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_4515803
_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_absolute_configuration ad
_chemical_formula_moiety         'C16 H14 Cl2 F6 N2 O2 W'
_chemical_formula_sum            'C16 H14 Cl2 F6 N2 O2 W'
_chemical_formula_weight         635.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-10-27
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0005(5)
_cell_length_b                   12.4893(5)
_cell_length_c                   13.5857(6)
_cell_measurement_reflns_used    3873
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.506
_cell_measurement_theta_min      2.215
_cell_volume                     2036.20(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
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 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  0.0745
_diffrn_reflns_av_unetI/netI     0.0946
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25431
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         2.215
_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    6.004
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.2816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 5591 single and  11294 composite reflections used for parameter fitting.
 For component 1:
 wR2(int) was 0.0949 before and 0.0749 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.931
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.194
_refine_ls_abs_structure_details
;
 Flack x determined using 1853 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack, 2004). By classical hole-in-one fit to all 
 intensities, x= -0.003(14). Hooft parameter y = 0.013(6).
;
_refine_ls_abs_structure_Flack   0.022(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         25431
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0470P)^2^+4.0460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4308
_reflns_number_total             4692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            W-bisimido.cif
_cod_data_source_block           7_12srv022
_cod_database_code               4515803
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.509
_shelx_estimated_absorpt_t_min   0.352
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7838(14)
 0.2162(14)
2. 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
3. Restrained distances
 C5-C6 \\sim C7-C6 \\sim C7-C8 \\sim C9-C8 \\sim C9-C10 \\sim C5-C10
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C5, C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C13(H13), C15(H15)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_twin_special_details
;
 Twin components were deconvoluted using CELL_NOW 2008/4 (Sheldrick, 2008a). 
Twin law: rotation by 180\% about reciprocal axis [0 0.852 1] and real axis 
[0 1 0.989]. Integrated using SAINT V7.46A to generate a combined raw intensity
file in MUL file. Reduced using TWINABS 2012/1 to generate structure factors in 
HKLF5 format, from all observations involving domains 1 and 2:
     6368 data (   1984 unique ) involve domain  1 only,  mean I/sigma  14.8
     6470 data (   1995 unique ) involve domain  2 only,  mean I/sigma   6.7
    12979 data (   4559 unique ) involve   2 domains,  mean I/sigma  14.5
;
_shelx_res_checksum              77216
_shelx_hkl_checksum              66735
_olex2_submission_special_instructions 'No special instructions were received'