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_4333699
_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_absolute_configuration ad
_chemical_formula_moiety         'C38 H37 N2 Ni1 O1 P1'
_chemical_formula_sum            'C38 H37 N2 Ni O P'
_chemical_formula_weight         627.41
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-08-17
_audit_creation_method           CRYSTALS_ver_14.05
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7830(2)
_cell_length_b                   15.0674(2)
_cell_length_c                   21.6014(15)
_cell_measurement_reflns_used    22147
_cell_measurement_temperature    123
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     3184.1(2)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22147
_diffrn_reflns_theta_full        27.484
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.118
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 12
_diffrn_standards_number         7309
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.58
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.002(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9425
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.0015360
_refine_ls_shift/su_mean         3.3815005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 47.5 58.5 21.3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0458
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0458
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                6875
_reflns_number_total             7309
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0271
_oxford_refine_ls_scale          1.0587(11)
_oxford_reflns_number_all        7294
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic3021904_si_002_2.cif
_cod_data_source_block           3a_ZL175
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C38 H37 N2 Ni1 O1 P1'
_cod_database_code               4333699