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_4326461
_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
'2(C38 H54 N4 O12 V2 W2), C1.50 Cl1.50 O, 2(C H Cl3), 2(C H3 O) '
_chemical_formula_sum            'C84.5 H116 Cl7.5 N8 O30 V4 W4'
_chemical_formula_weight         2928.95
_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'
_cell_angle_alpha                72.9803(9)
_cell_angle_beta                 80.3509(9)
_cell_angle_gamma                88.1885(9)
_cell_formula_units_Z            1
_cell_length_a                   10.1338(3)
_cell_length_b                   15.6779(5)
_cell_length_c                   19.7520(6)
_cell_measurement_reflns_used    21614
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.2
_cell_volume                     2957.74(16)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      113.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24398
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_exptl_absorpt_coefficient_mu    4.415
_exptl_absorpt_correction_T_max  0.414
_exptl_absorpt_correction_T_min  0.336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             1434.50
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.97
_refine_diff_density_min         -0.99
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     677
_refine_ls_number_reflns         10737
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0444P)^2^+17.9114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                9929
_reflns_number_total             10737
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic2009094_si_002.cif
_cod_data_source_block           '_VW'
_cod_original_cell_volume        2957.75(15)
_cod_original_formula_sum        'C84.50 H116 Cl7.50 N8 O30 V4 W4 '
_cod_database_code               4326461