data_shelxl _publ_contact_author_name 'Werner Kaminsky' _publ_contact_author_address ; Department of Chemistry, BOX 351700 University of Washington Seattle, WA 98195 USA ; _publ_contact_author_email 'wernerka@u.washington.edu' _publ_requested_journal 'Journal title here' _publ_section_title ; title here ; loop_ _publ_author_name _publ_author_address 'Brian Cochran' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'John Freudenthal' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'Forest Michael' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; _publ_section_abstract ; Abstract here ; _publ_section_comment ; Details and comments here ; _publ_section_exptl_prep ; details of preparation here ; _publ_section_exptl_refinement ; All H atoms were initially located in a difference Fourier map and were refined with a riding model. H atoms were placed in geometrically idealised positions and constrained to ride on their parent atoms with C---H distances in the range 0.95-1.00 \%A. U~iso~ values were fixed such that they were 1.2U~eq~ of their parent atom U~eq~ for CH's and 1.5U~eq~ of their parent atom U~eq~ in case of methyl groups. ; _publ_section_references ; Altomare, A.; Cascarano, G.; Giacovazzo, C.; Burla, M.C.; Polidori, G.; Camalli, M. (1994) J. Appl. Cryst. 27, 435-442. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W. P., Garcia-Granada, S., Gould, R. O., Smits, J. M. M. & Smykalla, C. (1996) The DIRDIF96 Program System. Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. MacKay, S.; Gilmore, C.J.; Edwards, C.; Tremayne, M.; Stewart, N.; Shankland, K. (1998) "maXus: a computer program for the solution and refinement of crystal structures from diffraction data" University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan. Otwinowski, Z.; Minor, W. (1996) Methods in Enzymology, 276, 307-326. Sheldrick, G. M. (1997) SHELXL97 University of G\"ottingen, Germany. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'BMC-N-163' ; _chemical_name_common 'BMC-N-163' _chemical_melting_point ? _chemical_formula_moiety 'C15 H22 N2 O4 S' _chemical_formula_sum 'C15 H22 N2 O4 S' _chemical_formula_weight 326.41 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' 'N' 'N' 0.0061 0.0033 '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_space_group_name_H-M 'P 21/C' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 6.7394(4) _cell_length_b 26.2661(14) _cell_length_c 11.2310(6) _cell_angle_alpha 90.00 _cell_angle_beta 124.744(2) _cell_angle_gamma 90.00 _cell_volume 1633.52(16) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 534 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description 'cut-block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8807 _exptl_absorpt_correction_T_max 0.8807 _exptl_absorpt_process_details 'HKL2000' _exptl_special_details ; ?Data was collected with \w and \f scans in 2^o^ increments with 60 second exposures per degree. Crystal-to-detector distance was 30 mm. 25126 full and partial reflection were integrated. ; _diffrn_ambient_temperature 130(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 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 6016 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.38 _reflns_number_total 3293 _reflns_number_gt 2036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material 'SHELXL-97 (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^)+(0.0550P)^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 3293 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _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 S1 S 0.23796(12) 0.10582(2) 0.30772(7) 0.0366(2) Uani 1 1 d . . . O1 O 0.5531(3) 0.19197(6) 0.47926(17) 0.0350(4) Uani 1 1 d . . . O2 O -0.2001(3) 0.18813(7) 0.3485(2) 0.0418(5) Uani 1 1 d . . . H2 H -0.2833 0.1774 0.3773 0.063 Uiso 1 1 calc R . . O3 O 0.4235(3) 0.10897(6) 0.28331(19) 0.0416(5) Uani 1 1 d . . . O4 O 0.0119(3) 0.08237(7) 0.20201(19) 0.0445(5) Uani 1 1 d . . . N1 N 0.2445(3) 0.24513(7) 0.4198(2) 0.0310(5) Uani 1 1 d . . . N2 N 0.1629(4) 0.16380(7) 0.3230(2) 0.0353(5) Uani 1 1 d . . . H2A H 0.0090 0.1721 0.2726 0.042 Uiso 1 1 calc R . . C1 C 0.3355(4) 0.20052(9) 0.4137(3) 0.0305(6) Uani 1 1 d . . . C2 C 0.4020(4) 0.28992(9) 0.4836(3) 0.0340(6) Uani 1 1 d . . . H2B H 0.5569 0.2843 0.4946 0.041 Uiso 1 1 calc R . . H2C H 0.4357 0.2981 0.5795 0.041 Uiso 1 1 calc R . . C3 C 0.2565(4) 0.33244(9) 0.3745(3) 0.0328(6) Uani 1 1 d . . . C4 C 0.0040(4) 0.31949(10) 0.3317(3) 0.0368(6) Uani 1 1 d . . . H4A H -0.1194 0.3348 0.2368 0.044 Uiso 1 1 calc R . . H4B H -0.0210 0.3324 0.4051 0.044 Uiso 1 1 calc R . . C5 C -0.0134(4) 0.26101(9) 0.3230(3) 0.0338(6) Uani 1 1 d . . . H5 H -0.0822 0.2497 0.2215 0.041 Uiso 1 1 calc R . . C6 C -0.1684(5) 0.24159(10) 0.3704(3) 0.0396(6) Uani 1 1 d . . . H6A H -0.0906 0.2495 0.4742 0.048 Uiso 1 1 calc R . . H6B H -0.3276 0.2587 0.3140 0.048 Uiso 1 1 calc R . . C7 C 0.2716(5) 0.32819(10) 0.2442(3) 0.0400(6) Uani 1 1 d . . . H7A H 0.4335 0.3382 0.2730 0.060 Uiso 1 1 calc R . . H7B H 0.1514 0.3507 0.1667 0.060 Uiso 1 1 calc R . . H7C H 0.2398 0.2930 0.2093 0.060 Uiso 1 1 calc R . . C8 C 0.3441(5) 0.38467(9) 0.4445(3) 0.0406(6) Uani 1 1 d . . . H8A H 0.3316 0.3872 0.5271 0.061 Uiso 1 1 calc R . . H8B H 0.2443 0.4111 0.3734 0.061 Uiso 1 1 calc R . . H8C H 0.5129 0.3893 0.4782 0.061 Uiso 1 1 calc R . . C9 C 0.3558(4) 0.07599(9) 0.4758(3) 0.0342(6) Uani 1 1 d . . . C10 C 0.1974(5) 0.05975(10) 0.5088(3) 0.0387(6) Uani 1 1 d . . . H10 H 0.0286 0.0649 0.4420 0.046 Uiso 1 1 calc R . . C11 C 0.2870(5) 0.03583(10) 0.6401(3) 0.0406(7) Uani 1 1 d . . . H11 H 0.1786 0.0247 0.6632 0.049 Uiso 1 1 calc R . . C12 C 0.5331(5) 0.02791(9) 0.7383(3) 0.0383(6) Uani 1 1 d . . . C13 C 0.6877(5) 0.04420(10) 0.7020(3) 0.0417(7) Uani 1 1 d . . . H13 H 0.8565 0.0388 0.7681 0.050 Uiso 1 1 calc R . . C14 C 0.6005(4) 0.06822(9) 0.5709(3) 0.0372(6) Uani 1 1 d . . . H14 H 0.7082 0.0792 0.5471 0.045 Uiso 1 1 calc R . . C15 C 0.6326(5) 0.00276(10) 0.8829(3) 0.0484(7) Uani 1 1 d . . . H15A H 0.7568 -0.0220 0.9027 0.073 Uiso 1 1 calc R . . H15B H 0.5018 -0.0147 0.8804 0.073 Uiso 1 1 calc R . . H15C H 0.7038 0.0287 0.9593 0.073 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 S1 0.0426(4) 0.0310(4) 0.0349(4) -0.0045(3) 0.0213(3) -0.0031(3) O1 0.0336(10) 0.0353(10) 0.0325(10) 0.0017(7) 0.0167(8) 0.0021(8) O2 0.0411(11) 0.0395(11) 0.0498(12) 0.0033(9) 0.0289(9) -0.0024(8) O3 0.0528(11) 0.0378(11) 0.0460(11) -0.0026(8) 0.0350(10) -0.0008(9) O4 0.0448(11) 0.0376(10) 0.0383(11) -0.0087(8) 0.0160(9) -0.0083(9) N1 0.0275(11) 0.0309(12) 0.0289(12) 0.0010(9) 0.0127(10) 0.0031(9) N2 0.0328(11) 0.0301(12) 0.0362(12) -0.0023(9) 0.0155(10) -0.0007(9) C1 0.0314(14) 0.0292(14) 0.0308(14) 0.0002(11) 0.0177(12) -0.0006(11) C2 0.0319(13) 0.0307(14) 0.0308(14) -0.0007(11) 0.0129(12) -0.0030(11) C3 0.0396(14) 0.0278(14) 0.0277(13) 0.0004(10) 0.0171(12) 0.0015(11) C4 0.0369(14) 0.0346(14) 0.0316(14) 0.0036(11) 0.0150(12) 0.0063(12) C5 0.0330(13) 0.0332(14) 0.0318(14) 0.0000(11) 0.0165(12) 0.0026(11) C6 0.0375(15) 0.0424(17) 0.0378(16) -0.0004(12) 0.0208(13) 0.0001(12) C7 0.0482(16) 0.0335(15) 0.0368(15) 0.0030(11) 0.0234(13) 0.0022(12) C8 0.0481(16) 0.0298(14) 0.0370(15) -0.0023(11) 0.0201(13) -0.0007(12) C9 0.0412(15) 0.0245(13) 0.0399(15) -0.0065(11) 0.0248(13) -0.0059(11) C10 0.0404(15) 0.0364(16) 0.0428(17) -0.0052(12) 0.0258(14) -0.0014(12) C11 0.0532(17) 0.0353(15) 0.0454(17) -0.0068(12) 0.0353(15) -0.0076(13) C12 0.0506(17) 0.0253(14) 0.0406(16) -0.0064(11) 0.0269(14) -0.0036(12) C13 0.0412(15) 0.0356(15) 0.0431(17) 0.0002(13) 0.0211(14) -0.0015(12) C14 0.0377(14) 0.0305(14) 0.0476(17) -0.0004(12) 0.0268(14) -0.0030(12) C15 0.070(2) 0.0358(16) 0.0468(18) 0.0005(13) 0.0379(16) 0.0017(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 S1 O3 1.4272(17) . ? S1 O4 1.4309(18) . ? S1 N2 1.644(2) . ? S1 C9 1.760(3) . ? O1 C1 1.229(3) . ? O2 C6 1.421(3) . ? O2 H2 0.8400 . ? N1 C1 1.342(3) . ? N1 C2 1.469(3) . ? N1 C5 1.491(3) . ? N2 C1 1.404(3) . ? N2 H2A 0.8800 . ? C2 C3 1.530(3) . ? C2 H2B 0.9900 . ? C2 H2C 0.9900 . ? C3 C4 1.520(3) . ? C3 C8 1.523(3) . ? C3 C7 1.528(3) . ? C4 C5 1.539(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.506(3) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.376(3) . ? C9 C10 1.382(3) . ? C10 C11 1.386(4) . ? C10 H10 0.9500 . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 C13 1.385(4) . ? C12 C15 1.510(4) . ? C13 C14 1.388(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 O3 S1 O4 120.04(11) . . ? O3 S1 N2 108.77(10) . . ? O4 S1 N2 103.88(11) . . ? O3 S1 C9 108.82(11) . . ? O4 S1 C9 108.32(12) . . ? N2 S1 C9 106.13(11) . . ? C6 O2 H2 109.5 . . ? C1 N1 C2 120.00(19) . . ? C1 N1 C5 125.71(19) . . ? C2 N1 C5 110.46(18) . . ? C1 N2 S1 122.34(17) . . ? C1 N2 H2A 118.8 . . ? S1 N2 H2A 118.8 . . ? O1 C1 N1 123.5(2) . . ? O1 C1 N2 121.4(2) . . ? N1 C1 N2 115.0(2) . . ? N1 C2 C3 103.84(18) . . ? N1 C2 H2B 111.0 . . ? C3 C2 H2B 111.0 . . ? N1 C2 H2C 111.0 . . ? C3 C2 H2C 111.0 . . ? H2B C2 H2C 109.0 . . ? C4 C3 C8 113.5(2) . . ? C4 C3 C7 110.8(2) . . ? C8 C3 C7 110.0(2) . . ? C4 C3 C2 100.42(19) . . ? C8 C3 C2 111.2(2) . . ? C7 C3 C2 110.6(2) . . ? C3 C4 C5 105.91(19) . . ? C3 C4 H4A 110.6 . . ? C5 C4 H4A 110.6 . . ? C3 C4 H4B 110.6 . . ? C5 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? N1 C5 C6 113.7(2) . . ? N1 C5 C4 102.59(18) . . ? C6 C5 C4 111.0(2) . . ? N1 C5 H5 109.8 . . ? C6 C5 H5 109.8 . . ? C4 C5 H5 109.8 . . ? O2 C6 C5 109.9(2) . . ? O2 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? O2 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 120.9(2) . . ? C14 C9 S1 120.45(19) . . ? C10 C9 S1 118.7(2) . . ? C9 C10 C11 119.4(2) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C10 C11 C12 120.8(2) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 118.6(2) . . ? C13 C12 C15 120.3(2) . . ? C11 C12 C15 121.2(2) . . ? C14 C13 C12 121.2(2) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C9 C14 C13 119.1(2) . . ? C9 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 O3 S1 N2 C1 -48.7(2) . . . . ? O4 S1 N2 C1 -177.69(18) . . . . ? C9 S1 N2 C1 68.2(2) . . . . ? C2 N1 C1 O1 12.2(4) . . . . ? C5 N1 C1 O1 168.0(2) . . . . ? C2 N1 C1 N2 -166.35(19) . . . . ? C5 N1 C1 N2 -10.5(3) . . . . ? S1 N2 C1 O1 4.7(3) . . . . ? S1 N2 C1 N1 -176.68(17) . . . . ? C1 N1 C2 C3 133.6(2) . . . . ? C5 N1 C2 C3 -25.6(2) . . . . ? N1 C2 C3 C4 38.8(2) . . . . ? N1 C2 C3 C8 159.3(2) . . . . ? N1 C2 C3 C7 -78.2(2) . . . . ? C8 C3 C4 C5 -157.6(2) . . . . ? C7 C3 C4 C5 78.0(2) . . . . ? C2 C3 C4 C5 -38.9(2) . . . . ? C1 N1 C5 C6 83.6(3) . . . . ? C2 N1 C5 C6 -118.7(2) . . . . ? C1 N1 C5 C4 -156.5(2) . . . . ? C2 N1 C5 C4 1.2(2) . . . . ? C3 C4 C5 N1 24.0(2) . . . . ? C3 C4 C5 C6 145.8(2) . . . . ? N1 C5 C6 O2 -70.4(3) . . . . ? C4 C5 C6 O2 174.57(19) . . . . ? O3 S1 C9 C14 11.6(2) . . . . ? O4 S1 C9 C14 143.6(2) . . . . ? N2 S1 C9 C14 -105.3(2) . . . . ? O3 S1 C9 C10 -167.25(19) . . . . ? O4 S1 C9 C10 -35.2(2) . . . . ? N2 S1 C9 C10 75.8(2) . . . . ? C14 C9 C10 C11 0.7(4) . . . . ? S1 C9 C10 C11 179.48(19) . . . . ? C9 C10 C11 C12 -0.2(4) . . . . ? C10 C11 C12 C13 -0.3(4) . . . . ? C10 C11 C12 C15 178.8(2) . . . . ? C11 C12 C13 C14 0.4(4) . . . . ? C15 C12 C13 C14 -178.8(2) . . . . ? C10 C9 C14 C13 -0.7(4) . . . . ? S1 C9 C14 C13 -179.4(2) . . . . ? C12 C13 C14 C9 0.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.379 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.055