Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Prof Xian-He Bu' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071 CHINA ; _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_section_title ; Formation of 3D networks by H-bonding from novel trinuclear or 1D chain complexes of zinc(II) and cadmium(II) with isonicotinic acid analogues and the effects of pi-pi stacking ; loop_ _publ_author_name 'Xian-He Bu.' 'Ho-Chol Chang.' 'Susumu Kitagawa.' 'Jian-Rong Li.' ; Li-Jun Li ; 'Ming-Liang Tong.' data_zn_a _database_code_depnum_ccdc_archive 'CCDC 228091' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 N2 O5 Zn' _chemical_formula_weight 427.70 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' Zn Zn 0.2839 1.4301 '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 14.923(3) _cell_length_b 14.426(3) _cell_length_c 7.544(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.90(3) _cell_angle_gamma 90.00 _cell_volume 1623.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 862 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 26.79 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.553 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6883 _exptl_absorpt_correction_T_max 0.7070 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996; Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku Mercury/MSC CCD' _diffrn_measurement_method dtintegrate.ref' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2247 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 30.34 _reflns_number_total 1553 _reflns_number_gt 1343 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0454P)^2^+8.3728P] 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 1553 _refine_ls_number_parameters 133 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.5000 0.5000 0.0198(2) Uani 1 2 d S . . O1 O 0.39586(19) 0.57308(19) 0.5872(3) 0.0365(7) Uani 1 1 d . . . O2 O 0.4069(2) 0.59261(19) 0.8824(3) 0.0372(7) Uani 1 1 d . . . O1W O 0.5000 0.5845(2) 0.2500 0.0208(7) Uani 1 2 d SD . . H1W H 0.456(2) 0.622(2) 0.256(6) 0.047(14) Uiso 1 1 d D . . N1 N 0.1465(2) 0.79481(19) 0.7329(3) 0.0256(7) Uani 1 1 d . . . C1 C 0.3731(2) 0.6069(2) 0.7317(4) 0.0239(7) Uani 1 1 d . . . C2 C 0.2933(2) 0.6728(2) 0.7220(4) 0.0221(8) Uani 1 1 d . . . C3 C 0.2995(3) 0.7564(2) 0.8085(4) 0.0254(8) Uani 1 1 d . . . H3 H 0.3527 0.7739 0.8670 0.030 Uiso 1 1 calc R . . C4 C 0.2239(3) 0.8157(2) 0.8075(4) 0.0256(8) Uani 1 1 d . . . H4 H 0.2299 0.8729 0.8633 0.031 Uiso 1 1 calc R . . C5 C 0.1389(2) 0.7130(2) 0.6407(4) 0.0235(8) Uani 1 1 d . . . C6 C 0.0566(3) 0.6921(3) 0.5565(5) 0.0330(9) Uani 1 1 d . . . H6 H 0.0089 0.7332 0.5644 0.040 Uiso 1 1 calc R . . C7 C 0.0458(3) 0.6115(3) 0.4623(5) 0.0381(9) Uani 1 1 d . . . H7 H -0.0094 0.5981 0.4073 0.046 Uiso 1 1 calc R . . C8 C 0.1174(3) 0.5488(3) 0.4481(5) 0.0361(10) Uani 1 1 d . . . H8 H 0.1094 0.4943 0.3835 0.043 Uiso 1 1 calc R . . C9 C 0.1981(3) 0.5677(2) 0.5286(4) 0.0299(9) Uani 1 1 d . . . H9 H 0.2452 0.5262 0.5164 0.036 Uiso 1 1 calc R . . C10 C 0.2121(2) 0.6493(2) 0.6308(4) 0.0221(7) 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 Zn1 0.0205(4) 0.0216(3) 0.0173(2) -0.00324(17) 0.0020(2) 0.00084(19) O1 0.0374(19) 0.0493(15) 0.0232(11) 0.0010(11) 0.0072(11) 0.0200(13) O2 0.0428(19) 0.0449(15) 0.0239(12) 0.0011(10) -0.0004(11) 0.0235(13) O1W 0.024(2) 0.0196(14) 0.0190(14) 0.000 0.0027(13) 0.000 N1 0.029(2) 0.0253(13) 0.0228(12) 0.0028(10) 0.0017(13) 0.0079(12) C1 0.028(2) 0.0231(14) 0.0210(13) 0.0025(11) 0.0022(13) 0.0041(13) C2 0.029(2) 0.0216(13) 0.0165(13) 0.0048(11) 0.0079(13) 0.0058(13) C3 0.026(2) 0.0289(15) 0.0215(14) 0.0015(12) 0.0008(13) 0.0038(14) C4 0.033(3) 0.0224(14) 0.0217(13) -0.0023(11) 0.0042(15) 0.0035(14) C5 0.023(2) 0.0289(15) 0.0185(13) 0.0023(11) 0.0012(14) 0.0033(13) C6 0.025(3) 0.046(2) 0.0283(16) 0.0012(15) 0.0023(16) 0.0051(16) C7 0.031(3) 0.051(2) 0.0325(18) -0.0030(16) -0.0014(17) -0.0075(18) C8 0.043(3) 0.0365(19) 0.0292(16) -0.0072(14) 0.0039(17) -0.0098(17) C9 0.036(3) 0.0267(16) 0.0277(16) -0.0003(13) 0.0062(16) 0.0024(15) C10 0.022(2) 0.0269(15) 0.0179(13) 0.0031(11) 0.0029(13) 0.0019(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.007(2) . ? Zn1 O1 2.007(2) 5_666 ? Zn1 O2 2.102(3) 6_565 ? Zn1 O2 2.102(3) 2_656 ? Zn1 O1W 2.2456(17) 5_666 ? Zn1 O1W 2.2456(17) . ? O1 C1 1.252(4) . ? O2 C1 1.246(4) . ? O2 Zn1 2.102(3) 2_656 ? O1W Zn1 2.2456(17) 2_655 ? O1W H1W 0.851(10) . ? N1 C4 1.304(5) . ? N1 C5 1.373(4) . ? C1 C2 1.523(5) . ? C2 C3 1.374(4) . ? C2 C10 1.414(5) . ? C3 C4 1.415(5) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.398(6) . ? C5 C10 1.431(5) . ? C6 C7 1.369(5) . ? C6 H6 0.9300 . ? C7 C8 1.407(6) . ? C7 H7 0.9300 . ? C8 C9 1.358(6) . ? C8 H8 0.9300 . ? C9 C10 1.420(5) . ? C9 H9 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 180.0 . 5_666 ? O1 Zn1 O2 87.95(12) . 6_565 ? O1 Zn1 O2 92.05(12) 5_666 6_565 ? O1 Zn1 O2 92.05(12) . 2_656 ? O1 Zn1 O2 87.95(12) 5_666 2_656 ? O2 Zn1 O2 180.00(12) 6_565 2_656 ? O1 Zn1 O1W 89.33(8) . 5_666 ? O1 Zn1 O1W 90.67(8) 5_666 5_666 ? O2 Zn1 O1W 89.49(9) 6_565 5_666 ? O2 Zn1 O1W 90.51(9) 2_656 5_666 ? O1 Zn1 O1W 90.67(8) . . ? O1 Zn1 O1W 89.33(8) 5_666 . ? O2 Zn1 O1W 90.51(9) 6_565 . ? O2 Zn1 O1W 89.49(9) 2_656 . ? O1W Zn1 O1W 180.000(1) 5_666 . ? C1 O1 Zn1 136.5(2) . . ? C1 O2 Zn1 137.1(2) . 2_656 ? Zn1 O1W Zn1 114.25(13) 2_655 . ? Zn1 O1W H1W 114(3) 2_655 . ? Zn1 O1W H1W 106(3) . . ? C4 N1 C5 118.2(3) . . ? O2 C1 O1 128.1(3) . . ? O2 C1 C2 116.1(3) . . ? O1 C1 C2 115.8(3) . . ? C3 C2 C10 119.0(3) . . ? C3 C2 C1 119.0(3) . . ? C10 C2 C1 122.0(3) . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? N1 C4 C3 123.9(3) . . ? N1 C4 H4 118.0 . . ? C3 C4 H4 118.0 . . ? N1 C5 C6 118.1(3) . . ? N1 C5 C10 121.9(3) . . ? C6 C5 C10 119.9(3) . . ? C7 C6 C5 120.4(4) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.6(4) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 120.1(4) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 121.5(3) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C2 C10 C9 124.9(3) . . ? C2 C10 C5 117.6(3) . . ? C9 C10 C5 117.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn1 O1 C1 13(100) 5_666 . . . ? O2 Zn1 O1 C1 130.5(4) 6_565 . . . ? O2 Zn1 O1 C1 -49.5(4) 2_656 . . . ? O1W Zn1 O1 C1 41.0(4) 5_666 . . . ? O1W Zn1 O1 C1 -139.0(4) . . . . ? O1 Zn1 O1W Zn1 -129.28(9) . . . 2_655 ? O1 Zn1 O1W Zn1 50.72(9) 5_666 . . 2_655 ? O2 Zn1 O1W Zn1 -41.33(8) 6_565 . . 2_655 ? O2 Zn1 O1W Zn1 138.67(8) 2_656 . . 2_655 ? O1W Zn1 O1W Zn1 94(100) 5_666 . . 2_655 ? Zn1 O2 C1 O1 -10.7(7) 2_656 . . . ? Zn1 O2 C1 C2 168.5(3) 2_656 . . . ? Zn1 O1 C1 O2 -11.6(6) . . . . ? Zn1 O1 C1 C2 169.3(2) . . . . ? O2 C1 C2 C3 48.5(4) . . . . ? O1 C1 C2 C3 -132.2(3) . . . . ? O2 C1 C2 C10 -129.6(3) . . . . ? O1 C1 C2 C10 49.6(4) . . . . ? C10 C2 C3 C4 1.5(4) . . . . ? C1 C2 C3 C4 -176.7(3) . . . . ? C5 N1 C4 C3 -4.0(5) . . . . ? C2 C3 C4 N1 2.1(5) . . . . ? C4 N1 C5 C6 -178.1(3) . . . . ? C4 N1 C5 C10 2.5(4) . . . . ? N1 C5 C6 C7 179.8(3) . . . . ? C10 C5 C6 C7 -0.9(5) . . . . ? C5 C6 C7 C8 -0.4(6) . . . . ? C6 C7 C8 C9 0.2(6) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? C3 C2 C10 C9 176.5(3) . . . . ? C1 C2 C10 C9 -5.3(4) . . . . ? C3 C2 C10 C5 -2.8(4) . . . . ? C1 C2 C10 C5 175.4(3) . . . . ? C8 C9 C10 C2 178.4(3) . . . . ? C8 C9 C10 C5 -2.3(5) . . . . ? N1 C5 C10 C2 0.8(4) . . . . ? C6 C5 C10 C2 -178.5(3) . . . . ? N1 C5 C10 C9 -178.5(3) . . . . ? C6 C5 C10 C9 2.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W N1 0.851(10) 1.950(11) 2.801(3) 179(5) 7_566 _diffrn_measured_fraction_theta_max 0.633 _diffrn_reflns_theta_full 30.34 _diffrn_measured_fraction_theta_full 0.633 _refine_diff_density_max 0.601 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.189 data_zn _database_code_depnum_ccdc_archive 'CCDC 228093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H75 N6 O19.50 Zn3' _chemical_formula_weight 1748.67 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 19.997(2) _cell_length_b 19.997(2) _cell_length_c 19.997(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7996.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25111 _cell_measurement_theta_min 3.0539 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Cubic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3612 _exptl_absorpt_coefficient_mu 0.971 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8147 _exptl_absorpt_correction_T_max 0.8147 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku Mercury/MSC CCD' _diffrn_measurement_method dtintegrate.ref' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25796 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.48 _reflns_number_total 2470 _reflns_number_gt 2186 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0799P)^2^+8.7754P] 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 2470 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Zn1 Zn 0.120890(16) 0.620890(16) 0.879110(16) 0.0189(2) Uani 1 3 d S . . Zn2 Zn 0.0000 0.5000 1.0000 0.0175(2) Uani 1 6 d S . . O1 O 0.02766(10) 0.60039(12) 0.84338(11) 0.0302(5) Uani 1 1 d . . . O2 O -0.01568(11) 0.51205(11) 0.89755(10) 0.0263(5) Uani 1 1 d . . . O3 O 0.10344(11) 0.71961(11) 0.83906(11) 0.0293(5) Uani 1 1 d . . . H3 H 0.1338 0.7373 0.8086 0.035 Uiso 1 1 calc R . . N1 N -0.20458(13) 0.60032(14) 0.75541(14) 0.0310(6) Uani 1 1 d . . . C1 C -0.01810(14) 0.56038(14) 0.85869(14) 0.0195(6) Uani 1 1 d . . . C2 C -0.08403(14) 0.57345(15) 0.82352(15) 0.0225(6) Uani 1 1 d . . . C3 C -0.09979(15) 0.53836(15) 0.76515(15) 0.0255(7) Uani 1 1 d . . . C4 C -0.05756(17) 0.48884(17) 0.73656(17) 0.0320(7) Uani 1 1 d . . . H4A H -0.0176 0.4779 0.7577 0.038 Uiso 1 1 calc R . . C5 C -0.07451(19) 0.45733(19) 0.6791(2) 0.0416(9) Uani 1 1 d . . . H5A H -0.0461 0.4253 0.6609 0.050 Uiso 1 1 calc R . . C6 C -0.1357(2) 0.4732(2) 0.6465(2) 0.0453(9) Uani 1 1 d . . . H6A H -0.1466 0.4517 0.6068 0.054 Uiso 1 1 calc R . . C7 C -0.17790(18) 0.51865(19) 0.67189(18) 0.0383(8) Uani 1 1 d . . . H7A H -0.2181 0.5274 0.6502 0.046 Uiso 1 1 calc R . . C8 C -0.16160(16) 0.55384(16) 0.73200(16) 0.0293(7) Uani 1 1 d . . . C9 C -0.18901(15) 0.63359(16) 0.81154(16) 0.0282(7) Uani 1 1 d . . . C10 C -0.23333(16) 0.68401(18) 0.83470(19) 0.0369(8) Uani 1 1 d . . . H10A H -0.2727 0.6927 0.8114 0.044 Uiso 1 1 calc R . . C11 C -0.21872(19) 0.7196(2) 0.8904(2) 0.0434(9) Uani 1 1 d . . . H11A H -0.2478 0.7530 0.9045 0.052 Uiso 1 1 calc R . . C12 C -0.15978(19) 0.70668(19) 0.92777(19) 0.0400(8) Uani 1 1 d . . . H12A H -0.1512 0.7310 0.9664 0.048 Uiso 1 1 calc R . . C13 C -0.11595(17) 0.65909(18) 0.90748(17) 0.0327(8) Uani 1 1 d . . . H13A H -0.0776 0.6509 0.9325 0.039 Uiso 1 1 calc R . . C14 C -0.12817(15) 0.62148(15) 0.84813(16) 0.0245(6) Uani 1 1 d . . . C15 C 0.0471(2) 0.7582(2) 0.8580(2) 0.0476(10) Uani 1 1 d . . . H15A H 0.0481 0.8003 0.8350 0.071 Uiso 1 1 calc R . . H15B H 0.0481 0.7658 0.9054 0.071 Uiso 1 1 calc R . . H15C H 0.0069 0.7346 0.8464 0.071 Uiso 1 1 calc R . . O1W O -0.1155(6) 0.8845(6) 0.8845(6) 0.141(8) Uani 0.50 3 d SP . . O2W O 0.0000 0.5000 0.5000 0.176(16) Uani 0.50 6 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0189(2) 0.0189(2) 0.0189(2) 0.00038(12) 0.00038(12) -0.00038(12) Zn2 0.0175(2) 0.0175(2) 0.0175(2) 0.00019(17) 0.00019(17) -0.00019(17) O1 0.0187(10) 0.0387(13) 0.0333(12) 0.0069(10) -0.0041(9) -0.0056(10) O2 0.0313(12) 0.0283(12) 0.0194(10) 0.0016(9) -0.0053(9) 0.0009(9) O3 0.0339(12) 0.0263(11) 0.0277(12) 0.0052(9) 0.0019(9) 0.0014(9) N1 0.0229(13) 0.0361(14) 0.0341(15) 0.0055(12) -0.0076(11) 0.0009(11) C1 0.0213(14) 0.0208(14) 0.0164(13) -0.0017(11) -0.0003(11) 0.0014(11) C2 0.0200(14) 0.0233(14) 0.0242(14) 0.0053(12) -0.0030(12) -0.0029(12) C3 0.0228(15) 0.0279(16) 0.0259(16) 0.0057(13) -0.0042(12) -0.0038(12) C4 0.0300(17) 0.0323(17) 0.0337(18) -0.0027(14) -0.0091(14) 0.0019(14) C5 0.042(2) 0.0375(19) 0.046(2) -0.0129(16) -0.0068(17) 0.0003(16) C6 0.052(2) 0.051(2) 0.0330(19) -0.0089(17) -0.0162(17) -0.0077(19) C7 0.0347(18) 0.048(2) 0.0320(18) 0.0002(16) -0.0126(15) -0.0054(16) C8 0.0250(16) 0.0340(17) 0.0289(17) 0.0058(13) -0.0065(13) -0.0057(13) C9 0.0217(15) 0.0310(16) 0.0320(17) 0.0098(14) -0.0003(13) -0.0018(13) C10 0.0226(16) 0.0404(19) 0.048(2) 0.0053(16) -0.0034(14) 0.0080(14) C11 0.038(2) 0.041(2) 0.051(2) -0.0004(17) 0.0065(17) 0.0146(17) C12 0.040(2) 0.044(2) 0.0359(19) -0.0057(16) 0.0018(16) 0.0041(16) C13 0.0299(17) 0.0386(19) 0.0295(17) 0.0003(14) -0.0038(13) 0.0039(14) C14 0.0203(15) 0.0278(16) 0.0254(16) 0.0046(12) 0.0001(12) 0.0001(12) C15 0.059(3) 0.040(2) 0.044(2) 0.0028(17) 0.0015(19) 0.0190(19) O1W 0.141(8) 0.141(8) 0.141(8) -0.027(7) -0.027(7) -0.027(7) O2W 0.176(16) 0.176(16) 0.176(16) -0.024(16) 0.024(16) -0.024(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.038(2) 11_466 ? Zn1 O1 2.038(2) . ? Zn1 O1 2.038(2) 8_656 ? Zn1 O3 2.159(2) 11_466 ? Zn1 O3 2.159(2) . ? Zn1 O3 2.159(2) 8_656 ? Zn2 O2 2.087(2) 23_656 ? Zn2 O2 2.087(2) 11_466 ? Zn2 O2 2.087(2) 13_567 ? Zn2 O2 2.087(2) . ? Zn2 O2 2.087(2) 8_656 ? Zn2 O2 2.087(2) 20_466 ? O1 C1 1.253(4) . ? O2 C1 1.241(4) . ? O3 C15 1.417(4) . ? O3 H3 0.9300 . ? N1 C9 1.341(4) . ? N1 C8 1.350(4) . ? C1 C2 1.517(4) . ? C2 C14 1.394(4) . ? C2 C3 1.398(4) . ? C3 C4 1.421(5) . ? C3 C8 1.436(4) . ? C4 C5 1.354(5) . ? C4 H4A 0.9300 . ? C5 C6 1.422(5) . ? C5 H5A 0.9300 . ? C6 C7 1.340(6) . ? C6 H6A 0.9300 . ? C7 C8 1.431(5) . ? C7 H7A 0.9300 . ? C9 C10 1.420(5) . ? C9 C14 1.440(4) . ? C10 C11 1.354(5) . ? C10 H10A 0.9300 . ? C11 C12 1.419(6) . ? C11 H11A 0.9300 . ? C12 C13 1.356(5) . ? C12 H12A 0.9300 . ? C13 C14 1.426(5) . ? C13 H13A 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 Zn1 O1 101.96(8) 11_466 . ? O1 Zn1 O1 101.96(8) 11_466 8_656 ? O1 Zn1 O1 101.96(8) . 8_656 ? O1 Zn1 O3 84.61(9) 11_466 11_466 ? O1 Zn1 O3 165.40(9) . 11_466 ? O1 Zn1 O3 89.21(9) 8_656 11_466 ? O1 Zn1 O3 89.21(9) 11_466 . ? O1 Zn1 O3 84.61(9) . . ? O1 Zn1 O3 165.40(9) 8_656 . ? O3 Zn1 O3 82.44(9) 11_466 . ? O1 Zn1 O3 165.40(9) 11_466 8_656 ? O1 Zn1 O3 89.21(9) . 8_656 ? O1 Zn1 O3 84.61(9) 8_656 8_656 ? O3 Zn1 O3 82.44(9) 11_466 8_656 ? O3 Zn1 O3 82.44(9) . 8_656 ? O2 Zn2 O2 180.0 23_656 11_466 ? O2 Zn2 O2 92.95(8) 23_656 13_567 ? O2 Zn2 O2 87.05(8) 11_466 13_567 ? O2 Zn2 O2 87.05(8) 23_656 . ? O2 Zn2 O2 92.95(8) 11_466 . ? O2 Zn2 O2 180.0 13_567 . ? O2 Zn2 O2 87.05(8) 23_656 8_656 ? O2 Zn2 O2 92.95(8) 11_466 8_656 ? O2 Zn2 O2 87.05(8) 13_567 8_656 ? O2 Zn2 O2 92.95(8) . 8_656 ? O2 Zn2 O2 92.95(8) 23_656 20_466 ? O2 Zn2 O2 87.05(8) 11_466 20_466 ? O2 Zn2 O2 92.95(8) 13_567 20_466 ? O2 Zn2 O2 87.05(8) . 20_466 ? O2 Zn2 O2 180.0 8_656 20_466 ? C1 O1 Zn1 135.3(2) . . ? C1 O2 Zn2 135.28(19) . . ? C15 O3 Zn1 121.8(2) . . ? C15 O3 H3 119.1 . . ? Zn1 O3 H3 119.1 . . ? C9 N1 C8 118.9(3) . . ? O2 C1 O1 128.4(3) . . ? O2 C1 C2 117.3(3) . . ? O1 C1 C2 114.3(2) . . ? C14 C2 C3 119.9(3) . . ? C14 C2 C1 120.3(3) . . ? C3 C2 C1 119.8(3) . . ? C2 C3 C4 123.5(3) . . ? C2 C3 C8 118.1(3) . . ? C4 C3 C8 118.4(3) . . ? C5 C4 C3 121.1(3) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 120.0(4) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C7 C6 C5 121.3(3) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 120.5(3) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? N1 C8 C7 119.0(3) . . ? N1 C8 C3 122.4(3) . . ? C7 C8 C3 118.5(3) . . ? N1 C9 C10 118.7(3) . . ? N1 C9 C14 122.5(3) . . ? C10 C9 C14 118.7(3) . . ? C11 C10 C9 120.4(3) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 121.1(3) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C14 120.6(3) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C2 C14 C13 123.3(3) . . ? C2 C14 C9 118.1(3) . . ? C13 C14 C9 118.6(3) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn1 O1 C1 -64.7(3) 11_466 . . . ? O1 Zn1 O1 C1 40.4(3) 8_656 . . . ? O3 Zn1 O1 C1 179.6(3) 11_466 . . . ? O3 Zn1 O1 C1 -152.8(3) . . . . ? O3 Zn1 O1 C1 124.7(3) 8_656 . . . ? O2 Zn2 O2 C1 179.3(3) 23_656 . . . ? O2 Zn2 O2 C1 -0.7(3) 11_466 . . . ? O2 Zn2 O2 C1 96(100) 13_567 . . . ? O2 Zn2 O2 C1 -93.8(2) 8_656 . . . ? O2 Zn2 O2 C1 86.2(2) 20_466 . . . ? O1 Zn1 O3 C15 -46.2(3) 11_466 . . . ? O1 Zn1 O3 C15 55.9(3) . . . . ? O1 Zn1 O3 C15 173.5(4) 8_656 . . . ? O3 Zn1 O3 C15 -130.9(3) 11_466 . . . ? O3 Zn1 O3 C15 145.8(3) 8_656 . . . ? Zn2 O2 C1 O1 64.4(4) . . . . ? Zn2 O2 C1 C2 -116.6(3) . . . . ? Zn1 O1 C1 O2 -11.5(5) . . . . ? Zn1 O1 C1 C2 169.5(2) . . . . ? O2 C1 C2 C14 98.1(3) . . . . ? O1 C1 C2 C14 -82.8(3) . . . . ? O2 C1 C2 C3 -83.5(3) . . . . ? O1 C1 C2 C3 95.6(3) . . . . ? C14 C2 C3 C4 179.8(3) . . . . ? C1 C2 C3 C4 1.4(4) . . . . ? C14 C2 C3 C8 0.5(4) . . . . ? C1 C2 C3 C8 -177.8(3) . . . . ? C2 C3 C4 C5 -178.5(3) . . . . ? C8 C3 C4 C5 0.7(5) . . . . ? C3 C4 C5 C6 -0.4(6) . . . . ? C4 C5 C6 C7 -0.8(6) . . . . ? C5 C6 C7 C8 1.7(6) . . . . ? C9 N1 C8 C7 -179.6(3) . . . . ? C9 N1 C8 C3 0.3(5) . . . . ? C6 C7 C8 N1 178.5(3) . . . . ? C6 C7 C8 C3 -1.3(5) . . . . ? C2 C3 C8 N1 -0.4(5) . . . . ? C4 C3 C8 N1 -179.7(3) . . . . ? C2 C3 C8 C7 179.4(3) . . . . ? C4 C3 C8 C7 0.1(4) . . . . ? C8 N1 C9 C10 177.9(3) . . . . ? C8 N1 C9 C14 -0.2(5) . . . . ? N1 C9 C10 C11 -178.7(3) . . . . ? C14 C9 C10 C11 -0.5(5) . . . . ? C9 C10 C11 C12 -1.2(6) . . . . ? C10 C11 C12 C13 1.3(6) . . . . ? C11 C12 C13 C14 0.3(6) . . . . ? C3 C2 C14 C13 179.6(3) . . . . ? C1 C2 C14 C13 -2.0(5) . . . . ? C3 C2 C14 C9 -0.5(4) . . . . ? C1 C2 C14 C9 177.9(3) . . . . ? C12 C13 C14 C2 177.9(3) . . . . ? C12 C13 C14 C9 -2.0(5) . . . . ? N1 C9 C14 C2 0.3(4) . . . . ? C10 C9 C14 C2 -177.8(3) . . . . ? N1 C9 C14 C13 -179.8(3) . . . . ? C10 C9 C14 C13 2.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 N1 0.93 2.21 2.784(3) 118.8 24_556 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.090 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.084 data_cd _database_code_depnum_ccdc_archive 'CCDC 228094' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H75 Cd3 N6 O19.50' _chemical_formula_weight 1889.76 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 Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 20.3420(5) _cell_length_b 20.3420(5) _cell_length_c 20.3420(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8417.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26697 _cell_measurement_theta_min 2.0024 _cell_measurement_theta_max 29.5736 _exptl_crystal_description Cubic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3828 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8392 _exptl_absorpt_correction_T_max 0.8523 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku Mercury/MSC CCD' _diffrn_measurement_method dtintegrate.ref' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27210 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0121 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.47 _reflns_number_total 2599 _reflns_number_gt 2339 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0458P)^2^+7.6069P] 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 2599 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.171 _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 0.120346(9) 0.620346(9) 0.879654(9) 0.02013(13) Uani 1 3 d S . . Cd2 Cd 0.0000 0.5000 1.0000 0.01898(14) Uani 1 6 d S . . O1 O 0.02072(10) 0.60256(12) 0.83911(11) 0.0418(6) Uani 1 1 d . . . O2 O -0.01661(11) 0.51297(11) 0.89095(10) 0.0353(5) Uani 1 1 d . . . O3 O 0.10180(11) 0.72561(10) 0.83865(10) 0.0357(5) Uani 1 1 d . . . H3A H 0.1311 0.7436 0.8086 0.043 Uiso 1 1 calc R . . N1 N -0.20716(12) 0.60008(14) 0.75683(13) 0.0377(6) Uani 1 1 d . . . C1 C -0.02230(13) 0.56165(14) 0.85431(13) 0.0242(6) Uani 1 1 d . . . C2 C -0.08818(13) 0.57359(14) 0.82176(13) 0.0249(6) Uani 1 1 d . . . C3 C -0.10458(14) 0.53886(14) 0.76487(14) 0.0282(6) Uani 1 1 d . . . C4 C -0.06333(16) 0.49007(15) 0.73623(16) 0.0369(7) Uani 1 1 d . . . H4A H -0.0238 0.4792 0.7565 0.044 Uiso 1 1 calc R . . C5 C -0.08080(18) 0.45947(18) 0.68009(18) 0.0487(9) Uani 1 1 d . . . H5A H -0.0530 0.4282 0.6616 0.058 Uiso 1 1 calc R . . C6 C -0.1418(2) 0.4748(2) 0.64884(19) 0.0546(10) Uani 1 1 d . . . H6A H -0.1534 0.4531 0.6103 0.065 Uiso 1 1 calc R . . C7 C -0.18249(18) 0.51985(19) 0.67436(17) 0.0465(9) Uani 1 1 d . . . H7A H -0.2221 0.5289 0.6535 0.056 Uiso 1 1 calc R . . C8 C -0.16562(14) 0.55412(15) 0.73335(15) 0.0339(7) Uani 1 1 d . . . C9 C -0.19060(14) 0.63309(15) 0.81145(15) 0.0327(7) Uani 1 1 d . . . C10 C -0.23384(16) 0.68334(17) 0.83524(18) 0.0443(8) Uani 1 1 d . . . H10A H -0.2732 0.6915 0.8134 0.053 Uiso 1 1 calc R . . C11 C -0.21826(18) 0.71875(19) 0.88864(19) 0.0516(9) Uani 1 1 d . . . H11A H -0.2462 0.7522 0.9025 0.062 Uiso 1 1 calc R . . C12 C -0.15943(18) 0.70586(18) 0.92441(18) 0.0474(8) Uani 1 1 d . . . H12A H -0.1499 0.7302 0.9619 0.057 Uiso 1 1 calc R . . C13 C -0.11743(15) 0.65843(17) 0.90427(16) 0.0376(7) Uani 1 1 d . . . H13A H -0.0794 0.6502 0.9283 0.045 Uiso 1 1 calc R . . C14 C -0.13075(14) 0.62107(14) 0.84680(15) 0.0278(6) Uani 1 1 d . . . C15 C 0.0464(2) 0.76263(19) 0.8589(2) 0.0580(10) Uani 1 1 d . . . H15A H 0.0464 0.8043 0.8369 0.087 Uiso 1 1 calc R . . H15B H 0.0483 0.7695 0.9056 0.087 Uiso 1 1 calc R . . H15C H 0.0070 0.7391 0.8481 0.087 Uiso 1 1 calc R . . O1W O -0.1122(6) 0.8878(6) 0.8878(6) 0.193(12) Uani 0.50 3 d SP . . O2W O 0.0000 0.5000 0.5000 0.182(15) Uani 0.50 6 d SP . . 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 0.02013(13) 0.02013(13) 0.02013(13) -0.00011(7) -0.00011(7) 0.00011(7) Cd2 0.01898(14) 0.01898(14) 0.01898(14) 0.00001(10) 0.00001(10) -0.00001(10) O1 0.0248(11) 0.0592(14) 0.0415(13) 0.0122(11) -0.0087(9) -0.0116(10) O2 0.0450(13) 0.0375(12) 0.0233(10) 0.0034(9) -0.0095(9) 0.0064(10) O3 0.0458(12) 0.0301(11) 0.0310(11) 0.0087(9) 0.0015(9) 0.0025(9) N1 0.0249(12) 0.0465(15) 0.0416(15) 0.0080(12) -0.0105(11) 0.0007(11) C1 0.0221(13) 0.0322(15) 0.0182(12) -0.0017(11) -0.0026(11) 0.0010(11) C2 0.0213(13) 0.0286(14) 0.0248(13) 0.0088(11) -0.0030(11) -0.0040(11) C3 0.0254(13) 0.0312(15) 0.0280(14) 0.0060(12) -0.0040(11) -0.0040(12) C4 0.0324(16) 0.0378(17) 0.0407(18) -0.0021(14) -0.0072(13) 0.0014(13) C5 0.049(2) 0.046(2) 0.051(2) -0.0158(17) -0.0091(17) 0.0006(17) C6 0.062(2) 0.057(2) 0.045(2) -0.0122(18) -0.0208(19) -0.007(2) C7 0.0410(19) 0.058(2) 0.0402(19) 0.0011(16) -0.0186(15) -0.0072(17) C8 0.0283(15) 0.0388(17) 0.0345(16) 0.0060(13) -0.0090(12) -0.0055(13) C9 0.0239(14) 0.0375(16) 0.0367(16) 0.0096(13) -0.0029(12) -0.0004(12) C10 0.0303(16) 0.049(2) 0.054(2) 0.0081(17) -0.0031(15) 0.0113(14) C11 0.043(2) 0.048(2) 0.064(2) 0.0007(18) 0.0089(17) 0.0141(16) C12 0.046(2) 0.050(2) 0.046(2) -0.0101(16) 0.0049(16) 0.0021(16) C13 0.0326(16) 0.0465(19) 0.0336(16) -0.0002(14) -0.0033(13) 0.0014(13) C14 0.0216(13) 0.0315(15) 0.0303(15) 0.0071(11) 0.0003(11) -0.0018(11) C15 0.079(3) 0.045(2) 0.050(2) 0.0036(17) 0.001(2) 0.025(2) O1W 0.193(12) 0.193(12) 0.193(12) -0.051(9) -0.051(9) -0.051(9) O2W 0.182(15) 0.182(15) 0.182(15) 0.011(12) -0.011(12) 0.011(12) _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 2.218(2) . ? Cd1 O1 2.218(2) 11_466 ? Cd1 O1 2.218(2) 8_656 ? Cd1 O3 2.329(2) 11_466 ? Cd1 O3 2.329(2) 8_656 ? Cd1 O3 2.329(2) . ? Cd2 O2 2.259(2) 8_656 ? Cd2 O2 2.259(2) . ? Cd2 O2 2.259(2) 11_466 ? Cd2 O2 2.259(2) 23_656 ? Cd2 O2 2.259(2) 13_567 ? Cd2 O2 2.259(2) 20_466 ? O1 C1 1.247(3) . ? O2 C1 1.245(3) . ? O3 C15 1.417(4) . ? O3 H3A 0.9300 . ? N1 C9 1.341(4) . ? N1 C8 1.348(4) . ? C1 C2 1.514(4) . ? C2 C14 1.394(4) . ? C2 C3 1.396(4) . ? C3 C4 1.424(4) . ? C3 C8 1.432(4) . ? C4 C5 1.348(5) . ? C4 H4A 0.9300 . ? C5 C6 1.428(5) . ? C5 H5A 0.9300 . ? C6 C7 1.340(6) . ? C6 H6A 0.9300 . ? C7 C8 1.429(5) . ? C7 H7A 0.9300 . ? C9 C10 1.433(5) . ? C9 C14 1.435(4) . ? C10 C11 1.341(5) . ? C10 H10A 0.9300 . ? C11 C12 1.425(5) . ? C11 H11A 0.9300 . ? C12 C13 1.352(5) . ? C12 H12A 0.9300 . ? C13 C14 1.420(5) . ? C13 H13A 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 104.57(7) . 11_466 ? O1 Cd1 O1 104.57(7) . 8_656 ? O1 Cd1 O1 104.57(7) 11_466 8_656 ? O1 Cd1 O3 163.52(8) . 11_466 ? O1 Cd1 O3 82.46(8) 11_466 11_466 ? O1 Cd1 O3 87.64(8) 8_656 11_466 ? O1 Cd1 O3 87.64(8) . 8_656 ? O1 Cd1 O3 163.52(8) 11_466 8_656 ? O1 Cd1 O3 82.46(8) 8_656 8_656 ? O3 Cd1 O3 82.97(8) 11_466 8_656 ? O1 Cd1 O3 82.46(8) . . ? O1 Cd1 O3 87.64(8) 11_466 . ? O1 Cd1 O3 163.52(8) 8_656 . ? O3 Cd1 O3 82.97(8) 11_466 . ? O3 Cd1 O3 82.97(8) 8_656 . ? O2 Cd2 O2 92.84(8) 8_656 . ? O2 Cd2 O2 92.84(8) 8_656 11_466 ? O2 Cd2 O2 92.84(8) . 11_466 ? O2 Cd2 O2 87.16(8) 8_656 23_656 ? O2 Cd2 O2 87.16(8) . 23_656 ? O2 Cd2 O2 180.0 11_466 23_656 ? O2 Cd2 O2 87.16(8) 8_656 13_567 ? O2 Cd2 O2 180.0 . 13_567 ? O2 Cd2 O2 87.16(8) 11_466 13_567 ? O2 Cd2 O2 92.84(8) 23_656 13_567 ? O2 Cd2 O2 180.0 8_656 20_466 ? O2 Cd2 O2 87.16(8) . 20_466 ? O2 Cd2 O2 87.16(8) 11_466 20_466 ? O2 Cd2 O2 92.84(8) 23_656 20_466 ? O2 Cd2 O2 92.84(8) 13_567 20_466 ? C1 O1 Cd1 131.15(19) . . ? C1 O2 Cd2 134.00(19) . . ? C15 O3 Cd1 120.9(2) . . ? C15 O3 H3A 119.6 . . ? Cd1 O3 H3A 119.6 . . ? C9 N1 C8 118.9(2) . . ? O2 C1 O1 127.9(3) . . ? O2 C1 C2 118.1(2) . . ? O1 C1 C2 113.9(2) . . ? C14 C2 C3 120.3(2) . . ? C14 C2 C1 120.1(2) . . ? C3 C2 C1 119.5(2) . . ? C2 C3 C4 123.4(3) . . ? C2 C3 C8 118.0(3) . . ? C4 C3 C8 118.6(3) . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C7 C6 C5 120.9(3) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C6 C7 C8 120.7(3) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? N1 C8 C7 119.0(3) . . ? N1 C8 C3 122.4(3) . . ? C7 C8 C3 118.6(3) . . ? N1 C9 C10 118.9(3) . . ? N1 C9 C14 122.9(3) . . ? C10 C9 C14 118.2(3) . . ? C11 C10 C9 120.8(3) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 120.9(3) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 H13A 119.6 . . ? C14 C13 H13A 119.6 . . ? C2 C14 C13 123.6(3) . . ? C2 C14 C9 117.5(3) . . ? C13 C14 C9 118.9(3) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd1 O1 C1 -69.2(2) 11_466 . . . ? O1 Cd1 O1 C1 40.4(3) 8_656 . . . ? O3 Cd1 O1 C1 177.2(2) 11_466 . . . ? O3 Cd1 O1 C1 122.0(3) 8_656 . . . ? O3 Cd1 O1 C1 -154.8(3) . . . . ? O2 Cd2 O2 C1 -98.5(2) 8_656 . . . ? O2 Cd2 O2 C1 -5.5(3) 11_466 . . . ? O2 Cd2 O2 C1 174.5(3) 23_656 . . . ? O2 Cd2 O2 C1 56(100) 13_567 . . . ? O2 Cd2 O2 C1 81.5(2) 20_466 . . . ? O1 Cd1 O3 C15 56.9(3) . . . . ? O1 Cd1 O3 C15 -48.1(3) 11_466 . . . ? O1 Cd1 O3 C15 173.5(3) 8_656 . . . ? O3 Cd1 O3 C15 -130.8(3) 11_466 . . . ? O3 Cd1 O3 C15 145.5(3) 8_656 . . . ? Cd2 O2 C1 O1 68.3(4) . . . . ? Cd2 O2 C1 C2 -113.5(3) . . . . ? Cd1 O1 C1 O2 -11.5(5) . . . . ? Cd1 O1 C1 C2 170.20(19) . . . . ? O2 C1 C2 C14 101.6(3) . . . . ? O1 C1 C2 C14 -79.9(3) . . . . ? O2 C1 C2 C3 -81.3(3) . . . . ? O1 C1 C2 C3 97.2(3) . . . . ? C14 C2 C3 C4 179.5(3) . . . . ? C1 C2 C3 C4 2.4(4) . . . . ? C14 C2 C3 C8 0.6(4) . . . . ? C1 C2 C3 C8 -176.5(2) . . . . ? C2 C3 C4 C5 -178.0(3) . . . . ? C8 C3 C4 C5 1.0(5) . . . . ? C3 C4 C5 C6 -1.1(6) . . . . ? C4 C5 C6 C7 0.4(6) . . . . ? C5 C6 C7 C8 0.4(6) . . . . ? C9 N1 C8 C7 -178.7(3) . . . . ? C9 N1 C8 C3 0.5(4) . . . . ? C6 C7 C8 N1 178.7(3) . . . . ? C6 C7 C8 C3 -0.5(5) . . . . ? C2 C3 C8 N1 -0.3(4) . . . . ? C4 C3 C8 N1 -179.3(3) . . . . ? C2 C3 C8 C7 178.8(3) . . . . ? C4 C3 C8 C7 -0.2(4) . . . . ? C8 N1 C9 C10 178.1(3) . . . . ? C8 N1 C9 C14 -0.9(4) . . . . ? N1 C9 C10 C11 -178.2(3) . . . . ? C14 C9 C10 C11 0.9(5) . . . . ? C9 C10 C11 C12 -2.2(6) . . . . ? C10 C11 C12 C13 1.4(6) . . . . ? C11 C12 C13 C14 0.7(5) . . . . ? C3 C2 C14 C13 -179.9(3) . . . . ? C1 C2 C14 C13 -2.8(4) . . . . ? C3 C2 C14 C9 -0.9(4) . . . . ? C1 C2 C14 C9 176.1(2) . . . . ? C12 C13 C14 C2 177.1(3) . . . . ? C12 C13 C14 C9 -1.9(5) . . . . ? N1 C9 C14 C2 1.1(4) . . . . ? C10 C9 C14 C2 -177.9(3) . . . . ? N1 C9 C14 C13 -179.9(3) . . . . ? C10 C9 C14 C13 1.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A N1 0.93 2.17 2.749(3) 119.1 24_556 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.922 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.082 data_205 _database_code_depnum_ccdc_archive 'CCDC 228095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H85 Cd3 N6 O18.50' _chemical_formula_weight 1955.90 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 Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 20.6146(13) _cell_length_b 20.6146(13) _cell_length_c 20.6146(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8760.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1022 _cell_measurement_theta_min 2.2091 _cell_measurement_theta_max 25.5725 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3980 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8199 _exptl_absorpt_correction_T_max 0.8321 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD ' _diffrn_measurement_method 'Omig and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19668 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2987 _reflns_number_gt 2208 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0388P)^2^+2.6498P] 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 2987 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.119124(10) 0.619124(10) 0.880876(10) 0.03066(12) Uani 1 3 d S A . Cd2 Cd 0.0000 0.5000 1.0000 0.02658(13) Uani 1 6 d S . . N1 N -0.20350(13) 0.59668(16) 0.75502(15) 0.0563(8) Uani 1 1 d . . . C1 C -0.02230(15) 0.56011(15) 0.85482(14) 0.0344(7) Uani 1 1 d . . . C2 C -0.08663(14) 0.57132(15) 0.82088(14) 0.0355(7) Uani 1 1 d . . . C3 C -0.10177(15) 0.53723(16) 0.76499(16) 0.0413(8) Uani 1 1 d . . . C4 C -0.06080(18) 0.48952(18) 0.73737(19) 0.0571(10) Uani 1 1 d . . . H4A H -0.0216 0.4798 0.7575 0.069 Uiso 1 1 calc R . . C5 C -0.0774(2) 0.4579(2) 0.6825(2) 0.0752(13) Uani 1 1 d . . . H5A H -0.0493 0.4276 0.6645 0.090 Uiso 1 1 calc R . . C6 C -0.1384(2) 0.4709(3) 0.6521(2) 0.0830(14) Uani 1 1 d . . . H6A H -0.1500 0.4483 0.6149 0.100 Uiso 1 1 calc R . . C7 C -0.1790(2) 0.5154(2) 0.6766(2) 0.0707(12) Uani 1 1 d . . . H7A H -0.2185 0.5229 0.6562 0.085 Uiso 1 1 calc R . . C8 C -0.16279(17) 0.55135(19) 0.73344(17) 0.0507(9) Uani 1 1 d . . . C9 C -0.18768(16) 0.63022(18) 0.80890(17) 0.0471(8) Uani 1 1 d . . . C10 C -0.22938(19) 0.6803(2) 0.8303(2) 0.0662(11) Uani 1 1 d . . . H10A H -0.2668 0.6896 0.8069 0.079 Uiso 1 1 calc R . . C11 C -0.2155(2) 0.7145(2) 0.8840(2) 0.0733(12) Uani 1 1 d . . . H11A H -0.2432 0.7477 0.8968 0.088 Uiso 1 1 calc R . . C12 C -0.1600(2) 0.7010(2) 0.9210(2) 0.0648(11) Uani 1 1 d . . . H12A H -0.1517 0.7247 0.9585 0.078 Uiso 1 1 calc R . . C13 C -0.11879(17) 0.65417(18) 0.90252(17) 0.0488(8) Uani 1 1 d . . . H13A H -0.0825 0.6452 0.9278 0.059 Uiso 1 1 calc R . . C14 C -0.12974(14) 0.61791(15) 0.84469(15) 0.0386(7) Uani 1 1 d . . . C15 C 0.1381(5) 0.5753(5) 0.7251(4) 0.069(2) Uani 0.50 1 d P A 1 H15A H 0.1596 0.5954 0.6884 0.082 Uiso 0.50 1 calc PR A 1 H15B H 0.0929 0.5882 0.7234 0.082 Uiso 0.50 1 calc PR A 1 C16 C 0.1409(10) 0.5028(8) 0.7155(14) 0.135(9) Uani 0.50 1 d P A 1 H16A H 0.1211 0.4917 0.6748 0.202 Uiso 0.50 1 calc PR A 1 H16B H 0.1182 0.4816 0.7501 0.202 Uiso 0.50 1 calc PR A 1 H16C H 0.1854 0.4889 0.7153 0.202 Uiso 0.50 1 calc PR A 1 C16' C 0.124(2) 0.5317(14) 0.7033(18) 0.37(3) Uani 0.50 1 d P A 2 H16D H 0.1147 0.4900 0.6849 0.551 Uiso 0.50 1 calc PR A 2 H16E H 0.1546 0.5542 0.6758 0.551 Uiso 0.50 1 calc PR A 2 H16F H 0.0853 0.5566 0.7070 0.551 Uiso 0.50 1 calc PR A 2 C15' C 0.1462(8) 0.5251(9) 0.7518(7) 0.097(4) Uani 0.50 1 d P A 2 H15C H 0.1853 0.4991 0.7491 0.116 Uiso 0.50 1 calc PR A 2 H15D H 0.1158 0.5038 0.7808 0.116 Uiso 0.50 1 calc PR A 2 O1 O -0.01830(11) 0.51370(11) 0.89277(10) 0.0469(6) Uani 1 1 d . . . O2 O 0.02128(11) 0.59867(13) 0.83930(12) 0.0548(7) Uani 1 1 d . . . O3 O 0.16341(14) 0.60011(16) 0.77854(12) 0.0638(8) Uani 1 1 d . . . H3 H 0.1994(17) 0.6049(17) 0.7747(17) 0.041(11) Uiso 1 1 d . . . O1W O 0.0211(12) 0.4789(12) 0.5211(12) 0.18(2) Uani 0.25 3 d SP . . 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 0.03066(12) 0.03066(12) 0.03066(12) 0.00158(9) 0.00158(9) -0.00158(9) Cd2 0.02658(13) 0.02658(13) 0.02658(13) 0.00031(12) 0.00031(12) -0.00031(12) N1 0.0370(16) 0.079(2) 0.0529(19) 0.0077(17) -0.0128(15) 0.0081(16) C1 0.0362(17) 0.0403(18) 0.0268(16) -0.0040(14) -0.0012(13) 0.0026(14) C2 0.0313(16) 0.0424(18) 0.0327(16) 0.0093(14) -0.0031(13) -0.0066(14) C3 0.0351(17) 0.051(2) 0.0383(18) 0.0039(16) -0.0052(14) -0.0043(15) C4 0.051(2) 0.059(2) 0.060(2) -0.0104(19) -0.0136(18) 0.0059(18) C5 0.073(3) 0.083(3) 0.070(3) -0.032(2) -0.012(2) 0.009(2) C6 0.081(3) 0.107(4) 0.061(3) -0.029(3) -0.022(3) -0.010(3) C7 0.056(2) 0.104(4) 0.052(2) -0.008(2) -0.020(2) -0.007(2) C8 0.043(2) 0.069(2) 0.041(2) 0.0034(18) -0.0075(16) -0.0047(18) C9 0.0375(18) 0.056(2) 0.048(2) 0.0077(17) -0.0017(16) 0.0073(16) C10 0.050(2) 0.077(3) 0.072(3) 0.010(2) -0.007(2) 0.021(2) C11 0.070(3) 0.069(3) 0.082(3) -0.002(2) 0.009(2) 0.027(2) C12 0.069(3) 0.064(3) 0.062(3) -0.006(2) 0.006(2) 0.012(2) C13 0.044(2) 0.059(2) 0.0432(19) -0.0001(17) 0.0005(16) 0.0025(18) C14 0.0325(17) 0.0465(18) 0.0368(17) 0.0096(14) 0.0005(13) -0.0017(14) C15 0.085(6) 0.076(7) 0.045(5) -0.010(5) -0.005(4) 0.007(5) C16 0.135(12) 0.073(10) 0.20(2) -0.068(12) 0.060(15) -0.020(9) C16' 0.62(6) 0.16(3) 0.32(4) -0.12(3) -0.30(4) 0.08(3) C15' 0.121(10) 0.077(10) 0.092(9) -0.014(8) 0.008(8) -0.002(8) O1 0.0580(15) 0.0489(14) 0.0337(12) 0.0038(10) -0.0123(11) 0.0066(11) O2 0.0354(13) 0.0753(17) 0.0537(15) 0.0125(13) -0.0087(11) -0.0106(12) O3 0.0430(16) 0.105(2) 0.0439(16) -0.0122(14) 0.0078(13) 0.0053(16) O1W 0.18(2) 0.18(2) 0.18(2) -0.05(2) 0.05(2) -0.05(2) _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 2.232(2) . ? Cd1 O2 2.232(2) 8_656 ? Cd1 O2 2.232(2) 11_466 ? Cd1 O3 2.332(3) 11_466 ? Cd1 O3 2.332(3) 8_656 ? Cd1 O3 2.332(3) . ? Cd2 O1 2.260(2) 23_656 ? Cd2 O1 2.260(2) 8_656 ? Cd2 O1 2.260(2) . ? Cd2 O1 2.260(2) 11_466 ? Cd2 O1 2.260(2) 13_567 ? Cd2 O1 2.260(2) 20_466 ? N1 C8 1.332(5) . ? N1 C9 1.348(5) . ? C1 O1 1.239(4) . ? C1 O2 1.242(4) . ? C1 C2 1.517(4) . ? C2 C3 1.385(4) . ? C2 C14 1.397(4) . ? C3 C4 1.416(5) . ? C3 C8 1.446(5) . ? C4 C5 1.349(5) . ? C4 H4A 0.9300 . ? C5 C6 1.430(6) . ? C5 H5A 0.9300 . ? C6 C7 1.340(6) . ? C6 H6A 0.9300 . ? C7 C8 1.426(5) . ? C7 H7A 0.9300 . ? C9 C10 1.414(5) . ? C9 C14 1.427(4) . ? C10 C11 1.343(6) . ? C10 H10A 0.9300 . ? C11 C12 1.403(6) . ? C11 H11A 0.9300 . ? C12 C13 1.341(5) . ? C12 H12A 0.9300 . ? C13 C14 1.425(5) . ? C13 H13A 0.9300 . ? C15 O3 1.322(9) . ? C15 C16 1.509(18) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C16' C15' 1.10(3) . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C15' O3 1.680(16) . ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? O3 H3 0.75(4) . ? O1W O1W 1.50(9) 13_566 ? 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 O2 104.41(7) . 8_656 ? O2 Cd1 O2 104.41(7) . 11_466 ? O2 Cd1 O2 104.41(7) 8_656 11_466 ? O2 Cd1 O3 82.45(10) . 11_466 ? O2 Cd1 O3 162.97(10) 8_656 11_466 ? O2 Cd1 O3 88.55(10) 11_466 11_466 ? O2 Cd1 O3 162.97(10) . 8_656 ? O2 Cd1 O3 88.55(10) 8_656 8_656 ? O2 Cd1 O3 82.45(10) 11_466 8_656 ? O3 Cd1 O3 82.17(12) 11_466 8_656 ? O2 Cd1 O3 88.55(10) . . ? O2 Cd1 O3 82.45(10) 8_656 . ? O2 Cd1 O3 162.97(11) 11_466 . ? O3 Cd1 O3 82.17(12) 11_466 . ? O3 Cd1 O3 82.17(12) 8_656 . ? O1 Cd2 O1 86.45(8) 23_656 8_656 ? O1 Cd2 O1 86.45(8) 23_656 . ? O1 Cd2 O1 93.55(8) 8_656 . ? O1 Cd2 O1 180.0 23_656 11_466 ? O1 Cd2 O1 93.55(8) 8_656 11_466 ? O1 Cd2 O1 93.55(8) . 11_466 ? O1 Cd2 O1 93.55(8) 23_656 13_567 ? O1 Cd2 O1 86.45(8) 8_656 13_567 ? O1 Cd2 O1 180.0 . 13_567 ? O1 Cd2 O1 86.45(8) 11_466 13_567 ? O1 Cd2 O1 93.55(8) 23_656 20_466 ? O1 Cd2 O1 180.000(1) 8_656 20_466 ? O1 Cd2 O1 86.45(8) . 20_466 ? O1 Cd2 O1 86.45(8) 11_466 20_466 ? O1 Cd2 O1 93.55(8) 13_567 20_466 ? C8 N1 C9 118.8(3) . . ? O1 C1 O2 127.5(3) . . ? O1 C1 C2 117.8(3) . . ? O2 C1 C2 114.6(3) . . ? C3 C2 C14 119.8(3) . . ? C3 C2 C1 120.2(3) . . ? C14 C2 C1 119.9(3) . . ? C2 C3 C4 123.5(3) . . ? C2 C3 C8 117.9(3) . . ? C4 C3 C8 118.5(3) . . ? C5 C4 C3 121.4(4) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 120.0(4) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C7 C6 C5 120.8(4) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C6 C7 C8 121.2(4) . . ? C6 C7 H7A 119.4 . . ? C8 C7 H7A 119.4 . . ? N1 C8 C7 119.4(3) . . ? N1 C8 C3 122.6(3) . . ? C7 C8 C3 118.0(4) . . ? N1 C9 C10 118.9(3) . . ? N1 C9 C14 122.5(3) . . ? C10 C9 C14 118.5(3) . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 121.1(4) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C13 C12 C11 120.4(4) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C14 121.0(3) . . ? C12 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C2 C14 C13 123.6(3) . . ? C2 C14 C9 118.2(3) . . ? C13 C14 C9 118.2(3) . . ? O3 C15 C16 118.5(15) . . ? O3 C15 H15A 107.7 . . ? C16 C15 H15A 107.7 . . ? O3 C15 H15B 107.7 . . ? C16 C15 H15B 107.7 . . ? H15A C15 H15B 107.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C16' C15' O3 106(2) . . ? C16' C15' H15C 110.6 . . ? O3 C15' H15C 110.6 . . ? C16' C15' H15D 110.6 . . ? O3 C15' H15D 110.6 . . ? H15C C15' H15D 108.8 . . ? C1 O1 Cd2 136.5(2) . . ? C1 O2 Cd1 132.5(2) . . ? C15 O3 C15' 44.5(7) . . ? C15 O3 Cd1 131.6(5) . . ? C15' O3 Cd1 111.6(5) . . ? C15 O3 H3 111(3) . . ? C15' O3 H3 107(3) . . ? Cd1 O3 H3 117(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -83.5(4) . . . . ? O2 C1 C2 C3 94.7(4) . . . . ? O1 C1 C2 C14 98.9(3) . . . . ? O2 C1 C2 C14 -82.9(4) . . . . ? C14 C2 C3 C4 179.7(3) . . . . ? C1 C2 C3 C4 2.0(5) . . . . ? C14 C2 C3 C8 -0.4(4) . . . . ? C1 C2 C3 C8 -178.0(3) . . . . ? C2 C3 C4 C5 -179.5(4) . . . . ? C8 C3 C4 C5 0.5(6) . . . . ? C3 C4 C5 C6 -1.8(7) . . . . ? C4 C5 C6 C7 1.4(8) . . . . ? C5 C6 C7 C8 0.3(8) . . . . ? C9 N1 C8 C7 179.8(3) . . . . ? C9 N1 C8 C3 -0.9(5) . . . . ? C6 C7 C8 N1 177.7(4) . . . . ? C6 C7 C8 C3 -1.6(6) . . . . ? C2 C3 C8 N1 1.9(5) . . . . ? C4 C3 C8 N1 -178.1(3) . . . . ? C2 C3 C8 C7 -178.8(3) . . . . ? C4 C3 C8 C7 1.2(5) . . . . ? C8 N1 C9 C10 177.2(3) . . . . ? C8 N1 C9 C14 -1.6(5) . . . . ? N1 C9 C10 C11 179.6(4) . . . . ? C14 C9 C10 C11 -1.5(6) . . . . ? C9 C10 C11 C12 -1.0(7) . . . . ? C10 C11 C12 C13 1.3(7) . . . . ? C11 C12 C13 C14 1.1(6) . . . . ? C3 C2 C14 C13 178.6(3) . . . . ? C1 C2 C14 C13 -3.8(5) . . . . ? C3 C2 C14 C9 -1.9(4) . . . . ? C1 C2 C14 C9 175.7(3) . . . . ? C12 C13 C14 C2 175.9(3) . . . . ? C12 C13 C14 C9 -3.6(5) . . . . ? N1 C9 C14 C2 3.1(5) . . . . ? C10 C9 C14 C2 -175.8(3) . . . . ? N1 C9 C14 C13 -177.4(3) . . . . ? C10 C9 C14 C13 3.7(5) . . . . ? O2 C1 O1 Cd2 65.0(5) . . . . ? C2 C1 O1 Cd2 -117.1(3) . . . . ? O1 Cd2 O1 C1 177.9(3) 23_656 . . . ? O1 Cd2 O1 C1 -95.9(3) 8_656 . . . ? O1 Cd2 O1 C1 -2.1(3) 11_466 . . . ? O1 Cd2 O1 C1 51(86) 13_567 . . . ? O1 Cd2 O1 C1 84.1(3) 20_466 . . . ? O1 C1 O2 Cd1 -13.3(5) . . . . ? C2 C1 O2 Cd1 168.7(2) . . . . ? O2 Cd1 O2 C1 43.5(3) 8_656 . . . ? O2 Cd1 O2 C1 -65.9(3) 11_466 . . . ? O3 Cd1 O2 C1 -152.4(3) 11_466 . . . ? O3 Cd1 O2 C1 -177.9(3) 8_656 . . . ? O3 Cd1 O2 C1 125.3(3) . . . . ? C16 C15 O3 C15' -10.1(12) . . . . ? C16 C15 O3 Cd1 -88.5(11) . . . . ? C16' C15' O3 C15 -1(3) . . . . ? C16' C15' O3 Cd1 127(3) . . . . ? O2 Cd1 O3 C15 -11.2(7) . . . . ? O2 Cd1 O3 C15 93.6(7) 8_656 . . . ? O2 Cd1 O3 C15 -151.3(7) 11_466 . . . ? O3 Cd1 O3 C15 -93.7(7) 11_466 . . . ? O3 Cd1 O3 C15 -176.8(7) 8_656 . . . ? O2 Cd1 O3 C15' -58.8(7) . . . . ? O2 Cd1 O3 C15' 46.0(7) 8_656 . . . ? O2 Cd1 O3 C15' 161.1(7) 11_466 . . . ? O3 Cd1 O3 C15' -141.4(7) 11_466 . . . ? O3 Cd1 O3 C15' 135.5(7) 8_656 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 N1 0.75(4) 2.10(4) 2.830(4) 164(4) 14_657 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.511 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.067