Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Wei-Yin, Sun' 'Fan, Jian' 'Okamura, Taka-aki' 'Sui, Bin' 'Tang, Wen-Xia' 'Ueyama, Norikazu' _publ_contact_author_name 'Prof Sun Wei-Yin' _publ_contact_author_address ; Prof Sun Wei-Yin Coordination Chemistry Institute Nanjing University Nanjing CHINA ; _publ_contact_author_email 'SUNWY@NJU.EDU.CN' _publ_section_title ; Synthesis, structures and properties of two-dimensional honeycomb and stepwise networks from self-assembly of tripodal ligand 1,3,5-tris(imidazol-1-ylmethyl)-2,4,6-trimethylbenzene with metal salts ; data_1 _database_code_CSD 180727 _audit_creation_method SHELXL-97 _audit_creation_date 'Thu Jan 4 15:57:06 2001' _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Zn(L)2](ClO4)2 (1) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H48 Cl2 N12 O8 Zn ' _chemical_formula_sum 'C42 H48 Cl2 N12 O8 Zn' _chemical_formula_weight 985.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 '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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 13.5818(8) _cell_length_b 13.5818(8) _cell_length_c 13.5818(8) _cell_angle_alpha 46.194(2) _cell_angle_beta 46.194(2) _cell_angle_gamma 46.194(2) _cell_volume 1190.71(12) _cell_formula_units_Z 1 _cell_measurement_temperature 200 _cell_measurement_reflns_used 11586 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.4 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.417 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3599 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.1298 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1833 _reflns_number_gt 1039 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1833 _refine_ls_number_parameters 100 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.0000 0.0461(3) Uani 1 6 d S . . Cl1 Cl 0.17219(3) 0.17219(3) 0.17219(3) 0.0402(3) Uani 1 3 d SU . . O1 O 0.21065(13) 0.21065(13) 0.21065(13) 0.1106(18) Uani 1 3 d SU . . O2 O 0.1252(3) 0.3013(3) 0.0555(3) 0.0894(9) Uani 1 1 d U . . N11 N -0.1090(3) 0.2247(3) -0.3611(3) 0.0458(6) Uani 1 1 d . . . N12 N -0.0236(3) 0.1279(3) -0.2078(3) 0.0482(6) Uani 1 1 d . . . C1 C -0.3269(3) 0.4118(3) -0.4318(3) 0.0385(6) Uani 1 1 d . . . C2 C -0.4665(3) 0.4285(3) -0.3090(3) 0.0404(6) Uani 1 1 d . . . C11 C -0.1977(3) 0.2583(3) -0.4145(3) 0.0475(7) Uani 1 1 d . . . H1 H -0.2379 0.1816 -0.3432 0.082 Uiso 1 1 calc R . . H2 H -0.1311 0.2515 -0.5122 0.082 Uiso 1 1 calc R . . C12 C -0.1199(4) 0.1437(4) -0.2223(3) 0.0538(8) Uani 1 1 d . . . H3 H -0.1911 0.1011 -0.1408 0.082 Uiso 1 1 calc R . . C13 C 0.0548(5) 0.2019(6) -0.3450(4) 0.1104(19) Uani 1 1 d . . . H4 H 0.1359 0.2096 -0.3721 0.082 Uiso 1 1 calc R . . C14 C 0.0023(6) 0.2647(6) -0.4403(5) 0.128(2) Uani 1 1 d . . . H5 H 0.0374 0.3259 -0.5442 0.137 Uiso 1 1 calc R . . C21 C -0.4841(4) 0.2974(3) -0.1576(3) 0.0562(9) Uani 1 1 d . . . H6 H -0.5899 0.3145 -0.0964 0.082 Uiso 1 1 calc R . . H7 H -0.4479 0.2871 -0.1076 0.082 Uiso 1 1 calc R . . H8 H -0.4260 0.2057 -0.1710 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0466(3) 0.0466(3) 0.0466(3) -0.01917(18) -0.01917(18) -0.01917(18) Cl1 0.0335(4) 0.0335(4) 0.0335(4) -0.0116(2) -0.0116(2) -0.0116(2) O1 0.130(3) 0.130(3) 0.130(3) -0.0590(15) -0.0590(15) -0.0590(15) O2 0.0685(17) 0.0596(16) 0.0475(14) -0.0026(12) -0.0317(13) -0.0085(13) N11 0.0445(14) 0.0432(14) 0.0388(14) -0.0128(11) -0.0185(12) -0.0170(12) N12 0.0482(15) 0.0455(15) 0.0495(15) -0.0174(13) -0.0230(12) -0.0177(12) C1 0.0415(16) 0.0398(15) 0.0450(17) -0.0212(14) -0.0203(13) -0.0135(13) C2 0.0474(17) 0.0398(16) 0.0439(17) -0.0183(13) -0.0194(14) -0.0190(14) C11 0.0510(18) 0.0480(18) 0.0472(18) -0.0243(15) -0.0208(15) -0.0160(15) C12 0.055(2) 0.058(2) 0.0428(18) -0.0142(16) -0.0195(16) -0.0286(17) C13 0.118(4) 0.150(5) 0.062(3) 0.025(3) -0.054(3) -0.106(4) C14 0.121(4) 0.182(6) 0.050(2) 0.031(3) -0.046(3) -0.120(4) C21 0.055(2) 0.0453(18) 0.0457(18) -0.0134(15) -0.0160(16) -0.0232(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N12 2.186(5) . ? Zn1 N12 2.186(5) 4 ? Zn1 N12 2.186(5) 6 ? Zn1 N12 2.186(5) 5 ? Zn1 N12 2.186(5) 2 ? Zn1 N12 2.186(5) 3 ? Cl1 O1 1.397(2) . ? Cl1 O2 1.413(2) 2 ? Cl1 O2 1.413(2) . ? Cl1 O2 1.413(2) 3 ? N11 C12 1.325(4) . ? N11 C14 1.347(11) . ? N11 C11 1.475(8) . ? N12 C12 1.306(9) . ? N12 C13 1.326(4) . ? C1 C2 1.402(4) 2_564 ? C1 C2 1.407(4) . ? C1 C11 1.519(4) . ? C2 C1 1.402(4) 3_465 ? C2 C21 1.515(4) . ? C11 H1 0.9900 . ? C11 H2 0.9900 . ? C12 H3 0.9500 . ? C13 C14 1.349(12) . ? C13 H4 0.9500 . ? C14 H5 0.9500 . ? C21 H6 0.9800 . ? C21 H7 0.9800 . ? C21 H8 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Zn1 N12 180.0 . 4 ? N12 Zn1 N12 89.57(9) . 6 ? N12 Zn1 N12 90.42(9) 4 6 ? N12 Zn1 N12 89.58(9) . 5 ? N12 Zn1 N12 90.42(9) 4 5 ? N12 Zn1 N12 90.42(9) 6 5 ? N12 Zn1 N12 90.42(9) . 2 ? N12 Zn1 N12 89.58(9) 4 2 ? N12 Zn1 N12 89.58(9) 6 2 ? N12 Zn1 N12 180.0 5 2 ? N12 Zn1 N12 90.42(9) . 3 ? N12 Zn1 N12 89.58(9) 4 3 ? N12 Zn1 N12 180.0 6 3 ? N12 Zn1 N12 89.58(9) 5 3 ? N12 Zn1 N12 90.42(9) 2 3 ? O1 Cl1 O2 107.21(14) . 2 ? O1 Cl1 O2 107.21(14) . . ? O2 Cl1 O2 111.63(13) 2 . ? O1 Cl1 O2 107.21(14) . 3 ? O2 Cl1 O2 111.63(13) 2 3 ? O2 Cl1 O2 111.63(13) . 3 ? C12 N11 C14 104.4(3) . . ? C12 N11 C11 126.9(3) . . ? C14 N11 C11 128.7(3) . . ? C12 N12 C13 104.5(3) . . ? C12 N12 Zn1 125.8(2) . . ? C13 N12 Zn1 129.7(5) . . ? C2 C1 C2 120.5(3) 2_564 . ? C2 C1 C11 120.0(3) 2_564 . ? C2 C1 C11 119.4(3) . . ? C1 C2 C1 119.5(3) 3_465 . ? C1 C2 C21 120.3(3) 3_465 . ? C1 C2 C21 120.1(3) . . ? N11 C11 C1 113.6(2) . . ? N11 C11 H1 108.8 . . ? C1 C11 H1 108.8 . . ? N11 C11 H2 108.8 . . ? C1 C11 H2 108.8 . . ? H1 C11 H2 107.7 . . ? N12 C12 N11 113.8(3) . . ? N12 C12 H3 123.1 . . ? N11 C12 H3 123.1 . . ? N12 C13 C14 109.9(8) . . ? N12 C13 H4 125.1 . . ? C14 C13 H4 125.1 . . ? N11 C14 C13 107.4(3) . . ? N11 C14 H5 126.3 . . ? C13 C14 H5 126.3 . . ? C2 C21 H6 109.5 . . ? C2 C21 H7 109.5 . . ? H6 C21 H7 109.5 . . ? C2 C21 H8 109.5 . . ? H6 C21 H8 109.5 . . ? H7 C21 H8 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Zn1 N12 C12 -123(3) 4 . . . ? N12 Zn1 N12 C12 -100.0(2) 6 . . . ? N12 Zn1 N12 C12 169.6(3) 5 . . . ? N12 Zn1 N12 C12 -10.4(3) 2 . . . ? N12 Zn1 N12 C12 80.0(2) 3 . . . ? N12 Zn1 N12 C13 59(3) 4 . . . ? N12 Zn1 N12 C13 82.1(4) 6 . . . ? N12 Zn1 N12 C13 -8.3(4) 5 . . . ? N12 Zn1 N12 C13 171.7(4) 2 . . . ? N12 Zn1 N12 C13 -97.9(4) 3 . . . ? C2 C1 C2 C1 -0.3(5) 2_564 . . 3_465 ? C11 C1 C2 C1 -176.4(5) . . . 3_465 ? C2 C1 C2 C21 -178.6(5) 2_564 . . . ? C11 C1 C2 C21 5.2(4) . . . . ? C12 N11 C11 C1 99.2(4) . . . . ? C14 N11 C11 C1 -82.6(5) . . . . ? C2 C1 C11 N11 95.4(3) 2_564 . . . ? C2 C1 C11 N11 -88.6(3) . . . . ? C13 N12 C12 N11 -0.4(4) . . . . ? Zn1 N12 C12 N11 -178.77(18) . . . . ? C14 N11 C12 N12 -0.8(4) . . . . ? C11 N11 C12 N12 177.8(3) . . . . ? C12 N12 C13 C14 1.5(6) . . . . ? Zn1 N12 C13 C14 179.8(3) . . . . ? C12 N11 C14 C13 1.7(5) . . . . ? C11 N11 C14 C13 -176.9(4) . . . . ? N12 C13 C14 N11 -2.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.487 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.062 #========END data_2 _database_code_CSD 180728 _audit_creation_date 'Fri Apr 6 15:40:26 2001' _audit_creation_method SHELXL-97 _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Mn(L)2](SO4)¡¤16H2O (2) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H80 N12 Mn O20 S ' _chemical_formula_sum 'C42 H80 Mn N12 O20 S' _chemical_formula_weight 1160.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.7906(2) _cell_length_b 20.4405(3) _cell_length_c 24.3496(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.328(2) _cell_angle_gamma 90.00 _cell_volume 5820.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 25531 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2468 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11792 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.1509 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6677 _reflns_number_gt 3785 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare, 1994)' _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^)+(0.0917P)^2^+9.6231P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6677 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1103 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2082 _refine_ls_wR_factor_gt 0.1951 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Mn1 Mn 1.0000 0.0000 0.5000 0.0245(2) Uani 1 2 d S . . S1 S 1.0000 0.02263(7) 0.2500 0.0289(3) Uani 1 2 d S . . O1 O 0.9067(3) 0.06445(16) 0.22383(13) 0.0434(8) Uani 1 1 d . . . O2 O 0.9548(3) -0.01881(15) 0.29204(12) 0.0384(7) Uani 1 1 d . . . O3 O 1.2457(3) 0.08967(19) 0.36899(16) 0.0604(10) Uani 1 1 d . . . O4 O 1.5000 0.1152(3) 0.2500 0.0585(13) Uani 1 2 d S . . O5 O 1.4399(3) 0.16001(19) 0.35025(18) 0.0649(11) Uani 1 1 d . . . O6 O 1.4676(3) 0.28577(18) 0.39864(14) 0.0530(9) Uani 1 1 d . . . O7 O 1.4407(3) 0.34706(17) 0.29569(14) 0.0507(9) Uani 1 1 d . . . O8 O 1.7203(3) 0.05922(19) 0.29276(15) 0.0555(9) Uani 1 1 d . . . O9 O 0.6564(4) 0.2226(2) 0.46578(18) 0.0802(13) Uani 1 1 d . . . O10 O 0.6571(3) 0.1089(2) 0.39643(16) 0.0648(11) Uani 1 1 d . . . O11 O 0.5000 0.0000 0.5000 0.017(14) Uiso 0.079(14) 2 d SP . . N11 N 0.9410(3) 0.16276(16) 0.37884(13) 0.0282(7) Uani 1 1 d . . . N12 N 0.9633(3) 0.08909(17) 0.44579(14) 0.0332(8) Uani 1 1 d . . . N31 N 1.2664(3) 0.09794(17) 0.61890(13) 0.0297(8) Uani 1 1 d . . . N32 N 1.1403(3) 0.05914(17) 0.55182(14) 0.0296(7) Uani 1 1 d . . . N51 N 1.2292(3) -0.07292(17) 0.38296(13) 0.0285(8) Uani 1 1 d . . . N52 N 1.1370(3) -0.03674(18) 0.45035(13) 0.0320(8) Uani 1 1 d . . . C1 C 0.9411(3) 0.26291(19) 0.32205(15) 0.0264(8) Uani 1 1 d . . . C2 C 0.8434(3) 0.3028(2) 0.32261(15) 0.0264(8) Uani 1 1 d . . . C3 C 0.8567(3) 0.3706(2) 0.32408(15) 0.0263(8) Uani 1 1 d . . . C4 C 0.9646(3) 0.4001(2) 0.32578(15) 0.0278(8) Uani 1 1 d . . . C5 C 1.0606(3) 0.3597(2) 0.32370(15) 0.0264(8) Uani 1 1 d . . . C6 C 1.0498(3) 0.2915(2) 0.32291(15) 0.0277(8) Uani 1 1 d . . . C11 C 0.9278(4) 0.1897(2) 0.32196(16) 0.0339(9) Uani 1 1 d . . . H10 H 0.8513 0.1780 0.3029 0.060 Uiso 1 1 calc R . . H11 H 0.9859 0.1698 0.3011 0.060 Uiso 1 1 calc R . . C12 C 0.9640(3) 0.0994(2) 0.39194(16) 0.0273(8) Uani 1 1 d . . . H1 H 0.9785 0.0666 0.3661 0.060 Uiso 1 1 calc R . . C13 C 0.9369(4) 0.1489(2) 0.46723(17) 0.0358(10) Uani 1 1 d . . . H2 H 0.9292 0.1567 0.5050 0.060 Uiso 1 1 calc R . . C14 C 0.9236(4) 0.1946(2) 0.42697(17) 0.0355(10) Uani 1 1 d . . . H3 H 0.9059 0.2396 0.4310 0.060 Uiso 1 1 calc R . . C21 C 0.7261(4) 0.2727(2) 0.3249(2) 0.0402(11) Uani 1 1 d . . . H12 H 0.7348 0.2299 0.3431 0.060 Uiso 1 1 calc R . . H13 H 0.6870 0.2672 0.2872 0.060 Uiso 1 1 calc R . . H14 H 0.6809 0.3015 0.3458 0.060 Uiso 1 1 calc R . . C31 C 0.7526(3) 0.4140(2) 0.32506(15) 0.0306(9) Uani 1 1 d . . . H15 H 0.7653 0.4560 0.3066 0.060 Uiso 1 1 calc R . . H16 H 0.6852 0.3925 0.3042 0.060 Uiso 1 1 calc R . . C32 C 1.1814(3) 0.0551(2) 0.60504(16) 0.0296(9) Uani 1 1 d . . . H4 H 1.1539 0.0255 0.6303 0.060 Uiso 1 1 calc R . . C33 C 1.2804(4) 0.1328(2) 0.57191(17) 0.0388(10) Uani 1 1 d . . . H5 H 1.3336 0.1670 0.5688 0.060 Uiso 1 1 calc R . . C34 C 1.2030(4) 0.1084(2) 0.53086(18) 0.0377(10) Uani 1 1 d . . . H6 H 1.1934 0.1229 0.4935 0.060 Uiso 1 1 calc R . . C41 C 0.9802(4) 0.4728(2) 0.3308(2) 0.0403(10) Uani 1 1 d . . . H17 H 0.9140 0.4921 0.3453 0.060 Uiso 1 1 calc R . . H18 H 0.9869 0.4914 0.2942 0.060 Uiso 1 1 calc R . . H19 H 1.0498 0.4824 0.3560 0.060 Uiso 1 1 calc R . . C51 C 1.1769(3) 0.3907(2) 0.32386(16) 0.0309(9) Uani 1 1 d . . . H20 H 1.2255 0.3617 0.3041 0.038 Uiso 1 1 calc R . . H21 H 1.1685 0.4329 0.3038 0.038 Uiso 1 1 calc R . . C52 C 1.1304(3) -0.0497(2) 0.39655(16) 0.0301(9) Uani 1 1 d . . . H7 H 1.0636 -0.0433 0.3709 0.037 Uiso 1 1 calc R . . C53 C 1.2480(4) -0.0523(2) 0.47206(17) 0.0395(11) Uani 1 1 d . . . H8 H 1.2788 -0.0486 0.5099 0.060 Uiso 1 1 calc R . . C54 C 1.3061(4) -0.0738(3) 0.43057(18) 0.0443(12) Uani 1 1 d . . . H9 H 1.3840 -0.0868 0.4339 0.060 Uiso 1 1 calc R . . C61 C 1.1532(4) 0.2464(2) 0.32557(18) 0.0383(10) Uani 1 1 d . . . H22 H 1.2233 0.2721 0.3346 0.047 Uiso 1 1 calc R . . H23 H 1.1543 0.2250 0.2896 0.047 Uiso 1 1 calc R . . H24 H 1.1486 0.2132 0.3542 0.047 Uiso 1 1 calc R . . H25 H 1.4938 0.1461 0.2787 0.060 Uiso 1 1 d . . . H26 H 1.3799 0.1405 0.3640 0.060 Uiso 1 1 d . . . H27 H 1.4532 0.2172 0.3531 0.060 Uiso 1 1 d . . . H28 H 1.5374 0.2653 0.4253 0.060 Uiso 1 1 d . . . H29 H 1.4063 0.2934 0.4240 0.060 Uiso 1 1 d . . . H30 H 1.6555 0.0783 0.2756 0.060 Uiso 1 1 d . . . H31 H 1.7799 0.0617 0.2701 0.060 Uiso 1 1 d . . . H32 H 0.6858 0.0870 0.3669 0.060 Uiso 1 1 d . . . H33 H 0.5769 0.0918 0.3911 0.060 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0242(4) 0.0246(5) 0.0249(4) -0.0001(4) 0.0035(3) 0.0005(3) S1 0.0282(7) 0.0299(8) 0.0289(7) 0.000 0.0049(5) 0.000 O1 0.0401(17) 0.0439(19) 0.0459(18) 0.0112(15) 0.0039(14) 0.0079(14) O2 0.0458(18) 0.0400(18) 0.0306(15) 0.0085(13) 0.0091(13) 0.0000(14) O3 0.055(2) 0.053(2) 0.071(2) 0.0041(19) 0.0007(19) -0.0034(18) O4 0.064(3) 0.056(3) 0.055(3) 0.000 0.005(3) 0.000 O5 0.054(2) 0.058(2) 0.085(3) -0.013(2) 0.018(2) -0.0032(18) O6 0.056(2) 0.053(2) 0.049(2) -0.0056(17) 0.0040(17) 0.0027(17) O7 0.046(2) 0.055(2) 0.051(2) 0.0055(17) 0.0094(16) 0.0019(16) O8 0.0409(19) 0.070(3) 0.057(2) 0.0068(18) 0.0116(16) 0.0123(17) O9 0.073(3) 0.081(3) 0.084(3) -0.029(2) 0.000(2) 0.014(2) O10 0.057(2) 0.070(3) 0.064(2) -0.015(2) -0.0051(19) -0.003(2) N11 0.0343(18) 0.0219(18) 0.0279(16) 0.0010(14) 0.0024(14) 0.0011(14) N12 0.0375(19) 0.030(2) 0.0313(18) -0.0060(15) 0.0029(15) 0.0013(15) N31 0.0263(17) 0.034(2) 0.0287(17) 0.0032(15) 0.0031(13) -0.0043(14) N32 0.0249(16) 0.0301(19) 0.0335(18) -0.0017(15) 0.0020(14) -0.0055(14) N51 0.0228(16) 0.037(2) 0.0264(17) 0.0004(15) 0.0043(13) 0.0061(14) N52 0.0298(18) 0.039(2) 0.0284(17) 0.0004(15) 0.0064(14) 0.0078(15) C1 0.033(2) 0.020(2) 0.0259(19) -0.0007(16) 0.0034(16) -0.0008(15) C2 0.0246(19) 0.029(2) 0.0247(18) 0.0023(16) 0.0008(15) -0.0017(15) C3 0.0263(19) 0.030(2) 0.0218(18) 0.0021(16) 0.0018(15) 0.0032(16) C4 0.030(2) 0.028(2) 0.0249(19) -0.0022(16) 0.0029(16) -0.0030(16) C5 0.0236(18) 0.031(2) 0.0244(18) -0.0007(16) 0.0024(15) -0.0017(16) C6 0.029(2) 0.030(2) 0.0241(19) 0.0011(16) 0.0034(15) 0.0050(16) C11 0.045(3) 0.028(2) 0.028(2) 0.0018(18) 0.0030(18) -0.0036(18) C12 0.031(2) 0.023(2) 0.0277(19) 0.0036(16) 0.0046(16) -0.0005(16) C13 0.045(3) 0.032(2) 0.030(2) -0.0022(18) 0.0052(18) 0.0028(19) C14 0.042(2) 0.032(2) 0.032(2) -0.0042(19) 0.0040(18) 0.0072(18) C21 0.027(2) 0.042(3) 0.051(3) 0.005(2) 0.0031(19) -0.0054(19) C31 0.030(2) 0.037(2) 0.0252(19) 0.0006(17) 0.0050(16) 0.0079(17) C32 0.0251(19) 0.033(2) 0.030(2) -0.0037(17) 0.0025(16) -0.0055(16) C33 0.038(2) 0.042(3) 0.036(2) 0.003(2) 0.0051(19) -0.015(2) C34 0.040(2) 0.042(3) 0.031(2) 0.0016(19) 0.0019(18) -0.009(2) C41 0.043(3) 0.029(2) 0.051(3) -0.001(2) 0.013(2) 0.0001(19) C51 0.027(2) 0.037(2) 0.028(2) 0.0013(18) 0.0025(16) -0.0052(17) C52 0.027(2) 0.034(2) 0.029(2) 0.0041(18) 0.0034(16) 0.0032(17) C53 0.031(2) 0.060(3) 0.027(2) -0.004(2) 0.0009(17) 0.009(2) C54 0.033(2) 0.067(4) 0.033(2) 0.001(2) 0.0044(19) 0.016(2) C61 0.037(2) 0.039(3) 0.038(2) 0.002(2) 0.0028(19) 0.0105(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N12 2.258(4) 5_756 ? Mn1 N12 2.258(4) . ? Mn1 N52 2.266(3) 5_756 ? Mn1 N52 2.266(3) . ? Mn1 N32 2.293(3) 5_756 ? Mn1 N32 2.293(3) . ? S1 O1 1.472(3) 2_755 ? S1 O1 1.472(3) . ? S1 O2 1.479(3) 2_755 ? S1 O2 1.479(3) . ? O4 H25 0.95 . ? O5 H26 0.91 . ? O5 H27 1.18 . ? O6 H28 1.07 . ? O6 H29 1.02 . ? O8 H30 0.91 . ? O8 H31 0.95 . ? O10 H32 0.95 . ? O10 H33 1.00 . ? N11 C12 1.353(5) . ? N11 C14 1.379(5) . ? N11 C11 1.480(5) . ? N12 C12 1.329(5) . ? N12 C13 1.380(5) . ? N31 C32 1.341(5) . ? N31 C33 1.375(5) . ? N31 C51 1.485(5) 7_756 ? N32 C32 1.327(5) . ? N32 C34 1.384(5) . ? N51 C52 1.338(5) . ? N51 C54 1.378(5) . ? N51 C31 1.495(5) 3_545 ? N52 C52 1.329(5) . ? N52 C53 1.384(5) . ? C1 C6 1.406(6) . ? C1 C2 1.413(5) . ? C1 C11 1.505(6) . ? C2 C3 1.396(6) . ? C2 C21 1.521(5) . ? C3 C4 1.404(5) . ? C3 C31 1.517(5) . ? C4 C5 1.407(5) . ? C4 C41 1.500(6) . ? C5 C6 1.399(6) . ? C5 C51 1.510(5) . ? C6 C61 1.523(6) . ? C11 H10 0.9900 . ? C11 H11 0.9900 . ? C12 H1 0.9500 . ? C13 C14 1.350(6) . ? C13 H2 0.9500 . ? C14 H3 0.9500 . ? C21 H12 0.9800 . ? C21 H13 0.9800 . ? C21 H14 0.9800 . ? C31 N51 1.495(5) 3_455 ? C31 H15 0.9900 . ? C31 H16 0.9900 . ? C32 H4 0.9500 . ? C33 C34 1.359(6) . ? C33 H5 0.9500 . ? C34 H6 0.9500 . ? C41 H17 0.9800 . ? C41 H18 0.9800 . ? C41 H19 0.9800 . ? C51 N31 1.485(5) 7_756 ? C51 H20 0.9900 . ? C51 H21 0.9900 . ? C52 H7 0.9500 . ? C53 C54 1.364(6) . ? C53 H8 0.9500 . ? C54 H9 0.9500 . ? C61 H22 0.9800 . ? C61 H23 0.9800 . ? C61 H24 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Mn1 N12 179.998(1) 5_756 . ? N12 Mn1 N52 92.98(12) 5_756 5_756 ? N12 Mn1 N52 87.02(12) . 5_756 ? N12 Mn1 N52 87.02(12) 5_756 . ? N12 Mn1 N52 92.98(12) . . ? N52 Mn1 N52 180.0 5_756 . ? N12 Mn1 N32 88.14(12) 5_756 5_756 ? N12 Mn1 N32 91.86(12) . 5_756 ? N52 Mn1 N32 87.42(12) 5_756 5_756 ? N52 Mn1 N32 92.58(12) . 5_756 ? N12 Mn1 N32 91.86(12) 5_756 . ? N12 Mn1 N32 88.14(12) . . ? N52 Mn1 N32 92.58(12) 5_756 . ? N52 Mn1 N32 87.42(12) . . ? N32 Mn1 N32 180.0 5_756 . ? O1 S1 O1 109.0(3) 2_755 . ? O1 S1 O2 108.48(17) 2_755 2_755 ? O1 S1 O2 110.36(18) . 2_755 ? O1 S1 O2 110.37(18) 2_755 . ? O1 S1 O2 108.49(17) . . ? O2 S1 O2 110.1(3) 2_755 . ? H26 O5 H27 121.0 . . ? H28 O6 H29 104.0 . . ? H30 O8 H31 110.5 . . ? H32 O10 H33 99.2 . . ? C12 N11 C14 107.4(3) . . ? C12 N11 C11 124.8(3) . . ? C14 N11 C11 127.6(3) . . ? C12 N12 C13 105.3(3) . . ? C12 N12 Mn1 132.8(3) . . ? C13 N12 Mn1 121.9(3) . . ? C32 N31 C33 107.1(3) . . ? C32 N31 C51 124.8(3) . 7_756 ? C33 N31 C51 127.8(3) . 7_756 ? C32 N32 C34 105.0(3) . . ? C32 N32 Mn1 130.8(3) . . ? C34 N32 Mn1 124.2(3) . . ? C52 N51 C54 107.3(3) . . ? C52 N51 C31 124.6(3) . 3_545 ? C54 N51 C31 127.6(3) . 3_545 ? C52 N52 C53 105.3(3) . . ? C52 N52 Mn1 129.5(3) . . ? C53 N52 Mn1 125.2(3) . . ? C6 C1 C2 120.2(4) . . ? C6 C1 C11 120.5(4) . . ? C2 C1 C11 119.3(4) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C21 120.1(4) . . ? C1 C2 C21 120.9(4) . . ? C2 C3 C4 121.7(4) . . ? C2 C3 C31 119.5(3) . . ? C4 C3 C31 118.7(4) . . ? C3 C4 C5 118.5(4) . . ? C3 C4 C41 121.9(4) . . ? C5 C4 C41 119.6(4) . . ? C6 C5 C4 120.9(4) . . ? C6 C5 C51 119.9(4) . . ? C4 C5 C51 119.2(4) . . ? C5 C6 C1 119.7(4) . . ? C5 C6 C61 122.1(4) . . ? C1 C6 C61 118.2(4) . . ? N11 C11 C1 111.7(3) . . ? N11 C11 H10 109.3 . . ? C1 C11 H10 109.3 . . ? N11 C11 H11 109.3 . . ? C1 C11 H11 109.3 . . ? H10 C11 H11 107.9 . . ? N12 C12 N11 111.0(3) . . ? N12 C12 H1 124.5 . . ? N11 C12 H1 124.5 . . ? C14 C13 N12 110.5(4) . . ? C14 C13 H2 124.8 . . ? N12 C13 H2 124.8 . . ? C13 C14 N11 105.9(4) . . ? C13 C14 H3 127.1 . . ? N11 C14 H3 127.1 . . ? C2 C21 H12 109.5 . . ? C2 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C2 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? N51 C31 C3 111.5(3) 3_455 . ? N51 C31 H15 109.3 3_455 . ? C3 C31 H15 109.3 . . ? N51 C31 H16 109.3 3_455 . ? C3 C31 H16 109.3 . . ? H15 C31 H16 108.0 . . ? N32 C32 N31 112.0(4) . . ? N32 C32 H4 124.0 . . ? N31 C32 H4 124.0 . . ? C34 C33 N31 106.4(4) . . ? C34 C33 H5 126.8 . . ? N31 C33 H5 126.8 . . ? C33 C34 N32 109.6(4) . . ? C33 C34 H6 125.2 . . ? N32 C34 H6 125.2 . . ? C4 C41 H17 109.5 . . ? C4 C41 H18 109.5 . . ? H17 C41 H18 109.5 . . ? C4 C41 H19 109.5 . . ? H17 C41 H19 109.5 . . ? H18 C41 H19 109.5 . . ? N31 C51 C5 111.6(3) 7_756 . ? N31 C51 H20 109.3 7_756 . ? C5 C51 H20 109.3 . . ? N31 C51 H21 109.3 7_756 . ? C5 C51 H21 109.3 . . ? H20 C51 H21 108.0 . . ? N52 C52 N51 111.8(3) . . ? N52 C52 H7 124.1 . . ? N51 C52 H7 124.1 . . ? C54 C53 N52 109.3(4) . . ? C54 C53 H8 125.3 . . ? N52 C53 H8 125.3 . . ? C53 C54 N51 106.3(4) . . ? C53 C54 H9 126.9 . . ? N51 C54 H9 126.9 . . ? C6 C61 H22 109.5 . . ? C6 C61 H23 109.5 . . ? H22 C61 H23 109.5 . . ? C6 C61 H24 109.5 . . ? H22 C61 H24 109.5 . . ? H23 C61 H24 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Mn1 N12 C12 -13(32) 5_756 . . . ? N52 Mn1 N12 C12 -145.4(4) 5_756 . . . ? N52 Mn1 N12 C12 34.6(4) . . . . ? N32 Mn1 N12 C12 -58.1(4) 5_756 . . . ? N32 Mn1 N12 C12 121.9(4) . . . . ? N12 Mn1 N12 C13 169(32) 5_756 . . . ? N52 Mn1 N12 C13 36.8(3) 5_756 . . . ? N52 Mn1 N12 C13 -143.2(3) . . . . ? N32 Mn1 N12 C13 124.1(3) 5_756 . . . ? N32 Mn1 N12 C13 -55.9(3) . . . . ? N12 Mn1 N32 C32 -29.2(4) 5_756 . . . ? N12 Mn1 N32 C32 150.8(4) . . . . ? N52 Mn1 N32 C32 63.8(4) 5_756 . . . ? N52 Mn1 N32 C32 -116.2(4) . . . . ? N32 Mn1 N32 C32 -177(11) 5_756 . . . ? N12 Mn1 N32 C34 149.5(3) 5_756 . . . ? N12 Mn1 N32 C34 -30.5(3) . . . . ? N52 Mn1 N32 C34 -117.5(3) 5_756 . . . ? N52 Mn1 N32 C34 62.5(3) . . . . ? N32 Mn1 N32 C34 1(11) 5_756 . . . ? N12 Mn1 N52 C52 124.0(4) 5_756 . . . ? N12 Mn1 N52 C52 -56.0(4) . . . . ? N52 Mn1 N52 C52 -77(14) 5_756 . . . ? N32 Mn1 N52 C52 36.0(4) 5_756 . . . ? N32 Mn1 N52 C52 -144.0(4) . . . . ? N12 Mn1 N52 C53 -54.0(4) 5_756 . . . ? N12 Mn1 N52 C53 126.0(4) . . . . ? N52 Mn1 N52 C53 105(14) 5_756 . . . ? N32 Mn1 N52 C53 -142.0(4) 5_756 . . . ? N32 Mn1 N52 C53 38.0(4) . . . . ? C6 C1 C2 C3 -0.1(5) . . . . ? C11 C1 C2 C3 178.4(3) . . . . ? C6 C1 C2 C21 -176.6(4) . . . . ? C11 C1 C2 C21 1.9(6) . . . . ? C1 C2 C3 C4 -0.9(6) . . . . ? C21 C2 C3 C4 175.7(4) . . . . ? C1 C2 C3 C31 -179.6(3) . . . . ? C21 C2 C3 C31 -3.0(5) . . . . ? C2 C3 C4 C5 2.6(5) . . . . ? C31 C3 C4 C5 -178.7(3) . . . . ? C2 C3 C4 C41 -176.3(4) . . . . ? C31 C3 C4 C41 2.4(6) . . . . ? C3 C4 C5 C6 -3.3(5) . . . . ? C41 C4 C5 C6 175.5(4) . . . . ? C3 C4 C5 C51 178.3(3) . . . . ? C41 C4 C5 C51 -2.8(5) . . . . ? C4 C5 C6 C1 2.4(6) . . . . ? C51 C5 C6 C1 -179.2(3) . . . . ? C4 C5 C6 C61 -174.7(3) . . . . ? C51 C5 C6 C61 3.6(6) . . . . ? C2 C1 C6 C5 -0.7(6) . . . . ? C11 C1 C6 C5 -179.2(3) . . . . ? C2 C1 C6 C61 176.6(3) . . . . ? C11 C1 C6 C61 -1.9(5) . . . . ? C12 N11 C11 C1 -161.4(4) . . . . ? C14 N11 C11 C1 24.4(6) . . . . ? C6 C1 C11 N11 87.5(4) . . . . ? C2 C1 C11 N11 -90.9(4) . . . . ? C13 N12 C12 N11 1.0(5) . . . . ? Mn1 N12 C12 N11 -177.0(3) . . . . ? C14 N11 C12 N12 -0.6(5) . . . . ? C11 N11 C12 N12 -175.8(4) . . . . ? C12 N12 C13 C14 -0.9(5) . . . . ? Mn1 N12 C13 C14 177.3(3) . . . . ? N12 C13 C14 N11 0.6(5) . . . . ? C12 N11 C14 C13 0.0(5) . . . . ? C11 N11 C14 C13 175.0(4) . . . . ? C2 C3 C31 N51 89.1(4) . . . 3_455 ? C4 C3 C31 N51 -89.7(4) . . . 3_455 ? C34 N32 C32 N31 -0.7(5) . . . . ? Mn1 N32 C32 N31 178.2(3) . . . . ? C33 N31 C32 N32 1.0(5) . . . . ? C51 N31 C32 N32 174.5(4) 7_756 . . . ? C32 N31 C33 C34 -0.9(5) . . . . ? C51 N31 C33 C34 -174.2(4) 7_756 . . . ? N31 C33 C34 N32 0.5(5) . . . . ? C32 N32 C34 C33 0.1(5) . . . . ? Mn1 N32 C34 C33 -178.9(3) . . . . ? C6 C5 C51 N31 -91.1(4) . . . 7_756 ? C4 C5 C51 N31 87.3(4) . . . 7_756 ? C53 N52 C52 N51 0.5(5) . . . . ? Mn1 N52 C52 N51 -177.7(3) . . . . ? C54 N51 C52 N52 -1.4(5) . . . . ? C31 N51 C52 N52 -173.8(4) 3_545 . . . ? C52 N52 C53 C54 0.5(5) . . . . ? Mn1 N52 C53 C54 178.9(3) . . . . ? N52 C53 C54 N51 -1.3(6) . . . . ? C52 N51 C54 C53 1.6(5) . . . . ? C31 N51 C54 C53 173.7(4) 3_545 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.448 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.091 #========END data_3 _database_code_CSD 180729 _audit_creation_date 'Sat Jan 13 13:22:09 2001' _audit_creation_method SHELXL-97 _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Cd3(L)2(SO4)4(H2O)2(CH3CH2OH)2][Cd(H2O)6]¡¤2H2O (3) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H70 Cd4 N12 O28 S4 ' _chemical_formula_sum 'C46 H70 Cd4 N12 O28 S4' _chemical_formula_weight 1816.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3739(13) _cell_length_b 14.5578(15) _cell_length_c 10.1860(10) _cell_angle_alpha 95.632(3) _cell_angle_beta 110.726(7) _cell_angle_gamma 69.367(3) _cell_volume 1605.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 200 _cell_measurement_reflns_used 7332 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 910 _exptl_absorpt_coefficient_mu 1.530 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.255 _exptl_absorpt_correction_T_max 0.631 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10861 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7053 _reflns_number_gt 5839 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1985)' _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^)+(0.0899P)^2^+1.6579P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7053 _refine_ls_number_parameters 536 _refine_ls_number_restraints 149 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1441 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.006 _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 Cd1 Cd 0.5000 0.0000 0.5000 0.04812(16) Uani 1 2 d S . . Cd2 Cd 0.1443(3) 0.3564(5) 0.0992(3) 0.0314(4) Uani 0.70(2) 1 d P . . Cd2B Cd 0.1255(7) 0.3867(11) 0.0892(4) 0.0285(10) Uani 0.30(2) 1 d P . . Cd3 Cd 0.5000 0.5000 0.5000 0.04257(15) Uani 1 2 d S . . S1 S 0.42235(12) 0.22948(9) 0.36699(13) 0.0442(3) Uani 1 1 d . . . S2 S -0.12075(12) 0.39156(9) -0.18319(13) 0.0440(3) Uani 1 1 d . . . O11 O 0.4023(4) 0.1351(3) 0.3429(4) 0.0587(10) Uani 1 1 d U . . O12 O 0.3119(5) 0.3092(4) 0.3172(8) 0.0447(15) Uani 0.699(12) 1 d PU . . O12B O 0.3339(19) 0.3064(12) 0.2551(16) 0.072(5) Uani 0.301(12) 1 d PU . . O13 O 0.4784(8) 0.2360(6) 0.5183(6) 0.068(2) Uani 0.699(12) 1 d PU . . O13B O 0.3780(15) 0.2866(10) 0.4997(14) 0.053(4) Uani 0.301(12) 1 d PU . . O14 O 0.5116(4) 0.2321(3) 0.2997(6) 0.0364(12) Uani 0.699(12) 1 d PU . . O14B O 0.5390(16) 0.2216(11) 0.405(3) 0.086(8) Uani 0.301(12) 1 d PU . . O21 O -0.0018(8) 0.3447(11) -0.1024(10) 0.075(3) Uani 0.548(9) 1 d PU . . O21B O -0.0149(11) 0.3019(7) -0.0983(12) 0.048(2) Uani 0.452(9) 1 d PU . . O22 O -0.1947(7) 0.4890(5) -0.1534(7) 0.0522(19) Uani 0.548(9) 1 d PU . . O22B O -0.0654(7) 0.4717(5) -0.0840(8) 0.043(2) Uani 0.452(9) 1 d PU . . O23 O -0.136(2) 0.4006(17) -0.333(2) 0.082(7) Uani 0.548(9) 1 d PU . . O23B O -0.120(2) 0.3991(14) -0.320(2) 0.046(4) Uani 0.452(9) 1 d PU . . O24 O -0.1974(7) 0.3260(6) -0.1841(8) 0.053(2) Uani 0.548(9) 1 d PU . . O24B O -0.2281(7) 0.4017(8) -0.1626(8) 0.049(3) Uani 0.452(9) 1 d PU . . O31 O 0.4585(18) 0.4432(8) 0.2732(15) 0.041(3) Uani 0.82(11) 1 d PU . . O31B O 0.428(13) 0.443(6) 0.256(10) 0.074(16) Uani 0.18(11) 1 d PU . . O32 O 0.3298(3) 0.4698(3) 0.5019(3) 0.0449(8) Uani 1 1 d U . . O33 O 0.639(3) 0.3445(9) 0.5724(18) 0.056(5) Uani 0.51(8) 1 d PU . . O33B O 0.600(4) 0.3496(16) 0.593(4) 0.096(9) Uani 0.49(8) 1 d PU . . O41 O 0.9478(10) 0.1502(6) 0.9783(10) 0.146(3) Uani 1 1 d U . . O101 O 0.6381(5) 0.0789(4) 0.6504(5) 0.0723(12) Uani 1 1 d DU . . O102 O 0.1931(6) 0.1786(4) 0.0950(7) 0.0906(16) Uani 1 1 d U . . H25 H 0.1321 0.1652 0.0941 0.070 Uiso 1 1 calc R . . N11 N 0.7624(4) -0.0573(3) 0.2818(4) 0.0389(8) Uani 1 1 d . . . N12 N 0.6401(4) -0.0589(3) 0.3939(4) 0.0414(8) Uani 1 1 d . . . N31 N 0.3975(3) 0.3026(3) -0.1284(4) 0.0352(7) Uani 1 1 d . . . N32 N 0.2467(4) 0.3481(3) -0.0441(4) 0.0394(8) Uani 1 1 d . . . N51 N -0.1025(3) 0.3466(3) 0.3120(4) 0.0335(7) Uani 1 1 d . . . N52 N 0.0344(3) 0.3654(3) 0.2360(4) 0.0354(7) Uani 1 1 d . . . C1 C 0.7631(4) 0.0849(3) 0.1657(5) 0.0340(8) Uani 1 1 d . . . C2 C 0.6649(4) 0.1159(3) 0.0386(4) 0.0337(8) Uani 1 1 d . . . C3 C 0.6178(4) 0.2141(3) -0.0056(4) 0.0333(8) Uani 1 1 d . . . C4 C 0.6627(4) 0.2839(3) 0.0807(5) 0.0342(8) Uani 1 1 d . . . C5 C 0.7513(4) 0.2539(3) 0.2132(4) 0.0324(8) Uani 1 1 d . . . C6 C 0.8045(4) 0.1544(3) 0.2553(4) 0.0356(9) Uani 1 1 d . . . C11 C 0.8234(5) -0.0231(3) 0.2058(6) 0.0462(11) Uani 1 1 d . . . H10 H 0.8225 -0.0613 0.1197 0.058 Uiso 1 1 calc R . . H11 H 0.9104 -0.0360 0.2656 0.058 Uiso 1 1 calc R . . C12 C 0.6689(4) -0.0037(3) 0.3247(5) 0.0384(9) Uani 1 1 d . . . H1 H 0.6284 0.0650 0.3078 0.047 Uiso 1 1 calc R . . C13 C 0.7203(5) -0.1528(3) 0.3949(6) 0.0491(12) Uani 1 1 d . . . H2 H 0.7227 -0.2087 0.4382 0.059 Uiso 1 1 calc R . . C14 C 0.7949(6) -0.1536(3) 0.3255(6) 0.0511(12) Uani 1 1 d . . . H3 H 0.8576 -0.2091 0.3094 0.062 Uiso 1 1 calc R . . C21 C 0.6083(5) 0.0432(4) -0.0481(5) 0.0488(12) Uani 1 1 d . . . H16 H 0.5187 0.0743 -0.0858 0.059 Uiso 1 1 calc R . . H17 H 0.6296 -0.0141 0.0112 0.059 Uiso 1 1 calc R . . H18 H 0.6399 0.0222 -0.1258 0.059 Uiso 1 1 calc R . . C31 C 0.5166(4) 0.2482(4) -0.1455(5) 0.0429(10) Uani 1 1 d . . . H12 H 0.5376 0.2910 -0.1952 0.053 Uiso 1 1 calc R . . H13 H 0.5102 0.1906 -0.2038 0.053 Uiso 1 1 calc R . . C32 C 0.3602(4) 0.2904(4) -0.0249(4) 0.0406(10) Uani 1 1 d . . . H4 H 0.4098 0.2456 0.0527 0.048 Uiso 1 1 calc R . . C33 C 0.2080(4) 0.3993(3) -0.1674(5) 0.0400(9) Uani 1 1 d . . . H5 H 0.1286 0.4464 -0.2090 0.048 Uiso 1 1 calc R . . C34 C 0.3002(4) 0.3725(3) -0.2214(4) 0.0370(9) Uani 1 1 d . . . H6 H 0.2981 0.3969 -0.3058 0.045 Uiso 1 1 calc R . . C41 C 0.6101(5) 0.3900(3) 0.0311(6) 0.0485(11) Uani 1 1 d . . . H19 H 0.6726 0.4211 0.0729 0.058 Uiso 1 1 calc R . . H20 H 0.5385 0.4243 0.0595 0.058 Uiso 1 1 calc R . . H21 H 0.5852 0.3935 -0.0715 0.058 Uiso 1 1 calc R . . C51 C 0.7863(4) 0.3309(4) 0.3141(5) 0.0424(10) Uani 1 1 d . . . H14 H 0.7167 0.3939 0.2899 0.052 Uiso 1 1 calc R . . H15 H 0.8005 0.3107 0.4105 0.052 Uiso 1 1 calc R . . C52 C -0.0662(4) 0.3422(4) 0.2010(5) 0.0400(10) Uani 1 1 d . . . H7 H -0.1075 0.3247 0.1095 0.047 Uiso 1 1 calc R . . C53 C 0.0629(4) 0.3873(3) 0.3756(4) 0.0371(9) Uani 1 1 d . . . H8 H 0.1306 0.4071 0.4300 0.044 Uiso 1 1 calc R . . C54 C -0.0215(4) 0.3759(3) 0.4236(4) 0.0345(8) Uani 1 1 d . . . H9 H -0.0237 0.3863 0.5163 0.042 Uiso 1 1 calc R . . C61 C 0.9027(6) 0.1242(5) 0.3991(6) 0.0651(16) Uani 1 1 d . . . H22 H 0.9152 0.0567 0.4228 0.078 Uiso 1 1 calc R . . H23 H 0.8763 0.1684 0.4695 0.078 Uiso 1 1 calc R . . H24 H 0.9798 0.1280 0.3980 0.078 Uiso 1 1 calc R . . C101 C 0.7704(17) 0.0558(19) 0.677(2) 0.250(14) Uani 1 1 d D . . C102 C 0.8775(17) 0.0026(14) 0.770(2) 0.102(8) Uani 0.56(4) 1 d PD . . C103 C 0.838(3) 0.098(4) 0.803(3) 0.19(3) Uani 0.44(4) 1 d PD . . 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 Cd1 0.0648(4) 0.0558(3) 0.0409(3) -0.0015(2) 0.0256(2) -0.0331(3) Cd2 0.0281(5) 0.0374(12) 0.0313(4) -0.0039(5) 0.0144(4) -0.0108(7) Cd2B 0.0195(12) 0.036(3) 0.0322(7) 0.0024(11) 0.0109(7) -0.0096(15) Cd3 0.0395(3) 0.0572(3) 0.0340(2) 0.00901(19) -0.00036(18) -0.0302(2) S1 0.0479(7) 0.0450(6) 0.0448(6) 0.0121(5) 0.0145(5) -0.0199(5) S2 0.0459(7) 0.0472(6) 0.0459(6) 0.0057(5) 0.0278(5) -0.0098(5) O11 0.068(3) 0.053(2) 0.065(2) 0.0065(18) 0.018(2) -0.0364(19) O12 0.040(3) 0.042(3) 0.047(4) -0.003(2) 0.013(2) -0.011(2) O12B 0.093(12) 0.067(9) 0.028(7) 0.018(6) 0.023(7) 0.013(8) O13 0.085(6) 0.106(5) 0.041(3) -0.008(3) 0.030(3) -0.057(5) O13B 0.064(10) 0.058(8) 0.056(7) -0.003(6) 0.022(6) -0.041(7) O14 0.038(3) 0.038(2) 0.036(3) 0.0070(19) 0.020(2) -0.0072(18) O14B 0.051(9) 0.054(8) 0.17(3) -0.007(11) 0.052(12) -0.020(7) O21 0.021(3) 0.127(10) 0.056(5) -0.010(6) -0.005(3) -0.022(5) O21B 0.047(6) 0.041(5) 0.056(5) 0.004(4) 0.007(4) -0.025(4) O22 0.052(4) 0.061(4) 0.056(4) -0.017(3) 0.028(3) -0.029(3) O22B 0.046(4) 0.045(4) 0.040(4) -0.005(3) 0.013(3) -0.019(3) O23 0.095(15) 0.117(13) 0.040(7) -0.006(7) 0.048(9) -0.018(10) O23B 0.039(6) 0.053(8) 0.058(10) 0.012(6) 0.026(5) -0.016(5) O24 0.053(4) 0.054(5) 0.060(4) 0.009(3) 0.022(3) -0.022(3) O24B 0.033(4) 0.083(7) 0.039(4) 0.002(4) 0.009(3) -0.030(4) O31 0.039(5) 0.069(6) 0.028(3) 0.004(3) 0.007(3) -0.037(4) O31B 0.07(3) 0.15(4) 0.04(2) -0.023(19) 0.03(2) -0.09(3) O32 0.051(2) 0.058(2) 0.0398(17) -0.0036(14) 0.0173(14) -0.0340(16) O33 0.032(7) 0.045(6) 0.092(7) 0.012(5) 0.006(6) -0.028(5) O33B 0.037(11) 0.110(11) 0.117(14) 0.060(9) -0.046(9) -0.052(7) O41 0.199(9) 0.104(5) 0.135(7) -0.011(5) 0.054(7) -0.058(6) O101 0.084(3) 0.096(3) 0.060(3) -0.020(2) 0.033(2) -0.055(3) O102 0.085(4) 0.079(3) 0.097(4) -0.023(3) 0.031(3) -0.022(3) N11 0.046(2) 0.0296(17) 0.042(2) 0.0018(14) 0.0159(16) -0.0130(15) N12 0.048(2) 0.042(2) 0.038(2) 0.0029(15) 0.0129(16) -0.0207(17) N31 0.0340(18) 0.0454(19) 0.0254(16) 0.0008(13) 0.0129(13) -0.0094(15) N32 0.039(2) 0.050(2) 0.0347(18) -0.0044(15) 0.0206(15) -0.0140(16) N51 0.0335(18) 0.0406(18) 0.0365(18) -0.0079(14) 0.0191(14) -0.0191(15) N52 0.0314(18) 0.048(2) 0.0318(17) -0.0063(14) 0.0166(14) -0.0146(15) C1 0.032(2) 0.0321(19) 0.043(2) 0.0029(16) 0.0185(17) -0.0104(16) C2 0.035(2) 0.039(2) 0.037(2) -0.0062(16) 0.0203(17) -0.0185(17) C3 0.030(2) 0.041(2) 0.031(2) 0.0002(16) 0.0156(16) -0.0103(17) C4 0.033(2) 0.035(2) 0.043(2) 0.0008(16) 0.0240(18) -0.0097(16) C5 0.031(2) 0.040(2) 0.037(2) -0.0061(16) 0.0186(16) -0.0182(17) C6 0.031(2) 0.043(2) 0.034(2) 0.0031(17) 0.0115(16) -0.0130(17) C11 0.046(3) 0.037(2) 0.058(3) 0.008(2) 0.026(2) -0.0063(19) C12 0.044(2) 0.032(2) 0.041(2) 0.0055(16) 0.0165(19) -0.0104(18) C13 0.064(3) 0.033(2) 0.056(3) 0.0055(19) 0.022(2) -0.019(2) C14 0.064(3) 0.027(2) 0.062(3) 0.0020(19) 0.022(3) -0.013(2) C21 0.062(3) 0.056(3) 0.044(3) -0.013(2) 0.024(2) -0.035(3) C31 0.039(2) 0.060(3) 0.029(2) 0.0017(18) 0.0176(18) -0.008(2) C32 0.038(2) 0.053(3) 0.027(2) 0.0049(17) 0.0127(17) -0.009(2) C33 0.039(2) 0.037(2) 0.041(2) 0.0000(17) 0.0131(18) -0.0094(18) C34 0.038(2) 0.044(2) 0.031(2) 0.0036(16) 0.0120(17) -0.0140(18) C41 0.054(3) 0.037(2) 0.062(3) 0.009(2) 0.031(2) -0.010(2) C51 0.040(2) 0.055(3) 0.049(3) -0.019(2) 0.029(2) -0.027(2) C52 0.037(2) 0.059(3) 0.036(2) -0.0173(19) 0.0210(18) -0.025(2) C53 0.033(2) 0.049(2) 0.031(2) -0.0022(17) 0.0083(16) -0.0186(18) C54 0.040(2) 0.043(2) 0.0269(18) -0.0073(15) 0.0142(16) -0.0207(18) C61 0.056(3) 0.071(4) 0.052(3) 0.012(3) -0.001(3) -0.020(3) C101 0.24(2) 0.47(4) 0.181(17) -0.13(2) 0.109(17) -0.28(3) C102 0.102(14) 0.086(12) 0.102(14) 0.000(9) 0.043(11) -0.004(10) C103 0.09(2) 0.34(8) 0.18(4) 0.06(4) 0.08(2) -0.06(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N12 2.237(4) . ? Cd1 N12 2.237(4) 2_656 ? Cd1 O11 2.337(4) . ? Cd1 O11 2.338(4) 2_656 ? Cd1 O101 2.402(4) . ? Cd1 O101 2.402(4) 2_656 ? Cd2 N32 2.217(4) . ? Cd2 O12B 2.223(18) . ? Cd2 N52 2.233(4) . ? Cd2 O21 2.244(9) . ? Cd2 O22B 2.343(10) 2_565 ? Cd2 O12 2.395(7) . ? Cd2 O102 2.441(8) . ? Cd2 O22 2.503(8) 2_565 ? Cd2 O21B 2.557(11) . ? Cd2B O22B 1.928(16) 2_565 ? Cd2B O22 2.213(12) 2_565 ? Cd2B O21 2.221(10) . ? Cd2B N32 2.260(6) . ? Cd2B N52 2.266(5) . ? Cd2B O22B 2.375(12) . ? Cd2B O12B 2.460(19) . ? Cd2B O12 2.622(10) . ? Cd2B O21B 2.626(12) . ? Cd3 O33B 2.210(17) 2_666 ? Cd3 O33B 2.210(17) . ? Cd3 O32 2.304(3) 2_666 ? Cd3 O32 2.304(3) . ? Cd3 O33 2.305(16) 2_666 ? Cd3 O33 2.305(16) . ? Cd3 O31 2.318(15) 2_666 ? Cd3 O31 2.318(15) . ? Cd3 O31B 2.49(10) . ? Cd3 O31B 2.49(10) 2_666 ? S1 O14B 1.320(16) . ? S1 O12 1.407(5) . ? S1 O13 1.458(6) . ? S1 O11 1.463(4) . ? S1 O12B 1.502(13) . ? S1 O14 1.504(5) . ? S1 O13B 1.674(15) . ? S2 O21 1.362(9) . ? S2 O24B 1.373(8) . ? S2 O23B 1.42(2) . ? S2 O22 1.462(7) . ? S2 O23 1.479(19) . ? S2 O21B 1.544(11) . ? S2 O24 1.562(7) . ? S2 O22B 1.641(7) . ? O21 O22B 1.755(16) . ? O22 Cd2B 2.213(12) 2_565 ? O22 Cd2 2.503(8) 2_565 ? O22B Cd2B 1.928(16) 2_565 ? O22B Cd2 2.343(10) 2_565 ? O101 C101 1.479(16) . ? O102 H25 0.8400 . ? N11 C12 1.339(6) . ? N11 C14 1.386(6) . ? N11 C11 1.475(6) . ? N12 C12 1.327(6) . ? N12 C13 1.376(7) . ? N31 C32 1.340(5) . ? N31 C34 1.378(6) . ? N31 C31 1.471(6) . ? N32 C32 1.313(6) . ? N32 C33 1.367(6) . ? N51 C52 1.345(5) . ? N51 C54 1.372(5) . ? N51 C51 1.479(5) 1_455 ? N52 C52 1.323(6) . ? N52 C53 1.373(5) . ? C1 C2 1.404(6) . ? C1 C6 1.404(6) . ? C1 C11 1.510(6) . ? C2 C3 1.393(6) . ? C2 C21 1.514(6) . ? C3 C4 1.410(6) . ? C3 C31 1.510(6) . ? C4 C5 1.395(6) . ? C4 C41 1.509(6) . ? C5 C6 1.403(6) . ? C5 C51 1.517(6) . ? C6 C61 1.518(7) . ? C11 H10 0.9900 . ? C11 H11 0.9900 . ? C12 H1 0.9500 . ? C13 C14 1.344(8) . ? C13 H2 0.9500 . ? C14 H3 0.9500 . ? C21 H16 0.9800 . ? C21 H17 0.9800 . ? C21 H18 0.9800 . ? C31 H12 0.9900 . ? C31 H13 0.9900 . ? C32 H4 0.9500 . ? C33 C34 1.359(6) . ? C33 H5 0.9500 . ? C34 H6 0.9500 . ? C41 H19 0.9800 . ? C41 H20 0.9800 . ? C41 H21 0.9800 . ? C51 N51 1.479(5) 1_655 ? C51 H14 0.9900 . ? C51 H15 0.9900 . ? C52 H7 0.9500 . ? C53 C54 1.362(6) . ? C53 H8 0.9500 . ? C54 H9 0.9500 . ? C61 H22 0.9800 . ? C61 H23 0.9800 . ? C61 H24 0.9800 . ? C101 C102 1.34(2) . ? C101 C103 1.47(2) . ? 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 N12 Cd1 N12 180 . 2_656 ? N12 Cd1 O11 88.83(15) . . ? N12 Cd1 O11 91.17(15) 2_656 . ? N12 Cd1 O11 91.17(15) . 2_656 ? N12 Cd1 O11 88.83(15) 2_656 2_656 ? O11 Cd1 O11 180 . 2_656 ? N12 Cd1 O101 84.98(15) . . ? N12 Cd1 O101 95.02(15) 2_656 . ? O11 Cd1 O101 90.58(16) . . ? O11 Cd1 O101 89.42(16) 2_656 . ? N12 Cd1 O101 95.02(15) . 2_656 ? N12 Cd1 O101 84.98(15) 2_656 2_656 ? O11 Cd1 O101 89.42(16) . 2_656 ? O11 Cd1 O101 90.58(16) 2_656 2_656 ? O101 Cd1 O101 180 . 2_656 ? N32 Cd2 O12B 81.4(5) . . ? N32 Cd2 N52 177.7(2) . . ? O12B Cd2 N52 100.8(6) . . ? N32 Cd2 O21 82.3(3) . . ? O12B Cd2 O21 153.3(6) . . ? N52 Cd2 O21 95.4(3) . . ? N32 Cd2 O22B 92.5(3) . 2_565 ? O12B Cd2 O22B 109.8(5) . 2_565 ? N52 Cd2 O22B 87.1(3) . 2_565 ? O21 Cd2 O22B 92.0(5) . 2_565 ? N32 Cd2 O12 100.0(2) . . ? O12B Cd2 O12 18.6(5) . . ? N52 Cd2 O12 82.3(2) . . ? O21 Cd2 O12 160.0(5) . . ? O22B Cd2 O12 107.6(2) 2_565 . ? N32 Cd2 O102 90.9(2) . . ? O12B Cd2 O102 79.0(5) . . ? N52 Cd2 O102 89.1(3) . . ? O21 Cd2 O102 80.2(4) . . ? O22B Cd2 O102 171.0(3) 2_565 . ? O12 Cd2 O102 80.0(3) . . ? N32 Cd2 O22 78.6(2) . 2_565 ? O12B Cd2 O22 76.7(5) . 2_565 ? N52 Cd2 O22 102.3(2) . 2_565 ? O21 Cd2 O22 120.4(5) . 2_565 ? O22B Cd2 O22 34.4(3) 2_565 2_565 ? O12 Cd2 O22 79.3(2) . 2_565 ? O102 Cd2 O22 154.6(3) . 2_565 ? N32 Cd2 O21B 89.9(3) . . ? O12B Cd2 O21B 144.6(6) . . ? N52 Cd2 O21B 88.0(3) . . ? O21 Cd2 O21B 15.2(4) . . ? O22B Cd2 O21B 104.9(3) 2_565 . ? O12 Cd2 O21B 145.5(4) . . ? O102 Cd2 O21B 66.8(3) . . ? O22 Cd2 O21B 135.2(4) 2_565 . ? O22B Cd2B O22 40.0(4) 2_565 2_565 ? O22B Cd2B O21 105.2(6) 2_565 . ? O22 Cd2B O21 136.7(7) 2_565 . ? O22B Cd2B N32 103.6(4) 2_565 . ? O22 Cd2B N32 84.2(3) 2_565 . ? O21 Cd2B N32 81.9(4) . . ? O22B Cd2B N52 97.3(5) 2_565 . ? O22 Cd2B N52 111.1(4) 2_565 . ? O21 Cd2B N52 95.1(4) . . ? N32 Cd2B N52 159.0(7) . . ? O22B Cd2B O22B 61.1(5) 2_565 . ? O22 Cd2B O22B 98.3(6) 2_565 . ? O21 Cd2B O22B 44.7(4) . . ? N32 Cd2B O22B 99.1(3) . . ? N52 Cd2B O22B 93.0(3) . . ? O22B Cd2B O12B 116.2(6) 2_565 . ? O22 Cd2B O12B 77.8(5) 2_565 . ? O21 Cd2B O12B 136.3(8) . . ? N32 Cd2B O12B 75.6(5) . . ? N52 Cd2B O12B 93.1(6) . . ? O22B Cd2B O12B 173.6(6) . . ? O22B Cd2B O12 113.5(4) 2_565 . ? O22 Cd2B O12 80.1(3) 2_565 . ? O21 Cd2B O12 141.1(7) . . ? N32 Cd2B O12 92.5(4) . . ? N52 Cd2B O12 76.8(3) . . ? O22B Cd2B O12 168.0(4) . . ? O12B Cd2B O12 16.9(4) . . ? O22B Cd2B O21B 116.3(5) 2_565 . ? O22 Cd2B O21B 150.4(5) 2_565 . ? O21 Cd2B O21B 13.7(4) . . ? N32 Cd2B O21B 87.3(4) . . ? N52 Cd2B O21B 85.7(3) . . ? O22B Cd2B O21B 55.3(3) . . ? O12B Cd2B O21B 127.2(8) . . ? O12 Cd2B O21B 128.7(6) . . ? O33B Cd3 O33B 180 2_666 . ? O33B Cd3 O32 83.9(13) 2_666 2_666 ? O33B Cd3 O32 96.1(13) . 2_666 ? O33B Cd3 O32 96.1(13) 2_666 . ? O33B Cd3 O32 83.9(13) . . ? O32 Cd3 O32 180 2_666 . ? O33B Cd3 O33 14.3(12) 2_666 2_666 ? O33B Cd3 O33 165.7(12) . 2_666 ? O32 Cd3 O33 96.8(7) 2_666 2_666 ? O32 Cd3 O33 83.2(7) . 2_666 ? O33B Cd3 O33 165.7(12) 2_666 . ? O33B Cd3 O33 14.3(12) . . ? O32 Cd3 O33 83.2(7) 2_666 . ? O32 Cd3 O33 96.8(7) . . ? O33 Cd3 O33 180 2_666 . ? O33B Cd3 O31 92.3(12) 2_666 2_666 ? O33B Cd3 O31 87.7(12) . 2_666 ? O32 Cd3 O31 87.0(5) 2_666 2_666 ? O32 Cd3 O31 93.0(5) . 2_666 ? O33 Cd3 O31 87.0(5) 2_666 2_666 ? O33 Cd3 O31 93.0(5) . 2_666 ? O33B Cd3 O31 87.7(12) 2_666 . ? O33B Cd3 O31 92.3(12) . . ? O32 Cd3 O31 93.0(5) 2_666 . ? O32 Cd3 O31 87.0(5) . . ? O33 Cd3 O31 93.0(5) 2_666 . ? O33 Cd3 O31 87.0(5) . . ? O31 Cd3 O31 180 2_666 . ? O33B Cd3 O31B 86(2) 2_666 . ? O33B Cd3 O31B 94(2) . . ? O32 Cd3 O31B 100(3) 2_666 . ? O32 Cd3 O31B 80(3) . . ? O33 Cd3 O31B 90(2) 2_666 . ? O33 Cd3 O31B 90(2) . . ? O31 Cd3 O31B 173(3) 2_666 . ? O31 Cd3 O31B 7(3) . . ? O33B Cd3 O31B 94(2) 2_666 2_666 ? O33B Cd3 O31B 86(2) . 2_666 ? O32 Cd3 O31B 80(3) 2_666 2_666 ? O32 Cd3 O31B 100(3) . 2_666 ? O33 Cd3 O31B 90(2) 2_666 2_666 ? O33 Cd3 O31B 90(2) . 2_666 ? O31 Cd3 O31B 7(3) 2_666 2_666 ? O31 Cd3 O31B 173(3) . 2_666 ? O31B Cd3 O31B 179.998(10) . 2_666 ? O14B S1 O12 132.7(8) . . ? O14B S1 O13 67.6(13) . . ? O12 S1 O13 109.4(4) . . ? O14B S1 O11 113.7(7) . . ? O12 S1 O11 112.1(3) . . ? O13 S1 O11 106.9(3) . . ? O14B S1 O12B 115.5(13) . . ? O12 S1 O12B 30.3(6) . . ? O13 S1 O12B 131.6(7) . . ? O11 S1 O12B 113.5(8) . . ? O14B S1 O14 41.3(12) . . ? O12 S1 O14 110.4(3) . . ? O13 S1 O14 107.9(3) . . ? O11 S1 O14 110.0(3) . . ? O12B S1 O14 82.4(9) . . ? O14B S1 O13B 104.6(12) . . ? O12 S1 O13B 68.9(6) . . ? O13 S1 O13B 42.6(5) . . ? O11 S1 O13B 110.9(4) . . ? O12B S1 O13B 96.8(8) . . ? O14 S1 O13B 135.5(4) . . ? O21 S2 O24B 130.2(6) . . ? O21 S2 O23B 106.0(11) . . ? O24B S2 O23B 120.4(10) . . ? O21 S2 O22 123.3(6) . . ? O24B S2 O22 61.6(5) . . ? O23B S2 O22 106.0(9) . . ? O21 S2 O23 112.7(11) . . ? O24B S2 O23 113.1(10) . . ? O23B S2 O23 7.3(18) . . ? O22 S2 O23 103.4(10) . . ? O21 S2 O21B 27.2(5) . . ? O24B S2 O21B 110.7(6) . . ? O23B S2 O21B 112.4(10) . . ? O22 S2 O21B 137.1(5) . . ? O23 S2 O21B 116.9(11) . . ? O21 S2 O24 108.1(7) . . ? O24B S2 O24 41.7(5) . . ? O23B S2 O24 109.6(8) . . ? O22 S2 O24 103.3(4) . . ? O23 S2 O24 104.0(10) . . ? O21B S2 O24 81.3(4) . . ? O21 S2 O22B 70.9(6) . . ? O24B S2 O22B 106.8(5) . . ? O23B S2 O22B 109.1(8) . . ? O22 S2 O22B 54.9(4) . . ? O23 S2 O22B 113.5(9) . . ? O21B S2 O22B 94.0(5) . . ? O24 S2 O22B 139.7(4) . . ? S1 O11 Cd1 126.0(2) . . ? S1 O12 Cd2 135.9(4) . . ? S1 O12 Cd2B 142.8(5) . . ? Cd2 O12 Cd2B 8.19(16) . . ? S1 O12B Cd2 143.4(14) . . ? S1 O12B Cd2B 150.4(14) . . ? Cd2 O12B Cd2B 8.62(17) . . ? S2 O21 O22B 62.0(6) . . ? S2 O21 Cd2B 132.7(9) . . ? O22B O21 Cd2B 72.3(6) . . ? S2 O21 Cd2 142.3(8) . . ? O22B O21 Cd2 83.0(5) . . ? Cd2B O21 Cd2 10.9(2) . . ? S2 O21B Cd2 110.8(5) . . ? S2 O21B Cd2B 101.5(5) . . ? Cd2 O21B Cd2B 9.26(16) . . ? S2 O22 Cd2B 123.8(5) . 2_565 ? S2 O22 Cd2 129.8(4) . 2_565 ? Cd2B O22 Cd2 7.53(19) 2_565 2_565 ? S2 O22B O21 47.1(3) . . ? S2 O22B Cd2B 131.9(5) . 2_565 ? O21 O22B Cd2B 170.2(6) . 2_565 ? S2 O22B Cd2 129.6(4) . 2_565 ? O21 O22B Cd2 169.1(6) . 2_565 ? Cd2B O22B Cd2 2.30(15) 2_565 2_565 ? S2 O22B Cd2B 109.2(5) . . ? O21 O22B Cd2B 63.0(4) . . ? Cd2B O22B Cd2B 118.9(5) 2_565 . ? Cd2 O22B Cd2B 121.1(4) 2_565 . ? C101 O101 Cd1 129.4(8) . . ? Cd2 O102 H25 109.5 . . ? C12 N11 C14 106.9(4) . . ? C12 N11 C11 128.0(4) . . ? C14 N11 C11 125.2(4) . . ? C12 N12 C13 105.6(4) . . ? C12 N12 Cd1 124.2(3) . . ? C13 N12 Cd1 130.0(3) . . ? C32 N31 C34 107.1(4) . . ? C32 N31 C31 127.0(4) . . ? C34 N31 C31 125.8(4) . . ? C32 N32 C33 106.0(4) . . ? C32 N32 Cd2 125.3(3) . . ? C33 N32 Cd2 128.8(3) . . ? C32 N32 Cd2B 134.0(4) . . ? C33 N32 Cd2B 119.6(4) . . ? Cd2 N32 Cd2B 10.81(19) . . ? C52 N51 C54 107.1(3) . . ? C52 N51 C51 127.5(4) . 1_455 ? C54 N51 C51 125.2(4) . 1_455 ? C52 N52 C53 106.2(3) . . ? C52 N52 Cd2 126.3(3) . . ? C53 N52 Cd2 127.2(3) . . ? C52 N52 Cd2B 127.0(3) . . ? C53 N52 Cd2B 126.3(3) . . ? Cd2 N52 Cd2B 10.8(2) . . ? C2 C1 C6 120.0(4) . . ? C2 C1 C11 119.8(4) . . ? C6 C1 C11 120.2(4) . . ? C3 C2 C1 119.8(4) . . ? C3 C2 C21 120.2(4) . . ? C1 C2 C21 120.0(4) . . ? C2 C3 C4 120.4(4) . . ? C2 C3 C31 120.8(4) . . ? C4 C3 C31 118.8(4) . . ? C5 C4 C3 119.1(4) . . ? C5 C4 C41 121.3(4) . . ? C3 C4 C41 119.6(4) . . ? C4 C5 C6 120.8(4) . . ? C4 C5 C51 119.1(4) . . ? C6 C5 C51 120.1(4) . . ? C5 C6 C1 119.4(4) . . ? C5 C6 C61 119.4(4) . . ? C1 C6 C61 121.2(4) . . ? N11 C11 C1 113.0(4) . . ? N11 C11 H10 109.0 . . ? C1 C11 H10 109.0 . . ? N11 C11 H11 109.0 . . ? C1 C11 H11 109.0 . . ? H10 C11 H11 107.8 . . ? N12 C12 N11 111.4(4) . . ? N12 C12 H1 124.3 . . ? N11 C12 H1 124.3 . . ? C14 C13 N12 109.8(4) . . ? C14 C13 H2 125.1 . . ? N12 C13 H2 125.1 . . ? C13 C14 N11 106.4(5) . . ? C13 C14 H3 126.8 . . ? N11 C14 H3 126.8 . . ? C2 C21 H16 109.5 . . ? C2 C21 H17 109.5 . . ? H16 C21 H17 109.5 . . ? C2 C21 H18 109.5 . . ? H16 C21 H18 109.5 . . ? H17 C21 H18 109.5 . . ? N31 C31 C3 111.7(3) . . ? N31 C31 H12 109.3 . . ? C3 C31 H12 109.3 . . ? N31 C31 H13 109.3 . . ? C3 C31 H13 109.3 . . ? H12 C31 H13 107.9 . . ? N32 C32 N31 111.5(4) . . ? N32 C32 H4 124.2 . . ? N31 C32 H4 124.2 . . ? C34 C33 N32 109.7(4) . . ? C34 C33 H5 125.1 . . ? N32 C33 H5 125.1 . . ? C33 C34 N31 105.7(4) . . ? C33 C34 H6 127.1 . . ? N31 C34 H6 127.1 . . ? C4 C41 H19 109.5 . . ? C4 C41 H20 109.5 . . ? H19 C41 H20 109.5 . . ? C4 C41 H21 109.5 . . ? H19 C41 H21 109.5 . . ? H20 C41 H21 109.5 . . ? N51 C51 C5 113.3(3) 1_655 . ? N51 C51 H14 108.9 1_655 . ? C5 C51 H14 108.9 . . ? N51 C51 H15 108.9 1_655 . ? C5 C51 H15 108.9 . . ? H14 C51 H15 107.7 . . ? N52 C52 N51 111.1(4) . . ? N52 C52 H7 124.4 . . ? N51 C52 H7 124.4 . . ? C54 C53 N52 109.0(4) . . ? C54 C53 H8 125.5 . . ? N52 C53 H8 125.5 . . ? C53 C54 N51 106.6(4) . . ? C53 C54 H9 126.7 . . ? N51 C54 H9 126.7 . . ? C6 C61 H22 109.5 . . ? C6 C61 H23 109.5 . . ? H22 C61 H23 109.5 . . ? C6 C61 H24 109.5 . . ? H22 C61 H24 109.5 . . ? H23 C61 H24 109.5 . . ? C102 C101 C103 57(2) . . ? C102 C101 O101 137(2) . . ? C103 C101 O101 116.2(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O14B S1 O11 Cd1 53.1(15) . . . . ? O12 S1 O11 Cd1 -139.2(4) . . . . ? O13 S1 O11 Cd1 -19.3(5) . . . . ? O12B S1 O11 Cd1 -172.1(9) . . . . ? O14 S1 O11 Cd1 97.6(3) . . . . ? O13B S1 O11 Cd1 -64.3(7) . . . . ? N12 Cd1 O11 S1 -93.9(3) . . . . ? N12 Cd1 O11 S1 86.1(3) 2_656 . . . ? O11 Cd1 O11 S1 80(63) 2_656 . . . ? O101 Cd1 O11 S1 -8.9(3) . . . . ? O101 Cd1 O11 S1 171.1(3) 2_656 . . . ? O14B S1 O12 Cd2 111.2(18) . . . . ? O13 S1 O12 Cd2 -171.7(5) . . . . ? O11 S1 O12 Cd2 -53.4(7) . . . . ? O12B S1 O12 Cd2 45.8(17) . . . . ? O14 S1 O12 Cd2 69.6(6) . . . . ? O13B S1 O12 Cd2 -158.2(7) . . . . ? O14B S1 O12 Cd2B 104.3(19) . . . . ? O13 S1 O12 Cd2B -178.6(6) . . . . ? O11 S1 O12 Cd2B -60.2(7) . . . . ? O12B S1 O12 Cd2B 39.0(17) . . . . ? O14 S1 O12 Cd2B 62.7(7) . . . . ? O13B S1 O12 Cd2B -165.0(8) . . . . ? N32 Cd2 O12 S1 -53.8(6) . . . . ? O12B Cd2 O12 S1 -50.0(15) . . . . ? N52 Cd2 O12 S1 125.8(6) . . . . ? O21 Cd2 O12 S1 41.2(13) . . . . ? O22B Cd2 O12 S1 -149.7(5) 2_565 . . . ? O102 Cd2 O12 S1 35.3(6) . . . . ? O22 Cd2 O12 S1 -130.1(6) 2_565 . . . ? O21B Cd2 O12 S1 50.8(9) . . . . ? N32 Cd2 O12 Cd2B 95.7(9) . . . . ? O12B Cd2 O12 Cd2B 99.5(18) . . . . ? N52 Cd2 O12 Cd2B -84.7(8) . . . . ? O21 Cd2 O12 Cd2B -169.3(14) . . . . ? O22B Cd2 O12 Cd2B -0.2(8) 2_565 . . . ? O102 Cd2 O12 Cd2B -175.2(9) . . . . ? O22 Cd2 O12 Cd2B 19.5(9) 2_565 . . . ? O21B Cd2 O12 Cd2B -159.7(11) . . . . ? O22B Cd2B O12 S1 -144.6(7) 2_565 . . . ? O22 Cd2B O12 S1 -122.2(7) 2_565 . . . ? O21 Cd2B O12 S1 41.5(10) . . . . ? N32 Cd2B O12 S1 -38.6(8) . . . . ? N52 Cd2B O12 S1 123.2(6) . . . . ? O22B Cd2B O12 S1 155(2) . . . . ? O12B Cd2B O12 S1 -41.7(16) . . . . ? O21B Cd2B O12 S1 49.9(8) . . . . ? O22B Cd2B O12 Cd2 179.7(10) 2_565 . . . ? O22 Cd2B O12 Cd2 -157.9(10) 2_565 . . . ? O21 Cd2B O12 Cd2 5.9(8) . . . . ? N32 Cd2B O12 Cd2 -74.3(10) . . . . ? N52 Cd2B O12 Cd2 87.5(8) . . . . ? O22B Cd2B O12 Cd2 119(3) . . . . ? O12B Cd2B O12 Cd2 -77.3(18) . . . . ? O21B Cd2B O12 Cd2 14.2(8) . . . . ? O14B S1 O12B Cd2 163(2) . . . . ? O12 S1 O12B Cd2 -64(2) . . . . ? O13 S1 O12B Cd2 -114.6(16) . . . . ? O11 S1 O12B Cd2 29(2) . . . . ? O14 S1 O12B Cd2 138.0(18) . . . . ? O13B S1 O12B Cd2 -86.9(18) . . . . ? O14B S1 O12B Cd2B 173(2) . . . . ? O12 S1 O12B Cd2B -55(2) . . . . ? O13 S1 O12B Cd2B -105(2) . . . . ? O11 S1 O12B Cd2B 39(2) . . . . ? O14 S1 O12B Cd2B 147(2) . . . . ? O13B S1 O12B Cd2B -78(2) . . . . ? N32 Cd2 O12B S1 -126.9(18) . . . . ? N52 Cd2 O12B S1 52.6(19) . . . . ? O21 Cd2 O12B S1 -74(3) . . . . ? O22B Cd2 O12B S1 143.5(17) 2_565 . . . ? O12 Cd2 O12B S1 56.9(19) . . . . ? O102 Cd2 O12B S1 -34.4(17) . . . . ? O22 Cd2 O12B S1 152.9(19) 2_565 . . . ? O21B Cd2 O12B S1 -49(2) . . . . ? N32 Cd2 O12B Cd2B 85.4(10) . . . . ? N52 Cd2 O12B Cd2B -95.1(9) . . . . ? O21 Cd2 O12B Cd2B 139(2) . . . . ? O22B Cd2 O12B Cd2B -4.2(9) 2_565 . . . ? O12 Cd2 O12B Cd2B -90.8(18) . . . . ? O102 Cd2 O12B Cd2B 178.0(10) . . . . ? O22 Cd2 O12B Cd2B 5.2(10) 2_565 . . . ? O21B Cd2 O12B Cd2B 163.0(16) . . . . ? O22B Cd2B O12B S1 134(2) 2_565 . . . ? O22 Cd2B O12B S1 146(2) 2_565 . . . ? O21 Cd2B O12B S1 -66(2) . . . . ? N32 Cd2B O12B S1 -127(2) . . . . ? N52 Cd2B O12B S1 35(2) . . . . ? O22B Cd2B O12B S1 -162(5) . . . . ? O12 Cd2B O12B S1 49.6(19) . . . . ? O21B Cd2B O12B S1 -52(2) . . . . ? O22B Cd2B O12B Cd2 174.6(11) 2_565 . . . ? O22 Cd2B O12B Cd2 -174.1(11) 2_565 . . . ? O21 Cd2B O12B Cd2 -25.8(13) . . . . ? N32 Cd2B O12B Cd2 -87.1(11) . . . . ? N52 Cd2B O12B Cd2 75.0(9) . . . . ? O22B Cd2B O12B Cd2 -122(7) . . . . ? O12 Cd2B O12B Cd2 89.7(19) . . . . ? O21B Cd2B O12B Cd2 -12.0(11) . . . . ? O24B S2 O21 O22B -96.1(8) . . . . ? O23B S2 O21 O22B 105.1(8) . . . . ? O22 S2 O21 O22B -17.0(7) . . . . ? O23 S2 O21 O22B 108.2(10) . . . . ? O21B S2 O21 O22B -146.8(18) . . . . ? O24 S2 O21 O22B -137.4(4) . . . . ? O24B S2 O21 Cd2B -79.9(14) . . . . ? O23B S2 O21 Cd2B 121.3(12) . . . . ? O22 S2 O21 Cd2B -0.8(14) . . . . ? O23 S2 O21 Cd2B 124.4(13) . . . . ? O21B S2 O21 Cd2B -131(2) . . . . ? O24 S2 O21 Cd2B -121.2(10) . . . . ? O22B S2 O21 Cd2B 16.2(9) . . . . ? O24B S2 O21 Cd2 -72.1(17) . . . . ? O23B S2 O21 Cd2 129.1(15) . . . . ? O22 S2 O21 Cd2 6.9(18) . . . . ? O23 S2 O21 Cd2 132.2(15) . . . . ? O21B S2 O21 Cd2 -123(3) . . . . ? O24 S2 O21 Cd2 -113.4(13) . . . . ? O22B S2 O21 Cd2 24.0(12) . . . . ? O22B Cd2B O21 S2 -24.9(12) 2_565 . . . ? O22 Cd2B O21 S2 -54.4(14) 2_565 . . . ? N32 Cd2B O21 S2 -126.8(12) . . . . ? N52 Cd2B O21 S2 74.1(12) . . . . ? O22B Cd2B O21 S2 -15.0(9) . . . . ? O12B Cd2B O21 S2 174.1(11) . . . . ? O12 Cd2B O21 S2 149.3(9) . . . . ? O21B Cd2B O21 S2 121(2) . . . . ? O22B Cd2B O21 O22B -9.9(6) 2_565 . . . ? O22 Cd2B O21 O22B -39.4(9) 2_565 . . . ? N32 Cd2B O21 O22B -111.8(6) . . . . ? N52 Cd2B O21 O22B 89.1(6) . . . . ? O12B Cd2B O21 O22B -171.0(8) . . . . ? O12 Cd2B O21 O22B 164.3(5) . . . . ? O21B Cd2B O21 O22B 136(2) . . . . ? O22B Cd2B O21 Cd2 -178.9(9) 2_565 . . . ? O22 Cd2B O21 Cd2 151.6(12) 2_565 . . . ? N32 Cd2B O21 Cd2 79.2(9) . . . . ? N52 Cd2B O21 Cd2 -79.9(7) . . . . ? O22B Cd2B O21 Cd2 -169.0(9) . . . . ? O12B Cd2B O21 Cd2 20.0(11) . . . . ? O12 Cd2B O21 Cd2 -4.7(6) . . . . ? O21B Cd2B O21 Cd2 -33(2) . . . . ? N32 Cd2 O21 S2 -123.1(15) . . . . ? O12B Cd2 O21 S2 -176.1(14) . . . . ? N52 Cd2 O21 S2 56.5(15) . . . . ? O22B Cd2 O21 S2 -30.9(15) 2_565 . . . ? O12 Cd2 O21 S2 138.8(12) . . . . ? O102 Cd2 O21 S2 144.6(15) . . . . ? O22 Cd2 O21 S2 -51.3(15) 2_565 . . . ? O21B Cd2 O21 S2 118(3) . . . . ? N32 Cd2 O21 O22B -102.0(5) . . . . ? O12B Cd2 O21 O22B -155.0(14) . . . . ? N52 Cd2 O21 O22B 77.6(5) . . . . ? O22B Cd2 O21 O22B -9.7(6) 2_565 . . . ? O12 Cd2 O21 O22B 159.9(8) . . . . ? O102 Cd2 O21 O22B 165.8(5) . . . . ? O22 Cd2 O21 O22B -30.1(6) 2_565 . . . ? O21B Cd2 O21 O22B 139(2) . . . . ? N32 Cd2 O21 Cd2B -91.4(8) . . . . ? O12B Cd2 O21 Cd2B -144.4(17) . . . . ? N52 Cd2 O21 Cd2B 88.2(7) . . . . ? O22B Cd2 O21 Cd2B 0.9(7) 2_565 . . . ? O12 Cd2 O21 Cd2B 170.5(13) . . . . ? O102 Cd2 O21 Cd2B 176.3(8) . . . . ? O22 Cd2 O21 Cd2B -19.5(8) 2_565 . . . ? O21B Cd2 O21 Cd2B 149(2) . . . . ? O21 S2 O21B Cd2 28.8(13) . . . . ? O24B S2 O21B Cd2 -112.0(6) . . . . ? O23B S2 O21B Cd2 110.1(10) . . . . ? O22 S2 O21B Cd2 -42.0(9) . . . . ? O23 S2 O21B Cd2 116.5(11) . . . . ? O24 S2 O21B Cd2 -142.1(6) . . . . ? O22B S2 O21B Cd2 -2.4(6) . . . . ? O21 S2 O21B Cd2B 28.8(14) . . . . ? O24B S2 O21B Cd2B -112.1(5) . . . . ? O23B S2 O21B Cd2B 110.1(9) . . . . ? O22 S2 O21B Cd2B -42.0(8) . . . . ? O23 S2 O21B Cd2B 116.5(11) . . . . ? O24 S2 O21B Cd2B -142.2(5) . . . . ? O22B S2 O21B Cd2B -2.5(5) . . . . ? N32 Cd2 O21B S2 -90.6(6) . . . . ? O12B Cd2 O21B S2 -165.5(10) . . . . ? N52 Cd2 O21B S2 88.5(6) . . . . ? O21 Cd2 O21B S2 -30.8(14) . . . . ? O22B Cd2 O21B S2 2.0(7) 2_565 . . . ? O12 Cd2 O21B S2 161.8(4) . . . . ? O102 Cd2 O21B S2 178.4(7) . . . . ? O22 Cd2 O21B S2 -17.0(9) 2_565 . . . ? N32 Cd2 O21B Cd2B -90.3(8) . . . . ? O12B Cd2 O21B Cd2B -165.2(14) . . . . ? N52 Cd2 O21B Cd2B 88.8(7) . . . . ? O21 Cd2 O21B Cd2B -30(2) . . . . ? O22B Cd2 O21B Cd2B 2.3(7) 2_565 . . . ? O12 Cd2 O21B Cd2B 162.1(10) . . . . ? O102 Cd2 O21B Cd2B 178.7(8) . . . . ? O22 Cd2 O21B Cd2B -16.7(8) 2_565 . . . ? O22B Cd2B O21B S2 2.8(7) 2_565 . . . ? O22 Cd2B O21B S2 -27.9(13) 2_565 . . . ? O21 Cd2B O21B S2 -34.6(16) . . . . ? N32 Cd2B O21B S2 -101.0(6) . . . . ? N52 Cd2B O21B S2 98.7(6) . . . . ? O22B Cd2B O21B S2 2.1(4) . . . . ? O12B Cd2B O21B S2 -170.6(7) . . . . ? O12 Cd2B O21B S2 168.0(4) . . . . ? O22B Cd2B O21B Cd2 -176.9(10) 2_565 . . . ? O22 Cd2B O21B Cd2 152.4(15) 2_565 . . . ? O21 Cd2B O21B Cd2 146(2) . . . . ? N32 Cd2B O21B Cd2 79.3(9) . . . . ? N52 Cd2B O21B Cd2 -81.0(7) . . . . ? O22B Cd2B O21B Cd2 -177.6(9) . . . . ? O12B Cd2B O21B Cd2 9.7(9) . . . . ? O12 Cd2B O21B Cd2 -11.8(7) . . . . ? O21 S2 O22 Cd2B 43.2(9) . . . 2_565 ? O24B S2 O22 Cd2B 164.7(7) . . . 2_565 ? O23B S2 O22 Cd2B -79.0(10) . . . 2_565 ? O23 S2 O22 Cd2B -86.0(11) . . . 2_565 ? O21B S2 O22 Cd2B 74.3(8) . . . 2_565 ? O24 S2 O22 Cd2B 165.7(5) . . . 2_565 ? O22B S2 O22 Cd2B 23.4(4) . . . 2_565 ? O21 S2 O22 Cd2 48.9(9) . . . 2_565 ? O24B S2 O22 Cd2 170.4(7) . . . 2_565 ? O23B S2 O22 Cd2 -73.3(10) . . . 2_565 ? O23 S2 O22 Cd2 -80.4(11) . . . 2_565 ? O21B S2 O22 Cd2 80.0(8) . . . 2_565 ? O24 S2 O22 Cd2 171.4(5) . . . 2_565 ? O22B S2 O22 Cd2 29.1(5) . . . 2_565 ? O24B S2 O22B O21 127.6(7) . . . . ? O23B S2 O22B O21 -100.9(12) . . . . ? O22 S2 O22B O21 162.6(7) . . . . ? O23 S2 O22B O21 -107.2(12) . . . . ? O21B S2 O22B O21 14.5(8) . . . . ? O24 S2 O22B O21 95.7(8) . . . . ? O21 S2 O22B Cd2B 166.8(9) . . . 2_565 ? O24B S2 O22B Cd2B -65.7(7) . . . 2_565 ? O23B S2 O22B Cd2B 65.9(12) . . . 2_565 ? O22 S2 O22B Cd2B -30.6(5) . . . 2_565 ? O23 S2 O22B Cd2B 59.6(12) . . . 2_565 ? O21B S2 O22B Cd2B -178.7(7) . . . 2_565 ? O24 S2 O22B Cd2B -97.5(7) . . . 2_565 ? O21 S2 O22B Cd2 166.2(8) . . . 2_565 ? O24B S2 O22B Cd2 -66.3(6) . . . 2_565 ? O23B S2 O22B Cd2 65.3(11) . . . 2_565 ? O22 S2 O22B Cd2 -31.2(5) . . . 2_565 ? O23 S2 O22B Cd2 59.0(12) . . . 2_565 ? O21B S2 O22B Cd2 -179.3(6) . . . 2_565 ? O24 S2 O22B Cd2 -98.1(7) . . . 2_565 ? O21 S2 O22B Cd2B -11.7(6) . . . . ? O24B S2 O22B Cd2B 115.9(5) . . . . ? O23B S2 O22B Cd2B -112.6(11) . . . . ? O22 S2 O22B Cd2B 150.9(6) . . . . ? O23 S2 O22B Cd2B -118.9(11) . . . . ? O21B S2 O22B Cd2B 2.8(6) . . . . ? O24 S2 O22B Cd2B 84.0(7) . . . . ? Cd2B O21 O22B S2 -167.6(6) . . . . ? Cd2 O21 O22B S2 -165.5(7) . . . . ? S2 O21 O22B Cd2B -89(3) . . . 2_565 ? Cd2B O21 O22B Cd2B 104(3) . . . 2_565 ? Cd2 O21 O22B Cd2B 106(3) . . . 2_565 ? S2 O21 O22B Cd2 -77(3) . . . 2_565 ? Cd2B O21 O22B Cd2 115(3) . . . 2_565 ? Cd2 O21 O22B Cd2 117(3) . . . 2_565 ? S2 O21 O22B Cd2B 167.6(6) . . . . ? Cd2 O21 O22B Cd2B 2.08(16) . . . . ? O22B Cd2B O22B S2 178.7(7) 2_565 . . . ? O22 Cd2B O22B S2 163.5(4) 2_565 . . . ? O21 Cd2B O22B S2 9.6(5) . . . . ? N32 Cd2B O22B S2 78.2(5) . . . . ? N52 Cd2B O22B S2 -84.7(5) . . . . ? O12B Cd2B O22B S2 112(6) . . . . ? O12 Cd2B O22B S2 -115(3) . . . . ? O21B Cd2B O22B S2 -2.0(4) . . . . ? O22B Cd2B O22B O21 169.1(7) 2_565 . . . ? O22 Cd2B O22B O21 153.9(5) 2_565 . . . ? N32 Cd2B O22B O21 68.5(6) . . . . ? N52 Cd2B O22B O21 -94.3(6) . . . . ? O12B Cd2B O22B O21 103(6) . . . . ? O12 Cd2B O22B O21 -125(3) . . . . ? O21B Cd2B O22B O21 -11.6(6) . . . . ? O22B Cd2B O22B Cd2B 0.0 2_565 . . 2_565 ? O22 Cd2B O22B Cd2B -15.2(4) 2_565 . . 2_565 ? O21 Cd2B O22B Cd2B -169.1(7) . . . 2_565 ? N32 Cd2B O22B Cd2B -100.5(5) . . . 2_565 ? N52 Cd2B O22B Cd2B 96.6(5) . . . 2_565 ? O12B Cd2B O22B Cd2B -66(6) . . . 2_565 ? O12 Cd2B O22B Cd2B 66(3) . . . 2_565 ? O21B Cd2B O22B Cd2B 179.3(6) . . . 2_565 ? O22B Cd2B O22B Cd2 0.60(18) 2_565 . . 2_565 ? O22 Cd2B O22B Cd2 -14.6(5) 2_565 . . 2_565 ? O21 Cd2B O22B Cd2 -168.5(7) . . . 2_565 ? N32 Cd2B O22B Cd2 -99.9(5) . . . 2_565 ? N52 Cd2B O22B Cd2 97.2(5) . . . 2_565 ? O12B Cd2B O22B Cd2 -66(6) . . . 2_565 ? O12 Cd2B O22B Cd2 67(3) . . . 2_565 ? O21B Cd2B O22B Cd2 179.9(6) . . . 2_565 ? N12 Cd1 O101 C101 -19.3(13) . . . . ? N12 Cd1 O101 C101 160.7(13) 2_656 . . . ? O11 Cd1 O101 C101 -108.1(13) . . . . ? O11 Cd1 O101 C101 71.9(13) 2_656 . . . ? O101 Cd1 O101 C101 73(10) 2_656 . . . ? N12 Cd1 N12 C12 180(8) 2_656 . . . ? O11 Cd1 N12 C12 25.8(4) . . . . ? O11 Cd1 N12 C12 -154.2(4) 2_656 . . . ? O101 Cd1 N12 C12 -64.9(4) . . . . ? O101 Cd1 N12 C12 115.1(4) 2_656 . . . ? N12 Cd1 N12 C13 -7(8) 2_656 . . . ? O11 Cd1 N12 C13 -160.7(4) . . . . ? O11 Cd1 N12 C13 19.3(4) 2_656 . . . ? O101 Cd1 N12 C13 108.6(4) . . . . ? O101 Cd1 N12 C13 -71.4(4) 2_656 . . . ? O12B Cd2 N32 C32 26.7(6) . . . . ? N52 Cd2 N32 C32 -142(9) . . . . ? O21 Cd2 N32 C32 -132.0(6) . . . . ? O22B Cd2 N32 C32 136.3(4) 2_565 . . . ? O12 Cd2 N32 C32 27.9(5) . . . . ? O102 Cd2 N32 C32 -52.1(4) . . . . ? O22 Cd2 N32 C32 104.7(5) 2_565 . . . ? O21B Cd2 N32 C32 -118.8(5) . . . . ? O12B Cd2 N32 C33 -153.5(6) . . . . ? N52 Cd2 N32 C33 38(9) . . . . ? O21 Cd2 N32 C33 47.8(6) . . . . ? O22B Cd2 N32 C33 -43.9(4) 2_565 . . . ? O12 Cd2 N32 C33 -152.3(4) . . . . ? O102 Cd2 N32 C33 127.7(4) . . . . ? O22 Cd2 N32 C33 -75.5(4) 2_565 . . . ? O21B Cd2 N32 C33 60.9(5) . . . . ? O12B Cd2 N32 Cd2B -119.9(9) . . . . ? N52 Cd2 N32 Cd2B 72(9) . . . . ? O21 Cd2 N32 Cd2B 81.4(9) . . . . ? O22B Cd2 N32 Cd2B -10.3(7) 2_565 . . . ? O12 Cd2 N32 Cd2B -118.7(7) . . . . ? O102 Cd2 N32 Cd2B 161.4(8) . . . . ? O22 Cd2 N32 Cd2B -41.9(7) 2_565 . . . ? O21B Cd2 N32 Cd2B 94.6(8) . . . . ? O22B Cd2B N32 C32 128.4(6) 2_565 . . . ? O22 Cd2B N32 C32 93.2(7) 2_565 . . . ? O21 Cd2B N32 C32 -127.9(6) . . . . ? N52 Cd2B N32 C32 -44.8(9) . . . . ? O22B Cd2B N32 C32 -169.3(5) . . . . ? O12B Cd2B N32 C32 14.4(8) . . . . ? O12 Cd2B N32 C32 13.5(7) . . . . ? O21B Cd2B N32 C32 -115.2(5) . . . . ? O22B Cd2B N32 C33 -42.7(4) 2_565 . . . ? O22 Cd2B N32 C33 -77.8(4) 2_565 . . . ? O21 Cd2B N32 C33 61.1(7) . . . . ? N52 Cd2B N32 C33 144.2(6) . . . . ? O22B Cd2B N32 C33 19.6(6) . . . . ? O12B Cd2B N32 C33 -156.7(6) . . . . ? O12 Cd2B N32 C33 -157.6(4) . . . . ? O21B Cd2B N32 C33 73.8(6) . . . . ? O22B Cd2B N32 Cd2 167.1(9) 2_565 . . . ? O22 Cd2B N32 Cd2 132.0(8) 2_565 . . . ? O21 Cd2B N32 Cd2 -89.1(10) . . . . ? N52 Cd2B N32 Cd2 -6.0(5) . . . . ? O22B Cd2B N32 Cd2 -130.6(10) . . . . ? O12B Cd2B N32 Cd2 53.1(8) . . . . ? O12 Cd2B N32 Cd2 52.2(7) . . . . ? O21B Cd2B N32 Cd2 -76.4(9) . . . . ? N32 Cd2 N52 C52 25(9) . . . . ? O12B Cd2 N52 C52 -142.8(6) . . . . ? O21 Cd2 N52 C52 15.9(6) . . . . ? O22B Cd2 N52 C52 107.7(4) 2_565 . . . ? O12 Cd2 N52 C52 -144.1(4) . . . . ? O102 Cd2 N52 C52 -64.1(5) . . . . ? O22 Cd2 N52 C52 138.7(4) 2_565 . . . ? O21B Cd2 N52 C52 2.7(5) . . . . ? N32 Cd2 N52 C53 -161(8) . . . . ? O12B Cd2 N52 C53 30.9(7) . . . . ? O21 Cd2 N52 C53 -170.4(5) . . . . ? O22B Cd2 N52 C53 -78.6(4) 2_565 . . . ? O12 Cd2 N52 C53 29.6(4) . . . . ? O102 Cd2 N52 C53 109.6(4) . . . . ? O22 Cd2 N52 C53 -47.6(5) 2_565 . . . ? O21B Cd2 N52 C53 176.4(4) . . . . ? N32 Cd2 N52 Cd2B -72(9) . . . . ? O12B Cd2 N52 Cd2B 119.9(9) . . . . ? O21 Cd2 N52 Cd2B -81.4(9) . . . . ? O22B Cd2 N52 Cd2B 10.3(7) 2_565 . . . ? O12 Cd2 N52 Cd2B 118.6(8) . . . . ? O102 Cd2 N52 Cd2B -161.4(8) . . . . ? O22 Cd2 N52 Cd2B 41.4(7) 2_565 . . . ? O21B Cd2 N52 Cd2B -94.6(8) . . . . ? O22B Cd2B N52 C52 102.0(5) 2_565 . . . ? O22 Cd2B N52 C52 140.8(4) 2_565 . . . ? O21 Cd2B N52 C52 -4.1(9) . . . . ? N32 Cd2B N52 C52 -84.7(8) . . . . ? O22B Cd2B N52 C52 40.8(7) . . . . ? O12B Cd2B N52 C52 -141.1(6) . . . . ? O12 Cd2B N52 C52 -145.5(4) . . . . ? O21B Cd2B N52 C52 -14.1(7) . . . . ? O22B Cd2B N52 C53 -68.2(5) 2_565 . . . ? O22 Cd2B N52 C53 -29.4(8) 2_565 . . . ? O21 Cd2B N52 C53 -174.3(5) . . . . ? N32 Cd2B N52 C53 105.1(7) . . . . ? O22B Cd2B N52 C53 -129.5(4) . . . . ? O12B Cd2B N52 C53 48.7(8) . . . . ? O12 Cd2B N52 C53 44.3(6) . . . . ? O21B Cd2B N52 C53 175.7(4) . . . . ? O22B Cd2B N52 Cd2 -167.3(9) 2_565 . . . ? O22 Cd2B N52 Cd2 -128.5(8) 2_565 . . . ? O21 Cd2B N52 Cd2 86.6(10) . . . . ? N32 Cd2B N52 Cd2 6.0(5) . . . . ? O22B Cd2B N52 Cd2 131.5(10) . . . . ? O12B Cd2B N52 Cd2 -50.4(8) . . . . ? O12 Cd2B N52 Cd2 -54.8(7) . . . . ? O21B Cd2B N52 Cd2 76.7(9) . . . . ? C6 C1 C2 C3 7.2(6) . . . . ? C11 C1 C2 C3 -173.2(4) . . . . ? C6 C1 C2 C21 -171.2(4) . . . . ? C11 C1 C2 C21 8.4(6) . . . . ? C1 C2 C3 C4 -4.2(6) . . . . ? C21 C2 C3 C4 174.2(4) . . . . ? C1 C2 C3 C31 176.8(4) . . . . ? C21 C2 C3 C31 -4.8(6) . . . . ? C2 C3 C4 C5 -2.5(6) . . . . ? C31 C3 C4 C5 176.5(4) . . . . ? C2 C3 C4 C41 -179.8(4) . . . . ? C31 C3 C4 C41 -0.8(6) . . . . ? C3 C4 C5 C6 6.3(6) . . . . ? C41 C4 C5 C6 -176.5(4) . . . . ? C3 C4 C5 C51 -171.3(4) . . . . ? C41 C4 C5 C51 6.0(6) . . . . ? C4 C5 C6 C1 -3.3(6) . . . . ? C51 C5 C6 C1 174.2(4) . . . . ? C4 C5 C6 C61 178.7(5) . . . . ? C51 C5 C6 C61 -3.8(6) . . . . ? C2 C1 C6 C5 -3.5(6) . . . . ? C11 C1 C6 C5 176.9(4) . . . . ? C2 C1 C6 C61 174.5(5) . . . . ? C11 C1 C6 C61 -5.1(7) . . . . ? C12 N11 C11 C1 -4.7(7) . . . . ? C14 N11 C11 C1 176.9(4) . . . . ? C2 C1 C11 N11 -87.4(5) . . . . ? C6 C1 C11 N11 92.3(5) . . . . ? C13 N12 C12 N11 0.1(5) . . . . ? Cd1 N12 C12 N11 174.9(3) . . . . ? C14 N11 C12 N12 0.6(6) . . . . ? C11 N11 C12 N12 -178.1(4) . . . . ? C12 N12 C13 C14 -0.8(6) . . . . ? Cd1 N12 C13 C14 -175.2(4) . . . . ? N12 C13 C14 N11 1.1(6) . . . . ? C12 N11 C14 C13 -1.0(6) . . . . ? C11 N11 C14 C13 177.6(5) . . . . ? C32 N31 C31 C3 -29.6(7) . . . . ? C34 N31 C31 C3 154.3(4) . . . . ? C2 C3 C31 N31 105.3(5) . . . . ? C4 C3 C31 N31 -73.7(5) . . . . ? C33 N32 C32 N31 0.9(5) . . . . ? Cd2 N32 C32 N31 -179.3(3) . . . . ? Cd2B N32 C32 N31 -171.0(5) . . . . ? C34 N31 C32 N32 -0.7(5) . . . . ? C31 N31 C32 N32 -177.4(4) . . . . ? C32 N32 C33 C34 -0.7(5) . . . . ? Cd2 N32 C33 C34 179.4(3) . . . . ? Cd2B N32 C33 C34 172.6(4) . . . . ? N32 C33 C34 N31 0.3(5) . . . . ? C32 N31 C34 C33 0.2(5) . . . . ? C31 N31 C34 C33 176.9(4) . . . . ? C4 C5 C51 N51 -96.3(5) . . . 1_655 ? C6 C5 C51 N51 86.2(5) . . . 1_655 ? C53 N52 C52 N51 -1.0(5) . . . . ? Cd2 N52 C52 N51 173.7(4) . . . . ? Cd2B N52 C52 N51 -172.8(5) . . . . ? C54 N51 C52 N52 1.1(6) . . . . ? C51 N51 C52 N52 176.6(4) 1_455 . . . ? C52 N52 C53 C54 0.6(5) . . . . ? Cd2 N52 C53 C54 -174.2(4) . . . . ? Cd2B N52 C53 C54 172.4(5) . . . . ? N52 C53 C54 N51 0.1(5) . . . . ? C52 N51 C54 C53 -0.7(5) . . . . ? C51 N51 C54 C53 -176.3(4) 1_455 . . . ? Cd1 O101 C101 C102 -94(3) . . . . ? Cd1 O101 C101 C103 -163(2) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.782 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.131 #========END