The reactivity of 1,1-dialkoxyalkanes with niobium and tantalum pentahalides. Formation of coordination compounds, C‒H and C‒C bond activation and the X-ray structure of the stable carboxonium species [Me2CCHC(OMe)Me][NbCl5(OMe)]
Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Dalton Transactions  (2009) 8096–8106; doi:10.1039/b907774j

data_7002336
_publ_section_title
;
 The reactivity of 1,1-dialkoxyalkanes with niobium and tantalum
 pentahalides. Formation of coordination compounds, C--H and C--C bond
 activation and the X-ray structure of the stable carboxonium species
 [Me2C&#xE001;CHC(&#xE001;OMe)Me][NbCl5(OMe)]
;
_journal_issue                   38
_journal_name_full               'Dalton Transactions'
_journal_page_first              8096
_journal_page_last               8106
_journal_paper_doi               10.1039/b907774j
_journal_year                    2009
_chemical_formula_sum            'C4 H12 Cl6 O4 Ta2'
_chemical_formula_weight         698.74
_chemical_name_systematic
;
?
;
_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_method           SHELXL-97
_cell_angle_alpha                75.852(3)
_cell_angle_beta                 89.165(3)
_cell_angle_gamma                85.452(3)
_cell_formula_units_Z            2
_cell_length_a                   8.170(2)
_cell_length_b                   9.062(2)
_cell_length_c                   10.634(3)
_cell_measurement_reflns_used    4589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.317
_cell_measurement_theta_min      2.325
_cell_volume                     761.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8153
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    15.413
_exptl_absorpt_correction_T_max  0.2592
_exptl_absorpt_correction_T_min  0.1577
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.121
_refine_diff_density_min         -2.710
_refine_diff_density_rms         0.480
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3374
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+49.0290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                2875
_reflns_number_total             3374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907774j.txt
_cod_data_source_block           ppp-1
_cod_original_cell_volume        761.1(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002336