data_(10) _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,5¡¯-Oxy-bis(5-thiatellurocane) Bis(tetrafluoroborate ; _chemical_melting_point 'not measured' _chemical_formula_moiety '(Te (CH2)6 S)2 O1 (BF4)2' _chemical_formula_sum 'C12 H24 B2 F8 O S2 Te2' _chemical_formula_weight 677.25 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'Te' 'Te' -0.5308 1.6751 '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 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5331(8) _cell_length_b 9.0124(8) _cell_length_c 13.0975(11) _cell_angle_alpha 90.00 _cell_angle_beta 109.4920(10) _cell_angle_gamma 90.00 _cell_volume 1060.79(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5605 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 28.19 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.120 _exptl_crystal_density_method none _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 3.016 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_absorpt_correction_T_min 0.6952 _exptl_absorpt_correction_T_max 0.7525 _exptl_special_details ; ? ; _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 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 9120 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4662 _reflns_number_gt 3943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-93 (Sheldrick, 1993)' _computing_publication_material 'SHELXCIF-93 (Sheldrick, 1993)' _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^)+(0.0413P)^2^+0.4797P] 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 na _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_number_reflns 4662 _refine_ls_number_parameters 232 _refine_ls_number_restraints 167 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.226 _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 Te1 Te 0.82667(4) 0.65589(6) 0.14174(3) 0.02690(12) Uani 1 1 d . . . Te2 Te 0.70815(4) 0.66047(6) 0.37780(3) 0.02777(11) Uani 1 1 d . . . S1 S 0.8305(2) 0.6762(3) -0.07178(14) 0.0340(5) Uani 1 1 d . . . S2 S 0.6367(2) 0.7023(2) 0.56688(15) 0.0336(5) Uani 1 1 d . . . O1 O 0.7989(7) 0.5776(6) 0.2745(4) 0.0409(13) Uani 1 1 d . . . C1 C 0.8715(9) 0.4304(8) 0.1125(6) 0.0337(17) Uani 1 1 d . . . H1A H 0.9803 0.4139 0.1421 0.040 Uiso 1 1 calc R . . H1B H 0.8247 0.3649 0.1526 0.040 Uiso 1 1 calc R . . C2 C 0.8167(9) 0.3849(9) -0.0057(6) 0.0362(17) Uani 1 1 d . . . H2A H 0.8460 0.2806 -0.0114 0.043 Uiso 1 1 calc R . . H2B H 0.7067 0.3896 -0.0333 0.043 Uiso 1 1 calc R . . C3 C 0.8765(9) 0.4805(9) -0.0762(6) 0.0348(17) Uani 1 1 d . . . H3A H 0.8355 0.4450 -0.1520 0.042 Uiso 1 1 calc R . . H3B H 0.9861 0.4696 -0.0525 0.042 Uiso 1 1 calc R . . C4 C 0.6288(8) 0.6791(11) -0.1324(6) 0.040(2) Uani 1 1 d . . . H4A H 0.6000 0.7384 -0.1998 0.048 Uiso 1 1 calc R . . H4B H 0.5914 0.5767 -0.1512 0.048 Uiso 1 1 calc R . . C5 C 0.5592(9) 0.7461(10) -0.0535(6) 0.0391(19) Uani 1 1 d . . . H5A H 0.5955 0.8492 -0.0365 0.047 Uiso 1 1 calc R . . H5B H 0.4499 0.7501 -0.0888 0.047 Uiso 1 1 calc R . . C6 C 0.5952(6) 0.6589(13) 0.0511(5) 0.0344(13) Uani 1 1 d . . . H6A H 0.5598 0.5556 0.0340 0.041 Uiso 1 1 calc R . . H6B H 0.5407 0.7030 0.0962 0.041 Uiso 1 1 calc R . . C7 C 0.6842(9) 0.4364(8) 0.4218(6) 0.0338(17) Uani 1 1 d . . . H7A H 0.5812 0.4037 0.3824 0.041 Uiso 1 1 calc R . . H7B H 0.7519 0.3732 0.3975 0.041 Uiso 1 1 calc R . . C8 C 0.7166(9) 0.4103(8) 0.5425(6) 0.0390(18) Uani 1 1 d . . . H8A H 0.8222 0.4340 0.5821 0.047 Uiso 1 1 calc R . . H8B H 0.7006 0.3042 0.5548 0.047 Uiso 1 1 calc R . . C9 C 0.6174(10) 0.5051(9) 0.5874(7) 0.0411(19) Uani 1 1 d . . . H9A H 0.6433 0.4854 0.6659 0.049 Uiso 1 1 calc R . . H9B H 0.5123 0.4759 0.5516 0.049 Uiso 1 1 calc R . . C10 C 0.8276(9) 0.7428(10) 0.6502(6) 0.040(2) Uani 1 1 d . . . H10A H 0.8281 0.8119 0.7090 0.048 Uiso 1 1 calc R . . H10B H 0.8780 0.6501 0.6835 0.048 Uiso 1 1 calc R . . C11 C 0.9102(10) 0.8119(10) 0.5813(7) 0.042(2) Uani 1 1 d . . . H11A H 1.0114 0.8405 0.6284 0.051 Uiso 1 1 calc R . . H11B H 0.8577 0.9032 0.5469 0.051 Uiso 1 1 calc R . . C12 C 0.9224(8) 0.7074(9) 0.4938(6) 0.0387(19) Uani 1 1 d . . . H12A H 0.9696 0.6135 0.5275 0.046 Uiso 1 1 calc R . . H12B H 0.9866 0.7528 0.4565 0.046 Uiso 1 1 calc R . . B1 B 0.7804(15) 0.0307(15) 0.2396(11) 0.038(4) Uiso 0.587(11) 1 d PDU A 1 F1 F 0.7366(10) 0.1585(15) 0.2774(7) 0.066(3) Uiso 0.587(11) 1 d PDU A 1 F2 F 0.8663(12) -0.0557(11) 0.3263(8) 0.055(3) Uiso 0.587(11) 1 d PDU A 1 F3 F 0.6574(12) -0.0603(13) 0.1933(10) 0.054(3) Uiso 0.587(11) 1 d PDU A 1 F4 F 0.8507(14) 0.0756(14) 0.1697(10) 0.096(5) Uiso 0.587(11) 1 d PDU A 1 B1X B 0.762(2) 0.025(2) 0.2637(15) 0.051(8) Uiso 0.413(11) 1 d PDU A 2 F1X F 0.7871(16) 0.1716(17) 0.2407(11) 0.077(5) Uiso 0.413(11) 1 d PDU A 2 F2X F 0.9021(16) -0.0436(17) 0.3015(13) 0.062(5) Uiso 0.413(11) 1 d PDU A 2 F3X F 0.6707(17) -0.0411(17) 0.1690(12) 0.050(5) Uiso 0.413(11) 1 d PDU A 2 F4X F 0.700(2) 0.044(3) 0.3432(16) 0.138(10) Uiso 0.413(11) 1 d PDU A 2 B2 B 0.7034(10) 0.1133(9) 0.7582(7) 0.046(2) Uiso 1 1 d DU B 1 F5 F 0.6266(15) 0.2357(13) 0.7804(12) 0.071(4) Uiso 0.554(13) 1 d PDU B 1 F6 F 0.6409(13) 0.0755(12) 0.6516(7) 0.053(3) Uiso 0.554(13) 1 d PDU B 1 F7 F 0.8434(11) 0.1648(19) 0.7586(10) 0.093(4) Uiso 0.554(13) 1 d PDU B 1 F8 F 0.732(2) 0.0085(17) 0.8336(12) 0.139(7) Uiso 0.554(13) 1 d PDU B 1 F5X F 0.6526(15) 0.2571(12) 0.7562(12) 0.050(4) Uiso 0.446(13) 1 d PDU B 2 F6X F 0.696(3) 0.057(3) 0.6634(15) 0.170(13) Uiso 0.446(13) 1 d PDU B 2 F7X F 0.8408(14) 0.0955(18) 0.8266(13) 0.087(6) Uiso 0.446(13) 1 d PDU B 2 F8X F 0.6046(15) 0.0239(14) 0.7946(10) 0.063(4) Uiso 0.446(13) 1 d PDU B 2 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 Te1 0.0291(2) 0.0276(2) 0.02502(19) -0.0023(4) 0.01036(15) -0.0040(5) Te2 0.0311(2) 0.0279(2) 0.02448(19) 0.0013(4) 0.00947(16) 0.0011(5) S1 0.0374(8) 0.0374(13) 0.0315(8) 0.0015(10) 0.0172(7) 0.0001(10) S2 0.0328(9) 0.0373(12) 0.0331(9) -0.0029(7) 0.0143(8) 0.0000(7) O1 0.057(4) 0.041(3) 0.032(3) 0.006(2) 0.024(3) 0.010(3) C1 0.043(4) 0.031(4) 0.028(4) -0.001(3) 0.013(3) 0.005(3) C2 0.038(4) 0.033(4) 0.037(4) -0.005(3) 0.011(4) 0.002(3) C3 0.035(4) 0.040(4) 0.033(4) -0.006(3) 0.016(3) 0.004(3) C4 0.044(4) 0.037(6) 0.035(4) 0.004(4) 0.008(3) 0.006(4) C5 0.034(4) 0.048(5) 0.032(4) -0.002(3) 0.006(3) 0.009(4) C6 0.031(3) 0.038(3) 0.038(3) -0.002(6) 0.017(3) -0.002(6) C7 0.042(4) 0.025(4) 0.039(4) 0.000(3) 0.020(4) 0.003(3) C8 0.049(5) 0.027(4) 0.045(5) 0.007(3) 0.020(4) -0.002(3) C9 0.052(5) 0.038(5) 0.040(4) 0.003(4) 0.024(4) -0.007(4) C10 0.042(5) 0.047(5) 0.031(4) -0.009(3) 0.013(4) -0.005(4) C11 0.041(5) 0.048(5) 0.039(5) -0.009(4) 0.014(4) -0.014(4) C12 0.030(4) 0.052(5) 0.034(4) 0.003(3) 0.010(3) -0.006(3) _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 Te1 O1 1.974(5) . ? Te1 C6 2.129(6) . ? Te1 C1 2.138(7) . ? Te1 S1 2.8147(17) . ? Te1 Te2 3.6290(6) . ? Te2 O1 1.980(5) . ? Te2 C7 2.133(7) . ? Te2 C12 2.142(7) . ? Te2 S2 2.8046(19) . ? S1 C4 1.818(8) . ? S1 C3 1.824(8) . ? S2 C9 1.816(8) . ? S2 C10 1.819(8) . ? C1 C2 1.516(9) . ? C2 C3 1.507(11) . ? C4 C5 1.526(11) . ? C5 C6 1.516(10) . ? C7 C8 1.524(10) . ? C8 C9 1.530(11) . ? C10 C11 1.515(11) . ? C11 C12 1.518(11) . ? B1 F4 1.364(14) . ? B1 F1 1.373(14) . ? B1 F3 1.393(13) . ? B1 F2 1.395(13) . ? B1X F4X 1.372(16) . ? B1X F1X 1.391(17) . ? B1X F3X 1.391(15) . ? B1X F2X 1.402(15) . ? B2 F8 1.327(13) . ? B2 F6 1.366(11) . ? B2 F5 1.407(12) . ? B2 F7 1.411(12) . ? 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 Te1 C6 94.4(2) . . ? O1 Te1 C1 84.9(3) . . ? C6 Te1 C1 98.3(4) . . ? O1 Te1 S1 161.45(18) . . ? C6 Te1 S1 78.45(16) . . ? C1 Te1 S1 79.3(2) . . ? O1 Te1 Te2 23.44(16) . . ? C6 Te1 Te2 85.15(16) . . ? C1 Te1 Te2 107.5(2) . . ? S1 Te1 Te2 163.06(4) . . ? O1 Te2 C7 86.4(3) . . ? O1 Te2 C12 91.6(3) . . ? C7 Te2 C12 99.1(3) . . ? O1 Te2 S2 160.85(16) . . ? C7 Te2 S2 79.0(2) . . ? C12 Te2 S2 78.6(2) . . ? O1 Te2 Te1 23.36(16) . . ? C7 Te2 Te1 108.1(2) . . ? C12 Te2 Te1 96.4(2) . . ? S2 Te2 Te1 172.02(5) . . ? C4 S1 C3 103.3(4) . . ? C4 S1 Te1 94.1(2) . . ? C3 S1 Te1 93.0(2) . . ? C9 S2 C10 103.8(4) . . ? C9 S2 Te2 93.7(3) . . ? C10 S2 Te2 93.9(2) . . ? Te1 O1 Te2 133.2(3) . . ? C2 C1 Te1 114.8(5) . . ? C3 C2 C1 113.6(7) . . ? C2 C3 S1 112.9(5) . . ? C5 C4 S1 110.2(5) . . ? C6 C5 C4 112.8(7) . . ? C5 C6 Te1 113.0(5) . . ? C8 C7 Te2 115.1(5) . . ? C7 C8 C9 112.0(7) . . ? C8 C9 S2 112.6(5) . . ? C11 C10 S2 109.9(6) . . ? C10 C11 C12 112.4(7) . . ? C11 C12 Te2 111.3(5) . . ? F4 B1 F1 105.7(11) . . ? F4 B1 F3 114.4(12) . . ? F1 B1 F3 109.7(11) . . ? F4 B1 F2 115.2(12) . . ? F1 B1 F2 110.0(11) . . ? F3 B1 F2 101.9(11) . . ? F4X B1X F1X 101.1(16) . . ? F4X B1X F3X 115.4(16) . . ? F1X B1X F3X 108.4(15) . . ? F4X B1X F2X 112.9(16) . . ? F1X B1X F2X 106.6(14) . . ? F3X B1X F2X 111.4(15) . . ? F8 B2 F6 119.6(10) . . ? F8 B2 F5 113.4(12) . . ? F6 B2 F5 109.1(9) . . ? F8 B2 F7 105.7(11) . . ? F6 B2 F7 100.1(10) . . ? F5 B2 F7 107.4(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 C6 Te1 Te2 O1 113.0(5) . . . . ? C1 Te1 Te2 O1 15.8(5) . . . . ? S1 Te1 Te2 O1 127.4(5) . . . . ? O1 Te1 Te2 C7 -22.7(5) . . . . ? C6 Te1 Te2 C7 90.3(4) . . . . ? C1 Te1 Te2 C7 -6.9(3) . . . . ? S1 Te1 Te2 C7 104.7(3) . . . . ? O1 Te1 Te2 C12 79.1(5) . . . . ? C6 Te1 Te2 C12 -167.9(4) . . . . ? C1 Te1 Te2 C12 94.9(3) . . . . ? S1 Te1 Te2 C12 -153.5(3) . . . . ? O1 Te1 Te2 S2 130.2(5) . . . . ? C6 Te1 Te2 S2 -116.8(4) . . . . ? C1 Te1 Te2 S2 146.0(4) . . . . ? S1 Te1 Te2 S2 -102.4(4) . . . . ? O1 Te1 S1 C4 69.3(6) . . . . ? C6 Te1 S1 C4 0.6(5) . . . . ? C1 Te1 S1 C4 101.4(4) . . . . ? Te2 Te1 S1 C4 -14.1(4) . . . . ? O1 Te1 S1 C3 -34.3(6) . . . . ? C6 Te1 S1 C3 -103.1(4) . . . . ? C1 Te1 S1 C3 -2.2(3) . . . . ? Te2 Te1 S1 C3 -117.7(3) . . . . ? O1 Te2 S2 C9 -42.6(6) . . . . ? C7 Te2 S2 C9 -1.3(4) . . . . ? C12 Te2 S2 C9 -103.0(4) . . . . ? Te1 Te2 S2 C9 -155.2(4) . . . . ? O1 Te2 S2 C10 61.5(6) . . . . ? C7 Te2 S2 C10 102.8(4) . . . . ? C12 Te2 S2 C10 1.0(4) . . . . ? Te1 Te2 S2 C10 -51.1(4) . . . . ? C6 Te1 O1 Te2 -66.9(5) . . . . ? C1 Te1 O1 Te2 -164.9(5) . . . . ? S1 Te1 O1 Te2 -133.3(4) . . . . ? C7 Te2 O1 Te1 158.5(5) . . . . ? C12 Te2 O1 Te1 -102.6(4) . . . . ? S2 Te2 O1 Te1 -161.1(2) . . . . ? O1 Te1 C1 C2 144.7(6) . . . . ? C6 Te1 C1 C2 50.9(6) . . . . ? S1 Te1 C1 C2 -25.5(5) . . . . ? Te2 Te1 C1 C2 138.4(5) . . . . ? Te1 C1 C2 C3 56.3(8) . . . . ? C1 C2 C3 S1 -58.2(8) . . . . ? C4 S1 C3 C2 -65.3(6) . . . . ? Te1 S1 C3 C2 29.7(6) . . . . ? C3 S1 C4 C5 122.4(6) . . . . ? Te1 S1 C4 C5 28.3(6) . . . . ? S1 C4 C5 C6 -60.7(9) . . . . ? C4 C5 C6 Te1 63.2(9) . . . . ? O1 Te1 C6 C5 167.1(6) . . . . ? C1 Te1 C6 C5 -107.4(7) . . . . ? S1 Te1 C6 C5 -30.2(6) . . . . ? Te2 Te1 C6 C5 145.5(7) . . . . ? O1 Te2 C7 C8 140.1(6) . . . . ? C12 Te2 C7 C8 49.0(6) . . . . ? S2 Te2 C7 C8 -27.4(5) . . . . ? Te1 Te2 C7 C8 148.9(5) . . . . ? Te2 C7 C8 C9 57.7(8) . . . . ? C7 C8 C9 S2 -58.0(8) . . . . ? C10 S2 C9 C8 -65.5(7) . . . . ? Te2 S2 C9 C8 29.4(6) . . . . ? C9 S2 C10 C11 123.8(6) . . . . ? Te2 S2 C10 C11 29.0(6) . . . . ? S2 C10 C11 C12 -63.1(8) . . . . ? C10 C11 C12 Te2 65.4(8) . . . . ? O1 Te2 C12 C11 165.3(6) . . . . ? C7 Te2 C12 C11 -108.0(6) . . . . ? S2 Te2 C12 C11 -31.3(5) . . . . ? Te1 Te2 C12 C11 142.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.103 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.122