Bis(1,1,5,5-tetramethyl-2-thiobiuretato)nickel(II)
Jonathan D Crane; Matthew Whittingham; Acta Crystallographica Section E 60 (2004) m449–m451; doi:10.1107/S1600536804006294

data_2203459
_publ_section_title
;
 Bis(1,1,5,5-tetramethyl-2-thiobiuretato)nickel(II)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m449
_journal_page_last               m451
_journal_paper_doi               10.1107/S1600536804006294
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (C6 H12 N3 O1 S1)2]'
_chemical_formula_moiety         'C12 H24 N6 Ni O2 S2'
_chemical_formula_sum            'C12 H24 N6 Ni O2 S2'
_chemical_formula_weight         407.20
_chemical_name_systematic
;
Bis(1,1,5,5-tetramethyl-2-thiobiuretato)nickel(II)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9350(10)
_cell_length_b                   7.0123(5)
_cell_length_c                   18.4739(18)
_cell_measurement_reflns_used    10003
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.20
_cell_volume                     1805.2(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (STOE 2001)'
_computing_data_reduction        'X-RED (STOE 2001)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia 1997)'
_computing_publication_material  'WinGX and PLATON (Spek 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'X-STEP32 (STOE 2001) and WinGX (Farrugia 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS-II area-detector'
_diffrn_measurement_method       \w
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18236
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.6298
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 2001)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.258
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0271P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0595
_reflns_number_gt                1936
_reflns_number_total             2820
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6184.cif
_cod_data_source_block           I
_cod_database_code               2203459
_cod_database_fobs_code          2203459