Spectrophotometric Study of the Equilibria between Nickel(II) Schiff-Base Complexes and Alkaline Earth or Nickel(II) Cations in Acetonitrile Solution
Laura Carbonaro; Mauro Isola; Piero La Pegna; Lucio Senatore; Fabio Marchetti; Inorganic Chemistry 38 (1999) 5519–5525; doi:10.1021/ic990189j

data_4322416
_publ_section_title
;
 Spectrophotometric Study of the Equilibria between Nickel(II) Schiff-Base
 Complexes and Alkaline Earth or Nickel(II) Cations in Acetonitrile
 Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5519
_journal_page_last               5525
_journal_paper_doi               10.1021/ic990189j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C32 H32 Cl2 N4 Ni3 O14'
_chemical_formula_weight         943.65
_chemical_name_systematic
;
di-[(N,N'-ethylenebis(salicylideneiminato)nickel(ii)]-di-aquo-nickel(ii)perc
hlorate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 118.98(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3020(15)
_cell_length_b                   21.818(3)
_cell_length_c                   17.796(4)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      5.0
_cell_volume                     3499.1(13)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w/2\q
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3848
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.22
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Ruby red'
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          '0.28 mm'
_exptl_crystal_size_mid          '0.14 mm'
_exptl_crystal_size_min          '0.07 mm'
_refine_diff_density_max         1.168
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=3D1/[\s^2^(Fo^2^)+(0.0778P)^2^+6.7532P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1650
_reflns_number_gt                1956
_reflns_number_total             3085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990189j_2.cif
_cod_data_source_block           nini2
_cod_original_cell_volume        3499.1(10)
_cod_database_code               4322416