Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name I.Goldberg _publ_contact_author_address ; School of Chemistry Tel Aviv University Ramat Aviv Tel Aviv 69978 ISRAEL ; _publ_contact_author_email GOLDBERG@POST.TAU.AC.IL _publ_section_title ; Self-assembly of uniquely structured porphyrin network solids by charged N-H***Cl and N-H***O hydrogen bonds ; loop_ _publ_author_name I.Goldberg 'Sumod George' 'Sophia Lipstman' 'Sankar Muniappan' # Attachment 'sg347fin.cif' data_Compound-I _database_code_depnum_ccdc_archive 'CCDC 612488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H30 N8, 2Cl, 2(I3)' _chemical_formula_sum 'C40 H30 Cl2 I6 N8' _chemical_formula_weight 1455.02 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' I I -0.4742 1.8119 '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 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x, y, -z' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 14.4525(4) _cell_length_b 20.8624(7) _cell_length_c 7.8359(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.1133(17) _cell_angle_gamma 90.00 _cell_volume 2232.39(11) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2554 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 28.28 _exptl_crystal_description plates _exptl_crystal_colour violet _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 4.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4105 _exptl_absorpt_correction_T_max 0.6711 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9878 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 28.20 _reflns_number_total 2764 _reflns_number_gt 2023 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0919P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00016(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2764 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_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_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 0.45005(10) 0.13809(7) 0.10428(17) 0.0305(4) Uani 1 1 d . . . C2 C 0.40523(10) 0.16772(7) 0.22152(19) 0.0356(4) Uani 1 1 d . . . H2 H 0.4027 0.2124 0.2429 0.043 Uiso 1 1 calc R . . C3 C 0.36678(10) 0.12033(7) 0.29721(18) 0.0337(4) Uani 1 1 d . . . H3 H 0.3319 0.1257 0.3801 0.040 Uiso 1 1 calc R . . C4 C 0.38909(9) 0.06041(7) 0.22756(17) 0.0286(4) Uani 1 1 d . . . N5 N 0.44102(7) 0.07269(6) 0.11221(15) 0.0299(3) Uani 1 1 d . . . H5 H 0.4642 0.0440 0.0543 0.036 Uiso 0.50 1 calc PR . . C6 C 0.36432(12) 0.0000 0.2798(2) 0.0286(5) Uani 1 2 d S . . C7 C 0.30437(12) 0.0000 0.4019(3) 0.0290(5) Uani 1 2 d S . . C8 C 0.20476(13) 0.0000 0.3351(3) 0.0327(6) Uani 1 2 d S . . H8 H 0.1723 0.0000 0.2083 0.039 Uiso 1 2 calc SR . . C9 C 0.15089(13) 0.0000 0.4522(3) 0.0340(6) Uani 1 2 d S . . H9 H 0.0814 0.0000 0.4061 0.041 Uiso 1 2 calc SR . . N10 N 0.19734(11) 0.0000 0.6313(2) 0.0367(5) Uani 1 2 d S . . H10 H 0.1649(16) 0.0000 0.706(3) 0.044 Uiso 1 2 d S . . C11 C 0.29535(16) 0.0000 0.7036(3) 0.0468(7) Uani 1 2 d S . . H11 H 0.3260 0.0000 0.8309 0.056 Uiso 1 2 calc SR . . C12 C 0.35107(14) 0.0000 0.5890(3) 0.0388(6) Uani 1 2 d S . . H12 H 0.4205 0.0000 0.6375 0.047 Uiso 1 2 calc SR . . C13 C 0.5000 0.16963(9) 0.0000 0.0297(5) Uani 1 2 d S . . C14 C 0.5000 0.24110(9) 0.0000 0.0270(5) Uani 1 2 d S . . C15 C 0.41285(10) 0.27567(8) -0.03759(18) 0.0342(4) Uani 1 1 d . . . H15 H 0.3522 0.2536 -0.0655 0.041 Uiso 1 1 calc R . . C16 C 0.41470(11) 0.34188(8) -0.0343(2) 0.0392(4) Uani 1 1 d . . . H16 H 0.3558 0.3656 -0.0563 0.047 Uiso 1 1 calc R . . N17 N 0.5000 0.37216(9) 0.0000 0.0382(5) Uani 1 2 d S . . H17 H 0.5000 0.4136(12) 0.0000 0.046 Uiso 1 2 d S . . I18 I 0.0000 0.165305(6) 0.5000 0.03637(4) Uani 1 2 d S . . I19 I 0.212955(8) 0.169404(6) 0.653308(17) 0.05265(4) Uani 1 1 d . . . Cl20 Cl 0.07996(3) 0.0000 0.87726(6) 0.03554(13) Uani 1 2 d S . . 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 0.0392(6) 0.0197(6) 0.0350(6) -0.0012(5) 0.0153(5) -0.0034(5) C2 0.0505(7) 0.0190(7) 0.0452(7) -0.0007(5) 0.0263(5) 0.0011(5) C3 0.0429(6) 0.0232(7) 0.0412(6) -0.0019(6) 0.0221(5) 0.0026(5) C4 0.0349(5) 0.0202(6) 0.0333(6) -0.0032(5) 0.0146(4) -0.0009(5) N5 0.0358(5) 0.0201(5) 0.0356(5) 0.0007(5) 0.0144(4) -0.0021(4) C6 0.0267(7) 0.0276(9) 0.0308(8) 0.000 0.0086(6) 0.000 C7 0.0378(7) 0.0096(7) 0.0493(8) 0.000 0.0273(6) 0.000 C8 0.0242(7) 0.0334(11) 0.0400(9) 0.000 0.0097(7) 0.000 C9 0.0298(8) 0.0330(11) 0.0420(9) 0.000 0.0157(7) 0.000 N10 0.0463(7) 0.0313(9) 0.0440(7) 0.000 0.0304(5) 0.000 C11 0.0466(10) 0.0605(15) 0.0365(9) 0.000 0.0180(7) 0.000 C12 0.0331(8) 0.0525(13) 0.0307(9) 0.000 0.0104(7) 0.000 C13 0.0357(8) 0.0158(9) 0.0399(9) 0.000 0.0155(7) 0.000 C14 0.0408(8) 0.0124(8) 0.0328(7) 0.000 0.0187(6) 0.000 C15 0.0399(6) 0.0250(7) 0.0377(6) -0.0020(6) 0.0126(5) 0.0014(6) C16 0.0464(7) 0.0231(7) 0.0485(7) 0.0000(6) 0.0162(6) 0.0058(6) N17 0.0526(9) 0.0207(8) 0.0402(8) 0.000 0.0135(7) 0.000 I18 0.04868(6) 0.02356(6) 0.04122(6) 0.000 0.02065(5) 0.000 I19 0.04802(5) 0.03843(6) 0.07469(7) -0.01888(5) 0.02443(5) -0.00375(4) Cl20 0.0491(2) 0.0259(2) 0.03881(19) 0.000 0.02425(16) 0.000 _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 N5 1.3739(18) . ? C1 C13 1.4172(17) . ? C1 C2 1.427(2) . ? C2 C3 1.362(2) . ? C2 H2 0.9500 . ? C3 C4 1.442(2) . ? C3 H3 0.9500 . ? C4 N5 1.375(2) . ? C4 C6 1.4072(17) . ? N5 H5 0.8800 . ? C6 C4 1.4072(17) 2 ? C6 C7 1.486(3) . ? C7 C8 1.361(2) . ? C7 C12 1.399(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 N10 1.342(2) . ? C9 H9 0.9500 . ? N10 C11 1.342(3) . ? N10 H10 0.86(3) . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C1 1.4173(17) 6_655 ? C13 C14 1.491(3) . ? C14 C15 1.3966(17) 6_655 ? C14 C15 1.3966(17) . ? C15 C16 1.382(2) . ? C15 H15 0.9500 . ? C16 N17 1.3319(18) . ? C16 H16 0.9500 . ? N17 C16 1.3319(18) 6_655 ? N17 H17 0.86(3) . ? I18 I19 2.91571(14) 6_556 ? I18 I19 2.91575(14) . ? 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 N5 C1 C13 124.13(14) . . ? N5 C1 C2 109.36(13) . . ? C13 C1 C2 126.47(13) . . ? C3 C2 C1 107.57(13) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? C2 C3 C4 106.91(14) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N5 C4 C6 127.15(14) . . ? N5 C4 C3 108.96(12) . . ? C6 C4 C3 123.82(15) . . ? C1 N5 C4 107.16(12) . . ? C1 N5 H5 126.4 . . ? C4 N5 H5 126.4 . . ? C4 C6 C4 127.2(2) . 2 ? C4 C6 C7 116.41(10) . . ? C4 C6 C7 116.41(10) 2 . ? C8 C7 C12 119.3(2) . . ? C8 C7 C6 121.23(17) . . ? C12 C7 C6 119.46(16) . . ? C7 C8 C9 119.90(18) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? N10 C9 C8 119.70(17) . . ? N10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 N10 C9 122.6(2) . . ? C11 N10 H10 116.5(13) . . ? C9 N10 H10 120.9(13) . . ? N10 C11 C12 118.83(19) . . ? N10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C11 C12 C7 119.65(18) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C1 C13 C1 124.66(17) . 6_655 ? C1 C13 C14 117.67(9) . . ? C1 C13 C14 117.67(9) 6_655 . ? C15 C14 C15 117.82(18) 6_655 . ? C15 C14 C13 121.09(9) 6_655 . ? C15 C14 C13 121.09(9) . . ? C16 C15 C14 120.11(13) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? N17 C16 C15 119.27(15) . . ? N17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 N17 C16 123.38(19) . 6_655 ? C16 N17 H17 118.31(10) . . ? C16 N17 H17 118.31(10) 6_655 . ? I19 I18 I19 176.639(7) 6_556 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H10 Cl20 0.86(3) 2.09(3) 2.9557(19) 177.2(18) . N17 H17 Cl20 0.86(3) 2.498(18) 3.1783(15) 136.2(4) 3_554 N17 H17 Cl20 0.86(3) 2.498(18) 3.1783(15) 136.2(4) 7_556 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.643 _refine_diff_density_min -1.433 _refine_diff_density_rms 0.195 # Attachment 'so26fin.cif' data_Compound-II _database_code_depnum_ccdc_archive 'CCDC 612489' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H24 N4 O8 Pt, 2(N H4)' _chemical_formula_sum 'C48 H32 N6 O8 Pt' _chemical_formula_weight 1015.89 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.7150(6) _cell_length_b 24.5928(6) _cell_length_c 8.1377(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.6466(17) _cell_angle_gamma 90.00 _cell_volume 5584.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6110 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 2.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5669 _exptl_absorpt_correction_T_max 0.6284 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25674 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.87 _reflns_number_total 6381 _reflns_number_gt 5039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The DMF and additional water/ammonium solvent is severely disordered within the interporphyrin channels, and could not be modeled reliably. Conventional least-squares refinement converged at R=0.06, but the residual electron-density map showed 5 2-4 e/A^3^ peaks. One of these peaks could represent ammonium or hydronium ion to account for the charge balance. The ammonium ion bridged porphyrin lattice consists only 62% of the crystal volume. The residual electron-density within the channel voids was assessed to be about 280e per unit cell, which may correspond to 7 molecules of DMF or an appropriate combination of DMF, water and ammonium species. In the final calculations the contribution of the disordered solvent was subtracted from the diffraction data by the Squeeze procedure (Spek, 2003). Within the molecular framework the C26-O27-O28 carboxylate group is partially disordered in its orientation, but this disorder could not be resolved. The H-atoms of the ammonium ion were located in a difference-Fourier map and their coordinates were subjected to unconstrained refinement. ; _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^)+(0.0358P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6381 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 Pt Pt 0.0000 0.057014(9) 0.7500 0.02189(7) Uani 1 2 d S . . C1 C 0.0000 0.1975(2) 0.7500 0.0238(12) Uani 1 2 d S . . C2 C 0.04343(13) 0.16992(15) 0.7586(4) 0.0235(8) Uani 1 1 d . . . C3 C 0.08914(14) 0.19677(16) 0.7704(5) 0.0284(9) Uani 1 1 d . . . H3 H 0.0952 0.2347 0.7837 0.034 Uiso 1 1 calc R . . C4 C 0.12141(14) 0.15771(15) 0.7588(5) 0.0282(9) Uani 1 1 d . . . H4 H 0.1545 0.1630 0.7648 0.034 Uiso 1 1 calc R . . C5 C 0.09608(13) 0.10652(16) 0.7358(5) 0.0238(8) Uani 1 1 d . . . C6 C 0.11570(13) 0.05701(16) 0.7032(4) 0.0241(7) Uani 1 1 d . . . C7 C 0.09179(13) 0.00753(15) 0.6910(5) 0.0232(8) Uani 1 1 d . . . C8 C 0.10982(14) -0.04382(15) 0.6460(5) 0.0282(9) Uani 1 1 d . . . H8 H 0.1392 -0.0493 0.6141 0.034 Uiso 1 1 calc R . . C9 C 0.07778(13) -0.08247(16) 0.6570(5) 0.0248(8) Uani 1 1 d . . . H9 H 0.0802 -0.1201 0.6333 0.030 Uiso 1 1 calc R . . C10 C 0.03893(13) -0.05639(15) 0.7115(4) 0.0210(7) Uani 1 1 d . . . C11 C 0.0000 -0.0829(2) 0.7500 0.0234(11) Uani 1 2 d S . . N12 N 0.04858(11) 0.11504(12) 0.7419(4) 0.0227(7) Uani 1 1 d . . . N13 N 0.04721(11) -0.00077(12) 0.7246(3) 0.0208(6) Uani 1 1 d . . . C14 C 0.0000 0.2579(2) 0.7500 0.0234(11) Uani 1 2 d S . . C15 C 0.02829(14) 0.28720(15) 0.8836(5) 0.0263(8) Uani 1 1 d . . . H15 H 0.0476 0.2683 0.9768 0.032 Uiso 1 1 calc R . . C16 C 0.02855(14) 0.34336(15) 0.8821(5) 0.0268(9) Uani 1 1 d . . . H16 H 0.0487 0.3625 0.9733 0.032 Uiso 1 1 calc R . . C17 C 0.0000 0.3723(2) 0.7500 0.0272(12) Uani 1 2 d S . . C18 C 0.0000 0.4338(2) 0.7500 0.0278(13) Uani 1 2 d S . . O19 O 0.02726(12) 0.45815(11) 0.8712(4) 0.0366(7) Uani 1 1 d . . . C20 C 0.16618(13) 0.05812(16) 0.6836(5) 0.0257(8) Uani 1 1 d . . . C21 C 0.17873(14) 0.09006(16) 0.5593(5) 0.0314(9) Uani 1 1 d . . . H21 H 0.1547 0.1102 0.4834 0.038 Uiso 1 1 calc R . . C22 C 0.22584(16) 0.09276(18) 0.5450(6) 0.0371(10) Uani 1 1 d . . . H22 H 0.2337 0.1151 0.4603 0.045 Uiso 1 1 calc R . . C23 C 0.26145(15) 0.06338(18) 0.6523(6) 0.0371(10) Uani 1 1 d . . . C24 C 0.24910(16) 0.02972(19) 0.7728(6) 0.0417(11) Uani 1 1 d . . . H24 H 0.2729 0.0082 0.8446 0.050 Uiso 1 1 calc R . . C25 C 0.20163(15) 0.02755(18) 0.7884(5) 0.0347(10) Uani 1 1 d . . . H25 H 0.1936 0.0048 0.8719 0.042 Uiso 1 1 calc R . . C26 C 0.31303(18) 0.0679(2) 0.6385(7) 0.0539(14) Uani 1 1 d . . . O27 O 0.32163(14) 0.0977(3) 0.5303(6) 0.1081(19) Uani 1 1 d . . . O28 O 0.34350(15) 0.0421(2) 0.7382(8) 0.117(2) Uani 1 1 d . . . C29 C 0.0000 -0.1448(3) 0.7500 0.0287(13) Uani 1 2 d S . . C30 C 0.03840(13) -0.17280(16) 0.8489(4) 0.0234(8) Uani 1 1 d . . . H30 H 0.0646 -0.1535 0.9172 0.028 Uiso 1 1 calc R . . C31 C 0.03848(15) -0.22944(16) 0.8477(5) 0.0285(9) Uani 1 1 d . . . H31 H 0.0650 -0.2486 0.9142 0.034 Uiso 1 1 calc R . . C32 C 0.0000 -0.2583(2) 0.7500 0.0269(12) Uani 1 2 d S . . C33 C 0.0000 -0.3197(2) 0.7500 0.0307(13) Uani 1 2 d S . . O34 O -0.03875(12) -0.34375(11) 0.6834(4) 0.0406(7) Uani 1 1 d . . . N35 N 0.05869(13) 0.44835(16) 0.2276(5) 0.0297(8) Uani 1 1 d . . . H35A H 0.0461(18) 0.4492(18) 0.121(7) 0.045 Uiso 1 1 d . . . H35B H 0.0474(17) 0.474(2) 0.286(6) 0.045 Uiso 1 1 d . . . H35C H 0.087(2) 0.451(2) 0.243(6) 0.045 Uiso 1 1 d . . . H35D H 0.0465(16) 0.412(2) 0.251(5) 0.045 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 Pt 0.02005(11) 0.01824(11) 0.02736(12) 0.000 0.00554(8) 0.000 C1 0.031(3) 0.017(3) 0.023(3) 0.000 0.007(2) 0.000 C2 0.025(2) 0.0168(18) 0.0294(19) 0.0002(16) 0.0089(15) -0.0005(16) C3 0.030(2) 0.0190(19) 0.038(2) -0.0056(16) 0.0104(17) -0.0084(16) C4 0.023(2) 0.021(2) 0.041(2) -0.0017(16) 0.0090(17) -0.0056(16) C5 0.0159(19) 0.027(2) 0.028(2) 0.0004(15) 0.0038(15) 0.0000(15) C6 0.0229(18) 0.0229(18) 0.0260(18) 0.0001(16) 0.0046(14) 0.0000(17) C7 0.0179(19) 0.025(2) 0.0254(19) 0.0010(15) 0.0029(15) 0.0016(15) C8 0.025(2) 0.026(2) 0.033(2) 0.0017(16) 0.0069(17) 0.0026(16) C9 0.026(2) 0.0188(19) 0.030(2) -0.0040(15) 0.0066(16) 0.0034(16) C10 0.0223(18) 0.0165(17) 0.0225(18) -0.0012(15) 0.0016(14) 0.0035(16) C11 0.023(3) 0.016(3) 0.029(3) 0.000 0.003(2) 0.000 N12 0.0247(18) 0.0205(17) 0.0222(16) 0.0004(12) 0.0039(13) 0.0023(13) N13 0.0210(17) 0.0207(16) 0.0189(15) -0.0004(12) 0.0008(12) -0.0045(13) C14 0.029(3) 0.009(2) 0.035(3) 0.000 0.012(2) 0.000 C15 0.032(2) 0.021(2) 0.030(2) -0.0001(15) 0.0153(17) 0.0013(16) C16 0.033(2) 0.020(2) 0.029(2) -0.0043(15) 0.0100(17) -0.0035(16) C17 0.033(3) 0.021(3) 0.032(3) 0.000 0.017(3) 0.000 C18 0.035(3) 0.020(3) 0.031(3) 0.000 0.013(3) 0.000 O19 0.053(2) 0.0182(15) 0.0383(17) -0.0017(12) 0.0114(15) -0.0055(13) C20 0.0216(19) 0.0201(18) 0.036(2) -0.0013(17) 0.0077(15) 0.0007(17) C21 0.024(2) 0.026(2) 0.043(2) -0.0037(17) 0.0075(18) -0.0026(17) C22 0.035(3) 0.032(2) 0.049(3) -0.0048(19) 0.018(2) -0.0070(19) C23 0.023(2) 0.036(3) 0.055(3) -0.008(2) 0.0141(19) -0.0025(19) C24 0.025(2) 0.039(3) 0.059(3) 0.006(2) 0.006(2) 0.008(2) C25 0.025(2) 0.033(2) 0.047(3) 0.0039(19) 0.0106(19) 0.0026(18) C26 0.028(3) 0.064(4) 0.072(4) -0.012(3) 0.017(3) -0.009(2) O27 0.034(2) 0.186(6) 0.109(4) 0.032(4) 0.026(2) -0.028(3) O28 0.026(2) 0.149(5) 0.180(5) 0.066(4) 0.033(3) 0.023(3) C29 0.022(3) 0.048(4) 0.019(3) 0.000 0.008(2) 0.000 C30 0.0184(19) 0.028(2) 0.0213(18) -0.0015(16) -0.0004(14) -0.0001(16) C31 0.032(2) 0.024(2) 0.031(2) 0.0032(16) 0.0106(17) 0.0048(17) C32 0.039(3) 0.015(3) 0.030(3) 0.000 0.016(3) 0.000 C33 0.046(4) 0.021(3) 0.028(3) 0.000 0.014(3) 0.000 O34 0.050(2) 0.0205(16) 0.0502(18) -0.0028(13) 0.0098(15) -0.0070(14) N35 0.0219(17) 0.028(2) 0.038(2) -0.0030(16) 0.0051(15) -0.0010(17) _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 Pt N13 2.008(3) 2_556 ? Pt N13 2.008(3) . ? Pt N12 2.007(3) 2_556 ? Pt N12 2.008(3) . ? C1 C2 1.407(4) 2_556 ? C1 C2 1.407(4) . ? C1 C14 1.486(7) . ? C2 N12 1.368(5) . ? C2 C3 1.452(5) . ? C3 C4 1.353(5) . ? C3 H3 0.9500 . ? C4 C5 1.444(5) . ? C4 H4 0.9500 . ? C5 N12 1.392(4) . ? C5 C6 1.393(5) . ? C6 C7 1.389(5) . ? C6 C20 1.495(5) . ? C7 N13 1.386(4) . ? C7 C8 1.445(5) . ? C8 C9 1.340(5) . ? C8 H8 0.9500 . ? C9 C10 1.444(5) . ? C9 H9 0.9500 . ? C10 N13 1.388(5) . ? C10 C11 1.392(4) . ? C11 C10 1.392(4) 2_556 ? C11 C29 1.522(8) . ? C14 C15 1.394(5) 2_556 ? C14 C15 1.394(5) . ? C15 C16 1.381(5) . ? C15 H15 0.9500 . ? C16 C17 1.385(5) . ? C16 H16 0.9500 . ? C17 C16 1.385(5) 2_556 ? C17 C18 1.513(7) . ? C18 O19 1.256(4) . ? C18 O19 1.256(4) 2_556 ? C20 C25 1.385(6) . ? C20 C21 1.394(5) . ? C21 C22 1.386(6) . ? C21 H21 0.9500 . ? C22 C23 1.382(6) . ? C22 H22 0.9500 . ? C23 C24 1.392(6) . ? C23 C26 1.516(6) . ? C24 C25 1.399(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O27 1.216(7) . ? C26 O28 1.220(7) . ? C29 C30 1.386(5) . ? C29 C30 1.386(5) 2_556 ? C30 C31 1.393(5) . ? C30 H30 0.9500 . ? C31 C32 1.393(5) . ? C31 H31 0.9500 . ? C32 C31 1.393(5) 2_556 ? C32 C33 1.512(7) . ? C33 O34 1.263(4) . ? C33 O34 1.264(4) 2_556 ? N35 H35A 0.86(5) . ? N35 H35B 0.90(5) . ? N35 H35C 0.78(5) . ? N35 H35D 1.00(5) . ? 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 N13 Pt N13 89.90(17) 2_556 . ? N13 Pt N12 90.49(12) 2_556 2_556 ? N13 Pt N12 176.09(12) . 2_556 ? N13 Pt N12 176.09(12) 2_556 . ? N13 Pt N12 90.49(12) . . ? N12 Pt N12 89.39(17) 2_556 . ? C2 C1 C2 122.3(5) 2_556 . ? C2 C1 C14 118.8(2) 2_556 . ? C2 C1 C14 118.8(2) . . ? N12 C2 C1 125.9(4) . . ? N12 C2 C3 109.8(3) . . ? C1 C2 C3 124.1(4) . . ? C4 C3 C2 107.2(3) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? C3 C4 C5 107.2(3) . . ? C3 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? N12 C5 C6 125.6(3) . . ? N12 C5 C4 109.4(3) . . ? C6 C5 C4 125.0(3) . . ? C5 C6 C7 124.3(3) . . ? C5 C6 C20 116.7(3) . . ? C7 C6 C20 118.9(3) . . ? N13 C7 C6 125.4(3) . . ? N13 C7 C8 108.9(3) . . ? C6 C7 C8 125.7(3) . . ? C9 C8 C7 108.1(3) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? C8 C9 C10 107.3(3) . . ? C8 C9 H9 126.3 . . ? C10 C9 H9 126.3 . . ? N13 C10 C11 125.2(3) . . ? N13 C10 C9 109.3(3) . . ? C11 C10 C9 125.5(4) . . ? C10 C11 C10 124.2(5) 2_556 . ? C10 C11 C29 117.9(2) 2_556 . ? C10 C11 C29 117.9(2) . . ? C2 N12 C5 106.4(3) . . ? C2 N12 Pt 127.3(2) . . ? C5 N12 Pt 126.0(2) . . ? C7 N13 C10 106.2(3) . . ? C7 N13 Pt 126.4(2) . . ? C10 N13 Pt 126.7(2) . . ? C15 C14 C15 117.8(5) 2_556 . ? C15 C14 C1 121.1(2) 2_556 . ? C15 C14 C1 121.1(2) . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 121.2(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C16 118.1(5) 2_556 . ? C16 C17 C18 120.9(2) 2_556 . ? C16 C17 C18 120.9(2) . . ? O19 C18 O19 123.2(5) . 2_556 ? O19 C18 C17 118.4(3) . . ? O19 C18 C17 118.4(3) 2_556 . ? C25 C20 C21 118.3(4) . . ? C25 C20 C6 121.0(3) . . ? C21 C20 C6 120.7(3) . . ? C20 C21 C22 120.8(4) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 118.9(4) . . ? C22 C23 C26 120.4(4) . . ? C24 C23 C26 120.8(4) . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C20 C25 C24 120.9(4) . . ? C20 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? O27 C26 O28 124.0(5) . . ? O27 C26 C23 117.8(5) . . ? O28 C26 C23 118.2(5) . . ? C30 C29 C30 120.3(6) . 2_556 ? C30 C29 C11 119.8(3) . . ? C30 C29 C11 119.9(3) 2_556 . ? C29 C30 C31 119.7(4) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 120.7(4) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C31 118.8(5) 2_556 . ? C31 C32 C33 120.6(2) 2_556 . ? C31 C32 C33 120.6(2) . . ? O34 C33 O34 124.3(5) . 2_556 ? O34 C33 C32 117.9(3) . . ? O34 C33 C32 117.9(3) 2_556 . ? H35A N35 H35B 114(4) . . ? H35A N35 H35C 109(5) . . ? H35B N35 H35C 109(5) . . ? H35A N35 H35D 98(4) . . ? H35B N35 H35D 110(4) . . ? H35C N35 H35D 116(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N35 H35A O19 0.86(5) 1.99(5) 2.838(5) 171(5) 1_554 N35 H35B O19 0.90(5) 1.94(5) 2.822(5) 166(4) 6_565 N35 H35C O28 0.79(5) 1.98(5) 2.766(5) 175(5) 7_556 N35 H35D O34 1.01(5) 1.77(5) 2.768(5) 167(4) 5_556 _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.280 _refine_diff_density_min -1.744 _refine_diff_density_rms 0.122