# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email lfelipe@unam.mx _publ_contact_author_name 'Dr Luis del Castillo Davila' loop_ _publ_author_name 'Vera-Cruz, Paula' 'Toscano, Ruben' 'Balmaseda, Jorge' 'Basterrechea, Mario' 'Nino, Netzahualcoyotl' 'del Castillo Davila, Luis' _publ_section_title ; Synthesis and crystal structure of three new cadmium tartrates with open frameworks ; # Attachment '- Compound_I.cif' data_Compound_I _database_code_depnum_ccdc_archive 'CCDC 872860' #TrackingRef '- Compound_I.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration rmad _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 Cd3 O19, H2 O' _chemical_formula_sum 'C12 H16 Cd3 O20' _chemical_formula_weight 817.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' 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' _cell_length_a 6.4001(3) _cell_length_b 17.2148(9) _cell_length_c 18.6406(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2053.76(18) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9092 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 25.30 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.074 _exptl_crystal_size_mid 0.116 _exptl_crystal_size_max 0.492 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 3.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4117 _exptl_absorpt_correction_T_max 0.7985 _exptl_absorpt_process_details '(Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Apex CCD diffractometer 01-670-01' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 0.661 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16295 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.33 _reflns_number_total 3729 _reflns_number_gt 3679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 7.34A (Bruker, 2006)' _computing_structure_solution 'SIR2008 (Burla et. al., 2007)' _computing_structure_refinement 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _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^)+(0.0145P)^2^+2.7909P] 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 0.01(2) _refine_ls_number_reflns 3729 _refine_ls_number_parameters 340 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0177 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0400 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.069 _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 0.08671(4) 0.489785(14) 0.220983(14) 0.02287(7) Uani 1 1 d . . . Cd2 Cd 0.94016(4) 0.244553(15) 0.379516(14) 0.02323(7) Uani 1 1 d . . . Cd3 Cd 0.35892(5) 0.591980(16) 0.493636(15) 0.03143(8) Uani 1 1 d . . . O1 O 0.2261(4) 0.42787(15) 0.11793(14) 0.0275(6) Uani 1 1 d . . . O2 O 0.4166(6) 0.34155(19) 0.06071(16) 0.0508(9) Uani 1 1 d . . . O3 O 0.4267(5) 0.41090(16) 0.24339(13) 0.0305(6) Uani 1 1 d D . . H3A H 0.445(8) 0.398(3) 0.2871(9) 0.046 Uiso 1 1 d D . . O4 O 0.7806(5) 0.43720(16) 0.15923(15) 0.0307(6) Uani 1 1 d D . . H4 H 0.668(4) 0.458(3) 0.173(3) 0.046 Uiso 1 1 d D . . O5 O 0.7695(4) 0.27427(15) 0.27775(15) 0.0312(6) Uani 1 1 d . . . O6 O 0.9824(4) 0.37605(15) 0.27192(14) 0.0286(6) Uani 1 1 d . . . O7 O 0.2194(4) 0.53658(15) 0.32708(14) 0.0285(6) Uani 1 1 d . . . O8 O 0.3805(4) 0.63523(15) 0.38263(14) 0.0304(6) Uani 1 1 d . . . O9 O 0.3999(4) 0.57091(14) 0.19944(13) 0.0249(6) Uani 1 1 d D . . H9 H 0.393(8) 0.598(2) 0.1619(14) 0.037 Uiso 1 1 d D . . O10 O 0.7561(4) 0.53564(15) 0.28585(15) 0.0301(6) Uani 1 1 d D . . H10A H 0.776(8) 0.532(3) 0.3305(7) 0.045 Uiso 1 1 d D . . O11 O 0.7654(5) 0.71447(16) 0.18568(16) 0.0348(7) Uani 1 1 d . . . O12 O 0.9625(4) 0.60786(15) 0.17824(14) 0.0304(6) Uani 1 1 d . . . O13 O 1.1360(4) 0.26863(16) 0.47961(14) 0.0334(6) Uani 1 1 d . . . O14 O 1.1736(5) 0.33321(15) 0.58191(14) 0.0299(6) Uani 1 1 d . . . O15 O 0.8456(4) 0.36408(15) 0.42886(14) 0.0287(6) Uani 1 1 d D . . H15 H 0.721(3) 0.372(3) 0.415(2) 0.043 Uiso 1 1 d D . . O16 O 1.1636(4) 0.47946(17) 0.46732(15) 0.0340(7) Uani 1 1 d D . . H16 H 1.137(8) 0.475(3) 0.4232(8) 0.051 Uiso 1 1 d D . . O17 O 0.6352(4) 0.51856(18) 0.52161(18) 0.0456(8) Uani 1 1 d . . . O18 O 0.8186(7) 0.5584(2) 0.4294(2) 0.0735(13) Uani 1 1 d . . . O19 O 0.5938(6) 0.69646(18) 0.51285(17) 0.0483(8) Uani 1 1 d D . . H19A H 0.544(7) 0.736(2) 0.491(2) 0.073 Uiso 1 1 d D . . H19B H 0.699(6) 0.682(3) 0.488(2) 0.073 Uiso 1 1 d D . . O20 O 0.4453(5) 0.3662(2) 0.38971(17) 0.0524(9) Uani 1 1 d D . . H20A H 0.4244 0.3178 0.3827 0.079 Uiso 1 1 d RD . . H20B H 0.3698 0.3737 0.4268 0.079 Uiso 1 1 d RD . . C1 C 0.3662(6) 0.3761(2) 0.1181(2) 0.0254(8) Uani 1 1 d . . . C2 C 0.4832(6) 0.3560(2) 0.1883(2) 0.0250(8) Uani 1 1 d . . . H2 H 0.4434 0.3037 0.2037 0.030 Uiso 1 1 calc R . . C3 C 0.7214(6) 0.3593(2) 0.1781(2) 0.0237(8) Uani 1 1 d . . . H3 H 0.7623 0.3238 0.1395 0.028 Uiso 1 1 calc R . . C4 C 0.8353(6) 0.3359(2) 0.24839(19) 0.0215(7) Uani 1 1 d . . . C5 C 0.3418(6) 0.5942(2) 0.32795(19) 0.0218(7) Uani 1 1 d . . . C6 C 0.4569(6) 0.6195(2) 0.25910(18) 0.0216(8) Uani 1 1 d . . . H6 H 0.4195 0.6733 0.2480 0.026 Uiso 1 1 calc R . . C7 C 0.6958(5) 0.6144(2) 0.2712(2) 0.0218(8) Uani 1 1 d . . . H7 H 0.7309 0.6460 0.3132 0.026 Uiso 1 1 calc R . . C8 C 0.8151(5) 0.6468(2) 0.20667(19) 0.0223(8) Uani 1 1 d . . . C9 C 1.0856(6) 0.32234(19) 0.52190(18) 0.0219(7) Uani 1 1 d . . . C10 C 0.9074(5) 0.37881(18) 0.50129(18) 0.0207(7) Uani 1 1 d . . . H10 H 0.7879 0.3700 0.5331 0.025 Uiso 1 1 calc R . . C11 C 0.9782(6) 0.4645(2) 0.5078(2) 0.0240(8) Uani 1 1 d . . . H11 H 1.0086 0.4751 0.5585 0.029 Uiso 1 1 calc R . . C12 C 0.8004(7) 0.5185(2) 0.4842(2) 0.0303(9) 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 0.01950(12) 0.02592(13) 0.02318(13) 0.00119(10) 0.00011(11) -0.00244(10) Cd2 0.02281(13) 0.02760(13) 0.01929(13) -0.00450(10) -0.00132(11) 0.00315(12) Cd3 0.04096(17) 0.02977(14) 0.02357(14) -0.00049(12) 0.01086(13) -0.00556(12) O1 0.0241(13) 0.0365(14) 0.0220(13) 0.0021(11) -0.0068(12) 0.0054(11) O2 0.061(2) 0.0585(19) 0.0326(16) -0.0164(15) -0.0190(17) 0.0234(19) O3 0.0303(14) 0.0425(15) 0.0187(12) 0.0009(12) 0.0008(12) 0.0061(14) O4 0.0333(16) 0.0322(15) 0.0266(15) 0.0106(12) -0.0014(13) -0.0031(13) O5 0.0325(14) 0.0283(14) 0.0327(15) 0.0102(12) -0.0091(13) -0.0081(11) O6 0.0244(13) 0.0339(14) 0.0275(14) 0.0059(11) -0.0080(12) -0.0072(11) O7 0.0283(15) 0.0348(15) 0.0225(13) 0.0018(11) 0.0052(12) -0.0092(12) O8 0.0327(16) 0.0366(14) 0.0219(13) -0.0030(12) 0.0016(12) -0.0060(12) O9 0.0276(14) 0.0314(13) 0.0158(12) 0.0023(10) 0.0015(11) -0.0017(12) O10 0.0278(13) 0.0328(14) 0.0295(15) 0.0120(13) 0.0012(14) 0.0066(12) O11 0.0287(15) 0.0338(15) 0.0420(17) 0.0152(13) 0.0083(13) -0.0014(13) O12 0.0256(15) 0.0368(15) 0.0288(14) 0.0050(12) 0.0092(12) 0.0023(12) O13 0.0320(15) 0.0378(15) 0.0304(15) -0.0098(12) -0.0085(12) 0.0103(12) O14 0.0352(16) 0.0351(15) 0.0194(13) -0.0050(11) -0.0090(12) 0.0031(12) O15 0.0296(14) 0.0318(14) 0.0246(14) -0.0034(11) -0.0079(12) 0.0041(12) O16 0.0277(14) 0.0395(16) 0.0347(16) -0.0065(13) 0.0108(13) -0.0097(13) O17 0.0276(15) 0.0488(18) 0.060(2) 0.0161(16) 0.0010(15) 0.0031(14) O18 0.080(3) 0.084(3) 0.056(2) 0.034(2) 0.028(2) 0.043(2) O19 0.062(2) 0.0395(17) 0.0431(19) 0.0047(14) -0.0064(18) -0.0103(16) O20 0.0392(19) 0.080(2) 0.0385(18) 0.0105(17) 0.0057(16) 0.0138(18) C1 0.0230(19) 0.0270(18) 0.0264(19) -0.0022(15) -0.0050(17) -0.0016(15) C2 0.026(2) 0.0225(18) 0.026(2) 0.0000(15) -0.0090(16) -0.0010(15) C3 0.026(2) 0.0266(19) 0.0189(18) -0.0010(15) -0.0025(15) -0.0013(16) C4 0.0181(17) 0.0251(18) 0.0214(18) -0.0005(14) -0.0002(15) 0.0049(15) C5 0.0175(17) 0.0266(18) 0.0211(18) 0.0018(15) 0.0001(14) 0.0061(15) C6 0.0240(19) 0.0200(16) 0.0207(18) 0.0006(13) 0.0009(15) -0.0017(15) C7 0.0189(18) 0.0263(18) 0.0201(19) 0.0016(15) 0.0000(14) -0.0011(14) C8 0.0155(17) 0.0299(19) 0.0214(19) 0.0015(15) -0.0021(15) -0.0048(14) C9 0.0205(17) 0.0239(17) 0.0213(18) 0.0008(14) 0.0032(15) -0.0048(15) C10 0.0217(17) 0.0234(16) 0.0169(16) -0.0009(13) 0.0014(16) -0.0015(14) C11 0.0285(19) 0.0272(18) 0.0164(17) -0.0033(14) 0.0041(16) -0.0038(14) C12 0.050(3) 0.0256(19) 0.0157(18) -0.0019(15) 0.0058(17) 0.0037(17) _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 2.276(3) 1_455 ? Cd1 O7 2.298(3) . ? Cd1 O12 2.323(3) 1_455 ? Cd1 O1 2.371(3) . ? Cd1 O4 2.446(3) 1_455 ? Cd1 O9 2.476(3) . ? Cd1 O10 2.562(3) 1_455 ? Cd1 O3 2.599(3) . ? Cd2 O5 2.248(3) . ? Cd2 O14 2.285(3) 4_456 ? Cd2 O13 2.286(3) . ? Cd2 O11 2.302(3) 3_745 ? Cd2 O15 2.334(3) . ? Cd3 O8 2.203(3) . ? Cd3 O17 2.235(3) . ? Cd3 O16 2.357(3) 1_455 ? Cd3 O19 2.371(3) . ? Cd3 O1 2.404(3) 2_565 ? Cd3 O2 2.446(3) 2_565 ? O1 C1 1.264(4) . ? O1 Cd3 2.404(3) 2_564 ? O2 C1 1.266(5) . ? O2 Cd3 2.446(3) 2_564 ? O3 C2 1.441(5) . ? O4 C3 1.437(5) . ? O4 Cd1 2.446(3) 1_655 ? O5 C4 1.266(4) . ? O6 C4 1.248(4) . ? O6 Cd1 2.276(3) 1_655 ? O7 C5 1.263(4) . ? O8 C5 1.265(4) . ? O9 C6 1.438(4) . ? O10 C7 1.436(4) . ? O10 Cd1 2.562(3) 1_655 ? O11 C8 1.269(5) . ? O11 Cd2 2.302(3) 3_755 ? O12 C8 1.273(4) . ? O12 Cd1 2.323(3) 1_655 ? O13 C9 1.257(4) . ? O14 C9 1.266(4) . ? O14 Cd2 2.285(3) 4_556 ? O15 C10 1.430(4) . ? O16 C11 1.430(4) . ? O16 Cd3 2.357(3) 1_655 ? O17 C12 1.266(5) . ? O18 C12 1.238(5) . ? C1 C2 1.547(5) . ? C2 C3 1.537(5) . ? C3 C4 1.553(5) . ? C5 C6 1.543(5) . ? C6 C7 1.548(5) . ? C7 C8 1.530(5) . ? C9 C10 1.547(5) . ? C10 C11 1.548(4) . ? C11 C12 1.534(5) . ? 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 O7 92.92(9) 1_455 . ? O6 Cd1 O12 142.68(10) 1_455 1_455 ? O7 Cd1 O12 96.59(10) . 1_455 ? O6 Cd1 O1 93.54(9) 1_455 . ? O7 Cd1 O1 135.71(10) . . ? O12 Cd1 O1 104.14(9) 1_455 . ? O6 Cd1 O4 69.09(9) 1_455 1_455 ? O7 Cd1 O4 146.16(10) . 1_455 ? O12 Cd1 O4 83.59(9) 1_455 1_455 ? O1 Cd1 O4 75.74(9) . 1_455 ? O6 Cd1 O9 142.22(9) 1_455 . ? O7 Cd1 O9 69.07(8) . . ? O12 Cd1 O9 74.21(9) 1_455 . ? O1 Cd1 O9 79.49(9) . . ? O4 Cd1 O9 141.34(8) 1_455 . ? O6 Cd1 O10 79.97(9) 1_455 1_455 ? O7 Cd1 O10 77.93(10) . 1_455 ? O12 Cd1 O10 67.02(8) 1_455 1_455 ? O1 Cd1 O10 146.27(9) . 1_455 ? O4 Cd1 O10 71.01(10) 1_455 1_455 ? O9 Cd1 O10 124.85(9) . 1_455 ? O6 Cd1 O3 74.28(9) 1_455 . ? O7 Cd1 O3 74.67(9) . . ? O12 Cd1 O3 143.01(9) 1_455 . ? O1 Cd1 O3 65.18(8) . . ? O4 Cd1 O3 123.57(9) 1_455 . ? O9 Cd1 O3 69.08(9) . . ? O10 Cd1 O3 140.97(8) 1_455 . ? O5 Cd2 O14 92.07(10) . 4_456 ? O5 Cd2 O13 156.07(9) . . ? O14 Cd2 O13 105.00(10) 4_456 . ? O5 Cd2 O11 90.20(11) . 3_745 ? O14 Cd2 O11 130.23(10) 4_456 3_745 ? O13 Cd2 O11 91.31(10) . 3_745 ? O5 Cd2 O15 90.34(10) . . ? O14 Cd2 O15 101.48(10) 4_456 . ? O13 Cd2 O15 70.15(9) . . ? O11 Cd2 O15 128.23(10) 3_745 . ? O8 Cd3 O17 111.14(11) . . ? O8 Cd3 O16 96.63(10) . 1_455 ? O17 Cd3 O16 90.19(11) . 1_455 ? O8 Cd3 O19 81.13(10) . . ? O17 Cd3 O19 83.81(12) . . ? O16 Cd3 O19 172.31(12) 1_455 . ? O8 Cd3 O1 165.27(9) . 2_565 ? O17 Cd3 O1 82.75(10) . 2_565 ? O16 Cd3 O1 87.92(9) 1_455 2_565 ? O19 Cd3 O1 96.07(10) . 2_565 ? O8 Cd3 O2 111.54(10) . 2_565 ? O17 Cd3 O2 135.69(12) . 2_565 ? O16 Cd3 O2 96.23(11) 1_455 2_565 ? O19 Cd3 O2 91.43(13) . 2_565 ? O1 Cd3 O2 53.89(9) 2_565 2_565 ? C1 O1 Cd1 125.6(2) . . ? C1 O1 Cd3 93.6(2) . 2_564 ? Cd1 O1 Cd3 139.41(11) . 2_564 ? C1 O2 Cd3 91.6(2) . 2_564 ? C2 O3 Cd1 116.0(2) . . ? C3 O4 Cd1 116.2(2) . 1_655 ? C4 O5 Cd2 113.2(2) . . ? C4 O6 Cd1 123.4(2) . 1_655 ? C5 O7 Cd1 121.0(2) . . ? C5 O8 Cd3 123.7(2) . . ? C6 O9 Cd1 114.07(19) . . ? C7 O10 Cd1 115.0(2) . 1_655 ? C8 O11 Cd2 99.4(2) . 3_755 ? C8 O12 Cd1 124.9(2) . 1_655 ? C9 O13 Cd2 120.3(2) . . ? C9 O14 Cd2 121.6(2) . 4_556 ? C10 O15 Cd2 117.2(2) . . ? C11 O16 Cd3 118.6(2) . 1_655 ? C12 O17 Cd3 122.2(3) . . ? O1 C1 O2 120.7(3) . . ? O1 C1 C2 120.2(3) . . ? O2 C1 C2 119.1(3) . . ? O3 C2 C3 108.2(3) . . ? O3 C2 C1 109.6(3) . . ? C3 C2 C1 111.5(3) . . ? O4 C3 C2 109.0(3) . . ? O4 C3 C4 109.0(3) . . ? C2 C3 C4 110.6(3) . . ? O6 C4 O5 124.3(3) . . ? O6 C4 C3 120.5(3) . . ? O5 C4 C3 115.2(3) . . ? O7 C5 O8 124.8(3) . . ? O7 C5 C6 120.5(3) . . ? O8 C5 C6 114.8(3) . . ? O9 C6 C5 111.0(3) . . ? O9 C6 C7 109.3(3) . . ? C5 C6 C7 109.6(3) . . ? O10 C7 C8 111.1(3) . . ? O10 C7 C6 110.2(3) . . ? C8 C7 C6 111.0(3) . . ? O11 C8 O12 122.8(3) . . ? O11 C8 C7 116.9(3) . . ? O12 C8 C7 120.3(3) . . ? O13 C9 O14 123.3(3) . . ? O13 C9 C10 119.7(3) . . ? O14 C9 C10 117.0(3) . . ? O15 C10 C9 109.1(3) . . ? O15 C10 C11 108.9(3) . . ? C9 C10 C11 111.3(3) . . ? O16 C11 C12 110.8(3) . . ? O16 C11 C10 111.9(3) . . ? C12 C11 C10 109.7(3) . . ? O18 C12 O17 122.2(4) . . ? O18 C12 C11 120.2(4) . . ? O17 C12 C11 117.6(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 C1 C2 C3 C4 -177.8(3) . . . . ? C5 C6 C7 C8 -174.3(3) . . . . ? C9 C10 C11 C12 177.8(3) . . . . ? O3 C2 C3 O4 -58.2(4) . . . . ? O9 C6 C7 O10 -59.6(4) . . . . ? O15 C10 C11 O16 -65.9(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 O20 0.850(10) 1.992(13) 2.836(4) 172(5) . O4 H4 O3 0.847(10) 2.17(4) 2.792(4) 130(4) . O4 H4 O9 0.847(10) 2.64(2) 3.435(4) 157(4) . O9 H9 O14 0.845(10) 1.949(14) 2.783(3) 169(5) 2_664 O10 H10A O18 0.845(10) 1.918(18) 2.733(5) 162(5) . O15 H15 O20 0.850(10) 1.828(15) 2.664(4) 167(5) . O16 H16 O7 0.844(10) 2.15(4) 2.816(4) 136(4) 1_655 O19 H19A O2 0.855(10) 2.07(3) 2.850(4) 151(5) 3_655 O19 H19B O18 0.851(10) 2.51(4) 3.184(5) 137(5) . O20 H20A O11 0.85 2.50 3.258(5) 147.9 3_645 O20 H20B O16 0.85 2.37 3.024(4) 133.6 1_455 O20 H20B O13 0.85 2.55 3.090(4) 122.6 1_455 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.851 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.071 # Attachment '- Compound_II.cif' data_Compound_II _database_code_depnum_ccdc_archive 'CCDC 872861' #TrackingRef '- Compound_II.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration rmad _chemical_melting_point ? _chemical_formula_moiety '2(C8 H10 Cd3 O14), 11(H2 O)' _chemical_formula_sum 'C16 H42 Cd6 O39' _chemical_formula_weight 1532.90 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' 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 13.7005(14) _cell_length_b 15.6523(16) _cell_length_c 9.4417(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2024.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_min 0.122 _exptl_crystal_size_mid 0.142 _exptl_crystal_size_max 0.198 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 3.216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6090 _exptl_absorpt_correction_T_max 0.6794 _exptl_absorpt_process_details '(Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD diffractometer' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 0.661 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19407 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 30.04 _reflns_number_total 5914 _reflns_number_gt 5447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 7.34A (Bruker, 2006)' _computing_structure_solution 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _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^)+(0.0455P)^2^+2.1024P] 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 0.03(5) _refine_ls_number_reflns 5914 _refine_ls_number_parameters 315 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.388 _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 0.13221(4) 0.49733(4) 0.39626(5) 0.00964(12) Uani 1 1 d . . . Cd2 Cd 0.00129(5) 0.61262(3) 0.13413(5) 0.00939(12) Uani 1 1 d . . . Cd3 Cd 0.26833(4) 0.22264(4) 0.20859(6) 0.01083(12) Uani 1 1 d . . . O1 O 0.2397(5) 0.3859(4) 0.3251(6) 0.0157(13) Uani 1 1 d . . . O2 O 0.3104(5) 0.3485(4) 0.1239(7) 0.0172(13) Uani 1 1 d . . . O3 O 0.2719(4) 0.5543(4) 0.2764(6) 0.0123(11) Uani 1 1 d D . . H3A H 0.319(5) 0.550(7) 0.334(8) 0.018 Uiso 1 1 d D . . O4 O 0.1074(4) 0.5011(4) 0.1462(5) 0.0102(10) Uani 1 1 d . . . O5 O 0.1356(4) 0.6497(4) -0.0036(6) 0.0135(12) Uani 1 1 d . . . O6 O 0.2750(5) 0.6036(4) -0.0917(6) 0.0137(12) Uani 1 1 d . . . O7 O -0.0956(4) 0.7308(4) 0.1819(6) 0.0122(12) Uani 1 1 d . . . O8 O -0.1455(4) 0.8000(4) 0.3732(7) 0.0150(13) Uani 1 1 d . . . O9 O 0.0915(4) 0.7310(4) 0.2704(6) 0.0120(12) Uani 1 1 d D . . H9 H 0.089(7) 0.757(6) 0.191(5) 0.018 Uiso 1 1 d D . . O10 O -0.0008(5) 0.5934(3) 0.3832(5) 0.0116(10) Uani 1 1 d . . . O11 O 0.1579(4) 0.6035(4) 0.5583(7) 0.0125(12) Uani 1 1 d . . . O12 O 0.1007(4) 0.7225(4) 0.6551(7) 0.0155(12) Uani 1 1 d . . . O13 O 0.1737(4) 0.4319(4) 0.6194(7) 0.0146(12) Uani 1 1 d D . . H13A H 0.189(5) 0.3793(12) 0.621(13) 0.022 Uiso 1 1 d D . . H13B H 0.227(3) 0.459(4) 0.623(12) 0.022 Uiso 1 1 d D . . O14 O -0.0727(5) 0.6362(4) -0.0804(7) 0.0176(14) Uani 1 1 d D . . H14A H -0.065(8) 0.6874(18) -0.108(10) 0.026 Uiso 1 1 d D . . H14B H -0.040(6) 0.606(4) -0.138(8) 0.026 Uiso 1 1 d D . . O15 O 0.3544(5) 0.4856(5) 0.7290(7) 0.0253(16) Uani 1 1 d D . . H15A H 0.390(7) 0.449(5) 0.772(9) 0.038 Uiso 1 1 d D . . H15B H 0.344(8) 0.525(5) 0.788(8) 0.038 Uiso 1 1 d D . . O16 O 0.4137(6) 0.5496(5) 0.4648(10) 0.037(2) Uani 1 1 d D . . H16A H 0.4737(6) 0.5630(5) 0.471(12) 0.056 Uiso 1 1 d D . . H16B H 0.401(7) 0.521(8) 0.539(8) 0.056 Uiso 1 1 d D . . O17 O 0.4409(5) 0.3617(5) 0.9106(7) 0.0229(15) Uani 1 1 d D . . H17A H 0.400(5) 0.347(3) 0.973(5) 0.034 Uiso 1 1 d D . . H17B H 0.497(3) 0.355(7) 0.948(8) 0.034 Uiso 1 1 d D . . O18 O 0.7073(5) 0.2447(4) 0.3592(7) 0.0199(14) Uani 1 1 d D . . H18A H 0.764(3) 0.258(6) 0.331(10) 0.030 Uiso 1 1 d D . . H18B H 0.696(6) 0.276(6) 0.431(8) 0.030 Uiso 1 1 d D . . O19 O 0.5518(5) 0.3033(5) 0.1754(8) 0.0262(16) Uani 1 1 d D . . H19A H 0.507(4) 0.299(8) 0.238(7) 0.039 Uiso 1 1 d D . . H19B H 0.606(3) 0.299(8) 0.220(8) 0.039 Uiso 1 1 d D . . O20 O 0.0000 0.5000 0.7547(8) 0.0188(17) Uani 1 2 d SD . . H20A H 0.0542(9) 0.493(5) 0.7127(11) 0.028 Uiso 1 1 d D . . C1 C 0.2793(6) 0.4045(5) 0.2118(9) 0.0119(15) Uani 1 1 d DU . . C2 C 0.2822(5) 0.4973(6) 0.1619(7) 0.0128(13) Uani 1 1 d DU . . H2 H 0.3437 0.5092 0.1085 0.015 Uiso 1 1 calc R . . C3 C 0.1917(5) 0.5092(5) 0.0652(8) 0.0107(14) Uani 1 1 d DU . . H3 H 0.1920 0.4622 -0.0067 0.013 Uiso 1 1 calc R . . C4 C 0.2005(6) 0.5931(5) -0.0125(8) 0.0104(15) Uani 1 1 d DU . . C5 C -0.0808(6) 0.7609(5) 0.3041(9) 0.0100(11) Uani 1 1 d D . . C6 C 0.0185(5) 0.7478(4) 0.3740(8) 0.0100(11) Uani 1 1 d D . . H6 H 0.0365 0.7982 0.4336 0.012 Uiso 1 1 calc R . . C7 C 0.0094(6) 0.6657(4) 0.4660(7) 0.0091(10) Uani 1 1 d D . . H7 H -0.0507 0.6713 0.5253 0.011 Uiso 1 1 calc R . . C8 C 0.0965(6) 0.6625(5) 0.5652(8) 0.0091(10) Uani 1 1 d 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 0.0132(2) 0.0080(2) 0.0077(2) 0.0002(3) 0.00029(17) 0.0001(2) Cd2 0.0139(2) 0.0070(2) 0.0073(2) -0.00003(17) -0.0001(3) 0.0010(2) Cd3 0.0130(2) 0.0084(2) 0.0111(3) -0.0018(2) -0.0011(2) 0.0014(2) O1 0.020(3) 0.015(3) 0.012(3) 0.004(2) 0.002(2) 0.001(3) O2 0.031(3) 0.010(3) 0.010(3) 0.000(2) 0.002(3) 0.001(3) O3 0.017(3) 0.008(3) 0.011(3) 0.001(2) 0.001(2) 0.001(2) O4 0.015(2) 0.010(2) 0.005(2) 0.000(3) 0.0009(18) 0.001(3) O5 0.020(3) 0.007(3) 0.013(3) 0.001(2) 0.000(2) 0.004(2) O6 0.018(3) 0.012(3) 0.012(3) 0.001(2) 0.008(2) -0.001(2) O7 0.016(3) 0.007(3) 0.014(3) -0.003(2) 0.001(2) 0.001(2) O8 0.018(3) 0.013(3) 0.013(3) -0.003(2) 0.002(2) 0.006(2) O9 0.019(3) 0.011(3) 0.006(3) -0.003(2) 0.002(2) 0.001(2) O10 0.016(2) 0.013(3) 0.006(2) 0.0022(19) 0.000(3) -0.001(3) O11 0.016(3) 0.007(3) 0.015(3) -0.003(2) -0.004(2) 0.002(2) O12 0.016(3) 0.009(3) 0.022(3) -0.006(3) -0.005(2) -0.003(2) O13 0.023(3) 0.008(3) 0.013(3) 0.001(2) -0.003(3) 0.003(2) O14 0.021(3) 0.013(3) 0.019(3) 0.000(3) -0.001(3) 0.001(3) O15 0.031(4) 0.024(4) 0.021(3) -0.009(3) -0.003(3) 0.007(3) O16 0.039(4) 0.030(5) 0.043(5) 0.011(4) -0.025(4) -0.008(4) O17 0.028(4) 0.021(4) 0.019(4) -0.002(3) 0.007(3) -0.001(3) O18 0.022(3) 0.022(4) 0.016(3) -0.006(3) 0.004(3) -0.006(2) O19 0.017(3) 0.029(4) 0.033(4) -0.007(3) -0.001(3) -0.001(3) O20 0.022(4) 0.016(4) 0.018(4) 0.000 0.000 0.011(4) C1 0.011(3) 0.013(3) 0.012(4) 0.000(3) -0.002(3) 0.004(3) C2 0.014(3) 0.013(3) 0.012(3) 0.002(3) 0.001(2) 0.001(3) C3 0.014(3) 0.007(3) 0.011(3) -0.001(3) 0.004(2) 0.001(3) C4 0.014(4) 0.008(3) 0.010(4) -0.001(3) 0.001(3) -0.001(3) C5 0.019(3) 0.005(2) 0.006(2) 0.0033(19) -0.001(2) 0.001(2) C6 0.019(3) 0.005(2) 0.006(2) 0.0033(19) -0.001(2) 0.001(2) C7 0.013(3) 0.006(2) 0.008(2) 0.0028(19) -0.002(2) 0.001(2) C8 0.013(3) 0.006(2) 0.008(2) 0.0028(19) -0.002(2) 0.001(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 O11 2.286(6) . ? Cd1 O10 2.296(6) 2_565 ? Cd1 O10 2.365(6) . ? Cd1 O1 2.379(6) . ? Cd1 O4 2.386(5) . ? Cd1 O3 2.395(6) . ? Cd1 O13 2.410(6) . ? Cd2 O4 2.275(6) . ? Cd2 O14 2.295(7) . ? Cd2 O7 2.321(6) . ? Cd2 O4 2.324(6) 2_565 ? Cd2 O5 2.327(6) . ? Cd2 O10 2.371(5) . ? Cd2 O9 2.572(6) . ? Cd3 O2 2.203(6) . ? Cd3 O12 2.208(6) 3_546 ? Cd3 O6 2.245(6) 3_545 ? Cd3 O8 2.318(6) 2_565 ? Cd3 O7 2.489(5) 2_565 ? Cd3 O5 2.604(6) 3_545 ? Cd3 C5 2.735(7) 2_565 ? O1 C1 1.234(10) . ? O2 C1 1.280(10) . ? O3 C2 1.409(10) . ? O4 C3 1.391(9) . ? O4 Cd2 2.324(6) 2_565 ? O5 C4 1.258(10) . ? O5 Cd3 2.604(6) 3 ? O6 C4 1.275(10) . ? O6 Cd3 2.245(6) 3 ? O7 C5 1.263(10) . ? O7 Cd3 2.489(5) 2_565 ? O8 C5 1.259(10) . ? O8 Cd3 2.318(6) 2_565 ? O9 C6 1.424(9) . ? O10 C7 1.383(9) . ? O10 Cd1 2.296(6) 2_565 ? O11 C8 1.251(10) . ? O12 C8 1.267(10) . ? O12 Cd3 2.208(6) 3_556 ? C1 C2 1.528(10) . ? C2 C3 1.551(9) . ? C3 C4 1.510(9) . ? C5 C6 1.526(9) . ? C5 Cd3 2.735(7) 2_565 ? C6 C7 1.555(9) . ? C7 C8 1.518(9) . ? 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 O11 Cd1 O10 127.3(2) . 2_565 ? O11 Cd1 O10 72.02(19) . . ? O10 Cd1 O10 77.6(2) 2_565 . ? O11 Cd1 O1 128.8(2) . . ? O10 Cd1 O1 91.0(2) 2_565 . ? O10 Cd1 O1 158.1(2) . . ? O11 Cd1 O4 131.8(2) . . ? O10 Cd1 O4 81.41(19) 2_565 . ? O10 Cd1 O4 79.83(18) . . ? O1 Cd1 O4 80.0(2) . . ? O11 Cd1 O3 85.6(2) . . ? O10 Cd1 O3 146.24(19) 2_565 . ? O10 Cd1 O3 110.74(19) . . ? O1 Cd1 O3 69.2(2) . . ? O4 Cd1 O3 68.72(19) . . ? O11 Cd1 O13 71.8(2) . . ? O10 Cd1 O13 88.2(2) 2_565 . ? O10 Cd1 O13 119.82(19) . . ? O1 Cd1 O13 77.8(2) . . ? O4 Cd1 O13 155.3(2) . . ? O3 Cd1 O13 112.5(2) . . ? O4 Cd2 O14 116.7(2) . . ? O4 Cd2 O7 165.3(2) . . ? O14 Cd2 O7 77.9(2) . . ? O4 Cd2 O4 79.61(19) . 2_565 ? O14 Cd2 O4 83.3(2) . 2_565 ? O7 Cd2 O4 103.5(2) . 2_565 ? O4 Cd2 O5 73.4(2) . . ? O14 Cd2 O5 79.4(2) . . ? O7 Cd2 O5 111.3(2) . . ? O4 Cd2 O5 136.5(2) 2_565 . ? O4 Cd2 O10 81.97(19) . . ? O14 Cd2 O10 152.9(2) . . ? O7 Cd2 O10 84.4(2) . . ? O4 Cd2 O10 81.16(19) 2_565 . ? O5 Cd2 O10 126.5(2) . . ? O4 Cd2 O9 102.8(2) . . ? O14 Cd2 O9 122.5(2) . . ? O7 Cd2 O9 66.6(2) . . ? O4 Cd2 O9 146.65(18) 2_565 . ? O5 Cd2 O9 73.7(2) . . ? O10 Cd2 O9 66.51(19) . . ? O2 Cd3 O12 90.0(2) . 3_546 ? O2 Cd3 O6 129.2(2) . 3_545 ? O12 Cd3 O6 120.1(2) 3_546 3_545 ? O2 Cd3 O8 124.8(2) . 2_565 ? O12 Cd3 O8 101.5(2) 3_546 2_565 ? O6 Cd3 O8 90.6(2) 3_545 2_565 ? O2 Cd3 O7 87.1(2) . 2_565 ? O12 Cd3 O7 146.3(2) 3_546 2_565 ? O6 Cd3 O7 86.7(2) 3_545 2_565 ? O8 Cd3 O7 54.71(19) 2_565 2_565 ? O2 Cd3 O5 89.4(2) . 3_545 ? O12 Cd3 O5 91.3(2) 3_546 3_545 ? O6 Cd3 O5 53.4(2) 3_545 3_545 ? O8 Cd3 O5 142.9(2) 2_565 3_545 ? O7 Cd3 O5 122.3(2) 2_565 3_545 ? O2 Cd3 C5 106.3(2) . 2_565 ? O12 Cd3 C5 124.8(2) 3_546 2_565 ? O6 Cd3 C5 89.6(2) 3_545 2_565 ? O8 Cd3 C5 27.3(2) 2_565 2_565 ? O7 Cd3 C5 27.5(2) 2_565 2_565 ? O5 Cd3 C5 139.6(2) 3_545 2_565 ? C1 O1 Cd1 110.1(5) . . ? C1 O2 Cd3 106.8(5) . . ? C2 O3 Cd1 102.0(4) . . ? C3 O4 Cd2 115.7(5) . . ? C3 O4 Cd2 125.1(5) . 2_565 ? Cd2 O4 Cd2 100.10(19) . 2_565 ? C3 O4 Cd1 115.4(4) . . ? Cd2 O4 Cd1 99.2(2) . . ? Cd2 O4 Cd1 96.9(2) 2_565 . ? C4 O5 Cd2 114.9(5) . . ? C4 O5 Cd3 84.4(5) . 3 ? Cd2 O5 Cd3 157.6(3) . 3 ? C4 O6 Cd3 100.6(5) . 3 ? C5 O7 Cd2 112.5(5) . . ? C5 O7 Cd3 87.2(4) . 2_565 ? Cd2 O7 Cd3 142.9(3) . 2_565 ? C5 O8 Cd3 95.1(5) . 2_565 ? C6 O9 Cd2 98.0(4) . . ? C7 O10 Cd1 123.7(5) . 2_565 ? C7 O10 Cd1 114.4(5) . . ? Cd1 O10 Cd1 102.0(2) 2_565 . ? C7 O10 Cd2 117.1(4) . . ? Cd1 O10 Cd2 98.1(2) 2_565 . ? Cd1 O10 Cd2 97.1(2) . . ? C8 O11 Cd1 117.9(5) . . ? C8 O12 Cd3 115.3(5) . 3_556 ? O1 C1 O2 123.2(7) . . ? O1 C1 C2 120.2(7) . . ? O2 C1 C2 116.3(7) . . ? O3 C2 C1 111.3(6) . . ? O3 C2 C3 107.2(6) . . ? C1 C2 C3 105.9(6) . . ? O4 C3 C4 114.4(6) . . ? O4 C3 C2 109.2(6) . . ? C4 C3 C2 109.0(6) . . ? O5 C4 O6 120.9(7) . . ? O5 C4 C3 121.6(7) . . ? O6 C4 C3 117.5(7) . . ? O8 C5 O7 122.8(7) . . ? O8 C5 C6 117.9(7) . . ? O7 C5 C6 119.2(7) . . ? O8 C5 Cd3 57.6(4) . 2_565 ? O7 C5 Cd3 65.4(4) . 2_565 ? C6 C5 Cd3 173.1(5) . 2_565 ? O9 C6 C5 110.7(6) . . ? O9 C6 C7 106.7(6) . . ? C5 C6 C7 106.4(6) . . ? O10 C7 C8 113.7(6) . . ? O10 C7 C6 111.6(6) . . ? C8 C7 C6 108.0(6) . . ? O11 C8 O12 123.5(7) . . ? O11 C8 C7 121.4(7) . . ? O12 C8 C7 115.1(7) . . ? 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 C1 C2 C3 C4 -168.3(6) . . . . ? C5 C6 C7 C8 -165.9(6) . . . . ? O3 C2 C3 O4 -52.8(8) . . . . ? O9 C6 C7 O10 -49.8(8) . . . . ? 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 O16 0.8500(14) 1.789(14) 2.636(9) 174(11) . O9 H9 O17 0.8500(14) 1.94(6) 2.702(9) 148(10) 3_556 O13 H13A O18 0.8500(14) 1.965(16) 2.809(9) 172(9) 4_456 O13 H13B O15 0.8500(15) 2.05(5) 2.811(9) 149(9) . O14 H14A O19 0.8500(14) 1.931(11) 2.780(10) 178(12) 3 O14 H14B O20 0.8500(14) 2.02(3) 2.822(8) 158(8) 1_554 O15 H15A O17 0.8500(14) 2.02(3) 2.847(10) 164(11) . O15 H15B O6 0.8500(14) 1.92(4) 2.732(9) 160(11) 1_556 O16 H16A O16 0.8500(15) 2.342(12) 2.827(17) 116.6(11) 2_665 O16 H16B O15 0.8500(14) 1.98(4) 2.808(12) 163(13) . O17 H17A O2 0.8500(14) 1.877(15) 2.701(9) 163(4) 1_556 O17 H17B O19 0.8500(15) 2.41(6) 3.065(10) 134(7) 1_556 O18 H18A O9 0.8500(14) 2.065(19) 2.906(9) 171(10) 2_665 O18 H18B O8 0.8500(14) 2.01(5) 2.803(9) 154(10) 3_546 O19 H19A O12 0.8500(14) 2.15(6) 2.920(9) 150(11) 3_546 O19 H19B O18 0.8500(14) 2.10(4) 2.897(10) 157(10) . O20 H20A O13 0.8500(14) 2.09(3) 2.904(7) 161(7) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.883 _refine_diff_density_min -1.255 _refine_diff_density_rms 0.214 # Attachment '- Compound_III.cif' data_Compound_III _database_code_depnum_ccdc_archive 'CCDC 872862' #TrackingRef '- Compound_III.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration rmad _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 Cd2 O13, 3(H2 O)' _chemical_formula_sum 'C8 H16 Cd2 O16' _chemical_formula_weight 593.01 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.6393(8) _cell_length_b 11.5121(12) _cell_length_c 9.0174(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.3050(10) _cell_angle_gamma 90.00 _cell_volume 782.59(14) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6807 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.39 _exptl_crystal_description tetrahedron _exptl_crystal_colour colorless _exptl_crystal_size_min 0.114 _exptl_crystal_size_mid 0.142 _exptl_crystal_size_max 0.202 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 2.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6587 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details '(Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Apex CCD diffractometer 01-670-01' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 0.661 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6492 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.40 _reflns_number_total 2854 _reflns_number_gt 2725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 7.34A (Bruker, 2006)' _computing_structure_solution 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _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^)+(0.0202P)^2^] 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 0.02(2) _refine_ls_number_reflns 2854 _refine_ls_number_parameters 271 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0197 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0420 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.001 _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 0.26647(3) 0.654884(19) 0.26233(2) 0.02620(7) Uani 1 1 d . . . Cd2 Cd 0.13979(3) 0.16122(2) 0.28817(2) 0.02772(7) Uani 1 1 d . . . O1 O 0.3659(3) 0.1755(2) 0.4773(3) 0.0375(6) Uani 1 1 d . . . O2 O 0.5232(4) 0.2841(2) 0.6527(3) 0.0436(7) Uani 1 1 d . . . O3 O 0.1125(4) 0.3381(3) 0.4149(3) 0.0465(7) Uani 1 1 d D . . H3A H 0.035(4) 0.300(4) 0.434(3) 0.070 Uiso 1 1 d D . . O4 O 0.3956(4) 0.4985(3) 0.4277(3) 0.0437(7) Uani 1 1 d D . . H4 H 0.372(6) 0.451(3) 0.366(3) 0.066 Uiso 1 1 d D . . C1 C 0.3888(5) 0.2643(3) 0.5580(4) 0.0297(8) Uani 1 1 d . . . C2 C 0.2405(5) 0.3542(3) 0.5492(4) 0.0300(9) Uani 1 1 d D . . H2 H 0.1801 0.3434 0.6362 0.036 Uiso 1 1 calc R . . C3 C 0.3070(5) 0.4774(3) 0.5511(4) 0.0296(8) Uani 1 1 d D . . H3 H 0.3930 0.4880 0.6432 0.035 Uiso 1 1 calc R . . C4 C 0.1561(5) 0.5632(3) 0.5551(4) 0.0295(8) Uani 1 1 d . . . O5 O 0.1189(4) 0.6387(3) 0.4568(3) 0.0426(8) Uani 1 1 d . . . O6 O 0.0751(4) 0.5502(3) 0.6637(3) 0.0437(7) Uani 1 1 d . . . O7 O -0.0414(3) 0.2123(2) 0.0690(3) 0.0326(6) Uani 1 1 d . . . O8 O -0.0652(4) 0.2869(2) -0.1608(3) 0.0336(7) Uani 1 1 d . . . O9 O 0.2920(3) 0.2781(2) 0.1439(3) 0.0314(6) Uani 1 1 d D . . H9 H 0.394(2) 0.282(4) 0.154(5) 0.047 Uiso 1 1 d D . . O10 O 0.1185(4) 0.4883(2) 0.1374(3) 0.0294(6) Uani 1 1 d D . . H10 H 0.062(6) 0.543(3) 0.139(6) 0.044 Uiso 1 1 d D . . O11 O 0.4291(3) 0.5879(2) 0.0993(3) 0.0341(6) Uani 1 1 d . . . O12 O 0.4599(4) 0.4665(3) -0.0852(3) 0.0533(8) Uani 1 1 d . . . C5 C 0.0190(5) 0.2669(3) -0.0296(4) 0.0256(8) Uani 1 1 d . . . C6 C 0.2036(4) 0.3195(3) 0.0038(4) 0.0250(7) Uani 1 1 d . . . H6 H 0.2709 0.2966 -0.0752 0.030 Uiso 1 1 calc R . . C7 C 0.1935(5) 0.4530(3) 0.0094(4) 0.0237(7) Uani 1 1 d . . . H7 H 0.1140 0.4792 -0.0807 0.028 Uiso 1 1 calc R . . C8 C 0.3748(5) 0.5068(3) 0.0072(4) 0.0279(8) Uani 1 1 d . . . O13 O 0.2419(4) 0.0036(3) 0.1857(5) 0.0563(10) Uani 1 1 d D . . H13A H 0.332(5) 0.009(6) 0.158(8) 0.084 Uiso 1 1 d D . . H13B H 0.195(7) -0.056(3) 0.182(7) 0.084 Uiso 1 1 d D . . O14 O 0.7754(7) 0.4099(6) 0.4414(9) 0.114(2) Uani 1 1 d D . . H14A H 0.737(12) 0.365(7) 0.491(11) 0.171 Uiso 1 1 d D . . H14B H 0.700(10) 0.453(7) 0.412(12) 0.171 Uiso 1 1 d D . . O15 O 0.6343(5) 0.2659(5) 0.1870(5) 0.0904(15) Uani 1 1 d D . . H15A H 0.687(10) 0.231(6) 0.135(8) 0.136 Uiso 1 1 d D . . H15B H 0.695(10) 0.310(6) 0.236(8) 0.136 Uiso 1 1 d D . . O16 O 0.7881(6) 0.5608(5) 0.1986(6) 0.0952(15) Uani 1 1 d D . . H16A H 0.793(13) 0.4940(19) 0.207(11) 0.143 Uiso 1 1 d D . . H16B H 0.692(5) 0.577(8) 0.163(9) 0.143 Uiso 1 1 d 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 0.02846(12) 0.02430(11) 0.02499(12) 0.00021(16) 0.00174(9) 0.00148(16) Cd2 0.02869(13) 0.02612(11) 0.02744(12) -0.00048(16) 0.00181(9) -0.00228(16) O1 0.0385(13) 0.0299(17) 0.0399(13) -0.0073(13) -0.0056(10) 0.0077(13) O2 0.0444(17) 0.0327(14) 0.0454(17) -0.0073(13) -0.0175(14) 0.0136(12) O3 0.0297(15) 0.0435(17) 0.0600(19) -0.0193(15) -0.0113(14) 0.0100(12) O4 0.0440(17) 0.0494(17) 0.0434(18) 0.0155(14) 0.0241(15) 0.0209(14) C1 0.033(2) 0.0283(18) 0.0255(19) -0.0004(15) -0.0008(16) 0.0025(16) C2 0.0269(19) 0.033(2) 0.029(2) -0.0035(17) 0.0022(16) 0.0035(16) C3 0.032(2) 0.0325(19) 0.0238(19) 0.0071(15) 0.0034(16) 0.0044(16) C4 0.034(2) 0.0318(18) 0.0231(19) -0.0008(15) 0.0069(17) 0.0020(16) O5 0.0512(15) 0.046(2) 0.0331(12) 0.0150(14) 0.0156(11) 0.0256(15) O6 0.0545(19) 0.0464(16) 0.0350(16) 0.0130(13) 0.0215(15) 0.0255(14) O7 0.0235(13) 0.0374(13) 0.0349(14) 0.0061(12) -0.0010(11) -0.0077(11) O8 0.0398(17) 0.0285(14) 0.0283(15) 0.0034(12) -0.0073(13) -0.0042(12) O9 0.0179(13) 0.0397(15) 0.0341(15) 0.0109(12) -0.0034(12) -0.0005(12) O10 0.0246(14) 0.0283(14) 0.0376(16) -0.0060(12) 0.0120(12) 0.0018(11) O11 0.0268(14) 0.0370(14) 0.0392(16) -0.0040(12) 0.0076(12) -0.0082(11) O12 0.0485(19) 0.067(2) 0.0529(19) -0.0236(16) 0.0345(16) -0.0207(16) C5 0.0235(18) 0.0169(17) 0.035(2) -0.0082(14) -0.0004(16) -0.0006(14) C6 0.0271(19) 0.0261(17) 0.0220(18) -0.0012(14) 0.0044(15) 0.0007(15) C7 0.0232(18) 0.0261(17) 0.0218(18) -0.0006(14) 0.0037(14) -0.0016(13) C8 0.0291(19) 0.0264(17) 0.030(2) 0.0024(15) 0.0089(16) -0.0030(15) O13 0.038(2) 0.0333(17) 0.104(3) -0.0151(19) 0.0331(19) -0.0026(14) O14 0.088(4) 0.104(5) 0.154(6) 0.018(4) 0.029(4) 0.010(3) O15 0.036(2) 0.150(5) 0.083(3) -0.045(3) 0.0031(19) 0.026(2) O16 0.042(2) 0.152(4) 0.085(3) 0.002(3) -0.010(2) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O11 2.212(3) . ? Cd1 O2 2.233(3) 2_656 ? Cd1 O5 2.241(3) . ? Cd1 O8 2.249(3) 2 ? Cd1 O10 2.411(3) . ? Cd1 O4 2.442(3) . ? Cd2 O6 2.179(2) 2_546 ? Cd2 O1 2.229(2) . ? Cd2 O13 2.233(3) . ? Cd2 O7 2.299(3) . ? Cd2 O9 2.312(3) . ? Cd2 O3 2.360(3) . ? O1 C1 1.251(5) . ? O2 C1 1.246(4) . ? O2 Cd1 2.233(3) 2_646 ? O3 C2 1.440(5) . ? O4 C3 1.414(5) . ? C1 C2 1.527(5) . ? C2 C3 1.505(5) . ? C3 C4 1.523(5) . ? C4 O5 1.242(4) . ? C4 O6 1.249(4) . ? O6 Cd2 2.179(2) 2_556 ? O7 C5 1.238(4) . ? O8 C5 1.273(5) . ? O8 Cd1 2.249(3) 2_545 ? O9 C6 1.415(4) . ? O10 C7 1.428(4) . ? O11 C8 1.274(4) . ? O12 C8 1.228(4) . ? C5 C6 1.519(5) . ? C6 C7 1.540(5) . ? C7 C8 1.520(5) . ? 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 O11 Cd1 O2 90.58(11) . 2_656 ? O11 Cd1 O5 154.07(10) . . ? O2 Cd1 O5 102.23(12) 2_656 . ? O11 Cd1 O8 112.68(10) . 2 ? O2 Cd1 O8 95.52(10) 2_656 2 ? O5 Cd1 O8 88.69(10) . 2 ? O11 Cd1 O10 71.55(9) . . ? O2 Cd1 O10 161.36(10) 2_656 . ? O5 Cd1 O10 92.43(10) . . ? O8 Cd1 O10 96.27(10) 2 . ? O11 Cd1 O4 86.21(9) . . ? O2 Cd1 O4 94.85(10) 2_656 . ? O5 Cd1 O4 70.47(9) . . ? O8 Cd1 O4 158.29(10) 2 . ? O10 Cd1 O4 79.13(10) . . ? O6 Cd2 O1 114.00(11) 2_546 . ? O6 Cd2 O13 86.02(11) 2_546 . ? O1 Cd2 O13 95.56(13) . . ? O6 Cd2 O7 87.29(10) 2_546 . ? O1 Cd2 O7 157.47(10) . . ? O13 Cd2 O7 93.10(14) . . ? O6 Cd2 O9 156.52(11) 2_546 . ? O1 Cd2 O9 89.40(10) . . ? O13 Cd2 O9 89.94(13) . . ? O7 Cd2 O9 69.82(9) . . ? O6 Cd2 O3 106.34(10) 2_546 . ? O1 Cd2 O3 71.59(10) . . ? O13 Cd2 O3 164.83(11) . . ? O7 Cd2 O3 96.18(9) . . ? O9 Cd2 O3 82.08(11) . . ? C1 O1 Cd2 121.6(2) . . ? C1 O2 Cd1 125.5(2) . 2_646 ? C2 O3 Cd2 114.7(2) . . ? C3 O4 Cd1 114.2(2) . . ? O2 C1 O1 124.8(3) . . ? O2 C1 C2 115.7(3) . . ? O1 C1 C2 119.4(3) . . ? O3 C2 C3 108.2(3) . . ? O3 C2 C1 110.7(3) . . ? C3 C2 C1 113.1(3) . . ? O4 C3 C2 110.9(3) . . ? O4 C3 C4 111.6(3) . . ? C2 C3 C4 110.8(3) . . ? O5 C4 O6 123.9(3) . . ? O5 C4 C3 121.6(3) . . ? O6 C4 C3 114.5(3) . . ? C4 O5 Cd1 122.1(2) . . ? C4 O6 Cd2 124.8(2) . 2_556 ? C5 O7 Cd2 120.3(2) . . ? C5 O8 Cd1 117.8(2) . 2_545 ? C6 O9 Cd2 119.2(2) . . ? C7 O10 Cd1 112.6(2) . . ? C8 O11 Cd1 122.0(2) . . ? O7 C5 O8 124.6(3) . . ? O7 C5 C6 120.2(3) . . ? O8 C5 C6 115.2(3) . . ? O9 C6 C5 109.6(3) . . ? O9 C6 C7 109.0(3) . . ? C5 C6 C7 110.7(3) . . ? O10 C7 C8 112.3(3) . . ? O10 C7 C6 109.8(3) . . ? C8 C7 C6 110.8(3) . . ? O12 C8 O11 124.6(3) . . ? O12 C8 C7 116.0(3) . . ? O11 C8 C7 119.4(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 C1 C2 C3 C4 -175.3(3) . . . . ? C5 C6 C7 C8 -167.1(3) . . . . ? O3 C2 C3 O4 -62.8(4) . . . . ? O9 C6 C7 O10 -52.6(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 O5 0.775(18) 2.49(3) 3.223(4) 159(4) 2_546 O4 H4 O3 0.776(18) 2.47(3) 2.832(4) 110.3(19) . O9 H9 O15 0.773(18) 1.82(2) 2.584(4) 171(5) . O10 H10 O16 0.768(18) 2.25(4) 2.797(5) 129(5) 1_455 O13 H13A O12 0.770(18) 1.88(3) 2.619(4) 161(7) 2_645 O13 H13B O8 0.771(18) 2.058(19) 2.829(4) 177(7) 2_545 O14 H14A O2 0.775(18) 2.53(5) 3.260(7) 157(9) . O14 H14B O4 0.775(18) 2.41(6) 3.059(6) 142(9) . O15 H15A O7 0.771(18) 2.26(6) 2.916(4) 143(8) 1_655 O15 H15B O14 0.772(18) 2.18(4) 2.893(10) 153(8) . O16 H16A O14 0.773(18) 2.34(9) 2.808(9) 120(9) . O16 H16B O11 0.774(18) 2.00(3) 2.762(5) 166(10) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.369 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.064