Unexpected Formation of Chiral Pincer CNN Nickel Complexes with β-Diketiminato Type Ligands via C-H Activation: Synthesis, Properties, Structures, and Computational Studies
Zhengliang Lu; Srinivas Abbina; Jared R. Sabin; Victor N. Nemykin; Guodong Du; Inorganic Chemistry 52 (2013) 1454–1465; doi:10.1021/ic3021904

data_4333698
_publ_contact_author
;
     Dr. Guodong Du
     Department of Chemistry
     University of North Dakota
     151 Cornell St. Stop 9024
     Grand Forks, ND 58202
     USA

     Dr. Victor N. Nemykin
     Department of Chemistry& Biochemistry
     University of Minnesota Duluth
     1039 University Drive
     Duluth, MN 55812
     USA
;
_publ_contact_author_email       'gdu@chem.und.edu, vnemykin@d.umn.edu'
_publ_contact_author_fax         '1(701)7772331, 1(218)7266729'
_publ_contact_author_phone       1(701)7772241
_publ_section_title
;
 Unexpected Formation of Chiral Pincer CNN Nickel Complexes with
 \b-Diketiminato Type Ligands via C-H Activation: Synthesis, Properties,
 Structures, and Computational Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1454
_journal_page_last               1465
_journal_paper_doi               10.1021/ic3021904
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C85 H73 Ni2 P5'
_chemical_formula_sum            'C85 H73 Ni2 P5'
_chemical_formula_weight         1366.74
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.185(2)
_cell_angle_beta                 88.302(2)
_cell_angle_gamma                61.962(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7404(4)
_cell_length_b                   12.8703(4)
_cell_length_c                   24.2765(7)
_cell_measurement_temperature    173(2)
_cell_volume                     3413.1(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1086
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            86941
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.9551
_exptl_absorpt_correction_T_min  0.6580
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         16805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0561
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                9748
_reflns_number_total             16805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3021904_si_002_1.cif
_cod_data_source_block           4_ZL119byproduct
_cod_original_cell_volume        3413.08(18)
_cod_database_code               4333698