#------------------------------------------------------------------------------ #$Date: 2021-03-13 07:57:55 +0200 (Sat, 13 Mar 2021) $ #$Revision: 263025 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022344.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022344 loop_ _publ_author_name 'Shaw, Thomas E.' 'Sattelberger, Alfred P.' 'Jurca, Titel' _publ_section_title ; A 35-year-old mystery solved: a facile synthetic route and structural confirmation of tetrachlorobis(diethyl ether)tungsten(IV) ; _journal_coeditor_code YP3213 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229621002412 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac '[W Cl4 (C4 H10 O)2]' _chemical_formula_moiety 'C8 H20 Cl4 O2 W' _chemical_formula_sum 'C8 H20 Cl4 O2 W' _chemical_formula_weight 473.89 _chemical_name_systematic ; trans-Tetrachloridobis(diethyl ether-\kO)tungsten(IV) ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _cell_angle_alpha 90 _cell_angle_beta 106.339(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.5962(3) _cell_length_b 11.4871(4) _cell_length_c 9.0245(4) _cell_measurement_reflns_used 2974 _cell_measurement_temperature 297.22(10) _cell_measurement_theta_max 29.6070 _cell_measurement_theta_min 2.9320 _cell_volume 755.66(5) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2019) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2019) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2019) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 297.22(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.941 _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini II' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 5730 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.667 _diffrn_reflns_theta_min 2.946 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 8.332 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_correction_T_min 0.514 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2019) ; _exptl_crystal_colour 'clear dark yellow' _exptl_crystal_density_diffrn 2.083 _exptl_crystal_description block _exptl_crystal_F_000 452 _exptl_crystal_size_max 0.258 _exptl_crystal_size_mid 0.152 _exptl_crystal_size_min 0.084 _refine_diff_density_max 0.970 _refine_diff_density_min -0.837 _refine_ls_extinction_coef 0.0042(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 2198 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0255 _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^)+(0.0201P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.0577 _reflns_number_gt 1587 _reflns_number_total 2198 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL exp_229_a.res in P2(1)/n exp_229.res created by SHELXL-2018/3 at 13:21:40 on 28-Feb-2021 REM Old TITL exp_229 in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.092, Rweak 0.001, Alpha 0.018 REM 0.560 for 87 systematic absences, Orientation as input REM Formula found by SHELXT: C16 C3 Cl1 W CELL 0.71073 7.5962 11.4871 9.0245 90 106.339 90 ZERR 2 0.0003 0.0004 0.0004 0 0.004 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl O W UNIT 16 40 8 4 2 L.S. 15 PLAN 5 CONF MORE -1 BOND $H fmap 2 acta OMIT 2 2 0 OMIT 0 5 11 OMIT -10 0 4 REM REM REM WGHT 0.020100 EXTI 0.004224 FVAR 0.77547 W1 5 0.500000 0.500000 0.500000 10.50000 0.02576 0.03029 = 0.02982 0.00141 0.01026 -0.00172 CL1 3 0.501317 0.626636 0.294588 11.00000 0.06378 0.04343 = 0.04164 0.01068 0.02364 0.00156 CL2 3 0.187546 0.462612 0.379500 11.00000 0.02967 0.06035 = 0.05692 -0.00779 0.00741 -0.00428 O1 4 0.571255 0.362736 0.379855 11.00000 0.03414 0.03095 = 0.04663 -0.00612 0.02177 -0.00521 C3 1 0.478177 0.248943 0.360301 11.00000 0.04464 0.03510 = 0.05158 -0.00762 0.01639 -0.01194 AFIX 23 H3A 2 0.431735 0.231808 0.250967 11.00000 -1.20000 H3B 2 0.374195 0.252988 0.402553 11.00000 -1.20000 AFIX 0 C1 1 0.719131 0.371883 0.302743 11.00000 0.03634 0.04382 = 0.05259 -0.00248 0.02568 0.00067 AFIX 23 H1A 2 0.809652 0.311634 0.342222 11.00000 -1.20000 H1B 2 0.779554 0.446707 0.327048 11.00000 -1.20000 AFIX 0 C2 1 0.646699 0.359704 0.131124 11.00000 0.06914 0.07250 = 0.05279 -0.00349 0.02868 0.00565 AFIX 137 H2A 2 0.741798 0.378525 0.084061 11.00000 -1.50000 H2B 2 0.545042 0.411744 0.093420 11.00000 -1.50000 H2C 2 0.606815 0.281033 0.105847 11.00000 -1.50000 AFIX 0 C4 1 0.602601 0.152136 0.438146 11.00000 0.08165 0.03480 = 0.07463 0.00435 0.02070 0.00102 AFIX 137 H4A 2 0.699018 0.142437 0.389573 11.00000 -1.50000 H4B 2 0.533600 0.081207 0.429453 11.00000 -1.50000 H4C 2 0.654820 0.170806 0.545233 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_229_a.res in P2(1)/n REM wR2 = 0.0577, GooF = S = 1.013, Restrained GooF = 1.013 for all data REM R1 = 0.0255 for 1587 Fo > 4sig(Fo) and 0.0427 for all 2198 data REM 73 parameters refined using 0 restraints END WGHT 0.0201 0.0000 REM Highest difference peak 0.970, deepest hole -0.837, 1-sigma level 0.129 Q1 1 0.3777 0.5015 0.5189 11.00000 0.05 0.97 Q2 1 0.2540 0.5003 0.3367 11.00000 0.05 0.67 Q3 1 0.3834 0.4444 0.4197 11.00000 0.05 0.63 Q4 1 0.3797 0.5016 0.3451 11.00000 0.05 0.57 Q5 1 0.6081 0.6217 0.2948 11.00000 0.05 0.50 REM The information below was added by Olex2. REM REM R1 = 0.0255 for 1587 Fo > 4sig(Fo) and 0.0427 for all 5945 data REM 73 parameters refined using n/a restraints REM Highest difference peak 0.97, deepest hole -0.84 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0427 REM R1_gt = 0.0255 REM wR_ref = 0.0577 REM GOOF = 1.013 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 5945 REM Reflections_gt = 1587 REM Parameters = 73 REM Hole = -0.84 REM Peak = 0.97 REM Flack = n/a ; _cod_data_source_file yp3213sup1.cif _cod_data_source_block I _cod_database_code 2022344 _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W W1 0.500000 0.500000 0.500000 0.02813(8) Uani d 1 . . Cl Cl1 0.50132(15) 0.62664(9) 0.29459(12) 0.0478(3) Uani d 1 . . Cl Cl2 0.18755(13) 0.46261(10) 0.37950(14) 0.0499(3) Uani d 1 . . O O1 0.5713(3) 0.36274(19) 0.3799(3) 0.0351(6) Uani d 1 . . C C3 0.4782(5) 0.2489(3) 0.3603(4) 0.0432(9) Uani d 1 . . H H3A 0.431735 0.231808 0.250967 0.052 Uiso calc 1 . . H H3B 0.374195 0.252988 0.402553 0.052 Uiso calc 1 . . C C1 0.7191(5) 0.3719(3) 0.3027(4) 0.0416(9) Uani d 1 . . H H1A 0.809652 0.311634 0.342222 0.050 Uiso calc 1 . . H H1B 0.779554 0.446707 0.327048 0.050 Uiso calc 1 . . C C2 0.6467(5) 0.3597(4) 0.1311(5) 0.0625(13) Uani d 1 . . H H2A 0.741798 0.378525 0.084061 0.094 Uiso calc 1 . . H H2B 0.545042 0.411744 0.093420 0.094 Uiso calc 1 . . H H2C 0.606815 0.281033 0.105847 0.094 Uiso calc 1 . . C C4 0.6026(5) 0.1521(3) 0.4381(5) 0.0640(13) Uani d 1 . . H H4A 0.699018 0.142437 0.389573 0.096 Uiso calc 1 . . H H4B 0.533600 0.081207 0.429453 0.096 Uiso calc 1 . . H H4C 0.654820 0.170806 0.545233 0.096 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W1 0.02576(11) 0.03029(12) 0.02982(12) -0.00172(8) 0.01026(8) 0.00141(10) Cl1 0.0638(7) 0.0434(6) 0.0416(6) 0.0016(5) 0.0236(5) 0.0107(5) Cl2 0.0297(4) 0.0603(6) 0.0569(7) -0.0043(4) 0.0074(5) -0.0078(6) O1 0.0341(13) 0.0310(13) 0.0466(16) -0.0052(10) 0.0218(12) -0.0061(12) C3 0.045(2) 0.035(2) 0.052(3) -0.0119(17) 0.016(2) -0.008(2) C1 0.036(2) 0.044(2) 0.053(3) 0.0007(16) 0.0257(19) -0.002(2) C2 0.069(3) 0.073(3) 0.053(3) 0.006(2) 0.029(3) -0.003(3) C4 0.082(3) 0.035(2) 0.075(3) 0.001(2) 0.021(3) 0.004(2) 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' 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_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 0 0 1 0 0 -1 0 0 -1 0 0 2 0 0 -2 0 0 2 0 0 -2 0 0 -3 0 0 -3 0 0 3 0 0 3 0 0 4 0 0 -4 0 0 -4 0 0 -5 0 0 -5 0 0 5 0 0 6 0 0 -6 0 0 -7 0 0 -8 0 0 -9 0 0 -10 0 0 -11 0 0 -12 0 -1 0 0 1 -1 0 1 -1 0 1 1 0 -1 -1 0 -1 1 0 -1 1 0 1 -2 0 1 -2 0 1 -2 0 -1 2 0 -1 -2 0 -1 -2 0 1 2 0 -1 -3 0 1 -3 0 1 -3 0 -1 -3 0 -1 3 0 1 3 0 -1 -3 0 1 3 0 -1 -4 0 1 4 0 -1 -4 0 1 -4 0 -1 4 0 1 4 0 -1 4 0 1 -4 0 -1 -5 0 -1 -5 0 -1 5 0 1 -5 0 1 -5 0 -1 -5 0 1 -6 0 1 -6 0 -1 -6 0 -1 6 0 1 -7 0 -1 7 0 -1 -7 0 1 -8 0 -1 -8 0 -1 8 0 1 -9 0 -1 -9 0 -1 -10 0 1 -10 0 1 -11 0 -1 -11 0 1 -12 0 -1 -12 0 2 0 0 -2 0 0 2 1 0 2 1 0 -2 1 0 -2 1 0 -2 -1 0 2 -1 0 2 -1 0 2 -2 0 -2 -2 0 2 2 0 -2 -2 0 2 -2 0 2 -2 0 -2 2 0 2 2 0 2 2 0 -2 2 0 2 3 0 2 -3 0 -2 3 0 2 3 0 2 -3 0 2 -3 0 -2 -3 0 2 3 0 2 4 0 2 -4 0 -2 4 0 2 -4 0 -2 -4 0 2 -4 0 -2 -4 0 -2 -4 0 2 4 0 -2 -5 0 2 -5 0 2 -5 0 2 -5 0 2 -6 0 -2 6 0 -2 -6 0 2 -6 0 -2 -7 0 -2 7 0 2 -7 0 2 -8 0 -2 -8 0 2 -9 0 -2 -9 0 2 -10 0 -2 -10 0 -2 -11 0 2 -11 0 2 -12 0 -2 -12 0 3 0 0 3 0 0 -3 0 0 -3 1 0 3 -1 0 -3 -1 0 3 1 0 -3 1 0 3 1 0 3 1 0 -3 1 0 3 -2 0 3 -2 0 3 2 0 -3 2 0 3 -2 0 -3 2 0 -3 -2 0 -3 -2 0 3 2 0 -3 3 0 -3 3 0 3 3 0 3 3 0 3 -3 0 -3 -3 0 3 3 0 -3 -3 0 3 -3 0 3 -3 0 3 4 0 3 -4 0 3 -4 0 -3 -4 0 3 -4 0 -3 -5 0 3 -5 0 3 -5 0 3 -6 0 3 -6 0 -3 -6 0 -3 7 0 -3 -7 0 3 -7 0 3 -8 0 -3 -8 0 3 -9 0 -3 -9 0 3 -10 0 -3 -10 0 -3 -11 0 3 -11 0 -4 0 0 4 0 0 4 0 0 -4 1 0 -4 -1 0 4 -1 0 -4 1 0 -4 -1 0 -4 1 0 4 2 0 -4 2 0 4 -2 0 4 2 0 4 2 0 4 -2 0 -4 2 0 -4 -2 0 4 -2 0 4 2 0 -4 2 0 4 -3 0 -4 3 0 -4 3 0 4 3 0 4 -3 0 4 3 0 -4 -3 0 4 -3 0 -4 -3 0 -4 4 0 -4 -4 0 4 -4 0 4 -4 0 -4 -4 0 4 -4 0 4 4 0 4 -5 0 4 -5 0 -4 -5 0 -4 -6 0 4 -6 0 4 -6 0 4 -7 0 -4 -7 0 4 -7 0 4 -8 0 -4 -8 0 4 -9 0 -4 -9 0 4 -10 0 4 -11 0 -5 0 0 5 0 0 -5 0 0 -5 0 0 5 0 0 -5 1 0 -5 -1 0 -5 -1 0 -5 -1 0 5 -1 0 5 -1 0 -5 1 0 -5 2 0 -5 -2 0 -5 2 0 5 -2 0 5 -2 0 -5 2 0 5 2 0 5 -2 0 5 -3 0 5 -3 0 -5 3 0 -5 3 0 5 -3 0 -5 4 0 5 -4 0 5 -4 0 -5 -4 0 -5 -5 0 5 -5 0 5 -5 0 -5 -6 0 5 -6 0 5 -6 0 -5 -7 0 5 -7 0 5 -7 0 5 -8 0 5 -9 0 5 -10 0 5 -11 0 -6 0 0 6 0 0 -6 0 0 6 0 0 -6 0 0 6 -1 0 -6 1 0 -6 -1 0 -6 -1 0 6 -1 0 -6 2 0 6 -2 0 -6 -2 0 -6 -2 0 6 -2 0 -6 3 0 6 -3 0 6 -3 0 -6 3 0 6 -4 0 6 -4 0 -6 4 0 6 -5 0 -6 5 0 6 -5 0 6 -6 0 6 -6 0 6 -7 0 6 -7 0 6 -8 0 6 -9 0 6 -10 0 6 -11 0 7 0 0 -7 0 0 -7 -1 0 7 -1 0 -7 1 0 7 -2 0 7 -2 0 -7 2 0 7 -3 0 7 -3 0 -7 3 0 7 -4 0 -7 4 0 7 -4 0 7 -5 0 7 -5 0 -7 5 0 7 -6 0 7 -6 0 7 -7 0 7 -7 0 7 -8 0 7 -8 0 7 -9 0 7 -10 0 7 -11 0 8 0 0 -8 0 0 -8 1 0 8 -1 0 -8 2 0 8 -2 0 8 2 0 8 -3 0 -8 3 0 8 -4 0 -8 4 0 8 -5 0 -8 5 0 8 -6 0 8 -6 0 8 -7 0 8 -7 0 8 -8 0 8 -8 0 8 -9 0 8 -10 0 -9 0 0 9 0 0 9 1 0 -9 1 0 -9 -1 0 9 -1 0 9 -2 0 -9 2 0 -9 3 0 9 -3 0 9 -4 0 -9 4 0 -9 5 0 9 -5 0 -9 6 0 9 -6 0 9 -7 0 9 -8 0 -10 0 0 10 0 0 10 -1 0 10 1 0 -10 1 0 -10 -1 0 10 -2 0 -10 2 0 10 -3 0 -10 3 0 10 -4 0 -10 4 0 10 -5 0 -10 5 0 10 -6 0 10 -7 0 10 -8 0 -11 0 0 11 0 0 -11 -1 0 11 -1 0 -11 1 0 11 -2 0 -11 -2 0 -11 3 0 11 -3 0 -11 4 0 11 -4 0 -11 5 0 11 -5 0 11 -6 0 11 -7 0 11 -8 0 11 -9 0 12 0 0 -12 0 0 -12 -1 0 -12 1 0 12 -1 0 -12 -2 0 12 -2 0 -12 2 0 -12 -3 0 12 -3 0 -12 3 0 12 -4 0 -12 4 0 -12 5 0 12 -5 0 12 -6 0 12 -7 0 12 -8 0 -13 0 0 13 -1 0 -13 1 0 -13 -1 0 13 -2 0 -13 -2 0 -13 2 0 -13 3 0 13 -3 0 -13 4 0 13 -4 0 -13 -4 0 13 -5 0 13 -6 0 13 -7 0 -14 0 0 -14 1 0 -14 -1 0 -14 -2 0 -14 2 0 14 -2 0 -14 3 0 -14 -3 0 14 -3 0 -14 4 0 14 -4 0 -14 -4 0 -14 -5 0 14 -5 0 14 -6 0 -15 0 0 -15 -1 0 15 -2 0 -15 -2 0 -15 2 0 -15 3 0 -15 -3 0 15 -3 0 -15 -4 0 15 -4 0 -16 0 0 -16 -1 0 -16 1 0 -16 2 0 -16 3 1 0 -12 1 0 -11 1 0 -10 1 0 -9 1 0 -8 -1 0 7 1 0 -7 -1 0 6 1 0 -6 1 0 -5 -1 0 5 1 0 -5 -1 0 4 1 0 -4 -1 0 4 -1 0 4 1 0 -4 -1 0 3 1 0 -3 -1 0 3 1 0 -3 -1 0 2 -1 0 2 1 0 -2 -1 0 2 -1 0 2 1 0 -2 1 0 -1 1 0 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-1 -9 2 -2 -9 -2 -2 9 2 2 -9 2 -3 -9 -2 -3 9 2 3 9 3 -9 9 3 -8 9 3 -7 9 3 -7 9 3 -6 9 3 -6 9 3 -6 9 3 -5 9 3 -5 9 3 -5 9 3 -4 9 3 -4 9 3 -3 9 -3 -3 9 3 -3 -9 3 2 9 3 -2 -9 3 1 -9 -3 1 9 3 -1 -9 -3 0 -9 3 0 9 3 0 -9 3 -1 -9 -3 -1 -9 -3 -2 -9 3 -2 9 3 2 -9 3 -3 -9 -3 -3 9 3 3 9 4 -9 9 4 -8 9 4 -7 9 4 -7 9 4 -6 9 4 -6 9 4 -6 9 4 -5 9 4 -5 9 4 -5 9 4 -4 9 4 -4 -9 4 3 9 4 -3 9 4 -3 -9 4 2 9 4 -2 9 4 -2 -9 -4 1 -9 4 1 9 4 -1 -9 -4 0 -9 4 0 9 4 0 -9 -4 -1 -9 4 -1 9 4 1 -9 -4 -2 -9 4 -2 9 4 2 9 5 -8 9 5 -7 9 5 -7 9 5 -6 9 5 -6 9 5 -6 9 5 -5 9 5 -5 9 5 -5 9 5 -4 9 5 -4 9 5 -3 9 5 -3 -9 5 2 9 5 -2 9 5 -2 -9 5 1 9 5 -1 9 5 -1 -9 -5 0 -9 5 0 9 5 0 -9 -5 -1 -9 5 -1 9 5 1 -9 -5 -2 -9 5 -2 9 6 -7 9 6 -7 9 6 -6 9 6 -6 9 6 -6 9 6 -5 9 6 -5 9 6 -5 9 6 -4 9 6 -4 9 6 -4 9 6 -3 9 6 -3 -9 6 2 9 6 -2 9 6 -2 -9 6 1 9 6 -1 9 6 -1 -9 -6 0 -9 6 0 9 6 0 9 6 0 -9 -6 -1 -9 6 -1 9 6 1 9 7 -7 9 7 -6 9 7 -6 9 7 -6 9 7 -5 9 7 -5 9 7 -5 9 7 -4 9 7 -4 9 7 -4 9 7 -3 9 7 -3 9 7 -2 9 7 -2 -9 7 1 9 7 -1 9 7 -1 -9 7 0 9 7 0 9 7 0 -9 -7 -1 9 7 1 -9 7 -1 9 7 1 9 8 -5 9 8 -5 9 8 -5 9 8 -4 9 8 -4 9 8 -4 9 8 -3 9 8 -3 9 8 -2 9 8 -2 9 8 -1 -9 8 1 9 8 -1 9 8 0 -9 8 0 9 8 0 9 9 -2 10 0 -5 10 0 -4 10 0 -4 10 0 -2 10 0 -1 -10 0 0 10 0 0 -10 0 -1 10 1 -5 10 1 -5 10 1 -5 10 1 -4 10 1 -4 10 1 -3 10 -1 -3 10 1 -3 10 1 -2 10 -1 -2 -10 -1 1 10 1 -1 10 -1 -1 -10 -1 0 10 1 0 10 -1 0 -10 -1 -1 10 2 -7 10 2 -6 10 2 -6 10 2 -5 10 2 -5 10 2 -5 10 2 -4 10 -2 -4 10 2 -4 10 2 -3 10 -2 -3 10 2 -3 10 2 -2 10 -2 -2 -10 -2 1 10 2 -1 10 -2 -1 -10 -2 0 10 3 -7 10 3 -7 10 3 -6 10 3 -6 10 3 -6 10 3 -5 10 3 -5 10 3 -5 10 3 -4 10 3 -4 10 3 -3 10 -3 -3 10 3 -3 10 -3 -2 10 3 -2 -10 3 1 10 3 -1 -10 3 0 -10 -3 0 10 3 0 10 4 -6 10 4 -6 10 4 -6 10 4 -5 10 4 -5 10 4 -5 10 4 -4 10 4 -4 10 4 -3 10 -4 -3 10 4 -3 -10 4 2 10 4 -2 10 4 -2 -10 4 1 10 4 -1 10 5 -6 10 5 -5 10 5 -5 10 5 -5 10 5 -4 10 5 -4 10 5 -3 10 5 -3 -10 5 2 10 5 -2 10 5 -2 -10 5 1 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -6 12 -1 0.0909 -10 5 6 0.0912 6 8 -10 0.0953 10 -3 -7 0.1184 -1 -12 8 0.0348 -10 -3 2 0.0967 2 -10 -10 0.0433 0 10 9 0.0307 -7 2 -7 0.0851 3 -1 -13 0.0760 -2 -6 -10 0.0605 6 13 -3 0.0961 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 W1 Cl1 . 3_666 180.0 y Cl2 W1 Cl1 . 3_666 91.37(4) y Cl2 W1 Cl1 3_666 . 91.37(4) ? Cl2 W1 Cl1 3_666 3_666 88.63(4) ? Cl2 W1 Cl1 . . 88.63(4) y Cl2 W1 Cl2 3_666 . 180.0 y O1 W1 Cl1 3_666 3_666 89.92(7) ? O1 W1 Cl1 . . 89.92(7) y O1 W1 Cl1 3_666 . 90.08(7) ? O1 W1 Cl1 . 3_666 90.08(7) y O1 W1 Cl2 . 3_666 90.16(7) y O1 W1 Cl2 3_666 . 90.16(7) ? O1 W1 Cl2 . . 89.84(7) y O1 W1 Cl2 3_666 3_666 89.84(7) ? O1 W1 O1 . 3_666 180.0 y C3 O1 W1 . . 123.46(18) ? C3 O1 C1 . . 114.1(2) ? C1 O1 W1 . . 122.43(19) ? O1 C3 H3A . . 109.1 ? O1 C3 H3B . . 109.1 ? O1 C3 C4 . . 112.6(3) ? H3A C3 H3B . . 107.8 ? C4 C3 H3A . . 109.1 ? C4 C3 H3B . . 109.1 ? O1 C1 H1A . . 109.2 ? O1 C1 H1B . . 109.2 ? O1 C1 C2 . . 111.9(3) ? H1A C1 H1B . . 107.9 ? C2 C1 H1A . . 109.2 ? C2 C1 H1B . . 109.2 ? C1 C2 H2A . . 109.5 ? C1 C2 H2B . . 109.5 ? C1 C2 H2C . . 109.5 ? H2A C2 H2B . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? C3 C4 H4A . . 109.5 ? C3 C4 H4B . . 109.5 ? C3 C4 H4C . . 109.5 ? H4A C4 H4B . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 Cl1 3_666 2.3586(10) ? W1 Cl1 . 2.3586(10) y W1 Cl2 3_666 2.3554(10) ? W1 Cl2 . 2.3554(10) y W1 O1 3_666 2.070(2) ? W1 O1 . 2.070(2) y O1 C1 . 1.482(3) y O1 C3 . 1.473(4) y C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C3 C4 . 1.500(5) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C1 C2 . 1.497(4) ? C2 H2A . 0.9600 ? C2 H2B . 0.9600 ? C2 H2C . 0.9600 ? C4 H4A . 0.9600 ? C4 H4B . 0.9600 ? C4 H4C . 0.9600 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag W1 O1 C3 C4 . . . . -115.4(3) ? W1 O1 C1 C2 . . . . -115.7(3) ? C3 O1 C1 C2 . . . . 63.1(4) ? C1 O1 C3 C4 . . . . 65.8(4) ?