Synthesis and Catalytic Properties of Molybdenum(VI) Complexes with Tris(3,5-dimethyl-1-pyrazolyl)methane
Patrícia Neves; Sandra Gago; Salete S. Balula; André D. Lopes; Anabela A. Valente; Luís Cunha-Silva; Filipe A. Almeida Paz; Martyn Pillinger; João Rocha; Carlos M. Silva; Isabel S. Gonçalves; Inorganic Chemistry 50 (2011) 3490–3500; doi:10.1021/ic102456z

data_4324869
_publ_contact_author_address
; Department of Chemistry
  University of Aveiro
  CICECO
  3810-193
  Aveiro
  Portugal
;
_publ_contact_author_email       igoncalves@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
;
 Synthesis and Catalytic Properties of Molybdenum(VI) Complexes with
 Tris(3,5-dimethyl-1-pyrazolyl)methane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3490
_journal_page_last               3500
_journal_paper_doi               10.1021/ic102456z
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C32 H44 Mo2 N12 O5, 2(B F4)'
_chemical_formula_sum            'C32 H44 B2 F8 Mo2 N12 O5'
_chemical_formula_weight         1042.29
_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             '01 February 2010'
_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_cell_angle_alpha                73.354(2)
_cell_angle_beta                 75.827(2)
_cell_angle_gamma                68.6830(10)
_cell_formula_units_Z            6
_cell_length_a                   17.9727(5)
_cell_length_b                   18.8894(5)
_cell_length_c                   23.4086(7)
_cell_measurement_reflns_used    2532
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.57
_cell_measurement_theta_min      2.37
_cell_volume                     7004.4(4)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            190551
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.9295
_exptl_absorpt_correction_T_min  0.9184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       Block
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         3.774
_refine_diff_density_min         -2.835
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1509
_refine_ls_number_reflns         25019
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1783P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2531
_refine_ls_wR_factor_ref         0.2712
_reflns_number_gt                16812
_reflns_number_total             25019
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic102456z_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        7004.4(3)
_cod_database_code               4324869