Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Qing-Jin Meng' _publ_contact_author_address ; Nanjing University Nanjing 210093 CHINA ; _publ_contact_author_email MENGQJ@NJU.EDU.CN _publ_section_title ; Syntheses, structures and properties of a series of organic-inorganic complexes based on methylenediisophthalic acid (H4MDIP ; loop_ _publ_author_name 'Qingjin Meng' 'Xianying Duan' 'Yizhi Li' 'Jian-Guo Lin' 'Chengjian Zhu' data_sad _database_code_depnum_ccdc_archive 'CCDC 651544' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H18 Mg O12, 3(H2 O)' _chemical_formula_sum 'C17 H24 Mg O15' _chemical_formula_weight 492.67 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0000 '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 8.0984(14) _cell_length_b 16.458(3) _cell_length_c 16.621(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2215.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 9114 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.00 _exptl_crystal_description block _exptl_crystal_colour clolorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11888 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2477 _reflns_number_gt 2033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.05P)^2^+0.22P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? #_refine_ls_abs_structure_details # 'Flack H D (1983), Acta Cryst. A39, 876-881' #_refine_ls_abs_structure_Flack -10(10) _refine_ls_number_reflns 2477 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 C1 C 0.8592(5) 0.2823(2) 0.6822(2) 0.0282(9) Uani 1 1 d . . . C2 C 0.8898(5) 0.3594(2) 0.7098(2) 0.0322(9) Uani 1 1 d . . . H2 H 0.9487 0.3670 0.7573 0.039 Uiso 1 1 calc R . . C3 C 0.8334(5) 0.4259(2) 0.6672(2) 0.0308(9) Uani 1 1 d . . . C4 C 0.7398(5) 0.4139(2) 0.5977(2) 0.0314(9) Uani 1 1 d . . . H4 H 0.7004 0.4585 0.5693 0.038 Uiso 1 1 calc R . . C5 C 0.7047(5) 0.3356(2) 0.5705(2) 0.0261(8) Uani 1 1 d . . . C6 C 0.7679(5) 0.2706(3) 0.6133(2) 0.0304(9) Uani 1 1 d . . . H6 H 0.7483 0.2180 0.5952 0.036 Uiso 1 1 calc R . . C7 C 0.6048(5) 0.3212(2) 0.4951(2) 0.0297(9) Uani 1 1 d . . . H7A H 0.5563 0.3722 0.4778 0.036 Uiso 1 1 calc R . . H7B H 0.5153 0.2840 0.5072 0.036 Uiso 1 1 calc R . . C8 C 0.7080(5) 0.2866(2) 0.4271(2) 0.0295(9) Uani 1 1 d . . . C9 C 0.8040(5) 0.3364(3) 0.3793(2) 0.0332(9) Uani 1 1 d . . . H9 H 0.8080 0.3919 0.3898 0.040 Uiso 1 1 calc R . . C10 C 0.8946(5) 0.3045(2) 0.3157(2) 0.0289(9) Uani 1 1 d . . . C11 C 0.8933(5) 0.2218(3) 0.3026(2) 0.0307(9) Uani 1 1 d . . . H11 H 0.9538 0.2003 0.2601 0.037 Uiso 1 1 calc R . . C12 C 0.8046(5) 0.1705(3) 0.3511(2) 0.0317(9) Uani 1 1 d . . . C13 C 0.7089(5) 0.2033(2) 0.4128(2) 0.0295(9) Uani 1 1 d . . . H13 H 0.6451 0.1692 0.4447 0.035 Uiso 1 1 calc R . . C14 C 0.9318(5) 0.2126(2) 0.7273(2) 0.0313(9) Uani 1 1 d . . . C15 C 0.8743(5) 0.5115(3) 0.6917(3) 0.0352(10) Uani 1 1 d . . . C16 C 0.9928(5) 0.3587(2) 0.2630(2) 0.0257(8) Uani 1 1 d . . . C17 C 0.8079(5) 0.0792(2) 0.3406(2) 0.0294(9) Uani 1 1 d . . . Mg1 Mg 1.04929(16) 0.16895(8) 0.90080(8) 0.0266(3) Uani 1 1 d . . . O1 O 0.9099(3) 0.14183(17) 0.69411(16) 0.0331(7) Uani 1 1 d . . . H1 H 0.9677 0.1080 0.7170 0.050 Uiso 1 1 calc R . . O2 O 1.0041(4) 0.22324(16) 0.79076(15) 0.0339(7) Uani 1 1 d . . . O3 O 0.9413(4) 0.51940(17) 0.76052(15) 0.0360(7) Uani 1 1 d . . . O4 O 0.8442(4) 0.56722(18) 0.64504(17) 0.0365(7) Uani 1 1 d . . . O5 O 1.0205(4) 0.43032(17) 0.29215(16) 0.0424(8) Uani 1 1 d . . . H5 H 1.0701 0.4578 0.2588 0.064 Uiso 1 1 calc R . . O6 O 1.0377(4) 0.33689(17) 0.19540(15) 0.0351(7) Uani 1 1 d . . . O7 O 0.7610(4) 0.03686(18) 0.39815(16) 0.0400(7) Uani 1 1 d . . . O8 O 0.8566(4) 0.05283(16) 0.27444(16) 0.0315(6) Uani 1 1 d . . . O9 O 1.2862(3) 0.22336(17) 0.90202(16) 0.0349(7) Uani 1 1 d . . . H9B H 1.3484 0.2027 0.8662 0.042 Uiso 1 1 d R . . H9C H 1.2655 0.2729 0.8918 0.042 Uiso 1 1 d R . . O10 O 1.0877(4) 0.12431(19) 1.01573(16) 0.0408(8) Uani 1 1 d . . . H10A H 1.1889 0.1227 1.0293 0.049 Uiso 1 1 d R . . H10B H 1.0306 0.1486 1.0513 0.049 Uiso 1 1 d R . . O11 O 0.8168(3) 0.11970(16) 0.90076(17) 0.0330(6) Uani 1 1 d . . . H11A H 0.7528 0.1437 0.8679 0.040 Uiso 1 1 d R . . H11B H 0.8182 0.0690 0.8908 0.040 Uiso 1 1 d R . . O12 O 0.9604(4) 0.27526(17) 0.95013(16) 0.0410(7) Uani 1 1 d . . . H12A H 0.9393 0.3113 0.9150 0.049 Uiso 1 1 d R . . H12B H 0.8773 0.2677 0.9805 0.049 Uiso 1 1 d R . . O13 O 0.3248(4) 0.38509(16) 0.87718(16) 0.0353(7) Uani 1 1 d . . . H13A H 0.3126 0.3996 0.8285 0.042 Uiso 1 1 d R . . H13C H 0.2931 0.4228 0.9085 0.042 Uiso 1 1 d R . . O14 O 0.8226(4) 0.02195(18) 0.55733(18) 0.0408(7) Uani 1 1 d . . . H14A H 0.7883 0.0359 0.5110 0.049 Uiso 1 1 d R . . H14C H 0.8009 0.0591 0.5913 0.049 Uiso 1 1 d R . . O15 O 0.3769(4) 0.05918(19) 0.08889(18) 0.0469(8) Uani 1 1 d . . . H15A H 0.3710 0.0408 0.1366 0.056 Uiso 1 1 d R . . H15C H 0.4613 0.0398 0.0654 0.056 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(2) 0.0227(19) 0.034(2) 0.0035(17) 0.0076(17) 0.0020(16) C2 0.035(2) 0.032(2) 0.029(2) 0.0042(17) -0.0036(17) -0.0001(18) C3 0.032(2) 0.032(2) 0.028(2) 0.0018(18) 0.0023(17) -0.0020(18) C4 0.033(2) 0.031(2) 0.030(2) 0.0107(18) 0.0032(19) 0.0085(17) C5 0.0243(19) 0.027(2) 0.0272(18) 0.0034(16) 0.0029(15) -0.0027(17) C6 0.033(2) 0.033(2) 0.0251(19) -0.0028(17) 0.0037(17) -0.0015(18) C7 0.033(2) 0.026(2) 0.0299(19) 0.0006(16) -0.0084(17) 0.0018(17) C8 0.025(2) 0.036(2) 0.0275(19) 0.0008(17) -0.0042(16) 0.0051(18) C9 0.033(2) 0.029(2) 0.038(2) 0.0003(18) -0.0117(17) 0.0001(19) C10 0.033(2) 0.025(2) 0.029(2) 0.0004(16) -0.0026(17) -0.0033(17) C11 0.030(2) 0.037(2) 0.0248(18) 0.0013(18) 0.0008(17) 0.0014(18) C12 0.032(2) 0.030(2) 0.034(2) -0.0002(18) -0.0086(17) -0.0019(18) C13 0.031(2) 0.028(2) 0.0293(19) -0.0001(17) -0.0014(17) 0.0018(17) C14 0.031(2) 0.030(2) 0.033(2) -0.0008(18) 0.0043(18) 0.0017(18) C15 0.032(2) 0.034(2) 0.040(2) -0.001(2) 0.000(2) -0.0058(18) C16 0.030(2) 0.026(2) 0.0217(18) -0.0013(15) 0.0003(16) -0.0024(16) C17 0.028(2) 0.026(2) 0.034(2) -0.0020(18) 0.0019(18) 0.0009(17) Mg1 0.0269(6) 0.0248(6) 0.0280(6) 0.0007(6) -0.0046(5) -0.0003(6) O1 0.0374(18) 0.0345(16) 0.0274(14) 0.0047(12) -0.0108(13) 0.0058(12) O2 0.0443(18) 0.0289(15) 0.0284(13) 0.0012(12) -0.0111(13) 0.0016(13) O3 0.0512(19) 0.0301(15) 0.0265(13) 0.0028(12) -0.0190(14) -0.0096(14) O4 0.0379(17) 0.0321(16) 0.0394(16) 0.0078(14) -0.0084(14) -0.0042(13) O5 0.059(2) 0.0331(16) 0.0354(15) -0.0007(13) 0.0221(15) -0.0241(15) O6 0.0404(16) 0.0364(15) 0.0285(14) -0.0049(12) 0.0109(12) -0.0166(14) O7 0.0488(19) 0.0411(17) 0.0302(14) 0.0009(14) 0.0132(15) -0.0046(14) O8 0.0467(18) 0.0239(14) 0.0238(13) -0.0024(11) 0.0078(13) 0.0067(13) O9 0.0308(15) 0.0420(17) 0.0318(14) 0.0004(14) -0.0011(13) 0.0016(13) O10 0.0369(18) 0.058(2) 0.0276(14) 0.0137(15) -0.0051(13) 0.0043(15) O11 0.0294(14) 0.0289(14) 0.0408(16) 0.0104(13) -0.0141(13) -0.0058(12) O12 0.0518(19) 0.0379(16) 0.0333(14) 0.0023(13) 0.0117(14) 0.0034(16) O13 0.054(2) 0.0254(15) 0.0266(13) 0.0014(12) 0.0004(13) 0.0011(14) O14 0.0517(19) 0.0326(16) 0.0381(16) 0.0027(14) -0.0019(15) -0.0095(15) O15 0.055(2) 0.0475(18) 0.0381(16) 0.0113(15) -0.0071(16) 0.0115(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 C1 C2 1.373(6) . ? C1 C6 1.376(6) . ? C1 C14 1.491(5) . ? C2 C3 1.381(6) . ? C2 H2 0.9300 . ? C3 C4 1.396(6) . ? C3 C15 1.502(6) . ? C4 C5 1.395(6) . ? C4 H4 0.9300 . ? C5 C6 1.383(5) . ? C5 C7 1.510(5) . ? C6 H6 0.9300 . ? C7 C8 1.517(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.382(6) . ? C8 C13 1.390(6) . ? C9 C10 1.390(6) . ? C9 H9 0.9300 . ? C10 C11 1.380(6) . ? C10 C16 1.481(5) . ? C11 C12 1.369(6) . ? C11 H11 0.9300 . ? C12 C13 1.394(6) . ? C12 C17 1.513(6) . ? C13 H13 0.9300 . ? C14 O2 1.220(5) . ? C14 O1 1.300(5) . ? C15 O4 1.226(5) . ? C15 O3 1.272(5) . ? C16 O6 1.234(4) . ? C16 O5 1.295(5) . ? C17 O7 1.243(5) . ? C17 O8 1.246(5) . ? Mg1 O4 2.032(3) 3_746 ? Mg1 O11 2.050(3) . ? Mg1 O12 2.062(3) . ? Mg1 O2 2.068(3) . ? Mg1 O10 2.070(3) . ? Mg1 O9 2.117(3) . ? O1 H1 0.8200 . ? O4 Mg1 2.032(3) 3_756 ? O5 H5 0.8200 . ? O9 H9B 0.8501 . ? O9 H9C 0.8500 . ? O10 H10A 0.8500 . ? O10 H10B 0.8500 . ? O11 H11A 0.8500 . ? O11 H11B 0.8501 . ? O12 H12A 0.8501 . ? O12 H12B 0.8500 . ? O13 H13A 0.8500 . ? O13 H13C 0.8499 . ? O14 H14A 0.8500 . ? O14 H14C 0.8501 . ? O15 H15A 0.8500 . ? O15 H15C 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.2(4) . . ? C2 C1 C14 118.2(4) . . ? C6 C1 C14 121.5(4) . . ? C1 C2 C3 120.2(4) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 C15 122.1(4) . . ? C4 C3 C15 118.5(4) . . ? C5 C4 C3 120.7(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 118.2(4) . . ? C6 C5 C7 120.3(3) . . ? C4 C5 C7 121.5(3) . . ? C1 C6 C5 121.3(4) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C5 C7 C8 112.4(3) . . ? C5 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C5 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C13 118.9(4) . . ? C9 C8 C7 121.0(4) . . ? C13 C8 C7 120.1(4) . . ? C8 C9 C10 120.7(4) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 119.2(4) . . ? C11 C10 C16 120.3(4) . . ? C9 C10 C16 120.4(3) . . ? C12 C11 C10 121.3(4) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 119.1(4) . . ? C11 C12 C17 122.3(4) . . ? C13 C12 C17 118.6(4) . . ? C8 C13 C12 120.7(4) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? O2 C14 O1 124.1(4) . . ? O2 C14 C1 120.9(4) . . ? O1 C14 C1 115.0(3) . . ? O4 C15 O3 125.2(4) . . ? O4 C15 C3 119.1(4) . . ? O3 C15 C3 115.7(4) . . ? O6 C16 O5 123.7(3) . . ? O6 C16 C10 121.5(3) . . ? O5 C16 C10 114.8(3) . . ? O7 C17 O8 125.5(4) . . ? O7 C17 C12 117.6(4) . . ? O8 C17 C12 117.0(4) . . ? O4 Mg1 O11 93.67(13) 3_746 . ? O4 Mg1 O12 175.27(15) 3_746 . ? O11 Mg1 O12 90.86(13) . . ? O4 Mg1 O2 95.71(12) 3_746 . ? O11 Mg1 O2 90.46(12) . . ? O12 Mg1 O2 85.60(12) . . ? O4 Mg1 O10 89.41(13) 3_746 . ? O11 Mg1 O10 89.89(13) . . ? O12 Mg1 O10 89.24(13) . . ? O2 Mg1 O10 174.83(13) . . ? O4 Mg1 O9 88.14(13) 3_746 . ? O11 Mg1 O9 178.19(13) . . ? O12 Mg1 O9 87.34(13) . . ? O2 Mg1 O9 89.20(12) . . ? O10 Mg1 O9 90.28(12) . . ? C14 O1 H1 109.5 . . ? C14 O2 Mg1 142.0(3) . . ? C15 O4 Mg1 140.3(3) . 3_756 ? C16 O5 H5 109.5 . . ? Mg1 O9 H9B 111.2 . . ? Mg1 O9 H9C 103.0 . . ? H9B O9 H9C 111.1 . . ? Mg1 O10 H10A 113.6 . . ? Mg1 O10 H10B 113.1 . . ? H10A O10 H10B 110.8 . . ? Mg1 O11 H11A 112.1 . . ? Mg1 O11 H11B 112.0 . . ? H11A O11 H11B 109.8 . . ? Mg1 O12 H12A 112.9 . . ? Mg1 O12 H12B 112.8 . . ? H12A O12 H12B 110.5 . . ? H13A O13 H13C 110.1 . . ? H14A O14 H14C 109.8 . . ? H15A O15 H15C 109.9 . . ? 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 O1 H1 O3 0.82 1.68 2.466(4) 160.8 3_746 O5 H5 O8 0.82 1.76 2.506(4) 150.0 3_755 O9 H9B O6 0.85 1.96 2.785(4) 164.6 4_556 O9 H9C O13 0.85 1.92 2.712(4) 153.8 1_655 O10 H10A O15 0.85 2.10 2.848(4) 147.3 1_656 O10 H10B O13 0.85 2.12 2.780(4) 134.0 4_557 O11 H11A O6 0.85 2.06 2.859(4) 156.3 4_456 O11 H11B O7 0.85 1.86 2.653(4) 154.2 2_655 O12 H12A O15 0.85 2.19 2.881(4) 138.2 4_556 O12 H12B O9 0.85 2.09 2.834(4) 145.4 4_457 O13 H13A O8 0.85 1.91 2.732(4) 160.8 4_456 O13 H13C O14 0.85 1.97 2.772(4) 158.0 3_656 O14 H14A O7 0.85 1.89 2.703(4) 160.1 . O14 H14C O1 0.85 2.36 3.092(4) 145.0 . O15 H15A O3 0.85 2.06 2.865(4) 158.7 4_456 O15 H15C O14 0.85 2.03 2.825(5) 155.9 2_654 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.212 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.049 # Attachment '2.cif.txt' data_Ca _database_code_depnum_ccdc_archive 'CCDC 651545' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H16 Ca2 O12, C H4 O, 4(H2 O)' _chemical_formula_sum 'C18 H28 Ca2 O17' _chemical_formula_weight 596.56 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 19.436(18) _cell_length_b 13.549(13) _cell_length_c 20.662(19) _cell_angle_alpha 90.00 _cell_angle_beta 116.932(17) _cell_angle_gamma 90.00 _cell_volume 4851(8) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 868 _cell_measurement_theta_min 2.458 _cell_measurement_theta_max 27.846 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8515 _exptl_absorpt_correction_T_max 0.8879 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12664 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4744 _reflns_number_gt 3681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0461P)^2^+7.7043P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4744 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.36568(17) 0.0414(2) 0.19122(18) 0.0386(7) Uani 1 1 d . . . C2 C 0.34781(17) 0.1273(2) 0.21630(17) 0.0372(7) Uani 1 1 d . . . H2 H 0.3157 0.1254 0.2387 0.045 Uiso 1 1 calc R . . C3 C 0.37797(17) 0.2166(2) 0.20796(17) 0.0378(7) Uani 1 1 d . . . C4 C 0.42207(16) 0.2198(2) 0.17127(16) 0.0363(7) Uani 1 1 d . . . H4 H 0.4392 0.2804 0.1630 0.044 Uiso 1 1 calc R . . C5 C 0.4414(2) 0.1333(2) 0.14631(18) 0.0460(8) Uani 1 1 d . . . C6 C 0.41371(18) 0.0448(3) 0.15817(18) 0.0420(7) Uani 1 1 d . . . H6 H 0.4276 -0.0137 0.1437 0.050 Uiso 1 1 calc R . . C7 C 0.48803(17) 0.1352(2) 0.10378(17) 0.0376(7) Uani 1 1 d . . . H7A H 0.5177 0.1958 0.1145 0.045 Uiso 1 1 calc R . . H7B H 0.5240 0.0803 0.1189 0.045 Uiso 1 1 calc R . . C8 C 0.43644(19) 0.1286(3) 0.02304(18) 0.0431(8) Uani 1 1 d . . . C9 C 0.41624(18) 0.2128(2) -0.01967(17) 0.0401(7) Uani 1 1 d . . . H9 H 0.4352 0.2737 0.0016 0.048 Uiso 1 1 calc R . . C10 C 0.36810(17) 0.2076(2) -0.09374(17) 0.0388(7) Uani 1 1 d . . . C11 C 0.33624(18) 0.1177(2) -0.12603(18) 0.0402(7) Uani 1 1 d . . . H11 H 0.3030 0.1145 -0.1755 0.048 Uiso 1 1 calc R . . C12 C 0.35467(18) 0.0328(2) -0.08361(18) 0.0389(7) Uani 1 1 d . . . C13 C 0.40585(17) 0.0394(2) -0.01037(17) 0.0371(7) Uani 1 1 d . . . H13 H 0.4201 -0.0181 0.0172 0.044 Uiso 1 1 calc R . . C14 C 0.32963(19) -0.0555(2) 0.19561(18) 0.0404(7) Uani 1 1 d . . . C15 C 0.36067(16) 0.3085(2) 0.23919(16) 0.0327(6) Uani 1 1 d . . . C16 C 0.35003(18) 0.2988(2) -0.14029(18) 0.0402(7) Uani 1 1 d . . . C17 C 0.31798(18) -0.0644(2) -0.11698(18) 0.0383(7) Uani 1 1 d . . . C18 C 0.26921(18) 0.3789(2) 0.99361(18) 0.0378(7) Uani 1 1 d . . . H18A H 0.2977 0.3407 1.0367 0.057 Uiso 1 1 calc R . . H18B H 0.2502 0.3362 0.9520 0.057 Uiso 1 1 calc R . . H18C H 0.2266 0.4106 0.9966 0.057 Uiso 1 1 calc R . . Ca1 Ca 0.25342(4) -0.24453(5) 0.17113(4) 0.04155(18) Uani 1 1 d . . . Ca2 Ca 0.16060(4) 0.00807(5) 0.21055(4) 0.04079(18) Uani 1 1 d . . . O1 O 0.36352(14) -0.13381(18) 0.19675(12) 0.0485(6) Uani 1 1 d . . . O2 O 0.26574(13) -0.05461(17) 0.19671(12) 0.0435(5) Uani 1 1 d . . . O3 O 0.33347(13) 0.29892(16) 0.28303(13) 0.0482(6) Uani 1 1 d . . . O4 O 0.37499(14) 0.39161(18) 0.22116(13) 0.0507(6) Uani 1 1 d . . . O5 O 0.36292(12) 0.38256(16) -0.10900(11) 0.0386(5) Uani 1 1 d . . . O6 O 0.32463(13) 0.29177(15) -0.20749(12) 0.0427(5) Uani 1 1 d . . . O7 O 0.25987(13) -0.06439(17) -0.17801(12) 0.0468(6) Uani 1 1 d . . . O8 O 0.34641(13) -0.14347(16) -0.08294(12) 0.0433(5) Uani 1 1 d . . . O9 O 0.19899(13) -0.15285(15) 0.05710(11) 0.0419(5) Uani 1 1 d . . . H9A H 0.1504 -0.1532 0.0416 0.050 Uiso 1 1 d R . . H9B H 0.2079 -0.1888 0.0280 0.050 Uiso 1 1 d R . . O10 O 0.32966(13) -0.31857(16) 0.11924(12) 0.0426(5) Uani 1 1 d . . . H10A H 0.3028 -0.3626 0.0891 0.051 Uiso 1 1 d R . . H10B H 0.3690 -0.3465 0.1524 0.051 Uiso 1 1 d R . . O11 O 0.05892(14) -0.07466(18) 0.10626(13) 0.0577(7) Uani 1 1 d . . . H11A H 0.0155 -0.0692 0.1066 0.069 Uiso 1 1 d R . . H11B H 0.0676 -0.1334 0.0974 0.069 Uiso 1 1 d R . . O12 O 0.05002(13) 0.08727(16) 0.20814(12) 0.0433(5) Uani 1 1 d . . . H12C H 0.0090 0.0639 0.1741 0.052 Uiso 1 1 d R . . H12B H 0.0531 0.1487 0.2016 0.052 Uiso 1 1 d R . . O13 O 0.40542(13) 0.50060(19) 0.12892(13) 0.0505(6) Uani 1 1 d . . . H13D H 0.4008 0.4939 0.1677 0.061 Uiso 1 1 d R . . H13B H 0.3653 0.4786 0.0930 0.061 Uiso 1 1 d R . . O14 O 0.31767(12) 0.45058(17) 0.98702(12) 0.0440(5) Uani 1 1 d . . . H14A H 0.3354 0.4273 0.9594 0.053 Uiso 1 1 d R . . O15 O 0.41539(13) 0.77560(18) 0.05373(13) 0.0521(7) Uani 1 1 d . . . H15A H 0.3923 0.7985 0.0109 0.063 Uiso 1 1 d R . . H15B H 0.4036 0.8096 0.0818 0.063 Uiso 1 1 d R . . O16 O 0.00206(13) 0.28942(16) 0.18791(12) 0.0467(6) Uani 1 1 d . . . H16C H 0.0023 0.2780 0.2285 0.056 Uiso 1 1 d R . . H16D H 0.0467 0.3087 0.1955 0.056 Uiso 1 1 d R . . O17 O 0.03233(13) 0.91732(18) 0.97659(13) 0.0508(6) Uani 1 1 d . . . H17D H 0.0573 0.9370 0.9543 0.061 Uiso 1 1 d R . . H17B H 0.0258 0.8584 0.9608 0.061 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0320(16) 0.0369(17) 0.0446(18) -0.0004(14) 0.0153(14) 0.0004(13) C2 0.0325(16) 0.0399(17) 0.0385(17) -0.0018(13) 0.0157(14) 0.0002(13) C3 0.0332(16) 0.0345(16) 0.0393(17) -0.0022(13) 0.0108(13) 0.0003(13) C4 0.0298(15) 0.0349(16) 0.0363(17) -0.0012(13) 0.0079(13) -0.0023(12) C5 0.0446(19) 0.0396(19) 0.0391(19) -0.0003(14) 0.0061(15) -0.0022(15) C6 0.0370(17) 0.0445(19) 0.0425(18) 0.0000(15) 0.0163(14) 0.0011(14) C7 0.0265(15) 0.0416(18) 0.0381(17) -0.0014(14) 0.0090(13) -0.0028(13) C8 0.0410(18) 0.0429(19) 0.0390(18) 0.0007(14) 0.0126(15) -0.0017(15) C9 0.0373(16) 0.0361(17) 0.0409(18) -0.0020(14) 0.0123(14) -0.0051(13) C10 0.0342(15) 0.0373(17) 0.0394(17) 0.0021(14) 0.0120(13) -0.0002(13) C11 0.0358(17) 0.0391(18) 0.0367(17) -0.0003(14) 0.0087(14) -0.0036(14) C12 0.0375(17) 0.0358(17) 0.0426(18) -0.0024(14) 0.0174(14) -0.0049(13) C13 0.0316(15) 0.0379(17) 0.0423(18) 0.0029(14) 0.0173(14) 0.0012(13) C14 0.0362(17) 0.0393(18) 0.0446(19) -0.0014(15) 0.0172(14) -0.0046(14) C15 0.0274(14) 0.0419(18) 0.0297(15) -0.0051(13) 0.0137(12) -0.0006(12) C16 0.0345(16) 0.0364(17) 0.0433(19) 0.0023(14) 0.0121(14) -0.0033(14) C17 0.0372(17) 0.0373(17) 0.0405(18) -0.0037(14) 0.0179(14) -0.0050(14) C18 0.0401(17) 0.0455(18) 0.0449(19) 0.0067(14) 0.0342(15) -0.0066(14) Ca1 0.0386(3) 0.0421(4) 0.0427(4) -0.0023(3) 0.0174(3) -0.0033(3) Ca2 0.0347(3) 0.0420(4) 0.0428(4) 0.0041(3) 0.0150(3) 0.0009(3) O1 0.0549(15) 0.0451(14) 0.0382(13) -0.0024(10) 0.0148(11) -0.0014(11) O2 0.0453(13) 0.0429(13) 0.0344(12) -0.0033(10) 0.0110(10) -0.0077(10) O3 0.0508(14) 0.0352(12) 0.0489(14) -0.0173(10) 0.0141(12) -0.0075(10) O4 0.0468(14) 0.0483(15) 0.0472(14) -0.0060(12) 0.0125(11) -0.0036(11) O5 0.0414(12) 0.0386(12) 0.0291(11) 0.0007(9) 0.0102(9) -0.0025(9) O6 0.0524(13) 0.0283(11) 0.0375(13) 0.0039(9) 0.0118(10) -0.0050(10) O7 0.0421(13) 0.0459(14) 0.0435(13) -0.0052(10) 0.0114(11) -0.0090(10) O8 0.0508(13) 0.0372(13) 0.0331(12) 0.0002(10) 0.0115(10) -0.0032(10) O9 0.0481(13) 0.0380(12) 0.0318(11) 0.0021(9) 0.0112(10) -0.0197(10) O10 0.0437(12) 0.0395(12) 0.0438(13) -0.0176(10) 0.0191(10) -0.0082(10) O11 0.0506(14) 0.0459(14) 0.0499(15) 0.0010(11) -0.0008(12) -0.0170(12) O12 0.0413(12) 0.0402(13) 0.0432(13) 0.0101(10) 0.0146(10) 0.0079(10) O13 0.0448(13) 0.0669(16) 0.0545(14) -0.0009(12) 0.0354(12) -0.0169(12) O14 0.0398(12) 0.0503(14) 0.0388(13) -0.0045(10) 0.0152(10) -0.0015(10) O15 0.0434(13) 0.0623(17) 0.0458(14) 0.0197(12) 0.0160(11) -0.0148(11) O16 0.0474(13) 0.0383(12) 0.0479(14) -0.0162(10) 0.0158(11) 0.0020(10) O17 0.0464(14) 0.0470(14) 0.0463(14) 0.0122(11) 0.0098(11) 0.0190(11) _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 C1 C2 1.381(4) . ? C1 C6 1.384(4) . ? C1 C14 1.510(5) . ? C2 C3 1.388(4) . ? C2 H2 0.9300 . ? C3 C4 1.378(5) . ? C3 C15 1.509(4) . ? C4 C5 1.399(5) . ? C4 H4 0.9300 . ? C5 C6 1.381(5) . ? C5 C7 1.521(5) . ? C6 H6 0.9300 . ? C7 C8 1.510(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.385(5) . ? C8 C13 1.386(5) . ? C9 C10 1.388(5) . ? C9 H9 0.9300 . ? C10 C11 1.391(5) . ? C10 C16 1.507(4) . ? C11 C12 1.391(4) . ? C11 H11 0.9300 . ? C12 C13 1.387(5) . ? C12 C17 1.508(4) . ? C13 H13 0.9300 . ? C14 O1 1.243(4) . ? C14 O2 1.252(4) . ? C14 Ca1 2.886(4) . ? C15 O3 1.245(4) . ? C15 O4 1.257(4) . ? C15 Ca2 2.992(4) 4 ? C16 O6 1.249(4) . ? C16 O5 1.273(4) . ? C16 Ca2 2.954(4) 7 ? C17 O7 1.255(4) . ? C17 O8 1.263(4) . ? C17 Ca1 2.911(4) 7_545 ? C18 O14 1.402(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? Ca1 O6 2.339(3) 6_556 ? Ca1 O3 2.355(3) 4_545 ? Ca1 O10 2.406(3) . ? Ca1 O9 2.440(3) . ? Ca1 O1 2.466(3) . ? Ca1 O8 2.487(3) 7_545 ? Ca1 O7 2.612(3) 7_545 ? Ca1 O2 2.616(3) . ? Ca1 C17 2.911(4) 7_545 ? Ca1 Ca2 4.038(3) 4_545 ? Ca1 Ca2 4.118(3) . ? Ca1 H9B 2.7804 . ? Ca2 O2 2.347(3) . ? Ca2 O7 2.363(3) 6_556 ? Ca2 O12 2.382(3) . ? Ca2 O4 2.417(3) 4_545 ? Ca2 O5 2.437(3) 7 ? Ca2 O11 2.439(3) . ? Ca2 O6 2.731(3) 7 ? Ca2 O3 2.837(4) 4_545 ? Ca2 C16 2.954(4) 7 ? Ca2 C15 2.992(4) 4_545 ? Ca2 Ca1 4.038(3) 4 ? Ca2 H12B 2.7716 . ? O3 Ca1 2.355(3) 4 ? O3 Ca2 2.837(4) 4 ? O4 Ca2 2.417(3) 4 ? O5 Ca2 2.437(3) 7 ? O6 Ca1 2.339(3) 6 ? O6 Ca2 2.731(3) 7 ? O7 Ca2 2.363(3) 6 ? O7 Ca1 2.612(3) 7_545 ? O8 Ca1 2.487(3) 7_545 ? O9 H9A 0.8498 . ? O9 H9B 0.8502 . ? O10 H10A 0.8499 . ? O10 H10B 0.8503 . ? O11 H11A 0.8504 . ? O11 H11B 0.8496 . ? O12 H12C 0.8501 . ? O12 H12B 0.8499 . ? O13 H13D 0.8504 . ? O13 H13B 0.8499 . ? O14 H14A 0.8499 . ? O15 H15A 0.8499 . ? O15 H15B 0.8501 . ? O16 H16C 0.8501 . ? O16 H16D 0.8500 . ? O17 H17D 0.8500 . ? O17 H17B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.8(3) . . ? C2 C1 C14 120.5(3) . . ? C6 C1 C14 119.6(3) . . ? C1 C2 C3 119.7(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 C15 121.6(3) . . ? C2 C3 C15 118.5(3) . . ? C3 C4 C5 120.9(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 118.1(3) . . ? C6 C5 C7 119.9(3) . . ? C4 C5 C7 121.9(3) . . ? C5 C6 C1 121.4(3) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? C8 C7 C5 111.5(3) . . ? C8 C7 H7A 109.3 . . ? C5 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? C5 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C13 117.8(3) . . ? C9 C8 C7 120.6(3) . . ? C13 C8 C7 121.5(3) . . ? C8 C9 C10 121.1(3) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C11 120.3(3) . . ? C9 C10 C16 120.5(3) . . ? C11 C10 C16 119.2(3) . . ? C12 C11 C10 119.3(3) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C13 C12 C11 119.2(3) . . ? C13 C12 C17 120.8(3) . . ? C11 C12 C17 120.1(3) . . ? C8 C13 C12 122.2(3) . . ? C8 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? O1 C14 O2 122.0(3) . . ? O1 C14 C1 119.1(3) . . ? O2 C14 C1 118.9(3) . . ? O1 C14 Ca1 58.11(18) . . ? O2 C14 Ca1 65.01(17) . . ? C1 C14 Ca1 167.5(2) . . ? O3 C15 O4 122.2(3) . . ? O3 C15 C3 118.4(3) . . ? O4 C15 C3 119.4(3) . . ? O3 C15 Ca2 70.77(17) . 4 ? O4 C15 Ca2 51.45(17) . 4 ? C3 C15 Ca2 170.7(2) . 4 ? O6 C16 O5 121.4(3) . . ? O6 C16 C10 120.5(3) . . ? O5 C16 C10 118.1(3) . . ? O6 C16 Ca2 67.48(17) . 7 ? O5 C16 Ca2 54.13(16) . 7 ? C10 C16 Ca2 169.9(2) . 7 ? O7 C17 O8 121.8(3) . . ? O7 C17 C12 118.9(3) . . ? O8 C17 C12 119.3(3) . . ? O7 C17 Ca1 63.81(17) . 7_545 ? O8 C17 Ca1 58.12(17) . 7_545 ? C12 C17 Ca1 175.6(2) . 7_545 ? O14 C18 H18A 109.5 . . ? O14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O6 Ca1 O3 79.69(10) 6_556 4_545 ? O6 Ca1 O10 100.31(10) 6_556 . ? O3 Ca1 O10 169.10(8) 4_545 . ? O6 Ca1 O9 164.10(8) 6_556 . ? O3 Ca1 O9 100.65(10) 4_545 . ? O10 Ca1 O9 82.37(10) . . ? O6 Ca1 O1 84.36(9) 6_556 . ? O3 Ca1 O1 118.18(10) 4_545 . ? O10 Ca1 O1 72.53(10) . . ? O9 Ca1 O1 81.50(8) . . ? O6 Ca1 O8 120.33(9) 6_556 7_545 ? O3 Ca1 O8 89.05(11) 4_545 7_545 ? O10 Ca1 O8 81.53(10) . 7_545 ? O9 Ca1 O8 75.52(9) . 7_545 ? O1 Ca1 O8 147.30(9) . 7_545 ? O6 Ca1 O7 72.27(7) 6_556 7_545 ? O3 Ca1 O7 96.85(8) 4_545 7_545 ? O10 Ca1 O7 72.97(8) . 7_545 ? O9 Ca1 O7 123.14(8) . 7_545 ? O1 Ca1 O7 133.53(9) . 7_545 ? O8 Ca1 O7 51.06(8) 7_545 7_545 ? O6 Ca1 O2 95.56(8) 6_556 . ? O3 Ca1 O2 71.91(8) 4_545 . ? O10 Ca1 O2 118.79(8) . . ? O9 Ca1 O2 69.78(8) . . ? O1 Ca1 O2 50.75(8) . . ? O8 Ca1 O2 135.88(8) 7_545 . ? O7 Ca1 O2 165.06(8) 7_545 . ? O6 Ca1 C14 92.72(9) 6_556 . ? O3 Ca1 C14 96.45(10) 4_545 . ? O10 Ca1 C14 94.43(10) . . ? O9 Ca1 C14 71.41(9) . . ? O1 Ca1 C14 25.33(8) . . ? O8 Ca1 C14 146.93(9) 7_545 . ? O7 Ca1 C14 157.74(9) 7_545 . ? O2 Ca1 C14 25.72(8) . . ? O6 Ca1 C17 96.68(10) 6_556 7_545 ? O3 Ca1 C17 94.18(10) 4_545 7_545 ? O10 Ca1 C17 74.97(10) . 7_545 ? O9 Ca1 C17 99.14(10) . 7_545 ? O1 Ca1 C17 147.11(9) . 7_545 ? O8 Ca1 C17 25.55(8) 7_545 7_545 ? O7 Ca1 C17 25.54(8) 7_545 7_545 ? O2 Ca1 C17 159.48(9) . 7_545 ? C14 Ca1 C17 166.91(10) . 7_545 ? O6 Ca1 Ca2 40.71(5) 6_556 4_545 ? O3 Ca1 Ca2 98.02(7) 4_545 4_545 ? O10 Ca1 Ca2 75.77(8) . 4_545 ? O9 Ca1 Ca2 152.46(6) . 4_545 ? O1 Ca1 Ca2 107.10(8) . 4_545 ? O8 Ca1 Ca2 84.76(8) 7_545 4_545 ? O7 Ca1 Ca2 33.72(6) 7_545 4_545 ? O2 Ca1 Ca2 136.00(7) . 4_545 ? C14 Ca1 Ca2 126.27(9) . 4_545 ? C17 Ca1 Ca2 59.27(9) 7_545 4_545 ? O6 Ca1 Ca2 96.59(7) 6_556 . ? O3 Ca1 Ca2 41.80(6) 4_545 . ? O10 Ca1 Ca2 147.98(6) . . ? O9 Ca1 Ca2 74.38(8) . . ? O1 Ca1 Ca2 82.38(9) . . ? O8 Ca1 Ca2 112.68(8) 7_545 . ? O7 Ca1 Ca2 138.58(7) 7_545 . ? O2 Ca1 Ca2 31.88(6) . . ? C14 Ca1 Ca2 57.59(9) . . ? C17 Ca1 Ca2 129.77(9) 7_545 . ? Ca2 Ca1 Ca2 131.94(5) 4_545 . ? O6 Ca1 H9B 164.5 6_556 . ? O3 Ca1 H9B 114.8 4_545 . ? O10 Ca1 H9B 66.6 . . ? O9 Ca1 H9B 17.2 . . ? O1 Ca1 H9B 83.7 . . ? O8 Ca1 H9B 67.6 7_545 . ? O7 Ca1 H9B 109.6 7_545 . ? O2 Ca1 H9B 84.5 . . ? C14 Ca1 H9B 80.6 . . ? C17 Ca1 H9B 88.1 7_545 . ? Ca2 Ca1 H9B 135.6 4_545 . ? Ca2 Ca1 H9B 91.6 . . ? O2 Ca2 O7 82.17(10) . 6_556 ? O2 Ca2 O12 170.91(8) . . ? O7 Ca2 O12 101.87(10) 6_556 . ? O2 Ca2 O4 109.28(10) . 4_545 ? O7 Ca2 O4 88.01(11) 6_556 4_545 ? O12 Ca2 O4 79.18(10) . 4_545 ? O2 Ca2 O5 87.09(9) . 7 ? O7 Ca2 O5 113.24(10) 6_556 7 ? O12 Ca2 O5 83.83(8) . 7 ? O4 Ca2 O5 155.21(9) 4_545 7 ? O2 Ca2 O11 97.35(11) . . ? O7 Ca2 O11 170.67(9) 6_556 . ? O12 Ca2 O11 79.99(11) . . ? O4 Ca2 O11 83.35(11) 4_545 . ? O5 Ca2 O11 75.98(10) 7 . ? O2 Ca2 O6 104.48(8) . 7 ? O7 Ca2 O6 69.74(8) 6_556 7 ? O12 Ca2 O6 69.85(9) . 7 ? O4 Ca2 O6 136.27(9) 4_545 7 ? O5 Ca2 O6 49.98(8) 7 7 ? O11 Ca2 O6 119.19(8) . 7 ? O2 Ca2 O3 67.98(8) . 4_545 ? O7 Ca2 O3 106.21(8) 6_556 4_545 ? O12 Ca2 O3 117.91(8) . 4_545 ? O4 Ca2 O3 48.47(9) 4_545 4_545 ? O5 Ca2 O3 129.46(8) 7 4_545 ? O11 Ca2 O3 65.27(8) . 4_545 ? O6 Ca2 O3 172.15(7) 7 4_545 ? O2 Ca2 C16 97.56(9) . 7 ? O7 Ca2 C16 92.14(10) 6_556 7 ? O12 Ca2 C16 74.28(9) . 7 ? O4 Ca2 C16 152.91(9) 4_545 7 ? O5 Ca2 C16 25.05(8) 7 7 ? O11 Ca2 C16 97.16(10) . 7 ? O6 Ca2 C16 24.99(8) 7 7 ? O3 Ca2 C16 154.18(9) 4_545 7 ? O2 Ca2 C15 88.86(9) . 4_545 ? O7 Ca2 C15 97.69(10) 6_556 4_545 ? O12 Ca2 C15 98.58(9) . 4_545 ? O4 Ca2 C15 23.99(8) 4_545 4_545 ? O5 Ca2 C15 147.88(8) 7 4_545 ? O11 Ca2 C15 72.97(10) . 4_545 ? O6 Ca2 C15 159.74(8) 7 4_545 ? O3 Ca2 C15 24.49(8) 4_545 4_545 ? C16 Ca2 C15 168.92(8) 7 4_545 ? O2 Ca2 Ca1 103.28(7) . 4 ? O7 Ca2 Ca1 37.86(6) 6_556 4 ? O12 Ca2 Ca1 76.16(8) . 4 ? O4 Ca2 Ca1 109.74(9) 4_545 4 ? O5 Ca2 Ca1 83.18(9) 7 4 ? O11 Ca2 Ca1 149.77(7) . 4 ? O6 Ca2 Ca1 33.96(6) 7 4 ? O3 Ca2 Ca1 143.52(6) 4_545 4 ? C16 Ca2 Ca1 58.66(9) 7 4 ? C15 Ca2 Ca1 128.65(9) 4_545 4 ? O2 Ca2 Ca1 36.06(6) . . ? O7 Ca2 Ca1 102.92(8) 6_556 . ? O12 Ca2 Ca1 147.35(6) . . ? O4 Ca2 Ca1 80.79(9) 4_545 . ? O5 Ca2 Ca1 105.26(8) 7 . ? O11 Ca2 Ca1 72.28(9) . . ? O6 Ca2 Ca1 139.51(7) 7 . ? O3 Ca2 Ca1 33.59(6) 4_545 . ? C16 Ca2 Ca1 125.33(9) 7 . ? C15 Ca2 Ca1 57.27(8) 4_545 . ? Ca1 Ca2 Ca1 135.34(5) 4 . ? O2 Ca2 H12B 155.8 . . ? O7 Ca2 H12B 95.8 6_556 . ? O12 Ca2 H12B 16.9 . . ? O4 Ca2 H12B 94.7 4_545 . ? O5 Ca2 H12B 71.5 7 . ? O11 Ca2 H12B 88.4 . . ? O6 Ca2 H12B 53.1 7 . ? O3 Ca2 H12B 134.7 4_545 . ? C16 Ca2 H12B 58.4 7 . ? C15 Ca2 H12B 115.2 4_545 . ? Ca1 Ca2 H12B 64.1 4 . ? Ca1 Ca2 H12B 160.5 . . ? C14 O1 Ca1 96.6(2) . . ? C14 O2 Ca2 158.6(2) . . ? C14 O2 Ca1 89.28(19) . . ? Ca2 O2 Ca1 112.05(9) . . ? C15 O3 Ca1 159.5(2) . 4 ? C15 O3 Ca2 84.75(19) . 4 ? Ca1 O3 Ca2 104.61(9) 4 4 ? C15 O4 Ca2 104.6(2) . 4 ? C16 O5 Ca2 100.8(2) . 7 ? C16 O6 Ca1 163.1(2) . 6 ? C16 O6 Ca2 87.53(18) . 7 ? Ca1 O6 Ca2 105.33(8) 6 7 ? C17 O7 Ca2 160.9(2) . 6 ? C17 O7 Ca1 90.65(19) . 7_545 ? Ca2 O7 Ca1 108.42(9) 6 7_545 ? C17 O8 Ca1 96.33(19) . 7_545 ? Ca1 O9 H9A 106.4 . . ? Ca1 O9 H9B 104.7 . . ? H9A O9 H9B 106.1 . . ? Ca1 O10 H10A 108.7 . . ? Ca1 O10 H10B 109.7 . . ? H10A O10 H10B 108.0 . . ? Ca2 O11 H11A 111.3 . . ? Ca2 O11 H11B 117.4 . . ? H11A O11 H11B 112.1 . . ? Ca2 O12 H12C 110.4 . . ? Ca2 O12 H12B 108.5 . . ? H12C O12 H12B 109.9 . . ? H13D O13 H13B 109.8 . . ? C18 O14 H14A 107.6 . . ? H15A O15 H15B 109.5 . . ? H16C O16 H16D 108.9 . . ? H17D O17 H17B 96.3 . . ? 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 O9 H9A O17 0.85 2.28 3.047(4) 150.6 1_544 O12 H12C O13 0.85 1.99 2.791(4) 156.8 3_445 O12 H12B O16 0.85 2.11 2.862(4) 147.6 . O13 H13D O4 0.85 1.97 2.680(4) 139.8 . O13 H13B O14 0.85 1.99 2.727(4) 144.4 1_554 O14 H14A O5 0.85 1.83 2.672(4) 173.2 1_556 O15 H15A O8 0.85 1.90 2.747(4) 175.9 1_565 O16 H16C O16 0.85 1.77 2.603(5) 164.3 2 O17 H17B O15 0.85 2.24 2.972(4) 144.8 7_566 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.257 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.055 # Attachment '3.cif.txt' data_Sr _database_code_depnum_ccdc_archive 'CCDC 651546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H22 O15 Sr2, 2(H2 O)' _chemical_formula_sum 'C17 H26 O17 Sr2' _chemical_formula_weight 677.62 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' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.852(2) _cell_length_b 12.688(3) _cell_length_c 17.865(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.793(4) _cell_angle_gamma 90.00 _cell_volume 2459.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 905 _cell_measurement_theta_min 2.281 _cell_measurement_theta_max 27.020 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 4.418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.262 _exptl_absorpt_correction_T_max 0.342 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12858 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4818 _reflns_number_gt 3460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0777P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4818 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 C1 C -0.0306(5) 0.3521(4) 0.4109(3) 0.0439(12) Uani 1 1 d . . . C2 C 0.0746(5) 0.4127(4) 0.4235(3) 0.0452(12) Uani 1 1 d . . . H2 H 0.1011 0.4577 0.3859 0.054 Uiso 1 1 calc R . . C3 C 0.1406(5) 0.4083(4) 0.4896(3) 0.0424(12) Uani 1 1 d . . . C4 C 0.0993(5) 0.3410(4) 0.5451(3) 0.0428(12) Uani 1 1 d . . . H4 H 0.1409 0.3387 0.5909 0.051 Uiso 1 1 calc R . . C5 C -0.0022(5) 0.2775(4) 0.5335(3) 0.0445(12) Uani 1 1 d . . . C6 C -0.0671(5) 0.2821(4) 0.4664(3) 0.0465(13) Uani 1 1 d . . . H6 H -0.1350 0.2386 0.4584 0.056 Uiso 1 1 calc R . . C7 C -0.1035(5) 0.3577(4) 0.3396(3) 0.0450(12) Uani 1 1 d . . . C8 C 0.2537(4) 0.4734(4) 0.5010(3) 0.0440(13) Uani 1 1 d . . . H8A H 0.2410 0.5203 0.5430 0.053 Uiso 1 1 calc R . . H8B H 0.2656 0.5167 0.4569 0.053 Uiso 1 1 calc R . . C9 C -0.0447(5) 0.2013(5) 0.5908(3) 0.0460(13) Uani 1 1 d . . . C10 C 0.5392(5) 0.3598(4) 0.5967(3) 0.0452(12) Uani 1 1 d . . . C11 C 0.4312(5) 0.4164(4) 0.5830(3) 0.0435(12) Uani 1 1 d . . . H11 H 0.4000 0.4594 0.6204 0.052 Uiso 1 1 calc R . . C12 C 0.3700(5) 0.4099(4) 0.5155(3) 0.0450(12) Uani 1 1 d . . . C13 C 0.4169(5) 0.3451(4) 0.4595(3) 0.0446(12) Uani 1 1 d . . . H13 H 0.3776 0.3420 0.4129 0.053 Uiso 1 1 calc R . . C14 C 0.5227(4) 0.2851(4) 0.4732(3) 0.0387(11) Uani 1 1 d . . . C15 C 0.5830(5) 0.2954(4) 0.5417(3) 0.0454(13) Uani 1 1 d . . . H15 H 0.6552 0.2575 0.5505 0.054 Uiso 1 1 calc R . . C16 C 0.6113(5) 0.3712(4) 0.6684(3) 0.0447(12) Uani 1 1 d . . . C17 C 0.5753(5) 0.2125(4) 0.4161(3) 0.0447(13) Uani 1 1 d . . . O1 O -0.0919(3) 0.4394(3) 0.2997(2) 0.0458(9) Uani 1 1 d . . . O2 O -0.1746(3) 0.2844(3) 0.32203(19) 0.0425(8) Uani 1 1 d . . . O3 O -0.0227(3) 0.2175(3) 0.6599(2) 0.0452(8) Uani 1 1 d . . . O4 O -0.1026(3) 0.1205(3) 0.5697(2) 0.0452(8) Uani 1 1 d . . . O5 O 0.6929(3) 0.3044(3) 0.6835(2) 0.0452(9) Uani 1 1 d . . . O6 O 0.5909(3) 0.4472(3) 0.7104(2) 0.0451(9) Uani 1 1 d . . . O7 O 0.6495(3) 0.1430(3) 0.43960(19) 0.0383(8) Uani 1 1 d . . . O8 O 0.5480(3) 0.2219(3) 0.3478(2) 0.0402(8) Uani 1 1 d . . . O9 O -0.3792(3) 0.4503(3) 0.07915(19) 0.0394(8) Uani 1 1 d . . . H9A H -0.3674 0.4125 0.0407 0.047 Uiso 1 1 d R . . H9B H -0.3611 0.5136 0.0682 0.047 Uiso 1 1 d R . . O10 O -0.1818(3) 0.5831(3) 0.1710(2) 0.0443(8) Uani 1 1 d . . . H10A H -0.1900 0.5995 0.1250 0.053 Uiso 1 1 d R . . H10B H -0.1086 0.5971 0.1853 0.053 Uiso 1 1 d R . . O11 O -0.4197(3) 0.4044(3) 0.26832(19) 0.0413(8) Uani 1 1 d . . . H11A H -0.4522 0.4640 0.2590 0.062 Uiso 1 1 d R . . H11B H -0.4704 0.3557 0.2570 0.062 Uiso 1 1 d R . . O12 O -0.0347(3) 0.1079(3) 0.24797(18) 0.0378(8) Uani 1 1 d . . . H12A H -0.0366 0.1586 0.2168 0.045 Uiso 1 1 d R . . H12B H -0.0187 0.0515 0.2244 0.045 Uiso 1 1 d R . . O13 O -0.3757(3) -0.0757(3) 0.3701(2) 0.0467(9) Uani 1 1 d . . . H13B H -0.3766 -0.1247 0.3377 0.056 Uiso 1 1 d R . . H13A H -0.4468 -0.0582 0.3789 0.056 Uiso 1 1 d R . . O14 O -0.1042(3) 0.0300(3) 0.42534(19) 0.0424(8) Uani 1 1 d . . . H14A H -0.0938 0.0776 0.4583 0.051 Uiso 1 1 d R . . H14B H -0.0348 0.0083 0.4101 0.051 Uiso 1 1 d R . . O15 O -0.1731(3) -0.0907(3) 0.2640(2) 0.0432(8) Uani 1 1 d . . . H15A H -0.2264 -0.1393 0.2686 0.052 Uiso 1 1 d R . . H15B H -0.1050 -0.1095 0.2840 0.052 Uiso 1 1 d R . . O16 O -0.2551(3) 0.6272(3) 0.0198(2) 0.0490(9) Uani 1 1 d . . . H16A H -0.2968 0.6526 -0.0166 0.059 Uiso 1 1 d R . . H16C H -0.1847 0.6083 0.0045 0.059 Uiso 1 1 d R . . O17 O 0.6636(3) 0.7417(3) 0.2468(2) 0.0546(11) Uani 1 1 d . . . H17A H 0.6033 0.7299 0.2171 0.066 Uiso 1 1 d R . . H17B H 0.7067 0.6859 0.2500 0.066 Uiso 1 1 d R . . Sr1 Sr -0.23332(4) 0.38300(4) 0.19183(3) 0.04185(14) Uani 1 1 d . . . Sr2 Sr -0.25007(5) 0.09127(4) 0.31458(3) 0.046 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 C1 0.048(3) 0.037(3) 0.047(3) 0.001(2) 0.000(2) 0.002(2) C2 0.053(3) 0.041(3) 0.042(3) 0.002(2) 0.010(2) 0.000(2) C3 0.046(3) 0.046(3) 0.036(3) -0.004(2) 0.000(2) -0.002(2) C4 0.041(3) 0.043(3) 0.044(3) -0.005(2) -0.005(2) 0.000(2) C5 0.047(3) 0.036(3) 0.051(3) -0.002(2) 0.005(2) 0.001(2) C6 0.043(3) 0.048(3) 0.048(3) -0.001(2) 0.001(2) -0.002(2) C7 0.048(3) 0.039(3) 0.047(3) -0.004(2) -0.001(2) 0.002(2) C8 0.048(3) 0.041(3) 0.043(3) 0.004(2) -0.007(2) 0.000(2) C9 0.047(3) 0.050(3) 0.041(3) 0.005(3) 0.000(2) 0.009(3) C10 0.053(3) 0.033(3) 0.050(3) -0.004(2) -0.004(3) 0.000(2) C11 0.052(3) 0.041(3) 0.038(3) -0.001(2) 0.004(2) 0.001(2) C12 0.040(3) 0.047(3) 0.048(3) -0.001(2) -0.007(2) -0.005(2) C13 0.050(3) 0.046(3) 0.038(3) 0.003(2) -0.007(2) -0.002(2) C14 0.039(2) 0.039(3) 0.038(3) -0.005(2) 0.002(2) -0.005(2) C15 0.043(3) 0.040(3) 0.052(3) 0.003(3) -0.005(2) 0.000(2) C16 0.049(3) 0.041(3) 0.043(3) 0.004(3) 0.001(2) -0.003(3) C17 0.042(3) 0.051(3) 0.041(3) -0.002(2) 0.001(2) -0.007(2) O1 0.049(2) 0.041(2) 0.048(2) 0.0105(17) -0.0106(16) -0.0176(17) O2 0.0446(19) 0.040(2) 0.043(2) -0.0021(16) -0.0094(16) -0.0054(16) O3 0.046(2) 0.044(2) 0.045(2) 0.0014(17) -0.0035(16) -0.0084(17) O4 0.051(2) 0.043(2) 0.042(2) 0.0013(17) 0.0025(16) -0.0150(17) O5 0.047(2) 0.045(2) 0.044(2) -0.0007(17) -0.0075(16) 0.0091(16) O6 0.0450(19) 0.039(2) 0.051(2) -0.0094(17) -0.0097(16) 0.0128(16) O7 0.0391(17) 0.0343(18) 0.042(2) -0.0045(15) 0.0047(15) 0.0115(15) O8 0.0317(17) 0.043(2) 0.045(2) -0.0004(16) -0.0048(15) 0.0079(15) O9 0.0382(18) 0.0365(18) 0.0434(19) -0.0021(15) 0.0003(15) -0.0002(15) O10 0.054(2) 0.0374(19) 0.042(2) 0.0042(16) -0.0105(16) -0.0088(16) O11 0.0387(18) 0.040(2) 0.045(2) 0.0060(16) 0.0106(16) 0.0134(15) O12 0.0332(17) 0.047(2) 0.0337(18) 0.0017(15) 0.0064(14) 0.0067(15) O13 0.0409(19) 0.053(2) 0.047(2) -0.0053(17) 0.0095(16) -0.0089(17) O14 0.047(2) 0.044(2) 0.0351(18) -0.0093(15) -0.0160(15) 0.0146(16) O15 0.0326(17) 0.040(2) 0.057(2) -0.0108(17) 0.0060(16) 0.0006(15) O16 0.042(2) 0.051(2) 0.053(2) -0.0009(18) 0.0091(17) -0.0041(17) O17 0.056(2) 0.057(2) 0.050(2) -0.0152(19) -0.0295(19) -0.0015(19) Sr1 0.0390(3) 0.0409(3) 0.0456(3) -0.0006(2) -0.0016(2) -0.0005(2) Sr2 0.048 0.043 0.047 -0.001 -0.001 0.001 _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 C1 C6 1.392(8) . ? C1 C2 1.393(7) . ? C1 C7 1.491(8) . ? C2 C3 1.374(7) . ? C2 H2 0.9300 . ? C3 C4 1.387(7) . ? C3 C8 1.491(7) . ? C4 C5 1.378(7) . ? C4 H4 0.9300 . ? C5 C6 1.382(7) . ? C5 C9 1.487(8) . ? C6 H6 0.9300 . ? C7 O2 1.246(6) . ? C7 O1 1.265(6) . ? C7 Sr1 2.993(5) . ? C8 C12 1.516(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O4 1.257(7) . ? C9 O3 1.270(6) . ? C9 Sr1 2.948(6) 4_566 ? C10 C15 1.368(8) . ? C10 C11 1.393(7) . ? C10 C16 1.499(8) . ? C11 C12 1.370(7) . ? C11 H11 0.9300 . ? C12 C13 1.397(8) . ? C13 C14 1.396(7) . ? C13 H13 0.9300 . ? C14 C15 1.386(7) . ? C14 C17 1.495(7) . ? C15 H15 0.9300 . ? C16 O6 1.243(6) . ? C16 O5 1.252(6) . ? C16 Sr2 3.033(5) 4_666 ? C17 O8 1.257(6) . ? C17 O7 1.262(6) . ? C17 Sr2 3.056(6) 1_655 ? O1 Sr1 2.549(3) . ? O2 Sr2 2.586(3) . ? O2 Sr1 2.710(3) . ? O3 Sr1 2.686(4) 4_566 ? O4 Sr1 2.619(4) 4_566 ? O5 Sr1 2.513(4) 4_666 ? O5 Sr2 2.753(4) 4_666 ? O6 Sr2 2.568(3) 4_666 ? O7 Sr2 2.583(3) 1_655 ? O8 Sr2 2.817(3) 1_655 ? O9 Sr1 2.683(3) . ? O9 H9A 0.8500 . ? O9 H9B 0.8501 . ? O10 Sr1 2.627(3) . ? O10 H10A 0.8499 . ? O10 H10B 0.8500 . ? O11 Sr1 2.471(3) . ? O11 H11A 0.8500 . ? O11 H11B 0.8499 . ? O12 Sr2 2.646(3) . ? O12 H12A 0.8502 . ? O12 H12B 0.8499 . ? O13 Sr2 2.714(4) . ? O13 H13B 0.8501 . ? O13 H13A 0.8200 . ? O14 Sr2 2.634(3) . ? O14 H14A 0.8500 . ? O14 H14B 0.8500 . ? O15 Sr2 2.620(3) . ? O15 H15A 0.8499 . ? O15 H15B 0.8501 . ? O16 H16A 0.8500 . ? O16 H16C 0.8500 . ? O17 H17A 0.8500 . ? O17 H17B 0.8499 . ? Sr1 O5 2.513(4) 4_465 ? Sr1 O4 2.619(4) 4_565 ? Sr1 O3 2.686(4) 4_565 ? Sr1 C9 2.948(6) 4_565 ? Sr1 Sr2 4.3074(11) . ? Sr1 H11A 2.8668 . ? Sr1 H11B 2.8597 . ? Sr2 O6 2.568(3) 4_465 ? Sr2 O7 2.583(3) 1_455 ? Sr2 O5 2.753(4) 4_465 ? Sr2 O8 2.817(3) 1_455 ? Sr2 C16 3.033(5) 4_465 ? Sr2 C17 3.056(6) 1_455 ? 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 C6 C1 C2 118.5(5) . . ? C6 C1 C7 119.1(5) . . ? C2 C1 C7 122.3(5) . . ? C3 C2 C1 122.2(5) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C4 118.0(5) . . ? C2 C3 C8 120.9(5) . . ? C4 C3 C8 121.1(5) . . ? C5 C4 C3 121.2(5) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.2(5) . . ? C4 C5 C9 122.1(5) . . ? C6 C5 C9 117.7(5) . . ? C5 C6 C1 119.9(5) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? O2 C7 O1 122.4(5) . . ? O2 C7 C1 119.9(5) . . ? O1 C7 C1 117.7(5) . . ? O2 C7 Sr1 64.9(3) . . ? O1 C7 Sr1 57.6(3) . . ? C1 C7 Sr1 174.9(4) . . ? C3 C8 C12 114.3(5) . . ? C3 C8 H8A 108.7 . . ? C12 C8 H8A 108.7 . . ? C3 C8 H8B 108.7 . . ? C12 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? O4 C9 O3 120.6(5) . . ? O4 C9 C5 118.8(5) . . ? O3 C9 C5 120.5(5) . . ? O4 C9 Sr1 62.6(3) . 4_566 ? O3 C9 Sr1 65.6(3) . 4_566 ? C5 C9 Sr1 151.9(4) . 4_566 ? C15 C10 C11 118.8(5) . . ? C15 C10 C16 119.3(5) . . ? C11 C10 C16 121.9(5) . . ? C12 C11 C10 121.3(5) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 119.2(5) . . ? C11 C12 C8 120.7(5) . . ? C13 C12 C8 120.0(5) . . ? C14 C13 C12 120.1(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 118.8(5) . . ? C15 C14 C17 118.7(5) . . ? C13 C14 C17 122.5(5) . . ? C10 C15 C14 121.7(5) . . ? C10 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? O6 C16 O5 121.8(5) . . ? O6 C16 C10 119.7(5) . . ? O5 C16 C10 118.5(5) . . ? O6 C16 Sr2 56.6(3) . 4_666 ? O5 C16 Sr2 65.2(3) . 4_666 ? C10 C16 Sr2 176.2(4) . 4_666 ? O8 C17 O7 122.0(5) . . ? O8 C17 C14 121.1(5) . . ? O7 C17 C14 116.8(5) . . ? O8 C17 Sr2 67.2(3) . 1_655 ? O7 C17 Sr2 56.5(3) . 1_655 ? C14 C17 Sr2 164.0(3) . 1_655 ? C7 O1 Sr1 97.6(3) . . ? C7 O2 Sr2 156.2(3) . . ? C7 O2 Sr1 90.5(3) . . ? Sr2 O2 Sr1 108.82(11) . . ? C9 O3 Sr1 88.9(3) . 4_566 ? C9 O4 Sr1 92.2(3) . 4_566 ? C16 O5 Sr1 151.3(3) . 4_666 ? C16 O5 Sr2 90.4(3) . 4_666 ? Sr1 O5 Sr2 109.68(12) 4_666 4_666 ? C16 O6 Sr2 99.6(3) . 4_666 ? C17 O7 Sr2 99.4(3) . 1_655 ? C17 O8 Sr2 88.6(3) . 1_655 ? Sr1 O9 H9A 109.4 . . ? Sr1 O9 H9B 109.7 . . ? H9A O9 H9B 108.1 . . ? Sr1 O10 H10A 110.7 . . ? Sr1 O10 H10B 111.1 . . ? H10A O10 H10B 109.0 . . ? Sr1 O11 H11A 109.3 . . ? Sr1 O11 H11B 108.7 . . ? H11A O11 H11B 109.5 . . ? Sr2 O12 H12A 109.9 . . ? Sr2 O12 H12B 110.1 . . ? H12A O12 H12B 108.4 . . ? Sr2 O13 H13B 108.9 . . ? Sr2 O13 H13A 109.7 . . ? H13B O13 H13A 109.0 . . ? Sr2 O14 H14A 112.5 . . ? Sr2 O14 H14B 112.4 . . ? H14A O14 H14B 110.1 . . ? Sr2 O15 H15A 112.7 . . ? Sr2 O15 H15B 112.4 . . ? H15A O15 H15B 110.1 . . ? H16A O16 H16C 109.5 . . ? H17A O17 H17B 108.3 . . ? O11 Sr1 O5 82.77(12) . 4_465 ? O11 Sr1 O1 92.27(13) . . ? O5 Sr1 O1 119.89(11) 4_465 . ? O11 Sr1 O4 156.83(12) . 4_565 ? O5 Sr1 O4 96.34(12) 4_465 4_565 ? O1 Sr1 O4 107.89(12) . 4_565 ? O11 Sr1 O10 98.61(12) . . ? O5 Sr1 O10 166.96(11) 4_465 . ? O1 Sr1 O10 73.09(11) . . ? O4 Sr1 O10 77.25(12) 4_565 . ? O11 Sr1 O9 84.32(11) . . ? O5 Sr1 O9 94.15(11) 4_465 . ? O1 Sr1 O9 145.15(11) . . ? O4 Sr1 O9 72.63(11) 4_565 . ? O10 Sr1 O9 73.17(10) . . ? O11 Sr1 O3 151.06(11) . 4_565 ? O5 Sr1 O3 79.04(12) 4_465 4_565 ? O1 Sr1 O3 77.80(12) . 4_565 ? O4 Sr1 O3 48.88(11) 4_565 4_565 ? O10 Sr1 O3 104.18(11) . 4_565 ? O9 Sr1 O3 119.13(11) . 4_565 ? O11 Sr1 O2 76.15(11) . . ? O5 Sr1 O2 71.64(11) 4_465 . ? O1 Sr1 O2 49.34(10) . . ? O4 Sr1 O2 125.69(11) 4_565 . ? O10 Sr1 O2 121.33(10) . . ? O9 Sr1 O2 156.99(10) . . ? O3 Sr1 O2 76.84(11) 4_565 . ? O11 Sr1 C9 163.48(14) . 4_565 ? O5 Sr1 C9 81.03(14) 4_465 4_565 ? O1 Sr1 C9 98.55(13) . 4_565 ? O4 Sr1 C9 25.22(13) 4_565 4_565 ? O10 Sr1 C9 96.46(14) . 4_565 ? O9 Sr1 C9 93.66(13) . 4_565 ? O3 Sr1 C9 25.51(13) 4_565 4_565 ? O2 Sr1 C9 101.59(14) . 4_565 ? O11 Sr1 C7 84.43(14) . . ? O5 Sr1 C7 95.54(13) 4_465 . ? O1 Sr1 C7 24.77(13) . . ? O4 Sr1 C7 118.62(13) 4_565 . ? O10 Sr1 C7 97.49(13) . . ? O9 Sr1 C7 164.10(13) . . ? O3 Sr1 C7 75.21(13) 4_565 . ? O2 Sr1 C7 24.60(12) . . ? C9 Sr1 C7 100.28(15) 4_565 . ? O11 Sr1 Sr2 76.83(8) . . ? O5 Sr1 Sr2 37.01(8) 4_465 . ? O1 Sr1 Sr2 83.41(8) . . ? O4 Sr1 Sr2 115.89(8) 4_565 . ? O10 Sr1 Sr2 155.95(8) . . ? O9 Sr1 Sr2 128.82(7) . . ? O3 Sr1 Sr2 75.07(8) 4_565 . ? O2 Sr1 Sr2 34.63(7) . . ? C9 Sr1 Sr2 91.98(12) 4_565 . ? C7 Sr1 Sr2 58.75(11) . . ? O11 Sr1 H11A 16.3 . . ? O5 Sr1 H11A 95.7 4_465 . ? O1 Sr1 H11A 94.4 . . ? O4 Sr1 H11A 144.7 4_565 . ? O10 Sr1 H11A 83.8 . . ? O9 Sr1 H11A 73.5 . . ? O3 Sr1 H11A 166.4 4_565 . ? O2 Sr1 H11A 89.6 . . ? C9 Sr1 H11A 166.6 4_565 . ? C7 Sr1 H11A 93.0 . . ? Sr2 Sr1 H11A 93.1 . . ? O11 Sr1 H11B 16.3 . . ? O5 Sr1 H11B 67.8 4_465 . ? O1 Sr1 H11B 105.2 . . ? O4 Sr1 H11B 146.9 4_565 . ? O10 Sr1 H11B 111.7 . . ? O9 Sr1 H11B 79.6 . . ? O3 Sr1 H11B 143.4 4_565 . ? O2 Sr1 H11B 78.3 . . ? C9 Sr1 H11B 147.3 4_565 . ? C7 Sr1 H11B 92.5 . . ? Sr2 Sr1 H11B 69.2 . . ? H11A Sr1 H11B 28.1 . . ? O6 Sr2 O7 112.79(12) 4_465 1_455 ? O6 Sr2 O2 115.27(11) 4_465 . ? O7 Sr2 O2 81.50(11) 1_455 . ? O6 Sr2 O15 78.28(12) 4_465 . ? O7 Sr2 O15 131.47(11) 1_455 . ? O2 Sr2 O15 138.61(11) . . ? O6 Sr2 O14 151.55(12) 4_465 . ? O7 Sr2 O14 71.46(11) 1_455 . ? O2 Sr2 O14 93.12(11) . . ? O15 Sr2 O14 78.92(11) . . ? O6 Sr2 O12 106.18(11) 4_465 . ? O7 Sr2 O12 138.98(11) 1_455 . ? O2 Sr2 O12 70.50(11) . . ? O15 Sr2 O12 68.13(11) . . ? O14 Sr2 O12 80.56(11) . . ? O6 Sr2 O13 77.32(11) 4_465 . ? O7 Sr2 O13 70.24(11) 1_455 . ? O2 Sr2 O13 151.74(12) . . ? O15 Sr2 O13 66.58(11) . . ? O14 Sr2 O13 78.15(11) . . ? O12 Sr2 O13 132.69(11) . . ? O6 Sr2 O5 48.24(11) 4_465 4_465 ? O7 Sr2 O5 121.38(11) 1_455 4_465 ? O2 Sr2 O5 69.86(11) . 4_465 ? O15 Sr2 O5 101.49(12) . 4_465 ? O14 Sr2 O5 155.04(11) . 4_465 ? O12 Sr2 O5 76.63(10) . 4_465 ? O13 Sr2 O5 125.31(10) . 4_465 ? O6 Sr2 O8 75.36(11) 4_465 1_455 ? O7 Sr2 O8 47.93(10) 1_455 1_455 ? O2 Sr2 O8 71.25(11) . 1_455 ? O15 Sr2 O8 147.52(10) . 1_455 ? O14 Sr2 O8 118.47(10) . 1_455 ? O12 Sr2 O8 137.92(10) . 1_455 ? O13 Sr2 O8 89.21(11) . 1_455 ? O5 Sr2 O8 74.32(11) 4_465 1_455 ? O6 Sr2 C16 23.85(13) 4_465 4_465 ? O7 Sr2 C16 119.61(13) 1_455 4_465 ? O2 Sr2 C16 92.79(13) . 4_465 ? O15 Sr2 C16 89.90(13) . 4_465 ? O14 Sr2 C16 168.18(13) . 4_465 ? O12 Sr2 C16 91.79(13) . 4_465 ? O13 Sr2 C16 101.04(13) . 4_465 ? O5 Sr2 C16 24.39(12) 4_465 4_465 ? O8 Sr2 C16 73.18(13) 1_455 4_465 ? O6 Sr2 C17 96.28(13) 4_465 1_455 ? O7 Sr2 C17 24.04(12) 1_455 1_455 ? O2 Sr2 C17 72.03(13) . 1_455 ? O15 Sr2 C17 148.35(13) . 1_455 ? O14 Sr2 C17 94.25(13) . 1_455 ? O12 Sr2 C17 141.77(13) . 1_455 ? O13 Sr2 C17 81.78(13) . 1_455 ? O5 Sr2 C17 97.40(13) 4_465 1_455 ? O8 Sr2 C17 24.28(12) 1_455 1_455 ? C16 Sr2 C17 97.31(14) 4_465 1_455 ? O6 Sr2 Sr1 80.05(8) 4_465 . ? O7 Sr2 Sr1 104.08(8) 1_455 . ? O2 Sr2 Sr1 36.54(7) . . ? O15 Sr2 Sr1 124.45(9) . . ? O14 Sr2 Sr1 127.37(8) . . ? O12 Sr2 Sr1 70.04(7) . . ? O13 Sr2 Sr1 151.85(8) . . ? O5 Sr2 Sr1 33.32(7) 4_465 . ? O8 Sr2 Sr1 68.90(7) 1_455 . ? C16 Sr2 Sr1 56.69(11) 4_465 . ? C17 Sr2 Sr1 84.29(11) 1_455 . ? 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 O9 H9B O16 0.85 2.04 2.830(5) 153.7 . O10 H10A O16 0.85 2.03 2.861(5) 165.2 . O14 H14A O4 0.85 2.07 2.824(5) 147.9 . O9 H9A O7 0.85 1.95 2.781(5) 166.1 4_465 O10 H10B O12 0.85 1.95 2.761(5) 158.8 2 O11 H11A O6 0.85 1.96 2.676(5) 140.7 3_566 O11 H11B O17 0.85 2.55 3.365(5) 161.7 2_545 O12 H12A O3 0.85 1.88 2.721(5) 170.0 4_565 O16 H16A O13 0.85 2.39 3.031(5) 132.2 4_565 O16 H16C O14 0.85 2.42 3.095(5) 136.4 4_565 O12 H12B O1 0.85 1.91 2.687(5) 150.5 2_545 O13 H13B O17 0.85 2.39 3.230(5) 168.8 1_445 O15 H15A O17 0.85 1.96 2.783(5) 162.3 1_445 O13 H13A O9 0.82 2.04 2.841(5) 163.9 2_445 O14 H14B O4 0.85 2.24 2.946(5) 140.9 3_556 O15 H15B O3 0.85 2.18 2.979(5) 155.7 3_556 O17 H17A O8 0.85 2.00 2.843(4) 171.8 2_655 O17 H17B O10 0.85 2.28 2.961(5) 136.9 1_655 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.420 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.113 # Attachment '4.cif.txt' data_Ba _database_code_depnum_ccdc_archive 'CCDC 651547' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H24 Ba2 O16, 2(H0.80 O0.40), 1.2(H2 O)' _chemical_formula_sum 'C17 H28 Ba2 O18' _chemical_formula_weight 795.07 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 21.440(5) _cell_length_b 13.160(3) _cell_length_c 10.837(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.847(3) _cell_angle_gamma 90.00 _cell_volume 2652.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 922 _cell_measurement_theta_min 3.287 _cell_measurement_theta_max 27.945 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 3.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_T_max 0.48 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6924 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2606 _reflns_number_gt 2118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.07P)^2^+1.77P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2606 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Ba1 Ba 0.187168(19) 0.10245(3) 0.42995(4) 0.03462(15) Uani 1 1 d . . . C1 C 0.0814(3) 0.2133(4) 0.1386(6) 0.0358(13) Uani 1 1 d . . . C2 C 0.0259(3) 0.2852(4) 0.0344(7) 0.0373(14) Uani 1 1 d . . . C3 C 0.0380(3) 0.3464(4) -0.0542(7) 0.0356(13) Uani 1 1 d . . . H3 H 0.0824 0.3436 -0.0499 0.043 Uiso 1 1 calc R . . C4 C -0.0141(3) 0.4121(4) -0.1500(6) 0.0303(12) Uani 1 1 d . . . C5 C -0.0787(3) 0.4177(4) -0.1522(6) 0.0305(12) Uani 1 1 d . . . H5 H -0.1137 0.4626 -0.2148 0.037 Uiso 1 1 calc R . . C6 C -0.0932(3) 0.3577(5) -0.0627(6) 0.0337(12) Uani 1 1 d . . . C7 C -0.0401(3) 0.2925(4) 0.0311(6) 0.0332(13) Uani 1 1 d . . . H7 H -0.0483 0.2530 0.0928 0.040 Uiso 1 1 calc R . . C8 C 0.0000 0.4767(6) -0.2500 0.0301(17) Uani 1 2 d S . . H8A H 0.0413 0.5200 -0.1945 0.036 Uiso 1 1 d R . . C9 C -0.1634(3) 0.3650(4) -0.0649(7) 0.0365(13) Uani 1 1 d . . . O1 O 0.0603(2) 0.1456(3) 0.1909(5) 0.0356(10) Uani 1 1 d . . . O2 O 0.1455(2) 0.2220(3) 0.1685(5) 0.0413(10) Uani 1 1 d . . . O3 O -0.1785(2) 0.2990(3) -0.0017(5) 0.0336(9) Uani 1 1 d . . . O4 O -0.2045(2) 0.4371(3) -0.1314(5) 0.0402(10) Uani 1 1 d . . . O5 O 0.1358(3) -0.0672(4) 0.2441(6) 0.0549(13) Uani 1 1 d . . . H5A H 0.1199 -0.1126 0.2771 0.066 Uiso 1 1 d R . . H5B H 0.1703 -0.0902 0.2348 0.066 Uiso 1 1 d R . . O6 O 0.2635(3) 0.1192(3) 0.7293(5) 0.0494(12) Uani 1 1 d . . . H6A H 0.2909 0.1810 0.7562 0.059 Uiso 1 1 d R . . H6B H 0.2954 0.0622 0.7688 0.059 Uiso 1 1 d R . . O7 O 0.0657(2) 0.0357(4) 0.4495(5) 0.0476(11) Uani 1 1 d . . . H7B H 0.0290 0.0696 0.3917 0.057 Uiso 1 1 d R . . H7C H 0.0732 0.0466 0.5331 0.057 Uiso 1 1 d R . . O8 O 0.2238(2) -0.0874(3) 0.5647(5) 0.0368(10) Uani 1 1 d . . . H8E H 0.1898 -0.1290 0.5171 0.044 Uiso 1 1 d R . . H8C H 0.2306 -0.0804 0.6588 0.044 Uiso 1 1 d R . . O9 O 1.0000 0.8712(6) 0.2500 0.0426(18) Uani 0.80 2 d SP . . H9A H 0.9809 0.8197 0.1971 0.051 Uiso 0.40 1 d PR . . H9B H 1.0103 0.8571 0.3346 0.051 Uiso 0.40 1 d PR . . O10 O 0.1879(4) -0.2569(5) 0.4457(8) 0.0371(16) Uani 0.60 1 d P . . H10A H 0.2056 -0.3037 0.5080 0.045 Uiso 0.60 1 d PR . . H10C H 0.2033 -0.2633 0.3874 0.045 Uiso 0.60 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0306(2) 0.0368(2) 0.0323(2) 0.00004(15) 0.01253(16) 0.00128(14) C1 0.034(3) 0.036(3) 0.033(3) 0.002(2) 0.013(3) 0.003(2) C2 0.033(3) 0.031(3) 0.036(3) 0.003(2) 0.008(3) -0.002(2) C3 0.038(3) 0.033(3) 0.036(3) 0.001(2) 0.019(3) 0.000(2) C4 0.029(3) 0.035(3) 0.032(3) -0.008(2) 0.019(3) -0.005(2) C5 0.026(3) 0.039(3) 0.030(3) 0.001(2) 0.016(2) 0.005(2) C6 0.038(3) 0.035(3) 0.026(3) 0.000(2) 0.015(3) -0.002(2) C7 0.036(3) 0.030(3) 0.029(3) 0.002(2) 0.013(3) -0.003(2) C8 0.040(4) 0.031(4) 0.036(4) 0.000 0.032(4) 0.000 C9 0.033(3) 0.033(3) 0.040(3) 0.003(3) 0.015(3) -0.004(2) O1 0.027(2) 0.0332(19) 0.041(2) 0.0255(18) 0.0129(19) 0.0066(16) O2 0.031(2) 0.043(2) 0.046(3) 0.008(2) 0.016(2) 0.0019(18) O3 0.028(2) 0.036(2) 0.047(2) 0.0156(19) 0.0272(19) 0.0019(16) O4 0.028(2) 0.041(2) 0.058(3) 0.024(2) 0.026(2) 0.0136(17) O5 0.059(3) 0.052(3) 0.053(3) -0.015(2) 0.028(3) 0.000(2) O6 0.054(3) 0.039(2) 0.040(3) 0.009(2) 0.012(2) -0.008(2) O7 0.034(2) 0.063(3) 0.043(3) 0.013(2) 0.016(2) 0.004(2) O8 0.032(2) 0.032(2) 0.040(2) 0.0191(17) 0.0127(19) 0.0028(16) O9 0.037(4) 0.045(4) 0.038(4) 0.000 0.012(4) 0.000 O10 0.050(4) 0.020(3) 0.052(5) 0.009(3) 0.033(4) 0.001(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 Ba1 O1 2.724(4) . ? Ba1 O3 2.733(4) 2 ? Ba1 O4 2.766(4) 8_556 ? Ba1 O8 2.802(4) . ? Ba1 O6 2.822(5) . ? Ba1 O5 2.837(5) . ? Ba1 O7 2.854(4) . ? Ba1 O3 2.898(4) 8_556 ? Ba1 O2 2.964(4) . ? Ba1 C1 3.180(6) . ? Ba1 C9 3.205(6) 8_556 ? Ba1 Ba1 4.5358(10) 7_556 ? C1 O2 1.251(7) . ? C1 O1 1.255(7) . ? C1 C2 1.499(8) . ? C2 C3 1.374(9) . ? C2 C7 1.400(9) . ? C3 C4 1.386(9) . ? C3 H3 0.9300 . ? C4 C5 1.374(8) . ? C4 C8 1.522(7) . ? C5 C6 1.401(9) . ? C5 H5 0.9300 . ? C6 C7 1.384(8) . ? C6 C9 1.496(9) . ? C7 H7 0.9300 . ? C8 C4 1.522(7) 2_554 ? C8 H8A 0.9699 . ? C9 O3 1.245(7) . ? C9 O4 1.250(7) . ? C9 Ba1 3.205(6) 8_455 ? O3 Ba1 2.733(4) 2 ? O3 Ba1 2.898(4) 8_455 ? O4 Ba1 2.766(4) 8_455 ? O5 H5A 0.8499 . ? O5 H5B 0.8500 . ? O6 H6A 0.9600 . ? O6 H6B 0.9598 . ? O7 H7B 0.8501 . ? O7 H7C 0.8500 . ? O8 H8E 0.8501 . ? O8 H8C 0.9600 . ? O9 H9A 0.8499 . ? O9 H9B 0.8500 . ? O10 H10A 0.8501 . ? O10 H10C 0.8499 . ? 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 Ba1 O3 84.05(13) . 2 ? O1 Ba1 O4 111.81(14) . 8_556 ? O3 Ba1 O4 115.49(11) 2 8_556 ? O1 Ba1 O8 124.76(12) . . ? O3 Ba1 O8 137.44(13) 2 . ? O4 Ba1 O8 84.61(14) 8_556 . ? O1 Ba1 O6 144.11(15) . . ? O3 Ba1 O6 71.44(13) 2 . ? O4 Ba1 O6 102.42(15) 8_556 . ? O8 Ba1 O6 67.59(13) . . ? O1 Ba1 O5 68.77(14) . . ? O3 Ba1 O5 152.81(14) 2 . ? O4 Ba1 O5 75.93(14) 8_556 . ? O8 Ba1 O5 65.00(15) . . ? O6 Ba1 O5 132.51(15) . . ? O1 Ba1 O7 67.59(13) . . ? O3 Ba1 O7 94.40(12) 2 . ? O4 Ba1 O7 150.06(13) 8_556 . ? O8 Ba1 O7 73.52(13) . . ? O6 Ba1 O7 88.11(15) . . ? O5 Ba1 O7 76.37(15) . . ? O1 Ba1 O3 123.00(12) . 8_556 ? O3 Ba1 O3 72.73(11) 2 8_556 ? O4 Ba1 O3 45.49(10) 8_556 8_556 ? O8 Ba1 O3 106.29(12) . 8_556 ? O6 Ba1 O3 74.78(13) . 8_556 ? O5 Ba1 O3 121.26(13) . 8_556 ? O7 Ba1 O3 161.06(13) . 8_556 ? O1 Ba1 O2 45.33(11) . . ? O3 Ba1 O2 74.88(13) 2 . ? O4 Ba1 O2 76.06(13) 8_556 . ? O8 Ba1 O2 147.62(13) . . ? O6 Ba1 O2 141.63(12) . . ? O5 Ba1 O2 85.01(15) . . ? O7 Ba1 O2 112.51(12) . . ? O3 Ba1 O2 78.16(12) 8_556 . ? O1 Ba1 C1 22.92(14) . . ? O3 Ba1 C1 74.49(14) 2 . ? O4 Ba1 C1 96.71(16) 8_556 . ? O8 Ba1 C1 143.43(14) . . ? O6 Ba1 C1 145.52(15) . . ? O5 Ba1 C1 79.81(15) . . ? O7 Ba1 C1 89.37(15) . . ? O3 Ba1 C1 100.09(14) 8_556 . ? O2 Ba1 C1 23.16(14) . . ? O1 Ba1 C9 120.34(15) . 8_556 ? O3 Ba1 C9 94.42(13) 2 8_556 ? O4 Ba1 C9 22.68(14) 8_556 8_556 ? O8 Ba1 C9 95.24(14) . 8_556 ? O6 Ba1 C9 88.10(16) . 8_556 ? O5 Ba1 C9 98.57(15) . 8_556 ? O7 Ba1 C9 168.75(14) . 8_556 ? O3 Ba1 C9 22.83(13) 8_556 8_556 ? O2 Ba1 C9 76.61(14) . 8_556 ? C1 Ba1 C9 99.71(16) . 8_556 ? O1 Ba1 Ba1 106.59(9) . 7_556 ? O3 Ba1 Ba1 37.60(7) 2 7_556 ? O4 Ba1 Ba1 79.13(8) 8_556 7_556 ? O8 Ba1 Ba1 128.54(9) . 7_556 ? O6 Ba1 Ba1 68.93(9) . 7_556 ? O5 Ba1 Ba1 150.17(11) . 7_556 ? O7 Ba1 Ba1 130.59(10) . 7_556 ? O3 Ba1 Ba1 35.13(7) 8_556 7_556 ? O2 Ba1 Ba1 73.25(9) . 7_556 ? C1 Ba1 Ba1 87.18(11) . 7_556 ? C9 Ba1 Ba1 57.16(11) 8_556 7_556 ? O2 C1 O1 123.0(5) . . ? O2 C1 C2 119.7(6) . . ? O1 C1 C2 117.3(5) . . ? O2 C1 Ba1 68.7(3) . . ? O1 C1 Ba1 57.7(3) . . ? C2 C1 Ba1 160.7(4) . . ? C3 C2 C7 118.8(5) . . ? C3 C2 C1 122.7(6) . . ? C7 C2 C1 118.4(6) . . ? C2 C3 C4 121.7(6) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 118.6(6) . . ? C5 C4 C8 120.9(5) . . ? C3 C4 C8 120.6(5) . . ? C4 C5 C6 121.8(5) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C7 C6 C5 118.2(6) . . ? C7 C6 C9 120.4(5) . . ? C5 C6 C9 121.4(5) . . ? C6 C7 C2 120.9(6) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C4 C8 C4 112.1(6) . 2_554 ? C4 C8 H8A 109.3 . . ? C4 C8 H8A 109.1 2_554 . ? O3 C9 O4 123.1(6) . . ? O3 C9 C6 118.8(5) . . ? O4 C9 C6 118.1(5) . . ? O3 C9 Ba1 64.6(3) . 8_455 ? O4 C9 Ba1 58.5(3) . 8_455 ? C6 C9 Ba1 176.0(4) . 8_455 ? C1 O1 Ba1 99.4(4) . . ? C1 O2 Ba1 88.2(3) . . ? C9 O3 Ba1 152.9(4) . 2 ? C9 O3 Ba1 92.6(4) . 8_455 ? Ba1 O3 Ba1 107.27(11) 2 8_455 ? C9 O4 Ba1 98.8(3) . 8_455 ? Ba1 O5 H5A 110.4 . . ? Ba1 O5 H5B 108.1 . . ? H5A O5 H5B 110.8 . . ? Ba1 O6 H6A 109.4 . . ? Ba1 O6 H6B 109.2 . . ? H6A O6 H6B 109.5 . . ? Ba1 O7 H7B 109.2 . . ? Ba1 O7 H7C 109.4 . . ? H7B O7 H7C 108.1 . . ? Ba1 O8 H8E 108.9 . . ? Ba1 O8 H8C 108.8 . . ? H8E O8 H8C 109.7 . . ? H9A O9 H9B 109.5 . . ? H10A O10 H10C 109.5 . . ? 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 O8 H8E O10 0.85 1.85 2.500(8) 132.6 . O5 H5A O9 0.85 2.45 3.054(6) 129.0 1_445 O5 H5B O6 0.85 2.07 2.904(7) 168.7 6 O6 H6A O2 0.96 1.74 2.691(6) 168.5 7_556 O6 H6B O4 0.96 1.97 2.730(6) 134.7 3_546 O8 H8C O4 0.96 2.00 2.877(6) 150.3 3_546 O7 H7B O1 0.85 1.94 2.759(6) 162.2 2 O7 H7C O5 0.85 2.01 2.799(7) 154.0 6_556 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.950 _refine_diff_density_min -1.560 _refine_diff_density_rms 0.131 # Attachment '5.cif.txt' data_Mn _database_code_depnum_ccdc_archive 'CCDC 651548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C17 H12 Mn O9), H2 O' _chemical_formula_sum 'C34 H26 Mn2 O19' _chemical_formula_weight 848.43 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3196(17) _cell_length_b 10.067(2) _cell_length_c 11.818(3) _cell_angle_alpha 75.913(3) _cell_angle_beta 75.671(4) _cell_angle_gamma 74.625(4) _cell_volume 798.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 884 _cell_measurement_theta_min 3.054 _cell_measurement_theta_max 28.013 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 0.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7773 _exptl_absorpt_correction_T_max 0.8158 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7344 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3134 _reflns_number_gt 2755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0642P)^2^+0.6542P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3134 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 C1 C -0.0769(5) 0.4598(4) 0.3750(3) 0.0298(7) Uani 1 1 d . . . C2 C 0.1140(5) 0.4490(4) 0.3160(3) 0.0353(8) Uani 1 1 d . . . H2 H 0.1872 0.3632 0.2981 0.042 Uiso 1 1 calc R . . C3 C 0.1961(5) 0.5649(4) 0.2835(3) 0.0318(8) Uani 1 1 d . . . C4 C 0.0857(5) 0.6933(4) 0.3100(3) 0.0366(9) Uani 1 1 d . . . H4 H 0.1404 0.7715 0.2877 0.044 Uiso 1 1 calc R . . C5 C -0.1054(5) 0.7056(4) 0.3695(3) 0.0313(8) Uani 1 1 d . . . C6 C -0.1872(5) 0.5880(4) 0.4016(3) 0.0276(7) Uani 1 1 d . . . H6 H -0.3154 0.5953 0.4408 0.033 Uiso 1 1 calc R . . C7 C 0.4140(5) 0.5551(4) 0.2410(3) 0.0313(8) Uani 1 1 d . . . H7A H 0.4653 0.5710 0.3036 0.038 Uiso 1 1 calc R . . H7B H 0.4753 0.4607 0.2277 0.038 Uiso 1 1 calc R . . C8 C 0.4677(5) 0.6588(4) 0.1275(3) 0.0289(7) Uani 1 1 d . . . C9 C 0.6057(5) 0.7329(4) 0.1164(3) 0.0261(7) Uani 1 1 d . . . H9 H 0.6647 0.7218 0.1803 0.031 Uiso 1 1 calc R . . C10 C 0.6589(5) 0.8238(4) 0.0121(3) 0.0284(7) Uani 1 1 d . . . C11 C 0.5718(5) 0.8400(4) -0.0859(3) 0.0312(8) Uani 1 1 d . . . H11 H 0.6073 0.9001 -0.1569 0.037 Uiso 1 1 calc R . . C12 C 0.4353(5) 0.7665(4) -0.0749(3) 0.0275(7) Uani 1 1 d . . . C13 C 0.3810(5) 0.6763(4) 0.0317(3) 0.0275(7) Uani 1 1 d . . . H13 H 0.2859 0.6277 0.0382 0.033 Uiso 1 1 calc R . . C14 C -0.1650(5) 0.3401(4) 0.3992(3) 0.0267(7) Uani 1 1 d . . . C15 C -0.2133(5) 0.8414(3) 0.4089(3) 0.0251(7) Uani 1 1 d . . . C16 C 0.8069(5) 0.9055(3) 0.0048(3) 0.0254(7) Uani 1 1 d . . . C17 C 0.3449(5) 0.7837(3) -0.1784(3) 0.0272(7) Uani 1 1 d . . . Mn1 Mn 0.32801(8) 0.87811(5) -0.45308(5) 0.02638(17) Uani 1 1 d . . . O1 O -0.0690(4) 0.2338(3) 0.3521(2) 0.0322(6) Uani 1 1 d . . . O2 O -0.3246(4) 0.3381(3) 0.4664(2) 0.0337(6) Uani 1 1 d . . . O3 O -0.3832(4) 0.8535(3) 0.4668(2) 0.0358(6) Uani 1 1 d . . . O4 O -0.1330(4) 0.9453(3) 0.3822(2) 0.0336(6) Uani 1 1 d . . . O5 O 0.8797(3) 0.8876(3) 0.0917(2) 0.0298(6) Uani 1 1 d . . . O6 O 0.8470(3) 0.9883(3) -0.0946(2) 0.0284(5) Uani 1 1 d . . . H6A H 0.9243 1.0458 -0.0953 0.043 Uiso 1 1 d R . . O7 O 0.4220(3) 0.8281(2) -0.2792(2) 0.0265(5) Uani 1 1 d . . . O8 O 0.1796(3) 0.7450(3) -0.1513(2) 0.0285(5) Uani 1 1 d . . . H8 H 0.1245 0.7524 -0.2125 0.043 Uiso 1 1 d R . . O9 O 0.2356(4) 0.9861(3) -0.6164(2) 0.0340(6) Uani 1 1 d . . . H9C H 0.1296 0.9592 -0.5989 0.041 Uiso 1 1 d R . . H9B H 0.1846 1.0734 -0.6254 0.041 Uiso 1 1 d R . . O10 O 0.0000 0.5000 0.0000 0.0324(8) Uani 1 2 d S . . H10C H 0.0948 0.5399 -0.0287 0.049 Uiso 0.50 1 d PR . . H10D H 0.0317 0.4281 0.0522 0.049 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0284(18) 0.0340(18) 0.0274(17) -0.0032(14) -0.0095(14) -0.0059(15) C2 0.0261(18) 0.044(2) 0.0272(17) -0.0013(15) -0.0059(14) 0.0028(15) C3 0.0211(17) 0.0274(17) 0.041(2) -0.0035(15) 0.0013(14) -0.0042(14) C4 0.0281(19) 0.041(2) 0.0254(17) 0.0032(15) -0.0012(14) 0.0052(16) C5 0.0307(18) 0.0298(18) 0.0249(16) 0.0024(14) -0.0062(14) 0.0016(15) C6 0.0222(16) 0.0315(17) 0.0233(16) -0.0023(13) -0.0024(13) -0.0003(13) C7 0.0287(18) 0.0342(19) 0.0224(16) -0.0047(14) 0.0007(13) 0.0019(15) C8 0.0277(17) 0.0278(17) 0.0257(17) -0.0088(14) 0.0008(14) 0.0012(14) C9 0.0200(15) 0.0258(16) 0.0308(17) -0.0048(13) -0.0021(13) -0.0054(13) C10 0.0218(16) 0.0287(17) 0.0285(17) 0.0010(14) -0.0008(13) -0.0047(14) C11 0.0318(19) 0.0242(17) 0.0321(18) 0.0017(14) -0.0048(15) -0.0048(14) C12 0.0214(16) 0.0294(17) 0.0274(17) -0.0047(14) 0.0008(13) -0.0040(13) C13 0.0165(15) 0.0319(18) 0.0309(17) -0.0123(14) 0.0036(13) -0.0020(13) C14 0.0251(17) 0.0329(18) 0.0221(15) 0.0026(13) -0.0193(13) 0.0005(14) C15 0.0244(16) 0.0243(16) 0.0231(15) -0.0051(12) -0.0026(13) -0.0006(13) C16 0.0347(18) 0.0262(16) 0.0227(15) -0.0061(12) -0.0069(13) -0.0163(14) C17 0.0288(17) 0.0204(15) 0.0259(17) -0.0061(13) -0.0091(14) 0.0106(13) Mn1 0.0251(3) 0.0257(3) 0.0239(3) -0.00431(19) -0.00146(19) -0.0014(2) O1 0.0349(13) 0.0240(12) 0.0379(14) -0.0021(10) -0.0118(11) -0.0056(10) O2 0.0256(13) 0.0305(13) 0.0438(15) -0.0009(11) -0.0003(11) -0.0160(10) O3 0.0211(12) 0.0271(13) 0.0512(16) -0.0109(11) 0.0077(11) -0.0021(10) O4 0.0288(13) 0.0284(13) 0.0410(14) -0.0105(11) -0.0033(11) -0.0014(10) O5 0.0233(12) 0.0288(12) 0.0385(14) 0.0087(10) -0.0127(10) -0.0152(10) O6 0.0284(13) 0.0305(12) 0.0297(12) 0.0045(10) -0.0046(10) -0.0222(11) O7 0.0278(12) 0.0231(11) 0.0325(13) -0.0027(9) -0.0103(10) -0.0105(10) O8 0.0191(11) 0.0480(15) 0.0255(12) -0.0105(10) -0.0087(9) -0.0119(10) O9 0.0405(15) 0.0316(13) 0.0304(13) -0.0006(10) -0.0159(11) -0.0051(11) O10 0.0185(16) 0.046(2) 0.0340(18) -0.0107(16) -0.0173(14) 0.0048(15) _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 C1 C2 1.387(5) . ? C1 C6 1.392(5) . ? C1 C14 1.450(5) . ? C2 C3 1.382(5) . ? C2 H2 0.9300 . ? C3 C4 1.392(5) . ? C3 C7 1.533(5) . ? C4 C5 1.389(5) . ? C4 H4 0.9300 . ? C5 C6 1.396(5) . ? C5 C15 1.505(5) . ? C6 H6 0.9300 . ? C7 C8 1.523(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.371(5) . ? C8 C13 1.384(5) . ? C9 C10 1.382(5) . ? C9 H9 0.9300 . ? C10 C11 1.412(5) . ? C10 C16 1.500(5) . ? C11 C12 1.358(5) . ? C11 H11 0.9300 . ? C12 C13 1.399(5) . ? C12 C17 1.483(5) . ? C13 H13 0.9300 . ? C14 O2 1.241(4) . ? C14 O1 1.283(4) . ? C15 O3 1.252(4) . ? C15 O4 1.270(4) . ? C16 O5 1.225(4) . ? C16 O6 1.282(4) . ? C17 O7 1.217(4) . ? C17 O8 1.310(4) . ? Mn1 O3 2.067(2) 1_654 ? Mn1 O9 2.145(2) . ? Mn1 O4 2.165(3) 2_575 ? Mn1 O2 2.227(3) 2_565 ? Mn1 O7 2.227(2) . ? Mn1 O1 2.376(3) 2_565 ? O1 Mn1 2.376(3) 2_565 ? O2 Mn1 2.227(3) 2_565 ? O3 Mn1 2.067(2) 1_456 ? O4 Mn1 2.165(3) 2_575 ? O6 H6A 0.9079 . ? O8 H8 0.8908 . ? O9 H9C 0.8500 . ? O9 H9B 0.8500 . ? O10 H10C 0.8502 . ? O10 H10D 0.8501 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.0(4) . . ? C2 C1 C14 119.5(3) . . ? C6 C1 C14 120.3(3) . . ? C3 C2 C1 120.5(4) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.5(3) . . ? C2 C3 C7 123.0(3) . . ? C4 C3 C7 116.4(3) . . ? C5 C4 C3 120.7(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 119.4(3) . . ? C4 C5 C15 119.1(3) . . ? C6 C5 C15 121.2(3) . . ? C1 C6 C5 120.0(3) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C3 114.1(3) . . ? C8 C7 H7A 108.7 . . ? C3 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C3 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C13 118.8(3) . . ? C9 C8 C7 121.3(3) . . ? C13 C8 C7 119.9(3) . . ? C8 C9 C10 121.4(3) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 119.7(3) . . ? C9 C10 C16 119.6(3) . . ? C11 C10 C16 120.7(3) . . ? C12 C11 C10 118.9(3) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 120.8(3) . . ? C11 C12 C17 118.6(3) . . ? C13 C12 C17 120.6(3) . . ? C8 C13 C12 120.5(3) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? O2 C14 O1 120.9(3) . . ? O2 C14 C1 121.4(3) . . ? O1 C14 C1 117.6(3) . . ? O3 C15 O4 119.5(3) . . ? O3 C15 C5 120.5(3) . . ? O4 C15 C5 120.0(3) . . ? O5 C16 O6 125.7(3) . . ? O5 C16 C10 118.6(3) . . ? O6 C16 C10 115.7(3) . . ? O7 C17 O8 123.9(3) . . ? O7 C17 C12 121.8(3) . . ? O8 C17 C12 114.3(3) . . ? O3 Mn1 O9 92.63(11) 1_654 . ? O3 Mn1 O4 129.54(10) 1_654 2_575 ? O9 Mn1 O4 84.08(10) . 2_575 ? O3 Mn1 O2 91.85(10) 1_654 2_565 ? O9 Mn1 O2 97.73(10) . 2_565 ? O4 Mn1 O2 138.56(10) 2_575 2_565 ? O3 Mn1 O7 87.37(11) 1_654 . ? O9 Mn1 O7 163.59(9) . . ? O4 Mn1 O7 83.30(10) 2_575 . ? O2 Mn1 O7 98.67(9) 2_565 . ? O3 Mn1 O1 146.80(10) 1_654 2_565 ? O9 Mn1 O1 101.77(10) . 2_565 ? O4 Mn1 O1 82.08(9) 2_575 2_565 ? O2 Mn1 O1 56.90(9) 2_565 2_565 ? O7 Mn1 O1 86.82(9) . 2_565 ? C14 O1 Mn1 87.1(2) . 2_565 ? C14 O2 Mn1 95.0(2) . 2_565 ? C15 O3 Mn1 174.5(3) . 1_456 ? C15 O4 Mn1 110.1(2) . 2_575 ? C16 O6 H6A 115.2 . . ? C17 O7 Mn1 132.4(2) . . ? C17 O8 H8 115.6 . . ? Mn1 O9 H9C 95.5 . . ? Mn1 O9 H9B 119.6 . . ? H9C O9 H9B 95.7 . . ? H10C O10 H10D 109.5 . . ? 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 O6 H6A O5 0.91 1.75 2.635(3) 164.0 2_775 O8 H8 O1 0.89 1.76 2.635(3) 167.0 2_565 O9 H9B O1 0.85 2.14 2.887(4) 146.9 1_564 O9 H9C O4 0.85 2.03 2.839(4) 157.9 1_554 O10 H10C O8 0.85 2.35 3.069(2) 142.4 . O10 H10D O8 0.85 2.52 3.069(2) 123.4 2_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.525 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.077 # Attachment '6.cif.txt' data_p1 _database_code_depnum_ccdc_archive 'CCDC 651549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C17 H12 Co O9), H2 O' _chemical_formula_sum 'C34 H26 Co2 O19' _chemical_formula_weight 856.41 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2984(17) _cell_length_b 9.985(2) _cell_length_c 11.724(3) _cell_angle_alpha 76.244(3) _cell_angle_beta 75.3920(10) _cell_angle_gamma 74.173(5) _cell_volume 782.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 815 _cell_measurement_theta_min 2.560 _cell_measurement_theta_max 27.879 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.760 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4187 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2979 _reflns_number_gt 2179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0500P)^2^+1.9900P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2979 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Co1 Co 0.17644(11) 0.12592(8) 0.44822(6) 0.0336(2) Uani 1 1 d . . . C1 C 0.9363(7) 0.7658(5) -0.0766(4) 0.0331(11) Uani 1 1 d . . . C2 C 1.0763(8) 0.8384(6) -0.0884(5) 0.0351(12) Uani 1 1 d . . . H2 H 1.1158 0.8957 -0.1607 0.042 Uiso 1 1 calc R . . C3 C 1.1585(7) 0.8247(5) 0.0103(5) 0.0325(11) Uani 1 1 d . . . C4 C 1.1034(7) 0.7339(5) 0.1169(5) 0.0301(11) Uani 1 1 d . . . H4 H 1.1621 0.7233 0.1813 0.036 Uiso 1 1 calc R . . C5 C 0.9648(8) 0.6601(5) 0.1284(4) 0.0332(12) Uani 1 1 d . . . C6 C 0.8784(7) 0.6786(5) 0.0312(4) 0.0299(11) Uani 1 1 d . . . H6 H 0.7806 0.6322 0.0382 0.036 Uiso 1 1 calc R . . C7 C 0.9108(7) 0.5594(6) 0.2420(4) 0.0324(11) Uani 1 1 d . . . H7A H 0.9699 0.4637 0.2280 0.039 Uiso 1 1 calc R . . H7B H 0.9674 0.5744 0.3031 0.039 Uiso 1 1 calc R . . C8 C 0.6975(8) 0.5699(5) 0.2906(5) 0.0361(12) Uani 1 1 d . . . C9 C 0.6172(7) 0.4542(5) 0.3148(4) 0.0300(11) Uani 1 1 d . . . H9 H 0.6940 0.3695 0.2931 0.036 Uiso 1 1 calc R . . C10 C 0.4233(7) 0.4611(5) 0.3710(4) 0.0300(11) Uani 1 1 d . . . C11 C 0.3078(7) 0.5879(5) 0.4038(4) 0.0287(11) Uani 1 1 d . . . H11 H 0.1790 0.5934 0.4431 0.034 Uiso 1 1 calc R . . C12 C 0.3883(7) 0.7071(6) 0.3767(4) 0.0356(12) Uani 1 1 d . . . C13 C 0.5797(7) 0.6972(5) 0.3189(4) 0.0316(11) Uani 1 1 d . . . H13 H 0.6308 0.7775 0.2984 0.038 Uiso 1 1 calc R . . C14 C 0.8440(7) 0.7827(5) -0.1803(4) 0.0312(11) Uani 1 1 d . . . C15 C 1.3056(7) 0.9042(5) 0.0036(4) 0.0302(11) Uani 1 1 d . . . C16 C 0.3381(8) 0.3360(6) 0.3977(5) 0.0331(12) Uani 1 1 d . . . C17 C 0.2675(7) 0.8426(5) 0.4132(4) 0.0285(10) Uani 1 1 d . . . O1 O 0.9238(5) 0.8248(4) -0.2832(3) 0.0361(8) Uani 1 1 d . . . O2 O 0.6782(5) 0.7460(4) -0.1520(3) 0.0403(9) Uani 1 1 d . . . H2A H 0.6321 0.7622 -0.2121 0.048 Uiso 1 1 calc R . . O3 O 1.3458(5) 0.9895(4) -0.0959(3) 0.0356(8) Uani 1 1 d . . . H3 H 1.4334 1.0249 -0.0933 0.043 Uiso 1 1 calc R . . O4 O 1.3788(5) 0.8903(4) 0.0907(3) 0.0365(9) Uani 1 1 d . . . O5 O 0.4364(5) 0.2268(3) 0.3531(3) 0.0324(8) Uani 1 1 d . . . O6 O 0.1769(5) 0.3328(4) 0.4630(3) 0.0378(9) Uani 1 1 d . . . O7 O 0.0993(5) 0.8507(4) 0.4677(4) 0.0444(10) Uani 1 1 d . . . O8 O 0.3456(5) 0.9475(4) 0.3890(3) 0.0372(9) Uani 1 1 d . . . O9 O 0.2678(5) 0.0374(4) 0.6131(3) 0.0343(8) Uani 1 1 d . . . H9A H 0.2762 -0.0514 0.6303 0.041 Uiso 1 1 d R . . H9B H 0.3773 0.0535 0.6108 0.041 Uiso 1 1 d R . . O10 O 0.5000 0.5000 0.0000 0.0555(16) Uani 1 2 d S . . H10C H 0.4874 0.5885 -0.0064 0.067 Uiso 0.50 1 d PR . . H10B H 0.4877 0.4469 0.0686 0.067 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0317(4) 0.0323(4) 0.0322(4) -0.0063(3) -0.0003(3) -0.0051(3) C1 0.031(3) 0.034(3) 0.032(3) -0.013(2) 0.001(2) -0.005(2) C2 0.039(3) 0.035(3) 0.028(3) -0.007(2) -0.001(2) -0.008(2) C3 0.028(3) 0.030(3) 0.036(3) -0.003(2) 0.000(2) -0.008(2) C4 0.026(2) 0.027(3) 0.035(3) -0.003(2) -0.007(2) -0.003(2) C5 0.037(3) 0.030(3) 0.029(3) -0.008(2) -0.001(2) -0.005(2) C6 0.027(2) 0.035(3) 0.027(2) -0.008(2) -0.0007(19) -0.010(2) C7 0.030(3) 0.033(3) 0.029(3) 0.000(2) -0.004(2) -0.006(2) C8 0.040(3) 0.030(3) 0.034(3) -0.002(2) -0.003(2) -0.010(2) C9 0.032(3) 0.024(2) 0.032(3) -0.007(2) -0.007(2) -0.002(2) C10 0.030(3) 0.032(3) 0.027(2) -0.004(2) -0.004(2) -0.009(2) C11 0.027(2) 0.027(3) 0.027(2) -0.006(2) 0.0007(19) -0.003(2) C12 0.030(3) 0.038(3) 0.031(3) -0.001(2) -0.002(2) -0.004(2) C13 0.031(3) 0.034(3) 0.028(3) -0.001(2) -0.002(2) -0.010(2) C14 0.036(3) 0.029(3) 0.028(3) -0.007(2) -0.006(2) -0.004(2) C15 0.037(3) 0.030(3) 0.026(2) -0.002(2) -0.003(2) -0.017(2) C16 0.037(3) 0.031(3) 0.033(3) 0.001(2) -0.017(2) -0.008(2) C17 0.032(3) 0.025(2) 0.024(2) -0.0053(19) -0.007(2) 0.002(2) O1 0.042(2) 0.033(2) 0.033(2) -0.0039(16) -0.0074(16) -0.0102(17) O2 0.038(2) 0.058(3) 0.0297(19) -0.0100(18) -0.0069(16) -0.0176(19) O3 0.035(2) 0.040(2) 0.0357(19) 0.0009(16) -0.0049(15) -0.0230(17) O4 0.041(2) 0.039(2) 0.0338(19) 0.0087(16) -0.0189(16) -0.0191(17) O5 0.0334(19) 0.0268(18) 0.040(2) -0.0068(15) -0.0119(16) -0.0065(15) O6 0.036(2) 0.033(2) 0.044(2) -0.0086(16) 0.0012(17) -0.0147(17) O7 0.0263(19) 0.035(2) 0.060(3) -0.0159(18) 0.0148(17) -0.0031(16) O8 0.037(2) 0.033(2) 0.039(2) -0.0128(16) -0.0010(16) -0.0046(16) O9 0.042(2) 0.0296(19) 0.0317(19) -0.0049(15) -0.0105(16) -0.0068(16) O10 0.046(3) 0.053(4) 0.051(4) -0.003(3) 0.012(3) -0.011(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 Co1 O7 1.982(3) 2_566 ? Co1 O8 2.033(4) 1_545 ? Co1 O6 2.114(4) . ? Co1 O9 2.117(3) . ? Co1 O1 2.141(4) 2_665 ? Co1 O5 2.302(4) . ? C1 C2 1.369(7) . ? C1 C6 1.393(7) . ? C1 C14 1.489(7) . ? C2 C3 1.395(7) . ? C2 H2 0.9300 . ? C3 C4 1.397(7) . ? C3 C15 1.477(7) . ? C4 C5 1.369(7) . ? C4 H4 0.9300 . ? C5 C6 1.389(7) . ? C5 C7 1.501(7) . ? C6 H6 0.9300 . ? C7 C8 1.500(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.375(7) . ? C8 C13 1.388(7) . ? C9 C10 1.393(7) . ? C9 H9 0.9300 . ? C10 C11 1.395(7) . ? C10 C16 1.478(7) . ? C11 C12 1.403(7) . ? C11 H11 0.9300 . ? C12 C13 1.378(7) . ? C12 C17 1.493(7) . ? C13 H13 0.9300 . ? C14 O1 1.228(6) . ? C14 O2 1.300(6) . ? C15 O4 1.231(6) . ? C15 O3 1.290(6) . ? C16 O6 1.236(6) . ? C16 O5 1.277(6) . ? C17 O7 1.223(6) . ? C17 O8 1.267(6) . ? O1 Co1 2.141(4) 2_665 ? O2 H2A 0.8200 . ? O3 H3 0.8200 . ? O7 Co1 1.982(3) 2_566 ? O8 Co1 2.033(4) 1_565 ? O9 H9A 0.8500 . ? O9 H9B 0.8500 . ? O10 H10C 0.8500 . ? O10 H10B 0.8500 . ? 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 O7 Co1 O8 125.23(16) 2_566 1_545 ? O7 Co1 O6 91.09(15) 2_566 . ? O8 Co1 O6 143.65(15) 1_545 . ? O7 Co1 O9 90.41(16) 2_566 . ? O8 Co1 O9 86.74(14) 1_545 . ? O6 Co1 O9 92.17(14) . . ? O7 Co1 O1 87.68(16) 2_566 2_665 ? O8 Co1 O1 85.39(14) 1_545 2_665 ? O6 Co1 O1 98.86(14) . 2_665 ? O9 Co1 O1 168.84(13) . 2_665 ? O7 Co1 O5 148.79(14) 2_566 . ? O8 Co1 O5 85.51(14) 1_545 . ? O6 Co1 O5 58.57(13) . . ? O9 Co1 O5 97.33(13) . . ? O1 Co1 O5 89.94(13) 2_665 . ? C2 C1 C6 120.8(5) . . ? C2 C1 C14 119.0(5) . . ? C6 C1 C14 120.2(5) . . ? C1 C2 C3 118.6(5) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C2 C3 C4 120.1(5) . . ? C2 C3 C15 120.8(4) . . ? C4 C3 C15 119.1(5) . . ? C5 C4 C3 121.3(5) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 118.2(5) . . ? C4 C5 C7 121.0(5) . . ? C6 C5 C7 120.9(5) . . ? C5 C6 C1 120.9(5) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C5 116.4(4) . . ? C8 C7 H7A 108.2 . . ? C5 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? C5 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? C9 C8 C13 118.8(5) . . ? C9 C8 C7 121.6(5) . . ? C13 C8 C7 119.5(5) . . ? C8 C9 C10 121.4(5) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 119.5(5) . . ? C9 C10 C16 121.1(5) . . ? C11 C10 C16 119.4(4) . . ? C10 C11 C12 119.3(4) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 119.8(5) . . ? C13 C12 C17 120.5(5) . . ? C11 C12 C17 119.8(4) . . ? C12 C13 C8 121.3(5) . . ? C12 C13 H13 119.4 . . ? C8 C13 H13 119.4 . . ? O1 C14 O2 124.4(5) . . ? O1 C14 C1 121.4(5) . . ? O2 C14 C1 114.2(4) . . ? O4 C15 O3 123.4(5) . . ? O4 C15 C3 120.4(4) . . ? O3 C15 C3 116.1(4) . . ? O6 C16 O5 119.0(5) . . ? O6 C16 C10 122.3(5) . . ? O5 C16 C10 118.7(5) . . ? O7 C17 O8 121.1(4) . . ? O7 C17 C12 120.7(5) . . ? O8 C17 C12 118.2(4) . . ? C14 O1 Co1 130.6(3) . 2_665 ? C14 O2 H2A 109.5 . . ? C15 O3 H3 109.5 . . ? C16 O5 Co1 86.3(3) . . ? C16 O6 Co1 96.1(3) . . ? C17 O7 Co1 177.0(4) . 2_566 ? C17 O8 Co1 116.0(3) . 1_565 ? Co1 O9 H9A 111.2 . . ? Co1 O9 H9B 110.8 . . ? H9A O9 H9B 109.1 . . ? H10C O10 H10B 120.5 . . ? 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 O2 H2A O5 0.82 1.82 2.627(5) 170.1 2_665 O3 H3 O4 0.82 1.81 2.626(5) 177.6 2_875 O9 H9A O5 0.85 2.35 2.934(5) 125.7 2_656 O9 H9B O8 0.85 2.02 2.860(5) 169.4 2_666 O10 H10C O2 0.85 2.46 3.065(4) 128.9 . O10 H10B O2 0.85 2.43 3.065(4) 131.9 2_665 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.506 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.098