Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Chung, Young Keun' 'Lee, Seung Jung' 'Park, Kang Hyun' 'Son, Seung Uk' 'Sweigart, D.' _publ_contact_author_name 'Prof Young Keun Chung' _publ_contact_author_address ; Prof Young Keun Chung School of Chemistry Seoul National University Center for Molecular Catalysis Seoul 151-747 KOREA ; _publ_contact_author_email 'YKCHUNG@PLAZA.SNU.AC.KR' data_ct _database_code_CSD 157495 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 Mn O6 P' _chemical_formula_weight 532.39 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.0816(7) _cell_length_b 15.0390(4) _cell_length_c 10.9049(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.422(3) _cell_angle_gamma 90.00 _cell_volume 1325.34(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3105 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3105 _reflns_number_gt 2973 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1265P)^2^+3.7783P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 3105 _refine_ls_number_parameters 318 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.486 _refine_ls_restrained_S_all 0.486 _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 Mn Mn 0.20201(8) 0.63076(3) 0.65854(6) 0.04320(18) Uani 1 1 d . . . P P 0.36116(14) 0.69122(6) 0.94686(10) 0.0394(2) Uani 1 1 d . . . C1 C 0.1862(6) 0.7615(3) 0.7327(4) 0.0413(9) Uani 1 1 d . . . C2 C 0.1965(5) 0.6977(2) 0.8323(4) 0.0395(8) Uani 1 1 d . . . C3 C 0.0542(6) 0.6422(3) 0.8204(4) 0.0464(9) Uani 1 1 d . . . H3 H 0.0277 0.5948 0.8712 0.056 Uiso 1 1 calc R . . C4 C -0.0397(8) 0.6714(3) 0.7186(6) 0.0541(12) Uani 1 1 d . . . H4 H -0.1382 0.6460 0.6911 0.065 Uiso 1 1 calc R . . C5 C 0.0406(7) 0.7459(3) 0.6647(5) 0.0517(11) Uani 1 1 d . . . C6 C -0.0299(11) 0.8015(4) 0.5607(7) 0.0757(18) Uani 1 1 d . . . H6A H 0.0460 0.8485 0.5414 0.091 Uiso 1 1 calc R . . H6B H -0.1338 0.8266 0.5852 0.091 Uiso 1 1 calc R . . H6C H -0.0465 0.7647 0.4898 0.091 Uiso 1 1 calc R . . C7 C 0.3074(6) 0.8374(2) 0.7150(4) 0.0419(9) Uani 1 1 d . . . H7 H 0.4068 0.8276 0.7652 0.050 Uiso 1 1 calc R . . C8 C 0.4636(11) 0.9184(5) 0.5766(7) 0.082(2) Uani 1 1 d . . . H8A H 0.4943 0.9236 0.4911 0.098 Uiso 1 1 calc R . . H8B H 0.5634 0.9079 0.6244 0.098 Uiso 1 1 calc R . . C9 C 0.3823(10) 1.0040(4) 0.6185(6) 0.0717(18) Uani 1 1 d . . . H9A H 0.4603 1.0529 0.6134 0.086 Uiso 1 1 calc R . . H9B H 0.2879 1.0176 0.5665 0.086 Uiso 1 1 calc R . . C10 C 0.3274(7) 0.9920(3) 0.7490(5) 0.0503(11) Uani 1 1 d . . . H10 H 0.4239 0.9848 0.8030 0.060 Uiso 1 1 calc R . . C11 C 0.2163(9) 1.0665(3) 0.7966(7) 0.0702(17) Uani 1 1 d . . . H11A H 0.1146 1.0690 0.7490 0.084 Uiso 1 1 calc R . . H11B H 0.1884 1.0558 0.8817 0.084 Uiso 1 1 calc R . . C12 C 0.2037(13) 1.2192(5) 0.8221(13) 0.126(5) Uani 1 1 d . . . H12A H 0.2639 1.2736 0.8108 0.152 Uiso 1 1 calc R . . H12B H 0.1754 1.2129 0.9070 0.152 Uiso 1 1 calc R . . H12C H 0.1044 1.2206 0.7732 0.152 Uiso 1 1 calc R . . C13 C 0.2756(6) 0.7606(2) 1.0691(4) 0.0396(8) Uani 1 1 d . . . C14 C 0.3401(7) 0.7525(3) 1.1858(5) 0.0510(11) Uani 1 1 d . . . H14 H 0.4153 0.7073 1.2029 0.061 Uiso 1 1 calc R . . C15 C 0.2939(10) 0.8112(4) 1.2789(6) 0.0700(18) Uani 1 1 d . . . H15 H 0.3379 0.8050 1.3574 0.084 Uiso 1 1 calc R . . C16 C 0.1819(10) 0.8787(3) 1.2532(6) 0.0727(19) Uani 1 1 d . . . H16 H 0.1519 0.9186 1.3143 0.087 Uiso 1 1 calc R . . C17 C 0.1155(10) 0.8863(3) 1.1375(6) 0.0707(18) Uani 1 1 d . . . H17 H 0.0393 0.9312 1.1210 0.085 Uiso 1 1 calc R . . C18 C 0.1602(7) 0.8280(3) 1.0446(5) 0.0520(12) Uani 1 1 d . . . H18 H 0.1139 0.8336 0.9667 0.062 Uiso 1 1 calc R . . C19 C 0.3269(6) 0.5771(3) 1.0033(5) 0.0437(9) Uani 1 1 d . . . C20 C 0.2125(7) 0.5545(2) 1.0902(5) 0.0504(11) Uani 1 1 d . . . H20 H 0.1490 0.5986 1.1268 0.061 Uiso 1 1 calc R . . C21 C 0.1907(8) 0.4656(3) 1.1242(6) 0.0635(15) Uani 1 1 d . . . H21 H 0.1131 0.4509 1.1834 0.076 Uiso 1 1 calc R . . C22 C 0.2823(10) 0.4004(3) 1.0711(7) 0.0688(18) Uani 1 1 d . . . H22 H 0.2660 0.3412 1.0927 0.083 Uiso 1 1 calc R . . C23 C 0.3971(9) 0.4220(3) 0.9868(7) 0.074(2) Uani 1 1 d . . . H23 H 0.4596 0.3770 0.9514 0.089 Uiso 1 1 calc R . . C24 C 0.4247(8) 0.5097(3) 0.9514(6) 0.0580(13) Uani 1 1 d . . . H24 H 0.5061 0.5233 0.8946 0.070 Uiso 1 1 calc R . . C25 C 0.1647(9) 0.6176(4) 0.4968(6) 0.0687(15) Uani 1 1 d . . . C26 C 0.4194(8) 0.6391(5) 0.6358(6) 0.0679(16) Uani 1 1 d . . . C27 C 0.2182(8) 0.5124(3) 0.6736(6) 0.0601(14) Uani 1 1 d . . . O1 O 0.2227(4) 0.91426(17) 0.7560(3) 0.0474(7) Uani 1 1 d . . . O2 O 0.3501(6) 0.8444(2) 0.5918(4) 0.0665(12) Uani 1 1 d . . . O3 O 0.3028(7) 1.1466(2) 0.7857(7) 0.0946(19) Uani 1 1 d . . . O4 O 0.1403(11) 0.6088(4) 0.3958(5) 0.110(2) Uani 1 1 d . . . O5 O 0.5570(8) 0.6459(5) 0.6208(7) 0.118(3) Uani 1 1 d . . . O6 O 0.2311(9) 0.4369(3) 0.6815(6) 0.100(2) 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 Mn 0.0407(4) 0.0508(3) 0.0381(4) -0.0094(2) -0.0023(3) -0.0069(2) P 0.0389(6) 0.0441(5) 0.0353(6) -0.0045(3) 0.0028(4) -0.0003(3) C1 0.044(3) 0.047(2) 0.033(2) -0.0041(13) 0.0028(18) 0.0012(14) C2 0.039(2) 0.0430(19) 0.037(2) -0.0041(13) 0.0017(16) -0.0007(13) C3 0.037(3) 0.052(2) 0.049(3) -0.0023(15) 0.0029(19) -0.0068(15) C4 0.041(3) 0.069(3) 0.052(3) -0.0033(18) 0.002(2) -0.0074(17) C5 0.045(3) 0.060(3) 0.050(3) -0.0001(16) -0.005(2) -0.0008(16) C6 0.074(5) 0.093(4) 0.060(4) 0.010(3) -0.014(4) 0.012(3) C7 0.048(3) 0.047(2) 0.030(2) -0.0011(12) 0.0048(18) -0.0031(14) C8 0.096(6) 0.092(4) 0.058(4) -0.006(3) 0.031(4) -0.038(4) C9 0.094(5) 0.065(3) 0.056(4) 0.014(2) 0.005(3) -0.028(3) C10 0.052(3) 0.044(2) 0.055(3) 0.0035(15) -0.004(2) -0.0047(15) C11 0.061(4) 0.046(3) 0.103(5) -0.004(2) -0.001(3) 0.000(2) C12 0.101(8) 0.051(4) 0.227(14) -0.031(5) -0.013(8) 0.007(3) C13 0.047(3) 0.0351(17) 0.036(2) -0.0042(12) 0.0051(17) -0.0036(13) C14 0.063(3) 0.051(2) 0.039(3) -0.0036(15) 0.002(2) 0.0024(17) C15 0.101(6) 0.070(3) 0.040(3) -0.0140(19) 0.000(3) -0.007(3) C16 0.107(6) 0.058(3) 0.053(3) -0.023(2) 0.011(4) 0.006(3) C17 0.095(5) 0.054(3) 0.063(4) -0.009(2) 0.015(3) 0.023(2) C18 0.067(4) 0.048(2) 0.041(3) -0.0005(15) 0.004(2) 0.0103(17) C19 0.039(2) 0.042(2) 0.050(3) -0.0057(15) -0.0093(19) 0.0072(14) C20 0.056(3) 0.040(2) 0.056(3) -0.0007(15) 0.003(2) 0.0041(15) C21 0.068(4) 0.048(3) 0.074(4) 0.012(2) -0.006(3) -0.0044(19) C22 0.088(5) 0.039(2) 0.079(4) -0.0013(19) -0.028(4) 0.008(2) C23 0.087(5) 0.049(3) 0.085(5) -0.023(2) -0.027(4) 0.030(3) C24 0.058(4) 0.056(3) 0.060(3) -0.0134(19) -0.007(3) 0.020(2) C25 0.074(5) 0.084(4) 0.048(3) -0.015(2) -0.006(3) -0.008(3) C26 0.048(3) 0.093(4) 0.063(4) -0.039(3) 0.009(3) -0.010(3) C27 0.061(4) 0.064(3) 0.055(4) -0.015(2) 0.005(3) -0.005(2) O1 0.050(2) 0.0400(15) 0.053(2) -0.0007(10) 0.0059(15) -0.0030(11) O2 0.082(3) 0.073(2) 0.045(2) -0.0106(14) 0.021(2) -0.0284(18) O3 0.072(4) 0.047(2) 0.165(6) -0.010(2) 0.000(3) -0.0085(17) O4 0.137(7) 0.149(5) 0.044(3) -0.022(3) -0.024(4) -0.005(4) O5 0.044(4) 0.178(6) 0.132(6) -0.080(5) 0.021(4) -0.014(3) O6 0.142(6) 0.053(3) 0.105(5) -0.008(2) 0.025(4) 0.005(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 Mn C26 1.780(6) . ? Mn C27 1.793(5) . ? Mn C25 1.798(6) . ? Mn C1 2.130(4) . ? Mn C3 2.145(5) . ? Mn C2 2.147(4) . ? Mn C4 2.153(6) . ? Mn C5 2.169(5) . ? P C2 1.821(4) . ? P C13 1.833(4) . ? P C19 1.845(4) . ? C1 C5 1.406(7) . ? C1 C2 1.451(6) . ? C1 C7 1.517(6) . ? C2 C3 1.426(6) . ? C3 C4 1.409(8) . ? C4 C5 1.424(7) . ? C5 C6 1.517(8) . ? C7 O2 1.394(6) . ? C7 O1 1.418(5) . ? C8 O2 1.453(6) . ? C8 C9 1.517(11) . ? C9 C10 1.504(8) . ? C10 O1 1.446(5) . ? C10 C11 1.529(7) . ? C11 O3 1.397(7) . ? C12 O3 1.413(9) . ? C13 C14 1.377(7) . ? C13 C18 1.401(6) . ? C14 C15 1.398(7) . ? C15 C16 1.388(11) . ? C16 C17 1.372(10) . ? C17 C18 1.391(6) . ? C19 C20 1.372(7) . ? C19 C24 1.407(6) . ? C20 C21 1.399(6) . ? C21 C22 1.361(9) . ? C22 C23 1.350(11) . ? C23 C24 1.392(9) . ? C25 O4 1.125(8) . ? C26 O5 1.130(8) . ? C27 O6 1.143(7) . ? 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 C26 Mn C27 90.6(3) . . ? C26 Mn C25 91.7(3) . . ? C27 Mn C25 89.5(3) . . ? C26 Mn C1 92.9(2) . . ? C27 Mn C1 152.4(2) . . ? C25 Mn C1 117.7(2) . . ? C26 Mn C3 131.7(2) . . ? C27 Mn C3 92.6(2) . . ? C25 Mn C3 136.5(3) . . ? C1 Mn C3 65.03(16) . . ? C26 Mn C2 96.7(2) . . ? C27 Mn C2 112.8(2) . . ? C25 Mn C2 156.0(2) . . ? C1 Mn C2 39.66(15) . . ? C3 Mn C2 38.80(15) . . ? C26 Mn C4 157.0(2) . . ? C27 Mn C4 108.6(2) . . ? C25 Mn C4 100.6(3) . . ? C1 Mn C4 64.26(18) . . ? C3 Mn C4 38.3(2) . . ? C2 Mn C4 64.76(19) . . ? C26 Mn C5 122.9(3) . . ? C27 Mn C5 146.4(3) . . ? C25 Mn C5 91.3(3) . . ? C1 Mn C5 38.18(19) . . ? C3 Mn C5 64.6(2) . . ? C2 Mn C5 65.29(18) . . ? C4 Mn C5 38.47(19) . . ? C2 P C13 101.0(2) . . ? C2 P C19 99.66(19) . . ? C13 P C19 103.24(19) . . ? C5 C1 C2 109.1(4) . . ? C5 C1 C7 126.6(4) . . ? C2 C1 C7 124.0(4) . . ? C5 C1 Mn 72.4(3) . . ? C2 C1 Mn 70.8(2) . . ? C7 C1 Mn 127.2(3) . . ? C3 C2 C1 106.1(4) . . ? C3 C2 P 128.1(3) . . ? C1 C2 P 125.9(3) . . ? C3 C2 Mn 70.5(3) . . ? C1 C2 Mn 69.6(2) . . ? P C2 Mn 124.1(2) . . ? C4 C3 C2 108.6(4) . . ? C4 C3 Mn 71.2(3) . . ? C2 C3 Mn 70.7(3) . . ? C3 C4 C5 109.0(5) . . ? C3 C4 Mn 70.6(3) . . ? C5 C4 Mn 71.4(3) . . ? C1 C5 C4 107.2(5) . . ? C1 C5 C6 127.6(5) . . ? C4 C5 C6 125.0(6) . . ? C1 C5 Mn 69.4(3) . . ? C4 C5 Mn 70.2(3) . . ? C6 C5 Mn 129.8(5) . . ? O2 C7 O1 111.5(4) . . ? O2 C7 C1 110.1(3) . . ? O1 C7 C1 105.0(4) . . ? O2 C8 C9 109.9(6) . . ? C10 C9 C8 108.3(5) . . ? O1 C10 C9 108.9(4) . . ? O1 C10 C11 103.3(4) . . ? C9 C10 C11 114.3(5) . . ? O3 C11 C10 107.9(6) . . ? C14 C13 C18 119.2(4) . . ? C14 C13 P 118.6(3) . . ? C18 C13 P 121.8(4) . . ? C13 C14 C15 120.9(5) . . ? C16 C15 C14 119.5(6) . . ? C17 C16 C15 119.8(5) . . ? C16 C17 C18 121.0(5) . . ? C17 C18 C13 119.6(5) . . ? C20 C19 C24 118.9(4) . . ? C20 C19 P 124.4(3) . . ? C24 C19 P 116.8(4) . . ? C19 C20 C21 120.4(5) . . ? C22 C21 C20 120.4(6) . . ? C23 C22 C21 119.6(5) . . ? C22 C23 C24 122.0(5) . . ? C23 C24 C19 118.6(6) . . ? O4 C25 Mn 179.4(8) . . ? O5 C26 Mn 178.8(8) . . ? O6 C27 Mn 178.6(6) . . ? C7 O1 C10 111.0(4) . . ? C7 O2 C8 109.2(4) . . ? C11 O3 C12 110.9(7) . . ? _diffrn_measured_fraction_theta_max 0.664 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.664 _refine_diff_density_max 0.181 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.049 data_no _database_code_CSD 157496 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3.25 H3 Mn0.13 O0.75 P0.13' _chemical_formula_weight 64.80 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.6659(2) _cell_length_b 17.7774(8) _cell_length_c 18.6479(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2541.33(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 268 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4238 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4238 _reflns_number_gt 3965 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0687P)^2^+1.7932P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 4238 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.22194(8) 0.50641(3) 0.85028(4) 0.04738(18) Uani 1 1 d . . . P1 P 0.63190(13) 0.50919(6) 0.93158(5) 0.0448(2) Uani 1 1 d . . . O1 O 0.4465(5) 0.6190(2) 0.71746(18) 0.0611(8) Uani 1 1 d . . . O2 O 0.6314(4) 0.67312(15) 0.80214(17) 0.0518(7) Uani 1 1 d . . . O3 O 1.0215(8) 0.7601(3) 0.7389(4) 0.122(2) Uani 1 1 d . . . O4 O 0.0615(8) 0.3846(2) 0.9348(3) 0.1065(17) Uani 1 1 d . . . O5 O 0.4487(7) 0.4054(2) 0.7672(3) 0.0956(15) Uani 1 1 d . . . O6 O -0.0602(7) 0.5015(3) 0.7435(3) 0.1065(17) Uani 1 1 d . . . C1 C 0.4036(5) 0.5967(2) 0.8403(2) 0.0441(8) Uani 1 1 d . . . C2 C 0.4308(6) 0.5582(2) 0.9077(2) 0.0444(9) Uani 1 1 d . . . C3 C 0.2713(6) 0.5663(2) 0.9476(2) 0.0525(10) Uani 1 1 d . . . H3 H 0.2509 0.5474 0.9934 0.063 Uiso 1 1 calc R . . C4 C 0.1506(7) 0.6075(2) 0.9060(3) 0.0596(12) Uani 1 1 d . . . H4 H 0.0375 0.6201 0.9194 0.072 Uiso 1 1 calc R . . C5 C 0.2325(6) 0.6263(2) 0.8400(3) 0.0512(10) Uani 1 1 d . . . H5 H 0.1819 0.6535 0.8028 0.061 Uiso 1 1 calc R . . C6 C 0.5341(6) 0.6089(2) 0.7823(2) 0.0467(9) Uani 1 1 d . . . H6 H 0.6115 0.5652 0.7789 0.056 Uiso 1 1 calc R . . C7 C 0.5680(8) 0.6346(3) 0.6602(3) 0.0737(14) Uani 1 1 d . . . H7A H 0.5046 0.6434 0.6160 0.088 Uiso 1 1 calc R . . H7B H 0.6438 0.5916 0.6531 0.088 Uiso 1 1 calc R . . C8 C 0.6768(8) 0.7032(3) 0.6783(3) 0.0710(14) Uani 1 1 d . . . H8A H 0.7648 0.7110 0.6416 0.085 Uiso 1 1 calc R . . H8B H 0.6032 0.7475 0.6803 0.085 Uiso 1 1 calc R . . C9 C 0.7626(6) 0.6904(2) 0.7497(3) 0.0560(11) Uani 1 1 d . . . H9 H 0.8385 0.6463 0.7452 0.067 Uiso 1 1 calc R . . C10 C 0.8746(9) 0.7562(3) 0.7846(5) 0.100(3) Uani 1 1 d . . . H10A H 0.8106 0.8033 0.7846 0.120 Uiso 1 1 calc R . . H10B H 0.9085 0.7439 0.8333 0.120 Uiso 1 1 calc R . . C11 C 1.1385(12) 0.8172(5) 0.7575(7) 0.140(4) Uani 1 1 d . . . H11A H 1.2358 0.8165 0.7251 0.168 Uiso 1 1 calc R . . H11B H 1.1793 0.8092 0.8056 0.168 Uiso 1 1 calc R . . H11C H 1.0808 0.8650 0.7546 0.168 Uiso 1 1 calc R . . C12 C 0.7314(6) 0.5758(2) 0.9947(2) 0.0497(9) Uani 1 1 d . . . C13 C 0.7100(8) 0.6528(3) 0.9878(3) 0.0673(13) Uani 1 1 d . . . H13 H 0.6322 0.6722 0.9543 0.081 Uiso 1 1 calc R . . C14 C 0.8072(10) 0.7013(3) 1.0319(4) 0.0863(19) Uani 1 1 d . . . H14 H 0.7944 0.7530 1.0266 0.104 Uiso 1 1 calc R . . C15 C 0.9167(10) 0.6751(4) 1.0811(4) 0.091(2) Uani 1 1 d . . . H15 H 0.9745 0.7083 1.1115 0.109 Uiso 1 1 calc R . . C16 C 0.9448(9) 0.5987(4) 1.0873(3) 0.0820(18) Uani 1 1 d . . . H16 H 1.0261 0.5803 1.1198 0.098 Uiso 1 1 calc R . . C17 C 0.8506(8) 0.5498(3) 1.0444(3) 0.0662(13) Uani 1 1 d . . . H17 H 0.8680 0.4983 1.0492 0.079 Uiso 1 1 calc R . . C18 C 0.5482(6) 0.4350(2) 0.9905(3) 0.0514(10) Uani 1 1 d . . . C19 C 0.4794(7) 0.4478(3) 1.0584(3) 0.0597(11) Uani 1 1 d . . . H19 H 0.4804 0.4962 1.0774 0.072 Uiso 1 1 calc R . . C20 C 0.4090(9) 0.3888(4) 1.0981(3) 0.0766(16) Uani 1 1 d . . . H20 H 0.3633 0.3976 1.1436 0.092 Uiso 1 1 calc R . . C21 C 0.4076(10) 0.3163(3) 1.0690(4) 0.088(2) Uani 1 1 d . . . H21 H 0.3574 0.2770 1.0947 0.105 Uiso 1 1 calc R . . C22 C 0.4788(11) 0.3028(3) 1.0038(4) 0.087(2) Uani 1 1 d . . . H22 H 0.4796 0.2542 0.9854 0.104 Uiso 1 1 calc R . . C23 C 0.5518(8) 0.3621(3) 0.9635(3) 0.0676(14) Uani 1 1 d . . . H23 H 0.6021 0.3525 0.9191 0.081 Uiso 1 1 calc R . . C24 C 0.1245(8) 0.4312(3) 0.9003(3) 0.0659(13) Uani 1 1 d . . . C25 C 0.3569(7) 0.4444(2) 0.7990(3) 0.0620(12) Uani 1 1 d . . . C26 C 0.0510(7) 0.5027(3) 0.7854(3) 0.0680(13) 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 Mn1 0.0428(3) 0.0449(3) 0.0544(3) 0.0057(3) 0.0004(3) -0.0041(2) P1 0.0438(5) 0.0512(5) 0.0393(4) -0.0003(4) 0.0038(4) 0.0019(4) O1 0.0522(19) 0.084(2) 0.0472(18) 0.0056(14) -0.0034(15) -0.0068(15) O2 0.0547(18) 0.0492(15) 0.0515(16) -0.0004(12) 0.0098(14) -0.0057(12) O3 0.105(4) 0.129(4) 0.133(5) 0.008(3) -0.012(4) -0.049(3) O4 0.118(4) 0.081(3) 0.121(4) 0.039(3) 0.012(4) -0.031(3) O5 0.111(4) 0.082(3) 0.093(3) -0.028(2) 0.029(3) 0.000(3) O6 0.108(4) 0.088(3) 0.123(4) 0.018(3) -0.061(3) -0.006(3) C1 0.042(2) 0.0411(18) 0.049(2) 0.0043(15) 0.0032(18) -0.0011(14) C2 0.044(2) 0.0443(19) 0.045(2) -0.0010(15) 0.0080(17) -0.0007(15) C3 0.051(2) 0.056(2) 0.051(2) 0.0023(17) 0.009(2) 0.0001(18) C4 0.047(3) 0.055(2) 0.077(3) -0.004(2) 0.012(2) 0.0049(18) C5 0.043(2) 0.050(2) 0.060(3) 0.0084(17) 0.005(2) 0.0056(15) C6 0.046(2) 0.0443(19) 0.050(2) 0.0037(16) 0.0057(18) 0.0001(15) C7 0.073(4) 0.106(4) 0.042(3) 0.011(2) 0.002(2) -0.008(3) C8 0.073(3) 0.075(3) 0.065(3) 0.023(2) 0.013(3) -0.006(2) C9 0.057(3) 0.0455(19) 0.065(3) 0.0078(18) 0.012(2) -0.0052(17) C10 0.076(4) 0.052(3) 0.171(8) 0.002(3) 0.042(5) -0.017(3) C11 0.097(6) 0.101(5) 0.222(12) 0.037(6) -0.008(7) -0.040(5) C12 0.040(2) 0.065(2) 0.044(2) -0.0027(17) 0.0058(18) -0.0083(17) C13 0.069(3) 0.063(3) 0.071(3) -0.013(2) -0.005(3) 0.002(2) C14 0.096(5) 0.068(3) 0.094(5) -0.030(3) 0.007(4) -0.006(3) C15 0.086(5) 0.118(5) 0.068(4) -0.032(3) 0.000(4) -0.034(4) C16 0.071(4) 0.129(5) 0.046(3) 0.003(3) -0.005(3) -0.027(3) C17 0.065(3) 0.082(3) 0.052(3) 0.012(2) -0.005(2) -0.015(2) C18 0.048(2) 0.054(2) 0.052(2) 0.0090(18) -0.0050(19) -0.0039(17) C19 0.064(3) 0.063(3) 0.052(3) 0.007(2) 0.001(2) -0.011(2) C20 0.072(4) 0.101(4) 0.057(3) 0.022(3) 0.001(3) -0.019(3) C21 0.102(5) 0.067(3) 0.093(5) 0.029(3) -0.026(4) -0.028(3) C22 0.113(5) 0.051(3) 0.097(5) 0.009(3) -0.024(4) -0.012(3) C23 0.082(4) 0.056(3) 0.065(3) 0.007(2) -0.009(3) 0.009(2) C24 0.064(3) 0.058(3) 0.075(3) 0.011(2) 0.003(3) -0.011(2) C25 0.065(3) 0.051(2) 0.070(3) -0.008(2) 0.002(3) -0.004(2) C26 0.070(3) 0.052(2) 0.082(3) 0.010(2) -0.023(3) -0.005(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 Mn1 C26 1.785(5) . ? Mn1 C25 1.789(5) . ? Mn1 C24 1.794(5) . ? Mn1 C1 2.134(4) . ? Mn1 C2 2.135(5) . ? Mn1 C3 2.138(5) . ? Mn1 C5 2.141(4) . ? Mn1 C4 2.147(5) . ? P1 C2 1.826(4) . ? P1 C18 1.833(4) . ? P1 C12 1.836(4) . ? O1 C6 1.395(5) . ? O1 C7 1.444(6) . ? O2 C6 1.412(5) . ? O2 C9 1.435(5) . ? O3 C11 1.398(9) . ? O3 C10 1.413(9) . ? O4 C24 1.154(7) . ? O5 C25 1.152(7) . ? O6 C26 1.156(6) . ? C1 C5 1.413(6) . ? C1 C2 1.447(6) . ? C1 C6 1.490(6) . ? C2 C3 1.438(6) . ? C3 C4 1.412(7) . ? C4 C5 1.421(7) . ? C7 C8 1.514(8) . ? C8 C9 1.503(7) . ? C9 C10 1.589(8) . ? C12 C17 1.381(7) . ? C12 C13 1.385(7) . ? C13 C14 1.406(8) . ? C14 C15 1.328(10) . ? C15 C16 1.380(10) . ? C16 C17 1.384(8) . ? C18 C23 1.390(7) . ? C18 C19 1.391(7) . ? C19 C20 1.393(7) . ? C20 C21 1.398(9) . ? C21 C22 1.355(10) . ? C22 C23 1.410(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C26 Mn1 C25 92.3(3) . . ? C26 Mn1 C24 91.1(3) . . ? C25 Mn1 C24 93.4(3) . . ? C26 Mn1 C1 116.6(2) . . ? C25 Mn1 C1 92.31(19) . . ? C24 Mn1 C1 151.4(2) . . ? C26 Mn1 C2 155.04(19) . . ? C25 Mn1 C2 95.8(2) . . ? C24 Mn1 C2 111.9(2) . . ? C1 Mn1 C2 39.61(15) . . ? C26 Mn1 C3 136.4(2) . . ? C25 Mn1 C3 131.2(2) . . ? C24 Mn1 C3 90.2(2) . . ? C1 Mn1 C3 65.38(16) . . ? C2 Mn1 C3 39.34(16) . . ? C26 Mn1 C5 90.2(2) . . ? C25 Mn1 C5 123.0(2) . . ? C24 Mn1 C5 143.5(2) . . ? C1 Mn1 C5 38.60(15) . . ? C2 Mn1 C5 65.63(16) . . ? C3 Mn1 C5 64.76(17) . . ? C26 Mn1 C4 99.9(2) . . ? C25 Mn1 C4 157.2(2) . . ? C24 Mn1 C4 105.4(2) . . ? C1 Mn1 C4 65.06(18) . . ? C2 Mn1 C4 65.62(18) . . ? C3 Mn1 C4 38.50(19) . . ? C5 Mn1 C4 38.71(18) . . ? C2 P1 C18 101.2(2) . . ? C2 P1 C12 101.5(2) . . ? C18 P1 C12 103.0(2) . . ? C6 O1 C7 110.8(4) . . ? C6 O2 C9 111.4(3) . . ? C11 O3 C10 113.4(7) . . ? C5 C1 C2 108.3(4) . . ? C5 C1 C6 124.5(4) . . ? C2 C1 C6 127.1(4) . . ? C5 C1 Mn1 71.0(2) . . ? C2 C1 Mn1 70.3(2) . . ? C6 C1 Mn1 127.7(3) . . ? C3 C2 C1 106.2(4) . . ? C3 C2 P1 129.8(3) . . ? C1 C2 P1 124.0(3) . . ? C3 C2 Mn1 70.4(3) . . ? C1 C2 Mn1 70.1(2) . . ? P1 C2 Mn1 123.3(2) . . ? C4 C3 C2 109.0(4) . . ? C4 C3 Mn1 71.1(3) . . ? C2 C3 Mn1 70.2(2) . . ? C3 C4 C5 107.9(4) . . ? C3 C4 Mn1 70.4(2) . . ? C5 C4 Mn1 70.4(2) . . ? C1 C5 C4 108.6(4) . . ? C1 C5 Mn1 70.4(2) . . ? C4 C5 Mn1 70.9(2) . . ? O1 C6 O2 112.2(3) . . ? O1 C6 C1 109.0(3) . . ? O2 C6 C1 106.4(3) . . ? O1 C7 C8 110.2(4) . . ? C9 C8 C7 108.5(4) . . ? O2 C9 C8 109.2(4) . . ? O2 C9 C10 105.0(4) . . ? C8 C9 C10 119.2(5) . . ? O3 C10 C9 102.7(6) . . ? C17 C12 C13 118.2(5) . . ? C17 C12 P1 119.3(4) . . ? C13 C12 P1 121.9(4) . . ? C12 C13 C14 119.3(6) . . ? C15 C14 C13 121.6(6) . . ? C14 C15 C16 120.1(5) . . ? C15 C16 C17 119.3(6) . . ? C12 C17 C16 121.5(6) . . ? C23 C18 C19 119.3(4) . . ? C23 C18 P1 116.6(4) . . ? C19 C18 P1 124.1(3) . . ? C18 C19 C20 120.5(5) . . ? C19 C20 C21 119.4(6) . . ? C22 C21 C20 120.6(5) . . ? C21 C22 C23 120.4(6) . . ? C18 C23 C22 119.7(6) . . ? O4 C24 Mn1 177.4(6) . . ? O5 C25 Mn1 177.7(5) . . ? O6 C26 Mn1 178.9(5) . . ? _diffrn_measured_fraction_theta_max 0.829 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.829 _refine_diff_density_max 0.455 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.106