Bis(Imido) Tungsten Complexes: Efficient Precatalysts for the Homogeneous Dimerization of Ethylene
Messinis, Antonis M.; Batsanov, Andrei S.; Wright, William R. H.; Howard, Judith A. K.; Hanton, Martin J.; Dyer, Philip W.; ACS Catalysis 8 (2018) 11249–; doi:10.1021/acscatal.8b02202

data_4515801
_publ_section_title
;
 Bis(Imido) Tungsten Complexes: Efficient Precatalysts for the Homogeneous
 Dimerization of Ethylene
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              11249
_journal_paper_doi               10.1021/acscatal.8b02202
_journal_volume                  8
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H44 Cl2 N4 W'
_chemical_formula_sum            'C34 H44 Cl2 N4 W'
_chemical_formula_weight         763.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8622(9)
_cell_length_b                   17.5716(13)
_cell_length_c                   19.3465(16)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.32
_cell_volume                     3352.6(5)
_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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39577
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        29.992
_diffrn_reflns_theta_max         29.992
_diffrn_reflns_theta_min         1.566
_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    3.633
_exptl_absorpt_correction_T_max  0.9174
_exptl_absorpt_correction_T_min  0.5257
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2010) was used for absorption correction.
wR2(int) was 0.0858 before and 0.0709 after correction.
The Ratio of minimum to maximum transmission is 0.5730.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.248
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 3402 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack, 2004). By classical hole-in-one fit 
 to all intensities, x=-0.004(8). Hooft parameter y = -0.007(5).
;
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         9510
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0595
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                8357
_reflns_number_total             9510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            W-bisimido.cif
_cod_data_source_block           5_11srv263
_cod_database_code               4515801
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.530
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22A-C20 \\sim C22B-C20
 with sigma of 0.01
 C21B-C20 \\sim C21A-C20
 with sigma of 0.01
3. Others
 Uiso(H18A)=Uiso(H18B)=Uiso(H18C)=FVAR(1)
 Uiso(H19A)=Uiso(H19B)=Uiso(H19C)=FVAR(2)
 Uiso(H21A)=Uiso(H21B)=Uiso(H21C)=Uiso(H21D)=Uiso(H21E)=Uiso(H21F)=FVAR(3)
 Uiso(H34A)=Uiso(H34B)=Uiso(H34C)=FVAR(4)
 Uiso(H30A)=Uiso(H30B)=Uiso(H30C)=FVAR(5)
 Uiso(H31A)=Uiso(H31B)=Uiso(H31C)=FVAR(6)
 Fixed Sof: H20(0.67) H20A(0.33) C21A(0.67) H21A(0.67) H21B(0.67) H21C(0.67)
 C22A(0.67) H22A(0.67) H22B(0.67) H22C(0.67) C21B(0.33) H21D(0.33) H21E(0.33)
 H21F(0.33) C22B(0.33) H22D(0.33) H22E(0.33) H22F(0.33)
4.a Riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C13(H13), C14(H14), C15(H15), C17(H17), C20(H20), C20(H20A),
 C25(H25), C26(H26), C27(H27), C29(H29), C32(H32)
4.b Rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21A(H21A,H21B,H21C), C22A(H22A,
 H22B,H22C), C21B(H21D,H21E,H21F), C22B(H22D,H22E,H22F), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              36885
_shelx_hkl_checksum              3212