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#$Date: 2016-03-25 08:26:03 +0100 (vie 25 de mar de 2016) $
#$Revision: 179721 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/23/7002336.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7002336
loop_
_publ_author_name
'Marchetti, Fabio'
'Pampaloni, Guido'
'Zacchini, Stefano'
_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CHC(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/[σ²(Fo²)+(0.0415P)²+49.0290P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.567(2) 0.033(2) 0.2516(14) 0.025(4) Uani 1 1 d . . .
H1A H 0.4804 0.0881 0.1915 0.038 Uiso 1 1 calc R . .
H1B H 0.5965 -0.0666 0.2336 0.038 Uiso 1 1 calc R . .
H1C H 0.6640 0.0924 0.2403 0.038 Uiso 1 1 calc R . .
C2 C 0.423(3) 0.428(2) 0.1837(17) 0.030(4) Uani 1 1 d . . .
H2A H 0.5201 0.4078 0.1338 0.045 Uiso 1 1 calc R . .
H2B H 0.4158 0.5351 0.1889 0.045 Uiso 1 1 calc R . .
H2C H 0.3242 0.4091 0.1407 0.045 Uiso 1 1 calc R . .
C3 C 0.938(2) -0.008(2) 0.7602(15) 0.021(3) Uani 1 1 d . . .
H3A H 0.9110 0.0963 0.7079 0.032 Uiso 1 1 calc R . .
H3B H 0.8400 -0.0649 0.7706 0.032 Uiso 1 1 calc R . .
H3C H 1.0239 -0.0586 0.7167 0.032 Uiso 1 1 calc R . .
C4 C 0.976(3) 0.431(2) 0.6772(18) 0.035(4) Uani 1 1 d . . .
H4A H 1.0949 0.4267 0.6635 0.053 Uiso 1 1 calc R . .
H4B H 0.9362 0.5352 0.6808 0.053 Uiso 1 1 calc R . .
H4C H 0.9216 0.4040 0.6055 0.053 Uiso 1 1 calc R . .
Cl1 Cl 0.7470(5) 0.2203(5) 0.4636(4) 0.0228(8) Uani 1 1 d . . .
Cl2 Cl 0.4339(6) 0.3415(5) 0.6180(4) 0.0260(8) Uani 1 1 d . . .
Cl3 Cl 0.1778(5) 0.1643(5) 0.4818(4) 0.0210(8) Uani 1 1 d . . .
Cl4 Cl 1.2338(5) 0.2303(5) 0.9646(4) 0.0222(8) Uani 1 1 d . . .
Cl5 Cl 0.8891(5) 0.3465(5) 1.0969(4) 0.0239(8) Uani 1 1 d . . .
Cl6 Cl 0.6722(5) 0.1522(5) 0.9487(4) 0.0210(8) Uani 1 1 d . . .
O1 O 0.5077(14) 0.0116(13) 0.3866(9) 0.018(2) Uani 1 1 d . . .
O2 O 0.4349(13) 0.3306(12) 0.3116(10) 0.016(2) Uani 1 1 d U . .
O3 O 0.9976(14) -0.0014(13) 0.8878(10) 0.018(2) Uani 1 1 d . . .
O4 O 0.9399(13) 0.3282(12) 0.7952(11) 0.018(2) Uani 1 1 d . . .
Ta1 Ta 0.46173(7) 0.19532(7) 0.46545(5) 0.01496(19) Uani 1 1 d . . .
Ta2 Ta 0.95287(7) 0.19318(7) 0.95236(6) 0.01492(19) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 O1 Ta1 120.3(10) . . ?
C1 O1 Ta1 125.5(9) . 2_656 ?
Ta1 O1 Ta1 110.9(4) . 2_656 ?
C2 O2 Ta1 174.6(11) . . ?
C3 O3 Ta2 120.3(9) . . ?
C3 O3 Ta2 125.4(10) . 2_757 ?
Ta2 O3 Ta2 110.2(4) . 2_757 ?
C4 O4 Ta2 164.6(12) . . ?
O2 Ta1 O1 94.3(4) . . ?
O2 Ta1 O1 163.2(4) . 2_656 ?
O1 Ta1 O1 69.1(4) . 2_656 ?
O2 Ta1 Cl2 104.8(4) . . ?
O1 Ta1 Cl2 160.7(3) . . ?
O1 Ta1 Cl2 91.9(3) 2_656 . ?
O2 Ta1 Cl3 91.6(4) . . ?
O1 Ta1 Cl3 92.8(3) . . ?
O1 Ta1 Cl3 86.4(3) 2_656 . ?
Cl2 Ta1 Cl3 89.09(15) . . ?
O2 Ta1 Cl1 91.8(4) . . ?
O1 Ta1 Cl1 88.3(3) . . ?
O1 Ta1 Cl1 90.7(3) 2_656 . ?
Cl2 Ta1 Cl1 88.78(15) . . ?
Cl3 Ta1 Cl1 176.36(13) . . ?
O4 Ta2 O3 97.6(5) . . ?
O4 Ta2 O3 166.2(4) . 2_757 ?
O3 Ta2 O3 69.8(4) . 2_757 ?
O4 Ta2 Cl5 103.3(4) . . ?
O3 Ta2 Cl5 158.7(3) . . ?
O3 Ta2 Cl5 89.7(3) 2_757 . ?
O4 Ta2 Cl6 92.3(4) . . ?
O3 Ta2 Cl6 87.0(3) . . ?
O3 Ta2 Cl6 92.7(3) 2_757 . ?
Cl5 Ta2 Cl6 88.14(14) . . ?
O4 Ta2 Cl4 89.8(4) . . ?
O3 Ta2 Cl4 93.4(3) . . ?
O3 Ta2 Cl4 85.4(3) 2_757 . ?
Cl5 Ta2 Cl4 90.71(15) . . ?
Cl6 Ta2 Cl4 177.83(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.481(17) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O2 1.430(19) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 O3 1.463(17) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 O4 1.41(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
Cl1 Ta1 2.359(4) . ?
Cl2 Ta1 2.331(4) . ?
Cl3 Ta1 2.358(4) . ?
Cl4 Ta2 2.356(4) . ?
Cl5 Ta2 2.339(4) . ?
Cl6 Ta2 2.355(4) . ?
O1 Ta1 2.047(11) . ?
O1 Ta1 2.132(11) 2_656 ?
O2 Ta1 1.793(11) . ?
O3 Ta2 2.049(11) . ?
O3 Ta2 2.130(11) 2_757 ?
O4 Ta2 1.813(11) . ?
Ta1 O1 2.132(11) 2_656 ?
Ta2 O3 2.130(11) 2_757 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O2 Ta1 O1 -24(12) . . . . ?
C2 O2 Ta1 O1 -34(12) . . . 2_656 ?
C2 O2 Ta1 Cl2 154(12) . . . . ?
C2 O2 Ta1 Cl3 -117(12) . . . . ?
C2 O2 Ta1 Cl1 65(12) . . . . ?
C1 O1 Ta1 O2 22.4(11) . . . . ?
Ta1 O1 Ta1 O2 -176.9(5) 2_656 . . . ?
C1 O1 Ta1 O1 -160.7(14) . . . 2_656 ?
Ta1 O1 Ta1 O1 0.0 2_656 . . 2_656 ?
C1 O1 Ta1 Cl2 -150.6(10) . . . . ?
Ta1 O1 Ta1 Cl2 10.1(14) 2_656 . . . ?
C1 O1 Ta1 Cl3 114.3(10) . . . . ?
Ta1 O1 Ta1 Cl3 -85.0(5) 2_656 . . . ?
C1 O1 Ta1 Cl1 -69.2(10) . . . . ?
Ta1 O1 Ta1 Cl1 91.5(5) 2_656 . . . ?
C4 O4 Ta2 O3 -86(5) . . . . ?
C4 O4 Ta2 O3 -62(5) . . . 2_757 ?
C4 O4 Ta2 Cl5 98(5) . . . . ?
C4 O4 Ta2 Cl6 -174(5) . . . . ?
C4 O4 Ta2 Cl4 7(5) . . . . ?
C3 O3 Ta2 O4 -27.6(11) . . . . ?
Ta2 O3 Ta2 O4 174.1(5) 2_757 . . . ?
C3 O3 Ta2 O3 158.3(14) . . . 2_757 ?
Ta2 O3 Ta2 O3 0.0 2_757 . . 2_757 ?
C3 O3 Ta2 Cl5 141.3(9) . . . . ?
Ta2 O3 Ta2 Cl5 -17.0(13) 2_757 . . . ?
C3 O3 Ta2 Cl6 64.3(10) . . . . ?
Ta2 O3 Ta2 Cl6 -94.0(5) 2_757 . . . ?
C3 O3 Ta2 Cl4 -117.9(10) . . . . ?
Ta2 O3 Ta2 Cl4 83.8(5) 2_757 . . . ?
