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_4515805
_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         'C22 H14 Cl2 F18 N2 O2 W'
_chemical_formula_sum            'C22 H14 Cl2 F18 N2 O2 W'
_chemical_formula_weight         935.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 105.516(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5254(6)
_cell_length_b                   27.3985(15)
_cell_length_c                   9.0867(5)
_cell_measurement_reflns_used    9790
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.76
_cell_measurement_theta_min      2.44
_cell_volume                     3004.7(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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            56012
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.125
_diffrn_reflns_theta_min         1.486
_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    4.160
_exptl_absorpt_correction_T_max  0.4874
_exptl_absorpt_correction_T_min  0.4073
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
 SADABS-2009/1 (Bruker,2010) was used for absorption correction. 
 wR2(int) was 0.0697 before and 0.0457 after correction. The Ratio 
 of minimum to maximum transmission is 0.8357. The \l/2 correction 
 factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         10835
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0130P)^2^+2.9820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9928
_reflns_number_total             10835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            W-bisimido.cif
_cod_data_source_block           9_12srv094
_cod_database_code               4515805
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.475
_shelx_estimated_absorpt_t_min   0.435
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F13A-C21 \\sim F13C-C21 \\sim F14B-C21 \\sim F15A-C21 \\sim F15C-C21 \\sim
F13B-C21 \\sim F14A-C21 ~
 F14C-C21 \\sim F15B-C21
 with sigma of 0.02
 F5B-C18B \\sim F6B-C18B \\sim F4B-C18B \\sim F6A-C18A \\sim F5A-C18A \\sim
F4A-C18A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F15A) = Uanis(F15B)
Uanis(F13B) = Uanis(F13A)
Uanis(F14B) = Uanis(F14A)
4. Others
 Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(1)
 Uiso(H4A)=Uiso(H4B)=Uiso(H4C)=FVAR(2)
 Fixed Sof: F4A(0.5) F5A(0.5) F6A(0.5) F4B(0.5) F5B(0.5) F6B(0.5) F13A(0.15)
 F14A(0.15) F15A(0.15) F13B(0.6) F14B(0.6) F15B(0.6) F13C(0.25) F14C(0.25)
 F15C(0.25) C18A(0.5) C18B(0.5)
5.a Rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C13(H13), C15(H15)
;
_shelx_res_checksum              12139
_shelx_hkl_checksum              84018