Tetra- and Dinuclear Nickel(II)-Vanadium(IV/V) Heterometal Complexes of a Phenol-Based N2O2 Ligand: Synthesis, Structures, and Magnetic and Redox Properties
Debdas Mandal; Pabitra Baran Chatterjee; Rakesh Ganguly; Edward R. T. Tiekink; Rodolphe Clérac; Muktimoy Chaudhury; Inorganic Chemistry 47 (2008) 584–591; doi:10.1021/ic701925j

data_4304422
_publ_section_title
;
Tetra- and Dinuclear Nickel(II)-Vanadium(IV/V) Heterometal Complexes of a
Phenol-Based N2O2 Ligand: Synthesis, Structures, and Magnetic and Redox
Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              584
_journal_page_last               591
_journal_paper_doi               10.1021/ic701925j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C58 H70 N4 Ni2 O12 V2 '
_chemical_formula_sum            'C58 H70 N4 Ni2 O12 V2'
_chemical_formula_weight         1234.44
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3548(6)
_cell_length_b                   17.9752(7)
_cell_length_c                   23.1855(10)
_cell_measurement_reflns_used    6788
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.1
_cell_volume                     5565.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            44603
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.8
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.65
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.24
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         8127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.24
_refine_ls_R_factor_all          0.095
_refine_ls_R_factor_gt           0.069
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+6.3258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.149
_refine_ls_wR_factor_ref         0.162
_reflns_number_gt                6190
_reflns_number_total             8127
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701925j-file001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     '-P 2ac 2ab '
_cod_original_formula_sum        'C58 H70 N4 Ni2 O12 V2 '
_cod_database_code               4304422