#------------------------------------------------------------------------------ #$Date: 2024-07-28 01:36:44 +0300 (Sun, 28 Jul 2024) $ #$Revision: 293571 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/91/7249123.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7249123 loop_ _publ_author_name 'D'Agostino, Simone' 'Ocak, Samet' 'Braga, Dario' _publ_section_title ; Effect of Supramolecular Complexation of Alkali Hydrogenselenates with Crown Ethers and solid-solutions with their Hydrogensulfate Counterparts on the Solid-to-Solid Phase Transition Behaviors ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00514G _journal_year 2024 _chemical_formula_moiety 'C12 H25 K O10 S0.5 Se0.5' _chemical_formula_sum 'C12 H25 K O10 S0.5 Se0.5' _chemical_formula_weight 423.93 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-04-16 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.684(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3093(8) _cell_length_b 8.5230(6) _cell_length_c 21.5977(15) _cell_measurement_reflns_used 956 _cell_measurement_temperature 295 _cell_measurement_theta_max 19.5320 _cell_measurement_theta_min 2.0720 _cell_volume 1870.7(2) _computing_cell_refinement 'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro system (CCD 42.85a 64-bit (release 03-03-2023))' _computing_data_reduction 'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2016/6 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 295 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1385 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.825 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -51.00 15.00 1.00 125.00 -- -16.52 -19.00-120.00 66 2 \w -33.00 88.00 1.00 125.00 -- 17.46 0.00 -30.00 121 3 \w 63.00 90.00 1.00 125.00 -- 17.46 178.00 150.00 27 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0555814000 _diffrn_orient_matrix_UB_12 0.0476209000 _diffrn_orient_matrix_UB_13 0.0019314000 _diffrn_orient_matrix_UB_21 0.0149722000 _diffrn_orient_matrix_UB_22 0.0473670000 _diffrn_orient_matrix_UB_23 -0.0248796000 _diffrn_orient_matrix_UB_31 -0.0395002000 _diffrn_orient_matrix_UB_32 -0.0490776000 _diffrn_orient_matrix_UB_33 -0.0220887000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_unetI/netI 0.2040 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.825 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 8510 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.825 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.521 _diffrn_reflns_theta_min 2.070 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.96077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.117a (Rigaku Oxford Diffraction, 2024) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.505 _exptl_crystal_description block _exptl_crystal_F_000 884 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.312 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 268 _refine_ls_number_reflns 4312 _refine_ls_number_restraints 471 _refine_ls_restrained_S_all 0.953 _refine_ls_R_factor_all 0.2703 _refine_ls_R_factor_gt 0.0800 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1083 _refine_ls_wR_factor_ref 0.1624 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1396 _reflns_number_total 4312 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00514g2.cif _cod_data_source_block K-Se-S_sol-sod _cod_original_formula_sum 'C12 H25 K O10 S0.50 Se0.50' _cod_database_code 7249123 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula 'C12 O10 S0.5 Se0.5 K1 H25 ' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.960 _shelx_estimated_absorpt_t_min 0.935 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All O(H) groups 2. Restrained distances O006-H006 0.85 with sigma of 0.01 O11-H11 0.85 with sigma of 0.01 Se1-H006 2.072321 with sigma of 0.02 K002-H006 3.612806 with sigma of 0.02 S1-H11 1.969188 with sigma of 0.02 K002-H11 3.688742 with sigma of 0.02 3. Rigid body (RIGU) restrains C1, H1A, H1B, C2, O6, H2A, H2B, O1, C12, K002, C3, C11, H12A, H12B, O5, O13, O3, O12, O006, O11, O4, O2, Se1, S1, H3A, H3B, C4, H11A, H11B, C10, C6, C7, H006, H11, C8, C9, C5, O8, O9, O7, O10, H4A, H4B, H10A, H10B, H6A, H6B, H7A, H7B, H8A, H8B, H9A, H9B, H5A, H5B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Fixed Sof: O006(0.5) H006(0.5) O7(0.5) O8(0.5) O9(0.5) O10(0.5) O11(0.5) H11(0.5) O12(0.5) O13(0.5) S1(0.5) Se1(0.5) 5.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B) ; _shelx_res_file ; TITL k_solsol_s_se_rt_r2_a.res in P2(1)/n k_solsol_s_se_rt_r2.res created by SHELXL-2016/6 at 11:46:13 on 16-Apr-2024 REM Old TITL K_solsol_S_Se_RT_R2 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.269, Rweak 0.119, Alpha 0.081, Orientation as input REM Formula found by SHELXT: C12 O10 K Se CELL 0.71073 10.3093 8.523 21.5977 90 99.684 90 ZERR 4 0.0008 0.0006 0.0015 0 0.007 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H K O S Se UNIT 48 100 4 40 2 2 DFIX 0.85 0.01 O006 H006 DANG 2.072321 0.02 Se1 H006 DANG 3.612806 0.02 K002 H006 DFIX 0.85 0.01 O11 H11 DANG 1.969188 0.02 S1 H11 DANG 3.688742 0.02 K002 H11 RIGU C1 H1a H1b C2 O6 H2a H2b O1 C12 K002 C3 C11 H12a H12b O5 O13 O3 O12 = O006 O11 O4 O2 SE1 S1 H3A H3B C4 H11A H11B C10 C6 C7 H006 H11 C8 C9 C5 O8 = O9 O7 O10 H4A H4B H10A H10B H6A H6B H7A H7B H8A H8B H9A H9B H5A H5B L.S. 200 PLAN 5 SIZE 0.05 0.04 0.03 TEMP 21.85 CONF BOND $H list 4 MORE -1 fmap 2 53 acta 50 REM REM REM WGHT 0.037500 FVAR 0.41470 C1 1 1.007768 0.949624 0.357161 11.00000 0.07124 0.11659 = 0.13890 -0.06539 0.03033 -0.03877 AFIX 23 H1A 2 1.097633 0.968654 0.351233 11.00000 -1.20000 H1B 2 0.994991 0.998068 0.396328 11.00000 -1.20000 AFIX 0 C2 1 0.912937 1.017539 0.303310 11.00000 0.12301 0.10036 = 0.12612 -0.04974 0.05008 -0.04227 AFIX 23 H2A 2 0.934481 1.126932 0.297915 11.00000 -1.20000 H2B 2 0.921773 0.962226 0.264989 11.00000 -1.20000 AFIX 0 C3 1 0.693713 1.082484 0.264921 11.00000 0.18591 0.06988 = 0.06243 0.01724 -0.01222 -0.02562 AFIX 23 H3A 2 0.695766 1.034484 0.224375 11.00000 -1.20000 H3B 2 0.714810 1.192918 0.262216 11.00000 -1.20000 AFIX 0 C4 1 0.561454 1.064120 0.282136 11.00000 0.17250 0.09462 = 0.08945 0.00897 -0.02395 0.00927 AFIX 23 H4A 2 0.562398 1.105351 0.324071 11.00000 -1.20000 H4B 2 0.498146 1.124295 0.253265 11.00000 -1.20000 AFIX 0 C5 1 0.394817 0.895891 0.296293 11.00000 0.09729 0.13903 = 0.11765 -0.01483 0.01994 0.04220 AFIX 23 H5A 2 0.330792 0.951106 0.265957 11.00000 -1.20000 H5B 2 0.392676 0.940329 0.337455 11.00000 -1.20000 AFIX 0 C6 1 0.361179 0.729978 0.296334 11.00000 0.06892 0.16454 = 0.13453 -0.04231 0.01868 0.01381 AFIX 23 H6A 2 0.272941 0.717192 0.305614 11.00000 -1.20000 H6B 2 0.363708 0.684917 0.255312 11.00000 -1.20000 AFIX 0 C7 1 0.413584 0.494347 0.350002 11.00000 0.08989 0.16377 = 0.16640 -0.01507 0.05969 -0.05867 AFIX 23 H7A 2 0.409297 0.435569 0.311252 11.00000 -1.20000 H7B 2 0.328047 0.489468 0.362971 11.00000 -1.20000 AFIX 0 C8 1 0.514764 0.426449 0.399161 11.00000 0.17664 0.12566 = 0.11024 -0.02143 0.05321 -0.06907 AFIX 23 H8A 2 0.519382 0.487457 0.437384 11.00000 -1.20000 H8B 2 0.489716 0.320188 0.408095 11.00000 -1.20000 AFIX 0 C9 1 0.731365 0.337742 0.425655 11.00000 0.22236 0.08494 = 0.06193 0.03333 -0.01691 -0.04114 AFIX 23 H9A 2 0.710196 0.226769 0.423677 11.00000 -1.20000 H9B 2 0.730305 0.373995 0.468140 11.00000 -1.20000 AFIX 0 C10 1 0.861759 0.362673 0.409236 11.00000 0.20684 0.07627 = 0.08801 0.01597 -0.01377 0.03018 AFIX 23 H10A 2 0.925619 0.299351 0.436495 11.00000 -1.20000 H10B 2 0.861159 0.328608 0.366336 11.00000 -1.20000 AFIX 0 C11 1 1.033174 0.540254 0.408045 11.00000 0.10014 0.16425 = 0.08927 0.00406 -0.00242 0.06232 AFIX 23 H11A 2 1.050138 0.496161 0.368779 11.00000 -1.20000 H11B 2 1.091995 0.490756 0.442256 11.00000 -1.20000 AFIX 0 C12 1 1.055524 0.710938 0.408935 11.00000 0.06644 0.18477 = 0.10061 -0.01898 0.00708 0.02348 AFIX 23 H12A 2 1.032973 0.754886 0.447170 11.00000 -1.20000 H12B 2 1.147923 0.731862 0.408690 11.00000 -1.20000 AFIX 0 K002 3 0.712183 0.748218 0.378700 11.00000 0.06565 0.06614 = 0.06534 0.00024 0.01490 -0.00199 O1 4 0.788856 1.006663 0.313031 11.00000 0.11660 0.07895 = 0.08497 -0.00291 0.03511 -0.02172 O2 4 0.524809 0.915399 0.280452 11.00000 0.11544 0.08368 = 0.08301 -0.00725 0.00307 0.01801 O3 4 0.448472 0.656386 0.340226 11.00000 0.07365 0.15226 = 0.09547 -0.01733 0.01705 -0.00714 O4 4 0.634447 0.424322 0.381615 11.00000 0.14080 0.08843 = 0.07354 0.00579 0.01875 -0.03996 O5 4 0.897739 0.512666 0.414740 11.00000 0.12551 0.08417 = 0.07716 -0.00792 -0.00618 0.02091 O6 4 0.982569 0.779835 0.358983 11.00000 0.07143 0.13026 = 0.08117 -0.03586 0.00048 -0.00557 PART 1 O006 4 0.587685 0.800790 0.485507 10.50000 0.06251 0.08535 = 0.08030 -0.00388 0.01129 -0.00559 H006 2 0.514665 0.811027 0.498705 10.50000 -1.50000 PART 2 O7 4 0.752763 0.798572 0.581431 10.50000 0.07560 0.14656 = 0.11580 0.06003 -0.00161 -0.01387 PART 1 O8 4 0.700722 0.845545 0.592140 10.50000 0.10465 0.10844 = 0.07730 -0.01954 0.03588 -0.03470 O9 4 0.649145 1.058738 0.549628 10.50000 0.09123 0.11556 = 0.09046 -0.04643 -0.00438 0.02072 PART 2 O10 4 0.660182 1.087546 0.523128 10.50000 0.08612 0.06666 = 0.08569 0.02074 0.02291 -0.03460 O11 4 0.572694 0.838919 0.475870 10.50000 0.06466 0.09438 = 0.09459 -0.02478 0.00225 -0.00229 H11 2 0.506756 0.872760 0.491637 10.50000 -1.50000 PART 1 O12 4 0.800636 0.935104 0.483210 10.50000 0.09280 0.09198 = 0.09587 -0.00851 0.04383 -0.01599 PART 2 O13 4 0.823148 0.873793 0.499364 10.50000 0.06575 0.12563 = 0.08606 -0.01168 0.01575 -0.00976 S1 5 0.693569 0.908047 0.525116 10.50000 0.06151 0.07128 = 0.06616 0.01343 0.01812 -0.03745 PART 1 SE1 6 0.702177 0.898427 0.526750 10.50000 0.06067 0.08099 = 0.06861 -0.02066 0.01269 -0.00781 HKLF 4 REM k_solsol_s_se_rt_r2_a.res in P2(1)/n REM R1 = 0.0800 for 1396 Fo > 4sig(Fo) and 0.2703 for all 4312 data REM 268 parameters refined using 471 restraints END WGHT 0.0378 0.0000 REM Highest difference peak 0.312, deepest hole -0.214, 1-sigma level 0.060 Q1 1 0.6321 0.9358 0.2820 11.00000 0.05 0.31 Q2 1 0.7991 1.0442 0.2594 11.00000 0.05 0.29 Q3 1 0.5773 0.5351 0.3748 11.00000 0.05 0.27 Q4 1 0.8707 0.9659 0.3444 11.00000 0.05 0.25 Q5 1 1.0111 0.9415 0.3379 11.00000 0.05 0.24 ; _shelx_res_checksum 87957 _shelx_hkl_file ; 0 0 -3 0.08 3.24 0 0 3 -1.20 2.67 0 0 4 414.83 16.49 0 0 4 412.61 17.21 0 0 -4 425.69 17.00 0 0 5 1.73 4.14 0 0 5 -2.91 4.18 0 0 -5 -3.43 5.14 0 0 -6 9.09 5.66 0 0 6 18.42 6.33 0 0 6 4.73 4.46 0 0 7 3.64 6.52 0 0 -7 -2.60 6.67 0 0 7 -0.99 7.03 0 0 8 680.29 30.72 0 0 8 718.65 30.13 0 0 -8 714.81 31.94 0 0 -9 -7.35 7.82 0 0 9 2.29 6.22 0 0 9 4.02 5.97 0 0 -10 559.35 32.50 0 0 10 557.89 31.18 0 0 10 605.30 30.87 0 0 11 1.43 6.12 0 0 11 -2.33 7.55 0 0 -11 -0.54 7.67 0 0 12 117.14 15.52 0 0 12 124.81 17.36 0 0 -12 119.25 17.00 0 0 13 -1.29 5.14 0 0 -13 -7.15 10.04 0 0 14 35.24 10.78 0 0 -14 9.31 7.47 0 0 15 2.16 6.15 0 0 -15 -9.53 8.35 0 0 -16 126.25 21.35 0 0 -17 -8.10 10.91 0 0 -17 -15.96 10.07 0 0 -18 120.76 24.59 0 0 -18 124.08 22.11 0 0 -19 4.46 10.62 0 0 -19 -9.70 9.87 0 0 -20 135.83 24.87 0 0 -20 135.49 26.71 0 0 -21 2.41 10.61 0 0 -21 15.74 12.38 0 0 -22 8.91 11.34 0 0 -22 37.22 17.00 0 0 -23 -7.70 12.21 0 0 -23 -8.00 12.38 0 0 -24 -3.62 9.21 0 0 -24 -7.80 12.16 0 0 -25 -13.67 12.61 0 0 -25 2.60 9.69 0 0 -26 -14.25 16.00 0 0 -27 2.72 12.36 0 0 -28 -14.90 19.42 0 -1 0 -0.13 2.39 0 1 0 4.73 3.27 0 1 1 740.93 16.94 0 -1 1 725.05 21.12 0 1 -1 757.00 21.15 0 -1 2 1075.91 28.48 0 1 -2 1074.28 28.02 0 1 -3 780.82 26.44 0 1 3 777.60 24.71 0 1 3 726.74 18.62 0 -1 3 752.23 25.73 0 -1 -4 1394.45 28.10 0 1 -4 1348.38 37.91 0 -1 4 1464.89 38.95 0 1 4 1417.06 28.05 0 1 4 1457.75 37.26 0 1 -5 9653.67 107.61 0 1 5 9922.37 104.07 0 -1 5 9728.58 108.36 0 -1 -5 9888.79 82.47 0 -1 -5 9960.80 61.06 0 -1 -5 9999.00 105.03 0 1 5 9888.39 63.26 0 1 5 9889.02 81.93 0 1 6 683.70 24.15 0 -1 6 662.14 30.70 0 1 -6 670.26 31.57 0 -1 -6 695.37 31.11 0 -1 -6 679.54 24.34 0 1 6 688.17 19.27 0 1 6 744.40 30.80 0 1 7 15.23 5.21 0 -1 -7 12.82 6.00 0 -1 -7 10.07 8.99 0 1 7 10.05 5.34 0 1 -7 25.65 10.38 0 -1 7 6.75 6.33 0 -1 -8 54.44 12.44 0 1 8 54.11 7.72 0 -1 -8 40.03 7.19 0 1 8 48.62 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13.77 11 -2 0 46.42 22.38 11 2 1 -10.86 12.75 11 -2 1 6.51 14.22 11 2 2 32.79 15.37 11 -2 2 5.73 15.42 -11 2 -2 4.09 7.50 11 2 3 39.46 19.66 -11 2 -3 -1.01 10.67 11 -2 3 3.15 12.72 -11 2 -3 6.19 11.93 11 2 4 21.32 15.55 -11 2 -4 27.39 16.01 -11 2 -4 -5.29 11.52 11 2 5 25.76 18.73 -11 2 -5 13.30 12.07 -11 2 -5 5.62 12.22 11 2 6 8.02 11.26 -11 2 -6 9.53 12.67 -11 2 -6 16.82 15.78 -11 2 -7 -0.16 10.40 -11 2 -7 2.25 10.31 -11 2 -8 -10.51 13.08 -11 2 -8 -4.51 13.44 -11 2 -9 3.70 10.41 -11 2 -9 -27.15 19.59 -11 2 -10 43.60 22.75 -11 2 -11 -14.28 18.64 11 -3 -18 -14.82 13.14 11 -3 -17 -0.68 13.06 11 -3 -16 2.32 16.01 11 3 -15 46.40 23.73 11 -3 -15 11.73 19.14 11 -3 -14 -13.96 12.91 11 3 -14 -4.25 18.14 11 -3 -13 -14.79 16.69 11 3 -13 -1.21 13.46 11 -3 -12 15.05 14.65 11 3 -12 15.34 15.84 11 -3 -11 -11.15 13.09 11 3 -11 -13.16 18.03 11 -3 -10 -16.19 15.75 11 3 -10 17.79 13.12 11 -3 -9 34.11 23.13 11 3 -9 22.31 18.01 11 -3 -8 45.15 24.30 11 3 -8 14.51 16.31 11 -3 -7 14.16 17.06 11 3 -7 10.40 13.46 11 3 -6 7.37 13.30 11 -3 -6 -14.71 16.03 11 3 -5 -1.54 11.16 11 -3 -5 63.68 26.22 11 3 -4 -5.57 12.93 11 -3 -4 13.96 14.90 11 -3 -3 29.65 19.62 11 3 -3 64.30 24.03 11 -3 -2 5.42 11.52 11 3 -2 -11.63 10.10 11 -3 -1 45.43 18.44 11 3 -1 29.18 16.86 11 -3 0 28.04 19.23 11 3 0 -13.71 14.64 11 3 1 -9.44 13.05 -11 3 -2 -4.87 16.93 11 3 2 33.53 14.91 -11 3 -2 6.17 10.65 -11 3 -3 42.50 20.80 11 3 3 51.21 18.32 -11 3 -3 13.49 12.57 -11 3 -4 26.92 19.82 11 3 4 18.22 14.37 -11 3 -4 -1.75 10.06 -11 3 -5 9.85 11.95 11 3 5 23.29 14.90 -11 3 -5 13.61 14.26 -11 3 -6 6.87 11.05 -11 3 -6 24.36 14.06 -11 3 -7 -5.55 12.71 -11 3 -7 -18.82 15.58 -11 3 -8 12.46 13.05 -11 3 -8 13.67 14.47 -11 3 -9 24.45 15.15 -11 3 -9 7.49 15.19 -11 3 -10 33.76 17.23 -11 3 -10 -4.81 11.60 -11 3 -11 -12.40 15.44 11 -4 -16 7.50 15.44 11 -4 -15 32.18 23.12 11 -4 -14 -8.80 15.89 11 -4 -13 1.42 16.24 11 4 -13 17.04 16.31 11 -4 -12 -3.31 12.49 11 4 -12 4.83 12.87 11 4 -11 33.84 16.54 11 -4 -11 7.32 12.83 11 -4 -10 11.12 16.26 11 4 -10 -7.93 15.26 11 -4 -9 39.13 24.76 11 4 -9 4.31 13.27 11 4 -8 41.53 20.05 11 -4 -8 -29.52 21.31 11 4 -7 16.65 16.60 11 -4 -7 -0.81 14.55 11 4 -6 29.02 20.56 11 -4 -6 41.39 21.48 11 4 -5 4.54 15.73 11 -4 -5 14.79 13.19 11 4 -4 4.43 10.59 11 -4 -4 54.24 24.27 11 4 -3 7.70 11.32 11 -4 -3 46.38 20.78 11 4 -2 -5.40 11.47 11 4 -1 4.81 12.01 11 4 0 16.77 13.85 -11 4 0 11.48 15.06 11 4 1 21.16 14.24 -11 4 -1 22.46 18.22 11 4 2 20.27 14.31 -11 4 -2 -1.51 11.72 -11 4 -3 5.06 12.86 -11 4 -4 -9.07 14.82 -11 4 -4 -8.09 9.38 -11 4 -5 -19.53 19.96 -11 4 -5 14.32 13.11 -11 4 -6 -3.90 11.60 -11 4 -6 8.82 13.38 -11 4 -7 -14.15 17.31 -11 4 -7 12.80 11.59 -11 4 -8 -2.33 11.61 -11 4 -8 17.30 17.95 -11 4 -9 -27.45 17.30 -11 4 -9 8.04 12.03 -11 4 -10 32.13 18.62 -11 4 -10 -14.52 13.81 11 -5 -13 -50.32 23.84 11 -5 -12 -40.58 27.92 11 -5 -11 18.99 16.10 11 5 -11 -22.74 17.58 11 -5 -10 14.00 17.74 11 5 -10 24.53 18.41 11 5 -9 -15.27 15.60 11 -5 -9 -36.12 22.86 11 5 -8 36.94 21.55 11 -5 -8 6.52 14.68 11 5 -7 -3.48 12.54 11 -5 -7 -0.54 13.47 11 5 -6 -5.47 12.32 11 -5 -6 0.07 15.50 11 5 -5 -1.39 12.11 11 -5 -5 2.21 18.03 11 5 -4 -21.84 18.04 11 -5 -4 9.76 20.51 11 5 -3 -2.26 11.86 -11 5 2 16.48 16.41 11 5 -2 -6.44 10.01 -11 5 1 -15.96 11.71 11 5 -1 16.22 15.00 -11 5 0 17.70 20.23 11 5 0 -3.32 12.67 -11 5 -1 -12.88 17.51 -11 5 -2 15.06 16.00 -11 5 -3 -7.46 12.38 -11 5 -4 -20.06 17.30 -11 5 -5 -2.93 12.53 -11 5 -6 -1.49 8.90 -11 5 -7 10.10 14.65 -11 5 -8 -13.42 12.00 11 6 -13 -18.43 18.42 11 6 -9 -2.98 15.89 11 6 -8 42.67 19.01 11 6 -7 11.85 14.76 11 6 -6 7.42 13.51 11 6 -5 4.06 13.06 11 6 -4 23.68 15.96 11 6 -3 -12.11 13.67 11 6 -2 -21.13 15.68 12 0 -14 13.53 19.53 12 0 -13 -32.40 20.09 12 0 -12 2.55 14.84 12 0 -11 -14.75 13.75 12 0 -10 33.76 19.44 12 0 -9 -13.33 14.60 12 0 -8 27.79 14.76 12 0 -7 18.24 17.77 12 0 -6 -1.68 14.19 12 0 -5 32.27 21.78 12 0 -4 22.53 16.76 12 0 -3 4.75 11.23 12 0 -2 12.83 12.70 12 0 -1 -21.62 19.68 12 0 0 20.75 19.07 12 0 1 27.31 18.75 12 0 2 18.92 14.70 12 0 3 2.79 12.11 12 0 4 25.12 15.58 12 0 5 -1.27 16.05 12 0 6 -21.99 18.65 12 0 7 -2.28 11.37 12 0 8 7.69 15.31 12 1 -13 26.38 17.57 12 -1 -13 11.69 19.32 12 1 -12 7.14 17.38 12 -1 -12 -23.70 18.63 12 -1 -11 20.74 12.72 12 1 -11 -12.75 14.73 12 -1 -10 4.97 14.04 12 1 -10 14.59 13.50 12 -1 -9 9.37 17.93 12 1 -9 23.75 19.01 12 -1 -8 -6.54 16.18 12 1 -8 21.81 18.85 12 -1 -7 -26.57 24.19 12 1 -7 -22.48 21.61 12 -1 -6 3.26 13.60 12 1 -6 8.61 11.78 12 -1 -5 -24.13 19.54 12 1 -5 34.50 21.30 12 -1 -4 -5.61 18.27 12 1 -4 32.80 17.79 12 -1 -3 4.69 13.29 12 1 -3 17.16 16.02 12 -1 -2 -5.38 14.25 12 1 -2 7.03 14.98 12 -1 -1 9.24 11.95 12 1 -1 2.18 13.74 12 -1 0 3.28 12.82 12 1 0 -21.29 17.43 12 -1 1 -8.88 15.85 12 1 1 16.26 16.84 12 1 2 -10.23 17.52 12 -1 2 0.69 12.83 12 1 3 -53.76 21.59 12 -1 3 13.63 16.87 12 1 4 26.03 16.80 -12 1 -4 2.08 12.03 12 -1 4 14.35 11.27 12 1 5 10.68 16.53 -12 1 -5 -13.78 14.73 12 -1 5 4.73 12.43 12 1 6 4.52 10.74 12 -1 6 -22.14 19.50 12 1 7 6.01 10.78 12 -1 7 37.27 20.52 12 -1 8 7.89 12.10 12 -1 9 2.80 15.31 12 -1 10 -12.39 14.79 12 -2 -13 9.94 17.41 12 2 -12 -8.56 12.93 12 -2 -12 -24.21 16.35 12 2 -11 -21.27 18.38 12 -2 -11 39.12 21.02 12 2 -10 0.56 14.78 12 -2 -10 4.73 15.49 12 2 -9 10.63 16.15 12 -2 -9 7.82 15.66 12 -2 -8 -20.90 20.00 12 2 -8 37.72 21.13 12 -2 -7 18.41 18.81 12 2 -7 -2.15 17.91 12 -2 -6 24.59 19.55 12 2 -6 11.03 15.96 12 -2 -5 9.74 14.76 12 2 -5 14.41 17.44 12 -2 -4 -29.23 16.89 12 2 -4 -1.47 13.19 12 -2 -3 36.82 24.50 12 2 -3 4.08 12.24 12 2 -2 -23.19 15.46 12 -2 -2 -10.47 18.20 12 2 -1 4.66 11.56 12 -2 -1 37.57 23.50 12 2 0 22.89 17.68 12 -2 0 -7.86 17.75 12 2 1 -5.95 17.51 12 -2 1 33.35 22.20 12 2 2 19.08 14.05 12 -2 2 1.57 16.69 12 2 3 14.24 14.41 -12 2 -3 -2.49 12.03 12 -2 3 -18.52 19.68 12 2 4 -33.14 19.12 -12 2 -4 13.47 17.21 12 -2 4 6.90 18.97 -12 2 -5 14.13 15.72 12 2 5 6.65 11.58 12 -2 5 23.35 21.35 -12 2 -6 8.83 13.83 12 -2 6 -7.20 15.88 -12 2 -6 16.18 15.48 -12 2 -7 1.33 10.45 12 -2 7 27.87 15.92 -12 2 -7 18.32 16.69 12 -2 8 2.15 15.94 -12 2 -8 -21.27 15.81 -12 2 -9 8.22 14.59 12 -3 -11 36.85 24.90 12 3 -11 16.65 16.24 12 -3 -10 -9.78 13.19 12 3 -10 57.41 24.34 12 -3 -9 -20.64 19.29 12 3 -9 -6.55 15.84 12 -3 -8 2.58 17.95 12 3 -8 -4.88 13.03 12 -3 -7 -16.32 14.39 12 3 -7 6.75 15.65 12 -3 -6 -4.55 16.40 12 3 -6 30.04 16.70 12 -3 -5 4.10 16.24 12 3 -5 -27.61 20.11 12 3 -4 8.54 14.74 12 -3 -4 -22.86 20.77 12 3 -3 -29.15 20.60 12 -3 -3 80.46 33.33 12 -3 -2 -4.29 12.94 12 3 -2 15.15 14.87 12 -3 -1 5.99 18.08 12 3 -1 24.65 21.18 12 -3 0 27.90 20.25 12 3 0 31.30 19.12 -12 3 -1 9.69 15.51 12 -3 1 14.29 15.91 12 3 1 36.79 21.87 -12 3 -2 -8.26 15.52 12 -3 2 24.86 19.84 12 3 2 -6.03 14.45 -12 3 -3 12.20 15.86 12 -3 3 2.49 13.48 12 3 3 2.95 14.16 -12 3 -4 8.45 15.78 -12 3 -5 0.92 10.60 -12 3 -6 18.17 17.96 -12 3 -6 -16.93 16.63 -12 3 -7 -9.59 14.41 -12 3 -7 -16.07 14.47 -12 3 -8 7.38 15.59 -12 3 -8 -4.40 11.29 12 4 -9 26.84 19.76 12 4 -8 13.25 15.06 12 4 -7 -2.10 13.15 12 4 -6 -17.61 16.63 12 4 -5 -6.72 13.56 12 4 -4 -0.83 14.21 12 4 -3 14.09 14.56 12 4 -2 7.04 12.23 12 4 -1 2.30 10.37 12 4 0 21.12 13.20 -12 4 0 -20.10 17.45 12 4 1 -9.85 13.46 -12 4 -1 -28.02 21.87 -12 4 -2 14.90 12.14 -12 4 -3 14.85 11.22 12 5 -7 53.90 22.68 12 5 -6 10.54 14.58 12 5 -5 8.01 13.69 12 5 -4 15.03 17.04 12 5 -3 12.38 13.24 12 5 -2 -3.41 13.53 12 6 -4 4.27 12.66 13 0 -5 21.34 19.18 13 0 -4 9.86 12.74 13 0 -3 -8.47 13.93 13 0 -2 22.79 17.13 13 0 -1 -10.94 13.51 13 0 0 -9.51 13.15 13 0 1 30.28 21.34 13 0 2 -27.24 19.04 13 0 3 -12.77 15.88 13 0 4 24.17 20.83 13 0 5 -35.02 22.45 13 1 -6 -25.94 14.59 13 1 -5 -16.20 13.94 13 1 -4 20.08 12.07 13 1 -3 -2.15 12.45 13 1 -2 -25.54 20.60 13 1 -1 -18.47 15.21 13 1 0 -6.70 17.16 13 1 1 -2.21 12.90 13 1 2 5.47 11.44 13 1 3 -4.13 11.54 -13 1 -3 8.68 12.49 13 1 4 20.98 19.47 13 1 5 31.19 20.21 13 2 -5 50.25 25.82 13 2 -4 39.45 25.19 13 2 -3 -15.35 16.43 13 2 -2 -29.08 20.24 13 2 -1 -23.90 18.16 13 2 0 -2.54 11.65 13 2 1 -0.97 13.19 -13 2 -2 -5.60 14.38 13 2 2 25.41 22.64 -13 2 -3 -29.94 18.07 13 2 3 17.22 16.87 -13 2 -4 15.27 16.45 13 3 -4 6.86 15.50 13 3 -3 26.50 18.38 13 3 -2 -10.98 12.81 13 3 -1 8.83 12.72 13 3 0 4.67 14.12 13 3 1 -11.72 13.32 13 4 -2 -44.31 21.05 13 4 -1 -10.37 14.22 0 0 0 0.00 0.00 TITL K_solsol_S_Se_RT_R2 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 10.309273 8.523017 21.597708 90.0000 99.6841 90.0000 ZERR 4.00 0.000767 0.000602 0.001510 0.0000 0.0070 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H O S K Se UNIT 48.00 100.00 40.00 2.00 4.00 2.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 33190 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.084 _oxdiff_exptl_absorpt_empirical_full_min 0.938 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0078(8) 0.9496(10) 0.3572(4) 0.107(3) Uani 1 1 d . . . . . H1A H 1.097633 0.968654 0.351233 0.129 Uiso 1 1 calc R U . . . H1B H 0.994991 0.998068 0.396328 0.129 Uiso 1 1 calc R U . . . C2 C 0.9129(9) 1.0175(10) 0.3033(4) 0.113(3) Uani 1 1 d . . . . . H2A H 0.934481 1.126932 0.297915 0.136 Uiso 1 1 calc R U . . . H2B H 0.921773 0.962226 0.264989 0.136 Uiso 1 1 calc R U . . . C3 C 0.6937(10) 1.0825(10) 0.2649(3) 0.110(3) Uani 1 1 d . . . . . H3A H 0.695766 1.034484 0.224375 0.132 Uiso 1 1 calc R U . . . H3B H 0.714810 1.192918 0.262216 0.132 Uiso 1 1 calc R U . . . C4 C 0.5615(10) 1.0641(12) 0.2821(4) 0.124(3) Uani 1 1 d . . . . . H4A H 0.562398 1.105351 0.324071 0.149 Uiso 1 1 calc R U . . . H4B H 0.498146 1.124295 0.253265 0.149 Uiso 1 1 calc R U . . . C5 C 0.3948(9) 0.8959(11) 0.2963(4) 0.118(3) Uani 1 1 d . . . . . H5A H 0.330792 0.951106 0.265957 0.141 Uiso 1 1 calc R U . . . H5B H 0.392676 0.940329 0.337455 0.141 Uiso 1 1 calc R U . . . C6 C 0.3612(8) 0.7300(12) 0.2963(4) 0.122(3) Uani 1 1 d . . . . . H6A H 0.272941 0.717192 0.305614 0.147 Uiso 1 1 calc R U . . . H6B H 0.363708 0.684917 0.255312 0.147 Uiso 1 1 calc R U . . . C7 C 0.4136(9) 0.4943(13) 0.3500(5) 0.136(3) Uani 1 1 d . . . . . H7A H 0.409297 0.435569 0.311252 0.163 Uiso 1 1 calc R U . . . H7B H 0.328047 0.489468 0.362971 0.163 Uiso 1 1 calc R U . . . C8 C 0.5148(11) 0.4264(12) 0.3992(4) 0.134(3) Uani 1 1 d . . . . . H8A H 0.519382 0.487457 0.437384 0.161 Uiso 1 1 calc R U . . . H8B H 0.489716 0.320188 0.408095 0.161 Uiso 1 1 calc R U . . . C9 C 0.7314(10) 0.3377(10) 0.4257(4) 0.128(3) Uani 1 1 d . . . . . H9A H 0.710196 0.226769 0.423677 0.153 Uiso 1 1 calc R U . . . H9B H 0.730305 0.373995 0.468140 0.153 Uiso 1 1 calc R U . . . C10 C 0.8618(11) 0.3627(11) 0.4092(4) 0.128(3) Uani 1 1 d . . . . . H10A H 0.925619 0.299351 0.436495 0.154 Uiso 1 1 calc R U . . . H10B H 0.861159 0.328608 0.366336 0.154 Uiso 1 1 calc R U . . . C11 C 1.0332(9) 0.5403(12) 0.4080(4) 0.120(3) Uani 1 1 d . . . . . H11A H 1.050138 0.496161 0.368779 0.144 Uiso 1 1 calc R U . . . H11B H 1.091995 0.490756 0.442256 0.144 Uiso 1 1 calc R U . . . C12 C 1.0555(8) 0.7109(12) 0.4089(4) 0.118(3) Uani 1 1 d . . . . . H12A H 1.032973 0.754886 0.447170 0.142 Uiso 1 1 calc R U . . . H12B H 1.147923 0.731862 0.408690 0.142 Uiso 1 1 calc R U . . . K002 K 0.71218(14) 0.74822(18) 0.37870(6) 0.0653(5) Uani 1 1 d D . . . . O1 O 0.7889(6) 1.0067(6) 0.3130(2) 0.0914(16) Uani 1 1 d . . . . . O2 O 0.5248(6) 0.9154(7) 0.2805(2) 0.0956(16) Uani 1 1 d . . . . . O3 O 0.4485(5) 0.6564(8) 0.3402(2) 0.1068(18) Uani 1 1 d . . . . . O4 O 0.6344(6) 0.4243(6) 0.3816(2) 0.1008(17) Uani 1 1 d . . . . . O5 O 0.8977(6) 0.5127(7) 0.4147(2) 0.0983(17) Uani 1 1 d . . . . . O6 O 0.9826(5) 0.7798(7) 0.3590(2) 0.0957(16) Uani 1 1 d . . . . . O006 O 0.588(3) 0.801(5) 0.4855(14) 0.076(6) Uani 0.5 1 d D . P A 1 H006 H 0.515(4) 0.811(15) 0.499(3) 0.114 Uiso 0.5 1 d D U P B 1 O7 O 0.753(2) 0.799(3) 0.5814(10) 0.115(7) Uani 0.5 1 d . . P A 2 O8 O 0.701(2) 0.846(3) 0.5921(9) 0.094(6) Uani 0.5 1 d . . P A 1 O9 O 0.649(2) 1.059(3) 0.5496(8) 0.101(6) Uani 0.5 1 d . . P A 1 O10 O 0.660(2) 1.088(2) 0.5231(8) 0.079(5) Uani 0.5 1 d . . P A 2 O11 O 0.573(3) 0.839(5) 0.4759(15) 0.086(8) Uani 0.5 1 d D . P A 2 H11 H 0.507(3) 0.873(16) 0.492(3) 0.129 Uiso 0.5 1 d D U P C 2 O12 O 0.801(2) 0.935(2) 0.4832(9) 0.090(6) Uani 0.5 1 d . . P A 1 O13 O 0.823(2) 0.874(3) 0.4994(9) 0.092(5) Uani 0.5 1 d . . P A 2 S1 S 0.694(2) 0.908(2) 0.5251(10) 0.065(4) Uani 0.5 1 d D . P A 2 Se1 Se 0.7022(9) 0.8984(10) 0.5268(4) 0.0699(18) Uani 0.5 1 d D . P A 1 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 C1 0.071(5) 0.117(6) 0.139(7) -0.065(6) 0.030(5) -0.039(5) C2 0.123(6) 0.100(7) 0.126(7) -0.050(5) 0.050(5) -0.042(6) C3 0.186(7) 0.070(6) 0.062(5) 0.017(5) -0.012(5) -0.026(6) C4 0.173(8) 0.095(6) 0.089(6) 0.009(6) -0.024(6) 0.009(7) C5 0.097(6) 0.139(7) 0.118(7) -0.015(7) 0.020(5) 0.042(6) C6 0.069(6) 0.165(8) 0.135(8) -0.042(7) 0.019(5) 0.014(6) C7 0.090(6) 0.164(8) 0.166(9) -0.015(7) 0.060(6) -0.059(6) C8 0.177(8) 0.126(8) 0.110(7) -0.021(6) 0.053(6) -0.069(7) C9 0.222(9) 0.085(6) 0.062(5) 0.033(5) -0.017(6) -0.041(7) C10 0.207(8) 0.076(6) 0.088(6) 0.016(6) -0.014(7) 0.030(7) C11 0.100(6) 0.164(8) 0.089(6) 0.004(7) -0.002(5) 0.062(6) C12 0.066(5) 0.185(8) 0.101(6) -0.019(7) 0.007(4) 0.023(6) K002 0.0657(11) 0.0661(11) 0.0653(9) 0.0002(9) 0.0149(7) -0.0020(8) O1 0.117(4) 0.079(4) 0.085(3) -0.003(3) 0.035(3) -0.022(3) O2 0.115(4) 0.084(4) 0.083(3) -0.007(3) 0.003(3) 0.018(4) O3 0.074(4) 0.152(5) 0.095(4) -0.017(4) 0.017(3) -0.007(4) O4 0.141(5) 0.088(4) 0.074(3) 0.006(3) 0.019(3) -0.040(4) O5 0.126(4) 0.084(4) 0.077(3) -0.008(3) -0.006(3) 0.021(4) O6 0.071(3) 0.130(5) 0.081(3) -0.036(4) 0.000(3) -0.006(3) O006 0.063(9) 0.085(15) 0.080(8) -0.004(9) 0.011(7) -0.006(8) O7 0.076(13) 0.147(17) 0.116(11) 0.060(13) -0.002(8) -0.014(9) O8 0.105(17) 0.108(12) 0.077(6) -0.020(7) 0.036(8) -0.035(10) O9 0.091(12) 0.116(11) 0.090(13) -0.046(9) -0.004(9) 0.021(11) O10 0.086(9) 0.067(6) 0.086(13) 0.021(7) 0.023(10) -0.035(6) O11 0.065(8) 0.094(18) 0.095(11) -0.025(12) 0.002(7) -0.002(9) O12 0.093(12) 0.092(13) 0.096(10) -0.009(8) 0.044(9) -0.016(8) O13 0.066(7) 0.126(16) 0.086(9) -0.012(9) 0.016(7) -0.010(9) S1 0.062(8) 0.071(7) 0.066(7) 0.013(6) 0.018(5) -0.037(5) Se1 0.061(3) 0.081(4) 0.069(3) -0.021(3) 0.013(2) -0.008(2) 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' K K 0.2009 0.2494 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 H1A C1 H1B 108.5 . . ? C2 C1 H1A 110.2 . . ? C2 C1 H1B 110.2 . . ? O6 C1 H1A 110.2 . . ? O6 C1 H1B 110.2 . . ? O6 C1 C2 107.7(6) . . ? C1 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? O1 C2 C1 111.6(8) . . ? O1 C2 H2A 109.3 . . ? O1 C2 H2B 109.3 . . ? H3A C3 H3B 108.4 . . ? C4 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? O1 C3 H3A 110.1 . . ? O1 C3 H3B 110.1 . . ? O1 C3 C4 108.2(7) . . ? C3 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? O2 C4 C3 111.4(10) . . ? O2 C4 H4A 109.3 . . ? O2 C4 H4B 109.3 . . ? H5A C5 H5B 108.2 . . ? C6 C5 H5A 109.7 . . ? C6 C5 H5B 109.7 . . ? O2 C5 H5A 109.7 . . ? O2 C5 H5B 109.7 . . ? O2 C5 C6 110.0(8) . . ? C5 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O3 C6 C5 108.8(8) . . ? O3 C6 H6A 109.9 . . ? O3 C6 H6B 109.9 . . ? H7A C7 H7B 108.4 . . ? C8 C7 H7A 110.0 . . ? C8 C7 H7B 110.0 . . ? O3 C7 H7A 110.0 . . ? O3 C7 H7B 110.0 . . ? O3 C7 C8 108.4(8) . . ? C7 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C7 C8 K002 87.6(6) . . ? H8A C8 H8B 107.9 . . ? K002 C8 H8A 74.9 . . ? K002 C8 H8B 160.1 . . ? O4 C8 C7 111.8(8) . . ? O4 C8 H8A 109.2 . . ? O4 C8 H8B 109.2 . . ? O4 C8 K002 52.8(4) . . ? H9A C9 H9B 108.3 . . ? C10 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? O4 C9 H9A 109.9 . . ? O4 C9 H9B 109.9 . . ? O4 C9 C10 109.0(7) . . ? C9 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? O5 C10 C9 111.8(9) . . ? O5 C10 H10A 109.3 . . ? O5 C10 H10B 109.3 . . ? H11A C11 H11B 108.4 . . ? C12 C11 H11A 110.1 . . ? C12 C11 H11B 110.1 . . ? O5 C11 H11A 110.1 . . ? O5 C11 H11B 110.1 . . ? O5 C11 C12 108.1(7) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 K002 86.3(5) . . ? H12A C12 H12B 108.1 . . ? K002 C12 H12A 75.2 . . ? K002 C12 H12B 160.8 . . ? O6 C12 C11 110.9(8) . . ? O6 C12 H12A 109.5 . . ? O6 C12 H12B 109.5 . . ? O6 C12 K002 53.0(4) . . ? O1 K002 O2 57.90(17) . . ? O1 K002 O3 114.15(19) . . ? O1 K002 O4 150.18(14) . . ? O1 K002 O6 59.57(17) . . ? O1 K002 O006 119.2(8) . . ? O1 K002 O11 112.4(8) . . ? O1 K002 O13 93.6(4) . . ? O1 K002 S1 102.4(3) . . ? O1 K002 Se1 103.38(17) . . ? O2 K002 S1 109.4(4) . . ? O2 K002 Se1 111.4(2) . . ? O3 K002 O2 56.30(19) . . ? O3 K002 O4 58.77(19) . . ? O3 K002 O6 152.33(15) . . ? O3 K002 O006 74.9(6) . . ? O3 K002 O11 73.2(7) . . ? O3 K002 O13 126.1(5) . . ? O3 K002 S1 100.3(3) . . ? O3 K002 Se1 101.42(18) . . ? O4 K002 O2 108.94(17) . . ? O4 K002 O6 111.72(18) . . ? O4 K002 S1 107.3(3) . . ? O4 K002 Se1 106.43(16) . . ? O5 K002 O1 117.88(19) . . ? O5 K002 O2 150.90(15) . . ? O5 K002 O3 117.7(2) . . ? O5 K002 O4 58.97(18) . . ? O5 K002 O6 58.52(19) . . ? O5 K002 O006 105.5(7) . . ? O5 K002 O11 113.4(8) . . ? O5 K002 O13 82.3(4) . . ? O5 K002 S1 99.7(4) . . ? O5 K002 Se1 97.7(2) . . ? O6 K002 O2 112.00(18) . . ? O6 K002 S1 107.4(3) . . ? O6 K002 Se1 106.25(17) . . ? O006 K002 O2 100.0(7) . . ? O006 K002 O4 88.2(8) . . ? O006 K002 O6 132.6(6) . . ? O006 K002 Se1 27.0(7) . . ? O11 K002 O2 92.7(7) . . ? O11 K002 O4 93.9(8) . . ? O11 K002 O6 134.5(7) . . ? O11 K002 O13 53.3(8) . . ? O11 K002 S1 27.2(7) . . ? O12 K002 O1 83.1(4) . . ? O12 K002 O2 112.8(4) . . ? O12 K002 O3 124.4(5) . . ? O12 K002 O4 125.8(4) . . ? O12 K002 O5 94.0(4) . . ? O12 K002 O6 82.8(5) . . ? O12 K002 O006 52.2(8) . . ? O12 K002 Se1 25.5(5) . . ? O13 K002 O2 125.4(4) . . ? O13 K002 O4 114.1(4) . . ? O13 K002 O6 81.5(5) . . ? O13 K002 S1 26.3(6) . . ? C2 O1 C3 113.9(7) . . ? C2 O1 K002 119.6(5) . . ? C3 O1 K002 119.8(5) . . ? C4 O2 C5 112.1(8) . . ? C4 O2 K002 106.9(5) . . ? C5 O2 K002 107.0(5) . . ? C6 O3 C7 113.1(8) . . ? C6 O3 K002 125.1(6) . . ? C7 O3 K002 118.2(5) . . ? C8 O4 C9 112.4(7) . . ? C8 O4 K002 105.3(6) . . ? C9 O4 K002 109.7(4) . . ? C10 O5 C11 114.0(8) . . ? C10 O5 K002 119.9(6) . . ? C11 O5 K002 118.9(5) . . ? C1 O6 K002 105.9(4) . . ? C12 O6 C1 112.0(7) . . ? C12 O6 K002 105.3(5) . . ? K002 O006 H006 146(4) . . ? Se1 O006 K002 98.2(12) . . ? Se1 O006 H006 112(3) . . ? K002 O11 H11 156(5) . . ? S1 O11 K002 99.0(14) . . ? S1 O11 H11 101(3) . . ? Se1 O12 K002 102.8(13) . . ? S1 O13 K002 99.2(14) . . ? O7 S1 K002 113.4(13) . . ? O7 S1 O11 117(2) . . ? O10 S1 K002 113.8(11) . . ? O10 S1 O7 130.9(19) . . ? O10 S1 O11 101(2) . . ? O11 S1 K002 53.9(11) . . ? O13 S1 K002 54.6(11) . . ? O13 S1 O7 85.4(16) . . ? O13 S1 O10 111.8(13) . . ? O13 S1 O11 108.1(19) . . ? O006 Se1 K002 54.8(9) . . ? O8 Se1 K002 140.6(9) . . ? O8 Se1 O006 104.4(16) . . ? O8 Se1 O9 84.6(10) . . ? O8 Se1 O12 139.6(13) . . ? O9 Se1 K002 132.4(8) . . ? O9 Se1 O006 111.4(15) . . ? O12 Se1 K002 51.8(10) . . ? O12 Se1 O006 105.7(15) . . ? O12 Se1 O9 108.4(11) . . ? 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 C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.504(10) . ? C1 O6 1.472(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 O1 1.334(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.481(11) . ? C3 O1 1.455(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 O2 1.321(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C6 1.456(10) . ? C5 O2 1.447(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 O3 1.347(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.476(11) . ? C7 O3 1.451(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 K002 3.487(10) . ? C8 O4 1.350(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.462(12) . ? C9 O4 1.459(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 O5 1.331(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.472(11) . ? C11 O5 1.447(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 K002 3.504(8) . ? C12 O6 1.342(9) . ? K002 O1 2.805(5) . ? K002 O2 2.981(5) . ? K002 O3 2.817(5) . ? K002 O4 2.878(5) . ? K002 O5 2.792(5) . ? K002 O6 2.902(5) . ? K002 O006 2.86(3) . ? K002 O11 2.84(3) . ? K002 O12 2.79(2) . ? K002 O13 2.87(2) . ? K002 S1 3.48(2) . ? K002 Se1 3.462(9) . ? O006 H006 0.853(10) . ? O006 Se1 1.59(3) . ? O7 S1 1.57(3) . ? O8 Se1 1.48(2) . ? O9 Se1 1.58(2) . ? O10 S1 1.57(3) . ? O11 H11 0.860(10) . ? O11 S1 1.61(4) . ? O12 Se1 1.53(2) . ? O13 S1 1.56(3) . ? 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 C2 O1 C3 175.1(6) . . . . ? C1 C2 O1 K002 -33.7(8) . . . . ? C2 C1 O6 C12 -174.8(7) . . . . ? C2 C1 O6 K002 -60.6(7) . . . . ? C3 C4 O2 C5 -179.2(7) . . . . ? C3 C4 O2 K002 64.0(8) . . . . ? C4 C3 O1 C2 -178.9(7) . . . . ? C4 C3 O1 K002 29.9(9) . . . . ? C5 C6 O3 C7 172.2(8) . . . . ? C5 C6 O3 K002 -29.6(10) . . . . ? C6 C5 O2 C4 -177.7(8) . . . . ? C6 C5 O2 K002 -60.8(8) . . . . ? C7 C8 O4 C9 -171.8(8) . . . . ? C7 C8 O4 K002 68.8(8) . . . . ? C8 C7 O3 C6 -179.5(8) . . . . ? C8 C7 O3 K002 20.7(10) . . . . ? C9 C10 O5 C11 171.4(7) . . . . ? C9 C10 O5 K002 -38.7(10) . . . . ? C10 C9 O4 C8 -170.7(8) . . . . ? C10 C9 O4 K002 -53.9(9) . . . . ? C11 C12 O6 C1 -177.3(7) . . . . ? C11 C12 O6 K002 68.1(8) . . . . ? C12 C11 O5 C10 174.5(8) . . . . ? C12 C11 O5 K002 24.3(9) . . . . ? K002 C8 O4 C9 119.4(6) . . . . ? K002 C12 O6 C1 114.6(6) . . . . ? K002 O006 Se1 O8 -142.7(11) . . . . ? K002 O006 Se1 O9 127.5(10) . . . . ? K002 O006 Se1 O12 10.0(16) . . . . ? K002 O11 S1 O7 -100.5(17) . . . . ? K002 O11 S1 O10 111.2(14) . . . . ? K002 O11 S1 O13 -6(2) . . . . ? K002 O12 Se1 O006 -10.4(16) . . . . ? K002 O12 Se1 O8 126.3(18) . . . . ? K002 O12 Se1 O9 -129.9(10) . . . . ? K002 O13 S1 O7 123.1(13) . . . . ? K002 O13 S1 O10 -104.4(16) . . . . ? K002 O13 S1 O11 6(2) . . . . ? O1 C3 C4 O2 -65.6(9) . . . . ? O2 C5 C6 O3 61.4(10) . . . . ? O3 C7 C8 K002 -14.6(7) . . . . ? O3 C7 C8 O4 -62.6(11) . . . . ? O4 C9 C10 O5 63.0(10) . . . . ? O5 C11 C12 K002 -16.8(6) . . . . ? O5 C11 C12 O6 -64.7(10) . . . . ? O6 C1 C2 O1 65.8(9) . . . . ?