Electronic Structure Control of the Nucleophilicity of Transition Metal-Thiolate Complexes: An Experimental and Theoretical Study
Derek C. Fox; Adam T. Fiedler; Heather L. Halfen; Thomas C. Brunold; Jason A. Halfen; Journal of the American Chemical Society 126 (2004) 7627–7638; doi:10.1021/ja039419q

data_4112675
_publ_section_title
;
 Electronic Structure Control of the Nucleophilicity of Transition
 Metal-Thiolate Complexes: An Experimental and Theoretical Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7627
_journal_page_last               7638
_journal_paper_doi               10.1021/ja039419q
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C49 H51 B N4 Ni S'
_chemical_formula_weight         797.52
_chemical_name_common            'complex 3'
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.16(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.860(1)
_cell_length_b                   18.999(1)
_cell_length_c                   20.344(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.37
_cell_measurement_theta_min      9.54
_cell_volume                     4196.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'omega 2-theta scans'
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7808
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.00
_diffrn_standards_interval_time  '5400 seconds'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9572
_exptl_absorpt_correction_type   'psi-scan corrections'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0332P)^2^+1.1972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                4911
_reflns_number_total             7391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039419qsi20031104_024531.cif
_cod_data_source_block           3
_cod_database_code               4112675