#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:47:08 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515785.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_4515785 loop_ _publ_author_name 'Messinis, Antonis M.' 'Wright, William R. H.' 'Batsanov, Andrei S.' 'Howard, Judith A. K.' 'Hanton, Martin J.' 'Dyer, Philip W.' _publ_section_title ; Exploration of Homogeneous Ethylene Dimerization Mediated by Tungsten Mono(imido) Complexes ; _journal_issue 12 _journal_name_full 'ACS Catalysis' _journal_page_first 11235 _journal_paper_doi 10.1021/acscatal.8b02201 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C16 H25 Cl4 N O W' _chemical_formula_sum 'C16 H25 Cl4 N O W' _chemical_formula_weight 573.02 _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 heavy _atom_sites_solution_secondary difmap _audit_creation_date 2016-11-30 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267) ; _cell_angle_alpha 95.674(10) _cell_angle_beta 98.423(9) _cell_angle_gamma 97.281(9) _cell_formula_units_Z 4 _cell_length_a 8.5798(7) _cell_length_b 14.0708(10) _cell_length_c 17.3875(14) _cell_measurement_reflns_used 9973 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 34.58 _cell_measurement_theta_min 2.39 _cell_volume 2044.9(3) _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 2014/7 multi-CPU version (Sheldrick, 2015)' _computing_structure_solution 'SHELXS 2013/1 (Sheldrick, 2008)' _diffrn_ambient_temperature 120.0 _diffrn_detector_area_resol_mean 5.6 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.948 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_unetI/netI 0.0417 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.948 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 47614 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.948 _diffrn_reflns_theta_full 32.500 _diffrn_reflns_theta_max 34.987 _diffrn_reflns_theta_min 1.192 _diffrn_source 'sealed X-ray tube' _exptl_absorpt_coefficient_mu 6.174 _exptl_absorpt_correction_T_max 0.8004 _exptl_absorpt_correction_T_min 0.3666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0568 before and 0.0442 after correction. The Ratio of minimum to maximum transmission is 0.4580. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.861 _exptl_crystal_description blade _exptl_crystal_F_000 1112 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _refine_diff_density_max 3.136 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.150 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 443 _refine_ls_number_reflns 17049 _refine_ls_number_restraints 21 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0284 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.8250P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.0645 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13303 _reflns_number_total 17049 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b02201_si_002.cif _cod_data_source_block 2g _cod_database_code 4515785 _ccdc_comments 'redetermination of XAKNAB, CCDC-1434397' _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 0.790 _shelx_estimated_absorpt_t_min 0.319 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups 2. Restrained distances C23A-C24 \\sim C23B-C24 \\sim C26B-C25B \\sim C26A-C25A \\sim C25A-C24 \\sim C25B-C24 with sigma of 0.02 O2-C23A \\sim O2-C23B \\sim O2-C26B \\sim O2-C26A with sigma of 0.02 3. Others Uiso(H12A)=Uiso(H12B)=Uiso(H12C)=FVAR(1) Uiso(H13A)=Uiso(H13B)=Uiso(H13C)=FVAR(2) Uiso(H15A)=Uiso(H15B)=Uiso(H15C)=FVAR(3) Uiso(H16A)=Uiso(H16B)=Uiso(H16C)=FVAR(4) Uiso(H28A)=Uiso(H28B)=Uiso(H28C)=FVAR(5) Uiso(H29A)=Uiso(H29B)=Uiso(H29C)=FVAR(6) Uiso(H31A)=Uiso(H31B)=Uiso(H31C)=FVAR(7) Uiso(H32A)=Uiso(H32B)=Uiso(H32C)=FVAR(8) Fixed Sof: C23A(0.667) H23A(0.667) H23B(0.667) C23B(0.333) H23C(0.333) H23D(0.333) H24A(0.667) H24B(0.667) H24C(0.333) H24D(0.333) C25A(0.667) H25A(0.667) H25B(0.667) C25B(0.333) H25C(0.333) H25D(0.333) C26A(0.667) H26A(0.667) H26B(0.667) C26B(0.333) H26C(0.333) H26D(0.333) 4.a Riding coordinates: C3(H3), C4(H4), C5(H5), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11), C14(H14), C19(H19), C20(H20), C21(H21), C23A(H23A,H23B), C23B(H23C, H23D), C24(H24A,H24B), C24(H24C,H24D), C25A(H25A,H25B), C25B(H25C,H25D), C26A(H26A,H26B), C26B(H26C,H26D), C27(H27), C30(H30) 4.b Rotating group: C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B, H16C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A, H32B,H32C) ; _shelx_res_file ; test.res created by SHELXL-2014/7 TITL 11srv264 in P-1 #2 REM reset to P-1 #2 CELL 0.71073 8.5798 14.0708 17.3875 95.674 98.423 97.281 ZERR 4 0.0007 0.001 0.0014 0.01 0.009 0.009 LATT 1 SFAC C H Cl N O W UNIT 64 100 16 4 4 4 SADI C23A C24 C23B C24 C26B C25B C26A C25A C25A C24 C25B C24 SADI O2 C23A O2 C23B O2 C26B O2 C26A L.S. 7 PLAN 7 SIZE 0.04 0.1 0.24 TEMP -153.15 BOND fmap 2 acta 65 REM REM REM WGHT 0.024000 0.825000 FVAR 0.28278 0.06135 0.06143 0.04971 0.05094 0.09980 0.03656 FVAR 0.06735 0.06151 W1 6 0.083642 0.318004 0.653386 11.00000 0.01329 0.01644 = 0.01924 0.00275 0.00184 0.00283 CL1 3 -0.004449 0.330384 0.773592 11.00000 0.02249 0.02943 = 0.02193 0.00052 0.00625 0.00495 CL2 3 -0.081869 0.171336 0.615328 11.00000 0.02028 0.02077 = 0.03016 -0.00067 0.00247 -0.00090 CL3 3 0.123849 0.321945 0.523073 11.00000 0.02088 0.03344 = 0.02079 0.00766 0.00337 0.00655 CL4 3 0.201469 0.479774 0.678466 11.00000 0.02054 0.01794 = 0.03899 0.00360 0.00225 0.00107 O1 5 -0.139741 0.380165 0.613744 11.00000 0.01350 0.02315 = 0.03045 0.01142 0.00434 0.00462 N1 4 0.253720 0.269350 0.684672 11.00000 0.01824 0.01512 = 0.01694 0.00103 0.00152 0.00107 C1 1 0.387306 0.227387 0.709841 11.00000 0.01558 0.01860 = 0.01716 0.00532 0.00255 0.00385 C2 1 0.414839 0.144117 0.664190 11.00000 0.02236 0.02138 = 0.02117 0.00608 0.00751 0.00551 C3 1 0.548149 0.102446 0.691873 11.00000 0.02417 0.02268 = 0.03478 0.00758 0.01037 0.00965 AFIX 3 H3 2 0.570789 0.046416 0.662873 11.00000 -1.20000 AFIX 0 C4 1 0.647718 0.140915 0.760482 11.00000 0.01853 0.03177 = 0.03595 0.01643 0.00522 0.01041 AFIX 3 H4 2 0.737808 0.111205 0.777872 11.00000 -1.20000 AFIX 0 C5 1 0.617979 0.222225 0.804257 11.00000 0.02168 0.02941 = 0.02245 0.01165 0.00040 0.00472 AFIX 3 H5 2 0.687109 0.246805 0.851797 11.00000 -1.20000 AFIX 0 C6 1 0.488288 0.268938 0.779935 11.00000 0.01784 0.02136 = 0.01731 0.00561 0.00227 0.00152 C7 1 -0.301603 0.334565 0.619221 11.00000 0.01674 0.03820 = 0.04729 0.01673 0.00861 0.00514 AFIX 3 H7A 2 -0.305603 0.312885 0.671431 11.00000 -1.20000 H7B 2 -0.336673 0.278355 0.578681 11.00000 -1.20000 AFIX 0 C8 1 -0.404661 0.412454 0.606092 11.00000 0.01690 0.03188 = 0.03865 0.00995 0.00552 0.00600 AFIX 3 H8A 2 -0.407801 0.452224 0.655952 11.00000 -1.20000 H8B 2 -0.514671 0.384445 0.581872 11.00000 -1.20000 AFIX 0 C9 1 -0.323588 0.471728 0.550980 11.00000 0.02074 0.03330 = 0.02717 0.00944 0.00387 0.00911 AFIX 3 H9A 2 -0.350048 0.538338 0.554990 11.00000 -1.20000 H9B 2 -0.354458 0.441688 0.496000 11.00000 -1.20000 AFIX 0 C10 1 -0.147618 0.470806 0.579969 11.00000 0.01918 0.02704 = 0.04211 0.01703 0.01046 0.01088 AFIX 3 H10A 2 -0.086228 0.473396 0.536059 11.00000 -1.20000 H10B 2 -0.104308 0.526606 0.619949 11.00000 -1.20000 AFIX 0 C11 1 0.309550 0.102516 0.587521 11.00000 0.03288 0.02717 = 0.02354 -0.00184 0.00536 0.01017 AFIX 3 H11 2 0.215380 0.137946 0.581401 11.00000 -1.20000 AFIX 0 C12 1 0.398507 0.118884 0.519106 11.00000 0.05603 0.05211 = 0.02196 0.00981 0.00616 0.00028 AFIX 7 H12A 2 0.418994 0.188161 0.515054 11.00000 21.00000 H12B 2 0.333828 0.085658 0.470461 11.00000 21.00000 H12C 2 0.499890 0.093303 0.527893 11.00000 21.00000 AFIX 0 C13 1 0.248648 -0.003601 0.585746 11.00000 0.06558 0.03466 = 0.03083 -0.00500 0.00800 -0.01372 AFIX 7 H13A 2 0.338958 -0.039883 0.592367 11.00000 31.00000 H13B 2 0.180704 -0.027139 0.535369 11.00000 31.00000 H13C 2 0.186853 -0.012462 0.628301 11.00000 31.00000 AFIX 0 C14 1 0.457358 0.358853 0.827301 11.00000 0.02687 0.02593 = 0.02084 0.00087 -0.00205 0.00289 AFIX 3 H14 2 0.379808 0.390323 0.793271 11.00000 -1.20000 AFIX 0 C15 1 0.609127 0.431958 0.853871 11.00000 0.03970 0.03335 = 0.03871 -0.00043 -0.00053 -0.00381 AFIX 7 H15A 2 0.682200 0.405610 0.892179 11.00000 41.00000 H15B 2 0.581380 0.492231 0.877835 11.00000 41.00000 H15C 2 0.660670 0.444733 0.808479 11.00000 41.00000 AFIX 0 C16 1 0.381367 0.331652 0.897899 11.00000 0.03542 0.04553 = 0.02638 -0.00149 0.00839 0.00525 AFIX 7 H16A 2 0.281734 0.287777 0.879731 11.00000 51.00000 H16B 2 0.359138 0.390108 0.927368 11.00000 51.00000 H16C 2 0.454587 0.299673 0.931798 11.00000 51.00000 AFIX 0 W2 6 0.701055 0.797539 0.791523 11.00000 0.01826 0.01712 = 0.01716 0.00231 0.00118 0.00252 CL5 3 0.614056 0.933245 0.848526 11.00000 0.03055 0.02128 = 0.02840 0.00023 0.00760 0.00611 CL6 3 0.764584 0.882604 0.688873 11.00000 0.02705 0.03568 = 0.02168 0.01096 0.00458 0.00433 CL7 3 0.735513 0.655062 0.718200 11.00000 0.02701 0.02647 = 0.03332 -0.00799 -0.00170 0.00756 CL8 3 0.581487 0.705204 0.876685 11.00000 0.02636 0.02775 = 0.03204 0.01271 0.00584 0.00119 O2 5 0.455595 0.770776 0.720312 11.00000 0.01887 0.02919 = 0.01932 -0.00006 0.00068 0.00404 N2 4 0.890733 0.818514 0.845258 11.00000 0.02037 0.01632 = 0.01822 0.00294 0.00373 0.00190 C17 1 1.042228 0.834573 0.888394 11.00000 0.01838 0.01844 = 0.01415 -0.00015 0.00180 -0.00037 C18 1 1.102584 0.756446 0.922275 11.00000 0.02168 0.02129 = 0.01654 0.00154 0.00281 0.00369 C19 1 1.252791 0.776182 0.968497 11.00000 0.02406 0.03478 = 0.02467 0.00487 0.00097 0.00486 AFIX 3 H19 2 1.297632 0.725582 0.991957 11.00000 -1.20000 AFIX 0 C20 1 1.337089 0.867879 0.980698 11.00000 0.02197 0.04265 = 0.03666 0.00611 -0.00413 -0.00609 AFIX 3 H20 2 1.438199 0.879849 1.013328 11.00000 -1.20000 AFIX 0 C21 1 1.276639 0.943027 0.946023 11.00000 0.02745 0.03098 = 0.03449 0.00374 0.00306 -0.01063 AFIX 3 H21 2 1.337869 1.005387 0.954523 11.00000 -1.20000 AFIX 0 C22 1 1.128871 0.928753 0.899322 11.00000 0.02206 0.02086 = 0.01806 0.00086 0.00607 -0.00246 PART 1 C23A 1 0.411927 0.715429 0.642233 10.66700 0.01863 0.03157 = 0.02291 -0.00482 -0.00360 -0.00121 AFIX 3 H23A 2 0.419067 0.646209 0.645373 10.66700 -1.20000 H23B 2 0.483167 0.739529 0.606293 10.66700 -1.20000 AFIX 0 PART 0 PART 2 C23B 1 0.420789 0.764790 0.633832 10.33300 0.02558 AFIX 3 H23C 2 0.480639 0.717530 0.609482 10.33300 -1.20000 H23D 2 0.448509 0.828190 0.615362 10.33300 -1.20000 AFIX 0 PART 0 C24 1 0.242263 0.729652 0.614195 11.00000 0.02766 0.02908 = 0.03561 0.00263 -0.00771 0.00212 PART 1 AFIX 3 H24A 2 0.182903 0.672282 0.579775 10.66700 -1.20000 H24B 2 0.238723 0.787032 0.585655 10.66700 -1.20000 AFIX 3 PART 0 PART 2 H24C 2 0.195313 0.755742 0.566655 10.33300 -1.20000 H24D 2 0.219373 0.658312 0.605655 10.33300 -1.20000 AFIX 0 PART 0 PART 1 C25A 1 0.175111 0.745164 0.690066 10.66700 0.01518 0.03360 = 0.05076 -0.00194 -0.00074 0.00329 AFIX 3 H25A 2 0.083271 0.781364 0.683746 10.66700 -1.20000 H25B 2 0.141671 0.682584 0.708566 10.66700 -1.20000 AFIX 0 PART 0 PART 2 C25B 1 0.178849 0.768506 0.686044 10.33300 0.03825 AFIX 3 H25C 2 0.075289 0.730906 0.690024 10.33300 -1.20000 H25D 2 0.165239 0.837116 0.684164 10.33300 -1.20000 AFIX 0 PART 0 PART 1 C26A 1 0.313010 0.801272 0.746421 10.66700 0.02048 0.03791 = 0.03337 0.00028 0.00338 0.01208 AFIX 3 H26A 2 0.313150 0.871292 0.744051 10.66700 -1.20000 H26B 2 0.308130 0.787712 0.800871 10.66700 -1.20000 AFIX 0 PART 0 PART 2 C26B 1 0.306373 0.755957 0.751364 10.33300 0.02692 AFIX 3 H26C 2 0.307343 0.805187 0.796304 10.33300 -1.20000 H26D 2 0.287353 0.691057 0.768544 10.33300 -1.20000 AFIX 0 PART 0 C27 1 1.010124 0.655935 0.911231 11.00000 0.03394 0.01765 = 0.02328 0.00490 -0.00401 0.00381 AFIX 3 H27 2 0.916034 0.653035 0.869201 11.00000 -1.20000 AFIX 0 C28 1 1.112813 0.578163 0.886329 11.00000 0.06373 0.02014 = 0.05177 -0.00826 0.03274 0.00446 AFIX 7 H28A 2 1.155228 0.594037 0.839058 11.00000 61.00000 H28B 2 1.046638 0.514783 0.875450 11.00000 61.00000 H28C 2 1.201204 0.576690 0.928659 11.00000 61.00000 AFIX 0 C29 1 0.950261 0.634119 0.986621 11.00000 0.03554 0.02693 = 0.03958 0.00869 0.01293 0.00044 AFIX 7 H29A 2 1.041169 0.636894 1.028508 11.00000 71.00000 H29B 2 0.888200 0.569475 0.978679 11.00000 71.00000 H29C 2 0.882783 0.681928 1.001245 11.00000 71.00000 AFIX 0 C30 1 1.065282 1.011503 0.861094 11.00000 0.03144 0.01980 = 0.02431 0.00300 0.00581 -0.00254 AFIX 3 H30 2 0.955641 0.986803 0.832364 11.00000 -1.20000 AFIX 0 C31 1 1.166033 1.046020 0.801377 11.00000 0.09747 0.04525 = 0.05167 0.02429 0.04960 0.02936 AFIX 7 H31A 2 1.275975 1.067284 0.827366 11.00000 81.00000 H31B 2 1.123119 1.099954 0.778300 11.00000 81.00000 H31C 2 1.163934 0.992962 0.760054 11.00000 81.00000 AFIX 0 C32 1 1.052303 1.095677 0.920653 11.00000 0.06785 0.03154 = 0.03204 0.00039 0.01843 0.01763 AFIX 7 H32A 2 0.977128 1.074432 0.954963 11.00000 91.00000 H32B 2 1.014342 1.148040 0.893293 11.00000 91.00000 H32C 2 1.157120 1.118800 0.952132 11.00000 91.00000 AFIX 0 HKLF 4 REM 11srv264 in P-1 #2 REM R1 = 0.0284 for 13303 Fo > 4sig(Fo) and 0.0433 for all 17049 data REM 443 parameters refined using 21 restraints END WGHT 0.0242 0.8561 REM Highest difference peak 3.136, deepest hole -1.107, 1-sigma level 0.150 Q1 1 0.5372 0.1627 0.4856 11.00000 0.05 3.14 Q2 1 0.3184 0.2784 0.9298 11.00000 0.05 2.54 Q3 1 0.5127 0.0868 0.7617 11.00000 0.05 2.50 Q4 1 1.1290 0.5654 0.9025 11.00000 0.05 1.60 Q5 1 0.4843 0.1612 0.6134 11.00000 0.05 1.03 Q6 1 0.5705 0.6449 0.7623 11.00000 0.05 1.02 Q7 1 0.0997 0.3088 0.6217 11.00000 0.05 1.01 ; _shelx_res_checksum 32543 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.08364(2) 0.31800(2) 0.65339(2) 0.01630(3) Uani 1 1 d . . . . Cl1 Cl -0.00445(8) 0.33038(5) 0.77359(4) 0.02441(12) Uani 1 1 d . . . . Cl2 Cl -0.08187(8) 0.17134(5) 0.61533(4) 0.02449(12) Uani 1 1 d . . . . Cl3 Cl 0.12385(8) 0.32194(5) 0.52307(4) 0.02450(12) Uani 1 1 d . . . . Cl4 Cl 0.20147(8) 0.47977(5) 0.67847(4) 0.02622(13) Uani 1 1 d . . . . O1 O -0.1397(2) 0.38017(13) 0.61374(11) 0.0216(4) Uani 1 1 d . . . . N1 N 0.2537(2) 0.26935(15) 0.68467(12) 0.0171(4) Uani 1 1 d . . . . C1 C 0.3873(3) 0.22739(18) 0.70984(14) 0.0168(4) Uani 1 1 d . . . . C2 C 0.4148(3) 0.14412(19) 0.66419(15) 0.0208(5) Uani 1 1 d . . . . C3 C 0.5481(3) 0.1024(2) 0.69187(18) 0.0258(6) Uani 1 1 d . . . . H3 H 0.5708 0.0464 0.6629 0.031 Uiso 1 1 d R . . . C4 C 0.6477(3) 0.1409(2) 0.76048(18) 0.0272(6) Uani 1 1 d . . . . H4 H 0.7378 0.1112 0.7779 0.033 Uiso 1 1 d R . . . C5 C 0.6180(3) 0.2222(2) 0.80426(16) 0.0242(5) Uani 1 1 d . . . . H5 H 0.6871 0.2468 0.8518 0.029 Uiso 1 1 d R . . . C6 C 0.4883(3) 0.26894(18) 0.77994(14) 0.0188(5) Uani 1 1 d . . . . C7 C -0.3016(3) 0.3346(2) 0.6192(2) 0.0328(7) Uani 1 1 d . . . . H7A H -0.3056 0.3129 0.6714 0.039 Uiso 1 1 d R . . . H7B H -0.3367 0.2784 0.5787 0.039 Uiso 1 1 d R . . . C8 C -0.4047(3) 0.4125(2) 0.60609(19) 0.0284(6) Uani 1 1 d . . . . H8A H -0.4078 0.4522 0.6560 0.034 Uiso 1 1 d R . . . H8B H -0.5147 0.3844 0.5819 0.034 Uiso 1 1 d R . . . C9 C -0.3236(3) 0.4717(2) 0.55098(17) 0.0262(6) Uani 1 1 d . . . . H9A H -0.3500 0.5383 0.5550 0.031 Uiso 1 1 d R . . . H9B H -0.3545 0.4417 0.4960 0.031 Uiso 1 1 d R . . . C10 C -0.1476(3) 0.4708(2) 0.57997(19) 0.0273(6) Uani 1 1 d . . . . H10A H -0.0862 0.4734 0.5361 0.033 Uiso 1 1 d R . . . H10B H -0.1043 0.5266 0.6199 0.033 Uiso 1 1 d R . . . C11 C 0.3096(4) 0.1025(2) 0.58752(17) 0.0276(6) Uani 1 1 d . . . . H11 H 0.2154 0.1379 0.5814 0.033 Uiso 1 1 d R . . . C12 C 0.3985(5) 0.1189(3) 0.51911(19) 0.0437(9) Uani 1 1 d . . . . H12A H 0.4190 0.1882 0.5151 0.061(8) Uiso 1 1 d GR . . . H12B H 0.3338 0.0857 0.4705 0.061(8) Uiso 1 1 d GR . . . H12C H 0.4999 0.0933 0.5279 0.061(8) Uiso 1 1 d GR . . . C13 C 0.2486(5) -0.0036(3) 0.5857(2) 0.0461(9) Uani 1 1 d . . . . H13A H 0.3390 -0.0399 0.5924 0.061(8) Uiso 1 1 d GR . . . H13B H 0.1807 -0.0271 0.5354 0.061(8) Uiso 1 1 d GR . . . H13C H 0.1869 -0.0125 0.6283 0.061(8) Uiso 1 1 d GR . . . C14 C 0.4574(3) 0.3589(2) 0.82730(16) 0.0254(5) Uani 1 1 d . . . . H14 H 0.3798 0.3903 0.7933 0.030 Uiso 1 1 d R . . . C15 C 0.6091(4) 0.4320(2) 0.8539(2) 0.0391(8) Uani 1 1 d . . . . H15A H 0.6822 0.4056 0.8922 0.050(7) Uiso 1 1 d GR . . . H15B H 0.5814 0.4922 0.8778 0.050(7) Uiso 1 1 d GR . . . H15C H 0.6607 0.4447 0.8085 0.050(7) Uiso 1 1 d GR . . . C16 C 0.3814(4) 0.3317(3) 0.89790(18) 0.0359(7) Uani 1 1 d . . . . H16A H 0.2817 0.2878 0.8797 0.051(7) Uiso 1 1 d GR . . . H16B H 0.3591 0.3901 0.9274 0.051(7) Uiso 1 1 d GR . . . H16C H 0.4546 0.2997 0.9318 0.051(7) Uiso 1 1 d GR . . . W2 W 0.70105(2) 0.79754(2) 0.79152(2) 0.01767(3) Uani 1 1 d . . . . Cl5 Cl 0.61406(8) 0.93325(5) 0.84853(4) 0.02643(13) Uani 1 1 d . . . . Cl6 Cl 0.76458(8) 0.88260(5) 0.68887(4) 0.02757(14) Uani 1 1 d . . . . Cl7 Cl 0.73551(9) 0.65506(5) 0.71820(4) 0.03006(15) Uani 1 1 d . . . . Cl8 Cl 0.58149(8) 0.70520(5) 0.87669(4) 0.02821(14) Uani 1 1 d . . . . O2 O 0.4556(2) 0.77078(14) 0.72031(11) 0.0229(4) Uani 1 1 d D . . . N2 N 0.8907(3) 0.81851(15) 0.84526(12) 0.0182(4) Uani 1 1 d . . . . C17 C 1.0422(3) 0.83457(18) 0.88839(14) 0.0175(4) Uani 1 1 d . . . . C18 C 1.1026(3) 0.75645(19) 0.92228(15) 0.0199(5) Uani 1 1 d . . . . C19 C 1.2528(3) 0.7762(2) 0.96850(17) 0.0280(6) Uani 1 1 d . . . . H19 H 1.2976 0.7256 0.9920 0.034 Uiso 1 1 d R . . . C20 C 1.3371(4) 0.8679(3) 0.9807(2) 0.0355(7) Uani 1 1 d . . . . H20 H 1.4382 0.8798 1.0133 0.043 Uiso 1 1 d R . . . C21 C 1.2766(4) 0.9430(2) 0.94602(19) 0.0325(7) Uani 1 1 d . . . . H21 H 1.3379 1.0054 0.9545 0.039 Uiso 1 1 d R . . . C22 C 1.1289(3) 0.92875(19) 0.89932(15) 0.0206(5) Uani 1 1 d . . . . C23A C 0.4119(5) 0.7154(3) 0.6422(2) 0.0260(8) Uani 0.667 1 d D P A 1 H23A H 0.4191 0.6462 0.6454 0.031 Uiso 0.667 1 d R P A 1 H23B H 0.4832 0.7395 0.6063 0.031 Uiso 0.667 1 d R P A 1 C23B C 0.4208(9) 0.7648(7) 0.6338(5) 0.0256(17) Uiso 0.333 1 d D P A 2 H23C H 0.4806 0.7175 0.6095 0.031 Uiso 0.333 1 d R P A 2 H23D H 0.4485 0.8282 0.6154 0.031 Uiso 0.333 1 d R P A 2 C24 C 0.2423(4) 0.7297(2) 0.61419(19) 0.0323(7) Uani 1 1 d D . . . H24A H 0.1829 0.6723 0.5798 0.039 Uiso 0.667 1 d R P A 1 H24B H 0.2387 0.7870 0.5857 0.039 Uiso 0.667 1 d R P A 1 H24C H 0.1953 0.7557 0.5667 0.039 Uiso 0.333 1 d R P A 2 H24D H 0.2194 0.6583 0.6057 0.039 Uiso 0.333 1 d R P A 2 C25A C 0.1751(7) 0.7452(7) 0.6901(4) 0.0343(16) Uani 0.667 1 d D P A 1 H25A H 0.0833 0.7814 0.6837 0.041 Uiso 0.667 1 d R P A 1 H25B H 0.1417 0.6826 0.7086 0.041 Uiso 0.667 1 d R P A 1 C25B C 0.1788(19) 0.7685(13) 0.6860(7) 0.038(5) Uiso 0.333 1 d D P A 2 H25C H 0.0753 0.7309 0.6900 0.046 Uiso 0.333 1 d R P A 2 H25D H 0.1652 0.8371 0.6842 0.046 Uiso 0.333 1 d R P A 2 C26A C 0.3130(5) 0.8013(4) 0.7464(3) 0.0303(10) Uani 0.667 1 d D P A 1 H26A H 0.3131 0.8713 0.7441 0.036 Uiso 0.667 1 d R P A 1 H26B H 0.3081 0.7877 0.8009 0.036 Uiso 0.667 1 d R P A 1 C26B C 0.3064(10) 0.7560(7) 0.7514(5) 0.027(2) Uiso 0.333 1 d D P A 2 H26C H 0.3073 0.8052 0.7963 0.032 Uiso 0.333 1 d R P A 2 H26D H 0.2874 0.6911 0.7685 0.032 Uiso 0.333 1 d R P A 2 C27 C 1.0101(4) 0.65593(19) 0.91123(16) 0.0257(6) Uani 1 1 d . . . . H27 H 0.9160 0.6530 0.8692 0.031 Uiso 1 1 d R . . . C28 C 1.1128(5) 0.5782(2) 0.8863(2) 0.0438(9) Uani 1 1 d . . . . H28A H 1.1552 0.5940 0.8391 0.100(11) Uiso 1 1 d GR . . . H28B H 1.0466 0.5148 0.8754 0.100(11) Uiso 1 1 d GR . . . H28C H 1.2012 0.5767 0.9287 0.100(11) Uiso 1 1 d GR . . . C29 C 0.9503(4) 0.6341(2) 0.98662(19) 0.0334(7) Uani 1 1 d . . . . H29A H 1.0412 0.6369 1.0285 0.037(6) Uiso 1 1 d GR . . . H29B H 0.8882 0.5695 0.9787 0.037(6) Uiso 1 1 d GR . . . H29C H 0.8828 0.6819 1.0012 0.037(6) Uiso 1 1 d GR . . . C30 C 1.0653(4) 1.01150(19) 0.86109(16) 0.0256(5) Uani 1 1 d . . . . H30 H 0.9556 0.9868 0.8324 0.031 Uiso 1 1 d R . . . C31 C 1.1660(6) 1.0460(3) 0.8014(2) 0.0580(13) Uani 1 1 d . . . . H31A H 1.2760 1.0673 0.8274 0.067(8) Uiso 1 1 d GR . . . H31B H 1.1231 1.1000 0.7783 0.067(8) Uiso 1 1 d GR . . . H31C H 1.1639 0.9930 0.7601 0.067(8) Uiso 1 1 d GR . . . C32 C 1.0523(5) 1.0957(2) 0.9207(2) 0.0421(8) Uani 1 1 d . . . . H32A H 0.9771 1.0744 0.9550 0.062(8) Uiso 1 1 d GR . . . H32B H 1.0143 1.1480 0.8933 0.062(8) Uiso 1 1 d GR . . . H32C H 1.1571 1.1188 0.9521 0.062(8) Uiso 1 1 d GR . . . 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 W1 0.01329(4) 0.01644(5) 0.01924(5) 0.00275(3) 0.00184(3) 0.00283(3) Cl1 0.0225(3) 0.0294(3) 0.0219(3) 0.0005(2) 0.0063(2) 0.0050(2) Cl2 0.0203(3) 0.0208(3) 0.0302(3) -0.0007(2) 0.0025(2) -0.0009(2) Cl3 0.0209(3) 0.0334(3) 0.0208(3) 0.0077(2) 0.0034(2) 0.0066(2) Cl4 0.0205(3) 0.0179(3) 0.0390(4) 0.0036(2) 0.0023(3) 0.0011(2) O1 0.0135(8) 0.0232(9) 0.0305(10) 0.0114(8) 0.0043(7) 0.0046(7) N1 0.0182(9) 0.0151(9) 0.0169(9) 0.0010(7) 0.0015(7) 0.0011(7) C1 0.0156(10) 0.0186(11) 0.0172(11) 0.0053(8) 0.0026(8) 0.0039(8) C2 0.0224(12) 0.0214(12) 0.0212(12) 0.0061(9) 0.0075(10) 0.0055(10) C3 0.0242(13) 0.0227(13) 0.0348(15) 0.0076(11) 0.0104(11) 0.0096(10) C4 0.0185(12) 0.0318(15) 0.0359(15) 0.0164(12) 0.0052(11) 0.0104(11) C5 0.0217(12) 0.0294(14) 0.0224(13) 0.0117(10) 0.0004(10) 0.0047(10) C6 0.0178(11) 0.0214(12) 0.0173(11) 0.0056(9) 0.0023(9) 0.0015(9) C7 0.0167(12) 0.0382(17) 0.0473(19) 0.0167(14) 0.0086(12) 0.0051(12) C8 0.0169(12) 0.0319(15) 0.0386(16) 0.0099(12) 0.0055(11) 0.0060(11) C9 0.0207(12) 0.0333(15) 0.0272(14) 0.0094(11) 0.0039(10) 0.0091(11) C10 0.0192(12) 0.0270(14) 0.0421(17) 0.0170(12) 0.0105(11) 0.0109(10) C11 0.0329(15) 0.0272(14) 0.0235(13) -0.0018(10) 0.0054(11) 0.0102(12) C12 0.056(2) 0.052(2) 0.0220(15) 0.0098(14) 0.0062(15) 0.0003(18) C13 0.066(3) 0.0347(18) 0.0308(17) -0.0050(14) 0.0080(17) -0.0137(17) C14 0.0269(13) 0.0259(13) 0.0208(12) 0.0009(10) -0.0020(10) 0.0029(11) C15 0.0397(18) 0.0333(17) 0.0387(18) -0.0004(14) -0.0005(15) -0.0038(14) C16 0.0354(17) 0.0455(19) 0.0264(15) -0.0015(13) 0.0084(13) 0.0053(14) W2 0.01826(5) 0.01712(5) 0.01716(5) 0.00231(3) 0.00118(4) 0.00252(4) Cl5 0.0306(3) 0.0213(3) 0.0284(3) 0.0002(2) 0.0076(3) 0.0061(2) Cl6 0.0271(3) 0.0357(4) 0.0217(3) 0.0110(3) 0.0046(2) 0.0043(3) Cl7 0.0270(3) 0.0265(3) 0.0333(4) -0.0080(3) -0.0017(3) 0.0076(3) Cl8 0.0264(3) 0.0277(3) 0.0320(3) 0.0127(3) 0.0058(3) 0.0012(3) O2 0.0189(9) 0.0292(10) 0.0193(9) -0.0001(7) 0.0007(7) 0.0040(7) N2 0.0204(10) 0.0163(9) 0.0182(10) 0.0029(7) 0.0037(8) 0.0019(8) C17 0.0184(11) 0.0184(11) 0.0141(10) -0.0002(8) 0.0018(8) -0.0004(9) C18 0.0217(12) 0.0213(12) 0.0165(11) 0.0015(9) 0.0028(9) 0.0037(9) C19 0.0241(13) 0.0348(15) 0.0247(14) 0.0049(11) 0.0010(11) 0.0049(11) C20 0.0220(14) 0.0427(18) 0.0367(17) 0.0061(14) -0.0041(12) -0.0061(13) C21 0.0275(15) 0.0310(15) 0.0345(16) 0.0037(12) 0.0031(12) -0.0106(12) C22 0.0221(12) 0.0209(12) 0.0181(11) 0.0009(9) 0.0061(9) -0.0025(9) C23A 0.0186(18) 0.032(2) 0.023(2) -0.0048(17) -0.0036(15) -0.0012(16) C24 0.0277(15) 0.0291(15) 0.0356(16) 0.0026(12) -0.0077(12) 0.0021(12) C25A 0.015(2) 0.034(4) 0.051(4) -0.002(3) -0.0007(19) 0.003(2) C26A 0.020(2) 0.038(3) 0.033(2) 0.000(2) 0.0034(17) 0.0121(19) C27 0.0339(15) 0.0176(12) 0.0233(13) 0.0049(10) -0.0040(11) 0.0038(11) C28 0.064(2) 0.0201(14) 0.052(2) -0.0083(14) 0.0327(19) 0.0045(15) C29 0.0355(16) 0.0269(15) 0.0396(17) 0.0087(12) 0.0129(14) 0.0004(12) C30 0.0314(14) 0.0198(12) 0.0243(13) 0.0030(10) 0.0058(11) -0.0025(10) C31 0.097(4) 0.045(2) 0.052(2) 0.0243(18) 0.050(2) 0.029(2) C32 0.068(3) 0.0315(17) 0.0320(17) 0.0004(13) 0.0184(17) 0.0176(17) 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' 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 1.00 1.00 0.0200 0.00 -1.00 -1.00 0.0200 0.00 -2.00 1.00 0.0400 0.00 2.00 -1.00 0.0400 1.00 1.00 -1.00 0.0800 -1.00 2.00 -1.00 0.0800 3.00 -1.00 -2.00 0.1100 -1.00 0.00 1.00 0.1100 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Cl1 W1 Cl2 90.38(3) Cl1 W1 Cl3 167.40(2) Cl1 W1 Cl4 90.00(3) Cl2 W1 Cl3 88.97(3) Cl2 W1 Cl4 167.28(2) Cl4 W1 Cl3 87.90(3) O1 W1 Cl1 83.10(5) O1 W1 Cl2 83.25(5) O1 W1 Cl3 84.32(5) O1 W1 Cl4 84.17(5) N1 W1 Cl1 96.25(7) N1 W1 Cl2 96.27(7) N1 W1 Cl3 96.33(7) N1 W1 Cl4 96.32(7) N1 W1 O1 179.20(8) C7 O1 W1 124.22(16) C10 O1 W1 125.99(15) C10 O1 C7 109.78(19) C1 N1 W1 178.13(18) N1 C1 C2 118.1(2) N1 C1 C6 118.8(2) C6 C1 C2 123.1(2) C1 C2 C11 122.6(2) C3 C2 C1 116.8(2) C3 C2 C11 120.6(2) C4 C3 C2 121.4(3) C3 C4 C5 120.8(2) C4 C5 C6 121.3(3) C1 C6 C14 122.1(2) C5 C6 C1 116.7(2) C5 C6 C14 121.2(2) O1 C7 C8 104.7(2) C7 C8 C9 103.6(2) C8 C9 C10 102.9(2) O1 C10 C9 105.3(2) C2 C11 C12 110.2(3) C13 C11 C2 112.4(3) C13 C11 C12 110.5(3) C6 C14 C15 112.3(2) C6 C14 C16 110.1(2) C16 C14 C15 110.5(3) Cl5 W2 Cl6 89.62(3) Cl5 W2 Cl7 167.97(3) Cl5 W2 Cl8 89.61(3) Cl6 W2 Cl7 88.88(3) Cl8 W2 Cl6 167.15(3) Cl8 W2 Cl7 89.21(3) O2 W2 Cl5 84.05(5) O2 W2 Cl6 83.60(5) O2 W2 Cl7 83.92(5) O2 W2 Cl8 83.56(5) N2 W2 Cl5 96.16(7) N2 W2 Cl6 95.72(7) N2 W2 Cl7 95.86(7) N2 W2 Cl8 97.12(7) N2 W2 O2 179.29(9) C23A O2 W2 125.23(19) C23B O2 W2 124.8(3) C26A O2 W2 125.2(2) C26A O2 C23A 109.5(3) C26B O2 W2 125.8(4) C26B O2 C23B 109.4(5) C17 N2 W2 179.6(2) N2 C17 C18 118.4(2) N2 C17 C22 119.0(2) C22 C17 C18 122.5(2) C17 C18 C27 122.7(2) C19 C18 C17 117.0(2) C19 C18 C27 120.3(2) C20 C19 C18 121.1(3) C19 C20 C21 121.0(3) C22 C21 C20 121.1(3) C17 C22 C30 122.2(2) C21 C22 C17 117.3(3) C21 C22 C30 120.5(2) O2 C23A C24 105.4(3) O2 C23B C24 104.0(5) C23A C24 C25A 103.0(3) C25B C24 C23B 103.5(7) C26A C25A C24 103.6(4) C26B C25B C24 102.5(9) O2 C26A C25A 105.5(4) O2 C26B C25B 105.7(8) C18 C27 C28 111.8(3) C18 C27 C29 109.9(2) C29 C27 C28 109.6(2) C22 C30 C31 111.4(3) C22 C30 C32 112.4(2) C32 C30 C31 110.1(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance W1 Cl1 2.3225(7) W1 Cl2 2.3292(7) W1 Cl3 2.3463(7) W1 Cl4 2.3419(7) W1 O1 2.2518(17) W1 N1 1.729(2) O1 C7 1.475(3) O1 C10 1.461(3) N1 C1 1.389(3) C1 C2 1.414(4) C1 C6 1.414(3) C2 C3 1.396(4) C2 C11 1.515(4) C3 C4 1.379(4) C4 C5 1.383(4) C5 C6 1.397(4) C6 C14 1.514(4) C7 C8 1.507(4) C8 C9 1.518(4) C9 C10 1.522(4) C11 C12 1.525(4) C11 C13 1.514(4) C14 C15 1.535(4) C14 C16 1.531(4) W2 Cl5 2.3215(7) W2 Cl6 2.3361(7) W2 Cl7 2.3425(7) W2 Cl8 2.3282(7) W2 O2 2.2479(19) W2 N2 1.728(2) O2 C23A 1.469(4) O2 C23B 1.481(8) O2 C26A 1.464(4) O2 C26B 1.460(9) N2 C17 1.382(3) C17 C18 1.417(4) C17 C22 1.416(3) C18 C19 1.395(4) C18 C27 1.511(4) C19 C20 1.377(4) C20 C21 1.387(5) C21 C22 1.382(4) C22 C30 1.518(4) C23A C24 1.511(5) C23B C24 1.526(8) C24 C25A 1.522(7) C24 C25B 1.515(12) C25A C26A 1.501(7) C25B C26B 1.498(13) C27 C28 1.557(4) C27 C29 1.521(4) C30 C31 1.522(4) C30 C32 1.521(4)