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_4312676
_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 H37 N3 Ni O14 S'
_chemical_formula_weight         550.23
_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                100.3600(6)
_cell_angle_beta                 109.7881(7)
_cell_angle_gamma                93.5550(10)
_cell_formula_units_Z            2
_cell_length_a                   8.86900(10)
_cell_length_b                   11.9180(2)
_cell_length_c                   12.1220(2)
_cell_measurement_reflns_used    4914
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.49
_cell_volume                     1175.49(3)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11257
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.8663
_exptl_absorpt_correction_T_min  0.7566
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+1.8776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                4914
_reflns_number_total             5285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0346174si20030604_081154_2.cif
_cod_data_source_block           Compound-1b
_cod_database_code               4312676