#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:47:08 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515786.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_4515786 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 'C24 H34 Cl7 N2 W2 1-,C8 H20 N 1+' _chemical_formula_sum 'C32 H54 Cl7 N3 W2' _chemical_formula_weight 1096.63 _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' _space_group_name_H-M_alt 'P c c n' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_date 2016-12-26 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.5696(3) _cell_length_b 10.7140(3) _cell_length_c 40.8756(12) _cell_measurement_reflns_used 9187 _cell_measurement_temperature 120 _cell_measurement_theta_max 28.85 _cell_measurement_theta_min 2.75 _cell_volume 4190.9(2) _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 2014/7 multi-CPU version (Sheldrick, 2015)' _computing_structure_solution 'SHELXS 2013/1 (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 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method 'narrow-frame \w scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_unetI/netI 0.0191 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_number 50787 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 28.000 _diffrn_reflns_theta_max 28.998 _diffrn_reflns_theta_min 1.993 _diffrn_source 'sealed X-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.956 _exptl_absorpt_correction_T_max 0.6686 _exptl_absorpt_correction_T_min 0.1473 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; SADABS-2009/1 (Bruker, 2010) was used for absorption correction. wR2(int) was 0.0617 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.2203. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2136 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.06 _refine_diff_density_max 2.366 _refine_diff_density_min -3.684 _refine_diff_density_rms 0.199 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.287 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 235 _refine_ls_number_reflns 5565 _refine_ls_number_restraints 194 _refine_ls_restrained_S_all 1.285 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0926 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+92.2660P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1621 _refine_ls_wR_factor_ref 0.1673 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4705 _reflns_number_total 5565 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b02201_si_002.cif _cod_data_source_block 3 _cod_database_code 4515786 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.716 _shelx_estimated_absorpt_t_min 0.199 _olex2_refinement_description ; 1. 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, All C(H,H,H,H,H,H) groups 2. Restrained distances C14-C13 1.5 with sigma of 0.02 C5-C4B \\sim C5-C4A \\sim C6B-C5 \\sim C6A-C5 with sigma of 0.02 C16-C15B \\sim C16-C15A with sigma of 0.02 N2-C15B \\sim N2-C15A \\sim N2-C13 with sigma of 0.02 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(1) Uiso(H3A)=Uiso(H3B)=Uiso(H3C)=FVAR(2) Uiso(H4AA)=Uiso(H4AB)=Uiso(H4AC)=FVAR(3) Fixed Sof: H5A(0.67) H5B(0.33) C4A(0.67) H4AA(0.67) H4AB(0.67) H4AC(0.67) C6A(0.67) H6AA(0.67) H6AB(0.67) H6AC(0.67) C4B(0.33) H4BA(0.33) H4BB(0.33) H4BC(0.33) C6B(0.33) H6BA(0.33) H6BB(0.33) H6BC(0.33) C15A(0.5) H15A(0.5) H15B(0.5) C15B(0.5) H15C(0.5) H15D(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H16E(0.5) H16F(0.5) H16D(0.5) 5.a Riding coordinates: C5(H5A,H5B), C4B(H4BA,H4BB,H4BC), C6B(H6BA,H6BB,H6BC), C13(H13A,H13B), C15A(H15A,H15B), C15B(H15C,H15D), C16(H16A,H16B,H16C,H16E,H16F,H16D) 5.b Rotating group: C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4A(H4AA,H4AB,H4AC), C6A(H6AA,H6AB,H6AC) 5.c Ternary CH refined with riding coordinates: C2(H2) 5.d Aromatic/amide H refined with riding coordinates: C9(H9), C10(H10), C11(H11) 5.e Idealised Me refined as rotating group: C14(H14A,H14B,H14C) ; _shelx_res_file ; 13srv064.res created by SHELXL-2014/7 TITL 13srv064 in Pccn #56 REM reset to Pccn #56 CELL 0.71073 9.5696 10.714 40.8756 90 90 90 ZERR 4 0.0003 0.0003 0.0012 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,+Z SYMM 0.5+X,-Y,0.5-Z SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N W UNIT 128 216 28 12 8 DFIX 1.5 C14 C13 SADI C5 C4B C5 C4A C6B C5 C6A C5 SADI C16 C15B C16 C15A SADI N2 C15B N2 C15A N2 C13 RIGU L.S. 7 PLAN 20 TEMP -153.15 BIND C15A C16 BIND C16 H16d BIND H16e C16 BIND H16f C16 BOND fmap 2 acta 56 OMIT 7 4 13 OMIT 1 3 25 OMIT 7 3 15 OMIT 2 1 23 OMIT 7 4 3 OMIT 2 4 7 OMIT 8 4 5 OMIT 6 4 11 REM REM REM WGHT 0.000000 92.265938 FVAR 0.11874 0.04350 0.05448 0.08829 W 5 0.735945 0.618759 0.651154 11.00000 0.04772 0.08270 = 0.03825 0.02147 -0.00125 -0.01986 CL1 3 0.546289 0.766222 0.645108 11.00000 0.03928 0.07843 = 0.04012 -0.01595 0.00851 -0.01463 CL2 3 0.750000 0.750000 0.704337 10.50000 0.07395 0.17302 = 0.03122 0.00000 0.00000 -0.04401 CL3 3 0.551130 0.492420 0.670915 11.00000 0.07060 0.11557 = 0.06837 0.04449 0.00756 -0.03251 CL4 3 0.883325 0.473682 0.677964 11.00000 0.08064 0.13066 = 0.08959 0.07839 -0.00965 -0.01421 N1 4 0.740645 0.571018 0.610889 11.00000 0.02894 0.03871 = 0.05051 0.01198 0.00252 -0.01291 C1 1 0.425092 0.590902 0.580406 11.00000 0.02922 0.03826 = 0.05556 0.00030 0.00124 -0.00417 AFIX 7 H1A 2 0.346663 0.646412 0.585537 11.00000 21.00000 H1B 2 0.457913 0.550679 0.600535 11.00000 21.00000 H1C 2 0.394449 0.526994 0.564845 11.00000 21.00000 AFIX 0 C2 1 0.545179 0.667613 0.565162 11.00000 0.03172 0.03005 = 0.03341 -0.00617 -0.00437 -0.00717 AFIX 13 H2 2 0.582599 0.723599 0.582667 11.00000 -1.20000 AFIX 0 C3 1 0.489297 0.750725 0.538010 11.00000 0.04390 0.04846 = 0.05309 0.00560 -0.01137 -0.00410 AFIX 7 H3A 2 0.566687 0.797172 0.528069 11.00000 31.00000 H3B 2 0.421170 0.809527 0.547100 11.00000 31.00000 H3C 2 0.443993 0.699005 0.521300 11.00000 31.00000 AFIX 0 C5 1 0.954874 0.390397 0.594669 11.00000 0.03868 0.04725 = 0.11189 0.00371 -0.00316 -0.01278 PART 1 AFIX 3 H5A 2 0.907074 0.395417 0.616389 10.67000 -1.20000 PART 0 PART 2 H5B 2 0.958124 0.455417 0.612199 10.33000 -1.20000 AFIX 0 PART 0 C7 1 0.754425 0.534276 0.578218 11.00000 0.02765 0.03231 = 0.05222 -0.00248 0.00280 -0.01314 C8 1 0.664157 0.582483 0.554460 11.00000 0.03323 0.02828 = 0.04105 -0.01139 0.00007 -0.00850 C9 1 0.679915 0.546393 0.522264 11.00000 0.03947 0.06717 = 0.04618 -0.02964 -0.00201 -0.01666 AFIX 43 H9 2 0.619267 0.579065 0.505979 11.00000 -1.20000 AFIX 0 C10 1 0.783004 0.463377 0.513680 11.00000 0.05056 0.07983 = 0.07765 -0.03881 0.00809 -0.00416 AFIX 43 H10 2 0.794465 0.440199 0.491408 11.00000 -1.20000 AFIX 0 C11 1 0.868484 0.414323 0.536796 11.00000 0.03657 0.05930 = 0.09134 -0.03111 0.00826 -0.00954 AFIX 43 H11 2 0.937684 0.355716 0.530337 11.00000 -1.20000 AFIX 0 C12 1 0.858478 0.446284 0.569017 11.00000 0.03112 0.03392 = 0.08852 -0.01380 0.00842 -0.01163 PART 1 C4A 1 0.986597 0.253525 0.587639 10.67000 0.06296 0.05041 = 0.18140 -0.00335 -0.01221 -0.00951 AFIX 7 H4AA 2 0.899157 0.208696 0.583378 10.67000 41.00000 H4AB 2 1.047361 0.247766 0.568410 10.67000 41.00000 H4AC 2 1.033762 0.216114 0.606530 10.67000 41.00000 AFIX 0 C6A 1 1.092207 0.459736 0.597166 10.67000 0.04349 0.05698 = 0.12658 0.00843 -0.00996 -0.01690 AFIX 7 H6AA 2 1.144826 0.429379 0.616137 10.67000 -1.50000 H6AB 2 1.146859 0.445454 0.577236 10.67000 -1.50000 H6AC 2 1.074197 0.549327 0.599665 10.67000 -1.50000 AFIX 0 PART 0 PART 2 C4B 1 0.897844 0.276756 0.612330 10.33000 0.03699 0.06881 = 0.15067 0.03155 -0.00847 -0.01646 AFIX 3 H4BA 2 0.967374 0.248266 0.628260 10.33000 -1.50000 H4BB 2 0.810664 0.297346 0.623680 10.33000 -1.50000 H4BC 2 0.880304 0.210416 0.596350 10.33000 -1.50000 AFIX 0 C6B 1 1.105935 0.379839 0.583197 10.33000 0.03969 0.05644 = 0.15346 0.01067 0.00504 -0.01355 AFIX 3 H6BA 2 1.132115 0.457759 0.572237 10.33000 -1.50000 H6BB 2 1.167575 0.366019 0.601997 10.33000 -1.50000 H6BC 2 1.115125 0.310109 0.567828 10.33000 -1.50000 AFIX 0 PART 0 N2 4 0.250000 0.750000 0.734680 10.50000 0.08020 0.07318 = 0.05999 0.00000 0.00000 0.00432 C13 1 0.282952 0.857679 0.711038 11.00000 0.13171 0.10098 = 0.10395 0.02427 0.00053 -0.01025 AFIX 3 H13A 2 0.353362 0.829119 0.694948 11.00000 -1.20000 H13B 2 0.196522 0.877639 0.698798 11.00000 -1.20000 AFIX 0 C14 1 0.281592 0.982934 0.726096 11.00000 0.17420 0.10952 = 0.18267 0.00053 -0.03275 0.00281 AFIX 3 H14A 2 0.303512 0.976074 0.749446 11.00000 -1.50000 H14B 2 0.189392 1.021424 0.723416 11.00000 -1.50000 H14C 2 0.352322 1.034664 0.715296 11.00000 -1.50000 AFIX 0 PART 2 C15A 1 0.096805 0.787351 0.739250 10.50000 0.08847 0.07309 = 0.05995 0.01574 -0.00446 0.00610 AFIX 3 H15A 2 0.094775 0.872091 0.748900 10.50000 -1.20000 H15B 2 0.052205 0.792311 0.717440 10.50000 -1.20000 AFIX 0 PART 0 PART -1 C15B 1 0.174602 0.732976 0.767255 10.50000 0.07574 0.05605 = 0.06536 0.00921 0.00150 0.03462 AFIX 3 H15C 2 0.212282 0.657496 0.778085 10.50000 -1.20000 H15D 2 0.194512 0.807166 0.780945 10.50000 -1.20000 AFIX 0 C16 1 0.019429 0.719680 0.764439 11.00000 0.07731 0.16311 = 0.09470 0.05346 -0.00452 0.02536 AFIX 3 H16A 2 -0.019511 0.793730 0.753729 10.50000 -1.50000 H16B 2 -0.001321 0.645540 0.751269 10.50000 -1.50000 H16C 2 -0.022331 0.710360 0.786199 10.50000 -1.50000 PART 0 PART 2 H16E 2 -0.076681 0.750900 0.765609 10.50000 -1.50000 H16F 2 0.018369 0.630790 0.758810 10.50000 -1.50000 H16D 2 0.065139 0.730980 0.785689 10.50000 -1.50000 AFIX 0 HKLF 4 REM 13srv064 in Pccn #56 REM R1 = 0.0927 for 4705 Fo > 4sig(Fo) and 0.1054 for all 5565 data REM 234 parameters refined using 194 restraints END WGHT 0.0000 92.6278 REM Highest difference peak 2.367, deepest hole -3.687, 1-sigma level 0.199 Q1 1 0.7014 0.3749 0.6500 11.00000 0.05 2.37 Q2 1 0.7976 0.3210 0.6541 11.00000 0.05 2.29 Q3 1 0.7861 0.6164 0.6382 11.00000 0.05 2.28 Q4 1 0.7120 0.5624 0.6430 11.00000 0.05 2.20 Q5 1 0.6594 0.6401 0.6496 11.00000 0.05 2.07 Q6 1 0.7005 0.6724 0.6498 11.00000 0.05 2.05 Q7 1 0.8431 0.5793 0.6529 11.00000 0.05 1.75 Q8 1 0.7545 0.6052 0.6595 11.00000 0.05 1.43 Q9 1 0.1847 0.8595 0.7190 11.00000 0.05 1.21 Q10 1 0.2695 0.8929 0.6830 11.00000 0.05 1.16 Q11 1 0.7208 0.6479 0.5489 11.00000 0.05 1.03 Q12 1 0.7169 0.6251 0.5539 11.00000 0.05 1.03 Q13 1 0.5953 0.7721 0.6734 11.00000 0.05 1.00 Q14 1 0.6708 0.8575 0.5495 11.00000 0.05 0.95 Q15 1 0.9880 0.4647 0.6434 11.00000 0.05 0.93 Q16 1 0.5045 0.5037 0.6494 11.00000 0.05 0.91 Q17 1 0.8656 0.4067 0.6656 11.00000 0.05 0.90 Q18 1 0.7262 0.3354 0.5440 11.00000 0.05 0.89 Q19 1 0.6432 0.5292 0.6705 11.00000 0.05 0.87 Q20 1 0.2186 0.8852 0.7323 11.00000 0.05 0.87 ; _shelx_res_checksum 25333 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W W 0.73594(6) 0.61876(6) 0.65115(2) 0.05622(19) Uani 1 1 d . U . . . Cl1 Cl 0.5463(3) 0.7662(4) 0.64511(6) 0.0526(8) Uani 1 1 d . U . . . Cl2 Cl 0.7500 0.7500 0.70434(11) 0.093(2) Uani 1 2 d S TU P . . Cl3 Cl 0.5511(4) 0.4924(5) 0.67092(10) 0.0848(14) Uani 1 1 d . U . . . Cl4 Cl 0.8833(5) 0.4737(5) 0.67796(12) 0.1003(17) Uani 1 1 d . U . . . N1 N 0.7406(9) 0.5710(8) 0.6109(2) 0.0394(17) Uani 1 1 d . U . . . C1 C 0.4251(11) 0.5909(10) 0.5804(3) 0.041(2) Uani 1 1 d . U . . . H1A H 0.3467 0.6464 0.5855 0.043(19) Uiso 1 1 d GR . . . . H1B H 0.4579 0.5507 0.6005 0.043(19) Uiso 1 1 d GR . . . . H1C H 0.3944 0.5270 0.5648 0.043(19) Uiso 1 1 d GR . . . . C2 C 0.5452(10) 0.6676(9) 0.5652(2) 0.0317(18) Uani 1 1 d . U . . . H2 H 0.5826 0.7236 0.5827 0.038 Uiso 1 1 calc R . . . . C3 C 0.4893(12) 0.7507(13) 0.5380(3) 0.048(3) Uani 1 1 d . U . . . H3A H 0.5667 0.7972 0.5281 0.05(2) Uiso 1 1 d GR . . . . H3B H 0.4212 0.8095 0.5471 0.05(2) Uiso 1 1 d GR . . . . H3C H 0.4440 0.6990 0.5213 0.05(2) Uiso 1 1 d GR . . . . C5 C 0.9549(13) 0.3904(12) 0.5947(4) 0.066(3) Uani 1 1 d D U . . . H5A H 0.9071 0.3954 0.6164 0.079 Uiso 0.67 1 d R . . A 1 H5B H 0.9581 0.4554 0.6122 0.079 Uiso 0.33 1 d R . . B 2 C7 C 0.7544(11) 0.5343(9) 0.5782(3) 0.0374(18) Uani 1 1 d . U . . . C8 C 0.6642(10) 0.5825(9) 0.5545(3) 0.0342(19) Uani 1 1 d . U . . . C9 C 0.6799(12) 0.5464(12) 0.5223(3) 0.051(3) Uani 1 1 d . U . . . H9 H 0.6193 0.5791 0.5060 0.061 Uiso 1 1 calc R . . . . C10 C 0.7830(14) 0.4634(14) 0.5137(4) 0.069(3) Uani 1 1 d . U . . . H10 H 0.7945 0.4402 0.4914 0.083 Uiso 1 1 calc R . . . . C11 C 0.8685(13) 0.4143(13) 0.5368(4) 0.062(3) Uani 1 1 d . U . . . H11 H 0.9377 0.3557 0.5303 0.075 Uiso 1 1 calc R . . . . C12 C 0.8585(12) 0.4463(11) 0.5690(4) 0.051(2) Uani 1 1 d . U . . . C4A C 0.987(3) 0.2535(19) 0.5876(8) 0.098(8) Uani 0.67 1 d D U . C 1 H4AA H 0.8992 0.2087 0.5834 0.09(5) Uiso 0.67 1 d GR . . C 1 H4AB H 1.0474 0.2478 0.5684 0.09(5) Uiso 0.67 1 d GR . . C 1 H4AC H 1.0338 0.2161 0.6065 0.09(5) Uiso 0.67 1 d GR . . C 1 C6A C 1.092(2) 0.460(2) 0.5972(7) 0.076(7) Uani 0.67 1 d D U . C 1 H6AA H 1.1448 0.4294 0.6161 0.114 Uiso 0.67 1 d GR . . C 1 H6AB H 1.1469 0.4455 0.5772 0.114 Uiso 0.67 1 d GR . . C 1 H6AC H 1.0742 0.5493 0.5997 0.114 Uiso 0.67 1 d GR . . C 1 C4B C 0.898(4) 0.277(4) 0.6123(13) 0.085(14) Uani 0.33 1 d D U . C 2 H4BA H 0.9674 0.2483 0.6283 0.128 Uiso 0.33 1 d R . . C 2 H4BB H 0.8107 0.2973 0.6237 0.128 Uiso 0.33 1 d R . . C 2 H4BC H 0.8803 0.2104 0.5963 0.128 Uiso 0.33 1 d R . . C 2 C6B C 1.106(3) 0.380(5) 0.5832(14) 0.083(11) Uani 0.33 1 d D U . C 2 H6BA H 1.1321 0.4578 0.5722 0.125 Uiso 0.33 1 d R . . C 2 H6BB H 1.1676 0.3660 0.6020 0.125 Uiso 0.33 1 d R . . C 2 H6BC H 1.1151 0.3101 0.5678 0.125 Uiso 0.33 1 d R . . C 2 N2 N 0.2500 0.7500 0.7347(4) 0.071(4) Uani 1 2 d DS TU P . . C13 C 0.283(3) 0.8577(16) 0.7110(5) 0.112(6) Uani 1 1 d D U . . . H13A H 0.3534 0.8291 0.6949 0.135 Uiso 1 1 d R . . . . H13B H 0.1965 0.8776 0.6988 0.135 Uiso 1 1 d R . . . . C14 C 0.282(3) 0.983(2) 0.7261(6) 0.155(10) Uani 1 1 d D U . . . H14A H 0.3035 0.9761 0.7494 0.233 Uiso 1 1 d R . . . . H14B H 0.1894 1.0214 0.7234 0.233 Uiso 1 1 d R . . . . H14C H 0.3523 1.0347 0.7153 0.233 Uiso 1 1 d R . . . . C15A C 0.097(2) 0.787(3) 0.7393(7) 0.074(8) Uani 0.5 1 d D U . D 2 H15A H 0.0948 0.8721 0.7489 0.089 Uiso 0.5 1 d R . . D 2 H15B H 0.0522 0.7923 0.7174 0.089 Uiso 0.5 1 d R . . D 2 C15B C 0.175(2) 0.733(3) 0.7673(5) 0.066(6) Uani 0.5 1 d D U . D -1 H15C H 0.2123 0.6575 0.7781 0.079 Uiso 0.5 1 d R . . D -1 H15D H 0.1945 0.8072 0.7809 0.079 Uiso 0.5 1 d R . . D -1 C16 C 0.0194(19) 0.720(2) 0.7644(4) 0.112(8) Uani 1 1 d D U . D -1 H16A H -0.0195 0.7937 0.7537 0.168 Uiso 0.5 1 d R . . D -1 H16B H -0.0013 0.6455 0.7513 0.168 Uiso 0.5 1 d R . . D -1 H16C H -0.0223 0.7104 0.7862 0.168 Uiso 0.5 1 d R . . D -1 H16E H -0.0767 0.7509 0.7656 0.168 Uiso 0.5 1 d R . . D 2 H16F H 0.0184 0.6308 0.7588 0.168 Uiso 0.5 1 d R . . D 2 H16D H 0.0651 0.7310 0.7857 0.168 Uiso 0.5 1 d R . . D 2 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 0.0477(3) 0.0827(4) 0.0383(2) 0.0215(2) -0.0012(2) -0.0199(3) Cl1 0.0393(13) 0.078(2) 0.0401(13) -0.0159(15) 0.0085(11) -0.0146(14) Cl2 0.074(3) 0.173(6) 0.0312(19) 0.000 0.000 -0.044(4) Cl3 0.071(2) 0.116(3) 0.068(2) 0.044(2) 0.0076(19) -0.033(2) Cl4 0.081(3) 0.131(4) 0.090(3) 0.078(3) -0.010(2) -0.014(3) N1 0.029(4) 0.039(4) 0.051(3) 0.012(3) 0.003(3) -0.013(3) C1 0.029(4) 0.038(5) 0.056(6) 0.000(4) 0.001(4) -0.004(4) C2 0.032(4) 0.030(4) 0.033(4) -0.006(3) -0.004(3) -0.007(3) C3 0.044(6) 0.048(5) 0.053(5) 0.006(5) -0.011(5) -0.004(5) C5 0.039(5) 0.047(6) 0.112(8) 0.004(6) -0.003(5) -0.013(4) C7 0.028(4) 0.032(4) 0.052(4) -0.002(3) 0.003(3) -0.013(3) C8 0.033(4) 0.028(4) 0.041(4) -0.011(3) 0.000(3) -0.009(3) C9 0.039(5) 0.067(7) 0.046(5) -0.030(4) -0.002(4) -0.017(4) C10 0.051(6) 0.080(8) 0.078(6) -0.039(5) 0.008(5) -0.004(6) C11 0.037(5) 0.059(7) 0.091(6) -0.031(5) 0.008(4) -0.010(5) C12 0.031(4) 0.034(5) 0.089(6) -0.014(4) 0.008(4) -0.012(3) C4A 0.063(12) 0.050(7) 0.18(2) -0.003(8) -0.012(14) -0.010(7) C6A 0.043(7) 0.057(10) 0.127(19) 0.008(11) -0.010(9) -0.017(7) C4B 0.037(15) 0.069(17) 0.15(3) 0.03(2) -0.008(15) -0.016(12) C6B 0.040(8) 0.06(2) 0.15(3) 0.01(2) 0.005(9) -0.014(9) N2 0.080(9) 0.073(9) 0.060(8) 0.000 0.000 0.004(8) C13 0.132(14) 0.101(10) 0.104(11) 0.024(8) 0.001(10) -0.010(10) C14 0.17(3) 0.110(11) 0.18(2) 0.001(10) -0.03(2) 0.003(12) C15A 0.088(11) 0.073(18) 0.060(15) 0.016(13) -0.004(8) 0.006(10) C15B 0.076(10) 0.056(15) 0.065(10) 0.009(9) 0.001(7) 0.035(10) C16 0.077(9) 0.16(2) 0.095(12) 0.053(13) -0.005(7) 0.025(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' N N 0.0061 0.0033 '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 0.0300 0.00 0.00 1.00 0.0300 1.00 0.00 0.00 0.1700 -1.00 0.00 0.00 0.1800 0.00 1.00 5.00 0.1200 0.00 -1.00 5.00 0.1200 0.00 1.00 -5.00 0.1200 0.00 -1.00 -5.00 0.1200 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 Cl1 W W 54.64(8) . 2_665 Cl1 W W 54.15(9) 2_665 2_665 Cl1 W Cl1 107.54(9) . 2_665 Cl1 W Cl2 76.47(8) 2_665 . Cl1 W Cl2 76.72(7) . . Cl2 W W 56.98(5) . 2_665 Cl3 W W 129.78(14) . 2_665 Cl3 W Cl1 81.25(15) . . Cl3 W Cl1 164.41(12) . 2_665 Cl3 W Cl2 93.60(13) . . Cl4 W W 126.64(14) . 2_665 Cl4 W Cl1 157.37(14) . . Cl4 W Cl1 82.49(14) . 2_665 Cl4 W Cl2 86.39(16) . . Cl4 W Cl3 84.94(16) . . N1 W W 107.0(3) . 2_665 N1 W Cl1 91.8(3) . 2_665 N1 W Cl1 96.7(3) . . N1 W Cl2 163.7(3) . . N1 W Cl3 100.1(3) . . N1 W Cl4 103.4(3) . . W Cl1 W 71.21(8) . 2_665 W Cl2 W 66.03(11) 2_665 . C7 N1 W 176.0(8) . . C3 C2 C1 110.2(9) . . C3 C2 C8 113.8(9) . . C8 C2 C1 110.7(8) . . C12 C5 C4A 111.7(16) . . C12 C5 C6B 113(3) . . C6A C5 C12 112.4(14) . . C6A C5 C4A 108.2(16) . . C4B C5 C12 115(2) . . C4B C5 C6B 115(3) . . N1 C7 C8 120.1(10) . . N1 C7 C12 120.3(11) . . C8 C7 C12 119.6(10) . . C7 C8 C2 118.9(9) . . C9 C8 C2 121.6(10) . . C9 C8 C7 119.4(10) . . C10 C9 C8 120.2(13) . . C11 C10 C9 120.4(13) . . C10 C11 C12 122.2(13) . . C7 C12 C5 120.3(12) . . C11 C12 C5 121.6(12) . . C11 C12 C7 118.1(13) . . C13 N2 C13 102.1(17) . 2_565 C15A N2 C13 94.4(16) . 2_565 C15A N2 C13 94.4(16) 2_565 . C15A N2 C13 94.4(13) 2_565 2_565 C15A N2 C13 94.4(13) . . C15A N2 C15A 166(2) . 2_565 C15B N2 C13 137.3(14) . . C15B N2 C13 111.2(14) . 2_565 C14 C13 N2 114.7(17) . . C16 C15A N2 116.2(16) . . C16 C15B N2 114.4(15) . . H16E C16 C15A 109.9 . . H16E C16 H16D 109.5 . . H16F C16 C15A 108.8 . . H16F C16 H16E 109.5 . . H16F C16 H16D 109.4 . . H16D C16 C15A 109.7 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 W W 2.8251(13) 2_665 W Cl1 2.434(3) 2_665 W Cl1 2.419(4) . W Cl2 2.592(4) . W Cl3 2.369(4) . W Cl4 2.368(4) . W N1 1.724(9) . Cl1 W 2.434(3) 2_665 Cl2 W 2.592(4) 2_665 N1 C7 1.398(13) . C1 C2 1.544(14) . C2 C3 1.520(14) . C2 C8 1.523(14) . C5 C12 1.52(2) . C5 C4A 1.525(19) . C5 C6A 1.513(17) . C5 C4B 1.52(2) . C5 C6B 1.52(2) . C7 C8 1.399(15) . C7 C12 1.422(16) . C8 C9 1.380(14) . C9 C10 1.374(18) . C10 C11 1.36(2) . C11 C12 1.364(19) . N2 C13 1.538(15) 2_565 N2 C13 1.538(15) . N2 C15A 1.531(19) . N2 C15A 1.531(19) 2_565 N2 C15B 1.525(18) . C13 C14 1.476(17) . C15A C16 1.46(3) . C15B C16 1.50(3) . C16 H16E 0.9798 . C16 H16F 0.9798 . C16 H16D 0.9800 .