Synthesis and Single-crystal Characterization of the Square Planar Complex [Ni{(SPPh2)2N-S,S'}2].2THF
Eugenio Simón-Manso; Mauricio Valderrama; Daphne Boys; Inorganic Chemistry 40 (2001) 3647–3649; doi:10.1021/ic001184l

data_4319920
_publ_section_title
;
 Synthesis and Single-crystal Characterization of the Square Planar
 Complex [Ni{(SPPh2)2N-S,S'}2].2THF
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3647
_journal_page_last               3649
_journal_paper_doi               10.1021/ic001184l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C56 H56 N2 Ni O2 P4 S4'
_chemical_formula_weight         1099.86
_chemical_name_systematic
;
 Bis(dithioimidodiphosphinate)nickel(II) ditetrahydrophuran
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                113.600(10)
_cell_angle_beta                 90.660(10)
_cell_angle_gamma                99.98(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6860(10)
_cell_length_b                   11.588(2)
_cell_length_c                   13.564(2)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     1368.5(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Siemens R3m/V 4-circle diffractometer'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0142
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6698
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 'every 98 reflections'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_meas      ?
_exptl_crystal_description       brick
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.058
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          -0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+0.2607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1310
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                4932
_reflns_number_total             6323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001184l.cif
_cod_data_source_block           eug
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1368.5(3)
_cod_database_code               4319920