#------------------------------------------------------------------------------ #$Date: 2020-07-06 04:47:58 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253786 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/65/7126501.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_7126501 loop_ _publ_author_name 'Sasmal, Sheuli' 'Sinha, Soumya Kumar' 'Lahiri, Goutam Kumar' 'Maiti, Debabrata' _publ_section_title ; A directing group-assisted ruthenium-catalyzed approach to access meta-nitrated phenols. ; _journal_issue 52 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 7100 _journal_page_last 7103 _journal_paper_doi 10.1039/d0cc02851g _journal_volume 56 _journal_year 2020 _chemical_formula_moiety '0.444(C12 H10 N2 O4)' _chemical_formula_sum 'C5.33 H4.44 N0.89 O1.78' _chemical_formula_weight 109.43 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-04-13 _audit_creation_method ; Olex2 1.3 (compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003) ; _audit_update_record ; 2020-04-13 deposited with the CCDC. 2020-05-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.333(5) _cell_angle_gamma 90 _cell_formula_units_Z 9 _cell_length_a 8.5310(4) _cell_length_b 11.1285(5) _cell_length_c 12.0481(6) _cell_measurement_reflns_used 4162 _cell_measurement_temperature 150 _cell_measurement_theta_max 31.0820 _cell_measurement_theta_min 3.5960 _cell_volume 1072.54(9) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 28.5714 _diffrn_detector_type 'Rigaku Saturn724+' _diffrn_measured_fraction_theta_full 0.950 _diffrn_measured_fraction_theta_max 0.950 _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 -72.00 53.50 0.50 8.00 -- -20.00 0.00-108.00 251 2 \w -13.50 18.00 0.50 8.00 -- -20.00 -72.00 108.00 63 3 \w -73.00 -43.00 0.50 8.00 -- -20.00 -72.00 36.00 60 4 \w -107.00 -3.50 0.50 8.00 -- -20.00 0.00 -36.00 207 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'Mitegen 50um' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0700860000 _diffrn_orient_matrix_UB_12 -0.0317796000 _diffrn_orient_matrix_UB_13 0.0381990000 _diffrn_orient_matrix_UB_21 0.0321351000 _diffrn_orient_matrix_UB_22 0.0541235000 _diffrn_orient_matrix_UB_23 0.0305490000 _diffrn_orient_matrix_UB_31 -0.0437565000 _diffrn_orient_matrix_UB_32 -0.0111068000 _diffrn_orient_matrix_UB_33 0.0393876000 _diffrn_radiation_collimation 0.3 _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 0.0344 _diffrn_reflns_av_unetI/netI 0.0270 _diffrn_reflns_Laue_measured_fraction_full 0.950 _diffrn_reflns_Laue_measured_fraction_max 0.950 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 5567 _diffrn_reflns_point_group_measured_fraction_full 0.950 _diffrn_reflns_point_group_measured_fraction_max 0.950 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 3.146 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_current 24.0 _diffrn_source_power 1.2 _diffrn_source_target Mo _diffrn_source_type 'Enhance (Mo) X-ray Source' _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.41573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 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 1.525 _exptl_crystal_description trapezoid _exptl_crystal_F_000 512 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.089 _exptl_crystal_size_min 0.076 _refine_diff_density_max 0.230 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 164 _refine_ls_number_reflns 1797 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0414 _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^)+(0.0704P)^2^+0.3562P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.1143 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1633 _reflns_number_total 1797 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc02851g2.cif _cod_data_source_block dm-ta-53_mo _cod_depositor_comments 'Adding full bibliography for 7126500--7126501.cif.' _cod_original_cell_volume 1072.55(9) _cod_database_code 7126501 _shelx_shelxl_version_number 2014/7 _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 0.991 _shelx_estimated_absorpt_t_min 0.987 _reflns_odcompleteness_completeness 79.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 31.06 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C008(H008), C009(H009), C00A(H00D), C00B(H00E), C00C(H00F), C00H(H00H), C00I(H00I) 2.b Idealised Me refined as rotating group: C007(H00A,H00B,H00C) ; _shelx_res_file ; dm-ta-53_mo.res created by SHELXL-2014/7 TITL dm-ta-53_mo_a.res in P2(1)/c REM Old TITL dm-ta-53_mo_a.res in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.145, Rweak 0.003, Alpha 0.021, Orientation as input REM Formula found by SHELXT: C13 N O4 CELL 0.71073 8.531048 11.128502 12.048073 90 110.3328 90 ZERR 9 0.000354 0.000506 0.000569 0 0.0051 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 48 40 8 16 L.S. 50 PLAN 5 SIZE 0.076 0.089 0.11 TEMP -123.15 CONF BOND $H list 4 MORE -1 fmap 2 acta 52 OMIT -3 50 OMIT 1 3 0 OMIT 1 2 1 OMIT 1 2 2 OMIT -1 0 2 OMIT 1 3 2 OMIT 0 2 0 OMIT 0 1 1 OMIT 1 1 0 OMIT 1 0 0 REM REM REM WGHT 0.070400 0.356200 FVAR 7.99987 O001 4 0.396022 0.385023 0.282799 11.00000 0.01981 0.01740 = 0.01285 0.00129 0.00713 0.00232 O002 4 0.277801 0.427374 0.706255 11.00000 0.01805 0.02416 = 0.01323 -0.00509 0.00889 -0.00445 O003 4 0.562979 0.132413 0.528632 11.00000 0.02065 0.01607 = 0.02651 0.00598 0.00918 0.00282 O004 4 0.640408 0.243502 0.409244 11.00000 0.01957 0.02367 = 0.02092 0.00143 0.01348 0.00172 N005 3 0.064039 0.286439 0.646946 11.00000 0.01402 0.01905 = 0.01449 0.00092 0.00508 0.00235 N006 3 0.554218 0.225132 0.470466 11.00000 0.01354 0.01552 = 0.01294 -0.00134 0.00365 -0.00189 C007 1 0.319869 0.469100 0.188644 11.00000 0.02320 0.01894 = 0.01207 0.00276 0.00582 0.00020 AFIX 137 H00A 2 0.362462 0.455161 0.123952 11.00000 -1.50000 H00B 2 0.346981 0.551252 0.218429 11.00000 -1.50000 H00C 2 0.198321 0.458126 0.159452 11.00000 -1.50000 AFIX 0 C008 1 0.405229 0.324237 0.584319 11.00000 0.01251 0.01570 = 0.01318 -0.00001 0.00416 -0.00466 AFIX 43 H008 2 0.456622 0.269284 0.646729 11.00000 -1.20000 AFIX 0 C009 1 0.219854 0.490017 0.504872 11.00000 0.01256 0.01540 = 0.01875 -0.00358 0.00640 -0.00203 AFIX 43 H009 2 0.145184 0.549154 0.514352 11.00000 -1.20000 AFIX 0 C00A 1 -0.051755 0.222384 0.674611 11.00000 0.01406 0.01815 = 0.02169 0.00379 0.00690 0.00280 AFIX 43 H00D 2 -0.119886 0.168025 0.617227 11.00000 -1.20000 AFIX 0 C00B 1 0.250258 0.482582 0.399213 11.00000 0.01350 0.01462 = 0.01445 0.00088 0.00318 -0.00245 AFIX 43 H00E 2 0.195032 0.536270 0.336496 11.00000 -1.20000 AFIX 0 C00C 1 0.023854 0.311113 0.865680 11.00000 0.02366 0.02732 = 0.01569 0.00867 0.01156 0.01158 AFIX 43 H00F 2 0.010457 0.319177 0.940377 11.00000 -1.20000 AFIX 0 C00D 1 0.156942 0.360815 0.728770 11.00000 0.01277 0.01635 = 0.01419 0.00408 0.00609 0.00547 C00E 1 0.360961 0.397236 0.383787 11.00000 0.01293 0.01473 = 0.01170 -0.00270 0.00537 -0.00494 C00F 1 0.436776 0.318209 0.478501 11.00000 0.01038 0.01312 = 0.01634 -0.00238 0.00422 -0.00304 C00G 1 0.298028 0.411494 0.596536 11.00000 0.01431 0.01918 = 0.01315 -0.00421 0.00703 -0.00577 C00H 1 0.142586 0.377947 0.839703 11.00000 0.01851 0.02186 = 0.01246 0.00127 0.00430 0.00775 AFIX 43 H00H 2 0.211957 0.433489 0.895034 11.00000 -1.20000 AFIX 0 C00I 1 -0.076691 0.231375 0.781254 11.00000 0.01846 0.02184 = 0.02629 0.01040 0.01238 0.00645 AFIX 43 H00I 2 -0.159870 0.184698 0.796961 11.00000 -1.20000 AFIX 0 HKLF 4 REM dm-ta-53_mo_a.res in P2(1)/c REM R1 = 0.0414 for 1633 Fo > 4sig(Fo) and 0.0455 for all 1797 data REM 164 parameters refined using 0 restraints END WGHT 0.0705 0.3488 REM Highest difference peak 0.230, deepest hole -0.231, 1-sigma level 0.058 Q1 1 0.2629 0.3925 0.3965 11.00000 0.05 0.23 Q2 1 0.4244 0.3676 0.4392 11.00000 0.05 0.23 Q3 1 -0.1140 0.2578 0.7178 11.00000 0.05 0.22 Q4 1 0.5873 0.0395 0.5163 11.00000 0.05 0.21 Q5 1 0.4211 0.3092 0.2625 11.00000 0.05 0.20 ; _shelx_res_checksum 36379 _shelx_hkl_file ; 0 0 -2 5525.27 181.369 1 0 0 -2 5603.81 179.871 4 0 0 3 8.80689 17.5051 4 0 0 -3 40.8249 25.4057 4 0 0 -3 23.4342 18.2032 1 0 0 -4 1486.67 137.659 1 0 0 4 1242.31 123.494 4 0 0 -4 1228.03 128.187 4 0 0 -5 30.4823 28.8613 4 0 0 -5-17.3742 35.0812 1 0 0 -6 8676.17 427.619 4 0 0 -6 8045.10 407.045 1 0 0 -7 22.5544 53.9012 4 0 0 -7 18.0770 36.2555 1 0 0 -8 7781.11 475.994 4 0 0 -8 8444.39 495.324 1 0 0 -9-17.7028 76.9798 1 0 0 -9 95.3126 57.9789 4 0 0 -10 60572.0 1488.82 1 0 0 -10 60885.9 1484.86 4 0 0 -11-0.47636 81.9758 1 0 0 -11 32.6214 72.0016 4 0 0 -12 667.463 188.990 4 0 0 -12 978.320 240.352 1 0 0 -13-85.1583 100.722 1 0 0 -13 75.5759 130.274 4 0 0 -14 364.396 168.914 4 0 0 -14 828.653 292.286 3 0 0 -14 401.659 182.155 1 0 0 -15-14.3768 145.046 3 0 1 0 2.60307 5.51714 1 0 -1 0-2.13415 5.37657 1 0 1 -1-2.59733 5.66627 4 0 1 -1 7.33003 9.00389 3 0 1 -1 0.92993 5.55832 1 0 1 -2 7849.15 235.592 1 0 -1 2-6.07742 11.1564 4 0 1 -2 7779.01 229.213 4 0 -1 2 3.71261 9.98600 1 0 1 -3 2534.15 160.244 4 0 -1 3 2983.95 170.458 4 0 -1 3 3172.15 178.298 1 0 1 -3 3052.69 176.486 1 0 1 -4 27805.4 600.211 4 0 -1 4 26269.3 562.822 4 0 -1 4 26049.4 553.090 1 0 1 -4 28002.4 609.075 1 0 -1 -4 25278.4 579.544 4 0 -1 5 94.6922 52.9448 4 0 -1 -5 206.554 57.7572 4 0 1 -5 51.9877 29.3188 1 0 1 -5 162.974 50.9750 4 0 1 -6 2056.90 205.516 1 0 -1 -6 1926.26 198.950 4 0 -1 6 1683.22 174.062 4 0 1 -6 2159.33 209.435 4 0 -1 -7 55353.6 1167.04 4 0 1 -7 54781.4 1145.26 1 0 1 -7 52683.3 1117.75 4 0 -1 -8 3429.43 314.230 4 0 1 -8 3401.86 308.461 1 0 -1 -8 3478.86 318.436 1 0 1 -8 3312.77 303.039 4 0 1 -9 132675. 2084.32 4 0 -1 -9 135099. 2138.08 4 0 1 -9 134203. 2096.31 1 0 -1 -9 138714. 2147.98 1 0 1 -10 28981.4 1036.71 1 0 1 -10 29420.9 1037.85 4 0 -1 -10 30444.9 1100.20 4 0 -1 -10 29481.0 1079.47 1 0 1 -11 653.697 174.925 4 0 -1 -11 369.455 142.992 4 0 1 -11 638.755 181.178 1 0 -1 -11 486.050 155.773 1 0 1 -12 1488.35 262.218 4 0 1 -12 1153.33 258.681 3 0 1 -12 1106.98 236.786 1 0 -1 -12 1224.68 248.174 4 0 -1 -12 1195.75 240.034 1 0 1 -13 4209.72 459.059 4 0 -1 -13 2903.11 382.554 4 0 1 -13 3324.50 433.999 1 0 1 -13 3469.65 474.864 3 0 -1 -13 3240.68 424.676 1 0 1 -14 38.2733 134.600 1 0 1 -14 168.337 138.085 3 0 -1 -14-121.788 139.963 4 0 1 -14 145.597 130.593 4 0 -1 -14 111.180 155.525 1 0 1 -15 190.524 236.600 3 0 -1 -15-122.095 192.690 3 0 2 0 0.54801 8.14950 1 0 -2 1 23438.1 424.513 4 0 2 -1 52790.7 651.689 1 0 -2 -1 53254.2 633.986 1 0 2 -1 52413.5 630.669 4 0 -2 1 11051.6 229.070 3 0 -2 1 24877.2 458.154 1 0 -2 -2 16047.8 381.796 1 0 2 -2 15081.8 377.630 1 0 2 -2 14893.2 367.086 4 0 -2 2 19.5348 26.6437 1 0 2 -2 15879.2 335.659 3 0 -2 3 5604.94 255.663 1 0 -2 3 5151.54 240.759 4 0 2 -3 4919.43 237.897 1 0 2 -3 5344.04 243.467 3 0 2 -3 5082.24 238.596 4 0 -2 4 12409.6 413.952 1 0 -2 4 13045.1 421.021 4 0 2 -4 12207.4 422.331 1 0 2 -4 12957.1 434.786 4 0 -2 5 31849.7 753.257 1 0 -2 5 31330.5 746.493 4 0 2 -5 29167.4 707.359 4 0 2 -5 29778.5 728.352 1 0 -2 6 97.4225 56.9777 4 0 -2 6 221.320 61.0665 2 0 2 -6 113.012 54.7163 1 0 2 -6 100.039 58.3708 4 0 -2 6 62.2125 44.9961 1 0 -2 -6 72.0969 57.4321 4 0 2 -7 14232.1 591.045 1 0 2 -7 12815.7 553.850 4 0 -2 -7 13591.0 586.904 4 0 -2 -8 133.295 72.4660 4 0 2 -8 352.614 109.699 4 0 2 -8-20.4258 61.2088 1 0 -2 8 310.330 130.623 2 0 -2 -9 6801.70 475.884 4 0 2 -9 7753.53 504.311 1 0 2 -9 7298.04 477.964 4 0 -2 -9 7725.35 503.433 1 0 -2 -10 37390.4 1170.15 1 0 -2 -10 35333.5 1163.26 4 0 2 -10 35506.7 1114.44 4 0 2 -10 37492.1 1167.69 1 0 2 -10 33867.6 1189.75 3 0 2 -11 27181.8 1073.26 1 0 2 -11 25970.1 1014.87 4 0 2 -11 24767.5 1084.86 3 0 -2 -11 27601.1 1085.97 1 0 -2 -11 27257.1 1086.21 4 0 2 -12 199.904 136.081 3 0 2 -12 116.706 130.318 1 0 2 -12 108.035 101.677 4 0 -2 -12 307.509 158.190 1 0 -2 -12 481.508 176.615 4 0 2 -13 141.049 128.535 1 0 -2 -13 440.271 186.621 4 0 2 -13 166.441 148.079 4 0 2 -13 67.5633 112.068 3 0 -2 -13 345.340 168.860 1 0 -2 -14 166.198 131.069 4 0 2 -14 114.994 145.114 3 0 -2 -14 60.9738 99.3232 1 0 2 -14 555.439 209.298 1 0 2 -14 515.847 183.874 4 0 2 -15 6252.79 688.871 3 0 3 0-19.6017 14.9860 1 0 -3 0-2.79251 20.7910 1 0 3 -1 55384.2 787.231 1 0 3 -1 55094.8 754.766 4 0 -3 1 56275.0 568.615 3 0 3 1 50963.1 733.563 1 0 -3 -1 56278.8 770.873 1 0 -3 -2 12046.2 382.393 1 0 -3 2 4614.91 236.323 4 0 3 -2 11639.4 371.979 4 0 -3 2 12441.1 319.042 3 0 3 -2 13013.0 406.031 1 0 3 -2 11720.3 314.235 3 0 -3 2 4189.63 231.542 1 0 -3 3 68324.1 975.662 4 0 3 -3 62308.4 834.559 3 0 3 -3 64755.0 959.836 1 0 -3 3 65567.2 973.400 1 0 -3 -3 69149.8 989.970 1 0 3 -3 64595.2 945.126 4 0 -3 4 71700.5 1097.31 1 0 3 -4 71442.4 1094.22 1 0 3 -4 68614.4 1014.18 3 0 -3 4 71431.3 1070.55 4 0 3 -4 70804.3 1066.67 4 0 -3 5 1965.69 193.843 1 0 3 -5 2078.87 198.691 3 0 3 -5 2372.53 209.940 4 0 3 -5 2189.06 204.993 1 0 -3 5 1760.98 181.648 4 0 3 -6 97327.5 1488.32 1 0 3 -6 101601. 1478.50 4 0 3 -7 62334.7 1279.78 1 0 -3 -7 60879.9 1299.66 4 0 3 -7 62652.4 1285.29 3 0 3 -7 65274.4 1280.33 4 0 3 -8 14525.1 670.736 3 0 3 -8 14659.3 659.459 1 0 3 -8 14829.7 650.914 4 0 -3 -8 13274.7 635.976 4 0 3 -9 3872.39 378.690 3 0 3 -9 4611.59 385.171 4 0 -3 -9 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550.303 2 -8 -7 3 4001.13 411.467 4 -8 -7 3 4107.81 434.515 1 -8 7 3 4006.09 444.547 4 -8 7 3 4808.18 496.708 1 -8 7 2 189.451 171.642 1 8 -7 -2-40.2557 148.832 2 -8 -7 2 237.236 122.696 4 -8 -7 2 275.624 151.151 1 -8 7 2 100.971 91.3310 4 8 -7 -1 1325.59 304.140 2 -8 -7 1 1831.89 325.401 1 -8 -7 1 1526.07 311.006 4 -8 7 1 1733.56 285.859 4 -8 7 1 2009.32 346.795 1 8 -7 0 3001.33 446.494 2 -8 -7 0 2753.49 404.639 4 -8 -7 0 3805.27 486.530 1 -8 7 0 3184.06 435.644 4 -8 7 0 3352.06 451.349 1 -8 -7 -1 6670.60 634.392 4 -8 -7 -1 5868.12 618.154 1 -8 7 -1 6302.78 619.150 4 -8 7 -1 6181.81 638.126 1 8 -7 1 5498.79 592.232 2 -8 -7 -2 6667.78 691.197 4 -8 -7 -2 6878.14 689.246 1 -8 7 -2 6502.29 648.017 4 -8 7 -2 6284.17 661.026 1 8 -7 2 6691.00 647.594 2 -8 -7 -3 148.913 174.522 4 -8 7 -3 49.0732 146.322 4 -8 -7 -3 559.345 232.008 1 -8 7 -3 216.616 206.180 1 -8 -7 -4 1114.40 335.026 4 -8 7 -4 1209.67 321.750 4 -8 -7 -4 508.113 264.591 1 -8 7 -4 1102.37 346.090 1 -8 -7 -5 2262.38 485.807 4 -8 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8611.42 721.084 4 -9 8 2 8993.50 756.779 1 -9 8 1 2114.78 407.574 1 -9 -8 1 1722.39 353.873 4 -9 8 1 1848.74 352.073 4 -9 -8 1 1649.34 359.543 1 -9 8 0 403.163 211.739 1 -9 -8 0 286.935 185.216 4 -9 8 0 416.122 222.216 4 -9 -8 0 390.154 242.336 1 -9 -8 -1 1112.66 312.471 4 -9 8 -1 1558.18 381.100 4 -9 -8 -1 1276.58 371.625 1 -9 8 -1 1440.24 373.004 1 -9 -8 -2 1612.93 401.767 4 -9 -8 -2 1567.61 423.829 1 -9 9 6 5083.78 544.148 1 -9 9 5 159.587 141.644 1 -9 9 4 1261.90 321.713 1 -9 9 3 5436.38 576.122 4 -9 9 3 4968.92 561.002 1 -9 9 2 3979.47 524.084 4 -9 9 2 5241.80 604.158 1 -9 -9 1 3376.92 501.528 4 -9 -9 1 3485.28 526.035 1 -9 9 1 3589.77 494.236 4 -9 9 0 2931.58 466.699 4 -9 -9 0 2791.67 492.736 4 -9 -9 0 1867.40 408.507 1 -9 9 0 3719.05 529.908 1 -9 -9 -1 723.422 305.026 4 -9 -9 -1 8.52969 189.626 1 -9 10 6 8430.82 742.460 1 -9 10 5 12152.3 909.866 1 -9 10 4 418.744 250.579 1 -9 10 3 1045.31 313.177 1 -9 10 2 7463.50 719.127 4 -9 10 2 7361.61 714.568 1 -9 -10 1 432.641 235.616 4 -9 -10 0 169.470 214.541 4 -9 -10 0 97.9285 213.651 1 -9 11 5 13346.8 967.625 1 10 0 -13-224.139 257.705 2 10 0 -12 3767.07 648.170 2 10 0 -11 253.597 277.910 2 10 0 -10 1382.94 452.535 2 10 0 -9 131.941 253.556 2 10 0 -8 4392.11 663.879 2 10 0 -7 134.281 214.845 2 10 0 -6 20092.8 1347.94 2 10 0 -5-151.726 151.391 2 -10 0 4 2282.20 310.135 4 -10 0 4 3366.76 390.682 1 -10 0 3 101.036 127.907 1 -10 0 3-24.6159 93.8423 4 -10 0 2 14236.5 843.393 4 -10 0 2 16052.5 912.855 1 -10 0 1-38.7462 94.7557 1 -10 0 1-16.4897 112.887 4 -10 0 0 19099.3 1079.14 4 -10 0 0 20223.3 1112.82 1 -10 0 -1 297.764 220.234 1 -10 0 -1 62.3367 112.940 4 -10 0 -2 1044.47 327.712 1 -10 0 -2 836.507 302.750 4 -10 0 -3-47.4083 146.028 1 -10 0 -3-165.076 176.064 4 10 1 -14 1159.56 417.128 2 10 1 -13 5934.53 778.352 2 10 -1 -12 9494.80 1019.52 2 10 1 -12 8349.24 961.294 2 10 1 -11 533.979 354.551 2 10 -1 -11 287.685 272.082 2 10 1 -10 5117.81 772.080 2 10 -1 -10 5260.57 762.802 2 10 1 -9 2982.80 561.992 2 10 -1 -9 3225.78 595.939 2 10 1 -8 230.008 198.537 2 10 -1 -8 395.294 252.298 2 10 1 -7 2721.39 496.577 2 10 -1 -7 3272.11 582.115 2 10 1 -6 323.329 212.419 2 10 -1 -6 438.498 227.632 2 10 -1 -5 1692.88 420.832 2 -10 1 4 24148.0 1005.86 4 -10 1 4 24016.7 1029.89 1 10 -1 -4 25919.5 1502.30 2 -10 -1 3 5881.52 506.630 4 -10 1 3 5315.75 493.579 4 -10 -1 3 5321.94 499.184 1 -10 1 3 6375.04 556.922 1 10 -1 -3 5044.15 676.780 2 -10 1 2 2131.03 340.079 4 -10 -1 2 996.550 251.301 1 -10 -1 2 1834.82 308.923 4 -10 1 2 1903.97 332.064 1 -10 -1 1 227.129 186.343 1 -10 1 1 279.097 167.562 1 -10 -1 1 59.8087 119.998 4 -10 1 1 344.890 161.277 4 -10 -1 0 74.4945 127.793 1 -10 1 0 175.584 163.711 1 -10 -1 0 587.063 216.960 4 -10 1 0 126.601 145.663 4 -10 -1 -1 2522.28 420.284 4 -10 1 -1 3158.30 470.676 4 -10 -1 -1 3018.25 475.963 1 -10 1 -1 3685.86 519.834 1 -10 1 -2 2164.66 419.325 1 -10 -1 -2 2789.09 489.868 1 -10 -1 -2 2310.97 432.739 4 -10 1 -2 2742.25 453.800 4 -10 -1 -3 1699.33 395.303 1 -10 1 -3 1351.94 351.516 1 -10 -1 -3 1724.49 392.226 4 -10 1 -3 1421.03 353.659 4 10 2 -14 140.280 240.251 2 10 2 -13 10326.3 1027.96 2 10 2 -12 145.765 237.174 2 10 -2 -12 227.288 264.712 2 10 2 -11 694.135 328.795 2 10 -2 -11 1026.64 354.848 2 10 2 -10 1749.48 461.610 2 10 -2 -10 2615.38 557.476 2 10 2 -9 127.730 187.992 2 10 -2 -9 668.928 369.769 2 10 2 -8 331.755 230.550 2 10 -2 -8 34.6887 167.760 2 10 2 -7 1496.51 385.094 2 10 -2 -7 1706.41 419.229 2 10 -2 -6 6356.82 807.116 2 10 -2 -5 282.661 184.028 2 10 -2 -4 378.814 218.274 2 -10 2 4 701.044 190.327 4 -10 2 4 613.460 182.591 1 10 -2 -3 229.168 190.237 2 -10 -2 3 53.9259 115.533 1 -10 -2 3 61.0950 89.7577 4 -10 2 3-101.696 104.063 4 -10 2 3 39.7653 116.350 1 -10 -2 2 7186.18 599.070 4 -10 2 2 9314.16 689.839 4 -10 -2 2 8125.44 649.754 1 -10 2 2 9069.21 699.449 1 10 -2 -2 10133.5 946.173 2 10 -2 -1 619.244 308.753 2 -10 -2 1 333.441 181.317 1 -10 -2 1 588.177 193.041 4 -10 2 1 324.807 179.009 1 -10 2 1 293.327 154.694 4 -10 -2 0 10744.1 808.746 4 -10 2 0 11251.0 827.456 4 -10 -2 0 9908.95 801.993 1 -10 2 0 9709.59 776.591 1 -10 -2 -1 439.288 211.854 1 -10 2 -1 755.987 257.989 1 -10 -2 -1 548.315 220.458 4 -10 2 -1 754.070 227.699 4 -10 -2 -2 1006.37 308.290 1 -10 2 -2 1788.63 397.763 1 -10 -2 -2 1768.97 369.233 4 -10 2 -2 2128.39 409.668 4 -10 -2 -3 42547.5 1845.75 4 -10 2 -3 46518.5 1906.19 4 -10 -2 -3 44257.2 1929.69 1 -10 2 -3 45763.4 1936.20 1 10 3 -13 2404.51 527.479 2 10 3 -12 3312.54 592.465 2 10 -3 -11 8356.52 958.863 2 10 3 -11 8283.09 883.761 2 10 3 -10-42.8871 180.293 2 10 -3 -10 652.421 374.029 2 10 3 -9 4932.99 659.279 2 10 -3 -9 6865.02 885.429 2 10 3 -8 457.375 245.365 2 10 -3 -8 1767.14 461.998 2 10 -3 -7 4241.81 700.456 2 10 -3 -6 46704.4 2194.00 2 10 -3 -5 6812.69 844.613 2 10 -3 -4 2097.82 471.943 2 -10 3 4 2308.99 353.551 4 -10 3 4 2311.40 350.073 1 10 -3 -3-113.756 149.572 2 -10 -3 3 40.7361 132.678 1 -10 -3 3 48.0197 113.482 4 -10 3 3 6.31925 106.532 4 -10 3 3 15.6377 105.524 1 -10 -3 2 1387.13 303.441 1 10 -3 -2 1215.21 363.314 2 -10 -3 2 620.820 190.830 4 -10 3 2 1213.32 275.564 4 -10 3 2 1064.34 256.501 1 -10 -3 1 7950.05 691.343 4 -10 3 1 7122.90 636.989 4 -10 -3 1 9016.24 739.108 1 -10 3 1 7192.39 654.628 1 10 -3 -1 7600.81 822.071 2 -10 -3 0 8697.11 753.443 4 -10 3 0 8570.70 722.530 4 -10 -3 0 7644.56 719.506 1 -10 3 0 9007.81 772.204 1 10 -3 0 7769.68 837.561 2 10 -3 1 865.011 306.319 2 -10 -3 -1 414.533 254.384 4 -10 3 -1 233.336 209.702 1 -10 3 -1 646.929 247.374 4 -10 -3 -1 637.932 240.461 1 -10 -3 -2 8082.58 798.584 4 -10 3 -2 6499.34 696.803 4 -10 -3 -2 8189.01 808.591 1 -10 3 -2 6903.77 725.343 1 10 -3 2 6915.07 775.147 2 10 -3 3 751.090 342.481 2 -10 3 -3 1965.82 431.693 1 -10 -3 -3 1685.77 426.416 4 -10 3 -3 2263.29 446.383 4 -10 -3 -3 2401.73 464.285 1 10 4 -12 556.489 303.066 2 10 4 -11 4209.62 608.290 2 10 -4 -10 11854.3 1145.31 2 10 4 -10 5947.78 717.444 2 10 -4 -9 4943.10 737.675 2 10 4 -9 3785.75 597.257 2 10 -4 -8 22908.5 1574.12 2 10 -4 -7 34146.1 1945.30 2 10 -4 -6 23272.8 1603.74 2 -10 4 5 5179.55 509.065 4 -10 4 5 5006.83 521.168 1 10 -4 -5 5811.77 784.200 2 10 -4 -4 3438.76 597.806 2 -10 4 4 2894.74 398.402 4 -10 4 4 3211.36 426.735 1 10 -4 -3 1935.10 490.890 2 -10 4 3 924.765 231.501 4 -10 4 3 1542.23 299.810 1 10 -4 -2 749.768 297.884 2 -10 -4 2 917.343 238.139 4 -10 4 2 966.645 258.442 4 -10 4 2 1169.74 285.931 1 -10 -4 2 1148.61 296.813 1 10 -4 -1 1733.13 415.809 2 -10 -4 1 1893.68 360.780 4 -10 4 1 2158.01 347.512 4 -10 4 1 1698.02 347.471 1 -10 -4 1 1960.42 355.787 1 -10 4 0 3515.21 474.475 4 -10 -4 0 2894.20 460.719 1 -10 -4 0 2551.36 430.621 4 -10 4 0 2979.82 458.181 1 10 -4 0 3363.18 594.332 2 10 -4 1 111.006 215.977 2 -10 -4 -1 4.99904 148.178 4 -10 4 -1 17.5723 130.470 4 -10 4 -1 306.734 211.015 1 -10 -4 -1 318.198 205.585 1 10 -4 2 236.877 278.735 2 -10 -4 -2-65.1533 147.950 4 -10 4 -2 28.8083 135.878 4 -10 4 -2-81.8920 193.181 1 -10 -4 -2 464.796 272.192 1 -10 -4 -3-172.320 228.201 4 -10 -4 -3 226.887 234.817 1 10 5 -12 1116.72 363.936 2 10 5 -11 117.590 163.407 2 10 5 -10 1909.83 431.933 2 10 -5 -9 8037.93 953.434 2 10 -5 -8 6513.02 856.641 2 10 -5 -7 2342.53 518.813 2 10 -5 -6 8003.79 944.826 2 10 -5 -5-29.9140 205.112 2 -10 5 5 201.263 147.363 1 -10 5 5 219.131 154.133 4 -10 5 4 231.743 179.680 1 10 -5 -4 145.663 219.067 2 -10 5 4 62.4105 110.286 4 10 -5 -3 1703.30 467.184 2 -10 5 3 1109.85 268.473 4 -10 5 3 1325.03 395.342 1 10 -5 -2 566.558 297.439 2 -10 -5 2 677.119 207.817 4 -10 5 2 931.790 261.202 4 -10 5 2 813.728 240.894 1 -10 -5 2 739.388 251.315 1 -10 -5 1 2555.82 418.991 4 10 -5 -1 3120.97 577.497 2 -10 5 1 2876.78 409.437 4 -10 5 1 2423.73 419.041 1 -10 -5 1 2284.26 401.865 1 10 -5 0 577.163 303.794 2 -10 -5 0 750.018 275.651 4 -10 5 0 735.437 259.492 4 -10 5 0 496.913 206.175 1 -10 -5 0 545.439 241.394 1 10 -5 1-136.795 239.415 2 -10 -5 -1 533.513 269.336 4 -10 5 -1-64.2572 124.839 4 -10 5 -1 115.622 191.446 1 -10 -5 -1 219.068 182.975 1 -10 -5 -2 77.8554 156.291 4 -10 5 -2 355.453 240.492 4 -10 5 -2 153.202 195.778 1 -10 -5 -2 21.4758 196.008 1 10 6 -11 883.531 302.842 2 10 6 -10 2743.18 501.855 2 10 -6 -7 351.255 382.766 2 10 -6 -6 6538.45 819.858 2 10 -6 -5 68.9533 165.897 2 -10 6 5 273.426 155.196 1 -10 6 5 324.291 172.652 4 -10 6 4 5425.31 552.252 4 -10 6 4 6059.70 595.291 1 10 -6 -4 5394.37 734.729 2 -10 6 3 9063.22 725.930 4 -10 6 3 11838.2 864.002 1 10 -6 -3 11475.1 1100.43 2 10 -6 -2 2656.50 548.796 2 -10 6 2 3001.29 452.042 4 -10 6 2 2276.36 377.848 1 -10 -6 1 3738.92 501.813 4 -10 6 1 5135.23 581.045 4 -10 -6 1 3632.10 509.323 1 -10 6 1 4168.59 552.330 1 10 -6 -1 4754.82 706.883 2 10 -6 0 77.9633 223.088 2 -10 -6 0-92.7769 178.795 4 -10 6 0 3.96331 149.011 4 -10 -6 0-23.7128 145.362 1 -10 6 0 210.525 215.221 1 10 -6 1 1162.87 372.449 2 -10 -6 -1 1826.21 405.327 4 -10 6 -1 2206.23 425.539 4 -10 -6 -1 1490.22 377.858 1 -10 6 -1 2271.70 437.039 1 -10 -6 -2-32.4435 201.655 4 -10 -6 -2-48.2247 167.055 1 10 -7 -5 730.654 328.404 2 -10 7 5 602.756 250.586 1 -10 7 5 430.347 197.123 4 10 -7 -4 838.501 343.459 2 -10 7 4 538.399 228.845 1 -10 7 4 564.638 238.017 4 10 -7 -3 77.3117 179.731 2 -10 7 3 145.339 171.712 1 -10 7 3 82.2847 150.584 4 -10 7 2 2160.82 408.665 1 10 -7 -2 2202.51 484.285 2 -10 7 2 2004.32 381.642 4 -10 7 1 1047.49 325.727 1 10 -7 -1 466.450 270.068 2 -10 -7 1 980.825 290.414 4 -10 7 1 1181.04 318.418 4 -10 -7 1 274.764 151.663 1 -10 -7 0 6419.32 725.059 4 -10 7 0 7678.41 748.532 4 -10 -7 0 6921.15 803.043 1 -10 7 0 5774.62 674.091 1 10 -7 0 6713.44 775.480 2 -10 -7 -1 5071.65 676.504 4 -10 -7 -1 5033.05 728.332 1 -10 8 5 6752.43 673.864 1 -10 8 4 2469.55 418.315 1 -10 8 4 2371.32 414.163 4 -10 8 3 1038.55 310.095 1 -10 8 3 918.057 255.894 4 -10 8 2 436.057 210.964 1 -10 8 2 66.1571 141.830 4 -10 8 1 3753.65 514.844 4 -10 8 1 4244.95 571.818 1 -10 -8 0 9325.26 930.502 4 -10 9 5 23869.7 1318.68 1 -10 9 4-125.292 212.136 1 -10 9 3 863.488 285.045 1 -10 9 3 1438.29 347.950 4 11 0 -11 63.7280 217.677 2 11 0 -10 1952.27 547.648 2 11 0 -9 5.28592 211.148 2 11 0 -8 6967.01 857.549 2 11 0 -7 362.141 261.019 2 11 0 -6 8891.38 939.367 2 11 0 -5-82.8487 156.402 2 11 0 -4 13296.7 1117.69 2 -11 0 2 2600.88 399.536 4 -11 0 2 2916.95 426.287 1 -11 0 1-246.814 189.535 1 -11 0 1 51.2821 159.613 4 -11 0 0 174.716 169.659 1 -11 0 0 299.205 175.828 4 -11 0 -1-162.446 185.859 1 -11 0 -1 62.0557 192.612 4 11 1 -11 2961.05 589.526 2 11 1 -10 2359.78 563.028 2 11 -1 -10 2500.81 577.723 2 11 1 -9 6232.77 825.487 2 11 -1 -9 7951.59 981.671 2 11 1 -8 3445.64 591.883 2 11 -1 -8 3078.43 592.281 2 11 1 -7 4468.36 681.091 2 11 -1 -7 4008.25 686.848 2 11 1 -6 984.388 357.126 2 11 -1 -6 1624.28 449.853 2 11 -1 -5 262.322 206.110 2 11 -1 -4 4203.25 648.275 2 11 -1 -3 122.182 240.109 2 -11 -1 2 9464.62 737.761 4 -11 1 2 9047.76 721.224 4 -11 -1 2 7390.55 684.755 1 -11 1 2 10220.0 783.310 1 11 -1 -2 7976.15 878.082 2 -11 -1 1 196.756 181.306 1 -11 1 1 208.713 219.146 1 -11 -1 1 80.0263 142.812 4 -11 1 1-91.8855 117.623 4 -11 -1 0 851.854 295.436 1 -11 1 0 1261.85 332.759 1 -11 -1 0 2010.35 414.792 4 -11 1 0 1474.02 331.741 4 -11 -1 -1 342.801 295.565 1 -11 1 -1 175.007 175.469 1 -11 -1 -1-12.8575 176.823 4 -11 1 -1 346.543 241.926 4 11 2 -11 638.660 304.816 2 11 2 -10 513.226 331.055 2 11 -2 -10 292.623 361.738 2 11 2 -9 2864.42 568.391 2 11 -2 -9 4382.47 757.627 2 11 2 -8 6710.27 842.704 2 11 -2 -8 8254.19 1019.41 2 11 2 -7 14452.9 1177.73 2 11 -2 -7 17534.6 1406.54 2 11 -2 -6 2084.66 514.211 2 11 -2 -5 2499.13 533.339 2 11 -2 -4 3486.21 619.322 2 11 -2 -3 1282.07 382.890 2 11 -2 -2 254.927 198.302 2 -11 2 2 732.795 242.141 4 -11 2 2 944.823 305.747 1 11 -2 -1 1237.39 411.670 2 -11 -2 1 715.012 264.591 1 -11 -2 1 745.545 262.097 4 -11 2 1 418.651 182.964 4 -11 2 1 740.087 260.344 1 11 -2 0 1338.46 365.398 2 -11 -2 0 1089.08 352.865 1 -11 -2 0 1615.92 382.883 4 -11 2 0 1293.47 354.691 1 -11 2 0 1919.93 406.854 4 11 -2 1 1605.73 469.160 2 -11 -2 -1 1303.13 401.396 1 -11 2 -1 1784.04 393.672 1 -11 -2 -1 1318.02 352.122 4 -11 2 -1 2139.15 429.006 4 11 3 -11-8.45090 209.731 2 11 3 -10 467.134 276.487 2 11 3 -9 402.844 319.219 2 11 -3 -9 1022.84 423.917 2 11 3 -8 445.671 276.258 2 11 -3 -8-38.7730 241.850 2 11 -3 -7 13116.3 1253.30 2 11 -3 -6 9190.56 1049.24 2 11 -3 -5-81.6698 186.417 2 11 -3 -4 1672.22 455.437 2 11 -3 -3 1878.14 477.041 2 -11 3 3 1659.04 322.135 4 -11 3 3 2285.83 374.462 1 11 -3 -2 1192.52 404.051 2 -11 3 2 1709.47 339.287 4 -11 3 2 1692.53 345.130 1 11 -3 -1 3082.19 573.423 2 -11 -3 1 2908.82 454.100 4 -11 3 1 4114.66 509.838 4 -11 -3 1 3150.99 492.036 1 -11 3 1 3693.18 506.123 1 11 -3 0 320.150 305.584 2 -11 -3 0-113.342 201.637 1 -11 -3 0 240.184 204.817 4 -11 3 0 243.962 168.593 4 -11 3 0 186.363 217.124 1 11 -3 1 3624.70 632.236 2 -11 -3 -1 2846.66 554.168 1 -11 -3 -1 3193.25 531.767 4 11 4 -11 1938.12 487.287 2 11 4 -10 1336.11 410.668 2 11 4 -9 6250.24 771.214 2 11 -4 -8 12473.3 1244.90 2 11 -4 -7 2552.11 617.994 2 11 -4 -6 5906.91 881.979 2 11 -4 -5 1950.13 571.323 2 11 -4 -4 1688.54 467.196 2 11 -4 -3 183.487 234.867 2 -11 4 3 510.614 226.148 4 -11 4 3 180.813 169.545 1 11 -4 -2 2407.91 567.143 2 -11 4 2 1802.58 349.263 4 -11 4 2 1648.40 369.511 1 11 -4 -1 1630.62 467.598 2 -11 4 1 1786.14 337.910 4 -11 4 1 1165.32 311.689 1 -11 -4 0 343.218 245.666 1 -11 -4 0 490.395 273.311 4 -11 4 0 168.042 230.957 4 -11 4 0-109.678 156.528 1 -11 -4 -1 10008.4 932.867 4 -11 -4 -1 11009.6 1035.52 1 11 -4 1 9327.35 985.693 2 11 5 -9 459.307 294.168 2 11 -5 -6 90.5338 224.361 2 11 -5 -5 10924.7 1181.60 2 11 -5 -4 1203.92 458.710 2 11 -5 -3 303.593 310.483 2 -11 5 3 144.267 183.603 4 -11 5 3 242.799 229.740 1 -11 5 2 86.4418 148.516 4 -11 5 2 31.0856 153.694 1 11 -5 -1 1835.18 536.564 2 -11 5 1 2593.39 428.659 4 -11 5 1 2425.01 444.113 1 11 -5 0 1264.16 464.490 2 -11 6 3 370.756 192.886 1 -11 6 3 770.170 253.610 4 -11 6 2 420.150 216.308 4 -11 6 2 182.553 192.867 1 0 0 0 0.00 0.00 0 TITL DM-TA-53_Mo in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 8.531048 11.128502 12.048073 90.0000 110.3328 90.0000 ZERR 9.00 0.000354 0.000506 0.000569 0.0000 0.0051 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 99.00 90.00 9.00 9.00 TREF HKLF 4 END ; _shelx_hkl_checksum 39290 _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 - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.811 _oxdiff_exptl_absorpt_empirical_full_min 0.735 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 O001 O 0.39602(13) 0.38502(10) 0.28280(9) 0.0163(3) Uani 1 1 d . . . . . O002 O 0.27780(13) 0.42737(10) 0.70626(9) 0.0176(3) Uani 1 1 d . . . . . O003 O 0.56298(13) 0.13241(10) 0.52863(10) 0.0208(3) Uani 1 1 d . . . . . O004 O 0.64041(13) 0.24350(10) 0.40924(10) 0.0197(3) Uani 1 1 d . . . . . N005 N 0.06404(15) 0.28644(12) 0.64695(11) 0.0158(3) Uani 1 1 d . . . . . N006 N 0.55422(15) 0.22513(12) 0.47047(11) 0.0142(3) Uani 1 1 d . . . . . C007 C 0.31987(19) 0.46910(15) 0.18864(13) 0.0182(4) Uani 1 1 d . . . . . H00A H 0.3625 0.4552 0.1240 0.027 Uiso 1 1 calc R U . . . H00B H 0.3470 0.5513 0.2184 0.027 Uiso 1 1 calc R U . . . H00C H 0.1983 0.4581 0.1595 0.027 Uiso 1 1 calc R U . . . C008 C 0.40523(17) 0.32424(14) 0.58432(13) 0.0139(4) Uani 1 1 d . . . . . H008 H 0.4566 0.2693 0.6467 0.017 Uiso 1 1 calc R U . . . C009 C 0.21985(18) 0.49002(14) 0.50487(13) 0.0153(4) Uani 1 1 d . . . . . H009 H 0.1452 0.5492 0.5144 0.018 Uiso 1 1 calc R U . . . C00A C -0.05175(18) 0.22238(15) 0.67461(14) 0.0178(4) Uani 1 1 d . . . . . H00D H -0.1199 0.1680 0.6172 0.021 Uiso 1 1 calc R U . . . C00B C 0.25026(17) 0.48258(14) 0.39921(13) 0.0146(4) Uani 1 1 d . . . . . H00E H 0.1950 0.5363 0.3365 0.018 Uiso 1 1 calc R U . . . C00C C 0.02385(19) 0.31111(15) 0.86568(14) 0.0210(4) Uani 1 1 d . . . . . H00F H 0.0105 0.3192 0.9404 0.025 Uiso 1 1 calc R U . . . C00D C 0.15694(17) 0.36081(14) 0.72877(13) 0.0141(4) Uani 1 1 d . . . . . C00E C 0.36096(17) 0.39724(14) 0.38379(13) 0.0128(4) Uani 1 1 d . . . . . C00F C 0.43678(17) 0.31821(14) 0.47850(13) 0.0134(4) Uani 1 1 d . . . . . C00G C 0.29803(18) 0.41149(14) 0.59654(13) 0.0149(4) Uani 1 1 d . . . . . C00H C 0.14259(19) 0.37795(15) 0.83970(13) 0.0179(4) Uani 1 1 d . . . . . H00H H 0.2120 0.4335 0.8950 0.021 Uiso 1 1 calc R U . . . C00I C -0.07669(19) 0.23137(15) 0.78125(15) 0.0210(4) Uani 1 1 d . . . . . H00I H -0.1599 0.1847 0.7970 0.025 Uiso 1 1 calc R U . . . 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 O001 0.0198(6) 0.0174(6) 0.0129(6) 0.0013(4) 0.0071(4) 0.0023(4) O002 0.0181(5) 0.0242(7) 0.0132(6) -0.0051(4) 0.0089(5) -0.0044(4) O003 0.0206(6) 0.0161(6) 0.0265(7) 0.0060(5) 0.0092(5) 0.0028(4) O004 0.0196(6) 0.0237(7) 0.0209(6) 0.0014(5) 0.0135(5) 0.0017(4) N005 0.0140(6) 0.0191(7) 0.0145(7) 0.0009(5) 0.0051(5) 0.0023(5) N006 0.0135(6) 0.0155(7) 0.0129(6) -0.0013(5) 0.0036(5) -0.0019(5) C007 0.0232(8) 0.0189(9) 0.0121(7) 0.0028(6) 0.0058(6) 0.0002(6) C008 0.0125(7) 0.0157(8) 0.0132(7) 0.0000(6) 0.0042(6) -0.0047(6) C009 0.0126(7) 0.0154(8) 0.0188(8) -0.0036(6) 0.0064(6) -0.0020(6) C00A 0.0141(7) 0.0182(9) 0.0217(8) 0.0038(6) 0.0069(6) 0.0028(6) C00B 0.0135(7) 0.0146(8) 0.0145(8) 0.0009(6) 0.0032(6) -0.0025(6) C00C 0.0237(8) 0.0273(10) 0.0157(8) 0.0087(7) 0.0116(7) 0.0116(7) C00D 0.0128(7) 0.0164(8) 0.0142(7) 0.0041(6) 0.0061(6) 0.0055(6) C00E 0.0129(7) 0.0147(8) 0.0117(8) -0.0027(6) 0.0054(6) -0.0049(6) C00F 0.0104(7) 0.0131(8) 0.0163(8) -0.0024(6) 0.0042(6) -0.0030(6) C00G 0.0143(7) 0.0192(8) 0.0131(8) -0.0042(6) 0.0070(6) -0.0058(6) C00H 0.0185(8) 0.0219(9) 0.0125(8) 0.0013(6) 0.0043(6) 0.0078(6) C00I 0.0185(8) 0.0218(9) 0.0263(9) 0.0104(7) 0.0124(7) 0.0064(6) 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' O O 0.0106 0.0060 '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 C00E O001 C007 117.50(12) . . ? C00D O002 C00G 117.76(12) . . ? C00D N005 C00A 116.59(13) . . ? O003 N006 C00F 117.41(12) . . ? O004 N006 O003 123.37(13) . . ? O004 N006 C00F 119.20(12) . . ? O001 C007 H00A 109.5 . . ? O001 C007 H00B 109.5 . . ? O001 C007 H00C 109.5 . . ? H00A C007 H00B 109.5 . . ? H00A C007 H00C 109.5 . . ? H00B C007 H00C 109.5 . . ? C00F C008 H008 120.7 . . ? C00G C008 H008 120.7 . . ? C00G C008 C00F 118.60(14) . . ? C00B C009 H009 119.9 . . ? C00G C009 H009 119.9 . . ? C00G C009 C00B 120.17(14) . . ? N005 C00A H00D 118.1 . . ? N005 C00A C00I 123.73(15) . . ? C00I C00A H00D 118.1 . . ? C009 C00B H00E 119.6 . . ? C009 C00B C00E 120.89(14) . . ? C00E C00B H00E 119.6 . . ? C00H C00C H00F 120.3 . . ? C00H C00C C00I 119.44(15) . . ? C00I C00C H00F 120.3 . . ? O002 C00D C00H 115.95(14) . . ? N005 C00D O002 119.26(13) . . ? N005 C00D C00H 124.80(14) . . ? O001 C00E C00B 123.88(13) . . ? O001 C00E C00F 118.82(13) . . ? C00B C00E C00F 117.29(14) . . ? C008 C00F N006 116.60(13) . . ? C008 C00F C00E 122.10(14) . . ? C00E C00F N006 121.30(13) . . ? C008 C00G O002 119.58(14) . . ? C008 C00G C009 120.92(14) . . ? C009 C00G O002 119.31(14) . . ? C00C C00H C00D 117.36(15) . . ? C00C C00H H00H 121.3 . . ? C00D C00H H00H 121.3 . . ? C00A C00I C00C 118.08(15) . . ? C00A C00I H00I 121.0 . . ? C00C C00I H00I 121.0 . . ? 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 O001 C007 1.4395(18) . ? O001 C00E 1.3569(18) . ? O002 C00D 1.3710(19) . ? O002 C00G 1.4025(19) . ? O003 N006 1.2349(17) . ? O004 N006 1.2261(17) . ? N005 C00A 1.351(2) . ? N005 C00D 1.320(2) . ? N006 C00F 1.467(2) . ? C007 H00A 0.9800 . ? C007 H00B 0.9800 . ? C007 H00C 0.9800 . ? C008 H008 0.9500 . ? C008 C00F 1.393(2) . ? C008 C00G 1.376(2) . ? C009 H009 0.9500 . ? C009 C00B 1.387(2) . ? C009 C00G 1.384(2) . ? C00A H00D 0.9500 . ? C00A C00I 1.377(2) . ? C00B H00E 0.9500 . ? C00B C00E 1.397(2) . ? C00C H00F 0.9500 . ? C00C C00H 1.377(2) . ? C00C C00I 1.397(2) . ? C00D C00H 1.397(2) . ? C00E C00F 1.407(2) . ? C00H H00H 0.9500 . ? C00I H00I 0.9500 . ? 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 O001 C00E C00F N006 1.1(2) . . . . ? O001 C00E C00F C008 -179.16(12) . . . . ? O002 C00D C00H C00C -179.11(13) . . . . ? O003 N006 C00F C008 29.26(17) . . . . ? O003 N006 C00F C00E -150.96(13) . . . . ? O004 N006 C00F C008 -149.28(13) . . . . ? O004 N006 C00F C00E 30.50(19) . . . . ? N005 C00A C00I C00C -0.2(2) . . . . ? N005 C00D C00H C00C 0.8(2) . . . . ? C007 O001 C00E C00B 3.0(2) . . . . ? C007 O001 C00E C00F -178.46(12) . . . . ? C009 C00B C00E O001 179.87(13) . . . . ? C009 C00B C00E C00F 1.3(2) . . . . ? C00A N005 C00D O002 179.34(12) . . . . ? C00A N005 C00D C00H -0.5(2) . . . . ? C00B C009 C00G O002 174.18(12) . . . . ? C00B C009 C00G C008 -0.7(2) . . . . ? C00B C00E C00F N006 179.70(12) . . . . ? C00B C00E C00F C008 -0.5(2) . . . . ? C00D O002 C00G C008 -88.77(16) . . . . ? C00D O002 C00G C009 96.25(16) . . . . ? C00D N005 C00A C00I 0.2(2) . . . . ? C00F C008 C00G O002 -173.41(12) . . . . ? C00F C008 C00G C009 1.5(2) . . . . ? C00G O002 C00D N005 -0.83(19) . . . . ? C00G O002 C00D C00H 179.05(12) . . . . ? C00G C008 C00F N006 178.92(13) . . . . ? C00G C008 C00F C00E -0.9(2) . . . . ? C00G C009 C00B C00E -0.7(2) . . . . ? C00H C00C C00I C00A 0.4(2) . . . . ? C00I C00C C00H C00D -0.7(2) . . . . ?