data_global _journal_name_full Phys.Chem.Chem.Phys.(PCCP) _journal_coden_cambridge 1326 loop_ _publ_author_name 'Ewa Kurach' 'David Djurado' 'Jan Rimarcik' 'Aleksandra Kornet' 'Marek Wlostowski' 'Vladimir Lukes' 'Jacques P caut' 'Malgorzata Zagorska' 'Adam Pron' _publ_contact_author 'David Djurado' _publ_contact_author_email david.djurado@cea.fr data_echo15 _database_code_depnum_ccdc_archive 'CCDC 774463' #TrackingRef 'EChO15-CCCD.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3,6-bis(2',2-bi-5-thienyl)-1,2,4,5-tetrazine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 'C18H10N4S4' ; _chemical_formula_sum 'C27 H15 N6 S6' _chemical_formula_weight 615.81 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' 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 'P 1 21/c 1' 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 5.8286(2) _cell_length_b 22.7537(9) _cell_length_c 19.7775(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.418(4) _cell_angle_gamma 90.00 _cell_volume 2615.14(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(2) _cell_measurement_reflns_used 2945 _cell_measurement_theta_min 3.0920 _cell_measurement_theta_max 28.9411 _exptl_crystal_description 'long plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.948 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(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 '\k-geometry diffractometer' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10794 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.1064 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3751 _reflns_number_gt 2146 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -13.00 39.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.1550 77.0000 180.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 2 omega -6.00 43.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.1550 45.0000 90.0000 0.0000 0.0000 49 #__ type_ start__ end____ width___ exp.time_ 3 omega -54.00 -4.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.1550 -45.0000 90.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 4 omega -9.00 32.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.1550 -56.0000 209.0000 0.0000 0.0000 41 #__ type_ start__ end____ width___ exp.time_ 5 omega 4.00 48.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -18.7175 56.0000 171.0000 0.0000 0.0000 44 #__ type_ start__ end____ width___ exp.time_ 6 omega -78.00 -37.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -18.7175 -77.0000 300.0000 0.0000 0.0000 41 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0183P)^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 3751 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0607 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 0.820 _refine_ls_restrained_S_all 0.820 _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 S1 S 0.61889(17) 0.70709(4) 0.46733(4) 0.0371(3) Uani 1 1 d . . . S2 S 0.58196(16) 0.61437(4) 0.65916(4) 0.0257(3) Uani 1 1 d . . . S3 S 0.81396(15) 0.44308(4) 0.96561(4) 0.0260(3) Uani 1 1 d . . . S4 S 1.08829(17) 0.33217(4) 1.13226(4) 0.0328(3) Uani 1 1 d . . . N1 N 0.7113(5) 0.53837(12) 0.77937(13) 0.0243(7) Uani 1 1 d . . . N2 N 1.0553(5) 0.50113(12) 0.73633(13) 0.0239(7) Uani 1 1 d . . . N3 N 1.1011(5) 0.47111(12) 0.79249(14) 0.0248(7) Uani 1 1 d . . . N4 N 0.7572(5) 0.50818(13) 0.83551(13) 0.0254(8) Uani 1 1 d . . . C1 C 0.3888(6) 0.75295(15) 0.45573(17) 0.0328(10) Uani 1 1 d . . . H1 H 0.3641 0.7786 0.4193 0.039 Uiso 1 1 calc R . . C2 C 0.2472(6) 0.74748(16) 0.50576(17) 0.0340(10) Uani 1 1 d . . . H2 H 0.1134 0.7694 0.5078 0.041 Uiso 1 1 calc R . . C3 C 0.3207(6) 0.70536(14) 0.55467(16) 0.0257(9) Uani 1 1 d . . . H3 H 0.2406 0.6965 0.5923 0.031 Uiso 1 1 calc R . . C4 C 0.5209(6) 0.67891(15) 0.54127(15) 0.0218(9) Uani 1 1 d . . . C5 C 0.6573(6) 0.63559(14) 0.57961(16) 0.0238(9) Uani 1 1 d . . . C6 C 0.8509(6) 0.60717(15) 0.56386(16) 0.0278(9) Uani 1 1 d . . . H6 H 0.9163 0.6123 0.5228 0.033 Uiso 1 1 calc R . . C7 C 0.9430(6) 0.56964(14) 0.61475(16) 0.0237(9) Uani 1 1 d . . . H7 H 1.0758 0.5476 0.6112 0.028 Uiso 1 1 calc R . . C8 C 0.8172(6) 0.56876(14) 0.67048(16) 0.0203(9) Uani 1 1 d . . . C9 C 0.8607(6) 0.53492(14) 0.73165(16) 0.0203(9) Uani 1 1 d . . . C10 C 0.9508(6) 0.47681(14) 0.84146(16) 0.0205(9) Uani 1 1 d . . . C11 C 1.0074(6) 0.44557(14) 0.90400(15) 0.0201(9) Uani 1 1 d . . . C12 C 1.2022(6) 0.41465(15) 0.92365(17) 0.0278(9) Uani 1 1 d . . . H12 H 1.3255 0.4106 0.8968 0.033 Uiso 1 1 calc R . . C13 C 1.1975(6) 0.38979(15) 0.98813(16) 0.0280(10) Uani 1 1 d . . . H13 H 1.3176 0.3676 1.0085 0.034 Uiso 1 1 calc R . . C14 C 0.9994(6) 0.40123(14) 1.01820(16) 0.0211(9) Uani 1 1 d . . . C15 C 0.9289(6) 0.38375(13) 1.08346(15) 0.0196(8) Uani 1 1 d . . . C16 C 0.7398(6) 0.40257(13) 1.11616(15) 0.0186(9) Uani 1 1 d . . . H16 H 0.6328 0.4300 1.0986 0.022 Uiso 1 1 calc R . . C17 C 0.7316(6) 0.37454(14) 1.17968(16) 0.0275(10) Uani 1 1 d . . . H17 H 0.6168 0.3821 1.2086 0.033 Uiso 1 1 calc R . . C18 C 0.9027(6) 0.33603(16) 1.19507(15) 0.0294(10) Uani 1 1 d . . . H18 H 0.9183 0.3142 1.2349 0.035 Uiso 1 1 calc R . . S21 S 0.09572(19) 0.69288(4) 0.18182(4) 0.0444(3) Uani 1 1 d . . . S22 S 0.14545(16) 0.61020(4) 0.38163(4) 0.0270(3) Uani 1 1 d . . . N21 N 0.3079(5) 0.53430(12) 0.49860(14) 0.0236(7) Uani 1 1 d . . . N22 N 0.6369(5) 0.49814(13) 0.44788(13) 0.0251(8) Uani 1 1 d . . . C21 C -0.1554(7) 0.73123(16) 0.1724(2) 0.0462(12) Uani 1 1 d . . . H21 H -0.2046 0.7516 0.1332 0.055 Uiso 1 1 calc R . . C22 C -0.2755(7) 0.72885(16) 0.2281(2) 0.0456(12) Uani 1 1 d . . . H22 H -0.4157 0.7477 0.2316 0.055 Uiso 1 1 calc R . . C23 C -0.1638(6) 0.69450(14) 0.28023(16) 0.0251(9) Uani 1 1 d . . . H23 H -0.2227 0.6882 0.3220 0.030 Uiso 1 1 calc R . . C24 C 0.0400(6) 0.67150(15) 0.26270(15) 0.0261(9) Uani 1 1 d . . . C25 C 0.1974(6) 0.63191(14) 0.30052(15) 0.0215(9) Uani 1 1 d . . . C26 C 0.3893(6) 0.60568(15) 0.28046(16) 0.0241(9) Uani 1 1 d . . . H26 H 0.4432 0.6118 0.2380 0.029 Uiso 1 1 calc R . . C27 C 0.4999(6) 0.56848(14) 0.32923(16) 0.0218(9) Uani 1 1 d . . . H27 H 0.6336 0.5476 0.3228 0.026 Uiso 1 1 calc R . . C28 C 0.3871(6) 0.56672(13) 0.38750(16) 0.0203(9) Uani 1 1 d . . . C29 C 0.4468(6) 0.53154(15) 0.44678(16) 0.0204(9) 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 S1 0.0348(7) 0.0404(7) 0.0370(6) 0.0111(5) 0.0095(5) 0.0045(6) S2 0.0260(6) 0.0268(6) 0.0247(5) 0.0015(4) 0.0049(4) 0.0054(5) S3 0.0209(6) 0.0295(6) 0.0275(5) 0.0014(5) 0.0008(4) 0.0021(5) S4 0.0328(7) 0.0337(6) 0.0316(6) 0.0008(5) 0.0013(5) 0.0039(6) N1 0.029(2) 0.0241(19) 0.0195(18) -0.0017(15) 0.0012(15) 0.0045(16) N2 0.029(2) 0.0196(18) 0.0229(18) 0.0016(14) 0.0015(15) 0.0001(17) N3 0.0226(19) 0.0241(19) 0.0278(18) 0.0004(15) 0.0028(15) 0.0010(16) N4 0.025(2) 0.031(2) 0.0198(18) -0.0017(15) 0.0005(15) 0.0046(16) C1 0.033(3) 0.026(2) 0.038(2) 0.0083(19) -0.005(2) 0.000(2) C2 0.031(3) 0.031(2) 0.039(2) 0.004(2) 0.000(2) 0.004(2) C3 0.024(2) 0.022(2) 0.030(2) 0.0088(18) 0.0004(17) 0.004(2) C4 0.025(2) 0.019(2) 0.021(2) -0.0002(17) -0.0025(17) -0.004(2) C5 0.028(2) 0.018(2) 0.025(2) -0.0072(18) 0.0025(18) -0.004(2) C6 0.029(2) 0.026(2) 0.029(2) 0.0000(19) 0.0074(18) 0.003(2) C7 0.021(2) 0.026(2) 0.025(2) 0.0017(18) 0.0055(18) 0.0039(19) C8 0.015(2) 0.015(2) 0.031(2) -0.0002(17) -0.0003(17) 0.0013(18) C9 0.018(2) 0.018(2) 0.024(2) -0.0026(18) -0.0040(19) 0.0006(19) C10 0.019(2) 0.019(2) 0.023(2) -0.0082(18) -0.0015(18) -0.0079(19) C11 0.019(2) 0.023(2) 0.018(2) -0.0004(17) -0.0005(17) 0.0030(19) C12 0.027(3) 0.032(2) 0.025(2) 0.0009(18) 0.0027(18) 0.000(2) C13 0.021(2) 0.033(2) 0.030(2) 0.001(2) -0.0009(19) 0.002(2) C14 0.020(2) 0.014(2) 0.028(2) -0.0017(17) -0.0011(17) -0.0018(18) C15 0.023(2) 0.014(2) 0.020(2) -0.0010(17) -0.0044(17) -0.0028(18) C16 0.026(2) 0.015(2) 0.015(2) -0.0003(16) 0.0031(17) -0.0026(18) C17 0.024(2) 0.026(2) 0.033(2) -0.0106(19) 0.0032(18) 0.007(2) C18 0.034(3) 0.036(3) 0.019(2) -0.0028(18) 0.0063(17) -0.004(2) S21 0.0625(9) 0.0372(7) 0.0318(6) 0.0062(5) -0.0067(5) 0.0056(6) S22 0.0302(6) 0.0269(6) 0.0236(5) 0.0008(5) 0.0003(4) 0.0062(5) N21 0.028(2) 0.0224(18) 0.0200(16) 0.0034(14) -0.0011(15) 0.0051(16) N22 0.024(2) 0.0275(19) 0.0239(18) 0.0022(15) 0.0032(15) 0.0061(16) C21 0.045(3) 0.030(3) 0.059(3) 0.009(2) -0.028(2) 0.002(2) C22 0.027(3) 0.030(3) 0.078(3) 0.011(2) -0.007(2) 0.000(2) C23 0.023(2) 0.019(2) 0.032(2) 0.0092(18) -0.0054(18) -0.004(2) C24 0.033(3) 0.017(2) 0.027(2) 0.0030(18) -0.0055(18) -0.005(2) C25 0.025(2) 0.022(2) 0.017(2) -0.0011(17) -0.0017(17) -0.004(2) C26 0.029(2) 0.025(2) 0.019(2) 0.0031(18) 0.0007(18) -0.005(2) C27 0.018(2) 0.022(2) 0.026(2) -0.0046(18) 0.0017(17) 0.0036(19) C28 0.022(2) 0.017(2) 0.022(2) -0.0003(18) 0.0005(17) -0.0012(19) C29 0.022(2) 0.017(2) 0.023(2) -0.0040(18) 0.0023(18) -0.0003(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 S1 C1 1.701(4) . ? S1 C4 1.733(3) . ? S2 C8 1.720(3) . ? S2 C5 1.734(3) . ? S3 C11 1.724(3) . ? S3 C14 1.727(3) . ? S4 C18 1.711(3) . ? S4 C15 1.742(3) . ? N1 N4 1.316(3) . ? N1 C9 1.335(4) . ? N2 N3 1.314(3) . ? N2 C9 1.367(4) . ? N3 C10 1.361(4) . ? N4 C10 1.333(4) . ? C1 C2 1.342(4) . ? C2 C3 1.405(4) . ? C3 C4 1.357(4) . ? C4 C5 1.444(4) . ? C5 C6 1.357(4) . ? C6 C7 1.395(4) . ? C7 C8 1.370(4) . ? C8 C9 1.440(4) . ? C10 C11 1.443(4) . ? C11 C12 1.367(4) . ? C12 C13 1.397(4) . ? C13 C14 1.364(4) . ? C14 C15 1.440(4) . ? C15 C16 1.388(4) . ? C16 C17 1.413(4) . ? C17 C18 1.345(4) . ? S21 C21 1.702(4) . ? S21 C24 1.727(3) . ? S22 C28 1.718(3) . ? S22 C25 1.727(3) . ? N21 N22 1.310(3) 3_666 ? N21 C29 1.356(4) . ? N22 N21 1.310(3) 3_666 ? N22 C29 1.342(4) . ? C21 C22 1.350(5) . ? C22 C23 1.413(4) . ? C23 C24 1.367(4) . ? C24 C25 1.452(4) . ? C25 C26 1.354(4) . ? C26 C27 1.402(4) . ? C27 C28 1.371(4) . ? C28 C29 1.440(4) . ? 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 S1 C4 91.90(18) . . ? C8 S2 C5 91.78(17) . . ? C11 S3 C14 91.76(17) . . ? C18 S4 C15 91.59(17) . . ? N4 N1 C9 117.7(3) . . ? N3 N2 C9 117.6(3) . . ? N2 N3 C10 116.9(3) . . ? N1 N4 C10 118.0(3) . . ? C2 C1 S1 111.5(3) . . ? C1 C2 C3 113.5(4) . . ? C4 C3 C2 112.9(3) . . ? C3 C4 C5 130.3(3) . . ? C3 C4 S1 110.2(2) . . ? C5 C4 S1 119.4(3) . . ? C6 C5 C4 129.7(3) . . ? C6 C5 S2 110.4(3) . . ? C4 C5 S2 119.9(3) . . ? C5 C6 C7 114.0(3) . . ? C8 C7 C6 112.9(3) . . ? C7 C8 C9 127.8(3) . . ? C7 C8 S2 110.9(3) . . ? C9 C8 S2 121.3(3) . . ? N1 C9 N2 124.6(3) . . ? N1 C9 C8 118.7(3) . . ? N2 C9 C8 116.7(3) . . ? N4 C10 N3 125.1(3) . . ? N4 C10 C11 118.4(3) . . ? N3 C10 C11 116.5(3) . . ? C12 C11 C10 128.9(3) . . ? C12 C11 S3 110.9(3) . . ? C10 C11 S3 120.2(3) . . ? C11 C12 C13 113.2(3) . . ? C14 C13 C12 113.4(3) . . ? C13 C14 C15 130.4(3) . . ? C13 C14 S3 110.7(2) . . ? C15 C14 S3 118.9(3) . . ? C16 C15 C14 128.6(3) . . ? C16 C15 S4 111.0(2) . . ? C14 C15 S4 120.4(3) . . ? C15 C16 C17 110.9(3) . . ? C18 C17 C16 114.8(3) . . ? C17 C18 S4 111.6(3) . . ? C21 S21 C24 91.4(2) . . ? C28 S22 C25 91.49(17) . . ? N22 N21 C29 117.4(3) 3_666 . ? N21 N22 C29 118.9(3) 3_666 . ? C22 C21 S21 112.7(3) . . ? C21 C22 C23 112.3(4) . . ? C24 C23 C22 112.8(3) . . ? C23 C24 C25 129.3(3) . . ? C23 C24 S21 110.9(2) . . ? C25 C24 S21 119.7(3) . . ? C26 C25 C24 128.8(3) . . ? C26 C25 S22 110.7(2) . . ? C24 C25 S22 120.5(3) . . ? C25 C26 C27 114.3(3) . . ? C28 C27 C26 111.8(3) . . ? C27 C28 C29 126.8(3) . . ? C27 C28 S22 111.7(3) . . ? C29 C28 S22 121.4(3) . . ? N22 C29 N21 123.7(3) . . ? N22 C29 C28 118.4(3) . . ? N21 C29 C28 117.9(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.267 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.056