{4,4'-Di-<i>tert</i>-butyl-6,6'-bis(dimethoxymethyl)-2,2'-[propane-1,3-diylbis(nitrilomethylidyne)]bis(thiophenolato)-κ^4^<i>S,N,N</i>',<i>S</i>'}nickel(II)
Bjernemose, Jens K.; McKenzie, Christine J.; Raithby, Paul R.; Teat, Simon J.; Acta Crystallographica Section E 60 (2004) m1841–m1843; doi:10.1107/S1600536804028879

data_2204811
_publ_section_title
{4,4'-Di-<i>tert</i>-butyl-6,6'-bis(dimethoxymethyl)-2,2'-[propane-1,3-diylbis(nitrilomethylidyne)]bis(thiophenolato)-\k^4^<i>S,N,N</i>',<i>S</i>'}nickel(II)
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1841
_journal_page_last               m1843
_journal_paper_doi               10.1107/S1600536804028879
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (C31 H44 N2 O4 S2)]'
_chemical_formula_moiety         'C31 H44 N2 Ni1 O4 S2'
_chemical_formula_sum            'C31 H44 N2 Ni O4 S2'
_chemical_formula_weight         631.51
_chemical_name_common            (pabtp)Ni
_chemical_name_systematic
;
{4,4'-Di-tert-butyl-6,6'-bis(dimethoxymethyl)-2,2'-[propane-1,3-
diylbis(nitrilomethylidyne)]bis(thiophenolato)-\k^4^S,N,N',S'}nickel(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 102.178(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.352(4)
_cell_length_b                   9.1532(11)
_cell_length_c                   12.1556(15)
_cell_measurement_reflns_used    6249
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.23
_cell_measurement_theta_min      2.77
_cell_volume                     3083.5(7)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       '0.20 \% \w rotation, 3 s a frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6881
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9981
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.77
_refine_diff_density_min         -1.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         9981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.098
_refine_ls_R_factor_gt           0.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.169P)^2^+0.2945P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.213
_refine_ls_wR_factor_ref         0.228
_reflns_number_gt                8220
_reflns_number_total             9981
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wk6035.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C31 H44 N2 Ni1 O4 S2'
_cod_database_code               2204811
_cod_database_fobs_code          2204811