Anion dependent deprotection of a thioether group in Schiff base NS2 ligands results in new mononuclear and dinuclear thiolato nickel complexes
Bouwman, Elisabeth; Henderson, Richard K.; Powell, Annie K.; Reedijk, Jan; Smeets, Wilberth J. J.; Spek, Anthony L.; Veldman, Nora; Wocadlo, Sigrid; Journal of the Chemical Society, Dalton Transactions  (1998) 3495–; doi:10.1039/a805428b

data_7027003
_publ_section_title
;
 Anion dependent deprotection of a thioether group in Schiff base NS2
 ligands results in new mononuclear and dinuclear thiolato nickel
 complexes
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3495
_journal_paper_doi               10.1039/a805428b
_journal_year                    1998
_chemical_formula_moiety         'C34 H36 N2 Ni S4'
_chemical_formula_sum            'C34 H36 N2 Ni S4'
_chemical_formula_weight         659.60
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.45(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.665(4)
_cell_length_b                   14.800(7)
_cell_length_c                   14.923(6)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      10.4
_cell_volume                     3229(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0929
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3429
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        0.81
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0006(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   1.209
_refine_ls_goodness_of_fit_obs   1.383
_refine_ls_hydrogen_treatment    'riding positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         3224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.232
_refine_ls_restrained_S_obs      1.383
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_obs          0.0520
_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^)+(0.0509P)^2^+13.3441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1744
_refine_ls_wR_factor_obs         0.1506
_reflns_number_observed          2049
_reflns_number_total             3228
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            805428bsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+13.3441P] 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^)+(0.0509P)^2^+13.3441P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3229.2(22)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7027003