Dioxomolybdenum(VI) Complexes with Ene-1,2-dithiolate Ligands: Synthesis, Spectroscopy, and Oxygen Atom Transfer Reactivity
Hideki Sugimoto; Susumu Tatemoto; Koichiro Suyama; Hiroyuki Miyake; Shinobu Itoh; Chao Dong; Jing Yang; Martin L. Kirk; Inorganic Chemistry 48 (2009) 10581–10590; doi:10.1021/ic901112s

data_4303561
_publ_contact_author_email       sugimoto@mls.eng.osaka-u.ac.jp
_publ_contact_author_fax         +81-6-6879-7933
_publ_contact_author_name        'Hideki Sugimoto'
_publ_contact_author_phone       +81-6-6879-7933
_publ_section_title
;
Dioxomolybdenum(VI) Complexes with Ene-1,2-dithiolate Ligands: Synthesis,
Spectroscopy, and Oxygen Atom Transfer Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10581
_journal_page_last               10590
_journal_paper_doi               10.1021/ic901112s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C88 H104 Mo2 N2 O20 P2 S8 '
_chemical_formula_sum            'C44 H52 Mo N O10 P S4'
_chemical_formula_weight         1010.05
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.658(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.610(2)
_cell_length_b                   13.5961(14)
_cell_length_c                   19.795(2)
_cell_measurement_reflns_used    21558
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4.0
_cell_volume                     4605.4(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR2002
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44597
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2096.00
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.34
_refine_diff_density_min         -1.23
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  7794 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     1199
_refine_ls_number_reflns         16894
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.0196
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0024Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                16834
_reflns_number_total             18152
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic901112s_si_002_4.cif
_cod_data_source_block           '__6'
_cod_original_cell_volume        4605.3(8)
_cod_original_formula_sum        'C88 H104 Mo2 N2 O20 P2 S8 '
_cod_database_code               4303561