# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- compound1.cif' #========================================================================== #========================================================================== # SUBMISSION DETAILS _publ_contact_letter ; Date of submission: 2012-04-01 Please consider this CIF submission for publication. All authors have seen and approved this submission. The CIF has passed the Chester CHECKCIF routines and gives a satisfactory PRINTCIF file. Best wishes, Dr. Alexander Brice\~no ; #========================================================================== _publ_contact_author_name 'Dr. Alexander Briceno' _publ_contact_author_address ; Centro de Qu\'imica Instituto Venezolano de Investigaciones Cient\'ifica (IVIC) Apartado 21827 Caracas 1020-A Venezuela ; _publ_contact_author_phone '(58-212) 504-1320' _publ_contact_author_fax '(58-212) 504-1350' _publ_contact_author_email abriceno@ivic.ve _publ_requested_category ? _publ_requested_coeditor_name ? #========================================================================== #========================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Exploring the use of anionic homoleptic complexes as templates in the design of photoreactive multi-component supramolecular assemblies. ; loop_ _publ_author_name _publ_author_address A.Briceno ; Centro de Qu\'imica Instituto Venezolano de Investigaciones Cient\'ifica (IVIC) Apartado 21827 Caracas 1020-A Venezuela ; 'Yennifer Hill' ; Centro de Qu\'imica Instituto Venezolano de Investigaciones Cient\'ifica (IVIC) Apartado 21827 Caracas 1020-A Venezuela ; data_shelxle _database_code_depnum_ccdc_archive 'CCDC 874862' #TrackingRef '- compound1.cif' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '20 August 2008' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H11 N2, 0.5(C12 H12 N2), C4 N4 S4 Zn, 2(H2 O)' _chemical_formula_sum 'C22 H21 N7 O2 S4 Zn' _chemical_formula_weight 609.07 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.3938(15) _cell_length_b 21.103(4) _cell_length_c 16.647(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.118(5) _cell_angle_gamma 90.00 _cell_volume 2883.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1154 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.54 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type 'Multi Scan' _exptl_absorpt_correction_T_min 0.960 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device 'Mercury (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30245 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5350 _reflns_number_gt 4019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _computing_publication_material ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003). ; _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^)+(0.0367P)^2^+2.8934P] 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 5350 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Zn1 Zn 0.09345(4) -0.185496(18) -0.33442(2) 0.05121(14) Uani 1 1 d . . . S1 S -0.20625(15) -0.14960(6) -0.60033(7) 0.0860(4) Uani 1 1 d . . . S2 S -0.13008(14) -0.37112(5) -0.24613(7) 0.0752(3) Uani 1 1 d . . . S3 S 0.66160(14) -0.18883(8) -0.26555(9) 0.1071(5) Uani 1 1 d . . . S4 S -0.12314(13) 0.00098(5) -0.24615(7) 0.0759(3) Uani 1 1 d . . . O1W O 0.8929(5) -0.14514(17) 0.2152(2) 0.1287(15) Uani 1 1 d . . . H2W1 H 0.9388 -0.1636 0.2594 0.154 Uiso 1 1 d R . . H1W1 H 0.8693 -0.1131 0.2414 0.154 Uiso 1 1 d R . . O2W O 0.3181(3) 0.02799(13) -0.24886(16) 0.0816(8) Uani 1 1 d . . . H1W2 H 0.3208 0.0077 -0.2045 0.098 Uiso 1 1 d R . . H2W2 H 0.3940 0.0554 -0.2417 0.098 Uiso 1 1 d R . . N5 N 0.9654(4) -0.15266(17) 0.0669(2) 0.0737(9) Uani 1 1 d . . . H5A H 0.9542 -0.1454 0.1163 0.088 Uiso 1 1 calc R . . N6 N 0.6568(4) 0.04814(14) 0.10295(18) 0.0633(8) Uani 1 1 d . . . N7 N 0.3286(3) -0.02787(14) -0.39412(17) 0.0566(7) Uani 1 1 d . . . C1 C -0.0888(5) -0.16702(17) -0.5140(2) 0.0607(9) Uani 1 1 d . . . N1 N -0.0069(5) -0.17957(17) -0.4513(2) 0.0816(10) Uani 1 1 d . . . C2 C -0.0432(4) -0.30720(17) -0.2702(2) 0.0535(8) Uani 1 1 d . . . N2 N 0.0175(4) -0.26186(15) -0.2881(2) 0.0657(8) Uani 1 1 d . . . C3 C 0.4667(5) -0.19021(16) -0.2944(2) 0.0592(9) Uani 1 1 d . . . N3 N 0.3291(4) -0.18961(16) -0.3171(2) 0.0754(9) Uani 1 1 d . . . C4 C -0.0322(4) -0.06221(17) -0.2686(2) 0.0568(8) Uani 1 1 d . . . N4 N 0.0317(4) -0.10758(15) -0.2847(2) 0.0709(9) Uani 1 1 d . . . H7N H 0.3055 -0.0069 -0.3475 0.085 Uiso 1 1 d R . . C5 C 0.7586(5) -0.0093(2) -0.0045(3) 0.0758(11) Uani 1 1 d . . . H5 H 0.7615 -0.0106 -0.0600 0.091 Uiso 1 1 calc R . . C6 C 0.8235(5) -0.0549(2) 0.0402(3) 0.0758(11) Uani 1 1 d . . . H6 H 0.8211 -0.0540 0.0957 0.091 Uiso 1 1 calc R . . C7 C 0.9039(4) -0.11041(18) 0.0086(2) 0.0625(9) Uani 1 1 d . . . C8 C 1.0432(6) -0.2057(2) 0.0529(3) 0.0898(14) Uani 1 1 d . . . H8 H 1.0859 -0.2330 0.0959 0.108 Uiso 1 1 calc R . . C9 C 1.0591(6) -0.2192(2) -0.0253(4) 0.0938(15) Uani 1 1 d . . . H9 H 1.1108 -0.2561 -0.0368 0.113 Uiso 1 1 calc R . . C10 C 0.9965(6) -0.1768(3) -0.0867(3) 0.0874(14) Uani 1 1 d . . . H10 H 1.0059 -0.1850 -0.1404 0.105 Uiso 1 1 calc R . . C11 C 0.9207(5) -0.1229(2) -0.0693(3) 0.0778(11) Uani 1 1 d . . . H11 H 0.8802 -0.0943 -0.1111 0.093 Uiso 1 1 calc R . . C12 C 0.6787(4) 0.04573(17) 0.0252(2) 0.0592(9) Uani 1 1 d . . . C13 C 0.5870(5) 0.1000(2) 0.1244(3) 0.0772(11) Uani 1 1 d . . . H13 H 0.5719 0.1026 0.1780 0.093 Uiso 1 1 calc R . . C14 C 0.5356(6) 0.1500(2) 0.0732(3) 0.0844(13) Uani 1 1 d . . . H14 H 0.4883 0.1853 0.0919 0.101 Uiso 1 1 calc R . . C15 C 0.5550(6) 0.1467(2) -0.0047(3) 0.0904(14) Uani 1 1 d . . . H15 H 0.5203 0.1798 -0.0410 0.108 Uiso 1 1 calc R . . C16 C 0.6265(5) 0.0942(2) -0.0301(3) 0.0775(12) Uani 1 1 d . . . H16 H 0.6399 0.0911 -0.0841 0.093 Uiso 1 1 calc R . . C17 C 0.0577(4) -0.00379(16) -0.4662(2) 0.0539(8) Uani 1 1 d . . . H17 H 0.0366 0.0108 -0.4168 0.065 Uiso 1 1 calc R . . C18 C 0.2147(4) -0.03335(16) -0.4648(2) 0.0522(8) Uani 1 1 d . . . C19 C 0.4796(5) -0.0518(2) -0.3849(2) 0.0701(11) Uani 1 1 d . . . H19 H 0.5533 -0.0470 -0.3351 0.084 Uiso 1 1 calc R . . C20 C 0.5255(5) -0.0831(2) -0.4478(3) 0.0757(11) Uani 1 1 d . . . H20 H 0.6308 -0.0989 -0.4420 0.091 Uiso 1 1 calc R . . C21 C 0.4125(5) -0.0910(2) -0.5208(3) 0.0757(11) Uani 1 1 d . . . H21 H 0.4407 -0.1133 -0.5640 0.091 Uiso 1 1 calc R . . C22 C 0.2591(5) -0.06606(18) -0.5292(2) 0.0645(10) Uani 1 1 d . . . H22 H 0.1840 -0.0711 -0.5785 0.077 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 Zn1 0.0511(2) 0.0458(2) 0.0553(3) 0.00183(18) 0.00786(17) -0.00215(17) S1 0.0969(8) 0.1013(9) 0.0530(6) 0.0153(6) 0.0004(5) -0.0166(7) S2 0.0861(7) 0.0656(6) 0.0738(7) 0.0123(5) 0.0166(5) -0.0181(5) S3 0.0526(6) 0.1414(12) 0.1189(11) -0.0374(9) -0.0013(6) 0.0170(7) S4 0.0829(7) 0.0557(6) 0.0833(8) -0.0049(5) 0.0043(6) 0.0185(5) O1W 0.234(5) 0.093(3) 0.082(2) -0.0042(19) 0.083(3) -0.002(3) O2W 0.104(2) 0.083(2) 0.0554(16) 0.0063(14) 0.0122(14) -0.0190(16) N5 0.087(2) 0.077(2) 0.065(2) -0.0018(18) 0.0349(18) 0.0039(19) N6 0.079(2) 0.0537(18) 0.0538(19) -0.0013(15) 0.0053(15) -0.0002(15) N7 0.0569(18) 0.0661(19) 0.0453(17) 0.0031(14) 0.0070(13) -0.0089(14) C1 0.072(2) 0.058(2) 0.053(2) 0.0022(18) 0.0163(19) -0.0106(18) N1 0.095(3) 0.077(2) 0.065(2) 0.0096(19) -0.001(2) -0.0088(19) C2 0.054(2) 0.055(2) 0.050(2) 0.0048(17) 0.0079(15) 0.0027(16) N2 0.0648(19) 0.0552(19) 0.079(2) 0.0114(16) 0.0180(16) 0.0017(15) C3 0.060(2) 0.052(2) 0.066(2) -0.0128(18) 0.0168(18) 0.0068(17) N3 0.055(2) 0.082(2) 0.091(3) -0.0100(19) 0.0188(17) -0.0041(17) C4 0.060(2) 0.048(2) 0.060(2) 0.0003(17) 0.0070(16) -0.0033(16) N4 0.074(2) 0.0519(19) 0.087(2) -0.0038(17) 0.0186(17) 0.0028(16) C5 0.073(3) 0.081(3) 0.072(3) -0.001(2) 0.010(2) -0.016(2) C6 0.077(3) 0.079(3) 0.070(3) 0.000(2) 0.011(2) -0.009(2) C7 0.061(2) 0.059(2) 0.068(3) -0.006(2) 0.0160(18) -0.0004(17) C8 0.102(3) 0.075(3) 0.100(4) 0.025(3) 0.040(3) 0.018(3) C9 0.099(3) 0.071(3) 0.122(4) -0.011(3) 0.049(3) 0.013(3) C10 0.089(3) 0.114(4) 0.065(3) -0.021(3) 0.028(2) 0.001(3) C11 0.085(3) 0.085(3) 0.061(3) 0.007(2) 0.010(2) 0.006(2) C12 0.059(2) 0.054(2) 0.063(2) -0.0138(18) 0.0110(17) -0.0064(16) C13 0.106(3) 0.063(3) 0.064(3) -0.012(2) 0.021(2) 0.003(2) C14 0.095(3) 0.056(3) 0.101(4) -0.006(3) 0.017(3) 0.007(2) C15 0.100(4) 0.066(3) 0.101(4) 0.021(3) 0.011(3) -0.001(2) C16 0.091(3) 0.083(3) 0.059(3) 0.005(2) 0.019(2) -0.016(2) C17 0.060(2) 0.058(2) 0.0435(19) 0.0021(16) 0.0100(14) -0.0088(16) C18 0.060(2) 0.051(2) 0.045(2) 0.0092(15) 0.0101(16) -0.0110(15) C19 0.059(2) 0.085(3) 0.063(3) 0.013(2) 0.0039(18) -0.005(2) C20 0.067(3) 0.088(3) 0.075(3) 0.014(2) 0.021(2) 0.009(2) C21 0.088(3) 0.077(3) 0.068(3) 0.006(2) 0.029(2) 0.005(2) C22 0.073(3) 0.073(3) 0.047(2) 0.0000(18) 0.0101(18) -0.0029(19) _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 Zn1 N3 1.940(3) . ? Zn1 N2 1.950(3) . ? Zn1 N1 1.955(4) . ? Zn1 N4 1.959(3) . ? S1 C1 1.605(4) . ? S2 C2 1.623(4) . ? S3 C3 1.606(4) . ? S4 C4 1.619(4) . ? O1W H2W1 0.8501 . ? O1W H1W1 0.8500 . ? O2W H1W2 0.8499 . ? O2W H2W2 0.8500 . ? N5 C7 1.339(5) . ? N5 C8 1.341(5) . ? N5 H5A 0.8600 . ? N6 C13 1.325(5) . ? N6 C12 1.345(5) . ? N7 C19 1.343(5) . ? N7 C18 1.356(4) . ? N7 H7N 0.9479 . ? C1 N1 1.154(5) . ? C2 N2 1.152(4) . ? C3 N3 1.137(4) . ? C4 N4 1.156(4) . ? C5 C6 1.267(6) . ? C5 C12 1.478(5) . ? C5 H5 0.9300 . ? C6 C7 1.501(6) . ? C6 H6 0.9300 . ? C7 C11 1.359(5) . ? C8 C9 1.366(6) . ? C8 H8 0.9300 . ? C9 C10 1.377(7) . ? C9 H9 0.9300 . ? C10 C11 1.364(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C16 1.385(5) . ? C13 C14 1.367(6) . ? C13 H13 0.9300 . ? C14 C15 1.342(6) . ? C14 H14 0.9300 . ? C15 C16 1.369(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C17 1.331(6) 3_554 ? C17 C18 1.453(5) . ? C17 H17 0.9300 . ? C18 C22 1.390(5) . ? C19 C20 1.361(6) . ? C19 H19 0.9300 . ? C20 C21 1.385(6) . ? C20 H20 0.9300 . ? C21 C22 1.371(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? 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 N3 Zn1 N2 108.17(14) . . ? N3 Zn1 N1 111.35(16) . . ? N2 Zn1 N1 109.75(14) . . ? N3 Zn1 N4 109.07(14) . . ? N2 Zn1 N4 112.87(13) . . ? N1 Zn1 N4 105.67(15) . . ? H2W1 O1W H1W1 92.0 . . ? H1W2 O2W H2W2 109.7 . . ? C7 N5 C8 123.8(4) . . ? C7 N5 H5A 118.1 . . ? C8 N5 H5A 118.1 . . ? C13 N6 C12 116.6(3) . . ? C19 N7 C18 122.9(3) . . ? C19 N7 H7N 115.6 . . ? C18 N7 H7N 121.5 . . ? N1 C1 S1 178.7(4) . . ? C1 N1 Zn1 164.9(4) . . ? N2 C2 S2 179.3(4) . . ? C2 N2 Zn1 170.9(3) . . ? N3 C3 S3 177.5(4) . . ? C3 N3 Zn1 169.3(3) . . ? N4 C4 S4 179.5(4) . . ? C4 N4 Zn1 165.8(3) . . ? C6 C5 C12 124.7(4) . . ? C6 C5 H5 117.6 . . ? C12 C5 H5 117.6 . . ? C5 C6 C7 123.8(4) . . ? C5 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? N5 C7 C11 117.5(4) . . ? N5 C7 C6 113.5(4) . . ? C11 C7 C6 129.0(4) . . ? N5 C8 C9 119.3(4) . . ? N5 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C8 C9 C10 118.2(4) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C11 C10 C9 120.5(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C7 C11 C10 120.7(4) . . ? C7 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? N6 C12 C16 121.6(3) . . ? N6 C12 C5 121.0(4) . . ? C16 C12 C5 117.4(4) . . ? N6 C13 C14 124.7(4) . . ? N6 C13 H13 117.7 . . ? C14 C13 H13 117.7 . . ? C15 C14 C13 118.4(4) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C14 C15 C16 119.4(4) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C12 119.3(4) . . ? C15 C16 H16 120.3 . . ? C12 C16 H16 120.3 . . ? C17 C17 C18 124.2(4) 3_554 . ? C17 C17 H17 117.9 3_554 . ? C18 C17 H17 117.9 . . ? N7 C18 C22 117.2(3) . . ? N7 C18 C17 116.7(3) . . ? C22 C18 C17 126.1(3) . . ? N7 C19 C20 120.5(4) . . ? N7 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 118.7(4) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C22 C21 C20 120.0(4) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C18 120.6(4) . . ? C21 C22 H22 119.7 . . ? C18 C22 H22 119.7 . . ? _diffrn_measured_fraction_theta_max 0.806 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.659 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.053 # Attachment '- compound2.cif' data_shelxle_2 _database_code_depnum_ccdc_archive 'CCDC 874863' #TrackingRef '- compound2.cif' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '20 August 2008' #========================================================================== #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 N2, C4 N4 S4 Zn, 2(H2 O)' _chemical_formula_sum 'C16 H16 N6 O2 S4 Zn' _chemical_formula_weight 517.96 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' 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 14.140(5) _cell_length_b 14.784(4) _cell_length_c 11.087(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.242(11) _cell_angle_gamma 90.00 _cell_volume 2256.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1012 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.80 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.483 _exptl_absorpt_correction_type 'Multi Scan' _exptl_absorpt_correction_T_min 0.565 _exptl_absorpt_correction_T_max 0.767 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device 'Mercury (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12836 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.80 _reflns_number_total 2292 _reflns_number_gt 1814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _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^)+(0.0543P)^2^+2.9407P] 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 2292 _refine_ls_number_parameters 181 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.033 _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 Zn1 Zn 0.37163(4) 0.5000 0.07551(5) 0.0567(2) Uani 1 2 d S . . S1 S 0.63675(10) 0.5000 0.41937(14) 0.0775(4) Uani 1 2 d S . . S2 S 0.11393(10) 0.5000 0.28404(11) 0.0656(3) Uani 1 2 d S . . S3 S 0.35755(7) 0.24741(7) -0.18595(8) 0.0714(3) Uani 1 1 d . . . N1 N 0.3567(2) 0.3919(2) -0.0272(3) 0.0782(9) Uani 1 1 d . . . N2 N 0.2691(3) 0.5000 0.1703(4) 0.0643(10) Uani 1 2 d S . . N3 N 0.4915(3) 0.5000 0.2047(5) 0.0734(11) Uani 1 2 d S . . C1 C 0.5522(3) 0.5000 0.2934(5) 0.0581(11) Uani 1 2 d S . . C2 C 0.2053(3) 0.5000 0.2199(4) 0.0493(10) Uani 1 2 d S . . C3 C 0.3576(2) 0.3325(2) -0.0939(3) 0.0564(8) Uani 1 1 d . . . C6 C 0.3819(5) 0.1291(3) 0.3358(6) 0.0311(15) Uani 0.50 1 d PGU . 1 N4 N 0.4051(8) 0.1848(5) 0.2457(6) 0.0486(18) Uani 0.50 1 d PGU . 1 H4N H 0.4163 0.1615 0.1792 0.058 Uiso 0.50 1 calc PR . 1 C10 C 0.4100(12) 0.2779(5) 0.2629(9) 0.067(3) Uani 0.50 1 d PGU . 1 H10A H 0.4255 0.3151 0.2027 0.081 Uiso 0.50 1 calc PR . 1 C9 C 0.3918(13) 0.3154(3) 0.3703(11) 0.060(3) Uani 0.50 1 d PGU . 1 H9A H 0.3951 0.3778 0.3819 0.072 Uiso 0.50 1 calc PR . 1 C8 C 0.3686(10) 0.2598(5) 0.4604(8) 0.041(2) Uani 0.50 1 d PGU . 1 H8A H 0.3565 0.2849 0.5323 0.049 Uiso 0.50 1 calc PR . 1 C7 C 0.3637(6) 0.1666(4) 0.4432(6) 0.0338(16) Uani 0.50 1 d PGU . 1 H7A H 0.3482 0.1294 0.5035 0.041 Uiso 0.50 1 calc PR . 1 C4 C 0.3823(4) 0.0320(3) 0.3079(6) 0.0431(12) Uani 0.50 1 d PU . 1 H4 H 0.3944 0.0000 0.2109 0.052 Uiso 1 2 d SR . 1 C6A C 0.3744(6) 0.1298(3) 0.3820(6) 0.0404(18) Uani 0.50 1 d PGU . 2 N4A N 0.3931(7) 0.1643(5) 0.2731(6) 0.0405(17) Uani 0.50 1 d PGU . 2 H4NA H 0.3986 0.1282 0.2143 0.049 Uiso 0.50 1 calc PR . 2 C10A C 0.4028(10) 0.2571(5) 0.2595(8) 0.049(2) Uani 0.50 1 d PGU . 2 H10B H 0.4154 0.2801 0.1867 0.059 Uiso 0.50 1 calc PR . 2 C9A C 0.3939(13) 0.3153(4) 0.3546(11) 0.053(3) Uani 0.50 1 d PGU . 2 H9AA H 0.4004 0.3774 0.3455 0.063 Uiso 0.50 1 calc PR . 2 C8A C 0.3752(11) 0.2808(5) 0.4635(9) 0.057(3) Uani 0.50 1 d PGU . 2 H8AA H 0.3692 0.3198 0.5271 0.069 Uiso 0.50 1 calc PR . 2 C7A C 0.3654(8) 0.1881(5) 0.4771(6) 0.053(2) Uani 0.50 1 d PGU . 2 H7AA H 0.3529 0.1650 0.5499 0.064 Uiso 0.50 1 calc PR . 2 C4A C 0.3712(4) 0.0298(3) 0.3880(6) 0.0468(14) Uani 0.50 1 d PU . 2 H4A H 0.3596 0.0000 0.4588 0.056 Uiso 1 2 d SR . 2 O1W O 0.41129(19) 0.09815(18) 0.0381(2) 0.0805(8) Uani 1 1 d . . . H2W1 H 0.3836 0.1296 -0.0172 0.097 Uiso 1 1 d R . . H1W1 H 0.3789 0.0520 0.0253 0.097 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0678(4) 0.0431(3) 0.0643(4) 0.000 0.0253(3) 0.000 S1 0.0719(9) 0.0590(8) 0.0977(10) 0.000 0.0117(7) 0.000 S2 0.0752(8) 0.0761(9) 0.0523(6) 0.000 0.0286(6) 0.000 S3 0.0836(7) 0.0601(6) 0.0675(6) -0.0143(4) 0.0113(5) 0.0050(4) N1 0.109(3) 0.0550(18) 0.079(2) -0.0104(15) 0.0395(18) -0.0045(17) N2 0.064(3) 0.066(3) 0.066(2) 0.000 0.023(2) 0.000 N3 0.061(3) 0.069(3) 0.092(3) 0.000 0.022(2) 0.000 C1 0.052(3) 0.041(2) 0.088(3) 0.000 0.030(3) 0.000 C2 0.060(3) 0.044(2) 0.043(2) 0.000 0.0087(19) 0.000 C3 0.061(2) 0.0494(19) 0.0596(19) 0.0023(15) 0.0162(14) 0.0015(15) C6 0.038(3) 0.039(3) 0.022(4) 0.001(3) 0.018(3) 0.005(2) N4 0.064(4) 0.037(4) 0.050(4) 0.016(3) 0.024(3) -0.004(3) C10 0.086(7) 0.040(4) 0.078(6) -0.001(4) 0.023(5) 0.002(5) C9 0.071(8) 0.035(5) 0.069(6) 0.004(4) 0.009(6) 0.002(6) C8 0.048(5) 0.021(4) 0.052(4) -0.008(3) 0.007(3) -0.002(3) C7 0.051(3) 0.026(3) 0.031(4) -0.011(3) 0.023(3) 0.001(3) C4 0.049(3) 0.038(3) 0.045(3) -0.001(2) 0.017(2) 0.000(2) C6A 0.049(3) 0.046(3) 0.032(5) 0.005(3) 0.022(4) -0.002(3) N4A 0.052(4) 0.043(4) 0.031(3) 0.005(3) 0.017(3) 0.002(3) C10A 0.061(5) 0.041(5) 0.044(4) 0.011(3) 0.010(3) -0.002(4) C9A 0.056(7) 0.048(6) 0.057(5) -0.003(4) 0.020(5) -0.002(6) C8A 0.066(6) 0.038(4) 0.072(5) 0.005(4) 0.022(5) -0.010(5) C7A 0.067(4) 0.046(5) 0.050(5) -0.023(4) 0.020(4) 0.004(4) C4A 0.056(3) 0.044(3) 0.044(3) 0.002(2) 0.018(2) 0.001(2) O1W 0.0973(19) 0.0716(17) 0.0644(14) -0.0137(12) 0.0017(13) 0.0082(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 1.945(3) . ? Zn1 N1 1.945(3) 6_565 ? Zn1 N3 1.953(5) . ? Zn1 N2 1.976(4) . ? S1 C1 1.617(6) . ? S2 C2 1.612(5) . ? S3 C3 1.620(3) . ? N1 C3 1.150(4) . ? N2 C2 1.159(5) . ? N3 C1 1.148(6) . ? C6 N4 1.3900 . ? C6 C7 1.3900 . ? C6 C4 1.469(7) . ? N4 C10 1.3900 . ? N4 H4N 0.8600 . ? C10 C9 1.3900 . ? C10 H10A 0.9300 . ? C9 C8 1.3900 . ? C9 H9A 0.9300 . ? C8 C7 1.3900 . ? C8 H8A 0.9300 . ? C7 H7A 0.9300 . ? C4 C4 0.946(10) 6 ? C4 H4 1.2215 . ? C6A N4A 1.3900 . ? C6A C7A 1.3900 . ? C6A C4A 1.481(7) . ? N4A C10A 1.3900 . ? N4A H4NA 0.8600 . ? C10A C9A 1.3900 . ? C10A H10B 0.9300 . ? C9A C8A 1.3900 . ? C9A H9AA 0.9300 . ? C8A C7A 1.3900 . ? C8A H8AA 0.9300 . ? C7A H7AA 0.9300 . ? C4A C4A 0.881(10) 6 ? C4A H4A 0.9473 . ? O1W H2W1 0.7973 . ? O1W H1W1 0.8155 . ? 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 Zn1 N1 110.47(19) . 6_565 ? N1 Zn1 N3 112.88(12) . . ? N1 Zn1 N3 112.88(12) 6_565 . ? N1 Zn1 N2 108.47(11) . . ? N1 Zn1 N2 108.47(11) 6_565 . ? N3 Zn1 N2 103.26(18) . . ? C3 N1 Zn1 171.1(3) . . ? C2 N2 Zn1 176.4(4) . . ? C1 N3 Zn1 169.1(4) . . ? N3 C1 S1 179.3(5) . . ? N2 C2 S2 177.9(4) . . ? N1 C3 S3 178.6(3) . . ? N4 C6 C7 120.0 . . ? N4 C6 C4 114.4(5) . . ? C7 C6 C4 125.5(5) . . ? C10 N4 C6 120.0 . . ? C10 N4 H4N 120.0 . . ? C6 N4 H4N 120.0 . . ? N4 C10 C9 120.0 . . ? N4 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C4 C4 C6 167.8(3) 6 . ? C4 C4 H4 67.2 6 . ? C6 C4 H4 124.9 . . ? N4A C6A C7A 120.0 . . ? N4A C6A C4A 114.8(5) . . ? C7A C6A C4A 125.1(5) . . ? C10A N4A C6A 120.0 . . ? C10A N4A H4NA 120.0 . . ? C6A N4A H4NA 120.0 . . ? N4A C10A C9A 120.0 . . ? N4A C10A H10B 120.0 . . ? C9A C10A H10B 120.0 . . ? C8A C9A C10A 120.0 . . ? C8A C9A H9AA 120.0 . . ? C10A C9A H9AA 120.0 . . ? C7A C8A C9A 120.0 . . ? C7A C8A H8AA 120.0 . . ? C9A C8A H8AA 120.0 . . ? C8A C7A C6A 120.0 . . ? C8A C7A H7AA 120.0 . . ? C6A C7A H7AA 120.0 . . ? C4A C4A C6A 176.6(4) 6 . ? C4A C4A H4A 62.3 6 . ? C6A C4A H4A 121.0 . . ? H2W1 O1W H1W1 101.4 . . ? _diffrn_measured_fraction_theta_max 0.822 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.276 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.057 # Attachment '- compound3.cif1.txt' data_shelxle_3 _database_code_depnum_ccdc_archive 'CCDC 874864' #TrackingRef '- compound3.cif1.txt' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '20 August 2008' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 N2, C4 N4 S4 Zn' _chemical_formula_sum 'C16 H12 N6 S4 Zn' _chemical_formula_weight 481.93 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 4.722(3) _cell_length_b 21.523(11) _cell_length_c 20.208(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.513(16) _cell_angle_gamma 90.00 _cell_volume 2049.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 960 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.59 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.619 _exptl_absorpt_correction_type 'Multi Scan' _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device 'Mercury (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8419 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.59 _reflns_number_total 2712 _reflns_number_gt 1908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _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^)+(0.0448P)^2^+1.6314P] 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 2712 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1089 _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 Zn1 Zn -0.39940(12) -0.24195(3) -0.26590(3) 0.0582(3) Uani 1 1 d . . . S1 S -0.9101(3) -0.42104(7) -0.20922(8) 0.0759(5) Uani 1 1 d . . . S2 S -0.9267(3) -0.06732(7) -0.34623(8) 0.0778(5) Uani 1 1 d . . . S3 S 0.1625(3) -0.18514(6) -0.07267(7) 0.0628(4) Uani 1 1 d . . . S4 S 0.1375(3) -0.33196(6) -0.43123(7) 0.0601(4) Uani 1 1 d . . . N1 N -0.6297(9) -0.3115(2) -0.2373(2) 0.0659(13) Uani 1 1 d . . . N2 N -0.6269(9) -0.1693(2) -0.2962(2) 0.0696(14) Uani 1 1 d . . . N3 N -0.1553(9) -0.2150(2) -0.1889(2) 0.0691(13) Uani 1 1 d . . . N4 N -0.1889(10) -0.2710(2) -0.3404(3) 0.0717(14) Uani 1 1 d . . . N5 N -0.3065(9) -0.2962(2) -0.0179(2) 0.0618(12) Uani 1 1 d . . . H5B H -0.3598 -0.2580 -0.0162 0.074 Uiso 1 1 calc R . . N6 N -0.4430(7) -0.50062(19) -0.3013(2) 0.0531(11) Uani 1 1 d . . . H6A H -0.5322 -0.4971 -0.2656 0.064 Uiso 1 1 calc R . . C1 C -0.7507(10) -0.3564(3) -0.2260(2) 0.0535(13) Uani 1 1 d . . . C2 C -0.7534(10) -0.1273(2) -0.3164(3) 0.0538(13) Uani 1 1 d . . . C3 C -0.0205(10) -0.2033(2) -0.1408(3) 0.0541(13) Uani 1 1 d . . . C4 C -0.0536(10) -0.2969(2) -0.3780(3) 0.0539(13) Uani 1 1 d . . . C5 C -0.0674(10) -0.4840(2) -0.0240(2) 0.0560(13) Uani 1 1 d . . . H5A H -0.1189 -0.5053 -0.0629 0.067 Uiso 1 1 calc R . . C6 C -0.1434(9) -0.4179(2) -0.0215(3) 0.0507(12) Uani 1 1 d . . . C7 C -0.3453(10) -0.3942(2) -0.0686(3) 0.0613(14) Uani 1 1 d . . . H7A H -0.4258 -0.4197 -0.1018 0.074 Uiso 1 1 calc R . . C8 C -0.4223(11) -0.3333(3) -0.0652(3) 0.0632(15) Uani 1 1 d . . . H8A H -0.5570 -0.3173 -0.0962 0.076 Uiso 1 1 calc R . . C9 C -0.1096(11) -0.3172(2) 0.0268(3) 0.0605(14) Uani 1 1 d . . . H9A H -0.0307 -0.2903 0.0589 0.073 Uiso 1 1 calc R . . C10 C -0.0225(10) -0.3775(2) 0.0263(3) 0.0550(13) Uani 1 1 d . . . H10A H 0.1160 -0.3916 0.0574 0.066 Uiso 1 1 calc R . . C11 C -0.0057(9) -0.5202(2) -0.4756(2) 0.0517(12) Uani 1 1 d . . . H11A H 0.0941 -0.5572 -0.4794 0.062 Uiso 1 1 calc R . . C12 C -0.1629(8) -0.5120(2) -0.4154(2) 0.0485(12) Uani 1 1 d . . . C13 C -0.3304(9) -0.4599(2) -0.4042(3) 0.0537(13) Uani 1 1 d . . . H13A H -0.3488 -0.4285 -0.4358 0.064 Uiso 1 1 calc R . . C14 C -0.4673(9) -0.4553(2) -0.3466(3) 0.0588(14) Uani 1 1 d . . . H14A H -0.5776 -0.4206 -0.3389 0.071 Uiso 1 1 calc R . . C15 C -0.2844(10) -0.5513(2) -0.3096(3) 0.0621(14) Uani 1 1 d . . . H15A H -0.2701 -0.5818 -0.2770 0.075 Uiso 1 1 calc R . . C16 C -0.1434(10) -0.5579(2) -0.3665(3) 0.0582(13) Uani 1 1 d . . . H16A H -0.0342 -0.5932 -0.3725 0.070 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 Zn1 0.0663(4) 0.0562(5) 0.0510(5) -0.0024(3) -0.0045(3) 0.0041(3) S1 0.0798(10) 0.0716(12) 0.0776(13) -0.0022(8) 0.0165(8) -0.0108(7) S2 0.1090(12) 0.0659(12) 0.0585(11) -0.0009(8) 0.0054(8) 0.0296(8) S3 0.0712(8) 0.0603(10) 0.0557(11) 0.0011(7) -0.0063(6) -0.0100(6) S4 0.0737(8) 0.0520(10) 0.0547(10) 0.0030(7) 0.0052(6) 0.0040(6) N1 0.079(3) 0.053(4) 0.064(4) 0.003(2) -0.004(2) 0.002(2) N2 0.077(3) 0.054(3) 0.078(4) 0.009(3) 0.005(2) 0.009(2) N3 0.074(3) 0.073(4) 0.059(4) -0.009(3) -0.005(2) 0.002(2) N4 0.072(3) 0.087(4) 0.055(4) -0.009(3) -0.007(2) 0.006(2) N5 0.084(3) 0.041(3) 0.062(4) 0.002(2) 0.016(2) 0.008(2) N6 0.063(2) 0.054(3) 0.042(3) -0.004(2) 0.0080(18) -0.0057(19) C1 0.066(3) 0.054(4) 0.040(3) -0.005(3) -0.005(2) 0.017(2) C2 0.065(3) 0.052(4) 0.045(4) -0.006(3) 0.006(2) -0.001(2) C3 0.060(3) 0.046(4) 0.057(4) 0.002(3) 0.011(3) 0.000(2) C4 0.061(3) 0.045(4) 0.053(4) 0.009(3) -0.014(2) -0.010(2) C5 0.072(3) 0.046(4) 0.049(4) -0.011(3) -0.001(2) 0.003(2) C6 0.062(3) 0.041(3) 0.051(4) -0.004(2) 0.012(2) 0.001(2) C7 0.074(3) 0.058(4) 0.051(4) -0.012(3) -0.005(3) 0.006(3) C8 0.084(4) 0.055(4) 0.050(4) 0.003(3) -0.004(3) 0.012(3) C9 0.079(4) 0.052(4) 0.050(4) -0.007(3) 0.003(3) -0.007(3) C10 0.069(3) 0.045(4) 0.050(4) -0.002(3) -0.001(2) -0.002(2) C11 0.061(3) 0.043(4) 0.051(4) -0.007(2) 0.004(2) 0.002(2) C12 0.048(2) 0.048(3) 0.050(4) -0.005(2) 0.000(2) -0.008(2) C13 0.060(3) 0.052(4) 0.050(4) 0.004(2) 0.006(2) 0.003(2) C14 0.062(3) 0.059(4) 0.057(4) -0.002(3) 0.009(3) 0.009(2) C15 0.076(4) 0.055(4) 0.056(4) 0.004(3) 0.007(3) -0.002(3) C16 0.073(3) 0.053(4) 0.049(4) 0.000(3) 0.009(3) 0.007(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 Zn1 N4 1.957(5) . ? Zn1 N1 1.958(5) . ? Zn1 N3 1.966(5) . ? Zn1 N2 1.973(5) . ? S1 C1 1.627(6) . ? S2 C2 1.624(5) . ? S3 C3 1.628(6) . ? S4 C4 1.631(6) . ? N1 C1 1.153(6) . ? N2 C2 1.146(6) . ? N3 C3 1.157(6) . ? N4 C4 1.164(6) . ? N5 C9 1.336(6) . ? N5 C8 1.336(6) . ? N5 H5B 0.8600 . ? N6 C14 1.337(6) . ? N6 C15 1.340(6) . ? N6 H6A 0.8600 . ? C5 C5 1.320(9) 3_545 ? C5 C6 1.470(6) . ? C5 H5A 0.9300 . ? C6 C10 1.395(6) . ? C6 C7 1.401(7) . ? C7 C8 1.364(6) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 C10 1.360(6) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C11 1.321(9) 3_544 ? C11 C12 1.474(6) . ? C11 H11A 0.9300 . ? C12 C16 1.398(6) . ? C12 C13 1.398(6) . ? C13 C14 1.370(6) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.370(6) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? 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 N4 Zn1 N1 107.47(19) . . ? N4 Zn1 N3 113.72(19) . . ? N1 Zn1 N3 107.54(19) . . ? N4 Zn1 N2 107.8(2) . . ? N1 Zn1 N2 113.33(18) . . ? N3 Zn1 N2 107.07(19) . . ? C1 N1 Zn1 172.1(5) . . ? C2 N2 Zn1 177.0(5) . . ? C3 N3 Zn1 174.2(5) . . ? C4 N4 Zn1 168.5(5) . . ? C9 N5 C8 121.2(5) . . ? C9 N5 H5B 119.4 . . ? C8 N5 H5B 119.4 . . ? C14 N6 C15 122.2(5) . . ? C14 N6 H6A 118.9 . . ? C15 N6 H6A 118.9 . . ? N1 C1 S1 177.8(5) . . ? N2 C2 S2 178.6(5) . . ? N3 C3 S3 178.2(5) . . ? N4 C4 S4 179.0(5) . . ? C5 C5 C6 126.0(6) 3_545 . ? C5 C5 H5A 117.0 3_545 . ? C6 C5 H5A 117.0 . . ? C10 C6 C7 118.5(5) . . ? C10 C6 C5 122.4(5) . . ? C7 C6 C5 119.1(5) . . ? C8 C7 C6 119.2(5) . . ? C8 C7 H7A 120.4 . . ? C6 C7 H7A 120.4 . . ? N5 C8 C7 120.8(5) . . ? N5 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? N5 C9 C10 121.1(5) . . ? N5 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C9 C10 C6 119.2(5) . . ? C9 C10 H10A 120.4 . . ? C6 C10 H10A 120.4 . . ? C11 C11 C12 125.7(6) 3_544 . ? C11 C11 H11A 117.1 3_544 . ? C12 C11 H11A 117.1 . . ? C16 C12 C13 117.8(5) . . ? C16 C12 C11 118.9(4) . . ? C13 C12 C11 123.2(5) . . ? C14 C13 C12 119.7(5) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? N6 C14 C13 120.3(5) . . ? N6 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? N6 C15 C16 119.7(5) . . ? N6 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C15 C16 C12 120.3(5) . . ? C15 C16 H16A 119.8 . . ? C12 C16 H16A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.571 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.684 _refine_diff_density_max 0.376 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.060 # Attachment '- compound4.cif' data_shelxle_4 _database_code_depnum_ccdc_archive 'CCDC 874865' #TrackingRef '- compound4.cif' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '20 August 2008' #========================================================================== #========================================================================== #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 Fe N6 S6, 4(C12 H11 N2), 4(H2 O)' _chemical_formula_sum 'C54 H52 Fe N14 O4 S6' _chemical_formula_weight 1209.31 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' Fe Fe 0.3463 0.8444 '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' S S 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.756(7) _cell_length_b 12.820(6) _cell_length_c 16.142(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.053(13) _cell_angle_gamma 90.00 _cell_volume 3007(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2257 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 28.1 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.515 _exptl_absorpt_correction_type 'Multi Scan' _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 0.896 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device 'Mercury (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30366 _diffrn_reflns_av_R_equivalents 0.1201 _diffrn_reflns_av_sigmaI/netI 0.1053 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.15 _reflns_number_total 6016 _reflns_number_gt 2993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _computing_publication_material ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003). ; _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^)+(0.1460P)^2^+1.2553P] 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 6016 _refine_ls_number_parameters 520 _refine_ls_number_restraints 894 _refine_ls_R_factor_all 0.2002 _refine_ls_R_factor_gt 0.1100 _refine_ls_wR_factor_ref 0.3234 _refine_ls_wR_factor_gt 0.2647 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.026 _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 Fe1A Fe 0.5000 0.0000 1.0000 0.0656(4) Uani 1 2 d S . . S1 S 0.27099(15) -0.02606(17) 1.17883(14) 0.1079(7) Uani 1 1 d . . . S3 S 0.30685(14) -0.22362(15) 0.80342(12) 0.1004(7) Uani 1 1 d . . . S2 S 0.38751(13) 0.29647(15) 0.82883(12) 0.0956(6) Uani 1 1 d . . . C1 C 0.3483(4) -0.0098(4) 1.1213(4) 0.0723(16) Uani 1 1 d . . . C2 C 0.4181(4) 0.1996(5) 0.8900(4) 0.0725(16) Uani 1 1 d . . . C3 C 0.3695(4) -0.1465(5) 0.8709(4) 0.0690(15) Uani 1 1 d . . . O1WA O 0.1034(4) 0.0260(5) 0.5954(4) 0.1093(16) Uani 1 1 d . . . H2W1 H 0.0862 -0.0171 0.6296 0.13(3) Uiso 1 1 d R . . H1W1 H 0.1235 -0.0297 0.5765 0.32(10) Uiso 1 1 d R . . O2WA O 0.0231(4) 0.8189(6) 0.4746(4) 0.1238(18) Uani 1 1 d . . . H1W2 H -0.0040 0.8690 0.4946 0.13(4) Uiso 1 1 d R . . H2W2 H 0.0354 0.7903 0.5228 0.16(4) Uiso 1 1 d R . . N2 N 0.4406(3) 0.1290(4) 0.9356(3) 0.0784(14) Uani 1 1 d . . . N3 N 0.4142(4) -0.0947(4) 0.9180(3) 0.0817(15) Uani 1 1 d . . . N1 N 0.4034(4) 0.0026(4) 1.0780(3) 0.0780(14) Uani 1 1 d . . . C5 C 0.2871(10) 0.2568(9) 0.5511(7) 0.071(3) Uani 0.576(14) 1 d PU A 1 H5A H 0.3228 0.3063 0.5296 0.085 Uiso 0.576(14) 1 calc PR A 1 C4 C 0.1943(11) 0.2679(12) 0.5288(9) 0.079(3) Uani 0.576(14) 1 d PU A 1 H4A H 0.1573 0.2186 0.5488 0.095 Uiso 0.576(14) 1 calc PR A 1 C6 C 0.1489(8) 0.3512(9) 0.4760(10) 0.077(3) Uani 0.576(14) 1 d PGU A 1 N4 N 0.0533(8) 0.3501(10) 0.4646(12) 0.084(3) Uani 0.576(14) 1 d PGU A 1 C7 C 0.0029(5) 0.4293(12) 0.4192(13) 0.093(3) Uani 0.576(14) 1 d PGU A 1 H7A H -0.0610 0.4285 0.4116 0.112 Uiso 0.576(14) 1 calc PR A 1 C8 C 0.0480(8) 0.5095(10) 0.3851(12) 0.093(3) Uani 0.576(14) 1 d PGU A 1 H8A H 0.0142 0.5625 0.3547 0.112 Uiso 0.576(14) 1 calc PR A 1 C9 C 0.1436(8) 0.5106(9) 0.3964(10) 0.099(4) Uani 0.576(14) 1 d PGU A 1 H9A H 0.1737 0.5642 0.3736 0.119 Uiso 0.576(14) 1 calc PR A 1 C10 C 0.1940(5) 0.4314(10) 0.4419(10) 0.089(3) Uani 0.576(14) 1 d PGU A 1 H10A H 0.2580 0.4321 0.4495 0.107 Uiso 0.576(14) 1 calc PR A 1 C11 C 0.3353(8) 0.1798(9) 0.6023(8) 0.071(3) Uani 0.576(14) 1 d PGU A 1 N5 N 0.2846(5) 0.1022(10) 0.6334(9) 0.071(3) Uani 0.576(14) 1 d PGU A 1 H5B H 0.2257 0.1008 0.6190 0.085 Uiso 0.576(14) 1 calc PR A 1 C12 C 0.3292(7) 0.0268(9) 0.6877(9) 0.073(3) Uani 0.576(14) 1 d PGU A 1 H12A H 0.2953 -0.0251 0.7085 0.088 Uiso 0.576(14) 1 calc PR A 1 C13 C 0.4244(7) 0.0291(9) 0.7109(8) 0.075(3) Uani 0.576(14) 1 d PGU A 1 H13A H 0.4542 -0.0213 0.7472 0.090 Uiso 0.576(14) 1 calc PR A 1 C14 C 0.4751(5) 0.1067(11) 0.6798(9) 0.079(3) Uani 0.576(14) 1 d PGU A 1 H14A H 0.5388 0.1082 0.6953 0.095 Uiso 0.576(14) 1 calc PR A 1 C15 C 0.4306(8) 0.1820(9) 0.6255(9) 0.081(3) Uani 0.576(14) 1 d PGU A 1 H15A H 0.4645 0.2340 0.6047 0.098 Uiso 0.576(14) 1 calc PR A 1 C4A C 0.2386(13) 0.3089(13) 0.5131(10) 0.073(3) Uani 0.424(14) 1 d PU A 2 H4AA H 0.2983 0.3283 0.5087 0.087 Uiso 0.424(14) 1 calc PR A 2 C5A C 0.2323(15) 0.2314(14) 0.5563(11) 0.068(3) Uani 0.424(14) 1 d PU A 2 H5AA H 0.1727 0.2082 0.5570 0.082 Uiso 0.424(14) 1 calc PR A 2 C6A C 0.1657(10) 0.3753(14) 0.4674(15) 0.082(4) Uani 0.424(14) 1 d PGU A 2 N4A N 0.0755(12) 0.3420(13) 0.4639(17) 0.082(3) Uani 0.424(14) 1 d PGU A 2 C7A C 0.0031(8) 0.4015(15) 0.4216(19) 0.092(4) Uani 0.424(14) 1 d PGU A 2 H7AA H -0.0572 0.3792 0.4192 0.111 Uiso 0.424(14) 1 calc PR A 2 C8A C 0.0210(11) 0.4942(14) 0.3828(17) 0.094(4) Uani 0.424(14) 1 d PGU A 2 H8AA H -0.0274 0.5339 0.3545 0.113 Uiso 0.424(14) 1 calc PR A 2 C9A C 0.1113(13) 0.5275(12) 0.3863(14) 0.100(5) Uani 0.424(14) 1 d PGU A 2 H9AA H 0.1232 0.5895 0.3603 0.120 Uiso 0.424(14) 1 calc PR A 2 C10A C 0.1836(9) 0.4681(15) 0.4286(14) 0.094(4) Uani 0.424(14) 1 d PGU A 2 H10B H 0.2440 0.4903 0.4309 0.113 Uiso 0.424(14) 1 calc PR A 2 C11A C 0.3084(9) 0.1681(13) 0.6087(13) 0.069(3) Uani 0.424(14) 1 d PGU A 2 N5A N 0.2878(8) 0.0750(14) 0.6455(15) 0.075(4) Uani 0.424(14) 1 d PGU A 2 H5AB H 0.2317 0.0539 0.6394 0.090 Uiso 0.424(14) 1 calc PR A 2 C12A C 0.3578(13) 0.0161(11) 0.6921(14) 0.077(4) Uani 0.424(14) 1 d PGU A 2 H12B H 0.3440 -0.0462 0.7167 0.093 Uiso 0.424(14) 1 calc PR A 2 C13A C 0.4485(10) 0.0503(13) 0.7019(13) 0.079(4) Uani 0.424(14) 1 d PGU A 2 H13B H 0.4953 0.0109 0.7330 0.094 Uiso 0.424(14) 1 calc PR A 2 C14A C 0.4691(7) 0.1434(14) 0.6651(13) 0.083(4) Uani 0.424(14) 1 d PGU A 2 H14B H 0.5297 0.1662 0.6716 0.100 Uiso 0.424(14) 1 calc PR A 2 C15A C 0.3991(11) 0.2023(11) 0.6185(12) 0.080(4) Uani 0.424(14) 1 d PGU A 2 H15B H 0.4129 0.2646 0.5939 0.096 Uiso 0.424(14) 1 calc PR A 2 C16 C 0.1195(10) 1.0338(11) 0.3788(9) 0.070(3) Uani 0.526(13) 1 d PU B 1 H16A H 0.0822 0.9879 0.4022 0.084 Uiso 0.526(13) 1 calc PR B 1 C17 C 0.2118(10) 1.0173(10) 0.3954(8) 0.066(3) Uani 0.526(13) 1 d PU B 1 H17A H 0.2471 1.0620 0.3685 0.079 Uiso 0.526(13) 1 calc PR B 1 C18 C 0.0756(9) 1.1175(10) 0.3275(10) 0.074(3) Uani 0.526(13) 1 d PGU B 1 N7 N -0.0190(9) 1.1257(11) 0.3235(11) 0.080(3) Uani 0.526(13) 1 d PGU B 1 C19 C -0.0668(6) 1.2088(13) 0.2810(13) 0.094(4) Uani 0.526(13) 1 d PGU B 1 H19A H -0.1301 1.2143 0.2783 0.112 Uiso 0.526(13) 1 calc PR B 1 C20 C -0.0200(10) 1.2836(10) 0.2426(11) 0.098(4) Uani 0.526(13) 1 d PGU B 1 H20A H -0.0520 1.3392 0.2141 0.117 Uiso 0.526(13) 1 calc PR B 1 C21 C 0.0746(10) 1.2754(10) 0.2466(10) 0.097(4) Uani 0.526(13) 1 d PGU B 1 H21A H 0.1059 1.3255 0.2209 0.116 Uiso 0.526(13) 1 calc PR B 1 C22 C 0.1224(6) 1.1923(12) 0.2891(10) 0.086(3) Uani 0.526(13) 1 d PGU B 1 H22A H 0.1857 1.1868 0.2918 0.104 Uiso 0.526(13) 1 calc PR B 1 C23 C 0.2620(9) 0.9401(10) 0.4489(9) 0.069(3) Uani 0.526(13) 1 d PGU B 1 N6 N 0.2088(6) 0.8684(11) 0.4838(10) 0.076(3) Uani 0.526(13) 1 d PGU B 1 H6A H 0.1498 0.8716 0.4720 0.091 Uiso 0.526(13) 1 calc PR B 1 C24 C 0.2511(8) 0.7914(11) 0.5378(12) 0.084(3) Uani 0.526(13) 1 d PGU B 1 H24A H 0.2156 0.7434 0.5611 0.101 Uiso 0.526(13) 1 calc PR B 1 C25 C 0.3466(9) 0.7862(12) 0.5569(12) 0.082(3) Uani 0.526(13) 1 d PGU B 1 H25A H 0.3749 0.7348 0.5930 0.099 Uiso 0.526(13) 1 calc PR B 1 C26 C 0.3997(6) 0.8580(12) 0.5221(12) 0.081(3) Uani 0.526(13) 1 d PGU B 1 H26A H 0.4636 0.8545 0.5349 0.097 Uiso 0.526(13) 1 calc PR B 1 C27 C 0.3574(8) 0.9349(10) 0.4681(11) 0.075(3) Uani 0.526(13) 1 d PGU B 1 H27A H 0.3930 0.9829 0.4447 0.090 Uiso 0.526(13) 1 calc PR B 1 C17A C 0.1594(12) 0.9888(12) 0.4067(9) 0.072(3) Uani 0.474(13) 1 d PU B 2 H17B H 0.0994 0.9705 0.4110 0.087 Uiso 0.474(13) 1 calc PR B 2 C16A C 0.1680(12) 1.0652(12) 0.3616(9) 0.073(3) Uani 0.474(13) 1 d PU B 2 H16B H 0.2280 1.0796 0.3548 0.088 Uiso 0.474(13) 1 calc PR B 2 C18A C 0.0992(8) 1.1351(13) 0.3180(12) 0.074(3) Uani 0.474(13) 1 d PGU B 2 N7A N 0.0095(10) 1.1112(11) 0.3267(12) 0.079(3) Uani 0.474(13) 1 d PGU B 2 C19A C -0.0631(7) 1.1725(13) 0.2873(13) 0.085(4) Uani 0.474(13) 1 d PGU B 2 H19B H -0.1231 1.1565 0.2932 0.102 Uiso 0.474(13) 1 calc PR B 2 C20A C -0.0460(9) 1.2578(11) 0.2391(13) 0.092(4) Uani 0.474(13) 1 d PGU B 2 H20B H -0.0945 1.2988 0.2128 0.110 Uiso 0.474(13) 1 calc PR B 2 C21A C 0.0437(12) 1.2817(12) 0.2303(12) 0.098(4) Uani 0.474(13) 1 d PGU B 2 H21B H 0.0552 1.3387 0.1981 0.118 Uiso 0.474(13) 1 calc PR B 2 C22A C 0.1163(8) 1.2204(14) 0.2698(12) 0.090(4) Uani 0.474(13) 1 d PGU B 2 H22B H 0.1764 1.2364 0.2639 0.108 Uiso 0.474(13) 1 calc PR B 2 C23A C 0.2337(8) 0.9224(11) 0.4552(10) 0.064(3) Uani 0.474(13) 1 d PGU B 2 N6A N 0.2070(7) 0.8376(13) 0.4989(12) 0.082(3) Uani 0.474(13) 1 d PGU B 2 H6AA H 0.1496 0.8228 0.4951 0.099 Uiso 0.474(13) 1 calc PR B 2 C24A C 0.2731(12) 0.7768(13) 0.5487(13) 0.091(4) Uani 0.474(13) 1 d PGU B 2 H24B H 0.2552 0.7200 0.5780 0.109 Uiso 0.474(13) 1 calc PR B 2 C25A C 0.3659(10) 0.8007(14) 0.5548(14) 0.085(4) Uani 0.474(13) 1 d PGU B 2 H25B H 0.4101 0.7600 0.5881 0.102 Uiso 0.474(13) 1 calc PR B 2 C26A C 0.3926(7) 0.8855(14) 0.5111(14) 0.087(4) Uani 0.474(13) 1 d PGU B 2 H26B H 0.4547 0.9015 0.5151 0.104 Uiso 0.474(13) 1 calc PR B 2 C27A C 0.3265(10) 0.9463(11) 0.4612(11) 0.074(3) Uani 0.474(13) 1 d PGU B 2 H27B H 0.3444 1.0030 0.4320 0.089 Uiso 0.474(13) 1 calc PR B 2 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 Fe1A 0.0435(7) 0.0740(8) 0.0780(8) -0.0050(6) 0.0071(5) 0.0054(5) S1 0.0968(15) 0.1257(16) 0.1123(15) 0.0110(12) 0.0490(12) 0.0049(11) S3 0.0905(14) 0.0927(13) 0.1046(13) -0.0023(10) -0.0197(10) -0.0108(9) S2 0.0821(13) 0.0996(13) 0.1050(13) 0.0148(10) 0.0159(10) 0.0298(10) C1 0.069(4) 0.076(4) 0.071(4) -0.007(3) 0.011(3) 0.019(3) C2 0.045(3) 0.089(4) 0.085(4) -0.009(4) 0.012(3) 0.010(3) C3 0.056(4) 0.075(4) 0.075(4) 0.009(3) 0.008(3) 0.004(3) O1WA 0.098(4) 0.113(4) 0.125(4) -0.002(3) 0.044(3) -0.017(3) O2WA 0.078(4) 0.160(5) 0.134(5) 0.023(5) 0.022(3) -0.016(4) N2 0.061(3) 0.080(3) 0.094(4) -0.005(3) 0.012(3) 0.007(3) N3 0.067(3) 0.083(4) 0.090(4) -0.010(3) 0.002(3) -0.006(3) N1 0.062(3) 0.088(4) 0.085(3) -0.002(3) 0.017(3) 0.013(3) C5 0.064(6) 0.069(6) 0.085(6) 0.006(4) 0.025(5) -0.013(5) C4 0.062(6) 0.083(7) 0.096(7) 0.009(5) 0.021(5) -0.012(5) C6 0.066(6) 0.080(6) 0.086(6) -0.002(5) 0.015(5) -0.007(5) N4 0.062(5) 0.092(6) 0.098(6) 0.001(5) 0.013(5) -0.006(5) C7 0.072(5) 0.099(8) 0.105(7) 0.017(7) 0.008(5) -0.008(5) C8 0.063(7) 0.104(7) 0.107(6) 0.029(6) -0.001(7) -0.010(6) C9 0.064(7) 0.105(7) 0.121(8) 0.034(6) -0.006(7) -0.005(6) C10 0.069(6) 0.086(8) 0.106(8) 0.020(6) -0.001(5) -0.006(5) C11 0.067(6) 0.073(5) 0.079(6) 0.004(4) 0.030(5) -0.004(5) N5 0.068(5) 0.067(7) 0.080(6) 0.017(5) 0.021(4) 0.003(4) C12 0.050(6) 0.081(6) 0.090(7) 0.017(5) 0.014(6) 0.010(5) C13 0.051(6) 0.085(6) 0.091(6) 0.005(5) 0.018(6) -0.014(5) C14 0.065(5) 0.074(8) 0.101(8) 0.006(6) 0.018(5) -0.010(5) C15 0.062(6) 0.080(7) 0.103(7) 0.004(5) 0.016(6) 0.004(5) C4A 0.062(6) 0.074(7) 0.084(7) 0.006(5) 0.017(6) -0.011(5) C5A 0.060(7) 0.065(7) 0.082(8) 0.004(5) 0.019(6) -0.015(6) C6A 0.068(6) 0.085(7) 0.088(7) 0.006(6) 0.003(6) -0.005(6) N4A 0.065(6) 0.088(6) 0.095(7) 0.004(6) 0.017(6) 0.004(5) C7A 0.073(6) 0.096(8) 0.105(7) 0.018(7) 0.008(6) 0.004(6) C8A 0.066(8) 0.105(8) 0.106(8) 0.022(7) -0.001(8) -0.007(7) C9A 0.069(9) 0.108(8) 0.115(8) 0.032(7) -0.009(9) -0.007(7) C10A 0.072(7) 0.094(9) 0.108(9) 0.026(7) -0.007(7) -0.009(6) C11A 0.059(6) 0.074(6) 0.077(7) 0.003(5) 0.021(6) -0.012(5) N5A 0.067(6) 0.073(8) 0.084(8) 0.008(6) 0.011(6) 0.003(5) C12A 0.059(8) 0.085(7) 0.090(7) 0.016(6) 0.017(7) 0.002(6) C13A 0.055(7) 0.083(9) 0.100(8) 0.010(7) 0.018(7) -0.001(7) C14A 0.070(6) 0.078(10) 0.100(9) 0.013(8) 0.011(6) -0.004(6) C15A 0.059(7) 0.081(7) 0.100(8) 0.007(6) 0.010(7) -0.007(6) C16 0.046(6) 0.079(6) 0.086(6) 0.008(5) 0.016(5) -0.009(5) C17 0.043(6) 0.080(6) 0.075(6) 0.004(5) 0.011(5) -0.013(4) C18 0.056(6) 0.088(6) 0.075(6) 0.003(5) 0.000(6) -0.009(5) N7 0.048(6) 0.096(7) 0.089(6) 0.004(5) -0.005(6) -0.002(5) C19 0.078(6) 0.099(10) 0.098(8) 0.023(8) -0.001(6) 0.001(6) C20 0.076(8) 0.115(8) 0.097(7) 0.025(7) -0.001(7) -0.003(7) C21 0.079(8) 0.116(7) 0.090(8) 0.027(6) 0.000(7) -0.004(7) C22 0.076(6) 0.096(8) 0.081(8) 0.024(6) -0.002(6) -0.008(5) C23 0.051(6) 0.071(6) 0.088(6) 0.001(5) 0.014(6) -0.002(5) N6 0.049(5) 0.078(8) 0.099(7) 0.011(5) 0.008(5) 0.000(4) C24 0.049(6) 0.090(7) 0.110(7) 0.019(5) 0.006(6) 0.015(5) C25 0.052(6) 0.085(7) 0.109(7) 0.014(5) 0.012(6) 0.003(5) C26 0.057(5) 0.073(8) 0.110(8) 0.018(6) 0.006(5) 0.003(5) C27 0.043(6) 0.081(7) 0.101(7) 0.008(5) 0.016(6) 0.012(5) C17A 0.051(7) 0.082(7) 0.082(7) 0.005(5) 0.008(6) -0.006(5) C16A 0.056(6) 0.085(7) 0.079(7) 0.003(5) 0.012(5) -0.014(5) C18A 0.062(6) 0.084(7) 0.074(7) 0.002(5) 0.004(6) -0.016(5) N7A 0.066(7) 0.088(6) 0.079(6) 0.014(5) -0.003(7) 0.001(6) C19A 0.071(6) 0.086(9) 0.089(7) 0.028(7) -0.008(6) 0.006(6) C20A 0.071(7) 0.097(8) 0.101(8) 0.032(7) -0.001(7) -0.012(7) C21A 0.070(9) 0.116(7) 0.098(8) 0.028(6) -0.011(8) -0.012(7) C22A 0.076(7) 0.101(8) 0.087(9) 0.023(6) -0.001(6) -0.008(6) C23A 0.040(6) 0.075(7) 0.080(6) -0.006(5) 0.017(5) -0.005(5) N6A 0.059(6) 0.085(8) 0.099(8) 0.016(6) 0.004(5) 0.003(5) C24A 0.055(7) 0.099(7) 0.116(8) 0.013(6) 0.006(7) 0.011(6) C25A 0.053(6) 0.085(7) 0.112(7) 0.004(6) 0.005(6) 0.010(6) C26A 0.054(6) 0.091(8) 0.112(8) 0.009(7) 0.006(6) 0.006(5) C27A 0.049(7) 0.080(7) 0.092(7) 0.003(5) 0.013(7) 0.004(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 Fe1A N1 2.060(6) 3_657 ? Fe1A N1 2.060(5) . ? Fe1A N3 2.060(6) . ? Fe1A N3 2.060(6) 3_657 ? Fe1A N2 2.066(6) . ? Fe1A N2 2.066(6) 3_657 ? S1 C1 1.606(7) . ? S3 C3 1.633(7) . ? S2 C2 1.601(7) . ? C1 N1 1.172(7) . ? C2 N2 1.178(7) . ? C3 N3 1.131(7) . ? O1WA H2W1 0.8499 . ? O1WA H1W1 0.8501 . ? O2WA H1W2 0.8500 . ? O2WA H2W2 0.8500 . ? C5 C4 1.36(2) . ? C5 C11 1.400(14) . ? C5 H5A 0.9300 . ? C4 C6 1.455(17) . ? C4 H4A 0.9300 . ? C6 N4 1.3900 . ? C6 C10 1.3900 . ? N4 C7 1.3900 . ? C7 C8 1.3900 . ? C7 H7A 0.9300 . ? C8 C9 1.3900 . ? C8 H8A 0.9300 . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 N5 1.3900 . ? C11 C15 1.3900 . ? N5 C12 1.3900 . ? N5 H5B 0.8600 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C4A C5A 1.23(3) . ? C4A C6A 1.47(2) . ? C4A H4AA 0.9300 . ? C5A C11A 1.52(2) . ? C5A H5AA 0.9300 . ? C6A N4A 1.3900 . ? C6A C10A 1.3900 . ? N4A C7A 1.3900 . ? C7A C8A 1.3900 . ? C7A H7AA 0.9300 . ? C8A C9A 1.3900 . ? C8A H8AA 0.9300 . ? C9A C10A 1.3900 . ? C9A H9AA 0.9300 . ? C10A H10B 0.9300 . ? C11A N5A 1.3900 . ? C11A C15A 1.3900 . ? N5A C12A 1.3900 . ? N5A H5AB 0.8600 . ? C12A C13A 1.3900 . ? C12A H12B 0.9300 . ? C13A C14A 1.3900 . ? C13A H13B 0.9300 . ? C14A C15A 1.3900 . ? C14A H14B 0.9300 . ? C15A H15B 0.9300 . ? C16 C17 1.36(2) . ? C16 C18 1.439(16) . ? C16 H16A 0.9300 . ? C17 C23 1.432(15) . ? C17 H17A 0.9300 . ? C18 N7 1.3900 . ? C18 C22 1.3900 . ? N7 C19 1.3900 . ? C19 C20 1.3900 . ? C19 H19A 0.9300 . ? C20 C21 1.3900 . ? C20 H20A 0.9300 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 N6 1.3900 . ? C23 C27 1.3900 . ? N6 C24 1.3900 . ? N6 H6A 0.8600 . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.3900 . ? C25 H25A 0.9300 . ? C26 C27 1.3900 . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C17A C16A 1.24(3) . ? C17A C23A 1.496(18) . ? C17A H17B 0.9300 . ? C16A C18A 1.442(18) . ? C16A H16B 0.9300 . ? C18A N7A 1.3900 . ? C18A C22A 1.3900 . ? N7A C19A 1.3900 . ? C19A C20A 1.3900 . ? C19A H19B 0.9300 . ? C20A C21A 1.3900 . ? C20A H20B 0.9300 . ? C21A C22A 1.3900 . ? C21A H21B 0.9300 . ? C22A H22B 0.9300 . ? C23A N6A 1.3900 . ? C23A C27A 1.3900 . ? N6A C24A 1.3900 . ? N6A H6AA 0.8600 . ? C24A C25A 1.3900 . ? C24A H24B 0.9300 . ? C25A C26A 1.3900 . ? C25A H25B 0.9300 . ? C26A C27A 1.3900 . ? C26A H26B 0.9300 . ? C27A H27B 0.9300 . ? 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 Fe1A N1 180.000(1) 3_657 . ? N1 Fe1A N3 90.6(2) 3_657 . ? N1 Fe1A N3 89.4(2) . . ? N1 Fe1A N3 89.4(2) 3_657 3_657 ? N1 Fe1A N3 90.6(2) . 3_657 ? N3 Fe1A N3 180.000(1) . 3_657 ? N1 Fe1A N2 89.05(19) 3_657 . ? N1 Fe1A N2 90.95(19) . . ? N3 Fe1A N2 89.4(2) . . ? N3 Fe1A N2 90.6(2) 3_657 . ? N1 Fe1A N2 90.95(19) 3_657 3_657 ? N1 Fe1A N2 89.05(19) . 3_657 ? N3 Fe1A N2 90.6(2) . 3_657 ? N3 Fe1A N2 89.4(2) 3_657 3_657 ? N2 Fe1A N2 180.000(1) . 3_657 ? N1 C1 S1 178.7(6) . . ? N2 C2 S2 179.4(6) . . ? N3 C3 S3 178.6(6) . . ? H2W1 O1WA H1W1 81.4 . . ? H1W2 O2WA H2W2 91.0 . . ? C2 N2 Fe1A 168.2(5) . . ? C3 N3 Fe1A 177.4(5) . . ? C1 N1 Fe1A 171.2(5) . . ? C4 C5 C11 127.9(14) . . ? C4 C5 H5A 116.0 . . ? C11 C5 H5A 116.0 . . ? C5 C4 C6 124.8(14) . . ? C5 C4 H4A 117.6 . . ? C6 C4 H4A 117.6 . . ? N4 C6 C10 120.0 . . ? N4 C6 C4 115.0(9) . . ? C10 C6 C4 124.9(9) . . ? C7 N4 C6 120.0 . . ? N4 C7 C8 120.0 . . ? N4 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 C6 120.0 . . ? C9 C10 H10A 120.0 . . ? C6 C10 H10A 120.0 . . ? N5 C11 C15 120.0 . . ? N5 C11 C5 117.9(9) . . ? C15 C11 C5 122.1(9) . . ? C12 N5 C11 120.0 . . ? C12 N5 H5B 120.0 . . ? C11 N5 H5B 120.0 . . ? N5 C12 C13 120.0 . . ? N5 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C11 120.0 . . ? C14 C15 H15A 120.0 . . ? C11 C15 H15A 120.0 . . ? C5A C4A C6A 129(2) . . ? C5A C4A H4AA 115.3 . . ? C6A C4A H4AA 115.3 . . ? C4A C5A C11A 129(2) . . ? C4A C5A H5AA 115.6 . . ? C11A C5A H5AA 115.6 . . ? N4A C6A C10A 120.0 . . ? N4A C6A C4A 117.1(13) . . ? C10A C6A C4A 122.9(13) . . ? C6A N4A C7A 120.0 . . ? C8A C7A N4A 120.0 . . ? C8A C7A H7AA 120.0 . . ? N4A C7A H7AA 120.0 . . ? C9A C8A C7A 120.0 . . ? C9A C8A H8AA 120.0 . . ? C7A C8A H8AA 120.0 . . ? C10A C9A C8A 120.0 . . ? C10A C9A H9AA 120.0 . . ? C8A C9A H9AA 120.0 . . ? C9A C10A C6A 120.0 . . ? C9A C10A H10B 120.0 . . ? C6A C10A H10B 120.0 . . ? N5A C11A C15A 120.0 . . ? N5A C11A C5A 120.1(13) . . ? C15A C11A C5A 119.9(13) . . ? C11A N5A C12A 120.0 . . ? C11A N5A H5AB 120.0 . . ? C12A N5A H5AB 120.0 . . ? C13A C12A N5A 120.0 . . ? C13A C12A H12B 120.0 . . ? N5A C12A H12B 120.0 . . ? C12A C13A C14A 120.0 . . ? C12A C13A H13B 120.0 . . ? C14A C13A H13B 120.0 . . ? C15A C14A C13A 120.0 . . ? C15A C14A H14B 120.0 . . ? C13A C14A H14B 120.0 . . ? C14A C15A C11A 120.0 . . ? C14A C15A H15B 120.0 . . ? C11A C15A H15B 120.0 . . ? C17 C16 C18 124.4(14) . . ? C17 C16 H16A 117.8 . . ? C18 C16 H16A 117.8 . . ? C16 C17 C23 128.4(14) . . ? C16 C17 H17A 115.8 . . ? C23 C17 H17A 115.8 . . ? N7 C18 C22 120.0 . . ? N7 C18 C16 115.5(10) . . ? C22 C18 C16 124.2(10) . . ? C18 N7 C19 120.0 . . ? C20 C19 N7 120.0 . . ? C20 C19 H19A 120.0 . . ? N7 C19 H19A 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C18 120.0 . . ? C21 C22 H22A 120.0 . . ? C18 C22 H22A 120.0 . . ? N6 C23 C27 120.0 . . ? N6 C23 C17 115.7(9) . . ? C27 C23 C17 124.3(9) . . ? C24 N6 C23 120.0 . . ? C24 N6 H6A 120.0 . . ? C23 N6 H6A 120.0 . . ? N6 C24 C25 120.0 . . ? N6 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C23 120.0 . . ? C26 C27 H27A 120.0 . . ? C23 C27 H27A 120.0 . . ? C16A C17A C23A 128.0(18) . . ? C16A C17A H17B 116.0 . . ? C23A C17A H17B 116.0 . . ? C17A C16A C18A 130.0(18) . . ? C17A C16A H16B 115.0 . . ? C18A C16A H16B 115.0 . . ? N7A C18A C22A 120.0 . . ? N7A C18A C16A 114.5(12) . . ? C22A C18A C16A 125.5(12) . . ? C18A N7A C19A 120.0 . . ? N7A C19A C20A 120.0 . . ? N7A C19A H19B 120.0 . . ? C20A C19A H19B 120.0 . . ? C21A C20A C19A 120.0 . . ? C21A C20A H20B 120.0 . . ? C19A C20A H20B 120.0 . . ? C20A C21A C22A 120.0 . . ? C20A C21A H21B 120.0 . . ? C22A C21A H21B 120.0 . . ? C21A C22A C18A 120.0 . . ? C21A C22A H22B 120.0 . . ? C18A C22A H22B 120.0 . . ? N6A C23A C27A 120.0 . . ? N6A C23A C17A 117.6(11) . . ? C27A C23A C17A 122.3(11) . . ? C23A N6A C24A 120.0 . . ? C23A N6A H6AA 120.0 . . ? C24A N6A H6AA 120.0 . . ? C25A C24A N6A 120.0 . . ? C25A C24A H24B 120.0 . . ? N6A C24A H24B 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25B 120.0 . . ? C26A C25A H25B 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26B 120.0 . . ? C25A C26A H26B 120.0 . . ? C26A C27A C23A 120.0 . . ? C26A C27A H27B 120.0 . . ? C23A C27A H27B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.817 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.710 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.095 # Attachment '- compound6.cif' data_shelxle_6 _database_code_depnum_ccdc_archive 'CCDC 874866' #TrackingRef '- compound6.cif' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '20 August 2011' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C13 H12 N), C4 Co N4 S4' _chemical_formula_sum 'C30 H24 Co N6 S4' _chemical_formula_weight 655.72 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 14.545(3) _cell_length_b 13.784(3) _cell_length_c 16.111(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.06(3) _cell_angle_gamma 90.00 _cell_volume 3170.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1439 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 28.00 _exptl_crystal_description plate _exptl_crystal_colour 'dark Blue' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type 'Multi Scan' _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_T_max 0.827 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device 'Mercury (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25646 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6036 _reflns_number_gt 2685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _computing_publication_material ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003). ; _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^)+(0.0603P)^2^+4.4525P] 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 6036 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1881 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2284 _refine_ls_wR_factor_gt 0.1792 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 Co1 Co 0.29665(7) 0.56622(7) 0.10533(6) 0.0896(4) Uani 1 1 d . . . S2 S 0.39010(18) 0.88621(14) 0.17803(13) 0.1126(8) Uani 1 1 d . . . S3 S -0.01431(17) 0.55079(15) 0.14602(17) 0.1204(8) Uani 1 1 d . . . S4 S 0.46802(18) 0.35212(16) 0.30232(14) 0.1172(8) Uani 1 1 d . . . S1 S 0.41113(18) 0.49553(16) -0.13834(16) 0.1189(8) Uani 1 1 d . . . C1 C 0.1300(6) 0.9433(6) 0.0120(6) 0.122(3) Uani 1 1 d . . . H1A H 0.1558 0.9282 0.0679 0.146 Uiso 1 1 calc R . . C2 C 0.1321(6) 1.0343(6) -0.0120(6) 0.120(3) Uani 1 1 d . . . H2A H 0.1079 1.0476 -0.0685 0.143 Uiso 1 1 calc R . . C3 C 0.0886(5) 0.8626(5) -0.0454(5) 0.086(2) Uani 1 1 d . . . C4 C 0.0520(5) 0.8729(6) -0.1304(6) 0.103(2) Uani 1 1 d . . . H4A H 0.0504 0.9337 -0.1556 0.124 Uiso 1 1 calc R . . C5 C 0.0187(5) 0.7954(6) -0.1768(5) 0.102(2) Uani 1 1 d . . . H5A H -0.0067 0.8030 -0.2340 0.123 Uiso 1 1 calc R . . C6 C 0.0568(6) 0.6947(5) -0.0618(6) 0.099(2) Uani 1 1 d . . . H6A H 0.0586 0.6325 -0.0392 0.119 Uiso 1 1 calc R . . C7 C 0.0910(6) 0.7697(5) -0.0107(5) 0.097(2) Uani 1 1 d . . . H7A H 0.1156 0.7595 0.0463 0.117 Uiso 1 1 calc R . . C8 C 0.1687(5) 1.1164(5) 0.0416(6) 0.089(2) Uani 1 1 d . . . C9 C 0.2055(6) 1.1081(6) 0.1248(6) 0.099(2) Uani 1 1 d . . . H9A H 0.2097 1.0477 0.1510 0.119 Uiso 1 1 calc R . . C10 C 0.2365(6) 1.1900(8) 0.1701(6) 0.114(3) Uani 1 1 d . . . H10A H 0.2639 1.1850 0.2270 0.137 Uiso 1 1 calc R . . C11 C 0.2273(7) 1.2780(7) 0.1321(8) 0.126(3) Uani 1 1 d . . . H11A H 0.2445 1.3335 0.1642 0.151 Uiso 1 1 calc R . . C12 C 0.1936(7) 1.2864(7) 0.0481(7) 0.124(3) Uani 1 1 d . . . H12A H 0.1909 1.3467 0.0218 0.149 Uiso 1 1 calc R . . C13 C 0.1638(6) 1.2057(6) 0.0029(6) 0.113(3) Uani 1 1 d . . . H13A H 0.1398 1.2107 -0.0547 0.136 Uiso 1 1 calc R . . C14 C 0.6484(5) 1.0185(7) 0.0694(6) 0.109(3) Uani 1 1 d . . . H14A H 0.6522 1.0335 0.0138 0.131 Uiso 1 1 calc R . . C15 C 0.6181(6) 0.9364(7) 0.0823(7) 0.120(3) Uani 1 1 d . . . H15A H 0.6166 0.9199 0.1380 0.144 Uiso 1 1 calc R . . C16 C 0.5838(4) 0.8614(5) 0.0149(5) 0.0814(19) Uani 1 1 d . . . C17 C 0.5721(5) 0.8775(5) -0.0706(6) 0.092(2) Uani 1 1 d . . . H17A H 0.5871 0.9374 -0.0910 0.111 Uiso 1 1 calc R . . C18 C 0.5384(5) 0.8044(7) -0.1254(5) 0.101(2) Uani 1 1 d . . . H18A H 0.5296 0.8147 -0.1835 0.121 Uiso 1 1 calc R . . C19 C 0.5275(6) 0.7023(6) -0.0147(7) 0.106(3) Uani 1 1 d . . . H19A H 0.5103 0.6425 0.0041 0.128 Uiso 1 1 calc R . . C20 C 0.5621(5) 0.7716(6) 0.0422(5) 0.096(2) Uani 1 1 d . . . H20A H 0.5712 0.7583 0.0998 0.115 Uiso 1 1 calc R . . C21 C 0.6788(5) 1.0945(6) 0.1335(6) 0.088(2) Uani 1 1 d . . . C22 C 0.6871(6) 1.0860(6) 0.2202(6) 0.112(3) Uani 1 1 d . . . H22A H 0.6766 1.0266 0.2440 0.135 Uiso 1 1 calc R . . C23 C 0.7104(6) 1.1640(8) 0.2700(6) 0.124(3) Uani 1 1 d . . . H23A H 0.7141 1.1575 0.3280 0.149 Uiso 1 1 calc R . . C24 C 0.7286(6) 1.2509(7) 0.2389(8) 0.122(3) Uani 1 1 d . . . H24A H 0.7438 1.3037 0.2748 0.146 Uiso 1 1 calc R . . C25 C 0.7245(6) 1.2607(6) 0.1524(8) 0.117(3) Uani 1 1 d . . . H25A H 0.7390 1.3196 0.1298 0.141 Uiso 1 1 calc R . . C26 C 0.6992(5) 1.1836(7) 0.1019(5) 0.097(2) Uani 1 1 d . . . H26A H 0.6954 1.1905 0.0439 0.116 Uiso 1 1 calc R . . C27 C 0.3561(6) 0.5111(5) -0.0591(6) 0.093(2) Uani 1 1 d . . . C28 C 0.3560(5) 0.7790(5) 0.1439(4) 0.087(2) Uani 1 1 d . . . C29 C 0.0893(6) 0.5530(5) 0.1282(5) 0.085(2) Uani 1 1 d . . . C30 C 0.4124(5) 0.4342(5) 0.2402(4) 0.0812(19) Uani 1 1 d . . . N1 N 0.3194(5) 0.5224(5) -0.0041(4) 0.100(2) Uani 1 1 d . . . N2 N 0.3327(5) 0.7026(4) 0.1203(4) 0.0976(19) Uani 1 1 d . . . N3 N 0.3707(4) 0.4905(4) 0.1953(4) 0.0957(18) Uani 1 1 d . . . N4 N 0.1642(5) 0.5554(4) 0.1157(4) 0.097(2) Uani 1 1 d . . . N5 N 0.0216(4) 0.7073(5) -0.1417(5) 0.1005(19) Uani 1 1 d . . . H5B H 0.0000 0.6582 -0.1723 0.121 Uiso 1 1 calc R . . N6 N 0.5180(4) 0.7183(5) -0.0958(5) 0.100(2) Uani 1 1 d . . . H6B H 0.4982 0.6724 -0.1308 0.120 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 Co1 0.0976(8) 0.0771(7) 0.0913(8) 0.0032(5) 0.0112(5) -0.0060(5) S2 0.161(2) 0.0694(12) 0.0981(16) 0.0092(10) 0.0020(14) -0.0078(12) S3 0.1046(19) 0.0930(15) 0.167(2) 0.0078(14) 0.0354(16) 0.0013(11) S4 0.147(2) 0.1067(16) 0.0876(15) 0.0035(12) -0.0037(13) 0.0152(13) S1 0.143(2) 0.1003(16) 0.1190(19) -0.0159(13) 0.0382(16) -0.0180(13) C1 0.153(9) 0.092(6) 0.114(7) 0.006(5) 0.009(6) 0.010(5) C2 0.155(9) 0.101(6) 0.102(7) 0.009(5) 0.023(6) -0.018(5) C3 0.095(6) 0.074(5) 0.086(5) -0.011(4) 0.005(4) 0.004(4) C4 0.099(6) 0.084(5) 0.116(7) -0.005(5) -0.006(5) 0.007(4) C5 0.099(6) 0.105(6) 0.091(6) 0.010(5) -0.013(4) 0.003(5) C6 0.112(6) 0.080(5) 0.104(7) -0.001(5) 0.017(5) -0.012(4) C7 0.123(7) 0.087(5) 0.077(5) 0.005(4) 0.011(4) 0.002(4) C8 0.093(6) 0.072(5) 0.102(6) -0.012(4) 0.016(5) 0.001(4) C9 0.111(7) 0.087(5) 0.106(7) 0.006(5) 0.036(5) 0.001(4) C10 0.101(7) 0.142(8) 0.100(7) -0.006(6) 0.025(5) 0.000(6) C11 0.113(8) 0.104(7) 0.158(10) -0.030(7) 0.014(7) -0.014(5) C12 0.129(8) 0.098(7) 0.136(9) 0.010(6) 0.002(6) -0.019(5) C13 0.119(7) 0.089(6) 0.125(7) 0.007(5) 0.007(5) -0.003(5) C14 0.093(6) 0.107(6) 0.126(8) -0.002(6) 0.018(5) 0.016(5) C15 0.088(6) 0.108(7) 0.165(9) 0.016(6) 0.030(6) 0.018(5) C16 0.059(4) 0.082(5) 0.099(6) -0.011(4) 0.005(4) 0.005(3) C17 0.089(6) 0.075(5) 0.122(7) 0.003(5) 0.041(5) 0.012(4) C18 0.081(6) 0.126(7) 0.092(6) -0.009(5) 0.008(4) 0.019(5) C19 0.101(7) 0.091(6) 0.128(8) 0.006(6) 0.026(6) -0.012(4) C20 0.100(6) 0.091(5) 0.095(6) -0.003(5) 0.013(4) -0.011(4) C21 0.061(4) 0.089(5) 0.107(7) -0.026(5) -0.001(4) -0.004(3) C22 0.134(8) 0.086(6) 0.107(7) -0.013(5) -0.001(6) -0.009(5) C23 0.127(8) 0.132(8) 0.107(7) -0.020(6) 0.004(5) -0.001(6) C24 0.110(7) 0.085(6) 0.159(10) -0.035(6) -0.005(6) -0.007(5) C25 0.099(7) 0.092(6) 0.155(9) 0.009(6) 0.009(6) 0.006(5) C26 0.076(5) 0.110(6) 0.103(6) -0.003(5) 0.011(4) 0.013(4) C27 0.088(6) 0.074(5) 0.109(7) 0.020(5) -0.004(5) -0.020(4) C28 0.103(6) 0.086(5) 0.066(5) 0.015(4) 0.006(4) -0.001(4) C29 0.098(6) 0.067(4) 0.086(6) 0.000(3) 0.007(5) 0.002(4) C30 0.088(5) 0.085(5) 0.069(5) -0.018(4) 0.010(4) -0.003(4) N1 0.111(6) 0.098(5) 0.093(5) 0.000(4) 0.028(4) -0.009(4) N2 0.114(5) 0.080(4) 0.097(5) -0.001(3) 0.016(4) -0.014(3) N3 0.092(5) 0.094(4) 0.097(5) 0.008(4) 0.009(4) 0.011(3) N4 0.102(5) 0.087(4) 0.097(5) 0.005(3) 0.008(4) 0.000(4) N5 0.096(5) 0.106(5) 0.095(5) -0.016(4) 0.006(4) -0.015(4) N6 0.077(4) 0.087(5) 0.134(7) -0.022(4) 0.018(4) 0.002(3) _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 Co1 N3 1.937(6) . ? Co1 N1 1.950(7) . ? Co1 N2 1.955(6) . ? Co1 N4 1.971(8) . ? S2 C28 1.621(8) . ? S3 C29 1.587(9) . ? S4 C30 1.620(8) . ? S1 C27 1.646(10) . ? C1 C2 1.313(10) . ? C1 C3 1.498(10) . ? C1 H1A 0.9300 . ? C2 C8 1.461(10) . ? C2 H2A 0.9300 . ? C3 C4 1.378(9) . ? C3 C7 1.395(9) . ? C4 C5 1.339(10) . ? C4 H4A 0.9300 . ? C5 N5 1.338(9) . ? C5 H5A 0.9300 . ? C6 N5 1.302(9) . ? C6 C7 1.355(9) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.348(10) . ? C8 C13 1.376(10) . ? C9 C10 1.373(11) . ? C9 H9A 0.9300 . ? C10 C11 1.353(11) . ? C10 H10A 0.9300 . ? C11 C12 1.353(11) . ? C11 H11A 0.9300 . ? C12 C13 1.355(10) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.246(10) . ? C14 C21 1.477(10) . ? C14 H14A 0.9300 . ? C15 C16 1.513(11) . ? C15 H15A 0.9300 . ? C16 C20 1.371(9) . ? C16 C17 1.373(10) . ? C17 C18 1.368(10) . ? C17 H17A 0.9300 . ? C18 N6 1.333(9) . ? C18 H18A 0.9300 . ? C19 N6 1.305(9) . ? C19 C20 1.353(10) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C26 1.384(10) . ? C21 C22 1.383(10) . ? C22 C23 1.345(11) . ? C22 H22A 0.9300 . ? C23 C24 1.344(12) . ? C23 H23A 0.9300 . ? C24 C25 1.389(12) . ? C24 H24A 0.9300 . ? C25 C26 1.346(11) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 N1 1.130(9) . ? C28 N2 1.148(8) . ? C29 N4 1.146(9) . ? C30 N3 1.151(8) . ? N5 H5B 0.8600 . ? N6 H6B 0.8600 . ? 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 N3 Co1 N1 110.0(3) . . ? N3 Co1 N2 109.2(3) . . ? N1 Co1 N2 108.7(3) . . ? N3 Co1 N4 108.0(3) . . ? N1 Co1 N4 113.0(3) . . ? N2 Co1 N4 107.8(3) . . ? C2 C1 C3 123.8(9) . . ? C2 C1 H1A 118.1 . . ? C3 C1 H1A 118.1 . . ? C1 C2 C8 126.3(9) . . ? C1 C2 H2A 116.9 . . ? C8 C2 H2A 116.9 . . ? C4 C3 C7 117.9(7) . . ? C4 C3 C1 124.8(7) . . ? C7 C3 C1 117.2(7) . . ? C5 C4 C3 120.1(8) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? N5 C5 C4 120.6(8) . . ? N5 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? N5 C6 C7 121.9(7) . . ? N5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C6 C7 C3 118.6(7) . . ? C6 C7 H7A 120.7 . . ? C3 C7 H7A 120.7 . . ? C9 C8 C13 120.2(7) . . ? C9 C8 C2 123.5(8) . . ? C13 C8 C2 116.4(8) . . ? C8 C9 C10 119.0(8) . . ? C8 C9 H9A 120.5 . . ? C10 C9 H9A 120.5 . . ? C11 C10 C9 120.2(9) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C12 C11 C10 120.9(9) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C13 C12 C11 119.0(9) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C12 C13 C8 120.5(9) . . ? C12 C13 H13A 119.7 . . ? C8 C13 H13A 119.7 . . ? C15 C14 C21 126.5(10) . . ? C15 C14 H14A 116.8 . . ? C21 C14 H14A 116.8 . . ? C14 C15 C16 125.4(10) . . ? C14 C15 H15A 117.3 . . ? C16 C15 H15A 117.3 . . ? C20 C16 C17 118.4(7) . . ? C20 C16 C15 116.8(8) . . ? C17 C16 C15 124.8(8) . . ? C18 C17 C16 119.3(7) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? N6 C18 C17 120.0(8) . . ? N6 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? N6 C19 C20 120.9(8) . . ? N6 C19 H19A 119.5 . . ? C20 C19 H19A 119.5 . . ? C19 C20 C16 119.9(8) . . ? C19 C20 H20A 120.0 . . ? C16 C20 H20A 120.0 . . ? C26 C21 C22 117.5(7) . . ? C26 C21 C14 115.4(9) . . ? C22 C21 C14 127.1(8) . . ? C23 C22 C21 119.9(8) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C24 C23 C22 122.3(10) . . ? C24 C23 H23A 118.8 . . ? C22 C23 H23A 118.8 . . ? C23 C24 C25 119.2(8) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C26 C25 C24 118.9(9) . . ? C26 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C25 C26 C21 122.1(8) . . ? C25 C26 H26A 118.9 . . ? C21 C26 H26A 118.9 . . ? N1 C27 S1 179.0(8) . . ? N2 C28 S2 179.2(8) . . ? N4 C29 S3 179.4(8) . . ? N3 C30 S4 177.9(7) . . ? C27 N1 Co1 160.0(7) . . ? C28 N2 Co1 168.1(6) . . ? C30 N3 Co1 169.8(6) . . ? C29 N4 Co1 174.1(7) . . ? C6 N5 C5 120.9(7) . . ? C6 N5 H5B 119.5 . . ? C5 N5 H5B 119.5 . . ? C19 N6 C18 121.4(7) . . ? C19 N6 H6B 119.3 . . ? C18 N6 H6B 119.3 . . ? _diffrn_measured_fraction_theta_max 0.789 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.516 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.060 # Attachment '- compound7.cif' data_shelxle_7 _database_code_depnum_ccdc_archive 'CCDC 874867' #TrackingRef '- compound7.cif' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '20 August 2008' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C13 H12 N), Cl4 Zn' _chemical_formula_sum 'C26 H24 Cl4 N2 Zn' _chemical_formula_weight 571.64 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.956(3) _cell_length_b 13.690(3) _cell_length_c 13.951(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.09(3) _cell_angle_gamma 90.00 _cell_volume 2632.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 964 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.96 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.356 _exptl_absorpt_correction_type 'Multi Scan' _exptl_absorpt_correction_T_min 0.599 _exptl_absorpt_correction_T_max 0.737 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device 'Mercury (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14045 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.96 _reflns_number_total 2618 _reflns_number_gt 2201 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _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^)+(0.0459P)^2^+2.7775P] 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 2618 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Zn1 Zn 0.5000 0.25833(3) 0.2500 0.04924(16) Uani 1 2 d S . . Cl2 Cl 0.38759(5) 0.16205(5) 0.15884(6) 0.0673(2) Uani 1 1 d . . . Cl1 Cl 0.58654(5) 0.34961(5) 0.15851(5) 0.0570(2) Uani 1 1 d . . . C1 C 0.3714(2) -0.1322(2) 0.0024(2) 0.0603(7) Uani 1 1 d . . . H1A H 0.3916 -0.1925 -0.0177 0.072 Uiso 1 1 calc R . . C2 C 0.4337(2) -0.0834(2) 0.0647(2) 0.0595(7) Uani 1 1 d . . . H2A H 0.4138 -0.0231 0.0852 0.071 Uiso 1 1 calc R . . C3 C 0.53189(19) -0.1160(2) 0.10483(19) 0.0538(6) Uani 1 1 d . . . C4 C 0.5724(2) -0.2046(3) 0.0821(2) 0.0699(8) Uani 1 1 d . . . H4A H 0.5365 -0.2474 0.0386 0.084 Uiso 1 1 calc R . . C5 C 0.6640(3) -0.2284(3) 0.1233(3) 0.0825(10) Uani 1 1 d . . . H5A H 0.6908 -0.2875 0.1081 0.099 Uiso 1 1 calc R . . C6 C 0.6806(2) -0.0823(3) 0.2098(2) 0.0750(9) Uani 1 1 d . . . H6A H 0.7183 -0.0415 0.2539 0.090 Uiso 1 1 calc R . . C7 C 0.5888(2) -0.0550(3) 0.1697(2) 0.0651(7) Uani 1 1 d . . . H7A H 0.5644 0.0048 0.1861 0.078 Uiso 1 1 calc R . . C8 C 0.27237(18) -0.1006(2) -0.03889(19) 0.0540(6) Uani 1 1 d . . . C9 C 0.2195(2) -0.1596(2) -0.1076(3) 0.0753(9) Uani 1 1 d . . . H9A H 0.2470 -0.2173 -0.1257 0.090 Uiso 1 1 calc R . . C10 C 0.1270(2) -0.1353(3) -0.1500(3) 0.0833(10) Uani 1 1 d . . . H10A H 0.0930 -0.1762 -0.1967 0.100 Uiso 1 1 calc R . . C11 C 0.0845(2) -0.0512(3) -0.1242(2) 0.0710(8) Uani 1 1 d . . . H11A H 0.0220 -0.0346 -0.1531 0.085 Uiso 1 1 calc R . . C12 C 0.1353(2) 0.0082(2) -0.0549(2) 0.0690(8) Uani 1 1 d . . . H12A H 0.1069 0.0652 -0.0364 0.083 Uiso 1 1 calc R . . C13 C 0.2284(2) -0.0161(2) -0.0125(2) 0.0633(7) Uani 1 1 d . . . H13A H 0.2620 0.0247 0.0344 0.076 Uiso 1 1 calc R . . N1 N 0.71566(18) -0.1675(3) 0.1855(2) 0.0782(9) Uani 1 1 d . . . H1B H 0.7737 -0.1838 0.2108 0.094 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 Zn1 0.0348(2) 0.0500(3) 0.0599(3) 0.000 -0.00194(17) 0.000 Cl2 0.0471(4) 0.0600(4) 0.0872(5) -0.0228(3) -0.0130(3) 0.0033(3) Cl1 0.0453(4) 0.0609(4) 0.0646(4) 0.0123(3) 0.0076(3) 0.0082(3) C1 0.0528(16) 0.0609(17) 0.0653(17) -0.0023(13) 0.0032(13) 0.0115(13) C2 0.0507(16) 0.0641(17) 0.0622(16) -0.0006(13) 0.0039(12) 0.0086(13) C3 0.0400(13) 0.0691(17) 0.0521(14) 0.0095(12) 0.0065(11) 0.0081(12) C4 0.0550(18) 0.078(2) 0.0732(19) -0.0056(16) -0.0014(14) 0.0128(16) C5 0.056(2) 0.095(3) 0.095(3) 0.005(2) 0.0053(18) 0.0256(19) C6 0.0543(19) 0.106(3) 0.0613(18) 0.0065(17) -0.0007(14) -0.0183(19) C7 0.0543(17) 0.075(2) 0.0655(17) 0.0032(15) 0.0088(13) 0.0019(15) C8 0.0394(13) 0.0615(17) 0.0597(15) 0.0078(12) 0.0032(11) 0.0070(12) C9 0.0579(19) 0.072(2) 0.090(2) -0.0157(17) -0.0062(16) 0.0177(15) C10 0.060(2) 0.087(2) 0.092(2) -0.0210(19) -0.0189(17) 0.0133(18) C11 0.0431(16) 0.080(2) 0.084(2) 0.0008(17) -0.0092(14) 0.0131(15) C12 0.0589(18) 0.0684(19) 0.077(2) -0.0018(15) 0.0027(15) 0.0203(15) C13 0.0557(17) 0.0689(19) 0.0612(17) -0.0048(13) -0.0036(13) 0.0034(14) N1 0.0356(14) 0.115(3) 0.0821(18) 0.0298(17) 0.0022(12) 0.0134(15) _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 Zn1 Cl1 2.2665(8) . ? Zn1 Cl1 2.2665(8) 2_655 ? Zn1 Cl2 2.2771(9) . ? Zn1 Cl2 2.2771(9) 2_655 ? C1 C2 1.311(4) . ? C1 C8 1.476(4) . ? C1 H1A 0.9300 . ? C2 C3 1.466(4) . ? C2 H2A 0.9300 . ? C3 C7 1.386(4) . ? C3 C4 1.396(4) . ? C4 C5 1.356(4) . ? C4 H4A 0.9300 . ? C5 N1 1.331(5) . ? C5 H5A 0.9300 . ? C6 N1 1.329(5) . ? C6 C7 1.366(4) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.376(4) . ? C8 C13 1.386(4) . ? C9 C10 1.373(4) . ? C9 H9A 0.9300 . ? C10 C11 1.369(5) . ? C10 H10A 0.9300 . ? C11 C12 1.372(4) . ? C11 H11A 0.9300 . ? C12 C13 1.380(4) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? N1 H1B 0.8600 . ? 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 Cl1 Zn1 Cl1 113.08(4) . 2_655 ? Cl1 Zn1 Cl2 112.71(3) . . ? Cl1 Zn1 Cl2 104.61(3) 2_655 . ? Cl1 Zn1 Cl2 104.61(3) . 2_655 ? Cl1 Zn1 Cl2 112.71(3) 2_655 2_655 ? Cl2 Zn1 Cl2 109.27(5) . 2_655 ? C2 C1 C8 126.2(3) . . ? C2 C1 H1A 116.9 . . ? C8 C1 H1A 116.9 . . ? C1 C2 C3 125.4(3) . . ? C1 C2 H2A 117.3 . . ? C3 C2 H2A 117.3 . . ? C7 C3 C4 117.5(3) . . ? C7 C3 C2 118.1(3) . . ? C4 C3 C2 124.5(3) . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? N1 C5 C4 120.3(3) . . ? N1 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? N1 C6 C7 119.6(3) . . ? N1 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C6 C7 C3 120.4(3) . . ? C6 C7 H7A 119.8 . . ? C3 C7 H7A 119.8 . . ? C9 C8 C13 117.6(3) . . ? C9 C8 C1 117.7(3) . . ? C13 C8 C1 124.6(3) . . ? C10 C9 C8 121.4(3) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C12 119.1(3) . . ? C10 C11 H11A 120.4 . . ? C12 C11 H11A 120.4 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C12 C13 C8 120.9(3) . . ? C12 C13 H13A 119.5 . . ? C8 C13 H13A 119.5 . . ? C6 N1 C5 122.2(3) . . ? C6 N1 H1B 118.9 . . ? C5 N1 H1B 118.9 . . ? _diffrn_measured_fraction_theta_max 0.828 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.451 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.053 # Attachment '- compound5.CIF' data_shelxle_5 _database_code_depnum_ccdc_archive 'CCDC 885531' #TrackingRef '- compound5.CIF' _audit_creation_method SHELXL-97 #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C13 H12 N), C4 N4 S4 Zn' _chemical_formula_sum 'C30 H24 N6 S4 Zn' _chemical_formula_weight 662.16 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 14.585(7) _cell_length_b 13.793(6) _cell_length_c 16.038(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.247(14) _cell_angle_gamma 90.00 _cell_volume 3164(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1.102 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 28.10 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type 'Multi Scan' _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device 'Mercury (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 36837 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.15 _reflns_number_total 6502 _reflns_number_gt 2717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _computing_publication_material ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003). ; _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^)+(0.0573P)^2^+3.0908P] 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 6502 _refine_ls_number_parameters 370 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1887 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1453 _refine_ls_goodness_of_fit_ref 1.035 _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 Zn1 Zn 1.29678(5) -0.06558(5) -0.39629(5) 0.0859(3) Uani 1 1 d . . . S1 S 1.46725(15) 0.14693(15) -0.19736(13) 0.1121(7) Uani 1 1 d . . . S2 S 1.41248(16) 0.00356(16) -0.63826(15) 0.1229(8) Uani 1 1 d . . . S3 S 1.38853(15) -0.38540(13) -0.32302(12) 0.1037(6) Uani 1 1 d . . . S4 S 0.98817(14) -0.05017(14) -0.35290(16) 0.1166(7) Uani 1 1 d . . . N1 N 1.3720(4) 0.0078(4) -0.3046(4) 0.0989(18) Uani 1 1 d . . . N2 N 1.3153(5) -0.0199(4) -0.5082(4) 0.0979(19) Uani 1 1 d . . . N3 N 1.3326(4) -0.2021(4) -0.3830(4) 0.0952(17) Uani 1 1 d . . . N4 N 1.1672(4) -0.0538(4) -0.3858(4) 0.0955(18) Uani 1 1 d . . . N5 N 0.9818(3) 0.2805(5) 0.0952(5) 0.0942(17) Uani 1 1 d . . . H5B H 1.0025 0.3259 0.1307 0.113 Uiso 1 1 calc R . . N6 N 0.5193(4) -0.2914(5) -0.1410(4) 0.0958(17) Uani 1 1 d . . . H6B H 0.4962 -0.3400 -0.1716 0.115 Uiso 1 1 calc R . . C1 C 1.4117(4) 0.0645(5) -0.2597(4) 0.0794(17) Uani 1 1 d . . . C2 C 1.3546(4) -0.0115(5) -0.5579(5) 0.0835(19) Uani 1 1 d . . . C3 C 1.3546(4) -0.2798(5) -0.3586(4) 0.0788(17) Uani 1 1 d . . . C4 C 1.0948(5) -0.0519(4) -0.3718(4) 0.0801(18) Uani 1 1 d . . . C5 C 0.8520(4) -0.0207(7) -0.0724(6) 0.114(3) Uani 1 1 d D . . H5A H 0.8487 -0.0369 -0.0168 0.137 Uiso 1 1 calc R . . C6 C 0.8832(5) 0.0645(6) -0.0836(6) 0.121(3) Uani 1 1 d D . . H6A H 0.8857 0.0823 -0.1390 0.145 Uiso 1 1 calc R . . C7 C 0.9161(4) 0.1385(5) -0.0143(5) 0.0804(18) Uani 1 1 d . . . C8 C 0.9388(5) 0.2273(6) -0.0437(5) 0.0914(19) Uani 1 1 d . . . H8A H 0.9318 0.2389 -0.1018 0.110 Uiso 1 1 calc R . . C9 C 0.9715(5) 0.2973(5) 0.0132(7) 0.098(2) Uani 1 1 d . . . H9A H 0.9868 0.3578 -0.0057 0.117 Uiso 1 1 calc R . . C10 C 0.9606(5) 0.1934(7) 0.1249(5) 0.097(2) Uani 1 1 d . . . H10A H 0.9684 0.1822 0.1830 0.117 Uiso 1 1 calc R . . C11 C 0.9284(4) 0.1243(5) 0.0696(6) 0.0867(19) Uani 1 1 d . . . H11A H 0.9139 0.0641 0.0898 0.104 Uiso 1 1 calc R . . C12 C 0.8211(4) -0.0958(5) -0.1368(5) 0.0828(19) Uani 1 1 d . . . C13 C 0.8011(4) -0.1836(6) -0.1046(5) 0.095(2) Uani 1 1 d . . . H13A H 0.8050 -0.1908 -0.0464 0.113 Uiso 1 1 calc R . . C14 C 0.7758(5) -0.2602(6) -0.1570(8) 0.109(2) Uani 1 1 d . . . H14A H 0.7613 -0.3193 -0.1348 0.130 Uiso 1 1 calc R . . C15 C 0.7715(5) -0.2505(7) -0.2416(8) 0.115(3) Uani 1 1 d . . . H15A H 0.7560 -0.3037 -0.2772 0.138 Uiso 1 1 calc R . . C16 C 0.7893(6) -0.1649(8) -0.2745(5) 0.119(3) Uani 1 1 d . . . H16A H 0.7848 -0.1586 -0.3329 0.143 Uiso 1 1 calc R . . C17 C 0.8144(5) -0.0863(6) -0.2223(6) 0.105(2) Uani 1 1 d . . . H17A H 0.8267 -0.0269 -0.2453 0.127 Uiso 1 1 calc R . . C18 C 0.6320(4) -0.0580(5) 0.0130(5) 0.093(2) Uani 1 1 d . . . H18A H 0.6582 -0.0728 0.0692 0.111 Uiso 1 1 calc R . . C19 C 0.6340(4) 0.0319(6) -0.0109(5) 0.095(2) Uani 1 1 d . . . H19A H 0.6096 0.0447 -0.0678 0.115 Uiso 1 1 calc R . . C20 C 0.6707(4) 0.1155(5) 0.0423(5) 0.0788(17) Uani 1 1 d . . . C21 C 0.7086(4) 0.1102(5) 0.1265(5) 0.0843(18) Uani 1 1 d . . . H21A H 0.7147 0.0499 0.1531 0.101 Uiso 1 1 calc R . . C22 C 0.7376(4) 0.1906(6) 0.1726(5) 0.095(2) Uani 1 1 d . . . H22A H 0.7633 0.1855 0.2303 0.115 Uiso 1 1 calc R . . C23 C 0.7289(5) 0.2801(6) 0.1336(7) 0.106(2) Uani 1 1 d . . . H23A H 0.7478 0.3355 0.1653 0.128 Uiso 1 1 calc R . . C24 C 0.6932(5) 0.2878(6) 0.0498(6) 0.107(2) Uani 1 1 d . . . H24A H 0.6881 0.3482 0.0235 0.129 Uiso 1 1 calc R . . C25 C 0.6645(5) 0.2064(6) 0.0036(5) 0.099(2) Uani 1 1 d . . . H25A H 0.6406 0.2117 -0.0544 0.119 Uiso 1 1 calc R . . C26 C 0.5905(4) -0.1387(4) -0.0434(4) 0.0736(16) Uani 1 1 d . . . C27 C 0.5927(4) -0.2307(5) -0.0102(4) 0.0857(18) Uani 1 1 d . . . H27A H 0.6189 -0.2415 0.0467 0.103 Uiso 1 1 calc R . . C28 C 0.5565(5) -0.3056(5) -0.0609(6) 0.097(2) Uani 1 1 d . . . H28A H 0.5581 -0.3679 -0.0384 0.117 Uiso 1 1 calc R . . C29 C 0.5161(5) -0.2040(6) -0.1764(5) 0.097(2) Uani 1 1 d . . . H29A H 0.4895 -0.1957 -0.2336 0.117 Uiso 1 1 calc R . . C30 C 0.5519(5) -0.1270(5) -0.1283(5) 0.0927(19) Uani 1 1 d . . . H30A H 0.5503 -0.0658 -0.1528 0.111 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 Zn1 0.0965(5) 0.0700(5) 0.0902(6) -0.0014(4) 0.0157(4) 0.0053(4) S1 0.1454(17) 0.0955(15) 0.0852(14) -0.0012(11) -0.0022(12) -0.0143(12) S2 0.1488(18) 0.1002(16) 0.1298(18) 0.0154(13) 0.0523(15) 0.0189(13) S3 0.1480(16) 0.0588(11) 0.0980(14) -0.0102(10) 0.0080(11) 0.0051(10) S4 0.1025(13) 0.0859(14) 0.167(2) -0.0067(13) 0.0401(13) -0.0006(10) N1 0.105(4) 0.087(4) 0.099(5) -0.010(4) 0.008(3) -0.010(3) N2 0.134(5) 0.082(4) 0.085(5) 0.002(3) 0.041(4) 0.002(3) N3 0.112(4) 0.078(4) 0.093(4) -0.006(3) 0.013(3) 0.010(3) N4 0.083(4) 0.086(4) 0.117(5) -0.004(3) 0.018(3) 0.008(3) N5 0.080(3) 0.087(5) 0.114(6) -0.030(4) 0.014(4) 0.011(3) N6 0.087(4) 0.095(5) 0.102(5) -0.015(4) 0.009(3) -0.021(3) C1 0.086(4) 0.076(5) 0.074(5) 0.020(4) 0.012(3) 0.008(4) C2 0.084(4) 0.062(4) 0.096(6) -0.009(4) -0.001(4) 0.017(3) C3 0.094(4) 0.072(5) 0.069(4) -0.020(4) 0.013(3) -0.007(4) C4 0.101(5) 0.053(4) 0.077(5) -0.002(3) -0.004(4) 0.001(3) C5 0.071(4) 0.120(7) 0.152(8) 0.022(6) 0.023(5) 0.022(4) C6 0.080(5) 0.117(7) 0.171(9) 0.022(7) 0.037(5) 0.034(5) C7 0.064(3) 0.074(5) 0.102(6) -0.024(4) 0.013(4) 0.005(3) C8 0.100(5) 0.079(5) 0.094(5) -0.004(5) 0.016(4) -0.003(4) C9 0.091(5) 0.075(5) 0.128(7) 0.011(5) 0.021(5) -0.001(4) C10 0.087(5) 0.114(7) 0.094(6) 0.008(6) 0.023(4) 0.027(4) C11 0.084(4) 0.064(4) 0.118(7) -0.005(5) 0.035(4) 0.002(3) C12 0.065(4) 0.086(5) 0.092(6) -0.035(4) 0.003(3) -0.001(3) C13 0.075(4) 0.101(6) 0.108(6) 0.008(5) 0.017(4) 0.012(4) C14 0.091(5) 0.073(6) 0.159(9) 0.007(6) 0.018(5) -0.007(4) C15 0.103(6) 0.092(7) 0.141(9) -0.032(6) 0.004(6) -0.007(4) C16 0.134(7) 0.129(8) 0.090(6) -0.025(6) 0.010(5) -0.006(6) C17 0.126(6) 0.091(6) 0.097(6) -0.003(5) 0.017(5) -0.012(4) C18 0.093(4) 0.081(5) 0.103(5) 0.008(4) 0.016(4) 0.008(4) C19 0.088(4) 0.091(6) 0.106(6) 0.010(5) 0.018(4) 0.002(4) C20 0.077(4) 0.071(5) 0.089(5) -0.016(4) 0.018(4) -0.008(3) C21 0.092(4) 0.072(5) 0.095(6) -0.005(4) 0.032(4) 0.000(3) C22 0.095(5) 0.108(6) 0.088(5) -0.014(5) 0.027(4) -0.002(4) C23 0.088(5) 0.088(6) 0.141(8) -0.026(6) 0.016(5) -0.007(4) C24 0.115(6) 0.069(5) 0.131(7) 0.002(5) 0.008(5) -0.017(4) C25 0.106(5) 0.082(5) 0.107(6) 0.017(5) 0.014(4) 0.003(4) C26 0.077(4) 0.064(4) 0.077(5) -0.013(4) 0.009(3) -0.001(3) C27 0.100(4) 0.069(5) 0.085(5) 0.004(4) 0.011(4) -0.008(4) C28 0.111(5) 0.068(5) 0.113(7) 0.002(5) 0.021(5) -0.011(4) C29 0.097(5) 0.096(6) 0.088(5) 0.011(5) -0.008(4) 0.001(4) C30 0.099(5) 0.071(5) 0.101(6) -0.002(4) 0.002(4) -0.003(4) _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 Zn1 N4 1.936(6) . ? Zn1 N1 1.940(6) . ? Zn1 N3 1.955(6) . ? Zn1 N2 1.970(6) . ? S1 C1 1.622(8) . ? S2 C2 1.685(8) . ? S3 C3 1.607(8) . ? S4 C4 1.642(8) . ? N1 C1 1.141(7) . ? N2 C2 1.075(7) . ? N3 C3 1.164(7) . ? N4 C4 1.122(7) . ? N5 C9 1.315(9) . ? N5 C10 1.350(9) . ? N5 H5B 0.8600 . ? N6 C28 1.308(8) . ? N6 C29 1.330(8) . ? N6 H6B 0.8600 . ? C5 C6 1.285(4) . ? C5 C12 1.470(10) . ? C5 H5A 0.9300 . ? C6 C7 1.516(11) . ? C6 H6A 0.9300 . ? C7 C11 1.337(9) . ? C7 C8 1.376(9) . ? C8 C9 1.351(9) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C11 1.324(9) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C17 1.362(9) . ? C12 C13 1.370(9) . ? C13 C14 1.355(10) . ? C13 H13A 0.9300 . ? C14 C15 1.353(11) . ? C14 H14A 0.9300 . ? C15 C16 1.340(11) . ? C15 H15A 0.9300 . ? C16 C17 1.374(10) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.300(8) . ? C18 C26 1.487(9) . ? C18 H18A 0.9300 . ? C19 C20 1.472(9) . ? C19 H19A 0.9300 . ? C20 C21 1.357(8) . ? C20 C25 1.394(9) . ? C21 C22 1.355(9) . ? C21 H21A 0.9300 . ? C22 C23 1.379(10) . ? C22 H22A 0.9300 . ? C23 C24 1.348(10) . ? C23 H23A 0.9300 . ? C24 C25 1.364(9) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.374(8) . ? C26 C30 1.377(8) . ? C27 C28 1.357(9) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 C30 1.356(9) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? 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 N4 Zn1 N1 107.9(2) . . ? N4 Zn1 N3 108.4(2) . . ? N1 Zn1 N3 108.7(2) . . ? N4 Zn1 N2 111.2(3) . . ? N1 Zn1 N2 111.5(3) . . ? N3 Zn1 N2 109.0(2) . . ? C1 N1 Zn1 168.1(6) . . ? C2 N2 Zn1 153.9(7) . . ? C3 N3 Zn1 166.8(6) . . ? C4 N4 Zn1 172.7(6) . . ? C9 N5 C10 121.3(7) . . ? C9 N5 H5B 119.4 . . ? C10 N5 H5B 119.4 . . ? C28 N6 C29 122.0(6) . . ? C28 N6 H6B 119.0 . . ? C29 N6 H6B 119.0 . . ? N1 C1 S1 178.7(7) . . ? N2 C2 S2 177.7(7) . . ? N3 C3 S3 177.9(6) . . ? N4 C4 S4 179.0(7) . . ? C6 C5 C12 127.9(9) . . ? C6 C5 H5A 116.0 . . ? C12 C5 H5A 116.0 . . ? C5 C6 C7 125.7(9) . . ? C5 C6 H6A 117.2 . . ? C7 C6 H6A 117.2 . . ? C11 C7 C8 118.8(7) . . ? C11 C7 C6 126.9(7) . . ? C8 C7 C6 114.2(8) . . ? C9 C8 C7 118.7(7) . . ? C9 C8 H8A 120.6 . . ? C7 C8 H8A 120.6 . . ? N5 C9 C8 120.5(7) . . ? N5 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C11 C10 N5 118.8(7) . . ? C11 C10 H10A 120.6 . . ? N5 C10 H10A 120.6 . . ? C10 C11 C7 121.9(7) . . ? C10 C11 H11A 119.0 . . ? C7 C11 H11A 119.0 . . ? C17 C12 C13 119.0(7) . . ? C17 C12 C5 126.3(8) . . ? C13 C12 C5 114.6(8) . . ? C14 C13 C12 120.5(8) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C15 C14 C13 119.9(8) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C16 C15 C14 120.5(8) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 120.2(8) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C12 C17 C16 119.7(8) . . ? C12 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C19 C18 C26 124.4(7) . . ? C19 C18 H18A 117.8 . . ? C26 C18 H18A 117.8 . . ? C18 C19 C20 127.1(7) . . ? C18 C19 H19A 116.5 . . ? C20 C19 H19A 116.5 . . ? C21 C20 C25 118.1(6) . . ? C21 C20 C19 124.4(7) . . ? C25 C20 C19 117.5(7) . . ? C22 C21 C20 121.5(7) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C23 119.6(8) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C24 C23 C22 120.4(8) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.7(8) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C24 C25 C20 120.8(7) . . ? C24 C25 H25A 119.6 . . ? C20 C25 H25A 119.6 . . ? C27 C26 C30 117.8(6) . . ? C27 C26 C18 118.6(7) . . ? C30 C26 C18 123.6(6) . . ? C28 C27 C26 119.6(7) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? N6 C28 C27 120.8(7) . . ? N6 C28 H28A 119.6 . . ? C27 C28 H28A 119.6 . . ? N6 C29 C30 119.2(7) . . ? N6 C29 H29A 120.4 . . ? C30 C29 H29A 120.4 . . ? C29 C30 C26 120.6(7) . . ? C29 C30 H30A 119.7 . . ? C26 C30 H30A 119.7 . . ? _diffrn_measured_fraction_theta_max 0.837 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.481 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.055