# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Yunyin Niu' _publ_contact_author_email niuyy@zzu.edu.cn _publ_section_title ; Four Novel Metal Coordination Polymers Directed By 1, 1'-dibutyl-4, 4'-bipyridinium dibromide (BBP) and Their Framework Dependent Luminescent Properties ; loop_ _publ_author_name 'Jun-Ming Yue' 'Yunyin Niu' 'Bing Zhang' 'Seik-Weng Ng' 'Hong-Wei Hou' # end Validation Reply Form # Attachment '- revised CIF3.cif' data_100426bm _database_code_depnum_ccdc_archive 'CCDC 793445' #TrackingRef '- revised CIF3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H26 N2, 2(C2 Cu N2 S2)' _chemical_formula_sum 'C22 H26 Cu2 N6 S4' _chemical_formula_weight 629.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 8.5848(14) _cell_length_b 15.017(2) _cell_length_c 10.5180(16) _cell_angle_alpha 90.00 _cell_angle_beta 101.338(3) _cell_angle_gamma 90.00 _cell_volume 1329.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2423 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.88 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 1.937 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8803 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3268 _reflns_number_gt 2307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In the refinement, carbon C8-C11 atoms were apparently found to be disordered over two sites. Then, some restraints, e.g. DFIX and SADI, were used to restrain the C-C distances in the refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0170(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3268 _refine_ls_number_parameters 194 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.978 _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 Cu1 Cu 0.82068(4) 0.77389(2) 0.66903(3) 0.05714(17) Uani 1 1 d . . . C1 C 0.6796(3) 0.67672(16) 0.4144(2) 0.0469(6) Uani 1 1 d . . . C2 C 0.9476(3) 0.67261(16) 0.9235(2) 0.0430(6) Uani 1 1 d . . . C3 C 0.5341(4) 0.6172(2) 0.7705(3) 0.0793(10) Uani 1 1 d . A . H3 H 0.6075 0.6362 0.7220 0.095 Uiso 1 1 calc R . . C4 C 0.5816(4) 0.5626(2) 0.8733(3) 0.0728(9) Uani 1 1 d . . . H4 H 0.6877 0.5455 0.8950 0.087 Uiso 1 1 calc R . . C5 C 0.4758(3) 0.53160(16) 0.9466(3) 0.0524(7) Uani 1 1 d . . . C6 C 0.3213(4) 0.5608(2) 0.9105(3) 0.0791(10) Uani 1 1 d . . . H6 H 0.2455 0.5420 0.9568 0.095 Uiso 1 1 calc R . . C7 C 0.2781(4) 0.6172(2) 0.8073(4) 0.0816(10) Uani 1 1 d . A . H7 H 0.1736 0.6370 0.7853 0.098 Uiso 1 1 calc R . . C8 C 0.3377(19) 0.6998(6) 0.6183(7) 0.072(5) Uani 0.55 1 d PD A 1 H8A H 0.4314 0.7126 0.5829 0.087 Uiso 0.55 1 calc PR A 1 H8B H 0.2941 0.7560 0.6406 0.087 Uiso 0.55 1 calc PR A 1 C9 C 0.2147(10) 0.6520(5) 0.5158(7) 0.088(3) Uani 0.55 1 d PD A 1 H9A H 0.1206 0.6400 0.5510 0.106 Uiso 0.55 1 calc PR A 1 H9B H 0.1840 0.6907 0.4411 0.106 Uiso 0.55 1 calc PR A 1 C10 C 0.2781(10) 0.5657(5) 0.4731(7) 0.0801(19) Uani 0.55 1 d PD A 1 H10A H 0.2918 0.5225 0.5429 0.096 Uiso 0.55 1 calc PR A 1 H10B H 0.3801 0.5754 0.4488 0.096 Uiso 0.55 1 calc PR A 1 C11 C 0.157(3) 0.5322(9) 0.3570(13) 0.144(7) Uani 0.55 1 d PD A 1 H11A H 0.0515 0.5440 0.3707 0.216 Uiso 0.55 1 calc PR A 1 H11B H 0.1702 0.4693 0.3472 0.216 Uiso 0.55 1 calc PR A 1 H11C H 0.1727 0.5623 0.2799 0.216 Uiso 0.55 1 calc PR A 1 N1 N 0.7039(3) 0.70541(15) 0.5171(2) 0.0587(6) Uani 1 1 d . . . N2 N 0.9227(3) 0.70013(15) 0.8198(2) 0.0521(5) Uani 1 1 d . . . N3 N 0.3834(3) 0.64412(14) 0.7379(3) 0.0639(7) Uani 1 1 d D . . S1 S 0.64456(11) 0.63440(5) 0.26710(7) 0.0666(2) Uani 1 1 d . . . S2 S 0.98655(9) 0.63134(4) 1.07230(6) 0.0528(2) Uani 1 1 d . . . C8' C 0.317(3) 0.7011(7) 0.6231(9) 0.099(9) Uani 0.45 1 d PD A 2 H8'1 H 0.3870 0.7511 0.6184 0.119 Uiso 0.45 1 calc PR A 2 H8'2 H 0.2139 0.7244 0.6319 0.119 Uiso 0.45 1 calc PR A 2 C9' C 0.2989(12) 0.6446(7) 0.4983(7) 0.083(3) Uani 0.45 1 d PD A 2 H9'1 H 0.2761 0.6835 0.4232 0.099 Uiso 0.45 1 calc PR A 2 H9'2 H 0.3982 0.6142 0.4969 0.099 Uiso 0.45 1 calc PR A 2 C10' C 0.1669(12) 0.5767(7) 0.4904(10) 0.101(3) Uani 0.45 1 d PD A 2 H10C H 0.0668 0.6084 0.4815 0.121 Uiso 0.45 1 calc PR A 2 H10D H 0.1829 0.5444 0.5718 0.121 Uiso 0.45 1 calc PR A 2 C11' C 0.153(3) 0.5090(11) 0.3797(15) 0.136(9) Uani 0.45 1 d PD A 2 H11D H 0.1090 0.5377 0.2990 0.205 Uiso 0.45 1 calc PR A 2 H11E H 0.0839 0.4613 0.3944 0.205 Uiso 0.45 1 calc PR A 2 H11F H 0.2557 0.4856 0.3764 0.205 Uiso 0.45 1 calc PR A 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 Cu1 0.0709(3) 0.0701(3) 0.0326(2) 0.00040(14) 0.01552(16) -0.00842(17) C1 0.0541(15) 0.0494(14) 0.0406(14) 0.0018(11) 0.0178(11) -0.0125(12) C2 0.0385(13) 0.0525(14) 0.0415(14) -0.0044(11) 0.0164(11) 0.0050(11) C3 0.053(2) 0.098(2) 0.088(3) 0.020(2) 0.0171(17) -0.0238(18) C4 0.0451(17) 0.089(2) 0.082(2) 0.0145(18) 0.0070(15) -0.0224(16) C5 0.0604(17) 0.0477(14) 0.0533(16) -0.0196(11) 0.0217(14) -0.0116(13) C6 0.082(2) 0.088(2) 0.084(2) 0.0073(19) 0.056(2) 0.0231(19) C7 0.072(2) 0.088(2) 0.097(3) 0.004(2) 0.045(2) 0.0298(19) C8 0.070(7) 0.063(9) 0.091(11) 0.010(7) 0.036(7) 0.008(6) C9 0.074(5) 0.099(6) 0.094(6) 0.033(5) 0.027(5) 0.041(6) C10 0.089(6) 0.074(5) 0.080(5) 0.019(4) 0.022(4) 0.013(4) C11 0.249(17) 0.100(11) 0.062(6) 0.037(7) -0.019(8) 0.021(10) N1 0.0739(16) 0.0682(14) 0.0388(12) -0.0058(11) 0.0228(11) -0.0248(12) N2 0.0538(13) 0.0659(13) 0.0410(12) 0.0007(11) 0.0200(10) 0.0086(11) N3 0.0730(18) 0.0503(13) 0.0724(17) -0.0037(12) 0.0243(14) -0.0049(13) S1 0.0932(6) 0.0680(5) 0.0428(4) -0.0147(3) 0.0236(4) -0.0274(4) S2 0.0575(4) 0.0632(4) 0.0404(4) 0.0064(3) 0.0162(3) 0.0146(3) C8' 0.082(11) 0.066(12) 0.143(19) 0.046(11) 0.007(12) -0.005(8) C9' 0.080(7) 0.092(8) 0.077(6) 0.029(5) 0.018(5) 0.012(6) C10' 0.083(7) 0.100(8) 0.113(8) 0.030(6) 0.000(6) -0.005(6) C11' 0.26(2) 0.064(7) 0.057(8) 0.025(7) -0.045(10) 0.007(8) _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 Cu1 N2 1.990(2) . ? Cu1 N1 1.997(2) . ? Cu1 S2 2.3786(8) 4_575 ? Cu1 S1 2.4206(9) 4_576 ? C1 N1 1.143(3) . ? C1 S1 1.647(3) . ? C2 N2 1.146(3) . ? C2 S2 1.656(3) . ? C3 N3 1.334(4) . ? C3 C4 1.355(4) . ? C3 H3 0.9300 . ? C4 C5 1.383(4) . ? C4 H4 0.9300 . ? C5 C6 1.378(4) . ? C5 C5 1.467(6) 3_667 ? C6 C7 1.370(4) . ? C6 H6 0.9300 . ? C7 N3 1.332(4) . ? C7 H7 0.9300 . ? C8 N3 1.498(7) . ? C8 C9 1.531(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.508(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.526(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? N3 C8' 1.499(7) . ? S1 Cu1 2.4206(9) 4_575 ? S2 Cu1 2.3787(8) 4_576 ? C8' C9' 1.545(9) . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C9' C10' 1.515(8) . ? C9' H9'1 0.9700 . ? C9' H9'2 0.9700 . ? C10' C11' 1.533(10) . ? C10' H10C 0.9700 . ? C10' H10D 0.9700 . ? C11' H11D 0.9600 . ? C11' H11E 0.9600 . ? C11' H11F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 115.09(10) . . ? N2 Cu1 S2 117.85(7) . 4_575 ? N1 Cu1 S2 102.37(7) . 4_575 ? N2 Cu1 S1 101.01(6) . 4_576 ? N1 Cu1 S1 112.14(8) . 4_576 ? S2 Cu1 S1 108.57(3) 4_575 4_576 ? N1 C1 S1 179.4(2) . . ? N2 C2 S2 178.7(2) . . ? N3 C3 C4 120.9(3) . . ? N3 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 121.4(3) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 116.2(3) . . ? C6 C5 C5 122.0(3) . 3_667 ? C4 C5 C5 121.8(3) . 3_667 ? C7 C6 C5 120.8(3) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? N3 C7 C6 121.0(3) . . ? N3 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? N3 C8 C9 111.1(7) . . ? N3 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N3 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 111.9(7) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 107.0(9) . . ? C9 C10 H10A 110.3 . . ? C11 C10 H10A 110.3 . . ? C9 C10 H10B 110.3 . . ? C11 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? C1 N1 Cu1 156.9(2) . . ? C2 N2 Cu1 158.3(2) . . ? C7 N3 C3 119.7(3) . . ? C7 N3 C8 122.4(7) . . ? C3 N3 C8 117.8(7) . . ? C7 N3 C8' 114.9(10) . . ? C3 N3 C8' 125.3(10) . . ? C1 S1 Cu1 99.64(9) . 4_575 ? C2 S2 Cu1 98.85(8) . 4_576 ? N3 C8' C9' 109.2(7) . . ? N3 C8' H8'1 109.8 . . ? C9' C8' H8'1 109.8 . . ? N3 C8' H8'2 109.8 . . ? C9' C8' H8'2 109.8 . . ? H8'1 C8' H8'2 108.3 . . ? C10' C9' C8' 111.3(12) . . ? C10' C9' H9'1 109.4 . . ? C8' C9' H9'1 109.4 . . ? C10' C9' H9'2 109.4 . . ? C8' C9' H9'2 109.4 . . ? H9'1 C9' H9'2 108.0 . . ? C9' C10' C11' 115.8(14) . . ? C9' C10' H10C 108.3 . . ? C11' C10' H10C 108.3 . . ? C9' C10' H10D 108.3 . . ? C11' C10' H10D 108.3 . . ? H10C C10' H10D 107.4 . . ? C10' C11' H11D 109.5 . . ? C10' C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C10' C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C3 C4 C5 1.1(5) . . . . ? C3 C4 C5 C6 -1.2(5) . . . . ? C3 C4 C5 C5 176.4(3) . . . 3_667 ? C4 C5 C6 C7 0.1(5) . . . . ? C5 C5 C6 C7 -177.5(3) 3_667 . . . ? C5 C6 C7 N3 1.1(5) . . . . ? N3 C8 C9 C10 -61.3(13) . . . . ? C8 C9 C10 C11 -171.0(11) . . . . ? N2 Cu1 N1 C1 -110.2(6) . . . . ? S2 Cu1 N1 C1 18.9(6) 4_575 . . . ? S1 Cu1 N1 C1 135.0(6) 4_576 . . . ? N1 Cu1 N2 C2 -117.0(6) . . . . ? S2 Cu1 N2 C2 122.0(6) 4_575 . . . ? S1 Cu1 N2 C2 3.9(6) 4_576 . . . ? C6 C7 N3 C3 -1.2(5) . . . . ? C6 C7 N3 C8 175.0(5) . . . . ? C6 C7 N3 C8' 176.4(6) . . . . ? C4 C3 N3 C7 0.1(5) . . . . ? C4 C3 N3 C8 -176.3(5) . . . . ? C4 C3 N3 C8' -177.2(6) . . . . ? C9 C8 N3 C7 -59.6(11) . . . . ? C9 C8 N3 C3 116.7(9) . . . . ? C7 N3 C8' C9' -103.2(14) . . . . ? C3 N3 C8' C9' 74.2(16) . . . . ? N3 C8' C9' C10' 70.3(19) . . . . ? C8' C9' C10' C11' -172.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.292 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.060 # Attachment '- revised CIF2.cif' data_100426dm _database_code_depnum_ccdc_archive 'CCDC 793446' #TrackingRef '- revised CIF2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '5(C18 H26 N2), I22 Pb6, 2(C3 H7 N O)' _chemical_formula_sum 'C96 H144 I22 N12 O2 Pb6' _chemical_formula_weight 5533.17 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 15.7586(10) _cell_length_b 13.6737(9) _cell_length_c 33.957(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.383(1) _cell_angle_gamma 90.00 _cell_volume 7197.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3610 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 19.01 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4956 _exptl_absorpt_coefficient_mu 11.753 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45805 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14112 _reflns_number_gt 7401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In the refinement, some carbon atoms, C17/C18, C30-C32 and C42-C45, were apparently found to be seriously disordered. We have tried many times to refine their coordinates by using the iPARTi command. But we are failed each time. Then, we have used the command of iISORi to restrain their unstable thermal factors. ; _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^)+(0.0710P)^2^] 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 14112 _refine_ls_number_parameters 629 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.1310 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.925 _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 Pb1 Pb 0.11558(4) 0.22522(4) 0.357978(17) 0.06119(18) Uani 1 1 d . . . Pb2 Pb -0.15926(4) 0.12281(4) 0.394309(16) 0.05954(18) Uani 1 1 d . . . Pb3 Pb 0.13140(3) 0.05945(4) 0.483036(16) 0.05882(17) Uani 1 1 d . . . C1 C 1.1344(13) 0.5973(13) 0.3917(5) 0.088(6) Uani 1 1 d . . . H1 H 1.1642 0.5590 0.3760 0.106 Uiso 1 1 calc R . . C2 C 1.0699(12) 0.5602(13) 0.4064(5) 0.087(5) Uani 1 1 d . . . H2 H 1.0536 0.4966 0.3989 0.104 Uiso 1 1 calc R . . C3 C 1.0253(11) 0.6052(10) 0.4311(4) 0.065(4) Uani 1 1 d . . . C4 C 1.0542(13) 0.7013(13) 0.4386(5) 0.092(5) Uani 1 1 d . . . H4 H 1.0270 0.7391 0.4554 0.111 Uiso 1 1 calc R . . C5 C 1.1192(15) 0.7434(13) 0.4232(5) 0.096(6) Uani 1 1 d . . . H5 H 1.1360 0.8075 0.4295 0.116 Uiso 1 1 calc R . . C6 C 0.9573(10) 0.5644(12) 0.4459(4) 0.062(4) Uani 1 1 d . . . C7 C 0.9181(13) 0.6131(13) 0.4731(6) 0.092(6) Uani 1 1 d . . . H7 H 0.9367 0.6762 0.4805 0.111 Uiso 1 1 calc R . . C8 C 0.8557(14) 0.5754(13) 0.4893(6) 0.101(6) Uani 1 1 d . . . H8 H 0.8300 0.6124 0.5069 0.121 Uiso 1 1 calc R . . C9 C 0.8634(13) 0.4304(14) 0.4545(5) 0.089(6) Uani 1 1 d . . . H9 H 0.8469 0.3660 0.4486 0.107 Uiso 1 1 calc R . . C10 C 0.9214(13) 0.4727(13) 0.4378(5) 0.086(5) Uani 1 1 d . . . H10 H 0.9412 0.4371 0.4180 0.103 Uiso 1 1 calc R . . C11 C 1.2331(14) 0.7360(12) 0.3851(5) 0.099(6) Uani 1 1 d . . . H11A H 1.2379 0.7082 0.3594 0.119 Uiso 1 1 calc R . . H11B H 1.2232 0.8057 0.3814 0.119 Uiso 1 1 calc R . . C12 C 1.3146(14) 0.7210(16) 0.4129(6) 0.116(7) Uani 1 1 d . . . H12A H 1.3259 0.6515 0.4159 0.139 Uiso 1 1 calc R . . H12B H 1.3096 0.7472 0.4389 0.139 Uiso 1 1 calc R . . C13 C 1.3940(19) 0.773(2) 0.3975(10) 0.196(13) Uani 1 1 d . . . H13A H 1.4043 0.7404 0.3734 0.235 Uiso 1 1 calc R . . H13B H 1.3795 0.8405 0.3908 0.235 Uiso 1 1 calc R . . C14 C 1.4709(18) 0.769(2) 0.4273(8) 0.205(15) Uani 1 1 d . . . H14A H 1.4561 0.7537 0.4528 0.308 Uiso 1 1 calc R . . H14B H 1.4992 0.8317 0.4288 0.308 Uiso 1 1 calc R . . H14C H 1.5089 0.7200 0.4202 0.308 Uiso 1 1 calc R . . C15 C 0.7539(11) 0.4385(13) 0.4961(5) 0.103(6) Uani 1 1 d D . . H15A H 0.7531 0.4641 0.5227 0.123 Uiso 1 1 calc R . . H15B H 0.7610 0.3681 0.4982 0.123 Uiso 1 1 calc R . . C16 C 0.6678(11) 0.4624(16) 0.4685(5) 0.133(8) Uani 1 1 d D . . H16A H 0.6566 0.5321 0.4687 0.160 Uiso 1 1 calc R . . H16B H 0.6697 0.4426 0.4412 0.160 Uiso 1 1 calc R . . C17 C 0.5974(13) 0.406(2) 0.4845(7) 0.207(13) Uani 1 1 d DU . . H17A H 0.5897 0.4314 0.5103 0.248 Uiso 1 1 calc R . . H17B H 0.6112 0.3370 0.4872 0.248 Uiso 1 1 calc R . . C18 C 0.5155(13) 0.424(2) 0.4523(8) 0.237(15) Uani 1 1 d DU . . H18A H 0.5210 0.4845 0.4389 0.355 Uiso 1 1 calc R . . H18B H 0.4657 0.4259 0.4649 0.355 Uiso 1 1 calc R . . H18C H 0.5092 0.3712 0.4332 0.355 Uiso 1 1 calc R . . C19 C 0.1827(15) 0.2448(13) 0.6378(5) 0.105(7) Uani 1 1 d . . . H19 H 0.2137 0.2024 0.6243 0.126 Uiso 1 1 calc R . . C20 C 0.1157(12) 0.2085(13) 0.6538(5) 0.086(5) Uani 1 1 d . . . H20 H 0.1022 0.1423 0.6513 0.103 Uiso 1 1 calc R . . C21 C 0.0696(10) 0.2675(11) 0.6732(4) 0.061(4) Uani 1 1 d . . . C22 C 0.0929(11) 0.3658(13) 0.6758(4) 0.078(5) Uani 1 1 d . . . H22 H 0.0621 0.4094 0.6888 0.094 Uiso 1 1 calc R . . C23 C 0.1597(13) 0.3987(13) 0.6595(5) 0.085(5) Uani 1 1 d . . . H23 H 0.1736 0.4648 0.6617 0.102 Uiso 1 1 calc R . . C24 C -0.0008(10) 0.2350(10) 0.6905(4) 0.057(4) Uani 1 1 d . . . C25 C -0.0395(13) 0.1473(12) 0.6781(5) 0.087(5) Uani 1 1 d . . . H25 H -0.0213 0.1120 0.6578 0.104 Uiso 1 1 calc R . . C26 C -0.1072(12) 0.1109(11) 0.6963(5) 0.080(5) Uani 1 1 d . . . H26 H -0.1320 0.0507 0.6883 0.096 Uiso 1 1 calc R . . C27 C -0.0978(13) 0.2447(16) 0.7359(5) 0.100(6) Uani 1 1 d . . . H27 H -0.1174 0.2804 0.7558 0.120 Uiso 1 1 calc R . . C28 C -0.0316(12) 0.2805(11) 0.7197(5) 0.080(5) Uani 1 1 d . . . H28 H -0.0066 0.3394 0.7293 0.096 Uiso 1 1 calc R . . C29 C 0.2790(11) 0.3791(13) 0.6252(5) 0.095(6) Uani 1 1 d D . . H29A H 0.2690 0.4471 0.6178 0.114 Uiso 1 1 calc R . . H29B H 0.2861 0.3427 0.6015 0.114 Uiso 1 1 calc R . . C30 C 0.3614(13) 0.370(2) 0.6574(7) 0.192(12) Uani 1 1 d DU . . H30A H 0.3563 0.4085 0.6809 0.230 Uiso 1 1 calc R . . H30B H 0.3721 0.3024 0.6654 0.230 Uiso 1 1 calc R . . C31 C 0.4344(16) 0.410(4) 0.6371(8) 0.39(3) Uani 1 1 d DU . . H31A H 0.4615 0.3575 0.6246 0.463 Uiso 1 1 calc R . . H31B H 0.4126 0.4584 0.6170 0.463 Uiso 1 1 calc R . . C32 C 0.499(2) 0.456(3) 0.6718(12) 0.36(3) Uani 1 1 d DU . . H32A H 0.4678 0.4956 0.6878 0.545 Uiso 1 1 calc R . . H32B H 0.5391 0.4962 0.6611 0.545 Uiso 1 1 calc R . . H32C H 0.5292 0.4053 0.6880 0.545 Uiso 1 1 calc R . . C33 C -0.2047(11) 0.1199(12) 0.7421(5) 0.083(5) Uani 1 1 d . . . H33A H -0.2079 0.1551 0.7666 0.099 Uiso 1 1 calc R . . H33B H -0.1920 0.0520 0.7491 0.099 Uiso 1 1 calc R . . C34 C -0.2918(11) 0.1260(12) 0.7141(5) 0.088(5) Uani 1 1 d . . . H34A H -0.3030 0.1933 0.7058 0.106 Uiso 1 1 calc R . . H34B H -0.2900 0.0871 0.6904 0.106 Uiso 1 1 calc R . . C35 C -0.3638(15) 0.0900(17) 0.7340(7) 0.141(8) Uani 1 1 d . . . H35A H -0.3674 0.1303 0.7572 0.169 Uiso 1 1 calc R . . H35B H -0.3522 0.0233 0.7431 0.169 Uiso 1 1 calc R . . C36 C -0.4523(15) 0.0943(19) 0.7035(7) 0.165(10) Uani 1 1 d . . . H36A H -0.4607 0.1589 0.6924 0.247 Uiso 1 1 calc R . . H36B H -0.4988 0.0786 0.7172 0.247 Uiso 1 1 calc R . . H36C H -0.4513 0.0480 0.6823 0.247 Uiso 1 1 calc R . . C37 C 0.5530(18) 0.098(3) 0.4273(10) 0.180(13) Uani 1 1 d . . . H37 H 0.6009 0.1028 0.4149 0.216 Uiso 1 1 calc R . . C38 C 0.5557(15) 0.034(2) 0.4585(9) 0.154(10) Uani 1 1 d . . . H38 H 0.6019 -0.0088 0.4637 0.185 Uiso 1 1 calc R . . C39 C 0.4973(12) 0.0300(15) 0.4820(6) 0.099(7) Uani 1 1 d . . . C40 C 0.4306(15) 0.089(2) 0.4702(8) 0.124(8) Uani 1 1 d . . . H40 H 0.3881 0.0933 0.4859 0.149 Uiso 1 1 calc R . . C41 C 0.4217(13) 0.142(2) 0.4371(10) 0.145(10) Uani 1 1 d . . . H41 H 0.3694 0.1740 0.4291 0.174 Uiso 1 1 calc R . . C42 C 0.4876(17) 0.227(2) 0.3822(6) 0.168(10) Uani 1 1 d DU . . H42A H 0.5465 0.2500 0.3837 0.201 Uiso 1 1 calc R . . H42B H 0.4514 0.2832 0.3854 0.201 Uiso 1 1 calc R . . C43 C 0.4555(19) 0.1758(16) 0.3423(7) 0.196(12) Uani 1 1 d DU . . H43A H 0.3961 0.1548 0.3405 0.235 Uiso 1 1 calc R . . H43B H 0.4909 0.1192 0.3394 0.235 Uiso 1 1 calc R . . C44 C 0.4631(19) 0.2534(16) 0.3101(7) 0.184(11) Uani 1 1 d DU . . H44A H 0.4194 0.3035 0.3097 0.220 Uiso 1 1 calc R . . H44B H 0.5195 0.2842 0.3156 0.220 Uiso 1 1 calc R . . C45 C 0.450(3) 0.199(3) 0.2697(7) 0.40(3) Uani 1 1 d DU . . H45A H 0.5048 0.1759 0.2649 0.594 Uiso 1 1 calc R . . H45B H 0.4257 0.2433 0.2487 0.594 Uiso 1 1 calc R . . H45C H 0.4119 0.1450 0.2704 0.594 Uiso 1 1 calc R . . C46 C 0.7351(17) -0.0759(18) 0.2558(7) 0.166(10) Uani 1 1 d . . . H46A H 0.7496 -0.1271 0.2389 0.249 Uiso 1 1 calc R . . H46B H 0.6809 -0.0905 0.2637 0.249 Uiso 1 1 calc R . . H46C H 0.7792 -0.0709 0.2792 0.249 Uiso 1 1 calc R . . C47 C 0.6875(14) 0.0909(18) 0.2546(6) 0.137(8) Uani 1 1 d . . . H47A H 0.7168 0.0971 0.2818 0.206 Uiso 1 1 calc R . . H47B H 0.6282 0.0744 0.2541 0.206 Uiso 1 1 calc R . . H47C H 0.6908 0.1518 0.2408 0.206 Uiso 1 1 calc R . . C48 C 0.7578(16) 0.030(2) 0.2045(7) 0.135(9) Uani 1 1 d . . . H48 H 0.7830 -0.0206 0.1924 0.162 Uiso 1 1 calc R . . I1 I 0.26006(7) 0.36734(9) 0.40320(4) 0.0907(4) Uani 1 1 d . . . I2 I 0.19638(8) 0.16039(8) 0.28664(3) 0.0836(3) Uani 1 1 d . . . I3 I 0.02007(9) 0.39906(9) 0.31468(4) 0.1063(5) Uani 1 1 d . . . I4 I 0.21093(7) 0.02315(8) 0.40514(3) 0.0756(3) Uani 1 1 d . . . I5 I 0.02331(7) 0.23459(9) 0.43947(4) 0.0862(3) Uani 1 1 d . . . I6 I -0.06067(7) 0.09132(8) 0.32409(3) 0.0721(3) Uani 1 1 d . . . I7 I -0.25587(8) 0.31460(8) 0.36030(4) 0.0889(4) Uani 1 1 d . . . I8 I -0.30589(8) -0.01291(10) 0.36341(4) 0.1005(4) Uani 1 1 d . . . I9 I -0.04172(7) -0.06142(8) 0.43921(3) 0.0742(3) Uani 1 1 d . . . I10 I 0.22166(9) -0.14596(9) 0.51803(3) 0.0920(4) Uani 1 1 d . . . I11 I 0.26669(7) 0.20281(9) 0.52806(3) 0.0843(3) Uani 1 1 d . . . N1 N 1.1572(9) 0.6910(10) 0.3993(4) 0.072(4) Uani 1 1 d . . . N2 N 0.8287(9) 0.4822(10) 0.4801(4) 0.074(4) Uani 1 1 d . . . N3 N 0.2059(9) 0.3411(11) 0.6408(4) 0.074(4) Uani 1 1 d . . . N4 N -0.1352(9) 0.1605(10) 0.7242(4) 0.069(3) Uani 1 1 d . . . N5 N 0.4829(14) 0.1530(16) 0.4137(7) 0.146(8) Uani 1 1 d . . . N6 N 0.7285(11) 0.0140(12) 0.2347(5) 0.098(5) Uani 1 1 d . . . O1 O 0.7545(13) 0.1131(14) 0.1896(5) 0.176(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0610(4) 0.0543(4) 0.0665(4) -0.0080(3) 0.0067(3) 0.0053(3) Pb2 0.0606(4) 0.0583(4) 0.0584(4) -0.0060(3) 0.0071(3) 0.0097(3) Pb3 0.0602(3) 0.0577(4) 0.0582(3) -0.0084(3) 0.0095(3) 0.0072(3) C1 0.116(16) 0.055(12) 0.087(13) -0.025(9) -0.001(11) 0.042(11) C2 0.096(13) 0.068(12) 0.095(13) -0.042(10) 0.011(11) -0.018(11) C3 0.092(12) 0.037(9) 0.055(9) -0.012(7) -0.018(9) 0.028(9) C4 0.119(16) 0.068(13) 0.085(13) -0.005(10) 0.006(12) 0.005(11) C5 0.16(2) 0.053(11) 0.074(12) -0.009(9) 0.022(13) 0.006(12) C6 0.070(10) 0.049(10) 0.060(10) -0.012(8) -0.007(8) 0.016(9) C7 0.097(14) 0.066(12) 0.108(15) -0.005(11) 0.004(12) -0.031(11) C8 0.127(18) 0.049(12) 0.114(16) -0.028(11) -0.015(13) 0.011(11) C9 0.127(17) 0.058(12) 0.077(13) -0.004(10) 0.003(12) 0.020(12) C10 0.121(16) 0.059(12) 0.075(12) -0.008(10) 0.008(11) 0.025(11) C11 0.151(19) 0.060(12) 0.075(12) -0.011(9) -0.006(13) 0.016(12) C12 0.127(18) 0.120(18) 0.091(15) -0.019(13) -0.002(14) 0.014(15) C13 0.14(3) 0.18(3) 0.27(4) -0.01(3) 0.03(3) 0.01(2) C14 0.15(3) 0.28(4) 0.18(3) -0.04(3) 0.01(2) -0.08(3) C15 0.138(18) 0.062(12) 0.101(14) -0.007(10) 0.001(14) 0.030(12) C16 0.137(19) 0.15(2) 0.114(17) 0.009(15) 0.025(15) -0.029(17) C17 0.200(15) 0.211(16) 0.210(15) -0.003(9) 0.036(10) 0.008(10) C18 0.232(17) 0.243(17) 0.235(17) -0.014(10) 0.042(10) 0.010(10) C19 0.15(2) 0.059(13) 0.084(14) -0.033(10) -0.023(13) 0.027(13) C20 0.088(13) 0.059(12) 0.108(14) 0.019(10) 0.011(11) 0.019(10) C21 0.065(10) 0.043(9) 0.063(10) -0.006(7) -0.021(8) 0.025(8) C22 0.091(13) 0.081(13) 0.059(10) -0.020(9) 0.005(9) 0.028(10) C23 0.102(14) 0.062(12) 0.087(13) -0.011(10) 0.002(11) -0.003(11) C24 0.070(10) 0.032(8) 0.059(9) -0.012(7) -0.012(8) 0.008(7) C25 0.128(16) 0.070(13) 0.062(11) -0.001(9) 0.014(11) 0.012(11) C26 0.109(14) 0.039(9) 0.083(12) -0.005(9) -0.010(11) 0.020(9) C27 0.093(14) 0.118(18) 0.080(13) -0.047(12) -0.004(11) 0.014(13) C28 0.086(12) 0.051(10) 0.094(13) -0.030(9) -0.005(10) 0.000(9) C29 0.110(15) 0.093(14) 0.084(13) -0.018(10) 0.022(12) -0.006(12) C30 0.177(14) 0.196(15) 0.204(14) 0.011(9) 0.038(9) -0.010(9) C31 0.38(3) 0.39(3) 0.39(3) 0.004(10) 0.069(11) 0.003(10) C32 0.36(3) 0.36(3) 0.36(3) -0.004(10) 0.060(11) 0.000(10) C33 0.095(13) 0.089(13) 0.060(10) -0.011(9) 0.002(10) -0.001(10) C34 0.095(13) 0.077(12) 0.088(13) -0.007(10) 0.005(11) -0.003(10) C35 0.13(2) 0.116(19) 0.18(2) 0.008(17) 0.05(2) 0.020(16) C36 0.114(19) 0.18(3) 0.19(3) -0.02(2) 0.000(19) -0.004(18) C37 0.13(2) 0.22(4) 0.22(3) 0.02(3) 0.12(2) 0.06(2) C38 0.093(17) 0.18(3) 0.20(3) 0.02(2) 0.048(19) 0.062(18) C39 0.047(9) 0.109(19) 0.14(2) -0.035(13) 0.019(15) 0.027(12) C40 0.087(17) 0.15(2) 0.14(2) -0.010(18) 0.025(16) -0.007(16) C41 0.050(13) 0.16(3) 0.22(3) -0.05(2) 0.010(18) 0.014(15) C42 0.162(13) 0.167(13) 0.175(13) -0.005(9) 0.032(9) 0.007(9) C43 0.189(14) 0.194(14) 0.201(14) -0.009(10) 0.024(9) 0.002(9) C44 0.186(14) 0.180(14) 0.184(14) 0.007(9) 0.031(9) 0.003(9) C45 0.39(3) 0.40(3) 0.40(3) 0.000(10) 0.075(11) -0.003(10) C46 0.24(3) 0.13(2) 0.13(2) -0.005(18) 0.06(2) 0.06(2) C47 0.124(18) 0.19(3) 0.107(17) 0.008(16) 0.038(14) 0.016(18) C48 0.18(2) 0.13(2) 0.108(18) 0.023(16) 0.069(17) 0.038(19) I1 0.0713(7) 0.0806(8) 0.1122(9) -0.0127(7) -0.0053(7) 0.0014(6) I2 0.0931(8) 0.0764(8) 0.0864(8) -0.0021(6) 0.0297(6) 0.0047(6) I3 0.1127(10) 0.0651(8) 0.1222(10) -0.0244(7) -0.0297(8) 0.0267(7) I4 0.0941(8) 0.0667(7) 0.0687(7) -0.0016(5) 0.0222(6) 0.0142(6) I5 0.0876(8) 0.0774(8) 0.0903(8) -0.0138(6) 0.0069(6) 0.0097(6) I6 0.0809(7) 0.0693(7) 0.0672(7) 0.0018(5) 0.0163(5) 0.0046(6) I7 0.0983(8) 0.0695(8) 0.0934(8) 0.0019(6) 0.0023(7) 0.0227(7) I8 0.0878(9) 0.0954(10) 0.1145(10) -0.0107(8) 0.0082(7) 0.0026(7) I9 0.0754(7) 0.0723(7) 0.0740(7) -0.0077(6) 0.0107(5) 0.0072(6) I10 0.1289(10) 0.0771(8) 0.0758(8) 0.0007(6) 0.0339(7) 0.0323(7) I11 0.0715(7) 0.0893(9) 0.0894(8) -0.0153(6) 0.0070(6) 0.0019(6) N1 0.093(10) 0.055(9) 0.061(8) 0.005(7) -0.002(7) 0.024(8) N2 0.080(9) 0.063(9) 0.074(9) 0.003(7) 0.002(7) 0.024(8) N3 0.085(10) 0.071(10) 0.063(8) 0.001(7) 0.007(7) 0.010(8) N4 0.084(10) 0.059(9) 0.061(8) -0.008(7) 0.007(7) 0.020(8) N5 0.104(14) 0.154(19) 0.19(2) -0.011(15) 0.067(15) 0.043(14) N6 0.136(14) 0.079(12) 0.088(11) 0.014(9) 0.042(11) 0.004(10) O1 0.25(2) 0.143(16) 0.148(15) 0.055(12) 0.080(14) 0.017(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 Pb1 I3 3.0463(13) . ? Pb1 I2 3.0639(12) . ? Pb1 I1 3.1715(12) . ? Pb1 I6 3.3524(12) . ? Pb1 I5 3.3525(14) . ? Pb1 I4 3.4043(12) . ? Pb2 I8 3.0016(14) . ? Pb2 I6 3.1017(12) . ? Pb2 I7 3.1456(12) . ? Pb2 I10 3.3140(12) 3_556 ? Pb2 I9 3.3292(12) . ? Pb2 I5 3.3726(13) . ? Pb3 I11 3.0903(12) . ? Pb3 I5 3.1490(13) . ? Pb3 I4 3.1635(11) . ? Pb3 I9 3.2116(12) 3_556 ? Pb3 I10 3.2733(13) . ? Pb3 I9 3.3053(12) . ? C1 C2 1.31(2) . ? C1 N1 1.34(2) . ? C1 H1 0.9300 . ? C2 C3 1.34(2) . ? C2 H2 0.9300 . ? C3 C6 1.38(2) . ? C3 C4 1.40(2) . ? C4 C5 1.36(2) . ? C4 H4 0.9300 . ? C5 N1 1.31(2) . ? C5 H5 0.9300 . ? C6 C7 1.37(2) . ? C6 C10 1.38(2) . ? C7 C8 1.31(2) . ? C7 H7 0.9300 . ? C8 N2 1.36(2) . ? C8 H8 0.9300 . ? C9 C10 1.30(2) . ? C9 N2 1.314(19) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.46(2) . ? C11 N1 1.50(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.61(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.43(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N2 1.51(2) . ? C15 C16 1.54(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.53(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.55(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.36(2) . ? C19 C20 1.37(2) . ? C19 H19 0.9300 . ? C20 C21 1.34(2) . ? C20 H20 0.9300 . ? C21 C22 1.39(2) . ? C21 C24 1.42(2) . ? C22 C23 1.35(2) . ? C22 H22 0.9300 . ? C23 N3 1.31(2) . ? C23 H23 0.9300 . ? C24 C28 1.33(2) . ? C24 C25 1.38(2) . ? C25 C26 1.42(2) . ? C25 H25 0.9300 . ? C26 N4 1.304(19) . ? C26 H26 0.9300 . ? C27 N4 1.32(2) . ? C27 C28 1.36(2) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 N3 1.447(19) . ? C29 C30 1.54(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.54(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.55(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 N4 1.457(19) . ? C33 C34 1.52(2) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.50(2) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.58(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N5 1.35(3) . ? C37 C38 1.36(3) . ? C37 H37 0.9300 . ? C38 C39 1.32(3) . ? C38 H38 0.9300 . ? C39 C40 1.33(3) . ? C39 C39 1.46(4) 3_656 ? C40 C41 1.32(3) . ? C40 H40 0.9300 . ? C41 N5 1.36(3) . ? C41 H41 0.9300 . ? C42 N5 1.49(3) . ? C42 C43 1.53(3) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.54(3) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.54(4) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 N6 1.42(2) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 N6 1.46(2) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 N6 1.22(2) . ? C48 O1 1.24(2) . ? C48 H48 0.9300 . ? I9 Pb3 3.2114(12) 3_556 ? I10 Pb2 3.3141(12) 3_556 ? 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 I3 Pb1 I2 94.80(4) . . ? I3 Pb1 I1 90.27(4) . . ? I2 Pb1 I1 101.28(4) . . ? I3 Pb1 I6 87.35(3) . . ? I2 Pb1 I6 90.41(3) . . ? I1 Pb1 I6 168.22(3) . . ? I3 Pb1 I5 96.81(4) . . ? I2 Pb1 I5 165.37(4) . . ? I1 Pb1 I5 87.55(3) . . ? I6 Pb1 I5 81.28(3) . . ? I3 Pb1 I4 176.53(4) . . ? I2 Pb1 I4 85.76(3) . . ? I1 Pb1 I4 92.98(3) . . ? I6 Pb1 I4 89.22(3) . . ? I5 Pb1 I4 82.13(3) . . ? I8 Pb2 I6 96.09(4) . . ? I8 Pb2 I7 95.51(4) . . ? I6 Pb2 I7 96.31(3) . . ? I8 Pb2 I10 92.22(4) . 3_556 ? I6 Pb2 I10 167.06(3) . 3_556 ? I7 Pb2 I10 92.74(3) . 3_556 ? I8 Pb2 I9 91.26(3) . . ? I6 Pb2 I9 86.14(3) . . ? I7 Pb2 I9 172.51(3) . . ? I10 Pb2 I9 83.77(3) 3_556 . ? I8 Pb2 I5 168.23(4) . . ? I6 Pb2 I5 84.73(3) . . ? I7 Pb2 I5 96.08(3) . . ? I10 Pb2 I5 85.13(3) 3_556 . ? I9 Pb2 I5 77.06(3) . . ? I11 Pb3 I5 90.95(3) . . ? I11 Pb3 I4 99.86(3) . . ? I5 Pb3 I4 89.36(3) . . ? I11 Pb3 I9 87.40(3) . 3_556 ? I5 Pb3 I9 95.67(3) . 3_556 ? I4 Pb3 I9 171.12(3) . 3_556 ? I11 Pb3 I10 98.56(4) . . ? I5 Pb3 I10 170.37(4) . . ? I4 Pb3 I10 87.54(3) . . ? I9 Pb3 I10 86.31(3) 3_556 . ? I11 Pb3 I9 168.44(3) . . ? I5 Pb3 I9 80.56(3) . . ? I4 Pb3 I9 87.95(3) . . ? I9 Pb3 I9 85.67(3) 3_556 . ? I10 Pb3 I9 90.22(3) . . ? C2 C1 N1 119.5(17) . . ? C2 C1 H1 120.2 . . ? N1 C1 H1 120.2 . . ? C1 C2 C3 126.3(17) . . ? C1 C2 H2 116.9 . . ? C3 C2 H2 116.9 . . ? C2 C3 C6 124.8(16) . . ? C2 C3 C4 110.8(18) . . ? C6 C3 C4 124.3(16) . . ? C5 C4 C3 124.8(19) . . ? C5 C4 H4 117.6 . . ? C3 C4 H4 117.6 . . ? N1 C5 C4 118.0(18) . . ? N1 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C7 C6 C3 121.4(16) . . ? C7 C6 C10 110.9(17) . . ? C3 C6 C10 127.7(16) . . ? C8 C7 C6 123.5(18) . . ? C8 C7 H7 118.3 . . ? C6 C7 H7 118.3 . . ? C7 C8 N2 119.9(19) . . ? C7 C8 H8 120.0 . . ? N2 C8 H8 120.0 . . ? C10 C9 N2 117.4(18) . . ? C10 C9 H9 121.3 . . ? N2 C9 H9 121.3 . . ? C9 C10 C6 127.8(18) . . ? C9 C10 H10 116.1 . . ? C6 C10 H10 116.1 . . ? C12 C11 N1 113.2(16) . . ? C12 C11 H11A 108.9 . . ? N1 C11 H11A 108.9 . . ? C12 C11 H11B 108.9 . . ? N1 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 C13 112(2) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 111(3) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 110.9(13) . . ? N2 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 107.0(11) . . ? C17 C16 H16A 110.3 . . ? C15 C16 H16A 110.3 . . ? C17 C16 H16B 110.3 . . ? C15 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? C16 C17 C18 103.7(12) . . ? C16 C17 H17A 111.0 . . ? C18 C17 H17A 111.0 . . ? C16 C17 H17B 111.0 . . ? C18 C17 H17B 111.0 . . ? H17A C17 H17B 109.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 122.4(19) . . ? N3 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C21 C20 C19 120.3(18) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 117.0(17) . . ? C20 C21 C24 123.5(16) . . ? C22 C21 C24 119.6(15) . . ? C23 C22 C21 120.7(16) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? N3 C23 C22 122.7(17) . . ? N3 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C28 C24 C25 115.7(16) . . ? C28 C24 C21 125.4(15) . . ? C25 C24 C21 118.8(15) . . ? C24 C25 C26 120.0(16) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? N4 C26 C25 120.9(16) . . ? N4 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? N4 C27 C28 121.7(17) . . ? N4 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C24 C28 C27 122.9(16) . . ? C24 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? N3 C29 C30 109.7(14) . . ? N3 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? N3 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C29 104.9(12) . . ? C31 C30 H30A 110.8 . . ? C29 C30 H30A 110.8 . . ? C31 C30 H30B 110.8 . . ? C29 C30 H30B 110.8 . . ? H30A C30 H30B 108.8 . . ? C32 C31 C30 104.1(13) . . ? C32 C31 H31A 110.9 . . ? C30 C31 H31A 110.9 . . ? C32 C31 H31B 110.9 . . ? C30 C31 H31B 110.9 . . ? H31A C31 H31B 108.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C33 C34 112.3(13) . . ? N4 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? N4 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 111.7(16) . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? C33 C34 H34B 109.3 . . ? H34A C34 H34B 107.9 . . ? C34 C35 C36 110.0(19) . . ? C34 C35 H35A 109.7 . . ? C36 C35 H35A 109.7 . . ? C34 C35 H35B 109.7 . . ? C36 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 C38 122(2) . . ? N5 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C39 C38 C37 125(2) . . ? C39 C38 H38 117.6 . . ? C37 C38 H38 117.6 . . ? C38 C39 C40 113(2) . . ? C38 C39 C39 126(2) . 3_656 ? C40 C39 C39 121(3) . 3_656 ? C41 C40 C39 123(3) . . ? C41 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? C40 C41 N5 125(3) . . ? C40 C41 H41 117.3 . . ? N5 C41 H41 117.3 . . ? N5 C42 C43 105.6(19) . . ? N5 C42 H42A 110.6 . . ? C43 C42 H42A 110.6 . . ? N5 C42 H42B 110.6 . . ? C43 C42 H42B 110.6 . . ? H42A C42 H42B 108.8 . . ? C42 C43 C44 104.7(12) . . ? C42 C43 H43A 110.8 . . ? C44 C43 H43A 110.8 . . ? C42 C43 H43B 110.8 . . ? C44 C43 H43B 110.8 . . ? H43A C43 H43B 108.9 . . ? C45 C44 C43 106.6(13) . . ? C45 C44 H44A 110.4 . . ? C43 C44 H44A 110.4 . . ? C45 C44 H44B 110.4 . . ? C43 C44 H44B 110.4 . . ? H44A C44 H44B 108.6 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N6 C46 H46A 109.5 . . ? N6 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N6 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N6 C47 H47A 109.5 . . ? N6 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N6 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N6 C48 O1 121(2) . . ? N6 C48 H48 119.5 . . ? O1 C48 H48 119.5 . . ? Pb3 I4 Pb1 93.34(3) . . ? Pb3 I5 Pb1 94.61(3) . . ? Pb3 I5 Pb2 102.35(4) . . ? Pb1 I5 Pb2 93.94(3) . . ? Pb2 I6 Pb1 99.15(3) . . ? Pb3 I9 Pb3 94.33(3) 3_556 . ? Pb3 I9 Pb2 94.54(3) 3_556 . ? Pb3 I9 Pb2 100.01(3) . . ? Pb3 I10 Pb2 93.68(3) . 3_556 ? C5 N1 C1 120.5(17) . . ? C5 N1 C11 117.1(16) . . ? C1 N1 C11 122.0(16) . . ? C9 N2 C8 120.3(18) . . ? C9 N2 C15 118.1(16) . . ? C8 N2 C15 121.5(16) . . ? C23 N3 C19 116.8(17) . . ? C23 N3 C29 120.6(16) . . ? C19 N3 C29 122.6(17) . . ? C26 N4 C27 118.8(17) . . ? C26 N4 C33 118.9(16) . . ? C27 N4 C33 122.3(15) . . ? C37 N5 C41 111(2) . . ? C37 N5 C42 119(2) . . ? C41 N5 C42 129(2) . . ? C48 N6 C46 125(2) . . ? C48 N6 C47 122(2) . . ? C46 N6 C47 112.9(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C37 H37 I8 0.93 2.94 3.70(2) 139.5 1_655 C7 H7 I5 0.93 2.94 3.607(19) 129.7 3_666 C11 H11A O1 0.97 2.13 3.08(2) 165.5 2_755 C19 H19 I8 0.93 2.96 3.722(17) 139.7 3_556 C22 H22 I3 0.93 2.91 3.717(16) 145.3 3_566 C27 H27 I6 0.93 2.92 3.702(17) 143.0 4_566 C4 H4 I9 0.93 2.95 3.581(18) 126.5 1_665 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.207 _refine_diff_density_min -1.783 _refine_diff_density_rms 0.183 # start Validation Reply Form _vrf_PLAT220_100426dm ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.79 Ratio RESPONSE: This is due to some untreated disorders of some carbon atoms. ; _vrf_PLAT241_100426dm ; PROBLEM: Check High Ueq as Compared to Neighbors for C31 RESPONSE: This is due to some untreated disorders of some carbon atoms. ; _vrf_PLAT242_100426dm ; PROBLEM: Check Low Ueq as Compared to Neighbors for C44 RESPONSE: This is due to some untreated disorders of some carbon atoms. ; _vrf_PLAT234_100426dm ; PROBLEM: Large Hirshfeld Difference C16-- C17 .. 0.33 Ang. RESPONSE: This is due to some untreated disorders of some carbon atoms. ; # Attachment '- revised CIF1.cif' data_ag _database_code_depnum_ccdc_archive 'CCDC 793447' #TrackingRef '- revised CIF1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H26 N2, 0.5(Ag2 I6)' _chemical_formula_sum 'C18 H26 Ag I3 N2' _chemical_formula_weight 758.98 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/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 26.5920(13) _cell_length_b 11.1777(5) _cell_length_c 16.1137(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.9930(10) _cell_angle_gamma 90.00 _cell_volume 4471.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.4 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 5.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5181 _exptl_absorpt_correction_T_max 0.6323 _exptl_absorpt_process_details 'SADABS, Sheldrick,1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20362 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5140 _reflns_number_gt 4492 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+12.6567P] 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 5140 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.003 _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 I1 I 0.708660(9) 0.32963(2) 0.868531(15) 0.02005(7) Uani 1 1 d . . . I2 I 0.859685(10) 0.10280(2) 0.898949(16) 0.02585(7) Uani 1 1 d . . . I3 I 0.880705(10) 0.47801(2) 1.039021(16) 0.02596(7) Uani 1 1 d . . . Ag1 Ag 0.818355(11) 0.27225(3) 0.986590(19) 0.02444(7) Uani 1 1 d . . . N1 N 0.54525(15) 0.2982(3) 0.5720(2) 0.0315(8) Uani 1 1 d . . . N2 N 0.71723(12) 0.9273(3) 0.80926(19) 0.0205(6) Uani 1 1 d . . . C1 C 0.57923(17) 0.3290(3) 0.6527(3) 0.0295(9) Uani 1 1 d . . . H1 H 0.6154 0.3490 0.6608 0.035 Uiso 1 1 calc R . . C2 C 0.56245(15) 0.3322(4) 0.7240(3) 0.0271(8) Uani 1 1 d . . . H2 H 0.5871 0.3530 0.7813 0.032 Uiso 1 1 calc R . . C3 C 0.50943(15) 0.3050(3) 0.7118(3) 0.0240(8) Uani 1 1 d . . . C4 C 0.47470(16) 0.2758(4) 0.6274(3) 0.0302(9) Uani 1 1 d . . . H4 H 0.4380 0.2583 0.6170 0.036 Uiso 1 1 calc R . . C5 C 0.49352(18) 0.2724(4) 0.5590(3) 0.0352(10) Uani 1 1 d . . . H5 H 0.4697 0.2513 0.5012 0.042 Uiso 1 1 calc R . . C6 C 0.5651(2) 0.2939(4) 0.4967(3) 0.0431(12) Uani 1 1 d . B . H6A H 0.5597 0.2123 0.4710 0.052 Uiso 1 1 calc R . . H6B H 0.6042 0.3113 0.5190 0.052 Uiso 1 1 calc R . . C7 C 0.53586(18) 0.3835(4) 0.4247(3) 0.0359(10) Uani 1 1 d . . . H7A H 0.5465 0.4657 0.4470 0.043 Uiso 0.50 1 calc PR A 1 H7B H 0.4965 0.3757 0.4099 0.043 Uiso 0.50 1 calc PR A 1 H7C H 0.5272 0.4561 0.4523 0.043 Uiso 0.50 1 d PR A 2 H7D H 0.5016 0.3481 0.3849 0.043 Uiso 0.50 1 d PR A 2 C8 C 0.5493(4) 0.3626(9) 0.3405(6) 0.035(2) Uani 0.50 1 d P B 1 H8A H 0.5374 0.2817 0.3165 0.042 Uiso 0.50 1 calc PR B 1 H8B H 0.5303 0.4220 0.2945 0.042 Uiso 0.50 1 calc PR B 1 C9 C 0.6092(4) 0.3744(10) 0.3637(7) 0.042(2) Uani 0.50 1 d P B 1 H9A H 0.6180 0.3619 0.3103 0.063 Uiso 0.50 1 calc PR B 1 H9B H 0.6278 0.3144 0.4086 0.063 Uiso 0.50 1 calc PR B 1 H9C H 0.6207 0.4546 0.3875 0.063 Uiso 0.50 1 calc PR B 1 C8' C 0.5711(4) 0.4177(9) 0.3684(6) 0.0316(18) Uani 0.50 1 d P B 2 H8'1 H 0.5508 0.4742 0.3209 0.038 Uiso 0.50 1 calc PR B 2 H8'2 H 0.6042 0.4588 0.4071 0.038 Uiso 0.50 1 calc PR B 2 C9' C 0.5868(4) 0.3090(9) 0.3265(6) 0.037(2) Uani 0.50 1 d P B 2 H9'1 H 0.6090 0.3343 0.2926 0.056 Uiso 0.50 1 calc PR B 2 H9'2 H 0.5542 0.2695 0.2866 0.056 Uiso 0.50 1 calc PR B 2 H9'3 H 0.6072 0.2531 0.3733 0.056 Uiso 0.50 1 calc PR B 2 C10 C 0.71660(16) 0.8074(3) 0.8018(3) 0.0265(8) Uani 1 1 d . . . H10 H 0.7068 0.7718 0.7447 0.032 Uiso 1 1 calc R . . C11 C 0.72982(16) 0.7363(3) 0.8753(3) 0.0248(8) Uani 1 1 d . . . H11 H 0.7291 0.6518 0.8689 0.030 Uiso 1 1 calc R . . C12 C 0.74434(14) 0.7868(3) 0.9594(2) 0.0206(7) Uani 1 1 d . . . C13 C 0.74685(15) 0.9109(3) 0.9650(3) 0.0253(8) Uani 1 1 d . . . H13 H 0.7583 0.9486 1.0215 0.030 Uiso 1 1 calc R . . C14 C 0.73304(15) 0.9792(3) 0.8896(2) 0.0235(8) Uani 1 1 d . . . H14 H 0.7346 1.0639 0.8943 0.028 Uiso 1 1 calc R . . C15 C 0.69720(16) 1.0044(4) 0.7295(2) 0.0261(8) Uani 1 1 d . . . H15A H 0.7003 0.9612 0.6779 0.031 Uiso 1 1 calc R . . H15B H 0.7196 1.0775 0.7393 0.031 Uiso 1 1 calc R . . C16 C 0.63870(16) 1.0390(4) 0.7097(3) 0.0270(8) Uani 1 1 d . . . H16A H 0.6367 1.0888 0.7592 0.032 Uiso 1 1 calc R . . H16B H 0.6262 1.0885 0.6552 0.032 Uiso 1 1 calc R . . C17 C 0.60113(16) 0.9338(4) 0.6972(3) 0.0303(9) Uani 1 1 d . . . H17A H 0.6100 0.8906 0.7543 0.036 Uiso 1 1 calc R . . H17B H 0.6064 0.8779 0.6534 0.036 Uiso 1 1 calc R . . C18 C 0.54245(18) 0.9729(5) 0.6651(4) 0.0465(12) Uani 1 1 d . . . H18A H 0.5193 0.9024 0.6568 0.070 Uiso 1 1 calc R . . H18B H 0.5335 1.0157 0.6086 0.070 Uiso 1 1 calc R . . H18C H 0.5368 1.0260 0.7094 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 I1 0.01688(12) 0.02262(12) 0.02106(12) -0.00032(8) 0.00729(9) -0.00130(8) I2 0.02427(13) 0.02750(13) 0.02870(13) 0.00109(9) 0.01304(10) 0.00397(9) I3 0.02238(13) 0.02885(14) 0.02807(13) -0.00173(10) 0.01077(10) -0.00565(10) Ag1 0.02012(14) 0.02745(15) 0.02691(15) -0.00151(11) 0.00986(11) -0.00169(11) N1 0.036(2) 0.0302(18) 0.0343(19) 0.0037(14) 0.0202(16) 0.0112(15) N2 0.0177(14) 0.0247(15) 0.0217(15) 0.0035(12) 0.0103(12) 0.0013(12) C1 0.025(2) 0.025(2) 0.040(2) 0.0033(16) 0.0150(18) 0.0016(16) C2 0.0179(18) 0.031(2) 0.032(2) 0.0010(16) 0.0092(16) 0.0008(15) C3 0.0199(18) 0.0203(18) 0.032(2) 0.0013(15) 0.0099(16) 0.0028(14) C4 0.0224(19) 0.032(2) 0.034(2) -0.0047(17) 0.0083(17) -0.0018(16) C5 0.033(2) 0.040(2) 0.030(2) -0.0044(18) 0.0084(18) 0.0041(19) C6 0.055(3) 0.043(3) 0.043(3) 0.009(2) 0.033(2) 0.024(2) C7 0.035(2) 0.039(2) 0.039(2) 0.0049(19) 0.020(2) 0.0132(19) C8 0.030(5) 0.039(5) 0.036(5) -0.007(4) 0.012(4) -0.008(4) C9 0.036(5) 0.050(6) 0.048(6) 0.003(5) 0.025(5) 0.003(5) C8' 0.034(5) 0.031(5) 0.035(5) 0.002(4) 0.018(4) 0.002(4) C9' 0.039(5) 0.043(5) 0.033(5) 0.002(4) 0.017(4) 0.001(4) C10 0.032(2) 0.0247(19) 0.0281(19) -0.0006(15) 0.0171(17) 0.0021(16) C11 0.032(2) 0.0195(18) 0.0265(19) -0.0027(14) 0.0147(16) 0.0005(15) C12 0.0159(16) 0.0217(18) 0.0260(18) 0.0000(14) 0.0097(14) 0.0013(14) C13 0.0256(19) 0.0248(19) 0.0239(18) -0.0032(14) 0.0071(15) -0.0006(15) C14 0.0210(18) 0.0230(19) 0.0274(19) -0.0047(14) 0.0097(15) -0.0015(14) C15 0.030(2) 0.030(2) 0.0239(18) 0.0041(15) 0.0156(16) 0.0053(16) C16 0.029(2) 0.029(2) 0.0260(19) -0.0024(15) 0.0124(16) 0.0068(16) C17 0.025(2) 0.036(2) 0.029(2) 0.0004(17) 0.0096(16) 0.0052(17) C18 0.028(2) 0.056(3) 0.054(3) -0.001(2) 0.013(2) 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 I1 Ag1 2.9093(4) 7_657 ? I1 Ag1 2.9263(4) . ? I2 Ag1 2.8111(4) . ? I3 Ag1 2.7836(4) . ? Ag1 I1 2.9094(4) 7_657 ? N1 C1 1.335(6) . ? N1 C5 1.347(6) . ? N1 C6 1.487(5) . ? N2 C14 1.342(5) . ? N2 C10 1.346(5) . ? N2 C15 1.479(5) . ? C1 C2 1.375(6) . ? C1 H1 0.9500 . ? C2 C3 1.386(5) . ? C2 H2 0.9500 . ? C3 C4 1.382(6) . ? C3 C3 1.486(7) 2_656 ? C4 C5 1.364(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.519(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.541(10) . ? C7 C8' 1.569(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 H7C 0.9900 . ? C7 H7D 0.9900 . ? C8 C9 1.504(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C8' C9' 1.518(13) . ? C8' H8'1 0.9900 . ? C8' H8'2 0.9900 . ? C9' H9'1 0.9800 . ? C9' H9'2 0.9800 . ? C9' H9'3 0.9800 . ? C10 C11 1.363(5) . ? C10 H10 0.9500 . ? C11 C12 1.390(5) . ? C11 H11 0.9500 . ? C12 C13 1.391(5) . ? C12 C12 1.481(7) 7_667 ? C13 C14 1.368(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.522(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.510(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.522(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag1 I1 Ag1 82.399(10) 7_657 . ? I3 Ag1 I2 114.307(12) . . ? I3 Ag1 I1 111.798(12) . 7_657 ? I2 Ag1 I1 113.125(12) . 7_657 ? I3 Ag1 I1 111.276(12) . . ? I2 Ag1 I1 107.408(12) . . ? I1 Ag1 I1 97.598(10) 7_657 . ? C1 N1 C5 120.3(4) . . ? C1 N1 C6 119.2(4) . . ? C5 N1 C6 120.5(4) . . ? C14 N2 C10 120.4(3) . . ? C14 N2 C15 118.6(3) . . ? C10 N2 C15 120.9(3) . . ? N1 C1 C2 120.8(4) . . ? N1 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C1 C2 C3 119.6(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 118.6(4) . . ? C4 C3 C3 120.7(4) . 2_656 ? C2 C3 C3 120.7(4) . 2_656 ? C5 C4 C3 119.5(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 121.2(4) . . ? N1 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? N1 C6 C7 111.5(3) . . ? N1 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N1 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C6 C7 C8 110.8(5) . . ? C6 C7 C8' 110.7(5) . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? C8' C7 H7B 132.9 . . ? H7A C7 H7B 108.1 . . ? C6 C7 H7C 109.6 . . ? C8 C7 H7C 133.1 . . ? C8' C7 H7C 110.0 . . ? H7B C7 H7C 77.6 . . ? C6 C7 H7D 109.4 . . ? C8' C7 H7D 108.9 . . ? H7A C7 H7D 133.1 . . ? H7C C7 H7D 108.1 . . ? C9 C8 C7 109.1(8) . . ? C9 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? C9 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C9' C8' C7 112.2(7) . . ? C9' C8' H8'1 109.2 . . ? C7 C8' H8'1 109.2 . . ? C9' C8' H8'2 109.2 . . ? C7 C8' H8'2 109.2 . . ? H8'1 C8' H8'2 107.9 . . ? C8' C9' H9'1 109.5 . . ? C8' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C8' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? N2 C10 C11 120.8(3) . . ? N2 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C13 117.2(3) . . ? C11 C12 C12 122.3(4) . 7_667 ? C13 C12 C12 120.5(4) . 7_667 ? C14 C13 C12 120.5(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? N2 C14 C13 120.5(3) . . ? N2 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? N2 C15 C16 110.7(3) . . ? N2 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 114.1(3) . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C16 C17 C18 111.7(4) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag1 I1 Ag1 I3 -116.998(14) 7_657 . . . ? Ag1 I1 Ag1 I2 117.198(14) 7_657 . . . ? Ag1 I1 Ag1 I1 0.0 7_657 . . 7_657 ? C5 N1 C1 C2 1.5(6) . . . . ? C6 N1 C1 C2 -179.0(4) . . . . ? N1 C1 C2 C3 -1.0(6) . . . . ? C1 C2 C3 C4 -0.3(6) . . . . ? C1 C2 C3 C3 178.5(3) . . . 2_656 ? C2 C3 C4 C5 1.2(6) . . . . ? C3 C3 C4 C5 -177.7(3) 2_656 . . . ? C1 N1 C5 C4 -0.6(6) . . . . ? C6 N1 C5 C4 179.9(4) . . . . ? C3 C4 C5 N1 -0.8(6) . . . . ? C1 N1 C6 C7 -117.6(5) . . . . ? C5 N1 C6 C7 61.8(6) . . . . ? N1 C6 C7 C8 -169.8(5) . . . . ? N1 C6 C7 C8' 156.1(5) . . . . ? C6 C7 C8 C9 -59.0(9) . . . . ? C8' C7 C8 C9 37.1(9) . . . . ? C6 C7 C8' C9' 57.2(9) . . . . ? C8 C7 C8' C9' -39.2(9) . . . . ? C14 N2 C10 C11 2.7(6) . . . . ? C15 N2 C10 C11 -173.2(3) . . . . ? N2 C10 C11 C12 -0.1(6) . . . . ? C10 C11 C12 C13 -2.6(6) . . . . ? C10 C11 C12 C12 176.0(4) . . . 7_667 ? C11 C12 C13 C14 2.9(6) . . . . ? C12 C12 C13 C14 -175.8(4) 7_667 . . . ? C10 N2 C14 C13 -2.4(5) . . . . ? C15 N2 C14 C13 173.6(3) . . . . ? C12 C13 C14 N2 -0.5(6) . . . . ? C14 N2 C15 C16 -80.7(4) . . . . ? C10 N2 C15 C16 95.3(4) . . . . ? N2 C15 C16 C17 -56.9(4) . . . . ? C15 C16 C17 C18 -172.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.088 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.137 # Attachment '- revised CIF4.CIF' data_cu _database_code_depnum_ccdc_archive 'CCDC 793448' #TrackingRef '- revised CIF4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Cu4 N8 S6' _chemical_formula_weight 873.05 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' Cu Cu 0.3201 1.2651 '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 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 12.6080(7) _cell_length_b 9.7404(5) _cell_length_c 25.4217(14) _cell_angle_alpha 90.00 _cell_angle_beta 96.4030(10) _cell_angle_gamma 90.00 _cell_volume 3102.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 3.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3664 _exptl_absorpt_correction_T_max 0.7441 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14174 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3579 _reflns_number_gt 3320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-SEED (Barbour, 2001)' _computing_publication_material 'publCIF (Westrip, 2010)' _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^)+(0.0275P)^2^+4.2668P] 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 3579 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.651977(18) 0.93789(2) 0.826227(9) 0.01654(7) Uani 1 1 d . . . Cu2 Cu 0.498270(17) 0.72265(2) 0.849111(8) 0.01381(7) Uani 1 1 d . . . S1 S 0.52352(4) 0.97275(5) 0.647376(17) 0.01338(9) Uani 1 1 d . . . S2 S 0.94797(4) 1.13651(5) 0.927944(17) 0.01459(10) Uani 1 1 d . . . S3 S 0.67091(3) 0.68465(5) 0.823096(17) 0.01206(9) Uani 1 1 d . . . N1 N 0.63090(12) 0.33233(15) 0.87893(6) 0.0118(3) Uani 1 1 d . . . N2 N 0.63209(12) 0.98938(16) 0.75068(6) 0.0146(3) Uani 1 1 d . . . N3 N 0.76681(13) 1.00395(17) 0.87665(6) 0.0160(3) Uani 1 1 d . . . N4 N 0.60076(12) 0.66352(16) 0.71398(6) 0.0135(3) Uani 1 1 d . . . C1 C 0.88261(19) 0.6269(2) 0.99502(9) 0.0315(5) Uani 1 1 d . . . H1A H 0.9279 0.6281 1.0290 0.047 Uiso 1 1 calc R . . H1B H 0.8347 0.7064 0.9929 0.047 Uiso 1 1 calc R . . H1C H 0.9276 0.6306 0.9660 0.047 Uiso 1 1 calc R . . C2 C 0.81663(18) 0.4952(2) 0.99065(8) 0.0245(4) Uani 1 1 d . . . H2A H 0.8653 0.4151 0.9936 0.029 Uiso 1 1 calc R . . H2B H 0.7724 0.4909 1.0204 0.029 Uiso 1 1 calc R . . C3 C 0.74450(15) 0.4867(2) 0.93879(7) 0.0153(4) Uani 1 1 d . . . H3A H 0.7875 0.5004 0.9089 0.018 Uiso 1 1 calc R . . H3B H 0.6905 0.5609 0.9375 0.018 Uiso 1 1 calc R . . C4 C 0.68842(15) 0.34839(19) 0.93294(7) 0.0150(4) Uani 1 1 d . . . H4A H 0.7417 0.2739 0.9396 0.018 Uiso 1 1 calc R . . H4B H 0.6370 0.3406 0.9595 0.018 Uiso 1 1 calc R . . C5 C 0.52410(15) 0.33952(19) 0.87119(7) 0.0142(3) Uani 1 1 d . . . H5A H 0.4848 0.3470 0.9008 0.017 Uiso 1 1 calc R . . C6 C 0.47048(15) 0.33619(19) 0.82093(7) 0.0148(4) Uani 1 1 d . . . H6 H 0.3948 0.3427 0.8160 0.018 Uiso 1 1 calc R . . C7 C 0.52777(14) 0.32321(17) 0.77729(7) 0.0107(3) Uani 1 1 d . . . C8 C 0.63831(14) 0.31162(19) 0.78669(7) 0.0138(3) Uani 1 1 d . . . H8 H 0.6793 0.2997 0.7579 0.017 Uiso 1 1 calc R . . C9 C 0.68841(15) 0.31740(19) 0.83764(7) 0.0143(4) Uani 1 1 d . . . H9 H 0.7640 0.3108 0.8437 0.017 Uiso 1 1 calc R . . C10 C 0.58842(14) 0.98485(18) 0.70812(7) 0.0137(3) Uani 1 1 d . . . C11 C 0.84128(14) 1.05718(18) 0.89791(7) 0.0130(3) Uani 1 1 d . . . C12 C 0.62994(13) 0.67013(18) 0.75860(7) 0.0119(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01476(12) 0.01993(13) 0.01442(12) -0.00270(8) -0.00057(9) -0.00306(9) Cu2 0.01310(12) 0.01718(12) 0.01109(11) -0.00036(8) 0.00100(8) -0.00173(8) S1 0.0144(2) 0.0134(2) 0.0127(2) 0.00157(15) 0.00286(16) -0.00021(17) S2 0.0143(2) 0.0188(2) 0.0105(2) -0.00129(16) 0.00031(16) -0.00472(17) S3 0.0114(2) 0.0137(2) 0.01089(19) 0.00027(15) 0.00028(15) 0.00081(16) N1 0.0131(7) 0.0104(7) 0.0117(7) 0.0000(5) 0.0014(6) 0.0001(6) N2 0.0143(7) 0.0136(7) 0.0166(8) -0.0004(6) 0.0045(6) -0.0028(6) N3 0.0164(8) 0.0188(8) 0.0134(7) -0.0016(6) 0.0034(6) -0.0015(6) N4 0.0116(7) 0.0139(7) 0.0151(8) 0.0002(6) 0.0021(6) 0.0012(6) C1 0.0290(12) 0.0321(13) 0.0314(12) -0.0086(10) -0.0043(9) -0.0091(10) C2 0.0273(11) 0.0313(12) 0.0136(9) -0.0004(8) -0.0033(8) -0.0096(9) C3 0.0139(8) 0.0182(9) 0.0138(8) -0.0005(7) 0.0011(7) -0.0013(7) C4 0.0160(9) 0.0192(9) 0.0095(8) 0.0000(7) -0.0003(7) 0.0000(7) C5 0.0142(8) 0.0151(9) 0.0142(8) -0.0008(7) 0.0052(7) -0.0002(7) C6 0.0117(8) 0.0167(9) 0.0162(9) 0.0003(7) 0.0029(7) 0.0008(7) C7 0.0131(8) 0.0067(7) 0.0124(8) 0.0006(6) 0.0019(7) -0.0006(6) C8 0.0128(8) 0.0144(9) 0.0149(8) -0.0017(7) 0.0041(7) 0.0003(7) C9 0.0112(8) 0.0167(9) 0.0155(8) -0.0002(7) 0.0030(7) 0.0013(7) C10 0.0125(8) 0.0098(8) 0.0201(9) -0.0005(7) 0.0073(7) -0.0011(7) C11 0.0156(9) 0.0140(8) 0.0098(8) 0.0003(6) 0.0027(6) 0.0003(7) C12 0.0097(8) 0.0099(8) 0.0164(9) 0.0006(6) 0.0032(6) 0.0007(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 Cu1 N3 1.9337(16) . ? Cu1 N2 1.9738(15) . ? Cu1 S1 2.4068(5) 2_656 ? Cu1 S3 2.4803(5) . ? Cu1 Cu2 2.9565(3) . ? Cu2 N4 2.0041(15) 2_656 ? Cu2 S2 2.3251(5) 3_445 ? Cu2 S3 2.3735(5) . ? Cu2 S1 2.4543(5) 2_656 ? S1 C10 1.6692(19) . ? S1 Cu1 2.4068(5) 2_656 ? S1 Cu2 2.4543(5) 2_656 ? S2 C11 1.6615(19) . ? S2 Cu2 2.3251(5) 3 ? S3 C12 1.6691(18) . ? N1 C5 1.341(2) . ? N1 C9 1.349(2) . ? N1 C4 1.488(2) . ? N2 C10 1.159(2) . ? N3 C11 1.153(2) . ? N4 C12 1.155(2) . ? N4 Cu2 2.0041(15) 2_656 ? C1 C2 1.526(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.518(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.521(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.378(3) . ? C5 H5A 0.9500 . ? C6 C7 1.395(2) . ? C6 H6 0.9500 . ? C7 C8 1.392(2) . ? C7 C7 1.483(3) 2_656 ? C8 C9 1.377(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? 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 Cu1 N2 124.40(7) . . ? N3 Cu1 S1 114.32(5) . 2_656 ? N2 Cu1 S1 102.39(5) . 2_656 ? N3 Cu1 S3 106.53(5) . . ? N2 Cu1 S3 102.93(5) . . ? S1 Cu1 S3 104.125(17) 2_656 . ? N3 Cu1 Cu2 124.35(5) . . ? N2 Cu1 Cu2 110.90(5) . . ? S1 Cu1 Cu2 53.275(13) 2_656 . ? S3 Cu1 Cu2 50.850(12) . . ? N4 Cu2 S2 112.38(5) 2_656 3_445 ? N4 Cu2 S3 103.95(5) 2_656 . ? S2 Cu2 S3 122.050(18) 3_445 . ? N4 Cu2 S1 104.60(5) 2_656 2_656 ? S2 Cu2 S1 106.524(17) 3_445 2_656 ? S3 Cu2 S1 105.950(17) . 2_656 ? N4 Cu2 Cu1 114.19(4) 2_656 . ? S2 Cu2 Cu1 132.320(15) 3_445 . ? S3 Cu2 Cu1 54.135(13) . . ? S1 Cu2 Cu1 51.815(12) 2_656 . ? C10 S1 Cu1 97.07(6) . 2_656 ? C10 S1 Cu2 94.69(6) . 2_656 ? Cu1 S1 Cu2 74.911(15) 2_656 2_656 ? C11 S2 Cu2 93.23(6) . 3 ? C12 S3 Cu2 95.39(6) . . ? C12 S3 Cu1 95.48(6) . . ? Cu2 S3 Cu1 75.014(15) . . ? C5 N1 C9 120.64(16) . . ? C5 N1 C4 120.55(15) . . ? C9 N1 C4 118.73(15) . . ? C10 N2 Cu1 153.43(14) . . ? C11 N3 Cu1 166.11(15) . . ? C12 N4 Cu2 150.70(14) . 2_656 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 112.18(18) . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C2 C3 C4 111.08(16) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N1 C4 C3 110.90(15) . . ? N1 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? N1 C5 C6 121.05(16) . . ? N1 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C7 119.70(17) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 117.90(16) . . ? C8 C7 C7 121.33(19) . 2_656 ? C6 C7 C7 120.8(2) . 2_656 ? C9 C8 C7 120.23(16) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? N1 C9 C8 120.42(17) . . ? N1 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N2 C10 S1 177.87(17) . . ? N3 C11 S2 178.95(18) . . ? N4 C12 S3 178.26(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 Cu2 N4 -173.64(7) . . . 2_656 ? N2 Cu1 Cu2 N4 -0.19(7) . . . 2_656 ? S1 Cu1 Cu2 N4 89.90(5) 2_656 . . 2_656 ? S3 Cu1 Cu2 N4 -90.07(5) . . . 2_656 ? N3 Cu1 Cu2 S2 19.57(6) . . . 3_445 ? N2 Cu1 Cu2 S2 -166.98(5) . . . 3_445 ? S1 Cu1 Cu2 S2 -76.89(2) 2_656 . . 3_445 ? S3 Cu1 Cu2 S2 103.14(2) . . . 3_445 ? N3 Cu1 Cu2 S3 -83.57(6) . . . . ? N2 Cu1 Cu2 S3 89.88(5) . . . . ? S1 Cu1 Cu2 S3 179.97(2) 2_656 . . . ? N3 Cu1 Cu2 S1 96.46(6) . . . 2_656 ? N2 Cu1 Cu2 S1 -90.09(5) . . . 2_656 ? S3 Cu1 Cu2 S1 -179.97(2) . . . 2_656 ? N4 Cu2 S3 C12 15.73(8) 2_656 . . . ? S2 Cu2 S3 C12 143.92(6) 3_445 . . . ? S1 Cu2 S3 C12 -94.22(6) 2_656 . . . ? Cu1 Cu2 S3 C12 -94.24(6) . . . . ? N4 Cu2 S3 Cu1 109.97(5) 2_656 . . . ? S2 Cu2 S3 Cu1 -121.840(19) 3_445 . . . ? S1 Cu2 S3 Cu1 0.025(16) 2_656 . . . ? N3 Cu1 S3 C12 -144.72(8) . . . . ? N2 Cu1 S3 C12 -12.44(8) . . . . ? S1 Cu1 S3 C12 94.10(6) 2_656 . . . ? Cu2 Cu1 S3 C12 94.13(6) . . . . ? N3 Cu1 S3 Cu2 121.16(5) . . . . ? N2 Cu1 S3 Cu2 -106.57(5) . . . . ? S1 Cu1 S3 Cu2 -0.025(16) 2_656 . . . ? N3 Cu1 N2 C10 178.8(3) . . . . ? S1 Cu1 N2 C10 -49.8(3) 2_656 . . . ? S3 Cu1 N2 C10 58.1(3) . . . . ? Cu2 Cu1 N2 C10 5.4(3) . . . . ? N2 Cu1 N3 C11 -0.6(7) . . . . ? S1 Cu1 N3 C11 -127.1(6) 2_656 . . . ? S3 Cu1 N3 C11 118.5(6) . . . . ? Cu2 Cu1 N3 C11 172.0(6) . . . . ? C1 C2 C3 C4 174.08(18) . . . . ? C5 N1 C4 C3 -106.97(18) . . . . ? C9 N1 C4 C3 69.7(2) . . . . ? C2 C3 C4 N1 -171.45(16) . . . . ? C9 N1 C5 C6 -2.0(3) . . . . ? C4 N1 C5 C6 174.58(17) . . . . ? N1 C5 C6 C7 0.9(3) . . . . ? C5 C6 C7 C8 1.1(3) . . . . ? C5 C6 C7 C7 -178.31(12) . . . 2_656 ? C6 C7 C8 C9 -2.0(3) . . . . ? C7 C7 C8 C9 177.40(13) 2_656 . . . ? C5 N1 C9 C8 1.1(3) . . . . ? C4 N1 C9 C8 -175.58(17) . . . . ? C7 C8 C9 N1 1.0(3) . . . . ? Cu1 N2 C10 S1 -21(5) . . . . ? Cu1 S1 C10 N2 53(5) 2_656 . . . ? Cu2 S1 C10 N2 -22(5) 2_656 . . . ? Cu1 N3 C11 S2 43(11) . . . . ? Cu2 S2 C11 N3 -49(10) 3 . . . ? Cu2 N4 C12 S3 -30(6) 2_656 . . . ? Cu2 S3 C12 N4 64(5) . . . . ? Cu1 S3 C12 N4 -11(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.518 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.072