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_4070434
_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         'C74 H114 Br2 Li2 N4 Ni2 O4'
_chemical_formula_sum            'C74 H114 Br2 Li2 N4 Ni2 O4'
_chemical_formula_weight         1414.81
_chemical_name_systematic
; 
 Bis((\m^3^-bromido)-bis(tetrahydrofuran-O-)-(\m^2^-lithium)-(N,N'-
bis(2,6-di-isopropylphenyl)pentan-2,4-di-iminato-N,N')-nickel(I)) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.549(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8673(6)
_cell_length_b                   19.8655(5)
_cell_length_c                   17.5029(5)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     7600.6(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,231 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  0.1791
_diffrn_reflns_av_sigmaI/netI    0.2296
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36919
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.593
_exptl_absorpt_correction_T_max  0.9390
_exptl_absorpt_correction_T_min  0.5030
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The crystal faces were indexed by microscope on the diffractometer. After 
that a numerical absorption correction basing on a Gaussian algorithsm 
was applied, which is implemented in the X-RED program (Stoe, 2002).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         16561
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.1682
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0284P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                7492
_reflns_number_total             16561
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om9007983_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4070434