A Remarkable Member of the Polyoxometalates: The Eight-Nickel-Capped α-Keggin Polyoxoazonickelate
Lanjun Dong; Rudan Huang; Yongge Wei; Wei Chu; Inorganic Chemistry 48 (2009) 7528–7530; doi:10.1021/ic9012872

data_4302980
_publ_section_title
;
A Remarkable Member of the Polyoxometalates: The Eight-Nickel-Capped
\a-Keggin Polyoxoazonickelate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7528
_journal_page_last               7530
_journal_paper_doi               10.1021/ic9012872
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C9 H18 N6.5 Ni5 O10 S6.25'
_chemical_formula_weight         871.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            8
_cell_length_a                   13.7540(19)
_cell_length_b                   13.7540(19)
_cell_length_c                   28.029(6)
_cell_measurement_reflns_used    16099
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     5302.3(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker Smart-Apex CCD diffractometer'
_diffrn_measurement_method       '\w scan'
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            16099
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         3.58
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.035
_exptl_absorpt_correction_T_max  0.2952
_exptl_absorpt_correction_T_min  0.2375
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             3500
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.421
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4722
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0920P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                2966
_reflns_number_total             4722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9012872_si_002.cif
_cod_data_source_block           ni20
_cod_original_formula_sum        'C9 H18 N6.50 Ni5 O10 S6.25'
_cod_database_code               4302980