# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'M. Hosseini' 'Pierre Dechambenoit' 'Sylvie Ferlay' 'Nathalie Kyritsakas' _publ_contact_author_name 'M. Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg 67000 FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_requested_journal 'Chemical Communications' _publ_section_title ; Molecular tectonics: polymorphism and enhancement of networks dimensionality by combination of primary and secondary H-bond sites ; data_e905a _database_code_depnum_ccdc_archive 'CCDC 650826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N4 O2, 2(H2 O), 2(Cl)' _chemical_formula_sum 'C14 H24 Cl2 N4 O4' _chemical_formula_weight 383.27 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' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall '-P 2yn' 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 13.0888(8) _cell_length_b 4.5837(3) _cell_length_c 15.0058(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.515(4) _cell_angle_gamma 90.00 _cell_volume 887.89(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1554 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 23.91 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 0.392 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9222 _exptl_absorpt_correction_T_max 0.9845 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7711 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.62 _reflns_number_total 2038 _reflns_number_gt 1471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0397P)^2^+0.1384P] 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 2038 _refine_ls_number_parameters 118 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 Cl1 Cl 0.48214(3) 0.49404(10) 0.77688(3) 0.02906(14) Uani 1 1 d . . . N1 N 0.24730(10) 0.9060(3) 1.04536(10) 0.0198(3) Uani 1 1 d . . . H1A H 0.2382 0.8434 1.0989 0.024 Uiso 1 1 calc R . . N2 N 0.18639(11) 0.9369(3) 0.89318(10) 0.0213(3) Uani 1 1 d . . . H2 H 0.1347 0.9077 0.8486 0.026 Uiso 1 1 calc R . . C1 C 0.17655(12) 0.8450(3) 0.97454(11) 0.0183(4) Uani 1 1 d . . . C5 C 0.08497(12) 0.6691(3) 0.98742(11) 0.0170(3) Uani 1 1 d . . . C2 C 0.34096(13) 1.0751(4) 1.03780(12) 0.0218(4) Uani 1 1 d . . . H2A H 0.3983 1.0171 1.0862 0.026 Uiso 1 1 calc R . . H2B H 0.3275 1.2859 1.0444 0.026 Uiso 1 1 calc R . . C4 C 0.27897(13) 1.0848(4) 0.87332(12) 0.0228(4) Uani 1 1 d . . . H4A H 0.2670 1.2982 0.8705 0.027 Uiso 1 1 calc R . . H4B H 0.2938 1.0198 0.8139 0.027 Uiso 1 1 calc R . . C6 C 0.05016(13) 0.6703(4) 1.07013(11) 0.0200(4) Uani 1 1 d . . . H6 H 0.0846 0.7872 1.1181 0.024 Uiso 1 1 calc R . . C7 C 0.03408(12) 0.4969(3) 0.91673(11) 0.0190(3) Uani 1 1 d . . . H7 H 0.0573 0.4948 0.8600 0.023 Uiso 1 1 calc R . . C3 C 0.37059(13) 1.0162(3) 0.94606(12) 0.0199(4) Uani 1 1 d . . . H3 H 0.4316 1.1383 0.9376 0.024 Uiso 1 1 calc R . . O1 O 0.39675(9) 0.7154(2) 0.94580(9) 0.0258(3) Uani 1 1 d . . . H1 H 0.4245 0.6787 0.9004 0.039 Uiso 1 1 calc R . . O2 O 0.28659(11) 0.6355(3) 0.21619(9) 0.0292(3) Uani 1 1 d D . . H2C H 0.2595(18) 0.479(4) 0.2296(16) 0.052(8) Uiso 1 1 d D . . H2D H 0.3534(13) 0.606(6) 0.2174(17) 0.068(8) Uiso 1 1 d 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 Cl1 0.0247(2) 0.0416(3) 0.0202(2) -0.00300(19) 0.00183(17) 0.00118(19) N1 0.0178(7) 0.0249(7) 0.0177(7) -0.0008(6) 0.0056(6) -0.0046(6) N2 0.0182(8) 0.0255(8) 0.0196(8) 0.0029(6) 0.0012(6) -0.0041(6) C1 0.0164(8) 0.0176(8) 0.0212(9) -0.0008(6) 0.0037(7) 0.0027(6) C5 0.0136(8) 0.0188(8) 0.0186(9) 0.0020(6) 0.0029(7) 0.0011(6) C2 0.0174(9) 0.0237(9) 0.0240(10) -0.0026(7) 0.0026(7) -0.0055(7) C4 0.0201(9) 0.0245(9) 0.0244(10) 0.0042(7) 0.0059(7) -0.0058(7) C6 0.0174(8) 0.0225(9) 0.0193(9) -0.0027(7) 0.0013(7) -0.0006(7) C7 0.0179(8) 0.0225(8) 0.0174(8) 0.0004(7) 0.0050(7) 0.0001(7) C3 0.0171(8) 0.0185(8) 0.0250(9) 0.0006(7) 0.0059(7) -0.0013(7) O1 0.0274(7) 0.0205(6) 0.0319(7) -0.0004(5) 0.0123(6) 0.0014(5) O2 0.0254(8) 0.0320(8) 0.0305(8) 0.0054(6) 0.0050(6) 0.0025(6) _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 C1 1.319(2) . ? N1 C2 1.471(2) . ? N1 H1A 0.8800 . ? N2 C1 1.318(2) . ? N2 C4 1.462(2) . ? N2 H2 0.8800 . ? C1 C5 1.483(2) . ? C5 C6 1.391(2) . ? C5 C7 1.399(2) . ? C2 C3 1.515(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C4 C3 1.515(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C6 C7 1.383(2) 3_567 ? C6 H6 0.9500 . ? C7 C6 1.383(2) 3_567 ? C7 H7 0.9500 . ? C3 O1 1.4207(19) . ? C3 H3 1.0000 . ? O1 H1 0.8400 . ? O2 H2C 0.838(16) . ? O2 H2D 0.882(16) . ? 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 C1 N1 C2 122.19(14) . . ? C1 N1 H1A 118.9 . . ? C2 N1 H1A 118.9 . . ? C1 N2 C4 123.26(14) . . ? C1 N2 H2 118.4 . . ? C4 N2 H2 118.4 . . ? N2 C1 N1 121.04(15) . . ? N2 C1 C5 119.95(15) . . ? N1 C1 C5 119.01(15) . . ? C6 C5 C7 119.56(15) . . ? C6 C5 C1 120.33(15) . . ? C7 C5 C1 120.09(15) . . ? N1 C2 C3 108.54(13) . . ? N1 C2 H2A 110.0 . . ? C3 C2 H2A 110.0 . . ? N1 C2 H2B 110.0 . . ? C3 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? N2 C4 C3 109.92(13) . . ? N2 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C7 C6 C5 120.75(15) 3_567 . ? C7 C6 H6 119.6 3_567 . ? C5 C6 H6 119.6 . . ? C6 C7 C5 119.69(15) 3_567 . ? C6 C7 H7 120.2 3_567 . ? C5 C7 H7 120.2 . . ? O1 C3 C2 105.87(13) . . ? O1 C3 C4 111.23(14) . . ? C2 C3 C4 109.06(14) . . ? O1 C3 H3 110.2 . . ? C2 C3 H3 110.2 . . ? C4 C3 H3 110.2 . . ? C3 O1 H1 109.5 . . ? H2C O2 H2D 109(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.262 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.056 # Attachment '2-Ni Alpha phase.cif' data_e743a _database_code_depnum_ccdc_archive 'CCDC 650827' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N4 O2, C4 N4 Ni' _chemical_formula_sum 'C18 H20 N8 Ni O2' _chemical_formula_weight 439.13 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' Ni Ni 0.3393 1.1124 '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' H H 0.0000 0.0000 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.6008(4) _cell_length_b 10.3677(10) _cell_length_c 10.6835(10) _cell_angle_alpha 110.610(2) _cell_angle_beta 99.751(2) _cell_angle_gamma 90.156(2) _cell_volume 469.02(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2323 _cell_measurement_theta_min 3.44 _cell_measurement_theta_max 30.80 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 228 _exptl_absorpt_coefficient_mu 1.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8648 _exptl_absorpt_correction_T_max 0.9194 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6277 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 31.06 _reflns_number_total 2973 _reflns_number_gt 2547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0457P)^2^+0.4371P] 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_number_reflns 2973 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 C1 C 0.6942(4) 0.85628(18) 0.74876(18) 0.0126(3) Uani 1 1 d . . . N1 N 0.7203(4) 0.72265(16) 0.71376(16) 0.0137(3) Uani 1 1 d . . . H1A H 0.6677 0.6796 0.7651 0.016 Uiso 1 1 calc R . . C2 C 0.8346(4) 0.64395(18) 0.59156(18) 0.0143(3) Uani 1 1 d . . . H2A H 0.7609 0.5458 0.5593 0.017 Uiso 1 1 calc R . . H2B H 1.0533 0.6487 0.6122 0.017 Uiso 1 1 calc R . . C3 C 0.7330(4) 0.70422(19) 0.48229(18) 0.0139(3) Uani 1 1 d . . . H3 H 0.8168 0.6544 0.3991 0.017 Uiso 1 1 calc R . . O1 O 0.4192(3) 0.68596(16) 0.45225(14) 0.0195(3) Uani 1 1 d . . . H1 H 0.3555 0.7068 0.3838 0.029 Uiso 1 1 calc R . . C4 C 0.8351(5) 0.85657(19) 0.53724(19) 0.0169(4) Uani 1 1 d . . . H4A H 1.0520 0.8667 0.5445 0.020 Uiso 1 1 calc R . . H4B H 0.7410 0.9010 0.4738 0.020 Uiso 1 1 calc R . . N2 N 0.7562(4) 0.92480(16) 0.67154(16) 0.0151(3) Uani 1 1 d . . . H2 H 0.7497 1.0152 0.7022 0.018 Uiso 1 1 calc R . . C5 C 0.5937(4) 0.93158(18) 0.87810(18) 0.0132(3) Uani 1 1 d . . . C6 C 0.4179(4) 1.04292(19) 0.88971(18) 0.0143(3) Uani 1 1 d . . . H6 H 0.3631 1.0720 0.8145 0.017 Uiso 1 1 calc R . . C7 C 0.3231(4) 1.11134(19) 1.01127(18) 0.0148(3) Uani 1 1 d . . . H7 H 0.2022 1.1870 1.0194 0.018 Uiso 1 1 calc R . . Ni1 Ni 1.0000 0.5000 1.0000 0.01448(11) Uani 1 2 d S . . C8 C 0.9067(5) 0.3282(2) 0.8600(2) 0.0165(4) Uani 1 1 d . . . N3 N 0.8485(5) 0.22299(18) 0.77161(18) 0.0232(4) Uani 1 1 d . . . C9 C 0.7724(5) 0.44794(19) 1.1058(2) 0.0184(4) Uani 1 1 d . . . N4 N 0.6272(5) 0.4190(2) 1.17182(19) 0.0254(4) Uani 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 C1 0.0131(8) 0.0115(7) 0.0122(7) 0.0031(6) 0.0023(6) -0.0003(6) N1 0.0171(8) 0.0116(7) 0.0135(7) 0.0042(5) 0.0065(6) 0.0004(5) C2 0.0165(9) 0.0107(7) 0.0149(8) 0.0019(6) 0.0065(6) 0.0013(6) C3 0.0142(8) 0.0144(8) 0.0129(7) 0.0031(6) 0.0059(6) -0.0019(6) O1 0.0153(7) 0.0266(8) 0.0169(6) 0.0090(6) 0.0012(5) -0.0025(5) C4 0.0223(10) 0.0144(8) 0.0158(8) 0.0045(7) 0.0100(7) -0.0023(7) N2 0.0206(8) 0.0103(7) 0.0146(7) 0.0031(6) 0.0066(6) -0.0013(6) C5 0.0144(8) 0.0124(7) 0.0116(7) 0.0022(6) 0.0035(6) -0.0012(6) C6 0.0164(9) 0.0146(8) 0.0120(7) 0.0047(6) 0.0025(6) 0.0004(6) C7 0.0164(9) 0.0135(8) 0.0140(8) 0.0042(6) 0.0032(6) 0.0016(6) Ni1 0.02034(19) 0.01060(16) 0.01271(16) 0.00365(12) 0.00481(12) -0.00407(12) C8 0.0192(9) 0.0149(8) 0.0174(8) 0.0080(7) 0.0035(7) -0.0013(7) N3 0.0340(10) 0.0155(8) 0.0193(8) 0.0063(7) 0.0023(7) -0.0018(7) C9 0.0232(10) 0.0136(8) 0.0169(8) 0.0038(7) 0.0030(7) -0.0031(7) N4 0.0317(11) 0.0234(9) 0.0234(9) 0.0086(7) 0.0109(8) -0.0041(7) _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 C1 N1 1.313(2) . ? C1 N2 1.326(2) . ? C1 C5 1.480(2) . ? N1 C2 1.460(2) . ? N1 H1A 0.8800 . ? C2 C3 1.517(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O1 1.422(2) . ? C3 C4 1.520(3) . ? C3 H3 1.0000 . ? O1 H1 0.8400 . ? C4 N2 1.468(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.393(3) . ? C5 C7 1.400(3) 2_677 ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 C5 1.400(3) 2_677 ? C7 H7 0.9500 . ? Ni1 C9 1.869(2) 2_767 ? Ni1 C9 1.869(2) . ? Ni1 C8 1.870(2) . ? Ni1 C8 1.870(2) 2_767 ? C8 N3 1.158(3) . ? C9 N4 1.158(3) . ? 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 C1 N2 121.69(17) . . ? N1 C1 C5 118.79(16) . . ? N2 C1 C5 119.52(16) . . ? C1 N1 C2 121.42(15) . . ? C1 N1 H1A 119.3 . . ? C2 N1 H1A 119.3 . . ? N1 C2 C3 108.93(15) . . ? N1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? N1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O1 C3 C2 106.58(15) . . ? O1 C3 C4 110.96(16) . . ? C2 C3 C4 108.78(15) . . ? O1 C3 H3 110.2 . . ? C2 C3 H3 110.2 . . ? C4 C3 H3 110.2 . . ? C3 O1 H1 109.5 . . ? N2 C4 C3 110.12(15) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 122.93(16) . . ? C1 N2 H2 118.5 . . ? C4 N2 H2 118.5 . . ? C6 C5 C7 120.38(17) . 2_677 ? C6 C5 C1 120.71(16) . . ? C7 C5 C1 118.91(17) 2_677 . ? C7 C6 C5 119.92(17) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C5 119.70(17) . 2_677 ? C6 C7 H7 120.1 . . ? C5 C7 H7 120.1 2_677 . ? C9 Ni1 C9 179.999(1) 2_767 . ? C9 Ni1 C8 89.28(8) 2_767 . ? C9 Ni1 C8 90.72(8) . . ? C9 Ni1 C8 90.72(8) 2_767 2_767 ? C9 Ni1 C8 89.28(8) . 2_767 ? C8 Ni1 C8 180.000(1) . 2_767 ? N3 C8 Ni1 178.75(17) . . ? N4 C9 Ni1 178.1(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 31.06 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.674 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.104 # Attachment '2-Pd Alpha phase.cif' data_e881a _database_code_depnum_ccdc_archive 'CCDC 650828' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N4 O2, C4 N4 Pd' _chemical_formula_sum 'C18 H20 N8 O2 Pd' _chemical_formula_weight 486.82 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' Pd Pd -0.9988 1.0072 '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' H H 0.0000 0.0000 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.6215(2) _cell_length_b 10.5270(4) _cell_length_c 10.8108(4) _cell_angle_alpha 111.288(2) _cell_angle_beta 99.763(2) _cell_angle_gamma 89.328(2) _cell_volume 482.25(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3141 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 30.05 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 246 _exptl_absorpt_coefficient_mu 0.996 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8732 _exptl_absorpt_correction_T_max 0.9246 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5021 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 29.90 _reflns_number_total 2717 _reflns_number_gt 2657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0457P)^2^+0.0000P] 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_number_reflns 2717 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 C1 C 0.6938(4) 0.85547(18) 0.74919(16) 0.0142(3) Uani 1 1 d . . . N1 N 0.7202(3) 0.72344(16) 0.71402(14) 0.0155(3) Uani 1 1 d . . . H1A H 0.6690 0.6816 0.7648 0.019 Uiso 1 1 calc R . . C2 C 0.8340(4) 0.64421(18) 0.59112(17) 0.0163(3) Uani 1 1 d . . . H2A H 0.7606 0.5476 0.5584 0.020 Uiso 1 1 calc R . . H2B H 1.0515 0.6475 0.6109 0.020 Uiso 1 1 calc R . . C3 C 0.7326(4) 0.70406(19) 0.48435(17) 0.0167(3) Uani 1 1 d . . . H3 H 0.8168 0.6544 0.4015 0.020 Uiso 1 1 calc R . . O1 O 0.4195(3) 0.68673(16) 0.45437(13) 0.0214(3) Uani 1 1 d . . . H1 H 0.3566 0.7047 0.3853 0.032 Uiso 1 1 calc R . . C4 C 0.8325(4) 0.8543(2) 0.53969(18) 0.0192(3) Uani 1 1 d . . . H4A H 1.0481 0.8634 0.5463 0.023 Uiso 1 1 calc R . . H4B H 0.7376 0.8983 0.4775 0.023 Uiso 1 1 calc R . . N2 N 0.7544(4) 0.92298(16) 0.67384(15) 0.0171(3) Uani 1 1 d . . . H2 H 0.7476 1.0125 0.7051 0.021 Uiso 1 1 calc R . . C5 C 0.5934(4) 0.93126(18) 0.87850(16) 0.0145(3) Uani 1 1 d . . . C6 C 0.4183(4) 1.04191(19) 0.89120(17) 0.0165(3) Uani 1 1 d . . . H6 H 0.3629 1.0702 0.8169 0.020 Uiso 1 1 calc R . . C7 C 0.3236(4) 1.11145(19) 1.01266(17) 0.0166(3) Uani 1 1 d . . . H7 H 0.2038 1.1871 1.0216 0.020 Uiso 1 1 calc R . . Pd1 Pd 1.0000 0.5000 1.0000 0.01507(7) Uani 1 2 d S . . C8 C 0.8998(4) 0.3186(2) 0.85094(18) 0.0193(3) Uani 1 1 d . . . N3 N 0.8426(5) 0.21540(18) 0.76391(17) 0.0263(4) Uani 1 1 d . . . C9 C 0.7658(4) 0.44561(19) 1.11382(18) 0.0192(3) Uani 1 1 d . . . N4 N 0.6299(4) 0.4168(2) 1.17999(18) 0.0272(4) Uani 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 C1 0.0145(7) 0.0151(8) 0.0119(6) 0.0036(6) 0.0025(5) 0.0003(6) N1 0.0209(7) 0.0141(7) 0.0136(6) 0.0059(5) 0.0071(5) 0.0022(6) C2 0.0201(8) 0.0124(8) 0.0158(7) 0.0027(6) 0.0074(6) 0.0025(6) C3 0.0191(8) 0.0167(8) 0.0144(7) 0.0045(6) 0.0059(6) 0.0001(6) O1 0.0193(6) 0.0287(8) 0.0177(6) 0.0103(5) 0.0031(5) 0.0002(5) C4 0.0260(9) 0.0182(9) 0.0166(7) 0.0069(7) 0.0112(7) 0.0010(7) N2 0.0250(7) 0.0109(7) 0.0163(6) 0.0041(5) 0.0079(6) 0.0001(6) C5 0.0166(7) 0.0138(8) 0.0123(6) 0.0031(6) 0.0043(6) 0.0002(6) C6 0.0212(8) 0.0157(8) 0.0131(7) 0.0060(6) 0.0023(6) 0.0011(7) C7 0.0201(8) 0.0139(8) 0.0162(7) 0.0057(6) 0.0038(6) 0.0034(6) Pd1 0.02045(11) 0.01187(11) 0.01392(9) 0.00551(7) 0.00386(7) -0.00184(7) C8 0.0257(9) 0.0176(9) 0.0174(7) 0.0096(7) 0.0038(7) 0.0012(7) N3 0.0391(10) 0.0171(8) 0.0232(8) 0.0089(7) 0.0028(7) -0.0006(7) C9 0.0243(9) 0.0152(8) 0.0180(7) 0.0065(7) 0.0025(7) -0.0018(7) N4 0.0329(9) 0.0263(9) 0.0253(8) 0.0109(7) 0.0089(7) -0.0032(7) _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 C1 N1 1.311(2) . ? C1 N2 1.322(2) . ? C1 C5 1.486(2) . ? N1 C2 1.469(2) . ? N1 H1A 0.8800 . ? C2 C3 1.512(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O1 1.427(2) . ? C3 C4 1.520(3) . ? C3 H3 1.0000 . ? O1 H1 0.8400 . ? C4 N2 1.472(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.389(3) . ? C5 C7 1.400(2) 2_677 ? C6 C7 1.393(2) . ? C6 H6 0.9500 . ? C7 C5 1.400(2) 2_677 ? C7 H7 0.9500 . ? Pd1 C8 1.9976(19) . ? Pd1 C8 1.9976(19) 2_767 ? Pd1 C9 1.9978(19) . ? Pd1 C9 1.9979(19) 2_767 ? C8 N3 1.147(3) . ? C9 N4 1.145(3) . ? 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 C1 N2 122.25(15) . . ? N1 C1 C5 118.57(15) . . ? N2 C1 C5 119.18(16) . . ? C1 N1 C2 121.08(15) . . ? C1 N1 H1A 119.5 . . ? C2 N1 H1A 119.5 . . ? N1 C2 C3 108.96(14) . . ? N1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? N1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O1 C3 C2 106.59(15) . . ? O1 C3 C4 111.10(15) . . ? C2 C3 C4 109.01(15) . . ? O1 C3 H3 110.0 . . ? C2 C3 H3 110.0 . . ? C4 C3 H3 110.0 . . ? C3 O1 H1 109.5 . . ? N2 C4 C3 110.27(14) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 122.59(16) . . ? C1 N2 H2 118.7 . . ? C4 N2 H2 118.7 . . ? C6 C5 C7 120.44(15) . 2_677 ? C6 C5 C1 120.73(15) . . ? C7 C5 C1 118.82(16) 2_677 . ? C5 C6 C7 120.18(16) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C5 119.37(16) . 2_677 ? C6 C7 H7 120.3 . . ? C5 C7 H7 120.3 2_677 . ? C8 Pd1 C8 180.000(1) . 2_767 ? C8 Pd1 C9 90.61(8) . . ? C8 Pd1 C9 89.39(7) 2_767 . ? C8 Pd1 C9 89.39(7) . 2_767 ? C8 Pd1 C9 90.61(8) 2_767 2_767 ? C9 Pd1 C9 179.999(1) . 2_767 ? N3 C8 Pd1 178.93(17) . . ? N4 C9 Pd1 178.75(18) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.90 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.552 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.082 # Attachment '2-Pt Alpha phase.cif' data_e885a _database_code_depnum_ccdc_archive 'CCDC 650829' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N4 O2, C4 N4 Pt' _chemical_formula_sum 'C18 H20 N8 O2 Pt' _chemical_formula_weight 575.51 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' Pt Pt -1.7033 8.3905 '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' H H 0.0000 0.0000 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.6482(2) _cell_length_b 10.4381(5) _cell_length_c 10.8458(4) _cell_angle_alpha 111.0191(10) _cell_angle_beta 99.3081(10) _cell_angle_gamma 88.850(2) _cell_volume 484.32(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6959 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 29.88 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 278 _exptl_absorpt_coefficient_mu 7.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5298 _exptl_absorpt_correction_T_max 0.6693 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10251 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 30.04 _reflns_number_total 2810 _reflns_number_gt 2809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^+0.0000P] 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_number_reflns 2810 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0176 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0385 _refine_ls_wR_factor_gt 0.0385 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 C1 C 0.6908(5) 0.8553(2) 0.7491(2) 0.0154(4) Uani 1 1 d . . . N1 N 0.7148(4) 0.7225(2) 0.71254(17) 0.0161(4) Uani 1 1 d . . . H1A H 0.6612 0.6797 0.7624 0.019 Uiso 1 1 calc R . . C2 C 0.8292(5) 0.6430(2) 0.5902(2) 0.0166(4) Uani 1 1 d . . . H2A H 0.7558 0.5463 0.5572 0.020 Uiso 1 1 calc R . . H2B H 1.0450 0.6448 0.6092 0.020 Uiso 1 1 calc R . . C3 C 0.7305(5) 0.7058(2) 0.4853(2) 0.0167(4) Uani 1 1 d . . . H3 H 0.8145 0.6561 0.4024 0.020 Uiso 1 1 calc R . . O1 O 0.4195(3) 0.6908(2) 0.45661(16) 0.0226(4) Uani 1 1 d . . . H1 H 0.3589 0.7046 0.3853 0.034 Uiso 1 1 calc R . . C4 C 0.8298(5) 0.8557(3) 0.5405(2) 0.0194(5) Uani 1 1 d . . . H4A H 1.0438 0.8634 0.5459 0.023 Uiso 1 1 calc R . . H4B H 0.7361 0.9015 0.4797 0.023 Uiso 1 1 calc R . . N2 N 0.7525(4) 0.9240(2) 0.67472(18) 0.0175(4) Uani 1 1 d . . . H2 H 0.7473 1.0142 0.7066 0.021 Uiso 1 1 calc R . . C5 C 0.5916(5) 0.9313(2) 0.8786(2) 0.0147(4) Uani 1 1 d . . . C6 C 0.4177(5) 1.0440(2) 0.8927(2) 0.0167(4) Uani 1 1 d . . . H6 H 0.3620 1.0737 0.8194 0.020 Uiso 1 1 calc R . . C7 C 0.3257(5) 1.1128(2) 1.0142(2) 0.0172(4) Uani 1 1 d . . . H7 H 0.2067 1.1898 1.0243 0.021 Uiso 1 1 calc R . . Pt1 Pt 1.0000 0.5000 1.0000 0.01430(4) Uani 1 2 d S . . C8 C 0.8938(5) 0.3214(3) 0.8521(2) 0.0195(5) Uani 1 1 d . . . N3 N 0.8347(5) 0.2182(2) 0.7645(2) 0.0266(5) Uani 1 1 d . . . C9 C 0.7734(5) 0.4459(2) 1.1158(2) 0.0186(4) Uani 1 1 d . . . N4 N 0.6441(5) 0.4167(2) 1.1841(2) 0.0269(5) Uani 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 C1 0.0153(9) 0.0154(12) 0.0136(9) 0.0033(8) 0.0019(7) 0.0004(8) N1 0.0218(9) 0.0136(10) 0.0142(8) 0.0049(7) 0.0069(7) 0.0025(7) C2 0.0197(10) 0.0135(12) 0.0159(9) 0.0028(8) 0.0073(8) 0.0028(8) C3 0.0189(10) 0.0162(12) 0.0147(9) 0.0032(8) 0.0073(7) 0.0006(8) O1 0.0178(8) 0.0313(11) 0.0188(7) 0.0096(7) 0.0023(6) -0.0006(7) C4 0.0253(11) 0.0171(12) 0.0177(10) 0.0054(9) 0.0107(8) 0.0003(9) N2 0.0255(10) 0.0108(10) 0.0157(8) 0.0024(7) 0.0073(7) 0.0003(8) C5 0.0176(10) 0.0122(11) 0.0121(8) 0.0012(8) 0.0034(7) -0.0009(8) C6 0.0204(10) 0.0158(12) 0.0140(9) 0.0054(8) 0.0030(7) 0.0027(8) C7 0.0206(10) 0.0143(12) 0.0160(9) 0.0043(8) 0.0042(8) 0.0041(9) Pt1 0.01888(6) 0.01191(7) 0.01273(5) 0.00506(4) 0.00273(4) -0.00082(4) C8 0.0248(11) 0.0189(13) 0.0184(10) 0.0112(9) 0.0029(8) 0.0004(9) N3 0.0382(12) 0.0173(12) 0.0227(10) 0.0065(9) 0.0018(8) -0.0025(9) C9 0.0221(11) 0.0151(12) 0.0175(9) 0.0049(9) 0.0023(8) -0.0016(9) N4 0.0327(11) 0.0261(13) 0.0241(10) 0.0103(9) 0.0070(8) -0.0032(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 C1 N1 1.306(3) . ? C1 N2 1.322(3) . ? C1 C5 1.487(3) . ? N1 C2 1.467(3) . ? N1 H1A 0.8800 . ? C2 C3 1.513(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O1 1.428(3) . ? C3 C4 1.512(3) . ? C3 H3 1.0000 . ? O1 H1 0.8400 . ? C4 N2 1.473(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C7 1.394(3) 2_677 ? C5 C6 1.390(3) . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 C5 1.394(3) 2_677 ? C7 H7 0.9500 . ? Pt1 C8 1.982(3) . ? Pt1 C8 1.982(3) 2_767 ? Pt1 C9 1.992(2) 2_767 ? Pt1 C9 1.992(2) . ? C8 N3 1.154(3) . ? C9 N4 1.147(3) . ? 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 C1 N2 122.0(2) . . ? N1 C1 C5 118.87(19) . . ? N2 C1 C5 119.1(2) . . ? C1 N1 C2 121.43(19) . . ? C1 N1 H1A 119.3 . . ? C2 N1 H1A 119.3 . . ? N1 C2 C3 108.66(18) . . ? N1 C2 H2A 110.0 . . ? C3 C2 H2A 110.0 . . ? N1 C2 H2B 110.0 . . ? C3 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? O1 C3 C2 106.60(17) . . ? O1 C3 C4 111.00(19) . . ? C2 C3 C4 109.13(18) . . ? O1 C3 H3 110.0 . . ? C2 C3 H3 110.0 . . ? C4 C3 H3 110.0 . . ? C3 O1 H1 109.5 . . ? N2 C4 C3 110.34(18) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 122.6(2) . . ? C1 N2 H2 118.7 . . ? C4 N2 H2 118.7 . . ? C7 C5 C6 120.40(19) 2_677 . ? C7 C5 C1 118.9(2) 2_677 . ? C6 C5 C1 120.69(19) . . ? C7 C6 C5 119.74(19) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C5 119.9(2) . 2_677 ? C6 C7 H7 120.1 . . ? C5 C7 H7 120.1 2_677 . ? C8 Pt1 C8 180.000(2) . 2_767 ? C8 Pt1 C9 89.19(9) . 2_767 ? C8 Pt1 C9 90.81(9) 2_767 2_767 ? C8 Pt1 C9 90.82(9) . . ? C8 Pt1 C9 89.19(9) 2_767 . ? C9 Pt1 C9 179.999(1) 2_767 . ? N3 C8 Pt1 178.8(2) . . ? N4 C9 Pt1 178.9(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.569 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.123 # Attachment '2-Pt beta phase.cif' data_e811a _database_code_depnum_ccdc_archive 'CCDC 650830' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N4 O2, C4 N4 Pt' _chemical_formula_sum 'C18 H20 N8 O2 Pt' _chemical_formula_weight 575.51 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0141(3) _cell_length_b 10.7311(4) _cell_length_c 10.7497(4) _cell_angle_alpha 67.893(2) _cell_angle_beta 69.080(2) _cell_angle_gamma 69.861(2) _cell_volume 969.85(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3138 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 7.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4759 _exptl_absorpt_correction_T_max 0.5302 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18020 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.11 _reflns_number_total 5654 _reflns_number_gt 3297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0274P)^2^+0.0000P] 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_number_reflns 5654 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _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 C1 C 0.3366(6) 0.2533(6) 0.3484(6) 0.0147(12) Uani 1 1 d . . . N1 N 0.1947(5) 0.2980(5) 0.4060(5) 0.0172(11) Uani 1 1 d . . . H1A H 0.1518 0.2513 0.4894 0.021 Uiso 1 1 calc R . . C2 C 0.1108(6) 0.4266(6) 0.3284(6) 0.0196(13) Uani 1 1 d . . . H2A H 0.0198 0.4645 0.3926 0.023 Uiso 1 1 calc R . . H2B H 0.0827 0.4084 0.2586 0.023 Uiso 1 1 calc R . . C3 C 0.2054(6) 0.5280(6) 0.2577(6) 0.0221(14) Uani 1 1 d . . . H3 H 0.1488 0.6180 0.2070 0.027 Uiso 1 1 calc R . . O1 O 0.2439(5) 0.5478(5) 0.3615(5) 0.0314(11) Uani 1 1 d . . . H1 H 0.2828 0.6155 0.3269 0.047 Uiso 1 1 calc R . . C4 C 0.3412(7) 0.4701(7) 0.1551(7) 0.0266(15) Uani 1 1 d . . . H4A H 0.3138 0.4734 0.0739 0.032 Uiso 1 1 calc R . . H4B H 0.4144 0.5260 0.1217 0.032 Uiso 1 1 calc R . . N2 N 0.4041(5) 0.3257(5) 0.2268(5) 0.0188(11) Uani 1 1 d . . . H2C H 0.4930 0.2851 0.1857 0.023 Uiso 1 1 calc R . . C5 C 0.4212(6) 0.1229(6) 0.4258(6) 0.0159(12) Uani 1 1 d . . . C6 C 0.3518(6) 0.0170(6) 0.5174(6) 0.0151(12) Uani 1 1 d . . . H6 H 0.2499 0.0296 0.5289 0.018 Uiso 1 1 calc R . . C7 C 0.5717(6) 0.1048(6) 0.4091(6) 0.0159(12) Uani 1 1 d . . . H7 H 0.6201 0.1760 0.3475 0.019 Uiso 1 1 calc R . . C8 C 0.2532(6) 0.3401(6) 0.8447(6) 0.0138(12) Uani 1 1 d . . . N3 N 0.2979(5) 0.2066(6) 0.9013(6) 0.0188(11) Uani 1 1 d . . . H3A H 0.2565 0.1687 0.9890 0.023 Uiso 1 1 calc R . . C9 C 0.4157(6) 0.1200(6) 0.8198(6) 0.0180(13) Uani 1 1 d . . . H9A H 0.3740 0.0893 0.7687 0.022 Uiso 1 1 calc R . . H9B H 0.4654 0.0366 0.8825 0.022 Uiso 1 1 calc R . . C10 C 0.5254(6) 0.2032(6) 0.7185(6) 0.0180(12) Uani 1 1 d . . . H10 H 0.6009 0.1474 0.6567 0.022 Uiso 1 1 calc R . . O2 O 0.5972(5) 0.2382(5) 0.7889(5) 0.0272(10) Uani 1 1 d . . . H2 H 0.6629 0.1690 0.8159 0.041 Uiso 1 1 calc R . . C11 C 0.4495(6) 0.3353(6) 0.6309(6) 0.0235(14) Uani 1 1 d . . . H11A H 0.5178 0.3970 0.5787 0.028 Uiso 1 1 calc R . . H11B H 0.4211 0.3148 0.5627 0.028 Uiso 1 1 calc R . . N4 N 0.3172(5) 0.4056(5) 0.7186(5) 0.0197(11) Uani 1 1 d . . . H4 H 0.2797 0.4946 0.6850 0.024 Uiso 1 1 calc R . . C12 C 0.1232(6) 0.4237(6) 0.9262(6) 0.0140(11) Uani 1 1 d . . . C13 C 0.0072(6) 0.3632(6) 1.0133(6) 0.0167(12) Uani 1 1 d . . . H13 H 0.0129 0.2700 1.0226 0.020 Uiso 1 1 calc R . . C14 C -0.1178(6) 0.4402(6) 1.0872(6) 0.0154(12) Uani 1 1 d . . . H14 H -0.1984 0.4004 1.1459 0.018 Uiso 1 1 calc R . . Pt1 Pt 0.0000 0.0000 0.5000 0.01376(10) Uani 1 2 d S . . C15 C 0.1285(6) 0.0392(6) 0.3044(6) 0.0200(13) Uani 1 1 d . . . N5 N 0.2023(5) 0.0627(6) 0.1939(6) 0.0255(12) Uani 1 1 d . . . C16 C -0.1297(6) 0.1916(6) 0.4480(6) 0.0180(12) Uani 1 1 d . . . N6 N -0.2057(5) 0.2988(6) 0.4171(5) 0.0234(12) Uani 1 1 d . . . Pt2 Pt 1.0000 0.0000 0.0000 0.01498(11) Uani 1 2 d S . . C17 C 0.9461(6) -0.1279(6) 0.1910(6) 0.0178(12) Uani 1 1 d . . . N7 N 0.9107(6) -0.2003(6) 0.2996(5) 0.0300(14) Uani 1 1 d . . . C18 C 0.8062(6) 0.1352(6) 0.0419(6) 0.0181(12) Uani 1 1 d . . . N8 N 0.6965(5) 0.2117(6) 0.0694(5) 0.0267(13) Uani 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 C1 0.017(3) 0.014(3) 0.013(3) -0.003(2) -0.006(2) -0.002(2) N1 0.011(2) 0.018(3) 0.014(2) -0.002(2) 0.0016(19) -0.001(2) C2 0.020(3) 0.016(3) 0.018(3) -0.005(2) -0.006(2) 0.002(2) C3 0.017(3) 0.014(3) 0.026(3) -0.001(3) -0.008(2) 0.004(2) O1 0.033(3) 0.025(3) 0.040(3) -0.011(2) -0.010(2) -0.010(2) C4 0.022(3) 0.020(3) 0.021(3) 0.006(3) -0.001(3) -0.002(3) N2 0.016(3) 0.015(3) 0.014(3) 0.000(2) 0.001(2) 0.000(2) C5 0.016(3) 0.015(3) 0.010(3) -0.002(2) -0.004(2) 0.002(2) C6 0.011(3) 0.017(3) 0.019(3) -0.005(2) -0.006(2) -0.002(2) C7 0.019(3) 0.010(3) 0.015(3) 0.000(2) -0.004(2) -0.003(2) C8 0.008(3) 0.016(3) 0.014(3) -0.007(2) -0.002(2) 0.002(2) N3 0.016(3) 0.018(3) 0.017(3) -0.004(2) -0.002(2) -0.001(2) C9 0.012(3) 0.009(3) 0.024(3) -0.005(2) 0.000(2) 0.003(2) C10 0.017(3) 0.012(3) 0.016(3) -0.002(2) -0.002(2) 0.000(2) O2 0.021(2) 0.026(3) 0.035(3) -0.004(2) -0.013(2) -0.005(2) C11 0.019(3) 0.021(3) 0.017(3) -0.007(3) 0.001(2) 0.006(3) N4 0.017(3) 0.013(3) 0.020(3) -0.004(2) -0.002(2) 0.003(2) C12 0.013(3) 0.014(3) 0.010(3) -0.003(2) 0.000(2) -0.002(2) C13 0.018(3) 0.015(3) 0.018(3) -0.007(2) -0.004(2) -0.002(2) C14 0.014(3) 0.018(3) 0.013(3) -0.004(2) -0.001(2) -0.007(2) Pt1 0.0116(2) 0.0129(2) 0.0129(2) -0.00116(18) -0.00201(17) -0.00244(17) C15 0.016(3) 0.016(3) 0.019(3) 0.001(2) -0.004(2) 0.001(2) N5 0.017(3) 0.026(3) 0.023(3) -0.002(2) -0.005(2) 0.001(2) C16 0.018(3) 0.018(3) 0.011(3) -0.001(2) 0.005(2) -0.009(2) N6 0.019(3) 0.020(3) 0.023(3) -0.004(2) -0.001(2) -0.003(2) Pt2 0.0121(2) 0.0151(2) 0.0132(2) -0.00333(19) 0.00028(17) -0.00247(18) C17 0.011(3) 0.014(3) 0.020(3) -0.005(2) -0.002(2) 0.004(2) N7 0.024(3) 0.029(3) 0.017(3) -0.005(2) 0.004(2) 0.006(2) C18 0.015(3) 0.016(3) 0.014(3) 0.001(2) 0.001(2) -0.005(2) N8 0.020(3) 0.026(3) 0.021(3) -0.005(2) 0.003(2) -0.001(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 C1 N2 1.318(8) . ? C1 N1 1.326(7) . ? C1 C5 1.476(8) . ? N1 C2 1.463(7) . ? N1 H1A 0.8800 . ? C2 C3 1.493(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O1 1.408(7) . ? C3 C4 1.521(8) . ? C3 H3 1.0000 . ? O1 H1 0.8400 . ? C4 N2 1.472(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2C 0.8800 . ? C5 C6 1.399(8) . ? C5 C7 1.404(7) . ? C6 C7 1.373(7) 2_656 ? C6 H6 0.9500 . ? C7 C6 1.373(7) 2_656 ? C7 H7 0.9500 . ? C8 N4 1.309(8) . ? C8 N3 1.312(7) . ? C8 C12 1.497(7) . ? N3 C9 1.464(6) . ? N3 H3A 0.8800 . ? C9 C10 1.510(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O2 1.421(7) . ? C10 C11 1.496(8) . ? C10 H10 1.0000 . ? O2 H2 0.8400 . ? C11 N4 1.473(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N4 H4 0.8800 . ? C12 C13 1.391(8) . ? C12 C14 1.397(8) 2_567 ? C13 C14 1.397(7) . ? C13 H13 0.9500 . ? C14 C12 1.397(8) 2_567 ? C14 H14 0.9500 . ? Pt1 C15 2.007(6) 2_556 ? Pt1 C15 2.007(6) . ? Pt1 C16 2.010(6) . ? Pt1 C16 2.010(6) 2_556 ? C15 N5 1.139(8) . ? C16 N6 1.142(7) . ? Pt2 C17 1.997(6) . ? Pt2 C17 1.997(6) 2_755 ? Pt2 C18 2.001(5) . ? Pt2 C18 2.001(5) 2_755 ? C17 N7 1.142(8) . ? C18 N8 1.139(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 121.3(5) . . ? N2 C1 C5 119.7(5) . . ? N1 C1 C5 118.9(6) . . ? C1 N1 C2 118.8(5) . . ? C1 N1 H1A 120.6 . . ? C2 N1 H1A 120.6 . . ? N1 C2 C3 108.2(5) . . ? N1 C2 H2A 110.0 . . ? C3 C2 H2A 110.0 . . ? N1 C2 H2B 110.0 . . ? C3 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? O1 C3 C2 107.5(5) . . ? O1 C3 C4 111.4(5) . . ? C2 C3 C4 109.0(5) . . ? O1 C3 H3 109.6 . . ? C2 C3 H3 109.6 . . ? C4 C3 H3 109.6 . . ? C3 O1 H1 109.5 . . ? N2 C4 C3 108.2(5) . . ? N2 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? N2 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C1 N2 C4 124.5(5) . . ? C1 N2 H2C 117.8 . . ? C4 N2 H2C 117.8 . . ? C6 C5 C7 119.5(5) . . ? C6 C5 C1 120.2(5) . . ? C7 C5 C1 120.2(6) . . ? C7 C6 C5 121.2(5) 2_656 . ? C7 C6 H6 119.4 2_656 . ? C5 C6 H6 119.4 . . ? C6 C7 C5 119.3(6) 2_656 . ? C6 C7 H7 120.3 2_656 . ? C5 C7 H7 120.3 . . ? N4 C8 N3 123.1(5) . . ? N4 C8 C12 117.5(5) . . ? N3 C8 C12 119.4(5) . . ? C8 N3 C9 120.6(5) . . ? C8 N3 H3A 119.7 . . ? C9 N3 H3A 119.7 . . ? N3 C9 C10 108.9(5) . . ? N3 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N3 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O2 C10 C11 107.9(5) . . ? O2 C10 C9 111.3(5) . . ? C11 C10 C9 110.4(5) . . ? O2 C10 H10 109.1 . . ? C11 C10 H10 109.1 . . ? C9 C10 H10 109.1 . . ? C10 O2 H2 109.5 . . ? N4 C11 C10 110.4(5) . . ? N4 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? N4 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C8 N4 C11 122.3(5) . . ? C8 N4 H4 118.9 . . ? C11 N4 H4 118.9 . . ? C13 C12 C14 121.1(5) . 2_567 ? C13 C12 C8 118.3(5) . . ? C14 C12 C8 120.6(5) 2_567 . ? C12 C13 C14 119.6(5) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C12 C14 C13 119.3(5) 2_567 . ? C12 C14 H14 120.3 2_567 . ? C13 C14 H14 120.3 . . ? C15 Pt1 C15 180.0 2_556 . ? C15 Pt1 C16 91.3(2) 2_556 . ? C15 Pt1 C16 88.7(2) . . ? C15 Pt1 C16 88.7(2) 2_556 2_556 ? C15 Pt1 C16 91.3(2) . 2_556 ? C16 Pt1 C16 180.0 . 2_556 ? N5 C15 Pt1 178.9(6) . . ? N6 C16 Pt1 177.9(6) . . ? C17 Pt2 C17 180.0 . 2_755 ? C17 Pt2 C18 89.9(2) . . ? C17 Pt2 C18 90.1(2) 2_755 . ? C17 Pt2 C18 90.1(2) . 2_755 ? C17 Pt2 C18 89.9(2) 2_755 2_755 ? C18 Pt2 C18 180.000(1) . 2_755 ? N7 C17 Pt2 177.7(6) . . ? N8 C18 Pt2 177.9(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.226 _refine_diff_density_min -1.867 _refine_diff_density_rms 0.225