#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:47:08 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515789.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_4515789 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 'C15 H26 Al Cl4 N W' _chemical_formula_sum 'C15 H26 Al Cl4 N W' _chemical_formula_weight 573.00 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_date 2016-12-25 _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 96.616(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.0824(5) _cell_length_b 16.3429(10) _cell_length_c 13.3029(7) _cell_measurement_reflns_used 9630 _cell_measurement_temperature 120 _cell_measurement_theta_max 34.93 _cell_measurement_theta_min 2.38 _cell_volume 2177.4(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 1.000 _diffrn_measured_fraction_theta_max 0.967 _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 0.0224 _diffrn_reflns_av_unetI/netI 0.0165 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.967 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 50007 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 32.500 _diffrn_reflns_theta_max 34.982 _diffrn_reflns_theta_min 1.982 _diffrn_source 'sealed X-ray tube' _diffrn_source_target Mo _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.833 _exptl_absorpt_correction_T_max 0.4370 _exptl_absorpt_correction_T_min 0.3573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2009/1 (Bruker,2010) was used for absorption correction. wR2(int) was 0.0618 before and 0.0375 after correction. The Ratio of minimum to maximum transmission is 0.8176. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1112 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _refine_diff_density_max 1.505 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.083 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 212 _refine_ls_number_reflns 9270 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0161 _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^)+(0.0132P)^2^+1.1294P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0351 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8368 _reflns_number_total 9270 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b02201_si_002.cif _cod_data_source_block 7 _cod_database_code 4515789 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Others Uiso(H14A)=Uiso(H14B)=Uiso(H14C)=FVAR(1) Uiso(H15A)=Uiso(H15B)=Uiso(H15C)=FVAR(2) Uiso(H3AA)=Uiso(H3AB)=Uiso(H3AC)=Uiso(H3BD)=Uiso(H3BE)=Uiso(H3BF)=FVAR(3) Uiso(H2A)=Uiso(H2B)=Uiso(H2C)=FVAR(4) Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(5) Uiso(H12A)=Uiso(H12B)=Uiso(H12C)=FVAR(6) Uiso(H11A)=Uiso(H11B)=Uiso(H11C)=FVAR(7) Fixed Sof: H3AA(0.67) H3AB(0.67) H3AC(0.67) H3BD(0.33) H3BE(0.33) H3BF(0.33) 3.a Riding coordinates: C3(H3AA,H3AB,H3AC,H3BD,H3BE,H3BF), C6(H6), C7(H7), C8(H8), C10(H10), C13(H13) 3.b Rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C) ; _shelx_res_file ; 12srv174.res created by SHELXL-2014/7 TITL 12srv174 in P21/c #14 REM reset to P21/c #14 CELL 0.71073 10.0824 16.3429 13.3029 90 96.616 90 ZERR 4 0.0005 0.001 0.0007 0 0.006 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Al Cl N W UNIT 60 104 4 16 4 4 L.S. 7 PLAN 7 TEMP -153.15 BOND fmap 2 acta 65 REM REM REM WGHT 0.013200 1.129400 FVAR 0.20703 0.03772 0.03857 0.04591 0.06213 0.05054 0.03441 FVAR 0.03839 W 6 0.693906 0.469366 0.754343 11.00000 0.01652 0.01684 = 0.01262 0.00038 0.00271 0.00025 CL1 4 0.663806 0.374029 0.911364 11.00000 0.02692 0.02390 = 0.01652 0.00267 0.00072 -0.00580 CL2 4 0.983546 0.381228 1.045565 11.00000 0.02967 0.06177 = 0.03668 0.00350 -0.00671 0.00289 CL3 4 0.724185 0.503890 1.117663 11.00000 0.07271 0.02450 = 0.02204 -0.00432 0.00438 0.00666 CL4 4 0.713290 0.291705 1.149740 11.00000 0.07929 0.02916 = 0.02566 0.00868 0.00861 -0.01048 AL 3 0.778850 0.388948 1.063337 11.00000 0.03326 0.01945 = 0.01544 0.00136 0.00039 -0.00115 N 5 0.715365 0.520391 0.643923 11.00000 0.01814 0.01691 = 0.01554 -0.00097 0.00309 0.00065 C1 1 0.527753 0.401158 0.695777 11.00000 0.01985 0.02785 = 0.02014 0.00002 0.00040 -0.00358 AFIX 7 H1A 2 0.550123 0.342768 0.698736 11.00000 61.00000 H1B 2 0.501322 0.417089 0.625287 11.00000 61.00000 H1C 2 0.453763 0.411558 0.735747 11.00000 61.00000 AFIX 0 C2 1 0.885279 0.418109 0.769397 11.00000 0.01919 0.03698 = 0.02401 0.00586 0.00324 0.00471 AFIX 7 H2A 2 0.933679 0.434770 0.834286 11.00000 51.00000 H2B 2 0.933568 0.437228 0.714026 11.00000 51.00000 H2C 2 0.878229 0.358289 0.766919 11.00000 51.00000 AFIX 0 C3 1 0.656600 0.568214 0.846451 11.00000 0.03979 0.02349 = 0.01870 -0.00414 0.00937 0.00089 PART 1 AFIX 3 H3AA 2 0.581790 0.554944 0.884541 10.67000 41.00000 H3AB 2 0.634120 0.616614 0.804341 10.67000 41.00000 H3AC 2 0.736360 0.579584 0.893821 10.67000 41.00000 PART 0 PART 2 H3BD 2 0.670190 0.556604 0.909061 10.33000 41.00000 H3BE 2 0.718110 0.611734 0.831201 10.33000 41.00000 H3BF 2 0.564530 0.585344 0.825041 10.33000 41.00000 AFIX 0 PART 0 C4 1 0.745796 0.551357 0.551579 11.00000 0.01533 0.01787 = 0.01344 0.00079 0.00149 0.00037 C5 1 0.754220 0.637086 0.539529 11.00000 0.01622 0.01733 = 0.01744 0.00100 0.00230 0.00025 C6 1 0.788396 0.666313 0.447667 11.00000 0.02168 0.01938 = 0.02045 0.00464 0.00331 -0.00011 AFIX 3 H6 2 0.793776 0.723643 0.436957 11.00000 -1.20000 AFIX 0 C7 1 0.814755 0.612634 0.371508 11.00000 0.02309 0.02617 = 0.01716 0.00554 0.00452 0.00092 AFIX 3 H7 2 0.838975 0.633614 0.309578 11.00000 -1.20000 AFIX 0 C8 1 0.806099 0.528964 0.384869 11.00000 0.02300 0.02374 = 0.01415 -0.00017 0.00309 0.00278 AFIX 3 H8 2 0.825199 0.493314 0.332009 11.00000 -1.20000 AFIX 0 C9 1 0.769857 0.495788 0.474470 11.00000 0.01682 0.01876 = 0.01469 -0.00042 0.00016 0.00137 C10 1 0.732255 0.693308 0.626421 11.00000 0.02326 0.01638 = 0.02321 -0.00135 0.00600 0.00116 AFIX 3 H10 2 0.661195 0.668478 0.663291 11.00000 -1.20000 AFIX 0 C11 1 0.685913 0.779078 0.592425 11.00000 0.03664 0.01932 = 0.03707 0.00122 0.01120 0.00526 AFIX 7 H11A 2 0.758753 0.807718 0.564495 11.00000 81.00000 H11B 2 0.660233 0.809628 0.650555 11.00000 81.00000 H11C 2 0.609023 0.774808 0.540465 11.00000 81.00000 AFIX 0 C12 1 0.860549 0.698122 0.700408 11.00000 0.03144 0.02854 = 0.02664 -0.01068 0.00131 0.00028 AFIX 7 H12A 2 0.891377 0.642652 0.718900 11.00000 71.00000 H12B 2 0.842549 0.727794 0.761407 11.00000 71.00000 H12C 2 0.929629 0.726950 0.668178 11.00000 71.00000 AFIX 0 C13 1 0.750586 0.404283 0.483673 11.00000 0.02167 0.01827 = 0.01775 -0.00115 0.00243 0.00214 AFIX 3 H13 2 0.749676 0.390933 0.556942 11.00000 -1.20000 AFIX 0 C14 1 0.615645 0.379538 0.427647 11.00000 0.02101 0.02543 = 0.03668 -0.00259 0.00013 -0.00328 AFIX 7 H14A 2 0.544505 0.410908 0.454147 11.00000 21.00000 H14B 2 0.600805 0.320948 0.437537 11.00000 21.00000 H14C 2 0.615035 0.390878 0.355237 11.00000 21.00000 AFIX 0 C15 1 0.862812 0.355532 0.444498 11.00000 0.02580 0.02507 = 0.03566 -0.00210 0.00502 0.00695 AFIX 7 H15A 2 0.858759 0.362510 0.371018 11.00000 31.00000 H15B 2 0.852815 0.297453 0.460332 11.00000 31.00000 H15C 2 0.949032 0.375354 0.476886 11.00000 31.00000 AFIX 0 HKLF 4 REM 12srv174 in P21/c #14 REM R1 = 0.0161 for 8368 Fo > 4sig(Fo) and 0.0198 for all 9270 data REM 212 parameters refined using 0 restraints END WGHT 0.0132 1.1292 REM Highest difference peak 1.505, deepest hole -0.705, 1-sigma level 0.083 Q1 1 0.6949 0.5918 0.7575 11.00000 0.05 1.51 Q2 1 0.9190 0.4703 0.7392 11.00000 0.05 1.29 Q3 1 0.9622 0.4197 1.0417 11.00000 0.05 0.53 Q4 1 0.7649 0.4511 0.4783 11.00000 0.05 0.51 Q5 1 0.7425 0.4675 0.7928 11.00000 0.05 0.47 Q6 1 0.7505 0.6502 0.4864 11.00000 0.05 0.47 Q7 1 0.7414 0.5236 0.5069 11.00000 0.05 0.47 ; _shelx_res_checksum 4644 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W W 0.69391(2) 0.46937(2) 0.75434(2) 0.01524(2) Uani 1 1 d . . . . Cl1 Cl 0.66381(4) 0.37403(2) 0.91136(2) 0.02259(6) Uani 1 1 d . . . . Cl2 Cl 0.98355(5) 0.38123(4) 1.04557(4) 0.04352(11) Uani 1 1 d . . . . Cl3 Cl 0.72418(6) 0.50389(3) 1.11766(3) 0.03984(10) Uani 1 1 d . . . . Cl4 Cl 0.71329(6) 0.29170(3) 1.14974(3) 0.04450(12) Uani 1 1 d . . . . Al Al 0.77885(5) 0.38895(3) 1.06334(3) 0.02290(9) Uani 1 1 d . . . . N N 0.71536(11) 0.52039(7) 0.64392(8) 0.01677(19) Uani 1 1 d . . . . C1 C 0.52775(14) 0.40116(9) 0.69578(11) 0.0228(3) Uani 1 1 d . . . . H1A H 0.5501 0.3428 0.6987 0.051(4) Uiso 1 1 d GR . . . H1B H 0.5013 0.4171 0.6253 0.051(4) Uiso 1 1 d GR . . . H1C H 0.4538 0.4116 0.7357 0.051(4) Uiso 1 1 d GR . . . C2 C 0.88528(14) 0.41811(11) 0.76940(12) 0.0267(3) Uani 1 1 d . . . . H2A H 0.9337 0.4348 0.8343 0.062(5) Uiso 1 1 d GR . . . H2B H 0.9336 0.4372 0.7140 0.062(5) Uiso 1 1 d GR . . . H2C H 0.8782 0.3583 0.7669 0.062(5) Uiso 1 1 d GR . . . C3 C 0.65660(17) 0.56821(9) 0.84645(11) 0.0269(3) Uani 1 1 d . . . . H3AA H 0.5818 0.5549 0.8845 0.046(5) Uiso 0.67 1 d R P A 1 H3AB H 0.6341 0.6166 0.8043 0.046(5) Uiso 0.67 1 d R P A 1 H3AC H 0.7364 0.5796 0.8938 0.046(5) Uiso 0.67 1 d R P A 1 H3BD H 0.6702 0.5566 0.9091 0.046(5) Uiso 0.33 1 d R P B 2 H3BE H 0.7181 0.6117 0.8312 0.046(5) Uiso 0.33 1 d R P B 2 H3BF H 0.5645 0.5853 0.8250 0.046(5) Uiso 0.33 1 d R P B 2 C4 C 0.74580(12) 0.55136(8) 0.55158(9) 0.0156(2) Uani 1 1 d . . . . C5 C 0.75422(13) 0.63709(8) 0.53953(10) 0.0170(2) Uani 1 1 d . . . . C6 C 0.78840(14) 0.66631(8) 0.44767(10) 0.0204(2) Uani 1 1 d . . . . H6 H 0.7938 0.7236 0.4370 0.025 Uiso 1 1 d R . . . C7 C 0.81476(14) 0.61263(9) 0.37151(10) 0.0220(3) Uani 1 1 d . . . . H7 H 0.8390 0.6336 0.3096 0.026 Uiso 1 1 d R . . . C8 C 0.80610(14) 0.52896(9) 0.38487(10) 0.0202(2) Uani 1 1 d . . . . H8 H 0.8252 0.4933 0.3320 0.024 Uiso 1 1 d R . . . C9 C 0.76986(13) 0.49579(8) 0.47447(9) 0.0169(2) Uani 1 1 d . . . . C10 C 0.73226(14) 0.69331(8) 0.62642(11) 0.0207(2) Uani 1 1 d . . . . H10 H 0.6612 0.6685 0.6633 0.025 Uiso 1 1 d R . . . C11 C 0.68591(18) 0.77908(9) 0.59243(13) 0.0305(3) Uani 1 1 d . . . . H11A H 0.7588 0.8077 0.5645 0.038(3) Uiso 1 1 d GR . . . H11B H 0.6602 0.8096 0.6506 0.038(3) Uiso 1 1 d GR . . . H11C H 0.6090 0.7748 0.5405 0.038(3) Uiso 1 1 d GR . . . C12 C 0.86055(17) 0.69812(10) 0.70041(12) 0.0290(3) Uani 1 1 d . . . . H12A H 0.8914 0.6427 0.7189 0.034(3) Uiso 1 1 d GR . . . H12B H 0.8425 0.7278 0.7614 0.034(3) Uiso 1 1 d GR . . . H12C H 0.9296 0.7270 0.6682 0.034(3) Uiso 1 1 d GR . . . C13 C 0.75059(13) 0.40428(8) 0.48367(10) 0.0192(2) Uani 1 1 d . . . . H13 H 0.7497 0.3909 0.5569 0.023 Uiso 1 1 d R . . . C14 C 0.61564(15) 0.37954(10) 0.42765(13) 0.0280(3) Uani 1 1 d . . . . H14A H 0.5445 0.4109 0.4541 0.038(3) Uiso 1 1 d GR . . . H14B H 0.6008 0.3209 0.4375 0.038(3) Uiso 1 1 d GR . . . H14C H 0.6150 0.3909 0.3552 0.038(3) Uiso 1 1 d GR . . . C15 C 0.86281(16) 0.35553(10) 0.44450(13) 0.0287(3) Uani 1 1 d . . . . H15A H 0.8588 0.3625 0.3710 0.039(3) Uiso 1 1 d GR . . . H15B H 0.8528 0.2975 0.4603 0.039(3) Uiso 1 1 d GR . . . H15C H 0.9490 0.3754 0.4769 0.039(3) 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 W 0.01652(2) 0.01684(2) 0.01262(2) 0.00038(2) 0.00271(2) 0.00025(2) Cl1 0.02692(15) 0.02390(15) 0.01652(13) 0.00267(11) 0.00072(11) -0.00580(12) Cl2 0.0297(2) 0.0618(3) 0.0367(2) 0.0035(2) -0.00671(17) 0.00289(19) Cl3 0.0727(3) 0.02450(17) 0.02204(17) -0.00432(14) 0.00438(18) 0.00666(19) Cl4 0.0793(4) 0.0292(2) 0.02566(19) 0.00868(15) 0.0086(2) -0.0105(2) Al 0.0333(2) 0.01945(19) 0.01544(18) 0.00136(15) 0.00039(16) -0.00115(17) N 0.0181(5) 0.0169(5) 0.0155(5) -0.0010(4) 0.0031(4) 0.0006(4) C1 0.0198(6) 0.0279(7) 0.0201(6) 0.0000(5) 0.0004(5) -0.0036(5) C2 0.0192(6) 0.0370(8) 0.0240(6) 0.0059(6) 0.0032(5) 0.0047(6) C3 0.0398(8) 0.0235(7) 0.0187(6) -0.0041(5) 0.0094(6) 0.0009(6) C4 0.0153(5) 0.0179(5) 0.0134(5) 0.0008(4) 0.0015(4) 0.0004(4) C5 0.0162(5) 0.0173(5) 0.0174(5) 0.0010(4) 0.0023(4) 0.0002(4) C6 0.0217(6) 0.0194(6) 0.0205(6) 0.0046(5) 0.0033(5) -0.0001(5) C7 0.0231(6) 0.0262(6) 0.0172(6) 0.0055(5) 0.0045(5) 0.0009(5) C8 0.0230(6) 0.0237(6) 0.0142(5) -0.0002(5) 0.0031(4) 0.0028(5) C9 0.0168(5) 0.0188(5) 0.0147(5) -0.0004(4) 0.0002(4) 0.0014(4) C10 0.0233(6) 0.0164(5) 0.0232(6) -0.0014(5) 0.0060(5) 0.0012(5) C11 0.0366(8) 0.0193(6) 0.0371(8) 0.0012(6) 0.0112(7) 0.0053(6) C12 0.0314(8) 0.0285(7) 0.0266(7) -0.0107(6) 0.0013(6) 0.0003(6) C13 0.0217(6) 0.0183(5) 0.0177(5) -0.0012(4) 0.0024(4) 0.0021(5) C14 0.0210(6) 0.0254(7) 0.0367(8) -0.0026(6) 0.0001(6) -0.0033(5) C15 0.0258(7) 0.0251(7) 0.0357(8) -0.0021(6) 0.0050(6) 0.0069(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N W Cl1 172.93(4) N W C1 96.57(5) N W C2 94.03(6) N W C3 100.05(6) C1 W Cl1 79.65(4) C1 W C2 120.91(6) C1 W C3 116.18(6) C2 W Cl1 82.95(4) C3 W Cl1 87.00(4) C3 W C2 118.70(7) Al Cl1 W 123.807(18) Cl2 Al Cl1 107.83(3) Cl2 Al Cl3 112.94(3) Cl2 Al Cl4 112.83(3) Cl3 Al Cl1 106.23(3) Cl3 Al Cl4 111.92(3) Cl4 Al Cl1 104.42(3) C4 N W 170.94(10) N C4 C5 118.78(11) N C4 C9 118.69(11) C9 C4 C5 122.51(12) C4 C5 C10 119.95(11) C6 C5 C4 117.63(12) C6 C5 C10 122.36(12) C7 C6 C5 120.75(12) C8 C7 C6 120.70(12) C7 C8 C9 121.36(13) C4 C9 C13 122.82(11) C8 C9 C4 117.02(12) C8 C9 C13 120.07(12) C5 C10 C11 113.41(12) C5 C10 C12 109.54(11) C11 C10 C12 110.42(13) C9 C13 C14 109.70(11) C9 C13 C15 112.41(12) C15 C13 C14 110.44(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance W Cl1 2.6512(3) W N 1.7243(11) W C1 2.0869(14) W C2 2.0918(14) W C3 2.0878(14) Cl1 Al 2.2253(6) Cl2 Al 2.1080(7) Cl3 Al 2.1087(6) Cl4 Al 2.1116(6) N C4 1.3951(16) C4 C5 1.4139(18) C4 C9 1.4118(18) C5 C6 1.3919(18) C5 C10 1.5128(19) C6 C7 1.389(2) C7 C8 1.383(2) C8 C9 1.3959(18) C9 C13 1.5148(19) C10 C11 1.529(2) C10 C12 1.535(2) C13 C14 1.529(2) C13 C15 1.524(2)