R-Allyl Nickel(II) Complexes with Chelating N-Heterocyclic Carbenes: Synthesis, Structural Characterization, and Catalytic Activity
Ben\?ítez Junquera, Lourdes; Puerta, M. Carmen; Valerga, Pedro; Organometallics 31 (2012) 2175–; doi:10.1021/om200937d

data_4076331
_publ_section_title
;
 R-Allyl Nickel(II) Complexes with Chelating N-Heterocyclic Carbenes:
 Synthesis, Structural Characterization, and Catalytic Activity
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2175
_journal_paper_doi               10.1021/om200937d
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C32 H12 B F24, C18 H18 N3 Ni, C4 H10 O'
_chemical_formula_sum            'C54 H40 B F24 N3 Ni O'
_chemical_formula_weight         1272.41
_chemical_name_common
;
(\h^3^-Allyl)-{1-(2-picolyl)-3-(phenyl)-imidazolylidene-\k^2^ N,C}-nickel (II)
tetrakis{3,5-bis(trifluoromethyl)phenyl}borate dichloromethane diethylether 
solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.180(6)
_cell_length_b                   12.912(3)
_cell_length_c                   28.568(6)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.951
_cell_measurement_theta_min      2.205
_cell_volume                     11110(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 vers. 1.08 (Farrugia, 2005)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '1700 omega scan frames, 0.3 deg, 10 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36542
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.43
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0076
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.681
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         9795
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+108.9115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2305
_refine_ls_wR_factor_ref         0.2373
_reflns_number_gt                8795
_reflns_number_total             9795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200937d_si_002.cif
_cod_data_source_block           pv1002
_cod_original_cell_volume        11109(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4076331