Synthesis and Structure of Nickel-Containing Cuboidal Clusters Derived from [W3Se4(H2O)9]4+. Site-Differentiated Substitution at the Nickel Site in the Series [W3NiQ4(H2O)10]4+(Q = S, Se)
Hernández-Molina, Rita; Sokolov, Maxim N.; Clausen, Maria; Clegg, William; Inorganic Chemistry 45 (2006) 10567–10575; doi:10.1021/ic061146n

data_4332967
_publ_section_title
;
 Synthesis and Structure of Nickel-Containing Cuboidal Clusters Derived
 from [W3Se4(H2O)9]4+. Site-Differentiated Substitution at the Nickel Site
 in the Series [W3NiQ4(H2O)10]4+(Q = S, Se)
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10567
_journal_page_last               10575
_journal_paper_doi               10.1021/ic061146n
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C56 H128 Ni2 O60 S8 Se8 W6'
_chemical_formula_weight         3870.26
_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                77.827(2)
_cell_angle_beta                 84.375(2)
_cell_angle_gamma                82.585(2)
_cell_formula_units_Z            1
_cell_length_a                   11.6936(6)
_cell_length_b                   14.7813(7)
_cell_length_c                   16.4159(8)
_cell_measurement_reflns_used    6902
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.62
_cell_volume                     2743.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23255
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.498
_exptl_absorpt_correction_T_max  0.395
_exptl_absorpt_correction_T_min  0.106
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.678
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.00059(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         12290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+16.1449P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                11042
_reflns_number_total             12290
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic061146nsup1.cif
_cod_data_source_block           rh1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332967