#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:54:14 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225918 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515806.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_4515806 loop_ _publ_author_name 'Messinis, Antonis M.' 'Batsanov, Andrei S.' 'Wright, William R. H.' 'Howard, Judith A. K.' 'Hanton, Martin J.' 'Dyer, Philip W.' _publ_section_title ; Bis(Imido) Tungsten Complexes: Efficient Precatalysts for the Homogeneous Dimerization of Ethylene ; _journal_issue 12 _journal_name_full 'ACS Catalysis' _journal_page_first 11249 _journal_paper_doi 10.1021/acscatal.8b02202 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C16 H10 Cl2 F10 N2 O2 W' _chemical_formula_sum 'C16 H10 Cl2 F10 N2 O2 W' _chemical_formula_weight 707.01 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2017-11-08 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 87.953(7) _cell_angle_beta 81.828(7) _cell_angle_gamma 87.079(7) _cell_formula_units_Z 2 _cell_length_a 7.3379(3) _cell_length_b 7.8387(4) _cell_length_c 17.8616(8) _cell_measurement_reflns_used 9984 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 34.773 _cell_measurement_theta_min 2.305 _cell_volume 1015.22(8) _computing_cell_refinement 'SAINT v7.46A (Bruker, 2008)' _computing_data_collection 'SMART v5.630 (Bruker, 2003)' _computing_data_reduction 'SAINT v7.46A (Bruker, 2008)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2016/6 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 5.6 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.946 _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.946 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 23707 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.946 _diffrn_reflns_theta_full 32.500 _diffrn_reflns_theta_max 34.959 _diffrn_reflns_theta_min 1.152 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 35.0 _diffrn_source_power 1.75 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.061 _exptl_absorpt_correction_T_max 0.6519 _exptl_absorpt_correction_T_min 0.4938 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; SADABS-2009/1 (Bruker,2010) was used for absorption correction. wR2(int) was 0.0549 before and 0.0347 after correction. The Ratio of minimum to maximum transmission is 0.7575. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 2.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 668 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.290 _refine_diff_density_min -1.177 _refine_diff_density_rms 0.120 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 302 _refine_ls_number_reflns 8443 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0200 _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^)+(0.0247P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0464 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7664 _reflns_number_total 8443 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file W-bisimido.cif _cod_data_source_block 10_12srv099 _cod_database_code 4515806 _shelx_shelxl_version_number 2016/6 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups 2. Others Uiso(H4A)=Uiso(H4B)=Uiso(H4C)=FVAR(1) Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(2) 3.a Riding coordinates: C2(H2A,H2B), C3(H3A,H3B) 3.b Rotating group: C1(H1A,H1B,H1C), C4(H4A,H4B,H4C) ; _shelx_res_file ; TITL 12srv099 in P-1 #2 12srv099.res created by SHELXL-2016/6 at 15:36:02 on 08-Nov-2017 REM reset to P-1 #2 CELL 0.71073 7.3379 7.8387 17.8616 87.953 81.828 87.079 ZERR 2 0.0003 0.0004 0.0008 0.007 0.007 0.007 LATT 1 SFAC C H Cl F N O W UNIT 32 20 4 20 4 4 2 L.S. 7 PLAN 6 TEMP -153.15 BOND $H fmap 2 acta 65 REM REM REM WGHT 0.024700 FVAR 0.40334 0.03863 0.02807 W 7 0.302689 0.223701 0.247092 11.00000 0.01376 0.01289 = 0.01397 -0.00136 -0.00315 -0.00131 CL1 3 0.010924 0.355345 0.293145 11.00000 0.01924 0.02508 = 0.02580 -0.00260 0.00018 0.00507 CL2 3 0.521860 0.005810 0.202137 11.00000 0.01697 0.01729 = 0.02203 -0.00331 -0.00063 0.00148 F1 4 0.640204 0.166816 0.425576 11.00000 0.03311 0.01287 = 0.03324 0.00071 -0.01421 0.00007 F2 4 0.828643 0.377227 0.498756 11.00000 0.02786 0.02783 = 0.03126 0.00014 -0.01797 0.00016 F3 4 0.797399 0.720539 0.473918 11.00000 0.02780 0.02538 = 0.03227 -0.00957 -0.01171 -0.00802 F4 4 0.574767 0.853151 0.375845 11.00000 0.04111 0.01276 = 0.04243 -0.00160 -0.01684 -0.00420 F5 4 0.388537 0.643427 0.299768 11.00000 0.03771 0.01703 = 0.03107 0.00197 -0.02037 0.00077 F6 4 0.152602 0.526640 0.066396 11.00000 0.01567 0.02711 = 0.03032 0.00296 -0.00765 -0.00223 F7 4 0.288996 0.776296 -0.029490 11.00000 0.02867 0.02773 = 0.02550 0.00781 -0.01238 0.00276 F8 4 0.635500 0.882742 -0.024734 11.00000 0.02926 0.02035 = 0.02340 0.00546 0.00192 -0.00207 F9 4 0.833180 0.751530 0.081960 11.00000 0.01787 0.02569 = 0.03234 -0.00040 -0.00542 -0.00684 F10 4 0.696553 0.504518 0.180630 11.00000 0.02311 0.02719 = 0.02508 0.00449 -0.01262 -0.00113 O1 6 0.177775 0.001952 0.323055 11.00000 0.01854 0.01958 = 0.01603 -0.00073 -0.00210 -0.00499 O2 6 0.127613 0.069052 0.180228 11.00000 0.01911 0.02079 = 0.01929 0.00090 -0.00871 -0.00517 N1 5 0.415822 0.292485 0.320315 11.00000 0.01735 0.01542 = 0.01871 -0.00229 -0.00446 -0.00093 N2 5 0.354369 0.373269 0.172422 11.00000 0.01757 0.01535 = 0.01942 -0.00057 -0.00283 0.00112 C1 1 0.147688 0.015396 0.404380 11.00000 0.03081 0.02662 = 0.01620 0.00218 -0.00160 -0.00433 AFIX 7 H1A 2 0.258347 0.056797 0.421348 11.00000 31.00000 H1B 2 0.121334 -0.097164 0.427910 11.00000 31.00000 H1C 2 0.042962 0.095676 0.419042 11.00000 31.00000 AFIX 0 C2 1 0.031184 -0.084076 0.296205 11.00000 0.02120 0.02317 = 0.02590 0.00198 -0.00387 -0.00857 AFIX 3 H2A 2 -0.087176 -0.017296 0.307415 11.00000 -1.20000 H2B 2 0.017524 -0.198816 0.320775 11.00000 -1.20000 AFIX 0 C3 1 0.085349 -0.098476 0.212276 11.00000 0.02811 0.01929 = 0.02480 -0.00142 -0.00922 -0.00885 AFIX 3 H3A 2 0.194429 -0.178056 0.201676 11.00000 -1.20000 H3B 2 -0.017001 -0.143596 0.189426 11.00000 -1.20000 AFIX 0 C4 1 -0.009523 0.145752 0.137544 11.00000 0.02009 0.03076 = 0.02818 0.00313 -0.01221 -0.00418 AFIX 7 H4A 2 -0.127830 0.158128 0.170530 11.00000 21.00000 H4B 2 -0.022702 0.072747 0.095397 11.00000 21.00000 H4C 2 0.028753 0.258491 0.117686 11.00000 21.00000 AFIX 0 C5 1 0.509897 0.397811 0.359320 11.00000 0.01572 0.01493 = 0.01478 -0.00246 -0.00313 -0.00127 C6 1 0.622441 0.334905 0.412089 11.00000 0.01793 0.01309 = 0.01657 -0.00106 -0.00377 -0.00062 C7 1 0.719634 0.441665 0.450096 11.00000 0.01417 0.02017 = 0.01766 -0.00118 -0.00536 0.00035 C8 1 0.703855 0.616176 0.437370 11.00000 0.01760 0.01807 = 0.01986 -0.00551 -0.00337 -0.00388 C9 1 0.591276 0.683470 0.386988 11.00000 0.02368 0.01345 = 0.02268 -0.00299 -0.00455 -0.00218 C10 1 0.496576 0.575657 0.348318 11.00000 0.01999 0.01515 = 0.01822 -0.00041 -0.00580 -0.00079 C11 1 0.420125 0.507056 0.126640 11.00000 0.01792 0.01438 = 0.01469 -0.00118 -0.00166 0.00104 C12 1 0.319626 0.582669 0.072230 11.00000 0.01531 0.01818 = 0.01898 -0.00259 -0.00412 0.00224 C13 1 0.388213 0.710402 0.022566 11.00000 0.02113 0.01663 = 0.01666 0.00079 -0.00463 0.00273 C14 1 0.562910 0.765770 0.025244 11.00000 0.02247 0.01495 = 0.01590 -0.00017 -0.00029 0.00003 C15 1 0.665703 0.695274 0.078923 11.00000 0.01593 0.01613 = 0.02032 -0.00228 -0.00318 -0.00016 C16 1 0.594852 0.569606 0.129318 11.00000 0.01807 0.01671 = 0.01679 -0.00147 -0.00577 0.00202 HKLF 4 REM 12srv099 in P-1 #2 REM R1 = 0.0200 for 7664 Fo > 4sig(Fo) and 0.0247 for all 8443 data REM 302 parameters refined using 0 restraints END WGHT 0.0247 0.0000 REM Highest difference peak 1.290, deepest hole -1.177, 1-sigma level 0.120 Q1 1 0.2752 0.1664 0.2790 11.00000 0.05 1.29 Q2 1 0.3157 0.2833 0.2058 11.00000 0.05 1.22 Q3 1 0.3839 0.2076 0.2227 11.00000 0.05 1.02 Q4 1 0.0939 0.3247 0.2593 11.00000 0.05 1.00 Q5 1 0.6072 0.7369 0.0585 11.00000 0.05 0.70 Q6 1 0.0510 -0.0956 0.2526 11.00000 0.05 0.69 ; _shelx_res_checksum 6143 _shelx_hkl_file ; -1 0 0 2231.51 49.9428 2 -1 0 0 2204.71 49.7986 3 -1 0 0 2235.11 54.4148 5 -1 0 0 2337.69 47.0745 1 1 0 0 2221.83 46.5521 1 1 0 0 2211.08 50.3441 3 1 0 0 2271.17 53.0930 5 1 0 0 2267.75 53.8722 2 -2 0 0 805.432 18.4048 1 -2 0 0 818.560 17.8304 5 2 0 0 796.144 18.2527 3 2 0 0 824.440 17.8522 2 2 0 0 797.314 17.5795 5 -3 0 0 2053.41 43.5087 1 -3 0 0 2037.60 42.4896 5 3 0 0 1939.57 42.0286 5 3 0 0 2015.05 43.2878 3 3 0 0 1994.03 42.2579 2 -4 0 0 2.08173 1.21699 5 -4 0 0 3.22137 2.93465 1 4 0 0 2.59015 2.19053 2 4 0 0 2.97431 2.90025 3 4 0 0 3.00112 1.43179 5 -5 0 0 704.807 19.4618 1 5 0 0 681.647 18.6687 3 5 0 0 687.617 18.0456 2 -6 0 0 932.444 25.1539 1 6 0 0 918.101 24.3777 3 6 0 0 905.693 23.4107 2 -7 0 0 743.898 23.0962 1 7 0 0 776.956 22.3277 3 7 0 0 772.539 21.6135 2 -8 0 0 269.219 13.9215 1 8 0 0 293.121 12.5348 2 8 0 0 307.214 13.4554 3 -9 0 0 49.9171 8.50296 1 9 0 0 55.8701 7.39724 2 9 0 0 48.4805 7.91367 3 -10 0 0 495.418 21.2190 1 10 0 0 470.379 19.6999 3 10 0 0 488.663 18.8186 2 -11 0 0 31.8066 9.78558 1 11 0 0 49.8060 8.68836 2 11 0 0 37.5080 8.85620 3 11 -1 0 121.550 12.6307 3 -11 1 0 116.501 12.7272 1 10 -1 0 49.6354 8.61462 3 10 -1 0 45.9254 7.72823 2 -10 1 0 44.8927 9.12360 1 9 -1 0 441.215 16.3455 2 9 -1 0 404.202 17.1488 3 -9 1 0 393.117 18.1924 1 8 -1 0 85.9256 8.38445 3 8 -1 0 92.0565 7.83456 2 -8 1 0 92.7365 9.25349 1 7 -1 0 310.220 13.2925 3 7 -1 0 332.695 12.3289 2 -7 1 0 295.813 13.6619 1 6 -1 0 713.147 19.2687 2 6 -1 0 711.780 20.4890 3 -6 1 0 691.332 20.6815 1 5 -1 0 130.060 6.71889 2 5 -1 0 122.068 7.60150 3 -5 1 0 127.515 7.53481 1 4 -1 0 960.067 23.5639 3 4 -1 0 952.538 22.4975 2 -4 1 0 971.594 23.7082 1 3 -1 0 772.204 17.9530 2 3 -1 0 794.219 18.9543 3 -3 1 0 747.360 18.7194 1 2 -1 0 574.908 13.1480 2 2 -1 0 566.592 12.5284 5 2 -1 0 556.145 12.6795 5 2 -1 0 563.228 13.8148 3 -2 1 0 550.964 13.6076 1 -2 1 0 565.446 13.2889 4 1 -1 0 5076.98 111.835 4 1 -1 0 4993.17 109.265 5 1 -1 0 4831.61 110.614 3 1 -1 0 5041.92 105.200 1 -1 1 0 5083.43 113.497 2 -1 1 0 4951.72 106.548 4 -1 1 0 5025.73 108.287 1 -1 1 0 5098.48 109.554 5 0 -1 0 18.0917 1.51991 1 0 -1 0 16.8090 1.50747 5 0 -1 0 16.7444 1.42049 3 0 -1 0 16.4086 1.40659 2 0 1 0 15.5443 1.74918 2 0 1 0 16.4069 1.65591 1 0 1 0 19.4020 2.03144 5 -1 -1 0 2282.02 49.1253 1 -1 -1 0 2225.06 49.9590 5 -1 -1 0 2168.08 46.7343 3 1 1 0 2225.41 49.6995 3 1 1 0 2277.50 46.7236 5 1 1 0 2215.90 49.5788 2 -2 -1 0 1589.99 33.5544 1 -2 -1 0 1558.79 33.2603 5 2 1 0 1550.85 33.2180 3 2 1 0 1531.55 32.8074 2 -3 -1 0 90.2116 5.34126 1 3 1 0 84.3368 4.84127 3 3 1 0 76.4940 4.49503 2 -4 -1 0 690.228 16.2601 5 -4 -1 0 683.035 18.3045 1 4 1 0 682.967 17.2383 2 4 1 0 704.582 17.5963 3 -5 -1 0 76.7940 4.24958 5 -5 -1 0 91.2550 7.03924 1 5 1 0 78.7840 5.70145 2 5 1 0 78.4860 6.18420 3 -6 -1 0 816.452 23.4557 1 -6 -1 0 822.915 19.4971 5 6 1 0 837.963 21.9886 2 6 1 0 882.577 22.6786 3 -7 -1 0 634.753 20.3339 1 7 1 0 593.218 18.2306 2 7 1 0 599.700 18.8246 3 -8 -1 0 221.487 12.6409 1 8 1 0 192.403 11.0786 3 8 1 0 202.107 10.3368 2 -9 -1 0 483.608 20.0053 1 9 1 0 482.903 17.7381 2 9 1 0 494.590 18.3408 3 -10 -1 0 49.9143 9.78580 1 10 1 0 55.3910 8.54622 3 10 1 0 54.3158 8.06654 2 -11 -1 0 165.688 14.5601 1 11 1 0 114.342 10.8716 2 11 -2 0 56.1763 10.1151 3 -11 2 0 66.2211 11.0150 1 10 -2 0 306.924 16.3883 3 -10 2 0 317.591 17.3326 1 9 -2 0 42.1137 7.99385 3 9 -2 0 41.4027 6.90032 2 -9 2 0 60.1992 9.05971 1 8 -2 0 515.197 19.1013 3 8 -2 0 548.728 18.0043 2 -8 2 0 537.620 19.7692 1 7 -2 0 261.463 11.1774 2 7 -2 0 258.035 12.6077 3 -7 2 0 246.340 12.6115 1 6 -2 0 326.710 11.8188 2 6 -2 0 323.776 12.9862 3 -6 2 0 328.460 13.0020 1 5 -2 0 114.664 6.53111 2 5 -2 0 101.710 7.44170 3 -5 2 0 109.198 7.35855 1 4 -2 0 13.2885 3.48436 3 4 -2 0 14.0573 3.01104 2 -4 2 0 13.2084 3.29245 1 3 -2 0 3122.74 66.4652 5 3 -2 0 3315.80 67.1720 5 3 -2 0 3207.51 68.3099 3 -3 2 0 3218.99 67.9116 1 2 -2 0 1122.96 23.9353 5 2 -2 0 1077.26 24.9189 3 2 -2 0 1125.86 24.4887 4 -2 2 0 1070.58 24.2552 2 -2 2 0 1087.37 24.5334 1 1 -2 0 1454.22 30.7246 5 1 -2 0 1389.13 30.3091 4 1 -2 0 1431.04 30.8994 3 -1 2 0 1426.49 30.3793 1 -1 2 0 1426.76 30.3948 2 0 -2 0 1869.74 39.9130 5 0 -2 0 1831.51 39.0608 1 0 -2 0 1890.35 39.5976 3 0 2 0 1882.51 39.4505 1 0 2 0 1887.49 39.1468 2 -1 -2 0 14.4759 2.52482 5 1 2 0 11.6585 2.37345 2 1 2 0 17.1938 1.92412 3 1 2 0 13.3750 1.97046 1 -2 -2 0 2980.70 60.6702 1 -2 -2 0 2849.69 61.0450 5 2 2 0 2889.30 59.9239 2 2 2 0 2870.29 60.2630 3 -3 -2 0 2396.30 51.1029 1 -3 -2 0 2342.88 50.8054 5 3 2 0 2394.26 50.3805 3 3 2 0 2384.80 50.3125 2 -4 -2 0 26.5383 3.88946 1 -4 -2 0 24.5292 3.17077 5 4 2 0 26.6002 3.48933 2 4 2 0 30.7821 3.42338 3 -5 -2 0 681.289 19.0517 1 -5 -2 0 657.447 17.0024 5 5 2 0 676.306 17.9129 2 5 2 0 671.152 17.7854 3 -6 -2 0 59.8853 6.40653 1 -6 -2 0 50.0038 4.85813 5 6 2 0 50.6828 5.31790 2 6 2 0 64.6569 5.83770 3 -7 -2 0 488.145 17.5769 1 7 2 0 504.724 16.4744 3 7 2 0 495.431 16.2402 2 -8 -2 0 345.345 15.6964 1 8 2 0 344.548 14.1212 3 8 2 0 333.413 13.5060 2 -9 -2 0 44.4177 8.23036 1 9 2 0 47.7624 6.89273 2 9 2 0 40.4725 6.87525 3 -10 -2 0 200.022 14.1607 1 10 2 0 171.139 11.3856 2 10 2 0 182.709 12.4033 3 -11 -2 0 10.0011 8.53267 1 11 2 0 -3.4752 6.01794 2 10 -3 0 32.1356 8.96525 3 -10 3 0 38.6109 8.04959 2 -10 3 0 42.9398 9.58326 1 9 -3 0 342.224 16.4773 3 -9 3 0 318.005 15.0996 2 -9 3 0 347.699 16.8700 1 8 -3 0 28.1756 6.83222 3 -8 3 0 31.8651 6.26382 2 -8 3 0 23.8281 6.83070 1 7 -3 0 1003.53 28.8237 3 -7 3 0 1016.93 28.6328 1 -7 3 0 1046.41 27.7989 2 6 -3 0 709.750 21.2104 3 -6 3 0 685.687 19.8564 2 -6 3 0 657.530 20.3261 1 5 -3 0 530.169 16.5273 3 -5 3 0 507.112 15.6101 2 -5 3 0 516.494 16.0228 1 4 -3 0 480.938 14.6569 3 4 -3 0 460.200 11.5254 5 -4 3 0 483.856 13.8891 2 -4 3 0 463.923 14.0470 1 3 -3 0 29.1695 2.72133 5 3 -3 0 28.1012 3.90185 3 3 -3 0 27.3804 3.91617 4 -3 3 0 34.9556 3.64528 2 -3 3 0 27.5918 3.59601 1 2 -3 0 1693.90 38.1588 3 2 -3 0 1632.94 37.3132 4 2 -3 0 1826.21 37.5770 5 -2 3 0 1728.28 37.4193 1 -2 3 0 1745.23 37.5104 2 1 -3 0 1555.92 34.2235 3 1 -3 0 1571.82 34.2363 5 -1 3 0 1535.99 33.3957 1 -1 3 0 1578.70 33.9569 2 0 -3 0 18.0740 2.79831 5 0 -3 0 19.0961 2.63111 3 0 3 0 22.7456 2.29007 1 0 3 0 16.3762 2.61350 2 -1 -3 0 2975.63 62.7538 5 -1 -3 0 2943.02 61.5151 3 1 3 0 2907.47 61.2971 1 1 3 0 2985.14 61.4857 2 -2 -3 0 271.326 8.31469 1 -2 -3 0 251.947 9.07712 5 2 3 0 283.145 9.09427 2 2 3 0 267.235 7.53900 3 -3 -3 0 2151.57 48.0931 5 -3 -3 0 2189.21 47.6334 1 3 3 0 2267.52 47.6255 2 3 3 0 2186.44 46.7277 3 -4 -3 0 533.351 15.2199 5 -4 -3 0 550.331 15.5853 1 4 3 0 556.613 14.4787 3 4 3 0 564.930 15.5278 2 -5 -3 0 456.023 14.8131 1 -5 -3 0 428.013 13.4052 5 5 3 0 451.294 14.1547 2 5 3 0 474.368 13.4963 3 -6 -3 0 471.515 14.3754 5 -6 -3 0 484.605 16.4275 1 6 3 0 456.614 15.0476 2 6 3 0 475.550 14.5861 3 -7 -3 0 64.6551 6.21231 5 -7 -3 0 90.2159 8.34705 1 7 3 0 93.5329 7.59329 3 7 3 0 73.8902 7.05073 2 -8 -3 0 552.654 20.2634 1 8 3 0 535.561 18.3584 2 8 3 0 534.135 18.1003 3 -9 -3 0 316.199 16.4373 1 9 3 0 337.572 14.5931 2 -10 -3 0 11.4293 7.41710 1 10 3 0 6.12173 5.88449 2 -11 -3 0 187.308 15.2405 1 11 3 0 173.066 12.4770 2 10 -4 0 131.195 12.5112 3 -10 4 0 114.457 12.4531 1 9 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1629.20 35.9671 1 0 -5 -3 961.434 24.2722 3 0 -5 -3 995.267 24.9399 5 0 5 3 982.369 24.4690 2 -1 -5 -3 1047.40 26.0101 5 -1 -5 -3 963.392 22.0765 1 -1 -5 -3 1046.83 24.8689 3 1 5 3 1025.91 25.0853 2 -2 -5 -3 2008.72 45.8223 5 -2 -5 -3 1930.72 42.2388 1 2 5 3 2028.20 44.6677 2 2 5 3 1999.38 44.0880 3 -3 -5 -3 24.0943 4.43862 5 -3 -5 -3 30.8234 3.42806 1 3 5 3 28.3407 3.74942 3 3 5 3 28.6337 4.34507 2 -4 -5 -3 554.341 17.3004 5 -4 -5 -3 541.773 15.5317 1 4 5 3 572.637 16.8828 2 4 5 3 536.974 15.4223 3 -5 -5 -3 592.282 17.6041 1 -5 -5 -3 618.170 19.0227 5 5 5 3 611.600 18.3765 2 5 5 3 612.786 17.3484 3 -6 -5 -3 59.7895 6.84851 5 6 5 3 69.9558 6.68420 2 6 5 3 62.7252 6.17686 3 -7 -5 -3 411.181 16.1330 1 -7 -5 -3 422.885 15.5612 5 7 5 3 434.975 15.8834 2 7 5 3 440.313 15.1278 3 -8 -5 -3 -6.8728 5.14113 1 -8 -5 -3 5.38935 4.57642 5 8 5 3 2.21640 4.47576 2 -9 -5 -3 278.553 15.4034 1 9 5 3 261.310 13.3654 2 -10 -5 -3 193.935 14.1705 1 10 5 3 190.267 12.3207 2 9 -6 -3 26.8863 8.80401 3 -9 6 3 34.5417 8.37463 2 -9 6 3 30.0965 8.42425 1 8 -6 -3 52.6783 9.10445 3 -8 6 3 39.8885 7.83585 1 -8 6 3 40.1772 8.08213 2 7 -6 -3 733.882 24.9293 3 -7 6 3 725.867 24.0608 2 -7 6 3 691.704 22.6795 1 6 -6 -3 55.8135 7.90436 3 -6 6 3 55.7031 7.47074 2 -6 6 3 36.8913 6.22960 1 5 -6 -3 143.073 10.0324 3 -5 6 3 146.624 9.95541 2 -5 6 3 136.651 8.57034 1 4 -6 -3 125.503 9.10734 3 4 -6 -3 114.895 6.74896 5 4 -6 -3 105.649 8.62326 4 -4 6 3 107.224 7.07527 1 -4 6 3 116.078 8.49225 2 3 -6 -3 247.551 11.5440 3 3 -6 -3 252.852 11.5052 4 3 -6 -3 246.392 10.0449 5 -3 6 3 242.694 9.16228 1 -3 6 3 259.196 11.4668 2 2 -6 -3 289.594 11.9069 3 2 -6 -3 286.985 11.9483 4 2 -6 -3 275.517 10.8969 5 -2 6 3 313.037 12.0264 2 -2 6 3 272.373 8.94307 1 1 -6 -3 431.092 14.1071 3 1 -6 -3 418.174 14.3136 4 1 -6 -3 407.679 13.9461 5 -1 6 3 389.489 10.6155 1 -1 6 3 402.894 14.0355 2 0 -6 -3 675.358 18.9637 3 0 -6 -3 673.364 19.7078 5 0 6 3 676.912 19.2216 2 -1 -6 -3 95.3405 7.03293 3 -1 -6 -3 101.476 7.45217 5 1 6 3 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53.0614 7.42730 2 4 -7 -3 200.566 11.3923 4 4 -7 -3 235.113 12.1018 3 -4 7 3 187.328 9.02925 1 -4 7 3 205.258 11.3865 2 3 -7 -3 584.872 19.0991 3 3 -7 -3 572.005 19.1139 4 3 -7 -3 594.288 17.9508 5 -3 7 3 543.570 15.6934 1 -3 7 3 593.451 19.2384 2 2 -7 -3 154.938 9.64740 3 2 -7 -3 148.895 9.00427 5 2 -7 -3 150.844 9.78557 4 -2 7 3 150.217 9.43745 2 1 -7 -3 747.165 21.8015 3 1 -7 -3 765.737 22.0935 5 1 -7 -3 775.254 22.3779 4 -1 7 3 746.134 22.0686 2 0 -7 -3 141.545 8.56242 3 0 -7 -3 131.393 8.69721 5 0 7 3 134.879 8.70334 2 -1 -7 -3 697.820 19.9219 3 -1 -7 -3 697.602 21.1554 5 1 7 3 708.187 20.7898 2 -2 -7 -3 638.942 20.3143 5 2 7 3 656.197 18.2735 3 2 7 3 645.654 19.5995 2 -3 -7 -3 -3.8368 4.53359 5 3 7 3 9.15213 4.13790 2 3 7 3 3.03627 3.46960 3 -4 -7 -3 1337.81 32.7179 1 -4 -7 -3 1480.21 37.3557 5 4 7 3 1382.27 33.2485 3 4 7 3 1426.59 35.8073 2 -5 -7 -3 22.5934 4.50526 1 -5 -7 -3 37.3043 6.58552 5 5 7 3 32.1660 5.79404 2 -6 -7 -3 215.792 12.2208 5 -6 -7 -3 189.276 10.3532 1 6 7 3 194.633 11.0798 2 -7 -7 -3 414.930 16.7304 1 -7 -7 -3 450.431 18.2512 5 7 7 3 475.185 17.8494 2 -8 -7 -3 10.5273 6.09943 5 8 7 3 13.4670 5.78734 2 9 7 3 137.268 10.7406 2 10 7 3 31.3009 7.67252 2 -8 8 3 72.0502 10.5783 2 7 -8 -3 179.906 13.8361 3 -7 8 3 178.879 12.8891 2 6 -8 -3 91.3709 10.2553 3 -6 8 3 95.8998 10.2541 2 5 -8 -3 441.586 18.1543 3 -5 8 3 416.378 17.4490 2 4 -8 -3 186.957 11.6188 3 4 -8 -3 178.980 11.6193 4 -4 8 3 189.911 11.5948 2 3 -8 -3 116.322 9.97411 4 3 -8 -3 106.677 8.41130 5 3 -8 -3 129.680 9.89839 3 -3 8 3 136.483 9.75074 2 2 -8 -3 178.579 10.9347 3 2 -8 -3 186.871 10.4500 5 2 -8 -3 205.538 11.7080 4 -2 8 3 192.288 10.9697 2 1 -8 -3 38.2985 7.00331 4 1 -8 -3 41.0993 6.38644 5 1 -8 -3 30.0091 6.03816 3 -1 8 3 43.6969 6.40383 2 0 -8 -3 673.163 21.4349 5 0 -8 -3 678.336 20.5503 3 0 -8 -3 685.522 21.6930 4 0 8 3 665.470 21.0852 2 -1 -8 -3 130.833 8.80317 3 -1 -8 -3 120.496 9.16519 5 1 8 3 104.685 8.30054 2 -2 -8 -3 330.420 14.4830 5 2 8 3 335.343 12.5783 3 2 8 3 359.219 14.2109 2 -3 -8 -3 621.983 20.5569 5 3 8 3 578.465 19.2873 2 3 8 3 553.090 17.0168 3 -4 -8 -3 15.9255 5.82450 5 4 8 3 25.7163 5.67193 2 -5 -8 -3 533.538 20.1305 5 5 8 3 535.717 19.0660 2 -6 -8 -3 188.516 12.2079 5 6 8 3 176.649 11.0261 2 -7 -8 -3 92.7705 10.2560 5 7 8 3 98.2759 9.21126 2 -8 -8 -3 198.191 13.2573 5 8 8 3 200.823 12.7719 2 9 8 3 6.75846 6.33117 2 7 -9 -3 4.99711 7.60205 3 -7 9 3 -1.8210 6.62143 2 6 -9 -3 221.863 14.5976 3 -6 9 3 219.797 14.0124 2 5 -9 -3 35.0105 8.12618 3 -5 9 3 34.0103 7.72450 2 4 -9 -3 324.588 16.3576 4 4 -9 -3 335.627 16.0446 3 -4 9 3 354.185 16.2327 2 3 -9 -3 175.684 12.5718 4 3 -9 -3 192.711 12.0324 3 3 -9 -3 181.122 10.9311 5 -3 9 3 204.223 12.0637 2 2 -9 -3 145.560 9.97804 5 2 -9 -3 149.256 10.5837 3 2 -9 -3 166.117 11.5828 4 -2 9 3 152.476 10.5839 2 1 -9 -3 189.272 11.1542 5 1 -9 -3 193.679 12.2009 4 1 -9 -3 196.685 11.1174 3 -1 9 3 177.113 11.2265 2 0 -9 -3 36.8284 6.82010 5 0 -9 -3 37.9165 6.56694 3 0 -9 -3 46.9748 7.60008 4 -1 -9 -3 778.735 24.7517 5 -1 -9 -3 775.788 22.6420 3 1 9 3 746.603 23.8491 2 -2 -9 -3 333.523 15.0019 5 2 9 3 307.783 14.2632 2 -3 -9 -3 150.408 10.8903 5 3 9 3 153.797 10.1475 2 -4 -9 -3 512.989 20.1720 5 4 9 3 528.196 19.3698 2 -5 -9 -3 -4.4335 5.26656 5 5 9 3 4.98301 4.92284 2 -6 -9 -3 145.679 11.8110 5 6 9 3 119.104 10.0077 2 -7 -9 -3 114.828 11.5444 5 7 9 3 110.500 10.1298 2 -8 -9 -3 34.9289 8.72045 5 8 9 3 19.8713 6.96294 2 6 -10 -3 34.1714 9.19781 3 -6 10 3 17.7357 7.50969 2 5 -10 -3 188.830 13.8313 3 -5 10 3 196.944 13.5975 2 4 -10 -3 9.09581 6.87430 3 -4 10 3 19.2522 7.20101 2 3 -10 -3 355.120 16.5013 3 3 -10 -3 362.844 17.6640 4 -3 10 3 359.438 16.7903 2 2 -10 -3 302.021 14.6901 5 2 -10 -3 282.648 14.4198 3 2 -10 -3 296.505 15.6182 4 -2 10 3 306.497 15.2780 2 1 -10 -3 32.4287 6.95489 3 1 -10 -3 35.0797 8.25229 4 1 -10 -3 41.4804 7.44849 5 -1 10 3 34.6104 7.15287 2 0 -10 -3 286.347 14.9722 4 0 -10 -3 267.909 14.3254 5 0 -10 -3 281.134 13.6368 3 0 10 3 289.647 14.2252 2 -1 -10 -3 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11.1607 1 3 -3 26 56.2545 9.75564 5 -4 3 -26 209.256 15.7031 1 2 2 -26 53.7886 9.69674 1 -2 -2 26 33.8298 9.13799 5 1 2 -26 68.3580 9.91870 1 -1 -2 26 24.7469 8.70784 5 0 2 -26 154.016 13.0196 1 0 -2 26 181.917 13.5742 5 -1 2 -26 4.25358 7.03514 1 1 -2 26 -4.9420 6.70622 5 -2 2 -26 81.4037 10.8813 1 2 -2 26 97.0437 11.2447 5 -3 2 -26 228.182 15.1709 1 3 -2 26 214.254 15.1341 5 4 -2 26 69.1465 10.5272 5 -5 2 -26 83.2355 11.7875 1 -3 -1 26 23.0384 9.01897 1 2 1 -26 69.7462 10.2234 1 -2 -1 26 71.4944 10.2431 5 1 1 -26 93.0791 10.7305 1 -1 -1 26 76.2980 10.2383 5 0 1 -26 8.44888 7.12773 1 0 -1 26 16.9415 7.93775 5 -1 1 -26 323.927 16.6823 1 1 -1 26 340.893 17.6488 5 -2 1 -26 39.8241 8.49442 1 2 -1 26 47.8906 8.98414 5 -3 1 -26 179.754 13.6181 1 3 -1 26 188.466 13.9257 5 3 -1 26 166.772 13.4814 3 -4 1 -26 123.591 12.2804 1 4 -1 26 147.649 12.7650 3 4 -1 26 135.349 12.5418 5 -5 1 -26 10.8631 7.95466 1 5 -1 26 1.75376 8.02478 3 5 -1 26 -0.1395 7.31742 5 -6 1 -26 62.4747 11.3739 1 6 -1 26 68.9118 10.7438 3 -2 0 26 10.3295 7.57567 5 -1 0 26 55.3097 9.60530 5 0 0 -26 287.520 15.0508 1 0 0 26 301.009 16.4332 5 -1 0 -26 13.9875 6.67079 1 1 0 26 6.46305 7.22612 5 -2 0 -26 204.251 13.1589 1 2 0 26 221.826 14.6697 3 2 0 26 213.215 14.5298 5 -3 0 -26 38.6610 8.56249 1 3 0 26 44.7725 9.42061 3 -4 0 -26 112.217 11.5107 1 -4 0 -26 108.966 12.0607 5 4 0 26 127.303 12.4563 3 -5 0 -26 103.625 11.9289 5 5 0 26 111.817 12.5344 3 6 0 26 0.26462 8.38088 3 -1 1 26 55.0860 9.38842 5 0 1 26 63.7036 9.76511 5 0 1 26 60.9526 9.47246 3 -1 -1 -26 319.455 17.2053 5 1 1 26 299.254 16.2594 3 -2 -1 -26 7.11664 7.02440 5 2 1 26 5.61227 7.29399 3 -3 -1 -26 111.183 11.7272 5 3 1 26 115.570 11.8653 3 -4 -1 -26 128.332 12.5205 5 4 1 26 136.331 13.3130 3 -5 -1 -26 79.9680 10.9703 5 5 1 26 76.1717 11.4394 3 -1 2 26 171.380 13.4856 3 0 -2 -26 62.1138 9.90443 5 0 2 26 60.5546 9.70848 3 -1 -2 -26 44.8596 9.04079 5 1 2 26 13.4279 7.89764 3 -2 -2 -26 263.027 16.0054 5 2 2 26 289.290 16.4293 3 -3 -2 -26 15.8684 7.64832 5 3 2 26 15.9479 8.29797 3 -4 -2 -26 121.602 12.2824 5 4 2 26 129.010 12.7733 3 -5 -2 -26 141.271 13.0822 5 5 2 26 139.861 13.4908 3 -2 3 26 130.237 13.1148 3 1 -3 -26 -1.3985 6.88905 5 -1 3 26 5.26495 8.07888 3 0 -3 -26 129.715 12.2697 5 0 3 26 110.539 11.8985 3 -1 -3 -26 124.951 12.2743 5 1 3 26 102.548 11.8826 3 -2 -3 -26 57.4785 9.83172 5 2 3 26 53.1527 9.72729 3 -3 -3 -26 264.373 16.1787 5 3 3 26 274.272 16.6462 3 -4 -3 -26 63.1520 10.0878 5 4 3 26 34.4051 9.41507 3 5 3 26 135.048 13.5299 3 -1 4 26 349.579 19.3984 3 0 -4 -26 23.5862 8.39235 5 0 4 26 21.8136 8.96047 3 -1 -4 -26 124.821 12.4556 5 1 4 26 123.163 12.9859 3 -2 -4 -26 318.848 18.0565 5 2 4 26 343.255 18.5193 3 -3 -4 -26 16.4482 8.12023 5 3 4 26 6.12393 8.33341 3 4 4 26 271.054 17.0802 3 0 -5 -26 184.539 14.5767 5 -1 -5 -26 37.5088 9.45922 5 -2 -5 -26 19.7618 8.66726 5 -1 3 -27 3.79782 7.83480 1 -2 3 -27 138.038 13.7408 1 1 2 -27 121.743 12.5491 1 -1 -2 27 123.310 12.3569 5 0 2 -27 -0.3894 7.16654 1 0 -2 27 -6.0854 7.10154 5 -1 2 -27 96.0832 11.2659 1 1 -2 27 92.0557 11.6091 5 -2 2 -27 48.6912 9.73647 1 2 -2 27 46.7351 9.71846 5 -3 2 -27 133.926 13.0409 1 -4 2 -27 241.385 16.3553 1 -2 -1 27 15.8089 8.82503 5 1 1 -27 81.8450 10.7901 1 -1 -1 27 83.1498 10.5263 5 0 1 -27 242.119 14.7380 1 0 -1 27 249.204 15.6725 5 -1 1 -27 8.27806 7.24489 1 1 -1 27 -2.8861 7.16875 5 -2 1 -27 227.971 14.6577 1 2 -1 27 204.374 14.7861 5 -3 1 -27 123.576 12.2089 1 3 -1 27 132.581 12.3283 5 -4 1 -27 119.845 12.5327 1 -5 1 -27 223.173 15.6257 1 5 -1 27 183.373 14.7901 3 -1 0 27 30.8457 8.75561 5 0 0 27 52.5286 9.77299 5 1 0 27 471.850 21.0519 5 2 0 27 21.8632 8.32320 5 3 0 27 45.3640 9.56029 3 3 0 27 51.6509 9.73607 5 4 0 27 92.2568 11.9249 3 5 0 27 5.97314 8.13951 3 -1 1 27 120.423 12.1909 5 0 1 27 126.601 12.5111 5 1 1 27 32.1299 8.97777 3 -2 -1 -27 232.275 15.7481 5 2 1 27 213.899 14.6740 3 -3 -1 -27 13.5691 7.97994 5 3 1 27 37.3533 9.48448 3 -4 -1 -27 65.2049 10.4300 5 4 1 27 53.8637 10.5532 3 5 1 27 57.8633 11.0224 3 -1 2 27 43.7535 9.48817 5 0 -2 -27 94.7321 11.5063 5 0 2 27 69.2171 10.5332 3 -1 -2 -27 107.812 12.2015 5 1 2 27 103.839 11.7499 3 -2 -2 -27 20.3506 8.61146 5 2 2 27 10.7844 8.09938 3 -3 -2 -27 221.997 15.6463 5 3 2 27 203.232 14.9910 3 4 2 27 103.206 12.2014 3 -1 3 27 147.410 13.8283 3 0 -3 -27 25.0876 9.27144 5 0 3 27 48.2582 10.1807 3 -1 -3 -27 23.0397 8.83705 5 1 3 27 21.5302 8.90884 3 -2 -3 -27 167.426 14.1173 5 2 3 27 158.675 14.0945 3 -3 -3 -27 1.64313 7.40873 5 3 3 27 2.53979 7.92235 3 0 -4 -27 183.879 14.6466 5 -1 -4 -27 88.9360 11.6096 5 0 1 -28 31.8406 8.80789 1 -1 1 -28 193.809 14.1209 1 -2 1 -28 16.2659 8.06586 1 -3 1 -28 96.3089 11.9250 1 0 0 28 151.911 13.7877 5 1 0 28 37.5700 9.40866 5 4 0 28 95.8024 12.3400 3 -1 1 28 74.3242 10.9128 5 0 1 28 56.3870 9.97191 5 1 1 28 163.802 13.5233 5 2 1 28 23.7219 8.79430 3 3 1 28 146.491 14.1218 3 1 2 28 18.2826 8.99584 3 2 2 28 144.678 13.5498 3 3 2 28 4.61955 7.92964 3 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 6994 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 W W 0.30269(2) 0.22370(2) 0.24709(2) 0.01338(2) Uani 1 1 d . Cl1 Cl 0.01092(7) 0.35535(6) 0.29315(3) 0.02386(9) Uani 1 1 d . Cl2 Cl 0.52186(6) 0.00581(6) 0.20214(3) 0.01898(8) Uani 1 1 d . F1 F 0.64020(18) 0.16682(14) 0.42558(8) 0.0256(3) Uani 1 1 d . F2 F 0.82864(18) 0.37723(17) 0.49876(8) 0.0277(3) Uani 1 1 d . F3 F 0.79740(18) 0.72054(16) 0.47392(8) 0.0273(3) Uani 1 1 d . F4 F 0.5748(2) 0.85315(15) 0.37585(8) 0.0309(3) Uani 1 1 d . F5 F 0.38854(19) 0.64343(15) 0.29977(8) 0.0272(3) Uani 1 1 d . F6 F 0.15260(16) 0.52664(16) 0.06640(7) 0.0240(2) Uani 1 1 d . F7 F 0.28900(18) 0.77630(16) -0.02949(7) 0.0268(3) Uani 1 1 d . F8 F 0.63550(18) 0.88274(15) -0.02473(7) 0.0250(3) Uani 1 1 d . F9 F 0.83318(17) 0.75153(16) 0.08196(8) 0.0249(2) Uani 1 1 d . F10 F 0.69655(17) 0.50452(16) 0.18063(7) 0.0244(2) Uani 1 1 d . O1 O 0.17777(19) 0.00195(17) 0.32305(8) 0.0179(2) Uani 1 1 d . O2 O 0.12761(19) 0.06905(17) 0.18023(8) 0.0190(3) Uani 1 1 d . N1 N 0.4158(2) 0.29248(19) 0.32031(9) 0.0169(3) Uani 1 1 d . N2 N 0.3544(2) 0.3733(2) 0.17242(9) 0.0175(3) Uani 1 1 d . C1 C 0.1477(3) 0.0154(3) 0.40438(11) 0.0247(4) Uani 1 1 d . H1A H 0.258347 0.056797 0.421348 0.028(4) Uiso 1 1 d GR H1B H 0.121334 -0.097164 0.427910 0.028(4) Uiso 1 1 d GR H1C H 0.042962 0.095676 0.419042 0.028(4) Uiso 1 1 d GR C2 C 0.0312(3) -0.0841(3) 0.29621(12) 0.0232(4) Uani 1 1 d . H2A H -0.087176 -0.017296 0.307415 0.028 Uiso 1 1 d R H2B H 0.017524 -0.198816 0.320775 0.028 Uiso 1 1 d R C3 C 0.0853(3) -0.0985(3) 0.21228(12) 0.0232(4) Uani 1 1 d . H3A H 0.194429 -0.178056 0.201676 0.028 Uiso 1 1 d R H3B H -0.017001 -0.143596 0.189426 0.028 Uiso 1 1 d R C4 C -0.0095(3) 0.1458(3) 0.13754(13) 0.0255(4) Uani 1 1 d . H4A H -0.127830 0.158128 0.170530 0.039(5) Uiso 1 1 d GR H4B H -0.022702 0.072747 0.095397 0.039(5) Uiso 1 1 d GR H4C H 0.028753 0.258491 0.117686 0.039(5) Uiso 1 1 d GR C5 C 0.5099(2) 0.3978(2) 0.35932(10) 0.0150(3) Uani 1 1 d . C6 C 0.6224(3) 0.3349(2) 0.41209(10) 0.0157(3) Uani 1 1 d . C7 C 0.7196(3) 0.4417(2) 0.45010(11) 0.0171(3) Uani 1 1 d . C8 C 0.7039(3) 0.6162(2) 0.43737(11) 0.0182(3) Uani 1 1 d . C9 C 0.5913(3) 0.6835(2) 0.38699(11) 0.0197(3) Uani 1 1 d . C10 C 0.4966(3) 0.5757(2) 0.34832(11) 0.0175(3) Uani 1 1 d . C11 C 0.4201(3) 0.5071(2) 0.12664(10) 0.0158(3) Uani 1 1 d . C12 C 0.3196(3) 0.5827(2) 0.07223(11) 0.0174(3) Uani 1 1 d . C13 C 0.3882(3) 0.7104(2) 0.02257(11) 0.0181(3) Uani 1 1 d . C14 C 0.5629(3) 0.7658(2) 0.02524(11) 0.0180(3) Uani 1 1 d . C15 C 0.6657(3) 0.6953(2) 0.07892(11) 0.0174(3) Uani 1 1 d . C16 C 0.5949(3) 0.5696(2) 0.12932(10) 0.0169(3) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.01376(3) 0.01289(3) 0.01397(3) -0.00136(2) -0.00315(2) -0.00131(2) Cl1 0.0192(2) 0.0251(2) 0.0258(2) -0.00260(18) 0.00018(17) 0.00507(17) Cl2 0.01697(19) 0.01729(18) 0.0220(2) -0.00331(15) -0.00063(15) 0.00148(14) F1 0.0331(7) 0.0129(5) 0.0332(7) 0.0007(5) -0.0142(6) 0.0001(4) F2 0.0279(6) 0.0278(6) 0.0313(7) 0.0001(5) -0.0180(5) 0.0002(5) F3 0.0278(6) 0.0254(6) 0.0323(7) -0.0096(5) -0.0117(5) -0.0080(5) F4 0.0411(8) 0.0128(5) 0.0424(8) -0.0016(5) -0.0168(6) -0.0042(5) F5 0.0377(7) 0.0170(5) 0.0311(7) 0.0020(5) -0.0204(6) 0.0008(5) F6 0.0157(5) 0.0271(6) 0.0303(6) 0.0030(5) -0.0077(5) -0.0022(4) F7 0.0287(6) 0.0277(6) 0.0255(6) 0.0078(5) -0.0124(5) 0.0028(5) F8 0.0293(6) 0.0203(5) 0.0234(6) 0.0055(5) 0.0019(5) -0.0021(5) F9 0.0179(5) 0.0257(6) 0.0323(7) -0.0004(5) -0.0054(5) -0.0068(5) F10 0.0231(6) 0.0272(6) 0.0251(6) 0.0045(5) -0.0126(5) -0.0011(5) O1 0.0185(6) 0.0196(6) 0.0160(6) -0.0007(5) -0.0021(5) -0.0050(5) O2 0.0191(6) 0.0208(6) 0.0193(6) 0.0009(5) -0.0087(5) -0.0052(5) N1 0.0174(7) 0.0154(6) 0.0187(7) -0.0023(5) -0.0045(6) -0.0009(5) N2 0.0176(7) 0.0153(6) 0.0194(7) -0.0006(5) -0.0028(6) 0.0011(5) C1 0.0308(11) 0.0266(9) 0.0162(8) 0.0022(7) -0.0016(8) -0.0043(8) C2 0.0212(9) 0.0232(9) 0.0259(10) 0.0020(7) -0.0039(7) -0.0086(7) C3 0.0281(10) 0.0193(8) 0.0248(9) -0.0014(7) -0.0092(8) -0.0089(7) C4 0.0201(9) 0.0308(10) 0.0282(10) 0.0031(8) -0.0122(8) -0.0042(8) C5 0.0157(7) 0.0149(7) 0.0148(7) -0.0025(6) -0.0031(6) -0.0013(6) C6 0.0179(8) 0.0131(7) 0.0166(8) -0.0011(6) -0.0038(6) -0.0006(6) C7 0.0142(7) 0.0202(8) 0.0177(8) -0.0012(6) -0.0054(6) 0.0003(6) C8 0.0176(8) 0.0181(8) 0.0199(8) -0.0055(6) -0.0034(7) -0.0039(6) C9 0.0237(9) 0.0135(7) 0.0227(9) -0.0030(6) -0.0045(7) -0.0022(6) C10 0.0200(8) 0.0152(7) 0.0182(8) -0.0004(6) -0.0058(7) -0.0008(6) C11 0.0179(8) 0.0144(7) 0.0147(7) -0.0012(6) -0.0017(6) 0.0010(6) C12 0.0153(8) 0.0182(8) 0.0190(8) -0.0026(6) -0.0041(6) 0.0022(6) C13 0.0211(8) 0.0166(7) 0.0167(8) 0.0008(6) -0.0046(7) 0.0027(6) C14 0.0225(9) 0.0150(7) 0.0159(8) -0.0002(6) -0.0003(7) 0.0000(6) C15 0.0159(8) 0.0161(7) 0.0203(8) -0.0023(6) -0.0032(6) -0.0002(6) C16 0.0181(8) 0.0167(7) 0.0168(8) -0.0015(6) -0.0058(6) 0.0020(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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 -1.00 0.0550 0.00 0.00 1.00 0.0550 0.00 1.00 0.00 0.0500 0.00 -1.00 0.00 0.0500 -2.00 -1.00 0.00 0.0500 2.00 1.00 0.00 0.0500 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Cl2 W Cl1 158.634(18) O1 W Cl1 80.53(4) O1 W Cl2 82.39(4) O2 W Cl1 82.45(4) O2 W Cl2 79.83(4) O2 W O1 70.60(5) N1 W Cl1 95.45(5) N1 W Cl2 97.66(5) N1 W O1 91.24(6) N1 W O2 161.83(6) N2 W Cl1 95.10(5) N2 W Cl2 97.73(5) N2 W O1 163.65(6) N2 W O2 93.26(6) N2 W N1 104.91(7) C1 O1 W 120.36(11) C2 O1 W 116.44(11) C2 O1 C1 111.72(15) C3 O2 W 114.87(11) C4 O2 W 123.34(12) C4 O2 C3 114.28(15) C5 N1 W 158.62(14) C11 N2 W 165.55(14) O1 C1 H1A 109.5 O1 C1 H1B 109.5 O1 C1 H1C 109.5 H1A C1 H1B 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 O1 C2 H2A 110.5 O1 C2 H2B 110.5 O1 C2 C3 106.06(16) H2A C2 H2B 108.7 C3 C2 H2A 110.5 C3 C2 H2B 110.5 O2 C3 C2 108.59(16) O2 C3 H3A 110.0 O2 C3 H3B 110.0 C2 C3 H3A 110.0 C2 C3 H3B 110.0 H3A C3 H3B 108.3 O2 C4 H4A 109.5 O2 C4 H4B 109.5 O2 C4 H4C 109.5 H4A C4 H4B 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 N1 C5 C6 122.34(16) N1 C5 C10 121.07(16) C6 C5 C10 116.59(16) F1 C6 C5 119.61(16) F1 C6 C7 118.38(16) C7 C6 C5 122.00(16) F2 C7 C6 120.44(17) F2 C7 C8 119.87(17) C8 C7 C6 119.70(17) F3 C8 C7 120.12(17) F3 C8 C9 119.81(17) C9 C8 C7 120.07(17) F4 C9 C8 119.63(17) F4 C9 C10 120.47(18) C8 C9 C10 119.89(17) F5 C10 C5 119.34(16) F5 C10 C9 118.92(16) C9 C10 C5 121.73(17) N2 C11 C12 121.46(17) N2 C11 C16 121.87(16) C12 C11 C16 116.60(17) F6 C12 C11 119.26(17) F6 C12 C13 118.41(16) C13 C12 C11 122.31(17) F7 C13 C12 120.24(17) F7 C13 C14 120.06(17) C12 C13 C14 119.66(17) F8 C14 C13 120.62(17) F8 C14 C15 119.69(18) C13 C14 C15 119.66(17) F9 C15 C14 119.29(17) F9 C15 C16 120.37(17) C16 C15 C14 120.34(17) F10 C16 C11 119.54(16) F10 C16 C15 119.06(17) C15 C16 C11 121.38(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance W Cl1 2.3791(5) W Cl2 2.3663(5) W O1 2.3115(13) W O2 2.2901(13) W N1 1.7593(16) W N2 1.7570(16) F1 C6 1.334(2) F2 C7 1.332(2) F3 C8 1.338(2) F4 C9 1.340(2) F5 C10 1.335(2) F6 C12 1.342(2) F7 C13 1.335(2) F8 C14 1.333(2) F9 C15 1.336(2) F10 C16 1.334(2) O1 C1 1.445(2) O1 C2 1.444(2) O2 C3 1.444(2) O2 C4 1.442(2) N1 C5 1.371(2) N2 C11 1.371(2) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 H2A 0.9900 C2 H2B 0.9900 C2 C3 1.502(3) C3 H3A 0.9900 C3 H3B 0.9901 C4 H4A 0.9799 C4 H4B 0.9801 C4 H4C 0.9799 C5 C6 1.400(3) C5 C10 1.401(2) C6 C7 1.382(2) C7 C8 1.380(3) C8 C9 1.380(3) C9 C10 1.383(3) C11 C12 1.399(3) C11 C16 1.403(3) C12 C13 1.380(3) C13 C14 1.382(3) C14 C15 1.385(3) C15 C16 1.381(3)