Supplementary information (ESI) for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Qing-Jin Meng' _publ_contact_author_address ; State Key Laboratory of Coordination Chemistry Coordination Chemistry Institute Nanjing 210093 CHINA ; _publ_contact_author_email MENGQJ@NJU.EDU.CN _publ_section_title ; Three coordination polymers with helical chains based on methylenediisophthalic acid (H4MDIP) ; loop_ _publ_author_name 'Qingjin Meng' 'Xianying Duan' 'Yizhi Li' 'Jian-Guo Lin' 'Chengjian Zhu' # Attachment '1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 656229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C25 H22 Mn2 N4 O10), H4 O2' _chemical_formula_sum 'C50 H48 Mn4 N8 O22' _chemical_formula_weight 1332.72 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' 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' N N 0.0061 0.0033 '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' _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 24.995(6) _cell_length_b 8.6663(19) _cell_length_c 17.347(4) _cell_angle_alpha 90.00 _cell_angle_beta 133.949(17) _cell_angle_gamma 90.00 _cell_volume 2705.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.264 _cell_measurement_theta_max 28.141 _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 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.79 _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 '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 7075 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2647 _reflns_number_gt 1867 _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^)+(0.0580P)^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 2647 _refine_ls_number_parameters 195 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.8421(2) 0.2961(5) 0.7136(4) 0.0360(10) Uani 1 1 d . . . C2 C 0.8154(2) 0.1781(5) 0.6415(4) 0.0371(10) Uani 1 1 d . . . H2 H 0.7763 0.1170 0.6197 0.045 Uiso 1 1 calc R . . C3 C 0.8470(2) 0.1502(5) 0.6011(3) 0.0297(9) Uani 1 1 d . . . C4 C 0.9071(2) 0.2396(4) 0.6385(3) 0.0272(9) Uani 1 1 d . . . H4 H 0.9293 0.2197 0.6134 0.033 Uiso 1 1 calc R . . C5 C 0.9349(2) 0.3563(5) 0.7113(4) 0.0407(11) Uani 1 1 d . . . C6 C 0.9010(2) 0.3841(5) 0.7480(4) 0.0368(11) Uani 1 1 d . . . H6 H 0.9185 0.4635 0.7967 0.044 Uiso 1 1 calc R . . C7 C 1.0000 0.4493(7) 0.7500 0.0372(15) Uani 1 2 d S . . H7A H 1.0157 0.5154 0.8078 0.045 Uiso 1 1 d R . . C8 C 0.8074(2) 0.3276(5) 0.7563(4) 0.0349(10) Uani 1 1 d . . . C9 C 0.8166(2) 0.0322(5) 0.5180(3) 0.0284(9) Uani 1 1 d . . . C10 C 0.9016(2) 0.7837(5) 0.7342(3) 0.0337(10) Uani 1 1 d . . . H10 H 0.9018 0.7250 0.6896 0.040 Uiso 1 1 calc R . . C11 C 0.9560(3) 0.8761(5) 0.8101(4) 0.0383(11) Uani 1 1 d . . . H11 H 0.9999 0.8953 0.8273 0.046 Uiso 1 1 calc R . . C12 C 0.8672(2) 0.8829(5) 0.8059(3) 0.0306(10) Uani 1 1 d . . . H12 H 0.8396 0.9101 0.8214 0.037 Uiso 1 1 calc R . . C13 C 0.9773(2) 1.0443(4) 0.94948(18) 0.0403(11) Uani 1 1 d D . . H13A H 0.9431 1.1110 0.9429 0.048 Uiso 1 1 calc R . . H13B H 1.0093 1.1086 0.9500 0.048 Uiso 1 1 calc R . . Mn1 Mn 0.74147(3) 0.65908(8) 0.63858(5) 0.0266(2) Uani 1 1 d . . . N1 N 0.8445(2) 0.7858(4) 0.7297(3) 0.0362(9) Uani 1 1 d . . . N2 N 0.93548(18) 0.9380(4) 0.8584(3) 0.0350(9) Uani 1 1 d . . . O1 O 0.79267(16) 0.4664(3) 0.7569(2) 0.0325(7) Uani 1 1 d . . . O2 O 0.79685(17) 0.2192(4) 0.7902(3) 0.0356(8) Uani 1 1 d . . . O3 O 0.76024(14) -0.0464(3) 0.4791(2) 0.0277(6) Uani 1 1 d . . . O4 O 0.84513(16) 0.0145(4) 0.4805(2) 0.0372(8) Uani 1 1 d . . . O5 O 0.67810(16) 0.8513(4) 0.5205(3) 0.0413(8) Uani 1 1 d . . . H5A H 0.6993 0.8776 0.5000 0.050 Uiso 1 1 d R . . H5C H 0.6772 0.9278 0.5502 0.050 Uiso 1 1 d R . . O6 O 0.9087(4) 0.5490(7) 0.9649(5) 0.0491(18) Uani 0.50 1 d P . . H6B H 0.9505 0.5060 1.0146 0.074 Uiso 0.50 1 d PR . . H6C H 0.9154 0.6349 0.9491 0.074 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 0.034(2) 0.030(2) 0.028(2) 0.0015(18) 0.016(2) 0.0028(19) C2 0.038(2) 0.030(2) 0.030(2) 0.0018(19) 0.019(2) -0.004(2) C3 0.035(2) 0.027(2) 0.032(2) 0.0092(18) 0.0248(19) 0.0114(19) C4 0.032(2) 0.025(2) 0.030(2) -0.0016(17) 0.024(2) -0.0009(17) C5 0.033(2) 0.032(2) 0.038(3) 0.005(2) 0.017(2) 0.002(2) C6 0.032(2) 0.029(2) 0.031(2) 0.0033(19) 0.015(2) 0.0030(19) C7 0.045(4) 0.022(3) 0.052(4) 0.000 0.036(4) 0.000 C8 0.030(2) 0.026(2) 0.034(2) -0.0038(19) 0.017(2) -0.0014(19) C9 0.038(2) 0.025(2) 0.035(2) 0.0059(17) 0.030(2) 0.0107(18) C10 0.035(2) 0.035(2) 0.023(2) 0.0002(18) 0.017(2) 0.004(2) C11 0.034(2) 0.038(3) 0.039(3) -0.003(2) 0.024(2) -0.007(2) C12 0.032(2) 0.025(2) 0.035(2) -0.0055(18) 0.024(2) -0.0023(18) C13 0.027(2) 0.035(3) 0.030(2) -0.0122(19) 0.0095(19) -0.0136(19) Mn1 0.0292(3) 0.0332(4) 0.0308(4) -0.0159(3) 0.0259(3) -0.0143(3) N1 0.035(2) 0.0236(18) 0.032(2) -0.0040(16) 0.0164(18) -0.0063(16) N2 0.0210(17) 0.034(2) 0.031(2) -0.0019(17) 0.0112(16) -0.0069(16) O1 0.0451(17) 0.0323(17) 0.0409(17) -0.0049(13) 0.0376(16) 0.0019(13) O2 0.052(2) 0.0372(17) 0.049(2) -0.0041(14) 0.0468(19) -0.0044(14) O3 0.0302(15) 0.0279(15) 0.0300(16) -0.0101(12) 0.0227(14) -0.0110(12) O4 0.0387(17) 0.056(2) 0.0319(17) -0.0200(15) 0.0300(15) -0.0156(15) O5 0.0366(16) 0.0451(18) 0.047(2) 0.0030(16) 0.0310(16) 0.0019(16) O6 0.044(4) 0.032(4) 0.037(4) -0.015(3) 0.016(3) -0.006(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 C1 C6 1.374(6) . ? C1 C2 1.378(6) . ? C1 C8 1.507(6) . ? C2 C3 1.394(6) . ? C2 H2 0.9300 . ? C3 C4 1.386(6) . ? C3 C9 1.478(6) . ? C4 C5 1.372(6) . ? C4 H4 0.9300 . ? C5 C6 1.389(7) . ? C5 C7 1.494(5) . ? C6 H6 0.9300 . ? C7 C5 1.494(5) 2_756 ? C7 H7A 0.9700 . ? C8 O2 1.229(5) . ? C8 O1 1.260(5) . ? C9 O3 1.259(5) . ? C9 O4 1.264(5) . ? C9 Mn1 2.599(4) 7_656 ? C10 C11 1.319(6) . ? C10 N1 1.374(6) . ? C10 H10 0.9300 . ? C11 N2 1.360(6) . ? C11 H11 0.9300 . ? C12 N1 1.317(6) . ? C12 N2 1.345(5) . ? C12 H12 0.9300 . ? C13 N2 1.465(5) . ? C13 C13 1.4795(11) 5_777 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? Mn1 O2 2.088(3) 4_656 ? Mn1 N1 2.165(4) . ? Mn1 O5 2.230(3) . ? Mn1 O1 2.234(3) . ? Mn1 O3 2.237(3) 7_656 ? Mn1 O4 2.238(3) 7_656 ? Mn1 C9 2.599(4) 7_656 ? O2 Mn1 2.088(3) 4_646 ? O3 Mn1 2.237(3) 7_656 ? O4 Mn1 2.238(3) 7_656 ? O5 H5A 0.8499 . ? O5 H5C 0.8499 . ? O6 H6B 0.8500 . ? O6 H6C 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 C6 C1 C2 120.3(5) . . ? C6 C1 C8 119.7(4) . . ? C2 C1 C8 120.0(4) . . ? C1 C2 C3 119.9(4) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 118.4(4) . . ? C4 C3 C9 120.1(4) . . ? C2 C3 C9 121.5(4) . . ? C5 C4 C3 122.4(4) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C4 C5 C6 118.0(4) . . ? C4 C5 C7 120.6(4) . . ? C6 C5 C7 121.4(4) . . ? C1 C6 C5 121.0(4) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C5 C7 C5 114.7(5) . 2_756 ? C5 C7 H7A 108.4 . . ? C5 C7 H7A 108.8 2_756 . ? O2 C8 O1 124.5(4) . . ? O2 C8 C1 118.9(4) . . ? O1 C8 C1 116.5(4) . . ? O3 C9 O4 118.7(4) . . ? O3 C9 C3 121.6(3) . . ? O4 C9 C3 119.6(4) . . ? O3 C9 Mn1 59.3(2) . 7_656 ? O4 C9 Mn1 59.4(2) . 7_656 ? C3 C9 Mn1 175.8(3) . 7_656 ? C11 C10 N1 111.0(4) . . ? C11 C10 H10 124.5 . . ? N1 C10 H10 124.5 . . ? C10 C11 N2 106.6(4) . . ? C10 C11 H11 126.7 . . ? N2 C11 H11 126.7 . . ? N1 C12 N2 111.6(4) . . ? N1 C12 H12 124.2 . . ? N2 C12 H12 124.2 . . ? N2 C13 C13 109.7(4) . 5_777 ? N2 C13 H13A 109.7 . . ? C13 C13 H13A 109.7 5_777 . ? N2 C13 H13B 109.7 . . ? C13 C13 H13B 109.7 5_777 . ? H13A C13 H13B 108.2 . . ? O2 Mn1 N1 104.07(14) 4_656 . ? O2 Mn1 O5 91.83(12) 4_656 . ? N1 Mn1 O5 91.07(13) . . ? O2 Mn1 O1 81.26(11) 4_656 . ? N1 Mn1 O1 94.33(13) . . ? O5 Mn1 O1 172.09(11) . . ? O2 Mn1 O3 157.41(11) 4_656 7_656 ? N1 Mn1 O3 98.48(13) . 7_656 ? O5 Mn1 O3 86.35(12) . 7_656 ? O1 Mn1 O3 98.54(10) . 7_656 ? O2 Mn1 O4 99.59(12) 4_656 7_656 ? N1 Mn1 O4 155.98(13) . 7_656 ? O5 Mn1 O4 92.24(13) . 7_656 ? O1 Mn1 O4 85.18(12) . 7_656 ? O3 Mn1 O4 58.04(10) 7_656 7_656 ? O2 Mn1 C9 128.65(13) 4_656 7_656 ? N1 Mn1 C9 127.23(14) . 7_656 ? O5 Mn1 C9 89.49(13) . 7_656 ? O1 Mn1 C9 91.83(12) . 7_656 ? O3 Mn1 C9 28.95(11) 7_656 7_656 ? O4 Mn1 C9 29.09(11) 7_656 7_656 ? C12 N1 C10 104.1(4) . . ? C12 N1 Mn1 121.5(3) . . ? C10 N1 Mn1 134.2(3) . . ? C12 N2 C11 106.6(4) . . ? C12 N2 C13 125.0(4) . . ? C11 N2 C13 128.4(4) . . ? C8 O1 Mn1 133.7(3) . . ? C8 O2 Mn1 144.2(3) . 4_646 ? C9 O3 Mn1 91.7(2) . 7_656 ? C9 O4 Mn1 91.5(2) . 7_656 ? Mn1 O5 H5A 109.5 . . ? Mn1 O5 H5C 109.1 . . ? H5A O5 H5C 109.5 . . ? H6B O6 H6C 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 O5 H5A O3 0.85 1.91 2.750(4) 169.5 1_565 O5 H5C O6 0.85 2.23 2.910(8) 136.4 4_656 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.405 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.084 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 656230' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '.20 Mn3 O20.60, C10 H8 N2, 0.6(H2O), 0.6(H2O), 0.4(H2O), 0.4(H2O), 0.4(H2O)' _chemical_formula_sum 'C44 H39 Mn3 N2 O23' _chemical_formula_weight 1128.59 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.4159(15) _cell_length_b 15.596(2) _cell_length_c 28.849(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.997(2) _cell_angle_gamma 90.00 _cell_volume 5073.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6061 _cell_measurement_theta_min 2.229 _cell_measurement_theta_max 27.961 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area dtector' _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 26555 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0834 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9940 _reflns_number_gt 6654 _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^)+(0.0600P)^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 9940 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.3688(3) -0.1494(3) 0.75950(13) 0.0303(9) Uani 1 1 d . . . C2 C 0.4458(4) -0.2148(3) 0.76791(16) 0.0410(10) Uani 1 1 d . . . H2A H 0.4955 -0.2243 0.7458 0.049 Uiso 1 1 calc R . . C3 C 0.4586(4) -0.2688(3) 0.80564(14) 0.0368(10) Uani 1 1 d . . . C4 C 0.3852(3) -0.2571(3) 0.83786(16) 0.0351(9) Uani 1 1 d . . . H4A H 0.3892 -0.2949 0.8630 0.042 Uiso 1 1 calc R . . C5 C 0.3042(4) -0.1899(3) 0.83420(15) 0.0384(10) Uani 1 1 d . . . C6 C 0.2943(3) -0.1333(2) 0.79406(16) 0.0352(10) Uani 1 1 d . . . H6A H 0.2410 -0.0878 0.7908 0.042 Uiso 1 1 calc R . . C7 C 0.2296(4) -0.1643(3) 0.87184(15) 0.0381(10) Uani 1 1 d . . . H7A H 0.1710 -0.1224 0.8586 0.046 Uiso 1 1 calc R . . H7B H 0.2809 -0.1369 0.8976 0.046 Uiso 1 1 calc R . . C8 C 0.1647(3) -0.2408(3) 0.89155(16) 0.0371(10) Uani 1 1 d . . . C9 C 0.2100(4) -0.2827(3) 0.93171(16) 0.0403(10) Uani 1 1 d . . . H9A H 0.2858 -0.2697 0.9469 0.048 Uiso 1 1 calc R . . C10 C 0.1415(4) -0.3466(3) 0.95065(15) 0.0400(10) Uani 1 1 d . . . C11 C 0.0327(4) -0.3705(3) 0.92482(16) 0.0407(11) Uani 1 1 d . . . H11A H -0.0147 -0.4108 0.9368 0.049 Uiso 1 1 calc R . . C12 C -0.0039(4) -0.3341(3) 0.88167(16) 0.0424(11) Uani 1 1 d . . . C13 C 0.0609(4) -0.2699(3) 0.86382(16) 0.0404(10) Uani 1 1 d . . . H13A H 0.0358 -0.2469 0.8342 0.048 Uiso 1 1 calc R . . C14 C 0.3572(3) -0.0909(3) 0.72039(15) 0.0318(9) Uani 1 1 d . . . C15 C 0.5431(4) -0.3430(3) 0.80893(16) 0.0405(11) Uani 1 1 d . . . C16 C 0.1890(5) -0.3872(3) 0.99743(17) 0.0478(13) Uani 1 1 d . . . C17 C -0.1153(4) -0.3679(3) 0.85248(18) 0.0467(12) Uani 1 1 d . . . C18 C 0.1406(4) 0.3256(3) 0.74331(14) 0.0375(10) Uani 1 1 d . . . C19 C 0.0464(4) 0.3904(3) 0.73652(16) 0.0429(11) Uani 1 1 d . . . H19B H -0.0095 0.3932 0.7567 0.051 Uiso 1 1 calc R . . C20 C 0.0421(4) 0.4469(3) 0.69973(15) 0.0373(10) Uani 1 1 d . . . C21 C 0.1201(4) 0.4328(2) 0.66687(15) 0.0343(9) Uani 1 1 d . . . H21A H 0.1167 0.4703 0.6416 0.041 Uiso 1 1 calc R . . C22 C 0.2022(4) 0.3656(2) 0.67027(15) 0.0347(9) Uani 1 1 d . . . C23 C 0.2164(4) 0.3144(3) 0.71194(15) 0.0414(11) Uani 1 1 d . . . H23A H 0.2768 0.2740 0.7175 0.050 Uiso 1 1 calc R . . C24 C 0.2728(4) 0.3445(3) 0.63176(15) 0.0405(10) Uani 1 1 d . . . H24A H 0.2751 0.2889 0.6203 0.049 Uiso 1 1 calc R . . C25 C 0.3382(4) 0.4146(3) 0.61281(16) 0.0397(11) Uani 1 1 d . . . C26 C 0.3043(4) 0.4402(3) 0.56538(16) 0.0459(12) Uani 1 1 d . . . H26E H 0.2375 0.4163 0.5475 0.055 Uiso 1 1 calc R . . C27 C 0.3722(4) 0.5018(3) 0.54537(15) 0.0382(10) Uani 1 1 d . . . C28 C 0.4659(4) 0.5381(3) 0.57208(16) 0.0395(10) Uani 1 1 d . . . H28A H 0.5060 0.5814 0.5589 0.047 Uiso 1 1 calc R . . C29 C 0.5063(4) 0.5150(3) 0.61777(16) 0.0405(10) Uani 1 1 d . . . C30 C 0.4393(4) 0.4513(3) 0.63786(15) 0.0382(10) Uani 1 1 d . . . H30A H 0.4643 0.4340 0.6687 0.046 Uiso 1 1 calc R . . C31 C 0.1461(4) 0.2685(3) 0.78648(16) 0.0403(10) Uani 1 1 d . . . C32 C -0.0393(4) 0.5188(3) 0.69359(16) 0.0368(10) Uani 1 1 d . . . C33 C 0.6183(4) 0.5503(3) 0.64634(15) 0.0391(10) Uani 1 1 d . . . C35 C 0.8294(4) 0.3296(3) 0.27710(15) 0.0376(10) Uani 1 1 d . . . H35A H 0.8820 0.2868 0.2893 0.045 Uiso 1 1 calc R . . C36 C 0.8481(4) 0.3692(2) 0.23767(15) 0.0336(10) Uani 1 1 d . . . H36A H 0.9128 0.3544 0.2233 0.040 Uiso 1 1 calc R . . C37 C 0.7707(4) 0.4321(2) 0.21865(16) 0.0407(11) Uani 1 1 d . . . C38 C 0.6735(4) 0.4539(3) 0.24388(15) 0.0389(10) Uani 1 1 d . . . H38A H 0.6197 0.4967 0.2328 0.047 Uiso 1 1 calc R . . C39 C 0.6633(4) 0.4116(3) 0.28273(16) 0.0393(10) Uani 1 1 d . . . H39A H 0.6015 0.4263 0.2987 0.047 Uiso 1 1 calc R . . C40 C 0.7859(3) 0.4782(3) 0.17529(15) 0.0335(9) Uani 1 1 d . . . C41 C 0.9059(4) 0.4996(2) 0.16868(14) 0.0324(9) Uani 1 1 d . . . H41A H 0.9719 0.4818 0.1895 0.039 Uiso 1 1 calc R . . C42 C 0.9158(4) 0.5481(3) 0.12931(16) 0.0396(10) Uani 1 1 d . . . H42A H 0.9904 0.5685 0.1258 0.048 Uiso 1 1 calc R . . C43 C 0.7135(4) 0.5468(3) 0.10397(15) 0.0426(11) Uani 1 1 d . . . H43A H 0.6492 0.5642 0.0821 0.051 Uiso 1 1 calc R . . C44 C 0.6917(4) 0.5009(3) 0.14311(16) 0.0458(11) Uani 1 1 d . . . H44A H 0.6149 0.4863 0.1470 0.055 Uiso 1 1 calc R . . C45 C 0.3461(4) 0.5188(3) 0.49308(16) 0.0467(12) Uani 1 1 d . . . Mn1 Mn 0.32712(5) 0.00578(3) 0.643260(19) 0.02418(14) Uani 1 1 d . . . Mn2 Mn 0.25066(6) 0.09096(4) 0.75064(2) 0.03601(17) Uani 1 1 d . . . Mn3 Mn 0.16498(5) 0.16671(4) 0.86070(2) 0.03528(17) Uani 1 1 d . . . N1 N 0.7373(3) 0.3488(2) 0.30032(13) 0.0429(10) Uani 1 1 d . . . N2 N 0.8246(3) 0.5675(2) 0.09613(14) 0.0428(9) Uani 1 1 d . . . O1 O 0.4246(2) -0.10045(16) 0.68874(10) 0.0304(6) Uani 1 1 d . . . O2 O 0.2838(3) -0.02905(18) 0.71575(10) 0.0392(7) Uani 1 1 d . . . O3 O 0.6050(3) -0.35167(19) 0.77685(10) 0.0403(7) Uani 1 1 d . . . O4 O 0.5423(3) -0.39622(18) 0.84172(11) 0.0413(7) Uani 1 1 d . . . O5 O 0.2988(3) -0.39338(19) 1.00885(11) 0.0462(8) Uani 1 1 d . . . O6 O 0.1145(3) -0.41235(19) 1.02152(10) 0.0409(7) Uani 1 1 d . . . H6D H 0.0666 -0.3649 1.0285 0.049 Uiso 1 1 d R . . O7 O -0.1932(2) -0.40270(17) 0.87498(10) 0.0365(7) Uani 1 1 d . . . O8 O -0.1236(3) -0.36597(17) 0.80947(11) 0.0387(7) Uani 1 1 d . . . O9 O 0.2193(3) 0.20887(18) 0.78945(11) 0.0453(8) Uani 1 1 d . . . O10 O 0.0830(2) 0.28031(17) 0.81658(10) 0.0335(6) Uani 1 1 d . . . O11 O -0.1047(3) 0.52793(18) 0.72553(10) 0.0398(7) Uani 1 1 d . . . O12 O -0.0464(2) 0.56587(18) 0.65887(11) 0.0374(7) Uani 1 1 d . . . O13 O 0.2804(3) 0.46789(19) 0.46971(10) 0.0449(8) Uani 1 1 d . . . H13D H 0.3148 0.4116 0.4730 0.054 Uiso 1 1 d R . . O14 O 0.3823(3) 0.58965(17) 0.47921(10) 0.0405(8) Uani 1 1 d . . . O15 O 0.6945(3) 0.57116(18) 0.62328(11) 0.0413(7) Uani 1 1 d . . . O16 O 0.6206(3) 0.55518(18) 0.68883(11) 0.0414(7) Uani 1 1 d . . . O17 O 0.1983(3) -0.09099(18) 0.61241(10) 0.0375(7) Uani 1 1 d . . . H17A H 0.1457 -0.0674 0.5923 0.045 Uiso 1 1 d R . . H17B H 0.2334 -0.1298 0.5991 0.045 Uiso 1 1 d R . . O18 O 0.4033(2) -0.01112(19) 0.57985(10) 0.0420(7) Uani 1 1 d . . . H18A H 0.3737 0.0254 0.5595 0.050 Uiso 1 1 d R . . H18C H 0.3884 -0.0614 0.5692 0.050 Uiso 1 1 d R . . O19 O 0.2981(2) 0.25175(17) 0.90291(10) 0.0375(7) Uani 1 1 d . . . H19A H 0.2927 0.2462 0.9318 0.045 Uiso 1 1 d R . . H19C H 0.2851 0.3037 0.8947 0.045 Uiso 1 1 d R . . O20 O 0.0590(2) 0.19248(17) 0.91537(9) 0.0346(6) Uani 1 1 d . . . H20A H 0.0720 0.1537 0.9362 0.042 Uiso 1 1 d R . . H20C H -0.0142 0.1926 0.9038 0.042 Uiso 1 1 d R . . O21 O 0.0037(8) 0.8963(5) 0.9893(3) 0.061(3) Uani 0.40 1 d P . . H21D H 0.0205 0.8478 0.9786 0.074 Uiso 0.40 1 d PR . . H21B H 0.0579 0.9321 0.9860 0.074 Uiso 0.40 1 d PR . . O22 O 0.4953(6) 0.6160(4) 0.9662(2) 0.0654(17) Uani 0.60 1 d P . . H22A H 0.4869 0.5685 0.9798 0.078 Uiso 0.60 1 d PR . . H22B H 0.4376 0.6490 0.9690 0.078 Uiso 0.60 1 d PR . . O23 O 0.4637(4) 0.2609(3) 0.84862(17) 0.0424(13) Uani 0.60 1 d P . . H23B H 0.4174 0.2261 0.8595 0.051 Uiso 0.60 1 d PR . . H23C H 0.4374 0.2712 0.8199 0.051 Uiso 0.60 1 d PR . . O24 O 0.5757(6) 0.7153(4) 0.5032(3) 0.0413(18) Uani 0.40 1 d P . . H24C H 0.5163 0.6845 0.4922 0.050 Uiso 0.40 1 d PR . . H24B H 0.6240 0.7169 0.4836 0.050 Uiso 0.40 1 d PR . . O25 O 0.7757(6) 0.2653(4) 0.3853(2) 0.0390(17) Uani 0.40 1 d P . . H25D H 0.7553 0.3115 0.3975 0.047 Uiso 0.40 1 d PR . . H25A H 0.7913 0.2755 0.3580 0.047 Uiso 0.40 1 d PR . . O26 O 0.9042(5) 0.6564(3) 0.02864(19) 0.0476(13) Uani 0.60 1 d P . . H26A H 0.9795 0.6578 0.0339 0.057 Uiso 0.60 1 d PR . . H26C H 0.8771 0.7072 0.0287 0.057 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 C1 0.029(2) 0.045(2) 0.0179(18) 0.0202(17) 0.0056(15) 0.0026(17) C2 0.047(3) 0.037(2) 0.041(3) 0.008(2) 0.014(2) -0.006(2) C3 0.058(3) 0.024(2) 0.030(2) 0.0052(17) 0.009(2) 0.0040(19) C4 0.031(2) 0.034(2) 0.040(2) 0.0043(19) 0.0033(18) 0.0004(17) C5 0.032(2) 0.048(3) 0.031(2) -0.008(2) -0.0085(18) -0.0081(19) C6 0.0208(19) 0.025(2) 0.055(3) 0.0027(19) -0.0098(19) 0.0049(15) C7 0.030(2) 0.049(3) 0.030(2) -0.004(2) -0.0120(17) 0.0046(18) C8 0.028(2) 0.036(2) 0.046(3) 0.008(2) 0.0031(19) -0.0009(17) C9 0.044(2) 0.033(2) 0.041(3) -0.011(2) -0.002(2) 0.0155(19) C10 0.044(2) 0.044(2) 0.030(2) -0.014(2) -0.0016(19) 0.007(2) C11 0.039(2) 0.034(2) 0.042(3) -0.008(2) -0.017(2) 0.0039(18) C12 0.052(3) 0.034(2) 0.042(3) -0.004(2) 0.010(2) 0.003(2) C13 0.042(2) 0.044(2) 0.034(2) -0.016(2) 0.0032(19) 0.011(2) C14 0.0222(19) 0.037(2) 0.036(2) 0.0064(18) 0.0051(17) 0.0106(16) C15 0.032(2) 0.041(2) 0.041(3) 0.004(2) -0.015(2) -0.0042(18) C16 0.069(3) 0.029(2) 0.038(3) 0.016(2) -0.013(2) 0.006(2) C17 0.049(3) 0.038(2) 0.050(3) -0.019(2) -0.004(2) 0.014(2) C18 0.043(2) 0.043(2) 0.022(2) -0.0021(18) -0.0068(18) -0.0073(19) C19 0.034(2) 0.050(3) 0.040(3) -0.013(2) -0.010(2) -0.0009(19) C20 0.039(2) 0.035(2) 0.033(2) 0.0031(19) -0.0093(19) 0.0133(18) C21 0.044(2) 0.0224(19) 0.037(2) -0.0028(17) 0.0104(19) -0.0111(17) C22 0.043(2) 0.029(2) 0.034(2) 0.0137(18) 0.0112(19) -0.0006(18) C23 0.053(3) 0.031(2) 0.037(2) -0.0059(19) -0.002(2) -0.0065(19) C24 0.046(3) 0.040(2) 0.037(2) 0.013(2) 0.011(2) 0.018(2) C25 0.036(2) 0.037(2) 0.051(3) -0.007(2) 0.019(2) -0.0207(18) C26 0.029(2) 0.059(3) 0.044(3) -0.026(2) -0.013(2) 0.013(2) C27 0.045(2) 0.036(2) 0.034(2) -0.0092(19) 0.0075(19) -0.017(2) C28 0.035(2) 0.042(2) 0.040(2) 0.015(2) 0.0004(19) 0.0017(18) C29 0.050(3) 0.029(2) 0.041(3) 0.0005(19) 0.002(2) 0.0004(19) C30 0.035(2) 0.048(3) 0.035(2) -0.005(2) 0.0152(19) -0.0035(19) C31 0.048(3) 0.033(2) 0.039(2) -0.004(2) 0.002(2) 0.020(2) C32 0.033(2) 0.039(2) 0.039(2) -0.016(2) 0.0045(19) -0.0053(18) C33 0.043(3) 0.048(3) 0.027(2) 0.001(2) 0.005(2) -0.001(2) C35 0.033(2) 0.042(2) 0.036(2) 0.003(2) -0.0011(18) -0.0071(18) C36 0.037(2) 0.026(2) 0.035(2) -0.0184(18) -0.0020(18) -0.0124(17) C37 0.048(3) 0.024(2) 0.043(3) 0.0007(19) -0.012(2) 0.0008(18) C38 0.035(2) 0.043(2) 0.038(2) -0.008(2) 0.0032(19) 0.0069(18) C39 0.034(2) 0.036(2) 0.047(3) 0.000(2) 0.004(2) 0.0161(18) C40 0.023(2) 0.039(2) 0.041(2) 0.0051(19) 0.0138(18) -0.0096(17) C41 0.037(2) 0.0239(19) 0.038(2) -0.0230(18) 0.0110(17) -0.0086(16) C42 0.042(2) 0.030(2) 0.052(3) -0.013(2) 0.024(2) -0.0110(18) C43 0.042(3) 0.047(3) 0.034(2) 0.014(2) -0.013(2) -0.008(2) C44 0.043(3) 0.047(3) 0.045(3) 0.002(2) -0.001(2) -0.015(2) C45 0.042(3) 0.053(3) 0.037(3) 0.014(2) -0.018(2) -0.011(2) Mn1 0.0278(3) 0.0272(3) 0.0180(3) -0.0009(2) 0.0051(2) -0.0024(2) Mn2 0.0345(3) 0.0389(3) 0.0338(3) 0.0000(3) 0.0028(3) 0.0006(3) Mn3 0.0323(3) 0.0347(3) 0.0394(4) 0.0000(3) 0.0072(3) -0.0002(3) N1 0.041(2) 0.038(2) 0.043(2) -0.0062(17) -0.0174(18) -0.0194(16) N2 0.033(2) 0.043(2) 0.050(2) -0.0056(18) 0.0003(18) 0.0024(16) O1 0.0275(13) 0.0284(14) 0.0396(16) 0.0106(12) 0.0183(12) 0.0141(11) O2 0.0359(16) 0.0421(16) 0.0388(17) 0.0072(14) 0.0028(13) 0.0053(13) O3 0.0440(17) 0.0413(16) 0.0350(17) -0.0126(14) 0.0043(14) 0.0020(14) O4 0.0471(18) 0.0382(16) 0.0396(18) 0.0054(14) 0.0096(14) 0.0112(14) O5 0.0485(19) 0.0415(17) 0.0419(18) 0.0138(15) -0.0138(15) 0.0095(14) O6 0.0366(16) 0.0500(18) 0.0350(16) 0.0170(14) 0.0026(13) -0.0134(13) O7 0.0339(15) 0.0333(15) 0.0429(17) 0.0003(13) 0.0077(13) -0.0183(12) O8 0.0420(17) 0.0279(15) 0.0437(19) -0.0062(13) -0.0014(14) -0.0035(12) O9 0.0461(18) 0.0395(17) 0.0460(19) 0.0024(14) -0.0059(15) 0.0081(14) O10 0.0255(14) 0.0361(15) 0.0434(17) 0.0062(13) 0.0195(12) 0.0120(11) O11 0.0439(17) 0.0404(16) 0.0342(16) 0.0054(13) 0.0029(14) 0.0090(13) O12 0.0279(15) 0.0392(16) 0.0463(18) 0.0037(14) 0.0093(13) -0.0020(12) O13 0.0511(19) 0.0457(17) 0.0367(17) -0.0038(14) 0.0028(14) -0.0365(15) O14 0.0396(16) 0.0334(15) 0.0402(17) 0.0127(13) -0.0201(14) -0.0181(12) O15 0.0454(18) 0.0394(16) 0.0351(17) 0.0018(14) -0.0057(14) -0.0117(14) O16 0.0475(18) 0.0396(16) 0.0363(17) -0.0049(14) 0.0041(14) -0.0118(14) O17 0.0417(16) 0.0433(16) 0.0297(15) -0.0029(13) 0.0127(13) -0.0185(13) O18 0.0375(16) 0.0466(17) 0.0374(16) -0.0110(14) -0.0079(13) -0.0252(14) O19 0.0325(15) 0.0348(15) 0.0435(18) -0.0054(13) 0.0005(13) 0.0001(12) O20 0.0365(15) 0.0397(15) 0.0276(14) -0.0129(12) 0.0048(12) -0.0157(12) O21 0.084(7) 0.031(4) 0.066(6) 0.009(4) 0.003(5) 0.002(4) O22 0.085(5) 0.067(4) 0.049(4) -0.014(3) 0.024(3) -0.012(3) O23 0.046(3) 0.043(3) 0.033(3) 0.007(2) -0.011(2) -0.028(2) O24 0.036(4) 0.045(4) 0.038(4) -0.003(3) -0.012(3) -0.013(3) O25 0.049(4) 0.036(4) 0.029(4) -0.002(3) -0.001(3) -0.008(3) O26 0.053(3) 0.044(3) 0.053(3) -0.002(3) 0.029(3) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.344(6) . ? C1 C6 1.430(6) . ? C1 C14 1.440(5) . ? C2 C3 1.365(6) . ? C2 H2A 0.9300 . ? C3 C4 1.357(6) . ? C3 C15 1.501(6) . ? C4 C5 1.391(6) . ? C4 H4A 0.9300 . ? C5 C6 1.446(6) . ? C5 C7 1.534(6) . ? C6 H6A 0.9300 . ? C7 C8 1.559(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.360(6) . ? C8 C13 1.397(6) . ? C9 C10 1.426(7) . ? C9 H9A 0.9300 . ? C10 C11 1.396(6) . ? C10 C16 1.512(6) . ? C11 C12 1.372(6) . ? C11 H11A 0.9300 . ? C12 C13 1.391(6) . ? C12 C17 1.507(6) . ? C13 H13A 0.9300 . ? C14 O2 1.272(5) . ? C14 O1 1.291(5) . ? C15 O3 1.256(6) . ? C15 O4 1.260(5) . ? C16 O6 1.243(6) . ? C16 O5 1.249(6) . ? C17 O8 1.230(6) . ? C17 O7 1.299(6) . ? C18 C23 1.357(6) . ? C18 C19 1.467(6) . ? C18 C31 1.523(6) . ? C19 C20 1.375(6) . ? C19 H19B 0.9300 . ? C20 C21 1.416(6) . ? C20 C32 1.450(6) . ? C21 C22 1.398(6) . ? C21 H21A 0.9300 . ? C22 C23 1.431(6) . ? C22 C24 1.507(6) . ? C23 H23A 0.9300 . ? C24 C25 1.476(6) . ? C24 H24A 0.9300 . ? C25 C30 1.386(6) . ? C25 C26 1.420(6) . ? C26 C27 1.413(6) . ? C26 H26E 0.9300 . ? C27 C28 1.342(6) . ? C27 C45 1.515(6) . ? C28 C29 1.374(6) . ? C28 H28A 0.9300 . ? C29 C30 1.430(6) . ? C29 C33 1.513(6) . ? C30 H30A 0.9300 . ? C31 O10 1.226(5) . ? C31 O9 1.244(5) . ? C32 O12 1.234(5) . ? C32 O11 1.281(5) . ? C33 O15 1.219(5) . ? C33 O16 1.224(5) . ? C35 C36 1.341(6) . ? C35 N1 1.365(6) . ? C35 H35A 0.9300 . ? C36 C37 1.375(6) . ? C36 H36A 0.9300 . ? C37 C38 1.459(7) . ? C37 C40 1.477(6) . ? C38 C39 1.321(6) . ? C38 H38A 0.9300 . ? C39 N1 1.340(5) . ? C39 H39A 0.9300 . ? C40 C44 1.353(6) . ? C40 C41 1.451(5) . ? C41 C42 1.384(6) . ? C41 H41A 0.9300 . ? C42 N2 1.333(6) . ? C42 H42A 0.9300 . ? C43 N2 1.362(6) . ? C43 C44 1.392(6) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 O13 1.220(5) . ? C45 O14 1.267(5) . ? Mn1 O7 2.097(3) 2_556 ? Mn1 O4 2.131(3) 2_656 ? Mn1 O18 2.161(3) . ? Mn1 O17 2.196(3) . ? Mn1 O2 2.288(3) . ? Mn1 O1 2.291(2) . ? Mn2 O3 2.134(3) 2_656 ? Mn2 O11 2.138(3) 2_546 ? Mn2 O16 2.172(3) 2_646 ? Mn2 O8 2.185(3) 2_556 ? Mn2 O2 2.186(3) . ? Mn2 O9 2.211(3) . ? Mn3 O12 2.094(3) 2_546 ? Mn3 O20 2.170(3) . ? Mn3 O15 2.185(3) 2_646 ? Mn3 O19 2.230(3) . ? Mn3 O10 2.294(3) . ? Mn3 O9 2.332(3) . ? O3 Mn2 2.134(3) 2_646 ? O4 Mn1 2.131(3) 2_646 ? O6 H6D 0.9601 . ? O7 Mn1 2.097(3) 2_546 ? O8 Mn2 2.185(3) 2_546 ? O11 Mn2 2.138(3) 2_556 ? O12 Mn3 2.094(3) 2_556 ? O13 H13D 0.9601 . ? O15 Mn3 2.185(3) 2_656 ? O16 Mn2 2.172(3) 2_656 ? O17 H17A 0.8502 . ? O17 H17B 0.8501 . ? O18 H18A 0.8500 . ? O18 H18C 0.8500 . ? O19 H19A 0.8500 . ? O19 H19C 0.8501 . ? O20 H20A 0.8500 . ? O20 H20C 0.8499 . ? O21 H21D 0.8500 . ? O21 H21B 0.8500 . ? O22 H22A 0.8500 . ? O22 H22B 0.8501 . ? O23 H23B 0.8500 . ? O23 H23C 0.8500 . ? O24 H24C 0.8501 . ? O24 H24B 0.8503 . ? O25 H25D 0.8500 . ? O25 H25A 0.8500 . ? O26 H26A 0.8500 . ? O26 H26C 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 116.8(3) . . ? C2 C1 C14 126.8(4) . . ? C6 C1 C14 116.3(3) . . ? C1 C2 C3 126.6(4) . . ? C1 C2 H2A 116.7 . . ? C3 C2 H2A 116.7 . . ? C4 C3 C2 117.6(4) . . ? C4 C3 C15 121.3(4) . . ? C2 C3 C15 120.9(4) . . ? C3 C4 C5 121.6(4) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? C4 C5 C6 119.2(4) . . ? C4 C5 C7 125.3(4) . . ? C6 C5 C7 115.2(4) . . ? C1 C6 C5 118.1(3) . . ? C1 C6 H6A 121.0 . . ? C5 C6 H6A 121.0 . . ? C5 C7 C8 114.0(4) . . ? C5 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C5 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C13 120.4(4) . . ? C9 C8 C7 122.7(4) . . ? C13 C8 C7 116.7(4) . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 118.5(4) . . ? C11 C10 C16 122.0(4) . . ? C9 C10 C16 119.5(4) . . ? C12 C11 C10 119.5(5) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 122.0(4) . . ? C11 C12 C17 118.2(4) . . ? C13 C12 C17 119.8(4) . . ? C12 C13 C8 118.3(4) . . ? C12 C13 H13A 120.8 . . ? C8 C13 H13A 120.8 . . ? O2 C14 O1 117.9(4) . . ? O2 C14 C1 122.8(4) . . ? O1 C14 C1 119.3(3) . . ? O3 C15 O4 123.6(4) . . ? O3 C15 C3 117.8(4) . . ? O4 C15 C3 118.4(4) . . ? O6 C16 O5 125.0(4) . . ? O6 C16 C10 116.8(4) . . ? O5 C16 C10 118.2(5) . . ? O8 C17 O7 124.3(4) . . ? O8 C17 C12 118.7(5) . . ? O7 C17 C12 116.8(4) . . ? C23 C18 C19 122.0(4) . . ? C23 C18 C31 121.4(4) . . ? C19 C18 C31 116.6(4) . . ? C20 C19 C18 118.8(4) . . ? C20 C19 H19B 120.6 . . ? C18 C19 H19B 120.6 . . ? C19 C20 C21 117.9(4) . . ? C19 C20 C32 122.3(4) . . ? C21 C20 C32 119.8(4) . . ? C22 C21 C20 123.6(4) . . ? C22 C21 H21A 118.2 . . ? C20 C21 H21A 118.2 . . ? C21 C22 C23 117.6(4) . . ? C21 C22 C24 122.8(4) . . ? C23 C22 C24 119.6(4) . . ? C18 C23 C22 119.2(4) . . ? C18 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C25 C24 C22 118.1(4) . . ? C25 C24 H24A 121.0 . . ? C22 C24 H24A 121.0 . . ? C30 C25 C26 117.7(4) . . ? C30 C25 C24 122.8(4) . . ? C26 C25 C24 119.2(4) . . ? C27 C26 C25 120.1(4) . . ? C27 C26 H26E 120.0 . . ? C25 C26 H26E 120.0 . . ? C28 C27 C26 119.4(4) . . ? C28 C27 C45 120.9(4) . . ? C26 C27 C45 119.4(4) . . ? C27 C28 C29 123.9(4) . . ? C27 C28 H28A 118.0 . . ? C29 C28 H28A 118.0 . . ? C28 C29 C30 116.7(4) . . ? C28 C29 C33 123.7(4) . . ? C30 C29 C33 119.5(4) . . ? C25 C30 C29 122.0(4) . . ? C25 C30 H30A 119.0 . . ? C29 C30 H30A 119.0 . . ? O10 C31 O9 121.7(4) . . ? O10 C31 C18 122.5(4) . . ? O9 C31 C18 115.8(4) . . ? O12 C32 O11 123.1(4) . . ? O12 C32 C20 121.2(4) . . ? O11 C32 C20 115.6(4) . . ? O15 C33 O16 128.6(4) . . ? O15 C33 C29 114.5(4) . . ? O16 C33 C29 116.9(4) . . ? C36 C35 N1 123.6(4) . . ? C36 C35 H35A 118.2 . . ? N1 C35 H35A 118.2 . . ? C35 C36 C37 119.3(4) . . ? C35 C36 H36A 120.4 . . ? C37 C36 H36A 120.4 . . ? C36 C37 C38 117.3(4) . . ? C36 C37 C40 122.2(4) . . ? C38 C37 C40 120.5(4) . . ? C39 C38 C37 118.8(4) . . ? C39 C38 H38A 120.6 . . ? C37 C38 H38A 120.6 . . ? C38 C39 N1 123.5(4) . . ? C38 C39 H39A 118.2 . . ? N1 C39 H39A 118.2 . . ? C44 C40 C41 121.0(4) . . ? C44 C40 C37 121.5(4) . . ? C41 C40 C37 117.5(4) . . ? C42 C41 C40 115.7(4) . . ? C42 C41 H41A 122.2 . . ? C40 C41 H41A 122.2 . . ? N2 C42 C41 123.9(4) . . ? N2 C42 H42A 118.0 . . ? C41 C42 H42A 118.0 . . ? N2 C43 C44 123.1(4) . . ? N2 C43 H43A 118.5 . . ? C44 C43 H43A 118.5 . . ? C40 C44 C43 117.9(4) . . ? C40 C44 H44A 121.1 . . ? C43 C44 H44A 121.1 . . ? O13 C45 O14 126.6(4) . . ? O13 C45 C27 116.4(4) . . ? O14 C45 C27 116.4(4) . . ? O7 Mn1 O4 91.26(12) 2_556 2_656 ? O7 Mn1 O18 104.16(12) 2_556 . ? O4 Mn1 O18 84.16(11) 2_656 . ? O7 Mn1 O17 87.15(12) 2_556 . ? O4 Mn1 O17 167.91(11) 2_656 . ? O18 Mn1 O17 84.61(10) . . ? O7 Mn1 O2 97.91(11) 2_556 . ? O4 Mn1 O2 103.22(11) 2_656 . ? O18 Mn1 O2 156.60(11) . . ? O17 Mn1 O2 88.88(11) . . ? O7 Mn1 O1 154.89(11) 2_556 . ? O4 Mn1 O1 98.09(11) 2_656 . ? O18 Mn1 O1 99.95(11) . . ? O17 Mn1 O1 88.26(11) . . ? O2 Mn1 O1 57.31(9) . . ? O3 Mn2 O11 176.34(12) 2_656 2_546 ? O3 Mn2 O16 86.68(11) 2_656 2_646 ? O11 Mn2 O16 94.96(12) 2_546 2_646 ? O3 Mn2 O8 91.80(11) 2_656 2_556 ? O11 Mn2 O8 86.71(11) 2_546 2_556 ? O16 Mn2 O8 176.98(11) 2_646 2_556 ? O3 Mn2 O2 89.35(12) 2_656 . ? O11 Mn2 O2 87.36(11) 2_546 . ? O16 Mn2 O2 90.36(11) 2_646 . ? O8 Mn2 O2 92.23(11) 2_556 . ? O3 Mn2 O9 92.02(12) 2_656 . ? O11 Mn2 O9 91.34(12) 2_546 . ? O16 Mn2 O9 87.10(11) 2_646 . ? O8 Mn2 O9 90.35(11) 2_556 . ? O2 Mn2 O9 177.04(11) . . ? O12 Mn3 O20 85.67(11) 2_546 . ? O12 Mn3 O15 88.12(11) 2_546 2_646 ? O20 Mn3 O15 116.54(12) . 2_646 ? O12 Mn3 O19 161.89(12) 2_546 . ? O20 Mn3 O19 84.42(10) . . ? O15 Mn3 O19 82.82(11) 2_646 . ? O12 Mn3 O10 103.89(11) 2_546 . ? O20 Mn3 O10 91.99(10) . . ? O15 Mn3 O10 150.02(11) 2_646 . ? O19 Mn3 O10 91.58(11) . . ? O12 Mn3 O9 102.93(12) 2_546 . ? O20 Mn3 O9 147.50(11) . . ? O15 Mn3 O9 95.24(11) 2_646 . ? O19 Mn3 O9 93.52(11) . . ? O10 Mn3 O9 55.58(10) . . ? C39 N1 C35 117.5(4) . . ? C42 N2 C43 118.0(4) . . ? C14 O1 Mn1 91.9(2) . . ? C14 O2 Mn2 139.5(3) . . ? C14 O2 Mn1 92.5(3) . . ? Mn2 O2 Mn1 107.17(12) . . ? C15 O3 Mn2 151.0(3) . 2_646 ? C15 O4 Mn1 122.6(3) . 2_646 ? C16 O6 H6D 109.6 . . ? C17 O7 Mn1 133.5(3) . 2_546 ? C17 O8 Mn2 136.9(3) . 2_546 ? C31 O9 Mn2 138.4(3) . . ? C31 O9 Mn3 90.2(3) . . ? Mn2 O9 Mn3 107.35(12) . . ? C31 O10 Mn3 92.5(2) . . ? C32 O11 Mn2 148.5(3) . 2_556 ? C32 O12 Mn3 128.5(3) . 2_556 ? C45 O13 H13D 109.5 . . ? C33 O15 Mn3 129.0(3) . 2_656 ? C33 O16 Mn2 136.6(3) . 2_656 ? Mn1 O17 H17A 109.6 . . ? Mn1 O17 H17B 109.8 . . ? H17A O17 H17B 109.5 . . ? Mn1 O18 H18A 109.5 . . ? Mn1 O18 H18C 109.5 . . ? H18A O18 H18C 109.5 . . ? Mn3 O19 H19A 109.1 . . ? Mn3 O19 H19C 109.9 . . ? H19A O19 H19C 109.5 . . ? Mn3 O20 H20A 109.1 . . ? Mn3 O20 H20C 109.8 . . ? H20A O20 H20C 109.5 . . ? H21D O21 H21B 109.5 . . ? H22A O22 H22B 109.8 . . ? H23B O23 H23C 109.5 . . ? H24C O24 H24B 109.4 . . ? H25D O25 H25A 109.5 . . ? H26A O26 H26C 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 H6D O26 0.96 1.88 2.666(6) 136.7 1_446 O13 H13D O24 0.96 2.38 3.327(8) 167.3 3_666 O19 H19C N2 0.85 2.40 3.151(4) 146.8 3_666 O26 H26C O20 0.85 2.28 2.851(6) 124.3 3_666 O17 H17A O6 0.85 2.04 2.647(4) 127.5 4 O18 H18C O5 0.85 2.00 2.660(4) 133.2 4 O17 H17B O25 0.85 2.17 2.734(8) 124.1 3_656 O18 H18A O22 0.85 2.26 2.741(7) 115.6 2_646 O19 H19A O24 0.85 2.26 2.919(7) 133.9 2_646 O20 H20A O21 0.85 2.56 3.257(9) 140.1 3_567 O20 H20C O25 0.85 2.46 3.282(8) 161.7 4_466 O22 H22B O5 0.85 2.20 2.726(7) 119.9 1_565 O26 H26A O6 0.85 1.97 2.666(6) 138.7 1_664 O23 H23B O19 0.85 2.03 2.640(6) 128.1 . O24 H24C O14 0.85 2.12 2.951(7) 166.3 . O25 H25A N1 0.85 2.03 2.750(8) 141.6 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.776 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.066 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 656231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H32 Co5 O25, 6(H2 O)' _chemical_formula_sum 'C34 H44 Co5 O31' _chemical_formula_weight 1243.34 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9387(16) _cell_length_b 8.4653(14) _cell_length_c 25.115(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.560(3) _cell_angle_gamma 90.00 _cell_volume 2112.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 706 _cell_measurement_theta_min 2.539 _cell_measurement_theta_max 21.932 _exptl_crystal_description piece _exptl_crystal_colour purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1262 _exptl_absorpt_coefficient_mu 2.033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.72 _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 11046 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4154 _reflns_number_gt 3444 _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^)+(0.0800P)^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 4154 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.1063(6) 0.1385(6) 0.1275(2) 0.0434(12) Uani 1 1 d . . . C2 C 0.1248(5) 0.0326(6) 0.1688(2) 0.0385(11) Uani 1 1 d . . . H2 H 0.0512 -0.0100 0.1863 0.046 Uiso 1 1 calc R . . C3 C 0.2584(5) -0.0105(6) 0.18406(19) 0.0353(10) Uani 1 1 d . . . C4 C 0.3655(5) 0.0567(5) 0.15821(18) 0.0334(10) Uani 1 1 d . . . H4 H 0.4529 0.0320 0.1689 0.040 Uiso 1 1 calc R . . C5 C 0.3435(5) 0.1630(6) 0.11549(19) 0.0377(11) Uani 1 1 d . . . C6 C 0.2148(4) 0.2034(5) 0.10079(17) 0.0297(9) Uani 1 1 d . . . H6 H 0.2002 0.2741 0.0730 0.036 Uiso 1 1 calc R . . C7 C -0.0351(4) 0.1949(6) 0.11410(19) 0.0352(10) Uani 1 1 d . . . C8 C 0.4610(4) 0.2439(6) 0.08950(18) 0.0328(10) Uani 1 1 d . . . C9 C 0.2809(5) -0.1310(6) 0.2288(2) 0.0378(11) Uani 1 1 d . . . H9A H 0.2031 -0.1997 0.2314 0.045 Uiso 1 1 calc R . . H9B H 0.3587 -0.1958 0.2209 0.045 Uiso 1 1 calc R . . C10 C 0.3030(5) -0.0461(6) 0.28053(19) 0.0377(11) Uani 1 1 d . . . C11 C 0.1961(5) -0.0007(6) 0.3110(2) 0.0409(11) Uani 1 1 d . . . H11 H 0.1092 -0.0193 0.2984 0.049 Uiso 1 1 calc R . . C12 C 0.2140(5) 0.0734(6) 0.3607(2) 0.0366(10) Uani 1 1 d . . . C13 C 0.3410(4) 0.1059(6) 0.37869(18) 0.0348(10) Uani 1 1 d . . . H13 H 0.3535 0.1572 0.4111 0.042 Uiso 1 1 calc R . . C14 C 0.4519(4) 0.0623(5) 0.34853(18) 0.0321(10) Uani 1 1 d . . . C15 C 0.4342(5) -0.0168(6) 0.3006(2) 0.0401(11) Uani 1 1 d . . . H15 H 0.5087 -0.0506 0.2816 0.048 Uiso 1 1 calc R . . C16 C 0.0927(5) 0.1167(6) 0.3926(2) 0.0397(11) Uani 1 1 d . . . C17 C 0.5909(5) 0.1002(6) 0.36798(18) 0.0363(10) Uani 1 1 d . . . Co1 Co -0.25494(7) 0.32667(8) 0.08763(3) 0.0381(2) Uani 1 1 d . . . Co2 Co -0.31571(7) 0.70410(8) 0.09786(3) 0.0383(2) Uani 1 1 d . . . Co3 Co -0.5000 0.5000 0.0000 0.0292(2) Uani 1 2 d S . . O1 O -0.3194(4) 0.5138(4) 0.04284(14) 0.0399(8) Uani 1 1 d . . . H1A H -0.2487 0.5351 0.0169 0.048 Uiso 1 1 calc R . . O2 O -0.1375(3) 0.1509(4) 0.13924(13) 0.0364(7) Uani 1 1 d . . . O3 O -0.0508(3) 0.2957(4) 0.07606(14) 0.0409(8) Uani 1 1 d . . . O4 O 0.4429(3) 0.2925(4) 0.04316(13) 0.0388(8) Uani 1 1 d . . . O5 O 0.5667(3) 0.2570(4) 0.11703(14) 0.0386(8) Uani 1 1 d . . . O6 O -0.0160(4) 0.1354(4) 0.36789(14) 0.0396(8) Uani 1 1 d . . . O7 O 0.1058(3) 0.1326(4) 0.44282(13) 0.0395(8) Uani 1 1 d . . . O8 O 0.6075(3) 0.2157(4) 0.39800(13) 0.0353(8) Uani 1 1 d . . . O9 O 0.6906(3) 0.0183(4) 0.35464(13) 0.0345(7) Uani 1 1 d . . . O10 O -0.2873(4) 0.1836(4) 0.01879(14) 0.0429(8) Uani 1 1 d . . . H10B H -0.2717 0.2421 -0.0080 0.051 Uiso 1 1 d R . . H10C H -0.3702 0.1597 0.0168 0.051 Uiso 1 1 d R . . O11 O -0.3525(3) 0.8670(4) 0.04083(12) 0.0353(7) Uani 1 1 d . . . H11A H -0.3582 0.8217 0.0107 0.053 Uiso 1 1 d R . . H11C H -0.2884 0.9334 0.0405 0.053 Uiso 1 1 d R . . O12 O -0.3143(3) 0.8833(4) 0.15785(13) 0.0378(8) Uani 1 1 d . . . H12C H -0.2469 0.8687 0.1784 0.045 Uiso 1 1 d R . . H12A H -0.3085 0.9739 0.1435 0.057 Uiso 1 1 d R . . O13 O 0.6646(3) 0.6769(4) 0.24695(12) 0.0372(8) Uani 1 1 d . . . H13D H 0.6033 0.6179 0.2339 0.045 Uiso 1 1 d R . . H13C H 0.6385 0.7146 0.2765 0.045 Uiso 1 1 d R . . O14 O 0.9697(4) 0.1155(4) 0.97144(15) 0.0476(9) Uani 1 1 d . . . H14D H 0.8973 0.0833 0.9855 0.057 Uiso 1 1 d R . . H14B H 0.9695 0.0872 0.9390 0.057 Uiso 1 1 d R . . O15 O 0.5962(3) 0.3432(4) 0.23008(13) 0.0368(8) Uani 1 1 d . . . H15A H 0.5813 0.2504 0.2185 0.044 Uiso 1 1 d R . . H15C H 0.6787 0.3662 0.2259 0.044 Uiso 1 1 d R . . O16 O 0.9376(7) 0.5160(9) 0.9997(3) 0.0436(17) Uani 0.50 1 d P . . H16D H 0.8591 0.5154 1.0129 0.052 Uiso 0.50 1 d PR . . H16B H 0.9514 0.6043 0.9846 0.065 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 0.048(3) 0.040(3) 0.043(3) 0.001(2) 0.002(2) -0.003(2) C2 0.030(2) 0.048(3) 0.038(3) 0.003(2) -0.0043(19) -0.005(2) C3 0.031(2) 0.042(3) 0.032(2) 0.006(2) 0.0061(18) 0.002(2) C4 0.042(3) 0.028(2) 0.030(2) 0.0017(18) -0.0029(19) 0.0017(19) C5 0.042(3) 0.041(3) 0.030(2) 0.0021(19) 0.001(2) -0.001(2) C6 0.027(2) 0.029(2) 0.033(2) 0.0102(18) -0.0034(17) -0.0032(17) C7 0.026(2) 0.041(3) 0.039(2) 0.011(2) -0.0035(18) 0.0040(19) C8 0.028(2) 0.038(2) 0.033(2) -0.0007(19) 0.0010(18) -0.0025(19) C9 0.028(2) 0.044(3) 0.042(3) -0.003(2) -0.0022(19) 0.006(2) C10 0.031(2) 0.045(3) 0.037(3) -0.004(2) -0.0065(19) 0.003(2) C11 0.043(3) 0.035(3) 0.044(3) -0.006(2) 0.003(2) -0.004(2) C12 0.038(3) 0.030(2) 0.042(3) 0.003(2) 0.001(2) 0.0045(19) C13 0.029(2) 0.044(3) 0.031(2) 0.004(2) -0.0004(18) -0.003(2) C14 0.026(2) 0.030(2) 0.040(2) 0.0022(19) -0.0051(18) 0.0001(17) C15 0.042(3) 0.046(3) 0.033(2) 0.000(2) -0.002(2) 0.001(2) C16 0.043(3) 0.034(2) 0.043(3) -0.008(2) 0.005(2) 0.003(2) C17 0.044(3) 0.036(3) 0.029(2) -0.0025(19) -0.0070(19) -0.003(2) Co1 0.0401(4) 0.0302(3) 0.0439(4) -0.0021(3) -0.0014(3) -0.0006(3) Co2 0.0401(4) 0.0302(4) 0.0445(4) -0.0018(3) -0.0010(3) 0.0011(3) Co3 0.0282(4) 0.0307(5) 0.0287(4) -0.0018(3) 0.0017(3) -0.0007(3) O1 0.0464(19) 0.0312(17) 0.0419(19) -0.0010(14) -0.0057(15) 0.0026(15) O2 0.0426(18) 0.0304(17) 0.0362(17) -0.0069(13) -0.0034(14) 0.0007(14) O3 0.0372(18) 0.043(2) 0.0428(19) -0.0034(16) -0.0082(15) -0.0050(15) O4 0.0343(17) 0.043(2) 0.0389(18) -0.0070(15) -0.0006(14) 0.0081(15) O5 0.0450(19) 0.0267(16) 0.0442(19) -0.0089(14) 0.0107(15) 0.0003(14) O6 0.045(2) 0.0308(18) 0.0433(19) 0.0001(14) 0.0036(16) -0.0037(15) O7 0.0383(18) 0.046(2) 0.0348(18) -0.0004(15) 0.0014(14) 0.0091(15) O8 0.0297(16) 0.0314(17) 0.0449(19) 0.0226(15) 0.0013(14) 0.0048(13) O9 0.0413(18) 0.0281(16) 0.0341(17) 0.0024(13) -0.0022(14) -0.0001(14) O10 0.048(2) 0.0382(19) 0.0422(19) 0.0057(15) 0.0002(16) -0.0079(15) O11 0.0274(15) 0.0448(19) 0.0334(17) -0.0099(14) -0.0190(13) 0.0078(14) O12 0.0293(16) 0.0397(19) 0.0445(19) 0.0043(15) 0.0030(14) 0.0023(14) O13 0.0389(18) 0.0442(19) 0.0284(16) 0.0042(14) -0.0030(13) -0.0152(15) O14 0.054(2) 0.043(2) 0.046(2) 0.0137(17) 0.0059(17) -0.0053(17) O15 0.0360(17) 0.0384(18) 0.0361(17) -0.0150(14) 0.0010(14) 0.0176(14) O16 0.027(3) 0.052(4) 0.051(4) 0.016(3) -0.013(3) 0.007(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 C1 C2 1.381(7) . ? C1 C6 1.390(7) . ? C1 C7 1.518(7) . ? C2 C3 1.426(7) . ? C2 H2 0.9300 . ? C3 C4 1.375(7) . ? C3 C9 1.532(7) . ? C4 C5 1.416(6) . ? C4 H4 0.9300 . ? C5 C6 1.371(7) . ? C5 C8 1.508(7) . ? C6 H6 0.9300 . ? C7 O2 1.260(6) . ? C7 O3 1.290(6) . ? C8 O4 1.246(6) . ? C8 O5 1.257(6) . ? C9 C10 1.500(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.370(7) . ? C10 C15 1.416(7) . ? C11 C12 1.408(7) . ? C11 H11 0.9300 . ? C12 C13 1.364(7) . ? C12 C16 1.499(7) . ? C13 C14 1.393(6) . ? C13 H13 0.9300 . ? C14 C15 1.388(7) . ? C14 C17 1.496(6) . ? C15 H15 0.9300 . ? C16 O6 1.250(6) . ? C16 O7 1.274(6) . ? C17 O8 1.244(6) . ? C17 O9 1.257(6) . ? Co1 O5 2.015(3) 1_455 ? Co1 O1 2.042(3) . ? Co1 O3 2.069(3) . ? Co1 O10 2.132(4) . ? Co1 O9 2.263(3) 2 ? Co1 O2 2.286(3) . ? Co2 O6 1.976(4) 2_455 ? Co2 O11 2.019(3) . ? Co2 O8 2.074(3) 2 ? Co2 O1 2.122(3) . ? Co2 O12 2.138(3) . ? Co2 O9 2.327(3) 2 ? Co3 O1 2.087(4) 3_465 ? Co3 O1 2.087(4) . ? Co3 O7 2.112(3) 2_455 ? Co3 O7 2.112(3) 4_565 ? Co3 O4 2.144(4) 1_455 ? Co3 O4 2.144(4) 3_565 ? O1 H1A 0.9800 . ? O4 Co3 2.144(4) 1_655 ? O5 Co1 2.015(3) 1_655 ? O6 Co2 1.976(4) 2_445 ? O7 Co3 2.112(3) 2_445 ? O8 Co2 2.074(3) 2_545 ? O9 Co1 2.263(3) 2_545 ? O9 Co2 2.327(3) 2_545 ? O10 H10B 0.8500 . ? O10 H10C 0.8500 . ? O11 H11A 0.8499 . ? O11 H11C 0.8501 . ? O12 H12C 0.8499 . ? O12 H12A 0.8500 . ? O13 H13D 0.8501 . ? O13 H13C 0.8499 . ? O14 H14D 0.8500 . ? O14 H14B 0.8500 . ? O15 H15A 0.8499 . ? O15 H15C 0.8501 . ? O16 O16 1.271(13) 3_767 ? O16 H16D 0.8499 . ? O16 H16B 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 121.4(5) . . ? C2 C1 C7 119.1(4) . . ? C6 C1 C7 119.3(4) . . ? C1 C2 C3 119.0(4) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 119.3(4) . . ? C4 C3 C9 120.9(4) . . ? C2 C3 C9 119.8(4) . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.9(4) . . ? C6 C5 C8 119.6(4) . . ? C4 C5 C8 120.2(4) . . ? C5 C6 C1 119.9(4) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? O2 C7 O3 118.3(4) . . ? O2 C7 C1 123.1(4) . . ? O3 C7 C1 118.5(4) . . ? O4 C8 O5 126.7(4) . . ? O4 C8 C5 116.7(4) . . ? O5 C8 C5 116.6(4) . . ? C10 C9 C3 109.6(4) . . ? C10 C9 H9A 109.8 . . ? C3 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? C3 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C15 118.0(5) . . ? C11 C10 C9 120.7(4) . . ? C15 C10 C9 121.2(4) . . ? C10 C11 C12 121.9(5) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 119.5(5) . . ? C13 C12 C16 121.4(5) . . ? C11 C12 C16 119.2(5) . . ? C12 C13 C14 120.1(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.4(4) . . ? C15 C14 C17 119.7(4) . . ? C13 C14 C17 119.9(4) . . ? C14 C15 C10 120.1(4) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? O6 C16 O7 123.9(4) . . ? O6 C16 C12 117.5(4) . . ? O7 C16 C12 118.6(5) . . ? O8 C17 O9 119.7(4) . . ? O8 C17 C14 118.8(4) . . ? O9 C17 C14 121.5(4) . . ? O5 Co1 O1 99.01(15) 1_455 . ? O5 Co1 O3 151.85(15) 1_455 . ? O1 Co1 O3 108.86(14) . . ? O5 Co1 O10 90.27(14) 1_455 . ? O1 Co1 O10 87.13(14) . . ? O3 Co1 O10 87.40(14) . . ? O5 Co1 O9 102.65(13) 1_455 2 ? O1 Co1 O9 83.22(13) . 2 ? O3 Co1 O9 84.80(13) . 2 ? O10 Co1 O9 164.92(12) . 2 ? O5 Co1 O2 92.74(14) 1_455 . ? O1 Co1 O2 166.58(13) . . ? O3 Co1 O2 60.10(13) . . ? O10 Co1 O2 99.33(13) . . ? O9 Co1 O2 87.92(12) 2 . ? O6 Co2 O11 111.19(14) 2_455 . ? O6 Co2 O8 147.23(15) 2_455 2 ? O11 Co2 O8 100.21(13) . 2 ? O6 Co2 O1 92.91(14) 2_455 . ? O11 Co2 O1 93.12(13) . . ? O8 Co2 O1 94.54(13) 2 . ? O6 Co2 O12 84.38(13) 2_455 . ? O11 Co2 O12 90.88(13) . . ? O8 Co2 O12 86.06(12) 2 . ? O1 Co2 O12 175.78(13) . . ? O6 Co2 O9 91.62(13) 2_455 2 ? O11 Co2 O9 156.58(12) . 2 ? O8 Co2 O9 58.54(13) 2 2 ? O1 Co2 O9 80.00(12) . 2 ? O12 Co2 O9 96.81(12) . 2 ? O1 Co3 O1 180.00(17) 3_465 . ? O1 Co3 O7 87.06(13) 3_465 2_455 ? O1 Co3 O7 92.94(13) . 2_455 ? O1 Co3 O7 92.94(13) 3_465 4_565 ? O1 Co3 O7 87.06(13) . 4_565 ? O7 Co3 O7 180.00(13) 2_455 4_565 ? O1 Co3 O4 89.08(13) 3_465 1_455 ? O1 Co3 O4 90.92(13) . 1_455 ? O7 Co3 O4 87.46(12) 2_455 1_455 ? O7 Co3 O4 92.54(12) 4_565 1_455 ? O1 Co3 O4 90.92(13) 3_465 3_565 ? O1 Co3 O4 89.08(13) . 3_565 ? O7 Co3 O4 92.54(12) 2_455 3_565 ? O7 Co3 O4 87.46(12) 4_565 3_565 ? O4 Co3 O4 180.00(19) 1_455 3_565 ? Co1 O1 Co3 120.25(16) . . ? Co1 O1 Co2 103.11(16) . . ? Co3 O1 Co2 112.79(15) . . ? Co1 O1 H1A 106.6 . . ? Co3 O1 H1A 106.6 . . ? Co2 O1 H1A 106.6 . . ? C7 O2 Co1 86.2(3) . . ? C7 O3 Co1 95.3(3) . . ? C8 O4 Co3 134.9(3) . 1_655 ? C8 O5 Co1 123.9(3) . 1_655 ? C16 O6 Co2 123.5(3) . 2_445 ? C16 O7 Co3 124.7(3) . 2_445 ? C17 O8 Co2 96.8(3) . 2_545 ? C17 O9 Co1 116.3(3) . 2_545 ? C17 O9 Co2 84.8(3) . 2_545 ? Co1 O9 Co2 90.56(12) 2_545 2_545 ? Co1 O10 H10B 106.5 . . ? Co1 O10 H10C 108.7 . . ? H10B O10 H10C 106.1 . . ? Co2 O11 H11A 109.5 . . ? Co2 O11 H11C 109.1 . . ? H11A O11 H11C 109.5 . . ? Co2 O12 H12C 108.9 . . ? Co2 O12 H12A 109.9 . . ? H12C O12 H12A 109.5 . . ? H13D O13 H13C 109.5 . . ? H14D O14 H14B 108.3 . . ? H15A O15 H15C 109.5 . . ? O16 O16 H16D 153.4 3_767 . ? O16 O16 H16B 91.7 3_767 . ? H16D O16 H16B 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 O1 H1A O16 0.98 1.91 2.783(8) 146.8 1_454 O10 H10B O7 0.85 2.03 2.674(5) 132.4 4_565 O10 H10C O4 0.85 2.27 2.906(5) 131.3 1_455 O11 H11A O4 0.85 1.86 2.653(4) 155.4 3_565 O11 H11C O10 0.85 2.19 2.814(5) 130.4 1_565 O12 H12A O2 0.85 2.27 2.907(5) 132.0 1_565 O13 H13D O15 0.85 2.33 2.935(5) 128.6 . O13 H13C O2 0.85 2.18 2.882(5) 139.2 2 O14 H14D O10 0.85 2.19 2.886(5) 138.4 1_656 O16 H16D O1 0.85 1.93 2.783(8) 180.0 1_656 O15 H15C O13 0.85 2.33 2.818(4) 116.6 2_645 O16 H16B O3 0.85 2.01 2.733(8) 142.3 3_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.400 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.089