Synthesis of (Imido)Vanadium(V) Dichloride Complexes Containing Anionic N-Heterocyclic Carbenes That Contain a Weakly Coordinating Borate Moiety: New MAO-Free Ethylene Polymerization Catalysts
Igarashi, Atsushi; Kolychev, Eugene L.; Tamm, Matthias; Nomura, Kotohiro; Organometallics 35 (2016) 1778–; doi:10.1021/acs.organomet.6b00200

data_4088573
_publ_section_title
;
 Synthesis of (Imido)Vanadium(V) Dichloride Complexes Containing Anionic
 N-Heterocyclic Carbenes That Contain a Weakly Coordinating Borate Moiety:
 New MAO-Free Ethylene Polymerization Catalysts
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1778
_journal_paper_doi               10.1021/acs.organomet.6b00200
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C53.5 H36 B Cl2 F15 N3 V'
_chemical_formula_weight         1138.50
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.032(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.696(3)
_cell_length_b                   19.462(4)
_cell_length_c                   18.195(4)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     4919.5(18)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b29'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b29'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41436
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.8871
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         10998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+11.7398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1759
_reflns_number_gt                8187
_reflns_number_total             10998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00200_si_002.cif
_cod_data_source_block           vanadium2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C53.50 H36 B Cl2 F15 N3 V'
_cod_database_code               4088573