# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 188/197 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. Magnus Sandstr\"om Department of Chemistry, Inorganic Chemistry Royal Institute of Technology S-100 44 Stockholm Sweden ; _publ_contact_author_phone '+46-8-790 8156' _publ_contact_author_fax '+46-8 21 26 26' _publ_contact_author_email 'magnus@inorg.kth.se' _publ_requested_journal 'J. Chem. Soc., Perkin 2' #===================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; The Crystal and Liquid Structures of N,N-Dimethylthioformamide and N,N-Dimethylformamide Showing Stronger Effect of C-H...S than of C-H...O Hydrogen Bonding ; loop_ _publ_author_name _publ_author_address 'Dr. Christina M. V. St\%alhandske' ; Department of Chemistry, Swedish University of Agricultural Sciences, P.O. Box 7015 S-750 07 Uppsala Sweden ; 'Dr. Horst Borrmann' ; Max-Planck-Institut f\"ur Festk\"orperforschung Heisenbergstr. 1 D-70569 Stuttgart Germany ; 'Prof. Ingmar Persson' ; Department of Chemistry, Swedish University of Agricultural Sciences, P.O. Box 7015 S-750 07 Uppsala Sweden ; 'Prof. Magnus Sandstr\"om' ; Department of Chemistry, Inorganic Chemistry Royal Institute of Technology S-100 44 Stockholm Sweden ; #===================================================================== # 3. RESULTS data_csdmtf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'N,N-Dimethylthioformamide' _chemical_formula_moiety ? _chemical_formula_sum 'C3 H7 N S' _chemical_formula_weight 89.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0015 0.0009 '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' 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2~1~2~1~2~1~ loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 4.7487(7) _cell_length_b 5.9711(9) _cell_length_c 17.017(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 482.51(12) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 19.40 _cell_measurement_theta_max 23.46 _exptl_crystal_description cylinder _exptl_crystal_colour colorless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 192 _exptl_absorpt_coefficient_mu 0.253 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.767 _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.56086 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Syntex P2~1~' _diffrn_measurement_method '\w-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 73 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5764 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 30.0 _reflns_number_total 2885 _reflns_number_gt 2646 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1995)' _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 w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment iso _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 0.04(7) _refine_ls_number_reflns 2885 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0468 _refine_ls_wR_factor_gt 0.0463 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.003 _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 S S 0.07826(3) 0.19556(2) 0.378818(8) 0.02260(3) Uani 1 d . . . N N 0.41622(10) 0.55623(7) 0.37728(3) 0.02184(7) Uani 1 d . . . C1 C 0.31429(11) 0.37750(9) 0.41313(3) 0.02006(8) Uani 1 d . . . H11 H 0.3921(18) 0.3599(17) 0.4645(6) 0.030(2) Uiso 1 d . . . C2 C 0.33669(16) 0.62066(11) 0.29782(4) 0.03026(12) Uani 1 d . . . H21 H 0.258(2) 0.7696(18) 0.2993(7) 0.039(3) Uiso 1 d . . . H22 H 0.492(2) 0.615(2) 0.2644(6) 0.042(3) Uiso 1 d . . . H23 H 0.196(2) 0.516(2) 0.2778(6) 0.042(3) Uiso 1 d . . . C3 C 0.62445(12) 0.69899(11) 0.41587(5) 0.03386(13) Uani 1 d . . . H31 H 0.568(2) 0.8559(19) 0.4200(7) 0.045(3) Uiso 1 d . . . H32 H 0.806(2) 0.6923(19) 0.3851(7) 0.047(3) Uiso 1 d . . . H33 H 0.662(2) 0.6406(18) 0.4706(7) 0.040(3) Uiso 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 S 0.02531(5) 0.01885(5) 0.02363(5) -0.00107(4) 0.00172(5) -0.00419(4) N 0.01936(15) 0.01694(13) 0.02921(18) 0.00037(14) 0.0025(2) -0.00021(14) C1 0.02031(19) 0.01737(17) 0.0225(2) 0.00075(15) -0.00097(16) 0.00112(15) C2 0.0446(3) 0.0211(2) 0.0251(2) 0.00359(18) 0.0112(2) 0.0009(2) C3 0.0206(2) 0.0219(2) 0.0590(4) -0.0062(3) -0.0022(2) -0.00242(19) _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 S C1 1.6666(6) . ? N C1 1.3211(7) . ? N C2 1.4556(8) . ? N C3 1.4614(8) . ? C1 H11 0.955(10) . ? C2 H22 0.934(11) . ? C2 H21 0.965(10) . ? C2 H23 0.976(11) . ? C3 H31 0.977(11) . ? C3 H32 1.010(11) . ? C3 H33 1.009(11) . ? 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 N C2 123.19(5) . . ? C1 N C3 120.77(6) . . ? C2 N C3 116.03(5) . . ? N C1 S 127.68(4) . . ? N C1 H11 111.7(6) . . ? S C1 H11 120.6(6) . . ? N C2 H22 110.5(7) . . ? N C2 H21 108.7(7) . . ? H22 C2 H21 110.8(9) . . ? N C2 H23 109.4(7) . . ? H22 C2 H23 108.0(9) . . ? H21 C2 H23 109.3(8) . . ? N C3 H31 114.0(7) . . ? N C3 H32 108.7(7) . . ? H31 C3 H32 108.0(10) . . ? N C3 H33 109.4(6) . . ? H31 C3 H33 108.3(9) . . ? H32 C3 H33 108.3(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.335 _refine_diff_density_min -0.154 _refine_diff_density_rms 0.039 #===============================END=============================== data_csdmf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'N,N-Dimethylformamide' _chemical_formula_moiety ? _chemical_formula_sum 'C3 H7 N O' _chemical_formula_weight 73.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0015 0.0009 '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' 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0056 0.0036 '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 5.9455(9) _cell_length_b 7.0042(10) _cell_length_c 10.4041(19) _cell_angle_alpha 77.238(13) _cell_angle_beta 88.132(14) _cell_angle_gamma 75.280(12) _cell_volume 408.56(11) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 15.45 _cell_measurement_theta_max 20.62 _exptl_crystal_description cylinder _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 160 _exptl_absorpt_coefficient_mu 0.055 _exptl_absorpt_correction_type 'not appl.' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.56086 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'long fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Syntex P2~1~' _diffrn_measurement_method '\w-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 73 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.2 _diffrn_reflns_number 9920 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 30.0 _reflns_number_total 4902 _reflns_number_gt 3459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens P3' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1995)' _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 w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment iso _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4902 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.32890(7) 0.61982(6) 0.11632(4) 0.02498(9) Uani 1 d . . . C1 C 0.18759(8) 0.67672(7) 0.02323(5) 0.01859(8) Uani 1 d . . . H11 H 0.2340(12) 0.6666(11) -0.0672(7) 0.0221(17) Uiso 1 d . . . N1 N -0.04167(7) 0.75373(6) 0.03204(4) 0.01759(7) Uani 1 d . . . C2 C -0.14499(10) 0.77149(10) 0.15863(5) 0.02541(11) Uani 1 d . . . H21 H -0.1978(17) 0.9106(15) 0.1682(9) 0.049(3) Uiso 1 d . . . H22 H -0.2737(17) 0.7128(15) 0.1688(9) 0.048(3) Uiso 1 d . . . H23 H -0.0366(18) 0.6970(15) 0.2269(10) 0.051(3) Uiso 1 d . . . C3 C -0.19487(9) 0.82711(8) -0.08411(5) 0.02112(9) Uani 1 d . . . H31 H -0.2641(13) 0.9701(12) -0.0970(7) 0.0262(19) Uiso 1 d . . . H32 H -0.3159(13) 0.7561(11) -0.0747(7) 0.0270(19) Uiso 1 d . . . H33 H -0.1049(14) 0.8030(12) -0.1627(8) 0.028(2) Uiso 1 d . . . O2 O 0.83027(7) 0.21167(7) 0.34272(4) 0.02745(9) Uani 1 d . . . C4 C 0.62022(8) 0.26785(8) 0.35979(5) 0.01878(9) Uani 1 d . . . H41 H 0.5087(13) 0.3290(12) 0.2864(7) 0.0252(18) Uiso 1 d . . . N2 N 0.51875(6) 0.25245(6) 0.47723(4) 0.01645(7) Uani 1 d . . . C5 C 0.65339(8) 0.16506(8) 0.59959(5) 0.01964(9) Uani 1 d . . . H51 H 0.6418(14) 0.2683(12) 0.6505(8) 0.030(2) Uiso 1 d . . . H52 H 0.5897(13) 0.0564(12) 0.6505(7) 0.0260(18) Uiso 1 d . . . H53 H 0.8130(14) 0.1067(12) 0.5840(8) 0.032(2) Uiso 1 d . . . C6 C 0.26806(8) 0.32025(9) 0.48729(5) 0.02196(9) Uani 1 d . . . H61 H 0.2306(13) 0.4271(11) 0.5343(7) 0.0236(18) Uiso 1 d . . . H62 H 0.2074(13) 0.2087(12) 0.5308(8) 0.0272(19) Uiso 1 d . . . H63 H 0.1973(15) 0.3744(13) 0.4016(8) 0.037(2) Uiso 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 O1 0.02094(16) 0.02608(19) 0.02555(18) -0.00416(15) -0.00613(13) -0.00217(14) C1 0.01854(17) 0.01812(19) 0.01881(18) -0.00426(15) 0.00069(14) -0.00396(14) N1 0.01743(15) 0.02113(18) 0.01366(15) -0.00355(13) 0.00009(12) -0.00409(13) C2 0.0239(2) 0.0352(3) 0.01683(19) -0.00603(19) 0.00473(16) -0.0072(2) C3 0.02128(19) 0.0227(2) 0.01847(19) -0.00393(16) -0.00377(15) -0.00398(16) O2 0.01877(15) 0.0389(2) 0.02190(17) -0.00633(16) 0.00531(12) -0.00330(15) C4 0.01819(17) 0.0219(2) 0.01536(17) -0.00377(15) 0.00010(13) -0.00365(15) N2 0.01240(13) 0.02094(17) 0.01505(14) -0.00386(13) -0.00057(11) -0.00245(12) C5 0.01840(18) 0.0235(2) 0.01573(17) -0.00324(16) -0.00245(14) -0.00352(16) C6 0.01281(16) 0.0276(2) 0.0249(2) -0.00759(18) 0.00060(14) -0.00264(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 O1 C1 1.2309(6) . ? C1 N1 1.3407(6) . ? C1 H11 0.985(7) . ? N1 C2 1.4520(7) . ? N1 C3 1.4537(7) . ? C2 H21 0.971(10) . ? C2 H22 0.949(10) . ? C2 H23 0.942(10) . ? C3 H31 0.962(8) . ? C3 H32 0.965(8) . ? C3 H33 0.985(8) . ? O2 C4 1.2299(6) . ? C4 N2 1.3399(6) . ? C4 H41 0.975(8) . ? N2 C5 1.4524(7) . ? N2 C6 1.4526(6) . ? C5 H51 0.974(8) . ? C5 H52 0.979(8) . ? C5 H53 0.957(8) . ? C6 H61 0.959(8) . ? C6 H62 0.960(8) . ? C6 H63 0.954(8) . ? 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 N1 125.21(5) . . ? O1 C1 H11 122.1(4) . . ? N1 C1 H11 112.7(4) . . ? C1 N1 C2 120.80(4) . . ? C1 N1 C3 121.65(4) . . ? C2 N1 C3 117.53(4) . . ? N1 C2 H21 113.1(6) . . ? N1 C2 H22 108.9(6) . . ? H21 C2 H22 108.7(8) . . ? N1 C2 H23 109.5(6) . . ? H21 C2 H23 109.3(8) . . ? H22 C2 H23 107.0(8) . . ? N1 C3 H31 111.1(4) . . ? N1 C3 H32 109.7(4) . . ? H31 C3 H32 109.3(6) . . ? N1 C3 H33 109.5(5) . . ? H31 C3 H33 108.0(6) . . ? H32 C3 H33 109.1(6) . . ? O2 C4 N2 125.23(4) . . ? O2 C4 H41 122.1(5) . . ? N2 C4 H41 112.7(5) . . ? C4 N2 C5 121.67(4) . . ? C4 N2 C6 121.19(4) . . ? C5 N2 C6 117.13(4) . . ? N2 C5 H51 109.7(4) . . ? N2 C5 H52 108.6(4) . . ? H51 C5 H52 109.1(6) . . ? N2 C5 H53 111.8(5) . . ? H51 C5 H53 110.2(7) . . ? H52 C5 H53 107.4(6) . . ? N2 C6 H61 109.8(4) . . ? N2 C6 H62 109.8(5) . . ? H61 C6 H62 110.7(6) . . ? N2 C6 H63 110.1(5) . . ? H61 C6 H63 107.0(7) . . ? H62 C6 H63 109.4(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.374 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.041 #==============================END===========================