This journal is © The Owner Societies 2000 # CCDC Number: 1326/7 data_global _publ_requested_journal 'PCCP' _publ_contact_author ; R. H. Jones Department of Chemistry, Keele University, Keele Staffs ST5 5BG United Kingdom ; _publ_contact_author_email 'cha35@chem.keele.ac.uk' _publ_section_title ; Evidence for ordering of cobalt ions in the microporous solid acid catalyst DAF-4 by single crystal x-ray diffraction and resonant x-ray powder diffraction. ; _publ_section_references ? data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common Co-DAF4 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum ; 'C11.56 H26.43 Al7.35 Co1.65 N1.65 O37.05 P9' ; _chemical_formula_weight 1355.67 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 13.192(3) _cell_length_b 13.192(3) _cell_length_c 46.149(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6954.8(26) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method ? _exptl_crystal_F_000 4073 _exptl_absorpt_coefficient_mu 1.154 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FAST area detector' _diffrn_measurement_method MADNESS _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 9424 _diffrn_reflns_av_R_equivalents 0.1075 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.06 _reflns_number_total 1318 _reflns_number_observed 606 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction MADNESS _computing_structure_solution 'Inspection' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Inspection _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens omitted _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1312 _refine_ls_number_parameters 116 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_obs 0.0591 _refine_ls_wR_factor_all 0.1774 _refine_ls_wR_factor_obs 0.1453 _refine_ls_goodness_of_fit_all 0.880 _refine_ls_goodness_of_fit_obs 1.226 _refine_ls_restrained_S_all 0.966 _refine_ls_restrained_S_obs 1.211 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1 Al -0.00455(11) 0.23417(13) 0.03378(3) 0.0263(7) Uani 0.799(6) d P . Co1 Co -0.00455(11) 0.23417(13) 0.03378(3) 0.0263(7) Uani 0.201(6) d P . Al2 Al 0.2421(2) 0.0000 0.2500 0.0228(9) Uani 0.852(8) d SP . Co2 Co 0.2421(2) 0.0000 0.2500 0.0228(9) Uani 0.148(7) d SP . P1 P 0.24286(15) 0.00553(12) -0.03371(4) 0.0294(6) Uani 1 d . . P2 P 0.0000 0.2403(2) 0.7500 0.0246(7) Uani 1 d S . O1 O -0.0347(4) 0.3219(4) 0.05640(11) 0.059(2) Uani 1 d . . O2 O 0.3198(4) -0.0221(4) -0.05265(9) 0.0526(15) Uani 1 d . . O3 O 0.1351(4) -0.1232(4) 0.54207(8) 0.0490(12) Uani 1 d . . O4 O 0.1153(4) -0.0856(4) -0.03751(10) 0.0526(14) Uani 1 d . . O5 O 0.2832(4) 0.0077(4) -0.00276(11) 0.0479(13) Uani 1 d . . O6 O -0.2116(4) 0.2268(4) 0.08720(9) 0.0543(13) Uani 1 d . . C1 C 0.6106(29) 0.2070(6) 0.9801(8) 0.220(10) Uiso 0.41 d PD . C2 C 0.7366(27) 0.2775(29) 0.9920(8) 0.220(10) Uiso 0.41 d PD . C3 C 0.5554(58) 0.0829(8) 0.9903(11) 0.220(10) Uiso 0.14 d PD . C4 C 0.5521(52) 0.2699(39) 1.0246(8) 0.220(10) Uiso 0.14 d P . C11 C 0.2067(6) 0.6093(33) 1.0534(8) 0.220(10) Uiso 0.41 d PD . C12 C 0.2766(33) 0.7359(31) 1.0413(8) 0.220(10) Uiso 0.41 d PD . C13 C 0.0552(42) 0.1218(53) 0.9190(8) 0.220(10) Uiso 0.14 d P . C14 C 0.2842(38) 0.7269(40) 1.0087(8) 0.220(10) Uiso 0.14 d PD . O100 O 0.6667 0.3333 1.0203(11) 0.134(17) Uiso 0.26 d SP . O200 O 0.0000 0.0000 0.9045(10) 0.105(13) Uiso 0.26 d SP . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0241(10) 0.0327(11) 0.0233(11) -0.0027(7) 0.0020(7) 0.0150(8) Co1 0.0241(10) 0.0327(11) 0.0233(11) -0.0027(7) 0.0020(7) 0.0150(8) Al2 0.0210(11) 0.0218(14) 0.026(2) -0.0042(9) -0.0021(5) 0.0109(7) Co2 0.0210(11) 0.0218(14) 0.026(2) -0.0042(9) -0.0021(5) 0.0109(7) P1 0.0372(11) 0.0224(10) 0.0272(12) -0.0010(7) 0.0066(8) 0.0140(8) P2 0.0220(13) 0.0224(10) 0.029(2) 0.0030(5) 0.0061(10) 0.0110(7) O1 0.054(3) 0.058(3) 0.058(4) -0.014(3) 0.015(3) 0.021(3) O2 0.047(3) 0.053(3) 0.054(4) -0.014(2) 0.012(2) 0.022(3) O3 0.059(3) 0.030(3) 0.037(2) 0.006(2) -0.003(3) 0.007(2) O4 0.039(3) 0.036(3) 0.075(3) -0.002(2) 0.006(3) 0.013(2) O5 0.063(3) 0.049(3) 0.033(3) 0.000(2) 0.001(3) 0.029(3) O6 0.039(3) 0.034(3) 0.070(3) -0.008(3) 0.013(3) 0.003(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 Al1 O1 1.745(5) . ? Al1 O3 1.748(5) 24 ? Al1 O4 1.772(5) 19 ? Al1 O5 1.779(5) 2 ? Co1 O1 1.745(5) . ? Co1 O3 1.748(5) 24 ? Co1 O4 1.772(5) 19 ? Co1 O5 1.779(5) 2 ? Al2 O6 1.714(5) 34_545 ? Al2 O6 1.714(5) 27 ? Al2 O2 1.742(4) 9 ? Al2 O2 1.742(4) 16_544 ? Co2 O6 1.714(5) 34_545 ? Co2 O6 1.714(5) 27 ? Co2 O2 1.742(4) 9 ? Co2 O2 1.742(4) 16_544 ? P1 O3 1.511(5) 5 ? P1 O4 1.511(5) . ? P1 O2 1.515(5) . ? P1 O5 1.519(5) . ? P2 O6 1.501(5) 10_455 ? P2 O6 1.501(5) 14 ? P2 O1 1.509(5) 14 ? P2 O1 1.509(5) 10_455 ? O1 P2 1.509(5) 9_454 ? O2 Co2 1.742(4) 14_544 ? O2 Al2 1.742(4) 14_544 ? O3 P1 1.511(5) 5 ? O3 Al1 1.748(5) 24_556 ? O3 Co1 1.748(5) 24_556 ? O4 Co1 1.772(5) 19 ? O4 Al1 1.772(5) 19 ? O5 Co1 1.779(5) 3 ? O5 Al1 1.779(5) 3 ? O6 P2 1.501(5) 9_454 ? O6 Al2 1.714(5) 26_455 ? O6 Co2 1.714(5) 26_455 ? C1 C14 1.32(5) 19_667 ? C1 C3 1.498(10) . ? C1 C2 1.545(7) 3_665 ? C1 C2 1.545(10) . ? C1 C11 1.55(4) 21_657 ? C1 C14 1.59(5) 21_657 ? C1 C12 1.62(5) 19_667 ? C1 C12 1.87(4) 21_657 ? C2 C14 0.25(5) 19_667 ? C2 C4 1.510(10) 2_655 ? C2 C1 1.545(7) 2_655 ? C2 C12 1.55(4) 19_667 ? C4 O100 1.33(6) . ? C4 C2 1.510(10) 3_665 ? C4 C14 1.54(4) 21_657 ? C11 C13 1.490(10) 34 ? C11 C12 1.545(7) 2_665 ? C11 C12 1.554(10) . ? C11 C1 1.55(4) 20_567 ? C11 O200 1.66(3) 34 ? C12 C14 1.518(10) . ? C12 C11 1.545(7) 3_565 ? C12 C2 1.55(4) 19_667 ? C12 C1 1.62(5) 19_667 ? C12 C1 1.87(5) 20_567 ? C13 C11 1.489(10) 28 ? C13 O200 1.55(5) . ? C14 C2 0.25(5) 19_667 ? C14 C1 1.32(5) 19_667 ? C14 C4 1.54(4) 20_567 ? C14 C1 1.59(5) 20_567 ? C14 O100 1.83(6) 19_667 ? O100 C4 1.33(6) 2_655 ? O100 C4 1.33(6) 3_665 ? O100 C14 1.83(6) 19_667 ? O100 C14 1.83(6) 20_557 ? O100 C14 1.83(6) 21_657 ? O200 C13 1.55(5) 3 ? O200 C13 1.55(6) 2 ? O200 C11 1.66(3) 29_445 ? O200 C11 1.66(3) 30_455 ? O200 C11 1.66(3) 28 ? 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 Al1 O3 108.5(2) . 24 ? O1 Al1 O4 109.9(2) . 19 ? O3 Al1 O4 113.0(2) 24 19 ? O1 Al1 O5 108.4(2) . 2 ? O3 Al1 O5 109.6(2) 24 2 ? O4 Al1 O5 107.4(2) 19 2 ? O1 Co1 O3 108.5(2) . 24 ? O1 Co1 O4 109.9(2) . 19 ? O3 Co1 O4 113.0(2) 24 19 ? O1 Co1 O5 108.4(2) . 2 ? O3 Co1 O5 109.6(2) 24 2 ? O4 Co1 O5 107.4(2) 19 2 ? O6 Al2 O6 109.8(3) 34_545 27 ? O6 Al2 O2 108.6(2) 34_545 9 ? O6 Al2 O2 110.1(2) 27 9 ? O6 Al2 O2 110.1(2) 34_545 16_544 ? O6 Al2 O2 108.6(2) 27 16_544 ? O2 Al2 O2 109.8(3) 9 16_544 ? O6 Co2 O6 109.8(3) 34_545 27 ? O6 Co2 O2 108.6(2) 34_545 9 ? O6 Co2 O2 110.1(2) 27 9 ? O6 Co2 O2 110.1(2) 34_545 16_544 ? O6 Co2 O2 108.6(2) 27 16_544 ? O2 Co2 O2 109.8(3) 9 16_544 ? O3 P1 O4 108.2(3) 5 . ? O3 P1 O2 109.7(3) 5 . ? O4 P1 O2 110.8(3) . . ? O3 P1 O5 110.8(2) 5 . ? O4 P1 O5 111.3(3) . . ? O2 P1 O5 106.0(3) . . ? O6 P2 O6 110.0(4) 10_455 14 ? O6 P2 O1 107.1(3) 10_455 14 ? O6 P2 O1 110.4(2) 14 14 ? O6 P2 O1 110.4(2) 10_455 10_455 ? O6 P2 O1 107.1(3) 14 10_455 ? O1 P2 O1 111.8(4) 14 10_455 ? P2 O1 Al1 148.8(3) 9_454 . ? P2 O1 Co1 148.8(3) 9_454 . ? Al1 O1 Co1 0.00(15) . . ? P1 O2 Co2 148.4(3) . 14_544 ? P1 O2 Al2 148.4(3) . 14_544 ? Co2 O2 Al2 0.00(11) 14_544 14_544 ? P1 O3 Al1 148.2(3) 5 24_556 ? P1 O3 Co1 148.2(3) 5 24_556 ? Al1 O3 Co1 0.0(2) 24_556 24_556 ? P1 O4 Co1 147.4(3) . 19 ? P1 O4 Al1 147.4(3) . 19 ? Co1 O4 Al1 0.0(2) 19 19 ? P1 O5 Co1 141.5(3) . 3 ? P1 O5 Al1 141.5(3) . 3 ? Co1 O5 Al1 0.0(2) 3 3 ? P2 O6 Al2 163.4(3) 9_454 26_455 ? P2 O6 Co2 163.4(3) 9_454 26_455 ? Al2 O6 Co2 0.00(11) 26_455 26_455 ? C14 C1 C3 111.8(24) 19_667 . ? C14 C1 C2 102.9(26) 19_667 3_665 ? C3 C1 C2 109.4(9) . 3_665 ? C14 C1 C2 4.8(26) 19_667 . ? C3 C1 C2 109.4(10) . . ? C2 C1 C2 107.7(9) 3_665 . ? C14 C1 C11 118.2(30) 19_667 21_657 ? C3 C1 C11 108.6(16) . 21_657 ? C2 C1 C11 105.3(21) 3_665 21_657 ? C2 C1 C11 116.2(18) . 21_657 ? C14 C1 C14 95.9(47) 19_667 21_657 ? C3 C1 C14 117.9(21) . 21_657 ? C2 C1 C14 9.1(20) 3_665 21_657 ? C2 C1 C14 100.7(23) . 21_657 ? C11 C1 C14 104.1(26) 21_657 21_657 ? C14 C1 C12 61.1(22) 19_667 19_667 ? C3 C1 C12 122.0(14) . 19_667 ? C2 C1 C12 128.5(11) 3_665 19_667 ? C2 C1 C12 58.4(17) . 19_667 ? C11 C1 C12 58.2(15) 21_657 19_667 ? C14 C1 C12 120.0(16) 21_657 19_667 ? C14 C1 C12 119.7(21) 19_667 21_657 ? C3 C1 C12 127.8(14) . 21_657 ? C2 C1 C12 52.8(15) 3_665 21_657 ? C2 C1 C12 122.6(12) . 21_657 ? C11 C1 C12 52.9(14) 21_657 21_657 ? C14 C1 C12 51.2(14) 21_657 21_657 ? C12 C1 C12 90.9(16) 19_667 21_657 ? C14 C2 C4 93.1(100) 19_667 2_655 ? C14 C2 C1 94.8(100) 19_667 2_655 ? C4 C2 C1 108.5(9) 2_655 2_655 ? C14 C2 C1 25.8(100) 19_667 . ? C4 C2 C1 108.3(10) 2_655 . ? C1 C2 C1 108.3(9) 2_655 . ? C14 C2 C12 78.7(100) 19_667 19_667 ? C4 C2 C12 171.6(24) 2_655 19_667 ? C1 C2 C12 74.6(18) 2_655 19_667 ? C1 C2 C12 63.3(20) . 19_667 ? O100 C4 C2 86.2(28) . 3_665 ? O100 C4 C14 78.8(34) . 21_657 ? C2 C4 C14 9.4(21) 3_665 21_657 ? C13 C11 C12 110.2(9) 34 2_665 ? C13 C11 C12 110.0(11) 34 . ? C12 C11 C12 107.3(9) 2_665 . ? C13 C11 C1 173.2(22) 34 20_567 ? C12 C11 C1 63.1(20) 2_665 20_567 ? C12 C11 C1 74.1(18) . 20_567 ? C13 C11 O200 58.4(26) 34 34 ? C12 C11 O200 76.8(10) 2_665 34 ? C12 C11 O200 76.5(10) . 34 ? C1 C11 O200 118.8(17) 20_567 34 ? C14 C12 C11 107.5(9) . 3_565 ? C14 C12 C2 9.4(21) . 19_667 ? C11 C12 C2 116.6(19) 3_565 19_667 ? C14 C12 C11 107.4(10) . . ? C11 C12 C11 108.1(9) 3_565 . ? C2 C12 C11 105.2(20) 19_667 . ? C14 C12 C1 49.7(16) . 19_667 ? C11 C12 C1 58.7(16) 3_565 19_667 ? C2 C12 C1 58.3(16) 19_667 19_667 ? C11 C12 C1 129.1(10) . 19_667 ? C14 C12 C1 54.6(16) . 20_567 ? C11 C12 C1 123.4(11) 3_565 20_567 ? C2 C12 C1 52.7(14) 19_667 20_567 ? C11 C12 C1 52.9(13) . 20_567 ? C1 C12 C1 91.2(17) 19_667 20_567 ? C11 C13 O200 66.4(20) 28 . ? C2 C14 C1 149.4(100) 19_667 19_667 ? C2 C14 C12 91.9(100) 19_667 . ? C1 C14 C12 69.3(20) 19_667 . ? C2 C14 C4 77.5(95) 19_667 20_567 ? C1 C14 C4 119.4(36) 19_667 20_567 ? C12 C14 C4 169.2(42) . 20_567 ? C2 C14 C1 76.1(100) 19_667 20_567 ? C1 C14 C1 118.6(31) 19_667 20_567 ? C12 C14 C1 74.2(16) . 20_567 ? C4 C14 C1 104.8(30) 20_567 20_567 ? C2 C14 O100 113.1(100) 19_667 19_667 ? C1 C14 O100 95.2(33) 19_667 19_667 ? C12 C14 O100 144.1(36) . 19_667 ? C4 C14 O100 45.3(27) 20_567 19_667 ? C1 C14 O100 86.8(28) 20_567 19_667 ? C4 O100 C4 117.8(13) 2_655 . ? C4 O100 C4 117.8(13) 2_655 3_665 ? C4 O100 C4 117.8(13) . 3_665 ? C4 O100 C14 55.9(22) 2_655 19_667 ? C4 O100 C14 112.0(28) . 19_667 ? C4 O100 C14 121.0(29) 3_665 19_667 ? C4 O100 C14 112.0(27) 2_655 20_557 ? C4 O100 C14 121.0(29) . 20_557 ? C4 O100 C14 55.9(23) 3_665 20_557 ? C14 O100 C14 72.6(27) 19_667 20_557 ? C4 O100 C14 121.0(29) 2_655 21_657 ? C4 O100 C14 55.9(23) . 21_657 ? C4 O100 C14 112.0(27) 3_665 21_657 ? C14 O100 C14 72.6(27) 19_667 21_657 ? C14 O100 C14 72.6(28) 20_557 21_657 ? C13 O200 C13 102.6(28) . 3 ? C13 O200 C13 102.6(29) . 2 ? C13 O200 C13 102.6(28) 3 2 ? C13 O200 C11 127.3(8) . 29_445 ? C13 O200 C11 55.1(12) 3 29_445 ? C13 O200 C11 127.3(8) 2 29_445 ? C13 O200 C11 127.3(7) . 30_455 ? C13 O200 C11 127.3(8) 3 30_455 ? C13 O200 C11 55.1(12) 2 30_455 ? C11 O200 C11 97.8(22) 29_445 30_455 ? C13 O200 C11 55.1(12) . 28 ? C13 O200 C11 127.3(8) 3 28 ? C13 O200 C11 127.3(8) 2 28 ? C11 O200 C11 97.8(22) 29_445 28 ? C11 O200 C11 97.8(22) 30_455 28 ? _refine_diff_density_max 1.088 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.170 #==END