Nickel(II) complexes with N2OS and N2S2 co-ordination spheres: reduction and spectroscopic study of the corresponding Ni(I) complexes
Gomes, Lígia; Pereira, Eulália; de Castro, Baltazar; Journal of the Chemical Society, Dalton Transactions  (2000) 1373–; doi:10.1039/a908330h

data_7009044
_publ_section_title
;
 Nickel(II) complexes with N2OS and N2S2 co-ordination spheres:
 reduction and spectroscopic study of the corresponding Ni(I) complexes
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1373
_journal_paper_doi               10.1039/a908330h
_journal_year                    2000
_chemical_formula_sum            'C17 H14 Cl2 N2 Ni O S'
_chemical_formula_weight         423.95
_chemical_name_systematic
; 
 2-{[1,2-ethanediyilbis(nitrilomethyllidyne)]-2'dichlorophenolate)
benzenethiolate}nickel(II) 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.511(2)
_cell_length_b                   11.616(4)
_cell_length_c                   19.228(6)
_cell_measurement_reflns_used    378
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      56.3
_cell_measurement_theta_min      9.5
_cell_volume                     1677.6(9)
_computing_cell_refinement       'Stoe Expose'
_computing_data_collection       'Stoe Expose'
_computing_data_reduction        'Stoe - Integrate'
_computing_molecular_graphics    Ortep
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       Stoe-IPDS
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1252
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12282
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         5.04
_exptl_absorpt_coefficient_mu    1.576
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark orange '
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       'Transparent needles '
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         .893
_refine_diff_density_min         -.750
_refine_diff_density_rms         .159
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_obs          0.0656
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1064P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2009
_refine_ls_wR_factor_obs         0.1562
_reflns_number_observed          2699
_reflns_number_total             4011
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908330h.txt
_cod_data_source_block           l3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1064P)^2^+0.0000P] 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^)+( 0.1064P)^2^+0.0000P] 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)2(1)2(1)
_cod_database_code               7009044