A low-coordinate nickel(ii) hydride complex and its reactivity
Pfirrmann, Stefan; Limberg, Christian; Ziemer, Burkhard; Dalton Transactions  (2008) 6689–6691; doi:10.1039/b816136b

data_7004815
_publ_section_title
;
 A low-coordinate nickel(ii) hydride complex and its reactivity
;
_journal_issue                   47
_journal_name_full               'Dalton Transactions'
_journal_page_first              6689
_journal_page_last               6691
_journal_paper_doi               10.1039/b816136b
_journal_year                    2008
_chemical_formula_moiety         'C36 H51 N4 Ni'
_chemical_formula_sum            'C36 H51 N4 Ni'
_chemical_formula_weight         598.52
_chemical_name_common
;
(N,N'-Bis(2,6-di-isopropylphenyl)-pentan-2,4-di-iminato-N,N')
-(4-dimethylaminopyridine-N)-nickel(i)
;
_chemical_name_systematic
;
(N,N'-Bis(2,6-di-isopropylphenyl)-pentan-2,4-di-iminato-N,N')
-(4-dimethylaminopyridine-N)-nickel(I)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.210(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6270(5)
_cell_length_b                   22.8973(13)
_cell_length_c                   16.9475(10)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     3347.0(3)
_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 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device       'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,201 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  0.1074
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26845
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.9305
_exptl_absorpt_correction_T_min  0.7425
_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            orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.500
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881.
SHELXL97 set here the Flack parameter to 0.0 without su. It may be because
our crystal was twice twinned and 3 BASF parameters had to be calculated.
So the parameter becoms meaningless.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         11309
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0921
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1762P)^2^+3.6848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.2655
_reflns_number_gt                8731
_reflns_number_total             11309
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b816136b.txt
_cod_data_source_block           pfirr13
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7004815