Redetermination of bis(<i>O</i>,<i>O</i>'-diethyl dithiophosphato-κ^2^<i>S</i>,<i>S</i>')nickel(II)
Paliwoda, Damian; Chojnacki, Jarosław; Mietlarek-Kropidłowska, Anna; Becker, Barbara; Acta Crystallographica Section E 65 (2009) m662–; doi:10.1107/S160053680901767X

data_2222138
_publ_section_title
;
 Redetermination of bis(<i>O</i>,<i>O</i>'-diethyl
 dithiophosphato-\k^2^<i>S</i>,<i>S</i>')nickel(II)
;
_journal_coeditor_code           SI2169
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m662
_journal_paper_doi               10.1107/S160053680901767X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C4 H10 O2 P1 S2)2]'
_chemical_formula_moiety         'C8 H20 Ni1 O4 P2 S4'
_chemical_formula_sum            'C8 H20 Ni O4 P2 S4'
_chemical_formula_weight         429.13
_chemical_melting_point          378
_chemical_name_systematic
;
bis(<i>O</i>,<i>O</i>'-diethyl
dithiophosphato-\k^2^<i>S</i>,<i>S</i>')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
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.820(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4810(4)
_cell_length_b                   10.2777(3)
_cell_length_c                   8.7541(3)
_cell_measurement_reflns_used    5670
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      32.286
_cell_measurement_theta_min      1.9772
_cell_volume                     919.49(6)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2008)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '4-axis \k geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction KM-4-CCD'
_diffrn_measurement_method       '\w (0.75\% width)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7073
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.5304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2008)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.55
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.323
_refine_ls_extinction_coef       0.027(2)
_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   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         2012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0441P)^2^+0.3217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                1768
_reflns_number_total             2012
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2169.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C8 H20 Ni1 O4 P2 S4'
_cod_database_code               2222138
_cod_database_fobs_code          2222138