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_7004679
_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 Nb2 O3'
_chemical_formula_weight         575.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   7.0287(5)
_cell_length_b                   13.5297(9)
_cell_length_c                   17.5555(12)
_cell_measurement_reflns_used    7726
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6855
_cell_measurement_theta_min      2.320
_cell_volume                     1669.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9274
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    2.644
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.6067
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    2.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0138
_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^)+(0.0129P)^2^+0.2996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0325
_refine_ls_wR_factor_ref         0.0327
_reflns_number_gt                3496
_reflns_number_total             3564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b810210d.txt
_cod_data_source_block           p212121
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7004679