Novel Heterotetranuclear V2Mo2 or V2W2 Complexes with 4,4'-Di-tert-butyl-2,2'-bipyridine: Syntheses, Crystal Structures, and Catalytic Activities
Shintaro Kodama; Akihiro Nomoto; Shigenobu Yano; Michio Ueshima; Akiya Ogawa; Inorganic Chemistry 50 (2011) 9942–9947; doi:10.1021/ic2009094

data_4326462
_publ_contact_author_address
;
Department of Applied Chemistry
Graduate School of Engineering
Osaka Prefecture University
1-1 Gakuen-cho
Nakaku
Sakai
Osaka 599?8531
Japan
;
_publ_section_title
;
 Novel Heterotetranuclear V2Mo2 or V2W2 Complexes with
 4,4'-Di-tert-butyl-2,2'-bipyridine: Syntheses, Crystal Structures, and
 Catalytic Activities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9942
_journal_page_last               9947
_journal_paper_doi               10.1021/ic2009094
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'C38 H54 Mo2 N4 O12 V2, C38 H36 Mo2 N4 O12 V2, 6(C H Cl3), 2(C Cl3)'
_chemical_formula_sum            'C84 H96 Cl24 Mo4 N8 O24 V4'
_chemical_formula_weight         3040.12
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                105.0638(7)
_cell_angle_beta                 97.1994(7)
_cell_angle_gamma                93.2327(7)
_cell_formula_units_Z            1
_cell_length_a                   10.21631(18)
_cell_length_b                   16.2648(4)
_cell_length_c                   19.0493(4)
_cell_measurement_reflns_used    43682
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.10
_cell_volume                     3019.38(11)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52629
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             1516.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.510
_refine_diff_density_min         -1.600
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     732
_refine_ls_number_reflns         13821
_refine_ls_number_restraints     6
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0804P)^2^+14.3942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1651
_reflns_number_gt                11931
_reflns_number_total             13821
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic2009094_si_003.cif
_cod_data_source_block           V2Mo2(e389)
_cod_database_code               4326462