Tetrakis[tris(2,2'-bi-1<i>H</i>-benzimidazole)nickel(II)] bis(phosphate) sulfate
Ling, Chun-Sheng; Yan, Lin; Acta Crystallographica Section E 64 (2008) m1399–; doi:10.1107/S1600536808032571

data_2219750
_publ_section_title
;
 Tetrakis[tris(2,2'-bi-1<i>H</i>-benzimidazole)nickel(II)]
 bis(phosphate) sulfate
;
_journal_coeditor_code           AT2642
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1399
_journal_paper_doi               10.1107/S1600536808032571
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C14 H10 N4)3]4 (P O4)2 (S O4)'
_chemical_formula_moiety         '4C42 H30 N12 Ni1 2+ , 2P O4 3- , S O4 2-'
_chemical_formula_sum            'C168 H120 N48 Ni4 O12 P2 S'
_chemical_formula_weight         3331.96
_chemical_name_systematic
;
Tetrakis[tris(2,2'-bi-1<i>H</i>-benzimidazole)nickel(II)]
bis(phosphate) sulfate
;
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_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                   24.964(7)
_cell_length_b                   24.964(7)
_cell_length_c                   24.964(7)
_cell_measurement_reflns_used    3375
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.21
_cell_measurement_theta_min      2.31
_cell_volume                     15558(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20222
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.8761
_exptl_absorpt_correction_T_min  0.8335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6872
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.203
_refine_ls_abs_structure_details 'Flack (1983), 1182 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0528P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                1782
_reflns_number_total             2551
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2642.cif
_cod_data_source_block           I
_cod_database_code               2219750
_cod_database_fobs_code          2219750