Trapping Unstable Terminal M-O Multiple Bonds of Monocyclopentadienyl Niobium and Tantalum Complexes with Lewis Acids
Javier Sánchez-Nieves; Luis M. Frutos; Pascual Royo; Obis Castaño; Eberhardt Herdtweck; Marta E. G. Mosquera; Inorganic Chemistry 49 (2010) 10642–10648; doi:10.1021/ic1016609

data_4317074
_publ_contact_author_address
;
       Department Chemie,
       Lehrstuhl f\"ur Anorganische Chemie,
       Technische Universit\"at M\"unchen,
       Lichtenbergstrasse 4,
       D-85747 Garching bei M\"unchen,
       Germany.

       Departamento de Qu\'imica Inorg\'anica
       Facultad de Farmacia
       Universidad de Alcal\'a
       Campus Universitario
       28871 Alcal\'a de Henares
       Spain
;
_publ_contact_author_email       eberhardt.herdtweck@ch.tum.de
_publ_contact_author_fax         '+49(0)89 289 13473'
_publ_contact_author_name
;
       Dr. Eberhardt Herdtweck
       Dr. Marta E. G. Mosquera
;
_publ_contact_author_phone       '+49(0)89 289 13143'
_publ_section_title
;
 Trapping Unstable Terminal M-O Multiple Bonds of Monocyclopentadienyl
 Niobium and Tantalum Complexes with Lewis Acids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10642
_journal_page_last               10648
_journal_paper_doi               10.1021/ic1016609
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C28 H15 Al Cl2 F15 O Ta'
_chemical_formula_weight         931.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_method           SHELXL-97
_cell_angle_alpha                90.945(9)
_cell_angle_beta                 110.889(7)
_cell_angle_gamma                104.017(8)
_cell_formula_units_Z            2
_cell_length_a                   10.7086(10)
_cell_length_b                   11.2122(10)
_cell_length_c                   14.0319(14)
_cell_measurement_reflns_used    125
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.566
_cell_measurement_theta_min      4.244
_cell_volume                     1517.3(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34266
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    3.944
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_correction_T_min  0.166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.382
_refine_diff_density_max         1.572
_refine_diff_density_min         -1.919
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.0122(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0216P)^2^+1.0156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                6182
_reflns_number_total             6811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016609_si_001_1.cif
_cod_data_source_block           3a
_cod_original_cell_volume        1517.3(2)
_cod_database_code               4317074