#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:54:14 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225918 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515803.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_4515803 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_absolute_configuration ad _chemical_formula_moiety 'C16 H14 Cl2 F6 N2 O2 W' _chemical_formula_sum 'C16 H14 Cl2 F6 N2 O2 W' _chemical_formula_weight 635.04 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_date 2017-10-27 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.0005(5) _cell_length_b 12.4893(5) _cell_length_c 13.5857(6) _cell_measurement_reflns_used 3873 _cell_measurement_temperature 120 _cell_measurement_theta_max 27.506 _cell_measurement_theta_min 2.215 _cell_volume 2036.20(15) _computing_cell_refinement 'SAINT v7.46A (Bruker, 2008)' _computing_data_collection 'SMART v5.625 (Bruker, 2001)' _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 'CCD area detector' _diffrn_detector_area_resol_mean 5.6 _diffrn_detector_type 'Bruker SMART CCD 6000 area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_unetI/netI 0.0946 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 25431 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.535 _diffrn_reflns_theta_min 2.215 _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 6.004 _exptl_absorpt_correction_T_max 0.4305 _exptl_absorpt_correction_T_min 0.2816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; TWINABS-2012/1 (Bruker,2012) was used for absorption correction. 5591 single and 11294 composite reflections used for parameter fitting. For component 1: wR2(int) was 0.0949 before and 0.0749 after correction. The Ratio of minimum to maximum transmission not present. The \l/2 correction factor is Not present ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1208 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _refine_diff_density_max 1.931 _refine_diff_density_min -1.399 _refine_diff_density_rms 0.194 _refine_ls_abs_structure_details ; Flack x determined using 1853 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack, 2004). By classical hole-in-one fit to all intensities, x= -0.003(14). Hooft parameter y = 0.013(6). ; _refine_ls_abs_structure_Flack 0.022(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 265 _refine_ls_number_reflns 25431 _refine_ls_number_restraints 51 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0486 _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^)+(0.0470P)^2^+4.0460P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1290 _refine_ls_wR_factor_ref 0.1377 _reflns_Friedel_coverage 0.769 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 4308 _reflns_number_total 4692 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file W-bisimido.cif _cod_data_source_block 7_12srv022 _cod_database_code 4515803 _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. ; _shelx_estimated_absorpt_t_max 0.509 _shelx_estimated_absorpt_t_min 0.352 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.7838(14) 0.2162(14) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances C5-C6 \\sim C7-C6 \\sim C7-C8 \\sim C9-C8 \\sim C9-C10 \\sim C5-C10 with sigma of 0.02 4. Rigid body (RIGU) restrains C5, C6, C7, C8, C9, C10 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B) 5.b Aromatic/amide H refined with riding coordinates: C7(H7), C9(H9), C13(H13), C15(H15) 5.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C4(H4A,H4B,H4C) ; _twin_special_details ; Twin components were deconvoluted using CELL_NOW 2008/4 (Sheldrick, 2008a). Twin law: rotation by 180\% about reciprocal axis [0 0.852 1] and real axis [0 1 0.989]. Integrated using SAINT V7.46A to generate a combined raw intensity file in MUL file. Reduced using TWINABS 2012/1 to generate structure factors in HKLF5 format, from all observations involving domains 1 and 2: 6368 data ( 1984 unique ) involve domain 1 only, mean I/sigma 14.8 6470 data ( 1995 unique ) involve domain 2 only, mean I/sigma 6.7 12979 data ( 4559 unique ) involve 2 domains, mean I/sigma 14.5 ; _shelx_res_file ; TITL twin4 in P212121 #19 12srv022.res created by SHELXL-2016/6 at 15:05:26 on 27-Oct-2017 REM reset to P212121 #19 CELL 0.71073 12.0005 12.4893 13.5857 90 90 90 ZERR 4 0.0005 0.0005 0.0006 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H Cl F N O W UNIT 64 56 8 24 8 8 4 SADI C5 C6 C7 C6 C7 C8 C9 C8 C9 C10 C5 C10 RIGU C5 C6 C7 C8 C9 C10 L.S. 7 PLAN 10 SIZE 0.13 0.15 0.22 TEMP -153.15 BOND fmap 2 acta OMIT 7 3 6 OMIT 4 -2 -6 OMIT -7 2 -8 OMIT 3 -2 -6 OMIT -5 2 6 REM REM REM WGHT 0.047000 4.046000 BASF 0.21619 FVAR 0.32446 W 7 0.368311 0.597590 0.619960 11.00000 0.02250 0.01863 = 0.01633 0.00023 0.00146 0.00017 CL1 3 0.534185 0.623867 0.711521 11.00000 0.02440 0.03598 = 0.02637 -0.00692 -0.00397 -0.00055 CL2 3 0.192547 0.520504 0.581539 11.00000 0.02480 0.02820 = 0.02141 -0.00119 0.00001 -0.00343 F1 4 0.447809 0.430431 0.356511 11.00000 0.04541 0.02365 = 0.02700 -0.00728 0.01116 -0.00991 F2 4 0.586001 0.686005 0.134583 11.00000 0.04099 0.04866 = 0.02219 0.00617 0.00669 -0.00683 F3 4 0.510293 0.782516 0.461407 11.00000 0.04121 0.02169 = 0.03297 -0.00157 0.01088 -0.00832 F4 4 0.271036 0.777252 0.423704 11.00000 0.04656 0.03102 = 0.02078 -0.00694 -0.00489 0.00544 F5 4 0.207741 1.138360 0.501377 11.00000 0.04160 0.02500 = 0.04139 0.00287 -0.00475 0.00640 F6 4 0.315208 0.898715 0.748915 11.00000 0.05379 0.02568 = 0.01900 -0.00470 -0.00834 0.00049 O1 6 0.401494 0.422169 0.664129 11.00000 0.03530 0.01921 = 0.01861 -0.00117 0.00318 0.00405 O2 6 0.304954 0.568360 0.779345 11.00000 0.03399 0.01741 = 0.01949 0.00456 0.00019 0.00465 N1 5 0.431216 0.580496 0.504050 11.00000 0.02300 0.02026 = 0.01761 -0.00082 -0.00662 -0.00282 N2 5 0.323576 0.730852 0.618999 11.00000 0.02717 0.02583 = 0.02524 -0.00682 -0.00154 -0.00703 C1 1 0.414820 0.338513 0.591030 11.00000 0.05526 0.01980 = 0.02385 -0.00726 0.00371 0.01048 AFIX 137 H1A 2 0.455940 0.366809 0.534396 11.00000 -1.50000 H1B 2 0.341298 0.313648 0.569505 11.00000 -1.50000 H1C 2 0.456225 0.278553 0.619794 11.00000 -1.50000 AFIX 0 C2 1 0.335332 0.383798 0.745925 11.00000 0.05829 0.02262 = 0.02156 0.01105 0.00816 0.00668 AFIX 23 H2A 2 0.366035 0.315500 0.771075 11.00000 -1.20000 H2B 2 0.257453 0.371462 0.724732 11.00000 -1.20000 AFIX 0 C3 1 0.339253 0.467530 0.824209 11.00000 0.05192 0.02042 = 0.02706 0.00775 -0.00464 0.00370 AFIX 23 H3A 2 0.288296 0.448498 0.878780 11.00000 -1.20000 H3B 2 0.415738 0.473840 0.850893 11.00000 -1.20000 AFIX 0 C4 1 0.305593 0.652824 0.850780 11.00000 0.03214 0.03050 = 0.01651 -0.00382 0.00169 -0.00173 AFIX 137 H4A 2 0.285069 0.720400 0.818913 11.00000 -1.50000 H4B 2 0.380302 0.659311 0.879291 11.00000 -1.50000 H4C 2 0.251844 0.636506 0.902975 11.00000 -1.50000 AFIX 0 C5 1 0.473338 0.605520 0.412443 11.00000 0.01631 0.02062 = 0.02097 0.00624 -0.00082 -0.00006 C6 1 0.479986 0.532814 0.336495 11.00000 0.02177 0.02292 = 0.02409 0.00443 -0.00151 -0.00916 C7 1 0.516457 0.555980 0.242821 11.00000 0.02365 0.03262 = 0.01913 -0.00349 0.00065 -0.00336 AFIX 43 H7 2 0.517521 0.503551 0.192167 11.00000 -1.20000 AFIX 0 C8 1 0.550965 0.658551 0.226967 11.00000 0.01897 0.03795 = 0.02351 0.01305 0.00170 -0.00260 C9 1 0.550246 0.737999 0.297832 11.00000 0.02123 0.02537 = 0.02728 0.01236 0.00683 -0.00147 AFIX 43 H9 2 0.575458 0.808609 0.284408 11.00000 -1.20000 AFIX 0 C10 1 0.510825 0.708579 0.388893 11.00000 0.02310 0.02306 = 0.02812 0.00094 0.00288 -0.00025 C11 1 0.294841 0.832790 0.588772 11.00000 0.01750 0.01769 = 0.02655 0.00557 -0.00225 -0.00055 C12 1 0.268364 0.857900 0.490650 11.00000 0.02654 0.02514 = 0.01948 -0.00416 0.00351 -0.00169 C13 1 0.238854 0.959813 0.459046 11.00000 0.02956 0.02262 = 0.01633 0.00683 -0.00497 -0.00037 AFIX 43 H13 2 0.219813 0.973784 0.392399 11.00000 -1.20000 AFIX 0 C14 1 0.238539 1.039289 0.528723 11.00000 0.01983 0.01696 = 0.03814 0.00433 0.00448 -0.00053 C15 1 0.264070 1.022111 0.626260 11.00000 0.03328 0.01696 = 0.02895 -0.00813 0.00171 -0.00241 AFIX 43 H15 2 0.262798 1.078707 0.672966 11.00000 -1.20000 AFIX 0 C16 1 0.291678 0.918527 0.653090 11.00000 0.02303 0.03293 = 0.01717 -0.00287 0.00196 -0.00278 HKLF 5 REM twin4 in P212121 #19 REM R1 = 0.0486 for 22160 Fo > 4sig(Fo) and 0.0580 for all 25431 data REM 265 parameters refined using 51 restraints END WGHT 0.0466 4.0083 REM Highest difference peak 1.931, deepest hole -1.399, 1-sigma level 0.194 Q1 1 0.3693 0.2045 0.6226 11.00000 0.05 1.93 Q2 1 0.6010 0.4058 0.1188 11.00000 0.05 1.77 Q3 1 0.1331 0.3987 0.6401 11.00000 0.05 1.72 Q4 1 0.3640 0.6651 0.6964 11.00000 0.05 1.23 Q5 1 0.3731 0.6017 0.5374 11.00000 0.05 1.13 Q6 1 0.3633 0.6735 0.5333 11.00000 0.05 0.99 Q7 1 0.6037 0.7950 0.1214 11.00000 0.05 0.97 Q8 1 0.3771 0.5689 0.6958 11.00000 0.05 0.97 Q9 1 0.3644 0.5867 0.7783 11.00000 0.05 0.95 Q10 1 0.3259 0.5938 0.7195 11.00000 0.05 0.87 ; _shelx_res_checksum 77216 _shelx_hkl_file ; -1 0 0 2.92120 3.28343 -2 1 0 0 2.92120 3.28343 1 1 0 0 1.14858 2.62123 -2 -1 0 0 1.14858 2.62123 1 -2 0 0 551.568 38.3361 -2 2 0 0 551.568 38.3361 1 2 0 0 584.265 36.2588 -2 -2 0 0 584.265 36.2588 1 -3 0 0 2.39735 8.39353 -2 3 0 0 2.39735 8.39353 1 3 0 0 5.98263 7.06712 -2 -3 0 0 5.98263 7.06712 1 -4 0 0 287.592 25.3917 -2 4 0 0 287.592 25.3917 1 4 0 0 308.365 24.3447 -2 -4 0 0 308.365 24.3447 1 5 0 0 -0.8904 8.56021 -2 -5 0 0 -0.8904 8.56021 1 -5 0 0 -10.600 8.79307 -2 5 0 0 -10.600 8.79307 1 6 0 0 590.222 42.4279 -2 -6 0 0 590.222 42.4279 1 -6 0 0 523.353 43.6963 -2 6 0 0 523.353 43.6963 1 -7 0 0 -7.0224 11.7789 -2 7 0 0 -7.0224 11.7789 1 7 0 0 -4.7817 10.9012 -2 -7 0 0 -4.7817 10.9012 1 8 0 0 1091.09 77.2367 -2 -8 0 0 1091.09 77.2367 1 -8 0 0 1141.51 82.4287 -2 8 0 0 1141.51 82.4287 1 -9 0 0 -7.1823 17.9434 -2 9 0 0 -7.1823 17.9434 1 9 0 0 -2.3990 10.5399 -2 -9 0 0 -2.3990 10.5399 1 -10 0 0 84.4420 23.6556 -2 10 0 0 84.4420 23.6556 1 10 0 0 95.0895 19.9867 -2 -10 0 0 95.0895 19.9867 1 11 0 0 -14.473 13.5415 -2 -11 0 0 -14.473 13.5415 1 -11 0 0 -7.0275 19.3618 -2 11 0 0 -7.0275 19.3618 1 -12 0 0 1642.12 119.354 -2 12 0 0 1642.12 119.354 1 12 0 0 1542.08 112.792 -2 -12 0 0 1542.08 112.792 1 13 0 0 -9.0273 15.0647 -2 -13 0 0 -9.0273 15.0647 1 -13 0 0 8.03386 21.4688 -2 13 0 0 8.03386 21.4688 1 -14 0 0 85.8693 28.0408 -2 14 0 0 85.8693 28.0408 1 14 0 0 54.5479 21.8594 -2 -14 0 0 54.5479 21.8594 1 -15 0 0 6.48329 23.8616 -2 15 0 0 6.48329 23.8616 1 15 0 0 -6.4295 18.2788 -2 -15 0 0 -6.4295 18.2788 1 0 0 1 4.37242 3.23824 -2 0 1 0 4.37242 3.23824 1 0 0 -1 1.80385 2.51388 -2 0 -1 0 1.80385 2.51388 1 0 1 0 3.76833 1.83479 1 0 1 0 -0.0478 1.75197 2 1 0 -1 3202.96 204.875 -2 -1 -1 0 3202.96 204.875 1 1 0 -1 3151.53 188.689 -2 -1 -1 0 3151.53 188.689 1 1 0 1 3285.59 189.180 -2 -1 1 0 3285.59 189.180 1 -1 0 1 3284.35 205.341 -2 1 1 0 3284.35 205.341 1 1 1 0 901.923 52.1062 2 -1 -1 0 765.212 54.0555 2 -1 1 0 892.000 52.1238 2 1 -1 0 818.238 53.8676 2 1 1 0 2634.54 164.892 1 1 1 0 2627.40 158.970 1 -1 1 0 2683.59 164.690 1 -1 1 0 2629.59 159.540 1 2 0 -1 2925.99 173.131 -2 -2 -1 0 2925.99 173.131 1 2 0 1 2969.12 173.486 -2 -2 1 0 2969.12 173.486 1 -2 1 0 443.669 30.1611 2 -2 -1 0 410.666 30.5444 2 -2 1 0 420.806 27.0508 2 2 -1 0 1503.39 91.7361 1 2 1 0 1510.55 91.9589 1 2 1 0 1305.60 87.2346 1 3 -1 0 4764.70 303.175 1 3 1 0 4989.17 303.616 1 3 0 -1 7440.62 431.954 -2 -3 -1 0 7440.62 431.954 1 3 0 1 7406.45 432.223 -2 -3 1 0 7406.45 432.223 1 -3 -1 0 1424.29 94.8221 2 -3 1 0 1541.69 94.4972 2 -3 1 0 1422.76 88.5798 2 4 0 -1 4202.00 244.439 -2 -4 -1 0 4202.00 244.439 1 -4 0 1 4091.55 259.863 -2 4 1 0 4091.55 259.863 1 4 0 1 4120.66 244.807 -2 -4 1 0 4120.66 244.807 1 -4 -1 0 1262.88 84.5174 2 4 -1 0 3756.36 236.359 1 -5 0 1 4028.44 254.616 -2 5 1 0 4028.44 254.616 1 -5 0 1 4435.78 269.021 -2 5 1 0 4435.78 269.021 1 -5 0 -1 4252.64 268.664 -2 5 -1 0 4252.64 268.664 1 5 0 -1 4290.69 252.945 -2 -5 -1 0 4290.69 252.945 1 5 0 1 4280.54 253.161 -2 -5 1 0 4280.54 253.161 1 6 0 1 1595.99 101.804 -2 -6 1 0 1595.99 101.804 1 -6 0 -1 1638.54 107.784 -2 6 -1 0 1638.54 107.784 1 -6 0 1 1624.98 107.866 -2 6 1 0 1624.98 107.866 1 6 0 -1 1493.89 100.735 -2 -6 -1 0 1493.89 100.735 1 7 0 1 411.145 34.6871 -2 -7 1 0 411.145 34.6871 1 7 0 -1 347.774 33.0858 -2 -7 -1 0 347.774 33.0858 1 -7 0 -1 391.215 36.0464 -2 7 -1 0 391.215 36.0464 1 -7 0 1 379.240 36.1382 -2 7 1 0 379.240 36.1382 1 -8 0 -1 37.0439 17.4500 -2 8 -1 0 37.0439 17.4500 1 8 0 1 32.5294 14.2044 -2 -8 1 0 32.5294 14.2044 1 -8 0 1 46.8676 16.6672 -2 8 1 0 46.8676 16.6672 1 8 0 -1 43.6115 14.4071 -2 -8 -1 0 43.6115 14.4071 1 -9 0 1 388.578 37.9593 -2 9 1 0 388.578 37.9593 1 9 0 1 380.450 36.8704 -2 -9 1 0 380.450 36.8704 1 -9 0 -1 362.903 39.2043 -2 9 -1 0 362.903 39.2043 1 9 0 -1 377.709 36.0214 -2 -9 -1 0 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195.698 30.3605 -2 -8 10 -1 195.698 30.3605 1 -9 2 -11 117.883 33.3226 -2 9 -10 1 117.883 33.3226 1 9 0 11 51.5381 23.0933 -2 -9 10 1 51.5381 23.0933 1 9 0 -11 125.399 24.8732 -2 -9 -10 -1 125.399 24.8732 1 9 -2 11 107.012 25.6387 -2 -9 10 -1 107.012 25.6387 1 9 2 -11 138.322 25.5313 -2 -9 -10 1 138.322 25.5313 1 -9 0 11 115.340 23.7220 -2 9 10 1 115.340 23.7220 1 -9 0 -11 91.7711 27.9938 -2 9 -10 -1 91.7711 27.9938 1 -9 -10 1 87.3471 23.0685 1 10 0 -11 348.252 40.1769 -2 -10 -10 -1 348.252 40.1769 1 10 0 11 363.960 42.8698 -2 -10 10 1 363.960 42.8698 1 -10 2 -11 435.997 49.0395 -2 10 -10 1 435.997 49.0395 1 10 2 -11 320.817 40.9311 -2 -10 -10 1 320.817 40.9311 1 10 -2 11 350.267 41.8816 -2 -10 10 -1 350.267 41.8816 1 10 2 -11 356.048 41.0531 -2 -10 -10 1 356.048 41.0531 1 -10 0 -11 390.297 46.1818 -2 10 -10 -1 390.297 46.1818 1 11 0 11 546.571 53.1648 -2 -11 10 1 546.571 53.1648 1 11 0 -11 414.674 46.6386 -2 -11 -10 -1 414.674 46.6386 1 -11 2 -11 357.994 48.6117 -2 11 -10 1 357.994 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12 1 271.378 34.1150 1 -3 0 -13 286.178 35.6866 -2 3 -12 -1 286.178 35.6866 1 3 -2 13 334.121 38.5156 -2 -3 12 -1 334.121 38.5156 1 -4 2 -13 437.951 45.4651 -2 4 -12 1 437.951 45.4651 1 -4 -2 13 419.208 42.6823 -2 4 12 -1 419.208 42.6823 1 -4 2 -13 351.105 39.3297 -2 4 -12 1 351.105 39.3297 1 4 0 13 484.847 44.8464 -2 -4 12 1 484.847 44.8464 1 4 0 -13 406.944 39.2083 -2 -4 -12 -1 406.944 39.2083 1 4 0 13 415.525 40.7138 -2 -4 12 1 415.525 40.7138 1 4 -2 13 400.903 42.4585 -2 -4 12 -1 400.903 42.4585 1 -4 0 -13 379.895 43.5914 -2 4 -12 -1 379.895 43.5914 1 -4 0 13 434.414 42.9177 -2 4 12 1 434.414 42.9177 1 -5 2 -13 454.573 46.2008 -2 5 -12 1 454.573 46.2008 1 5 0 -13 200.743 27.2574 -2 -5 -12 -1 200.743 27.2574 1 5 0 13 226.524 30.3601 -2 -5 12 1 226.524 30.3601 1 -5 0 13 277.799 32.5808 -2 5 12 1 277.799 32.5808 1 5 -2 13 392.908 43.2092 -2 -5 12 -1 392.908 43.2092 1 6 0 -13 319.166 33.1343 -2 -6 -12 -1 319.166 33.1343 1 -6 2 -13 85.8124 25.0763 -2 6 -12 1 85.8124 25.0763 1 -6 -2 13 106.950 29.6696 -2 6 12 -1 106.950 29.6696 1 6 -2 13 92.4436 26.0590 -2 -6 12 -1 92.4436 26.0590 1 6 -2 13 86.2035 22.6391 -2 -6 12 -1 86.2035 22.6391 1 -6 0 13 260.318 34.3085 -2 6 12 1 260.318 34.3085 1 -6 0 -13 324.487 37.6769 -2 6 -12 -1 324.487 37.6769 1 -7 -2 13 158.805 33.9854 -2 7 12 -1 158.805 33.9854 1 -7 2 -13 128.390 27.8800 -2 7 -12 1 128.390 27.8800 1 7 0 -13 120.662 22.3433 -2 -7 -12 -1 120.662 22.3433 1 7 0 13 132.987 28.3083 -2 -7 12 1 132.987 28.3083 1 -7 0 13 147.585 25.7066 -2 7 12 1 147.585 25.7066 1 -7 0 -13 160.866 28.9228 -2 7 -12 -1 160.866 28.9228 1 7 -2 13 105.196 23.8166 -2 -7 12 -1 105.196 23.8166 1 -8 -2 13 334.259 45.0388 -2 8 12 -1 334.259 45.0388 1 -8 2 -13 326.169 42.1843 -2 8 -12 1 326.169 42.1843 1 8 0 13 307.657 39.4445 -2 -8 12 1 307.657 39.4445 1 8 0 -13 282.267 34.6312 -2 -8 -12 -1 282.267 34.6312 1 8 -2 13 252.793 34.9704 -2 -8 12 -1 252.793 34.9704 1 8 2 -13 252.283 38.6634 -2 -8 -12 1 252.283 38.6634 1 -8 0 -13 343.933 40.5778 -2 8 -12 -1 343.933 40.5778 1 -8 0 13 290.835 35.7313 -2 8 12 1 290.835 35.7313 1 -9 2 -13 309.142 43.6019 -2 9 -12 1 309.142 43.6019 1 -9 -2 13 376.432 49.9183 -2 9 12 -1 376.432 49.9183 1 9 0 13 207.312 33.6407 -2 -9 12 1 207.312 33.6407 1 9 0 -13 203.443 29.7076 -2 -9 -12 -1 203.443 29.7076 1 9 2 -13 375.820 44.7854 -2 -9 -12 1 375.820 44.7854 1 9 -2 13 305.591 37.7181 -2 -9 12 -1 305.591 37.7181 1 -9 0 -13 314.048 39.0487 -2 9 -12 -1 314.048 39.0487 1 10 0 13 141.063 28.5315 -2 -10 12 1 141.063 28.5315 1 10 0 -13 113.050 25.2678 -2 -10 -12 -1 113.050 25.2678 1 -10 2 -13 114.075 31.6366 -2 10 -12 1 114.075 31.6366 1 10 -2 13 94.4000 26.4172 -2 -10 12 -1 94.4000 26.4172 1 10 2 -13 120.215 29.1999 -2 -10 -12 1 120.215 29.1999 1 -10 0 -13 128.968 31.2910 -2 10 -12 -1 128.968 31.2910 1 0 -2 14 712.052 60.2862 -2 0 13 -1 712.052 60.2862 1 0 0 14 716.344 60.0939 -2 0 13 1 716.344 60.0939 1 0 0 -14 602.858 56.8133 -2 0 -13 -1 602.858 56.8133 1 1 0 -14 430.450 43.4630 -2 -1 -13 -1 430.450 43.4630 1 1 0 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885.052 61.1589 1 -3 4 2 891.194 61.8356 1 -3 4 2 930.166 60.5027 1 -3 4 2 220.282 21.8035 2 -3 4 2 260.217 21.4392 2 3 -2 4 2396.70 144.086 -2 -3 4 -2 2396.70 144.086 1 3 2 -4 2415.50 142.334 -2 -3 -4 2 2415.50 142.334 1 3 -2 4 2380.02 154.636 -2 -3 4 -2 2380.02 154.636 1 3 2 -4 2450.32 149.141 -2 -3 -4 2 2450.32 149.141 1 3 4 2 906.482 61.6564 1 3 -4 -2 996.561 63.2515 1 3 4 2 880.618 61.3146 1 3 -4 -2 224.798 22.7570 2 3 4 2 273.942 24.4289 2 -3 -4 2 285.103 27.7854 2 3 4 2 289.897 22.5356 2 -4 -2 4 210.980 27.1025 -2 4 4 -2 210.980 27.1025 1 -4 2 -4 215.785 21.2090 -2 4 -4 2 215.785 21.2090 1 -4 -2 4 254.357 25.9599 -2 4 4 -2 254.357 25.9599 1 -4 -4 -2 152.637 18.4360 1 -4 4 2 118.492 14.0284 1 -4 4 2 143.705 18.5287 1 -4 4 2 34.9970 8.95036 2 -4 4 2 39.1267 8.85395 2 4 4 2 59.7476 13.3738 2 -4 -4 2 48.1012 13.3315 2 4 4 2 48.1560 9.45451 2 4 -4 -2 43.2116 12.2581 2 4 4 2 161.230 17.4455 1 4 4 2 152.696 16.4917 1 4 -4 -2 176.884 18.2210 1 4 -2 4 249.507 23.4187 -2 -4 4 -2 249.507 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479.778 48.6638 1 13 -4 5 513.559 52.4072 -2 -13 5 -4 513.559 52.4072 1 -14 4 -5 158.151 36.7030 -2 14 -5 4 158.151 36.7030 1 -14 -4 5 87.2179 25.4692 -2 14 5 -4 87.2179 25.4692 1 -14 -4 5 89.8819 30.6863 -2 14 5 -4 89.8819 30.6863 1 14 3 6 30.3931 20.6245 -2 -14 5 4 30.3931 20.6245 1 14 -3 -6 21.3962 20.3920 -2 -14 -5 -4 21.3962 20.3920 1 14 -4 5 105.455 29.6218 -2 -14 5 -4 105.455 29.6218 1 14 4 -5 77.4013 23.4103 -2 -14 -5 4 77.4013 23.4103 1 -14 -3 -6 85.0461 38.8507 -2 14 -5 -4 85.0461 38.8507 1 0 -4 6 1546.84 105.346 -2 0 6 -4 1546.84 105.346 1 0 4 -6 1529.61 102.032 -2 0 -6 4 1529.61 102.032 1 0 -4 6 1500.27 104.716 -2 0 6 -4 1500.27 104.716 1 0 6 4 484.388 39.4832 2 0 6 4 1425.19 94.5838 1 0 -3 -7 1606.21 106.060 -2 0 -6 -4 1606.21 106.060 1 -1 -4 6 756.908 57.5371 -2 1 6 -4 756.908 57.5371 1 -1 -4 6 728.234 56.5846 -2 1 6 -4 728.234 56.5846 1 -1 4 -6 763.011 55.1437 -2 1 -6 4 763.011 55.1437 1 1 -3 -7 1057.33 68.9117 -2 -1 -6 -4 1057.33 68.9117 1 -1 6 4 152.570 18.7972 2 -1 6 4 448.330 33.8620 1 1 -4 6 692.626 56.5853 -2 -1 6 -4 692.626 56.5853 1 1 4 -6 703.392 55.1035 -2 -1 -6 4 703.392 55.1035 1 -1 -3 -7 849.055 67.4266 -2 1 -6 -4 849.055 67.4266 1 1 6 4 119.887 17.5047 2 1 6 4 335.238 31.8599 1 -2 6 4 22.1798 10.7130 2 -2 -6 -4 36.5632 9.52307 2 -2 -4 6 746.633 58.9499 -2 2 6 -4 746.633 58.9499 1 -2 -4 6 719.941 59.8516 -2 2 6 -4 719.941 59.8516 1 -2 4 -6 834.412 57.3339 -2 2 -6 4 834.412 57.3339 1 2 -3 -7 248.673 28.2388 -2 -2 -6 -4 248.673 28.2388 1 -2 6 4 122.538 16.9632 1 2 -4 6 708.214 59.0590 -2 -2 6 -4 708.214 59.0590 1 2 4 -6 795.293 57.2965 -2 -2 -6 4 795.293 57.2965 1 2 6 4 124.687 17.1462 1 -2 6 -4 163.078 13.8491 1 2 -6 -4 137.391 14.7294 1 -2 -3 -7 297.059 31.3452 -2 2 -6 -4 297.059 31.3452 1 2 6 4 36.6357 11.0496 2 -3 -6 -4 465.179 38.3394 2 -3 6 4 452.324 38.9753 2 3 6 -4 507.269 32.4836 2 -3 -4 6 2059.80 139.785 -2 3 6 -4 2059.80 139.785 1 -3 4 -6 2022.20 131.470 -2 3 -6 4 2022.20 131.470 1 -3 -4 6 1988.80 137.662 -2 3 6 -4 1988.80 137.662 1 3 -3 -7 1619.11 107.882 -2 -3 -6 -4 1619.11 107.882 1 3 3 7 1698.59 109.112 -2 -3 6 4 1698.59 109.112 1 -3 6 4 1532.01 100.964 1 3 4 -6 1994.15 120.582 -2 -3 -6 4 1994.15 120.582 1 3 -4 6 2013.94 136.718 -2 -3 6 -4 2013.94 136.718 1 3 4 -6 2078.09 132.530 -2 -3 -6 4 2078.09 132.530 1 3 6 4 1487.51 101.768 1 -3 6 -4 1608.09 95.4275 1 3 -6 -4 1504.10 100.869 1 3 6 4 482.113 39.1006 2 4 3 7 1979.55 123.832 -2 -4 6 4 1979.55 123.832 1 4 -3 -7 1790.54 121.359 -2 -4 -6 -4 1790.54 121.359 1 -4 4 -6 1959.41 125.734 -2 4 -6 4 1959.41 125.734 1 -4 -4 6 2021.88 135.307 -2 4 6 -4 2021.88 135.307 1 -4 -4 6 1910.83 132.871 -2 4 6 -4 1910.83 132.871 1 -4 6 4 493.686 42.9485 2 4 6 -4 570.044 38.0871 2 -4 -6 -4 549.342 44.0867 2 -4 6 4 1856.03 115.635 1 4 4 -6 1944.01 127.173 -2 -4 -6 4 1944.01 127.173 1 4 4 -6 1863.69 116.838 -2 -4 -6 4 1863.69 116.838 1 4 -4 6 1874.23 131.711 -2 -4 6 -4 1874.23 131.711 1 4 -6 -4 1730.86 116.762 1 4 6 4 1692.72 114.305 1 -4 6 -4 1818.25 110.594 1 4 6 4 1755.14 115.776 1 4 6 4 544.713 42.6270 2 -5 6 4 85.8600 15.0053 1 -5 -4 6 210.791 28.7635 -2 5 6 -4 210.791 28.7635 1 -5 -4 6 207.785 31.8615 -2 5 6 -4 207.785 31.8615 1 -5 4 -6 201.617 24.4961 -2 5 -6 4 201.617 24.4961 1 -5 6 4 26.1229 10.8291 2 5 6 -4 16.9939 8.21825 2 5 -3 -7 253.358 30.1090 -2 -5 -6 -4 253.358 30.1090 1 5 3 7 339.316 34.5746 -2 -5 6 4 339.316 34.5746 1 5 6 4 106.078 18.2231 1 5 6 4 93.4276 14.7936 1 5 4 -6 251.788 22.1202 -2 -5 -6 4 251.788 22.1202 1 5 4 -6 291.218 29.0188 -2 -5 -6 4 291.218 29.0188 1 5 -4 6 232.907 23.8690 -2 -5 6 -4 232.907 23.8690 1 -5 -3 -7 402.023 33.2991 -2 5 -6 -4 402.023 33.2991 1 5 6 4 28.1457 10.0626 2 -6 -4 6 319.295 36.6686 -2 6 6 -4 319.295 36.6686 1 -6 4 -6 250.772 25.1803 -2 6 -6 4 250.772 25.1803 1 -6 -4 6 235.224 30.6593 -2 6 6 -4 235.224 30.6593 1 -6 6 4 6.21249 8.29876 2 -6 6 4 83.4239 14.7404 1 6 3 7 99.4616 21.7967 -2 -6 6 4 99.4616 21.7967 1 6 -3 -7 103.284 18.8311 -2 -6 -6 -4 103.284 18.8311 1 6 -4 6 240.995 31.0059 -2 -6 6 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368.379 46.1082 -2 10 6 -4 368.379 46.1082 1 -10 -4 6 370.754 43.8414 -2 10 6 -4 370.754 43.8414 1 10 -4 6 432.440 42.8884 -2 -10 6 -4 432.440 42.8884 1 10 4 -6 383.425 37.8143 -2 -10 -6 4 383.425 37.8143 1 -10 3 7 226.998 28.6453 -2 10 6 4 226.998 28.6453 1 -10 -3 -7 241.796 36.3930 -2 10 -6 -4 241.796 36.3930 1 -11 -4 6 192.508 36.0580 -2 11 6 -4 192.508 36.0580 1 -11 -4 6 201.881 32.5562 -2 11 6 -4 201.881 32.5562 1 11 3 7 213.703 34.1863 -2 -11 6 4 213.703 34.1863 1 11 -3 -7 198.625 30.7760 -2 -11 -6 -4 198.625 30.7760 1 11 4 -6 221.212 28.0555 -2 -11 -6 4 221.212 28.0555 1 11 -4 6 188.518 31.4584 -2 -11 6 -4 188.518 31.4584 1 -11 -3 -7 255.928 44.8608 -2 11 -6 -4 255.928 44.8608 1 -12 -4 6 477.712 53.3716 -2 12 6 -4 477.712 53.3716 1 -12 -4 6 423.276 52.3752 -2 12 6 -4 423.276 52.3752 1 12 3 7 507.957 51.9044 -2 -12 6 4 507.957 51.9044 1 12 -3 -7 390.957 46.9506 -2 -12 -6 -4 390.957 46.9506 1 -12 -3 -7 548.280 58.9145 -2 12 -6 -4 548.280 58.9145 1 12 -4 6 518.841 51.0490 -2 -12 6 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760.775 53.2854 -2 0 -7 4 760.775 53.2854 1 0 -4 7 593.329 49.3101 -2 0 7 -4 593.329 49.3101 1 0 -4 7 560.340 51.1534 -2 0 7 -4 560.340 51.1534 1 -1 4 -7 170.215 24.9381 -2 1 -7 4 170.215 24.9381 1 -1 -4 7 135.159 26.5213 -2 1 7 -4 135.159 26.5213 1 -1 -4 7 154.740 21.8236 -2 1 7 -4 154.740 21.8236 1 1 -7 4 32.2755 6.83610 1 1 3 8 123.307 18.8465 -2 -1 7 4 123.307 18.8465 1 1 -3 -8 108.242 21.2448 -2 -1 -7 -4 108.242 21.2448 1 -1 -3 -8 81.6548 21.1178 -2 1 -7 -4 81.6548 21.1178 1 -1 3 8 103.316 18.2705 -2 1 7 4 103.316 18.2705 1 1 4 -7 171.395 24.4341 -2 -1 -7 4 171.395 24.4341 1 1 -4 7 152.702 25.0372 -2 -1 7 -4 152.702 25.0372 1 -2 4 -7 3204.12 205.986 -2 2 -7 4 3204.12 205.986 1 -2 -4 7 3239.53 213.827 -2 2 7 -4 3239.53 213.827 1 -2 -4 7 3340.75 217.591 -2 2 7 -4 3340.75 217.591 1 2 3 8 3770.10 234.254 -2 -2 7 4 3770.10 234.254 1 2 -3 -8 3793.44 230.442 -2 -2 -7 -4 3793.44 230.442 1 2 -4 7 3394.41 214.615 -2 -2 7 -4 3394.41 214.615 1 2 4 -7 3144.99 206.501 -2 -2 -7 4 3144.99 206.501 1 -2 7 -4 3070.70 182.675 1 -2 3 8 3769.01 234.784 -2 2 7 4 3769.01 234.784 1 -2 -3 -8 3700.36 231.644 -2 2 -7 -4 3700.36 231.644 1 -3 -4 7 1036.80 78.1293 -2 3 7 -4 1036.80 78.1293 1 -3 4 -7 1096.39 74.4763 -2 3 -7 4 1096.39 74.4763 1 -3 -4 7 992.274 77.5776 -2 3 7 -4 992.274 77.5776 1 3 3 8 511.111 39.7816 -2 -3 7 4 511.111 39.7816 1 3 -3 -8 456.126 39.8453 -2 -3 -7 -4 456.126 39.8453 1 -3 3 8 480.944 40.3033 -2 3 7 4 480.944 40.3033 1 -3 -3 -8 392.168 35.3586 -2 3 -7 -4 392.168 35.3586 1 3 4 -7 1127.04 75.9145 -2 -3 -7 4 1127.04 75.9145 1 3 4 -7 903.248 62.8355 -2 -3 -7 4 903.248 62.8355 1 -3 7 -4 454.629 33.6674 1 4 3 8 108.788 21.6469 -2 -4 7 4 108.788 21.6469 1 4 -3 -8 138.418 20.9368 -2 -4 -7 -4 138.418 20.9368 1 4 3 8 120.087 19.3684 -2 -4 7 4 120.087 19.3684 1 -4 4 -7 317.970 33.1523 -2 4 -7 4 317.970 33.1523 1 -4 -4 7 289.220 35.2301 -2 4 7 -4 289.220 35.2301 1 -4 -4 7 310.073 38.8669 -2 4 7 -4 310.073 38.8669 1 4 7 -4 15.6762 7.08338 2 -4 7 4 24.9110 7.13696 2 -4 7 -4 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325.689 49.5792 1 -4 -14 -6 364.865 53.3768 -2 4 -4 -16 364.865 53.3768 1 4 4 16 59.6135 20.9501 2 -5 -4 -16 125.004 30.4724 1 -5 4 16 93.5470 25.2975 1 -5 4 16 18.3459 16.5854 2 -5 15 -3 125.968 30.5098 -2 5 -4 16 125.968 30.5098 1 -5 -15 3 151.907 41.8017 -2 5 4 -16 151.907 41.8017 1 5 -15 3 170.348 36.9190 -2 -5 4 -16 170.348 36.9190 1 5 15 -3 138.002 29.0871 -2 -5 -4 16 138.002 29.0871 1 5 4 16 15.2765 15.4934 2 -5 -14 -6 121.506 39.6488 -2 5 -4 -16 121.506 39.6488 1 5 4 16 145.496 31.2965 1 0 5 16 75.9953 23.1478 2 0 14 7 447.598 52.2879 -2 0 5 16 447.598 52.2879 1 0 -14 -7 443.253 57.7423 -2 0 -5 -16 443.253 57.7423 1 0 15 -4 280.882 40.6619 -2 0 -5 16 280.882 40.6619 1 -1 5 16 48.4354 19.4949 2 1 14 7 346.076 47.2849 -2 -1 5 16 346.076 47.2849 1 1 -14 -7 367.761 53.9339 -2 -1 -5 -16 367.761 53.9339 1 -1 15 -4 413.305 50.8622 -2 1 -5 16 413.305 50.8622 1 1 5 16 64.6357 22.8129 2 1 15 -4 508.000 54.7481 -2 -1 -5 16 508.000 54.7481 1 -1 14 7 379.863 47.7481 -2 1 5 16 379.863 47.7481 1 -1 -14 -7 400.612 54.3050 -2 1 -5 -16 400.612 54.3050 1 2 -14 -7 32.0705 36.2298 -2 -2 -5 -16 32.0705 36.2298 1 2 14 7 58.9026 26.8225 -2 -2 5 16 58.9026 26.8225 1 -2 5 16 -17.197 12.8688 2 -2 15 -4 39.3136 25.9080 -2 2 -5 16 39.3136 25.9080 1 -2 14 7 15.3890 28.1175 -2 2 5 16 15.3890 28.1175 1 -2 -14 -7 51.3164 37.8581 -2 2 -5 -16 51.3164 37.8581 1 2 15 -4 36.9826 23.7129 -2 -2 -5 16 36.9826 23.7129 1 2 5 16 -11.881 13.7312 2 -3 5 16 17.4544 17.9117 2 3 -14 -7 314.703 51.5807 -2 -3 -5 -16 314.703 51.5807 1 3 14 7 304.348 43.2400 -2 -3 5 16 304.348 43.2400 1 -3 15 -4 316.635 44.3717 -2 3 -5 16 316.635 44.3717 1 3 15 -4 322.242 42.9396 -2 -3 -5 16 322.242 42.9396 1 -3 14 7 346.738 47.6353 -2 3 5 16 346.738 47.6353 1 -3 -14 -7 354.011 53.5572 -2 3 -5 -16 354.011 53.5572 1 3 5 16 56.6241 20.6855 2 4 -14 -7 269.089 45.8721 -2 -4 -5 -16 269.089 45.8721 1 4 14 7 258.082 39.1452 -2 -4 5 16 258.082 39.1452 1 -4 5 16 57.9977 22.4347 2 -4 15 -4 155.213 33.7078 -2 4 -5 16 155.213 33.7078 1 -4 14 7 198.219 40.4089 -2 4 5 16 198.219 40.4089 1 -4 -14 -7 181.828 43.3694 -2 4 -5 -16 181.828 43.3694 1 4 5 16 29.4172 17.9521 2 4 15 -4 155.934 32.8035 -2 -4 -5 16 155.934 32.8035 1 0 -14 -8 602.306 66.6036 -2 0 -6 -16 602.306 66.6036 1 0 14 8 557.567 60.8022 -2 0 6 16 557.567 60.8022 1 0 15 -5 532.851 60.1385 -2 0 -6 16 532.851 60.1385 1 1 14 8 201.248 37.5042 -2 -1 6 16 201.248 37.5042 1 1 -14 -8 159.056 43.0709 -2 -1 -6 -16 159.056 43.0709 1 -1 15 -5 161.311 35.0855 -2 1 -6 16 161.311 35.0855 1 1 15 -5 286.120 40.8599 -2 -1 -6 16 286.120 40.8599 1 -1 -14 -8 181.505 42.4435 -2 1 -6 -16 181.505 42.4435 1 -1 14 8 269.350 40.4155 -2 1 6 16 269.350 40.4155 1 2 -14 -8 16.7854 34.5740 -2 -2 -6 -16 16.7854 34.5740 1 2 14 8 51.3280 27.2516 -2 -2 6 16 51.3280 27.2516 1 -2 15 -5 128.549 32.8272 -2 2 -6 16 128.549 32.8272 1 2 15 -5 117.613 30.9172 -2 -2 -6 16 117.613 30.9172 1 -2 -14 -8 16.6986 34.7716 -2 2 -6 -16 16.6986 34.7716 1 -2 14 8 29.8993 28.2598 -2 2 6 16 29.8993 28.2598 1 3 -14 -8 259.714 46.0452 -2 -3 -6 -16 259.714 46.0452 1 3 14 8 209.463 37.5106 -2 -3 6 16 209.463 37.5106 1 -3 15 -5 154.365 35.0529 -2 3 -6 16 154.365 35.0529 1 -3 14 8 211.231 37.8240 -2 3 6 16 211.231 37.8240 1 -3 -14 -8 214.925 44.3851 -2 3 -6 -16 214.925 44.3851 1 3 15 -5 163.925 35.4214 -2 -3 -6 16 163.925 35.4214 1 0 0 17 -11.542 13.5025 1 0 0 17 -11.665 13.3661 2 1 0 17 -3.9565 14.2049 1 -1 0 17 6.26965 15.2883 1 -1 0 17 -5.9952 12.7754 2 1 0 17 -19.398 12.4150 2 2 0 17 764.464 71.0440 1 -2 0 17 844.554 72.8128 1 2 0 17 141.249 29.4355 2 -2 0 17 138.346 28.4884 2 -3 0 17 10.6352 15.7468 1 3 0 17 0.23319 15.3726 1 -3 0 17 -1.7812 14.5316 2 3 0 17 -18.049 12.9373 2 4 0 17 -4.4675 17.9155 1 -4 0 17 29.3374 18.1633 1 4 0 17 -0.9251 15.3096 2 -4 0 17 -8.2382 13.4523 2 0 16 0 433.347 50.1362 -2 0 -1 17 433.347 50.1362 1 0 1 17 11.4184 15.6649 2 0 1 17 176.332 34.3818 1 -1 16 0 171.718 35.1346 -2 1 -1 17 171.718 35.1346 1 -1 1 17 158.954 31.7773 1 -1 1 17 -0.9200 14.4758 2 1 1 17 22.6619 16.4575 2 1 16 0 167.098 34.4324 -2 -1 -1 17 167.098 34.4324 1 1 1 17 160.443 33.2759 1 -2 1 17 20.9810 18.5762 1 -2 16 0 53.4150 28.3161 -2 2 -1 17 53.4150 28.3161 1 -2 1 17 -2.0160 13.7015 2 2 16 0 7.41597 26.1989 -2 -2 -1 17 7.41597 26.1989 1 2 1 17 4.53645 16.5390 1 2 1 17 -4.0927 15.2771 2 -3 1 17 477.064 51.6446 1 3 -1 17 546.225 54.9163 1 -3 1 17 63.7258 22.4337 2 -3 -1 17 35.5975 18.9648 2 3 1 17 83.6567 24.1777 2 3 1 17 552.682 55.7491 1 -3 -1 17 468.223 51.6852 1 4 -1 17 291.834 38.4746 1 -4 1 17 282.595 37.8429 1 -4 1 17 39.8136 19.6103 2 -4 -1 17 255.793 35.5501 1 4 1 17 265.173 37.9165 1 -4 1 -17 119.766 28.0145 2 4 1 17 54.3001 20.0783 2 -4 -1 17 43.9082 20.0079 2 0 16 -1 -4.2388 23.4552 -2 0 -2 17 -4.2388 23.4552 1 0 2 17 23.7568 17.6851 1 0 -2 -17 -12.156 21.2160 2 0 2 17 -0.1299 13.8876 2 -1 2 17 54.6038 19.7362 2 -1 -2 -17 112.745 31.2338 2 -1 2 17 438.522 47.9065 1 -1 16 -1 441.475 53.0457 -2 1 -2 17 441.475 53.0457 1 1 -2 -17 123.654 30.5837 2 1 2 17 75.2604 22.0070 2 1 16 -1 508.036 55.1029 -2 -1 -2 17 508.036 55.1029 1 1 2 17 405.019 46.7936 1 -2 2 17 12.7280 14.1856 2 -2 -2 -17 2.10414 22.4047 2 -2 16 -1 147.124 33.5504 -2 2 -2 17 147.124 33.5504 1 -2 2 17 99.2291 26.4244 1 2 2 17 110.813 29.5207 1 2 2 17 6.24091 15.0623 2 2 -2 -17 -1.0176 19.2397 2 2 16 -1 171.911 34.3445 -2 -2 -2 17 171.911 34.3445 1 -3 2 17 238.785 40.0655 1 3 -2 17 280.674 37.5236 1 -3 2 17 31.9200 18.3536 2 -3 -2 -17 64.6567 26.2273 2 3 2 -17 96.9809 26.5548 2 -3 -2 17 265.247 37.2150 1 3 2 17 268.556 37.0625 1 3 2 17 47.7682 20.7907 2 -3 2 -17 90.1236 27.1496 2 0 3 17 493.970 52.3553 1 0 -3 -17 493.265 52.8687 1 0 16 -2 502.453 54.6913 -2 0 -3 17 502.453 54.6913 1 0 3 17 51.4686 21.0477 2 -1 16 -2 138.881 31.1154 -2 1 -3 17 138.881 31.1154 1 -1 -3 -17 64.6048 23.9383 1 -1 3 17 45.2800 21.8611 1 -1 3 17 9.96858 15.9718 2 1 3 17 12.0161 16.3668 2 1 16 -2 128.851 29.2175 -2 -1 -3 17 128.851 29.2175 1 1 3 17 34.0140 19.0531 1 -1 -15 -5 96.7565 37.7044 -2 1 -3 -17 96.7565 37.7044 1 2 3 -17 55.5566 23.1939 2 -2 3 17 -4.8083 14.3117 2 -2 -3 -17 15.0279 16.3509 1 2 -3 17 29.1161 19.8335 1 -2 3 17 2.72986 16.3041 1 2 3 -17 23.9258 23.6404 1 -2 -3 17 20.1546 17.2484 1 2 3 17 25.8266 20.7253 1 2 -3 -17 2.19380 16.9789 1 -2 3 -17 0.89791 14.2012 2 2 3 17 -11.665 14.0468 2 3 -3 17 112.983 27.8063 1 -3 -3 -17 96.9112 26.0328 1 -3 3 17 51.9000 22.9767 1 3 3 -17 84.5607 30.0207 1 3 3 -17 31.3570 21.1484 2 -3 3 17 11.0906 16.5091 2 3 -3 -17 106.602 28.8397 1 -3 -3 17 76.0560 24.1373 1 3 3 17 79.0298 26.0355 1 -3 3 -17 20.5080 18.3881 2 3 3 17 9.10026 16.4921 2 0 -4 17 7.31644 16.3042 1 0 4 -17 3.71732 21.6078 1 0 4 17 8.60951 15.2687 2 0 4 -17 9.89604 16.3312 2 0 -4 17 1.91497 16.8062 2 0 -15 -6 224.076 45.6917 -2 0 -4 -17 224.076 45.6917 1 0 15 6 222.209 39.0421 -2 0 4 17 222.209 39.0421 1 1 -15 -6 153.928 38.7812 -2 -1 -4 -17 153.928 38.7812 1 1 15 6 66.4709 29.6603 -2 -1 4 17 66.4709 29.6603 1 1 -4 17 144.241 30.7825 1 1 4 -17 120.831 33.2136 1 -1 4 17 7.82543 15.8234 2 1 4 -17 76.6787 23.7044 2 1 -4 17 48.8862 18.2108 2 -1 4 -17 90.3624 29.2876 1 -1 -4 17 155.271 30.1169 1 1 4 17 13.2197 17.3086 2 -1 4 -17 65.8456 22.6182 2 -1 -4 17 13.0910 17.5351 2 -1 -15 -6 76.2314 38.8920 -2 1 -4 -17 76.2314 38.8920 1 -1 15 6 109.393 33.3927 -2 1 4 17 109.393 33.3927 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 66735 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -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 W W 0.36831(6) 0.59759(6) 0.61996(5) 0.01915(18) Uani 1 1 d . . Cl1 Cl 0.5342(4) 0.6239(4) 0.7115(4) 0.0289(12) Uani 1 1 d . . Cl2 Cl 0.1925(4) 0.5205(4) 0.5815(4) 0.0248(10) Uani 1 1 d . . F1 F 0.4478(10) 0.4304(9) 0.3565(8) 0.032(3) Uani 1 1 d . . F2 F 0.5860(10) 0.6860(10) 0.1346(9) 0.037(3) Uani 1 1 d . . F3 F 0.5103(10) 0.7825(9) 0.4614(9) 0.032(3) Uani 1 1 d . . F4 F 0.2710(10) 0.7773(10) 0.4237(8) 0.033(3) Uani 1 1 d . . F5 F 0.2077(11) 1.1384(10) 0.5014(10) 0.036(3) Uani 1 1 d . . F6 F 0.3152(10) 0.8987(11) 0.7489(8) 0.033(3) Uani 1 1 d . . O1 O 0.4015(11) 0.4222(10) 0.6641(9) 0.024(3) Uani 1 1 d . . O2 O 0.3050(11) 0.5684(10) 0.7793(10) 0.024(3) Uani 1 1 d . . N1 N 0.4312(12) 0.5805(13) 0.5041(11) 0.020(3) Uani 1 1 d . . N2 N 0.3236(13) 0.7309(12) 0.6190(14) 0.026(3) Uani 1 1 d . . C1 C 0.415(2) 0.3385(16) 0.5910(15) 0.033(5) Uani 1 1 d . . H1A H 0.455940 0.366809 0.534396 0.049 Uiso 1 1 calc GR . H1B H 0.341298 0.313648 0.569505 0.049 Uiso 1 1 calc GR . H1C H 0.456225 0.278553 0.619794 0.049 Uiso 1 1 calc GR . C2 C 0.335(2) 0.3838(16) 0.7459(15) 0.034(6) Uani 1 1 d . . H2A H 0.366035 0.315500 0.771075 0.041 Uiso 1 1 calc R . H2B H 0.257453 0.371462 0.724732 0.041 Uiso 1 1 calc R . C3 C 0.3393(19) 0.4675(16) 0.8242(16) 0.033(5) Uani 1 1 d . . H3A H 0.288296 0.448498 0.878780 0.040 Uiso 1 1 calc R . H3B H 0.415738 0.473840 0.850893 0.040 Uiso 1 1 calc R . C4 C 0.3056(18) 0.6528(17) 0.8508(14) 0.026(4) Uani 1 1 d . . H4A H 0.285069 0.720400 0.818913 0.040 Uiso 1 1 calc GR . H4B H 0.380302 0.659311 0.879291 0.040 Uiso 1 1 calc GR . H4C H 0.251844 0.636506 0.902975 0.040 Uiso 1 1 calc GR . C5 C 0.4733(14) 0.6055(16) 0.4124(12) 0.019(4) Uani 1 1 d D U C6 C 0.4800(16) 0.5328(16) 0.3365(14) 0.023(4) Uani 1 1 d D U C7 C 0.5165(17) 0.5560(16) 0.2428(15) 0.025(4) Uani 1 1 d D U H7 H 0.517521 0.503551 0.192167 0.030 Uiso 1 1 calc R . C8 C 0.5510(16) 0.6586(17) 0.2270(15) 0.027(5) Uani 1 1 d D U C9 C 0.5502(16) 0.7380(16) 0.2978(14) 0.025(4) Uani 1 1 d D U H9 H 0.575458 0.808609 0.284408 0.030 Uiso 1 1 calc R . C10 C 0.5108(15) 0.7086(15) 0.3889(15) 0.025(4) Uani 1 1 d D U C11 C 0.2948(16) 0.8328(15) 0.5888(14) 0.021(4) Uani 1 1 d . . C12 C 0.2684(17) 0.8579(17) 0.4907(15) 0.024(4) Uani 1 1 d . . C13 C 0.2389(17) 0.9598(15) 0.4590(15) 0.023(4) Uani 1 1 d . . H13 H 0.219813 0.973784 0.392399 0.027 Uiso 1 1 calc R . C14 C 0.2385(16) 1.0393(16) 0.5287(17) 0.025(5) Uani 1 1 d . . C15 C 0.2641(16) 1.0221(15) 0.6263(18) 0.026(4) Uani 1 1 d . . H15 H 0.262798 1.078707 0.672966 0.032 Uiso 1 1 calc R . C16 C 0.2917(16) 0.9185(18) 0.6531(13) 0.024(4) 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 0.0225(3) 0.0186(3) 0.0163(3) 0.0002(3) 0.0015(3) 0.0002(3) Cl1 0.024(3) 0.036(3) 0.026(3) -0.007(2) -0.004(2) -0.001(2) Cl2 0.025(3) 0.028(3) 0.021(2) -0.001(2) 0.0000(19) -0.003(2) F1 0.045(7) 0.024(6) 0.027(7) -0.007(5) 0.011(5) -0.010(5) F2 0.041(7) 0.049(8) 0.022(7) 0.006(6) 0.007(5) -0.007(6) F3 0.041(7) 0.022(6) 0.033(7) -0.002(5) 0.011(5) -0.008(5) F4 0.047(8) 0.031(7) 0.021(6) -0.007(6) -0.005(5) 0.005(6) F5 0.042(8) 0.025(7) 0.041(8) 0.003(6) -0.005(6) 0.006(6) F6 0.054(7) 0.026(6) 0.019(6) -0.005(6) -0.008(5) 0.000(7) O1 0.035(8) 0.019(7) 0.019(6) -0.001(5) 0.003(5) 0.004(5) O2 0.034(8) 0.017(7) 0.019(7) 0.005(5) 0.000(6) 0.005(6) N1 0.023(8) 0.020(9) 0.018(8) -0.001(7) -0.007(6) -0.003(7) N2 0.027(8) 0.026(8) 0.025(8) -0.007(9) -0.002(8) -0.007(6) C1 0.055(14) 0.020(11) 0.024(11) -0.007(8) 0.004(9) 0.010(9) C2 0.058(15) 0.023(12) 0.022(10) 0.011(9) 0.008(9) 0.007(9) C3 0.052(16) 0.020(11) 0.027(12) 0.008(9) -0.005(10) 0.004(9) C4 0.032(12) 0.031(11) 0.017(10) -0.004(8) 0.002(8) -0.002(9) C5 0.016(8) 0.021(9) 0.021(8) 0.006(7) -0.001(6) 0.000(8) C6 0.022(10) 0.023(10) 0.024(9) 0.004(8) -0.002(8) -0.009(8) C7 0.024(11) 0.033(10) 0.019(9) -0.003(8) 0.001(8) -0.003(8) C8 0.019(11) 0.038(11) 0.024(10) 0.013(8) 0.002(8) -0.003(9) C9 0.021(10) 0.025(10) 0.027(10) 0.012(8) 0.007(8) -0.001(8) C10 0.023(9) 0.023(9) 0.028(10) 0.001(9) 0.003(9) 0.000(7) C11 0.018(9) 0.018(10) 0.027(10) 0.006(8) -0.002(7) -0.001(7) C12 0.027(11) 0.025(11) 0.019(10) -0.004(8) 0.004(8) -0.002(8) C13 0.030(11) 0.023(11) 0.016(10) 0.007(8) -0.005(8) 0.000(8) C14 0.020(10) 0.017(11) 0.038(12) 0.004(9) 0.004(9) -0.001(8) C15 0.033(11) 0.017(9) 0.029(11) -0.008(11) 0.002(10) -0.002(8) C16 0.023(10) 0.033(12) 0.017(9) -0.003(9) 0.002(7) -0.003(9) 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Cl1 W Cl2 156.46(18) O1 W Cl1 81.4(4) O1 W Cl2 80.0(4) O1 W O2 70.4(4) O2 W Cl1 78.9(4) O2 W Cl2 81.4(4) N1 W Cl1 97.2(5) N1 W Cl2 97.8(5) N1 W O1 92.5(6) N1 W O2 162.8(6) N2 W Cl1 97.5(5) N2 W Cl2 96.4(5) N2 W O1 163.5(7) N2 W O2 93.2(7) N2 W N1 103.9(8) C1 O1 W 121.7(11) C2 O1 W 114.8(11) C2 O1 C1 110.3(15) C3 O2 W 115.6(12) C4 O2 W 120.9(11) C4 O2 C3 110.5(14) C5 N1 W 159.6(15) C11 N2 W 162.9(17) O1 C2 C3 107.3(17) O2 C3 C2 107.4(16) N1 C5 C10 122.2(17) C6 C5 N1 123.2(16) C6 C5 C10 114.6(16) F1 C6 C5 116.9(16) F1 C6 C7 118.1(17) C7 C6 C5 124.9(18) C8 C7 C6 116.1(19) F2 C8 C9 117.5(17) C7 C8 F2 118.3(19) C7 C8 C9 124.2(18) C10 C9 C8 115.9(17) F3 C10 C5 117.4(17) F3 C10 C9 118.4(16) C9 C10 C5 124.2(18) N2 C11 C12 122.9(19) N2 C11 C16 122.2(18) C16 C11 C12 114.9(18) F4 C12 C11 117.7(18) F4 C12 C13 118.6(18) C13 C12 C11 123.7(19) C14 C13 C12 116.8(18) F5 C14 C13 118.4(19) F5 C14 C15 118.1(19) C13 C14 C15 123.4(18) C14 C15 C16 116.9(19) F6 C16 C11 117.4(18) F6 C16 C15 118.3(19) C11 C16 C15 124.3(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance W Cl1 2.370(5) W Cl2 2.377(5) W O1 2.306(12) W O2 2.324(13) W N1 1.759(15) W N2 1.749(15) F1 C6 1.36(2) F2 C8 1.37(2) F3 C10 1.35(2) F4 C12 1.36(2) F5 C14 1.34(2) F6 C16 1.35(2) O1 C1 1.45(2) O1 C2 1.45(2) O2 C3 1.46(2) O2 C4 1.43(2) N1 C5 1.38(2) N2 C11 1.38(2) C2 C3 1.49(3) C5 C6 1.38(2) C5 C10 1.40(2) C6 C7 1.38(2) C7 C8 1.36(2) C8 C9 1.38(2) C9 C10 1.37(2) C11 C12 1.41(3) C11 C16 1.38(3) C12 C13 1.39(3) C13 C14 1.37(3) C14 C15 1.38(3) C15 C16 1.38(3) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.7838(14) ref 1 0 0 0 1 0 0 0 1 2 0.2162(14) mt_II -1 0 0 0 -0.074 0.915 0 1.087 0.074