Exploration of Homogeneous Ethylene Dimerization Mediated by Tungsten Mono(imido) Complexes
Messinis, Antonis M.; Wright, William R. H.; Batsanov, Andrei S.; Howard, Judith A. K.; Hanton, Martin J.; Dyer, Philip W.; ACS Catalysis 8 (2018) 11235–; doi:10.1021/acscatal.8b02201

data_4515785
_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         'C16 H25 Cl4 N O W'
_chemical_formula_sum            'C16 H25 Cl4 N O W'
_chemical_formula_weight         573.02
_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                95.674(10)
_cell_angle_beta                 98.423(9)
_cell_angle_gamma                97.281(9)
_cell_formula_units_Z            4
_cell_length_a                   8.5798(7)
_cell_length_b                   14.0708(10)
_cell_length_c                   17.3875(14)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.58
_cell_measurement_theta_min      2.39
_cell_volume                     2044.9(3)
_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      120.0
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47614
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        32.500
_diffrn_reflns_theta_max         34.987
_diffrn_reflns_theta_min         1.192
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.174
_exptl_absorpt_correction_T_max  0.8004
_exptl_absorpt_correction_T_min  0.3666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0568 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.4580.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       blade
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.136
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         17049
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.8250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13303
_reflns_number_total             17049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02201_si_002.cif
_cod_data_source_block           2g
_cod_database_code               4515785
_ccdc_comments                   'redetermination of XAKNAB, CCDC-1434397'
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.319
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C23A-C24 \\sim C23B-C24 \\sim C26B-C25B \\sim C26A-C25A \\sim C25A-C24 \\sim
C25B-C24
 with sigma of 0.02
 O2-C23A \\sim O2-C23B \\sim O2-C26B \\sim O2-C26A
 with sigma of 0.02
3. Others
 Uiso(H12A)=Uiso(H12B)=Uiso(H12C)=FVAR(1)
 Uiso(H13A)=Uiso(H13B)=Uiso(H13C)=FVAR(2)
 Uiso(H15A)=Uiso(H15B)=Uiso(H15C)=FVAR(3)
 Uiso(H16A)=Uiso(H16B)=Uiso(H16C)=FVAR(4)
 Uiso(H28A)=Uiso(H28B)=Uiso(H28C)=FVAR(5)
 Uiso(H29A)=Uiso(H29B)=Uiso(H29C)=FVAR(6)
 Uiso(H31A)=Uiso(H31B)=Uiso(H31C)=FVAR(7)
 Uiso(H32A)=Uiso(H32B)=Uiso(H32C)=FVAR(8)
 Fixed Sof: C23A(0.667) H23A(0.667) H23B(0.667) C23B(0.333) H23C(0.333)
 H23D(0.333) H24A(0.667) H24B(0.667) H24C(0.333) H24D(0.333) C25A(0.667)
 H25A(0.667) H25B(0.667) C25B(0.333) H25C(0.333) H25D(0.333) C26A(0.667)
 H26A(0.667) H26B(0.667) C26B(0.333) H26C(0.333) H26D(0.333)
4.a Riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B),
  C11(H11), C14(H14), C19(H19), C20(H20), C21(H21), C23A(H23A,H23B), C23B(H23C,
 H23D), C24(H24A,H24B), C24(H24C,H24D), C25A(H25A,H25B), C25B(H25C,H25D),
 C26A(H26A,H26B), C26B(H26C,H26D), C27(H27), C30(H30)
4.b Rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
;
_shelx_res_checksum              32543