A New Ni12 Cluster Based on Polyoxometalate Ligands
Hong-Mei Zhang; Yang-Guang Li; Ying Lu; Rodolphe Clérac; Zhi-Ming Zhang; Qiong Wu; Xiao-Jia Feng; En-Bo Wang; Inorganic Chemistry 48 (2009) 10889–10891; doi:10.1021/ic901552f

data_4303715
_publ_contact_author             'Enbo Wang'
_publ_contact_author_address
;
 Key Laboratory of Polyoxometalate Science of Ministry of Education,
 Department of Chemistry, 
 Northeast Normal University, 
 Changchun, Jilin, 
 130024 
 P. R. China
;
_publ_contact_author_email       wangeb889@nenu.edu.cn
_publ_contact_author_fax         86-431-85098787
_publ_contact_author_phone       86-431-85098787
_publ_section_title
;
A New Ni12 Cluster Based on Polyoxometalate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10889
_journal_page_last               10891
_journal_paper_doi               10.1021/ic901552f
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'H182 Na25 Ni12 O228 P3 W35'
_chemical_formula_weight         11638.39
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.49(3)
_cell_angle_beta                 74.21(3)
_cell_angle_gamma                62.52(3)
_cell_formula_units_Z            2
_cell_length_a                   21.505(4)
_cell_length_b                   22.959(5)
_cell_length_c                   26.026(5)
_cell_measurement_temperature    150(2)
_cell_volume                     10392(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.1041
_diffrn_reflns_av_sigmaI/netI    0.1460
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            70966
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.544
_exptl_absorpt_correction_T_max  0.0835
_exptl_absorpt_correction_T_min  0.0689
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(blessing, 1995,1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10504
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         3.724
_refine_diff_density_min         -3.593
_refine_diff_density_rms         0.544
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1656
_refine_ls_number_reflns         33706
_refine_ls_number_restraints     1574
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                21722
_reflns_number_total             33706
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901552f_si_001.cif
_cod_data_source_block           z66a
_cod_original_cell_volume        10392(4)
_cod_database_code               4303715