#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:47:08 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515784.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_4515784 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 'C10 H10 Cl4 F3 N O W' _chemical_formula_sum 'C10 H10 Cl4 F3 N O W' _chemical_formula_weight 542.84 _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 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 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269) ; _cell_angle_alpha 90 _cell_angle_beta 100.845(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.3589(5) _cell_length_b 11.3408(5) _cell_length_c 11.9422(6) _cell_measurement_reflns_used 9923 _cell_measurement_temperature 120 _cell_measurement_theta_max 34.45 _cell_measurement_theta_min 2.50 _cell_volume 1510.91(12) _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 _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 0.966 _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_radiation_xray_symbol K-L~3~ _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0297 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 31676 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 32.500 _diffrn_reflns_theta_max 34.986 _diffrn_reflns_theta_min 1.825 _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 8.376 _exptl_absorpt_correction_T_max 0.6074 _exptl_absorpt_correction_T_min 0.3876 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0534 before and 0.0394 after correction. The Ratio of minimum to maximum transmission is 0.6381. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'greenish blue' _exptl_crystal_colour_modifier greenish _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 2.386 _exptl_crystal_description block _exptl_crystal_F_000 1016 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _refine_diff_density_max 2.440 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.138 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 6423 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.997 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0209 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0230P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.0488 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4968 _reflns_number_total 6423 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b02201_si_002.cif _cod_data_source_block 2f _cod_database_code 4515784 _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 0.592 _shelx_estimated_absorpt_t_min 0.348 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5) ; _shelx_res_file ; 11srv241.res created by SHELXL-2014/7 TITL 11srv241 in P2(1)/c REM reset to P21/c #14 CELL 0.71073 11.3589 11.3408 11.9422 90 100.845 90 ZERR 4 0.0005 0.0005 0.0006 0 0.006 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl F N O W UNIT 40 40 16 12 4 4 4 L.S. 6 PLAN 6 SIZE 0.07 0.12 0.16 TEMP -153.15 BOND $H fmap 2 acta 65 REM REM REM WGHT 0.023000 FVAR 0.07624 W 7 0.745756 0.375630 0.512904 11.00000 0.01989 0.01634 = 0.02080 -0.00066 0.00354 0.00089 CL1 3 0.620459 0.373719 0.646662 11.00000 0.02692 0.03207 = 0.03391 -0.00391 0.01408 -0.00111 CL2 3 0.752312 0.580719 0.521191 11.00000 0.03613 0.01716 = 0.03271 -0.00004 0.00432 0.00257 CL3 3 0.903882 0.378143 0.414032 11.00000 0.02872 0.02855 = 0.02445 0.00099 0.01041 -0.00001 CL4 3 0.770749 0.172151 0.538855 11.00000 0.02995 0.01732 = 0.03380 0.00000 0.00617 0.00010 F1 4 0.625596 0.508342 0.208463 11.00000 0.03586 0.03944 = 0.03915 0.00983 0.00606 -0.00996 F2 4 0.244915 0.365056 0.045754 11.00000 0.03502 0.04760 = 0.03624 -0.00491 -0.01350 0.00451 F3 4 0.443348 0.220305 0.398461 11.00000 0.03882 0.03492 = 0.03349 0.00974 0.00271 -0.00710 O 6 0.891901 0.388562 0.666640 11.00000 0.02352 0.02286 = 0.02181 -0.00362 0.00348 0.00437 N 5 0.631770 0.368313 0.395431 11.00000 0.02524 0.01975 = 0.02598 -0.00198 0.00538 0.00228 C1 1 0.537052 0.365187 0.305853 11.00000 0.02292 0.02106 = 0.02368 -0.00216 0.00423 0.00307 C2 1 0.531760 0.437663 0.210693 11.00000 0.02687 0.02313 = 0.02803 0.00016 0.00765 0.00146 C3 1 0.434589 0.439922 0.122800 11.00000 0.03379 0.02970 = 0.02249 0.00237 0.00569 0.00506 AFIX 43 H3 2 0.431294 0.491708 0.059759 11.00000 -1.20000 AFIX 0 C4 1 0.342146 0.363604 0.130320 11.00000 0.02617 0.03398 = 0.02564 -0.00802 -0.00254 0.00732 C5 1 0.341802 0.287112 0.219888 11.00000 0.02503 0.02980 = 0.03207 -0.00236 0.00060 -0.00193 AFIX 43 H5 2 0.276786 0.234700 0.220978 11.00000 -1.20000 AFIX 0 C6 1 0.439452 0.289721 0.307689 11.00000 0.02883 0.02372 = 0.02525 0.00169 0.00526 0.00186 C7 1 0.998527 0.312406 0.691155 11.00000 0.02836 0.03644 = 0.02667 -0.00176 0.00071 0.01106 AFIX 23 H7A 2 1.038316 0.307910 0.624300 11.00000 -1.20000 H7B 2 0.976368 0.231728 0.711145 11.00000 -1.20000 AFIX 0 C8 1 1.079642 0.369526 0.790520 11.00000 0.02632 0.03714 = 0.02577 0.00333 0.00058 -0.00336 AFIX 23 H8A 2 1.133725 0.427459 0.764241 11.00000 -1.20000 H8B 2 1.128448 0.309886 0.839078 11.00000 -1.20000 AFIX 0 C9 1 0.992395 0.430188 0.854478 11.00000 0.03702 0.03036 = 0.02383 -0.00278 0.00442 -0.00702 AFIX 23 H9A 2 0.959905 0.373926 0.904310 11.00000 -1.20000 H9B 2 1.031404 0.496433 0.901294 11.00000 -1.20000 AFIX 0 C10 1 0.896318 0.473449 0.760429 11.00000 0.03351 0.03142 = 0.02919 -0.01238 0.00581 -0.00065 AFIX 23 H10A 2 0.818246 0.476480 0.785762 11.00000 -1.20000 H10B 2 0.915730 0.553357 0.735885 11.00000 -1.20000 AFIX 0 HKLF 4 REM 11srv241 in P2(1)/c REM R1 = 0.0209 for 4968 Fo > 4sig(Fo) and 0.0317 for all 6423 data REM 181 parameters refined using 0 restraints END WGHT 0.0234 0.0000 REM Highest difference peak 2.440, deepest hole -0.724, 1-sigma level 0.138 Q1 1 0.7476 0.3772 0.4573 11.00000 0.05 2.44 Q2 1 0.8009 0.3738 0.5264 11.00000 0.05 1.70 Q3 1 0.2533 0.3704 -0.0128 11.00000 0.05 1.29 Q4 1 0.7212 0.1693 0.4821 11.00000 0.05 1.28 Q5 1 0.8590 0.3743 0.3607 11.00000 0.05 1.15 Q6 1 0.6857 0.3766 0.4910 11.00000 0.05 1.11 ; _shelx_res_checksum 9078 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 W W 0.74576(2) 0.37563(2) 0.51290(2) 0.01905(3) Uani 1 1 d . Cl1 Cl 0.62046(5) 0.37372(5) 0.64666(5) 0.02988(11) Uani 1 1 d . Cl2 Cl 0.75231(5) 0.58072(5) 0.52119(5) 0.02895(11) Uani 1 1 d . Cl3 Cl 0.90388(5) 0.37814(5) 0.41403(5) 0.02654(10) Uani 1 1 d . Cl4 Cl 0.77075(5) 0.17215(5) 0.53885(5) 0.02700(11) Uani 1 1 d . F1 F 0.62560(13) 0.50834(13) 0.20846(13) 0.0383(3) Uani 1 1 d . F2 F 0.24492(14) 0.36506(14) 0.04575(16) 0.0422(4) Uani 1 1 d . F3 F 0.44335(13) 0.22031(12) 0.39846(13) 0.0363(3) Uani 1 1 d . O O 0.89190(14) 0.38856(12) 0.66664(13) 0.0228(3) Uani 1 1 d . N N 0.63177(17) 0.36831(15) 0.39543(16) 0.0236(3) Uani 1 1 d . C1 C 0.53705(19) 0.36519(18) 0.30585(19) 0.0226(4) Uani 1 1 d . C2 C 0.5318(2) 0.43766(19) 0.2107(2) 0.0257(4) Uani 1 1 d . C3 C 0.4346(2) 0.4399(2) 0.12280(19) 0.0286(5) Uani 1 1 d . H3 H 0.4313 0.4917 0.0598 0.034 Uiso 1 1 calc R C4 C 0.3421(2) 0.3636(2) 0.1303(2) 0.0296(5) Uani 1 1 d . C5 C 0.3418(2) 0.2871(2) 0.2199(2) 0.0296(5) Uani 1 1 d . H5 H 0.2768 0.2347 0.2210 0.036 Uiso 1 1 calc R C6 C 0.4395(2) 0.28972(19) 0.3077(2) 0.0259(4) Uani 1 1 d . C7 C 0.9985(2) 0.3124(2) 0.6912(2) 0.0311(5) Uani 1 1 d . H7A H 1.0383 0.3079 0.6243 0.037 Uiso 1 1 calc R H7B H 0.9764 0.2317 0.7111 0.037 Uiso 1 1 calc R C8 C 1.0796(2) 0.3695(2) 0.7905(2) 0.0303(5) Uani 1 1 d . H8A H 1.1337 0.4275 0.7642 0.036 Uiso 1 1 calc R H8B H 1.1284 0.3099 0.8391 0.036 Uiso 1 1 calc R C9 C 0.9924(2) 0.4302(2) 0.8545(2) 0.0306(5) Uani 1 1 d . H9A H 0.9599 0.3739 0.9043 0.037 Uiso 1 1 calc R H9B H 1.0314 0.4964 0.9013 0.037 Uiso 1 1 calc R C10 C 0.8963(2) 0.4734(2) 0.7604(2) 0.0314(5) Uani 1 1 d . H10A H 0.8182 0.4765 0.7858 0.038 Uiso 1 1 calc R H10B H 0.9157 0.5534 0.7359 0.038 Uiso 1 1 calc R 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 0.01989(4) 0.01634(4) 0.02080(4) -0.00066(3) 0.00354(3) 0.00089(3) Cl1 0.0269(2) 0.0321(3) 0.0339(3) -0.0039(2) 0.0141(2) -0.0011(2) Cl2 0.0361(3) 0.0172(2) 0.0327(3) -0.00004(19) 0.0043(2) 0.0026(2) Cl3 0.0287(2) 0.0286(2) 0.0245(2) 0.0010(2) 0.01041(19) 0.0000(2) Cl4 0.0300(3) 0.0173(2) 0.0338(3) 0.00000(19) 0.0062(2) 0.00010(19) F1 0.0359(8) 0.0394(8) 0.0392(9) 0.0098(7) 0.0061(7) -0.0100(6) F2 0.0350(8) 0.0476(9) 0.0362(8) -0.0049(7) -0.0135(6) 0.0045(7) F3 0.0388(8) 0.0349(8) 0.0335(8) 0.0097(6) 0.0027(6) -0.0071(6) O 0.0235(7) 0.0229(7) 0.0218(7) -0.0036(5) 0.0035(6) 0.0044(6) N 0.0252(9) 0.0197(8) 0.0260(9) -0.0020(7) 0.0054(7) 0.0023(7) C1 0.0229(9) 0.0211(9) 0.0237(9) -0.0022(7) 0.0042(7) 0.0031(8) C2 0.0269(11) 0.0231(10) 0.0280(11) 0.0002(8) 0.0077(8) 0.0015(8) C3 0.0338(12) 0.0297(11) 0.0225(10) 0.0024(8) 0.0057(9) 0.0051(9) C4 0.0262(11) 0.0340(12) 0.0256(11) -0.0080(9) -0.0025(8) 0.0073(9) C5 0.0250(11) 0.0298(11) 0.0321(12) -0.0024(9) 0.0006(9) -0.0019(9) C6 0.0288(11) 0.0237(10) 0.0252(10) 0.0017(8) 0.0053(9) 0.0019(8) C7 0.0284(11) 0.0364(13) 0.0267(11) -0.0018(9) 0.0007(9) 0.0111(10) C8 0.0263(11) 0.0371(12) 0.0258(11) 0.0033(10) 0.0006(8) -0.0034(10) C9 0.0370(13) 0.0304(12) 0.0238(11) -0.0028(9) 0.0044(9) -0.0070(10) C10 0.0335(12) 0.0314(12) 0.0292(12) -0.0124(9) 0.0058(10) -0.0007(10) 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 Cl4 88.54(2) Cl2 W Cl1 89.94(2) Cl2 W Cl4 167.93(2) Cl3 W Cl1 167.57(2) Cl3 W Cl2 89.30(2) Cl3 W Cl4 89.615(19) O W Cl1 83.84(4) O W Cl2 83.50(4) O W Cl3 83.75(4) O W Cl4 84.44(4) N W Cl1 95.47(6) N W Cl2 95.50(6) N W Cl3 96.95(6) N W Cl4 96.56(6) N W O 178.78(7) C7 O W 125.52(13) C10 O W 125.58(13) C10 O C7 108.90(17) C1 N W 176.77(16) N C1 C2 121.9(2) N C1 C6 120.7(2) C2 C1 C6 117.3(2) F1 C2 C1 117.2(2) F1 C2 C3 120.2(2) C3 C2 C1 122.6(2) C2 C3 H3 121.6 C2 C3 C4 116.9(2) C4 C3 H3 121.6 F2 C4 C3 118.1(2) F2 C4 C5 117.9(2) C5 C4 C3 124.1(2) C4 C5 H5 121.4 C6 C5 C4 117.3(2) C6 C5 H5 121.4 F3 C6 C1 117.8(2) F3 C6 C5 120.4(2) C5 C6 C1 121.8(2) O C7 H7A 110.7 O C7 H7B 110.7 O C7 C8 105.25(18) H7A C7 H7B 108.8 C8 C7 H7A 110.7 C8 C7 H7B 110.7 C7 C8 H8A 111.1 C7 C8 H8B 111.1 C7 C8 C9 103.30(19) H8A C8 H8B 109.1 C9 C8 H8A 111.1 C9 C8 H8B 111.1 C8 C9 H9A 111.2 C8 C9 H9B 111.2 H9A C9 H9B 109.1 C10 C9 C8 102.90(19) C10 C9 H9A 111.2 C10 C9 H9B 111.2 O C10 C9 105.84(18) O C10 H10A 110.6 O C10 H10B 110.6 C9 C10 H10A 110.6 C9 C10 H10B 110.6 H10A C10 H10B 108.7 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance W Cl1 2.3309(5) W Cl2 2.3286(6) W Cl3 2.3279(5) W Cl4 2.3385(5) W O 2.2363(15) W N 1.7227(19) F1 C2 1.338(3) F2 C4 1.349(3) F3 C6 1.334(3) O C7 1.471(3) O C10 1.471(2) N C1 1.368(3) C1 C2 1.395(3) C1 C6 1.404(3) C2 C3 1.373(3) C3 H3 0.9500 C3 C4 1.377(3) C4 C5 1.378(3) C5 H5 0.9500 C5 C6 1.376(3) C7 H7A 0.9900 C7 H7B 0.9900 C7 C8 1.505(3) C8 H8A 0.9900 C8 H8B 0.9900 C8 C9 1.524(3) C9 H9A 0.9900 C9 H9B 0.9900 C9 C10 1.494(3) C10 H10A 0.9900 C10 H10B 0.9900