Unusual Structural Types in Nickel Cluster Chemistry from the Use of Pyridyl Oximes: Ni5, Ni12Na2, and Ni14 Clusters
Theocharis C. Stamatatos; Albert Escuer; Khalil A. Abboud; Catherine P. Raptopoulou; Spyros P. Perlepes; George Christou; Inorganic Chemistry 47 (2008) 11825–11838; doi:10.1021/ic801555e

data_4306740
_publ_section_title
;
Unusual Structural Types in Nickel Cluster Chemistry from the Use of
Pyridyl Oximes: Ni5, Ni12Na2, and Ni14 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11825
_journal_page_last               11838
_journal_paper_doi               10.1021/ic801555e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C58 H53 N20 Ni5 O30.5'
_chemical_formula_weight         1811.75
_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                98.269(17)
_cell_angle_beta                 96.167(16)
_cell_angle_gamma                106.223(16)
_cell_formula_units_Z            2
_cell_length_a                   17.680(9)
_cell_length_b                   14.989(9)
_cell_length_c                   15.584(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.0
_cell_measurement_theta_min      5.5
_cell_volume                     3877(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       '\q/2\q scans'
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11828
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        -0.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.286
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             1850
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         11353
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+9.0636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1678
_reflns_number_gt                8682
_reflns_number_total             11353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801555e_si_002_3.cif
_cod_data_source_block           pexs855
_cod_original_formula_sum        'C58 H53 N20 Ni5 O30.50'
_cod_database_code               4306740