Bis(3-acetyl-6-methyl-2-oxo-2<i>H</i>-pyran-4-olato)bis(dimethyl sulfoxide)nickel(II)
Djedouani, Amel; Boufas, Sihem; Bendaas, Abderrahmen; Allain, Magali; Bouet, Gilles; Acta Crystallographica Section E 65 (2009) m1205–m1206; doi:10.1107/S1600536809034655

data_2223414
_publ_section_title
;
 Bis(3-acetyl-6-methyl-2-oxo-2<i>H</i>-pyran-4-olato)bis(dimethyl
 sulfoxide)nickel(II)
;
_journal_coeditor_code           HG2559
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1205
_journal_page_last               m1206
_journal_paper_doi               10.1107/S1600536809034655
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C8 H7 O4)2 (C2 H6 O S)2]'
_chemical_formula_moiety         'C20 H26 Ni O10 S2'
_chemical_formula_sum            'C20 H26 Ni O10 S2'
_chemical_formula_weight         549.24
_chemical_name_systematic
;
Bis(3-acetyl-6-methyl-2-oxo-2<i>H</i>-pyran-4-olato)bis(dimethyl
sulfoxide)nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 123.525(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3850(10)
_cell_length_b                   6.2833(4)
_cell_length_c                   19.7434(15)
_cell_measurement_reflns_used    2190
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.82
_cell_volume                     1177.40(18)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'DIAMOND (Brandenburg, 1998) and Mercury (Macrae <i>et al.</i>,  2006)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14084
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.9019
_exptl_absorpt_correction_T_min  0.9019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.973
_refine_ls_extinction_coef       0.0084(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^+0.3428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                1962
_reflns_number_total             2628
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2559.cif
_cod_data_source_block           I
_cod_original_cell_volume        1177.40(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2223414
_cod_database_fobs_code          2223414