An Octanuclear Molybdenum(VI) Complex Containing Coordinatively Bound 4,4'-di-tert-Butyl-2,2'-Bipyridine, [Mo8O22(OH)4(di-tBu-bipy)4]: Synthesis, Structure, and Catalytic Epoxidation of Bio-Derived Olefins
Tatiana R. Amarante; Patrícia Neves; Cátia Tomé; Marta Abrantes; Anabela A. Valente; Filipe A. Almeida Paz; Martyn Pillinger; Isabel S. Gonçalves; Inorganic Chemistry 51 (2012) 3666–3676; doi:10.1021/ic202640a

data_4328669
_publ_contact_author_address
; Department of Chemistry
  University of Aveiro
  CICECO
  3810-193
  Aveiro
  Portugal
;
_publ_contact_author_email       igoncalves@dq.ua.pt
_publ_contact_author_fax         '+351 234 370084'
_publ_contact_author_name        'Professor Isabel Goncalves'
_publ_contact_author_phone       '+351 234 378190'
_publ_section_title
;
 An Octanuclear Molybdenum(VI) Complex Containing Coordinatively Bound
 4,4'-di-tert-Butyl-2,2'-Bipyridine, [Mo8O22(OH)4(di-tBu-bipy)4]:
 Synthesis, Structure, and Catalytic Epoxidation of Bio-Derived Olefins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3666
_journal_page_last               3676
_journal_paper_doi               10.1021/ic202640a
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C72 H100 Mo8 N8 O26'
_chemical_formula_sum            'C72 H100 Mo8 N8 O26'
_chemical_formula_weight         2261.12
_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_date             '30 November 2011'
_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_cell_angle_alpha                65.98(4)
_cell_angle_beta                 85.61(5)
_cell_angle_gamma                84.51(5)
_cell_formula_units_Z            1
_cell_length_a                   12.90(2)
_cell_length_b                   13.111(18)
_cell_length_c                   13.46(2)
_cell_measurement_reflns_used    521
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.45
_cell_measurement_theta_min      2.30
_cell_volume                     2068(5)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT+ (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\w / \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3014
_diffrn_reflns_av_sigmaI/netI    0.5457
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21721
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  0.9876
_exptl_absorpt_correction_T_min  0.9876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       Block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.500
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         7211
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.3317
_refine_ls_R_factor_gt           0.0995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1181P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.3114
_reflns_number_gt                2086
_reflns_number_total             7211
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic202640a_si_002.cif
_cod_data_source_block           2
_cod_database_code               4328669