Metalation of Cyclic Pseudopeptidic Thiosulfinates with Ni(II) and Zn(II) after Ring Opening: A Mechanistic Investigation
Erwan Galardon; Emilie Bourles; Isabelle Artaud; Jean-Claude Daran; Pascal Roussel; Alain Tomas; Inorganic Chemistry 46 (2007) 4515–4522; doi:10.1021/ic062480m

data_4308032
_publ_section_title
;
Metalation of Cyclic Pseudopeptidic Thiosulfinates with Ni(II) and Zn(II)
after Ring Opening: A Mechanistic Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4515
_journal_page_last               4522
_journal_paper_doi               10.1021/ic062480m
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C32 H60 N4 Ni O4 S2'
_chemical_formula_weight         687.67
_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                 112.602(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.833(4)
_cell_length_b                   11.800(2)
_cell_length_c                   19.114(4)
_cell_measurement_temperature    120(2)
_cell_volume                     3505.0(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24233
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.713
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+1.0938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                5458
_reflns_number_total             7225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062480m-file002.cif
_cod_data_source_block           ni
_cod_original_cell_volume        3505.2(12)
_cod_database_code               4308032