#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:47:08 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515781.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_4515781 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 'C12 H4 Cl8 F6 N2 W2, 2(C7 H8)' _chemical_formula_sum 'C26 H20 Cl8 F6 N2 W2' _chemical_formula_weight 1125.74 _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 68.524(16) _cell_angle_beta 86.291(18) _cell_angle_gamma 81.137(18) _cell_formula_units_Z 1 _cell_length_a 7.1984(5) _cell_length_b 9.6255(6) _cell_length_c 12.8058(8) _cell_measurement_reflns_used 9983 _cell_measurement_temperature 120 _cell_measurement_theta_max 35.380 _cell_measurement_theta_min 2.864 _cell_volume 815.79(13) _computing_cell_refinement 'SAINT V8.30C (Bruker, 2013)' _computing_data_collection 'APEX v.2013.4-1' _computing_data_reduction 'SAINT V8.30C (Bruker, 2013)' _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_area_resol_mean 10.4 _diffrn_detector_type 'Bruker PHOTON 100 CMOS' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.905 _diffrn_measurement_device '3-circle area detector diffractometer' _diffrn_measurement_device_type D8V_Mo _diffrn_measurement_method \w-scan _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_unetI/netI 0.0407 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.905 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 16041 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.905 _diffrn_reflns_theta_full 32.500 _diffrn_reflns_theta_max 35.568 _diffrn_reflns_theta_min 2.864 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\mS microsource' _exptl_absorpt_coefficient_mu 7.757 _exptl_absorpt_correction_T_max 0.7836 _exptl_absorpt_correction_T_min 0.1618 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; SADABS-2009/1 (Bruker,2010) was used for absorption correction. wR2(int) was 0.1117 before and 0.0471 after correction. The Ratio of minimum to maximum transmission is 0.2065. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.243 _exptl_crystal_size_mid 0.215 _exptl_crystal_size_min 0.048 _refine_diff_density_max 1.902 _refine_diff_density_min -1.751 _refine_diff_density_rms 0.173 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 6780 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0240 _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^)+(0.0216P)^2^+0.3818P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.0580 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6226 _reflns_number_total 6780 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b02201_si_002.cif _cod_data_source_block 1f _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_original_cell_volume 815.80(13) _cod_database_code 4515781 _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 0.707 _shelx_estimated_absorpt_t_min 0.254 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13) 2.b Idealised Me refined as rotating group: C7(H7A,H7B,H7C) ; _shelx_res_file ; 13srv191.res created by SHELXL-2014/7 TITL 13srv191 in P-1 #2 REM reset to P-1 #2 CELL 0.71073 7.1984 9.6255 12.8058 68.524 86.291 81.137 ZERR 1 0.0005 0.0006 0.0008 0.016 0.018 0.018 LATT 1 SFAC C H Cl F N W UNIT 26 20 8 6 2 2 L.S. 7 PLAN 6 SIZE 0.048 0.215 0.243 TEMP -153.15 BOND fmap 2 acta 65 OMIT -4 -9 7 OMIT -4 -9 8 REM REM REM WGHT 0.021600 0.381800 FVAR 0.46889 W 6 0.617107 0.526561 0.626750 11.00000 0.01792 0.01279 = 0.01102 -0.00574 -0.00064 -0.00025 CL1 3 0.809619 0.659534 0.488674 11.00000 0.02171 0.02151 = 0.01573 -0.00706 0.00274 -0.00462 CL2 3 0.863368 0.362513 0.723178 11.00000 0.02459 0.02169 = 0.01751 -0.00746 -0.00658 0.00515 CL3 3 0.404615 0.370424 0.734771 11.00000 0.02813 0.01962 = 0.01542 -0.00600 0.00239 -0.00809 CL4 3 0.359609 0.649307 0.495120 11.00000 0.02014 0.01467 = 0.01508 -0.00775 -0.00315 0.00357 F1 4 0.643185 0.555017 0.922692 11.00000 0.02523 0.01793 = 0.01766 -0.00377 -0.00249 0.00459 F2 4 0.334635 1.014742 0.934545 11.00000 0.03675 0.03462 = 0.03859 -0.02937 0.00170 0.00295 F3 4 0.399846 0.936092 0.593863 11.00000 0.03552 0.02313 = 0.01467 -0.00237 -0.00062 -0.00016 N 5 0.575055 0.650024 0.697956 11.00000 0.01976 0.01395 = 0.01346 -0.00550 0.00084 -0.00264 C1 1 0.522693 0.742671 0.756644 11.00000 0.01642 0.01567 = 0.01416 -0.00859 0.00155 -0.00461 C2 1 0.552191 0.694214 0.872006 11.00000 0.01491 0.01631 = 0.01700 -0.00662 -0.00134 -0.00023 C3 1 0.490924 0.783114 0.934062 11.00000 0.01959 0.02498 = 0.01955 -0.01275 -0.00061 -0.00164 AFIX 43 H3 2 0.510648 0.748211 1.012669 11.00000 -1.20000 AFIX 0 C4 1 0.399195 0.925833 0.876082 11.00000 0.02045 0.02177 = 0.02622 -0.01615 0.00154 -0.00189 C5 1 0.366369 0.983139 0.761788 11.00000 0.02205 0.01471 = 0.02744 -0.00950 0.00066 -0.00151 AFIX 43 H5 2 0.303936 1.082461 0.725162 11.00000 -1.20000 AFIX 0 C6 1 0.428328 0.889604 0.704081 11.00000 0.01882 0.01652 = 0.01679 -0.00494 0.00037 -0.00351 C7 1 0.996131 0.754463 1.004487 11.00000 0.02751 0.02862 = 0.02136 -0.00870 -0.00165 0.00062 AFIX 137 H7A 2 0.877472 0.723731 1.040972 11.00000 -1.50000 H7B 2 1.021462 0.842872 1.019034 11.00000 -1.50000 H7C 2 1.098647 0.671506 1.034528 11.00000 -1.50000 AFIX 0 C8 1 0.982053 0.793195 0.880272 11.00000 0.01610 0.01764 = 0.01997 -0.00590 0.00011 -0.00293 C9 1 1.048129 0.686421 0.832133 11.00000 0.01705 0.01789 = 0.02264 -0.00639 0.00029 -0.00087 AFIX 43 H9 2 1.104197 0.588830 0.878339 11.00000 -1.20000 AFIX 0 C10 1 1.033311 0.720428 0.717590 11.00000 0.02153 0.02580 = 0.02637 -0.01280 0.00414 -0.00796 AFIX 43 H10 2 1.079163 0.646254 0.686087 11.00000 -1.20000 AFIX 0 C11 1 0.951609 0.862638 0.648926 11.00000 0.02965 0.03275 = 0.01748 -0.00586 -0.00222 -0.01228 AFIX 43 H11 2 0.940045 0.886042 0.570635 11.00000 -1.20000 AFIX 0 C12 1 0.887041 0.970170 0.696308 11.00000 0.02851 0.01981 = 0.02681 -0.00087 -0.00706 -0.00379 AFIX 43 H12 2 0.832867 1.068252 0.649867 11.00000 -1.20000 AFIX 0 C13 1 0.901023 0.935516 0.810677 11.00000 0.02291 0.01633 = 0.02715 -0.00729 -0.00392 -0.00027 AFIX 43 H13 2 0.854757 1.009768 0.842036 11.00000 -1.20000 AFIX 0 HKLF 4 REM 13srv191 in P-1 #2 REM R1 = 0.0240 for 6226 Fo > 4sig(Fo) and 0.0286 for all 6780 data REM 200 parameters refined using 0 restraints END WGHT 0.0216 0.3790 REM Highest difference peak 1.902, deepest hole -1.751, 1-sigma level 0.173 Q1 1 0.6517 0.5964 0.5451 11.00000 0.05 1.90 Q2 1 0.8541 0.5752 0.8820 11.00000 0.05 1.87 Q3 1 0.6401 0.5967 0.6198 11.00000 0.05 1.72 Q4 1 0.5781 0.4522 0.7021 11.00000 0.05 1.63 Q5 1 0.7137 0.5610 0.6037 11.00000 0.05 1.57 Q6 1 0.6051 0.5816 0.4997 11.00000 0.05 1.52 ; _shelx_res_checksum 39707 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 W W 0.61711(2) 0.52656(2) 0.62675(2) 0.01369(3) Uani 1 1 d . Cl1 Cl 0.80962(8) 0.65953(7) 0.48867(5) 0.01951(10) Uani 1 1 d . Cl2 Cl 0.86337(8) 0.36251(7) 0.72318(5) 0.02180(11) Uani 1 1 d . Cl3 Cl 0.40461(9) 0.37042(7) 0.73477(5) 0.02074(11) Uani 1 1 d . Cl4 Cl 0.35961(8) 0.64931(6) 0.49512(5) 0.01649(9) Uani 1 1 d . F1 F 0.6432(2) 0.55502(16) 0.92269(12) 0.0218(3) Uani 1 1 d . F2 F 0.3346(3) 1.0147(2) 0.93455(16) 0.0331(4) Uani 1 1 d . F3 F 0.3998(2) 0.93609(18) 0.59386(13) 0.0261(3) Uani 1 1 d . N N 0.5751(3) 0.6500(2) 0.69796(16) 0.0156(3) Uani 1 1 d . C1 C 0.5227(3) 0.7427(2) 0.75664(19) 0.0143(4) Uani 1 1 d . C2 C 0.5522(3) 0.6942(3) 0.8720(2) 0.0161(4) Uani 1 1 d . C3 C 0.4909(3) 0.7831(3) 0.9341(2) 0.0202(4) Uani 1 1 d . H3 H 0.5106 0.7482 1.0127 0.024 Uiso 1 1 calc R C4 C 0.3992(3) 0.9258(3) 0.8761(2) 0.0209(4) Uani 1 1 d . C5 C 0.3664(3) 0.9831(3) 0.7618(2) 0.0210(5) Uani 1 1 d . H5 H 0.3039 1.0825 0.7252 0.025 Uiso 1 1 calc R C6 C 0.4283(3) 0.8896(3) 0.7041(2) 0.0176(4) Uani 1 1 d . C7 C 0.9961(4) 0.7545(3) 1.0045(2) 0.0264(5) Uani 1 1 d . H7A H 0.8775 0.7237 1.0410 0.040 Uiso 1 1 calc GR H7B H 1.0215 0.8429 1.0190 0.040 Uiso 1 1 calc GR H7C H 1.0986 0.6715 1.0345 0.040 Uiso 1 1 calc GR C8 C 0.9821(3) 0.7932(3) 0.8803(2) 0.0181(4) Uani 1 1 d . C9 C 1.0481(3) 0.6864(3) 0.8321(2) 0.0197(4) Uani 1 1 d . H9 H 1.1042 0.5888 0.8783 0.024 Uiso 1 1 calc R C10 C 1.0333(4) 0.7204(3) 0.7176(2) 0.0233(5) Uani 1 1 d . H10 H 1.0792 0.6463 0.6861 0.028 Uiso 1 1 calc R C11 C 0.9516(4) 0.8626(3) 0.6489(2) 0.0266(5) Uani 1 1 d . H11 H 0.9400 0.8860 0.5706 0.032 Uiso 1 1 calc R C12 C 0.8870(4) 0.9702(3) 0.6963(2) 0.0268(5) Uani 1 1 d . H12 H 0.8329 1.0683 0.6499 0.032 Uiso 1 1 calc R C13 C 0.9010(3) 0.9355(3) 0.8107(2) 0.0224(5) Uani 1 1 d . H13 H 0.8548 1.0098 0.8420 0.027 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 0.01792(4) 0.01279(4) 0.01102(4) -0.00574(3) -0.00064(3) -0.00025(3) Cl1 0.0217(2) 0.0215(3) 0.0157(2) -0.0071(2) 0.00274(19) -0.0046(2) Cl2 0.0246(3) 0.0217(3) 0.0175(2) -0.0075(2) -0.0066(2) 0.0052(2) Cl3 0.0281(3) 0.0196(2) 0.0154(2) -0.0060(2) 0.0024(2) -0.0081(2) Cl4 0.0201(2) 0.0147(2) 0.0151(2) -0.00775(18) -0.00315(18) 0.00357(18) F1 0.0252(7) 0.0179(7) 0.0177(7) -0.0038(6) -0.0025(5) 0.0046(5) F2 0.0368(9) 0.0346(9) 0.0386(10) -0.0294(8) 0.0017(8) 0.0030(7) F3 0.0355(8) 0.0231(7) 0.0147(6) -0.0024(6) -0.0006(6) -0.0002(6) N 0.0198(8) 0.0140(8) 0.0135(8) -0.0055(7) 0.0008(7) -0.0026(7) C1 0.0164(9) 0.0157(9) 0.0142(9) -0.0086(8) 0.0015(7) -0.0046(7) C2 0.0149(8) 0.0163(9) 0.0170(10) -0.0066(8) -0.0013(7) -0.0002(7) C3 0.0196(10) 0.0250(11) 0.0195(11) -0.0128(9) -0.0006(8) -0.0016(9) C4 0.0205(10) 0.0218(11) 0.0262(12) -0.0162(10) 0.0015(9) -0.0019(8) C5 0.0221(10) 0.0147(10) 0.0274(12) -0.0095(9) 0.0007(9) -0.0015(8) C6 0.0188(9) 0.0165(10) 0.0168(10) -0.0049(8) 0.0004(8) -0.0035(8) C7 0.0275(12) 0.0286(13) 0.0214(12) -0.0087(10) -0.0017(10) 0.0006(10) C8 0.0161(9) 0.0176(10) 0.0200(10) -0.0059(9) 0.0001(8) -0.0029(8) C9 0.0170(9) 0.0179(10) 0.0226(11) -0.0064(9) 0.0003(8) -0.0009(8) C10 0.0215(10) 0.0258(12) 0.0264(12) -0.0128(10) 0.0041(9) -0.0080(9) C11 0.0297(12) 0.0328(14) 0.0175(11) -0.0059(10) -0.0022(9) -0.0123(11) C12 0.0285(12) 0.0198(11) 0.0268(13) -0.0009(10) -0.0071(10) -0.0038(10) C13 0.0229(11) 0.0163(10) 0.0272(12) -0.0073(9) -0.0039(9) -0.0003(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' 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' 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 0.1400 0.00 1.00 1.00 0.1030 0.00 0.00 1.00 0.0460 0.00 0.00 -1.00 0.0020 -2.00 0.00 1.00 0.1050 2.00 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 _geom_angle_site_symmetry_3 Cl1 W Cl3 166.45(2) . Cl1 W Cl4 83.42(2) 2_666 Cl1 W Cl4 86.75(2) . Cl2 W Cl1 92.50(3) . Cl2 W Cl3 91.21(3) . Cl2 W Cl4 85.17(2) 2_666 Cl2 W Cl4 162.97(2) . Cl3 W Cl4 83.91(2) 2_666 Cl3 W Cl4 85.91(2) . Cl4 W Cl4 77.84(2) 2_666 N W Cl1 97.87(6) . N W Cl2 101.75(7) . N W Cl3 94.12(6) . N W Cl4 172.87(7) 2_666 N W Cl4 95.20(7) . W Cl4 W 102.16(2) 2_666 C1 N W 173.69(17) . N C1 C2 121.7(2) . N C1 C6 121.1(2) . C2 C1 C6 117.2(2) . F1 C2 C1 117.7(2) . F1 C2 C3 119.7(2) . C3 C2 C1 122.6(2) . C2 C3 C4 116.6(2) . F2 C4 C3 118.1(2) . F2 C4 C5 117.5(2) . C3 C4 C5 124.4(2) . C6 C5 C4 116.7(2) . F3 C6 C1 117.3(2) . F3 C6 C5 120.3(2) . C5 C6 C1 122.5(2) . C9 C8 C7 120.5(2) . C9 C8 C13 118.4(2) . C13 C8 C7 121.1(2) . C10 C9 C8 121.0(2) . C9 C10 C11 120.2(2) . C10 C11 C12 119.1(2) . C13 C12 C11 120.5(2) . C12 C13 C8 120.8(2) . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 W Cl1 2.2929(7) . W Cl2 2.2701(8) . W Cl3 2.3290(7) . W Cl4 2.4381(8) . W Cl4 2.6725(6) 2_666 W N 1.7269(19) . Cl4 W 2.6725(6) 2_666 F1 C2 1.339(3) . F2 C4 1.346(3) . F3 C6 1.335(3) . N C1 1.361(3) . C1 C2 1.397(3) . C1 C6 1.407(3) . C2 C3 1.376(3) . C3 C4 1.383(4) . C4 C5 1.384(4) . C5 C6 1.370(3) . C7 C8 1.501(4) . C8 C9 1.392(3) . C8 C13 1.392(3) . C9 C10 1.389(4) . C10 C11 1.389(4) . C11 C12 1.389(4) . C12 C13 1.385(4) .