# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (C2H8N)2(Cd3(C21H9O6)2.67)(C3H8NO)6.67(H2O)4 _chemical_formula_sum C80H101.33N8.67O26.67Cd3 _chemical_formula_weight 1948.2693 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 26.5879(6) _cell_length_b 26.5879(6) _cell_length_c 67.331(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 41221(3) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11376 _exptl_absorpt_coefficient_mu 5.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2553 _exptl_absorpt_correction_T_max 0.4730 _exptl_absorpt_process_details 'SADABS (SHELDRICK,1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 49367 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -74 _diffrn_reflns_limit_l_max 78 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 65.34 _reflns_number_total 7756 _reflns_number_gt 6155 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _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^)+(0.0791P)^2^+363.2252P] 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 7756 _refine_ls_number_parameters 340 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1775 _refine_ls_wR_factor_gt 0.1709 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.007 _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 Cd2 Cd 0.81427(2) 0.67095(2) 0.614262(8) 0.05249(19) Uani 1 1 d . . . O2 O 0.7482(2) 0.6441(3) 0.58810(8) 0.0646(14) Uani 1 1 d . . . O1 O 0.8310(2) 0.6488(3) 0.58233(9) 0.092(2) Uani 1 1 d . . . C1 C 0.7821(3) 0.6388(3) 0.57691(12) 0.0575(19) Uani 1 1 d . . . C4 C 0.7944(2) 0.6064(3) 0.52235(9) 0.0385(14) Uani 1 1 d . . . C3 C 0.8077(3) 0.6238(3) 0.54210(10) 0.0483(17) Uani 1 1 d . . . H3 H 0.8455 0.6377 0.5466 0.058 Uiso 1 1 calc R . . C21 C 0.7099(3) 0.6011(3) 0.54897(10) 0.0456(16) Uani 1 1 d . . . H21 H 0.6816 0.5983 0.5577 0.055 Uiso 1 1 calc R . . C20 C 0.6965(3) 0.5850(3) 0.52916(10) 0.0440(15) Uani 1 1 d . . . H20 H 0.6589 0.5727 0.5248 0.053 Uiso 1 1 calc R . . C2 C 0.7657(3) 0.6210(3) 0.55533(11) 0.0497(17) Uani 1 1 d . . . C5 C 0.8367(3) 0.6043(3) 0.50927(11) 0.0455(16) Uani 1 1 d . . . C11 C 0.8202(3) 0.5813(3) 0.49034(9) 0.0436(15) Uani 1 1 d . . . C18 C 0.7213(3) 0.5677(3) 0.49536(8) 0.0358(13) Uani 1 1 d . . . C17 C 0.6660(3) 0.5512(3) 0.48792(9) 0.0418(14) Uani 1 1 d . . . H17 H 0.6389 0.5530 0.4962 0.050 Uiso 1 1 calc R . . C19 C 0.7370(3) 0.5864(3) 0.51563(9) 0.0369(13) Uani 1 1 d . . . C12 C 0.7623(3) 0.5638(3) 0.48244(9) 0.0437(15) Uani 1 1 d . . . C10 C 0.8585(3) 0.5715(3) 0.47858(11) 0.0490(16) Uani 1 1 d . . . H10 H 0.8477 0.5566 0.4658 0.059 Uiso 1 1 calc R . . C15 C 0.6505(3) 0.5320(3) 0.46818(9) 0.0499(17) Uani 1 1 d . . . C13 C 0.7454(3) 0.5454(4) 0.46269(11) 0.070(2) Uani 1 1 d . . . H13 H 0.7718 0.5440 0.4540 0.084 Uiso 1 1 calc R . . C14 C 0.6909(3) 0.5296(5) 0.45614(11) 0.073(3) Uani 1 1 d . . . H14 H 0.6808 0.5167 0.4431 0.088 Uiso 1 1 calc R . . C8 C 0.9125(3) 0.5840(3) 0.48607(10) 0.0450(16) Uani 1 1 d . . . C7 C 0.9299(3) 0.6100(3) 0.50445(11) 0.0543(18) Uani 1 1 d . . . H7 H 0.9666 0.6202 0.5093 0.065 Uiso 1 1 calc R . . C6 C 0.8933(3) 0.6206(3) 0.51559(12) 0.0548(19) Uani 1 1 d . . . H6 H 0.9062 0.6393 0.5278 0.066 Uiso 1 1 calc R . . Cd1 Cd 0.8333 0.6667 0.6667 0.0446(2) Uani 1 2 d S . . O7 O 0.7801(4) 0.5803(3) 0.62259(12) 0.103(2) Uani 1 1 d U . . C22 C 0.7845(3) 0.5573(3) 0.63823(16) 0.071(3) Uani 1 1 d . . . C9 C 0.9486(3) 0.5662(3) 0.47427(12) 0.0515(18) Uani 1 1 d . . . O8 O 0.8005(3) 0.5784(3) 0.65507(10) 0.0829(18) Uani 1 1 d U . . C16 C 0.5905(3) 0.5135(4) 0.46094(11) 0.0532(18) Uani 1 1 d . . . C23 C 0.7646(3) 0.4935(3) 0.63745(13) 0.0598(19) Uani 1 1 d U . . O6 O 0.5563(2) 0.5211(2) 0.47182(7) 0.0535(12) Uani 1 1 d . . . O3 O 0.99298(17) 0.56943(19) 0.48175(7) 0.0487(11) Uani 1 1 d . . . O4 O 0.9335(2) 0.5499(3) 0.45627(8) 0.0689(16) Uani 1 1 d . . . O5 O 0.5764(2) 0.4908(3) 0.44403(8) 0.0756(17) Uani 1 1 d . . . C25 C 0.6864(3) 0.3932(3) 0.63625(13) 0.0584(19) Uani 1 1 d U . . C26 C 0.7263(3) 0.3744(3) 0.63577(12) 0.0571(18) Uani 1 1 d U . . C24 C 0.7070(4) 0.4540(3) 0.63664(14) 0.067(2) Uani 1 1 d U . . H24 H 0.6804 0.4670 0.6363 0.080 Uiso 1 1 calc R . . C27 C 0.7857(5) 0.4150(5) 0.6371(2) 0.103(3) Uani 1 1 d U . . H27 H 0.8128 0.4026 0.6375 0.123 Uiso 1 1 calc R . . C28 C 0.8041(6) 0.4747(5) 0.6378(2) 0.112(4) Uani 1 1 d U . . H28 H 0.8435 0.5017 0.6385 0.134 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 Cd2 0.0519(3) 0.0434(3) 0.0561(3) -0.0288(2) -0.0184(2) 0.0193(2) O2 0.053(3) 0.088(4) 0.051(3) -0.026(3) -0.005(2) 0.033(3) O1 0.049(3) 0.154(6) 0.075(4) -0.062(4) -0.031(3) 0.052(4) C1 0.050(4) 0.047(4) 0.067(5) -0.025(4) -0.003(4) 0.018(3) C4 0.028(3) 0.042(3) 0.049(4) -0.009(3) -0.002(3) 0.020(3) C3 0.031(3) 0.058(4) 0.050(4) -0.030(3) -0.010(3) 0.017(3) C21 0.038(3) 0.060(4) 0.042(4) -0.022(3) -0.007(3) 0.027(3) C20 0.028(3) 0.055(4) 0.054(4) -0.011(3) -0.008(3) 0.024(3) C2 0.032(3) 0.050(4) 0.061(4) -0.023(3) -0.013(3) 0.016(3) C5 0.026(3) 0.037(3) 0.067(4) -0.011(3) -0.002(3) 0.011(3) C11 0.039(3) 0.060(4) 0.037(3) 0.002(3) -0.002(3) 0.029(3) C18 0.038(3) 0.050(4) 0.024(3) 0.005(2) 0.001(2) 0.026(3) C17 0.038(3) 0.054(4) 0.042(4) 0.007(3) -0.001(3) 0.029(3) C19 0.037(3) 0.037(3) 0.040(3) -0.003(3) -0.001(3) 0.021(3) C12 0.038(3) 0.070(4) 0.031(3) 0.003(3) 0.006(3) 0.033(3) C10 0.034(3) 0.066(4) 0.048(4) 0.002(3) 0.006(3) 0.025(3) C15 0.041(4) 0.086(5) 0.033(3) 0.001(3) -0.006(3) 0.039(4) C13 0.052(4) 0.131(8) 0.038(4) 0.000(4) 0.009(3) 0.054(5) C14 0.059(5) 0.140(8) 0.037(4) -0.009(5) -0.007(3) 0.062(6) C8 0.028(3) 0.058(4) 0.046(4) 0.011(3) 0.015(3) 0.019(3) C7 0.028(3) 0.069(5) 0.059(4) -0.014(4) -0.004(3) 0.020(3) C6 0.035(3) 0.065(5) 0.063(5) -0.022(4) 0.001(3) 0.024(3) Cd1 0.0469(4) 0.0260(3) 0.0499(4) -0.0091(3) 0.0003(3) 0.0099(3) O7 0.134(5) 0.070(3) 0.099(4) -0.028(3) -0.019(3) 0.046(3) C22 0.048(4) 0.034(4) 0.108(7) -0.049(5) -0.011(4) 0.003(3) C9 0.030(3) 0.051(4) 0.072(5) 0.005(4) 0.023(3) 0.019(3) O8 0.097(4) 0.054(3) 0.091(3) -0.007(3) -0.001(3) 0.033(3) C16 0.053(4) 0.074(5) 0.045(4) 0.008(4) -0.003(3) 0.041(4) C23 0.051(3) 0.044(3) 0.087(4) -0.012(3) -0.010(3) 0.026(3) O6 0.044(3) 0.081(3) 0.046(3) 0.005(2) -0.005(2) 0.040(3) O3 0.024(2) 0.046(3) 0.070(3) 0.010(2) 0.013(2) 0.0131(19) O4 0.055(3) 0.114(5) 0.050(3) 0.013(3) 0.022(3) 0.051(3) O5 0.066(3) 0.129(5) 0.052(3) -0.014(3) -0.014(3) 0.063(4) C25 0.050(3) 0.047(3) 0.083(4) -0.007(3) -0.003(3) 0.029(3) C26 0.045(3) 0.047(3) 0.082(4) -0.005(3) -0.011(3) 0.026(3) C24 0.062(4) 0.052(3) 0.094(4) -0.012(3) 0.009(3) 0.035(3) C27 0.088(5) 0.090(5) 0.147(6) -0.002(4) -0.014(4) 0.057(4) C28 0.097(5) 0.097(5) 0.149(6) -0.003(4) -0.008(4) 0.054(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd2 O7 2.181(8) . ? Cd2 O4 2.260(5) 34_665 ? Cd2 O1 2.331(6) . ? Cd2 O2 2.333(5) . ? Cd2 O5 2.385(5) 36 ? Cd2 O6 2.389(5) 36 ? Cd2 C1 2.656(8) . ? Cd2 C16 2.719(7) 36 ? O2 C1 1.235(9) . ? O1 C1 1.246(9) . ? C1 C2 1.523(10) . ? C4 C3 1.395(9) . ? C4 C19 1.416(8) . ? C4 C5 1.452(9) . ? C3 C2 1.402(9) . ? C3 H3 0.9300 . ? C21 C2 1.370(9) . ? C21 C20 1.392(9) . ? C21 H21 0.9300 . ? C20 C19 1.396(9) . ? C20 H20 0.9300 . ? C5 C11 1.387(9) . ? C5 C6 1.408(9) . ? C11 C10 1.413(9) . ? C11 C12 1.466(9) . ? C18 C17 1.401(8) . ? C18 C12 1.439(8) . ? C18 C19 1.441(8) . ? C17 C15 1.409(9) . ? C17 H17 0.9300 . ? C12 C13 1.411(10) . ? C10 C8 1.396(9) . ? C10 H10 0.9300 . ? C15 C14 1.373(10) . ? C15 C16 1.497(9) . ? C13 C14 1.363(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C8 C7 1.379(10) . ? C8 C9 1.495(9) . ? C7 C6 1.366(9) . ? C7 H7 0.9300 . ? C6 H6 0.9300 . ? Cd1 O8 2.197(6) . ? Cd1 O8 2.197(6) 25_666 ? Cd1 O3 2.302(5) 16_545 ? Cd1 O3 2.302(5) 34_665 ? Cd1 O6 2.306(5) 18_655 ? Cd1 O6 2.307(5) 36 ? O7 C22 1.252(12) . ? C22 O8 1.242(10) . ? C22 C23 1.506(10) . ? C9 O3 1.245(9) . ? C9 O4 1.282(9) . ? C16 O5 1.254(9) . ? C16 O6 1.258(8) . ? C16 Cd2 2.719(7) 30_455 ? C23 C24 1.357(11) . ? C23 C28 1.368(13) . ? O6 Cd1 2.306(5) 18_655 ? O6 Cd2 2.389(5) 30_455 ? O3 Cd1 2.302(5) 16_545 ? O4 Cd2 2.260(5) 28_665 ? O5 Cd2 2.385(5) 30_455 ? C25 C26 1.382(10) . ? C25 C24 1.423(10) . ? C25 C26 1.430(10) 2_655 ? C26 C27 1.402(13) . ? C26 C25 1.430(10) 3_665 ? C24 H24 0.9300 . ? C27 C28 1.410(15) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Cd2 O4 129.7(3) . 34_665 ? O7 Cd2 O1 89.1(3) . . ? O4 Cd2 O1 127.5(2) 34_665 . ? O7 Cd2 O2 91.3(3) . . ? O4 Cd2 O2 85.7(2) 34_665 . ? O1 Cd2 O2 55.68(18) . . ? O7 Cd2 O5 133.9(3) . 36 ? O4 Cd2 O5 88.5(2) 34_665 36 ? O1 Cd2 O5 83.4(2) . 36 ? O2 Cd2 O5 119.9(2) . 36 ? O7 Cd2 O6 91.1(2) . 36 ? O4 Cd2 O6 96.93(19) 34_665 36 ? O1 Cd2 O6 118.89(18) . 36 ? O2 Cd2 O6 174.03(17) . 36 ? O5 Cd2 O6 55.01(17) 36 36 ? O7 Cd2 C1 89.9(3) . . ? O4 Cd2 C1 107.7(2) 34_665 . ? O1 Cd2 C1 28.0(2) . . ? O2 Cd2 C1 27.7(2) . . ? O5 Cd2 C1 102.8(2) 36 . ? O6 Cd2 C1 146.8(2) 36 . ? O7 Cd2 C16 114.0(3) . 36 ? O4 Cd2 C16 92.7(2) 34_665 36 ? O1 Cd2 C16 102.2(2) . 36 ? O2 Cd2 C16 147.3(2) . 36 ? O5 Cd2 C16 27.5(2) 36 36 ? O6 Cd2 C16 27.56(19) 36 36 ? C1 Cd2 C16 126.8(2) . 36 ? C1 O2 Cd2 90.8(5) . . ? C1 O1 Cd2 90.7(5) . . ? O2 C1 O1 122.7(7) . . ? O2 C1 C2 120.4(7) . . ? O1 C1 C2 116.8(7) . . ? O2 C1 Cd2 61.4(4) . . ? O1 C1 Cd2 61.3(4) . . ? C2 C1 Cd2 178.1(5) . . ? C3 C4 C19 118.5(5) . . ? C3 C4 C5 121.2(5) . . ? C19 C4 C5 120.2(6) . . ? C4 C3 C2 121.6(6) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C2 C21 C20 118.7(6) . . ? C2 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C20 C19 122.7(6) . . ? C21 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? C21 C2 C3 120.2(6) . . ? C21 C2 C1 120.3(6) . . ? C3 C2 C1 119.5(6) . . ? C11 C5 C6 117.9(6) . . ? C11 C5 C4 119.6(5) . . ? C6 C5 C4 122.3(6) . . ? C5 C11 C10 119.8(6) . . ? C5 C11 C12 121.6(6) . . ? C10 C11 C12 118.5(6) . . ? C17 C18 C12 118.4(5) . . ? C17 C18 C19 121.6(5) . . ? C12 C18 C19 120.0(5) . . ? C18 C17 C15 121.4(6) . . ? C18 C17 H17 119.3 . . ? C15 C17 H17 119.3 . . ? C20 C19 C4 118.3(6) . . ? C20 C19 C18 121.6(5) . . ? C4 C19 C18 120.2(5) . . ? C13 C12 C18 118.2(6) . . ? C13 C12 C11 123.7(6) . . ? C18 C12 C11 118.1(5) . . ? C8 C10 C11 120.2(6) . . ? C8 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C14 C15 C17 118.7(6) . . ? C14 C15 C16 121.5(6) . . ? C17 C15 C16 119.8(6) . . ? C14 C13 C12 121.2(6) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 122.0(7) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C7 C8 C10 119.5(6) . . ? C7 C8 C9 121.8(6) . . ? C10 C8 C9 118.6(6) . . ? C6 C7 C8 120.0(6) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C6 C5 122.2(7) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? O8 Cd1 O8 180.0(4) . 25_666 ? O8 Cd1 O3 90.5(2) . 16_545 ? O8 Cd1 O3 89.5(2) 25_666 16_545 ? O8 Cd1 O3 89.5(2) . 34_665 ? O8 Cd1 O3 90.5(2) 25_666 34_665 ? O3 Cd1 O3 179.990(3) 16_545 34_665 ? O8 Cd1 O6 91.6(2) . 18_655 ? O8 Cd1 O6 88.4(2) 25_666 18_655 ? O3 Cd1 O6 84.95(18) 16_545 18_655 ? O3 Cd1 O6 95.06(18) 34_665 18_655 ? O8 Cd1 O6 88.4(2) . 36 ? O8 Cd1 O6 91.6(2) 25_666 36 ? O3 Cd1 O6 95.05(18) 16_545 36 ? O3 Cd1 O6 84.94(18) 34_665 36 ? O6 Cd1 O6 179.99(13) 18_655 36 ? C22 O7 Cd2 131.8(6) . . ? O8 C22 O7 129.9(8) . . ? O8 C22 C23 112.9(9) . . ? O7 C22 C23 117.1(7) . . ? O3 C9 O4 122.2(6) . . ? O3 C9 C8 120.0(7) . . ? O4 C9 C8 117.8(6) . . ? C22 O8 Cd1 132.1(6) . . ? O5 C16 O6 122.7(7) . . ? O5 C16 C15 117.8(6) . . ? O6 C16 C15 119.5(6) . . ? O5 C16 Cd2 61.3(4) . 30_455 ? O6 C16 Cd2 61.4(4) . 30_455 ? C15 C16 Cd2 178.4(6) . 30_455 ? C24 C23 C28 119.5(8) . . ? C24 C23 C22 119.9(7) . . ? C28 C23 C22 120.6(8) . . ? C16 O6 Cd1 150.8(5) . 18_655 ? C16 O6 Cd2 91.0(4) . 30_455 ? Cd1 O6 Cd2 99.14(17) 18_655 30_455 ? C9 O3 Cd1 128.0(4) . 16_545 ? C9 O4 Cd2 101.7(4) . 28_665 ? C16 O5 Cd2 91.3(4) . 30_455 ? C26 C25 C24 118.7(7) . . ? C26 C25 C26 119.8(7) . 2_655 ? C24 C25 C26 121.4(7) . 2_655 ? C25 C26 C27 119.7(7) . . ? C25 C26 C25 120.1(7) . 3_665 ? C27 C26 C25 119.9(7) . 3_665 ? C23 C24 C25 121.6(7) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C28 C27 C26 119.4(10) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C23 C28 C27 120.9(11) . . ? C23 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? 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 O7 Cd2 O2 C1 -87.4(5) . . . . ? O4 Cd2 O2 C1 142.8(5) 34_665 . . . ? O1 Cd2 O2 C1 0.6(5) . . . . ? O5 Cd2 O2 C1 57.0(5) 36 . . . ? O6 Cd2 O2 C1 26(2) 36 . . . ? C16 Cd2 O2 C1 54.6(7) 36 . . . ? O7 Cd2 O1 C1 91.5(6) . . . . ? O4 Cd2 O1 C1 -51.0(6) 34_665 . . . ? O2 Cd2 O1 C1 -0.6(5) . . . . ? O5 Cd2 O1 C1 -134.0(6) 36 . . . ? O6 Cd2 O1 C1 -177.7(5) 36 . . . ? C16 Cd2 O1 C1 -154.1(5) 36 . . . ? Cd2 O2 C1 O1 -1.2(9) . . . . ? Cd2 O2 C1 C2 -179.4(6) . . . . ? Cd2 O1 C1 O2 1.2(9) . . . . ? Cd2 O1 C1 C2 179.5(6) . . . . ? O7 Cd2 C1 O2 92.9(5) . . . . ? O4 Cd2 C1 O2 -39.2(5) 34_665 . . . ? O1 Cd2 C1 O2 -178.9(8) . . . . ? O5 Cd2 C1 O2 -131.8(5) 36 . . . ? O6 Cd2 C1 O2 -175.2(4) 36 . . . ? C16 Cd2 C1 O2 -146.6(4) 36 . . . ? O7 Cd2 C1 O1 -88.2(6) . . . . ? O4 Cd2 C1 O1 139.7(6) 34_665 . . . ? O2 Cd2 C1 O1 178.9(8) . . . . ? O5 Cd2 C1 O1 47.1(6) 36 . . . ? O6 Cd2 C1 O1 3.7(8) 36 . . . ? C16 Cd2 C1 O1 32.3(7) 36 . . . ? O7 Cd2 C1 C2 -102(17) . . . . ? O4 Cd2 C1 C2 126(17) 34_665 . . . ? O1 Cd2 C1 C2 -14(17) . . . . ? O2 Cd2 C1 C2 165(17) . . . . ? O5 Cd2 C1 C2 33(17) 36 . . . ? O6 Cd2 C1 C2 -10(17) 36 . . . ? C16 Cd2 C1 C2 18(17) 36 . . . ? C19 C4 C3 C2 1.3(10) . . . . ? C5 C4 C3 C2 -174.1(7) . . . . ? C2 C21 C20 C19 2.2(11) . . . . ? C20 C21 C2 C3 -1.2(11) . . . . ? C20 C21 C2 C1 -179.7(7) . . . . ? C4 C3 C2 C21 -0.4(11) . . . . ? C4 C3 C2 C1 178.1(7) . . . . ? O2 C1 C2 C21 -11.3(11) . . . . ? O1 C1 C2 C21 170.3(8) . . . . ? Cd2 C1 C2 C21 -176(100) . . . . ? O2 C1 C2 C3 170.2(7) . . . . ? O1 C1 C2 C3 -8.2(11) . . . . ? Cd2 C1 C2 C3 5(17) . . . . ? C3 C4 C5 C11 173.6(7) . . . . ? C19 C4 C5 C11 -1.7(10) . . . . ? C3 C4 C5 C6 -1.2(11) . . . . ? C19 C4 C5 C6 -176.5(6) . . . . ? C6 C5 C11 C10 4.0(10) . . . . ? C4 C5 C11 C10 -171.0(6) . . . . ? C6 C5 C11 C12 -179.2(7) . . . . ? C4 C5 C11 C12 5.8(10) . . . . ? C12 C18 C17 C15 -1.0(10) . . . . ? C19 C18 C17 C15 -179.0(6) . . . . ? C21 C20 C19 C4 -1.3(10) . . . . ? C21 C20 C19 C18 177.9(6) . . . . ? C3 C4 C19 C20 -0.4(9) . . . . ? C5 C4 C19 C20 175.1(6) . . . . ? C3 C4 C19 C18 -179.6(6) . . . . ? C5 C4 C19 C18 -4.2(9) . . . . ? C17 C18 C19 C20 4.8(9) . . . . ? C12 C18 C19 C20 -173.1(6) . . . . ? C17 C18 C19 C4 -175.9(6) . . . . ? C12 C18 C19 C4 6.1(9) . . . . ? C17 C18 C12 C13 2.1(10) . . . . ? C19 C18 C12 C13 -179.9(7) . . . . ? C17 C18 C12 C11 179.8(6) . . . . ? C19 C18 C12 C11 -2.1(9) . . . . ? C5 C11 C12 C13 173.7(8) . . . . ? C10 C11 C12 C13 -9.4(11) . . . . ? C5 C11 C12 C18 -3.9(10) . . . . ? C10 C11 C12 C18 173.0(6) . . . . ? C5 C11 C10 C8 1.1(11) . . . . ? C12 C11 C10 C8 -175.8(6) . . . . ? C18 C17 C15 C14 0.1(11) . . . . ? C18 C17 C15 C16 178.5(6) . . . . ? C18 C12 C13 C14 -2.4(13) . . . . ? C11 C12 C13 C14 180.0(8) . . . . ? C12 C13 C14 C15 1.6(16) . . . . ? C17 C15 C14 C13 -0.4(14) . . . . ? C16 C15 C14 C13 -178.8(9) . . . . ? C11 C10 C8 C7 -4.7(11) . . . . ? C11 C10 C8 C9 172.4(6) . . . . ? C10 C8 C7 C6 3.1(11) . . . . ? C9 C8 C7 C6 -173.9(7) . . . . ? C8 C7 C6 C5 2.1(12) . . . . ? C11 C5 C6 C7 -5.7(12) . . . . ? C4 C5 C6 C7 169.1(7) . . . . ? O4 Cd2 O7 C22 -77.0(10) 34_665 . . . ? O1 Cd2 O7 C22 141.9(10) . . . . ? O2 Cd2 O7 C22 -162.5(10) . . . . ? O5 Cd2 O7 C22 62.0(11) 36 . . . ? O6 Cd2 O7 C22 23.0(10) 36 . . . ? C1 Cd2 O7 C22 169.8(10) . . . . ? C16 Cd2 O7 C22 38.8(10) 36 . . . ? Cd2 O7 C22 O8 15.3(17) . . . . ? Cd2 O7 C22 C23 -168.7(6) . . . . ? C7 C8 C9 O3 7.1(10) . . . . ? C10 C8 C9 O3 -170.0(6) . . . . ? C7 C8 C9 O4 -170.5(7) . . . . ? C10 C8 C9 O4 12.4(10) . . . . ? O7 C22 O8 Cd1 -3.2(16) . . . . ? C23 C22 O8 Cd1 -179.4(5) . . . . ? O8 Cd1 O8 C22 131(13) 25_666 . . . ? O3 Cd1 O8 C22 -138.1(8) 16_545 . . . ? O3 Cd1 O8 C22 41.9(8) 34_665 . . . ? O6 Cd1 O8 C22 137.0(8) 18_655 . . . ? O6 Cd1 O8 C22 -43.0(8) 36 . . . ? C14 C15 C16 O5 6.0(12) . . . . ? C17 C15 C16 O5 -172.4(7) . . . . ? C14 C15 C16 O6 -173.9(8) . . . . ? C17 C15 C16 O6 7.7(11) . . . . ? C14 C15 C16 Cd2 60(18) . . . 30_455 ? C17 C15 C16 Cd2 -118(17) . . . 30_455 ? O8 C22 C23 C24 103.9(10) . . . . ? O7 C22 C23 C24 -72.8(12) . . . . ? O8 C22 C23 C28 -75.3(12) . . . . ? O7 C22 C23 C28 108.1(12) . . . . ? O5 C16 O6 Cd1 112.5(9) . . . 18_655 ? C15 C16 O6 Cd1 -67.6(13) . . . 18_655 ? Cd2 C16 O6 Cd1 110.9(10) 30_455 . . 18_655 ? O5 C16 O6 Cd2 1.6(8) . . . 30_455 ? C15 C16 O6 Cd2 -178.5(6) . . . 30_455 ? O4 C9 O3 Cd1 -93.8(8) . . . 16_545 ? C8 C9 O3 Cd1 88.8(7) . . . 16_545 ? O3 C9 O4 Cd2 8.9(8) . . . 28_665 ? C8 C9 O4 Cd2 -173.5(5) . . . 28_665 ? O6 C16 O5 Cd2 -1.6(8) . . . 30_455 ? C15 C16 O5 Cd2 178.5(6) . . . 30_455 ? C24 C25 C26 C27 4.5(14) . . . . ? C26 C25 C26 C27 -177.2(7) 2_655 . . . ? C24 C25 C26 C25 177.3(6) . . . 3_665 ? C26 C25 C26 C25 -4.5(17) 2_655 . . 3_665 ? C28 C23 C24 C25 0.3(15) . . . . ? C22 C23 C24 C25 -178.8(9) . . . . ? C26 C25 C24 C23 -3.0(14) . . . . ? C26 C25 C24 C23 178.8(9) 2_655 . . . ? C25 C26 C27 C28 -3.5(17) . . . . ? C25 C26 C27 C28 -176.2(11) 3_665 . . . ? C24 C23 C28 C27 0.8(18) . . . . ? C22 C23 C28 C27 179.9(11) . . . . ? C26 C27 C28 C23 1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 65.34 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.072 _refine_diff_density_min -1.317 _refine_diff_density_rms 0.102 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 1 -0.021 -0.039 -0.001 24377.6 5235.7 _platon_squeeze_details ; ? ; # start Validation Reply Form _vrf_CHEMW03_1 ; PROBLEM: The ratio of given/expected molecular weight as RESPONSE: The highly disordered solvent molecules and counterions can not be identified, deduced by means of EA and TGA measurement, but it needed to calculate molecular mass. ; _vrf_DENSD01_1 ; PROBLEM: The ratio of the submitted crystal density and that RESPONSE: The highly disordered solvent molecules and counterions can not be identified, deduced by means of EA and TGA measurement, but it needed to calculate molecular mass. ; _vrf_PLAT046_1 ; PROBLEM: Reported Z, MW and D(calc) are Inconsistent RESPONSE: The highly disordered solvent molecules and counterions can not be identified, deduced by means of EA and TGA measurement, but it needed to calculate molecular mass. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 920789'