Acetate/Di-2-pyridyl Ketone Oximate "Blend" as a Source of High-Nuclearity Nickel(II) Clusters: Dependence of the Nuclearity on the Nature of the Inorganic Anion Present
Theocharis C. Stamatatos; Eleanna Diamantopoulou; Catherine P. Raptopoulou; Vassilis Psycharis; Albert Escuer; Spyros P. Perlepes; Inorganic Chemistry 46 (2007) 2350–2352; doi:10.1021/ic062262t

data_4307761
_publ_section_title
;
Acetate/Di-2-pyridyl Ketone Oximate "Blend" as a Source of
High-Nuclearity Nickel(II) Clusters: Dependence of the Nuclearity on the
Nature of the Inorganic Anion Present
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2350
_journal_page_last               2352
_journal_paper_doi               10.1021/ic062262t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C51.2 H51.2 N13 Ni4 O12.9 S'
_chemical_formula_weight         1321.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.92(2)
_cell_angle_beta                 69.26(3)
_cell_angle_gamma                66.57(3)
_cell_formula_units_Z            2
_cell_length_a                   16.390(13)
_cell_length_b                   15.295(11)
_cell_length_c                   14.013(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      5.3
_cell_volume                     2976(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       \q/2\q
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9218
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             1361
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         8764
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0901P)^2^+6.7646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                6758
_reflns_number_total             8764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062262tsi20061128_095052.cif
_cod_data_source_block           ped566
_cod_original_formula_sum        'C51.20 H51.20 N13 Ni4 O12.90 S'
_cod_database_code               4307761