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_4515789
_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         'C15 H26 Al Cl4 N W'
_chemical_formula_sum            'C15 H26 Al Cl4 N W'
_chemical_formula_weight         573.00
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.616(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0824(5)
_cell_length_b                   16.3429(10)
_cell_length_c                   13.3029(7)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    120
_cell_measurement_theta_max      34.93
_cell_measurement_theta_min      2.38
_cell_volume                     2177.4(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 2014/7 multi-CPU version (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS 2013/1 (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 0.967
_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  0.0224
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50007
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        32.500
_diffrn_reflns_theta_max         34.982
_diffrn_reflns_theta_min         1.982
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.833
_exptl_absorpt_correction_T_max  0.4370
_exptl_absorpt_correction_T_min  0.3573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS-2009/1 (Bruker,2010) was used for absorption correction. wR2(int) 
 was 0.0618 before and 0.0375 after correction. The Ratio of minimum to maximum 
 transmission is 0.8176. The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         9270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+1.1294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0342
_refine_ls_wR_factor_ref         0.0351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8368
_reflns_number_total             9270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02201_si_002.cif
_cod_data_source_block           7
_cod_database_code               4515789
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Uiso(H14A)=Uiso(H14B)=Uiso(H14C)=FVAR(1)
 Uiso(H15A)=Uiso(H15B)=Uiso(H15C)=FVAR(2)
 Uiso(H3AA)=Uiso(H3AB)=Uiso(H3AC)=Uiso(H3BD)=Uiso(H3BE)=Uiso(H3BF)=FVAR(3)
 Uiso(H2A)=Uiso(H2B)=Uiso(H2C)=FVAR(4)
 Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(5)
 Uiso(H12A)=Uiso(H12B)=Uiso(H12C)=FVAR(6)
 Uiso(H11A)=Uiso(H11B)=Uiso(H11C)=FVAR(7)
 Fixed Sof: H3AA(0.67) H3AB(0.67) H3AC(0.67) H3BD(0.33) H3BE(0.33) H3BF(0.33)
3.a Riding coordinates:
 C3(H3AA,H3AB,H3AC,H3BD,H3BE,H3BF), C6(H6), C7(H7), C8(H8), C10(H10), C13(H13)
3.b Rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              4644