#------------------------------------------------------------------------------ #$Date: 2025-02-11 01:12:53 +0200 (Tue, 11 Feb 2025) $ #$Revision: 297670 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573870.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_1573870 loop_ _publ_author_name 'Smoljan, Courtney S.' 'Formalik, Filip' 'Barsoum, Michael L.' 'Fahy, Kira M.' 'Gaidimas, Madeleine A.' 'Son, Florencia A.' 'Xie, Haomiao' 'Idrees, Karam B.' 'Farha, Omar K.' 'Snurr, Randall Q.' _publ_section_title ; Exceeding flexpectations: a combined experimental and computational investigation of structural flexibility in 3-dimensional linker-based metal--organic frameworks ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC06360K _journal_year 2025 _chemical_formula_moiety 'C7 O5 V' _chemical_formula_sum 'C7 H2.4 O6.2 V' _chemical_formula_weight 236.63 _space_group_crystal_system orthorhombic _space_group_IT_number 74 _space_group_name_Hall '-I 2b 2' _space_group_name_H-M_alt 'I m m a' _atom_sites_solution_primary direct _audit_creation_date 2024-04-09 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-04-10 deposited with the CCDC. 2025-02-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.342(3) _cell_length_b 6.8717(8) _cell_length_c 10.284(3) _cell_measurement_reflns_used 1411 _cell_measurement_temperature 111(2) _cell_measurement_theta_max 69.8770 _cell_measurement_theta_min 5.0570 _cell_volume 1154.9(4) _computing_cell_refinement 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 111.15 _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 -71.00 11.00 0.50 10.00 -- -47.42 79.00 35.00 164 2 \w -21.00 54.00 0.50 10.00 -- 47.42 -79.00 -89.00 150 3 \w -95.00 -69.00 0.50 20.00 -- -106.00 79.00 35.00 52 4 \w -174.00 -83.00 0.50 20.00 -- -106.00 -79.00 -89.00 182 5 \w 72.00 98.00 0.50 20.00 -- 113.25 -79.00 -89.00 52 6 \w 140.00 166.00 0.50 20.00 -- 113.25 79.00 35.00 52 7 \w -38.00 26.00 0.50 10.00 -- -47.42 37.00-180.00 128 8 \w -18.00 14.00 0.50 10.00 -- -47.42 19.00 -60.00 64 9 \w -108.00 -83.00 0.50 10.00 -- -47.42-125.00 60.00 50 10 \w -19.00 14.00 0.50 10.00 -- -47.42 19.00 -30.00 66 11 \w -117.00 -92.00 0.50 10.00 -- -47.42-125.00 30.00 50 12 \w -117.00 -85.00 0.50 10.00 -- -47.42 0.00-150.00 64 13 \w 85.00 112.00 0.50 10.00 -- 47.42 125.00-120.00 54 14 \w -23.00 36.00 0.50 10.00 -- 47.42 -37.00 -30.00 118 15 \w -27.00 -2.00 0.50 10.00 -- 47.42 -19.00 30.00 50 16 \w -64.00 -38.00 0.50 20.00 -- -106.00 125.00 150.00 52 17 \w -108.00 -70.00 0.50 20.00 -- -106.00 110.00 -15.66 76 18 \w -73.00 -47.00 0.50 20.00 -- -106.00 61.00-180.00 52 19 \w -177.00 -89.00 0.50 20.00 -- -106.00 -61.00 -30.00 176 20 \w -111.00 -80.00 0.50 20.00 -- -106.00 125.00 150.00 62 21 \w -68.00 -43.00 0.50 20.00 -- -106.00 107.00 -88.49 50 22 \w -73.00 -34.00 0.50 20.00 -- -106.00 61.00 30.00 78 23 \w -173.00 -98.00 0.50 20.00 -- -106.00 -61.00-120.00 150 24 \w -65.00 -38.00 0.50 20.00 -- -106.00 61.00-120.00 54 25 \w -106.00 -77.00 0.50 20.00 -- -106.00 107.00 -88.49 58 26 \w -176.00-107.00 0.50 20.00 -- -106.00 -61.00 0.00 138 27 \w -72.00 -43.00 0.50 20.00 -- -106.00 61.00-150.00 58 28 \w -66.00 -39.00 0.50 20.00 -- -106.00 110.00 -15.66 54 29 \w 142.00 177.00 0.50 20.00 -- 113.25 77.00 -60.00 70 30 \w 95.00 130.00 0.50 20.00 -- 113.25 77.00 -60.00 70 31 \w 68.00 106.00 0.50 20.00 -- 113.25 -94.00 90.00 76 32 \w 44.00 71.00 0.50 20.00 -- 113.25 -61.00 30.00 54 33 \w 42.00 71.00 0.50 20.00 -- 113.25 -61.00 60.00 58 34 \w 43.00 106.00 0.50 20.00 -- 113.25 -94.00-150.00 126 35 \w 82.00 111.00 0.50 20.00 -- 113.25-125.00 90.00 58 36 \w 42.00 76.00 0.50 20.00 -- 113.25-125.00 90.00 68 37 \w 57.00 91.00 0.50 20.00 -- 113.25 -94.00 -90.00 68 38 \w 42.00 92.00 0.50 20.00 -- 113.25 -94.00 120.00 100 39 \w 123.00 177.00 0.50 20.00 -- 113.25 0.00-180.00 108 40 \w 102.00 178.00 0.50 20.00 -- 113.25 77.00 60.00 152 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1071 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 5436 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.441 _diffrn_reflns_theta_max 67.441 _diffrn_reflns_theta_min 5.081 _exptl_absorpt_coefficient_mu 7.279 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.361 _exptl_crystal_description needle _exptl_crystal_F_000 468 _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _refine_diff_density_max 1.706 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.212 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.594 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 45 _refine_ls_number_reflns 594 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.591 _refine_ls_R_factor_all 0.1523 _refine_ls_R_factor_gt 0.1448 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3655 _refine_ls_wR_factor_ref 0.3719 _reflns_Friedel_coverage 0.000 _reflns_number_gt 493 _reflns_number_total 594 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06360k2.cif _cod_data_source_block nu-2003 _cod_original_formula_sum 'C7 H2.40 O6.20 V' _cod_database_code 1573870 _shelx_shelxl_version_number 2019/1 _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 0.931 _shelx_estimated_absorpt_t_min 0.868 _olex2_refinement_description ; 1. Restrained distances C3-C2 \\sim C3-C2_$3 with sigma of 0.01 C3-C2 \\sim C4_$1-C2 with sigma of 0.01 C4-C3 \\sim C4_$1-C3 with sigma of 0.01 2. Uiso/Uaniso restraints and constraints C4 \\sim C4 \\sim C3 \\sim C4 \\sim C3 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 3. Others Fixed Sof: C4(0.5) C3(0.25) ; _shelx_res_file ; TITL NU-2003_a.res in Imma nu-2003.res created by SHELXL-2019/1 at 19:28:37 on 09-Apr-2024 REM Old TITL NU-2003 in Imma REM SHELXT solution in Imma: R1 0.301, Rweak 0.261, Alpha 0.052 REM 1.335 for 33 systematic absences, Orientation as input REM Formula found by SHELXT: C4 O5 V CELL 1.54184 16.342 6.8717 10.284 90 90 90 ZERR 4 0.0025 0.0008 0.0028 0 0 0 LATT 2 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O V UNIT 28 9.6 24.8 4 EQIV $1 +X,1.5-Y,+Z EQIV $2 0.5-X,1.5-Y,0.5-Z EQIV $3 0.5-X,+Y,0.5-Z SADI 0.01 C3 C2 C3 C2_$3 SADI 0.01 C3 C2 C4_$1 C2 SADI 0.01 C4 C3 C4_$1 C3 SIMU 0.01 0.02 2 C4 C4 C3 C4 C3 C4 L.S. 10 0 0 PLAN 5 SIZE 0.01 0.02 0.01 TEMP -162 CONF BIND C2 C3_$2 FREE C4 C3_$1 FREE C4 C3 list 4 MORE -1 ABIN fmap 2 53 acta OMIT -3 135 REM REM REM WGHT 0.200000 FVAR 0.52602 V1 4 0.500000 0.500000 0.500000 10.25000 0.05566 0.03993 = 0.09693 0.00033 0.00000 0.00000 O1 3 0.500000 0.250000 0.409150 10.25000 0.12828 0.03353 = 0.07795 0.00000 0.00000 0.00000 O2 3 0.413375 0.589756 0.378289 11.00000 0.11954 0.04596 = 0.18519 -0.00195 -0.06909 0.00068 C1 1 0.382122 0.750000 0.347836 10.50000 0.09477 0.03935 = 0.16403 0.00000 -0.06435 0.00000 C2 1 0.304266 0.750000 0.288245 10.50000 0.09230 0.06050 = 0.29940 0.00000 -0.07337 0.00000 PART -1 C4 1 0.231961 0.596451 0.295352 10.50000 0.10993 0.12384 = 0.19928 0.02627 -0.06397 -0.02951 PART 0 C3 1 0.218704 0.750000 0.361359 10.25000 0.12598 0.15717 = 0.21507 0.00000 -0.05752 0.00000 HKLF 4 REM NU-2003_a.res in Imma REM wR2 = 0.3719, GooF = S = 1.594, Restrained GooF = 1.591 for all data REM R1 = 0.1448 for 493 Fo > 4sig(Fo) and 0.1523 for all 594 data REM 45 parameters refined using 10 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.706, deepest hole -0.534, 1-sigma level 0.212 Q1 1 0.5359 0.5036 0.4327 11.00000 0.05 1.71 Q2 1 0.5000 0.1904 0.4864 10.50000 0.05 0.79 Q3 1 0.5000 0.2500 0.3444 10.25000 0.05 0.79 Q4 1 0.3851 0.5520 0.3529 11.00000 0.05 0.62 Q5 1 0.1441 0.7500 0.3128 10.50000 0.05 0.54 ; _shelx_res_checksum 40829 _shelx_fab_file ; 0 0 2 26.7233 -3.0512 0 0 4 -3.0336 -2.3085 0 0 6 0.9560 -1.5953 0 0 8 -0.1851 -0.9693 0 0 10 -1.7241 -0.4882 0 0 12 0.3561 -0.1930 0 1 1 -14.8589 -0.8612 0 1 3 -1.0841 0.0158 0 1 5 10.9299 0.1489 0 1 7 -2.9312 0.1454 0 1 9 0.2800 0.0933 0 1 11 0.5524 0.0946 0 2 0 -32.8060 -2.7624 0 2 2 6.0153 -2.2903 0 2 4 4.0498 -1.9799 0 2 6 -3.7826 -1.4316 0 2 8 -0.3426 -0.8849 0 2 10 0.4275 -0.4732 0 2 12 0.1421 -0.2540 0 3 1 12.8646 0.1163 0 3 3 -1.5633 -0.0379 0 3 5 1.2089 0.0591 0 3 7 -4.2826 0.0427 0 3 9 0.9240 -0.0130 0 3 11 -0.2935 -0.0832 0 4 0 10.6690 -2.3136 0 4 2 -2.5913 -2.1809 0 4 4 -1.4645 -1.7937 0 4 6 -0.3469 -1.2910 0 4 8 0.1849 -0.8262 0 4 10 -0.8766 -0.5096 0 5 1 -5.2385 0.0209 0 5 3 -0.4970 0.0193 0 5 5 -0.3683 0.0020 0 5 7 2.0974 -0.0443 0 5 9 0.8026 -0.0972 0 6 0 -7.6579 -1.5440 0 6 2 1.2456 -1.5815 0 6 4 0.5575 -1.3688 0 6 6 0.8077 -1.0170 0 6 8 -0.5900 -0.5612 0 7 1 3.5632 -0.0217 0 7 3 -3.1513 -0.0387 0 7 5 -1.3036 -0.1630 0 7 7 -2.8744 0.0855 0 8 0 0.1119 -1.1312 0 8 2 -1.6693 -1.0534 0 8 4 1.8592 -0.8219 1 0 1 -30.7605 0.6241 1 0 3 -13.3174 1.3444 1 0 5 6.4027 1.1118 1 0 7 -1.4770 0.7614 1 0 9 1.5433 0.5991 1 0 11 0.5944 0.2964 1 1 2 12.7626 0.0792 1 1 4 -7.1926 0.2166 1 1 6 -1.8916 -0.0674 1 1 8 1.0258 0.2409 1 1 10 -0.4120 0.0301 1 1 12 -0.7656 0.0452 1 2 1 14.5418 2.2686 1 2 3 -9.4813 1.3539 1 2 5 2.6679 1.2518 1 2 7 0.6926 0.8348 1 2 9 0.2655 0.4230 1 2 11 -0.3235 0.1507 1 3 2 -3.2971 0.0337 1 3 4 1.2259 0.0136 1 3 6 0.7764 -0.0171 1 3 8 2.3295 -0.0286 1 3 10 -1.7083 -0.0802 1 3 12 0.8035 0.0009 1 4 1 -1.4971 2.1549 1 4 3 0.3664 1.1618 1 4 5 0.7527 1.1496 1 4 7 -2.0625 0.5873 1 4 9 1.1712 0.3009 1 4 11 -0.0251 -0.0188 1 5 2 -0.1145 0.1187 1 5 4 0.3483 0.0116 1 5 6 -2.2410 0.0656 1 5 8 -0.4739 -0.0606 1 5 10 0.4871 -0.0664 1 6 1 1.6282 1.6367 1 6 3 -0.7373 0.8538 1 6 5 -0.5835 0.8149 1 6 7 1.6244 0.2769 1 6 9 0.3304 -0.0120 1 7 2 0.0670 -0.0376 1 7 4 3.1379 -0.0353 1 7 6 1.9740 -0.1117 1 8 1 0.8699 0.7893 1 8 3 -0.4370 0.5120 1 8 5 -0.7290 0.2921 2 0 0 25.5333 0.8349 2 0 2 25.8661 -0.5538 2 0 4 -2.3780 -0.1694 2 0 6 -2.0629 -0.2797 2 0 8 0.3908 -0.0832 2 0 10 -0.6694 -0.0416 2 0 12 -0.4585 -0.0728 2 1 1 -7.8943 -0.1352 2 1 3 -3.7480 0.3098 2 1 5 4.0230 -0.2341 2 1 7 -1.0634 0.0967 2 1 9 0.4904 -0.0584 2 1 11 -0.2504 -0.0380 2 2 0 -13.4722 -4.6488 2 2 2 2.1663 0.0940 2 2 4 1.2379 -0.9015 2 2 6 0.0889 -0.0362 2 2 8 -0.3450 -0.2246 2 2 10 -0.3667 -0.0210 2 2 12 0.5738 -0.1346 2 3 1 0.7094 -0.2715 2 3 3 -3.4751 -0.0872 2 3 5 2.7573 0.0395 2 3 7 -3.7193 0.0892 2 3 9 -0.2357 -0.0052 2 3 11 0.2794 -0.0178 2 4 0 -1.4497 -3.9102 2 4 2 1.8604 0.5237 2 4 4 0.9151 -0.6021 2 4 6 -0.7009 0.1771 2 4 8 0.2761 -0.1706 2 4 10 -0.3349 0.1026 2 5 1 1.6711 0.1637 2 5 3 -0.1290 0.0048 2 5 5 -0.5161 0.1086 2 5 7 2.6695 -0.0364 2 5 9 0.0892 -0.0887 2 6 0 -1.1123 -2.6427 2 6 2 -0.2845 0.3629 2 6 4 -0.4781 -0.4524 2 6 6 0.7278 0.1039 2 6 8 -1.2489 -0.2227 2 7 1 1.7996 0.1216 2 7 3 -3.2854 -0.0505 2 7 5 0.2896 -0.0116 2 7 7 -0.5181 -0.0965 2 8 0 1.1474 -1.8002 2 8 2 -0.9470 0.2258 2 8 4 3.3700 -0.6246 3 0 1 -23.7070 -0.0287 3 0 3 -6.0393 -0.1781 3 0 5 4.6289 -0.0450 3 0 7 -1.9078 -0.3096 3 0 9 0.1876 -0.0246 3 0 11 1.1587 -0.2049 3 1 2 9.4181 -0.3936 3 1 4 -2.1190 0.2661 3 1 6 0.1714 -0.3960 3 1 8 0.1137 0.1717 3 1 10 0.5051 -0.2299 3 1 12 -1.1731 0.0955 3 2 1 3.9764 0.5092 3 2 3 -4.9358 -0.9565 3 2 5 0.7747 -0.3506 3 2 7 -1.7665 -0.3333 3 2 9 0.7923 -0.1698 3 2 11 -0.0871 -0.0314 3 3 2 0.1442 -0.0399 3 3 4 2.4414 -0.0279 3 3 6 -2.3420 0.0055 3 3 8 4.6625 0.0720 3 3 10 0.1739 0.0159 3 3 12 0.8554 0.1079 3 4 1 -2.5875 0.3979 3 4 3 0.2372 -0.8093 3 4 5 -0.6720 -0.0873 3 4 7 3.1737 -0.2754 3 4 9 -0.3177 -0.0543 3 4 11 0.3113 -0.1886 3 5 2 2.3099 0.1357 3 5 4 -0.2863 -0.0850 3 5 6 0.9398 0.1371 3 5 8 -3.9351 0.0342 3 5 10 1.1955 -0.0192 3 6 1 1.9240 0.3196 3 6 3 -0.6242 -0.6408 3 6 5 1.2071 -0.0241 3 6 7 -2.5030 -0.2005 3 6 9 1.5420 -0.1820 3 7 2 -0.0733 0.1433 3 7 4 2.4676 -0.0355 3 7 6 -4.2402 0.1145 3 8 1 -0.0150 0.3961 3 8 3 -2.3604 -0.2747 4 0 0 13.7085 0.1835 4 0 2 13.1800 0.7332 4 0 4 -3.1993 0.6192 4 0 6 -1.2809 0.3645 4 0 8 0.7504 0.1930 4 0 10 -0.6183 0.1098 4 0 12 -0.7093 -0.1338 4 1 1 -1.1430 0.1109 4 1 3 -3.8495 0.2019 4 1 5 -1.2257 -0.1641 4 1 7 -0.3010 -0.0757 4 1 9 -0.1578 -0.0622 4 1 11 0.6191 -0.0925 4 2 0 3.8217 -3.7892 4 2 2 -0.7083 2.0422 4 2 4 -0.2363 -0.0771 4 2 6 1.2418 0.6735 4 2 8 0.1658 -0.0052 4 2 10 0.1956 0.2168 4 2 12 0.4444 -0.1121 4 3 1 -3.7948 0.1731 4 3 3 -3.2787 -0.0410 4 3 5 0.4033 -0.0410 4 3 7 -0.2094 -0.0575 4 3 9 -2.2530 -0.0042 4 3 11 -0.2138 0.0423 4 4 0 -4.1310 -3.2115 4 4 2 2.7237 1.7279 4 4 4 -0.5282 -0.2612 4 4 6 1.2874 0.6370 4 4 8 -1.2963 -0.0911 4 4 10 -0.0091 0.3531 4 5 1 2.2449 0.0014 4 5 3 -0.2851 -0.1368 4 5 5 2.5875 -0.0331 4 5 7 0.8841 0.0495 4 5 9 0.0588 0.0516 4 6 0 1.9766 -2.3573 4 6 2 -0.7648 1.1887 4 6 4 0.3335 -0.1776 4 6 6 -1.0757 0.6403 4 6 8 -0.3214 -0.2374 4 7 1 0.2826 0.0252 4 7 3 -2.6747 0.0300 4 7 5 0.2175 0.1239 4 7 7 3.1354 0.0060 4 8 0 0.1350 -1.3899 4 8 2 -0.0411 0.9425 4 8 4 4.2447 -0.3666 5 0 1 -0.9739 -0.0474 5 0 3 -6.5650 -0.3609 5 0 5 3.0650 -0.0762 5 0 7 -1.0468 -0.2754 5 0 9 0.0455 0.0015 5 0 11 0.1527 -0.1518 5 1 2 -7.0363 -0.4901 5 1 4 4.7240 0.2780 5 1 6 0.5795 -0.2371 5 1 8 0.1087 0.2216 5 1 10 0.0654 -0.2358 5 1 12 -1.4338 0.1856 5 2 1 -6.9172 0.4212 5 2 3 7.5549 -0.4494 5 2 5 -1.4827 0.1169 5 2 7 0.6756 -0.0943 5 2 9 -0.1853 -0.0069 5 2 11 -0.2451 0.0991 5 3 2 6.6330 0.0967 5 3 4 0.1263 0.1317 5 3 6 -0.7091 -0.0457 5 3 8 1.5706 0.0343 5 3 10 0.4880 -0.0523 5 4 1 2.9080 0.3111 5 4 3 -2.6610 -0.3674 5 4 5 0.3997 -0.0827 5 4 7 -0.3786 -0.1172 5 4 9 -0.4665 0.0150 5 4 11 0.7835 -0.0028 5 5 2 -2.0518 0.0639 5 5 4 -1.3289 -0.2082 5 5 6 -2.2608 -0.0115 5 5 8 -1.0054 -0.0894 5 5 10 1.3694 0.0764 5 6 1 -0.7400 0.1807 5 6 3 0.8677 -0.3463 5 6 5 -0.9367 -0.0108 5 6 7 0.4468 0.0686 5 7 2 -0.1423 0.1195 5 7 4 1.1258 -0.2025 5 7 6 -1.2282 0.2005 5 8 1 -0.5831 0.1904 5 8 3 -1.5156 -0.3215 6 0 0 -2.2147 -0.3038 6 0 2 -1.2733 -0.2826 6 0 4 -0.6764 -0.4184 6 0 6 0.3410 -0.1417 6 0 8 0.8162 -0.1886 6 0 10 0.3055 0.0491 6 0 12 0.4263 -0.2059 6 1 1 2.7523 -0.2377 6 1 3 2.1515 -0.1899 6 1 5 -1.1222 0.1039 6 1 7 1.1565 0.0086 6 1 9 -0.5865 0.1831 6 1 11 1.1962 -0.0503 6 2 0 2.7410 -3.5678 6 2 2 -1.1850 1.0007 6 2 4 -1.5792 -0.7763 6 2 6 0.0928 0.3457 6 2 8 -1.2679 -0.3912 6 2 10 0.6626 0.1950 6 2 12 0.0795 -0.1891 6 3 1 3.6577 0.0351 6 3 3 -1.2694 0.0644 6 3 5 -0.3532 0.1096 6 3 7 0.0324 -0.0909 6 3 9 -1.8815 0.1130 6 3 11 0.2219 -0.1503 6 4 0 2.6975 -3.2898 6 4 2 -1.3077 0.8360 6 4 4 -1.1017 -0.8452 6 4 6 0.2853 0.2238 6 4 8 -0.2334 -0.4734 6 4 10 0.1090 -0.0567 6 5 1 -2.6344 0.0114 6 5 3 1.4155 0.0697 6 5 5 2.6614 -0.0871 6 5 7 0.6321 0.0585 6 5 9 0.1633 -0.0722 6 6 0 -1.0504 -2.3431 6 6 2 -0.5574 0.6757 6 6 4 1.2578 -0.7953 6 6 6 0.0579 0.3019 6 6 8 0.1402 -0.6335 6 7 1 0.8883 0.0521 6 7 3 0.5311 -0.1262 6 7 5 -1.3294 0.0372 6 8 0 -0.1567 -1.5428 6 8 2 0.7330 0.2386 7 0 1 0.5166 -0.0317 7 0 3 2.0840 0.2331 7 0 5 0.0582 0.1955 7 0 7 1.1952 0.1396 7 0 9 -0.9302 0.1800 7 0 11 -0.6658 0.0731 7 1 2 -1.2496 0.1387 7 1 4 0.1481 0.2250 7 1 6 -0.7272 -0.1092 7 1 8 -1.2226 0.2104 7 1 10 0.0885 -0.0720 7 1 12 -0.9516 0.0889 7 2 1 1.6167 0.8619 7 2 3 1.7135 0.2428 7 2 5 -0.7884 0.3223 7 2 7 1.9041 0.1904 7 2 9 -0.3759 0.0352 7 2 11 -0.0674 -0.0452 7 3 2 -4.3156 -0.1125 7 3 4 1.4081 -0.0777 7 3 6 -0.2833 -0.0682 7 3 8 0.5994 0.0131 7 3 10 0.3395 -0.0959 7 4 1 -0.2615 0.7509 7 4 3 1.5307 0.2761 7 4 5 -0.2566 0.1976 7 4 7 -1.1241 0.2551 7 4 9 0.0517 0.0261 7 5 2 -0.3546 0.1241 7 5 4 -4.2084 -0.0235 7 5 6 -1.1589 0.1116 7 5 8 0.6464 -0.0765 7 6 1 -0.4555 0.7922 7 6 3 -0.1719 0.1091 7 6 5 -0.2665 0.2424 7 6 7 0.9005 0.1346 7 7 2 -0.6813 -0.0953 7 7 4 1.2757 0.0657 7 7 6 1.2017 0.0088 7 8 1 0.6266 0.2729 8 0 0 1.6382 0.0776 8 0 2 -1.7577 -0.0319 8 0 4 2.4585 -0.0940 8 0 6 -0.4014 0.0510 8 0 8 -1.4331 -0.1072 8 0 10 1.7899 0.1199 8 0 12 0.3616 -0.1387 8 1 1 0.0415 -0.0436 8 1 3 2.8001 0.0341 8 1 5 -0.3845 0.1388 8 1 7 1.0378 -0.1080 8 1 9 0.6036 0.1459 8 1 11 -0.2689 -0.2301 8 2 0 -1.5710 -3.4190 8 2 2 -0.5755 0.7115 8 2 4 -1.4164 -0.8274 8 2 6 -0.6849 0.2931 8 2 8 -0.5770 -0.3527 8 2 10 -0.0572 0.1904 8 3 1 4.3443 0.0049 8 3 3 -0.7786 -0.0991 8 3 5 1.3076 0.0067 8 3 7 -0.1379 -0.0815 8 3 9 -0.9899 0.1000 8 3 11 0.9938 -0.0639 8 4 0 0.6582 -3.0787 8 4 2 -1.3755 0.6545 8 4 4 2.0197 -0.6153 8 4 6 -0.8958 0.4339 8 4 8 0.6974 -0.1457 8 4 10 -0.3415 0.1501 8 5 1 -1.2387 0.0788 8 5 3 4.3719 0.0087 8 5 5 -0.1203 0.0035 8 5 7 0.4788 0.1298 8 5 9 -0.0990 -0.1659 8 6 0 -0.1048 -2.1050 8 6 2 0.2038 0.4887 8 6 4 -1.0175 -0.3993 8 6 6 1.1181 0.3795 8 6 8 -0.1041 -0.4692 8 7 1 1.1062 -0.0727 8 7 3 0.7870 0.0842 8 7 5 -0.3389 -0.0519 8 8 0 0.3920 -1.1423 9 0 1 -4.9663 -0.0665 9 0 3 1.3898 -0.0293 9 0 5 -1.7655 -0.1241 9 0 7 1.8526 0.0035 9 0 9 -1.1444 -0.0233 9 0 11 -0.7262 -0.0724 9 1 2 2.9914 -0.1932 9 1 4 -2.1420 0.0576 9 1 6 -1.0499 -0.1381 9 1 8 -1.3393 0.0343 9 1 10 0.5795 -0.0460 9 2 1 2.7528 0.4501 9 2 3 -1.8433 -0.1929 9 2 5 -0.0512 -0.2214 9 2 7 0.8850 -0.0797 9 2 9 -0.3465 -0.1241 9 2 11 0.5158 -0.0468 9 3 2 -4.3414 -0.0362 9 3 4 0.4680 0.0353 9 3 6 -1.3096 -0.0574 9 3 8 1.1934 0.1036 9 3 10 0.5942 -0.0252 9 4 1 -1.4692 0.2280 9 4 3 0.0584 -0.2019 9 4 5 -0.1918 -0.3066 9 4 7 1.0472 0.1030 9 4 9 0.7891 -0.3180 9 5 2 0.4365 0.0387 9 5 4 -2.1520 -0.0153 9 5 6 1.4761 0.1526 9 5 8 -0.3486 -0.0675 9 6 1 0.7476 0.1800 9 6 3 0.0718 -0.2002 9 6 5 0.2911 -0.1363 9 6 7 -0.9070 -0.1292 9 7 2 -1.7127 0.1556 9 7 4 -0.4424 -0.1346 10 0 0 4.9735 0.0018 10 0 2 3.0985 0.1629 10 0 4 2.1609 0.2241 10 0 6 -1.9853 0.1761 10 0 8 -0.2415 0.0364 10 0 10 1.0063 0.1117 10 1 1 -0.7172 0.1453 10 1 3 -1.0194 0.0604 10 1 5 -0.2284 0.0544 10 1 7 1.8294 -0.1700 10 1 9 0.1202 0.0896 10 1 11 -1.1766 -0.1269 10 2 0 0.8979 -2.7562 10 2 2 -1.4738 1.0853 10 2 4 0.7574 -0.2023 10 2 6 0.3164 0.4363 10 2 8 -0.0974 -0.0800 10 2 10 -0.1991 0.1560 10 3 1 -0.6705 -0.0552 10 3 3 1.0002 0.0429 10 3 5 1.1088 -0.0586 10 3 7 -0.1644 0.0652 10 3 9 -0.8887 -0.0537 10 4 0 -1.8028 -2.3412 10 4 2 1.8669 1.1733 10 4 4 0.0597 -0.2928 10 4 6 -0.6114 0.4770 10 4 8 -0.5624 -0.1460 10 5 1 0.4966 -0.0104 10 5 3 1.1701 -0.0054 10 5 5 -0.0083 -0.0062 10 5 7 0.0166 -0.0384 10 6 0 0.6958 -1.6332 10 6 2 -0.1603 0.8998 10 6 4 -0.0213 -0.1545 10 6 6 0.1076 0.2184 10 7 1 0.4885 0.2134 10 7 3 0.8408 -0.1128 11 0 1 -0.5348 0.1433 11 0 3 -2.1945 -0.0210 11 0 5 -3.2076 -0.0704 11 0 7 2.0167 -0.0101 11 0 9 -0.4438 -0.1082 11 0 11 0.1169 -0.0782 11 1 2 -0.7852 -0.2534 11 1 4 -1.1403 0.0901 11 1 6 1.4588 -0.1256 11 1 8 -0.8358 0.0267 11 1 10 0.6712 -0.0580 11 2 1 -1.7853 0.1276 11 2 3 0.9948 -0.3039 11 2 5 1.1222 -0.1757 11 2 7 -0.1675 0.1137 11 2 9 -0.2584 -0.0237 11 3 2 1.8438 -0.0052 11 3 4 0.1467 0.1105 11 3 6 -1.1759 0.0722 11 3 8 0.2476 0.0479 11 3 10 0.5919 0.0064 11 4 1 0.7037 0.1262 11 4 3 -0.6942 -0.0865 11 4 5 0.0645 0.0192 11 4 7 0.2598 0.1132 11 4 9 1.3709 -0.3223 11 5 2 -0.4038 0.0521 11 5 4 -0.4139 -0.0200 11 5 6 0.3410 -0.1212 11 5 8 -0.0539 -0.0407 11 6 1 -0.0773 0.1624 11 6 3 -0.0747 -0.1002 11 6 5 -0.1651 -0.1391 11 7 2 -0.9290 0.1970 12 0 0 -0.1816 -0.0909 12 0 2 -0.4146 -0.0267 12 0 4 0.5352 -0.1501 12 0 6 0.5390 -0.1125 12 0 8 0.1542 -0.0554 12 0 10 -0.2871 -0.0311 12 1 1 -0.8125 -0.0499 12 1 3 -0.4603 -0.1608 12 1 5 0.4138 -0.0403 12 1 7 0.1204 -0.0580 12 1 9 0.0518 0.0852 12 2 0 0.7673 -2.5235 12 2 2 -0.6477 0.7430 12 2 4 0.4502 -0.5184 12 2 6 -0.1676 0.2352 12 2 8 -0.4443 -0.2153 12 2 10 0.3259 -0.0122 12 3 1 -0.6029 -0.0222 12 3 3 0.0069 -0.0559 12 3 5 -0.2322 0.0952 12 3 7 0.0122 0.0513 12 3 9 0.0330 -0.0281 12 4 0 -0.3525 -2.1106 12 4 2 0.2580 0.5813 12 4 4 -1.2786 -0.4322 12 4 6 0.5366 0.0156 12 4 8 -0.9921 -0.2885 12 5 1 0.0904 -0.0603 12 5 3 -0.4954 0.1524 12 5 5 0.3140 -0.1419 12 5 7 -0.1796 0.0404 12 6 0 0.3577 -1.5248 12 6 2 -0.3021 0.2926 12 6 4 0.9316 -0.4925 13 0 1 1.9607 -0.0449 13 0 3 0.2545 0.0587 13 0 5 -0.9899 0.0646 13 0 7 0.3029 0.1320 13 0 9 -0.8411 -0.0661 13 1 2 0.0143 0.0647 13 1 4 0.3418 0.1455 13 1 6 1.0626 0.0416 13 1 8 -1.1883 0.1067 13 2 1 -0.3981 0.4578 13 2 3 1.3704 0.1645 13 2 5 -0.7332 0.2225 13 2 7 -0.2782 0.1908 13 2 9 1.3566 -0.1014 13 3 2 1.1458 -0.0373 13 3 4 -0.5437 0.0431 13 3 6 0.4289 -0.1129 13 3 8 1.0304 -0.1563 13 4 1 0.7546 0.4209 13 4 3 0.0190 0.2212 13 4 5 0.6146 -0.0381 13 4 7 0.4478 0.1668 13 5 2 -0.7612 0.0479 13 5 4 1.0233 -0.2232 13 5 6 -0.5852 0.0899 13 6 1 -0.4873 0.4707 13 6 3 0.1112 0.0132 14 0 0 -0.0627 -0.0003 14 0 2 -2.5117 -0.0053 14 0 4 0.3187 -0.0890 14 0 6 3.5233 0.0232 14 0 8 -1.9309 0.0010 14 1 1 -1.6755 -0.0671 14 1 3 1.2798 -0.0552 14 1 5 0.3081 0.1598 14 1 7 -3.1159 -0.0273 14 1 9 1.5438 0.0835 14 2 0 -1.3369 -2.0444 14 2 2 1.2260 0.4802 14 2 4 -0.5183 -0.4136 14 2 6 -0.7413 0.1984 14 2 8 0.2737 -0.2043 14 3 1 1.6520 0.0252 14 3 3 -1.4720 0.1384 14 3 5 -0.1714 -0.0277 14 3 7 -0.2708 -0.1502 14 4 0 1.1061 -1.7013 14 4 2 -1.5861 0.5173 14 4 4 0.5602 -0.4790 14 4 6 0.0976 0.1356 14 5 1 -0.2133 0.0478 14 5 3 0.3074 -0.1953 14 5 5 -0.7924 0.0270 14 6 0 0.1160 -1.0936 14 6 2 0.0870 -0.2146 15 0 1 -0.9602 -0.1149 15 0 3 1.0813 0.0036 15 0 5 -0.8832 -0.0393 15 0 7 -1.6176 -0.0455 15 0 9 1.8420 -0.1719 15 1 2 0.7221 -0.1090 15 1 4 -0.6382 -0.0290 15 1 6 1.0243 -0.0687 15 1 8 1.3897 -0.0854 15 2 1 0.0536 0.1895 15 2 3 -0.4611 0.0449 15 2 5 -0.6077 -0.1011 15 2 7 0.8715 -0.1218 15 3 2 -0.1782 0.0195 15 3 4 0.1190 -0.0574 15 3 6 1.0243 -0.0483 15 4 1 0.2089 0.1247 15 4 3 -0.0856 -0.1402 15 4 5 -0.4481 -0.3106 15 5 2 -0.3788 0.0680 15 5 4 0.4796 0.0036 16 0 0 -1.4757 0.0439 16 0 2 1.9396 0.0989 16 0 4 -0.4313 0.0742 16 0 6 1.4098 0.1004 16 0 8 0.3453 0.0086 16 1 1 2.4161 0.1177 16 1 3 0.7047 0.0669 16 1 5 0.2638 0.1448 16 1 7 -1.0708 -0.1552 16 2 0 2.7080 -1.3915 16 2 2 -0.1833 0.6185 16 2 4 0.3180 -0.1304 16 2 6 0.5599 0.1140 16 3 1 -1.1440 0.0042 16 3 3 0.0935 -0.0447 16 3 5 0.1212 -0.1255 16 4 0 -1.0669 -1.2833 16 4 2 0.5094 0.3732 16 4 4 0.3311 -0.0369 16 5 1 0.3997 0.0156 16 5 3 -0.8661 0.0504 17 0 1 -0.6952 0.0609 17 0 3 0.1923 -0.0116 17 0 5 -0.5623 -0.0808 17 0 7 -0.5368 0.0525 17 1 2 -1.3159 -0.0756 17 1 4 -1.9694 0.0604 17 1 6 0.7982 -0.0592 17 2 1 -0.4450 0.0869 17 2 3 -0.9350 -0.1413 17 2 5 -0.0702 -0.2533 17 3 2 -0.4978 -0.0339 17 3 4 -0.0744 -0.1288 17 3 6 0.8579 0.2079 17 4 1 -0.2549 0.0602 17 4 3 0.2345 -0.0353 18 0 0 0.7921 -0.0819 18 0 2 0.4659 -0.0741 18 0 4 -0.7938 0.0661 18 0 6 -0.6228 -0.0932 18 1 1 0.2673 -0.0170 18 1 3 1.2394 -0.0844 18 1 5 0.3844 -0.1714 18 2 0 -1.1736 -1.2357 18 2 2 0.3512 0.4057 18 2 4 0.3976 -0.2692 18 3 1 0.3767 -0.0633 18 3 3 0.4415 -0.1345 18 4 0 -0.3464 -0.9397 18 4 2 -0.2345 0.0201 19 0 1 0.7661 0.1651 19 0 3 0.5565 -0.0504 19 0 5 0.4694 -0.1697 19 1 2 -1.0908 0.0874 19 1 4 -1.6058 -0.0007 19 2 1 0.5631 0.0165 19 2 3 -0.7010 -0.1748 19 3 2 -0.2655 0.0572 20 0 0 -0.1415 -0.2680 20 0 2 -1.0118 -0.1992 20 1 1 -0.5544 -0.1139 20 1 3 1.3149 0.0582 20 2 0 -2.2057 -0.8136 0 0 0 0.0 0.0 ; _shelx_fab_checksum 44361 _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 ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-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 V1 V 0.500000 0.500000 0.500000 0.0642(12) Uani 1 4 d S T P . . O1 O 0.500000 0.250000 0.4091(9) 0.080(3) Uani 1 4 d S T P . . O2 O 0.4134(4) 0.5898(8) 0.3783(8) 0.117(3) Uani 1 1 d . . . . . C1 C 0.3821(8) 0.750000 0.3478(17) 0.099(5) Uani 1 2 d S T P A . C2 C 0.3043(9) 0.750000 0.288(2) 0.151(9) Uani 1 2 d DS T P . . C4 C 0.2320(16) 0.596(4) 0.295(3) 0.144(12) Uani 0.5 1 d D U P A -1 C3 C 0.2187(17) 0.750000 0.361(3) 0.166(14) Uani 0.5 2 d DS TU P A . 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 V1 0.0557(16) 0.0399(17) 0.097(2) 0.0003(9) 0.000 0.000 O1 0.128(9) 0.034(5) 0.078(6) 0.000 0.000 0.000 O2 0.120(5) 0.046(4) 0.185(7) -0.002(3) -0.069(5) 0.001(3) C1 0.095(7) 0.039(5) 0.164(12) 0.000 -0.064(8) 0.000 C2 0.092(9) 0.061(8) 0.30(3) 0.000 -0.073(14) 0.000 C4 0.110(19) 0.12(2) 0.20(4) 0.026(14) -0.06(2) -0.030(13) C3 0.13(2) 0.16(3) 0.22(4) 0.000 -0.06(2) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.0687 2.1097 '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 O1 V1 O1 180.0 9_666 . ? O1 V1 O2 91.6(3) 9_666 12_655 ? O1 V1 O2 88.4(3) 9_666 9_666 ? O1 V1 O2 91.6(3) . 9_666 ? O1 V1 O2 88.4(3) . . ? O1 V1 O2 88.4(3) . 12_655 ? O1 V1 O2 88.4(3) 9_666 4_566 ? O1 V1 O2 91.6(3) 9_666 . ? O1 V1 O2 91.6(3) . 4_566 ? O2 V1 O2 89.2(5) 9_666 12_655 ? O2 V1 O2 89.2(5) . 4_566 ? O2 V1 O2 90.8(5) . 12_655 ? O2 V1 O2 180.0(3) 12_655 4_566 ? O2 V1 O2 90.8(5) 9_666 4_566 ? O2 V1 O2 180.0 . 9_666 ? V1 O1 V1 122.9(5) . 2_655 ? C1 O2 V1 136.1(6) . . ? O2 C1 O2 122.9(10) 11_575 . ? O2 C1 C2 118.4(5) . . ? O2 C1 C2 118.4(5) 11_575 . ? C1 C2 C2 178(3) . 7_545 ? C1 C2 C4 130.6(15) . . ? C1 C2 C4 130.6(15) . 11_575 ? C1 C2 C3 129(2) . 13_565 ? C1 C2 C3 126(3) . . ? C1 C2 C3 126(3) . 11_575 ? C4 C2 C2 48.5(12) . 7_545 ? C4 C2 C2 48.5(12) 11_575 7_545 ? C4 C2 C4 83(2) . 11_575 ? C4 C2 C3 47.3(13) 11_575 11_575 ? C4 C2 C3 47.3(13) . . ? C4 C2 C3 47.3(13) . 11_575 ? C4 C2 C3 47.3(13) 11_575 . ? C3 C2 C2 52.2(8) . 7_545 ? C3 C2 C2 52.4(8) 13_565 7_545 ? C3 C2 C2 52.2(8) 11_575 7_545 ? C3 C2 C4 82.4(13) 13_565 . ? C3 C2 C4 82.4(13) 13_565 11_575 ? C3 C2 C3 104.6(16) 13_565 11_575 ? C3 C2 C3 104.6(16) 13_565 . ? C3 C2 C3 0.0(10) 11_575 . ? C2 C3 C2 75.4(16) 7_545 . ? C4 C3 C2 61.5(18) 11_575 7_545 ? C4 C3 C2 66.3(8) 11_575 . ? C3 C3 C2 0(10) 11_575 . ? C3 C3 C2 0(10) 11_575 7_545 ? C3 C3 C4 0(10) 11_575 11_575 ? 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 V1 O1 1.956(5) 9_666 ? V1 O1 1.956(5) . ? V1 O2 1.988(6) 9_666 ? V1 O2 1.988(6) . ? V1 O2 1.988(6) 4_566 ? V1 O2 1.988(6) 12_655 ? O2 C1 1.254(8) . ? C1 C2 1.412(19) . ? C2 C2 1.94(3) 7_545 ? C2 C4 1.59(2) . ? C2 C4 1.59(2) 11_575 ? C2 C3 1.58(2) 13_565 ? C2 C3 1.59(2) 11_575 ? C2 C3 1.59(2) . ? C3 C3 0.00(10) 11_575 ? 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 V1 O2 C1 O2 14(3) . . . 11_575 ? V1 O2 C1 C2 -159.7(13) . . . . ? O2 C1 C2 C4 -148(2) 11_575 . . . ? O2 C1 C2 C4 26(4) . . . . ? O2 C1 C2 C4 -26(4) 11_575 . . 11_575 ? O2 C1 C2 C4 148(2) . . . 11_575 ? O2 C1 C2 C3 -93.1(16) . . . 13_565 ? O2 C1 C2 C3 86.9(16) . . . . ? O2 C1 C2 C3 86.9(16) . . . 11_575 ? O2 C1 C2 C3 -86.9(16) 11_575 . . . ? O2 C1 C2 C3 -86.9(16) 11_575 . . 11_575 ? O2 C1 C2 C3 93.1(16) 11_575 . . 13_565 ? C1 C2 C3 C2 180.000(3) . . . 7_545 ? C1 C2 C3 C4 115.1(17) . . . 11_575 ? C1 C2 C3 C3 0(100) . . . 11_575 ? C2 C2 C3 C4 -64.9(17) 7_545 . . 11_575 ? C2 C2 C3 C3 0.0(15) 7_545 . . 11_575 ? C4 C2 C3 C2 64.9(17) 11_575 . . 7_545 ? C4 C2 C3 C2 -64.9(17) . . . 7_545 ? C4 C2 C3 C4 -130(3) . . . 11_575 ? C4 C2 C3 C3 0(3) . . . 11_575 ? C4 C2 C3 C3 0.0(5) 11_575 . . 11_575 ? C3 C2 C3 C2 0(100) 11_575 . . 7_545 ? C3 C2 C3 C2 0.000(1) 13_565 . . 7_545 ? C3 C2 C3 C4 0(100) 11_575 . . 11_575 ? C3 C2 C3 C4 -64.9(17) 13_565 . . 11_575 ? C3 C2 C3 C3 0.0(15) 13_565 . . 11_575 ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.803 0.500 213.3 24.2 '2.4 H2O' 2 0.500 -0.636 0.000 213.3 24.2 '2.4 H2O'