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_4515788
_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         'C9 H14 Cl N W'
_chemical_formula_sum            'C9 H14 Cl N W'
_chemical_formula_weight         355.51
_chemical_name_systematic        '(phenylimido)trimethyl tungsten chloride'
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_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                 93.604(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3483(10)
_cell_length_b                   7.2804(11)
_cell_length_c                   11.9671(18)
_cell_measurement_reflns_used    6012
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      2.80
_cell_volume                     552.00(15)
_computing_cell_refinement       'SAINT version 6.45A (Bruker, 2003)'
_computing_data_collection       'SMART version 5.049 (Bruker, 1998)'
_computing_data_reduction        'SAINT version 6.45A (Bruker, 2003)'
_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 7.9
_diffrn_detector_type            'Bruker SMART CCD 1000 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K 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  0.0238
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6554
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.008
_diffrn_reflns_theta_min         1.705
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    10.656
_exptl_absorpt_correction_T_max  0.2932
_exptl_absorpt_correction_T_min  0.0797
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; SADABS 2009-1 (Bruker, 2009) was used for absorption correction. 
 R(int) was 0.159 before and 0.0236 after correction. 
 The \l/2 correction factor is 0.0015
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0069(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.323
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0152
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+1.2380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1543
_reflns_number_total             1572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02201_si_002.cif
_cod_data_source_block           6b
_cod_database_code               4515788
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Uiso(H13)=Uiso(H11)=Uiso(H12)=FVAR(1)
 Uiso(H21)=Uiso(H22)=FVAR(2)
 Fixed Sof: C3(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C7(0.5)
 H7(0.5) C8(0.5) H8(0.5)
3.a Riding coordinates:
 C2(H21,H22), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
3.b Rotating group:
 C1(H13,H11,H12)
;
_shelx_res_checksum              17116