From 1,2-dialkoxyalkanes to 1,4-dioxanes. A transformation mediated by NbCl(5)via multiple C-O bond cleavage at room temperature.
Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Chemical communications (Cambridge, England)  (2008) 3651–3653; doi:10.1039/b804432e

data_7103277
_publ_section_title
;
 From 1,2-dialkoxyalkanes to 1,4-dioxanes. A transformation mediated by
 NbCl(5)via multiple C-O bond cleavage at room temperature.
;
_journal_issue                   31
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3651
_journal_page_last               3653
_journal_paper_doi               10.1039/b804432e
_journal_year                    2008
_chemical_formula_sum            'C4 H10 Cl3 Nb O3'
_chemical_formula_weight         305.38
_chemical_name_common            trichloro(1,2dimethoxyethane)oxoniobium(V)
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.3270(7)
_cell_length_b                   11.9741(11)
_cell_length_c                   23.187(2)
_cell_measurement_reflns_used    3394
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.127
_cell_measurement_theta_min      3.289
_cell_volume                     2034.2(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 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10475
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  0.8155
_exptl_absorpt_correction_T_min  0.7474
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
G. M. Sheldrick, SADABS, Universitat
Gottingen, Gottingen, Germany
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0274P)^2^+0.3857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                1784
_reflns_number_total             2150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b804432e.txt
_cod_data_source_block           pbca
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7103277