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_4515809
_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_formula_moiety
'C25 H38 Cl2 N2 O2 W, 0.375(C6 H14), 0.25(C H2 Cl2)'
_chemical_formula_sum            'C27.5 H43.75 Cl2.5 N2 O2 W'
_chemical_formula_weight         706.87
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-11-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                112.357(9)
_cell_angle_beta                 90.965(9)
_cell_angle_gamma                99.035(9)
_cell_formula_units_Z            2
_cell_length_a                   9.0974(5)
_cell_length_b                   12.8175(8)
_cell_length_c                   14.1008(10)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.27
_cell_volume                     1496.5(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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 6000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27439
_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         30.002
_diffrn_reflns_theta_min         1.567
_diffrn_source                   'fine-focus sealed 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    4.109
_exptl_absorpt_correction_T_max  0.8468
_exptl_absorpt_correction_T_min  0.4978
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
 SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) 
 was 0.0554 before and 0.0458 after correction. The Ratio of minimum to maximum 
 transmission is 0.5879. The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.693
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         8717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.2143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7801
_reflns_number_total             8717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            W-bisimido.cif
_cod_data_source_block           13_11srv151
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_source_target' value 'MO' was changed to 'Mo' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1496.49(19)
_cod_original_formula_sum        'C27.50 H43.75 Cl2.50 N2 O2 W'
_cod_database_code               4515809
_shelx_shelxl_version_number     2016/6
_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
2. Others
 Uiso(H13A)=Uiso(H13B)=Uiso(H13C)=FVAR(1)
 Uiso(H24A)=Uiso(H24B)=Uiso(H24C)=FVAR(2)
 Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(3)
 Uiso(H25A)=Uiso(H25B)=Uiso(H25C)=FVAR(4)
 Uiso(H4A)=Uiso(H4B)=Uiso(H4C)=FVAR(5)
 Uiso(H11A)=Uiso(H11B)=Uiso(H11C)=FVAR(6)
 Uiso(H12A)=Uiso(H12B)=Uiso(H12C)=FVAR(7)
 Uiso(H22A)=Uiso(H22B)=Uiso(H22C)=FVAR(8)
 Uiso(H21A)=Uiso(H21B)=Uiso(H21C)=FVAR(9)
 Fixed Sof: C27(0.75) H27A(0.75) H27B(0.75) H27C(0.75) C28(0.75) H28A(0.75)
 H28B(0.75) C29(0.75) H29A(0.75) H29B(0.75) Cl3(0.25) Cl4(0.25) C26(0.25)
 H26A(0.25) H26B(0.25)
3.a Riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C7(H7), C9(H9), C16(H16), C17(H17), C18(H18),
 C20(H20), C23(H23), C27(H27A,H27B,H27C)
3.b Rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
3.c Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C26(H26A,H26B)
;
_shelx_res_checksum              72303
_shelx_hkl_checksum              34233
_olex2_submission_special_instructions 'No special instructions were received'