Nickel Complexes of a Pincer NN2 Ligand: Multiple Carbon-Chloride Activation of CH2Cl2 and CHCl3 Leads to Selective Carbon-Carbon Bond Formation
Zsolt Csok; Oleg Vechorkin; Seth B. Harkins; Rosario Scopelliti; Xile Hu; Journal of the American Chemical Society 130 (2008) 8156–8157; doi:10.1021/ja8025938

data_4107970
_publ_section_title
;
 Nickel Complexes of a Pincer NN2 Ligand: Multiple Carbon-Chloride
 Activation of CH2Cl2 and CHCl3 Leads to Selective Carbon-Carbon Bond
 Formation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8156
_journal_page_last               8157
_journal_paper_doi               10.1021/ja8025938
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C22 H25 N3 Ni'
_chemical_formula_sum            'C22 H25 N3 Ni'
_chemical_formula_weight         390.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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                 106.74(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.520(13)
_cell_length_b                   7.298(3)
_cell_length_c                   20.276(13)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.582
_cell_measurement_theta_min      3.180
_cell_volume                     1916(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3882
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, Sheldrick G.M., 2003'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       irregular
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.051
_refine_diff_density_min         -1.783
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.1861
_refine_ls_R_factor_gt           0.1586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+82.5961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3969
_refine_ls_wR_factor_ref         0.4088
_reflns_number_gt                2928
_reflns_number_total             3882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8025938-file007.cif
_cod_data_source_block           cz1032-1
_cod_database_code               4107970