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_4324202
_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         'C16 H14 Cl2 Mo2 N6 O5, C2 H3 N'
_chemical_formula_sum            'C18 H17 Cl2 Mo2 N7 O5'
_chemical_formula_weight         674.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 93.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.856(2)
_cell_length_b                   12.715(3)
_cell_length_c                   16.935(3)
_cell_measurement_reflns_used    10685
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     2332.6(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'SHELXTL (Bruker 2001)'
_computing_publication_material  'SHELXTL (Bruker 2001)'
_computing_structure_refinement  'SHELXTL (Bruker 2001)'
_computing_structure_solution    'SIR-92 (Altomare at al. 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12968
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_description       Block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.360
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5328
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.274
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+17.9162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                4683
_reflns_number_total             5328
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101384p_si_002.cif
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4324202