# 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_DiOBuDMF _database_code_depnum_ccdc_archive 'CCDC 910962' #TrackingRef '3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DiOBuDMF _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H47 N O9' _chemical_formula_weight 697.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.4651(9) _cell_length_b 21.2583(18) _cell_length_c 15.0509(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.064(4) _cell_angle_gamma 90.00 _cell_volume 3659.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3711 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.82 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9611 _exptl_absorpt_correction_T_max 0.9738 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD Diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15103 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3600 _reflns_number_gt 2632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. There is disorder associated with teh dmf molecule as is sits on a special position. This has been successfully modelled with partial occupancies of 50% where appropriate. The list of instructions / restraints are as follows: EQIV $1 -X,Y,1/2-Z FREE C21 C23_$1 FREE C23 C21_$1 FREE C21 O5_$1 FREE O5 C21_$1 EADP C20 C21 C23 N1 O5 FREE H21C O5_$1 FREE H21A C23_$1 FREE H21C C23_$1 FREE C23 H21A_$1 FREE C23 H21C_$1 FREE H23 C21_$1 FREE H23_$1 C21 ; _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^)+(0.0705P)^2^+4.7650P] 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 3600 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 O1 O 0.12524(13) 0.26643(7) 0.32334(10) 0.0263(4) Uani 1 1 d . . . H1O H 0.0584 0.2663 0.3428 0.032 Uiso 1 1 calc R . . C1 C 0.16654(17) 0.19095(10) 0.44213(13) 0.0202(4) Uani 1 1 d . . . O2 O 0.09380(12) 0.27938(6) 0.12908(9) 0.0196(3) Uani 1 1 d . . . C2 C 0.23717(18) 0.14159(9) 0.47361(13) 0.0207(4) Uani 1 1 d . . . H2 H 0.2225 0.1221 0.5285 0.025 Uiso 1 1 calc R . . O3 O 0.37007(13) 0.03740(7) 0.52586(10) 0.0291(4) Uani 1 1 d . . . H3O H 0.4173 0.0082 0.5396 0.035 Uiso 1 1 calc R . . C3 C 0.32929(18) 0.12006(9) 0.42602(13) 0.0208(5) Uani 1 1 d . . . O4 O 0.49324(13) 0.05309(7) 0.41908(10) 0.0293(4) Uani 1 1 d . . . C4 C 0.35103(18) 0.14866(10) 0.34542(13) 0.0211(4) Uani 1 1 d . . . H4 H 0.4148 0.1345 0.3137 0.025 Uiso 1 1 calc R . . C5 C 0.28169(17) 0.19713(10) 0.31085(13) 0.0204(4) Uani 1 1 d . . . C6 C 0.18865(18) 0.21814(9) 0.35978(14) 0.0205(4) Uani 1 1 d . . . C7 C 0.30008(18) 0.22471(10) 0.21972(14) 0.0232(5) Uani 1 1 d . . . H7A H 0.2798 0.2700 0.2193 0.028 Uiso 1 1 calc R . . H7B H 0.3835 0.2208 0.2075 0.028 Uiso 1 1 calc R . . C8 C 0.22522(18) 0.19113(10) 0.14731(13) 0.0214(5) Uani 1 1 d . . . C9 C 0.2524(2) 0.12944(10) 0.12344(14) 0.0260(5) Uani 1 1 d . . . H9 H 0.3202 0.1097 0.1506 0.031 Uiso 1 1 calc R . . C10 C 0.1815(2) 0.09678(10) 0.06054(15) 0.0281(5) Uani 1 1 d . . . H10 H 0.2018 0.0552 0.0443 0.034 Uiso 1 1 calc R . . C11 C 0.08147(19) 0.12438(10) 0.02154(14) 0.0238(5) Uani 1 1 d . . . H11 H 0.0332 0.1015 -0.0210 0.029 Uiso 1 1 calc R . . C12 C 0.05038(18) 0.18576(9) 0.04393(13) 0.0209(4) Uani 1 1 d . . . C13 C 0.12468(18) 0.21832(9) 0.10533(13) 0.0190(4) Uani 1 1 d . . . C14 C -0.06488(18) 0.21309(10) 0.00604(13) 0.0214(5) Uani 1 1 d . . . H14A H -0.0787 0.2003 -0.0571 0.026 Uiso 1 1 calc R . . H14B H -0.0606 0.2596 0.0081 0.026 Uiso 1 1 calc R . . C15 C 0.40344(18) 0.06669(10) 0.45908(13) 0.0206(4) Uani 1 1 d . . . C16 C 0.14317(19) 0.32863(9) 0.07598(14) 0.0232(5) Uani 1 1 d . . . H16A H 0.1036 0.3291 0.0154 0.028 Uiso 1 1 calc R . . H16B H 0.2275 0.3208 0.0707 0.028 Uiso 1 1 calc R . . C17 C 0.1261(2) 0.39104(10) 0.12139(14) 0.0259(5) Uani 1 1 d . . . H17A H 0.0424 0.3954 0.1326 0.031 Uiso 1 1 calc R . . H17B H 0.1455 0.4251 0.0801 0.031 Uiso 1 1 calc R . . C18 C 0.1985(2) 0.40017(11) 0.20886(16) 0.0360(6) Uani 1 1 d . . . H18A H 0.2816 0.3914 0.1996 0.043 Uiso 1 1 calc R . . H18B H 0.1727 0.3695 0.2529 0.043 Uiso 1 1 calc R . . C19 C 0.1881(3) 0.46663(12) 0.24640(18) 0.0466(7) Uani 1 1 d . . . H19A H 0.2144 0.4972 0.2034 0.070 Uiso 1 1 calc R . . H19B H 0.2369 0.4701 0.3023 0.070 Uiso 1 1 calc R . . H19C H 0.1064 0.4751 0.2575 0.070 Uiso 1 1 calc R . . N1 N 0.0000 0.02015(15) 0.2500 0.0481(5) Uani 1 2 d S . . C20 C 0.0000 0.08669(18) 0.2500 0.0481(5) Uani 1 2 d S . . H20A H -0.0075 0.1021 0.3107 0.072 Uiso 0.50 1 calc PR . . H20B H -0.0659 0.1021 0.2109 0.072 Uiso 0.50 1 calc PR . . H20C H 0.0734 0.1021 0.2283 0.072 Uiso 0.50 1 calc PR . . C21 C -0.0387(6) -0.0026(3) 0.1641(4) 0.0481(5) Uani 0.50 1 d P . . H21A H 0.0249 0.0009 0.1242 0.072 Uiso 0.50 1 calc PR . . H21B H -0.1058 0.0223 0.1404 0.072 Uiso 0.50 1 calc PR . . H21C H -0.0619 -0.0468 0.1686 0.072 Uiso 0.50 1 calc PR . . O5 O -0.0311(4) -0.07444(17) 0.3223(2) 0.0481(5) Uani 0.50 1 d P . . C23 C -0.0091(6) -0.0203(3) 0.3239(4) 0.0481(5) Uani 0.50 1 d P . . H23 H 0.0040 -0.0017 0.3812 0.058 Uiso 0.50 1 calc PR . . 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 O1 0.0228(8) 0.0262(8) 0.0311(8) 0.0109(6) 0.0095(6) 0.0077(6) C1 0.0201(10) 0.0185(10) 0.0220(10) -0.0013(8) 0.0011(8) -0.0018(8) O2 0.0210(7) 0.0146(7) 0.0240(7) 0.0033(6) 0.0078(6) 0.0010(6) C2 0.0220(11) 0.0183(10) 0.0214(10) 0.0005(8) -0.0004(8) -0.0030(9) O3 0.0271(8) 0.0249(8) 0.0350(9) 0.0070(7) -0.0003(7) 0.0048(7) C3 0.0196(11) 0.0173(10) 0.0249(10) -0.0012(8) -0.0038(8) -0.0012(8) O4 0.0242(8) 0.0280(9) 0.0359(9) 0.0050(7) 0.0026(7) 0.0031(7) C4 0.0175(10) 0.0211(11) 0.0248(10) -0.0007(8) 0.0023(8) 0.0001(9) C5 0.0176(10) 0.0202(10) 0.0237(10) 0.0024(8) 0.0025(8) -0.0013(8) C6 0.0188(10) 0.0178(10) 0.0248(10) 0.0013(8) 0.0002(8) -0.0012(8) C7 0.0168(11) 0.0242(11) 0.0292(11) 0.0056(9) 0.0068(9) 0.0012(9) C8 0.0211(11) 0.0220(11) 0.0223(10) 0.0052(8) 0.0105(8) 0.0016(9) C9 0.0275(12) 0.0244(11) 0.0275(11) 0.0062(9) 0.0122(9) 0.0089(9) C10 0.0379(13) 0.0185(11) 0.0300(11) 0.0019(9) 0.0183(10) 0.0035(10) C11 0.0287(12) 0.0197(11) 0.0243(10) -0.0003(9) 0.0111(9) -0.0006(9) C12 0.0245(11) 0.0189(10) 0.0205(10) 0.0039(8) 0.0108(8) -0.0011(9) C13 0.0207(10) 0.0168(10) 0.0207(10) 0.0036(8) 0.0106(8) 0.0013(8) C14 0.0258(11) 0.0193(11) 0.0196(10) -0.0001(8) 0.0040(8) -0.0017(9) C15 0.0163(10) 0.0203(11) 0.0251(11) -0.0038(8) 0.0001(8) -0.0019(8) C16 0.0260(11) 0.0186(11) 0.0259(11) 0.0064(9) 0.0081(9) -0.0009(9) C17 0.0294(12) 0.0185(11) 0.0303(11) 0.0048(9) 0.0056(9) 0.0005(9) C18 0.0475(16) 0.0213(12) 0.0383(13) 0.0056(10) -0.0038(11) -0.0034(11) C19 0.071(2) 0.0283(14) 0.0386(14) -0.0027(11) -0.0093(13) -0.0017(13) N1 0.0653(14) 0.0353(10) 0.0454(10) 0.000 0.0164(10) 0.000 C20 0.0653(14) 0.0353(10) 0.0454(10) 0.000 0.0164(10) 0.000 C21 0.0653(14) 0.0353(10) 0.0454(10) 0.000 0.0164(10) 0.000 O5 0.0653(14) 0.0353(10) 0.0454(10) 0.000 0.0164(10) 0.000 C23 0.0653(14) 0.0353(10) 0.0454(10) 0.000 0.0164(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C6 1.352(2) . ? C1 C2 1.388(3) . ? C1 C6 1.407(3) . ? C1 C14 1.522(3) 2 ? O2 C13 1.398(2) . ? O2 C16 1.456(2) . ? C2 C3 1.395(3) . ? O3 C15 1.264(2) . ? C3 C4 1.395(3) . ? C3 C15 1.482(3) . ? O4 C15 1.263(2) . ? C4 C5 1.380(3) . ? C5 C6 1.411(3) . ? C5 C7 1.520(3) . ? C7 C8 1.517(3) . ? C8 C13 1.400(3) . ? C8 C9 1.401(3) . ? C9 C10 1.390(3) . ? C10 C11 1.381(3) . ? C11 C12 1.400(3) . ? C12 C13 1.395(3) . ? C12 C14 1.517(3) . ? C14 C1 1.522(3) 2 ? C16 C17 1.511(3) . ? C17 C18 1.518(3) . ? C18 C19 1.529(3) . ? N1 C20 1.414(5) . ? N1 C23 1.416(6) 2 ? N1 C23 1.416(6) . ? N1 C21 1.422(6) . ? N1 C21 1.422(6) 2 ? O5 C23 1.178(7) . ? 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 C2 C1 C6 118.31(18) . . ? C2 C1 C14 120.53(18) . 2 ? C6 C1 C14 121.12(18) . 2 ? C13 O2 C16 114.32(14) . . ? C1 C2 C3 121.16(19) . . ? C2 C3 C4 119.47(19) . . ? C2 C3 C15 121.06(18) . . ? C4 C3 C15 119.47(18) . . ? C5 C4 C3 121.30(19) . . ? C4 C5 C6 118.43(18) . . ? C4 C5 C7 121.00(18) . . ? C6 C5 C7 120.47(18) . . ? O1 C6 C1 122.98(18) . . ? O1 C6 C5 115.69(17) . . ? C1 C6 C5 121.32(19) . . ? C8 C7 C5 111.05(16) . . ? C13 C8 C9 117.5(2) . . ? C13 C8 C7 122.41(18) . . ? C9 C8 C7 119.99(19) . . ? C10 C9 C8 120.8(2) . . ? C11 C10 C9 120.4(2) . . ? C10 C11 C12 120.8(2) . . ? C13 C12 C11 117.89(19) . . ? C13 C12 C14 122.24(18) . . ? C11 C12 C14 119.75(19) . . ? C12 C13 O2 118.42(18) . . ? C12 C13 C8 122.59(19) . . ? O2 C13 C8 118.90(18) . . ? C12 C14 C1 111.54(16) . 2 ? O4 C15 O3 124.70(19) . . ? O4 C15 C3 118.87(18) . . ? O3 C15 C3 116.43(18) . . ? O2 C16 C17 108.37(16) . . ? C16 C17 C18 115.10(19) . . ? C17 C18 C19 112.7(2) . . ? C20 N1 C23 127.4(3) . 2 ? C20 N1 C23 127.4(3) . . ? C23 N1 C23 105.2(5) 2 . ? C20 N1 C21 109.9(3) . . ? C23 N1 C21 27.7(3) 2 . ? C23 N1 C21 118.2(4) . . ? C20 N1 C21 109.9(3) . 2 ? C23 N1 C21 118.2(4) 2 2 ? C23 N1 C21 27.7(3) . 2 ? C21 N1 C21 140.2(5) . 2 ? O5 C23 N1 127.2(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.666 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.057 data_PCH163 _database_code_depnum_ccdc_archive 'CCDC 910963' #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PCH163 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H62 Cd N4 O11' _chemical_formula_weight 1079.50 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9671(5) _cell_length_b 14.2215(6) _cell_length_c 18.5034(8) _cell_angle_alpha 110.695(2) _cell_angle_beta 90.387(2) _cell_angle_gamma 106.035(2) _cell_volume 2577.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9970 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 35.64 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9903 _exptl_absorpt_correction_T_max 0.9951 _exptl_absorpt_process_details 'SADABS 2004/1 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD Diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44494 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 36.06 _reflns_number_total 18545 _reflns_number_gt 13353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAITN' _computing_data_reduction 'Bruker SAITN' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'local program' _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. There was disorder present in the solvent ligand of the Cd centre and this was modelled at partial occupancy of 50% in each case as water and DMF. Additional disordered DMF was located and refined as well as another 50% occupancy water molecule. Despite the ability to model most of the disorder one DMF molecule could not be modelled aprpopriately. Given this the routine SQUEEZE was applied to the data. This had the effect of markedly improving the agreement indices. SQUEEZE suggested an electron count a little greater than that of DMF, suggesting validity of the model. Calculated and reported formulae differ due to the application of SQUEEZE and the H atoms of ligated and free H2O. Restraints used in refinement are listed below. DFIX 1.2 0.02 O9 C51 DFIX 1.2 0.02 C54 O11 DFIX 1.35 0.02 C51 N3 DFIX 1.35 0.02 N4 C54 DFIX 1.45 0.02 C52 N3 DFIX 1.45 0.02 N3 C53 DFIX 1.45 0.02 N4 C56 DFIX 1.45 0.02 N4 C55 EADP O9 O10 O11 O12 C51 C52 C53 C54 C55 C56 N3 N4 ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18545 _refine_ls_number_parameters 594 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1980 _refine_ls_wR_factor_gt 0.1850 _refine_ls_goodness_of_fit_ref 1.275 _refine_ls_restrained_S_all 1.277 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.869900(19) 0.707428(18) 0.565488(12) 0.03577(8) Uani 1 1 d . . . O1 O 1.56232(18) 1.10171(18) 0.82415(13) 0.0370(5) Uani 1 1 d . . . H1 H 1.6252 1.0832 0.8052 0.044 Uiso 1 1 calc R . . O2 O 1.78342(17) 1.11288(18) 0.76392(12) 0.0345(4) Uani 1 1 d . . . O3 O 1.77236(18) 1.32784(17) 0.83155(12) 0.0322(4) Uani 1 1 d . . . H3 H 1.7282 1.3464 0.8679 0.039 Uiso 1 1 calc R . . O4 O 1.58331(17) 1.32336(15) 0.92548(11) 0.0285(4) Uani 1 1 d . . . O5 O 0.99665(18) 0.86213(19) 0.66544(14) 0.0389(5) Uani 1 1 d . A . O6 O 1.09647(19) 0.77483(16) 0.57478(13) 0.0341(4) Uani 1 1 d . A . O7 O 1.8961(4) 1.5602(3) 0.5930(2) 0.0858(13) Uani 1 1 d . . . O8 O 1.7889(4) 1.6549(3) 0.6678(2) 0.0817(12) Uani 1 1 d . . . O9 O 0.8428(7) 0.5962(5) 0.4373(4) 0.0592(5) Uani 0.50 1 d PD A 2 O10 O 0.8773(7) 0.5770(6) 0.4438(4) 0.0592(5) Uani 0.50 1 d P A 1 O11 O 0.6969(7) 0.4672(6) 0.3122(4) 0.0592(5) Uani 0.50 1 d PD B 1 N1 N 0.8408(2) 0.8027(2) 0.48799(14) 0.0314(5) Uani 1 1 d . A . N2 N 0.6486(2) 0.6848(2) 0.53863(17) 0.0427(6) Uani 1 1 d . A . N3 N 0.8032(7) 0.4399(6) 0.3393(4) 0.0592(5) Uani 0.50 1 d PD A 2 N4 N 0.7088(7) 0.3089(6) 0.2392(4) 0.0592(5) Uani 0.50 1 d PD B 1 C1 C 1.3412(2) 1.0583(2) 0.80180(16) 0.0281(5) Uani 1 1 d . . . C2 C 1.2260(2) 0.9937(2) 0.75721(16) 0.0278(5) Uani 1 1 d . A . H2 H 1.1482 1.0047 0.7752 0.033 Uiso 1 1 calc R . . C3 C 1.2227(2) 0.9134(2) 0.68688(16) 0.0266(5) Uani 1 1 d . . . C4 C 1.3363(2) 0.8956(2) 0.66186(17) 0.0294(5) Uani 1 1 d . A . H4 H 1.3340 0.8409 0.6136 0.035 Uiso 1 1 calc R . . C5 C 1.4538(2) 0.9566(2) 0.70628(17) 0.0306(5) Uani 1 1 d . . . C6 C 1.4544(2) 1.0391(2) 0.77621(16) 0.0300(5) Uani 1 1 d . A . C7 C 1.5762(3) 0.9335(3) 0.6786(2) 0.0388(7) Uani 1 1 d . A . H7A H 1.6299 0.9367 0.7231 0.047 Uiso 1 1 calc R . . H7B H 1.5546 0.8611 0.6393 0.047 Uiso 1 1 calc R . . C8 C 1.6522(2) 1.0094(3) 0.64354(17) 0.0351(6) Uani 1 1 d . . . C9 C 1.6216(3) 0.9940(3) 0.56616(19) 0.0399(7) Uani 1 1 d . A . H9 H 1.5555 0.9334 0.5347 0.048 Uiso 1 1 calc R . . C10 C 1.6859(3) 1.0653(3) 0.53459(18) 0.0398(7) Uani 1 1 d . . . H10 H 1.6665 1.0520 0.4811 0.048 Uiso 1 1 calc R A . C11 C 1.7781(3) 1.1561(3) 0.58033(17) 0.0385(7) Uani 1 1 d . A . H11 H 1.8187 1.2068 0.5588 0.046 Uiso 1 1 calc R . . C12 C 1.8127(2) 1.1744(3) 0.65831(17) 0.0365(6) Uani 1 1 d . . . C13 C 1.7512(2) 1.0991(3) 0.68730(16) 0.0343(6) Uani 1 1 d . A . C14 C 1.9105(2) 1.2771(3) 0.70786(18) 0.0415(7) Uani 1 1 d . A . H14A H 1.9388 1.2717 0.7568 0.050 Uiso 1 1 calc R . . H14B H 1.9860 1.2900 0.6797 0.050 Uiso 1 1 calc R . . C15 C 1.8562(2) 1.3683(3) 0.72681(17) 0.0375(6) Uani 1 1 d . . . C16 C 1.8724(3) 1.4320(3) 0.68222(19) 0.0493(9) Uani 1 1 d . A . H16 H 1.9221 1.4191 0.6399 0.059 Uiso 1 1 calc R . . C17 C 1.8174(3) 1.5135(3) 0.6984(2) 0.0494(9) Uani 1 1 d . . . C18 C 1.7462(3) 1.5309(3) 0.7593(2) 0.0439(7) Uani 1 1 d . A . H18 H 1.7079 1.5860 0.7702 0.053 Uiso 1 1 calc R . . C19 C 1.7273(3) 1.4708(2) 0.80600(18) 0.0352(6) Uani 1 1 d . . . C20 C 1.7827(2) 1.3899(2) 0.78900(16) 0.0323(5) Uani 1 1 d . A . C21 C 1.6469(3) 1.4935(2) 0.87159(19) 0.0366(6) Uani 1 1 d . A . H21A H 1.6370 1.5643 0.8834 0.044 Uiso 1 1 calc R . . H21B H 1.6913 1.4941 0.9186 0.044 Uiso 1 1 calc R . . C22 C 1.5160(3) 1.4133(2) 0.85307(17) 0.0325(5) Uani 1 1 d . . . C23 C 1.4210(3) 1.4210(3) 0.80699(19) 0.0374(6) Uani 1 1 d . A . H23 H 1.4383 1.4771 0.7883 0.045 Uiso 1 1 calc R . . C24 C 1.3014(3) 1.3472(3) 0.7883(2) 0.0386(6) Uani 1 1 d . . . H24 H 1.2357 1.3544 0.7588 0.046 Uiso 1 1 calc R A . C25 C 1.2778(2) 1.2632(2) 0.81242(18) 0.0348(6) Uani 1 1 d . A . H25 H 1.1958 1.2125 0.7985 0.042 Uiso 1 1 calc R . . C26 C 1.3714(2) 1.2507(2) 0.85686(16) 0.0305(5) Uani 1 1 d . . . C27 C 1.4884(2) 1.3295(2) 0.87870(15) 0.0289(5) Uani 1 1 d . A . C28 C 1.3462(2) 1.1518(2) 0.87515(17) 0.0329(5) Uani 1 1 d . A . H28A H 1.2640 1.1393 0.8973 0.039 Uiso 1 1 calc R . . H28B H 1.4147 1.1608 0.9142 0.039 Uiso 1 1 calc R . . C29 C 1.0972(2) 0.8460(2) 0.63876(17) 0.0298(5) Uani 1 1 d . A . C30 C 1.8362(5) 1.5810(4) 0.6498(2) 0.0709(16) Uani 1 1 d . . . C31 C 1.8857(3) 1.0721(3) 0.7752(2) 0.0434(7) Uani 1 1 d . . . H31A H 1.9672 1.1136 0.7644 0.052 Uiso 1 1 calc R . . H31B H 1.8675 0.9978 0.7397 0.052 Uiso 1 1 calc R . . C32 C 1.8946(5) 1.0805(4) 0.8581(2) 0.0647(12) Uani 1 1 d . . . H32A H 1.8212 1.0251 0.8631 0.078 Uiso 1 1 calc R . . H32B H 1.9730 1.0636 0.8688 0.078 Uiso 1 1 calc R . . C33 C 1.8972(5) 1.1814(5) 0.9200(3) 0.0737(14) Uani 1 1 d . . . H33A H 1.8215 1.2019 0.9098 0.088 Uiso 1 1 calc R . . H33B H 1.8937 1.1729 0.9709 0.088 Uiso 1 1 calc R . . C34 C 2.0106(6) 1.2616(6) 0.9225(4) 0.0874(18) Uani 1 1 d . . . H34A H 2.0853 1.2424 0.9348 0.131 Uiso 1 1 calc R . . H34B H 2.0100 1.3285 0.9626 0.131 Uiso 1 1 calc R . . H34C H 2.0145 1.2690 0.8718 0.131 Uiso 1 1 calc R . . C35 C 1.5719(3) 1.3679(3) 1.00733(16) 0.0367(6) Uani 1 1 d . . . H35A H 1.4929 1.3254 1.0197 0.044 Uiso 1 1 calc R . . H35B H 1.5669 1.4406 1.0211 0.044 Uiso 1 1 calc R . . C36 C 1.6858(3) 1.3692(3) 1.05307(18) 0.0394(6) Uani 1 1 d . . . H36A H 1.6960 1.2977 1.0337 0.047 Uiso 1 1 calc R . . H36B H 1.6698 1.3866 1.1082 0.047 Uiso 1 1 calc R . . C37 C 1.8083(3) 1.4463(3) 1.0489(2) 0.0500(9) Uani 1 1 d . . . H37A H 1.7946 1.5160 1.0609 0.060 Uiso 1 1 calc R . . H37B H 1.8314 1.4229 0.9952 0.060 Uiso 1 1 calc R . . C38 C 1.9184(4) 1.4578(6) 1.1046(3) 0.0840(18) Uani 1 1 d . . . H38A H 1.8988 1.4859 1.1582 0.126 Uiso 1 1 calc R . . H38B H 1.9964 1.5062 1.0976 0.126 Uiso 1 1 calc R . . H38C H 1.9311 1.3889 1.0940 0.126 Uiso 1 1 calc R . . C39 C 0.9351(3) 0.8620(2) 0.46537(19) 0.0368(6) Uani 1 1 d . . . H39 H 1.0198 0.8773 0.4877 0.044 Uiso 1 1 calc R A . C40 C 0.9154(4) 0.9037(3) 0.4096(2) 0.0467(8) Uani 1 1 d . A . H40 H 0.9856 0.9470 0.3950 0.056 Uiso 1 1 calc R . . C41 C 0.7968(5) 0.8819(3) 0.3772(2) 0.0496(9) Uani 1 1 d . . . H41 H 0.7822 0.9093 0.3391 0.059 Uiso 1 1 calc R A . C42 C 0.6933(4) 0.8180(3) 0.39968(18) 0.0417(7) Uani 1 1 d . A . C43 C 0.7203(3) 0.7805(2) 0.45601(16) 0.0331(5) Uani 1 1 d . . . C44 C 0.5614(5) 0.7901(4) 0.3679(2) 0.0611(13) Uani 1 1 d . . . H44 H 0.5421 0.8144 0.3288 0.073 Uiso 1 1 calc R A . C45 C 0.4679(4) 0.7321(4) 0.3919(2) 0.0625(13) Uani 1 1 d . A . H45 H 0.3829 0.7135 0.3686 0.075 Uiso 1 1 calc R . . C46 C 0.4918(3) 0.6965(3) 0.4523(2) 0.0548(10) Uani 1 1 d . . . C47 C 0.6187(3) 0.7183(3) 0.48329(18) 0.0398(7) Uani 1 1 d . A . C48 C 0.3955(3) 0.6390(4) 0.4824(3) 0.0709(15) Uani 1 1 d . A . H48 H 0.3087 0.6212 0.4624 0.085 Uiso 1 1 calc R . . C49 C 0.4254(4) 0.6089(4) 0.5393(3) 0.0797(17) Uani 1 1 d . . . H49 H 0.3597 0.5725 0.5615 0.096 Uiso 1 1 calc R A . C50 C 0.5547(4) 0.6312(4) 0.5665(3) 0.0623(12) Uani 1 1 d . A . H50 H 0.5749 0.6072 0.6056 0.075 Uiso 1 1 calc R . . C51 C 0.8581(9) 0.5089(7) 0.4105(5) 0.0592(5) Uani 0.50 1 d PD A 2 H51 H 0.9100 0.4894 0.4406 0.071 Uiso 0.50 1 calc PR A 2 C52 C 0.7319(10) 0.4687(9) 0.2916(6) 0.0592(5) Uani 0.50 1 d PD A 2 H52A H 0.6994 0.4093 0.2422 0.089 Uiso 0.50 1 calc PR A 2 H52B H 0.7867 0.5291 0.2816 0.089 Uiso 0.50 1 calc PR A 2 H52C H 0.6601 0.4878 0.3178 0.089 Uiso 0.50 1 calc PR A 2 C53 C 0.8226(10) 0.3377(8) 0.3091(6) 0.0592(5) Uani 0.50 1 d PD A 2 H53A H 0.7760 0.2981 0.2569 0.089 Uiso 0.50 1 calc PR A 2 H53B H 0.7910 0.2996 0.3434 0.089 Uiso 0.50 1 calc PR A 2 H53C H 0.9139 0.3458 0.3064 0.089 Uiso 0.50 1 calc PR A 2 C54 C 0.6460(9) 0.3807(7) 0.2689(5) 0.0592(5) Uani 0.50 1 d PD B 1 H54 H 0.5567 0.3606 0.2542 0.071 Uiso 0.50 1 calc PR B 1 C55 C 0.8411(9) 0.3391(8) 0.2836(6) 0.0592(5) Uani 0.50 1 d PD B 1 H55A H 0.8814 0.2837 0.2598 0.089 Uiso 0.50 1 calc PR B 1 H55B H 0.8321 0.3475 0.3380 0.089 Uiso 0.50 1 calc PR B 1 H55C H 0.8944 0.4056 0.2813 0.089 Uiso 0.50 1 calc PR B 1 C56 C 0.6625(9) 0.2105(7) 0.1830(5) 0.0592(5) Uani 0.50 1 d PD B 1 H56A H 0.7297 0.1758 0.1739 0.089 Uiso 0.50 1 calc PR B 1 H56B H 0.6346 0.2163 0.1347 0.089 Uiso 0.50 1 calc PR B 1 H56C H 0.5898 0.1689 0.2002 0.089 Uiso 0.50 1 calc PR B 1 O12 O 0.6264(6) 0.1316(5) 0.1173(4) 0.0592(5) Uani 0.50 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03051(10) 0.03872(12) 0.02937(11) 0.01659(9) -0.00557(7) -0.00819(7) O1 0.0203(8) 0.0407(11) 0.0334(10) -0.0009(9) 0.0017(7) 0.0027(7) O2 0.0208(8) 0.0501(12) 0.0250(9) 0.0049(9) -0.0010(6) 0.0103(8) O3 0.0295(9) 0.0416(11) 0.0251(9) 0.0143(8) 0.0059(7) 0.0072(8) O4 0.0248(8) 0.0314(9) 0.0210(8) 0.0036(7) 0.0030(6) 0.0036(7) O5 0.0239(8) 0.0437(12) 0.0392(12) 0.0113(10) -0.0025(8) 0.0000(8) O6 0.0298(9) 0.0301(9) 0.0342(10) 0.0094(8) -0.0060(7) -0.0002(7) O7 0.102(3) 0.075(2) 0.0527(19) 0.0376(17) 0.0012(18) -0.0341(19) O8 0.094(3) 0.072(2) 0.071(2) 0.052(2) -0.0209(19) -0.0209(19) O9 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) O10 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) O11 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) N1 0.0274(10) 0.0362(12) 0.0298(11) 0.0138(10) 0.0051(8) 0.0060(8) N2 0.0307(11) 0.0462(15) 0.0343(13) 0.0105(12) 0.0006(9) -0.0085(10) N3 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) N4 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) C1 0.0214(9) 0.0279(11) 0.0286(12) 0.0083(10) 0.0021(8) 0.0001(8) C2 0.0215(9) 0.0281(11) 0.0303(12) 0.0120(10) 0.0015(8) 0.0005(8) C3 0.0222(9) 0.0238(11) 0.0319(12) 0.0123(10) -0.0011(8) 0.0012(8) C4 0.0281(11) 0.0232(11) 0.0320(13) 0.0065(10) -0.0017(9) 0.0050(9) C5 0.0252(10) 0.0283(12) 0.0306(13) 0.0051(10) -0.0007(9) 0.0038(9) C6 0.0233(10) 0.0288(12) 0.0297(12) 0.0053(10) 0.0009(9) 0.0026(9) C7 0.0301(12) 0.0356(14) 0.0425(16) 0.0017(13) -0.0011(11) 0.0142(11) C8 0.0237(11) 0.0421(15) 0.0317(13) 0.0008(12) 0.0011(9) 0.0146(10) C9 0.0251(11) 0.0470(17) 0.0342(14) -0.0032(13) -0.0043(10) 0.0146(11) C10 0.0310(12) 0.0544(19) 0.0261(13) 0.0007(13) -0.0012(10) 0.0191(13) C11 0.0248(11) 0.0580(19) 0.0267(13) 0.0074(13) 0.0027(9) 0.0142(12) C12 0.0182(10) 0.0551(18) 0.0262(12) 0.0048(12) 0.0019(8) 0.0093(10) C13 0.0198(10) 0.0470(16) 0.0262(12) 0.0014(11) -0.0006(8) 0.0111(10) C14 0.0182(10) 0.063(2) 0.0268(13) 0.0062(13) 0.0015(9) 0.0010(11) C15 0.0199(10) 0.0511(17) 0.0276(13) 0.0121(12) -0.0017(9) -0.0074(10) C16 0.0327(13) 0.066(2) 0.0271(14) 0.0174(14) -0.0032(10) -0.0204(14) C17 0.0463(17) 0.0469(18) 0.0400(17) 0.0235(15) -0.0116(13) -0.0189(14) C18 0.0419(15) 0.0374(15) 0.0405(17) 0.0171(13) -0.0118(12) -0.0100(12) C19 0.0297(12) 0.0326(13) 0.0334(14) 0.0125(11) -0.0062(10) -0.0063(10) C20 0.0248(10) 0.0373(14) 0.0258(12) 0.0117(11) -0.0025(9) -0.0046(9) C21 0.0385(14) 0.0269(12) 0.0354(15) 0.0076(11) -0.0019(11) 0.0010(10) C22 0.0320(12) 0.0281(12) 0.0299(13) 0.0036(10) 0.0019(10) 0.0067(9) C23 0.0373(13) 0.0340(14) 0.0384(15) 0.0091(12) 0.0013(11) 0.0124(11) C24 0.0320(13) 0.0387(15) 0.0415(16) 0.0070(13) 0.0003(11) 0.0154(11) C25 0.0229(10) 0.0362(14) 0.0347(14) 0.0019(11) 0.0021(9) 0.0073(10) C26 0.0249(10) 0.0308(12) 0.0264(12) 0.0025(10) 0.0051(9) 0.0047(9) C27 0.0241(10) 0.0299(12) 0.0242(11) 0.0022(10) 0.0024(8) 0.0052(9) C28 0.0239(10) 0.0353(13) 0.0303(13) 0.0076(11) 0.0065(9) 0.0008(9) C29 0.0265(10) 0.0265(11) 0.0344(13) 0.0163(11) -0.0038(9) -0.0016(8) C30 0.072(3) 0.067(3) 0.041(2) 0.031(2) -0.0252(18) -0.043(2) C31 0.0300(13) 0.063(2) 0.0358(15) 0.0109(15) 0.0014(11) 0.0206(14) C32 0.078(3) 0.089(3) 0.043(2) 0.023(2) 0.0042(19) 0.050(3) C33 0.061(3) 0.104(4) 0.053(3) 0.027(3) 0.000(2) 0.023(3) C34 0.076(3) 0.115(5) 0.085(4) 0.038(4) 0.036(3) 0.048(4) C35 0.0354(13) 0.0394(15) 0.0225(12) 0.0028(11) 0.0049(10) 0.0024(11) C36 0.0390(14) 0.0451(17) 0.0251(13) 0.0080(12) -0.0005(10) 0.0052(12) C37 0.0394(15) 0.062(2) 0.0284(15) 0.0070(15) -0.0048(12) -0.0027(14) C38 0.044(2) 0.142(5) 0.039(2) 0.018(3) -0.0142(16) 0.007(3) C39 0.0405(14) 0.0334(14) 0.0363(15) 0.0151(12) 0.0118(11) 0.0074(11) C40 0.074(2) 0.0329(15) 0.0374(17) 0.0152(13) 0.0209(16) 0.0182(15) C41 0.091(3) 0.0385(17) 0.0285(15) 0.0123(13) 0.0102(16) 0.0334(18) C42 0.0589(19) 0.0396(16) 0.0264(13) 0.0029(12) -0.0024(12) 0.0265(15) C43 0.0335(12) 0.0389(14) 0.0234(12) 0.0061(11) 0.0003(9) 0.0125(11) C44 0.078(3) 0.062(2) 0.0351(18) -0.0114(17) -0.0222(18) 0.046(2) C45 0.049(2) 0.067(3) 0.046(2) -0.0150(19) -0.0213(17) 0.0250(19) C46 0.0315(14) 0.056(2) 0.0451(19) -0.0150(17) -0.0096(13) 0.0085(14) C47 0.0283(12) 0.0444(16) 0.0298(14) -0.0001(12) -0.0026(10) 0.0032(11) C48 0.0287(15) 0.072(3) 0.064(3) -0.013(2) -0.0054(16) -0.0070(16) C49 0.0357(18) 0.079(3) 0.073(3) 0.000(3) 0.0120(19) -0.0252(19) C50 0.0464(19) 0.063(2) 0.051(2) 0.0162(19) 0.0096(16) -0.0190(17) C51 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) C52 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) C53 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) C54 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) C55 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) C56 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) O12 0.0663(14) 0.0565(11) 0.0521(13) 0.0223(10) -0.0009(10) 0.0115(10) _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 O9 2.301(7) . ? Cd1 O8 2.363(3) 1_445 ? Cd1 O5 2.365(2) . ? Cd1 N1 2.366(2) . ? Cd1 O10 2.377(8) . ? Cd1 N2 2.383(3) . ? Cd1 O6 2.384(2) . ? Cd1 O7 2.410(4) 1_445 ? Cd1 C29 2.699(2) . ? Cd1 C30 2.725(4) 1_445 ? O1 C6 1.351(3) . ? O1 H1 0.8400 . ? O2 C13 1.390(3) . ? O2 C31 1.442(4) . ? O3 C20 1.360(3) . ? O3 H3 0.8400 . ? O4 C27 1.390(3) . ? O4 C35 1.442(3) . ? O5 C29 1.256(4) . ? O6 C29 1.255(4) . ? O7 C30 1.233(7) . ? O7 Cd1 2.410(4) 1_665 ? O8 C30 1.241(8) . ? O8 Cd1 2.363(3) 1_665 ? O9 C51 1.223(10) . ? O11 C54 1.177(10) . ? N1 C39 1.316(4) . ? N1 C43 1.350(3) . ? N2 C50 1.326(4) . ? N2 C47 1.345(5) . ? N3 C51 1.346(10) . ? N3 C52 1.407(10) . ? N3 C53 1.438(11) . ? N4 C54 1.347(10) . ? N4 C56 1.366(10) . ? N4 C55 1.534(11) . ? C1 C2 1.390(3) . ? C1 C6 1.395(4) . ? C1 C28 1.516(4) . ? C2 C3 1.387(4) . ? C2 H2 0.9500 . ? C3 C4 1.389(4) . ? C3 C29 1.503(3) . ? C4 C5 1.398(4) . ? C4 H4 0.9500 . ? C5 C6 1.405(4) . ? C5 C7 1.518(4) . ? C7 C8 1.512(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.393(4) . ? C8 C13 1.398(4) . ? C9 C10 1.377(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 C12 1.402(4) . ? C11 H11 0.9500 . ? C12 C13 1.379(5) . ? C12 C14 1.516(4) . ? C14 C15 1.506(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.403(4) . ? C15 C16 1.405(5) . ? C16 C17 1.394(6) . ? C16 H16 0.9500 . ? C17 C18 1.364(6) . ? C17 C30 1.508(5) . ? C18 C19 1.395(4) . ? C18 H18 0.9500 . ? C19 C20 1.387(5) . ? C19 C21 1.500(5) . ? C21 C22 1.513(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.393(4) . ? C22 C23 1.393(4) . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C24 C25 1.379(5) . ? C24 H24 0.9500 . ? C25 C26 1.397(4) . ? C25 H25 0.9500 . ? C26 C27 1.395(4) . ? C26 C28 1.513(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C30 Cd1 2.726(4) 1_665 ? C31 C32 1.498(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.479(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.424(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.496(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.504(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.517(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.401(5) . ? C39 H39 0.9500 . ? C40 C41 1.335(6) . ? C40 H40 0.9500 . ? C41 C42 1.411(6) . ? C41 H41 0.9500 . ? C42 C43 1.391(4) . ? C42 C44 1.449(5) . ? C43 C47 1.435(5) . ? C44 C45 1.314(8) . ? C44 H44 0.9500 . ? C45 C46 1.429(7) . ? C45 H45 0.9500 . ? C46 C48 1.396(7) . ? C46 C47 1.409(4) . ? C48 C49 1.340(8) . ? C48 H48 0.9500 . ? C49 C50 1.411(7) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 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 O9 Cd1 O8 124.4(2) . 1_445 ? O9 Cd1 O5 147.5(2) . . ? O8 Cd1 O5 85.30(11) 1_445 . ? O9 Cd1 N1 72.35(17) . . ? O8 Cd1 N1 142.99(14) 1_445 . ? O5 Cd1 N1 92.00(9) . . ? O9 Cd1 O10 13.58(19) . . ? O8 Cd1 O10 119.3(2) 1_445 . ? O5 Cd1 O10 142.95(19) . . ? N1 Cd1 O10 83.57(17) . . ? O9 Cd1 N2 82.29(19) . . ? O8 Cd1 N2 79.88(12) 1_445 . ? O5 Cd1 N2 119.45(9) . . ? N1 Cd1 N2 69.43(9) . . ? O10 Cd1 N2 93.39(18) . . ? O9 Cd1 O6 95.85(19) . . ? O8 Cd1 O6 116.08(11) 1_445 . ? O5 Cd1 O6 55.30(8) . . ? N1 Cd1 O6 91.62(8) . . ? O10 Cd1 O6 87.97(19) . . ? N2 Cd1 O6 160.68(9) . . ? O9 Cd1 O7 84.75(19) . 1_445 ? O8 Cd1 O7 53.93(16) 1_445 1_445 ? O5 Cd1 O7 107.05(10) . 1_445 ? N1 Cd1 O7 157.04(11) . 1_445 ? O10 Cd1 O7 73.51(19) . 1_445 ? N2 Cd1 O7 109.88(12) . 1_445 ? O6 Cd1 O7 89.00(11) . 1_445 ? O9 Cd1 C29 122.9(2) . . ? O8 Cd1 C29 100.00(10) 1_445 . ? O5 Cd1 C29 27.73(8) . . ? N1 Cd1 C29 94.06(8) . . ? O10 Cd1 C29 115.67(19) . . ? N2 Cd1 C29 145.22(10) . . ? O6 Cd1 C29 27.71(8) . . ? O7 Cd1 C29 97.05(11) 1_445 . ? O9 Cd1 C30 105.7(2) . 1_445 ? O8 Cd1 C30 27.05(17) 1_445 1_445 ? O5 Cd1 C30 96.38(10) . 1_445 ? N1 Cd1 C30 165.16(13) . 1_445 ? O10 Cd1 C30 96.8(2) . 1_445 ? N2 Cd1 C30 95.75(14) . 1_445 ? O6 Cd1 C30 103.23(12) . 1_445 ? O7 Cd1 C30 26.89(17) 1_445 1_445 ? C29 Cd1 C30 99.06(9) . 1_445 ? C6 O1 H1 109.5 . . ? C13 O2 C31 114.7(2) . . ? C20 O3 H3 109.5 . . ? C27 O4 C35 113.0(2) . . ? C29 O5 Cd1 91.11(17) . . ? C29 O6 Cd1 90.26(16) . . ? C30 O7 Cd1 91.0(4) . 1_665 ? C30 O8 Cd1 93.0(3) . 1_665 ? C51 O9 Cd1 128.3(6) . . ? C39 N1 C43 118.8(3) . . ? C39 N1 Cd1 124.0(2) . . ? C43 N1 Cd1 116.40(19) . . ? C50 N2 C47 118.6(3) . . ? C50 N2 Cd1 125.1(3) . . ? C47 N2 Cd1 115.7(2) . . ? C51 N3 C52 120.6(8) . . ? C51 N3 C53 120.4(7) . . ? C52 N3 C53 119.0(8) . . ? C54 N4 C56 127.8(8) . . ? C54 N4 C55 113.3(7) . . ? C56 N4 C55 118.3(8) . . ? C2 C1 C6 119.0(3) . . ? C2 C1 C28 121.2(2) . . ? C6 C1 C28 119.7(2) . . ? C3 C2 C1 121.0(2) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.4(2) . . ? C2 C3 C29 120.1(2) . . ? C4 C3 C29 120.5(2) . . ? C3 C4 C5 121.3(3) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 118.0(2) . . ? C4 C5 C7 120.3(3) . . ? C6 C5 C7 121.7(2) . . ? O1 C6 C1 115.8(2) . . ? O1 C6 C5 122.9(2) . . ? C1 C6 C5 121.2(2) . . ? C8 C7 C5 113.1(3) . . ? C8 C7 H7A 109.0 . . ? C5 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? C5 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C13 117.5(3) . . ? C9 C8 C7 120.4(3) . . ? C13 C8 C7 122.1(3) . . ? C10 C9 C8 121.0(3) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 117.8(3) . . ? C13 C12 C14 122.9(3) . . ? C11 C12 C14 119.2(3) . . ? C12 C13 O2 120.0(3) . . ? C12 C13 C8 122.7(3) . . ? O2 C13 C8 117.3(3) . . ? C15 C14 C12 111.4(2) . . ? C15 C14 H14A 109.3 . . ? C12 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C12 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C20 C15 C16 117.6(3) . . ? C20 C15 C14 120.2(3) . . ? C16 C15 C14 122.2(3) . . ? C17 C16 C15 121.7(3) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C18 C17 C16 118.4(3) . . ? C18 C17 C30 120.8(4) . . ? C16 C17 C30 120.8(4) . . ? C17 C18 C19 122.6(4) . . ? C17 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C20 C19 C18 118.2(3) . . ? C20 C19 C21 121.9(3) . . ? C18 C19 C21 119.9(3) . . ? O3 C20 C19 123.1(3) . . ? O3 C20 C15 115.4(3) . . ? C19 C20 C15 121.5(3) . . ? C19 C21 C22 112.6(2) . . ? C19 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C19 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C27 C22 C23 118.6(3) . . ? C27 C22 C21 121.9(3) . . ? C23 C22 C21 119.5(3) . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 121.7(3) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 117.0(3) . . ? C27 C26 C28 122.9(3) . . ? C25 C26 C28 120.0(2) . . ? O4 C27 C22 118.1(2) . . ? O4 C27 C26 119.5(3) . . ? C22 C27 C26 122.3(3) . . ? C26 C28 C1 110.0(2) . . ? C26 C28 H28A 109.7 . . ? C1 C28 H28A 109.7 . . ? C26 C28 H28B 109.7 . . ? C1 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? O6 C29 O5 122.7(2) . . ? O6 C29 C3 119.1(2) . . ? O5 C29 C3 118.2(3) . . ? O6 C29 Cd1 62.03(14) . . ? O5 C29 Cd1 61.16(14) . . ? C3 C29 Cd1 171.44(18) . . ? O7 C30 O8 122.1(4) . . ? O7 C30 C17 119.2(6) . . ? O8 C30 C17 118.7(5) . . ? O7 C30 Cd1 62.1(3) . 1_665 ? O8 C30 Cd1 60.0(2) . 1_665 ? C17 C30 Cd1 178.5(4) . 1_665 ? O2 C31 C32 107.0(3) . . ? O2 C31 H31A 110.3 . . ? C32 C31 H31A 110.3 . . ? O2 C31 H31B 110.3 . . ? C32 C31 H31B 110.3 . . ? H31A C31 H31B 108.6 . . ? C33 C32 C31 118.7(4) . . ? C33 C32 H32A 107.6 . . ? C31 C32 H32A 107.6 . . ? C33 C32 H32B 107.6 . . ? C31 C32 H32B 107.6 . . ? H32A C32 H32B 107.1 . . ? C34 C33 C32 110.2(5) . . ? C34 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O4 C35 C36 109.2(2) . . ? O4 C35 H35A 109.8 . . ? C36 C35 H35A 109.8 . . ? O4 C35 H35B 109.8 . . ? C36 C35 H35B 109.8 . . ? H35A C35 H35B 108.3 . . ? C35 C36 C37 113.9(3) . . ? C35 C36 H36A 108.8 . . ? C37 C36 H36A 108.8 . . ? C35 C36 H36B 108.8 . . ? C37 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C36 C37 C38 113.0(4) . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? C36 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 C40 122.6(3) . . ? N1 C39 H39 118.7 . . ? C40 C39 H39 118.7 . . ? C41 C40 C39 119.2(3) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 119.9(3) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C43 C42 C41 117.6(3) . . ? C43 C42 C44 118.5(4) . . ? C41 C42 C44 123.9(4) . . ? N1 C43 C42 122.0(3) . . ? N1 C43 C47 117.8(3) . . ? C42 C43 C47 120.2(3) . . ? C45 C44 C42 121.6(4) . . ? C45 C44 H44 119.2 . . ? C42 C44 H44 119.2 . . ? C44 C45 C46 121.2(3) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C48 C46 C47 117.1(4) . . ? C48 C46 C45 123.5(4) . . ? C47 C46 C45 119.4(4) . . ? N2 C47 C46 122.7(3) . . ? N2 C47 C43 118.4(2) . . ? C46 C47 C43 118.8(3) . . ? C49 C48 C46 120.0(4) . . ? C49 C48 H48 120.0 . . ? C46 C48 H48 120.0 . . ? C48 C49 C50 120.0(4) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? N2 C50 C49 121.5(5) . . ? N2 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? O9 C51 N3 121.4(8) . . ? O9 C51 H51 119.3 . . ? N3 C51 H51 119.3 . . ? N3 C52 H52A 109.5 . . ? N3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N3 C53 H53A 109.5 . . ? N3 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N3 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O11 C54 N4 122.9(9) . . ? O11 C54 H54 118.5 . . ? N4 C54 H54 118.5 . . ? N4 C55 H55A 109.5 . . ? N4 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N4 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N4 C56 H56A 109.5 . . ? N4 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N4 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 36.06 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.075 _refine_diff_density_min -3.529 _refine_diff_density_rms 0.111 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.009 0.000 0.000 393 60 ' ' _platon_squeeze_details ; Despite the ability to model most of the disorder one DMF molecule could not be modelled aprpopriately. Given this the routine SQUEEZE was applied to the data. This had the effect of markedly improving the agreement indices. SQUEEZE suggested an electron count a little greater than that of DMF, suggesting validity of the model. ; data_PCH244 _database_code_depnum_ccdc_archive 'CCDC 910964' #TrackingRef '8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PCH244 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C107 H118 Cd2 N6 O23' _chemical_formula_weight 2080.87 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.2266(10) _cell_length_b 24.9668(14) _cell_length_c 20.7082(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.402(4) _cell_angle_gamma 90.00 _cell_volume 9833.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9676 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 31.15 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4328 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9229 _exptl_absorpt_correction_T_max 0.9799 _exptl_absorpt_process_details 'SADABS 2004 Bruker AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD Diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 71162 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 31.19 _reflns_number_total 24200 _reflns_number_gt 16891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'local program' _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. There is disorder presetn in one calixarene lower-rim alkyl chain and this was mdoelled over two positions with partial occupancy. There is also disorder present in two waters of crystallisation adn this has also been successfully modelled. Restraints used in refinement are listed below. Calculated and reported formulae differ due to H atoms of the water molecules. DFIX 1.54 0.02 C70A C71A DFIX 1.54 0.02 C70 C71 DFIX 1.54 0.02 C72 C71 DFIX 1.54 0.02 C71A C72A DFIX 1.45 0.02 O9 C69 DFIX 1.54 0.02 C70 C69 DFIX 1.54 0.02 C70A C69A DFIX 1.45 0.02 O9 C69A EXYZ C69 C69A EADP C69 C69A C70 C70A C71 C71A C72 C72A EXYZ C73 C73A EXYZ C74 C74A EXYZ C75 C75A EADP C73 C73A C74 C74A C75 C75A C76 C76A DFIX 1.54 0.02 C76A C75A DFIX 1.54 0.02 C75A C74A DFIX 1.54 0.02 C74A C73A DFIX 1.45 0.02 O11 C73A DFIX 1.45 0.02 O11 C73 DFIX 1.54 0.02 C73 C74 DFIX 1.54 0.02 C74 C75 DFIX 1.54 0.02 C76 C75 EADP O22 O22A EADP O21 O21A ; _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^)+(0.1102P)^2^+17.6529P] 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 24200 _refine_ls_number_parameters 1232 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.2121 _refine_ls_wR_factor_gt 0.1879 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.445673(17) 0.644835(12) 0.429633(14) 0.03821(9) Uani 1 1 d . . . Cd2 Cd 0.975918(19) 0.644554(13) 0.453769(16) 0.04364(10) Uani 1 1 d . . . O1 O 0.55867(13) 0.60684(11) 0.05972(12) 0.0310(5) Uani 1 1 d . . . O2 O 0.67999(14) 0.66330(12) 0.06891(14) 0.0346(6) Uani 1 1 d . . . H2O H 0.6408 0.6488 0.0702 0.042 Uiso 1 1 calc R . . O3 O 0.79275(13) 0.58551(11) 0.06981(12) 0.0318(6) Uani 1 1 d . . . O4 O 0.67757(14) 0.53196(12) 0.09536(13) 0.0361(6) Uani 1 1 d . . . H4O H 0.7159 0.5471 0.0922 0.043 Uiso 1 1 calc R . . O5 O 0.47660(18) 0.59334(13) 0.34337(14) 0.0445(7) Uani 1 1 d . . . O6 O 0.48107(18) 0.68049(13) 0.33334(15) 0.0442(7) Uani 1 1 d . . . O7 O 0.9384(2) 0.67765(15) 0.34274(17) 0.0551(9) Uani 1 1 d . . . O8 O 0.9524(2) 0.59259(15) 0.35991(17) 0.0670(12) Uani 1 1 d . . . O9 O 0.79688(15) 0.91045(13) 0.62078(18) 0.0476(8) Uani 1 1 d D . . O10 O 0.67605(16) 0.93450(13) 0.53930(17) 0.0452(7) Uani 1 1 d . . . H10O H 0.7139 0.9248 0.5617 0.054 Uiso 1 1 calc R . . O11 O 0.56954(14) 0.92078(12) 0.62783(16) 0.0417(7) Uani 1 1 d D . . O12 O 0.69143(14) 0.87471(12) 0.69259(16) 0.0407(7) Uani 1 1 d . . . H12O H 0.6526 0.8828 0.6707 0.049 Uiso 1 1 calc R . . O13 O 0.9118(4) 0.6792(2) 0.5720(3) 0.136(3) Uani 1 1 d . . . O14 O 0.9162(2) 0.71503(17) 0.4790(2) 0.0740(12) Uani 1 1 d . . . O15 O 0.43277(19) 0.73030(15) 0.45340(18) 0.0559(9) Uani 1 1 d . . . O16 O 0.4371(2) 0.69346(15) 0.5507(2) 0.0608(9) Uani 1 1 d . . . O17 O 0.56421(18) 0.64946(13) 0.47706(17) 0.0474(7) Uani 1 1 d . . . O18 O 0.8948(2) 0.58896(14) 0.49614(19) 0.0570(9) Uani 1 1 d . . . O19 O 0.7903(2) 0.59273(19) 0.3972(2) 0.0798(13) Uani 1 1 d . . . O20 O 0.9448(2) 0.77674(17) 0.2949(2) 0.0742(12) Uani 1 1 d . . . O21 O 0.4253(6) 0.6420(4) 0.6637(5) 0.078(2) Uani 0.50 1 d P A 1 O22 O 0.9841(5) 0.6596(4) 0.6987(4) 0.0871(19) Uani 0.60 1 d P B 1 O23 O 0.4382(3) 0.7923(3) 0.3156(4) 0.128(2) Uani 1 1 d . . . N00H N 1.0852(2) 0.68536(14) 0.45649(17) 0.0401(8) Uani 1 1 d . . . N00K N 0.3312(2) 0.61055(16) 0.40566(18) 0.0444(9) Uani 1 1 d . . . N00L N 1.0595(2) 0.59436(14) 0.52117(18) 0.0432(8) Uani 1 1 d . . . N00M N 0.7302(2) 0.64857(16) 0.3243(2) 0.0459(9) Uani 1 1 d . . . N00N N 0.4364(2) 0.57354(16) 0.49757(18) 0.0454(9) Uani 1 1 d . . . N00R N 0.6391(2) 0.71480(18) 0.5212(2) 0.0538(10) Uani 1 1 d . . . C1 C 0.54088(18) 0.56822(16) 0.16243(19) 0.0314(8) Uani 1 1 d . . . C2 C 0.52413(18) 0.57631(16) 0.22448(18) 0.0316(8) Uani 1 1 d . . . H2 H 0.5205 0.5463 0.2520 0.038 Uiso 1 1 calc R . . C3 C 0.51265(18) 0.62707(17) 0.24726(18) 0.0320(8) Uani 1 1 d . . . C4 C 0.52210(19) 0.67149(16) 0.20852(18) 0.0312(8) Uani 1 1 d . . . H4 H 0.5165 0.7065 0.2249 0.037 Uiso 1 1 calc R . . C5 C 0.53959(18) 0.66499(17) 0.14641(19) 0.0315(8) Uani 1 1 d . . . C6 C 0.54570(18) 0.61291(16) 0.12367(18) 0.0304(7) Uani 1 1 d . . . C7 C 0.55378(19) 0.71362(16) 0.10669(19) 0.0335(8) Uani 1 1 d . . . H7A H 0.5462 0.7041 0.0598 0.040 Uiso 1 1 calc R . . H7B H 0.5200 0.7423 0.1135 0.040 Uiso 1 1 calc R . . C8 C 0.6277(2) 0.73447(16) 0.12516(18) 0.0313(8) Uani 1 1 d . . . C9 C 0.6400(2) 0.78048(16) 0.1627(2) 0.0374(9) Uani 1 1 d . . . H9 H 0.6013 0.7987 0.1764 0.045 Uiso 1 1 calc R . . C10 C 0.7073(2) 0.80036(17) 0.1807(2) 0.0411(9) Uani 1 1 d . . . H10 H 0.7146 0.8322 0.2058 0.049 Uiso 1 1 calc R . . C11 C 0.7639(2) 0.77323(17) 0.1617(2) 0.0382(9) Uani 1 1 d . . . H11 H 0.8101 0.7868 0.1741 0.046 Uiso 1 1 calc R . . C12 C 0.75438(19) 0.72687(15) 0.12522(18) 0.0307(7) Uani 1 1 d . . . C13 C 0.68568(19) 0.70794(15) 0.10667(17) 0.0291(7) Uani 1 1 d . . . C14 C 0.8158(2) 0.69693(16) 0.10465(19) 0.0335(8) Uani 1 1 d . . . H14A H 0.8558 0.7218 0.1045 0.040 Uiso 1 1 calc R . . H14B H 0.8025 0.6832 0.0597 0.040 Uiso 1 1 calc R . . C15 C 0.83827(18) 0.65047(16) 0.15014(18) 0.0307(8) Uani 1 1 d . . . C16 C 0.87229(19) 0.66081(17) 0.21315(19) 0.0333(8) Uani 1 1 d . . . H16 H 0.8825 0.6968 0.2263 0.040 Uiso 1 1 calc R . . C17 C 0.89153(19) 0.61918(17) 0.25716(18) 0.0332(8) Uani 1 1 d . . . C18 C 0.87401(19) 0.56686(17) 0.23896(19) 0.0346(8) Uani 1 1 d . . . H18 H 0.8855 0.5387 0.2695 0.042 Uiso 1 1 calc R . . C19 C 0.83990(19) 0.55514(16) 0.17663(19) 0.0316(8) Uani 1 1 d . . . C20 C 0.82553(18) 0.59742(16) 0.13254(18) 0.0300(7) Uani 1 1 d . . . C21 C 0.8180(2) 0.49851(16) 0.1592(2) 0.0353(8) Uani 1 1 d . . . H21A H 0.8553 0.4737 0.1790 0.042 Uiso 1 1 calc R . . H21B H 0.8129 0.4942 0.1112 0.042 Uiso 1 1 calc R . . C22 C 0.74925(19) 0.48353(15) 0.18242(19) 0.0313(7) Uani 1 1 d . . . C23 C 0.7494(2) 0.45107(16) 0.2367(2) 0.0360(8) Uani 1 1 d . . . H23 H 0.7929 0.4383 0.2590 0.043 Uiso 1 1 calc R . . C24 C 0.6877(2) 0.43679(17) 0.2591(2) 0.0399(9) Uani 1 1 d . . . H24 H 0.6888 0.4139 0.2958 0.048 Uiso 1 1 calc R . . C25 C 0.6249(2) 0.45614(16) 0.2277(2) 0.0366(8) Uani 1 1 d . . . H25 H 0.5825 0.4469 0.2435 0.044 Uiso 1 1 calc R . . C26 C 0.6220(2) 0.48888(15) 0.17341(19) 0.0316(7) Uani 1 1 d . . . C27 C 0.6846(2) 0.50219(15) 0.15053(18) 0.0309(7) Uani 1 1 d . . . C28 C 0.55367(19) 0.51170(16) 0.1399(2) 0.0329(8) Uani 1 1 d . . . H28A H 0.5145 0.4884 0.1487 0.039 Uiso 1 1 calc R . . H28B H 0.5542 0.5119 0.0921 0.039 Uiso 1 1 calc R . . C29 C 0.4890(2) 0.63424(18) 0.31193(19) 0.0352(8) Uani 1 1 d . . . C30 C 0.9299(2) 0.6306(2) 0.3239(2) 0.0403(9) Uani 1 1 d . . . C31 C 0.4969(2) 0.5953(2) 0.0137(2) 0.0453(11) Uani 1 1 d . . . H31A H 0.4564 0.6153 0.0262 0.054 Uiso 1 1 calc R . . H31B H 0.4862 0.5566 0.0151 0.054 Uiso 1 1 calc R . . C32 C 0.5065(3) 0.6100(4) -0.0519(2) 0.078(2) Uani 1 1 d . . . H32A H 0.4742 0.5863 -0.0805 0.094 Uiso 1 1 calc R . . H32B H 0.4864 0.6465 -0.0582 0.094 Uiso 1 1 calc R . . C33 C 0.5650(4) 0.6115(5) -0.0795(3) 0.124(4) Uani 1 1 d . . . H33A H 0.5876 0.5760 -0.0714 0.149 Uiso 1 1 calc R . . H33B H 0.5965 0.6377 -0.0542 0.149 Uiso 1 1 calc R . . C34 C 0.5664(3) 0.6237(2) -0.1485(2) 0.0547(12) Uani 1 1 d . . . H34A H 0.5257 0.6071 -0.1752 0.082 Uiso 1 1 calc R . . H34B H 0.6098 0.6097 -0.1617 0.082 Uiso 1 1 calc R . . H34C H 0.5645 0.6626 -0.1549 0.082 Uiso 1 1 calc R . . C35 C 0.8400(2) 0.57277(19) 0.0241(2) 0.0382(9) Uani 1 1 d . . . H35A H 0.8666 0.5397 0.0377 0.046 Uiso 1 1 calc R . . H35B H 0.8739 0.6023 0.0221 0.046 Uiso 1 1 calc R . . C36 C 0.7962(2) 0.56478(19) -0.0420(2) 0.0415(9) Uani 1 1 d . . . H36A H 0.7583 0.5388 -0.0374 0.050 Uiso 1 1 calc R . . H36B H 0.8262 0.5489 -0.0719 0.050 Uiso 1 1 calc R . . C37 C 0.7630(2) 0.61575(19) -0.0729(2) 0.0436(10) Uani 1 1 d . . . H37A H 0.7282 0.6061 -0.1112 0.052 Uiso 1 1 calc R . . H37B H 0.7376 0.6341 -0.0410 0.052 Uiso 1 1 calc R . . C38 C 0.8163(3) 0.6539(2) -0.0943(3) 0.0529(12) Uani 1 1 d . . . H38A H 0.8471 0.6674 -0.0559 0.079 Uiso 1 1 calc R . . H38B H 0.7918 0.6839 -0.1181 0.079 Uiso 1 1 calc R . . H38C H 0.8446 0.6350 -0.1228 0.079 Uiso 1 1 calc R . . C39 C 0.83325(19) 0.81964(18) 0.6434(2) 0.0365(8) Uani 1 1 d . . . C40 C 0.8583(2) 0.77263(18) 0.6201(2) 0.0388(9) Uani 1 1 d . . . H40 H 0.8691 0.7434 0.6492 0.047 Uiso 1 1 calc R . . C41 C 0.8680(2) 0.76697(19) 0.5555(2) 0.0427(10) Uani 1 1 d . . . C42 C 0.8490(2) 0.8088(2) 0.5127(2) 0.0442(10) Uani 1 1 d . . . H42 H 0.8536 0.8045 0.4679 0.053 Uiso 1 1 calc R . . C43 C 0.8238(2) 0.85595(19) 0.5330(2) 0.0431(10) Uani 1 1 d . . . C44 C 0.8187(2) 0.86190(17) 0.5989(2) 0.0393(9) Uani 1 1 d . . . C45 C 0.7995(2) 0.8997(2) 0.4837(3) 0.0543(13) Uani 1 1 d . . . H45A H 0.8036 0.9349 0.5060 0.065 Uiso 1 1 calc R . . H45B H 0.8306 0.9002 0.4496 0.065 Uiso 1 1 calc R . . C46 C 0.7243(2) 0.8916(2) 0.4518(2) 0.0466(11) Uani 1 1 d . . . C47 C 0.7105(3) 0.8656(2) 0.3918(3) 0.0536(12) Uani 1 1 d . . . H47 H 0.7487 0.8535 0.3713 0.064 Uiso 1 1 calc R . . C48 C 0.6423(3) 0.8571(2) 0.3614(3) 0.0564(13) Uani 1 1 d . . . H48 H 0.6337 0.8395 0.3203 0.068 Uiso 1 1 calc R C . C49 C 0.5869(3) 0.8747(2) 0.3917(2) 0.0512(11) Uani 1 1 d . . . H49 H 0.5401 0.8691 0.3708 0.061 Uiso 1 1 calc R . . C50 C 0.5978(2) 0.90000(19) 0.4516(2) 0.0430(10) Uani 1 1 d . . . C51 C 0.6673(2) 0.90827(19) 0.4817(2) 0.0432(10) Uani 1 1 d . . . C52 C 0.5374(2) 0.91671(19) 0.4872(2) 0.0445(10) Uani 1 1 d . D . H52A H 0.5504 0.9496 0.5129 0.053 Uiso 1 1 calc R . . H52B H 0.4953 0.9247 0.4551 0.053 Uiso 1 1 calc R . . C53 C 0.5209(2) 0.87209(19) 0.5323(2) 0.0392(9) Uani 1 1 d . . . C54 C 0.4910(2) 0.82539(19) 0.5059(2) 0.0393(9) Uani 1 1 d . D . H54 H 0.4789 0.8226 0.4599 0.047 Uiso 1 1 calc R . . C55 C 0.47801(19) 0.78244(18) 0.5446(2) 0.0368(9) Uani 1 1 d . . . C56 C 0.49930(19) 0.78519(17) 0.6118(2) 0.0361(8) Uani 1 1 d . D . H56 H 0.4922 0.7553 0.6385 0.043 Uiso 1 1 calc R . . C57 C 0.53060(19) 0.83095(18) 0.6401(2) 0.0354(8) Uani 1 1 d . . . C58 C 0.53914(19) 0.87479(18) 0.6000(2) 0.0365(8) Uani 1 1 d . D . C59 C 0.5584(2) 0.83041(19) 0.7126(2) 0.0385(9) Uani 1 1 d . D . H59A H 0.5661 0.8676 0.7286 0.046 Uiso 1 1 calc R . . H59B H 0.5234 0.8135 0.7368 0.046 Uiso 1 1 calc R . . C60 C 0.6268(2) 0.79962(17) 0.72492(19) 0.0342(8) Uani 1 1 d . . . C61 C 0.6286(2) 0.74710(18) 0.7473(2) 0.0395(9) Uani 1 1 d . D . H61 H 0.5863 0.7303 0.7552 0.047 Uiso 1 1 calc R . . C62 C 0.6912(2) 0.71880(19) 0.7581(2) 0.0447(10) Uani 1 1 d . . . H62 H 0.6916 0.6828 0.7729 0.054 Uiso 1 1 calc R D . C63 C 0.7535(2) 0.74323(18) 0.7473(2) 0.0403(9) Uani 1 1 d . D . H63 H 0.7964 0.7239 0.7556 0.048 Uiso 1 1 calc R . . C64 C 0.7538(2) 0.79527(17) 0.72464(19) 0.0355(8) Uani 1 1 d . . . C65 C 0.6895(2) 0.82311(17) 0.71278(19) 0.0345(8) Uani 1 1 d . D . C66 C 0.8208(2) 0.82296(19) 0.7134(2) 0.0399(9) Uani 1 1 d . D . H66A H 0.8185 0.8611 0.7261 0.048 Uiso 1 1 calc R . . H66B H 0.8610 0.8064 0.7417 0.048 Uiso 1 1 calc R . . C67 C 0.8999(3) 0.7169(2) 0.5340(3) 0.0535(12) Uani 1 1 d . . . C68 C 0.4464(2) 0.7322(2) 0.5151(2) 0.0455(10) Uani 1 1 d . D . C70 C 0.8142(6) 0.9794(5) 0.6994(7) 0.0650(10) Uani 0.50 1 d PD C 1 H70A H 0.7833 1.0056 0.6732 0.078 Uiso 0.50 1 calc PR C 1 H70B H 0.7845 0.9567 0.7234 0.078 Uiso 0.50 1 calc PR C 1 C71 C 0.8699(6) 1.0100(4) 0.7493(6) 0.0650(10) Uani 0.50 1 d PD C 1 H71A H 0.8961 0.9830 0.7782 0.078 Uiso 0.50 1 calc PR C 1 H71B H 0.9039 1.0272 0.7242 0.078 Uiso 0.50 1 calc PR C 1 C72 C 0.8433(6) 1.0541(4) 0.7940(7) 0.0650(10) Uani 0.50 1 d PD C 1 H72A H 0.8837 1.0701 0.8217 0.097 Uiso 0.50 1 calc PR C 1 H72B H 0.8117 1.0378 0.8214 0.097 Uiso 0.50 1 calc PR C 1 H72C H 0.8180 1.0819 0.7666 0.097 Uiso 0.50 1 calc PR C 1 C73 C 0.5187(3) 0.9588(2) 0.6459(4) 0.0732(9) Uani 0.50 1 d PD D 1 H73A H 0.4938 0.9431 0.6800 0.088 Uiso 0.50 1 calc PR D 1 H73B H 0.4835 0.9673 0.6075 0.088 Uiso 0.50 1 calc PR D 1 C74 C 0.5561(3) 1.0084(3) 0.6710(3) 0.0732(9) Uani 0.50 1 d PD D 1 H74A H 0.5876 1.0200 0.6398 0.088 Uiso 0.50 1 calc PR D 1 H74B H 0.5213 1.0372 0.6737 0.088 Uiso 0.50 1 calc PR D 1 C75 C 0.5977(3) 1.0009(3) 0.7354(3) 0.0732(9) Uani 0.50 1 d PD D 1 H75A H 0.6312 0.9708 0.7343 0.088 Uiso 0.50 1 calc PR D 1 H75B H 0.5666 0.9926 0.7681 0.088 Uiso 0.50 1 calc PR D 1 C76 C 0.6387(6) 1.0546(5) 0.7534(7) 0.0732(9) Uani 0.50 1 d PD D 1 H76A H 0.6673 1.0511 0.7964 0.110 Uiso 0.50 1 calc PR D 1 H76B H 0.6051 1.0840 0.7544 0.110 Uiso 0.50 1 calc PR D 1 H76C H 0.6694 1.0623 0.7206 0.110 Uiso 0.50 1 calc PR D 1 C77 C 0.5914(3) 0.6953(2) 0.4774(3) 0.0564(13) Uani 1 1 d . . . H77 H 0.5749 0.7180 0.4416 0.068 Uiso 1 1 calc R . . C78 C 0.6659(5) 0.6808(3) 0.5794(4) 0.107(3) Uani 1 1 d . . . H78A H 0.6570 0.6990 0.6193 0.161 Uiso 1 1 calc R . . H78B H 0.7166 0.6751 0.5811 0.161 Uiso 1 1 calc R . . H78C H 0.6417 0.6461 0.5758 0.161 Uiso 1 1 calc R . . C79 C 0.6657(3) 0.7674(2) 0.5276(4) 0.0761(19) Uani 1 1 d . . . H79A H 0.6483 0.7879 0.4882 0.114 Uiso 1 1 calc R . . H79B H 0.7172 0.7663 0.5334 0.114 Uiso 1 1 calc R . . H79C H 0.6502 0.7845 0.5656 0.114 Uiso 1 1 calc R . . C80 C 1.0972(3) 0.72896(19) 0.4250(2) 0.0496(11) Uani 1 1 d . . . H80 H 1.0588 0.7463 0.3993 0.059 Uiso 1 1 calc R . . C81 C 1.1651(3) 0.7512(2) 0.4276(2) 0.0510(11) Uani 1 1 d . . . H81 H 1.1721 0.7830 0.4041 0.061 Uiso 1 1 calc R . . C82 C 1.2197(3) 0.7267(2) 0.4641(2) 0.0470(10) Uani 1 1 d . . . H82 H 1.2656 0.7415 0.4668 0.056 Uiso 1 1 calc R . . C83 C 1.2092(2) 0.67985(18) 0.4977(2) 0.0404(9) Uani 1 1 d . . . C84 C 1.1403(2) 0.66047(17) 0.4930(2) 0.0377(9) Uani 1 1 d . . . C85 C 1.2657(3) 0.65111(19) 0.5354(2) 0.0451(10) Uani 1 1 d . . . H85 H 1.3124 0.6644 0.5390 0.054 Uiso 1 1 calc R . . C86 C 1.2526(3) 0.6058(2) 0.5652(2) 0.0469(11) Uani 1 1 d . . . H86 H 1.2908 0.5869 0.5892 0.056 Uiso 1 1 calc R . . C87 C 1.1838(3) 0.58460(18) 0.5625(2) 0.0431(10) Uani 1 1 d . . . C88 C 1.1263(2) 0.61199(16) 0.5262(2) 0.0386(9) Uani 1 1 d . . . C89 C 1.1678(3) 0.53692(19) 0.5931(2) 0.0503(11) Uani 1 1 d . . . H89 H 1.2045 0.5167 0.6174 0.060 Uiso 1 1 calc R . . C90 C 1.1014(3) 0.51974(19) 0.5884(2) 0.0533(12) Uani 1 1 d . . . H90 H 1.0907 0.4877 0.6097 0.064 Uiso 1 1 calc R . . C91 C 1.0475(3) 0.54963(19) 0.5515(2) 0.0521(12) Uani 1 1 d . . . H91 H 1.0005 0.5370 0.5484 0.062 Uiso 1 1 calc R . . C92 C 0.4858(3) 0.5582(2) 0.5453(3) 0.0558(12) Uani 1 1 d . . . H92 H 0.5278 0.5786 0.5538 0.067 Uiso 1 1 calc R . . C93 C 0.4784(4) 0.5130(2) 0.5838(3) 0.0651(15) Uani 1 1 d . . . H93 H 0.5141 0.5035 0.6185 0.078 Uiso 1 1 calc R . . C94 C 0.4186(4) 0.4829(2) 0.5704(3) 0.0643(15) Uani 1 1 d . . . H94 H 0.4133 0.4514 0.5950 0.077 Uiso 1 1 calc R . . C95 C 0.3657(3) 0.4982(2) 0.5208(3) 0.0576(14) Uani 1 1 d . . . C96 C 0.3765(3) 0.54477(19) 0.4851(2) 0.0474(11) Uani 1 1 d . . . C97 C 0.3012(4) 0.4699(2) 0.5051(3) 0.0697(17) Uani 1 1 d . . . H97 H 0.2951 0.4371 0.5269 0.084 Uiso 1 1 calc R . . C98 C 0.2488(4) 0.4879(2) 0.4609(3) 0.0696(17) Uani 1 1 d . . . H98 H 0.2061 0.4683 0.4527 0.083 Uiso 1 1 calc R . . C99 C 0.2567(3) 0.5362(2) 0.4259(3) 0.0567(13) Uani 1 1 d . . . C100 C 0.3216(3) 0.5641(2) 0.4367(2) 0.0497(11) Uani 1 1 d . . . C101 C 0.2027(3) 0.5591(3) 0.3830(3) 0.0661(16) Uani 1 1 d . . . H101 H 0.1585 0.5414 0.3743 0.079 Uiso 1 1 calc R . . C102 C 0.2123(3) 0.6060(3) 0.3538(3) 0.0631(15) Uani 1 1 d . . . H102 H 0.1749 0.6223 0.3255 0.076 Uiso 1 1 calc R . . C103 C 0.2781(3) 0.6304(2) 0.3658(2) 0.0540(12) Uani 1 1 d . . . H103 H 0.2849 0.6630 0.3441 0.065 Uiso 1 1 calc R . . C104 C 0.7718(3) 0.6384(2) 0.3792(3) 0.0559(13) Uani 1 1 d . . . H104 H 0.7884 0.6677 0.4064 0.067 Uiso 1 1 calc R . . C105 C 0.7104(5) 0.7021(3) 0.3046(4) 0.095(3) Uani 1 1 d . . . H10A H 0.7378 0.7276 0.3339 0.143 Uiso 1 1 calc R . . H10B H 0.6602 0.7072 0.3066 0.143 Uiso 1 1 calc R . . H10C H 0.7195 0.7080 0.2598 0.143 Uiso 1 1 calc R . . C106 C 0.7059(3) 0.6076(3) 0.2779(3) 0.0757(19) Uani 1 1 d . . . H10D H 0.7286 0.5736 0.2919 0.114 Uiso 1 1 calc R . . H10E H 0.7178 0.6175 0.2350 0.114 Uiso 1 1 calc R . . H10F H 0.6548 0.6039 0.2750 0.114 Uiso 1 1 calc R . . C107 C 0.8891(3) 0.8034(2) 0.3186(3) 0.0614(14) Uani 1 1 d . . . H10G H 0.8932 0.7983 0.3659 0.092 Uiso 1 1 calc R . . H10H H 0.8442 0.7888 0.2975 0.092 Uiso 1 1 calc R . . H10I H 0.8913 0.8418 0.3088 0.092 Uiso 1 1 calc R . . O21A O 0.4772(6) 0.6399(4) 0.6847(5) 0.078(2) Uani 0.50 1 d P E 2 C70A C 0.8356(6) 0.9940(4) 0.6743(6) 0.0650(10) Uani 0.50 1 d PD F 2 H70C H 0.7960 1.0100 0.6447 0.078 Uiso 0.50 1 calc PR F 2 H70D H 0.8767 1.0183 0.6775 0.078 Uiso 0.50 1 calc PR F 2 C76A C 0.5451(6) 1.0025(5) 0.7877(7) 0.0732(9) Uani 0.50 1 d PD D 2 H76D H 0.5715 0.9974 0.8315 0.110 Uiso 0.50 1 calc PR D 2 H76E H 0.5102 0.9738 0.7784 0.110 Uiso 0.50 1 calc PR D 2 H76F H 0.5211 1.0372 0.7855 0.110 Uiso 0.50 1 calc PR D 2 C71A C 0.8168(6) 0.9840(4) 0.7361(6) 0.0650(10) Uani 0.50 1 d PD F 2 H71C H 0.8491 0.9569 0.7588 0.078 Uiso 0.50 1 calc PR F 2 H71D H 0.7687 0.9689 0.7306 0.078 Uiso 0.50 1 calc PR F 2 C72A C 0.8190(6) 1.0374(4) 0.7815(7) 0.0650(10) Uani 0.50 1 d PD F 2 H72D H 0.8060 1.0279 0.8241 0.097 Uiso 0.50 1 calc PR F 2 H72E H 0.7858 1.0640 0.7602 0.097 Uiso 0.50 1 calc PR F 2 H72F H 0.8666 1.0525 0.7876 0.097 Uiso 0.50 1 calc PR F 2 C69 C 0.8523(3) 0.9435(2) 0.6527(3) 0.0650(10) Uani 0.50 1 d PD C 1 H69A H 0.8731 0.9657 0.6208 0.078 Uiso 0.50 1 calc PR C 1 H69B H 0.8897 0.9216 0.6779 0.078 Uiso 0.50 1 calc PR C 1 C69A C 0.8523(3) 0.9435(2) 0.6527(3) 0.0650(10) Uani 0.50 1 d PD F 2 H69C H 0.8760 0.9234 0.6910 0.078 Uiso 0.50 1 calc PR F 2 H69D H 0.8871 0.9483 0.6224 0.078 Uiso 0.50 1 calc PR F 2 C75A C 0.5977(3) 1.0009(3) 0.7354(3) 0.0732(9) Uani 0.50 1 d PD D 2 H75C H 0.6332 1.0297 0.7442 0.088 Uiso 0.50 1 calc PR D 2 H75D H 0.6225 0.9660 0.7373 0.088 Uiso 0.50 1 calc PR D 2 C74A C 0.5561(3) 1.0084(3) 0.6710(3) 0.0732(9) Uani 0.50 1 d PD D 2 H74C H 0.5876 1.0200 0.6398 0.088 Uiso 0.50 1 calc PR D 2 H74D H 0.5213 1.0372 0.6737 0.088 Uiso 0.50 1 calc PR D 2 C73A C 0.5187(3) 0.9588(2) 0.6459(4) 0.0732(9) Uani 0.50 1 d PD D 2 H73C H 0.4938 0.9431 0.6800 0.088 Uiso 0.50 1 calc PR D 2 H73D H 0.4835 0.9673 0.6075 0.088 Uiso 0.50 1 calc PR D 2 O22A O 1.0221(7) 0.6094(5) 0.6933(6) 0.0871(19) Uani 0.40 1 d P G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04341(19) 0.03993(17) 0.03333(15) 0.00191(11) 0.01241(12) 0.00051(12) Cd2 0.0461(2) 0.03810(18) 0.04331(18) 0.00647(12) -0.00489(14) -0.01138(13) O1 0.0179(12) 0.0438(15) 0.0322(13) 0.0008(11) 0.0072(10) 0.0008(10) O2 0.0207(12) 0.0427(15) 0.0419(15) -0.0057(12) 0.0095(11) -0.0036(11) O3 0.0202(12) 0.0432(15) 0.0331(13) -0.0003(11) 0.0083(10) 0.0005(10) O4 0.0223(13) 0.0457(16) 0.0408(14) 0.0096(12) 0.0069(11) -0.0017(11) O5 0.0531(19) 0.0456(17) 0.0384(15) 0.0019(13) 0.0191(14) -0.0062(14) O6 0.0518(19) 0.0447(17) 0.0385(15) 0.0013(13) 0.0149(13) 0.0003(14) O7 0.058(2) 0.055(2) 0.0472(18) -0.0080(15) -0.0100(16) 0.0115(17) O8 0.085(3) 0.059(2) 0.0477(19) 0.0184(16) -0.0197(18) -0.035(2) O9 0.0196(13) 0.0430(17) 0.079(2) -0.0054(15) 0.0042(14) -0.0002(12) O10 0.0277(15) 0.0476(17) 0.0614(19) 0.0073(15) 0.0106(13) 0.0018(13) O11 0.0224(13) 0.0435(16) 0.0616(19) -0.0030(14) 0.0140(13) -0.0006(12) O12 0.0216(13) 0.0446(16) 0.0563(18) 0.0073(14) 0.0066(12) 0.0011(12) O13 0.223(8) 0.104(4) 0.068(3) -0.023(3) -0.018(4) 0.104(5) O14 0.084(3) 0.062(2) 0.089(3) -0.016(2) 0.058(3) -0.016(2) O15 0.051(2) 0.056(2) 0.057(2) -0.0159(16) -0.0017(16) 0.0102(16) O16 0.057(2) 0.050(2) 0.075(2) -0.0115(18) 0.0097(19) -0.0104(17) O17 0.0440(18) 0.0451(18) 0.0539(19) 0.0009(14) 0.0101(15) 0.0017(14) O18 0.063(2) 0.0425(18) 0.068(2) 0.0024(16) 0.0170(18) -0.0138(16) O19 0.072(3) 0.073(3) 0.090(3) 0.023(2) -0.002(2) 0.013(2) O20 0.079(3) 0.061(2) 0.092(3) -0.010(2) 0.045(2) -0.018(2) O21 0.076(4) 0.072(4) 0.092(5) 0.033(3) 0.031(4) -0.005(4) O22 0.096(5) 0.085(5) 0.083(4) -0.002(4) 0.023(4) 0.001(4) O23 0.082(4) 0.133(5) 0.162(6) -0.035(5) -0.010(4) 0.014(4) N00H 0.047(2) 0.0332(18) 0.0384(17) 0.0020(14) -0.0015(15) -0.0055(15) N00K 0.052(2) 0.049(2) 0.0364(18) -0.0026(15) 0.0210(16) -0.0020(17) N00L 0.056(2) 0.0322(18) 0.0399(18) 0.0041(14) 0.0031(16) -0.0040(16) N00M 0.0324(19) 0.055(2) 0.050(2) 0.0074(17) 0.0051(16) -0.0048(16) N00N 0.056(2) 0.044(2) 0.0399(19) 0.0046(15) 0.0174(17) 0.0073(18) N00R 0.047(2) 0.061(3) 0.056(2) -0.004(2) 0.0150(19) -0.0058(19) C1 0.0136(15) 0.041(2) 0.0397(19) 0.0033(15) 0.0037(13) -0.0035(14) C2 0.0174(16) 0.043(2) 0.0339(18) 0.0058(15) 0.0035(13) -0.0022(14) C3 0.0158(16) 0.046(2) 0.0339(18) 0.0025(16) 0.0042(13) 0.0004(14) C4 0.0201(17) 0.040(2) 0.0348(18) 0.0028(15) 0.0071(14) 0.0011(14) C5 0.0174(16) 0.042(2) 0.0354(18) 0.0066(15) 0.0052(14) 0.0017(14) C6 0.0152(15) 0.043(2) 0.0340(18) 0.0019(15) 0.0076(13) -0.0008(14) C7 0.0229(17) 0.041(2) 0.0378(19) 0.0081(16) 0.0090(15) 0.0050(15) C8 0.0271(18) 0.0357(19) 0.0317(17) 0.0077(14) 0.0065(14) 0.0012(14) C9 0.038(2) 0.032(2) 0.044(2) 0.0058(16) 0.0155(17) 0.0049(16) C10 0.045(2) 0.033(2) 0.047(2) 0.0002(17) 0.0105(19) -0.0027(17) C11 0.035(2) 0.037(2) 0.043(2) 0.0050(16) 0.0065(17) -0.0083(16) C12 0.0253(18) 0.0352(19) 0.0326(17) 0.0064(14) 0.0078(14) -0.0025(14) C13 0.0254(17) 0.0318(18) 0.0310(17) 0.0054(14) 0.0076(14) -0.0008(14) C14 0.0233(18) 0.041(2) 0.0376(19) 0.0071(16) 0.0089(15) -0.0047(15) C15 0.0172(16) 0.042(2) 0.0342(18) 0.0052(15) 0.0079(13) -0.0025(14) C16 0.0225(17) 0.040(2) 0.0380(19) 0.0016(16) 0.0065(14) -0.0041(15) C17 0.0204(17) 0.046(2) 0.0337(18) 0.0020(16) 0.0071(14) -0.0064(15) C18 0.0213(17) 0.044(2) 0.0387(19) 0.0062(16) 0.0064(14) -0.0045(15) C19 0.0181(16) 0.039(2) 0.0387(19) 0.0006(15) 0.0072(14) -0.0008(14) C20 0.0152(15) 0.041(2) 0.0351(18) 0.0006(15) 0.0079(13) -0.0023(14) C21 0.0251(18) 0.037(2) 0.044(2) 0.0016(16) 0.0079(16) 0.0050(15) C22 0.0248(18) 0.0313(18) 0.0382(19) -0.0001(14) 0.0057(14) -0.0009(14) C23 0.033(2) 0.034(2) 0.041(2) 0.0021(16) 0.0035(16) 0.0005(15) C24 0.039(2) 0.040(2) 0.040(2) 0.0055(17) 0.0048(17) -0.0046(18) C25 0.032(2) 0.037(2) 0.042(2) 0.0021(16) 0.0120(16) -0.0073(16) C26 0.0273(18) 0.0312(18) 0.0365(19) -0.0014(14) 0.0051(15) -0.0018(14) C27 0.0285(18) 0.0315(18) 0.0334(18) -0.0010(14) 0.0068(14) -0.0010(14) C28 0.0198(17) 0.038(2) 0.041(2) 0.0003(15) 0.0051(14) -0.0062(14) C29 0.0247(18) 0.048(2) 0.0324(18) 0.0032(16) 0.0047(14) -0.0009(16) C30 0.027(2) 0.059(3) 0.035(2) 0.0009(18) 0.0071(16) -0.0102(18) C31 0.0205(19) 0.074(3) 0.040(2) 0.007(2) -0.0001(16) -0.0034(19) C32 0.046(3) 0.155(7) 0.034(2) -0.017(3) 0.009(2) -0.038(4) C33 0.056(4) 0.279(13) 0.036(3) 0.011(5) 0.003(3) -0.080(6) C34 0.047(3) 0.074(3) 0.044(2) -0.008(2) 0.013(2) -0.019(3) C35 0.0277(19) 0.050(2) 0.040(2) 0.0021(17) 0.0141(16) 0.0068(17) C36 0.040(2) 0.048(2) 0.039(2) -0.0012(18) 0.0135(17) 0.0037(19) C37 0.037(2) 0.052(3) 0.042(2) -0.0026(19) 0.0067(18) 0.0021(19) C38 0.042(3) 0.062(3) 0.055(3) 0.009(2) 0.008(2) 0.001(2) C39 0.0159(17) 0.048(2) 0.046(2) -0.0012(17) 0.0061(15) -0.0032(15) C40 0.0237(19) 0.044(2) 0.049(2) 0.0015(18) 0.0042(16) 0.0016(16) C41 0.0208(18) 0.055(3) 0.053(2) -0.005(2) 0.0065(17) -0.0024(17) C42 0.0238(19) 0.062(3) 0.049(2) 0.005(2) 0.0136(17) -0.0061(18) C43 0.0205(18) 0.053(3) 0.057(3) 0.013(2) 0.0115(17) -0.0074(17) C44 0.0156(17) 0.043(2) 0.060(3) 0.0021(19) 0.0071(16) -0.0013(15) C45 0.032(2) 0.066(3) 0.069(3) 0.025(3) 0.020(2) -0.005(2) C46 0.032(2) 0.056(3) 0.055(3) 0.022(2) 0.0141(19) 0.0022(19) C47 0.045(3) 0.068(3) 0.053(3) 0.018(2) 0.025(2) 0.009(2) C48 0.052(3) 0.074(4) 0.046(3) 0.010(2) 0.017(2) 0.008(2) C49 0.041(3) 0.068(3) 0.046(2) 0.015(2) 0.009(2) 0.002(2) C50 0.032(2) 0.052(3) 0.047(2) 0.0176(19) 0.0119(18) 0.0050(18) C51 0.037(2) 0.046(2) 0.049(2) 0.0149(19) 0.0144(19) 0.0023(18) C52 0.033(2) 0.051(3) 0.052(2) 0.012(2) 0.0127(18) 0.0071(18) C53 0.0196(18) 0.051(2) 0.048(2) 0.0080(19) 0.0107(16) 0.0032(16) C54 0.0209(18) 0.056(3) 0.041(2) 0.0005(18) 0.0044(15) 0.0056(17) C55 0.0168(17) 0.049(2) 0.046(2) -0.0037(18) 0.0096(15) 0.0017(15) C56 0.0210(17) 0.045(2) 0.045(2) 0.0046(17) 0.0134(15) 0.0011(15) C57 0.0150(16) 0.051(2) 0.042(2) 0.0008(17) 0.0095(14) -0.0001(15) C58 0.0145(16) 0.048(2) 0.048(2) -0.0011(18) 0.0081(15) -0.0003(15) C59 0.0255(19) 0.050(2) 0.042(2) 0.0027(18) 0.0117(16) 0.0011(17) C60 0.0221(18) 0.048(2) 0.0336(18) 0.0005(16) 0.0059(14) -0.0021(15) C61 0.030(2) 0.050(2) 0.040(2) 0.0047(18) 0.0070(16) -0.0045(17) C62 0.043(2) 0.046(2) 0.045(2) 0.0065(19) 0.0077(19) -0.0015(19) C63 0.034(2) 0.050(2) 0.038(2) -0.0006(17) 0.0068(16) 0.0017(18) C64 0.0245(18) 0.045(2) 0.0371(19) -0.0027(16) 0.0046(15) -0.0018(16) C65 0.0238(18) 0.043(2) 0.0370(19) -0.0025(16) 0.0056(15) -0.0019(15) C66 0.0218(18) 0.050(2) 0.047(2) -0.0031(18) 0.0052(16) -0.0019(16) C67 0.039(3) 0.062(3) 0.059(3) -0.020(2) 0.006(2) 0.005(2) C68 0.028(2) 0.052(3) 0.058(3) -0.011(2) 0.0094(19) 0.0048(18) C70 0.045(2) 0.0451(19) 0.102(3) -0.0036(19) 0.001(2) -0.0062(14) C71 0.045(2) 0.0451(19) 0.102(3) -0.0036(19) 0.001(2) -0.0062(14) C72 0.045(2) 0.0451(19) 0.102(3) -0.0036(19) 0.001(2) -0.0062(14) C73 0.056(2) 0.067(2) 0.098(3) -0.0074(18) 0.0157(17) 0.0080(15) C74 0.056(2) 0.067(2) 0.098(3) -0.0074(18) 0.0157(17) 0.0080(15) C75 0.056(2) 0.067(2) 0.098(3) -0.0074(18) 0.0157(17) 0.0080(15) C76 0.056(2) 0.067(2) 0.098(3) -0.0074(18) 0.0157(17) 0.0080(15) C77 0.038(3) 0.070(4) 0.062(3) 0.007(3) 0.009(2) 0.008(2) C78 0.136(8) 0.093(6) 0.078(5) 0.021(4) -0.032(5) -0.014(5) C79 0.029(3) 0.060(3) 0.136(6) -0.008(4) 0.003(3) -0.002(2) C80 0.053(3) 0.041(2) 0.051(3) 0.0080(19) -0.005(2) -0.008(2) C81 0.057(3) 0.045(3) 0.049(3) 0.003(2) 0.003(2) -0.016(2) C82 0.046(3) 0.052(3) 0.043(2) -0.0077(19) 0.0063(19) -0.012(2) C83 0.039(2) 0.047(2) 0.035(2) -0.0097(17) 0.0059(17) 0.0012(18) C84 0.045(2) 0.035(2) 0.0337(19) -0.0042(15) 0.0060(17) -0.0017(17) C85 0.043(2) 0.053(3) 0.040(2) -0.0113(19) 0.0081(18) 0.005(2) C86 0.043(3) 0.054(3) 0.042(2) -0.010(2) 0.0040(19) 0.012(2) C87 0.057(3) 0.038(2) 0.0336(19) -0.0054(16) 0.0074(18) 0.0098(19) C88 0.048(2) 0.032(2) 0.0340(19) -0.0061(15) 0.0035(17) 0.0013(17) C89 0.063(3) 0.039(2) 0.046(2) -0.0009(19) 0.002(2) 0.010(2) C90 0.077(4) 0.034(2) 0.048(3) 0.0085(19) 0.005(2) 0.000(2) C91 0.062(3) 0.040(2) 0.053(3) 0.005(2) 0.003(2) -0.010(2) C92 0.068(3) 0.050(3) 0.050(3) 0.007(2) 0.014(2) 0.003(2) C93 0.082(4) 0.060(3) 0.054(3) 0.016(3) 0.014(3) 0.016(3) C94 0.087(4) 0.044(3) 0.067(3) 0.012(2) 0.029(3) 0.009(3) C95 0.076(4) 0.043(3) 0.063(3) 0.004(2) 0.039(3) 0.005(2) C96 0.059(3) 0.042(2) 0.046(2) -0.0011(19) 0.024(2) 0.001(2) C97 0.096(5) 0.046(3) 0.077(4) -0.002(3) 0.045(4) -0.009(3) C98 0.085(5) 0.056(3) 0.074(4) -0.012(3) 0.034(3) -0.018(3) C99 0.062(3) 0.061(3) 0.053(3) -0.015(2) 0.025(2) -0.012(3) C100 0.064(3) 0.048(3) 0.042(2) -0.0098(19) 0.026(2) -0.004(2) C101 0.066(4) 0.090(4) 0.045(3) -0.013(3) 0.018(3) -0.017(3) C102 0.056(3) 0.091(4) 0.044(3) -0.006(3) 0.012(2) -0.006(3) C103 0.057(3) 0.070(3) 0.037(2) 0.002(2) 0.012(2) 0.000(3) C104 0.042(3) 0.067(3) 0.061(3) 0.011(2) 0.012(2) -0.003(2) C105 0.122(7) 0.067(4) 0.088(5) 0.024(4) -0.015(5) -0.008(4) C106 0.038(3) 0.096(5) 0.090(4) -0.028(4) 0.001(3) -0.002(3) C107 0.070(4) 0.053(3) 0.059(3) -0.001(2) 0.000(3) 0.001(3) O21A 0.076(4) 0.072(4) 0.092(5) 0.033(3) 0.031(4) -0.005(4) C70A 0.045(2) 0.0451(19) 0.102(3) -0.0036(19) 0.001(2) -0.0062(14) C76A 0.056(2) 0.067(2) 0.098(3) -0.0074(18) 0.0157(17) 0.0080(15) C71A 0.045(2) 0.0451(19) 0.102(3) -0.0036(19) 0.001(2) -0.0062(14) C72A 0.045(2) 0.0451(19) 0.102(3) -0.0036(19) 0.001(2) -0.0062(14) C69 0.045(2) 0.0451(19) 0.102(3) -0.0036(19) 0.001(2) -0.0062(14) C69A 0.045(2) 0.0451(19) 0.102(3) -0.0036(19) 0.001(2) -0.0062(14) C75A 0.056(2) 0.067(2) 0.098(3) -0.0074(18) 0.0157(17) 0.0080(15) C74A 0.056(2) 0.067(2) 0.098(3) -0.0074(18) 0.0157(17) 0.0080(15) C73A 0.056(2) 0.067(2) 0.098(3) -0.0074(18) 0.0157(17) 0.0080(15) O22A 0.096(5) 0.085(5) 0.083(4) -0.002(4) 0.023(4) 0.001(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 Cd1 O15 2.212(3) . ? Cd1 N00N 2.292(4) . ? Cd1 N00K 2.345(4) . ? Cd1 O5 2.347(3) . ? Cd1 O17 2.349(3) . ? Cd1 O6 2.372(3) . ? Cd1 C29 2.701(4) . ? Cd2 O14 2.205(4) . ? Cd2 O8 2.326(4) . ? Cd2 N00H 2.328(4) . ? Cd2 N00L 2.334(4) . ? Cd2 O18 2.351(3) . ? Cd2 O7 2.450(3) . ? Cd2 C30 2.728(4) . ? O1 C6 1.391(4) . ? O1 C31 1.438(5) . ? O2 C13 1.357(5) . ? O3 C20 1.391(4) . ? O3 C35 1.440(4) . ? O4 C27 1.353(5) . ? O5 C29 1.253(5) . ? O6 C29 1.254(5) . ? O7 C30 1.242(6) . ? O8 C30 1.244(6) . ? O9 C44 1.380(5) . ? O9 C69 1.430(6) . ? O10 C51 1.349(6) . ? O11 C58 1.376(5) . ? O11 C73 1.451(6) . ? O12 C65 1.357(5) . ? O13 C67 1.226(8) . ? O14 C67 1.226(6) . ? O15 C68 1.266(6) . ? O16 C68 1.245(6) . ? O17 C77 1.258(6) . ? O19 C104 1.236(7) . ? O20 C107 1.409(7) . ? N00H C80 1.307(6) . ? N00H C84 1.359(6) . ? N00K C103 1.312(7) . ? N00K C100 1.352(6) . ? N00L C91 1.318(6) . ? N00L C88 1.346(6) . ? N00M C104 1.315(7) . ? N00M C105 1.432(8) . ? N00M C106 1.434(7) . ? N00N C92 1.323(7) . ? N00N C96 1.350(7) . ? N00R C77 1.286(7) . ? N00R C79 1.409(7) . ? N00R C78 1.503(8) . ? C1 C2 1.385(5) . ? C1 C6 1.385(5) . ? C1 C28 1.518(6) . ? C2 C3 1.381(6) . ? C3 C4 1.396(5) . ? C3 C29 1.487(5) . ? C4 C5 1.386(5) . ? C5 C6 1.394(6) . ? C5 C7 1.514(5) . ? C7 C8 1.510(5) . ? C8 C9 1.388(6) . ? C8 C13 1.397(5) . ? C9 C10 1.385(6) . ? C10 C11 1.386(6) . ? C11 C12 1.380(6) . ? C12 C13 1.403(5) . ? C12 C14 1.510(5) . ? C14 C15 1.517(5) . ? C15 C20 1.386(5) . ? C15 C16 1.396(5) . ? C16 C17 1.396(6) . ? C17 C18 1.388(6) . ? C17 C30 1.495(6) . ? C18 C19 1.391(5) . ? C19 C20 1.397(5) . ? C19 C21 1.504(6) . ? C21 C22 1.518(5) . ? C22 C23 1.385(5) . ? C22 C27 1.400(5) . ? C23 C24 1.382(6) . ? C24 C25 1.374(6) . ? C25 C26 1.384(5) . ? C26 C27 1.397(5) . ? C26 C28 1.505(5) . ? C31 C32 1.445(7) . ? C32 C33 1.333(8) . ? C33 C34 1.466(7) . ? C35 C36 1.512(6) . ? C36 C37 1.521(6) . ? C37 C38 1.511(7) . ? C39 C40 1.382(6) . ? C39 C44 1.402(6) . ? C39 C66 1.505(6) . ? C40 C41 1.385(6) . ? C41 C42 1.384(7) . ? C41 C67 1.489(7) . ? C42 C43 1.363(7) . ? C43 C44 1.392(7) . ? C43 C45 1.521(7) . ? C45 C46 1.512(7) . ? C46 C47 1.391(8) . ? C46 C51 1.400(6) . ? C47 C48 1.386(8) . ? C48 C49 1.385(7) . ? C49 C50 1.381(7) . ? C50 C51 1.405(6) . ? C50 C52 1.522(6) . ? C52 C53 1.516(6) . ? C53 C54 1.377(7) . ? C53 C58 1.396(6) . ? C54 C55 1.383(6) . ? C55 C56 1.394(6) . ? C55 C68 1.487(6) . ? C56 C57 1.381(6) . ? C57 C58 1.398(6) . ? C57 C59 1.519(6) . ? C59 C60 1.512(6) . ? C60 C61 1.389(6) . ? C60 C65 1.396(5) . ? C61 C62 1.386(6) . ? C62 C63 1.391(6) . ? C63 C64 1.382(6) . ? C64 C65 1.409(6) . ? C64 C66 1.511(6) . ? C70 C71 1.574(13) . ? C70 C69 1.575(12) . ? C71 C72 1.569(13) . ? C73 C74 1.487(8) . ? C74 C75 1.463(8) . ? C75 C76 1.574(12) . ? C80 C81 1.412(7) . ? C81 C82 1.348(7) . ? C82 C83 1.392(7) . ? C83 C84 1.400(6) . ? C83 C85 1.434(7) . ? C84 C88 1.437(6) . ? C85 C86 1.331(7) . ? C86 C87 1.418(7) . ? C87 C89 1.404(7) . ? C87 C88 1.418(6) . ? C89 C90 1.337(8) . ? C90 C91 1.408(7) . ? C92 C93 1.401(7) . ? C93 C94 1.367(9) . ? C94 C95 1.390(9) . ? C95 C96 1.410(7) . ? C95 C97 1.422(9) . ? C96 C100 1.429(7) . ? C97 C98 1.336(10) . ? C98 C99 1.428(8) . ? C99 C101 1.386(9) . ? C99 C100 1.418(7) . ? C101 C102 1.345(9) . ? C102 C103 1.393(8) . ? C70A C71A 1.403(14) . ? C71A C72A 1.628(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O15 Cd1 N00N 126.26(14) . . ? O15 Cd1 N00K 105.48(14) . . ? N00N Cd1 N00K 72.05(15) . . ? O15 Cd1 O5 138.33(13) . . ? N00N Cd1 O5 95.32(12) . . ? N00K Cd1 O5 88.46(12) . . ? O15 Cd1 O17 89.60(12) . . ? N00N Cd1 O17 86.51(13) . . ? N00K Cd1 O17 158.32(13) . . ? O5 Cd1 O17 90.40(12) . . ? O15 Cd1 O6 83.13(13) . . ? N00N Cd1 O6 149.87(12) . . ? N00K Cd1 O6 109.54(12) . . ? O5 Cd1 O6 55.25(11) . . ? O17 Cd1 O6 87.31(12) . . ? O15 Cd1 C29 110.77(14) . . ? N00N Cd1 C29 122.66(13) . . ? N00K Cd1 C29 100.18(12) . . ? O5 Cd1 C29 27.60(12) . . ? O17 Cd1 C29 88.50(12) . . ? O6 Cd1 C29 27.65(12) . . ? O14 Cd2 O8 126.79(17) . . ? O14 Cd2 N00H 98.29(14) . . ? O8 Cd2 N00H 109.22(14) . . ? O14 Cd2 N00L 128.58(16) . . ? O8 Cd2 N00L 103.48(14) . . ? N00H Cd2 N00L 71.35(13) . . ? O14 Cd2 O18 89.20(14) . . ? O8 Cd2 O18 85.63(13) . . ? N00H Cd2 O18 153.46(13) . . ? N00L Cd2 O18 84.04(14) . . ? O14 Cd2 O7 82.04(15) . . ? O8 Cd2 O7 53.79(12) . . ? N00H Cd2 O7 90.90(13) . . ? N00L Cd2 O7 145.55(13) . . ? O18 Cd2 O7 115.42(13) . . ? O14 Cd2 C30 103.36(17) . . ? O8 Cd2 C30 27.03(13) . . ? N00H Cd2 C30 103.96(12) . . ? N00L Cd2 C30 128.06(14) . . ? O18 Cd2 C30 98.94(13) . . ? O7 Cd2 C30 27.08(13) . . ? C6 O1 C31 114.0(3) . . ? C20 O3 C35 114.7(3) . . ? C29 O5 Cd1 92.2(3) . . ? C29 O6 Cd1 90.9(2) . . ? C30 O7 Cd2 89.0(3) . . ? C30 O8 Cd2 94.8(3) . . ? C44 O9 C69 114.6(3) . . ? C58 O11 C73 113.2(4) . . ? C67 O14 Cd2 117.6(4) . . ? C68 O15 Cd1 104.3(3) . . ? C77 O17 Cd1 115.1(3) . . ? C80 N00H C84 118.6(4) . . ? C80 N00H Cd2 125.2(3) . . ? C84 N00H Cd2 116.2(3) . . ? C103 N00K C100 118.3(5) . . ? C103 N00K Cd1 128.0(4) . . ? C100 N00K Cd1 113.7(3) . . ? C91 N00L C88 118.1(4) . . ? C91 N00L Cd2 125.9(4) . . ? C88 N00L Cd2 115.9(3) . . ? C104 N00M C105 122.0(5) . . ? C104 N00M C106 122.6(5) . . ? C105 N00M C106 115.3(5) . . ? C92 N00N C96 119.2(4) . . ? C92 N00N Cd1 124.9(4) . . ? C96 N00N Cd1 115.8(3) . . ? C77 N00R C79 129.1(5) . . ? C77 N00R C78 118.5(5) . . ? C79 N00R C78 111.9(5) . . ? C2 C1 C6 117.7(4) . . ? C2 C1 C28 119.4(3) . . ? C6 C1 C28 122.9(3) . . ? C3 C2 C1 121.4(4) . . ? C2 C3 C4 119.5(4) . . ? C2 C3 C29 120.2(4) . . ? C4 C3 C29 120.3(4) . . ? C5 C4 C3 120.6(4) . . ? C4 C5 C6 117.8(4) . . ? C4 C5 C7 119.9(4) . . ? C6 C5 C7 122.3(3) . . ? C1 C6 O1 120.0(4) . . ? C1 C6 C5 122.7(3) . . ? O1 C6 C5 117.3(3) . . ? C8 C7 C5 112.1(3) . . ? C9 C8 C13 118.0(4) . . ? C9 C8 C7 120.2(4) . . ? C13 C8 C7 121.8(4) . . ? C10 C9 C8 121.5(4) . . ? C9 C10 C11 119.3(4) . . ? C12 C11 C10 121.2(4) . . ? C11 C12 C13 118.5(4) . . ? C11 C12 C14 121.6(4) . . ? C13 C12 C14 120.0(3) . . ? O2 C13 C8 123.2(3) . . ? O2 C13 C12 115.4(3) . . ? C8 C13 C12 121.5(4) . . ? C12 C14 C15 111.5(3) . . ? C20 C15 C16 117.6(4) . . ? C20 C15 C14 123.0(3) . . ? C16 C15 C14 119.4(4) . . ? C15 C16 C17 121.1(4) . . ? C18 C17 C16 119.5(4) . . ? C18 C17 C30 119.8(4) . . ? C16 C17 C30 120.6(4) . . ? C17 C18 C19 120.9(4) . . ? C18 C19 C20 118.0(4) . . ? C18 C19 C21 119.9(4) . . ? C20 C19 C21 122.1(4) . . ? C15 C20 O3 119.2(3) . . ? C15 C20 C19 122.7(4) . . ? O3 C20 C19 117.9(3) . . ? C19 C21 C22 112.4(3) . . ? C23 C22 C27 118.3(4) . . ? C23 C22 C21 120.2(4) . . ? C27 C22 C21 121.6(3) . . ? C24 C23 C22 121.6(4) . . ? C25 C24 C23 119.2(4) . . ? C24 C25 C26 121.4(4) . . ? C25 C26 C27 118.7(4) . . ? C25 C26 C28 121.9(4) . . ? C27 C26 C28 119.4(3) . . ? O4 C27 C26 115.6(3) . . ? O4 C27 C22 123.6(3) . . ? C26 C27 C22 120.7(4) . . ? C26 C28 C1 112.3(3) . . ? O5 C29 O6 121.7(4) . . ? O5 C29 C3 118.5(4) . . ? O6 C29 C3 119.9(4) . . ? O5 C29 Cd1 60.2(2) . . ? O6 C29 Cd1 61.4(2) . . ? C3 C29 Cd1 178.7(3) . . ? O7 C30 O8 121.0(4) . . ? O7 C30 C17 119.7(4) . . ? O8 C30 C17 119.4(4) . . ? O7 C30 Cd2 63.9(2) . . ? O8 C30 Cd2 58.1(2) . . ? C17 C30 Cd2 168.6(3) . . ? O1 C31 C32 111.5(4) . . ? C33 C32 C31 129.8(6) . . ? C32 C33 C34 124.0(6) . . ? O3 C35 C36 107.6(3) . . ? C35 C36 C37 114.4(4) . . ? C38 C37 C36 113.0(4) . . ? C40 C39 C44 117.1(4) . . ? C40 C39 C66 119.7(4) . . ? C44 C39 C66 123.1(4) . . ? C39 C40 C41 121.8(4) . . ? C42 C41 C40 118.8(4) . . ? C42 C41 C67 121.6(4) . . ? C40 C41 C67 119.6(4) . . ? C43 C42 C41 121.8(4) . . ? C42 C43 C44 118.3(4) . . ? C42 C43 C45 120.2(5) . . ? C44 C43 C45 121.5(4) . . ? O9 C44 C43 118.9(4) . . ? O9 C44 C39 119.1(4) . . ? C43 C44 C39 121.9(4) . . ? C46 C45 C43 112.1(4) . . ? C47 C46 C51 118.3(4) . . ? C47 C46 C45 119.9(4) . . ? C51 C46 C45 121.8(5) . . ? C48 C47 C46 121.5(5) . . ? C49 C48 C47 118.9(5) . . ? C50 C49 C48 121.8(5) . . ? C49 C50 C51 118.4(4) . . ? C49 C50 C52 122.3(4) . . ? C51 C50 C52 119.3(4) . . ? O10 C51 C46 122.1(4) . . ? O10 C51 C50 116.8(4) . . ? C46 C51 C50 121.0(5) . . ? C53 C52 C50 109.8(4) . . ? C54 C53 C58 117.9(4) . . ? C54 C53 C52 119.4(4) . . ? C58 C53 C52 122.6(4) . . ? C53 C54 C55 121.8(4) . . ? C54 C55 C56 119.3(4) . . ? C54 C55 C68 120.9(4) . . ? C56 C55 C68 119.7(4) . . ? C57 C56 C55 120.7(4) . . ? C56 C57 C58 118.5(4) . . ? C56 C57 C59 118.7(4) . . ? C58 C57 C59 122.7(4) . . ? O11 C58 C53 119.3(4) . . ? O11 C58 C57 118.9(4) . . ? C53 C58 C57 121.6(4) . . ? C60 C59 C57 110.0(3) . . ? C61 C60 C65 118.4(4) . . ? C61 C60 C59 121.0(4) . . ? C65 C60 C59 120.6(4) . . ? C62 C61 C60 120.9(4) . . ? C61 C62 C63 119.9(4) . . ? C64 C63 C62 120.9(4) . . ? C63 C64 C65 118.4(4) . . ? C63 C64 C66 121.9(4) . . ? C65 C64 C66 119.6(4) . . ? O12 C65 C60 121.2(4) . . ? O12 C65 C64 117.3(3) . . ? C60 C65 C64 121.4(4) . . ? C39 C66 C64 112.5(3) . . ? O14 C67 O13 121.2(5) . . ? O14 C67 C41 118.8(5) . . ? O13 C67 C41 119.9(5) . . ? O16 C68 O15 122.9(5) . . ? O16 C68 C55 119.8(4) . . ? O15 C68 C55 117.3(5) . . ? C71 C70 C69 110.3(8) . . ? C72 C71 C70 118.6(9) . . ? O11 C73 C74 109.0(5) . . ? C75 C74 C73 112.5(6) . . ? C74 C75 C76 107.2(7) . . ? O17 C77 N00R 126.9(5) . . ? N00H C80 C81 122.5(5) . . ? C82 C81 C80 118.9(5) . . ? C81 C82 C83 120.2(5) . . ? C82 C83 C84 117.5(4) . . ? C82 C83 C85 122.6(4) . . ? C84 C83 C85 119.9(4) . . ? N00H C84 C83 122.3(4) . . ? N00H C84 C88 117.8(4) . . ? C83 C84 C88 119.9(4) . . ? C86 C85 C83 119.9(5) . . ? C85 C86 C87 122.5(4) . . ? C89 C87 C86 124.2(4) . . ? C89 C87 C88 116.3(5) . . ? C86 C87 C88 119.5(4) . . ? N00L C88 C87 123.0(4) . . ? N00L C88 C84 118.8(4) . . ? C87 C88 C84 118.3(4) . . ? C90 C89 C87 120.6(5) . . ? C89 C90 C91 119.3(5) . . ? N00L C91 C90 122.8(5) . . ? N00N C92 C93 122.4(6) . . ? C94 C93 C92 118.7(6) . . ? C93 C94 C95 120.2(5) . . ? C94 C95 C96 117.7(5) . . ? C94 C95 C97 123.5(5) . . ? C96 C95 C97 118.7(6) . . ? N00N C96 C95 121.7(5) . . ? N00N C96 C100 118.5(4) . . ? C95 C96 C100 119.7(5) . . ? C98 C97 C95 122.2(6) . . ? C97 C98 C99 120.5(6) . . ? C101 C99 C100 117.3(5) . . ? C101 C99 C98 123.3(6) . . ? C100 C99 C98 119.4(6) . . ? N00K C100 C99 121.7(5) . . ? N00K C100 C96 119.0(5) . . ? C99 C100 C96 119.2(5) . . ? C102 C101 C99 120.5(6) . . ? C101 C102 C103 118.7(6) . . ? N00K C103 C102 123.5(5) . . ? O19 C104 N00M 123.5(6) . . ? C70A C71A C72A 113.2(10) . . ? O9 C69 C70 103.3(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 31.19 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.034 _refine_diff_density_min -2.911 _refine_diff_density_rms 0.108