Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andrew D. Burrows' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_email A.D.BURROWS@BATH.AC.UK _publ_section_title ; Syntheses, structures and properties of cadmium benzenedicarboxylate metal-organic frameworks ; loop_ _publ_author_name 'Andrew D. Burrows' 'Kevin Cassar' 'Richard M. W. Friend' 'Mary F. Mahon' 'Sean P. Rigby' ; T.L.Savarese ; # Attachment 'cassar.cif' data_compound_1_bath84 _database_code_depnum_ccdc_archive 'CCDC 651815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H11 Cd N O5' _chemical_formula_weight 349.61 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 7.4523(9) _cell_length_b 9.7764(12) _cell_length_c 9.8469(12) _cell_angle_alpha 118.255(2) _cell_angle_beta 102.118(2) _cell_angle_gamma 91.358(2) _cell_volume 611.51(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 1.797 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68970 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART 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 8031 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 32.01 _reflns_number_total 4205 _reflns_number_gt 3856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^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 4205 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0965 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Cd1 Cd 0.23786(2) -0.026218(19) 0.484304(18) 0.01245(7) Uani 1 1 d . . . O1 O 0.2321(3) -0.1290(3) 0.6720(3) 0.0229(4) Uani 1 1 d . . . O2 O 0.0696(3) 0.0563(2) 0.6704(2) 0.0164(3) Uani 1 1 d . . . O3 O 0.4793(3) -0.1061(2) 0.3271(2) 0.0203(4) Uani 1 1 d . . . O4 O 0.2409(3) -0.2702(2) 0.2874(3) 0.0239(4) Uani 1 1 d . . . O5 O 0.2530(3) 0.1955(2) 0.4635(3) 0.0208(4) Uani 1 1 d . . . N1 N 0.3268(4) 0.3291(4) 0.3427(4) 0.0305(6) Uani 1 1 d . . . C1 C 0.1265(4) -0.0322(3) 0.7287(3) 0.0166(4) Uani 1 1 d . . . C2 C 0.0630(3) -0.0139(3) 0.8709(3) 0.0152(4) Uani 1 1 d . . . C3 C 0.1037(4) -0.1190(3) 0.9277(3) 0.0183(5) Uani 1 1 d . . . H3 H 0.1740 -0.2003 0.8784 0.022 Uiso 1 1 calc R . . C4 C -0.0405(4) 0.1040(3) 0.9427(3) 0.0183(5) Uani 1 1 d . . . H4 H -0.0686 0.1750 0.9035 0.022 Uiso 1 1 calc R . . C5 C 0.3864(4) -0.2423(3) 0.2543(3) 0.0169(5) Uani 1 1 d . . . C6 C 0.4465(4) -0.3742(3) 0.1217(3) 0.0150(4) Uani 1 1 d . . . C7 C 0.6347(4) -0.3829(3) 0.1277(3) 0.0175(5) Uani 1 1 d . . . H7 H 0.7263 -0.3033 0.2147 0.021 Uiso 1 1 calc R . . C8 C 0.3135(4) -0.4916(3) -0.0059(3) 0.0173(5) Uani 1 1 d . . . H8 H 0.1857 -0.4856 -0.0094 0.021 Uiso 1 1 calc R . . C9 C 0.3418(4) 0.2142(4) 0.3785(4) 0.0207(5) Uani 1 1 d . . . H9 H 0.4250 0.1423 0.3368 0.025 Uiso 1 1 calc R . . C10 C 0.4306(6) 0.3385(6) 0.2372(6) 0.0498(11) Uani 1 1 d . . . H10A H 0.5198 0.2634 0.2183 0.075 Uiso 1 1 calc R . . H10B H 0.4971 0.4449 0.2864 0.075 Uiso 1 1 calc R . . H10C H 0.3450 0.3133 0.1356 0.075 Uiso 1 1 calc R . . C11 C 0.1970(6) 0.4405(5) 0.3975(6) 0.0442(10) Uani 1 1 d . . . H11A H 0.1271 0.4127 0.4569 0.066 Uiso 1 1 calc R . . H11B H 0.1110 0.4372 0.3054 0.066 Uiso 1 1 calc R . . H11C H 0.2657 0.5465 0.4668 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01494(10) 0.01207(10) 0.01113(10) 0.00459(7) 0.00738(6) 0.00357(6) O1 0.0281(11) 0.0278(11) 0.0200(10) 0.0133(9) 0.0156(8) 0.0108(9) O2 0.0168(8) 0.0218(9) 0.0115(8) 0.0081(7) 0.0058(6) 0.0021(7) O3 0.0217(9) 0.0140(8) 0.0159(9) 0.0008(7) 0.0026(7) 0.0061(7) O4 0.0335(11) 0.0175(9) 0.0226(10) 0.0065(8) 0.0185(9) 0.0087(8) O5 0.0243(10) 0.0161(9) 0.0250(10) 0.0114(8) 0.0081(8) 0.0029(7) N1 0.0266(13) 0.0305(14) 0.0466(17) 0.0304(14) 0.0046(12) 0.0034(10) C1 0.0160(10) 0.0215(12) 0.0124(10) 0.0072(9) 0.0069(8) 0.0004(9) C2 0.0144(10) 0.0217(12) 0.0111(10) 0.0083(9) 0.0057(8) 0.0033(8) C3 0.0218(12) 0.0219(12) 0.0154(11) 0.0101(10) 0.0100(9) 0.0076(9) C4 0.0216(12) 0.0216(12) 0.0167(11) 0.0115(10) 0.0092(9) 0.0068(9) C5 0.0244(12) 0.0158(11) 0.0111(10) 0.0058(9) 0.0071(9) 0.0104(9) C6 0.0205(11) 0.0120(10) 0.0121(10) 0.0045(8) 0.0067(8) 0.0039(8) C7 0.0201(12) 0.0137(10) 0.0141(11) 0.0020(9) 0.0070(9) 0.0045(8) C8 0.0195(11) 0.0138(10) 0.0163(11) 0.0040(9) 0.0081(9) 0.0045(9) C9 0.0178(12) 0.0208(12) 0.0273(14) 0.0158(11) 0.0035(10) 0.0028(9) C10 0.047(2) 0.067(3) 0.065(3) 0.055(3) 0.014(2) 0.001(2) C11 0.042(2) 0.0251(16) 0.066(3) 0.0275(19) 0.0010(19) 0.0084(14) _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 O4 2.256(2) . ? Cd1 O5 2.274(2) . ? Cd1 O2 2.2788(19) . ? Cd1 O3 2.349(2) 2_656 ? Cd1 O2 2.3947(19) 2_556 ? Cd1 O1 2.494(2) . ? Cd1 O3 2.517(2) . ? Cd1 C5 2.730(2) . ? Cd1 C1 2.731(2) . ? O1 C1 1.243(3) . ? O2 C1 1.283(3) . ? O2 Cd1 2.3947(19) 2_556 ? O3 C5 1.269(4) . ? O3 Cd1 2.349(2) 2_656 ? O4 C5 1.255(3) . ? O5 C9 1.242(3) . ? N1 C9 1.328(4) . ? N1 C10 1.453(5) . ? N1 C11 1.458(5) . ? C1 C2 1.503(3) . ? C2 C4 1.386(4) . ? C2 C3 1.396(4) . ? C3 C4 1.397(4) 2_557 ? C4 C3 1.397(4) 2_557 ? C5 C6 1.499(3) . ? C6 C8 1.392(4) . ? C6 C7 1.397(4) . ? C7 C8 1.385(3) 2_645 ? C8 C7 1.385(3) 2_645 ? 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 O4 Cd1 O5 125.22(8) . . ? O4 Cd1 O2 129.72(8) . . ? O5 Cd1 O2 96.71(7) . . ? O4 Cd1 O3 116.77(8) . 2_656 ? O5 Cd1 O3 81.20(7) . 2_656 ? O2 Cd1 O3 93.78(7) . 2_656 ? O4 Cd1 O2 84.07(8) . 2_556 ? O5 Cd1 O2 79.34(7) . 2_556 ? O2 Cd1 O2 77.32(7) . 2_556 ? O3 Cd1 O2 157.43(7) 2_656 2_556 ? O4 Cd1 O1 90.53(8) . . ? O5 Cd1 O1 144.16(8) . . ? O2 Cd1 O1 54.87(7) . . ? O3 Cd1 O1 79.75(8) 2_656 . ? O2 Cd1 O1 110.26(7) 2_556 . ? O4 Cd1 O3 54.70(7) . . ? O5 Cd1 O3 86.36(7) . . ? O2 Cd1 O3 168.02(7) . . ? O3 Cd1 O3 75.20(8) 2_656 . ? O2 Cd1 O3 114.65(7) 2_556 . ? O1 Cd1 O3 117.27(7) . . ? O4 Cd1 C5 27.08(8) . . ? O5 Cd1 C5 107.06(8) . . ? O2 Cd1 C5 155.27(8) . . ? O3 Cd1 C5 96.44(8) 2_656 . ? O2 Cd1 C5 100.11(7) 2_556 . ? O1 Cd1 C5 105.03(7) . . ? O3 Cd1 C5 27.62(8) . . ? O4 Cd1 C1 111.70(8) . . ? O5 Cd1 C1 121.45(8) . . ? O2 Cd1 C1 27.85(8) . . ? O3 Cd1 C1 85.45(8) 2_656 . ? O2 Cd1 C1 95.01(7) 2_556 . ? O1 Cd1 C1 27.05(7) . . ? O3 Cd1 C1 143.39(7) . . ? C5 Cd1 C1 131.05(8) . . ? C1 O1 Cd1 87.15(16) . . ? C1 O2 Cd1 96.06(16) . . ? C1 O2 Cd1 125.17(17) . 2_556 ? Cd1 O2 Cd1 102.68(7) . 2_556 ? C5 O3 Cd1 138.41(18) . 2_656 ? C5 O3 Cd1 85.57(16) . . ? Cd1 O3 Cd1 104.80(8) 2_656 . ? C5 O4 Cd1 97.98(17) . . ? C9 O5 Cd1 122.87(18) . . ? C9 N1 C10 119.9(3) . . ? C9 N1 C11 121.3(3) . . ? C10 N1 C11 118.6(3) . . ? O1 C1 O2 121.8(2) . . ? O1 C1 C2 120.6(2) . . ? O2 C1 C2 117.6(2) . . ? O1 C1 Cd1 65.80(14) . . ? O2 C1 Cd1 56.09(13) . . ? C2 C1 Cd1 172.7(2) . . ? C4 C2 C3 119.9(2) . . ? C4 C2 C1 120.3(2) . . ? C3 C2 C1 119.7(2) . . ? C2 C3 C4 119.6(2) . 2_557 ? C2 C4 C3 120.5(2) . 2_557 ? O4 C5 O3 121.7(2) . . ? O4 C5 C6 118.2(2) . . ? O3 C5 C6 120.1(2) . . ? O4 C5 Cd1 54.93(13) . . ? O3 C5 Cd1 66.82(14) . . ? C6 C5 Cd1 173.0(2) . . ? C8 C6 C7 119.8(2) . . ? C8 C6 C5 119.5(2) . . ? C7 C6 C5 120.6(2) . . ? C8 C7 C6 119.4(2) 2_645 . ? C7 C8 C6 120.7(2) 2_645 . ? O5 C9 N1 123.7(3) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 32.01 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.893 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.181 #===END data_compound_2_h06kc4 _database_code_depnum_ccdc_archive 'CCDC 651816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Cd3 N4 O16' _chemical_formula_weight 1121.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 28.1090(4) _cell_length_b 9.1930(1) _cell_length_c 17.8780(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.112(1) _cell_angle_gamma 90.00 _cell_volume 4183.12(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 61182 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 1.585 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29343 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4776 _reflns_number_gt 4421 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+5.6474P] 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 4776 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0463 _refine_ls_wR_factor_gt 0.0450 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.139661(5) 0.322663(14) 0.320972(8) 0.01435(4) Uani 1 1 d . . . Cd2 Cd 0.0000 0.241905(19) 0.2500 0.01442(5) Uani 1 2 d S . . O1 O 0.16245(5) 0.23064(15) 0.45151(8) 0.0208(3) Uani 1 1 d . . . O2 O 0.07745(5) 0.27533(14) 0.38237(8) 0.0196(3) Uani 1 1 d . . . O3 O 0.11265(5) 0.38150(17) 0.18517(8) 0.0272(3) Uani 1 1 d . . . O4 O 0.04715(5) 0.41802(15) 0.22107(8) 0.0225(3) Uani 1 1 d . . . O5 O 0.15606(6) 0.55899(15) 0.36469(9) 0.0275(3) Uani 1 1 d . . . O6 O 0.22050(5) 0.27739(16) 0.32792(9) 0.0250(3) Uani 1 1 d . . . O7 O 0.11712(5) -0.09067(15) 0.77062(8) 0.0227(3) Uani 1 1 d . . . O8 O 0.03069(5) -0.08330(16) 0.68787(9) 0.0253(3) Uani 1 1 d . . . N1 N 0.12269(7) 0.77220(18) 0.38602(12) 0.0274(4) Uani 1 1 d . . . N2 N 0.27870(7) 0.0923(2) 0.35352(12) 0.0305(4) Uani 1 1 d . . . C1 C 0.11603(7) 0.2264(2) 0.44545(11) 0.0168(4) Uani 1 1 d . . . C2 C 0.10692(7) 0.16041(19) 0.51491(11) 0.0164(4) Uani 1 1 d . . . C3 C 0.14786(7) 0.0924(2) 0.58036(12) 0.0218(4) Uani 1 1 d . . . H3 H 0.1821 0.0917 0.5822 0.026 Uiso 1 1 calc R . . C4 C 0.13892(8) 0.0254(2) 0.64294(12) 0.0225(4) Uani 1 1 d . . . H4 H 0.1670 -0.0206 0.6875 0.027 Uiso 1 1 calc R . . C5 C 0.08853(7) 0.0259(2) 0.64022(11) 0.0177(4) Uani 1 1 d . . . C6 C 0.04797(7) 0.0952(2) 0.57554(12) 0.0219(4) Uani 1 1 d . . . H6 H 0.0138 0.0970 0.5739 0.026 Uiso 1 1 calc R . . C7 C 0.05706(8) 0.1622(2) 0.51298(12) 0.0212(4) Uani 1 1 d . . . H7 H 0.0291 0.2093 0.4688 0.025 Uiso 1 1 calc R . . C8 C 0.06591(7) 0.4162(2) 0.16741(12) 0.0206(4) Uani 1 1 d . . . C9 C 0.03168(7) 0.4589(2) 0.08071(11) 0.0176(4) Uani 1 1 d . . . C10 C -0.01460(7) 0.5356(2) 0.06292(12) 0.0201(4) Uani 1 1 d . . . H10 H -0.0246 0.5594 0.1060 0.024 Uiso 1 1 calc R . . C11 C 0.04603(7) 0.4228(2) 0.01732(12) 0.0200(4) Uani 1 1 d . . . H11 H 0.0774 0.3696 0.0293 0.024 Uiso 1 1 calc R . . C12 C 0.11847(8) 0.6384(2) 0.35702(13) 0.0247(4) Uani 1 1 d . . . H12 H 0.0841 0.5999 0.3281 0.030 Uiso 1 1 calc R . . C13 C 0.17384(10) 0.8401(3) 0.4290(2) 0.0491(7) Uani 1 1 d . . . H13A H 0.1817 0.8507 0.4877 0.074 Uiso 1 1 calc R . . H13B H 0.1736 0.9362 0.4051 0.074 Uiso 1 1 calc R . . H13C H 0.2007 0.7792 0.4233 0.074 Uiso 1 1 calc R . . C14 C 0.07670(9) 0.8572(2) 0.37726(15) 0.0328(5) Uani 1 1 d . . . H14A H 0.0447 0.8038 0.3427 0.049 Uiso 1 1 calc R . . H14B H 0.0771 0.9508 0.3513 0.049 Uiso 1 1 calc R . . H14C H 0.0775 0.8740 0.4319 0.049 Uiso 1 1 calc R . . C15 C 0.24593(7) 0.1737(2) 0.37087(13) 0.0236(4) Uani 1 1 d . . . H15 H 0.2415 0.1514 0.4194 0.028 Uiso 1 1 calc R . . C16 C 0.30995(11) -0.0201(3) 0.41059(19) 0.0522(7) Uani 1 1 d . . . H16A H 0.2996 -0.0282 0.4563 0.078 Uiso 1 1 calc R . . H16B H 0.3473 0.0056 0.4324 0.078 Uiso 1 1 calc R . . H16C H 0.3041 -0.1134 0.3815 0.078 Uiso 1 1 calc R . . C17 C 0.28742(10) 0.1175(3) 0.27979(16) 0.0427(6) Uani 1 1 d . . . H17A H 0.2635 0.1936 0.2462 0.064 Uiso 1 1 calc R . . H17B H 0.2808 0.0274 0.2476 0.064 Uiso 1 1 calc R . . H17C H 0.3238 0.1483 0.2960 0.064 Uiso 1 1 calc R . . C18 C 0.07836(8) -0.0558(2) 0.70521(12) 0.0191(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01480(7) 0.01654(7) 0.01272(7) 0.00106(5) 0.00683(6) 0.00073(5) Cd2 0.01485(9) 0.01640(9) 0.01496(10) 0.000 0.00917(8) 0.000 O1 0.0203(7) 0.0275(7) 0.0170(7) 0.0021(6) 0.0101(6) -0.0024(6) O2 0.0226(7) 0.0227(7) 0.0152(7) 0.0040(5) 0.0097(6) 0.0032(5) O3 0.0203(7) 0.0370(8) 0.0206(7) 0.0088(6) 0.0049(6) 0.0003(6) O4 0.0281(7) 0.0248(7) 0.0144(6) 0.0024(5) 0.0090(6) -0.0078(6) O5 0.0272(7) 0.0199(7) 0.0374(9) -0.0023(6) 0.0157(7) 0.0000(6) O6 0.0181(7) 0.0293(8) 0.0301(8) 0.0049(6) 0.0126(6) 0.0044(6) O7 0.0286(7) 0.0217(7) 0.0174(7) 0.0050(6) 0.0095(6) 0.0011(6) O8 0.0255(7) 0.0293(8) 0.0262(8) 0.0082(6) 0.0158(6) -0.0004(6) N1 0.0305(9) 0.0180(8) 0.0356(11) -0.0019(7) 0.0157(8) -0.0002(7) N2 0.0252(9) 0.0319(10) 0.0349(10) -0.0014(8) 0.0133(8) 0.0078(8) C1 0.0214(9) 0.0155(8) 0.0149(9) -0.0019(7) 0.0091(8) -0.0008(7) C2 0.0203(9) 0.0161(8) 0.0143(9) -0.0010(7) 0.0089(8) -0.0016(7) C3 0.0170(9) 0.0291(10) 0.0200(10) 0.0034(8) 0.0087(8) -0.0022(8) C4 0.0196(9) 0.0292(10) 0.0168(10) 0.0070(8) 0.0059(8) -0.0004(8) C5 0.0228(9) 0.0170(9) 0.0159(9) 0.0018(7) 0.0107(8) 0.0000(7) C6 0.0200(9) 0.0276(10) 0.0228(10) 0.0057(8) 0.0136(8) 0.0052(8) C7 0.0238(10) 0.0234(10) 0.0192(10) 0.0085(8) 0.0118(8) 0.0085(8) C8 0.0227(9) 0.0188(9) 0.0183(9) 0.0025(7) 0.0070(8) -0.0052(8) C9 0.0168(8) 0.0196(9) 0.0149(9) 0.0033(7) 0.0055(7) -0.0050(7) C10 0.0212(9) 0.0253(10) 0.0162(9) 0.0000(8) 0.0101(8) -0.0032(8) C11 0.0165(9) 0.0243(10) 0.0189(9) 0.0022(8) 0.0073(8) -0.0002(7) C12 0.0282(10) 0.0222(10) 0.0285(11) -0.0032(8) 0.0169(9) -0.0034(8) C13 0.0363(13) 0.0260(12) 0.069(2) -0.0126(12) 0.0072(13) -0.0041(10) C14 0.0389(12) 0.0228(10) 0.0449(14) 0.0002(10) 0.0257(11) 0.0043(9) C15 0.0162(9) 0.0261(10) 0.0280(11) -0.0028(8) 0.0090(8) -0.0018(8) C16 0.0511(16) 0.0456(16) 0.0577(18) 0.0086(13) 0.0210(14) 0.0262(13) C17 0.0429(14) 0.0507(15) 0.0435(15) -0.0076(12) 0.0270(12) 0.0084(12) C18 0.0270(10) 0.0163(9) 0.0186(10) 0.0014(7) 0.0141(8) 0.0012(7) _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 O6 2.2611(13) . ? Cd1 O3 2.2801(14) . ? Cd1 O5 2.2886(14) . ? Cd1 O7 2.2970(13) 6 ? Cd1 O1 2.3030(13) . ? Cd1 O2 2.4661(13) . ? Cd1 O4 2.6035(14) . ? Cd2 O8 2.2175(13) 5_556 ? Cd2 O8 2.2175(13) 6 ? Cd2 O4 2.2863(13) . ? Cd2 O4 2.2863(13) 2 ? Cd2 O2 2.4620(13) . ? Cd2 O2 2.4620(13) 2 ? O1 C1 1.263(2) . ? O2 C1 1.270(2) . ? O3 C8 1.255(2) . ? O4 C8 1.276(2) . ? O5 C12 1.243(2) . ? O6 C15 1.242(2) . ? O7 C18 1.255(2) . ? O7 Cd1 2.2970(13) 6_556 ? O8 C18 1.266(2) . ? O8 Cd2 2.2175(13) 5_556 ? N1 C12 1.321(3) . ? N1 C13 1.452(3) . ? N1 C14 1.461(3) . ? N2 C15 1.322(3) . ? N2 C16 1.456(3) . ? N2 C17 1.458(3) . ? C1 C2 1.499(3) . ? C2 C7 1.387(3) . ? C2 C3 1.393(3) . ? C3 C4 1.390(3) . ? C4 C5 1.396(3) . ? C5 C6 1.387(3) . ? C5 C18 1.509(2) . ? C6 C7 1.392(3) . ? C8 C9 1.489(3) . ? C9 C10 1.392(3) . ? C9 C11 1.395(3) . ? C10 C11 1.382(3) 5_565 ? C11 C10 1.382(3) 5_565 ? 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 O6 Cd1 O3 88.57(5) . . ? O6 Cd1 O5 95.96(5) . . ? O3 Cd1 O5 93.80(6) . . ? O6 Cd1 O7 87.38(5) . 6 ? O3 Cd1 O7 83.75(5) . 6 ? O5 Cd1 O7 175.82(5) . 6 ? O6 Cd1 O1 92.06(5) . . ? O3 Cd1 O1 171.85(5) . . ? O5 Cd1 O1 94.22(5) . . ? O7 Cd1 O1 88.16(5) 6 . ? O6 Cd1 O2 146.00(5) . . ? O3 Cd1 O2 122.49(5) . . ? O5 Cd1 O2 95.37(5) . . ? O7 Cd1 O2 83.15(5) 6 . ? O1 Cd1 O2 55.17(5) . . ? O6 Cd1 O4 141.96(5) . . ? O3 Cd1 O4 53.51(4) . . ? O5 Cd1 O4 84.98(5) . . ? O7 Cd1 O4 90.84(5) 6 . ? O1 Cd1 O4 125.88(4) . . ? O2 Cd1 O4 70.99(4) . . ? O8 Cd2 O8 97.78(8) 5_556 6 ? O8 Cd2 O4 164.81(5) 5_556 . ? O8 Cd2 O4 88.06(5) 6 . ? O8 Cd2 O4 88.06(5) 5_556 2 ? O8 Cd2 O4 164.81(5) 6 2 ? O4 Cd2 O4 89.83(7) . 2 ? O8 Cd2 O2 88.50(5) 5_556 . ? O8 Cd2 O2 100.97(5) 6 . ? O4 Cd2 O2 76.59(4) . . ? O4 Cd2 O2 93.16(5) 2 . ? O8 Cd2 O2 100.97(5) 5_556 2 ? O8 Cd2 O2 88.50(5) 6 2 ? O4 Cd2 O2 93.16(5) . 2 ? O4 Cd2 O2 76.59(4) 2 2 ? O2 Cd2 O2 165.66(6) . 2 ? C1 O1 Cd1 95.24(11) . . ? C1 O2 Cd2 152.03(12) . . ? C1 O2 Cd1 87.59(11) . . ? Cd2 O2 Cd1 95.68(4) . . ? C8 O3 Cd1 99.76(12) . . ? C8 O4 Cd2 128.68(12) . . ? C8 O4 Cd1 84.28(11) . . ? Cd2 O4 Cd1 96.46(5) . . ? C12 O5 Cd1 118.76(13) . . ? C15 O6 Cd1 118.45(13) . . ? C18 O7 Cd1 126.03(12) . 6_556 ? C18 O8 Cd2 127.22(12) . 5_556 ? C12 N1 C13 120.79(19) . . ? C12 N1 C14 121.87(19) . . ? C13 N1 C14 117.33(18) . . ? C15 N2 C16 120.7(2) . . ? C15 N2 C17 121.58(19) . . ? C16 N2 C17 117.59(19) . . ? O1 C1 O2 121.83(17) . . ? O1 C1 C2 118.34(17) . . ? O2 C1 C2 119.83(16) . . ? C7 C2 C3 119.46(17) . . ? C7 C2 C1 120.04(17) . . ? C3 C2 C1 120.47(17) . . ? C4 C3 C2 120.51(17) . . ? C3 C4 C5 119.85(18) . . ? C6 C5 C4 119.54(17) . . ? C6 C5 C18 120.88(17) . . ? C4 C5 C18 119.50(17) . . ? C5 C6 C7 120.46(17) . . ? C2 C7 C6 120.17(18) . . ? O3 C8 O4 122.37(18) . . ? O3 C8 C9 118.36(17) . . ? O4 C8 C9 119.25(17) . . ? C10 C9 C11 119.96(17) . . ? C10 C9 C8 119.97(17) . . ? C11 C9 C8 120.07(17) . . ? C11 C10 C9 120.07(17) 5_565 . ? C10 C11 C9 119.97(18) 5_565 . ? O5 C12 N1 125.0(2) . . ? O6 C15 N2 124.4(2) . . ? O7 C18 O8 125.95(17) . . ? O7 C18 C5 118.11(17) . . ? O8 C18 C5 115.94(17) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.679 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.082 #===END data_compound_3_h04adb1 _database_code_depnum_ccdc_archive 'CCDC 651817' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Cd3 N4 O16' _chemical_formula_weight 1121.92 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' 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' N N 0.0061 0.0033 '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 10.1270(1) _cell_length_b 12.6120(1) _cell_length_c 16.6790(2) _cell_angle_alpha 75.459(1) _cell_angle_beta 88.924(1) _cell_angle_gamma 87.271(1) _cell_volume 2059.65(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35550 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.999 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.610 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.871 _exptl_absorpt_process_details ? _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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46686 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 31.00 _reflns_number_total 12980 _reflns_number_gt 11342 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo & Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+1.0234P] 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 SHELXL _refine_ls_extinction_coef 0.0034(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12980 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.060110(11) -0.218617(10) -0.102688(7) 0.01412(4) Uani 1 1 d . . . Cd2 Cd 0.0000 0.0000 0.0000 0.01277(4) Uani 1 2 d S . . Cd3 Cd 0.591850(11) -0.721051(10) 0.400527(7) 0.01347(4) Uani 1 1 d . . . Cd4 Cd 0.5000 -0.5000 0.5000 0.01286(4) Uani 1 2 d S . . O1 O 0.14845(13) -0.13934(11) 0.00971(9) 0.0230(3) Uani 1 1 d . . . O2 O 0.10229(14) -0.29714(11) -0.01955(9) 0.0243(3) Uani 1 1 d . . . O3 O 0.48774(14) -0.58606(11) 0.30941(8) 0.0239(3) Uani 1 1 d . . . O4 O 0.47091(16) -0.44126(12) 0.36444(9) 0.0282(3) Uani 1 1 d . . . O5 O 0.04950(15) -0.08772(11) -0.18960(9) 0.0258(3) Uani 1 1 d . . . O6 O 0.02794(15) 0.05982(11) -0.13755(8) 0.0251(3) Uani 1 1 d . . . O7 O 0.44793(13) 0.19768(11) -0.50565(9) 0.0231(3) Uani 1 1 d . . . O8 O 0.36654(13) 0.35709(11) -0.48496(8) 0.0216(3) Uani 1 1 d . . . O9 O -0.27443(13) -0.13409(12) -0.12321(8) 0.0224(3) Uani 1 1 d . . . O10 O -0.16262(12) -0.11599(10) -0.01564(8) 0.0183(2) Uani 1 1 d . . . O11 O -0.06441(16) -0.29206(12) -0.21228(9) 0.0283(3) Uani 1 1 d . . . O12 O -0.17036(16) -0.37287(13) -0.01954(9) 0.0317(3) Uani 1 1 d . . . O13 O 0.79840(12) -0.63506(11) 0.37680(8) 0.0212(3) Uani 1 1 d . . . O14 O 0.67807(12) -0.61682(10) 0.48486(8) 0.0181(2) Uani 1 1 d . . . O15 O 0.72666(14) -0.87079(12) 0.47264(9) 0.0261(3) Uani 1 1 d . . . O16 O 0.55569(15) -0.81017(11) 0.30076(9) 0.0253(3) Uani 1 1 d . . . N1 N -0.09859(16) -0.23648(15) -0.35010(10) 0.0257(4) Uani 1 1 d . . . N2 N -0.16482(19) -0.40326(15) 0.12080(11) 0.0289(4) Uani 1 1 d . . . N3 N 0.57713(16) -0.71282(15) 0.16646(10) 0.0240(3) Uani 1 1 d . . . N4 N 0.73207(19) -0.92438(15) 0.61289(11) 0.0308(4) Uani 1 1 d . . . C1 C 0.15699(17) -0.24134(15) 0.02288(11) 0.0184(3) Uani 1 1 d . . . C2 C 0.23855(17) -0.30470(15) 0.09522(11) 0.0185(3) Uani 1 1 d . . . C3 C 0.2855(2) -0.25176(16) 0.15184(13) 0.0276(4) Uani 1 1 d . . . H3 H 0.2698 -0.1749 0.1435 0.033 Uiso 1 1 calc R . . C4 C 0.3557(2) -0.31113(16) 0.22083(13) 0.0279(4) Uani 1 1 d . . . H4 H 0.3860 -0.2750 0.2601 0.033 Uiso 1 1 calc R . . C5 C 0.38141(18) -0.42330(15) 0.23235(11) 0.0181(3) Uani 1 1 d . . . C6 C 0.33748(19) -0.47532(15) 0.17432(12) 0.0212(4) Uani 1 1 d . . . H6 H 0.3571 -0.5515 0.1812 0.025 Uiso 1 1 calc R . . C7 C 0.26505(19) -0.41684(16) 0.10617(12) 0.0215(4) Uani 1 1 d . . . H7 H 0.2338 -0.4532 0.0672 0.026 Uiso 1 1 calc R . . C8 C 0.45330(17) -0.48881(15) 0.30847(11) 0.0175(3) Uani 1 1 d . . . C9 C 0.06899(17) 0.01029(15) -0.19013(11) 0.0180(3) Uani 1 1 d . . . C10 C 0.14860(18) 0.07415(15) -0.26198(11) 0.0178(3) Uani 1 1 d . . . C11 C 0.1428(2) 0.18811(16) -0.28249(13) 0.0253(4) Uani 1 1 d . . . H11 H 0.0884 0.2262 -0.2509 0.030 Uiso 1 1 calc R . . C12 C 0.2161(2) 0.24695(16) -0.34906(13) 0.0254(4) Uani 1 1 d . . . H12 H 0.2109 0.3248 -0.3630 0.030 Uiso 1 1 calc R . . C13 C 0.29693(17) 0.19177(14) -0.39511(11) 0.0176(3) Uani 1 1 d . . . C14 C 0.3031(2) 0.07763(15) -0.37418(12) 0.0230(4) Uani 1 1 d . . . H14 H 0.3587 0.0394 -0.4051 0.028 Uiso 1 1 calc R . . C15 C 0.2285(2) 0.01907(16) -0.30850(12) 0.0232(4) Uani 1 1 d . . . H15 H 0.2322 -0.0588 -0.2954 0.028 Uiso 1 1 calc R . . C16 C 0.37694(17) 0.25457(15) -0.46688(11) 0.0179(3) Uani 1 1 d . . . C17 C -0.26808(17) -0.10106(15) -0.05874(11) 0.0178(3) Uani 1 1 d . . . C18 C -0.38729(17) -0.04747(15) -0.02842(12) 0.0182(3) Uani 1 1 d . . . C19 C -0.50089(18) -0.02294(16) -0.07727(12) 0.0217(4) Uani 1 1 d . . . H19 H -0.5013 -0.0387 -0.1300 0.026 Uiso 1 1 calc R . . C20 C -0.38689(18) -0.02447(16) 0.04878(12) 0.0214(4) Uani 1 1 d . . . H20 H -0.3099 -0.0412 0.0821 0.026 Uiso 1 1 calc R . . C21 C -0.0294(2) -0.24258(16) -0.28367(12) 0.0229(4) Uani 1 1 d . . . H21 H 0.0524 -0.2074 -0.2899 0.028 Uiso 1 1 calc R . . C22 C -0.0532(2) -0.1791(2) -0.43180(14) 0.0356(5) Uani 1 1 d . . . H22A H -0.1142 -0.1165 -0.4545 0.053 Uiso 1 1 calc R . . H22B H -0.0503 -0.2292 -0.4683 0.053 Uiso 1 1 calc R . . H22C H 0.0354 -0.1530 -0.4278 0.053 Uiso 1 1 calc R . . C23 C -0.2254(2) -0.2876(3) -0.34474(16) 0.0420(6) Uani 1 1 d . . . H23A H -0.2433 -0.3259 -0.2871 0.063 Uiso 1 1 calc R . . H23B H -0.2229 -0.3402 -0.3792 0.063 Uiso 1 1 calc R . . H23C H -0.2954 -0.2311 -0.3643 0.063 Uiso 1 1 calc R . . C24 C -0.1219(2) -0.41789(16) 0.04905(13) 0.0275(4) Uani 1 1 d . . . H24 H -0.0476 -0.4671 0.0499 0.033 Uiso 1 1 calc R . . C25 C -0.2765(3) -0.3285(3) 0.12547(18) 0.0524(7) Uani 1 1 d . . . H25A H -0.2443 -0.2577 0.1289 0.079 Uiso 1 1 calc R . . H25B H -0.3297 -0.3592 0.1748 0.079 Uiso 1 1 calc R . . H25C H -0.3309 -0.3181 0.0759 0.079 Uiso 1 1 calc R . . C26 C -0.0927(3) -0.4534(2) 0.19712(14) 0.0387(5) Uani 1 1 d . . . H26A H -0.0286 -0.5094 0.1871 0.058 Uiso 1 1 calc R . . H26B H -0.1552 -0.4874 0.2405 0.058 Uiso 1 1 calc R . . H26C H -0.0462 -0.3969 0.2149 0.058 Uiso 1 1 calc R . . C27 C 0.78403(17) -0.60209(14) 0.44114(11) 0.0166(3) Uani 1 1 d . . . C28 C 0.89530(16) -0.54801(14) 0.47142(11) 0.0173(3) Uani 1 1 d . . . C29 C 1.00721(18) -0.52083(16) 0.42203(12) 0.0204(4) Uani 1 1 d . . . H29 H 1.0121 -0.5351 0.3687 0.024 Uiso 1 1 calc R . . C30 C 0.88822(18) -0.52704(16) 0.54961(12) 0.0204(4) Uani 1 1 d . . . H30 H 0.8120 -0.5454 0.5835 0.024 Uiso 1 1 calc R . . C31 C 0.6887(2) -0.92833(17) 0.53983(13) 0.0264(4) Uani 1 1 d . . . H31 H 0.6232 -0.9793 0.5386 0.032 Uiso 1 1 calc R . . C32 C 0.8302(3) -0.8469(3) 0.62045(18) 0.0551(8) Uani 1 1 d . . . H32A H 0.9114 -0.8871 0.6440 0.083 Uiso 1 1 calc R . . H32B H 0.7958 -0.8017 0.6568 0.083 Uiso 1 1 calc R . . H32C H 0.8494 -0.7997 0.5656 0.083 Uiso 1 1 calc R . . C33 C 0.6811(3) -0.9940(3) 0.68927(17) 0.0550(8) Uani 1 1 d . . . H33A H 0.6190 -1.0443 0.6760 0.083 Uiso 1 1 calc R . . H33B H 0.6355 -0.9483 0.7217 0.083 Uiso 1 1 calc R . . H33C H 0.7546 -1.0363 0.7215 0.083 Uiso 1 1 calc R . . C34 C 0.5156(2) -0.77748(16) 0.22820(12) 0.0227(4) Uani 1 1 d . . . H34 H 0.4323 -0.8018 0.2165 0.027 Uiso 1 1 calc R . . C35 C 0.7029(3) -0.6689(3) 0.17920(17) 0.0517(8) Uani 1 1 d . . . H35A H 0.6930 -0.5889 0.1683 0.078 Uiso 1 1 calc R . . H35B H 0.7693 -0.6886 0.1413 0.078 Uiso 1 1 calc R . . H35C H 0.7312 -0.6996 0.2365 0.078 Uiso 1 1 calc R . . C36 C 0.5204(2) -0.6801(2) 0.08376(13) 0.0346(5) Uani 1 1 d . . . H36A H 0.4321 -0.7089 0.0851 0.052 Uiso 1 1 calc R . . H36B H 0.5771 -0.7093 0.0454 0.052 Uiso 1 1 calc R . . H36C H 0.5140 -0.5999 0.0652 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01449(6) 0.01492(6) 0.01196(6) -0.00156(4) -0.00071(4) -0.00018(4) Cd2 0.01343(8) 0.01301(8) 0.01142(8) -0.00231(6) 0.00027(6) -0.00018(6) Cd3 0.01325(6) 0.01438(6) 0.01188(6) -0.00137(4) -0.00105(4) -0.00148(4) Cd4 0.01419(8) 0.01308(8) 0.01096(8) -0.00209(6) -0.00124(6) -0.00156(6) O1 0.0211(6) 0.0188(6) 0.0250(7) 0.0010(5) -0.0020(5) 0.0061(5) O2 0.0260(7) 0.0235(7) 0.0217(7) -0.0027(5) -0.0102(5) 0.0042(5) O3 0.0285(7) 0.0225(7) 0.0188(7) -0.0024(5) -0.0079(5) 0.0071(5) O4 0.0465(9) 0.0220(7) 0.0149(6) -0.0021(5) -0.0093(6) -0.0009(6) O5 0.0350(8) 0.0223(7) 0.0201(7) -0.0042(5) 0.0089(6) -0.0107(6) O6 0.0351(8) 0.0237(7) 0.0143(6) -0.0013(5) 0.0071(5) 0.0006(6) O7 0.0216(6) 0.0241(7) 0.0214(7) -0.0015(5) 0.0078(5) -0.0034(5) O8 0.0218(6) 0.0176(6) 0.0228(7) 0.0012(5) -0.0007(5) -0.0079(5) O9 0.0189(6) 0.0296(7) 0.0201(7) -0.0096(6) -0.0008(5) 0.0021(5) O10 0.0130(6) 0.0196(6) 0.0229(7) -0.0064(5) -0.0005(5) -0.0013(4) O11 0.0425(9) 0.0262(7) 0.0183(7) -0.0082(6) -0.0001(6) -0.0080(6) O12 0.0429(9) 0.0296(8) 0.0210(7) -0.0006(6) -0.0005(6) -0.0168(7) O13 0.0181(6) 0.0269(7) 0.0199(7) -0.0072(5) -0.0004(5) -0.0058(5) O14 0.0123(6) 0.0196(6) 0.0227(7) -0.0059(5) -0.0013(5) -0.0011(4) O15 0.0266(7) 0.0251(7) 0.0223(7) 0.0005(6) -0.0011(5) 0.0067(5) O16 0.0372(8) 0.0210(7) 0.0186(7) -0.0070(5) -0.0054(6) 0.0022(6) N1 0.0178(8) 0.0398(10) 0.0194(8) -0.0077(7) 0.0003(6) 0.0005(7) N2 0.0412(10) 0.0239(9) 0.0192(8) -0.0010(7) 0.0023(7) -0.0014(7) N3 0.0222(8) 0.0315(9) 0.0194(8) -0.0079(7) 0.0013(6) -0.0044(6) N4 0.0380(10) 0.0277(9) 0.0220(9) 0.0033(7) -0.0034(7) -0.0045(7) C1 0.0148(8) 0.0211(9) 0.0168(8) -0.0010(7) 0.0013(6) 0.0029(6) C2 0.0185(8) 0.0190(8) 0.0162(8) -0.0015(6) -0.0021(6) 0.0029(6) C3 0.0429(12) 0.0162(9) 0.0227(10) -0.0033(7) -0.0113(8) 0.0058(8) C4 0.0425(12) 0.0200(9) 0.0216(10) -0.0065(7) -0.0125(8) 0.0047(8) C5 0.0203(8) 0.0192(8) 0.0131(8) -0.0015(6) -0.0030(6) 0.0020(6) C6 0.0276(9) 0.0155(8) 0.0189(9) -0.0021(7) -0.0072(7) 0.0054(7) C7 0.0274(9) 0.0197(9) 0.0173(9) -0.0046(7) -0.0083(7) 0.0034(7) C8 0.0168(8) 0.0203(8) 0.0134(8) -0.0006(6) -0.0009(6) -0.0006(6) C9 0.0188(8) 0.0210(9) 0.0122(8) -0.0001(6) -0.0003(6) -0.0016(6) C10 0.0207(8) 0.0181(8) 0.0135(8) -0.0018(6) 0.0018(6) -0.0037(6) C11 0.0331(10) 0.0192(9) 0.0246(10) -0.0079(7) 0.0116(8) -0.0035(7) C12 0.0329(10) 0.0157(9) 0.0263(10) -0.0034(7) 0.0099(8) -0.0041(7) C13 0.0194(8) 0.0167(8) 0.0157(8) -0.0018(6) 0.0006(6) -0.0037(6) C14 0.0278(10) 0.0176(9) 0.0231(9) -0.0046(7) 0.0110(7) -0.0023(7) C15 0.0297(10) 0.0158(8) 0.0225(9) -0.0024(7) 0.0085(7) -0.0025(7) C16 0.0158(8) 0.0213(9) 0.0156(8) -0.0015(7) -0.0012(6) -0.0056(6) C17 0.0145(8) 0.0172(8) 0.0202(9) -0.0020(7) 0.0003(6) -0.0014(6) C18 0.0128(8) 0.0211(9) 0.0210(9) -0.0059(7) 0.0013(6) -0.0005(6) C19 0.0172(8) 0.0284(10) 0.0206(9) -0.0087(7) -0.0007(7) 0.0012(7) C20 0.0149(8) 0.0279(10) 0.0222(9) -0.0081(7) -0.0027(7) 0.0016(7) C21 0.0247(9) 0.0246(9) 0.0209(9) -0.0079(7) -0.0017(7) -0.0022(7) C22 0.0345(12) 0.0475(14) 0.0206(10) -0.0024(9) 0.0015(9) 0.0068(10) C23 0.0225(11) 0.0718(19) 0.0341(13) -0.0159(12) -0.0032(9) -0.0099(11) C24 0.0377(11) 0.0194(9) 0.0242(10) -0.0018(8) 0.0038(8) -0.0095(8) C25 0.0575(17) 0.0571(18) 0.0362(14) -0.0043(13) 0.0089(12) 0.0170(14) C26 0.0607(16) 0.0291(12) 0.0231(11) -0.0008(9) -0.0040(10) 0.0000(10) C27 0.0138(7) 0.0147(8) 0.0201(9) -0.0016(6) -0.0029(6) -0.0006(6) C28 0.0137(8) 0.0169(8) 0.0209(9) -0.0034(7) -0.0024(6) -0.0010(6) C29 0.0176(8) 0.0250(9) 0.0195(9) -0.0070(7) -0.0005(7) -0.0027(7) C30 0.0144(8) 0.0263(9) 0.0210(9) -0.0062(7) 0.0006(6) -0.0046(7) C31 0.0271(10) 0.0208(9) 0.0277(10) 0.0008(8) -0.0050(8) 0.0013(7) C32 0.0693(19) 0.0628(19) 0.0338(14) -0.0078(13) -0.0053(13) -0.0300(15) C33 0.080(2) 0.0487(16) 0.0275(13) 0.0091(11) 0.0017(13) -0.0191(15) C34 0.0271(10) 0.0229(9) 0.0197(9) -0.0080(7) -0.0001(7) -0.0028(7) C35 0.0314(13) 0.090(2) 0.0355(14) -0.0143(14) 0.0056(10) -0.0293(13) C36 0.0373(12) 0.0447(13) 0.0198(10) -0.0030(9) -0.0001(9) -0.0084(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 O2 2.2021(13) . ? Cd1 O5 2.2296(13) . ? Cd1 O11 2.2490(14) . ? Cd1 O9 2.3641(13) . ? Cd1 O10 2.3707(13) . ? Cd1 O12 2.3977(14) . ? Cd2 O1 2.2336(13) . ? Cd2 O1 2.2336(13) 2 ? Cd2 O6 2.2449(13) 2 ? Cd2 O6 2.2449(13) . ? Cd2 O10 2.3145(12) . ? Cd2 O10 2.3145(12) 2 ? Cd3 O7 2.2078(13) 1_546 ? Cd3 O3 2.2158(13) . ? Cd3 O16 2.2733(14) . ? Cd3 O15 2.3564(13) . ? Cd3 O14 2.3565(13) . ? Cd3 O13 2.3827(13) . ? Cd4 O4 2.2161(14) . ? Cd4 O4 2.2161(14) 2_646 ? Cd4 O8 2.2651(12) 2_655 ? Cd4 O8 2.2651(12) 1_546 ? Cd4 O14 2.3244(12) . ? Cd4 O14 2.3244(12) 2_646 ? O1 C1 1.249(2) . ? O2 C1 1.267(2) . ? O3 C8 1.255(2) . ? O4 C8 1.249(2) . ? O5 C9 1.259(2) . ? O6 C9 1.253(2) . ? O7 C16 1.271(2) . ? O7 Cd3 2.2078(13) 1_564 ? O8 C16 1.251(2) . ? O8 Cd4 2.2651(12) 1_564 ? O9 C17 1.251(2) . ? O10 C17 1.279(2) . ? O11 C21 1.251(2) . ? O12 C24 1.241(3) . ? O13 C27 1.248(2) . ? O14 C27 1.280(2) . ? O15 C31 1.238(2) . ? O16 C34 1.246(2) . ? N1 C21 1.306(3) . ? N1 C22 1.451(3) . ? N1 C23 1.455(3) . ? N2 C24 1.319(3) . ? N2 C25 1.451(3) . ? N2 C26 1.463(3) . ? N3 C34 1.310(3) . ? N3 C35 1.453(3) . ? N3 C36 1.457(3) . ? N4 C31 1.316(3) . ? N4 C32 1.455(3) . ? N4 C33 1.455(3) . ? C1 C2 1.506(2) . ? C2 C3 1.388(3) . ? C2 C7 1.393(3) . ? C3 C4 1.392(3) . ? C4 C5 1.392(3) . ? C5 C6 1.389(3) . ? C5 C8 1.508(2) . ? C6 C7 1.390(2) . ? C9 C10 1.509(2) . ? C10 C11 1.390(3) . ? C10 C15 1.390(3) . ? C11 C12 1.394(3) . ? C12 C13 1.391(3) . ? C13 C14 1.392(3) . ? C13 C16 1.505(2) . ? C14 C15 1.390(3) . ? C17 C18 1.497(2) . ? C18 C20 1.389(3) . ? C18 C19 1.399(3) . ? C19 C20 1.390(3) 2_455 ? C20 C19 1.390(3) 2_455 ? C27 C28 1.502(2) . ? C28 C29 1.393(3) . ? C28 C30 1.394(3) . ? C29 C30 1.390(3) 2_746 ? C30 C29 1.390(3) 2_746 ? 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 O2 Cd1 O5 99.65(5) . . ? O2 Cd1 O11 109.89(6) . . ? O5 Cd1 O11 83.56(5) . . ? O2 Cd1 O9 150.36(5) . . ? O5 Cd1 O9 98.13(5) . . ? O11 Cd1 O9 95.49(5) . . ? O2 Cd1 O10 97.90(5) . . ? O5 Cd1 O10 100.29(5) . . ? O11 Cd1 O10 150.97(5) . . ? O9 Cd1 O10 55.50(4) . . ? O2 Cd1 O12 80.12(5) . . ? O5 Cd1 O12 173.35(5) . . ? O11 Cd1 O12 90.25(5) . . ? O9 Cd1 O12 84.86(5) . . ? O10 Cd1 O12 86.31(5) . . ? O1 Cd2 O1 180.00(10) . 2 ? O1 Cd2 O6 87.00(5) . 2 ? O1 Cd2 O6 93.00(5) 2 2 ? O1 Cd2 O6 93.00(5) . . ? O1 Cd2 O6 87.00(5) 2 . ? O6 Cd2 O6 180.00(11) 2 . ? O1 Cd2 O10 88.57(5) . . ? O1 Cd2 O10 91.43(5) 2 . ? O6 Cd2 O10 87.93(5) 2 . ? O6 Cd2 O10 92.07(5) . . ? O1 Cd2 O10 91.43(5) . 2 ? O1 Cd2 O10 88.57(5) 2 2 ? O6 Cd2 O10 92.07(5) 2 2 ? O6 Cd2 O10 87.93(5) . 2 ? O10 Cd2 O10 180.00(7) . 2 ? O7 Cd3 O3 108.87(5) 1_546 . ? O7 Cd3 O16 99.18(5) 1_546 . ? O3 Cd3 O16 80.98(5) . . ? O7 Cd3 O15 80.62(5) 1_546 . ? O3 Cd3 O15 167.89(5) . . ? O16 Cd3 O15 90.22(5) . . ? O7 Cd3 O14 94.53(5) 1_546 . ? O3 Cd3 O14 98.47(5) . . ? O16 Cd3 O14 165.69(5) . . ? O15 Cd3 O14 88.00(5) . . ? O7 Cd3 O13 145.91(5) 1_546 . ? O3 Cd3 O13 93.01(5) . . ? O16 Cd3 O13 110.10(5) . . ? O15 Cd3 O13 82.16(5) . . ? O14 Cd3 O13 55.60(4) . . ? O4 Cd4 O4 180.000(1) . 2_646 ? O4 Cd4 O8 85.42(5) . 2_655 ? O4 Cd4 O8 94.58(5) 2_646 2_655 ? O4 Cd4 O8 94.58(5) . 1_546 ? O4 Cd4 O8 85.42(5) 2_646 1_546 ? O8 Cd4 O8 180.00(4) 2_655 1_546 ? O4 Cd4 O14 92.82(5) . . ? O4 Cd4 O14 87.18(5) 2_646 . ? O8 Cd4 O14 91.43(5) 2_655 . ? O8 Cd4 O14 88.57(5) 1_546 . ? O4 Cd4 O14 87.18(5) . 2_646 ? O4 Cd4 O14 92.82(5) 2_646 2_646 ? O8 Cd4 O14 88.57(5) 2_655 2_646 ? O8 Cd4 O14 91.43(5) 1_546 2_646 ? O14 Cd4 O14 180.0 . 2_646 ? C1 O1 Cd2 141.55(12) . . ? C1 O2 Cd1 118.47(11) . . ? C8 O3 Cd3 133.80(12) . . ? C8 O4 Cd4 133.36(12) . . ? C9 O5 Cd1 132.45(12) . . ? C9 O6 Cd2 130.76(12) . . ? C16 O7 Cd3 119.60(12) . 1_564 ? C16 O8 Cd4 138.19(12) . 1_564 ? C17 O9 Cd1 92.02(11) . . ? C17 O10 Cd2 132.78(11) . . ? C17 O10 Cd1 91.01(11) . . ? Cd2 O10 Cd1 103.16(5) . . ? C21 O11 Cd1 123.31(13) . . ? C24 O12 Cd1 117.21(13) . . ? C27 O13 Cd3 90.96(10) . . ? C27 O14 Cd4 132.60(11) . . ? C27 O14 Cd3 91.36(11) . . ? Cd4 O14 Cd3 102.93(5) . . ? C31 O15 Cd3 119.83(13) . . ? C34 O16 Cd3 132.26(13) . . ? C21 N1 C22 121.93(18) . . ? C21 N1 C23 120.85(18) . . ? C22 N1 C23 117.22(18) . . ? C24 N2 C25 121.1(2) . . ? C24 N2 C26 120.7(2) . . ? C25 N2 C26 117.9(2) . . ? C34 N3 C35 120.67(19) . . ? C34 N3 C36 121.41(17) . . ? C35 N3 C36 117.90(19) . . ? C31 N4 C32 121.0(2) . . ? C31 N4 C33 121.8(2) . . ? C32 N4 C33 117.2(2) . . ? O1 C1 O2 125.54(17) . . ? O1 C1 C2 117.99(17) . . ? O2 C1 C2 116.47(16) . . ? C3 C2 C7 119.95(17) . . ? C3 C2 C1 120.00(16) . . ? C7 C2 C1 120.04(17) . . ? C2 C3 C4 120.08(18) . . ? C5 C4 C3 120.12(18) . . ? C6 C5 C4 119.58(17) . . ? C6 C5 C8 120.02(16) . . ? C4 C5 C8 120.38(17) . . ? C5 C6 C7 120.53(17) . . ? C6 C7 C2 119.69(17) . . ? O4 C8 O3 126.75(17) . . ? O4 C8 C5 116.73(16) . . ? O3 C8 C5 116.51(16) . . ? O6 C9 O5 126.50(17) . . ? O6 C9 C10 117.17(16) . . ? O5 C9 C10 116.32(16) . . ? C11 C10 C15 119.37(17) . . ? C11 C10 C9 120.60(16) . . ? C15 C10 C9 120.02(16) . . ? C10 C11 C12 120.51(18) . . ? C13 C12 C11 120.08(17) . . ? C12 C13 C14 119.29(16) . . ? C12 C13 C16 120.48(16) . . ? C14 C13 C16 120.23(16) . . ? C15 C14 C13 120.57(17) . . ? C14 C15 C10 120.17(17) . . ? O8 C16 O7 125.28(16) . . ? O8 C16 C13 118.36(16) . . ? O7 C16 C13 116.34(16) . . ? O9 C17 O10 121.31(16) . . ? O9 C17 C18 120.04(16) . . ? O10 C17 C18 118.59(16) . . ? C20 C18 C19 119.83(16) . . ? C20 C18 C17 120.39(16) . . ? C19 C18 C17 119.76(16) . . ? C20 C19 C18 120.17(17) 2_455 . ? C18 C20 C19 120.00(17) . 2_455 ? O11 C21 N1 123.87(19) . . ? O12 C24 N2 125.5(2) . . ? O13 C27 O14 121.87(16) . . ? O13 C27 C28 119.97(16) . . ? O14 C27 C28 118.09(16) . . ? C29 C28 C30 119.81(16) . . ? C29 C28 C27 119.98(16) . . ? C30 C28 C27 120.20(16) . . ? C30 C29 C28 120.30(17) 2_746 . ? C29 C30 C28 119.90(17) 2_746 . ? O15 C31 N4 125.1(2) . . ? O16 C34 N3 126.23(19) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.424 _refine_diff_density_min -1.301 _refine_diff_density_rms 0.116 #===END data_compound_4_h03kc2 _database_code_depnum_ccdc_archive 'CCDC 651818' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H38 Cd N4 O10' _chemical_formula_weight 679.00 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 9.7830(2) _cell_length_b 21.2010(4) _cell_length_c 27.8110(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5768.26(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17175 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Tabloid _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.76 _exptl_absorpt_process_details ? _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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15349 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4207 _reflns_number_gt 3873 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo & Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+1.6071P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.038(16) _refine_ls_number_reflns 4207 _refine_ls_number_parameters 247 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.0000 0.499892(11) 0.01661(5) Uani 1 2 d S . . O1 O 0.39084(18) 0.09695(9) 0.52893(6) 0.0338(4) Uani 1 1 d . . . O2 O 0.3211(3) 0.00679(8) 0.55820(8) 0.0372(5) Uani 1 1 d . . . O3 O -0.14278(15) 0.17073(7) 0.70687(5) 0.0268(3) Uani 1 1 d . . . O4 O -0.0700(3) 0.26043(9) 0.67641(8) 0.0372(5) Uani 1 1 d . . . O5 O 0.0009(3) 0.26240(18) 0.47696(15) 0.0408(9) Uani 0.50 1 d P A 1 O6 O 0.1041(3) 0.14414(16) 0.46393(13) 0.0383(8) Uani 0.50 1 d P B 2 N1 N -0.1589(3) 0.22934(17) 0.53009(13) 0.0301(7) Uani 0.50 1 d P A 1 N2 N -0.0114(4) 0.06055(15) 0.4950(3) 0.0268(11) Uani 0.50 1 d P B 2 N3 N 0.3584(2) 0.14767(10) 0.43316(7) 0.0396(4) Uani 1 1 d D . . C1 C 0.3148(2) 0.06563(11) 0.55588(7) 0.0246(4) Uani 1 1 d . . . C2 C 0.2123(2) 0.10044(10) 0.58701(7) 0.0202(4) Uani 1 1 d . . . C3 C 0.1996(2) 0.16530(10) 0.58375(8) 0.0239(4) Uani 1 1 d . . . H3 H 0.2542 0.1880 0.5614 0.029 Uiso 1 1 calc R . . C4 C 0.1073(2) 0.19747(10) 0.61299(7) 0.0254(4) Uani 1 1 d . . . H4 H 0.0987 0.2419 0.6102 0.030 Uiso 1 1 calc R . . C5 C 0.0282(2) 0.16539(9) 0.64604(7) 0.0190(4) Uani 1 1 d . . . C6 C 0.0394(2) 0.10042(10) 0.64897(7) 0.0230(4) Uani 1 1 d . . . H6 H -0.0155 0.0778 0.6712 0.028 Uiso 1 1 calc R . . C7 C 0.1305(2) 0.06789(9) 0.61954(7) 0.0240(4) Uani 1 1 d . . . H7 H 0.1368 0.0233 0.6217 0.029 Uiso 1 1 calc R . . C8 C -0.0690(2) 0.20174(10) 0.67842(7) 0.0229(4) Uani 1 1 d . . . C9 C -0.0872(4) 0.2729(2) 0.50738(15) 0.0304(9) Uani 0.50 1 d P A 1 H9 H -0.1051 0.3158 0.5152 0.037 Uiso 0.50 1 calc PR A 1 C10 C -0.2500 0.2500 0.56611(14) 0.0508(10) Uani 1 2 d S A 1 H10A H -0.2357 0.2252 0.5954 0.076 Uiso 0.50 1 calc PR A 1 H10B H -0.3443 0.2445 0.5550 0.076 Uiso 0.50 1 calc PR A 1 H10C H -0.2334 0.2947 0.5730 0.076 Uiso 0.50 1 calc PR A 1 C11 C -0.1355(5) 0.1622(2) 0.52277(18) 0.0357(10) Uani 0.50 1 d P A 1 H11A H -0.0716 0.1562 0.4960 0.053 Uiso 0.50 1 calc PR A 1 H11B H -0.2224 0.1414 0.5153 0.053 Uiso 0.50 1 calc PR A 1 H11C H -0.0966 0.1438 0.5521 0.053 Uiso 0.50 1 calc PR A 1 C12 C 0.0834(5) 0.0869(2) 0.46786(18) 0.0282(11) Uani 0.50 1 d P B 2 H12 H 0.1406 0.0595 0.4498 0.034 Uiso 0.50 1 calc PR B 2 C13 C -0.1048(5) 0.1002(2) 0.52216(18) 0.0294(10) Uani 0.50 1 d P B 2 H13A H -0.1980 0.0838 0.5190 0.044 Uiso 0.50 1 calc PR B 2 H13B H -0.1012 0.1434 0.5096 0.044 Uiso 0.50 1 calc PR B 2 H13C H -0.0781 0.1003 0.5561 0.044 Uiso 0.50 1 calc PR B 2 C14 C 0.0000 0.0000 0.4978(4) 0.0554(11) Uani 1 2 d S B 2 H14A H 0.0497 -0.0158 0.4697 0.083 Uiso 0.50 1 calc PR B 2 H14B H -0.0912 -0.0191 0.4988 0.083 Uiso 0.50 1 calc PR B 2 H14C H 0.0502 -0.0111 0.5271 0.083 Uiso 0.50 1 calc PR B 2 C15 C 0.3766(3) 0.14921(14) 0.38153(9) 0.0508(6) Uani 1 1 d . C 4 H15A H 0.3252 0.1145 0.3668 0.076 Uiso 1 1 calc R C 4 H15B H 0.4739 0.1447 0.3739 0.076 Uiso 1 1 calc R C 4 H15C H 0.3431 0.1895 0.3689 0.076 Uiso 1 1 calc R C 4 C16 C 0.4304(6) 0.2134(3) 0.4535(3) 0.0564(15) Uani 0.50 1 d P C 4 H16A H 0.5180 0.2200 0.4371 0.085 Uiso 0.50 1 calc PR C 4 H16B H 0.4460 0.2097 0.4882 0.085 Uiso 0.50 1 calc PR C 4 H16C H 0.3699 0.2493 0.4471 0.085 Uiso 0.50 1 calc PR C 4 C16A C 0.2045(4) 0.1551(2) 0.44209(18) 0.0370(10) Uani 0.50 1 d P C 4 H16D H 0.1767 0.1984 0.4344 0.056 Uiso 0.50 1 calc PR C 4 H16E H 0.1843 0.1462 0.4759 0.056 Uiso 0.50 1 calc PR C 4 H16F H 0.1541 0.1255 0.4216 0.056 Uiso 0.50 1 calc PR C 4 H3A H 0.387(3) 0.1092(7) 0.4410(13) 0.090(12) Uiso 1 1 d D D 1 H3B H 0.407(3) 0.1699(13) 0.4544(9) 0.059(9) Uiso 1 1 d D E 1 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 0.01528(7) 0.01792(7) 0.01664(7) 0.000 0.000 0.00068(11) O1 0.0278(8) 0.0461(10) 0.0275(8) -0.0004(7) 0.0129(7) 0.0027(7) O2 0.0414(10) 0.0310(10) 0.0391(12) 0.0005(7) 0.0118(10) 0.0150(8) O3 0.0203(7) 0.0384(9) 0.0218(7) -0.0061(6) 0.0076(6) -0.0001(6) O4 0.0414(10) 0.0273(8) 0.0427(12) -0.0067(8) 0.0098(10) 0.0091(9) O5 0.042(2) 0.0311(17) 0.049(2) 0.0026(16) 0.0203(16) 0.0003(13) O6 0.0336(17) 0.0359(19) 0.045(2) 0.0116(16) 0.0013(15) 0.0020(14) N1 0.0296(17) 0.0344(18) 0.0262(17) 0.0020(15) 0.0007(14) 0.0033(15) N2 0.0230(15) 0.0244(14) 0.033(3) 0.0039(19) 0.0037(16) 0.0022(14) N3 0.0471(11) 0.0380(11) 0.0339(10) 0.0119(9) 0.0048(9) 0.0163(9) C1 0.0190(9) 0.0371(11) 0.0176(9) -0.0066(8) -0.0015(7) 0.0096(8) C2 0.0174(7) 0.0247(10) 0.0184(9) -0.0021(8) 0.0011(8) 0.0016(8) C3 0.0225(9) 0.0238(10) 0.0252(10) -0.0002(8) 0.0091(8) -0.0041(8) C4 0.0267(10) 0.0207(9) 0.0288(10) -0.0037(8) 0.0061(8) 0.0003(8) C5 0.0170(8) 0.0224(10) 0.0175(9) -0.0041(7) 0.0012(7) -0.0010(7) C6 0.0256(9) 0.0241(10) 0.0194(9) 0.0028(8) 0.0052(8) -0.0018(8) C7 0.0274(10) 0.0223(9) 0.0224(9) -0.0025(8) 0.0018(8) 0.0033(8) C8 0.0157(8) 0.0336(11) 0.0195(9) -0.0070(8) -0.0014(7) 0.0022(8) C9 0.033(2) 0.031(2) 0.027(2) 0.0018(17) 0.0028(17) 0.0006(17) C10 0.053(2) 0.066(3) 0.0329(18) 0.000 0.000 0.0213(18) C11 0.038(2) 0.037(3) 0.032(2) 0.0025(19) -0.001(2) -0.0082(19) C12 0.023(2) 0.028(2) 0.034(3) 0.0033(18) 0.0047(18) 0.0004(17) C13 0.0212(19) 0.039(3) 0.028(2) -0.008(2) 0.0004(17) 0.0014(19) C14 0.075(2) 0.056(2) 0.035(2) 0.000 0.000 0.035(3) C15 0.0553(14) 0.0614(17) 0.0357(12) 0.0147(13) -0.0042(11) -0.0101(15) C16 0.046(3) 0.036(3) 0.087(5) -0.004(3) 0.019(3) -0.006(2) C16A 0.029(2) 0.041(3) 0.041(3) -0.004(2) -0.0026(19) 0.0048(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.3143(15) 7_544 ? Cd1 O3 2.3143(15) 12_554 ? Cd1 O2 2.391(2) . ? Cd1 O2 2.391(2) 2_655 ? Cd1 O1 2.4530(18) . ? Cd1 O1 2.4530(18) 2_655 ? O1 C1 1.247(3) . ? O2 C1 1.251(3) . ? O3 C8 1.257(3) . ? O3 Cd1 2.3143(15) 3 ? O4 C8 1.245(3) . ? O5 C9 1.228(5) . ? O6 C12 1.235(6) . ? N1 C9 1.321(6) . ? N1 C10 1.411(4) . ? N1 C11 1.457(5) . ? N2 C14 1.291(3) . ? N2 C12 1.320(8) . ? N2 C13 1.454(7) . ? N3 C15 1.447(3) . ? N3 C16A 1.534(5) . ? N3 C16 1.661(7) . ? C1 C2 1.517(3) . ? C2 C3 1.384(3) . ? C2 C7 1.391(3) . ? C3 C4 1.394(3) . ? C4 C5 1.381(3) . ? C5 C6 1.384(3) . ? C5 C8 1.519(3) . ? C6 C7 1.393(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 O3 Cd1 O3 117.74(8) 7_544 12_554 ? O3 Cd1 O2 93.58(6) 7_544 . ? O3 Cd1 O2 129.70(5) 12_554 . ? O3 Cd1 O2 129.70(5) 7_544 2_655 ? O3 Cd1 O2 93.58(6) 12_554 2_655 ? O2 Cd1 O2 94.57(12) . 2_655 ? O3 Cd1 O1 125.55(5) 7_544 . ? O3 Cd1 O1 76.05(6) 12_554 . ? O2 Cd1 O1 53.66(6) . . ? O2 Cd1 O1 98.39(7) 2_655 . ? O3 Cd1 O1 76.05(6) 7_544 2_655 ? O3 Cd1 O1 125.55(5) 12_554 2_655 ? O2 Cd1 O1 98.39(7) . 2_655 ? O2 Cd1 O1 53.66(6) 2_655 2_655 ? O1 Cd1 O1 141.56(8) . 2_655 ? C1 O1 Cd1 90.64(13) . . ? C1 O2 Cd1 93.48(15) . . ? C8 O3 Cd1 101.89(13) . 3 ? C9 N1 C10 117.2(3) . . ? C9 N1 C11 122.3(4) . . ? C10 N1 C11 120.1(3) . . ? C14 N2 C12 113.3(5) . . ? C14 N2 C13 126.8(7) . . ? C12 N2 C13 119.6(4) . . ? C15 N3 C16A 106.2(3) . . ? C15 N3 C16 105.4(3) . . ? C16A N3 C16 106.0(3) . . ? O1 C1 O2 122.2(2) . . ? O1 C1 C2 118.57(19) . . ? O2 C1 C2 119.2(2) . . ? C3 C2 C7 118.95(18) . . ? C3 C2 C1 120.37(18) . . ? C7 C2 C1 120.68(18) . . ? C2 C3 C4 120.42(18) . . ? C5 C4 C3 120.72(19) . . ? C4 C5 C6 118.99(19) . . ? C4 C5 C8 119.70(18) . . ? C6 C5 C8 121.31(19) . . ? C5 C6 C7 120.60(19) . . ? C2 C7 C6 120.31(18) . . ? O4 C8 O3 123.1(2) . . ? O4 C8 C5 119.0(2) . . ? O3 C8 C5 117.85(19) . . ? O5 C9 N1 125.1(4) . . ? O6 C12 N2 125.6(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.222 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.061 #===END data_compound_5_bath121 _database_code_depnum_ccdc_archive 'CCDC 651819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H34 Cd3 N2 O14' _chemical_formula_weight 1031.83 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 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 25.0960(11) _cell_length_b 10.7885(5) _cell_length_c 17.5107(8) _cell_angle_alpha 90.00 _cell_angle_beta 128.996(3) _cell_angle_gamma 90.00 _cell_volume 3684.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12236 _cell_measurement_theta_min 3.007 _cell_measurement_theta_max 29.388 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.038 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.785 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6868 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART 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 18981 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 29.42 _reflns_number_total 5385 _reflns_number_gt 4936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+3.5224P] 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 5385 _refine_ls_number_parameters 304 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.055 _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 0.0000 0.718171(18) 0.2500 0.02349(6) Uani 1 2 d S . . Cd2 Cd 0.174338(6) 0.820979(12) 0.387377(8) 0.02455(5) Uani 1 1 d . . . O1 O 0.04776(8) 0.58879(17) 0.21209(13) 0.0438(4) Uani 1 1 d . A . O2 O 0.15759(9) 0.6452(2) 0.30891(13) 0.0537(5) Uani 1 1 d . A . O3 O 0.09924(7) 0.26375(15) -0.08146(9) 0.0304(3) Uani 1 1 d . . . O4 O 0.20923(7) 0.29854(15) 0.02518(10) 0.0345(3) Uani 1 1 d . . . O5 O 0.05326(7) 0.87875(16) 0.23516(10) 0.0370(3) Uani 1 1 d . A . O6 O 0.14550(8) 0.9282(2) 0.25427(12) 0.0615(6) Uani 1 1 d . A . O7 O 0.1842(3) 0.9939(5) 0.4702(3) 0.0510(10) Uani 0.70 1 d P A 1 N1 N 0.1409(4) 1.1703(5) 0.4763(5) 0.1039(15) Uani 0.70 1 d PU A 1 C1 C 0.10727(10) 0.5879(2) 0.23869(14) 0.0333(4) Uani 1 1 d . . . C2 C 0.11882(10) 0.5101(2) 0.17873(14) 0.0320(4) Uani 1 1 d . A . C3 C 0.06724(11) 0.4371(3) 0.10240(17) 0.0453(6) Uani 1 1 d . . . H3 H 0.0247 0.4310 0.0901 0.054 Uiso 1 1 calc R A . C4 C 0.07694(11) 0.3722(3) 0.04325(17) 0.0449(6) Uani 1 1 d . A . H4 H 0.0407 0.3238 -0.0101 0.054 Uiso 1 1 calc R . . C5 C 0.13933(9) 0.37830(19) 0.06212(13) 0.0294(4) Uani 1 1 d . . . C6 C 0.19161(11) 0.4492(3) 0.14013(18) 0.0451(6) Uani 1 1 d . A . H6 H 0.2350 0.4521 0.1546 0.054 Uiso 1 1 calc R . . C7 C 0.18111(11) 0.5162(3) 0.19746(18) 0.0456(6) Uani 1 1 d . . . H7 H 0.2169 0.5664 0.2497 0.055 Uiso 1 1 calc R A . C8 C 0.14968(9) 0.31077(17) -0.00191(13) 0.0251(3) Uani 1 1 d . A . C9 C 0.08187(10) 0.9200(2) 0.20214(14) 0.0352(4) Uani 1 1 d . A . C10 C 0.03922(9) 0.9628(2) 0.09766(13) 0.0320(4) Uani 1 1 d . . . C11 C 0.06982(10) 1.0150(3) 0.06208(16) 0.0519(7) Uani 1 1 d . . . H11 H 0.1181 1.0259 0.1047 0.062 Uiso 1 1 calc R . . C12 C -0.03087(11) 0.9483(3) 0.03523(17) 0.0485(6) Uani 1 1 d . . . H12 H -0.0527 0.9130 0.0590 0.058 Uiso 1 1 calc R . . C13 C 0.1407(4) 1.0761(5) 0.4306(5) 0.0886(15) Uani 0.70 1 d PU A 1 H13 H 0.1045 1.0700 0.3618 0.106 Uiso 0.70 1 calc PR A 1 C14 C 0.1953(5) 1.1804(7) 0.5857(7) 0.110(2) Uani 0.70 1 d PU A 1 H14A H 0.1753 1.2224 0.6127 0.131 Uiso 0.70 1 calc PR A 1 H14B H 0.2085 1.0956 0.6136 0.131 Uiso 0.70 1 calc PR A 1 C15 C 0.2563(6) 1.2456(9) 0.6189(7) 0.125(3) Uani 0.70 1 d PU A 1 H15A H 0.2885 1.2468 0.6909 0.188 Uiso 0.70 1 calc PR A 1 H15B H 0.2445 1.3309 0.5941 0.188 Uiso 0.70 1 calc PR A 1 H15C H 0.2776 1.2038 0.5945 0.188 Uiso 0.70 1 calc PR A 1 C16 C 0.0742(6) 1.2531(8) 0.4131(7) 0.122(2) Uani 0.70 1 d PU A 1 H16A H 0.0367 1.2060 0.3546 0.146 Uiso 0.70 1 calc PR A 1 H16B H 0.0596 1.2739 0.4526 0.146 Uiso 0.70 1 calc PR A 1 C17 C 0.0855(6) 1.3567(8) 0.3846(8) 0.145(3) Uani 0.70 1 d PU A 1 H17A H 0.0451 1.4104 0.3515 0.217 Uiso 0.70 1 calc PR A 1 H17B H 0.0945 1.3365 0.3391 0.217 Uiso 0.70 1 calc PR A 1 H17C H 0.1253 1.3997 0.4421 0.217 Uiso 0.70 1 calc PR A 1 O7A O 0.1804(9) 1.0096(15) 0.4406(8) 0.063(3) Uani 0.30 1 d P A 2 N1A N 0.1919(9) 1.1804(14) 0.5362(13) 0.093(2) Uani 0.30 1 d PU A 2 C13A C 0.2002(9) 1.0499(17) 0.5214(12) 0.090(3) Uani 0.30 1 d PU A 2 H13A H 0.2214 0.9943 0.5753 0.108 Uiso 0.30 1 calc PR A 2 C14A C 0.2161(11) 1.2032(19) 0.6372(14) 0.095(3) Uani 0.30 1 d PU A 2 H14C H 0.2218 1.1242 0.6703 0.114 Uiso 0.30 1 calc PR A 2 H14D H 0.1833 1.2563 0.6358 0.114 Uiso 0.30 1 calc PR A 2 C15A C 0.2834(11) 1.2672(19) 0.6883(15) 0.110(4) Uani 0.30 1 d PU A 2 H15D H 0.3017 1.2894 0.7551 0.165 Uiso 0.30 1 calc PR A 2 H15E H 0.2770 1.3425 0.6520 0.165 Uiso 0.30 1 calc PR A 2 H15F H 0.3156 1.2117 0.6913 0.165 Uiso 0.30 1 calc PR A 2 C16A C 0.1557(10) 1.256(2) 0.4607(12) 0.098(3) Uani 0.30 1 d PU A 2 H16C H 0.1408 1.2132 0.4000 0.118 Uiso 0.30 1 calc PR A 2 H16D H 0.1831 1.3294 0.4712 0.118 Uiso 0.30 1 calc PR A 2 C17A C 0.0980(12) 1.291(2) 0.4532(15) 0.111(5) Uani 0.30 1 d PU A 2 H17D H 0.0665 1.3398 0.3932 0.166 Uiso 0.30 1 calc PR A 2 H17E H 0.1133 1.3410 0.5105 0.166 Uiso 0.30 1 calc PR A 2 H17F H 0.0745 1.2167 0.4506 0.166 Uiso 0.30 1 calc PR A 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 0.01649(8) 0.03690(10) 0.01984(8) 0.000 0.01276(7) 0.000 Cd2 0.01862(7) 0.03511(8) 0.01774(7) 0.00484(4) 0.01039(6) 0.00066(4) O1 0.0380(8) 0.0576(10) 0.0485(9) -0.0157(8) 0.0333(7) -0.0023(7) O2 0.0358(8) 0.0748(12) 0.0436(9) -0.0293(9) 0.0217(8) -0.0005(8) O3 0.0221(6) 0.0471(8) 0.0210(6) -0.0074(5) 0.0130(5) -0.0034(5) O4 0.0193(6) 0.0572(9) 0.0266(6) -0.0120(6) 0.0143(5) 0.0000(6) O5 0.0317(7) 0.0516(9) 0.0273(6) 0.0124(6) 0.0184(6) 0.0000(6) O6 0.0254(7) 0.1075(17) 0.0340(8) 0.0356(10) 0.0103(6) -0.0013(9) O7 0.0618(19) 0.0395(18) 0.040(2) -0.0010(17) 0.026(2) 0.0133(14) N1 0.142(3) 0.067(2) 0.097(3) 0.0078(19) 0.072(3) 0.045(2) C1 0.0331(9) 0.0417(10) 0.0289(8) -0.0047(8) 0.0213(8) 0.0040(8) C2 0.0281(8) 0.0433(10) 0.0278(8) -0.0075(8) 0.0191(7) 0.0015(7) C3 0.0298(9) 0.0721(16) 0.0437(11) -0.0240(11) 0.0277(9) -0.0106(10) C4 0.0270(9) 0.0722(16) 0.0404(11) -0.0278(11) 0.0236(9) -0.0118(10) C5 0.0214(7) 0.0430(10) 0.0245(8) -0.0082(7) 0.0148(7) -0.0003(7) C6 0.0255(9) 0.0660(15) 0.0480(12) -0.0283(11) 0.0251(9) -0.0087(9) C7 0.0274(9) 0.0633(15) 0.0445(11) -0.0278(11) 0.0218(9) -0.0087(9) C8 0.0201(7) 0.0355(9) 0.0212(7) -0.0030(6) 0.0137(6) 0.0006(6) C9 0.0270(8) 0.0472(11) 0.0249(8) 0.0137(8) 0.0132(7) 0.0000(8) C10 0.0227(8) 0.0452(10) 0.0242(8) 0.0141(7) 0.0129(7) 0.0018(7) C11 0.0208(8) 0.091(2) 0.0324(10) 0.0279(12) 0.0111(8) -0.0038(10) C12 0.0246(9) 0.0827(18) 0.0340(10) 0.0275(11) 0.0164(8) 0.0005(10) C13 0.132(3) 0.058(2) 0.079(3) 0.016(2) 0.067(3) 0.046(2) C14 0.148(4) 0.078(3) 0.100(3) 0.004(3) 0.077(3) 0.032(3) C15 0.157(6) 0.096(4) 0.119(5) 0.007(4) 0.086(4) 0.024(4) C16 0.151(4) 0.081(3) 0.113(3) 0.010(3) 0.073(3) 0.050(3) C17 0.174(6) 0.094(4) 0.128(5) 0.018(4) 0.077(5) 0.049(4) O7A 0.085(6) 0.060(6) 0.040(6) -0.002(5) 0.037(6) -0.003(5) N1A 0.101(5) 0.103(5) 0.084(4) -0.003(4) 0.063(4) 0.001(4) C13A 0.099(6) 0.097(6) 0.084(5) 0.000(5) 0.061(5) 0.001(5) C14A 0.101(5) 0.101(6) 0.086(5) -0.001(5) 0.061(5) -0.001(5) C15A 0.105(7) 0.098(7) 0.099(7) 0.003(6) 0.051(6) -0.002(6) C16A 0.103(5) 0.110(6) 0.085(5) -0.007(4) 0.061(5) -0.004(5) C17A 0.111(7) 0.109(7) 0.085(6) -0.020(6) 0.048(6) -0.005(7) _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 O1 2.1971(15) 2 ? Cd1 O1 2.1971(15) . ? Cd1 O5 2.3005(15) 2 ? Cd1 O5 2.3005(15) . ? Cd1 O3 2.3876(13) 6_566 ? Cd1 O3 2.3876(13) 5_565 ? Cd2 O7A 2.203(16) . ? Cd2 O2 2.2209(18) . ? Cd2 O6 2.2741(16) . ? Cd2 O7 2.279(5) . ? Cd2 O4 2.3043(13) 4 ? Cd2 O4 2.3649(14) 6_566 ? Cd2 O3 2.4453(13) 6_566 ? Cd2 O5 2.5560(15) . ? Cd2 C9 2.7523(18) . ? O1 C1 1.254(2) . ? O2 C1 1.239(3) . ? O3 C8 1.257(2) . ? O3 Cd1 2.3876(13) 5_565 ? O3 Cd2 2.4453(13) 6_565 ? O4 C8 1.259(2) . ? O4 Cd2 2.3043(13) 4_545 ? O4 Cd2 2.3649(13) 6_565 ? O5 C9 1.253(2) . ? O6 C9 1.248(3) . ? O7 C13 1.228(8) . ? N1 C13 1.292(7) . ? N1 C14 1.502(11) . ? N1 C16 1.579(11) . ? C1 C2 1.508(2) . ? C2 C3 1.380(3) . ? C2 C7 1.382(3) . ? C3 C4 1.392(3) . ? C4 C5 1.383(3) . ? C5 C6 1.385(3) . ? C5 C8 1.491(2) . ? C6 C7 1.390(3) . ? C9 C10 1.497(2) . ? C10 C12 1.376(3) . ? C10 C11 1.377(3) . ? C11 C12 1.385(3) 5_575 ? C12 C11 1.385(3) 5_575 ? C14 C15 1.433(15) . ? C16 C17 1.326(15) . ? O7A C13A 1.246(18) . ? N1A C16A 1.31(2) . ? N1A C13A 1.47(2) . ? N1A C14A 1.49(2) . ? C14A C15A 1.49(3) . ? C16A C17A 1.42(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 O1 Cd1 O1 101.11(10) 2 . ? O1 Cd1 O5 88.75(6) 2 2 ? O1 Cd1 O5 168.17(7) . 2 ? O1 Cd1 O5 168.17(7) 2 . ? O1 Cd1 O5 88.75(6) . . ? O5 Cd1 O5 82.29(8) 2 . ? O1 Cd1 O3 91.23(6) 2 6_566 ? O1 Cd1 O3 94.72(6) . 6_566 ? O5 Cd1 O3 91.55(5) 2 6_566 ? O5 Cd1 O3 81.36(5) . 6_566 ? O1 Cd1 O3 94.72(6) 2 5_565 ? O1 Cd1 O3 91.23(6) . 5_565 ? O5 Cd1 O3 81.36(5) 2 5_565 ? O5 Cd1 O3 91.55(5) . 5_565 ? O3 Cd1 O3 170.63(8) 6_566 5_565 ? O7A Cd2 O2 170.4(3) . . ? O7A Cd2 O6 81.7(2) . . ? O2 Cd2 O6 89.19(9) . . ? O7A Cd2 O7 12.5(3) . . ? O2 Cd2 O7 174.33(16) . . ? O6 Cd2 O7 94.19(13) . . ? O7A Cd2 O4 95.4(5) . 4 ? O2 Cd2 O4 89.35(6) . 4 ? O6 Cd2 O4 100.79(5) . 4 ? O7 Cd2 O4 94.49(16) . 4 ? O7A Cd2 O4 100.9(2) . 6_566 ? O2 Cd2 O4 88.29(7) . 6_566 ? O6 Cd2 O4 176.21(7) . 6_566 ? O7 Cd2 O4 88.56(11) . 6_566 ? O4 Cd2 O4 76.36(5) 4 6_566 ? O7A Cd2 O3 96.3(4) . 6_566 ? O2 Cd2 O3 86.94(7) . 6_566 ? O6 Cd2 O3 128.76(5) . 6_566 ? O7 Cd2 O3 87.39(16) . 6_566 ? O4 Cd2 O3 130.20(5) 4 6_566 ? O4 Cd2 O3 53.92(4) 6_566 6_566 ? O7A Cd2 O5 86.4(4) . . ? O2 Cd2 O5 85.70(6) . . ? O6 Cd2 O5 53.44(5) . . ? O7 Cd2 O5 92.64(13) . . ? O4 Cd2 O5 153.74(5) 4 . ? O4 Cd2 O5 129.12(5) 6_566 . ? O3 Cd2 O5 75.31(4) 6_566 . ? O7A Cd2 C9 85.5(3) . . ? O2 Cd2 C9 84.92(7) . . ? O6 Cd2 C9 26.63(6) . . ? O7 Cd2 C9 96.07(12) . . ? O4 Cd2 C9 126.88(5) 4 . ? O4 Cd2 C9 155.57(5) 6_566 . ? O3 Cd2 C9 102.21(5) 6_566 . ? O5 Cd2 C9 26.99(5) . . ? C1 O1 Cd1 129.91(14) . . ? C1 O2 Cd2 135.91(15) . . ? C8 O3 Cd1 151.21(14) . 5_565 ? C8 O3 Cd2 91.04(10) . 6_565 ? Cd1 O3 Cd2 96.06(4) 5_565 6_565 ? C8 O4 Cd2 161.43(13) . 4_545 ? C8 O4 Cd2 94.77(11) . 6_565 ? Cd2 O4 Cd2 103.64(5) 4_545 6_565 ? C9 O5 Cd1 149.54(16) . . ? C9 O5 Cd2 85.27(11) . . ? Cd1 O5 Cd2 95.31(5) . . ? C9 O6 Cd2 98.58(12) . . ? C13 O7 Cd2 122.0(4) . . ? C13 N1 C14 119.6(6) . . ? C13 N1 C16 115.0(7) . . ? C14 N1 C16 124.4(6) . . ? O2 C1 O1 126.62(18) . . ? O2 C1 C2 116.51(18) . . ? O1 C1 C2 116.86(18) . . ? C3 C2 C7 119.24(17) . . ? C3 C2 C1 121.18(17) . . ? C7 C2 C1 119.52(18) . . ? C2 C3 C4 120.71(18) . . ? C5 C4 C3 119.99(19) . . ? C4 C5 C6 119.29(17) . . ? C4 C5 C8 120.26(17) . . ? C6 C5 C8 120.44(16) . . ? C5 C6 C7 120.48(18) . . ? C2 C7 C6 120.3(2) . . ? O3 C8 O4 120.27(16) . . ? O3 C8 C5 120.00(15) . . ? O4 C8 C5 119.70(16) . . ? O6 C9 O5 121.92(18) . . ? O6 C9 C10 118.29(17) . . ? O5 C9 C10 119.79(17) . . ? O6 C9 Cd2 54.79(10) . . ? O5 C9 Cd2 67.75(10) . . ? C10 C9 Cd2 169.77(16) . . ? C12 C10 C11 119.01(17) . . ? C12 C10 C9 120.62(17) . . ? C11 C10 C9 120.36(17) . . ? C10 C11 C12 120.70(18) . 5_575 ? C10 C12 C11 120.29(18) . 5_575 ? O7 C13 N1 124.2(7) . . ? C15 C14 N1 115.8(10) . . ? C17 C16 N1 110.9(10) . . ? C13A O7A Cd2 132.4(12) . . ? C16A N1A C13A 120.1(16) . . ? C16A N1A C14A 127.0(16) . . ? C13A N1A C14A 111.8(15) . . ? O7A C13A N1A 122.3(16) . . ? N1A C14A C15A 104.6(17) . . ? N1A C16A C17A 106.2(17) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 29.42 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.659 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.076 #===END