1) . . . ? Pt(1) N(11) C(12) 108(1) . . . ? Pt(1) N(11) H(11) 106.2 . . . no C(11) N(11) C(12) 117(2) . . . ? C(11) N(11) H(11) 106.2 . . . no C(12) N(11) H(11) 106.2 . . . no Pt(1) N(12) C(13) 108(1) . . . ? Pt(1) N(12) H(12A) 109.8 . . . no Pt(1) N(12) H(12B) 109.9 . . . no C(13) N(12) H(12A) 109.9 . . . no C(13) N(12) H(12B) 109.9 . . . no H(12A) N(12) H(12B) 109.4 . . . no O(4') C(1') N(9) 108(1) . . . ? O(4') C(1') C(2') 102(2) . . . ? O(4') C(1') H(1') 111.4 . . . no N(9) C(1') C(2') 112(2) . . . ? N(9) C(1') H(1') 111.4 . . . no C(2') C(1') H(1') 111.4 . . . no N(1) C(2) N(3) 130(2) . . . ? N(1) C(2) H(2) 115.1 . . . no N(3) C(2) H(2) 115.1 . . . no O(2') C(2') C(1') 114(2) . . . ? O(2') C(2') C(3') 108(2) . . . ? O(2') C(2') H(2') 108.3 . . . no C(1') C(2') C(3') 110(2) . . . ? C(1') C(2') H(2') 108.3 . . . no C(3') C(2') H(2') 108.2 . . . no O(3') C(3') C(2') 121(2) . . . ? O(3') C(3') C(4') 113(2) . . . ? O(3') C(3') H(3') 107.1 . . . no C(2') C(3') C(4') 100(2) . . . ? C(2') C(3') H(3') 107.1 . . . no C(4') C(3') H(3') 107.1 . . . no N(3) C(4) N(9) 126(2) . . . ? N(3) C(4) C(5) 122(2) . . . ? N(9) C(4) C(5) 111(2) . . . ? O(4') C(4') C(3') 102(1) . . . ? O(4') C(4') C(5') 106(2) . . . ? O(4') C(4') H(4') 108.0 . . . no C(3') C(4') C(5') 123(2) . . . ? C(3') C(4') H(4') 108.0 . . . no C(5') C(4') H(4') 107.9 . . . no N(7) C(5) C(4) 105(1) . . . ? N(7) C(5) C(6) 135(2) . . . ? C(4) C(5) C(6) 120(2) . . . ? O(5') C(5') C(4') 97(2) . . . ? O(5') C(5') H(5') 112.5 . . . no O(5') C(5') H(5'') 112.5 . . . no C(4') C(5') H(5') 112.4 . . . no C(4') C(5') H(5'') 112.5 . . . no H(5') C(5') H(5'') 109.4 . . . no N(1) C(6) N(6) 115(2) . . . ? N(1) C(6) C(5) 120(2) . . . ? N(6) C(6) C(5) 126(2) . . . ? N(7) C(8) N(9) 113(2) . . . ? N(7) C(8) H(8) 123.6 . . . no N(9) C(8) H(8) 123.6 . . . no N(10) C(10) C(11) 106(2) . . . ? N(10) C(10) H(101) 110.3 . . . no N(10) C(10) H(102) 110.3 . . . no C(11) C(10) H(101) 110.3 . . . no C(11) C(10) H(102) 110.3 . . . no H(101) C(10) H(102) 109.5 . . . no N(11) C(11) C(10) 110(2) . . . ? N(11) C(11) H(111) 109.3 . . . no N(11) C(11) H(112) 109.3 . . . no C(10) C(11) H(111) 109.3 . . . no C(10) C(11) H(112) 109.3 . . . no H(111) C(11) H(112) 109.5 . . . no N(11) C(12) C(13) 106(2) . . . ? N(11) C(12) H(121) 110.3 . . . no N(11) C(12) H(122) 110.3 . . . no C(13) C(12) H(121) 110.3 . . . no C(13) C(12) H(122) 110.3 . . . no H(121) C(12) H(122) 109.5 . . . no N(12) C(13) C(12) 106(2) . . . ? N(12) C(13) H(131) 110.3 . . . no N(12) C(13) H(132) 110.4 . . . no C(12) C(13) H(131) 110.3 . . . no C(12) C(13) H(132) 110.3 . . . no H(131) C(13) H(132) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt(1) O(5) 3.45(2) . 3_456 no O(1) O(6) 3.06(3) . 1_554 no O(1) N(10) 3.11(2) . 1_655 no O(1) N(11) 3.20(2) . 3 no O(1) C(12) 3.32(3) . 3 no O(1) C(1') 3.39(3) . 4_645 no O(1) N(9) 3.45(3) . 4_645 no O(2) N(12) 2.96(2) . 4_645 no O(2) C(8) 3.47(3) . 4_645 no O(2) C(12) 3.51(3) . 3 no O(2) N(7) 3.52(2) . 4_645 no O(2) O(5') 3.59(3) . 3_556 no O(2') N(1) 2.80(2) . 2_465 no O(2') C(2) 3.37(2) . 2_465 no O(2') O(9) 3.47(2) . 4_556 no O(2') O(8) 3.58(5) . 1_455 no O(3) C(8) 3.21(3) . 1_655 no O(3) N(10) 3.22(2) . 1_655 no O(3) C(4) 3.30(2) . 4_645 no O(3) C(5) 3.49(3) . 4_645 no O(3) N(3) 3.56(2) . 4_645 no O(3) C(3') 3.57(3) . 1_655 no O(3) N(7) 3.58(2) . 1_655 no O(3') O(8) 2.80(4) . 1_455 no O(3') O(9) 2.85(3) . . no O(3') N(12) 3.53(2) . 4_545 no O(4) O(5') 2.93(3) . 3_556 no O(4) C(4) 3.13(2) . 1_655 no O(4) C(5) 3.15(3) . 1_655 no O(4) N(9) 3.22(2) . 1_655 no O(4) N(7) 3.28(2) . 1_655 no O(4) C(8) 3.30(3) . 1_655 no O(4) C(11) 3.56(3) . 3 no O(4') C(13) 3.35(2) . 2_565 no O(5) C(8) 3.21(3) . 3_556 no O(5) N(10) 3.38(3) . 3_556 no O(5) C(2) 3.57(3) . 2_565 no O(5') O(9) 2.96(3) . . no O(5') N(6) 3.51(3) . 4_545 no O(6) N(10) 3.19(3) . 1_656 no O(6) N(11) 3.37(3) . 3_556 no O(6) N(6) 3.46(3) . 1_656 no O(6) C(10) 3.48(3) . 3_556 no O(7) C(13) 3.55(4) . 4_645 no O(7) C(10) 3.59(5) . 1_656 no O(7) O(9) 3.60(5) . 1_655 no O(8) C(11) 3.20(4) . 1_656 no O(8) C(2) 3.60(5) . 2_565 no O(9) N(12) 3.01(3) . 4_545 no O(9) C(2) 3.18(3) . 3_556 no O(9) N(6) 3.21(2) . 4_545 no O(9) C(13) 3.31(3) . 4_545 no O(9) C(12) 3.47(3) . 4_545 no N(3) N(6) 3.18(2) . 2_465 no N(6) C(2) 3.46(3) . 2_464 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pt(1) N(7) C(5) C(4) . . . . -170(1) no Pt(1) N(7) C(5) C(6) . . . . 11(3) no Pt(1) N(7) C(8) N(9) . . . . 172(1) no Pt(1) N(10) C(10) C(11) . . . . -25(2) no Pt(1) N(11) C(11) C(10) . . . . -44(2) no Pt(1) N(11) C(12) C(13) . . . . 47(2) no Pt(1) N(12) C(13) C(12) . . . . 37(2) no O(2') C(2') C(1') O(4') . . . . 97(2) no O(2') C(2') C(1') N(9) . . . . -147(2) no O(2') C(2') C(3') O(3') . . . . 34(3) no O(2') C(2') C(3') C(4') . . . . -91(2) no O(3') C(3') C(2') C(1') . . . . 159(2) no O(3') C(3') C(4') O(4') . . . . -161(2) no O(3') C(3') C(4') C(5') . . . . 80(3) no O(4') C(1') N(9) C(4) . . . . -175(2) no O(4') C(1') N(9) C(8) . . . . -3(2) no O(4') C(1') C(2') C(3') . . . . -24(2) no O(4') C(4') C(3') C(2') . . . . -30(2) no O(4') C(4') C(5') O(5') . . . . 164(2) no O(5') C(5') C(4') C(3') . . . . -79(3) no N(1) C(2) N(3) C(4) . . . . 0(3) no N(1) C(6) C(5) N(7) . . . . -178(2) no N(1) C(6) C(5) C(4) . . . . 3(3) no N(3) C(2) N(1) C(6) . . . . 3(3) no N(3) C(4) N(9) C(1') . . . . -7(3) no N(3) C(4) N(9) C(8) . . . . 179(2) no N(3) C(4) C(5) N(7) . . . . -179(2) no N(3) C(4) C(5) C(6) . . . . -0(3) no N(6) C(6) N(1) C(2) . . . . 177(2) no N(6) C(6) C(5) N(7) . . . . 1(4) no N(6) C(6) C(5) C(4) . . . . -178(2) no N(7) Pt(1) N(10) C(10) . . . . -172(1) no N(7) Pt(1) N(11) C(11) . . . . 109(8) no N(7) Pt(1) N(11) C(12) . . . . -120(8) no N(7) Pt(1) N(12) C(13) . . . . 166(1) no N(7) C(5) C(4) N(9) . . . . -2(2) no N(7) C(8) N(9) C(1') . . . . -176(2) no N(7) C(8) N(9) C(4) . . . . -2(2) no N(9) C(1') O(4') C(4') . . . . -116(2) no N(9) C(1') C(2') C(3') . . . . 91(2) no N(9) C(4) N(3) C(2) . . . . -178(2) no N(9) C(4) C(5) C(6) . . . . 177(2) no N(9) C(8) N(7) C(5) . . . . 1(2) no N(10) Pt(1) N(7) C(5) . . . . -112(2) no N(10) Pt(1) N(7) C(8) . . . . 79(2) no N(10) Pt(1) N(11) C(11) . . . . 23(2) no N(10) Pt(1) N(11) C(12) . . . . 154(1) no N(10) Pt(1) N(12) C(13) . . . . -37(4) no N(10) C(10) C(11) N(11) . . . . 44(2) no N(11) Pt(1) N(7) C(5) . . . . 163(7) no N(11) Pt(1) N(7) C(8) . . . . -7(9) no N(11) Pt(1) N(10) C(10) . . . . 3(1) no N(11) Pt(1) N(12) C(13) . . . . -9(1) no N(11) C(12) C(13) N(12) . . . . -55(2) no N(12) Pt(1) N(7) C(5) . . . . 64(2) no N(12) Pt(1) N(7) C(8) . . . . -106(2) no N(12) Pt(1) N(10) C(10) . . . . 31(4) no N(12) Pt(1) N(11) C(11) . . . . -152(2) no N(12) Pt(1) N(11) C(12) . . . . -21(1) no C(1') O(4') C(4') C(3') . . . . 18(2) no C(1') O(4') C(4') C(5') . . . . 149(2) no C(1') N(9) C(4) C(5) . . . . 176(2) no C(1') C(2') C(3') C(4') . . . . 34(2) no C(2) N(1) C(6) C(5) . . . . -4(3) no C(2) N(3) C(4) C(5) . . . . -1(3) no C(2') C(1') O(4') C(4') . . . . 2(2) no C(2') C(1') N(9) C(4) . . . . 73(2) no C(2') C(1') N(9) C(8) . . . . -115(2) no C(2') C(3') C(4') C(5') . . . . -150(2) no C(4) C(5) N(7) C(8) . . . . 1(2) no C(5) C(4) N(9) C(8) . . . . 2(2) no C(6) C(5) N(7) C(8) . . . . -178(2) no C(10) C(11) N(11) C(12) . . . . -169(2) no C(11) N(11) C(12) C(13) . . . . 175(2) no #------------------------------------------------------------------------------ #==================================================================== data_[Pt(dien)(Ado-N1)](ClO4) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; 2(C14 H31 N8 O4 Pt), 4(Cl O4), 5.54(H2 O) ; _chemical_formula_structural 'C14 H31.54 Cl2 N8 O14.77 Pt' _chemical_formula_analytical ? _chemical_formula_sum 'C14 H31.54 Cl2 N8 O14.77 Pt' _chemical_formula_weight 814.32 _chemical_melting_point 'not measured' _chemical_compound_source 'synthesis' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 12.167(4) _cell_length_b 14.644(2) _cell_length_c 8.746(2) _cell_angle_alpha 105.170(10) _cell_angle_beta 108.40(2) _cell_angle_gamma 70.95(2) _cell_volume 1375.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.03 _cell_measurement_theta_max 20.06 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method ? _exptl_crystal_F_000 803 _exptl_absorpt_coefficient_mu 5.376 _exptl_absorpt_correction_type ; empirical via \y scans (North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968).Acta Cryst. A24, 351-359.) ; _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method 'w\--2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 6631 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6627 _reflns_number_observed 5422 _reflns_observed_criterion >2sigma(I) _computing_data_collection ; Molecular Structure Corporation (1995), MSC/AFC Diffractomer Controll Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_cell_refinement ; Molecular Structure Corporation (1995), MSC/AFC Diffractomer Controll Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_data_reduction ; Molecular Structure Corporation (1989), TEXSAN. Single Crystal Structure Analysis Software. Version 5.0. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_structure_solution ; SHELXS-86 (Sheldrick, G. M. (1985). Program for the Solution of Crystal Structures. University of G\"ottingen, Germany. ; _computing_structure_refinement ; SHELXL-92 (Sheldrick, G. M. (1993). Program for the Crystal Structure Refinement. University of G\"ottingen, Germany. ; _computing_molecular_graphics ; ORTEPII (Johnson, C.K (1976). Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA) ; _computing_publication_material ; SHELXL-92 (Sheldrick, G. M. (1993). Program for the Crystal Structure Refinement. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+3.8370P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.008(12) _refine_ls_number_reflns 6626 _refine_ls_number_parameters 360 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_obs 0.0438 _refine_ls_wR_factor_all 0.1160 _refine_ls_wR_factor_obs 0.1057 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 1.052 _refine_ls_restrained_S_obs 1.068 _refine_ls_shift/esd_max -0.028 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.3105 0.6655 0.0662 0.03309(8) Uani 1 d . . O2'A O 0.2505(8) 0.1294(7) 0.0662(12) 0.110(3) Uiso 1 d D . O3'A O 0.4815(17) 0.0016(10) 0.1308(22) 0.244(9) Uiso 1 d D . O4'A O 0.3484(6) 0.1836(5) 0.4311(8) 0.062(2) Uiso 1 d D . O5'A O 0.4635(19) 0.0669(19) 0.6586(21) 0.319(13) Uiso 1 d D . C1'A C 0.3142(7) 0.2399(5) 0.3107(9) 0.042(2) Uiso 1 d D . H1'A H 0.2270(7) 0.2689(5) 0.2839(9) 0.050 Uiso 1 calc R . C2'A C 0.3531(8) 0.1636(6) 0.1609(12) 0.069(3) Uiso 1 d D . H2'A H 0.3777(8) 0.1950(6) 0.0956(12) 0.083 Uiso 1 calc R . C3'A C 0.4637(9) 0.0899(8) 0.2507(11) 0.092(4) Uiso 1 d D . H3'A H 0.5350(9) 0.1150(8) 0.2936(11) 0.110 Uiso 1 calc R . C4'A C 0.4131(9) 0.0871(7) 0.3833(11) 0.072(3) Uiso 1 d D . H4'A H 0.3542(9) 0.0486(7) 0.3327(11) 0.087 Uiso 1 calc R . C5'A C 0.5097(18) 0.0329(17) 0.5165(19) 0.216(12) Uiso 1 d D . H5'1 H 0.5224(18) -0.0376(17) 0.4829(19) 0.260 Uiso 1 calc R . H5'2 H 0.5854(18) 0.0486(17) 0.5379(19) 0.260 Uiso 1 calc R . N1A N 0.3383(5) 0.5503(4) 0.1757(7) 0.0350(14) Uiso 1 d D . N3A N 0.2633(5) 0.4112(4) 0.1453(7) 0.0321(13) Uiso 1 d D . N6A N 0.5091(5) 0.5816(4) 0.3807(7) 0.0323(13) Uiso 1 d D . H6A1 H 0.5183(5) 0.6169(4) 0.3232(7) 0.039 Uiso 1 calc R . H6A2 H 0.5584(5) 0.5735(4) 0.4744(7) 0.039 Uiso 1 calc R . N7A N 0.5115(5) 0.4054(4) 0.5065(7) 0.0307(13) Uiso 1 d D . N9A N 0.3781(5) 0.3167(4) 0.3637(7) 0.0300(13) Uiso 1 d D . N10A N 0.4032(6) 0.5776(5) -0.1036(8) 0.041(2) Uiso 1 d . . H10A H 0.4801(6) 0.5514(5) -0.0536(8) 0.049 Uiso 1 calc R . H10B H 0.3695(6) 0.5284(5) -0.1604(8) 0.049 Uiso 1 calc R . N11A N 0.2947(6) 0.7734(5) -0.0536(9) 0.049(2) Uiso 1 d D . H11A H 0.2267(6) 0.7716(5) -0.1355(9) 0.059 Uiso 1 calc R . N12A N 0.2306(6) 0.7789(5) 0.2300(8) 0.044(2) Uiso 1 d . . H12A H 0.1729(6) 0.7625(5) 0.2522(8) 0.053 Uiso 1 calc R . H12B H 0.2859(6) 0.7899(5) 0.3243(8) 0.053 Uiso 1 calc R . C2A C 0.2641(6) 0.4888(5) 0.1032(8) 0.037(2) Uiso 1 d D . H2A H 0.2056(6) 0.5060(5) 0.0094(8) 0.045 Uiso 1 calc R . C4A C 0.3498(7) 0.3941(5) 0.2869(9) 0.035(2) Uiso 1 d D . C5A C 0.4257(6) 0.4557(5) 0.3828(8) 0.0274(14) Uiso 1 d D . C6A C 0.4142(6) 0.5373(5) 0.3215(9) 0.032(2) Uiso 1 d D . C8A C 0.4739(6) 0.3301(5) 0.4962(8) 0.032(2) Uiso 1 d D . H8A H 0.5088(6) 0.2882(5) 0.5723(8) 0.039 Uiso 1 calc R . C10A C 0.3965(10) 0.6438(7) -0.2187(13) 0.065(3) Uiso 1 d . . H10A H 0.4692(10) 0.6204(7) -0.2571(13) 0.078 Uiso 1 calc R . H10B H 0.3290(10) 0.6395(7) -0.3133(13) 0.078 Uiso 1 calc R . C11A C 0.3829(8) 0.7463(7) -0.1378(12) 0.061(3) Uiso 1 d D . H11A H 0.4585(8) 0.7542(7) -0.0623(12) 0.074 Uiso 1 calc R . H11B H 0.3606(8) 0.7879(7) -0.2186(12) 0.074 Uiso 1 calc R . C12A C 0.2572(9) 0.8670(7) 0.0557(12) 0.068(3) Uiso 1 d D . H12A H 0.2167(9) 0.9179(7) -0.0106(12) 0.082 Uiso 1 calc R . H12B H 0.3290(9) 0.8836(7) 0.1299(12) 0.082 Uiso 1 calc R . C13A C 0.1775(7) 0.8693(6) 0.1545(10) 0.049(2) Uiso 1 d D . H13A H 0.0972(7) 0.8700(6) 0.0856(10) 0.059 Uiso 1 calc R . H13B H 0.1725(7) 0.9275(6) 0.2389(10) 0.059 Uiso 1 calc R . Pt2 Pt 0.88532(3) 0.33662(2) 1.13232(4) 0.03418(9) Uani 1 d . . O2'B O 1.0289(6) 0.8034(5) 0.7401(8) 0.063(2) Uiso 1 d D . O3'B O 0.8304(6) 0.9447(5) 0.6502(8) 0.060(2) Uiso 1 d D . O4'B O 0.8866(5) 0.8140(4) 0.9644(7) 0.0485(14) Uiso 1 d D . O5'B O 0.6294(16) 0.8946(13) 0.8734(30) 0.145(9) Uiso 0.50 d PD . O5'C O 0.7454(22) 0.9861(18) 1.1147(19) 0.132(9) Uiso 0.50 d PD . C1'B C 0.9265(7) 0.7345(5) 0.8467(9) 0.041(2) Uiso 1 d D . H1'B H 1.0108(7) 0.7018(5) 0.8918(9) 0.049 Uiso 1 calc R . C2'B C 0.9177(6) 0.7766(5) 0.7019(9) 0.045(2) Uiso 1 d D . H2'B H 0.9032(6) 0.7315(5) 0.5974(9) 0.054 Uiso 1 calc R . C3'B C 0.8159(7) 0.8718(6) 0.7110(9) 0.049(2) Uiso 1 d D . H3'B H 0.7386(7) 0.8577(6) 0.6511(9) 0.058 Uiso 1 calc R . C4'B C 0.8212(8) 0.9034(7) 0.8949(11) 0.061(3) Uiso 1 d D . H4'B H 0.8743(8) 0.9472(7) 0.9387(11) 0.073 Uiso 1 calc R . C5'B C 0.7014(12) 0.9627(13) 0.9365(18) 0.169(9) Uiso 1 d D . H5'B H 0.6652(12) 1.0218(13) 0.8867(18) 0.202 Uiso 1 calc R . N1B N 0.8762(5) 0.4431(4) 1.0128(7) 0.0271(13) Uiso 1 d D . N3B N 0.9626(5) 0.5710(4) 1.0260(7) 0.0295(13) Uiso 1 d D . N6B N 0.7162(6) 0.4068(5) 0.8029(8) 0.037(2) Uiso 1 d D . H6B1 H 0.6741(6) 0.4089(5) 0.7037(8) 0.044 Uiso 1 calc R . H6B2 H 0.7188(6) 0.3617(5) 0.8512(8) 0.044 Uiso 1 calc R . N7B N 0.7137(6) 0.5846(4) 0.6747(8) 0.0350(15) Uiso 1 d D . N9B N 0.8534(5) 0.6627(4) 0.8038(7) 0.0340(14) Uiso 1 d D . N10B N 0.9526(7) 0.2244(5) 0.9671(10) 0.053(2) Uiso 1 d D . H10C H 0.8998(7) 0.2251(5) 0.8683(10) 0.064 Uiso 1 calc R . H10D H 1.0213(7) 0.2311(5) 0.9584(10) 0.064 Uiso 1 calc R . N11B N 0.9184(6) 0.2305(5) 1.2594(8) 0.049(2) Uiso 1 d D . N12B N 0.8224(7) 0.4292(6) 1.3244(9) 0.048(2) Uiso 1 d . . H12C H 0.8688(7) 0.4708(6) 1.3742(9) 0.057 Uiso 1 calc R . H12D H 0.7472(7) 0.4650(6) 1.2861(9) 0.057 Uiso 1 calc R . C2B C 0.9575(6) 0.4961(5) 1.0785(8) 0.033(2) Uiso 1 d D . H2B H 1.0165(6) 0.4778(5) 1.1711(8) 0.039 Uiso 1 calc R . C4B C 0.8712(6) 0.5944(5) 0.8927(8) 0.0259(14) Uiso 1 d D . C5B C 0.7812(7) 0.5507(6) 0.8186(10) 0.035(2) Uiso 1 d D . C6B C 0.7754(7) 0.4713(5) 0.8794(9) 0.028(2) Uiso 1 d D . C8B C 0.7554(7) 0.6571(6) 0.6776(10) 0.040(2) Uiso 1 d D . H8B H 0.7219(7) 0.6994(6) 0.6022(10) 0.048 Uiso 1 calc R . C10B C 0.9766(8) 0.1291(6) 1.0212(9) 0.053(2) Uiso 1 d D . C11B C 1.0074(15) 0.1414(12) 1.2065(14) 0.055(6) Uiso 0.40 d PD . C11C C 0.9160(11) 0.1397(9) 1.1506(14) 0.044(3) Uiso 0.60 d PD . C12B C 0.9166(16) 0.2775(11) 1.4295(19) 0.056(6) Uiso 0.40 d PD . C12C C 0.8361(13) 0.2672(9) 1.3736(18) 0.059(4) Uiso 0.60 d PD . C13B C 0.8220(9) 0.3758(6) 1.4438(13) 0.056(3) Uiso 1 d D . Cl1 Cl 0.5462(2) 0.2944(2) 0.9819(4) 0.0887(9) Uani 1 d D . O1 O 0.5571(12) 0.3894(6) 1.0552(16) 0.200(7) Uiso 1 d D . O2 O 0.4353(8) 0.2968(10) 0.8843(15) 0.206(7) Uiso 1 d D . O3 O 0.5742(11) 0.2447(7) 1.1088(11) 0.157(5) Uiso 1 d D . O4 O 0.6387(6) 0.2510(6) 0.9021(8) 0.078(2) Uiso 1 d D . Cl2 Cl 0.6723(2) 0.6893(2) 0.2165(3) 0.0521(7) Uani 1 d D . O5 O 0.6798(6) 0.7391(5) 0.1071(8) 0.074(2) Uiso 1 d D . O6 O 0.6021(7) 0.7433(6) 0.3238(9) 0.090(3) Uiso 1 d D . O7 O 0.6362(6) 0.6034(4) 0.1285(8) 0.060(2) Uiso 1 d D . O8 O 0.7885(6) 0.6529(5) 0.3154(8) 0.073(2) Uiso 1 d D . Cl3 Cl 0.1096(5) 0.9954(4) 0.5951(6) 0.1015(8) Uani 1 d D . O9 O 0.1070(13) 1.0371(11) 0.7526(11) 0.231(9) Uiso 1 d D . O10 O -0.0020(9) 1.0201(11) 0.4823(15) 0.234(9) Uiso 1 d D . O11 O 0.1885(8) 1.0228(8) 0.5436(15) 0.205(7) Uiso 1 d D . O12 O 0.1445(13) 0.8942(6) 0.5819(17) 0.185(6) Uiso 1 d D . Cl4 Cl 0.1234(3) 0.4964(3) 0.5760(4) 0.0765(11) Uani 1 d D . O13 O 0.1407(10) 0.5664(6) 0.5140(14) 0.193(7) Uiso 1 d D . O14 O 0.2210(8) 0.4629(8) 0.6944(11) 0.135(4) Uiso 1 d D . O15 O 0.0193(8) 0.5377(13) 0.6292(17) 0.300 Uiso 1 d D . O16 O 0.1050(10) 0.4200(6) 0.4475(11) 0.132(4) Uiso 1 d D . O17 O 0.0493(7) 0.7227(6) 0.2996(9) 0.073(2) Uiso 1 d . . O18 O 0.1091(11) 0.3141(9) 0.8703(15) 0.131(4) Uiso 1 d . . O19 O 0.7884(10) 0.1609(8) 0.6531(13) 0.110(3) Uiso 1 d . . O20 O 0.8419(10) 0.8758(8) 0.3382(14) 0.126(4) Uiso 1 d . . O21 O 0.4218(12) 0.8305(10) 0.5224(16) 0.129(4) Uiso 1 d . . O22 O 0.1441(18) 0.2259(15) 0.5517(25) 0.113(6) Uiso 0.54(5) d P . 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 0.03614(12) 0.03107(12) 0.03262(12) 0.00916(9) 0.00275(10) -0.01263(10) Pt2 0.0460(2) 0.02785(13) 0.03133(13) 0.00788(10) 0.00819(12) -0.01260(12) Cl1 0.0675(12) 0.128(2) 0.103(2) 0.0550(13) 0.0291(11) -0.0342(13) Cl2 0.0603(13) 0.0508(11) 0.0411(10) 0.0055(9) 0.0121(10) -0.0121(10) Cl3 0.176(2) 0.0935(13) 0.0721(11) -0.0133(10) 0.0653(12) -0.0730(12) Cl4 0.067(2) 0.0712(13) 0.069(2) 0.0148(13) -0.0066(14) -0.0107(14) _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 N1A 2.036(7) . ? Pt1 N11A 2.043(8) . ? Pt1 N10A 2.060(7) . ? Pt1 N12A 2.082(7) . ? O2'A C2'A 1.426(13) . ? O3'A C3'A 1.44(2) . ? O4'A C1'A 1.385(10) . ? O4'A C4'A 1.401(10) . ? O5'A C5'A 1.43(2) . ? C1'A N9A 1.467(10) . ? C1'A C2'A 1.572(11) . ? C1'A H1'A 0.98 . ? C2'A C3'A 1.556(11) . ? C2'A H2'A 0.98 . ? C3'A C4'A 1.489(13) . ? C3'A H3'A 0.98 . ? C4'A C5'A 1.54(2) . ? C4'A H4'A 0.98 . ? C5'A H5'1 0.97 . ? C5'A H5'2 0.97 . ? N1A C6A 1.335(9) . ? N1A C2A 1.379(10) . ? N3A C2A 1.287(10) . ? N3A C4A 1.368(9) . ? N6A C6A 1.399(10) . ? N6A H6A1 0.86 . ? N6A H6A2 0.86 . ? N7A C8A 1.298(10) . ? N7A C5A 1.416(8) . ? N9A C4A 1.361(10) . ? N9A C8A 1.385(8) . ? N10A C10A 1.539(14) . ? N10A H10A 0.90 . ? N10A H10B 0.90 . ? N11A C11A 1.386(12) . ? N11A C12A 1.476(11) . ? N11A H11A 0.91 . ? N12A C13A 1.495(11) . ? N12A H12A 0.90 . ? N12A H12B 0.90 . ? C2A H2A 0.93 . ? C4A C5A 1.425(10) . ? C5A C6A 1.384(11) . ? C8A H8A 0.93 . ? C10A C11A 1.462(14) . ? C10A H10A 0.97 . ? C10A H10B 0.97 . ? C11A H11A 0.97 . ? C11A H11B 0.97 . ? C12A C13A 1.477(14) . ? C12A H12A 0.97 . ? C12A H12B 0.97 . ? C13A H13A 0.97 . ? C13A H13B 0.97 . ? Pt2 N11B 2.007(8) . ? Pt2 N10B 2.021(8) . ? Pt2 N12B 2.047(8) . ? Pt2 N1B 2.051(7) . ? O2'B C2'B 1.444(10) . ? O3'B C3'B 1.391(11) . ? O4'B C1'B 1.404(9) . ? O4'B C4'B 1.466(10) . ? O5'B C5'B 1.43(2) . ? O5'C C5'B 1.47(2) . ? C1'B N9B 1.494(11) . ? C1'B C2'B 1.509(11) . ? C1'B H1'B 0.98 . ? C2'B C3'B 1.536(10) . ? C2'B H2'B 0.98 . ? C3'B C4'B 1.539(11) . ? C3'B H3'B 0.98 . ? C4'B C5'B 1.53(2) . ? C4'B H4'B 0.98 . ? C5'B H5'B 0.98 . ? N1B C2B 1.348(10) . ? N1B C6B 1.433(9) . ? N3B C2B 1.321(11) . ? N3B C4B 1.363(8) . ? N6B C6B 1.292(10) . ? N6B H6B1 0.86 . ? N6B H6B2 0.86 . ? N7B C8B 1.310(11) . ? N7B C5B 1.383(10) . ? N9B C4B 1.345(10) . ? N9B C8B 1.354(9) . ? N10B C10B 1.500(12) . ? N10B H10C 0.90 . ? N10B H10D 0.90 . ? N11B C11C 1.421(13) . ? N11B C12B 1.47(2) . ? N11B C11B 1.472(14) . ? N11B C12C 1.51(2) . ? N12B C13B 1.461(14) . ? N12B H12C 0.90 . ? N12B H12D 0.90 . ? C2B H2B 0.93 . ? C4B C5B 1.350(11) . ? C5B C6B 1.429(13) . ? C8B H8B 0.93 . ? C10B C11C 1.485(15) . ? C10B C11B 1.519(13) . ? C11B C11C 1.07(2) . ? C12B C12C 0.99(2) . ? C12B C13B 1.526(14) . ? C12C C13B 1.521(15) . ? Cl1 O2 1.345(9) . ? Cl1 O3 1.379(10) . ? Cl1 O4 1.397(7) . ? Cl1 O1 1.401(9) . ? Cl2 O6 1.383(8) . ? Cl2 O5 1.385(8) . ? Cl2 O8 1.417(6) . ? Cl2 O7 1.418(6) . ? Cl3 O9 1.359(10) . ? Cl3 O11 1.381(12) . ? Cl3 O12 1.387(9) . ? Cl3 O10 1.403(10) . ? Cl4 O14 1.354(8) . ? Cl4 O13 1.376(11) . ? Cl4 O16 1.382(8) . ? Cl4 O15 1.382(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Pt1 N11A 174.8(3) . . ? N1A Pt1 N10A 92.0(3) . . ? N11A Pt1 N10A 83.0(3) . . ? N1A Pt1 N12A 99.3(3) . . ? N11A Pt1 N12A 85.5(3) . . ? N10A Pt1 N12A 167.0(3) . . ? C1'A O4'A C4'A 112.4(7) . . ? O4'A C1'A N9A 110.2(6) . . ? O4'A C1'A C2'A 103.3(6) . . ? N9A C1'A C2'A 111.1(7) . . ? O4'A C1'A H1'A 110.7(5) . . ? N9A C1'A H1'A 110.7(3) . . ? C2'A C1'A H1'A 110.7(4) . . ? O2'A C2'A C3'A 117.9(9) . . ? O2'A C2'A C1'A 106.2(8) . . ? C3'A C2'A C1'A 100.8(7) . . ? O2'A C2'A H2'A 110.5(6) . . ? C3'A C2'A H2'A 110.5(6) . . ? C1'A C2'A H2'A 110.5(5) . . ? O3'A C3'A C4'A 116.1(13) . . ? O3'A C3'A C2'A 105.1(9) . . ? C4'A C3'A C2'A 97.9(8) . . ? O3'A C3'A H3'A 112.2(10) . . ? C4'A C3'A H3'A 112.2(6) . . ? C2'A C3'A H3'A 112.2(6) . . ? O4'A C4'A C3'A 106.3(8) . . ? O4'A C4'A C5'A 118.2(10) . . ? C3'A C4'A C5'A 111.8(11) . . ? O4'A C4'A H4'A 106.6(5) . . ? C3'A C4'A H4'A 106.6(6) . . ? C5'A C4'A H4'A 106.6(11) . . ? O5'A C5'A C4'A 105.3(15) . . ? O5'A C5'A H5'1 110.7(16) . . ? C4'A C5'A H5'1 110.7(9) . . ? O5'A C5'A H5'2 110.7(13) . . ? C4'A C5'A H5'2 110.7(11) . . ? H5'1 C5'A H5'2 108.8 . . ? C6A N1A C2A 118.2(7) . . ? C6A N1A Pt1 124.0(6) . . ? C2A N1A Pt1 117.4(4) . . ? C2A N3A C4A 110.4(6) . . ? C6A N6A H6A1 120.0(4) . . ? C6A N6A H6A2 120.0(4) . . ? H6A1 N6A H6A2 120.0 . . ? C8A N7A C5A 104.2(6) . . ? C4A N9A C8A 104.9(6) . . ? C4A N9A C1'A 124.5(6) . . ? C8A N9A C1'A 130.6(6) . . ? C10A N10A Pt1 106.6(5) . . ? C10A N10A H10A 110.4(5) . . ? Pt1 N10A H10A 110.4(2) . . ? C10A N10A H10B 110.4(4) . . ? Pt1 N10A H10B 110.4(2) . . ? H10A N10A H10B 108.6 . . ? C11A N11A C12A 128.2(9) . . ? C11A N11A Pt1 111.2(6) . . ? C12A N11A Pt1 105.7(6) . . ? C11A N11A H11A 102.9(5) . . ? C12A N11A H11A 102.9(4) . . ? Pt1 N11A H11A 102.9(2) . . ? C13A N12A Pt1 108.6(5) . . ? C13A N12A H12A 110.0(5) . . ? Pt1 N12A H12A 110.0(2) . . ? C13A N12A H12B 110.0(4) . . ? Pt1 N12A H12B 110.0(2) . . ? H12A N12A H12B 108.4 . . ? N3A C2A N1A 129.9(6) . . ? N3A C2A H2A 115.0(4) . . ? N1A C2A H2A 115.1(4) . . ? N9A C4A N3A 126.8(7) . . ? N9A C4A C5A 107.3(6) . . ? N3A C4A C5A 125.9(7) . . ? C6A C5A N7A 134.8(7) . . ? C6A C5A C4A 116.4(6) . . ? N7A C5A C4A 107.5(6) . . ? N1A C6A C5A 118.6(7) . . ? N1A C6A N6A 119.5(8) . . ? C5A C6A N6A 117.9(6) . . ? N7A C8A N9A 115.2(6) . . ? N7A C8A H8A 122.4(4) . . ? N9A C8A H8A 122.4(4) . . ? C11A C10A N10A 112.1(9) . . ? C11A C10A H10A 109.2(7) . . ? N10A C10A H10A 109.2(5) . . ? C11A C10A H10B 109.2(5) . . ? N10A C10A H10B 109.2(5) . . ? H10A C10A H10B 107.9 . . ? N11A C11A C10A 109.1(10) . . ? N11A C11A H11A 109.9(5) . . ? C10A C11A H11A 109.9(5) . . ? N11A C11A H11B 109.9(5) . . ? C10A C11A H11B 109.9(6) . . ? H11A C11A H11B 108.3 . . ? N11A C12A C13A 116.5(9) . . ? N11A C12A H12A 108.2(5) . . ? C13A C12A H12A 108.2(5) . . ? N11A C12A H12B 108.2(5) . . ? C13A C12A H12B 108.2(5) . . ? H12A C12A H12B 107.3 . . ? C12A C13A N12A 106.9(7) . . ? C12A C13A H13A 110.3(5) . . ? N12A C13A H13A 110.3(4) . . ? C12A C13A H13B 110.3(5) . . ? N12A C13A H13B 110.3(4) . . ? H13A C13A H13B 108.6 . . ? N11B Pt2 N10B 83.9(3) . . ? N11B Pt2 N12B 85.0(3) . . ? N10B Pt2 N12B 168.8(3) . . ? N11B Pt2 N1B 172.2(3) . . ? N10B Pt2 N1B 94.3(3) . . ? N12B Pt2 N1B 96.9(3) . . ? C1'B O4'B C4'B 112.0(6) . . ? O4'B C1'B N9B 110.1(7) . . ? O4'B C1'B C2'B 106.8(6) . . ? N9B C1'B C2'B 112.9(6) . . ? O4'B C1'B H1'B 109.0(4) . . ? N9B C1'B H1'B 109.0(3) . . ? C2'B C1'B H1'B 109.0(4) . . ? O2'B C2'B C1'B 104.9(6) . . ? O2'B C2'B C3'B 107.8(7) . . ? C1'B C2'B C3'B 103.7(6) . . ? O2'B C2'B H2'B 113.2(4) . . ? C1'B C2'B H2'B 113.2(4) . . ? C3'B C2'B H2'B 113.2(4) . . ? O3'B C3'B C2'B 113.0(7) . . ? O3'B C3'B C4'B 110.9(7) . . ? C2'B C3'B C4'B 103.9(6) . . ? O3'B C3'B H3'B 109.6(4) . . ? C2'B C3'B H3'B 109.6(4) . . ? C4'B C3'B H3'B 109.6(5) . . ? O4'B C4'B C5'B 117.9(11) . . ? O4'B C4'B C3'B 104.8(6) . . ? C5'B C4'B C3'B 115.4(8) . . ? O4'B C4'B H4'B 105.9(5) . . ? C5'B C4'B H4'B 105.9(8) . . ? C3'B C4'B H4'B 105.9(5) . . ? O5'B C5'B O5'C 117.3(21) . . ? O5'B C5'B C4'B 103.3(13) . . ? O5'C C5'B C4'B 98.8(13) . . ? O5'B C5'B H5'B 112.1(11) . . ? O5'C C5'B H5'B 112.1(13) . . ? C4'B C5'B H5'B 112.1(8) . . ? C2B N1B C6B 120.5(7) . . ? C2B N1B Pt2 118.0(5) . . ? C6B N1B Pt2 120.8(5) . . ? C2B N3B C4B 112.5(6) . . ? C6B N6B H6B1 120.0(5) . . ? C6B N6B H6B2 120.0(5) . . ? H6B1 N6B H6B2 120.0 . . ? C8B N7B C5B 103.7(7) . . ? C4B N9B C8B 107.7(7) . . ? C4B N9B C1'B 124.7(6) . . ? C8B N9B C1'B 127.5(7) . . ? C10B N10B Pt2 109.4(6) . . ? C10B N10B H10C 109.8(4) . . ? Pt2 N10B H10C 109.8(2) . . ? C10B N10B H10D 109.8(5) . . ? Pt2 N10B H10D 109.8(3) . . ? H10C N10B H10D 108.2 . . ? C11C N11B C12B 141.3(11) . . ? C11C N11B C11B 43.4(9) . . ? C12B N11B C11B 126.2(8) . . ? C11C N11B C12C 118.2(10) . . ? C12B N11B C12C 38.6(9) . . ? C11B N11B C12C 140.3(11) . . ? C11C N11B Pt2 109.8(7) . . ? C12B N11B Pt2 107.8(8) . . ? C11B N11B Pt2 111.8(9) . . ? C12C N11B Pt2 107.7(7) . . ? C13B N12B Pt2 112.0(5) . . ? C13B N12B H12C 109.2(5) . . ? Pt2 N12B H12C 109.2(2) . . ? C13B N12B H12D 109.2(5) . . ? Pt2 N12B H12D 109.2(2) . . ? H12C N12B H12D 107.9 . . ? N3B C2B N1B 127.3(6) . . ? N3B C2B H2B 116.4(4) . . ? N1B C2B H2B 116.4(4) . . ? N9B C4B C5B 105.5(6) . . ? N9B C4B N3B 127.9(7) . . ? C5B C4B N3B 126.6(8) . . ? C4B C5B N7B 110.8(8) . . ? C4B C5B C6B 120.2(7) . . ? N7B C5B C6B 128.5(7) . . ? N6B C6B C5B 127.5(7) . . ? N6B C6B N1B 116.1(7) . . ? C5B C6B N1B 112.7(7) . . ? N7B C8B N9B 111.7(7) . . ? N7B C8B H8B 124.2(4) . . ? N9B C8B H8B 124.2(5) . . ? C11C C10B N10B 112.5(8) . . ? C11C C10B C11B 41.7(9) . . ? N10B C10B C11B 111.5(9) . . ? C11C C11B N11B 65.8(10) . . ? C11C C11B C10B 67.5(10) . . ? N11B C11B C10B 105.5(9) . . ? C11B C11C N11B 70.8(10) . . ? C11B C11C C10B 70.8(11) . . ? N11B C11C C10B 110.0(10) . . ? C12C C12B N11B 73.1(12) . . ? C12C C12B C13B 70.8(11) . . ? N11B C12B C13B 113.4(11) . . ? C12B C12C N11B 68.3(13) . . ? C12B C12C C13B 71.4(11) . . ? N11B C12C C13B 111.3(12) . . ? N12B C13B C12C 111.5(9) . . ? N12B C13B C12B 107.9(11) . . ? C12C C13B C12B 37.9(9) . . ? O2 Cl1 O3 112.7(9) . . ? O2 Cl1 O4 114.5(7) . . ? O3 Cl1 O4 106.1(6) . . ? O2 Cl1 O1 111.0(8) . . ? O3 Cl1 O1 106.0(7) . . ? O4 Cl1 O1 106.0(7) . . ? O6 Cl2 O5 116.2(5) . . ? O6 Cl2 O8 105.9(4) . . ? O5 Cl2 O8 109.8(5) . . ? O6 Cl2 O7 111.3(5) . . ? O5 Cl2 O7 109.1(4) . . ? O8 Cl2 O7 103.8(4) . . ? O9 Cl3 O11 112.3(9) . . ? O9 Cl3 O12 108.9(9) . . ? O11 Cl3 O12 108.7(9) . . ? O9 Cl3 O10 113.6(8) . . ? O11 Cl3 O10 105.8(9) . . ? O12 Cl3 O10 107.3(9) . . ? O14 Cl4 O13 110.9(7) . . ? O14 Cl4 O16 109.5(6) . . ? O13 Cl4 O16 107.1(7) . . ? O14 Cl4 O15 113.5(8) . . ? O13 Cl4 O15 107.3(9) . . ? O16 Cl4 O15 108.3(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 O4'A C1'A N9A C4A -168.0(7) . . . . ? O4'B C1'B N9B C4B -81.2(8) . . . . ? _refine_diff_density_max 0.957 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.163 #===END