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_4304425
_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         'C54 H55 N3 Ni O7 V'
_chemical_formula_sum            'C54 H55 N3 Ni O7 V'
_chemical_formula_weight         967.66
_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                83.331(1)
_cell_angle_beta                 86.659(1)
_cell_angle_gamma                77.124(1)
_cell_formula_units_Z            2
_cell_length_a                   11.2938(4)
_cell_length_b                   12.8014(5)
_cell_length_c                   17.2832(7)
_cell_measurement_reflns_used    7703
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      2.2
_cell_volume                     2418.07(16)
_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 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.018
_diffrn_reflns_av_sigmaI/netI    0.038
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20669
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.2
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            green-yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.29
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         13282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.057
_refine_ls_R_factor_gt           0.044
_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^)+(0.0642P)^2^+0.3942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.111
_refine_ls_wR_factor_ref         0.120
_reflns_number_gt                10655
_reflns_number_total             13282
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701925j-file004.cif
_cod_data_source_block           4
_cod_original_cell_volume        2418.08(16)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_database_code               4304425