Supplementary Material (ESI) for Organic & Biomolecular Chemistry This journal is (c) The Royal Society of Chemistry 2007 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_c:\backup\helix\h02ihw1\maxus\h02ihw1 _database_code_depnum_ccdc_archive 'CCDC 652216' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H9 Br O5' _chemical_formula_weight 241.04 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c 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 11.4120(5) _cell_length_b 5.8870(3) _cell_length_c 12.3790(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.337(2) _cell_angle_gamma 90.00 _cell_volume 830.24(7) _cell_formula_units_Z 4 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 7132 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Tabloid _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 4.932 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.67 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 30(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5751 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1883 _reflns_number_gt 1420 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0365P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _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_number_reflns 1883 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Br1 Br 0.07524(3) 0.19321(6) 0.32757(3) 0.01188(15) Uani 1 1 d . . . O1 O 0.50812(19) 0.0000(4) 0.3056(2) 0.0122(6) Uani 1 1 d . . . O2 O 0.4235(2) -0.2377(4) 0.4189(2) 0.0125(6) Uani 1 1 d . . . H2 H 0.4932 -0.2631 0.4414 0.015 Uiso 1 1 calc R . . O3 O 0.3597(2) 0.2429(4) 0.4781(2) 0.0113(6) Uani 1 1 d . . . O4 O 0.1978(2) 0.1601(4) 0.5651(2) 0.0132(6) Uani 1 1 d . . . H4 H 0.2358 0.2189 0.6182 0.016 Uiso 1 1 calc R . . O5 O 0.3087(2) 0.1968(4) 0.2433(2) 0.0121(6) Uani 1 1 d . . . H5 H 0.3777 0.2452 0.2539 0.015 Uiso 1 1 calc R . . C1 C 0.4221(3) -0.0800(6) 0.3421(3) 0.0109(8) Uani 1 1 d . . . C2 C 0.2975(3) -0.0162(6) 0.2974(3) 0.0105(8) Uani 1 1 d . . . C3 C 0.2095(3) 0.0110(6) 0.3876(3) 0.0117(8) Uani 1 1 d . . . C4 C 0.2632(3) 0.1546(6) 0.4821(3) 0.0104(8) Uani 1 1 d . . . C5 C 0.2561(3) -0.1893(6) 0.2091(3) 0.0080(7) Uani 1 1 d . . . H5A H 0.1777 -0.1471 0.1793 0.012 Uiso 1 1 calc R . . H5B H 0.2534 -0.3415 0.2409 0.012 Uiso 1 1 calc R . . H5C H 0.3111 -0.1889 0.1511 0.012 Uiso 1 1 calc R . . C6 C 0.1580(3) -0.2121(6) 0.4279(3) 0.0115(8) Uani 1 1 d . . . H6A H 0.2213 -0.3068 0.4603 0.017 Uiso 1 1 calc R . . H6B H 0.1186 -0.2930 0.3668 0.017 Uiso 1 1 calc R . . H6C H 0.1012 -0.1790 0.4821 0.017 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.01017(19) 0.0161(2) 0.0090(2) -0.00034(18) -0.00252(13) 0.00102(16) O1 0.0115(11) 0.0164(14) 0.0086(14) 0.0009(12) -0.0008(10) 0.0009(11) O2 0.0096(12) 0.0166(14) 0.0109(14) 0.0018(11) -0.0037(10) 0.0014(10) O3 0.0127(12) 0.0140(14) 0.0069(14) 0.0001(10) -0.0011(10) -0.0003(10) O4 0.0119(12) 0.0205(16) 0.0070(14) -0.0045(12) -0.0017(10) -0.0022(11) O5 0.0104(12) 0.0162(14) 0.0094(14) 0.0049(12) -0.0032(10) -0.0032(11) C1 0.0161(17) 0.011(2) 0.0055(19) -0.0066(16) -0.0030(15) 0.0018(16) C2 0.0119(16) 0.0104(19) 0.009(2) 0.0002(16) -0.0041(14) -0.0035(15) C3 0.0090(15) 0.020(2) 0.0057(19) -0.0021(17) -0.0051(14) 0.0037(15) C4 0.0127(17) 0.010(2) 0.008(2) 0.0010(15) -0.0029(14) 0.0047(15) C5 0.0086(15) 0.0058(17) 0.0103(19) -0.0049(16) 0.0071(14) -0.0042(15) C6 0.0123(17) 0.0128(19) 0.009(2) 0.0005(16) -0.0016(15) -0.0034(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C3 1.979(3) . ? O1 C1 1.200(4) . ? O2 C1 1.328(4) . ? O3 C4 1.221(4) . ? O4 C4 1.305(4) . ? O5 C2 1.430(4) . ? C1 C2 1.542(4) . ? C2 C5 1.548(5) . ? C2 C3 1.553(5) . ? C3 C6 1.534(5) . ? C3 C4 1.541(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 124.6(3) . . ? O1 C1 C2 121.8(3) . . ? O2 C1 C2 113.5(3) . . ? O5 C2 C1 106.0(3) . . ? O5 C2 C5 106.2(3) . . ? C1 C2 C5 109.3(3) . . ? O5 C2 C3 109.0(3) . . ? C1 C2 C3 112.9(3) . . ? C5 C2 C3 113.1(3) . . ? C6 C3 C4 111.5(3) . . ? C6 C3 C2 114.9(3) . . ? C4 C3 C2 110.9(3) . . ? C6 C3 Br1 106.5(2) . . ? C4 C3 Br1 104.7(2) . . ? C2 C3 Br1 107.7(2) . . ? O3 C4 O4 125.4(3) . . ? O3 C4 C3 121.5(3) . . ? O4 C4 C3 113.0(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.793 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.160 data_c:\backup\kappa\k03gb1\maxus\k03gb1 _database_code_depnum_ccdc_archive 'CCDC 652217' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Br O6' _chemical_formula_weight 258.05 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2390(3) _cell_length_b 7.2280(4) _cell_length_c 11.1710(8) _cell_angle_alpha 85.342(2) _cell_angle_beta 82.801(2) _cell_angle_gamma 69.105(3) _cell_volume 466.56(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19739 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 258 _exptl_absorpt_coefficient_mu 4.403 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.65 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8440 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 27.34 _reflns_number_total 2075 _reflns_number_gt 1623 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0485P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0096(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2075 _refine_ls_number_parameters 134 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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 Br1 Br 0.44652(5) 0.97112(5) 0.27585(3) 0.02928(17) Uani 1 1 d . . . O1 O 0.9809(4) 0.7929(3) 0.4758(2) 0.0311(6) Uani 1 1 d . . . O2 O 0.7943(4) 1.0789(3) 0.3827(2) 0.0332(6) Uani 1 1 d . . . H2 H 0.8742 1.1207 0.4211 0.040 Uiso 1 1 calc R . . O3 O 0.7460(4) 0.6787(4) 0.0370(2) 0.0337(6) Uani 1 1 d . . . O4 O 0.7803(5) 0.4376(4) 0.1803(2) 0.0345(6) Uani 1 1 d . . . H4 H 0.7524 0.3781 0.1261 0.046(13) Uiso 1 1 calc R . . O5 O 0.9638(4) 0.8566(3) 0.1555(2) 0.0247(5) Uani 1 1 d . . . H5 H 0.8447 0.9393 0.1291 0.044(12) Uiso 1 1 calc R . . O6 O 0.7000(4) 1.2083(3) 0.0366(2) 0.0276(5) Uani 1 1 d D . . C1 C 0.8477(6) 0.8887(5) 0.4042(3) 0.0261(7) Uani 1 1 d . . . C2 C 0.7363(5) 0.7808(5) 0.3328(3) 0.0252(7) Uani 1 1 d . . . C3 C 0.9080(5) 0.6980(5) 0.2192(3) 0.0250(7) Uani 1 1 d . . . C4 C 0.6699(6) 0.6283(5) 0.4164(3) 0.0271(7) Uani 1 1 d . . . H4A H 0.8089 0.5299 0.4459 0.041 Uiso 1 1 calc R . . H4B H 0.5936 0.5621 0.3721 0.041 Uiso 1 1 calc R . . H4C H 0.5644 0.6949 0.4850 0.041 Uiso 1 1 calc R . . C5 C 1.1364(5) 0.5445(5) 0.2504(3) 0.0278(8) Uani 1 1 d . . . H5A H 1.2307 0.4892 0.1760 0.042 Uiso 1 1 calc R . . H5B H 1.1071 0.4381 0.3021 0.042 Uiso 1 1 calc R . . H5C H 1.2183 0.6075 0.2932 0.042 Uiso 1 1 calc R . . C6 C 0.7994(5) 0.6061(5) 0.1346(3) 0.0267(8) Uani 1 1 d . . . H6A H 0.558(4) 1.245(7) 0.015(4) 0.060(14) Uiso 1 1 d D . . H6B H 0.802(7) 1.197(7) -0.028(3) 0.066(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0175(2) 0.0286(2) 0.0382(3) 0.00057(15) -0.00236(14) -0.00445(14) O1 0.0347(13) 0.0232(12) 0.0366(14) -0.0001(11) -0.0141(12) -0.0083(11) O2 0.0405(14) 0.0209(13) 0.0417(16) 0.0000(11) -0.0164(12) -0.0113(11) O3 0.0302(13) 0.0353(14) 0.0344(15) -0.0025(12) -0.0101(11) -0.0075(11) O4 0.0453(15) 0.0306(14) 0.0339(15) -0.0042(12) -0.0066(12) -0.0192(12) O5 0.0186(11) 0.0270(13) 0.0289(13) 0.0028(10) -0.0011(10) -0.0097(10) O6 0.0229(13) 0.0310(13) 0.0317(15) -0.0025(11) -0.0025(11) -0.0127(11) C1 0.0256(17) 0.0235(17) 0.0278(19) -0.0003(15) -0.0003(15) -0.0076(14) C2 0.0204(16) 0.0232(17) 0.0297(19) 0.0033(14) -0.0015(14) -0.0060(13) C3 0.0187(16) 0.0269(17) 0.0282(19) 0.0009(15) -0.0006(14) -0.0074(13) C4 0.0255(17) 0.0265(17) 0.031(2) 0.0010(15) 0.0001(15) -0.0131(14) C5 0.0200(16) 0.0275(18) 0.033(2) -0.0021(15) -0.0046(14) -0.0039(14) C6 0.0225(17) 0.0238(17) 0.032(2) -0.0029(15) -0.0022(15) -0.0058(14) _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 Br1 C2 1.984(3) . ? O1 C1 1.215(4) . ? O2 C1 1.303(4) . ? O3 C6 1.204(4) . ? O4 C6 1.321(4) . ? O5 C3 1.425(4) . ? C1 C2 1.535(5) . ? C2 C4 1.523(4) . ? C2 C3 1.562(5) . ? C3 C5 1.522(4) . ? C3 C6 1.542(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 124.1(3) . . ? O1 C1 C2 118.6(3) . . ? O2 C1 C2 117.3(3) . . ? C4 C2 C1 109.1(3) . . ? C4 C2 C3 116.0(3) . . ? C1 C2 C3 107.2(2) . . ? C4 C2 Br1 106.7(2) . . ? C1 C2 Br1 110.0(2) . . ? C3 C2 Br1 107.8(2) . . ? O5 C3 C5 105.9(3) . . ? O5 C3 C6 109.0(3) . . ? C5 C3 C6 108.9(3) . . ? O5 C3 C2 108.9(3) . . ? C5 C3 C2 113.2(3) . . ? C6 C3 C2 110.8(3) . . ? O3 C6 O4 124.9(3) . . ? O3 C6 C3 123.0(3) . . ? O4 C6 C3 112.1(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.34 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.675 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.120