data_Global _audit_creation_method SHELXL-97 #------------------------------------------------------------------------------ _publ_contact_author ; Masood Parvez Department of Chemistry University of Calgary 2500 University Drive N.W. Calgary, Alberta, Canada T2N 1N4 ; #----------------------------------------------------------------------------- _publ_requested_journal ' ? ' _publ_requested_coeditor_name ' ? ' _publ_contact_author_phone ' (403)220-5348 ' _publ_contact_author_fax ' (403)289-9488 ' _publ_contact_author_email ' parvez@ucalgary.ca ' #------------------------------------------------------------------------------ _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address 'Parvez, Masood' ; Department of Chemistry The University of Calgary 2500 University Drive NW Calgary Alberta Canada T2N 1N4 ; #------------------------------------------------------------------------------ data_Compound_I #----------------------------------------------------------------------------- _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SAPI91 (Fan, 1991)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' #----------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 B2 N2' _chemical_formula_weight 314.03 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' 'B' 'B' 0.0013 0.0007 '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.889(3) _cell_length_b 13.432(3) _cell_length_c 13.471(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.972(16) _cell_angle_gamma 90.00 _cell_volume 1786.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7812 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9921 _exptl_absorpt_correction_T_max 0.9947 _exptl_absorpt_process_details ' SORTAV: (Blessing, 1997) ' _diffrn_ambient_temperature 173(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 '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7812 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4062 _reflns_number_gt 2877 _reflns_threshold_expression >2sigma(I) _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^)+(0.0680P)^2^+0.5100P] 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 4062 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 N1 N 0.66209(12) 0.02482(9) 0.43107(9) 0.0318(3) Uani 1 1 d . . . N2 N 0.53954(12) 0.05752(9) 0.38368(9) 0.0325(3) Uani 1 1 d . . . C1 C 0.72096(18) -0.06138(11) 0.39417(12) 0.0398(4) Uani 1 1 d . . . H1 H 0.8043 -0.0859 0.4246 0.048 Uiso 1 1 d R . . C2 C 0.66839(19) -0.11276(12) 0.31648(13) 0.0464(4) Uani 1 1 d . . . H2 H 0.7132 -0.1714 0.2941 0.056 Uiso 1 1 d R . . C3 C 0.54550(19) -0.07988(13) 0.26871(13) 0.0476(4) Uani 1 1 d . . . H3 H 0.5070 -0.1157 0.2124 0.057 Uiso 1 1 d R . . C4 C 0.48610(18) 0.00191(13) 0.30375(12) 0.0423(4) Uani 1 1 d . . . H4 H 0.4017 0.0212 0.2708 0.051 Uiso 1 1 d R . . C5 C 0.85314(16) 0.04316(12) 0.57119(12) 0.0381(4) Uani 1 1 d . . . H5 H 0.8975 -0.0177 0.5545 0.046 Uiso 1 1 d R . . C6 C 0.90373(15) 0.09979(12) 0.64783(12) 0.0378(4) Uani 1 1 d . . . H6 H 0.9837 0.0788 0.6856 0.045 Uiso 1 1 d R . . C7 C 0.84513(14) 0.19244(11) 0.67782(11) 0.0325(3) Uani 1 1 d . . . C8 C 0.73049(15) 0.22798(11) 0.62923(11) 0.0313(3) Uani 1 1 d . . . H8 H 0.6921 0.2900 0.6492 0.038 Uiso 1 1 d R . . C9 C 0.66248(14) 0.17637(10) 0.54804(10) 0.0295(3) Uani 1 1 d . . . C10 C 0.53950(14) 0.20919(10) 0.50094(11) 0.0297(3) Uani 1 1 d . . . C11 C 0.46999(15) 0.29774(11) 0.53008(11) 0.0336(3) Uani 1 1 d . . . H11 H 0.5118 0.3407 0.5796 0.040 Uiso 1 1 d R . . C12 C 0.34577(15) 0.32462(11) 0.48984(11) 0.0349(4) Uani 1 1 d . . . C13 C 0.27822(16) 0.26387(12) 0.41474(12) 0.0388(4) Uani 1 1 d . . . H13 H 0.1896 0.2819 0.3884 0.047 Uiso 1 1 d R . . C14 C 0.33312(16) 0.17997(12) 0.37642(11) 0.0383(4) Uani 1 1 d . . . H14 H 0.2839 0.1438 0.3248 0.046 Uiso 1 1 d R . . C15 C 0.91175(16) 0.24428(12) 0.76786(11) 0.0385(4) Uani 1 1 d . . . H15 H 1.0077 0.2373 0.7625 0.046 Uiso 1 1 d R . . C16 C 0.8700(2) 0.19341(15) 0.86283(13) 0.0559(5) Uani 1 1 d . . . H16A H 0.9125 0.2263 0.9195 0.067 Uiso 1 1 d R . . H16B H 0.8976 0.1249 0.8624 0.067 Uiso 1 1 d R . . H16C H 0.7734 0.1971 0.8663 0.067 Uiso 1 1 d R . . C17 C 0.88440(19) 0.35526(13) 0.77335(14) 0.0485(4) Uani 1 1 d . . . H17A H 0.9298 0.3825 0.8319 0.058 Uiso 1 1 d R . . H17B H 0.7887 0.3659 0.7760 0.058 Uiso 1 1 d R . . H17C H 0.9167 0.3875 0.7156 0.058 Uiso 1 1 d R . . C18 C 0.27497(17) 0.41674(12) 0.52723(13) 0.0417(4) Uani 1 1 d . . . H18 H 0.3400 0.4523 0.5691 0.050 Uiso 1 1 d R . . C19 C 0.1561(2) 0.38776(15) 0.58876(15) 0.0559(5) Uani 1 1 d . . . H19A H 0.1124 0.4465 0.6119 0.067 Uiso 1 1 d R . . H19B H 0.1875 0.3482 0.6446 0.067 Uiso 1 1 d R . . H19C H 0.0929 0.3498 0.5476 0.067 Uiso 1 1 d R . . C20 C 0.2309(2) 0.48788(14) 0.44418(15) 0.0533(5) Uani 1 1 d . . . H20A H 0.1874 0.5451 0.4709 0.064 Uiso 1 1 d R . . H20B H 0.1687 0.4539 0.3988 0.064 Uiso 1 1 d R . . H20C H 0.3086 0.5087 0.4097 0.064 Uiso 1 1 d R . . B1 B 0.72487(17) 0.07969(12) 0.51444(12) 0.0312(4) Uani 1 1 d . . . B2 B 0.47245(17) 0.14693(13) 0.41834(12) 0.0315(4) 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 N1 0.0367(7) 0.0299(6) 0.0294(6) 0.0011(5) 0.0065(5) 0.0017(5) N2 0.0368(7) 0.0341(7) 0.0267(6) -0.0007(5) 0.0028(5) -0.0048(5) C1 0.0520(10) 0.0330(8) 0.0355(8) -0.0009(6) 0.0130(7) 0.0057(7) C2 0.0663(12) 0.0354(8) 0.0389(9) -0.0061(7) 0.0168(8) 0.0002(8) C3 0.0617(11) 0.0464(9) 0.0353(9) -0.0110(7) 0.0102(8) -0.0119(8) C4 0.0487(10) 0.0471(9) 0.0313(8) -0.0068(7) 0.0035(7) -0.0093(7) C5 0.0385(8) 0.0357(8) 0.0403(9) 0.0007(7) 0.0054(7) 0.0104(6) C6 0.0309(8) 0.0418(9) 0.0404(9) 0.0027(7) -0.0008(6) 0.0095(6) C7 0.0292(7) 0.0365(8) 0.0317(8) 0.0021(6) 0.0010(6) 0.0018(6) C8 0.0326(8) 0.0277(7) 0.0336(8) -0.0002(6) 0.0009(6) 0.0029(6) C9 0.0299(7) 0.0296(7) 0.0291(7) 0.0021(6) 0.0031(6) 0.0002(6) C10 0.0306(7) 0.0297(7) 0.0288(7) 0.0034(6) 0.0018(6) 0.0007(6) C11 0.0338(8) 0.0311(8) 0.0353(8) 0.0002(6) -0.0032(6) 0.0025(6) C12 0.0350(8) 0.0347(8) 0.0346(8) 0.0049(6) -0.0003(6) 0.0043(6) C13 0.0338(8) 0.0450(9) 0.0369(8) 0.0081(7) -0.0055(6) 0.0037(7) C14 0.0411(9) 0.0423(9) 0.0306(8) 0.0021(6) -0.0058(6) -0.0045(7) C15 0.0317(8) 0.0481(9) 0.0351(8) -0.0007(7) -0.0046(6) 0.0053(7) C16 0.0729(13) 0.0581(11) 0.0361(9) 0.0042(8) -0.0028(9) 0.0040(10) C17 0.0538(11) 0.0468(10) 0.0436(10) -0.0070(8) -0.0092(8) -0.0046(8) C18 0.0398(9) 0.0403(9) 0.0444(9) 0.0008(7) -0.0033(7) 0.0095(7) C19 0.0600(12) 0.0564(11) 0.0520(11) 0.0028(9) 0.0116(9) 0.0149(9) C20 0.0617(12) 0.0455(10) 0.0527(11) 0.0060(8) 0.0032(9) 0.0165(9) B1 0.0341(9) 0.0309(8) 0.0292(8) 0.0021(7) 0.0056(7) 0.0002(7) B2 0.0350(9) 0.0321(8) 0.0277(8) 0.0034(7) 0.0037(7) -0.0018(7) _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 N1 C1 1.3989(19) . ? N1 N2 1.4103(17) . ? N1 B1 1.455(2) . ? N2 C4 1.3919(19) . ? N2 B2 1.460(2) . ? C1 C2 1.336(2) . ? C1 H1 0.9600 . ? C2 C3 1.416(3) . ? C2 H2 0.9601 . ? C3 C4 1.343(2) . ? C3 H3 0.9600 . ? C4 H4 0.9600 . ? C5 C6 1.357(2) . ? C5 B1 1.528(2) . ? C5 H5 0.9600 . ? C6 C7 1.440(2) . ? C6 H6 0.9600 . ? C7 C8 1.365(2) . ? C7 C15 1.519(2) . ? C8 C9 1.433(2) . ? C8 H8 0.9601 . ? C9 C10 1.413(2) . ? C9 B1 1.517(2) . ? C10 C11 1.438(2) . ? C10 B2 1.517(2) . ? C11 C12 1.365(2) . ? C11 H11 0.9600 . ? C12 C13 1.437(2) . ? C12 C18 1.520(2) . ? C13 C14 1.364(2) . ? C13 H13 0.9600 . ? C14 B2 1.528(2) . ? C14 H14 0.9599 . ? C15 C17 1.518(2) . ? C15 C16 1.526(2) . ? C15 H15 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.518(2) . ? C18 C19 1.524(3) . ? C18 H18 0.9600 . ? C19 H19A 0.9601 . ? C19 H19B 0.9600 . ? C19 H19C 0.9599 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? 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 C1 N1 N2 117.43(12) . . ? C1 N1 B1 121.64(13) . . ? N2 N1 B1 120.93(12) . . ? C4 N2 N1 117.77(13) . . ? C4 N2 B2 121.88(13) . . ? N1 N2 B2 120.35(12) . . ? C2 C1 N1 123.61(16) . . ? C2 C1 H1 116.7 . . ? N1 C1 H1 119.7 . . ? C1 C2 C3 119.00(16) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 118.43(16) . . ? C4 C3 H3 121.7 . . ? C2 C3 H3 119.9 . . ? C3 C4 N2 123.74(16) . . ? C3 C4 H4 116.3 . . ? N2 C4 H4 119.9 . . ? C6 C5 B1 117.68(14) . . ? C6 C5 H5 120.0 . . ? B1 C5 H5 122.3 . . ? C5 C6 C7 124.07(14) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 116.0 . . ? C8 C7 C6 120.27(14) . . ? C8 C7 C15 122.52(14) . . ? C6 C7 C15 117.14(13) . . ? C7 C8 C9 122.82(13) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 117.2 . . ? C10 C9 C8 123.43(13) . . ? C10 C9 B1 119.15(13) . . ? C8 C9 B1 117.38(13) . . ? C9 C10 C11 123.22(13) . . ? C9 C10 B2 119.39(13) . . ? C11 C10 B2 117.33(13) . . ? C12 C11 C10 122.90(14) . . ? C12 C11 H11 117.6 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 120.33(14) . . ? C11 C12 C18 120.26(14) . . ? C13 C12 C18 119.35(13) . . ? C14 C13 C12 123.78(14) . . ? C14 C13 H13 116.3 . . ? C12 C13 H13 119.9 . . ? C13 C14 B2 117.98(14) . . ? C13 C14 H14 119.7 . . ? B2 C14 H14 122.3 . . ? C17 C15 C7 114.72(13) . . ? C17 C15 C16 110.02(15) . . ? C7 C15 C16 109.83(14) . . ? C17 C15 H15 106.2 . . ? C7 C15 H15 106.5 . . ? C16 C15 H15 109.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.3 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.7 . . ? C15 C17 H17B 109.0 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.7 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C12 112.80(14) . . ? C20 C18 C19 111.21(15) . . ? C12 C18 C19 110.72(14) . . ? C20 C18 H18 106.1 . . ? C12 C18 H18 107.1 . . ? C19 C18 H18 108.6 . . ? C18 C19 H19A 109.9 . . ? C18 C19 H19B 109.9 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 108.6 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 110.2 . . ? C18 C20 H20B 108.7 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 B1 C9 120.00(13) . . ? N1 B1 C5 122.25(14) . . ? C9 B1 C5 117.75(14) . . ? N2 B2 C10 119.96(13) . . ? N2 B2 C14 122.46(14) . . ? C10 B2 C14 117.56(14) . . ? 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 C1 N1 N2 C4 -0.06(19) . . . . ? B1 N1 N2 C4 179.33(13) . . . . ? C1 N1 N2 B2 179.97(13) . . . . ? B1 N1 N2 B2 -0.65(19) . . . . ? N2 N1 C1 C2 0.9(2) . . . . ? B1 N1 C1 C2 -178.47(15) . . . . ? N1 C1 C2 C3 -0.8(3) . . . . ? C1 C2 C3 C4 -0.2(3) . . . . ? C2 C3 C4 N2 1.1(3) . . . . ? N1 N2 C4 C3 -0.9(2) . . . . ? B2 N2 C4 C3 179.04(15) . . . . ? B1 C5 C6 C7 -0.9(2) . . . . ? C5 C6 C7 C8 0.9(2) . . . . ? C5 C6 C7 C15 177.68(15) . . . . ? C6 C7 C8 C9 0.5(2) . . . . ? C15 C7 C8 C9 -176.11(14) . . . . ? C7 C8 C9 C10 176.10(14) . . . . ? C7 C8 C9 B1 -1.7(2) . . . . ? C8 C9 C10 C11 -0.2(2) . . . . ? B1 C9 C10 C11 177.55(14) . . . . ? C8 C9 C10 B2 -177.47(13) . . . . ? B1 C9 C10 B2 0.3(2) . . . . ? C9 C10 C11 C12 -174.42(14) . . . . ? B2 C10 C11 C12 2.9(2) . . . . ? C10 C11 C12 C13 -0.1(2) . . . . ? C10 C11 C12 C18 177.26(14) . . . . ? C11 C12 C13 C14 -2.6(2) . . . . ? C18 C12 C13 C14 179.98(15) . . . . ? C12 C13 C14 B2 2.1(2) . . . . ? C8 C7 C15 C17 -25.7(2) . . . . ? C6 C7 C15 C17 157.63(15) . . . . ? C8 C7 C15 C16 98.86(18) . . . . ? C6 C7 C15 C16 -77.85(18) . . . . ? C11 C12 C18 C20 127.22(17) . . . . ? C13 C12 C18 C20 -55.4(2) . . . . ? C11 C12 C18 C19 -107.42(18) . . . . ? C13 C12 C18 C19 69.98(19) . . . . ? C1 N1 B1 C9 176.13(13) . . . . ? N2 N1 B1 C9 -3.2(2) . . . . ? C1 N1 B1 C5 -4.2(2) . . . . ? N2 N1 B1 C5 176.42(13) . . . . ? C10 C9 B1 N1 3.4(2) . . . . ? C8 C9 B1 N1 -178.76(13) . . . . ? C10 C9 B1 C5 -176.30(13) . . . . ? C8 C9 B1 C5 1.6(2) . . . . ? C6 C5 B1 N1 179.98(14) . . . . ? C6 C5 B1 C9 -0.4(2) . . . . ? C4 N2 B2 C10 -175.65(13) . . . . ? N1 N2 B2 C10 4.3(2) . . . . ? C4 N2 B2 C14 6.1(2) . . . . ? N1 N2 B2 C14 -173.93(13) . . . . ? C9 C10 B2 N2 -4.1(2) . . . . ? C11 C10 B2 N2 178.47(13) . . . . ? C9 C10 B2 C14 174.25(13) . . . . ? C11 C10 B2 C14 -3.2(2) . . . . ? C13 C14 B2 N2 179.10(14) . . . . ? C13 C14 B2 C10 0.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.221 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.038 # start Validation Reply Form _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: Will appear in the paper ; # end Validation Reply Form