Selective ethylene oligomerisation using supported tungsten mono-imido catalysts
Wright, Christopher M. R.; Williams, Thomas J.; Turner, Zoë R.; Buffet, Jean-Charles; O'Hare, Dermot; Inorganic Chemistry Frontiers 4 (2017) 1048–; doi:10.1039/C7QI00128B

data_4349699
_publ_section_title
;
 Selective ethylene oligomerisation using supported tungsten mono-imido
 catalysts
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1048
_journal_paper_doi               10.1039/C7QI00128B
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C10 H11 Cl4 F2 N O W'
_chemical_formula_sum            'C10 H11 Cl4 F2 N O W'
_chemical_formula_weight         524.85
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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
_audit_block_doi                 10.5517/ccdc.csd.cc1mzdnn
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-23 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                87.462(2)
_cell_angle_beta                 86.122(2)
_cell_angle_gamma                79.773(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1651(2)
_cell_length_b                   9.4012(3)
_cell_length_c                   9.9731(3)
_cell_measurement_reflns_used    12717
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.2240
_cell_measurement_theta_min      3.7990
_cell_volume                     751.26(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
Ortep III for windows
L. J. Farrugia, J. Appl. Crystallogr., 1997, 30, 565.
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
;
Superflip L. Palatinus and G. Chapuis,  
J. Appl. Crystallogr., 2007, 40, 786-790.
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15868
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.958
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.410
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0156
_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^)+(0.0188P)^2^+0.3739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0379
_refine_ls_wR_factor_ref         0.0385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3325
_reflns_number_total             3447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00128b2.cif
_cod_data_source_block           032zrt16
_cod_database_code               4349699
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.266
_shelx_estimated_absorpt_t_max   0.499
_shelx_res_checksum              17122