# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author ; Prof. Mike Ward Department of Chemistry University of Sheffield SHEFFIELD S3 7HF ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_contact_letter ; This CIF contains details of the three crystal structure in the paper ?A triple helix of double helicates...' by A. Stephenson and M. D. Ward, submitted to Chem. Comm. for publication. ; _publ_contact_author_name 'Prof. Mike Ward' loop_ _publ_author_name 'Andrew Stephenson' 'Mike Ward' #======================================================== data_imw1687p63 _database_code_depnum_ccdc_archive 'CCDC 862638' #TrackingRef '- helix_of_helicates.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 3(C62H48Ag2N12O2),6(ClO4),3(CH3NO2) _chemical_formula_sum 'C63 H51 Ag2 Cl2 N13 O12' _chemical_formula_weight 1468.81 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' Ag Ag -0.8971 1.1015 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6322 _symmetry_space_group_name_Hall 'P 6c 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-y, -x, -z+1/2' 'x-y, -y, -z' 'x, x-y, -z+1/2' 'y, x, -z' '-x+y, y, -z+1/2' '-x, -x+y, -z' _cell_length_a 21.5080(7) _cell_length_b 21.5080(7) _cell_length_c 25.7514(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10316.5(7) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9205 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.64 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8530 _exptl_absorpt_correction_T_max 0.9256 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 118981 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4963 _reflns_number_gt 4578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. It is a polymeric structure composed of [Ag2(C31H24N6O)2] units which are connected together via Ag...Ag interactions. There are also two [ClO4]- anions and one nitromethane per Ag2 complex. The space group was confirmed by Platon. All hydrogens were added in calculated positions. The structure was inverted to bring the Flack parameter close to 0. The structure grows such that three of the Ag2 complexes are present in the Unit cell. Two of the [ClO4]- anions grow such that they have S6 symmetry and each oxygen is disordered over two positions. All atoms have therefore been made half occupancy Although some alerts in the cif check suggest close O - O contacts these are not real. The structure contained solvent accessible voids and therefore the Platon Squeeze program was employed: loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.333 0.667 0.750 355 134 ' ' 2 0.333 0.667 0.250 80 52 ' ' 3 0.667 0.333 0.250 355 134 ' ' 4 0.666 0.333 0.750 80 52 ' ' _platon_squeeze_details All 6 and 5 membered rings were fixed using geometric restraints as were the anions and nitromethane solvent molecule. Global displacement restraints have been used to achieve a consistent model. The crystals were relatively weakly diffracting and the data was cut at an appropriate point. 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^)+(0.1233P)^2^+72.6720P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(10) _refine_ls_number_reflns 4963 _refine_ls_number_parameters 383 _refine_ls_number_restraints 479 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0946 _refine_ls_wR_factor_ref 0.2603 _refine_ls_wR_factor_gt 0.2553 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.097 _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 Ag1 Ag 0.68358(6) 0.95557(7) 0.54841(5) 0.0718(4) Uani 1 1 d . . . N11 N 0.6803(4) 1.0479(4) 0.5846(3) 0.061(2) Uani 1 1 d GU . . C12 C 0.7245(4) 1.0806(5) 0.6272(3) 0.065(3) Uani 1 1 d GU . . C13 C 0.7225(5) 1.1366(5) 0.6526(3) 0.088(4) Uani 1 1 d GU . . H13 H 0.7520 1.1586 0.6810 0.105 Uiso 1 1 calc R . . C14 C 0.6762(6) 1.1598(5) 0.6354(4) 0.094(4) Uani 1 1 d GU . . H14 H 0.6748 1.1973 0.6523 0.113 Uiso 1 1 calc R . . C15 C 0.6320(5) 1.1271(5) 0.5928(4) 0.087(4) Uani 1 1 d GU . . H15 H 0.6011 1.1426 0.5813 0.104 Uiso 1 1 calc R . . C16 C 0.6341(4) 1.0711(5) 0.5674(3) 0.065(3) Uani 1 1 d GU . . H16 H 0.6045 1.0491 0.5389 0.078 Uiso 1 1 calc R . . N21 N 0.8190(4) 0.9843(4) 0.6406(3) 0.059(2) Uani 1 1 d GU . . N22 N 0.7634(3) 0.9946(4) 0.6204(3) 0.057(2) Uani 1 1 d GU . . C23 C 0.7716(4) 1.0591(4) 0.6418(3) 0.064(3) Uani 1 1 d GU . . C24 C 0.8322(5) 1.0887(4) 0.6751(4) 0.083(4) Uani 1 1 d GU . . H24 H 0.8497 1.1310 0.6941 0.100 Uiso 1 1 calc R . . C25 C 0.8615(4) 1.0424(5) 0.6744(3) 0.079(4) Uani 1 1 d GU . . H25 H 0.9016 1.0491 0.6929 0.094 Uiso 1 1 calc R . . C26 C 0.8249(6) 0.9250(7) 0.6271(5) 0.061(3) Uani 1 1 d U . . H26A H 0.8716 0.9334 0.6380 0.073 Uiso 1 1 calc R . . H26B H 0.8226 0.9204 0.5896 0.073 Uiso 1 1 calc R . . N31 N 0.7080(5) 0.8242(4) 1.0062(3) 0.070(3) Uani 1 1 d GU . . C32 C 0.6485(4) 0.8321(5) 1.0150(4) 0.086(3) Uani 1 1 d GU . . C33 C 0.6557(6) 0.8902(7) 1.0436(5) 0.123(5) Uani 1 1 d GU . . H33 H 0.6160 0.8955 1.0495 0.148 Uiso 1 1 calc R . . C34 C 0.7224(7) 0.9403(6) 1.0634(5) 0.132(5) Uani 1 1 d GU . . H34 H 0.7272 0.9792 1.0825 0.158 Uiso 1 1 calc R . . C35 C 0.7818(5) 0.9325(5) 1.0546(5) 0.111(4) Uani 1 1 d GU . . H35 H 0.8264 0.9660 1.0678 0.133 Uiso 1 1 calc R . . C36 C 0.7746(4) 0.8744(5) 1.0260(4) 0.074(3) Uani 1 1 d GU . . H36 H 0.8144 0.8691 1.0200 0.088 Uiso 1 1 calc R . . N41 N 0.5065(5) 0.6838(6) 0.9504(4) 0.119(4) Uani 1 1 d GDU . . N42 N 0.5786(4) 0.7260(6) 0.9674(4) 0.093(4) Uani 1 1 d GU . . C43 C 0.5855(5) 0.7878(6) 0.9927(4) 0.096(4) Uani 1 1 d GU . . C44 C 0.5176(6) 0.7838(7) 0.9913(5) 0.111(4) Uani 1 1 d GU . . H44 H 0.5070 0.8174 1.0051 0.133 Uiso 1 1 calc R . . C45 C 0.4688(4) 0.7196(8) 0.9651(5) 0.124(5) Uani 1 1 d GU . . H45 H 0.4205 0.7037 0.9588 0.149 Uiso 1 1 calc R . . C46 C 0.4825(9) 0.6225(9) 0.9218(7) 0.123(5) Uani 1 1 d DU . . H46A H 0.4317 0.6022 0.9148 0.148 Uiso 1 1 calc R . . H46B H 0.4886 0.5876 0.9417 0.148 Uiso 1 1 calc R . . C51 C 0.6608(2) 0.7282(3) 0.69656(18) 0.064(3) Uani 1 1 d GU . . C52 C 0.7237(2) 0.7726(3) 0.7235(2) 0.072(3) Uani 1 1 d GU . . H52 H 0.7303 0.7603 0.7569 0.086 Uiso 1 1 calc R . . C53 C 0.7768(3) 0.8355(3) 0.7007(2) 0.071(3) Uani 1 1 d GU . . H53 H 0.8188 0.8652 0.7187 0.086 Uiso 1 1 calc R . . C54 C 0.7669(3) 0.8539(3) 0.6508(2) 0.061(3) Uani 1 1 d GU . . C55 C 0.7041(3) 0.8094(4) 0.6239(2) 0.070(3) Uani 1 1 d GU . . H55 H 0.6975 0.8217 0.5905 0.084 Uiso 1 1 calc R . . C56 C 0.6510(3) 0.7466(4) 0.64672(17) 0.067(3) Uani 1 1 d GU . . H56 H 0.6089 0.7169 0.6287 0.080 Uiso 1 1 calc R . . C61 C 0.5806(2) 0.6536(3) 0.7730(2) 0.074(3) Uani 1 1 d GU . . C62 C 0.5845(3) 0.7122(3) 0.79884(19) 0.079(3) Uani 1 1 d GU . . H62 H 0.6067 0.7571 0.7831 0.094 Uiso 1 1 calc R . . C63 C 0.5552(4) 0.7035(4) 0.8482(2) 0.087(4) Uani 1 1 d GU . . H63 H 0.5578 0.7427 0.8655 0.105 Uiso 1 1 calc R . . C64 C 0.5220(3) 0.6364(5) 0.8717(2) 0.102(4) Uani 1 1 d GU . . C65 C 0.5181(3) 0.5778(4) 0.8458(3) 0.096(4) Uani 1 1 d GU . . H65 H 0.4959 0.5329 0.8616 0.116 Uiso 1 1 calc R . . C66 C 0.5474(3) 0.5864(3) 0.7965(3) 0.089(4) Uani 1 1 d GU . . H66 H 0.5448 0.5472 0.7792 0.107 Uiso 1 1 calc R . . C71 C 0.6028(8) 0.6546(8) 0.7189(6) 0.072(3) Uani 1 1 d U . . O72 O 0.5731(6) 0.6036(6) 0.6904(5) 0.100(4) Uani 1 1 d . . . Cl11 Cl 0.0000 1.0000 0.7500 0.0383(13) Uani 1 6 d SDU . . O12 O 0.0000 1.0000 0.6918(6) 0.051(5) Uani 0.50 3 d SPDU . . O13 O 0.0098(8) 0.9411(6) 0.7647(6) 0.050(3) Uani 0.50 1 d PDU . . Cl21 Cl 0.56612(19) 1.0000 1.0000 0.0816(16) Uani 1 2 d SDU . . O22 O 0.5044(8) 0.9346(5) 1.0173(7) 0.225(10) Uani 1 1 d DU . . O23 O 0.5971(7) 0.9819(7) 0.9572(5) 0.144(6) Uani 1 1 d DU . . Cl31 Cl 0.6667 0.3333 0.5872(3) 0.043(2) Uani 0.50 3 d SPDU . . O32 O 0.6608(8) 0.3931(5) 0.6063(3) 0.056(4) Uani 0.50 1 d PDU . . O33 O 0.6667 0.3333 0.5312(3) 0.084(8) Uani 0.50 3 d SPDU . . Cl41 Cl 0.0000 1.0000 0.5000 0.101(4) Uani 1 6 d SDU . . O42 O 0.0000 1.0000 0.55590(8) 0.124(8) Uani 0.50 3 d SPDU . . O43 O -0.0180(12) 0.9313(6) 0.4785(9) 0.123(7) Uani 0.50 1 d PDU . . C1S C 0.7287(14) 0.6097(13) 0.7082(11) 0.115(6) Uani 0.50 1 d PDU . . H1S1 H 0.7069 0.6330 0.7263 0.173 Uiso 0.50 1 calc PR . . H1S2 H 0.7561 0.6390 0.6794 0.173 Uiso 0.50 1 calc PR . . H1S3 H 0.7599 0.6032 0.7314 0.173 Uiso 0.50 1 calc PR . . N2S N 0.6726(11) 0.5395(11) 0.6890(8) 0.121(6) Uani 0.50 1 d PDU . . O3S O 0.6353(14) 0.4940(12) 0.7206(8) 0.126(6) Uani 0.50 1 d PDU . . O4S O 0.6629(15) 0.5331(14) 0.6415(7) 0.125(6) Uani 0.50 1 d PDU . . 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 Ag1 0.0626(6) 0.1041(9) 0.0684(6) -0.0198(7) -0.0131(5) 0.0566(6) N11 0.037(5) 0.079(6) 0.061(5) -0.004(5) 0.000(4) 0.024(4) C12 0.059(6) 0.068(6) 0.068(6) 0.005(5) -0.009(5) 0.031(5) C13 0.082(8) 0.085(8) 0.103(9) -0.015(7) -0.021(7) 0.048(6) C14 0.099(8) 0.084(8) 0.115(9) -0.022(7) -0.031(7) 0.057(7) C15 0.079(8) 0.089(8) 0.104(9) -0.017(7) -0.024(7) 0.051(6) C16 0.056(6) 0.080(7) 0.074(7) 0.010(6) 0.005(5) 0.046(6) N21 0.027(4) 0.071(5) 0.078(6) 0.024(4) 0.006(4) 0.024(4) N22 0.033(4) 0.074(6) 0.065(5) 0.022(5) 0.009(4) 0.028(4) C23 0.040(5) 0.068(6) 0.071(6) 0.021(5) 0.000(5) 0.016(5) C24 0.060(7) 0.064(7) 0.094(8) 0.024(6) -0.027(6) 0.007(6) C25 0.052(6) 0.064(7) 0.087(7) 0.028(6) -0.011(6) 0.005(5) C26 0.035(5) 0.088(7) 0.075(7) 0.019(6) 0.007(5) 0.043(5) N31 0.079(6) 0.064(6) 0.070(6) 0.015(5) -0.001(5) 0.038(5) C32 0.093(7) 0.087(7) 0.100(8) 0.016(6) 0.001(6) 0.062(6) C33 0.117(9) 0.114(9) 0.168(11) -0.023(8) -0.019(9) 0.080(7) C34 0.128(10) 0.100(9) 0.181(12) -0.039(9) -0.024(10) 0.067(8) C35 0.108(9) 0.077(8) 0.147(10) -0.027(8) -0.034(9) 0.044(7) C36 0.087(7) 0.062(6) 0.081(7) -0.002(6) -0.017(6) 0.044(6) N41 0.048(5) 0.146(9) 0.105(7) 0.019(7) 0.025(6) 0.004(6) N42 0.058(6) 0.110(8) 0.081(7) 0.036(6) 0.021(5) 0.019(6) C43 0.068(6) 0.114(8) 0.097(8) 0.033(6) 0.025(6) 0.040(6) C44 0.068(7) 0.137(10) 0.123(10) 0.030(8) 0.027(8) 0.049(7) C45 0.063(7) 0.152(11) 0.115(10) 0.030(9) 0.022(8) 0.022(7) C46 0.056(8) 0.133(10) 0.095(8) 0.014(7) -0.006(7) -0.016(8) C51 0.055(5) 0.065(6) 0.077(6) 0.006(5) 0.000(5) 0.033(5) C52 0.059(6) 0.064(7) 0.073(7) 0.019(6) -0.013(6) 0.016(5) C53 0.068(7) 0.060(6) 0.075(7) 0.013(5) -0.006(6) 0.023(6) C54 0.052(5) 0.077(6) 0.066(6) 0.015(5) 0.003(5) 0.041(5) C55 0.047(6) 0.099(8) 0.063(7) 0.014(6) 0.004(5) 0.037(5) C56 0.053(6) 0.085(7) 0.070(6) 0.002(6) 0.008(5) 0.040(5) C61 0.055(6) 0.069(6) 0.082(6) 0.018(5) -0.012(5) 0.020(5) C62 0.072(7) 0.084(7) 0.073(7) 0.015(6) -0.016(6) 0.034(6) C63 0.073(8) 0.097(8) 0.072(7) 0.021(6) -0.020(6) 0.027(7) C64 0.051(6) 0.106(8) 0.084(7) 0.020(6) -0.023(6) -0.009(7) C65 0.041(6) 0.097(8) 0.089(7) 0.026(7) -0.028(6) -0.012(6) C66 0.048(7) 0.078(7) 0.090(7) 0.022(6) -0.018(6) -0.008(6) C71 0.061(7) 0.062(6) 0.087(7) 0.006(6) 0.002(6) 0.026(5) O72 0.085(8) 0.058(6) 0.109(8) -0.008(6) -0.011(7) -0.001(6) Cl11 0.0215(16) 0.0215(16) 0.072(4) 0.000 0.000 0.0108(8) O12 0.039(6) 0.039(6) 0.075(9) 0.000 0.000 0.020(3) O13 0.049(7) 0.018(6) 0.080(9) 0.019(6) 0.003(6) 0.015(5) Cl21 0.0544(17) 0.132(5) 0.084(3) -0.032(3) -0.0161(16) 0.066(2) O22 0.093(10) 0.259(17) 0.189(16) -0.069(14) 0.051(10) -0.012(11) O23 0.115(10) 0.146(12) 0.134(10) -0.044(9) 0.043(8) 0.037(9) Cl31 0.038(3) 0.038(3) 0.052(5) 0.000 0.000 0.0190(14) O32 0.041(8) 0.025(7) 0.103(11) -0.011(7) 0.004(8) 0.018(6) O33 0.095(12) 0.095(12) 0.060(11) 0.000 0.000 0.048(6) Cl41 0.049(3) 0.049(3) 0.205(13) 0.000 0.000 0.0246(13) O42 0.082(8) 0.082(8) 0.208(16) 0.000 0.000 0.041(4) O43 0.084(11) 0.064(9) 0.226(18) -0.016(10) -0.003(11) 0.042(8) C1S 0.150(14) 0.134(13) 0.115(11) -0.007(10) 0.032(11) 0.111(12) N2S 0.154(14) 0.137(13) 0.117(11) -0.007(10) 0.032(11) 0.106(12) O3S 0.158(14) 0.139(13) 0.119(11) -0.005(10) 0.031(11) 0.103(12) O4S 0.157(14) 0.139(13) 0.118(11) -0.008(10) 0.032(11) 0.103(12) _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 Ag1 N11 2.226(6) . ? Ag1 N42 2.27(9) 9_566 ? Ag1 N31 2.334(7) 9_566 ? Ag1 N22 2.376(6) . ? Ag1 Ag1 2.993(3) 8_676 ? N11 C12 1.3900 . ? N11 C16 1.3900 . ? C12 C23 1.358(8) . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? N21 C26 1.387(14) . ? N21 N22 1.4200 . ? N21 C25 1.4200 . ? N22 C23 1.4200 . ? C23 C24 1.4200 . ? C24 C25 1.4200 . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C54 1.536(13) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? N31 C32 1.3900 . ? N31 C36 1.3900 . ? N31 Ag1 2.334(7) 9_566 ? C32 C43 1.335(12) . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N41 C46 1.367(16) . ? N41 N42 1.4200 . ? N41 C45 1.4200 . ? N42 C43 1.4200 . ? N42 Ag1 2.273(8) 9_566 ? C43 C44 1.4200 . ? C44 C45 1.4200 . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C64 1.489(18) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C51 C71 1.556(15) . ? C52 C53 1.3900 . ? C52 H52 0.9300 . ? C53 C54 1.3900 . ? C53 H53 0.9300 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C62 1.3897 . ? C61 C66 1.3903 . ? C61 C71 1.468(16) . ? C62 C63 1.3902 . ? C62 H62 0.9300 . ? C63 C64 1.3900 . ? C63 H63 0.9300 . ? C64 C65 1.3902 . ? C65 C66 1.3897 . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 O72 1.204(18) . ? Cl11 O13 1.435(10) . ? Cl11 O13 1.435(10) 11_456 ? Cl11 O13 1.435(11) 3_675 ? Cl11 O13 1.435(10) 9_576 ? Cl11 O13 1.435(10) 5_465 ? Cl11 O13 1.435(10) 7_666 ? Cl11 O12 1.500(15) . ? Cl11 O12 1.500(15) 7_666 ? O12 O13 1.781(18) 9_576 ? O12 O13 1.781(18) 7_666 ? O12 O13 1.781(18) 11_456 ? O13 O13 1.30(3) 7_666 ? O13 O12 1.781(18) 7_666 ? Cl21 O23 1.439(2) . ? Cl21 O23 1.439(2) 8_677 ? Cl21 O22 1.440(2) . ? Cl21 O22 1.440(2) 8_677 ? Cl31 O32 1.440(2) 5_665 ? Cl31 O33 1.440(2) . ? Cl31 O32 1.440(2) 3_655 ? Cl31 O32 1.440(2) . ? Cl41 O43 1.439(2) . ? Cl41 O43 1.439(2) 8_676 ? Cl41 O43 1.439(2) 3_675 ? Cl41 O43 1.439(2) 5_465 ? Cl41 O43 1.439(2) 10_466 ? Cl41 O43 1.439(2) 12_556 ? Cl41 O42 1.439(2) . ? Cl41 O42 1.439(2) 8_676 ? O42 O43 1.60(2) 10_466 ? O42 O43 1.60(2) 12_556 ? O42 O43 1.60(2) 8_676 ? O43 O43 1.30(4) 12_556 ? O43 O42 1.60(2) 8_676 ? C1S N2S 1.469(2) . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? N2S O3S 1.216(13) . ? N2S O4S 1.237(13) . ? 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 N11 Ag1 N42 119(2) . 9_566 ? N11 Ag1 N31 163.8(3) . 9_566 ? N42 Ag1 N31 72(2) 9_566 9_566 ? N11 Ag1 N22 72.4(3) . . ? N42 Ag1 N22 132.4(7) 9_566 . ? N31 Ag1 N22 110.0(3) 9_566 . ? N11 Ag1 Ag1 85.5(2) . 8_676 ? N42 Ag1 Ag1 108.5(5) 9_566 8_676 ? N31 Ag1 Ag1 79.4(2) 9_566 8_676 ? N22 Ag1 Ag1 118.74(19) . 8_676 ? C12 N11 C16 120.0 . . ? C12 N11 Ag1 117.7(4) . . ? C16 N11 Ag1 122.3(4) . . ? C23 C12 C13 121.1(6) . . ? C23 C12 N11 118.8(6) . . ? C13 C12 N11 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 N11 120.0 . . ? C15 C16 H16 120.0 . . ? N11 C16 H16 120.0 . . ? C26 N21 N22 121.6(7) . . ? C26 N21 C25 130.4(7) . . ? N22 N21 C25 108.0 . . ? N21 N22 C23 108.0 . . ? N21 N22 Ag1 138.3(4) . . ? C23 N22 Ag1 111.2(4) . . ? C12 C23 C24 133.5(7) . . ? C12 C23 N22 118.5(7) . . ? C24 C23 N22 108.0 . . ? C25 C24 C23 108.0 . . ? C25 C24 H24 126.0 . . ? C23 C24 H24 126.0 . . ? C24 C25 N21 108.0 . . ? C24 C25 H25 126.0 . . ? N21 C25 H25 126.0 . . ? N21 C26 C54 114.5(9) . . ? N21 C26 H26A 108.6 . . ? C54 C26 H26A 108.6 . . ? N21 C26 H26B 108.6 . . ? C54 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C32 N31 C36 120.0 . . ? C32 N31 Ag1 113.2(5) . 9_566 ? C36 N31 Ag1 126.6(5) . 9_566 ? C43 C32 C33 119.1(9) . . ? C43 C32 N31 120.6(9) . . ? C33 C32 N31 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 N31 120.0 . . ? C35 C36 H36 120.0 . . ? N31 C36 H36 120.0 . . ? C46 N41 N42 123.1(12) . . ? C46 N41 C45 128.7(12) . . ? N42 N41 C45 108.0 . . ? N41 N42 C43 108.0 . . ? N41 N42 Ag1 135.6(6) . 9_566 ? C43 N42 Ag1 115.2(6) . 9_566 ? C32 C43 C44 134.4(10) . . ? C32 C43 N42 117.4(10) . . ? C44 C43 N42 108.0 . . ? C43 C44 C45 108.0 . . ? C43 C44 H44 126.0 . . ? C45 C44 H44 126.0 . . ? N41 C45 C44 108.0 . . ? N41 C45 H45 126.0 . . ? C44 C45 H45 126.0 . . ? N41 C46 C64 111.8(12) . . ? N41 C46 H46A 109.3 . . ? C64 C46 H46A 109.3 . . ? N41 C46 H46B 109.3 . . ? C64 C46 H46B 109.3 . . ? H46A C46 H46B 107.9 . . ? C52 C51 C56 120.0 . . ? C52 C51 C71 121.6(6) . . ? C56 C51 C71 118.2(6) . . ? C51 C52 C53 120.0 . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 C26 120.8(6) . . ? C53 C54 C26 119.1(6) . . ? C54 C55 C56 120.0 . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 C71 124.7(6) . . ? C66 C61 C71 115.0(6) . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 C46 122.0(9) . . ? C65 C64 C46 117.6(9) . . ? C66 C65 C64 120.0 . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? O72 C71 C61 123.1(13) . . ? O72 C71 C51 119.4(13) . . ? C61 C71 C51 117.1(11) . . ? O13 Cl11 O13 80.3(12) . 11_456 ? O13 Cl11 O13 113.3(5) . 3_675 ? O13 Cl11 O13 165.4(12) 11_456 3_675 ? O13 Cl11 O13 165.4(12) . 9_576 ? O13 Cl11 O13 113.3(5) 11_456 9_576 ? O13 Cl11 O13 53.8(12) 3_675 9_576 ? O13 Cl11 O13 113.3(5) . 5_465 ? O13 Cl11 O13 53.8(12) 11_456 5_465 ? O13 Cl11 O13 113.3(5) 3_675 5_465 ? O13 Cl11 O13 80.3(12) 9_576 5_465 ? O13 Cl11 O13 53.9(12) . 7_666 ? O13 Cl11 O13 113.3(5) 11_456 7_666 ? O13 Cl11 O13 80.3(12) 3_675 7_666 ? O13 Cl11 O13 113.3(5) 9_576 7_666 ? O13 Cl11 O13 165.4(12) 5_465 7_666 ? O13 Cl11 O12 105.3(6) . . ? O13 Cl11 O12 74.7(6) 11_456 . ? O13 Cl11 O12 105.3(6) 3_675 . ? O13 Cl11 O12 74.7(6) 9_576 . ? O13 Cl11 O12 105.3(6) 5_465 . ? O13 Cl11 O12 74.7(6) 7_666 . ? O13 Cl11 O12 74.7(6) . 7_666 ? O13 Cl11 O12 105.3(6) 11_456 7_666 ? O13 Cl11 O12 74.7(6) 3_675 7_666 ? O13 Cl11 O12 105.3(6) 9_576 7_666 ? O13 Cl11 O12 74.7(6) 5_465 7_666 ? O13 Cl11 O12 105.3(6) 7_666 7_666 ? O12 Cl11 O12 180.000(13) . 7_666 ? Cl11 O12 O13 51.0(6) . 9_576 ? Cl11 O12 O13 51.0(6) . 7_666 ? O13 O12 O13 84.6(9) 9_576 7_666 ? Cl11 O12 O13 51.0(6) . 11_456 ? O13 O12 O13 84.6(9) 9_576 11_456 ? O13 O12 O13 84.6(9) 7_666 11_456 ? O13 O13 Cl11 63.1(6) 7_666 . ? O13 O13 O12 97.3(11) 7_666 7_666 ? Cl11 O13 O12 54.3(6) . 7_666 ? O23 Cl21 O23 106.4(14) . 8_677 ? O23 Cl21 O22 107.4(2) . . ? O23 Cl21 O22 102.8(11) 8_677 . ? O23 Cl21 O22 102.8(11) . 8_677 ? O23 Cl21 O22 107.4(2) 8_677 8_677 ? O22 Cl21 O22 128.5(18) . 8_677 ? O32 Cl31 O33 110.0(2) 5_665 . ? O32 Cl31 O32 108.9(2) 5_665 3_655 ? O33 Cl31 O32 110.0(2) . 3_655 ? O32 Cl31 O32 108.9(2) 5_665 . ? O33 Cl31 O32 110.0(2) . . ? O32 Cl31 O32 108.9(2) 3_655 . ? O43 Cl41 O43 151.7(18) . 8_676 ? O43 Cl41 O43 106.1(11) . 3_675 ? O43 Cl41 O43 53.5(18) 8_676 3_675 ? O43 Cl41 O43 106.1(11) . 5_465 ? O43 Cl41 O43 99.2(19) 8_676 5_465 ? O43 Cl41 O43 106.1(11) 3_675 5_465 ? O43 Cl41 O43 99.2(19) . 10_466 ? O43 Cl41 O43 106.1(11) 8_676 10_466 ? O43 Cl41 O43 151.7(18) 3_675 10_466 ? O43 Cl41 O43 53.5(18) 5_465 10_466 ? O43 Cl41 O43 53.5(18) . 12_556 ? O43 Cl41 O43 106.1(11) 8_676 12_556 ? O43 Cl41 O43 99.2(19) 3_675 12_556 ? O43 Cl41 O43 151.7(18) 5_465 12_556 ? O43 Cl41 O43 106.1(11) 10_466 12_556 ? O43 Cl41 O42 112.7(10) . . ? O43 Cl41 O42 67.3(10) 8_676 . ? O43 Cl41 O42 112.7(10) 3_675 . ? O43 Cl41 O42 112.7(10) 5_465 . ? O43 Cl41 O42 67.3(10) 10_466 . ? O43 Cl41 O42 67.3(10) 12_556 . ? O43 Cl41 O42 67.3(10) . 8_676 ? O43 Cl41 O42 112.7(10) 8_676 8_676 ? O43 Cl41 O42 67.3(10) 3_675 8_676 ? O43 Cl41 O42 67.3(10) 5_465 8_676 ? O43 Cl41 O42 112.7(10) 10_466 8_676 ? O43 Cl41 O42 112.7(10) 12_556 8_676 ? O42 Cl41 O42 180.000(2) . 8_676 ? Cl41 O42 O43 56.3(5) . 10_466 ? Cl41 O42 O43 56.3(5) . 12_556 ? O43 O42 O43 92.2(7) 10_466 12_556 ? Cl41 O42 O43 56.3(5) . 8_676 ? O43 O42 O43 92.2(7) 10_466 8_676 ? O43 O42 O43 92.2(7) 12_556 8_676 ? O43 O43 Cl41 63.2(9) 12_556 . ? O43 O43 O42 111.5(13) 12_556 8_676 ? Cl41 O43 O42 56.3(5) . 8_676 ? N2S C1S H1S1 109.5 . . ? N2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? N2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O3S N2S O4S 124.4(3) . . ? O3S N2S C1S 118.4(9) . . ? O4S N2S C1S 116.9(9) . . ? 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 N42 Ag1 N11 C12 130.7(8) 9_566 . . . ? N31 Ag1 N11 C12 -99.7(11) 9_566 . . . ? N22 Ag1 N11 C12 1.4(5) . . . . ? Ag1 Ag1 N11 C12 -120.7(5) 8_676 . . . ? N42 Ag1 N11 C16 -46.7(9) 9_566 . . . ? N31 Ag1 N11 C16 83.0(12) 9_566 . . . ? N22 Ag1 N11 C16 -176.0(6) . . . . ? Ag1 Ag1 N11 C16 62.0(5) 8_676 . . . ? C16 N11 C12 C23 -177.0(9) . . . . ? Ag1 N11 C12 C23 5.6(9) . . . . ? C16 N11 C12 C13 0.0 . . . . ? Ag1 N11 C12 C13 -177.4(6) . . . . ? C23 C12 C13 C14 177.0(10) . . . . ? N11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 N11 0.0 . . . . ? C12 N11 C16 C15 0.0 . . . . ? Ag1 N11 C16 C15 177.3(6) . . . . ? C26 N21 N22 C23 179.4(10) . . . . ? C25 N21 N22 C23 0.0 . . . . ? C26 N21 N22 Ag1 -21.1(11) . . . . ? C25 N21 N22 Ag1 159.5(7) . . . . ? N11 Ag1 N22 N21 -166.6(7) . . . . ? N42 Ag1 N22 N21 80(3) 9_566 . . . ? N31 Ag1 N22 N21 -3.5(7) 9_566 . . . ? Ag1 Ag1 N22 N21 -92.1(6) 8_676 . . . ? N11 Ag1 N22 C23 -7.5(4) . . . . ? N42 Ag1 N22 C23 -121(3) 9_566 . . . ? N31 Ag1 N22 C23 155.6(4) 9_566 . . . ? Ag1 Ag1 N22 C23 67.0(4) 8_676 . . . ? C13 C12 C23 C24 -11.5(12) . . . . ? N11 C12 C23 C24 165.5(6) . . . . ? C13 C12 C23 N22 169.8(6) . . . . ? N11 C12 C23 N22 -13.3(11) . . . . ? N21 N22 C23 C12 179.0(9) . . . . ? Ag1 N22 C23 C12 13.5(9) . . . . ? N21 N22 C23 C24 0.0 . . . . ? Ag1 N22 C23 C24 -165.5(5) . . . . ? C12 C23 C24 C25 -178.8(11) . . . . ? N22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 N21 0.0 . . . . ? C26 N21 C25 C24 -179.4(11) . . . . ? N22 N21 C25 C24 0.0 . . . . ? N22 N21 C26 C54 -71.7(12) . . . . ? C25 N21 C26 C54 107.6(10) . . . . ? C36 N31 C32 C43 174.5(12) . . . . ? Ag1 N31 C32 C43 -0.8(11) 9_566 . . . ? C36 N31 C32 C33 0.0 . . . . ? Ag1 N31 C32 C33 -175.3(6) 9_566 . . . ? C43 C32 C33 C34 -174.6(12) . . . . ? N31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 N31 0.0 . . . . ? C32 N31 C36 C35 0.0 . . . . ? Ag1 N31 C36 C35 174.6(7) 9_566 . . . ? C46 N41 N42 C43 176.0(15) . . . . ? C45 N41 N42 C43 0.0 . . . . ? C46 N41 N42 Ag1 9.3(16) . . . 9_566 ? C45 N41 N42 Ag1 -166.7(10) . . . 9_566 ? C33 C32 C43 C44 -1.2(15) . . . . ? N31 C32 C43 C44 -175.8(8) . . . . ? C33 C32 C43 N42 -175.0(7) . . . . ? N31 C32 C43 N42 10.5(14) . . . . ? N41 N42 C43 C32 175.3(12) . . . . ? Ag1 N42 C43 C32 -15.0(11) 9_566 . . . ? N41 N42 C43 C44 0.0 . . . . ? Ag1 N42 C43 C44 169.7(7) 9_566 . . . ? C32 C43 C44 C45 -174.2(15) . . . . ? N42 C43 C44 C45 0.0 . . . . ? C46 N41 C45 C44 -175.7(15) . . . . ? N42 N41 C45 C44 0.0 . . . . ? C43 C44 C45 N41 0.0 . . . . ? N42 N41 C46 C64 -60(2) . . . . ? C45 N41 C46 C64 115.6(14) . . . . ? C56 C51 C52 C53 0.0 . . . . ? C71 C51 C52 C53 175.2(7) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C52 C53 C54 C26 177.6(7) . . . . ? N21 C26 C54 C55 92.9(10) . . . . ? N21 C26 C54 C53 -84.6(9) . . . . ? C53 C54 C55 C56 0.0 . . . . ? C26 C54 C55 C56 -177.5(7) . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? C71 C51 C56 C55 -175.3(7) . . . . ? C66 C61 C62 C63 0.0 . . . . ? C71 C61 C62 C63 173.3(8) . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C62 C63 C64 C46 -172.9(10) . . . . ? N41 C46 C64 C63 -24.7(19) . . . . ? N41 C46 C64 C65 162.3(11) . . . . ? C63 C64 C65 C66 0.0 . . . . ? C46 C64 C65 C66 173.2(10) . . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? C71 C61 C66 C65 -173.9(7) . . . . ? C62 C61 C71 O72 -146.1(13) . . . . ? C66 C61 C71 O72 27.5(17) . . . . ? C62 C61 C71 C51 26.0(14) . . . . ? C66 C61 C71 C51 -160.4(7) . . . . ? C52 C51 C71 O72 -139.5(12) . . . . ? C56 C51 C71 O72 35.8(16) . . . . ? C52 C51 C71 C61 48.2(13) . . . . ? C56 C51 C71 C61 -136.6(8) . . . . ? O13 Cl11 O12 O13 -164.8(12) . . . 9_576 ? O13 Cl11 O12 O13 120.000(6) 11_456 . . 9_576 ? O13 Cl11 O12 O13 -44.8(12) 3_675 . . 9_576 ? O13 Cl11 O12 O13 75.2(12) 5_465 . . 9_576 ? O13 Cl11 O12 O13 -120.000(5) 7_666 . . 9_576 ? O12 Cl11 O12 O13 -22(100) 7_666 . . 9_576 ? O13 Cl11 O12 O13 -44.8(12) . . . 7_666 ? O13 Cl11 O12 O13 -120.000(10) 11_456 . . 7_666 ? O13 Cl11 O12 O13 75.2(12) 3_675 . . 7_666 ? O13 Cl11 O12 O13 120.000(10) 9_576 . . 7_666 ? O13 Cl11 O12 O13 -164.8(12) 5_465 . . 7_666 ? O12 Cl11 O12 O13 98(100) 7_666 . . 7_666 ? O13 Cl11 O12 O13 75.2(12) . . . 11_456 ? O13 Cl11 O12 O13 -164.8(12) 3_675 . . 11_456 ? O13 Cl11 O12 O13 -120.000(1) 9_576 . . 11_456 ? O13 Cl11 O12 O13 -44.8(12) 5_465 . . 11_456 ? O13 Cl11 O12 O13 120.000(2) 7_666 . . 11_456 ? O12 Cl11 O12 O13 -142(100) 7_666 . . 11_456 ? O13 Cl11 O13 O13 128.4(17) 11_456 . . 7_666 ? O13 Cl11 O13 O13 -57(2) 3_675 . . 7_666 ? O13 Cl11 O13 O13 -30.6(11) 9_576 . . 7_666 ? O13 Cl11 O13 O13 172.0(8) 5_465 . . 7_666 ? O12 Cl11 O13 O13 57.4(13) . . . 7_666 ? O12 Cl11 O13 O13 -122.6(13) 7_666 . . 7_666 ? O13 Cl11 O13 O12 -108.9(8) 11_456 . . 7_666 ? O13 Cl11 O13 O12 65.4(8) 3_675 . . 7_666 ? O13 Cl11 O13 O12 92.00(19) 9_576 . . 7_666 ? O13 Cl11 O13 O12 -65.4(8) 5_465 . . 7_666 ? O13 Cl11 O13 O12 122.6(13) 7_666 . . 7_666 ? O12 Cl11 O13 O12 180.000(13) . . . 7_666 ? O43 Cl41 O42 O43 -91(2) . . . 10_466 ? O43 Cl41 O42 O43 120.000(2) 8_676 . . 10_466 ? O43 Cl41 O42 O43 149(2) 3_675 . . 10_466 ? O43 Cl41 O42 O43 29(2) 5_465 . . 10_466 ? O43 Cl41 O42 O43 -120.000(2) 12_556 . . 10_466 ? O42 Cl41 O42 O43 78(100) 8_676 . . 10_466 ? O43 Cl41 O42 O43 29(2) . . . 12_556 ? O43 Cl41 O42 O43 -120.000(14) 8_676 . . 12_556 ? O43 Cl41 O42 O43 -91(2) 3_675 . . 12_556 ? O43 Cl41 O42 O43 149(2) 5_465 . . 12_556 ? O43 Cl41 O42 O43 120.000(13) 10_466 . . 12_556 ? O42 Cl41 O42 O43 -162(100) 8_676 . . 12_556 ? O43 Cl41 O42 O43 149(2) . . . 8_676 ? O43 Cl41 O42 O43 29(2) 3_675 . . 8_676 ? O43 Cl41 O42 O43 -91(2) 5_465 . . 8_676 ? O43 Cl41 O42 O43 -120.000(7) 10_466 . . 8_676 ? O43 Cl41 O42 O43 120.000(5) 12_556 . . 8_676 ? O42 Cl41 O42 O43 -42(100) 8_676 . . 8_676 ? O43 Cl41 O43 O43 49.8(18) 8_676 . . 12_556 ? O43 Cl41 O43 O43 90(3) 3_675 . . 12_556 ? O43 Cl41 O43 O43 -157.8(19) 5_465 . . 12_556 ? O43 Cl41 O43 O43 -103(2) 10_466 . . 12_556 ? O42 Cl41 O43 O43 -34(2) . . . 12_556 ? O42 Cl41 O43 O43 146(2) 8_676 . . 12_556 ? O43 Cl41 O43 O42 -96.1(5) 8_676 . . 8_676 ? O43 Cl41 O43 O42 -56.3(11) 3_675 . . 8_676 ? O43 Cl41 O43 O42 56.3(11) 5_465 . . 8_676 ? O43 Cl41 O43 O42 110.8(9) 10_466 . . 8_676 ? O43 Cl41 O43 O42 -146(2) 12_556 . . 8_676 ? O42 Cl41 O43 O42 180.000(13) . . . 8_676 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.963 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.150 #===END data_imw1616p63 _database_code_depnum_ccdc_archive 'CCDC 862639' #TrackingRef '- helix_of_helicates.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C62 H48 Ag2 N12 O2),3(C H3 N O2),6(B F4),H2O' _chemical_formula_sum 'C63 H51.667 Ag2 B2 F8 N13 O4.333' _chemical_formula_weight 1449.53 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P6(3) ' _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' _cell_length_a 21.2675(6) _cell_length_b 21.2675(6) _cell_length_c 25.9142(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10150.8(6) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9981 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 21.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4388 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8800 _exptl_absorpt_correction_T_max 0.9433 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 154617 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.64 _reflns_number_total 15618 _reflns_number_gt 12188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. It is a polymeric structure composed of [Ag2(C31H24N6O)2] units which are connected together via Ag...Ag interactions. There are also two [BF4]- anions, one nitromethane and a third of a water molecule per Ag2 complex. The space group was confirmed by Platon. All hydrogens were added in calculated positions. The structure was inverted to bring the Flack parameter close to 0. The structure grows such that three of the Ag2 complexes are present in the unit cell. Only 5 of the expected 6 [BF4]- anions were located, the other was too disordered and could not be modelled. Also the protons on the water molecule were not located and so were omitted from the refinement. These have both caused a difference between expected and reported formulae which is found in the cif check. The structure contained solvent accessible voids and therefore the Platon Squeeze program was emoployed: loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.253 101 35 ' ' 2 0.000 0.000 0.753 101 35 ' ' 3 0.333 0.667 0.920 456 194 ' ' 4 0.333 0.667 0.515 319 93 ' ' 5 0.667 0.333 0.420 456 195 ' ' 6 0.667 0.333 0.015 319 93 ' ' _platon_squeeze_details All 6 and 5 membered rings were fixed using geometric restraints as were the anions and nitromethane solvent molecule. Global displacement restraints have been used to achieve a consistent model. HFIX 33 was employed for the methyl group on the nitromethane as with HFIX 137 the protons would not reach convergence. The crystals were generally weakly diffracting and with the voids present in the structure this was the best final r-factor that could be achieved. Refinement of F^2^ was 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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(5) _refine_ls_number_reflns 15618 _refine_ls_number_parameters 674 _refine_ls_number_restraints 815 _refine_ls_R_factor_all 0.1342 _refine_ls_R_factor_gt 0.1200 _refine_ls_wR_factor_ref 0.3673 _refine_ls_wR_factor_gt 0.3588 _refine_ls_goodness_of_fit_ref 1.481 _refine_ls_restrained_S_all 1.471 _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 Ag1 Ag 1.30902(5) 1.03173(5) 0.20227(4) 0.0582(3) Uani 1 1 d . . . Ag2 Ag 1.31889(5) 1.26397(4) -0.20031(4) 0.0576(3) Uani 1 1 d . . . N111 N 1.3129(3) 0.9354(3) 0.1676(3) 0.053(2) Uani 1 1 d GU . . C112 C 1.2741(4) 0.9063(4) 0.1222(3) 0.057(2) Uani 1 1 d GU . . C113 C 1.2808(5) 0.8530(4) 0.0959(3) 0.071(3) Uani 1 1 d GU . . H113 H 1.2549 0.8335 0.0655 0.085 Uiso 1 1 calc R . . C114 C 1.3261(5) 0.8288(4) 0.1148(3) 0.076(3) Uani 1 1 d GU . . H114 H 1.3305 0.7931 0.0972 0.091 Uiso 1 1 calc R . . C115 C 1.3648(5) 0.8579(5) 0.1602(4) 0.069(3) Uani 1 1 d GU . . H115 H 1.3952 0.8418 0.1729 0.083 Uiso 1 1 calc R . . C116 C 1.3582(4) 0.9113(4) 0.1865(3) 0.060(3) Uani 1 1 d GU . . H116 H 1.3841 0.9307 0.2169 0.072 Uiso 1 1 calc R . . N121 N 1.1766(3) 1.0037(3) 0.1055(3) 0.0512(19) Uani 1 1 d GU . . N122 N 1.2328(3) 0.9946(3) 0.1274(3) 0.054(2) Uani 1 1 d GU . . C123 C 1.2299(3) 0.9327(4) 0.1043(4) 0.058(2) Uani 1 1 d GU . . C124 C 1.1720(4) 0.9036(3) 0.0681(3) 0.060(3) Uani 1 1 d GU . . H124 H 1.1581 0.8629 0.0475 0.072 Uiso 1 1 calc R . . C125 C 1.1390(4) 0.9474(4) 0.0689(3) 0.059(3) Uani 1 1 d GU . . H125 H 1.0997 0.9405 0.0489 0.071 Uiso 1 1 calc R . . C126 C 1.1722(5) 1.0651(6) 0.1212(5) 0.055(2) Uani 1 1 d U . . H12A H 1.1793 1.0714 0.1582 0.066 Uiso 1 1 calc R . . H12B H 1.1242 1.0574 0.1134 0.066 Uiso 1 1 calc R . . N131 N 1.2879(4) 1.1630(4) -0.2573(3) 0.058(2) Uani 1 1 d GU . . C132 C 1.3472(3) 1.1556(5) -0.2704(4) 0.077(3) Uani 1 1 d GU . . C133 C 1.3394(5) 1.1038(6) -0.3065(5) 0.098(4) Uani 1 1 d GU . . H133 H 1.3791 1.0988 -0.3153 0.118 Uiso 1 1 calc R . . C134 C 1.2723(6) 1.0594(6) -0.3294(5) 0.104(4) Uani 1 1 d GU . . H134 H 1.2671 1.0247 -0.3535 0.125 Uiso 1 1 calc R . . C135 C 1.2130(4) 1.0668(5) -0.3162(4) 0.093(4) Uani 1 1 d GU . . H135 H 1.1681 1.0372 -0.3315 0.112 Uiso 1 1 calc R . . C136 C 1.2208(3) 1.1186(4) -0.2802(4) 0.066(3) Uani 1 1 d GU . . H136 H 1.1811 1.1236 -0.2713 0.080 Uiso 1 1 calc R . . N141 N 1.4944(4) 1.2952(5) -0.2012(4) 0.083(3) Uani 1 1 d GU . . N142 N 1.4211(3) 1.2589(5) -0.2182(4) 0.059(2) Uani 1 1 d GU . . C143 C 1.4091(4) 1.1974(5) -0.2475(4) 0.076(3) Uani 1 1 d GU . . C144 C 1.4750(5) 1.1957(5) -0.2486(5) 0.084(3) Uani 1 1 d GU . . H144 H 1.4823 1.1611 -0.2652 0.101 Uiso 1 1 calc R . . C145 C 1.5277(4) 1.2562(6) -0.2200(5) 0.089(4) Uani 1 1 d GU . . H145 H 1.5757 1.2681 -0.2146 0.107 Uiso 1 1 calc R . . C146 C 1.5147(8) 1.3626(10) -0.1729(7) 0.084(4) Uani 1 1 d U . . H14A H 1.5668 1.3888 -0.1674 0.101 Uiso 1 1 calc R . . H14B H 1.5025 1.3930 -0.1936 0.101 Uiso 1 1 calc R . . C151 C 1.2286(3) 1.1327(3) 0.0943(2) 0.051(2) Uani 1 1 d GU . . C152 C 1.2947(3) 1.1753(3) 0.11892(17) 0.058(2) Uani 1 1 d GU . . H152 H 1.3038 1.1609 0.1506 0.070 Uiso 1 1 calc R . . C153 C 1.3472(3) 1.2396(3) 0.09626(15) 0.059(2) Uani 1 1 d GU . . H153 H 1.3914 1.2681 0.1128 0.071 Uiso 1 1 calc R . . C154 C 1.3335(2) 1.2612(2) 0.04894(16) 0.058(2) Uani 1 1 d GU . . C155 C 1.26742(19) 1.2186(2) 0.02429(18) 0.060(3) Uani 1 1 d GU . . H155 H 1.2583 1.2330 -0.0074 0.072 Uiso 1 1 calc R . . C156 C 1.2149(2) 1.1543(3) 0.0469(2) 0.052(2) Uani 1 1 d GU . . H156 H 1.1707 1.1258 0.0304 0.063 Uiso 1 1 calc R . . C161 C 1.4789(3) 1.3492(3) -0.12419(19) 0.057(2) Uani 1 1 d GU . . C162 C 1.4832(3) 1.4095(3) -0.0998(2) 0.066(3) Uani 1 1 d GU . . H162 H 1.5080 1.4549 -0.1154 0.079 Uiso 1 1 calc R . . C163 C 1.4506(3) 1.4019(2) -0.0520(2) 0.068(3) Uani 1 1 d GU . . H163 H 1.4535 1.4422 -0.0356 0.081 Uiso 1 1 calc R . . C164 C 1.4135(2) 1.33412(19) -0.02858(17) 0.058(2) Uani 1 1 d GU . . C165 C 1.4092(2) 1.2739(2) -0.05300(16) 0.058(2) Uani 1 1 d GU . . H165 H 1.3844 1.2285 -0.0374 0.069 Uiso 1 1 calc R . . C166 C 1.4418(3) 1.2814(3) -0.10080(18) 0.054(2) Uani 1 1 d GU . . H166 H 1.4389 1.2411 -0.1171 0.064 Uiso 1 1 calc R . . C171 C 1.3905(6) 1.3302(6) 0.0290(5) 0.053(2) Uani 1 1 d U . . O172 O 1.4220(5) 1.3875(5) 0.0537(5) 0.078(3) Uani 1 1 d . . . N211 N 1.2942(4) 1.1109(3) 0.2523(3) 0.058(2) Uani 1 1 d GU . . C212 C 1.3524(3) 1.1816(4) 0.2534(4) 0.067(3) Uani 1 1 d GU . . C213 C 1.3426(5) 1.2377(3) 0.2714(5) 0.084(4) Uani 1 1 d GU . . H213 H 1.3815 1.2850 0.2721 0.101 Uiso 1 1 calc R . . C214 C 1.2746(6) 1.2230(4) 0.2884(5) 0.103(4) Uani 1 1 d GU . . H214 H 1.2680 1.2605 0.3004 0.124 Uiso 1 1 calc R . . C215 C 1.2164(4) 1.1523(5) 0.2873(5) 0.085(4) Uani 1 1 d GU . . H215 H 1.1709 1.1425 0.2987 0.102 Uiso 1 1 calc R . . C216 C 1.2262(3) 1.0963(3) 0.2693(4) 0.059(3) Uani 1 1 d GU . . H216 H 1.1873 1.0490 0.2686 0.070 Uiso 1 1 calc R . . N221 N 1.4939(4) 1.1645(5) 0.1972(4) 0.070(2) Uani 1 1 d GU . . N222 N 1.4213(3) 1.1368(4) 0.2143(4) 0.069(3) Uani 1 1 d GU . . C223 C 1.4166(4) 1.1945(5) 0.2380(4) 0.071(3) Uani 1 1 d GU . . C224 C 1.4862(5) 1.2578(4) 0.2355(5) 0.087(4) Uani 1 1 d GU . . H224 H 1.4983 1.3034 0.2482 0.104 Uiso 1 1 calc R . . C225 C 1.5340(3) 1.2393(4) 0.2103(5) 0.087(4) Uani 1 1 d GU . . H225 H 1.5829 1.2707 0.2035 0.104 Uiso 1 1 calc R . . C226 C 1.5129(6) 1.1187(8) 0.1732(6) 0.066(3) Uani 1 1 d U . . H22A H 1.4959 1.0748 0.1935 0.079 Uiso 1 1 calc R . . H22B H 1.5653 1.1421 0.1705 0.079 Uiso 1 1 calc R . . N231 N 1.3179(4) 1.3616(3) -0.1671(3) 0.053(2) Uani 1 1 d GU . . C232 C 1.2726(4) 1.3496(3) -0.1251(3) 0.057(2) Uani 1 1 d GU . . C233 C 1.2778(6) 1.4082(5) -0.0976(3) 0.085(4) Uani 1 1 d GU . . H233 H 1.2475 1.4002 -0.0695 0.101 Uiso 1 1 calc R . . C234 C 1.3282(7) 1.4787(4) -0.1121(4) 0.092(4) Uani 1 1 d GU . . H234 H 1.3317 1.5178 -0.0937 0.110 Uiso 1 1 calc R . . C235 C 1.3735(6) 1.4906(3) -0.1542(4) 0.079(4) Uani 1 1 d GU . . H235 H 1.4072 1.5378 -0.1639 0.095 Uiso 1 1 calc R . . C236 C 1.3683(4) 1.4321(3) -0.1816(3) 0.061(3) Uani 1 1 d GU . . H236 H 1.3986 1.4401 -0.2098 0.073 Uiso 1 1 calc R . . N241 N 1.1791(3) 1.1562(3) -0.1134(3) 0.055(2) Uani 1 1 d GDU . . N242 N 1.2362(3) 1.2240(3) -0.1312(3) 0.0481(18) Uani 1 1 d GU . . C243 C 1.2254(4) 1.2797(3) -0.1105(3) 0.057(2) Uani 1 1 d GU . . C244 C 1.1615(4) 1.2463(4) -0.0798(3) 0.059(3) Uani 1 1 d GU . . H244 H 1.1419 1.2702 -0.0617 0.071 Uiso 1 1 calc R . . C245 C 1.1329(3) 1.1700(4) -0.0816(3) 0.061(3) Uani 1 1 d GU . . H245 H 1.0912 1.1352 -0.0649 0.073 Uiso 1 1 calc R . . C246 C 1.1729(7) 1.0910(6) -0.1256(6) 0.062(3) Uani 1 1 d DU . . H24A H 1.1745 1.0870 -0.1628 0.074 Uiso 1 1 calc R . . H24B H 1.1263 1.0522 -0.1137 0.074 Uiso 1 1 calc R . . C251 C 1.4771(3) 1.0983(4) 0.1162(2) 0.064(2) Uani 1 1 d GU . . C252 C 1.4789(3) 1.0419(4) 0.0903(2) 0.067(3) Uani 1 1 d GU . . H252 H 1.4998 1.0174 0.1060 0.081 Uiso 1 1 calc R . . C253 C 1.4495(3) 1.0222(4) 0.0411(2) 0.069(3) Uani 1 1 d GU . . H253 H 1.4507 0.9845 0.0238 0.083 Uiso 1 1 calc R . . C254 C 1.4184(2) 1.0589(3) 0.01772(18) 0.065(2) Uani 1 1 d GU . . C255 C 1.4166(2) 1.1153(3) 0.04358(18) 0.071(3) Uani 1 1 d GU . . H255 H 1.3957 1.1398 0.0279 0.086 Uiso 1 1 calc R . . C256 C 1.4460(3) 1.1349(4) 0.0928(2) 0.071(3) Uani 1 1 d GU . . H256 H 1.4448 1.1726 0.1101 0.085 Uiso 1 1 calc R . . C261 C 1.2336(3) 1.0819(3) -0.1012(2) 0.064(3) Uani 1 1 d GU . . C262 C 1.2957(3) 1.0980(4) -0.12920(19) 0.061(3) Uani 1 1 d GU . . H262 H 1.3013 1.1158 -0.1627 0.073 Uiso 1 1 calc R . . C263 C 1.3493(3) 1.0875(4) -0.10713(16) 0.061(3) Uani 1 1 d GU . . H263 H 1.3908 1.0983 -0.1258 0.074 Uiso 1 1 calc R . . C264 C 1.3409(2) 1.0609(3) -0.05709(16) 0.060(2) Uani 1 1 d GU . . C265 C 1.27879(19) 1.0448(3) -0.02913(18) 0.063(3) Uani 1 1 d GU . . H265 H 1.2731 1.0270 0.0043 0.075 Uiso 1 1 calc R . . C266 C 1.2252(2) 1.0553(4) -0.0512(2) 0.054(2) Uani 1 1 d GU . . H266 H 1.1836 1.0445 -0.0325 0.064 Uiso 1 1 calc R . . C271 C 1.4004(7) 1.0472(9) -0.0376(6) 0.072(3) Uani 1 1 d U . . O272 O 1.4308(5) 1.0233(8) -0.0626(4) 0.084(3) Uani 1 1 d . . . B11 B 0.6667 0.3333 0.6638(5) 0.046(4) Uani 1 3 d SDU . . F12 F 0.6667 0.3333 0.7168(5) 0.112(6) Uani 1 3 d SDU . . F13 F 0.6062(5) 0.2708(4) 0.6464(4) 0.076(2) Uani 1 1 d DU . . B21 B 1.0000 1.0000 0.5057(6) 0.048(4) Uani 1 3 d SDU . . F22 F 1.0562(3) 1.0636(3) 0.4862(3) 0.0669(19) Uani 1 1 d DU . . F23 F 1.0000 1.0000 0.5599(5) 0.069(3) Uani 1 3 d SDU . . B31 B 0.4392(7) 0.4357(6) 0.2520(5) 0.065(3) Uani 1 1 d DU . . F32 F 0.4727(6) 0.5078(4) 0.2611(5) 0.119(4) Uani 1 1 d DU . . F33 F 0.3795(6) 0.4002(5) 0.2840(4) 0.104(4) Uani 1 1 d DU . . F34 F 0.4880(5) 0.4124(5) 0.2637(4) 0.094(3) Uani 1 1 d DU . . F35 F 0.4184(7) 0.4185(8) 0.2032(4) 0.133(5) Uani 1 1 d DU . . C11S C 0.341(2) 0.4632(17) 0.1026(12) 0.163(5) Uani 1 1 d DU . . H11A H 0.3704 0.5134 0.1118 0.245 Uiso 1 1 calc R . . H11B H 0.3706 0.4406 0.1027 0.245 Uiso 1 1 calc R . . H11C H 0.3024 0.4392 0.1270 0.245 Uiso 1 1 calc R . . N12S N 0.3101(12) 0.4573(11) 0.0499(10) 0.166(5) Uani 1 1 d DU . . O13S O 0.3099(14) 0.5058(10) 0.0230(11) 0.168(5) Uani 1 1 d DU . . O14S O 0.2731(13) 0.3934(9) 0.0381(10) 0.164(5) Uani 1 1 d DU . . O1S O 0.6667 0.3333 0.8777(12) 0.116(8) Uani 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0526(4) 0.0554(5) 0.0707(5) 0.0091(4) 0.0024(4) 0.0299(4) Ag2 0.0537(5) 0.0459(4) 0.0651(5) 0.0046(4) 0.0042(4) 0.0188(3) N111 0.033(4) 0.037(4) 0.095(6) 0.002(4) -0.010(4) 0.020(3) C112 0.038(4) 0.040(4) 0.084(6) 0.009(4) 0.015(4) 0.012(4) C113 0.060(6) 0.044(5) 0.097(8) -0.005(5) 0.000(6) 0.017(4) C114 0.066(6) 0.056(6) 0.101(8) -0.007(6) 0.014(6) 0.027(5) C115 0.067(6) 0.065(6) 0.083(7) -0.002(5) 0.009(5) 0.038(5) C116 0.054(5) 0.037(4) 0.091(7) -0.025(4) 0.002(5) 0.024(4) N121 0.028(3) 0.048(4) 0.070(5) 0.010(4) -0.007(3) 0.013(3) N122 0.030(4) 0.042(4) 0.082(6) 0.014(4) 0.008(4) 0.014(3) C123 0.035(4) 0.034(4) 0.088(6) 0.007(4) -0.010(4) 0.005(3) C124 0.031(4) 0.034(4) 0.110(7) 0.012(5) -0.011(5) 0.011(4) C125 0.041(5) 0.041(4) 0.099(7) 0.000(5) -0.021(5) 0.024(4) C126 0.034(4) 0.057(5) 0.077(6) 0.027(5) 0.002(4) 0.026(4) N131 0.047(4) 0.047(4) 0.079(6) 0.016(4) -0.002(4) 0.022(4) C132 0.076(6) 0.059(5) 0.112(7) 0.002(5) -0.007(6) 0.046(5) C133 0.078(7) 0.091(8) 0.136(10) -0.028(7) -0.029(7) 0.050(6) C134 0.080(7) 0.102(9) 0.142(10) -0.036(8) -0.045(7) 0.055(7) C135 0.078(7) 0.078(7) 0.130(10) -0.024(7) -0.046(7) 0.044(6) C136 0.058(5) 0.048(5) 0.084(7) 0.017(4) -0.033(5) 0.020(4) N141 0.041(4) 0.098(6) 0.093(6) 0.012(5) 0.020(5) 0.021(4) N142 0.035(4) 0.072(5) 0.069(5) 0.021(4) 0.002(4) 0.025(4) C143 0.061(5) 0.074(6) 0.105(7) 0.023(5) -0.003(5) 0.042(5) C144 0.055(6) 0.087(7) 0.108(9) 0.012(7) 0.013(6) 0.033(5) C145 0.055(6) 0.096(8) 0.107(9) 0.022(7) 0.013(6) 0.031(5) C146 0.055(6) 0.089(7) 0.084(7) 0.021(6) 0.021(6) 0.017(6) C151 0.056(5) 0.043(4) 0.061(5) 0.010(4) 0.018(4) 0.031(4) C152 0.053(5) 0.064(6) 0.066(6) 0.023(5) 0.015(4) 0.035(4) C153 0.043(5) 0.055(5) 0.084(7) 0.005(5) -0.005(5) 0.027(4) C154 0.040(4) 0.052(5) 0.085(6) 0.004(4) -0.006(4) 0.025(4) C155 0.054(5) 0.033(4) 0.077(6) 0.014(4) -0.016(5) 0.010(4) C156 0.040(4) 0.037(4) 0.080(6) 0.005(4) -0.017(4) 0.019(4) C161 0.045(5) 0.053(5) 0.060(5) 0.009(4) -0.014(4) 0.016(4) C162 0.058(6) 0.046(5) 0.087(7) 0.005(5) -0.016(5) 0.021(5) C163 0.063(6) 0.039(5) 0.073(6) -0.009(4) -0.031(5) 0.004(4) C164 0.046(5) 0.047(4) 0.079(6) 0.004(4) -0.008(4) 0.021(4) C165 0.056(5) 0.035(4) 0.073(6) -0.002(4) -0.001(5) 0.016(4) C166 0.044(5) 0.051(5) 0.057(5) 0.015(4) -0.006(4) 0.018(4) C171 0.034(4) 0.039(4) 0.079(6) 0.003(4) -0.011(4) 0.012(4) O172 0.046(4) 0.040(4) 0.135(10) -0.021(5) 0.005(5) 0.012(4) N211 0.049(4) 0.042(4) 0.087(6) 0.015(4) 0.009(4) 0.026(4) C212 0.065(5) 0.047(5) 0.084(7) 0.019(5) 0.010(5) 0.023(4) C213 0.100(8) 0.042(5) 0.110(9) 0.014(6) 0.014(7) 0.034(5) C214 0.103(8) 0.061(6) 0.139(10) 0.005(7) 0.027(8) 0.037(6) C215 0.084(7) 0.065(6) 0.119(9) 0.002(6) 0.025(7) 0.046(5) C216 0.053(5) 0.050(5) 0.088(7) 0.024(5) 0.017(5) 0.037(4) N221 0.033(4) 0.078(5) 0.091(6) 0.018(5) -0.004(4) 0.022(4) N222 0.039(4) 0.079(6) 0.081(7) 0.023(5) -0.001(4) 0.022(4) C223 0.051(5) 0.051(5) 0.110(7) 0.013(5) -0.012(5) 0.025(4) C224 0.052(6) 0.073(7) 0.116(9) 0.033(6) -0.006(6) 0.017(5) C225 0.050(5) 0.090(7) 0.122(9) 0.023(7) -0.010(6) 0.036(5) C226 0.038(5) 0.085(7) 0.082(6) 0.018(5) 0.014(4) 0.036(5) N231 0.047(4) 0.043(4) 0.058(5) 0.024(4) 0.005(4) 0.014(3) C232 0.050(5) 0.048(5) 0.071(6) 0.016(4) 0.005(4) 0.024(4) C233 0.094(8) 0.067(6) 0.092(8) 0.019(6) 0.023(7) 0.039(6) C234 0.130(9) 0.044(5) 0.098(8) -0.001(5) 0.035(7) 0.041(6) C235 0.104(8) 0.041(5) 0.084(7) 0.010(5) 0.024(6) 0.030(5) C236 0.060(6) 0.030(4) 0.080(6) -0.005(4) -0.003(5) 0.015(4) N241 0.038(4) 0.047(4) 0.075(5) 0.024(4) 0.001(4) 0.017(3) N242 0.034(4) 0.038(4) 0.069(5) 0.014(4) 0.004(3) 0.016(3) C243 0.033(4) 0.065(5) 0.072(6) 0.022(4) 0.005(4) 0.025(4) C244 0.037(4) 0.071(6) 0.079(6) 0.028(5) 0.023(4) 0.034(4) C245 0.029(4) 0.078(6) 0.077(6) 0.024(5) 0.015(4) 0.028(4) C246 0.044(5) 0.053(5) 0.083(7) 0.013(5) -0.006(5) 0.019(4) C251 0.046(5) 0.076(6) 0.074(6) 0.018(5) 0.012(4) 0.034(4) C252 0.051(5) 0.087(7) 0.084(6) 0.028(5) 0.014(5) 0.049(5) C253 0.041(5) 0.092(7) 0.089(7) 0.033(6) 0.011(5) 0.044(5) C254 0.049(5) 0.068(5) 0.090(6) 0.039(5) 0.024(4) 0.039(4) C255 0.068(6) 0.072(6) 0.083(6) 0.033(5) 0.008(5) 0.042(5) C256 0.045(5) 0.084(7) 0.078(6) 0.018(6) 0.009(5) 0.028(5) C261 0.050(5) 0.048(5) 0.082(6) 0.022(5) 0.003(5) 0.016(4) C262 0.053(5) 0.055(5) 0.068(6) 0.004(5) 0.007(5) 0.023(5) C263 0.052(5) 0.054(5) 0.071(6) 0.012(5) 0.019(5) 0.021(5) C264 0.041(4) 0.068(5) 0.083(6) 0.012(5) 0.026(4) 0.037(4) C265 0.032(4) 0.077(6) 0.075(6) 0.021(5) 0.011(4) 0.024(4) C266 0.044(5) 0.050(5) 0.074(6) 0.003(4) 0.001(4) 0.028(4) C271 0.051(5) 0.087(7) 0.100(7) 0.029(6) 0.014(5) 0.052(5) O272 0.046(5) 0.134(10) 0.078(6) -0.007(6) 0.012(4) 0.048(6) B11 0.052(6) 0.052(6) 0.035(8) 0.000 0.000 0.026(3) F12 0.148(10) 0.148(10) 0.039(7) 0.000 0.000 0.074(5) F13 0.075(5) 0.055(4) 0.095(6) -0.010(4) -0.014(4) 0.030(4) B21 0.039(5) 0.039(5) 0.068(9) 0.000 0.000 0.019(2) F22 0.034(3) 0.035(3) 0.114(6) 0.001(3) -0.010(3) 0.004(2) F23 0.069(4) 0.069(4) 0.068(7) 0.000 0.000 0.035(2) B31 0.081(8) 0.036(5) 0.070(7) 0.009(5) 0.014(6) 0.024(5) F32 0.100(7) 0.029(3) 0.202(11) 0.005(5) -0.015(8) 0.013(4) F33 0.120(8) 0.087(6) 0.093(7) 0.031(5) 0.062(6) 0.044(6) F34 0.102(7) 0.063(5) 0.098(6) 0.012(5) 0.020(5) 0.028(5) F35 0.108(8) 0.205(13) 0.083(6) -0.038(8) -0.007(6) 0.074(9) C11S 0.165(11) 0.102(7) 0.217(13) 0.018(9) 0.012(10) 0.062(8) N12S 0.166(11) 0.103(7) 0.217(13) 0.019(9) 0.013(10) 0.059(8) O13S 0.168(11) 0.104(7) 0.217(13) 0.021(9) 0.012(10) 0.058(8) O14S 0.164(11) 0.103(7) 0.216(13) 0.018(9) 0.014(10) 0.060(8) O1S 0.117(12) 0.117(12) 0.115(18) 0.000 0.000 0.058(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 Ag1 N211 2.269(6) . ? Ag1 N111 2.275(5) . ? Ag1 N222 2.336(6) . ? Ag1 N122 2.396(5) . ? Ag1 Ag2 2.9870(14) 6_565 ? Ag2 N231 2.258(5) . ? Ag2 N142 2.278(6) . ? Ag2 N242 2.350(5) . ? Ag2 N131 2.410(7) . ? Ag2 Ag1 2.9869(14) 2_654 ? N111 C112 1.3900 . ? N111 C116 1.3900 . ? C112 C113 1.3900 . ? C112 C123 1.395(7) . ? C113 C114 1.3900 . ? C113 H113 0.9300 . ? C114 C115 1.3900 . ? C114 H114 0.9300 . ? C115 C116 1.3900 . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? N121 C126 1.415(14) . ? N121 N122 1.4200 . ? N121 C125 1.4200 . ? N122 C123 1.4200 . ? C123 C124 1.4200 . ? C124 C125 1.4200 . ? C124 H124 0.9300 . ? C125 H125 0.9300 . ? C126 C151 1.506(11) . ? C126 H12A 0.9700 . ? C126 H12B 0.9700 . ? N131 C132 1.3900 . ? N131 C136 1.3900 . ? C132 C143 1.306(9) . ? C132 C133 1.3900 . ? C133 C134 1.3900 . ? C133 H133 0.9300 . ? C134 C135 1.3900 . ? C134 H134 0.9300 . ? C135 C136 1.3900 . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? N141 C145 1.4200 . ? N141 N142 1.4200 . ? N141 C146 1.47(2) . ? N142 C143 1.4200 . ? C143 C144 1.4200 . ? C144 C145 1.4200 . ? C144 H144 0.9300 . ? C145 H145 0.9300 . ? C146 C161 1.427(17) . ? C146 H14A 0.9700 . ? C146 H14B 0.9700 . ? C151 C152 1.3900 . ? C151 C156 1.3900 . ? C152 C153 1.3900 . ? C152 H152 0.9300 . ? C153 C154 1.3900 . ? C153 H153 0.9300 . ? C154 C155 1.3900 . ? C154 C171 1.453(11) . ? C155 C156 1.3900 . ? C155 H155 0.9300 . ? C156 H156 0.9300 . ? C161 C162 1.3900 . ? C161 C166 1.3900 . ? C162 C163 1.3900 . ? C162 H162 0.9300 . ? C163 C164 1.3900 . ? C163 H163 0.9300 . ? C164 C165 1.3902 . ? C164 C171 1.560(14) . ? C165 C166 1.3897 . ? C165 H165 0.9300 . ? C166 H166 0.9300 . ? C171 O172 1.237(15) . ? N211 C212 1.3900 . ? N211 C216 1.3900 . ? C212 C223 1.312(9) . ? C212 C213 1.3900 . ? C213 C214 1.3900 . ? C213 H213 0.9300 . ? C214 C215 1.3900 . ? C214 H214 0.9300 . ? C215 C216 1.3900 . ? C215 H215 0.9300 . ? C216 H216 0.9300 . ? N221 C226 1.375(16) . ? N221 N222 1.4200 . ? N221 C225 1.4200 . ? N222 C223 1.4200 . ? C223 C224 1.4200 . ? C224 C225 1.4200 . ? C224 H224 0.9300 . ? C225 H225 0.9300 . ? C226 C251 1.618(16) . ? C226 H22A 0.9700 . ? C226 H22B 0.9700 . ? N231 C232 1.3900 . ? N231 C236 1.3900 . ? C232 C243 1.368(7) . ? C232 C233 1.3900 . ? C233 C234 1.3900 . ? C233 H233 0.9300 . ? C234 C235 1.3900 . ? C234 H234 0.9300 . ? C235 C236 1.3900 . ? C235 H235 0.9300 . ? C236 H236 0.9300 . ? N241 C246 1.365(12) . ? N241 N242 1.4200 . ? N241 C245 1.4200 . ? N242 C243 1.4200 . ? C243 C244 1.4200 . ? C244 C245 1.4200 . ? C244 H244 0.9300 . ? C245 H245 0.9300 . ? C246 C261 1.533(13) . ? C246 H24A 0.9700 . ? C246 H24B 0.9700 . ? C251 C252 1.3900 . ? C251 C256 1.3900 . ? C252 C253 1.3900 . ? C252 H252 0.9300 . ? C253 C254 1.3900 . ? C253 H253 0.9300 . ? C254 C255 1.3900 . ? C254 C271 1.473(18) . ? C255 C256 1.3900 . ? C255 H255 0.9300 . ? C256 H256 0.9300 . ? C261 C266 1.3900 . ? C261 C262 1.3900 . ? C262 C263 1.3899 . ? C262 H262 0.9300 . ? C263 C264 1.3900 . ? C263 H263 0.9300 . ? C264 C265 1.3900 . ? C264 C271 1.520(12) . ? C265 C266 1.3899 . ? C265 H265 0.9300 . ? C266 H266 0.9300 . ? C271 O272 1.193(18) . ? B11 F12 1.374(16) . ? B11 F13 1.384(8) . ? B11 F13 1.384(8) 3_655 ? B11 F13 1.384(8) 5_665 ? B21 F22 1.377(8) 3_765 ? B21 F22 1.377(8) 5_675 ? B21 F22 1.377(8) . ? B21 F23 1.402(16) . ? B31 F35 1.331(14) . ? B31 F32 1.349(12) . ? B31 F33 1.383(13) . ? B31 F34 1.389(14) . ? C11S N12S 1.493(19) . ? C11S H11A 0.9600 . ? C11S H11B 0.9600 . ? C11S H11C 0.9600 . ? N12S O14S 1.220(17) . ? N12S O13S 1.247(17) . ? 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 N211 Ag1 N111 167.1(3) . . ? N211 Ag1 N222 70.7(3) . . ? N111 Ag1 N222 115.7(3) . . ? N211 Ag1 N122 112.7(3) . . ? N111 Ag1 N122 72.9(2) . . ? N222 Ag1 N122 128.5(3) . . ? N211 Ag1 Ag2 81.6(2) . 6_565 ? N111 Ag1 Ag2 85.6(2) . 6_565 ? N222 Ag1 Ag2 109.7(2) . 6_565 ? N122 Ag1 Ag2 121.74(17) . 6_565 ? N231 Ag2 N142 124.7(3) . . ? N231 Ag2 N242 72.1(2) . . ? N142 Ag2 N242 134.2(3) . . ? N231 Ag2 N131 158.2(3) . . ? N142 Ag2 N131 71.0(3) . . ? N242 Ag2 N131 108.8(3) . . ? N231 Ag2 Ag1 83.49(19) . 2_654 ? N142 Ag2 Ag1 106.6(2) . 2_654 ? N242 Ag2 Ag1 118.15(17) . 2_654 ? N131 Ag2 Ag1 77.02(19) . 2_654 ? C112 N111 C116 120.0 . . ? C112 N111 Ag1 117.1(3) . . ? C116 N111 Ag1 122.5(3) . . ? C113 C112 N111 120.0 . . ? C113 C112 C123 121.9(6) . . ? N111 C112 C123 118.1(6) . . ? C114 C113 C112 120.0 . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C116 C115 C114 120.0 . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C115 C116 N111 120.0 . . ? C115 C116 H116 120.0 . . ? N111 C116 H116 120.0 . . ? C126 N121 N122 117.3(6) . . ? C126 N121 C125 134.5(6) . . ? N122 N121 C125 108.0 . . ? N121 N122 C123 108.0 . . ? N121 N122 Ag1 139.1(4) . . ? C123 N122 Ag1 110.8(4) . . ? C112 C123 C124 131.0(6) . . ? C112 C123 N122 120.5(6) . . ? C124 C123 N122 108.0 . . ? C125 C124 C123 108.0 . . ? C125 C124 H124 126.0 . . ? C123 C124 H124 126.0 . . ? C124 C125 N121 108.0 . . ? C124 C125 H125 126.0 . . ? N121 C125 H125 126.0 . . ? N121 C126 C151 111.0(9) . . ? N121 C126 H12A 109.4 . . ? C151 C126 H12A 109.4 . . ? N121 C126 H12B 109.4 . . ? C151 C126 H12B 109.4 . . ? H12A C126 H12B 108.0 . . ? C132 N131 C136 120.0 . . ? C132 N131 Ag2 113.1(4) . . ? C136 N131 Ag2 126.6(4) . . ? C143 C132 C133 121.8(7) . . ? C143 C132 N131 118.2(7) . . ? C133 C132 N131 120.0 . . ? C132 C133 C134 120.0 . . ? C132 C133 H133 120.0 . . ? C134 C133 H133 120.0 . . ? C133 C134 C135 120.0 . . ? C133 C134 H134 120.0 . . ? C135 C134 H134 120.0 . . ? C136 C135 C134 120.0 . . ? C136 C135 H135 120.0 . . ? C134 C135 H135 120.0 . . ? C135 C136 N131 120.0 . . ? C135 C136 H136 120.0 . . ? N131 C136 H136 120.0 . . ? C145 N141 N142 108.0 . . ? C145 N141 C146 138.8(9) . . ? N142 N141 C146 113.1(9) . . ? C143 N142 N141 108.0 . . ? C143 N142 Ag2 114.6(5) . . ? N141 N142 Ag2 136.5(5) . . ? C132 C143 C144 130.1(8) . . ? C132 C143 N142 121.8(7) . . ? C144 C143 N142 108.0 . . ? C143 C144 C145 108.0 . . ? C143 C144 H144 126.0 . . ? C145 C144 H144 126.0 . . ? C144 C145 N141 108.0 . . ? C144 C145 H145 126.0 . . ? N141 C145 H145 126.0 . . ? C161 C146 N141 112.4(11) . . ? C161 C146 H14A 109.1 . . ? N141 C146 H14A 109.1 . . ? C161 C146 H14B 109.1 . . ? N141 C146 H14B 109.1 . . ? H14A C146 H14B 107.9 . . ? C152 C151 C156 120.0 . . ? C152 C151 C126 118.2(5) . . ? C156 C151 C126 121.8(5) . . ? C153 C152 C151 120.0 . . ? C153 C152 H152 120.0 . . ? C151 C152 H152 120.0 . . ? C152 C153 C154 120.0 . . ? C152 C153 H153 120.0 . . ? C154 C153 H153 120.0 . . ? C155 C154 C153 120.0 . . ? C155 C154 C171 123.8(5) . . ? C153 C154 C171 116.2(5) . . ? C156 C155 C154 120.0 . . ? C156 C155 H155 120.0 . . ? C154 C155 H155 120.0 . . ? C155 C156 C151 120.0 . . ? C155 C156 H156 120.0 . . ? C151 C156 H156 120.0 . . ? C162 C161 C166 120.0 . . ? C162 C161 C146 115.9(8) . . ? C166 C161 C146 124.1(8) . . ? C161 C162 C163 120.0 . . ? C161 C162 H162 120.0 . . ? C163 C162 H162 120.0 . . ? C164 C163 C162 120.0 . . ? C164 C163 H163 120.0 . . ? C162 C163 H163 120.0 . . ? C163 C164 C165 120.0 . . ? C163 C164 C171 118.2(4) . . ? C165 C164 C171 120.8(4) . . ? C166 C165 C164 120.0 . . ? C166 C165 H165 120.0 . . ? C164 C165 H165 120.0 . . ? C165 C166 C161 120.0 . . ? C165 C166 H166 120.0 . . ? C161 C166 H166 120.0 . . ? O172 C171 C154 125.4(12) . . ? O172 C171 C164 116.2(10) . . ? C154 C171 C164 118.4(8) . . ? C212 N211 C216 120.0 . . ? C212 N211 Ag1 115.8(4) . . ? C216 N211 Ag1 122.0(4) . . ? C223 C212 C213 120.7(6) . . ? C223 C212 N211 119.3(6) . . ? C213 C212 N211 120.0 . . ? C212 C213 C214 120.0 . . ? C212 C213 H213 120.0 . . ? C214 C213 H213 120.0 . . ? C215 C214 C213 120.0 . . ? C215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C216 C215 C214 120.0 . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? C215 C216 N211 120.0 . . ? C215 C216 H216 120.0 . . ? N211 C216 H216 120.0 . . ? C226 N221 N222 119.3(8) . . ? C226 N221 C225 132.7(8) . . ? N222 N221 C225 108.0 . . ? C223 N222 N221 108.0 . . ? C223 N222 Ag1 113.8(4) . . ? N221 N222 Ag1 137.3(4) . . ? C212 C223 C224 133.9(7) . . ? C212 C223 N222 117.9(7) . . ? C224 C223 N222 108.0 . . ? C223 C224 C225 108.0 . . ? C223 C224 H224 126.0 . . ? C225 C224 H224 126.0 . . ? C224 C225 N221 108.0 . . ? C224 C225 H225 126.0 . . ? N221 C225 H225 126.0 . . ? N221 C226 C251 109.8(9) . . ? N221 C226 H22A 109.7 . . ? C251 C226 H22A 109.7 . . ? N221 C226 H22B 109.7 . . ? C251 C226 H22B 109.7 . . ? H22A C226 H22B 108.2 . . ? C232 N231 C236 120.0 . . ? C232 N231 Ag2 117.0(3) . . ? C236 N231 Ag2 122.1(3) . . ? C243 C232 N231 118.7(6) . . ? C243 C232 C233 121.3(6) . . ? N231 C232 C233 120.0 . . ? C234 C233 C232 120.0 . . ? C234 C233 H233 120.0 . . ? C232 C233 H233 120.0 . . ? C233 C234 C235 120.0 . . ? C233 C234 H234 120.0 . . ? C235 C234 H234 120.0 . . ? C236 C235 C234 120.0 . . ? C236 C235 H235 120.0 . . ? C234 C235 H235 120.0 . . ? C235 C236 N231 120.0 . . ? C235 C236 H236 120.0 . . ? N231 C236 H236 120.0 . . ? C246 N241 N242 123.7(7) . . ? C246 N241 C245 128.3(7) . . ? N242 N241 C245 108.0 . . ? C243 N242 N241 108.0 . . ? C243 N242 Ag2 113.0(4) . . ? N241 N242 Ag2 136.2(4) . . ? C232 C243 N242 117.7(6) . . ? C232 C243 C244 134.2(6) . . ? N242 C243 C244 108.0 . . ? C245 C244 C243 108.0 . . ? C245 C244 H244 126.0 . . ? C243 C244 H244 126.0 . . ? N241 C245 C244 108.0 . . ? N241 C245 H245 126.0 . . ? C244 C245 H245 126.0 . . ? N241 C246 C261 112.0(9) . . ? N241 C246 H24A 109.2 . . ? C261 C246 H24A 109.2 . . ? N241 C246 H24B 109.2 . . ? C261 C246 H24B 109.2 . . ? H24A C246 H24B 107.9 . . ? C252 C251 C256 120.0 . . ? C252 C251 C226 117.4(6) . . ? C256 C251 C226 122.6(6) . . ? C253 C252 C251 120.0 . . ? C253 C252 H252 120.0 . . ? C251 C252 H252 120.0 . . ? C252 C253 C254 120.0 . . ? C252 C253 H253 120.0 . . ? C254 C253 H253 120.0 . . ? C255 C254 C253 120.0 . . ? C255 C254 C271 119.9(5) . . ? C253 C254 C271 119.0(5) . . ? C254 C255 C256 120.0 . . ? C254 C255 H255 120.0 . . ? C256 C255 H255 120.0 . . ? C255 C256 C251 120.0 . . ? C255 C256 H256 120.0 . . ? C251 C256 H256 120.0 . . ? C266 C261 C262 120.0 . . ? C266 C261 C246 119.3(6) . . ? C262 C261 C246 120.7(6) . . ? C263 C262 C261 120.0 . . ? C263 C262 H262 120.0 . . ? C261 C262 H262 120.0 . . ? C262 C263 C264 120.0 . . ? C262 C263 H263 120.0 . . ? C264 C263 H263 120.0 . . ? C263 C264 C265 120.0 . . ? C263 C264 C271 115.9(6) . . ? C265 C264 C271 124.0(6) . . ? C266 C265 C264 120.0 . . ? C266 C265 H265 120.0 . . ? C264 C265 H265 120.0 . . ? C265 C266 C261 120.0 . . ? C265 C266 H266 120.0 . . ? C261 C266 H266 120.0 . . ? O272 C271 C254 116.8(10) . . ? O272 C271 C264 125.6(14) . . ? C254 C271 C264 117.5(10) . . ? F12 B11 F13 109.0(7) . . ? F12 B11 F13 109.0(7) . 3_655 ? F13 B11 F13 110.0(7) . 3_655 ? F12 B11 F13 109.0(7) . 5_665 ? F13 B11 F13 110.0(7) . 5_665 ? F13 B11 F13 110.0(7) 3_655 5_665 ? F22 B21 F22 107.2(8) 3_765 5_675 ? F22 B21 F22 107.2(8) 3_765 . ? F22 B21 F22 107.2(8) 5_675 . ? F22 B21 F23 111.6(7) 3_765 . ? F22 B21 F23 111.6(7) 5_675 . ? F22 B21 F23 111.6(7) . . ? F35 B31 F32 113.2(11) . . ? F35 B31 F33 109.4(11) . . ? F32 B31 F33 109.6(10) . . ? F35 B31 F34 108.3(12) . . ? F32 B31 F34 107.6(10) . . ? F33 B31 F34 108.7(9) . . ? N12S C11S H11A 109.5 . . ? N12S C11S H11B 109.5 . . ? H11A C11S H11B 109.5 . . ? N12S C11S H11C 109.5 . . ? H11A C11S H11C 109.5 . . ? H11B C11S H11C 109.5 . . ? O14S N12S O13S 121(2) . . ? O14S N12S C11S 110(2) . . ? O13S N12S C11S 129(2) . . ? 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 N211 Ag1 N111 C112 119.9(11) . . . . ? N222 Ag1 N111 C112 -122.9(4) . . . . ? N122 Ag1 N111 C112 2.2(4) . . . . ? Ag2 Ag1 N111 C112 127.4(4) 6_565 . . . ? N211 Ag1 N111 C116 -67.6(12) . . . . ? N222 Ag1 N111 C116 49.6(5) . . . . ? N122 Ag1 N111 C116 174.7(5) . . . . ? Ag2 Ag1 N111 C116 -60.2(4) 6_565 . . . ? C116 N111 C112 C113 0.0 . . . . ? Ag1 N111 C112 C113 172.7(5) . . . . ? C116 N111 C112 C123 -179.3(8) . . . . ? Ag1 N111 C112 C123 -6.6(7) . . . . ? N111 C112 C113 C114 0.0 . . . . ? C123 C112 C113 C114 179.3(8) . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 N111 0.0 . . . . ? C112 N111 C116 C115 0.0 . . . . ? Ag1 N111 C116 C115 -172.3(5) . . . . ? C126 N121 N122 C123 -176.6(8) . . . . ? C125 N121 N122 C123 0.0 . . . . ? C126 N121 N122 Ag1 22.5(10) . . . . ? C125 N121 N122 Ag1 -160.9(7) . . . . ? N211 Ag1 N122 N121 -5.0(7) . . . . ? N111 Ag1 N122 N121 162.7(7) . . . . ? N222 Ag1 N122 N121 -87.7(7) . . . . ? Ag2 Ag1 N122 N121 89.1(6) 6_565 . . . ? N211 Ag1 N122 C123 -165.5(4) . . . . ? N111 Ag1 N122 C123 2.1(4) . . . . ? N222 Ag1 N122 C123 111.8(4) . . . . ? Ag2 Ag1 N122 C123 -71.4(4) 6_565 . . . ? C113 C112 C123 C124 18.2(11) . . . . ? N111 C112 C123 C124 -162.5(6) . . . . ? C113 C112 C123 N122 -170.2(5) . . . . ? N111 C112 C123 N122 9.1(9) . . . . ? N121 N122 C123 C112 -173.3(9) . . . . ? Ag1 N122 C123 C112 -6.6(7) . . . . ? N121 N122 C123 C124 0.0 . . . . ? Ag1 N122 C123 C124 166.7(5) . . . . ? C112 C123 C124 C125 172.4(10) . . . . ? N122 C123 C124 C125 0.0 . . . . ? C123 C124 C125 N121 0.0 . . . . ? C126 N121 C125 C124 175.7(10) . . . . ? N122 N121 C125 C124 0.0 . . . . ? N122 N121 C126 C151 78.0(10) . . . . ? C125 N121 C126 C151 -97.5(9) . . . . ? N231 Ag2 N131 C132 139.8(7) . . . . ? N142 Ag2 N131 C132 -0.1(5) . . . . ? N242 Ag2 N131 C132 -131.5(5) . . . . ? Ag1 Ag2 N131 C132 112.9(5) 2_654 . . . ? N231 Ag2 N131 C136 -34.3(11) . . . . ? N142 Ag2 N131 C136 -174.1(7) . . . . ? N242 Ag2 N131 C136 54.5(6) . . . . ? Ag1 Ag2 N131 C136 -61.2(6) 2_654 . . . ? C136 N131 C132 C143 -178.9(11) . . . . ? Ag2 N131 C132 C143 6.6(10) . . . . ? C136 N131 C132 C133 0.0 . . . . ? Ag2 N131 C132 C133 -174.5(6) . . . . ? C143 C132 C133 C134 178.9(11) . . . . ? N131 C132 C133 C134 0.0 . . . . ? C132 C133 C134 C135 0.0 . . . . ? C133 C134 C135 C136 0.0 . . . . ? C134 C135 C136 N131 0.0 . . . . ? C132 N131 C136 C135 0.0 . . . . ? Ag2 N131 C136 C135 173.7(7) . . . . ? C145 N141 N142 C143 0.0 . . . . ? C146 N141 N142 C143 176.6(11) . . . . ? C145 N141 N142 Ag2 168.1(9) . . . . ? C146 N141 N142 Ag2 -15.3(13) . . . . ? N231 Ag2 N142 C143 -168.9(5) . . . . ? N242 Ag2 N142 C143 92.3(6) . . . . ? N131 Ag2 N142 C143 -5.8(5) . . . . ? Ag1 Ag2 N142 C143 -75.3(5) 2_654 . . . ? N231 Ag2 N142 N141 23.5(9) . . . . ? N242 Ag2 N142 N141 -75.2(9) . . . . ? N131 Ag2 N142 N141 -173.4(9) . . . . ? Ag1 Ag2 N142 N141 117.1(8) 2_654 . . . ? C133 C132 C143 C144 -7.4(14) . . . . ? N131 C132 C143 C144 171.4(7) . . . . ? C133 C132 C143 N142 168.0(7) . . . . ? N131 C132 C143 N142 -13.1(14) . . . . ? N141 N142 C143 C132 -176.4(12) . . . . ? Ag2 N142 C143 C132 12.6(12) . . . . ? N141 N142 C143 C144 0.0 . . . . ? Ag2 N142 C143 C144 -171.0(7) . . . . ? C132 C143 C144 C145 176.0(14) . . . . ? N142 C143 C144 C145 0.0 . . . . ? C143 C144 C145 N141 0.0 . . . . ? N142 N141 C145 C144 0.0 . . . . ? C146 N141 C145 C144 -175.3(16) . . . . ? C145 N141 C146 C161 -116.6(12) . . . . ? N142 N141 C146 C161 68.2(15) . . . . ? N121 C126 C151 C152 -93.6(9) . . . . ? N121 C126 C151 C156 88.8(7) . . . . ? C156 C151 C152 C153 0.0 . . . . ? C126 C151 C152 C153 -177.6(6) . . . . ? C151 C152 C153 C154 0.0 . . . . ? C152 C153 C154 C155 0.0 . . . . ? C152 C153 C154 C171 178.1(6) . . . . ? C153 C154 C155 C156 0.0 . . . . ? C171 C154 C155 C156 -177.9(6) . . . . ? C154 C155 C156 C151 0.0 . . . . ? C152 C151 C156 C155 0.0 . . . . ? C126 C151 C156 C155 177.5(7) . . . . ? N141 C146 C161 C162 -167.3(9) . . . . ? N141 C146 C161 C166 13.3(17) . . . . ? C166 C161 C162 C163 0.0 . . . . ? C146 C161 C162 C163 -179.4(9) . . . . ? C161 C162 C163 C164 0.0 . . . . ? C162 C163 C164 C165 0.0 . . . . ? C162 C163 C164 C171 168.5(5) . . . . ? C163 C164 C165 C166 0.0 . . . . ? C171 C164 C165 C166 -168.2(5) . . . . ? C164 C165 C166 C161 0.0 . . . . ? C162 C161 C166 C165 0.0 . . . . ? C146 C161 C166 C165 179.4(10) . . . . ? C155 C154 C171 O172 129.5(10) . . . . ? C153 C154 C171 O172 -48.5(13) . . . . ? C155 C154 C171 C164 -48.8(10) . . . . ? C153 C154 C171 C164 133.2(6) . . . . ? C163 C164 C171 O172 -17.7(11) . . . . ? C165 C164 C171 O172 150.8(8) . . . . ? C163 C164 C171 C154 160.8(6) . . . . ? C165 C164 C171 C154 -30.8(10) . . . . ? N111 Ag1 N211 C212 135.8(11) . . . . ? N222 Ag1 N211 C212 13.9(5) . . . . ? N122 Ag1 N211 C212 -110.7(5) . . . . ? Ag2 Ag1 N211 C212 128.3(5) 6_565 . . . ? N111 Ag1 N211 C216 -61.2(13) . . . . ? N222 Ag1 N211 C216 177.0(6) . . . . ? N122 Ag1 N211 C216 52.3(6) . . . . ? Ag2 Ag1 N211 C216 -68.7(5) 6_565 . . . ? C216 N211 C212 C223 179.0(11) . . . . ? Ag1 N211 C212 C223 -17.7(10) . . . . ? C216 N211 C212 C213 0.0 . . . . ? Ag1 N211 C212 C213 163.4(6) . . . . ? C223 C212 C213 C214 -179.0(11) . . . . ? N211 C212 C213 C214 0.0 . . . . ? C212 C213 C214 C215 0.0 . . . . ? C213 C214 C215 C216 0.0 . . . . ? C214 C215 C216 N211 0.0 . . . . ? C212 N211 C216 C215 0.0 . . . . ? Ag1 N211 C216 C215 -162.3(7) . . . . ? C226 N221 N222 C223 179.3(11) . . . . ? C225 N221 N222 C223 0.0 . . . . ? C226 N221 N222 Ag1 -13.2(13) . . . . ? C225 N221 N222 Ag1 167.6(9) . . . . ? N211 Ag1 N222 C223 -9.7(5) . . . . ? N111 Ag1 N222 C223 -177.5(5) . . . . ? N122 Ag1 N222 C223 94.4(6) . . . . ? Ag2 Ag1 N222 C223 -82.8(5) 6_565 . . . ? N211 Ag1 N222 N221 -176.7(8) . . . . ? N111 Ag1 N222 N221 15.4(9) . . . . ? N122 Ag1 N222 N221 -72.7(8) . . . . ? Ag2 Ag1 N222 N221 110.1(7) 6_565 . . . ? C213 C212 C223 C224 1.2(14) . . . . ? N211 C212 C223 C224 -177.7(8) . . . . ? C213 C212 C223 N222 -172.6(6) . . . . ? N211 C212 C223 N222 8.5(12) . . . . ? N221 N222 C223 C212 175.3(11) . . . . ? Ag1 N222 C223 C212 4.5(10) . . . . ? N221 N222 C223 C224 0.0 . . . . ? Ag1 N222 C223 C224 -170.8(7) . . . . ? C212 C223 C224 C225 -174.2(13) . . . . ? N222 C223 C224 C225 0.0 . . . . ? C223 C224 C225 N221 0.0 . . . . ? C226 N221 C225 C224 -179.1(13) . . . . ? N222 N221 C225 C224 0.0 . . . . ? N222 N221 C226 C251 71.7(11) . . . . ? C225 N221 C226 C251 -109.3(11) . . . . ? N142 Ag2 N231 C232 -131.2(5) . . . . ? N242 Ag2 N231 C232 0.7(5) . . . . ? N131 Ag2 N231 C232 96.8(8) . . . . ? Ag1 Ag2 N231 C232 123.1(5) 2_654 . . . ? N142 Ag2 N231 C236 38.2(6) . . . . ? N242 Ag2 N231 C236 170.1(6) . . . . ? N131 Ag2 N231 C236 -93.8(8) . . . . ? Ag1 Ag2 N231 C236 -67.5(5) 2_654 . . . ? C236 N231 C232 C243 -177.6(9) . . . . ? Ag2 N231 C232 C243 -8.0(9) . . . . ? C236 N231 C232 C233 0.0 . . . . ? Ag2 N231 C232 C233 169.6(6) . . . . ? C243 C232 C233 C234 177.5(9) . . . . ? N231 C232 C233 C234 0.0 . . . . ? C232 C233 C234 C235 0.0 . . . . ? C233 C234 C235 C236 0.0 . . . . ? C234 C235 C236 N231 0.0 . . . . ? C232 N231 C236 C235 0.0 . . . . ? Ag2 N231 C236 C235 -169.1(6) . . . . ? C246 N241 N242 C243 -179.4(10) . . . . ? C245 N241 N242 C243 0.0 . . . . ? C246 N241 N242 Ag2 22.0(11) . . . . ? C245 N241 N242 Ag2 -158.7(7) . . . . ? N231 Ag2 N242 C243 6.0(4) . . . . ? N142 Ag2 N242 C243 127.4(5) . . . . ? N131 Ag2 N242 C243 -151.1(4) . . . . ? Ag1 Ag2 N242 C243 -66.0(4) 2_654 . . . ? N231 Ag2 N242 N241 163.9(6) . . . . ? N142 Ag2 N242 N241 -74.7(7) . . . . ? N131 Ag2 N242 N241 6.8(6) . . . . ? Ag1 Ag2 N242 N241 91.9(6) 2_654 . . . ? N231 C232 C243 N242 13.9(10) . . . . ? C233 C232 C243 N242 -163.6(6) . . . . ? N231 C232 C243 C244 -161.6(7) . . . . ? C233 C232 C243 C244 20.8(11) . . . . ? N241 N242 C243 C232 -176.7(9) . . . . ? Ag2 N242 C243 C232 -12.6(8) . . . . ? N241 N242 C243 C244 0.0 . . . . ? Ag2 N242 C243 C244 164.1(5) . . . . ? C232 C243 C244 C245 175.9(11) . . . . ? N242 C243 C244 C245 0.0 . . . . ? C246 N241 C245 C244 179.3(10) . . . . ? N242 N241 C245 C244 0.0 . . . . ? C243 C244 C245 N241 0.0 . . . . ? N242 N241 C246 C261 67.6(12) . . . . ? C245 N241 C246 C261 -111.6(9) . . . . ? N221 C226 C251 C252 -168.0(7) . . . . ? N221 C226 C251 C256 12.5(11) . . . . ? C256 C251 C252 C253 0.0 . . . . ? C226 C251 C252 C253 -179.6(6) . . . . ? C251 C252 C253 C254 0.0 . . . . ? C252 C253 C254 C255 0.0 . . . . ? C252 C253 C254 C271 168.4(7) . . . . ? C253 C254 C255 C256 0.0 . . . . ? C271 C254 C255 C256 -168.3(7) . . . . ? C254 C255 C256 C251 0.0 . . . . ? C252 C251 C256 C255 0.0 . . . . ? C226 C251 C256 C255 179.5(6) . . . . ? N241 C246 C261 C266 85.9(9) . . . . ? N241 C246 C261 C262 -95.9(10) . . . . ? C266 C261 C262 C263 0.0 . . . . ? C246 C261 C262 C263 -178.2(6) . . . . ? C261 C262 C263 C264 0.0 . . . . ? C262 C263 C264 C265 0.0 . . . . ? C262 C263 C264 C271 176.5(8) . . . . ? C263 C264 C265 C266 0.0 . . . . ? C271 C264 C265 C266 -176.3(8) . . . . ? C264 C265 C266 C261 0.0 . . . . ? C262 C261 C266 C265 0.0 . . . . ? C246 C261 C266 C265 178.2(6) . . . . ? C255 C254 C271 O272 148.2(11) . . . . ? C253 C254 C271 O272 -20.1(16) . . . . ? C255 C254 C271 C264 -36.3(13) . . . . ? C253 C254 C271 C264 155.3(7) . . . . ? C263 C264 C271 O272 -38.2(17) . . . . ? C265 C264 C271 O272 138.2(13) . . . . ? C263 C264 C271 C254 146.8(8) . . . . ? C265 C264 C271 C254 -36.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.531 _refine_diff_density_min -2.295 _refine_diff_density_rms 0.193 #===END data_imw1601pbcn _database_code_depnum_ccdc_archive 'CCDC 862640' #TrackingRef '- helix_of_helicates.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H24 N6 O' _chemical_formula_sum 'C31 H24 N6 O' _chemical_formula_weight 496.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbcn ' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.5827(3) _cell_length_b 13.3565(5) _cell_length_c 21.0613(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2414.36(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3278 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 26.82 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9745 _exptl_absorpt_correction_T_max 0.9829 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19035 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.58 _reflns_number_total 2792 _reflns_number_gt 2016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. A small number of gentle restraints were used to keep all thermal parameters in line. Hydrogens were added in calculated positions. 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^)+(0.0901P)^2^+0.8238P] 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 2792 _refine_ls_number_parameters 173 _refine_ls_number_restraints 183 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.066 _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 N11 N 0.2511(2) 0.09398(15) 0.62748(8) 0.0405(5) Uani 1 1 d U . . C12 C 0.2544(2) 0.05878(15) 0.56777(9) 0.0301(4) Uani 1 1 d U . . C13 C 0.1572(3) -0.01766(16) 0.54766(10) 0.0387(5) Uani 1 1 d U . . H13 H 0.1633 -0.0423 0.5054 0.046 Uiso 1 1 calc R . . C14 C 0.0502(3) -0.05794(17) 0.59057(11) 0.0435(6) Uani 1 1 d U . . H14 H -0.0196 -0.1092 0.5776 0.052 Uiso 1 1 calc R . . C15 C 0.0472(3) -0.02272(17) 0.65144(11) 0.0402(5) Uani 1 1 d U . . H15 H -0.0243 -0.0490 0.6816 0.048 Uiso 1 1 calc R . . C16 C 0.1502(3) 0.05179(19) 0.66802(11) 0.0445(6) Uani 1 1 d U . . H16 H 0.1498 0.0747 0.7107 0.053 Uiso 1 1 calc R . . N21 N 0.47903(18) 0.14904(12) 0.43848(8) 0.0307(4) Uani 1 1 d U . . N22 N 0.36294(19) 0.09075(12) 0.46153(7) 0.0298(4) Uani 1 1 d U . . C23 C 0.3642(2) 0.10884(15) 0.52428(9) 0.0293(4) Uani 1 1 d U . . C24 C 0.4785(2) 0.17937(17) 0.54057(10) 0.0365(5) Uani 1 1 d U . . H24 H 0.5016 0.2050 0.5816 0.044 Uiso 1 1 calc R . . C25 C 0.5493(2) 0.20309(17) 0.48435(10) 0.0369(5) Uani 1 1 d U . . H25 H 0.6325 0.2491 0.4787 0.044 Uiso 1 1 calc R . . C26 C 0.5031(2) 0.15626(16) 0.37027(9) 0.0333(5) Uani 1 1 d U . . H26A H 0.5082 0.0881 0.3519 0.040 Uiso 1 1 calc R . . H26B H 0.6039 0.1898 0.3619 0.040 Uiso 1 1 calc R . . C31 C 0.1295(2) 0.32036(14) 0.28043(8) 0.0252(4) Uani 1 1 d U . . C32 C 0.1794(2) 0.22853(14) 0.25608(9) 0.0262(4) Uani 1 1 d U . . H32 H 0.1294 0.2012 0.2198 0.031 Uiso 1 1 calc R . . C33 C 0.3012(2) 0.17679(14) 0.28446(9) 0.0274(4) Uani 1 1 d U . . H33 H 0.3356 0.1151 0.2668 0.033 Uiso 1 1 calc R . . C34 C 0.3731(2) 0.21458(15) 0.33835(9) 0.0284(4) Uani 1 1 d U . . C35 C 0.3255(2) 0.30752(16) 0.36185(9) 0.0322(5) Uani 1 1 d U . . H35 H 0.3755 0.3348 0.3982 0.039 Uiso 1 1 calc R . . C36 C 0.2064(2) 0.36035(14) 0.33286(9) 0.0302(4) Uani 1 1 d U . . H36 H 0.1769 0.4241 0.3488 0.036 Uiso 1 1 calc R . . C41 C 0.0000 0.3777(2) 0.2500 0.0257(5) Uani 1 2 d SU . . O42 O 0.0000 0.46878(14) 0.2500 0.0336(5) Uani 1 2 d SU . . 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 N11 0.0400(10) 0.0464(11) 0.0351(9) -0.0012(8) -0.0005(8) -0.0126(8) C12 0.0292(9) 0.0248(10) 0.0362(10) 0.0052(8) -0.0059(8) 0.0028(8) C13 0.0449(12) 0.0290(11) 0.0422(11) 0.0000(9) -0.0058(9) -0.0029(10) C14 0.0459(12) 0.0296(12) 0.0551(13) 0.0044(10) -0.0062(10) -0.0099(10) C15 0.0366(11) 0.0381(12) 0.0461(12) 0.0131(10) -0.0010(9) -0.0026(10) C16 0.0436(12) 0.0533(15) 0.0366(11) 0.0022(10) -0.0009(9) -0.0106(11) N21 0.0255(8) 0.0323(9) 0.0344(9) 0.0036(7) -0.0029(6) 0.0026(7) N22 0.0274(8) 0.0274(9) 0.0346(9) 0.0025(7) -0.0030(6) 0.0030(7) C23 0.0270(9) 0.0261(10) 0.0347(10) 0.0006(8) -0.0059(7) 0.0044(8) C24 0.0351(10) 0.0377(12) 0.0366(11) 0.0010(9) -0.0075(8) -0.0047(9) C25 0.0296(10) 0.0372(12) 0.0438(11) 0.0026(9) -0.0061(9) -0.0065(9) C26 0.0275(9) 0.0381(12) 0.0344(10) 0.0031(9) 0.0023(8) 0.0063(9) C31 0.0243(8) 0.0214(9) 0.0297(9) 0.0027(7) 0.0016(7) -0.0004(7) C32 0.0241(9) 0.0238(9) 0.0307(9) -0.0017(7) 0.0035(7) -0.0021(7) C33 0.0246(9) 0.0236(9) 0.0340(9) -0.0021(8) 0.0052(7) 0.0024(8) C34 0.0245(9) 0.0291(10) 0.0315(9) 0.0034(7) 0.0043(7) 0.0030(8) C35 0.0331(10) 0.0334(11) 0.0301(10) -0.0033(8) -0.0029(8) 0.0019(9) C36 0.0334(9) 0.0239(10) 0.0335(10) -0.0044(8) -0.0002(8) 0.0041(8) C41 0.0264(12) 0.0233(13) 0.0275(12) 0.000 0.0027(10) 0.000 O42 0.0359(10) 0.0177(10) 0.0472(12) 0.000 -0.0062(9) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N11 C16 1.340(3) . ? N11 C12 1.343(3) . ? C12 C13 1.385(3) . ? C12 C23 1.475(3) . ? C13 C14 1.396(3) . ? C13 H13 0.9500 . ? C14 C15 1.366(3) . ? C14 H14 0.9500 . ? C15 C16 1.376(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C25 1.348(3) . ? N21 N22 1.355(2) . ? N21 C26 1.455(2) . ? N22 C23 1.343(2) . ? C23 C24 1.402(3) . ? C24 C25 1.368(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C34 1.518(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C36 1.393(3) . ? C31 C32 1.397(3) . ? C31 C41 1.494(2) . ? C32 C33 1.389(3) . ? C32 H32 0.9500 . ? C33 C34 1.387(3) . ? C33 H33 0.9500 . ? C34 C35 1.397(3) . ? C35 C36 1.384(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 O42 1.216(3) . ? C41 C31 1.494(2) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 N11 C12 117.60(19) . . ? N11 C12 C13 122.12(19) . . ? N11 C12 C23 115.89(18) . . ? C13 C12 C23 121.96(18) . . ? C12 C13 C14 118.8(2) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 119.2(2) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 118.3(2) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? N11 C16 C15 123.9(2) . . ? N11 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? C25 N21 N22 112.32(16) . . ? C25 N21 C26 127.48(17) . . ? N22 N21 C26 119.79(16) . . ? C23 N22 N21 104.07(16) . . ? N22 C23 C24 111.55(18) . . ? N22 C23 C12 121.61(17) . . ? C24 C23 C12 126.84(18) . . ? C25 C24 C23 104.74(18) . . ? C25 C24 H24 127.6 . . ? C23 C24 H24 127.6 . . ? N21 C25 C24 107.31(18) . . ? N21 C25 H25 126.3 . . ? C24 C25 H25 126.3 . . ? N21 C26 C34 111.51(16) . . ? N21 C26 H26A 109.3 . . ? C34 C26 H26A 109.3 . . ? N21 C26 H26B 109.3 . . ? C34 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C36 C31 C32 118.85(17) . . ? C36 C31 C41 119.73(17) . . ? C32 C31 C41 121.38(17) . . ? C33 C32 C31 120.65(17) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 120.39(17) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 118.90(17) . . ? C33 C34 C26 120.17(17) . . ? C35 C34 C26 120.92(18) . . ? C36 C35 C34 120.83(17) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C31 120.28(17) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? O42 C41 C31 120.84(12) . 3 ? O42 C41 C31 120.84(12) . . ? C31 C41 C31 118.3(2) 3 . ? 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 C16 N11 C12 C13 0.6(3) . . . . ? C16 N11 C12 C23 178.59(19) . . . . ? N11 C12 C13 C14 1.3(3) . . . . ? C23 C12 C13 C14 -176.57(19) . . . . ? C12 C13 C14 C15 -1.7(3) . . . . ? C13 C14 C15 C16 0.2(3) . . . . ? C12 N11 C16 C15 -2.2(4) . . . . ? C14 C15 C16 N11 1.9(4) . . . . ? C25 N21 N22 C23 -1.0(2) . . . . ? C26 N21 N22 C23 -174.24(17) . . . . ? N21 N22 C23 C24 1.1(2) . . . . ? N21 N22 C23 C12 -179.60(16) . . . . ? N11 C12 C23 N22 -170.25(18) . . . . ? C13 C12 C23 N22 7.8(3) . . . . ? N11 C12 C23 C24 9.0(3) . . . . ? C13 C12 C23 C24 -173.0(2) . . . . ? N22 C23 C24 C25 -0.7(2) . . . . ? C12 C23 C24 C25 179.97(19) . . . . ? N22 N21 C25 C24 0.6(2) . . . . ? C26 N21 C25 C24 173.19(19) . . . . ? C23 C24 C25 N21 0.1(2) . . . . ? C25 N21 C26 C34 -101.6(2) . . . . ? N22 N21 C26 C34 70.5(2) . . . . ? C36 C31 C32 C33 1.4(3) . . . . ? C41 C31 C32 C33 179.17(15) . . . . ? C31 C32 C33 C34 1.4(3) . . . . ? C32 C33 C34 C35 -2.8(3) . . . . ? C32 C33 C34 C26 178.25(17) . . . . ? N21 C26 C34 C33 -131.86(19) . . . . ? N21 C26 C34 C35 49.3(3) . . . . ? C33 C34 C35 C36 1.4(3) . . . . ? C26 C34 C35 C36 -179.69(17) . . . . ? C34 C35 C36 C31 1.5(3) . . . . ? C32 C31 C36 C35 -2.9(3) . . . . ? C41 C31 C36 C35 179.36(16) . . . . ? C36 C31 C41 O42 31.22(18) . . . . ? C32 C31 C41 O42 -146.50(13) . . . . ? C36 C31 C41 C31 -148.78(18) . . . 3 ? C32 C31 C41 C31 33.50(13) . . . 3 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.296 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.079 #===END