Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Rita Delgado' _publ_contact_author_address ; ITQB - Instituto de Tecnologia Quimica e Biologica, UNL Apartado 127 Oeiras 2781-901 PORTUGAL ; _publ_contact_author_email DELGADO@ITQB.UNL.PT loop_ _publ_author_name _publ_author_address V.Felix ;Departamento Quimica, CICECO, Universidade de Aveiro 3810-193 Portugal ; 'Li Feng.' ;Instituto de Tecnologia Quimica e Biologica UNL, Apartado 127 2781-901 Oeiras Portugal ; R.Delgado ;Instituto de Tecnologia Quimica e Biologica UNL, Apartado 127 2781-901 Oeiras Portugal ; M.G.B.Drew ;School of Chemistry University of Reading Whiteknights, Reading UK RG6 6AD ; _publ_section_title ; Dioxadiaza- and trioxadiaza- macrocycles containing one dibenzofuran unit selective for cadmium ; data_compound1 _database_code_depnum_ccdc_archive 'CCDC 614587' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H26 N4 O9' _chemical_formula_weight 466.45 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 20.845(2) _cell_length_b 12.2298(13) _cell_length_c 17.2467(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.285(9) _cell_angle_gamma 90.00 _cell_volume 4378.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 1.0 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'XCalibur-CCD from Oxford Diffraction Ltd' _diffrn_measurement_method '321 frames at 3 s' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14304 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.1240 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 30.15 _reflns_number_total 6364 _reflns_number_gt 3092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction Ltd software' _computing_cell_refinement 'Oxford Diffraction Ltd software' _computing_data_reduction 'Oxford Diffraction Ltd software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2003) _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 w=1/[\s^2^(Fo^2^)+(0.0867P)^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 6364 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1733 _refine_ls_wR_factor_gt 0.1626 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.30538(10) 0.29584(17) 0.10170(11) 0.0211(5) Uani 1 d . . . C12 C 0.33434(11) 0.20934(17) 0.14423(12) 0.0244(5) Uani 1 d . . . C13 C 0.40121(11) 0.2173(2) 0.15867(13) 0.0326(6) Uani 1 d . . . H13 H 0.4238 0.1609 0.1876 0.039 Uiso 1 calc R . . C14 C 0.43622(12) 0.3052(2) 0.13222(14) 0.0356(6) Uani 1 d . . . H14 H 0.4817 0.3072 0.1435 0.043 Uiso 1 calc R . . C15 C 0.40547(11) 0.3890(2) 0.08996(13) 0.0323(6) Uani 1 d . . . H15 H 0.4294 0.4481 0.0715 0.039 Uiso 1 calc R . . C16 C 0.33903(11) 0.38528(18) 0.07495(12) 0.0257(5) Uani 1 d . . . C17 C 0.29013(11) 0.45668(17) 0.03617(11) 0.0242(5) Uani 1 d . . . C18 C 0.28980(12) 0.55942(18) 0.00032(12) 0.0305(6) Uani 1 d . . . H18 H 0.3289 0.5971 -0.0054 0.037 Uiso 1 calc R . . C19 C 0.23164(13) 0.60441(19) -0.02632(13) 0.0351(6) Uani 1 d . . . H19 H 0.2308 0.6740 -0.0509 0.042 Uiso 1 calc R . . C20 C 0.17360(12) 0.55007(18) -0.01806(12) 0.0296(5) Uani 1 d . . . H20 H 0.1343 0.5839 -0.0372 0.036 Uiso 1 calc R . . C21 C 0.17171(11) 0.44764(18) 0.01746(11) 0.0245(5) Uani 1 d . . . C22 C 0.23129(11) 0.40444(16) 0.04347(11) 0.0213(5) Uani 1 d . . . O23 O 0.23963(7) 0.30474(11) 0.08221(7) 0.0204(3) Uani 1 d . . . C24 C 0.10975(11) 0.38878(18) 0.02753(12) 0.0267(5) Uani 1 d . . . H24A H 0.1151 0.3100 0.0166 0.032 Uiso 1 calc R . . H24B H 0.0753 0.4177 -0.0103 0.032 Uiso 1 calc R . . N25 N 0.09021(8) 0.40265(15) 0.10885(9) 0.0241(4) Uani 1 d . . . H25A H 0.1162 0.3592 0.1420 0.029 Uiso 1 calc R . . H25B H 0.0974 0.4741 0.1239 0.029 Uiso 1 calc R . . C26 C 0.02155(11) 0.3748(2) 0.11772(14) 0.0311(5) Uani 1 d . . . H26A H 0.0119 0.3919 0.1715 0.037 Uiso 1 calc R . . H26B H -0.0067 0.4207 0.0818 0.037 Uiso 1 calc R . . C27 C 0.00709(11) 0.2574(2) 0.10112(15) 0.0385(6) Uani 1 d . . . H27A H -0.0377 0.2399 0.1114 0.046 Uiso 1 calc R . . H27B H 0.0127 0.2400 0.0461 0.046 Uiso 1 calc R . . O28 O 0.05200(8) 0.19658(14) 0.15230(10) 0.0429(5) Uani 1 d . . . C29 C 0.04064(13) 0.0847(2) 0.14965(15) 0.0414(7) Uani 1 d . . . H29A H 0.0419 0.0583 0.0956 0.050 Uiso 1 calc R . . H29B H -0.0028 0.0695 0.1659 0.050 Uiso 1 calc R . . C30 C 0.08942(12) 0.0260(2) 0.20141(15) 0.0385(6) Uani 1 d . . . H30A H 0.0938 0.0614 0.2532 0.046 Uiso 1 calc R . . H30B H 0.0752 -0.0504 0.2082 0.046 Uiso 1 calc R . . O31 O 0.15016(9) 0.02605(14) 0.17000(10) 0.0418(5) Uani 1 d . . . C32 C 0.19773(13) -0.03450(19) 0.21465(14) 0.0381(6) Uani 1 d . . . H32A H 0.2273 -0.0673 0.1793 0.046 Uiso 1 calc R . . H32B H 0.1767 -0.0950 0.2408 0.046 Uiso 1 calc R . . C33 C 0.23680(12) 0.03312(18) 0.27566(13) 0.0309(6) Uani 1 d . . . H33A H 0.2088 0.0554 0.3163 0.037 Uiso 1 calc R . . H33B H 0.2721 -0.0124 0.3008 0.037 Uiso 1 calc R . . N34 N 0.26510(9) 0.13378(14) 0.24157(9) 0.0252(4) Uani 1 d . . . H34A H 0.2329 0.1845 0.2313 0.030 Uiso 1 calc R . . H34B H 0.2951 0.1635 0.2781 0.030 Uiso 1 calc R . . C35 C 0.29665(11) 0.11315(18) 0.16831(12) 0.0260(5) Uani 1 d . . . H35A H 0.3258 0.0494 0.1763 0.031 Uiso 1 calc R . . H35B H 0.2631 0.0948 0.1259 0.031 Uiso 1 calc R . . N51 N 0.14456(9) 0.30933(15) 0.28742(10) 0.0256(4) Uani 1 d . . . O52 O 0.17686(7) 0.30576(12) 0.22758(8) 0.0264(4) Uani 1 d . . . O53 O 0.10533(8) 0.38479(13) 0.29303(9) 0.0356(4) Uani 1 d . . . O54 O 0.15394(9) 0.23801(14) 0.33829(9) 0.0425(5) Uani 1 d . . . N41 N 0.09267(11) 0.67936(18) 0.11191(12) 0.0374(5) Uani 1 d . . . O42 O 0.04841(9) 0.63956(16) 0.06730(11) 0.0495(5) Uani 1 d . . . O43 O 0.10684(12) 0.77608(17) 0.11048(14) 0.0685(7) Uani 1 d . . . O44 O 0.12266(9) 0.61481(15) 0.16080(9) 0.0457(5) Uani 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 C11 0.0170(11) 0.0273(12) 0.0191(10) -0.0072(8) 0.0028(8) -0.0011(9) C12 0.0260(12) 0.0258(12) 0.0213(10) -0.0060(9) 0.0021(9) 0.0029(10) C13 0.0266(13) 0.0427(15) 0.0273(12) -0.0089(10) -0.0045(10) 0.0087(11) C14 0.0200(13) 0.0505(17) 0.0360(13) -0.0181(12) 0.0013(10) -0.0031(12) C15 0.0258(13) 0.0398(15) 0.0322(12) -0.0103(10) 0.0078(10) -0.0131(11) C16 0.0272(12) 0.0300(12) 0.0206(10) -0.0071(9) 0.0063(9) -0.0064(10) C17 0.0287(13) 0.0259(12) 0.0186(10) -0.0038(9) 0.0047(9) -0.0064(10) C18 0.0433(16) 0.0252(12) 0.0236(11) -0.0061(9) 0.0065(10) -0.0126(11) C19 0.0591(18) 0.0207(12) 0.0259(12) 0.0004(9) 0.0060(12) -0.0031(12) C20 0.0435(15) 0.0253(12) 0.0196(10) 0.0001(9) 0.0002(10) 0.0083(11) C21 0.0319(13) 0.0242(12) 0.0170(10) -0.0036(8) -0.0003(9) 0.0012(10) C22 0.0301(13) 0.0186(11) 0.0155(9) -0.0006(8) 0.0037(9) -0.0022(9) O23 0.0205(8) 0.0219(8) 0.0190(7) 0.0031(6) 0.0018(6) -0.0004(6) C24 0.0268(13) 0.0294(12) 0.0233(11) -0.0018(9) -0.0016(9) 0.0031(10) N25 0.0225(10) 0.0267(10) 0.0226(9) 0.0005(7) -0.0001(8) 0.0036(8) C26 0.0204(12) 0.0404(14) 0.0326(12) 0.0000(10) 0.0030(10) 0.0028(11) C27 0.0222(13) 0.0464(17) 0.0466(14) 0.0056(12) 0.0019(11) 0.0007(12) O28 0.0351(10) 0.0354(10) 0.0566(11) 0.0051(8) -0.0048(9) -0.0031(8) C29 0.0365(16) 0.0419(16) 0.0457(15) 0.0044(12) 0.0021(12) -0.0166(12) C30 0.0453(16) 0.0279(13) 0.0445(14) 0.0082(11) 0.0159(12) -0.0019(12) O31 0.0421(11) 0.0403(11) 0.0426(10) 0.0159(8) 0.0012(9) -0.0043(9) C32 0.0490(17) 0.0289(14) 0.0354(13) 0.0126(11) -0.0016(12) -0.0018(12) C33 0.0401(15) 0.0279(13) 0.0250(11) 0.0089(9) 0.0051(10) 0.0029(11) N34 0.0327(11) 0.0224(10) 0.0200(9) 0.0023(7) -0.0004(8) 0.0053(8) C35 0.0320(13) 0.0273(12) 0.0188(10) -0.0015(9) 0.0028(9) 0.0056(10) N51 0.0268(11) 0.0271(10) 0.0226(9) -0.0042(8) -0.0001(8) -0.0024(9) O52 0.0254(9) 0.0309(9) 0.0234(8) 0.0017(6) 0.0054(7) 0.0029(7) O53 0.0323(10) 0.0369(10) 0.0385(9) -0.0061(7) 0.0084(8) 0.0085(8) O54 0.0566(13) 0.0452(11) 0.0262(8) 0.0079(8) 0.0073(8) 0.0081(9) N41 0.0367(13) 0.0349(13) 0.0414(12) -0.0095(10) 0.0076(10) 0.0047(11) O42 0.0396(11) 0.0542(12) 0.0507(11) -0.0114(9) -0.0164(9) 0.0122(10) O43 0.0837(17) 0.0337(12) 0.0887(16) -0.0061(11) 0.0114(13) -0.0122(12) O44 0.0566(13) 0.0445(11) 0.0324(9) -0.0044(8) -0.0159(9) 0.0069(9) _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 C11 O23 1.385(2) . ? C11 C12 1.393(3) . ? C11 C16 1.400(3) . ? C12 C13 1.397(3) . ? C12 C35 1.494(3) . ? C13 C14 1.399(3) . ? C14 C15 1.381(3) . ? C15 C16 1.386(3) . ? C16 C17 1.457(3) . ? C17 C22 1.399(3) . ? C17 C18 1.400(3) . ? C18 C19 1.371(3) . ? C19 C20 1.399(3) . ? C20 C21 1.397(3) . ? C21 C22 1.386(3) . ? C21 C24 1.502(3) . ? C22 O23 1.393(2) . ? C24 N25 1.506(3) . ? N25 C26 1.493(3) . ? C26 C27 1.490(3) . ? C27 O28 1.434(3) . ? O28 C29 1.388(3) . ? C29 C30 1.476(3) . ? C30 O31 1.422(3) . ? O31 C32 1.409(3) . ? C32 C33 1.515(3) . ? C33 N34 1.508(3) . ? N34 C35 1.499(3) . ? N51 O54 1.240(2) . ? N51 O53 1.243(2) . ? N51 O52 1.284(2) . ? N41 O43 1.220(3) . ? N41 O42 1.245(3) . ? N41 O44 1.276(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O23 C11 C12 123.96(19) . . ? O23 C11 C16 111.90(18) . . ? C12 C11 C16 124.1(2) . . ? C11 C12 C13 114.7(2) . . ? C11 C12 C35 122.1(2) . . ? C13 C12 C35 123.2(2) . . ? C12 C13 C14 122.5(2) . . ? C15 C14 C13 120.8(2) . . ? C14 C15 C16 118.8(2) . . ? C15 C16 C11 119.1(2) . . ? C15 C16 C17 135.3(2) . . ? C11 C16 C17 105.61(19) . . ? C22 C17 C18 118.7(2) . . ? C22 C17 C16 105.49(18) . . ? C18 C17 C16 135.7(2) . . ? C19 C18 C17 118.4(2) . . ? C18 C19 C20 121.4(2) . . ? C21 C20 C19 122.0(2) . . ? C22 C21 C20 115.0(2) . . ? C22 C21 C24 122.29(19) . . ? C20 C21 C24 122.7(2) . . ? C21 C22 O23 123.86(19) . . ? C21 C22 C17 124.33(19) . . ? O23 C22 C17 111.78(18) . . ? C11 O23 C22 105.19(15) . . ? C21 C24 N25 111.28(17) . . ? C26 N25 C24 114.46(17) . . ? C27 C26 N25 112.26(19) . . ? O28 C27 C26 105.8(2) . . ? C29 O28 C27 113.0(2) . . ? O28 C29 C30 110.7(2) . . ? O31 C30 C29 110.9(2) . . ? C32 O31 C30 113.46(18) . . ? O31 C32 C33 113.5(2) . . ? N34 C33 C32 112.29(17) . . ? C35 N34 C33 114.16(16) . . ? C12 C35 N34 112.61(17) . . ? O54 N51 O53 121.96(19) . . ? O54 N51 O52 118.99(18) . . ? O53 N51 O52 119.05(17) . . ? O43 N41 O42 122.3(2) . . ? O43 N41 O44 120.6(2) . . ? O42 N41 O44 117.2(2) . . ? _diffrn_measured_fraction_theta_max 0.470 _diffrn_reflns_theta_full 30.15 _diffrn_measured_fraction_theta_full 0.470 _refine_diff_density_max 0.844 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.072 #==END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 614588' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H26 Cd N4 O10' _chemical_formula_weight 594.85 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' Cd Cd -0.8075 1.2024 '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 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4122(4) _cell_length_b 17.2444(9) _cell_length_c 15.3981(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.138(5) _cell_angle_gamma 90.00 _cell_volume 2233.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'XCalibur-CCD from Oxford Diffraction Ltd' _diffrn_measurement_method '321 frames at 3 s' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14057 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 30.08 _reflns_number_total 6382 _reflns_number_gt 4696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction Ltd software' _computing_cell_refinement 'Oxford Diffraction Ltd software' _computing_data_reduction 'Oxford Diffraction Ltd software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2003) _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 w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+1.7762P] 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 6382 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd -0.209185(18) -0.002063(11) -0.291390(11) 0.02087(5) Uani 1 d . . . O23 O -0.18781(19) 0.03399(10) -0.12624(11) 0.0223(4) Uani 1 d . . . O28 O -0.1286(2) -0.08816(12) -0.41348(12) 0.0316(4) Uani 1 d . . . O31 O -0.2723(4) 0.04141(14) -0.43846(14) 0.0659(8) Uani 1 d . . . O42 O -0.4599(3) -0.0828(2) -0.34125(16) 0.0739(10) Uani 1 d . . . O43 O -0.4601(2) -0.02306(14) -0.22151(16) 0.0465(6) Uani 1 d . . . O44 O -0.6787(2) -0.07335(13) -0.27124(14) 0.0401(5) Uani 1 d . . . O100 O 0.0543(2) 0.03870(14) -0.29646(15) 0.0316(5) Uani 1 d . . . H101 H 0.126(4) 0.0127(19) -0.285(2) 0.036(9) Uiso 1 d . . . H102 H 0.069(4) 0.082(2) -0.298(2) 0.038(10) Uiso 1 d . . . N25 N -0.1091(2) -0.11674(13) -0.23011(14) 0.0248(4) Uani 1 d . . . H25 H -0.1973 -0.1463 -0.2159 0.030 Uiso 1 calc R . . N34 N -0.2822(3) 0.12888(14) -0.29096(15) 0.0343(5) Uani 1 d . . . H34 H -0.3927 0.1270 -0.2939 0.041 Uiso 1 calc R . . N41 N -0.5354(2) -0.05898(15) -0.27819(15) 0.0305(5) Uani 1 d . . . C11 C -0.3190(3) 0.16021(15) -0.13603(18) 0.0272(5) Uani 1 d . . . C12 C -0.2812(3) 0.09269(14) -0.09198(17) 0.0236(5) Uani 1 d . . . C13 C -0.4142(3) 0.21176(16) -0.0904(2) 0.0324(6) Uani 1 d . . . H13 H -0.4448 0.2593 -0.1170 0.039 Uiso 1 calc R . . C14 C -0.4657(3) 0.19532(18) -0.0066(2) 0.0350(7) Uani 1 d . . . H14 H -0.5313 0.2318 0.0220 0.042 Uiso 1 calc R . . C15 C -0.4238(3) 0.12772(17) 0.03563(19) 0.0314(6) Uani 1 d . . . H15 H -0.4581 0.1176 0.0929 0.038 Uiso 1 calc R . . C16 C -0.3291(3) 0.07444(15) -0.00838(17) 0.0248(5) Uani 1 d . . . C17 C -0.2610(3) -0.00102(16) 0.01160(15) 0.0250(5) Uani 1 d . . . C18 C -0.2593(3) -0.05047(17) 0.08342(17) 0.0306(6) Uani 1 d . . . H18 H -0.3138 -0.0373 0.1348 0.037 Uiso 1 calc R . . C19 C -0.1758(3) -0.11914(18) 0.07715(18) 0.0335(6) Uani 1 d . . . H19 H -0.1717 -0.1534 0.1255 0.040 Uiso 1 calc R . . C20 C -0.0975(3) -0.13938(16) 0.00145(18) 0.0288(6) Uani 1 d . . . H20 H -0.0426 -0.1874 -0.0005 0.035 Uiso 1 calc R . . C21 C -0.0972(3) -0.09161(14) -0.07130(16) 0.0230(5) Uani 1 d . . . C22 C -0.1787(3) -0.02254(15) -0.06207(16) 0.0225(5) Uani 1 d . . . C24 C -0.0094(3) -0.11299(17) -0.15162(17) 0.0298(6) Uani 1 d . . . H24A H 0.0759 -0.0745 -0.1606 0.036 Uiso 1 calc R . . H24B H 0.0418 -0.1641 -0.1424 0.036 Uiso 1 calc R . . C26 C -0.0244(3) -0.16129(15) -0.29716(17) 0.0277(6) Uani 1 d . . . H26A H -0.0039 -0.2145 -0.2756 0.033 Uiso 1 calc R . . H26B H 0.0795 -0.1365 -0.3078 0.033 Uiso 1 calc R . . C27 C -0.1181(4) -0.16536(17) -0.38062(19) 0.0350(6) Uani 1 d . . . H27A H -0.0642 -0.1994 -0.4226 0.042 Uiso 1 calc R . . H27B H -0.2256 -0.1864 -0.3704 0.042 Uiso 1 calc R . . C29 C -0.2224(4) -0.0831(2) -0.49108(18) 0.0397(7) Uani 1 d . . . H29A H -0.3284 -0.1064 -0.4821 0.048 Uiso 1 calc R . . H29B H -0.1702 -0.1114 -0.5386 0.048 Uiso 1 calc R . . C30 C -0.2391(4) 0.0000(2) -0.51364(18) 0.0415(7) Uani 1 d . . . H30A H -0.1394 0.0193 -0.5390 0.050 Uiso 1 calc R . . H30B H -0.3263 0.0069 -0.5571 0.050 Uiso 1 calc R . . C32 C -0.3129(4) 0.12048(18) -0.4488(2) 0.0409(7) Uani 1 d . . . H32A H -0.4299 0.1267 -0.4491 0.049 Uiso 1 calc R . . H32B H -0.2727 0.1401 -0.5047 0.049 Uiso 1 calc R . . C33 C -0.2399(3) 0.16469(17) -0.37534(18) 0.0318(6) Uani 1 d . . . H33A H -0.2780 0.2190 -0.3772 0.038 Uiso 1 calc R . . H33B H -0.1229 0.1652 -0.3809 0.038 Uiso 1 calc R . . C35 C -0.2516(4) 0.17935(17) -0.2212(2) 0.0420(8) Uani 1 d . . . H35A H -0.2911 0.2314 -0.2382 0.050 Uiso 1 calc R . . H35B H -0.1348 0.1835 -0.2134 0.050 Uiso 1 calc R . . O52 O -0.6372(2) 0.12713(14) -0.31231(18) 0.0516(6) Uani 1 d . . . O53 O -0.8542(2) 0.19278(12) -0.31041(16) 0.0408(5) Uani 1 d . . . O54 O -0.6284(2) 0.25297(14) -0.30211(17) 0.0489(6) Uani 1 d . . . N51 N -0.7043(2) 0.19201(15) -0.30855(15) 0.0303(5) Uani 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 Cd 0.01983(8) 0.02483(9) 0.01791(8) -0.00025(9) -0.00050(5) -0.00029(8) O23 0.0232(8) 0.0214(8) 0.0225(9) -0.0003(7) 0.0026(7) 0.0011(7) O28 0.0334(10) 0.0378(11) 0.0234(10) -0.0034(8) -0.0027(8) -0.0026(8) O31 0.138(3) 0.0384(14) 0.0204(11) 0.0010(10) -0.0088(14) 0.0201(15) O42 0.0358(12) 0.155(3) 0.0308(13) -0.0152(16) 0.0064(10) 0.0037(16) O43 0.0277(10) 0.0540(14) 0.0579(15) -0.0185(12) 0.0010(10) -0.0102(9) O44 0.0168(8) 0.0569(14) 0.0467(13) -0.0029(11) 0.0017(8) -0.0086(9) O100 0.0212(9) 0.0323(12) 0.0411(13) 0.0040(10) -0.0016(8) -0.0017(9) N25 0.0243(10) 0.0270(11) 0.0231(11) -0.0022(9) 0.0010(8) 0.0040(8) N34 0.0490(14) 0.0288(12) 0.0249(12) 0.0026(10) -0.0036(11) 0.0037(11) N41 0.0202(10) 0.0448(14) 0.0265(12) 0.0057(11) 0.0017(9) -0.0013(9) C11 0.0269(12) 0.0222(12) 0.0325(15) -0.0039(11) -0.0006(11) -0.0018(10) C12 0.0194(11) 0.0237(12) 0.0276(14) -0.0085(10) -0.0004(9) -0.0011(9) C13 0.0289(13) 0.0242(13) 0.0437(18) -0.0084(12) -0.0064(12) 0.0031(10) C14 0.0257(14) 0.0366(15) 0.0427(18) -0.0174(13) -0.0015(13) 0.0028(11) C15 0.0270(12) 0.0407(16) 0.0264(14) -0.0140(12) -0.0009(10) -0.0014(11) C16 0.0204(11) 0.0297(13) 0.0242(13) -0.0092(11) -0.0036(9) -0.0017(10) C17 0.0228(10) 0.0320(12) 0.0199(11) -0.0042(13) -0.0034(8) -0.0032(12) C18 0.0291(13) 0.0447(16) 0.0179(13) -0.0023(12) -0.0014(10) -0.0036(12) C19 0.0398(15) 0.0403(16) 0.0201(13) 0.0083(12) -0.0063(11) -0.0039(13) C20 0.0300(13) 0.0293(13) 0.0267(14) 0.0038(11) -0.0062(11) 0.0004(11) C21 0.0227(11) 0.0253(12) 0.0210(12) -0.0002(10) -0.0029(9) -0.0020(9) C22 0.0222(11) 0.0254(12) 0.0199(12) -0.0008(9) -0.0020(9) -0.0044(9) C24 0.0317(13) 0.0320(14) 0.0256(14) -0.0004(11) -0.0014(11) 0.0086(11) C26 0.0285(12) 0.0246(13) 0.0301(14) -0.0042(11) 0.0041(11) 0.0009(10) C27 0.0425(16) 0.0321(15) 0.0305(15) -0.0112(13) 0.0015(12) -0.0020(12) C29 0.0405(15) 0.057(2) 0.0211(14) -0.0093(14) -0.0031(12) -0.0005(15) C30 0.0414(15) 0.062(2) 0.0208(12) 0.0016(16) -0.0022(11) 0.0024(17) C32 0.0507(18) 0.0407(17) 0.0308(16) 0.0108(14) -0.0102(14) 0.0009(14) C33 0.0318(14) 0.0336(14) 0.0298(15) 0.0110(12) -0.0064(11) -0.0034(11) C35 0.059(2) 0.0234(14) 0.0435(19) 0.0035(13) 0.0112(15) 0.0004(13) O52 0.0259(10) 0.0501(14) 0.0785(19) -0.0075(13) -0.0049(11) 0.0084(10) O53 0.0184(8) 0.0381(11) 0.0658(16) -0.0083(11) 0.0007(9) 0.0024(8) O54 0.0331(11) 0.0506(14) 0.0631(16) 0.0044(12) -0.0003(10) -0.0146(10) N51 0.0231(10) 0.0435(14) 0.0242(12) -0.0026(10) 0.0000(9) -0.0017(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 Cd O100 2.3284(19) . ? Cd N34 2.340(2) . ? Cd N25 2.341(2) . ? Cd O43 2.415(2) . ? Cd O31 2.434(2) . ? Cd O28 2.4997(19) . ? Cd O23 2.6206(17) . ? Cd O42 2.629(3) . ? O23 C22 1.389(3) . ? O23 C12 1.392(3) . ? O28 C29 1.421(3) . ? O28 C27 1.426(4) . ? O31 C30 1.393(4) . ? O31 C32 1.414(4) . ? O42 N41 1.241(3) . ? O43 N41 1.235(3) . ? O44 N41 1.238(3) . ? O100 H101 0.77(4) . ? O100 H102 0.76(3) . ? N25 C24 1.459(3) . ? N25 C26 1.481(3) . ? N25 H25 0.9300 . ? N34 C35 1.402(4) . ? N34 C33 1.488(3) . ? N34 H34 0.9300 . ? C11 C12 1.381(4) . ? C11 C13 1.396(4) . ? C11 C35 1.477(4) . ? C12 C16 1.393(4) . ? C13 C14 1.399(4) . ? C13 H13 0.9500 . ? C14 C15 1.377(4) . ? C14 H14 0.9500 . ? C15 C16 1.400(3) . ? C15 H15 0.9500 . ? C16 C17 1.452(4) . ? C17 C22 1.391(3) . ? C17 C18 1.396(4) . ? C18 C19 1.381(4) . ? C18 H18 0.9500 . ? C19 C20 1.395(4) . ? C19 H19 0.9500 . ? C20 C21 1.390(4) . ? C20 H20 0.9500 . ? C21 C22 1.383(3) . ? C21 C24 1.499(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 C27 1.496(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C29 C30 1.480(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C32 C33 1.487(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? O52 N51 1.255(3) . ? O53 N51 1.261(3) . ? O54 N51 1.233(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O100 Cd N34 87.65(9) . . ? O100 Cd N25 86.19(8) . . ? N34 Cd N25 155.02(8) . . ? O100 Cd O43 154.31(8) . . ? N34 Cd O43 84.93(8) . . ? N25 Cd O43 90.24(8) . . ? O100 Cd O31 93.79(10) . . ? N34 Cd O31 69.70(8) . . ? N25 Cd O31 134.86(8) . . ? O43 Cd O31 106.51(10) . . ? O100 Cd O28 83.20(7) . . ? N34 Cd O28 130.57(7) . . ? N25 Cd O28 72.58(7) . . ? O43 Cd O28 119.89(7) . . ? O31 Cd O28 62.65(7) . . ? O100 Cd O23 85.06(7) . . ? N34 Cd O23 77.37(7) . . ? N25 Cd O23 78.00(6) . . ? O43 Cd O23 69.33(7) . . ? O31 Cd O23 147.06(7) . . ? O28 Cd O23 148.91(6) . . ? O100 Cd O42 155.34(8) . . ? N34 Cd O42 107.64(10) . . ? N25 Cd O42 87.14(9) . . ? O43 Cd O42 49.29(7) . . ? O31 Cd O42 74.49(10) . . ? O28 Cd O42 72.15(7) . . ? O23 Cd O42 116.63(6) . . ? C22 O23 C12 105.32(19) . . ? C22 O23 Cd 121.71(14) . . ? C12 O23 Cd 120.80(15) . . ? C29 O28 C27 112.6(2) . . ? C29 O28 Cd 116.20(17) . . ? C27 O28 Cd 107.66(15) . . ? C30 O31 C32 116.9(2) . . ? C30 O31 Cd 124.84(19) . . ? C32 O31 Cd 116.74(18) . . ? N41 O42 Cd 90.91(19) . . ? N41 O43 Cd 101.59(16) . . ? Cd O100 H101 124(2) . . ? Cd O100 H102 117(3) . . ? H101 O100 H102 117(3) . . ? C24 N25 C26 108.90(19) . . ? C24 N25 Cd 119.53(17) . . ? C26 N25 Cd 109.36(15) . . ? C24 N25 H25 106.1 . . ? C26 N25 H25 106.1 . . ? Cd N25 H25 106.1 . . ? C35 N34 C33 111.6(2) . . ? C35 N34 Cd 123.84(19) . . ? C33 N34 Cd 109.31(17) . . ? C35 N34 H34 103.2 . . ? C33 N34 H34 103.2 . . ? Cd N34 H34 103.2 . . ? O43 N41 O44 121.8(2) . . ? O43 N41 O42 117.1(2) . . ? O44 N41 O42 121.1(3) . . ? C12 C11 C13 114.7(3) . . ? C12 C11 C35 122.4(2) . . ? C13 C11 C35 122.6(3) . . ? C11 C12 O23 123.6(2) . . ? C11 C12 C16 125.2(2) . . ? O23 C12 C16 111.2(2) . . ? C11 C13 C14 121.8(3) . . ? C11 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C15 C14 C13 121.7(2) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 118.0(3) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? C12 C16 C15 118.5(3) . . ? C12 C16 C17 106.1(2) . . ? C15 C16 C17 135.4(3) . . ? C22 C17 C18 119.1(3) . . ? C22 C17 C16 105.5(2) . . ? C18 C17 C16 135.4(2) . . ? C19 C18 C17 117.7(2) . . ? C19 C18 H18 121.1 . . ? C17 C18 H18 121.1 . . ? C18 C19 C20 121.5(3) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 122.3(3) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C22 C21 C20 114.7(2) . . ? C22 C21 C24 123.4(2) . . ? C20 C21 C24 121.9(2) . . ? C21 C22 O23 123.5(2) . . ? C21 C22 C17 124.7(2) . . ? O23 C22 C17 111.8(2) . . ? N25 C24 C21 114.2(2) . . ? N25 C24 H24A 108.7 . . ? C21 C24 H24A 108.7 . . ? N25 C24 H24B 108.7 . . ? C21 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? N25 C26 C27 111.7(2) . . ? N25 C26 H26A 109.3 . . ? C27 C26 H26A 109.3 . . ? N25 C26 H26B 109.3 . . ? C27 C26 H26B 109.3 . . ? H26A C26 H26B 107.9 . . ? O28 C27 C26 106.8(2) . . ? O28 C27 H27A 110.4 . . ? C26 C27 H27A 110.4 . . ? O28 C27 H27B 110.4 . . ? C26 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? O28 C29 C30 107.8(2) . . ? O28 C29 H29A 110.2 . . ? C30 C29 H29A 110.2 . . ? O28 C29 H29B 110.2 . . ? C30 C29 H29B 110.2 . . ? H29A C29 H29B 108.5 . . ? O31 C30 C29 108.7(2) . . ? O31 C30 H30A 109.9 . . ? C29 C30 H30A 109.9 . . ? O31 C30 H30B 109.9 . . ? C29 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? O31 C32 C33 108.3(2) . . ? O31 C32 H32A 110.0 . . ? C33 C32 H32A 110.0 . . ? O31 C32 H32B 110.0 . . ? C33 C32 H32B 110.0 . . ? H32A C32 H32B 108.4 . . ? C32 C33 N34 110.5(2) . . ? C32 C33 H33A 109.6 . . ? N34 C33 H33A 109.6 . . ? C32 C33 H33B 109.6 . . ? N34 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? N34 C35 C11 118.3(3) . . ? N34 C35 H35A 107.7 . . ? C11 C35 H35A 107.7 . . ? N34 C35 H35B 107.7 . . ? C11 C35 H35B 107.7 . . ? H35A C35 H35B 107.1 . . ? O54 N51 O52 122.1(2) . . ? O54 N51 O53 120.6(2) . . ? O52 N51 O53 117.3(2) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.602 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.072