Chemistry and Catalytic Activity of Molybdenum(VI)-Pyrazolylpyridine Complexes in Olefin Epoxidation. Crystal Structures of Monomeric Dioxo, Dioxo-μ-oxo, and Oxodiperoxo Derivatives
Ana C. Coelho; Mariela Nolasco; Salete S. Balula; Margarida M. Antunes; Cláudia C. L. Pereira; Filipe A. Almeida Paz; Anabela A. Valente; Martyn Pillinger; Paulo Ribeiro-Claro; Jacek Klinowski; Isabel S. Gonçalves; Inorganic Chemistry 50 (2011) 525–538; doi:10.1021/ic101384p

data_4324201
_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
;
 Chemistry and Catalytic Activity of Molybdenum(VI)-Pyrazolylpyridine
 Complexes in Olefin Epoxidation. Crystal Structures of Monomeric Dioxo,
 Dioxo-\m-oxo, and Oxodiperoxo Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              525
_journal_page_last               538
_journal_paper_doi               10.1021/ic101384p
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C8 H7 Cl2 Mo N3 O2, C8 H8 N3, Cl'
_chemical_formula_sum            'C16 H15 Cl3 Mo N6 O2'
_chemical_formula_weight         525.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '06 February 2010'
_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.1428(8)
_cell_length_b                   8.2630(3)
_cell_length_c                   19.8535(7)
_cell_measurement_reflns_used    9606
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.22
_cell_measurement_theta_min      2.77
_cell_volume                     4106.9(2)
_computing_cell_refinement       'APEX2 '
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL '
_computing_structure_refinement  'SHELXTL '
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'omega/phi 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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            42926
_diffrn_reflns_theta_full        36.35
_diffrn_reflns_theta_max         36.35
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.8665
_exptl_absorpt_correction_T_min  0.8169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         9914
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+5.2216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                8090
_reflns_number_total             9914
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101384p_si_001.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4324201