# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name E.McInnes _publ_contact_author_name 'Dr Eric McInnes' _publ_contact_author_email eric.mcinnes@manchester.ac.uk data_prm067 _database_code_depnum_ccdc_archive 'CCDC 660844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (C10H6N4O4).(C4H8O2) _chemical_formula_sum 'C14 H14 N4 O6' _chemical_formula_weight 334.29 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' _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 6.4941(6) _cell_length_b 6.5761(6) _cell_length_c 9.3664(8) _cell_angle_alpha 85.2000(10) _cell_angle_beta 87.9100(10) _cell_angle_gamma 66.0050(10) _cell_volume 364.15(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2575 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 28.7 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.81 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 174 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.812777 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3240 _diffrn_reflns_av_R_equivalents 0.0135 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.72 _reflns_number_total 1686 _reflns_number_gt 1628 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0672P)^2^+0.0993P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.12(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1686 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 N1 N 0.20178(16) 0.12486(16) 0.48139(11) 0.0254(3) Uani 1 1 d . . . C2 C 0.03143(17) 0.07805(17) 0.53853(11) 0.0216(3) Uani 1 1 d . . . C3 C -0.08407(19) 0.16798(19) 0.66234(12) 0.0260(3) Uani 1 1 d . . . H3 H -0.2031 0.1302 0.6995 0.031 Uiso 1 1 calc R . . C4 C -0.0213(2) 0.3135(2) 0.72980(13) 0.0274(3) Uani 1 1 d . . . H4 H -0.0953 0.3782 0.8144 0.033 Uiso 1 1 calc R . . C5 C 0.15298(19) 0.36131(18) 0.66962(12) 0.0247(3) Uani 1 1 d . . . N51 N 0.22402(17) 0.51596(17) 0.73608(12) 0.0299(3) Uani 1 1 d . . . O51 O 0.12969(17) 0.59318(18) 0.84701(12) 0.0432(3) Uani 1 1 d . . . O52 O 0.37390(17) 0.56077(17) 0.67732(11) 0.0391(3) Uani 1 1 d . . . C6 C 0.26183(19) 0.26517(19) 0.54698(13) 0.0260(3) Uani 1 1 d . . . H6 H 0.3821 0.2998 0.5085 0.031 Uiso 1 1 calc R . . C2S C 0.6132(2) 1.1395(2) 0.99918(13) 0.0307(3) Uani 1 1 d . . . H2S1 H 0.6103 1.2916 0.9944 0.037 Uiso 1 1 calc R . . H2S2 H 0.7717 1.0309 1.0121 0.037 Uiso 1 1 calc R . . O1S O 0.52784(15) 1.10708(14) 0.86877(9) 0.0303(3) Uani 1 1 d . . . C3S C 0.4747(2) 1.1097(2) 1.12436(14) 0.0317(3) Uani 1 1 d . . . H3S1 H 0.5384 1.1290 1.2141 0.038 Uiso 1 1 calc R . . H3S2 H 0.3185 1.2248 1.1147 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0246(5) 0.0272(5) 0.0288(5) -0.0032(4) -0.0006(4) -0.0148(4) C2 0.0206(5) 0.0208(5) 0.0244(5) -0.0002(4) -0.0033(4) -0.0095(4) C3 0.0245(5) 0.0280(6) 0.0295(6) -0.0042(4) 0.0013(4) -0.0144(4) C4 0.0264(6) 0.0276(6) 0.0300(6) -0.0073(4) 0.0002(4) -0.0118(5) C5 0.0251(5) 0.0207(5) 0.0300(6) -0.0018(4) -0.0074(4) -0.0105(4) N51 0.0281(5) 0.0245(5) 0.0394(6) -0.0046(4) -0.0084(4) -0.0119(4) O51 0.0398(6) 0.0445(6) 0.0517(6) -0.0247(5) 0.0020(4) -0.0199(5) O52 0.0419(6) 0.0378(5) 0.0494(6) -0.0044(4) -0.0037(4) -0.0278(4) C6 0.0236(5) 0.0267(6) 0.0318(6) -0.0018(4) -0.0022(4) -0.0143(4) C2S 0.0357(6) 0.0327(6) 0.0316(6) -0.0023(5) -0.0038(5) -0.0217(5) O1S 0.0385(5) 0.0325(5) 0.0265(4) -0.0002(3) -0.0026(3) -0.0212(4) C3S 0.0384(7) 0.0300(6) 0.0306(6) -0.0085(4) 0.0016(5) -0.0169(5) _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 N1 C6 1.3363(15) . ? N1 C2 1.3458(14) . ? C2 C3 1.3957(16) . ? C2 C2 1.492(2) 2_556 ? C3 C4 1.3854(16) . ? C4 C5 1.3819(16) . ? C5 C6 1.3849(17) . ? C5 N51 1.4639(14) . ? N51 O51 1.2254(15) . ? N51 O52 1.2265(15) . ? C2S O1S 1.4263(14) . ? C2S C3S 1.5004(17) . ? O1S C3S 1.4283(15) 2_677 ? C3S O1S 1.4283(15) 2_677 ? 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 C6 N1 C2 117.92(10) . . ? N1 C2 C3 123.31(10) . . ? N1 C2 C2 116.24(12) . 2_556 ? C3 C2 C2 120.45(12) . 2_556 ? C4 C3 C2 118.52(11) . . ? C5 C4 C3 117.63(11) . . ? C4 C5 C6 121.00(11) . . ? C4 C5 N51 119.69(11) . . ? C6 C5 N51 119.30(11) . . ? O51 N51 O52 123.96(11) . . ? O51 N51 C5 117.96(11) . . ? O52 N51 C5 118.09(11) . . ? N1 C6 C5 121.62(11) . . ? O1S C2S C3S 110.61(10) . . ? C2S O1S C3S 110.14(9) . 2_677 ? O1S C3S C2S 110.46(10) 2_677 . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.355 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.060 data_prm168 _database_code_depnum_ccdc_archive 'CCDC 838414' #TrackingRef '- 3-NO2-bipy.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 N3 O2' _chemical_formula_sum 'C10 H7 N3 O2' _chemical_formula_weight 201.19 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.4647(3) _cell_length_b 10.1931(4) _cell_length_c 11.7396(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 893.25(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1047 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour beige _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details 'SADABS 2004/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5306 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.02 _reflns_number_total 935 _reflns_number_gt 833 _reflns_threshold_expression I>2\s(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'PLATON, ENCIFER, XCIF' _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^)+(0.0346P)^2^+0.0717P] 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(10) _refine_ls_number_reflns 935 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 N1 N -0.1188(2) 0.14138(17) 0.81480(14) 0.0251(4) Uani 1 1 d . . . C2 C 0.0518(3) 0.1804(2) 0.80890(17) 0.0208(5) Uani 1 1 d . . . C3 C 0.1071(3) 0.2613(2) 0.72006(16) 0.0222(5) Uani 1 1 d . . . C4 C -0.0106(3) 0.3016(2) 0.63647(18) 0.0243(5) Uani 1 1 d . . . H4 H 0.0288 0.3542 0.5745 0.029 Uiso 1 1 calc R . . C5 C -0.1863(3) 0.2634(2) 0.64559(17) 0.0268(5) Uani 1 1 d . . . H5 H -0.2727 0.2906 0.5911 0.032 Uiso 1 1 calc R . . C6 C -0.2342(3) 0.1843(2) 0.73625(17) 0.0264(5) Uani 1 1 d . . . H6 H -0.3562 0.1591 0.7431 0.032 Uiso 1 1 calc R . . N3 N 0.2904(2) 0.31268(18) 0.71207(15) 0.0258(4) Uani 1 1 d . . . O31 O 0.3771(2) 0.28359(18) 0.62697(13) 0.0378(4) Uani 1 1 d . . . O32 O 0.3422(2) 0.38556(16) 0.78785(12) 0.0342(4) Uani 1 1 d . . . N1' N 0.3479(2) 0.11583(16) 0.86941(14) 0.0231(4) Uani 1 1 d . . . C2' C 0.1752(3) 0.1299(2) 0.89857(17) 0.0205(5) Uani 1 1 d . . . C3' C 0.1091(3) 0.0987(2) 1.00588(17) 0.0256(5) Uani 1 1 d . . . H3' H -0.0140 0.1110 1.0234 0.031 Uiso 1 1 calc R . . C4' C 0.2262(3) 0.0495(2) 1.08659(17) 0.0263(5) Uani 1 1 d . . . H4' H 0.1846 0.0253 1.1601 0.032 Uiso 1 1 calc R . . C5' C 0.4051(3) 0.0364(2) 1.05816(17) 0.0259(5) Uani 1 1 d . . . H5' H 0.4891 0.0043 1.1122 0.031 Uiso 1 1 calc R . . C6' C 0.4593(3) 0.0707(2) 0.94979(18) 0.0258(5) Uani 1 1 d . . . H6' H 0.5825 0.0618 0.9311 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0205(11) 0.0282(10) 0.0266(9) -0.0005(8) 0.0019(8) 0.0022(8) C2 0.0197(11) 0.0206(10) 0.0221(10) -0.0044(9) 0.0011(9) 0.0033(9) C3 0.0223(12) 0.0220(11) 0.0222(10) -0.0020(9) -0.0003(9) 0.0028(9) C4 0.0249(13) 0.0238(12) 0.0241(11) 0.0018(10) 0.0021(9) 0.0036(9) C5 0.0246(13) 0.0306(13) 0.0251(11) -0.0003(10) -0.0039(10) 0.0037(10) C6 0.0182(12) 0.0298(12) 0.0312(12) -0.0033(10) -0.0012(9) 0.0004(10) N3 0.0249(10) 0.0261(10) 0.0264(9) 0.0084(9) -0.0039(8) -0.0013(8) O31 0.0262(9) 0.0556(11) 0.0315(9) 0.0069(8) 0.0061(7) -0.0017(8) O32 0.0350(10) 0.0306(9) 0.0370(8) 0.0028(8) -0.0124(8) -0.0063(8) N1' 0.0216(11) 0.0228(10) 0.0250(9) 0.0011(8) -0.0010(8) 0.0014(8) C2' 0.0205(12) 0.0177(10) 0.0233(10) -0.0015(9) -0.0015(9) -0.0015(8) C3' 0.0266(12) 0.0253(12) 0.0250(10) -0.0008(10) 0.0040(10) -0.0004(9) C4' 0.0346(14) 0.0242(11) 0.0200(10) 0.0013(10) 0.0002(9) -0.0029(10) C5' 0.0298(13) 0.0232(11) 0.0249(10) 0.0003(9) -0.0068(9) 0.0030(10) C6' 0.0211(12) 0.0251(12) 0.0311(11) 0.0025(10) -0.0021(9) 0.0014(9) _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 N1 C2 1.336(3) . ? N1 C6 1.336(3) . ? C2 C3 1.392(3) . ? C2 C2' 1.491(3) . ? C3 C4 1.380(3) . ? C3 N3 1.468(3) . ? C4 H4 0.950 . ? C4 C5 1.372(3) . ? C5 H5 0.950 . ? C5 C6 1.382(3) . ? C6 H6 0.950 . ? N3 O31 1.227(2) . ? N3 O32 1.222(2) . ? N1' C2' 1.342(3) . ? N1' C6' 1.339(3) . ? C2' C3' 1.390(3) . ? C3' H3' 0.950 . ? C3' C4' 1.383(3) . ? C4' H4' 0.950 . ? C4' C5' 1.383(3) . ? C5' H5' 0.950 . ? C5' C6' 1.380(3) . ? C6' H6' 0.950 . ? 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 C2 N1 C6 118.77(19) . . ? N1 C2 C3 119.87(18) . . ? N1 C2 C2' 116.72(18) . . ? C3 C2 C2' 123.38(18) . . ? C2 C3 C4 121.3(2) . . ? C2 C3 N3 122.39(17) . . ? C4 C3 N3 116.21(18) . . ? C3 C4 H4 121.0 . . ? C3 C4 C5 117.9(2) . . ? H4 C4 C5 121.0 . . ? C4 C5 H5 120.9 . . ? C4 C5 C6 118.2(2) . . ? H5 C5 C6 120.9 . . ? N1 C6 C5 123.8(2) . . ? N1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? C3 N3 O31 117.21(18) . . ? C3 N3 O32 117.72(17) . . ? O31 N3 O32 124.98(19) . . ? C2' N1' C6' 116.98(18) . . ? C2 C2' N1' 116.79(17) . . ? C2 C2' C3' 119.98(18) . . ? N1' C2' C3' 123.23(19) . . ? C2' C3' H3' 120.7 . . ? C2' C3' C4' 118.6(2) . . ? H3' C3' C4' 120.7 . . ? C3' C4' H4' 120.7 . . ? C3' C4' C5' 118.7(2) . . ? H4' C4' C5' 120.7 . . ? C4' C5' H5' 120.6 . . ? C4' C5' C6' 118.7(2) . . ? H5' C5' C6' 120.6 . . ? N1' C6' C5' 123.7(2) . . ? N1' C6' H6' 118.1 . . ? C5' C6' H6' 118.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.134 _refine_diff_density_min -0.122 _refine_diff_density_rms 0.035 # Attachment '- [Pt(3,3-(NO2)2-bpy)Cl2].CIF' data_prm064 _database_code_depnum_ccdc_archive 'CCDC 838415' #TrackingRef '- [Pt(3,3-(NO2)2-bpy)Cl2].CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H19 Cl4 N9 O9 Pt2' _chemical_formula_weight 1097.45 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.3359(12) _cell_length_b 14.1844(12) _cell_length_c 14.9479(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.909(2) _cell_angle_gamma 90.00 _cell_volume 2994.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7311 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.5 _exptl_crystal_description Block _exptl_crystal_colour Dark _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 9.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.630299 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS - Bruker Nonius' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method '\f \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18668 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.86 _reflns_number_total 7207 _reflns_number_gt 6226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0200P)^2^+3.5906P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7207 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.655060(11) 0.908023(11) 0.514133(11) 0.01714(5) Uani 1 1 d . . . C10 C 0.6040(3) 1.1102(3) 0.5062(3) 0.0230(10) Uani 1 1 d . . . H10A H 0.6140 1.1053 0.5705 0.028 Uiso 1 1 calc R . . Pt2 Pt 0.377020(11) 0.506736(11) -0.016575(11) 0.01746(5) Uani 1 1 d . . . N7 N 0.4185(2) 0.6310(2) 0.0414(2) 0.0189(7) Uani 1 1 d . . . Cl3 Cl 0.38503(8) 0.55167(8) -0.16202(7) 0.0263(2) Uani 1 1 d . . . N1 N 0.6545(2) 0.8775(2) 0.3831(2) 0.0177(7) Uani 1 1 d . . . C12 C 0.4550(3) 0.7942(3) 0.0322(3) 0.0259(10) Uani 1 1 d . . . Cl5 Cl 0.32709(8) 0.36157(8) -0.07289(8) 0.0276(2) Uani 1 1 d . . . C9 C 0.5736(3) 1.1947(3) 0.4662(3) 0.0254(10) Uani 1 1 d . . . H9A H 0.5685 1.2491 0.5021 0.030 Uiso 1 1 calc R . . Cl1 Cl 0.65877(8) 0.95437(9) 0.66136(7) 0.0277(2) Uani 1 1 d . . . N8 N 0.3755(2) 0.4756(2) 0.1143(2) 0.0167(7) Uani 1 1 d . . . Cl2 Cl 0.68724(9) 0.75801(8) 0.56822(8) 0.0288(3) Uani 1 1 d . . . N6 N 0.4881(3) 0.5775(3) 0.3352(3) 0.0237(8) Uani 1 1 d . . . C15 C 0.4196(3) 0.6370(3) 0.1321(3) 0.0176(8) Uani 1 1 d . . . C16 C 0.4087(3) 0.5439(3) 0.1751(3) 0.0176(8) Uani 1 1 d . . . O7 O 0.5500(2) 0.6257(2) 0.3107(2) 0.0268(7) Uani 1 1 d . . . C7 C 0.5625(3) 1.1185(3) 0.3237(3) 0.0202(9) Uani 1 1 d . . . O5 O 0.4489(3) 0.8142(2) 0.3030(2) 0.0378(9) Uani 1 1 d . . . N5 N 0.4078(3) 0.7471(3) 0.2613(3) 0.0264(9) Uani 1 1 d . . . O2 O 0.6905(2) 1.0886(2) 0.1973(2) 0.0302(8) Uani 1 1 d . . . O6 O 0.3477(2) 0.6987(2) 0.2889(2) 0.0325(8) Uani 1 1 d . . . O3 O 0.4887(2) 1.0453(2) 0.1928(2) 0.0263(7) Uani 1 1 d . . . C6 C 0.6047(3) 1.0372(3) 0.3649(3) 0.0167(8) Uani 1 1 d . . . O1 O 0.6291(3) 0.9931(2) 0.0901(2) 0.0352(9) Uani 1 1 d . . . C17 C 0.4312(3) 0.5181(3) 0.2659(3) 0.0198(9) Uani 1 1 d . . . C8 C 0.5508(3) 1.1984(3) 0.3731(3) 0.0242(10) Uani 1 1 d . . . C4 C 0.6566(3) 0.9358(3) 0.2360(3) 0.0186(9) Uani 1 1 d . . . C5 C 0.6381(3) 0.9511(3) 0.3233(3) 0.0162(8) Uani 1 1 d . . . C1 C 0.6794(3) 0.7921(3) 0.3556(3) 0.0219(9) Uani 1 1 d . . . H1A H 0.6903 0.7422 0.3985 0.026 Uiso 1 1 calc R . . C13 C 0.4489(3) 0.8045(3) 0.1223(3) 0.0250(10) Uani 1 1 d . . . H13A H 0.4584 0.8644 0.1509 0.030 Uiso 1 1 calc R . . C2 C 0.6897(4) 0.7750(3) 0.2671(3) 0.0262(10) Uani 1 1 d . . . N3 N 0.6583(3) 1.0125(3) 0.1695(3) 0.0237(8) Uani 1 1 d . . . N4 N 0.5168(3) 1.1206(3) 0.2279(3) 0.0238(8) Uani 1 1 d . . . C3 C 0.6811(3) 0.8483(3) 0.2072(3) 0.0237(10) Uani 1 1 d . . . H3A H 0.6918 0.8392 0.1468 0.028 Uiso 1 1 calc R . . C14 C 0.4286(3) 0.7267(3) 0.1708(3) 0.0203(9) Uani 1 1 d . . . O4 O 0.5063(3) 1.1968(2) 0.1900(2) 0.0382(9) Uani 1 1 d . . . N2 N 0.6198(2) 1.0346(2) 0.4569(2) 0.0177(7) Uani 1 1 d . . . O8 O 0.4731(3) 0.5735(3) 0.4132(2) 0.0339(8) Uani 1 1 d . . . N9 N 0.7340(3) 1.4424(3) 0.5294(3) 0.0264(9) Uani 1 1 d . . . O9 O 0.6250(3) 1.4073(3) 0.4048(3) 0.0439(10) Uani 1 1 d . . . C19 C 0.3654(4) 0.3659(3) 0.2338(3) 0.0281(11) Uani 1 1 d . . . C18 C 0.4076(3) 0.4300(3) 0.2963(3) 0.0235(10) Uani 1 1 d . . . H18A H 0.4204 0.4147 0.3591 0.028 Uiso 1 1 calc R . . C11 C 0.4353(3) 0.7074(3) -0.0069(3) 0.0228(9) Uani 1 1 d . . . C20 C 0.3533(3) 0.3897(3) 0.1431(3) 0.0236(10) Uani 1 1 d . . . H20A H 0.3283 0.3438 0.0992 0.028 Uiso 1 1 calc R . . C21 C 0.6652(4) 1.4632(4) 0.4614(3) 0.0308(11) Uani 1 1 d . . . H21A H 0.6451 1.5271 0.4558 0.037 Uiso 1 1 calc R . . C23 C 0.7798(4) 1.5147(4) 0.5898(4) 0.0385(13) Uani 1 1 d . . . H23A H 0.7475 1.5750 0.5751 0.058 Uiso 1 1 calc R . . H23B H 0.8462 1.5203 0.5825 0.058 Uiso 1 1 calc R . . H23C H 0.7766 1.4976 0.6527 0.058 Uiso 1 1 calc R . . C22 C 0.7737(4) 1.3489(3) 0.5432(4) 0.0393(13) Uani 1 1 d . . . H22A H 0.7379 1.3055 0.4991 0.059 Uiso 1 1 calc R . . H22B H 0.7700 1.3277 0.6049 0.059 Uiso 1 1 calc R . . H22C H 0.8400 1.3501 0.5350 0.059 Uiso 1 1 calc R . . H2 H 0.705(3) 0.719(3) 0.255(3) 0.008(10) Uiso 1 1 d . . . H19 H 0.346(4) 0.311(4) 0.253(4) 0.033(14) Uiso 1 1 d . . . H11 H 0.440(3) 0.693(3) -0.068(3) 0.015(11) Uiso 1 1 d . . . H12 H 0.466(4) 0.839(4) -0.008(4) 0.043(16) Uiso 1 1 d . . . H8 H 0.528(3) 1.250(4) 0.340(3) 0.029(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01664(9) 0.02023(9) 0.01394(8) 0.00097(6) 0.00089(6) -0.00199(6) C10 0.024(2) 0.023(2) 0.022(2) -0.0067(18) 0.0058(19) -0.0011(18) Pt2 0.01529(9) 0.02024(9) 0.01599(9) -0.00327(6) 0.00027(6) 0.00259(6) N7 0.0179(19) 0.0199(18) 0.0192(18) -0.0018(15) 0.0039(15) 0.0005(14) Cl3 0.0226(6) 0.0385(6) 0.0175(5) -0.0014(5) 0.0027(4) 0.0038(5) N1 0.0190(19) 0.0177(17) 0.0151(17) -0.0023(14) -0.0011(14) -0.0037(14) C12 0.029(3) 0.020(2) 0.028(3) 0.003(2) 0.001(2) 0.0016(18) Cl5 0.0282(6) 0.0246(6) 0.0281(6) -0.0106(5) -0.0004(5) 0.0007(4) C9 0.024(2) 0.022(2) 0.031(3) -0.011(2) 0.004(2) -0.0027(18) Cl1 0.0282(6) 0.0395(7) 0.0154(5) -0.0017(5) 0.0038(4) -0.0043(5) N8 0.0126(17) 0.0194(17) 0.0173(18) -0.0016(14) 0.0000(14) 0.0029(14) Cl2 0.0347(7) 0.0260(6) 0.0250(6) 0.0103(5) 0.0032(5) 0.0029(5) N6 0.021(2) 0.025(2) 0.022(2) -0.0012(16) -0.0019(16) 0.0033(16) C15 0.015(2) 0.019(2) 0.018(2) 0.0000(17) 0.0014(16) 0.0042(16) C16 0.013(2) 0.022(2) 0.018(2) -0.0002(17) 0.0021(16) 0.0000(16) O7 0.0256(18) 0.0265(17) 0.0261(17) 0.0010(14) -0.0018(14) -0.0044(14) C7 0.019(2) 0.022(2) 0.019(2) -0.0014(18) -0.0007(17) -0.0035(17) O5 0.053(2) 0.0293(19) 0.0302(19) -0.0138(16) 0.0041(17) 0.0011(17) N5 0.029(2) 0.023(2) 0.026(2) -0.0032(17) 0.0027(17) 0.0093(17) O2 0.032(2) 0.0236(17) 0.037(2) 0.0008(15) 0.0114(16) -0.0075(14) O6 0.0289(19) 0.041(2) 0.0300(19) -0.0020(16) 0.0113(15) 0.0065(16) O3 0.0236(17) 0.0321(18) 0.0211(17) -0.0043(14) -0.0019(13) 0.0000(14) C6 0.018(2) 0.017(2) 0.016(2) -0.0029(17) 0.0051(16) -0.0047(16) O1 0.053(2) 0.036(2) 0.0165(17) 0.0013(15) 0.0047(16) 0.0077(17) C17 0.017(2) 0.024(2) 0.018(2) -0.0025(18) 0.0031(17) 0.0000(17) C8 0.025(2) 0.019(2) 0.027(2) -0.0005(19) 0.0015(19) 0.0010(18) C4 0.019(2) 0.020(2) 0.017(2) 0.0017(17) 0.0027(17) 0.0009(17) C5 0.010(2) 0.018(2) 0.020(2) -0.0021(17) -0.0001(16) -0.0010(15) C1 0.027(2) 0.015(2) 0.023(2) 0.0006(18) 0.0021(18) -0.0021(17) C13 0.024(2) 0.017(2) 0.031(3) -0.0055(19) -0.0041(19) -0.0015(18) C2 0.034(3) 0.020(2) 0.024(2) -0.008(2) 0.004(2) 0.005(2) N3 0.027(2) 0.026(2) 0.020(2) 0.0008(16) 0.0099(17) 0.0039(16) N4 0.023(2) 0.0233(19) 0.025(2) -0.0011(17) 0.0042(16) 0.0027(16) C3 0.026(2) 0.028(2) 0.017(2) -0.0032(19) 0.0022(18) 0.0038(19) C14 0.017(2) 0.021(2) 0.021(2) -0.0027(18) -0.0021(17) 0.0024(17) O4 0.053(2) 0.0284(19) 0.0305(19) 0.0104(16) 0.0003(17) 0.0104(17) N2 0.0171(18) 0.0171(17) 0.0185(18) -0.0032(15) 0.0021(14) -0.0026(14) O8 0.038(2) 0.045(2) 0.0170(17) -0.0014(15) 0.0011(15) 0.0030(17) N9 0.025(2) 0.0224(19) 0.032(2) 0.0021(17) 0.0055(17) -0.0002(16) O9 0.050(3) 0.040(2) 0.039(2) -0.0051(18) -0.0003(19) -0.0135(18) C19 0.031(3) 0.022(2) 0.032(3) 0.006(2) 0.006(2) 0.000(2) C18 0.022(2) 0.026(2) 0.023(2) 0.0043(19) 0.0047(19) 0.0041(18) C11 0.021(2) 0.025(2) 0.023(2) 0.0019(19) 0.0034(18) 0.0036(18) C20 0.022(2) 0.021(2) 0.028(2) -0.0017(19) 0.0041(19) 0.0028(18) C21 0.027(3) 0.034(3) 0.031(3) 0.003(2) 0.002(2) -0.003(2) C23 0.043(3) 0.035(3) 0.034(3) -0.007(2) -0.003(2) 0.012(2) C22 0.041(3) 0.032(3) 0.049(3) 0.014(3) 0.017(3) 0.006(2) _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 N1 2.004(3) . ? Pt1 N2 2.015(4) . ? Pt1 Cl1 2.2887(11) . ? Pt1 Cl2 2.2947(11) . ? C10 N2 1.343(5) . ? C10 C9 1.375(6) . ? C10 H10A 0.9500 . ? Pt2 N7 2.008(3) . ? Pt2 N8 2.009(4) . ? Pt2 Cl3 2.2874(11) . ? Pt2 Cl5 2.2921(11) . ? N7 C11 1.347(6) . ? N7 C15 1.357(5) . ? N1 C1 1.348(5) . ? N1 C5 1.368(5) . ? C12 C11 1.371(6) . ? C12 C13 1.373(7) . ? C12 H12 0.91(6) . ? C9 C8 1.376(7) . ? C9 H9A 0.9500 . ? N8 C20 1.349(5) . ? N8 C16 1.357(5) . ? N6 O8 1.222(5) . ? N6 O7 1.225(5) . ? N6 C17 1.469(6) . ? C15 C14 1.393(6) . ? C15 C16 1.489(6) . ? C16 C17 1.390(6) . ? C7 C8 1.378(6) . ? C7 C6 1.395(6) . ? C7 N4 1.470(6) . ? O5 N5 1.232(5) . ? N5 O6 1.227(5) . ? N5 C14 1.464(6) . ? O2 N3 1.218(5) . ? O3 N4 1.227(5) . ? C6 N2 1.355(5) . ? C6 C5 1.487(6) . ? O1 N3 1.221(5) . ? C17 C18 1.391(6) . ? C8 H8 0.91(5) . ? C4 C3 1.379(6) . ? C4 C5 1.393(6) . ? C4 N3 1.477(5) . ? C1 C2 1.378(6) . ? C1 H1A 0.9500 . ? C13 C14 1.377(6) . ? C13 H13A 0.9500 . ? C2 C3 1.363(7) . ? C2 H2 0.85(4) . ? N4 O4 1.218(5) . ? C3 H3A 0.9500 . ? N9 C21 1.322(6) . ? N9 C22 1.444(6) . ? N9 C23 1.447(6) . ? O9 C21 1.229(6) . ? C19 C18 1.368(7) . ? C19 C20 1.377(7) . ? C19 H19 0.88(5) . ? C18 H18A 0.9500 . ? C11 H11 0.95(4) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 N1 Pt1 N2 79.56(14) . . ? N1 Pt1 Cl1 175.63(10) . . ? N2 Pt1 Cl1 96.61(10) . . ? N1 Pt1 Cl2 96.37(10) . . ? N2 Pt1 Cl2 174.93(10) . . ? Cl1 Pt1 Cl2 87.57(4) . . ? N2 C10 C9 121.9(4) . . ? N2 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? N7 Pt2 N8 79.92(14) . . ? N7 Pt2 Cl3 96.07(10) . . ? N8 Pt2 Cl3 175.85(10) . . ? N7 Pt2 Cl5 175.89(10) . . ? N8 Pt2 Cl5 96.03(10) . . ? Cl3 Pt2 Cl5 87.99(4) . . ? C11 N7 C15 120.8(4) . . ? C11 N7 Pt2 122.8(3) . . ? C15 N7 Pt2 116.0(3) . . ? C1 N1 C5 120.8(4) . . ? C1 N1 Pt1 122.4(3) . . ? C5 N1 Pt1 116.4(3) . . ? C11 C12 C13 118.1(4) . . ? C11 C12 H12 113(3) . . ? C13 C12 H12 129(3) . . ? C10 C9 C8 118.3(4) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C20 N8 C16 120.4(4) . . ? C20 N8 Pt2 123.5(3) . . ? C16 N8 Pt2 115.7(3) . . ? O8 N6 O7 124.5(4) . . ? O8 N6 C17 118.6(4) . . ? O7 N6 C17 116.9(4) . . ? N7 C15 C14 117.1(4) . . ? N7 C15 C16 113.0(4) . . ? C14 C15 C16 129.8(4) . . ? N8 C16 C17 117.6(4) . . ? N8 C16 C15 113.3(4) . . ? C17 C16 C15 129.1(4) . . ? C8 C7 C6 121.8(4) . . ? C8 C7 N4 115.5(4) . . ? C6 C7 N4 122.2(4) . . ? O6 N5 O5 124.4(4) . . ? O6 N5 C14 117.9(4) . . ? O5 N5 C14 117.7(4) . . ? N2 C6 C7 116.9(4) . . ? N2 C6 C5 113.3(4) . . ? C7 C6 C5 129.9(4) . . ? C16 C17 C18 121.7(4) . . ? C16 C17 N6 123.1(4) . . ? C18 C17 N6 115.0(4) . . ? C9 C8 C7 118.8(4) . . ? C9 C8 H8 125(3) . . ? C7 C8 H8 116(3) . . ? C3 C4 C5 122.2(4) . . ? C3 C4 N3 114.7(4) . . ? C5 C4 N3 122.9(4) . . ? N1 C5 C4 117.0(4) . . ? N1 C5 C6 112.7(4) . . ? C4 C5 C6 130.3(4) . . ? N1 C1 C2 121.9(4) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C12 C13 C14 119.0(4) . . ? C12 C13 H13A 120.5 . . ? C14 C13 H13A 120.5 . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2 125(3) . . ? C1 C2 H2 116(3) . . ? O2 N3 O1 125.3(4) . . ? O2 N3 C4 118.2(4) . . ? O1 N3 C4 116.5(4) . . ? O4 N4 O3 124.7(4) . . ? O4 N4 C7 118.0(4) . . ? O3 N4 C7 117.3(4) . . ? C2 C3 C4 118.7(4) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C13 C14 C15 121.8(4) . . ? C13 C14 N5 115.0(4) . . ? C15 C14 N5 123.0(4) . . ? C10 N2 C6 121.5(4) . . ? C10 N2 Pt1 122.2(3) . . ? C6 N2 Pt1 116.1(3) . . ? C21 N9 C22 122.6(5) . . ? C21 N9 C23 121.3(4) . . ? C22 N9 C23 115.9(4) . . ? C18 C19 C20 118.4(4) . . ? C18 C19 H19 119(3) . . ? C20 C19 H19 122(3) . . ? C19 C18 C17 118.6(4) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? N7 C11 C12 122.4(4) . . ? N7 C11 H11 113(3) . . ? C12 C11 H11 124(3) . . ? N8 C20 C19 122.6(4) . . ? N8 C20 H20A 118.7 . . ? C19 C20 H20A 118.7 . . ? O9 C21 N9 125.8(5) . . ? O9 C21 H21A 117.1 . . ? N9 C21 H21A 117.1 . . ? N9 C23 H23A 109.5 . . ? N9 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N9 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N9 C22 H22A 109.5 . . ? N9 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N9 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 28.86 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.029 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.164 # Validation Reply Form _vrf_PLAT029_I ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.918 RESPONSE: Data/parameter ratio is over 16. Structure was determined at least five years ago, we no longer have the original frames or compound to carry out further data collection. It is very unlikely that the missing data will # significantly change the final refinement result. ;