#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:47:08 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515780.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_4515780 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 'C4 H10 Cl8 N2 W2' _chemical_formula_sum 'C4 H10 Cl8 N2 W2' _chemical_formula_weight 737.44 _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 2012-07-28 _audit_creation_method ; Olex2 1.2-alpha (compiled 2012.07.25 svn.r2431, GUI svn.r4294) ; _cell_angle_alpha 97.754(3) _cell_angle_beta 108.946(3) _cell_angle_gamma 112.350(4) _cell_formula_units_Z 1 _cell_length_a 7.7134(3) _cell_length_b 7.8170(3) _cell_length_c 7.9908(3) _cell_measurement_reflns_used 4387 _cell_measurement_temperature 120 _cell_measurement_theta_max 32.2798 _cell_measurement_theta_min 2.8153 _cell_volume 402.67(3) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET) (compiled Apr 6 2011,09:17:13) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET) (compiled Apr 6 2011,09:17:13) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET) (compiled Apr 6 2011,09:17:13) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 16.1511 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.925 _diffrn_measurement_device 'Agilent Technologies, Gemini S Ultra kappa-diffractometer' _diffrn_measurement_device_type 'Sapphire3 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0389031000 _diffrn_orient_matrix_UB_12 -0.0418026000 _diffrn_orient_matrix_UB_13 0.0615255000 _diffrn_orient_matrix_UB_21 0.0129479000 _diffrn_orient_matrix_UB_22 0.0910885000 _diffrn_orient_matrix_UB_23 0.0458867000 _diffrn_orient_matrix_UB_31 -0.1010207000 _diffrn_orient_matrix_UB_32 -0.0223753000 _diffrn_orient_matrix_UB_33 -0.0613066000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 10156 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 32.35 _diffrn_reflns_theta_min 2.82 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 15.575 _exptl_absorpt_correction_T_max 0.4345 _exptl_absorpt_correction_T_min 0.3540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2009/1, R(int)=0.1296 before correction ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 3.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 332 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.2 _refine_diff_density_max 2.359 _refine_diff_density_min -1.557 _refine_diff_density_rms 0.253 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 74 _refine_ls_number_reflns 2654 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.117 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0300 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.1107P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.0665 _reflns_number_gt 2463 _reflns_number_total 2654 _reflns_threshold_expression I>2\s(I) _cod_data_source_file cs8b02201_si_002.cif _cod_data_source_block 1a _cod_database_code 4515780 _ccdc_comments 'redetermination of SEPHAW' _shelx_res_file ; TITL 12SRV133 in P-1 #2 CELL 0.71073 7.71338 7.817013 7.990791 97.7544 108.9457 112.35 ZERR 1 0.000298 0.000297 0.000281 0.003 0.0034 0.0036 LATT 1 SFAC C H N Cl W UNIT 4 10 2 8 2 L.S. 7 0 0 511 PLAN 7 TEMP -153.15 REM reset to P-1 #2 BOND $H REM OMIT -3 60 fmap 2 acta 60 OMIT 1 0 0 OMIT 0 -4 5 OMIT -2 4 2 OMIT -6 4 2 OMIT -4 4 4 OMIT -4 4 2 REM I:/andrei/datasets/12srv133/12SRV133.hkl WGHT 0.027000 0.110700 FVAR 0.46034 W 5 0.238503 0.404996 0.273913 11.00000 0.01614 0.01513 = 0.01780 0.00775 0.00810 0.00748 CL1 4 0.345480 0.415826 0.599473 11.00000 0.01837 0.01780 = 0.01815 0.00918 0.00960 0.00782 CL2 4 0.284599 0.716938 0.369659 11.00000 0.02234 0.01699 = 0.02512 0.00927 0.01060 0.01053 CL3 4 0.233800 0.437506 -0.007075 11.00000 0.02732 0.02776 = 0.01978 0.01190 0.01196 0.01500 CL4 4 0.282368 0.128135 0.224532 11.00000 0.02505 0.01666 = 0.02421 0.00587 0.00877 0.01131 N 3 -0.017031 0.289529 0.222832 11.00000 0.01890 0.01701 = 0.01985 0.00740 0.00886 0.00899 C1 1 -0.226595 0.184490 0.196064 11.00000 0.01658 0.01806 = 0.02825 0.01037 0.01067 0.00773 AFIX 23 H1A 2 -0.317980 0.146181 0.063306 11.00000 -1.20000 H1B 2 -0.263691 0.268273 0.267035 11.00000 -1.20000 AFIX 0 C2 1 -0.256683 0.004366 0.260380 11.00000 0.02922 0.02183 = 0.03572 0.01295 0.01789 0.00928 AFIX 137 H2A 2 -0.214490 -0.075721 0.193575 11.00000 -1.50000 H2B 2 -0.401918 -0.069984 0.235265 11.00000 -1.50000 H2C 2 -0.172980 0.043030 0.393638 11.00000 -1.50000 HKLF 4 REM 12SRV133 in P-1 #2 REM R1 = 0.0300 for 2463 Fo > 4sig(Fo) and 0.0340 for all 2654 data REM 74 parameters refined using 0 restraints END WGHT 0.0270 0.1106 REM Highest difference peak 2.359, deepest hole -1.557, 1-sigma level 0.253 Q1 1 0.1852 0.3178 0.1727 11.00000 0.05 2.36 Q2 1 0.3041 0.4971 0.3805 11.00000 0.05 2.18 Q3 1 0.1202 0.2795 0.2378 11.00000 0.05 1.31 Q4 1 0.2458 -0.0944 0.2746 11.00000 0.05 1.26 Q5 1 0.2451 0.5443 0.3146 11.00000 0.05 1.25 Q6 1 0.2242 0.6372 0.2669 11.00000 0.05 1.21 Q7 1 0.2743 0.2747 0.2734 11.00000 0.05 1.07 REM The information below was added by Olex2. REM REM R1 = 0.0300 for 2463 Fo > 4sig(Fo) and n/a for all 10179 data REM n/a parameters refined using n/a restraints REM Highest difference peak 2.36, deepest hole -1.56 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = n/a REM R1_gt = 0.0300 REM wR_ref = 0.0665 REM GOOF = 1.117 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 10179 REM Reflections_gt = 2463 REM Parameters = n/a REM Hole = 2.36 REM Peak = -1.56 REM Flack = n/a ; loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags W W 0.23850(3) 0.40500(3) 0.27391(2) 0.01557(7) Uani 1 1 d . Cl1 Cl 0.34548(17) 0.41583(17) 0.59947(15) 0.0172(2) Uani 1 1 d . Cl2 Cl 0.28460(18) 0.71694(18) 0.36966(17) 0.0203(2) Uani 1 1 d . Cl3 Cl 0.23380(19) 0.4375(2) -0.00707(16) 0.0229(2) Uani 1 1 d . Cl4 Cl 0.28237(18) 0.12813(18) 0.22453(16) 0.0217(2) Uani 1 1 d . N N -0.0170(6) 0.2895(6) 0.2228(6) 0.0178(8) Uani 1 1 d . C1 C -0.2266(7) 0.1845(7) 0.1961(7) 0.0202(9) Uani 1 1 d . H1A H -0.3180 0.1462 0.0633 0.024 Uiso 1 1 calc R H1B H -0.2637 0.2683 0.2670 0.024 Uiso 1 1 calc R C2 C -0.2567(9) 0.0044(8) 0.2604(9) 0.0279(11) Uani 1 1 d . H2A H -0.2145 -0.0757 0.1936 0.042 Uiso 1 1 calc R H2B H -0.4019 -0.0700 0.2353 0.042 Uiso 1 1 calc R H2C H -0.1730 0.0430 0.3936 0.042 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 0.01614(10) 0.01513(11) 0.01780(10) 0.00775(7) 0.00810(7) 0.00748(7) Cl1 0.0184(5) 0.0178(5) 0.0181(5) 0.0092(4) 0.0096(4) 0.0078(4) Cl2 0.0223(5) 0.0170(6) 0.0251(5) 0.0093(4) 0.0106(4) 0.0105(4) Cl3 0.0273(6) 0.0278(6) 0.0198(5) 0.0119(5) 0.0120(5) 0.0150(5) Cl4 0.0250(6) 0.0167(5) 0.0242(5) 0.0059(4) 0.0088(5) 0.0113(5) N 0.0189(18) 0.017(2) 0.0198(18) 0.0074(16) 0.0089(15) 0.0090(16) C1 0.017(2) 0.018(2) 0.028(2) 0.010(2) 0.0107(19) 0.0077(18) C2 0.029(3) 0.022(3) 0.036(3) 0.013(2) 0.018(2) 0.009(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' N N 0.0061 0.0033 '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' 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 78.05(4) 2_666 Cl2 W Cl1 86.50(4) . Cl2 W Cl1 82.90(4) 2_666 Cl2 W Cl4 165.19(4) . Cl3 W Cl1 164.19(4) . Cl3 W Cl1 86.14(4) 2_666 Cl3 W Cl2 91.43(5) . Cl3 W Cl4 91.51(5) . Cl4 W Cl1 82.82(4) 2_666 Cl4 W Cl1 86.74(4) . N W Cl1 94.46(14) . N W Cl1 172.49(14) 2_666 N W Cl2 97.33(14) . N W Cl3 101.35(14) . N W Cl4 96.31(15) . W Cl1 W 101.95(4) 2_666 C1 N W 173.9(4) . N C1 H1A 109.6 . N C1 H1B 109.6 . N C1 C2 110.2(4) . H1A C1 H1B 108.1 . C2 C1 H1A 109.6 . C2 C1 H1B 109.6 . 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 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 W Cl1 2.7155(11) 2_666 W Cl1 2.4391(11) . W Cl2 2.3062(12) . W Cl3 2.2837(12) . W Cl4 2.3167(12) . W N 1.700(4) . Cl1 W 2.7154(11) 2_666 N C1 1.432(6) . C1 H1A 0.9900 . C1 H1B 0.9900 . C1 C2 1.525(8) . C2 H2A 0.9800 . C2 H2B 0.9800 . C2 H2C 0.9800 .