Complexation to FeII, NiII, and ZnII of Multidentate Ligands Resulting from Condensation of 2-Pyridinecarboxaldehyde with α,ω-Triamines: Selective Imidazolidine/Hexahydropyrimidine Ring Opening Revisited
Nicolas Bréfuel; Christine Lepetit; Sergiu Shova; Françoise Dahan; Jean-Pierre Tuchagues; Inorganic Chemistry 44 (2005) 8916–8928; doi:10.1021/ic050791b

data_4310049
_publ_section_title
;
Complexation to FeII, NiII, and ZnII of Multidentate Ligands Resulting from
Condensation of 2-Pyridinecarboxaldehyde with \a,\w-Triamines: Selective
Imidazolidine/Hexahydropyrimidine Ring Opening Revisited
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8916
_journal_page_last               8928
_journal_paper_doi               10.1021/ic050791b
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C20 H23 Fe N7 S2'
_chemical_formula_sum            'C20 H23 Fe N7 S2'
_chemical_formula_weight         481.42
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 101.851(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0433(9)
_cell_length_b                   9.5361(7)
_cell_length_c                   14.4027(15)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      51.8
_cell_measurement_theta_min      4.2
_cell_volume                     1081.16(19)
_computing_cell_refinement       'STOE-IPDS software (Stoe, 2.87, 1997)'
_computing_data_collection       'STOE-IPDS software (Stoe, 2.87, 1997)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.1208
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7696
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'c.f. r.h. blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         1917
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.127
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+10.0963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2162
_refine_ls_wR_factor_ref         0.2194
_reflns_number_gt                1771
_reflns_number_total             1917
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050791bsi20050817_040730.cif
_cod_data_source_block           '[FeLC(NCS)]NCS'
_cod_original_cell_volume        1081.16(18)
_cod_database_code               4310049