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_4515808
_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_formula_moiety         'C20 H36 Cl2 N2 O2 W'
_chemical_formula_sum            'C20 H36 Cl2 N2 O2 W'
_chemical_formula_weight         591.26
_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             2017-11-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                70.528(8)
_cell_angle_beta                 85.509(8)
_cell_angle_gamma                71.846(8)
_cell_formula_units_Z            2
_cell_length_a                   9.8343(6)
_cell_length_b                   9.9604(6)
_cell_length_c                   13.7645(8)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.26
_cell_measurement_theta_min      2.18
_cell_volume                     1207.40(15)
_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(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 6000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.095726
_diffrn_orient_matrix_UB_12      0.010602
_diffrn_orient_matrix_UB_13      -0.024944
_diffrn_orient_matrix_UB_21      -0.028286
_diffrn_orient_matrix_UB_22      0.011550
_diffrn_orient_matrix_UB_23      -0.071332
_diffrn_orient_matrix_UB_31      -0.039224
_diffrn_orient_matrix_UB_32      0.110797
_diffrn_orient_matrix_UB_33      -0.014882
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21874
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         1.570
_diffrn_source                   'fine-focus sealed 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    5.021
_exptl_absorpt_correction_T_max  0.6710
_exptl_absorpt_correction_T_min  0.3625
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
 SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
 wR2(int) was 0.0650 before and 0.0496 after correction. The Ratio 
 of minimum to maximum transmission is 0.5402. The \l/2 correction 
 factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.720
_refine_diff_density_min         -1.704
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         7040
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0350P)^2^+1.7260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6447
_reflns_number_total             7040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            W-bisimido.cif
_cod_data_source_block           12_11srv013
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_source_target' value 'MO' was changed to 'Mo' 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_database_code               4515808
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 W, N1, C5, C7, C6, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Uiso(H17A)=Uiso(H17B)=Uiso(H17C)=FVAR(1)
 Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(2)
 Uiso(H19A)=Uiso(H19B)=Uiso(H19C)=FVAR(3)
 Uiso(H4A)=Uiso(H4B)=Uiso(H4C)=FVAR(4)
 Uiso(H7A)=Uiso(H7B)=Uiso(H7C)=FVAR(5)
 Uiso(H16A)=Uiso(H16B)=Uiso(H16C)=FVAR(6)
 Uiso(H20A)=Uiso(H20B)=Uiso(H20C)=FVAR(7)
 Uiso(H8A)=Uiso(H8B)=Uiso(H8C)=FVAR(8)
 Uiso(H6A)=Uiso(H6B)=Uiso(H6C)=FVAR(9)
4.a Riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11), C12(H12), C13(H13), C15(H15), C18(H18)
4.b Rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C6(H6A,H6B,H6C),
  C8(H8A,H8B,H8C)
;
_shelx_res_checksum              78661
_shelx_hkl_checksum              6459