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_4515787
_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         'C21 H45 Cl N P3 W'
_chemical_formula_sum            'C21 H45 Cl N P3 W'
_chemical_formula_weight         623.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7347(5)
_cell_length_b                   13.6973(4)
_cell_length_c                   12.7686(4)
_cell_measurement_reflns_used    18327
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.3027
_cell_measurement_theta_min      2.5837
_cell_volume                     2751.93(15)
_computing_cell_refinement
; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 
(release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 
(release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (2011)'
_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_area_resol_mean 16.15
_diffrn_detector_type            'Sapphire3 CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
  1 omega  -98.00  -35.90   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -      -25.3968  -38.0000  -60.0000 207

  2 omega  -43.00   42.20   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -      -25.3968   38.0000  120.0000 284

  3 omega  -89.00  -62.00   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -      -25.3968 -162.0000  -64.0000 90

  4 omega   44.00   91.10   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -       26.1780 -138.0000 -170.0000 157

  5 omega   63.00   91.80   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -       26.1780 -162.0000  -64.0000 96

  6 omega  -38.00   19.00   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -       26.1780  -57.0000 -150.0000 190

  7 omega  -96.00    3.90   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -      -25.3968  -77.0000  150.0000 333

  8 omega  -98.00   -1.10   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -      -25.3968  -38.0000    0.0000 323

  9 omega  -94.00   -4.00   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -      -25.3968  -57.0000 -150.0000 300

 10 omega  -47.00   43.00   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -      -25.3968   57.0000  -60.0000 300

 11 omega   53.00  101.90   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -       26.1780 -179.0000   60.0000 163

 12 omega  -43.00   35.00   0.3000    2.6700
omega____ theta____ kappa____ phi______ frames
    -       26.1780  -57.0000    0.0000 260
;
_diffrn_measurement_device_type
'Agilent Technologies, Gemini S Ultra kappa-diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0054164000
_diffrn_orient_matrix_UB_12      -0.0287139000
_diffrn_orient_matrix_UB_13      -0.0395797000
_diffrn_orient_matrix_UB_21      0.0049671000
_diffrn_orient_matrix_UB_22      -0.0342011000
_diffrn_orient_matrix_UB_23      0.0333938000
_diffrn_orient_matrix_UB_31      -0.0550690000
_diffrn_orient_matrix_UB_32      -0.0060629000
_diffrn_orient_matrix_UB_33      -0.0008778000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51754
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.376
_diffrn_reflns_theta_min         2.974
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'greenish black'
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       brick
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.319
_exptl_crystal_size_min          0.313
_refine_diff_density_max         4.043
_refine_diff_density_min         -5.494
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.386
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         4846
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.368
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0545
_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^)+41.7180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4561
_reflns_number_total             4846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02201_si_002.cif
_cod_data_source_block           5
_cod_database_code               4515787
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All W(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14A) = Uanis(C14B)
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(H8A)=Uiso(H8B)=Uiso(H8C)=FVAR(1)
 Uiso(H10A)=Uiso(H10B)=Uiso(H10C)=FVAR(2)
 Fixed Sof: P2B(0.25) C11B(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C12B(0.5)
 H12A(0.5) H12B(0.5) H12C(0.5) C13B(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
 C14B(0.25) H14A(0.5) H14B(0.25) C15B(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
 P2A(0.25) C11A(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C12A(0.5) H12D(0.5)
 H12E(0.5) H12F(0.5) C13A(0.5) H13D(0.5) H13E(0.5) H13F(0.5) C14A(0.25)
 H14C(0.5) H14D(0.25) C15A(0.5) H15D(0.5) H15E(0.5) H15F(0.5)
5.a Riding coordinates:
 W(H0), C11B(H11A,H11B,H11C), C12B(H12A,H12B,H12C), C13B(H13A,H13B,H13C),
 C14B(H14A,H14B), C15B(H15A,H15B,H15C), C11A(H11D,H11E,H11F), C12A(H12D,H12E,
 H12F), C13A(H13D,H13E,H13F), C14A(H14C,H14D), C15A(H15D,H15E,H15F)
5.b Ternary CH refined with riding coordinates:
 C7(H7), C9(H9)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              43519