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_4324870
_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         'C16 H24 Mo2 N6 O9, 3(H2 O)'
_chemical_formula_sum            'C16 H30 Mo2 N6 O12'
_chemical_formula_weight         690.34
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '21 January 2010'
_audit_creation_method           'SELEXL-97, manual editing and enCIFer'
_cell_angle_alpha                90.00
_cell_angle_beta                 115.405(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7169(6)
_cell_length_b                   15.6739(8)
_cell_length_c                   13.9182(7)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.20
_cell_volume                     2505.9(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      180(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66423
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  0.9385
_exptl_absorpt_correction_T_min  0.8143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick, G.M. (Univesity of Gottingen, 2007)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6731
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0200P)^2^+2.7601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                5420
_reflns_number_total             6731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102456z_si_003.cif
_cod_data_source_block           3
_cod_database_code               4324870