Equilibrium Studies in Solution Involving Nickel(II) Complexes of Flexidentate Schiff Base Ligands: Isolation and Structural Characterization of the Planar Red and Octahedral Green Species Involved in the Equilibrium
Suman Mukhopadhyay; Debdas Mandal; Dipesh Ghosh; Israel Goldberg; Muktimoy Chaudhury; Inorganic Chemistry 42 (2003) 8439–8445; doi:10.1021/ic0346174

data_4312677
_publ_section_title
;
 Equilibrium Studies in Solution Involving Nickel(II) Complexes of
 Flexidentate Schiff Base Ligands: Isolation and Structural
 Characterization of the Planar Red and Octahedral Green Species Involved
 in the Equilibrium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8439
_journal_page_last               8445
_journal_paper_doi               10.1021/ic0346174
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C13 H28 N4 Ni O12 S'
_chemical_formula_weight         523.16
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.6760(9)
_cell_angle_beta                 72.6110(10)
_cell_angle_gamma                64.2060(6)
_cell_formula_units_Z            2
_cell_length_a                   9.05700(10)
_cell_length_b                   9.52800(10)
_cell_length_c                   14.2900(2)
_cell_measurement_reflns_used    4425
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.65
_cell_volume                     1054.55(2)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi & Omega 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  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9204
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.8990
_exptl_absorpt_correction_T_min  0.7726
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                4425
_reflns_number_total             4673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0346174si20030604_081154_3.cif
_cod_data_source_block           Compound-2
_cod_database_code               4312677