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_4515810
_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         'C22 H29 Cl5 N2 O2 W, C6 H6'
_chemical_formula_sum            'C28 H35 Cl5 N2 O2 W'
_chemical_formula_weight         792.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-11-08
_audit_creation_method
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Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
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_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1544(12)
_cell_length_b                   10.4027(11)
_cell_length_c                   24.447(2)
_cell_measurement_reflns_used    24097
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.1920
_cell_measurement_theta_min      2.5660
_cell_volume                     3090.6(5)
_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
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 CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 
 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54)
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_computing_data_reduction
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 CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 
 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54)
;
_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 16.1511
_diffrn_detector_type            'Sapphire3 CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device
'Agilent Technologies, Gemini S Ultra kappa-diffractometer'
_diffrn_measurement_device_type  Gemini
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0091325000
_diffrn_orient_matrix_UB_12      0.0638595000
_diffrn_orient_matrix_UB_13      -0.0090166000
_diffrn_orient_matrix_UB_21      -0.0020461000
_diffrn_orient_matrix_UB_22      0.0219960000
_diffrn_orient_matrix_UB_23      0.0274313000
_diffrn_orient_matrix_UB_31      0.0576037000
_diffrn_orient_matrix_UB_32      -0.0093507000
_diffrn_orient_matrix_UB_33      0.0029056000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       17
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_diffrn_reflns_number            48940
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.930
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_diffrn_reflns_theta_max         32.265
_diffrn_reflns_theta_min         2.571
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    4.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59903
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.2007
_exptl_crystal_size_mid          0.1734
_exptl_crystal_size_min          0.0561
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         10201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0180
_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^)+(0.0149P)^2^+1.6001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0387
_refine_ls_wR_factor_ref         0.0396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9560
_reflns_number_total             10201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            W-bisimido.cif
_cod_data_source_block           14_11srv228
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' 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_database_code               4515810
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Uiso(H4A)=Uiso(H4B)=Uiso(H4C)=FVAR(1)
 Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(2)
 Uiso(H18A)=Uiso(H18B)=Uiso(H18C)=FVAR(3)
 Uiso(H19A)=Uiso(H19B)=Uiso(H19C)=FVAR(4)
 Uiso(H21A)=Uiso(H21B)=Uiso(H21C)=FVAR(5)
 Uiso(H22A)=Uiso(H22B)=Uiso(H22C)=FVAR(6)
3.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28)
3.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              36074
_shelx_hkl_checksum              10463
_olex2_submission_special_instructions 'No special instructions were received'