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_4515786
_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         'C24 H34 Cl7 N2 W2 1-,C8 H20 N 1+'
_chemical_formula_sum            'C32 H54 Cl7 N3 W2'
_chemical_formula_weight         1096.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5696(3)
_cell_length_b                   10.7140(3)
_cell_length_c                   40.8756(12)
_cell_measurement_reflns_used    9187
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.75
_cell_volume                     4190.9(2)
_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 2014/7 multi-CPU version (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS 2013/1 (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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       'narrow-frame \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            50787
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         1.993
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.956
_exptl_absorpt_correction_T_max  0.6686
_exptl_absorpt_correction_T_min  0.1473
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker, 2010) was used for absorption correction.
wR2(int) was 0.0617 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.2203.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.366
_refine_diff_density_min         -3.684
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5565
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0926
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+92.2660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4705
_reflns_number_total             5565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02201_si_002.cif
_cod_data_source_block           3
_cod_database_code               4515786
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.199
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C14-C13
 1.5 with sigma of 0.02
 C5-C4B \\sim C5-C4A \\sim C6B-C5 \\sim C6A-C5
 with sigma of 0.02
 C16-C15B \\sim C16-C15A
 with sigma of 0.02
 N2-C15B \\sim N2-C15A \\sim N2-C13
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(1)
 Uiso(H3A)=Uiso(H3B)=Uiso(H3C)=FVAR(2)
 Uiso(H4AA)=Uiso(H4AB)=Uiso(H4AC)=FVAR(3)
 Fixed Sof: H5A(0.67) H5B(0.33) C4A(0.67) H4AA(0.67) H4AB(0.67) H4AC(0.67)
 C6A(0.67) H6AA(0.67) H6AB(0.67) H6AC(0.67) C4B(0.33) H4BA(0.33) H4BB(0.33)
 H4BC(0.33) C6B(0.33) H6BA(0.33) H6BB(0.33) H6BC(0.33) C15A(0.5) H15A(0.5)
 H15B(0.5) C15B(0.5) H15C(0.5) H15D(0.5) H16A(0.5) H16B(0.5) H16C(0.5)
 H16E(0.5) H16F(0.5) H16D(0.5)
5.a Riding coordinates:
 C5(H5A,H5B), C4B(H4BA,H4BB,H4BC), C6B(H6BA,H6BB,H6BC), C13(H13A,H13B),
 C15A(H15A,H15B), C15B(H15C,H15D), C16(H16A,H16B,H16C,H16E,H16F,H16D)
5.b Rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4A(H4AA,H4AB,H4AC), C6A(H6AA,H6AB,H6AC)
5.c Ternary CH refined with riding coordinates:
 C2(H2)
5.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11)
5.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              25333