A Reduced β-Diketiminato-Ligated Ni3H4 Unit Catalyzing H/D Exchange
Stefan Pfirrmann; Christian Limberg; Christian Herwig; Christina Knispel; Beatrice Braun; Eckhard Bill; Reinhard Stösser; Journal of the American Chemical Society 132 (2010) 13684–13691; doi:10.1021/ja106266v

data_4103174
_publ_section_title
;
 A Reduced \b-Diketiminato-Ligated Ni3H4 Unit Catalyzing H/D Exchange
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13684
_journal_page_last               13691
_journal_paper_doi               10.1021/ja106266v
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         ' C58 H86 K2 N4 Ni3, C6 H14'
_chemical_formula_sum            'C64 H100 K2 N4 Ni3'
_chemical_formula_weight         1179.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 124.252(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.9902(8)
_cell_length_b                   19.8449(6)
_cell_length_c                   12.4857(6)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     3274.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9965
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.9229
_exptl_absorpt_correction_T_min  0.7920
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         .690
_refine_diff_density_min         -.554
_refine_diff_density_rms         .059
_refine_ls_extinction_coef       0.00068(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   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         5122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                4013
_reflns_number_total             5122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106266v_si_003.cif
_cod_data_source_block           chris160
_cod_original_cell_volume        3274.9(2)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4103174