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_4088574
_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            'C46 H30 B Cl4 F15 N3 V'
_chemical_formula_weight         1113.28
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.884(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.806(8)
_cell_length_b                   20.402(13)
_cell_length_c                   20.961(15)
_cell_measurement_reflns_used    11141
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     4522(5)
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46992
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.9568
_exptl_absorpt_correction_T_min  0.8596
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10291
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0721P)^2^+1.1701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                7643
_reflns_number_total             10291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00200_si_002.cif
_cod_data_source_block           vanadium3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/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_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088574