# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 207/312


data_KE3SPH
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C24 H28 O4 S' 
_chemical_formula_weight          412.52 
 
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' 
 'S'  'S'   0.1246   0.1234 
 '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 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 
_cell_length_a                    5.939(4) 
_cell_length_b                    14.950(7) 
_cell_length_c                    11.748(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.14(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      1042.9(11) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     35 
_cell_measurement_theta_min       10 
_cell_measurement_theta_max       16 
 
_exptl_crystal_description        tablet 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.31 
_exptl_crystal_size_mid           0.22 
_exptl_crystal_size_min           0.14 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.314 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              440 
_exptl_absorpt_coefficient_mu     0.183 
_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      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Stoe Stadi-4 four-circle' 
_diffrn_measurement_method        'omega-theta' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%         'random variation +/-8' 
_diffrn_reflns_number             3195 
_diffrn_reflns_av_R_equivalents   ?
_diffrn_reflns_av_sigmaI/netI     0.1174 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.72 
_diffrn_reflns_theta_max          25.06 
_reflns_number_total              3195 
_reflns_number_gt                 2171 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'STADI4 v1.07 (Stoe, 1997)' 
_computing_cell_refinement        'STADI4 v1.07' 
_computing_data_reduction         'XRED v1.09 (Stoe, 1996)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL v5.03 (Sheldrick, 1994)' 
_computing_publication_material   SHELXL-97 
 
_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 w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+6.0861P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'Direct methods' 
_atom_sites_solution_secondary    'Difference map' 
_atom_sites_solution_hydrogens    'geometrically idealised' 
_refine_ls_hydrogen_treatment     'riding model' 
_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    0.2(6) 
_refine_ls_number_reflns          3195 
_refine_ls_number_parameters      263 
_refine_ls_number_restraints      82 
_refine_ls_R_factor_all           0.1605 
_refine_ls_R_factor_gt            0.0988 
_refine_ls_wR_factor_ref          0.2436 
_refine_ls_wR_factor_gt           0.1951 
_refine_ls_goodness_of_fit_ref    1.195 
_refine_ls_restrained_S_all       1.181 
_refine_ls_shift/su_max           0.005 
_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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
S1 S 0.7248(5) 0.3795(5) 0.54750(19) 0.0241(6) Uani 1 d U . . 
O1 O 1.0063(14) 0.2508(5) 0.4814(5) 0.0292(19) Uani 1 d U . . 
C1 C 0.9717(18) 0.2628(8) 0.3788(8) 0.022(2) Uani 1 d U . . 
O2 O 0.8646(13) 0.4390(5) 0.1676(5) 0.0267(18) Uani 1 d U . . 
C2 C 0.8744(17) 0.3481(7) 0.3343(7) 0.018(2) Uani 1 d U . . 
O3 O 0.8718(13) 0.5821(5) 0.4578(6) 0.0267(17) Uani 1 d U . . 
H3 H 0.8898 0.6372 0.4686 0.040 Uiso 1 calc R . . 
C3 C 0.8913(18) 0.3652(8) 0.2098(7) 0.021(2) Uani 1 d U . . 
O4 O 0.3802(12) 0.3899(5) 0.2598(5) 0.0246(16) Uani 1 d U . . 
C4 C 0.941(2) 0.2858(7) 0.1335(8) 0.026(3) Uani 1 d U . . 
H4A H 1.1030 0.2876 0.1144 0.031 Uiso 1 calc R . . 
H4B H 0.8537 0.2928 0.0615 0.031 Uiso 1 calc R . . 
C5 C 0.889(2) 0.1937(7) 0.1832(8) 0.026(2) Uani 1 d U . . 
C6 C 1.021(2) 0.1903(8) 0.2960(8) 0.027(2) Uani 1 d U . . 
H6A H 0.9903 0.1322 0.3329 0.033 Uiso 1 calc R . . 
H6B H 1.1837 0.1921 0.2795 0.033 Uiso 1 calc R . . 
C7 C 0.6928(18) 0.5688(7) 0.3878(7) 0.020(2) Uani 1 d U . . 
C8 C 0.6319(19) 0.4833(7) 0.3584(8) 0.0194(19) Uani 1 d U . . 
C9 C 0.4376(19) 0.4657(7) 0.2855(8) 0.022(2) Uani 1 d U . . 
C10 C 0.2899(18) 0.5443(7) 0.2485(9) 0.024(2) Uani 1 d U . . 
H10A H 0.1688 0.5524 0.3043 0.029 Uiso 1 calc R . . 
H10B H 0.2181 0.5304 0.1738 0.029 Uiso 1 calc R . . 
C11 C 0.4254(19) 0.6330(8) 0.2388(8) 0.024(2) Uani 1 d U . . 
C12 C 0.559(2) 0.6481(8) 0.3497(9) 0.028(2) Uani 1 d U . . 
H12A H 0.6622 0.6993 0.3393 0.034 Uiso 1 calc R . . 
H12B H 0.4527 0.6644 0.4102 0.034 Uiso 1 calc R . . 
C13 C 0.252(2) 0.7093(8) 0.2207(9) 0.033(3) Uani 1 d U . . 
H13A H 0.1673 0.6993 0.1494 0.049 Uiso 1 calc R . . 
H13B H 0.3310 0.7667 0.2170 0.049 Uiso 1 calc R . . 
H13C H 0.1476 0.7101 0.2843 0.049 Uiso 1 calc R . . 
C14 C 0.582(2) 0.6297(8) 0.1377(8) 0.028(3) Uani 1 d U . . 
H14A H 0.6917 0.5812 0.1488 0.042 Uiso 1 calc R . . 
H14B H 0.6623 0.6868 0.1315 0.042 Uiso 1 calc R . . 
H14C H 0.4939 0.6189 0.0677 0.042 Uiso 1 calc R . . 
C15 C 0.6385(19) 0.1865(8) 0.2001(10) 0.035(3) Uani 1 d U . . 
H15A H 0.6034 0.1280 0.2329 0.052 Uiso 1 calc R . . 
H15B H 0.5596 0.1929 0.1265 0.052 Uiso 1 calc R . . 
H15C H 0.5899 0.2339 0.2517 0.052 Uiso 1 calc R . . 
C16 C 0.974(2) 0.1213(8) 0.1031(9) 0.032(3) Uani 1 d U . . 
H16A H 0.9436 0.0622 0.1355 0.048 Uiso 1 calc R . . 
H16B H 1.1369 0.1283 0.0935 0.048 Uiso 1 calc R . . 
H16C H 0.8970 0.1268 0.0290 0.048 Uiso 1 calc R . . 
C17 C 0.7600(17) 0.4042(7) 0.4036(8) 0.021(2) Uani 1 d U . . 
C18 C 0.4921(19) 0.4535(8) 0.5880(8) 0.026(2) Uani 1 d U . . 
H18A H 0.5328 0.5171 0.5767 0.031 Uiso 1 calc R . . 
H18B H 0.3541 0.4401 0.5426 0.031 Uiso 1 calc R . . 
C19 C 0.4573(18) 0.4332(5) 0.7150(7) 0.023(2) Uani 1 d DU . . 
C20 C 0.6182(19) 0.4575(3) 0.7945(8) 0.022(2) Uani 1 d DU . . 
H20 H 0.7535 0.4850 0.7706 0.027 Uiso 1 calc R . . 
C21 C 0.585(2) 0.4422(5) 0.9101(8) 0.028(2) Uani 1 d DU . . 
H21 H 0.6970 0.4591 0.9650 0.034 Uiso 1 calc R . . 
C22 C 0.3860(19) 0.4019(6) 0.9438(8) 0.031(3) Uani 1 d DU . . 
H22 H 0.3621 0.3914 1.0224 0.037 Uiso 1 calc R . . 
C23 C 0.2255(18) 0.3773(7) 0.8660(8) 0.030(2) Uani 1 d DU . . 
H23 H 0.0907 0.3494 0.8901 0.036 Uiso 1 calc R . . 
C24 C 0.2601(17) 0.3935(6) 0.7479(8) 0.026(2) Uani 1 d DU . . 
H24 H 0.1485 0.3770 0.6927 0.031 Uiso 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 
S1 0.0364(17) 0.0256(14) 0.0104(11) 0.0001(11) 0.0014(10) 0.0050(15) 
O1 0.049(5) 0.027(4) 0.012(3) 0.007(3) -0.004(3) 0.005(4) 
C1 0.026(6) 0.030(5) 0.011(4) -0.002(4) 0.000(4) 0.003(5) 
O2 0.046(5) 0.023(4) 0.011(3) 0.004(3) 0.005(3) 0.005(4) 
C2 0.022(6) 0.024(5) 0.008(4) 0.000(3) -0.002(4) -0.004(4) 
O3 0.037(5) 0.017(4) 0.025(4) -0.002(3) -0.007(3) -0.001(3) 
C3 0.028(6) 0.029(5) 0.005(4) -0.004(4) 0.000(4) 0.002(5) 
O4 0.034(4) 0.019(3) 0.021(3) -0.002(3) -0.008(3) 0.007(4) 
C4 0.044(7) 0.028(5) 0.006(4) 0.003(4) 0.004(5) 0.006(5) 
C5 0.048(7) 0.023(5) 0.008(4) 0.000(4) 0.012(4) 0.009(5) 
C6 0.045(7) 0.023(5) 0.014(4) 0.003(4) 0.006(4) 0.007(5) 
C7 0.030(6) 0.029(4) 0.002(4) -0.002(4) 0.002(3) -0.001(4) 
C8 0.028(5) 0.022(4) 0.009(4) 0.002(3) 0.004(4) -0.004(4) 
C9 0.030(6) 0.023(5) 0.012(5) 0.001(4) 0.002(4) 0.000(4) 
C10 0.022(6) 0.028(5) 0.022(5) -0.003(4) -0.003(4) 0.004(4) 
C11 0.030(6) 0.024(5) 0.017(5) -0.004(4) -0.005(4) 0.004(5) 
C12 0.041(7) 0.026(5) 0.017(5) -0.003(4) -0.006(4) 0.000(5) 
C13 0.045(7) 0.031(6) 0.023(5) -0.003(5) -0.005(5) 0.008(5) 
C14 0.044(7) 0.023(5) 0.017(5) 0.005(4) 0.000(5) 0.000(5) 
C15 0.041(6) 0.025(6) 0.038(7) -0.004(5) 0.000(5) -0.006(5) 
C16 0.048(8) 0.023(5) 0.026(5) -0.005(4) 0.007(6) 0.001(6) 
C17 0.022(5) 0.024(5) 0.019(4) 0.006(4) 0.008(4) -0.005(4) 
C18 0.033(7) 0.033(6) 0.011(4) -0.002(4) -0.001(4) 0.007(5) 
C19 0.034(6) 0.025(5) 0.010(4) 0.007(4) 0.005(4) 0.008(5) 
C20 0.035(6) 0.015(5) 0.016(4) -0.004(4) 0.000(4) 0.010(4) 
C21 0.044(6) 0.022(6) 0.018(4) -0.007(4) -0.002(5) 0.013(5) 
C22 0.046(7) 0.035(7) 0.011(4) -0.003(4) 0.004(4) 0.002(5) 
C23 0.041(6) 0.032(6) 0.017(4) 0.009(5) 0.005(4) -0.003(6) 
C24 0.032(6) 0.022(6) 0.022(4) -0.001(4) -0.006(4) -0.001(5) 
 
_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 
S1 C17 1.747(9) . ? 
S1 C18 1.841(11) . ? 
O1 C1 1.232(11) . ? 
C1 C6 1.490(13) . ? 
C1 C2 1.490(14) . ? 
O2 C3 1.219(12) . ? 
C2 C17 1.361(13) . ? 
C2 C3 1.490(12) . ? 
O3 C7 1.346(13) . ? 
C3 C4 1.521(13) . ? 
O4 C9 1.220(12) . ? 
C4 C5 1.530(14) . ? 
C5 C15 1.511(15) . ? 
C5 C6 1.525(15) . ? 
C5 C16 1.527(13) . ? 
C7 C8 1.371(14) . ? 
C7 C12 1.491(15) . ? 
C8 C9 1.447(15) . ? 
C8 C17 1.497(14) . ? 
C9 C10 1.524(14) . ? 
C10 C11 1.557(15) . ? 
C11 C14 1.526(13) . ? 
C11 C12 1.527(15) . ? 
C11 C13 1.549(15) . ? 
C18 C19 1.541(12) . ? 
C19 C20 1.372(15) . ? 
C19 C24 1.375(14) . ? 
C20 C21 1.394(13) . ? 
C21 C22 1.393(16) . ? 
C22 C23 1.358(15) . ? 
C23 C24 1.428(13) . ? 
 
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 
C17 S1 C18 103.1(5) . . ? 
O1 C1 C6 120.1(10) . . ? 
O1 C1 C2 121.6(9) . . ? 
C6 C1 C2 118.2(8) . . ? 
C17 C2 C3 121.7(9) . . ? 
C17 C2 C1 120.8(8) . . ? 
C3 C2 C1 117.3(8) . . ? 
O2 C3 C2 123.0(8) . . ? 
O2 C3 C4 119.5(8) . . ? 
C2 C3 C4 117.5(9) . . ? 
C3 C4 C5 115.7(7) . . ? 
C15 C5 C6 111.9(8) . . ? 
C15 C5 C16 111.6(10) . . ? 
C6 C5 C16 110.0(9) . . ? 
C15 C5 C4 108.7(9) . . ? 
C6 C5 C4 104.9(9) . . ? 
C16 C5 C4 109.3(8) . . ? 
C1 C6 C5 116.1(9) . . ? 
O3 C7 C8 119.5(10) . . ? 
O3 C7 C12 118.5(9) . . ? 
C8 C7 C12 121.9(10) . . ? 
C7 C8 C9 121.5(10) . . ? 
C7 C8 C17 121.2(10) . . ? 
C9 C8 C17 117.3(9) . . ? 
O4 C9 C8 122.1(10) . . ? 
O4 C9 C10 119.3(10) . . ? 
C8 C9 C10 118.4(9) . . ? 
C9 C10 C11 112.5(9) . . ? 
C14 C11 C12 110.7(10) . . ? 
C14 C11 C13 109.4(9) . . ? 
C12 C11 C13 109.9(9) . . ? 
C14 C11 C10 110.7(8) . . ? 
C12 C11 C10 108.9(9) . . ? 
C13 C11 C10 107.1(9) . . ? 
C7 C12 C11 113.8(9) . . ? 
C2 C17 C8 122.1(8) . . ? 
C2 C17 S1 121.3(8) . . ? 
C8 C17 S1 116.2(7) . . ? 
C19 C18 S1 104.3(7) . . ? 
C20 C19 C24 120.6(9) . . ? 
C20 C19 C18 120.1(9) . . ? 
C24 C19 C18 119.2(10) . . ? 
C19 C20 C21 120.7(10) . . ? 
C22 C21 C20 119.0(11) . . ? 
C23 C22 C21 121.0(9) . . ? 
C22 C23 C24 119.7(10) . . ? 
C19 C24 C23 119.1(10) . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O1 C1 C2 C17 -19.7(16) . . . . ? 
C6 C1 C2 C17 158.6(10) . . . . ? 
O1 C1 C2 C3 165.3(10) . . . . ? 
C6 C1 C2 C3 -16.5(14) . . . . ? 
C17 C2 C3 O2 21.7(16) . . . . ? 
C1 C2 C3 O2 -163.3(10) . . . . ? 
C17 C2 C3 C4 -157.6(10) . . . . ? 
C1 C2 C3 C4 17.4(14) . . . . ? 
O2 C3 C4 C5 -158.8(11) . . . . ? 
C2 C3 C4 C5 20.5(14) . . . . ? 
C3 C4 C5 C15 64.6(12) . . . . ? 
C3 C4 C5 C6 -55.3(12) . . . . ? 
C3 C4 C5 C16 -173.3(10) . . . . ? 
O1 C1 C6 C5 155.5(10) . . . . ? 
C2 C1 C6 C5 -22.8(14) . . . . ? 
C15 C5 C6 C1 -60.9(13) . . . . ? 
C16 C5 C6 C1 174.3(9) . . . . ? 
C4 C5 C6 C1 56.8(11) . . . . ? 
O3 C7 C8 C9 178.5(8) . . . . ? 
C12 C7 C8 C9 2.0(13) . . . . ? 
O3 C7 C8 C17 0.5(13) . . . . ? 
C12 C7 C8 C17 -176.0(9) . . . . ? 
C7 C8 C9 O4 -179.1(9) . . . . ? 
C17 C8 C9 O4 -1.0(13) . . . . ? 
C7 C8 C9 C10 -4.4(13) . . . . ? 
C17 C8 C9 C10 173.6(8) . . . . ? 
O4 C9 C10 C11 -154.8(8) . . . . ? 
C8 C9 C10 C11 30.4(12) . . . . ? 
C9 C10 C11 C14 70.0(11) . . . . ? 
C9 C10 C11 C12 -52.0(11) . . . . ? 
C9 C10 C11 C13 -170.8(8) . . . . ? 
O3 C7 C12 C11 157.0(9) . . . . ? 
C8 C7 C12 C11 -26.4(14) . . . . ? 
C14 C11 C12 C7 -72.0(12) . . . . ? 
C13 C11 C12 C7 167.1(9) . . . . ? 
C10 C11 C12 C7 50.0(12) . . . . ? 
C3 C2 C17 C8 3.9(15) . . . . ? 
C1 C2 C17 C8 -170.9(9) . . . . ? 
C3 C2 C17 S1 175.5(8) . . . . ? 
C1 C2 C17 S1 0.7(14) . . . . ? 
C7 C8 C17 C2 -116.1(11) . . . . ? 
C9 C8 C17 C2 65.8(12) . . . . ? 
C7 C8 C17 S1 71.9(11) . . . . ? 
C9 C8 C17 S1 -106.2(9) . . . . ? 
C18 S1 C17 C2 -162.6(9) . . . . ? 
C18 S1 C17 C8 9.5(9) . . . . ? 
C17 S1 C18 C19 -179.9(8) . . . . ? 
S1 C18 C19 C20 68.6(8) . . . . ? 
S1 C18 C19 C24 -113.7(6) . . . . ? 
C24 C19 C20 C21 0.1(3) . . . . ? 
C18 C19 C20 C21 177.8(7) . . . . ? 
C19 C20 C21 C22 0.0(3) . . . . ? 
C20 C21 C22 C23 0.2(6) . . . . ? 
C21 C22 C23 C24 -0.4(8) . . . . ? 
C20 C19 C24 C23 -0.4(6) . . . . ? 
C18 C19 C24 C23 -178.1(8) . . . . ? 
C22 C23 C24 C19 0.5(8) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              25.06 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.41 
_refine_diff_density_min   -0.55 
_refine_diff_density_rms    0.11