Unique Reactivity of a Tetradentate N2S2 Complex of Nickel: Intermediates in the Production of Sulfur Oxygenates
Vincent E. Kaasjager; Elisabeth Bouwman; S. Gorter; Jan Reedijk; Craig A. Grapperhaus; Joseph H. Reibenspies; Jason J. Smee; Marcetta Y. Darensbourg; Agnes Derecskei-Kovacs; Lisa M. Thomson; Inorganic Chemistry 41 (2002) 1837–1844; doi:10.1021/ic010784x

data_4317769
_publ_section_title
;
 Unique Reactivity of a Tetradentate N2S2 Complex of Nickel: Intermediates
 in the Production of Sulfur Oxygenates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1837
_journal_page_last               1844
_journal_paper_doi               10.1021/ic010784x
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C8 H20 N2 Ni O3 S2'
_chemical_formula_weight         315.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   11.659(2)
_cell_length_b                   13.119(3)
_cell_length_c                   16.869(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      12
_cell_volume                     2580.2(9)
_computing_cell_refinement       'CRT (MSC, 1999)'
_computing_data_collection       'CRT (MSC, 1999)'
_computing_data_reduction        'CRT (MSC, 1999)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  diffractometer
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1918
_diffrn_reflns_theta_full        60.05
_diffrn_reflns_theta_max         60.05
_diffrn_reflns_theta_min         5.24
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.175
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00049(6)
_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   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+2.6649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                1512
_reflns_number_total             1918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010784x_2.cif
_cod_data_source_block           md213a
_cod_database_code               4317769