Synthesis, spectroscopic and electrochemical study of nickel-(II) and -(I) complexes with Schiff-base ligands giving a NN′OS co-ordination sphere
Pereira, Eulália; Gomes, Lígia; Castro, Baltazar de; Journal of the Chemical Society, Dalton Transactions  (1998) 629–; doi:10.1039/a705685k

data_7028187
_publ_section_title
;
 Synthesis, spectroscopic and electrochemical study of nickel-(II) and
 -(I) complexes with Schiff-base ligands giving a NN&#x2032;OS
 co-ordination sphere
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              629
_journal_paper_doi               10.1039/a705685k
_journal_year                    1998
_chemical_formula_analytical     'C17 H20 N2 Ni S2'
_chemical_formula_moiety         ' '
_chemical_formula_structural     'C17 H20 N2 Ni S2'
_chemical_formula_sum            'C17 H20 N2 Ni O S2'
_chemical_formula_weight         391.16
_chemical_name_common            '[Ni(cdsalpd)]'
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.94(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.924(5)
_cell_length_b                   16.889(8)
_cell_length_c                   12.051(6)
_cell_measurement_reflns_used    3707
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.09
_cell_volume                     1798.9(16)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Stoe stadi IV 4-circle-diffractometer'
_diffrn_measurement_method       'Profile fitted 2\q/\w scans (Clegg, 1981)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4091
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         15
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  ****
_exptl_absorpt_correction_T_min  ****
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.058
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_obs          0.0271
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.6495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0749
_refine_ls_wR_factor_obs         0.0687
_reflns_number_observed          3289
_reflns_number_total             3713
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            k705685sup1.cif
_cod_data_source_block           l4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.6495P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.6495P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7028187