Structural study of four complexes of the <i>M</i>-N~2~S~2~ type derived from diethylphenylazothioformamide and the metals palladium, platinum, copper and nickel
Nielsen, Kim T.; Harris, Pernille; Bechgaard, Klaus; Krebs, Frederik C.; Acta Crystallographica Section B 63 (2007) 151–156; doi:10.1107/S0108768106047306

data_2102683
_publ_section_title
;
 Structural study of four complexes of the <i>M</i>-N~2~S~2~ type
 derived from diethylphenylazothioformamide and the metals palladium,
 platinum, copper and nickel
;
_journal_coeditor_code           BK5045
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              151
_journal_page_last               156
_journal_paper_doi               10.1107/S0108768106047306
_journal_volume                  63
_journal_year                    2007
_chemical_formula_sum            'C22 H30 N6 Ni S2'
_chemical_formula_weight         501.35
_chemical_name_systematic
;
 Trans-(di(N,N-diethyl-(2-phenyldiazenyl)thioformamide-\kS,\kN^2^))nickel
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2852(3)
_cell_length_b                   10.2852(3)
_cell_length_c                   22.2862(13)
_cell_measurement_reflns_used    12044
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      31.004
_cell_measurement_theta_min      2.695
_cell_volume                     2357.55(17)
_computing_cell_refinement       'Bruker SMART (Bruker AXS,1998)'
_computing_data_collection       'Bruker SMART (Bruker AXS,1998)'
_computing_data_reduction        'Bruker SHELXTL (Sheldrick,2001)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick,2001)'
_computing_publication_material
;
WinGX publication routines (Farrugia, 1999)
;
_computing_structure_refinement  'Bruker SHELXTL (Sheldrick,2001)'
_computing_structure_solution    'Bruker SHELXTL (Sheldrick,2001)'
_diffrn_ambient_temperature      118
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega 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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31608
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS,ver2.03 (Sheldrick,2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Quadratic bi-pyramidal shaped'
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.262
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.3442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                3436
_reflns_number_total             3630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bk5045.cif
_cod_data_source_block           NiL20
_cod_database_code               2102683