Bis(tetraethylammonium) bis[<i>N</i>,<i>N</i>'-bis(4-methylbenzothiazol-2-yl)pyridine-2,6-dicarboxamidato(2‒)]nickel(II) hemihydrate
Liu, Sheng-Gui; Ni, Chun-Lin; Acta Crystallographica Section E 63 (2007) m1373–m1374; doi:10.1107/S1600536807016492

data_2213394
_publ_section_title
;Bis(tetraethylammonium)
 bis[<i>N</i>,<i>N</i>'-bis(4-methylbenzothiazol-2-yl)pyridine-2,6-dicarboxamidato(2--)]nickel(II)
 hemihydrate
;
_journal_coeditor_code           HK2215
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1373
_journal_page_last               m1374
_journal_paper_doi               10.1107/S1600536807016492
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'(C8 H20 N)2 [Ni (C23 H15 N5 O2 S2)2], 0.5H2 O'
_chemical_formula_moiety
'2(C8 H20 N +), C46 H30 N10 Ni O4 S4 2-, 0.5H2 O'
_chemical_formula_sum            'C62 H71 N12 Ni O4.5 S4'
_chemical_formula_weight         1243.28
_chemical_name_systematic
;
Bis(tetraethylammonium) bis[N,N'-bis(4-methylbenzothiazol-2-yl)pyridine-
2,6-dicarboxamidato(2-)]nickel(II) hemihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.642(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4474(15)
_cell_length_b                   19.514(2)
_cell_length_c                   21.771(2)
_cell_measurement_reflns_used    10496
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      0.0
_cell_volume                     6083.3(10)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32320
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         11915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0524
_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^)+(0.072P)^2^+7.8259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                10496
_reflns_number_total             11951
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2215.cif
_cod_data_source_block           I
_cod_original_cell_volume        6083.2(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C62 H71 N12 Ni1 O4.5 S4'
_cod_database_code               2213394
_cod_database_fobs_code          2213394