β-Diketiminato Nickel(I) Complexes with Very Weak Ligation Allowing for H2and N2Activation
Pfirrmann, Stefan; Yao, Shenglai; Ziemer, Burkhard; Stösser, Reinhard; Driess, Matthias; Limberg, Christian; Organometallics 28 (2009) 6855–; doi:10.1021/om9007983

data_4070432
_publ_section_title
;
 \b-Diketiminato Nickel(I) Complexes with Very Weak Ligation Allowing for
 H2and N2Activation
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6855
_journal_paper_doi               10.1021/om9007983
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C42 H61 N2 Ni'
_chemical_formula_sum            'C42 H61 N2 Ni'
_chemical_formula_weight         652.64
_chemical_name_systematic
; 
 (\h^2^-Toluene)-(N,N'-bis(2,6-di-isopropylphenyl)-2,2,6,6-tetramethyl
heptan-3,5-di-iminato-N,N')-nickel(I) 
;
_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                 96.818(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9120(4)
_cell_length_b                   16.9945(5)
_cell_length_c                   22.2217(9)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     3716.8(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,180 exposures'
_diffrn_radiation_collimation    '0.5 mm diameter monocapillary'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'long fine focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27049
_diffrn_reflns_theta_full        26.25
_diffrn_reflns_theta_max         26.25
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.9169
_exptl_absorpt_correction_T_min  0.8094
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
The correction was carried out by ABSCOR (Stoe, 1997), a modification of
DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166.
In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones.
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.830
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0292P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                4680
_reflns_number_total             7461
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om9007983_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4070432