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_4103173
_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         '2(C58 H84 K N4 Ni2), C7 H16, C6 H14'
_chemical_formula_sum            'C64.5 H99 K N4 Ni2'
_chemical_formula_weight         1087.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3031(14)
_cell_length_b                   21.144(3)
_cell_length_c                   25.310(3)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.25
_cell_volume                     6048.9(13)
_computing_cell_refinement       'Bruker SAINT+ (1999)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'APEX Area Detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'INCOATEC microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            70946
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.9370
_exptl_absorpt_correction_T_min  0.7583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (1996)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         .913
_refine_diff_density_min         -.736
_refine_diff_density_rms         .087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   .15(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         11884
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0485P)^2^+8.4320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                8671
_reflns_number_total             11884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106266v_si_002.cif
_cod_data_source_block           twin
_cod_original_formula_sum        'C64.50 H99 K N4 Ni2'
_cod_database_code               4103173