Unusual room temperature activation of 1,2-dialkoxyalkanes by niobium and tantalum pentachlorides
Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Dalton Transactions  (2008) 7026–7035; doi:10.1039/b810210d

data_7004680
_publ_section_title
;
 Unusual room temperature activation of 1,2-dialkoxyalkanes by niobium
 and tantalum pentachlorides
;
_journal_issue                   48
_journal_name_full               'Dalton Transactions'
_journal_page_first              7026
_journal_page_last               7035
_journal_paper_doi               10.1039/b810210d
_journal_year                    2008
_chemical_formula_sum            'C4 H10 Cl8 O3 Ta2'
_chemical_formula_weight         751.62
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.1160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6388(3)
_cell_length_b                   26.0083(13)
_cell_length_c                   9.9726(5)
_cell_measurement_reflns_used    8234
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.400
_cell_measurement_theta_min      2.6175
_cell_volume                     1676.99(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18476
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    14.305
_exptl_absorpt_correction_T_max  0.2786
_exptl_absorpt_correction_T_min  0.2080
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.336
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0194P)^2^+0.7379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                3236
_reflns_number_total             3666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b810210d.txt
_cod_data_source_block           p21n
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7004680