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_4103175
_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 K N4 Ni3, C4 H10 O'
_chemical_formula_sum            'C62 H96 K N4 Ni3 O'
_chemical_formula_weight         1128.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.221(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0286(8)
_cell_length_b                   21.2222(11)
_cell_length_c                   20.5735(12)
_cell_measurement_reflns_used    22937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.51
_cell_measurement_theta_min      3.99
_cell_volume                     6115.4(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'PLATON (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            128657
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.7913
_exptl_absorpt_correction_T_min  0.7354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON (1990)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         .362
_refine_diff_density_min         -.429
_refine_diff_density_rms         .044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         12022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+2.3815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                10598
_reflns_number_total             12022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106266v_si_004.cif
_cod_data_source_block           chris164new_raw
_cod_database_code               4103175