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_7004816
_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         'C58 H84 N4 Ni2, C4 H10 O'
_chemical_formula_sum            'C62 H94 N4 Ni2 O'
_chemical_formula_weight         1028.83
_chemical_name_common
;
Bis(mu!2$-hydrido)-(N,N'-bis(2,6-di-isopropylphenyl) -pentan-
2,4-di-iminato-N,N')-nickel(ii)
;
_chemical_name_systematic
;
Bis(\m~2~-hydrido)-(N,N'-bis(2,6-di-isopropylphenyl)
-pentan-2,4-di-iminato-N,N')-nickel(II)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.742(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5933(13)
_cell_length_b                   18.187(2)
_cell_length_c                   28.265(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     5890.4(13)
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-rotation,\f-incr.=1.4\%,157 exposures'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            31426
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.8759
_exptl_absorpt_correction_T_min  0.6856
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The program XSHAPE1.02 (Stoe, 1997) was used for crystal optimisation
before the numerical absorption correction basing on a Gaussian algorithsm
and implemented in XRED1.08 (Stoe, 1997) was applied.
In XSHAPE 150 strong reflections with 4 symmetry equivalents in each case
were used for that optimisation. XSHAPE bases on the program HABITUS
(Herrendorf, W. (1993). PhD thesis. Universit\"at Karlsruhe, Germany).
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.00054(11)
_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   0.811
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         10624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.811
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0345P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                6456
_reflns_number_total             10624
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b816136b.txt
_cod_data_source_block           pfirr14
_cod_original_cell_volume        5890.4(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7004816