#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:47:08 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515782.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_4515782 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 Cl8 N2 W2' _chemical_formula_sum 'C24 H34 Cl8 N2 W2' _chemical_formula_weight 1001.83 _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 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269) ; _cell_angle_alpha 106.301(8) _cell_angle_beta 106.481(8) _cell_angle_gamma 110.355(8) _cell_formula_units_Z 1 _cell_length_a 9.6082(6) _cell_length_b 9.7882(7) _cell_length_c 10.2905(6) _cell_measurement_reflns_used 9907 _cell_measurement_temperature 120 _cell_measurement_theta_max 34.763 _cell_measurement_theta_min 2.277 _cell_volume 788.82(14) _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 0.999 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART 6000' _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 0.0265 _diffrn_reflns_av_unetI/netI 0.0250 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.951 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 22919 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.951 _diffrn_reflns_theta_full 32.500 _diffrn_reflns_theta_max 34.979 _diffrn_reflns_theta_min 2.277 _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 _exptl_absorpt_coefficient_mu 7.982 _exptl_absorpt_correction_T_max 0.4756 _exptl_absorpt_correction_T_min 0.2685 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; SADABS-2009/1 (Bruker,2010) was used for absorption correction. wR2(int) was 0.0800 before and 0.0414 after correction. The Ratio of minimum to maximum transmission is 0.5646. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.109 _exptl_crystal_description block _exptl_crystal_F_000 476 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _refine_diff_density_max 1.464 _refine_diff_density_min -1.843 _refine_diff_density_rms 0.166 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 171 _refine_ls_number_reflns 6611 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.239 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0246 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+3.4000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.0638 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6162 _reflns_number_total 6611 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b02201_si_002.cif _cod_data_source_block 1g _cod_original_cell_volume 788.82(11) _cod_database_code 4515782 _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(H8A)=Uiso(H8B)=Uiso(H8C)=FVAR(1) Uiso(H9A)=Uiso(H9B)=Uiso(H9C)=FVAR(2) Uiso(H11A)=Uiso(H11B)=Uiso(H11C)=FVAR(3) Uiso(H12A)=Uiso(H12B)=Uiso(H12C)=FVAR(4) 3.a Ternary CH refined with riding coordinates: C7(H7), C10(H10) 3.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5) 3.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C) ; _shelx_res_file ; 12srv051.res created by SHELXL-2014/7 TITL 12srv051 in P-1 REM reset to P-1 #2 CELL 0.71073 9.6082 9.7882 10.2905 106.301 106.481 110.355 ZERR 1 0.0006 0.0007 0.0006 0.008 0.008 0.008 LATT 1 SFAC C H Cl N W UNIT 24 34 8 2 2 L.S. 7 PLAN 6 TEMP -153 BOND fmap 2 acta 65 REM REM REM WGHT 0.000000 3.400000 FVAR 0.41079 0.03507 0.03567 0.03210 0.02693 W 5 0.686670 0.986055 0.634700 11.00000 0.02153 0.01714 = 0.01815 0.01160 0.01047 0.01320 CL1 3 0.395050 0.822822 0.483540 11.00000 0.02264 0.01825 = 0.02123 0.01315 0.01107 0.01326 CL2 3 0.620411 1.107442 0.819145 11.00000 0.03463 0.02498 = 0.01929 0.01197 0.01432 0.02106 CL3 3 0.943593 1.198254 0.742318 11.00000 0.02353 0.02218 = 0.03408 0.01582 0.00961 0.01142 CL4 3 0.715502 0.885575 0.416925 11.00000 0.03368 0.02632 = 0.02492 0.01741 0.01952 0.02157 N 4 0.722886 0.853217 0.702401 11.00000 0.02072 0.01924 = 0.01707 0.01099 0.01062 0.01328 C1 1 0.754141 0.745851 0.754919 11.00000 0.01880 0.01947 = 0.01598 0.01051 0.00946 0.01369 C2 1 0.905191 0.742478 0.772248 11.00000 0.01981 0.01848 = 0.01985 0.01208 0.00963 0.01197 C3 1 0.932653 0.633323 0.825890 11.00000 0.02149 0.02341 = 0.02992 0.01832 0.01345 0.01518 AFIX 43 H3 2 1.032530 0.628135 0.840454 11.00000 -1.20000 AFIX 0 C4 1 0.819746 0.533245 0.858242 11.00000 0.02609 0.02480 = 0.02741 0.01870 0.01323 0.01776 AFIX 43 H4 2 0.842694 0.461002 0.894950 11.00000 -1.20000 AFIX 0 C5 1 0.672031 0.537746 0.837253 11.00000 0.02358 0.02058 = 0.02522 0.01579 0.01331 0.01296 AFIX 43 H5 2 0.593949 0.466023 0.857421 11.00000 -1.20000 AFIX 0 C6 1 0.636210 0.644859 0.787434 11.00000 0.02018 0.01736 = 0.01876 0.01037 0.00988 0.01217 C7 1 1.030631 0.853163 0.739277 11.00000 0.02169 0.02081 = 0.02393 0.01367 0.01278 0.01363 AFIX 13 H7 2 0.971923 0.882105 0.662953 11.00000 -1.20000 AFIX 0 C8 1 1.151275 1.008325 0.881112 11.00000 0.02341 0.02718 = 0.02656 0.01453 0.00799 0.00696 AFIX 137 H8A 2 1.090570 1.058113 0.920210 11.00000 21.00000 H8B 2 1.227562 1.082855 0.857253 11.00000 21.00000 H8C 2 1.212795 0.983168 0.956516 11.00000 21.00000 AFIX 0 C9 1 1.124278 0.775260 0.676529 11.00000 0.03933 0.03320 = 0.06004 0.03097 0.03786 0.02674 AFIX 137 H9A 2 1.184834 0.748021 0.750558 11.00000 31.00000 H9B 2 1.201354 0.850542 0.653884 11.00000 31.00000 H9C 2 1.046658 0.677294 0.584933 11.00000 31.00000 AFIX 0 C10 1 0.472970 0.645529 0.760510 11.00000 0.01936 0.01899 = 0.01984 0.01070 0.01043 0.01123 AFIX 13 H10 2 0.488422 0.755328 0.771738 11.00000 -1.20000 AFIX 0 C11 1 0.407704 0.606384 0.872374 11.00000 0.02640 0.03667 = 0.03221 0.02210 0.01951 0.01852 AFIX 137 H11A 2 0.383344 0.495806 0.857557 11.00000 41.00000 H11B 2 0.307521 0.617673 0.856517 11.00000 41.00000 H11C 2 0.490572 0.680676 0.974483 11.00000 41.00000 AFIX 0 C12 1 0.347982 0.525345 0.600459 11.00000 0.02400 0.02212 = 0.02389 0.01119 0.00768 0.01290 AFIX 137 H12A 2 0.392301 0.549006 0.530059 11.00000 51.00000 H12B 2 0.246146 0.534100 0.579726 11.00000 51.00000 H12C 2 0.325529 0.416032 0.589187 11.00000 51.00000 AFIX 0 HKLF 4 REM 12srv051 in P-1 REM R1 = 0.0246 for 6162 Fo > 4sig(Fo) and 0.0269 for all 6611 data REM 171 parameters refined using 0 restraints END WGHT 0.0000 3.3997 REM Highest difference peak 1.464, deepest hole -1.843, 1-sigma level 0.166 Q1 1 0.6553 0.3613 0.9026 11.00000 0.05 1.46 Q2 1 0.2755 0.3914 0.6348 11.00000 0.05 1.42 Q3 1 0.6479 1.0311 0.6305 11.00000 0.05 1.41 Q4 1 0.7197 0.9254 0.6317 11.00000 0.05 1.30 Q5 1 0.7053 1.0272 0.7118 11.00000 0.05 1.20 Q6 1 0.6625 0.9401 0.5589 11.00000 0.05 1.17 ; _shelx_res_checksum 51557 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 0.68667(2) 0.98606(2) 0.63470(2) 0.01600(3) Uani 1 1 d . Cl1 Cl 0.39505(10) 0.82282(9) 0.48354(9) 0.01783(13) Uani 1 1 d . Cl2 Cl 0.62041(11) 1.10744(10) 0.81914(9) 0.02257(15) Uani 1 1 d . Cl3 Cl 0.94359(11) 1.19825(11) 0.74232(11) 0.02601(16) Uani 1 1 d . Cl4 Cl 0.71550(11) 0.88557(10) 0.41692(9) 0.02236(15) Uani 1 1 d . N N 0.7229(3) 0.8532(3) 0.7024(3) 0.0162(5) Uani 1 1 d . C1 C 0.7541(4) 0.7459(4) 0.7549(3) 0.0152(5) Uani 1 1 d . C2 C 0.9052(4) 0.7425(4) 0.7722(4) 0.0171(5) Uani 1 1 d . C3 C 0.9327(4) 0.6333(4) 0.8259(4) 0.0210(6) Uani 1 1 d . H3 H 1.0325 0.6281 0.8405 0.025 Uiso 1 1 calc R C4 C 0.8197(4) 0.5332(4) 0.8582(4) 0.0218(6) Uani 1 1 d . H4 H 0.8427 0.4610 0.8949 0.026 Uiso 1 1 calc R C5 C 0.6720(4) 0.5377(4) 0.8373(4) 0.0199(6) Uani 1 1 d . H5 H 0.5939 0.4660 0.8574 0.024 Uiso 1 1 calc R C6 C 0.6362(4) 0.6449(4) 0.7874(4) 0.0165(5) Uani 1 1 d . C7 C 1.0306(4) 0.8532(4) 0.7393(4) 0.0191(6) Uani 1 1 d . H7 H 0.9719 0.8821 0.6630 0.023 Uiso 1 1 calc R C8 C 1.1513(5) 1.0083(5) 0.8811(4) 0.0271(7) Uani 1 1 d . H8A H 1.0906 1.0581 0.9202 0.035(8) Uiso 1 1 calc GR H8B H 1.2276 1.0829 0.8573 0.035(8) Uiso 1 1 calc GR H8C H 1.2128 0.9832 0.9565 0.035(8) Uiso 1 1 calc GR C9 C 1.1243(6) 0.7753(5) 0.6765(6) 0.0338(9) Uani 1 1 d . H9A H 1.1848 0.7480 0.7506 0.036(8) Uiso 1 1 calc GR H9B H 1.2014 0.8505 0.6539 0.036(8) Uiso 1 1 calc GR H9C H 1.0467 0.6773 0.5849 0.036(8) Uiso 1 1 calc GR C10 C 0.4730(4) 0.6455(4) 0.7605(4) 0.0175(5) Uani 1 1 d . H10 H 0.4884 0.7553 0.7717 0.021 Uiso 1 1 calc R C11 C 0.4077(5) 0.6064(5) 0.8724(5) 0.0268(7) Uani 1 1 d . H11A H 0.3833 0.4958 0.8576 0.032(8) Uiso 1 1 calc GR H11B H 0.3075 0.6177 0.8565 0.032(8) Uiso 1 1 calc GR H11C H 0.4906 0.6807 0.9745 0.032(8) Uiso 1 1 calc GR C12 C 0.3480(4) 0.5253(4) 0.6005(4) 0.0229(6) Uani 1 1 d . H12A H 0.3923 0.5490 0.5301 0.027(7) Uiso 1 1 calc GR H12B H 0.2461 0.5341 0.5797 0.027(7) Uiso 1 1 calc GR H12C H 0.3255 0.4160 0.5892 0.027(7) Uiso 1 1 calc 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 0.02153(6) 0.01714(5) 0.01815(6) 0.01160(4) 0.01047(4) 0.01320(5) Cl1 0.0226(3) 0.0182(3) 0.0212(3) 0.0131(3) 0.0111(3) 0.0133(3) Cl2 0.0346(4) 0.0250(4) 0.0193(3) 0.0120(3) 0.0143(3) 0.0211(3) Cl3 0.0235(4) 0.0222(4) 0.0341(4) 0.0158(3) 0.0096(3) 0.0114(3) Cl4 0.0337(4) 0.0263(4) 0.0249(4) 0.0174(3) 0.0195(3) 0.0216(3) N 0.0207(12) 0.0192(11) 0.0171(11) 0.0110(9) 0.0106(10) 0.0133(10) C1 0.0188(13) 0.0195(13) 0.0160(12) 0.0105(10) 0.0095(10) 0.0137(11) C2 0.0198(14) 0.0185(13) 0.0198(13) 0.0121(11) 0.0096(11) 0.0120(11) C3 0.0215(15) 0.0234(15) 0.0299(16) 0.0183(13) 0.0134(13) 0.0152(13) C4 0.0261(16) 0.0248(15) 0.0274(16) 0.0187(13) 0.0132(13) 0.0178(14) C5 0.0236(15) 0.0206(14) 0.0252(15) 0.0158(12) 0.0133(12) 0.0130(12) C6 0.0202(14) 0.0174(13) 0.0188(13) 0.0104(11) 0.0099(11) 0.0122(11) C7 0.0217(14) 0.0208(14) 0.0239(14) 0.0137(12) 0.0128(12) 0.0136(12) C8 0.0234(16) 0.0272(17) 0.0266(17) 0.0145(14) 0.0080(14) 0.0070(14) C9 0.039(2) 0.033(2) 0.060(3) 0.031(2) 0.038(2) 0.0267(18) C10 0.0194(14) 0.0190(13) 0.0198(13) 0.0107(11) 0.0104(11) 0.0112(11) C11 0.0264(17) 0.037(2) 0.0322(18) 0.0221(16) 0.0195(15) 0.0185(16) C12 0.0240(16) 0.0221(15) 0.0239(15) 0.0112(12) 0.0077(13) 0.0129(13) 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_ _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 Cl1 77.24(3) 2_676 Cl2 W Cl1 83.01(3) 2_676 Cl2 W Cl1 86.57(3) . Cl2 W Cl4 166.21(3) . Cl3 W Cl1 159.92(3) . Cl3 W Cl1 82.70(3) 2_676 Cl3 W Cl2 91.81(4) . Cl3 W Cl4 91.10(4) . Cl4 W Cl1 83.99(3) 2_676 Cl4 W Cl1 86.08(3) . N W Cl1 98.31(10) . N W Cl1 175.54(10) 2_676 N W Cl2 96.85(9) . N W Cl3 101.76(10) . N W Cl4 95.75(9) . W Cl1 W 102.76(3) 2_676 C1 N W 178.6(2) . N C1 C2 117.7(3) . N C1 C6 119.3(3) . C6 C1 C2 122.9(3) . C1 C2 C7 122.1(3) . C3 C2 C1 116.1(3) . C3 C2 C7 121.8(3) . C4 C3 C2 122.2(3) . C3 C4 C5 120.1(3) . C6 C5 C4 121.5(3) . C1 C6 C10 121.7(3) . C5 C6 C1 117.1(3) . C5 C6 C10 121.1(3) . C2 C7 C8 109.9(3) . C2 C7 C9 112.7(3) . C9 C7 C8 109.9(3) . C6 C10 C11 112.4(3) . C6 C10 C12 109.6(3) . C12 C10 C11 110.1(3) . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 W Cl1 2.7119(7) 2_676 W Cl1 2.4168(9) . W Cl2 2.3163(8) . W Cl3 2.2858(10) . W Cl4 2.3175(8) . W N 1.727(3) . Cl1 W 2.7118(7) 2_676 N C1 1.390(4) . C1 C2 1.424(4) . C1 C6 1.412(4) . C2 C3 1.400(4) . C2 C7 1.507(5) . C3 C4 1.377(5) . C4 C5 1.392(5) . C5 C6 1.390(4) . C6 C10 1.516(4) . C7 C8 1.533(5) . C7 C9 1.529(5) . C10 C11 1.535(5) . C10 C12 1.532(5) .